# Electronic Supplementary Material (ESI) for Dalton Transactions.
# This journal is © The Royal Society of Chemistry 2020

####################################################################### 
# 
# 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. 
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data_Tp_100K
_database_code_depnum_ccdc_archive 'CCDC 1974447'
loop_
_audit_author_name
_audit_author_address
'Xin-Hua Zhao'
;Southern University of Science and Technology
China
;
_audit_update_record             
;
2020-03-27 deposited with the CCDC.	2020-04-01 downloaded from the CCDC.
;
_audit_creation_date             2020-03-13
_audit_creation_method           
;
Olex2 1.2
(compiled 2018.05.29 svn.r3508 for OlexSys, GUI svn.r5506)
;
_shelx_SHELXL_version_number     2014/7
_chemical_name_common            ?
_chemical_name_systematic        Fe2FebnbpenTp100k
_chemical_formula_moiety         
'C60 H54 B2 Fe3 N22, 4(C H4 O), 0.5(H4 O2), 3[CH3OH]'
_chemical_formula_sum            'C67 H84 B2 Fe3 N22 O8'
_chemical_formula_weight         1514.73
_chemical_melting_point          ?
loop_
_atom_type_symbol
_atom_type_description
_atom_type_scat_dispersion_real
_atom_type_scat_dispersion_imag
_atom_type_scat_source
C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
B B 0.0013 0.0007 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Fe Fe 0.3463 0.8444 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'

_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      monoclinic
_space_group_IT_number           15
_space_group_name_H-M_alt        'C 1 2/c 1'
_space_group_name_Hall           '-C 2yc'
loop_
_space_group_symop_operation_xyz
'x, y, z'
'-x, y, -z+1/2'
'x+1/2, y+1/2, z'
'-x+1/2, y+1/2, -z+1/2'
'-x, -y, -z'
'x, -y, z-1/2'
'-x+1/2, -y+1/2, -z'
'x+1/2, -y+1/2, z-1/2'

_cell_length_a                   19.3698(6)
_cell_length_b                   18.5637(5)
_cell_length_c                   23.0499(7)
_cell_angle_alpha                90
_cell_angle_beta                 114.0340(10)
_cell_angle_gamma                90
_cell_volume                     7569.6(4)
_cell_formula_units_Z            4
_cell_measurement_reflns_used    9339
_cell_measurement_temperature    100(2)
_cell_measurement_theta_max      27.924
_cell_measurement_theta_min      2.844
_shelx_estimated_absorpt_T_max   0.994
_shelx_estimated_absorpt_T_min   0.987
_exptl_absorpt_coefficient_mu    0.634
_exptl_absorpt_correction_T_max  0.7456
_exptl_absorpt_correction_T_min  0.6575
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   
'SADABS-2016/2 (Bruker,2016/2) was used for absorption correction. wR2(int) was 0.0898 before and 0.0486 after correction. The Ratio of minimum to maximum transmission is 0.8818. The λ/2 correction factor is Not present.'
_exptl_absorpt_special_details   ?
_exptl_crystal_colour            'metallic dark red'
_exptl_crystal_colour_lustre     metallic
_exptl_crystal_colour_modifier   dark
_exptl_crystal_colour_primary    red
_exptl_crystal_density_diffrn    1.329
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    ?
_exptl_crystal_description       block
_exptl_crystal_F_000             3168
_exptl_crystal_size_max          0.02
_exptl_crystal_size_mid          0.012
_exptl_crystal_size_min          0.01
_exptl_transmission_factor_max   ?
_exptl_transmission_factor_min   ?
_diffrn_reflns_av_R_equivalents  0.0379
_diffrn_reflns_av_unetI/netI     0.0273
_diffrn_reflns_Laue_measured_fraction_full 0.983
_diffrn_reflns_Laue_measured_fraction_max 0.984
_diffrn_reflns_limit_h_max       25
_diffrn_reflns_limit_h_min       -25
_diffrn_reflns_limit_k_max       24
_diffrn_reflns_limit_k_min       -21
_diffrn_reflns_limit_l_max       30
_diffrn_reflns_limit_l_min       -30
_diffrn_reflns_number            48628
_diffrn_reflns_point_group_measured_fraction_full 0.983
_diffrn_reflns_point_group_measured_fraction_max 0.984
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         27.940
_diffrn_reflns_theta_min         2.398
_diffrn_ambient_temperature      99.99
_diffrn_detector_area_resol_mean ?
_diffrn_measured_fraction_theta_full 0.983
_diffrn_measured_fraction_theta_max 0.984
_diffrn_measurement_device_type  'Bruker APEX-II CCD'
_diffrn_measurement_method       'φ and ω scans'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_source                   ?
_diffrn_standards_number         0
_reflns_Friedel_coverage         0.000
_reflns_Friedel_fraction_full    .
_reflns_Friedel_fraction_max     .
_reflns_number_gt                7981
_reflns_number_total             8955
_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       'SAINT V8.38A (?, 2016)'
_computing_data_collection       'Bruker APEX3'
_computing_data_reduction        'SAINT V8.38A (?, 2016)'
_computing_molecular_graphics    'Olex2 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 (Dolomanov et al., 2009)'
_computing_structure_refinement  'XL (Sheldrick, 2008)'
_computing_structure_solution    'olex2.solve (Bourhis et al., 2015)'
_refine_diff_density_max         0.583
_refine_diff_density_min         -0.799
_refine_diff_density_rms         0.060
_refine_ls_extinction_coef       .
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.028
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     500
_refine_ls_number_reflns         8955
_refine_ls_number_restraints     92
_refine_ls_R_factor_all          0.0507
_refine_ls_R_factor_gt           0.0443
_refine_ls_restrained_S_all      1.039
_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)+(0.0409P)²+19.9420P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1083
_refine_ls_wR_factor_ref         0.1129
_refine_special_details          ?
_olex2_refinement_description    
;
1. Fixed Uiso
 At 1.2 times of:
  All B(H) groups, All C(H) groups, All C(H,H) groups
 At 1.5 times of:
  All C(H,H,H) groups, All O(H) groups, All O(H,H) groups
2. Restrained distances
 O1B-C31B = O1A-C31A
 1.45 with sigma of 0.02
 O4-C34 = O1C-C31C
 1.45 with sigma of 0.02
3. Rigid bond restraints
 C11, C12, C13, C14, C15, C16
 with sigma for 1-2 distances of 0.01 and sigma for 1-3 distances of 0.01
 C13, C14
 with sigma for 1-2 distances of 0.01 and sigma for 1-3 distances of 0.01
4. Uiso/Uaniso restraints and constraints
C11 \\sim C12 \\sim C13 \\sim C14 \\sim C15 \\sim C16: within 2A with sigma of
0.01 and sigma for terminal atoms of 0.02
C13 \\sim C14: within 2A with sigma of 0.005 and sigma for terminal atoms of
0.01
Uanis(C34) \\sim Ueq, Uanis(O4) \\sim Ueq, Uanis(O1C) \\sim Ueq, Uanis(C31C)
\\sim Ueq, Uanis(O1A) \\sim Ueq, Uanis(C31A) \\sim Ueq, Uanis(C31B) \\sim Ueq,
Uanis(O1B) \\sim Ueq: with sigma of 0.01 and sigma for terminal atoms of 0.02
Uanis(C31B) \\sim Ueq, Uanis(C31A) \\sim Ueq: with sigma of 0.005 and sigma for
terminal atoms of 0.01
Uanis(O1A) = Uanis(O1B)
Uanis(C31A) = Uanis(C31B)
Uanis(O4) = Uanis(O1C)
Uanis(C34) = Uanis(C31C)
5. Others
 1*[Sof(O1A)+Sof(H1AA)+Sof(C31A)+Sof(H31A)+Sof(H31B)+Sof(H31C)]+1*[Sof(O1B)+
 Sof(H1B)+Sof(C31B)+Sof(H31D)+Sof(H31E)+Sof(H31F)]+1*[Sof(O1C)+Sof(H1C)+
 Sof(C31C)+Sof(H31G)+Sof(H31H)+Sof(H31I)]=1 with esd of 0
 Sof(O1A)=Sof(H1AA)=Sof(C31A)=Sof(H31A)=Sof(H31B)=Sof(H31C)=FVAR(1)
 Sof(O1B)=Sof(H1B)=Sof(C31B)=Sof(H31D)=Sof(H31E)=Sof(H31F)=FVAR(2)
 Sof(O1C)=Sof(H1C)=Sof(C31C)=Sof(H31G)=Sof(H31H)=Sof(H31I)=FVAR(3)
 Fixed Sof: O4(0.5) H4A(0.5) H5A(0.5) H5B(0.5) C34(0.5) H34A(0.5) H34B(0.5)
 H34C(0.5)
6.a Free rotating group:
 O5(H5A,H5B)
6.b Ternary CH refined with riding coordinates:
 B1(H1A)
6.c Secondary CH2 refined with riding coordinates:
 C6(H6A,H6B), C7(H7A,H7B), C18(H18A,H18B)
6.d Aromatic/amide H refined with riding coordinates:
 C1(H1), C2(H2), C3(H3), C4(H4), C8(H8), C9(H9), C12(H12), C13(H13), C14(H14),
 C15(H15), C16(H16), C22(H22), C23(H23), C24(H24), C25(H25), C26(H26), C27(H27),
  C28(H28), C29(H29), C30(H30)
6.e Idealised Me refined as rotating group:
 C31A(H31A,H31B,H31C), C31B(H31D,H31E,H31F), C31C(H31G,H31H,H31I), C32(H32A,
 H32B,H32C), C33(H33A,H33B,H33C), C34(H34A,H34B,H34C)
6.f Idealised tetrahedral OH refined as rotating group:
 O1A(H1AA), O1B(H1B), O1C(H1C), O2(H2A), O3(H3A), O4(H4A)
;
_atom_sites_solution_hydrogens   mixed
_atom_sites_solution_primary     iterative
_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
Fe1 Fe 0.5000 0.41941(2) 0.2500 0.01358(9) Uani 1 2 d S T P . .
Fe2 Fe 0.68596(2) 0.60499(2) 0.37218(2) 0.02812(9) Uani 1 1 d . . . . .
O1A O 0.5943(2) -0.0260(2) 0.3371(3) 0.0756(14) Uani 0.551(3) 1 d D U . A 1
H1AA H 0.5814 0.0052 0.3572 0.113 Uiso 0.551(3) 1 calc GR . . A 1
O1B O 0.6751(7) -0.0294(7) 0.4209(8) 0.0756(14) Uani 0.191(3) 1 d D U . B 2
H1B H 0.6903 0.0084 0.4424 0.113 Uiso 0.191(3) 1 calc GR . . B 2
O1C O 0.5554(12) 0.0411(13) 0.4150(9) 0.079(2) Uani 0.258(3) 1 d D U . C 3
H1C H 0.5483 0.0686 0.3842 0.119 Uiso 0.258(3) 1 calc GR . . C 3
O2 O 0.16625(12) 0.40294(13) 0.19591(10) 0.0562(5) Uani 1 1 d . . . . .
H2A H 0.1769 0.4235 0.1682 0.084 Uiso 1 1 calc GR . . . .
O3 O 0.47373(14) 0.14053(15) 0.34541(16) 0.0805(8) Uani 1 1 d . . . . .
H3A H 0.4979 0.1078 0.3706 0.121 Uiso 1 1 calc GR . . . .
O4 O 0.5695(5) 0.0456(6) 0.4407(4) 0.079(2) Uani 0.5 1 d D U . D 1
H4A H 0.6163 0.0411 0.4617 0.119 Uiso 0.5 1 calc GR . . D 1
O5 O 0.5000 0.0704(3) 0.2500 0.0961(14) Uani 1 2 d S T P . .
H5A H 0.5467 0.0588 0.2733 0.144 Uiso 0.5 1 d G . . . .
H5B H 0.4858 0.0950 0.2754 0.144 Uiso 0.5 1 d G . . . .
N1 N 0.45662(8) 0.42178(8) 0.31425(7) 0.0157(3) Uani 1 1 d . . . . .
N2 N 0.42200(8) 0.34006(8) 0.21236(7) 0.0174(3) Uani 1 1 d . . . . .
N3 N 0.57265(10) 0.49132(9) 0.29428(8) 0.0234(3) Uani 1 1 d . . . . .
N4 N 0.80534(18) 0.48900(14) 0.39277(18) 0.0751(10) Uani 1 1 d . . . . .
N5 N 0.66024(14) 0.54096(11) 0.48505(10) 0.0416(5) Uani 1 1 d . . . . .
N6 N 0.69927(10) 0.71624(10) 0.28921(8) 0.0288(4) Uani 1 1 d . . . . .
N7 N 0.69929(11) 0.64386(11) 0.29747(8) 0.0321(4) Uani 1 1 d . . . . .
N8 N 0.75408(9) 0.74552(9) 0.40420(8) 0.0223(3) Uani 1 1 d . . . . .
N9 N 0.75916(9) 0.67631(9) 0.42478(7) 0.0234(3) Uani 1 1 d . . . . .
N10 N 0.61526(10) 0.74616(10) 0.34260(8) 0.0280(4) Uani 1 1 d . . . . .
N11 N 0.60370(10) 0.67633(10) 0.35454(8) 0.0299(4) Uani 1 1 d . . . . .
C1 C 0.48320(10) 0.45948(10) 0.36925(8) 0.0198(3) Uani 1 1 d . . . . .
H1 H 0.5334 0.4777 0.3851 0.024 Uiso 1 1 calc R . . . .
C2 C 0.43982(11) 0.47245(10) 0.40323(9) 0.0235(4) Uani 1 1 d . . . . .
H2 H 0.4597 0.4998 0.4413 0.028 Uiso 1 1 calc R . . . .
C3 C 0.36714(12) 0.44514(12) 0.38111(9) 0.0267(4) Uani 1 1 d . . . . .
H3 H 0.3363 0.4537 0.4035 0.032 Uiso 1 1 calc R . . . .
C4 C 0.34026(11) 0.40497(12) 0.32560(9) 0.0274(4) Uani 1 1 d . . . . .
H4 H 0.2909 0.3847 0.3099 0.033 Uiso 1 1 calc R . . . .
C5 C 0.38626(10) 0.39466(10) 0.29325(8) 0.0197(3) Uani 1 1 d . . . . .
C6 C 0.35766(10) 0.35865(11) 0.22942(8) 0.0224(4) Uani 1 1 d . . . . .
H6A H 0.3298 0.3143 0.2304 0.027 Uiso 1 1 calc R . . . .
H6B H 0.3223 0.3913 0.1969 0.027 Uiso 1 1 calc R . . . .
C7 C 0.39363(10) 0.33254(11) 0.14120(8) 0.0211(4) Uani 1 1 d . . . . .
H7A H 0.4357 0.3149 0.1311 0.025 Uiso 1 1 calc R . . . .
H7B H 0.3795 0.3809 0.1219 0.025 Uiso 1 1 calc R . . . .
C8 C 0.33679(13) 0.20949(12) 0.09871(9) 0.0298(4) Uani 1 1 d . . . . .
H8 H 0.3865 0.1906 0.1118 0.036 Uiso 1 1 calc R . . . .
C9 C 0.27556(14) 0.16521(12) 0.06875(10) 0.0344(5) Uani 1 1 d . . . . .
H9 H 0.2835 0.1164 0.0607 0.041 Uiso 1 1 calc R . . . .
C10 C 0.20122(13) 0.19130(12) 0.04977(9) 0.0309(5) Uani 1 1 d . . . . .
C11 C 0.19022(12) 0.26460(12) 0.06055(9) 0.0282(4) Uani 1 1 d . U . . .
C12 C 0.13575(16) 0.14657(15) 0.02005(10) 0.0438(6) Uani 1 1 d . U . . .
H12 H 0.1417 0.0973 0.0121 0.053 Uiso 1 1 calc R . . . .
C13 C 0.06541(16) 0.17430(18) 0.00330(12) 0.0506(7) Uani 1 1 d . U . . .
H13 H 0.0226 0.1439 -0.0157 0.061 Uiso 1 1 calc R . . . .
C14 C 0.05485(15) 0.24735(19) 0.01358(12) 0.0507(7) Uani 1 1 d . U . . .
H14 H 0.0052 0.2660 0.0011 0.061 Uiso 1 1 calc R . . . .
C15 C 0.11604(13) 0.29175(16) 0.04155(11) 0.0405(6) Uani 1 1 d . U . . .
H15 H 0.1086 0.3411 0.0482 0.049 Uiso 1 1 calc R . . . .
C16 C 0.25468(11) 0.30918(11) 0.09013(9) 0.0245(4) Uani 1 1 d . U . . .
H16 H 0.2477 0.3588 0.0962 0.029 Uiso 1 1 calc R . . . .
C17 C 0.32673(11) 0.28270(11) 0.11022(8) 0.0225(4) Uani 1 1 d . . . . .
C18 C 0.45929(11) 0.27259(10) 0.24609(8) 0.0212(4) Uani 1 1 d . . . . .
H18A H 0.4327 0.2300 0.2212 0.025 Uiso 1 1 calc R . . . .
H18B H 0.4572 0.2704 0.2883 0.025 Uiso 1 1 calc R . . . .
C19 C 0.61514(13) 0.53517(12) 0.32168(10) 0.0315(5) Uani 1 1 d . . . . .
C20 C 0.67097(13) 0.56556(12) 0.44351(10) 0.0314(5) Uani 1 1 d . . . . .
C21 C 0.76207(17) 0.53317(13) 0.38674(14) 0.0452(7) Uani 1 1 d . . . . .
C22 C 0.70324(11) 0.73066(15) 0.23320(10) 0.0337(5) Uani 1 1 d . . . . .
H22 H 0.7038 0.7772 0.2163 0.040 Uiso 1 1 calc R . . . .
C23 C 0.70631(13) 0.66604(16) 0.20493(10) 0.0415(6) Uani 1 1 d . . . . .
H23 H 0.7096 0.6592 0.1653 0.050 Uiso 1 1 calc R . . . .
C24 C 0.70352(14) 0.61286(15) 0.24651(10) 0.0391(6) Uani 1 1 d . . . . .
H24 H 0.7045 0.5624 0.2398 0.047 Uiso 1 1 calc R . . . .
C25 C 0.55336(12) 0.78558(16) 0.33288(10) 0.0379(5) Uani 1 1 d . . . . .
H25 H 0.5475 0.8357 0.3239 0.045 Uiso 1 1 calc R . . . .
C26 C 0.49957(13) 0.74016(17) 0.33820(11) 0.0445(7) Uani 1 1 d . . . . .
H26 H 0.4500 0.7526 0.3336 0.053 Uiso 1 1 calc R . . . .
C27 C 0.53311(12) 0.67304(15) 0.35164(10) 0.0379(6) Uani 1 1 d . . . . .
H27 H 0.5096 0.6306 0.3579 0.045 Uiso 1 1 calc R . . . .
C28 C 0.80832(11) 0.78510(11) 0.44854(9) 0.0248(4) Uani 1 1 d . . . . .
H28 H 0.8166 0.8352 0.4457 0.030 Uiso 1 1 calc R . . . .
C29 C 0.84978(11) 0.74112(12) 0.49855(9) 0.0264(4) Uani 1 1 d . . . . .
H29 H 0.8918 0.7542 0.5364 0.032 Uiso 1 1 calc R . . . .
C30 C 0.81708(11) 0.67346(11) 0.48194(9) 0.0261(4) Uani 1 1 d . . . . .
H30 H 0.8334 0.6314 0.5074 0.031 Uiso 1 1 calc R . . . .
C31A C 0.6681(6) -0.0073(8) 0.3381(5) 0.095(3) Uani 0.551(3) 1 d D U . A 1
H31A H 0.6808 -0.0410 0.3113 0.143 Uiso 0.551(3) 1 calc GR . . A 1
H31B H 0.7065 -0.0100 0.3818 0.143 Uiso 0.551(3) 1 calc GR . . A 1
H31C H 0.6663 0.0418 0.3219 0.143 Uiso 0.551(3) 1 calc GR . . A 1
C31B C 0.673(2) -0.019(3) 0.3610(13) 0.095(3) Uani 0.191(3) 1 d D U . B 2
H31D H 0.6199 -0.0130 0.3306 0.143 Uiso 0.191(3) 1 calc GR . . B 2
H31E H 0.6948 -0.0605 0.3488 0.143 Uiso 0.191(3) 1 calc GR . . B 2
H31F H 0.7012 0.0246 0.3608 0.143 Uiso 0.191(3) 1 calc GR . . B 2
C31C C 0.6155(12) -0.0036(13) 0.4241(11) 0.124(4) Uani 0.258(3) 1 d D U . C 3
H31G H 0.6096 -0.0247 0.3833 0.186 Uiso 0.258(3) 1 calc GR . . C 3
H31H H 0.6173 -0.0421 0.4537 0.186 Uiso 0.258(3) 1 calc GR . . C 3
H31I H 0.6626 0.0242 0.4417 0.186 Uiso 0.258(3) 1 calc GR . . C 3
C32 C 0.0940(2) 0.4176(3) 0.1856(3) 0.0946(16) Uani 1 1 d . . . . .
H32A H 0.0606 0.4036 0.1421 0.142 Uiso 1 1 calc GR . . . .
H32B H 0.0886 0.4693 0.1913 0.142 Uiso 1 1 calc GR . . . .
H32C H 0.0803 0.3904 0.2158 0.142 Uiso 1 1 calc GR . . . .
C33 C 0.40367(18) 0.1516(2) 0.3500(2) 0.0734(11) Uani 1 1 d . . . . .
H33A H 0.3652 0.1652 0.3082 0.110 Uiso 1 1 calc GR . . . .
H33B H 0.4091 0.1902 0.3805 0.110 Uiso 1 1 calc GR . . . .
H33C H 0.3883 0.1071 0.3643 0.110 Uiso 1 1 calc GR . . . .
C34 C 0.5316(6) 0.0092(7) 0.4708(5) 0.124(4) Uani 0.5 1 d D U . D 1
H34A H 0.5122 -0.0364 0.4487 0.186 Uiso 0.5 1 calc GR . . D 1
H34B H 0.4894 0.0386 0.4702 0.186 Uiso 0.5 1 calc GR . . D 1
H34C H 0.5662 -0.0007 0.5148 0.186 Uiso 0.5 1 calc GR . . D 1
B1 B 0.69093(12) 0.76588(13) 0.33950(10) 0.0263(5) Uani 1 1 d . . . . .
H1A H 0.6931 0.8179 0.3292 0.032 Uiso 1 1 calc R . . . .


