#------------------------------------------------------------------------------
#$Date: 2023-10-03 01:53:09 +0300 (Tue, 03 Oct 2023) $
#$Revision: 286630 $
#$URL: file:///home/coder/svn-repositories/cod/cif/7/71/40/7714086.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_7714086
loop_
_publ_author_name
'Kulmaczewski, Rafal'
'Halcrow, Malcolm'
_publ_section_title
;
 Iron(II) Complexes of 2,6-Bis(imidazo[1,2‑a]pyridin-2-yl)pyridine
 and Related Ligands with Annelated Distal Heterocyclic Donors
;
_journal_name_full               'Dalton Transactions'
_journal_paper_doi               10.1039/D3DT02747C
_journal_year                    2023
_chemical_formula_moiety         'C38 H26 Fe N10, 2(B F4), 1.5(C H4 O)'
_chemical_formula_sum            'C39.5 H32 B2 F8 Fe N10 O1.5'
_chemical_formula_weight         900.22
_chemical_name_systematic
'Bis[2,6-Bis(imidazo[1,2-a]pyridin-2-yl)pyridine]iron(II)ditetrafluoroborate methanol (1.5/1.41) solvate'
_space_group_crystal_system      orthorhombic
_space_group_IT_number           33
_space_group_name_Hall           'P 2c -2n'
_space_group_name_H-M_alt        'P n a 21'
_atom_sites_solution_hydrogens   geom
_audit_creation_date             2022-08-11
_audit_creation_method
;
Olex2 1.5
(compiled 2021.07.19 svn.r715e62df for OlexSys, GUI svn.r6383)
;
_audit_update_record
;
2023-08-15 deposited with the CCDC.	2023-10-02 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 90
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   25.2181(6)
_cell_length_b                   12.4550(2)
_cell_length_c                   12.9419(3)
_cell_measurement_reflns_used    5458
_cell_measurement_temperature    120(2)
_cell_measurement_theta_max      73.62
_cell_measurement_theta_min      4.90
_cell_volume                     4064.94(15)
_computing_cell_refinement       'CrysAlisPro, Agilent Technologies'
_computing_data_collection       'CrysAlisPro, Agilent Technologies'
_computing_data_reduction        'CrysAlisPro, Agilent Technologies'
_computing_molecular_graphics    'Olex2 1.5 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 1.5 (Dolomanov et al., 2009)'
_computing_structure_refinement  'SHELXL 2018/3 (Sheldrick, 2015)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_diffrn_ambient_temperature      120.15
_diffrn_detector_area_resol_mean 5.3095
_diffrn_measured_fraction_theta_full 0.988
_diffrn_measured_fraction_theta_max 0.975
_diffrn_measurement_device_type  'SuperNova, Dual, Cu at zero, Atlas'
_diffrn_measurement_method       'ω scans'
_diffrn_radiation_type           CuK\a
_diffrn_radiation_wavelength     1.54184
_diffrn_reflns_av_R_equivalents  0.0282
_diffrn_reflns_av_unetI/netI     0.0373
_diffrn_reflns_Laue_measured_fraction_full 0.988
_diffrn_reflns_Laue_measured_fraction_max 0.975
_diffrn_reflns_limit_h_max       29
_diffrn_reflns_limit_h_min       -31
_diffrn_reflns_limit_k_max       14
_diffrn_reflns_limit_k_min       -15
_diffrn_reflns_limit_l_max       15
_diffrn_reflns_limit_l_min       -13
_diffrn_reflns_number            10785
_diffrn_reflns_point_group_measured_fraction_full 0.751
_diffrn_reflns_point_group_measured_fraction_max 0.737
_diffrn_reflns_theta_full        72.000
_diffrn_reflns_theta_max         73.650
_diffrn_reflns_theta_min         3.505
_diffrn_source                   'sealed X-ray tube'
_diffrn_source_type              'SuperNova (Cu) X-ray Source'
_exptl_absorpt_coefficient_mu    3.722
_exptl_absorpt_correction_T_max  1.000
_exptl_absorpt_correction_T_min  0.750
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
CrysAlisPro, Agilent Technologies,
Version 1.171.36.24 (release 03-12-2012 CrysAlis171 .NET)
Empirical absorption correction using spherical harmonics,
 implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_crystal_colour            red
_exptl_crystal_density_diffrn    1.471
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       needle
_exptl_crystal_F_000             1836
_exptl_crystal_preparation       'Magnetic properties'
_exptl_crystal_recrystallization_method
'Re-crystallisation from solvent: methanol/diethyl ether'
_exptl_crystal_size_max          0.35
_exptl_crystal_size_mid          0.10
_exptl_crystal_size_min          0.10
_refine_diff_density_max         1.106
_refine_diff_density_min         -0.454
_refine_diff_density_rms         0.081
_refine_ls_abs_structure_details
;
 Refined as an inversion twin.
;
_refine_ls_abs_structure_Flack   0.498(7)
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.061
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     574
_refine_ls_number_reflns         6058
_refine_ls_number_restraints     5
_refine_ls_restrained_S_all      1.062
_refine_ls_R_factor_all          0.0526
_refine_ls_R_factor_gt           0.0499
_refine_ls_shift/su_max          0.012
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[σ²(Fo²)+(0.0995P)²+1.8975P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1419
_refine_ls_wR_factor_ref         0.1451
_reflns_Friedel_coverage         0.445
_reflns_Friedel_fraction_full    0.490
_reflns_Friedel_fraction_max     0.476
_reflns_number_gt                5723
_reflns_number_total             6058
_reflns_threshold_expression     'I > 2σ(I)'
_cod_data_source_file            d3dt02747c2.cif
_cod_data_source_block           146ameoh
_cod_original_formula_sum        'C39.50 H32 B2 F8 Fe N10 O1.50'
_cod_database_code               7714086
_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.
