# Electronic Supplementary Material (ESI) for Chemical Science.
# This journal is © The Royal Society of Chemistry 2021

####################################################################### 
# 
# 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. 
# 
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data_Fe_bpp_Noxid_NHoxid_240K
_database_code_depnum_ccdc_archive 'CCDC 1832962'
loop_
_audit_author_name
_audit_author_address
'Ver?nica Jornet Moll?'
;Universitat de Val?ncia
Spain
;
_audit_update_record             
;
2018-10-29 deposited with the CCDC.	2020-11-23 downloaded from the CCDC.
;
# start Validation Reply Form
_vrf_PLAT303_Fe_bpp_Noxid_NHoxid_240K 
;
PROBLEM: Full Occupancy Atom H1O       with # Connections       2.00 Check
RESPONSE: This hydrogen atom is located between two oxygen atoms that belong to different carboxylate groups, forming a very strong hydrogen bond (the distance between the heteroatoms, O5 and O1, is 2.425 \%A). As a proton-transfer reaction is observed between the two carboxylate anions, different H?O distances are observed at different temperatures. Such a type of proton-transfer reaction is common when strong hydrogen bonds are established (see, for example Angew. Chem. Int. Ed. 2002, 41, 48-76).
;
# Added during the CSD deposition process: Monday 29 October 2018 04:34 PM
# end Validation Reply Form


_audit_creation_method           SHELXL-2017/1
_shelx_SHELXL_version_number     2017/1
_chemical_name_systematic        ?
_chemical_name_common            ?
_chemical_melting_point          ?
_chemical_formula_moiety         
'C22 H18 Fe N10 2+, C12 H9 N2 O6 1-, C6 H4 N O3 1-, 5(H2 O)'
_chemical_formula_sum            'C40 H41 Fe N13 O14'
_chemical_formula_weight         983.705

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      triclinic
_space_group_IT_number           2
_space_group_name_H-M_alt        'P -1'
_space_group_name_Hall           '-P 1'

_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'

_cell_length_a                   10.01048(19)
_cell_length_b                   13.6732(3)
_cell_length_c                   17.5596(3)
_cell_angle_alpha                73.5259(18)
_cell_angle_beta                 85.7741(15)
_cell_angle_gamma                69.1588(18)
_cell_volume                     2153.01(8)
_cell_formula_units_Z            2
_cell_measurement_temperature    239.9(2)
_cell_measurement_reflns_used    37492
_cell_measurement_theta_min      2.7110
_cell_measurement_theta_max      27.1370

_exptl_crystal_description       cube
_exptl_crystal_colour            light-red
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    ?
_exptl_crystal_density_diffrn    1.517
_exptl_crystal_F_000             1020.000
_exptl_transmission_factor_min   ?
_exptl_transmission_factor_max   ?
_exptl_crystal_size_max          0.550
_exptl_crystal_size_mid          0.223
_exptl_crystal_size_min          0.139
_exptl_absorpt_coefficient_mu    0.435
_shelx_estimated_absorpt_T_min   ?
_shelx_estimated_absorpt_T_max   ?
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_correction_T_min  0.826
_exptl_absorpt_correction_T_max  0.948
_exptl_absorpt_process_details   
;
CrysAlisPro 1.171.38.46 (Rigaku Oxford Diffraction, 2015)
Empirical absorption correction using spherical harmonics,
 implemented in SCALE3 ABSPACK scaling algorithm.
;
_diffrn_ambient_temperature      239.9(2)
_diffrn_ambient_environment      N~2~
_diffrn_radiation_wavelength     0.71073
_diffrn_radiation_type           MoK\a
_diffrn_source                   'micro-focus sealed X-ray tube'
_diffrn_radiation_monochromator  mirror
_diffrn_measurement_device       'four-circle diffractometer'
_diffrn_measurement_device_type  
;
SuperNova, Single source at offset, Sapphire3
;
_diffrn_measurement_method       'ω scans'
_diffrn_detector_area_resol_mean 16.0267
_diffrn_reflns_number            82269
_diffrn_reflns_av_unetI/netI     0.0516
_diffrn_reflns_av_R_equivalents  0.0431
_diffrn_reflns_limit_h_min       -12
_diffrn_reflns_limit_h_max       12
_diffrn_reflns_limit_k_min       -17
_diffrn_reflns_limit_k_max       17
_diffrn_reflns_limit_l_min       -22
_diffrn_reflns_limit_l_max       22
_diffrn_reflns_theta_min         2.3410
_diffrn_reflns_theta_max         27.4246
_diffrn_reflns_theta_full        24.9737
_diffrn_measured_fraction_theta_max 0.9299
_diffrn_measured_fraction_theta_full 0.9992
_diffrn_reflns_Laue_measured_fraction_max 0.930
_diffrn_reflns_Laue_measured_fraction_full 0.999
_diffrn_reflns_point_group_measured_fraction_max 0.930
_diffrn_reflns_point_group_measured_fraction_full 0.999
_reflns_number_total             9117
_reflns_number_gt                7964
_diffrn_orient_matrix_type       
;
CrysAlisPro convention (1999,Acta A55,543-557)
;
_diffrn_orient_matrix_UB_11      0.0338628000
_diffrn_orient_matrix_UB_12      0.0264470000
_diffrn_orient_matrix_UB_13      0.0173293000
_diffrn_orient_matrix_UB_21      0.0144867000
_diffrn_orient_matrix_UB_22      -0.0435969000
_diffrn_orient_matrix_UB_23      0.0353211000
_diffrn_orient_matrix_UB_31      0.0663089000
_diffrn_orient_matrix_UB_32      -0.0271147000
_diffrn_orient_matrix_UB_33      -0.0151032000
_diffrn_measurement_details      
;
List of Runs (angles in degrees, time in seconds):

  # Type    Start    End  Width  tₑₓₚ   ω     θ     κ     φ   Frames
#--------------------------------------------------------------------------
  1  ω    -96.00  15.72   0.84    7.50    --  -20.19 -77.00 -30.00  133
  2  ω    -57.00  54.72   0.84    7.50    --  -20.19  77.00 -30.00  133
  3  ω    -49.00  52.64   0.84    7.50    --  -20.19  57.00  90.00  121
  4  ω    -51.00  50.64   0.84    7.50    --   21.05 -57.00-150.00  121
  5  ω     -9.00  93.48   0.84    7.50    --   21.05  57.00-120.00  122
  6  ω    -20.00  69.04   0.84    7.50    --   21.05 -99.00 150.00  106
  7  ω    -16.00  95.72   0.84    7.50    --   21.05  77.00 -30.00  133
  8  ω     -9.00  93.48   0.84    7.50    --   21.05  57.00 120.00  122
  9  ω    -57.00  54.72   0.84    7.50    --  -20.19  77.00-150.00  133
 10  ω   -107.00 -34.76   0.84    7.50    --  -20.19 178.00  90.00   86
 11  ω    -20.00  28.72   0.84    7.50    --  -20.19 -99.00 120.00   58
 12  ω    -20.00  28.72   0.84    7.50    --  -20.19 -99.00-180.00   58
 13  ω    -51.00  50.64   0.84    7.50    --   21.05 -57.00 150.00  121
 14  ω    -20.00  69.04   0.84    7.50    --   21.05 -99.00 -30.00  106
 15  ω    -51.00  50.64   0.84    7.50    --   21.05 -57.00-120.00  121
 16  ω    -60.00 101.28   0.84    7.50    --   21.05   0.00-150.00  192
 17  ω    -60.00 101.28   0.84    7.50    --   21.05   0.00-120.00  192
 18  ω    -60.00 101.28   0.84    7.50    --   21.05   0.00 -90.00  192
 19  ω    -60.00 101.28   0.84    7.50    --   21.05   0.00 -60.00  192
 20  ω    -60.00  86.16   0.84    7.50    --   21.05   0.00 -30.00  174
 21  ω    -60.00 101.28   0.84    7.50    --   21.05   0.00-180.00  192
;
_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 1.171.38.43 (Rigaku OD, 2015)
;
_computing_cell_refinement       
;
CrysAlisPro 1.171.38.43 (Rigaku OD, 2015)
;
_computing_data_reduction        
;
CrysAlisPro 1.171.38.43 (Rigaku OD, 2015)
;
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1997)'
_computing_structure_refinement  'SHELXL-2017/1 (Sheldrick, 2017)'
_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)+(0.0366P)²+0.9319P] where P=(Fo²+2Fc²)/3'
_atom_sites_solution_primary     difmap
_atom_sites_solution_secondary   difmap
_atom_sites_solution_hydrogens   mixed
_refine_ls_hydrogen_treatment    hetero
_refine_ls_extinction_method     none
_refine_ls_extinction_coef       .
_refine_ls_number_reflns         9117
_refine_ls_number_parameters     658
_refine_ls_number_restraints     0
_refine_ls_R_factor_all          0.0405
_refine_ls_R_factor_gt           0.0328
_refine_ls_wR_factor_ref         0.0836
_refine_ls_wR_factor_gt          0.0784
_refine_ls_goodness_of_fit_ref   1.047
_refine_ls_restrained_S_all      1.047
_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 0.03323(2) 0.54401(2) 0.23262(2) 0.02231(7) Uani 1 1 d . . . . .
N1 N 0.16361(14) 0.49381(11) 0.41136(8) 0.0297(3) Uani 1 1 d . . . . .
H1N H 0.189(2) 0.5521(17) 0.3963(12) 0.044 Uiso 1 1 d . U . . .
N2 N 0.09582(14) 0.47423(10) 0.35709(7) 0.0259(3) Uani 1 1 d . . . . .
N3 N -0.04417(13) 0.41273(10) 0.27301(7) 0.0249(3) Uani 1 1 d . . . . .
N4 N -0.07844(14) 0.54455(11) 0.12986(7) 0.0287(3) Uani 1 1 d . . . . .
N5 N -0.10541(16) 0.60010(13) 0.05248(8) 0.0351(3) Uani 1 1 d . . . . .
H5N H -0.072(2) 0.6536(18) 0.0315(13) 0.053 Uiso 1 1 d . U . . .
N6 N -0.25868(14) 0.69107(12) 0.30790(8) 0.0291(3) Uani 1 1 d . . . . .
H6N H -0.290(2) 0.6404(17) 0.3261(12) 0.044 Uiso 1 1 d . U . . .
N7 N -0.14554(13) 0.67721(10) 0.25987(7) 0.0247(3) Uani 1 1 d . . . . .
N8 N 0.08015(13) 0.68657(10) 0.17733(7) 0.0224(2) Uani 1 1 d . . . . .
N9 N 0.24132(13) 0.48882(10) 0.17914(7) 0.0247(3) Uani 1 1 d . . . . .
N10 N 0.34296(14) 0.39536(11) 0.17313(8) 0.0286(3) Uani 1 1 d . . . . .
H10N H 0.332(2) 0.3351(17) 0.1987(12) 0.043 Uiso 1 1 d . U . . .
C1 C 0.16981(18) 0.42286(14) 0.48307(9) 0.0355(4) Uani 1 1 d . . . . .
H1 H 0.211118 0.421423 0.529297 0.043 Uiso 1 1 calc R U . . .
C2 C 0.10446(18) 0.35295(13) 0.47603(9) 0.0337(4) Uani 1 1 d . . . . .
H2 H 0.093057 0.294897 0.515547 0.040 Uiso 1 1 calc R U . . .
C3 C 0.05862(16) 0.38832(12) 0.39609(8) 0.0254(3) Uani 1 1 d . . . . .
C4 C -0.02456(16) 0.35423(12) 0.34984(9) 0.0256(3) Uani 1 1 d . . . . .
C5 C -0.08339(17) 0.27370(13) 0.38005(10) 0.0319(3) Uani 1 1 d . . . . .
H5 H -0.068561 0.233308 0.433093 0.038 Uiso 1 1 calc R U . . .
C6 C -0.16488(18) 0.25521(13) 0.32891(11) 0.0365(4) Uani 1 1 d . . . . .
H6 H -0.205653 0.201767 0.347644 0.044 Uiso 1 1 calc R U . . .
C7 C -0.18596(18) 0.31588(14) 0.25003(11) 0.0350(4) Uani 1 1 d . . . . .
H7 H -0.240874 0.303889 0.215564 0.042 Uiso 1 1 calc R U . . .
C8 C -0.12365(16) 0.39487(12) 0.22339(9) 0.0274(3) Uani 1 1 d . . . . .
C9 C -0.13697(16) 0.46748(13) 0.14230(9) 0.0289(3) Uani 1 1 d . . . . .
C10 C -0.20139(19) 0.47385(16) 0.07183(10) 0.0406(4) Uani 1 1 d . . . . .
H10 H -0.249128 0.429871 0.064429 0.049 Uiso 1 1 calc R U . . .
C11 C -0.17840(19) 0.55902(17) 0.01650(10) 0.0437(4) Uani 1 1 d . . . . .
H11 H -0.208036 0.584159 -0.036694 0.052 Uiso 1 1 calc R U . . .
C12 C -0.31296(18) 0.79360(14) 0.31341(10) 0.0340(4) Uani 1 1 d . . . . .
H12 H -0.391033 0.821256 0.342993 0.041 Uiso 1 1 calc R U . . .
C13 C -0.23324(17) 0.85054(14) 0.26782(10) 0.0312(3) Uani 1 1 d . . . . .
H13 H -0.245249 0.923333 0.260224 0.037 Uiso 1 1 calc R U . . .
C14 C -0.13014(16) 0.77509(12) 0.23536(8) 0.0235(3) Uani 1 1 d . . . . .
C15 C -0.01256(16) 0.78382(12) 0.18208(8) 0.0235(3) Uani 1 1 d . . . . .
C16 C 0.00507(17) 0.88048(12) 0.13875(9) 0.0294(3) Uani 1 1 d . . . . .
H16 H -0.060428 0.947421 0.141670 0.035 Uiso 1 1 calc R U . . .
C17 C 0.12289(18) 0.87447(13) 0.09107(10) 0.0324(4) Uani 1 1 d . . . . .
H17 H 0.137164 0.937964 0.061568 0.039 Uiso 1 1 calc R U . . .
C18 C 0.21945(17) 0.77403(12) 0.08726(9) 0.0285(3) Uani 1 1 d . . . . .
H18 H 0.299272 0.769272 0.055879 0.034 Uiso 1 1 calc R U . . .
C19 C 0.19444(16) 0.68069(12) 0.13132(8) 0.0231(3) Uani 1 1 d . . . . .
C20 C 0.28516(16) 0.56876(12) 0.13389(8) 0.0241(3) Uani 1 1 d . . . . .
C21 C 0.41471(17) 0.52503(13) 0.09910(10) 0.0317(3) Uani 1 1 d . . . . .
H21 H 0.467013 0.562624 0.065189 0.038 Uiso 1 1 calc R U . . .
C22 C 0.44780(18) 0.41433(14) 0.12601(10) 0.0333(4) Uani 1 1 d . . . . .
H22 H 0.528590 0.361827 0.113733 0.040 Uiso 1 1 calc R U . . .
N11 N -0.39726(16) 1.01294(12) 0.07123(8) 0.0360(3) Uani 1 1 d . . . . .
O1 O -0.48656(14) 0.67134(10) 0.19374(7) 0.0414(3) Uani 1 1 d . . . . .
O2 O -0.63643(15) 0.78475(11) 0.25850(8) 0.0453(3) Uani 1 1 d . . . . .
O3 O -0.34427(16) 1.08783(12) 0.03369(7) 0.0523(4) Uani 1 1 d . . . . .
C23 C -0.54851(18) 0.76429(14) 0.20702(9) 0.0325(4) Uani 1 1 d . . . . .
C24 C -0.50171(17) 0.85322(13) 0.15433(9) 0.0294(3) Uani 1 1 d . . . . .
C25 C -0.38914(18) 0.83072(14) 0.10340(9) 0.0330(4) Uani 1 1 d . . . . .
H25 H -0.348427 0.761096 0.096833 0.040 Uiso 1 1 calc R U . . .
C26 C -0.56378(19) 0.95877(14) 0.15975(10) 0.0365(4) Uani 1 1 d . . . . .
H26 H -0.641497 0.976395 0.192085 0.044 Uiso 1 1 calc R U . . .
C27 C -0.5111(2) 1.03792(15) 0.11748(10) 0.0397(4) Uani 1 1 d . . . . .
H27 H -0.554183 1.109020 0.120822 0.048 Uiso 1 1 calc R U . . .
C28 C -0.33780(19) 0.91100(15) 0.06270(9) 0.0359(4) Uani 1 1 d . . . . .
H28 H -0.261701 0.895332 0.029044 0.043 Uiso 1 1 calc R U . . .
N12 N -0.49492(14) 0.19034(10) 0.50865(8) 0.0285(3) Uani 1 1 d . . . . .
O4 O -0.36915(13) 0.52274(10) 0.37810(7) 0.0389(3) Uani 1 1 d . . . . .
O5 O -0.51585(16) 0.51493(11) 0.29104(8) 0.0513(4) Uani 1 1 d . . . . .
H1O H -0.501(3) 0.592(2) 0.2459(15) 0.077 Uiso 1 1 d . U . . .
O6 O -0.51090(13) 0.10206(9) 0.55561(7) 0.0372(3) Uani 1 1 d . . . . .
C29 C -0.44567(18) 0.48084(13) 0.35708(10) 0.0315(3) Uani 1 1 d . . . . .
C30 C -0.46317(17) 0.37889(13) 0.41089(9) 0.0281(3) Uani 1 1 d . . . . .
C31 C -0.41711(17) 0.34092(13) 0.48966(9) 0.0307(3) Uani 1 1 d . . . . .
H31 H -0.374509 0.378718 0.510241 0.037 Uiso 1 1 calc R U . . .
C32 C -0.52502(18) 0.31938(13) 0.38233(9) 0.0314(3) Uani 1 1 d . . . . .
H32 H -0.557251 0.343315 0.329618 0.038 Uiso 1 1 calc R U . . .
C33 C -0.53899(18) 0.22557(13) 0.43121(9) 0.0318(3) Uani 1 1 d . . . . .
H33 H -0.578987 0.185861 0.411055 0.038 Uiso 1 1 calc R U . . .
C34 C -0.43398(18) 0.24742(14) 0.53782(9) 0.0319(3) Uani 1 1 d . . . . .
H34 H -0.403416 0.222992 0.590847 0.038 Uiso 1 1 calc R U . . .
N13 N 0.07013(14) 0.94440(11) 0.38123(8) 0.0304(3) Uani 1 1 d . . . . .
O7 O 0.19372(15) 1.22120(11) 0.16277(7) 0.0454(3) Uani 1 1 d . . . . .
O8 O 0.32436(13) 1.20453(10) 0.26591(7) 0.0396(3) Uani 1 1 d . . . . .
O9 O 0.02261(14) 0.86807(10) 0.42592(7) 0.0400(3) Uani 1 1 d . . . . .
C35 C 0.23472(17) 1.18174(13) 0.23358(10) 0.0305(3) Uani 1 1 d . . . . .
C36 C 0.17531(16) 1.09860(12) 0.28616(9) 0.0277(3) Uani 1 1 d . . . . .
C37 C 0.20797(18) 1.05699(13) 0.36706(10) 0.0326(4) Uani 1 1 d . . . . .
H37 H 0.267280 1.080733 0.389907 0.039 Uiso 1 1 calc R U . . .
C38 C 0.08642(18) 1.06051(14) 0.25500(9) 0.0341(4) Uani 1 1 d . . . . .
H38 H 0.060972 1.087197 0.201182 0.041 Uiso 1 1 calc R U . . .
C39 C 0.03573(19) 0.98366(15) 0.30309(10) 0.0365(4) Uani 1 1 d . . . . .
H39 H -0.023144 0.958431 0.281331 0.044 Uiso 1 1 calc R U . . .
C40 C 0.15419(18) 0.98143(13) 0.41387(10) 0.0334(4) Uani 1 1 d . . . . .
H40 H 0.175562 0.955572 0.468165 0.040 Uiso 1 1 calc R U . . .
O1W O 0.72676(16) 0.99346(12) 0.42074(8) 0.0449(3) Uani 1 1 d . . . . .
H1A H 0.807(3) 0.946(2) 0.4227(15) 0.067 Uiso 1 1 d . U . . .
H1B H 0.671(3) 0.961(2) 0.4344(15) 0.067 Uiso 1 1 d . U . . .
O2W O 0.63348(17) 0.12690(12) 0.26622(9) 0.0471(3) Uani 1 1 d . . . . .
H2A H 0.660(3) 0.090(2) 0.3103(16) 0.071 Uiso 1 1 d . U . . .
H2B H 0.545(3) 0.142(2) 0.2666(15) 0.071 Uiso 1 1 d . U . . .
O3W O 0.19603(18) 0.68998(12) 0.36365(9) 0.0486(3) Uani 1 1 d . . . . .
H3A H 0.247(3) 0.712(2) 0.3311(16) 0.073 Uiso 1 1 d . U . . .
H3B H 0.144(3) 0.740(2) 0.3831(16) 0.073 Uiso 1 1 d . U . . .
O4W O 0.04131(18) 0.21752(13) 0.04207(8) 0.0529(4) Uani 1 1 d . . . . .
H4A H -0.033(3) 0.211(2) 0.0577(17) 0.079 Uiso 1 1 d . U . . .
H4B H 0.079(3) 0.216(2) 0.0837(17) 0.079 Uiso 1 1 d . U . . .
O5W O -0.2211(2) 1.17186(16) 0.12167(10) 0.0630(5) Uani 1 1 d . . . . .
H5A H -0.254(3) 1.159(3) 0.1621(19) 0.094 Uiso 1 1 d . U . . .
H5B H -0.261(3) 1.150(2) 0.0931(19) 0.094 Uiso 1 1 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 N8 2.1152(12) . ?
Fe1 N3 2.1242(12) . ?
Fe1 N2 2.1618(12) . ?
Fe1 N9 2.1876(13) . ?
Fe1 N4 2.1885(13) . ?
Fe1 N7 2.1904(13) . ?
N1 C1 1.344(2) . ?
N1 N2 1.3453(17) . ?
N1 H1N 0.88(2) . ?
N2 C3 1.3434(19) . ?
N3 C8 1.3464(19) . ?
N3 C4 1.3467(19) . ?
N4 C9 1.338(2) . ?
N4 N5 1.3487(18) . ?
N5 C11 1.345(2) . ?
N5 H5N 0.89(2) . ?
N6 C12 1.341(2) . ?
N6 N7 1.3517(18) . ?
N6 H6N 0.83(2) . ?
N7 C14 1.3455(19) . ?
N8 C19 1.3428(19) . ?
N8 C15 1.3453(19) . ?
N9 N10 1.3472(18) . ?
N9 C20 1.3476(18) . ?
N10 C22 1.341(2) . ?
N10 H10N 0.86(2) . ?
C1 C2 1.371(2) . ?
C1 H1 0.9300 . ?
C2 C3 1.402(2) . ?
C2 H2 0.9300 . ?
C3 C4 1.470(2) . ?
C4 C5 1.387(2) . ?
C5 C6 1.385(2) . ?
C5 H5 0.9300 . ?
C6 C7 1.385(3) . ?
C6 H6 0.9300 . ?
C7 C8 1.387(2) . ?
C7 H7 0.9300 . ?
C8 C9 1.471(2) . ?
C9 C10 1.404(2) . ?
C10 C11 1.367(3) . ?
C10 H10 0.9300 . ?
C11 H11 0.9300 . ?
C12 C13 1.370(2) . ?
C12 H12 0.9300 . ?
C13 C14 1.394(2) . ?
C13 H13 0.9300 . ?
C14 C15 1.466(2) . ?
C15 C16 1.390(2) . ?
C16 C17 1.387(2) . ?
C16 H16 0.9300 . ?
C17 C18 1.387(2) . ?
C17 H17 0.9300 . ?
C18 C19 1.389(2) . ?
C18 H18 0.9300 . ?
C19 C20 1.465(2) . ?
C20 C21 1.397(2) . ?
C21 C22 1.373(2) . ?
C21 H21 0.9300 . ?
C22 H22 0.9300 . ?
N11 O3 1.3102(17) . ?
N11 C27 1.348(2) . ?
N11 C28 1.354(2) . ?
O1 C23 1.281(2) . ?
O1 H1O 1.25(3) . ?
O2 C23 1.233(2) . ?
C23 C24 1.502(2) . ?
C24 C26 1.382(2) . ?
C24 C25 1.388(2) . ?
C25 C28 1.372(2) . ?
C25 H25 0.9300 . ?
C26 C27 1.376(2) . ?
C26 H26 0.9300 . ?
C27 H27 0.9300 . ?
C28 H28 0.9300 . ?
N12 O6 1.3100(17) . ?
N12 C33 1.357(2) . ?
N12 C34 1.362(2) . ?
O4 C29 1.235(2) . ?
O5 C29 1.279(2) . ?
O5 H1O 1.18(3) . ?
C29 C30 1.506(2) . ?
C30 C31 1.383(2) . ?
C30 C32 1.390(2) . ?
C31 C34 1.378(2) . ?
C31 H31 0.9300 . ?
C32 C33 1.374(2) . ?
C32 H32 0.9300 . ?
C33 H33 0.9300 . ?
C34 H34 0.9300 . ?
N13 O9 1.3286(17) . ?
N13 C39 1.345(2) . ?
N13 C40 1.353(2) . ?
O7 C35 1.242(2) . ?
O8 C35 1.265(2) . ?
C35 C36 1.518(2) . ?
C36 C38 1.388(2) . ?
C36 C37 1.388(2) . ?
C37 C40 1.372(2) . ?
C37 H37 0.9300 . ?
C38 C39 1.374(2) . ?
C38 H38 0.9300 . ?
C39 H39 0.9300 . ?
C40 H40 0.9300 . ?
O1W H1A 0.83(3) . ?
O1W H1B 0.81(3) . ?
O2W H2A 0.80(3) . ?
O2W H2B 0.83(3) . ?
O3W H3A 0.80(3) . ?
O3W H3B 0.84(3) . ?
O4W H4A 0.80(3) . ?
O4W H4B 0.84(3) . ?
O5W H5A 0.76(3) . ?
O5W H5B 0.84(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
N8 Fe1 N3 169.85(5) . . ?
N8 Fe1 N2 114.70(5) . . ?
N3 Fe1 N2 74.28(5) . . ?
N8 Fe1 N9 74.39(5) . . ?
N3 Fe1 N9 109.61(5) . . ?
N2 Fe1 N9 100.04(5) . . ?
N8 Fe1 N4 96.39(5) . . ?
N3 Fe1 N4 74.41(5) . . ?
N2 Fe1 N4 148.65(5) . . ?
N9 Fe1 N4 91.79(5) . . ?
N8 Fe1 N7 74.78(5) . . ?
N3 Fe1 N7 101.16(5) . . ?
N2 Fe1 N7 90.80(5) . . ?
N9 Fe1 N7 149.10(5) . . ?
N4 Fe1 N7 93.72(5) . . ?
C1 N1 N2 111.23(14) . . ?
C1 N1 H1N 131.0(13) . . ?
N2 N1 H1N 117.5(13) . . ?
C3 N2 N1 105.76(12) . . ?
C3 N2 Fe1 116.75(9) . . ?
N1 N2 Fe1 137.47(10) . . ?
C8 N3 C4 120.29(13) . . ?
C8 N3 Fe1 119.65(10) . . ?
C4 N3 Fe1 119.79(10) . . ?
C9 N4 N5 105.70(13) . . ?
C9 N4 Fe1 115.71(10) . . ?
N5 N4 Fe1 138.56(11) . . ?
C11 N5 N4 111.05(15) . . ?
C11 N5 H5N 128.9(14) . . ?
N4 N5 H5N 120.0(14) . . ?
C12 N6 N7 111.35(13) . . ?
C12 N6 H6N 128.7(14) . . ?
N7 N6 H6N 119.6(14) . . ?
C14 N7 N6 104.99(12) . . ?
C14 N7 Fe1 114.56(10) . . ?
N6 N7 Fe1 138.90(10) . . ?
C19 N8 C15 120.35(12) . . ?
C19 N8 Fe1 119.78(10) . . ?
C15 N8 Fe1 119.53(10) . . ?
N10 N9 C20 105.27(12) . . ?
N10 N9 Fe1 139.44(10) . . ?
C20 N9 Fe1 115.18(10) . . ?
C22 N10 N9 111.51(13) . . ?
C22 N10 H10N 130.8(13) . . ?
N9 N10 H10N 117.7(13) . . ?
N1 C1 C2 107.92(14) . . ?
N1 C1 H1 126.0 . . ?
C2 C1 H1 126.0 . . ?
C1 C2 C3 104.77(14) . . ?
C1 C2 H2 127.6 . . ?
C3 C2 H2 127.6 . . ?
N2 C3 C2 110.31(14) . . ?
N2 C3 C4 116.18(13) . . ?
C2 C3 C4 133.43(14) . . ?
N3 C4 C5 121.60(14) . . ?
N3 C4 C3 112.90(13) . . ?
C5 C4 C3 125.45(14) . . ?
C6 C5 C4 118.07(15) . . ?
C6 C5 H5 121.0 . . ?
C4 C5 H5 121.0 . . ?
C7 C6 C5 120.36(15) . . ?
C7 C6 H6 119.8 . . ?
C5 C6 H6 119.8 . . ?
C6 C7 C8 118.77(15) . . ?
C6 C7 H7 120.6 . . ?
C8 C7 H7 120.6 . . ?
N3 C8 C7 120.91(15) . . ?
N3 C8 C9 113.21(13) . . ?
C7 C8 C9 125.87(14) . . ?
N4 C9 C10 110.49(15) . . ?
N4 C9 C8 116.86(13) . . ?
C10 C9 C8 132.65(15) . . ?
C11 C10 C9 104.72(16) . . ?
C11 C10 H10 127.6 . . ?
C9 C10 H10 127.6 . . ?
N5 C11 C10 108.04(15) . . ?
N5 C11 H11 126.0 . . ?
C10 C11 H11 126.0 . . ?
N6 C12 C13 108.03(14) . . ?
N6 C12 H12 126.0 . . ?
C13 C12 H12 126.0 . . ?
C12 C13 C14 104.67(14) . . ?
C12 C13 H13 127.7 . . ?
C14 C13 H13 127.7 . . ?
N7 C14 C13 110.96(13) . . ?
N7 C14 C15 116.93(13) . . ?
C13 C14 C15 132.11(14) . . ?
N8 C15 C16 121.41(14) . . ?
N8 C15 C14 113.08(12) . . ?
C16 C15 C14 125.51(14) . . ?
C17 C16 C15 118.26(15) . . ?
C17 C16 H16 120.9 . . ?
C15 C16 H16 120.9 . . ?
C18 C17 C16 120.17(14) . . ?
C18 C17 H17 119.9 . . ?
C16 C17 H17 119.9 . . ?
C17 C18 C19 118.59(14) . . ?
C17 C18 H18 120.7 . . ?
C19 C18 H18 120.7 . . ?
N8 C19 C18 121.20(14) . . ?
N8 C19 C20 113.23(12) . . ?
C18 C19 C20 125.56(14) . . ?
N9 C20 C21 110.58(13) . . ?
N9 C20 C19 116.75(13) . . ?
C21 C20 C19 132.66(14) . . ?
C22 C21 C20 104.79(14) . . ?
C22 C21 H21 127.6 . . ?
C20 C21 H21 127.6 . . ?
N10 C22 C21 107.85(14) . . ?
N10 C22 H22 126.1 . . ?
C21 C22 H22 126.1 . . ?
O3 N11 C27 119.93(15) . . ?
O3 N11 C28 119.61(15) . . ?
C27 N11 C28 120.46(14) . . ?
C23 O1 H1O 115.3(11) . . ?
O2 C23 O1 126.54(15) . . ?
O2 C23 C24 119.52(15) . . ?
O1 C23 C24 113.91(15) . . ?
C26 C24 C25 118.27(15) . . ?
C26 C24 C23 120.30(15) . . ?
C25 C24 C23 121.27(15) . . ?
C28 C25 C24 120.12(16) . . ?
C28 C25 H25 119.9 . . ?
C24 C25 H25 119.9 . . ?
C27 C26 C24 120.27(16) . . ?
C27 C26 H26 119.9 . . ?
C24 C26 H26 119.9 . . ?
N11 C27 C26 120.35(16) . . ?
N11 C27 H27 119.8 . . ?
C26 C27 H27 119.8 . . ?
N11 C28 C25 120.41(15) . . ?
N11 C28 H28 119.8 . . ?
C25 C28 H28 119.8 . . ?
O6 N12 C33 120.52(13) . . ?
O6 N12 C34 119.75(13) . . ?
C33 N12 C34 119.73(13) . . ?
C29 O5 H1O 115.2(12) . . ?
O4 C29 O5 126.50(16) . . ?
O4 C29 C30 120.48(15) . . ?
O5 C29 C30 113.02(14) . . ?
C31 C30 C32 117.97(15) . . ?
C31 C30 C29 121.29(14) . . ?
C32 C30 C29 120.74(14) . . ?
C34 C31 C30 120.36(15) . . ?
C34 C31 H31 119.8 . . ?
C30 C31 H31 119.8 . . ?
C33 C32 C30 120.64(15) . . ?
C33 C32 H32 119.7 . . ?
C30 C32 H32 119.7 . . ?
N12 C33 C32 120.57(14) . . ?
N12 C33 H33 119.7 . . ?
C32 C33 H33 119.7 . . ?
N12 C34 C31 120.73(15) . . ?
N12 C34 H34 119.6 . . ?
C31 C34 H34 119.6 . . ?
O9 N13 C39 119.58(13) . . ?
O9 N13 C40 120.24(13) . . ?
C39 N13 C40 120.17(14) . . ?
O7 C35 O8 125.04(15) . . ?
O7 C35 C36 118.41(14) . . ?
O8 C35 C36 116.55(14) . . ?
C38 C36 C37 117.20(14) . . ?
C38 C36 C35 121.16(14) . . ?
C37 C36 C35 121.64(14) . . ?
C40 C37 C36 121.08(15) . . ?
C40 C37 H37 119.5 . . ?
C36 C37 H37 119.5 . . ?
C39 C38 C36 120.47(15) . . ?
C39 C38 H38 119.8 . . ?
C36 C38 H38 119.8 . . ?
N13 C39 C38 120.88(15) . . ?
N13 C39 H39 119.6 . . ?
C38 C39 H39 119.6 . . ?
N13 C40 C37 120.17(14) . . ?
N13 C40 H40 119.9 . . ?
C37 C40 H40 119.9 . . ?
H1A O1W H1B 106(2) . . ?
H2A O2W H2B 104(3) . . ?
H3A O3W H3B 110(3) . . ?
H4A O4W H4B 102(3) . . ?
H5A O5W H5B 104(3) . . ?

_refine_diff_density_max         0.244
_refine_diff_density_min         -0.462
_refine_diff_density_rms         0.068


_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_Fe_bpp_Noxid_NHoxid_Neutrons_50K_HSLS
_database_code_depnum_ccdc_archive 'CCDC 1984957'
loop_
_audit_author_name
_audit_author_address
'Veronica Jornet Molla'
;University of Valencia
Spain
;
_audit_update_record             
;
2020-02-21 deposited with the CCDC.	2020-11-23 downloaded from the CCDC.
;
# start Validation Reply Form
_vrf_PLAT029_Fe_bpp_Noxid_NHoxid_Neutrons_50K_HSLS 
;
PROBLEM: _diffrn_measured_fraction_theta_full value Low .      0.848 Why?
RESPONSE: The wavelength used for this experiment is 1.45470 \%A. Therefore, the number of collected reflections is low and this results in a low value of measured fraction theta full.
;
_vrf_PLAT088_Fe_bpp_Noxid_NHoxid_Neutrons_50K_HSLS 
;
PROBLEM: Poor Data / Parameter Ratio ....................       6.52 Note
RESPONSE: The wavelength used for this experiment is 1.45470 \%A. Therefore, the number of collected reflections is low and not enough to yield a data/parameter ratio of 10. In addition, there are 272 non-hydrogen atoms in the unit cell of this structure (68 in the asymmetric unit), which were refined anisotropically. Thus, the data/parameter ratio is low due to the large number of refined parameters and the wavelength used. 
;
_vrf_PLAT110_Fe_bpp_Noxid_NHoxid_Neutrons_50K_HSLS 
;
PROBLEM: ADDSYM Detects Potential Lattice Translation ...          ? Check
RESPONSE: The asymmetric unit contains two crystallographically independent Fe(II) complexes (and Z = 4) having clearly different Fe-N distances which correspond to two different spin states (high and low), as confirmed by magnetic susceptibility measurements. The alerts arise because the structure can also be solved with a smaller unit cell (with parameters very similar to the high temperature structure  solution) having half volume and only one Fe(II) complex (and Z = 2) with intermediate Fe-N distances between the corresponding high and low spin states. This solution also exhibits more elongated thermal ellipsoids in the N and C atoms of the ligands, suggesting that they can be split in two different positions corresponding to the high and low spin states. Therefore, the structure solution with Z = 4 has been adopted.
;
_vrf_PLAT112_Fe_bpp_Noxid_NHoxid_Neutrons_50K_HSLS 
;
PROBLEM: ADDSYM Detects New (Pseudo) Symm. Elem         B        100 %Fit
RESPONSE: The asymmetric unit contains two crystallographically independent Fe(II) complexes (and Z = 4) having clearly different Fe-N distances which correspond to two different spin states (high and low), as confirmed by magnetic susceptibility measurements. The alerts arise because the structure can also be solved with a smaller unit cell (with parameters very similar to the high temperature structure  solution) having half volume and only one Fe(II) complex (and Z = 2) with intermediate Fe-N distances between the corresponding high and low spin states. This solution also exhibits more elongated thermal ellipsoids in the N and C atoms of the ligands, suggesting that they can be split in two different positions corresponding to the high and low spin states. Therefore, the structure solution with Z = 4 has been adopted.
;
_vrf_PLAT113_Fe_bpp_Noxid_NHoxid_Neutrons_50K_HSLS 
;
PROBLEM: ADDSYM Suggests Possible Pseudo/New  Space Group        P-1 Check
RESPONSE: The asymmetric unit contains two crystallographically independent Fe(II) complexes (and Z = 4) having clearly different Fe-N distances which correspond to two different spin states (high and low), as confirmed by magnetic susceptibility measurements. The alerts arise because the structure can also be solved with a smaller unit cell (with parameters very similar to the high temperature structure  solution) having half volume and only one Fe(II) complex (and Z = 2) with intermediate Fe-N distances between the corresponding high and low spin states. This solution also exhibits more elongated thermal ellipsoids in the N and C atoms of the ligands, suggesting that they can be split in two different positions corresponding to the high and low spin states. Therefore, the structure solution with Z = 4 has been adopted.
;
_vrf_PLAT911_Fe_bpp_Noxid_NHoxid_Neutrons_50K_HSLS 
;
PROBLEM: Missing FCF Refl Between Thmin & STh/L=    0.599       2278 Report
RESPONSE: Some reflections are missing due to the restrictions of the experiment. The sample was placed on a close-circuit displex device on the monochromatic four-circle diffractometer D19 at ILL (Grenoble, France). The measurement strategy consisted on 25 omega (\w) scans with steps of 0.07\% at different \c and \f positions. These omega scans cover either 79\% or 64\% depending on the \c angle, in order to avoid collisions with the sample environment. Absorption correction removes reflections due to the environment provided by the neutron setup.
;
_vrf_PLAT303_Fe_bpp_Noxid_NHoxid_Neutrons_50K_HSLS 
;
PROBLEM: Full Occupancy Atom H1OB      with # Connections       2.00 Check
RESPONSE: This hydrogen atom is located between two oxygen atoms that belong to  different carboxylate groups, forming a very strong hydrogen bond (the distance  between the heteroatoms, O5B and O1A, is 2.420 \%A). As a proton-transfer  reaction is observed between the two carboxylate anions, different H...O distances  are observed at different temperatures. Such a type of proton-transfer reaction  is common when strong hydrogen bonds are established (see, for example Angew. Chem.  Int. Ed. 2002, 41, 48-76)
;
_vrf_PLAT303_Fe_bpp_Noxid_NHoxid_Neutrons_50K_HSLS_2 
;
PROBLEM: Full Occupancy Atom H1OA      with # Connections       2.00 Check
RESPONSE: This hydrogen atom is located between two oxygen atoms that belong to  different carboxylate groups, forming a very strong hydrogen bond (the distance  between the heteroatoms, O5A and O1B, is 2.414 \%A). As a proton-transfer reaction  is observed between the two carboxylate anions, different H?O distances are  observed at different temperatures. Such a type of proton-transfer reaction is  common when strong hydrogen bonds are established (see, for example Angew.  Chem. Int. Ed. 2002, 41, 48-76).
;
# Added during the CSD deposition process: Friday 21 February 2020 08:15 PM
# end Validation Reply Form


_audit_creation_method           SHELXL-2018/3
_shelx_SHELXL_version_number     2018/3
_chemical_name_systematic        ?
_chemical_name_common            ?
_chemical_melting_point          ?
_chemical_formula_moiety         
'C22 H18 Fe N10 2+, C12 H9 N2 O6 1-, C6 H4 N O3 1-, 5(H2 O)'
_chemical_formula_sum            'C40 H41 Fe N13 O14'
_chemical_formula_weight         983.71

loop_
_atom_type_symbol
_atom_type_description
_atom_type_scat_dispersion_real
_atom_type_scat_dispersion_imag
_atom_type_scat_source
C C 0.0000 0.0000
'Neutron Data Booklet, ILL Grenoble, France (2003) ISBN 0-9704143-7-4'
H H 0.0000 0.0000
'Neutron Data Booklet, ILL Grenoble, France (2003) ISBN 0-9704143-7-4'
N N 0.0000 0.0000
'Neutron Data Booklet, ILL Grenoble, France (2003) ISBN 0-9704143-7-4'
O O 0.0000 0.0000
'Neutron Data Booklet, ILL Grenoble, France (2003) ISBN 0-9704143-7-4'
Fe Fe 0.0000 0.0000
'Neutron Data Booklet, ILL Grenoble, France (2003) ISBN 0-9704143-7-4'

_space_group_crystal_system      triclinic
_space_group_IT_number           2
_space_group_name_H-M_alt        'P -1'
_space_group_name_Hall           '-P 1'

_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'

_cell_length_a                   13.5851(9)
_cell_length_b                   18.7551(9)
_cell_length_c                   19.6424(8)
_cell_angle_alpha                64.608(3)
_cell_angle_beta                 71.048(4)
_cell_angle_gamma                71.168(4)
_cell_volume                     4176.3(4)
_cell_formula_units_Z            4
_cell_measurement_temperature    50(1)
_cell_measurement_reflns_used    12837
_cell_measurement_theta_min      4.510
_cell_measurement_theta_max      60.871

_exptl_crystal_description       cube
_exptl_crystal_colour            dark-red
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    ?
_exptl_crystal_density_diffrn    1.564
_exptl_crystal_F_000             1300
_exptl_transmission_factor_min   ?
_exptl_transmission_factor_max   ?
_exptl_crystal_size_max          1.85
_exptl_crystal_size_mid          1.5
_exptl_crystal_size_min          0.7
_exptl_absorpt_coefficient_mu    0.193
_shelx_estimated_absorpt_T_min   ?
_shelx_estimated_absorpt_T_max   ?
_exptl_absorpt_correction_type   numerical
_exptl_absorpt_correction_T_min  ?
_exptl_absorpt_correction_T_max  ?
_exptl_absorpt_process_details   
; 
Absorption corretion done through d19face, d19abs and d19abscan 
programs from ILL
;
_diffrn_ambient_temperature      50(1)
_diffrn_radiation_wavelength     1.454696
_diffrn_radiation_type           neutrons
_diffrn_source                   'neutron source'
_diffrn_source_type              'ILL High Flux Reactor, beam H11'
_diffrn_source_power             57MW
_diffrn_measurement_device_type  
'D19 position-sensitive detector diffractometer'
_diffrn_radiation_monochromator  'copper 220'
_diffrn_measurement_method       'omega step-scans'
_diffrn_detector_area_resol_mean '1.56 mm vert. 2.5 mm hor.'
_diffrn_reflns_number            24974
_diffrn_reflns_av_unetI/netI     0.0286
_diffrn_reflns_av_R_equivalents  0.0435
_diffrn_reflns_limit_h_min       -16
_diffrn_reflns_limit_h_max       15
_diffrn_reflns_limit_k_min       -22
_diffrn_reflns_limit_k_max       22
_diffrn_reflns_limit_l_min       -18
_diffrn_reflns_limit_l_max       23
_diffrn_reflns_theta_min         4.511
_diffrn_reflns_theta_max         60.698
_diffrn_reflns_theta_full        60.698
_diffrn_measured_fraction_theta_max 0.848
_diffrn_measured_fraction_theta_full 0.848
_diffrn_reflns_Laue_measured_fraction_max 0.848
_diffrn_reflns_Laue_measured_fraction_full 0.848
_diffrn_reflns_point_group_measured_fraction_max 0.848
_diffrn_reflns_point_group_measured_fraction_full 0.848
_reflns_number_total             12802
_reflns_number_gt                11135
_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       'The NOMAD software from ILL'
_computing_cell_refinement       'PFIND and DIRAX programs'
_computing_data_reduction        'RETREAT and RAFD19 programs'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1997)'
_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)+(0.1406P)²+63.7625P] where P=(Fo²+2Fc²)/3'
_atom_sites_solution_primary     difmap
_atom_sites_solution_secondary   difmap
_atom_sites_solution_hydrogens   difmap
_refine_ls_hydrogen_treatment    refall
_refine_ls_extinction_method     none
_refine_ls_extinction_coef       .
_refine_ls_number_reflns         12802
_refine_ls_number_parameters     1963
_refine_ls_number_restraints     0
_refine_ls_R_factor_all          0.0854
_refine_ls_R_factor_gt           0.0759
_refine_ls_wR_factor_ref         0.2358
_refine_ls_wR_factor_gt          0.2188
_refine_ls_goodness_of_fit_ref   1.172
_refine_ls_restrained_S_all      1.172
_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
Fe1A Fe 0.88472(17) 0.73144(12) 0.34414(12) 0.0115(4) Uani 1 1 d . . . . .
N1A N 0.88762(18) 0.91314(14) 0.21600(13) 0.0171(5) Uani 1 1 d . . . . .
H1NA H 0.8752(6) 0.8976(4) 0.1741(4) 0.0277(14) Uani 1 1 d . . . . .
N2A N 0.89009(18) 0.85740(13) 0.28655(13) 0.0166(5) Uani 1 1 d . . . . .
N3A N 0.88935(18) 0.77007(13) 0.43079(13) 0.0143(5) Uani 1 1 d . . . . .
N4A N 0.87769(18) 0.62662(13) 0.45103(13) 0.0153(5) Uani 1 1 d . . . . .
N5A N 0.87307(18) 0.54923(13) 0.47448(14) 0.0183(5) Uani 1 1 d . . . . .
H5NA H 0.8772(6) 0.5235(4) 0.4368(4) 0.0302(15) Uani 1 1 d . . . . .
N6A N 0.62521(18) 0.81016(13) 0.37789(14) 0.0159(5) Uani 1 1 d . . . . .
H6NA H 0.6252(6) 0.8322(4) 0.4171(4) 0.0299(15) Uani 1 1 d . . . . .
N7A N 0.71254(18) 0.76113(13) 0.35328(13) 0.0157(5) Uani 1 1 d . . . . .
N8A N 0.86293(17) 0.67569(12) 0.27856(13) 0.0131(4) Uani 1 1 d . . . . .
N9A N 1.04509(18) 0.67730(12) 0.29432(13) 0.0139(5) Uani 1 1 d . . . . .
N10A N 1.14727(18) 0.67145(13) 0.29233(13) 0.0159(5) Uani 1 1 d . . . . .
H10N H 1.1637(5) 0.7045(4) 0.3171(4) 0.0263(14) Uani 1 1 d . . . . .
C1A C 0.8886(3) 0.98687(19) 0.2119(2) 0.0181(7) Uani 1 1 d . . . . .
H1A H 0.8860(7) 1.0371(4) 0.1595(5) 0.0368(17) Uani 1 1 d . . . . .
C2A C 0.8933(3) 0.97782(18) 0.28486(19) 0.0169(7) Uani 1 1 d . . . . .
H2A H 0.8944(6) 1.0245(4) 0.3029(5) 0.0340(16) Uani 1 1 d . . . . .
C3A C 0.8932(2) 0.89620(18) 0.32970(18) 0.0141(6) Uani 1 1 d . . . . .
C4A C 0.8897(2) 0.84782(18) 0.41203(18) 0.0132(6) Uani 1 1 d . . . . .
C5A C 0.8826(3) 0.8777(2) 0.46800(19) 0.0182(7) Uani 1 1 d . . . . .
H5A H 0.8813(6) 0.9397(4) 0.4518(4) 0.0312(15) Uani 1 1 d . . . . .
C6A C 0.8742(3) 0.8244(2) 0.5444(2) 0.0181(7) Uani 1 1 d . . . . .
H6A H 0.8675(6) 0.8455(4) 0.5896(4) 0.0323(16) Uani 1 1 d . . . . .
C7A C 0.8728(3) 0.7436(2) 0.5637(2) 0.0174(7) Uani 1 1 d . . . . .
H7A H 0.8672(6) 0.7012(4) 0.6225(4) 0.0334(16) Uani 1 1 d . . . . .
C8A C 0.8812(2) 0.71867(18) 0.50409(18) 0.0148(6) Uani 1 1 d . . . . .
C9A C 0.8788(2) 0.63715(18) 0.51442(18) 0.0153(6) Uani 1 1 d . . . . .
C10A C 0.8743(3) 0.56581(19) 0.5790(2) 0.0204(7) Uani 1 1 d . . . . .
H10A H 0.8763(7) 0.5544(5) 0.6369(4) 0.0377(17) Uani 1 1 d . . . . .
C11A C 0.8709(3) 0.5101(2) 0.5509(2) 0.0209(7) Uani 1 1 d . . . . .
H11A H 0.8697(7) 0.4474(4) 0.5781(5) 0.0385(17) Uani 1 1 d . . . . .
C12A C 0.5413(3) 0.81679(19) 0.35129(19) 0.0170(7) Uani 1 1 d . . . . .
H12A H 0.4648(6) 0.8538(4) 0.3641(5) 0.0347(16) Uani 1 1 d . . . . .
C13A C 0.5746(3) 0.76968(18) 0.30692(18) 0.0148(6) Uani 1 1 d . . . . .
H13A H 0.5255(6) 0.7606(4) 0.2776(4) 0.0314(15) Uani 1 1 d . . . . .
C14A C 0.6828(2) 0.73604(17) 0.30958(18) 0.0119(6) Uani 1 1 d . . . . .
C15A C 0.7639(2) 0.68178(18) 0.27419(18) 0.0128(6) Uani 1 1 d . . . . .
C16A C 0.7442(3) 0.63707(19) 0.24007(19) 0.0156(7) Uani 1 1 d . . . . .
H16A H 0.6619(5) 0.6407(4) 0.2387(4) 0.0300(15) Uani 1 1 d . . . . .
C17A C 0.8305(2) 0.58876(18) 0.20784(18) 0.0131(6) Uani 1 1 d . . . . .
H17A H 0.8194(6) 0.5534(4) 0.1804(4) 0.0299(15) Uani 1 1 d . . . . .
C18A C 0.9334(3) 0.58382(19) 0.21131(19) 0.0147(7) Uani 1 1 d . . . . .
H18A H 1.0016(6) 0.5477(5) 0.1853(4) 0.0307(15) Uani 1 1 d . . . . .
C19A C 0.9467(2) 0.62858(16) 0.24799(17) 0.0107(6) Uani 1 1 d . . . . .
C20A C 1.0484(2) 0.63115(18) 0.25631(18) 0.0139(6) Uani 1 1 d . . . . .
C21A C 1.1539(2) 0.5958(2) 0.23029(19) 0.0162(7) Uani 1 1 d . . . . .
H21A H 1.1818(6) 0.5570(4) 0.1966(5) 0.0340(16) Uani 1 1 d . . . . .
C22A C 1.2156(3) 0.62355(19) 0.25407(18) 0.0166(7) Uani 1 1 d . . . . .
H22A H 1.3010(6) 0.6116(5) 0.2468(4) 0.0316(15) Uani 1 1 d . . . . .
Fe1B Fe 0.62295(16) 0.27416(12) 0.15347(12) 0.0104(4) Uani 1 1 d . . . . .
N1B N 0.62120(18) 0.10563(13) 0.28629(13) 0.0144(5) Uani 1 1 d . . . . .
H1NB H 0.6361(6) 0.1230(4) 0.3258(4) 0.0277(15) Uani 1 1 d . . . . .
N2B N 0.61623(18) 0.15847(13) 0.21483(13) 0.0151(5) Uani 1 1 d . . . . .
N3B N 0.61443(17) 0.24004(13) 0.07579(13) 0.0134(5) Uani 1 1 d . . . . .
N4B N 0.62669(17) 0.37588(12) 0.06221(13) 0.0139(5) Uani 1 1 d . . . . .
N5B N 0.63087(18) 0.45193(13) 0.04554(14) 0.0170(5) Uani 1 1 d . . . . .
H5NB H 0.6292(6) 0.4739(4) 0.0861(4) 0.0312(15) Uani 1 1 d . . . . .
N6B N 0.86384(18) 0.19548(13) 0.11230(14) 0.0161(5) Uani 1 1 d . . . . .
H6NB H 0.8608(6) 0.1753(4) 0.0724(4) 0.0292(15) Uani 1 1 d . . . . .
N7B N 0.78057(18) 0.24314(12) 0.14270(13) 0.0144(5) Uani 1 1 d . . . . .
N8B N 0.63897(17) 0.31886(12) 0.22069(13) 0.0123(4) Uani 1 1 d . . . . .
N9B N 0.47028(17) 0.31819(12) 0.19556(13) 0.0135(5) Uani 1 1 d . . . . .
N10B N 0.37271(17) 0.31963(13) 0.19194(13) 0.0137(5) Uani 1 1 d . . . . .
H10M H 0.3607(5) 0.2849(4) 0.1658(4) 0.0277(14) Uani 1 1 d . . . . .
C1B C 0.6207(3) 0.0309(2) 0.29420(19) 0.0174(7) Uani 1 1 d . . . . .
H1B H 0.6241(6) -0.0173(4) 0.3479(4) 0.0350(16) Uani 1 1 d . . . . .
C2B C 0.6133(3) 0.03484(18) 0.22361(19) 0.0159(7) Uani 1 1 d . . . . .
H2B H 0.6119(6) -0.0147(4) 0.2096(4) 0.0321(15) Uani 1 1 d . . . . .
C3B C 0.6117(2) 0.11569(17) 0.17565(18) 0.0129(6) Uani 1 1 d . . . . .
C4B C 0.6120(2) 0.16222(18) 0.09409(18) 0.0136(6) Uani 1 1 d . . . . .
C5B C 0.6142(3) 0.1342(2) 0.03829(19) 0.0172(7) Uani 1 1 d . . . . .
H5B H 0.6133(6) 0.0728(5) 0.0536(4) 0.0331(16) Uani 1 1 d . . . . .
C6B C 0.6180(3) 0.18971(19) -0.03768(19) 0.0161(7) Uani 1 1 d . . . . .
H6B H 0.6201(6) 0.1698(4) -0.0830(4) 0.0307(15) Uani 1 1 d . . . . .
C7B C 0.6211(3) 0.26922(19) -0.05608(19) 0.0166(7) Uani 1 1 d . . . . .
H7B H 0.6236(7) 0.3135(5) -0.1145(4) 0.0357(17) Uani 1 1 d . . . . .
C8B C 0.6196(2) 0.29247(19) 0.00239(18) 0.0152(6) Uani 1 1 d . . . . .
C9B C 0.6249(2) 0.37125(17) -0.00399(18) 0.0144(6) Uani 1 1 d . . . . .
C10B C 0.6282(3) 0.4472(2) -0.0640(2) 0.0195(7) Uani 1 1 d . . . . .
H10B H 0.6273(6) 0.4648(4) -0.1238(4) 0.0333(16) Uani 1 1 d . . . . .
C11B C 0.6322(3) 0.4976(2) -0.02999(19) 0.0186(7) Uani 1 1 d . . . . .
H11B H 0.6354(7) 0.5591(4) -0.0509(4) 0.0374(17) Uani 1 1 d . . . . .
C12B C 0.9519(3) 0.18382(19) 0.13710(19) 0.0175(7) Uani 1 1 d . . . . .
H12B H 1.0263(6) 0.1485(4) 0.1198(5) 0.0345(16) Uani 1 1 d . . . . .
C13B C 0.9254(2) 0.22648(18) 0.18569(18) 0.0146(6) Uani 1 1 d . . . . .
H13B H 0.9783(6) 0.2305(4) 0.2146(4) 0.0314(15) Uani 1 1 d . . . . .
C14B C 0.8164(2) 0.26255(17) 0.18741(18) 0.0115(6) Uani 1 1 d . . . . .
C15B C 0.7372(2) 0.31357(17) 0.22646(18) 0.0126(6) Uani 1 1 d . . . . .
C16B C 0.7549(3) 0.35571(18) 0.26446(18) 0.0141(6) Uani 1 1 d . . . . .
H16B H 0.8349(6) 0.3524(4) 0.2654(4) 0.0323(16) Uani 1 1 d . . . . .
C17B C 0.6668(3) 0.40267(19) 0.29709(18) 0.0145(6) Uani 1 1 d . . . . .
H17B H 0.6762(6) 0.4359(4) 0.3263(4) 0.0307(15) Uani 1 1 d . . . . .
C18B C 0.5648(3) 0.40751(18) 0.29193(18) 0.0141(7) Uani 1 1 d . . . . .
H18B H 0.4947(6) 0.4432(4) 0.3177(4) 0.0295(15) Uani 1 1 d . . . . .
C19B C 0.5534(2) 0.36435(18) 0.25255(17) 0.0125(6) Uani 1 1 d . . . . .
C20B C 0.4565(2) 0.36168(17) 0.23922(18) 0.0136(6) Uani 1 1 d . . . . .
C21B C 0.3470(2) 0.3919(2) 0.26312(19) 0.0163(7) Uani 1 1 d . . . . .
H21B H 0.3114(6) 0.4272(5) 0.2996(5) 0.0350(16) Uani 1 1 d . . . . .
C22B C 0.2964(3) 0.36324(19) 0.23232(19) 0.0174(7) Uani 1 1 d . . . . .
H22B H 0.2131(6) 0.3698(5) 0.2354(5) 0.0374(17) Uani 1 1 d . . . . .
O1A O 0.0802(3) 0.6918(2) 1.0648(2) 0.0162(7) Uani 1 1 d . . . . .
O2A O -0.0875(3) 0.7583(2) 1.0507(2) 0.0169(8) Uani 1 1 d . . . . .
O3A O 0.0206(3) 0.5339(2) 0.8637(2) 0.0199(8) Uani 1 1 d . . . . .
N11A N 0.01359(18) 0.57123(13) 0.90889(13) 0.0155(5) Uani 1 1 d . . . . .
C23A C -0.0056(3) 0.70572(18) 1.04220(18) 0.0143(6) Uani 1 1 d . . . . .
C24A C -0.0004(2) 0.65374(18) 1.00028(18) 0.0139(6) Uani 1 1 d . . . . .
C25A C 0.0948(2) 0.60273(18) 0.97980(19) 0.0145(6) Uani 1 1 d . . . . .
H25A H 0.1650(5) 0.5952(5) 0.9997(4) 0.0314(15) Uani 1 1 d . . . . .
C26A C -0.0896(3) 0.66037(19) 0.97621(19) 0.0166(7) Uani 1 1 d . . . . .
H26A H -0.1642(6) 0.6990(4) 0.9912(5) 0.0331(16) Uani 1 1 d . . . . .
C27A C -0.0814(3) 0.61780(18) 0.93104(19) 0.0163(7) Uani 1 1 d . . . . .
H27A H -0.1475(6) 0.6198(5) 0.9104(4) 0.0331(16) Uani 1 1 d . . . . .
C28A C 0.1009(3) 0.56232(19) 0.93385(19) 0.0153(7) Uani 1 1 d . . . . .
H28A H 0.1723(6) 0.5230(4) 0.9139(4) 0.0309(15) Uani 1 1 d . . . . .
O4A O 0.3820(3) 0.1195(2) 0.5180(2) 0.0174(8) Uani 1 1 d . . . . .
O5A O 0.4142(3) 0.2089(2) 0.3962(2) 0.0200(8) Uani 1 1 d . . . . .
H1OA H 0.4229(6) 0.2545(4) 0.4203(4) 0.0299(15) Uani 1 1 d . . . . .
O6A O 0.3315(3) -0.0541(2) 0.3228(2) 0.0172(8) Uani 1 1 d . . . . .
N12A N 0.34494(17) -0.00747(13) 0.35145(13) 0.0139(5) Uani 1 1 d . . . . .
C29A C 0.3919(3) 0.14181(17) 0.44787(19) 0.0147(6) Uani 1 1 d . . . . .
C30A C 0.3758(2) 0.08897(17) 0.41438(18) 0.0131(6) Uani 1 1 d . . . . .
C31A C 0.3727(2) 0.00828(18) 0.45803(18) 0.0138(6) Uani 1 1 d . . . . .
H31A H 0.3821(7) -0.0194(4) 0.5171(4) 0.0336(16) Uani 1 1 d . . . . .
C32A C 0.3632(3) 0.11999(18) 0.33791(18) 0.0148(6) Uani 1 1 d . . . . .
H32A H 0.3651(6) 0.1827(4) 0.3025(4) 0.0313(16) Uani 1 1 d . . . . .
C33A C 0.3471(2) 0.07172(18) 0.30772(18) 0.0137(6) Uani 1 1 d . . . . .
H33A H 0.3344(6) 0.0917(4) 0.2496(4) 0.0305(15) Uani 1 1 d . . . . .
C34A C 0.3576(3) -0.03928(18) 0.42543(18) 0.0147(6) Uani 1 1 d . . . . .
H34A H 0.3554(6) -0.1026(4) 0.4562(4) 0.0293(15) Uani 1 1 d . . . . .
O7A O 0.1590(3) 0.6609(2) 0.4595(2) 0.0188(8) Uani 1 1 d . . . . .
O8A O 0.1833(3) 0.7666(2) 0.3500(2) 0.0176(8) Uani 1 1 d . . . . .
O9A O 0.1088(3) 0.9278(2) 0.5892(2) 0.0187(8) Uani 1 1 d . . . . .
N13A N 0.11701(18) 0.88323(13) 0.54995(13) 0.0151(5) Uani 1 1 d . . . . .
C35A C 0.1638(3) 0.73365(18) 0.42273(19) 0.0152(6) Uani 1 1 d . . . . .
C36A C 0.1457(2) 0.78681(18) 0.46782(18) 0.0142(6) Uani 1 1 d . . . . .
C37A C 0.1408(3) 0.86987(19) 0.4301(2) 0.0164(7) Uani 1 1 d . . . . .
H37A H 0.1503(6) 0.8973(4) 0.3684(5) 0.0345(16) Uani 1 1 d . . . . .
C38A C 0.1339(3) 0.75375(19) 0.54811(19) 0.0173(7) Uani 1 1 d . . . . .
H38A H 0.1374(6) 0.6895(4) 0.5805(4) 0.0327(16) Uani 1 1 d . . . . .
C39A C 0.1197(3) 0.80295(19) 0.5880(2) 0.0189(7) Uani 1 1 d . . . . .
H39A H 0.1120(7) 0.7830(4) 0.6490(5) 0.0356(17) Uani 1 1 d . . . . .
C40A C 0.1262(3) 0.91719(19) 0.47182(19) 0.0158(7) Uani 1 1 d . . . . .
H40A H 0.1211(6) 0.9808(4) 0.4464(4) 0.0331(16) Uani 1 1 d . . . . .
O1B O 0.4230(3) 0.3061(2) 0.4429(2) 0.0154(7) Uani 1 1 d . . . . .
O2B O 0.5897(3) 0.2411(2) 0.4600(2) 0.0176(8) Uani 1 1 d . . . . .
O3B O 0.4777(3) 0.4717(2) 0.6391(2) 0.0195(8) Uani 1 1 d . . . . .
N11B N 0.48532(18) 0.43321(13) 0.59521(13) 0.0152(5) Uani 1 1 d . . . . .
C23B C 0.5075(3) 0.29399(18) 0.46587(19) 0.0159(7) Uani 1 1 d . . . . .
C24B C 0.5008(2) 0.34737(18) 0.50628(19) 0.0145(6) Uani 1 1 d . . . . .
C25B C 0.4055(3) 0.39871(18) 0.52517(19) 0.0155(7) Uani 1 1 d . . . . .
H25B H 0.3362(5) 0.4048(4) 0.5060(5) 0.0328(16) Uani 1 1 d . . . . .
C26B C 0.5898(3) 0.34233(19) 0.5307(2) 0.0164(7) Uani 1 1 d . . . . .
H26B H 0.6645(6) 0.3033(4) 0.5163(4) 0.0300(15) Uani 1 1 d . . . . .
C27B C 0.5811(3) 0.38609(18) 0.57441(19) 0.0161(7) Uani 1 1 d . . . . .
H27B H 0.6454(6) 0.3861(5) 0.5956(5) 0.0347(16) Uani 1 1 d . . . . .
C28B C 0.3986(3) 0.44123(19) 0.56978(19) 0.0161(7) Uani 1 1 d . . . . .
H28B H 0.3265(6) 0.4805(4) 0.5890(4) 0.0315(15) Uani 1 1 d . . . . .
O4B O 0.1224(3) 0.8761(2) 0.9875(2) 0.0171(8) Uani 1 1 d . . . . .
O5B O 0.0969(3) 0.7879(2) 1.1100(2) 0.0187(8) Uani 1 1 d . . . . .
H1OB H 0.0849(6) 0.7418(4) 1.0867(4) 0.0321(16) Uani 1 1 d . . . . .
O6B O 0.1659(3) 1.0633(2) 1.1724(2) 0.0157(7) Uani 1 1 d . . . . .
N12B N 0.15726(17) 1.01331(13) 1.14568(13) 0.0140(5) Uani 1 1 d . . . . .
C29B C 0.1161(2) 0.85462(18) 1.05741(18) 0.0138(6) Uani 1 1 d . . . . .
C30B C 0.1312(2) 0.91085(17) 1.08775(18) 0.0129(6) Uani 1 1 d . . . . .
C31B C 0.1329(2) 0.99112(18) 1.04170(19) 0.0140(6) Uani 1 1 d . . . . .
H31B H 0.1215(7) 1.0156(4) 0.9824(4) 0.0337(16) Uani 1 1 d . . . . .
C32B C 0.1445(3) 0.88328(18) 1.16298(19) 0.0144(6) Uani 1 1 d . . . . .
H32B H 0.1452(7) 0.8209(4) 1.2012(4) 0.0323(16) Uani 1 1 d . . . . .
C33B C 0.1585(3) 0.93469(18) 1.19084(19) 0.0151(6) Uani 1 1 d . . . . .
H33B H 0.1713(6) 0.9173(4) 1.2479(4) 0.0318(16) Uani 1 1 d . . . . .
C34B C 0.1459(3) 1.04132(19) 1.07130(19) 0.0155(7) Uani 1 1 d . . . . .
H34B H 0.1461(6) 1.1039(4) 1.0390(4) 0.0288(15) Uani 1 1 d . . . . .
O7B O 0.3400(3) 0.3317(2) 1.0301(2) 0.0179(8) Uani 1 1 d . . . . .
O8B O 0.3306(3) 0.2242(2) 1.1397(2) 0.0172(8) Uani 1 1 d . . . . .
O9B O 0.3792(3) 0.0639(2) 0.9058(2) 0.0182(8) Uani 1 1 d . . . . .
N13B N 0.37435(18) 0.10844(13) 0.94392(13) 0.0158(5) Uani 1 1 d . . . . .
C35B C 0.3409(2) 0.25745(18) 1.06769(19) 0.0149(6) Uani 1 1 d . . . . .
C36B C 0.3547(2) 0.20503(18) 1.02388(19) 0.0146(6) Uani 1 1 d . . . . .
C37B C 0.3650(3) 0.12127(19) 1.0611(2) 0.0158(7) Uani 1 1 d . . . . .
H37B H 0.3635(7) 0.0927(4) 1.1215(4) 0.0343(16) Uani 1 1 d . . . . .
C38B C 0.3556(3) 0.23815(18) 0.94501(18) 0.0157(7) Uani 1 1 d . . . . .
H38B H 0.3472(7) 0.3028(4) 0.9135(4) 0.0343(17) Uani 1 1 d . . . . .
C39B C 0.3651(3) 0.18926(19) 0.9058(2) 0.0178(7) Uani 1 1 d . . . . .
H39B H 0.3643(7) 0.2099(4) 0.8457(4) 0.0368(17) Uani 1 1 d . . . . .
C40B C 0.3759(3) 0.07443(18) 1.01997(19) 0.0165(7) Uani 1 1 d . . . . .
H40B H 0.3845(6) 0.0090(4) 1.0461(4) 0.0317(15) Uani 1 1 d . . . . .
O1WA O 0.5879(4) 0.0738(2) 0.8184(3) 0.0195(8) Uani 1 1 d . . . . .
H1C H 0.6124(7) 0.0589(4) 0.7745(5) 0.0337(16) Uani 1 1 d . . . . .
H1D H 0.5152(7) 0.0681(4) 0.8394(5) 0.0302(15) Uani 1 1 d . . . . .
O1WB O 0.9048(4) 0.9198(2) 0.6828(3) 0.0192(8) Uani 1 1 d . . . . .
H1E H 0.8817(6) 0.9352(4) 0.7282(5) 0.0318(16) Uani 1 1 d . . . . .
H1F H 0.9762(8) 0.9246(4) 0.6597(5) 0.0295(15) Uani 1 1 d . . . . .
O2WA O 0.3760(4) 0.7716(2) 0.2329(3) 0.0166(8) Uani 1 1 d . . . . .
H2C H 0.3149(8) 0.7707(4) 0.2736(6) 0.0341(16) Uani 1 1 d . . . . .
H2D H 0.3887(6) 0.8263(5) 0.2117(5) 0.0329(16) Uani 1 1 d . . . . .
O2WB O 0.1336(4) 0.2338(2) 0.2575(3) 0.0199(8) Uani 1 1 d . . . . .
H2E H 0.1948(7) 0.2341(5) 0.2141(5) 0.0337(16) Uani 1 1 d . . . . .
H2F H 0.1203(6) 0.1797(4) 0.2795(4) 0.0281(14) Uani 1 1 d . . . . .
O3WA O 0.8282(4) 0.8638(3) 0.1285(3) 0.0217(8) Uani 1 1 d . . . . .
H3C H 0.7572(6) 0.8877(4) 0.1192(5) 0.0325(16) Uani 1 1 d . . . . .
H3D H 0.8620(6) 0.8249(4) 0.1032(4) 0.0287(14) Uani 1 1 d . . . . .
O3WB O 0.6845(4) 0.1428(3) 0.3790(2) 0.0204(8) Uani 1 1 d . . . . .
H3E H 0.6482(6) 0.1806(5) 0.4053(4) 0.0309(15) Uani 1 1 d . . . . .
H3F H 0.7558(7) 0.1193(4) 0.3867(5) 0.0328(16) Uani 1 1 d . . . . .
O4WA O 0.1358(4) 0.5442(2) 0.6023(3) 0.0196(8) Uani 1 1 d . . . . .
H4C H 0.1398(6) 0.5918(5) 0.5542(5) 0.0353(17) Uani 1 1 d . . . . .
H4D H 0.0862(7) 0.5631(5) 0.6424(6) 0.0392(18) Uani 1 1 d . . . . .
O4WB O 0.3612(4) 0.4496(3) 0.8869(3) 0.0229(9) Uani 1 1 d . . . . .
H4E H 0.3578(6) 0.4032(5) 0.9358(5) 0.0364(17) Uani 1 1 d . . . . .
H4F H 0.4139(7) 0.4291(5) 0.8488(5) 0.0339(16) Uani 1 1 d . . . . .
O5WA O 0.9976(3) 0.6252(3) 0.7150(3) 0.0224(8) Uani 1 1 d . . . . .
H5C H 0.9562(6) 0.6758(4) 0.7184(4) 0.0295(15) Uani 1 1 d . . . . .
H5D H 1.0057(6) 0.5935(5) 0.7669(5) 0.0336(16) Uani 1 1 d . . . . .
O5WB O 0.5128(3) 0.3774(3) 0.7821(3) 0.0215(8) Uani 1 1 d . . . . .
H5E H 0.5457(6) 0.3241(5) 0.7822(4) 0.0318(15) Uani 1 1 d . . . . .
H5F H 0.5027(6) 0.4097(5) 0.7300(5) 0.0332(16) Uani 1 1 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
Fe1A N8A 2.108(3) . ?
Fe1A N3A 2.141(3) . ?
Fe1A N2A 2.152(3) . ?
Fe1A N4A 2.176(3) . ?
Fe1A N9A 2.185(3) . ?
Fe1A N7A 2.188(3) . ?
N1A N2A 1.334(3) . ?
N1A C1A 1.354(4) . ?
N1A H1NA 1.057(7) . ?
N2A C3A 1.350(4) . ?
N3A C8A 1.338(4) . ?
N3A C4A 1.343(4) . ?
N4A N5A 1.338(3) . ?
N4A C9A 1.347(4) . ?
N5A C11A 1.354(4) . ?
N5A H5NA 1.023(8) . ?
N6A N7A 1.338(3) . ?
N6A C12A 1.352(4) . ?
N6A H6NA 1.019(8) . ?
N7A C14A 1.348(4) . ?
N8A C15A 1.341(4) . ?
N8A C19A 1.341(4) . ?
N9A N10A 1.345(3) . ?
N9A C20A 1.348(4) . ?
N10A C22A 1.349(4) . ?
N10A H10N 1.043(7) . ?
C1A C2A 1.390(5) . ?
C1A H1A 1.057(8) . ?
C2A C3A 1.401(4) . ?
C2A H2A 1.081(7) . ?
C3A C4A 1.470(4) . ?
C4A C5A 1.399(5) . ?
C5A C6A 1.393(5) . ?
C5A H5A 1.062(8) . ?
C6A C7A 1.400(5) . ?
C6A H6A 1.087(8) . ?
C7A C8A 1.398(5) . ?
C7A H7A 1.080(8) . ?
C8A C9A 1.464(4) . ?
C9A C10A 1.397(4) . ?
C10A C11A 1.394(5) . ?
C10A H10A 1.071(8) . ?
C11A H11A 1.066(8) . ?
C12A C13A 1.375(5) . ?
C12A H12A 1.067(9) . ?
C13A C14A 1.408(4) . ?
C13A H13A 1.102(7) . ?
C14A C15A 1.456(4) . ?
C15A C16A 1.402(4) . ?
C16A C17A 1.386(5) . ?
C16A H16A 1.107(7) . ?
C17A C18A 1.393(4) . ?
C17A H17A 1.084(7) . ?
C18A C19A 1.399(4) . ?
C18A H18A 1.079(8) . ?
C19A C20A 1.461(4) . ?
C20A C21A 1.399(5) . ?
C21A C22A 1.391(5) . ?
C21A H21A 1.088(8) . ?
C22A H22A 1.081(8) . ?
Fe1B N8B 1.936(3) . ?
Fe1B N3B 1.937(3) . ?
Fe1B N4B 1.981(3) . ?
Fe1B N7B 1.994(3) . ?
Fe1B N2B 1.996(3) . ?
Fe1B N9B 2.008(3) . ?
N1B N2B 1.335(3) . ?
N1B C1B 1.345(4) . ?
N1B H1NB 1.055(7) . ?
N2B C3B 1.353(4) . ?
N3B C8B 1.347(4) . ?
N3B C4B 1.354(4) . ?
N4B N5B 1.336(3) . ?
N4B C9B 1.348(4) . ?
N5B C11B 1.356(4) . ?
N5B H5NB 1.034(8) . ?
N6B N7B 1.342(3) . ?
N6B C12B 1.354(4) . ?
N6B H6NB 1.023(9) . ?
N7B C14B 1.344(4) . ?
N8B C15B 1.343(4) . ?
N8B C19B 1.348(4) . ?
N9B N10B 1.341(3) . ?
N9B C20B 1.354(4) . ?
N10B C22B 1.359(4) . ?
N10B H10M 1.060(7) . ?
C1B C2B 1.391(5) . ?
C1B H1B 1.057(8) . ?
C2B C3B 1.398(4) . ?
C2B H2B 1.082(7) . ?
C3B C4B 1.458(4) . ?
C4B C5B 1.394(4) . ?
C5B C6B 1.402(5) . ?
C5B H5B 1.060(9) . ?
C6B C7B 1.387(4) . ?
C6B H6B 1.093(7) . ?
C7B C8B 1.385(5) . ?
C7B H7B 1.088(8) . ?
C8B C9B 1.452(4) . ?
C9B C10B 1.410(4) . ?
C10B C11B 1.393(5) . ?
C10B H10B 1.078(8) . ?
C11B H11B 1.056(8) . ?
C12B C13B 1.388(5) . ?
C12B H12B 1.055(9) . ?
C13B C14B 1.411(4) . ?
C13B H13B 1.089(7) . ?
C14B C15B 1.446(4) . ?
C15B C16B 1.409(4) . ?
C16B C17B 1.387(5) . ?
C16B H16B 1.074(8) . ?
C17B C18B 1.393(4) . ?
C17B H17B 1.066(7) . ?
C18B C19B 1.405(4) . ?
C18B H18B 1.085(8) . ?
C19B C20B 1.443(4) . ?
C20B C21B 1.408(5) . ?
C21B C22B 1.384(5) . ?
C21B H21B 1.077(9) . ?
C22B H22B 1.082(7) . ?
O1A C23A 1.291(5) . ?
O1A H1OB 1.213(8) . ?
O2A C23A 1.246(5) . ?
O3A N11A 1.312(5) . ?
N11A C27A 1.361(4) . ?
N11A C28A 1.362(4) . ?
C23A C24A 1.496(4) . ?
C24A C26A 1.390(4) . ?
C24A C25A 1.394(5) . ?
C25A C28A 1.376(5) . ?
C25A H25A 1.091(7) . ?
C26A C27A 1.387(5) . ?
C26A H26A 1.074(8) . ?
C27A H27A 1.083(8) . ?
C28A H28A 1.085(8) . ?
O4A C29A 1.229(5) . ?
O5A C29A 1.288(5) . ?
O5A H1OA 1.191(8) . ?
O6A N12A 1.306(4) . ?
N12A C34A 1.360(4) . ?
N12A C33A 1.365(4) . ?
C29A C30A 1.502(4) . ?
C30A C31A 1.390(4) . ?
C30A C32A 1.406(4) . ?
C31A C34A 1.393(4) . ?
C31A H31A 1.081(8) . ?
C32A C33A 1.376(4) . ?
C32A H32A 1.083(7) . ?
C33A H33A 1.093(7) . ?
C34A H34A 1.082(6) . ?
O7A C35A 1.253(5) . ?
O8A C35A 1.263(5) . ?
O9A N13A 1.320(5) . ?
N13A C39A 1.358(4) . ?
N13A C40A 1.366(4) . ?
C35A C36A 1.516(4) . ?
C36A C37A 1.398(4) . ?
C36A C38A 1.399(5) . ?
C37A C40A 1.379(5) . ?
C37A H37A 1.076(9) . ?
C38A C39A 1.382(5) . ?
C38A H38A 1.089(7) . ?
C39A H39A 1.070(9) . ?
C40A H40A 1.066(7) . ?
O1B C23B 1.285(5) . ?
O1B H1OA 1.227(8) . ?
O2B C23B 1.243(5) . ?
O3B N11B 1.305(4) . ?
N11B C27B 1.365(4) . ?
N11B C28B 1.365(4) . ?
C23B C24B 1.489(4) . ?
C24B C25B 1.389(5) . ?
C24B C26B 1.401(4) . ?
C25B C28B 1.382(5) . ?
C25B H25B 1.080(7) . ?
C26B C27B 1.378(5) . ?
C26B H26B 1.076(7) . ?
C27B H27B 1.083(8) . ?
C28B H28B 1.084(8) . ?
O4B C29B 1.236(5) . ?
O5B C29B 1.276(5) . ?
O5B H1OB 1.209(8) . ?
O6B N12B 1.305(4) . ?
N12B C33B 1.354(4) . ?
N12B C34B 1.367(4) . ?
C29B C30B 1.506(4) . ?
C30B C31B 1.388(4) . ?
C30B C32B 1.394(4) . ?
C31B C34B 1.378(4) . ?
C31B H31B 1.097(8) . ?
C32B C33B 1.380(4) . ?
C32B H32B 1.085(6) . ?
C33B H33B 1.080(7) . ?
C34B H34B 1.069(7) . ?
O7B C35B 1.264(5) . ?
O8B C35B 1.258(5) . ?
O9B N13B 1.315(4) . ?
N13B C40B 1.354(4) . ?
N13B C39B 1.356(4) . ?
C35B C36B 1.498(4) . ?
C36B C38B 1.398(4) . ?
C36B C37B 1.400(4) . ?
C37B C40B 1.376(5) . ?
C37B H37B 1.069(8) . ?
C38B C39B 1.384(5) . ?
C38B H38B 1.086(6) . ?
C39B H39B 1.075(8) . ?
C40B H40B 1.091(6) . ?
O1WA H1C 0.947(13) . ?
O1WA H1D 0.960(12) . ?
O1WB H1E 0.978(11) . ?
O1WB H1F 0.943(13) . ?
O2WA H2C 0.945(15) . ?
O2WA H2D 0.978(9) . ?
O2WB H2E 0.978(14) . ?
O2WB H2F 0.969(9) . ?
O3WA H3C 0.964(9) . ?
O3WA H3D 0.968(10) . ?
O3WB H3E 0.967(11) . ?
O3WB H3F 0.957(11) . ?
O4WA H4C 0.983(10) . ?
O4WA H4D 0.971(14) . ?
O4WB H4E 0.981(11) . ?
O4WB H4F 0.970(13) . ?
O5WA H5C 0.952(10) . ?
O5WA H5D 0.957(10) . ?
O5WB H5E 0.953(10) . ?
O5WB H5F 0.970(11) . ?

