#------------------------------------------------------------------------------
#$Date: 2023-09-27 02:05:22 +0300 (Wed, 27 Sep 2023) $
#$Revision: 286546 $
#$URL: file:///home/coder/svn-repositories/cod/cif/7/71/40/7714022.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_7714022
loop_
_publ_author_name
'Guthardt, Robin'
'Jacob, Hannes Lukas'
'Bruhn, Clemens'
'Siemeling, Ulrich'
_publ_section_title
;
 A complete series of N-heterocyclic tetrylenes (Si -- Pb) with a
 1,1’-ferrocenediyl backbone enabled by 1,3,2-diazaborolyl
 N-substituents
;
_journal_name_full               'Dalton Transactions'
_journal_paper_doi               10.1039/D3DT02684A
_journal_year                    2023
_chemical_formula_moiety         'C62 H82 B2 Fe N6'
_chemical_formula_sum            'C62 H82 B2 Fe N6'
_chemical_formula_weight         988.80
_space_group_crystal_system      orthorhombic
_space_group_IT_number           41
_space_group_name_Hall           'A 2 -2ab'
_space_group_name_H-M_alt        'A e a 2'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     dual
_audit_creation_date             2023-07-12
_audit_creation_method
;
Olex2 1.5
(compiled 2023.03.06 svn.rbb2c1857 for OlexSys, GUI svn.r6748)
;
_audit_update_record
;
2023-08-16 deposited with the CCDC.	2023-09-26 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 90
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   8.9740(4)
_cell_length_b                   29.2515(17)
_cell_length_c                   21.3053(9)
_cell_measurement_reflns_used    7348
_cell_measurement_temperature    100(2)
_cell_measurement_theta_max      70.91
_cell_measurement_theta_min      3.02
_cell_volume                     5592.7(5)
_computing_cell_refinement
;
X-Area Recipe 1.37.0.0 (STOE, 2021)
;
_computing_data_collection
;
X-Area Pilatus3_SV 1.31.175.0 (STOE, 2021)
;
_computing_data_reduction
;
X-Area Integrate 2.5.1.0 (STOE, 2021)
X-Area LANA 2.6.2.0 (STOE, 2021)
;
_computing_molecular_graphics    'Olex2 1.5 (Dolomanov et al., 2009)'
_computing_publication_material
;
STOE & Cie GmbH, X-Area, software package for collecting single-crystal or
multi-domain crystal data on STOE area-detector diffractometers, for image 
processing, for the correction and scaling of reflection intensities and 
for outlier rejection, version 2.0, Darmstadt 2021
;
_computing_structure_refinement  'SHELXL 2014/7 (Sheldrick, 2015)'
_computing_structure_solution    'SHELXT  (Sheldrick, 2015)'
_diffrn_ambient_temperature      100(2)
_diffrn_detector                 Pilatus200K
_diffrn_detector_area_resol_mean 5.81
_diffrn_detector_type            'DECTRIS PILATUS 200K'
_diffrn_measured_fraction_theta_full 0.992
_diffrn_measured_fraction_theta_max 0.975
_diffrn_measurement_details
;
 862 frames, detector distance = 40 mm
;
_diffrn_measurement_device       'Eulerian 4-circle diffractometer'
_diffrn_measurement_device_type  'STOE STADIVARI'
_diffrn_measurement_method       'rotation method, ω scans'
_diffrn_radiation_collimation    '1.2 mm, 0.6 diameter'
_diffrn_radiation_monochromator  'Graded multilayer mirror'
_diffrn_radiation_polarisn_norm  0
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           'Cu K\a'
_diffrn_radiation_wavelength     1.54186
_diffrn_reflns_av_R_equivalents  0.0902
_diffrn_reflns_av_unetI/netI     0.0916
_diffrn_reflns_Laue_measured_fraction_full 0.992
_diffrn_reflns_Laue_measured_fraction_max 0.975
_diffrn_reflns_limit_h_max       10
_diffrn_reflns_limit_h_min       -7
_diffrn_reflns_limit_k_max       35
_diffrn_reflns_limit_k_min       -33
_diffrn_reflns_limit_l_max       12
_diffrn_reflns_limit_l_min       -25
_diffrn_reflns_number            10412
_diffrn_reflns_point_group_measured_fraction_full 0.993
_diffrn_reflns_point_group_measured_fraction_max 0.976
_diffrn_reflns_theta_full        67.686
_diffrn_reflns_theta_max         70.459
_diffrn_reflns_theta_min         3.021
_diffrn_source                   Cu-Genix
_diffrn_source_current           0.600
_diffrn_source_power             0.030
_diffrn_source_target            Cu
_diffrn_source_type              'Genix Cu 3D HF'