_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
Fe1 N1 1.9784(14) 2_655 ?
Fe1 N1 1.9785(14) . ?
Fe1 N2 2.0340(15) . ?
Fe1 N2 2.0341(15) 2_655 ?
Fe1 N3 1.9063(16) . ?
Fe1 N3 1.9064(16) 2_655 ?
Fe2 N7 1.9785(17) . ?
Fe2 N9 1.9579(16) . ?
Fe2 N11 1.983(2) . ?
Fe2 C19 1.902(2) . ?
Fe2 C20 1.927(2) . ?
Fe2 C21 1.913(3) . ?
O1A C31A 1.462(12) . ?
O1B C31B 1.376(19) . ?
O1C C31C 1.374(18) . ?
O2 C32 1.348(4) . ?
O3 C33 1.418(4) . ?
O4 C34 1.375(13) . ?
N1 C1 1.353(2) . ?
N1 C5 1.345(2) . ?
N2 C6 1.492(2) . ?
N2 C7 1.509(2) . ?
N2 C18 1.496(2) . ?
N3 C19 1.147(3) . ?
N4 C21 1.140(4) . ?
N5 C20 1.153(3) . ?
N6 N7 1.357(3) . ?
N6 C22 1.351(3) . ?
N6 B1 1.540(3) . ?
N7 C24 1.340(3) . ?
N8 N9 1.359(2) . ?
N8 C28 1.347(2) . ?
N8 B1 1.542(3) . ?
N9 C30 1.339(3) . ?
N10 N11 1.363(3) . ?
N10 C25 1.343(3) . ?
N10 B1 1.540(3) . ?
N11 C27 1.343(3) . ?
C1 C2 1.383(3) . ?
C2 C3 1.384(3) . ?
C3 C4 1.386(3) . ?
C4 C5 1.389(3) . ?
C5 C6 1.501(2) . ?
C7 C17 1.514(3) . ?
C8 C9 1.376(3) . ?
C8 C17 1.413(3) . ?
C9 C10 1.409(3) . ?
C10 C11 1.415(3) . ?
C10 C12 1.435(3) . ?
C11 C15 1.413(3) . ?
C11 C16 1.420(3) . ?
C12 C13 1.357(4) . ?
C13 C14 1.406(5) . ?
C14 C15 1.370(3) . ?
C16 C17 1.370(3) . ?
C18 C18 1.513(4) 2_655 ?
C22 C23 1.378(4) . ?
C23 C24 1.392(4) . ?
C25 C26 1.384(3) . ?
C26 C27 1.381(4) . ?
C28 C29 1.373(3) . ?
C29 C30 1.389(3) . ?

loop_
_geom_angle_atom_site_label_1
_geom_angle_atom_site_label_2
_geom_angle_atom_site_label_3
_geom_angle
_geom_angle_site_symmetry_1
_geom_angle_site_symmetry_3
_geom_angle_publ_flag
N1 Fe1 N1 177.44(9) 2_655 . ?
N1 Fe1 N2 82.38(6) 2_655 2_655 ?
N1 Fe1 N2 99.49(6) . 2_655 ?
N1 Fe1 N2 99.50(6) 2_655 . ?
N1 Fe1 N2 82.38(6) . . ?
N2 Fe1 N2 87.20(9) . 2_655 ?
N3 Fe1 N1 91.70(6) . . ?
N3 Fe1 N1 86.51(6) . 2_655 ?
N3 Fe1 N1 86.52(6) 2_655 . ?
N3 Fe1 N1 91.69(6) 2_655 2_655 ?
N3 Fe1 N2 91.19(7) . 2_655 ?
N3 Fe1 N2 173.51(6) . . ?
N3 Fe1 N2 91.19(7) 2_655 . ?
N3 Fe1 N2 173.51(6) 2_655 2_655 ?
N3 Fe1 N3 91.09(11) . 2_655 ?
N7 Fe2 N11 87.52(8) . . ?
N9 Fe2 N7 88.51(7) . . ?
N9 Fe2 N11 89.66(7) . . ?
C19 Fe2 N7 91.90(8) . . ?
C19 Fe2 N9 179.52(9) . . ?
C19 Fe2 N11 90.61(9) . . ?
C19 Fe2 C20 86.65(8) . . ?
C19 Fe2 C21 86.83(11) . . ?
C20 Fe2 N7 178.55(8) . . ?
C20 Fe2 N9 92.94(8) . . ?
C20 Fe2 N11 92.34(9) . . ?
C21 Fe2 N7 92.44(10) . . ?
C21 Fe2 N9 92.90(9) . . ?
C21 Fe2 N11 177.43(9) . . ?
C21 Fe2 C20 87.63(11) . . ?
C1 N1 Fe1 126.68(12) . . ?
C5 N1 Fe1 113.54(11) . . ?
C5 N1 C1 118.30(15) . . ?
C6 N2 Fe1 105.97(11) . . ?
C6 N2 C7 109.53(13) . . ?
C6 N2 C18 109.57(14) . . ?
C7 N2 Fe1 114.15(11) . . ?
C18 N2 Fe1 105.49(10) . . ?
C18 N2 C7 111.87(14) . . ?
C19 N3 Fe1 178.19(17) . . ?
N7 N6 B1 118.74(16) . . ?
C22 N6 N7 109.48(19) . . ?
C22 N6 B1 131.7(2) . . ?
N6 N7 Fe2 119.38(13) . . ?
C24 N7 Fe2 133.03(17) . . ?
C24 N7 N6 107.38(18) . . ?
N9 N8 B1 119.04(15) . . ?
C28 N8 N9 109.12(16) . . ?
C28 N8 B1 131.82(17) . . ?
N8 N9 Fe2 119.46(12) . . ?
C30 N9 Fe2 133.45(14) . . ?
C30 N9 N8 107.06(16) . . ?
N11 N10 B1 118.24(18) . . ?
C25 N10 N11 110.06(18) . . ?
C25 N10 B1 131.6(2) . . ?
N10 N11 Fe2 119.50(13) . . ?
C27 N11 Fe2 134.18(17) . . ?
C27 N11 N10 106.3(2) . . ?
N1 C1 C2 122.24(17) . . ?
C1 C2 C3 119.29(17) . . ?
C2 C3 C4 118.71(17) . . ?
C3 C4 C5 119.21(18) . . ?
N1 C5 C4 122.21(17) . . ?
N1 C5 C6 115.77(15) . . ?
C4 C5 C6 121.76(17) . . ?
N2 C6 C5 110.29(14) . . ?
N2 C7 C17 115.61(15) . . ?
C9 C8 C17 120.8(2) . . ?
C8 C9 C10 120.9(2) . . ?
C9 C10 C11 118.94(19) . . ?
C9 C10 C12 122.8(2) . . ?
C11 C10 C12 118.3(2) . . ?
C10 C11 C16 118.6(2) . . ?
C15 C11 C10 119.7(2) . . ?
C15 C11 C16 121.7(2) . . ?
C13 C12 C10 120.4(3) . . ?
C12 C13 C14 121.1(2) . . ?
C15 C14 C13 120.1(3) . . ?
C14 C15 C11 120.4(3) . . ?
C17 C16 C11 121.9(2) . . ?
C8 C17 C7 121.29(18) . . ?
C16 C17 C7 119.90(18) . . ?
C16 C17 C8 118.75(18) . . ?
N2 C18 C18 108.73(11) . 2_655 ?
N3 C19 Fe2 176.21(18) . . ?
N5 C20 Fe2 178.1(2) . . ?
N4 C21 Fe2 176.8(3) . . ?
N6 C22 C23 108.0(2) . . ?
C22 C23 C24 105.70(19) . . ?
N7 C24 C23 109.4(2) . . ?
N10 C25 C26 107.8(2) . . ?
C27 C26 C25 105.5(2) . . ?
N11 C27 C26 110.3(2) . . ?
N8 C28 C29 108.76(17) . . ?
C28 C29 C30 105.13(17) . . ?
N9 C30 C29 109.93(19) . . ?
N6 B1 N8 107.24(18) . . ?
N6 B1 N10 106.64(16) . . ?
N10 B1 N8 106.98(16) . . ?

loop_
_geom_hbond_atom_site_label_D
_geom_hbond_atom_site_label_H
_geom_hbond_atom_site_label_A
_geom_hbond_distance_DH
_geom_hbond_distance_HA
_geom_hbond_distance_DA
_geom_hbond_angle_DHA
_geom_hbond_site_symmetry_A
O1C H1C O3 0.84 1.90 2.53(2) 131.0 .
O2 H2A N4 0.84 1.99 2.819(3) 169.1 2_655
O3 H3A O1C 0.84 1.70 2.53(2) 170.8 .
O3 H3A O4 0.84 2.01 2.838(10) 168.4 .
O5 H5A O1A 0.87 2.09 2.753(6) 131.9 .
O5 H5B O3 0.87 1.92 2.775(4) 167.7 .

_olex2_submission_special_instructions 'No special instructions were received'
####################################################################### 
# 
# 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_Tp_300K
_database_code_depnum_ccdc_archive 'CCDC 1974448'
loop_
_audit_author_name
_audit_author_address
'Xin-Hua Zhao'
;Southern University of Science and Technology
China
;
_audit_update_record             
;
2020-03-28 deposited with the CCDC.	2020-04-01 downloaded from the CCDC.
;
_audit_creation_date             2020-03-16
_audit_creation_method           
;
Olex2 1.2
(compiled 2018.05.29 svn.r3508 for OlexSys, GUI svn.r5506)
;
_shelx_SHELXL_version_number     2014/7
_chemical_name_common            ?
_chemical_name_systematic        ?
_chemical_formula_moiety         'C60 H54 B2 Fe3 N22, 7[CH3OH], 1[H2O]'
_chemical_formula_sum            'C67 H84 B2 Fe3 N22 O8'
_chemical_formula_weight         1514.73
_chemical_melting_point          ?
loop_
_atom_type_symbol
_atom_type_description
_atom_type_scat_dispersion_real
_atom_type_scat_dispersion_imag
_atom_type_scat_source
B B 0.0013 0.0007 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Fe Fe 0.3463 0.8444 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'

_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      monoclinic
_space_group_IT_number           15
_space_group_name_H-M_alt        'C 1 2/c 1'
_space_group_name_Hall           '-C 2yc'
loop_
_space_group_symop_operation_xyz
'x, y, z'
'-x, y, -z+1/2'
'x+1/2, y+1/2, z'
'-x+1/2, y+1/2, -z+1/2'
'-x, -y, -z'
'x, -y, z-1/2'
'-x+1/2, -y+1/2, -z'
'x+1/2, -y+1/2, z-1/2'

_cell_length_a                   19.309(4)
_cell_length_b                   18.909(4)
_cell_length_c                   23.215(4)
_cell_angle_alpha                90
_cell_angle_beta                 113.646(5)
_cell_angle_gamma                90
_cell_volume                     7764(3)
_cell_formula_units_Z            4
_cell_measurement_reflns_used    9855
_cell_measurement_temperature    299(2)
_cell_measurement_theta_max      24.717
_cell_measurement_theta_min      2.357
_shelx_estimated_absorpt_T_max   0.930
_shelx_estimated_absorpt_T_min   0.876
_exptl_absorpt_coefficient_mu    0.618
_exptl_absorpt_correction_T_max  0.7451
_exptl_absorpt_correction_T_min  0.6025
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   
'SADABS-2016/2 (Bruker,2016/2) was used for absorption correction. wR2(int) was 0.1239 before and 0.0651 after correction. The Ratio of minimum to maximum transmission is 0.8086. The λ/2 correction factor is Not present.'
_exptl_absorpt_special_details   ?
_exptl_crystal_colour            'dark red'
_exptl_crystal_colour_modifier   dark
_exptl_crystal_colour_primary    red
_exptl_crystal_density_diffrn    1.296
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    ?
_exptl_crystal_description       block
_exptl_crystal_F_000             3168
_exptl_crystal_size_max          0.22
_exptl_crystal_size_mid          0.19
_exptl_crystal_size_min          0.12
_exptl_transmission_factor_max   ?
_exptl_transmission_factor_min   ?
_diffrn_reflns_av_R_equivalents  0.0475
_diffrn_reflns_av_unetI/netI     0.0370
_diffrn_reflns_Laue_measured_fraction_full 0.993
_diffrn_reflns_Laue_measured_fraction_max 0.993
_diffrn_reflns_limit_h_max       22
_diffrn_reflns_limit_h_min       -21
_diffrn_reflns_limit_k_max       19
_diffrn_reflns_limit_k_min       -22
_diffrn_reflns_limit_l_max       27
_diffrn_reflns_limit_l_min       -24
_diffrn_reflns_number            33317
_diffrn_reflns_point_group_measured_fraction_full 0.993
_diffrn_reflns_point_group_measured_fraction_max 0.993
_diffrn_reflns_theta_full        24.797
_diffrn_reflns_theta_max         24.797
_diffrn_reflns_theta_min         2.154
_diffrn_ambient_temperature      299.97
_diffrn_detector_area_resol_mean ?
_diffrn_measured_fraction_theta_full 0.993
_diffrn_measured_fraction_theta_max 0.993
_diffrn_measurement_device_type  'Bruker APEX-II CCD'
_diffrn_measurement_method       'φ and ω scans'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_source                   ?
_diffrn_standards_number         0
_reflns_Friedel_coverage         0.000
_reflns_Friedel_fraction_full    .
_reflns_Friedel_fraction_max     .
_reflns_number_gt                5045
_reflns_number_total             6644
_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       'SAINT V8.38A (?, 2016)'
_computing_data_collection       'Bruker APEX3'
_computing_data_reduction        'SAINT V8.38A (?, 2016)'
_computing_molecular_graphics    'Olex2 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 (Dolomanov et al., 2009)'
_computing_structure_refinement  'XL (Sheldrick, 2008)'
_computing_structure_solution    'XT (Sheldrick, 2015)'
_refine_diff_density_max         0.481
_refine_diff_density_min         -0.316
_refine_diff_density_rms         0.061
_refine_ls_extinction_coef       .
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.029
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     397
_refine_ls_number_reflns         6644
_refine_ls_number_restraints     35
_refine_ls_R_factor_all          0.0669
_refine_ls_R_factor_gt           0.0485
_refine_ls_restrained_S_all      1.043
_refine_ls_shift/su_max          0.002
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details     
'w=1/[σ²(Fo²)+(0.0614P)²+15.5211P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1229
_refine_ls_wR_factor_ref         0.1379
_refine_special_details          ?
_olex2_refinement_description    
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups, All C(H,H) groups
2. Rigid bond restraints
 C16, C15
 with sigma for 1-2 distances of 0.01 and sigma for 1-3 distances of 0.01
 C16, C17
 with sigma for 1-2 distances of 0.01 and sigma for 1-3 distances of 0.01
 C14, C15
 with sigma for 1-2 distances of 0.01 and sigma for 1-3 distances of 0.01
 C14, C13
 with sigma for 1-2 distances of 0.01 and sigma for 1-3 distances of 0.01
 C13, C12
 with sigma for 1-2 distances of 0.01 and sigma for 1-3 distances of 0.01
3. Uiso/Uaniso restraints and constraints
C15 \\sim C16: within 2A with sigma of 0.01 and sigma for terminal atoms of 0.02
C16 \\sim C17: within 2A with sigma of 0.01 and sigma for terminal atoms of 0.02
C14 \\sim C15: within 2A with sigma of 0.01 and sigma for terminal atoms of 0.02
C14 \\sim C13: within 2A with sigma of 0.01 and sigma for terminal atoms of 0.02
C13 \\sim C12: within 2A with sigma of 0.01 and sigma for terminal atoms of 0.02
4.a Secondary CH2 refined with riding coordinates:
 C6(H6A,H6B), C7(H7A,H7B), C18(H18A,H18B)
4.b Aromatic/amide H refined with riding coordinates:
 C1(H1), C2(H2), C3(H3), C4(H4), C9(H9), C14(H14), C11(H11), C12(H12),
 C13(H13), C16(H16), C17(H17), C22(H22), C23(H23), C24(H24), C25(H25), C26(H26),
  C27(H27), C28(H28), C29(H29), C30(H30)
;
_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
Fe1 Fe 0.5000 0.42321(3) 0.2500 0.03029(16) Uani 1 2 d S T P . .
Fe2 Fe 0.68447(3) 0.60543(3) 0.37218(2) 0.04715(16) Uani 1 1 d . . . . .
N1 N 0.45408(13) 0.42495(12) 0.31253(10) 0.0361(5) Uani 1 1 d . . . . .
N2 N 0.42204(13) 0.34553(12) 0.21194(10) 0.0378(5) Uani 1 1 d . . . . .
N3 N 0.57209(13) 0.49391(13) 0.29478(11) 0.0364(5) Uani 1 1 d . . . . .
N4 N 0.6556(3) 0.5455(2) 0.48323(17) 0.1008(14) Uani 1 1 d . . . . .
N5 N 0.8047(2) 0.4919(2) 0.3928(2) 0.1090(15) Uani 1 1 d . . . . .
N6 N 0.61475(17) 0.74422(16) 0.34260(13) 0.0577(7) Uani 1 1 d . . . . .
N7 N 0.60266(15) 0.67610(15) 0.35507(12) 0.0520(7) Uani 1 1 d . . . . .
N8 N 0.75285(16) 0.74342(15) 0.40370(13) 0.0546(7) Uani 1 1 d . . . . .
N9 N 0.75815(14) 0.67548(15) 0.42425(11) 0.0484(7) Uani 1 1 d . . . . .
N10 N 0.69914(16) 0.71425(17) 0.29029(12) 0.0595(8) Uani 1 1 d . . . . .
N11 N 0.69884(16) 0.64337(17) 0.29847(12) 0.0582(8) Uani 1 1 d . . . . .
C1 C 0.47969(18) 0.46005(17) 0.36784(13) 0.0434(7) Uani 1 1 d . . . . .
H1 H 0.5287 0.4779 0.3838 0.052 Uiso 1 1 calc R . . . .
C2 C 0.4359(2) 0.47020(19) 0.40137(14) 0.0548(9) Uani 1 1 d . . . . .
H2 H 0.4549 0.4955 0.4389 0.066 Uiso 1 1 calc R . . . .
C3 C 0.3646(2) 0.4432(2) 0.37963(17) 0.0677(11) Uani 1 1 d . . . . .
H3 H 0.3342 0.4499 0.4017 0.081 Uiso 1 1 calc R . . . .
C4 C 0.3386(2) 0.4055(2) 0.32392(17) 0.0658(10) Uani 1 1 d . . . . .
H4 H 0.2905 0.3857 0.3082 0.079 Uiso 1 1 calc R . . . .
C5 C 0.38488(17) 0.39778(17) 0.29181(14) 0.0436(7) Uani 1 1 d . . . . .
C6 C 0.35702(18) 0.36330(19) 0.22828(14) 0.0500(8) Uani 1 1 d . . . . .
H6A H 0.3294 0.3206 0.2286 0.060 Uiso 1 1 calc R . . . .
H6B H 0.3229 0.3951 0.1969 0.060 Uiso 1 1 calc R . . . .
C7 C 0.39465(18) 0.33744(18) 0.14156(12) 0.0464(8) Uani 1 1 d . . . . .
H7A H 0.3784 0.3834 0.1224 0.056 Uiso 1 1 calc R . . . .
H7B H 0.4370 0.3228 0.1320 0.056 Uiso 1 1 calc R . . . .
C8 C 0.3311(2) 0.28589(18) 0.11141(14) 0.0512(8) Uani 1 1 d . . . . .
C9 C 0.2577(2) 0.3068(2) 0.09109(14) 0.0614(10) Uani 1 1 d . . . . .
H9 H 0.2473 0.3540 0.0958 0.074 Uiso 1 1 calc R . . . .
C14 C 0.1499(4) 0.1398(4) 0.0255(2) 0.127(2) Uani 1 1 d . U . . .
H14 H 0.1589 0.0928 0.0189 0.153 Uiso 1 1 calc R . . . .
C15 C 0.2113(3) 0.1897(3) 0.05380(17) 0.0903(15) Uani 1 1 d . U . . .
C10 C 0.1966(3) 0.2594(3) 0.06303(16) 0.0796(14) Uani 1 1 d . . . . .
C11 C 0.1216(3) 0.2809(4) 0.0440(2) 0.117(2) Uani 1 1 d . . . . .
H11 H 0.1114 0.3279 0.0496 0.141 Uiso 1 1 calc R . . . .
C12 C 0.0628(4) 0.2351(5) 0.0176(3) 0.149(3) Uani 1 1 d . U . . .
H12 H 0.0130 0.2500 0.0054 0.178 Uiso 1 1 calc R . . . .
C13 C 0.0802(5) 0.1643(5) 0.0094(3) 0.147(3) Uani 1 1 d . U . . .
H13 H 0.0403 0.1328 -0.0085 0.176 Uiso 1 1 calc R . . . .
C16 C 0.2852(3) 0.1682(2) 0.07236(19) 0.0903(14) Uani 1 1 d . U . . .
H16 H 0.2952 0.1216 0.0653 0.108 Uiso 1 1 calc R . . . .
C17 C 0.3455(3) 0.2146(2) 0.10156(17) 0.0755(12) Uani 1 1 d . U . . .
H17 H 0.3950 0.1986 0.1145 0.091 Uiso 1 1 calc R . . . .
C18 C 0.45926(19) 0.27973(17) 0.24586(14) 0.0513(8) Uani 1 1 d . . . . .
H18A H 0.4336 0.2385 0.2219 0.062 Uiso 1 1 calc R . . . .
H18B H 0.4564 0.2779 0.2866 0.062 Uiso 1 1 calc R . . . .
C19 C 0.61418(18) 0.53667(17) 0.32253(13) 0.0430(7) Uani 1 1 d . . . . .
C20 C 0.6678(2) 0.5676(2) 0.44233(16) 0.0615(10) Uani 1 1 d . . . . .
C21 C 0.7611(2) 0.5347(2) 0.38706(19) 0.0664(10) Uani 1 1 d . . . . .
C22 C 0.7046(2) 0.7284(3) 0.23568(18) 0.0765(13) Uani 1 1 d . . . . .
H22 H 0.7053 0.7731 0.2192 0.092 Uiso 1 1 calc R . . . .
C23 C 0.7088(3) 0.6659(3) 0.20882(19) 0.0919(15) Uani 1 1 d . . . . .
H23 H 0.7139 0.6595 0.1710 0.110 Uiso 1 1 calc R . . . .
C24 C 0.7041(2) 0.6136(3) 0.24839(17) 0.0757(12) Uani 1 1 d . . . . .
H24 H 0.7046 0.5652 0.2413 0.091 Uiso 1 1 calc R . . . .
C25 C 0.5528(2) 0.7820(2) 0.33293(19) 0.0746(11) Uani 1 1 d . . . . .
H25 H 0.5468 0.8300 0.3234 0.090 Uiso 1 1 calc R . . . .
C26 C 0.4997(2) 0.7390(3) 0.3393(2) 0.0814(13) Uani 1 1 d . . . . .
H26 H 0.4514 0.7515 0.3354 0.098 Uiso 1 1 calc R . . . .
C27 C 0.5324(2) 0.6735(2) 0.35260(17) 0.0647(10) Uani 1 1 d . . . . .
H27 H 0.5091 0.6330 0.3590 0.078 Uiso 1 1 calc R . . . .
C28 C 0.8069(2) 0.7819(2) 0.44741(18) 0.0680(11) Uani 1 1 d . . . . .
H28 H 0.8154 0.8299 0.4448 0.082 Uiso 1 1 calc R . . . .
C29 C 0.8469(2) 0.7388(2) 0.49612(19) 0.0726(12) Uani 1 1 d . . . . .
H29 H 0.8877 0.7514 0.5329 0.087 Uiso 1 1 calc R . . . .
C30 C 0.8155(2) 0.6732(2) 0.48039(15) 0.0612(10) Uani 1 1 d . . . . .
H30 H 0.8318 0.6329 0.5052 0.073 Uiso 1 1 calc R . . . .
B1 B 0.6903(3) 0.7632(2) 0.3395(2) 0.0620(11) Uani 1 1 d . . . . .
H1A H 0.6935(18) 0.8202(19) 0.3279(15) 0.060(10) Uiso 1 1 d . . . . .


_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
Fe1 N1 1.982(2) . ?
Fe1 N1 1.982(2) 2_655 ?
Fe1 N2 2.034(2) . ?
Fe1 N2 2.034(2) 2_655 ?
Fe1 N3 1.909(2) . ?
Fe1 N3 1.909(2) 2_655 ?
Fe2 N7 1.984(3) . ?
Fe2 N9 1.965(2) . ?
Fe2 N11 1.975(3) . ?
Fe2 C19 1.899(3) . ?
Fe2 C20 1.920(4) . ?
Fe2 C21 1.921(5) . ?
N1 C1 1.351(3) . ?
N1 C5 1.328(4) . ?
N2 C6 1.488(4) . ?
N2 C7 1.510(3) . ?
N2 C18 1.494(4) . ?
N3 C19 1.144(4) . ?
N4 C20 1.145(5) . ?
N5 C21 1.135(5) . ?
N6 N7 1.361(4) . ?
N6 C25 1.333(5) . ?
N6 B1 1.531(5) . ?
N7 C27 1.336(4) . ?
N8 N9 1.360(4) . ?
N8 C28 1.341(4) . ?
N8 B1 1.541(5) . ?
N9 C30 1.330(4) . ?
N10 N11 1.354(4) . ?
N10 C22 1.340(4) . ?
N10 B1 1.533(6) . ?
N11 C24 1.332(4) . ?
C1 C2 1.373(4) . ?
C2 C3 1.361(5) . ?
C3 C4 1.382(5) . ?
C4 C5 1.383(4) . ?
C5 C6 1.501(4) . ?
C7 C8 1.502(4) . ?
C8 C9 1.361(5) . ?
C8 C17 1.413(5) . ?
C9 C10 1.415(5) . ?
C14 C15 1.451(6) . ?
C14 C13 1.328(10) . ?
C15 C10 1.383(7) . ?
C15 C16 1.376(7) . ?
C10 C11 1.395(7) . ?
C11 C12 1.363(8) . ?
C12 C13 1.413(11) . ?
C16 C17 1.398(6) . ?
C18 C18 1.507(7) 2_655 ?
C22 C23 1.355(7) . ?
C23 C24 1.377(6) . ?
C25 C26 1.362(6) . ?
C26 C27 1.369(6) . ?
C28 C29 1.356(6) . ?
C29 C30 1.364(5) . ?

loop_
_geom_angle_atom_site_label_1
_geom_angle_atom_site_label_2
_geom_angle_atom_site_label_3
_geom_angle
_geom_angle_site_symmetry_1
_geom_angle_site_symmetry_3
_geom_angle_publ_flag
N1 Fe1 N1 178.09(14) . 2_655 ?
N1 Fe1 N2 99.46(9) . 2_655 ?
N1 Fe1 N2 81.93(9) 2_655 2_655 ?
N1 Fe1 N2 99.46(9) 2_655 . ?
N1 Fe1 N2 81.93(9) . . ?
N2 Fe1 N2 87.54(14) . 2_655 ?
N3 Fe1 N1 86.81(9) 2_655 . ?
N3 Fe1 N1 86.81(9) . 2_655 ?
N3 Fe1 N1 91.85(9) 2_655 2_655 ?
N3 Fe1 N1 91.85(9) . . ?
N3 Fe1 N2 91.04(10) 2_655 . ?
N3 Fe1 N2 173.29(9) . . ?
N3 Fe1 N2 91.04(10) . 2_655 ?
N3 Fe1 N2 173.30(9) 2_655 2_655 ?
N3 Fe1 N3 91.11(14) . 2_655 ?
N9 Fe2 N7 89.48(11) . . ?
N9 Fe2 N11 88.25(11) . . ?
N11 Fe2 N7 87.65(13) . . ?
C19 Fe2 N7 91.24(12) . . ?
C19 Fe2 N9 179.19(14) . . ?
C19 Fe2 N11 92.14(12) . . ?
C19 Fe2 C20 86.43(13) . . ?
C19 Fe2 C21 86.78(15) . . ?
C20 Fe2 N7 91.70(15) . . ?
C20 Fe2 N9 93.19(12) . . ?
C20 Fe2 N11 178.42(13) . . ?
C20 Fe2 C21 88.14(18) . . ?
C21 Fe2 N7 178.02(13) . . ?
C21 Fe2 N9 92.49(14) . . ?
C21 Fe2 N11 92.46(16) . . ?
C1 N1 Fe1 127.1(2) . . ?
C5 N1 Fe1 114.14(18) . . ?
C5 N1 C1 117.8(3) . . ?
C6 N2 Fe1 106.22(17) . . ?
C6 N2 C7 109.5(2) . . ?
C6 N2 C18 109.3(2) . . ?
C7 N2 Fe1 114.85(18) . . ?
C18 N2 Fe1 104.88(17) . . ?
C18 N2 C7 111.8(2) . . ?
C19 N3 Fe1 178.2(2) . . ?
N7 N6 B1 118.7(3) . . ?
C25 N6 N7 108.9(3) . . ?
C25 N6 B1 132.4(4) . . ?
N6 N7 Fe2 119.3(2) . . ?
C27 N7 Fe2 134.2(3) . . ?
C27 N7 N6 106.5(3) . . ?
N9 N8 B1 119.2(3) . . ?
C28 N8 N9 108.7(3) . . ?
C28 N8 B1 132.1(3) . . ?
N8 N9 Fe2 119.15(19) . . ?
C30 N9 Fe2 133.9(3) . . ?
C30 N9 N8 106.9(3) . . ?
N11 N10 B1 119.0(3) . . ?
C22 N10 N11 109.7(3) . . ?
C22 N10 B1 131.2(4) . . ?
N10 N11 Fe2 119.4(2) . . ?
C24 N11 Fe2 133.6(3) . . ?
C24 N11 N10 106.8(3) . . ?
N1 C1 C2 122.3(3) . . ?
C3 C2 C1 119.9(3) . . ?
C2 C3 C4 118.3(3) . . ?
C3 C4 C5 119.2(3) . . ?
N1 C5 C4 122.5(3) . . ?
N1 C5 C6 115.8(2) . . ?
C4 C5 C6 121.4(3) . . ?
N2 C6 C5 110.0(2) . . ?
C8 C7 N2 115.9(2) . . ?
C9 C8 C7 121.0(3) . . ?
C9 C8 C17 117.8(3) . . ?
C17 C8 C7 121.1(4) . . ?
C8 C9 C10 122.3(4) . . ?
C13 C14 C15 116.9(7) . . ?
C10 C15 C14 120.6(6) . . ?
C16 C15 C14 120.4(6) . . ?
C16 C15 C10 119.0(4) . . ?
C15 C10 C9 119.4(5) . . ?
C15 C10 C11 118.8(5) . . ?
C11 C10 C9 121.9(5) . . ?
C12 C11 C10 121.9(7) . . ?
C11 C12 C13 117.5(7) . . ?
C14 C13 C12 124.3(6) . . ?
C15 C16 C17 121.6(5) . . ?
C16 C17 C8 119.8(5) . . ?
N2 C18 C18 108.9(2) . 2_655 ?
N3 C19 Fe2 177.3(3) . . ?
N4 C20 Fe2 177.9(4) . . ?
N5 C21 Fe2 176.6(4) . . ?
N10 C22 C23 107.6(4) . . ?
C22 C23 C24 106.7(4) . . ?
N11 C24 C23 109.1(4) . . ?
N6 C25 C26 109.0(4) . . ?
C25 C26 C27 105.4(4) . . ?
N7 C27 C26 110.2(4) . . ?
N8 C28 C29 108.4(3) . . ?
C28 C29 C30 106.2(3) . . ?
N9 C30 C29 109.8(4) . . ?
N6 B1 N8 106.9(3) . . ?
N6 B1 N10 106.6(3) . . ?
N10 B1 N8 107.2(3) . . ?

