# Electronic Supplementary Material (ESI) for Dalton Transactions.
# This journal is © The Royal Society of Chemistry 2022

####################################################################### 
# 
# This file contains crystal structure data downloaded from the 
# Cambridge Structural Database (CSD) hosted by the Cambridge 
# Crystallographic Data Centre (CCDC).
# 
# Full information about CCDC data access policies and citation 
# guidelines are available at http://www.ccdc.cam.ac.uk/access/V1 
# 
# Audit and citation data items may have been added by the CCDC. 
# Please retain this information to preserve the provenance of 
# this file and to allow appropriate attribution of the data. 
# 
#######################################################################

data_tpafe36clo4_cu_300_9
_database_code_depnum_ccdc_archive 'CCDC 2164127'
loop_
_audit_author_name
_audit_author_address
'Oleg Demidov'
;North Caucasus Federal University, Department of Chemistry
Russia
;
_audit_update_record             
;
2022-04-03 deposited with the CCDC.	2022-06-27 downloaded from the CCDC.
;
_audit_creation_date             2021-09-08
_audit_creation_method           
;
Olex2 1.3
(compiled 2020.11.12 svn.r5f609507 for OlexSys, GUI svn.r6272)
;
_shelx_SHELXL_version_number     2014/7
_chemical_name_systematic        
'3 - (3,6-Di-tert-butylcatecholato)-(tris(2-pyridylmethyl)amine)-iron(iii) percholrate'
_chemical_name_common            
'3 - (3,6-Di-tert-butylcatecholato)-(tris(2-pyridylmethyl)amine)-iron(iii) percholrate'
_chemical_formula_moiety         'C32 H38 Fe N4 O2, Cl O4, 0.5(H2 O)'
_chemical_formula_sum            'C32 H39 Cl Fe N4 O6.50'
_chemical_compound_source        'Rostov-on-Don, Russia'
_chemical_formula_weight         674.97
_exptl_crystal_description       block
_exptl_crystal_colour            'dark violet'
_diffrn_ambient_temperature      293(2)
_chemical_oxdiff_formula         'C32 H38 Cl1 Fe1 N4 O6'
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'
Cl Cl 0.3639 0.7018 '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'

_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.
;
_space_group_crystal_system      triclinic
_space_group_IT_number           2
_space_group_name_H-M_alt        'P -1'
_space_group_name_Hall           '-P 1'
loop_
_space_group_symop_operation_xyz
'x, y, z'
'-x, -y, -z'

_cell_length_a                   8.5899(3)
_cell_length_b                   10.3201(3)
_cell_length_c                   20.3051(6)
_cell_angle_alpha                94.917(2)
_cell_angle_beta                 93.923(3)
_cell_angle_gamma                106.867(3)
_cell_volume                     1708.01(10)
_cell_formula_units_Z            2
_cell_measurement_reflns_used    10926
_cell_measurement_temperature    293(2)
_cell_measurement_theta_max      75.1590
_cell_measurement_theta_min      4.5290
_shelx_estimated_absorpt_T_max   0.349
_shelx_estimated_absorpt_T_min   0.197
_exptl_absorpt_coefficient_mu    4.662
_exptl_absorpt_correction_T_max  0.754
_exptl_absorpt_correction_T_min  0.228
_exptl_absorpt_correction_type   gaussian
_exptl_absorpt_process_details   
;
CrysAlisPro 1.171.40.67a (Rigaku Oxford Diffraction, 2019)
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_absorpt_special_details   ?
_exptl_crystal_colour_lustre     .
_exptl_crystal_colour_modifier   dark
_exptl_crystal_colour_primary    violet
_exptl_crystal_density_diffrn    1.312
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    ?
_exptl_crystal_F_000             708
loop_
_exptl_crystal_face_index_h
_exptl_crystal_face_index_k
_exptl_crystal_face_index_l
_exptl_crystal_face_perp_dist
-3 -2 9 0.1832
-2 -5 8 0.1703
-1 -6 -2 0.1540
1 -7 3 0.1439
1 -6 6 0.1656
-5 4 -4 0.1800
6 -1 -1 0.1412
5 -2 2 0.1574
0 -3 12 0.2133
-6 1 1 0.1457
-5 2 -7 0.1747
4 2 3 0.1319
-4 -3 1 0.1398
3 3 5 0.1416
2 4 7 0.1494
-1 -6 1 0.1436
-1 4 -11 0.1748
0 6 -2 0.1924
0 5 7 0.1515
1 -7 1 0.1439
1 -6 -4 0.1677
-2 5 8 0.1737
4 -6 0 0.1656
4 -5 -5 0.1956
-3 6 -3 0.1935
4 -1 -9 0.2233
-5 1 4 0.1313

_exptl_crystal_size_max          0.516
_exptl_crystal_size_mid          0.348
_exptl_crystal_size_min          0.286
loop_
_exptl_oxdiff_crystal_face_indexfrac_h
_exptl_oxdiff_crystal_face_indexfrac_k
_exptl_oxdiff_crystal_face_indexfrac_l
_exptl_oxdiff_crystal_face_x
_exptl_oxdiff_crystal_face_y
_exptl_oxdiff_crystal_face_z
-3.4931 -1.7300 9.4585 0.1486 -0.7904 0.5943
-1.5428 -4.6520 8.1928 0.4599 -0.4332 0.7751
-0.9574 -5.7933 -1.5778 0.9568 -0.1245 0.2626
1.1714 -6.6200 2.9230 0.7326 0.1380 0.6665
1.3614 -6.1640 6.1781 0.5263 0.0999 0.8444
-4.6713 4.3798 -4.2796 -0.0896 -0.6973 -0.7112
5.5517 -1.3786 -1.4569 -0.1806 0.9671 0.1794
5.3909 -2.4810 2.3689 -0.1610 0.8585 0.4869
-0.2372 -3.4603 11.7192 0.0519 -0.2895 0.9558
-5.5592 1.4539 1.2159 0.1799 -0.9632 -0.1997
-4.6122 1.9120 -6.6409 0.3474 -0.6354 -0.6896
4.3732 1.8398 2.8536 -0.7127 0.6745 0.1928
-3.9607 -3.1102 0.7630 0.7196 -0.6819 0.1313
3.1380 3.1739 4.9280 -0.8863 0.4212 0.1924
1.6249 4.1128 6.7566 -0.9727 0.1267 0.1946
-0.6132 -6.1473 0.7869 0.8880 -0.1170 0.4447
-1.4112 3.7979 -11.2188 0.0092 0.0010 -1.0000
0.3806 6.2526 -2.2580 -0.8274 0.1093 -0.5508
-0.1172 4.8969 7.4452 -0.9748 -0.1819 0.1290
1.0342 -6.6600 1.2742 0.8132 0.1503 0.5622
0.5452 -6.0385 -3.9594 0.9673 0.1798 0.1788
-1.8169 5.0232 7.8174 -0.8747 -0.4763 0.0894
3.6288 -6.1279 0.0959 0.5816 0.6123 0.5356
3.5757 -5.3200 -5.2754 0.6806 0.7181 0.1449
-3.3878 6.1215 -3.0836 -0.4830 -0.5076 -0.7135
4.3389 -0.7732 -8.9378 0.1198 0.9229 -0.3659
-5.3110 0.5126 4.0591 0.1831 -0.9819 0.0488

_exptl_transmission_factor_max   ?
_exptl_transmission_factor_min   ?
_diffrn_reflns_av_R_equivalents  0.0333
_diffrn_reflns_av_unetI/netI     0.0233
_diffrn_reflns_Laue_measured_fraction_full 0.999
_diffrn_reflns_Laue_measured_fraction_max 0.995
_diffrn_reflns_limit_h_max       10
_diffrn_reflns_limit_h_min       -10
_diffrn_reflns_limit_k_max       12
_diffrn_reflns_limit_k_min       -13
_diffrn_reflns_limit_l_max       25
_diffrn_reflns_limit_l_min       -22
_diffrn_reflns_number            35491
_diffrn_reflns_point_group_measured_fraction_full 0.999
_diffrn_reflns_point_group_measured_fraction_max 0.995
_diffrn_reflns_theta_full        67.684
_diffrn_reflns_theta_max         76.530
_diffrn_reflns_theta_min         4.392
_diffrn_detector                 'CCD plate'
_diffrn_detector_area_resol_mean 5.2529
_diffrn_detector_type            AtlasS2
_diffrn_measured_fraction_theta_full 0.999
_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    -69.00  32.00   1.00    7.00    --  -41.35  57.00-120.00  101
  2  ω   -116.00 -17.00   1.00    7.00    --  -41.35 -38.00 -30.00   99
  3  ω   -113.00 -13.00   1.00    7.00    --  -41.35 -57.00  90.00  100
  4  ω      7.00  33.00   1.00    7.00    --   41.35  84.00  90.64   26
  5  ω      6.00  82.00   1.00    7.00    --   41.35 -99.00 -60.00   76
  6  ω     17.00 116.00   1.00    7.00    --   41.35  38.00-150.00   99
  7  ω     30.00 106.00   1.00   28.00    --  112.00 -95.00-180.00   76
  8  ω     36.00 109.00   1.00   28.00    --  112.00-111.00  90.00   73
  9  ω     30.00 106.00   1.00   28.00    --  112.00 -95.00 -90.00   76
 10  ω     36.00 109.00   1.00   28.00    --  112.00-111.00 -90.00   73
 11  ω     36.00 109.00   1.00   28.00    --  112.00-111.00  30.00   73
 12  ω     86.00 178.00   1.00   28.00    --  112.00  45.00-150.00   92
 13  ω     30.00 106.00   1.00   28.00    --  112.00 -95.00 -60.00   76
 14  ω     36.00 140.00   1.00   28.00    --  112.00 -30.00 150.00  104
 15  ω    104.00 178.00   1.00   28.00    --  112.00 111.00  30.00   74
 16  ω     36.00 109.00   1.00   28.00    --  112.00-111.00-180.00   73
 17  ω     59.00 178.00   1.00   28.00    --  112.00  15.00  90.00  119
 18  ω     61.00 146.00   1.00   28.00    --  112.00 178.00-150.00   85
 19  ω     61.00 146.00   1.00   28.00    --  112.00 178.00  90.00   85
 20  ω     83.00 178.00   1.00   28.00    --  112.00  61.00  90.00   95
 21  ω     40.00 141.00   1.00   28.00    --  112.00 -61.00 120.00  101
 22  ω     36.00 109.00   1.00   28.00    --  112.00-111.00   0.00   73
 23  ω     36.00 109.00   1.00   28.00    --  112.00-111.00 120.00   73
 24  ω     36.00 109.00   1.00   28.00    --  112.00-111.00 -30.00   73
 25  ω     30.00 106.00   1.00   28.00    --  112.00 -95.00 -30.00   76
 26  ω     30.00 106.00   1.00   28.00    --  112.00 -95.00  60.00   76
 27  ω     86.00 178.00   1.00   28.00    --  112.00  45.00  90.00   92
 28  ω     30.00 165.00   1.00   28.00    --  112.00 -15.00 120.00  135
 29  ω     33.00 146.00   1.00   28.00    --  112.00 -83.00 108.79  113
 30  ω     36.00 145.00   1.00   28.00    --  112.00 -77.00 -30.00  109
 31  ω    103.00 178.00   1.00   28.00    --  112.00  77.00 -60.00   75
 32  ω     30.00 106.00   1.00   28.00    --  112.00 -95.00 150.00   76
 33  ω     36.00 109.00   1.00   28.00    --  112.00-111.00-120.00   73
 34  ω     36.00 109.00   1.00   28.00    --  112.00-111.00  60.00   73
 35  ω     36.00 109.00   1.00   28.00    --  112.00-111.00 150.00   73
 36  ω    138.00 177.00   1.00   28.00    --  112.00 111.00 -30.00   39
 37  ω    117.00 172.00   1.00   28.00    --  112.00 111.00   0.00   55
 38  ω     86.00 156.00   1.00   28.00    --  112.00  61.00 -30.00   70
 39  ω     39.00  84.00   1.00   28.00    --  112.00 -47.00 -45.00   45
 40  ω    104.00 129.00   1.00   28.00    --  112.00 -47.00 -45.00   25
 41  ω     90.00 141.00   1.00   28.00    --  112.00 -61.00-150.00   51
 42  ω    101.00 130.00   1.00   28.00    --  112.00 -77.00  60.00   29
 43  ω    111.00 159.00   1.00   28.00    --  112.00  61.00 120.00   48
;
_diffrn_measurement_device       'four-circle diffractometer'
_diffrn_measurement_device_type  'SuperNova, Dual, Cu at home/near, AtlasS2'
_diffrn_measurement_method       'ω scans'
_diffrn_orient_matrix_type       
'CrysAlisPro convention (1999,Acta A55,543-557)'
_diffrn_orient_matrix_UB_11      -0.0779348000
_diffrn_orient_matrix_UB_12      -0.1416689000
_diffrn_orient_matrix_UB_13      -0.0389792000
_diffrn_orient_matrix_UB_21      0.1684361000
_diffrn_orient_matrix_UB_22      -0.0005098000
_diffrn_orient_matrix_UB_23      -0.0214486000
_diffrn_orient_matrix_UB_31      0.0318783000
_diffrn_orient_matrix_UB_32      -0.0675505000
_diffrn_orient_matrix_UB_33      0.0622543000
_diffrn_radiation_monochromator  mirror
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           'Cu K\a'
_diffrn_radiation_wavelength     1.54184
_diffrn_source                   'micro-focus sealed X-ray tube'
_diffrn_source_type              'SuperNova (Cu) X-ray Source'
_reflns_Friedel_coverage         0.000
_reflns_Friedel_fraction_full    .
_reflns_Friedel_fraction_max     .
_reflns_number_gt                6365
_reflns_number_total             7137
_reflns_odcompleteness_completeness 98.56
_reflns_odcompleteness_iscentric 1
_reflns_odcompleteness_theta     77.17
_reflns_special_details          
;
 Reflections were merged by SHELXL according to the crystal
 class for the calculation of statistics and refinement.
 
 _reflns_Friedel_fraction is defined as the number of unique
 Friedel pairs measured divided by the number that would be
 possible theoretically, ignoring centric projections and
 systematic absences.
;
_reflns_threshold_expression     'I > 2σ(I)'
_computing_cell_refinement       'CrysAlisPro 1.171.40.67a (Rigaku OD, 2019)'
_computing_data_collection       'CrysAlisPro 1.171.40.67a (Rigaku OD, 2019)'
_computing_data_reduction        'CrysAlisPro 1.171.40.67a (Rigaku OD, 2019)'
_computing_molecular_graphics    'Olex2 1.3 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 1.3 (Dolomanov et al., 2009)'
_computing_structure_refinement  'SHELXL 2014/7 (Sheldrick, 2015)'
_computing_structure_solution    'SHELXT 2014/5 (Sheldrick, 2014)'
_refine_diff_density_max         0.221
_refine_diff_density_min         -0.270
_refine_diff_density_rms         0.034
_refine_ls_extinction_coef       .
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.026
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     565
_refine_ls_number_reflns         7137
_refine_ls_number_restraints     0
_refine_ls_R_factor_all          0.0468
_refine_ls_R_factor_gt           0.0418
_refine_ls_restrained_S_all      1.026
_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)+(0.0682P)²+0.1762P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1149
_refine_ls_wR_factor_ref         0.1220
_refine_special_details          ?
_olex2_refinement_description    
;
1. 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, All O(H,H) groups
2. Uiso/Uaniso restraints and constraints
Uanis(N3A) = Uanis(N3)
3. Others
 Sof(Cl1)=Sof(O3A)=Sof(O4A)=Sof(O5A)=Sof(O6A)=1-FVAR(1)
 Sof(Cl2)=Sof(O3)=Sof(O4)=Sof(O5)=Sof(O6)=FVAR(1)
 Sof(N3A)=Sof(C21')=Sof(H21')=Sof(C22')=Sof(H22')=Sof(C23')=Sof(H23')=
 Sof(C24')=Sof(H24')=Sof(C25')=Sof(C26')=Sof(H26C)=Sof(H26D)=1-FVAR(2)
 Sof(N3)=Sof(C25)=Sof(C26)=Sof(H26A)=Sof(H26B)=Sof(C21)=Sof(H21)=Sof(C23)=
 Sof(H23)=Sof(C24)=Sof(H24)=Sof(C22)=Sof(H22)=FVAR(2)
 Sof(H15A)=Sof(C19')=Sof(C20')=Sof(H20C)=Sof(H20D)=Sof(C18')=Sof(H18')=
 Sof(C17')=Sof(H17')=Sof(C16')=Sof(H16')=1-FVAR(3)
 Sof(C19)=Sof(H15)=Sof(C20)=Sof(H20A)=Sof(H20B)=Sof(C16)=Sof(H16)=Sof(C18)=
 Sof(H18)=Sof(C17)=Sof(H17)=FVAR(3)
 Fixed Sof: O7(0.5) H7A(0.5) H7B(0.5)
4.a Free rotating group:
 O7(H7A,H7B)
4.b Secondary CH2 refined with riding coordinates:
 C20(H20A,H20B), C32(H32A,H32B), C26(H26A,H26B), C26'(H26C,H26D), C20'(H20C,
 H20D)
4.c Aromatic/amide H refined with riding coordinates:
 C27(H27), C4(H4), C5(H5), C15(H15), C15(H15A), C28(H28), C29(H29), C21(H21),
 C30(H30), C16(H16), C23(H23), C24(H24), C22(H22), C18(H18), C17(H17),
 C21'(H21'), C22'(H22'), C23'(H23'), C24'(H24'), C18'(H18'), C17'(H17'),
 C16'(H16')
4.d Idealised Me refined as rotating group:
 C13(H13A,H13B,H13C), C8(H8A,H8B,H8C), C10(H10A,H10B,H10C), C12(H12A,H12B,
 H12C), C9(H9A,H9B,H9C), C14(H14A,H14B,H14C)
;
_atom_sites_solution_hydrogens   mixed
_atom_sites_solution_primary     dual
_atom_sites_solution_secondary   ?
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
Fe Fe 0.55237(4) 0.32938(3) 0.24412(2) 0.06515(11) Uani 1 1 d . . . . .
Cl2 Cl 0.8390(6) 0.7235(5) 0.0603(2) 0.0967(8) Uani 0.470(11) 1 d . . P A 1
O1 O 0.68824(17) 0.50998(13) 0.27523(6) 0.0671(3) Uani 1 1 d . . . . .
O2 O 0.59664(19) 0.29058(14) 0.33149(7) 0.0719(3) Uani 1 1 d . . . . .
N4 N 0.7231(2) 0.25972(17) 0.18856(8) 0.0686(4) Uani 1 1 d . . . . .
N1 N 0.4016(2) 0.12503(18) 0.21120(10) 0.0718(4) Uani 1 1 d . . . . .
N3 N 0.3391(9) 0.3902(8) 0.2595(6) 0.0741(14) Uani 0.66(2) 1 d . . P B 1
N2 N 0.4794(2) 0.35469(19) 0.14270(9) 0.0780(4) Uani 1 1 d . . . . .
C1 C 0.7217(2) 0.52630(19) 0.34147(9) 0.0619(4) Uani 1 1 d . . . . .
C2 C 0.6728(2) 0.4044(2) 0.37263(9) 0.0650(4) Uani 1 1 d . . . . .
C6 C 0.7979(3) 0.6524(2) 0.37868(10) 0.0693(4) Uani 1 1 d . . . . .
C3 C 0.7012(3) 0.4037(2) 0.44118(10) 0.0762(5) Uani 1 1 d . . . . .
C7 C 0.8403(3) 0.7861(2) 0.34691(12) 0.0791(5) Uani 1 1 d . . . . .
C11 C 0.6456(4) 0.2716(3) 0.47389(12) 0.0918(7) Uani 1 1 d . . . . .
C27 C 0.8029(3) 0.1743(2) 0.20828(14) 0.0829(6) Uani 1 1 d . . . . .
H27 H 0.8016 0.1544 0.2521 0.099 Uiso 1 1 calc R U . . .
C19 C 0.338(2) 0.095(2) 0.1542(12) 0.071(4) Uani 0.41(4) 1 d . . P B 1
C25 C 0.2909(15) 0.4477(13) 0.2085(6) 0.080(2) Uani 0.66(2) 1 d . . P B 1
C31 C 0.7256(3) 0.2889(2) 0.12558(11) 0.0785(5) Uani 1 1 d . . . . .
C4 C 0.7807(4) 0.5283(3) 0.47631(11) 0.0921(7) Uani 1 1 d . . . . .
H4 H 0.8046 0.5324 0.5219 0.110 Uiso 1 1 calc R U . . .
C5 C 0.8266(4) 0.6482(3) 0.44652(11) 0.0872(6) Uani 1 1 d . . . . .
H5 H 0.8789 0.7292 0.4732 0.105 Uiso 1 1 calc R U . . .
C15 C 0.3944(3) 0.0168(3) 0.24487(14) 0.0866(6) Uani 1 1 d . . . . .
H15 H 0.4485 0.0297 0.2873 0.104 Uiso 0.41(4) 1 calc R U P B 1
H15A H 0.4192 0.0306 0.2907 0.104 Uiso 0.59(4) 1 calc R U P B 2
C13 C 0.7329(5) 0.1713(3) 0.44625(14) 0.1024(9) Uani 1 1 d . . . . .
H13A H 0.6996 0.1466 0.3996 0.154 Uiso 1 1 calc R U . . .
H13B H 0.7047 0.0911 0.4690 0.154 Uiso 1 1 calc R U . . .
H13C H 0.8490 0.2135 0.4528 0.154 Uiso 1 1 calc R U . . .
C20 C 0.343(4) 0.227(3) 0.1201(11) 0.079(3) Uani 0.41(4) 1 d . . P B 1
H20A H 0.3463 0.2058 0.0729 0.095 Uiso 0.41(4) 1 calc R U P B 1
H20B H 0.2410 0.2469 0.1258 0.095 Uiso 0.41(4) 1 calc R U P B 1
C32 C 0.6309(4) 0.3854(3) 0.10868(12) 0.0946(7) Uani 1 1 d . . . . .
H32A H 0.6971 0.4785 0.1226 0.113 Uiso 1 1 calc R U . . .
H32B H 0.6034 0.3760 0.0610 0.113 Uiso 1 1 calc R U . . .
C8 C 0.9564(4) 0.7841(3) 0.29378(15) 0.0936(7) Uani 1 1 d . . . . .
H8A H 1.0519 0.7651 0.3127 0.140 Uiso 1 1 calc R U . . .
H8B H 0.9879 0.8712 0.2769 0.140 Uiso 1 1 calc R U . . .
H8C H 0.9027 0.7147 0.2582 0.140 Uiso 1 1 calc R U . . .
C26 C 0.405(2) 0.470(2) 0.1542(8) 0.092(3) Uani 0.66(2) 1 d . . P B 1
H26A H 0.3453 0.4778 0.1133 0.110 Uiso 0.66(2) 1 calc R U P B 1
H26B H 0.4920 0.5544 0.1662 0.110 Uiso 0.66(2) 1 calc R U P B 1
C28 C 0.8871(4) 0.1146(3) 0.1658(2) 0.1073(9) Uani 1 1 d . . . . .
H28 H 0.9400 0.0540 0.1804 0.129 Uiso 1 1 calc R U . . .
O3 O 0.880(2) 0.8582(11) 0.0310(5) 0.130(5) Uani 0.470(11) 1 d . . P A 1
C29 C 0.8917(4) 0.1454(4) 0.1025(2) 0.1157(11) Uani 1 1 d . . . . .
H29 H 0.9491 0.1069 0.0733 0.139 Uiso 1 1 calc R U . . .
C10 C 0.9248(5) 0.9089(3) 0.39890(17) 0.1114(9) Uani 1 1 d . . . . .
H10A H 0.8544 0.9128 0.4333 0.167 Uiso 1 1 calc R U . . .
H10B H 0.9469 0.9913 0.3779 0.167 Uiso 1 1 calc R U . . .
H10C H 1.0256 0.8989 0.4179 0.167 Uiso 1 1 calc R U . . .
C21 C 0.2547(13) 0.3749(10) 0.3115(4) 0.0884(17) Uani 0.66(2) 1 d . . P B 1
H21 H 0.2879 0.3330 0.3463 0.106 Uiso 0.66(2) 1 calc R U P B 1
C30 C 0.8115(4) 0.2337(3) 0.08136(15) 0.1073(9) Uani 1 1 d . . . . .
H30 H 0.8147 0.2562 0.0380 0.129 Uiso 1 1 calc R U . . .
C12 C 0.4615(5) 0.2086(4) 0.45985(18) 0.1192(11) Uani 1 1 d . . . . .
H12A H 0.4074 0.2719 0.4769 0.179 Uiso 1 1 calc R U . . .
H12B H 0.4278 0.1266 0.4810 0.179 Uiso 1 1 calc R U . . .
H12C H 0.4332 0.1875 0.4128 0.179 Uiso 1 1 calc R U . . .
C9 C 0.6837(4) 0.8068(3) 0.31580(18) 0.1065(9) Uani 1 1 d . . . . .
H9A H 0.6321 0.7330 0.2820 0.160 Uiso 1 1 calc R U . . .
H9B H 0.7097 0.8912 0.2965 0.160 Uiso 1 1 calc R U . . .
H9C H 0.6109 0.8090 0.3494 0.160 Uiso 1 1 calc R U . . .
C16 C 0.316(3) -0.100(2) 0.2198(13) 0.099(5) Uani 0.41(4) 1 d . . P B 1
H16 H 0.3024 -0.1726 0.2453 0.118 Uiso 0.41(4) 1 calc R U P B 1
C14 C 0.6918(6) 0.2975(4) 0.54977(14) 0.1322(14) Uani 1 1 d . . . . .
H14A H 0.8068 0.3430 0.5588 0.198 Uiso 1 1 calc R U . . .
H14B H 0.6656 0.2122 0.5683 0.198 Uiso 1 1 calc R U . . .
H14C H 0.6316 0.3536 0.5694 0.198 Uiso 1 1 calc R U . . .
C23 C 0.0672(13) 0.4763(10) 0.2622(6) 0.096(3) Uani 0.66(2) 1 d . . P B 1
H23 H -0.0277 0.5023 0.2623 0.115 Uiso 0.66(2) 1 calc R U P B 1
C24 C 0.1550(12) 0.4945(8) 0.2091(6) 0.092(2) Uani 0.66(2) 1 d . . P B 1
H24 H 0.1251 0.5373 0.1740 0.111 Uiso 0.66(2) 1 calc R U P B 1
C22 C 0.1161(12) 0.4198(10) 0.3160(6) 0.099(2) Uani 0.66(2) 1 d . . P B 1
H22 H 0.0597 0.4117 0.3536 0.119 Uiso 0.66(2) 1 calc R U P B 1
C18 C 0.260(2) -0.020(2) 0.1206(14) 0.094(4) Uani 0.41(4) 1 d . . P B 1
H18 H 0.2159 -0.0303 0.0766 0.113 Uiso 0.41(4) 1 calc R U P B 1
C17 C 0.251(2) -0.123(2) 0.1570(19) 0.128(8) Uani 0.41(4) 1 d . . P B 1
H17 H 0.1991 -0.2121 0.1383 0.154 Uiso 0.41(4) 1 calc R U P B 1
O4 O 0.804(3) 0.7575(15) 0.1223(6) 0.188(7) Uani 0.470(11) 1 d . . P A 1
O5 O 0.6853(12) 0.6463(8) 0.0256(4) 0.146(5) Uani 0.470(11) 1 d . . P A 1
O6 O 0.9534(12) 0.6504(8) 0.0615(6) 0.183(5) Uani 0.470(11) 1 d . . P A 1
Cl1 Cl 0.7968(13) 0.7420(7) 0.0579(3) 0.151(2) Uani 0.530(11) 1 d . . P A 2
O3A O 0.919(2) 0.8432(13) 0.0362(7) 0.153(5) Uani 0.530(11) 1 d . . P A 2
O4A O 0.8061(16) 0.6296(8) 0.0107(3) 0.170(4) Uani 0.530(11) 1 d . . P A 2
O5A O 0.862(2) 0.7143(15) 0.1214(6) 0.235(10) Uani 0.530(11) 1 d . . P A 2
O6A O 0.6380(14) 0.735(2) 0.0569(6) 0.274(8) Uani 0.530(11) 1 d . . P A 2
O7 O 1.1027(18) 0.5620(10) 0.0509(4) 0.217(5) Uani 0.5 1 d G . P C 2
H7A H 1.0864 0.5088 0.0152 0.326 Uiso 0.5 1 d G U P C 2
H7B H 1.0747 0.6303 0.0399 0.326 Uiso 0.5 1 d G U P C 2
N3A N 0.337(2) 0.4048(18) 0.2392(9) 0.0741(14) Uani 0.34(2) 1 d . . P B 2
C21' C 0.240(2) 0.403(2) 0.2894(15) 0.102(5) Uani 0.34(2) 1 d . . P B 2
H21' H 0.2669 0.3689 0.3282 0.123 Uiso 0.34(2) 1 calc R U P B 2
C22' C 0.107(2) 0.448(3) 0.2855(14) 0.110(9) Uani 0.34(2) 1 d . . P B 2
H22' H 0.0416 0.4443 0.3204 0.132 Uiso 0.34(2) 1 calc R U P B 2
C23' C 0.071(3) 0.5003(17) 0.2259(18) 0.115(8) Uani 0.34(2) 1 d . . P B 2
H23' H -0.0190 0.5328 0.2213 0.138 Uiso 0.34(2) 1 calc R U P B 2
C24' C 0.167(2) 0.5033(15) 0.1755(16) 0.103(6) Uani 0.34(2) 1 d . . P B 2
H24' H 0.1414 0.5322 0.1352 0.123 Uiso 0.34(2) 1 calc R U P B 2
C25' C 0.308(3) 0.461(2) 0.1863(14) 0.082(5) Uani 0.34(2) 1 d . . P B 2
C26' C 0.418(6) 0.472(4) 0.1361(16) 0.095(7) Uani 0.34(2) 1 d . . P B 2
H26C H 0.5057 0.5566 0.1439 0.114 Uiso 0.34(2) 1 calc R U P B 2
H26D H 0.3611 0.4653 0.0924 0.114 Uiso 0.34(2) 1 calc R U P B 2
C19' C 0.3560(17) 0.1104(14) 0.1423(8) 0.069(3) Uani 0.59(4) 1 d . . P B 2
C20' C 0.365(2) 0.2268(17) 0.1057(9) 0.080(3) Uani 0.59(4) 1 d . . P B 2
H20C H 0.2568 0.2377 0.0986 0.096 Uiso 0.59(4) 1 calc R U P B 2
H20D H 0.4023 0.2108 0.0626 0.096 Uiso 0.59(4) 1 calc R U P B 2
C18' C 0.309(3) -0.0254(19) 0.1103(10) 0.110(4) Uani 0.59(4) 1 d . . P B 2
H18' H 0.2832 -0.0391 0.0645 0.132 Uiso 0.59(4) 1 calc R U P B 2
C17' C 0.298(3) -0.1391(16) 0.1446(9) 0.131(5) Uani 0.59(4) 1 d . . P B 2
H17' H 0.2575 -0.2263 0.1222 0.157 Uiso 0.59(4) 1 calc R U P B 2
C16' C 0.348(2) -0.1222(15) 0.2110(9) 0.102(4) Uani 0.59(4) 1 d . . P B 2
H16' H 0.3527 -0.1957 0.2337 0.122 Uiso 0.59(4) 1 calc R U P B 2


_geom_special_details            
;
 All esds (except the esd in the dihedral angle between two l.s. planes)
 are estimated using the full covariance matrix.  The cell esds are taken
 into account individually in the estimation of esds in distances, angles
 and torsion angles; correlations between esds in cell parameters are only
 used when they are defined by crystal symmetry.  An approximate (isotropic)
 treatment of cell esds is used for estimating esds involving l.s. planes.
;
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
Fe O1 1.9157(14) . ?
Fe O2 1.8894(14) . ?
Fe N4 2.1543(17) . ?
Fe N1 2.1508(18) . ?
Fe N3 2.135(8) . ?
Fe N2 2.1709(18) . ?
Fe N3A 2.208(18) . ?
Cl2 O3 1.516(13) . ?
Cl2 O4 1.354(14) . ?
Cl2 O5 1.428(8) . ?
Cl2 O6 1.403(10) . ?
O1 C1 1.342(2) . ?
O2 C2 1.348(3) . ?
N4 C27 1.334(3) . ?
N4 C31 1.339(3) . ?
N1 C19 1.22(2) . ?
N1 C15 1.347(3) . ?
N1 C19' 1.410(16) . ?
N3 C25 1.336(10) . ?
N3 C21 1.315(13) . ?
N2 C20 1.50(3) . ?
N2 C32 1.480(4) . ?
N2 C26 1.51(2) . ?
N2 C26' 1.46(4) . ?
N2 C20' 1.500(17) . ?
C1 C2 1.423(3) . ?
C1 C6 1.401(3) . ?
C2 C3 1.398(3) . ?
C6 C7 1.532(3) . ?
C6 C5 1.389(3) . ?
C3 C11 1.532(3) . ?
C3 C4 1.377(4) . ?
C7 C8 1.521(3) . ?
C7 C10 1.542(4) . ?
C7 C9 1.525(4) . ?
C11 C13 1.535(3) . ?
C11 C12 1.521(5) . ?
C11 C14 1.545(4) . ?
C27 H27 0.9300 . ?
C27 C28 1.379(4) . ?
C19 C20 1.57(3) . ?
C19 C18 1.29(3) . ?
C25 C26 1.514(19) . ?
C25 C24 1.387(17) . ?
C31 C32 1.504(4) . ?
C31 C30 1.387(4) . ?
C4 H4 0.9300 . ?
C4 C5 1.389(4) . ?
C5 H5 0.9300 . ?
C15 H15 0.9300 . ?
C15 H15A 0.9300 . ?
C15 C16 1.24(2) . ?
C15 C16' 1.467(17) . ?
C13 H13A 0.9600 . ?
C13 H13B 0.9600 . ?
C13 H13C 0.9600 . ?
C20 H20A 0.9700 . ?
C20 H20B 0.9700 . ?
C32 H32A 0.9700 . ?
C32 H32B 0.9700 . ?
C8 H8A 0.9600 . ?
C8 H8B 0.9600 . ?
C8 H8C 0.9600 . ?
C26 H26A 0.9700 . ?
C26 H26B 0.9700 . ?
C28 H28 0.9300 . ?
C28 C29 1.350(5) . ?
C29 H29 0.9300 . ?
C29 C30 1.370(5) . ?
C10 H10A 0.9600 . ?
C10 H10B 0.9600 . ?
C10 H10C 0.9600 . ?
C21 H21 0.9300 . ?
C21 C22 1.402(13) . ?
C30 H30 0.9300 . ?
C12 H12A 0.9600 . ?
C12 H12B 0.9600 . ?
C12 H12C 0.9600 . ?
C9 H9A 0.9600 . ?
C9 H9B 0.9600 . ?
C9 H9C 0.9600 . ?
C16 H16 0.9300 . ?
C16 C17 1.33(4) . ?
C14 H14A 0.9600 . ?
C14 H14B 0.9600 . ?
C14 H14C 0.9600 . ?
C23 H23 0.9300 . ?
C23 C24 1.352(15) . ?
C23 C22 1.378(12) . ?
C24 H24 0.9300 . ?
C22 H22 0.9300 . ?
C18 H18 0.9300 . ?
C18 C17 1.33(4) . ?
C17 H17 0.9300 . ?
Cl1 O3A 1.377(14) . ?
Cl1 O4A 1.465(13) . ?
Cl1 O5A 1.453(13) . ?
Cl1 O6A 1.343(15) . ?
O7 H7A 0.8501 . ?
O7 H7B 0.8498 . ?
N3A C21' 1.35(3) . ?
N3A C25' 1.31(2) . ?
C21' H21' 0.9300 . ?
C21' C22' 1.36(3) . ?
C22' H22' 0.9300 . ?
C22' C23' 1.42(3) . ?
C23' H23' 0.9300 . ?
C23' C24' 1.36(3) . ?
C24' H24' 0.9300 . ?
C24' C25' 1.41(3) . ?
C25' C26' 1.42(4) . ?
C26' H26C 0.9700 . ?
C26' H26D 0.9700 . ?
C19' C20' 1.45(2) . ?
C19' C18' 1.42(2) . ?
C20' H20C 0.9700 . ?
C20' H20D 0.9700 . ?
C18' H18' 0.9300 . ?
C18' C17' 1.40(3) . ?
C17' H17' 0.9300 . ?
C17' C16' 1.37(2) . ?
C16' H16' 0.9300 . ?