_diffrn_source_voltage           50
_exptl_absorpt_coefficient_mu    2.485
_exptl_absorpt_correction_T_max  0.8355
_exptl_absorpt_correction_T_min  0.2403
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
STOE X-Red32, absorption correction by Gaussian integration, analogous to
P. Coppens, "The Evaluation of Absorption and Extinction in Single-Crystal
Structure Analysis", published in: F. R. Ahmed (Editor), "Crystallographic
Computing", Munksgaard, Copenhagen (1970), 255 - 270. Afterwards scaling of
reflection intensities was performed within STOE LANA. J. Koziskova, F. Hahn,
J. Richter, J. Kozisek, Acta Chimica Slovaca, vol. 9, no. 2, 2016, pp. 136-140.
;
_exptl_crystal_colour            yellow
_exptl_crystal_colour_primary    yellow
_exptl_crystal_density_diffrn    1.174
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       plate
_exptl_crystal_F_000             2128
_exptl_crystal_size_max          0.131
_exptl_crystal_size_mid          0.124
_exptl_crystal_size_min          0.04
_refine_diff_density_max         0.755
_refine_diff_density_min         -0.340
_refine_diff_density_rms         0.086
_refine_ls_abs_structure_details
;
 Refined as an inversion twin.
;
_refine_ls_abs_structure_Flack   0.362(15)
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.055
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     330
_refine_ls_number_reflns         3424
_refine_ls_number_restraints     1
_refine_ls_restrained_S_all      1.055
_refine_ls_R_factor_all          0.1146
_refine_ls_R_factor_gt           0.0738
_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)+(0.0963P)²+1.7532P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1533
_refine_ls_wR_factor_ref         0.1736
_reflns_Friedel_coverage         0.944
_reflns_Friedel_fraction_full    0.993
_reflns_Friedel_fraction_max     0.977
_reflns_number_gt                2447
_reflns_number_total             3424
_reflns_threshold_expression     'I > 2σ(I)'
_cod_data_source_file            d3dt02684a2.cif
_cod_data_source_block           sv1129
_cod_original_sg_symbol_Hall     'A 2 -2ac'
_cod_database_code               7714022
_shelx_shelxl_version_number     2014/7
_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   0.907
_shelx_estimated_absorpt_t_min   0.737
_olex2_refinement_description
;
1. Twinned data refinement
 Scales: 0.638(15)
 0.362(15)
2. Fixed Uiso
 At 1.2 times of:
  All C(H) groups, All N(H) groups
 At 1.5 times of:
  All C(H,H,H) groups
3.a Ternary CH refined with riding coordinates:
 C14(H14), C17(H17), C26(H26), C29(H29)
3.b Aromatic/amide H refined with riding coordinates:
 N1(H1), C2(H2), C3(H3), C4(H4), C5(H5), C6(H6), C7(H7), C10(H10), C11(H11),
 C12(H12), C22(H22), C23(H23), C24(H24)
3.c Idealised Me refined as rotating group:
 C15(H15A,H15B,H15C), C16(H16A,H16B,H16C), C18(H18A,H18B,H18C), C19(H19A,H19B,
 H19C), C27(H27A,H27B,H27C), C28(H28A,H28B,H28C), C30(H30A,H30B,H30C), C31(H31A,
 H31B,H31C)
;
_olex2_submission_special_instructions 'No special instructions were received'
_stoe_detector_distance          '40.0 mm'
_stoe_detector_pixelsize_x       '0.172 mm'
_stoe_detector_pixelsize_y       '0.172 mm'
_stoe_detector_size_x            '7.0 cm'
_stoe_detector_size_y            '8.4 cm'
_stoe_evaluation_integration_a   4.0
_stoe_evaluation_integration_b   4.0
_stoe_evaluation_integration_ems 0.040
_stoe_evaluation_lana_bis_l_even_max -
_stoe_evaluation_lana_bis_l_odd_max -
_stoe_evaluation_lana_bos_l_even_max -
_stoe_evaluation_lana_bos_l_odd_max -
_stoe_evaluation_lana_completeness 64.0
_stoe_evaluation_lana_dxs_max_order 1
_stoe_evaluation_lana_dys_max_order 1
_stoe_evaluation_lana_fs_max_order 3
_stoe_evaluation_lana_max_2theta_available 141.1
_stoe_evaluation_lana_max_2theta_desired 141.1
_stoe_evaluation_lana_mean_redundancy 3.0
_stoe_evaluation_lana_number_refls_after_or 10412
_stoe_evaluation_lana_number_refls_outliers 2023
_stoe_evaluation_lana_number_refls_total 12435