_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 0.500 -0.345 1230.1 246.0 3.5CH3OH
2 0.500 0.000 -0.963 1230.1 246.0 3.5CH3OH

_olex2_submission_special_instructions 'No special instructions were received'
####################################################################### 
# 
# 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_Tp+_300K
_database_code_depnum_ccdc_archive 'CCDC 1974452'
loop_
_audit_author_name
_audit_author_address
'Xin-Hua Zhao'
;Southern University of Science and Technology
China
;
_audit_update_record             
;
2020-03-27 deposited with the CCDC.	2020-04-01 downloaded from the CCDC.
;
_audit_creation_date             2020-03-17
_audit_creation_method           
;
Olex2 1.2
(compiled 2018.05.29 svn.r3508 for OlexSys, GUI svn.r5506)
;
_shelx_SHELXL_version_number     2014/7
_chemical_name_common            ?
_chemical_name_systematic        bnbpenTp+300k
_chemical_formula_moiety         'C72 H78 B2 Fe3 N22, 6[CH3OH], 8[H2O]'
_chemical_formula_sum            'C78 H118 B2 Fe3 N22 O14'
_chemical_formula_weight         1777.11
_chemical_melting_point          ?
loop_
_atom_type_symbol
_atom_type_description
_atom_type_scat_dispersion_real
_atom_type_scat_dispersion_imag
_atom_type_scat_source
B B 0.0013 0.0007 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Fe Fe 0.3463 0.8444 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'

_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      monoclinic
_space_group_IT_number           15
_space_group_name_H-M_alt        'C 1 2/c 1'
_space_group_name_Hall           '-C 2yc'
loop_
_space_group_symop_operation_xyz
'x, y, z'
'-x, y, -z+1/2'
'x+1/2, y+1/2, z'
'-x+1/2, y+1/2, -z+1/2'
'-x, -y, -z'
'x, -y, z-1/2'
'-x+1/2, -y+1/2, -z'
'x+1/2, -y+1/2, z-1/2'

_cell_length_a                   23.678(7)
_cell_length_b                   21.345(8)
_cell_length_c                   22.221(9)
_cell_angle_alpha                90
_cell_angle_beta                 116.701(9)
_cell_angle_gamma                90
_cell_volume                     10033(6)
_cell_formula_units_Z            4
_cell_measurement_reflns_used    8612
_cell_measurement_temperature    100(2)
_cell_measurement_theta_max      27.070
_cell_measurement_theta_min      2.575
_shelx_estimated_absorpt_T_max   0.943
_shelx_estimated_absorpt_T_min   0.908
_exptl_absorpt_coefficient_mu    0.492
_exptl_absorpt_correction_T_max  0.7454
_exptl_absorpt_correction_T_min  0.6094
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   
'SADABS-2016/2 (Bruker,2016/2) was used for absorption correction. wR2(int) was 0.1316 before and 0.0705 after correction. The Ratio of minimum to maximum transmission is 0.8175. The λ/2 correction factor is Not present.'
_exptl_absorpt_special_details   ?
_exptl_crystal_colour            'dark red'
_exptl_crystal_colour_modifier   dark
_exptl_crystal_colour_primary    red
_exptl_crystal_density_diffrn    1.176
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    ?
_exptl_crystal_description       block
_exptl_crystal_F_000             3760
_exptl_crystal_size_max          0.2
_exptl_crystal_size_mid          0.15
_exptl_crystal_size_min          0.12
_exptl_transmission_factor_max   ?
_exptl_transmission_factor_min   ?
_diffrn_reflns_av_R_equivalents  0.0534
_diffrn_reflns_av_unetI/netI     0.0850
_diffrn_reflns_Laue_measured_fraction_full 0.989
_diffrn_reflns_Laue_measured_fraction_max 0.973
_diffrn_reflns_limit_h_max       24
_diffrn_reflns_limit_h_min       -29
_diffrn_reflns_limit_k_max       26
_diffrn_reflns_limit_k_min       -21
_diffrn_reflns_limit_l_max       27
_diffrn_reflns_limit_l_min       -19
_diffrn_reflns_number            22160
_diffrn_reflns_point_group_measured_fraction_full 0.989
_diffrn_reflns_point_group_measured_fraction_max 0.973
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         26.454
_diffrn_reflns_theta_min         2.167
_diffrn_ambient_temperature      100.02
_diffrn_detector_area_resol_mean ?
_diffrn_measured_fraction_theta_full 0.989
_diffrn_measured_fraction_theta_max 0.973
_diffrn_measurement_device_type  'Bruker APEX-II CCD'
_diffrn_measurement_method       'φ and ω scans'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_source                   ?
_diffrn_standards_number         0
_reflns_Friedel_coverage         0.000
_reflns_Friedel_fraction_full    .
_reflns_Friedel_fraction_max     .
_reflns_number_gt                5704
_reflns_number_total             10080
_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       'SAINT V8.38A (?, 2016)'
_computing_data_collection       'Bruker APEX3'
_computing_data_reduction        'SAINT V8.38A (?, 2016)'
_computing_molecular_graphics    'Olex2 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 (Dolomanov et al., 2009)'
_computing_structure_refinement  'XL (Sheldrick, 2008)'
_computing_structure_solution    'ShelXT (Sheldrick, 2015)'
_refine_diff_density_max         0.985
_refine_diff_density_min         -0.431
_refine_diff_density_rms         0.058
_refine_ls_extinction_coef       .
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.041
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     436
_refine_ls_number_reflns         10080
_refine_ls_number_restraints     66
_refine_ls_R_factor_all          0.1155
_refine_ls_R_factor_gt           0.0658
_refine_ls_restrained_S_all      1.041
_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+19.6436P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1553
_refine_ls_wR_factor_ref         0.1847
_refine_special_details          ?
_olex2_refinement_description    
;
1. Fixed Uiso
 At 1.2 times of:
  All B(H) groups, All C(H) groups, All C(H,H) groups, All C(H,H,H,H) groups
 At 1.5 times of:
  All C(H,H,H) groups
2. Uiso/Uaniso restraints and constraints
C9 \\sim C8 \\sim C17 \\sim C16 \\sim C15 \\sim C10 \\sim C11 \\sim C12 \\sim
C13 \\sim C14: within 2A with sigma of 0.02 and sigma for terminal atoms of 0.04
Uanis(C4BA) = Uanis(C9)
Uanis(C10) = Uanis(C9AA)
Uanis(C3) = Uanis(C8)
Uanis(C15) = Uanis(C3BA)
Uanis(C0BA) = Uanis(C17)
Uanis(C16) = Uanis(C4AA)
Uanis(C7AA) = Uanis(C11)
Uanis(C12) = Uanis(C5AA)
Uanis(C2BA) = Uanis(C13)
Uanis(C1BA) = Uanis(C14)
3. Others
 Sof(H7BC)=Sof(H7BD)=Sof(C7AA)=Sof(H7AC)=Sof(C2BA)=Sof(H2BA)=Sof(C1BA)=
 Sof(H1BA)=Sof(C5AA)=Sof(H5AA)=Sof(C4AA)=Sof(C0BA)=Sof(C3)=Sof(H3)=Sof(C4BA)=
 Sof(C9AA)=Sof(H9AA)=Sof(C3BA)=Sof(H3BA)=1-FVAR(1)
 Sof(H7AA)=Sof(H7AB)=Sof(C8)=Sof(H8)=Sof(C9)=Sof(C10)=Sof(H10)=Sof(C15)=
 Sof(H15)=Sof(C16)=Sof(C17)=Sof(C11)=Sof(H11)=Sof(C13)=Sof(H13)=Sof(C14)=
 Sof(H14)=Sof(C12)=Sof(H12)=FVAR(1)
4.a Ternary CH refined with riding coordinates:
 B1(H1A)
4.b Secondary CH2 refined with riding coordinates:
 C6(H6A,H6B), C7(H7AA,H7AB), C7(H7BC,H7BD), C18(H18A,H18B)
4.c Aromatic/amide H refined with riding coordinates:
 C24(H24), C1(H1), C29(H29), C2(H2), C4(H4), C2AA(H2AA), C34(H34), C8(H8),
 C10(H10), C15(H15), C11(H11), C13(H13), C14(H14), C12(H12), C7AA(H7AC),
 C2BA(H2BA), C1BA(H1BA), C5AA(H5AA), C3(H3), C9AA(H9AA), C3BA(H3BA)
4.d Naphthalene refined as free rotating group:
 C8(C9,C10,C15,C16,C17,C11,C13,C14,C12), C7AA(C2BA,C1BA,C5AA,C4AA,C0BA,C3,C4BA,
 C9AA,C3BA)
4.e Idealised Me refined as rotating group:
 C31(H31A,H31B,H31C), C26(H26A,H26B,H26C), C23(H23A,H23B,H23C), C28(H28A,H28B,
 H28C), C36(H36A,H36B,H36C), C33(H33A,H33B,H33C)
;
_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
Fe1 Fe 0.5000 0.58088(3) 0.7500 0.03911(19) Uani 1 2 d S T P . .
Fe2 Fe 0.38004(2) 0.41341(3) 0.57680(3) 0.04919(18) Uani 1 1 d . . . . .
N3 N 0.45412(14) 0.51503(14) 0.68144(15) 0.0461(7) Uani 1 1 d . . . . .
N1 N 0.43023(13) 0.58581(15) 0.78185(15) 0.0498(8) Uani 1 1 d . . . . .
N7 N 0.39664(14) 0.34252(15) 0.64182(15) 0.0525(8) Uani 1 1 d . . . . .
N9 N 0.45297(13) 0.38174(15) 0.56291(14) 0.0503(8) Uani 1 1 d . . . . .
N8 N 0.45476(14) 0.31902(16) 0.55015(16) 0.0558(8) Uani 1 1 d . . . . .
N6 N 0.40549(14) 0.28373(16) 0.62176(16) 0.0540(8) Uani 1 1 d . . . . .
N11 N 0.32072(14) 0.35836(16) 0.49981(16) 0.0560(8) Uani 1 1 d . . . . .
N2 N 0.53529(14) 0.65497(15) 0.82265(14) 0.0512(8) Uani 1 1 d . . . . .
N10 N 0.33862(15) 0.29775(17) 0.49810(17) 0.0594(9) Uani 1 1 d . . . . .
N4 N 0.27077(19) 0.4585(2) 0.6051(2) 0.0854(12) Uani 1 1 d . . . . .
N5 N 0.35773(18) 0.5242(2) 0.4797(2) 0.0770(11) Uani 1 1 d . . . . .
C19 C 0.42946(17) 0.47408(19) 0.64542(18) 0.0469(9) Uani 1 1 d . . . . .
C5 C 0.44783(17) 0.61557(19) 0.84121(19) 0.0535(10) Uani 1 1 d . . . . .
C24 C 0.41582(19) 0.2735(2) 0.7241(2) 0.0659(12) Uani 1 1 d . . . . .
H24 H 0.4220 0.2560 0.7659 0.079 Uiso 1 1 calc R . . . .
C1 C 0.37216(16) 0.5609(2) 0.75140(19) 0.0557(10) Uani 1 1 d . . . . .
H1 H 0.3600 0.5393 0.7100 0.067 Uiso 1 1 calc R . . . .
C31 C 0.52461(18) 0.4744(2) 0.58190(19) 0.0586(11) Uani 1 1 d . . . . .
H31A H 0.4877 0.5011 0.5568 0.088 Uiso 1 1 calc GR . . . .
H31B H 0.5581 0.4849 0.5691 0.088 Uiso 1 1 calc GR . . . .
H31C H 0.5400 0.4813 0.6303 0.088 Uiso 1 1 calc GR . . . .
C27 C 0.5075(2) 0.3057(2) 0.5444(2) 0.0645(11) Uani 1 1 d . . . . .
C25 C 0.40321(18) 0.3358(2) 0.7054(2) 0.0592(11) Uani 1 1 d . . . . .
C29 C 0.54068(19) 0.3611(2) 0.5536(2) 0.0610(11) Uani 1 1 d . . . . .
H29 H 0.5797 0.3662 0.5517 0.073 Uiso 1 1 calc R . . . .
C30 C 0.50659(17) 0.40798(19) 0.56593(17) 0.0499(9) Uani 1 1 d . . . . .
C21 C 0.36565(18) 0.4822(2) 0.5150(2) 0.0538(10) Uani 1 1 d . . . . .
C22 C 0.41769(17) 0.2419(2) 0.6716(2) 0.0610(11) Uani 1 1 d . . . . .
C6 C 0.51539(18) 0.6403(2) 0.87527(18) 0.0574(10) Uani 1 1 d . . . . .
H6A H 0.5175 0.6785 0.9015 0.069 Uiso 1 1 calc R . . . .
H6B H 0.5439 0.6084 0.9065 0.069 Uiso 1 1 calc R . . . .
C35 C 0.26248(18) 0.3660(2) 0.4460(2) 0.0659(12) Uani 1 1 d . . . . .
C26 C 0.3987(3) 0.3886(2) 0.7471(2) 0.0803(14) Uani 1 1 d . . . . .
H26A H 0.4316 0.4196 0.7539 0.121 Uiso 1 1 calc GR . . . .
H26B H 0.4046 0.3726 0.7908 0.121 Uiso 1 1 calc GR . . . .
H26C H 0.3570 0.4084 0.7238 0.121 Uiso 1 1 calc GR . . . .
C7 C 0.60711(16) 0.6625(2) 0.8557(2) 0.0595(11) Uani 1 1 d . . . . .
H7AA H 0.6209 0.6647 0.8198 0.071 Uiso 0.294(4) 1 calc R . . A 1
H7AB H 0.6265 0.6247 0.8829 0.071 Uiso 0.294(4) 1 calc R . . A 1
H7BC H 0.6263 0.6204 0.8687 0.071 Uiso 0.706(4) 1 calc R . . A 2
H7BD H 0.6191 0.6791 0.8214 0.071 Uiso 0.706(4) 1 calc R . . A 2
C2 C 0.3297(2) 0.5651(2) 0.7773(2) 0.0744(13) Uani 1 1 d . . . . .
H2 H 0.2887 0.5474 0.7540 0.089 Uiso 1 1 calc R . . . .
C4 C 0.4076(2) 0.6214(2) 0.8704(2) 0.0704(12) Uani 1 1 d . . . . .
H4 H 0.4206 0.6429 0.9120 0.085 Uiso 1 1 calc R . . . .
C2AA C 0.3474(2) 0.5952(2) 0.8375(3) 0.0780(14) Uani 1 1 d . . . . .
H2AA H 0.3189 0.5983 0.8567 0.094 Uiso 1 1 calc R . . . .
C20 C 0.31085(19) 0.4414(2) 0.5933(2) 0.0619(11) Uani 1 1 d . . . . .
C34 C 0.2444(2) 0.3102(3) 0.4112(2) 0.0766(14) Uani 1 1 d . . . . .
H34 H 0.2063 0.3024 0.3716 0.092 Uiso 1 1 calc R . . . .
C32 C 0.2919(2) 0.2682(2) 0.4445(2) 0.0717(13) Uani 1 1 d . . . . .
C18 C 0.50205(19) 0.71244(19) 0.7851(2) 0.0603(11) Uani 1 1 d . . . . .
H18A H 0.5252 0.7501 0.8099 0.072 Uiso 1 1 calc R . . . .
H18B H 0.4589 0.7139 0.7818 0.072 Uiso 1 1 calc R . . . .
C23 C 0.4304(2) 0.1742(2) 0.6647(3) 0.0820(14) Uani 1 1 d . . . . .
H23A H 0.3977 0.1579 0.6221 0.123 Uiso 1 1 calc GR . . . .
H23B H 0.4301 0.1504 0.7023 0.123 Uiso 1 1 calc GR . . . .
H23C H 0.4719 0.1700 0.6653 0.123 Uiso 1 1 calc GR . . . .
C28 C 0.5228(2) 0.2413(2) 0.5306(3) 0.0915(16) Uani 1 1 d . . . . .
H28A H 0.5271 0.2134 0.5674 0.137 Uiso 1 1 calc GR . . . .
H28B H 0.5627 0.2421 0.5272 0.137 Uiso 1 1 calc GR . . . .
H28C H 0.4889 0.2261 0.4882 0.137 Uiso 1 1 calc GR . . . .
C8 C 0.6548(6) 0.7136(4) 0.9716(5) 0.0709(18) Uani 0.294(4) 1 d . U . A 1
H8 H 0.6521 0.6734 0.9883 0.085 Uiso 0.294(4) 1 calc R . . A 1
C9 C 0.6336(6) 0.7226(4) 0.9028(4) 0.0572(15) Uani 0.294(4) 1 d G U . A 1
C10 C 0.6377(5) 0.7815(5) 0.8783(4) 0.0597(15) Uani 0.294(4) 1 d G U . A 1
H10 H 0.6231 0.7876 0.8314 0.072 Uiso 0.294(4) 1 calc R . . A 1
C15 C 0.6630(5) 0.8314(4) 0.9226(4) 0.0710(16) Uani 0.294(4) 1 d G U . A 1
H15 H 0.6657 0.8717 0.9059 0.085 Uiso 0.294(4) 1 calc R . . A 1
C16 C 0.6842(3) 0.8224(4) 0.9913(4) 0.0663(18) Uani 0.294(4) 1 d G U . A 1
C17 C 0.6802(4) 0.7635(4) 1.0158(4) 0.0694(17) Uani 0.294(4) 1 d G U . A 1
C11 C 0.7014(6) 0.7546(5) 1.0845(4) 0.122(3) Uani 0.294(4) 1 d G U . A 1
H11 H 0.6986 0.7143 1.1013 0.147 Uiso 0.294(4) 1 calc R . . A 1
C13 C 0.7267(6) 0.8045(6) 1.1288(4) 0.131(3) Uani 0.294(4) 1 d G U . A 1
H13 H 0.7412 0.7984 1.1758 0.158 Uiso 0.294(4) 1 calc R . . A 1
C14 C 0.7308(6) 0.8634(6) 1.1043(5) 0.118(3) Uani 0.294(4) 1 d G U . A 1
H14 H 0.7481 0.8975 1.1346 0.142 Uiso 0.294(4) 1 calc R . . A 1
C12 C 0.7095(6) 0.8724(4) 1.0356(5) 0.097(2) Uani 0.294(4) 1 d G U . A 1
H12 H 0.7123 0.9126 1.0189 0.116 Uiso 0.294(4) 1 calc R . . A 1
C36 C 0.2262(2) 0.4260(3) 0.4305(3) 0.0896(16) Uani 1 1 d . . . . .
H36A H 0.2117 0.4339 0.4648 0.134 Uiso 1 1 calc GR . . . .
H36B H 0.1895 0.4230 0.3861 0.134 Uiso 1 1 calc GR . . . .
H36C H 0.2534 0.4605 0.4303 0.134 Uiso 1 1 calc GR . . . .
C33 C 0.2962(3) 0.2003(3) 0.4300(3) 0.1003(18) Uani 1 1 d . . . . .
H33A H 0.3333 0.1936 0.4221 0.151 Uiso 1 1 calc GR . . . .
H33B H 0.2580 0.1879 0.3899 0.151 Uiso 1 1 calc GR . . . .
H33C H 0.3002 0.1751 0.4686 0.151 Uiso 1 1 calc GR . . . .
B1 B 0.4031(2) 0.2764(2) 0.5520(2) 0.0605(12) Uani 1 1 d . . . . .
H1A H 0.4110 0.2318 0.5443 0.073 Uiso 1 1 calc R . . . .
C7AA C 0.6786(2) 0.87111(15) 0.9507(2) 0.122(3) Uani 0.706(4) 1 d . . . A 2
H7AC H 0.6652 0.8864 0.9062 0.147 Uiso 0.706(4) 1 calc R . . A 2
C2BA C 0.7057(3) 0.91171(14) 1.0052(3) 0.131(3) Uani 0.706(4) 1 d G . . A 2
H2BA H 0.7109 0.9548 0.9980 0.158 Uiso 0.706(4) 1 calc R . . A 2
C1BA C 0.7253(2) 0.88931(18) 1.0703(2) 0.118(3) Uani 0.706(4) 1 d G . . A 2
H1BA H 0.7439 0.9171 1.1076 0.142 Uiso 0.706(4) 1 calc R . . A 2
C5AA C 0.7178(2) 0.82632(19) 1.08085(16) 0.097(2) Uani 0.706(4) 1 d G . . A 2
H5AA H 0.7312 0.8110 1.1253 0.116 Uiso 0.706(4) 1 calc R . . A 2
C4AA C 0.69070(13) 0.78572(15) 1.02632(13) 0.0663(18) Uani 0.706(4) 1 d G . . A
2
C0BA C 0.67111(15) 0.80812(14) 0.96125(14) 0.0694(17) Uani 0.706(4) 1 d G . . A
2
C3 C 0.6440(2) 0.76753(17) 0.90672(13) 0.0709(18) Uani 0.706(4) 1 d G . . A 2
H3 H 0.6306 0.7828 0.8622 0.085 Uiso 0.706(4) 1 calc R . . A 2
C4BA C 0.6365(2) 0.70453(16) 0.91726(17) 0.0572(15) Uani 0.706(4) 1 d G . . A 2
C9AA C 0.6561(2) 0.68214(14) 0.98234(19) 0.0597(15) Uani 0.706(4) 1 d G . . A 2
H9AA H 0.6509 0.6391 0.9895 0.072 Uiso 0.706(4) 1 calc R . . A 2
C3BA C 0.68317(18) 0.72273(16) 1.03687(15) 0.0710(16) Uani 0.706(4) 1 d G . . A
2
H3BA H 0.6966 0.7074 1.0813 0.085 Uiso 0.706(4) 1 calc R . . 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
Fe1 N3 1.997(3) . ?
Fe1 N3 1.997(3) 2_656 ?
Fe1 N1 2.072(3) 2_656 ?
Fe1 N1 2.072(3) . ?
Fe1 N2 2.143(3) 2_656 ?
Fe1 N2 2.143(3) . ?
Fe2 N7 2.005(3) . ?
Fe2 N9 2.003(3) . ?
Fe2 N11 2.030(3) . ?
Fe2 C19 1.941(4) . ?
Fe2 C21 1.933(5) . ?
Fe2 C20 1.928(4) . ?
N3 C19 1.151(4) . ?
N1 C5 1.350(5) . ?
N1 C1 1.340(4) . ?
N7 N6 1.379(4) . ?
N7 C25 1.357(5) . ?
N9 N8 1.373(4) . ?
N9 C30 1.361(4) . ?
N8 C27 1.340(5) . ?
N8 B1 1.540(5) . ?
N6 C22 1.349(5) . ?
N6 B1 1.533(6) . ?
N11 N10 1.367(4) . ?
N11 C35 1.370(5) . ?
N2 C6 1.477(5) . ?
N2 C7 1.528(4) . ?
N2 C18 1.493(5) . ?
N10 C32 1.362(5) . ?
N10 B1 1.527(6) . ?
N4 C20 1.151(5) . ?
N5 C21 1.150(5) . ?
C5 C6 1.524(5) . ?
C5 C4 1.379(5) . ?
C24 H24 0.9500 . ?
C24 C25 1.385(6) . ?
C24 C22 1.366(6) . ?
C1 H1 0.9500 . ?
C1 C2 1.368(5) . ?
C31 H31A 0.9800 . ?
C31 H31B 0.9800 . ?
C31 H31C 0.9800 . ?
C31 C30 1.477(5) . ?
C27 C29 1.384(6) . ?
C27 C28 1.488(6) . ?
C25 C26 1.494(6) . ?
C29 H29 0.9500 . ?
C29 C30 1.388(5) . ?
C22 C23 1.498(6) . ?
C6 H6A 0.9900 . ?
C6 H6B 0.9900 . ?
C35 C34 1.380(6) . ?
C35 C36 1.494(7) . ?
C26 H26A 0.9800 . ?
C26 H26B 0.9800 . ?
C26 H26C 0.9800 . ?
C7 H7AA 0.9900 . ?
C7 H7AB 0.9900 . ?
C7 H7BC 0.9900 . ?
C7 H7BD 0.9900 . ?
C7 C9 1.595(8) . ?
C7 C4BA 1.518(4) . ?
C2 H2 0.9500 . ?
C2 C2AA 1.370(6) . ?
C4 H4 0.9500 . ?
C4 C2AA 1.394(6) . ?
C2AA H2AA 0.9500 . ?
C34 H34 0.9500 . ?
C34 C32 1.366(7) . ?
C32 C33 1.498(7) . ?
C18 C18 1.519(8) 2_656 ?
C18 H18A 0.9900 . ?
C18 H18B 0.9900 . ?
C23 H23A 0.9800 . ?
C23 H23B 0.9800 . ?
C23 H23C 0.9800 . ?
C28 H28A 0.9800 . ?
C28 H28B 0.9800 . ?
C28 H28C 0.9800 . ?
C8 H8 0.9500 . ?
C8 C9 1.3900 . ?
C8 C17 1.3900 . ?
C9 C10 1.3900 . ?
C10 H10 0.9500 . ?
C10 C15 1.3900 . ?
C15 H15 0.9500 . ?
C15 C16 1.3900 . ?
C16 C17 1.3900 . ?
C16 C12 1.3900 . ?
C17 C11 1.3900 . ?
C11 H11 0.9500 . ?
C11 C13 1.3900 . ?
C13 H13 0.9500 . ?
C13 C14 1.3900 . ?
C14 H14 0.9500 . ?
C14 C12 1.3900 . ?
C12 H12 0.9500 . ?
C36 H36A 0.9800 . ?
C36 H36B 0.9800 . ?
C36 H36C 0.9800 . ?
C33 H33A 0.9800 . ?
C33 H33B 0.9800 . ?
C33 H33C 0.9800 . ?
B1 H1A 1.0000 . ?
C7AA H7AC 0.9500 . ?
C7AA C2BA 1.3900 . ?
C7AA C0BA 1.3900 . ?
C2BA H2BA 0.9500 . ?
C2BA C1BA 1.3900 . ?
C1BA H1BA 0.9500 . ?
C1BA C5AA 1.3900 . ?
C5AA H5AA 0.9500 . ?
C5AA C4AA 1.3900 . ?
C4AA C0BA 1.3900 . ?
C4AA C3BA 1.3900 . ?
C0BA C3 1.3900 . ?
C3 H3 0.9500 . ?
C3 C4BA 1.3900 . ?
C4BA C9AA 1.3900 . ?
C9AA H9AA 0.9500 . ?
C9AA C3BA 1.3900 . ?
C3BA H3BA 0.9500 . ?