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
O1 Fe N4 98.98(6) . . ?
O1 Fe N1 178.71(6) . . ?
O1 Fe N3 90.3(2) . . ?
O1 Fe N2 100.93(6) . . ?
O1 Fe N3A 89.7(4) . . ?
O2 Fe O1 84.80(6) . . ?
O2 Fe N4 103.99(6) . . ?
O2 Fe N1 93.94(7) . . ?
O2 Fe N3 97.8(3) . . ?
O2 Fe N2 173.93(7) . . ?
O2 Fe N3A 109.5(5) . . ?
N4 Fe N2 77.27(7) . . ?
N4 Fe N3A 146.1(5) . . ?
N1 Fe N4 81.06(7) . . ?
N1 Fe N2 80.34(7) . . ?
N1 Fe N3A 91.0(4) . . ?
N3 Fe N4 157.0(3) . . ?
N3 Fe N1 90.1(2) . . ?
N3 Fe N2 80.3(3) . . ?
N2 Fe N3A 68.9(5) . . ?
O4 Cl2 O3 102.9(8) . . ?
O4 Cl2 O5 104.9(10) . . ?
O4 Cl2 O6 111.7(9) . . ?
O5 Cl2 O3 104.2(7) . . ?
O6 Cl2 O3 119.3(9) . . ?
O6 Cl2 O5 112.6(7) . . ?
C1 O1 Fe 111.51(11) . . ?
C2 O2 Fe 112.05(11) . . ?
C27 N4 Fe 125.20(15) . . ?
C27 N4 C31 119.0(2) . . ?
C31 N4 Fe 114.90(15) . . ?
C19 N1 Fe 120.6(11) . . ?
C19 N1 C15 113.8(11) . . ?
C15 N1 Fe 124.43(17) . . ?
C15 N1 C19' 122.0(6) . . ?
C19' N1 Fe 110.5(6) . . ?
C25 N3 Fe 113.1(7) . . ?
C21 N3 Fe 127.3(5) . . ?
C21 N3 C25 119.6(8) . . ?
C20 N2 Fe 103.8(10) . . ?
C20 N2 C26 107.8(14) . . ?
C32 N2 Fe 105.78(14) . . ?
C32 N2 C20 119.7(9) . . ?
C32 N2 C26 116.4(8) . . ?
C32 N2 C20' 106.4(8) . . ?
C26 N2 Fe 100.8(6) . . ?
C26' N2 Fe 114.5(13) . . ?
C26' N2 C32 104.9(17) . . ?
C26' N2 C20' 111.5(17) . . ?
C20' N2 Fe 112.9(7) . . ?
O1 C1 C2 114.97(17) . . ?
O1 C1 C6 123.85(17) . . ?
C6 C1 C2 121.19(17) . . ?
O2 C2 C1 115.30(16) . . ?
O2 C2 C3 122.64(18) . . ?
C3 C2 C1 122.06(19) . . ?
C1 C6 C7 122.09(18) . . ?
C5 C6 C1 115.4(2) . . ?
C5 C6 C7 122.4(2) . . ?
C2 C3 C11 121.2(2) . . ?
C4 C3 C2 115.5(2) . . ?
C4 C3 C11 123.2(2) . . ?
C6 C7 C10 111.3(2) . . ?
C8 C7 C6 110.88(17) . . ?
C8 C7 C10 107.5(2) . . ?
C8 C7 C9 109.4(2) . . ?
C9 C7 C6 109.2(2) . . ?
C9 C7 C10 108.5(2) . . ?
C3 C11 C13 109.2(2) . . ?
C3 C11 C14 111.3(2) . . ?
C13 C11 C14 107.1(2) . . ?
C12 C11 C3 110.2(2) . . ?
C12 C11 C13 109.7(3) . . ?
C12 C11 C14 109.3(3) . . ?
N4 C27 H27 119.0 . . ?
N4 C27 C28 122.1(3) . . ?
C28 C27 H27 119.0 . . ?
N1 C19 C20 110.3(18) . . ?
N1 C19 C18 133(2) . . ?
C18 C19 C20 117(2) . . ?
N3 C25 C26 114.6(11) . . ?
N3 C25 C24 121.8(8) . . ?
C24 C25 C26 123.3(9) . . ?
N4 C31 C32 114.4(2) . . ?
N4 C31 C30 121.1(3) . . ?
C30 C31 C32 124.5(3) . . ?
C3 C4 H4 118.6 . . ?
C3 C4 C5 122.8(2) . . ?
C5 C4 H4 118.6 . . ?
C6 C5 H5 118.6 . . ?
C4 C5 C6 122.9(2) . . ?
C4 C5 H5 118.6 . . ?
N1 C15 H15 119.7 . . ?
N1 C15 H15A 119.2 . . ?
N1 C15 C16' 121.6(6) . . ?
C16 C15 N1 120.6(11) . . ?
C16 C15 H15 119.7 . . ?
C16' C15 H15A 119.2 . . ?
C11 C13 H13A 109.5 . . ?
C11 C13 H13B 109.5 . . ?
C11 C13 H13C 109.5 . . ?
H13A C13 H13B 109.5 . . ?
H13A C13 H13C 109.5 . . ?
H13B C13 H13C 109.5 . . ?
N2 C20 C19 119(2) . . ?
N2 C20 H20A 107.6 . . ?
N2 C20 H20B 107.6 . . ?
C19 C20 H20A 107.6 . . ?
C19 C20 H20B 107.6 . . ?
H20A C20 H20B 107.1 . . ?
N2 C32 C31 109.61(18) . . ?
N2 C32 H32A 109.7 . . ?
N2 C32 H32B 109.7 . . ?
C31 C32 H32A 109.7 . . ?
C31 C32 H32B 109.7 . . ?
H32A C32 H32B 108.2 . . ?
C7 C8 H8A 109.5 . . ?
C7 C8 H8B 109.5 . . ?
C7 C8 H8C 109.5 . . ?
H8A C8 H8B 109.5 . . ?
H8A C8 H8C 109.5 . . ?
H8B C8 H8C 109.5 . . ?
N2 C26 C25 112.3(11) . . ?
N2 C26 H26A 109.1 . . ?
N2 C26 H26B 109.1 . . ?
C25 C26 H26A 109.1 . . ?
C25 C26 H26B 109.1 . . ?
H26A C26 H26B 107.9 . . ?
C27 C28 H28 120.5 . . ?
C29 C28 C27 119.1(3) . . ?
C29 C28 H28 120.5 . . ?
C28 C29 H29 120.1 . . ?
C28 C29 C30 119.8(3) . . ?
C30 C29 H29 120.1 . . ?
C7 C10 H10A 109.5 . . ?
C7 C10 H10B 109.5 . . ?
C7 C10 H10C 109.5 . . ?
H10A C10 H10B 109.5 . . ?
H10A C10 H10C 109.5 . . ?
H10B C10 H10C 109.5 . . ?
N3 C21 H21 119.0 . . ?
N3 C21 C22 122.1(6) . . ?
C22 C21 H21 119.0 . . ?
C31 C30 H30 120.5 . . ?
C29 C30 C31 119.0(3) . . ?
C29 C30 H30 120.5 . . ?
C11 C12 H12A 109.5 . . ?
C11 C12 H12B 109.5 . . ?
C11 C12 H12C 109.5 . . ?
H12A C12 H12B 109.5 . . ?
H12A C12 H12C 109.5 . . ?
H12B C12 H12C 109.5 . . ?
C7 C9 H9A 109.5 . . ?
C7 C9 H9B 109.5 . . ?
C7 C9 H9C 109.5 . . ?
H9A C9 H9B 109.5 . . ?
H9A C9 H9C 109.5 . . ?
H9B C9 H9C 109.5 . . ?
C15 C16 H16 119.5 . . ?
C15 C16 C17 121.0(17) . . ?
C17 C16 H16 119.5 . . ?
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 . . ?
C24 C23 H23 119.5 . . ?
C24 C23 C22 121.1(9) . . ?
C22 C23 H23 119.5 . . ?
C25 C24 H24 120.9 . . ?
C23 C24 C25 118.2(7) . . ?
C23 C24 H24 120.9 . . ?
C21 C22 H22 121.5 . . ?
C23 C22 C21 117.1(8) . . ?
C23 C22 H22 121.5 . . ?
C19 C18 H18 124.5 . . ?
C19 C18 C17 111(3) . . ?
C17 C18 H18 124.5 . . ?
C16 C17 C18 121(2) . . ?
C16 C17 H17 119.6 . . ?
C18 C17 H17 119.6 . . ?
O3A Cl1 O4A 97.5(10) . . ?
O3A Cl1 O5A 106.4(11) . . ?
O5A Cl1 O4A 104.5(13) . . ?
O6A Cl1 O3A 126.7(13) . . ?
O6A Cl1 O4A 106.5(10) . . ?
O6A Cl1 O5A 112.3(11) . . ?
H7A O7 H7B 104.5 . . ?
C21' N3A Fe 123.4(10) . . ?
C25' N3A Fe 117.2(13) . . ?
C25' N3A C21' 119.3(17) . . ?
N3A C21' H21' 118.6 . . ?
N3A C21' C22' 122.9(16) . . ?
C22' C21' H21' 118.6 . . ?
C21' C22' H22' 121.4 . . ?
C21' C22' C23' 117.1(18) . . ?
C23' C22' H22' 121.4 . . ?
C22' C23' H23' 119.9 . . ?
C24' C23' C22' 120.3(17) . . ?
C24' C23' H23' 119.9 . . ?
C23' C24' H24' 121.1 . . ?
C23' C24' C25' 117.8(17) . . ?
C25' C24' H24' 121.1 . . ?
N3A C25' C24' 122.0(19) . . ?
N3A C25' C26' 118.6(19) . . ?
C24' C25' C26' 119(2) . . ?
N2 C26' H26C 111.2 . . ?
N2 C26' H26D 111.2 . . ?
C25' C26' N2 103(2) . . ?
C25' C26' H26C 111.2 . . ?
C25' C26' H26D 111.2 . . ?
H26C C26' H26D 109.1 . . ?
N1 C19' C20' 122.2(11) . . ?
N1 C19' C18' 115.7(14) . . ?
C18' C19' C20' 122.1(13) . . ?
N2 C20' H20C 109.4 . . ?
N2 C20' H20D 109.4 . . ?
C19' C20' N2 111.1(12) . . ?
C19' C20' H20C 109.4 . . ?
C19' C20' H20D 109.4 . . ?
H20C C20' H20D 108.0 . . ?
C19' C18' H18' 118.5 . . ?
C17' C18' C19' 123.1(16) . . ?
C17' C18' H18' 118.5 . . ?
C18' C17' H17' 120.0 . . ?
C16' C17' C18' 120.1(14) . . ?
C16' C17' H17' 120.0 . . ?
C15 C16' H16' 121.4 . . ?
C17' C16' C15 117.2(11) . . ?
C17' C16' H16' 121.4 . . ?

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
Fe O1 C1 C2 9.31(18) . . . . ?
Fe O1 C1 C6 -170.38(14) . . . . ?
Fe O2 C2 C1 -7.23(19) . . . . ?
Fe O2 C2 C3 172.35(15) . . . . ?
Fe N4 C27 C28 168.0(2) . . . . ?
Fe N4 C31 C32 10.1(2) . . . . ?
Fe N4 C31 C30 -170.57(19) . . . . ?
Fe N1 C19 C20 -15.3(19) . . . . ?
Fe N1 C19 C18 170.7(18) . . . . ?
Fe N1 C15 C16 -173.3(10) . . . . ?
Fe N1 C15 C16' -154.2(9) . . . . ?
Fe N1 C19' C20' -18.6(15) . . . . ?
Fe N1 C19' C18' 158.3(10) . . . . ?
Fe N3 C25 C26 -5.5(13) . . . . ?
Fe N3 C25 C24 -179.8(8) . . . . ?
Fe N3 C21 C22 179.8(7) . . . . ?
Fe N2 C20 C19 -25.6(18) . . . . ?
Fe N2 C32 C31 45.6(2) . . . . ?
Fe N2 C26 C25 -46.1(12) . . . . ?
Fe N2 C26' C25' -46(3) . . . . ?
Fe N2 C20' C19' -11.3(14) . . . . ?
Fe N3A C21' C22' -179.2(14) . . . . ?
Fe N3A C25' C24' 175.0(13) . . . . ?
Fe N3A C25' C26' -1(3) . . . . ?
O1 Fe O2 C2 9.75(12) . . . . ?
O1 C1 C2 O2 -1.5(2) . . . . ?
O1 C1 C2 C3 178.92(17) . . . . ?
O1 C1 C6 C7 4.2(3) . . . . ?
O1 C1 C6 C5 -178.15(19) . . . . ?
O2 C2 C3 C11 -0.4(3) . . . . ?
O2 C2 C3 C4 179.9(2) . . . . ?
N4 Fe O2 C2 107.74(12) . . . . ?
N4 C27 C28 C29 1.3(4) . . . . ?
N4 C31 C32 N2 -38.3(3) . . . . ?
N4 C31 C30 C29 1.5(4) . . . . ?
N1 Fe O2 C2 -170.51(12) . . . . ?
N1 C19 C20 N2 29(2) . . . . ?
N1 C19 C18 C17 0(3) . . . . ?
N1 C15 C16 C17 7(2) . . . . ?
N1 C15 C16' C17' -5.8(15) . . . . ?
N1 C19' C20' N2 20.4(18) . . . . ?
N1 C19' C18' C17' 3.4(19) . . . . ?
N3 Fe O2 C2 -79.9(2) . . . . ?
N3 C25 C26 N2 37.2(16) . . . . ?
N3 C25 C24 C23 -2.3(16) . . . . ?
N3 C21 C22 C23 2.6(15) . . . . ?
C1 C2 C3 C11 179.1(2) . . . . ?
C1 C2 C3 C4 -0.5(3) . . . . ?
C1 C6 C7 C8 -59.9(3) . . . . ?
C1 C6 C7 C10 -179.4(2) . . . . ?
C1 C6 C7 C9 60.8(3) . . . . ?
C1 C6 C5 C4 -1.2(4) . . . . ?
C2 C1 C6 C7 -175.48(17) . . . . ?
C2 C1 C6 C5 2.2(3) . . . . ?
C2 C3 C11 C13 61.8(3) . . . . ?
C2 C3 C11 C12 -58.8(3) . . . . ?
C2 C3 C11 C14 179.8(3) . . . . ?
C2 C3 C4 C5 1.6(4) . . . . ?
C6 C1 C2 O2 178.19(16) . . . . ?
C6 C1 C2 C3 -1.4(3) . . . . ?
C3 C4 C5 C6 -0.7(4) . . . . ?
C7 C6 C5 C4 176.4(2) . . . . ?
C11 C3 C4 C5 -178.1(2) . . . . ?
C27 N4 C31 C32 179.6(2) . . . . ?
C27 N4 C31 C30 -1.1(3) . . . . ?
C27 C28 C29 C30 -0.8(5) . . . . ?
C19 N1 C15 C16 -5.9(13) . . . . ?
C19 C18 C17 C16 1(3) . . . . ?
C25 N3 C21 C22 -1.3(15) . . . . ?
C31 N4 C27 C28 -0.3(4) . . . . ?
C4 C3 C11 C13 -118.6(3) . . . . ?
C4 C3 C11 C12 120.8(3) . . . . ?
C4 C3 C11 C14 -0.6(4) . . . . ?
C5 C6 C7 C8 122.6(3) . . . . ?
C5 C6 C7 C10 3.1(3) . . . . ?
C5 C6 C7 C9 -116.7(3) . . . . ?
C15 N1 C19 C20 176.8(12) . . . . ?
C15 N1 C19 C18 3(3) . . . . ?
C15 N1 C19' C20' -179.5(11) . . . . ?
C15 N1 C19' C18' -2.6(14) . . . . ?
C15 C16 C17 C18 -4(3) . . . . ?
C20 N2 C32 C31 -70.9(13) . . . . ?
C20 N2 C26 C25 62.4(15) . . . . ?
C20 C19 C18 C17 -174.0(18) . . . . ?
C32 N2 C20 C19 91.9(15) . . . . ?
C32 N2 C26 C25 -159.9(8) . . . . ?
C32 N2 C26' C25' -161.5(18) . . . . ?
C32 N2 C20' C19' 104.3(11) . . . . ?
C32 C31 C30 C29 -179.2(3) . . . . ?
C26 N2 C20 C19 -132.0(17) . . . . ?
C26 N2 C32 C31 156.5(7) . . . . ?
C26 C25 C24 C23 -176.1(11) . . . . ?
C28 C29 C30 C31 -0.6(5) . . . . ?
C21 N3 C25 C26 175.4(11) . . . . ?
C21 N3 C25 C24 1.2(17) . . . . ?
C30 C31 C32 N2 142.4(2) . . . . ?
C24 C25 C26 N2 -148.6(11) . . . . ?
C24 C23 C22 C21 -3.7(16) . . . . ?
C22 C23 C24 C25 3.6(15) . . . . ?
C18 C19 C20 N2 -156.3(15) . . . . ?
N3A Fe O2 C2 -78.0(5) . . . . ?
N3A C21' C22' C23' -1(3) . . . . ?
N3A C25' C26' N2 29(3) . . . . ?
C21' N3A C25' C24' -9(3) . . . . ?
C21' N3A C25' C26' 175(2) . . . . ?
C21' C22' C23' C24' 0(3) . . . . ?
C22' C23' C24' C25' -4(2) . . . . ?
C23' C24' C25' N3A 9(3) . . . . ?
C23' C24' C25' C26' -176(2) . . . . ?
C24' C25' C26' N2 -147(2) . . . . ?
C25' N3A C21' C22' 5(3) . . . . ?
C26' N2 C32 C31 167.0(14) . . . . ?
C26' N2 C20' C19' -141.8(19) . . . . ?
C19' N1 C15 C16' 3.9(10) . . . . ?
C19' C18' C17' C16' -6(2) . . . . ?
C20' N2 C32 C31 -74.7(7) . . . . ?
C20' N2 C26' C25' 84(2) . . . . ?
C20' C19' C18' C17' -179.7(14) . . . . ?
C18' C19' C20' N2 -156.3(11) . . . . ?
C18' C17' C16' C15 7(2) . . . . ?

_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
;
_oxdiff_exptl_absorpt_empirical_full_max 1.168
_oxdiff_exptl_absorpt_empirical_full_min 0.865
_symmetry_cell_setting           triclinic
_symmetry_space_group_name_h-m   'P -1'
_symmetry_int_tables_number      2
_chemical_absolute_configuration .

####################################################################### 
# 
# This file contains crystal structure data downloaded from the 
# Cambridge Structural Database (CSD) hosted by the Cambridge 
# Crystallographic Data Centre (CCDC).
# 
# Full information about CCDC data access policies and citation 
# guidelines are available at http://www.ccdc.cam.ac.uk/access/V1 
# 
# Audit and citation data items may have been added by the CCDC. 
# Please retain this information to preserve the provenance of 
# this file and to allow appropriate attribution of the data. 
# 
#######################################################################

data_tpafe36clo4_100
_database_code_depnum_ccdc_archive 'CCDC 2164128'
loop_
_audit_author_name
_audit_author_address
'Oleg Demidov'
;North Caucasus Federal University, Department of Chemistry
Russia
;
_audit_update_record             
;
2022-04-03 deposited with the CCDC.	2022-06-27 downloaded from the CCDC.
;
_audit_creation_date             2021-09-08
_audit_creation_method           
;
Olex2 1.3
(compiled 2020.11.12 svn.r5f609507 for OlexSys, GUI svn.r6272)
;
_shelx_SHELXL_version_number     2014/7
_chemical_name_systematic        
'3 - (3,6-Di-tert-butylcatecholato)-(tris(2-pyridylmethyl)amine)-iron(iii) percholrate'
_chemical_name_common            
'3 - (3,6-Di-tert-butylcatecholato)-(tris(2-pyridylmethyl)amine)-iron(iii) percholrate'
_chemical_formula_moiety         'C32 H38 Fe N4 O2, Cl O4, 0.5(H2 O)'
_chemical_formula_sum            'C32 H39 Cl Fe N4 O6.50'
_chemical_compound_source        'Rostov-on-Don, Russia'
_chemical_formula_weight         674.97
_chemical_melting_point          ?
_exptl_crystal_description       block
_exptl_crystal_colour            'dark violet'
_diffrn_ambient_temperature      100.01(11)
_chemical_oxdiff_formula         'C32 H38 Fe N4 O2, Cl O4'
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'
Cl Cl 0.3639 0.7018 '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'

_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.
;
_space_group_crystal_system      triclinic
_space_group_IT_number           2
_space_group_name_H-M_alt        'P -1'
_space_group_name_Hall           '-P 1'
loop_
_space_group_symop_operation_xyz
'x, y, z'
'-x, -y, -z'

_cell_length_a                   8.3709(2)
_cell_length_b                   10.3122(2)
_cell_length_c                   19.7722(3)
_cell_angle_alpha                97.511(2)
_cell_angle_beta                 92.574(2)
_cell_angle_gamma                106.888(2)
_cell_volume                     1612.97(6)
_cell_formula_units_Z            2
_cell_measurement_reflns_used    15672
_cell_measurement_temperature    100.01(11)
_cell_measurement_theta_max      75.8030
_cell_measurement_theta_min      4.5070
_shelx_estimated_absorpt_T_max   0.424
_shelx_estimated_absorpt_T_min   0.277
_exptl_absorpt_coefficient_mu    4.936
_exptl_absorpt_correction_T_max  1.000
_exptl_absorpt_correction_T_min  0.664
_exptl_absorpt_correction_type   gaussian
_exptl_absorpt_process_details   
;
CrysAlisPro 1.171.40.67a (Rigaku Oxford Diffraction, 2019)
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_absorpt_special_details   ?
_exptl_crystal_colour_lustre     .
_exptl_crystal_colour_modifier   dark
_exptl_crystal_colour_primary    violet
_exptl_crystal_density_diffrn    1.390
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    ?
_exptl_crystal_F_000             708
loop_
_exptl_crystal_face_index_h
_exptl_crystal_face_index_k
_exptl_crystal_face_index_l
_exptl_crystal_face_perp_dist
-3 5 5 0.1558
5 0 -4 0.1311
5 0 -1 0.0988
0 -6 3 0.1034
5 -1 4 0.1148
-5 0 -3 0.1292
0 -6 0 0.0994
3 0 10 0.1387
2 -4 11 0.1570
-1 7 -3 0.0988
0 1 12 0.1463
-1 -5 8 0.1460
3 -6 -2 0.1139
-5 0 4 0.1311
-5 0 0 0.1102
-4 -3 -2 0.1115
0 -6 1 0.0981
5 0 3 0.1102
1 4 6 0.1372
-1 0 -12 0.1577
0 -1 -13 0.1615
1 -6 -1 0.1021
-1 5 8 0.1472
2 -2 -11 0.1662

_exptl_crystal_size_max          0.35
_exptl_crystal_size_mid          0.232
_exptl_crystal_size_min          0.21
loop_
_exptl_oxdiff_crystal_face_indexfrac_h
_exptl_oxdiff_crystal_face_indexfrac_k
_exptl_oxdiff_crystal_face_indexfrac_l
_exptl_oxdiff_crystal_face_x
_exptl_oxdiff_crystal_face_y
_exptl_oxdiff_crystal_face_z
-3.4188 5.0662 5.4696 0.5190 -0.4895 -0.7007
5.0699 -0.2542 -4.3632 -0.9915 0.1296 -0.0090
5.2129 -0.0814 -0.5191 -0.9830 -0.1831 -0.0090
-0.4252 -6.2188 2.8146 0.3353 0.0604 0.9402
5.0496 -1.3313 3.9064 -0.8592 -0.4681 0.2063
-4.8443 -0.1053 -3.3733 0.8783 0.4780 0.0090
-0.4373 -6.1116 -0.4664 0.2981 0.3118 0.9022
2.7633 0.4479 9.8116 -0.4296 -0.9030 -0.0091
1.8771 -3.6634 11.0187 -0.1013 -0.7858 0.6101
-1.4419 6.6613 -2.9038 -0.0011 0.0093 -1.0000
-0.3782 0.6425 12.4925 0.1831 -0.9830 -0.0091
-0.7861 -5.1097 8.3007 0.4224 -0.3976 0.8146
2.7296 -6.2693 -1.9252 -0.3075 0.2941 0.9049
-5.0962 0.3757 4.3124 0.9915 -0.1296 -0.0092
-5.2392 0.2029 0.4683 0.9830 0.1831 -0.0092
-3.5412 -3.2822 -1.6272 0.7670 0.4186 0.4863
-0.4894 -6.1943 1.2779 0.3298 0.1818 0.9264
4.8706 -0.0161 3.4241 -0.8783 -0.4780 0.0092
1.3917 4.2353 6.3261 -0.3463 -0.7308 -0.5882
-1.2809 -0.4487 -11.7780 0.1296 0.9915 -0.0091
0.3519 -0.5211 -12.5433 -0.1831 0.9830 -0.0091
1.4928 -6.4946 -1.4316 -0.0615 0.3190 0.9458
-1.1937 4.6240 8.0250 0.1442 -0.7668 -0.6255
2.1850 -1.7478 -11.3882 -0.4710 0.8648 0.1740

_exptl_transmission_factor_max   ?
_exptl_transmission_factor_min   ?
_diffrn_reflns_av_R_equivalents  0.0289
_diffrn_reflns_av_unetI/netI     0.0214
_diffrn_reflns_Laue_measured_fraction_full 1.000
_diffrn_reflns_Laue_measured_fraction_max 0.996
_diffrn_reflns_limit_h_max       10
_diffrn_reflns_limit_h_min       -10
_diffrn_reflns_limit_k_max       9
_diffrn_reflns_limit_k_min       -12
_diffrn_reflns_limit_l_max       24
_diffrn_reflns_limit_l_min       -24
_diffrn_reflns_number            33846
_diffrn_reflns_point_group_measured_fraction_full 1.000
_diffrn_reflns_point_group_measured_fraction_max 0.996
_diffrn_reflns_theta_full        67.684
_diffrn_reflns_theta_max         76.446
_diffrn_reflns_theta_min         2.263
_diffrn_ambient_environment      N~2~
_diffrn_detector                 'CCD plate'
_diffrn_detector_area_resol_mean 5.2529
_diffrn_detector_type            AtlasS2
_diffrn_measured_fraction_theta_full 1.000
_diffrn_measured_fraction_theta_max 0.996
_diffrn_measurement_details      
;
List of Runs (angles in degrees, time in seconds):

  # Type    Start    End  Width  tₑₓₚ   ω     θ     κ     φ   Frames
#--------------------------------------------------------------------------
  1  ω   -113.00 -13.00   1.00    1.00    --  -41.35 -57.00-180.00  100
  2  ω   -114.00 -62.00   1.00    1.00    --  -41.35-148.00-106.00   52
  3  ω   -116.00 -17.00   1.00    1.00    --  -41.35 -38.00 -90.00   99
  4  ω     27.00  97.00   1.00    1.00    --   41.35-125.00  60.00   70
  5  ω     17.00 116.00   1.00    1.00    --   41.35  38.00 120.00   99
  6  ω    -21.00  74.00   1.00    1.00    --   41.35 -77.00-120.00   95
  7  ω      8.00  42.00   1.00    1.00    --   41.35  80.00 153.97   34
  8  ω     61.00 146.00   1.00    2.57    --  112.00 178.00  90.00   85
  9  ω     30.00 106.00   1.00    2.57    --  112.00 -95.00-120.00   76
 10  ω     37.00 136.00   1.00    2.57    --  112.00 -36.00-159.88   99
 11  ω     84.00 178.00   1.00    2.57    --  112.00  30.00 -90.00   94
 12  ω     36.00 109.00   1.00    2.57    --  112.00-111.00 -30.00   73
 13  ω     36.00 145.00   1.00    2.57    --  112.00 -77.00  90.00  109
 14  ω    103.00 178.00   1.00    2.57    --  112.00  77.00 120.00   75
 15  ω    104.00 178.00   1.00    2.57    --  112.00 111.00 -60.00   74
 16  ω     61.00 146.00   1.00    2.57    --  112.00 178.00  30.00   85
 17  ω     30.00 106.00   1.00    2.57    --  112.00 -95.00 -90.00   76
 18  ω    104.00 178.00   1.00    2.57    --  112.00 111.00  90.00   74
 19  ω     36.00 145.00   1.00    2.57    --  112.00 -77.00 -30.00  109
 20  ω    104.00 178.00   1.00    2.57    --  112.00 111.00 -30.00   74
 21  ω     36.00 109.00   1.00    2.57    --  112.00-111.00  30.00   73
 22  ω     30.00 106.00   1.00    2.57    --  112.00 -95.00  90.00   76
 23  ω     61.00 146.00   1.00    2.57    --  112.00 178.00 -30.00   85
 24  ω     40.00 141.00   1.00    2.57    --  112.00 -61.00   0.00  101
 25  ω     30.00 165.00   1.00    2.57    --  112.00 -15.00 -90.00  135
 26  ω     39.00 138.00   1.00    2.57    --  112.00 -45.00-120.00   99
 27  ω     30.00 106.00   1.00    2.57    --  112.00 -95.00-180.00   76
 28  ω     40.00 141.00   1.00    2.57    --  112.00 -61.00  30.00  101
 29  ω     36.00 145.00   1.00    2.57    --  112.00 -77.00-180.00  109
 30  ω     30.00 165.00   1.00    2.57    --  112.00 -15.00  60.00  135
 31  ω     61.00 146.00   1.00    2.57    --  112.00 178.00 150.00   85
 32  ω     36.00 109.00   1.00    2.57    --  112.00-111.00-120.00   73
 33  ω     36.00 109.00   1.00    2.57    --  112.00-111.00 -60.00   73
 34  ω     39.00 111.00   1.00    2.57    --  112.00-124.00  58.00   72
 35  ω     30.00 106.00   1.00    2.57    --  112.00 -95.00 -30.00   76
 36  ω     73.00 106.00   1.00    2.57    --  112.00 -95.00 120.00   33
 37  ω     95.00 175.00   1.00    2.57    --  112.00  45.00  60.00   80
 38  ω     90.00 147.00   1.00    2.57    --  112.00 -86.00  30.95   57
 39  ω     84.00 116.00   1.00    2.57    --  112.00  61.00  30.00   32
 40  ω    135.00 162.00   1.00    2.57    --  112.00  61.00  30.00   27
 41  ω     40.00  68.00   1.00    2.57    --  112.00 -61.00  90.00   28
 42  ω     77.00 132.00   1.00    2.57    --  112.00 -30.00 -30.00   55
 43  ω     40.00  67.00   1.00    2.57    --  112.00 -86.00  30.95   27
;
_diffrn_measurement_device       'four-circle diffractometer'
_diffrn_measurement_device_type  'SuperNova, Dual, Cu at home/near, AtlasS2'
_diffrn_measurement_method       'ω scans'
_diffrn_orient_matrix_type       
'CrysAlisPro convention (1999,Acta A55,543-557)'
_diffrn_orient_matrix_UB_11      -0.1880655000
_diffrn_orient_matrix_UB_12      -0.0361513000
_diffrn_orient_matrix_UB_13      0.0108268000
_diffrn_orient_matrix_UB_21      -0.0435410000
_diffrn_orient_matrix_UB_22      -0.0419626000
_diffrn_orient_matrix_UB_23      -0.0778507000
_diffrn_orient_matrix_UB_31      -0.0033656000
_diffrn_orient_matrix_UB_32      -0.1478900000
_diffrn_orient_matrix_UB_33      0.0067740000
_diffrn_radiation_monochromator  mirror
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           'Cu K\a'
_diffrn_radiation_wavelength     1.54184
_diffrn_source                   'micro-focus sealed X-ray tube'
_diffrn_source_type              'SuperNova (Cu) X-ray Source'
_reflns_Friedel_coverage         0.000
_reflns_Friedel_fraction_full    .
_reflns_Friedel_fraction_max     .
_reflns_number_gt                6557
_reflns_number_total             6759
_reflns_odcompleteness_completeness 98.69
_reflns_odcompleteness_iscentric 1
_reflns_odcompleteness_theta     77.17
_reflns_special_details          
;
 Reflections were merged by SHELXL according to the crystal
 class for the calculation of statistics and refinement.
 