_stoe_evaluation_lana_number_refls_unique 3424
_stoe_evaluation_lana_number_refls_written 10412
_stoe_evaluation_lana_or_c1      0.035
_stoe_evaluation_lana_or_c2      0
_stoe_evaluation_lana_or_c3      0
_stoe_evaluation_lana_or_c4      0.7
_stoe_evaluation_lana_point_group mm2
_stoe_evaluation_lana_table
;
#----------------------------------------------------------------------------
2Theta          12.8   28.0   43.2   58.4   73.6   88.8  104.0  119.2  134.4
#----------------------------------------------------------------------------
<Resolution>    5.57   3.08   2.07   1.55   1.29   1.09   0.97   0.90   0.84
N(total)          53    226    662   1288   2748   2797   1995   1977    689
<Redundancy>     1.6    1.7    2.0    2.8    4.5    3.9    2.9    2.8    1.8
Complet. [%%]    94.1   87.7   86.3   71.3   68.8   65.7   60.9   60.2   45.8
<I/sigma>      212.1   58.9   26.6   13.1    5.8    3.6    2.4    1.7    1.8
R(int)         0.016  0.023  0.037  0.041  0.088  0.131  0.178  0.242  0.238
#----------------------------------------------------------------------------
;
_stoe_measurement_identifier     sv1129
_stoe_measurement_max_exposure_per_frame '70.0 s'
_stoe_measurement_mean_exposure_per_frame '70.0 s'
_stoe_measurement_min_exposure_per_frame '70.0 s'
_stoe_measurement_total_exposure_time '16.8 h'
_stoe_measurement_total_frame_number 862
_stoe_measurement_total_run_number 17
_stoe_measurement_tube_power     '30.0 W'
loop_
_space_group_symop_operation_xyz
'x, y, z'
'-x, -y, z'
'x+1/2, -y+1/2, z'
'-x+1/2, y+1/2, z'
'x, y+1/2, z+1/2'
'-x, -y+1/2, z+1/2'
'x+1/2, -y+1, z+1/2'
'-x+1/2, y+1, z+1/2'
loop_
_atom_site_label
_atom_site_type_symbol
_atom_site_fract_x
_atom_site_fract_y
_atom_site_fract_z
_atom_site_U_iso_or_equiv
_atom_site_adp_type
_atom_site_occupancy
_atom_site_site_symmetry_order
_atom_site_calc_flag
_atom_site_refinement_flags_posn
_atom_site_refinement_flags_adp
_atom_site_refinement_flags_occupancy
_atom_site_disorder_assembly
_atom_site_disorder_group
C1 C 0.5550(9) 0.4391(3) 0.5768(4) 0.0206(18) Uani 1 1 d . . . . .
Fe1 Fe 0.5000 0.5000 0.62325(10) 0.0178(4) Uani 1 2 d S T P . .
N1 N 0.5001(7) 0.4204(2) 0.5208(3) 0.0185(13) Uani 1 1 d . . . . .
H1 H 0.5204 0.4380 0.4883 0.022 Uiso 1 1 calc R U . . .
B1 B 0.4194(10) 0.3801(3) 0.5025(4) 0.022(2) Uani 1 1 d . . . . .
C2 C 0.5039(8) 0.4310(2) 0.6388(3) 0.0181(18) Uani 1 1 d . . . . .
H2 H 0.4197 0.4132 0.6503 0.022 Uiso 1 1 calc R U . . .
N2 N 0.4091(7) 0.3665(2) 0.4384(3) 0.0188(14) Uani 1 1 d . . . . .
C3 C 0.6014(8) 0.4544(3) 0.6809(4) 0.0202(18) Uani 1 1 d . . . . .
H3 H 0.5957 0.4540 0.7254 0.024 Uiso 1 1 calc R U . . .
N3 N 0.3355(7) 0.3461(2) 0.5373(3) 0.0196(14) Uani 1 1 d . . . . .
C4 C 0.7084(8) 0.4782(3) 0.6445(4) 0.0214(18) Uani 1 1 d . . . . .
H4 H 0.7867 0.4969 0.6602 0.026 Uiso 1 1 calc R U . . .
C5 C 0.6773(8) 0.4693(3) 0.5806(4) 0.0204(18) Uani 1 1 d . . . . .
H5 H 0.7302 0.4815 0.5458 0.024 Uiso 1 1 calc R U . . .
C6 C 0.3235(9) 0.3266(3) 0.4352(4) 0.0260(19) Uani 1 1 d . . . . .
H6 H 0.3002 0.3105 0.3977 0.031 Uiso 1 1 calc R U . . .
C7 C 0.2796(8) 0.3146(3) 0.4923(4) 0.0255(19) Uani 1 1 d . . . . .
H7 H 0.2198 0.2887 0.5017 0.031 Uiso 1 1 calc R U . . .
C8 C 0.4710(8) 0.3884(3) 0.3836(4) 0.0191(17) Uani 1 1 d . . . . .
C9 C 0.3881(8) 0.4223(3) 0.3538(3) 0.0196(17) Uani 1 1 d . . . . .
C10 C 0.4481(9) 0.4423(3) 0.2999(4) 0.0273(19) Uani 1 1 d . . . . .
H10 H 0.3933 0.4651 0.2780 0.033 Uiso 1 1 calc R U . . .
C11 C 0.5868(9) 0.4292(3) 0.2785(4) 0.027(2) Uani 1 1 d . . . . .
H11 H 0.6265 0.4433 0.2420 0.032 Uiso 1 1 calc R U . . .
C12 C 0.6681(9) 0.3965(3) 0.3084(4) 0.028(2) Uani 1 1 d . . . . .
H12 H 0.7637 0.3886 0.2927 0.033 Uiso 1 1 calc R U . . .
C13 C 0.6134(8) 0.3744(3) 0.3620(4) 0.0215(18) Uani 1 1 d . . . . .
C14 C 0.2363(10) 0.4381(3) 0.3777(4) 0.0284(19) Uani 1 1 d . . . . .
H14 H 0.2013 0.4158 0.4100 0.034 Uiso 1 1 calc R U . . .
C15 C 0.2514(11) 0.4847(3) 0.4090(4) 0.041(2) Uani 1 1 d . . . . .