;
_olex2_refinement_description
;
1. Twinned data refinement
 Scales: 0.502(7)
 0.498(7)
2. Fixed Uiso
 At 1.2 times of:
  All C(H) groups, All O(H) groups
 At 1.5 times of:
  All C(H,H,H) groups
3. Restrained distances
 C60A-O61A = C60B-O61B = C62A-O63A = C62B-O63B
 1.42206 with sigma of 0.01
4. Others
 Fixed Sof: C60A(0.5) H60A(0.5) H60B(0.5) H60C(0.5) O61A(0.5) H61A(0.5)
 C62A(0.35) H62A(0.35) H62B(0.35) H62C(0.35) O63A(0.35) H63A(0.35) C60B(0.35)
 H60D(0.35) H60E(0.35) H60F(0.35) O61B(0.35) H61B(0.35) C62B(0.3) H62D(0.3)
 H62E(0.3) H62F(0.3) O63B(0.3) H63B(0.3)
5.a Aromatic/amide H refined with riding coordinates:
 C4(H4), C5(H5), C6(H6), C11(H11), C12(H12), C13(H13), C14(H14), C16(H16),
 C20(H20), C21(H21), C22(H22), C23(H23), C25(H25), C28(H28), C29(H29), C30(H30),
  C35(H35), C36(H36), C37(H37), C38(H38), C40(H40), C44(H44), C45(H45),
 C46(H46), C47(H47), C49(H49)
5.b Idealised Me refined as rotating group:
 C60A(H60A,H60B,H60C), C62A(H62A,H62B,H62C), C60B(H60D,H60E,H60F), C62B(H62D,
 H62E,H62F)
5.c Idealised tetrahedral OH refined as rotating group:
 O61A(H61A), O63A(H63A), O61B(H61B), O63B(H63B)
;
_olex2_submission_special_instructions 'No special instructions were received'
loop_
_space_group_symop_operation_xyz
'x, y, z'
'-x, -y, z+1/2'
'-x+1/2, y+1/2, z+1/2'
'x+1/2, -y+1/2, 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 0.83537(2) 0.73852(5) 0.83743(8) 0.02100(18) Uani 1 1 d . . . . .
N2 N 0.83042(15) 0.6236(3) 0.9631(3) 0.0229(8) Uani 1 1 d . . . . .
C3 C 0.86106(19) 0.5354(4) 0.9633(4) 0.0240(10) Uani 1 1 d . . . . .
C4 C 0.8579(2) 0.4599(4) 1.0424(4) 0.0308(11) Uani 1 1 d . . . . .
H4 H 0.879080 0.396906 1.040830 0.037 Uiso 1 1 calc R U . . .
C5 C 0.8233(2) 0.4784(5) 1.1234(5) 0.0352(12) Uani 1 1 d . . . . .
H5 H 0.821255 0.428502 1.178757 0.042 Uiso 1 1 calc R U . . .
C6 C 0.7917(2) 0.5692(4) 1.1242(4) 0.0322(11) Uani 1 1 d . . . . .
H6 H 0.768043 0.583045 1.179750 0.039 Uiso 1 1 calc R U . . .
C7 C 0.7956(2) 0.6397(4) 1.0409(4) 0.0263(9) Uani 1 1 d . . . . .
C8 C 0.89726(19) 0.5312(4) 0.8747(4) 0.0245(10) Uani 1 1 d . . . . .
N9 N 0.89607(15) 0.6167(3) 0.8062(3) 0.0239(8) Uani 1 1 d . . . . .
C10 C 0.93191(18) 0.5938(4) 0.7340(4) 0.0262(10) Uani 1 1 d . . . . .
C11 C 0.9475(2) 0.6495(5) 0.6454(5) 0.0346(12) Uani 1 1 d . . . . .
H11 H 0.931529 0.716323 0.628522 0.042 Uiso 1 1 calc R U . . .
C12 C 0.9855(2) 0.6074(5) 0.5837(5) 0.0449(15) Uani 1 1 d . . . . .
H12 H 0.996665 0.645329 0.523768 0.054 Uiso 1 1 calc R U . . .
C13 C 1.0089(3) 0.5064(6) 0.6084(6) 0.0498(17) Uani 1 1 d . . . . .
H13 H 1.035540 0.477721 0.564487 0.060 Uiso 1 1 calc R U . . .
C14 C 0.9939(2) 0.4514(5) 0.6922(5) 0.0437(15) Uani 1 1 d . . . . .
H14 H 1.009797 0.384274 0.708342 0.052 Uiso 1 1 calc R U . . .
N15 N 0.95499(17) 0.4943(4) 0.7546(4) 0.0309(10) Uani 1 1 d . . . . .
C16 C 0.93281(18) 0.4555(4) 0.8459(5) 0.0283(10) Uani 1 1 d . . . . .
H16 H 0.940885 0.390230 0.880339 0.034 Uiso 1 1 calc R U . . .
C17 C 0.7638(2) 0.7352(4) 1.0272(4) 0.0265(11) Uani 1 1 d . . . . .
N18 N 0.77327(16) 0.7992(3) 0.9414(3) 0.0254(8) Uani 1 1 d . . . . .
C19 C 0.73890(19) 0.8807(4) 0.9499(4) 0.0279(10) Uani 1 1 d . . . . .