 _reflns_Friedel_fraction is defined as the number of unique
 Friedel pairs measured divided by the number that would be
 possible theoretically, ignoring centric projections and
 systematic absences.
;
_reflns_threshold_expression     'I > 2σ(I)'
_computing_cell_refinement       'CrysAlisPro 1.171.40.67a (Rigaku OD, 2019)'
_computing_data_collection       'CrysAlisPro 1.171.40.67a (Rigaku OD, 2019)'
_computing_data_reduction        'CrysAlisPro 1.171.40.67a (Rigaku OD, 2019)'
_computing_molecular_graphics    'Olex2 1.3 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 1.3 (Dolomanov et al., 2009)'
_computing_structure_refinement  'SHELXL 2014/7 (Sheldrick, 2015)'
_computing_structure_solution    'SHELXT 2014/5 (Sheldrick, 2014)'
_refine_diff_density_max         0.314
_refine_diff_density_min         -0.662
_refine_diff_density_rms         0.053
_refine_ls_extinction_coef       .
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.039
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     452
_refine_ls_number_reflns         6759
_refine_ls_number_restraints     10
_refine_ls_R_factor_all          0.0369
_refine_ls_R_factor_gt           0.0355
_refine_ls_restrained_S_all      1.040
_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)+(0.0535P)²+0.8414P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0925
_refine_ls_wR_factor_ref         0.0941
_refine_special_details          ?
_olex2_refinement_description    
;
1. 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, All O(H,H) groups
2. Restrained distances
 O3A-O6A \\sim O6-O3
 with sigma of 0.04
 Cl1-O5 \\sim Cl1A-O5
 with sigma of 0.02
 Cl1-O3A \\sim Cl1A-O6
 with sigma of 0.02
 Cl1-O6A \\sim Cl1A-O3
 with sigma of 0.02
 Cl1-O4A \\sim Cl1A-O4
 with sigma of 0.02
 O5-O6A \\sim O5-O3
 with sigma of 0.04
 O6A-O4A \\sim O3-O4
 with sigma of 0.04
 O5-O3A \\sim O5-O6
 with sigma of 0.04
 O5-O4A \\sim O5-O4
 with sigma of 0.04
 O3A-O4A \\sim O6-O4
 with sigma of 0.04
3. Others
 Sof(O6)=Sof(O3)=Sof(Cl1A)=Sof(O4)=1-FVAR(1)
 Sof(Cl1)=Sof(O3A)=Sof(O6A)=Sof(O4A)=FVAR(1)
 Fixed Sof: O7(0.5) H7A(0.5) H7B(0.5)
4.a Free rotating group:
 O7(H7A,H7B)
4.b Secondary CH2 refined with riding coordinates:
 C26(H26A,H26B), C20(H20A,H20B), C32(H32A,H32B)
4.c Aromatic/amide H refined with riding coordinates:
 C27(H27), C30(H30), C29(H29), C15(H15), C21(H21), C5(H5), C23(H23), C4(H4),
 C22(H22), C24(H24), C18(H18), C16(H16), C28(H28), C17(H17)
4.d Idealised Me refined as rotating group:
 C9(H9A,H9B,H9C), C12(H12A,H12B,H12C), C13(H13A,H13B,H13C), C8(H8A,H8B,H8C),
 C10(H10A,H10B,H10C), C14(H14A,H14B,H14C)
;
_atom_sites_solution_hydrogens   mixed
_atom_sites_solution_primary     dual
_atom_sites_solution_secondary   ?
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
Fe Fe 0.42923(3) 0.18432(2) 0.76486(2) 0.01575(8) Uani 1 1 d . . . . .
O1 O 0.29075(14) 0.00313(11) 0.73180(6) 0.0182(2) Uani 1 1 d . . . . .
O2 O 0.39048(14) 0.22140(11) 0.67736(6) 0.0192(2) Uani 1 1 d . . . . .
N3 N 0.24983(17) 0.24640(13) 0.80670(7) 0.0184(3) Uani 1 1 d . . . . .
N4 N 0.62462(17) 0.12062(14) 0.74714(7) 0.0196(3) Uani 1 1 d . . . . .
N1 N 0.56917(17) 0.37218(14) 0.79983(7) 0.0205(3) Uani 1 1 d . . . . .
N2 N 0.47339(17) 0.14388(14) 0.85867(7) 0.0190(3) Uani 1 1 d . . . . .
C1 C 0.26883(19) -0.01558(16) 0.66349(8) 0.0179(3) Uani 1 1 d . . . . .
C2 C 0.3215(2) 0.10599(16) 0.63302(8) 0.0188(3) Uani 1 1 d . . . . .
C27 C 0.7191(2) 0.14217(18) 0.69394(9) 0.0237(3) Uani 1 1 d . . . . .
H27 H 0.6902 0.1892 0.6607 0.028 Uiso 1 1 calc R U . . .
C31 C 0.6646(2) 0.05082(16) 0.79534(9) 0.0213(3) Uani 1 1 d . . . . .
C26 C 0.3076(2) 0.10902(17) 0.88758(8) 0.0217(3) Uani 1 1 d . . . . .
H26A H 0.3226 0.1148 0.9369 0.026 Uiso 1 1 calc R U . . .
H26B H 0.2414 0.0164 0.8685 0.026 Uiso 1 1 calc R U . . .
C6 C 0.1946(2) -0.14486(17) 0.62280(9) 0.0205(3) Uani 1 1 d . . . . .
C19 C 0.6222(2) 0.39354(17) 0.86659(9) 0.0227(3) Uani 1 1 d . . . . .
C3 C 0.3000(2) 0.10468(18) 0.56162(8) 0.0225(3) Uani 1 1 d . . . . .
C30 C 0.8043(2) 0.00477(17) 0.79236(10) 0.0257(3) Uani 1 1 d . . . . .
H30 H 0.8321 -0.0410 0.8265 0.031 Uiso 1 1 calc R U . . .
C25 C 0.2204(2) 0.21019(16) 0.86927(8) 0.0203(3) Uani 1 1 d . . . . .
C7 C 0.1467(2) -0.27838(17) 0.65382(9) 0.0222(3) Uani 1 1 d . . . . .
C29 C 0.9021(2) 0.02780(18) 0.73776(10) 0.0277(4) Uani 1 1 d . . . . .
H29 H 0.9964 -0.0024 0.7349 0.033 Uiso 1 1 calc R U . . .
C15 C 0.5908(2) 0.48022(17) 0.76567(9) 0.0246(3) Uani 1 1 d . . . . .
H15 H 0.5541 0.4650 0.7194 0.029 Uiso 1 1 calc R U . . .
C20 C 0.5954(2) 0.26735(17) 0.90051(9) 0.0231(3) Uani 1 1 d . . . . .
H20A H 0.7019 0.2494 0.9079 0.028 Uiso 1 1 calc R U . . .
H20B H 0.5543 0.2839 0.9449 0.028 Uiso 1 1 calc R U . . .
C21 C 0.1786(2) 0.33569(17) 0.78403(9) 0.0222(3) Uani 1 1 d . . . . .
H21 H 0.1973 0.3588 0.7405 0.027 Uiso 1 1 calc R U . . .
C32 C 0.5447(2) 0.02664(17) 0.85007(9) 0.0226(3) Uani 1 1 d . . . . .
H32A H 0.4561 -0.0589 0.8366 0.027 Uiso 1 1 calc R U . . .
H32B H 0.6030 0.0218 0.8927 0.027 Uiso 1 1 calc R U . . .
C11 C 0.3567(2) 0.23690(19) 0.52996(9) 0.0263(4) Uani 1 1 d . . . . .
C9 C 0.0208(2) -0.27520(17) 0.70757(9) 0.0250(3) Uani 1 1 d . . . . .
H9A H 0.0715 -0.2029 0.7448 0.038 Uiso 1 1 calc R U . . .
H9B H -0.0112 -0.3614 0.7245 0.038 Uiso 1 1 calc R U . . .
H9C H -0.0766 -0.2593 0.6871 0.038 Uiso 1 1 calc R U . . .
C5 C 0.1737(2) -0.14308(18) 0.55283(9) 0.0257(3) Uani 1 1 d . . . . .
H5 H 0.1239 -0.2257 0.5243 0.031 Uiso 1 1 calc R U . . .
C23 C 0.0490(2) 0.35802(18) 0.88811(10) 0.0267(4) Uani 1 1 d . . . . .
H23 H -0.0176 0.3965 0.9157 0.032 Uiso 1 1 calc R U . . .
C4 C 0.2241(2) -0.02297(19) 0.52325(9) 0.0274(4) Uani 1 1 d . . . . .
H4 H 0.2058 -0.0291 0.4760 0.033 Uiso 1 1 calc R U . . .
C12 C 0.2603(3) 0.33558(19) 0.55803(9) 0.0291(4) Uani 1 1 d . . . . .
H12A H 0.1422 0.2924 0.5473 0.044 Uiso 1 1 calc R U . . .
H12B H 0.2942 0.4176 0.5375 0.044 Uiso 1 1 calc R U . . .
H12C H 0.2844 0.3584 0.6068 0.044 Uiso 1 1 calc R U . . .
C22 C 0.0782(2) 0.39410(18) 0.82372(10) 0.0273(4) Uani 1 1 d . . . . .
H22 H 0.0312 0.4566 0.8074 0.033 Uiso 1 1 calc R U . . .
C24 C 0.1201(2) 0.26365(18) 0.91113(9) 0.0242(3) Uani 1 1 d . . . . .
H24 H 0.1004 0.2371 0.9539 0.029 Uiso 1 1 calc R U . . .
C18 C 0.7009(2) 0.52382(19) 0.90137(10) 0.0310(4) Uani 1 1 d . . . . .
H18 H 0.7389 0.5366 0.9474 0.037 Uiso 1 1 calc R U . . .
C16 C 0.6662(3) 0.61263(19) 0.79772(11) 0.0321(4) Uani 1 1 d . . . . .
H16 H 0.6791 0.6860 0.7735 0.039 Uiso 1 1 calc R U . . .
C28 C 0.8580(2) 0.09616(18) 0.68754(10) 0.0275(4) Uani 1 1 d . . . . .
H28 H 0.9209 0.1108 0.6501 0.033 Uiso 1 1 calc R U . . .
C13 C 0.5455(3) 0.3059(2) 0.54741(10) 0.0332(4) Uani 1 1 d . . . . .
H13A H 0.5685 0.3315 0.5961 0.050 Uiso 1 1 calc R U . . .
H13B H 0.5805 0.3862 0.5256 0.050 Uiso 1 1 calc R U . . .
H13C H 0.6056 0.2431 0.5314 0.050 Uiso 1 1 calc R U . . .
C8 C 0.3062(2) -0.29747(19) 0.68782(10) 0.0294(4) Uani 1 1 d . . . . .
H8A H 0.3819 -0.3063 0.6537 0.044 Uiso 1 1 calc R U . . .
H8B H 0.2765 -0.3786 0.7092 0.044 Uiso 1 1 calc R U . . .
H8C H 0.3595 -0.2193 0.7218 0.044 Uiso 1 1 calc R U . . .
C10 C 0.0652(3) -0.40330(18) 0.59886(10) 0.0312(4) Uani 1 1 d . . . . .
H10A H -0.0347 -0.3931 0.5775 0.047 Uiso 1 1 calc R U . . .
H10B H 0.0373 -0.4850 0.6198 0.047 Uiso 1 1 calc R U . . .
H10C H 0.1423 -0.4099 0.5650 0.047 Uiso 1 1 calc R U . . .
C17 C 0.7222(3) 0.6351(2) 0.86645(12) 0.0367(4) Uani 1 1 d . . . . .
H17 H 0.7736 0.7236 0.8889 0.044 Uiso 1 1 calc R U . . .
C14 C 0.3219(3) 0.2087(2) 0.45153(10) 0.0380(5) Uani 1 1 d . . . . .
H14A H 0.3821 0.1481 0.4327 0.057 Uiso 1 1 calc R U . . .
H14B H 0.3580 0.2934 0.4334 0.057 Uiso 1 1 calc R U . . .
H14C H 0.2040 0.1669 0.4395 0.057 Uiso 1 1 calc R U . . .
Cl1 Cl 0.1792(2) -0.22273(13) 0.93926(5) 0.0239(3) Uani 0.582(4) 1 d D . P A 1
O5 O 0.1301(2) -0.35050(15) 0.97001(7) 0.0417(4) Uani 1 1 d D . . . .
O3A O 0.1958(16) -0.2594(14) 0.8680(4) 0.043(2) Uani 0.582(4) 1 d D . P A 1
O6A O 0.3378(4) -0.1353(3) 0.97208(14) 0.0363(7) Uani 0.582(4) 1 d D . P A 1
O4A O 0.0574(3) -0.1493(3) 0.94538(16) 0.0443(8) Uani 0.582(4) 1 d D . P A 1
O6 O 0.2342(8) -0.1235(4) 0.9854(2) 0.0471(13) Uani 0.418(4) 1 d D . P A 2
O3 O 0.161(2) -0.2420(19) 0.8731(6) 0.042(3) Uani 0.418(4) 1 d D . P A 2
Cl1A Cl 0.2369(3) -0.24466(18) 0.93913(8) 0.0271(4) Uani 0.418(4) 1 d D . P A 2
O4 O 0.4057(6) -0.2453(6) 0.9352(2) 0.0634(16) Uani 0.418(4) 1 d D . P A 2
O7 O -0.0711(6) -0.0594(4) 0.9473(2) 0.0584(9) Uani 0.5 1 d G . P B 2
H7A H 0.0191 -0.0735 0.9611 0.088 Uiso 0.5 1 d G U P B 2
H7B H -0.0801 0.0061 0.9763 0.088 Uiso 0.5 1 d G U P B 2


_geom_special_details            
;
 All esds (except the esd in the dihedral angle between two l.s. planes)
 are estimated using the full covariance matrix.  The cell esds are taken
 into account individually in the estimation of esds in distances, angles
 and torsion angles; correlations between esds in cell parameters are only
 used when they are defined by crystal symmetry.  An approximate (isotropic)
 treatment of cell esds is used for estimating esds involving l.s. planes.
;
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
Fe O1 1.9017(12) . ?
Fe O2 1.8545(11) . ?
Fe N3 1.9701(14) . ?
Fe N4 1.9608(14) . ?
Fe N1 1.9652(14) . ?
Fe N2 1.9952(13) . ?
O1 C1 1.3358(19) . ?
O2 C2 1.342(2) . ?
N3 C25 1.351(2) . ?
N3 C21 1.344(2) . ?
N4 C27 1.348(2) . ?
N4 C31 1.352(2) . ?
N1 C19 1.343(2) . ?
N1 C15 1.349(2) . ?
N2 C26 1.489(2) . ?
N2 C20 1.497(2) . ?
N2 C32 1.491(2) . ?
C1 C2 1.424(2) . ?
C1 C6 1.416(2) . ?
C2 C3 1.413(2) . ?
C27 H27 0.9300 . ?
C27 C28 1.382(2) . ?
C31 C30 1.385(2) . ?
C31 C32 1.504(2) . ?
C26 H26A 0.9700 . ?
C26 H26B 0.9700 . ?
C26 C25 1.506(2) . ?
C6 C7 1.535(2) . ?
C6 C5 1.390(2) . ?
C19 C20 1.505(2) . ?
C19 C18 1.384(3) . ?
C3 C11 1.533(2) . ?
C3 C4 1.386(3) . ?
C30 H30 0.9300 . ?
C30 C29 1.388(3) . ?
C25 C24 1.381(2) . ?
C7 C9 1.534(2) . ?
C7 C8 1.543(2) . ?
C7 C10 1.537(2) . ?
C29 H29 0.9300 . ?
C29 C28 1.386(3) . ?
C15 H15 0.9300 . ?
C15 C16 1.379(3) . ?
C20 H20A 0.9700 . ?
C20 H20B 0.9700 . ?
C21 H21 0.9300 . ?
C21 C22 1.383(2) . ?
C32 H32A 0.9700 . ?
C32 H32B 0.9700 . ?
C11 C12 1.538(2) . ?
C11 C13 1.535(3) . ?
C11 C14 1.538(3) . ?
C9 H9A 0.9600 . ?
C9 H9B 0.9600 . ?
C9 H9C 0.9600 . ?
C5 H5 0.9300 . ?
C5 C4 1.401(3) . ?
C23 H23 0.9300 . ?
C23 C22 1.385(3) . ?
C23 C24 1.392(3) . ?
C4 H4 0.9300 . ?
C12 H12A 0.9600 . ?
C12 H12B 0.9600 . ?
C12 H12C 0.9600 . ?
C22 H22 0.9300 . ?
C24 H24 0.9300 . ?
C18 H18 0.9300 . ?
C18 C17 1.387(3) . ?
C16 H16 0.9300 . ?
C16 C17 1.385(3) . ?
C28 H28 0.9300 . ?
C13 H13A 0.9600 . ?
C13 H13B 0.9600 . ?
C13 H13C 0.9600 . ?
C8 H8A 0.9600 . ?
C8 H8B 0.9600 . ?
C8 H8C 0.9600 . ?
C10 H10A 0.9600 . ?
C10 H10B 0.9600 . ?
C10 H10C 0.9600 . ?
C17 H17 0.9300 . ?
C14 H14A 0.9600 . ?
C14 H14B 0.9600 . ?
C14 H14C 0.9600 . ?
Cl1 O5 1.4805(18) . ?
Cl1 O3A 1.434(9) . ?
Cl1 O6A 1.439(3) . ?
Cl1 O4A 1.437(3) . ?
O5 Cl1A 1.421(2) . ?
O6 Cl1A 1.456(5) . ?
O3 Cl1A 1.435(12) . ?
Cl1A O4 1.420(5) . ?
O7 H7A 0.8498 . ?
O7 H7B 0.8502 . ?

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
O1 Fe N3 95.20(5) . . ?
O1 Fe N4 88.23(5) . . ?
O1 Fe N1 179.03(5) . . ?
O1 Fe N2 94.18(5) . . ?
O2 Fe O1 85.84(5) . . ?
O2 Fe N3 97.45(5) . . ?
O2 Fe N4 96.76(5) . . ?
O2 Fe N1 94.38(6) . . ?
O2 Fe N2 179.31(5) . . ?
N3 Fe N2 83.24(6) . . ?
N4 Fe N3 165.58(6) . . ?
N4 Fe N1 92.68(6) . . ?
N4 Fe N2 82.55(6) . . ?
N1 Fe N3 83.83(6) . . ?
N1 Fe N2 85.61(6) . . ?
C1 O1 Fe 110.02(9) . . ?
C2 O2 Fe 111.65(9) . . ?
C25 N3 Fe 113.62(11) . . ?
C21 N3 Fe 125.99(11) . . ?
C21 N3 C25 119.46(14) . . ?
C27 N4 Fe 126.50(12) . . ?
C27 N4 C31 119.55(14) . . ?
C31 N4 Fe 113.94(11) . . ?
C19 N1 Fe 114.57(11) . . ?
C19 N1 C15 119.47(15) . . ?
C15 N1 Fe 125.04(12) . . ?
C26 N2 Fe 105.47(10) . . ?
C26 N2 C20 111.39(13) . . ?
C26 N2 C32 112.80(13) . . ?
C20 N2 Fe 109.67(10) . . ?
C32 N2 Fe 106.58(10) . . ?
C32 N2 C20 110.66(13) . . ?
O1 C1 C2 115.21(14) . . ?
O1 C1 C6 123.80(14) . . ?
C6 C1 C2 120.97(15) . . ?
O2 C2 C1 114.87(14) . . ?
O2 C2 C3 122.85(14) . . ?
C3 C2 C1 122.28(15) . . ?
N4 C27 H27 119.1 . . ?
N4 C27 C28 121.73(16) . . ?
C28 C27 H27 119.1 . . ?
N4 C31 C30 121.26(16) . . ?
N4 C31 C32 114.68(14) . . ?
C30 C31 C32 124.04(15) . . ?
N2 C26 H26A 110.2 . . ?
N2 C26 H26B 110.2 . . ?
N2 C26 C25 107.55(13) . . ?
H26A C26 H26B 108.5 . . ?
C25 C26 H26A 110.2 . . ?
C25 C26 H26B 110.2 . . ?
C1 C6 C7 122.04(15) . . ?
C5 C6 C1 115.55(15) . . ?
C5 C6 C7 122.37(15) . . ?
N1 C19 C20 116.02(15) . . ?
N1 C19 C18 121.69(16) . . ?
C18 C19 C20 122.26(16) . . ?
C2 C3 C11 121.40(15) . . ?
C4 C3 C2 115.43(15) . . ?
C4 C3 C11 123.16(15) . . ?
C31 C30 H30 120.5 . . ?
C31 C30 C29 119.10(16) . . ?
C29 C30 H30 120.5 . . ?
N3 C25 C26 113.52(14) . . ?
N3 C25 C24 121.70(15) . . ?
C24 C25 C26 124.78(15) . . ?
C6 C7 C8 109.01(14) . . ?
C6 C7 C10 111.51(14) . . ?
C9 C7 C6 111.13(13) . . ?
C9 C7 C8 109.23(15) . . ?
C9 C7 C10 107.32(15) . . ?
C10 C7 C8 108.58(14) . . ?
C30 C29 H29 120.3 . . ?
C28 C29 C30 119.38(16) . . ?
C28 C29 H29 120.3 . . ?
N1 C15 H15 119.2 . . ?
N1 C15 C16 121.55(17) . . ?
C16 C15 H15 119.2 . . ?
N2 C20 C19 112.31(13) . . ?
N2 C20 H20A 109.1 . . ?
N2 C20 H20B 109.1 . . ?
C19 C20 H20A 109.1 . . ?
C19 C20 H20B 109.1 . . ?
H20A C20 H20B 107.9 . . ?
N3 C21 H21 119.1 . . ?
N3 C21 C22 121.72(16) . . ?
C22 C21 H21 119.1 . . ?
N2 C32 C31 107.17(13) . . ?
N2 C32 H32A 110.3 . . ?
N2 C32 H32B 110.3 . . ?
C31 C32 H32A 110.3 . . ?
C31 C32 H32B 110.3 . . ?
H32A C32 H32B 108.5 . . ?
C3 C11 C12 109.47(14) . . ?
C3 C11 C13 110.24(14) . . ?
C3 C11 C14 111.61(16) . . ?
C12 C11 C14 107.87(15) . . ?
C13 C11 C12 109.41(16) . . ?
C13 C11 C14 108.18(16) . . ?
C7 C9 H9A 109.5 . . ?
C7 C9 H9B 109.5 . . ?
C7 C9 H9C 109.5 . . ?
H9A C9 H9B 109.5 . . ?
H9A C9 H9C 109.5 . . ?
H9B C9 H9C 109.5 . . ?
C6 C5 H5 118.4 . . ?
C6 C5 C4 123.19(16) . . ?
C4 C5 H5 118.4 . . ?
C22 C23 H23 120.3 . . ?
C22 C23 C24 119.41(16) . . ?
C24 C23 H23 120.3 . . ?
C3 C4 C5 122.56(16) . . ?
C3 C4 H4 118.7 . . ?
C5 C4 H4 118.7 . . ?
C11 C12 H12A 109.5 . . ?
C11 C12 H12B 109.5 . . ?
C11 C12 H12C 109.5 . . ?
H12A C12 H12B 109.5 . . ?
H12A C12 H12C 109.5 . . ?
H12B C12 H12C 109.5 . . ?
C21 C22 C23 118.94(16) . . ?
C21 C22 H22 120.5 . . ?
C23 C22 H22 120.5 . . ?
C25 C24 C23 118.77(16) . . ?
C25 C24 H24 120.6 . . ?
C23 C24 H24 120.6 . . ?
C19 C18 H18 120.5 . . ?
C19 C18 C17 118.91(18) . . ?
C17 C18 H18 120.5 . . ?
C15 C16 H16 120.4 . . ?
C15 C16 C17 119.18(17) . . ?
C17 C16 H16 120.4 . . ?
C27 C28 C29 118.95(17) . . ?
C27 C28 H28 120.5 . . ?
C29 C28 H28 120.5 . . ?
C11 C13 H13A 109.5 . . ?
C11 C13 H13B 109.5 . . ?
C11 C13 H13C 109.5 . . ?
H13A C13 H13B 109.5 . . ?
H13A C13 H13C 109.5 . . ?
H13B C13 H13C 109.5 . . ?
C7 C8 H8A 109.5 . . ?
C7 C8 H8B 109.5 . . ?
C7 C8 H8C 109.5 . . ?
H8A C8 H8B 109.5 . . ?
H8A C8 H8C 109.5 . . ?
H8B C8 H8C 109.5 . . ?
C7 C10 H10A 109.5 . . ?
C7 C10 H10B 109.5 . . ?
C7 C10 H10C 109.5 . . ?
H10A C10 H10B 109.5 . . ?
H10A C10 H10C 109.5 . . ?
H10B C10 H10C 109.5 . . ?
C18 C17 H17 120.4 . . ?
C16 C17 C18 119.18(18) . . ?
C16 C17 H17 120.4 . . ?
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 . . ?
O3A Cl1 O5 107.8(6) . . ?
O3A Cl1 O6A 109.3(6) . . ?
O3A Cl1 O4A 108.7(4) . . ?
O6A Cl1 O5 109.38(16) . . ?
O4A Cl1 O5 112.52(16) . . ?
O4A Cl1 O6A 109.0(2) . . ?
O5 Cl1A O6 101.1(3) . . ?
O5 Cl1A O3 109.3(8) . . ?
O3 Cl1A O6 109.0(7) . . ?
O4 Cl1A O5 116.8(3) . . ?
O4 Cl1A O6 108.9(4) . . ?
O4 Cl1A O3 111.1(6) . . ?
H7A O7 H7B 104.5 . . ?

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
Fe O1 C1 C2 -12.13(16) . . . . ?
Fe O1 C1 C6 169.64(12) . . . . ?
Fe O2 C2 C1 9.55(16) . . . . ?
Fe O2 C2 C3 -171.38(12) . . . . ?
Fe N3 C25 C26 -10.72(17) . . . . ?
Fe N3 C25 C24 168.94(13) . . . . ?
Fe N3 C21 C22 -166.85(13) . . . . ?
Fe N4 C27 C28 177.89(13) . . . . ?
Fe N4 C31 C30 -176.70(13) . . . . ?
Fe N4 C31 C32 4.30(18) . . . . ?
Fe N1 C19 C20 11.25(18) . . . . ?
Fe N1 C19 C18 -170.49(14) . . . . ?
Fe N1 C15 C16 168.35(14) . . . . ?
Fe N2 C26 C25 -42.87(14) . . . . ?
Fe N2 C20 C19 11.97(16) . . . . ?
Fe N2 C32 C31 40.70(14) . . . . ?
O1 Fe O2 C2 -12.99(10) . . . . ?
O1 C1 C2 O2 2.0(2) . . . . ?
O1 C1 C2 C3 -177.06(14) . . . . ?
O1 C1 C6 C7 -5.7(2) . . . . ?
O1 C1 C6 C5 176.48(14) . . . . ?
O2 C2 C3 C11 0.6(2) . . . . ?
O2 C2 C3 C4 -178.96(15) . . . . ?
N3 Fe O2 C2 -107.70(10) . . . . ?
N3 C25 C24 C23 -0.5(3) . . . . ?
N3 C21 C22 C23 -0.8(3) . . . . ?
N4 Fe O2 C2 74.73(11) . . . . ?
N4 C27 C28 C29 -0.9(3) . . . . ?
N4 C31 C30 C29 -1.7(3) . . . . ?
N4 C31 C32 N2 -30.35(19) . . . . ?
N1 Fe O2 C2 167.96(10) . . . . ?
N1 C19 C20 N2 -15.5(2) . . . . ?
N1 C19 C18 C17 1.3(3) . . . . ?
N1 C15 C16 C17 0.6(3) . . . . ?
N2 C26 C25 N3 36.25(18) . . . . ?
N2 C26 C25 C24 -143.39(16) . . . . ?
C1 C2 C3 C11 179.64(15) . . . . ?
C1 C2 C3 C4 0.0(2) . . . . ?
C1 C6 C7 C9 59.1(2) . . . . ?
C1 C6 C7 C8 -61.3(2) . . . . ?
C1 C6 C7 C10 178.81(15) . . . . ?
C1 C6 C5 C4 0.9(2) . . . . ?
C2 C1 C6 C7 176.15(14) . . . . ?
C2 C1 C6 C5 -1.6(2) . . . . ?
C2 C3 C11 C12 -61.4(2) . . . . ?
C2 C3 C11 C13 59.0(2) . . . . ?
C2 C3 C11 C14 179.27(16) . . . . ?
C2 C3 C4 C5 -0.8(3) . . . . ?
C27 N4 C31 C30 2.2(2) . . . . ?
C27 N4 C31 C32 -176.84(15) . . . . ?
C31 N4 C27 C28 -0.8(3) . . . . ?
C31 C30 C29 C28 0.0(3) . . . . ?
C26 N2 C20 C19 -104.41(16) . . . . ?
C26 N2 C32 C31 155.98(13) . . . . ?
C26 C25 C24 C23 179.09(16) . . . . ?
C6 C1 C2 O2 -179.71(13) . . . . ?
C6 C1 C2 C3 1.2(2) . . . . ?
C6 C5 C4 C3 0.3(3) . . . . ?
C19 N1 C15 C16 -0.1(3) . . . . ?
C19 C18 C17 C16 -0.8(3) . . . . ?
C30 C31 C32 N2 150.69(16) . . . . ?
C30 C29 C28 C27 1.3(3) . . . . ?
C25 N3 C21 C22 1.4(2) . . . . ?
C7 C6 C5 C4 -176.85(16) . . . . ?
C15 N1 C19 C20 -179.15(15) . . . . ?
C15 N1 C19 C18 -0.9(2) . . . . ?
C15 C16 C17 C18 -0.1(3) . . . . ?
C20 N2 C26 C25 76.04(16) . . . . ?
C20 N2 C32 C31 -78.48(16) . . . . ?
C20 C19 C18 C17 179.47(18) . . . . ?
C21 N3 C25 C26 179.68(14) . . . . ?
C21 N3 C25 C24 -0.7(2) . . . . ?
C32 N2 C26 C25 -158.81(13) . . . . ?
C32 N2 C20 C19 129.26(14) . . . . ?
C32 C31 C30 C29 177.16(16) . . . . ?
C11 C3 C4 C5 179.62(16) . . . . ?
C5 C6 C7 C9 -123.24(17) . . . . ?
C5 C6 C7 C8 116.33(18) . . . . ?
C5 C6 C7 C10 -3.5(2) . . . . ?
C4 C3 C11 C12 118.19(19) . . . . ?
C4 C3 C11 C13 -121.40(19) . . . . ?
C4 C3 C11 C14 -1.2(2) . . . . ?
C22 C23 C24 C25 1.0(3) . . . . ?
C24 C23 C22 C21 -0.4(3) . . . . ?
C18 C19 C20 N2 166.23(16) . . . . ?

_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
;
_oxdiff_exptl_absorpt_empirical_full_max 1.466
_oxdiff_exptl_absorpt_empirical_full_min 0.779
_symmetry_cell_setting           triclinic
_symmetry_space_group_name_h-m   'P -1'
_symmetry_int_tables_number      2
_chemical_absolute_configuration .

####################################################################### 
# 
# This file contains crystal structure data downloaded from the 
# Cambridge Structural Database (CSD) hosted by the Cambridge 
# Crystallographic Data Centre (CCDC).
# 
# Full information about CCDC data access policies and citation 
# guidelines are available at http://www.ccdc.cam.ac.uk/access/V1 
# 
# Audit and citation data items may have been added by the CCDC. 
# Please retain this information to preserve the provenance of 
# this file and to allow appropriate attribution of the data. 
# 
#######################################################################

data_tpafe36bf4_100_2
_database_code_depnum_ccdc_archive 'CCDC 2164130'
loop_
_audit_author_name
_audit_author_address
'Oleg Demidov'
;North Caucasus Federal University, Department of Chemistry
Russia
;
_audit_update_record             
;
2022-04-03 deposited with the CCDC.	2022-06-27 downloaded from the CCDC.
;
_audit_creation_date             2021-09-08
_audit_creation_method           
;
Olex2 1.3
(compiled 2020.11.12 svn.r5f609507 for OlexSys, GUI svn.r6272)
;
_shelx_SHELXL_version_number     2014/7
_chemical_name_systematic        
'(3,6-Di-tert-butylcatecholato)-(tris(2-pyridylmethyl)amine)-iron(iii) tetrafluoroborate'
_chemical_name_common            
'(3,6-Di-tert-butylcatecholato)-(tris(2-pyridylmethyl)amine)-iron(iii) tetrafluoroborate'
_chemical_formula_moiety         
'C32 H38 Fe N4 O2, 0.5(H2 O), B0.439 F2.242, B0.561 F1.758'
_chemical_formula_sum            'C32 H39 B F4 Fe N4 O2.50'
_chemical_compound_source        'Rostov-on-Don, Russia'
_chemical_formula_weight         662.33
_exptl_crystal_description       plate
_exptl_crystal_colour            violet
_diffrn_ambient_temperature      100.02(11)
_chemical_oxdiff_formula         'C32 H38 Fe N4 O2, B F4'
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'

_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.
;
_space_group_crystal_system      triclinic
_space_group_IT_number           2
_space_group_name_H-M_alt        'P -1'
_space_group_name_Hall           '-P 1'
loop_
_space_group_symop_operation_xyz
'x, y, z'
'-x, -y, -z'

_cell_length_a                   8.3740(3)
_cell_length_b                   10.2623(3)
_cell_length_c                   19.6717(6)
_cell_angle_alpha                97.060(2)
_cell_angle_beta                 93.064(3)
_cell_angle_gamma                106.882(3)
_cell_volume                     1598.31(9)
_cell_formula_units_Z            2
_cell_measurement_reflns_used    10714
_cell_measurement_temperature    100.02(11)
_cell_measurement_theta_max      76.0130
_cell_measurement_theta_min      4.5000
_shelx_estimated_absorpt_T_max   0.670
_shelx_estimated_absorpt_T_min   0.302
_exptl_absorpt_coefficient_mu    4.303
_exptl_absorpt_correction_T_max  0.971
_exptl_absorpt_correction_T_min  0.904
_exptl_absorpt_correction_type   analytical
_exptl_absorpt_process_details   
;
CrysAlisPro 1.171.40.67a (Rigaku Oxford Diffraction, 2019)
Analytical numeric absorption correction using a multifaceted crystal
			model based on expressions derived by R.C. Clark & J.S. Reid.
(Clark, R. C. & Reid, J. S. (1995). Acta Cryst. A51, 887-897)
Empirical absorption correction using spherical harmonics,
 implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_absorpt_special_details   ?
_exptl_crystal_colour_lustre     .
_exptl_crystal_colour_modifier   .
_exptl_crystal_colour_primary    violet
_exptl_crystal_density_diffrn    1.376
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    ?
_exptl_crystal_F_000             692
loop_
_exptl_crystal_face_index_h
_exptl_crystal_face_index_k
_exptl_crystal_face_index_l
_exptl_crystal_face_perp_dist
1 1 -13 0.1311
1 -3 12 0.1605
0 6 0 0.1691
4 1 5 0.0932
-5 1 -5 0.0917
5 1 2 0.0739
-5 1 -1 0.0761
-5 2 3 0.0761
5 0 -2 0.0825
0 -6 -1 0.1463
5 0 -6 0.1009
4 0 -9 0.1106
-3 1 12 0.1237
-1 1 12 0.1340
0 6 -1 0.1725
-1 0 -12 0.1312
-2 0 -11 0.1230
4 -2 9 0.1330
5 -2 5 0.1197
5 1 2 0.0759
5 2 -2 0.0867
4 1 -6 0.0985
-5 -1 1 0.0180

_exptl_crystal_size_max          0.366
_exptl_crystal_size_mid          0.286
_exptl_crystal_size_min          0.101
loop_
_exptl_oxdiff_crystal_face_indexfrac_h
_exptl_oxdiff_crystal_face_indexfrac_k
_exptl_oxdiff_crystal_face_indexfrac_l
_exptl_oxdiff_crystal_face_x
_exptl_oxdiff_crystal_face_y
_exptl_oxdiff_crystal_face_z
0.8883 0.8360 -12.6816 0.6080 0.7939 -0.0092
0.8985 -3.0600 11.8799 -0.3195 -0.9067 -0.2753
-0.4626 6.4180 0.4436 -0.0046 0.0081 1.0000
4.3472 0.5815 5.1317 0.5296 -0.7703 0.3551
-4.7333 1.0772 -5.3151 -0.5634 0.8185 -0.1126
4.9371 0.5004 1.5358 0.7526 -0.5772 0.3171
-5.3126 1.2318 -1.4712 -0.7925 0.6070 -0.0590
-5.3710 1.5173 2.5652 -0.9422 0.3325 0.0409
5.2386 -0.3015 -2.4402 0.9326 -0.3296 0.1471
0.4665 -6.4094 -0.5521 0.0092 -0.0010 -1.0000
4.8079 -0.3574 -6.2367 0.9975 -0.0253 0.0655
3.8018 0.3843 -9.3166 0.9543 0.2834 0.0949
-2.5265 0.7747 11.5214 -0.8106 -0.5587 0.1754
-0.9664 1.0882 12.2334 -0.5788 -0.7569 0.3034
-0.2957 6.4590 -1.0602 0.0767 0.0964 0.9924
-0.7328 0.2759 -12.4136 0.3280 0.9302 -0.1648
-2.2752 0.2038 -10.9338 0.0241 0.9746 -0.2228
3.8094 -1.8884 8.6139 0.2849 -0.9585 -0.0091
4.8154 -1.8681 5.2848 0.5672 -0.8236 -0.0092
4.8199 0.8518 1.5156 0.7390 -0.5649 0.3672
4.6560 1.6203 -2.0942 0.8516 -0.2996 0.4301
4.4566 1.3061 -5.8038 0.9474 -0.0232 0.3191
-4.9841 -0.7628 0.9865 -0.8537 0.4070 -0.3248

_exptl_transmission_factor_max   ?
_exptl_transmission_factor_min   ?
_diffrn_reflns_av_R_equivalents  0.0550
_diffrn_reflns_av_unetI/netI     0.0408
_diffrn_reflns_Laue_measured_fraction_full 1.000
_diffrn_reflns_Laue_measured_fraction_max 0.992
_diffrn_reflns_limit_h_max       10
_diffrn_reflns_limit_h_min       -10
_diffrn_reflns_limit_k_max       12
_diffrn_reflns_limit_k_min       -9
_diffrn_reflns_limit_l_max       24
_diffrn_reflns_limit_l_min       -24
_diffrn_reflns_number            32634
_diffrn_reflns_point_group_measured_fraction_full 1.000
_diffrn_reflns_point_group_measured_fraction_max 0.992
_diffrn_reflns_theta_full        67.684
_diffrn_reflns_theta_max         76.451
_diffrn_reflns_theta_min         4.550
_diffrn_ambient_environment      N~2~
_diffrn_detector                 'CCD plate'
_diffrn_detector_area_resol_mean 5.2529
_diffrn_detector_type            AtlasS2
_diffrn_measured_fraction_theta_full 1.000
_diffrn_measured_fraction_theta_max 0.992
_diffrn_measurement_details      
;
List of Runs (angles in degrees, time in seconds):

