#------------------------------------------------------------------------------
#$Date: 2024-10-06 11:08:38 +0300 (Sun, 06 Oct 2024) $
#$Revision: 295269 $
#$URL: file:///home/coder/svn-repositories/cod/cif/7/71/68/7716844.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_7716844
loop_
_publ_author_name
'Hudson, Luke A.'
'Stroek, Wowa'
'Albrecht, Martin'
_publ_section_title
;
 Tailoring C-H amination activity via modification of the
 triazole-derived carbene ligand.
;
_journal_issue                   35
_journal_name_full
'Dalton transactions (Cambridge, England : 2003)'
_journal_page_first              14795
_journal_page_last               14800
_journal_paper_doi               10.1039/d4dt01715c
_journal_volume                  53
_journal_year                    2024
_chemical_formula_moiety         'C42 H48 Fe N6 O2'
_chemical_formula_sum            'C42 H48 Fe N6 O2'
_chemical_formula_weight         724.71
_space_group_crystal_system      monoclinic
_space_group_IT_number           14
_space_group_name_Hall           '-P 2yn'
_space_group_name_H-M_alt        'P 1 21/n 1'
_atom_sites_solution_hydrogens   geom
_audit_creation_date             2024-05-16
_audit_creation_method
;
Olex2 1.5
(compiled 2024.01.12 svn.r2f8d729c for OlexSys, GUI svn.r6928)
;
_audit_update_record
;
2024-06-07 deposited with the CCDC.	2024-08-12 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 95.8494(19)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   10.1907(2)
_cell_length_b                   24.2458(4)
_cell_length_c                   15.4249(3)
_cell_measurement_reflns_used    42537
_cell_measurement_temperature    173.01(10)
_cell_measurement_theta_max      33.161
_cell_measurement_theta_min      2.127
_cell_volume                     3791.37(12)
_computing_cell_refinement       'CrysAlisPro 1.171.42.94a (Rigaku OD, 2023)'
_computing_data_collection       'CrysAlisPro 1.171.42.94a (Rigaku OD, 2023)'
_computing_data_reduction        'CrysAlisPro 1.171.42.94a (Rigaku OD, 2023)'
_computing_molecular_graphics    'Olex2 1.5 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 1.5 (Dolomanov et al., 2009)'
_computing_structure_refinement  'SHELXL 2019/3 (Sheldrick, 2015)'
_computing_structure_solution    'SHELXT  (Sheldrick, 2015)'
_diffrn_ambient_temperature      173.15
_diffrn_detector_area_resol_mean 10
_diffrn_detector_type            'HyPix-Arc 100'
_diffrn_measured_fraction_theta_full 1.000
_diffrn_measured_fraction_theta_max 0.995
_diffrn_measurement_details
;
List of Runs (angles in degrees, time in seconds):

  # Type    Start    End  Width  tₑₓₚ   ω     θ     κ     φ   Frames
#--------------------------------------------------------------------------
  1  ω    -11.00  87.00   0.50    8.00    --   13.03  66.00 -38.00  196
  2  ω    -61.00  37.00   0.50    8.00    --   13.03 -66.00-173.00  196
  3  ω    -16.00  83.00   0.50    8.00    --   13.03  77.00 120.00  198
  4  ω    -25.00  68.00   0.50    8.00    --  -13.50  19.00  90.00  186
  5  ω    -19.00  29.00   0.50    8.00    --  -13.50 -99.00 -30.00   96
  6  ω    -19.00  29.00   0.50    8.00    --  -13.50 -99.00  60.00   96
  7  ω    -87.00 -42.00   0.50    8.00    --  -13.50-178.00 -60.00   90
  8  ω    -56.00  42.00   0.50    8.00    --   13.03 -77.00   0.00  196
  9  ω    -18.00  54.00   0.50    8.00    --   13.03 -99.00 -90.00  144
 10  ω    -18.00  54.00   0.50    8.00    --   13.03 -99.00 120.00  144
 11  ω    -19.00  22.00   0.50    8.00    --  -13.50 -99.00 150.00   82
 12  ω    -89.00 -40.00   0.50    8.00    --  -13.50 178.00-150.00   98
;
_diffrn_measurement_device       'four-circle diffractometer'
_diffrn_measurement_device_type  'XtaLAB Synergy R, HyPix-Arc 100'
_diffrn_measurement_method       'ω scans'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_unetI/netI     0.0405
_diffrn_reflns_Laue_measured_fraction_full 1.000
_diffrn_reflns_Laue_measured_fraction_max 0.995
_diffrn_reflns_limit_h_max       14
_diffrn_reflns_limit_h_min       -14
_diffrn_reflns_limit_k_max       34
_diffrn_reflns_limit_k_min       -34
_diffrn_reflns_limit_l_max       21
_diffrn_reflns_limit_l_min       -21
_diffrn_reflns_number            21589
_diffrn_reflns_point_group_measured_fraction_full 1.000
_diffrn_reflns_point_group_measured_fraction_max 0.995
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         30.527
_diffrn_reflns_theta_min         2.141
_exptl_absorpt_coefficient_mu    0.442
_exptl_absorpt_correction_T_max  0.973
_exptl_absorpt_correction_T_min  0.957
_exptl_absorpt_correction_type   gaussian
_exptl_absorpt_process_details
;
        CrysAlisPro 1.171.42.94a (Rigaku Oxford Diffraction, 2023)
        Numerical absorption correction based on gaussian integration over
        a multifaceted crystal model
        Empirical absorption correction using spherical harmonics,
        implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_crystal_colour            orange
_exptl_crystal_colour_primary    orange
_exptl_crystal_density_diffrn    1.270
_exptl_crystal_description       block
_exptl_crystal_F_000             1536
_exptl_crystal_size_max          0.156
_exptl_crystal_size_mid          0.096
_exptl_crystal_size_min          0.087
_refine_diff_density_max         0.342
_refine_diff_density_min         -0.296
_refine_diff_density_rms         0.050
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.028
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     471
_refine_ls_number_reflns         21589
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.028
_refine_ls_R_factor_all          0.0655
_refine_ls_R_factor_gt           0.0415
_refine_ls_shift/su_max          0.001
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[σ²(Fo²)+(0.0540P)²] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0936
_refine_ls_wR_factor_ref         0.0992
_reflns_Friedel_coverage         0.000
_reflns_number_gt                15592
_reflns_number_total             21589
_reflns_threshold_expression     'I > 2σ(I)'
_twin_special_details
;
Component 2 rotated by -179.9719° 
around [1.00 0.00 0.00] (reciprocal) or [1.00 0.00 0.07] (direct)
;
_cod_data_source_file            d4dt01715c2.cif
_cod_data_source_block           23ma017_lah065
_cod_depositor_comments
'Adding full bibliography for 7716844--7716845.cif.'
