#------------------------------------------------------------------------------
#$Date: 2019-11-26 13:25:29 +0200 (Tue, 26 Nov 2019) $
#$Revision: 243422 $
#$URL: file:///home/coder/svn-repositories/cod/cif/4/13/37/4133704.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_4133704
loop_
_publ_author_name
'Keilwerth, Martin'
'Hohenberger, Johannes'
'Heinemann, Frank W.'
'Sutter, Jörg'
'Scheurer, Andreas'
'Fang, Huayi'
'Bill, Eckhard'
'Neese, Frank'
'Ye, Shengfa'
'Meyer, Karsten'
_publ_section_title
;
 A Series of Iron Nitrosyl Complexes {Fe-NO}⁶⁻⁹ and a Fleeting
 {Fe-NO}¹⁰ Intermediate en Route to a Metalacyclic Iron
 Nitrosoalkane.
;
_journal_issue                   43
_journal_name_full               'Journal of the American Chemical Society'
_journal_page_first              17217
_journal_page_last               17235
_journal_paper_doi               10.1021/jacs.9b08053
_journal_volume                  141
_journal_year                    2019
_chemical_formula_moiety         '3(C14 H17 Fe0.33 N2.67 O0.33), B F4'
_chemical_formula_sum            'C42 H51 B F4 Fe N8 O'
_chemical_formula_weight         826.56
_space_group_crystal_system      trigonal
_space_group_IT_number           143
_space_group_name_Hall           'P 3'
_space_group_name_H-M_alt        'P 3'
_atom_sites_solution_hydrogens   geom
_audit_creation_date             2019-01-18
_audit_creation_method
;
Olex2 1.2
(compiled 2018.05.29 svn.r3508 for OlexSys, GUI svn.r5506)
;
_cell_angle_alpha                90
_cell_angle_beta                 90
_cell_angle_gamma                120
_cell_formula_units_Z            3
_cell_length_a                   19.1778(12)
_cell_length_b                   19.1778(12)
_cell_length_c                   9.8155(8)
_cell_measurement_reflns_used    9965
_cell_measurement_temperature    100(2)
_cell_measurement_theta_max      25.30
_cell_measurement_theta_min      2.41
_cell_volume                     3126.4(4)
_computing_cell_refinement       'Bruker SAINT'
_computing_data_collection       'Bruker APEX2'
_computing_data_reduction        'Bruker SAINT'
_computing_molecular_graphics    'SHELXTL 6.12 (Bruker AXS, 2002)'
_computing_publication_material  'Olex2 (Dolomanov et al., 2009)'
_computing_structure_refinement  'SHELXL-2016/6 (Sheldrick, 2008)'
_computing_structure_solution    'SHELXTL 6.12 (Bruker AXS, 2002)'
_diffrn_ambient_temperature      100(2)
_diffrn_detector_area_resol_mean 83.33
_diffrn_measured_fraction_theta_full 1.000
_diffrn_measured_fraction_theta_max 1.000
_diffrn_measurement_device_type  'Bruker Kappa APEX II CCD area detector'
_diffrn_measurement_method       'phi and omega scans'
_diffrn_radiation_monochromator  'Quazar focussing montel optics'
_diffrn_radiation_source         'ImuS micro-focus tube'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0826
_diffrn_reflns_av_unetI/netI     0.0521
_diffrn_reflns_Laue_measured_fraction_full 1.000
_diffrn_reflns_Laue_measured_fraction_max 1.000
_diffrn_reflns_limit_h_max       25
_diffrn_reflns_limit_h_min       -25
_diffrn_reflns_limit_k_max       24
_diffrn_reflns_limit_k_min       -25
_diffrn_reflns_limit_l_max       12
_diffrn_reflns_limit_l_min       -12
_diffrn_reflns_number            70125
_diffrn_reflns_point_group_measured_fraction_full 1.000
_diffrn_reflns_point_group_measured_fraction_max 1.000
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         27.887
_diffrn_reflns_theta_min         1.226
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    0.423
_exptl_absorpt_correction_T_max  0.7456
_exptl_absorpt_correction_T_min  0.5448
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
SADABS-2014/4 (Bruker,2014/4) was used for absorption correction.
wR2(int) was 0.1174 before and 0.0819 after correction.
The Ratio of minimum to maximum transmission is 0.7307.
The λ/2 correction factor is 0.00150.
;
_exptl_crystal_colour            violet
_exptl_crystal_density_diffrn    1.317
_exptl_crystal_description       block
_exptl_crystal_F_000             1302
_exptl_crystal_size_max          0.22
_exptl_crystal_size_mid          0.21
_exptl_crystal_size_min          0.12
_refine_diff_density_max         0.272
_refine_diff_density_min         -0.277
_refine_diff_density_rms         0.049
_refine_ls_abs_structure_details
;
 Flack x determined using 4238 quotients [(I+)-(I-)]/[(I+)+(I-)]
 (Parsons, Flack and Wagner, Acta Cryst. B69 (2013) 249-259).
