# Electronic Supplementary Material (ESI) for Dalton Transactions.
# This journal is © The Royal Society of Chemistry 2021

####################################################################### 
# 
# 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_cambpp-01a_500k_manual
_database_code_depnum_ccdc_archive 'CCDC 2085819'
loop_
_audit_author_name
_audit_author_address
'Pierre LeMaguere'
;Rigaku Americas Corporation
United States of America
;
_audit_update_record             
;
2021-05-25 deposited with the CCDC.	2021-07-28 downloaded from the CCDC.
;
_audit_creation_date             2018-05-09
_audit_creation_method           
;
Olex2 1.2
(compiled 2018.04.26 svn.r3504 for OlexSys, GUI svn.r5492)
;
_shelx_SHELXL_version_number     2014/7
_chemical_name_common            ?
_chemical_name_systematic        ?
_chemical_formula_moiety         'C24 H20 Fe N12 O2, 2(B F4)'
_chemical_formula_sum            'C24 H20 B2 F8 Fe N12 O2'
_chemical_formula_weight         737.99
_chemical_melting_point          ?
_chemical_oxdiff_formula         'C24 H20 B2 F8 Fe N12 O2'
_chemical_oxdiff_usercomment     'ruby test crystal'
loop_
_atom_type_symbol
_atom_type_description
_atom_type_scat_dispersion_real
_atom_type_scat_dispersion_imag
_atom_type_scat_source
C C 0.0181 0.0091 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
B B 0.0090 0.0039 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
F F 0.0727 0.0534 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Fe Fe -1.1336 3.1974 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
N N 0.0311 0.0180 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
O O 0.0492 0.0322 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'

_shelx_space_group_comment       
;
The symmetry employed for this shelxl refinement is uniquely defined
by the following loop, which should always be used as a source of
symmetry information in preference to the above space-group names.
They are only intended as comments.
;
_space_group_crystal_system      monoclinic
_space_group_IT_number           14
_space_group_name_H-M_alt        'P 1 21/n 1'
_space_group_name_Hall           '-P 2yn'
loop_
_space_group_symop_operation_xyz
'x, y, z'
'-x+1/2, y+1/2, -z+1/2'
'-x, -y, -z'
'x-1/2, -y-1/2, z-1/2'

_cell_length_a                   9.3506(6)
_cell_length_b                   33.3034(10)
_cell_length_c                   10.8189(8)
_cell_angle_alpha                90
_cell_angle_beta                 107.460(7)
_cell_angle_gamma                90
_cell_volume                     3213.9(3)
_cell_formula_units_Z            4
_cell_measurement_reflns_used    5586
_cell_measurement_temperature    499.99(10)
_cell_measurement_theta_max      73.8620
_cell_measurement_theta_min      4.4700
_shelx_estimated_absorpt_T_max   ?
_shelx_estimated_absorpt_T_min   ?
_exptl_absorpt_coefficient_mu    4.595
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.54078
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   
;
CrysAlisPro 1.171.40.3a (Rigaku Oxford Diffraction, 2018)
Empirical absorption correction using spherical harmonics,
 implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_absorpt_special_details   ?
_exptl_crystal_colour            'dark brown'
_exptl_crystal_colour_modifier   dark
_exptl_crystal_colour_primary    brown
_exptl_crystal_density_diffrn    1.525
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    ?
_exptl_crystal_description       block
_exptl_crystal_F_000             1488
loop_
_exptl_crystal_face_index_h
_exptl_crystal_face_index_k
_exptl_crystal_face_index_l
_exptl_crystal_face_perp_dist
0 21 1 0.1046
6 0 -2 0.0795
0 -21 -1 0.0906
-6 0 2 0.0561
0 0 -7 0.0363
0 0 7 0.0363
-2 -11 6 0.0727
2 12 5 0.0726
1 -15 5 0.0681
3 2 4 0.0544

_exptl_crystal_size_max          0.208
_exptl_crystal_size_mid          0.137
_exptl_crystal_size_min          0.073
loop_
_exptl_oxdiff_crystal_face_indexfrac_h
_exptl_oxdiff_crystal_face_indexfrac_k
_exptl_oxdiff_crystal_face_indexfrac_l
_exptl_oxdiff_crystal_face_x
_exptl_oxdiff_crystal_face_y
_exptl_oxdiff_crystal_face_z
0.0244 21.4130 0.8721 0.4455 0.1853 0.8759
6.0662 -0.1795 -2.2991 -0.8127 -0.3363 0.4759
0.3636 -21.3703 -1.0169 -0.4964 -0.2063 -0.8432
-6.0651 0.4133 2.3083 0.8174 0.3382 -0.4663
0.0750 -0.0196 -7.0156 0.3008 -0.9931 -0.0999
-0.0750 0.0196 7.0156 -0.3008 0.9931 0.0999
-2.0544 -11.0029 6.0014 -0.2096 0.8211 -0.5273
1.9359 12.0343 5.0224 -0.2402 0.7423 0.7245
0.9531 -14.9891 5.0311 -0.7089 0.6671 -0.4455
2.9504 2.0316 4.0368 -0.5766 0.5721 0.3942

_exptl_transmission_factor_max   ?
_exptl_transmission_factor_min   ?
_diffrn_reflns_av_R_equivalents  0.0432
_diffrn_reflns_av_unetI/netI     0.0465
_diffrn_reflns_Laue_measured_fraction_full 0.996
_diffrn_reflns_Laue_measured_fraction_max 0.996
_diffrn_reflns_limit_h_max       11
_diffrn_reflns_limit_h_min       -10
_diffrn_reflns_limit_k_max       39
_diffrn_reflns_limit_k_min       -30
_diffrn_reflns_limit_l_max       12
_diffrn_reflns_limit_l_min       -12
_diffrn_reflns_number            18409
_diffrn_reflns_point_group_measured_fraction_full 0.996
_diffrn_reflns_point_group_measured_fraction_max 0.996
_diffrn_reflns_theta_full        67.076
_diffrn_reflns_theta_max         67.076
_diffrn_reflns_theta_min         4.485
_diffrn_ambient_environment      air
_diffrn_ambient_temperature      499.99(10)
_diffrn_detector                 'CCD plate'
_diffrn_detector_area_resol_mean ?
_diffrn_detector_type            HyPix
_diffrn_measured_fraction_theta_full 0.996
_diffrn_measured_fraction_theta_max 0.996
_diffrn_measurement_details      
;
List of Runs (angles in degrees, time in seconds):