_cod_original_cell_volume        3791.39(13)
_cod_database_code               7716844
_shelx_shelxl_version_number     2019/3
_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.
;
_shelx_estimated_absorpt_t_max   0.963
_shelx_estimated_absorpt_t_min   0.934
_olex2_refinement_description
;
1. Twinned data refinement
 Scales: 0.6646(5)
 0.3354(5)
2. Fixed Uiso
 At 1.2 times of:
  All C(H) groups
 At 1.5 times of:
  All C(H,H,H) groups
3.a Ternary CH refined with riding coordinates:
 C16(H16), C40(H40), C19(H19), C37(H37)
3.b Aromatic/amide H refined with riding coordinates:
 C26(H26), C2(H2), C23(H23), C25(H25), C12(H12), C5(H5), C35(H35), C24(H24),
 C4(H4), C3(H3), C33(H33), C14(H14), C34(H34), C13(H13)
3.c Idealised Me refined as rotating group:
 C30(H30A,H30B,H30C), C9(H9A,H9B,H9C), C17(H17A,H17B,H17C), C18(H18A,H18B,
 H18C), C42(H42A,H42B,H42C), C38(H38A,H38B,H38C), C39(H39A,H39B,H39C), C41(H41A,
 H41B,H41C), C21(H21A,H21B,H21C), C20(H20A,H20B,H20C)
;
_olex2_submission_special_instructions 'No special instructions were received'
_oxdiff_exptl_absorpt_empirical_details
;
Empirical correction (ABSPACK) includes:
- Absorption correction using spherical harmonics
- Frame scaling
;
loop_
_space_group_symop_operation_xyz
'x, y, z'
'-x+1/2, y+1/2, -z+1/2'
'-x, -y, -z'
'x-1/2, -y-1/2, 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
Fe1 Fe 0.14695(2) 0.74456(2) 0.50930(2) 0.02383(6) Uani 1 1 d . . . . .
O2 O 0.06876(10) 0.79866(4) 0.42639(7) 0.0295(2) Uani 1 1 d . . . . .
O1 O 0.05949(10) 0.68979(4) 0.57488(7) 0.0300(2) Uani 1 1 d . . . . .
N4 N 0.35589(11) 0.72105(4) 0.29276(7) 0.0236(2) Uani 1 1 d . . . . .
N6 N 0.32688(11) 0.66953(4) 0.39725(7) 0.0242(2) Uani 1 1 d . . . . .
N3 N 0.27727(11) 0.82758(4) 0.65440(7) 0.0228(2) Uani 1 1 d . . . . .
N5 N 0.38087(12) 0.67005(4) 0.32162(8) 0.0257(3) Uani 1 1 d . . . . .
N1 N 0.28576(12) 0.78013(5) 0.76749(8) 0.0269(3) Uani 1 1 d . . . . .
N2 N 0.30858(12) 0.83096(5) 0.74083(8) 0.0283(3) Uani 1 1 d . . . . .
C29 C 0.26749(14) 0.71728(5) 0.41876(9) 0.0242(3) Uani 1 1 d . . . . .
C28 C 0.28854(13) 0.75167(5) 0.34850(9) 0.0223(3) Uani 1 1 d . . . . .
C22 C 0.13803(14) 0.82938(5) 0.37606(9) 0.0261(3) Uani 1 1 d . . . . .
C27 C 0.24824(14) 0.80955(5) 0.33565(9) 0.0252(3) Uani 1 1 d . . . . .
C8 C 0.23461(13) 0.77730(5) 0.62370(9) 0.0234(3) Uani 1 1 d . . . . .
C31 C 0.33591(15) 0.61912(5) 0.44824(9) 0.0264(3) Uani 1 1 d . . . . .