;
_refine_ls_abs_structure_Flack   -0.007(13)
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.021
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     524
_refine_ls_number_reflns         9958
_refine_ls_number_restraints     1
_refine_ls_restrained_S_all      1.020
_refine_ls_R_factor_all          0.0472
_refine_ls_R_factor_gt           0.0424
_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)+(0.0391P)²+1.8219P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0955
_refine_ls_wR_factor_ref         0.0984
_reflns_Friedel_coverage         1.000
_reflns_Friedel_fraction_full    1.000
_reflns_Friedel_fraction_max     1.000
_reflns_number_gt                9384
_reflns_number_total             9958
_reflns_threshold_expression     'I > 2σ(I)'
_cod_data_source_file            ja9b08053_si_002.cif
_cod_data_source_block           jh1505
_cod_original_cell_volume        3126.4(5)
_cod_database_code               4133704
_shelx_shelxl_version_number     2016/6
_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.
;
_shelx_estimated_absorpt_t_max   0.951
_shelx_estimated_absorpt_t_min   0.913
_olex2_refinement_description
;
1. Twinned data refinement
 Scales: 0.4100(14)
 0.5900(14)
2. Fixed Uiso
 At 1.2 times of:
  All C(H) groups, All C(H,H) groups
 At 1.5 times of:
  All C(H,H,H) groups
3.a Secondary CH2 refined with riding coordinates:
 C1(H1A,H1B), C2(H2A,H2B), C15(H15A,H15B), C16(H16A,H16B), C29(H29A,H29B),
 C30(H30A,H30B)
3.b Aromatic/amide H refined with riding coordinates:
 C4(H4), C5(H5), C8(H8), C10(H10), C18(H18), C19(H19), C22(H22), C24(H24),
 C32(H32), C33(H33), C36(H36), C38(H38)
3.c Idealised Me refined as rotating group:
 C12(H12A,H12B,H12C), C13(H13A,H13B,H13C), C14(H14A,H14B,H14C), C26(H26A,H26B,
 H26C), C27(H27A,H27B,H27C), C28(H28A,H28B,H28C), C40(H40A,H40B,H40C), C41(H41A,
 H41B,H41C), C42(H42A,H42B,H42C)
;
_olex2_submission_special_instructions 'No special instructions were received'
loop_
_space_group_symop_operation_xyz
'x, y, z'
'-y, x-y, z'
'-x+y, -x, 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
Fe1 Fe 0.333333 0.666667 0.54070(14) 0.0195(3) Uani 1 3 d S T P
O1 O 0.333333 0.666667 0.8344(8) 0.039(2) Uani 1 3 d S T P
N1 N 0.333333 0.666667 0.1816(11) 0.037(2) Uani 1 3 d S T P
N2 N 0.3438(3) 0.5374(3) 0.3633(5) 0.0296(11) Uani 1 1 d . . .
N3 N 0.4217(3) 0.5718(3) 0.5360(6) 0.0271(10) Uani 1 1 d . . .
N4 N 0.333333 0.666667 0.7123(9) 0.024(2) Uani 1 3 d S T P
C1 C 0.3218(5) 0.5879(5) 0.1438(6) 0.0438(18) Uani 1 1 d . . .
H1A H 0.374494 0.593435 0.119869 0.053 Uiso 1 1 calc R . .
H1B H 0.286701 0.567712 0.062451 0.053 Uiso 1 1 calc R . .
C2 C 0.2842(4) 0.5280(4) 0.2586(6) 0.0344(14) Uani 1 1 d . . .
H2A H 0.241450 0.534951 0.301647 0.041 Uiso 1 1 calc R . .
H2B H 0.258835 0.472738 0.220849 0.041 Uiso 1 1 calc R . .
C3 C 0.3662(3) 0.5864(3) 0.4739(6) 0.0244(11) Uani 1 1 d . . .
C4 C 0.3850(4) 0.4953(5) 0.3573(8) 0.0433(17) Uani 1 1 d . . .
H4 H 0.379889 0.458349 0.288180 0.052 Uiso 1 1 calc R . .
C5 C 0.4331(5) 0.5159(5) 0.4656(8) 0.0472(18) Uani 1 1 d . . .
H5 H 0.468154 0.496235 0.489552 0.057 Uiso 1 1 calc R . .
C6 C 0.4586(3) 0.6009(4) 0.6665(6) 0.0248(11) Uani 1 1 d . . .
C7 C 0.5326(3) 0.6719(4) 0.6742(7) 0.0265(12) Uani 1 1 d . . .
C8 C 0.5701(3) 0.6959(4) 0.8002(6) 0.0285(13) Uani 1 1 d . . .
H8 H 0.619520 0.745289 0.807673 0.034 Uiso 1 1 calc R . .
C9 C 0.5363(3) 0.6486(3) 0.9161(6) 0.0260(12) Uani 1 1 d . . .
C10 C 0.4627(4) 0.5772(4) 0.9048(7) 0.0304(13) Uani 1 1 d . . .
H10 H 0.439622 0.544439 0.983051 0.036 Uiso 1 1 calc R . .
C11 C 0.4226(3) 0.5532(3) 0.7811(7) 0.0277(11) Uani 1 1 d . . .
C12 C 0.5701(4) 0.7236(4) 0.5511(7) 0.0359(14) Uani 1 1 d . . .
H12A H 0.572553 0.690669 0.477042 0.054 Uiso 1 1 calc GR . .
H12B H 0.624612 0.766641 0.573485 0.054 Uiso 1 1 calc GR . .
H12C H 0.537515 0.747349 0.522325 0.054 Uiso 1 1 calc GR . .