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
N3 Fe1 N3 90.54(17) . 2_656 ?
N3 Fe1 N1 91.09(12) 2_656 . ?
N3 Fe1 N1 93.01(12) 2_656 2_656 ?
N3 Fe1 N1 93.01(12) . . ?
N3 Fe1 N1 91.09(12) . 2_656 ?
N3 Fe1 N2 171.19(11) 2_656 2_656 ?
N3 Fe1 N2 92.89(12) 2_656 . ?
N3 Fe1 N2 171.18(11) . . ?
N3 Fe1 N2 92.89(12) . 2_656 ?
N1 Fe1 N1 174.18(18) . 2_656 ?
N1 Fe1 N2 96.83(11) . 2_656 ?
N1 Fe1 N2 96.84(12) 2_656 . ?
N1 Fe1 N2 78.82(12) . . ?
N1 Fe1 N2 78.82(12) 2_656 2_656 ?
N2 Fe1 N2 84.90(17) 2_656 . ?
N7 Fe2 N11 90.45(13) . . ?
N9 Fe2 N7 87.30(13) . . ?
N9 Fe2 N11 89.58(13) . . ?
C19 Fe2 N7 94.80(14) . . ?
C19 Fe2 N9 95.11(13) . . ?
C19 Fe2 N11 173.11(15) . . ?
C21 Fe2 N7 178.94(15) . . ?
C21 Fe2 N9 92.05(15) . . ?
C21 Fe2 N11 90.38(15) . . ?
C21 Fe2 C19 84.43(16) . . ?
C20 Fe2 N7 90.30(16) . . ?
C20 Fe2 N9 177.57(16) . . ?
C20 Fe2 N11 90.84(15) . . ?
C20 Fe2 C19 84.69(16) . . ?
C20 Fe2 C21 90.34(17) . . ?
C19 N3 Fe1 175.3(3) . . ?
C5 N1 Fe1 114.5(2) . . ?
C1 N1 Fe1 127.0(3) . . ?
C1 N1 C5 118.5(3) . . ?
N6 N7 Fe2 117.6(2) . . ?
C25 N7 Fe2 136.3(3) . . ?
C25 N7 N6 106.1(3) . . ?
N8 N9 Fe2 118.0(2) . . ?
C30 N9 Fe2 134.7(3) . . ?
C30 N9 N8 107.3(3) . . ?
N9 N8 B1 118.2(3) . . ?
C27 N8 N9 110.0(3) . . ?
C27 N8 B1 131.4(4) . . ?
N7 N6 B1 118.6(3) . . ?
C22 N6 N7 110.1(3) . . ?
C22 N6 B1 131.2(4) . . ?
N10 N11 Fe2 117.7(2) . . ?
N10 N11 C35 107.0(3) . . ?
C35 N11 Fe2 135.3(3) . . ?
C6 N2 Fe1 106.6(2) . . ?
C6 N2 C7 108.9(3) . . ?
C6 N2 C18 109.9(3) . . ?
C7 N2 Fe1 114.4(2) . . ?
C18 N2 Fe1 104.8(2) . . ?
C18 N2 C7 112.0(3) . . ?
N11 N10 B1 118.3(3) . . ?
C32 N10 N11 108.8(4) . . ?
C32 N10 B1 132.9(4) . . ?
N3 C19 Fe2 172.3(3) . . ?
N1 C5 C6 116.3(3) . . ?
N1 C5 C4 121.9(4) . . ?
C4 C5 C6 121.9(4) . . ?
C25 C24 H24 126.2 . . ?
C22 C24 H24 126.2 . . ?
C22 C24 C25 107.6(4) . . ?
N1 C1 H1 118.6 . . ?
N1 C1 C2 122.9(4) . . ?
C2 C1 H1 118.6 . . ?
H31A C31 H31B 109.5 . . ?
H31A C31 H31C 109.5 . . ?
H31B C31 H31C 109.5 . . ?
C30 C31 H31A 109.5 . . ?
C30 C31 H31B 109.5 . . ?
C30 C31 H31C 109.5 . . ?
N8 C27 C29 107.3(4) . . ?
N8 C27 C28 122.6(4) . . ?
C29 C27 C28 130.1(4) . . ?
N7 C25 C24 108.9(4) . . ?
N7 C25 C26 124.0(4) . . ?
C24 C25 C26 127.1(4) . . ?
C27 C29 H29 126.2 . . ?
C27 C29 C30 107.6(3) . . ?
C30 C29 H29 126.2 . . ?
N9 C30 C31 124.7(3) . . ?
N9 C30 C29 107.8(4) . . ?
C29 C30 C31 127.5(3) . . ?
N5 C21 Fe2 178.1(4) . . ?
N6 C22 C24 107.3(4) . . ?
N6 C22 C23 122.2(4) . . ?
C24 C22 C23 130.5(4) . . ?
N2 C6 C5 108.5(3) . . ?
N2 C6 H6A 110.0 . . ?
N2 C6 H6B 110.0 . . ?
C5 C6 H6A 110.0 . . ?
C5 C6 H6B 110.0 . . ?
H6A C6 H6B 108.4 . . ?
N11 C35 C34 108.8(4) . . ?
N11 C35 C36 123.6(4) . . ?
C34 C35 C36 127.6(4) . . ?
C25 C26 H26A 109.5 . . ?
C25 C26 H26B 109.5 . . ?
C25 C26 H26C 109.5 . . ?
H26A C26 H26B 109.5 . . ?
H26A C26 H26C 109.5 . . ?
H26B C26 H26C 109.5 . . ?
N2 C7 H7AA 108.5 . . ?
N2 C7 H7AB 108.5 . . ?
N2 C7 H7BC 108.0 . . ?
N2 C7 H7BD 108.0 . . ?
N2 C7 C9 115.1(6) . . ?
H7AA C7 H7AB 107.5 . . ?
H7BC C7 H7BD 107.3 . . ?
C9 C7 H7AA 108.5 . . ?
C9 C7 H7AB 108.5 . . ?
C4BA C7 N2 117.1(3) . . ?
C4BA C7 H7BC 108.0 . . ?
C4BA C7 H7BD 108.0 . . ?
C1 C2 H2 120.6 . . ?
C1 C2 C2AA 118.8(4) . . ?
C2AA C2 H2 120.6 . . ?
C5 C4 H4 120.8 . . ?
C5 C4 C2AA 118.5(4) . . ?
C2AA C4 H4 120.8 . . ?
C2 C2AA C4 119.6(4) . . ?
C2 C2AA H2AA 120.2 . . ?
C4 C2AA H2AA 120.2 . . ?
N4 C20 Fe2 178.0(4) . . ?
C35 C34 H34 126.5 . . ?
C32 C34 C35 106.9(4) . . ?
C32 C34 H34 126.5 . . ?
N10 C32 C34 108.5(4) . . ?
N10 C32 C33 121.9(5) . . ?
C34 C32 C33 129.6(4) . . ?
N2 C18 C18 110.4(2) . 2_656 ?
N2 C18 H18A 109.6 . . ?
N2 C18 H18B 109.6 . . ?
C18 C18 H18A 109.6 2_656 . ?
C18 C18 H18B 109.6 2_656 . ?
H18A C18 H18B 108.1 . . ?
C22 C23 H23A 109.5 . . ?
C22 C23 H23B 109.5 . . ?
C22 C23 H23C 109.5 . . ?
H23A C23 H23B 109.5 . . ?
H23A C23 H23C 109.5 . . ?
H23B C23 H23C 109.5 . . ?
C27 C28 H28A 109.5 . . ?
C27 C28 H28B 109.5 . . ?
C27 C28 H28C 109.5 . . ?
H28A C28 H28B 109.5 . . ?
H28A C28 H28C 109.5 . . ?
H28B C28 H28C 109.5 . . ?
C9 C8 H8 120.0 . . ?
C9 C8 C17 120.0 . . ?
C17 C8 H8 120.0 . . ?
C8 C9 C7 116.9(6) . . ?
C8 C9 C10 120.0 . . ?
C10 C9 C7 123.1(6) . . ?
C9 C10 H10 120.0 . . ?
C15 C10 C9 120.0 . . ?
C15 C10 H10 120.0 . . ?
C10 C15 H15 120.0 . . ?
C10 C15 C16 120.0 . . ?
C16 C15 H15 120.0 . . ?
C15 C16 C12 120.0 . . ?
C17 C16 C15 120.0 . . ?
C17 C16 C12 120.0 . . ?
C16 C17 C8 120.0 . . ?
C16 C17 C11 120.0 . . ?
C11 C17 C8 120.0 . . ?
C17 C11 H11 120.0 . . ?
C13 C11 C17 120.0 . . ?
C13 C11 H11 120.0 . . ?
C11 C13 H13 120.0 . . ?
C14 C13 C11 120.0 . . ?
C14 C13 H13 120.0 . . ?
C13 C14 H14 120.0 . . ?
C13 C14 C12 120.0 . . ?
C12 C14 H14 120.0 . . ?
C16 C12 H12 120.0 . . ?
C14 C12 C16 120.0 . . ?
C14 C12 H12 120.0 . . ?
C35 C36 H36A 109.5 . . ?
C35 C36 H36B 109.5 . . ?
C35 C36 H36C 109.5 . . ?
H36A C36 H36B 109.5 . . ?
H36A C36 H36C 109.5 . . ?
H36B C36 H36C 109.5 . . ?
C32 C33 H33A 109.5 . . ?
C32 C33 H33B 109.5 . . ?
C32 C33 H33C 109.5 . . ?
H33A C33 H33B 109.5 . . ?
H33A C33 H33C 109.5 . . ?
H33B C33 H33C 109.5 . . ?
N8 B1 H1A 110.3 . . ?
N6 B1 N8 107.3(3) . . ?
N6 B1 H1A 110.3 . . ?
N10 B1 N8 109.2(4) . . ?
N10 B1 N6 109.4(3) . . ?
N10 B1 H1A 110.3 . . ?
C2BA C7AA H7AC 120.0 . . ?
C2BA C7AA C0BA 120.0 . . ?
C0BA C7AA H7AC 120.0 . . ?
C7AA C2BA H2BA 120.0 . . ?
C1BA C2BA C7AA 120.0 . . ?
C1BA C2BA H2BA 120.0 . . ?
C2BA C1BA H1BA 120.0 . . ?
C2BA C1BA C5AA 120.0 . . ?
C5AA C1BA H1BA 120.0 . . ?
C1BA C5AA H5AA 120.0 . . ?
C4AA C5AA C1BA 120.0 . . ?
C4AA C5AA H5AA 120.0 . . ?
C5AA C4AA C0BA 120.0 . . ?
C5AA C4AA C3BA 120.0 . . ?
C0BA C4AA C3BA 120.0 . . ?
C4AA C0BA C7AA 120.0 . . ?
C3 C0BA C7AA 120.0 . . ?
C3 C0BA C4AA 120.0 . . ?
C0BA C3 H3 120.0 . . ?
C0BA C3 C4BA 120.0 . . ?
C4BA C3 H3 120.0 . . ?
C3 C4BA C7 117.4(3) . . ?
C9AA C4BA C7 122.6(3) . . ?
C9AA C4BA C3 120.0 . . ?
C4BA C9AA H9AA 120.0 . . ?
C3BA C9AA C4BA 120.0 . . ?
C3BA C9AA H9AA 120.0 . . ?
C4AA C3BA H3BA 120.0 . . ?
C9AA C3BA C4AA 120.0 . . ?
C9AA C3BA H3BA 120.0 . . ?

_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 -0.797 -0.648 -0.554 3865.3 765.1 3CH3OH,4H2O

_olex2_submission_special_instructions 'No special instructions were received'
####################################################################### 
# 
# 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_Tp3Me_300K
_database_code_depnum_ccdc_archive 'CCDC 1974450'
loop_
_audit_author_name
_audit_author_address
'Xin-Hua Zhao'
;Southern University of Science and Technology
China
;
_audit_update_record             
;
2020-03-27 deposited with the CCDC.	2020-04-01 downloaded from the CCDC.
;
_audit_creation_date             2020-03-17
_audit_creation_method           
;
Olex2 1.2
(compiled 2018.05.29 svn.r3508 for OlexSys, GUI svn.r5506)
;
_shelx_SHELXL_version_number     2014/7
_chemical_name_common            ?
_chemical_name_systematic        ?
_chemical_formula_moiety         'C66 H66 B2 Fe3 N22, 3[CH3OH], 2[CH2Cl2]'
_chemical_formula_sum            'C71 H82 B2 Cl4 Fe3 N22 O3'
_chemical_formula_weight         1622.55
_chemical_melting_point          ?
loop_
_atom_type_symbol
_atom_type_description
_atom_type_scat_dispersion_real
_atom_type_scat_dispersion_imag
_atom_type_scat_source
B B 0.0013 0.0007 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Cl Cl 0.1484 0.1585 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Fe Fe 0.3463 0.8444 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'

_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      monoclinic
_space_group_IT_number           15
_space_group_name_H-M_alt        'C 1 2/c 1'
_space_group_name_Hall           '-C 2yc'
loop_
_space_group_symop_operation_xyz
'x, y, z'
'-x, y, -z+1/2'
'x+1/2, y+1/2, z'
'-x+1/2, y+1/2, -z+1/2'
'-x, -y, -z'
'x, -y, z-1/2'
'-x+1/2, -y+1/2, -z'
'x+1/2, -y+1/2, z-1/2'

_cell_length_a                   18.936(6)
_cell_length_b                   20.261(6)
_cell_length_c                   23.361(5)
_cell_angle_alpha                90
_cell_angle_beta                 113.627(9)
_cell_angle_gamma                90
_cell_volume                     8211(4)
_cell_formula_units_Z            4
_cell_measurement_reflns_used    7054
_cell_measurement_temperature    300(2)
_cell_measurement_theta_max      24.563
_cell_measurement_theta_min      2.348
_shelx_estimated_absorpt_T_max   ?
_shelx_estimated_absorpt_T_min   ?
_exptl_absorpt_coefficient_mu    0.711
_exptl_absorpt_correction_T_max  0.7451
_exptl_absorpt_correction_T_min  0.6321
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   
'SADABS-2016/2 (Bruker,2016/2) was used for absorption correction. wR2(int) was 0.1565 before and 0.0737 after correction. The Ratio of minimum to maximum transmission is 0.8483. The λ/2 correction factor is Not present.'
_exptl_absorpt_special_details   ?
_exptl_crystal_colour            'dark red'
_exptl_crystal_colour_modifier   dark
_exptl_crystal_colour_primary    red
_exptl_crystal_density_diffrn    1.312
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    ?
_exptl_crystal_description       block
_exptl_crystal_F_000             3368
_exptl_crystal_size_max          0.2
_exptl_crystal_size_mid          0.15
_exptl_crystal_size_min          0.12
_exptl_transmission_factor_max   ?
_exptl_transmission_factor_min   ?
_diffrn_reflns_av_R_equivalents  0.0933
_diffrn_reflns_av_unetI/netI     0.0825
_diffrn_reflns_Laue_measured_fraction_full 0.994
_diffrn_reflns_Laue_measured_fraction_max 0.994
_diffrn_reflns_limit_h_max       22
_diffrn_reflns_limit_h_min       -22
_diffrn_reflns_limit_k_max       20
_diffrn_reflns_limit_k_min       -23
_diffrn_reflns_limit_l_max       27
_diffrn_reflns_limit_l_min       -25
_diffrn_reflns_number            25887
_diffrn_reflns_point_group_measured_fraction_full 0.994
_diffrn_reflns_point_group_measured_fraction_max 0.994
_diffrn_reflns_theta_full        24.792
_diffrn_reflns_theta_max         24.792
_diffrn_reflns_theta_min         2.224
_diffrn_ambient_temperature      300.02
_diffrn_detector_area_resol_mean ?
_diffrn_measured_fraction_theta_full 0.994
_diffrn_measured_fraction_theta_max 0.994
_diffrn_measurement_device_type  'Bruker APEX-II CCD'
_diffrn_measurement_method       'φ and ω scans'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_source                   ?
_diffrn_standards_number         0
_reflns_Friedel_coverage         0.000
_reflns_Friedel_fraction_full    .
_reflns_Friedel_fraction_max     .
_reflns_number_gt                4840
_reflns_number_total             7032
_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       'SAINT V8.38A (?, 2016)'
_computing_data_collection       'Bruker APEX3'
_computing_data_reduction        'SAINT V8.38A (?, 2016)'
_computing_molecular_graphics    'Olex2 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 (Dolomanov et al., 2009)'
_computing_structure_refinement  'XL (Sheldrick, 2008)'
_computing_structure_solution    'ShelXT (Sheldrick, 2015)'
_refine_diff_density_max         0.554
_refine_diff_density_min         -0.610
_refine_diff_density_rms         0.075
_refine_ls_extinction_coef       .
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.034
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     470
_refine_ls_number_reflns         7032
_refine_ls_number_restraints     83
_refine_ls_R_factor_all          0.1053
_refine_ls_R_factor_gt           0.0704
_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)+(0.0937P)²+16.2862P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1792
_refine_ls_wR_factor_ref         0.1948
_refine_special_details          ?
_olex2_refinement_description    
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups, All C(H,H) groups, All C(H,H,H,H) groups
 At 1.5 times of:
  All C(H,H,H) groups
2. Rigid bond restraints
 C11, C16, C17, C8, C9, C10
 with sigma for 1-2 distances of 0.02 and sigma for 1-3 distances of 0.02
 C14, C13, C12, C11, C16, C15
 with sigma for 1-2 distances of 0.02 and sigma for 1-3 distances of 0.02
3. Uiso/Uaniso restraints and constraints
Uanis(C11) \\sim Ueq, Uanis(C16) \\sim Ueq, Uanis(C17) \\sim Ueq, Uanis(C8)
\\sim Ueq, Uanis(C9) \\sim Ueq, Uanis(C10) \\sim Ueq: with sigma of 0.02 and
sigma for terminal atoms of 0.04
Uanis(C14) \\sim Ueq, Uanis(C13) \\sim Ueq, Uanis(C12) \\sim Ueq, Uanis(C11)
\\sim Ueq, Uanis(C16) \\sim Ueq, Uanis(C15) \\sim Ueq: with sigma of 0.02 and
sigma for terminal atoms of 0.04
4. Others
 Sof(H7BC)=Sof(H7BD)=Sof(C17)=Sof(H17)=Sof(C8)=Sof(C9)=Sof(H9)=Sof(C10)=
 Sof(H10)=Sof(C11)=Sof(C16)=Sof(C15)=Sof(H15)=Sof(C14)=Sof(H14)=Sof(C13)=
 Sof(H13)=Sof(C12)=Sof(H12)=1-FVAR(1)
 Sof(H7AA)=Sof(H7AB)=Sof(C9A)=Sof(H9A)=Sof(C8A)=Sof(C17A)=Sof(H17A)=Sof(C16A)=
 Sof(H16A)=Sof(C15A)=Sof(C10A)=Sof(C11A)=Sof(H11A)=Sof(C12A)=Sof(H12A)=
 Sof(C13A)=Sof(H13A)=Sof(C14A)=Sof(H14A)=FVAR(1)
5.a Secondary CH2 refined with riding coordinates:
 C6(H6A,H6B), C18(H18A,H18B), C7(H7AA,H7AB), C7(H7BC,H7BD)
5.b Aromatic/amide H refined with riding coordinates:
 C1(H1), C2(H2), C4(H4), C22(H22), C3(H3), C23(H23), C30(H30), C26(H26),
 C31(H31), C27(H27), C9A(H9A), C17A(H17A), C16A(H16A), C11A(H11A), C12A(H12A),
 C13A(H13A), C14A(H14A), C17(H17), C9(H9), C10(H10), C15(H15), C14(H14),
 C13(H13), C12(H12)
5.c Naphthalene refined as free rotating group:
 C9A(C8A,C17A,C16A,C15A,C10A,C11A,C12A,C13A,C14A), C17(C8,C9,C10,C11,C16,C15,
 C14,C13,C12)
5.d Idealised Me refined as rotating group:
 C25(H25A,H25B,H25C), C33(H33A,H33B,H33C), C29(H29A,H29B,H29C)
;
_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
Fe1 Fe 0.5000 0.56567(4) 0.7500 0.0384(2) Uani 1 2 d S T P . .
Fe2 Fe 0.31860(4) 0.38714(3) 0.63095(3) 0.0513(2) Uani 1 1 d . . . . .
N3 N 0.42712(19) 0.49728(17) 0.70584(15) 0.0410(8) Uani 1 1 d . . . . .
N1 N 0.5460(2) 0.56807(16) 0.68712(14) 0.0449(9) Uani 1 1 d . . . . .
N11 N 0.4021(2) 0.31938(19) 0.64927(17) 0.0577(10) Uani 1 1 d . . . . .
N10 N 0.3846(3) 0.2549(2) 0.65881(18) 0.0657(12) Uani 1 1 d . . . . .
N2 N 0.5800(2) 0.63897(18) 0.78848(15) 0.0561(10) Uani 1 1 d . . . . .
N9 N 0.2413(2) 0.3235(2) 0.57295(18) 0.0647(11) Uani 1 1 d . . . . .
N7 N 0.2947(2) 0.3487(2) 0.70156(17) 0.0672(12) Uani 1 1 d . . . . .
C24 C 0.4754(3) 0.3182(2) 0.6551(2) 0.0585(13) Uani 1 1 d . . . . .
C1 C 0.5167(3) 0.5418(2) 0.62892(18) 0.0504(11) Uani 1 1 d . . . . .
H1 H 0.4680 0.5227 0.6139 0.061 Uiso 1 1 calc R . . . .
N6 N 0.2929(3) 0.2808(2) 0.70477(19) 0.0760(14) Uani 1 1 d . . . . .
N8 N 0.2444(3) 0.2597(2) 0.59182(19) 0.0737(13) Uani 1 1 d . . . . .
C19 C 0.3883(2) 0.4536(2) 0.68101(19) 0.0454(10) Uani 1 1 d . . . . .
C25 C 0.5178(3) 0.3752(3) 0.6486(3) 0.0706(15) Uani 1 1 d . . . . .
H25A H 0.4877 0.3980 0.6105 0.106 Uiso 1 1 calc GR . . . .
H25B H 0.5656 0.3610 0.6474 0.106 Uiso 1 1 calc GR . . . .
H25C H 0.5281 0.4043 0.6834 0.106 Uiso 1 1 calc GR . . . .
N4 N 0.3576(3) 0.4443(2) 0.5259(2) 0.0770(13) Uani 1 1 d . . . . .
C2 C 0.5578(3) 0.5426(3) 0.5911(2) 0.0635(13) Uani 1 1 d . . . . .
H2 H 0.5367 0.5242 0.5513 0.076 Uiso 1 1 calc R . . . .
C5 C 0.6153(3) 0.5964(2) 0.7066(2) 0.0582(13) Uani 1 1 d . . . . .
C4 C 0.6584(4) 0.5987(3) 0.6705(3) 0.0817(18) Uani 1 1 d . . . . .
H4 H 0.7064 0.6191 0.6856 0.098 Uiso 1 1 calc R . . . .
C20 C 0.3417(3) 0.4223(2) 0.5642(2) 0.0546(12) Uani 1 1 d . . . . .
C22 C 0.4472(4) 0.2166(3) 0.6696(2) 0.0791(17) Uani 1 1 d . . . . .
H22 H 0.4500 0.1714 0.6770 0.095 Uiso 1 1 calc R . . . .
C3 C 0.6288(4) 0.5706(3) 0.6126(3) 0.0811(18) Uani 1 1 d . . . . .
H3 H 0.6572 0.5707 0.5880 0.097 Uiso 1 1 calc R . . . .
C32 C 0.1843(3) 0.3273(3) 0.5156(2) 0.0779(17) Uani 1 1 d . . . . .
C23 C 0.5038(4) 0.2536(3) 0.6681(2) 0.0764(16) Uani 1 1 d . . . . .
H23 H 0.5531 0.2395 0.6744 0.092 Uiso 1 1 calc R . . . .
C21 C 0.2427(3) 0.4550(3) 0.6157(2) 0.0738(16) Uani 1 1 d . . . . .
C6 C 0.6457(3) 0.6212(3) 0.7725(2) 0.0706(16) Uani 1 1 d . . . . .
H6A H 0.6767 0.5873 0.8007 0.085 Uiso 1 1 calc R . . . .
H6B H 0.6781 0.6596 0.7767 0.085 Uiso 1 1 calc R . . . .
C28 C 0.2825(3) 0.3719(3) 0.7501(2) 0.0759(17) Uani 1 1 d . . . . .
C18 C 0.5412(4) 0.7008(2) 0.7545(2) 0.083(2) Uani 1 1 d . . . . .
H18A H 0.5670 0.7393 0.7784 0.100 Uiso 1 1 calc R . . . .
H18B H 0.5446 0.7028 0.7142 0.100 Uiso 1 1 calc R . . . .
N5 N 0.1987(3) 0.4972(4) 0.6091(3) 0.116(2) Uani 1 1 d . . . . .
C33 C 0.1623(4) 0.3888(4) 0.4782(3) 0.102(2) Uani 1 1 d . . . . .
H33A H 0.1540 0.4234 0.5030 0.153 Uiso 1 1 calc GR . . . .
H33B H 0.1157 0.3815 0.4418 0.153 Uiso 1 1 calc GR . . . .
H33C H 0.2028 0.4014 0.4657 0.153 Uiso 1 1 calc GR . . . .
C29 C 0.2819(4) 0.4443(4) 0.7634(3) 0.098(2) Uani 1 1 d . . . . .
H29A H 0.3325 0.4622 0.7737 0.148 Uiso 1 1 calc GR . . . .
H29B H 0.2673 0.4506 0.7979 0.148 Uiso 1 1 calc GR . . . .
H29C H 0.2457 0.4663 0.7271 0.148 Uiso 1 1 calc GR . . . .
C30 C 0.1906(4) 0.2250(3) 0.5475(3) 0.087(2) Uani 1 1 d . . . . .
H30 H 0.1810 0.1802 0.5495 0.105 Uiso 1 1 calc R . . . .
C26 C 0.2803(4) 0.2634(4) 0.7546(3) 0.090(2) Uani 1 1 d . . . . .
H26 H 0.2778 0.2205 0.7677 0.107 Uiso 1 1 calc R . . . .
C31 C 0.1525(4) 0.2651(4) 0.4996(3) 0.094(2) Uani 1 1 d . . . . .
H31 H 0.1122 0.2533 0.4623 0.113 Uiso 1 1 calc R . . . .
C27 C 0.2717(4) 0.3194(5) 0.7831(3) 0.106(3) Uani 1 1 d . . . . .
H27 H 0.2605 0.3218 0.8183 0.127 Uiso 1 1 calc R . . . .
B1 B 0.3059(4) 0.2391(4) 0.6559(3) 0.076(2) Uani 1 1 d . . . . .
C7 C 0.6085(3) 0.6478(2) 0.85872(19) 0.0634(14) Uani 1 1 d . . . . .
H7AA H 0.6205 0.6045 0.8780 0.076 Uiso 0.621(9) 1 calc R . . A 1
H7AB H 0.5665 0.6657 0.8677 0.076 Uiso 0.621(9) 1 calc R . . A 1
H7BC H 0.5640 0.6516 0.8692 0.076 Uiso 0.379(9) 1 calc R . . A 2
H7BD H 0.6361 0.6082 0.8788 0.076 Uiso 0.379(9) 1 calc R . . A 2
C9A C 0.6652(4) 0.7584(4) 0.8994(4) 0.080(4) Uani 0.621(9) 1 d . . . A 1
H9A H 0.6146 0.7725 0.8880 0.096 Uiso 0.621(9) 1 calc R . . A 1
C8A C 0.6803(5) 0.6929(3) 0.8908(5) 0.075(5) Uani 0.621(9) 1 d G . . A 1
C17A C 0.7559(5) 0.6718(3) 0.9079(4) 0.091(4) Uani 0.621(9) 1 d G . . A 1
H17A H 0.7660 0.6279 0.9021 0.110 Uiso 0.621(9) 1 calc R . . A 1
C16A C 0.8164(4) 0.7162(3) 0.9337(4) 0.106(5) Uani 0.621(9) 1 d G . . A 1
H16A H 0.8669 0.7021 0.9451 0.127 Uiso 0.621(9) 1 calc R . . A 1
C15A C 0.8013(3) 0.7817(3) 0.9423(2) 0.085(4) Uani 0.621(9) 1 d G . . A 1
C10A C 0.7257(4) 0.8029(3) 0.9252(3) 0.086(4) Uani 0.621(9) 1 d G . . A 1
C11A C 0.7106(5) 0.8684(3) 0.9338(3) 0.109(5) Uani 0.621(9) 1 d G . . A 1
H11A H 0.6601 0.8825 0.9224 0.131 Uiso 0.621(9) 1 calc R . . A 1
C12A C 0.7711(6) 0.9128(3) 0.9595(3) 0.131(6) Uani 0.621(9) 1 d G . . A 1
H12A H 0.7610 0.9567 0.9653 0.157 Uiso 0.621(9) 1 calc R . . A 1
C13A C 0.8467(5) 0.8917(4) 0.9767(4) 0.109(5) Uani 0.621(9) 1 d G . . A 1
H13A H 0.8871 0.9215 0.9939 0.131 Uiso 0.621(9) 1 calc R . . A 1
C14A C 0.8618(4) 0.8262(4) 0.9680(3) 0.114(5) Uani 0.621(9) 1 d G . . A 1
H14A H 0.9123 0.8121 0.9795 0.137 Uiso 0.621(9) 1 calc R . . A 1
C17 C 0.7392(7) 0.6957(5) 0.9052(8) 0.083(6) Uani 0.379(9) 1 d . U . A 2
H17 H 0.7570 0.6540 0.9009 0.099 Uiso 0.379(9) 1 calc R . . A 2
C8 C 0.6606(7) 0.7067(7) 0.8863(9) 0.067(6) Uani 0.379(9) 1 d G U . A 2
C9 C 0.6340(6) 0.7690(8) 0.8927(9) 0.083(6) Uani 0.379(9) 1 d G U . A 2
H9 H 0.5814 0.7764 0.8800 0.099 Uiso 0.379(9) 1 calc R . . A 2
C10 C 0.6859(6) 0.8203(6) 0.9181(7) 0.105(7) Uani 0.379(9) 1 d G U . A 2
H10 H 0.6681 0.8620 0.9224 0.126 Uiso 0.379(9) 1 calc R . . A 2
C11 C 0.7645(6) 0.8093(5) 0.9371(5) 0.098(6) Uani 0.379(9) 1 d G U . A 2
C16 C 0.7911(6) 0.7470(5) 0.9306(5) 0.103(7) Uani 0.379(9) 1 d G U . A 2
C15 C 0.8697(6) 0.7360(7) 0.9496(6) 0.114(6) Uani 0.379(9) 1 d G U . A 2
H15 H 0.8875 0.6943 0.9453 0.137 Uiso 0.379(9) 1 calc R . . A 2
C14 C 0.9217(6) 0.7873(8) 0.9750(6) 0.132(8) Uani 0.379(9) 1 d G U . A 2
H14 H 0.9742 0.7799 0.9877 0.159 Uiso 0.379(9) 1 calc R . . A 2
C13 C 0.8950(7) 0.8496(7) 0.9814(6) 0.108(7) Uani 0.379(9) 1 d G U . A 2
H13 H 0.9298 0.8839 0.9984 0.129 Uiso 0.379(9) 1 calc R . . A 2
C12 C 0.8164(8) 0.8606(6) 0.9625(6) 0.114(7) Uani 0.379(9) 1 d G U . A 2
H12 H 0.7986 0.9023 0.9668 0.136 Uiso 0.379(9) 1 calc R . . A 2
H1A H 0.311(3) 0.177(3) 0.664(2) 0.078(15) Uiso 1 1 d . . . . .