H15A H 0.3225 0.4826 0.4438 0.061 Uiso 1 1 calc R U . . .
H15B H 0.1541 0.4944 0.4251 0.061 Uiso 1 1 calc R U . . .
H15C H 0.2873 0.5071 0.3782 0.061 Uiso 1 1 calc R U . . .
C16 C 0.1194(10) 0.4397(3) 0.3246(5) 0.040(2) Uani 1 1 d . . . . .
H16A H 0.1418 0.4653 0.2964 0.060 Uiso 1 1 calc R U . . .
H16B H 0.0200 0.4440 0.3428 0.060 Uiso 1 1 calc R U . . .
H16C H 0.1219 0.4110 0.3010 0.060 Uiso 1 1 calc R U . . .
C17 C 0.6980(9) 0.3364(3) 0.3939(5) 0.037(2) Uani 1 1 d . . . . .
H17 H 0.6617 0.3347 0.4382 0.044 Uiso 1 1 calc R U . . .
C18 C 0.8680(10) 0.3453(4) 0.3962(5) 0.048(3) Uani 1 1 d . . . . .
H18A H 0.9084 0.3450 0.3535 0.072 Uiso 1 1 calc R U . . .
H18B H 0.9163 0.3214 0.4212 0.072 Uiso 1 1 calc R U . . .
H18C H 0.8868 0.3752 0.4154 0.072 Uiso 1 1 calc R U . . .
C19 C 0.6647(12) 0.2905(3) 0.3630(5) 0.053(3) Uani 1 1 d . . . . .
H19A H 0.6846 0.2926 0.3178 0.080 Uiso 1 1 calc R U . . .
H19B H 0.5598 0.2826 0.3697 0.080 Uiso 1 1 calc R U . . .
H19C H 0.7283 0.2669 0.3815 0.080 Uiso 1 1 calc R U . . .
C20 C 0.2821(8) 0.3427(2) 0.6006(3) 0.0184(17) Uani 1 1 d . . . . .
C21 C 0.1375(7) 0.3581(2) 0.6124(4) 0.0191(18) Uani 1 1 d . . . . .
C22 C 0.0839(9) 0.3544(3) 0.6734(4) 0.029(2) Uani 1 1 d . . . . .
H22 H -0.0140 0.3649 0.6824 0.035 Uiso 1 1 calc R U . . .
C23 C 0.1683(10) 0.3358(3) 0.7214(4) 0.033(2) Uani 1 1 d . . . . .
H23 H 0.1294 0.3336 0.7627 0.040 Uiso 1 1 calc R U . . .
C24 C 0.3135(9) 0.3204(3) 0.7075(4) 0.0264(19) Uani 1 1 d . . . . .
H24 H 0.3724 0.3072 0.7398 0.032 Uiso 1 1 calc R U . . .
C25 C 0.3718(8) 0.3241(2) 0.6472(4) 0.0196(18) Uani 1 1 d . . . . .
C26 C 0.0412(8) 0.3804(3) 0.5621(4) 0.0245(19) Uani 1 1 d . . . . .
H26 H 0.0782 0.3692 0.5206 0.029 Uiso 1 1 calc R U . . .
C27 C 0.0643(9) 0.4323(3) 0.5632(5) 0.037(2) Uani 1 1 d . . . . .
H27A H 0.0209 0.4450 0.6017 0.056 Uiso 1 1 calc R U . . .
H27B H 0.0155 0.4461 0.5267 0.056 Uiso 1 1 calc R U . . .
H27C H 0.1712 0.4392 0.5620 0.056 Uiso 1 1 calc R U . . .
C28 C -0.1235(9) 0.3679(3) 0.5662(4) 0.032(2) Uani 1 1 d . . . . .
H28A H -0.1770 0.3814 0.5307 0.048 Uiso 1 1 calc R U . . .
H28B H -0.1649 0.3796 0.6056 0.048 Uiso 1 1 calc R U . . .
H28C H -0.1343 0.3346 0.5650 0.048 Uiso 1 1 calc R U . . .
C29 C 0.5313(8) 0.3089(3) 0.6327(4) 0.0229(19) Uani 1 1 d . . . . .
H29 H 0.5730 0.3305 0.6009 0.028 Uiso 1 1 calc R U . . .
C30 C 0.5318(10) 0.2611(3) 0.6038(5) 0.042(3) Uani 1 1 d . . . . .
H30A H 0.4869 0.2394 0.6332 0.063 Uiso 1 1 calc R U . . .
H30B H 0.6345 0.2519 0.5948 0.063 Uiso 1 1 calc R U . . .
H30C H 0.4741 0.2614 0.5647 0.063 Uiso 1 1 calc R U . . .
C31 C 0.6337(9) 0.3099(3) 0.6897(4) 0.035(2) Uani 1 1 d . . . . .
H31A H 0.6343 0.3408 0.7077 0.052 Uiso 1 1 calc R U . . .
H31B H 0.7350 0.3016 0.6770 0.052 Uiso 1 1 calc R U . . .
H31C H 0.5977 0.2882 0.7212 0.052 Uiso 1 1 calc R U . . .