C13 C 0.5804(4) 0.6745(4) 1.0505(8) 0.0397(15) Uani 1 1 d . . .
H13A H 0.623207 0.660700 1.052166 0.060 Uiso 1 1 calc GR . .
H13B H 0.542587 0.646748 1.125114 0.060 Uiso 1 1 calc GR . .
H13C H 0.604113 0.732811 1.061314 0.060 Uiso 1 1 calc GR . .
C14 C 0.3408(4) 0.4789(4) 0.7716(8) 0.0373(14) Uani 1 1 d . . .
H14A H 0.300086 0.494612 0.755292 0.056 Uiso 1 1 calc GR . .
H14B H 0.328736 0.448674 0.857120 0.056 Uiso 1 1 calc GR . .
H14C H 0.340298 0.445159 0.696279 0.056 Uiso 1 1 calc GR . .
Fe2 Fe 0.666667 0.333333 0.78008(11) 0.0155(2) Uani 1 3 d S T P
O2 O 0.666667 0.333333 0.4907(8) 0.0258(16) Uani 1 3 d S T P
N5 N 0.666667 0.333333 1.1441(8) 0.0216(17) Uani 1 3 d S T P
N6 N 0.5223(3) 0.3101(3) 0.9610(5) 0.0217(9) Uani 1 1 d . . .
N7 N 0.5439(3) 0.3908(3) 0.7968(5) 0.0221(9) Uani 1 1 d . . .
N8 N 0.666667 0.333333 0.6091(10) 0.0230(17) Uani 1 3 d S T P
C15 C 0.5823(3) 0.3002(4) 1.1795(6) 0.0265(12) Uani 1 1 d . . .
H15A H 0.573217 0.344443 1.209041 0.032 Uiso 1 1 calc R . .
H15B H 0.568794 0.262528 1.256955 0.032 Uiso 1 1 calc R . .
C16 C 0.5270(3) 0.2562(3) 1.0607(6) 0.0243(12) Uani 1 1 d . . .
H16A H 0.546553 0.223227 1.014795 0.029 Uiso 1 1 calc R . .
H16B H 0.472351 0.219178 1.096101 0.029 Uiso 1 1 calc R . .
C17 C 0.5709(3) 0.3432(3) 0.8513(5) 0.0192(10) Uani 1 1 d . . .
C18 C 0.4678(4) 0.3368(4) 0.9754(6) 0.0305(13) Uani 1 1 d . . .
H18 H 0.428812 0.322120 1.045489 0.037 Uiso 1 1 calc R . .
C19 C 0.4805(4) 0.3877(4) 0.8711(7) 0.0321(14) Uani 1 1 d . . .
H19 H 0.452197 0.415519 0.852270 0.039 Uiso 1 1 calc R . .
C20 C 0.5728(3) 0.4369(3) 0.6715(6) 0.0219(11) Uani 1 1 d . . .
C21 C 0.6283(3) 0.5191(3) 0.6799(6) 0.0233(11) Uani 1 1 d . . .
C22 C 0.6541(3) 0.5624(3) 0.5567(6) 0.0261(11) Uani 1 1 d . . .
H22 H 0.693021 0.618174 0.558870 0.031 Uiso 1 1 calc R . .
C23 C 0.6239(4) 0.5254(4) 0.4328(6) 0.0289(13) Uani 1 1 d . . .
C24 C 0.5664(4) 0.4445(4) 0.4306(6) 0.0299(14) Uani 1 1 d . . .
H24 H 0.544120 0.419651 0.345643 0.036 Uiso 1 1 calc R . .
C25 C 0.5399(3) 0.3981(3) 0.5496(7) 0.0252(11) Uani 1 1 d . . .
C26 C 0.6633(4) 0.5617(3) 0.8110(6) 0.0290(13) Uani 1 1 d . . .
H26A H 0.623942 0.535692 0.884340 0.043 Uiso 1 1 calc GR . .
H26B H 0.676993 0.618063 0.802982 0.043 Uiso 1 1 calc GR . .
H26C H 0.712070 0.559302 0.831903 0.043 Uiso 1 1 calc GR . .
C27 C 0.6503(6) 0.5743(4) 0.3022(7) 0.0472(19) Uani 1 1 d . . .
H27A H 0.635064 0.616031 0.305484 0.071 Uiso 1 1 calc GR . .
H27B H 0.623981 0.538789 0.224209 0.071 Uiso 1 1 calc GR . .
H27C H 0.708831 0.599636 0.292577 0.071 Uiso 1 1 calc GR . .
C28 C 0.4784(4) 0.3096(3) 0.5438(8) 0.0345(13) Uani 1 1 d . . .
H28A H 0.505343 0.278049 0.555570 0.052 Uiso 1 1 calc GR . .
H28B H 0.451021 0.296946 0.455392 0.052 Uiso 1 1 calc GR . .
H28C H 0.438823 0.296403 0.616757 0.052 Uiso 1 1 calc GR . .
Fe3 Fe 0.000000 0.000000 0.52274(14) 0.0137(3) Uani 1 3 d S T P
O3 O 0.000000 0.000000 0.8123(9) 0.043(2) Uani 1 3 d S T P
N9 N 0.000000 0.000000 0.1417(8) 0.0159(16) Uani 1 3 d S T P
N10 N 0.0788(2) 0.1500(2) 0.3311(4) 0.0175(8) Uani 1 1 d . . .