  # Type    Start    End  Width  tₑₓₚ   ω     θ     κ     φ   Frames
#--------------------------------------------------------------------------
  1  ω    -61.00  22.00   0.50   12.00    --  -49.80  57.00-120.00  166
  2  ω    -43.00 -14.00   0.50   57.00    --  -84.25 125.00  60.00   58
  3  ω    -91.00 -63.00   0.50   57.00    --  -84.25 125.00  60.00   56
  4  ω    -93.00 -57.00   0.50   12.00    --  -49.80   0.00  90.00   72
  5  ω   -123.00 -91.00   0.50   57.00    --  -84.25   0.00  90.00   64
  6  ω   -119.00 -73.00   0.50   12.00    --  -49.80-125.00-120.00   92
  7  ω   -118.00 -91.00   0.50   12.00    --  -49.80-125.00-150.00   54
  8  ω    -82.00 -51.00   0.50   12.00    --  -49.80   0.00-150.00   62
  9  ω     36.00  73.00   0.50   57.00    --  105.75 -57.00 -30.00   74
 10  ω     40.00  83.00   0.50   57.00    --  105.75 -57.00   0.00   86
 11  ω     43.00  83.00   0.50   57.00    --  105.75 -57.00  60.00   80
 12  ω     52.00 111.00   0.50   57.00    --  105.75 -19.00  90.00  118
 13  ω     79.00 105.00   0.50   57.00    --  105.75   0.00  90.00   52
 14  ω     37.00  62.00   0.50   57.00    --  105.75 -37.00  90.00   50
 15  ω     34.00  59.00   0.50   57.00    --  105.75 -37.00  60.00   50
 16  ω     39.00 103.00   0.50   57.00    --  105.75-125.00  30.00  128
 17  ω     45.00  83.00   0.50   57.00    --  105.75 -57.00-120.00   76
 18  ω     46.00  86.00   0.50   57.00    --  105.75 -57.00-150.00   80
 19  ω     73.00 111.00   0.50   57.00    --  105.75   0.00-120.00   76
 20  ω     34.00  59.00   0.50   57.00    --  105.75 -37.00-180.00   50
 21  ω     36.00  61.00   0.50   57.00    --  105.75 -37.00-150.00   50
;
_diffrn_measurement_device       'four-circle diffractometer'
_diffrn_measurement_device_type  'XtaLAB Synergy, Dualflex, HyPix'
_diffrn_measurement_method       'ω scans'
_diffrn_orient_matrix_type       
'CrysAlisPro convention (1999,Acta A55,543-557)'
_diffrn_orient_matrix_UB_11      -0.1501753000
_diffrn_orient_matrix_UB_12      0.0227918000
_diffrn_orient_matrix_UB_13      -0.0445478000
_diffrn_orient_matrix_UB_21      -0.0017112000
_diffrn_orient_matrix_UB_22      0.0028905000
_diffrn_orient_matrix_UB_23      0.1415233000
_diffrn_orient_matrix_UB_31      0.0853409000
_diffrn_orient_matrix_UB_32      0.0401949000
_diffrn_orient_matrix_UB_33      0.0150369000
_diffrn_radiation_monochromator  mirror
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           CuK\a
_diffrn_radiation_wavelength     1.54184
_diffrn_source                   'micro-focus sealed X-ray tube'
_diffrn_source_type              'PhotonJet (Cu) X-ray Source'
_reflns_Friedel_coverage         0.000
_reflns_Friedel_fraction_full    .
_reflns_Friedel_fraction_max     .
_reflns_number_gt                3434
_reflns_number_total             5715
_reflns_odcompleteness_completeness 99.57
_reflns_odcompleteness_iscentric 1
_reflns_odcompleteness_theta     66.97
_reflns_special_details          
;
 Reflections were merged by SHELXL according to the crystal
 class for the calculation of statistics and refinement.
 