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'
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'
loop_
_exptl_crystal_face_index_h
_exptl_crystal_face_index_k
_exptl_crystal_face_index_l
_exptl_crystal_face_perp_dist
0 1 0 0.0300
0 -1 0 0.0100
5 -2 3 0.0780
-3 1 -1 0.0530
0 -1 5 0.0880
0 1 -5 0.0460
3 0 -4 0.0610
loop_
_geom_angle_atom_site_label_1
_geom_angle_atom_site_label_2
_geom_angle_atom_site_label_3
_geom_angle
_geom_angle_site_symmetry_1
_geom_angle_site_symmetry_3
_geom_angle_publ_flag
N1 C1 Fe1 130.6(5) . . ?
N1 C1 C2 127.9(7) . . ?
N1 C1 C5 124.4(7) . . ?
C2 C1 Fe1 68.1(4) . . ?
C5 C1 Fe1 68.0(4) . . ?
C5 C1 C2 107.7(7) . . ?
C1 Fe1 C1 123.7(5) . 2_665 ?
C2 Fe1 C1 40.0(3) . . ?
C2 Fe1 C1 156.8(3) . 2_665 ?
C2 Fe1 C1 40.0(3) 2_665 2_665 ?
C2 Fe1 C1 156.8(3) 2_665 . ?
C2 Fe1 C2 161.3(4) . 2_665 ?
C3 Fe1 C1 161.8(3) . 2_665 ?
C3 Fe1 C1 67.7(3) 2_665 2_665 ?
C3 Fe1 C1 161.8(3) 2_665 . ?
C3 Fe1 C1 67.7(3) . . ?
C3 Fe1 C2 123.9(3) 2_665 . ?
C3 Fe1 C2 41.0(3) 2_665 2_665 ?
C3 Fe1 C2 41.0(3) . . ?
C3 Fe1 C2 123.9(3) . 2_665 ?
C3 Fe1 C3 105.5(5) 2_665 . ?
C3 Fe1 C5 68.3(3) . . ?
C3 Fe1 C5 155.4(3) . 2_665 ?
C3 Fe1 C5 155.4(3) 2_665 . ?
C3 Fe1 C5 68.3(3) 2_665 2_665 ?
C4 Fe1 C1 67.8(3) 2_665 2_665 ?
C4 Fe1 C1 126.1(3) . 2_665 ?
C4 Fe1 C1 126.1(3) 2_665 . ?
C4 Fe1 C1 67.8(3) . . ?
C4 Fe1 C2 106.8(3) 2_665 . ?
C4 Fe1 C2 106.8(3) . 2_665 ?
C4 Fe1 C2 68.8(3) . . ?
C4 Fe1 C2 68.8(3) 2_665 2_665 ?
C4 Fe1 C3 40.9(3) . . ?
C4 Fe1 C3 119.0(3) . 2_665 ?
C4 Fe1 C3 119.0(3) 2_665 . ?
C4 Fe1 C3 40.9(3) 2_665 2_665 ?
C4 Fe1 C4 154.2(5) 2_665 . ?
C4 Fe1 C5 40.7(3) . . ?
C4 Fe1 C5 163.2(3) 2_665 . ?
C4 Fe1 C5 163.2(3) . 2_665 ?
C4 Fe1 C5 40.7(3) 2_665 2_665 ?
C5 Fe1 C1 110.3(3) . 2_665 ?
C5 Fe1 C1 110.3(3) 2_665 . ?
C5 Fe1 C1 39.8(3) 2_665 2_665 ?
C5 Fe1 C1 39.8(3) . . ?
C5 Fe1 C2 121.3(3) . 2_665 ?
C5 Fe1 C2 67.9(3) . . ?
C5 Fe1 C2 67.9(3) 2_665 2_665 ?
C5 Fe1 C2 121.3(3) 2_665 . ?
C5 Fe1 C5 127.1(5) 2_665 . ?
C1 N1 H1 111.7 . . ?
C1 N1 B1 136.7(7) . . ?
B1 N1 H1 111.7 . . ?
N1 B1 N3 133.3(8) . . ?
N2 B1 N1 121.4(8) . . ?
N2 B1 N3 105.3(7) . . ?
C1 C2 Fe1 71.9(4) . . ?
C1 C2 H2 126.1 . . ?
C1 C2 C3 107.8(7) . . ?
Fe1 C2 H2 124.7 . . ?
C3 C2 Fe1 68.9(4) . . ?
C3 C2 H2 126.1 . . ?
B1 N2 C8 128.7(6) . . ?
C6 N2 B1 108.4(7) . . ?
C6 N2 C8 122.9(6) . . ?
Fe1 C3 H3 126.0 . . ?
C2 C3 Fe1 70.1(4) . . ?
C2 C3 H3 126.0 . . ?
C4 C3 Fe1 69.4(4) . . ?
C4 C3 C2 107.9(7) . . ?
C4 C3 H3 126.0 . . ?
C7 N3 B1 106.5(6) . . ?
C7 N3 C20 118.1(6) . . ?
C20 N3 B1 134.5(7) . . ?
Fe1 C4 H4 125.5 . . ?
C3 C4 Fe1 69.7(4) . . ?