N11 N 0.0156(3) 0.1652(2) 0.4977(4) 0.0188(9) Uani 1 1 d . . .
N12 N 0.000000 0.000000 0.6940(8) 0.0186(17) Uani 1 3 d S T P
C29 C 0.0679(3) 0.0800(3) 0.1118(5) 0.0201(10) Uani 1 1 d . . .
H29A H 0.047187 0.114022 0.073865 0.024 Uiso 1 1 calc R . .
H29B H 0.102340 0.075207 0.041689 0.024 Uiso 1 1 calc R . .
C30 C 0.1187(3) 0.1212(3) 0.2371(5) 0.0188(10) Uani 1 1 d . . .
H30A H 0.130159 0.082817 0.285790 0.023 Uiso 1 1 calc R . .
H30B H 0.170768 0.167400 0.207792 0.023 Uiso 1 1 calc R . .
C31 C 0.0384(3) 0.1131(3) 0.4464(5) 0.0172(10) Uani 1 1 d . . .
C32 C 0.0795(3) 0.2220(3) 0.3087(6) 0.0237(11) Uani 1 1 d . . .
H32 H 0.102996 0.257362 0.233502 0.028 Uiso 1 1 calc R . .
C33 C 0.0408(3) 0.2316(3) 0.4128(6) 0.0222(11) Uani 1 1 d . . .
H33 H 0.032029 0.275629 0.426710 0.027 Uiso 1 1 calc R . .
C34 C -0.0164(3) 0.1619(3) 0.6332(5) 0.0200(10) Uani 1 1 d . . .
C35 C 0.0383(3) 0.1943(3) 0.7398(5) 0.0205(11) Uani 1 1 d . . .
C36 C 0.0083(3) 0.1976(3) 0.8678(6) 0.0233(11) Uani 1 1 d . . .
H36 H 0.044687 0.220867 0.941862 0.028 Uiso 1 1 calc R . .
C37 C -0.0735(3) 0.1675(3) 0.8896(6) 0.0226(11) Uani 1 1 d . . .
C38 C -0.1265(3) 0.1333(3) 0.7800(6) 0.0228(10) Uani 1 1 d . . .
H38 H -0.182623 0.110731 0.794971 0.027 Uiso 1 1 calc R . .
C39 C -0.0992(3) 0.1313(3) 0.6500(6) 0.0223(12) Uani 1 1 d . . .
C40 C 0.1268(4) 0.2228(4) 0.7220(6) 0.0271(13) Uani 1 1 d . . .
H40A H 0.134874 0.176215 0.721088 0.041 Uiso 1 1 calc GR . .
H40B H 0.157171 0.258462 0.797648 0.041 Uiso 1 1 calc GR . .
H40C H 0.145651 0.252101 0.635780 0.041 Uiso 1 1 calc GR . .
C41 C -0.1041(4) 0.1731(3) 1.0285(7) 0.0302(12) Uani 1 1 d . . .
H41A H -0.068862 0.171119 1.098871 0.045 Uiso 1 1 calc GR . .
H41B H -0.158924 0.127975 1.041026 0.045 Uiso 1 1 calc GR . .
H41C H -0.104314 0.223982 1.035923 0.045 Uiso 1 1 calc GR . .
C42 C -0.1563(3) 0.0958(3) 0.5315(6) 0.0273(11) Uani 1 1 d . . .
H42A H -0.139997 0.135971 0.458700 0.041 Uiso 1 1 calc GR . .
H42B H -0.211042 0.079990 0.561332 0.041 Uiso 1 1 calc GR . .
H42C H -0.155091 0.048424 0.497413 0.041 Uiso 1 1 calc GR . .
B1 B 0.0437(5) 0.7156(5) 0.0812(9) 0.0391(18) Uani 1 1 d . . .
F1 F 0.0518(3) 0.6479(3) 0.0719(4) 0.0508(11) Uani 1 1 d . . .
F2 F -0.0126(3) 0.6988(3) 0.1846(6) 0.0696(14) Uani 1 1 d . . .
F3 F 0.1148(3) 0.7833(3) 0.0980(8) 0.095(2) Uani 1 1 d . . .
F4 F 0.0085(3) 0.7205(3) -0.0379(6) 0.0785(19) 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 0.0033 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'
B B 0.0013 0.0007 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
F F 0.0171 0.0103 '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'
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
N4 Fe1 N1 180.0 . .
N4 Fe1 C3 108.74(16) . 3_565
N4 Fe1 C3 108.74(16) . 2_665
N4 Fe1 C3 108.74(16) . .
C3 Fe1 N1 71.26(16) . .
C3 Fe1 N1 71.26(16) 3_565 .
C3 Fe1 N1 71.26(16) 2_665 .
C3 Fe1 C3 110.19(16) 3_565 2_665
C3 Fe1 C3 110.19(16) 3_565 .
C3 Fe1 C3 110.19(16) 2_665 .
C1 N1 Fe1 104.7(5) 3_565 .
C1 N1 Fe1 104.7(5) . .
C1 N1 Fe1 104.7(5) 2_665 .
C1 N1 C1 113.8(4) 3_565 2_665
C1 N1 C1 113.8(4) 2_665 .
C1 N1 C1 113.8(4) 3_565 .
C3 N2 C2 126.8(5) . .
C3 N2 C4 111.2(5) . .