_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
Fe1 N3 1.936(4) 2_656 ?
Fe1 N3 1.936(4) . ?
Fe1 N1 1.987(3) 2_656 ?
Fe1 N1 1.987(3) . ?
Fe1 N2 2.053(4) 2_656 ?
Fe1 N2 2.053(4) . ?
Fe2 N11 2.006(4) . ?
Fe2 N9 2.012(4) . ?
Fe2 N7 2.032(4) . ?
Fe2 C19 1.920(5) . ?
Fe2 C20 1.918(5) . ?
Fe2 C21 1.916(7) . ?
N3 C19 1.148(5) . ?
N1 C1 1.355(5) . ?
N1 C5 1.334(6) . ?
N11 N10 1.387(5) . ?
N11 C24 1.340(6) . ?
N10 C22 1.353(7) . ?
N10 B1 1.499(8) . ?
N2 C6 1.481(7) . ?
N2 C18 1.507(6) . ?
N2 C7 1.519(5) . ?
N9 N8 1.359(6) . ?
N9 C32 1.344(6) . ?
N7 N6 1.380(6) . ?
N7 C28 1.331(7) . ?
C24 C25 1.448(7) . ?
C24 C23 1.402(7) . ?
C1 C2 1.391(7) . ?
N6 C26 1.326(7) . ?
N6 B1 1.517(9) . ?
N8 C30 1.326(6) . ?
N8 B1 1.541(7) . ?
N4 C20 1.142(6) . ?
C2 C3 1.358(8) . ?
C5 C4 1.388(7) . ?
C5 C6 1.498(6) . ?
C4 C3 1.365(7) . ?
C22 C23 1.320(8) . ?
C32 C33 1.483(9) . ?
C32 C31 1.382(8) . ?
C21 N5 1.161(8) . ?
C28 C29 1.500(9) . ?
C28 C27 1.375(9) . ?
C18 C18 1.490(13) 2_656 ?
C30 C31 1.337(9) . ?
C26 C27 1.357(10) . ?
C7 C8A 1.558(7) . ?
C7 C8 1.517(10) . ?
C9A C8A 1.3900 . ?
C9A C10A 1.3900 . ?
C8A C17A 1.3900 . ?
C17A C16A 1.3900 . ?
C16A C15A 1.3900 . ?
C15A C10A 1.3900 . ?
C15A C14A 1.3900 . ?
C10A C11A 1.3900 . ?
C11A C12A 1.3900 . ?
C12A C13A 1.3900 . ?
C13A C14A 1.3900 . ?
C17 C8 1.3900 . ?
C17 C16 1.3900 . ?
C8 C9 1.3900 . ?
C9 C10 1.3900 . ?
C10 C11 1.3900 . ?
C11 C16 1.3900 . ?
C11 C12 1.3900 . ?
C16 C15 1.3900 . ?
C15 C14 1.3900 . ?
C14 C13 1.3900 . ?
C13 C12 1.3900 . ?

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
N3 Fe1 N3 88.6(2) 2_656 . ?
N3 Fe1 N1 93.10(14) . . ?
N3 Fe1 N1 88.92(14) . 2_656 ?
N3 Fe1 N1 88.92(14) 2_656 . ?
N3 Fe1 N1 93.09(14) 2_656 2_656 ?
N3 Fe1 N2 173.83(14) . . ?
N3 Fe1 N2 92.37(15) . 2_656 ?
N3 Fe1 N2 173.83(14) 2_656 2_656 ?
N3 Fe1 N2 92.37(15) 2_656 . ?
N1 Fe1 N1 177.2(2) . 2_656 ?
N1 Fe1 N2 80.83(14) 2_656 2_656 ?
N1 Fe1 N2 97.11(15) . 2_656 ?
N1 Fe1 N2 97.11(15) 2_656 . ?
N1 Fe1 N2 80.83(14) . . ?
N2 Fe1 N2 87.3(2) . 2_656 ?
N11 Fe2 N9 90.18(17) . . ?
N11 Fe2 N7 88.71(18) . . ?
N9 Fe2 N7 87.86(17) . . ?
C19 Fe2 N11 93.40(17) . . ?
C19 Fe2 N9 175.12(18) . . ?
C19 Fe2 N7 95.54(17) . . ?
C20 Fe2 N11 90.61(19) . . ?
C20 Fe2 N9 91.82(18) . . ?
C20 Fe2 N7 179.2(2) . . ?
C20 Fe2 C19 84.82(18) . . ?
C21 Fe2 N11 177.2(2) . . ?
C21 Fe2 N9 92.6(2) . . ?
C21 Fe2 N7 91.8(2) . . ?
C21 Fe2 C19 83.8(2) . . ?
C21 Fe2 C20 88.9(2) . . ?
C19 N3 Fe1 175.0(3) . . ?
C1 N1 Fe1 127.4(3) . . ?
C5 N1 Fe1 115.0(3) . . ?
C5 N1 C1 117.5(4) . . ?
N10 N11 Fe2 117.4(3) . . ?
C24 N11 Fe2 136.8(3) . . ?
C24 N11 N10 105.8(4) . . ?
N11 N10 B1 119.4(5) . . ?
C22 N10 N11 108.8(5) . . ?
C22 N10 B1 131.8(5) . . ?
C6 N2 Fe1 105.1(3) . . ?
C6 N2 C18 110.5(4) . . ?
C6 N2 C7 109.3(4) . . ?
C18 N2 Fe1 104.6(3) . . ?
C18 N2 C7 111.0(4) . . ?
C7 N2 Fe1 116.0(3) . . ?
N8 N9 Fe2 117.8(3) . . ?
C32 N9 Fe2 135.3(4) . . ?
C32 N9 N8 106.9(4) . . ?
N6 N7 Fe2 116.4(3) . . ?
C28 N7 Fe2 136.8(4) . . ?
C28 N7 N6 106.8(5) . . ?
N11 C24 C25 124.8(5) . . ?
N11 C24 C23 109.2(5) . . ?
C23 C24 C25 125.9(5) . . ?
N1 C1 C2 121.6(4) . . ?
N7 N6 B1 119.9(4) . . ?
C26 N6 N7 109.2(5) . . ?
C26 N6 B1 130.9(6) . . ?
N9 N8 B1 119.3(4) . . ?
C30 N8 N9 109.4(4) . . ?
C30 N8 B1 131.3(5) . . ?
N3 C19 Fe2 173.2(4) . . ?
C3 C2 C1 119.6(4) . . ?
N1 C5 C4 123.0(4) . . ?
N1 C5 C6 114.5(4) . . ?
C4 C5 C6 122.3(5) . . ?
C3 C4 C5 118.7(5) . . ?
N4 C20 Fe2 177.6(4) . . ?
C23 C22 N10 109.2(5) . . ?
C2 C3 C4 119.5(5) . . ?
N9 C32 C33 124.0(5) . . ?
N9 C32 C31 107.8(6) . . ?
C31 C32 C33 128.2(5) . . ?
C22 C23 C24 107.0(6) . . ?
N5 C21 Fe2 176.9(5) . . ?
N2 C6 C5 109.0(4) . . ?
N7 C28 C29 122.6(6) . . ?
N7 C28 C27 108.7(6) . . ?
C27 C28 C29 128.7(6) . . ?
C18 C18 N2 109.6(4) 2_656 . ?
N8 C30 C31 108.6(5) . . ?
N6 C26 C27 107.9(6) . . ?
C30 C31 C32 107.3(5) . . ?
C26 C27 C28 107.3(6) . . ?
N10 B1 N6 107.8(4) . . ?
N10 B1 N8 109.7(4) . . ?
N6 B1 N8 107.0(6) . . ?
N2 C7 C8A 116.9(6) . . ?
C8 C7 N2 116.1(8) . . ?
C8A C9A C10A 120.0 . . ?
C9A C8A C7 116.1(5) . . ?
C9A C8A C17A 120.0 . . ?
C17A C8A C7 123.9(5) . . ?
C16A C17A C8A 120.0 . . ?
C17A C16A C15A 120.0 . . ?
C16A C15A C14A 120.0 . . ?
C10A C15A C16A 120.0 . . ?
C10A C15A C14A 120.0 . . ?
C15A C10A C9A 120.0 . . ?
C15A C10A C11A 120.0 . . ?
C11A C10A C9A 120.0 . . ?
C12A C11A C10A 120.0 . . ?
C11A C12A C13A 120.0 . . ?
C14A C13A C12A 120.0 . . ?
C13A C14A C15A 120.0 . . ?
C8 C17 C16 120.0 . . ?
C17 C8 C7 116.1(9) . . ?
C17 C8 C9 120.0 . . ?
C9 C8 C7 123.9(9) . . ?
C10 C9 C8 120.0 . . ?
C9 C10 C11 120.0 . . ?
C10 C11 C12 120.0 . . ?
C16 C11 C10 120.0 . . ?
C16 C11 C12 120.0 . . ?
C11 C16 C17 120.0 . . ?
C15 C16 C17 120.0 . . ?
C15 C16 C11 120.0 . . ?
C14 C15 C16 120.0 . . ?
C15 C14 C13 120.0 . . ?
C12 C13 C14 120.0 . . ?
C13 C12 C11 120.0 . . ?

_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 0.500 -0.965 1198.0 281.4 1.5CH3OH,1CH2Cl2
2 0.500 0.000 -0.679 1198.0 281.4 1.5CH3OH,1CH2Cl2

_olex2_submission_special_instructions 'No special instructions were received'
####################################################################### 
# 
# 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_Tpstar_100K
_database_code_depnum_ccdc_archive 'CCDC 1974451'
loop_
_audit_author_name
_audit_author_address
'Xin-Hua Zhao'
;Southern University of Science and Technology
China
;
_audit_update_record             
;
2020-03-27 deposited with the CCDC.	2020-04-01 downloaded from the CCDC.
;
_audit_creation_date             2020-03-10
_audit_creation_method           
;
Olex2 1.2
(compiled 2018.05.29 svn.r3508 for OlexSys, GUI svn.r5506)
;
_shelx_SHELXL_version_number     2014/7
_chemical_name_common            ?
_chemical_name_systematic        ?
_chemical_formula_moiety         'C72 H78 B2 Fe3 N22, 8(H2 O), 6(C H4 O)'
_chemical_formula_sum            'C78 H118 B2 Fe3 N22 O14'
_chemical_formula_weight         1777.11
_chemical_melting_point          ?
loop_
_atom_type_symbol
_atom_type_description
_atom_type_scat_dispersion_real
_atom_type_scat_dispersion_imag
_atom_type_scat_source
C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
B B 0.0013 0.0007 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Fe Fe 0.3463 0.8444 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'

_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      monoclinic
_space_group_IT_number           15
_space_group_name_H-M_alt        'C 1 2/c 1'
_space_group_name_Hall           '-C 2yc'
loop_
_space_group_symop_operation_xyz
'x, y, z'
'-x, y, -z+1/2'
'x+1/2, y+1/2, z'
'-x+1/2, y+1/2, -z+1/2'
'-x, -y, -z'
'x, -y, z-1/2'
'-x+1/2, -y+1/2, -z'
'x+1/2, -y+1/2, z-1/2'