C20 C 0.7302(2) 0.9710(4) 0.8857(5) 0.0339(12) Uani 1 1 d . . . . .
H20 H 0.750941 0.981628 0.825332 0.041 Uiso 1 1 calc R U . . .
C21 C 0.6917(2) 1.0419(5) 0.9116(5) 0.0399(13) Uani 1 1 d . . . . .
H21 H 0.685520 1.102446 0.868618 0.048 Uiso 1 1 calc R U . . .
C22 C 0.6605(2) 1.0275(5) 1.0023(6) 0.0425(14) Uani 1 1 d . . . . .
H22 H 0.633736 1.078310 1.019318 0.051 Uiso 1 1 calc R U . . .
C23 C 0.6687(2) 0.9423(5) 1.0637(5) 0.0384(14) Uani 1 1 d . . . . .
H23 H 0.648288 0.932742 1.124719 0.046 Uiso 1 1 calc R U . . .
N24 N 0.70732(18) 0.8688(4) 1.0369(4) 0.0317(9) Uani 1 1 d . . . . .
C25 C 0.7232(2) 0.7752(4) 1.0860(5) 0.0327(11) Uani 1 1 d . . . . .
H25 H 0.708999 0.745205 1.147549 0.039 Uiso 1 1 calc R U . . .
N26 N 0.83479(15) 0.8499(3) 0.7083(3) 0.0226(8) Uani 1 1 d . . . . .
C27 C 0.80325(18) 0.8305(4) 0.6266(4) 0.0260(10) Uani 1 1 d . . . . .
C28 C 0.8024(2) 0.8984(4) 0.5419(4) 0.0322(11) Uani 1 1 d . . . . .
H28 H 0.780559 0.883111 0.483970 0.039 Uiso 1 1 calc R U . . .
C29 C 0.8341(2) 0.9888(5) 0.5435(5) 0.0342(12) Uani 1 1 d . . . . .
H29 H 0.834329 1.036215 0.486036 0.041 Uiso 1 1 calc R U . . .
C30 C 0.8657(2) 1.0105(4) 0.6287(5) 0.0323(11) Uani 1 1 d . . . . .
H30 H 0.886687 1.073702 0.631587 0.039 Uiso 1 1 calc R U . . .
C31 C 0.86572(18) 0.9374(4) 0.7098(4) 0.0250(10) Uani 1 1 d . . . . .
C32 C 0.7715(2) 0.7330(4) 0.6384(5) 0.0273(11) Uani 1 1 d . . . . .
N33 N 0.77894(15) 0.6710(3) 0.7259(3) 0.0248(8) Uani 1 1 d . . . . .
C34 C 0.74622(19) 0.5881(4) 0.7160(4) 0.0275(10) Uani 1 1 d . . . . .
C35 C 0.7375(2) 0.4988(4) 0.7816(5) 0.0312(11) Uani 1 1 d . . . . .
H35 H 0.756219 0.491048 0.844770 0.037 Uiso 1 1 calc R U . . .
C36 C 0.7012(2) 0.4246(5) 0.7508(5) 0.0380(12) Uani 1 1 d . . . . .
H36 H 0.694720 0.364120 0.793694 0.046 Uiso 1 1 calc R U . . .
C37 C 0.6730(2) 0.4344(5) 0.6574(5) 0.0402(14) Uani 1 1 d . . . . .
H37 H 0.647821 0.381120 0.638484 0.048 Uiso 1 1 calc R U . . .
C38 C 0.6815(2) 0.5199(5) 0.5942(5) 0.0391(13) Uani 1 1 d . . . . .
H38 H 0.662818 0.526817 0.530821 0.047 Uiso 1 1 calc R U . . .
N39 N 0.71800(17) 0.5962(4) 0.6241(4) 0.0332(10) Uani 1 1 d . . . . .
C40 C 0.7342(2) 0.6890(5) 0.5755(5) 0.0342(12) Uani 1 1 d . . . . .
H40 H 0.721789 0.716534 0.511440 0.041 Uiso 1 1 calc R U . . .
C41 C 0.89791(18) 0.9454(4) 0.8030(4) 0.0256(10) Uani 1 1 d . . . . .
N42 N 0.89520(15) 0.8613(3) 0.8745(3) 0.0249(8) Uani 1 1 d . . . . .
C43 C 0.92827(19) 0.8885(4) 0.9504(4) 0.0248(10) Uani 1 1 d . . . . .
C44 C 0.9422(2) 0.8342(5) 1.0418(4) 0.0317(11) Uani 1 1 d . . . . .
H44 H 0.928676 0.764539 1.055931 0.038 Uiso 1 1 calc R U . . .
C45 C 0.9757(2) 0.8844(5) 1.1100(5) 0.0419(14) Uani 1 1 d . . . . .
H45 H 0.985171 0.849619 1.172610 0.050 Uiso 1 1 calc R U . . .
C46 C 0.9964(3) 0.9880(6) 1.0877(6) 0.0423(14) Uani 1 1 d . . . . .
H46 H 1.018535 1.022568 1.136941 0.051 Uiso 1 1 calc R U . . .
C47 C 0.9851(2) 1.0384(5) 0.9974(5) 0.0363(12) Uani 1 1 d . . . . .
H47 H 1.000059 1.106501 0.981728 0.044 Uiso 1 1 calc R U . . .
N48 N 0.95147(17) 0.9883(3) 0.9292(4) 0.0284(9) Uani 1 1 d . . . . .
C49 C 0.93210(18) 1.0224(3) 0.8360(5) 0.0269(9) Uani 1 1 d . . . . .
H49 H 0.940844 1.087223 0.801167 0.032 Uiso 1 1 calc R U . . .