  # Type    Start    End  Width  tₑₓₚ   ω     θ     κ     φ   Frames
#--------------------------------------------------------------------------
  1  ω    -69.00  33.00   1.00    5.16    --  -40.60  57.00-120.00  102
  2  ω   -113.00 -12.00   1.00    5.16    --  -40.60 -57.00  90.00  101
  3  ω    -21.00  73.00   1.00    5.16    --   40.60 -77.00 -60.00   94
  4  ω      7.00  42.00   1.00    5.16    --   40.60  82.00  70.40   35
  5  ω     16.00 115.00   1.00    5.16    --   40.60  38.00  30.00   99
  6  ω    -34.00  65.00   1.00    5.16    --   40.60 -38.00 -30.00   99
  7  ω      6.00  81.00   1.00    5.16    --   40.60 -99.00-120.00   75
  8  ω     86.00 178.00   1.00   20.63    --  112.00  45.00   0.00   92
  9  ω     30.00 106.00   1.00   20.63    --  112.00 -95.00-120.00   76
 10  ω     36.00 109.00   1.00   20.63    --  112.00-111.00-180.00   73
 11  ω    104.00 178.00   1.00   20.63    --  112.00 111.00-180.00   74
 12  ω    103.00 178.00   1.00   20.63    --  112.00  77.00  90.00   75
 13  ω    104.00 178.00   1.00   20.63    --  112.00 111.00 -60.00   74
 14  ω     36.00 109.00   1.00   20.63    --  112.00-111.00 -30.00   73
 15  ω     40.00 141.00   1.00   20.63    --  112.00 -61.00-180.00  101
 16  ω     86.00 178.00   1.00   20.63    --  112.00  45.00  30.00   92
 17  ω     36.00 109.00   1.00   20.63    --  112.00-111.00 -90.00   73
 18  ω    104.00 178.00   1.00   20.63    --  112.00 111.00  30.00   74
 19  ω     30.00 106.00   1.00   20.63    --  112.00 -95.00-180.00   76
 20  ω    104.00 178.00   1.00   20.63    --  112.00 111.00   0.00   74
 21  ω     36.00 109.00   1.00   20.63    --  112.00-111.00  60.00   73
 22  ω     39.00 138.00   1.00   20.63    --  112.00 -45.00-120.00   99
 23  ω     36.00 109.00   1.00   20.63    --  112.00-113.00  16.00   73
 24  ω     36.00 140.00   1.00   20.63    --  112.00 -30.00   0.00  104
 25  ω     40.00 141.00   1.00   20.63    --  112.00 -61.00-120.00  101
 26  ω     39.00 138.00   1.00   20.63    --  112.00 -45.00   0.00   99
 27  ω     84.00 178.00   1.00   20.63    --  112.00  30.00 -30.00   94
 28  ω    103.00 178.00   1.00   20.63    --  112.00  77.00-120.00   75
 29  ω     30.00 106.00   1.00   20.63    --  112.00 -95.00 150.00   76
 30  ω     36.00 109.00   1.00   20.63    --  112.00-111.00 -60.00   73
 31  ω     30.00 106.00   1.00   20.63    --  112.00 -95.00-150.00   76
 32  ω    104.00 178.00   1.00   20.63    --  112.00 111.00 -30.00   74
 33  ω     39.00 138.00   1.00   20.63    --  112.00 -45.00 -60.00   99
 34  ω     36.00 140.00   1.00   20.63    --  112.00 -30.00-150.00  104
 35  ω     40.00 141.00   1.00   20.63    --  112.00 -61.00 120.00  101
 36  ω     36.00 145.00   1.00   20.63    --  112.00 -77.00 -30.00  109
 37  ω     36.00 109.00   1.00   20.63    --  112.00-111.00-150.00   73
 38  ω     36.00 109.00   1.00   20.63    --  112.00-111.00-120.00   73
 39  ω     36.00 109.00   1.00   20.63    --  112.00-111.00 120.00   73
 40  ω     33.00 146.00   1.00   20.63    --  112.00 -83.00   4.78  113
 41  ω    113.00 141.00   1.00   20.63    --  112.00  77.00-180.00   28
 42  ω    120.00 145.00   1.00   20.63    --  112.00 -77.00  90.00   25
 43  ω     65.00  93.00   1.00   20.63    --  112.00  13.00  -8.88   28
 44  ω     76.00 112.00   1.00   20.63    --  112.00 -15.00 -30.00   36
 45  ω    123.00 164.00   1.00   20.63    --  112.00 -15.00 -30.00   41
;
_diffrn_measurement_device       'four-circle diffractometer'
_diffrn_measurement_device_type  'SuperNova, Dual, Cu at home/near, AtlasS2'
_diffrn_measurement_method       'ω scans'
_diffrn_orient_matrix_type       
'CrysAlisPro convention (1999,Acta A55,543-557)'
_diffrn_orient_matrix_UB_11      0.1621694000
_diffrn_orient_matrix_UB_12      0.0134370000
_diffrn_orient_matrix_UB_13      -0.0356976000
_diffrn_orient_matrix_UB_21      -0.0952548000
_diffrn_orient_matrix_UB_22      -0.0008109000
_diffrn_orient_matrix_UB_23      -0.0693278000
_diffrn_orient_matrix_UB_31      0.0437948000
_diffrn_orient_matrix_UB_32      0.1579791000
_diffrn_orient_matrix_UB_33      0.0142044000
_diffrn_radiation_monochromator  mirror
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           'Cu K\a'
_diffrn_radiation_wavelength     1.54184
_diffrn_source                   'micro-focus sealed X-ray tube'
_diffrn_source_type              'SuperNova (Cu) X-ray Source'
_reflns_Friedel_coverage         0.000
_reflns_Friedel_fraction_full    .
_reflns_Friedel_fraction_max     .
_reflns_number_gt                6087
_reflns_number_total             6673
_reflns_odcompleteness_completeness 98.19
_reflns_odcompleteness_iscentric 1
_reflns_odcompleteness_theta     77.17
_reflns_special_details          
;
 Reflections were merged by SHELXL according to the crystal
 class for the calculation of statistics and refinement.
 
 _reflns_Friedel_fraction is defined as the number of unique
 Friedel pairs measured divided by the number that would be
 possible theoretically, ignoring centric projections and
 systematic absences.
;
_reflns_threshold_expression     'I > 2σ(I)'
_computing_cell_refinement       'CrysAlisPro 1.171.40.67a (Rigaku OD, 2019)'
_computing_data_collection       'CrysAlisPro 1.171.40.67a (Rigaku OD, 2019)'
_computing_data_reduction        'CrysAlisPro 1.171.40.67a (Rigaku OD, 2019)'
_computing_molecular_graphics    'Olex2 1.3 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 1.3 (Dolomanov et al., 2009)'
_computing_structure_refinement  'SHELXL 2014/7 (Sheldrick, 2015)'
_computing_structure_solution    'SHELXT 2014/5 (Sheldrick, 2014)'
_refine_diff_density_max         0.525
_refine_diff_density_min         -0.450
_refine_diff_density_rms         0.065
_refine_ls_extinction_coef       .
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.042
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     455
_refine_ls_number_reflns         6673
_refine_ls_number_restraints     0
_refine_ls_R_factor_all          0.0576
_refine_ls_R_factor_gt           0.0519
_refine_ls_restrained_S_all      1.042
_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)+(0.0558P)²+1.8116P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1264
_refine_ls_wR_factor_ref         0.1317
_refine_special_details          ?
_olex2_refinement_description    
;
1. 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, All O(H,H) groups
2. Uiso/Uaniso restraints and constraints
Uanis(F2) = Uanis(F2A)
3. Others
 Sof(F4)=Sof(F1)=Sof(B1A)=Sof(F3)=Sof(F2)=1-FVAR(1)
 Sof(F2A)=Sof(F3A)=Sof(B1)=Sof(F1A)=Sof(F4A)=FVAR(1)
 Fixed Sof: O1S(0.5) H1SA(0.5) H1SB(0.5)
4.a Free rotating group:
 O1S(H1SA,H1SB)
4.b Secondary CH2 refined with riding coordinates:
 C26(H26A,H26B), C20(H20A,H20B), C32(H32A,H32B)
4.c Aromatic/amide H refined with riding coordinates:
 C27(H27), C29(H29), C24(H24), C4(H4), C5(H5), C23(H23), C21(H21), C22(H22),
 C15(H15), C28(H28), C30(H30), C18(H18), C16(H16), C17(H17)
4.d Idealised Me refined as rotating group:
 C9(H9A,H9B,H9C), C8(H8A,H8B,H8C), C12(H12A,H12B,H12C), C13(H13A,H13B,H13C),
 C10(H10A,H10B,H10C), C14(H14A,H14B,H14C)
;
_atom_sites_solution_hydrogens   mixed
_atom_sites_solution_primary     dual
_atom_sites_solution_secondary   ?
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
Fe Fe 0.43354(5) 0.68086(4) 0.26611(2) 0.02195(11) Uani 1 1 d . . . . .
O2 O 0.3927(2) 0.71944(17) 0.17822(9) 0.0250(3) Uani 1 1 d . . . . .
O1 O 0.2944(2) 0.49956(18) 0.23312(9) 0.0242(3) Uani 1 1 d . . . . .
N4 N 0.6294(3) 0.6177(2) 0.24765(12) 0.0267(4) Uani 1 1 d . . . . .
N3 N 0.2554(3) 0.7435(2) 0.30919(11) 0.0248(4) Uani 1 1 d . . . . .
N1 N 0.5744(3) 0.8693(2) 0.30094(11) 0.0265(4) Uani 1 1 d . . . . .
N2 N 0.4810(3) 0.6391(2) 0.36050(11) 0.0264(4) Uani 1 1 d . . . . .
C1 C 0.2715(3) 0.4817(2) 0.16442(13) 0.0227(5) Uani 1 1 d . . . . .
C2 C 0.3236(3) 0.6043(3) 0.13383(13) 0.0244(5) Uani 1 1 d . . . . .
C25 C 0.2291(3) 0.7068(3) 0.37231(13) 0.0267(5) Uani 1 1 d . . . . .
C27 C 0.7226(3) 0.6406(3) 0.19440(14) 0.0298(5) Uani 1 1 d . . . . .
H27 H 0.6920 0.6893 0.1603 0.036 Uiso 1 1 calc R U . . .
C6 C 0.1955(3) 0.3524(3) 0.12366(13) 0.0254(5) Uani 1 1 d . . . . .
C3 C 0.3014(3) 0.6033(3) 0.06226(13) 0.0282(5) Uani 1 1 d . . . . .
C31 C 0.6705(3) 0.5469(3) 0.29604(14) 0.0288(5) Uani 1 1 d . . . . .
C7 C 0.1486(3) 0.2179(3) 0.15486(14) 0.0290(5) Uani 1 1 d . . . . .
C26 C 0.3161(3) 0.6049(3) 0.39004(13) 0.0295(5) Uani 1 1 d . . . . .
H26A H 0.3330 0.6100 0.4406 0.035 Uiso 1 1 calc R U . . .
H26B H 0.2474 0.5103 0.3706 0.035 Uiso 1 1 calc R U . . .
C19 C 0.6291(3) 0.8904(3) 0.36791(14) 0.0295(5) Uani 1 1 d . . . . .
C11 C 0.3570(4) 0.7361(3) 0.03030(14) 0.0329(6) Uani 1 1 d . . . . .
C29 C 0.9076(3) 0.5265(3) 0.23812(17) 0.0355(6) Uani 1 1 d . . . . .
H29 H 1.0046 0.4967 0.2353 0.043 Uiso 1 1 calc R U . . .
C24 C 0.1318(3) 0.7622(3) 0.41497(14) 0.0314(6) Uani 1 1 d . . . . .
H24 H 0.1134 0.7348 0.4590 0.038 Uiso 1 1 calc R U . . .
C4 C 0.2239(4) 0.4759(3) 0.02369(14) 0.0331(6) Uani 1 1 d . . . . .
H4 H 0.2038 0.4703 -0.0247 0.040 Uiso 1 1 calc R U . . .
C5 C 0.1741(4) 0.3550(3) 0.05346(14) 0.0317(6) Uani 1 1 d . . . . .
H5 H 0.1231 0.2705 0.0241 0.038 Uiso 1 1 calc R U . . .
C23 C 0.0617(4) 0.8581(3) 0.39265(15) 0.0336(6) Uani 1 1 d . . . . .
H23 H -0.0036 0.8985 0.4216 0.040 Uiso 1 1 calc R U . . .
C20 C 0.6044(3) 0.7629(3) 0.40188(14) 0.0312(6) Uani 1 1 d . . . . .
H20A H 0.7135 0.7446 0.4087 0.037 Uiso 1 1 calc R U . . .
H20B H 0.5648 0.7793 0.4478 0.037 Uiso 1 1 calc R U . . .
C21 C 0.1851(3) 0.8343(3) 0.28701(14) 0.0271(5) Uani 1 1 d . . . . .
H21 H 0.2024 0.8581 0.2422 0.033 Uiso 1 1 calc R U . . .
C22 C 0.0878(4) 0.8944(3) 0.32770(15) 0.0326(6) Uani 1 1 d . . . . .
H22 H 0.0400 0.9593 0.3113 0.039 Uiso 1 1 calc R U . . .
C15 C 0.5942(3) 0.9783(3) 0.26683(15) 0.0306(5) Uani 1 1 d . . . . .
H15 H 0.5552 0.9634 0.2194 0.037 Uiso 1 1 calc R U . . .
C9 C 0.0242(4) 0.2211(3) 0.20924(15) 0.0319(6) Uani 1 1 d . . . . .
H9A H 0.0774 0.2945 0.2474 0.048 Uiso 1 1 calc R U . . .
H9B H -0.0088 0.1324 0.2265 0.048 Uiso 1 1 calc R U . . .
H9C H -0.0754 0.2383 0.1885 0.048 Uiso 1 1 calc R U . . .
C32 C 0.5511(4) 0.5214(3) 0.35105(14) 0.0313(6) Uani 1 1 d . . . . .
H32A H 0.4600 0.4341 0.3369 0.038 Uiso 1 1 calc R U . . .
H32B H 0.6111 0.5147 0.3946 0.038 Uiso 1 1 calc R U . . .
C28 C 0.8618(4) 0.5952(3) 0.18783(16) 0.0351(6) Uani 1 1 d . . . . .
H28 H 0.9250 0.6110 0.1494 0.042 Uiso 1 1 calc R U . . .
C30 C 0.8100(3) 0.5015(3) 0.29308(16) 0.0336(6) Uani 1 1 d . . . . .
H30 H 0.8391 0.4539 0.3279 0.040 Uiso 1 1 calc R U . . .
C8 C 0.3075(4) 0.1973(3) 0.18810(17) 0.0364(6) Uani 1 1 d . . . . .
H8A H 0.3847 0.1909 0.1530 0.055 Uiso 1 1 calc R U . . .
H8B H 0.2777 0.1122 0.2087 0.055 Uiso 1 1 calc R U . . .
H8C H 0.3618 0.2754 0.2239 0.055 Uiso 1 1 calc R U . . .
C12 C 0.2605(4) 0.8347(3) 0.05838(15) 0.0355(6) Uani 1 1 d . . . . .
H12A H 0.1400 0.7911 0.0463 0.053 Uiso 1 1 calc R U . . .
H12B H 0.2965 0.9200 0.0382 0.053 Uiso 1 1 calc R U . . .
H12C H 0.2834 0.8558 0.1085 0.053 Uiso 1 1 calc R U . . .
C18 C 0.7077(4) 1.0203(3) 0.40284(17) 0.0410(7) Uani 1 1 d . . . . .
H18 H 0.7475 1.0328 0.4500 0.049 Uiso 1 1 calc R U . . .
C16 C 0.6695(4) 1.1102(3) 0.29904(17) 0.0392(7) Uani 1 1 d . . . . .
H16 H 0.6816 1.1859 0.2743 0.047 Uiso 1 1 calc R U . . .
C13 C 0.5458(4) 0.8055(3) 0.04786(16) 0.0398(7) Uani 1 1 d . . . . .
H13A H 0.5702 0.8305 0.0978 0.060 Uiso 1 1 calc R U . . .
H13B H 0.5808 0.8886 0.0258 0.060 Uiso 1 1 calc R U . . .
H13C H 0.6071 0.7417 0.0311 0.060 Uiso 1 1 calc R U . . .
C10 C 0.0641(4) 0.0935(3) 0.09968(16) 0.0374(6) Uani 1 1 d . . . . .
H10A H -0.0383 0.1053 0.0783 0.056 Uiso 1 1 calc R U . . .
H10B H 0.0355 0.0093 0.1211 0.056 Uiso 1 1 calc R U . . .
H10C H 0.1410 0.0866 0.0645 0.056 Uiso 1 1 calc R U . . .
C17 C 0.7276(4) 1.1320(3) 0.36782(19) 0.0467(8) Uani 1 1 d . . . . .
H17 H 0.7805 1.2227 0.3908 0.056 Uiso 1 1 calc R U . . .
C14 C 0.3216(5) 0.7088(3) -0.04854(15) 0.0447(8) Uani 1 1 d . . . . .
H14A H 0.3841 0.6480 -0.0678 0.067 Uiso 1 1 calc R U . . .
H14B H 0.3568 0.7961 -0.0670 0.067 Uiso 1 1 calc R U . . .
H14C H 0.2013 0.6648 -0.0610 0.067 Uiso 1 1 calc R U . . .
O1S O -0.0774(9) 0.4433(6) 0.4484(3) 0.0640(15) Uani 0.5 1 d G . P A 2
H1SA H -0.0154 0.4210 0.4776 0.096 Uiso 0.5 1 d G U P A 2
H1SB H -0.1282 0.4904 0.4725 0.096 Uiso 0.5 1 d G U P A 2
F2A F 0.1955(14) 0.2453(11) 0.3692(5) 0.0575(18) Uani 0.561(6) 1 d . . P B 1
F3A F 0.0555(5) 0.3492(4) 0.4424(2) 0.0584(13) Uani 0.561(6) 1 d . . P B 1
B1 B 0.219(2) 0.262(2) 0.4425(10) 0.052(4) Uani 0.561(6) 1 d . . P B 2
F1A F 0.122(3) 0.157(2) 0.4692(9) 0.047(3) Uani 0.561(6) 1 d . . P B 1
F4A F 0.3226(7) 0.3626(4) 0.4734(2) 0.0602(16) Uani 0.561(6) 1 d . . P B 1
F4 F 0.2105(9) 0.3752(4) 0.4897(2) 0.0505(15) Uani 0.439(6) 1 d . . P B 2
F1 F 0.137(4) 0.147(3) 0.4683(11) 0.057(6) Uani 0.439(6) 1 d . . P B 2
B1A B 0.176(2) 0.281(2) 0.4385(10) 0.025(3) Uani 0.439(6) 1 d . . P B 1
F3 F 0.3896(7) 0.2717(7) 0.4376(3) 0.070(2) Uani 0.439(6) 1 d . . P B 2
F2 F 0.1488(18) 0.2631(15) 0.3806(7) 0.0575(18) Uani 0.439(6) 1 d . . P B 2


_geom_special_details            
;
 All esds (except the esd in the dihedral angle between two l.s. planes)
 are estimated using the full covariance matrix.  The cell esds are taken
 into account individually in the estimation of esds in distances, angles
 and torsion angles; correlations between esds in cell parameters are only
 used when they are defined by crystal symmetry.  An approximate (isotropic)
 treatment of cell esds is used for estimating esds involving l.s. planes.
;
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
Fe O2 1.8566(18) . ?
Fe O1 1.8984(18) . ?
Fe N4 1.966(2) . ?
Fe N3 1.978(2) . ?
Fe N1 1.966(2) . ?
Fe N2 2.002(2) . ?
O2 C2 1.338(3) . ?
O1 C1 1.337(3) . ?
N4 C27 1.343(4) . ?
N4 C31 1.354(4) . ?
N3 C25 1.352(3) . ?
N3 C21 1.340(3) . ?
N1 C19 1.341(4) . ?
N1 C15 1.348(4) . ?
N2 C26 1.491(3) . ?
N2 C20 1.496(3) . ?
N2 C32 1.486(3) . ?
C1 C2 1.425(4) . ?
C1 C6 1.415(3) . ?
C2 C3 1.409(4) . ?
C25 C26 1.500(4) . ?
C25 C24 1.384(4) . ?
C27 H27 0.9500 . ?
C27 C28 1.382(4) . ?
C6 C7 1.535(4) . ?
C6 C5 1.387(4) . ?
C3 C11 1.531(4) . ?
C3 C4 1.384(4) . ?
C31 C32 1.507(4) . ?
C31 C30 1.380(4) . ?
C7 C9 1.537(4) . ?
C7 C8 1.532(4) . ?
C7 C10 1.536(4) . ?
C26 H26A 0.9900 . ?
C26 H26B 0.9900 . ?
C19 C20 1.508(4) . ?
C19 C18 1.378(4) . ?
C11 C12 1.539(4) . ?
C11 C13 1.534(5) . ?
C11 C14 1.539(4) . ?
C29 H29 0.9500 . ?
C29 C28 1.382(4) . ?
C29 C30 1.394(5) . ?
C24 H24 0.9500 . ?
C24 C23 1.386(4) . ?
C4 H4 0.9500 . ?
C4 C5 1.401(4) . ?
C5 H5 0.9500 . ?
C23 H23 0.9500 . ?
C23 C22 1.385(4) . ?
C20 H20A 0.9900 . ?
C20 H20B 0.9900 . ?
C21 H21 0.9500 . ?
C21 C22 1.388(4) . ?
C22 H22 0.9500 . ?
C15 H15 0.9500 . ?
C15 C16 1.372(4) . ?
C9 H9A 0.9800 . ?
C9 H9B 0.9800 . ?
C9 H9C 0.9800 . ?
C32 H32A 0.9900 . ?
C32 H32B 0.9900 . ?
C28 H28 0.9500 . ?
C30 H30 0.9500 . ?
C8 H8A 0.9800 . ?
C8 H8B 0.9800 . ?
C8 H8C 0.9800 . ?
C12 H12A 0.9800 . ?
C12 H12B 0.9800 . ?
C12 H12C 0.9800 . ?
C18 H18 0.9500 . ?
C18 C17 1.383(5) . ?
C16 H16 0.9500 . ?
C16 C17 1.382(5) . ?
C13 H13A 0.9800 . ?
C13 H13B 0.9800 . ?
C13 H13C 0.9800 . ?
C10 H10A 0.9800 . ?
C10 H10B 0.9800 . ?
C10 H10C 0.9800 . ?
C17 H17 0.9500 . ?
C14 H14A 0.9800 . ?
C14 H14B 0.9800 . ?
C14 H14C 0.9800 . ?
O1S H1SA 0.8499 . ?
O1S H1SB 0.8509 . ?
F2A B1A 1.40(2) . ?
F3A B1A 1.385(14) . ?
B1 F4 1.41(2) . ?
B1 F1 1.35(3) . ?
B1 F3 1.41(2) . ?
B1 F2 1.33(2) . ?
F1A B1A 1.44(3) . ?
F4A B1A 1.36(2) . ?

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 Fe O1 85.93(8) . . ?
O2 Fe N4 96.58(9) . . ?
O2 Fe N3 97.69(8) . . ?
O2 Fe N1 94.19(9) . . ?
O2 Fe N2 179.13(9) . . ?
O1 Fe N4 88.52(8) . . ?
O1 Fe N3 95.36(8) . . ?
O1 Fe N1 179.04(8) . . ?
O1 Fe N2 94.24(8) . . ?
N4 Fe N3 165.44(9) . . ?
N4 Fe N1 92.41(9) . . ?
N4 Fe N2 82.57(9) . . ?
N3 Fe N2 83.15(9) . . ?
N1 Fe N3 83.69(9) . . ?
N1 Fe N2 85.65(9) . . ?
C2 O2 Fe 111.52(15) . . ?
C1 O1 Fe 109.82(15) . . ?
C27 N4 Fe 126.70(19) . . ?
C27 N4 C31 119.7(2) . . ?
C31 N4 Fe 113.63(18) . . ?
C25 N3 Fe 113.47(17) . . ?
C21 N3 Fe 125.79(18) . . ?
C21 N3 C25 119.7(2) . . ?
C19 N1 Fe 114.61(18) . . ?
C19 N1 C15 119.3(2) . . ?
C15 N1 Fe 125.10(19) . . ?
C26 N2 Fe 105.24(15) . . ?
C26 N2 C20 111.4(2) . . ?
C20 N2 Fe 109.35(16) . . ?
C32 N2 Fe 106.22(16) . . ?
C32 N2 C26 113.2(2) . . ?
C32 N2 C20 111.1(2) . . ?
O1 C1 C2 115.3(2) . . ?
O1 C1 C6 123.6(2) . . ?
C6 C1 C2 121.0(2) . . ?
O2 C2 C1 114.9(2) . . ?
O2 C2 C3 123.0(2) . . ?
C3 C2 C1 122.1(2) . . ?
N3 C25 C26 113.6(2) . . ?
N3 C25 C24 121.2(2) . . ?
C24 C25 C26 125.2(2) . . ?
N4 C27 H27 119.1 . . ?
N4 C27 C28 121.8(3) . . ?
C28 C27 H27 119.1 . . ?
C1 C6 C7 122.0(2) . . ?
C5 C6 C1 115.5(2) . . ?
C5 C6 C7 122.4(2) . . ?
C2 C3 C11 121.4(2) . . ?
C4 C3 C2 115.7(2) . . ?
C4 C3 C11 122.9(2) . . ?
N4 C31 C32 114.7(2) . . ?
N4 C31 C30 121.3(3) . . ?
C30 C31 C32 124.1(3) . . ?
C6 C7 C9 110.9(2) . . ?
C6 C7 C10 111.3(2) . . ?
C8 C7 C6 109.3(2) . . ?
C8 C7 C9 109.5(2) . . ?
C8 C7 C10 108.7(2) . . ?
C10 C7 C9 107.1(2) . . ?
N2 C26 C25 107.9(2) . . ?
N2 C26 H26A 110.1 . . ?
N2 C26 H26B 110.1 . . ?
C25 C26 H26A 110.1 . . ?
C25 C26 H26B 110.1 . . ?
H26A C26 H26B 108.4 . . ?
N1 C19 C20 115.9(2) . . ?
N1 C19 C18 122.0(3) . . ?
C18 C19 C20 122.1(3) . . ?
C3 C11 C12 109.4(2) . . ?
C3 C11 C13 110.1(2) . . ?
C3 C11 C14 111.8(2) . . ?
C12 C11 C14 107.9(2) . . ?
C13 C11 C12 109.5(2) . . ?
C13 C11 C14 108.0(3) . . ?
C28 C29 H29 120.3 . . ?
C28 C29 C30 119.3(3) . . ?
C30 C29 H29 120.3 . . ?
C25 C24 H24 120.4 . . ?
C25 C24 C23 119.2(3) . . ?
C23 C24 H24 120.4 . . ?
C3 C4 H4 118.8 . . ?
C3 C4 C5 122.4(3) . . ?
C5 C4 H4 118.8 . . ?
C6 C5 C4 123.3(2) . . ?
C6 C5 H5 118.4 . . ?
C4 C5 H5 118.4 . . ?
C24 C23 H23 120.3 . . ?
C22 C23 C24 119.3(3) . . ?
C22 C23 H23 120.3 . . ?
N2 C20 C19 112.5(2) . . ?
N2 C20 H20A 109.1 . . ?
N2 C20 H20B 109.1 . . ?
C19 C20 H20A 109.1 . . ?
C19 C20 H20B 109.1 . . ?
H20A C20 H20B 107.8 . . ?
N3 C21 H21 119.1 . . ?
N3 C21 C22 121.8(3) . . ?
C22 C21 H21 119.1 . . ?
C23 C22 C21 118.8(3) . . ?
C23 C22 H22 120.6 . . ?
C21 C22 H22 120.6 . . ?
N1 C15 H15 119.3 . . ?
N1 C15 C16 121.5(3) . . ?
C16 C15 H15 119.3 . . ?
C7 C9 H9A 109.5 . . ?
C7 C9 H9B 109.5 . . ?
C7 C9 H9C 109.5 . . ?
H9A C9 H9B 109.5 . . ?
H9A C9 H9C 109.5 . . ?
H9B C9 H9C 109.5 . . ?
N2 C32 C31 107.3(2) . . ?
N2 C32 H32A 110.3 . . ?
N2 C32 H32B 110.3 . . ?
C31 C32 H32A 110.3 . . ?
C31 C32 H32B 110.3 . . ?
H32A C32 H32B 108.5 . . ?
C27 C28 C29 118.9(3) . . ?
C27 C28 H28 120.5 . . ?
C29 C28 H28 120.5 . . ?
C31 C30 C29 119.0(3) . . ?
C31 C30 H30 120.5 . . ?
C29 C30 H30 120.5 . . ?
C7 C8 H8A 109.5 . . ?
C7 C8 H8B 109.5 . . ?
C7 C8 H8C 109.5 . . ?
H8A C8 H8B 109.5 . . ?
H8A C8 H8C 109.5 . . ?
H8B C8 H8C 109.5 . . ?
C11 C12 H12A 109.5 . . ?
C11 C12 H12B 109.5 . . ?
C11 C12 H12C 109.5 . . ?
H12A C12 H12B 109.5 . . ?
H12A C12 H12C 109.5 . . ?
H12B C12 H12C 109.5 . . ?
C19 C18 H18 120.7 . . ?
C19 C18 C17 118.7(3) . . ?
C17 C18 H18 120.7 . . ?
C15 C16 H16 120.3 . . ?
C15 C16 C17 119.4(3) . . ?
C17 C16 H16 120.3 . . ?
C11 C13 H13A 109.5 . . ?
C11 C13 H13B 109.5 . . ?
C11 C13 H13C 109.5 . . ?
H13A C13 H13B 109.5 . . ?
H13A C13 H13C 109.5 . . ?
H13B C13 H13C 109.5 . . ?
C7 C10 H10A 109.5 . . ?
C7 C10 H10B 109.5 . . ?
C7 C10 H10C 109.5 . . ?
H10A C10 H10B 109.5 . . ?
H10A C10 H10C 109.5 . . ?
H10B C10 H10C 109.5 . . ?
C18 C17 H17 120.4 . . ?
C16 C17 C18 119.2(3) . . ?
C16 C17 H17 120.4 . . ?
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 . . ?
H1SA O1S H1SB 104.4 . . ?
F1 B1 F4 106.4(19) . . ?
F1 B1 F3 111.3(18) . . ?
F3 B1 F4 108.3(14) . . ?
F2 B1 F4 111.4(12) . . ?
F2 B1 F1 110.6(19) . . ?
F2 B1 F3 108.9(16) . . ?
F2A B1A F1A 108.6(17) . . ?
F3A B1A F2A 108.7(11) . . ?
F3A B1A F1A 109.7(16) . . ?
F4A B1A F2A 111.4(14) . . ?
F4A B1A F3A 109.9(15) . . ?
F4A B1A F1A 108.6(13) . . ?

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
Fe O2 C2 C1 9.9(3) . . . . ?
Fe O2 C2 C3 -170.92(19) . . . . ?
Fe O1 C1 C2 -12.3(2) . . . . ?
Fe O1 C1 C6 170.02(19) . . . . ?
Fe N4 C27 C28 177.7(2) . . . . ?
Fe N4 C31 C32 4.5(3) . . . . ?
Fe N4 C31 C30 -176.49(19) . . . . ?
Fe N3 C25 C26 -11.0(3) . . . . ?
Fe N3 C25 C24 168.2(2) . . . . ?
Fe N3 C21 C22 -166.1(2) . . . . ?
Fe N1 C19 C20 11.9(3) . . . . ?
Fe N1 C19 C18 -170.2(2) . . . . ?
Fe N1 C15 C16 168.0(2) . . . . ?
Fe N2 C26 C25 -42.9(2) . . . . ?
Fe N2 C20 C19 12.4(3) . . . . ?
Fe N2 C32 C31 41.4(2) . . . . ?
O2 Fe O1 C1 14.19(15) . . . . ?
O2 C2 C3 C11 0.4(4) . . . . ?
O2 C2 C3 C4 -178.4(2) . . . . ?
O1 Fe O2 C2 -13.35(16) . . . . ?
O1 C1 C2 O2 1.9(3) . . . . ?
O1 C1 C2 C3 -177.3(2) . . . . ?
O1 C1 C6 C7 -6.5(4) . . . . ?
O1 C1 C6 C5 176.6(2) . . . . ?
N4 Fe O2 C2 74.69(16) . . . . ?
N4 Fe O1 C1 -82.51(16) . . . . ?
N4 C27 C28 C29 -1.1(4) . . . . ?
N4 C31 C32 N2 -31.1(3) . . . . ?
N4 C31 C30 C29 -1.6(4) . . . . ?
N3 Fe O2 C2 -108.22(16) . . . . ?
N3 Fe O1 C1 111.55(15) . . . . ?
N3 C25 C26 N2 36.6(3) . . . . ?
N3 C25 C24 C23 -0.7(4) . . . . ?
N3 C21 C22 C23 -0.7(4) . . . . ?
N1 Fe O2 C2 167.60(16) . . . . ?
N1 C19 C20 N2 -16.3(3) . . . . ?
N1 C19 C18 C17 1.3(5) . . . . ?
N1 C15 C16 C17 0.5(5) . . . . ?
N2 Fe O1 C1 -164.95(15) . . . . ?
C1 C2 C3 C11 179.5(2) . . . . ?
C1 C2 C3 C4 0.8(4) . . . . ?
C1 C6 C7 C9 59.4(3) . . . . ?
C1 C6 C7 C8 -61.4(3) . . . . ?
C1 C6 C7 C10 178.5(2) . . . . ?
C1 C6 C5 C4 0.3(4) . . . . ?
C2 C1 C6 C7 176.0(2) . . . . ?
C2 C1 C6 C5 -0.9(3) . . . . ?
C2 C3 C11 C12 -61.2(3) . . . . ?
C2 C3 C11 C13 59.2(3) . . . . ?
C2 C3 C11 C14 179.4(3) . . . . ?
C2 C3 C4 C5 -1.5(4) . . . . ?
C25 N3 C21 C22 1.3(4) . . . . ?
C25 C24 C23 C22 1.2(4) . . . . ?
C27 N4 C31 C32 -176.8(2) . . . . ?
C27 N4 C31 C30 2.2(4) . . . . ?
C6 C1 C2 O2 179.6(2) . . . . ?
C6 C1 C2 C3 0.4(4) . . . . ?
C3 C4 C5 C6 1.0(5) . . . . ?
C31 N4 C27 C28 -0.9(4) . . . . ?
C7 C6 C5 C4 -176.7(3) . . . . ?
C26 N2 C20 C19 -103.5(3) . . . . ?
C26 N2 C32 C31 156.4(2) . . . . ?
C26 C25 C24 C23 178.5(3) . . . . ?
C19 N1 C15 C16 0.2(4) . . . . ?
C19 C18 C17 C16 -0.5(5) . . . . ?
C11 C3 C4 C5 179.8(3) . . . . ?
C24 C25 C26 N2 -142.6(3) . . . . ?
C24 C23 C22 C21 -0.6(4) . . . . ?
C4 C3 C11 C12 117.5(3) . . . . ?
C4 C3 C11 C13 -122.1(3) . . . . ?
C4 C3 C11 C14 -2.0(4) . . . . ?
C5 C6 C7 C9 -123.9(3) . . . . ?
C5 C6 C7 C8 115.3(3) . . . . ?
C5 C6 C7 C10 -4.8(4) . . . . ?
C20 N2 C26 C25 75.4(3) . . . . ?
C20 N2 C32 C31 -77.4(3) . . . . ?
C20 C19 C18 C17 179.1(3) . . . . ?
C21 N3 C25 C26 -179.8(2) . . . . ?
C21 N3 C25 C24 -0.6(4) . . . . ?
C15 N1 C19 C20 -179.1(2) . . . . ?
C15 N1 C19 C18 -1.1(4) . . . . ?
C15 C16 C17 C18 -0.3(5) . . . . ?
C32 N2 C26 C25 -158.5(2) . . . . ?
C32 N2 C20 C19 129.3(2) . . . . ?
C32 C31 C30 C29 177.4(2) . . . . ?
C28 C29 C30 C31 -0.4(4) . . . . ?
C30 C31 C32 N2 149.9(2) . . . . ?
C30 C29 C28 C27 1.7(4) . . . . ?
C18 C19 C20 N2 165.8(3) . . . . ?