_cell_length_a                   23.0454(12)
_cell_length_b                   19.9288(12)
_cell_length_c                   21.8359(11)
_cell_angle_alpha                90
_cell_angle_beta                 114.754(2)
_cell_angle_gamma                90
_cell_volume                     9107.0(9)
_cell_formula_units_Z            4
_cell_measurement_reflns_used    9902
_cell_measurement_temperature    100(2)
_cell_measurement_theta_max      26.302
_cell_measurement_theta_min      2.288
_shelx_estimated_absorpt_T_max   0.948
_shelx_estimated_absorpt_T_min   0.923
_exptl_absorpt_coefficient_mu    0.542
_exptl_absorpt_correction_T_max  0.7454
_exptl_absorpt_correction_T_min  0.6323
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   
'SADABS-2016/2 (Bruker,2016/2) was used for absorption correction. wR2(int) was 0.0932 before and 0.0680 after correction. The Ratio of minimum to maximum transmission is 0.8483. The λ/2 correction factor is Not present.'
_exptl_absorpt_special_details   ?
_exptl_crystal_colour            'dark red'
_exptl_crystal_colour_modifier   dark
_exptl_crystal_colour_primary    red
_exptl_crystal_density_diffrn    1.296
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    ?
_exptl_crystal_description       block
_exptl_crystal_F_000             3760
_exptl_crystal_size_max          0.15
_exptl_crystal_size_mid          0.1
_exptl_crystal_size_min          0.1
_exptl_transmission_factor_max   ?
_exptl_transmission_factor_min   ?
_diffrn_reflns_av_R_equivalents  0.0832
_diffrn_reflns_av_unetI/netI     0.0452
_diffrn_reflns_Laue_measured_fraction_full 0.999
_diffrn_reflns_Laue_measured_fraction_max 0.996
_diffrn_reflns_limit_h_max       28
_diffrn_reflns_limit_h_min       -28
_diffrn_reflns_limit_k_max       24
_diffrn_reflns_limit_k_min       -24
_diffrn_reflns_limit_l_max       27
_diffrn_reflns_limit_l_min       -27
_diffrn_reflns_number            70340
_diffrn_reflns_point_group_measured_fraction_full 0.999
_diffrn_reflns_point_group_measured_fraction_max 0.996
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         26.472
_diffrn_reflns_theta_min         2.287
_diffrn_ambient_temperature      100.02
_diffrn_detector_area_resol_mean ?
_diffrn_measured_fraction_theta_full 0.999
_diffrn_measured_fraction_theta_max 0.996
_diffrn_measurement_device_type  'Bruker APEX-II CCD'
_diffrn_measurement_method       'φ and ω scans'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_source                   ?
_diffrn_standards_number         0
_reflns_Friedel_coverage         0.000
_reflns_Friedel_fraction_full    .
_reflns_Friedel_fraction_max     .
_reflns_number_gt                6220
_reflns_number_total             9355
_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       'SAINT V8.38A (?, 2016)'
_computing_data_collection       'Bruker APEX3'
_computing_data_reduction        'SAINT V8.38A (?, 2016)'
_computing_molecular_graphics    'Olex2 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 (Dolomanov et al., 2009)'
_computing_structure_refinement  'XL (Sheldrick, 2008)'
_computing_structure_solution    'olex2.solve (Bourhis et al., 2015)'
_refine_diff_density_max         0.691
_refine_diff_density_min         -0.767
_refine_diff_density_rms         0.095
_refine_ls_extinction_coef       .
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.053
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     562
_refine_ls_number_reflns         9355
_refine_ls_number_restraints     128
_refine_ls_R_factor_all          0.1153
_refine_ls_R_factor_gt           0.0719
_refine_ls_restrained_S_all      1.055
_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)+(0.1127P)²+44.4412P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1948
_refine_ls_wR_factor_ref         0.2408
_refine_special_details          ?
_olex2_refinement_description    
;
1. Fixed Uiso
 At 1.2 times of:
  All B(H) groups, All C(H) groups, All C(H,H) groups, All C(H,H,H,H) groups
 At 1.5 times of:
  All C(H,H,H) groups, All O(H) groups, All O(H,H) groups
2. Restrained distances
 O3B-C39B
 1.45 with sigma of 0.02
 C39A-O3A
 1.45 with sigma of 0.02
 O3A-C39A
 1.45 with sigma of 0.02
 H1B-H5A
 2.1 with sigma of 0.02
 H8B-H8B_$1
 2.1 with sigma of 0.01
 H8B_$4-H5B
 2.1 with sigma of 0.02
3. Rigid bond restraints
 O1, C37
 with sigma for 1-2 distances of 0.02 and sigma for 1-3 distances of 0.02
 O2, C38
 with sigma for 1-2 distances of 0.02 and sigma for 1-3 distances of 0.02
4. Uiso/Uaniso restraints and constraints
O1 \\sim C37: within 2A with sigma of 0.02 and sigma for terminal atoms of 0.04
C14 \\sim C12 \\sim C11 \\sim C13 \\sim C9 \\sim C8 \\sim C17 \\sim C16 \\sim
C15 \\sim C10: within 2A with sigma of 0.02 and sigma for terminal atoms of 0.04
O2 \\sim C38: within 2A with sigma of 0.02 and sigma for terminal atoms of 0.04
Uanis(O3B) \\sim Ueq, Uanis(C39B) \\sim Ueq: with sigma of 0.02 and sigma for
terminal atoms of 0.04
Uanis(O7) \\sim Ueq: with sigma of 0.02 and sigma for terminal atoms of 0.04
Uanis(O6B) \\sim Ueq: with sigma of 0.02 and sigma for terminal atoms of 0.04
Uanis(O3A) \\sim Ueq, Uanis(C39A) \\sim Ueq: with sigma of 0.02 and sigma for
terminal atoms of 0.04
Uanis(O4) \\sim Ueq: with sigma of 0.02 and sigma for terminal atoms of 0.04
Uanis(C8A) = Uanis(C8)
Uanis(C17) = Uanis(C9A)
Uanis(C17A) = Uanis(C9)
Uanis(C16) = Uanis(C10A)
Uanis(C16A) = Uanis(C10)
Uanis(C15) = Uanis(C11A)
Uanis(C15A) = Uanis(C11)
Uanis(C14) = Uanis(C12A)
Uanis(C14A) = Uanis(C12)
Uanis(C13A) = Uanis(C13)
Uanis(O3A) = Uanis(O3B)
Uanis(C39A) = Uanis(C39B)
5. Others
 Sof(H7BC)=Sof(H7BD)=Sof(C15A)=Sof(H15A)=Sof(C14A)=Sof(H14A)=Sof(C13A)=
 Sof(H13A)=Sof(C12A)=Sof(H12A)=Sof(C11A)=Sof(C16A)=Sof(C17A)=Sof(H17A)=Sof(C8A)=
 Sof(C9A)=Sof(H9A)=Sof(C10A)=Sof(H10A)=1-FVAR(1)
 Sof(H7AA)=Sof(H7AB)=Sof(C9)=Sof(H9)=Sof(C8)=Sof(C17)=Sof(H17)=Sof(C16)=
 Sof(H16)=Sof(C15)=Sof(C10)=Sof(C11)=Sof(H11)=Sof(C12)=Sof(H12)=Sof(C13)=
 Sof(H13)=Sof(C14)=Sof(H14)=FVAR(1)
 Sof(O3B)=Sof(H3B)=Sof(C39B)=Sof(H39D)=Sof(H39E)=Sof(H39F)=1-FVAR(2)
 Sof(O3A)=Sof(H3A)=Sof(C39A)=Sof(H39A)=Sof(H39B)=Sof(H39C)=FVAR(2)
 Sof(O6B)=Sof(H6BA)=Sof(H6BB)=1-FVAR(3)
 Sof(O6A)=Sof(H6AA)=Sof(H6AB)=FVAR(3)
 Fixed Sof: O4(0.5) H4A(0.5) H4B(0.5) O7(0.5) H7A(0.5) H7B(0.5)
6.a Riding coordinates:
 O4(H4A,H4B), O8(H8A,H8B), O2(H2A), O6B(H6BA,H6BB), O3A(H3A), O7(H7A,H7B),
 C39A(H39A,H39B,H39C), C38(H38A,H38B,H38C)
6.b Free rotating group:
 O6A(H6AA,H6AB), O5(H5A,H5B)
6.c Ternary CH refined with riding coordinates:
 B1(H1A)
6.d Secondary CH2 refined with riding coordinates:
 C18(H18A,H18B), C6(H6A,H6B), C7(H7AA,H7AB), C7(H7BC,H7BD)
6.e Aromatic/amide H refined with riding coordinates:
 C29(H29), C1(H1), C2(H2), C3(H3), C4(H4), C24(H24), C9(H9), C17(H17),
 C16(H16), C11(H11), C12(H12), C13(H13), C14(H14), C34(H34), C15A(H15A),
 C14A(H14A), C13A(H13A), C12A(H12A), C17A(H17A), C9A(H9A), C10A(H10A)
6.f Naphthalene refined as free rotating group:
 C9(C8,C17,C16,C15,C10,C11,C12,C13,C14), C15A(C14A,C13A,C12A,C11A,C16A,C17A,
 C8A,C9A,C10A)
6.g Idealised Me refined as rotating group:
 C23(H23A,H23B,H23C), C31(H31A,H31B,H31C), C33(H33A,H33B,H33C), C37(H37A,H37B,
 H37C), C26(H26A,H26B,H26C), C28(H28A,H28B,H28C), C36(H36A,H36B,H36C),
 C39B(H39D,H39E,H39F)
6.h Idealised tetrahedral OH refined as rotating group:
 O1(H1B), O3B(H3B)
;
_atom_sites_solution_hydrogens   mixed
_atom_sites_solution_primary     iterative
_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
Fe1 Fe 0.5000 0.59343(5) 0.7500 0.0335(2) Uani 1 2 d S T P . .
Fe2 Fe 0.61814(3) 0.41549(4) 0.91600(3) 0.0389(2) Uani 1 1 d . . . . .
O6A O 0.1475(4) 0.4602(6) 0.6145(6) 0.115(5) Uani 0.622(13) 1 d . . . A 1
H6AA H 0.1305 0.4724 0.5724 0.172 Uiso 0.622(13) 1 d G . . A 1
H6AB H 0.1884 0.4648 0.6270 0.172 Uiso 0.622(13) 1 d G . . A 1
O4 O 0.4539(8) 0.9963(7) 0.6424(11) 0.188(8) Uani 0.5 1 d . U . . .
H4A H 0.4702 0.9731 0.6197 0.282 Uiso 0.5 1 d R . . . .
H4B H 0.4531 0.9685 0.6728 0.282 Uiso 0.5 1 d R . . . .
O8 O 0.5502(2) 0.8903(6) 0.7324(6) 0.255(6) Uani 1 1 d . . . . .
H8A H 0.5102 0.8962 0.7057 0.383 Uiso 1 1 d R . . . .
H8B H 0.5497 0.8658 0.7652 0.383 Uiso 1 1 d DR . . . .
O1 O 0.7402(4) 0.4246(5) 0.6418(4) 0.161(3) Uani 1 1 d . U . . .
H1B H 0.7240 0.4597 0.6202 0.242 Uiso 1 1 calc DGR . . . .
O5 O 0.8619(6) 0.4736(6) 0.6992(7) 0.221(5) Uani 1 1 d . . . . .
H5A H 0.8209 0.4721 0.6873 0.331 Uiso 1 1 d DG . . . .
H5B H 0.8757 0.4346 0.7171 0.331 Uiso 1 1 d DG . . . .
O2 O 0.1583(6) 0.5470(5) 0.7150(7) 0.226(5) Uani 1 1 d . U . . .
H2A H 0.1420 0.5164 0.6863 0.338 Uiso 1 1 d R . . . .
O6B O 0.2113(14) 0.444(2) 0.7095(19) 0.259(18) Uani 0.378(13) 1 d . U . A 2
H6BA H 0.1818 0.4467 0.7243 0.388 Uiso 0.378(13) 1 d R . . A 2
H6BB H 0.2487 0.4492 0.7430 0.388 Uiso 0.378(13) 1 d R . . A 2
O3A O 0.6077(8) 0.8411(9) 0.6665(9) 0.174(5) Uani 0.589(8) 1 d D U . B 1
H3A H 0.6178 0.8649 0.7012 0.260 Uiso 0.589(8) 1 d R . . B 1
O3B O 0.6652(11) 0.7970(14) 0.7162(12) 0.174(5) Uani 0.411(8) 1 d D U . B 2
H3B H 0.6466 0.7670 0.7284 0.260 Uiso 0.411(8) 1 calc GR . . B 2
O7 O 0.0559(8) 0.5110(15) 0.4803(13) 0.269(13) Uani 0.5 1 d . U . . .
H7A H 0.0279 0.4829 0.4824 0.403 Uiso 0.5 1 d R . . . .
H7B H 0.0450 0.5228 0.4385 0.403 Uiso 0.5 1 d R . . . .
N1 N 0.56725(16) 0.5963(2) 0.71507(17) 0.0368(8) Uani 1 1 d . . . . .
N9 N 0.54552(16) 0.3819(2) 0.93515(17) 0.0393(9) Uani 1 1 d . . . . .
N7 N 0.60134(17) 0.3395(2) 0.85197(17) 0.0405(9) Uani 1 1 d . . . . .
N2 N 0.46322(16) 0.6688(2) 0.68004(17) 0.0378(8) Uani 1 1 d . . . . .
N6 N 0.59393(17) 0.2766(2) 0.87396(18) 0.0430(9) Uani 1 1 d . . . . .
N3 N 0.54373(16) 0.5242(2) 0.81495(16) 0.0344(8) Uani 1 1 d . . . . .
N8 N 0.54404(18) 0.3150(2) 0.94815(18) 0.0429(9) Uani 1 1 d . . . . .
N4 N 0.72665(19) 0.4621(2) 0.8792(2) 0.0535(11) Uani 1 1 d . . . . .
N10 N 0.66096(18) 0.2953(2) 0.99735(19) 0.0459(10) Uani 1 1 d . . . . .
N5 N 0.64390(19) 0.5347(3) 1.0139(2) 0.0580(12) Uani 1 1 d . . . . .
N11 N 0.67922(18) 0.3585(2) 0.99091(18) 0.0453(10) Uani 1 1 d . . . . .
C39A C 0.5569(13) 0.8747(13) 0.6079(14) 0.239(11) Uani 0.589(8) 1 d D U . B 1
H39A H 0.5239 0.8917 0.6210 0.359 Uiso 0.589(8) 1 d R . . B 1
H39B H 0.5378 0.8429 0.5706 0.359 Uiso 0.589(8) 1 d R . . B 1
H39C H 0.5759 0.9122 0.5937 0.359 Uiso 0.589(8) 1 d R . . B 1
C19 C 0.56844(19) 0.4800(2) 0.8502(2) 0.0348(9) Uani 1 1 d . . . . .
C21 C 0.6339(2) 0.4899(3) 0.9776(2) 0.0456(12) Uani 1 1 d . . . . .
C23 C 0.5686(2) 0.1600(3) 0.8329(3) 0.0526(12) Uani 1 1 d . . . . .
H23A H 0.6017 0.1426 0.8750 0.079 Uiso 1 1 calc GR . . . .
H23B H 0.5688 0.1341 0.7948 0.079 Uiso 1 1 calc GR . . . .
H23C H 0.5267 0.1561 0.8340 0.079 Uiso 1 1 calc GR . . . .
C25 C 0.5934(2) 0.3318(3) 0.7873(2) 0.0413(11) Uani 1 1 d . . . . .
C27 C 0.4900(2) 0.2999(3) 0.9562(2) 0.0448(11) Uani 1 1 d . . . . .
C29 C 0.4571(2) 0.3588(3) 0.9492(2) 0.0439(11) Uani 1 1 d . . . . .
H29 H 0.4177 0.3644 0.9529 0.053 Uiso 1 1 calc R . . . .
C31 C 0.4732(2) 0.4803(2) 0.9194(2) 0.0400(10) Uani 1 1 d . . . . .
H31A H 0.5110 0.5089 0.9408 0.060 Uiso 1 1 calc GR . . . .
H31B H 0.4414 0.4922 0.9364 0.060 Uiso 1 1 calc GR . . . .
H31C H 0.4550 0.4867 0.8704 0.060 Uiso 1 1 calc GR . . . .
C33 C 0.7003(3) 0.1963(3) 1.0732(3) 0.0680(17) Uani 1 1 d . . . . .
H33A H 0.6660 0.1943 1.0886 0.102 Uiso 1 1 calc GR . . . .
H33B H 0.7407 0.1825 1.1100 0.102 Uiso 1 1 calc GR . . . .
H33C H 0.6902 0.1661 1.0347 0.102 Uiso 1 1 calc GR . . . .
C35 C 0.7375(2) 0.3694(3) 1.0428(2) 0.0495(13) Uani 1 1 d . . . . .
C37 C 0.7125(7) 0.4100(7) 0.6818(8) 0.167(5) Uani 1 1 d . U . . .
H37A H 0.6841 0.3713 0.6637 0.250 Uiso 1 1 calc GR . . . .
H37B H 0.6875 0.4486 0.6848 0.250 Uiso 1 1 calc GR . . . .
H37C H 0.7451 0.3991 0.7269 0.250 Uiso 1 1 calc GR . . . .
C1 C 0.62604(19) 0.5692(2) 0.7442(2) 0.0386(10) Uani 1 1 d . . . . .
H1 H 0.6387 0.5473 0.7865 0.046 Uiso 1 1 calc R . . . .
C18 C 0.4967(2) 0.7317(3) 0.7143(2) 0.0445(11) Uani 1 1 d . . . . .
H18A H 0.4719 0.7714 0.6900 0.053 Uiso 1 1 calc R . . . .
H18B H 0.5395 0.7339 0.7139 0.053 Uiso 1 1 calc R . . . .
C2 C 0.6689(2) 0.5720(3) 0.7147(2) 0.0448(11) Uani 1 1 d . . . . .
H2 H 0.7097 0.5515 0.7360 0.054 Uiso 1 1 calc R . . . .
C20 C 0.6870(2) 0.4459(3) 0.8945(2) 0.0455(11) Uani 1 1 d . . . . .
C3 C 0.6514(2) 0.6049(3) 0.6541(2) 0.0471(12) Uani 1 1 d . . . . .
H3 H 0.6802 0.6081 0.6333 0.057 Uiso 1 1 calc R . . . .
C22 C 0.58183(19) 0.2313(3) 0.8249(2) 0.0429(11) Uani 1 1 d . . . . .
C4 C 0.5910(2) 0.6334(3) 0.6239(2) 0.0448(11) Uani 1 1 d . . . . .
H4 H 0.5778 0.6565 0.5822 0.054 Uiso 1 1 calc R . . . .
C24 C 0.5820(2) 0.2647(3) 0.7699(2) 0.0453(11) Uani 1 1 d . . . . .
H24 H 0.5756 0.2454 0.7277 0.054 Uiso 1 1 calc R . . . .
C5 C 0.5503(2) 0.6274(2) 0.6557(2) 0.0380(10) Uani 1 1 d . . . . .
C26 C 0.5952(3) 0.3884(3) 0.7438(2) 0.0500(12) Uani 1 1 d . . . . .
H26A H 0.5585 0.4179 0.7345 0.075 Uiso 1 1 calc GR . . . .
H26B H 0.5936 0.3706 0.7012 0.075 Uiso 1 1 calc GR . . . .
H26C H 0.6348 0.4139 0.7669 0.075 Uiso 1 1 calc GR . . . .
C6 C 0.4825(2) 0.6531(3) 0.6247(2) 0.0408(10) Uani 1 1 d . . . . .
H6A H 0.4797 0.6939 0.5977 0.049 Uiso 1 1 calc R . . . .
H6B H 0.4538 0.6186 0.5945 0.049 Uiso 1 1 calc R . . . .
C28 C 0.4756(3) 0.2312(3) 0.9712(3) 0.0567(13) Uani 1 1 d . . . . .
H28A H 0.4732 0.2009 0.9349 0.085 Uiso 1 1 calc GR . . . .
H28B H 0.4347 0.2311 0.9749 0.085 Uiso 1 1 calc GR . . . .
H28C H 0.5095 0.2161 1.0139 0.085 Uiso 1 1 calc GR . . . .
C7 C 0.3915(2) 0.6769(3) 0.6514(2) 0.0423(11) Uani 1 1 d . . . . .
H7AA H 0.3795 0.6852 0.6893 0.051 Uiso 0.745(4) 1 calc R . . C 1
H7AB H 0.3717 0.6338 0.6304 0.051 Uiso 0.745(4) 1 calc R . . C 1
H7BC H 0.3806 0.7023 0.6841 0.051 Uiso 0.255(4) 1 calc R . . C 2
H7BD H 0.3718 0.6319 0.6463 0.051 Uiso 0.255(4) 1 calc R . . C 2
C30 C 0.49196(19) 0.4090(2) 0.93545(19) 0.0383(10) Uani 1 1 d . . . . .
C9 C 0.34090(18) 0.71727(14) 0.53094(16) 0.0436(14) Uani 0.745(4) 1 d . U . C 1
H9 H 0.3430 0.6723 0.5176 0.052 Uiso 0.745(4) 1 calc R . . C 1
C8 C 0.36189(19) 0.73304(18) 0.59887(14) 0.0415(16) Uani 0.745(4) 1 d G U . C 1
C17 C 0.35884(19) 0.7989(2) 0.61831(13) 0.0507(16) Uani 0.745(4) 1 d G U . C 1
H17 H 0.3732 0.8097 0.6647 0.061 Uiso 0.745(4) 1 calc R . . C 1
C16 C 0.33479(19) 0.84895(16) 0.56983(16) 0.0537(16) Uani 0.745(4) 1 d G U . C
1
H16 H 0.3327 0.8940 0.5831 0.064 Uiso 0.745(4) 1 calc R . . C 1
C15 C 0.31379(13) 0.83318(14) 0.50190(14) 0.0526(17) Uani 0.745(4) 1 d G U . C
1
C10 C 0.31685(12) 0.76733(15) 0.48245(12) 0.0457(15) Uani 0.745(4) 1 d G U . C
1
C11 C 0.29585(19) 0.7516(2) 0.41453(13) 0.065(2) Uani 0.745(4) 1 d G U . C 1
H11 H 0.2979 0.7066 0.4012 0.078 Uiso 0.745(4) 1 calc R . . C 1
C12 C 0.2718(2) 0.8016(3) 0.36604(12) 0.074(2) Uani 0.745(4) 1 d G U . C 1
H12 H 0.2575 0.7908 0.3196 0.089 Uiso 0.745(4) 1 calc R . . C 1
C13 C 0.2687(2) 0.8675(2) 0.38549(17) 0.076(3) Uani 0.745(4) 1 d G U . C 1
H13 H 0.2523 0.9017 0.3524 0.091 Uiso 0.745(4) 1 calc R . . C 1
C14 C 0.2897(2) 0.88324(17) 0.45342(19) 0.065(2) Uani 0.745(4) 1 d G U . C 1
H14 H 0.2877 0.9282 0.4667 0.078 Uiso 0.745(4) 1 calc R . . C 1
C32 C 0.7063(2) 0.2660(3) 1.0527(2) 0.0526(14) Uani 1 1 d . . . . .
C34 C 0.7548(2) 0.3119(3) 1.0819(2) 0.0569(15) Uani 1 1 d . . . . .
H34 H 0.7931 0.3052 1.1214 0.068 Uiso 1 1 calc R . . . .
C36 C 0.7746(2) 0.4322(3) 1.0535(3) 0.0641(16) Uani 1 1 d . . . . .
H36A H 0.7984 0.4319 1.0254 0.096 Uiso 1 1 calc GR . . . .
H36B H 0.8046 0.4358 1.1011 0.096 Uiso 1 1 calc GR . . . .
H36C H 0.7454 0.4707 1.0412 0.096 Uiso 1 1 calc GR . . . .
C38 C 0.1208(9) 0.6034(8) 0.6925(10) 0.230(8) Uani 1 1 d . U . . .
H38A H 0.1423 0.6406 0.7228 0.346 Uiso 1 1 d R . . . .
H38B H 0.0796 0.5947 0.6942 0.346 Uiso 1 1 d R . . . .
H38C H 0.1137 0.6152 0.6463 0.346 Uiso 1 1 d R . . . .
C39B C 0.7246(17) 0.816(2) 0.773(2) 0.239(11) Uani 0.411(8) 1 d D U . B 2
H39D H 0.7167 0.8539 0.7968 0.359 Uiso 0.411(8) 1 calc GR . . B 2
H39E H 0.7565 0.8284 0.7564 0.359 Uiso 0.411(8) 1 calc GR . . B 2
H39F H 0.7404 0.7776 0.8039 0.359 Uiso 0.411(8) 1 calc GR . . B 2
C15A C 0.3237(6) 0.8892(5) 0.5350(5) 0.065(2) Uani 0.255(4) 1 d . . . C 2
H15A H 0.3383 0.9100 0.5780 0.078 Uiso 0.255(4) 1 calc R . . C 2
C14A C 0.2967(7) 0.9278(5) 0.4768(7) 0.074(2) Uani 0.255(4) 1 d G . . C 2
H14A H 0.2927 0.9750 0.4801 0.089 Uiso 0.255(4) 1 calc R . . C 2
C13A C 0.2753(7) 0.8974(6) 0.4139(6) 0.076(3) Uani 0.255(4) 1 d G . . C 2
H13A H 0.2568 0.9238 0.3741 0.091 Uiso 0.255(4) 1 calc R . . C 2
C12A C 0.2810(6) 0.8284(6) 0.4092(4) 0.065(2) Uani 0.255(4) 1 d G . . C 2
H12A H 0.2664 0.8076 0.3662 0.078 Uiso 0.255(4) 1 calc R . . C 2
C11A C 0.3081(4) 0.7898(5) 0.4674(4) 0.0526(17) Uani 0.255(4) 1 d G . . C 2
C16A C 0.3295(4) 0.8202(5) 0.5303(4) 0.0457(15) Uani 0.255(4) 1 d G . . C 2
C17A C 0.3566(6) 0.7816(6) 0.5885(4) 0.0436(14) Uani 0.255(4) 1 d G . . C 2
H17A H 0.3712 0.8024 0.6315 0.052 Uiso 0.255(4) 1 calc R . . C 2
C8A C 0.3623(6) 0.7126(6) 0.5838(5) 0.0415(16) Uani 0.255(4) 1 d G . . C 2
C9A C 0.3409(6) 0.6821(5) 0.5209(6) 0.0507(16) Uani 0.255(4) 1 d G . . C 2
H9A H 0.3448 0.6350 0.5176 0.061 Uiso 0.255(4) 1 calc R . . C 2
C10A C 0.3138(6) 0.7207(5) 0.4627(5) 0.0537(16) Uani 0.255(4) 1 d G . . C 2
H10A H 0.2992 0.6999 0.4196 0.064 Uiso 0.255(4) 1 calc R . . C 2
B1 B 0.5965(3) 0.2696(3) 0.9453(3) 0.0466(13) Uani 1 1 d . . . . .
H1A H 0.5895 0.2219 0.9549 0.056 Uiso 1 1 calc R . . . .


_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
Fe1 N1 1.994(3) . ?
Fe1 N1 1.994(3) 2_656 ?
Fe1 N2 2.055(4) . ?
Fe1 N2 2.055(4) 2_656 ?
Fe1 N3 1.932(4) 2_656 ?
Fe1 N3 1.932(4) . ?
Fe2 N9 2.002(4) . ?
Fe2 N7 1.985(4) . ?
Fe2 N11 2.004(4) . ?
Fe2 C19 1.911(5) . ?
Fe2 C21 1.932(5) . ?
Fe2 C20 1.932(5) . ?
O6A H6AA 0.8706 . ?
O6A H6AB 0.8686 . ?
O4 H4A 0.8698 . ?
O4 H4B 0.8700 . ?
O8 H8A 0.8688 . ?
O8 H8B 0.8713 . ?
O1 H1B 0.8400 . ?
O1 C37 1.314(13) . ?
O5 H5A 0.8700 . ?
O5 H5B 0.8701 . ?
O2 H2A 0.8408 . ?
O2 C38 1.376(15) . ?
O6B H6BA 0.8699 . ?
O6B H6BB 0.8709 . ?
O3A H3A 0.8400 . ?
O3A C39A 1.483(13) . ?
O3B H3B 0.8400 . ?
O3B C39B 1.460(19) . ?
O7 H7A 0.8707 . ?
O7 H7B 0.8705 . ?
N1 C1 1.346(6) . ?
N1 C5 1.340(5) . ?
N9 N8 1.367(6) . ?
N9 C30 1.350(5) . ?
N7 N6 1.380(6) . ?
N7 C25 1.353(5) . ?
N2 C18 1.498(6) . ?
N2 C6 1.486(5) . ?
N2 C7 1.512(5) . ?
N6 C22 1.337(6) . ?
N6 B1 1.541(6) . ?
N3 C19 1.151(6) . ?
N8 C27 1.363(6) . ?
N8 B1 1.532(6) . ?
N4 C20 1.143(6) . ?
N10 N11 1.353(6) . ?
N10 C32 1.355(6) . ?
N10 B1 1.532(7) . ?
N5 C21 1.151(7) . ?
N11 C35 1.365(6) . ?
C39A H39A 0.9798 . ?
C39A H39B 0.9800 . ?
C39A H39C 0.9802 . ?
C23 H23A 0.9800 . ?
C23 H23B 0.9800 . ?
C23 H23C 0.9800 . ?
C23 C22 1.478(7) . ?
C25 C24 1.384(7) . ?
C25 C26 1.487(7) . ?
C27 C29 1.371(7) . ?
C27 C28 1.476(8) . ?
C29 H29 0.9500 . ?
C29 C30 1.392(7) . ?
C31 H31A 0.9800 . ?
C31 H31B 0.9800 . ?
C31 H31C 0.9800 . ?
C31 C30 1.484(7) . ?
C33 H33A 0.9800 . ?
C33 H33B 0.9800 . ?
C33 H33C 0.9800 . ?
C33 C32 1.483(9) . ?
C35 C34 1.384(8) . ?
C35 C36 1.478(9) . ?
C37 H37A 0.9800 . ?
C37 H37B 0.9800 . ?
C37 H37C 0.9800 . ?
C1 H1 0.9500 . ?
C1 C2 1.387(6) . ?
C18 C18 1.504(9) 2_656 ?
C18 H18A 0.9900 . ?
C18 H18B 0.9900 . ?
C2 H2 0.9500 . ?
C2 C3 1.378(7) . ?
C3 H3 0.9500 . ?
C3 C4 1.388(7) . ?
C22 C24 1.377(7) . ?
C4 H4 0.9500 . ?
C4 C5 1.385(6) . ?
C24 H24 0.9500 . ?
C5 C6 1.507(6) . ?
C26 H26A 0.9800 . ?
C26 H26B 0.9800 . ?
C26 H26C 0.9800 . ?
C6 H6A 0.9900 . ?
C6 H6B 0.9900 . ?
C28 H28A 0.9800 . ?
C28 H28B 0.9800 . ?
C28 H28C 0.9800 . ?
C7 H7AA 0.9900 . ?
C7 H7AB 0.9900 . ?
C7 H7BC 0.9900 . ?
C7 H7BD 0.9900 . ?
C7 C8 1.541(5) . ?
C7 C8A 1.518(9) . ?
C9 H9 0.9500 . ?
C9 C8 1.3900 . ?
C9 C10 1.3900 . ?
C8 C17 1.3900 . ?
C17 H17 0.9500 . ?
C17 C16 1.3900 . ?
C16 H16 0.9500 . ?
C16 C15 1.3900 . ?
C15 C10 1.3900 . ?
C15 C14 1.3900 . ?
C10 C11 1.3900 . ?
C11 H11 0.9500 . ?
C11 C12 1.3900 . ?
C12 H12 0.9500 . ?
C12 C13 1.3900 . ?
C13 H13 0.9500 . ?
C13 C14 1.3900 . ?
C14 H14 0.9500 . ?
C32 C34 1.378(8) . ?
C34 H34 0.9500 . ?
C36 H36A 0.9800 . ?
C36 H36B 0.9800 . ?
C36 H36C 0.9800 . ?
C38 H38A 0.9803 . ?
C38 H38B 0.9810 . ?
C38 H38C 0.9804 . ?
C39B H39D 0.9800 . ?
C39B H39E 0.9800 . ?
C39B H39F 0.9800 . ?
C15A H15A 0.9500 . ?
C15A C14A 1.3900 . ?
C15A C16A 1.3900 . ?
C14A H14A 0.9500 . ?
C14A C13A 1.3900 . ?
C13A H13A 0.9500 . ?
C13A C12A 1.3900 . ?
C12A H12A 0.9500 . ?
C12A C11A 1.3900 . ?
C11A C16A 1.3900 . ?
C11A C10A 1.3900 . ?
C16A C17A 1.3900 . ?
C17A H17A 0.9500 . ?
C17A C8A 1.3900 . ?
C8A C9A 1.3900 . ?
C9A H9A 0.9500 . ?
C9A C10A 1.3900 . ?
C10A H10A 0.9500 . ?
B1 H1A 1.0000 . ?