C3 C4 H4 126.2 . . ?
C5 C4 Fe1 70.2(4) . . ?
C5 C4 C3 107.5(7) . . ?
C5 C4 H4 126.2 . . ?
C1 C5 Fe1 72.2(4) . . ?
C1 C5 C4 108.9(7) . . ?
C1 C5 H5 125.5 . . ?
Fe1 C5 H5 124.8 . . ?
C4 C5 Fe1 69.1(5) . . ?
C4 C5 H5 125.5 . . ?
N2 C6 H6 125.0 . . ?
C7 C6 N2 109.9(7) . . ?
C7 C6 H6 125.0 . . ?
N3 C7 H7 125.0 . . ?
C6 C7 N3 109.9(7) . . ?
C6 C7 H7 125.0 . . ?
C9 C8 N2 118.6(6) . . ?
C9 C8 C13 122.5(7) . . ?
C13 C8 N2 118.9(7) . . ?
C8 C9 C10 117.9(7) . . ?
C8 C9 C14 122.7(7) . . ?
C10 C9 C14 119.4(7) . . ?
C9 C10 H10 119.9 . . ?
C11 C10 C9 120.1(8) . . ?
C11 C10 H10 119.9 . . ?
C10 C11 H11 119.2 . . ?
C12 C11 C10 121.7(8) . . ?
C12 C11 H11 119.2 . . ?
C11 C12 H12 119.4 . . ?
C11 C12 C13 121.2(7) . . ?
C13 C12 H12 119.4 . . ?
C8 C13 C17 121.2(7) . . ?
C12 C13 C8 116.6(7) . . ?
C12 C13 C17 122.1(7) . . ?
C9 C14 H14 108.1 . . ?
C9 C14 C16 111.8(7) . . ?
C15 C14 C9 109.8(7) . . ?
C15 C14 H14 108.1 . . ?
C15 C14 C16 110.7(7) . . ?
C16 C14 H14 108.1 . . ?
C14 C15 H15A 109.5 . . ?
C14 C15 H15B 109.5 . . ?
C14 C15 H15C 109.5 . . ?
H15A C15 H15B 109.5 . . ?
H15A C15 H15C 109.5 . . ?
H15B C15 H15C 109.5 . . ?
C14 C16 H16A 109.5 . . ?
C14 C16 H16B 109.5 . . ?
C14 C16 H16C 109.5 . . ?
H16A C16 H16B 109.5 . . ?
H16A C16 H16C 109.5 . . ?
H16B C16 H16C 109.5 . . ?
C13 C17 H17 107.4 . . ?
C13 C17 C18 112.7(8) . . ?
C13 C17 C19 110.8(8) . . ?
C18 C17 H17 107.4 . . ?
C19 C17 H17 107.4 . . ?
C19 C17 C18 110.8(8) . . ?
C17 C18 H18A 109.5 . . ?
C17 C18 H18B 109.5 . . ?
C17 C18 H18C 109.5 . . ?
H18A C18 H18B 109.5 . . ?
H18A C18 H18C 109.5 . . ?
H18B C18 H18C 109.5 . . ?
C17 C19 H19A 109.5 . . ?
C17 C19 H19B 109.5 . . ?
C17 C19 H19C 109.5 . . ?
H19A C19 H19B 109.5 . . ?
H19A C19 H19C 109.5 . . ?
H19B C19 H19C 109.5 . . ?
C21 C20 N3 117.3(7) . . ?
C25 C20 N3 120.4(6) . . ?
C25 C20 C21 122.4(7) . . ?
C20 C21 C26 122.5(7) . . ?
C22 C21 C20 117.8(7) . . ?
C22 C21 C26 119.7(7) . . ?
C21 C22 H22 118.9 . . ?
C23 C22 C21 122.1(7) . . ?
C23 C22 H22 118.9 . . ?
C22 C23 H23 120.8 . . ?
C22 C23 C24 118.5(8) . . ?
C24 C23 H23 120.8 . . ?
C23 C24 H24 119.5 . . ?
C25 C24 C23 121.1(8) . . ?
C25 C24 H24 119.5 . . ?
C20 C25 C24 118.2(7) . . ?
C20 C25 C29 120.8(7) . . ?
C24 C25 C29 121.0(7) . . ?
C21 C26 H26 107.1 . . ?
C21 C26 C27 109.6(6) . . ?
C21 C26 C28 114.0(7) . . ?
C27 C26 H26 107.1 . . ?
C28 C26 H26 107.1 . . ?
C28 C26 C27 111.6(7) . . ?
C26 C27 H27A 109.5 . . ?
C26 C27 H27B 109.5 . . ?
C26 C27 H27C 109.5 . . ?
H27A C27 H27B 109.5 . . ?
H27A C27 H27C 109.5 . . ?
H27B C27 H27C 109.5 . . ?
C26 C28 H28A 109.5 . . ?
C26 C28 H28B 109.5 . . ?
C26 C28 H28C 109.5 . . ?
H28A C28 H28B 109.5 . . ?
H28A C28 H28C 109.5 . . ?
H28B C28 H28C 109.5 . . ?
C25 C29 H29 107.6 . . ?