C4 N2 C2 122.0(5) . .
C3 N3 C5 112.1(5) . .
C3 N3 C6 126.9(4) . .
C5 N3 C6 120.6(5) . .
O1 N4 Fe1 180.0 . .
N1 C1 H1A 109.3 . .
N1 C1 H1B 109.3 . .
N1 C1 C2 111.5(6) . .
H1A C1 H1B 108.0 . .
C2 C1 H1A 109.3 . .
C2 C1 H1B 109.3 . .
N2 C2 C1 112.3(6) . .
N2 C2 H2A 109.1 . .
N2 C2 H2B 109.1 . .
C1 C2 H2A 109.1 . .
C1 C2 H2B 109.1 . .
H2A C2 H2B 107.9 . .
N2 C3 Fe1 132.0(4) . .
N2 C3 N3 102.9(5) . .
N3 C3 Fe1 125.1(4) . .
N2 C4 H4 126.1 . .
C5 C4 N2 107.8(6) . .
C5 C4 H4 126.1 . .
N3 C5 H5 127.0 . .
C4 C5 N3 105.9(6) . .
C4 C5 H5 127.0 . .
C7 C6 N3 119.4(6) . .
C7 C6 C11 121.7(6) . .
C11 C6 N3 118.6(5) . .
C6 C7 C12 121.4(6) . .
C8 C7 C6 118.5(6) . .
C8 C7 C12 120.1(5) . .
C7 C8 H8 119.5 . .
C7 C8 C9 121.0(5) . .
C9 C8 H8 119.5 . .
C8 C9 C10 119.1(6) . .
C8 C9 C13 119.8(5) . .
C10 C9 C13 121.2(6) . .
C9 C10 H10 119.5 . .
C11 C10 C9 121.1(6) . .
C11 C10 H10 119.5 . .
C6 C11 C14 120.7(6) . .
C10 C11 C6 118.6(5) . .
C10 C11 C14 120.7(6) . .
C7 C12 H12A 109.5 . .
C7 C12 H12B 109.5 . .
C7 C12 H12C 109.5 . .
H12A C12 H12B 109.5 . .
H12A C12 H12C 109.5 . .
H12B C12 H12C 109.5 . .
C9 C13 H13A 109.5 . .
C9 C13 H13B 109.5 . .
C9 C13 H13C 109.5 . .
H13A C13 H13B 109.5 . .
H13A C13 H13C 109.5 . .
H13B C13 H13C 109.5 . .
C11 C14 H14A 109.5 . .
C11 C14 H14B 109.5 . .
C11 C14 H14C 109.5 . .
H14A C14 H14B 109.5 . .
H14A C14 H14C 109.5 . .
H14B C14 H14C 109.5 . .
N8 Fe2 N5 180.0 . .
N8 Fe2 C17 109.83(15) . .
N8 Fe2 C17 109.83(15) . 3_665
N8 Fe2 C17 109.83(15) . 2_655
C17 Fe2 N5 70.17(15) 3_665 .
C17 Fe2 N5 70.17(15) . .
C17 Fe2 N5 70.17(15) 2_655 .
C17 Fe2 C17 109.11(15) 3_665 .
C17 Fe2 C17 109.10(15) 2_655 3_665
C17 Fe2 C17 109.11(15) 2_655 .
C15 N5 Fe2 103.8(4) 2_655 .
C15 N5 Fe2 103.8(4) 3_665 .
C15 N5 Fe2 103.8(4) . .
C15 N5 C15 114.5(3) 3_665 .
C15 N5 C15 114.5(3) 2_655 3_665
C15 N5 C15 114.5(3) 2_655 .
C17 N6 C16 126.3(4) . .
C17 N6 C18 112.2(5) . .
C18 N6 C16 121.4(5) . .
C17 N7 C19 112.5(5) . .
C17 N7 C20 125.6(4) . .
C19 N7 C20 121.9(4) . .
O2 N8 Fe2 180.0 . .
N5 C15 H15A 109.2 . .
N5 C15 H15B 109.2 . .
N5 C15 C16 112.0(5) . .
H15A C15 H15B 107.9 . .
C16 C15 H15A 109.2 . .
C16 C15 H15B 109.2 . .
N6 C16 C15 113.3(5) . .
N6 C16 H16A 108.9 . .
N6 C16 H16B 108.9 . .
C15 C16 H16A 108.9 . .
C15 C16 H16B 108.9 . .
H16A C16 H16B 107.7 . .
N6 C17 Fe2 131.5(4) . .
N6 C17 N7 102.8(4) . .
N7 C17 Fe2 125.6(4) . .
N6 C18 H18 126.4 . .
C19 C18 N6 107.1(5) . .
C19 C18 H18 126.4 . .
N7 C19 H19 127.3 . .
C18 C19 N7 105.4(5) . .
C18 C19 H19 127.3 . .
C21 C20 N7 118.8(5) . .
C25 C20 N7 118.2(5) . .
C25 C20 C21 122.9(5) . .
C20 C21 C22 117.4(5) . .
C20 C21 C26 123.3(5) . .
C22 C21 C26 119.2(5) . .
C21 C22 H22 119.4 . .
C23 C22 C21 121.2(5) . .
C23 C22 H22 119.4 . .
C22 C23 C24 119.0(5) . .
C22 C23 C27 120.0(6) . .