loop_
_geom_angle_atom_site_label_1
_geom_angle_atom_site_label_2
_geom_angle_atom_site_label_3
_geom_angle
_geom_angle_site_symmetry_1
_geom_angle_site_symmetry_3
_geom_angle_publ_flag
N1 Fe1 N1 176.7(2) . 2_656 ?
N1 Fe1 N2 80.76(14) 2_656 2_656 ?
N1 Fe1 N2 80.76(14) . . ?
N1 Fe1 N2 96.82(14) 2_656 . ?
N1 Fe1 N2 96.82(14) . 2_656 ?
N2 Fe1 N2 86.1(2) 2_656 . ?
N3 Fe1 N1 89.41(14) 2_656 . ?
N3 Fe1 N1 89.41(14) . 2_656 ?
N3 Fe1 N1 92.94(14) . . ?
N3 Fe1 N1 92.93(14) 2_656 2_656 ?
N3 Fe1 N2 173.43(13) 2_656 2_656 ?
N3 Fe1 N2 173.44(13) . . ?
N3 Fe1 N2 92.87(15) . 2_656 ?
N3 Fe1 N2 92.87(15) 2_656 . ?
N3 Fe1 N3 88.9(2) 2_656 . ?
N9 Fe2 N11 90.17(15) . . ?
N7 Fe2 N9 87.63(16) . . ?
N7 Fe2 N11 90.35(16) . . ?
C19 Fe2 N9 95.25(16) . . ?
C19 Fe2 N7 96.04(16) . . ?
C19 Fe2 N11 171.78(19) . . ?
C19 Fe2 C21 83.41(19) . . ?
C19 Fe2 C20 84.34(19) . . ?
C21 Fe2 N9 92.37(18) . . ?
C21 Fe2 N7 179.45(19) . . ?
C21 Fe2 N11 90.21(18) . . ?
C20 Fe2 N9 177.84(18) . . ?
C20 Fe2 N7 90.31(18) . . ?
C20 Fe2 N11 90.47(18) . . ?
C20 Fe2 C21 89.7(2) . . ?
H6AA O6A H6AB 104.6 . . ?
H4A O4 H4B 104.5 . . ?
H8A O8 H8B 104.5 . . ?
C37 O1 H1B 109.5 . . ?
H5A O5 H5B 104.5 . . ?
C38 O2 H2A 107.9 . . ?
H6BA O6B H6BB 109.4 . . ?
C39A O3A H3A 110.1 . . ?
C39B O3B H3B 109.5 . . ?
H7A O7 H7B 109.5 . . ?
C1 N1 Fe1 126.7(3) . . ?
C5 N1 Fe1 115.2(3) . . ?
C5 N1 C1 118.1(4) . . ?
N8 N9 Fe2 117.7(3) . . ?
C30 N9 Fe2 135.5(3) . . ?
C30 N9 N8 106.7(4) . . ?
N6 N7 Fe2 117.7(3) . . ?
C25 N7 Fe2 136.3(4) . . ?
C25 N7 N6 106.0(4) . . ?
C18 N2 Fe1 106.0(3) . . ?
C18 N2 C7 111.2(4) . . ?
C6 N2 Fe1 106.3(3) . . ?
C6 N2 C18 108.3(3) . . ?
C6 N2 C7 109.5(3) . . ?
C7 N2 Fe1 115.2(3) . . ?
N7 N6 B1 118.4(4) . . ?
C22 N6 N7 110.5(4) . . ?
C22 N6 B1 131.0(5) . . ?
C19 N3 Fe1 175.6(3) . . ?
N9 N8 B1 118.6(4) . . ?
C27 N8 N9 110.2(4) . . ?
C27 N8 B1 130.9(5) . . ?
N11 N10 C32 109.7(4) . . ?
N11 N10 B1 118.8(4) . . ?
C32 N10 B1 131.5(5) . . ?
N10 N11 Fe2 118.0(3) . . ?
N10 N11 C35 107.6(4) . . ?
C35 N11 Fe2 134.3(4) . . ?
O3A C39A H39A 109.5 . . ?
O3A C39A H39B 110.1 . . ?
O3A C39A H39C 108.8 . . ?
H39A C39A H39B 109.5 . . ?
H39A C39A H39C 109.5 . . ?
H39B C39A H39C 109.5 . . ?
N3 C19 Fe2 172.1(4) . . ?
N5 C21 Fe2 179.0(5) . . ?
H23A C23 H23B 109.5 . . ?
H23A C23 H23C 109.5 . . ?
H23B C23 H23C 109.5 . . ?
C22 C23 H23A 109.5 . . ?
C22 C23 H23B 109.5 . . ?
C22 C23 H23C 109.5 . . ?
N7 C25 C24 109.0(4) . . ?
N7 C25 C26 123.5(4) . . ?
C24 C25 C26 127.5(4) . . ?
N8 C27 C29 106.8(4) . . ?
N8 C27 C28 122.4(4) . . ?
C29 C27 C28 130.8(4) . . ?
C27 C29 H29 126.4 . . ?
C27 C29 C30 107.3(4) . . ?
C30 C29 H29 126.4 . . ?
H31A C31 H31B 109.5 . . ?
H31A C31 H31C 109.5 . . ?
H31B C31 H31C 109.5 . . ?
C30 C31 H31A 109.5 . . ?
C30 C31 H31B 109.5 . . ?
C30 C31 H31C 109.5 . . ?
H33A C33 H33B 109.5 . . ?
H33A C33 H33C 109.5 . . ?
H33B C33 H33C 109.5 . . ?
C32 C33 H33A 109.5 . . ?
C32 C33 H33B 109.5 . . ?
C32 C33 H33C 109.5 . . ?
N11 C35 C34 108.0(5) . . ?
N11 C35 C36 124.7(5) . . ?
C34 C35 C36 127.3(5) . . ?
O1 C37 H37A 109.5 . . ?
O1 C37 H37B 109.5 . . ?
O1 C37 H37C 109.5 . . ?
H37A C37 H37B 109.5 . . ?
H37A C37 H37C 109.5 . . ?
H37B C37 H37C 109.5 . . ?
N1 C1 H1 118.8 . . ?
N1 C1 C2 122.4(4) . . ?
C2 C1 H1 118.8 . . ?
N2 C18 C18 108.9(3) . 2_656 ?
N2 C18 H18A 109.9 . . ?
N2 C18 H18B 109.9 . . ?
C18 C18 H18A 109.9 2_656 . ?
C18 C18 H18B 109.9 2_656 . ?
H18A C18 H18B 108.3 . . ?
C1 C2 H2 120.4 . . ?
C3 C2 C1 119.1(4) . . ?
C3 C2 H2 120.4 . . ?
N4 C20 Fe2 176.9(5) . . ?
C2 C3 H3 120.6 . . ?
C2 C3 C4 118.8(4) . . ?
C4 C3 H3 120.6 . . ?
N6 C22 C23 122.6(4) . . ?
N6 C22 C24 107.2(5) . . ?
C24 C22 C23 130.1(5) . . ?
C3 C4 H4 120.6 . . ?
C5 C4 C3 118.9(4) . . ?
C5 C4 H4 120.6 . . ?
C25 C24 H24 126.4 . . ?
C22 C24 C25 107.2(4) . . ?
C22 C24 H24 126.4 . . ?
N1 C5 C4 122.7(4) . . ?
N1 C5 C6 114.8(4) . . ?
C4 C5 C6 122.5(4) . . ?
C25 C26 H26A 109.5 . . ?
C25 C26 H26B 109.5 . . ?
C25 C26 H26C 109.5 . . ?
H26A C26 H26B 109.5 . . ?
H26A C26 H26C 109.5 . . ?
H26B C26 H26C 109.5 . . ?
N2 C6 C5 108.2(3) . . ?
N2 C6 H6A 110.1 . . ?
N2 C6 H6B 110.1 . . ?
C5 C6 H6A 110.1 . . ?
C5 C6 H6B 110.1 . . ?
H6A C6 H6B 108.4 . . ?
C27 C28 H28A 109.5 . . ?
C27 C28 H28B 109.5 . . ?
C27 C28 H28C 109.5 . . ?
H28A C28 H28B 109.5 . . ?
H28A C28 H28C 109.5 . . ?
H28B C28 H28C 109.5 . . ?
N2 C7 H7AA 108.1 . . ?
N2 C7 H7AB 108.1 . . ?
N2 C7 H7BC 108.6 . . ?
N2 C7 H7BD 108.6 . . ?
N2 C7 C8 116.9(4) . . ?
N2 C7 C8A 114.5(6) . . ?
H7AA C7 H7AB 107.3 . . ?
H7BC C7 H7BD 107.6 . . ?
C8 C7 H7AA 108.1 . . ?
C8 C7 H7AB 108.1 . . ?
C8A C7 H7BC 108.6 . . ?
C8A C7 H7BD 108.6 . . ?
N9 C30 C29 109.0(4) . . ?
N9 C30 C31 123.9(4) . . ?
C29 C30 C31 127.0(4) . . ?
C8 C9 H9 120.0 . . ?
C8 C9 C10 120.0 . . ?
C10 C9 H9 120.0 . . ?
C9 C8 C7 118.5(3) . . ?
C17 C8 C7 121.4(3) . . ?
C17 C8 C9 120.0 . . ?
C8 C17 H17 120.0 . . ?
C8 C17 C16 120.0 . . ?
C16 C17 H17 120.0 . . ?
C17 C16 H16 120.0 . . ?
C17 C16 C15 120.0 . . ?
C15 C16 H16 120.0 . . ?
C16 C15 C14 120.0 . . ?
C10 C15 C16 120.0 . . ?
C10 C15 C14 120.0 . . ?
C15 C10 C9 120.0 . . ?
C11 C10 C9 120.0 . . ?
C11 C10 C15 120.0 . . ?
C10 C11 H11 120.0 . . ?
C10 C11 C12 120.0 . . ?
C12 C11 H11 120.0 . . ?
C11 C12 H12 120.0 . . ?
C11 C12 C13 120.0 . . ?
C13 C12 H12 120.0 . . ?
C12 C13 H13 120.0 . . ?
C14 C13 C12 120.0 . . ?
C14 C13 H13 120.0 . . ?
C15 C14 H14 120.0 . . ?
C13 C14 C15 120.0 . . ?
C13 C14 H14 120.0 . . ?
N10 C32 C33 122.7(6) . . ?
N10 C32 C34 107.4(5) . . ?
C34 C32 C33 129.9(5) . . ?
C35 C34 H34 126.4 . . ?
C32 C34 C35 107.2(4) . . ?
C32 C34 H34 126.4 . . ?
C35 C36 H36A 109.5 . . ?
C35 C36 H36B 109.5 . . ?
C35 C36 H36C 109.5 . . ?
H36A C36 H36B 109.5 . . ?
H36A C36 H36C 109.5 . . ?
H36B C36 H36C 109.5 . . ?
O2 C38 H38A 108.2 . . ?
O2 C38 H38B 108.4 . . ?
O2 C38 H38C 111.8 . . ?
H38A C38 H38B 109.3 . . ?
H38A C38 H38C 109.5 . . ?
H38B C38 H38C 109.5 . . ?
O3B C39B H39D 109.5 . . ?
O3B C39B H39E 109.5 . . ?
O3B C39B H39F 109.5 . . ?
H39D C39B H39E 109.5 . . ?
H39D C39B H39F 109.5 . . ?
H39E C39B H39F 109.5 . . ?
C14A C15A H15A 120.0 . . ?
C14A C15A C16A 120.0 . . ?
C16A C15A H15A 120.0 . . ?
C15A C14A H14A 120.0 . . ?
C13A C14A C15A 120.0 . . ?
C13A C14A H14A 120.0 . . ?
C14A C13A H13A 120.0 . . ?
C14A C13A C12A 120.0 . . ?
C12A C13A H13A 120.0 . . ?
C13A C12A H12A 120.0 . . ?
C13A C12A C11A 120.0 . . ?
C11A C12A H12A 120.0 . . ?
C12A C11A C10A 120.0 . . ?
C16A C11A C12A 120.0 . . ?
C16A C11A C10A 120.0 . . ?
C11A C16A C15A 120.0 . . ?
C11A C16A C17A 120.0 . . ?
C17A C16A C15A 120.0 . . ?
C16A C17A H17A 120.0 . . ?
C8A C17A C16A 120.0 . . ?
C8A C17A H17A 120.0 . . ?
C17A C8A C7 114.1(7) . . ?
C9A C8A C7 125.9(7) . . ?
C9A C8A C17A 120.0 . . ?
C8A C9A H9A 120.0 . . ?
C10A C9A C8A 120.0 . . ?
C10A C9A H9A 120.0 . . ?
C11A C10A H10A 120.0 . . ?
C9A C10A C11A 120.0 . . ?
C9A C10A H10A 120.0 . . ?
N6 B1 H1A 110.7 . . ?
N8 B1 N6 106.9(4) . . ?
N8 B1 N10 108.0(4) . . ?
N8 B1 H1A 110.7 . . ?
N10 B1 N6 109.6(4) . . ?
N10 B1 H1A 110.7 . . ?

loop_
_geom_hbond_atom_site_label_D
_geom_hbond_atom_site_label_H
_geom_hbond_atom_site_label_A
_geom_hbond_distance_DH
_geom_hbond_distance_HA
_geom_hbond_distance_DA
_geom_hbond_angle_DHA
_geom_hbond_site_symmetry_A
O6A H6AB N4 0.87 2.02 2.845(8) 158.5 2_656
O4 H4A O7 0.87 2.03 2.60(4) 121.7 7_566
O4 H4B O5 0.87 2.40 2.90(3) 117.0 3_455
O1 H1B N5 0.84 2.28 2.863(9) 126.3 6_565
O5 H5A O1 0.87 1.95 2.728(15) 148.8 .
O5 H5B O8 0.87 1.82 2.561(15) 141.2 4_646
O2 H2A O6A 0.84 1.97 2.721(17) 147.7 .
O7 H7B O4 0.87 1.82 2.60(4) 147.8 7_566
C39A H39C O6A 0.98 1.79 2.65(3) 144.3 3
C37 H37C O6B 0.98 1.61 2.39(4) 133.2 2_656
C39B H39D O1 0.98 1.91 2.75(4) 141.8 4_656


# start Validation Reply Form
_vrf_PLAT417_Tpstar_100K         
;
PROBLEM: short inter D-H..H-D 
RESPONSE: The alert is related to the hydrogen atoms of lattice 
solvent molecule.It is very difficult to locate hydrogen atoms accurately 
using X-ray data because these atoms have low scattering power.Thes
result is the best.
;
_olex2_submission_special_instructions 'No special instructions were received'
####################################################################### 
# 
# 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_Tp3Me_100K
_database_code_depnum_ccdc_archive 'CCDC 1974449'
loop_
_audit_author_name
_audit_author_address
'Xin-Hua Zhao'
;Southern University of Science and Technology
China
;
_audit_update_record             
;
2020-03-27 deposited with the CCDC.	2020-04-01 downloaded from the CCDC.
;
_audit_creation_date             2020-03-17
_audit_creation_method           
;
Olex2 1.2
(compiled 2018.05.29 svn.r3508 for OlexSys, GUI svn.r5506)
;
_shelx_SHELXL_version_number     2014/7
_chemical_name_common            ?
_chemical_name_systematic        ?
_chemical_formula_moiety         'C66 H66 B2 Fe3 N22, 2(C H2 Cl2), 5(C H4 O)'
_chemical_formula_sum            'C73 H90 B2 Cl4 Fe3 N22 O5'
_chemical_formula_weight         1686.63
_chemical_melting_point          ?
loop_
_atom_type_symbol
_atom_type_description
_atom_type_scat_dispersion_real
_atom_type_scat_dispersion_imag
_atom_type_scat_source
C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
B B 0.0013 0.0007 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Cl Cl 0.1484 0.1585 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Fe Fe 0.3463 0.8444 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'

_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      monoclinic
_space_group_IT_number           15
_space_group_name_H-M_alt        'C 1 2/c 1'
_space_group_name_Hall           '-C 2yc'
loop_
_space_group_symop_operation_xyz
'x, y, z'
'-x, y, -z+1/2'
'x+1/2, y+1/2, z'
'-x+1/2, y+1/2, -z+1/2'
'-x, -y, -z'
'x, -y, z-1/2'
'-x+1/2, -y+1/2, -z'
'x+1/2, -y+1/2, z-1/2'