B50 B 0.9243(3) 0.7713(7) 0.3494(7) 0.0514(19) Uani 1 1 d . . . . .
F51 F 0.9004(3) 0.7504(4) 0.4395(5) 0.0717(15) Uani 1 1 d . . . . .
F52 F 0.97862(14) 0.7514(3) 0.3500(4) 0.0512(10) Uani 1 1 d . . . . .
F53 F 0.92091(19) 0.8858(3) 0.3350(4) 0.0669(11) Uani 1 1 d . . . . .
F54 F 0.9008(2) 0.7294(4) 0.2644(4) 0.0637(13) Uani 1 1 d . . . . .
B55 B 0.8451(2) 0.2346(5) 0.8388(7) 0.0327(11) Uani 1 1 d . . . . .
F56 F 0.87725(16) 0.2518(3) 0.7525(3) 0.0424(9) Uani 1 1 d . . . . .
F57 F 0.87676(15) 0.2190(3) 0.9256(3) 0.0430(8) Uani 1 1 d . . . . .
F58 F 0.81389(14) 0.1448(3) 0.8216(3) 0.0495(9) Uani 1 1 d . . . . .
F59 F 0.81216(14) 0.3214(3) 0.8558(3) 0.0494(10) Uani 1 1 d . . . . .
C60A C 0.5736(6) 0.7467(11) 0.9478(14) 0.056(4) Uiso 0.5 1 d D . P A 1
H60A H 0.578455 0.753629 1.022652 0.083 Uiso 0.5 1 calc R U P A 1
H60B H 0.550524 0.685149 0.933293 0.083 Uiso 0.5 1 calc R U P A 1
H60C H 0.557226 0.812246 0.920685 0.083 Uiso 0.5 1 calc R U P A 1
O61A O 0.6230(4) 0.7309(9) 0.9004(10) 0.055(3) Uiso 0.5 1 d D . P A 1
H61A H 0.619847 0.685835 0.852499 0.066 Uiso 0.5 1 calc R U P A 1
C62A C 0.5926(8) 0.6625(15) 0.7359(18) 0.053(5) Uiso 0.35 1 d D . P B 3
H62A H 0.611324 0.593560 0.735447 0.079 Uiso 0.35 1 calc R U P B 3
H62B H 0.584104 0.683520 0.664863 0.079 Uiso 0.35 1 calc R U P B 3
H62C H 0.559782 0.655636 0.775878 0.079 Uiso 0.35 1 calc R U P B 3
O63A O 0.6258(8) 0.7429(14) 0.7822(17) 0.068(5) Uiso 0.35 1 d D . P B 3
H63A H 0.633701 0.724236 0.842681 0.081 Uiso 0.35 1 calc R U P B 3
C60B C 0.5783(10) 0.882(2) 0.835(2) 0.084(7) Uiso 0.35 1 d D . P C 2
H60D H 0.578009 0.960546 0.834999 0.126 Uiso 0.35 1 calc R U P C 2
H60E H 0.568875 0.855744 0.765709 0.126 Uiso 0.35 1 calc R U P C 2
H60F H 0.613797 0.856110 0.853050 0.126 Uiso 0.35 1 calc R U P C 2
O61B O 0.5415(4) 0.8436(9) 0.9067(10) 0.039(3) Uiso 0.35 1 d D . P C 2
H61B H 0.535102 0.891773 0.950401 0.047 Uiso 0.35 1 calc R U P C 2
C62B C 0.6117(12) 0.6877(17) 0.810(3) 0.068(8) Uiso 0.3 1 d D . P D 4
H62D H 0.644706 0.646082 0.810733 0.103 Uiso 0.3 1 calc R U P D 4
H62E H 0.593092 0.675830 0.744733 0.103 Uiso 0.3 1 calc R U P D 4
H62F H 0.589136 0.664737 0.867685 0.103 Uiso 0.3 1 calc R U P D 4
O63B O 0.6240(8) 0.8010(15) 0.821(2) 0.074(5) Uiso 0.3 1 d D . P D 4
H63B H 0.612933 0.834473 0.769052 0.089 Uiso 0.3 1 calc R U P D 4
loop_
_atom_type_symbol
_atom_type_description
_atom_type_scat_dispersion_real
_atom_type_scat_dispersion_imag
_atom_type_scat_source
C C 0.0181 0.0091 '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'
B B 0.0090 0.0039 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
F F 0.0727 0.0534 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Fe Fe -1.1336 3.1974 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
N N 0.0311 0.0180 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
O O 0.0492 0.0322 '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
_geom_angle_publ_flag
N2 Fe1 N9 73.84(15) . . ?
N2 Fe1 N18 74.16(16) . . ?
N2 Fe1 N26 175.96(14) . . ?
N2 Fe1 N33 101.71(16) . . ?
N2 Fe1 N42 109.53(16) . . ?
N9 Fe1 N18 147.96(16) . . ?
N9 Fe1 N33 93.82(15) . . ?
N9 Fe1 N42 92.44(14) . . ?
N18 Fe1 N42 96.67(16) . . ?
N26 Fe1 N9 107.76(15) . . ?
N26 Fe1 N18 104.27(15) . . ?
N26 Fe1 N33 74.58(16) . . ?
N26 Fe1 N42 74.26(16) . . ?
N33 Fe1 N18 94.13(15) . . ?
N33 Fe1 N42 148.66(17) . . ?
C3 N2 Fe1 120.5(3) . . ?
C3 N2 C7 119.7(4) . . ?
C7 N2 Fe1 119.8(3) . . ?