C10 C 0.28694(14) 0.87780(5) 0.60472(9) 0.0239(3) Uani 1 1 d . . . . .
C7 C 0.24200(13) 0.74564(5) 0.70008(9) 0.0233(3) Uani 1 1 d . . . . .
C11 C 0.18930(14) 0.91767(5) 0.60991(9) 0.0262(3) Uani 1 1 d . . . . .
C1 C 0.11608(14) 0.66279(5) 0.64364(9) 0.0269(3) Uani 1 1 d . . . . .
C16 C 0.07394(14) 0.90951(6) 0.66346(10) 0.0303(3) Uani 1 1 d . . . . .
H16 H 0.076566 0.870420 0.684240 0.036 Uiso 1 1 calc R U . . .
C36 C 0.23483(15) 0.58010(5) 0.43224(9) 0.0293(3) Uani 1 1 d . . . . .
C6 C 0.20773(14) 0.68713(5) 0.70830(9) 0.0265(3) Uani 1 1 d . . . . .
C32 C 0.44181(15) 0.61302(6) 0.51172(10) 0.0322(3) Uani 1 1 d . . . . .
C40 C 0.11993(16) 0.58731(6) 0.36309(10) 0.0321(3) Uani 1 1 d . . . . .
H40 H 0.126914 0.624806 0.336944 0.039 Uiso 1 1 calc R U . . .
C15 C 0.39265(14) 0.88345(6) 0.55411(10) 0.0282(3) Uani 1 1 d . . . . .
C30 C 0.39876(15) 0.73472(6) 0.20758(10) 0.0284(3) Uani 1 1 d . . . . .
H30A H 0.484665 0.753200 0.215680 0.043 Uiso 1 1 calc R U . . .
H30B H 0.333955 0.759297 0.176185 0.043 Uiso 1 1 calc R U . . .
H30C H 0.406349 0.700822 0.173851 0.043 Uiso 1 1 calc R U . . .
C26 C 0.31935(16) 0.84649(6) 0.28813(10) 0.0307(3) Uani 1 1 d . . . . .
H26 H 0.395857 0.833786 0.263849 0.037 Uiso 1 1 calc R U . . .
C2 C 0.08274(16) 0.60696(6) 0.65503(11) 0.0346(3) Uani 1 1 d . . . . .
H2 H 0.018966 0.590170 0.614131 0.041 Uiso 1 1 calc R U . . .
C23 C 0.10048(16) 0.88473(6) 0.36088(10) 0.0333(3) Uani 1 1 d . . . . .
H23 H 0.025345 0.898546 0.385540 0.040 Uiso 1 1 calc R U . . .
C19 C 0.49725(15) 0.83897(6) 0.55345(10) 0.0345(3) Uani 1 1 d . . . . .
H19 H 0.451507 0.802425 0.549934 0.041 Uiso 1 1 calc R U . . .
C25 C 0.28114(17) 0.90061(6) 0.27581(11) 0.0386(4) Uani 1 1 d . . . . .
H25 H 0.330555 0.924895 0.243337 0.046 Uiso 1 1 calc R U . . .
C37 C 0.55036(16) 0.65599(6) 0.52889(11) 0.0370(4) Uani 1 1 d . . . . .
H37 H 0.537408 0.684642 0.482163 0.044 Uiso 1 1 calc R U . . .
C12 C 0.20189(16) 0.96631(6) 0.56311(11) 0.0346(4) Uani 1 1 d . . . . .
H12 H 0.138720 0.994904 0.565937 0.041 Uiso 1 1 calc R U . . .
C5 C 0.26705(16) 0.65422(6) 0.77604(10) 0.0339(3) Uani 1 1 d . . . . .
H5 H 0.331798 0.670028 0.817341 0.041 Uiso 1 1 calc R U . . .
C35 C 0.24534(17) 0.53273(6) 0.48357(11) 0.0367(4) Uani 1 1 d . . . . .
H35 H 0.180119 0.504781 0.474133 0.044 Uiso 1 1 calc R U . . .
C24 C 0.16945(18) 0.91931(6) 0.31141(11) 0.0392(4) Uani 1 1 d . . . . .
H24 H 0.140568 0.956234 0.301495 0.047 Uiso 1 1 calc R U . . .
C4 C 0.23372(17) 0.59945(6) 0.78420(12) 0.0408(4) Uani 1 1 d . . . . .
H4 H 0.274602 0.577916 0.830831 0.049 Uiso 1 1 calc R U . . .
C3 C 0.13991(18) 0.57616(6) 0.72362(12) 0.0411(4) Uani 1 1 d . . . . .
H3 H 0.115010 0.538694 0.729553 0.049 Uiso 1 1 calc R U . . .
C33 C 0.44518(17) 0.56515(7) 0.56192(11) 0.0404(4) Uani 1 1 d . . . . .
H33 H 0.515271 0.559693 0.606603 0.048 Uiso 1 1 calc R U . . .
C14 C 0.39870(16) 0.93256(6) 0.50801(11) 0.0369(4) Uani 1 1 d . . . . .
H14 H 0.468534 0.938148 0.472598 0.044 Uiso 1 1 calc R U . . .
C9 C 0.30213(19) 0.77112(7) 0.86190(10) 0.0398(4) Uani 1 1 d . . . . .