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
N8A Fe1A N3A 167.93(14) . . ?
N8A Fe1A N2A 116.22(13) . . ?
N3A Fe1A N2A 74.31(11) . . ?
N8A Fe1A N4A 95.23(11) . . ?
N3A Fe1A N4A 73.94(11) . . ?
N2A Fe1A N4A 148.22(14) . . ?
N8A Fe1A N9A 74.62(11) . . ?
N3A Fe1A N9A 110.47(12) . . ?
N2A Fe1A N9A 100.01(12) . . ?
N4A Fe1A N9A 92.30(11) . . ?
N8A Fe1A N7A 75.06(11) . . ?
N3A Fe1A N7A 99.85(12) . . ?
N2A Fe1A N7A 90.65(11) . . ?
N4A Fe1A N7A 93.35(11) . . ?
N9A Fe1A N7A 149.54(13) . . ?
N2A N1A C1A 112.3(2) . . ?
N2A N1A H1NA 118.7(4) . . ?
C1A N1A H1NA 128.5(4) . . ?
N1A N2A C3A 105.8(2) . . ?
N1A N2A Fe1A 137.09(19) . . ?
C3A N2A Fe1A 117.09(19) . . ?
C8A N3A C4A 120.9(3) . . ?
C8A N3A Fe1A 119.53(19) . . ?
C4A N3A Fe1A 119.25(19) . . ?
N5A N4A C9A 105.6(2) . . ?
N5A N4A Fe1A 137.89(19) . . ?
C9A N4A Fe1A 116.53(19) . . ?
N4A N5A C11A 111.8(3) . . ?
N4A N5A H5NA 122.2(4) . . ?
C11A N5A H5NA 125.8(4) . . ?
N7A N6A C12A 111.7(2) . . ?
N7A N6A H6NA 120.2(5) . . ?
C12A N6A H6NA 127.6(5) . . ?
N6A N7A C14A 105.3(2) . . ?
N6A N7A Fe1A 139.19(18) . . ?
C14A N7A Fe1A 114.02(19) . . ?
C15A N8A C19A 120.8(2) . . ?
C15A N8A Fe1A 119.2(2) . . ?
C19A N8A Fe1A 119.70(18) . . ?
N10A N9A C20A 105.7(2) . . ?
N10A N9A Fe1A 139.52(18) . . ?
C20A N9A Fe1A 114.66(19) . . ?
N9A N10A C22A 112.0(2) . . ?
N9A N10A H10N 118.8(4) . . ?
C22A N10A H10N 129.1(5) . . ?
N1A C1A C2A 106.6(3) . . ?
N1A C1A H1A 120.6(5) . . ?
C2A C1A H1A 132.8(5) . . ?
C1A C2A C3A 105.0(3) . . ?
C1A C2A H2A 126.9(5) . . ?
C3A C2A H2A 128.0(5) . . ?
N2A C3A C2A 110.4(3) . . ?
N2A C3A C4A 116.0(3) . . ?
C2A C3A C4A 133.6(3) . . ?
N3A C4A C5A 121.4(3) . . ?
N3A C4A C3A 113.3(3) . . ?
C5A C4A C3A 125.3(3) . . ?
C6A C5A C4A 117.9(3) . . ?
C6A C5A H5A 122.1(5) . . ?
C4A C5A H5A 119.9(5) . . ?
C5A C6A C7A 120.4(3) . . ?
C5A C6A H6A 120.1(5) . . ?
C7A C6A H6A 119.5(5) . . ?
C8A C7A C6A 117.9(3) . . ?
C8A C7A H7A 120.6(5) . . ?
C6A C7A H7A 121.6(5) . . ?
N3A C8A C7A 121.5(3) . . ?
N3A C8A C9A 113.6(3) . . ?
C7A C8A C9A 124.9(3) . . ?
N4A C9A C10A 111.2(3) . . ?
N4A C9A C8A 116.2(3) . . ?
C10A C9A C8A 132.6(3) . . ?
C11A C10A C9A 104.3(3) . . ?
C11A C10A H10A 126.7(5) . . ?
C9A C10A H10A 128.9(5) . . ?
N5A C11A C10A 107.1(3) . . ?
N5A C11A H11A 121.0(5) . . ?
C10A C11A H11A 131.8(6) . . ?
N6A C12A C13A 107.8(3) . . ?
N6A C12A H12A 122.9(5) . . ?
C13A C12A H12A 129.3(5) . . ?
C12A C13A C14A 104.2(3) . . ?
C12A C13A H13A 126.5(5) . . ?
C14A C13A H13A 129.3(5) . . ?
N7A C14A C13A 110.9(3) . . ?
N7A C14A C15A 117.1(2) . . ?
C13A C14A C15A 132.0(3) . . ?
N8A C15A C16A 121.2(3) . . ?
N8A C15A C14A 113.6(3) . . ?
C16A C15A C14A 125.2(3) . . ?
C17A C16A C15A 118.2(3) . . ?
C17A C16A H16A 121.0(5) . . ?
C15A C16A H16A 120.7(5) . . ?
C16A C17A C18A 120.2(3) . . ?
C16A C17A H17A 121.0(5) . . ?
C18A C17A H17A 118.8(5) . . ?
C17A C18A C19A 118.3(3) . . ?
C17A C18A H18A 121.2(5) . . ?
C19A C18A H18A 120.5(5) . . ?
N8A C19A C18A 121.2(3) . . ?
N8A C19A C20A 113.2(2) . . ?
C18A C19A C20A 125.6(3) . . ?
N9A C20A C21A 110.3(3) . . ?
N9A C20A C19A 117.1(3) . . ?
C21A C20A C19A 132.5(3) . . ?
C22A C21A C20A 105.2(3) . . ?
C22A C21A H21A 127.4(5) . . ?
C20A C21A H21A 127.3(5) . . ?
N10A C22A C21A 106.7(3) . . ?
N10A C22A H22A 122.4(5) . . ?
C21A C22A H22A 130.9(5) . . ?
N8B Fe1B N3B 172.96(15) . . ?
N8B Fe1B N4B 94.15(12) . . ?
N3B Fe1B N4B 79.30(12) . . ?
N8B Fe1B N7B 79.02(12) . . ?
N3B Fe1B N7B 98.75(13) . . ?
N4B Fe1B N7B 94.19(12) . . ?
N8B Fe1B N2B 107.69(13) . . ?
N3B Fe1B N2B 78.83(11) . . ?
N4B Fe1B N2B 158.13(15) . . ?
N7B Fe1B N2B 88.99(12) . . ?
N8B Fe1B N9B 78.68(12) . . ?
N3B Fe1B N9B 103.72(12) . . ?
N4B Fe1B N9B 90.18(12) . . ?
N7B Fe1B N9B 157.52(14) . . ?
N2B Fe1B N9B 95.11(13) . . ?
N2B N1B C1B 111.9(2) . . ?
N2B N1B H1NB 119.7(4) . . ?
C1B N1B H1NB 127.7(4) . . ?
N1B N2B C3B 105.7(2) . . ?
N1B N2B Fe1B 138.15(18) . . ?
C3B N2B Fe1B 116.03(19) . . ?
C8B N3B C4B 120.4(2) . . ?
C8B N3B Fe1B 119.46(19) . . ?
C4B N3B Fe1B 120.0(2) . . ?
N5B N4B C9B 106.7(2) . . ?
N5B N4B Fe1B 138.0(2) . . ?
C9B N4B Fe1B 115.34(18) . . ?
N4B N5B C11B 111.9(3) . . ?
N4B N5B H5NB 123.8(5) . . ?
C11B N5B H5NB 124.2(5) . . ?
N7B N6B C12B 110.9(2) . . ?
N7B N6B H6NB 123.2(4) . . ?
C12B N6B H6NB 125.7(5) . . ?
N6B N7B C14B 106.4(2) . . ?
N6B N7B Fe1B 137.58(18) . . ?
C14B N7B Fe1B 114.9(2) . . ?
C15B N8B C19B 120.4(2) . . ?
C15B N8B Fe1B 119.4(2) . . ?
C19B N8B Fe1B 119.57(19) . . ?
N10B N9B C20B 106.7(2) . . ?
N10B N9B Fe1B 138.50(18) . . ?
C20B N9B Fe1B 114.81(19) . . ?
N9B N10B C22B 110.8(2) . . ?
N9B N10B H10M 121.9(4) . . ?
C22B N10B H10M 126.9(4) . . ?
N1B C1B C2B 107.5(3) . . ?
N1B C1B H1B 120.3(5) . . ?
C2B C1B H1B 132.2(5) . . ?
C1B C2B C3B 104.3(3) . . ?
C1B C2B H2B 126.9(5) . . ?
C3B C2B H2B 128.8(5) . . ?
N2B C3B C2B 110.6(3) . . ?
N2B C3B C4B 114.2(2) . . ?
C2B C3B C4B 135.1(3) . . ?
N3B C4B C5B 121.4(3) . . ?
N3B C4B C3B 110.9(3) . . ?
C5B C4B C3B 127.6(3) . . ?
C4B C5B C6B 117.6(3) . . ?
C4B C5B H5B 120.3(5) . . ?
C6B C5B H5B 122.1(5) . . ?
C7B C6B C5B 120.6(3) . . ?
C7B C6B H6B 119.7(5) . . ?
C5B C6B H6B 119.6(5) . . ?
C8B C7B C6B 118.5(3) . . ?
C8B C7B H7B 119.5(5) . . ?
C6B C7B H7B 122.0(5) . . ?
N3B C8B C7B 121.5(3) . . ?
N3B C8B C9B 110.7(3) . . ?
C7B C8B C9B 127.8(3) . . ?
N4B C9B C10B 109.6(3) . . ?
N4B C9B C8B 115.1(3) . . ?
C10B C9B C8B 135.4(3) . . ?
C11B C10B C9B 105.3(3) . . ?
C11B C10B H10B 125.7(5) . . ?
C9B C10B H10B 129.0(5) . . ?
N5B C11B C10B 106.6(3) . . ?
N5B C11B H11B 119.6(5) . . ?
C10B C11B H11B 133.8(6) . . ?
N6B C12B C13B 108.1(3) . . ?
N6B C12B H12B 123.3(5) . . ?
C13B C12B H12B 128.6(5) . . ?
C12B C13B C14B 103.9(3) . . ?
C12B C13B H13B 126.7(5) . . ?
C14B C13B H13B 129.3(5) . . ?
N7B C14B C13B 110.6(3) . . ?
N7B C14B C15B 114.8(2) . . ?
C13B C14B C15B 134.5(3) . . ?
N8B C15B C16B 121.9(3) . . ?
N8B C15B C14B 110.8(2) . . ?
C16B C15B C14B 127.3(3) . . ?
C17B C16B C15B 117.7(3) . . ?
C17B C16B H16B 122.6(5) . . ?
C15B C16B H16B 119.7(5) . . ?
C16B C17B C18B 120.5(3) . . ?
C16B C17B H17B 120.5(5) . . ?
C18B C17B H17B 119.0(5) . . ?
C17B C18B C19B 118.6(3) . . ?
C17B C18B H18B 121.8(5) . . ?
C19B C18B H18B 119.7(5) . . ?
N8B C19B C18B 120.9(3) . . ?
N8B C19B C20B 111.2(3) . . ?
C18B C19B C20B 127.9(3) . . ?
N9B C20B C21B 109.9(3) . . ?
N9B C20B C19B 114.9(3) . . ?
C21B C20B C19B 135.2(3) . . ?
C22B C21B C20B 104.8(3) . . ?
C22B C21B H21B 128.1(5) . . ?
C20B C21B H21B 127.0(5) . . ?
N10B C22B C21B 107.8(3) . . ?
N10B C22B H22B 119.9(5) . . ?
C21B C22B H22B 132.3(6) . . ?
C23A O1A H1OB 115.4(5) . . ?
O3A N11A C27A 119.5(3) . . ?
O3A N11A C28A 119.8(3) . . ?
C27A N11A C28A 120.7(3) . . ?
O2A C23A O1A 126.0(3) . . ?
O2A C23A C24A 119.7(3) . . ?
O1A C23A C24A 114.3(3) . . ?
C26A C24A C25A 119.0(3) . . ?
C26A C24A C23A 119.8(3) . . ?
C25A C24A C23A 121.1(3) . . ?
C28A C25A C24A 120.2(3) . . ?
C28A C25A H25A 119.8(5) . . ?
C24A C25A H25A 120.0(5) . . ?
C27A C26A C24A 119.5(3) . . ?
C27A C26A H26A 119.7(5) . . ?
C24A C26A H26A 120.8(5) . . ?
N11A C27A C26A 120.5(3) . . ?
N11A C27A H27A 116.0(5) . . ?
C26A C27A H27A 123.5(5) . . ?
N11A C28A C25A 120.1(3) . . ?
N11A C28A H28A 114.9(5) . . ?
C25A C28A H28A 125.0(5) . . ?
C29A O5A H1OA 115.2(5) . . ?
O6A N12A C34A 118.9(3) . . ?
O6A N12A C33A 120.6(3) . . ?
C34A N12A C33A 120.5(2) . . ?
O4A C29A O5A 127.2(3) . . ?
O4A C29A C30A 120.1(3) . . ?
O5A C29A C30A 112.7(3) . . ?
C31A C30A C32A 118.2(3) . . ?
C31A C30A C29A 121.0(3) . . ?
C32A C30A C29A 120.7(3) . . ?
C30A C31A C34A 119.8(3) . . ?
C30A C31A H31A 121.9(5) . . ?
C34A C31A H31A 118.3(5) . . ?
C33A C32A C30A 120.6(3) . . ?
C33A C32A H32A 119.5(5) . . ?
C30A C32A H32A 119.9(5) . . ?
N12A C33A C32A 120.2(3) . . ?
N12A C33A H33A 114.8(5) . . ?
C32A C33A H33A 125.0(5) . . ?
N12A C34A C31A 120.7(3) . . ?
N12A C34A H34A 116.1(5) . . ?
C31A C34A H34A 123.2(5) . . ?
O9A N13A C39A 119.0(3) . . ?
O9A N13A C40A 120.2(3) . . ?
C39A N13A C40A 120.7(3) . . ?
O7A C35A O8A 124.7(3) . . ?
O7A C35A C36A 118.4(3) . . ?
O8A C35A C36A 116.9(3) . . ?
C37A C36A C38A 118.6(3) . . ?
C37A C36A C35A 120.7(3) . . ?
C38A C36A C35A 120.7(3) . . ?
C40A C37A C36A 120.0(3) . . ?
C40A C37A H37A 119.4(5) . . ?
C36A C37A H37A 120.6(5) . . ?
C39A C38A C36A 119.8(3) . . ?
C39A C38A H38A 118.4(5) . . ?
C36A C38A H38A 121.8(5) . . ?
N13A C39A C38A 120.6(3) . . ?
N13A C39A H39A 114.2(5) . . ?
C38A C39A H39A 125.2(5) . . ?
N13A C40A C37A 120.3(3) . . ?
N13A C40A H40A 116.2(5) . . ?
C37A C40A H40A 123.5(5) . . ?
C23B O1B H1OA 114.4(5) . . ?
O3B N11B C27B 119.2(3) . . ?
O3B N11B C28B 120.0(3) . . ?
C27B N11B C28B 120.8(3) . . ?
O2B C23B O1B 126.3(3) . . ?
O2B C23B C24B 118.9(3) . . ?
O1B C23B C24B 114.8(3) . . ?
C25B C24B C26B 118.7(3) . . ?
C25B C24B C23B 121.2(3) . . ?
C26B C24B C23B 119.9(3) . . ?
C28B C25B C24B 120.0(3) . . ?
C28B C25B H25B 119.7(5) . . ?
C24B C25B H25B 120.3(5) . . ?
C27B C26B C24B 120.1(3) . . ?
C27B C26B H26B 120.0(5) . . ?
C24B C26B H26B 119.9(5) . . ?
N11B C27B C26B 120.1(3) . . ?
N11B C27B H27B 114.8(5) . . ?
C26B C27B H27B 125.1(5) . . ?
N11B C28B C25B 120.2(3) . . ?
N11B C28B H28B 115.2(5) . . ?
C25B C28B H28B 124.5(5) . . ?
C29B O5B H1OB 114.4(5) . . ?
O6B N12B C33B 120.8(3) . . ?
O6B N12B C34B 119.2(3) . . ?
C33B N12B C34B 120.0(2) . . ?
O4B C29B O5B 127.2(3) . . ?
O4B C29B C30B 119.4(3) . . ?
O5B C29B C30B 113.4(3) . . ?
C31B C30B C32B 118.2(3) . . ?
C31B C30B C29B 121.1(3) . . ?
C32B C30B C29B 120.6(3) . . ?
C34B C31B C30B 119.8(3) . . ?
C34B C31B H31B 119.5(5) . . ?
C30B C31B H31B 120.6(5) . . ?
C33B C32B C30B 120.7(3) . . ?
C33B C32B H32B 117.9(5) . . ?
C30B C32B H32B 121.3(5) . . ?
N12B C33B C32B 120.2(3) . . ?
N12B C33B H33B 114.9(5) . . ?
C32B C33B H33B 124.9(5) . . ?
N12B C34B C31B 121.0(3) . . ?
N12B C34B H34B 115.8(5) . . ?
C31B C34B H34B 123.2(5) . . ?
O9B N13B C40B 120.6(3) . . ?
O9B N13B C39B 118.5(3) . . ?
C40B N13B C39B 120.9(3) . . ?
O8B C35B O7B 124.6(3) . . ?
O8B C35B C36B 117.3(3) . . ?
O7B C35B C36B 118.1(3) . . ?
C38B C36B C37B 117.9(3) . . ?
C38B C36B C35B 121.2(3) . . ?
C37B C36B C35B 120.9(3) . . ?
C40B C37B C36B 119.9(3) . . ?
C40B C37B H37B 118.9(5) . . ?
C36B C37B H37B 121.1(5) . . ?
C39B C38B C36B 120.6(3) . . ?
C39B C38B H38B 118.7(5) . . ?
C36B C38B H38B 120.7(5) . . ?
N13B C39B C38B 119.8(3) . . ?
N13B C39B H39B 114.7(5) . . ?
C38B C39B H39B 125.4(5) . . ?
N13B C40B C37B 120.9(3) . . ?
N13B C40B H40B 116.3(5) . . ?
C37B C40B H40B 122.8(5) . . ?
H1C O1WA H1D 107.0(8) . . ?
H1E O1WB H1F 108.8(7) . . ?
H2C O2WA H2D 106.3(8) . . ?
H2E O2WB H2F 105.8(8) . . ?
H3C O3WA H3D 108.4(7) . . ?
H3E O3WB H3F 111.1(7) . . ?
H4C O4WA H4D 106.5(8) . . ?
H4E O4WB H4F 105.8(8) . . ?
H5C O5WA H5D 102.8(8) . . ?
H5E O5WB H5F 105.4(8) . . ?

loop_
_geom_torsion_atom_site_label_1
_geom_torsion_atom_site_label_2
_geom_torsion_atom_site_label_3
_geom_torsion_atom_site_label_4
_geom_torsion
_geom_torsion_site_symmetry_1
_geom_torsion_site_symmetry_2
_geom_torsion_site_symmetry_3
_geom_torsion_site_symmetry_4
_geom_torsion_publ_flag
C1A N1A N2A C3A -0.3(3) . . . . ?
C1A N1A N2A Fe1A 177.0(2) . . . . ?
C9A N4A N5A C11A 0.1(3) . . . . ?
Fe1A N4A N5A C11A 179.5(2) . . . . ?
C12A N6A N7A C14A 0.1(3) . . . . ?
C12A N6A N7A Fe1A 164.4(2) . . . . ?
C20A N9A N10A C22A 0.3(3) . . . . ?
Fe1A N9A N10A C22A 176.0(2) . . . . ?
N2A N1A C1A C2A 0.7(3) . . . . ?
N1A C1A C2A C3A -0.9(3) . . . . ?
N1A N2A C3A C2A -0.3(3) . . . . ?
Fe1A N2A C3A C2A -178.2(2) . . . . ?
N1A N2A C3A C4A 176.3(2) . . . . ?
Fe1A N2A C3A C4A -1.6(3) . . . . ?
C1A C2A C3A N2A 0.7(4) . . . . ?
C1A C2A C3A C4A -175.1(3) . . . . ?
C8A N3A C4A C5A 0.6(4) . . . . ?
Fe1A N3A C4A C5A 173.9(2) . . . . ?
C8A N3A C4A C3A -176.8(3) . . . . ?
Fe1A N3A C4A C3A -3.5(3) . . . . ?
N2A C3A C4A N3A 3.3(4) . . . . ?
C2A C3A C4A N3A 178.9(3) . . . . ?
N2A C3A C4A C5A -174.1(3) . . . . ?
C2A C3A C4A C5A 1.6(6) . . . . ?
N3A C4A C5A C6A -0.5(5) . . . . ?
C3A C4A C5A C6A 176.6(3) . . . . ?
C4A C5A C6A C7A -0.1(5) . . . . ?
C5A C6A C7A C8A 0.7(5) . . . . ?
C4A N3A C8A C7A 0.0(4) . . . . ?
Fe1A N3A C8A C7A -173.3(2) . . . . ?
C4A N3A C8A C9A 178.2(3) . . . . ?
Fe1A N3A C8A C9A 4.9(3) . . . . ?
C6A C7A C8A N3A -0.6(5) . . . . ?
C6A C7A C8A C9A -178.6(3) . . . . ?
N5A N4A C9A C10A -0.3(3) . . . . ?
Fe1A N4A C9A C10A -179.8(2) . . . . ?
N5A N4A C9A C8A -178.6(2) . . . . ?
Fe1A N4A C9A C8A 1.8(3) . . . . ?
N3A C8A C9A N4A -4.3(4) . . . . ?
C7A C8A C9A N4A 173.8(3) . . . . ?
N3A C8A C9A C10A 177.8(3) . . . . ?
C7A C8A C9A C10A -4.0(6) . . . . ?
N4A C9A C10A C11A 0.3(4) . . . . ?
C8A C9A C10A C11A 178.3(3) . . . . ?
N4A N5A C11A C10A 0.1(3) . . . . ?
C9A C10A C11A N5A -0.3(3) . . . . ?
N7A N6A C12A C13A 0.1(3) . . . . ?
N6A C12A C13A C14A -0.2(3) . . . . ?
N6A N7A C14A C13A -0.2(3) . . . . ?
Fe1A N7A C14A C13A -169.1(2) . . . . ?
N6A N7A C14A C15A 179.3(2) . . . . ?
Fe1A N7A C14A C15A 10.5(3) . . . . ?
C12A C13A C14A N7A 0.3(3) . . . . ?
C12A C13A C14A C15A -179.2(3) . . . . ?
C19A N8A C15A C16A 2.3(4) . . . . ?
Fe1A N8A C15A C16A -171.4(2) . . . . ?
C19A N8A C15A C14A -179.4(3) . . . . ?
Fe1A N8A C15A C14A 6.9(3) . . . . ?
N7A C14A C15A N8A -11.6(4) . . . . ?
C13A C14A C15A N8A 167.9(3) . . . . ?
N7A C14A C15A C16A 166.7(3) . . . . ?
C13A C14A C15A C16A -13.8(5) . . . . ?
N8A C15A C16A C17A -2.7(5) . . . . ?
C14A C15A C16A C17A 179.2(3) . . . . ?
C15A C16A C17A C18A 1.5(5) . . . . ?
C16A C17A C18A C19A 0.1(5) . . . . ?
C15A N8A C19A C18A -0.6(4) . . . . ?
Fe1A N8A C19A C18A 173.1(2) . . . . ?
C15A N8A C19A C20A 178.4(2) . . . . ?
Fe1A N8A C19A C20A -8.0(3) . . . . ?
C17A C18A C19A N8A -0.6(4) . . . . ?
C17A C18A C19A C20A -179.4(3) . . . . ?
N10A N9A C20A C21A 0.1(3) . . . . ?
Fe1A N9A C20A C21A -176.8(2) . . . . ?
N10A N9A C20A C19A -178.3(2) . . . . ?
Fe1A N9A C20A C19A 4.8(3) . . . . ?
N8A C19A C20A N9A 1.7(4) . . . . ?
C18A C19A C20A N9A -179.3(3) . . . . ?
N8A C19A C20A C21A -176.3(3) . . . . ?
C18A C19A C20A C21A 2.7(5) . . . . ?
N9A C20A C21A C22A -0.5(4) . . . . ?
C19A C20A C21A C22A 177.6(3) . . . . ?
N9A N10A C22A C21A -0.6(3) . . . . ?
C20A C21A C22A N10A 0.6(3) . . . . ?
C1B N1B N2B C3B 0.4(3) . . . . ?
C1B N1B N2B Fe1B -174.7(2) . . . . ?
C9B N4B N5B C11B -0.1(3) . . . . ?
Fe1B N4B N5B C11B 179.7(2) . . . . ?
C12B N6B N7B C14B 0.3(3) . . . . ?
C12B N6B N7B Fe1B -166.3(2) . . . . ?
C20B N9B N10B C22B 0.1(3) . . . . ?
Fe1B N9B N10B C22B -177.7(2) . . . . ?
N2B N1B C1B C2B -0.9(3) . . . . ?
N1B C1B C2B C3B 1.1(3) . . . . ?
N1B N2B C3B C2B 0.4(3) . . . . ?
Fe1B N2B C3B C2B 176.7(2) . . . . ?
N1B N2B C3B C4B -176.7(2) . . . . ?
Fe1B N2B C3B C4B -0.3(3) . . . . ?
C1B C2B C3B N2B -0.9(3) . . . . ?
C1B C2B C3B C4B 175.3(3) . . . . ?
C8B N3B C4B C5B -0.3(4) . . . . ?
Fe1B N3B C4B C5B -175.0(2) . . . . ?
C8B N3B C4B C3B 177.2(2) . . . . ?
Fe1B N3B C4B C3B 2.5(3) . . . . ?
N2B C3B C4B N3B -1.3(4) . . . . ?
C2B C3B C4B N3B -177.4(3) . . . . ?
N2B C3B C4B C5B 176.0(3) . . . . ?
C2B C3B C4B C5B -0.1(6) . . . . ?
N3B C4B C5B C6B -0.6(4) . . . . ?
C3B C4B C5B C6B -177.7(3) . . . . ?
C4B C5B C6B C7B 1.0(5) . . . . ?
C5B C6B C7B C8B -0.5(5) . . . . ?
C4B N3B C8B C7B 0.9(4) . . . . ?
Fe1B N3B C8B C7B 175.6(2) . . . . ?
C4B N3B C8B C9B -178.1(3) . . . . ?
Fe1B N3B C8B C9B -3.4(3) . . . . ?
C6B C7B C8B N3B -0.5(5) . . . . ?
C6B C7B C8B C9B 178.3(3) . . . . ?
N5B N4B C9B C10B 0.0(3) . . . . ?
Fe1B N4B C9B C10B -179.9(2) . . . . ?
N5B N4B C9B C8B -179.6(2) . . . . ?
Fe1B N4B C9B C8B 0.6(3) . . . . ?
N3B C8B C9B N4B 1.7(4) . . . . ?
C7B C8B C9B N4B -177.2(3) . . . . ?
N3B C8B C9B C10B -177.7(3) . . . . ?
C7B C8B C9B C10B 3.4(6) . . . . ?
N4B C9B C10B C11B 0.1(3) . . . . ?
C8B C9B C10B C11B 179.6(4) . . . . ?
N4B N5B C11B C10B 0.2(3) . . . . ?
C9B C10B C11B N5B -0.2(3) . . . . ?
N7B N6B C12B C13B -0.5(3) . . . . ?
N6B C12B C13B C14B 0.5(3) . . . . ?
N6B N7B C14B C13B 0.0(3) . . . . ?
Fe1B N7B C14B C13B 170.1(2) . . . . ?
N6B N7B C14B C15B -179.3(2) . . . . ?
Fe1B N7B C14B C15B -9.3(3) . . . . ?
C12B C13B C14B N7B -0.3(3) . . . . ?
C12B C13B C14B C15B 178.9(3) . . . . ?
C19B N8B C15B C16B -1.0(4) . . . . ?
Fe1B N8B C15B C16B 169.8(2) . . . . ?
C19B N8B C15B C14B -179.3(2) . . . . ?
Fe1B N8B C15B C14B -8.5(3) . . . . ?
N7B C14B C15B N8B 11.3(4) . . . . ?
C13B C14B C15B N8B -167.8(3) . . . . ?
N7B C14B C15B C16B -166.9(3) . . . . ?
C13B C14B C15B C16B 14.0(6) . . . . ?
N8B C15B C16B C17B 0.8(4) . . . . ?
C14B C15B C16B C17B 178.9(3) . . . . ?
C15B C16B C17B C18B -0.1(4) . . . . ?
C16B C17B C18B C19B -0.5(5) . . . . ?
C15B N8B C19B C18B 0.4(4) . . . . ?
Fe1B N8B C19B C18B -170.4(2) . . . . ?
C15B N8B C19B C20B 179.8(2) . . . . ?
Fe1B N8B C19B C20B 9.0(3) . . . . ?
C17B C18B C19B N8B 0.3(4) . . . . ?
C17B C18B C19B C20B -178.9(3) . . . . ?
N10B N9B C20B C21B -0.5(3) . . . . ?
Fe1B N9B C20B C21B 177.8(2) . . . . ?
N10B N9B C20B C19B 177.5(2) . . . . ?
Fe1B N9B C20B C19B -4.1(3) . . . . ?
N8B C19B C20B N9B -2.8(4) . . . . ?
C18B C19B C20B N9B 176.5(3) . . . . ?
N8B C19B C20B C21B 174.6(3) . . . . ?
C18B C19B C20B C21B -6.1(6) . . . . ?
N9B C20B C21B C22B 0.8(4) . . . . ?
C19B C20B C21B C22B -176.7(3) . . . . ?
N9B N10B C22B C21B 0.4(3) . . . . ?
C20B C21B C22B N10B -0.7(3) . . . . ?
O2A C23A C24A C26A -4.8(5) . . . . ?
O1A C23A C24A C26A 177.0(3) . . . . ?
O2A C23A C24A C25A 170.5(3) . . . . ?
O1A C23A C24A C25A -7.7(4) . . . . ?
C26A C24A C25A C28A 2.6(5) . . . . ?
C23A C24A C25A C28A -172.7(3) . . . . ?
C25A C24A C26A C27A -1.5(5) . . . . ?
C23A C24A C26A C27A 173.9(3) . . . . ?
O3A N11A C27A C26A -177.4(3) . . . . ?
C28A N11A C27A C26A 3.3(4) . . . . ?
C24A C26A C27A N11A -1.4(5) . . . . ?
O3A N11A C28A C25A 178.5(3) . . . . ?
C27A N11A C28A C25A -2.2(4) . . . . ?
C24A C25A C28A N11A -0.8(5) . . . . ?
O4A C29A C30A C31A -14.2(5) . . . . ?
O5A C29A C30A C31A 166.8(3) . . . . ?
O4A C29A C30A C32A 165.8(3) . . . . ?
O5A C29A C30A C32A -13.3(5) . . . . ?
C32A C30A C31A C34A 0.1(5) . . . . ?
C29A C30A C31A C34A 180.0(3) . . . . ?
C31A C30A C32A C33A 0.7(5) . . . . ?
C29A C30A C32A C33A -179.2(3) . . . . ?
O6A N12A C33A C32A -178.8(3) . . . . ?
C34A N12A C33A C32A 0.6(4) . . . . ?
C30A C32A C33A N12A -1.1(5) . . . . ?
O6A N12A C34A C31A 179.6(3) . . . . ?
C33A N12A C34A C31A 0.2(4) . . . . ?
C30A C31A C34A N12A -0.5(5) . . . . ?
O7A C35A C36A C37A -174.3(3) . . . . ?
O8A C35A C36A C37A 6.0(5) . . . . ?
O7A C35A C36A C38A 6.0(5) . . . . ?
O8A C35A C36A C38A -173.8(3) . . . . ?
C38A C36A C37A C40A 0.9(5) . . . . ?
C35A C36A C37A C40A -178.8(3) . . . . ?
C37A C36A C38A C39A -1.1(5) . . . . ?
C35A C36A C38A C39A 178.7(3) . . . . ?
O9A N13A C39A C38A -176.5(3) . . . . ?
C40A N13A C39A C38A 1.3(5) . . . . ?
C36A C38A C39A N13A 0.0(5) . . . . ?
O9A N13A C40A C37A 176.3(3) . . . . ?
C39A N13A C40A C37A -1.5(4) . . . . ?
C36A C37A C40A N13A 0.4(5) . . . . ?
O2B C23B C24B C25B -169.8(3) . . . . ?
O1B C23B C24B C25B 7.4(5) . . . . ?
O2B C23B C24B C26B 5.7(5) . . . . ?
O1B C23B C24B C26B -177.0(3) . . . . ?
C26B C24B C25B C28B -2.5(5) . . . . ?
C23B C24B C25B C28B 173.1(3) . . . . ?
C25B C24B C26B C27B 1.8(5) . . . . ?
C23B C24B C26B C27B -173.9(3) . . . . ?
O3B N11B C27B C26B 177.4(3) . . . . ?
C28B N11B C27B C26B -3.6(4) . . . . ?
C24B C26B C27B N11B 1.2(5) . . . . ?
O3B N11B C28B C25B -178.1(3) . . . . ?
C27B N11B C28B C25B 2.9(4) . . . . ?
C24B C25B C28B N11B 0.2(5) . . . . ?
O4B C29B C30B C31B 11.7(5) . . . . ?
O5B C29B C30B C31B -167.9(3) . . . . ?
O4B C29B C30B C32B -167.8(3) . . . . ?
O5B C29B C30B C32B 12.5(5) . . . . ?
C32B C30B C31B C34B -1.0(5) . . . . ?
C29B C30B C31B C34B 179.4(3) . . . . ?
C31B C30B C32B C33B 0.3(5) . . . . ?
C29B C30B C32B C33B 179.9(3) . . . . ?
O6B N12B C33B C32B 177.1(3) . . . . ?
C34B N12B C33B C32B -2.4(4) . . . . ?
C30B C32B C33B N12B 1.4(5) . . . . ?
O6B N12B C34B C31B -177.8(3) . . . . ?
C33B N12B C34B C31B 1.7(4) . . . . ?
C30B C31B C34B N12B 0.0(5) . . . . ?
O8B C35B C36B C38B 173.3(3) . . . . ?
O7B C35B C36B C38B -6.4(5) . . . . ?
O8B C35B C36B C37B -5.5(5) . . . . ?
O7B C35B C36B C37B 174.8(3) . . . . ?
C38B C36B C37B C40B 0.2(5) . . . . ?
C35B C36B C37B C40B 179.0(3) . . . . ?
C37B C36B C38B C39B 0.8(5) . . . . ?
C35B C36B C38B C39B -178.1(3) . . . . ?
O9B N13B C39B C38B 177.4(3) . . . . ?
C40B N13B C39B C38B -1.0(4) . . . . ?
C36B C38B C39B N13B -0.4(5) . . . . ?
O9B N13B C40B C37B -176.4(3) . . . . ?
C39B N13B C40B C37B 1.9(4) . . . . ?
C36B C37B C40B N13B -1.5(5) . . . . ?

_refine_diff_density_max         1.622
_refine_diff_density_min         -1.696
_refine_diff_density_rms         0.304


_exptl_crystal_recrystallization_method 
'Re-crystallisation from solvent: MeOH/H2O'
_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_Fe_bpp_Noxid_NHoxid_210K
_database_code_depnum_ccdc_archive 'CCDC 1873602'
loop_
_audit_author_name
_audit_author_address
'Ver?nica Jornet Moll?'
;Universitat de Val?ncia
Spain
;
_audit_update_record             
;
2018-10-29 deposited with the CCDC.	2020-11-23 downloaded from the CCDC.
;
# start Validation Reply Form
_vrf_PLAT303_Fe_bpp_Noxid_NHoxid_210K 
;
PROBLEM: Full Occupancy Atom H1O       with # Connections       2.00 Check
RESPONSE: This hydrogen atom is located between two oxygen atoms that belong to different carboxylate groups, forming a very strong hydrogen bond (the distance between the heteroatoms, O5 and O1, is 2.421 \%A). As a proton-transfer reaction is observed between the two carboxylate anions, different H?O distances are observed at different temperatures. Such a type of proton-transfer reaction is common when strong hydrogen bonds are established (see, for example Angew. Chem. Int. Ed. 2002, 41, 48-76).
;
# Added during the CSD deposition process: Monday 29 October 2018 04:44 PM
# end Validation Reply Form


_audit_creation_method           SHELXL-2017/1
_shelx_SHELXL_version_number     2017/1
_chemical_name_systematic        ?
_chemical_name_common            ?
_chemical_melting_point          ?
_chemical_formula_moiety         
'C22 H18 Fe N10 2+, C12 H9 N2 O6 1-, C6 H4 N O3 1-, 5(H2 O)'
_chemical_formula_sum            'C40 H41 Fe N13 O14'
_chemical_formula_weight         983.705

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      triclinic
_space_group_IT_number           2
_space_group_name_H-M_alt        'P -1'
_space_group_name_Hall           '-P 1'

_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'

_cell_length_a                   9.99242(16)
_cell_length_b                   13.64829(17)
_cell_length_c                   17.4977(3)
_cell_angle_alpha                73.5796(13)
_cell_angle_beta                 85.7654(13)
_cell_angle_gamma                69.0385(13)
_cell_volume                     2136.52(6)
_cell_formula_units_Z            2
_cell_measurement_temperature    210.00(14)
_cell_measurement_reflns_used    43348
_cell_measurement_theta_min      2.9850
_cell_measurement_theta_max      27.5150

_exptl_crystal_description       cube
_exptl_crystal_colour            light-red
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    ?
_exptl_crystal_density_diffrn    1.529
_exptl_crystal_F_000             1020.000
_exptl_transmission_factor_min   ?
_exptl_transmission_factor_max   ?
_exptl_crystal_size_max          0.360
_exptl_crystal_size_mid          0.226
_exptl_crystal_size_min          0.166
_exptl_absorpt_coefficient_mu    0.439
_shelx_estimated_absorpt_T_min   ?
_shelx_estimated_absorpt_T_max   ?
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_correction_T_min  0.77970
_exptl_absorpt_correction_T_max  0.78544
_exptl_absorpt_process_details   
;
CrysAlisPro 1.171.38.46 (Rigaku Oxford Diffraction, 2015)
Empirical absorption correction using spherical harmonics,
 implemented in SCALE3 ABSPACK scaling algorithm.
;
_diffrn_ambient_temperature      210.00(14)
_diffrn_ambient_environment      N~2~
_diffrn_radiation_wavelength     0.71073
_diffrn_radiation_type           MoK\a
_diffrn_source                   'micro-focus sealed X-ray tube'
_diffrn_radiation_monochromator  mirror
_diffrn_measurement_device       'four-circle diffractometer'
_diffrn_measurement_device_type  
;
SuperNova, Single source at offset, Sapphire3
;
_diffrn_measurement_method       'ω scans'
_diffrn_detector_area_resol_mean 16.0267
_diffrn_reflns_number            82991
_diffrn_reflns_av_unetI/netI     0.0183
_diffrn_reflns_av_R_equivalents  0.0312
_diffrn_reflns_limit_h_min       -12
_diffrn_reflns_limit_h_max       13
_diffrn_reflns_limit_k_min       -16
_diffrn_reflns_limit_k_max       17
_diffrn_reflns_limit_l_min       -22
_diffrn_reflns_limit_l_max       22
_diffrn_reflns_theta_min         2.4660
_diffrn_reflns_theta_max         27.8098
_diffrn_reflns_theta_full        24.9737
_diffrn_measured_fraction_theta_max 0.9330
_diffrn_measured_fraction_theta_full 0.9989
_diffrn_reflns_Laue_measured_fraction_max 0.933
_diffrn_reflns_Laue_measured_fraction_full 0.999
_diffrn_reflns_point_group_measured_fraction_max 0.933
_diffrn_reflns_point_group_measured_fraction_full 0.999
_reflns_number_total             9432
_reflns_number_gt                8474
_diffrn_orient_matrix_type       
;
CrysAlisPro convention (1999,Acta A55,543-557)
;
_diffrn_orient_matrix_UB_11      -0.0203550000
_diffrn_orient_matrix_UB_12      -0.0016240000
_diffrn_orient_matrix_UB_13      0.0399133000
_diffrn_orient_matrix_UB_21      -0.0717011000
_diffrn_orient_matrix_UB_22      0.0100786000
_diffrn_orient_matrix_UB_23      -0.0108508000
_diffrn_orient_matrix_UB_31      0.0151052000
_diffrn_orient_matrix_UB_32      -0.0569805000
_diffrn_orient_matrix_UB_33      0.0087630000
_diffrn_measurement_details      
;
List of Runs (angles in degrees, time in seconds):