_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
;
_oxdiff_exptl_absorpt_empirical_full_max 2.016
_oxdiff_exptl_absorpt_empirical_full_min 0.615
_symmetry_cell_setting           triclinic
_symmetry_space_group_name_h-m   'P -1'
_symmetry_int_tables_number      2
_chemical_absolute_configuration .

####################################################################### 
# 
# This file contains crystal structure data downloaded from the 
# Cambridge Structural Database (CSD) hosted by the Cambridge 
# Crystallographic Data Centre (CCDC).
# 
# Full information about CCDC data access policies and citation 
# guidelines are available at http://www.ccdc.cam.ac.uk/access/V1 
# 
# Audit and citation data items may have been added by the CCDC. 
# Please retain this information to preserve the provenance of 
# this file and to allow appropriate attribution of the data. 
# 
#######################################################################

data_tpafe36bf4
_database_code_depnum_ccdc_archive 'CCDC 2164132'
loop_
_audit_author_name
_audit_author_address
'Oleg Demidov'
;North Caucasus Federal University, Department of Chemistry
Russia
;
_audit_update_record             
;
2022-04-03 deposited with the CCDC.	2022-06-27 downloaded from the CCDC.
;
_audit_creation_date             2021-09-08
_audit_creation_method           
;
Olex2 1.3
(compiled 2020.11.12 svn.r5f609507 for OlexSys, GUI svn.r6272)
;
_shelx_SHELXL_version_number     2014/7
_chemical_name_systematic        
'3 - (3,6-Di-tert-butylcatecholato)-(tris(2-pyridylmethyl)amine)-iron(iii) tetrafluoroborate'
_chemical_name_common            
'3 - (3,6-Di-tert-butylcatecholato)-(tris(2-pyridylmethyl)amine)-iron(iii) tetrafluoroborate'
_chemical_formula_moiety         'C32 H38 Fe N4 O2, B F4, 0.333(H2 O)'
_chemical_formula_sum            'C32 H38.67 B F4 Fe N4 O2.33'
_chemical_compound_source        'Rostov-on-Don, Russia'
_chemical_formula_weight         659.27
_exptl_crystal_description       plate
_exptl_crystal_colour            violet
_diffrn_ambient_temperature      293(2)
_chemical_oxdiff_formula         'C32 H38 B F4 Fe N4 O2'
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'

_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.
;
_space_group_crystal_system      triclinic
_space_group_IT_number           2
_space_group_name_H-M_alt        'P -1'
_space_group_name_Hall           '-P 1'
loop_
_space_group_symop_operation_xyz
'x, y, z'
'-x, -y, -z'

_cell_length_a                   8.5955(5)
_cell_length_b                   10.2994(4)
_cell_length_c                   20.1677(8)
_cell_angle_alpha                94.460(3)
_cell_angle_beta                 94.614(4)
_cell_angle_gamma                106.445(4)
_cell_volume                     1697.36(14)
_cell_formula_units_Z            2
_cell_measurement_reflns_used    5129
_cell_measurement_temperature    293(2)
_cell_measurement_theta_max      72.6600
_cell_measurement_theta_min      4.4210
_shelx_estimated_absorpt_T_max   0.567
_shelx_estimated_absorpt_T_min   0.270
_exptl_absorpt_coefficient_mu    4.046
_exptl_absorpt_correction_T_max  0.797
_exptl_absorpt_correction_T_min  0.548
_exptl_absorpt_correction_type   analytical
_exptl_absorpt_process_details   
;
CrysAlisPro 1.171.40.67a (Rigaku Oxford Diffraction, 2019)
Analytical numeric absorption correction using a multifaceted crystal
			model based on expressions derived by R.C. Clark & J.S. Reid.
(Clark, R. C. & Reid, J. S. (1995). Acta Cryst. A51, 887-897)
Empirical absorption correction using spherical harmonics,
 implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_absorpt_special_details   ?
_exptl_crystal_colour_lustre     .
_exptl_crystal_colour_modifier   .
_exptl_crystal_colour_primary    violet
_exptl_crystal_density_diffrn    1.290
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    ?
_exptl_crystal_F_000             689
loop_
_exptl_crystal_face_index_h
_exptl_crystal_face_index_k
_exptl_crystal_face_index_l
_exptl_crystal_face_perp_dist
-5 4 2 0.1412
-5 1 4 0.0885
5 -1 0 0.0794
-5 -1 1 0.0745
5 0 4 0.1143
-5 -1 -2 0.1115
-4 -1 -6 0.1553
2 5 2 0.1461
2 -7 2 0.1547
0 0 13 0.2090
0 -1 -13 0.2122
-3 6 2 0.1733
-3 0 12 0.1848
6 -3 -1 0.1023
5 -1 -4 0.0891
-5 1 3 0.0919
5 1 -2 0.0838
-5 -1 2 0.0760
-2 -5 3 0.1350
4 3 0 0.1226
0 -6 2 0.1476
-2 6 -6 0.1767
0 6 2 0.1684

_exptl_crystal_size_max          0.438
_exptl_crystal_size_mid          0.343
_exptl_crystal_size_min          0.158
loop_
_exptl_oxdiff_crystal_face_indexfrac_h
_exptl_oxdiff_crystal_face_indexfrac_k
_exptl_oxdiff_crystal_face_indexfrac_l
_exptl_oxdiff_crystal_face_x
_exptl_oxdiff_crystal_face_y
_exptl_oxdiff_crystal_face_z
-5.0360 4.3390 2.0791 0.5931 -0.4524 -0.6660
-5.4263 1.0536 3.7588 0.9135 -0.3219 -0.2489
5.4614 -0.7692 0.2357 -0.9363 0.0229 0.3505
-5.1158 -0.8240 1.4931 0.9953 -0.0249 -0.0931
4.9598 -0.0460 3.6494 -0.8951 -0.2669 0.3572
-4.6774 -1.3257 -2.4067 0.9484 0.2823 -0.1444
-3.9042 -1.2569 -6.3688 0.7975 0.5499 -0.2482
2.2865 4.7270 2.4029 -0.7690 -0.5286 -0.3596
2.0017 -6.6561 1.5304 0.1382 0.3852 0.9124
0.2291 -0.0536 12.9170 -0.0216 -0.8946 0.4463
0.0999 -0.7597 -12.7544 0.0230 0.9431 -0.3317
-2.5445 6.4179 1.9359 -0.0171 -0.6065 -0.7949
-2.9438 0.0080 11.6070 0.5499 -0.7975 0.2482
5.5225 -2.7481 -1.3910 -0.8005 0.2839 0.5278
5.3623 -0.7705 -4.1270 -0.9236 0.3265 0.2010
-5.4953 1.4766 3.2244 0.8935 -0.3162 -0.3187
5.0836 0.9179 -1.5986 -0.9967 0.0253 0.0772
-4.9890 -1.1743 1.8697 0.9991 -0.0253 -0.0342
-1.8548 -5.3960 2.6863 0.7470 0.2235 0.6261
3.7567 3.3720 0.2024 -0.9375 -0.2791 -0.2079
0.0783 -6.4240 2.2098 0.4718 0.3271 0.8188
-2.4476 5.9063 -6.1426 -0.0063 -0.0070 -1.0000
-0.0069 6.1946 2.0445 -0.4622 -0.6058 -0.6475

_exptl_transmission_factor_max   ?
_exptl_transmission_factor_min   ?
_diffrn_reflns_av_R_equivalents  0.0548
_diffrn_reflns_av_unetI/netI     0.0399
_diffrn_reflns_Laue_measured_fraction_full 1.000
_diffrn_reflns_Laue_measured_fraction_max 0.994
_diffrn_reflns_limit_h_max       10
_diffrn_reflns_limit_h_min       -10
_diffrn_reflns_limit_k_max       12
_diffrn_reflns_limit_k_min       -12
_diffrn_reflns_limit_l_max       25
_diffrn_reflns_limit_l_min       -24
_diffrn_reflns_number            27902
_diffrn_reflns_point_group_measured_fraction_full 1.000
_diffrn_reflns_point_group_measured_fraction_max 0.994
_diffrn_reflns_theta_full        67.684
_diffrn_reflns_theta_max         76.352
_diffrn_reflns_theta_min         2.210
_diffrn_detector                 'CCD plate'
_diffrn_detector_area_resol_mean 5.2529
_diffrn_detector_type            AtlasS2
_diffrn_measured_fraction_theta_full 1.000
_diffrn_measured_fraction_theta_max 0.994
_diffrn_measurement_details      
;
List of Runs (angles in degrees, time in seconds):

  # Type    Start    End  Width  tₑₓₚ   ω     θ     κ     φ   Frames
#--------------------------------------------------------------------------
  1  ω    -65.00  33.00   1.00    4.00    --  -40.97  38.00-180.00   98
  2  ω   -113.00 -13.00   1.00    4.00    --  -40.97 -57.00-120.00  100
  3  ω   -115.00 -16.00   1.00    4.00    --  -40.97 -38.00   0.00   99
  4  ω    -87.00  -6.00   1.00    4.00    --  -40.97 125.00 -60.00   81
  5  ω      6.00  32.00   1.00    4.00    --   40.97  85.00 134.59   26
  6  ω      6.00  82.00   1.00    4.00    --   40.97 -99.00-150.00   76
  7  ω     36.00 109.00   1.00   16.00    --  112.00-111.00 120.00   73
  8  ω     36.00 109.00   1.00   16.00    --  112.00-111.00 -60.00   73
  9  ω     83.00 178.00   1.00   16.00    --  112.00  61.00  60.00   95
 10  ω     36.00 109.00   1.00   16.00    --  112.00-111.00-180.00   73
 11  ω     30.00 106.00   1.00   16.00    --  112.00 -95.00  30.00   76
 12  ω     36.00 109.00   1.00   16.00    --  112.00-111.00 150.00   73
 13  ω     39.00 138.00   1.00   16.00    --  112.00 -45.00 -90.00   99
 14  ω     86.00 178.00   1.00   16.00    --  112.00  45.00-120.00   92
 15  ω     83.00 178.00   1.00   16.00    --  112.00  61.00  90.00   95
 16  ω     36.00 109.00   1.00   16.00    --  112.00-111.00 -90.00   73
 17  ω    104.00 178.00   1.00   16.00    --  112.00 111.00-180.00   74
 18  ω    104.00 178.00   1.00   16.00    --  112.00 111.00 -30.00   74
 19  ω     86.00 178.00   1.00   16.00    --  112.00  45.00 120.00   92
 20  ω    104.00 178.00   1.00   16.00    --  112.00 111.00  90.00   74
 21  ω    103.00 178.00   1.00   16.00    --  112.00  77.00 -30.00   75
 22  ω     36.00 109.00   1.00   16.00    --  112.00-111.00 -30.00   73
 23  ω     84.00 178.00   1.00   16.00    --  112.00  30.00 -60.00   94
 24  ω     40.00 141.00   1.00   16.00    --  112.00 -61.00  90.00  101
 25  ω     83.00 178.00   1.00   16.00    --  112.00  61.00 120.00   95
 26  ω     83.00 178.00   1.00   16.00    --  112.00  61.00 150.00   95
 27  ω     36.00 109.00   1.00   16.00    --  112.00-111.00  30.00   73
 28  ω     40.00 141.00   1.00   16.00    --  112.00 -61.00 -30.00  101
 29  ω     46.00  73.00   1.00   16.00    --  112.00 -77.00 -90.00   27
 30  ω     94.00 126.00   1.00   16.00    --  112.00 -77.00 -90.00   32
 31  ω     79.00 104.00   1.00   16.00    --  112.00-111.00-150.00   25
 32  ω     72.00 109.00   1.00   16.00    --  112.00-111.00-120.00   37
 33  ω    105.00 161.00   1.00   16.00    --  112.00 111.00 -60.00   56
 34  ω    107.00 140.00   1.00   16.00    --  112.00 111.00 150.00   33
 35  ω     65.00 131.00   1.00   16.00    --  112.00 178.00 -30.00   66
 36  ω     33.00  65.00   1.00   16.00    --  112.00 -95.00   0.00   32
 37  ω     69.00  97.00   1.00   16.00    --  112.00 178.00 120.00   28
 38  ω     96.00 123.00   1.00   16.00    --  112.00 -87.00 -67.78   27
 39  ω     75.00 102.00   1.00   16.00    --  112.00 -77.00 150.00   27
 40  ω     68.00 101.00   1.00   16.00    --  112.00  17.00 -74.92   33
 41  ω    128.00 155.00   1.00   16.00    --  112.00  17.00 -74.92   27
 42  ω     41.00  70.00   1.00   16.00    --  112.00 -87.00 -67.78   29
;
_diffrn_measurement_device       'four-circle diffractometer'
_diffrn_measurement_device_type  'SuperNova, Dual, Cu at home/near, AtlasS2'
_diffrn_measurement_method       'ω scans'
_diffrn_orient_matrix_type       
'CrysAlisPro convention (1999,Acta A55,543-557)'
_diffrn_orient_matrix_UB_11      -0.1820835000
_diffrn_orient_matrix_UB_12      -0.0752333000
_diffrn_orient_matrix_UB_13      0.0012486000
_diffrn_orient_matrix_UB_21      -0.0033603000
_diffrn_orient_matrix_UB_22      -0.0748642000
_diffrn_orient_matrix_UB_23      -0.0695095000
_diffrn_orient_matrix_UB_31      0.0464896000
_diffrn_orient_matrix_UB_32      -0.1154562000
_diffrn_orient_matrix_UB_33      0.0332504000
_diffrn_radiation_monochromator  mirror
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           'Cu K\a'
_diffrn_radiation_wavelength     1.54184
_diffrn_source                   'micro-focus sealed X-ray tube'
_diffrn_source_type              'SuperNova (Cu) X-ray Source'
_reflns_Friedel_coverage         0.000
_reflns_Friedel_fraction_full    .
_reflns_Friedel_fraction_max     .
_reflns_number_gt                5109
_reflns_number_total             7070
_reflns_odcompleteness_completeness 98.37
_reflns_odcompleteness_iscentric 1
_reflns_odcompleteness_theta     77.17
_reflns_special_details          
;
 Reflections were merged by SHELXL according to the crystal
 class for the calculation of statistics and refinement.
 
 _reflns_Friedel_fraction is defined as the number of unique
 Friedel pairs measured divided by the number that would be
 possible theoretically, ignoring centric projections and
 systematic absences.
;
_reflns_threshold_expression     'I > 2σ(I)'
_computing_cell_refinement       'CrysAlisPro 1.171.40.67a (Rigaku OD, 2019)'
_computing_data_collection       'CrysAlisPro 1.171.40.67a (Rigaku OD, 2019)'
_computing_data_reduction        'CrysAlisPro 1.171.40.67a (Rigaku OD, 2019)'
_computing_molecular_graphics    'Olex2 1.3 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 1.3 (Dolomanov et al., 2009)'
_computing_structure_refinement  'SHELXL 2014/7 (Sheldrick, 2015)'
_computing_structure_solution    'SHELXT 2014/5 (Sheldrick, 2014)'
_refine_diff_density_max         0.318
_refine_diff_density_min         -0.420
_refine_diff_density_rms         0.045
_refine_ls_extinction_coef       .
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.019
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     483
_refine_ls_number_reflns         7070
_refine_ls_number_restraints     40
_refine_ls_R_factor_all          0.0799
_refine_ls_R_factor_gt           0.0589
_refine_ls_restrained_S_all      1.037
_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)+(0.1061P)²+0.0488P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1612
_refine_ls_wR_factor_ref         0.1818
_refine_special_details          ?
_olex2_refinement_description    
;
1. 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, All O(H,H) groups
2. Restrained distances
 F1''-F1 \\sim F1''-F3 \\sim F1''-F2 \\sim F1-F2 \\sim F3-F2
 with sigma of 0.04
 B1-F1'' \\sim B1-F1 \\sim B1-F3 \\sim B1-F2
 with sigma of 0.02
 F3'-F2' \\sim F3'-F1' \\sim F2'-F1'
 with sigma of 0.04
 B1-F1'' \\sim B1-F3' \\sim B1-F2' \\sim B1-F1'
 with sigma of 0.02
3. Uiso/Uaniso restraints and constraints
Uanis(O1S) \\sim Ueq: with sigma of 0.01 and sigma for terminal atoms of 0.02
Uanis(C28) = Uanis(C28')
Uanis(C32') = Uanis(C32)
Uanis(N4) = Uanis(N4')
Uanis(C29') = Uanis(C29)
Uanis(C32) = Uanis(C32')
4. Others
 Sof(C32)=Sof(H32C)=Sof(H32D)=Sof(C31')=Sof(N4')=Sof(C27')=Sof(H27')=Sof(C28')=
 Sof(H28')=Sof(C29')=Sof(H29')=Sof(C30')=Sof(H30')=1-FVAR(1)
 Sof(N4)=Sof(C31)=Sof(C32')=Sof(H32A)=Sof(H32B)=Sof(C27)=Sof(H27)=Sof(C29)=
 Sof(H29)=Sof(C30)=Sof(H30)=Sof(C28)=Sof(H28)=FVAR(1)
 Sof(O1S)=Sof(H1SA)=Sof(H1SB)=FVAR(2)
 Fixed Sof: F1(0.55) F3'(0.45) F3(0.55) F2(0.55) F2'(0.45) F1'(0.45)
5.a Free rotating group:
 O1S(H1SA,H1SB)
5.b Secondary CH2 refined with riding coordinates:
 C26(H26A,H26B), C20(H20A,H20B), C32'(H32A,H32B), C32(H32C,H32D)
5.c Aromatic/amide H refined with riding coordinates:
 C21(H21), C5(H5), C15(H15), C4(H4), C24(H24), C22(H22), C27(H27), C29(H29),
 C23(H23), C30(H30), C16(H16), C18(H18), C28(H28), C17(H17), C27'(H27'),
 C28'(H28'), C29'(H29'), C30'(H30')
5.d Idealised Me refined as rotating group:
 C12(H12A,H12B,H12C), C9(H9A,H9B,H9C), C8(H8A,H8B,H8C), C13(H13A,H13B,H13C),
 C10(H10A,H10B,H10C), C14(H14A,H14B,H14C)
;
_atom_sites_solution_hydrogens   mixed
_atom_sites_solution_primary     dual
_atom_sites_solution_secondary   ?
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
Fe Fe 0.44589(6) 0.66685(5) 0.25843(2) 0.06926(17) Uani 1 1 d . . . . .
O2 O 0.4024(3) 0.7072(2) 0.17071(11) 0.0758(5) Uani 1 1 d . . . . .
O1 O 0.3099(3) 0.4872(2) 0.22673(10) 0.0715(5) Uani 1 1 d . . . . .
N3 N 0.2761(3) 0.7377(3) 0.31419(14) 0.0736(6) Uani 1 1 d . . . . .
N1 N 0.5980(3) 0.8702(3) 0.29115(14) 0.0750(6) Uani 1 1 d . . . . .
N2 N 0.5209(4) 0.6419(3) 0.36107(16) 0.0840(8) Uani 1 1 d . . . . .
C2 C 0.3260(4) 0.5941(3) 0.12836(15) 0.0674(7) Uani 1 1 d . . . . .
N4 N 0.667(3) 0.596(3) 0.2661(8) 0.0765(18) Uani 0.364(12) 1 d . . P A 1
C1 C 0.2780(4) 0.4724(3) 0.16008(15) 0.0662(6) Uani 1 1 d . . . . .
F1'' F 0.0994(5) 0.1562(3) 0.46597(18) 0.1574(14) Uani 1 1 d D . . . .
C6 C 0.2022(4) 0.3460(3) 0.12193(16) 0.0727(7) Uani 1 1 d . . . . .
C3 C 0.2989(5) 0.5961(3) 0.05937(16) 0.0804(9) Uani 1 1 d . . . . .
C7 C 0.1611(5) 0.2118(3) 0.15397(19) 0.0832(9) Uani 1 1 d . . . . .
C25 C 0.2755(5) 0.7097(4) 0.37727(18) 0.0822(8) Uani 1 1 d . . . . .
C19 C 0.6539(4) 0.8896(3) 0.3550(2) 0.0833(9) Uani 1 1 d . . . . .
C11 C 0.3549(6) 0.7284(4) 0.02640(19) 0.0953(12) Uani 1 1 d . . . . .
C21 C 0.1965(5) 0.8241(4) 0.2935(2) 0.0870(9) Uani 1 1 d . . . . .
H21 H 0.1959 0.8425 0.2491 0.104 Uiso 1 1 calc R U . . .
C5 C 0.1749(6) 0.3512(4) 0.05382(19) 0.0924(10) Uani 1 1 d . . . . .
H5 H 0.1237 0.2704 0.0269 0.111 Uiso 1 1 calc R U . . .
C31 C 0.693(3) 0.536(3) 0.3209(12) 0.080(5) Uani 0.364(12) 1 d . . P A 1
C15 C 0.6082(5) 0.9780(4) 0.2565(2) 0.0911(10) Uani 1 1 d . . . . .
H15 H 0.5685 0.9635 0.2114 0.109 Uiso 1 1 calc R U . . .
C26 C 0.3702(6) 0.6123(4) 0.3949(2) 0.0988(11) Uani 1 1 d . . . . .
H26A H 0.3979 0.6215 0.4430 0.119 Uiso 1 1 calc R U . . .
H26B H 0.3039 0.5195 0.3810 0.119 Uiso 1 1 calc R U . . .
C4 C 0.2199(6) 0.4708(4) 0.02342(19) 0.0983(12) Uani 1 1 d . . . . .
H4 H 0.1962 0.4669 -0.0226 0.118 Uiso 1 1 calc R U . . .
C20 C 0.6455(5) 0.7678(4) 0.3919(2) 0.0954(11) Uani 1 1 d . . . . .
H20A H 0.7515 0.7516 0.3945 0.115 Uiso 1 1 calc R U . . .
H20B H 0.6223 0.7877 0.4372 0.115 Uiso 1 1 calc R U . . .
C12 C 0.2678(7) 0.8290(4) 0.0536(2) 0.1071(14) Uani 1 1 d . . . . .
H12A H 0.2971 0.8499 0.1010 0.161 Uiso 1 1 calc R U . . .
H12B H 0.1519 0.7890 0.0448 0.161 Uiso 1 1 calc R U . . .
H12C H 0.2998 0.9111 0.0322 0.161 Uiso 1 1 calc R U . . .
C32' C 0.570(8) 0.527(8) 0.365(4) 0.096(6) Uani 0.364(12) 1 d . . P A 2
H32A H 0.4782 0.4450 0.3560 0.115 Uiso 0.364(12) 1 calc R U P A 2
H32B H 0.6296 0.5273 0.4074 0.115 Uiso 0.364(12) 1 calc R U P A 2
C24 C 0.1900(6) 0.7672(5) 0.4215(2) 0.1094(14) Uani 1 1 d . . . . .
H24 H 0.1866 0.7445 0.4652 0.131 Uiso 1 1 calc R U . . .
C9 C 0.0453(6) 0.2123(4) 0.2074(2) 0.0990(12) Uani 1 1 d . . . . .
H9A H 0.0985 0.2812 0.2434 0.149 Uiso 1 1 calc R U . . .
H9B H 0.0153 0.1249 0.2242 0.149 Uiso 1 1 calc R U . . .
H9C H -0.0508 0.2312 0.1882 0.149 Uiso 1 1 calc R U . . .
C22 C 0.1154(6) 0.8866(4) 0.3359(3) 0.1082(14) Uani 1 1 d . . . . .
H22 H 0.0639 0.9485 0.3207 0.130 Uiso 1 1 calc R U . . .
C27 C 0.754(3) 0.593(2) 0.2166(11) 0.097(5) Uani 0.364(12) 1 d . . P A 1
H27 H 0.7214 0.6214 0.1764 0.117 Uiso 0.364(12) 1 calc R U P A 1
C8 C 0.3183(6) 0.1901(4) 0.1855(3) 0.1096(14) Uani 1 1 d . . . . .
H8A H 0.3877 0.1826 0.1513 0.164 Uiso 1 1 calc R U . . .
H8B H 0.2924 0.1080 0.2071 0.164 Uiso 1 1 calc R U . . .
H8C H 0.3735 0.2660 0.2178 0.164 Uiso 1 1 calc R U . . .
C13 C 0.5389(7) 0.7897(5) 0.0416(3) 0.1245(18) Uani 1 1 d . . . . .
H13A H 0.5734 0.8716 0.0201 0.187 Uiso 1 1 calc R U . . .
H13B H 0.5926 0.7256 0.0252 0.187 Uiso 1 1 calc R U . . .
H13C H 0.5667 0.8106 0.0891 0.187 Uiso 1 1 calc R U . . .
C29 C 0.921(3) 0.496(2) 0.2782(12) 0.105(4) Uani 0.364(12) 1 d . . P A 1
H29 H 1.0081 0.4599 0.2832 0.126 Uiso 0.364(12) 1 calc R U P A 1
C23 C 0.1117(7) 0.8567(5) 0.4000(3) 0.1172(16) Uani 1 1 d . . . . .
H23 H 0.0562 0.8970 0.4292 0.141 Uiso 1 1 calc R U . . .
C10 C 0.0776(7) 0.0898(4) 0.1017(3) 0.1180(16) Uani 1 1 d . . . . .
H10A H -0.0270 0.0966 0.0846 0.177 Uiso 1 1 calc R U . . .
H10B H 0.0634 0.0068 0.1222 0.177 Uiso 1 1 calc R U . . .
H10C H 0.1441 0.0900 0.0657 0.177 Uiso 1 1 calc R U . . .
F1 F 0.1221(17) 0.3003(14) 0.3828(5) 0.211(7) Uani 0.55 1 d D . P B 1
C30 C 0.824(3) 0.4920(19) 0.3299(11) 0.099(5) Uani 0.364(12) 1 d . . P A 1
H30 H 0.8503 0.4595 0.3699 0.119 Uiso 0.364(12) 1 calc R U P A 1
C16 C 0.6754(7) 1.1083(4) 0.2856(3) 0.1209(17) Uani 1 1 d . . . . .
H16 H 0.6788 1.1820 0.2613 0.145 Uiso 1 1 calc R U . . .
C18 C 0.7258(8) 1.0185(5) 0.3869(3) 0.1281(19) Uani 1 1 d . . . . .
H18 H 0.7657 1.0313 0.4319 0.154 Uiso 1 1 calc R U . . .
C14 C 0.3108(10) 0.7037(6) -0.0498(2) 0.141(2) Uani 1 1 d . . . . .
H14A H 0.1980 0.6524 -0.0598 0.212 Uiso 1 1 calc R U . . .
H14B H 0.3777 0.6536 -0.0693 0.212 Uiso 1 1 calc R U . . .
H14C H 0.3293 0.7895 -0.0680 0.212 Uiso 1 1 calc R U . . .
F3' F 0.3060(15) 0.3533(10) 0.4751(6) 0.156(5) Uani 0.45 1 d D . P B 2
C28 C 0.897(2) 0.550(2) 0.2213(12) 0.103(3) Uani 0.364(12) 1 d . . P A 1
H28 H 0.9665 0.5581 0.1879 0.124 Uiso 0.364(12) 1 calc R U P A 1
B1 B 0.1680(9) 0.2745(6) 0.4422(3) 0.125(2) Uani 1 1 d D . . . .
C17 C 0.7371(9) 1.1275(5) 0.3507(4) 0.154(3) Uani 1 1 d . . . . .
H17 H 0.7874 1.2153 0.3711 0.184 Uiso 1 1 calc R U . . .
F3 F 0.1815(18) 0.3720(9) 0.4907(4) 0.183(4) Uani 0.55 1 d D . P B 1
F2 F 0.3318(14) 0.2774(15) 0.4408(7) 0.226(6) Uani 0.55 1 d D . P B 1
F2' F 0.0529(15) 0.3493(11) 0.4381(10) 0.206(5) Uani 0.45 1 d D . P B 2
F1' F 0.192(2) 0.2431(16) 0.3789(5) 0.200(7) Uani 0.45 1 d D . P B 2
C32 C 0.602(4) 0.524(4) 0.352(2) 0.096(6) Uani 0.636(12) 1 d . . P A 1
H32C H 0.6458 0.5106 0.3956 0.115 Uiso 0.636(12) 1 calc R U P A 1
H32D H 0.5163 0.4415 0.3350 0.115 Uiso 0.636(12) 1 calc R U P A 1
C31' C 0.706(2) 0.5449(15) 0.2946(7) 0.080(3) Uani 0.636(12) 1 d . . P A 2
N4' N 0.6557(14) 0.6025(12) 0.2430(5) 0.0765(18) Uani 0.636(12) 1 d . . P A 2
C27' C 0.7430(15) 0.6192(13) 0.1908(5) 0.090(2) Uani 0.636(12) 1 d . . P A 2
H27' H 0.7102 0.6617 0.1555 0.108 Uiso 0.636(12) 1 calc R U P A 2
C28' C 0.8824(11) 0.5750(11) 0.1873(5) 0.103(3) Uani 0.636(12) 1 d . . P A 2
H28' H 0.9385 0.5843 0.1496 0.124 Uiso 0.636(12) 1 calc R U P A 2
C29' C 0.9347(14) 0.5170(10) 0.2415(7) 0.105(4) Uani 0.636(12) 1 d . . P A 2
H29' H 1.0290 0.4897 0.2411 0.126 Uiso 0.636(12) 1 calc R U P A 2
C30' C 0.8467(13) 0.5003(10) 0.2953(6) 0.095(3) Uani 0.636(12) 1 d . . P A 2
H30' H 0.8790 0.4602 0.3316 0.114 Uiso 0.636(12) 1 calc R U P A 2
O1S O 0.902(2) 0.4405(17) 0.4524(9) 0.171(8) Uani 0.333(12) 1 d G U P C -1
H1SA H 0.9843 0.4385 0.4782 0.256 Uiso 0.333(12) 1 d G U P C -1
H1SB H 0.9420 0.4890 0.4223 0.256 Uiso 0.333(12) 1 d G U P C -1


_geom_special_details            
;
 All esds (except the esd in the dihedral angle between two l.s. planes)
 are estimated using the full covariance matrix.  The cell esds are taken
 into account individually in the estimation of esds in distances, angles
 and torsion angles; correlations between esds in cell parameters are only
 used when they are defined by crystal symmetry.  An approximate (isotropic)
 treatment of cell esds is used for estimating esds involving l.s. planes.
;
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
Fe O2 1.881(2) . ?
Fe O1 1.916(2) . ?
Fe N3 2.160(3) . ?
Fe N1 2.151(3) . ?
Fe N2 2.175(3) . ?
Fe N4 2.22(2) . ?
Fe N4' 2.127(12) . ?
O2 C2 1.356(4) . ?
O1 C1 1.338(4) . ?
N3 C25 1.326(4) . ?
N3 C21 1.339(4) . ?
N1 C19 1.317(5) . ?
N1 C15 1.344(4) . ?
N2 C26 1.479(6) . ?
N2 C20 1.482(5) . ?
N2 C32' 1.37(7) . ?
N2 C32 1.56(3) . ?
C2 C1 1.423(4) . ?
C2 C3 1.395(4) . ?
N4 C31 1.34(2) . ?
N4 C27 1.29(3) . ?
C1 C6 1.412(4) . ?
F1'' B1 1.339(6) . ?
C6 C7 1.534(4) . ?
C6 C5 1.383(5) . ?
C3 C11 1.534(5) . ?
C3 C4 1.390(6) . ?
C7 C9 1.525(5) . ?
C7 C8 1.528(6) . ?
C7 C10 1.538(6) . ?
C25 C26 1.506(6) . ?
C25 C24 1.399(6) . ?
C19 C20 1.496(5) . ?
C19 C18 1.377(6) . ?
C11 C12 1.534(5) . ?
C11 C13 1.523(8) . ?
C11 C14 1.537(6) . ?
C21 H21 0.9300 . ?
C21 C22 1.377(6) . ?
C5 H5 0.9300 . ?
C5 C4 1.388(6) . ?
C31 C30 1.34(4) . ?
C31 C32 1.02(4) . ?
C15 H15 0.9300 . ?
C15 C16 1.365(6) . ?
C26 H26A 0.9700 . ?
C26 H26B 0.9700 . ?
C4 H4 0.9300 . ?
C20 H20A 0.9700 . ?
C20 H20B 0.9700 . ?
C12 H12A 0.9600 . ?
C12 H12B 0.9600 . ?
C12 H12C 0.9600 . ?
C32' H32A 0.9700 . ?
C32' H32B 0.9700 . ?
C32' C31' 1.89(6) . ?
C24 H24 0.9300 . ?
C24 C23 1.363(7) . ?
C9 H9A 0.9600 . ?
C9 H9B 0.9600 . ?
C9 H9C 0.9600 . ?
C22 H22 0.9300 . ?
C22 C23 1.353(7) . ?
C27 H27 0.9300 . ?
C27 C28 1.42(3) . ?
C8 H8A 0.9600 . ?
C8 H8B 0.9600 . ?
C8 H8C 0.9600 . ?
C13 H13A 0.9600 . ?
C13 H13B 0.9600 . ?
C13 H13C 0.9600 . ?
C29 H29 0.9300 . ?
C29 C30 1.38(2) . ?
C29 C28 1.34(3) . ?
C23 H23 0.9300 . ?
C10 H10A 0.9600 . ?
C10 H10B 0.9600 . ?
C10 H10C 0.9600 . ?
F1 B1 1.301(9) . ?
C30 H30 0.9300 . ?
C16 H16 0.9300 . ?
C16 C17 1.354(8) . ?
C18 H18 0.9300 . ?
C18 C17 1.371(7) . ?
C14 H14A 0.9600 . ?
C14 H14B 0.9600 . ?
C14 H14C 0.9600 . ?
F3' B1 1.324(9) . ?
C28 H28 0.9300 . ?
B1 F3 1.320(9) . ?
B1 F2 1.403(11) . ?
B1 F2' 1.416(10) . ?
B1 F1' 1.339(11) . ?
C17 H17 0.9300 . ?
C32 H32C 0.9700 . ?
C32 H32D 0.9700 . ?
C31' N4' 1.340(14) . ?
C31' C30' 1.41(2) . ?
N4' C27' 1.334(14) . ?
C27' H27' 0.9300 . ?
C27' C28' 1.402(14) . ?
C28' H28' 0.9300 . ?
C28' C29' 1.388(14) . ?
C29' H29' 0.9300 . ?
C29' C30' 1.366(15) . ?
C30' H30' 0.9300 . ?
O1S H1SA 0.8502 . ?
O1S H1SB 0.8493 . ?