H9A H 0.384190 0.750833 0.877930 0.060 Uiso 1 1 calc R U . . .
H9B H 0.227345 0.749725 0.878990 0.060 Uiso 1 1 calc R U . . .
H9C H 0.305793 0.806795 0.891931 0.060 Uiso 1 1 calc R U . . .
C34 C 0.34798(18) 0.52555(6) 0.54757(12) 0.0424(4) Uani 1 1 d . . . . .
H34 H 0.352117 0.493083 0.582224 0.051 Uiso 1 1 calc R U . . .
C13 C 0.30504(17) 0.97334(6) 0.51278(12) 0.0399(4) Uani 1 1 d . . . . .
H13 H 0.311757 1.006620 0.481026 0.048 Uiso 1 1 calc R U . . .
C17 C 0.08669(18) 0.94665(7) 0.74387(11) 0.0467(4) Uani 1 1 d . . . . .
H17A H 0.170454 0.939024 0.778867 0.070 Uiso 1 1 calc R U . . .
H17B H 0.013400 0.939381 0.778754 0.070 Uiso 1 1 calc R U . . .
H17C H 0.084395 0.985374 0.725564 0.070 Uiso 1 1 calc R U . . .
C18 C -0.05776(17) 0.91823(8) 0.60922(13) 0.0509(5) Uani 1 1 d . . . . .
H18A H -0.063355 0.956315 0.587883 0.076 Uiso 1 1 calc R U . . .
H18B H -0.129788 0.911194 0.645276 0.076 Uiso 1 1 calc R U . . .
H18C H -0.064929 0.892798 0.559583 0.076 Uiso 1 1 calc R U . . .
C42 C -0.01213(17) 0.58396(8) 0.40192(12) 0.0478(4) Uani 1 1 d . . . . .
H42A H -0.022117 0.547232 0.426950 0.072 Uiso 1 1 calc R U . . .
H42B H -0.084232 0.590596 0.356049 0.072 Uiso 1 1 calc R U . . .
H42C H -0.014630 0.611902 0.447625 0.072 Uiso 1 1 calc R U . . .
C38 C 0.68814(17) 0.63081(8) 0.52606(13) 0.0469(4) Uani 1 1 d . . . . .
H38A H 0.754884 0.659915 0.534870 0.070 Uiso 1 1 calc R U . . .
H38B H 0.693654 0.613314 0.469275 0.070 Uiso 1 1 calc R U . . .
H38C H 0.703792 0.603117 0.572245 0.070 Uiso 1 1 calc R U . . .
C39 C 0.53921(18) 0.68419(8) 0.61637(13) 0.0492(5) Uani 1 1 d . . . . .
H39A H 0.550801 0.656763 0.663194 0.074 Uiso 1 1 calc R U . . .
H39B H 0.452053 0.701322 0.615972 0.074 Uiso 1 1 calc R U . . .
H39C H 0.607606 0.712563 0.626066 0.074 Uiso 1 1 calc R U . . .
C41 C 0.1257(2) 0.54485(7) 0.29051(12) 0.0523(5) Uani 1 1 d . . . . .
H41A H 0.209743 0.548357 0.265273 0.079 Uiso 1 1 calc R U . . .
H41B H 0.052702 0.551251 0.245175 0.079 Uiso 1 1 calc R U . . .
H41C H 0.118338 0.507676 0.314493 0.079 Uiso 1 1 calc R U . . .
C21 C 0.58031(19) 0.84289(9) 0.47703(13) 0.0571(5) Uani 1 1 d . . . . .
H21A H 0.522264 0.843735 0.422339 0.086 Uiso 1 1 calc R U . . .
H21B H 0.638792 0.810790 0.477270 0.086 Uiso 1 1 calc R U . . .
H21C H 0.633346 0.876665 0.482307 0.086 Uiso 1 1 calc R U . . .
C20 C 0.58949(18) 0.84026(8) 0.63844(12) 0.0511(5) Uani 1 1 d . . . . .
H20A H 0.634723 0.875945 0.643895 0.077 Uiso 1 1 calc R U . . .
H20B H 0.654857 0.810656 0.637709 0.077 Uiso 1 1 calc R U . . .
H20C H 0.537845 0.834990 0.688027 0.077 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 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Fe Fe 0.3463 0.8444 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
loop_
_exptl_crystal_face_index_h
_exptl_crystal_face_index_k
_exptl_crystal_face_index_l
_exptl_crystal_face_perp_dist
1 0 0 0.0466
-1 0 0 0.0449
-1 -1 -1 0.0546
1 1 1 0.0751
1 -1 0 0.0325
1 -1 1 0.0483
-1 1 -1 0.047
0 -1 -1 0.085
0 0 -1 0.0794
0 0 1 0.0539
0 -1 1 0.0448
0 1 0 0.0539
0 -1 0 0.0505
1 1 -1 0.0494
-1 -1 1 0.0464
-1 0 1 0.037
1 0 -1 0.0497
1 1 0 0.0627
-1 -1 0 0.0401
1 -1 -1 0.0553
2 24 -16 0.0467
6 -29 5 0.0371
5 -19 15 0.0414
7 28 -7 0.0577
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
O2 Fe1 C29 90.19(5) . . ?
O2 Fe1 C8 114.66(5) . . ?