  # Type    Start    End  Width  tₑₓₚ   ω     θ     κ     φ   Frames
#--------------------------------------------------------------------------
  1  ω    -41.00  52.00   0.75    7.50    --  -17.76  57.00 -30.00  124
  2  ω    -88.00   5.00   0.75    7.50    --  -17.76 -57.00-120.00  124
  3  ω    -88.00   5.00   0.75    7.50    --  -17.76 -57.00  60.00  124
  4  ω    -90.00  15.00   0.75    7.50    --  -17.76 -77.00 -30.00  140
  5  ω    -88.00   5.00   0.75    7.50    --  -17.76 -57.00-180.00  124
  6  ω    -20.00  62.50   0.75    7.50    --   18.62 -99.00 120.00  110
  7  ω    -20.00  62.50   0.75    7.50    --   18.62 -99.00  60.00  110
  8  ω    -54.00  51.00   0.75    7.50    --   18.62 -77.00-150.00  140
  9  ω    -51.00  54.00   0.75    7.50    --  -17.76  77.00-150.00  140
 10  ω    -20.00  26.50   0.75    7.50    --  -17.76 -99.00-120.00   62
 11  ω    -20.00  26.50   0.75    7.50    --  -17.76 -99.00  90.00   62
 12  ω    -20.00  62.50   0.75    7.50    --   18.62 -99.00 -60.00  110
 13  ω     -5.00  88.00   0.75    7.50    --   18.62  57.00 120.00  124
 14  ω     35.00  98.00   0.75    7.50    --   18.62 178.00-120.00   84
 15  ω    -51.00  54.00   0.75    7.50    --  -17.76  77.00  30.00  140
 16  ω    -97.00 -35.50   0.75    7.50    --  -17.76-178.00 120.00   82
 17  ω    -51.00  54.00   0.75    7.50    --  -17.76  77.00 -90.00  140
 18  ω    -56.00  94.00   0.75    7.50    --   18.62   0.00-120.00  200
 19  ω    -56.00  94.00   0.75    7.50    --   18.62   0.00-150.00  200
 20  ω    -56.00  94.00   0.75    7.50    --   18.62   0.00-180.00  200
 21  ω    -56.00  42.25   0.75    7.50    --   18.62   0.00 -60.00  131
 22  ω    -56.00  94.00   0.75    7.50    --   18.62   0.00 -90.00  200
;
_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 1.171.38.43 (Rigaku OD, 2015)
;
_computing_cell_refinement       
;
CrysAlisPro 1.171.38.43 (Rigaku OD, 2015)
;
_computing_data_reduction        
;
CrysAlisPro 1.171.38.43 (Rigaku OD, 2015)
;
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1997)'
_computing_structure_refinement  'SHELXL-2017/1 (Sheldrick, 2017)'
_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)+(0.0313P)²+0.9706P] where P=(Fo²+2Fc²)/3'
_atom_sites_solution_primary     difmap
_atom_sites_solution_secondary   difmap
_atom_sites_solution_hydrogens   mixed
_refine_ls_hydrogen_treatment    hetero
_refine_ls_extinction_method     none
_refine_ls_extinction_coef       .
_refine_ls_number_reflns         9431
_refine_ls_number_parameters     658
_refine_ls_number_restraints     0
_refine_ls_R_factor_all          0.0350
_refine_ls_R_factor_gt           0.0298
_refine_ls_wR_factor_ref         0.0757
_refine_ls_wR_factor_gt          0.0719
_refine_ls_goodness_of_fit_ref   1.037
_refine_ls_restrained_S_all      1.037
_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 0.03362(2) 0.54402(2) 0.23239(2) 0.02014(6) Uani 1 1 d . . . . .
N1 N 0.16404(13) 0.49385(11) 0.41129(7) 0.0283(3) Uani 1 1 d . . . . .
H1N H 0.187(2) 0.5525(16) 0.3949(11) 0.042 Uiso 1 1 d . U . . .
N2 N 0.09642(12) 0.47428(9) 0.35673(7) 0.0244(2) Uani 1 1 d . . . . .
N3 N -0.04364(12) 0.41308(9) 0.27255(7) 0.0232(2) Uani 1 1 d . . . . .
N4 N -0.07747(12) 0.54514(10) 0.12946(7) 0.0268(2) Uani 1 1 d . . . . .
N5 N -0.10469(14) 0.60083(11) 0.05196(7) 0.0330(3) Uani 1 1 d . . . . .
H5N H -0.072(2) 0.6555(16) 0.0318(12) 0.049 Uiso 1 1 d . U . . .
N6 N -0.25885(12) 0.69074(11) 0.30771(7) 0.0276(3) Uani 1 1 d . . . . .
H6N H -0.289(2) 0.6388(15) 0.3260(11) 0.041 Uiso 1 1 d . U . . .
N7 N -0.14548(11) 0.67689(9) 0.25972(6) 0.0228(2) Uani 1 1 d . . . . .
N8 N 0.08038(11) 0.68617(9) 0.17736(6) 0.0206(2) Uani 1 1 d . . . . .
N9 N 0.24170(12) 0.48830(9) 0.17917(6) 0.0227(2) Uani 1 1 d . . . . .
N10 N 0.34355(13) 0.39445(10) 0.17327(7) 0.0265(2) Uani 1 1 d . . . . .
H10N H 0.3325(19) 0.3334(15) 0.1991(11) 0.040 Uiso 1 1 d . U . . .
C1 C 0.17047(16) 0.42316(13) 0.48294(9) 0.0334(3) Uani 1 1 d . . . . .
H1 H 0.212014 0.421780 0.529257 0.040 Uiso 1 1 calc R U . . .
C2 C 0.10491(16) 0.35297(12) 0.47607(8) 0.0313(3) Uani 1 1 d . . . . .
H2 H 0.093411 0.294935 0.515736 0.038 Uiso 1 1 calc R U . . .
C3 C 0.05924(14) 0.38841(11) 0.39589(8) 0.0241(3) Uani 1 1 d . . . . .
C4 C -0.02392(14) 0.35438(11) 0.34942(8) 0.0238(3) Uani 1 1 d . . . . .
C5 C -0.08323(15) 0.27393(11) 0.37963(9) 0.0294(3) Uani 1 1 d . . . . .
H5 H -0.068516 0.233511 0.432853 0.035 Uiso 1 1 calc R U . . .
C6 C -0.16493(16) 0.25553(12) 0.32830(10) 0.0328(3) Uani 1 1 d . . . . .
H6 H -0.205811 0.202072 0.347037 0.039 Uiso 1 1 calc R U . . .
C7 C -0.18601(15) 0.31636(12) 0.24924(10) 0.0323(3) Uani 1 1 d . . . . .
H7 H -0.241117 0.304582 0.214566 0.039 Uiso 1 1 calc R U . . .
C8 C -0.12327(14) 0.39525(11) 0.22275(8) 0.0257(3) Uani 1 1 d . . . . .
C9 C -0.13669(14) 0.46821(12) 0.14165(8) 0.0269(3) Uani 1 1 d . . . . .
C10 C -0.20118(16) 0.47495(15) 0.07096(9) 0.0378(4) Uani 1 1 d . . . . .
H10 H -0.249055 0.431045 0.063383 0.045 Uiso 1 1 calc R U . . .
C11 C -0.17819(17) 0.56021(15) 0.01569(9) 0.0405(4) Uani 1 1 d . . . . .
H11 H -0.208099 0.585703 -0.037659 0.049 Uiso 1 1 calc R U . . .
C12 C -0.31366(16) 0.79337(13) 0.31356(9) 0.0322(3) Uani 1 1 d . . . . .
H12 H -0.391900 0.820907 0.343373 0.039 Uiso 1 1 calc R U . . .
C13 C -0.23418(15) 0.85054(12) 0.26792(9) 0.0288(3) Uani 1 1 d . . . . .
H13 H -0.246644 0.923557 0.260305 0.035 Uiso 1 1 calc R U . . .
C14 C -0.13042(14) 0.77491(11) 0.23541(8) 0.0220(3) Uani 1 1 d . . . . .
C15 C -0.01240(14) 0.78373(11) 0.18199(8) 0.0221(3) Uani 1 1 d . . . . .
C16 C 0.00487(15) 0.88035(11) 0.13885(8) 0.0271(3) Uani 1 1 d . . . . .
H16 H -0.061017 0.947438 0.141794 0.032 Uiso 1 1 calc R U . . .
C17 C 0.12321(16) 0.87424(11) 0.09110(9) 0.0292(3) Uani 1 1 d . . . . .
H17 H 0.137549 0.937847 0.061651 0.035 Uiso 1 1 calc R U . . .
C18 C 0.22009(15) 0.77353(11) 0.08721(8) 0.0260(3) Uani 1 1 d . . . . .
H18 H 0.300170 0.768643 0.055767 0.031 Uiso 1 1 calc R U . . .
C19 C 0.19497(14) 0.68032(11) 0.13121(7) 0.0214(3) Uani 1 1 d . . . . .
C20 C 0.28568(14) 0.56796(11) 0.13393(7) 0.0219(3) Uani 1 1 d . . . . .
C21 C 0.41586(15) 0.52393(12) 0.09910(9) 0.0289(3) Uani 1 1 d . . . . .
H21 H 0.468382 0.561464 0.065154 0.035 Uiso 1 1 calc R U . . .
C22 C 0.44894(15) 0.41306(12) 0.12612(9) 0.0309(3) Uani 1 1 d . . . . .
H22 H 0.529987 0.360243 0.113907 0.037 Uiso 1 1 calc R U . . .
N11 N -0.39668(14) 1.01249(11) 0.07091(7) 0.0325(3) Uani 1 1 d . . . . .
O1 O -0.48636(12) 0.67073(9) 0.19360(7) 0.0372(2) Uani 1 1 d . . . . .
O2 O -0.63652(13) 0.78487(10) 0.25850(7) 0.0410(3) Uani 1 1 d . . . . .
O3 O -0.34357(14) 1.08740(11) 0.03331(7) 0.0471(3) Uani 1 1 d . . . . .
C23 C -0.54843(15) 0.76395(12) 0.20686(8) 0.0295(3) Uani 1 1 d . . . . .
C24 C -0.50150(15) 0.85285(12) 0.15415(8) 0.0266(3) Uani 1 1 d . . . . .
C25 C -0.38833(15) 0.82997(12) 0.10322(8) 0.0300(3) Uani 1 1 d . . . . .
H25 H -0.347294 0.760085 0.096772 0.036 Uiso 1 1 calc R U . . .
C26 C -0.56411(16) 0.95897(12) 0.15940(9) 0.0332(3) Uani 1 1 d . . . . .
H26 H -0.642251 0.976845 0.191691 0.040 Uiso 1 1 calc R U . . .
C27 C -0.51130(18) 1.03801(13) 0.11713(9) 0.0364(3) Uani 1 1 d . . . . .
H27 H -0.554658 1.109368 0.120353 0.044 Uiso 1 1 calc R U . . .
C28 C -0.33687(16) 0.91031(13) 0.06235(8) 0.0326(3) Uani 1 1 d . . . . .
H28 H -0.260533 0.894475 0.028602 0.039 Uiso 1 1 calc R U . . .
N12 N -0.49441(12) 0.18974(9) 0.50894(7) 0.0260(2) Uani 1 1 d . . . . .
O4 O -0.36904(12) 0.52238(9) 0.37811(6) 0.0355(2) Uani 1 1 d . . . . .
O5 O -0.51616(14) 0.51455(10) 0.29096(7) 0.0459(3) Uani 1 1 d . . . . .
H1O H -0.504(2) 0.5923(19) 0.2483(13) 0.069 Uiso 1 1 d . U . . .
O6 O -0.51034(11) 0.10136(8) 0.55595(6) 0.0338(2) Uani 1 1 d . . . . .
C29 C -0.44574(15) 0.48047(12) 0.35704(9) 0.0286(3) Uani 1 1 d . . . . .
C30 C -0.46311(14) 0.37852(11) 0.41094(8) 0.0259(3) Uani 1 1 d . . . . .
C31 C -0.41681(15) 0.34048(12) 0.48995(8) 0.0283(3) Uani 1 1 d . . . . .
H31 H -0.374240 0.378359 0.510618 0.034 Uiso 1 1 calc R U . . .
C32 C -0.52502(15) 0.31875(12) 0.38230(9) 0.0287(3) Uani 1 1 d . . . . .
H32 H -0.557465 0.342691 0.329445 0.034 Uiso 1 1 calc R U . . .
C33 C -0.53864(15) 0.22486(12) 0.43130(8) 0.0290(3) Uani 1 1 d . . . . .
H33 H -0.578535 0.184964 0.411119 0.035 Uiso 1 1 calc R U . . .
C34 C -0.43343(15) 0.24679(12) 0.53817(8) 0.0289(3) Uani 1 1 d . . . . .
H34 H -0.402603 0.222240 0.591344 0.035 Uiso 1 1 calc R U . . .
N13 N 0.06974(12) 0.94411(10) 0.38167(7) 0.0277(2) Uani 1 1 d . . . . .
O7 O 0.19423(13) 1.22031(10) 0.16278(6) 0.0405(3) Uani 1 1 d . . . . .
O8 O 0.32477(11) 1.20367(9) 0.26631(7) 0.0355(2) Uani 1 1 d . . . . .
O9 O 0.02238(12) 0.86761(9) 0.42635(6) 0.0360(2) Uani 1 1 d . . . . .
C35 C 0.23495(15) 1.18098(11) 0.23379(9) 0.0278(3) Uani 1 1 d . . . . .
C36 C 0.17521(14) 1.09808(11) 0.28645(8) 0.0254(3) Uani 1 1 d . . . . .
C37 C 0.20777(15) 1.05675(12) 0.36758(9) 0.0301(3) Uani 1 1 d . . . . .
H37 H 0.267129 1.080546 0.390507 0.036 Uiso 1 1 calc R U . . .
C38 C 0.08654(16) 1.05985(12) 0.25509(9) 0.0309(3) Uani 1 1 d . . . . .
H38 H 0.061480 1.086410 0.201040 0.037 Uiso 1 1 calc R U . . .
C39 C 0.03543(16) 0.98320(13) 0.30309(9) 0.0329(3) Uani 1 1 d . . . . .
H39 H -0.023471 0.957972 0.281183 0.040 Uiso 1 1 calc R U . . .
C40 C 0.15363(15) 0.98123(12) 0.41451(9) 0.0303(3) Uani 1 1 d . . . . .
H40 H 0.174689 0.955527 0.469029 0.036 Uiso 1 1 calc R U . . .
O1W O 0.72646(14) 0.99327(10) 0.42092(7) 0.0396(3) Uani 1 1 d . . . . .
H1A H 0.808(3) 0.9460(18) 0.4233(13) 0.059 Uiso 1 1 d . U . . .
H1B H 0.670(2) 0.9626(18) 0.4347(13) 0.059 Uiso 1 1 d . U . . .
O2W O 0.63426(14) 0.12648(11) 0.26637(8) 0.0419(3) Uani 1 1 d . . . . .
H2A H 0.662(2) 0.0895(19) 0.3116(14) 0.063 Uiso 1 1 d . U . . .
H2B H 0.548(3) 0.1428(19) 0.2664(14) 0.063 Uiso 1 1 d . U . . .
O3W O 0.19630(15) 0.68998(11) 0.36360(8) 0.0446(3) Uani 1 1 d . . . . .
H3A H 0.244(3) 0.7137(19) 0.3303(14) 0.067 Uiso 1 1 d . U . . .
H3B H 0.143(3) 0.741(2) 0.3826(14) 0.067 Uiso 1 1 d . U . . .
O4W O 0.04013(16) 0.21716(12) 0.04240(8) 0.0475(3) Uani 1 1 d . . . . .
H4A H -0.034(3) 0.211(2) 0.0572(15) 0.071 Uiso 1 1 d . U . . .
H4B H 0.078(3) 0.2143(19) 0.0845(15) 0.071 Uiso 1 1 d . U . . .
O5W O -0.22137(16) 1.17180(13) 0.12156(9) 0.0551(4) Uani 1 1 d . . . . .
H5A H -0.255(3) 1.158(2) 0.1638(17) 0.083 Uiso 1 1 d . U . . .
H5B H -0.261(3) 1.148(2) 0.0935(16) 0.083 Uiso 1 1 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 N8 2.1061(11) . ?
Fe1 N3 2.1167(11) . ?
Fe1 N2 2.1534(11) . ?
Fe1 N4 2.1780(11) . ?
Fe1 N9 2.1798(11) . ?
Fe1 N7 2.1822(11) . ?
N1 C1 1.3381(19) . ?
N1 N2 1.3446(16) . ?
N1 H1N 0.876(19) . ?
N2 C3 1.3420(17) . ?
N3 C4 1.3441(17) . ?
N3 C8 1.3464(17) . ?
N4 C9 1.3406(19) . ?
N4 N5 1.3470(16) . ?
N5 C11 1.345(2) . ?
N5 H5N 0.89(2) . ?
N6 C12 1.340(2) . ?
N6 N7 1.3492(15) . ?
N6 H6N 0.841(19) . ?
N7 C14 1.3439(17) . ?
N8 C19 1.3431(16) . ?
N8 C15 1.3438(17) . ?
N9 C20 1.3438(16) . ?
N9 N10 1.3466(16) . ?
N10 C22 1.3413(19) . ?
N10 H10N 0.870(19) . ?
C1 C2 1.374(2) . ?
C1 H1 0.9300 . ?
C2 C3 1.4012(19) . ?
C2 H2 0.9300 . ?
C3 C4 1.4686(19) . ?
C4 C5 1.3884(19) . ?
C5 C6 1.385(2) . ?
C5 H5 0.9300 . ?
C6 C7 1.384(2) . ?
C6 H6 0.9300 . ?
C7 C8 1.387(2) . ?
C7 H7 0.9300 . ?
C8 C9 1.469(2) . ?
C9 C10 1.402(2) . ?
C10 C11 1.365(2) . ?
C10 H10 0.9300 . ?
C11 H11 0.9300 . ?
C12 C13 1.369(2) . ?
C12 H12 0.9300 . ?
C13 C14 1.3940(19) . ?
C13 H13 0.9300 . ?
C14 C15 1.4676(18) . ?
C15 C16 1.3854(19) . ?
C16 C17 1.388(2) . ?
C16 H16 0.9300 . ?
C17 C18 1.386(2) . ?
C17 H17 0.9300 . ?
C18 C19 1.3858(18) . ?
C18 H18 0.9300 . ?
C19 C20 1.4650(18) . ?
C20 C21 1.3983(19) . ?
C21 C22 1.372(2) . ?
C21 H21 0.9300 . ?
C22 H22 0.9300 . ?
N11 O3 1.3100(16) . ?
N11 C27 1.351(2) . ?
N11 C28 1.354(2) . ?
O1 C23 1.2799(18) . ?
O1 H1O 1.27(2) . ?
O2 C23 1.2335(18) . ?
C23 C24 1.5010(19) . ?
C24 C26 1.384(2) . ?
C24 C25 1.388(2) . ?
C25 C28 1.373(2) . ?
C25 H25 0.9300 . ?
C26 C27 1.374(2) . ?
C26 H26 0.9300 . ?
C27 H27 0.9300 . ?
C28 H28 0.9300 . ?
N12 O6 1.3092(15) . ?
N12 C33 1.3562(18) . ?
N12 C34 1.3602(18) . ?
O4 C29 1.2349(18) . ?
O5 C29 1.2769(18) . ?
O5 H1O 1.15(2) . ?
C29 C30 1.5042(19) . ?
C30 C31 1.383(2) . ?
C30 C32 1.392(2) . ?
C31 C34 1.377(2) . ?
C31 H31 0.9300 . ?
C32 C33 1.372(2) . ?
C32 H32 0.9300 . ?
C33 H33 0.9300 . ?
C34 H34 0.9300 . ?
N13 O9 1.3276(15) . ?
N13 C39 1.3478(19) . ?
N13 C40 1.3526(19) . ?
O7 C35 1.2405(18) . ?
O8 C35 1.2645(17) . ?
C35 C36 1.5159(19) . ?
C36 C38 1.387(2) . ?
C36 C37 1.387(2) . ?
C37 C40 1.373(2) . ?
C37 H37 0.9300 . ?
C38 C39 1.372(2) . ?
C38 H38 0.9300 . ?
C39 H39 0.9300 . ?
C40 H40 0.9300 . ?
O1W H1A 0.83(2) . ?
O1W H1B 0.80(2) . ?
O2W H2A 0.81(2) . ?
O2W H2B 0.81(2) . ?
O3W H3A 0.80(2) . ?
O3W H3B 0.85(2) . ?
O4W H4A 0.79(3) . ?
O4W H4B 0.84(3) . ?
O5W H5A 0.79(3) . ?
O5W H5B 0.84(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
N8 Fe1 N3 169.85(4) . . ?
N8 Fe1 N2 114.62(4) . . ?
N3 Fe1 N2 74.38(4) . . ?
N8 Fe1 N4 96.23(4) . . ?
N3 Fe1 N4 74.56(4) . . ?
N2 Fe1 N4 148.90(4) . . ?
N8 Fe1 N9 74.52(4) . . ?
N3 Fe1 N9 109.49(4) . . ?
N2 Fe1 N9 99.85(4) . . ?
N4 Fe1 N9 91.77(4) . . ?
N8 Fe1 N7 74.93(4) . . ?
N3 Fe1 N7 101.00(4) . . ?
N2 Fe1 N7 90.86(4) . . ?
N4 Fe1 N7 93.61(4) . . ?
N9 Fe1 N7 149.37(4) . . ?
C1 N1 N2 111.41(12) . . ?
C1 N1 H1N 132.8(12) . . ?
N2 N1 H1N 115.5(12) . . ?
C3 N2 N1 105.61(11) . . ?
C3 N2 Fe1 116.81(9) . . ?
N1 N2 Fe1 137.57(9) . . ?
C4 N3 C8 120.19(12) . . ?
C4 N3 Fe1 119.82(9) . . ?
C8 N3 Fe1 119.72(9) . . ?
C9 N4 N5 105.48(12) . . ?
C9 N4 Fe1 115.72(9) . . ?
N5 N4 Fe1 138.79(10) . . ?
C11 N5 N4 111.22(14) . . ?
C11 N5 H5N 129.5(13) . . ?
N4 N5 H5N 119.2(13) . . ?
C12 N6 N7 111.47(12) . . ?
C12 N6 H6N 129.4(13) . . ?
N7 N6 H6N 118.9(13) . . ?
C14 N7 N6 104.93(11) . . ?
C14 N7 Fe1 114.56(8) . . ?
N6 N7 Fe1 138.97(9) . . ?
C19 N8 C15 120.10(11) . . ?
C19 N8 Fe1 119.87(9) . . ?
C15 N8 Fe1 119.69(9) . . ?
C20 N9 N10 105.28(11) . . ?
C20 N9 Fe1 115.16(8) . . ?
N10 N9 Fe1 139.44(9) . . ?
C22 N10 N9 111.53(12) . . ?
C22 N10 H10N 130.4(12) . . ?
N9 N10 H10N 118.1(12) . . ?
N1 C1 C2 107.98(13) . . ?
N1 C1 H1 126.0 . . ?
C2 C1 H1 126.0 . . ?
C1 C2 C3 104.53(13) . . ?
C1 C2 H2 127.7 . . ?
C3 C2 H2 127.7 . . ?
N2 C3 C2 110.47(12) . . ?
N2 C3 C4 116.06(11) . . ?
C2 C3 C4 133.40(13) . . ?
N3 C4 C5 121.61(13) . . ?
N3 C4 C3 112.85(11) . . ?
C5 C4 C3 125.49(13) . . ?
C6 C5 C4 118.15(14) . . ?
C6 C5 H5 120.9 . . ?
C4 C5 H5 120.9 . . ?
C7 C6 C5 120.30(13) . . ?
C7 C6 H6 119.9 . . ?
C5 C6 H6 119.9 . . ?
C6 C7 C8 118.67(13) . . ?
C6 C7 H7 120.7 . . ?
C8 C7 H7 120.7 . . ?
N3 C8 C7 121.09(13) . . ?
N3 C8 C9 113.03(12) . . ?
C7 C8 C9 125.88(13) . . ?
N4 C9 C10 110.56(13) . . ?
N4 C9 C8 116.82(12) . . ?
C10 C9 C8 132.62(14) . . ?
C11 C10 C9 104.76(14) . . ?
C11 C10 H10 127.6 . . ?
C9 C10 H10 127.6 . . ?
N5 C11 C10 107.98(13) . . ?
N5 C11 H11 126.0 . . ?
C10 C11 H11 126.0 . . ?
N6 C12 C13 107.96(13) . . ?
N6 C12 H12 126.0 . . ?
C13 C12 H12 126.0 . . ?
C12 C13 C14 104.61(13) . . ?
C12 C13 H13 127.7 . . ?
C14 C13 H13 127.7 . . ?
N7 C14 C13 111.02(12) . . ?
N7 C14 C15 116.87(11) . . ?
C13 C14 C15 132.10(12) . . ?
N8 C15 C16 121.70(12) . . ?
N8 C15 C14 112.83(11) . . ?
C16 C15 C14 125.47(12) . . ?
C15 C16 C17 118.16(13) . . ?
C15 C16 H16 120.9 . . ?
C17 C16 H16 120.9 . . ?
C18 C17 C16 120.15(13) . . ?
C18 C17 H17 119.9 . . ?
C16 C17 H17 119.9 . . ?
C19 C18 C17 118.53(13) . . ?
C19 C18 H18 120.7 . . ?
C17 C18 H18 120.7 . . ?
N8 C19 C18 121.35(12) . . ?
N8 C19 C20 112.93(11) . . ?
C18 C19 C20 125.71(12) . . ?
N9 C20 C21 110.68(12) . . ?
N9 C20 C19 116.84(11) . . ?
C21 C20 C19 132.46(12) . . ?
C22 C21 C20 104.70(12) . . ?
C22 C21 H21 127.7 . . ?
C20 C21 H21 127.7 . . ?
N10 C22 C21 107.80(12) . . ?
N10 C22 H22 126.1 . . ?
C21 C22 H22 126.1 . . ?
O3 N11 C27 119.84(14) . . ?
O3 N11 C28 119.56(13) . . ?
C27 N11 C28 120.60(13) . . ?
C23 O1 H1O 113.3(10) . . ?
O2 C23 O1 126.64(14) . . ?
O2 C23 C24 119.34(13) . . ?
O1 C23 C24 113.99(13) . . ?
C26 C24 C25 118.27(13) . . ?
C26 C24 C23 120.36(13) . . ?
C25 C24 C23 121.22(13) . . ?
C28 C25 C24 120.12(14) . . ?
C28 C25 H25 119.9 . . ?
C24 C25 H25 119.9 . . ?
C27 C26 C24 120.29(14) . . ?
C27 C26 H26 119.9 . . ?
C24 C26 H26 119.9 . . ?
N11 C27 C26 120.26(14) . . ?
N11 C27 H27 119.9 . . ?
C26 C27 H27 119.9 . . ?
N11 C28 C25 120.33(13) . . ?
N11 C28 H28 119.8 . . ?
C25 C28 H28 119.8 . . ?
O6 N12 C33 120.38(12) . . ?
O6 N12 C34 119.80(12) . . ?
C33 N12 C34 119.82(12) . . ?
C29 O5 H1O 114.3(11) . . ?
O4 C29 O5 126.56(14) . . ?
O4 C29 C30 120.47(13) . . ?
O5 C29 C30 112.97(13) . . ?
C31 C30 C32 117.92(13) . . ?
C31 C30 C29 121.29(13) . . ?
C32 C30 C29 120.78(13) . . ?
C34 C31 C30 120.33(13) . . ?
C34 C31 H31 119.8 . . ?
C30 C31 H31 119.8 . . ?
C33 C32 C30 120.63(13) . . ?
C33 C32 H32 119.7 . . ?
C30 C32 H32 119.7 . . ?
N12 C33 C32 120.54(13) . . ?
N12 C33 H33 119.7 . . ?
C32 C33 H33 119.7 . . ?
N12 C34 C31 120.75(13) . . ?
N12 C34 H34 119.6 . . ?
C31 C34 H34 119.6 . . ?
O9 N13 C39 119.47(12) . . ?
O9 N13 C40 120.24(12) . . ?
C39 N13 C40 120.28(12) . . ?
O7 C35 O8 125.03(14) . . ?
O7 C35 C36 118.42(13) . . ?
O8 C35 C36 116.54(13) . . ?
C38 C36 C37 117.33(13) . . ?
C38 C36 C35 121.14(13) . . ?
C37 C36 C35 121.53(13) . . ?
C40 C37 C36 120.95(13) . . ?
C40 C37 H37 119.5 . . ?
C36 C37 H37 119.5 . . ?
C39 C38 C36 120.60(13) . . ?
C39 C38 H38 119.7 . . ?
C36 C38 H38 119.7 . . ?
N13 C39 C38 120.66(13) . . ?
N13 C39 H39 119.7 . . ?
C38 C39 H39 119.7 . . ?
N13 C40 C37 120.16(13) . . ?
N13 C40 H40 119.9 . . ?
C37 C40 H40 119.9 . . ?
H1A O1W H1B 108(2) . . ?
H2A O2W H2B 105(2) . . ?
H3A O3W H3B 108(2) . . ?
H4A O4W H4B 102(2) . . ?
H5A O5W H5B 103(2) . . ?

_refine_diff_density_max         0.302
_refine_diff_density_min         -0.352
_refine_diff_density_rms         0.051


_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_Fe_bpp_Noxid_NHoxid_PIHSrel_50K
_database_code_depnum_ccdc_archive 'CCDC 1984963'
loop_
_audit_author_name
_audit_author_address
'Veronica Jornet Molla'
;University of Valencia
Spain
;
_audit_update_record             
;
2020-02-18 deposited with the CCDC.	2020-11-23 downloaded from the CCDC.
;
# start Validation Reply Form
_vrf_PLAT213_Fe_bpp_Noxid_NHoxid_PIHSrel_50K 
;
PROBLEM: Atom C11             has ADP max/min Ratio .....        4.6 prolat
RESPONSE: The asymmetric unit of this structure contains a single independent Fe(II) centre with Fe-N bond lengths and octahedral distortion parameters indicating an intermediate state between those corresponding to HS and LS states. A mixed-spin phase has been trapped and this accounts for the high anisotropic displacement parameters obtained, resulting in large ellipsoids. Especially for those C and N atoms that are directly affected by the ligand bite angle, as is the case of C11.  The structure was attempted to be solved with a bigger unit cell having double volume and two Fe(II) complexes with corresponding high and low spin states. Nevertheless, it was not possible.
;
_vrf_PLAT303_Fe_bpp_Noxid_NHoxid_PIHSrel_50K 
;
PROBLEM: Full Occupancy Atom H1O       with # Connections       2.00 Check
RESPONSE: This hydrogen atom is located between two oxygen atoms that belong to  different carboxylate groups, forming a very strong hydrogen bond (the distance between the heteroatoms, O5 and O1, is 2.426 \%A). As a proton-transfer reaction is observed between the two carboxylate anions, different H...O distances are observed at different temperatures. Such a type of proton-transfer reaction is common when strong hydrogen bonds are established (see, for example Angew. Chem. Int. Ed. 2002, 41, 48-76)
;
# Added during the CSD deposition process: Tuesday 18 February 2020 10:39 PM
# end Validation Reply Form


_audit_creation_method           SHELXL-2018/3
_shelx_SHELXL_version_number     2018/3
_chemical_name_systematic        ?
_chemical_name_common            ?
_chemical_melting_point          ?
_chemical_formula_moiety         
'C22 H18 Fe N10 2+, C12 H9 N2 O6 1-, C6 H4 N O3 1-, 5(H2 O)'
_chemical_formula_sum            'C40 H41 Fe N13 O14'
_chemical_formula_weight         983.71

loop_
_atom_type_symbol
_atom_type_description
_atom_type_scat_dispersion_real
_atom_type_scat_dispersion_imag
_atom_type_scat_source
C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Fe Fe 0.3463 0.8444 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'

_space_group_crystal_system      triclinic
_space_group_IT_number           2
_space_group_name_H-M_alt        'P -1'
_space_group_name_Hall           '-P 1'

_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'

_cell_length_a                   9.9614(18)
_cell_length_b                   13.577(3)
_cell_length_c                   17.271(3)
_cell_angle_alpha                103.019(8)
_cell_angle_beta                 94.103(8)
_cell_angle_gamma                111.280(7)
_cell_volume                     2090.1(7)
_cell_formula_units_Z            2
_cell_measurement_temperature    50(1)
_cell_measurement_reflns_used    3840
_cell_measurement_theta_min      2.24
_cell_measurement_theta_max      21.45

_exptl_crystal_description       cube
_exptl_crystal_colour            red
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    ?
_exptl_crystal_density_diffrn    1.563
_exptl_crystal_F_000             1020
_exptl_transmission_factor_min   ?
_exptl_transmission_factor_max   ?
_exptl_crystal_size_max          0.494
_exptl_crystal_size_mid          0.166
_exptl_crystal_size_min          0.127
_exptl_absorpt_coefficient_mu    0.448
_shelx_estimated_absorpt_T_min   ?
_shelx_estimated_absorpt_T_max   ?
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_correction_T_min  0.6331
_exptl_absorpt_correction_T_max  0.7468
_exptl_absorpt_process_details   
;
 SADABS 2016/2: Krause, L., Herbst-Irmer, R., Sheldrick G.M. & Stalke D.,
 J. Appl. Cryst. 48 (2015) 3-10
;
_diffrn_ambient_temperature      50(1)
_diffrn_ambient_environment      He
_diffrn_radiation_wavelength     0.71073
_diffrn_radiation_type           MoK\a
_diffrn_source                   'micro-focus sealed X-ray tube'
_diffrn_radiation_monochromator  mirror
_diffrn_measurement_device_type  
;
Bruker SMART X2S benchtop crystallographic system
;
_diffrn_measurement_method       'ω scans'
_diffrn_detector_area_resol_mean 16.0267
_diffrn_reflns_number            38146
_diffrn_reflns_av_unetI/netI     0.1035
_diffrn_reflns_av_R_equivalents  0.0585
_diffrn_reflns_limit_h_min       -14
_diffrn_reflns_limit_h_max       15
_diffrn_reflns_limit_k_min       -19
_diffrn_reflns_limit_k_max       20
_diffrn_reflns_limit_l_min       -25
_diffrn_reflns_limit_l_max       26
_diffrn_reflns_theta_min         2.202
_diffrn_reflns_theta_max         34.308
_diffrn_reflns_theta_full        25.242
_diffrn_measured_fraction_theta_max 0.878
_diffrn_measured_fraction_theta_full 0.997
_diffrn_reflns_Laue_measured_fraction_max 0.878
_diffrn_reflns_Laue_measured_fraction_full 0.997
_diffrn_reflns_point_group_measured_fraction_max 0.878
_diffrn_reflns_point_group_measured_fraction_full 0.997
_reflns_number_total             15330
_reflns_number_gt                9930
_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       
;
'APEX3 v2017.3-0 (Bruker AXS)'
;
_computing_cell_refinement       
;
'APEX3 v2017.3-0 (Bruker AXS)'
SAINT Version 8.32B (Bruker AXS Inc., 2013) 
;
_computing_data_reduction        
;
APEX3 Version 2017.3 (Bruker AXS Inc.) 
SAINT Version 8.32B (Bruker AXS Inc., 2013) 
;
_computing_structure_solution    'SHELXT 2018/2 (Sheldrick, 2018)'
_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)+(0.0485P)²] where P=(Fo²+2Fc²)/3'
_atom_sites_solution_primary     difmap
_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         15330
_refine_ls_number_parameters     658
_refine_ls_number_restraints     0
_refine_ls_R_factor_all          0.0993
_refine_ls_R_factor_gt           0.0482
_refine_ls_wR_factor_ref         0.1156
_refine_ls_wR_factor_gt          0.1017
_refine_ls_goodness_of_fit_ref   1.035
_refine_ls_restrained_S_all      1.035
_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 0.91980(2) 0.45548(2) 0.22949(2) 0.00788(6) Uani 1 1 d . . . . .
C1 C 0.8971(2) 0.57185(18) 0.47899(12) 0.0299(5) Uani 1 1 d . . . . .
H1 H 0.856066 0.572050 0.525683 0.036 Uiso 1 1 calc R U . . .
C2 C 1.0332(2) 0.64263(16) 0.47314(11) 0.0243(4) Uani 1 1 d . . . . .
H2 H 1.101863 0.699885 0.513814 0.029 Uiso 1 1 calc R U . . .
C3 C 1.0449(2) 0.60870(14) 0.39148(10) 0.0167(4) Uani 1 1 d . . . . .
C4 C 1.16179(19) 0.64179(14) 0.34404(10) 0.0147(3) Uani 1 1 d . . . . .
C5 C 1.3017(2) 0.72112(14) 0.37304(11) 0.0166(3) Uani 1 1 d . . . . .
H5 H 1.328674 0.761910 0.426773 0.020 Uiso 1 1 calc R U . . .
C6 C 1.4009(2) 0.73820(14) 0.31963(11) 0.0187(4) Uani 1 1 d . . . . .
H6 H 1.495133 0.791557 0.337327 0.022 Uiso 1 1 calc R U . . .
C7 C 1.3587(2) 0.67537(14) 0.23994(11) 0.0196(4) Uani 1 1 d . . . . .
H7 H 1.424389 0.685690 0.203949 0.024 Uiso 1 1 calc R U . . .
C8 C 1.21775(19) 0.59726(14) 0.21483(10) 0.0164(4) Uani 1 1 d . . . . .
C9 C 1.1552(2) 0.52228(15) 0.13468(10) 0.0195(4) Uani 1 1 d . . . . .
C10 C 1.2069(3) 0.50805(19) 0.06107(11) 0.0334(6) Uani 1 1 d . . . . .
H10 H 1.297954 0.548351 0.050402 0.040 Uiso 1 1 calc R U . . .
C11 C 1.0945(3) 0.4222(2) 0.00857(11) 0.0408(7) Uani 1 1 d . . . . .
H11 H 1.094664 0.392884 -0.045543 0.049 Uiso 1 1 calc R U . . .
N1 N 0.83350(19) 0.50224(15) 0.40569(11) 0.0259(4) Uani 1 1 d . . . . .
H1N H 0.747(3) 0.4416(18) 0.3909(13) 0.039 Uiso 1 1 d . U . . .
N2 N 0.92221(16) 0.52300(12) 0.35067(9) 0.0188(3) Uani 1 1 d . . . . .
N3 N 1.12031(16) 0.58081(12) 0.26677(8) 0.0146(3) Uani 1 1 d . . . . .
N4 N 1.01773(17) 0.44780(12) 0.12633(8) 0.0182(3) Uani 1 1 d . . . . .
N5 N 0.9831(2) 0.38735(15) 0.04897(9) 0.0297(4) Uani 1 1 d . . . . .
H5N H 0.894(3) 0.3366(19) 0.0268(14) 0.045 Uiso 1 1 d . U . . .
C12 C 1.0284(2) 0.21578(16) 0.31576(10) 0.0209(4) Uani 1 1 d . . . . .
H12 H 1.081919 0.189916 0.346302 0.025 Uiso 1 1 calc R U . . .
C13 C 0.89224(19) 0.15636(14) 0.27129(10) 0.0163(3) Uani 1 1 d . . . . .
H13 H 0.834269 0.082960 0.265367 0.020 Uiso 1 1 calc R U . . .
C14 C 0.85902(17) 0.22986(12) 0.23665(9) 0.0092(3) Uani 1 1 d . . . . .
C15 C 0.73083(17) 0.21980(12) 0.18360(9) 0.0090(3) Uani 1 1 d . . . . .
C16 C 0.61696(17) 0.12325(13) 0.14063(9) 0.0110(3) Uani 1 1 d . . . . .
H16 H 0.615843 0.055518 0.143893 0.013 Uiso 1 1 calc R U . . .
C17 C 0.50424(17) 0.12999(13) 0.09246(9) 0.0113(3) Uani 1 1 d . . . . .
H17 H 0.426316 0.066336 0.063212 0.014 Uiso 1 1 calc R U . . .
C18 C 0.50828(17) 0.23205(12) 0.08812(9) 0.0105(3) Uani 1 1 d . . . . .
H18 H 0.433198 0.237654 0.056498 0.013 Uiso 1 1 calc R U . . .
C19 C 0.62676(17) 0.32535(12) 0.13198(9) 0.0090(3) Uani 1 1 d . . . . .
C20 C 0.65097(17) 0.43907(12) 0.13477(9) 0.0097(3) Uani 1 1 d . . . . .
C21 C 0.5672(2) 0.48723(14) 0.10155(10) 0.0175(4) Uani 1 1 d . . . . .
H21 H 0.476575 0.452157 0.068110 0.021 Uiso 1 1 calc R U . . .
C22 C 0.6489(2) 0.59818(15) 0.12942(11) 0.0235(4) Uani 1 1 d . . . . .
H22 H 0.622962 0.653500 0.118403 0.028 Uiso 1 1 calc R U . . .
N6 N 1.07148(16) 0.31809(13) 0.30768(8) 0.0172(3) Uani 1 1 d . . . . .
H6N H 1.146(2) 0.3651(17) 0.3239(12) 0.026 Uiso 1 1 d . U . . .
N7 N 0.96894(14) 0.32904(11) 0.25895(7) 0.0107(3) Uani 1 1 d . . . . .
N8 N 0.73587(14) 0.31892(10) 0.17845(7) 0.0083(3) Uani 1 1 d . . . . .
N9 N 0.77661(16) 0.51583(10) 0.17976(8) 0.0131(3) Uani 1 1 d . . . . .
N10 N 0.77218(19) 0.61251(11) 0.17517(9) 0.0210(4) Uani 1 1 d . . . . .
H10N H 0.846(2) 0.6746(17) 0.2048(12) 0.032 Uiso 1 1 d . U . . .
O4 O 0.34714(12) 0.48218(9) 0.37842(7) 0.0141(2) Uani 1 1 d . . . . .
O1 O 0.31486(12) 0.33209(9) 0.19221(7) 0.0133(2) Uani 1 1 d . . . . .
H1O H 0.408(2) 0.4024(15) 0.2403(11) 0.020 Uiso 1 1 d . U . . .
O6 O 0.90890(12) 0.90079(9) 0.55803(6) 0.0131(2) Uani 1 1 d . . . . .
O3 O -0.24430(12) -0.08456(9) 0.03128(7) 0.0162(3) Uani 1 1 d . . . . .
O7 O 1.09199(13) 0.78765(10) 0.16440(7) 0.0179(3) Uani 1 1 d . . . . .
O5 O 0.50359(13) 0.48698(9) 0.29000(7) 0.0156(2) Uani 1 1 d . . . . .
O8 O 0.97863(13) 0.80237(9) 0.27084(7) 0.0171(3) Uani 1 1 d . . . . .
O9 O 1.61521(13) 1.13738(10) 0.43110(7) 0.0175(3) Uani 1 1 d . . . . .
O2 O 0.34955(13) 0.21539(9) 0.25831(7) 0.0157(2) Uani 1 1 d . . . . .
N12 N 0.80468(14) 0.81338(10) 0.51022(8) 0.0104(3) Uani 1 1 d . . . . .
N11 N -0.11709(15) -0.01005(11) 0.06920(8) 0.0122(3) Uani 1 1 d . . . . .
N13 N 1.49215(15) 1.06036(12) 0.38608(8) 0.0147(3) Uani 1 1 d . . . . .
C23 C 0.28275(17) 0.23771(13) 0.20588(9) 0.0115(3) Uani 1 1 d . . . . .
C26 C 0.05686(17) 0.17379(13) 0.10187(9) 0.0105(3) Uani 1 1 d . . . . .
H26 H 0.085672 0.244302 0.095382 0.013 Uiso 1 1 calc R U . . .
C29 C 0.46669(18) 0.52296(13) 0.35673(9) 0.0112(3) Uani 1 1 d . . . . .
C24 C 0.14744(17) 0.14974(13) 0.15314(9) 0.0103(3) Uani 1 1 d . . . . .
C31 C 0.57593(17) 0.66300(13) 0.49111(9) 0.0109(3) Uani 1 1 d . . . . .
H31 H 0.495209 0.625340 0.512030 0.013 Uiso 1 1 calc R U . . .
C35 C 1.09134(19) 0.82596(13) 0.23723(10) 0.0144(3) Uani 1 1 d . . . . .
C34 C 0.68612(17) 0.75632(13) 0.53994(9) 0.0111(3) Uani 1 1 d . . . . .
H34 H 0.679587 0.780698 0.593804 0.013 Uiso 1 1 calc R U . . .
C28 C -0.02738(18) -0.03659(13) 0.11592(9) 0.0138(3) Uani 1 1 d . . . . .
H28 H -0.055034 -0.108483 0.119301 0.017 Uiso 1 1 calc R U . . .
C30 C 0.58492(17) 0.62505(13) 0.41099(9) 0.0100(3) Uani 1 1 d . . . . .
C32 C 0.70682(17) 0.68485(13) 0.38180(9) 0.0113(3) Uani 1 1 d . . . . .
H32 H 0.715540 0.661036 0.328240 0.014 Uiso 1 1 calc R U . . .
C27 C -0.07506(18) 0.09398(13) 0.06068(9) 0.0117(3) Uani 1 1 d . . . . .
H27 H -0.135635 0.110869 0.027025 0.014 Uiso 1 1 calc R U . . .
C33 C 0.81409(17) 0.77854(13) 0.43138(9) 0.0115(3) Uani 1 1 d . . . . .
H33 H 0.893818 0.818478 0.410847 0.014 Uiso 1 1 calc R U . . .
C40 C 1.37183(19) 1.02117(13) 0.42012(10) 0.0142(3) Uani 1 1 d . . . . .
H40 H 1.376952 1.045135 0.475530 0.017 Uiso 1 1 calc R U . . .
C37 C 1.24339(19) 0.94662(13) 0.37303(10) 0.0147(3) Uani 1 1 d . . . . .
H37 H 1.161081 0.921370 0.396749 0.018 Uiso 1 1 calc R U . . .
C25 C 0.10407(18) 0.04218(13) 0.15827(9) 0.0127(3) Uani 1 1 d . . . . .
H25 H 0.164434 0.023432 0.190582 0.015 Uiso 1 1 calc R U . . .
C36 C 1.23334(18) 0.90768(13) 0.29013(10) 0.0128(3) Uani 1 1 d . . . . .
C38 C 1.35985(19) 0.94767(14) 0.25766(10) 0.0159(3) Uani 1 1 d . . . . .
H38 H 1.357912 0.922789 0.202661 0.019 Uiso 1 1 calc R U . . .
C39 C 1.48720(19) 1.02335(15) 0.30602(10) 0.0172(4) Uani 1 1 d . . . . .
H39 H 1.570895 1.049441 0.283559 0.021 Uiso 1 1 calc R U . . .
O1W O 1.21488(14) 0.98914(10) 0.57724(7) 0.0150(3) Uani 1 1 d . . . . .
H1A H 1.256(2) 0.9425(16) 0.5740(11) 0.022 Uiso 1 1 d . U . . .
H1B H 1.134(2) 0.9618(16) 0.5678(12) 0.022 Uiso 1 1 d . U . . .
O2W O 1.25773(14) 1.12268(10) 0.73216(7) 0.0168(3) Uani 1 1 d . . . . .
H2A H 1.251(2) 1.0844(17) 0.6895(13) 0.025 Uiso 1 1 d . U . . .
H2B H 1.185(2) 1.1389(16) 0.7339(12) 0.025 Uiso 1 1 d . U . . .
O3W O 0.61079(15) 0.30744(12) 0.36100(8) 0.0231(3) Uani 1 1 d . . . . .
H3A H 0.536(3) 0.2844(18) 0.3268(13) 0.035 Uiso 1 1 d . U . . .
H3B H 0.612(2) 0.2547(18) 0.3874(12) 0.035 Uiso 1 1 d . U . . .
O4W O 1.25857(16) 0.78935(12) 0.04605(8) 0.0244(3) Uani 1 1 d . . . . .
H4A H 1.223(2) 0.7941(18) 0.0859(14) 0.037 Uiso 1 1 d . U . . .
H4B H 1.333(3) 0.795(2) 0.0612(14) 0.037 Uiso 1 1 d . U . . .
O5W O -0.44634(14) -0.16834(11) 0.12300(8) 0.0188(3) Uani 1 1 d . . . . .
H5A H -0.401(2) -0.1525(17) 0.1666(13) 0.028 Uiso 1 1 d . U . . .
H5B H -0.388(2) -0.1481(17) 0.0957(13) 0.028 Uiso 1 1 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 N8 2.0343(14) . ?
Fe1 N3 2.0384(16) . ?
Fe1 N2 2.0816(15) . ?
Fe1 N4 2.0919(14) . ?
Fe1 N7 2.1007(14) . ?
Fe1 N9 2.1057(15) . ?
C1 N1 1.345(3) . ?
C1 C2 1.374(3) . ?
C1 H1 0.9300 . ?
C2 C3 1.409(2) . ?
C2 H2 0.9300 . ?
C3 N2 1.349(2) . ?
C3 C4 1.467(2) . ?
C4 N3 1.346(2) . ?
C4 C5 1.386(2) . ?
C5 C6 1.394(2) . ?
C5 H5 0.9300 . ?
C6 C7 1.388(2) . ?
C6 H6 0.9300 . ?
C7 C8 1.382(3) . ?
C7 H7 0.9300 . ?
C8 N3 1.362(2) . ?
C8 C9 1.457(3) . ?
C9 N4 1.349(2) . ?
C9 C10 1.405(2) . ?
C10 C11 1.366(3) . ?
C10 H10 0.9300 . ?
C11 N5 1.349(3) . ?
C11 H11 0.9300 . ?
N1 N2 1.3504(19) . ?
N1 H1N 0.92(2) . ?
N4 N5 1.3461(19) . ?
N5 H5N 0.89(2) . ?
C12 N6 1.340(2) . ?
C12 C13 1.363(3) . ?
C12 H12 0.9300 . ?
C13 C14 1.394(2) . ?
C13 H13 0.9300 . ?
C14 N7 1.340(2) . ?
C14 C15 1.462(2) . ?
C15 N8 1.3516(19) . ?
C15 C16 1.385(2) . ?
C16 C17 1.392(2) . ?
C16 H16 0.9300 . ?
C17 C18 1.391(2) . ?
C17 H17 0.9300 . ?
C18 C19 1.388(2) . ?
C18 H18 0.9300 . ?
C19 N8 1.345(2) . ?
C19 C20 1.462(2) . ?
C20 N9 1.344(2) . ?
C20 C21 1.396(2) . ?
C21 C22 1.375(3) . ?
C21 H21 0.9300 . ?
C22 N10 1.338(3) . ?
C22 H22 0.9300 . ?
N6 N7 1.3482(19) . ?
N6 H6N 0.77(2) . ?
N9 N10 1.3489(19) . ?
N10 H10N 0.90(2) . ?
O4 C29 1.2426(19) . ?
O1 C23 1.2844(18) . ?
O1 H1O 1.164(19) . ?
O6 N12 1.3075(17) . ?
O3 N11 1.3078(17) . ?
O7 C35 1.2497(19) . ?
O5 C29 1.2803(18) . ?
O5 H1O 1.266(19) . ?
O8 C35 1.271(2) . ?
O9 N13 1.3295(18) . ?
O2 C23 1.2403(19) . ?
N12 C33 1.3589(19) . ?
N12 C34 1.364(2) . ?
N11 C28 1.357(2) . ?
N11 C27 1.366(2) . ?
N13 C39 1.351(2) . ?
N13 C40 1.358(2) . ?
C23 C24 1.496(2) . ?
C26 C27 1.376(2) . ?
C26 C24 1.391(2) . ?
C26 H26 0.9300 . ?
C29 C30 1.503(2) . ?
C24 C25 1.390(2) . ?
C31 C34 1.378(2) . ?
C31 C30 1.385(2) . ?
C31 H31 0.9300 . ?
C35 C36 1.512(2) . ?
C34 H34 0.9300 . ?
C28 C25 1.374(2) . ?
C28 H28 0.9300 . ?
C30 C32 1.394(2) . ?
C32 C33 1.373(2) . ?
C32 H32 0.9300 . ?
C27 H27 0.9300 . ?
C33 H33 0.9300 . ?
C40 C37 1.365(2) . ?
C40 H40 0.9300 . ?
C37 C36 1.393(2) . ?
C37 H37 0.9300 . ?
C25 H25 0.9300 . ?
C36 C38 1.393(2) . ?
C38 C39 1.370(2) . ?
C38 H38 0.9300 . ?
C39 H39 0.9300 . ?
O1W H1A 0.86(2) . ?
O1W H1B 0.74(2) . ?
O2W H2A 0.78(2) . ?
O2W H2B 0.83(2) . ?
O3W H3A 0.83(2) . ?
O3W H3B 0.93(2) . ?
O4W H4A 0.80(2) . ?
O4W H4B 0.74(2) . ?
O5W H5A 0.79(2) . ?
O5W H5B 0.79(2) . ?

loop_
_geom_angle_atom_site_label_1
_geom_angle_atom_site_label_2
_geom_angle_atom_site_label_3
_geom_angle
_geom_angle_site_symmetry_1
_geom_angle_site_symmetry_3
_geom_angle_publ_flag
N8 Fe1 N3 170.47(5) . . ?
N8 Fe1 N2 112.65(5) . . ?
N3 Fe1 N2 75.80(5) . . ?
N8 Fe1 N4 95.03(6) . . ?
N3 Fe1 N4 76.37(6) . . ?
N2 Fe1 N4 152.16(6) . . ?
N8 Fe1 N7 76.54(5) . . ?
N3 Fe1 N7 99.61(5) . . ?
N2 Fe1 N7 90.20(5) . . ?
N4 Fe1 N7 93.57(5) . . ?
N8 Fe1 N9 75.98(5) . . ?
N3 Fe1 N9 107.94(5) . . ?
N2 Fe1 N9 97.96(5) . . ?
N4 Fe1 N9 91.35(5) . . ?
N7 Fe1 N9 152.40(5) . . ?
N1 C1 C2 108.39(16) . . ?
N1 C1 H1 125.8 . . ?
C2 C1 H1 125.8 . . ?
C1 C2 C3 104.24(18) . . ?
C1 C2 H2 127.9 . . ?
C3 C2 H2 127.9 . . ?
N2 C3 C2 110.72(16) . . ?
N2 C3 C4 114.91(15) . . ?
C2 C3 C4 134.26(18) . . ?
N3 C4 C5 122.07(15) . . ?
N3 C4 C3 111.60(16) . . ?
C5 C4 C3 126.24(16) . . ?
C4 C5 C6 118.30(17) . . ?
C4 C5 H5 120.8 . . ?
C6 C5 H5 120.8 . . ?
C7 C6 C5 119.82(17) . . ?
C7 C6 H6 120.1 . . ?
C5 C6 H6 120.1 . . ?
C8 C7 C6 119.06(15) . . ?
C8 C7 H7 120.5 . . ?
C6 C7 H7 120.5 . . ?
N3 C8 C7 121.25(16) . . ?
N3 C8 C9 111.86(16) . . ?
C7 C8 C9 126.87(15) . . ?
N4 C9 C10 110.02(18) . . ?
N4 C9 C8 115.88(14) . . ?
C10 C9 C8 134.11(19) . . ?
C11 C10 C9 105.1(2) . . ?
C11 C10 H10 127.5 . . ?
C9 C10 H10 127.5 . . ?
N5 C11 C10 108.02(17) . . ?
N5 C11 H11 126.0 . . ?
C10 C11 H11 126.0 . . ?
C1 N1 N2 111.28(17) . . ?
C1 N1 H1N 129.5(14) . . ?
N2 N1 H1N 118.8(14) . . ?
C3 N2 N1 105.37(15) . . ?
C3 N2 Fe1 117.03(10) . . ?
N1 N2 Fe1 137.51(14) . . ?
C4 N3 C8 119.49(16) . . ?
C4 N3 Fe1 120.60(11) . . ?
C8 N3 Fe1 119.69(12) . . ?
N5 N4 C9 105.82(15) . . ?
N5 N4 Fe1 138.09(14) . . ?
C9 N4 Fe1 116.09(11) . . ?
N4 N5 C11 111.09(19) . . ?
N4 N5 H5N 123.4(15) . . ?
C11 N5 H5N 125.2(15) . . ?
N6 C12 C13 107.89(15) . . ?
N6 C12 H12 126.1 . . ?
C13 C12 H12 126.1 . . ?
C12 C13 C14 104.79(15) . . ?
C12 C13 H13 127.6 . . ?
C14 C13 H13 127.6 . . ?
N7 C14 C13 110.92(15) . . ?
N7 C14 C15 116.02(13) . . ?
C13 C14 C15 133.05(15) . . ?
N8 C15 C16 121.68(14) . . ?
N8 C15 C14 111.67(13) . . ?
C16 C15 C14 126.62(14) . . ?
C15 C16 C17 118.41(14) . . ?
C15 C16 H16 120.8 . . ?
C17 C16 H16 120.8 . . ?
C18 C17 C16 119.91(15) . . ?
C18 C17 H17 120.0 . . ?
C16 C17 H17 120.0 . . ?
C19 C18 C17 118.57(15) . . ?
C19 C18 H18 120.7 . . ?
C17 C18 H18 120.7 . . ?
N8 C19 C18 121.57(14) . . ?
N8 C19 C20 111.83(13) . . ?
C18 C19 C20 126.61(14) . . ?
N9 C20 C21 110.99(14) . . ?
N9 C20 C19 115.84(14) . . ?
C21 C20 C19 133.14(15) . . ?
C22 C21 C20 104.46(17) . . ?
C22 C21 H21 127.8 . . ?
C20 C21 H21 127.8 . . ?
N10 C22 C21 107.92(15) . . ?
N10 C22 H22 126.0 . . ?
C21 C22 H22 126.0 . . ?
C12 N6 N7 111.46(14) . . ?
C12 N6 H6N 127.4(16) . . ?
N7 N6 H6N 120.8(16) . . ?
C14 N7 N6 104.93(13) . . ?
C14 N7 Fe1 115.13(10) . . ?
N6 N7 Fe1 138.53(11) . . ?
C19 N8 C15 119.84(13) . . ?
C19 N8 Fe1 120.10(10) . . ?
C15 N8 Fe1 119.61(11) . . ?
C20 N9 N10 105.03(14) . . ?
C20 N9 Fe1 115.47(10) . . ?
N10 N9 Fe1 139.41(12) . . ?
C22 N10 N9 111.60(15) . . ?
C22 N10 H10N 130.6(13) . . ?
N9 N10 H10N 117.6(14) . . ?
C23 O1 H1O 113.2(9) . . ?
C29 O5 H1O 117.1(8) . . ?
O6 N12 C33 120.55(13) . . ?
O6 N12 C34 119.66(13) . . ?
C33 N12 C34 119.79(14) . . ?
O3 N11 C28 120.04(13) . . ?
O3 N11 C27 119.47(13) . . ?
C28 N11 C27 120.49(14) . . ?
O9 N13 C39 119.37(14) . . ?
O9 N13 C40 120.15(14) . . ?
C39 N13 C40 120.46(16) . . ?
O2 C23 O1 126.63(15) . . ?
O2 C23 C24 119.28(14) . . ?
O1 C23 C24 114.06(14) . . ?
C27 C26 C24 120.45(14) . . ?
C27 C26 H26 119.8 . . ?
C24 C26 H26 119.8 . . ?
O4 C29 O5 126.53(15) . . ?
O4 C29 C30 120.05(14) . . ?
O5 C29 C30 113.42(14) . . ?
C25 C24 C26 118.14(15) . . ?
C25 C24 C23 120.27(14) . . ?
C26 C24 C23 121.46(14) . . ?
C34 C31 C30 120.25(15) . . ?
C34 C31 H31 119.9 . . ?
C30 C31 H31 119.9 . . ?
O7 C35 O8 124.78(17) . . ?
O7 C35 C36 118.60(15) . . ?
O8 C35 C36 116.62(14) . . ?
N12 C34 C31 120.79(14) . . ?
N12 C34 H34 119.6 . . ?
C31 C34 H34 119.6 . . ?
N11 C28 C25 120.36(15) . . ?
N11 C28 H28 119.8 . . ?
C25 C28 H28 119.8 . . ?
C31 C30 C32 118.00(15) . . ?
C31 C30 C29 121.22(14) . . ?
C32 C30 C29 120.78(14) . . ?
C33 C32 C30 120.63(14) . . ?
C33 C32 H32 119.7 . . ?
C30 C32 H32 119.7 . . ?
N11 C27 C26 120.02(15) . . ?
N11 C27 H27 120.0 . . ?
C26 C27 H27 120.0 . . ?
N12 C33 C32 120.52(15) . . ?
N12 C33 H33 119.7 . . ?
C32 C33 H33 119.7 . . ?
N13 C40 C37 120.01(15) . . ?
N13 C40 H40 120.0 . . ?
C37 C40 H40 120.0 . . ?
C40 C37 C36 121.22(15) . . ?
C40 C37 H37 119.4 . . ?
C36 C37 H37 119.4 . . ?
C28 C25 C24 120.43(15) . . ?
C28 C25 H25 119.8 . . ?
C24 C25 H25 119.8 . . ?
C37 C36 C38 117.14(16) . . ?
C37 C36 C35 121.71(14) . . ?
C38 C36 C35 121.16(14) . . ?
C39 C38 C36 120.60(15) . . ?
C39 C38 H38 119.7 . . ?
C36 C38 H38 119.7 . . ?
N13 C39 C38 120.54(16) . . ?
N13 C39 H39 119.7 . . ?
C38 C39 H39 119.7 . . ?
H1A O1W H1B 112(2) . . ?
H2A O2W H2B 109(2) . . ?
H3A O3W H3B 111.6(19) . . ?
H4A O4W H4B 103(2) . . ?
H5A O5W H5B 105(2) . . ?

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 O3W 0.92(2) 1.76(2) 2.662(2) 166(2) . yes
N5 H5N O4W 0.89(2) 1.92(2) 2.777(2) 160(2) 2_765 yes
N6 H6N O4 0.77(2) 2.04(2) 2.8017(19) 173(2) 1_655 yes
N10 H10N O8 0.90(2) 1.81(2) 2.711(2) 173(2) . yes
O1 H1O O5 1.164(19) 1.266(19) 2.4258(16) 172.8(17) . yes
O1W H1A O9 0.86(2) 1.96(2) 2.8054(18) 168.3(18) 2_876 yes
O1W H1B O6 0.74(2) 2.07(2) 2.8037(17) 172(2) . yes
O2W H2A O1W 0.78(2) 2.00(2) 2.7780(18) 174(2) . yes
O2W H2B O8 0.83(2) 2.06(2) 2.8857(18) 171(2) 2_776 yes
O3W H3A O2 0.83(2) 1.91(2) 2.7313(18) 171(2) . yes
O3W H3B O9 0.93(2) 1.92(2) 2.8503(19) 174.2(19) 1_445 yes
O4W H4A O7 0.80(2) 1.94(2) 2.7222(18) 166(2) . yes
O4W H4B O5W 0.74(2) 2.20(2) 2.934(2) 171(3) 1_765 yes
O5W H5A O2W 0.79(2) 2.04(2) 2.8204(19) 169(2) 2_666 yes
O5W H5B O3 0.79(2) 1.95(2) 2.7313(17) 175(2) . yes

_refine_diff_density_max         0.597
_refine_diff_density_min         -0.818
_refine_diff_density_rms         0.097


_exptl_crystal_recrystallization_method 
'Re-crystallisation from solvent: MeOH/H2O'
_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_Fe_bpp_Noxid_NHoxid_Neutrons_50K_LS
_database_code_depnum_ccdc_archive 'CCDC 1984958'
loop_
_audit_author_name
_audit_author_address
'Veronica Jornet Molla'
;University of Valencia
Spain
;
_audit_update_record             
;
2020-02-21 deposited with the CCDC.	2020-11-23 downloaded from the CCDC.
;
# start Validation Reply Form
_vrf_PLAT029_Fe_bpp_Noxid_NHoxid_Neutrons_50K_LS 
;
PROBLEM: _diffrn_measured_fraction_theta_full value Low .      0.845 Why?
RESPONSE: The wavelength used for this experiment is 1.45470 \%A. Therefore, the number of collected reflections is low and this results in a low value of measured fraction theta full.
;
_vrf_PLAT088_Fe_bpp_Noxid_NHoxid_Neutrons_50K_LS 
;
PROBLEM: Poor Data / Parameter Ratio ....................       6.45 Note
RESPONSE: The wavelength used for this experiment is 1.45470 \%A. Therefore, the number of collected reflections is low and not enough to yield a data/parameter ratio of 10.
;
_vrf_PLAT911_Fe_bpp_Noxid_NHoxid_Neutrons_50K_LS 
;
PROBLEM: Missing FCF Refl Between Thmin & STh/L=    0.600       1015 Report
RESPONSE: Some reflections are missing due to the restrictions of the experiment. The sample was placed on a close-circuit displex device on the monochromatic four-circle diffractometer D19 at ILL (Grenoble, France). The measurement strategy consisted on 25 omega (\w) scans with steps of 0.07\% at different \c and \f positions. These omega scans cover either 79\% or 64\% depending on the \c angle, in order to avoid collisions with the sample environment. Absorption correction removes reflections due to the environment provided by the neutron setup.
;
_vrf_PLAT155_Fe_bpp_Noxid_NHoxid_Neutrons_50K_LS 
;
PROBLEM: The Triclinic Unitcell is NOT Reduced ..........     Please Do !
RESPONSE: The structural transition that takes place at low temperatures causes an increase in the gamma angle, changing from an acute angle (at higher temperatures) to an obtuse value, resulting in a non-reduced set of cell parameters. The non-reduced unit cell was preferred in order to facilitate comparisons with the crystal structure solutions at higher temperatures.
;
_vrf_PLAT303_Fe_bpp_Noxid_NHoxid_Neutrons_50K_LS 
;
PROBLEM: Full Occupancy Atom H1O       with # Connections       2.00 Check
RESPONSE: This hydrogen atom is located between two oxygen atoms that belong to different carboxylate groups, forming a very strong hydrogen bond (the distance between the heteroatoms, O5 and O1, is 2.419 \%A). As a proton-transfer reaction is observed between the two carboxylate anions, different H...O distances are observed at different temperatures. Such a type of proton-transfer reaction is common when strong hydrogen bonds are established (see, for example Angew. Chem. Int. Ed. 2002, 41, 48-76).
;
# Added during the CSD deposition process: Friday 21 February 2020 08:08 PM
# end Validation Reply Form


_audit_creation_method           SHELXL-2018/3
_shelx_SHELXL_version_number     2018/3
_chemical_name_systematic        ?
_chemical_name_common            ?
_chemical_melting_point          ?
_chemical_formula_moiety         
'C22 H18 Fe N10 2+, C12 H9 N2 O6 1-, C6 H4 N O3 1-, 5(H2 O)'
_chemical_formula_sum            'C40 H41 Fe N13 O14'
_chemical_formula_weight         983.71

loop_
_atom_type_symbol
_atom_type_description
_atom_type_scat_dispersion_real
_atom_type_scat_dispersion_imag
_atom_type_scat_source
C C 0.0000 0.0000
'Neutron Data Booklet, ILL Grenoble, France (2003) ISBN 0-9704143-7-4'
H H 0.0000 0.0000
'Neutron Data Booklet, ILL Grenoble, France (2003) ISBN 0-9704143-7-4'
Fe Fe 0.0000 0.0000
'Neutron Data Booklet, ILL Grenoble, France (2003) ISBN 0-9704143-7-4'
O O 0.0000 0.0000
'Neutron Data Booklet, ILL Grenoble, France (2003) ISBN 0-9704143-7-4'
N N 0.0000 0.0000
'Neutron Data Booklet, ILL Grenoble, France (2003) ISBN 0-9704143-7-4'

_space_group_crystal_system      triclinic
_space_group_IT_number           2
_space_group_name_H-M_alt        'P -1'
_space_group_name_Hall           '-P 1'

_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'

_cell_length_a                   9.9719(3)
_cell_length_b                   13.5419(4)
_cell_length_c                   17.0957(5)
_cell_angle_alpha                76.716(2)
_cell_angle_beta                 85.858(2)
_cell_angle_gamma                110.386(2)
_cell_volume                     2076.54(11)
_cell_formula_units_Z            2
_cell_measurement_temperature    50(1)
_cell_measurement_reflns_used    3521
_cell_measurement_theta_min      5.281
_cell_measurement_theta_max      59.875