N2 C3 C4 121.3(5) . . ?
N2 C3 C8 112.7(4) . . ?
C4 C3 C8 125.9(4) . . ?
C3 C4 H4 120.6 . . ?
C5 C4 C3 118.8(5) . . ?
C5 C4 H4 120.6 . . ?
C4 C5 H5 119.8 . . ?
C4 C5 C6 120.3(5) . . ?
C6 C5 H5 119.8 . . ?
C5 C6 H6 121.0 . . ?
C5 C6 C7 118.0(5) . . ?
C7 C6 H6 121.0 . . ?
N2 C7 C6 121.8(5) . . ?
N2 C7 C17 113.1(5) . . ?
C6 C7 C17 125.0(5) . . ?
N9 C8 C3 117.3(4) . . ?
C16 C8 C3 130.8(5) . . ?
C16 C8 N9 111.9(5) . . ?
C8 N9 Fe1 115.4(3) . . ?
C10 N9 Fe1 138.7(3) . . ?
C10 N9 C8 105.6(4) . . ?
N9 C10 C11 131.4(5) . . ?
N9 C10 N15 109.9(4) . . ?
N15 C10 C11 118.7(5) . . ?
C10 C11 H11 120.3 . . ?
C12 C11 C10 119.5(5) . . ?
C12 C11 H11 120.3 . . ?
C11 C12 H12 119.9 . . ?
C11 C12 C13 120.1(6) . . ?
C13 C12 H12 119.9 . . ?
C12 C13 H13 119.4 . . ?
C14 C13 C12 121.2(6) . . ?
C14 C13 H13 119.4 . . ?
C13 C14 H14 120.8 . . ?
C13 C14 N15 118.5(6) . . ?
N15 C14 H14 120.8 . . ?
C14 N15 C10 122.0(5) . . ?
C14 N15 C16 130.4(5) . . ?
C16 N15 C10 107.6(4) . . ?
C8 C16 N15 105.0(4) . . ?
C8 C16 H16 127.5 . . ?
N15 C16 H16 127.5 . . ?
N18 C17 C7 118.3(5) . . ?
C25 C17 C7 130.3(5) . . ?
C25 C17 N18 111.4(5) . . ?
C17 N18 Fe1 114.5(3) . . ?
C19 N18 Fe1 140.5(4) . . ?
C19 N18 C17 104.9(4) . . ?
N18 C19 C20 130.9(5) . . ?
N18 C19 N24 110.9(4) . . ?
N24 C19 C20 118.2(5) . . ?
C19 C20 H20 120.5 . . ?
C21 C20 C19 119.0(5) . . ?
C21 C20 H20 120.5 . . ?
C20 C21 H21 119.4 . . ?
C20 C21 C22 121.2(5) . . ?
C22 C21 H21 119.4 . . ?
C21 C22 H22 120.0 . . ?
C23 C22 C21 120.1(5) . . ?
C23 C22 H22 120.0 . . ?
C22 C23 H23 120.5 . . ?
C22 C23 N24 119.0(6) . . ?
N24 C23 H23 120.5 . . ?
C23 N24 C19 122.5(5) . . ?
C23 N24 C25 130.3(5) . . ?
C25 N24 C19 107.2(4) . . ?
C17 C25 N24 105.5(5) . . ?
C17 C25 H25 127.2 . . ?
N24 C25 H25 127.2 . . ?
C27 N26 Fe1 119.6(3) . . ?
C31 N26 Fe1 120.3(3) . . ?
C31 N26 C27 120.1(4) . . ?
N26 C27 C28 121.4(5) . . ?
N26 C27 C32 113.0(5) . . ?
C28 C27 C32 125.6(5) . . ?
C27 C28 H28 120.7 . . ?
C29 C28 C27 118.5(5) . . ?
C29 C28 H28 120.7 . . ?
C28 C29 H29 119.9 . . ?
C28 C29 C30 120.2(5) . . ?
C30 C29 H29 119.9 . . ?
C29 C30 H30 120.9 . . ?
C29 C30 C31 118.3(5) . . ?
C31 C30 H30 120.9 . . ?
N26 C31 C30 121.5(5) . . ?
N26 C31 C41 113.0(4) . . ?
C30 C31 C41 125.5(5) . . ?
N33 C32 C27 118.4(5) . . ?
C40 C32 C27 130.6(5) . . ?
C40 C32 N33 111.0(5) . . ?
C32 N33 Fe1 114.4(3) . . ?
C34 N33 Fe1 139.8(4) . . ?
C34 N33 C32 105.7(4) . . ?
N33 C34 C35 130.5(5) . . ?
N33 C34 N39 110.1(5) . . ?
N39 C34 C35 119.3(5) . . ?
C34 C35 H35 121.2 . . ?
C36 C35 C34 117.6(5) . . ?
C36 C35 H35 121.2 . . ?
C35 C36 H36 118.9 . . ?
C35 C36 C37 122.2(6) . . ?
C37 C36 H36 118.9 . . ?
C36 C37 H37 119.9 . . ?
C38 C37 C36 120.3(5) . . ?
C38 C37 H37 119.9 . . ?
C37 C38 H38 120.8 . . ?
C37 C38 N39 118.5(6) . . ?
N39 C38 H38 120.8 . . ?
C38 N39 C34 122.1(5) . . ?
C40 N39 C34 107.5(4) . . ?
C40 N39 C38 130.4(5) . . ?
C32 C40 N39 105.7(5) . . ?
C32 C40 H40 127.2 . . ?
N39 C40 H40 127.2 . . ?
N42 C41 C31 118.0(4) . . ?