O1 Fe1 O2 128.70(4) . . ?
O1 Fe1 C29 118.10(5) . . ?
O1 Fe1 C8 89.96(5) . . ?
C8 Fe1 C29 117.97(5) . . ?
C22 O2 Fe1 123.74(9) . . ?
C1 O1 Fe1 124.68(9) . . ?
N5 N4 C28 112.61(11) . . ?
N5 N4 C30 116.51(11) . . ?
C28 N4 C30 130.84(11) . . ?
N5 N6 C29 115.84(11) . . ?
N5 N6 C31 118.09(10) . . ?
C29 N6 C31 126.07(11) . . ?
N2 N3 C8 115.79(11) . . ?
N2 N3 C10 116.91(10) . . ?
C8 N3 C10 127.24(11) . . ?
N4 N5 N6 102.63(10) . . ?
N2 N1 C7 112.61(11) . . ?
N2 N1 C9 116.14(12) . . ?
C7 N1 C9 131.10(12) . . ?
N1 N2 N3 102.70(10) . . ?
N6 C29 Fe1 138.39(10) . . ?
N6 C29 C28 102.15(11) . . ?
C28 C29 Fe1 118.82(9) . . ?
N4 C28 C29 106.77(11) . . ?
N4 C28 C27 125.66(12) . . ?
C29 C28 C27 127.57(12) . . ?
O2 C22 C27 123.81(12) . . ?
O2 C22 C23 118.64(13) . . ?
C23 C22 C27 117.55(13) . . ?
C22 C27 C28 119.07(12) . . ?
C26 C27 C28 121.82(13) . . ?
C26 C27 C22 119.04(12) . . ?
N3 C8 Fe1 137.68(10) . . ?
N3 C8 C7 102.12(12) . . ?
C7 C8 Fe1 119.45(9) . . ?
C36 C31 N6 117.91(13) . . ?
C32 C31 N6 118.26(12) . . ?
C32 C31 C36 123.80(13) . . ?
C11 C10 N3 117.71(12) . . ?
C11 C10 C15 123.92(13) . . ?
C15 C10 N3 118.37(12) . . ?
N1 C7 C8 106.77(11) . . ?
N1 C7 C6 125.75(13) . . ?
C8 C7 C6 127.47(13) . . ?
C10 C11 C16 122.53(12) . . ?
C10 C11 C12 116.88(13) . . ?
C12 C11 C16 120.59(13) . . ?
O1 C1 C6 123.78(12) . . ?
O1 C1 C2 118.83(14) . . ?
C2 C1 C6 117.37(14) . . ?
C11 C16 H16 107.5 . . ?
C11 C16 C17 111.02(13) . . ?
C11 C16 C18 111.81(14) . . ?
C17 C16 H16 107.5 . . ?
C18 C16 H16 107.5 . . ?
C18 C16 C17 111.20(14) . . ?
C31 C36 C40 123.28(12) . . ?
C35 C36 C31 116.35(14) . . ?
C35 C36 C40 120.37(13) . . ?
C1 C6 C7 118.99(13) . . ?
C5 C6 C7 121.71(14) . . ?
C5 C6 C1 119.25(13) . . ?
C31 C32 C37 123.23(13) . . ?
C31 C32 C33 116.98(14) . . ?
C33 C32 C37 119.78(14) . . ?
C36 C40 H40 107.9 . . ?
C36 C40 C42 111.51(13) . . ?
C36 C40 C41 110.77(13) . . ?
C42 C40 H40 107.9 . . ?
C41 C40 H40 107.9 . . ?
C41 C40 C42 110.64(14) . . ?
C10 C15 C19 121.02(13) . . ?
C14 C15 C10 116.44(13) . . ?
C14 C15 C19 122.49(14) . . ?
N4 C30 H30A 109.5 . . ?
N4 C30 H30B 109.5 . . ?
N4 C30 H30C 109.5 . . ?
H30A C30 H30B 109.5 . . ?
H30A C30 H30C 109.5 . . ?
H30B C30 H30C 109.5 . . ?
C27 C26 H26 119.1 . . ?
C25 C26 C27 121.75(15) . . ?
C25 C26 H26 119.1 . . ?
C1 C2 H2 119.1 . . ?
C3 C2 C1 121.89(15) . . ?
C3 C2 H2 119.1 . . ?
C22 C23 H23 119.1 . . ?
C24 C23 C22 121.86(15) . . ?
C24 C23 H23 119.1 . . ?
C15 C19 H19 107.8 . . ?
C15 C19 C21 114.03(14) . . ?
C15 C19 C20 110.46(13) . . ?
C21 C19 H19 107.8 . . ?
C21 C19 C20 108.65(15) . . ?
C20 C19 H19 107.8 . . ?
C26 C25 H25 120.4 . . ?
C26 C25 C24 119.22(14) . . ?
C24 C25 H25 120.4 . . ?
C32 C37 H37 108.0 . . ?
C32 C37 C38 111.90(14) . . ?
C32 C37 C39 109.98(14) . . ?
C38 C37 H37 108.0 . . ?
C39 C37 H37 108.0 . . ?
C39 C37 C38 110.71(14) . . ?
C11 C12 H12 119.6 . . ?
C13 C12 C11 120.73(14) . . ?
C13 C12 H12 119.6 . . ?