 _reflns_Friedel_fraction is defined as the number of unique
 Friedel pairs measured divided by the number that would be
 possible theoretically, ignoring centric projections and
 systematic absences.
;
_reflns_threshold_expression     'I > 2σ(I)'
_computing_cell_refinement       'CrysAlisPro 1.171.40.3a (Rigaku OD, 2018)'
_computing_data_collection       'CrysAlisPro 1.171.40.3a (Rigaku OD, 2018)'
_computing_data_reduction        'CrysAlisPro 1.171.40.3a (Rigaku OD, 2018)'
_computing_molecular_graphics    'Olex2 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 (Dolomanov et al., 2009)'
_computing_structure_refinement  'ShelXL (Sheldrick, 2015)'
_computing_structure_solution    'ShelXT (Sheldrick, 2015)'
_refine_diff_density_max         0.233
_refine_diff_density_min         -0.230
_refine_diff_density_rms         0.044
_refine_ls_extinction_coef       0.00052(18)
_refine_ls_extinction_expression Fc^*^=kFc[1+0.001xFc²λ³/sin(2θ)]^-1/4^
_refine_ls_extinction_method     'SHELXL-2014/7 (Sheldrick 2014'
_refine_ls_goodness_of_fit_ref   1.008
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     499
_refine_ls_number_reflns         5715
_refine_ls_number_restraints     108
_refine_ls_R_factor_all          0.0858
_refine_ls_R_factor_gt           0.0575
_refine_ls_restrained_S_all      1.043
_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)+(0.1302P)²] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1712
_refine_ls_wR_factor_ref         0.1988
_refine_special_details          ?
_olex2_refinement_description    
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups, All N(H,H) groups
2. Restrained distances
 F00L-B019 \\sim F00K-B019 \\sim F2-B019 \\sim F015-B019 \\sim F01E-B019 \\sim
F00R-B019 \\sim F01D-B019
 with sigma of 0.01
 F0AA-B01A \\sim F00P-B01A \\sim F01C-B01A \\sim F0-B01A \\sim F014-B01A \\sim
F1-B01A
 with sigma of 0.01
3. Uiso/Uaniso restraints and constraints
F00K \\sim F00L \\sim F01D \\sim F01E \\sim F015 \\sim F2: within 2A with sigma
of 0.01 and sigma for terminal atoms of 0.02
F01C \\sim F1 \\sim F014 \\sim F0 \\sim F016 \\sim F0AA: within 2A with sigma
of 0.01 and sigma for terminal atoms of 0.02
4. Others
 Sof(F0AA)=Sof(F0)=Sof(F1)=1-FVAR(1)
 Sof(F014)=Sof(F016)=Sof(F01C)=FVAR(1)
 Sof(F00L)=Sof(F2)=Sof(F01E)=1-FVAR(2)
 Sof(F00K)=Sof(F015)=Sof(F01D)=FVAR(2)
5.a Aromatic/amide H refined with riding coordinates:
 C00H(H00H), C00J(H00J), C00N(H00N), C00O(H00O), C00Q(H00Q), C00S(H00S),
 C00V(H00V), C00W(H00W), C00X(H00X), C010(H010), C011(H011), C012(H012),
 C013(H013), C017(H017), C018(H018), C01B(H01B)
5.b X=CH2 refined with riding coordinates:
 N00M(H00A,H00B), N00Y(H00C,H00D)
;
_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
Fe01 Fe 0.79269(7) 0.36980(2) 0.71943(6) 0.1006(3) Uani 1 1 d . . . . .
N002 N 0.7858(3) 0.43054(7) 0.7539(3) 0.0945(7) Uani 1 1 d . . . . .
N003 N 0.7372(4) 0.41227(8) 0.9400(3) 0.1034(8) Uani 1 1 d . . . . .
N004 N 0.7904(3) 0.30805(8) 0.6984(3) 0.0963(8) Uani 1 1 d . . . . .
N005 N 0.7481(4) 0.37390(8) 0.8996(3) 0.1089(9) Uani 1 1 d . . . . .
N006 N 0.5408(4) 0.31523(8) 0.6068(3) 0.1068(8) Uani 1 1 d . . . . .
N007 N 0.8347(4) 0.43865(9) 0.5622(3) 0.1136(9) Uani 1 1 d . . . . .
N008 N 0.5693(4) 0.35558(9) 0.6220(4) 0.1214(10) Uani 1 1 d . . . . .
N009 N 1.0408(4) 0.31206(10) 0.7887(3) 0.1162(9) Uani 1 1 d . . . . .
C00A C 0.6618(4) 0.28890(10) 0.6466(4) 0.0994(9) Uani 1 1 d . . . . .
C00B C 0.7570(4) 0.44370(9) 0.8595(4) 0.1008(10) Uani 1 1 d . . . . .
N00C N 0.8381(5) 0.39771(10) 0.5603(4) 0.1277(11) Uani 1 1 d . . . . .
C00D C 0.8046(4) 0.45675(10) 0.6670(4) 0.1018(10) Uani 1 1 d . . . . .
O00E O 0.8970(5) 0.16262(9) 0.6822(5) 0.1769(16) Uani 1 1 d . . . . .
N00F N 1.0173(4) 0.35225(11) 0.7924(4) 0.1248(10) Uani 1 1 d . . . . .
C00G C 0.9153(5) 0.28716(10) 0.7390(4) 0.1026(10) Uani 1 1 d . . . . .
C00H C 0.9189(6) 0.24575(11) 0.7337(4) 0.1164(12) Uani 1 1 d . . . . .
H00H H 1.0085 0.2316 0.7629 0.140 Uiso 1 1 calc R . . . .
C00I C 0.7837(6) 0.22627(11) 0.6834(4) 0.1162(13) Uani 1 1 d . . . . .
C00J C 0.6525(5) 0.24773(11) 0.6363(4) 0.1150(12) Uani 1 1 d . . . . .
H00J H 0.5614 0.2349 0.5992 0.138 Uiso 1 1 calc R . . . .
F00K F 0.3793(17) 0.5043(3) 0.8364(14) 0.215(4) Uani 0.551(11) 1 d D U P A 1
C00L C 0.7618(6) 0.51085(10) 0.7913(5) 0.1281(14) Uani 1 1 d . . . . .
N00M N 0.6576(6) 0.16299(10) 0.6751(5) 0.178(2) Uani 1 1 d . . . . .
H00A H 0.6499 0.1373 0.6695 0.213 Uiso 1 1 calc R . . . .
H00B H 0.5813 0.1773 0.6758 0.213 Uiso 1 1 calc R . . . .
C00N C 0.7432(5) 0.48384(10) 0.8834(5) 0.1243(14) Uani 1 1 d . . . . .
H00N H 0.7224 0.4926 0.9579 0.149 Uiso 1 1 calc R . . . .
C00O C 0.7946(5) 0.49742(11) 0.6832(5) 0.1262(14) Uani 1 1 d . . . . .
H00O H 0.8096 0.5154 0.6224 0.151 Uiso 1 1 calc R . . . .
F00P F 0.3261(6) 0.21742(15) 0.9107(5) 0.254(3) Uani 1 1 d D . . . .
C00Q C 0.7166(5) 0.35149(13) 0.9884(5) 0.1271(14) Uani 1 1 d . . . . .
H00Q H 0.7156 0.3236 0.9872 0.152 Uiso 1 1 calc R . . . .
F00R F 0.3987(6) 0.44197(16) 0.8404(6) 0.271(3) Uani 1 1 d D . . . .
C00S C 0.6993(6) 0.41282(15) 1.0502(5) 0.1343(14) Uani 1 1 d . . . . .
H00S H 0.6849 0.4354 1.0958 0.161 Uiso 1 1 calc R . . . .
C00T C 0.7858(7) 0.18037(12) 0.6825(5) 0.1394(18) Uani 1 1 d . . . . .
O00U O 0.8478(7) 0.57655(11) 0.8001(8) 0.276(4) Uani 1 1 d . . . . .
C00V C 0.4385(7) 0.37291(16) 0.5774(6) 0.1465(18) Uani 1 1 d . . . . .
H00V H 0.4234 0.4005 0.5751 0.176 Uiso 1 1 calc R . . . .
C00W C 0.8749(6) 0.45367(19) 0.4624(5) 0.1471(16) Uani 1 1 d . . . . .
H00W H 0.8824 0.4807 0.4439 0.177 Uiso 1 1 calc R . . . .
C00X C 1.1512(8) 0.36842(19) 0.8352(6) 0.155(2) Uani 1 1 d . . . . .
H00X H 1.1694 0.3958 0.8476 0.186 Uiso 1 1 calc R . . . .
N00Y N 0.6342(8) 0.56873(12) 0.8324(9) 0.250(4) Uani 1 1 d . . . . .
H00C H 0.6245 0.5941 0.8428 0.300 Uiso 1 1 calc R . . . .
H00D H 0.5651 0.5524 0.8381 0.300 Uiso 1 1 calc R . . . .
C00Z C 0.7501(8) 0.55543(13) 0.8088(7) 0.172(2) Uani 1 1 d . . . . .
C010 C 0.3930(6) 0.30841(17) 0.5525(5) 0.1402(15) Uani 1 1 d . . . . .
H010 H 0.3460 0.2836 0.5317 0.168 Uiso 1 1 calc R . . . .
C011 C 0.6862(7) 0.37397(16) 1.0815(6) 0.1424(17) Uani 1 1 d . . . . .
H011 H 0.6611 0.3645 1.1532 0.171 Uiso 1 1 calc R . . . .
C012 C 1.2594(8) 0.3399(3) 0.8589(7) 0.182(3) Uani 1 1 d . . . . .
H012 H 1.3623 0.3442 0.8900 0.219 Uiso 1 1 calc R . . . .
C013 C 1.1892(7) 0.3041(3) 0.8287(6) 0.165(2) Uani 1 1 d . . . . .
H013 H 1.2343 0.2790 0.8344 0.198 Uiso 1 1 calc R . . . .
F014 F 0.5264(15) 0.1897(3) 0.8655(15) 0.244(5) Uani 0.576(8) 1 d D U P B 1
F015 F 0.1783(8) 0.4677(4) 0.7290(16) 0.213(4) Uani 0.551(11) 1 d D U P A 1
F016 F 0.5338(19) 0.2511(4) 0.9001(15) 0.286(6) Uani 0.576(8) 1 d . U P B 1
C017 C 0.3269(7) 0.3452(2) 0.5345(6) 0.165(2) Uani 1 1 d . . . . .
H017 H 0.2250 0.3504 0.4997 0.198 Uiso 1 1 calc R . . . .
C018 C 0.8786(8) 0.3890(2) 0.4571(6) 0.167(2) Uani 1 1 d . . . . .
H018 H 0.8897 0.3629 0.4304 0.200 Uiso 1 1 calc R . . . .
B019 B 0.3252(7) 0.47156(15) 0.7688(6) 0.147(2) Uani 1 1 d D . . . .
B01A B 0.4410(8) 0.22199(19) 0.8625(8) 0.176(3) Uani 1 1 d D . . . .
C01B C 0.9024(8) 0.4225(3) 0.3940(6) 0.171(2) Uani 1 1 d . . . . .
H01B H 0.9316 0.4236 0.3191 0.205 Uiso 1 1 calc R . . . .
F01C F 0.3714(11) 0.2256(3) 0.7326(8) 0.217(3) Uani 0.576(8) 1 d D U P B 1
F01D F 0.3857(16) 0.4719(4) 0.6720(11) 0.234(4) Uani 0.551(11) 1 d D U P A 1
F0AA F 0.4671(14) 0.2599(3) 0.8344(16) 0.195(4) Uani 0.424(8) 1 d D U P B 2
F0 F 0.5316(19) 0.2078(6) 0.9767(13) 0.280(6) Uani 0.424(8) 1 d D U P B 2
F1 F 0.4433(18) 0.1908(4) 0.7857(15) 0.218(5) Uani 0.424(8) 1 d D U P B 2
F00L F 0.388(2) 0.5069(3) 0.7650(18) 0.218(6) Uani 0.449(11) 1 d D U P A 2
F2 F 0.2079(14) 0.4795(5) 0.8091(16) 0.230(5) Uani 0.449(11) 1 d D U P A 2
F01E F 0.262(2) 0.4584(4) 0.6492(9) 0.219(5) Uani 0.449(11) 1 d D U P A 2