C30 C29 C25 110.5(6) . . ?
C30 C29 H29 107.6 . . ?
C31 C29 C25 113.4(7) . . ?
C31 C29 H29 107.6 . . ?
C31 C29 C30 109.9(7) . . ?
C29 C30 H30A 109.5 . . ?
C29 C30 H30B 109.5 . . ?
C29 C30 H30C 109.5 . . ?
H30A C30 H30B 109.5 . . ?
H30A C30 H30C 109.5 . . ?
H30B C30 H30C 109.5 . . ?
C29 C31 H31A 109.5 . . ?
C29 C31 H31B 109.5 . . ?
C29 C31 H31C 109.5 . . ?
H31A C31 H31B 109.5 . . ?
H31A C31 H31C 109.5 . . ?
H31B C31 H31C 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
C1 Fe1 2.096(8) . ?
C1 N1 1.402(10) . ?
C1 C2 1.419(12) . ?
C1 C5 1.410(11) . ?
Fe1 C1 2.096(8) 2_665 ?
Fe1 C2 2.046(7) . ?
Fe1 C2 2.046(7) 2_665 ?
Fe1 C3 2.030(7) 2_665 ?
Fe1 C3 2.030(7) . ?
Fe1 C4 2.027(7) 2_665 ?
Fe1 C4 2.027(8) . ?
Fe1 C5 2.041(7) 2_665 ?
Fe1 C5 2.041(7) . ?
N1 H1 0.8800 . ?
N1 B1 1.437(11) . ?
B1 N2 1.427(11) . ?
B1 N3 1.451(11) . ?
C2 H2 0.9500 . ?
C2 C3 1.427(10) . ?
N2 C6 1.398(10) . ?
N2 C8 1.442(10) . ?
C3 H3 0.9500 . ?
C3 C4 1.418(11) . ?
N3 C7 1.423(10) . ?
N3 C20 1.435(9) . ?
C4 H4 0.9500 . ?
C4 C5 1.415(11) . ?
C5 H5 0.9500 . ?
C6 H6 0.9500 . ?
C6 C7 1.325(11) . ?
C7 H7 0.9500 . ?
C8 C9 1.394(11) . ?
C8 C13 1.418(10) . ?
C9 C10 1.397(11) . ?
C9 C14 1.527(11) . ?
C10 H10 0.9500 . ?
C10 C11 1.380(11) . ?
C11 H11 0.9500 . ?
C11 C12 1.361(12) . ?
C12 H12 0.9500 . ?
C12 C13 1.400(11) . ?
C13 C17 1.508(11) . ?
C14 H14 1.0000 . ?
C14 C15 1.523(11) . ?
C14 C16 1.543(12) . ?
C15 H15A 0.9800 . ?
C15 H15B 0.9800 . ?
C15 H15C 0.9800 . ?
C16 H16A 0.9800 . ?
C16 H16B 0.9800 . ?
C16 H16C 0.9800 . ?
C17 H17 1.0000 . ?
C17 C18 1.549(13) . ?
C17 C19 1.525(14) . ?
C18 H18A 0.9800 . ?
C18 H18B 0.9800 . ?
C18 H18C 0.9800 . ?
C19 H19A 0.9800 . ?
C19 H19B 0.9800 . ?
C19 H19C 0.9800 . ?
C20 C21 1.396(10) . ?
C20 C25 1.390(10) . ?
C21 C22 1.390(11) . ?
C21 C26 1.524(11) . ?
C22 H22 0.9500 . ?
C22 C23 1.383(12) . ?
C23 H23 0.9500 . ?
C23 C24 1.410(11) . ?
C24 H24 0.9500 . ?
C24 C25 1.391(11) . ?
C25 C29 1.531(10) . ?
C26 H26 1.0000 . ?
C26 C27 1.534(12) . ?
C26 C28 1.525(11) . ?
C27 H27A 0.9800 . ?
C27 H27B 0.9800 . ?
C27 H27C 0.9800 . ?
C28 H28A 0.9800 . ?
C28 H28B 0.9800 . ?
C28 H28C 0.9800 . ?
C29 H29 1.0000 . ?
C29 C30 1.526(11) . ?
C29 C31 1.523(11) . ?
C30 H30A 0.9800 . ?
C30 H30B 0.9800 . ?
C30 H30C 0.9800 . ?
C31 H31A 0.9800 . ?
C31 H31B 0.9800 . ?
C31 H31C 0.9800 . ?
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
C1 N1 B1 N2 -165.9(8) . . . . ?
C1 N1 B1 N3 14.5(15) . . . . ?
C1 C2 C3 Fe1 61.7(5) . . . . ?
C1 C2 C3 C4 2.3(8) . . . . ?
Fe1 C1 N1 B1 -116.5(9) . . . . ?
Fe1 C1 C2 C3 -59.8(5) . . . . ?
Fe1 C1 C5 C4 59.6(5) . . . . ?
Fe1 C2 C3 C4 -59.4(5) . . . . ?
Fe1 C3 C4 C5 -60.3(5) . . . . ?
Fe1 C4 C5 C1 -61.5(5) . . . . ?
N1 C1 C2 Fe1 -125.1(8) . . . . ?