C6 C5 H5 119.2 . . ?
C4 C5 C6 121.63(15) . . ?
C4 C5 H5 119.2 . . ?
C36 C35 H35 119.3 . . ?
C34 C35 C36 121.44(15) . . ?
C34 C35 H35 119.3 . . ?
C23 C24 C25 120.43(14) . . ?
C23 C24 H24 119.8 . . ?
C25 C24 H24 119.8 . . ?
C5 C4 H4 120.3 . . ?
C5 C4 C3 119.32(15) . . ?
C3 C4 H4 120.3 . . ?
C2 C3 C4 120.40(14) . . ?
C2 C3 H3 119.8 . . ?
C4 C3 H3 119.8 . . ?
C32 C33 H33 119.6 . . ?
C34 C33 C32 120.89(16) . . ?
C34 C33 H33 119.6 . . ?
C15 C14 H14 119.4 . . ?
C13 C14 C15 121.23(15) . . ?
C13 C14 H14 119.4 . . ?
N1 C9 H9A 109.5 . . ?
N1 C9 H9B 109.5 . . ?
N1 C9 H9C 109.5 . . ?
H9A C9 H9B 109.5 . . ?
H9A C9 H9C 109.5 . . ?
H9B C9 H9C 109.5 . . ?
C35 C34 C33 120.52(14) . . ?
C35 C34 H34 119.7 . . ?
C33 C34 H34 119.7 . . ?
C12 C13 C14 120.78(14) . . ?
C12 C13 H13 119.6 . . ?
C14 C13 H13 119.6 . . ?
C16 C17 H17A 109.5 . . ?
C16 C17 H17B 109.5 . . ?
C16 C17 H17C 109.5 . . ?
H17A C17 H17B 109.5 . . ?
H17A C17 H17C 109.5 . . ?
H17B C17 H17C 109.5 . . ?
C16 C18 H18A 109.5 . . ?
C16 C18 H18B 109.5 . . ?
C16 C18 H18C 109.5 . . ?
H18A C18 H18B 109.5 . . ?
H18A C18 H18C 109.5 . . ?
H18B C18 H18C 109.5 . . ?
C40 C42 H42A 109.5 . . ?
C40 C42 H42B 109.5 . . ?
C40 C42 H42C 109.5 . . ?
H42A C42 H42B 109.5 . . ?
H42A C42 H42C 109.5 . . ?
H42B C42 H42C 109.5 . . ?
C37 C38 H38A 109.5 . . ?
C37 C38 H38B 109.5 . . ?
C37 C38 H38C 109.5 . . ?
H38A C38 H38B 109.5 . . ?
H38A C38 H38C 109.5 . . ?
H38B C38 H38C 109.5 . . ?
C37 C39 H39A 109.5 . . ?
C37 C39 H39B 109.5 . . ?
C37 C39 H39C 109.5 . . ?
H39A C39 H39B 109.5 . . ?
H39A C39 H39C 109.5 . . ?
H39B C39 H39C 109.5 . . ?
C40 C41 H41A 109.5 . . ?
C40 C41 H41B 109.5 . . ?
C40 C41 H41C 109.5 . . ?
H41A C41 H41B 109.5 . . ?
H41A C41 H41C 109.5 . . ?
H41B C41 H41C 109.5 . . ?
C19 C21 H21A 109.5 . . ?
C19 C21 H21B 109.5 . . ?
C19 C21 H21C 109.5 . . ?
H21A C21 H21B 109.5 . . ?
H21A C21 H21C 109.5 . . ?
H21B C21 H21C 109.5 . . ?
C19 C20 H20A 109.5 . . ?
C19 C20 H20B 109.5 . . ?
C19 C20 H20C 109.5 . . ?
H20A C20 H20B 109.5 . . ?
H20A C20 H20C 109.5 . . ?
H20B C20 H20C 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 O2 1.9451(10) . ?
Fe1 O1 1.9402(10) . ?
Fe1 C29 2.0607(14) . ?
Fe1 C8 2.0544(14) . ?
O2 C22 1.3295(17) . ?
O1 C1 1.3272(18) . ?
N4 N5 1.3299(15) . ?
N4 C28 1.3718(17) . ?
N4 C30 1.4644(18) . ?
N6 N5 1.3397(16) . ?
N6 C29 1.3629(16) . ?
N6 C31 1.4512(16) . ?
N3 N2 1.3414(16) . ?
N3 C8 1.3629(17) . ?
N3 C10 1.4474(17) . ?
N1 N2 1.3273(16) . ?
N1 C7 1.3729(18) . ?
N1 C9 1.465(2) . ?
C29 C28 1.4011(18) . ?
C28 C27 1.4698(18) . ?
C22 C27 1.423(2) . ?
C22 C23 1.4085(19) . ?
C27 C26 1.405(2) . ?
C8 C7 1.4017(19) . ?
C31 C36 1.402(2) . ?
C31 C32 1.389(2) . ?
C10 C11 1.3953(19) . ?
C10 C15 1.400(2) . ?
C7 C6 1.4695(18) . ?
C11 C16 1.517(2) . ?
C11 C12 1.396(2) . ?
C1 C6 1.423(2) . ?
C1 C2 1.411(2) . ?
C16 H16 1.0000 . ?