_geom_special_details            
;
 All esds (except the esd in the dihedral angle between two l.s. planes)
 are estimated using the full covariance matrix.  The cell esds are taken
 into account individually in the estimation of esds in distances, angles
 and torsion angles; correlations between esds in cell parameters are only
 used when they are defined by crystal symmetry.  An approximate (isotropic)
 treatment of cell esds is used for estimating esds involving l.s. planes.
;
loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
_geom_bond_publ_flag
Fe01 N002 2.061(2) . ?
Fe01 N004 2.068(3) . ?
Fe01 N005 2.117(4) . ?
Fe01 N008 2.092(4) . ?
Fe01 N00C 2.109(4) . ?
Fe01 N00F 2.093(4) . ?
N002 C00B 1.325(5) . ?
N002 C00D 1.332(5) . ?
N003 N005 1.364(4) . ?
N003 C00B 1.409(5) . ?
N003 C00S 1.343(5) . ?
N004 C00A 1.328(4) . ?
N004 C00G 1.316(4) . ?
N005 C00Q 1.318(5) . ?
N006 N008 1.370(4) . ?
N006 C00A 1.393(5) . ?
N006 C010 1.349(6) . ?
N007 N00C 1.364(5) . ?
N007 C00D 1.386(5) . ?
N007 C00W 1.342(6) . ?
N008 C00V 1.307(6) . ?
N009 N00F 1.359(5) . ?
N009 C00G 1.406(5) . ?
N009 C013 1.350(6) . ?
C00A C00J 1.376(5) . ?
C00B C00N 1.375(5) . ?
N00C C018 1.314(7) . ?
C00D C00O 1.372(5) . ?
O00E C00T 1.197(6) . ?
N00F C00X 1.313(7) . ?
C00G C00H 1.381(5) . ?
C00H H00H 0.9300 . ?
C00H C00I 1.379(6) . ?
C00I C00J 1.379(6) . ?
C00I C00T 1.529(5) . ?
C00J H00J 0.9300 . ?
F00K B019 1.325(7) . ?
C00L C00N 1.391(6) . ?
C00L C00O 1.371(6) . ?
C00L C00Z 1.505(5) . ?
N00M H00A 0.8600 . ?
N00M H00B 0.8600 . ?
N00M C00T 1.312(7) . ?
C00N H00N 0.9300 . ?
C00O H00O 0.9300 . ?
F00P B01A 1.336(6) . ?
C00Q H00Q 0.9300 . ?
C00Q C011 1.352(7) . ?
F00R B019 1.313(5) . ?
C00S H00S 0.9300 . ?
C00S C011 1.352(6) . ?
O00U C00Z 1.179(6) . ?
C00V H00V 0.9300 . ?
C00V C017 1.367(8) . ?
C00W H00W 0.9300 . ?
C00W C01B 1.343(8) . ?
C00X H00X 0.9300 . ?
C00X C012 1.354(9) . ?
N00Y H00C 0.8600 . ?
N00Y H00D 0.8600 . ?
N00Y C00Z 1.266(7) . ?
C010 H010 0.9300 . ?
C010 C017 1.359(8) . ?
C011 H011 0.9300 . ?
C012 H012 0.9300 . ?
C012 C013 1.353(10) . ?
C013 H013 0.9300 . ?
F014 B01A 1.335(7) . ?
F015 B019 1.317(7) . ?
F016 B01A 1.283(17) . ?
C017 H017 0.9300 . ?
C018 H018 0.9300 . ?
C018 C01B 1.363(9) . ?
B019 F01D 1.331(7) . ?
B019 F00L 1.323(7) . ?
B019 F2 1.323(7) . ?
B019 F01E 1.325(7) . ?
B01A F01C 1.365(7) . ?
B01A F0AA 1.339(7) . ?
B01A F0 1.357(8) . ?
B01A F1 1.335(8) . ?
C01B H01B 0.9300 . ?