C24 C23 C27 120.8(6) . .
C23 C24 H24 118.9 . .
C23 C24 C25 122.2(6) . .
C25 C24 H24 118.9 . .
C20 C25 C24 117.1(5) . .
C20 C25 C28 121.8(6) . .
C24 C25 C28 121.0(6) . .
C21 C26 H26A 109.5 . .
C21 C26 H26B 109.5 . .
C21 C26 H26C 109.5 . .
H26A C26 H26B 109.5 . .
H26A C26 H26C 109.5 . .
H26B C26 H26C 109.5 . .
C23 C27 H27A 109.5 . .
C23 C27 H27B 109.5 . .
C23 C27 H27C 109.5 . .
H27A C27 H27B 109.5 . .
H27A C27 H27C 109.5 . .
H27B C27 H27C 109.5 . .
C25 C28 H28A 109.5 . .
C25 C28 H28B 109.5 . .
C25 C28 H28C 109.5 . .
H28A C28 H28B 109.5 . .
H28A C28 H28C 109.5 . .
H28B C28 H28C 109.5 . .
N12 Fe3 N9 180.0 . .
N12 Fe3 C31 111.41(14) . .
N12 Fe3 C31 111.41(14) . 2
N12 Fe3 C31 111.41(14) . 3
C31 Fe3 N9 68.59(14) . .
C31 Fe3 N9 68.59(14) 3 .
C31 Fe3 N9 68.59(14) 2 .
C31 Fe3 C31 107.46(15) . 3
C31 Fe3 C31 107.46(15) . 2
C31 Fe3 C31 107.46(15) 2 3
C29 N9 Fe3 101.6(4) . .
C29 N9 Fe3 101.6(4) 2 .
C29 N9 Fe3 101.6(4) 3 .
C29 N9 C29 116.1(2) 2 3
C29 N9 C29 116.1(2) 3 .
C29 N9 C29 116.1(2) 2 .
C31 N10 C30 126.6(4) . .
C31 N10 C32 111.7(4) . .
C32 N10 C30 121.7(4) . .
C31 N11 C33 110.8(4) . .
C31 N11 C34 125.9(4) . .
C33 N11 C34 122.3(4) . .
O3 N12 Fe3 180.0 . .
N9 C29 H29A 109.1 . .
N9 C29 H29B 109.1 . .
N9 C29 C30 112.7(5) . .
H29A C29 H29B 107.8 . .
C30 C29 H29A 109.1 . .
C30 C29 H29B 109.1 . .
N10 C30 C29 112.5(4) . .
N10 C30 H30A 109.1 . .
N10 C30 H30B 109.1 . .
C29 C30 H30A 109.1 . .
C29 C30 H30B 109.1 . .
H30A C30 H30B 107.8 . .
N10 C31 Fe3 131.8(4) . .
N10 C31 N11 103.5(4) . .
N11 C31 Fe3 124.0(4) . .
N10 C32 H32 126.7 . .
C33 C32 N10 106.7(5) . .
C33 C32 H32 126.7 . .
N11 C33 H33 126.4 . .
C32 C33 N11 107.3(5) . .
C32 C33 H33 126.4 . .
C35 C34 N11 117.5(5) . .
C35 C34 C39 122.9(5) . .
C39 C34 N11 119.5(5) . .
C34 C35 C36 117.6(5) . .
C34 C35 C40 122.3(5) . .
C36 C35 C40 120.1(5) . .
C35 C36 H36 119.2 . .
C37 C36 C35 121.6(5) . .
C37 C36 H36 119.2 . .
C36 C37 C38 118.7(5) . .
C36 C37 C41 120.5(5) . .
C38 C37 C41 120.8(5) . .
C37 C38 H38 119.1 . .
C39 C38 C37 121.7(5) . .
C39 C38 H38 119.1 . .
C34 C39 C42 121.0(5) . .
C38 C39 C34 117.4(5) . .
C38 C39 C42 121.6(5) . .
C35 C40 H40A 109.5 . .
C35 C40 H40B 109.5 . .
C35 C40 H40C 109.5 . .
H40A C40 H40B 109.5 . .
H40A C40 H40C 109.5 . .
H40B C40 H40C 109.5 . .
C37 C41 H41A 109.5 . .
C37 C41 H41B 109.5 . .
C37 C41 H41C 109.5 . .
H41A C41 H41B 109.5 . .
H41A C41 H41C 109.5 . .
H41B C41 H41C 109.5 . .
C39 C42 H42A 109.5 . .
C39 C42 H42B 109.5 . .
C39 C42 H42C 109.5 . .
H42A C42 H42B 109.5 . .
H42A C42 H42C 109.5 . .
H42B C42 H42C 109.5 . .
F1 B1 F2 105.5(6) . .
F3 B1 F1 112.2(6) . .
F3 B1 F2 115.4(7) . .
F3 B1 F4 109.5(7) . .
F4 B1 F1 107.2(6) . .
F4 B1 F2 106.5(6) . .
loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
Fe1 N1 3.525(11) .
Fe1 N4 1.684(9) .
Fe1 C3 2.041(6) 2_665
Fe1 C3 2.041(6) 3_565
Fe1 C3 2.041(6) .
O1 N4 1.199(11) .
N1 C1 1.461(8) .
N1 C1 1.461(8) 3_565
N1 C1 1.461(8) 2_665
N2 C2 1.479(8) .