C16 C17 1.528(2) . ?
C16 C18 1.522(2) . ?
C36 C40 1.512(2) . ?
C36 C35 1.393(2) . ?
C6 C5 1.402(2) . ?
C32 C37 1.523(2) . ?
C32 C33 1.394(2) . ?
C40 H40 1.0000 . ?
C40 C42 1.530(2) . ?
C40 C41 1.526(2) . ?
C15 C19 1.517(2) . ?
C15 C14 1.392(2) . ?
C30 H30A 0.9800 . ?
C30 H30B 0.9800 . ?
C30 H30C 0.9800 . ?
C26 H26 0.9500 . ?
C26 C25 1.376(2) . ?
C2 H2 0.9500 . ?
C2 C3 1.375(2) . ?
C23 H23 0.9500 . ?
C23 C24 1.374(2) . ?
C19 H19 1.0000 . ?
C19 C21 1.523(2) . ?
C19 C20 1.534(2) . ?
C25 H25 0.9500 . ?
C25 C24 1.389(2) . ?
C37 H37 1.0000 . ?
C37 C38 1.536(2) . ?
C37 C39 1.527(2) . ?
C12 H12 0.9500 . ?
C12 C13 1.380(2) . ?
C5 H5 0.9500 . ?
C5 C4 1.380(2) . ?
C35 H35 0.9500 . ?
C35 C34 1.374(2) . ?
C24 H24 0.9500 . ?
C4 H4 0.9500 . ?
C4 C3 1.387(3) . ?
C3 H3 0.9500 . ?
C33 H33 0.9500 . ?
C33 C34 1.381(2) . ?
C14 H14 0.9500 . ?
C14 C13 1.381(2) . ?
C9 H9A 0.9800 . ?
C9 H9B 0.9800 . ?
C9 H9C 0.9800 . ?
C34 H34 0.9500 . ?
C13 H13 0.9500 . ?
C17 H17A 0.9800 . ?
C17 H17B 0.9800 . ?
C17 H17C 0.9800 . ?
C18 H18A 0.9800 . ?
C18 H18B 0.9800 . ?
C18 H18C 0.9800 . ?
C42 H42A 0.9800 . ?
C42 H42B 0.9800 . ?
C42 H42C 0.9800 . ?
C38 H38A 0.9800 . ?
C38 H38B 0.9800 . ?
C38 H38C 0.9800 . ?
C39 H39A 0.9800 . ?
C39 H39B 0.9800 . ?
C39 H39C 0.9800 . ?
C41 H41A 0.9800 . ?
C41 H41B 0.9800 . ?
C41 H41C 0.9800 . ?
C21 H21A 0.9800 . ?
C21 H21B 0.9800 . ?
C21 H21C 0.9800 . ?
C20 H20A 0.9800 . ?
C20 H20B 0.9800 . ?
C20 H20C 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
Fe1 O2 C22 C27 38.90(18) . . . . ?
Fe1 O2 C22 C23 -141.58(11) . . . . ?
Fe1 O1 C1 C6 38.03(18) . . . . ?
Fe1 O1 C1 C2 -143.13(11) . . . . ?
Fe1 C29 C28 N4 -171.78(9) . . . . ?
Fe1 C29 C28 C27 8.63(19) . . . . ?
Fe1 C8 C7 N1 -170.91(9) . . . . ?
Fe1 C8 C7 C6 8.02(19) . . . . ?
O2 C22 C27 C28 0.8(2) . . . . ?
O2 C22 C27 C26 -176.10(13) . . . . ?
O2 C22 C23 C24 178.31(14) . . . . ?
O1 C1 C6 C7 0.6(2) . . . . ?
O1 C1 C6 C5 -176.73(13) . . . . ?
O1 C1 C2 C3 178.42(14) . . . . ?
N4 C28 C27 C22 154.71(14) . . . . ?
N4 C28 C27 C26 -28.4(2) . . . . ?
N6 C29 C28 N4 0.71(14) . . . . ?
N6 C29 C28 C27 -178.88(13) . . . . ?
N6 C31 C36 C40 1.9(2) . . . . ?
N6 C31 C36 C35 -178.75(12) . . . . ?
N6 C31 C32 C37 -1.5(2) . . . . ?
N6 C31 C32 C33 177.59(13) . . . . ?
N3 C8 C7 N1 0.89(14) . . . . ?
N3 C8 C7 C6 179.83(13) . . . . ?
N3 C10 C11 C16 -1.4(2) . . . . ?
N3 C10 C11 C12 178.62(12) . . . . ?
N3 C10 C15 C19 -2.0(2) . . . . ?
N3 C10 C15 C14 -179.48(12) . . . . ?
N5 N4 C28 C29 -0.53(15) . . . . ?
N5 N4 C28 C27 179.07(13) . . . . ?
N5 N6 C29 Fe1 169.35(11) . . . . ?
N5 N6 C29 C28 -0.72(16) . . . . ?
N5 N6 C31 C36 -89.43(16) . . . . ?
N5 N6 C31 C32 92.46(15) . . . . ?
N1 C7 C6 C1 154.27(14) . . . . ?
N1 C7 C6 C5 -28.4(2) . . . . ?
N2 N3 C8 Fe1 168.56(11) . . . . ?
N2 N3 C8 C7 -0.81(15) . . . . ?