loop_
_geom_angle_atom_site_label_1
_geom_angle_atom_site_label_2
_geom_angle_atom_site_label_3
_geom_angle
_geom_angle_site_symmetry_1
_geom_angle_site_symmetry_3
_geom_angle_publ_flag
N002 Fe01 N004 174.67(11) . . ?
N002 Fe01 N005 75.20(11) . . ?
N002 Fe01 N008 103.46(12) . . ?
N002 Fe01 N00C 74.93(12) . . ?
N002 Fe01 N00F 106.74(13) . . ?
N004 Fe01 N005 99.63(11) . . ?
N004 Fe01 N008 75.14(12) . . ?
N004 Fe01 N00C 110.26(12) . . ?
N004 Fe01 N00F 74.93(13) . . ?
N008 Fe01 N005 92.06(14) . . ?
N008 Fe01 N00C 95.93(16) . . ?
N008 Fe01 N00F 149.76(14) . . ?
N00C Fe01 N005 150.11(11) . . ?
N00F Fe01 N005 97.10(14) . . ?
N00F Fe01 N00C 90.33(15) . . ?
C00B N002 Fe01 120.4(2) . . ?
C00B N002 C00D 119.7(3) . . ?
C00D N002 Fe01 119.8(2) . . ?
N005 N003 C00B 117.5(3) . . ?
C00S N003 N005 111.2(3) . . ?
C00S N003 C00B 131.1(3) . . ?
C00A N004 Fe01 120.1(2) . . ?
C00G N004 Fe01 120.7(3) . . ?
C00G N004 C00A 119.2(3) . . ?
N003 N005 Fe01 114.2(2) . . ?
C00Q N005 Fe01 141.6(3) . . ?
C00Q N005 N003 104.1(3) . . ?
N008 N006 C00A 118.0(3) . . ?
C010 N006 N008 110.8(3) . . ?
C010 N006 C00A 131.2(4) . . ?
N00C N007 C00D 117.3(3) . . ?
C00W N007 N00C 110.3(4) . . ?
C00W N007 C00D 132.2(4) . . ?
N006 N008 Fe01 114.3(2) . . ?
C00V N008 Fe01 140.2(3) . . ?
C00V N008 N006 105.2(4) . . ?
N00F N009 C00G 117.9(3) . . ?
C013 N009 N00F 110.1(5) . . ?
C013 N009 C00G 131.9(5) . . ?
N004 C00A N006 112.1(3) . . ?
N004 C00A C00J 122.6(4) . . ?
C00J C00A N006 125.2(4) . . ?
N002 C00B N003 112.7(3) . . ?
N002 C00B C00N 122.6(3) . . ?
C00N C00B N003 124.7(4) . . ?
N007 N00C Fe01 114.6(3) . . ?
C018 N00C Fe01 140.8(4) . . ?
C018 N00C N007 104.4(4) . . ?
N002 C00D N007 113.2(3) . . ?
N002 C00D C00O 121.9(4) . . ?
C00O C00D N007 124.9(3) . . ?
N009 N00F Fe01 114.6(3) . . ?
C00X N00F Fe01 139.6(4) . . ?
C00X N00F N009 105.6(4) . . ?
N004 C00G N009 111.8(3) . . ?
N004 C00G C00H 123.0(4) . . ?
C00H C00G N009 125.2(4) . . ?
C00G C00H H00H 121.5 . . ?
C00I C00H C00G 117.1(4) . . ?
C00I C00H H00H 121.5 . . ?
C00H C00I C00T 117.4(4) . . ?
C00J C00I C00H 120.7(3) . . ?
C00J C00I C00T 121.8(5) . . ?
C00A C00J C00I 117.3(4) . . ?
C00A C00J H00J 121.3 . . ?
C00I C00J H00J 121.3 . . ?
C00N C00L C00Z 121.2(4) . . ?
C00O C00L C00N 120.6(3) . . ?
C00O C00L C00Z 118.2(4) . . ?
H00A N00M H00B 120.0 . . ?
C00T N00M H00A 120.0 . . ?
C00T N00M H00B 120.0 . . ?
C00B C00N C00L 117.1(4) . . ?
C00B C00N H00N 121.5 . . ?
C00L C00N H00N 121.5 . . ?
C00D C00O H00O 120.9 . . ?
C00L C00O C00D 118.2(4) . . ?
C00L C00O H00O 120.9 . . ?
N005 C00Q H00Q 124.1 . . ?
N005 C00Q C011 111.9(4) . . ?
C011 C00Q H00Q 124.1 . . ?
N003 C00S H00S 127.0 . . ?
N003 C00S C011 106.1(4) . . ?
C011 C00S H00S 127.0 . . ?
O00E C00T C00I 120.4(5) . . ?
O00E C00T N00M 124.1(4) . . ?
N00M C00T C00I 115.4(4) . . ?
N008 C00V H00V 124.4 . . ?
N008 C00V C017 111.2(5) . . ?
C017 C00V H00V 124.4 . . ?
N007 C00W H00W 126.2 . . ?
N007 C00W C01B 107.6(6) . . ?
C01B C00W H00W 126.2 . . ?
N00F C00X H00X 124.5 . . ?
N00F C00X C012 111.0(6) . . ?
C012 C00X H00X 124.5 . . ?
H00C N00Y H00D 120.0 . . ?
C00Z N00Y H00C 120.0 . . ?
C00Z N00Y H00D 120.0 . . ?
O00U C00Z C00L 119.4(5) . . ?
O00U C00Z N00Y 122.6(5) . . ?
N00Y C00Z C00L 118.0(5) . . ?
N006 C010 H010 127.1 . . ?
N006 C010 C017 105.9(5) . . ?
C017 C010 H010 127.1 . . ?
C00Q C011 C00S 106.7(4) . . ?
C00Q C011 H011 126.6 . . ?
C00S C011 H011 126.6 . . ?
C00X C012 H012 126.5 . . ?
C013 C012 C00X 106.9(6) . . ?
C013 C012 H012 126.5 . . ?
N009 C013 C012 106.4(6) . . ?
N009 C013 H013 126.8 . . ?
C012 C013 H013 126.8 . . ?
C00V C017 H017 126.5 . . ?
C010 C017 C00V 107.0(5) . . ?
C010 C017 H017 126.5 . . ?
N00C C018 H018 124.0 . . ?
N00C C018 C01B 112.1(6) . . ?
C01B C018 H018 124.0 . . ?
F00K B019 F01D 104.2(8) . . ?
F00R B019 F00K 104.2(9) . . ?
F00R B019 F015 115.4(7) . . ?
F00R B019 F01D 101.5(7) . . ?
F00R B019 F00L 121.9(9) . . ?
F00R B019 F2 107.1(10) . . ?
F00R B019 F01E 109.1(7) . . ?
F015 B019 F00K 116.7(11) . . ?
F015 B019 F01D 113.0(9) . . ?
F00L B019 F2 104.6(12) . . ?
F00L B019 F01E 109.6(10) . . ?
F2 B019 F01E 102.7(10) . . ?
F00P B01A F01C 102.8(7) . . ?
F00P B01A F0AA 114.8(6) . . ?
F00P B01A F0 87.7(9) . . ?
F014 B01A F00P 116.3(8) . . ?
F014 B01A F01C 101.1(9) . . ?
F016 B01A F00P 120.6(10) . . ?
F016 B01A F014 105.0(12) . . ?
F016 B01A F01C 109.1(9) . . ?
F0AA B01A F0 115.4(12) . . ?
F1 B01A F00P 108.6(9) . . ?
F1 B01A F0AA 123.8(11) . . ?
F1 B01A F0 99.9(10) . . ?
C00W C01B C018 105.7(6) . . ?
C00W C01B H01B 127.2 . . ?
C018 C01B H01B 127.2 . . ?