C49 C41 C31 131.4(5) . . ?
C49 C41 N42 110.6(5) . . ?
C41 N42 Fe1 114.1(3) . . ?
C43 N42 Fe1 140.1(3) . . ?
C43 N42 C41 105.5(4) . . ?
N42 C43 C44 130.8(5) . . ?
N42 C43 N48 110.1(4) . . ?
N48 C43 C44 119.1(5) . . ?
C43 C44 H44 120.8 . . ?
C45 C44 C43 118.3(5) . . ?
C45 C44 H44 120.8 . . ?
C44 C45 H45 119.7 . . ?
C44 C45 C46 120.6(6) . . ?
C46 C45 H45 119.7 . . ?
C45 C46 H46 119.4 . . ?
C47 C46 C45 121.2(6) . . ?
C47 C46 H46 119.4 . . ?
C46 C47 H47 120.9 . . ?
C46 C47 N48 118.2(5) . . ?
N48 C47 H47 120.9 . . ?
C47 N48 C43 122.4(5) . . ?
C49 N48 C43 107.4(4) . . ?
C49 N48 C47 130.2(5) . . ?
C41 C49 N48 106.5(4) . . ?
C41 C49 H49 126.8 . . ?
N48 C49 H49 126.8 . . ?
F51 B50 F52 113.8(8) . . ?
F51 B50 F53 106.2(7) . . ?
F51 B50 F54 115.9(6) . . ?
F52 B50 F53 103.6(6) . . ?
F54 B50 F52 111.5(7) . . ?
F54 B50 F53 104.5(7) . . ?
F57 B55 F56 109.5(4) . . ?
F58 B55 F56 108.9(6) . . ?
F58 B55 F57 110.1(6) . . ?
F59 B55 F56 110.9(6) . . ?
F59 B55 F57 109.0(6) . . ?
F59 B55 F58 108.5(4) . . ?
H60A C60A H60B 109.5 . . ?
H60A C60A H60C 109.5 . . ?
H60B C60A H60C 109.5 . . ?
O61A C60A H60A 109.5 . . ?
O61A C60A H60B 109.5 . . ?
O61A C60A H60C 109.5 . . ?
C60A O61A H61A 109.5 . . ?
H62A C62A H62B 109.5 . . ?
H62A C62A H62C 109.5 . . ?
H62B C62A H62C 109.5 . . ?
O63A C62A H62A 109.5 . . ?
O63A C62A H62B 109.5 . . ?
O63A C62A H62C 109.5 . . ?
C62A O63A H63A 109.5 . . ?
H60D C60B H60E 109.5 . . ?
H60D C60B H60F 109.5 . . ?
H60E C60B H60F 109.5 . . ?
O61B C60B H60D 109.5 . . ?
O61B C60B H60E 109.5 . . ?
O61B C60B H60F 109.5 . . ?
C60B O61B H61B 109.5 . . ?
H62D C62B H62E 109.5 . . ?
H62D C62B H62F 109.5 . . ?
H62E C62B H62F 109.5 . . ?
O63B C62B H62D 109.5 . . ?
O63B C62B H62E 109.5 . . ?
O63B C62B H62F 109.5 . . ?
C62B O63B H63B 109.5 . . ?
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 N2 2.171(4) . ?
Fe1 N9 2.193(4) . ?
Fe1 N18 2.199(4) . ?
Fe1 N26 2.171(4) . ?
Fe1 N33 2.194(4) . ?
Fe1 N42 2.201(4) . ?
N2 C3 1.343(6) . ?
N2 C7 1.351(7) . ?
C3 C4 1.393(7) . ?
C3 C8 1.467(7) . ?
C4 H4 0.9500 . ?
C4 C5 1.382(8) . ?
C5 H5 0.9500 . ?
C5 C6 1.384(8) . ?
C6 H6 0.9500 . ?
C6 C7 1.394(7) . ?
C7 C17 1.445(7) . ?
C8 N9 1.385(6) . ?
C8 C16 1.353(7) . ?
N9 C10 1.331(6) . ?
C10 C11 1.397(8) . ?
C10 N15 1.395(6) . ?
C11 H11 0.9500 . ?
C11 C12 1.353(8) . ?
C12 H12 0.9500 . ?
C12 C13 1.425(10) . ?
C13 H13 0.9500 . ?
C13 C14 1.337(9) . ?
C14 H14 0.9500 . ?
C14 N15 1.380(7) . ?
N15 C16 1.393(7) . ?
C16 H16 0.9500 . ?
C17 N18 1.388(7) . ?
C17 C25 1.368(8) . ?
N18 C19 1.340(6) . ?
C19 C20 1.415(7) . ?
C19 N24 1.387(7) . ?
C20 H20 0.9500 . ?
C20 C21 1.353(8) . ?
C21 H21 0.9500 . ?
C21 C22 1.426(9) . ?
C22 H22 0.9500 . ?
C22 C23 1.342(9) . ?
C23 H23 0.9500 . ?
C23 N24 1.381(7) . ?
N24 C25 1.387(7) . ?
C25 H25 0.9500 . ?
N26 C27 1.345(6) . ?
N26 C31 1.341(6) . ?
C27 C28 1.385(7) . ?
C27 C32 1.461(7) . ?
C28 H28 0.9500 . ?
C28 C29 1.381(8) . ?
C29 H29 0.9500 . ?
C29 C30 1.386(8) . ?
C30 H30 0.9500 . ?
C30 C31 1.389(7) . ?
C31 C41 1.458(7) . ?
C32 N33 1.384(7) . ?
C32 C40 1.361(8) . ?