N2 C3 1.357(7) .
N2 C4 1.385(8) .
N3 C3 1.372(7) .
N3 C5 1.381(8) .
N3 C6 1.435(8) .
C1 H1A 0.9900 .
C1 H1B 0.9900 .
C1 C2 1.511(10) .
C2 H2A 0.9900 .
C2 H2B 0.9900 .
C4 H4 0.9500 .
C4 C5 1.332(10) .
C5 H5 0.9500 .
C6 C7 1.393(8) .
C6 C11 1.395(9) .
C7 C8 1.389(9) .
C7 C12 1.499(9) .
C8 H8 0.9500 .
C8 C9 1.396(9) .
C9 C10 1.396(9) .
C9 C13 1.511(9) .
C10 H10 0.9500 .
C10 C11 1.386(9) .
C11 C14 1.505(8) .
C12 H12A 0.9800 .
C12 H12B 0.9800 .
C12 H12C 0.9800 .
C13 H13A 0.9800 .
C13 H13B 0.9800 .
C13 H13C 0.9800 .
C14 H14A 0.9800 .
C14 H14B 0.9800 .
C14 H14C 0.9800 .
Fe2 N5 3.573(8) .
Fe2 N8 1.678(10) .
Fe2 C17 2.060(5) 3_665
Fe2 C17 2.060(5) 2_655
Fe2 C17 2.060(5) .
O2 N8 1.162(11) .
N5 C15 1.455(6) .
N5 C15 1.455(6) 2_655
N5 C15 1.455(6) 3_665
N6 C16 1.460(7) .
N6 C17 1.356(7) .
N6 C18 1.381(7) .
N7 C17 1.364(7) .
N7 C19 1.393(7) .
N7 C20 1.453(7) .
C15 H15A 0.9900 .
C15 H15B 0.9900 .
C15 C16 1.516(8) .
C16 H16A 0.9900 .
C16 H16B 0.9900 .
C18 H18 0.9500 .
C18 C19 1.350(9) .
C19 H19 0.9500 .
C20 C21 1.394(8) .
C20 C25 1.384(8) .
C21 C22 1.410(8) .
C21 C26 1.492(8) .
C22 H22 0.9500 .
C22 C23 1.381(9) .
C23 C24 1.382(9) .
C23 C27 1.519(9) .
C24 H24 0.9500 .
C24 C25 1.400(9) .
C25 C28 1.508(8) .
C26 H26A 0.9800 .
C26 H26B 0.9800 .
C26 H26C 0.9800 .
C27 H27A 0.9800 .
C27 H27B 0.9800 .
C27 H27C 0.9800 .
C28 H28A 0.9800 .
C28 H28B 0.9800 .
C28 H28C 0.9800 .
Fe3 N9 3.740(8) .
Fe3 N12 1.681(8) .
Fe3 C31 2.052(5) 3
Fe3 C31 2.052(5) 2
Fe3 C31 2.052(5) .
O3 N12 1.161(12) .
N9 C29 1.463(5) 2
N9 C29 1.463(5) .
N9 C29 1.463(5) 3
N10 C30 1.472(6) .
N10 C31 1.354(6) .
N10 C32 1.391(6) .
N11 C31 1.371(6) .
N11 C33 1.390(7) .
N11 C34 1.453(7) .
C29 H29A 0.9900 .
C29 H29B 0.9900 .
C29 C30 1.521(7) .
C30 H30A 0.9900 .
C30 H30B 0.9900 .
C32 H32 0.9500 .
C32 C33 1.329(8) .
C33 H33 0.9500 .
C34 C35 1.389(8) .
C34 C39 1.400(8) .
C35 C36 1.396(8) .
C35 C40 1.511(8) .
C36 H36 0.9500 .
C36 C37 1.391(8) .
C37 C38 1.398(8) .
C37 C41 1.509(8) .
C38 H38 0.9500 .
C38 C39 1.387(8) .
C39 C42 1.507(8) .
C40 H40A 0.9800 .
C40 H40B 0.9800 .
C40 H40C 0.9800 .
C41 H41A 0.9800 .
C41 H41B 0.9800 .
C41 H41C 0.9800 .
C42 H42A 0.9800 .
C42 H42B 0.9800 .
C42 H42C 0.9800 .
B1 F1 1.386(8) .
B1 F2 1.396(10) .
B1 F3 1.342(9) .
B1 F4 1.376(9) .
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
Fe1 N1 C1 C2 21.3(7) .
N1 C1 C2 N2 -79.9(7) .
N2 C4 C5 N3 -1.0(9) .
N3 C6 C7 C8 -175.3(5) .
N3 C6 C7 C12 7.0(8) .
N3 C6 C11 C10 173.2(5) .
N3 C6 C11 C14 -8.8(8) .
C1 N1 C1 C2 135.1(8) 2_665
C1 N1 C1 C2 -92.4(11) 3_565
C2 N2 C3 Fe1 -1.9(9) .
C2 N2 C3 N3 179.8(6) .
C2 N2 C4 C5 -179.4(6) .
C3 N2 C2 C1 88.2(7) .
C3 N2 C4 C5 1.2(9) .
C3 N3 C5 C4 0.5(8) .
C3 N3 C6 C7 -93.6(7) .
C3 N3 C6 C11 92.0(7) .