_cell_length_a                   18.4576(12)
_cell_length_b                   20.1964(13)
_cell_length_c                   23.1855(12)
_cell_angle_alpha                90
_cell_angle_beta                 113.46
_cell_angle_gamma                90
_cell_volume                     7928.8(8)
_cell_formula_units_Z            4
_cell_measurement_reflns_used    7341
_cell_measurement_temperature    100(2)
_cell_measurement_theta_max      24.663
_cell_measurement_theta_min      2.822
_shelx_estimated_absorpt_T_max   ?
_shelx_estimated_absorpt_T_min   ?
_exptl_absorpt_coefficient_mu    0.741
_exptl_absorpt_correction_T_max  0.7451
_exptl_absorpt_correction_T_min  0.6642
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   
'SADABS-2016/2 (Bruker,2016/2) was used for absorption correction. wR2(int) was 0.0801 before and 0.0552 after correction. The Ratio of minimum to maximum transmission is 0.8914. The λ/2 correction factor is Not present.'
_exptl_absorpt_special_details   ?
_exptl_crystal_colour            'dark red'
_exptl_crystal_colour_modifier   dark
_exptl_crystal_colour_primary    red
_exptl_crystal_density_diffrn    1.413
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    ?
_exptl_crystal_description       block
_exptl_crystal_F_000             3512
_exptl_crystal_size_max          0.2
_exptl_crystal_size_mid          0.15
_exptl_crystal_size_min          0.11
_exptl_transmission_factor_max   ?
_exptl_transmission_factor_min   ?
_diffrn_reflns_av_R_equivalents  0.0538
_diffrn_reflns_av_unetI/netI     0.0449
_diffrn_reflns_Laue_measured_fraction_full 0.991
_diffrn_reflns_Laue_measured_fraction_max 0.991
_diffrn_reflns_limit_h_max       19
_diffrn_reflns_limit_h_min       -21
_diffrn_reflns_limit_k_max       23
_diffrn_reflns_limit_k_min       -23
_diffrn_reflns_limit_l_max       27
_diffrn_reflns_limit_l_min       -27
_diffrn_reflns_number            28328
_diffrn_reflns_point_group_measured_fraction_full 0.991
_diffrn_reflns_point_group_measured_fraction_max 0.991
_diffrn_reflns_theta_full        24.818
_diffrn_reflns_theta_max         24.818
_diffrn_reflns_theta_min         2.233
_diffrn_ambient_temperature      100.0
_diffrn_detector_area_resol_mean ?
_diffrn_measured_fraction_theta_full 0.991
_diffrn_measured_fraction_theta_max 0.991
_diffrn_measurement_device_type  'Bruker APEX-II CCD'
_diffrn_measurement_method       'φ and ω scans'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_source                   ?
_diffrn_standards_number         0
_reflns_Friedel_coverage         0.000
_reflns_Friedel_fraction_full    .
_reflns_Friedel_fraction_max     .
_reflns_number_gt                5288
_reflns_number_total             6788
_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       'SAINT V8.38A (?, 2016)'
_computing_data_collection       'Bruker APEX3'
_computing_data_reduction        'SAINT V8.38A (?, 2016)'
_computing_molecular_graphics    'Olex2 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 (Dolomanov et al., 2009)'
_computing_structure_refinement  'XL (Sheldrick, 2008)'
_computing_structure_solution    'olex2.solve (Bourhis et al., 2015)'
_refine_diff_density_max         0.947
_refine_diff_density_min         -1.023
_refine_diff_density_rms         0.091
_refine_ls_extinction_coef       .
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.052
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     574
_refine_ls_number_reflns         6788
_refine_ls_number_restraints     195
_refine_ls_R_factor_all          0.0960
_refine_ls_R_factor_gt           0.0754
_refine_ls_restrained_S_all      1.062
_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)+(0.0977P)²+48.3672P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1937
_refine_ls_wR_factor_ref         0.2095
_refine_special_details          ?
_olex2_refinement_description    
;
1. Fixed Uiso
 At 1.2 times of:
  All B(H) groups, All C(H) groups, All C(H,H) groups, All C(H,H,H,H) groups
 At 1.5 times of:
  All C(H,H,H) groups, All C(H,H,H,H,H,H) groups, All O(H) groups
2. Restrained distances
 O2B-C35B = O2A-C35A
 1.42 with sigma of 0.02
 Cl1B-C37A = Cl2B-C37B = Cl2A-C37B = Cl1A-C37A
 1.79 with sigma of 0.02
 O3-C36
 1.42 with sigma of 0.02
 O1B-C34
 1.45 with sigma of 0.02
 Cl1B-Cl1A = Cl2B-Cl2A
 2.9 with sigma of 0.04
3. Rigid bond restraints
 C17, C8, C9, C10, C11, C16
 with sigma for 1-2 distances of 0.01 and sigma for 1-3 distances of 0.01
 C11, C16, C15, C14, C13, C12
 with sigma for 1-2 distances of 0.02 and sigma for 1-3 distances of 0.02
4. Uiso/Uaniso restraints and constraints
O2B \\sim C35B: within 2A with sigma of 0.01 and sigma for terminal atoms of
0.02
Cl1A \\sim Cl1B \\sim Cl2A \\sim Cl2B \\sim O3 \\sim C36 \\sim C37A \\sim C37B:
within 2A with sigma of 0.01 and sigma for terminal atoms of 0.02
Uanis(C11) \\sim Ueq, Uanis(C16) \\sim Ueq, Uanis(C17) \\sim Ueq, Uanis(C8)
\\sim Ueq, Uanis(C9) \\sim Ueq, Uanis(C10) \\sim Ueq: with sigma of 0.02 and
sigma for terminal atoms of 0.04
Uanis(C13) \\sim Ueq, Uanis(C12) \\sim Ueq, Uanis(C11) \\sim Ueq, Uanis(C16)
\\sim Ueq, Uanis(C15) \\sim Ueq, Uanis(C14) \\sim Ueq: with sigma of 0.02 and
sigma for terminal atoms of 0.04
Uanis(Cl1B) \\sim Ueq, Uanis(C37A) \\sim Ueq, Uanis(Cl1A) \\sim Ueq: with sigma
of 0.01 and sigma for terminal atoms of 0.02
Uanis(C35B) \\sim Ueq, Uanis(O2B) \\sim Ueq: with sigma of 0.01 and sigma for
terminal atoms of 0.02
Uanis(C37A) = Uanis(C37B)
Uanis(Cl1B) = Uanis(Cl2B)
Uanis(O1A) = Uanis(O1B)
Uanis(O2A) = Uanis(O2B)
Uanis(C35A) = Uanis(C35B)
Uanis(Cl1A) = Uanis(Cl2A)
5. Others
 Sof(H7BC)=Sof(H7BD)=Sof(C17)=Sof(H17)=Sof(C8)=Sof(C9)=Sof(H9)=Sof(C10)=
 Sof(H10)=Sof(C11)=Sof(C16)=Sof(C15)=Sof(H15)=Sof(C14)=Sof(H14)=Sof(C13)=
 Sof(H13)=Sof(C12)=Sof(H12)=1-FVAR(1)
 Sof(H7AA)=Sof(H7AB)=Sof(C9A)=Sof(H9A)=Sof(C8A)=Sof(C17A)=Sof(H17A)=Sof(C16A)=
 Sof(H16A)=Sof(C15A)=Sof(C10A)=Sof(C11A)=Sof(H11A)=Sof(C12A)=Sof(H12A)=
 Sof(C13A)=Sof(H13A)=Sof(C14A)=Sof(H14A)=FVAR(1)
 Sof(Cl2A)=Sof(Cl2B)=Sof(C37B)=Sof(H37C)=Sof(H37D)=1-FVAR(2)
 Sof(Cl1A)=Sof(Cl1B)=Sof(C37A)=Sof(H37A)=Sof(H37B)=FVAR(2)
 Sof(O1B)=Sof(H1B)=Sof(H34D)=Sof(H34E)=Sof(H34F)=1-FVAR(3)
 Sof(O1A)=Sof(H1AA)=Sof(H34A)=Sof(H34B)=Sof(H34C)=FVAR(3)
 Sof(O2B)=Sof(H2B)=Sof(C35B)=Sof(H35D)=Sof(H35E)=Sof(H35F)=1-FVAR(4)
 Sof(O2A)=Sof(H2A)=Sof(C35A)=Sof(H35A)=Sof(H35B)=Sof(H35C)=FVAR(4)
 Fixed Sof: O3(0.5) H3A(0.5) C36(0.5) H36A(0.5) H36B(0.5) H36C(0.5)
6.a Ternary CH refined with riding coordinates:
 B1(H1A)
6.b Secondary CH2 refined with riding coordinates:
 C6(H6A,H6B), C7(H7AA,H7AB), C7(H7BC,H7BD), C18(H18A,H18B), C37A(H37A,H37B),
 C37B(H37C,H37D)
6.c Me refined with everything fixed:
 C34(H34A,H34B,H34C), C34(H34D,H34E,H34F), C36(H36A,H36B,H36C)
6.d Aromatic/amide H refined with riding coordinates:
 C1(H1), C2(H2), C3(H3), C4(H4), C9A(H9A), C17A(H17A), C16A(H16A), C11A(H11A),
 C12A(H12A), C13A(H13A), C14A(H14A), C17(H17), C9(H9), C10(H10), C15(H15),
 C14(H14), C13(H13), C12(H12), C22(H22), C23(H23), C26(H26), C27(H27), C30(H30),
  C31(H31)
6.e Naphthalene refined as free rotating group:
 C9A(C8A,C17A,C16A,C15A,C10A,C11A,C12A,C13A,C14A), C17(C8,C9,C10,C11,C16,C15,
 C14,C13,C12)
6.f Idealised Me refined as rotating group:
 C25(H25A,H25B,H25C), C29(H29A,H29B,H29C), C33(H33A,H33B,H33C), C35A(H35A,H35B,
 H35C), C35B(H35D,H35E,H35F)
6.g Idealised tetrahedral OH refined with riding coordinates:
 O3(H3A)
6.h Idealised tetrahedral OH refined as rotating group:
 O1A(H1AA), O1B(H1B), O2A(H2A), O2B(H2B)
;
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     iterative
_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
Fe1 Fe 0.5000 0.56519(4) 0.7500 0.0266(3) Uani 1 2 d S T P . .
Fe2 Fe 0.31670(4) 0.38602(4) 0.63014(3) 0.0400(3) Uani 1 1 d . . . . .
Cl1A Cl 0.5479(2) 0.87238(19) 0.6861(2) 0.1316(13) Uani 0.775(4) 1 d D U . A 1
Cl1B Cl 0.5380(3) 0.7679(3) 0.5968(2) 0.1431(15) Uani 0.775(4) 1 d D U . A 1
Cl2A Cl 0.4965(8) 0.9020(7) 0.5519(7) 0.1316(13) Uani 0.225(4) 1 d D U . A 2
Cl2B Cl 0.5945(11) 0.7900(10) 0.6321(8) 0.1431(15) Uani 0.225(4) 1 d D U . A 2
O1A O 0.4161(9) 0.0611(6) 0.7239(6) 0.134(4) Uani 0.639(9) 1 d . . . B 1
H1AA H 0.3851 0.0935 0.7161 0.201 Uiso 0.639(9) 1 calc GR . . B 1
O1B O 0.4544(12) 0.0322(11) 0.6703(10) 0.134(4) Uani 0.361(9) 1 d D . . B 2
H1B H 0.4912 0.0329 0.7063 0.201 Uiso 0.361(9) 1 calc GR . . B 2
O2A O 0.8400(6) 0.6003(6) 0.8100(5) 0.114(3) Uani 0.762(13) 1 d D . . C 1
H2A H 0.8330 0.6384 0.8214 0.172 Uiso 0.762(13) 1 calc GR . . C 1
O2B O 0.860(2) 0.6153(18) 0.7851(16) 0.114(3) Uani 0.238(13) 1 d D U . C 2
H2B H 0.8538 0.6545 0.7940 0.172 Uiso 0.238(13) 1 calc GR . . C 2
O3 O 0.4609(13) 0.9550(11) 0.5056(12) 0.216(8) Uani 0.5 1 d D U . D -1
H3A H 0.4603 0.9134 0.5043 0.323 Uiso 0.5 1 calc R . . D -1
N1 N 0.5486(2) 0.56745(18) 0.68780(16) 0.0324(9) Uani 1 1 d . . . . .
N2 N 0.5810(3) 0.6383(2) 0.78962(18) 0.0458(12) Uani 1 1 d . . . . .
N3 N 0.4266(2) 0.49690(18) 0.70558(16) 0.0263(8) Uani 1 1 d . . . . .
N4 N 0.3566(3) 0.4455(2) 0.52433(19) 0.0489(12) Uani 1 1 d . . . . .
N5 N 0.1934(4) 0.4948(4) 0.6090(3) 0.091(2) Uani 1 1 d . . . . .
N6 N 0.2434(3) 0.2571(3) 0.5908(2) 0.0576(14) Uani 1 1 d . . . . .
N7 N 0.2390(3) 0.3221(3) 0.57203(19) 0.0515(13) Uani 1 1 d . . . . .
N8 N 0.3863(3) 0.2540(2) 0.65814(19) 0.0535(14) Uani 1 1 d . . . . .
N9 N 0.4029(3) 0.3187(2) 0.64845(18) 0.0417(11) Uani 1 1 d . . . . .
N10 N 0.2915(3) 0.2786(3) 0.7046(2) 0.0678(17) Uani 1 1 d . . . . .
N11 N 0.2926(3) 0.3467(3) 0.70078(19) 0.0547(14) Uani 1 1 d . . . . .
C1 C 0.5201(3) 0.5408(2) 0.62951(19) 0.0308(10) Uani 1 1 d . . . . .
H1 H 0.4688 0.5218 0.6135 0.037 Uiso 1 1 calc R . . . .
C2 C 0.5628(3) 0.5402(2) 0.5924(2) 0.0366(11) Uani 1 1 d . . . . .
H2 H 0.5412 0.5207 0.5517 0.044 Uiso 1 1 calc R . . . .
C3 C 0.6372(3) 0.5680(3) 0.6146(2) 0.0465(14) Uani 1 1 d . . . . .
H3 H 0.6677 0.5679 0.5898 0.056 Uiso 1 1 calc R . . . .
C4 C 0.6664(4) 0.5962(3) 0.6739(2) 0.0579(17) Uani 1 1 d . . . . .
H4 H 0.7171 0.6163 0.6904 0.069 Uiso 1 1 calc R . . . .
C5 C 0.6210(4) 0.5949(3) 0.7087(2) 0.0454(14) Uani 1 1 d . . . . .
C6 C 0.6498(4) 0.6202(3) 0.7748(2) 0.0564(17) Uani 1 1 d . . . . .
H6A H 0.6815 0.5856 0.8044 0.068 Uiso 1 1 calc R . . . .
H6B H 0.6838 0.6595 0.7796 0.068 Uiso 1 1 calc R . . . .
C7 C 0.6086(4) 0.6470(3) 0.8602(2) 0.0480(14) Uani 1 1 d . . . . .
H7AA H 0.6211 0.6027 0.8800 0.058 Uiso 0.659(8) 1 calc R . . E 1
H7AB H 0.5640 0.6650 0.8688 0.058 Uiso 0.659(8) 1 calc R . . E 1
H7BC H 0.6402 0.6078 0.8813 0.058 Uiso 0.341(8) 1 calc R . . E 2
H7BD H 0.5617 0.6483 0.8708 0.058 Uiso 0.341(8) 1 calc R . . E 2
C9A C 0.6652(3) 0.7580(3) 0.9016(3) 0.047(3) Uani 0.659(8) 1 d . . . E 1
H9A H 0.6122 0.7721 0.8900 0.056 Uiso 0.659(8) 1 calc R . . E 1
C8A C 0.6813(4) 0.6924(2) 0.8929(3) 0.048(3) Uani 0.659(8) 1 d G . . E 1
C17A C 0.7590(4) 0.6718(2) 0.9099(3) 0.055(3) Uani 0.659(8) 1 d G . . E 1
H17A H 0.7700 0.6270 0.9040 0.066 Uiso 0.659(8) 1 calc R . . E 1
C16A C 0.8205(3) 0.7168(2) 0.9356(3) 0.058(3) Uani 0.659(8) 1 d G . . E 1
H16A H 0.8735 0.7027 0.9472 0.070 Uiso 0.659(8) 1 calc R . . E 1
C15A C 0.8044(3) 0.7824(2) 0.94423(17) 0.054(3) Uani 0.659(8) 1 d G . . E 1
C10A C 0.7268(3) 0.8030(2) 0.92725(19) 0.050(3) Uani 0.659(8) 1 d G . . E 1
C11A C 0.7107(3) 0.8686(2) 0.9359(3) 0.066(3) Uani 0.659(8) 1 d G . . E 1
H11A H 0.6576 0.8827 0.9243 0.079 Uiso 0.659(8) 1 calc R . . E 1
C12A C 0.7722(4) 0.9136(2) 0.9616(3) 0.072(3) Uani 0.659(8) 1 d G . . E 1
H12A H 0.7612 0.9585 0.9675 0.086 Uiso 0.659(8) 1 calc R . . E 1
C13A C 0.8498(4) 0.8930(2) 0.9786(3) 0.062(3) Uani 0.659(8) 1 d G . . E 1
H13A H 0.8919 0.9238 0.9961 0.074 Uiso 0.659(8) 1 calc R . . E 1
C14A C 0.8659(3) 0.8274(3) 0.9699(2) 0.065(3) Uani 0.659(8) 1 d G . . E 1
H14A H 0.9190 0.8133 0.9815 0.078 Uiso 0.659(8) 1 calc R . . E 1
C17 C 0.7394(7) 0.7000(5) 0.9066(7) 0.066(5) Uani 0.341(8) 1 d . U . E 2
H17 H 0.7591 0.6574 0.9030 0.079 Uiso 0.341(8) 1 calc R . . E 2
C8 C 0.6585(7) 0.7099(6) 0.8869(8) 0.046(5) Uani 0.341(8) 1 d G U . E 2
C9 C 0.6297(6) 0.7722(7) 0.8922(7) 0.063(5) Uani 0.341(8) 1 d G U . E 2
H9 H 0.5744 0.7790 0.8787 0.075 Uiso 0.341(8) 1 calc R . . E 2
C10 C 0.6817(7) 0.8245(6) 0.9171(6) 0.075(6) Uani 0.341(8) 1 d G U . E 2
H10 H 0.6620 0.8671 0.9207 0.090 Uiso 0.341(8) 1 calc R . . E 2
C11 C 0.7625(6) 0.8146(5) 0.9368(4) 0.075(6) Uani 0.341(8) 1 d G U . E 2
C16 C 0.7913(6) 0.7523(5) 0.9316(4) 0.068(5) Uani 0.341(8) 1 d G U . E 2
C15 C 0.8722(6) 0.7424(6) 0.9513(6) 0.076(6) Uani 0.341(8) 1 d G U . E 2
H15 H 0.8919 0.6999 0.9477 0.091 Uiso 0.341(8) 1 calc R . . E 2
C14 C 0.9242(6) 0.7948(8) 0.9762(5) 0.075(5) Uani 0.341(8) 1 d G U . E 2
H14 H 0.9794 0.7880 0.9897 0.090 Uiso 0.341(8) 1 calc R . . E 2
C13 C 0.8953(8) 0.8571(7) 0.9815(5) 0.073(6) Uani 0.341(8) 1 d G U . E 2
H13 H 0.9309 0.8929 0.9986 0.088 Uiso 0.341(8) 1 calc R . . E 2
C12 C 0.8145(8) 0.8670(5) 0.9618(5) 0.079(6) Uani 0.341(8) 1 d G U . E 2
H12 H 0.7948 0.9096 0.9654 0.095 Uiso 0.341(8) 1 calc R . . E 2
C18 C 0.5422(4) 0.6998(2) 0.7551(2) 0.067(2) Uani 1 1 d . . . . .
H18A H 0.5686 0.7393 0.7799 0.081 Uiso 1 1 calc R . . . .
H18B H 0.5470 0.7017 0.7141 0.081 Uiso 1 1 calc R . . . .
C19 C 0.3871(3) 0.4524(2) 0.68025(19) 0.0296(10) Uani 1 1 d . . . . .
C20 C 0.3394(3) 0.4231(2) 0.5629(2) 0.0368(11) Uani 1 1 d . . . . .
C21 C 0.2379(4) 0.4529(4) 0.6155(3) 0.0583(16) Uani 1 1 d . . . . .
C22 C 0.4502(4) 0.2159(3) 0.6701(2) 0.067(2) Uani 1 1 d . . . . .
H22 H 0.4537 0.1696 0.6784 0.080 Uiso 1 1 calc R . . . .
C23 C 0.5079(4) 0.2542(3) 0.6683(2) 0.0573(16) Uani 1 1 d . . . . .
H23 H 0.5598 0.2402 0.6750 0.069 Uiso 1 1 calc R . . . .
C24 C 0.4786(3) 0.3182(3) 0.6548(2) 0.0421(13) Uani 1 1 d . . . . .
C25 C 0.5210(3) 0.3776(2) 0.6479(2) 0.0408(12) Uani 1 1 d . . . . .
H25A H 0.4889 0.4004 0.6087 0.061 Uiso 1 1 calc GR . . . .
H25B H 0.5714 0.3644 0.6467 0.061 Uiso 1 1 calc GR . . . .
H25C H 0.5307 0.4073 0.6836 0.061 Uiso 1 1 calc GR . . . .
C26 C 0.1889(4) 0.2218(3) 0.5454(2) 0.065(2) Uani 1 1 d . . . . .
H26 H 0.1805 0.1755 0.5465 0.077 Uiso 1 1 calc R . . . .
C27 C 0.1477(4) 0.2633(3) 0.4975(3) 0.0633(19) Uani 1 1 d . . . . .
H27 H 0.1043 0.2517 0.4597 0.076 Uiso 1 1 calc R . . . .
C28 C 0.1807(3) 0.3254(3) 0.5140(2) 0.0558(16) Uani 1 1 d . . . . .
C29 C 0.1582(4) 0.3877(3) 0.4766(3) 0.0658(18) Uani 1 1 d . . . . .
H29A H 0.1595 0.4247 0.5044 0.099 Uiso 1 1 calc GR . . . .
H29B H 0.1048 0.3832 0.4439 0.099 Uiso 1 1 calc GR . . . .
H29C H 0.1955 0.3962 0.4570 0.099 Uiso 1 1 calc GR . . . .
C30 C 0.2778(4) 0.2609(5) 0.7552(3) 0.083(3) Uani 1 1 d . . . . .
H30 H 0.2754 0.2169 0.7687 0.100 Uiso 1 1 calc R . . . .
C31 C 0.2679(4) 0.3171(5) 0.7835(3) 0.085(3) Uani 1 1 d . . . . .
H31 H 0.2561 0.3195 0.8198 0.102 Uiso 1 1 calc R . . . .
C32 C 0.2782(4) 0.3699(4) 0.7496(3) 0.065(2) Uani 1 1 d . . . . .
C33 C 0.2771(4) 0.4416(4) 0.7635(3) 0.077(2) Uani 1 1 d . . . . .
H33A H 0.3256 0.4624 0.7647 0.116 Uiso 1 1 calc GR . . . .
H33B H 0.2736 0.4471 0.8043 0.116 Uiso 1 1 calc GR . . . .
H33C H 0.2312 0.4624 0.7307 0.116 Uiso 1 1 calc GR . . . .
C34 C 0.3814(6) 0.0094(6) 0.6751(5) 0.115(3) Uani 1 1 d D . . . .
H34A H 0.3311 0.0252 0.6435 0.173 Uiso 0.6393 1 calc . . . B 1
H34B H 0.3724 -0.0310 0.6947 0.173 Uiso 0.6393 1 calc . . . B 1
H34C H 0.4178 -0.0002 0.6549 0.173 Uiso 0.6393 1 calc . . . B 1
H34D H 0.3598 -0.0283 0.6468 0.173 Uiso 0.3607 1 calc . . . B 2
H34E H 0.3427 0.0455 0.6633 0.173 Uiso 0.3607 1 calc . . . B 2
H34F H 0.3930 -0.0042 0.7185 0.173 Uiso 0.3607 1 calc . . . B 2
C35A C 0.9195(10) 0.5887(9) 0.8291(10) 0.159(6) Uani 0.762(13) 1 d D . . C 1
H35A H 0.9275 0.5482 0.8091 0.239 Uiso 0.762(13) 1 calc GR . . C 1
H35B H 0.9436 0.5835 0.8749 0.239 Uiso 0.762(13) 1 calc GR . . C 1
H35C H 0.9441 0.6262 0.8169 0.239 Uiso 0.762(13) 1 calc GR . . C 1
C35B C 0.836(5) 0.571(3) 0.822(3) 0.159(6) Uani 0.238(13) 1 d D U . C 2
H35D H 0.7812 0.5576 0.7981 0.239 Uiso 0.238(13) 1 calc GR . . C 2
H35E H 0.8409 0.5928 0.8609 0.239 Uiso 0.238(13) 1 calc GR . . C 2
H35F H 0.8700 0.5314 0.8321 0.239 Uiso 0.238(13) 1 calc GR . . C 2
C36 C 0.495(2) 0.9764(18) 0.5696(14) 0.210(9) Uani 0.5 1 d D U . D -1
H36A H 0.4576 1.0060 0.5776 0.315 Uiso 0.5 1 calc . . . F -1
H36B H 0.5441 1.0000 0.5778 0.315 Uiso 0.5 1 calc . . . G -1
H36C H 0.5052 0.9378 0.5974 0.315 Uiso 0.5 1 calc . . . H -1
C37A C 0.5856(11) 0.8428(9) 0.6333(8) 0.148(3) Uani 0.775(4) 1 d D U . A 1
H37A H 0.6430 0.8348 0.6557 0.178 Uiso 0.775(4) 1 calc R . . A 1
H37B H 0.5783 0.8767 0.6006 0.178 Uiso 0.775(4) 1 calc R . . A 1
C37B C 0.563(3) 0.8763(16) 0.6288(15) 0.148(3) Uani 0.225(4) 1 d D U . A 2
H37C H 0.5363 0.8823 0.6582 0.178 Uiso 0.225(4) 1 calc R . . A 2
H37D H 0.6098 0.9053 0.6431 0.178 Uiso 0.225(4) 1 calc R . . A 2
B1 B 0.3051(5) 0.2372(4) 0.6554(3) 0.065(2) Uani 1 1 d . . . . .
H1A H 0.3011 0.1889 0.6633 0.078 Uiso 1 1 calc R . . . .


_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
Fe1 N1 1.979(4) 2_656 ?
Fe1 N1 1.979(4) . ?
Fe1 N2 2.040(4) . ?
Fe1 N2 2.040(4) 2_656 ?
Fe1 N3 1.920(4) . ?
Fe1 N3 1.920(4) 2_656 ?
Fe2 N7 2.001(4) . ?
Fe2 N9 2.005(5) . ?
Fe2 N11 2.022(4) . ?
Fe2 C19 1.906(5) . ?
Fe2 C20 1.921(5) . ?
Fe2 C21 1.913(8) . ?
Cl1A C37A 1.738(14) . ?
Cl1B C37A 1.785(14) . ?
Cl2A C37B 1.79(2) . ?
Cl2B C37B 1.83(2) . ?
O1A C34 1.485(15) . ?
O1B C34 1.470(16) . ?
O2A C35A 1.373(15) . ?
O2B C35B 1.43(2) . ?
O3 C36 1.430(18) . ?
N1 C1 1.352(5) . ?
N1 C5 1.346(7) . ?
N2 C6 1.486(8) . ?
N2 C7 1.518(5) . ?
N2 C18 1.497(7) . ?
N3 C19 1.159(6) . ?
N4 C20 1.153(6) . ?
N5 C21 1.147(9) . ?
N6 N7 1.375(7) . ?
N6 C26 1.335(7) . ?
N6 B1 1.531(8) . ?
N7 C28 1.350(7) . ?
N8 N9 1.382(6) . ?
N8 C22 1.342(9) . ?
N8 B1 1.513(9) . ?
N9 C24 1.347(7) . ?
N10 N11 1.379(8) . ?
N10 C30 1.342(7) . ?
N10 B1 1.514(10) . ?
N11 C32 1.346(8) . ?
C1 C2 1.381(7) . ?
C2 C3 1.380(7) . ?
C3 C4 1.385(7) . ?
C4 C5 1.376(8) . ?
C5 C6 1.498(7) . ?
C7 C8A 1.552(6) . ?
C7 C8 1.547(10) . ?
C9A C8A 1.3900 . ?
C9A C10A 1.3900 . ?
C8A C17A 1.3900 . ?
C17A C16A 1.3900 . ?
C16A C15A 1.3900 . ?
C15A C10A 1.3900 . ?
C15A C14A 1.3900 . ?
C10A C11A 1.3900 . ?
C11A C12A 1.3900 . ?
C12A C13A 1.3900 . ?
C13A C14A 1.3900 . ?
C17 C8 1.3900 . ?
C17 C16 1.3900 . ?
C8 C9 1.3900 . ?
C9 C10 1.3900 . ?
C10 C11 1.3900 . ?
C11 C16 1.3900 . ?
C11 C12 1.3900 . ?
C16 C15 1.3900 . ?
C15 C14 1.3900 . ?
C14 C13 1.3900 . ?
C13 C12 1.3900 . ?
C18 C18 1.479(15) 2_656 ?
C22 C23 1.331(9) . ?
C23 C24 1.389(8) . ?
C24 C25 1.474(7) . ?
C26 C27 1.358(9) . ?
C27 C28 1.380(8) . ?
C28 C29 1.490(9) . ?
C30 C31 1.359(12) . ?
C31 C32 1.384(10) . ?
C32 C33 1.484(11) . ?

loop_
_geom_angle_atom_site_label_1
_geom_angle_atom_site_label_2
_geom_angle_atom_site_label_3
_geom_angle
_geom_angle_site_symmetry_1
_geom_angle_site_symmetry_3
_geom_angle_publ_flag
N1 Fe1 N1 177.4(2) . 2_656 ?
N1 Fe1 N2 81.27(16) 2_656 2_656 ?
N1 Fe1 N2 81.27(16) . . ?
N1 Fe1 N2 96.80(17) 2_656 . ?
N1 Fe1 N2 96.80(17) . 2_656 ?
N2 Fe1 N2 87.3(3) 2_656 . ?
N3 Fe1 N1 88.84(15) 2_656 . ?
N3 Fe1 N1 88.84(15) . 2_656 ?
N3 Fe1 N1 93.06(15) . . ?
N3 Fe1 N1 93.06(15) 2_656 2_656 ?
N3 Fe1 N2 174.27(15) 2_656 2_656 ?
N3 Fe1 N2 174.26(15) . . ?
N3 Fe1 N2 92.52(17) . 2_656 ?
N3 Fe1 N2 92.52(17) 2_656 . ?
N3 Fe1 N3 88.2(2) 2_656 . ?
N7 Fe2 N9 90.03(19) . . ?
N7 Fe2 N11 87.84(18) . . ?
N9 Fe2 N11 88.5(2) . . ?
C19 Fe2 N7 175.3(2) . . ?
C19 Fe2 N9 93.25(18) . . ?
C19 Fe2 N11 95.67(18) . . ?
C19 Fe2 C20 84.53(19) . . ?
C19 Fe2 C21 84.1(2) . . ?
C20 Fe2 N7 91.97(18) . . ?
C20 Fe2 N9 91.4(2) . . ?
C20 Fe2 N11 179.8(2) . . ?
C21 Fe2 N7 92.6(2) . . ?
C21 Fe2 N9 177.4(2) . . ?
C21 Fe2 N11 91.4(3) . . ?
C21 Fe2 C20 88.7(3) . . ?
C1 N1 Fe1 127.6(3) . . ?
C5 N1 Fe1 114.8(3) . . ?
C5 N1 C1 117.4(4) . . ?
C6 N2 Fe1 105.0(3) . . ?
C6 N2 C7 109.0(5) . . ?
C6 N2 C18 110.6(4) . . ?
C7 N2 Fe1 116.1(3) . . ?
C18 N2 Fe1 104.5(3) . . ?
C18 N2 C7 111.3(4) . . ?
C19 N3 Fe1 174.8(4) . . ?
N7 N6 B1 119.2(4) . . ?
C26 N6 N7 109.2(5) . . ?
C26 N6 B1 131.6(5) . . ?
N6 N7 Fe2 117.8(3) . . ?
C28 N7 Fe2 135.5(4) . . ?
C28 N7 N6 106.6(4) . . ?
N9 N8 B1 119.0(6) . . ?
C22 N8 N9 110.0(5) . . ?
C22 N8 B1 130.9(6) . . ?
N8 N9 Fe2 117.9(4) . . ?
C24 N9 Fe2 136.9(4) . . ?
C24 N9 N8 105.2(5) . . ?
N11 N10 B1 119.5(4) . . ?
C30 N10 N11 109.5(6) . . ?
C30 N10 B1 131.0(6) . . ?
N10 N11 Fe2 117.2(4) . . ?
C32 N11 Fe2 136.5(5) . . ?
C32 N11 N10 106.3(5) . . ?
N1 C1 C2 122.4(4) . . ?
C3 C2 C1 119.6(4) . . ?
C2 C3 C4 118.3(5) . . ?
C5 C4 C3 119.2(5) . . ?
N1 C5 C4 123.1(4) . . ?
N1 C5 C6 114.0(4) . . ?
C4 C5 C6 122.8(5) . . ?
N2 C6 C5 109.4(5) . . ?
N2 C7 C8A 116.7(5) . . ?
N2 C7 C8 114.7(7) . . ?
C8A C9A C10A 120.0 . . ?
C9A C8A C7 116.2(4) . . ?
C9A C8A C17A 120.0 . . ?
C17A C8A C7 123.7(4) . . ?
C16A C17A C8A 120.0 . . ?
C17A C16A C15A 120.0 . . ?
C16A C15A C14A 120.0 . . ?
C10A C15A C16A 120.0 . . ?
C10A C15A C14A 120.0 . . ?
C15A C10A C9A 120.0 . . ?
C11A C10A C9A 120.0 . . ?
C11A C10A C15A 120.0 . . ?
C10A C11A C12A 120.0 . . ?
C11A C12A C13A 120.0 . . ?
C14A C13A C12A 120.0 . . ?
C13A C14A C15A 120.0 . . ?
C8 C17 C16 120.0 . . ?
C17 C8 C7 113.8(8) . . ?
C9 C8 C7 126.2(8) . . ?
C9 C8 C17 120.0 . . ?
C10 C9 C8 120.0 . . ?
C9 C10 C11 120.0 . . ?
C10 C11 C12 120.0 . . ?
C16 C11 C10 120.0 . . ?
C16 C11 C12 120.0 . . ?
C11 C16 C17 120.0 . . ?
C15 C16 C17 120.0 . . ?
C15 C16 C11 120.0 . . ?
C16 C15 C14 120.0 . . ?
C13 C14 C15 120.0 . . ?
C12 C13 C14 120.0 . . ?
C13 C12 C11 120.0 . . ?
C18 C18 N2 109.6(4) 2_656 . ?
N3 C19 Fe2 173.2(4) . . ?
N4 C20 Fe2 176.9(4) . . ?
N5 C21 Fe2 176.6(6) . . ?
C23 C22 N8 108.0(5) . . ?
C22 C23 C24 107.7(6) . . ?
N9 C24 C23 109.0(5) . . ?
N9 C24 C25 123.7(5) . . ?
C23 C24 C25 127.3(6) . . ?
N6 C26 C27 108.5(5) . . ?
C26 C27 C28 106.9(5) . . ?
N7 C28 C27 108.7(5) . . ?
N7 C28 C29 123.3(5) . . ?
C27 C28 C29 128.0(5) . . ?
N10 C30 C31 108.0(7) . . ?
C30 C31 C32 107.1(6) . . ?
N11 C32 C31 109.1(7) . . ?
N11 C32 C33 123.1(6) . . ?
C31 C32 C33 127.7(6) . . ?
Cl1A C37A Cl1B 111.5(9) . . ?
Cl2A C37B Cl2B 113.4(18) . . ?
N8 B1 N6 108.7(5) . . ?
N8 B1 N10 107.6(5) . . ?
N10 B1 N6 108.1(7) . . ?


# start Validation Reply Form
_vrf_PLAT420_Tp3Me_100K          
;
PROBLEM: D-H Without Acceptor 
RESPONSE: These level B alerts are related to the hydrogen atoms of lattice 
solvent molecules.It is very difficult to locate hydrogen atoms accurately 
using X-ray data because these atoms have low scattering power.
;
_olex2_submission_special_instructions 'No special instructions were received'