loop_
_geom_torsion_atom_site_label_1
_geom_torsion_atom_site_label_2
_geom_torsion_atom_site_label_3
_geom_torsion_atom_site_label_4
_geom_torsion
_geom_torsion_site_symmetry_1
_geom_torsion_site_symmetry_2
_geom_torsion_site_symmetry_3
_geom_torsion_site_symmetry_4
_geom_torsion_publ_flag
Fe01 N002 C00B N003 1.4(4) . . . . ?
Fe01 N002 C00B C00N -176.4(3) . . . . ?
Fe01 N002 C00D N007 -3.0(4) . . . . ?
Fe01 N002 C00D C00O 177.2(3) . . . . ?
Fe01 N004 C00A N006 2.7(4) . . . . ?
Fe01 N004 C00A C00J -176.5(3) . . . . ?
Fe01 N004 C00G N009 -2.9(4) . . . . ?
Fe01 N004 C00G C00H 176.4(3) . . . . ?
Fe01 N005 C00Q C011 -174.3(4) . . . . ?
Fe01 N008 C00V C017 -172.5(4) . . . . ?
Fe01 N00C C018 C01B -174.6(5) . . . . ?
Fe01 N00F C00X C012 -174.2(4) . . . . ?
N002 C00B C00N C00L -0.4(7) . . . . ?
N002 C00D C00O C00L -1.1(7) . . . . ?
N003 N005 C00Q C011 0.3(6) . . . . ?
N003 C00B C00N C00L -177.9(4) . . . . ?
N003 C00S C011 C00Q -0.1(6) . . . . ?
N004 C00A C00J C00I 0.5(6) . . . . ?
N004 C00G C00H C00I -0.1(6) . . . . ?
N005 N003 C00B N002 -0.7(5) . . . . ?
N005 N003 C00B C00N 177.1(4) . . . . ?
N005 N003 C00S C011 0.3(6) . . . . ?
N005 C00Q C011 C00S -0.1(7) . . . . ?
N006 N008 C00V C017 0.2(6) . . . . ?
N006 C00A C00J C00I -178.6(3) . . . . ?
N006 C010 C017 C00V 0.8(7) . . . . ?
N007 N00C C018 C01B 0.5(7) . . . . ?
N007 C00D C00O C00L 179.1(4) . . . . ?
N007 C00W C01B C018 -0.6(8) . . . . ?
N008 N006 C00A N004 1.8(4) . . . . ?
N008 N006 C00A C00J -179.0(4) . . . . ?
N008 N006 C010 C017 -0.7(6) . . . . ?
N008 C00V C017 C010 -0.7(8) . . . . ?
N009 N00F C00X C012 0.1(7) . . . . ?
N009 C00G C00H C00I 179.0(4) . . . . ?
C00A N004 C00G N009 178.9(3) . . . . ?
C00A N004 C00G C00H -1.9(5) . . . . ?
C00A N006 N008 Fe01 -5.2(4) . . . . ?
C00A N006 N008 C00V 179.9(4) . . . . ?
C00A N006 C010 C017 179.8(4) . . . . ?
C00B N002 C00D N007 179.7(3) . . . . ?
C00B N002 C00D C00O -0.2(6) . . . . ?
C00B N003 N005 Fe01 -0.3(4) . . . . ?
C00B N003 N005 C00Q -176.6(4) . . . . ?
C00B N003 C00S C011 175.8(4) . . . . ?
N00C N007 C00D N002 1.3(5) . . . . ?
N00C N007 C00D C00O -178.9(4) . . . . ?
N00C N007 C00W C01B 0.9(6) . . . . ?
N00C C018 C01B C00W 0.0(8) . . . . ?
C00D N002 C00B N003 178.8(3) . . . . ?
C00D N002 C00B C00N 0.9(6) . . . . ?
C00D N007 N00C Fe01 0.9(5) . . . . ?
C00D N007 N00C C018 -175.8(4) . . . . ?
C00D N007 C00W C01B 174.8(5) . . . . ?
N00F N009 C00G N004 2.2(5) . . . . ?
N00F N009 C00G C00H -177.0(4) . . . . ?
N00F N009 C013 C012 0.6(7) . . . . ?
N00F C00X C012 C013 0.3(9) . . . . ?
C00G N004 C00A N006 -179.1(3) . . . . ?
C00G N004 C00A C00J 1.7(5) . . . . ?
C00G N009 N00F Fe01 -0.6(4) . . . . ?
C00G N009 N00F C00X -176.5(4) . . . . ?
C00G N009 C013 C012 175.9(5) . . . . ?
C00G C00H C00I C00J 2.4(6) . . . . ?
C00G C00H C00I C00T -177.5(3) . . . . ?
C00H C00I C00J C00A -2.5(6) . . . . ?
C00H C00I C00T O00E -24.9(7) . . . . ?
C00H C00I C00T N00M 158.7(5) . . . . ?
C00J C00I C00T O00E 155.2(5) . . . . ?
C00J C00I C00T N00M -21.2(7) . . . . ?
C00N C00L C00O C00D 1.6(7) . . . . ?
C00N C00L C00Z O00U 127.6(8) . . . . ?
C00N C00L C00Z N00Y -52.4(10) . . . . ?
C00O C00L C00N C00B -0.9(7) . . . . ?
C00O C00L C00Z O00U -51.0(10) . . . . ?
C00O C00L C00Z N00Y 128.9(8) . . . . ?
C00S N003 N005 Fe01 176.0(3) . . . . ?
C00S N003 N005 C00Q -0.3(5) . . . . ?
C00S N003 C00B N002 -176.1(4) . . . . ?
C00S N003 C00B C00N 1.7(7) . . . . ?
C00T C00I C00J C00A 177.3(4) . . . . ?
C00W N007 N00C Fe01 175.7(3) . . . . ?
C00W N007 N00C C018 -0.9(6) . . . . ?
C00W N007 C00D N002 -172.3(5) . . . . ?
C00W N007 C00D C00O 7.6(8) . . . . ?
C00X C012 C013 N009 -0.5(8) . . . . ?
C00Z C00L C00N C00B -179.6(5) . . . . ?
C00Z C00L C00O C00D -179.7(5) . . . . ?
C010 N006 N008 Fe01 175.2(3) . . . . ?
C010 N006 N008 C00V 0.3(5) . . . . ?
C010 N006 C00A N004 -178.7(4) . . . . ?
C010 N006 C00A C00J 0.5(7) . . . . ?
C013 N009 N00F Fe01 175.5(3) . . . . ?
C013 N009 N00F C00X -0.4(5) . . . . ?
C013 N009 C00G N004 -172.9(5) . . . . ?
C013 N009 C00G C00H 7.9(7) . . . . ?