N33 C34 1.329(6) . ?
C34 C35 1.415(7) . ?
C34 N39 1.391(7) . ?
C35 H35 0.9500 . ?
C35 C36 1.360(8) . ?
C36 H36 0.9500 . ?
C36 C37 1.408(9) . ?
C37 H37 0.9500 . ?
C37 C38 1.360(9) . ?
C38 H38 0.9500 . ?
C38 N39 1.378(7) . ?
N39 C40 1.378(7) . ?
C40 H40 0.9500 . ?
C41 N42 1.399(6) . ?
C41 C49 1.359(7) . ?
N42 C43 1.332(6) . ?
C43 C44 1.407(7) . ?
C43 N48 1.400(7) . ?
C44 H44 0.9500 . ?
C44 C45 1.374(8) . ?
C45 H45 0.9500 . ?
C45 C46 1.421(9) . ?
C46 H46 0.9500 . ?
C46 C47 1.357(9) . ?
C47 H47 0.9500 . ?
C47 N48 1.374(7) . ?
N48 C49 1.369(7) . ?
C49 H49 0.9500 . ?
B50 F51 1.338(11) . ?
B50 F52 1.393(9) . ?
B50 F53 1.440(10) . ?
B50 F54 1.355(10) . ?
B55 F56 1.398(9) . ?
B55 F57 1.392(9) . ?
B55 F58 1.385(7) . ?
B55 F59 1.380(6) . ?
C60A H60A 0.9800 . ?
C60A H60B 0.9800 . ?
C60A H60C 0.9800 . ?
C60A O61A 1.402(15) . ?
O61A H61A 0.8400 . ?
C62A H62A 0.9800 . ?
C62A H62B 0.9800 . ?
C62A H62C 0.9800 . ?
C62A O63A 1.436(17) . ?
O63A H63A 0.8400 . ?
C60B H60D 0.9800 . ?
C60B H60E 0.9800 . ?
C60B H60F 0.9800 . ?
C60B O61B 1.398(18) . ?
O61B H61B 0.8400 . ?
C62B H62D 0.9800 . ?
C62B H62E 0.9800 . ?
C62B H62F 0.9800 . ?
C62B O63B 1.452(18) . ?
O63B H63B 0.8400 . ?
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
Fe1 N2 C3 C4 -179.0(4) . . . . ?
Fe1 N2 C3 C8 2.3(5) . . . . ?
Fe1 N2 C7 C6 -178.8(4) . . . . ?
Fe1 N2 C7 C17 1.6(6) . . . . ?
Fe1 N9 C10 C11 5.1(9) . . . . ?
Fe1 N9 C10 N15 -172.9(4) . . . . ?
Fe1 N18 C19 C20 -1.6(10) . . . . ?
Fe1 N18 C19 N24 177.3(4) . . . . ?
Fe1 N26 C27 C28 -178.8(4) . . . . ?
Fe1 N26 C27 C32 1.2(5) . . . . ?
Fe1 N26 C31 C30 -179.3(4) . . . . ?
Fe1 N26 C31 C41 0.8(5) . . . . ?
Fe1 N33 C34 C35 -4.4(9) . . . . ?
Fe1 N33 C34 N39 176.2(4) . . . . ?
Fe1 N42 C43 C44 8.5(9) . . . . ?
Fe1 N42 C43 N48 -171.9(4) . . . . ?
N2 C3 C4 C5 -1.7(8) . . . . ?
N2 C3 C8 N9 1.4(6) . . . . ?
N2 C3 C8 C16 -178.0(5) . . . . ?
N2 C7 C17 N18 -2.1(7) . . . . ?
N2 C7 C17 C25 176.8(6) . . . . ?
C3 N2 C7 C6 2.5(7) . . . . ?
C3 N2 C7 C17 -177.2(4) . . . . ?
C3 C4 C5 C6 1.4(8) . . . . ?
C3 C8 N9 Fe1 -4.3(5) . . . . ?
C3 C8 N9 C10 -179.9(4) . . . . ?
C3 C8 C16 N15 179.0(5) . . . . ?
C4 C3 C8 N9 -177.2(5) . . . . ?
C4 C3 C8 C16 3.4(9) . . . . ?
C4 C5 C6 C7 0.7(9) . . . . ?
C5 C6 C7 N2 -2.7(8) . . . . ?
C5 C6 C7 C17 177.0(5) . . . . ?
C6 C7 C17 N18 178.2(5) . . . . ?
C6 C7 C17 C25 -2.9(10) . . . . ?
C7 N2 C3 C4 -0.3(7) . . . . ?
C7 N2 C3 C8 -179.0(4) . . . . ?
C7 C17 N18 Fe1 1.6(6) . . . . ?
C7 C17 N18 C19 -179.3(5) . . . . ?
C7 C17 C25 N24 179.8(6) . . . . ?
C8 C3 C4 C5 176.8(5) . . . . ?
C8 N9 C10 C11 179.1(6) . . . . ?
C8 N9 C10 N15 1.1(5) . . . . ?
N9 C8 C16 N15 -0.4(6) . . . . ?
N9 C10 C11 C12 -179.8(6) . . . . ?
N9 C10 N15 C14 -179.4(5) . . . . ?
N9 C10 N15 C16 -1.4(6) . . . . ?
C10 C11 C12 C13 0.9(10) . . . . ?
C10 N15 C16 C8 1.1(6) . . . . ?
C11 C10 N15 C14 2.4(8) . . . . ?
C11 C10 N15 C16 -179.7(5) . . . . ?
C11 C12 C13 C14 0.0(11) . . . . ?