_exptl_crystal_description       cube
_exptl_crystal_colour            dark-red
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    ?
_exptl_crystal_density_diffrn    1.573
_exptl_crystal_F_000             650
_exptl_transmission_factor_min   ?
_exptl_transmission_factor_max   ?
_exptl_crystal_size_max          1.85
_exptl_crystal_size_mid          1.50
_exptl_crystal_size_min          0.7
_exptl_absorpt_coefficient_mu    0.194
_shelx_estimated_absorpt_T_min   ?
_shelx_estimated_absorpt_T_max   ?
_exptl_absorpt_correction_type   numerical
_exptl_absorpt_correction_T_min  ?
_exptl_absorpt_correction_T_max  ?
_exptl_absorpt_process_details   
; 
Absorption corretion done through d19face, d19abs and d19abscan 
programs from ILL
;
_diffrn_ambient_temperature      50(1)
_diffrn_radiation_wavelength     1.454696
_diffrn_radiation_type           neutrons
_diffrn_source                   'neutron source'
_diffrn_source_type              'ILL High Flux Reactor, beam H11'
_diffrn_source_power             57MW
_diffrn_measurement_device_type  
'D19 position-sensitive detector diffractometer'
_diffrn_radiation_monochromator  'copper 220'
_diffrn_measurement_method       'omega step-scans'
_diffrn_detector_area_resol_mean '1.56 mm vert. 2.5 mm hor.'
_diffrn_reflns_number            12440
_diffrn_reflns_av_unetI/netI     0.0273
_diffrn_reflns_av_R_equivalents  0.0423
_diffrn_reflns_limit_h_min       -10
_diffrn_reflns_limit_h_max       2
_diffrn_reflns_limit_k_min       -15
_diffrn_reflns_limit_k_max       16
_diffrn_reflns_limit_l_min       -20
_diffrn_reflns_limit_l_max       20
_diffrn_reflns_theta_min         4.527
_diffrn_reflns_theta_max         60.738
_diffrn_reflns_theta_full        60.738
_diffrn_measured_fraction_theta_max 0.845
_diffrn_measured_fraction_theta_full 0.845
_diffrn_reflns_Laue_measured_fraction_max 0.845
_diffrn_reflns_Laue_measured_fraction_full 0.845
_diffrn_reflns_point_group_measured_fraction_max 0.845
_diffrn_reflns_point_group_measured_fraction_full 0.845
_reflns_number_total             6336
_reflns_number_gt                5963
_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       'The NOMAD software from ILL '
_computing_cell_refinement       'PFIND and DIRAX programs'
_computing_data_reduction        'RETREAT and RAFD19 programs'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1997)'
_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)+(0.1324P)²+21.6146P] where P=(Fo²+2Fc²)/3'
_atom_sites_solution_primary     difmap
_atom_sites_solution_secondary   difmap
_atom_sites_solution_hydrogens   difmap
_refine_ls_hydrogen_treatment    refall
_refine_ls_extinction_method     none
_refine_ls_extinction_coef       .
_refine_ls_number_reflns         6336
_refine_ls_number_parameters     982
_refine_ls_number_restraints     0
_refine_ls_R_factor_all          0.0717
_refine_ls_R_factor_gt           0.0689
_refine_ls_wR_factor_ref         0.1900
_refine_ls_wR_factor_gt          0.1862
_refine_ls_goodness_of_fit_ref   1.109
_refine_ls_restrained_S_all      1.109
_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
Fe1 Fe 0.0835(2) 0.54679(14) 0.22436(10) 0.0143(4) Uani 1 1 d . . . . .
N1 N 0.1779(2) 0.50521(16) 0.39455(11) 0.0180(4) Uani 1 1 d . . . . .
H1N H 0.2720(7) 0.5747(5) 0.3779(3) 0.0289(12) Uani 1 1 d . . . . .
N2 N 0.0884(2) 0.48225(15) 0.34069(11) 0.0167(4) Uani 1 1 d . . . . .
N3 N -0.1054(2) 0.42913(15) 0.25736(11) 0.0168(4) Uani 1 1 d . . . . .
N4 N 0.0045(2) 0.56512(15) 0.12225(11) 0.0178(4) Uani 1 1 d . . . . .
N5 N 0.0485(2) 0.63090(17) 0.04576(12) 0.0194(4) Uani 1 1 d . . . . .
H5N H 0.1491(7) 0.6891(5) 0.0253(3) 0.0298(12) Uani 1 1 d . . . . .
N6 N -0.0731(2) 0.66679(16) 0.30833(11) 0.0180(4) Uani 1 1 d . . . . .
H6N H -0.1739(6) 0.6023(5) 0.3287(3) 0.0294(12) Uani 1 1 d . . . . .
N7 N 0.0318(2) 0.66150(15) 0.25793(11) 0.0170(4) Uani 1 1 d . . . . .
N8 N 0.2614(2) 0.67310(15) 0.18007(11) 0.0170(4) Uani 1 1 d . . . . .
N9 N 0.2104(2) 0.47908(15) 0.18020(11) 0.0165(4) Uani 1 1 d . . . . .
N10 N 0.2058(2) 0.37921(16) 0.17912(11) 0.0184(4) Uani 1 1 d . . . . .
H10N H 0.1212(7) 0.3091(5) 0.2135(3) 0.0297(12) Uani 1 1 d . . . . .
C1 C 0.1177(3) 0.4378(2) 0.46990(17) 0.0193(6) Uani 1 1 d . . . . .
H1 H 0.1739(8) 0.4451(5) 0.5199(3) 0.0371(14) Uani 1 1 d . . . . .
C2 C -0.0189(3) 0.3657(2) 0.46530(15) 0.0174(6) Uani 1 1 d . . . . .
H2 H -0.0973(7) 0.3021(5) 0.5141(4) 0.0347(14) Uani 1 1 d . . . . .
C3 C -0.0330(3) 0.3974(2) 0.38294(16) 0.0172(6) Uani 1 1 d . . . . .
C4 C -0.1474(3) 0.3660(2) 0.33520(15) 0.0163(6) Uani 1 1 d . . . . .
C5 C -0.2867(3) 0.2874(2) 0.36208(17) 0.0194(6) Uani 1 1 d . . . . .
H5 H -0.3186(7) 0.2388(5) 0.4253(4) 0.0322(13) Uani 1 1 d . . . . .
C6 C -0.3829(3) 0.2728(2) 0.30641(16) 0.0203(6) Uani 1 1 d . . . . .
H6 H -0.4908(7) 0.2122(5) 0.3251(4) 0.0348(13) Uani 1 1 d . . . . .
C7 C -0.3387(3) 0.3389(2) 0.22556(17) 0.0193(6) Uani 1 1 d . . . . .
H7 H -0.4117(7) 0.3287(5) 0.1818(4) 0.0363(14) Uani 1 1 d . . . . .
C8 C -0.1986(3) 0.4171(2) 0.20380(16) 0.0170(6) Uani 1 1 d . . . . .
C9 C -0.1325(3) 0.4954(2) 0.12516(15) 0.0170(5) Uani 1 1 d . . . . .
C10 C -0.1751(3) 0.5179(2) 0.04845(16) 0.0186(6) Uani 1 1 d . . . . .
H10 H -0.2754(7) 0.4761(5) 0.0312(4) 0.0369(14) Uani 1 1 d . . . . .
C11 C -0.0564(3) 0.6051(2) -0.00071(17) 0.0210(6) Uani 1 1 d . . . . .
H11 H -0.0371(7) 0.6492(5) -0.0627(4) 0.0357(14) Uani 1 1 d . . . . .
C12 C -0.0356(3) 0.7668(2) 0.32116(16) 0.0195(6) Uani 1 1 d . . . . .
H12 H -0.1072(7) 0.7875(6) 0.3579(4) 0.0370(14) Uani 1 1 d . . . . .
C13 C 0.1011(3) 0.8310(2) 0.27693(16) 0.0191(6) Uani 1 1 d . . . . .
H13 H 0.1608(7) 0.9153(5) 0.2730(4) 0.0333(13) Uani 1 1 d . . . . .
C14 C 0.1393(3) 0.7618(2) 0.23844(15) 0.0161(5) Uani 1 1 d . . . . .
C15 C 0.2672(3) 0.7723(2) 0.18588(15) 0.0152(5) Uani 1 1 d . . . . .
C16 C 0.3816(3) 0.8673(2) 0.14359(16) 0.0182(6) Uani 1 1 d . . . . .
H16 H 0.3820(8) 0.9469(5) 0.1473(4) 0.0357(14) Uani 1 1 d . . . . .
C17 C 0.4947(3) 0.8591(2) 0.09558(15) 0.0173(6) Uani 1 1 d . . . . .
H17 H 0.5851(7) 0.9305(5) 0.0616(4) 0.0333(13) Uani 1 1 d . . . . .
C18 C 0.4886(3) 0.7570(2) 0.08989(16) 0.0180(6) Uani 1 1 d . . . . .
H18 H 0.5756(7) 0.7487(5) 0.0530(4) 0.0311(13) Uani 1 1 d . . . . .
C19 C 0.3693(3) 0.6641(2) 0.13363(15) 0.0156(5) Uani 1 1 d . . . . .
C20 C 0.3405(3) 0.5512(2) 0.13664(15) 0.0162(5) Uani 1 1 d . . . . .
C21 C 0.4191(3) 0.4949(2) 0.10731(17) 0.0193(6) Uani 1 1 d . . . . .
H21 H 0.5260(7) 0.5295(5) 0.0731(4) 0.0359(14) Uani 1 1 d . . . . .
C22 C 0.3297(3) 0.3855(2) 0.13589(17) 0.0199(6) Uani 1 1 d . . . . .
H22 H 0.3459(7) 0.3130(5) 0.1305(4) 0.0349(14) Uani 1 1 d . . . . .
N11 N 1.1184(2) 1.00911(17) 0.06929(12) 0.0201(4) Uani 1 1 d . . . . .
O1 O 0.6926(4) 0.6678(2) 0.19141(19) 0.0200(7) Uani 1 1 d . . . . .
O2 O 0.6559(4) 0.7844(3) 0.25831(19) 0.0222(7) Uani 1 1 d . . . . .
O3 O 1.2419(4) 1.0837(3) 0.0307(2) 0.0236(7) Uani 1 1 d . . . . .
C23 C 0.7234(3) 0.7620(2) 0.20537(16) 0.0193(6) Uani 1 1 d . . . . .
C24 C 0.8572(3) 0.8492(2) 0.15370(16) 0.0174(6) Uani 1 1 d . . . . .
C25 C 0.9473(3) 0.8256(2) 0.10087(16) 0.0178(6) Uani 1 1 d . . . . .
H25 H 0.9171(7) 0.7436(5) 0.0924(4) 0.0345(13) Uani 1 1 d . . . . .
C26 C 0.8986(3) 0.9552(2) 0.16113(16) 0.0195(6) Uani 1 1 d . . . . .
H26 H 0.8304(8) 0.9767(5) 0.2000(4) 0.0389(15) Uani 1 1 d . . . . .
C27 C 1.0284(3) 1.0344(2) 0.11783(17) 0.0207(6) Uani 1 1 d . . . . .
H27 H 1.0687(7) 1.1198(5) 0.1193(4) 0.0351(14) Uani 1 1 d . . . . .
C28 C 1.0782(3) 0.9067(2) 0.05912(16) 0.0202(6) Uani 1 1 d . . . . .
H28 H 1.1573(7) 0.8951(5) 0.0187(4) 0.0333(13) Uani 1 1 d . . . . .
N12 N 0.1987(2) 0.19004(15) 0.50952(11) 0.0176(4) Uani 1 1 d . . . . .
O4 O 0.6561(4) 0.5126(3) 0.37853(19) 0.0197(7) Uani 1 1 d . . . . .
O5 O 0.5032(4) 0.5134(3) 0.28723(19) 0.0222(7) Uani 1 1 d . . . . .
H1O H 0.5946(7) 0.5918(5) 0.2419(4) 0.0346(13) Uani 1 1 d . . . . .
O6 O 0.0936(4) 0.1053(3) 0.55780(18) 0.0202(7) Uani 1 1 d . . . . .
C29 C 0.5379(3) 0.4745(2) 0.35556(16) 0.0182(6) Uani 1 1 d . . . . .
C30 C 0.4197(3) 0.3741(2) 0.40927(16) 0.0174(6) Uani 1 1 d . . . . .
C31 C 0.4264(3) 0.3360(2) 0.49109(16) 0.0175(6) Uani 1 1 d . . . . .
H31 H 0.5181(6) 0.3779(5) 0.5171(4) 0.0326(13) Uani 1 1 d . . . . .
C32 C 0.2999(3) 0.3155(2) 0.37886(16) 0.0179(6) Uani 1 1 d . . . . .
H32 H 0.2901(7) 0.3428(5) 0.3159(3) 0.0341(14) Uani 1 1 d . . . . .
C33 C 0.1912(3) 0.2237(2) 0.42906(16) 0.0180(6) Uani 1 1 d . . . . .
H33 H 0.0950(7) 0.1749(5) 0.4096(4) 0.0363(14) Uani 1 1 d . . . . .
C34 C 0.3163(3) 0.2448(2) 0.54008(16) 0.0185(6) Uani 1 1 d . . . . .
H34 H 0.3137(7) 0.2118(5) 0.6040(3) 0.0323(13) Uani 1 1 d . . . . .
N13 N 0.4989(2) 1.06852(16) -0.39336(12) 0.0191(4) Uani 1 1 d . . . . .
O7 O 0.1074(4) 0.7981(3) -0.16925(19) 0.0215(7) Uani 1 1 d . . . . .
O8 O -0.0074(4) 0.8086(3) -0.27659(18) 0.0198(7) Uani 1 1 d . . . . .
O9 O 0.6193(3) 1.1460(2) -0.43886(19) 0.0189(7) Uani 1 1 d . . . . .
C35 C 0.1045(3) 0.8346(2) -0.24284(16) 0.0179(6) Uani 1 1 d . . . . .
C36 C 0.2440(3) 0.9166(2) -0.29637(16) 0.0171(6) Uani 1 1 d . . . . .
C37 C 0.2523(3) 0.9536(2) -0.38020(16) 0.0191(6) Uani 1 1 d . . . . .
H37 H 0.1601(7) 0.9258(5) -0.4091(4) 0.0355(14) Uani 1 1 d . . . . .
C38 C 0.3683(3) 0.9572(2) -0.26274(16) 0.0183(6) Uani 1 1 d . . . . .
H38 H 0.3686(7) 0.9318(5) -0.1986(3) 0.0364(14) Uani 1 1 d . . . . .
C39 C 0.4951(3) 1.0330(2) -0.31162(16) 0.0188(6) Uani 1 1 d . . . . .
H39 H 0.5952(8) 1.0710(5) -0.2914(4) 0.0370(14) Uani 1 1 d . . . . .
C40 C 0.3809(3) 1.0295(2) -0.42813(16) 0.0181(6) Uani 1 1 d . . . . .
H40 H 0.3934(7) 1.0599(5) -0.4926(4) 0.0342(13) Uani 1 1 d . . . . .
O1W O 0.2056(5) 0.9785(3) 0.4252(2) 0.0220(7) Uani 1 1 d . . . . .
H1A H 0.0993(8) 0.9413(5) 0.4394(4) 0.0357(14) Uani 1 1 d . . . . .
H1B H 0.2474(8) 0.9229(6) 0.4324(4) 0.0385(14) Uani 1 1 d . . . . .
O2W O 0.2470(5) 1.1159(3) 0.2719(2) 0.0235(8) Uani 1 1 d . . . . .
H2A H 0.2356(7) 1.0688(5) 0.3269(4) 0.0351(13) Uani 1 1 d . . . . .
H2B H 0.1638(9) 1.1348(6) 0.2725(4) 0.0365(14) Uani 1 1 d . . . . .
O3W O 0.3961(4) 0.6963(3) 0.3570(2) 0.0238(7) Uani 1 1 d . . . . .
H3A H 0.4843(9) 0.7257(5) 0.3204(4) 0.0362(14) Uani 1 1 d . . . . .
H3B H 0.3867(7) 0.7478(6) 0.3852(4) 0.0352(13) Uani 1 1 d . . . . .
O4W O 0.2791(5) 0.8014(3) -0.0527(2) 0.0231(7) Uani 1 1 d . . . . .
H4A H 0.2276(8) 0.8038(6) -0.0983(4) 0.0399(15) Uani 1 1 d . . . . .
H4B H 0.3754(9) 0.8097(6) -0.0744(5) 0.0410(15) Uani 1 1 d . . . . .
O5W O 1.4343(4) 1.1587(3) 0.1282(3) 0.0276(8) Uani 1 1 d . . . . .
H5A H 1.3655(7) 1.1322(5) 0.0940(4) 0.0345(13) Uani 1 1 d . . . . .
H5B H 1.3789(8) 1.1431(6) 0.1796(4) 0.0405(15) Uani 1 1 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 1.935(3) . ?
Fe1 N3 1.936(3) . ?
Fe1 N4 1.966(3) . ?
Fe1 N7 1.983(3) . ?
Fe1 N2 1.991(3) . ?
Fe1 N9 2.000(3) . ?
N1 N2 1.341(3) . ?
N1 C1 1.349(3) . ?
N1 H1N 1.034(7) . ?
N2 C3 1.352(3) . ?
N3 C8 1.347(3) . ?
N3 C4 1.351(3) . ?
N4 N5 1.344(3) . ?
N4 C9 1.353(4) . ?
N5 C11 1.357(4) . ?
N5 H5N 1.011(7) . ?
N6 N7 1.339(3) . ?
N6 C12 1.348(3) . ?
N6 H6N 1.045(6) . ?
N7 C14 1.352(3) . ?
N8 C19 1.347(3) . ?
N8 C15 1.351(3) . ?
N9 N10 1.342(3) . ?
N9 C20 1.355(3) . ?
N10 C22 1.359(4) . ?
N10 H10N 1.035(6) . ?
C1 C2 1.392(4) . ?
C1 H1 1.060(7) . ?
C2 C3 1.407(4) . ?
C2 H2 1.075(6) . ?
C3 C4 1.451(4) . ?
C4 C5 1.388(4) . ?
C5 C6 1.397(4) . ?
C5 H5 1.086(6) . ?
C6 C7 1.405(4) . ?
C6 H6 1.071(7) . ?
C7 C8 1.387(4) . ?
C7 H7 1.079(7) . ?
C8 C9 1.447(4) . ?
C9 C10 1.407(4) . ?
C10 C11 1.388(4) . ?
C10 H10 1.064(7) . ?
C11 H11 1.057(6) . ?
C12 C13 1.382(4) . ?
C12 H12 1.067(7) . ?
C13 C14 1.398(4) . ?
C13 H13 1.071(6) . ?
C14 C15 1.450(4) . ?
C15 C16 1.382(4) . ?
C16 C17 1.398(4) . ?
C16 H16 1.092(6) . ?
C17 C18 1.388(4) . ?
C17 H17 1.069(6) . ?
C18 C19 1.398(4) . ?
C18 H18 1.089(6) . ?
C19 C20 1.441(4) . ?
C20 C21 1.409(4) . ?
C21 C22 1.383(4) . ?
C21 H21 1.064(7) . ?
C22 H22 1.071(6) . ?
N11 O3 1.297(4) . ?
N11 C28 1.359(4) . ?
N11 C27 1.360(4) . ?
O1 C23 1.286(4) . ?
O1 H1O 1.237(7) . ?
O2 C23 1.243(4) . ?
C23 C24 1.486(4) . ?
C24 C26 1.387(4) . ?
C24 C25 1.393(4) . ?
C25 C28 1.388(4) . ?
C25 H25 1.092(6) . ?
C26 C27 1.380(4) . ?
C26 H26 1.074(6) . ?
C27 H27 1.091(6) . ?
C28 H28 1.087(7) . ?
N12 O6 1.303(4) . ?
N12 C33 1.362(3) . ?
N12 C34 1.363(3) . ?
O4 C29 1.243(4) . ?
O5 C29 1.290(4) . ?
O5 H1O 1.184(7) . ?
C29 C30 1.495(4) . ?
C30 C31 1.390(4) . ?
C30 C32 1.394(4) . ?
C31 C34 1.371(4) . ?
C31 H31 1.082(6) . ?
C32 C33 1.376(4) . ?
C32 H32 1.078(6) . ?
C33 H33 1.084(6) . ?
C34 H34 1.076(6) . ?
N13 O9 1.326(4) . ?
N13 C40 1.353(3) . ?
N13 C39 1.362(3) . ?
O7 C35 1.248(4) . ?
O8 C35 1.271(4) . ?
C35 C36 1.510(4) . ?
C36 C37 1.392(4) . ?
C36 C38 1.393(4) . ?
C37 C40 1.384(4) . ?
C37 H37 1.068(7) . ?
C38 C39 1.379(4) . ?
C38 H38 1.071(6) . ?
C39 H39 1.074(7) . ?
C40 H40 1.065(6) . ?
O1W H1A 0.985(10) . ?
O1W H1B 0.969(11) . ?
O2W H2A 0.981(8) . ?
O2W H2B 0.950(13) . ?
O3W H3A 0.941(10) . ?
O3W H3B 0.960(9) . ?
O4W H4A 0.965(10) . ?
O4W H4B 0.962(12) . ?
O5W H5A 0.963(9) . ?
O5W H5B 0.941(10) . ?

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 172.47(13) . . ?
N8 Fe1 N4 93.69(11) . . ?
N3 Fe1 N4 79.32(11) . . ?
N8 Fe1 N7 79.29(10) . . ?
N3 Fe1 N7 98.32(12) . . ?
N4 Fe1 N7 94.39(11) . . ?
N8 Fe1 N2 108.42(12) . . ?
N3 Fe1 N2 78.54(10) . . ?
N4 Fe1 N2 157.86(13) . . ?
N7 Fe1 N2 88.58(10) . . ?
N8 Fe1 N9 78.71(10) . . ?
N3 Fe1 N9 103.99(11) . . ?
N4 Fe1 N9 90.85(10) . . ?
N7 Fe1 N9 157.66(13) . . ?
N2 Fe1 N9 94.69(11) . . ?
N2 N1 C1 111.3(2) . . ?
N2 N1 H1N 120.1(4) . . ?
C1 N1 H1N 127.9(4) . . ?
N1 N2 C3 106.31(19) . . ?
N1 N2 Fe1 137.15(16) . . ?
C3 N2 Fe1 116.25(17) . . ?
C8 N3 C4 120.5(2) . . ?
C8 N3 Fe1 119.17(17) . . ?
C4 N3 Fe1 120.11(17) . . ?
N5 N4 C9 106.4(2) . . ?
N5 N4 Fe1 137.65(17) . . ?
C9 N4 Fe1 115.97(17) . . ?
N4 N5 C11 111.3(2) . . ?
N4 N5 H5N 123.7(4) . . ?
C11 N5 H5N 124.9(4) . . ?
N7 N6 C12 111.4(2) . . ?
N7 N6 H6N 122.0(4) . . ?
C12 N6 H6N 126.4(4) . . ?
N6 N7 C14 105.62(19) . . ?
N6 N7 Fe1 137.75(16) . . ?
C14 N7 Fe1 115.32(18) . . ?
C19 N8 C15 120.6(2) . . ?
C19 N8 Fe1 119.50(17) . . ?
C15 N8 Fe1 119.20(18) . . ?
N10 N9 C20 106.36(19) . . ?
N10 N9 Fe1 138.72(16) . . ?
C20 N9 Fe1 114.91(16) . . ?
N9 N10 C22 111.1(2) . . ?
N9 N10 H10N 121.3(4) . . ?
C22 N10 H10N 127.3(4) . . ?
N1 C1 C2 107.8(2) . . ?
N1 C1 H1 121.0(4) . . ?
C2 C1 H1 131.1(4) . . ?
C1 C2 C3 104.4(2) . . ?
C1 C2 H2 127.7(4) . . ?
C3 C2 H2 127.9(4) . . ?
N2 C3 C2 110.2(2) . . ?
N2 C3 C4 114.1(2) . . ?
C2 C3 C4 135.6(2) . . ?
N3 C4 C5 121.2(2) . . ?
N3 C4 C3 111.0(2) . . ?
C5 C4 C3 127.8(2) . . ?
C4 C5 C6 118.7(3) . . ?
C4 C5 H5 119.8(4) . . ?
C6 C5 H5 121.5(4) . . ?
C5 C6 C7 119.9(3) . . ?
C5 C6 H6 120.5(4) . . ?
C7 C6 H6 119.7(4) . . ?
C8 C7 C6 118.0(3) . . ?
C8 C7 H7 121.2(4) . . ?
C6 C7 H7 120.8(4) . . ?
N3 C8 C7 121.8(2) . . ?
N3 C8 C9 111.1(2) . . ?
C7 C8 C9 127.2(2) . . ?
N4 C9 C10 109.9(2) . . ?
N4 C9 C8 114.4(2) . . ?
C10 C9 C8 135.8(3) . . ?
C11 C10 C9 105.1(2) . . ?
C11 C10 H10 127.3(4) . . ?
C9 C10 H10 127.6(4) . . ?
N5 C11 C10 107.3(2) . . ?
N5 C11 H11 120.1(4) . . ?
C10 C11 H11 132.6(5) . . ?
N6 C12 C13 108.0(2) . . ?
N6 C12 H12 122.2(4) . . ?
C13 C12 H12 129.8(4) . . ?
C12 C13 C14 104.3(2) . . ?
C12 C13 H13 126.5(4) . . ?
C14 C13 H13 129.2(4) . . ?
N7 C14 C13 110.8(2) . . ?
N7 C14 C15 114.4(2) . . ?
C13 C14 C15 134.8(2) . . ?
N8 C15 C16 121.4(2) . . ?
N8 C15 C14 110.7(2) . . ?
C16 C15 C14 127.8(2) . . ?
C15 C16 C17 118.6(2) . . ?
C15 C16 H16 120.2(4) . . ?
C17 C16 H16 121.2(4) . . ?
C18 C17 C16 119.8(2) . . ?
C18 C17 H17 119.1(4) . . ?
C16 C17 H17 121.2(4) . . ?
C17 C18 C19 118.8(2) . . ?
C17 C18 H18 121.0(4) . . ?
C19 C18 H18 120.1(4) . . ?
N8 C19 C18 120.8(2) . . ?
N8 C19 C20 111.0(2) . . ?
C18 C19 C20 128.2(2) . . ?
N9 C20 C21 110.0(2) . . ?
N9 C20 C19 114.9(2) . . ?
C21 C20 C19 135.0(3) . . ?
C22 C21 C20 104.8(3) . . ?
C22 C21 H21 128.1(4) . . ?
C20 C21 H21 127.0(4) . . ?
N10 C22 C21 107.7(2) . . ?
N10 C22 H22 121.0(4) . . ?
C21 C22 H22 131.2(5) . . ?
O3 N11 C28 119.6(2) . . ?
O3 N11 C27 119.9(2) . . ?
C28 N11 C27 120.5(2) . . ?
C23 O1 H1O 114.7(4) . . ?
O2 C23 O1 126.6(3) . . ?
O2 C23 C24 118.7(3) . . ?
O1 C23 C24 114.6(3) . . ?
C26 C24 C25 118.8(3) . . ?
C26 C24 C23 119.9(2) . . ?
C25 C24 C23 121.2(2) . . ?
C28 C25 C24 119.8(2) . . ?
C28 C25 H25 119.2(4) . . ?
C24 C25 H25 120.9(4) . . ?
C27 C26 C24 120.0(3) . . ?
C27 C26 H26 119.2(4) . . ?
C24 C26 H26 120.8(4) . . ?
N11 C27 C26 120.6(2) . . ?
N11 C27 H27 114.5(4) . . ?
C26 C27 H27 124.9(4) . . ?
N11 C28 C25 120.2(2) . . ?
N11 C28 H28 114.7(4) . . ?
C25 C28 H28 125.0(4) . . ?
O6 N12 C33 120.3(2) . . ?
O6 N12 C34 119.5(2) . . ?
C33 N12 C34 120.2(2) . . ?
C29 O5 H1O 116.1(4) . . ?
O4 C29 O5 126.3(3) . . ?
O4 C29 C30 120.0(3) . . ?
O5 C29 C30 113.7(3) . . ?
C31 C30 C32 118.0(2) . . ?
C31 C30 C29 120.9(2) . . ?
C32 C30 C29 121.1(2) . . ?
C34 C31 C30 120.4(3) . . ?
C34 C31 H31 119.0(4) . . ?
C30 C31 H31 120.6(4) . . ?
C33 C32 C30 120.6(2) . . ?
C33 C32 H32 119.1(4) . . ?
C30 C32 H32 120.3(4) . . ?
N12 C33 C32 120.1(2) . . ?
N12 C33 H33 115.4(4) . . ?
C32 C33 H33 124.4(4) . . ?
N12 C34 C31 120.7(2) . . ?
N12 C34 H34 115.1(4) . . ?
C31 C34 H34 124.2(4) . . ?
O9 N13 C40 119.7(2) . . ?
O9 N13 C39 119.0(2) . . ?
C40 N13 C39 121.3(2) . . ?
O7 C35 O8 125.1(3) . . ?
O7 C35 C36 117.9(3) . . ?
O8 C35 C36 117.0(3) . . ?
C37 C36 C38 118.3(2) . . ?
C37 C36 C35 121.2(2) . . ?
C38 C36 C35 120.6(2) . . ?
C40 C37 C36 120.3(3) . . ?
C40 C37 H37 118.3(4) . . ?
C36 C37 H37 121.4(4) . . ?
C39 C38 C36 120.4(2) . . ?
C39 C38 H38 117.8(4) . . ?
C36 C38 H38 121.7(4) . . ?
N13 C39 C38 119.8(3) . . ?
N13 C39 H39 114.1(4) . . ?
C38 C39 H39 126.1(4) . . ?
N13 C40 C37 119.9(2) . . ?
N13 C40 H40 116.7(4) . . ?
C37 C40 H40 123.3(4) . . ?
H1A O1W H1B 108.0(6) . . ?
H2A O2W H2B 104.6(7) . . ?
H3A O3W H3B 111.3(6) . . ?
H4A O4W H4B 105.9(7) . . ?
H5A O5W H5B 105.6(7) . . ?

_refine_diff_density_max         1.633
_refine_diff_density_min         -1.329
_refine_diff_density_rms         0.277


_exptl_crystal_recrystallization_method 
'Re-crystallisation from solvent: MeOH/H2O'
_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_Fe_bpp_Noxid_NHoxid_Neutrons_95K
_database_code_depnum_ccdc_archive 'CCDC 1984959'
loop_
_audit_author_name
_audit_author_address
'Veronica Jornet Molla'
;University of Valencia
Spain
;
_audit_update_record             
;
2020-02-21 deposited with the CCDC.	2020-11-23 downloaded from the CCDC.
;
# start Validation Reply Form
_vrf_PLAT029_Fe_bpp_Noxid_NHoxid_Neutrons_95K 
;
PROBLEM: _diffrn_measured_fraction_theta_full value Low .      0.853 Why?
RESPONSE: The wavelength used for this experiment is 1.45510  \%A. Therefore, the number of collected reflections is low and this results in a low value of measured fraction theta full.
;
_vrf_PLAT088_Fe_bpp_Noxid_NHoxid_Neutrons_95K 
;
PROBLEM: Poor Data / Parameter Ratio ....................       6.52 Note
RESPONSE: The wavelength used for this experiment is  1.45510 \%A. Therefore, the number of collected reflections is low and not enough to yield a data/parameter ratio of 10.
;
_vrf_PLAT911_Fe_bpp_Noxid_NHoxid_Neutrons_95K 
;
PROBLEM: Missing FCF Refl Between Thmin & STh/L=    0.600        956 Report
RESPONSE: Some reflections are missing due to the restrictions of the experiment. The sample was placed on a close-circuit displex device on the monochromatic four-circle diffractometer D19 at ILL (Grenoble, France). The measurement strategy consisted on 25 omega (\w) scans with steps of 0.07\% at different \c and \f positions. These omega scans cover either 79\% or 64\% depending on the \c angle, in order to avoid collisions with the sample environment. Absorption correction removes reflections due to the environment provided by the neutron setup.
;
_vrf_PLAT155_Fe_bpp_Noxid_NHoxid_Neutrons_95K 
;
PROBLEM: The Triclinic Unitcell is NOT Reduced ..........     Please Do !
RESPONSE: The structural transition that takes place at low temperatures causes an increase in the gamma angle, changing from an acute angle (at higher temperatures) to an obtuse value, resulting in a non-reduced set of cell parameters. The non-reduced unit cell was preferred in order to facilitate comparisons with the crystal structure solutions at higher temperatures.
;
_vrf_PLAT303_Fe_bpp_Noxid_NHoxid_Neutrons_95K 
;
PROBLEM: Full Occupancy Atom H1O       with # Connections       2.00 Check
RESPONSE: This hydrogen atom is located between two oxygen atoms that belong to different carboxylate groups, forming a very strong hydrogen bond (the distance between the heteroatoms, O5 and O1, is 2.420 \%A). As a proton-transfer reaction is observed between the two carboxylate anions, different H...O distances are observed at different temperatures. Such a type of proton-transfer reaction is common when strong hydrogen bonds are established (see, for example Angew. Chem. Int. Ed. 2002, 41, 48-76).
;
# Added during the CSD deposition process: Friday 21 February 2020 08:20 PM
# end Validation Reply Form


_audit_creation_method           SHELXL-2018/3
_shelx_SHELXL_version_number     2018/3
_chemical_name_systematic        ?
_chemical_name_common            ?
_chemical_melting_point          ?
_chemical_formula_moiety         
'C22 H18 Fe N10 2+, C12 H9 N2 O6 1-, C6 H4 N O3 1-, 5(H2 O)'
_chemical_formula_sum            'C40 H41 Fe N13 O14'
_chemical_formula_weight         983.71

loop_
_atom_type_symbol
_atom_type_description
_atom_type_scat_dispersion_real
_atom_type_scat_dispersion_imag
_atom_type_scat_source
C C 0.0000 0.0000
'Neutron Data Booklet, ILL Grenoble, France (2003) ISBN 0-9704143-7-4'
H H 0.0000 0.0000
'Neutron Data Booklet, ILL Grenoble, France (2003) ISBN 0-9704143-7-4'
N N 0.0000 0.0000
'Neutron Data Booklet, ILL Grenoble, France (2003) ISBN 0-9704143-7-4'
O O 0.0000 0.0000
'Neutron Data Booklet, ILL Grenoble, France (2003) ISBN 0-9704143-7-4'
Fe Fe 0.0000 0.0000
'Neutron Data Booklet, ILL Grenoble, France (2003) ISBN 0-9704143-7-4'

_space_group_crystal_system      triclinic
_space_group_IT_number           2
_space_group_name_H-M_alt        'P -1'
_space_group_name_Hall           '-P 1'

_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'

_cell_length_a                   9.9677(4)
_cell_length_b                   13.5502(5)
_cell_length_c                   17.0822(5)
_cell_angle_alpha                76.876(2)
_cell_angle_beta                 85.729(2)
_cell_angle_gamma                110.376(2)
_cell_volume                     2076.34(13)
_cell_formula_units_Z            2
_cell_measurement_temperature    95(1)
_cell_measurement_reflns_used    3410
_cell_measurement_theta_min      5.329
_cell_measurement_theta_max      60.021

_exptl_crystal_description       cube
_exptl_crystal_colour            dark-red
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    ?
_exptl_crystal_density_diffrn    1.573
_exptl_crystal_F_000             650
_exptl_transmission_factor_min   ?
_exptl_transmission_factor_max   ?
_exptl_crystal_size_max          1.85
_exptl_crystal_size_mid          1.50
_exptl_crystal_size_min          0.7
_exptl_absorpt_coefficient_mu    0.194
_shelx_estimated_absorpt_T_min   ?
_shelx_estimated_absorpt_T_max   ?
_exptl_absorpt_correction_type   numerical
_exptl_absorpt_correction_T_min  ?
_exptl_absorpt_correction_T_max  ?
_exptl_absorpt_process_details   
; 
Absorption corretion done through d19face, d19abs and d19abscan 
programs from ILL
;
_diffrn_ambient_temperature      95(1)
_diffrn_radiation_wavelength     1.45510
_diffrn_radiation_type           neutrons
_diffrn_source                   'neutron source'
_diffrn_source_type              'ILL High Flux Reactor, beam H11'
_diffrn_source_power             57MW
_diffrn_measurement_device_type  
'D19 position-sensitive detector diffractometer'
_diffrn_radiation_monochromator  'copper 220'
_diffrn_measurement_method       'omega step-scans'
_diffrn_detector_area_resol_mean '1.56 mm vert. 2.5 mm hor.'
_diffrn_reflns_number            12460
_diffrn_reflns_av_unetI/netI     0.0319
_diffrn_reflns_av_R_equivalents  0.0417
_diffrn_reflns_limit_h_min       -10
_diffrn_reflns_limit_h_max       2
_diffrn_reflns_limit_k_min       -15
_diffrn_reflns_limit_k_max       16
_diffrn_reflns_limit_l_min       -20
_diffrn_reflns_limit_l_max       20
_diffrn_reflns_theta_min         4.530
_diffrn_reflns_theta_max         60.800
_diffrn_reflns_theta_full        60.800
_diffrn_measured_fraction_theta_max 0.853
_diffrn_measured_fraction_theta_full 0.853
_diffrn_reflns_Laue_measured_fraction_max 0.853
_diffrn_reflns_Laue_measured_fraction_full 0.853
_diffrn_reflns_point_group_measured_fraction_max 0.853
_diffrn_reflns_point_group_measured_fraction_full 0.853
_reflns_number_total             6404
_reflns_number_gt                5881
_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       'The NOMAD software from ILL '
_computing_cell_refinement       'PFIND and DIRAX programs'
_computing_data_reduction        'RETREAT and RAFD19 programs'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1997)'
_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)+(0.0860P)²+13.1541P] where P=(Fo²+2Fc²)/3'
_atom_sites_solution_primary     difmap
_atom_sites_solution_secondary   difmap
_atom_sites_solution_hydrogens   difmap
_refine_ls_hydrogen_treatment    refall
_refine_ls_extinction_method     none
_refine_ls_extinction_coef       .
_refine_ls_number_reflns         6404
_refine_ls_number_parameters     982
_refine_ls_number_restraints     0
_refine_ls_R_factor_all          0.0571
_refine_ls_R_factor_gt           0.0523
_refine_ls_wR_factor_ref         0.1400
_refine_ls_wR_factor_gt          0.1358
_refine_ls_goodness_of_fit_ref   1.133
_refine_ls_restrained_S_all      1.133
_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
Fe1 Fe 0.08315(16) 0.54669(11) 0.22439(8) 0.0137(3) Uani 1 1 d . . . . .
N1 N 0.17780(18) 0.50550(13) 0.39448(9) 0.0186(3) Uani 1 1 d . . . . .
H1N H 0.2734(5) 0.5759(4) 0.3770(3) 0.0299(10) Uani 1 1 d . . . . .
N2 N 0.08852(17) 0.48266(12) 0.34094(9) 0.0173(3) Uani 1 1 d . . . . .
N3 N -0.10560(17) 0.42920(12) 0.25787(9) 0.0169(3) Uani 1 1 d . . . . .
N4 N 0.00353(18) 0.56470(12) 0.12247(9) 0.0177(3) Uani 1 1 d . . . . .
N5 N 0.0473(2) 0.63005(14) 0.04625(9) 0.0197(4) Uani 1 1 d . . . . .
H5N H 0.1492(6) 0.6882(4) 0.0251(3) 0.0321(11) Uani 1 1 d . . . . .
N6 N -0.07320(19) 0.66604(14) 0.30858(9) 0.0195(3) Uani 1 1 d . . . . .
H6N H -0.1733(6) 0.6031(4) 0.3286(3) 0.0312(10) Uani 1 1 d . . . . .
N7 N 0.03185(18) 0.66150(12) 0.25782(9) 0.0170(3) Uani 1 1 d . . . . .
N8 N 0.26109(17) 0.67277(12) 0.17996(9) 0.0161(3) Uani 1 1 d . . . . .
N9 N 0.21030(17) 0.47912(12) 0.18029(9) 0.0158(3) Uani 1 1 d . . . . .
N10 N 0.20533(18) 0.37991(13) 0.17886(9) 0.0187(3) Uani 1 1 d . . . . .
H10N H 0.1204(6) 0.3088(4) 0.2126(3) 0.0312(10) Uani 1 1 d . . . . .
C1 C 0.1176(3) 0.43785(18) 0.46986(14) 0.0202(5) Uani 1 1 d . . . . .
H1 H 0.1767(6) 0.4471(5) 0.5196(3) 0.0408(12) Uani 1 1 d . . . . .
C2 C -0.0181(3) 0.36650(18) 0.46529(13) 0.0203(5) Uani 1 1 d . . . . .
H2 H -0.0956(6) 0.3033(4) 0.5139(3) 0.0360(11) Uani 1 1 d . . . . .
C3 C -0.0319(2) 0.39803(17) 0.38325(13) 0.0175(5) Uani 1 1 d . . . . .
C4 C -0.1472(2) 0.36588(17) 0.33575(13) 0.0168(4) Uani 1 1 d . . . . .
C5 C -0.2859(3) 0.28699(18) 0.36261(14) 0.0205(5) Uani 1 1 d . . . . .
H5 H -0.3177(6) 0.2391(4) 0.4255(3) 0.0380(12) Uani 1 1 d . . . . .
C6 C -0.3819(3) 0.27279(18) 0.30727(15) 0.0221(5) Uani 1 1 d . . . . .
H6 H -0.4905(6) 0.2122(4) 0.3259(3) 0.0398(12) Uani 1 1 d . . . . .
C7 C -0.3384(3) 0.33858(19) 0.22673(14) 0.0215(5) Uani 1 1 d . . . . .
H7 H -0.4122(6) 0.3283(4) 0.1835(3) 0.0383(12) Uani 1 1 d . . . . .
C8 C -0.1992(2) 0.41675(18) 0.20425(13) 0.0173(5) Uani 1 1 d . . . . .
C9 C -0.1326(3) 0.49513(18) 0.12568(13) 0.0180(5) Uani 1 1 d . . . . .
C10 C -0.1765(3) 0.5173(2) 0.04906(14) 0.0218(5) Uani 1 1 d . . . . .
H10 H -0.2762(7) 0.4764(5) 0.0316(3) 0.0437(13) Uani 1 1 d . . . . .
C11 C -0.0581(3) 0.6040(2) 0.00028(14) 0.0229(5) Uani 1 1 d . . . . .
H11 H -0.0387(6) 0.6493(5) -0.0624(3) 0.0391(12) Uani 1 1 d . . . . .
C12 C -0.0360(3) 0.76609(19) 0.32120(14) 0.0213(5) Uani 1 1 d . . . . .
H12 H -0.1059(6) 0.7870(5) 0.3586(3) 0.0413(13) Uani 1 1 d . . . . .
C13 C 0.1019(3) 0.83074(18) 0.27692(13) 0.0189(5) Uani 1 1 d . . . . .
H13 H 0.1612(6) 0.9143(4) 0.2732(3) 0.0348(11) Uani 1 1 d . . . . .
C14 C 0.1391(2) 0.76089(17) 0.23828(12) 0.0164(4) Uani 1 1 d . . . . .
C15 C 0.2670(2) 0.77152(17) 0.18592(12) 0.0157(4) Uani 1 1 d . . . . .
C16 C 0.3824(3) 0.86693(18) 0.14349(13) 0.0185(5) Uani 1 1 d . . . . .
H16 H 0.3830(6) 0.9461(4) 0.1476(3) 0.0354(11) Uani 1 1 d . . . . .
C17 C 0.4941(3) 0.85813(17) 0.09567(13) 0.0193(5) Uani 1 1 d . . . . .
H17 H 0.5852(6) 0.9299(4) 0.0609(3) 0.0369(12) Uani 1 1 d . . . . .
C18 C 0.4882(2) 0.75606(18) 0.08994(13) 0.0182(5) Uani 1 1 d . . . . .
H18 H 0.5755(5) 0.7482(4) 0.0531(3) 0.0311(10) Uani 1 1 d . . . . .
C19 C 0.3691(2) 0.66411(17) 0.13347(12) 0.0158(4) Uani 1 1 d . . . . .
C20 C 0.3405(2) 0.55104(17) 0.13639(12) 0.0157(4) Uani 1 1 d . . . . .
C21 C 0.4193(3) 0.49552(18) 0.10686(14) 0.0197(5) Uani 1 1 d . . . . .
H21 H 0.5248(6) 0.5299(4) 0.0722(3) 0.0373(11) Uani 1 1 d . . . . .
C22 C 0.3295(3) 0.38607(18) 0.13586(13) 0.0201(5) Uani 1 1 d . . . . .
H22 H 0.3443(6) 0.3136(4) 0.1297(4) 0.0397(12) Uani 1 1 d . . . . .
N11 N 1.11824(18) 1.00911(14) 0.06947(10) 0.0224(4) Uani 1 1 d . . . . .
O1 O 0.6926(3) 0.6680(2) 0.19162(16) 0.0216(6) Uani 1 1 d . . . . .
O2 O 0.6561(3) 0.7836(2) 0.25836(17) 0.0254(6) Uani 1 1 d . . . . .
O3 O 1.2422(3) 1.0842(2) 0.03091(17) 0.0285(6) Uani 1 1 d . . . . .
C23 C 0.7238(2) 0.76181(18) 0.20572(13) 0.0196(5) Uani 1 1 d . . . . .
C24 C 0.8573(2) 0.84912(18) 0.15370(13) 0.0185(5) Uani 1 1 d . . . . .
C25 C 0.9472(3) 0.82630(19) 0.10056(14) 0.0207(5) Uani 1 1 d . . . . .
H25 H 0.9177(6) 0.7457(4) 0.0929(3) 0.0385(12) Uani 1 1 d . . . . .
C26 C 0.8987(3) 0.95556(18) 0.16101(14) 0.0211(5) Uani 1 1 d . . . . .
H26 H 0.8302(6) 0.9757(4) 0.2009(3) 0.0419(13) Uani 1 1 d . . . . .
C27 C 1.0288(3) 1.03429(19) 0.11834(14) 0.0233(5) Uani 1 1 d . . . . .
H27 H 1.0694(6) 1.1185(4) 0.1196(4) 0.0438(13) Uani 1 1 d . . . . .
C28 C 1.0783(3) 0.90704(19) 0.05915(14) 0.0220(5) Uani 1 1 d . . . . .
H28 H 1.1557(6) 0.8948(5) 0.0185(3) 0.0415(12) Uani 1 1 d . . . . .
N12 N 0.19895(18) 0.19066(13) 0.50893(9) 0.0183(3) Uani 1 1 d . . . . .
O4 O 0.6555(3) 0.5127(2) 0.37811(16) 0.0222(6) Uani 1 1 d . . . . .
O5 O 0.5032(3) 0.5136(2) 0.28742(16) 0.0246(6) Uani 1 1 d . . . . .
H1O H 0.5968(6) 0.5927(4) 0.2420(3) 0.0383(12) Uani 1 1 d . . . . .
O6 O 0.0940(3) 0.1061(2) 0.55736(16) 0.0229(6) Uani 1 1 d . . . . .
C29 C 0.5381(3) 0.47526(18) 0.35477(13) 0.0193(5) Uani 1 1 d . . . . .
C30 C 0.4201(2) 0.37458(17) 0.40898(13) 0.0174(5) Uani 1 1 d . . . . .
C31 C 0.4269(3) 0.33687(18) 0.49056(13) 0.0185(5) Uani 1 1 d . . . . .
H31 H 0.5195(5) 0.3786(4) 0.5167(3) 0.0352(11) Uani 1 1 d . . . . .
C32 C 0.3003(3) 0.31655(18) 0.37865(13) 0.0202(5) Uani 1 1 d . . . . .
H32 H 0.2907(6) 0.3427(4) 0.3152(3) 0.0352(11) Uani 1 1 d . . . . .
C33 C 0.1913(3) 0.22496(19) 0.42870(13) 0.0203(5) Uani 1 1 d . . . . .
H33 H 0.0958(6) 0.1760(4) 0.4084(3) 0.0379(12) Uani 1 1 d . . . . .
C34 C 0.3163(3) 0.24554(18) 0.53965(13) 0.0192(5) Uani 1 1 d . . . . .
H34 H 0.3131(6) 0.2120(4) 0.6039(3) 0.0348(11) Uani 1 1 d . . . . .
N13 N 0.49878(18) 1.06853(13) -0.39305(10) 0.0197(3) Uani 1 1 d . . . . .
O7 O 0.1067(3) 0.7973(2) -0.16908(16) 0.0243(6) Uani 1 1 d . . . . .
O8 O -0.0074(3) 0.8085(2) -0.27586(16) 0.0227(6) Uani 1 1 d . . . . .
O9 O 0.6187(3) 1.1453(2) -0.43833(16) 0.0226(6) Uani 1 1 d . . . . .
C35 C 0.1044(2) 0.83435(17) -0.24281(13) 0.0186(5) Uani 1 1 d . . . . .
C36 C 0.2437(2) 0.91641(17) -0.29582(13) 0.0173(5) Uani 1 1 d . . . . .
C37 C 0.2517(3) 0.95388(17) -0.37951(13) 0.0191(5) Uani 1 1 d . . . . .
H37 H 0.1580(6) 0.9261(5) -0.4087(3) 0.0395(12) Uani 1 1 d . . . . .
C38 C 0.3680(3) 0.95674(19) -0.26267(14) 0.0207(5) Uani 1 1 d . . . . .
H38 H 0.3694(6) 0.9311(5) -0.1986(3) 0.0401(12) Uani 1 1 d . . . . .
C39 C 0.4943(3) 1.03241(19) -0.31164(14) 0.0209(5) Uani 1 1 d . . . . .
H39 H 0.5954(6) 1.0701(5) -0.2907(3) 0.0438(13) Uani 1 1 d . . . . .
C40 C 0.3807(3) 1.02952(18) -0.42762(13) 0.0191(5) Uani 1 1 d . . . . .
H40 H 0.3924(6) 1.0614(4) -0.4923(3) 0.0353(11) Uani 1 1 d . . . . .
O1W O 0.2055(4) 0.9789(3) 0.42515(17) 0.0238(6) Uani 1 1 d . . . . .
H1A H 0.1029(8) 0.9424(5) 0.4397(3) 0.0361(11) Uani 1 1 d . . . . .
H1B H 0.2474(6) 0.9231(5) 0.4319(3) 0.0362(11) Uani 1 1 d . . . . .
O2W O 0.2479(4) 1.1161(3) 0.27201(19) 0.0261(6) Uani 1 1 d . . . . .
H2A H 0.2369(6) 1.0697(5) 0.3263(4) 0.0375(11) Uani 1 1 d . . . . .
H2B H 0.1633(8) 1.1354(5) 0.2721(3) 0.0416(12) Uani 1 1 d . . . . .
O3W O 0.3959(4) 0.6965(2) 0.35700(19) 0.0256(6) Uani 1 1 d . . . . .
H3B H 0.3864(6) 0.7490(4) 0.3853(3) 0.0366(11) Uani 1 1 d . . . . .
H3A H 0.4861(7) 0.7257(5) 0.3201(3) 0.0408(12) Uani 1 1 d . . . . .
O4W O 0.2786(5) 0.7999(3) -0.05259(19) 0.0296(7) Uani 1 1 d . . . . .
H4A H 0.2280(7) 0.8021(5) -0.0983(4) 0.0422(12) Uani 1 1 d . . . . .
H4B H 0.3758(8) 0.8095(5) -0.0739(4) 0.0431(13) Uani 1 1 d . . . . .
O5W O 1.4345(4) 1.1578(3) 0.1281(2) 0.0337(7) Uani 1 1 d . . . . .
H5A H 1.3649(6) 1.1315(5) 0.0939(3) 0.0388(12) Uani 1 1 d . . . . .
H5B H 1.3790(7) 1.1434(5) 0.1803(4) 0.0448(13) Uani 1 1 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 1.934(2) . ?
Fe1 N3 1.934(2) . ?
Fe1 N4 1.967(2) . ?
Fe1 N7 1.980(2) . ?
Fe1 N2 1.996(2) . ?
Fe1 N9 1.998(2) . ?
N1 N2 1.335(2) . ?
N1 C1 1.351(3) . ?
N1 H1N 1.050(5) . ?
N2 C3 1.347(3) . ?
N3 C8 1.351(3) . ?
N3 C4 1.353(3) . ?
N4 N5 1.339(2) . ?
N4 C9 1.345(3) . ?
N5 C11 1.355(3) . ?
N5 H5N 1.021(6) . ?
N6 N7 1.336(2) . ?
N6 C12 1.348(3) . ?
N6 H6N 1.031(6) . ?
N7 C14 1.344(3) . ?
N8 C19 1.344(3) . ?
N8 C15 1.346(3) . ?
N9 N10 1.334(2) . ?
N9 C20 1.356(3) . ?
N10 C22 1.357(3) . ?
N10 H10N 1.042(5) . ?
C1 C2 1.382(3) . ?
C1 H1 1.075(5) . ?
C2 C3 1.401(3) . ?
C2 H2 1.068(5) . ?
C3 C4 1.455(3) . ?
C4 C5 1.385(3) . ?
C5 C6 1.391(3) . ?
C5 H5 1.080(6) . ?
C6 C7 1.400(3) . ?
C6 H6 1.076(6) . ?
C7 C8 1.381(3) . ?
C7 H7 1.079(6) . ?
C8 C9 1.449(3) . ?
C9 C10 1.412(3) . ?
C10 C11 1.382(3) . ?
C10 H10 1.059(7) . ?
C11 H11 1.072(6) . ?
C12 C13 1.391(3) . ?
C12 H12 1.061(6) . ?
C13 C14 1.400(3) . ?
C13 H13 1.063(5) . ?
C14 C15 1.446(3) . ?
C15 C16 1.391(3) . ?
C16 C17 1.386(3) . ?
C16 H16 1.088(5) . ?
C17 C18 1.390(3) . ?
C17 H17 1.079(5) . ?
C18 C19 1.390(3) . ?
C18 H18 1.086(5) . ?
C19 C20 1.446(3) . ?
C20 C21 1.401(3) . ?
C21 C22 1.386(3) . ?
C21 H21 1.056(6) . ?
C22 H22 1.069(6) . ?
N11 O3 1.302(3) . ?
N11 C27 1.356(3) . ?
N11 C28 1.357(3) . ?
O1 C23 1.282(4) . ?
O1 O2 2.243(4) . ?
O1 C24 2.335(3) . ?
O1 O5 2.420(4) . ?
O1 C25 2.751(4) . ?
O1 H1O 1.222(6) . ?
O2 C23 1.233(4) . ?
C23 C24 1.487(3) . ?
C24 C25 1.386(3) . ?
C24 C26 1.393(3) . ?
C25 C28 1.385(3) . ?
C25 H25 1.069(5) . ?
C26 C27 1.376(3) . ?
C26 H26 1.072(6) . ?
C27 H27 1.076(6) . ?
C28 H28 1.081(6) . ?
N12 O6 1.303(3) . ?
N12 C33 1.361(3) . ?
N12 C34 1.364(3) . ?
O4 C29 1.238(4) . ?
O4 O5 2.249(4) . ?
O5 C29 1.276(4) . ?
O5 C30 2.330(3) . ?
O5 C32 2.744(3) . ?
O5 H1O 1.200(6) . ?
C29 C30 1.500(3) . ?
C30 C31 1.386(3) . ?
C30 C32 1.391(3) . ?
C31 C34 1.375(3) . ?
C31 H31 1.088(5) . ?
C32 C33 1.376(3) . ?
C32 H32 1.083(5) . ?
C33 H33 1.086(5) . ?
C34 H34 1.082(5) . ?
N13 O9 1.319(3) . ?
N13 C40 1.351(3) . ?
N13 C39 1.357(3) . ?
O7 C35 1.251(4) . ?
O8 C35 1.263(4) . ?
C35 C36 1.504(3) . ?
C36 C38 1.389(3) . ?
C36 C37 1.390(3) . ?
C37 C40 1.386(3) . ?
C37 H37 1.082(6) . ?
C38 C39 1.375(3) . ?
C38 H38 1.073(5) . ?
C39 H39 1.087(6) . ?
C40 H40 1.072(5) . ?
O1W H1A 0.953(10) . ?
O1W H1B 0.973(9) . ?
O2W H2A 0.969(8) . ?
O2W H2B 0.966(10) . ?
O3W H3B 0.972(7) . ?
O3W H3A 0.957(8) . ?
O4W H4A 0.962(9) . ?
O4W H4B 0.962(10) . ?
O5W H5A 0.966(8) . ?
O5W H5B 0.953(8) . ?

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 172.61(11) . . ?
N8 Fe1 N4 93.77(9) . . ?
N3 Fe1 N4 79.40(9) . . ?
N8 Fe1 N7 79.18(8) . . ?
N3 Fe1 N7 98.39(9) . . ?
N4 Fe1 N7 94.21(9) . . ?
N8 Fe1 N2 108.31(9) . . ?
N3 Fe1 N2 78.47(8) . . ?
N4 Fe1 N2 157.87(11) . . ?
N7 Fe1 N2 88.64(8) . . ?
N8 Fe1 N9 78.64(8) . . ?
N3 Fe1 N9 104.11(9) . . ?
N4 Fe1 N9 91.14(8) . . ?
N7 Fe1 N9 157.47(10) . . ?
N2 Fe1 N9 94.58(9) . . ?
N2 N1 C1 111.24(17) . . ?
N2 N1 H1N 119.6(3) . . ?
C1 N1 H1N 128.5(3) . . ?
N1 N2 C3 106.11(15) . . ?
N1 N2 Fe1 137.31(13) . . ?
C3 N2 Fe1 116.33(14) . . ?
C8 N3 C4 120.48(18) . . ?
C8 N3 Fe1 119.07(14) . . ?
C4 N3 Fe1 120.25(14) . . ?
N5 N4 C9 106.58(16) . . ?
N5 N4 Fe1 137.53(14) . . ?
C9 N4 Fe1 115.89(14) . . ?
N4 N5 C11 111.05(18) . . ?
N4 N5 H5N 123.9(3) . . ?
C11 N5 H5N 124.9(3) . . ?
N7 N6 C12 110.99(17) . . ?
N7 N6 H6N 122.7(3) . . ?
C12 N6 H6N 125.9(3) . . ?
N6 N7 C14 106.22(16) . . ?
N6 N7 Fe1 137.18(13) . . ?
C14 N7 Fe1 115.21(14) . . ?
C19 N8 C15 120.28(17) . . ?
C19 N8 Fe1 119.77(14) . . ?
C15 N8 Fe1 119.23(14) . . ?
N10 N9 C20 106.31(15) . . ?
N10 N9 Fe1 138.62(13) . . ?
C20 N9 Fe1 115.04(13) . . ?
N9 N10 C22 111.02(16) . . ?
N9 N10 H10N 122.2(3) . . ?
C22 N10 H10N 126.5(3) . . ?
N1 C1 C2 107.81(19) . . ?
N1 C1 H1 119.7(4) . . ?
C2 C1 H1 132.5(4) . . ?
C1 C2 C3 104.3(2) . . ?
C1 C2 H2 127.5(4) . . ?
C3 C2 H2 128.1(4) . . ?
N2 C3 C2 110.49(19) . . ?
N2 C3 C4 114.15(18) . . ?
C2 C3 C4 135.2(2) . . ?
N3 C4 C5 121.2(2) . . ?
N3 C4 C3 110.77(18) . . ?
C5 C4 C3 128.0(2) . . ?
C4 C5 C6 118.5(2) . . ?
C4 C5 H5 119.8(4) . . ?
C6 C5 H5 121.6(4) . . ?
C5 C6 C7 120.1(2) . . ?
C5 C6 H6 120.6(4) . . ?
C7 C6 H6 119.3(4) . . ?
C8 C7 C6 118.4(2) . . ?
C8 C7 H7 121.0(4) . . ?
C6 C7 H7 120.6(4) . . ?
N3 C8 C7 121.3(2) . . ?
N3 C8 C9 110.76(19) . . ?
C7 C8 C9 127.9(2) . . ?
N4 C9 C10 110.06(19) . . ?
N4 C9 C8 114.79(19) . . ?
C10 C9 C8 135.1(2) . . ?
C11 C10 C9 104.5(2) . . ?
C11 C10 H10 127.0(4) . . ?
C9 C10 H10 128.5(4) . . ?
N5 C11 C10 107.79(19) . . ?
N5 C11 H11 119.7(4) . . ?
C10 C11 H11 132.6(4) . . ?
N6 C12 C13 108.2(2) . . ?
N6 C12 H12 122.7(4) . . ?
C13 C12 H12 129.2(4) . . ?
C12 C13 C14 103.7(2) . . ?
C12 C13 H13 126.7(4) . . ?
C14 C13 H13 129.6(4) . . ?
N7 C14 C13 110.92(19) . . ?
N7 C14 C15 114.83(18) . . ?
C13 C14 C15 134.2(2) . . ?
N8 C15 C16 121.47(19) . . ?
N8 C15 C14 110.53(17) . . ?
C16 C15 C14 128.0(2) . . ?
C17 C16 C15 118.3(2) . . ?
C17 C16 H16 121.5(3) . . ?
C15 C16 H16 120.2(3) . . ?
C16 C17 C18 120.2(2) . . ?
C16 C17 H17 121.0(4) . . ?
C18 C17 H17 118.8(4) . . ?
C19 C18 C17 118.5(2) . . ?
C19 C18 H18 120.7(3) . . ?
C17 C18 H18 120.7(3) . . ?
N8 C19 C18 121.24(19) . . ?
N8 C19 C20 110.83(18) . . ?
C18 C19 C20 127.9(2) . . ?
N9 C20 C21 110.39(18) . . ?
N9 C20 C19 114.72(18) . . ?
C21 C20 C19 134.8(2) . . ?
C22 C21 C20 104.3(2) . . ?
C22 C21 H21 128.3(4) . . ?
C20 C21 H21 127.3(3) . . ?
N10 C22 C21 107.9(2) . . ?
N10 C22 H22 120.7(4) . . ?
C21 C22 H22 131.3(4) . . ?
O3 N11 C27 119.6(2) . . ?
O3 N11 C28 119.8(2) . . ?
C27 N11 C28 120.55(19) . . ?
C23 O1 O2 26.35(14) . . ?
C23 O1 C24 35.34(14) . . ?
O2 O1 C24 61.68(11) . . ?
C23 O1 O5 117.4(2) . . ?
O2 O1 O5 91.34(13) . . ?
C24 O1 O5 151.73(15) . . ?
C23 O1 C25 65.50(16) . . ?
O2 O1 C25 91.77(12) . . ?
C24 O1 C25 30.24(8) . . ?
O5 O1 C25 167.61(15) . . ?
C23 O1 H1O 114.9(3) . . ?
O2 O1 H1O 88.8(3) . . ?
C24 O1 H1O 149.2(3) . . ?
O5 O1 H1O 2.6(3) . . ?
C25 O1 H1O 167.5(3) . . ?
C23 O2 O1 27.48(15) . . ?
O2 C23 O1 126.2(3) . . ?
O2 C23 C24 119.1(2) . . ?
O1 C23 C24 114.7(2) . . ?
C25 C24 C26 118.5(2) . . ?
C25 C24 C23 121.5(2) . . ?
C26 C24 C23 119.9(2) . . ?
C25 C24 O1 91.73(16) . . ?
C26 C24 O1 149.79(18) . . ?
C23 C24 O1 29.92(12) . . ?
C28 C25 C24 120.1(2) . . ?
C28 C25 O1 176.48(18) . . ?
C24 C25 O1 58.02(13) . . ?
C28 C25 H25 119.6(4) . . ?
C24 C25 H25 120.3(4) . . ?
O1 C25 H25 62.2(3) . . ?
C27 C26 C24 120.0(2) . . ?
C27 C26 H26 120.0(4) . . ?
C24 C26 H26 120.0(4) . . ?
N11 C27 C26 120.6(2) . . ?
N11 C27 H27 114.1(4) . . ?
C26 C27 H27 125.3(4) . . ?
N11 C28 C25 120.2(2) . . ?
N11 C28 H28 115.4(4) . . ?
C25 C28 H28 124.4(4) . . ?
O6 N12 C33 120.58(19) . . ?
O6 N12 C34 119.31(19) . . ?
C33 N12 C34 120.11(18) . . ?
C29 O4 O5 26.98(14) . . ?
C29 O5 O4 26.12(14) . . ?
C29 O5 C30 36.07(14) . . ?
O4 O5 C30 62.19(11) . . ?
C29 O5 O1 116.3(2) . . ?
O4 O5 O1 90.22(13) . . ?
C30 O5 O1 152.14(15) . . ?
C29 O5 C32 66.09(16) . . ?
O4 O5 C32 92.06(12) . . ?
C30 O5 C32 30.45(8) . . ?
O1 O5 C32 169.56(15) . . ?
C29 O5 H1O 115.4(3) . . ?
O4 O5 H1O 89.2(3) . . ?
C30 O5 H1O 151.4(3) . . ?
O1 O5 H1O 2.6(3) . . ?
C32 O5 H1O 172.1(3) . . ?
O4 C29 O5 126.9(2) . . ?
O4 C29 C30 119.2(2) . . ?
O5 C29 C30 113.9(2) . . ?
C31 C30 C32 118.2(2) . . ?
C31 C30 C29 121.1(2) . . ?
C32 C30 C29 120.7(2) . . ?
C31 C30 O5 149.55(18) . . ?
C32 C30 O5 91.47(16) . . ?
C29 C30 O5 30.06(12) . . ?
C34 C31 C30 120.3(2) . . ?
C34 C31 H31 119.0(3) . . ?
C30 C31 H31 120.8(3) . . ?
C33 C32 C30 120.7(2) . . ?
C33 C32 O5 173.08(18) . . ?
C30 C32 O5 58.08(13) . . ?
C33 C32 H32 118.6(3) . . ?
C30 C32 H32 120.7(3) . . ?
O5 C32 H32 63.1(3) . . ?
N12 C33 C32 120.2(2) . . ?
N12 C33 H33 115.9(3) . . ?
C32 C33 H33 124.0(4) . . ?
N12 C34 C31 120.6(2) . . ?
N12 C34 H34 114.8(3) . . ?
C31 C34 H34 124.5(4) . . ?
O9 N13 C40 119.79(19) . . ?
O9 N13 C39 119.36(19) . . ?
C40 N13 C39 120.82(18) . . ?
O7 C35 O8 124.5(2) . . ?
O7 C35 C36 118.0(2) . . ?
O8 C35 C36 117.5(2) . . ?
C38 C36 C37 118.0(2) . . ?
C38 C36 C35 121.01(19) . . ?
C37 C36 C35 120.9(2) . . ?
C40 C37 C36 120.3(2) . . ?
C40 C37 H37 118.3(4) . . ?
C36 C37 H37 121.4(4) . . ?
C39 C38 C36 120.5(2) . . ?
C39 C38 H38 117.7(4) . . ?
C36 C38 H38 121.9(4) . . ?
N13 C39 C38 120.3(2) . . ?
N13 C39 H39 114.2(4) . . ?
C38 C39 H39 125.4(4) . . ?
N13 C40 C37 120.0(2) . . ?
N13 C40 H40 116.7(3) . . ?
C37 C40 H40 123.3(4) . . ?
H1A O1W H1B 107.5(5) . . ?
H2A O2W H2B 105.4(6) . . ?
H3B O3W H3A 111.4(6) . . ?
H4A O4W H4B 106.0(6) . . ?
H5A O5W H5B 105.8(6) . . ?