N1 C1 C2 C3 175.1(7) . . . . ?
N1 C1 C5 Fe1 125.0(7) . . . . ?
N1 C1 C5 C4 -175.4(7) . . . . ?
N1 B1 N2 C6 -179.6(7) . . . . ?
N1 B1 N2 C8 -0.4(12) . . . . ?
N1 B1 N3 C7 179.3(8) . . . . ?
N1 B1 N3 C20 11.1(15) . . . . ?
B1 N2 C6 C7 0.2(9) . . . . ?
B1 N2 C8 C9 -87.7(9) . . . . ?
B1 N2 C8 C13 92.7(9) . . . . ?
B1 N3 C7 C6 0.5(9) . . . . ?
B1 N3 C20 C21 93.0(10) . . . . ?
B1 N3 C20 C25 -88.1(11) . . . . ?
C2 C1 N1 B1 -24.0(14) . . . . ?
C2 C1 C5 Fe1 -56.6(5) . . . . ?
C2 C1 C5 C4 3.0(9) . . . . ?
C2 C3 C4 Fe1 59.8(5) . . . . ?
C2 C3 C4 C5 -0.5(9) . . . . ?
N2 B1 N3 C7 -0.4(8) . . . . ?
N2 B1 N3 C20 -168.6(7) . . . . ?
N2 C6 C7 N3 -0.4(9) . . . . ?
N2 C8 C9 C10 -178.4(6) . . . . ?
N2 C8 C9 C14 1.7(10) . . . . ?
N2 C8 C13 C12 179.6(7) . . . . ?
N2 C8 C13 C17 1.9(10) . . . . ?
C3 C4 C5 C1 -1.6(9) . . . . ?
C3 C4 C5 Fe1 59.9(5) . . . . ?
N3 B1 N2 C6 0.2(8) . . . . ?
N3 B1 N2 C8 179.4(6) . . . . ?
N3 C20 C21 C22 179.1(7) . . . . ?
N3 C20 C21 C26 -3.7(10) . . . . ?
N3 C20 C25 C24 -178.2(7) . . . . ?
N3 C20 C25 C29 2.8(11) . . . . ?
C5 C1 N1 B1 154.1(8) . . . . ?
C5 C1 C2 Fe1 56.5(5) . . . . ?
C5 C1 C2 C3 -3.3(8) . . . . ?
C6 N2 C8 C9 91.4(9) . . . . ?
C6 N2 C8 C13 -88.2(9) . . . . ?
C7 N3 C20 C21 -74.3(9) . . . . ?
C7 N3 C20 C25 104.7(8) . . . . ?
C8 N2 C6 C7 -179.1(7) . . . . ?
C8 C9 C10 C11 -1.4(11) . . . . ?
C8 C9 C14 C15 105.1(9) . . . . ?
C8 C9 C14 C16 -131.6(8) . . . . ?
C8 C13 C17 C18 -142.8(8) . . . . ?
C8 C13 C17 C19 92.4(9) . . . . ?
C9 C8 C13 C12 0.0(11) . . . . ?
C9 C8 C13 C17 -177.7(7) . . . . ?
C9 C10 C11 C12 0.5(12) . . . . ?
C10 C9 C14 C15 -74.7(9) . . . . ?
C10 C9 C14 C16 48.6(10) . . . . ?
C10 C11 C12 C13 0.7(13) . . . . ?
C11 C12 C13 C8 -1.0(11) . . . . ?
C11 C12 C13 C17 176.7(8) . . . . ?
C12 C13 C17 C18 39.6(12) . . . . ?
C12 C13 C17 C19 -85.2(10) . . . . ?
C13 C8 C9 C10 1.2(11) . . . . ?
C13 C8 C9 C14 -178.7(7) . . . . ?
C14 C9 C10 C11 178.4(7) . . . . ?
C20 N3 C7 C6 171.0(7) . . . . ?
C20 C21 C22 C23 -0.6(11) . . . . ?
C20 C21 C26 C27 -91.1(8) . . . . ?
C20 C21 C26 C28 143.0(7) . . . . ?
C20 C25 C29 C30 -82.3(9) . . . . ?
C20 C25 C29 C31 153.9(7) . . . . ?
C21 C20 C25 C24 0.7(11) . . . . ?
C21 C20 C25 C29 -178.3(6) . . . . ?
C21 C22 C23 C24 0.1(12) . . . . ?
C22 C21 C26 C27 86.0(8) . . . . ?
C22 C21 C26 C28 -39.8(10) . . . . ?
C22 C23 C24 C25 0.8(12) . . . . ?
C23 C24 C25 C20 -1.2(11) . . . . ?
C23 C24 C25 C29 177.9(7) . . . . ?
C24 C25 C29 C30 98.8(9) . . . . ?
C24 C25 C29 C31 -25.1(10) . . . . ?
C25 C20 C21 C22 0.2(11) . . . . ?
C25 C20 C21 C26 177.3(6) . . . . ?
C26 C21 C22 C23 -177.8(7) . . . . ?
loop_
_twin_individual_id
_twin_individual_mass_fraction_refined
1 0.638(15)
2 0.362(15)