_olex2_submission_special_instructions 'No special instructions were received'
_oxdiff_exptl_absorpt_empirical_details 
;
Empirical correction (ABSPACK) includes:
- Absorption correction using spherical harmonics
- Frame scaling
;
_oxdiff_exptl_absorpt_empirical_full_max 2.284
_oxdiff_exptl_absorpt_empirical_full_min 0.633
_exptl_crystal_preparation       'Magnetic properties'
####################################################################### 
# 
# 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_M171020A
_database_code_depnum_ccdc_archive 'CCDC 2085821'
loop_
_audit_author_name
_audit_author_address
'Hiroki Akutsu'
;Osaka University
Japan
;
_audit_update_record             
;
2021-07-05 deposited with the CCDC.	2021-07-28 downloaded from the CCDC.
;

#==============================================================================
# CHEMICAL DATA

_chemical_formula_sum            'C24 H20 B2 F8 Fe N12 O2'
_chemical_formula_moiety         '2(C12 H10 N6 O) Fe, 2(B F4)'
_chemical_formula_weight         737.96
_chemical_melting_point          ?

#==============================================================================
# CRYSTAL DATA
_space_group_crystal_system      monoclinic
_space_group_name_H-M_alt        'P 1 21/n 1'
_space_group_name_Hall           '-P 2yn'
_space_group_IT_number           14
loop_
_space_group_symop_id
_space_group_symop_operation_xyz
1 +X,+Y,+Z
2 1/2-X,1/2+Y,1/2-Z
3 -X,-Y,-Z
4 -1/2+X,-1/2-Y,-1/2+Z
#------------------------------------------------------------------------------
_cell_length_a                   9.25463(17)
_cell_length_b                   32.5863(6)
_cell_length_c                   10.5351(2)
_cell_angle_alpha                90.0000
_cell_angle_beta                 109.620(8)
_cell_angle_gamma                90.0000
_cell_volume                     2992.66(17)
_cell_formula_units_Z            4
_cell_measurement_reflns_used    23130
_cell_measurement_theta_min      1.88
_cell_measurement_theta_max      27.45
_cell_measurement_temperature    290
#------------------------------------------------------------------------------
_exptl_crystal_description       block
_exptl_crystal_colour            brown
_exptl_crystal_size_max          0.180
_exptl_crystal_size_mid          0.180
_exptl_crystal_size_min          0.130
_exptl_crystal_density_diffrn    1.638
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    'not measured'
_exptl_crystal_F_000             1488.00
_exptl_absorpt_coefficient_mu    0.601
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   'ABSCOR (Rigaku, 1995)'
_exptl_absorpt_correction_T_min  0.853
_exptl_absorpt_correction_T_max  0.925

#==============================================================================
# EXPERIMENTAL DATA

_diffrn_ambient_temperature      290
_diffrn_radiation_type           'Mo K\a'
_diffrn_radiation_wavelength     0.71075
_diffrn_measurement_device_type  'Rigaku R-AXIS RAPID'
_diffrn_measurement_method       ω
_diffrn_detector_area_resol_mean 10.000
_diffrn_reflns_number            29045
_diffrn_reflns_av_unetI/netI     0.0168
_diffrn_reflns_av_R_equivalents  0.0208
_diffrn_reflns_theta_max         27.444
_diffrn_reflns_theta_min         2.145
_diffrn_reflns_theta_full        25.242
_diffrn_measured_fraction_theta_max 1.000
_diffrn_measured_fraction_theta_full 1.000
_diffrn_reflns_Laue_measured_fraction_max 1.000
_diffrn_reflns_Laue_measured_fraction_full 1.000
_diffrn_reflns_point_group_measured_fraction_max 1.000
_diffrn_reflns_point_group_measured_fraction_full 1.000
_diffrn_reflns_limit_h_min       -11
_diffrn_reflns_limit_h_max       11
_diffrn_reflns_limit_k_min       -41
_diffrn_reflns_limit_k_max       42
_diffrn_reflns_limit_l_min       -13
_diffrn_reflns_limit_l_max       13
_diffrn_standards_number         0
_diffrn_standards_interval_count .
_diffrn_standards_decay_%        ?
_reflns_number_total             6819
_reflns_number_gt                5627
_reflns_threshold_expression     F²>2.0σ(F²)
_reflns_Friedel_coverage         0.000
_reflns_Friedel_fraction_max     .
_reflns_Friedel_fraction_full    .