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 Fe O1 84.88(9) . . ?
O2 Fe N3 104.28(10) . . ?
O2 Fe N1 93.48(10) . . ?
O2 Fe N2 173.18(11) . . ?
O2 Fe N4 109.9(5) . . ?
O2 Fe N4' 97.4(3) . . ?
O1 Fe N3 99.14(10) . . ?
O1 Fe N1 178.36(10) . . ?
O1 Fe N2 101.56(10) . . ?
O1 Fe N4 91.5(6) . . ?
O1 Fe N4' 89.6(3) . . ?
N3 Fe N2 77.09(12) . . ?
N3 Fe N4 145.0(4) . . ?
N1 Fe N3 81.39(10) . . ?
N1 Fe N2 80.07(11) . . ?
N1 Fe N4 88.9(6) . . ?
N2 Fe N4 68.1(4) . . ?
N4' Fe N3 157.2(3) . . ?
N4' Fe N1 90.5(3) . . ?
N4' Fe N2 80.6(3) . . ?
C2 O2 Fe 112.47(17) . . ?
C1 O1 Fe 111.19(18) . . ?
C25 N3 Fe 115.1(2) . . ?
C25 N3 C21 119.2(3) . . ?
C21 N3 Fe 124.7(2) . . ?
C19 N1 Fe 114.1(2) . . ?
C19 N1 C15 119.6(3) . . ?
C15 N1 Fe 124.6(3) . . ?
C26 N2 Fe 105.5(2) . . ?
C26 N2 C20 112.5(3) . . ?
C26 N2 C32 116.8(12) . . ?
C20 N2 Fe 109.5(2) . . ?
C20 N2 C32 109.4(15) . . ?
C32' N2 Fe 111(3) . . ?
C32' N2 C26 104(3) . . ?
C32' N2 C20 114(3) . . ?
C32 N2 Fe 102.4(15) . . ?
O2 C2 C1 114.3(3) . . ?
O2 C2 C3 123.0(3) . . ?
C3 C2 C1 122.6(3) . . ?
C31 N4 Fe 116.2(17) . . ?
C27 N4 Fe 122.2(13) . . ?
C27 N4 C31 121(2) . . ?
O1 C1 C2 115.7(3) . . ?
O1 C1 C6 123.7(3) . . ?
C6 C1 C2 120.6(3) . . ?
C1 C6 C7 121.8(3) . . ?
C5 C6 C1 115.5(3) . . ?
C5 C6 C7 122.6(3) . . ?
C2 C3 C11 121.5(3) . . ?
C4 C3 C2 115.4(3) . . ?
C4 C3 C11 123.1(3) . . ?
C6 C7 C10 111.4(3) . . ?
C9 C7 C6 111.3(2) . . ?
C9 C7 C8 109.4(4) . . ?
C9 C7 C10 107.3(4) . . ?
C8 C7 C6 109.3(3) . . ?
C8 C7 C10 108.1(3) . . ?
N3 C25 C26 114.4(3) . . ?
N3 C25 C24 120.7(4) . . ?
C24 C25 C26 124.9(4) . . ?
N1 C19 C20 118.5(3) . . ?
N1 C19 C18 121.4(4) . . ?
C18 C19 C20 120.1(4) . . ?
C3 C11 C12 109.0(3) . . ?
C3 C11 C14 111.5(4) . . ?
C12 C11 C14 107.5(4) . . ?
C13 C11 C3 109.9(3) . . ?
C13 C11 C12 109.9(4) . . ?
C13 C11 C14 109.0(4) . . ?
N3 C21 H21 119.0 . . ?
N3 C21 C22 122.1(4) . . ?
C22 C21 H21 119.0 . . ?
C6 C5 H5 118.3 . . ?
C6 C5 C4 123.5(4) . . ?
C4 C5 H5 118.3 . . ?
C30 C31 N4 120(2) . . ?
C32 C31 N4 114(3) . . ?
C32 C31 C30 126(3) . . ?
N1 C15 H15 119.1 . . ?
N1 C15 C16 121.8(4) . . ?
C16 C15 H15 119.1 . . ?
N2 C26 C25 109.7(3) . . ?
N2 C26 H26A 109.7 . . ?
N2 C26 H26B 109.7 . . ?
C25 C26 H26A 109.7 . . ?
C25 C26 H26B 109.7 . . ?
H26A C26 H26B 108.2 . . ?
C3 C4 H4 118.8 . . ?
C5 C4 C3 122.3(4) . . ?
C5 C4 H4 118.8 . . ?
N2 C20 C19 114.2(3) . . ?
N2 C20 H20A 108.7 . . ?
N2 C20 H20B 108.7 . . ?
C19 C20 H20A 108.7 . . ?
C19 C20 H20B 108.7 . . ?
H20A C20 H20B 107.6 . . ?
C11 C12 H12A 109.5 . . ?
C11 C12 H12B 109.5 . . ?
C11 C12 H12C 109.5 . . ?
H12A C12 H12B 109.5 . . ?
H12A C12 H12C 109.5 . . ?
H12B C12 H12C 109.5 . . ?
N2 C32' H32A 111.7 . . ?
N2 C32' H32B 111.7 . . ?
N2 C32' C31' 100(4) . . ?
H32A C32' H32B 109.5 . . ?
C31' C32' H32A 111.7 . . ?
C31' C32' H32B 111.7 . . ?
C25 C24 H24 120.3 . . ?
C23 C24 C25 119.5(4) . . ?
C23 C24 H24 120.3 . . ?
C7 C9 H9A 109.5 . . ?
C7 C9 H9B 109.5 . . ?
C7 C9 H9C 109.5 . . ?
H9A C9 H9B 109.5 . . ?
H9A C9 H9C 109.5 . . ?
H9B C9 H9C 109.5 . . ?
C21 C22 H22 120.4 . . ?
C23 C22 C21 119.1(4) . . ?
C23 C22 H22 120.4 . . ?
N4 C27 H27 118.6 . . ?
N4 C27 C28 122.7(17) . . ?
C28 C27 H27 118.6 . . ?
C7 C8 H8A 109.5 . . ?
C7 C8 H8B 109.5 . . ?
C7 C8 H8C 109.5 . . ?
H8A C8 H8B 109.5 . . ?
H8A C8 H8C 109.5 . . ?
H8B C8 H8C 109.5 . . ?
C11 C13 H13A 109.5 . . ?
C11 C13 H13B 109.5 . . ?
C11 C13 H13C 109.5 . . ?
H13A C13 H13B 109.5 . . ?
H13A C13 H13C 109.5 . . ?
H13B C13 H13C 109.5 . . ?
C30 C29 H29 118.1 . . ?
C28 C29 H29 118.1 . . ?
C28 C29 C30 124(2) . . ?
C24 C23 H23 120.3 . . ?
C22 C23 C24 119.4(4) . . ?
C22 C23 H23 120.3 . . ?
C7 C10 H10A 109.5 . . ?
C7 C10 H10B 109.5 . . ?
C7 C10 H10C 109.5 . . ?
H10A C10 H10B 109.5 . . ?
H10A C10 H10C 109.5 . . ?
H10B C10 H10C 109.5 . . ?
C31 C30 C29 118(2) . . ?
C31 C30 H30 121.0 . . ?
C29 C30 H30 121.0 . . ?
C15 C16 H16 120.8 . . ?
C17 C16 C15 118.4(4) . . ?
C17 C16 H16 120.8 . . ?
C19 C18 H18 120.8 . . ?
C17 C18 C19 118.5(5) . . ?
C17 C18 H18 120.8 . . ?
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 . . ?
C27 C28 H28 123.2 . . ?
C29 C28 C27 113.5(18) . . ?
C29 C28 H28 123.2 . . ?
F1'' B1 F2 103.8(7) . . ?
F1'' B1 F2' 108.8(8) . . ?
F1'' B1 F1' 106.2(8) . . ?
F1 B1 F1'' 122.0(6) . . ?
F1 B1 F3 115.3(10) . . ?
F1 B1 F2 105.2(9) . . ?
F3' B1 F1'' 117.1(5) . . ?
F3' B1 F2' 109.0(9) . . ?
F3' B1 F1' 109.6(11) . . ?
F3 B1 F1'' 107.0(6) . . ?
F3 B1 F2 100.8(8) . . ?
F1' B1 F2' 105.6(9) . . ?
C16 C17 C18 120.4(5) . . ?
C16 C17 H17 119.8 . . ?
C18 C17 H17 119.8 . . ?
N2 C32 H32C 107.8 . . ?
N2 C32 H32D 107.8 . . ?
C31 C32 N2 118(3) . . ?
C31 C32 H32C 107.8 . . ?
C31 C32 H32D 107.8 . . ?
H32C C32 H32D 107.2 . . ?
N4' C31' C32' 114(3) . . ?
N4' C31' C30' 122.3(11) . . ?
C30' C31' C32' 124(3) . . ?
C31' N4' Fe 113.5(9) . . ?
C27' N4' Fe 127.9(6) . . ?
C27' N4' C31' 118.5(11) . . ?
N4' C27' H27' 118.8 . . ?
N4' C27' C28' 122.4(9) . . ?
C28' C27' H27' 118.8 . . ?
C27' C28' H28' 120.8 . . ?
C29' C28' C27' 118.4(9) . . ?
C29' C28' H28' 120.8 . . ?
C28' C29' H29' 120.3 . . ?
C30' C29' C28' 119.5(11) . . ?
C30' C29' H29' 120.3 . . ?
C31' C30' H30' 120.6 . . ?
C29' C30' C31' 118.8(10) . . ?
C29' C30' H30' 120.6 . . ?
H1SA O1S H1SB 104.6 . . ?

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
Fe O2 C2 C1 7.0(3) . . . . ?
Fe O2 C2 C3 -172.0(2) . . . . ?
Fe O1 C1 C2 -9.9(3) . . . . ?
Fe O1 C1 C6 170.0(2) . . . . ?
Fe N3 C25 C26 -10.6(4) . . . . ?
Fe N3 C25 C24 170.3(3) . . . . ?
Fe N3 C21 C22 -166.9(3) . . . . ?
Fe N1 C19 C20 15.8(4) . . . . ?
Fe N1 C19 C18 -167.2(4) . . . . ?
Fe N1 C15 C16 164.4(4) . . . . ?
Fe N2 C26 C25 -45.8(4) . . . . ?
Fe N2 C20 C19 16.6(5) . . . . ?
Fe N2 C32' C31' 46(4) . . . . ?
Fe N2 C32 C31 54(4) . . . . ?
Fe N4 C31 C30 -178.9(17) . . . . ?
Fe N4 C31 C32 4(4) . . . . ?
Fe N4 C27 C28 179.1(17) . . . . ?
Fe N4' C27' C28' 178.2(9) . . . . ?
O2 C2 C1 O1 2.0(4) . . . . ?
O2 C2 C1 C6 -177.8(3) . . . . ?
O2 C2 C3 C11 0.1(5) . . . . ?
O2 C2 C3 C4 179.6(3) . . . . ?
O1 Fe O2 C2 -9.88(19) . . . . ?
O1 C1 C6 C7 -4.7(5) . . . . ?
O1 C1 C6 C5 178.2(3) . . . . ?
N3 Fe O2 C2 -108.0(2) . . . . ?
N3 C25 C26 N2 38.9(5) . . . . ?
N3 C25 C24 C23 -2.4(7) . . . . ?
N3 C21 C22 C23 -2.1(7) . . . . ?
N1 Fe O2 C2 170.0(2) . . . . ?
N1 C19 C20 N2 -22.5(6) . . . . ?
N1 C19 C18 C17 0.5(9) . . . . ?
N1 C15 C16 C17 1.9(8) . . . . ?
N2 C32' C31' N4' -34(5) . . . . ?
N2 C32' C31' C30' 147(3) . . . . ?
C2 C1 C6 C7 175.2(3) . . . . ?
C2 C1 C6 C5 -2.0(4) . . . . ?
C2 C3 C11 C12 -61.5(5) . . . . ?
C2 C3 C11 C13 59.0(4) . . . . ?
C2 C3 C11 C14 180.0(4) . . . . ?
C2 C3 C4 C5 -1.7(6) . . . . ?
N4 Fe O2 C2 79.9(7) . . . . ?
N4 C31 C30 C29 -7(4) . . . . ?
N4 C31 C32 N2 -38(5) . . . . ?
N4 C27 C28 C29 8(3) . . . . ?
C1 C2 C3 C11 -178.8(3) . . . . ?
C1 C2 C3 C4 0.6(5) . . . . ?
C1 C6 C7 C9 59.7(5) . . . . ?
C1 C6 C7 C8 -61.3(4) . . . . ?
C1 C6 C7 C10 179.3(3) . . . . ?
C1 C6 C5 C4 1.0(6) . . . . ?
C6 C5 C4 C3 0.9(7) . . . . ?
C3 C2 C1 O1 -178.9(3) . . . . ?
C3 C2 C1 C6 1.2(4) . . . . ?
C7 C6 C5 C4 -176.1(4) . . . . ?
C25 N3 C21 C22 0.9(6) . . . . ?
C25 C24 C23 C22 1.2(8) . . . . ?
C19 N1 C15 C16 0.0(6) . . . . ?
C19 C18 C17 C16 1.5(11) . . . . ?
C11 C3 C4 C5 177.8(4) . . . . ?
C21 N3 C25 C26 -179.5(3) . . . . ?
C21 N3 C25 C24 1.4(5) . . . . ?
C21 C22 C23 C24 0.9(8) . . . . ?
C5 C6 C7 C9 -123.4(4) . . . . ?
C5 C6 C7 C8 115.6(4) . . . . ?
C5 C6 C7 C10 -3.8(5) . . . . ?
C31 N4 C27 C28 -11(4) . . . . ?
C15 N1 C19 C20 -178.2(4) . . . . ?
C15 N1 C19 C18 -1.2(6) . . . . ?
C15 C16 C17 C18 -2.6(11) . . . . ?
C26 N2 C20 C19 -100.4(4) . . . . ?
C26 N2 C32' C31' 159(2) . . . . ?
C26 N2 C32 C31 169(3) . . . . ?
C26 C25 C24 C23 178.5(4) . . . . ?
C4 C3 C11 C12 119.1(4) . . . . ?
C4 C3 C11 C13 -120.4(5) . . . . ?
C4 C3 C11 C14 0.6(6) . . . . ?
C20 N2 C26 C25 73.6(4) . . . . ?
C20 N2 C32' C31' -78(4) . . . . ?
C20 N2 C32 C31 -62(4) . . . . ?
C20 C19 C18 C17 177.4(6) . . . . ?
C32' N2 C26 C25 -163(4) . . . . ?
C32' N2 C20 C19 142(3) . . . . ?
C32' C31' N4' Fe 4(3) . . . . ?
C32' C31' N4' C27' -180(3) . . . . ?
C32' C31' C30' C29' 179(3) . . . . ?
C24 C25 C26 N2 -142.0(4) . . . . ?
C27 N4 C31 C30 11(4) . . . . ?
C27 N4 C31 C32 -167(3) . . . . ?
C30 C31 C32 N2 145(3) . . . . ?
C30 C29 C28 C27 -4(3) . . . . ?
C18 C19 C20 N2 160.5(5) . . . . ?
C28 C29 C30 C31 5(4) . . . . ?
C32 N2 C26 C25 -158.7(18) . . . . ?
C32 N2 C20 C19 128.1(14) . . . . ?
C32 C31 C30 C29 170(4) . . . . ?
C31' N4' C27' C28' 2.0(19) . . . . ?
N4' Fe O2 C2 79.0(4) . . . . ?
N4' C31' C30' C29' 0(2) . . . . ?
N4' C27' C28' C29' -2.8(18) . . . . ?
C27' C28' C29' C30' 2.3(16) . . . . ?
C28' C29' C30' C31' -1.1(16) . . . . ?
C30' C31' N4' Fe -177.5(10) . . . . ?
C30' C31' N4' C27' -1(2) . . . . ?

_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
;
_oxdiff_exptl_absorpt_empirical_full_max 1.547
_oxdiff_exptl_absorpt_empirical_full_min 0.575
_symmetry_cell_setting           triclinic
_symmetry_space_group_name_h-m   'P -1'
_symmetry_int_tables_number      2
_chemical_absolute_configuration .

####################################################################### 
# 
# This file contains crystal structure data downloaded from the 
# Cambridge Structural Database (CSD) hosted by the Cambridge 
# Crystallographic Data Centre (CCDC).
# 
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# guidelines are available at http://www.ccdc.cam.ac.uk/access/V1 
# 
# Audit and citation data items may have been added by the CCDC. 
# Please retain this information to preserve the provenance of 
# this file and to allow appropriate attribution of the data. 
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data_tpa36fepf6_100_2
_database_code_depnum_ccdc_archive 'CCDC 2164135'
loop_
_audit_author_name
_audit_author_address
'Oleg Demidov'
;North Caucasus Federal University, Department of Chemistry
Russia
;
_audit_update_record             
;
2022-04-03 deposited with the CCDC.	2022-06-27 downloaded from the CCDC.
;
_audit_creation_date             2021-09-09
_audit_creation_method           
;
Olex2 1.3
(compiled 2020.11.12 svn.r5f609507 for OlexSys, GUI svn.r6272)
;
_shelx_SHELXL_version_number     2014/7
_chemical_name_systematic        
'(3,6-Di-tert-butylcatecholato)-(tris(2-pyridylmethyl)amine)-iron(iii) hexafluorophosphate'
_chemical_name_common            
'(3,6-Di-tert-butylcatecholato)-(tris(2-pyridylmethyl)amine)-iron(iii) hexafluorophosphate'
_chemical_formula_moiety         'C32 H38 Fe N4 O2, 2.002(F3 P0.5)'
_chemical_formula_sum            'C32 H38 F6.01 Fe N4 O2 P'
_chemical_compound_source        'Rostov-on-Don, Russia'
_chemical_formula_weight         711.60
_exptl_crystal_description       block
_exptl_crystal_colour            violet
_diffrn_ambient_temperature      100.01(15)
_chemical_oxdiff_formula         'C32 H38 F6 Fe N4 O2 P'
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'
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'
P P 0.2955 0.4335 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'

_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.
;
_space_group_crystal_system      orthorhombic
_space_group_IT_number           60
_space_group_name_H-M_alt        'P b c n'
_space_group_name_Hall           '-P 2n 2ab'
loop_
_space_group_symop_operation_xyz
'x, y, z'
'-x+1/2, -y+1/2, z+1/2'
'-x, y, -z+1/2'
'x+1/2, -y+1/2, -z'
'-x, -y, -z'
'x-1/2, y-1/2, -z-1/2'
'x, -y, z-1/2'
'-x-1/2, y-1/2, z'

_cell_length_a                   23.8272(3)
_cell_length_b                   18.6423(2)
_cell_length_c                   15.0968(2)
_cell_angle_alpha                90
_cell_angle_beta                 90
_cell_angle_gamma                90
_cell_volume                     6705.91(14)
_cell_formula_units_Z            8
_cell_measurement_reflns_used    16830
_cell_measurement_temperature    100.01(15)
_cell_measurement_theta_max      76.1430
_cell_measurement_theta_min      3.6700
_shelx_estimated_absorpt_T_max   ?
_shelx_estimated_absorpt_T_min   ?
_exptl_absorpt_coefficient_mu    4.661
_exptl_absorpt_correction_T_max  0.969
_exptl_absorpt_correction_T_min  0.891
_exptl_absorpt_correction_type   gaussian
_exptl_absorpt_process_details   
;
CrysAlisPro 1.171.38.41 (Rigaku Oxford Diffraction, 2015)
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_absorpt_special_details   ?
_exptl_crystal_colour_lustre     .
_exptl_crystal_colour_modifier   .
_exptl_crystal_colour_primary    violet
_exptl_crystal_density_diffrn    1.410
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    ?
_exptl_crystal_F_000             2952
loop_
_exptl_crystal_face_index_h
_exptl_crystal_face_index_k
_exptl_crystal_face_index_l
_exptl_crystal_face_perp_dist
11 8 1 0.0493
6 -2 -9 0.1475
15 -2 1 0.0343
-15 2 -1 0.0343
14 -5 0 0.0343
-14 5 0 0.0327
-9 2 8 0.1349
3 -12 0 0.0429
-3 12 0 0.0429
8 10 -1 0.0452
-8 -10 1 0.0433
14 5 1 0.0408
15 0 -3 0.0638
-15 -1 0 0.0353
15 -2 0 0.0338
15 -2 -2 0.0484
14 -5 0 0.0338
-14 5 0 0.0338
12 -8 0 0.0369
-12 8 0 0.0369
-4 -12 0 0.0304

_exptl_crystal_size_max          0.362
_exptl_crystal_size_mid          0.086
_exptl_crystal_size_min          0.067
loop_
_exptl_oxdiff_crystal_face_indexfrac_h
_exptl_oxdiff_crystal_face_indexfrac_k
_exptl_oxdiff_crystal_face_indexfrac_l
_exptl_oxdiff_crystal_face_x
_exptl_oxdiff_crystal_face_y
_exptl_oxdiff_crystal_face_z
11.3735 8.1382 0.8439 -0.4585 0.8439 0.2784
5.6026 -2.2370 -8.9492 0.2416 -0.1126 0.9638
15.2396 -1.9143 0.5758 -0.8198 0.1084 0.5623
-15.2396 1.9143 -0.5758 0.8198 -0.1084 -0.5623
14.1110 -4.9172 0.4562 -0.8131 -0.1503 0.5623
-14.1545 4.8701 -0.1439 0.7949 0.1468 -0.5887
-9.1688 1.5533 7.7903 -0.0070 -0.0063 -1.0000
3.4646 -11.7916 0.4437 -0.4185 -0.8785 0.2305
-3.4646 11.7916 -0.4437 0.4185 0.8785 -0.2305
8.2097 10.2450 -0.5285 -0.1782 0.9534 0.2436
-8.2920 -10.1970 0.6153 0.1777 -0.9507 -0.2543
14.2800 4.6026 0.5040 -0.6462 0.6107 0.4577
14.7959 0.1933 -2.8500 -0.5448 0.2573 0.7981
-15.4006 -1.0816 0.0344 0.7335 -0.3476 -0.5841
15.2535 -1.9821 -0.0071 -0.7854 0.1013 0.6107
14.9999 -2.0534 -1.7092 -0.6680 0.0857 0.7392
14.1635 -4.8554 -0.1263 -0.7782 -0.1464 0.6107
-14.1635 4.8554 0.1263 0.7782 0.1464 -0.6107
12.0746 -7.5637 -0.1058 -0.7277 -0.3974 0.5591
-12.0746 7.5637 0.1058 0.7277 0.3974 -0.5591
-3.8495 -11.7309 -0.0874 -0.0252 -0.9996 -0.0091

_exptl_transmission_factor_max   ?
_exptl_transmission_factor_min   ?
_diffrn_reflns_av_R_equivalents  0.0274
_diffrn_reflns_av_unetI/netI     0.0198
_diffrn_reflns_Laue_measured_fraction_full 0.999
_diffrn_reflns_Laue_measured_fraction_max 0.995
_diffrn_reflns_limit_h_max       29
_diffrn_reflns_limit_h_min       -28
_diffrn_reflns_limit_k_max       19
_diffrn_reflns_limit_k_min       -23
_diffrn_reflns_limit_l_max       18
_diffrn_reflns_limit_l_min       -18
_diffrn_reflns_number            37644
_diffrn_reflns_point_group_measured_fraction_full 0.999
_diffrn_reflns_point_group_measured_fraction_max 0.995
_diffrn_reflns_theta_full        67.684
_diffrn_reflns_theta_max         76.412
_diffrn_reflns_theta_min         3.010
_diffrn_ambient_environment      N~2~
_diffrn_detector                 'CCD plate'
_diffrn_detector_area_resol_mean 5.2529
_diffrn_detector_type            AtlasS2
_diffrn_measured_fraction_theta_full 0.999
_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    -74.00  34.00   1.00    7.00    --  -41.72  77.00-120.00  108
  2  ω      9.00  42.00   1.00    7.00    --   41.72  76.00-167.26   33
  3  ω      8.00  42.00   1.00    7.00    --   41.72  81.00 -68.41   34
  4  ω      7.00  34.00   1.00    7.00    --   41.72  83.00  -5.86   27
  5  ω     27.00  98.00   1.00    7.00    --   41.72-125.00  90.00   71
  6  ω     36.00 109.00   1.00   28.00    --  112.00-111.00  60.00   73
  7  ω     83.00 178.00   1.00   28.00    --  112.00  61.00   0.00   95
  8  ω     36.00 109.00   1.00   28.00    --  112.00-111.00   0.00   73
  9  ω     36.00 104.00   1.00   28.00    --  112.00-111.00-150.00   68
 10  ω     63.00 118.00   1.00   28.00    --  112.00 178.00   0.00   55
 11  ω    117.00 154.00   1.00   28.00    --  112.00 111.00 -90.00   37
 12  ω    103.00 174.00   1.00   28.00    --  112.00  77.00 120.00   71
 13  ω    114.00 141.00   1.00   28.00    --  112.00 178.00 -30.00   27
 14  ω     91.00 123.00   1.00   28.00    --  112.00 178.00-150.00   32
 15  ω     80.00 109.00   1.00   28.00    --  112.00-111.00 150.00   29
 16  ω    116.00 142.00   1.00   28.00    --  112.00  77.00  30.00   26
 17  ω     83.00 177.00   1.00   28.00    --  112.00  61.00  90.00   94
 18  ω     52.00  80.00   1.00   28.00    --  112.00 -95.00 -60.00   28
;
_diffrn_measurement_device       'four-circle diffractometer'
_diffrn_measurement_device_type  'SuperNova, Dual, Cu at zero, AtlasS2'
_diffrn_measurement_method       'ω scans'
_diffrn_orient_matrix_type       
'CrysAlisPro convention (1999,Acta A55,543-557)'
_diffrn_orient_matrix_UB_11      -0.0490831000
_diffrn_orient_matrix_UB_12      0.0187229000
_diffrn_orient_matrix_UB_13      -0.0624056000
_diffrn_orient_matrix_UB_21      0.0169875000
_diffrn_orient_matrix_UB_22      0.0796152000
_diffrn_orient_matrix_UB_23      0.0033128000
_diffrn_orient_matrix_UB_31      0.0385352000
_diffrn_orient_matrix_UB_32      -0.0112674000
_diffrn_orient_matrix_UB_33      -0.0807587000
_diffrn_radiation_monochromator  mirror
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           'Cu K\a'
_diffrn_radiation_wavelength     1.54184
_diffrn_source                   'micro-focus sealed X-ray tube'
_diffrn_source_type              'SuperNova (Cu) X-ray Source'
_reflns_Friedel_coverage         0.000
_reflns_Friedel_fraction_full    .
_reflns_Friedel_fraction_max     .
_reflns_number_gt                6453
_reflns_number_total             7007
_reflns_odcompleteness_completeness 99.91
_reflns_odcompleteness_iscentric 1
_reflns_odcompleteness_theta     66.97
_reflns_special_details          
;
 Reflections were merged by SHELXL according to the crystal
 class for the calculation of statistics and refinement.
 
 Structure factors included contributions from the .fab file.
 
 _reflns_Friedel_fraction is defined as the number of unique
 Friedel pairs measured divided by the number that would be
 possible theoretically, ignoring centric projections and
 systematic absences.
;
_reflns_threshold_expression     'I > 2σ(I)'
_computing_cell_refinement       'CrysAlisPro 1.171.38.41 (Rigaku OD, 2015)'
_computing_data_collection       'CrysAlisPro 1.171.38.41 (Rigaku OD, 2015)'
_computing_data_reduction        'CrysAlisPro 1.171.38.41 (Rigaku OD, 2015)'
_computing_molecular_graphics    'Olex2 1.3 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 1.3 (Dolomanov et al., 2009)'
_computing_structure_refinement  'SHELXL 2014/7 (Sheldrick, 2015)'
_computing_structure_solution    'ShelXT (Sheldrick, 2015)'
_refine_diff_density_max         0.621
_refine_diff_density_min         -0.652
_refine_diff_density_rms         0.047
_refine_ls_extinction_coef       .
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.023
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     451
_refine_ls_number_reflns         7007
_refine_ls_number_restraints     0
_refine_ls_R_factor_all          0.0380
_refine_ls_R_factor_gt           0.0339
_refine_ls_restrained_S_all      1.023
_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)+(0.0401P)²+4.8656P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0842
_refine_ls_wR_factor_ref         0.0877
_refine_special_details          ?
_olex2_refinement_description    
;
1. 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
2. Others
 Sof(F9)=1-FVAR(1)
 Sof(F8)=Sof(F5)=Sof(F7)=Sof(F10)=Sof(F6)=FVAR(1)
3.a Secondary CH2 refined with riding coordinates:
 C26(H26A,H26B), C20(H20A,H20B), C32(H32A,H32B)
3.b Aromatic/amide H refined with riding coordinates:
 C15(H15), C24(H24), C5(H5), C16(H16), C21(H21), C4(H4), C27(H27), C23(H23),
 C18(H18), C22(H22), C28(H28), C17(H17), C30(H30), C29(H29)
3.c Idealised Me refined as rotating group:
 C13(H13A,H13B,H13C), C8(H8A,H8B,H8C), C9(H9A,H9B,H9C), C12(H12A,H12B,H12C),
 C10(H10A,H10B,H10C), C14(H14A,H14B,H14C)
;
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     dual
_atom_sites_solution_secondary   ?
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
Fe Fe 0.68214(2) 0.23448(2) 0.55600(2) 0.01889(7) Uani 1 1 d . . . . .
P2 P 0.5000 0.09063(3) 0.7500 0.02332(13) Uani 1 2 d S T P . .
P1 P 0.5000 0.46288(4) 0.7500 0.0489(2) Uani 1 2 d S T P . .
F3 F 0.5000 0.17757(8) 0.7500 0.0335(3) Uani 1 2 d S T P . .
F1 F 0.5000 0.00501(8) 0.7500 0.0312(3) Uani 1 2 d S T P . .
F2 F 0.55826(4) 0.09191(6) 0.69716(7) 0.0313(2) Uani 1 1 d . . . . .
F4 F 0.53341(5) 0.09112(6) 0.84212(7) 0.0349(2) Uani 1 1 d . . . . .
O2 O 0.74638(5) 0.17929(6) 0.52489(8) 0.0232(2) Uani 1 1 d . . . . .
O1 O 0.73559(5) 0.30530(6) 0.59263(8) 0.0244(2) Uani 1 1 d . . . . .
F8 F 0.5625(3) 0.4591(4) 0.7447(4) 0.0458(13) Uani 0.5015(19) 1 d . . P A 1
N3 N 0.67027(6) 0.19740(8) 0.68834(9) 0.0228(3) Uani 1 1 d . . . . .
N1 N 0.62359(6) 0.15855(7) 0.50846(9) 0.0207(3) Uani 1 1 d . . . . .
N2 N 0.60465(6) 0.28810(8) 0.59622(9) 0.0234(3) Uani 1 1 d . . . . .
N4 N 0.65985(6) 0.29472(8) 0.44019(9) 0.0248(3) Uani 1 1 d . . . . .
C25 C 0.63487(7) 0.23654(9) 0.73782(11) 0.0236(3) Uani 1 1 d . . . . .
C6 C 0.83534(7) 0.32183(9) 0.61302(10) 0.0233(3) Uani 1 1 d . . . . .
C3 C 0.84785(7) 0.17964(9) 0.53807(11) 0.0233(3) Uani 1 1 d . . . . .
C1 C 0.78857(7) 0.28138(9) 0.58570(10) 0.0211(3) Uani 1 1 d . . . . .
C2 C 0.79484(7) 0.21173(9) 0.54831(10) 0.0210(3) Uani 1 1 d . . . . .
C15 C 0.63674(7) 0.09876(9) 0.46270(11) 0.0246(3) Uani 1 1 d . . . . .
H15 H 0.6743 0.0865 0.4560 0.030 Uiso 1 1 calc R U . . .
C24 C 0.62546(8) 0.22113(10) 0.82665(11) 0.0291(4) Uani 1 1 d . . . . .
H24 H 0.6003 0.2484 0.8596 0.035 Uiso 1 1 calc R U . . .
C5 C 0.88745(7) 0.28904(10) 0.60242(11) 0.0275(4) Uani 1 1 d . . . . .
H5 H 0.9195 0.3138 0.6201 0.033 Uiso 1 1 calc R U . . .
C19 C 0.56943(7) 0.17630(9) 0.51888(11) 0.0236(3) Uani 1 1 d . . . . .
C16 C 0.59642(8) 0.05514(10) 0.42546(12) 0.0308(4) Uani 1 1 d . . . . .
H16 H 0.6065 0.0142 0.3940 0.037 Uiso 1 1 calc R U . . .
C21 C 0.69722(8) 0.14198(10) 0.72563(12) 0.0283(4) Uani 1 1 d . . . . .
H21 H 0.7213 0.1145 0.6910 0.034 Uiso 1 1 calc R U . . .
C26 C 0.60906(8) 0.30047(10) 0.69312(11) 0.0282(4) Uani 1 1 d . . . . .
H26A H 0.5720 0.3092 0.7175 0.034 Uiso 1 1 calc R U . . .
H26B H 0.6319 0.3426 0.7042 0.034 Uiso 1 1 calc R U . . .
C4 C 0.89352(7) 0.22065(10) 0.56640(11) 0.0274(4) Uani 1 1 d . . . . .
H4 H 0.9294 0.2015 0.5610 0.033 Uiso 1 1 calc R U . . .
C27 C 0.67908(8) 0.28258(10) 0.35776(12) 0.0299(4) Uani 1 1 d . . . . .
H27 H 0.7079 0.2495 0.3497 0.036 Uiso 1 1 calc R U . . .
C11 C 0.85443(8) 0.10377(10) 0.50059(12) 0.0291(4) Uani 1 1 d . . . . .
C23 C 0.65407(8) 0.16473(11) 0.86528(12) 0.0329(4) Uani 1 1 d . . . . .
H23 H 0.6490 0.1541 0.9249 0.039 Uiso 1 1 calc R U . . .
C20 C 0.55581(8) 0.24116(10) 0.57469(13) 0.0300(4) Uani 1 1 d . . . . .
H20A H 0.5280 0.2697 0.5438 0.036 Uiso 1 1 calc R U . . .
H20B H 0.5390 0.2250 0.6297 0.036 Uiso 1 1 calc R U . . .
F5 F 0.49423(11) 0.38606(14) 0.68976(19) 0.0380(6) Uani 0.5015(19) 1 d . . P A
1
C18 C 0.52681(7) 0.13474(11) 0.48289(12) 0.0310(4) Uani 1 1 d . . . . .
H18 H 0.4895 0.1479 0.4904 0.037 Uiso 1 1 calc R U . . .
C7 C 0.82845(8) 0.39785(10) 0.64988(12) 0.0285(4) Uani 1 1 d . . . . .
C22 C 0.69041(8) 0.12427(11) 0.81403(13) 0.0340(4) Uani 1 1 d . . . . .
H22 H 0.7099 0.0859 0.8386 0.041 Uiso 1 1 calc R U . . .
C28 C 0.65738(9) 0.31772(12) 0.28449(13) 0.0380(4) Uani 1 1 d . . . . .
H28 H 0.6718 0.3089 0.2283 0.046 Uiso 1 1 calc R U . . .
C17 C 0.54040(8) 0.07364(11) 0.43591(12) 0.0340(4) Uani 1 1 d . . . . .
H17 H 0.5123 0.0452 0.4115 0.041 Uiso 1 1 calc R U . . .
C31 C 0.61840(9) 0.34333(10) 0.45142(12) 0.0313(4) Uani 1 1 d . . . . .
C13 C 0.82871(9) 0.09885(11) 0.40714(13) 0.0366(4) Uani 1 1 d . . . . .
H13A H 0.7898 0.1121 0.4096 0.055 Uiso 1 1 calc R U . . .
H13B H 0.8320 0.0506 0.3856 0.055 Uiso 1 1 calc R U . . .
H13C H 0.8483 0.1308 0.3680 0.055 Uiso 1 1 calc R U . . .
C8 C 0.80124(10) 0.44502(10) 0.57870(14) 0.0384(4) Uani 1 1 d . . . . .
H8A H 0.8248 0.4460 0.5271 0.058 Uiso 1 1 calc R U . . .
H8B H 0.7967 0.4929 0.6011 0.058 Uiso 1 1 calc R U . . .
H8C H 0.7652 0.4257 0.5633 0.058 Uiso 1 1 calc R U . . .
C32 C 0.60221(9) 0.35635(10) 0.54657(12) 0.0328(4) Uani 1 1 d . . . . .
H32A H 0.6277 0.3909 0.5730 0.039 Uiso 1 1 calc R U . . .
H32B H 0.5645 0.3759 0.5493 0.039 Uiso 1 1 calc R U . . .
C9 C 0.79153(9) 0.39700(11) 0.73316(13) 0.0370(5) Uani 1 1 d . . . . .
H9A H 0.7561 0.3750 0.7196 0.056 Uiso 1 1 calc R U . . .
H9B H 0.7854 0.4453 0.7530 0.056 Uiso 1 1 calc R U . . .
H9C H 0.8100 0.3701 0.7790 0.056 Uiso 1 1 calc R U . . .
C12 C 0.82449(10) 0.05026(11) 0.56130(15) 0.0404(5) Uani 1 1 d . . . . .
H12A H 0.8422 0.0503 0.6184 0.061 Uiso 1 1 calc R U . . .
H12B H 0.8267 0.0031 0.5360 0.061 Uiso 1 1 calc R U . . .
H12C H 0.7858 0.0639 0.5675 0.061 Uiso 1 1 calc R U . . .
C10 C 0.88490(9) 0.43161(12) 0.67463(16) 0.0442(5) Uani 1 1 d . . . . .
H10A H 0.9030 0.4027 0.7188 0.066 Uiso 1 1 calc R U . . .
H10B H 0.8788 0.4790 0.6977 0.066 Uiso 1 1 calc R U . . .
H10C H 0.9083 0.4344 0.6229 0.066 Uiso 1 1 calc R U . . .
C30 C 0.59372(10) 0.37941(12) 0.38109(14) 0.0404(5) Uani 1 1 d . . . . .
H30 H 0.5645 0.4115 0.3906 0.048 Uiso 1 1 calc R U . . .
C29 C 0.61373(10) 0.36641(12) 0.29626(14) 0.0436(5) Uani 1 1 d . . . . .
H29 H 0.5981 0.3900 0.2478 0.052 Uiso 1 1 calc R U . . .
C14 C 0.91607(9) 0.08117(13) 0.49481(18) 0.0495(6) Uani 1 1 d . . . . .
H14A H 0.9358 0.1132 0.4559 0.074 Uiso 1 1 calc R U . . .
H14B H 0.9184 0.0331 0.4722 0.074 Uiso 1 1 calc R U . . .
H14C H 0.9327 0.0830 0.5527 0.074 Uiso 1 1 calc R U . . .
F7 F 0.50193(11) 0.50051(16) 0.64441(18) 0.0494(7) Uani 0.5015(19) 1 d . . P A
1
F10 F 0.50467(12) 0.54051(16) 0.7156(2) 0.0583(8) Uani 0.5015(19) 1 d . . P A 2
F6 F 0.51141(13) 0.4247(2) 0.66854(18) 0.0583(9) Uani 0.5015(19) 1 d . . P A 2
F9 F 0.5713(3) 0.4670(4) 0.7716(4) 0.0375(10) Uani 0.4985(19) 1 d . . P A 2