C4 N2 C2 C1 -91.2(8) .
C4 N2 C3 Fe1 177.6(5) .
C4 N2 C3 N3 -0.8(7) .
C5 N3 C3 Fe1 -178.4(5) .
C5 N3 C3 N2 0.2(7) .
C5 N3 C6 C7 94.3(7) .
C5 N3 C6 C11 -80.1(7) .
C6 N3 C3 Fe1 9.0(8) .
C6 N3 C3 N2 -172.4(5) .
C6 N3 C5 C4 173.7(6) .
C6 C7 C8 C9 2.4(8) .
C7 C6 C11 C10 -1.0(8) .
C7 C6 C11 C14 176.9(6) .
C7 C8 C9 C10 -1.6(8) .
C7 C8 C9 C13 177.2(6) .
C8 C9 C10 C11 -0.7(9) .
C9 C10 C11 C6 1.9(8) .
C9 C10 C11 C14 -176.0(6) .
C11 C6 C7 C8 -1.1(8) .
C11 C6 C7 C12 -178.8(5) .
C12 C7 C8 C9 -179.9(5) .
C13 C9 C10 C11 -179.4(6) .
Fe2 N5 C15 C16 17.6(5) .
N5 C15 C16 N6 -78.7(6) .
N6 C18 C19 N7 -0.7(7) .
N7 C20 C21 C22 -178.9(5) .
N7 C20 C21 C26 3.5(8) .
N7 C20 C25 C24 177.5(5) .
N7 C20 C25 C28 -2.6(7) .
C15 N5 C15 C16 -94.9(8) 2_655
C15 N5 C15 C16 130.1(7) 3_665
C16 N6 C17 Fe2 0.1(8) .
C16 N6 C17 N7 -177.1(5) .
C16 N6 C18 C19 177.5(5) .
C17 N6 C16 C15 89.2(6) .
C17 N6 C18 C19 1.0(7) .
C17 N7 C19 C18 0.3(7) .
C17 N7 C20 C21 -99.9(6) .
C17 N7 C20 C25 84.2(7) .
C18 N6 C16 C15 -86.8(6) .
C18 N6 C17 Fe2 176.4(4) .
C18 N6 C17 N7 -0.8(6) .
C19 N7 C17 Fe2 -177.1(4) .
C19 N7 C17 N6 0.3(6) .
C19 N7 C20 C21 83.8(7) .
C19 N7 C20 C25 -92.0(7) .
C20 N7 C17 Fe2 6.3(7) .
C20 N7 C17 N6 -176.2(5) .
C20 N7 C19 C18 176.9(5) .
C20 C21 C22 C23 1.8(8) .
C21 C20 C25 C24 1.8(8) .
C21 C20 C25 C28 -178.3(5) .
C21 C22 C23 C24 0.9(8) .
C21 C22 C23 C27 177.6(6) .
C22 C23 C24 C25 -2.5(9) .
C23 C24 C25 C20 1.1(8) .
C23 C24 C25 C28 -178.7(5) .
C25 C20 C21 C22 -3.2(8) .
C25 C20 C21 C26 179.2(5) .
C26 C21 C22 C23 179.5(5) .
C27 C23 C24 C25 -179.0(6) .
Fe3 N9 C29 C30 11.6(4) .
N9 C29 C30 N10 -73.9(5) .
N10 C32 C33 N11 -0.8(6) .
N11 C34 C35 C36 174.5(4) .
N11 C34 C35 C40 -7.6(7) .
N11 C34 C39 C38 -176.7(4) .
N11 C34 C39 C42 4.9(7) .
C29 N9 C29 C30 120.8(6) 2
C29 N9 C29 C30 -97.5(7) 3
C30 N10 C31 Fe3 -11.1(7) .
C30 N10 C31 N11 178.1(4) .
C30 N10 C32 C33 -178.2(5) .
C31 N10 C30 C29 99.7(6) .
C31 N10 C32 C33 1.5(6) .
C31 N11 C33 C32 -0.2(6) .
C31 N11 C34 C35 81.0(6) .
C31 N11 C34 C39 -102.9(6) .
C32 N10 C30 C29 -80.6(6) .
C32 N10 C31 Fe3 169.2(4) .
C32 N10 C31 N11 -1.6(6) .
C33 N11 C31 Fe3 -170.6(4) .
C33 N11 C31 N10 1.1(5) .
C33 N11 C34 C35 -86.6(6) .
C33 N11 C34 C39 89.5(6) .
C34 N11 C31 Fe3 20.6(7) .
C34 N11 C31 N10 -167.8(5) .
C34 N11 C33 C32 169.1(5) .
C34 C35 C36 C37 1.8(8) .
C35 C34 C39 C38 -0.8(8) .
C35 C34 C39 C42 -179.3(5) .
C35 C36 C37 C38 0.1(8) .
C35 C36 C37 C41 -178.9(5) .
C36 C37 C38 C39 -2.4(8) .
C37 C38 C39 C34 2.8(8) .
C37 C38 C39 C42 -178.8(5) .
C39 C34 C35 C36 -1.4(8) .
C39 C34 C35 C40 176.4(5) .
C40 C35 C36 C37 -176.1(5) .
C41 C37 C38 C39 176.5(5) .
loop_
_twin_individual_id
_twin_individual_mass_fraction_refined
1 0.4100(14)
2 0.5900(14)