C12 C13 C14 N15 0.3(11) . . . . ?
C13 C14 N15 C10 -1.5(9) . . . . ?
C13 C14 N15 C16 -179.0(6) . . . . ?
C14 N15 C16 C8 178.8(6) . . . . ?
N15 C10 C11 C12 -2.0(8) . . . . ?
C16 C8 N9 Fe1 175.2(3) . . . . ?
C16 C8 N9 C10 -0.5(6) . . . . ?
C17 N18 C19 C20 179.8(6) . . . . ?
C17 N18 C19 N24 -1.4(6) . . . . ?
N18 C17 C25 N24 -1.2(6) . . . . ?
N18 C19 C20 C21 179.0(6) . . . . ?
N18 C19 N24 C23 179.8(5) . . . . ?
N18 C19 N24 C25 0.7(6) . . . . ?
C19 C20 C21 C22 0.4(9) . . . . ?
C19 N24 C25 C17 0.3(6) . . . . ?
C20 C19 N24 C23 -1.2(8) . . . . ?
C20 C19 N24 C25 179.7(5) . . . . ?
C20 C21 C22 C23 -0.2(10) . . . . ?
C21 C22 C23 N24 -0.8(10) . . . . ?
C22 C23 N24 C19 1.5(9) . . . . ?
C22 C23 N24 C25 -179.6(6) . . . . ?
C23 N24 C25 C17 -178.6(6) . . . . ?
N24 C19 C20 C21 0.3(8) . . . . ?
C25 C17 N18 Fe1 -177.4(4) . . . . ?
C25 C17 N18 C19 1.6(6) . . . . ?
N26 C27 C28 C29 -1.3(8) . . . . ?
N26 C27 C32 N33 -3.1(7) . . . . ?
N26 C27 C32 C40 177.4(6) . . . . ?
N26 C31 C41 N42 3.4(6) . . . . ?
N26 C31 C41 C49 -176.9(5) . . . . ?
C27 N26 C31 C30 0.8(7) . . . . ?
C27 N26 C31 C41 -179.1(4) . . . . ?
C27 C28 C29 C30 -0.4(8) . . . . ?
C27 C32 N33 Fe1 3.5(6) . . . . ?
C27 C32 N33 C34 -179.1(5) . . . . ?
C27 C32 C40 N39 178.9(5) . . . . ?
C28 C27 C32 N33 176.9(5) . . . . ?
C28 C27 C32 C40 -2.6(9) . . . . ?
C28 C29 C30 C31 2.2(8) . . . . ?
C29 C30 C31 N26 -2.4(8) . . . . ?
C29 C30 C31 C41 177.5(5) . . . . ?
C30 C31 C41 N42 -176.5(5) . . . . ?
C30 C31 C41 C49 3.2(9) . . . . ?
C31 N26 C27 C28 1.1(7) . . . . ?
C31 N26 C27 C32 -178.9(4) . . . . ?
C31 C41 N42 Fe1 -5.8(5) . . . . ?
C31 C41 N42 C43 179.5(4) . . . . ?
C31 C41 C49 N48 -179.9(5) . . . . ?
C32 C27 C28 C29 178.7(5) . . . . ?
C32 N33 C34 C35 179.2(6) . . . . ?
C32 N33 C34 N39 -0.2(6) . . . . ?
N33 C32 C40 N39 -0.7(6) . . . . ?
N33 C34 C35 C36 -179.5(5) . . . . ?
N33 C34 N39 C38 179.4(5) . . . . ?
N33 C34 N39 C40 -0.2(6) . . . . ?
C34 C35 C36 C37 0.1(9) . . . . ?
C34 N39 C40 C32 0.5(6) . . . . ?
C35 C34 N39 C38 0.0(8) . . . . ?
C35 C34 N39 C40 -179.7(5) . . . . ?
C35 C36 C37 C38 0.3(10) . . . . ?
C36 C37 C38 N39 -0.4(10) . . . . ?
C37 C38 N39 C34 0.3(9) . . . . ?
C37 C38 N39 C40 179.9(6) . . . . ?
C38 N39 C40 C32 -179.1(6) . . . . ?
N39 C34 C35 C36 -0.2(8) . . . . ?
C40 C32 N33 Fe1 -176.9(4) . . . . ?
C40 C32 N33 C34 0.5(6) . . . . ?
C41 N42 C43 C44 -179.0(5) . . . . ?
C41 N42 C43 N48 0.6(5) . . . . ?
N42 C41 C49 N48 -0.2(6) . . . . ?
N42 C43 C44 C45 -176.5(6) . . . . ?
N42 C43 N48 C47 176.4(5) . . . . ?
N42 C43 N48 C49 -0.7(6) . . . . ?
C43 C44 C45 C46 -0.9(9) . . . . ?
C43 N48 C49 C41 0.5(5) . . . . ?
C44 C43 N48 C47 -3.9(8) . . . . ?
C44 C43 N48 C49 179.0(5) . . . . ?
C44 C45 C46 C47 -2.2(11) . . . . ?
C45 C46 C47 N48 2.3(10) . . . . ?
C46 C47 N48 C43 0.8(8) . . . . ?
C46 C47 N48 C49 177.2(6) . . . . ?
C47 N48 C49 C41 -176.3(5) . . . . ?
N48 C43 C44 C45 3.9(8) . . . . ?
C49 C41 N42 Fe1 174.4(3) . . . . ?
C49 C41 N42 C43 -0.3(6) . . . . ?
loop_
_twin_individual_id
_twin_individual_mass_fraction_refined
1 0.502(7)
2 0.498(7)