_geom_special_details            
;
 All esds (except the esd in the dihedral angle between two l.s. planes)
 are estimated using the full covariance matrix.  The cell esds are taken
 into account individually in the estimation of esds in distances, angles
 and torsion angles; correlations between esds in cell parameters are only
 used when they are defined by crystal symmetry.  An approximate (isotropic)
 treatment of cell esds is used for estimating esds involving l.s. planes.
;
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
Fe O2 1.9031(12) . ?
Fe O1 1.9160(12) . ?
Fe N3 2.1330(14) . ?
Fe N1 2.1129(14) . ?
Fe N2 2.1857(14) . ?
Fe N4 2.1448(15) . ?
P2 F3 1.6208(15) . ?
P2 F1 1.5961(15) . ?
P2 F2 1.6013(10) 3_656 ?
P2 F2 1.6013(10) . ?
P2 F4 1.6024(11) . ?
P2 F4 1.6024(11) 3_656 ?
P1 F8 1.494(7) . ?
P1 F8 1.494(7) 3_656 ?
P1 F5 1.702(3) . ?
P1 F5 1.702(3) 3_656 ?
P1 F7 1.742(3) . ?
P1 F7 1.742(3) 3_656 ?
P1 F10 1.541(3) 3_656 ?
P1 F10 1.541(3) . ?
P1 F6 1.447(3) 3_656 ?
P1 F6 1.447(3) . ?
P1 F9 1.731(6) . ?
P1 F9 1.731(6) 3_656 ?
O2 C2 1.351(2) . ?
O1 C1 1.343(2) . ?
N3 C25 1.342(2) . ?
N3 C21 1.340(2) . ?
N1 C15 1.348(2) . ?
N1 C19 1.342(2) . ?
N2 C26 1.485(2) . ?
N2 C20 1.492(2) . ?
N2 C32 1.478(2) . ?
N4 C27 1.345(2) . ?
N4 C31 1.351(2) . ?
C25 C24 1.390(2) . ?
C25 C26 1.501(2) . ?
C6 C1 1.407(2) . ?
C6 C5 1.393(3) . ?
C6 C7 1.531(2) . ?
C3 C2 1.406(2) . ?
C3 C4 1.397(2) . ?
C3 C11 1.531(2) . ?
C1 C2 1.424(2) . ?
C15 H15 0.9300 . ?
C15 C16 1.379(2) . ?
C24 H24 0.9300 . ?
C24 C23 1.382(3) . ?
C5 H5 0.9300 . ?
C5 C4 1.394(3) . ?
C19 C20 1.509(3) . ?
C19 C18 1.388(2) . ?
C16 H16 0.9300 . ?
C16 C17 1.388(3) . ?
C21 H21 0.9300 . ?
C21 C22 1.384(3) . ?
C26 H26A 0.9700 . ?
C26 H26B 0.9700 . ?
C4 H4 0.9300 . ?
C27 H27 0.9300 . ?
C27 C28 1.386(3) . ?
C11 C13 1.541(3) . ?
C11 C12 1.531(3) . ?
C11 C14 1.531(3) . ?
C23 H23 0.9300 . ?
C23 C22 1.385(3) . ?
C20 H20A 0.9700 . ?
C20 H20B 0.9700 . ?
C18 H18 0.9300 . ?
C18 C17 1.380(3) . ?
C7 C8 1.532(3) . ?
C7 C9 1.535(3) . ?
C7 C10 1.531(3) . ?
C22 H22 0.9300 . ?
C28 H28 0.9300 . ?
C28 C29 1.392(3) . ?
C17 H17 0.9300 . ?
C31 C32 1.507(2) . ?
C31 C30 1.388(3) . ?
C13 H13A 0.9600 . ?
C13 H13B 0.9600 . ?
C13 H13C 0.9600 . ?
C8 H8A 0.9600 . ?
C8 H8B 0.9600 . ?
C8 H8C 0.9600 . ?
C32 H32A 0.9700 . ?
C32 H32B 0.9700 . ?
C9 H9A 0.9600 . ?
C9 H9B 0.9600 . ?
C9 H9C 0.9600 . ?
C12 H12A 0.9600 . ?
C12 H12B 0.9600 . ?
C12 H12C 0.9600 . ?
C10 H10A 0.9600 . ?
C10 H10B 0.9600 . ?
C10 H10C 0.9600 . ?
C30 H30 0.9300 . ?
C30 C29 1.388(3) . ?
C29 H29 0.9300 . ?
C14 H14A 0.9600 . ?
C14 H14B 0.9600 . ?
C14 H14C 0.9600 . ?
F10 F10 1.061(6) 3_656 ?

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 Fe O1 84.79(5) . . ?
O2 Fe N3 99.36(5) . . ?
O2 Fe N1 94.88(5) . . ?
O2 Fe N2 174.41(5) . . ?
O2 Fe N4 106.32(5) . . ?
O1 Fe N3 92.36(5) . . ?
O1 Fe N1 176.86(5) . . ?
O1 Fe N2 99.56(5) . . ?
O1 Fe N4 92.23(5) . . ?
N3 Fe N2 77.05(5) . . ?
N3 Fe N4 154.21(6) . . ?
N1 Fe N3 90.78(5) . . ?
N1 Fe N2 80.97(5) . . ?
N1 Fe N4 84.86(5) . . ?
N4 Fe N2 77.16(6) . . ?
F1 P2 F3 180.0 . . ?
F1 P2 F2 90.85(4) . 3_656 ?
F1 P2 F2 90.85(4) . . ?
F1 P2 F4 90.32(5) . . ?
F1 P2 F4 90.32(5) . 3_656 ?
F2 P2 F3 89.15(4) . . ?
F2 P2 F3 89.15(4) 3_656 . ?
F2 P2 F2 178.30(9) 3_656 . ?
F2 P2 F4 90.09(6) 3_656 3_656 ?
F2 P2 F4 89.90(6) . 3_656 ?
F2 P2 F4 89.90(6) 3_656 . ?
F2 P2 F4 90.09(6) . . ?
F4 P2 F3 89.68(5) . . ?
F4 P2 F3 89.68(5) 3_656 . ?
F4 P2 F4 179.36(9) 3_656 . ?
F8 P1 F8 174.6(6) . 3_656 ?
F8 P1 F5 84.7(3) 3_656 . ?
F8 P1 F5 84.7(3) . 3_656 ?
F8 P1 F5 90.7(3) 3_656 3_656 ?
F8 P1 F5 90.7(3) . . ?
F8 P1 F7 95.4(2) 3_656 . ?
F8 P1 F7 86.8(3) . . ?
F8 P1 F7 86.8(3) 3_656 3_656 ?
F8 P1 F7 95.4(2) . 3_656 ?
F5 P1 F5 65.4(2) 3_656 . ?
F5 P1 F7 81.49(14) 3_656 3_656 ?
F5 P1 F7 81.50(14) . . ?
F5 P1 F7 145.64(15) . 3_656 ?
F5 P1 F7 145.65(15) 3_656 . ?
F7 P1 F7 132.5(2) . 3_656 ?
F10 P1 F10 40.3(2) . 3_656 ?
F10 P1 F9 87.2(3) 3_656 3_656 ?
F10 P1 F9 88.0(2) . 3_656 ?
F10 P1 F9 88.0(2) 3_656 . ?
F10 P1 F9 87.2(3) . . ?
F6 P1 F10 99.4(2) . . ?
F6 P1 F10 139.6(2) . 3_656 ?
F6 P1 F10 99.4(2) 3_656 3_656 ?
F6 P1 F10 139.6(2) 3_656 . ?
F6 P1 F6 121.0(3) . 3_656 ?
F6 P1 F9 92.7(2) 3_656 . ?
F6 P1 F9 92.7(2) . 3_656 ?
F6 P1 F9 89.8(2) . . ?
F6 P1 F9 89.8(2) 3_656 3_656 ?
F9 P1 F9 174.9(5) 3_656 . ?
C2 O2 Fe 112.40(10) . . ?
C1 O1 Fe 111.93(10) . . ?
C25 N3 Fe 115.36(11) . . ?
C21 N3 Fe 125.42(12) . . ?
C21 N3 C25 119.11(15) . . ?
C15 N1 Fe 125.06(11) . . ?
C19 N1 Fe 115.47(11) . . ?
C19 N1 C15 119.18(14) . . ?
C26 N2 Fe 106.56(10) . . ?
C26 N2 C20 111.17(14) . . ?
C20 N2 Fe 109.27(10) . . ?
C32 N2 Fe 106.62(11) . . ?
C32 N2 C26 111.64(14) . . ?
C32 N2 C20 111.34(15) . . ?
C27 N4 Fe 125.56(13) . . ?
C27 N4 C31 118.55(16) . . ?
C31 N4 Fe 115.46(11) . . ?
N3 C25 C24 121.73(17) . . ?
N3 C25 C26 116.03(14) . . ?
C24 C25 C26 122.12(16) . . ?
C1 C6 C7 121.16(16) . . ?
C5 C6 C1 115.91(16) . . ?
C5 C6 C7 122.92(15) . . ?
C2 C3 C11 121.70(15) . . ?
C4 C3 C2 115.68(16) . . ?
C4 C3 C11 122.60(16) . . ?
O1 C1 C6 122.93(15) . . ?
O1 C1 C2 115.62(14) . . ?
C6 C1 C2 121.45(15) . . ?
O2 C2 C3 123.28(15) . . ?
O2 C2 C1 114.99(15) . . ?
C3 C2 C1 121.72(15) . . ?
N1 C15 H15 118.8 . . ?
N1 C15 C16 122.33(17) . . ?
C16 C15 H15 118.8 . . ?
C25 C24 H24 120.5 . . ?
C23 C24 C25 119.01(18) . . ?
C23 C24 H24 120.5 . . ?
C6 C5 H5 118.7 . . ?
C6 C5 C4 122.59(16) . . ?
C4 C5 H5 118.7 . . ?
N1 C19 C20 118.03(15) . . ?
N1 C19 C18 121.34(16) . . ?
C18 C19 C20 120.57(16) . . ?
C15 C16 H16 120.7 . . ?
C15 C16 C17 118.52(18) . . ?
C17 C16 H16 120.7 . . ?
N3 C21 H21 118.9 . . ?
N3 C21 C22 122.17(18) . . ?
C22 C21 H21 118.9 . . ?
N2 C26 C25 110.40(14) . . ?
N2 C26 H26A 109.6 . . ?
N2 C26 H26B 109.6 . . ?
C25 C26 H26A 109.6 . . ?
C25 C26 H26B 109.6 . . ?
H26A C26 H26B 108.1 . . ?
C3 C4 H4 118.7 . . ?
C5 C4 C3 122.64(16) . . ?
C5 C4 H4 118.7 . . ?
N4 C27 H27 118.9 . . ?
N4 C27 C28 122.13(19) . . ?
C28 C27 H27 118.9 . . ?
C3 C11 C13 110.64(15) . . ?
C12 C11 C3 109.45(15) . . ?
C12 C11 C13 108.90(17) . . ?
C14 C11 C3 111.93(16) . . ?
C14 C11 C13 108.24(17) . . ?
C14 C11 C12 107.58(18) . . ?
C24 C23 H23 120.4 . . ?
C24 C23 C22 119.14(17) . . ?
C22 C23 H23 120.4 . . ?
N2 C20 C19 115.09(14) . . ?
N2 C20 H20A 108.5 . . ?
N2 C20 H20B 108.5 . . ?
C19 C20 H20A 108.5 . . ?
C19 C20 H20B 108.5 . . ?
H20A C20 H20B 107.5 . . ?
C19 C18 H18 120.3 . . ?
C17 C18 C19 119.35(17) . . ?
C17 C18 H18 120.3 . . ?
C6 C7 C8 108.76(15) . . ?
C6 C7 C9 110.47(14) . . ?
C6 C7 C10 112.00(16) . . ?
C8 C7 C9 109.75(17) . . ?
C10 C7 C8 107.87(17) . . ?
C10 C7 C9 107.93(16) . . ?
C21 C22 C23 118.82(18) . . ?
C21 C22 H22 120.6 . . ?
C23 C22 H22 120.6 . . ?
C27 C28 H28 120.5 . . ?
C27 C28 C29 119.03(18) . . ?
C29 C28 H28 120.5 . . ?
C16 C17 H17 120.4 . . ?
C18 C17 C16 119.29(17) . . ?
C18 C17 H17 120.4 . . ?
N4 C31 C32 114.51(16) . . ?
N4 C31 C30 122.60(17) . . ?
C30 C31 C32 122.87(18) . . ?
C11 C13 H13A 109.5 . . ?
C11 C13 H13B 109.5 . . ?
C11 C13 H13C 109.5 . . ?
H13A C13 H13B 109.5 . . ?
H13A C13 H13C 109.5 . . ?
H13B C13 H13C 109.5 . . ?
C7 C8 H8A 109.5 . . ?
C7 C8 H8B 109.5 . . ?
C7 C8 H8C 109.5 . . ?
H8A C8 H8B 109.5 . . ?
H8A C8 H8C 109.5 . . ?
H8B C8 H8C 109.5 . . ?
N2 C32 C31 109.55(14) . . ?
N2 C32 H32A 109.8 . . ?
N2 C32 H32B 109.8 . . ?
C31 C32 H32A 109.8 . . ?
C31 C32 H32B 109.8 . . ?
H32A C32 H32B 108.2 . . ?
C7 C9 H9A 109.5 . . ?
C7 C9 H9B 109.5 . . ?
C7 C9 H9C 109.5 . . ?
H9A C9 H9B 109.5 . . ?
H9A C9 H9C 109.5 . . ?
H9B C9 H9C 109.5 . . ?
C11 C12 H12A 109.5 . . ?
C11 C12 H12B 109.5 . . ?
C11 C12 H12C 109.5 . . ?
H12A C12 H12B 109.5 . . ?
H12A C12 H12C 109.5 . . ?
H12B C12 H12C 109.5 . . ?
C7 C10 H10A 109.5 . . ?
C7 C10 H10B 109.5 . . ?
C7 C10 H10C 109.5 . . ?
H10A C10 H10B 109.5 . . ?
H10A C10 H10C 109.5 . . ?
H10B C10 H10C 109.5 . . ?
C31 C30 H30 120.8 . . ?
C31 C30 C29 118.4(2) . . ?
C29 C30 H30 120.8 . . ?
C28 C29 H29 120.4 . . ?
C30 C29 C28 119.22(19) . . ?
C30 C29 H29 120.4 . . ?
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 . . ?
F10 F10 P1 69.86(12) 3_656 . ?

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
Fe O2 C2 C3 175.47(12) . . . . ?
Fe O2 C2 C1 -3.77(17) . . . . ?
Fe O1 C1 C6 -176.47(12) . . . . ?
Fe O1 C1 C2 3.72(17) . . . . ?
Fe N3 C25 C24 -176.38(13) . . . . ?
Fe N3 C25 C26 -0.17(19) . . . . ?
Fe N3 C21 C22 175.07(14) . . . . ?
Fe N1 C15 C16 -173.07(13) . . . . ?
Fe N1 C19 C20 -9.24(19) . . . . ?
Fe N1 C19 C18 173.56(13) . . . . ?
Fe N2 C26 C25 -40.46(16) . . . . ?
Fe N2 C20 C19 -9.50(18) . . . . ?
Fe N2 C32 C31 43.91(18) . . . . ?
Fe N4 C27 C28 171.53(14) . . . . ?
Fe N4 C31 C32 10.6(2) . . . . ?
Fe N4 C31 C30 -170.81(17) . . . . ?
O1 C1 C2 O2 0.0(2) . . . . ?
O1 C1 C2 C3 -179.24(14) . . . . ?
N3 C25 C24 C23 1.1(3) . . . . ?
N3 C25 C26 N2 28.4(2) . . . . ?
N3 C21 C22 C23 0.7(3) . . . . ?
N1 C15 C16 C17 -0.2(3) . . . . ?
N1 C19 C20 N2 12.9(2) . . . . ?
N1 C19 C18 C17 0.4(3) . . . . ?
N4 C27 C28 C29 -0.9(3) . . . . ?
N4 C31 C32 N2 -37.4(2) . . . . ?
N4 C31 C30 C29 -2.0(3) . . . . ?
C25 N3 C21 C22 -1.0(3) . . . . ?
C25 C24 C23 C22 -1.3(3) . . . . ?
C6 C1 C2 O2 -179.80(14) . . . . ?
C6 C1 C2 C3 0.9(2) . . . . ?
C6 C5 C4 C3 0.0(3) . . . . ?
C1 C6 C5 C4 0.5(2) . . . . ?
C1 C6 C7 C8 -60.5(2) . . . . ?
C1 C6 C7 C9 60.0(2) . . . . ?
C1 C6 C7 C10 -179.61(17) . . . . ?
C2 C3 C4 C5 -0.1(2) . . . . ?
C2 C3 C11 C13 58.5(2) . . . . ?
C2 C3 C11 C12 -61.6(2) . . . . ?
C2 C3 C11 C14 179.28(18) . . . . ?
C15 N1 C19 C20 176.63(15) . . . . ?
C15 N1 C19 C18 -0.6(2) . . . . ?
C15 C16 C17 C18 0.0(3) . . . . ?
C24 C25 C26 N2 -155.45(16) . . . . ?
C24 C23 C22 C21 0.4(3) . . . . ?
C5 C6 C1 O1 179.22(15) . . . . ?
C5 C6 C1 C2 -1.0(2) . . . . ?
C5 C6 C7 C8 118.03(19) . . . . ?
C5 C6 C7 C9 -121.46(19) . . . . ?
C5 C6 C7 C10 -1.1(2) . . . . ?
C19 N1 C15 C16 0.5(2) . . . . ?
C19 C18 C17 C16 -0.2(3) . . . . ?
C21 N3 C25 C24 0.0(2) . . . . ?
C21 N3 C25 C26 176.25(15) . . . . ?
C26 N2 C20 C19 -126.83(16) . . . . ?
C26 N2 C32 C31 159.92(16) . . . . ?
C26 C25 C24 C23 -174.89(17) . . . . ?
C4 C3 C2 O2 -179.55(15) . . . . ?
C4 C3 C2 C1 -0.4(2) . . . . ?
C4 C3 C11 C13 -123.29(18) . . . . ?
C4 C3 C11 C12 116.70(19) . . . . ?
C4 C3 C11 C14 -2.5(3) . . . . ?
C27 N4 C31 C32 -176.47(17) . . . . ?
C27 N4 C31 C30 2.1(3) . . . . ?
C27 C28 C29 C30 1.1(3) . . . . ?
C11 C3 C2 O2 -1.2(2) . . . . ?
C11 C3 C2 C1 178.01(15) . . . . ?
C11 C3 C4 C5 -178.47(16) . . . . ?
C20 N2 C26 C25 78.51(18) . . . . ?
C20 N2 C32 C31 -75.2(2) . . . . ?
C20 C19 C18 C17 -176.71(17) . . . . ?
C18 C19 C20 N2 -169.91(16) . . . . ?
C7 C6 C1 O1 -2.2(2) . . . . ?
C7 C6 C1 C2 177.62(15) . . . . ?
C7 C6 C5 C4 -178.06(16) . . . . ?
C31 N4 C27 C28 -0.7(3) . . . . ?
C31 C30 C29 C28 0.3(3) . . . . ?
C32 N2 C26 C25 -156.50(15) . . . . ?
C32 N2 C20 C19 108.01(17) . . . . ?
C32 C31 C30 C29 176.5(2) . . . . ?
C30 C31 C32 N2 144.0(2) . . . . ?
F6 P1 F10 F10 0.5(5) 3_656 . . 3_656 ?
F6 P1 F10 F10 -179.7(3) . . . 3_656 ?
F9 P1 F10 F10 87.9(4) 3_656 . . 3_656 ?
F9 P1 F10 F10 -90.3(4) . . . 3_656 ?

_smtbx_masks_special_details     ?
loop_
_smtbx_masks_void_nr
_smtbx_masks_void_average_x
_smtbx_masks_void_average_y
_smtbx_masks_void_average_z
_smtbx_masks_void_volume
_smtbx_masks_void_count_electrons
_smtbx_masks_void_content
1 0.000 0.268 0.750 72.8 5.7 ?
2 0.000 0.732 0.250 72.8 5.5 ?
3 0.196 -0.003 0.252 17.2 0.0 ?
4 0.196 0.003 0.752 17.2 0.0 ?
5 0.304 0.497 0.252 17.2 0.0 ?
6 0.304 0.503 0.752 17.2 0.2 ?
7 0.500 0.232 0.250 72.8 5.7 ?
8 0.500 0.768 0.750 72.8 5.5 ?
9 0.696 0.503 0.748 17.2 0.0 ?
10 0.696 0.497 0.248 17.2 0.0 ?
11 0.804 0.003 0.748 17.2 0.0 ?
12 0.804 0.997 0.248 17.2 0.0 ?

_smtbx_masks_void_probe_radius   1.2
_smtbx_masks_void_truncation_radius 1.2
_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
;
_oxdiff_exptl_absorpt_empirical_full_max 1.707
_oxdiff_exptl_absorpt_empirical_full_min 0.589
_symmetry_cell_setting           orthorhombic
_symmetry_space_group_name_h-m   'P b c n'
_symmetry_int_tables_number      60
_chemical_absolute_configuration .

####################################################################### 
# 
# This file contains crystal structure data downloaded from the 
# Cambridge Structural Database (CSD) hosted by the Cambridge 
# Crystallographic Data Centre (CCDC).
# 
# Full information about CCDC data access policies and citation 
# guidelines are available at http://www.ccdc.cam.ac.uk/access/V1 
# 
# Audit and citation data items may have been added by the CCDC. 
# Please retain this information to preserve the provenance of 
# this file and to allow appropriate attribution of the data. 
# 
#######################################################################

data_tpa36fepf6
_database_code_depnum_ccdc_archive 'CCDC 2164133'
loop_
_audit_author_name
_audit_author_address
'Oleg Demidov'
;North Caucasus Federal University, Department of Chemistry
Russia
;
_audit_update_record             
;
2022-04-03 deposited with the CCDC.	2022-06-27 downloaded from the CCDC.
;
_audit_creation_date             2021-09-09
_audit_creation_method           
;
Olex2 1.3
(compiled 2020.11.12 svn.r5f609507 for OlexSys, GUI svn.r6272)
;
_shelx_SHELXL_version_number     2014/7
_chemical_name_systematic        
'(3,6-Di-tert-butylcatecholato)-(tris(2-pyridylmethyl)amine)-iron(iii) hexafluorophosphate'
_chemical_name_common            
'(3,6-Di-tert-butylcatecholato)-(tris(2-pyridylmethyl)amine)-iron(iii) hexafluorophosphate'
_chemical_formula_moiety         'C32 H38 Fe N4 O2, 2(F3 P0.5)'
_chemical_formula_sum            'C32 H38 F6 Fe N4 O2 P'
_chemical_formula_weight         711.48
_exptl_crystal_description       block
_exptl_crystal_colour            violet
_diffrn_ambient_temperature      293(2)
_chemical_oxdiff_formula         'C32 H38 F6 Fe N4 O2 P'
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'
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'
P P 0.2955 0.4335 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'

_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.
;
_space_group_crystal_system      orthorhombic
_space_group_IT_number           60
_space_group_name_H-M_alt        'P b c n'
_space_group_name_Hall           '-P 2n 2ab'
loop_
_space_group_symop_operation_xyz
'x, y, z'
'-x+1/2, -y+1/2, z+1/2'
'-x, y, -z+1/2'
'x+1/2, -y+1/2, -z'
'-x, -y, -z'
'x-1/2, y-1/2, -z-1/2'
'x, -y, z-1/2'
'-x-1/2, y-1/2, z'

_cell_length_a                   24.0039(3)
_cell_length_b                   18.8295(2)
_cell_length_c                   15.30660(10)
_cell_angle_alpha                90
_cell_angle_beta                 90
_cell_angle_gamma                90
_cell_volume                     6918.30(12)
_cell_formula_units_Z            8
_cell_measurement_reflns_used    22603
_cell_measurement_temperature    293(2)
_cell_measurement_theta_max      76.0780
_cell_measurement_theta_min      2.9570
_shelx_estimated_absorpt_T_max   0.773
_shelx_estimated_absorpt_T_min   0.273
_exptl_absorpt_coefficient_mu    4.518
_exptl_absorpt_correction_T_max  1.000
_exptl_absorpt_correction_T_min  0.547
_exptl_absorpt_correction_type   gaussian
_exptl_absorpt_process_details   
;
CrysAlisPro 1.171.40.67a (Rigaku Oxford Diffraction, 2019)
Numerical absorption correction based on gaussian integration over
			a multifaceted crystal model
;
_exptl_absorpt_special_details   ?
_exptl_crystal_colour_lustre     .
_exptl_crystal_colour_modifier   .
_exptl_crystal_colour_primary    violet
_exptl_crystal_density_diffrn    1.366
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    ?
_exptl_crystal_F_000             2952
loop_
_exptl_crystal_face_index_h
_exptl_crystal_face_index_k
_exptl_crystal_face_index_l
_exptl_crystal_face_perp_dist
-5 11 1 0.0519
15 3 0 0.0353
13 6 0 0.0395
-6 -11 -1 0.0481
-6 4 9 0.1643
1 12 0 0.0481
-5 12 0 0.0475
5 -12 0 0.0475
9 -8 4 0.1091
-13 7 -1 0.0445
15 -3 0 0.0391
15 0 3 0.0721
-15 -3 1 0.0175
-15 -3 -1 0.0290
13 6 1 0.0375
9 2 -8 0.1406

_exptl_crystal_size_max          0.388
_exptl_crystal_size_mid          0.095
_exptl_crystal_size_min          0.06
loop_
_exptl_oxdiff_crystal_face_indexfrac_h
_exptl_oxdiff_crystal_face_indexfrac_k
_exptl_oxdiff_crystal_face_indexfrac_l
_exptl_oxdiff_crystal_face_x
_exptl_oxdiff_crystal_face_y
_exptl_oxdiff_crystal_face_z
-5.4453 11.3992 0.8804 0.2825 -0.9494 0.1375
14.9801 3.3580 0.0407 -0.7778 -0.2325 -0.5839
13.4021 6.2305 -0.0740 -0.6765 -0.4674 -0.5692
-6.1948 -11.1874 -0.6133 0.3162 0.8975 0.3075
-5.9307 3.9462 8.6105 -0.1647 -0.4609 0.8720
1.0004 12.1869 0.3708 -0.0246 -0.9885 -0.1490
-4.6905 11.6523 0.1696 0.2845 -0.9574 0.0490
4.6905 -11.6523 -0.1696 -0.2845 0.9574 -0.0490
9.4776 -7.9696 4.4981 -0.7890 0.6039 0.1129
-12.9805 6.7248 -0.5636 0.7432 -0.5701 0.3502
15.0515 -3.1440 0.2488 -0.8198 0.2905 -0.4935
14.9901 -0.3014 2.7014 -0.9455 0.0246 -0.3248
-14.9399 -3.2872 0.8923 0.7225 0.2133 0.6576
-14.9513 -3.3386 -0.6654 0.8121 0.2402 0.5318
13.2948 6.3340 0.5602 -0.7067 -0.4853 -0.5148
8.8332 1.6441 -8.0745 0.0037 0.0086 -1.0000

_exptl_transmission_factor_max   ?
_exptl_transmission_factor_min   ?
_diffrn_reflns_av_R_equivalents  0.1058
_diffrn_reflns_av_unetI/netI     0.0381
_diffrn_reflns_Laue_measured_fraction_full 1.000
_diffrn_reflns_Laue_measured_fraction_max 0.998
_diffrn_reflns_limit_h_max       27
_diffrn_reflns_limit_h_min       -30
_diffrn_reflns_limit_k_max       23
_diffrn_reflns_limit_k_min       -23
_diffrn_reflns_limit_l_max       19
_diffrn_reflns_limit_l_min       -15
_diffrn_reflns_number            104873
_diffrn_reflns_point_group_measured_fraction_full 1.000
_diffrn_reflns_point_group_measured_fraction_max 0.998
_diffrn_reflns_theta_full        67.684
_diffrn_reflns_theta_max         76.500
_diffrn_reflns_theta_min         2.983
_diffrn_detector                 'CCD plate'
_diffrn_detector_area_resol_mean 5.2529
_diffrn_detector_type            AtlasS2
_diffrn_measured_fraction_theta_full 1.000
_diffrn_measured_fraction_theta_max 0.998
_diffrn_measurement_details      
;
List of Runs (angles in degrees, time in seconds):

  # Type    Start    End  Width  tₑₓₚ   ω     θ     κ     φ   Frames
#--------------------------------------------------------------------------
  1  ω   -105.00 -19.00   1.00    4.50    --  -41.72 -38.00 -90.00   86
  2  ω    -71.00  34.00   1.00    4.50    --  -41.72  77.00  30.00  105
  3  ω    -60.00  19.00   1.00    4.50    --  -41.72  57.00 150.00   79
  4  ω   -115.00 -17.00   1.00    4.50    --  -41.72 -38.00-180.00   98
  5  ω     46.00  75.00   1.00    4.50    --   41.72  57.00 -60.00   29
  6  ω     39.00  95.00   1.00    4.50    --   41.72-125.00-120.00   56
  7  ω     84.00 148.00   1.00   18.00    --  112.00  61.00 120.00   64
  8  ω     81.00 107.00   1.00   18.00    --  112.00 -21.00  17.88   26
  9  ω     83.00 109.00   1.00   18.00    --  112.00 -87.00  83.69   26
 10  ω     40.00 109.00   1.00   18.00    --  112.00-111.00-120.00   69
 11  ω     73.00  98.00   1.00   18.00    --  112.00 -95.00 -30.00   25
 12  ω     36.00  62.00   1.00   18.00    --  112.00-111.00 -90.00   26
 13  ω     71.00 109.00   1.00   18.00    --  112.00-111.00 -90.00   38
 14  ω     69.00 120.00   1.00   18.00    --  112.00 178.00-180.00   51
 15  ω     60.00  93.00   1.00   18.00    --  112.00 -95.00 -90.00   33
 16  ω     58.00  85.00   1.00   18.00    --  112.00 -24.00  15.13   27
 17  ω     25.00  54.00   1.00   18.00    --  112.00   0.00 -60.00   29
 18  ω     73.00 109.00   1.00   18.00    --  112.00-111.00 -30.00   36
 19  ω     79.00 113.00   1.00   18.00    --  112.00   0.00 -60.00   34
 20  ω    120.00 178.00   1.00   18.00    --  112.00   0.00 -60.00   58
 21  ω     34.00  61.00   1.00   18.00    --  112.00 -15.00 -60.00   27
 22  ω     61.00 109.00   1.00   18.00    --  112.00-111.00  90.00   48
 23  ω     55.00  81.00   1.00   18.00    --  112.00 -95.00 -60.00   26
 24  ω    128.00 177.00   1.00   18.00    --  112.00  61.00   0.00   49
 25  ω     59.00 109.00   1.00   18.00    --  112.00-111.00-180.00   50
 26  ω     70.00 102.00   1.00   18.00    --  112.00-111.00 120.00   32
 27  ω     69.00 109.00   1.00   18.00    --  112.00-111.00 150.00   40
 28  ω     42.00 108.00   1.00   18.00    --  112.00 -45.00 -60.00   66
 29  ω     68.00  96.00   1.00   18.00    --  112.00  18.00  35.32   28
 30  ω     69.00 109.00   1.00   18.00    --  112.00-111.00-150.00   40
 31  ω     97.00 130.00   1.00   18.00    --  112.00 -61.00 -60.00   33
 32  ω     42.00  81.00   1.00   18.00    --  112.00 -61.00 -60.00   39
 33  ω    104.00 132.00   1.00   18.00    --  112.00 111.00  60.00   28
 34  ω     58.00 108.00   1.00   18.00    --  112.00 -45.00 120.00   50
 35  ω     54.00  86.00   1.00   18.00    --  112.00 -61.00-120.00   32
 36  ω     70.00 109.00   1.00   18.00    --  112.00-111.00  30.00   39
 37  ω     41.00 136.00   1.00   18.00    --  112.00 -30.00 -60.00   95
 38  ω     81.00 116.00   1.00   18.00    --  112.00  15.00-150.00   35
 39  ω    125.00 167.00   1.00   18.00    --  112.00  15.00-150.00   42
 40  ω     43.00  69.00   1.00   18.00    --  112.00 -45.00 150.00   26
 41  ω     84.00 133.00   1.00   18.00    --  112.00 -45.00 150.00   49
 42  ω     43.00  72.00   1.00   18.00    --  112.00 -61.00 -90.00   29
 43  ω     73.00 109.00   1.00   18.00    --  112.00-111.00  60.00   36
 44  ω     77.00 126.00   1.00   18.00    --  112.00 -15.00 -60.00   49
 45  ω     70.00 131.00   1.00   18.00    --  112.00 -30.00  60.00   61
 46  ω     43.00  98.00   1.00   18.00    --  112.00 -77.00  60.00   55
 47  ω    130.00 177.00   1.00   18.00    --  112.00  77.00 -90.00   47
 48  ω     66.00  91.00   1.00   18.00    --  112.00 178.00  60.00   25
 49  ω    118.00 144.00   1.00   18.00    --  112.00 178.00  60.00   26
 50  ω     73.00 120.00   1.00   18.00    --  112.00 -61.00  60.00   47
 51  ω    148.00 174.00   1.00   18.00    --  112.00  77.00  30.00   26
 52  ω     74.00 106.00   1.00   18.00    --  112.00-111.00   0.00   32
 53  ω     37.00  88.00   1.00   18.00    --  112.00 -26.00-134.70   51
 54  ω    106.00 133.00   1.00   18.00    --  112.00 111.00-150.00   27
 55  ω    120.00 145.00   1.00   18.00    --  112.00 111.00 -30.00   25
 56  ω     61.00  87.00   1.00   18.00    --  112.00 -95.00-180.00   26
 57  ω     55.00  80.00   1.00   18.00    --  112.00 -95.00  60.00   25
 58  ω    120.00 145.00   1.00   18.00    --  112.00 178.00 -30.00   25
 59  ω     32.00  57.00   1.00   18.00    --  112.00 -87.00  83.69   25
 60  ω     79.00 107.00   1.00   18.00    --  112.00 -83.00  -2.69   28
;
_diffrn_measurement_device       'four-circle diffractometer'
_diffrn_measurement_device_type  'SuperNova, Dual, Cu at home/near, AtlasS2'
_diffrn_measurement_method       'ω scans'
_diffrn_orient_matrix_type       
'CrysAlisPro convention (1999,Acta A55,543-557)'
_diffrn_orient_matrix_UB_11      -0.0526730000
_diffrn_orient_matrix_UB_12      0.0040453000
_diffrn_orient_matrix_UB_13      -0.0572582000
_diffrn_orient_matrix_UB_21      0.0026495000
_diffrn_orient_matrix_UB_22      -0.0808867000
_diffrn_orient_matrix_UB_23      -0.0146325000
_diffrn_orient_matrix_UB_31      -0.0365785000
_diffrn_orient_matrix_UB_32      -0.0117003000
_diffrn_orient_matrix_UB_33      0.0814438000
_diffrn_radiation_monochromator  mirror
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           'Cu K\a'
_diffrn_radiation_wavelength     1.54184
_diffrn_source                   'micro-focus sealed X-ray tube'
_diffrn_source_type              'SuperNova (Cu) X-ray Source'
_reflns_Friedel_coverage         0.000
_reflns_Friedel_fraction_full    .
_reflns_Friedel_fraction_max     .
_reflns_number_gt                6188
_reflns_number_total             7262
_reflns_odcompleteness_completeness 98.74
_reflns_odcompleteness_iscentric 1
_reflns_odcompleteness_theta     77.17
_reflns_special_details          
;
 Reflections were merged by SHELXL according to the crystal
 class for the calculation of statistics and refinement.
 