N2 N3 C10 C11 -74.49(16) . . . . ?
N2 N3 C10 C15 105.87(14) . . . . ?
N2 N1 C7 C8 -0.77(16) . . . . ?
N2 N1 C7 C6 -179.73(13) . . . . ?
C29 N6 N5 N4 0.42(15) . . . . ?
C29 N6 C31 C36 90.32(17) . . . . ?
C29 N6 C31 C32 -87.79(17) . . . . ?
C29 C28 C27 C22 -25.8(2) . . . . ?
C29 C28 C27 C26 151.07(15) . . . . ?
C28 N4 N5 N6 0.09(14) . . . . ?
C28 C27 C26 C25 179.69(15) . . . . ?
C22 C27 C26 C25 -3.5(2) . . . . ?
C22 C23 C24 C25 -1.2(3) . . . . ?
C27 C22 C23 C24 -2.1(2) . . . . ?
C27 C26 C25 C24 0.1(2) . . . . ?
C8 N3 N2 N1 0.37(15) . . . . ?
C8 N3 C10 C11 102.63(16) . . . . ?
C8 N3 C10 C15 -77.00(18) . . . . ?
C8 C7 C6 C1 -24.5(2) . . . . ?
C8 C7 C6 C5 152.81(14) . . . . ?
C31 N6 N5 N4 -179.81(12) . . . . ?
C31 N6 C29 Fe1 -10.4(2) . . . . ?
C31 N6 C29 C28 179.52(13) . . . . ?
C31 C36 C40 C42 -123.18(15) . . . . ?
C31 C36 C40 C41 113.14(16) . . . . ?
C31 C36 C35 C34 1.4(2) . . . . ?
C31 C32 C37 C38 -126.79(16) . . . . ?
C31 C32 C37 C39 109.73(17) . . . . ?
C31 C32 C33 C34 1.0(2) . . . . ?
C10 N3 N2 N1 177.83(11) . . . . ?
C10 N3 C8 Fe1 -8.6(2) . . . . ?
C10 N3 C8 C7 -177.96(12) . . . . ?
C10 C11 C16 C17 109.29(16) . . . . ?
C10 C11 C16 C18 -125.89(15) . . . . ?
C10 C11 C12 C13 1.5(2) . . . . ?
C10 C15 C19 C21 162.87(15) . . . . ?
C10 C15 C19 C20 -74.44(18) . . . . ?
C10 C15 C14 C13 0.3(2) . . . . ?
C7 N1 N2 N3 0.27(15) . . . . ?
C7 C6 C5 C4 179.29(14) . . . . ?
C11 C10 C15 C19 178.40(13) . . . . ?
C11 C10 C15 C14 0.9(2) . . . . ?
C11 C12 C13 C14 -0.4(2) . . . . ?
C1 C6 C5 C4 -3.4(2) . . . . ?
C1 C2 C3 C4 -0.3(3) . . . . ?
C16 C11 C12 C13 -178.52(14) . . . . ?
C36 C31 C32 C37 -179.47(14) . . . . ?
C36 C31 C32 C33 -0.4(2) . . . . ?
C36 C35 C34 C33 -0.9(3) . . . . ?
C6 C1 C2 C3 -2.7(2) . . . . ?
C6 C5 C4 C3 0.5(2) . . . . ?
C32 C31 C36 C40 179.85(14) . . . . ?
C32 C31 C36 C35 -0.7(2) . . . . ?
C32 C33 C34 C35 -0.3(3) . . . . ?
C40 C36 C35 C34 -179.18(15) . . . . ?
C15 C10 C11 C16 178.24(13) . . . . ?
C15 C10 C11 C12 -1.8(2) . . . . ?
C15 C14 C13 C12 -0.5(3) . . . . ?
C30 N4 N5 N6 -177.73(12) . . . . ?
C30 N4 C28 C29 176.89(14) . . . . ?
C30 N4 C28 C27 -3.5(2) . . . . ?
C26 C25 C24 C23 2.2(3) . . . . ?
C2 C1 C6 C7 -178.24(13) . . . . ?
C2 C1 C6 C5 4.4(2) . . . . ?
C23 C22 C27 C28 -178.70(13) . . . . ?
C23 C22 C27 C26 4.4(2) . . . . ?
C19 C15 C14 C13 -177.19(15) . . . . ?
C37 C32 C33 C34 -179.94(15) . . . . ?
C12 C11 C16 C17 -70.71(18) . . . . ?
C12 C11 C16 C18 54.12(19) . . . . ?
C5 C4 C3 C2 1.4(3) . . . . ?
C35 C36 C40 C42 57.44(18) . . . . ?
C35 C36 C40 C41 -66.24(18) . . . . ?
C33 C32 C37 C38 54.2(2) . . . . ?
C33 C32 C37 C39 -69.32(19) . . . . ?
C14 C15 C19 C21 -19.8(2) . . . . ?
C14 C15 C19 C20 102.90(18) . . . . ?
C9 N1 N2 N3 -175.78(12) . . . . ?
C9 N1 C7 C8 174.53(15) . . . . ?
C9 N1 C7 C6 -4.4(2) . . . . ?
loop_
_twin_individual_id
_twin_individual_mass_fraction_refined
1 0.6646(5)
2 0.3354(5)