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 O3W 1.050(5) 1.604(6) 2.638(3) 166.9(5) . yes
N5 H5N O4W 1.021(6) 1.785(6) 2.724(4) 151.2(5) . yes
N6 H6N O4 1.031(6) 1.728(6) 2.744(3) 167.3(5) 1_455 yes
N10 H10N O8 1.042(5) 1.660(6) 2.691(3) 169.7(5) 2_565 yes
O1W H1B O9 0.973(9) 1.868(7) 2.809(5) 162.0(5) 2_675 yes
O1W H1A O6 0.953(10) 1.832(8) 2.765(5) 165.6(5) 2_566 yes
O2W H2A O1W 0.969(8) 1.781(7) 2.749(5) 176.3(5) . yes
O2W H2B O8 0.966(10) 1.957(8) 2.918(5) 172.6(6) 2_575 yes
O3W H3A O2 0.957(8) 1.741(7) 2.697(4) 175.8(6) . yes
O3W H3B O9 0.972(7) 1.873(6) 2.844(4) 176.2(5) 2_675 yes
O4W H4A O7 0.962(9) 1.768(7) 2.719(5) 169.8(6) . yes
O4W H4B O5W 0.962(10) 1.898(8) 2.854(6) 172.4(6) 2_775 yes
O5W H5B O2W 0.953(8) 1.843(7) 2.788(5) 170.9(6) 1_655 yes
O5W H5A O3 0.966(8) 1.740(7) 2.706(5) 178.9(6) . yes

_refine_diff_density_max         0.927
_refine_diff_density_min         -1.004
_refine_diff_density_rms         0.202


_exptl_crystal_recrystallization_method 
'Re-crystallisation from solvent: MeOH/H2O'
_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_Fe_bpp_Noxid_NHoxid_Neutrons_240K
_database_code_depnum_ccdc_archive 'CCDC 1984961'
loop_
_audit_author_name
_audit_author_address
'Veronica Jornet Molla'
;University of Valencia
Spain
;
_audit_update_record             
;
2020-02-21 deposited with the CCDC.	2020-11-23 downloaded from the CCDC.
;
# start Validation Reply Form
_vrf_PLAT029_Fe_bpp_Noxid_NHoxid_Neutrons_240K 
;
PROBLEM: _diffrn_measured_fraction_theta_full value Low .      0.852 Why?
RESPONSE: The wavelength used for this experiment is 1.45510  \%A. Therefore, the number of collected reflections is low and this results in a low value of measured fraction theta full.
;
_vrf_PLAT088_Fe_bpp_Noxid_NHoxid_Neutrons_240K 
;
PROBLEM: Poor Data / Parameter Ratio ....................       6.66 Note
RESPONSE: The wavelength used for this experiment is  1.45510 \%A. Therefore, the number of collected reflections is low and not enough to yield a data/parameter ratio of 10.
;
_vrf_PLAT911_Fe_bpp_Noxid_NHoxid_Neutrons_240K 
;
PROBLEM: Missing FCF Refl Between Thmin & STh/L=    0.600        988 Report
RESPONSE: Some reflections are missing due to the restrictions of the experiment. The sample was placed on a close-circuit displex device on the monochromatic four-circle diffractometer D19 at ILL (Grenoble, France). The measurement strategy consisted on 25 omega (\w) scans with steps of 0.07\% at different \c and \f positions. These omega scans cover either 79\% or 64\% depending on the \c angle, in order to avoid collisions with the sample environment. Absorption correction removes reflections due to the environment provided by the neutron setup.
;
_vrf_PLAT303_Fe_bpp_Noxid_NHoxid_Neutrons_240K 
;
PROBLEM: Full Occupancy Atom H1O       with # Connections       2.00 Check
RESPONSE: This hydrogen atom is located between two oxygen atoms that belong to different carboxylate groups, forming a very strong hydrogen bond (the distance between the heteroatoms, O5 and O1, is 2.407 \%A). As a proton-transfer reaction is observed between the two carboxylate anions, different H...O distances are observed at different temperatures. Such a type of proton-transfer reaction is common when strong hydrogen bonds are established (see, for example Angew. Chem. Int. Ed. 2002, 41, 48-76).
;
# Added during the CSD deposition process: Friday 21 February 2020 08:29 PM
# end Validation Reply Form


_audit_creation_method           SHELXL-2018/3
_shelx_SHELXL_version_number     2018/3
_chemical_name_systematic        ?
_chemical_name_common            ?
_chemical_melting_point          ?
_chemical_formula_moiety         
'C22 H18 Fe N10 2+, C12 H9 N2 O6 1-, C6 H4 N O3 1-, 5(H2 O)'
_chemical_formula_sum            'C40 H41 Fe N13 O14'
_chemical_formula_weight         983.71

loop_
_atom_type_symbol
_atom_type_description
_atom_type_scat_dispersion_real
_atom_type_scat_dispersion_imag
_atom_type_scat_source
C C 0.0000 0.0000
'Neutron Data Booklet, ILL Grenoble, France (2003) ISBN 0-9704143-7-4'
H H 0.0000 0.0000
'Neutron Data Booklet, ILL Grenoble, France (2003) ISBN 0-9704143-7-4'
Fe Fe 0.0000 0.0000
'Neutron Data Booklet, ILL Grenoble, France (2003) ISBN 0-9704143-7-4'
O O 0.0000 0.0000
'Neutron Data Booklet, ILL Grenoble, France (2003) ISBN 0-9704143-7-4'
N N 0.0000 0.0000
'Neutron Data Booklet, ILL Grenoble, France (2003) ISBN 0-9704143-7-4'

_space_group_crystal_system      triclinic
_space_group_IT_number           2
_space_group_name_H-M_alt        'P -1'
_space_group_name_Hall           '-P 1'

_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'

_cell_length_a                   9.9726(3)
_cell_length_b                   13.6198(4)
_cell_length_c                   17.4815(5)
_cell_angle_alpha                73.5194(17)
_cell_angle_beta                 85.7393(18)
_cell_angle_gamma                69.1085(18)
_cell_volume                     2126.23(11)
_cell_formula_units_Z            2
_cell_measurement_temperature    240(1)
_cell_measurement_reflns_used    3662
_cell_measurement_theta_min      5.312
_cell_measurement_theta_max      60.124

_exptl_crystal_description       cube
_exptl_crystal_colour            light-red
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    ?
_exptl_crystal_density_diffrn    1.536
_exptl_crystal_F_000             650
_exptl_transmission_factor_min   ?
_exptl_transmission_factor_max   ?
_exptl_crystal_size_max          1.85
_exptl_crystal_size_mid          1.50
_exptl_crystal_size_min          0.7
_exptl_absorpt_coefficient_mu    0.190
_shelx_estimated_absorpt_T_min   ?
_shelx_estimated_absorpt_T_max   ?
_exptl_absorpt_correction_type   numerical
_exptl_absorpt_correction_T_min  ?
_exptl_absorpt_correction_T_max  ?
_exptl_absorpt_process_details   
; 
Absorption corretion done through d19face, d19abs and d19abscan 
programs from ILL
;
_diffrn_ambient_temperature      240(1)
_diffrn_radiation_wavelength     1.45510
_diffrn_radiation_type           neutrons
_diffrn_source                   'neutron source'
_diffrn_source_type              'ILL High Flux Reactor, beam H11'
_diffrn_source_power             57MW
_diffrn_measurement_device_type  
'D19 position-sensitive detector diffractometer'
_diffrn_radiation_monochromator  'copper 220'
_diffrn_measurement_method       'omega step-scans'
_diffrn_detector_area_resol_mean '1.56 mm vert. 2.5 mm hor.'
_diffrn_reflns_number            12723
_diffrn_reflns_av_unetI/netI     0.0362
_diffrn_reflns_av_R_equivalents  0.0473
_diffrn_reflns_limit_h_min       -10
_diffrn_reflns_limit_h_max       2
_diffrn_reflns_limit_k_min       -16
_diffrn_reflns_limit_k_max       16
_diffrn_reflns_limit_l_min       -20
_diffrn_reflns_limit_l_max       20
_diffrn_reflns_theta_min         4.481
_diffrn_reflns_theta_max         60.773
_diffrn_reflns_theta_full        60.773
_diffrn_measured_fraction_theta_max 0.851
_diffrn_measured_fraction_theta_full 0.852
_diffrn_reflns_Laue_measured_fraction_max 0.851
_diffrn_reflns_Laue_measured_fraction_full 0.852
_diffrn_reflns_point_group_measured_fraction_max 0.851
_diffrn_reflns_point_group_measured_fraction_full 0.852
_reflns_number_total             6543
_reflns_number_gt                5783
_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       'The NOMAD software from ILL '
_computing_cell_refinement       'PFIND and DIRAX programs'
_computing_data_reduction        'RETREAT and RAFD19 programs'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1997)'
_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)+(0.0660P)²+14.4346P] where P=(Fo²+2Fc²)/3'
_atom_sites_solution_primary     difmap
_atom_sites_solution_secondary   difmap
_atom_sites_solution_hydrogens   difmap
_refine_ls_hydrogen_treatment    refall
_refine_ls_extinction_method     none
_refine_ls_extinction_coef       .
_refine_ls_number_reflns         6543
_refine_ls_number_parameters     982
_refine_ls_number_restraints     0
_refine_ls_R_factor_all          0.0566
_refine_ls_R_factor_gt           0.0500
_refine_ls_wR_factor_ref         0.1336
_refine_ls_wR_factor_gt          0.1285
_refine_ls_goodness_of_fit_ref   1.120
_refine_ls_restrained_S_all      1.120
_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
Fe1 Fe 0.03334(17) 0.54400(11) 0.23265(8) 0.0255(3) Uani 1 1 d . . . . .
N1 N 0.1639(2) 0.49411(14) 0.41094(10) 0.0339(4) Uani 1 1 d . . . . .
H1N H 0.1911(6) 0.5629(5) 0.3948(3) 0.0482(12) Uani 1 1 d . . . . .
N2 N 0.09614(18) 0.47456(13) 0.35696(9) 0.0297(3) Uani 1 1 d . . . . .
N3 N -0.04422(18) 0.41251(13) 0.27300(9) 0.0295(3) Uani 1 1 d . . . . .
N4 N -0.07839(19) 0.54457(14) 0.12963(9) 0.0333(4) Uani 1 1 d . . . . .
N5 N -0.1054(2) 0.60014(16) 0.05255(10) 0.0388(4) Uani 1 1 d . . . . .
H5N H -0.0668(7) 0.6618(5) 0.0262(3) 0.0559(14) Uani 1 1 d . . . . .
N6 N -0.25884(19) 0.69040(15) 0.30785(9) 0.0327(4) Uani 1 1 d . . . . .
H6N H -0.2998(6) 0.6295(5) 0.3297(3) 0.0477(12) Uani 1 1 d . . . . .
N7 N -0.14595(18) 0.67725(12) 0.26004(9) 0.0285(3) Uani 1 1 d . . . . .
N8 N 0.08000(18) 0.68673(12) 0.17742(9) 0.0268(3) Uani 1 1 d . . . . .
N9 N 0.24140(18) 0.48850(12) 0.17918(9) 0.0288(3) Uani 1 1 d . . . . .
N10 N 0.34238(19) 0.39524(13) 0.17331(10) 0.0326(4) Uani 1 1 d . . . . .
H10N H 0.3330(6) 0.3208(4) 0.2054(3) 0.0470(12) Uani 1 1 d . . . . .
C1 C 0.1710(3) 0.4230(2) 0.48331(14) 0.0393(6) Uani 1 1 d . . . . .
H1 H 0.2200(8) 0.4292(6) 0.5329(3) 0.0666(16) Uani 1 1 d . . . . .
C2 C 0.1041(3) 0.3523(2) 0.47639(14) 0.0372(6) Uani 1 1 d . . . . .
H2 H 0.0892(8) 0.2869(5) 0.5225(3) 0.0627(15) Uani 1 1 d . . . . .
C3 C 0.0589(3) 0.38806(17) 0.39607(12) 0.0290(5) Uani 1 1 d . . . . .
C4 C -0.0241(3) 0.35426(17) 0.35010(13) 0.0288(5) Uani 1 1 d . . . . .
C5 C -0.0829(3) 0.27329(19) 0.38055(15) 0.0359(5) Uani 1 1 d . . . . .
H5 H -0.0668(7) 0.2273(5) 0.4426(3) 0.0572(14) Uani 1 1 d . . . . .
C6 C -0.1655(3) 0.2544(2) 0.32922(17) 0.0403(6) Uani 1 1 d . . . . .
H6 H -0.2133(8) 0.1933(5) 0.3508(4) 0.0647(16) Uani 1 1 d . . . . .
C7 C -0.1863(3) 0.3159(2) 0.24969(16) 0.0384(6) Uani 1 1 d . . . . .
H7 H -0.2508(8) 0.3029(5) 0.2095(4) 0.0658(16) Uani 1 1 d . . . . .
C8 C -0.1231(3) 0.39474(18) 0.22339(13) 0.0305(5) Uani 1 1 d . . . . .
C9 C -0.1368(3) 0.46700(19) 0.14244(13) 0.0321(5) Uani 1 1 d . . . . .
C10 C -0.2013(3) 0.4726(2) 0.07250(16) 0.0437(6) Uani 1 1 d . . . . .
H10 H -0.2554(8) 0.4220(7) 0.0624(5) 0.0751(19) Uani 1 1 d . . . . .
C11 C -0.1790(3) 0.5595(3) 0.01625(15) 0.0468(7) Uani 1 1 d . . . . .
H11 H -0.2061(8) 0.5945(7) -0.0467(3) 0.076(2) Uani 1 1 d . . . . .
C12 C -0.3142(3) 0.7936(2) 0.31402(15) 0.0369(6) Uani 1 1 d . . . . .
H12 H -0.4039(7) 0.8212(6) 0.3497(4) 0.0633(15) Uani 1 1 d . . . . .
C13 C -0.2337(3) 0.8513(2) 0.26771(14) 0.0347(5) Uani 1 1 d . . . . .
H13 H -0.2504(7) 0.9348(5) 0.2590(4) 0.0583(14) Uani 1 1 d . . . . .
C14 C -0.1300(2) 0.77494(17) 0.23544(12) 0.0270(4) Uani 1 1 d . . . . .
C15 C -0.0126(2) 0.78340(17) 0.18222(12) 0.0265(4) Uani 1 1 d . . . . .
C16 C 0.0041(3) 0.88130(18) 0.13882(14) 0.0327(5) Uani 1 1 d . . . . .
H16 H -0.0723(7) 0.9579(4) 0.1416(3) 0.0562(14) Uani 1 1 d . . . . .
C17 C 0.1234(3) 0.87526(19) 0.09117(14) 0.0357(5) Uani 1 1 d . . . . .
H17 H 0.1407(7) 0.9475(4) 0.0566(4) 0.0586(14) Uani 1 1 d . . . . .
C18 C 0.2200(3) 0.77422(18) 0.08709(13) 0.0318(5) Uani 1 1 d . . . . .
H18 H 0.3139(6) 0.7684(4) 0.0510(3) 0.0538(13) Uani 1 1 d . . . . .
C19 C 0.1947(2) 0.68030(17) 0.13135(12) 0.0259(4) Uani 1 1 d . . . . .
C20 C 0.2847(3) 0.56950(17) 0.13381(12) 0.0280(5) Uani 1 1 d . . . . .
C21 C 0.4157(3) 0.5255(2) 0.09878(15) 0.0357(5) Uani 1 1 d . . . . .
H21 H 0.4779(7) 0.5687(5) 0.0621(4) 0.0606(15) Uani 1 1 d . . . . .
C22 C 0.4490(3) 0.4132(2) 0.12601(15) 0.0369(5) Uani 1 1 d . . . . .
H22 H 0.5380(7) 0.3476(5) 0.1152(4) 0.0625(15) Uani 1 1 d . . . . .
N11 N -0.3969(2) 1.01286(16) 0.07097(10) 0.0401(4) Uani 1 1 d . . . . .
O1 O -0.4869(4) 0.6712(2) 0.19416(18) 0.0449(7) Uani 1 1 d . . . . .
H1O H -0.5032(7) 0.5953(5) 0.2443(4) 0.0615(15) Uani 1 1 d . . . . .
O2 O -0.6365(4) 0.7851(3) 0.25862(19) 0.0489(8) Uani 1 1 d . . . . .
O3 O -0.3447(5) 1.0880(3) 0.03354(19) 0.0575(10) Uani 1 1 d . . . . .
C23 C -0.5488(3) 0.76454(19) 0.20678(14) 0.0350(5) Uani 1 1 d . . . . .
C24 C -0.5020(3) 0.85316(18) 0.15444(13) 0.0320(5) Uani 1 1 d . . . . .
C25 C -0.3887(3) 0.8303(2) 0.10354(14) 0.0373(6) Uani 1 1 d . . . . .
H25 H -0.3391(7) 0.7492(5) 0.0975(4) 0.0634(15) Uani 1 1 d . . . . .
C26 C -0.5641(3) 0.9590(2) 0.16002(16) 0.0404(6) Uani 1 1 d . . . . .
H26 H -0.6515(8) 0.9787(5) 0.1980(4) 0.0704(18) Uani 1 1 d . . . . .
C27 C -0.5120(3) 1.0386(2) 0.11754(16) 0.0432(6) Uani 1 1 d . . . . .
H27 H -0.5533(9) 1.1219(5) 0.1188(5) 0.077(2) Uani 1 1 d . . . . .
C28 C -0.3370(3) 0.9108(2) 0.06246(14) 0.0388(6) Uani 1 1 d . . . . .
H28 H -0.2484(7) 0.8990(6) 0.0238(4) 0.0645(16) Uani 1 1 d . . . . .
N12 N -0.49474(19) 0.19022(14) 0.50868(10) 0.0330(4) Uani 1 1 d . . . . .
O4 O -0.3693(4) 0.5226(3) 0.37812(18) 0.0433(7) Uani 1 1 d . . . . .
O5 O -0.5151(4) 0.5145(3) 0.2907(2) 0.0551(9) Uani 1 1 d . . . . .
O6 O -0.5105(4) 0.1023(2) 0.55535(18) 0.0411(7) Uani 1 1 d . . . . .
C29 C -0.4456(3) 0.48049(19) 0.35712(14) 0.0349(5) Uani 1 1 d . . . . .
C30 C -0.4627(3) 0.37947(18) 0.41057(13) 0.0297(5) Uani 1 1 d . . . . .
C31 C -0.4168(3) 0.3410(2) 0.49003(13) 0.0336(5) Uani 1 1 d . . . . .
H31 H -0.3667(7) 0.3837(5) 0.5151(3) 0.0560(14) Uani 1 1 d . . . . .
C32 C -0.5254(3) 0.31993(19) 0.38197(13) 0.0335(5) Uani 1 1 d . . . . .
H32 H -0.5637(8) 0.3473(5) 0.3202(3) 0.0605(15) Uani 1 1 d . . . . .
C33 C -0.5394(3) 0.22549(19) 0.43102(14) 0.0349(5) Uani 1 1 d . . . . .
H33 H -0.5849(7) 0.1747(5) 0.4125(3) 0.0570(14) Uani 1 1 d . . . . .
C34 C -0.4334(3) 0.2470(2) 0.53789(14) 0.0345(5) Uani 1 1 d . . . . .
H34 H -0.4023(7) 0.2136(5) 0.5997(3) 0.0577(14) Uani 1 1 d . . . . .
N13 N 0.0698(2) 0.94445(14) 0.38160(10) 0.0350(4) Uani 1 1 d . . . . .
O7 O 0.1937(4) 1.2212(3) 0.16285(19) 0.0488(8) Uani 1 1 d . . . . .
O8 O 0.3238(4) 1.2049(3) 0.26579(19) 0.0444(7) Uani 1 1 d . . . . .
O9 O 0.0228(4) 0.8685(3) 0.42567(18) 0.0440(7) Uani 1 1 d . . . . .
C35 C 0.2347(3) 1.18187(19) 0.23389(14) 0.0352(5) Uani 1 1 d . . . . .
C36 C 0.1754(3) 1.09892(18) 0.28600(13) 0.0305(5) Uani 1 1 d . . . . .
C37 C 0.2085(3) 1.0577(2) 0.36718(15) 0.0371(6) Uani 1 1 d . . . . .
H37 H 0.2769(8) 1.0833(6) 0.3950(4) 0.0668(17) Uani 1 1 d . . . . .
C38 C 0.0861(3) 1.0608(2) 0.25464(14) 0.0386(6) Uani 1 1 d . . . . .
H38 H 0.0554(8) 1.0904(6) 0.1922(3) 0.0642(17) Uani 1 1 d . . . . .
C39 C 0.0349(3) 0.9832(2) 0.30276(15) 0.0409(6) Uani 1 1 d . . . . .
H39 H -0.0292(9) 0.9482(6) 0.2833(4) 0.0737(19) Uani 1 1 d . . . . .
C40 C 0.1541(3) 0.9809(2) 0.41453(15) 0.0373(6) Uani 1 1 d . . . . .
H40 H 0.1755(8) 0.9472(5) 0.4764(3) 0.0641(16) Uani 1 1 d . . . . .
O1W O 0.7276(6) 0.9925(3) 0.4206(2) 0.0473(8) Uani 1 1 d . . . . .
H1A H 0.6589(8) 0.9542(5) 0.4376(4) 0.0597(14) Uani 1 1 d . . . . .
H1B H 0.8190(9) 0.9387(6) 0.4248(4) 0.0589(14) Uani 1 1 d . . . . .
O2W O 0.6335(6) 0.1265(3) 0.2665(2) 0.0506(8) Uani 1 1 d . . . . .
H2A H 0.5300(9) 0.1475(6) 0.2659(4) 0.0600(15) Uani 1 1 d . . . . .
H2B H 0.6652(7) 0.0819(5) 0.3199(4) 0.0548(13) Uani 1 1 d . . . . .
O3W O 0.1967(5) 0.6903(3) 0.3634(2) 0.0507(8) Uani 1 1 d . . . . .
H3A H 0.2557(7) 0.7182(5) 0.3241(4) 0.0550(13) Uani 1 1 d . . . . .
H3B H 0.1347(7) 0.7483(5) 0.3833(4) 0.0565(13) Uani 1 1 d . . . . .
O4W O 0.0405(6) 0.2175(3) 0.0420(2) 0.0562(9) Uani 1 1 d . . . . .
H4A H -0.0480(10) 0.2094(6) 0.0592(5) 0.0713(18) Uani 1 1 d . . . . .
H4B H 0.0890(7) 0.2160(5) 0.0893(4) 0.0564(14) Uani 1 1 d . . . . .
O5W O -0.2222(5) 1.1717(4) 0.1213(3) 0.0660(11) Uani 1 1 d . . . . .
H5A H -0.2634(8) 1.1566(6) 0.1737(4) 0.0653(16) Uani 1 1 d . . . . .
H5B H -0.2664(7) 1.1436(5) 0.0904(4) 0.0583(14) Uani 1 1 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 2.107(2) . ?
Fe1 N3 2.120(2) . ?
Fe1 N2 2.150(2) . ?
Fe1 N9 2.178(2) . ?
Fe1 N4 2.184(2) . ?
Fe1 N7 2.184(2) . ?
N1 N2 1.335(2) . ?
N1 C1 1.347(3) . ?
N1 H1N 1.025(6) . ?
N2 C3 1.346(3) . ?
N3 C8 1.337(3) . ?
N3 C4 1.344(3) . ?
N4 C9 1.338(3) . ?
N4 N5 1.338(2) . ?
N5 C11 1.344(4) . ?
N5 H5N 1.024(7) . ?
N6 N7 1.341(2) . ?
N6 C12 1.348(3) . ?
N6 H6N 1.020(6) . ?
N7 C14 1.340(3) . ?
N8 C15 1.333(3) . ?
N8 C19 1.341(3) . ?
N9 N10 1.336(2) . ?
N9 C20 1.351(3) . ?
N10 C22 1.347(3) . ?
N10 H10N 1.043(5) . ?
C1 C2 1.386(4) . ?
C1 H1 1.064(6) . ?
C2 C3 1.400(3) . ?
C2 H2 1.065(6) . ?
C3 C4 1.457(3) . ?
C4 C5 1.388(3) . ?
C5 C6 1.394(4) . ?
C5 H5 1.078(6) . ?
C6 C7 1.392(4) . ?
C6 H6 1.067(6) . ?
C7 C8 1.385(3) . ?
C7 H7 1.076(7) . ?
C8 C9 1.460(3) . ?
C9 C10 1.394(3) . ?
C10 C11 1.383(4) . ?
C10 H10 1.070(7) . ?
C11 H11 1.079(6) . ?
C12 C13 1.383(4) . ?
C12 H12 1.068(7) . ?
C13 C14 1.396(3) . ?
C13 H13 1.055(6) . ?
C14 C15 1.457(3) . ?
C15 C16 1.395(3) . ?
C16 C17 1.392(4) . ?
C16 H16 1.062(7) . ?
C17 C18 1.388(3) . ?
C17 H17 1.064(6) . ?
C18 C19 1.392(3) . ?
C18 H18 1.081(6) . ?
C19 C20 1.445(3) . ?
C20 C21 1.404(3) . ?
C21 C22 1.388(4) . ?
C21 H21 1.063(6) . ?
C22 H22 1.062(7) . ?
N11 O3 1.303(4) . ?
N11 C28 1.350(3) . ?
N11 C27 1.356(3) . ?
O1 C23 1.275(4) . ?
O1 H1O 1.203(7) . ?
O2 C23 1.232(4) . ?
C23 C24 1.491(3) . ?
C24 C26 1.381(4) . ?
C24 C25 1.386(4) . ?
C25 C28 1.373(4) . ?
C25 H25 1.070(7) . ?
C26 C27 1.373(4) . ?
C26 H26 1.058(7) . ?
C27 H27 1.066(7) . ?
C28 H28 1.065(7) . ?
N12 O6 1.298(3) . ?
N12 C33 1.356(3) . ?
N12 C34 1.357(3) . ?
O4 C29 1.232(4) . ?
O5 C29 1.277(4) . ?
O5 H1O 1.206(7) . ?
C29 C30 1.486(3) . ?
C30 C31 1.387(3) . ?
C30 C32 1.391(3) . ?
C31 C34 1.375(3) . ?
C31 H31 1.079(6) . ?
C32 C33 1.376(3) . ?
C32 H32 1.088(6) . ?
C33 H33 1.078(6) . ?
C34 H34 1.069(6) . ?
N13 O9 1.312(3) . ?
N13 C40 1.347(3) . ?
N13 C39 1.352(3) . ?
O7 C35 1.240(4) . ?
O8 C35 1.254(4) . ?
C35 C36 1.506(3) . ?
C36 C37 1.387(3) . ?
C36 C38 1.388(4) . ?
C37 C40 1.386(4) . ?
C37 H37 1.066(7) . ?
C38 C39 1.380(4) . ?
C38 H38 1.076(5) . ?
C39 H39 1.045(8) . ?
C40 H40 1.054(6) . ?
O1W H1A 0.984(10) . ?
O1W H1B 0.935(12) . ?
O2W H2A 0.967(12) . ?
O2W H2B 0.962(9) . ?
O3W H3A 0.956(9) . ?
O3W H3B 0.949(10) . ?
O4W H4A 0.945(14) . ?
O4W H4B 0.981(9) . ?
O5W H5A 0.973(10) . ?
O5W H5B 0.952(10) . ?

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 169.79(10) . . ?
N8 Fe1 N2 114.52(9) . . ?
N3 Fe1 N2 74.50(7) . . ?
N8 Fe1 N9 74.56(7) . . ?
N3 Fe1 N9 109.50(9) . . ?
N2 Fe1 N9 99.95(9) . . ?
N8 Fe1 N4 96.41(8) . . ?
N3 Fe1 N4 74.35(8) . . ?
N2 Fe1 N4 148.82(9) . . ?
N9 Fe1 N4 91.74(8) . . ?
N8 Fe1 N7 74.80(7) . . ?
N3 Fe1 N7 101.08(9) . . ?
N2 Fe1 N7 90.77(8) . . ?
N9 Fe1 N7 149.29(9) . . ?
N4 Fe1 N7 93.71(9) . . ?
N2 N1 C1 111.59(19) . . ?
N2 N1 H1N 118.5(3) . . ?
C1 N1 H1N 129.4(3) . . ?
N1 N2 C3 105.96(16) . . ?
N1 N2 Fe1 137.52(13) . . ?
C3 N2 Fe1 116.51(14) . . ?
C8 N3 C4 120.75(18) . . ?
C8 N3 Fe1 119.62(14) . . ?
C4 N3 Fe1 119.36(14) . . ?
C9 N4 N5 106.05(17) . . ?
C9 N4 Fe1 115.44(14) . . ?
N5 N4 Fe1 138.49(15) . . ?
N4 N5 C11 111.2(2) . . ?
N4 N5 H5N 122.0(4) . . ?
C11 N5 H5N 126.7(4) . . ?
N7 N6 C12 111.40(18) . . ?
N7 N6 H6N 120.9(3) . . ?
C12 N6 H6N 127.3(4) . . ?
C14 N7 N6 105.64(16) . . ?
C14 N7 Fe1 114.22(14) . . ?
N6 N7 Fe1 138.63(13) . . ?
C15 N8 C19 120.75(17) . . ?
C15 N8 Fe1 119.47(14) . . ?
C19 N8 Fe1 119.44(13) . . ?
N10 N9 C20 105.86(16) . . ?
N10 N9 Fe1 139.35(13) . . ?
C20 N9 Fe1 114.68(14) . . ?
N9 N10 C22 111.95(17) . . ?
N9 N10 H10N 119.4(3) . . ?
C22 N10 H10N 128.6(4) . . ?
N1 C1 C2 107.5(2) . . ?
N1 C1 H1 120.4(5) . . ?
C2 C1 H1 132.0(4) . . ?
C1 C2 C3 104.4(2) . . ?
C1 C2 H2 127.3(4) . . ?
C3 C2 H2 128.4(4) . . ?
N2 C3 C2 110.5(2) . . ?
N2 C3 C4 116.29(18) . . ?
C2 C3 C4 133.1(2) . . ?
N3 C4 C5 121.3(2) . . ?
N3 C4 C3 113.24(18) . . ?
C5 C4 C3 125.4(2) . . ?
C4 C5 C6 118.3(2) . . ?
C4 C5 H5 120.8(4) . . ?
C6 C5 H5 120.9(4) . . ?
C7 C6 C5 119.7(2) . . ?
C7 C6 H6 120.0(5) . . ?
C5 C6 H6 120.3(5) . . ?
C8 C7 C6 118.7(2) . . ?
C8 C7 H7 120.7(4) . . ?
C6 C7 H7 120.6(4) . . ?
N3 C8 C7 121.2(2) . . ?
N3 C8 C9 113.49(19) . . ?
C7 C8 C9 125.3(2) . . ?
N4 C9 C10 110.7(2) . . ?
N4 C9 C8 116.94(19) . . ?
C10 C9 C8 132.3(2) . . ?
C11 C10 C9 104.4(2) . . ?
C11 C10 H10 126.3(5) . . ?
C9 C10 H10 129.3(5) . . ?
N5 C11 C10 107.7(2) . . ?
N5 C11 H11 119.8(5) . . ?
C10 C11 H11 132.5(5) . . ?
N6 C12 C13 107.6(2) . . ?
N6 C12 H12 123.5(4) . . ?
C13 C12 H12 128.9(4) . . ?
C12 C13 C14 104.4(2) . . ?
C12 C13 H13 126.5(4) . . ?
C14 C13 H13 129.2(4) . . ?
N7 C14 C13 111.02(19) . . ?
N7 C14 C15 117.05(18) . . ?
C13 C14 C15 131.9(2) . . ?
N8 C15 C16 121.7(2) . . ?
N8 C15 C14 113.33(17) . . ?
C16 C15 C14 124.9(2) . . ?
C17 C16 C15 117.8(2) . . ?
C17 C16 H16 121.2(4) . . ?
C15 C16 H16 121.0(4) . . ?
C18 C17 C16 120.0(2) . . ?
C18 C17 H17 119.2(4) . . ?
C16 C17 H17 120.8(4) . . ?
C17 C18 C19 118.7(2) . . ?
C17 C18 H18 120.7(4) . . ?
C19 C18 H18 120.6(4) . . ?
N8 C19 C18 120.9(2) . . ?
N8 C19 C20 113.55(17) . . ?
C18 C19 C20 125.5(2) . . ?
N9 C20 C21 110.26(19) . . ?
N9 C20 C19 117.10(19) . . ?
C21 C20 C19 132.6(2) . . ?
C22 C21 C20 104.6(2) . . ?
C22 C21 H21 127.8(4) . . ?
C20 C21 H21 127.5(4) . . ?
N10 C22 C21 107.3(2) . . ?
N10 C22 H22 121.5(4) . . ?
C21 C22 H22 131.2(4) . . ?
O3 N11 C28 119.8(3) . . ?
O3 N11 C27 119.4(3) . . ?
C28 N11 C27 120.8(2) . . ?
C23 O1 H1O 115.4(4) . . ?
O2 C23 O1 126.1(3) . . ?
O2 C23 C24 119.4(2) . . ?
O1 C23 C24 114.4(2) . . ?
C26 C24 C25 118.4(2) . . ?
C26 C24 C23 120.3(2) . . ?
C25 C24 C23 121.1(2) . . ?
C28 C25 C24 120.2(2) . . ?
C28 C25 H25 119.7(4) . . ?
C24 C25 H25 120.1(4) . . ?
C27 C26 C24 120.4(3) . . ?
C27 C26 H26 119.8(4) . . ?
C24 C26 H26 119.8(4) . . ?
N11 C27 C26 119.9(2) . . ?
N11 C27 H27 114.9(4) . . ?
C26 C27 H27 125.1(5) . . ?
N11 C28 C25 120.2(2) . . ?
N11 C28 H28 115.2(4) . . ?
C25 C28 H28 124.6(5) . . ?
O6 N12 C33 120.3(2) . . ?
O6 N12 C34 119.7(2) . . ?
C33 N12 C34 119.97(19) . . ?
C29 O5 H1O 116.1(4) . . ?
O4 C29 O5 126.3(3) . . ?
O4 C29 C30 120.5(2) . . ?
O5 C29 C30 113.3(2) . . ?
C31 C30 C32 117.8(2) . . ?
C31 C30 C29 121.6(2) . . ?
C32 C30 C29 120.6(2) . . ?
C34 C31 C30 120.2(2) . . ?
C34 C31 H31 119.0(4) . . ?
C30 C31 H31 120.7(4) . . ?
C33 C32 C30 120.8(2) . . ?
C33 C32 H32 118.9(4) . . ?
C30 C32 H32 120.4(4) . . ?
N12 C33 C32 120.3(2) . . ?
N12 C33 H33 115.1(4) . . ?
C32 C33 H33 124.6(4) . . ?
N12 C34 C31 121.0(2) . . ?
N12 C34 H34 114.9(4) . . ?
C31 C34 H34 124.2(4) . . ?
O9 N13 C40 120.2(2) . . ?
O9 N13 C39 118.9(2) . . ?
C40 N13 C39 120.9(2) . . ?
O7 C35 O8 124.8(3) . . ?
O7 C35 C36 118.1(2) . . ?
O8 C35 C36 117.0(2) . . ?
C37 C36 C38 117.6(2) . . ?
C37 C36 C35 121.1(2) . . ?
C38 C36 C35 121.3(2) . . ?
C40 C37 C36 120.6(2) . . ?
C40 C37 H37 118.0(4) . . ?
C36 C37 H37 121.4(4) . . ?
C39 C38 C36 120.7(2) . . ?
C39 C38 H38 118.1(4) . . ?
C36 C38 H38 121.2(4) . . ?
N13 C39 C38 120.1(2) . . ?
N13 C39 H39 114.6(4) . . ?
C38 C39 H39 125.3(4) . . ?
N13 C40 C37 120.0(2) . . ?
N13 C40 H40 116.3(4) . . ?
C37 C40 H40 123.7(4) . . ?
H1A O1W H1B 106.9(6) . . ?
H2A O2W H2B 105.5(7) . . ?
H3A O3W H3B 108.7(6) . . ?
H4A O4W H4B 106.4(7) . . ?
H5A O5W H5B 104.4(7) . . ?

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 O3W 1.025(6) 1.686(7) 2.695(4) 167.3(5) . yes
N5 H5N O4W 1.024(7) 1.828(7) 2.824(5) 163.2(5) 2_565 yes
N6 H6N O4 1.020(6) 1.802(6) 2.818(4) 174.3(5) . yes
N10 H10N O8 1.043(5) 1.661(6) 2.699(3) 173.3(5) 1_545 yes
O1 H1O O5 1.203(7) 1.206(7) 2.407(4) 175.1(7) . yes
O1W H1B O9 0.935(12) 1.912(9) 2.816(6) 161.9(6) 1_655 yes
O1W H1A O6 0.984(10) 1.877(8) 2.843(6) 166.1(6) 2_566 yes
O2W H2B O1W 0.962(9) 1.837(8) 2.799(6) 178.0(6) 1_545 yes
O2W H2A O8 0.967(12) 1.921(10) 2.885(6) 173.5(6) 1_545 yes
O3W H3A O2 0.956(9) 1.794(7) 2.743(5) 171.3(6) 1_655 yes
O3W H3B O9 0.949(10) 1.934(8) 2.881(6) 175.1(6) . yes
O4W H4B O7 0.981(9) 1.746(7) 2.719(6) 170.9(6) 1_545 yes
O4W H4A O5W 0.945(14) 2.122(11) 3.051(7) 167.7(7) 1_545 yes
O5W H5A O2W 0.973(10) 1.879(8) 2.845(6) 171.0(7) 1_465 yes
O5W H5B O3 0.952(10) 1.770(8) 2.722(6) 178.4(7) . yes

_refine_diff_density_max         0.661
_refine_diff_density_min         -0.913
_refine_diff_density_rms         0.166


_exptl_crystal_recrystallization_method 
'Re-crystallisation from solvent: MeOH/H2O'
_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_Fe_bpp_Noxid_NHoxid_PIHS_50K
_database_code_depnum_ccdc_archive 'CCDC 1984962'
loop_
_audit_author_name
_audit_author_address
'Veronica Jornet Molla'
;University of Valencia
Spain
;
_audit_update_record             
;
2020-02-18 deposited with the CCDC.	2020-11-23 downloaded from the CCDC.
;

_audit_creation_method           SHELXL-2018/3
_shelx_SHELXL_version_number     2018/3
_chemical_name_systematic        ?
_chemical_name_common            ?
_chemical_melting_point          ?
_chemical_formula_moiety         
'C22 H18 Fe N10 2+, C12 H9 N2 O6 1-, C6 H4 N O3 1-, 5(H2 O)'
_chemical_formula_sum            'C40 H41 Fe N13 O14'
_chemical_formula_weight         983.71

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      triclinic
_space_group_IT_number           2
_space_group_name_H-M_alt        'P -1'
_space_group_name_Hall           '-P 1'

_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'

_cell_length_a                   9.9402(13)
_cell_length_b                   13.5461(19)
_cell_length_c                   17.384(2)
_cell_angle_alpha                73.959(6)
_cell_angle_beta                 85.950(5)
_cell_angle_gamma                68.735(5)
_cell_volume                     2095.3(5)
_cell_formula_units_Z            2
_cell_measurement_temperature    50(1)
_cell_measurement_reflns_used    9899
_cell_measurement_theta_min      2.2010
_cell_measurement_theta_max      32.2789

_exptl_crystal_description       cube
_exptl_crystal_colour            light-red
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    ?
_exptl_crystal_density_diffrn    1.559
_exptl_crystal_F_000             1020
_exptl_transmission_factor_min   ?
_exptl_transmission_factor_max   ?
_exptl_crystal_size_max          0.494
_exptl_crystal_size_mid          0.166
_exptl_crystal_size_min          0.127
_exptl_absorpt_coefficient_mu    0.447
_shelx_estimated_absorpt_T_min   ?
_shelx_estimated_absorpt_T_max   ?
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_correction_T_min  0.6083
_exptl_absorpt_correction_T_max  0.7465
_exptl_absorpt_process_details   
;
 SADABS 2016/2: Krause, L., Herbst-Irmer, R., Sheldrick G.M. & Stalke D.,
 J. Appl. Cryst. 48 (2015) 3-10
;
_diffrn_ambient_temperature      50(1)
_diffrn_radiation_wavelength     0.71073
_diffrn_radiation_type           MoK\a
_diffrn_source                   'micro-focus sealed X-ray tube'
_diffrn_radiation_monochromator  mirror
_diffrn_measurement_device_type  
;
Bruker SMART X2S benchtop crystallographic system
;
_diffrn_measurement_method       'ω scans'
_diffrn_detector_area_resol_mean 16.0267
_diffrn_reflns_number            37908
_diffrn_reflns_av_unetI/netI     0.0852
_diffrn_reflns_av_R_equivalents  0.0573
_diffrn_reflns_limit_h_min       -15
_diffrn_reflns_limit_h_max       15
_diffrn_reflns_limit_k_min       -20
_diffrn_reflns_limit_k_max       20
_diffrn_reflns_limit_l_min       -25
_diffrn_reflns_limit_l_max       26
_diffrn_reflns_theta_min         2.200
_diffrn_reflns_theta_max         32.668
_diffrn_reflns_theta_full        25.242
_diffrn_measured_fraction_theta_max 0.974
_diffrn_measured_fraction_theta_full 0.998
_diffrn_reflns_Laue_measured_fraction_max 0.974
_diffrn_reflns_Laue_measured_fraction_full 0.998
_diffrn_reflns_point_group_measured_fraction_max 0.974
_diffrn_reflns_point_group_measured_fraction_full 0.998
_reflns_number_total             14987
_reflns_number_gt                10681
_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       
;
'APEX3 v2017.3-0 (Bruker AXS)'
;
_computing_cell_refinement       
;
'APEX3 v2017.3-0 (Bruker AXS)'
SAINT Version 8.32B (Bruker AXS Inc., 2013) 
;
_computing_data_reduction        
;
APEX3 Version 2017.3 (Bruker AXS Inc.) 
SAINT Version 8.32B (Bruker AXS Inc., 2013) 
;
_computing_structure_solution    'SHELXT 2018/2 (Sheldrick, 2018)'
_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)+(0.0420P)²+0.5189P] where P=(Fo²+2Fc²)/3'
_atom_sites_solution_primary     difmap
_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         14987
_refine_ls_number_parameters     662
_refine_ls_number_restraints     0
_refine_ls_R_factor_all          0.0803
_refine_ls_R_factor_gt           0.0460
_refine_ls_wR_factor_ref         0.1114
_refine_ls_wR_factor_gt          0.0999
_refine_ls_goodness_of_fit_ref   1.035
_refine_ls_restrained_S_all      1.035
_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 0.03528(2) 0.54278(2) 0.23332(2) 0.00557(5) Uani 1 1 d . . . . .
N1 N 0.16583(13) 0.49250(10) 0.41333(8) 0.0076(2) Uani 1 1 d . . . . .
H1N H 0.190(2) 0.5535(16) 0.3959(11) 0.011 Uiso 1 1 d . U . . .
N2 N 0.09751(13) 0.47277(10) 0.35848(7) 0.0070(2) Uani 1 1 d . . . . .
N3 N -0.04280(13) 0.41088(10) 0.27329(7) 0.0071(2) Uani 1 1 d . . . . .
N4 N -0.07711(14) 0.54353(10) 0.12920(7) 0.0082(2) Uani 1 1 d . . . . .
N5 N -0.10431(14) 0.59957(11) 0.05150(8) 0.0086(2) Uani 1 1 d . . . . .
H5N H -0.070(2) 0.6553(15) 0.0296(11) 0.013 Uiso 1 1 d . U . . .
N6 N -0.26287(14) 0.69290(11) 0.30726(8) 0.0077(2) Uani 1 1 d . . . . .
H6N H -0.295(2) 0.6454(15) 0.3263(11) 0.012 Uiso 1 1 d . U . . .
N7 N -0.14799(13) 0.67813(10) 0.25982(7) 0.0072(2) Uani 1 1 d . . . . .
N8 N 0.08005(13) 0.68681(10) 0.17729(7) 0.0061(2) Uani 1 1 d . . . . .
N9 N 0.24570(13) 0.48650(10) 0.17930(7) 0.0065(2) Uani 1 1 d . . . . .
N10 N 0.34906(14) 0.39197(10) 0.17337(8) 0.0077(2) Uani 1 1 d . . . . .
H10N H 0.341(2) 0.3285(16) 0.2008(11) 0.012 Uiso 1 1 d . U . . .
C1 C 0.17232(16) 0.42138(12) 0.48568(9) 0.0097(3) Uani 1 1 d . . . . .
H1 H 0.214076 0.420175 0.532310 0.012 Uiso 1 1 calc R U . . .
C2 C 0.10627(16) 0.35069(12) 0.47856(9) 0.0087(3) Uani 1 1 d . . . . .
H2 H 0.094767 0.292508 0.518305 0.010 Uiso 1 1 calc R U . . .
C3 C 0.06016(15) 0.38631(12) 0.39768(9) 0.0070(3) Uani 1 1 d . . . . .
C4 C -0.02405(16) 0.35231(12) 0.35088(9) 0.0070(3) Uani 1 1 d . . . . .
C5 C -0.08461(16) 0.27262(12) 0.38129(9) 0.0081(3) Uani 1 1 d . . . . .
H5 H -0.069896 0.232392 0.434804 0.010 Uiso 1 1 calc R U . . .
C6 C -0.16810(16) 0.25448(12) 0.32947(9) 0.0091(3) Uani 1 1 d . . . . .
H6 H -0.210261 0.201588 0.348262 0.011 Uiso 1 1 calc R U . . .
C7 C -0.18857(16) 0.31543(12) 0.24954(9) 0.0089(3) Uani 1 1 d . . . . .
H7 H -0.244566 0.304119 0.214532 0.011 Uiso 1 1 calc R U . . .
C8 C -0.12376(15) 0.39338(12) 0.22315(9) 0.0073(3) Uani 1 1 d . . . . .
C9 C -0.13682(16) 0.46620(12) 0.14143(9) 0.0075(3) Uani 1 1 d . . . . .
C10 C -0.20208(16) 0.47287(13) 0.07012(9) 0.0099(3) Uani 1 1 d . . . . .
H10 H -0.250190 0.428822 0.062239 0.012 Uiso 1 1 calc R U . . .
C11 C -0.17874(16) 0.55948(13) 0.01438(9) 0.0106(3) Uani 1 1 d . . . . .
H11 H -0.209036 0.585470 -0.039241 0.013 Uiso 1 1 calc R U . . .
C12 C -0.31963(16) 0.79737(12) 0.31275(9) 0.0088(3) Uani 1 1 d . . . . .
H12 H -0.399130 0.825801 0.342146 0.011 Uiso 1 1 calc R U . . .
C13 C -0.23891(16) 0.85428(12) 0.26712(9) 0.0085(3) Uani 1 1 d . . . . .
H13 H -0.251710 0.927909 0.259296 0.010 Uiso 1 1 calc R U . . .
C14 C -0.13323(15) 0.77684(12) 0.23507(9) 0.0063(3) Uani 1 1 d . . . . .
C15 C -0.01442(15) 0.78520(12) 0.18179(9) 0.0065(3) Uani 1 1 d . . . . .
C16 C 0.00157(16) 0.88286(12) 0.13811(9) 0.0079(3) Uani 1 1 d . . . . .
H16 H -0.065748 0.950547 0.140791 0.010 Uiso 1 1 calc R U . . .
C17 C 0.12108(16) 0.87655(12) 0.09024(9) 0.0085(3) Uani 1 1 d . . . . .
H17 H 0.134930 0.940568 0.060733 0.010 Uiso 1 1 calc R U . . .
C18 C 0.21986(16) 0.77445(12) 0.08654(9) 0.0076(3) Uani 1 1 d . . . . .
H18 H 0.300477 0.769161 0.055060 0.009 Uiso 1 1 calc R U . . .
C19 C 0.19518(16) 0.68056(12) 0.13100(9) 0.0068(3) Uani 1 1 d . . . . .
C20 C 0.28816(16) 0.56725(12) 0.13354(8) 0.0066(3) Uani 1 1 d . . . . .
C21 C 0.41924(16) 0.52342(12) 0.09812(9) 0.0083(3) Uani 1 1 d . . . . .
H21 H 0.470961 0.561464 0.063799 0.010 Uiso 1 1 calc R U . . .
C22 C 0.45460(16) 0.41068(12) 0.12566(9) 0.0085(3) Uani 1 1 d . . . . .
H22 H 0.536642 0.357435 0.113372 0.010 Uiso 1 1 calc R U . . .
N11 N -0.39580(14) 1.01192(10) 0.06970(7) 0.0087(2) Uani 1 1 d . . . . .
O1 O -0.48779(12) 0.66916(9) 0.19287(7) 0.0101(2) Uani 1 1 d . . . . .
H1O1 H -0.509(5) 0.620(5) 0.223(4) 0.015 Uiso 0.44(4) 1 d . U P A 1
H1O2 H -0.513(4) 0.571(4) 0.265(3) 0.015 Uiso 0.56(4) 1 d . U P A 2
O2 O -0.63947(12) 0.78604(9) 0.25808(7) 0.0114(2) Uani 1 1 d . . . . .
O3 O -0.34187(12) 1.08660(9) 0.03198(6) 0.0125(2) Uani 1 1 d . . . . .
C23 C -0.55025(16) 0.76368(12) 0.20630(9) 0.0082(3) Uani 1 1 d . . . . .
C24 C -0.50263(16) 0.85219(12) 0.15321(9) 0.0071(3) Uani 1 1 d . . . . .
C25 C -0.38644(16) 0.82743(12) 0.10309(9) 0.0085(3) Uani 1 1 d . . . . .
H25 H -0.344415 0.756482 0.097271 0.010 Uiso 1 1 calc R U . . .
C26 C -0.56686(17) 0.96037(12) 0.15739(9) 0.0095(3) Uani 1 1 d . . . . .
H26 H -0.646555 0.979480 0.189001 0.011 Uiso 1 1 calc R U . . .
C27 C -0.51321(17) 1.03921(12) 0.11507(9) 0.0101(3) Uani 1 1 d . . . . .
H27 H -0.557649 1.111587 0.117555 0.012 Uiso 1 1 calc R U . . .
C28 C -0.33385(16) 0.90754(13) 0.06226(9) 0.0094(3) Uani 1 1 d . . . . .
H28 H -0.255599 0.890385 0.029400 0.011 Uiso 1 1 calc R U . . .
N12 N -0.49209(13) 0.18622(10) 0.51016(7) 0.0075(2) Uani 1 1 d . . . . .
O4 O -0.37077(12) 0.52269(9) 0.37834(6) 0.0104(2) Uani 1 1 d . . . . .
O5 O -0.52075(13) 0.51385(10) 0.29121(7) 0.0126(2) Uani 1 1 d . . . . .
O6 O -0.50639(12) 0.09666(8) 0.55723(6) 0.0095(2) Uani 1 1 d . . . . .
C29 C -0.44849(16) 0.48006(12) 0.35742(9) 0.0083(3) Uani 1 1 d . . . . .
C30 C -0.46426(16) 0.37716(12) 0.41188(9) 0.0076(3) Uani 1 1 d . . . . .
C31 C -0.41644(16) 0.33904(12) 0.49141(9) 0.0085(3) Uani 1 1 d . . . . .
H31 H -0.374172 0.377601 0.512189 0.010 Uiso 1 1 calc R U . . .
C32 C -0.52591(16) 0.31650(12) 0.38298(9) 0.0089(3) Uani 1 1 d . . . . .
H32 H -0.559124 0.340475 0.329921 0.011 Uiso 1 1 calc R U . . .
C33 C -0.53818(16) 0.22162(12) 0.43203(9) 0.0085(3) Uani 1 1 d . . . . .
H33 H -0.578222 0.181324 0.411734 0.010 Uiso 1 1 calc R U . . .
C34 C -0.43129(16) 0.24419(12) 0.53981(9) 0.0082(3) Uani 1 1 d . . . . .
H34 H -0.399553 0.219561 0.593163 0.010 Uiso 1 1 calc R U . . .
N13 N 0.06719(13) 0.94518(10) 0.38145(8) 0.0078(2) Uani 1 1 d . . . . .
O7 O 0.19669(12) 1.22008(9) 0.16188(6) 0.0112(2) Uani 1 1 d . . . . .
O8 O 0.32807(12) 1.20223(9) 0.26742(6) 0.0102(2) Uani 1 1 d . . . . .
O9 O 0.01983(12) 0.86785(9) 0.42596(6) 0.0099(2) Uani 1 1 d . . . . .
C35 C 0.23691(16) 1.18051(12) 0.23380(9) 0.0078(3) Uani 1 1 d . . . . .
C36 C 0.17426(16) 1.09889(12) 0.28634(9) 0.0077(3) Uani 1 1 d . . . . .
C37 C 0.20592(16) 1.05825(12) 0.36830(9) 0.0090(3) Uani 1 1 d . . . . .
H37 H 0.264828 1.082589 0.391704 0.011 Uiso 1 1 calc R U . . .
C38 C 0.08515(16) 1.06065(12) 0.25387(9) 0.0092(3) Uani 1 1 d . . . . .
H38 H 0.060669 1.086982 0.199434 0.011 Uiso 1 1 calc R U . . .
C39 C 0.03309(16) 0.98394(12) 0.30207(9) 0.0091(3) Uani 1 1 d . . . . .
H39 H -0.026033 0.958546 0.279863 0.011 Uiso 1 1 calc R U . . .
C40 C 0.15107(16) 0.98239(12) 0.41523(9) 0.0089(3) Uani 1 1 d . . . . .
H40 H 0.171685 0.956775 0.470086 0.011 Uiso 1 1 calc R U . . .
O1W O 0.72479(13) 0.99534(10) 0.42105(7) 0.0117(2) Uani 1 1 d . . . . .
H1A H 0.807(2) 0.9465(17) 0.4232(12) 0.018 Uiso 1 1 d . U . . .
H1B H 0.671(2) 0.9669(17) 0.4318(12) 0.018 Uiso 1 1 d . U . . .
O2W O 0.63670(14) 0.12715(10) 0.26530(7) 0.0125(2) Uani 1 1 d . . . . .
H2A H 0.664(2) 0.0934(17) 0.3060(13) 0.019 Uiso 1 1 d . U . . .
H2B H 0.550(2) 0.1415(17) 0.2649(12) 0.019 Uiso 1 1 d . U . . .
O3W O 0.19560(14) 0.68963(10) 0.36375(7) 0.0131(2) Uani 1 1 d . . . . .
H3A H 0.245(2) 0.7121(17) 0.3316(13) 0.020 Uiso 1 1 d . U . . .
H3B H 0.142(2) 0.7422(17) 0.3823(12) 0.020 Uiso 1 1 d . U . . .
O4W O 0.03945(14) 0.21778(10) 0.04140(7) 0.0128(2) Uani 1 1 d . . . . .
H4A H -0.037(2) 0.2147(17) 0.0567(12) 0.019 Uiso 1 1 d . U . . .
H4B H 0.077(2) 0.2150(16) 0.0838(13) 0.019 Uiso 1 1 d . U . . .
O5W O -0.22026(14) 1.17407(10) 0.11996(8) 0.0154(2) Uani 1 1 d . . . . .
H5A H -0.252(2) 1.1603(17) 0.1613(13) 0.023 Uiso 1 1 d . U . . .
H5B H -0.262(2) 1.1494(17) 0.0935(13) 0.023 Uiso 1 1 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 N8 2.1147(13) . ?
Fe1 N3 2.1263(13) . ?
Fe1 N2 2.1541(13) . ?
Fe1 N4 2.1889(13) . ?
Fe1 N9 2.1908(13) . ?
Fe1 N7 2.1950(13) . ?
N1 N2 1.3438(17) . ?
N1 C1 1.3457(19) . ?
N1 H1N 0.911(19) . ?
N2 C3 1.3463(19) . ?
N3 C8 1.3474(19) . ?
N3 C4 1.3491(19) . ?
N4 C9 1.3435(19) . ?
N4 N5 1.3454(17) . ?
N5 C11 1.346(2) . ?
N5 H5N 0.914(19) . ?
N6 N7 1.3478(17) . ?
N6 C12 1.3483(19) . ?
N6 H6N 0.803(19) . ?
N7 C14 1.3454(19) . ?
N8 C19 1.3422(19) . ?
N8 C15 1.3430(18) . ?
N9 N10 1.3452(17) . ?
N9 C20 1.3468(19) . ?
N10 C22 1.344(2) . ?
N10 H10N 0.888(19) . ?
C1 C2 1.377(2) . ?
C1 H1 0.9300 . ?
C2 C3 1.406(2) . ?
C2 H2 0.9300 . ?
C3 C4 1.469(2) . ?
C4 C5 1.385(2) . ?
C5 C6 1.392(2) . ?
C5 H5 0.9300 . ?
C6 C7 1.392(2) . ?
C6 H6 0.9300 . ?
C7 C8 1.387(2) . ?
C7 H7 0.9300 . ?
C8 C9 1.472(2) . ?
C9 C10 1.405(2) . ?
C10 C11 1.381(2) . ?
C10 H10 0.9300 . ?
C11 H11 0.9300 . ?
C12 C13 1.374(2) . ?
C12 H12 0.9300 . ?
C13 C14 1.398(2) . ?
C13 H13 0.9300 . ?
C14 C15 1.466(2) . ?
C15 C16 1.390(2) . ?
C16 C17 1.392(2) . ?
C16 H16 0.9300 . ?
C17 C18 1.392(2) . ?
C17 H17 0.9300 . ?
C18 C19 1.390(2) . ?
C18 H18 0.9300 . ?
C19 C20 1.467(2) . ?
C20 C21 1.399(2) . ?
C21 C22 1.384(2) . ?
C21 H21 0.9300 . ?
C22 H22 0.9300 . ?
N11 O3 1.3107(16) . ?
N11 C27 1.356(2) . ?
N11 C28 1.3614(19) . ?
O1 C23 1.2835(18) . ?
O1 O5 2.4268(16) . ?
O1 H1O1 0.81(6) . ?
O2 C23 1.2376(18) . ?
C23 C24 1.501(2) . ?
C24 C26 1.391(2) . ?
C24 C25 1.394(2) . ?
C25 C28 1.374(2) . ?
C25 H25 0.9300 . ?
C26 C27 1.375(2) . ?
C26 H26 0.9300 . ?
C27 H27 0.9300 . ?
C28 H28 0.9300 . ?
N12 O6 1.3121(16) . ?
N12 C33 1.3612(19) . ?
N12 C34 1.3637(19) . ?
O4 C29 1.2418(18) . ?
O4 O5 2.2538(16) . ?
O5 C29 1.2795(18) . ?
O5 C30 2.3259(19) . ?
O5 H1O2 0.81(5) . ?
C29 C30 1.507(2) . ?
C30 C31 1.387(2) . ?
C30 C32 1.393(2) . ?
C31 C34 1.380(2) . ?
C31 H31 0.9300 . ?
C32 C33 1.374(2) . ?
C32 H32 0.9300 . ?
C33 H33 0.9300 . ?
C34 H34 0.9300 . ?
N13 O9 1.3327(16) . ?
N13 C39 1.3532(19) . ?
N13 C40 1.3534(19) . ?
O7 C35 1.2471(18) . ?
O8 C35 1.2698(18) . ?
C35 C36 1.518(2) . ?
C36 C37 1.391(2) . ?
C36 C38 1.392(2) . ?
C37 C40 1.378(2) . ?
C37 H37 0.9300 . ?
C38 C39 1.378(2) . ?
C38 H38 0.9300 . ?
C39 H39 0.9300 . ?
C40 H40 0.9300 . ?
O1W H1A 0.84(2) . ?
O1W H1B 0.75(2) . ?
O2W H2A 0.74(2) . ?
O2W H2B 0.81(2) . ?
O3W H3A 0.78(2) . ?
O3W H3B 0.85(2) . ?
O4W H4A 0.80(2) . ?
O4W H4B 0.83(2) . ?
O5W H5A 0.77(2) . ?
O5W H5B 0.84(2) . ?

loop_
_geom_angle_atom_site_label_1
_geom_angle_atom_site_label_2
_geom_angle_atom_site_label_3
_geom_angle
_geom_angle_site_symmetry_1
_geom_angle_site_symmetry_3
_geom_angle_publ_flag
N8 Fe1 N3 169.09(5) . . ?
N8 Fe1 N2 115.42(5) . . ?
N3 Fe1 N2 74.20(5) . . ?
N8 Fe1 N4 95.73(5) . . ?
N3 Fe1 N4 74.39(5) . . ?
N2 Fe1 N4 148.55(5) . . ?
N8 Fe1 N9 74.47(5) . . ?
N3 Fe1 N9 109.87(5) . . ?
N2 Fe1 N9 100.36(5) . . ?
N4 Fe1 N9 91.71(5) . . ?
N8 Fe1 N7 74.77(5) . . ?
N3 Fe1 N7 100.71(5) . . ?
N2 Fe1 N7 91.26(5) . . ?
N4 Fe1 N7 92.97(5) . . ?
N9 Fe1 N7 149.19(5) . . ?
N2 N1 C1 111.35(13) . . ?
N2 N1 H1N 115.2(11) . . ?
C1 N1 H1N 133.2(12) . . ?
N1 N2 C3 105.73(12) . . ?
N1 N2 Fe1 137.22(10) . . ?
C3 N2 Fe1 117.04(9) . . ?
C8 N3 C4 119.95(13) . . ?
C8 N3 Fe1 119.80(10) . . ?
C4 N3 Fe1 119.89(10) . . ?
C9 N4 N5 105.88(12) . . ?
C9 N4 Fe1 115.66(10) . . ?
N5 N4 Fe1 138.45(10) . . ?
N4 N5 C11 111.35(13) . . ?
N4 N5 H5N 120.7(12) . . ?
C11 N5 H5N 127.9(12) . . ?
N7 N6 C12 111.51(13) . . ?
N7 N6 H6N 122.5(14) . . ?
C12 N6 H6N 125.9(14) . . ?
C14 N7 N6 105.14(12) . . ?
C14 N7 Fe1 114.25(10) . . ?
N6 N7 Fe1 139.08(10) . . ?
C19 N8 C15 120.20(13) . . ?
C19 N8 Fe1 119.76(10) . . ?
C15 N8 Fe1 119.71(10) . . ?
N10 N9 C20 105.49(12) . . ?
N10 N9 Fe1 139.39(10) . . ?
C20 N9 Fe1 115.01(9) . . ?
C22 N10 N9 111.56(12) . . ?
C22 N10 H10N 129.5(12) . . ?
N9 N10 H10N 118.9(12) . . ?
N1 C1 C2 108.00(13) . . ?
N1 C1 H1 126.0 . . ?
C2 C1 H1 126.0 . . ?
C1 C2 C3 104.42(13) . . ?
C1 C2 H2 127.8 . . ?
C3 C2 H2 127.8 . . ?
N2 C3 C2 110.49(13) . . ?
N2 C3 C4 116.13(13) . . ?
C2 C3 C4 133.28(14) . . ?
N3 C4 C5 121.96(14) . . ?
N3 C4 C3 112.61(13) . . ?
C5 C4 C3 125.38(14) . . ?
C4 C5 C6 118.08(14) . . ?
C4 C5 H5 121.0 . . ?
C6 C5 H5 121.0 . . ?
C5 C6 C7 120.07(14) . . ?
C5 C6 H6 120.0 . . ?
C7 C6 H6 120.0 . . ?
C8 C7 C6 118.67(14) . . ?
C8 C7 H7 120.7 . . ?
C6 C7 H7 120.7 . . ?
N3 C8 C7 121.27(14) . . ?
N3 C8 C9 113.05(13) . . ?
C7 C8 C9 125.66(13) . . ?
N4 C9 C10 110.47(13) . . ?
N4 C9 C8 116.90(13) . . ?
C10 C9 C8 132.64(14) . . ?
C11 C10 C9 104.51(14) . . ?
C11 C10 H10 127.7 . . ?
C9 C10 H10 127.7 . . ?
N5 C11 C10 107.79(13) . . ?
N5 C11 H11 126.1 . . ?
C10 C11 H11 126.1 . . ?
N6 C12 C13 107.71(13) . . ?
N6 C12 H12 126.1 . . ?
C13 C12 H12 126.1 . . ?
C12 C13 C14 104.63(13) . . ?
C12 C13 H13 127.7 . . ?
C14 C13 H13 127.7 . . ?
N7 C14 C13 111.00(13) . . ?
N7 C14 C15 117.16(13) . . ?
C13 C14 C15 131.83(14) . . ?
N8 C15 C16 121.70(14) . . ?
N8 C15 C14 112.98(13) . . ?
C16 C15 C14 125.30(13) . . ?
C15 C16 C17 118.17(14) . . ?
C15 C16 H16 120.9 . . ?
C17 C16 H16 120.9 . . ?
C18 C17 C16 120.00(14) . . ?
C18 C17 H17 120.0 . . ?
C16 C17 H17 120.0 . . ?
C19 C18 C17 118.43(14) . . ?
C19 C18 H18 120.8 . . ?
C17 C18 H18 120.8 . . ?
N8 C19 C18 121.49(13) . . ?
N8 C19 C20 113.27(13) . . ?
C18 C19 C20 125.24(14) . . ?
N9 C20 C21 110.81(13) . . ?
N9 C20 C19 116.85(13) . . ?
C21 C20 C19 132.33(14) . . ?
C22 C21 C20 104.43(13) . . ?
C22 C21 H21 127.8 . . ?
C20 C21 H21 127.8 . . ?
N10 C22 C21 107.71(13) . . ?
N10 C22 H22 126.1 . . ?
C21 C22 H22 126.1 . . ?
O3 N11 C27 119.97(13) . . ?
O3 N11 C28 119.46(13) . . ?
C27 N11 C28 120.56(13) . . ?
C23 O1 O5 116.31(10) . . ?
C23 O1 H1O1 114(3) . . ?
O5 O1 H1O1 7(3) . . ?
O2 C23 O1 126.85(14) . . ?
O2 C23 C24 119.41(13) . . ?
O1 C23 C24 113.72(13) . . ?
C26 C24 C25 118.16(14) . . ?
C26 C24 C23 120.40(13) . . ?
C25 C24 C23 121.26(13) . . ?
C28 C25 C24 120.19(14) . . ?
C28 C25 H25 119.9 . . ?
C24 C25 H25 119.9 . . ?
C27 C26 C24 120.37(14) . . ?
C27 C26 H26 119.8 . . ?
C24 C26 H26 119.8 . . ?
N11 C27 C26 120.30(14) . . ?
N11 C27 H27 119.9 . . ?
C26 C27 H27 119.9 . . ?
N11 C28 C25 120.29(14) . . ?
N11 C28 H28 119.9 . . ?
C25 C28 H28 119.9 . . ?
O6 N12 C33 120.27(12) . . ?
O6 N12 C34 119.78(12) . . ?
C33 N12 C34 119.95(13) . . ?
C29 O4 O5 27.07(8) . . ?
C29 O5 O4 26.21(8) . . ?
C29 O5 C30 36.65(9) . . ?
O4 O5 C30 62.86(5) . . ?
C29 O5 O1 116.32(10) . . ?
O4 O5 O1 90.19(6) . . ?
C30 O5 O1 152.67(7) . . ?
C29 O5 H1O2 110(3) . . ?
O4 O5 H1O2 84(3) . . ?
C30 O5 H1O2 147(3) . . ?
O1 O5 H1O2 10(3) . . ?
O4 C29 O5 126.73(14) . . ?
O4 C29 C30 120.37(13) . . ?
O5 C29 C30 112.90(13) . . ?
C31 C30 C32 118.01(14) . . ?
C31 C30 C29 121.49(13) . . ?
C32 C30 C29 120.49(13) . . ?
C31 C30 O5 150.84(12) . . ?
C32 C30 O5 90.67(10) . . ?
C29 C30 O5 30.45(7) . . ?
C34 C31 C30 120.31(14) . . ?
C34 C31 H31 119.8 . . ?
C30 C31 H31 119.8 . . ?
C33 C32 C30 120.69(14) . . ?
C33 C32 O5 175.40(12) . . ?
C30 C32 O5 58.59(9) . . ?
C33 C32 H32 119.7 . . ?
C30 C32 H32 119.7 . . ?
O5 C32 H32 61.3 . . ?
N12 C33 C32 120.43(14) . . ?
N12 C33 H33 119.8 . . ?
C32 C33 H33 119.8 . . ?
N12 C34 C31 120.61(14) . . ?
N12 C34 H34 119.7 . . ?
C31 C34 H34 119.7 . . ?
O9 N13 C39 119.21(12) . . ?
O9 N13 C40 120.12(12) . . ?
C39 N13 C40 120.66(13) . . ?
O7 C35 O8 125.22(14) . . ?
O7 C35 C36 118.38(13) . . ?
O8 C35 C36 116.40(13) . . ?
C37 C36 C38 117.69(14) . . ?
C37 C36 C35 121.24(13) . . ?
C38 C36 C35 121.06(13) . . ?
C40 C37 C36 120.83(14) . . ?
C40 C37 H37 119.6 . . ?
C36 C37 H37 119.6 . . ?
C39 C38 C36 120.22(14) . . ?
C39 C38 H38 119.9 . . ?
C36 C38 H38 119.9 . . ?
N13 C39 C38 120.61(14) . . ?
N13 C39 H39 119.7 . . ?
C38 C39 H39 119.7 . . ?
N13 C40 C37 119.97(14) . . ?
N13 C40 H40 120.0 . . ?
C37 C40 H40 120.0 . . ?
H1A O1W H1B 108(2) . . ?
H2A O2W H2B 107(2) . . ?
H3A O3W H3B 108(2) . . ?
H4A O4W H4B 101(2) . . ?
H5A O5W H5B 101(2) . . ?