 Structure factors included contributions from the .fab file.
 
 _reflns_Friedel_fraction is defined as the number of unique
 Friedel pairs measured divided by the number that would be
 possible theoretically, ignoring centric projections and
 systematic absences.
;
_reflns_threshold_expression     'I > 2σ(I)'
_computing_cell_refinement       'CrysAlisPro 1.171.40.67a (Rigaku OD, 2019)'
_computing_data_collection       'CrysAlisPro 1.171.40.67a (Rigaku OD, 2019)'
_computing_data_reduction        'CrysAlisPro 1.171.40.67a (Rigaku OD, 2019)'
_computing_molecular_graphics    'Olex2 1.3 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 1.3 (Dolomanov et al., 2009)'
_computing_structure_refinement  'SHELXL 2014/7 (Sheldrick, 2015)'
_computing_structure_solution    'ShelXT (Sheldrick, 2015)'
_refine_diff_density_max         0.518
_refine_diff_density_min         -0.502
_refine_diff_density_rms         0.051
_refine_ls_extinction_coef       .
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.056
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     442
_refine_ls_number_reflns         7262
_refine_ls_number_restraints     0
_refine_ls_R_factor_all          0.0537
_refine_ls_R_factor_gt           0.0467
_refine_ls_restrained_S_all      1.056
_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)+(0.0784P)²+1.0696P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1256
_refine_ls_wR_factor_ref         0.1332
_refine_special_details          ?
_olex2_refinement_description    
;
1. 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
2. Others
 Sof(F7A)=Sof(F6A)=1-FVAR(1)
 Sof(F6)=Sof(F7)=FVAR(1)
3.a Secondary CH2 refined with riding coordinates:
 C32(H32A,H32B), C26(H26A,H26B), C20(H20A,H20B)
3.b Aromatic/amide H refined with riding coordinates:
 C21(H21), C15(H15), C5(H5), C4(H4), C30(H30), C27(H27), C16(H16), C18(H18),
 C29(H29), C24(H24), C28(H28), C22(H22), C17(H17), C23(H23)
3.c Idealised Me refined as rotating group:
 C14(H14A,H14B,H14C), C13(H13A,H13B,H13C), C12(H12A,H12B,H12C), C9(H9A,H9B,
 H9C), C8(H8A,H8B,H8C), C10(H10A,H10B,H10C)
;
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     dual
_atom_sites_solution_secondary   ?
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
Fe Fe 0.68297(2) 0.23311(2) 0.44244(2) 0.04127(11) Uani 1 1 d . . . . .
P1 P 0.5000 0.08617(4) 0.2500 0.0552(2) Uani 1 2 d S T P . .
P2 P 0.5000 0.46263(5) 0.2500 0.0646(2) Uani 1 2 d S T P . .
O2 O 0.74700(6) 0.17879(7) 0.47262(10) 0.0470(3) Uani 1 1 d . . . . .
O1 O 0.73576(6) 0.30370(7) 0.40775(10) 0.0487(3) Uani 1 1 d . . . . .
F4 F 0.5000 0.17123(12) 0.2500 0.0848(8) Uani 1 2 d S T P . .
F2 F 0.55696(8) 0.08824(10) 0.30239(14) 0.0860(5) Uani 1 1 d . . . . .
N3 N 0.65932(8) 0.29326(10) 0.55696(11) 0.0483(4) Uani 1 1 d . . . . .
N1 N 0.62328(7) 0.15844(9) 0.48895(11) 0.0451(3) Uani 1 1 d . . . . .
F3 F 0.5000 0.00201(13) 0.2500 0.0883(7) Uani 1 2 d S T P . .
N4 N 0.67112(8) 0.19743(10) 0.31027(12) 0.0500(4) Uani 1 1 d . . . . .
F1 F 0.46674(10) 0.08686(13) 0.33913(13) 0.1003(6) Uani 1 1 d . . . . .
N2 N 0.60598(8) 0.28703(9) 0.40127(11) 0.0471(4) Uani 1 1 d . . . . .
C1 C 0.78841(8) 0.28074(10) 0.41445(12) 0.0406(4) Uani 1 1 d . . . . .
C2 C 0.79496(8) 0.21120(10) 0.45026(11) 0.0407(4) Uani 1 1 d . . . . .
C6 C 0.83432(9) 0.32156(11) 0.38901(13) 0.0468(4) Uani 1 1 d . . . . .
C3 C 0.84757(9) 0.18014(11) 0.46014(13) 0.0456(4) Uani 1 1 d . . . . .
C31 C 0.63669(10) 0.23676(12) 0.26143(14) 0.0526(5) Uani 1 1 d . . . . .
C11 C 0.85468(10) 0.10445(13) 0.49536(16) 0.0582(5) Uani 1 1 d . . . . .
C7 C 0.82700(11) 0.39708(13) 0.35292(17) 0.0605(6) Uani 1 1 d . . . . .
C19 C 0.57011(9) 0.17724(12) 0.47788(13) 0.0485(4) Uani 1 1 d . . . . .
C21 C 0.67792(11) 0.28096(14) 0.63851(16) 0.0583(5) Uani 1 1 d . . . . .
H21 H 0.7062 0.2479 0.6470 0.070 Uiso 1 1 calc R U . . .
C15 C 0.63558(11) 0.10007(12) 0.53593(15) 0.0553(5) Uani 1 1 d . . . . .
H15 H 0.6727 0.0873 0.5432 0.066 Uiso 1 1 calc R U . . .
C25 C 0.61914(10) 0.34127(12) 0.54462(15) 0.0537(5) Uani 1 1 d . . . . .
C5 C 0.88616(9) 0.28974(14) 0.39980(16) 0.0570(5) Uani 1 1 d . . . . .
H5 H 0.9178 0.3150 0.3837 0.068 Uiso 1 1 calc R U . . .
C4 C 0.89247(10) 0.22180(14) 0.43359(15) 0.0564(5) Uani 1 1 d . . . . .
H4 H 0.9282 0.2033 0.4387 0.068 Uiso 1 1 calc R U . . .
C30 C 0.62778(13) 0.22191(16) 0.17419(16) 0.0670(6) Uani 1 1 d . . . . .
H30 H 0.6031 0.2493 0.1415 0.080 Uiso 1 1 calc R U . . .
C32 C 0.61130(12) 0.30011(14) 0.30603(14) 0.0613(6) Uani 1 1 d . . . . .
H32A H 0.6345 0.3415 0.2962 0.074 Uiso 1 1 calc R U . . .
H32B H 0.5748 0.3096 0.2814 0.074 Uiso 1 1 calc R U . . .
C27 C 0.69744(12) 0.14194(14) 0.27329(17) 0.0630(6) Uani 1 1 d . . . . .
H27 H 0.7206 0.1138 0.3076 0.076 Uiso 1 1 calc R U . . .
C26 C 0.60344(12) 0.35418(13) 0.45077(15) 0.0598(6) Uani 1 1 d . . . . .
H26A H 0.5660 0.3735 0.4478 0.072 Uiso 1 1 calc R U . . .
H26B H 0.6288 0.3885 0.4251 0.072 Uiso 1 1 calc R U . . .
C16 C 0.59491(14) 0.05881(16) 0.57343(19) 0.0721(7) Uani 1 1 d . . . . .
H16 H 0.6043 0.0188 0.6059 0.087 Uiso 1 1 calc R U . . .
C20 C 0.55766(10) 0.24020(14) 0.42023(18) 0.0592(5) Uani 1 1 d . . . . .
H20A H 0.5428 0.2229 0.3653 0.071 Uiso 1 1 calc R U . . .
H20B H 0.5288 0.2684 0.4479 0.071 Uiso 1 1 calc R U . . .
C18 C 0.52727(11) 0.13773(18) 0.51403(18) 0.0715(7) Uani 1 1 d . . . . .
H18 H 0.4904 0.1513 0.5061 0.086 Uiso 1 1 calc R U . . .
C29 C 0.65580(15) 0.16615(18) 0.13630(17) 0.0782(8) Uani 1 1 d . . . . .
H29 H 0.6509 0.1560 0.0773 0.094 Uiso 1 1 calc R U . . .
C24 C 0.59560(14) 0.37802(17) 0.61287(19) 0.0766(8) Uani 1 1 d . . . . .
H24 H 0.5676 0.4112 0.6029 0.092 Uiso 1 1 calc R U . . .
C28 C 0.69110(14) 0.12563(18) 0.18644(19) 0.0763(8) Uani 1 1 d . . . . .
H28 H 0.7104 0.0877 0.1619 0.092 Uiso 1 1 calc R U . . .
C22 C 0.65620(14) 0.31616(17) 0.70973(17) 0.0754(7) Uani 1 1 d . . . . .
H22 H 0.6697 0.3071 0.7656 0.090 Uiso 1 1 calc R U . . .
C17 C 0.54017(14) 0.0778(2) 0.5620(2) 0.0823(9) Uani 1 1 d . . . . .
H17 H 0.5119 0.0505 0.5864 0.099 Uiso 1 1 calc R U . . .
C14 C 0.91608(14) 0.0833(2) 0.5007(3) 0.0964(11) Uani 1 1 d . . . . .
H14A H 0.9326 0.0862 0.4437 0.145 Uiso 1 1 calc R U . . .
H14B H 0.9190 0.0355 0.5222 0.145 Uiso 1 1 calc R U . . .
H14C H 0.9352 0.1149 0.5397 0.145 Uiso 1 1 calc R U . . .
C13 C 0.82582(16) 0.05250(16) 0.4337(2) 0.0832(9) Uani 1 1 d . . . . .
H13A H 0.7872 0.0649 0.4286 0.125 Uiso 1 1 calc R U . . .
H13B H 0.8291 0.0052 0.4564 0.125 Uiso 1 1 calc R U . . .
H13C H 0.8431 0.0548 0.3771 0.125 Uiso 1 1 calc R U . . .
C23 C 0.61447(16) 0.3646(2) 0.69703(19) 0.0875(10) Uani 1 1 d . . . . .
H23 H 0.5989 0.3883 0.7444 0.105 Uiso 1 1 calc R U . . .
C12 C 0.82882(15) 0.09815(18) 0.5867(2) 0.0812(8) Uani 1 1 d . . . . .
H12A H 0.8487 0.1282 0.6267 0.122 Uiso 1 1 calc R U . . .
H12B H 0.8311 0.0498 0.6062 0.122 Uiso 1 1 calc R U . . .
H12C H 0.7905 0.1126 0.5845 0.122 Uiso 1 1 calc R U . . .
C9 C 0.79962(18) 0.44256(15) 0.4235(3) 0.0865(9) Uani 1 1 d . . . . .
H9A H 0.7642 0.4225 0.4388 0.130 Uiso 1 1 calc R U . . .
H9B H 0.7944 0.4899 0.4018 0.130 Uiso 1 1 calc R U . . .
H9C H 0.8231 0.4438 0.4742 0.130 Uiso 1 1 calc R U . . .
C8 C 0.79095(17) 0.39597(18) 0.2709(2) 0.0876(10) Uani 1 1 d . . . . .
H8A H 0.8092 0.3687 0.2263 0.131 Uiso 1 1 calc R U . . .
H8B H 0.7854 0.4437 0.2505 0.131 Uiso 1 1 calc R U . . .
H8C H 0.7555 0.3748 0.2841 0.131 Uiso 1 1 calc R U . . .
C10 C 0.88260(16) 0.4311(2) 0.3295(3) 0.1096(14) Uani 1 1 d . . . . .
H10A H 0.9053 0.4347 0.3810 0.164 Uiso 1 1 calc R U . . .
H10B H 0.8763 0.4776 0.3059 0.164 Uiso 1 1 calc R U . . .
H10C H 0.9013 0.4023 0.2868 0.164 Uiso 1 1 calc R U . . .
F5 F 0.56564(8) 0.46221(13) 0.24649(19) 0.1115(8) Uani 1 1 d . . . . .
F6 F 0.4946(3) 0.3871(3) 0.3031(6) 0.096(2) Uani 0.445(14) 1 d . . P A 1
F7 F 0.4990(3) 0.4966(6) 0.3503(5) 0.108(3) Uani 0.445(14) 1 d . . P A 1
F7A F 0.5022(3) 0.5369(5) 0.2900(9) 0.157(6) Uani 0.555(14) 1 d . . P A 2
F6A F 0.5062(4) 0.4207(9) 0.3302(5) 0.170(5) Uani 0.555(14) 1 d . . P A 2


_geom_special_details            
;
 All esds (except the esd in the dihedral angle between two l.s. planes)
 are estimated using the full covariance matrix.  The cell esds are taken
 into account individually in the estimation of esds in distances, angles
 and torsion angles; correlations between esds in cell parameters are only
 used when they are defined by crystal symmetry.  An approximate (isotropic)
 treatment of cell esds is used for estimating esds involving l.s. planes.
;
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
Fe O2 1.9033(14) . ?
Fe O1 1.9117(14) . ?
Fe N3 2.1627(18) . ?
Fe N1 2.1299(16) . ?
Fe N4 2.1506(18) . ?
Fe N2 2.2007(17) . ?
P1 F4 1.602(2) . ?
P1 F2 1.5856(16) 3_655 ?
P1 F2 1.5856(16) . ?
P1 F3 1.585(2) . ?
P1 F1 1.5808(19) . ?
P1 F1 1.5807(19) 3_655 ?
P2 F5 1.5765(19) . ?
P2 F5 1.5766(19) 3_655 ?
P2 F6 1.643(6) 3_655 ?
P2 F6 1.643(6) . ?
P2 F7 1.664(5) 3_655 ?
P2 F7 1.664(5) . ?
P2 F7A 1.527(5) . ?
P2 F7A 1.527(5) 3_655 ?
P2 F6A 1.467(6) 3_655 ?
P2 F6A 1.467(6) . ?
O2 C2 1.347(2) . ?
O1 C1 1.340(2) . ?
N3 C21 1.346(3) . ?
N3 C25 1.335(3) . ?
N1 C19 1.335(3) . ?
N1 C15 1.346(3) . ?
N4 C31 1.338(3) . ?
N4 C27 1.346(3) . ?
N2 C32 1.484(3) . ?
N2 C26 1.475(3) . ?
N2 C20 1.486(3) . ?
C1 C2 1.428(3) . ?
C1 C6 1.399(3) . ?
C2 C3 1.400(3) . ?
C6 C7 1.536(3) . ?
C6 C5 1.391(3) . ?
C3 C11 1.533(3) . ?
C3 C4 1.394(3) . ?
C31 C30 1.381(3) . ?
C31 C32 1.504(3) . ?
C11 C14 1.529(4) . ?
C11 C13 1.526(4) . ?
C11 C12 1.534(4) . ?
C7 C9 1.527(4) . ?
C7 C8 1.525(4) . ?
C7 C10 1.523(4) . ?
C19 C20 1.508(3) . ?
C19 C18 1.385(3) . ?
C21 H21 0.9300 . ?
C21 C22 1.378(4) . ?
C15 H15 0.9300 . ?
C15 C16 1.373(4) . ?
C25 C26 1.505(3) . ?
C25 C24 1.375(4) . ?
C5 H5 0.9300 . ?
C5 C4 1.388(4) . ?
C4 H4 0.9300 . ?
C30 H30 0.9300 . ?
C30 C29 1.375(4) . ?
C32 H32A 0.9700 . ?
C32 H32B 0.9700 . ?
C27 H27 0.9300 . ?
C27 C28 1.373(4) . ?
C26 H26A 0.9700 . ?
C26 H26B 0.9700 . ?
C16 H16 0.9300 . ?
C16 C17 1.373(5) . ?
C20 H20A 0.9700 . ?
C20 H20B 0.9700 . ?
C18 H18 0.9300 . ?
C18 C17 1.381(5) . ?
C29 H29 0.9300 . ?
C29 C28 1.374(5) . ?
C24 H24 0.9300 . ?
C24 C23 1.389(4) . ?
C28 H28 0.9300 . ?
C22 H22 0.9300 . ?
C22 C23 1.368(5) . ?
C17 H17 0.9300 . ?
C14 H14A 0.9600 . ?
C14 H14B 0.9600 . ?
C14 H14C 0.9600 . ?
C13 H13A 0.9600 . ?
C13 H13B 0.9600 . ?
C13 H13C 0.9600 . ?
C23 H23 0.9300 . ?
C12 H12A 0.9600 . ?
C12 H12B 0.9600 . ?
C12 H12C 0.9600 . ?
C9 H9A 0.9600 . ?
C9 H9B 0.9600 . ?
C9 H9C 0.9600 . ?
C8 H8A 0.9600 . ?
C8 H8B 0.9600 . ?
C8 H8C 0.9600 . ?
C10 H10A 0.9600 . ?
C10 H10B 0.9600 . ?
C10 H10C 0.9600 . ?
F6 F6 1.64(2) 3_655 ?
F7A F7A 1.23(3) 3_655 ?

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 Fe O1 84.58(6) . . ?
O2 Fe N3 107.26(7) . . ?
O2 Fe N1 96.17(6) . . ?
O2 Fe N4 99.63(7) . . ?
O2 Fe N2 174.65(7) . . ?
O1 Fe N3 92.01(7) . . ?
O1 Fe N1 176.15(7) . . ?
O1 Fe N4 92.49(7) . . ?
O1 Fe N2 99.00(6) . . ?
N3 Fe N2 76.71(7) . . ?
N1 Fe N3 84.16(7) . . ?
N1 Fe N4 91.11(7) . . ?
N1 Fe N2 80.52(7) . . ?
N4 Fe N3 153.04(7) . . ?
N4 Fe N2 76.33(7) . . ?
F2 P1 F4 88.59(7) . . ?
F2 P1 F4 88.59(7) 3_655 . ?
F2 P1 F2 177.18(15) . 3_655 ?
F3 P1 F4 180.0 . . ?
F3 P1 F2 91.41(7) . . ?
F3 P1 F2 91.41(7) . 3_655 ?
F1 P1 F4 89.53(9) 3_655 . ?
F1 P1 F4 89.53(9) . . ?
F1 P1 F2 89.93(12) 3_655 3_655 ?
F1 P1 F2 89.93(12) . . ?
F1 P1 F2 90.05(12) . 3_655 ?
F1 P1 F2 90.05(12) 3_655 . ?
F1 P1 F3 90.47(9) . . ?
F1 P1 F3 90.47(9) 3_655 . ?
F1 P1 F1 179.07(19) 3_655 . ?
F5 P2 F5 179.42(19) . 3_655 ?
F5 P2 F6 95.2(3) . . ?
F5 P2 F6 95.2(3) 3_655 3_655 ?
F5 P2 F6 84.3(3) . 3_655 ?
F5 P2 F6 84.3(3) 3_655 . ?
F5 P2 F7 92.8(3) . . ?
F5 P2 F7 87.4(3) 3_655 . ?
F5 P2 F7 92.8(3) 3_655 3_655 ?
F5 P2 F7 87.4(3) . 3_655 ?
F6 P2 F6 60.1(6) . 3_655 ?
F6 P2 F7 142.2(6) 3_655 . ?
F6 P2 F7 142.2(6) . 3_655 ?
F6 P2 F7 82.8(4) . . ?
F6 P2 F7 82.8(4) 3_655 3_655 ?
F7 P2 F7 134.8(8) . 3_655 ?
F7A P2 F5 91.5(3) 3_655 . ?
F7A P2 F5 91.5(3) . 3_655 ?
F7A P2 F5 89.1(3) . . ?
F7A P2 F5 89.1(3) 3_655 3_655 ?
F7A P2 F7A 47.4(12) . 3_655 ?
F6A P2 F5 94.0(4) 3_655 . ?
F6A P2 F5 85.7(4) 3_655 3_655 ?
F6A P2 F5 85.7(4) . . ?
F6A P2 F5 94.0(4) . 3_655 ?
F6A P2 F7A 98.9(5) . . ?
F6A P2 F7A 98.9(5) 3_655 3_655 ?
F6A P2 F7A 146.3(12) 3_655 . ?
F6A P2 F7A 146.3(12) . 3_655 ?
F6A P2 F6A 114.9(13) . 3_655 ?
C2 O2 Fe 112.65(12) . . ?
C1 O1 Fe 112.32(12) . . ?
C21 N3 Fe 125.07(17) . . ?
C25 N3 Fe 115.43(14) . . ?
C25 N3 C21 119.2(2) . . ?
C19 N1 Fe 115.19(14) . . ?
C19 N1 C15 119.60(19) . . ?
C15 N1 Fe 124.74(15) . . ?
C31 N4 Fe 115.74(15) . . ?
C31 N4 C27 119.0(2) . . ?
C27 N4 Fe 125.18(17) . . ?
C32 N2 Fe 106.60(14) . . ?
C32 N2 C20 110.96(19) . . ?
C26 N2 Fe 106.44(13) . . ?
C26 N2 C32 111.46(18) . . ?
C26 N2 C20 112.1(2) . . ?
C20 N2 Fe 109.02(13) . . ?
O1 C1 C2 115.42(17) . . ?
O1 C1 C6 122.99(18) . . ?
C6 C1 C2 121.59(19) . . ?
O2 C2 C1 114.75(17) . . ?
O2 C2 C3 123.65(18) . . ?
C3 C2 C1 121.59(19) . . ?
C1 C6 C7 121.3(2) . . ?
C5 C6 C1 115.8(2) . . ?
C5 C6 C7 123.0(2) . . ?
C2 C3 C11 121.8(2) . . ?
C4 C3 C2 115.5(2) . . ?
C4 C3 C11 122.7(2) . . ?
N4 C31 C30 121.6(2) . . ?
N4 C31 C32 115.84(19) . . ?
C30 C31 C32 122.5(2) . . ?
C3 C11 C12 110.3(2) . . ?
C14 C11 C3 111.6(2) . . ?
C14 C11 C12 108.7(3) . . ?
C13 C11 C3 109.1(2) . . ?
C13 C11 C14 107.7(3) . . ?
C13 C11 C12 109.3(3) . . ?
C9 C7 C6 108.3(2) . . ?
C8 C7 C6 110.4(2) . . ?
C8 C7 C9 110.2(3) . . ?
C10 C7 C6 111.9(2) . . ?
C10 C7 C9 107.9(3) . . ?
C10 C7 C8 108.0(3) . . ?
N1 C19 C20 118.17(19) . . ?
N1 C19 C18 121.1(2) . . ?
C18 C19 C20 120.6(2) . . ?
N3 C21 H21 119.2 . . ?
N3 C21 C22 121.7(3) . . ?
C22 C21 H21 119.2 . . ?
N1 C15 H15 119.0 . . ?
N1 C15 C16 121.9(3) . . ?
C16 C15 H15 119.0 . . ?
N3 C25 C26 115.2(2) . . ?
N3 C25 C24 122.0(2) . . ?
C24 C25 C26 122.8(2) . . ?
C6 C5 H5 118.7 . . ?
C4 C5 C6 122.6(2) . . ?
C4 C5 H5 118.7 . . ?
C3 C4 H4 118.6 . . ?
C5 C4 C3 122.9(2) . . ?
C5 C4 H4 118.6 . . ?
C31 C30 H30 120.4 . . ?
C29 C30 C31 119.1(3) . . ?
C29 C30 H30 120.4 . . ?
N2 C32 C31 110.43(18) . . ?
N2 C32 H32A 109.6 . . ?
N2 C32 H32B 109.6 . . ?
C31 C32 H32A 109.6 . . ?
C31 C32 H32B 109.6 . . ?
H32A C32 H32B 108.1 . . ?
N4 C27 H27 119.0 . . ?
N4 C27 C28 121.9(3) . . ?
C28 C27 H27 119.0 . . ?
N2 C26 C25 109.97(18) . . ?
N2 C26 H26A 109.7 . . ?
N2 C26 H26B 109.7 . . ?
C25 C26 H26A 109.7 . . ?
C25 C26 H26B 109.7 . . ?
H26A C26 H26B 108.2 . . ?
C15 C16 H16 120.7 . . ?
C17 C16 C15 118.6(3) . . ?
C17 C16 H16 120.7 . . ?
N2 C20 C19 115.23(18) . . ?
N2 C20 H20A 108.5 . . ?
N2 C20 H20B 108.5 . . ?
C19 C20 H20A 108.5 . . ?
C19 C20 H20B 108.5 . . ?
H20A C20 H20B 107.5 . . ?
C19 C18 H18 120.5 . . ?
C17 C18 C19 119.0(3) . . ?
C17 C18 H18 120.5 . . ?
C30 C29 H29 120.3 . . ?
C28 C29 C30 119.3(2) . . ?
C28 C29 H29 120.3 . . ?
C25 C24 H24 120.7 . . ?
C25 C24 C23 118.6(3) . . ?
C23 C24 H24 120.7 . . ?
C27 C28 C29 119.0(3) . . ?
C27 C28 H28 120.5 . . ?
C29 C28 H28 120.5 . . ?
C21 C22 H22 120.5 . . ?
C23 C22 C21 119.0(3) . . ?
C23 C22 H22 120.5 . . ?
C16 C17 C18 119.7(3) . . ?
C16 C17 H17 120.2 . . ?
C18 C17 H17 120.2 . . ?
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 . . ?
C11 C13 H13A 109.5 . . ?
C11 C13 H13B 109.5 . . ?
C11 C13 H13C 109.5 . . ?
H13A C13 H13B 109.5 . . ?
H13A C13 H13C 109.5 . . ?
H13B C13 H13C 109.5 . . ?
C24 C23 H23 120.3 . . ?
C22 C23 C24 119.5(3) . . ?
C22 C23 H23 120.3 . . ?
C11 C12 H12A 109.5 . . ?
C11 C12 H12B 109.5 . . ?
C11 C12 H12C 109.5 . . ?
H12A C12 H12B 109.5 . . ?
H12A C12 H12C 109.5 . . ?
H12B C12 H12C 109.5 . . ?
C7 C9 H9A 109.5 . . ?
C7 C9 H9B 109.5 . . ?
C7 C9 H9C 109.5 . . ?
H9A C9 H9B 109.5 . . ?
H9A C9 H9C 109.5 . . ?
H9B C9 H9C 109.5 . . ?
C7 C8 H8A 109.5 . . ?
C7 C8 H8B 109.5 . . ?
C7 C8 H8C 109.5 . . ?
H8A C8 H8B 109.5 . . ?
H8A C8 H8C 109.5 . . ?
H8B C8 H8C 109.5 . . ?
C7 C10 H10A 109.5 . . ?
C7 C10 H10B 109.5 . . ?
C7 C10 H10C 109.5 . . ?
H10A C10 H10B 109.5 . . ?
H10A C10 H10C 109.5 . . ?
H10B C10 H10C 109.5 . . ?
P2 F6 F6 60.0(3) . 3_655 ?
F7A F7A P2 66.3(6) 3_655 . ?

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
Fe O2 C2 C1 4.0(2) . . . . ?
Fe O2 C2 C3 -175.58(15) . . . . ?
Fe O1 C1 C2 -3.5(2) . . . . ?
Fe O1 C1 C6 176.93(15) . . . . ?
Fe N3 C21 C22 -172.4(2) . . . . ?
Fe N3 C25 C26 -9.6(3) . . . . ?
Fe N3 C25 C24 172.9(2) . . . . ?
Fe N1 C19 C20 11.3(2) . . . . ?
Fe N1 C19 C18 -172.42(19) . . . . ?
Fe N1 C15 C16 171.6(2) . . . . ?
Fe N4 C31 C30 176.5(2) . . . . ?
Fe N4 C31 C32 0.0(3) . . . . ?
Fe N4 C27 C28 -174.7(2) . . . . ?
Fe N2 C32 C31 41.2(2) . . . . ?
Fe N2 C26 C25 -43.4(2) . . . . ?
Fe N2 C20 C19 12.3(2) . . . . ?
O2 C2 C3 C11 1.9(3) . . . . ?
O2 C2 C3 C4 -179.85(19) . . . . ?
O1 C1 C2 O2 -0.3(2) . . . . ?
O1 C1 C2 C3 179.28(17) . . . . ?
O1 C1 C6 C7 1.2(3) . . . . ?
O1 C1 C6 C5 -179.65(19) . . . . ?
N3 C21 C22 C23 0.3(5) . . . . ?
N3 C25 C26 N2 36.6(3) . . . . ?
N3 C25 C24 C23 0.1(5) . . . . ?
N1 C19 C20 N2 -16.3(3) . . . . ?
N1 C19 C18 C17 -0.2(4) . . . . ?
N1 C15 C16 C17 0.3(4) . . . . ?
N4 C31 C30 C29 -1.2(4) . . . . ?
N4 C31 C32 N2 -28.7(3) . . . . ?
N4 C27 C28 C29 -1.6(5) . . . . ?
C1 C2 C3 C11 -177.68(19) . . . . ?
C1 C2 C3 C4 0.6(3) . . . . ?
C1 C6 C7 C9 61.2(3) . . . . ?
C1 C6 C7 C8 -59.6(3) . . . . ?
C1 C6 C7 C10 -179.9(3) . . . . ?
C1 C6 C5 C4 0.0(3) . . . . ?
C2 C1 C6 C7 -178.30(19) . . . . ?
C2 C1 C6 C5 0.8(3) . . . . ?
C2 C3 C11 C14 -179.4(2) . . . . ?
C2 C3 C11 C13 61.7(3) . . . . ?
C2 C3 C11 C12 -58.5(3) . . . . ?
C2 C3 C4 C5 0.2(3) . . . . ?
C6 C1 C2 O2 179.24(17) . . . . ?
C6 C1 C2 C3 -1.1(3) . . . . ?
C6 C5 C4 C3 -0.6(4) . . . . ?
C31 N4 C27 C28 1.7(4) . . . . ?
C31 C30 C29 C28 1.3(5) . . . . ?
C11 C3 C4 C5 178.5(2) . . . . ?
C7 C6 C5 C4 179.1(2) . . . . ?
C19 N1 C15 C16 -0.1(3) . . . . ?
C19 C18 C17 C16 0.4(5) . . . . ?
C21 N3 C25 C26 176.7(2) . . . . ?
C21 N3 C25 C24 -0.8(4) . . . . ?
C21 C22 C23 C24 -1.1(6) . . . . ?
C15 N1 C19 C20 -176.2(2) . . . . ?
C15 N1 C19 C18 0.1(3) . . . . ?
C15 C16 C17 C18 -0.4(5) . . . . ?
C25 N3 C21 C22 0.6(4) . . . . ?
C25 C24 C23 C22 0.9(6) . . . . ?
C5 C6 C7 C9 -117.8(3) . . . . ?
C5 C6 C7 C8 121.4(3) . . . . ?
C5 C6 C7 C10 1.1(4) . . . . ?
C4 C3 C11 C14 2.4(3) . . . . ?
C4 C3 C11 C13 -116.5(3) . . . . ?
C4 C3 C11 C12 123.4(3) . . . . ?
C30 C31 C32 N2 154.8(2) . . . . ?
C30 C29 C28 C27 0.0(5) . . . . ?
C32 N2 C26 C25 -159.3(2) . . . . ?
C32 N2 C20 C19 129.4(2) . . . . ?
C32 C31 C30 C29 175.0(3) . . . . ?
C27 N4 C31 C30 -0.3(4) . . . . ?
C27 N4 C31 C32 -176.8(2) . . . . ?
C26 N2 C32 C31 156.9(2) . . . . ?
C26 N2 C20 C19 -105.3(2) . . . . ?
C26 C25 C24 C23 -177.3(3) . . . . ?
C20 N2 C32 C31 -77.4(3) . . . . ?
C20 N2 C26 C25 75.7(3) . . . . ?
C20 C19 C18 C17 176.0(3) . . . . ?
C18 C19 C20 N2 167.4(2) . . . . ?
C24 C25 C26 N2 -145.8(3) . . . . ?
F5 P2 F6 F6 -80.3(4) . . . 3_655 ?
F5 P2 F6 F6 99.4(4) 3_655 . . 3_655 ?
F5 P2 F7A F7A 92.8(6) . . . 3_655 ?
F5 P2 F7A F7A -87.4(6) 3_655 . . 3_655 ?
F7 P2 F6 F6 -172.4(5) . . . 3_655 ?
F7 P2 F6 F6 12.3(8) 3_655 . . 3_655 ?
F6A P2 F7A F7A 178.3(6) . . . 3_655 ?
F6A P2 F7A F7A -3.0(10) 3_655 . . 3_655 ?

_smtbx_masks_special_details     ?
loop_
_smtbx_masks_void_nr
_smtbx_masks_void_average_x
_smtbx_masks_void_average_y
_smtbx_masks_void_average_z
_smtbx_masks_void_volume
_smtbx_masks_void_count_electrons
_smtbx_masks_void_content
1 0.000 0.268 0.250 79.6 5.9 ?
2 0.000 0.732 0.750 79.6 5.9 ?
3 0.197 0.003 0.254 19.8 0.0 ?
4 0.197 -0.003 0.754 19.8 0.0 ?
5 0.303 0.497 0.754 19.8 0.0 ?
6 0.303 0.503 0.254 19.8 0.0 ?
7 0.500 0.232 0.750 79.6 5.9 ?
8 0.500 0.768 0.250 79.6 5.9 ?
9 0.697 0.503 0.246 19.8 0.0 ?
10 0.697 0.497 0.746 19.8 0.0 ?
11 0.803 0.003 0.246 19.8 0.0 ?
12 0.803 0.997 0.746 19.8 0.0 ?

_smtbx_masks_void_probe_radius   1.2
_smtbx_masks_void_truncation_radius 1.2
_olex2_submission_special_instructions 'No special instructions were received'
_oxdiff_exptl_absorpt_empirical_details 
;
Empirical correction (ABSPACK) includes:
;
_oxdiff_exptl_absorpt_empirical_full_max 1.577
_oxdiff_exptl_absorpt_empirical_full_min 0.535
_symmetry_cell_setting           orthorhombic
_symmetry_space_group_name_h-m   'P b c n'
_symmetry_int_tables_number      60
_chemical_absolute_configuration .

