#------------------------------------------------------------------------------
#$Date: 2021-07-05 19:58:28 +0300 (Mon, 05 Jul 2021) $
#$Revision: 267097 $
#$URL: file:///home/coder/svn-repositories/cod/cif/1/55/96/1559647.cif $
#------------------------------------------------------------------------------
#
# This file is available in the Crystallography Open Database (COD),
# http://www.crystallography.net/
#
# All data on this site have been placed in the public domain by the
# contributors.
#
data_1559647
loop_
_publ_author_name
'Jornet-Mollá, Verónica'
'Giménez-Saiz, Carlos'
'Cañadillas-Delgado, Laura'
'Yufit, Dmitry S.'
'Howard, Judith A. K.'
'Romero, Francisco M.'
_publ_section_title
;
 Interplay between spin crossover and proton migration along short strong
 hydrogen bonds.
;
_journal_issue                   3
_journal_name_full               'Chemical science'
_journal_page_first              1038
_journal_page_last               1053
_journal_paper_doi               10.1039/d0sc04918b
_journal_volume                  12
_journal_year                    2020
_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
_space_group_crystal_system      triclinic
_space_group_IT_number           2
_space_group_name_Hall           '-P 1'
_space_group_name_H-M_alt        'P -1'
_atom_sites_solution_hydrogens   difmap
_atom_sites_solution_primary     difmap
_atom_sites_solution_secondary   difmap
_audit_creation_method           SHELXL-2018/3
_audit_update_record
;
2020-02-21 deposited with the CCDC.	2020-11-23 downloaded from the CCDC.
;
_cell_angle_alpha                76.876(2)
_cell_angle_beta                 85.729(2)
_cell_angle_gamma                110.376(2)
_cell_formula_units_Z            2
_cell_length_a                   9.9677(4)
_cell_length_b                   13.5502(5)
_cell_length_c                   17.0822(5)
_cell_measurement_reflns_used    3410
_cell_measurement_temperature    95(1)
_cell_measurement_theta_max      60.021
_cell_measurement_theta_min      5.329
_cell_volume                     2076.34(13)
_computing_cell_refinement       'PFIND and DIRAX programs'
_computing_data_collection       'The NOMAD software from ILL '
_computing_data_reduction        'RETREAT and RAFD19 programs'
_computing_structure_refinement  'SHELXL-2018/3 (Sheldrick, 2018)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1997)'
_diffrn_ambient_temperature      95(1)
_diffrn_detector_area_resol_mean '1.56 mm vert. 2.5 mm hor.'
_diffrn_measured_fraction_theta_full 0.853
_diffrn_measured_fraction_theta_max 0.853
_diffrn_measurement_device_type
'D19 position-sensitive detector diffractometer'
_diffrn_measurement_method       'omega step-scans'
_diffrn_radiation_monochromator  'copper 220'
_diffrn_radiation_type           neutrons
_diffrn_radiation_wavelength     1.45510
_diffrn_reflns_av_R_equivalents  0.0417
_diffrn_reflns_av_unetI/netI     0.0319
_diffrn_reflns_Laue_measured_fraction_full 0.853
_diffrn_reflns_Laue_measured_fraction_max 0.853
_diffrn_reflns_limit_h_max       2
_diffrn_reflns_limit_h_min       -10
_diffrn_reflns_limit_k_max       16
_diffrn_reflns_limit_k_min       -15
_diffrn_reflns_limit_l_max       20
_diffrn_reflns_limit_l_min       -20
_diffrn_reflns_number            12460
_diffrn_reflns_point_group_measured_fraction_full 0.853
_diffrn_reflns_point_group_measured_fraction_max 0.853
_diffrn_reflns_theta_full        60.800
_diffrn_reflns_theta_max         60.800
_diffrn_reflns_theta_min         4.530
_diffrn_source                   'neutron source'
_diffrn_source_power             57MW
_diffrn_source_type              'ILL High Flux Reactor, beam H11'
_exptl_absorpt_coefficient_mu    0.194
_exptl_absorpt_correction_type   numerical
_exptl_absorpt_process_details
; 
Absorption corretion done through d19face, d19abs and d19abscan 
programs from ILL
;
_exptl_crystal_colour            dark-red
_exptl_crystal_density_diffrn    1.573
_exptl_crystal_description       cube
_exptl_crystal_F_000             650
_exptl_crystal_preparation       'Magnetic properties'
_exptl_crystal_recrystallization_method
'Re-crystallisation from solvent: MeOH/H2O'
_exptl_crystal_size_max          1.85
_exptl_crystal_size_mid          1.50
_exptl_crystal_size_min          0.7
_refine_diff_density_max         0.927
_refine_diff_density_min         -1.004
_refine_diff_density_rms         0.202
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.133
_refine_ls_hydrogen_treatment    refall
_refine_ls_matrix_type           full
_refine_ls_number_parameters     982
_refine_ls_number_reflns         6404
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.133
_refine_ls_R_factor_all          0.0571
_refine_ls_R_factor_gt           0.0523
_refine_ls_shift/su_max          0.000
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[σ²(Fo²)+(0.0860P)²+13.1541P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1358
_refine_ls_wR_factor_ref         0.1400
_reflns_Friedel_coverage         0.000
_reflns_number_gt                5881
_reflns_number_total             6404
_reflns_threshold_expression     'I > 2σ(I)'
_cod_data_source_file            d0sc04918b2.cif
_cod_data_source_block           Fe_bpp_Noxid_NHoxid_Neutrons_95K
_cod_depositor_comments
;Adding full bibliography for 1559642--1559653.cif.

 Adding full bibliography for 1559642--1559653.cif.
;
_cod_database_code               1559647
_shelx_shelxl_version_number     2018/3
_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'
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 . . . . .
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'
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_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_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