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 O3W 0.911(19) 1.793(19) 2.6882(18) 167.2(17) . yes
N5 H5N O4W 0.914(19) 1.932(19) 2.8190(18) 163.1(17) 2_565 yes
N6 H6N O4 0.803(19) 2.031(19) 2.8330(17) 177.6(19) . yes
N10 H10N O8 0.888(19) 1.825(19) 2.7095(17) 173.4(18) 1_545 yes
O1 H1O1^a O5 0.81(6) 1.62(6) 2.4268(16) 169(5) . yes
O1W H1A O9 0.84(2) 1.99(2) 2.8055(17) 163.3(19) 1_655 yes
O1W H1B O6 0.75(2) 2.08(2) 2.8275(16) 171(2) 2_566 yes
O2W H2A O1W 0.74(2) 2.06(2) 2.7955(17) 175(2) 1_545 yes
O2W H2B O8 0.81(2) 2.06(2) 2.8616(17) 170(2) 1_545 yes
O3W H3A O2 0.78(2) 1.97(2) 2.7513(17) 172(2) 1_655 yes
O3W H3B O9 0.85(2) 2.01(2) 2.8579(17) 178(2) . yes
O4W H4B O7 0.83(2) 1.90(2) 2.7136(17) 165(2) 1_545 yes
O4W H4A O5W 0.80(2) 2.22(2) 3.0073(18) 167(2) 1_545 yes
O5W H5A O2W 0.77(2) 2.08(2) 2.8407(18) 172(2) 1_465 yes
O5W H5B O3 0.84(2) 1.90(2) 2.7398(17) 176(2) . yes

_refine_diff_density_max         0.662
_refine_diff_density_min         -0.739
_refine_diff_density_rms         0.091


_exptl_crystal_recrystallization_method 
'Re-crystallisation from solvent: MeOH/H2O'
_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_Fe_bpp_Noxid_NHoxid_PIHSrel_95K
_database_code_depnum_ccdc_archive 'CCDC 1984964'
loop_
_audit_author_name
_audit_author_address
'Veronica Jornet Molla'
;University of Valencia
Spain
;
_audit_update_record             
;
2020-02-18 deposited with the CCDC.	2020-11-23 downloaded from the CCDC.
;
# start Validation Reply Form
_vrf_PLAT155_Fe_bpp_Noxid_NHoxid_PIHSrel_95K 
;
PROBLEM: The Triclinic Unitcell is NOT Reduced ..........     Please Do !
RESPONSE: The structural transition that takes place at low temperatures causes an increase in the gamma angle, changing from an acute angle (at higher temperatures) to an obtuse value, resulting in a non-reduced set of cell parameters. The non-reduced unit cell was preferred in order to facilitate comparisons with the crystal structure solutions at higher temperatures.
;
_vrf_PLAT303_Fe_bpp_Noxid_NHoxid_PIHSrel_95K 
;
PROBLEM: Full Occupancy Atom H1O       with # Connections       2.00 Check
RESPONSE: This hydrogen atom is located between two oxygen atoms that belong to  different carboxylate groups, forming a very strong hydrogen bond (the distance between the heteroatoms, O5 and O1, is 2.432 \%A). As a proton-transfer reaction is observed between the two carboxylate anions, different H...O distances are observed at different temperatures. Such a type of proton-transfer reaction is common when strong hydrogen bonds are established (see, for example Angew. Chem. Int. Ed. 2002, 41, 48-76).
;
# Added during the CSD deposition process: Tuesday 18 February 2020 10:39 PM
# end Validation Reply Form


_audit_creation_method           SHELXL-2018/3
_shelx_SHELXL_version_number     2018/3
_chemical_name_systematic        ?
_chemical_name_common            ?
_chemical_melting_point          ?
_chemical_formula_moiety         
'C22 H18 Fe N10 2+, C12 H9 N2 O6 1-, C6 H4 N O3 1-, 5(H2 O)'
_chemical_formula_sum            'C40 H41 Fe N13 O14'
_chemical_formula_weight         983.71

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      triclinic
_space_group_IT_number           2
_space_group_name_H-M_alt        'P -1'
_space_group_name_Hall           '-P 1'

_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'

_cell_length_a                   10.008(4)
_cell_length_b                   13.653(7)
_cell_length_c                   17.130(6)
_cell_angle_alpha                76.955(14)
_cell_angle_beta                 85.823(12)
_cell_angle_gamma                110.551(14)
_cell_volume                     2105.3(16)
_cell_formula_units_Z            2
_cell_measurement_temperature    95(1)
_cell_measurement_reflns_used    6532
_cell_measurement_theta_min      2.2077
_cell_measurement_theta_max      23.2094

_exptl_crystal_description       cube
_exptl_crystal_colour            dark-red
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    ?
_exptl_crystal_density_diffrn    1.552
_exptl_crystal_F_000             1020
_exptl_transmission_factor_min   ?
_exptl_transmission_factor_max   ?
_exptl_crystal_size_max          0.494
_exptl_crystal_size_mid          0.166
_exptl_crystal_size_min          0.127
_exptl_absorpt_coefficient_mu    0.445
_shelx_estimated_absorpt_T_min   ?
_shelx_estimated_absorpt_T_max   ?
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_correction_T_min  0.6331
_exptl_absorpt_correction_T_max  0.7468
_exptl_absorpt_process_details   
;
 SADABS 2016/2: Krause, L., Herbst-Irmer, R., Sheldrick G.M. & Stalke D.,
 J. Appl. Cryst. 48 (2015) 3-10
;
_diffrn_ambient_temperature      95(1)
_diffrn_ambient_environment      He
_diffrn_radiation_wavelength     0.71073
_diffrn_radiation_type           MoK\a
_diffrn_source                   'micro-focus sealed X-ray tube'
_diffrn_radiation_monochromator  mirror
_diffrn_measurement_device_type  
;
Bruker SMART X2S benchtop crystallographic system
;
_diffrn_measurement_method       'ω scans'
_diffrn_detector_area_resol_mean 16.0267
_diffrn_reflns_number            36767
_diffrn_reflns_av_unetI/netI     0.1688
_diffrn_reflns_av_R_equivalents  0.1057
_diffrn_reflns_limit_h_min       -15
_diffrn_reflns_limit_h_max       14
_diffrn_reflns_limit_k_min       -20
_diffrn_reflns_limit_k_max       19
_diffrn_reflns_limit_l_min       -25
_diffrn_reflns_limit_l_max       25
_diffrn_reflns_theta_min         2.199
_diffrn_reflns_theta_max         32.680
_diffrn_reflns_theta_full        25.242
_diffrn_measured_fraction_theta_max 0.964
_diffrn_measured_fraction_theta_full 0.998
_diffrn_reflns_Laue_measured_fraction_max 0.964
_diffrn_reflns_Laue_measured_fraction_full 0.998
_diffrn_reflns_point_group_measured_fraction_max 0.964
_diffrn_reflns_point_group_measured_fraction_full 0.998
_reflns_number_total             14901
_reflns_number_gt                9374
_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       
;
'APEX3 v2017.3-0 (Bruker AXS)'
;
_computing_cell_refinement       
;
'APEX3 v2017.3-0 (Bruker AXS)'
SAINT Version 8.32B (Bruker AXS Inc., 2013) 
;
_computing_data_reduction        
;
APEX3 Version 2017.3 (Bruker AXS Inc.) 
SAINT Version 8.32B (Bruker AXS Inc., 2013) 
;
_computing_structure_solution    'SHELXT 2018/2 (Sheldrick, 2018)'
_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)+(0.0311P)²+2.1311P] where P=(Fo²+2Fc²)/3'
_atom_sites_solution_primary     difmap
_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         14901
_refine_ls_number_parameters     658
_refine_ls_number_restraints     0
_refine_ls_R_factor_all          0.1224
_refine_ls_R_factor_gt           0.0632
_refine_ls_wR_factor_ref         0.1659
_refine_ls_wR_factor_gt          0.1379
_refine_ls_goodness_of_fit_ref   0.931
_refine_ls_restrained_S_all      0.931
_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 0.08320(3) 0.54654(2) 0.22435(2) 0.00841(8) Uani 1 1 d . . . . .
N1 N 0.1779(2) 0.50517(16) 0.39448(12) 0.0122(4) Uani 1 1 d . . . . .
H1N H 0.260(3) 0.568(2) 0.3764(18) 0.018 Uiso 1 1 d . U . . .
N2 N 0.0886(2) 0.48256(15) 0.34042(12) 0.0106(4) Uani 1 1 d . . . . .
N3 N -0.1051(2) 0.42963(15) 0.25774(12) 0.0100(4) Uani 1 1 d . . . . .
N4 N 0.0033(2) 0.56480(15) 0.12261(12) 0.0113(4) Uani 1 1 d . . . . .
N5 N 0.0473(2) 0.63014(16) 0.04610(12) 0.0122(4) Uani 1 1 d . . . . .
H5N H 0.139(3) 0.682(2) 0.0282(18) 0.018 Uiso 1 1 d . U . . .
N6 N -0.0730(2) 0.66611(16) 0.30844(12) 0.0122(4) Uani 1 1 d . . . . .
H6N H -0.164(3) 0.609(2) 0.3292(18) 0.018 Uiso 1 1 d . U . . .
N7 N 0.0325(2) 0.66107(15) 0.25785(12) 0.0101(4) Uani 1 1 d . . . . .
N8 N 0.26112(19) 0.67244(14) 0.18003(12) 0.0088(4) Uani 1 1 d . . . . .
N9 N 0.2102(2) 0.47963(14) 0.18020(12) 0.0095(4) Uani 1 1 d . . . . .
N10 N 0.2054(2) 0.37981(15) 0.17865(13) 0.0122(4) Uani 1 1 d . . . . .
H10N H 0.126(3) 0.316(2) 0.2148(18) 0.018 Uiso 1 1 d . U . . .
C1 C 0.1167(3) 0.43764(19) 0.46937(15) 0.0154(5) Uani 1 1 d . . . . .
H1 H 0.158522 0.438716 0.516049 0.019 Uiso 1 1 calc R U . . .
C2 C -0.0179(3) 0.36711(19) 0.46475(15) 0.0145(5) Uani 1 1 d . . . . .
H2 H -0.084615 0.311347 0.506521 0.017 Uiso 1 1 calc R U . . .
C3 C -0.0322(2) 0.39793(17) 0.38322(14) 0.0114(4) Uani 1 1 d . . . . .
C4 C -0.1474(2) 0.36642(17) 0.33536(14) 0.0112(4) Uani 1 1 d . . . . .
C5 C -0.2865(2) 0.28729(18) 0.36215(16) 0.0136(5) Uani 1 1 d . . . . .
H5 H -0.315161 0.244832 0.415711 0.016 Uiso 1 1 calc R U . . .
C6 C -0.3813(3) 0.27374(18) 0.30633(16) 0.0158(5) Uani 1 1 d . . . . .
H6 H -0.474385 0.220944 0.322501 0.019 Uiso 1 1 calc R U . . .
C7 C -0.3381(2) 0.33844(19) 0.22659(16) 0.0150(5) Uani 1 1 d . . . . .
H7 H -0.401244 0.329246 0.189198 0.018 Uiso 1 1 calc R U . . .
C8 C -0.1989(2) 0.41702(18) 0.20392(15) 0.0120(4) Uani 1 1 d . . . . .
C9 C -0.1321(2) 0.49527(18) 0.12515(15) 0.0127(4) Uani 1 1 d . . . . .
C10 C -0.1753(3) 0.5186(2) 0.04890(16) 0.0164(5) Uani 1 1 d . . . . .
H10 H -0.264038 0.483793 0.034470 0.020 Uiso 1 1 calc R U . . .
C11 C -0.0576(3) 0.60398(19) 0.00045(15) 0.0154(5) Uani 1 1 d . . . . .
H11 H -0.051377 0.637713 -0.054047 0.018 Uiso 1 1 calc R U . . .
C12 C -0.0349(3) 0.76619(19) 0.32083(15) 0.0152(5) Uani 1 1 d . . . . .
H12 H -0.091046 0.788164 0.353415 0.018 Uiso 1 1 calc R U . . .
C13 C 0.1009(3) 0.82985(19) 0.27698(15) 0.0135(5) Uani 1 1 d . . . . .
H13 H 0.155117 0.902041 0.273814 0.016 Uiso 1 1 calc R U . . .
C14 C 0.1390(2) 0.76095(17) 0.23812(14) 0.0110(4) Uani 1 1 d . . . . .
C15 C 0.2677(2) 0.77152(17) 0.18578(14) 0.0098(4) Uani 1 1 d . . . . .
C16 C 0.3824(2) 0.86621(18) 0.14350(15) 0.0133(5) Uani 1 1 d . . . . .
H16 H 0.384665 0.933675 0.147178 0.016 Uiso 1 1 calc R U . . .
C17 C 0.4940(3) 0.85776(18) 0.09548(15) 0.0138(5) Uani 1 1 d . . . . .
H17 H 0.572591 0.919922 0.067024 0.017 Uiso 1 1 calc R U . . .
C18 C 0.4878(2) 0.75559(18) 0.09013(15) 0.0133(4) Uani 1 1 d . . . . .
H18 H 0.561575 0.749068 0.057994 0.016 Uiso 1 1 calc R U . . .
C19 C 0.3697(2) 0.66407(17) 0.13359(14) 0.0107(4) Uani 1 1 d . . . . .
C20 C 0.3400(2) 0.55047(17) 0.13630(14) 0.0102(4) Uani 1 1 d . . . . .
C21 C 0.4176(3) 0.49476(19) 0.10729(15) 0.0138(5) Uani 1 1 d . . . . .
H21 H 0.509167 0.524334 0.075665 0.017 Uiso 1 1 calc R U . . .
C22 C 0.3288(3) 0.38636(19) 0.13584(15) 0.0144(5) Uani 1 1 d . . . . .
H22 H 0.350029 0.328179 0.127187 0.017 Uiso 1 1 calc R U . . .
N11 N 1.1176(2) 1.00893(17) 0.06980(13) 0.0160(4) Uani 1 1 d . . . . .
O1 O 0.69257(19) 0.66795(13) 0.19156(11) 0.0169(4) Uani 1 1 d . . . . .
H1O H 0.594(3) 0.592(2) 0.2386(19) 0.025 Uiso 1 1 d . U . . .
O2 O 0.65616(18) 0.78331(14) 0.25873(11) 0.0177(4) Uani 1 1 d . . . . .
O3 O 1.24270(19) 1.08426(15) 0.03111(11) 0.0233(4) Uani 1 1 d . . . . .
C23 C 0.7236(2) 0.76155(19) 0.20582(15) 0.0139(5) Uani 1 1 d . . . . .
C24 C 0.8576(2) 0.84971(18) 0.15355(15) 0.0130(4) Uani 1 1 d . . . . .
C25 C 0.9478(3) 0.82709(19) 0.10054(15) 0.0150(5) Uani 1 1 d . . . . .
H25 H 0.920336 0.757875 0.092857 0.018 Uiso 1 1 calc R U . . .
C26 C 0.8990(3) 0.95521(19) 0.16070(15) 0.0149(5) Uani 1 1 d . . . . .
H26 H 0.838835 0.972672 0.194369 0.018 Uiso 1 1 calc R U . . .
C27 C 1.0283(3) 1.0341(2) 0.11842(16) 0.0174(5) Uani 1 1 d . . . . .
H27 H 1.054686 1.104686 0.123118 0.021 Uiso 1 1 calc R U . . .
C28 C 1.0779(3) 0.9069(2) 0.05939(15) 0.0160(5) Uani 1 1 d . . . . .
H28 H 1.138442 0.891288 0.024558 0.019 Uiso 1 1 calc R U . . .
N12 N 0.1992(2) 0.19075(15) 0.50908(13) 0.0128(4) Uani 1 1 d . . . . .
O4 O 0.65545(18) 0.51279(13) 0.37816(11) 0.0165(4) Uani 1 1 d . . . . .
O5 O 0.50325(19) 0.51355(14) 0.28762(11) 0.0197(4) Uani 1 1 d . . . . .
O6 O 0.09392(17) 0.10619(13) 0.55747(11) 0.0157(4) Uani 1 1 d . . . . .
C29 C 0.5380(3) 0.47502(18) 0.35498(15) 0.0137(5) Uani 1 1 d . . . . .
C30 C 0.4198(2) 0.37432(18) 0.40891(15) 0.0130(4) Uani 1 1 d . . . . .
C31 C 0.4268(3) 0.33670(18) 0.49045(15) 0.0138(5) Uani 1 1 d . . . . .
H31 H 0.506238 0.373265 0.511974 0.017 Uiso 1 1 calc R U . . .
C32 C 0.3002(3) 0.31615(19) 0.37877(15) 0.0138(5) Uani 1 1 d . . . . .
H32 H 0.293158 0.339170 0.324376 0.017 Uiso 1 1 calc R U . . .
C33 C 0.1920(3) 0.22460(19) 0.42899(15) 0.0142(5) Uani 1 1 d . . . . .
H33 H 0.113537 0.185656 0.407930 0.017 Uiso 1 1 calc R U . . .
C34 C 0.3165(3) 0.24553(19) 0.53960(15) 0.0137(5) Uani 1 1 d . . . . .
H34 H 0.322235 0.221184 0.594047 0.016 Uiso 1 1 calc R U . . .
N13 N 0.4990(2) 1.06878(15) -0.39315(13) 0.0131(4) Uani 1 1 d . . . . .
O7 O 0.10694(19) 0.79699(14) -0.16929(11) 0.0182(4) Uani 1 1 d . . . . .
O8 O -0.00670(18) 0.80877(13) -0.27644(11) 0.0159(4) Uani 1 1 d . . . . .
O9 O 0.61906(18) 1.14563(13) -0.43848(11) 0.0161(4) Uani 1 1 d . . . . .
C35 C 0.1046(3) 0.83464(18) -0.24277(15) 0.0134(5) Uani 1 1 d . . . . .
C36 C 0.2441(2) 0.91689(17) -0.29637(15) 0.0121(4) Uani 1 1 d . . . . .
C37 C 0.2525(3) 0.95405(18) -0.37983(15) 0.0134(5) Uani 1 1 d . . . . .
H37 H 0.171206 0.928221 -0.403622 0.016 Uiso 1 1 calc R U . . .
C38 C 0.3683(3) 0.95724(19) -0.26326(16) 0.0153(5) Uani 1 1 d . . . . .
H38 H 0.366303 0.933170 -0.207726 0.018 Uiso 1 1 calc R U . . .
C39 C 0.4941(3) 1.03258(19) -0.31217(15) 0.0158(5) Uani 1 1 d . . . . .
H39 H 0.576552 1.058920 -0.289385 0.019 Uiso 1 1 calc R U . . .
C40 C 0.3801(3) 1.02866(18) -0.42764(15) 0.0131(4) Uani 1 1 d . . . . .
H40 H 0.385053 1.051719 -0.483548 0.016 Uiso 1 1 calc R U . . .
O1W O 0.2063(2) 0.97887(15) 0.42527(12) 0.0185(4) Uani 1 1 d . . . . .
H1B H 0.242(3) 0.931(3) 0.4276(19) 0.028 Uiso 1 1 d . U . . .
H1A H 0.120(4) 0.948(3) 0.436(2) 0.028 Uiso 1 1 d . U . . .
O2W O 0.2482(2) 1.11644(16) 0.27176(13) 0.0226(4) Uani 1 1 d . . . . .
H2A H 0.175(4) 1.129(3) 0.273(2) 0.034 Uiso 1 1 d . U . . .
H2B H 0.234(4) 1.077(3) 0.312(2) 0.034 Uiso 1 1 d . U . . .
O3W O 0.3953(2) 0.69601(15) 0.35745(13) 0.0201(4) Uani 1 1 d . . . . .
H3A H 0.389(3) 0.739(3) 0.383(2) 0.030 Uiso 1 1 d . U . . .
H3B H 0.479(4) 0.722(3) 0.324(2) 0.030 Uiso 1 1 d . U . . .
O4W O 0.2794(2) 0.80048(17) -0.05233(12) 0.0234(4) Uani 1 1 d . . . . .
H4A H 0.241(4) 0.801(3) -0.092(2) 0.035 Uiso 1 1 d . U . . .
H4B H 0.362(4) 0.809(3) -0.073(2) 0.035 Uiso 1 1 d . U . . .
O5W O 1.4353(2) 1.15765(19) 0.12802(14) 0.0286(5) Uani 1 1 d . . . . .
H5A H 1.375(4) 1.133(3) 0.097(2) 0.043 Uiso 1 1 d . U . . .
H5B H 1.393(4) 1.145(3) 0.172(2) 0.043 Uiso 1 1 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 1.935(2) . ?
Fe1 N8 1.941(2) . ?
Fe1 N4 1.971(2) . ?
Fe1 N7 1.988(2) . ?
Fe1 N2 1.996(2) . ?
Fe1 N9 2.0019(19) . ?
N1 N2 1.344(3) . ?
N1 C1 1.351(3) . ?
N1 H1N 0.92(3) . ?
N2 C3 1.357(3) . ?
N3 C4 1.355(3) . ?
N3 C8 1.358(3) . ?
N4 C9 1.345(3) . ?
N4 N5 1.349(3) . ?
N5 C11 1.350(3) . ?
N5 H5N 0.92(3) . ?
N6 N7 1.347(3) . ?
N6 C12 1.354(3) . ?
N6 H6N 0.94(3) . ?
N7 C14 1.353(3) . ?
N8 C19 1.353(3) . ?
N8 C15 1.358(3) . ?
N9 N10 1.353(2) . ?
N9 C20 1.355(3) . ?
N10 C22 1.354(3) . ?
N10 H10N 0.99(3) . ?
C1 C2 1.374(3) . ?
C1 H1 0.9300 . ?
C2 C3 1.398(3) . ?
C2 H2 0.9300 . ?
C3 C4 1.462(3) . ?
C4 C5 1.394(3) . ?
C5 C6 1.392(4) . ?
C5 H5 0.9300 . ?
C6 C7 1.391(4) . ?
C6 H6 0.9300 . ?
C7 C8 1.388(3) . ?
C7 H7 0.9300 . ?
C8 C9 1.458(3) . ?
C9 C10 1.409(3) . ?
C10 C11 1.375(4) . ?
C10 H10 0.9300 . ?
C11 H11 0.9300 . ?
C12 C13 1.377(3) . ?
C12 H12 0.9300 . ?
C13 C14 1.404(3) . ?
C13 H13 0.9300 . ?
C14 C15 1.458(3) . ?
C15 C16 1.389(3) . ?
C16 C17 1.392(3) . ?
C16 H16 0.9300 . ?
C17 C18 1.398(3) . ?
C17 H17 0.9300 . ?
C18 C19 1.388(3) . ?
C18 H18 0.9300 . ?
C19 C20 1.462(3) . ?
C20 C21 1.400(3) . ?
C21 C22 1.381(3) . ?
C21 H21 0.9300 . ?
C22 H22 0.9300 . ?
N11 O3 1.316(3) . ?
N11 C27 1.359(3) . ?
N11 C28 1.365(3) . ?
O1 C23 1.290(3) . ?
O1 H1O 1.22(3) . ?
O2 C23 1.240(3) . ?
C23 C24 1.501(3) . ?
C24 C26 1.389(3) . ?
C24 C25 1.392(3) . ?
C25 C28 1.379(4) . ?
C25 H25 0.9300 . ?
C26 C27 1.375(3) . ?
C26 H26 0.9300 . ?
C27 H27 0.9300 . ?
C28 H28 0.9300 . ?
N12 O6 1.310(3) . ?
N12 C33 1.361(3) . ?
N12 C34 1.364(3) . ?
O4 C29 1.241(3) . ?
O5 C29 1.281(3) . ?
O5 H1O 1.21(3) . ?
C29 C30 1.506(3) . ?
C30 C31 1.391(3) . ?
C30 C32 1.392(3) . ?
C31 C34 1.379(3) . ?
C31 H31 0.9300 . ?
C32 C33 1.380(3) . ?
C32 H32 0.9300 . ?
C33 H33 0.9300 . ?
C34 H34 0.9300 . ?
N13 O9 1.326(3) . ?
N13 C39 1.354(3) . ?
N13 C40 1.363(3) . ?
O7 C35 1.253(3) . ?
O8 C35 1.268(3) . ?
C35 C36 1.517(3) . ?
C36 C37 1.390(3) . ?
C36 C38 1.391(3) . ?
C37 C40 1.377(3) . ?
C37 H37 0.9300 . ?
C38 C39 1.376(3) . ?
C38 H38 0.9300 . ?
C39 H39 0.9300 . ?
C40 H40 0.9300 . ?
O1W H1B 0.84(3) . ?
O1W H1A 0.80(3) . ?
O2W H2A 0.81(4) . ?
O2W H2B 0.74(4) . ?
O3W H3A 0.82(3) . ?
O3W H3B 0.89(3) . ?
O4W H4A 0.80(4) . ?
O4W H4B 0.84(4) . ?
O5W H5A 0.85(4) . ?
O5W H5B 0.79(4) . ?

loop_
_geom_angle_atom_site_label_1
_geom_angle_atom_site_label_2
_geom_angle_atom_site_label_3
_geom_angle
_geom_angle_site_symmetry_1
_geom_angle_site_symmetry_3
_geom_angle_publ_flag
N3 Fe1 N8 172.62(8) . . ?
N3 Fe1 N4 79.50(8) . . ?
N8 Fe1 N4 93.69(8) . . ?
N3 Fe1 N7 98.45(8) . . ?
N8 Fe1 N7 79.03(8) . . ?
N4 Fe1 N7 93.99(8) . . ?
N3 Fe1 N2 78.32(8) . . ?
N8 Fe1 N2 108.43(8) . . ?
N4 Fe1 N2 157.82(8) . . ?
N7 Fe1 N2 88.85(8) . . ?
N3 Fe1 N9 104.19(8) . . ?
N8 Fe1 N9 78.64(8) . . ?
N4 Fe1 N9 91.36(8) . . ?
N7 Fe1 N9 157.32(8) . . ?
N2 Fe1 N9 94.45(8) . . ?
N2 N1 C1 111.0(2) . . ?
N2 N1 H1N 116.0(18) . . ?
C1 N1 H1N 132.2(18) . . ?
N1 N2 C3 105.53(19) . . ?
N1 N2 Fe1 137.47(16) . . ?
C3 N2 Fe1 116.71(15) . . ?
C4 N3 C8 120.2(2) . . ?
C4 N3 Fe1 120.67(15) . . ?
C8 N3 Fe1 118.98(16) . . ?
C9 N4 N5 106.30(19) . . ?
C9 N4 Fe1 116.15(16) . . ?
N5 N4 Fe1 137.55(16) . . ?
N4 N5 C11 110.9(2) . . ?
N4 N5 H5N 122.8(18) . . ?
C11 N5 H5N 126.1(18) . . ?
N7 N6 C12 110.9(2) . . ?
N7 N6 H6N 124.5(17) . . ?
C12 N6 H6N 124.4(17) . . ?
N6 N7 C14 105.60(18) . . ?
N6 N7 Fe1 137.40(15) . . ?
C14 N7 Fe1 115.78(15) . . ?
C19 N8 C15 119.95(19) . . ?
C19 N8 Fe1 119.84(15) . . ?
C15 N8 Fe1 119.50(15) . . ?
N10 N9 C20 105.70(18) . . ?
N10 N9 Fe1 138.72(15) . . ?
C20 N9 Fe1 115.55(14) . . ?
N9 N10 C22 111.01(19) . . ?
N9 N10 H10N 118.0(16) . . ?
C22 N10 H10N 130.0(16) . . ?
N1 C1 C2 108.3(2) . . ?
N1 C1 H1 125.8 . . ?
C2 C1 H1 125.8 . . ?
C1 C2 C3 104.5(2) . . ?
C1 C2 H2 127.7 . . ?
C3 C2 H2 127.7 . . ?
N2 C3 C2 110.6(2) . . ?
N2 C3 C4 113.6(2) . . ?
C2 C3 C4 135.7(2) . . ?
N3 C4 C5 121.5(2) . . ?
N3 C4 C3 110.69(19) . . ?
C5 C4 C3 127.7(2) . . ?
C6 C5 C4 118.0(2) . . ?
C6 C5 H5 121.0 . . ?
C4 C5 H5 121.0 . . ?
C7 C6 C5 120.6(2) . . ?
C7 C6 H6 119.7 . . ?
C5 C6 H6 119.7 . . ?
C8 C7 C6 118.7(2) . . ?
C8 C7 H7 120.7 . . ?
C6 C7 H7 120.7 . . ?
N3 C8 C7 121.0(2) . . ?
N3 C8 C9 110.8(2) . . ?
C7 C8 C9 128.2(2) . . ?
N4 C9 C10 109.9(2) . . ?
N4 C9 C8 114.5(2) . . ?
C10 C9 C8 135.6(2) . . ?
C11 C10 C9 105.0(2) . . ?
C11 C10 H10 127.5 . . ?
C9 C10 H10 127.5 . . ?
N5 C11 C10 107.8(2) . . ?
N5 C11 H11 126.1 . . ?
C10 C11 H11 126.1 . . ?
N6 C12 C13 108.4(2) . . ?
N6 C12 H12 125.8 . . ?
C13 C12 H12 125.8 . . ?
C12 C13 C14 104.2(2) . . ?
C12 C13 H13 127.9 . . ?
C14 C13 H13 127.9 . . ?
N7 C14 C13 110.9(2) . . ?
N7 C14 C15 114.38(19) . . ?
C13 C14 C15 134.7(2) . . ?
N8 C15 C16 121.7(2) . . ?
N8 C15 C14 110.38(19) . . ?
C16 C15 C14 127.9(2) . . ?
C15 C16 C17 118.4(2) . . ?
C15 C16 H16 120.8 . . ?
C17 C16 H16 120.8 . . ?
C16 C17 C18 119.9(2) . . ?
C16 C17 H17 120.1 . . ?
C18 C17 H17 120.1 . . ?
C19 C18 C17 118.9(2) . . ?
C19 C18 H18 120.6 . . ?
C17 C18 H18 120.6 . . ?
N8 C19 C18 121.2(2) . . ?
N8 C19 C20 110.56(19) . . ?
C18 C19 C20 128.2(2) . . ?
N9 C20 C21 110.43(19) . . ?
N9 C20 C19 114.43(19) . . ?
C21 C20 C19 135.0(2) . . ?
C22 C21 C20 105.0(2) . . ?
C22 C21 H21 127.5 . . ?
C20 C21 H21 127.5 . . ?
N10 C22 C21 107.9(2) . . ?
N10 C22 H22 126.1 . . ?
C21 C22 H22 126.1 . . ?
O3 N11 C27 119.7(2) . . ?
O3 N11 C28 119.6(2) . . ?
C27 N11 C28 120.8(2) . . ?
C23 O1 H1O 116.7(14) . . ?
O2 C23 O1 126.4(2) . . ?
O2 C23 C24 118.7(2) . . ?
O1 C23 C24 114.9(2) . . ?
C26 C24 C25 118.3(2) . . ?
C26 C24 C23 120.4(2) . . ?
C25 C24 C23 121.2(2) . . ?
C28 C25 C24 120.3(2) . . ?
C28 C25 H25 119.9 . . ?
C24 C25 H25 119.9 . . ?
C27 C26 C24 120.6(2) . . ?
C27 C26 H26 119.7 . . ?
C24 C26 H26 119.7 . . ?
N11 C27 C26 120.1(2) . . ?
N11 C27 H27 120.0 . . ?
C26 C27 H27 120.0 . . ?
N11 C28 C25 120.0(2) . . ?
N11 C28 H28 120.0 . . ?
C25 C28 H28 120.0 . . ?
O6 N12 C33 120.6(2) . . ?
O6 N12 C34 119.5(2) . . ?
C33 N12 C34 119.9(2) . . ?
C29 O5 H1O 118.6(14) . . ?
O4 C29 O5 126.5(2) . . ?
O4 C29 C30 119.6(2) . . ?
O5 C29 C30 113.9(2) . . ?
C31 C30 C32 118.0(2) . . ?
C31 C30 C29 121.0(2) . . ?
C32 C30 C29 121.1(2) . . ?
C34 C31 C30 120.4(2) . . ?
C34 C31 H31 119.8 . . ?
C30 C31 H31 119.8 . . ?
C33 C32 C30 120.5(2) . . ?
C33 C32 H32 119.8 . . ?
C30 C32 H32 119.8 . . ?
N12 C33 C32 120.6(2) . . ?
N12 C33 H33 119.7 . . ?
C32 C33 H33 119.7 . . ?
N12 C34 C31 120.6(2) . . ?
N12 C34 H34 119.7 . . ?
C31 C34 H34 119.7 . . ?
O9 N13 C39 119.7(2) . . ?
O9 N13 C40 120.0(2) . . ?
C39 N13 C40 120.2(2) . . ?
O7 C35 O8 124.7(2) . . ?
O7 C35 C36 118.5(2) . . ?
O8 C35 C36 116.8(2) . . ?
C37 C36 C38 117.8(2) . . ?
C37 C36 C35 121.5(2) . . ?
C38 C36 C35 120.7(2) . . ?
C40 C37 C36 120.7(2) . . ?
C40 C37 H37 119.6 . . ?
C36 C37 H37 119.6 . . ?
C39 C38 C36 120.4(2) . . ?
C39 C38 H38 119.8 . . ?
C36 C38 H38 119.8 . . ?
N13 C39 C38 120.7(2) . . ?
N13 C39 H39 119.7 . . ?
C38 C39 H39 119.7 . . ?
N13 C40 C37 120.1(2) . . ?
N13 C40 H40 119.9 . . ?
C37 C40 H40 119.9 . . ?
H1B O1W H1A 107(3) . . ?
H2A O2W H2B 101(3) . . ?
H3A O3W H3B 112(3) . . ?
H4A O4W H4B 100(3) . . ?
H5A O5W H5B 109(4) . . ?

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 O3W 0.92(3) 1.74(3) 2.645(3) 167(3) . yes
N5 H5N O4W 0.92(3) 1.90(3) 2.741(3) 151(3) . yes
N6 H6N O4 0.94(3) 1.82(3) 2.757(3) 171(3) 1_455 yes
N10 H10N O8 0.99(3) 1.74(3) 2.714(3) 170(3) 2_565 yes
O1W H1B O9 0.84(3) 2.01(3) 2.823(3) 162(3) 2_675 yes
O1W H1A O6 0.80(3) 1.99(3) 2.780(3) 169(3) 2_566 yes
O2W H2B O1W 0.74(4) 2.03(4) 2.771(3) 176(4) . yes
O2W H2A O8 0.81(4) 2.14(4) 2.938(3) 169(3) 2_575 yes
O3W H3B O2 0.89(3) 1.83(4) 2.713(3) 175(3) . yes
O3W H3A O9 0.82(3) 2.04(3) 2.857(3) 175(3) 2_675 yes
O4W H4A O7 0.80(4) 1.95(4) 2.736(3) 166(4) . yes
O4W H4B O5W 0.84(4) 2.02(4) 2.853(3) 175(3) 2_775 yes
O5W H5B O2W 0.79(4) 2.03(4) 2.802(3) 167(4) 1_655 yes
O5W H5A O3 0.85(4) 1.85(4) 2.709(3) 178(4) . yes

_refine_diff_density_max         1.083
_refine_diff_density_min         -1.416
_refine_diff_density_rms         0.116


_exptl_crystal_recrystallization_method 
'Re-crystallisation from solvent: MeOH/H2O'
_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_Fe_bpp_Noxid_NHoxid_Neutrons_120K
_database_code_depnum_ccdc_archive 'CCDC 1984960'
loop_
_audit_author_name
_audit_author_address
'Veronica Jornet Molla'
;University of Valencia
Spain
;
_audit_update_record             
;
2020-02-21 deposited with the CCDC.	2020-11-23 downloaded from the CCDC.
;
# start Validation Reply Form
_vrf_PLAT029_Fe_bpp_Noxid_NHoxid_Neutrons_120K 
;
PROBLEM: _diffrn_measured_fraction_theta_full value Low .      0.849 Why?
RESPONSE: The wavelength used for this experiment is 1.45510  \%A. Therefore, the number of collected reflections is low and this results in a low value of measured fraction theta full.
;
_vrf_PLAT088_Fe_bpp_Noxid_NHoxid_Neutrons_120K 
;
PROBLEM: Poor Data / Parameter Ratio ....................       6.54 Note
RESPONSE: The wavelength used for this experiment is  1.45510 \%A. Therefore, the number of collected reflections is low and not enough to yield a data/parameter ratio of 10. In addition, there are 272 non-hydrogen atoms in the unit cell of this structure (68 in the asymmetric unit), which were refined anisotropically. Thus, the data/parameter ratio is low due to the large number of refined parameters and the wavelength used. 
;
_vrf_PLAT110_Fe_bpp_Noxid_NHoxid_Neutrons_120K 
;
PROBLEM: ADDSYM Detects Potential Lattice Translation ...          ? Check
RESPONSE: The asymmetric unit contains two crystallographically independent Fe(II) complexes (and Z = 4) having clearly different Fe-N distances which correspond to two different spin states (high and low), as confirmed by magnetic susceptibility measurements. The alerts arise because the structure can also be solved with a smaller unit cell (with parameters very similar to the high temperature structure  solution) having half volume and only one Fe(II) complex (and Z = 2) with intermediate Fe-N distances between the corresponding high and low spin states. This solution also exhibits more elongated thermal ellipsoids in the N and C atoms of the ligands, suggesting that they can be split in two different positions corresponding to the high and low spin states. Therefore, the structure solution with Z = 4 has been adopted.
;
_vrf_PLAT112_Fe_bpp_Noxid_NHoxid_Neutrons_120K 
;
PROBLEM: ADDSYM Detects New (Pseudo) Symm. Elem         B        100 %Fit
RESPONSE: The asymmetric unit contains two crystallographically independent Fe(II) complexes (and Z = 4) having clearly different Fe-N distances which correspond to two different spin states (high and low), as confirmed by magnetic susceptibility measurements. The alerts arise because the structure can also be solved with a smaller unit cell (with parameters very similar to the high temperature structure  solution) having half volume and only one Fe(II) complex (and Z = 2) with intermediate Fe-N distances between the corresponding high and low spin states. This solution also exhibits more elongated thermal ellipsoids in the N and C atoms of the ligands, suggesting that they can be split in two different positions corresponding to the high and low spin states. Therefore, the structure solution with Z = 4 has been adopted.
;
_vrf_PLAT113_Fe_bpp_Noxid_NHoxid_Neutrons_120K 
;
PROBLEM: ADDSYM Suggests Possible Pseudo/New  Space Group        P-1 Check
RESPONSE: The asymmetric unit contains two crystallographically independent Fe(II) complexes (and Z = 4) having clearly different Fe-N distances which correspond to two different spin states (high and low), as confirmed by magnetic susceptibility measurements. The alerts arise because the structure can also be solved with a smaller unit cell (with parameters very similar to the high temperature structure  solution) having half volume and only one Fe(II) complex (and Z = 2) with intermediate Fe-N distances between the corresponding high and low spin states. This solution also exhibits more elongated thermal ellipsoids in the N and C atoms of the ligands, suggesting that they can be split in two different positions corresponding to the high and low spin states. Therefore, the structure solution with Z = 4 has been adopted.
;
_vrf_PLAT911_Fe_bpp_Noxid_NHoxid_Neutrons_120K 
;
PROBLEM: Missing FCF Refl Between Thmin & STh/L=    0.600       2283 Report
RESPONSE: Some reflections are missing due to the restrictions of the experiment. The sample was placed on a close-circuit displex device on the monochromatic four-circle diffractometer D19 at ILL (Grenoble, France). The measurement strategy consisted on 25 omega (\w) scans with steps of 0.07\% at different \c and \f positions. These omega scans cover either 79\% or 64\% depending on the \c angle, in order to avoid collisions with the sample environment. Absorption correction removes reflections due to the environment provided by the neutron setup.
;
_vrf_PLAT303_Fe_bpp_Noxid_NHoxid_Neutrons_120K 
;
PROBLEM: Full Occupancy Atom H1OB      with # Connections       2.00 Check
RESPONSE: This hydrogen atom is located between two oxygen atoms that belong to different carboxylate groups, forming a very strong hydrogen bond (the distance between the heteroatoms, O5B and O1A, is 2.427 \%A). As a proton-transfer reaction is observed between the two carboxylate anions, different H...O distances are observed at different temperatures. Such a type of proton-transfer reaction is common when strong hydrogen bonds are established (see, for example Angew. Chem. Int. Ed. 2002, 41, 48-76).
;
_vrf_PLAT303_Fe_bpp_Noxid_NHoxid_Neutrons_120K_2 
;
PROBLEM: Full Occupancy Atom H1OA      with # Connections       2.00 Check
RESPONSE: This hydrogen atom is located between two oxygen atoms that belong to different carboxylate groups, forming a very strong hydrogen bond (the distance between the heteroatoms, O5A and O1B, is 2.416 \%A). As a proton-transfer reaction is observed between the two carboxylate anions, different H...O distances are observed at different temperatures. Such a type of proton-transfer reaction is common when strong hydrogen bonds are established (see, for example Angew. Chem. Int. Ed. 2002, 41, 48-76).
;
# Added during the CSD deposition process: Friday 21 February 2020 08:26 PM
# end Validation Reply Form


_audit_creation_method           SHELXL-2018/3
_shelx_SHELXL_version_number     2018/3
_chemical_name_systematic        ?
_chemical_name_common            ?
_chemical_melting_point          ?
_chemical_formula_moiety         
'C22 H18 Fe N10 2+, C12 H9 N2 O6 1-, C6 H4 N O3 1-, 5(H2 O)'
_chemical_formula_sum            'C40 H41 Fe N13 O14'
_chemical_formula_weight         983.71

loop_
_atom_type_symbol
_atom_type_description
_atom_type_scat_dispersion_real
_atom_type_scat_dispersion_imag
_atom_type_scat_source
C C 0.0000 0.0000
'Neutron Data Booklet, ILL Grenoble, France (2003) ISBN 0-9704143-7-4'
H H 0.0000 0.0000
'Neutron Data Booklet, ILL Grenoble, France (2003) ISBN 0-9704143-7-4'
N N 0.0000 0.0000
'Neutron Data Booklet, ILL Grenoble, France (2003) ISBN 0-9704143-7-4'
O O 0.0000 0.0000
'Neutron Data Booklet, ILL Grenoble, France (2003) ISBN 0-9704143-7-4'
Fe Fe 0.0000 0.0000
'Neutron Data Booklet, ILL Grenoble, France (2003) ISBN 0-9704143-7-4'

_space_group_crystal_system      triclinic
_space_group_IT_number           2
_space_group_name_H-M_alt        'P -1'
_space_group_name_Hall           '-P 1'

_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'

_cell_length_a                   13.5877(3)
_cell_length_b                   18.7535(5)
_cell_length_c                   19.6264(5)
_cell_angle_alpha                64.662(2)
_cell_angle_beta                 71.098(2)
_cell_angle_gamma                71.086(2)
_cell_volume                     4174.4(2)
_cell_formula_units_Z            4
_cell_measurement_temperature    120(1)
_cell_measurement_reflns_used    5210
_cell_measurement_theta_min      5.781
_cell_measurement_theta_max      60.256

_exptl_crystal_description       cube
_exptl_crystal_colour            red
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    ?
_exptl_crystal_density_diffrn    1.565
_exptl_crystal_F_000             1300
_exptl_transmission_factor_min   ?
_exptl_transmission_factor_max   ?
_exptl_crystal_size_max          1.85
_exptl_crystal_size_mid          1.50
_exptl_crystal_size_min          0.70
_exptl_absorpt_coefficient_mu    0.193
_shelx_estimated_absorpt_T_min   ?
_shelx_estimated_absorpt_T_max   ?
_exptl_absorpt_correction_type   numerical
_exptl_absorpt_correction_T_min  ?
_exptl_absorpt_correction_T_max  ?
_exptl_absorpt_process_details   
; 
Absorption corretion done through d19face, d19abs and d19abscan 
programs from ILL
;
_diffrn_ambient_temperature      120(1)
_diffrn_radiation_wavelength     1.45510
_diffrn_radiation_type           neutrons
_diffrn_source                   'neutron source'
_diffrn_source_type              'ILL High Flux Reactor, beam H11'
_diffrn_source_power             57MW
_diffrn_measurement_device_type  
'D19 position-sensitive detector diffractometer'
_diffrn_radiation_monochromator  'copper 220'
_diffrn_measurement_method       'omega step-scans'
_diffrn_detector_area_resol_mean '1.56 mm vert. 2.5 mm hor.'
_diffrn_reflns_number            25116
_diffrn_reflns_av_unetI/netI     0.0363
_diffrn_reflns_av_R_equivalents  0.0428
_diffrn_reflns_limit_h_min       -16
_diffrn_reflns_limit_h_max       15
_diffrn_reflns_limit_k_min       -22
_diffrn_reflns_limit_k_max       22
_diffrn_reflns_limit_l_min       -18
_diffrn_reflns_limit_l_max       23
_diffrn_reflns_theta_min         4.510
_diffrn_reflns_theta_max         60.871
_diffrn_reflns_theta_full        60.816
_diffrn_measured_fraction_theta_max 0.848
_diffrn_measured_fraction_theta_full 0.849
_diffrn_reflns_Laue_measured_fraction_max 0.848
_diffrn_reflns_Laue_measured_fraction_full 0.849
_diffrn_reflns_point_group_measured_fraction_max 0.848
_diffrn_reflns_point_group_measured_fraction_full 0.849
_reflns_number_total             12837
_reflns_number_gt                10517
_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       'The NOMAD software from ILL '
_computing_cell_refinement       'PFIND and DIRAX programs'
_computing_data_reduction        'RETREAT and RAFD19 programs'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1997)'
_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)+(0.1218P)²+17.2660P] where P=(Fo²+2Fc²)/3'
_atom_sites_solution_primary     difmap
_atom_sites_solution_secondary   difmap
_atom_sites_solution_hydrogens   difmap
_refine_ls_hydrogen_treatment    refall
_refine_ls_extinction_method     none
_refine_ls_extinction_coef       .
_refine_ls_number_reflns         12837
_refine_ls_number_parameters     1963
_refine_ls_number_restraints     0
_refine_ls_R_factor_all          0.0750
_refine_ls_R_factor_gt           0.0627
_refine_ls_wR_factor_ref         0.1884
_refine_ls_wR_factor_gt          0.1761
_refine_ls_goodness_of_fit_ref   1.114
_refine_ls_restrained_S_all      1.114
_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
Fe1A Fe 0.88450(14) 0.73159(10) 0.34428(10) 0.0179(4) Uani 1 1 d . . . . .
H1A H 0.8850(6) 1.0366(4) 0.1597(4) 0.0495(16) Uani 1 1 d . . . . .
N1A N 0.88681(15) 0.91287(11) 0.21622(12) 0.0242(4) Uani 1 1 d . . . . .
H1NA H 0.8750(5) 0.8974(3) 0.1749(3) 0.0372(13) Uani 1 1 d . . . . .
N2A N 0.88979(15) 0.85709(10) 0.28701(11) 0.0223(4) Uani 1 1 d . . . . .
N3A N 0.88910(15) 0.77022(11) 0.43038(11) 0.0209(4) Uani 1 1 d . . . . .
N4A N 0.87780(15) 0.62678(10) 0.45111(11) 0.0228(4) Uani 1 1 d . . . . .
N5A N 0.87304(16) 0.54937(11) 0.47442(13) 0.0265(4) Uani 1 1 d . . . . .
H5NA H 0.8763(5) 0.5245(3) 0.4371(4) 0.0406(14) Uani 1 1 d . . . . .
N6A N 0.62581(15) 0.81048(11) 0.37740(12) 0.0237(4) Uani 1 1 d . . . . .
H6NA H 0.6255(5) 0.8330(3) 0.4169(3) 0.0366(13) Uani 1 1 d . . . . .
N7A N 0.71275(14) 0.76116(10) 0.35283(10) 0.0198(4) Uani 1 1 d . . . . .
N8A N 0.86299(14) 0.67571(10) 0.27871(10) 0.0185(4) Uani 1 1 d . . . . .
N9A N 1.04434(15) 0.67715(10) 0.29467(11) 0.0208(4) Uani 1 1 d . . . . .
N10A N 1.14614(15) 0.67136(11) 0.29253(11) 0.0232(4) Uani 1 1 d . . . . .
H10N H 0.3610(4) 0.2857(3) 0.1658(3) 0.0340(12) Uani 1 1 d . . . . .
C1A C 0.8884(2) 0.98602(16) 0.21255(17) 0.0277(6) Uani 1 1 d . . . . .
C2A C 0.8930(2) 0.97760(16) 0.28530(17) 0.0260(6) Uani 1 1 d . . . . .
H2A H 0.8946(6) 1.0240(3) 0.3018(4) 0.0471(15) Uani 1 1 d . . . . .
C3A C 0.8928(2) 0.89591(14) 0.32977(15) 0.0201(5) Uani 1 1 d . . . . .
C4A C 0.8897(2) 0.84818(15) 0.41190(15) 0.0193(5) Uani 1 1 d . . . . .
C5A C 0.8829(2) 0.87743(16) 0.46755(16) 0.0246(6) Uani 1 1 d . . . . .
H5A H 0.8827(5) 0.9407(4) 0.4513(4) 0.0415(14) Uani 1 1 d . . . . .
C6A C 0.8757(2) 0.82460(17) 0.54351(17) 0.0269(6) Uani 1 1 d . . . . .
H6A H 0.8700(5) 0.8454(4) 0.5880(4) 0.0453(15) Uani 1 1 d . . . . .
C7A C 0.8737(2) 0.74407(17) 0.56294(17) 0.0266(6) Uani 1 1 d . . . . .
H7A H 0.8662(6) 0.7026(4) 0.6221(4) 0.0477(15) Uani 1 1 d . . . . .
C8A C 0.8809(2) 0.71905(16) 0.50371(15) 0.0229(6) Uani 1 1 d . . . . .
C9A C 0.8778(2) 0.63801(15) 0.51396(15) 0.0214(5) Uani 1 1 d . . . . .
C10A C 0.8741(2) 0.56633(16) 0.57859(17) 0.0284(6) Uani 1 1 d . . . . .
H10A H 0.8766(6) 0.5551(4) 0.6364(4) 0.0501(16) Uani 1 1 d . . . . .
C11A C 0.8715(2) 0.51107(17) 0.55035(17) 0.0316(7) Uani 1 1 d . . . . .
H11A H 0.8675(6) 0.4491(4) 0.5772(4) 0.0537(17) Uani 1 1 d . . . . .
C12A C 0.5422(2) 0.81711(16) 0.35047(16) 0.0244(6) Uani 1 1 d . . . . .
H12A H 0.4651(5) 0.8540(4) 0.3638(4) 0.0443(14) Uani 1 1 d . . . . .
C13A C 0.5764(2) 0.76955(16) 0.30637(16) 0.0233(6) Uani 1 1 d . . . . .
H13A H 0.5279(5) 0.7604(4) 0.2776(4) 0.0444(14) Uani 1 1 d . . . . .
C14A C 0.6833(2) 0.73571(14) 0.30953(15) 0.0192(5) Uani 1 1 d . . . . .
C15A C 0.7646(2) 0.68112(14) 0.27408(15) 0.0186(5) Uani 1 1 d . . . . .
C16A C 0.7451(2) 0.63726(15) 0.23951(15) 0.0213(6) Uani 1 1 d . . . . .
H16A H 0.6640(5) 0.6411(4) 0.2388(4) 0.0400(14) Uani 1 1 d . . . . .
C17A C 0.8318(2) 0.58871(15) 0.20765(16) 0.0229(6) Uani 1 1 d . . . . .
H17A H 0.8202(5) 0.5536(4) 0.1800(4) 0.0420(14) Uani 1 1 d . . . . .
C18A C 0.9338(2) 0.58377(15) 0.21144(15) 0.0213(6) Uani 1 1 d . . . . .
H18A H 1.0020(5) 0.5477(4) 0.1856(4) 0.0397(13) Uani 1 1 d . . . . .
C19A C 0.9464(2) 0.62871(14) 0.24797(14) 0.0179(5) Uani 1 1 d . . . . .
C20A C 1.0483(2) 0.63111(14) 0.25638(15) 0.0187(5) Uani 1 1 d . . . . .
C21A C 1.1537(2) 0.59540(16) 0.23036(16) 0.0228(6) Uani 1 1 d . . . . .
H21A H 1.1808(5) 0.5571(4) 0.1970(4) 0.0443(14) Uani 1 1 d . . . . .
C22A C 1.2141(2) 0.62314(15) 0.25479(16) 0.0241(6) Uani 1 1 d . . . . .
H22A H 1.2982(5) 0.6128(4) 0.2474(4) 0.0433(14) Uani 1 1 d . . . . .
Fe1B Fe 0.62268(13) 0.27431(9) 0.15337(10) 0.0151(3) Uani 1 1 d . . . . .
N1B N 0.62134(15) 0.10658(11) 0.28634(11) 0.0231(4) Uani 1 1 d . . . . .
H1NB H 0.6365(5) 0.1237(3) 0.3249(3) 0.0358(12) Uani 1 1 d . . . . .
N2B N 0.61622(14) 0.15862(10) 0.21486(10) 0.0197(4) Uani 1 1 d . . . . .
N3B N 0.61471(14) 0.23974(10) 0.07569(11) 0.0200(4) Uani 1 1 d . . . . .
N4B N 0.62699(15) 0.37531(10) 0.06191(11) 0.0212(4) Uani 1 1 d . . . . .
N5B N 0.63117(15) 0.45160(11) 0.04540(13) 0.0241(4) Uani 1 1 d . . . . .
H5NB H 0.6299(5) 0.4737(3) 0.0848(4) 0.0396(13) Uani 1 1 d . . . . .
N6B N 0.86333(15) 0.19507(10) 0.11279(11) 0.0217(4) Uani 1 1 d . . . . .
H6NB H 0.8596(5) 0.1754(3) 0.0715(3) 0.0343(12) Uani 1 1 d . . . . .
N7B N 0.78013(14) 0.24312(10) 0.14280(10) 0.0184(4) Uani 1 1 d . . . . .
N8B N 0.63854(14) 0.31914(10) 0.22048(11) 0.0187(4) Uani 1 1 d . . . . .
N9B N 0.47057(14) 0.31809(10) 0.19557(10) 0.0199(4) Uani 1 1 d . . . . .
N10B N 0.37364(15) 0.31987(11) 0.19179(11) 0.0237(4) Uani 1 1 d . . . . .
H10M H 1.1632(4) 0.7043(3) 0.3184(3) 0.0336(12) Uani 1 1 d . . . . .
C1B C 0.6201(2) 0.03158(16) 0.29441(16) 0.0248(6) Uani 1 1 d . . . . .
H1B H 0.6246(5) -0.0173(3) 0.3484(4) 0.0434(14) Uani 1 1 d . . . . .
C2B C 0.6135(2) 0.03513(15) 0.22333(16) 0.0251(6) Uani 1 1 d . . . . .
H2B H 0.6106(5) -0.0140(3) 0.2100(4) 0.0449(15) Uani 1 1 d . . . . .
C3B C 0.6117(2) 0.11601(14) 0.17545(15) 0.0203(5) Uani 1 1 d . . . . .
C4B C 0.6116(2) 0.16226(15) 0.09418(15) 0.0201(5) Uani 1 1 d . . . . .
C5B C 0.6138(2) 0.13421(17) 0.03886(16) 0.0249(6) Uani 1 1 d . . . . .
H5B H 0.6130(5) 0.0718(4) 0.0551(4) 0.0408(13) Uani 1 1 d . . . . .
C6B C 0.6175(2) 0.18881(16) -0.03709(16) 0.0250(6) Uani 1 1 d . . . . .
H6B H 0.6193(5) 0.1700(4) -0.0822(4) 0.0443(14) Uani 1 1 d . . . . .
C7B C 0.6208(2) 0.26864(16) -0.05599(16) 0.0249(6) Uani 1 1 d . . . . .
H7B H 0.6234(6) 0.3120(4) -0.1146(4) 0.0484(15) Uani 1 1 d . . . . .
C8B C 0.6196(2) 0.29190(15) 0.00261(15) 0.0214(5) Uani 1 1 d . . . . .
C9B C 0.6252(2) 0.37123(14) -0.00439(15) 0.0216(6) Uani 1 1 d . . . . .
C10B C 0.6287(2) 0.44674(16) -0.06459(17) 0.0281(6) Uani 1 1 d . . . . .
H10B H 0.6267(6) 0.4628(4) -0.1239(4) 0.0475(15) Uani 1 1 d . . . . .
C11B C 0.6323(2) 0.49656(16) -0.03019(17) 0.0279(6) Uani 1 1 d . . . . .
H11B H 0.6353(6) 0.5587(4) -0.0516(4) 0.0502(16) Uani 1 1 d . . . . .
C12B C 0.9505(2) 0.18358(15) 0.13775(16) 0.0239(6) Uani 1 1 d . . . . .
H12B H 1.0248(5) 0.1487(4) 0.1195(4) 0.0461(15) Uani 1 1 d . . . . .
C13B C 0.9236(2) 0.22625(15) 0.18603(16) 0.0224(6) Uani 1 1 d . . . . .
H13B H 0.9758(5) 0.2307(4) 0.2144(4) 0.0444(14) Uani 1 1 d . . . . .
C14B C 0.8160(2) 0.26248(14) 0.18758(14) 0.0179(5) Uani 1 1 d . . . . .
C15B C 0.7367(2) 0.31337(14) 0.22691(15) 0.0183(5) Uani 1 1 d . . . . .
C16B C 0.7538(2) 0.35575(15) 0.26415(15) 0.0216(6) Uani 1 1 d . . . . .
H16B H 0.8338(5) 0.3525(4) 0.2656(4) 0.0418(14) Uani 1 1 d . . . . .
C17B C 0.6659(2) 0.40234(15) 0.29731(16) 0.0238(6) Uani 1 1 d . . . . .
H17B H 0.6753(5) 0.4366(4) 0.3257(4) 0.0411(14) Uani 1 1 d . . . . .
C18B C 0.5647(2) 0.40716(15) 0.29166(15) 0.0206(5) Uani 1 1 d . . . . .
H18B H 0.4948(5) 0.4431(3) 0.3172(4) 0.0357(12) Uani 1 1 d . . . . .
C19B C 0.55327(19) 0.36451(14) 0.25247(14) 0.0177(5) Uani 1 1 d . . . . .
C20B C 0.4562(2) 0.36194(14) 0.23876(15) 0.0186(5) Uani 1 1 d . . . . .
C21B C 0.3474(2) 0.39192(16) 0.26321(17) 0.0239(6) Uani 1 1 d . . . . .
H21B H 0.3120(5) 0.4268(4) 0.2981(4) 0.0461(15) Uani 1 1 d . . . . .
C22B C 0.2971(2) 0.36368(16) 0.23179(16) 0.0249(6) Uani 1 1 d . . . . .
H22B H 0.2149(5) 0.3692(4) 0.2359(4) 0.0464(15) Uani 1 1 d . . . . .
O1A O 0.0796(3) 0.69183(18) 1.06448(18) 0.0252(7) Uani 1 1 d . . . . .
H1OB H 0.0851(5) 0.7424(4) 1.0857(4) 0.0420(14) Uani 1 1 d . . . . .
O2A O -0.0868(3) 0.75797(18) 1.0508(2) 0.0285(7) Uani 1 1 d . . . . .
O3A O 0.0202(3) 0.53439(19) 0.8645(2) 0.0327(8) Uani 1 1 d . . . . .
N11A N 0.01320(16) 0.57193(11) 0.90858(11) 0.0251(4) Uani 1 1 d . . . . .
C23A C -0.0056(2) 0.70584(15) 1.04210(15) 0.0216(5) Uani 1 1 d . . . . .
C24A C -0.0006(2) 0.65424(14) 1.00039(15) 0.0207(5) Uani 1 1 d . . . . .
C25A C 0.0945(2) 0.60293(15) 0.97988(16) 0.0237(6) Uani 1 1 d . . . . .
H25A H 0.1644(5) 0.5955(4) 0.9992(4) 0.0425(14) Uani 1 1 d . . . . .
C26A C -0.0887(2) 0.66067(16) 0.97558(16) 0.0243(6) Uani 1 1 d . . . . .
H26A H -0.1632(5) 0.6997(4) 0.9907(4) 0.0494(16) Uani 1 1 d . . . . .
C27A C -0.0808(2) 0.61902(16) 0.93039(17) 0.0260(6) Uani 1 1 d . . . . .
H27A H -0.1465(5) 0.6205(4) 0.9094(4) 0.0484(16) Uani 1 1 d . . . . .
C28A C 0.0999(2) 0.56244(15) 0.93402(16) 0.0241(6) Uani 1 1 d . . . . .
H28A H 0.1707(5) 0.5230(4) 0.9138(4) 0.0439(14) Uani 1 1 d . . . . .
O4A O 0.3820(3) 0.11948(18) 0.51849(18) 0.0258(7) Uani 1 1 d . . . . .
O5A O 0.4137(3) 0.20870(19) 0.3969(2) 0.0327(8) Uani 1 1 d . . . . .
H1OA H 0.4209(5) 0.2543(4) 0.4222(4) 0.0419(14) Uani 1 1 d . . . . .
O6A O 0.3330(2) -0.05283(19) 0.32229(18) 0.0254(7) Uani 1 1 d . . . . .
N12A N 0.34616(15) -0.00699(11) 0.35145(11) 0.0211(4) Uani 1 1 d . . . . .
C29A C 0.3917(2) 0.14225(15) 0.44780(15) 0.0220(6) Uani 1 1 d . . . . .
C30A C 0.3761(2) 0.08938(14) 0.41414(15) 0.0212(5) Uani 1 1 d . . . . .
H30A H 0.3657(5) 0.1830(3) 0.3030(3) 0.0402(14) Uani 1 1 d . . . . .
C31A C 0.3728(2) 0.00877(15) 0.45764(15) 0.0202(5) Uani 1 1 d . . . . .
H31A H 0.3827(6) -0.0181(4) 0.5166(3) 0.0428(14) Uani 1 1 d . . . . .
C32A C 0.3631(2) 0.12029(15) 0.33869(16) 0.0223(6) Uani 1 1 d . . . . .
C33A C 0.3480(2) 0.07191(15) 0.30818(16) 0.0220(6) Uani 1 1 d . . . . .
H33A H 0.3357(5) 0.0925(4) 0.2506(3) 0.0415(14) Uani 1 1 d . . . . .
C34A C 0.3582(2) -0.03837(15) 0.42543(16) 0.0230(6) Uani 1 1 d . . . . .
H34A H 0.3567(5) -0.1020(3) 0.4555(3) 0.0395(13) Uani 1 1 d . . . . .
O7A O 0.1579(3) 0.66111(19) 0.45976(19) 0.0304(7) Uani 1 1 d . . . . .
O8A O 0.1827(3) 0.76567(19) 0.35100(19) 0.0283(7) Uani 1 1 d . . . . .
O9A O 0.1089(3) 0.92758(19) 0.58900(19) 0.0268(7) Uani 1 1 d . . . . .
N13A N 0.11779(15) 0.88272(11) 0.54974(11) 0.0239(4) Uani 1 1 d . . . . .
C35A C 0.1636(2) 0.73341(15) 0.42273(15) 0.0225(6) Uani 1 1 d . . . . .
C36A C 0.1465(2) 0.78626(15) 0.46777(15) 0.0201(5) Uani 1 1 d . . . . .
C37A C 0.1419(2) 0.86889(16) 0.43077(17) 0.0247(6) Uani 1 1 d . . . . .
H37A H 0.1510(6) 0.8968(4) 0.3697(4) 0.0480(16) Uani 1 1 d . . . . .
C38A C 0.1342(2) 0.75377(15) 0.54778(16) 0.0248(6) Uani 1 1 d . . . . .
H38A H 0.1366(6) 0.6900(3) 0.5806(4) 0.0471(15) Uani 1 1 d . . . . .
C39A C 0.1203(2) 0.80296(16) 0.58761(17) 0.0271(6) Uani 1 1 d . . . . .
H39A H 0.1115(6) 0.7828(4) 0.6495(4) 0.0490(16) Uani 1 1 d . . . . .
C40A C 0.1268(2) 0.91613(15) 0.47252(16) 0.0241(6) Uani 1 1 d . . . . .
H40A H 0.1229(6) 0.9803(4) 0.4461(4) 0.0487(16) Uani 1 1 d . . . . .
O1B O 0.4235(3) 0.30620(18) 0.4431(2) 0.0280(7) Uani 1 1 d . . . . .
O2B O 0.5894(3) 0.24094(19) 0.4602(2) 0.0301(7) Uani 1 1 d . . . . .
O3B O 0.4792(3) 0.47131(19) 0.6388(2) 0.0338(8) Uani 1 1 d . . . . .
N11B N 0.48578(16) 0.43258(11) 0.59546(11) 0.0248(4) Uani 1 1 d . . . . .
C23B C 0.5075(2) 0.29380(15) 0.46629(16) 0.0242(6) Uani 1 1 d . . . . .
C24B C 0.5011(2) 0.34706(15) 0.50637(16) 0.0220(5) Uani 1 1 d . . . . .
C25B C 0.4062(2) 0.39905(15) 0.52527(16) 0.0238(6) Uani 1 1 d . . . . .
H25B H 0.3366(5) 0.4047(4) 0.5062(4) 0.0459(15) Uani 1 1 d . . . . .
C26B C 0.5892(2) 0.34149(16) 0.53100(16) 0.0246(6) Uani 1 1 d . . . . .
H26B H 0.6635(5) 0.3027(4) 0.5167(4) 0.0449(15) Uani 1 1 d . . . . .
C27B C 0.5802(2) 0.38516(16) 0.57511(17) 0.0277(6) Uani 1 1 d . . . . .
H27B H 0.6451(5) 0.3848(4) 0.5962(4) 0.0486(16) Uani 1 1 d . . . . .
C28B C 0.3992(2) 0.44140(16) 0.57007(16) 0.0246(6) Uani 1 1 d . . . . .
H28B H 0.3285(5) 0.4804(4) 0.5890(4) 0.0451(15) Uani 1 1 d . . . . .
O4B O 0.1229(3) 0.87567(18) 0.98759(19) 0.0265(7) Uani 1 1 d . . . . .
O5B O 0.0961(3) 0.78841(19) 1.10975(19) 0.0300(7) Uani 1 1 d . . . . .
O6B O 0.1646(3) 1.06274(19) 1.17306(18) 0.0257(7) Uani 1 1 d . . . . .
N12B N 0.15595(15) 1.01319(11) 1.14578(11) 0.0213(4) Uani 1 1 d . . . . .
C29B C 0.1156(2) 0.85473(15) 1.05767(15) 0.0218(5) Uani 1 1 d . . . . .
C30B C 0.1310(2) 0.91048(14) 1.08810(15) 0.0209(5) Uani 1 1 d . . . . .
C31B C 0.1323(2) 0.99058(15) 1.04222(16) 0.0219(6) Uani 1 1 d . . . . .
H31B H 0.1221(5) 1.0149(3) 0.9830(3) 0.0400(14) Uani 1 1 d . . . . .
C32B C 0.1441(2) 0.88270(15) 1.16328(16) 0.0229(6) Uani 1 1 d . . . . .
H32B H 0.1440(5) 0.8201(3) 1.2017(3) 0.0403(14) Uani 1 1 d . . . . .
C33B C 0.1574(2) 0.93431(15) 1.19096(16) 0.0238(6) Uani 1 1 d . . . . .
H33B H 0.1697(6) 0.9167(4) 1.2485(3) 0.0424(14) Uani 1 1 d . . . . .
C34B C 0.1448(2) 1.04078(16) 1.07217(15) 0.0226(6) Uani 1 1 d . . . . .
H34B H 0.1450(5) 1.1038(3) 1.0396(3) 0.0394(13) Uani 1 1 d . . . . .
O7B O 0.3401(3) 0.33178(18) 1.03057(18) 0.0277(7) Uani 1 1 d . . . . .
O8B O 0.3312(3) 0.22481(19) 1.13968(18) 0.0278(7) Uani 1 1 d . . . . .
O9B O 0.3795(3) 0.06383(19) 0.90581(19) 0.0276(7) Uani 1 1 d . . . . .
N13B N 0.37408(15) 0.10878(11) 0.94402(11) 0.0242(4) Uani 1 1 d . . . . .
C35B C 0.3411(2) 0.25798(15) 1.06770(15) 0.0217(5) Uani 1 1 d . . . . .
C36B C 0.3539(2) 0.20548(15) 1.02379(15) 0.0206(5) Uani 1 1 d . . . . .
C37B C 0.3645(2) 0.12214(16) 1.06084(16) 0.0239(6) Uani 1 1 d . . . . .
H37B H 0.3625(5) 0.0939(3) 1.1219(3) 0.0398(14) Uani 1 1 d . . . . .
C38B C 0.3556(2) 0.23823(15) 0.94528(15) 0.0235(6) Uani 1 1 d . . . . .
H38B H 0.3480(6) 0.3026(3) 0.9129(4) 0.0446(15) Uani 1 1 d . . . . .
C39B C 0.3651(2) 0.18972(16) 0.90630(16) 0.0250(6) Uani 1 1 d . . . . .
H39B H 0.3644(6) 0.2098(4) 0.8462(4) 0.0498(16) Uani 1 1 d . . . . .
C40B C 0.3755(2) 0.07466(15) 1.02007(16) 0.0235(6) Uani 1 1 d . . . . .
H40B H 0.3838(5) 0.0104(3) 1.0449(4) 0.0426(14) Uani 1 1 d . . . . .
O1WA O 0.5885(4) 0.0739(2) 0.8190(2) 0.0296(7) Uani 1 1 d . . . . .
H1C H 0.5150(6) 0.0690(3) 0.8400(4) 0.0388(13) Uani 1 1 d . . . . .
H1D H 0.6137(5) 0.0585(4) 0.7740(4) 0.0405(14) Uani 1 1 d . . . . .
O1WB O 0.9043(3) 0.9195(2) 0.6829(2) 0.0276(7) Uani 1 1 d . . . . .
H1E H 0.8817(6) 0.9355(4) 0.7280(5) 0.0456(15) Uani 1 1 d . . . . .
H1F H 0.9780(5) 0.9246(3) 0.6585(4) 0.0359(12) Uani 1 1 d . . . . .
O2WA O 0.3756(3) 0.7717(2) 0.2332(3) 0.0297(8) Uani 1 1 d . . . . .
H2C H 0.3137(7) 0.7708(4) 0.2754(4) 0.0437(15) Uani 1 1 d . . . . .
H2D H 0.3884(5) 0.8253(4) 0.2134(4) 0.0410(14) Uani 1 1 d . . . . .
O2WB O 0.1335(4) 0.2336(2) 0.2574(3) 0.0324(8) Uani 1 1 d . . . . .
H2E H 0.1208(5) 0.1802(4) 0.2786(4) 0.0435(14) Uani 1 1 d . . . . .
H2F H 0.1942(7) 0.2332(4) 0.2152(5) 0.0467(15) Uani 1 1 d . . . . .
O3WA O 0.8277(4) 0.8640(2) 0.1281(2) 0.0332(8) Uani 1 1 d . . . . .
H3C H 0.7579(6) 0.8881(4) 0.1189(4) 0.0409(14) Uani 1 1 d . . . . .
H3D H 0.8617(5) 0.8242(4) 0.1043(4) 0.0414(14) Uani 1 1 d . . . . .
O3WB O 0.6841(4) 0.1428(2) 0.3796(2) 0.0329(8) Uani 1 1 d . . . . .
H3E H 0.6493(5) 0.1803(4) 0.4044(4) 0.0384(13) Uani 1 1 d . . . . .
H3F H 0.7556(5) 0.1185(4) 0.3873(4) 0.0400(13) Uani 1 1 d . . . . .
O4WA O 0.1367(3) 0.5442(2) 0.6015(3) 0.0330(8) Uani 1 1 d . . . . .
H4C H 0.0865(6) 0.5634(5) 0.6416(4) 0.0491(16) Uani 1 1 d . . . . .
H4D H 0.1396(5) 0.5914(4) 0.5537(4) 0.0424(14) Uani 1 1 d . . . . .
O4WB O 0.3616(3) 0.4489(2) 0.8876(3) 0.0339(8) Uani 1 1 d . . . . .
H4E H 0.3587(6) 0.4036(4) 0.9354(4) 0.0463(15) Uani 1 1 d . . . . .
H4F H 0.4139(6) 0.4289(4) 0.8495(4) 0.0429(14) Uani 1 1 d . . . . .
O5WA O 0.9977(3) 0.6251(3) 0.7158(2) 0.0375(8) Uani 1 1 d . . . . .
H5C H 1.0065(5) 0.5924(4) 0.7676(4) 0.0448(14) Uani 1 1 d . . . . .
H5D H 0.9550(6) 0.6759(4) 0.7184(4) 0.0431(14) Uani 1 1 d . . . . .
O5WB O 0.5122(3) 0.3766(3) 0.7821(2) 0.0365(8) Uani 1 1 d . . . . .
H5E H 0.5021(5) 0.4099(4) 0.7303(4) 0.0428(14) Uani 1 1 d . . . . .
H5F H 0.5462(5) 0.3237(4) 0.7816(4) 0.0424(14) Uani 1 1 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
Fe1A N8A 2.106(2) . ?
Fe1A N3A 2.128(2) . ?
Fe1A N2A 2.145(2) . ?
Fe1A N4A 2.175(2) . ?
Fe1A N9A 2.180(3) . ?
Fe1A N7A 2.184(2) . ?
N1A N2A 1.338(3) . ?
N1A C1A 1.350(3) . ?
N1A H1NA 1.041(7) . ?
N2A C3A 1.342(3) . ?
N3A C8A 1.337(3) . ?
N3A C4A 1.350(3) . ?
N4A C9A 1.337(3) . ?
N4A N5A 1.340(3) . ?
N5A C11A 1.345(4) . ?
N5A H5NA 1.007(8) . ?
N6A N7A 1.337(3) . ?
N6A C12A 1.352(3) . ?
N6A H6NA 1.028(6) . ?
N7A C14A 1.342(3) . ?
N8A C15A 1.337(3) . ?
N8A C19A 1.338(3) . ?
N9A N10A 1.340(3) . ?
N9A C20A 1.346(3) . ?
N10A C22A 1.345(4) . ?
N10A H10M 1.062(6) . ?
C1A C2A 1.388(4) . ?
C1A H1A 1.067(7) . ?
C2A C3A 1.402(3) . ?
C2A H2A 1.059(7) . ?
C3A C4A 1.465(4) . ?
C4A C5A 1.384(4) . ?
C5A C6A 1.385(4) . ?
C5A H5A 1.089(6) . ?
C6A C7A 1.398(4) . ?
C6A H6A 1.073(7) . ?
C7A C8A 1.395(4) . ?
C7A H7A 1.079(7) . ?
C8A C9A 1.458(4) . ?
C9A C10A 1.401(4) . ?
C10A C11A 1.382(4) . ?
C10A H10A 1.072(7) . ?
C11A H11A 1.063(7) . ?
C12A C13A 1.376(4) . ?
C12A H12A 1.073(7) . ?
C13A C14A 1.395(4) . ?
C13A H13A 1.085(6) . ?
C14A C15A 1.460(4) . ?
C15A C16A 1.394(3) . ?
C16A C17A 1.386(4) . ?
C16A H16A 1.084(6) . ?
C17A C18A 1.383(4) . ?
C17A H17A 1.087(6) . ?
C18A C19A 1.394(3) . ?
C18A H18A 1.076(7) . ?
C19A C20A 1.463(3) . ?
C20A C21A 1.399(4) . ?
C21A C22A 1.386(4) . ?
C21A H21A 1.075(7) . ?
C22A H22A 1.066(7) . ?
Fe1B N8B 1.933(2) . ?
Fe1B N3B 1.938(2) . ?
Fe1B N4B 1.977(2) . ?
Fe1B N7B 1.992(2) . ?
Fe1B N2B 1.996(2) . ?
Fe1B N9B 2.001(3) . ?
N1B N2B 1.331(3) . ?
N1B C1B 1.351(3) . ?
N1B H1NB 1.034(7) . ?
N2B C3B 1.353(3) . ?
N3B C8B 1.341(3) . ?
N3B C4B 1.350(3) . ?
N4B N5B 1.341(3) . ?
N4B C9B 1.344(3) . ?
N5B C11B 1.355(4) . ?
N5B H5NB 1.015(8) . ?
N6B N7B 1.341(3) . ?
N6B C12B 1.345(3) . ?
N6B H6NB 1.043(6) . ?
N7B C14B 1.344(3) . ?
N8B C19B 1.344(3) . ?
N8B C15B 1.346(3) . ?
N9B N10B 1.332(3) . ?
N9B C20B 1.348(3) . ?
N10B C22B 1.357(4) . ?
N10B H10N 1.054(6) . ?
C1B C2B 1.399(4) . ?
C1B H1B 1.068(7) . ?
C2B C3B 1.398(3) . ?
C2B H2B 1.075(6) . ?
C3B C4B 1.454(4) . ?
C4B C5B 1.383(4) . ?
C5B C6B 1.397(4) . ?
C5B H5B 1.076(7) . ?
C6B C7B 1.392(4) . ?
C6B H6B 1.075(7) . ?
C7B C8B 1.388(4) . ?
C7B H7B 1.085(7) . ?
C8B C9B 1.459(3) . ?
C9B C10B 1.407(4) . ?
C10B C11B 1.387(4) . ?
C10B H10B 1.078(7) . ?
C11B H11B 1.067(6) . ?
C12B C13B 1.381(4) . ?
C12B H12B 1.055(7) . ?
C13B C14B 1.395(3) . ?
C13B H13B 1.074(6) . ?
C14B C15B 1.446(4) . ?
C15B C16B 1.395(3) . ?
C16B C17B 1.385(4) . ?
C16B H16B 1.079(6) . ?
C17B C18B 1.386(4) . ?
C17B H17B 1.070(6) . ?
C18B C19B 1.393(3) . ?
C18B H18B 1.084(7) . ?
C19B C20B 1.447(3) . ?
C20B C21B 1.402(4) . ?
C21B C22B 1.384(4) . ?
C21B H21B 1.046(8) . ?
C22B H22B 1.067(7) . ?
O1A C23A 1.279(4) . ?
O1A H1OB 1.216(7) . ?
O2A C23A 1.234(4) . ?
O3A N11A 1.296(4) . ?
N11A C27A 1.354(4) . ?
N11A C28A 1.355(3) . ?
C23A C24A 1.487(3) . ?
C24A C26A 1.385(4) . ?
C24A C25A 1.395(4) . ?
C25A C28A 1.378(4) . ?
C25A H25A 1.081(6) . ?
C26A C27A 1.373(4) . ?
C26A H26A 1.077(7) . ?
C27A H27A 1.085(6) . ?
C28A H28A 1.083(7) . ?
O4A C29A 1.239(4) . ?
O5A C29A 1.274(4) . ?
O5A H1OA 1.199(7) . ?
O6A N12A 1.299(4) . ?
N12A C34A 1.357(3) . ?
N12A C33A 1.358(3) . ?
C29A C30A 1.500(3) . ?
C30A C32A 1.388(4) . ?
C30A C31A 1.389(3) . ?
C31A C34A 1.376(4) . ?
C31A H31A 1.080(6) . ?
C32A C33A 1.375(4) . ?
C32A H30A 1.087(6) . ?
C33A H33A 1.078(6) . ?
C34A H34A 1.086(6) . ?
O7A C35A 1.249(4) . ?
O8A C35A 1.246(4) . ?
O9A N13A 1.321(4) . ?
N13A C40A 1.349(3) . ?
N13A C39A 1.350(3) . ?
C35A C36A 1.512(4) . ?
C36A C37A 1.391(4) . ?
C36A C38A 1.394(4) . ?
C37A C40A 1.376(4) . ?
C37A H37A 1.065(8) . ?
C38A C39A 1.381(4) . ?
C38A H38A 1.084(6) . ?
C39A H39A 1.085(7) . ?
C40A H40A 1.077(6) . ?
O1B C23B 1.280(4) . ?
O1B H1OA 1.221(7) . ?
O2B C23B 1.239(4) . ?
O3B N11B 1.302(4) . ?
N11B C27B 1.353(4) . ?
N11B C28B 1.358(3) . ?
C23B C24B 1.482(4) . ?
C24B C26B 1.389(4) . ?
C24B C25B 1.391(4) . ?
C25B C28B 1.381(4) . ?
C25B H25B 1.084(6) . ?
C26B C27B 1.382(4) . ?
C26B H26B 1.069(7) . ?
C27B H27B 1.086(7) . ?
C28B H28B 1.068(8) . ?
O4B C29B 1.237(4) . ?
O5B C29B 1.269(4) . ?
O5B H1OB 1.213(7) . ?
O6B N12B 1.304(4) . ?
N12B C34B 1.352(3) . ?
N12B C33B 1.358(3) . ?
C29B C30B 1.500(3) . ?
C30B C31B 1.384(4) . ?
C30B C32B 1.390(4) . ?
C31B C34B 1.380(4) . ?
C31B H31B 1.089(6) . ?
C32B C33B 1.376(4) . ?
C32B H32B 1.090(6) . ?
C33B H33B 1.086(6) . ?
C34B H34B 1.077(6) . ?
O7B C35B 1.256(4) . ?
O8B C35B 1.257(4) . ?
O9B N13B 1.320(4) . ?
N13B C40B 1.353(3) . ?
N13B C39B 1.358(3) . ?
C35B C36B 1.504(3) . ?
C36B C38B 1.388(4) . ?
C36B C37B 1.393(4) . ?
C37B C40B 1.379(4) . ?
C37B H37B 1.078(6) . ?
C38B C39B 1.373(4) . ?
C38B H38B 1.085(6) . ?
C39B H39B 1.077(7) . ?
C40B H40B 1.071(6) . ?
O1WA H1C 0.968(11) . ?
O1WA H1D 0.969(10) . ?
O1WB H1E 0.980(11) . ?
O1WB H1F 0.976(10) . ?
O2WA H2C 0.969(12) . ?
O2WA H2D 0.963(9) . ?
O2WB H2E 0.956(10) . ?
O2WB H2F 0.960(13) . ?
O3WA H3C 0.948(10) . ?
O3WA H3D 0.962(9) . ?
O3WB H3E 0.939(10) . ?
O3WB H3F 0.961(9) . ?
O4WA H4C 0.974(12) . ?
O4WA H4D 0.976(9) . ?
O4WB H4E 0.959(10) . ?
O4WB H4F 0.963(12) . ?
O5WA H5C 0.961(10) . ?
O5WA H5D 0.954(10) . ?
O5WB H5E 0.967(9) . ?
O5WB H5F 0.952(9) . ?

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
N8A Fe1A N3A 168.00(12) . . ?
N8A Fe1A N2A 116.33(10) . . ?
N3A Fe1A N2A 74.18(9) . . ?
N8A Fe1A N4A 95.17(9) . . ?
N3A Fe1A N4A 74.04(9) . . ?
N2A Fe1A N4A 148.18(11) . . ?
N8A Fe1A N9A 74.42(9) . . ?
N3A Fe1A N9A 110.58(10) . . ?
N2A Fe1A N9A 100.13(10) . . ?
N4A Fe1A N9A 92.16(9) . . ?
N8A Fe1A N7A 74.86(8) . . ?
N3A Fe1A N7A 100.14(10) . . ?
N2A Fe1A N7A 90.77(9) . . ?
N4A Fe1A N7A 93.48(9) . . ?
N9A Fe1A N7A 149.14(11) . . ?
N2A N1A C1A 111.7(2) . . ?
N2A N1A H1NA 118.8(3) . . ?
C1A N1A H1NA 129.1(4) . . ?
N1A N2A C3A 105.78(18) . . ?
N1A N2A Fe1A 136.84(15) . . ?
C3A N2A Fe1A 117.32(16) . . ?
C8A N3A C4A 120.5(2) . . ?
C8A N3A Fe1A 119.57(16) . . ?
C4A N3A Fe1A 119.65(16) . . ?
C9A N4A N5A 106.11(19) . . ?
C9A N4A Fe1A 116.13(16) . . ?
N5A N4A Fe1A 137.77(17) . . ?
N4A N5A C11A 111.1(2) . . ?
N4A N5A H5NA 121.9(4) . . ?
C11A N5A H5NA 126.8(4) . . ?
N7A N6A C12A 111.3(2) . . ?
N7A N6A H6NA 120.8(4) . . ?
C12A N6A H6NA 127.6(4) . . ?
N6A N7A C14A 105.78(18) . . ?
N6A N7A Fe1A 138.62(14) . . ?
C14A N7A Fe1A 114.18(16) . . ?
C15A N8A C19A 120.00(19) . . ?
C15A N8A Fe1A 119.72(16) . . ?
C19A N8A Fe1A 119.97(15) . . ?
N10A N9A C20A 105.33(19) . . ?
N10A N9A Fe1A 139.46(15) . . ?
C20A N9A Fe1A 115.13(15) . . ?
N9A N10A C22A 112.00(19) . . ?
N9A N10A H10M 119.0(4) . . ?
C22A N10A H10M 129.0(4) . . ?
N1A C1A C2A 107.4(2) . . ?
N1A C1A H1A 119.8(5) . . ?
C2A C1A H1A 132.8(5) . . ?
C1A C2A C3A 104.2(2) . . ?
C1A C2A H2A 126.3(4) . . ?
C3A C2A H2A 129.5(4) . . ?
N2A C3A C2A 110.9(2) . . ?
N2A C3A C4A 116.2(2) . . ?
C2A C3A C4A 132.8(2) . . ?
N3A C4A C5A 121.5(2) . . ?
N3A C4A C3A 112.6(2) . . ?
C5A C4A C3A 125.9(2) . . ?
C4A C5A C6A 118.5(2) . . ?
C4A C5A H5A 120.1(4) . . ?
C6A C5A H5A 121.4(4) . . ?
C5A C6A C7A 120.2(3) . . ?
C5A C6A H6A 120.3(4) . . ?
C7A C6A H6A 119.5(5) . . ?
C8A C7A C6A 118.0(3) . . ?
C8A C7A H7A 121.0(4) . . ?
C6A C7A H7A 121.0(5) . . ?
N3A C8A C7A 121.4(2) . . ?
N3A C8A C9A 113.4(2) . . ?
C7A C8A C9A 125.2(2) . . ?
N4A C9A C10A 110.7(2) . . ?
N4A C9A C8A 116.7(2) . . ?
C10A C9A C8A 132.6(3) . . ?
C11A C10A C9A 104.2(3) . . ?
C11A C10A H10A 127.1(4) . . ?
C9A C10A H10A 128.6(4) . . ?
N5A C11A C10A 107.8(2) . . ?
N5A C11A H11A 119.7(5) . . ?
C10A C11A H11A 132.5(5) . . ?
N6A C12A C13A 107.5(2) . . ?
N6A C12A H12A 122.6(4) . . ?
C13A C12A H12A 129.9(4) . . ?
C12A C13A C14A 104.7(2) . . ?
C12A C13A H13A 126.0(4) . . ?
C14A C13A H13A 129.3(4) . . ?
N7A C14A C13A 110.8(2) . . ?
N7A C14A C15A 117.3(2) . . ?
C13A C14A C15A 131.9(2) . . ?
N8A C15A C16A 121.9(2) . . ?
N8A C15A C14A 112.9(2) . . ?
C16A C15A C14A 125.2(2) . . ?
C17A C16A C15A 117.9(2) . . ?
C17A C16A H16A 122.1(4) . . ?
C15A C16A H16A 120.0(4) . . ?
C18A C17A C16A 120.4(2) . . ?
C18A C17A H17A 119.3(4) . . ?
C16A C17A H17A 120.4(4) . . ?
C17A C18A C19A 118.2(2) . . ?
C17A C18A H18A 121.3(4) . . ?
C19A C18A H18A 120.5(4) . . ?
N8A C19A C18A 121.6(2) . . ?
N8A C19A C20A 113.1(2) . . ?
C18A C19A C20A 125.3(2) . . ?
N9A C20A C21A 110.9(2) . . ?
N9A C20A C19A 116.7(2) . . ?
C21A C20A C19A 132.3(2) . . ?
C22A C21A C20A 104.4(2) . . ?
C22A C21A H21A 128.3(4) . . ?
C20A C21A H21A 127.3(4) . . ?
N10A C22A C21A 107.4(2) . . ?
N10A C22A H22A 121.3(4) . . ?
C21A C22A H22A 131.3(4) . . ?
N8B Fe1B N3B 172.97(12) . . ?
N8B Fe1B N4B 94.35(10) . . ?
N3B Fe1B N4B 79.17(10) . . ?
N8B Fe1B N7B 79.03(9) . . ?
N3B Fe1B N7B 98.58(11) . . ?
N4B Fe1B N7B 94.00(10) . . ?
N8B Fe1B N2B 107.66(10) . . ?
N3B Fe1B N2B 78.78(9) . . ?
N4B Fe1B N2B 157.95(12) . . ?
N7B Fe1B N2B 88.91(9) . . ?
N8B Fe1B N9B 78.57(9) . . ?
N3B Fe1B N9B 104.02(10) . . ?
N4B Fe1B N9B 90.69(10) . . ?
N7B Fe1B N9B 157.39(11) . . ?
N2B Fe1B N9B 94.98(10) . . ?
N2B N1B C1B 111.3(2) . . ?
N2B N1B H1NB 120.2(3) . . ?
C1B N1B H1NB 127.9(4) . . ?
N1B N2B C3B 106.44(18) . . ?
N1B N2B Fe1B 137.63(15) . . ?
C3B N2B Fe1B 115.77(16) . . ?
C8B N3B C4B 120.5(2) . . ?
C8B N3B Fe1B 119.36(16) . . ?
C4B N3B Fe1B 120.01(16) . . ?
N5B N4B C9B 106.42(19) . . ?
N5B N4B Fe1B 137.54(17) . . ?
C9B N4B Fe1B 116.04(15) . . ?
N4B N5B C11B 111.2(2) . . ?
N4B N5B H5NB 124.6(4) . . ?
C11B N5B H5NB 124.2(4) . . ?
N7B N6B C12B 110.7(2) . . ?
N7B N6B H6NB 122.4(4) . . ?
C12B N6B H6NB 126.6(4) . . ?
N6B N7B C14B 106.27(18) . . ?
N6B N7B Fe1B 137.56(14) . . ?
C14B N7B Fe1B 114.99(16) . . ?
C19B N8B C15B 120.17(19) . . ?
C19B N8B Fe1B 119.79(15) . . ?
C15B N8B Fe1B 119.50(17) . . ?
N10B N9B C20B 106.27(19) . . ?
N10B N9B Fe1B 138.53(16) . . ?
C20B N9B Fe1B 115.14(15) . . ?
N9B N10B C22B 111.14(19) . . ?
N9B N10B H10N 122.3(4) . . ?
C22B N10B H10N 126.3(4) . . ?
N1B C1B C2B 107.7(2) . . ?
N1B C1B H1B 120.4(4) . . ?
C2B C1B H1B 131.9(4) . . ?
C3B C2B C1B 104.1(2) . . ?
C3B C2B H2B 129.1(4) . . ?
C1B C2B H2B 126.8(4) . . ?
N2B C3B C2B 110.5(2) . . ?
N2B C3B C4B 114.4(2) . . ?
C2B C3B C4B 134.9(2) . . ?
N3B C4B C5B 121.4(2) . . ?
N3B C4B C3B 111.0(2) . . ?
C5B C4B C3B 127.5(2) . . ?
C4B C5B C6B 118.1(2) . . ?
C4B C5B H5B 119.8(4) . . ?
C6B C5B H5B 122.1(4) . . ?
C7B C6B C5B 120.3(2) . . ?
C7B C6B H6B 118.7(4) . . ?
C5B C6B H6B 121.0(4) . . ?
C8B C7B C6B 118.1(3) . . ?
C8B C7B H7B 120.4(4) . . ?
C6B C7B H7B 121.5(4) . . ?
N3B C8B C7B 121.5(2) . . ?
N3B C8B C9B 111.1(2) . . ?
C7B C8B C9B 127.3(2) . . ?
N4B C9B C10B 110.3(2) . . ?
N4B C9B C8B 114.2(2) . . ?
C10B C9B C8B 135.5(3) . . ?
C11B C10B C9B 104.6(2) . . ?
C11B C10B H10B 127.6(4) . . ?
C9B C10B H10B 127.7(5) . . ?
N5B C11B C10B 107.5(2) . . ?
N5B C11B H11B 119.5(5) . . ?
C10B C11B H11B 133.0(5) . . ?
N6B C12B C13B 108.1(2) . . ?
N6B C12B H12B 122.3(4) . . ?
C13B C12B H12B 129.5(4) . . ?
C12B C13B C14B 104.5(2) . . ?
C12B C13B H13B 126.6(4) . . ?
C14B C13B H13B 128.9(4) . . ?
N7B C14B C13B 110.4(2) . . ?
N7B C14B C15B 114.9(2) . . ?
C13B C14B C15B 134.6(2) . . ?
N8B C15B C16B 121.7(2) . . ?
N8B C15B C14B 110.7(2) . . ?
C16B C15B C14B 127.6(2) . . ?
C17B C16B C15B 118.2(2) . . ?
C17B C16B H16B 121.9(4) . . ?
C15B C16B H16B 119.9(4) . . ?
C16B C17B C18B 120.0(2) . . ?
C16B C17B H17B 120.8(4) . . ?
C18B C17B H17B 119.2(4) . . ?
C17B C18B C19B 119.0(2) . . ?
C17B C18B H18B 121.4(4) . . ?
C19B C18B H18B 119.7(4) . . ?
N8B C19B C18B 121.0(2) . . ?
N8B C19B C20B 110.9(2) . . ?
C18B C19B C20B 128.1(2) . . ?
N9B C20B C21B 110.6(2) . . ?
N9B C20B C19B 114.7(2) . . ?
C21B C20B C19B 134.6(2) . . ?
C22B C21B C20B 104.3(3) . . ?
C22B C21B H21B 127.7(4) . . ?
C20B C21B H21B 128.0(4) . . ?
N10B C22B C21B 107.7(2) . . ?
N10B C22B H22B 120.2(4) . . ?
C21B C22B H22B 132.0(5) . . ?
C23A O1A H1OB 115.4(4) . . ?
O3A N11A C27A 120.1(2) . . ?
O3A N11A C28A 119.7(2) . . ?
C27A N11A C28A 120.2(2) . . ?
O2A C23A O1A 126.0(3) . . ?
O2A C23A C24A 119.7(3) . . ?
O1A C23A C24A 114.3(3) . . ?
C26A C24A C25A 118.1(2) . . ?
C26A C24A C23A 120.5(2) . . ?
C25A C24A C23A 121.2(2) . . ?
C28A C25A C24A 120.0(2) . . ?
C28A C25A H25A 119.8(4) . . ?
C24A C25A H25A 120.1(4) . . ?
C27A C26A C24A 120.3(3) . . ?
C27A C26A H26A 119.9(4) . . ?
C24A C26A H26A 119.7(4) . . ?
N11A C27A C26A 120.7(2) . . ?
N11A C27A H27A 114.9(4) . . ?
C26A C27A H27A 124.5(4) . . ?
N11A C28A C25A 120.5(2) . . ?
N11A C28A H28A 114.4(4) . . ?
C25A C28A H28A 125.1(4) . . ?
C29A O5A H1OA 114.7(4) . . ?
O6A N12A C34A 119.6(2) . . ?
O6A N12A C33A 120.2(2) . . ?
C34A N12A C33A 120.1(2) . . ?
O4A C29A O5A 127.1(3) . . ?
O4A C29A C30A 120.0(2) . . ?
O5A C29A C30A 113.0(3) . . ?
C32A C30A C31A 118.2(2) . . ?
C32A C30A C29A 120.6(2) . . ?
C31A C30A C29A 121.1(2) . . ?
C34A C31A C30A 120.0(2) . . ?
C34A C31A H31A 119.1(4) . . ?
C30A C31A H31A 121.0(4) . . ?
C33A C32A C30A 120.5(2) . . ?
C33A C32A H30A 119.5(4) . . ?
C30A C32A H30A 120.0(4) . . ?
N12A C33A C32A 120.3(2) . . ?
N12A C33A H33A 115.5(4) . . ?
C32A C33A H33A 124.2(4) . . ?
N12A C34A C31A 120.8(2) . . ?
N12A C34A H34A 115.3(4) . . ?
C31A C34A H34A 123.9(4) . . ?
O9A N13A C40A 120.2(2) . . ?
O9A N13A C39A 119.1(2) . . ?
C40A N13A C39A 120.7(2) . . ?
O8A C35A O7A 124.9(3) . . ?
O8A C35A C36A 117.0(2) . . ?
O7A C35A C36A 118.0(3) . . ?
C37A C36A C38A 117.9(2) . . ?
C37A C36A C35A 121.1(2) . . ?
C38A C36A C35A 121.0(2) . . ?
C40A C37A C36A 120.4(3) . . ?
C40A C37A H37A 118.6(4) . . ?
C36A C37A H37A 121.0(4) . . ?
C39A C38A C36A 120.0(2) . . ?
C39A C38A H38A 117.9(4) . . ?
C36A C38A H38A 122.1(4) . . ?
N13A C39A C38A 120.5(3) . . ?
N13A C39A H39A 114.4(4) . . ?
C38A C39A H39A 125.0(4) . . ?
N13A C40A C37A 120.4(2) . . ?
N13A C40A H40A 116.8(4) . . ?
C37A C40A H40A 122.7(4) . . ?
C23B O1B H1OA 115.1(4) . . ?
O3B N11B C27B 119.1(2) . . ?
O3B N11B C28B 120.0(3) . . ?
C27B N11B C28B 120.9(2) . . ?
O2B C23B O1B 126.1(3) . . ?
O2B C23B C24B 119.0(3) . . ?
O1B C23B C24B 114.8(3) . . ?
C26B C24B C25B 118.3(2) . . ?
C26B C24B C23B 119.9(2) . . ?
C25B C24B C23B 121.6(2) . . ?
C28B C25B C24B 120.5(2) . . ?
C28B C25B H25B 119.9(4) . . ?
C24B C25B H25B 119.6(4) . . ?
C27B C26B C24B 119.9(3) . . ?
C27B C26B H26B 120.0(4) . . ?
C24B C26B H26B 120.1(4) . . ?
N11B C27B C26B 120.5(2) . . ?
N11B C27B H27B 114.8(4) . . ?
C26B C27B H27B 124.7(4) . . ?
N11B C28B C25B 119.7(3) . . ?
N11B C28B H28B 115.3(4) . . ?
C25B C28B H28B 125.0(4) . . ?
C29B O5B H1OB 114.1(4) . . ?
O6B N12B C34B 119.7(2) . . ?
O6B N12B C33B 120.4(2) . . ?
C34B N12B C33B 119.9(2) . . ?
O4B C29B O5B 126.8(3) . . ?
O4B C29B C30B 119.7(3) . . ?
O5B C29B C30B 113.6(2) . . ?
C31B C30B C32B 118.5(2) . . ?
C31B C30B C29B 120.9(2) . . ?
C32B C30B C29B 120.6(2) . . ?
C34B C31B C30B 119.7(2) . . ?
C34B C31B H31B 119.4(4) . . ?
C30B C31B H31B 120.9(4) . . ?
C33B C32B C30B 120.2(2) . . ?
C33B C32B H32B 118.3(4) . . ?
C30B C32B H32B 121.4(4) . . ?
N12B C33B C32B 120.5(2) . . ?
N12B C33B H33B 115.1(4) . . ?
C32B C33B H33B 124.4(4) . . ?
N12B C34B C31B 121.2(2) . . ?
N12B C34B H34B 115.8(4) . . ?
C31B C34B H34B 123.0(4) . . ?
O9B N13B C40B 120.3(2) . . ?
O9B N13B C39B 119.1(2) . . ?
C40B N13B C39B 120.6(2) . . ?
O7B C35B O8B 124.3(3) . . ?
O7B C35B C36B 118.3(3) . . ?
O8B C35B C36B 117.4(2) . . ?
C38B C36B C37B 117.9(2) . . ?
C38B C36B C35B 121.3(2) . . ?
C37B C36B C35B 120.8(2) . . ?
C40B C37B C36B 120.3(2) . . ?
C40B C37B H37B 119.0(4) . . ?
C36B C37B H37B 120.7(4) . . ?
C39B C38B C36B 120.6(2) . . ?
C39B C38B H38B 117.7(4) . . ?
C36B C38B H38B 121.7(4) . . ?
N13B C39B C38B 120.3(2) . . ?
N13B C39B H39B 113.8(4) . . ?
C38B C39B H39B 125.9(4) . . ?
N13B C40B C37B 120.3(2) . . ?
N13B C40B H40B 115.5(4) . . ?
C37B C40B H40B 124.2(4) . . ?
H1C O1WA H1D 107.5(6) . . ?
H1E O1WB H1F 108.6(6) . . ?
H2C O2WA H2D 105.4(7) . . ?
H2E O2WB H2F 104.9(7) . . ?
H3C O3WA H3D 109.9(6) . . ?
H3E O3WB H3F 111.7(6) . . ?
H4C O4WA H4D 106.2(7) . . ?
H4E O4WB H4F 106.0(7) . . ?
H5C O5WA H5D 105.0(7) . . ?
H5E O5WB H5F 106.3(6) . . ?

_refine_diff_density_max         1.376
_refine_diff_density_min         -1.154
_refine_diff_density_rms         0.222


_exptl_crystal_recrystallization_method 
'Re-crystallisation from solvent: MeOH/H2O'
_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_Fe_bpp_Noxid_NHoxid_95K
_database_code_depnum_ccdc_archive 'CCDC 1873604'
loop_
_audit_author_name
_audit_author_address
'Ver?nica Jornet Moll?'
;Universitat de Val?ncia
Spain
;
_audit_update_record             
;
2018-10-29 deposited with the CCDC.	2020-11-23 downloaded from the CCDC.
;
# start Validation Reply Form
_vrf_PLAT417_Fe_bpp_Noxid_NHoxid_95K 
;
PROBLEM: Short Inter D-H..H-D       H4A      ..H5N      .       2.04 Ang.
RESPONSE: H4A belongs to a water molecule (O4W), while H5N belongs to a bpp molecule. Both hydrogen atoms form H-bonds to O7 and O4W respectively, exhibiting typical geometrical parameters.
;
_vrf_PLAT155_Fe_bpp_Noxid_NHoxid_95K 
;
PROBLEM: The Triclinic Unitcell is NOT Reduced ..........     Please Do !
RESPONSE: The structural transition that takes place at low temperatures causes an increase in the gamma angle, changing from an acute angle (at higher temperatures) to an obtuse value, resulting in a non-reduced set of cell parameters. The non-reduced unit cell was preferred in order to facilitate comparisons with the crystal structure solutions at higher temperatures.
;
_vrf_PLAT303_Fe_bpp_Noxid_NHoxid_95K 
;
PROBLEM: Full Occupancy Atom H1O       with # Connections       2.00 Check
RESPONSE: This hydrogen atom is located between two oxygen atoms that belong to different carboxylate groups, forming a very strong hydrogen bond (the distance between the heteroatoms, O5 and O1, is 2.428 \%A). As a proton-transfer reaction is observed between the two carboxylate anions, different H?O distances are observed at different temperatures. Such a type of proton-transfer reaction is common when strong hydrogen bonds are established (see, for example Angew. Chem. Int. Ed. 2002, 41, 48-76).
;
_vrf_PLAT353_Fe_bpp_Noxid_NHoxid_95K 
;
PROBLEM: Long   N-H (N0.87,N1.01A)  N5       - H5N      .       1.05 Ang.
RESPONSE: H-N and H-O bond distances were not restricted in order to analyse changes in the hydrogen bonding network at different temperatures.
;
_vrf_PLAT353_Fe_bpp_Noxid_NHoxid_95K_2 
;
PROBLEM: Long   N-H (N0.87,N1.01A)  N6       - H6N      .       1.04 Ang.
RESPONSE: H-N and H-O bond distances were not restricted in order to analyse changes in the hydrogen bonding network at different temperatures.
;
# Added during the CSD deposition process: Monday 29 October 2018 04:59 PM
# end Validation Reply Form


_audit_creation_method           SHELXL-2017/1
_shelx_SHELXL_version_number     2017/1
_chemical_name_systematic        ?
_chemical_name_common            ?
_chemical_melting_point          ?
_chemical_formula_moiety         
'C22 H18 Fe N10 2+, C12 H9 N2 O6 1-, C6 H4 N O3 1-, 5(H2 O)'
_chemical_formula_sum            'C40 H41 Fe N13 O14'
_chemical_formula_weight         983.705

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      triclinic
_space_group_IT_number           2
_space_group_name_H-M_alt        'P -1'
_space_group_name_Hall           '-P 1'

_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'

_cell_length_a                   9.9953(3)
_cell_length_b                   13.6057(2)
_cell_length_c                   17.1602(3)
_cell_angle_alpha                76.8440(16)
_cell_angle_beta                 85.770(2)
_cell_angle_gamma                110.502(3)
_cell_volume                     2098.13(10)
_cell_formula_units_Z            2
_cell_measurement_temperature    94.9(2)
_cell_measurement_reflns_used    27094
_cell_measurement_theta_min      2.5480
_cell_measurement_theta_max      27.4800

_exptl_crystal_description       cube
_exptl_crystal_colour            dark-red
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    ?
_exptl_crystal_density_diffrn    1.557
_exptl_crystal_F_000             1020.000
_exptl_transmission_factor_min   ?
_exptl_transmission_factor_max   ?
_exptl_crystal_size_max          0.486
_exptl_crystal_size_mid          0.263
_exptl_crystal_size_min          0.146
_exptl_absorpt_coefficient_mu    0.447
_shelx_estimated_absorpt_T_min   ?
_shelx_estimated_absorpt_T_max   ?
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_correction_T_min  0.847
_exptl_absorpt_correction_T_max  0.946
_exptl_absorpt_process_details   
;
CrysAlisPro 1.171.38.46 (Rigaku Oxford Diffraction, 2015)
Empirical absorption correction using spherical harmonics,
 implemented in SCALE3 ABSPACK scaling algorithm.
;
_diffrn_ambient_temperature      94.9(2)
_diffrn_ambient_environment      N~2~
_diffrn_radiation_wavelength     0.71073
_diffrn_radiation_type           MoK\a
_diffrn_source                   'micro-focus sealed X-ray tube'
_diffrn_radiation_monochromator  mirror
_diffrn_measurement_device       'four-circle diffractometer'
_diffrn_measurement_device_type  
;
SuperNova, Single source at offset, Sapphire3
;
_diffrn_measurement_method       'ω scans'
_diffrn_detector_area_resol_mean 16.0267
_diffrn_reflns_number            79016
_diffrn_reflns_av_unetI/netI     0.1000
_diffrn_reflns_av_R_equivalents  0.0949
_diffrn_reflns_limit_h_min       -13
_diffrn_reflns_limit_h_max       12
_diffrn_reflns_limit_k_min       -17
_diffrn_reflns_limit_k_max       17
_diffrn_reflns_limit_l_min       -22
_diffrn_reflns_limit_l_max       22
_diffrn_reflns_theta_min         2.473
_diffrn_reflns_theta_max         27.752
_diffrn_reflns_theta_full        25.242
_diffrn_measured_fraction_theta_max 0.927
_diffrn_measured_fraction_theta_full 0.999
_diffrn_reflns_Laue_measured_fraction_max 0.927
_diffrn_reflns_Laue_measured_fraction_full 0.999
_diffrn_reflns_point_group_measured_fraction_max 0.927
_diffrn_reflns_point_group_measured_fraction_full 0.999
_reflns_number_total             9154
_reflns_number_gt                7258
_diffrn_orient_matrix_type       
;
CrysAlisPro convention (1999,Acta A55,543-557)
;
_diffrn_orient_matrix_UB_11      -0.0334946903
_diffrn_orient_matrix_UB_12      -0.0378062709
_diffrn_orient_matrix_UB_13      0.0124192091
_diffrn_orient_matrix_UB_21      -0.0648198225
_diffrn_orient_matrix_UB_22      0.0434178355
_diffrn_orient_matrix_UB_23      0.0003834643
_diffrn_orient_matrix_UB_31      -0.0242133530
_diffrn_orient_matrix_UB_32      0.0054368076
_diffrn_orient_matrix_UB_33      -0.0412307897
_diffrn_measurement_details      
;
List of Runs (angles in degrees, time in seconds):

  # Type    Start    End  Width  tₑₓₚ   ω     θ     κ     φ   Frames
#--------------------------------------------------------------------------
  1  ω    -50.00  54.50   0.95   10.00    --  -17.76  77.00 -30.00  110
  2  ω    -50.00  54.50   0.95   10.00    --  -17.76  77.00  60.00  110
  3  ω    -50.00  54.50   0.95   10.00    --  -17.76  77.00 150.00  110
  4  ω     -5.00  88.10   0.95   10.00    --   18.62  57.00 -30.00   98
  5  ω     -5.00  88.10   0.95   10.00    --   18.62  57.00 120.00   98
  6  ω    -20.00  62.65   0.95   10.00    --   18.62 -99.00-120.00   87
  7  ω     -5.00  88.10   0.95   10.00    --   18.62  57.00  60.00   98
  8  ω    -14.00  90.50   0.95   10.00    --   18.62  77.00-150.00  110
  9  ω    -84.00  57.55   0.95   10.00    --  -17.76  19.00-120.00  149
 10  ω    -20.00  26.55   0.95   10.00    --  -17.76 -99.00-180.00   49
 11  ω    -52.00  41.10   0.95   10.00    --   18.62 -57.00 -90.00   98
 12  ω    -52.00  41.10   0.95   10.00    --   18.62 -57.00   0.00   98
 13  ω    -20.00  62.65   0.95   10.00    --   18.62 -99.00  90.00   87
 14  ω     -5.00  88.10   0.95   10.00    --   18.62  57.00 -90.00   98
 15  ω    -13.00  91.50   0.95   10.00    --   18.62  38.00  60.00  110
 16  ω    -56.00  92.20   0.95   10.00    --   18.62   0.00-180.00  156
 17  ω    -56.00  92.20   0.95   10.00    --   18.62   0.00-150.00  156
 18  ω    -56.00  92.20   0.95   10.00    --   18.62   0.00-120.00  156
 19  ω    -20.00  62.65   0.95   10.00    --   18.62 -99.00 -60.00   87
 20  ω    -56.00  91.25   0.95   10.00    --   18.62   0.00 -90.00  155
;
_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 1.171.38.43 (Rigaku OD, 2015)
;
_computing_cell_refinement       
;
CrysAlisPro 1.171.38.43 (Rigaku OD, 2015)
;
_computing_data_reduction        
;
CrysAlisPro 1.171.38.43 (Rigaku OD, 2015)
;
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1997)'
_computing_structure_refinement  'SHELXL-2017/1 (Sheldrick, 2017)'
_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)+(0.0297P)²+2.3514P] where P=(Fo²+2Fc²)/3'
_atom_sites_solution_primary     difmap
_atom_sites_solution_secondary   difmap
_atom_sites_solution_hydrogens   mixed
_refine_ls_hydrogen_treatment    hetero
_refine_ls_extinction_method     none
_refine_ls_extinction_coef       .
_refine_ls_number_reflns         9154
_refine_ls_number_parameters     658
_refine_ls_number_restraints     4
_refine_ls_R_factor_all          0.0660
_refine_ls_R_factor_gt           0.0461
_refine_ls_wR_factor_ref         0.1072
_refine_ls_wR_factor_gt          0.0931
_refine_ls_goodness_of_fit_ref   1.048
_refine_ls_restrained_S_all      1.048
_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
Fe1 Fe 0.08282(3) 0.54634(2) 0.22483(2) 0.01175(9) Uani 1 1 d . . . . .
N1 N 0.1774(2) 0.50489(17) 0.39510(12) 0.0164(4) Uani 1 1 d . . . . .
H1N H 0.266(4) 0.573(3) 0.378(2) 0.067(12) Uiso 1 1 d . . . . .
N2 N 0.0878(2) 0.48243(15) 0.34074(11) 0.0149(4) Uani 1 1 d . . . . .
N3 N -0.1061(2) 0.42864(15) 0.25833(12) 0.0149(4) Uani 1 1 d . . . . .
N4 N 0.0016(2) 0.56354(15) 0.12319(12) 0.0161(4) Uani 1 1 d . . . . .
N5 N 0.0459(2) 0.62945(17) 0.04609(12) 0.0186(4) Uani 1 1 d . . . . .
H5N H 0.149(4) 0.691(3) 0.025(2) 0.064(11) Uiso 1 1 d . . . . .
N6 N -0.0732(2) 0.66742(16) 0.30818(12) 0.0166(4) Uani 1 1 d . . . . .
H6N H -0.175(4) 0.605(3) 0.3274(19) 0.050(10) Uiso 1 1 d . . . . .
N7 N 0.0325(2) 0.66219(15) 0.25750(11) 0.0135(4) Uani 1 1 d . . . . .
N8 N 0.2614(2) 0.67312(15) 0.17965(11) 0.0125(4) Uani 1 1 d . . . . .
N9 N 0.2111(2) 0.48012(15) 0.18012(11) 0.0139(4) Uani 1 1 d . . . . .
N10 N 0.2062(2) 0.38012(16) 0.17885(12) 0.0167(4) Uani 1 1 d . . . . .
H10N H 0.127(4) 0.315(3) 0.2090(19) 0.046(9) Uiso 1 1 d . . . . .
C1 C 0.1160(3) 0.4374(2) 0.46972(15) 0.0198(5) Uani 1 1 d . . . . .
H1 H 0.157565 0.438475 0.516401 0.024 Uiso 1 1 calc R U . . .
C2 C -0.0191(3) 0.3665(2) 0.46503(15) 0.0193(5) Uani 1 1 d . . . . .
H2 H -0.085912 0.310345 0.506751 0.023 Uiso 1 1 calc R U . . .
C3 C -0.0332(3) 0.39757(18) 0.38373(14) 0.0152(5) Uani 1 1 d . . . . .
C4 C -0.1485(2) 0.36606(18) 0.33589(14) 0.0151(5) Uani 1 1 d . . . . .
C5 C -0.2873(3) 0.28675(19) 0.36294(15) 0.0183(5) Uani 1 1 d . . . . .
H5 H -0.315621 0.244333 0.416549 0.022 Uiso 1 1 calc R U . . .
C6 C -0.3831(3) 0.27253(19) 0.30739(16) 0.0206(5) Uani 1 1 d . . . . .
H6 H -0.476275 0.219554 0.323748 0.025 Uiso 1 1 calc R U . . .
C7 C -0.3394(3) 0.33734(19) 0.22778(15) 0.0194(5) Uani 1 1 d . . . . .
H7 H -0.402587 0.328150 0.190483 0.023 Uiso 1 1 calc R U . . .
C8 C -0.2002(2) 0.41594(18) 0.20480(14) 0.0158(5) Uani 1 1 d . . . . .
C9 C -0.1338(3) 0.49431(19) 0.12599(14) 0.0171(5) Uani 1 1 d . . . . .
C10 C -0.1766(3) 0.5169(2) 0.04965(15) 0.0216(5) Uani 1 1 d . . . . .
H10 H -0.265149 0.481379 0.035203 0.026 Uiso 1 1 calc R U . . .
C11 C -0.0591(3) 0.6027(2) 0.00120(15) 0.0220(5) Uani 1 1 d . . . . .
H11 H -0.053291 0.636387 -0.053241 0.026 Uiso 1 1 calc R U . . .
C12 C -0.0346(3) 0.7676(2) 0.32005(14) 0.0188(5) Uani 1 1 d . . . . .
H12 H -0.090493 0.790065 0.352362 0.023 Uiso 1 1 calc R U . . .
C13 C 0.1012(3) 0.83070(19) 0.27641(14) 0.0172(5) Uani 1 1 d . . . . .
H13 H 0.155661 0.903125 0.273149 0.021 Uiso 1 1 calc R U . . .
C14 C 0.1396(2) 0.76206(18) 0.23797(13) 0.0135(5) Uani 1 1 d . . . . .
C15 C 0.2672(2) 0.77226(18) 0.18561(13) 0.0134(5) Uani 1 1 d . . . . .
C16 C 0.3827(2) 0.86725(19) 0.14337(14) 0.0166(5) Uani 1 1 d . . . . .
H16 H 0.385192 0.934939 0.147219 0.020 Uiso 1 1 calc R U . . .
C17 C 0.4941(2) 0.85904(19) 0.09534(14) 0.0169(5) Uani 1 1 d . . . . .
H17 H 0.572628 0.921558 0.066814 0.020 Uiso 1 1 calc R U . . .
C18 C 0.4883(2) 0.75706(19) 0.08991(14) 0.0159(5) Uani 1 1 d . . . . .
H18 H 0.562410 0.750638 0.057931 0.019 Uiso 1 1 calc R U . . .
C19 C 0.3699(2) 0.66527(18) 0.13310(13) 0.0129(5) Uani 1 1 d . . . . .
C20 C 0.3404(2) 0.55125(18) 0.13650(13) 0.0134(5) Uani 1 1 d . . . . .
C21 C 0.4189(3) 0.4963(2) 0.10680(14) 0.0182(5) Uani 1 1 d . . . . .
H21 H 0.510397 0.526091 0.074920 0.022 Uiso 1 1 calc R U . . .
C22 C 0.3298(3) 0.3881(2) 0.13561(15) 0.0192(5) Uani 1 1 d . . . . .
H22 H 0.351144 0.329841 0.126748 0.023 Uiso 1 1 calc R U . . .
N11 N 1.1176(2) 1.00894(17) 0.06983(12) 0.0190(4) Uani 1 1 d . . . . .
O1 O 0.69209(18) 0.66815(13) 0.19158(10) 0.0196(4) Uani 1 1 d . . . . .
O2 O 0.65522(18) 0.78345(14) 0.25873(10) 0.0217(4) Uani 1 1 d . . . . .
O3 O 1.24242(18) 1.08417(15) 0.03129(10) 0.0260(4) Uani 1 1 d . . . . .
C23 C 0.7226(3) 0.76141(19) 0.20587(14) 0.0173(5) Uani 1 1 d . . . . .
C24 C 0.8570(2) 0.84959(19) 0.15357(14) 0.0154(5) Uani 1 1 d . . . . .
C25 C 0.9470(3) 0.8271(2) 0.10083(14) 0.0182(5) Uani 1 1 d . . . . .
H25 H 0.919268 0.757673 0.093112 0.022 Uiso 1 1 calc R U . . .
C26 C 0.8991(3) 0.9554(2) 0.16081(15) 0.0192(5) Uani 1 1 d . . . . .
H26 H 0.839401 0.973075 0.194715 0.023 Uiso 1 1 calc R U . . .
C27 C 1.0281(3) 1.0339(2) 0.11826(15) 0.0212(5) Uani 1 1 d . . . . .
H27 H 1.054426 1.104829 0.122637 0.025 Uiso 1 1 calc R U . . .
C28 C 1.0774(3) 0.9069(2) 0.05975(14) 0.0202(5) Uani 1 1 d . . . . .
H28 H 1.137928 0.890973 0.025083 0.024 Uiso 1 1 calc R U . . .
N12 N 0.1988(2) 0.19055(15) 0.50901(12) 0.0152(4) Uani 1 1 d . . . . .
O4 O 0.65511(17) 0.51317(13) 0.37819(10) 0.0198(4) Uani 1 1 d . . . . .
O5 O 0.50289(19) 0.51360(14) 0.28776(10) 0.0229(4) Uani 1 1 d . . . . .
H1O H 0.601(5) 0.598(3) 0.240(2) 0.079(13) Uiso 1 1 d . . . . .
O6 O 0.09354(17) 0.10568(13) 0.55767(10) 0.0193(4) Uani 1 1 d . . . . .
C29 C 0.5378(3) 0.47532(19) 0.35538(14) 0.0168(5) Uani 1 1 d . . . . .
C30 C 0.4196(2) 0.37449(18) 0.40910(14) 0.0152(5) Uani 1 1 d . . . . .
C31 C 0.4269(2) 0.33692(19) 0.49026(14) 0.0165(5) Uani 1 1 d . . . . .
H31 H 0.506765 0.373295 0.511581 0.020 Uiso 1 1 calc R U . . .
C32 C 0.2994(3) 0.31594(19) 0.37918(14) 0.0172(5) Uani 1 1 d . . . . .
H32 H 0.292261 0.339056 0.324852 0.021 Uiso 1 1 calc R U . . .
C33 C 0.1917(3) 0.22471(19) 0.42917(14) 0.0175(5) Uani 1 1 d . . . . .
H33 H 0.112988 0.185793 0.408236 0.021 Uiso 1 1 calc R U . . .
C34 C 0.3161(2) 0.24579(19) 0.53939(14) 0.0164(5) Uani 1 1 d . . . . .
H34 H 0.321264 0.221662 0.593903 0.020 Uiso 1 1 calc R U . . .
N13 N 0.4981(2) 1.06797(16) -0.39249(12) 0.0171(4) Uani 1 1 d . . . . .
O7 O 0.10574(19) 0.79618(14) -0.16900(10) 0.0224(4) Uani 1 1 d . . . . .
O8 O -0.00794(18) 0.80792(13) -0.27579(10) 0.0201(4) Uani 1 1 d . . . . .
O9 O 0.61901(17) 1.14514(13) -0.43788(10) 0.0199(4) Uani 1 1 d . . . . .
C35 C 0.1037(3) 0.83365(18) -0.24230(15) 0.0167(5) Uani 1 1 d . . . . .
C36 C 0.2430(2) 0.91597(18) -0.29549(14) 0.0151(5) Uani 1 1 d . . . . .
C37 C 0.2519(3) 0.95344(19) -0.37927(15) 0.0180(5) Uani 1 1 d . . . . .
H37 H 0.170749 0.927476 -0.403144 0.022 Uiso 1 1 calc R U . . .
C38 C 0.3676(3) 0.9567(2) -0.26305(15) 0.0191(5) Uani 1 1 d . . . . .
H38 H 0.365814 0.932613 -0.207593 0.023 Uiso 1 1 calc R U . . .
C39 C 0.4931(3) 1.03198(19) -0.31179(14) 0.0186(5) Uani 1 1 d . . . . .
H39 H 0.575647 1.058513 -0.289093 0.022 Uiso 1 1 calc R U . . .
C40 C 0.3797(3) 1.02838(19) -0.42675(15) 0.0172(5) Uani 1 1 d . . . . .
H40 H 0.384849 1.052012 -0.482588 0.021 Uiso 1 1 calc R U . . .
O1W O 0.2068(2) 0.97981(15) 0.42499(11) 0.0218(4) Uani 1 1 d . . . . .
H1B H 0.247(4) 0.936(3) 0.4286(19) 0.041(10) Uiso 1 1 d . . . . .
H1A H 0.113(4) 0.941(3) 0.4385(19) 0.042(9) Uiso 1 1 d . . . . .
O2W O 0.2485(2) 1.11668(17) 0.27147(12) 0.0262(4) Uani 1 1 d . . . . .
H2A H 0.175(3) 1.132(2) 0.2749(17) 0.026(8) Uiso 1 1 d . . . . .
H2B H 0.243(4) 1.076(3) 0.316(2) 0.045(11) Uiso 1 1 d . . . . .
O3W O 0.3945(2) 0.69573(16) 0.35768(12) 0.0249(4) Uani 1 1 d . . . . .
H3A H 0.388(4) 0.742(3) 0.386(2) 0.048(10) Uiso 1 1 d . . . . .
H3B H 0.472(4) 0.719(3) 0.329(2) 0.037(10) Uiso 1 1 d . . . . .
O4W O 0.2777(2) 0.79934(17) -0.05187(12) 0.0288(4) Uani 1 1 d . . . . .
H4A H 0.233(4) 0.795(3) -0.088(2) 0.049(11) Uiso 1 1 d . . . . .
H4B H 0.362(5) 0.803(4) -0.073(3) 0.085(15) Uiso 1 1 d . . . . .
O5W O 1.4367(2) 1.15902(18) 0.12765(14) 0.0328(5) Uani 1 1 d . . . . .
H5A H 1.376(5) 1.135(3) 0.096(3) 0.078(14) Uiso 1 1 d . . . . .
H5B H 1.388(4) 1.148(3) 0.171(2) 0.041(10) Uiso 1 1 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 1.940(2) . ?
Fe1 N8 1.9474(19) . ?
Fe1 N4 1.9780(19) . ?
Fe1 N7 1.9921(19) . ?
Fe1 N2 1.9929(19) . ?
Fe1 N9 2.0059(19) . ?
N1 C1 1.347(3) . ?
N1 N2 1.352(3) . ?
N1 H1N 1.00(4) . ?
N2 C3 1.357(3) . ?
N3 C4 1.351(3) . ?
N3 C8 1.358(3) . ?
N4 C9 1.341(3) . ?
N4 N5 1.359(3) . ?
N5 C11 1.345(3) . ?
N5 H5N 1.05(4) . ?
N6 C12 1.348(3) . ?
N6 N7 1.350(3) . ?
N6 H6N 1.04(3) . ?
N7 C14 1.351(3) . ?
N8 C19 1.348(3) . ?
N8 C15 1.357(3) . ?
N9 C20 1.348(3) . ?
N9 N10 1.349(3) . ?
N10 C22 1.350(3) . ?
N10 H10N 0.95(3) . ?
C1 C2 1.378(3) . ?
C1 H1 0.9300 . ?
C2 C3 1.396(3) . ?
C2 H2 0.9300 . ?
C3 C4 1.463(3) . ?
C4 C5 1.390(3) . ?
C5 C6 1.397(3) . ?
C5 H5 0.9300 . ?
C6 C7 1.389(4) . ?
C6 H6 0.9300 . ?
C7 C8 1.386(3) . ?
C7 H7 0.9300 . ?
C8 C9 1.457(3) . ?
C9 C10 1.409(3) . ?
C10 C11 1.374(4) . ?
C10 H10 0.9300 . ?
C11 H11 0.9300 . ?
C12 C13 1.372(3) . ?
C12 H12 0.9300 . ?
C13 C14 1.396(3) . ?
C13 H13 0.9300 . ?
C14 C15 1.450(3) . ?
C15 C16 1.390(3) . ?
C16 C17 1.388(3) . ?
C16 H16 0.9300 . ?
C17 C18 1.393(3) . ?
C17 H17 0.9300 . ?
C18 C19 1.387(3) . ?
C18 H18 0.9300 . ?
C19 C20 1.460(3) . ?
C20 C21 1.401(3) . ?
C21 C22 1.375(3) . ?
C21 H21 0.9300 . ?
C22 H22 0.9300 . ?
N11 O3 1.310(2) . ?
N11 C27 1.356(3) . ?
N11 C28 1.359(3) . ?
O1 C23 1.282(3) . ?
O1 H1O 1.17(4) . ?
O2 C23 1.242(3) . ?
C23 C24 1.501(3) . ?
C24 C25 1.386(3) . ?
C24 C26 1.389(3) . ?
C25 C28 1.378(3) . ?
C25 H25 0.9300 . ?
C26 C27 1.370(3) . ?
C26 H26 0.9300 . ?
C27 H27 0.9300 . ?
C28 H28 0.9300 . ?
N12 O6 1.311(2) . ?
N12 C33 1.359(3) . ?
N12 C34 1.364(3) . ?
O4 C29 1.237(3) . ?
O5 C29 1.285(3) . ?
O5 H1O 1.27(4) . ?
C29 C30 1.502(3) . ?
C30 C31 1.387(3) . ?
C30 C32 1.396(3) . ?
C31 C34 1.378(3) . ?
C31 H31 0.9300 . ?
C32 C33 1.370(3) . ?
C32 H32 0.9300 . ?
C33 H33 0.9300 . ?
C34 H34 0.9300 . ?
N13 O9 1.330(2) . ?
N13 C39 1.351(3) . ?
N13 C40 1.355(3) . ?
O7 C35 1.250(3) . ?
O8 C35 1.269(3) . ?
C35 C36 1.511(3) . ?
C36 C38 1.388(3) . ?
C36 C37 1.397(3) . ?
C37 C40 1.375(3) . ?
C37 H37 0.9300 . ?
C38 C39 1.371(3) . ?
C38 H38 0.9300 . ?
C39 H39 0.9300 . ?
C40 H40 0.9300 . ?
O1W H1B 0.82(3) . ?
O1W H1A 0.88(4) . ?
O2W H2A 0.84(3) . ?
O2W H2B 0.83(4) . ?
O3W H3A 0.89(4) . ?
O3W H3B 0.81(3) . ?
O4W H4A 0.80(4) . ?
O4W H4B 0.87(5) . ?
O5W H5A 0.87(4) . ?
O5W H5B 0.81(4) . ?

loop_
_geom_angle_atom_site_label_1
_geom_angle_atom_site_label_2
_geom_angle_atom_site_label_3
_geom_angle
_geom_angle_site_symmetry_1
_geom_angle_site_symmetry_3
_geom_angle_publ_flag
N3 Fe1 N8 172.36(8) . . ?
N3 Fe1 N4 79.03(8) . . ?
N8 Fe1 N4 93.84(8) . . ?
N3 Fe1 N7 98.76(8) . . ?
N8 Fe1 N7 78.87(8) . . ?
N4 Fe1 N7 94.01(8) . . ?
N3 Fe1 N2 78.34(8) . . ?
N8 Fe1 N2 108.74(8) . . ?
N4 Fe1 N2 157.36(8) . . ?
N7 Fe1 N2 88.99(8) . . ?
N3 Fe1 N9 104.49(8) . . ?
N8 Fe1 N9 78.16(8) . . ?
N4 Fe1 N9 91.12(8) . . ?
N7 Fe1 N9 156.74(8) . . ?
N2 Fe1 N9 94.94(8) . . ?
C1 N1 N2 111.1(2) . . ?
C1 N1 H1N 130(2) . . ?
N2 N1 H1N 118(2) . . ?
N1 N2 C3 105.30(19) . . ?
N1 N2 Fe1 137.62(16) . . ?
C3 N2 Fe1 116.81(14) . . ?
C4 N3 C8 120.1(2) . . ?
C4 N3 Fe1 120.46(15) . . ?
C8 N3 Fe1 119.15(16) . . ?
C9 N4 N5 106.24(19) . . ?
C9 N4 Fe1 116.55(16) . . ?
N5 N4 Fe1 137.20(16) . . ?
C11 N5 N4 110.6(2) . . ?
C11 N5 H5N 125(2) . . ?
N4 N5 H5N 124(2) . . ?
C12 N6 N7 110.7(2) . . ?
C12 N6 H6N 125.9(18) . . ?
N7 N6 H6N 122.8(18) . . ?
N6 N7 C14 105.63(18) . . ?
N6 N7 Fe1 137.17(15) . . ?
C14 N7 Fe1 115.84(15) . . ?
C19 N8 C15 120.0(2) . . ?
C19 N8 Fe1 120.19(15) . . ?
C15 N8 Fe1 119.08(15) . . ?
C20 N9 N10 106.08(18) . . ?
C20 N9 Fe1 115.70(14) . . ?
N10 N9 Fe1 138.20(16) . . ?
C22 N10 N9 110.2(2) . . ?
C22 N10 H10N 127.9(19) . . ?
N9 N10 H10N 121.7(19) . . ?
N1 C1 C2 108.3(2) . . ?
N1 C1 H1 125.9 . . ?
C2 C1 H1 125.9 . . ?
C1 C2 C3 104.6(2) . . ?
C1 C2 H2 127.7 . . ?
C3 C2 H2 127.7 . . ?
N2 C3 C2 110.7(2) . . ?
N2 C3 C4 113.4(2) . . ?
C2 C3 C4 135.7(2) . . ?
N3 C4 C5 121.6(2) . . ?
N3 C4 C3 110.9(2) . . ?
C5 C4 C3 127.5(2) . . ?
C4 C5 C6 118.2(2) . . ?
C4 C5 H5 120.9 . . ?
C6 C5 H5 120.9 . . ?
C7 C6 C5 120.1(2) . . ?
C7 C6 H6 119.9 . . ?
C5 C6 H6 119.9 . . ?
C8 C7 C6 118.9(2) . . ?
C8 C7 H7 120.5 . . ?
C6 C7 H7 120.5 . . ?
N3 C8 C7 121.0(2) . . ?
N3 C8 C9 110.9(2) . . ?
C7 C8 C9 128.1(2) . . ?
N4 C9 C10 110.0(2) . . ?
N4 C9 C8 114.3(2) . . ?
C10 C9 C8 135.7(2) . . ?
C11 C10 C9 105.0(2) . . ?
C11 C10 H10 127.5 . . ?
C9 C10 H10 127.5 . . ?
N5 C11 C10 108.2(2) . . ?
N5 C11 H11 125.9 . . ?
C10 C11 H11 125.9 . . ?
N6 C12 C13 108.4(2) . . ?
N6 C12 H12 125.8 . . ?
C13 C12 H12 125.8 . . ?
C12 C13 C14 104.6(2) . . ?
C12 C13 H13 127.7 . . ?
C14 C13 H13 127.7 . . ?
N7 C14 C13 110.6(2) . . ?
N7 C14 C15 114.26(19) . . ?
C13 C14 C15 135.1(2) . . ?
N8 C15 C16 121.2(2) . . ?
N8 C15 C14 110.93(19) . . ?
C16 C15 C14 127.9(2) . . ?
C17 C16 C15 118.7(2) . . ?
C17 C16 H16 120.7 . . ?
C15 C16 H16 120.7 . . ?
C16 C17 C18 119.9(2) . . ?
C16 C17 H17 120.0 . . ?
C18 C17 H17 120.0 . . ?
C19 C18 C17 118.8(2) . . ?
C19 C18 H18 120.6 . . ?
C17 C18 H18 120.6 . . ?
N8 C19 C18 121.4(2) . . ?
N8 C19 C20 110.20(19) . . ?
C18 C19 C20 128.4(2) . . ?
N9 C20 C21 110.7(2) . . ?
N9 C20 C19 114.78(19) . . ?
C21 C20 C19 134.5(2) . . ?
C22 C21 C20 104.1(2) . . ?
C22 C21 H21 127.9 . . ?
C20 C21 H21 127.9 . . ?
N10 C22 C21 108.9(2) . . ?
N10 C22 H22 125.5 . . ?
C21 C22 H22 125.5 . . ?
O3 N11 C27 119.8(2) . . ?
O3 N11 C28 119.8(2) . . ?
C27 N11 C28 120.4(2) . . ?
C23 O1 H1O 113.4(19) . . ?
O2 C23 O1 126.7(2) . . ?
O2 C23 C24 118.7(2) . . ?
O1 C23 C24 114.5(2) . . ?
C25 C24 C26 118.2(2) . . ?
C25 C24 C23 121.5(2) . . ?
C26 C24 C23 120.3(2) . . ?
C28 C25 C24 120.4(2) . . ?
C28 C25 H25 119.8 . . ?
C24 C25 H25 119.8 . . ?
C27 C26 C24 120.3(2) . . ?
C27 C26 H26 119.8 . . ?
C24 C26 H26 119.8 . . ?
N11 C27 C26 120.6(2) . . ?
N11 C27 H27 119.7 . . ?
C26 C27 H27 119.7 . . ?
N11 C28 C25 120.1(2) . . ?
N11 C28 H28 119.9 . . ?
C25 C28 H28 119.9 . . ?
O6 N12 C33 120.83(19) . . ?
O6 N12 C34 119.38(19) . . ?
C33 N12 C34 119.8(2) . . ?
C29 O5 H1O 115.6(18) . . ?
O4 C29 O5 126.5(2) . . ?
O4 C29 C30 119.8(2) . . ?
O5 C29 C30 113.7(2) . . ?
C31 C30 C32 118.0(2) . . ?
C31 C30 C29 120.7(2) . . ?
C32 C30 C29 121.3(2) . . ?
C34 C31 C30 120.2(2) . . ?
C34 C31 H31 119.9 . . ?
C30 C31 H31 119.9 . . ?
C33 C32 C30 120.6(2) . . ?
C33 C32 H32 119.7 . . ?
C30 C32 H32 119.7 . . ?
N12 C33 C32 120.7(2) . . ?
N12 C33 H33 119.7 . . ?
C32 C33 H33 119.7 . . ?
N12 C34 C31 120.8(2) . . ?
N12 C34 H34 119.6 . . ?
C31 C34 H34 119.6 . . ?
O9 N13 C39 119.45(19) . . ?
O9 N13 C40 120.10(19) . . ?
C39 N13 C40 120.4(2) . . ?
O7 C35 O8 124.7(2) . . ?
O7 C35 C36 118.3(2) . . ?
O8 C35 C36 117.0(2) . . ?
C38 C36 C37 117.4(2) . . ?
C38 C36 C35 121.3(2) . . ?
C37 C36 C35 121.3(2) . . ?
C40 C37 C36 120.5(2) . . ?
C40 C37 H37 119.7 . . ?
C36 C37 H37 119.7 . . ?
C39 C38 C36 120.8(2) . . ?
C39 C38 H38 119.6 . . ?
C36 C38 H38 119.6 . . ?
N13 C39 C38 120.6(2) . . ?
N13 C39 H39 119.7 . . ?
C38 C39 H39 119.7 . . ?
N13 C40 C37 120.3(2) . . ?
N13 C40 H40 119.9 . . ?
C37 C40 H40 119.9 . . ?
H1B O1W H1A 107(3) . . ?
H2A O2W H2B 105(3) . . ?
H3A O3W H3B 111(3) . . ?
H4A O4W H4B 104(4) . . ?
H5A O5W H5B 107(3) . . ?

_refine_diff_density_max         0.598
_refine_diff_density_min         -0.684
_refine_diff_density_rms         0.081


_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_Fe_bpp_Noxid_NHoxid_120K
_database_code_depnum_ccdc_archive 'CCDC 1832988'
loop_
_audit_author_name
_audit_author_address
'Ver?nica Jornet Moll?'
;Universitat de Val?ncia
Spain
;
_audit_update_record             
;
2018-10-29 deposited with the CCDC.	2020-11-23 downloaded from the CCDC.
;
# start Validation Reply Form
_vrf_PLAT110_Fe_bpp_Noxid_NHoxid_120K 
;
PROBLEM: ADDSYM Detects Potential Lattice Translation ...          ? Check
RESPONSE: The asymmetric unit contains two crystallographically independent Fe(II) complexes (and Z = 4) having clearly different Fe-N distances which correspond to two different spin states (high and low), as confirmed by magnetic susceptibility measurements. The alerts arise because the structure can also be solved with a smaller unit cell (with parameters very similar to the high temperature structure solution) having half volume and only one Fe(II) complex (and Z = 2) with intermediate Fe-N distances between the corresponding high and low spin states. This solution also exhibits more elongated thermal ellipsoids in the N and C atoms of the ligands, suggesting that they can be split in two different positions corresponding to the high and low spin states. Therefore, the structure solution with Z = 4 has been adopted.
;
_vrf_PLAT112_Fe_bpp_Noxid_NHoxid_120K 
;
PROBLEM: ADDSYM Detects New (Pseudo) Symm. Elem         B        100 %Fit
RESPONSE: The asymmetric unit contains two crystallographically independent Fe(II) complexes (and Z = 4) having clearly different Fe-N distances which correspond to two different spin states (high and low), as confirmed by magnetic susceptibility measurements. The alerts arise because the structure can also be solved with a smaller unit cell (with parameters very similar to the high temperature structure solution) having half volume and only one Fe(II) complex (and Z = 2) with intermediate Fe-N distances between the corresponding high and low spin states. This solution also exhibits more elongated thermal ellipsoids in the N and C atoms of the ligands, suggesting that they can be split in two different positions corresponding to the high and low spin states. Therefore, the structure solution with Z = 4 has been adopted.
;
_vrf_PLAT113_Fe_bpp_Noxid_NHoxid_120K 
;
PROBLEM: ADDSYM Suggests Possible Pseudo/New  Space Group        P-1 Check
RESPONSE: The asymmetric unit contains two crystallographically independent Fe(II) complexes (and Z = 4) having clearly different Fe-N distances which correspond to two different spin states (high and low), as confirmed by magnetic susceptibility measurements. The alerts arise because the structure can also be solved with a smaller unit cell (with parameters very similar to the high temperature structure solution) having half volume and only one Fe(II) complex (and Z = 2) with intermediate Fe-N distances between the corresponding high and low spin states. This solution also exhibits more elongated thermal ellipsoids in the N and C atoms of the ligands, suggesting that they can be split in two different positions corresponding to the high and low spin states. Therefore, the structure solution with Z = 4 has been adopted.
;
_vrf_PLAT303_Fe_bpp_Noxid_NHoxid_120K 
;
PROBLEM: Full Occupancy Atom H1OB      with # Connections       2.00 Check
RESPONSE: This hydrogen atom is located between two oxygen atoms that belong to different carboxylate groups, forming a very strong hydrogen bond (the distance between the heteroatoms, O5B and O1A, is 2.426 \%A). As a proton-transfer reaction is observed between the two carboxylate anions, different H?O distances are observed at different temperatures. Such a type of proton-transfer reaction is common when strong hydrogen bonds are established (see, for example Angew. Chem. Int. Ed. 2002, 41, 48-76)
;
_vrf_PLAT303_Fe_bpp_Noxid_NHoxid_120K_2 
;
PROBLEM: Full Occupancy Atom H1OA      with # Connections       2.00 Check
RESPONSE: This hydrogen atom is located between two oxygen atoms that belong to different carboxylate groups, forming a very strong hydrogen bond (the distance between the heteroatoms, O5A and O1B, is 2.422 \%A). As a proton-transfer reaction is observed between the two carboxylate anions, different H?O distances are observed at different temperatures. Such a type of proton-transfer reaction is common when strong hydrogen bonds are established (see, for example Angew. Chem. Int. Ed. 2002, 41, 48-76).
;
# Added during the CSD deposition process: Monday 29 October 2018 04:20 PM
# end Validation Reply Form


_audit_creation_method           SHELXL-2017/1
_shelx_SHELXL_version_number     2017/1
_chemical_name_systematic        ?
_chemical_name_common            ?
_chemical_melting_point          ?
_chemical_formula_moiety         
'C22 H18 Fe N10 2+, C12 H9 N2 O6 1-, C6 H4 N O3 1-, 5(H2 O)'
_chemical_formula_sum            'C40 H41 Fe N13 O14'
_chemical_formula_weight         983.705

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      triclinic
_space_group_IT_number           2
_space_group_name_H-M_alt        'P -1'
_space_group_name_Hall           '-P 1'

_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'

_cell_length_a                   13.63358(18)
_cell_length_b                   18.8075(2)
_cell_length_c                   19.6686(2)
_cell_angle_alpha                64.7142(13)
_cell_angle_beta                 71.0809(12)
_cell_angle_gamma                71.0628(12)
_cell_volume                     4210.47(11)
_cell_formula_units_Z            4
_cell_measurement_temperature    120.00(14)
_cell_measurement_reflns_used    62124
_cell_measurement_theta_min      2.3050
_cell_measurement_theta_max      27.5760

_exptl_crystal_description       cube
_exptl_crystal_colour            dark-red
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    ?
_exptl_crystal_density_diffrn    1.552
_exptl_crystal_F_000             2040.000
_exptl_transmission_factor_min   ?
_exptl_transmission_factor_max   ?
_exptl_crystal_size_max          0.360
_exptl_crystal_size_mid          0.226
_exptl_crystal_size_min          0.166
_exptl_absorpt_coefficient_mu    0.445
_shelx_estimated_absorpt_T_min   ?
_shelx_estimated_absorpt_T_max   ?
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_correction_T_min  0.894
_exptl_absorpt_correction_T_max  0.943
_exptl_absorpt_process_details   
;
CrysAlisPro 1.171.38.46 (Rigaku Oxford Diffraction, 2015)
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           MoK\a
_diffrn_source                   'micro-focus sealed X-ray tube'
_diffrn_radiation_monochromator  mirror
_diffrn_measurement_device       'four-circle diffractometer'
_diffrn_measurement_device_type  
;
SuperNova, Single source at offset, Sapphire3
;
_diffrn_measurement_method       'ω scans'
_diffrn_detector_area_resol_mean 16.0267
_diffrn_reflns_number            162864
_diffrn_reflns_av_unetI/netI     0.0756
_diffrn_reflns_av_R_equivalents  0.1053
_diffrn_reflns_limit_h_min       -17
_diffrn_reflns_limit_h_max       17
_diffrn_reflns_limit_k_min       -24
_diffrn_reflns_limit_k_max       24
_diffrn_reflns_limit_l_min       -25
_diffrn_reflns_limit_l_max       25
_diffrn_reflns_theta_min         2.2224
_diffrn_reflns_theta_max         27.7456
_diffrn_reflns_theta_full        25.242
_diffrn_measured_fraction_theta_max 0.9379
_diffrn_measured_fraction_theta_full 0.9994
_diffrn_reflns_Laue_measured_fraction_max 0.938
_diffrn_reflns_Laue_measured_fraction_full 0.999
_diffrn_reflns_point_group_measured_fraction_max 0.938
_diffrn_reflns_point_group_measured_fraction_full 0.999
_reflns_number_total             18600
_reflns_number_gt                15687
_diffrn_orient_matrix_type       
;
CrysAlisPro convention (1999,Acta A55,543-557)
;
_diffrn_orient_matrix_UB_11      -0.0287072000
_diffrn_orient_matrix_UB_12      0.0406253000
_diffrn_orient_matrix_UB_13      -0.0103461000
_diffrn_orient_matrix_UB_21      -0.0359593000
_diffrn_orient_matrix_UB_22      -0.0096436000
_diffrn_orient_matrix_UB_23      0.0362999000
_diffrn_orient_matrix_UB_31      0.0325223000
_diffrn_orient_matrix_UB_32      0.0090936000
_diffrn_orient_matrix_UB_33      0.0156408000
_diffrn_measurement_details      
;
List of Runs (angles in degrees, time in seconds):

  # Type    Start    End  Width  tₑₓₚ   ω     θ     κ     φ   Frames
#--------------------------------------------------------------------------
  1  ω    -41.00  52.00   0.75    7.50    --  -17.76  57.00   0.00  124
  2  ω    -20.00  26.50   0.75    7.50    --  -17.76 -99.00-120.00   62
  3  ω    -51.00  54.00   0.75    7.50    --  -17.76  77.00  90.00  140
  4  ω    -13.00  92.00   0.75    7.50    --   18.62  38.00 -90.00  140
  5  ω    -20.00  62.50   0.75    7.50    --   18.62 -99.00-180.00  110
  6  ω    -52.00  41.00   0.75    7.50    --   18.62 -57.00-120.00  124
  7  ω    -14.00  91.00   0.75    7.50    --   18.62  77.00 120.00  140
  8  ω    -14.00  91.00   0.75    7.50    --   18.62  77.00   0.00  140
  9  ω    -20.00  62.50   0.75    7.50    --   18.62 -99.00   0.00  110
 10  ω    -49.00  56.00   0.75    7.50    --  -17.76  38.00-120.00  140
 11  ω    -91.00  14.00   0.75    7.50    --  -17.76 -38.00   0.00  140
 12  ω    -97.00 -35.50   0.75    7.50    --  -17.76-178.00 -90.00   82
 13  ω    -97.00 -35.50   0.75    7.50    --  -17.76-178.00 120.00   82
 14  ω    -20.00  62.50   0.75    7.50    --   18.62 -99.00  60.00  110
 15  ω    -27.00  60.00   0.75    7.50    --   18.62 -93.00-129.00  116
 16  ω    -55.00  50.00   0.75    7.50    --   18.62 -38.00 120.00  140
 17  ω    -91.00  14.00   0.75    7.50    --  -17.76 -38.00 150.00  140
 18  ω   -100.00 -34.00   0.75    7.50    --  -17.76 178.00 150.00   88
 19  ω    -91.00  14.00   0.75    7.50    --  -17.76 -38.00-120.00  140
 20  ω    -56.00  94.00   0.75    7.50    --   18.62   0.00-120.00  200
 21  ω    -56.00  94.00   0.75    7.50    --   18.62   0.00-150.00  200
 22  ω    -56.00  94.00   0.75    7.50    --   18.62   0.00-180.00  200
;
_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 1.171.38.43 (Rigaku OD, 2015)
;
_computing_cell_refinement       
;
CrysAlisPro 1.171.38.43 (Rigaku OD, 2015)
;
_computing_data_reduction        
;
CrysAlisPro 1.171.38.43 (Rigaku OD, 2015)
;
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1997)'
_computing_structure_refinement  'SHELXL-2017/1 (Sheldrick, 2017)'
_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)+(0.0511P)²+1.7476P] where P=(Fo²+2Fc²)/3'
_atom_sites_solution_primary     difmap
_atom_sites_solution_secondary   difmap
_atom_sites_solution_hydrogens   mixed
_refine_ls_hydrogen_treatment    hetero
_refine_ls_extinction_method     none
_refine_ls_extinction_coef       .
_refine_ls_number_reflns         18600
_refine_ls_number_parameters     1315
_refine_ls_number_restraints     0
_refine_ls_R_factor_all          0.0473
_refine_ls_R_factor_gt           0.0384
_refine_ls_wR_factor_ref         0.1125
_refine_ls_wR_factor_gt          0.1026
_refine_ls_goodness_of_fit_ref   1.045
_refine_ls_restrained_S_all      1.045
_refine_ls_shift/su_max          0.002
_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
Fe1A Fe 0.88436(2) 0.73167(2) 0.34435(2) 0.01302(6) Uani 1 1 d . . . . .
N1A N 0.88690(10) 0.91308(8) 0.21631(8) 0.0193(3) Uani 1 1 d . . . . .
H41A H 0.8784(15) 0.8975(12) 0.1817(11) 0.029 Uiso 1 1 d . U . . .
N2A N 0.88947(10) 0.85731(7) 0.28719(7) 0.0170(3) Uani 1 1 d . . . . .
N3A N 0.88890(9) 0.77039(7) 0.43019(7) 0.0156(3) Uani 1 1 d . . . . .
N4A N 0.87754(10) 0.62715(7) 0.45103(7) 0.0176(3) Uani 1 1 d . . . . .
N5A N 0.87320(10) 0.54923(8) 0.47482(8) 0.0213(3) Uani 1 1 d . . . . .
H42A H 0.8713(16) 0.5295(12) 0.4410(11) 0.032 Uiso 1 1 d . U . . .
N6A N 0.62534(10) 0.81075(8) 0.37696(8) 0.0179(3) Uani 1 1 d . . . . .
H43A H 0.6262(15) 0.8294(12) 0.4079(11) 0.027 Uiso 1 1 d . U . . .
N7A N 0.71297(10) 0.76111(7) 0.35267(7) 0.0153(3) Uani 1 1 d . . . . .
N8A N 0.86321(9) 0.67560(7) 0.27849(7) 0.0136(2) Uani 1 1 d . . . . .
N9A N 1.04425(10) 0.67702(7) 0.29460(7) 0.0153(3) Uani 1 1 d . . . . .
N10A N 1.14628(10) 0.67123(8) 0.29240(8) 0.0179(3) Uani 1 1 d . . . . .
H44A H 1.1592(14) 0.6970(12) 0.3170(11) 0.027 Uiso 1 1 d . U . . .
C1A C 0.88811(12) 0.98560(9) 0.21317(10) 0.0227(3) Uani 1 1 d . . . . .
H1A H 0.886054 1.032900 0.170125 0.027 Uiso 1 1 calc R U . . .
C2A C 0.89293(12) 0.97734(9) 0.28495(10) 0.0219(3) Uani 1 1 d . . . . .
H2A H 0.895741 1.016922 0.300304 0.026 Uiso 1 1 calc R U . . .
C3A C 0.89266(11) 0.89579(9) 0.33009(9) 0.0167(3) Uani 1 1 d . . . . .
C4A C 0.88950(11) 0.84790(9) 0.41204(9) 0.0167(3) Uani 1 1 d . . . . .
C5A C 0.88276(12) 0.87753(10) 0.46753(10) 0.0205(3) Uani 1 1 d . . . . .
H5A H 0.883393 0.931162 0.454237 0.025 Uiso 1 1 calc R U . . .
C6A C 0.87504(12) 0.82444(10) 0.54362(10) 0.0224(3) Uani 1 1 d . . . . .
H6A H 0.870751 0.842441 0.582010 0.027 Uiso 1 1 calc R U . . .
C7A C 0.87374(12) 0.74473(10) 0.56232(9) 0.0221(3) Uani 1 1 d . . . . .
H7A H 0.868077 0.709003 0.613089 0.027 Uiso 1 1 calc R U . . .
C8A C 0.88103(11) 0.71933(9) 0.50387(9) 0.0177(3) Uani 1 1 d . . . . .
C9A C 0.87793(11) 0.63801(9) 0.51386(9) 0.0185(3) Uani 1 1 d . . . . .
C10A C 0.87416(12) 0.56606(10) 0.57841(10) 0.0246(4) Uani 1 1 d . . . . .
H10A H 0.873639 0.557604 0.628680 0.030 Uiso 1 1 calc R U . . .
C11A C 0.87142(13) 0.51111(10) 0.55071(10) 0.0260(4) Uani 1 1 d . . . . .
H11A H 0.868809 0.457319 0.579172 0.031 Uiso 1 1 calc R U . . .
C12A C 0.54231(12) 0.81706(9) 0.35052(9) 0.0213(3) Uani 1 1 d . . . . .
H12A H 0.474263 0.847985 0.360167 0.026 Uiso 1 1 calc R U . . .
C13A C 0.57615(12) 0.76965(9) 0.30675(9) 0.0194(3) Uani 1 1 d . . . . .
H13A H 0.536659 0.761706 0.280909 0.023 Uiso 1 1 calc R U . . .
C14A C 0.68336(11) 0.73581(9) 0.30955(8) 0.0147(3) Uani 1 1 d . . . . .
C15A C 0.76446(11) 0.68109(9) 0.27419(8) 0.0145(3) Uani 1 1 d . . . . .
C16A C 0.74518(12) 0.63725(9) 0.23973(9) 0.0179(3) Uani 1 1 d . . . . .
H16A H 0.676434 0.640610 0.237937 0.022 Uiso 1 1 calc R U . . .
C17A C 0.83160(12) 0.58841(9) 0.20815(9) 0.0187(3) Uani 1 1 d . . . . .
H17A H 0.821034 0.558698 0.184582 0.022 Uiso 1 1 calc R U . . .
C18A C 0.93401(12) 0.58374(9) 0.21163(9) 0.0168(3) Uani 1 1 d . . . . .
H18A H 0.992397 0.551549 0.190240 0.020 Uiso 1 1 calc R U . . .
C19A C 0.94672(11) 0.62836(8) 0.24785(8) 0.0143(3) Uani 1 1 d . . . . .
C20A C 1.04827(11) 0.63124(9) 0.25650(8) 0.0148(3) Uani 1 1 d . . . . .
C21A C 1.15337(12) 0.59563(9) 0.23039(9) 0.0182(3) Uani 1 1 d . . . . .
H21A H 1.177255 0.561140 0.202985 0.022 Uiso 1 1 calc R U . . .
C22A C 1.21345(12) 0.62314(9) 0.25439(9) 0.0205(3) Uani 1 1 d . . . . .
H22A H 1.287182 0.610726 0.245881 0.025 Uiso 1 1 calc R U . . .
Fe1B Fe 0.62292(2) 0.27431(2) 0.15326(2) 0.01163(6) Uani 1 1 d . . . . .
N1B N 0.62150(10) 0.10645(8) 0.28626(7) 0.0166(3) Uani 1 1 d . . . . .
H41B H 0.6311(14) 0.1226(11) 0.3214(11) 0.025 Uiso 1 1 d . U . . .
N2B N 0.61639(9) 0.15886(7) 0.21427(7) 0.0149(3) Uani 1 1 d . . . . .
N3B N 0.61508(9) 0.23965(7) 0.07602(7) 0.0151(3) Uani 1 1 d . . . . .
N4B N 0.62716(9) 0.37510(7) 0.06188(7) 0.0157(3) Uani 1 1 d . . . . .
N5B N 0.63152(10) 0.45171(7) 0.04508(8) 0.0182(3) Uani 1 1 d . . . . .
H42B H 0.6315(15) 0.4692(11) 0.0816(11) 0.027 Uiso 1 1 d . U . . .
N6B N 0.86293(10) 0.19524(7) 0.11290(8) 0.0169(3) Uani 1 1 d . . . . .
H43B H 0.8590(15) 0.1804(11) 0.0778(11) 0.025 Uiso 1 1 d . U . . .
N7B N 0.77976(10) 0.24334(7) 0.14270(7) 0.0147(3) Uani 1 1 d . . . . .
N8B N 0.63863(9) 0.31901(7) 0.22056(7) 0.0132(2) Uani 1 1 d . . . . .
N9B N 0.47136(9) 0.31793(7) 0.19562(7) 0.0142(2) Uani 1 1 d . . . . .
N10B N 0.37355(10) 0.31988(8) 0.19183(8) 0.0169(3) Uani 1 1 d . . . . .
H44B H 0.3659(14) 0.2914(11) 0.1666(11) 0.025 Uiso 1 1 d . U . . .
C1B C 0.62062(12) 0.03198(9) 0.29336(9) 0.0207(3) Uani 1 1 d . . . . .
H1B H 0.624099 -0.013871 0.337730 0.025 Uiso 1 1 calc R U . . .
C2B C 0.61370(12) 0.03560(9) 0.22387(9) 0.0190(3) Uani 1 1 d . . . . .
H2B H 0.610859 -0.006190 0.211618 0.023 Uiso 1 1 calc R U . . .
C3B C 0.61186(11) 0.11617(9) 0.17545(9) 0.0162(3) Uani 1 1 d . . . . .
C4B C 0.61194(11) 0.16239(9) 0.09415(9) 0.0156(3) Uani 1 1 d . . . . .
C5B C 0.61413(12) 0.13477(10) 0.03841(9) 0.0191(3) Uani 1 1 d . . . . .
H5B H 0.613088 0.081325 0.051198 0.023 Uiso 1 1 calc R U . . .
C6B C 0.61792(12) 0.18890(10) -0.03694(9) 0.0210(3) Uani 1 1 d . . . . .
H6B H 0.618514 0.171841 -0.075055 0.025 Uiso 1 1 calc R U . . .
C7B C 0.62083(12) 0.26857(10) -0.05568(9) 0.0205(3) Uani 1 1 d . . . . .
H7B H 0.623346 0.305089 -0.105997 0.025 Uiso 1 1 calc R U . . .
C8B C 0.61989(11) 0.29220(9) 0.00247(9) 0.0162(3) Uani 1 1 d . . . . .
C9B C 0.62511(11) 0.37131(9) -0.00411(9) 0.0170(3) Uani 1 1 d . . . . .
C10B C 0.62859(12) 0.44675(10) -0.06402(9) 0.0225(3) Uani 1 1 d . . . . .
H10B H 0.628501 0.460319 -0.115350 0.027 Uiso 1 1 calc R U . . .
C11B C 0.63213(12) 0.49580(9) -0.02989(10) 0.0231(4) Uani 1 1 d . . . . .
H11B H 0.634528 0.550031 -0.054272 0.028 Uiso 1 1 calc R U . . .
C12B C 0.94990(12) 0.18421(9) 0.13746(9) 0.0207(3) Uani 1 1 d . . . . .
H12B H 1.016603 0.153408 0.124093 0.025 Uiso 1 1 calc R U . . .
C13B C 0.92342(12) 0.22615(9) 0.18559(9) 0.0188(3) Uani 1 1 d . . . . .
H13B H 0.967106 0.229513 0.211422 0.023 Uiso 1 1 calc R U . . .
C14B C 0.81639(11) 0.26260(9) 0.18710(8) 0.0150(3) Uani 1 1 d . . . . .
C15B C 0.73685(11) 0.31357(9) 0.22667(8) 0.0146(3) Uani 1 1 d . . . . .
C16B C 0.75342(12) 0.35527(9) 0.26421(9) 0.0177(3) Uani 1 1 d . . . . .
H16B H 0.821535 0.351792 0.267352 0.021 Uiso 1 1 calc R U . . .
C17B C 0.66571(12) 0.40226(9) 0.29691(9) 0.0188(3) Uani 1 1 d . . . . .
H17B H 0.674779 0.430614 0.322471 0.023 Uiso 1 1 calc R U . . .
C18B C 0.56401(12) 0.40714(9) 0.29160(9) 0.0172(3) Uani 1 1 d . . . . .
H18B H 0.504791 0.438214 0.313661 0.021 Uiso 1 1 calc R U . . .
C19B C 0.55331(11) 0.36459(8) 0.25268(8) 0.0144(3) Uani 1 1 d . . . . .
C20B C 0.45630(11) 0.36126(8) 0.23904(8) 0.0144(3) Uani 1 1 d . . . . .
C21B C 0.34804(12) 0.39143(9) 0.26292(9) 0.0194(3) Uani 1 1 d . . . . .
H21B H 0.316689 0.423345 0.292968 0.023 Uiso 1 1 calc R U . . .
C22B C 0.29842(12) 0.36310(9) 0.23180(9) 0.0203(3) Uani 1 1 d . . . . .
H22B H 0.225458 0.372275 0.237445 0.024 Uiso 1 1 calc R U . . .
O1A O 0.08031(9) 0.69149(7) 1.06469(6) 0.0221(2) Uani 1 1 d . . . . .
O2A O -0.08639(9) 0.75816(7) 1.05086(7) 0.0241(3) Uani 1 1 d . . . . .
O3A O 0.01998(10) 0.53482(7) 0.86384(7) 0.0286(3) Uani 1 1 d . . . . .
N11A N 0.01292(11) 0.57208(8) 0.90885(7) 0.0204(3) Uani 1 1 d . . . . .
C23A C -0.00531(12) 0.70595(9) 1.04239(9) 0.0181(3) Uani 1 1 d . . . . .
C24A C -0.00020(12) 0.65423(9) 1.00001(9) 0.0175(3) Uani 1 1 d . . . . .
C25A C 0.09384(12) 0.60265(9) 0.98025(9) 0.0195(3) Uani 1 1 d . . . . .
H25A H 0.153136 0.595238 0.998079 0.023 Uiso 1 1 calc R U . . .
C26A C -0.08866(13) 0.66079(9) 0.97562(9) 0.0208(3) Uani 1 1 d . . . . .
H26A H -0.153225 0.693326 0.989885 0.025 Uiso 1 1 calc R U . . .
C27A C -0.08100(13) 0.61929(10) 0.93044(10) 0.0232(3) Uani 1 1 d . . . . .
H27A H -0.140618 0.623618 0.914561 0.028 Uiso 1 1 calc R U . . .
C28A C 0.09946(13) 0.56247(9) 0.93431(9) 0.0213(3) Uani 1 1 d . . . . .
H28A H 0.162893 0.528558 0.920627 0.026 Uiso 1 1 calc R U . . .
O4A O 0.38209(9) 0.11955(7) 0.51859(6) 0.0226(2) Uani 1 1 d . . . . .
O5A O 0.41393(10) 0.20870(7) 0.39723(7) 0.0279(3) Uani 1 1 d . . . . .
H1OA H 0.4242(17) 0.2521(13) 0.4212(12) 0.042 Uiso 1 1 d . U . . .
O6A O 0.33278(9) -0.05305(7) 0.32220(6) 0.0210(2) Uani 1 1 d . . . . .
N12A N 0.34594(10) -0.00671(8) 0.35140(7) 0.0170(3) Uani 1 1 d . . . . .
C29A C 0.39170(12) 0.14205(9) 0.44799(9) 0.0189(3) Uani 1 1 d . . . . .
C30A C 0.37635(11) 0.08930(9) 0.41424(9) 0.0170(3) Uani 1 1 d . . . . .
C31A C 0.37278(12) 0.00896(9) 0.45757(9) 0.0181(3) Uani 1 1 d . . . . .
H31A H 0.380062 -0.012988 0.508402 0.022 Uiso 1 1 calc R U . . .
C32A C 0.36341(12) 0.11997(9) 0.33861(9) 0.0189(3) Uani 1 1 d . . . . .
H32A H 0.365566 0.173505 0.308336 0.023 Uiso 1 1 calc R U . . .
C33A C 0.34754(12) 0.07195(9) 0.30850(9) 0.0186(3) Uani 1 1 d . . . . .
H33A H 0.337800 0.093419 0.258313 0.022 Uiso 1 1 calc R U . . .
C34A C 0.35847(12) -0.03823(9) 0.42540(9) 0.0190(3) Uani 1 1 d . . . . .
H34A H 0.357360 -0.092157 0.454485 0.023 Uiso 1 1 calc R U . . .
O7A O 0.15771(10) 0.66118(7) 0.45990(7) 0.0252(3) Uani 1 1 d . . . . .
O8A O 0.18334(9) 0.76600(7) 0.35026(6) 0.0224(2) Uani 1 1 d . . . . .
O9A O 0.10914(9) 0.92761(7) 0.58898(7) 0.0223(2) Uani 1 1 d . . . . .
N13A N 0.11787(10) 0.88275(8) 0.54963(7) 0.0178(3) Uani 1 1 d . . . . .
C35A C 0.16316(12) 0.73316(9) 0.42313(9) 0.0182(3) Uani 1 1 d . . . . .
C36A C 0.14617(11) 0.78628(9) 0.46803(9) 0.0169(3) Uani 1 1 d . . . . .
C37A C 0.14234(12) 0.86863(9) 0.43107(9) 0.0194(3) Uani 1 1 d . . . . .
H37A H 0.150052 0.891800 0.377866 0.023 Uiso 1 1 calc R U . . .
C38A C 0.13414(12) 0.75443(9) 0.54740(9) 0.0203(3) Uani 1 1 d . . . . .
H38A H 0.135607 0.699746 0.573822 0.024 Uiso 1 1 calc R U . . .
C39A C 0.12006(13) 0.80291(9) 0.58739(9) 0.0210(3) Uani 1 1 d . . . . .
H39A H 0.111978 0.780864 0.640639 0.025 Uiso 1 1 calc R U . . .
C40A C 0.12731(12) 0.91593(9) 0.47238(9) 0.0198(3) Uani 1 1 d . . . . .
H40A H 0.123596 0.971007 0.447147 0.024 Uiso 1 1 calc R U . . .
O1B O 0.42316(9) 0.30650(7) 0.44324(7) 0.0243(3) Uani 1 1 d . . . . .
O2B O 0.58907(9) 0.24102(7) 0.46007(7) 0.0262(3) Uani 1 1 d . . . . .
O3B O 0.47827(11) 0.47112(7) 0.63934(7) 0.0298(3) Uani 1 1 d . . . . .
N11B N 0.48626(11) 0.43260(8) 0.59512(8) 0.0214(3) Uani 1 1 d . . . . .
C23B C 0.50715(13) 0.29351(9) 0.46629(9) 0.0194(3) Uani 1 1 d . . . . .
C24B C 0.50094(12) 0.34716(9) 0.50676(9) 0.0183(3) Uani 1 1 d . . . . .
C25B C 0.40653(12) 0.39915(9) 0.52536(9) 0.0199(3) Uani 1 1 d . . . . .
H25B H 0.347501 0.405661 0.507671 0.024 Uiso 1 1 calc R U . . .
C26B C 0.58879(13) 0.34177(10) 0.53102(9) 0.0216(3) Uani 1 1 d . . . . .
H26B H 0.653497 0.308871 0.517602 0.026 Uiso 1 1 calc R U . . .
C27B C 0.58044(13) 0.38498(10) 0.57490(10) 0.0233(3) Uani 1 1 d . . . . .
H27B H 0.639679 0.381479 0.590740 0.028 Uiso 1 1 calc R U . . .
C28B C 0.40028(13) 0.44101(9) 0.56990(9) 0.0212(3) Uani 1 1 d . . . . .
H28B H 0.336698 0.475253 0.582765 0.025 Uiso 1 1 calc R U . . .
O4B O 0.12333(9) 0.87587(7) 0.98740(6) 0.0229(2) Uani 1 1 d . . . . .
O5B O 0.09637(10) 0.78818(7) 1.10949(7) 0.0265(3) Uani 1 1 d . . . . .
H1OB H 0.0837(17) 0.7436(13) 1.0854(12) 0.040 Uiso 1 1 d . U . . .
O6B O 0.16449(9) 1.06289(7) 1.17298(7) 0.0218(2) Uani 1 1 d . . . . .
N12B N 0.15602(10) 1.01324(8) 1.14582(8) 0.0174(3) Uani 1 1 d . . . . .
C29B C 0.11601(12) 0.85491(9) 1.05721(9) 0.0187(3) Uani 1 1 d . . . . .
C30B C 0.13098(12) 0.91043(9) 1.08807(9) 0.0177(3) Uani 1 1 d . . . . .
C31B C 0.13236(12) 0.99058(9) 1.04230(9) 0.0190(3) Uani 1 1 d . . . . .
H31B H 0.124826 1.010232 0.991700 0.023 Uiso 1 1 calc R U . . .
C32B C 0.14439(12) 0.88320(9) 1.16311(9) 0.0192(3) Uani 1 1 d . . . . .
H32B H 0.144263 0.829731 1.194827 0.023 Uiso 1 1 calc R U . . .
C33B C 0.15778(12) 0.93452(9) 1.19067(9) 0.0190(3) Uani 1 1 d . . . . .
H33B H 0.168150 0.915227 1.240497 0.023 Uiso 1 1 calc R U . . .
C34B C 0.14485(12) 1.04099(9) 1.07162(9) 0.0183(3) Uani 1 1 d . . . . .
H34B H 0.145688 1.094540 1.040572 0.022 Uiso 1 1 calc R U . . .
O7B O 0.34097(10) 0.33116(7) 1.03042(7) 0.0247(3) Uani 1 1 d . . . . .
O8B O 0.33096(9) 0.22445(7) 1.13992(6) 0.0223(2) Uani 1 1 d . . . . .
O9B O 0.37932(9) 0.06364(7) 0.90577(7) 0.0226(2) Uani 1 1 d . . . . .
N13B N 0.37396(10) 0.10874(8) 0.94396(7) 0.0179(3) Uani 1 1 d . . . . .
C35B C 0.34127(12) 0.25821(9) 1.06746(9) 0.0180(3) Uani 1 1 d . . . . .
C36B C 0.35407(11) 0.20510(9) 1.02361(9) 0.0166(3) Uani 1 1 d . . . . .
C37B C 0.36429(12) 0.12219(9) 1.06037(9) 0.0186(3) Uani 1 1 d . . . . .
H37B H 0.363624 0.098612 1.112760 0.022 Uiso 1 1 calc R U . . .
C38B C 0.35550(12) 0.23774(9) 0.94556(9) 0.0202(3) Uani 1 1 d . . . . .
H38B H 0.349781 0.292905 0.919328 0.024 Uiso 1 1 calc R U . . .
C39B C 0.36532(12) 0.18928(9) 0.90652(9) 0.0204(3) Uani 1 1 d . . . . .
H39B H 0.366029 0.211881 0.854121 0.024 Uiso 1 1 calc R U . . .
C40B C 0.37535(12) 0.07479(9) 1.01995(9) 0.0186(3) Uani 1 1 d . . . . .
H40B H 0.383811 0.019276 1.044820 0.022 Uiso 1 1 calc R U . . .
O1WA O 0.58802(10) 0.07417(7) 0.81922(7) 0.0240(3) Uani 1 1 d . . . . .
H1C H 0.6074(17) 0.0598(13) 0.7814(13) 0.036 Uiso 1 1 d . U . . .
H1D H 0.5273(19) 0.0712(13) 0.8371(13) 0.036 Uiso 1 1 d . U . . .
O1WB O 0.90410(10) 0.91962(7) 0.68259(7) 0.0252(3) Uani 1 1 d . . . . .
H1E H 0.8868(18) 0.9349(13) 0.7198(13) 0.038 Uiso 1 1 d . U . . .
H1F H 0.9669(19) 0.9220(13) 0.6625(13) 0.038 Uiso 1 1 d . U . . .
O2WA O 0.37594(10) 0.77148(8) 0.23271(8) 0.0263(3) Uani 1 1 d . . . . .
H2C H 0.3253(19) 0.7702(14) 0.2694(14) 0.040 Uiso 1 1 d . U . . .
H2D H 0.3860(18) 0.8158(15) 0.2154(13) 0.040 Uiso 1 1 d . U . . .
O2WB O 0.13349(11) 0.23416(8) 0.25689(8) 0.0286(3) Uani 1 1 d . . . . .
H2E H 0.1195(18) 0.1894(15) 0.2787(14) 0.043 Uiso 1 1 d . U . . .
H2F H 0.1814(19) 0.2325(14) 0.2217(14) 0.043 Uiso 1 1 d . U . . .
O3WA O 0.82796(11) 0.86458(8) 0.12825(8) 0.0289(3) Uani 1 1 d . . . . .
H3C H 0.8566(18) 0.8319(14) 0.1062(13) 0.043 Uiso 1 1 d . U . . .
H3D H 0.7655(19) 0.8864(14) 0.1198(13) 0.043 Uiso 1 1 d . U . . .
O3WB O 0.68433(11) 0.14275(8) 0.37901(8) 0.0287(3) Uani 1 1 d . . . . .
H3E H 0.6521(18) 0.1738(14) 0.4036(13) 0.043 Uiso 1 1 d . U . . .
H3F H 0.7437(19) 0.1214(14) 0.3854(13) 0.043 Uiso 1 1 d . U . . .
O4WA O 0.13634(11) 0.54396(8) 0.60173(8) 0.0295(3) Uani 1 1 d . . . . .
H4C H 0.0974(19) 0.5595(14) 0.6356(14) 0.044 Uiso 1 1 d . U . . .
H4D H 0.1404(18) 0.5827(15) 0.5615(14) 0.044 Uiso 1 1 d . U . . .
O4WB O 0.36147(11) 0.44958(8) 0.88732(8) 0.0297(3) Uani 1 1 d . . . . .
H4E H 0.4046(19) 0.4326(14) 0.8571(14) 0.045 Uiso 1 1 d . U . . .
H4F H 0.3562(18) 0.4127(15) 0.9292(15) 0.045 Uiso 1 1 d . U . . .
O5WA O 0.99864(12) 0.62522(8) 0.71497(8) 0.0343(3) Uani 1 1 d . . . . .
H5C H 1.003(2) 0.5983(16) 0.7608(15) 0.051 Uiso 1 1 d . U . . .
H5D H 0.962(2) 0.6680(16) 0.7199(14) 0.051 Uiso 1 1 d . U . . .
O5WB O 0.51215(11) 0.37708(9) 0.78262(8) 0.0329(3) Uani 1 1 d . . . . .
H5E H 0.5031(19) 0.4039(15) 0.7390(15) 0.049 Uiso 1 1 d . U . . .
H5F H 0.540(2) 0.3307(16) 0.7825(14) 0.049 Uiso 1 1 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
Fe1A N8A 2.1165(12) . ?
Fe1A N3A 2.1288(13) . ?
Fe1A N2A 2.1539(12) . ?
Fe1A N4A 2.1781(13) . ?
Fe1A N7A 2.1870(12) . ?
Fe1A N9A 2.1880(12) . ?
N1A N2A 1.3430(18) . ?
N1A C1A 1.344(2) . ?
N1A H41A 0.90(2) . ?
N2A C3A 1.343(2) . ?
N3A C8A 1.346(2) . ?
N3A C4A 1.3469(19) . ?
N4A C9A 1.338(2) . ?
N4A N5A 1.3499(17) . ?
N5A C11A 1.348(2) . ?
N5A H42A 0.90(2) . ?
N6A C12A 1.344(2) . ?
N6A N7A 1.3469(17) . ?
N6A H43A 0.83(2) . ?
N7A C14A 1.342(2) . ?
N8A C19A 1.3435(19) . ?
N8A C15A 1.3440(19) . ?
N9A C20A 1.3417(19) . ?
N9A N10A 1.3473(17) . ?
N10A C22A 1.346(2) . ?
N10A H44A 0.90(2) . ?
C1A C2A 1.374(2) . ?
C1A H1A 0.9300 . ?
C2A C3A 1.407(2) . ?
C2A H2A 0.9300 . ?
C3A C4A 1.467(2) . ?
C4A C5A 1.390(2) . ?
C5A C6A 1.392(2) . ?
C5A H5A 0.9300 . ?
C6A C7A 1.388(2) . ?
C6A H6A 0.9300 . ?
C7A C8A 1.387(2) . ?
C7A H7A 0.9300 . ?
C8A C9A 1.469(2) . ?
C9A C10A 1.407(2) . ?
C10A C11A 1.373(3) . ?
C10A H10A 0.9300 . ?
C11A H11A 0.9300 . ?
C12A C13A 1.371(2) . ?
C12A H12A 0.9300 . ?
C13A C14A 1.401(2) . ?
C13A H13A 0.9300 . ?
C14A C15A 1.463(2) . ?
C15A C16A 1.393(2) . ?
C16A C17A 1.388(2) . ?
C16A H16A 0.9300 . ?
C17A C18A 1.393(2) . ?
C17A H17A 0.9300 . ?
C18A C19A 1.388(2) . ?
C18A H18A 0.9300 . ?
C19A C20A 1.469(2) . ?
C20A C21A 1.400(2) . ?
C21A C22A 1.377(2) . ?
C21A H21A 0.9300 . ?
C22A H22A 0.9300 . ?
Fe1B N3B 1.9342(13) . ?
Fe1B N8B 1.9380(12) . ?
Fe1B N4B 1.9800(12) . ?
Fe1B N7B 1.9905(12) . ?
Fe1B N2B 1.9982(12) . ?
Fe1B N9B 2.0010(12) . ?
N1B N2B 1.3448(17) . ?
N1B C1B 1.351(2) . ?
N1B H41B 0.922(19) . ?
N2B C3B 1.3484(19) . ?
N3B C4B 1.3521(19) . ?
N3B C8B 1.3538(19) . ?
N4B C9B 1.340(2) . ?
N4B N5B 1.3508(17) . ?
N5B C11B 1.347(2) . ?
N5B H42B 0.908(19) . ?
N6B N7B 1.3431(17) . ?
N6B C12B 1.345(2) . ?
N6B H43B 0.87(2) . ?
N7B C14B 1.347(2) . ?
N8B C15B 1.3501(19) . ?
N8B C19B 1.3513(19) . ?
N9B C20B 1.3446(19) . ?
N9B N10B 1.3473(17) . ?
N10B C22B 1.346(2) . ?
N10B H44B 0.917(19) . ?
C1B C2B 1.372(2) . ?
C1B H1B 0.9300 . ?
C2B C3B 1.401(2) . ?
C2B H2B 0.9300 . ?
C3B C4B 1.458(2) . ?
C4B C5B 1.388(2) . ?
C5B C6B 1.390(2) . ?
C5B H5B 0.9300 . ?
C6B C7B 1.393(2) . ?
C6B H6B 0.9300 . ?
C7B C8B 1.388(2) . ?
C7B H7B 0.9300 . ?
C8B C9B 1.461(2) . ?
C9B C10B 1.408(2) . ?
C10B C11B 1.372(2) . ?
C10B H10B 0.9300 . ?
C11B H11B 0.9300 . ?
C12B C13B 1.371(2) . ?
C12B H12B 0.9300 . ?
C13B C14B 1.393(2) . ?
C13B H13B 0.9300 . ?
C14B C15B 1.455(2) . ?
C15B C16B 1.389(2) . ?
C16B C17B 1.388(2) . ?
C16B H16B 0.9300 . ?
C17B C18B 1.394(2) . ?
C17B H17B 0.9300 . ?
C18B C19B 1.385(2) . ?
C18B H18B 0.9300 . ?
C19B C20B 1.457(2) . ?
C20B C21B 1.398(2) . ?
C21B C22B 1.377(2) . ?
C21B H21B 0.9300 . ?
C22B H22B 0.9300 . ?
O1A C23A 1.2856(19) . ?
O1A H1OB 1.23(2) . ?
O2A C23A 1.2368(19) . ?
O3A N11A 1.3096(17) . ?
N11A C27A 1.356(2) . ?
N11A C28A 1.358(2) . ?
C23A C24A 1.502(2) . ?
C24A C25A 1.388(2) . ?
C24A C26A 1.389(2) . ?
C25A C28A 1.376(2) . ?
C25A H25A 0.9300 . ?
C26A C27A 1.374(2) . ?
C26A H26A 0.9300 . ?
C27A H27A 0.9300 . ?
C28A H28A 0.9300 . ?
O4A C29A 1.2411(19) . ?
O5A C29A 1.2810(19) . ?
O5A H1OA 1.16(2) . ?
O6A N12A 1.3106(17) . ?
N12A C33A 1.358(2) . ?
N12A C34A 1.363(2) . ?
C29A C30A 1.502(2) . ?
C30A C31A 1.390(2) . ?
C30A C32A 1.396(2) . ?
C31A C34A 1.378(2) . ?
C31A H31A 0.9300 . ?
C32A C33A 1.371(2) . ?
C32A H32A 0.9300 . ?
C33A H33A 0.9300 . ?
C34A H34A 0.9300 . ?
O7A C35A 1.2473(19) . ?
O8A C35A 1.2687(19) . ?
O9A N13A 1.3258(16) . ?
N13A C40A 1.353(2) . ?
N13A C39A 1.356(2) . ?
C35A C36A 1.517(2) . ?
C36A C38A 1.386(2) . ?
C36A C37A 1.393(2) . ?
C37A C40A 1.373(2) . ?
C37A H37A 0.9300 . ?
C38A C39A 1.374(2) . ?
C38A H38A 0.9300 . ?
C39A H39A 0.9300 . ?
C40A H40A 0.9300 . ?
O1B C23B 1.279(2) . ?
O1B H1OA 1.26(2) . ?
O2B C23B 1.2393(19) . ?
O3B N11B 1.3110(17) . ?
N11B C28B 1.355(2) . ?
N11B C27B 1.355(2) . ?
C23B C24B 1.499(2) . ?
C24B C26B 1.387(2) . ?
C24B C25B 1.389(2) . ?
C25B C28B 1.375(2) . ?
C25B H25B 0.9300 . ?
C26B C27B 1.376(2) . ?
C26B H26B 0.9300 . ?
C27B H27B 0.9300 . ?
C28B H28B 0.9300 . ?
O4B C29B 1.2349(19) . ?
O5B C29B 1.2811(19) . ?
O5B H1OB 1.20(2) . ?
O6B N12B 1.3064(17) . ?
N12B C33B 1.359(2) . ?
N12B C34B 1.366(2) . ?
C29B C30B 1.504(2) . ?
C30B C31B 1.390(2) . ?
C30B C32B 1.394(2) . ?
C31B C34B 1.377(2) . ?
C31B H31B 0.9300 . ?
C32B C33B 1.373(2) . ?
C32B H32B 0.9300 . ?
C33B H33B 0.9300 . ?
C34B H34B 0.9300 . ?
O7B C35B 1.2481(19) . ?
O8B C35B 1.2686(19) . ?
O9B N13B 1.3258(17) . ?
N13B C40B 1.355(2) . ?
N13B C39B 1.356(2) . ?
C35B C36B 1.516(2) . ?
C36B C38B 1.385(2) . ?
C36B C37B 1.391(2) . ?
C37B C40B 1.375(2) . ?
C37B H37B 0.9300 . ?
C38B C39B 1.375(2) . ?
C38B H38B 0.9300 . ?
C39B H39B 0.9300 . ?
C40B H40B 0.9300 . ?
O1WA H1C 0.83(2) . ?
O1WA H1D 0.80(2) . ?
O1WB H1E 0.83(2) . ?
O1WB H1F 0.83(2) . ?
O2WA H2C 0.82(2) . ?
O2WA H2D 0.79(2) . ?
O2WB H2E 0.82(3) . ?
O2WB H2F 0.79(2) . ?
O3WA H3C 0.83(2) . ?
O3WA H3D 0.85(2) . ?
O3WB H3E 0.84(2) . ?
O3WB H3F 0.80(2) . ?
O4WA H4C 0.80(2) . ?
O4WA H4D 0.82(3) . ?
O4WB H4E 0.78(2) . ?
O4WB H4F 0.82(3) . ?
O5WA H5C 0.84(3) . ?
O5WA H5D 0.83(3) . ?
O5WB H5E 0.82(3) . ?
O5WB H5F 0.83(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
N8A Fe1A N3A 168.13(5) . . ?
N8A Fe1A N2A 116.38(5) . . ?
N3A Fe1A N2A 74.04(5) . . ?
N8A Fe1A N4A 95.19(5) . . ?
N3A Fe1A N4A 74.10(5) . . ?
N2A Fe1A N4A 148.11(5) . . ?
N8A Fe1A N7A 74.82(5) . . ?
N3A Fe1A N7A 100.29(5) . . ?
N2A Fe1A N7A 90.77(5) . . ?
N4A Fe1A N7A 93.49(5) . . ?
N8A Fe1A N9A 74.24(5) . . ?
N3A Fe1A N9A 110.65(5) . . ?
N2A Fe1A N9A 100.25(5) . . ?
N4A Fe1A N9A 92.19(5) . . ?
N7A Fe1A N9A 148.91(5) . . ?
N2A N1A C1A 111.44(14) . . ?
N2A N1A H41A 116.5(12) . . ?
C1A N1A H41A 131.7(12) . . ?
C3A N2A N1A 105.91(12) . . ?
C3A N2A Fe1A 117.19(10) . . ?
N1A N2A Fe1A 136.86(10) . . ?
C8A N3A C4A 120.00(13) . . ?
C8A N3A Fe1A 119.82(10) . . ?
C4A N3A Fe1A 119.87(10) . . ?
C9A N4A N5A 105.53(13) . . ?
C9A N4A Fe1A 116.34(10) . . ?
N5A N4A Fe1A 138.13(11) . . ?
C11A N5A N4A 111.47(14) . . ?
C11A N5A H42A 128.7(13) . . ?
N4A N5A H42A 119.9(13) . . ?
C12A N6A N7A 111.67(13) . . ?
C12A N6A H43A 128.3(14) . . ?
N7A N6A H43A 119.8(14) . . ?
C14A N7A N6A 105.22(12) . . ?
C14A N7A Fe1A 114.49(9) . . ?
N6A N7A Fe1A 138.82(10) . . ?
C19A N8A C15A 120.25(13) . . ?
C19A N8A Fe1A 120.05(10) . . ?
C15A N8A Fe1A 119.36(10) . . ?
C20A N9A N10A 105.27(12) . . ?
C20A N9A Fe1A 115.25(9) . . ?
N10A N9A Fe1A 139.40(10) . . ?
C22A N10A N9A 111.54(13) . . ?
C22A N10A H44A 130.5(12) . . ?
N9A N10A H44A 117.9(12) . . ?
N1A C1A C2A 107.76(14) . . ?
N1A C1A H1A 126.1 . . ?
C2A C1A H1A 126.1 . . ?
C1A C2A C3A 104.76(14) . . ?
C1A C2A H2A 127.6 . . ?
C3A C2A H2A 127.6 . . ?
N2A C3A C2A 110.14(14) . . ?
N2A C3A C4A 116.16(13) . . ?
C2A C3A C4A 133.61(15) . . ?
N3A C4A C5A 121.86(14) . . ?
N3A C4A C3A 112.67(13) . . ?
C5A C4A C3A 125.41(14) . . ?
C4A C5A C6A 117.95(15) . . ?
C4A C5A H5A 121.0 . . ?
C6A C5A H5A 121.0 . . ?
C7A C6A C5A 120.14(15) . . ?
C7A C6A H6A 119.9 . . ?
C5A C6A H6A 119.9 . . ?
C8A C7A C6A 118.74(15) . . ?
C8A C7A H7A 120.6 . . ?
C6A C7A H7A 120.6 . . ?
N3A C8A C7A 121.30(14) . . ?
N3A C8A C9A 112.93(13) . . ?
C7A C8A C9A 125.74(14) . . ?
N4A C9A C10A 110.67(14) . . ?
N4A C9A C8A 116.66(13) . . ?
C10A C9A C8A 132.67(15) . . ?
C11A C10A C9A 104.70(15) . . ?
C11A C10A H10A 127.6 . . ?
C9A C10A H10A 127.6 . . ?
N5A C11A C10A 107.63(14) . . ?
N5A C11A H11A 126.2 . . ?
C10A C11A H11A 126.2 . . ?
N6A C12A C13A 107.61(14) . . ?
N6A C12A H12A 126.2 . . ?
C13A C12A H12A 126.2 . . ?
C12A C13A C14A 104.75(14) . . ?
C12A C13A H13A 127.6 . . ?
C14A C13A H13A 127.6 . . ?
N7A C14A C13A 110.75(13) . . ?
N7A C14A C15A 117.25(13) . . ?
C13A C14A C15A 132.00(14) . . ?
N8A C15A C16A 121.57(13) . . ?
N8A C15A C14A 113.04(13) . . ?
C16A C15A C14A 125.39(13) . . ?
C17A C16A C15A 118.07(14) . . ?
C17A C16A H16A 121.0 . . ?
C15A C16A H16A 121.0 . . ?
C16A C17A C18A 120.27(14) . . ?
C16A C17A H17A 119.9 . . ?
C18A C17A H17A 119.9 . . ?
C19A C18A C17A 118.30(14) . . ?
C19A C18A H18A 120.9 . . ?
C17A C18A H18A 120.9 . . ?
N8A C19A C18A 121.52(13) . . ?
N8A C19A C20A 112.66(13) . . ?
C18A C19A C20A 125.82(13) . . ?
N9A C20A C21A 111.02(13) . . ?
N9A C20A C19A 117.09(13) . . ?
C21A C20A C19A 131.87(14) . . ?
C22A C21A C20A 104.47(14) . . ?
C22A C21A H21A 127.8 . . ?
C20A C21A H21A 127.8 . . ?
N10A C22A C21A 107.70(14) . . ?
N10A C22A H22A 126.2 . . ?
C21A C22A H22A 126.2 . . ?
N3B Fe1B N8B 173.16(5) . . ?
N3B Fe1B N4B 79.24(5) . . ?
N8B Fe1B N4B 94.47(5) . . ?
N3B Fe1B N7B 98.60(5) . . ?
N8B Fe1B N7B 79.00(5) . . ?
N4B Fe1B N7B 93.98(5) . . ?
N3B Fe1B N2B 78.46(5) . . ?
N8B Fe1B N2B 107.78(5) . . ?
N4B Fe1B N2B 157.70(5) . . ?
N7B Fe1B N2B 89.03(5) . . ?
N3B Fe1B N9B 104.15(5) . . ?
N8B Fe1B N9B 78.44(5) . . ?
N4B Fe1B N9B 90.77(5) . . ?
N7B Fe1B N9B 157.24(5) . . ?
N2B Fe1B N9B 94.96(5) . . ?
N2B N1B C1B 110.68(13) . . ?
N2B N1B H41B 120.1(11) . . ?
C1B N1B H41B 129.0(11) . . ?
N1B N2B C3B 106.07(12) . . ?
N1B N2B Fe1B 137.48(10) . . ?
C3B N2B Fe1B 116.30(10) . . ?
C4B N3B C8B 120.30(13) . . ?
C4B N3B Fe1B 120.36(10) . . ?
C8B N3B Fe1B 119.19(10) . . ?
C9B N4B N5B 106.06(12) . . ?
C9B N4B Fe1B 116.25(10) . . ?
N5B N4B Fe1B 137.69(11) . . ?
C11B N5B N4B 110.89(14) . . ?
C11B N5B H42B 126.9(12) . . ?
N4B N5B H42B 122.1(12) . . ?
N7B N6B C12B 110.81(13) . . ?
N7B N6B H43B 121.0(12) . . ?
C12B N6B H43B 127.6(12) . . ?
N6B N7B C14B 105.67(12) . . ?
N6B N7B Fe1B 137.61(10) . . ?
C14B N7B Fe1B 115.52(10) . . ?
C15B N8B C19B 120.02(13) . . ?
C15B N8B Fe1B 119.45(10) . . ?
C19B N8B Fe1B 119.91(10) . . ?
C20B N9B N10B 105.76(12) . . ?
C20B N9B Fe1B 115.65(9) . . ?
N10B N9B Fe1B 138.54(10) . . ?
C22B N10B N9B 110.82(13) . . ?
C22B N10B H44B 129.3(11) . . ?
N9B N10B H44B 119.7(11) . . ?
N1B C1B C2B 108.26(14) . . ?
N1B C1B H1B 125.9 . . ?
C2B C1B H1B 125.9 . . ?
C1B C2B C3B 104.72(14) . . ?
C1B C2B H2B 127.6 . . ?
C3B C2B H2B 127.6 . . ?
N2B C3B C2B 110.26(13) . . ?
N2B C3B C4B 114.08(13) . . ?
C2B C3B C4B 135.56(14) . . ?
N3B C4B C5B 121.31(14) . . ?
N3B C4B C3B 110.77(13) . . ?
C5B C4B C3B 127.84(14) . . ?
C4B C5B C6B 118.41(15) . . ?
C4B C5B H5B 120.8 . . ?
C6B C5B H5B 120.8 . . ?
C5B C6B C7B 120.35(15) . . ?
C5B C6B H6B 119.8 . . ?
C7B C6B H6B 119.8 . . ?
C8B C7B C6B 118.47(15) . . ?
C8B C7B H7B 120.8 . . ?
C6B C7B H7B 120.8 . . ?
N3B C8B C7B 121.14(14) . . ?
N3B C8B C9B 110.96(13) . . ?
C7B C8B C9B 127.90(14) . . ?
N4B C9B C10B 110.25(14) . . ?
N4B C9B C8B 114.29(13) . . ?
C10B C9B C8B 135.47(15) . . ?
C11B C10B C9B 104.73(14) . . ?
C11B C10B H10B 127.6 . . ?
C9B C10B H10B 127.6 . . ?
N5B C11B C10B 108.07(14) . . ?
N5B C11B H11B 126.0 . . ?
C10B C11B H11B 126.0 . . ?
N6B C12B C13B 108.33(13) . . ?
N6B C12B H12B 125.8 . . ?
C13B C12B H12B 125.8 . . ?
C12B C13B C14B 104.48(14) . . ?
C12B C13B H13B 127.8 . . ?
C14B C13B H13B 127.8 . . ?
N7B C14B C13B 110.71(13) . . ?
N7B C14B C15B 114.43(13) . . ?
C13B C14B C15B 134.83(14) . . ?
N8B C15B C16B 121.57(13) . . ?
N8B C15B C14B 110.66(13) . . ?
C16B C15B C14B 127.73(13) . . ?
C17B C16B C15B 118.28(14) . . ?
C17B C16B H16B 120.9 . . ?
C15B C16B H16B 120.9 . . ?
C16B C17B C18B 120.29(14) . . ?
C16B C17B H17B 119.9 . . ?
C18B C17B H17B 119.9 . . ?
C19B C18B C17B 118.41(14) . . ?
C19B C18B H18B 120.8 . . ?
C17B C18B H18B 120.8 . . ?
N8B C19B C18B 121.42(13) . . ?
N8B C19B C20B 110.40(13) . . ?
C18B C19B C20B 128.18(14) . . ?
N9B C20B C21B 110.84(13) . . ?
N9B C20B C19B 114.70(13) . . ?
C21B C20B C19B 134.43(14) . . ?
C22B C21B C20B 104.24(14) . . ?
C22B C21B H21B 127.9 . . ?
C20B C21B H21B 127.9 . . ?
N10B C22B C21B 108.34(14) . . ?
N10B C22B H22B 125.8 . . ?
C21B C22B H22B 125.8 . . ?
C23A O1A H1OB 113.5(10) . . ?
O3A N11A C27A 119.87(14) . . ?
O3A N11A C28A 119.73(13) . . ?
C27A N11A C28A 120.39(14) . . ?
O2A C23A O1A 126.43(15) . . ?
O2A C23A C24A 119.54(14) . . ?
O1A C23A C24A 114.00(13) . . ?
C25A C24A C26A 118.42(15) . . ?
C25A C24A C23A 121.25(14) . . ?
C26A C24A C23A 120.22(14) . . ?
C28A C25A C24A 120.11(15) . . ?
C28A C25A H25A 119.9 . . ?
C24A C25A H25A 119.9 . . ?
C27A C26A C24A 120.13(15) . . ?
C27A C26A H26A 119.9 . . ?
C24A C26A H26A 119.9 . . ?
N11A C27A C26A 120.46(15) . . ?
N11A C27A H27A 119.8 . . ?
C26A C27A H27A 119.8 . . ?
N11A C28A C25A 120.37(14) . . ?
N11A C28A H28A 119.8 . . ?
C25A C28A H28A 119.8 . . ?
C29A O5A H1OA 115.3(11) . . ?
O6A N12A C33A 120.56(13) . . ?
O6A N12A C34A 119.39(13) . . ?
C33A N12A C34A 120.04(13) . . ?
O4A C29A O5A 126.63(15) . . ?
O4A C29A C30A 120.21(14) . . ?
O5A C29A C30A 113.16(14) . . ?
C31A C30A C32A 117.93(14) . . ?
C31A C30A C29A 121.20(14) . . ?
C32A C30A C29A 120.86(14) . . ?
C34A C31A C30A 120.15(15) . . ?
C34A C31A H31A 119.9 . . ?
C30A C31A H31A 119.9 . . ?
C33A C32A C30A 120.65(14) . . ?
C33A C32A H32A 119.7 . . ?
C30A C32A H32A 119.7 . . ?
N12A C33A C32A 120.51(14) . . ?
N12A C33A H33A 119.7 . . ?
C32A C33A H33A 119.7 . . ?
N12A C34A C31A 120.70(14) . . ?
N12A C34A H34A 119.7 . . ?
C31A C34A H34A 119.7 . . ?
O9A N13A C40A 120.27(13) . . ?
O9A N13A C39A 119.28(13) . . ?
C40A N13A C39A 120.43(14) . . ?
O7A C35A O8A 125.12(15) . . ?
O7A C35A C36A 118.28(14) . . ?
O8A C35A C36A 116.60(13) . . ?
C38A C36A C37A 117.63(14) . . ?
C38A C36A C35A 121.08(14) . . ?
C37A C36A C35A 121.29(14) . . ?
C40A C37A C36A 120.68(15) . . ?
C40A C37A H37A 119.7 . . ?
C36A C37A H37A 119.7 . . ?
C39A C38A C36A 120.59(14) . . ?
C39A C38A H38A 119.7 . . ?
C36A C38A H38A 119.7 . . ?
N13A C39A C38A 120.37(15) . . ?
N13A C39A H39A 119.8 . . ?
C38A C39A H39A 119.8 . . ?
N13A C40A C37A 120.26(14) . . ?
N13A C40A H40A 119.9 . . ?
C37A C40A H40A 119.9 . . ?
C23B O1B H1OA 112.7(10) . . ?
O3B N11B C28B 119.64(13) . . ?
O3B N11B C27B 119.73(14) . . ?
C28B N11B C27B 120.64(14) . . ?
O2B C23B O1B 126.79(15) . . ?
O2B C23B C24B 118.71(14) . . ?
O1B C23B C24B 114.48(14) . . ?
C26B C24B C25B 118.44(15) . . ?
C26B C24B C23B 119.97(14) . . ?
C25B C24B C23B 121.46(14) . . ?
C28B C25B C24B 120.07(15) . . ?
C28B C25B H25B 120.0 . . ?
C24B C25B H25B 120.0 . . ?
C27B C26B C24B 120.15(15) . . ?
C27B C26B H26B 119.9 . . ?
C24B C26B H26B 119.9 . . ?
N11B C27B C26B 120.27(15) . . ?
N11B C27B H27B 119.9 . . ?
C26B C27B H27B 119.9 . . ?
N11B C28B C25B 120.34(14) . . ?
N11B C28B H28B 119.8 . . ?
C25B C28B H28B 119.8 . . ?
C29B O5B H1OB 113.9(10) . . ?
O6B N12B C33B 120.68(13) . . ?
O6B N12B C34B 119.55(13) . . ?
C33B N12B C34B 119.77(13) . . ?
O4B C29B O5B 126.75(15) . . ?
O4B C29B C30B 119.81(14) . . ?
O5B C29B C30B 113.44(14) . . ?
C31B C30B C32B 117.96(15) . . ?
C31B C30B C29B 120.83(14) . . ?
C32B C30B C29B 121.20(14) . . ?
C34B C31B C30B 120.20(15) . . ?
C34B C31B H31B 119.9 . . ?
C30B C31B H31B 119.9 . . ?
C33B C32B C30B 120.65(14) . . ?
C33B C32B H32B 119.7 . . ?
C30B C32B H32B 119.7 . . ?
N12B C33B C32B 120.60(14) . . ?
N12B C33B H33B 119.7 . . ?
C32B C33B H33B 119.7 . . ?
N12B C34B C31B 120.76(14) . . ?
N12B C34B H34B 119.6 . . ?
C31B C34B H34B 119.6 . . ?
O9B N13B C40B 120.28(13) . . ?
O9B N13B C39B 119.31(13) . . ?
C40B N13B C39B 120.40(14) . . ?
O7B C35B O8B 124.93(15) . . ?
O7B C35B C36B 118.36(14) . . ?
O8B C35B C36B 116.71(13) . . ?
C38B C36B C37B 117.84(14) . . ?
C38B C36B C35B 120.94(14) . . ?
C37B C36B C35B 121.22(14) . . ?
C40B C37B C36B 120.60(14) . . ?
C40B C37B H37B 119.7 . . ?
C36B C37B H37B 119.7 . . ?
C39B C38B C36B 120.54(14) . . ?
C39B C38B H38B 119.7 . . ?
C36B C38B H38B 119.7 . . ?
N13B C39B C38B 120.39(15) . . ?
N13B C39B H39B 119.8 . . ?
C38B C39B H39B 119.8 . . ?
N13B C40B C37B 120.19(14) . . ?
N13B C40B H40B 119.9 . . ?
C37B C40B H40B 119.9 . . ?
H1C O1WA H1D 107(2) . . ?
H1E O1WB H1F 107(2) . . ?
H2C O2WA H2D 106(2) . . ?
H2E O2WB H2F 108(2) . . ?
H3C O3WA H3D 109(2) . . ?
H3E O3WB H3F 113(2) . . ?
H4C O4WA H4D 108(2) . . ?
H4E O4WB H4F 108(2) . . ?
H5C O5WA H5D 99(2) . . ?
H5E O5WB H5F 105(2) . . ?

_refine_diff_density_max         0.423
_refine_diff_density_min         -1.023
_refine_diff_density_rms         0.066


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