#==============================================================================
# REFINEMENT DATA

_refine_special_details          
;
    Refinement was performed using all reflections. The weighted 
    R-factor (wR) and goodness of fit (S) are based on F².
    R-factor (gt) are based on F. The threshold expression of
    F² > 2.0 sigma(F²) is used only for calculating R-factor (gt).
;
_refine_ls_structure_factor_coef Fsqd
_refine_ls_R_factor_all          0.0507
_refine_ls_R_factor_gt           0.0388
_refine_ls_wR_factor_ref         0.0967
_refine_ls_wR_factor_gt          0.0908
_refine_ls_number_restraints     12
_refine_ls_hydrogen_treatment    mixed
_refine_ls_number_reflns         6819
_refine_ls_number_parameters     514
_refine_ls_goodness_of_fit_ref   1.033
_refine_ls_weighting_scheme      calc
_refine_ls_weighting_details     
'w = 1/[σ²(Fo²)+(0.0440P)²+1.8113P] where P=(Fo²+2Fc²)/3'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_refine_ls_shift/su_max          0.001
_refine_diff_density_max         0.35
_refine_diff_density_min         -0.30
_refine_ls_extinction_method     none
_refine_ls_extinction_coef       ?

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 for Crystallography
(Vol. C, Tables 4.2.6.8 and 6.1.1.4)
;
H H 0.0000 0.0000
;
International Tables for Crystallography
(Vol. C, Table 6.1.1.4)
;
B B 0.0013 0.0007
;
International Tables for Crystallography
(Vol. C, Tables 4.2.6.8 and 6.1.1.4)
;
F F 0.0171 0.0103
;
International Tables for Crystallography
(Vol. C, Tables 4.2.6.8 and 6.1.1.4)
;
Fe Fe 0.3463 0.8444
;
International Tables for Crystallography
(Vol. C, Tables 4.2.6.8 and 6.1.1.4)
;
O O 0.0106 0.0060
;
International Tables for Crystallography
(Vol. C, Tables 4.2.6.8 and 6.1.1.4)
;
N N 0.0061 0.0033
;
International Tables for Crystallography
(Vol. C, Tables 4.2.6.8 and 6.1.1.4)
;

#==============================================================================
# ATOMIC COORDINATES AND THERMAL PARAMETERS

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 0.77994(3) 0.12892(2) 0.71298(3) 0.02855(8) Uani 1 1 d . . . . .
B1 B 0.9297(3) 0.22653(7) 0.3438(3) 0.0608(8) Uani 1 1 d D . . . .
F11 F 0.9782(5) 0.26529(9) 0.3459(6) 0.0733(13) Uani 0.612(9) 1 d D . P A 1
F21 F 0.8925(7) 0.2114(3) 0.2180(6) 0.175(4) Uani 0.612(9) 1 d D . P A 1
F31 F 1.0461(5) 0.2040(2) 0.4290(12) 0.208(5) Uani 0.612(9) 1 d D . P A 1
F12 F 1.0417(14) 0.2541(4) 0.3985(15) 0.175(6) Uani 0.388(9) 1 d D . P A 2
F22 F 0.8522(9) 0.2381(3) 0.2125(5) 0.127(4) Uani 0.388(9) 1 d D . P A 2
F32 F 0.9976(10) 0.19141(14) 0.3313(8) 0.079(3) Uani 0.388(9) 1 d D . P A 2
F4 F 0.8127(2) 0.22230(5) 0.3939(2) 0.0763(5) Uani 1 1 d . . . . .
B2 B 0.3244(3) 0.02480(7) 0.7659(3) 0.0524(7) Uani 1 1 d D . . . .
F5 F 0.4032(2) 0.05678(5) 0.8420(2) 0.0840(5) Uani 1 1 d . . . . .
F61 F 0.3568(14) 0.0243(2) 0.6482(6) 0.105(2) Uani 0.660(17) 1 d D . P B 3
F71 F 0.3848(8) -0.01082(13) 0.8293(7) 0.0797(15) Uani 0.660(17) 1 d D . P B 3
F81 F 0.1722(5) 0.02593(19) 0.7458(12) 0.115(3) Uani 0.660(17) 1 d D . P B 3
F62 F 0.262(2) 0.0365(4) 0.6347(7) 0.094(4) Uani 0.340(17) 1 d D . P B 4
F72 F 0.3932(15) -0.0126(3) 0.783(3) 0.126(6) Uani 0.340(17) 1 d D . P B 4
F82 F 0.1963(11) 0.0184(4) 0.8001(15) 0.100(4) Uani 0.340(17) 1 d D . P B 4
O1 O 0.8979(2) 0.33549(4) 0.68497(19) 0.0547(4) Uani 1 1 d . . . . .
O2 O 0.8656(3) -0.07775(5) 0.8062(3) 0.0873(8) Uani 1 1 d . . . . .
N1 N 0.6452(3) 0.33500(6) 0.6550(3) 0.0544(6) Uani 1 1 d . . . . .
N2 N 0.78030(17) 0.18637(4) 0.68697(16) 0.0299(3) Uani 1 1 d . . . . .
N3 N 1.03548(18) 0.18064(5) 0.78822(18) 0.0360(4) Uani 1 1 d . . . . .
N4 N 1.00018(19) 0.13983(4) 0.79497(17) 0.0344(4) Uani 1 1 d . . . . .
N5 N 0.52500(19) 0.17881(4) 0.59042(17) 0.0348(4) Uani 1 1 d . . . . .
N6 N 0.56083(19) 0.13772(4) 0.61551(17) 0.0342(4) Uani 1 1 d . . . . .
N7 N 0.6371(3) -0.07015(6) 0.8311(3) 0.0786(9) Uani 1 1 d . . . . .
N8 N 0.77865(18) 0.07182(4) 0.74697(16) 0.0298(3) Uani 1 1 d . . . . .
N9 N 0.8315(2) 0.06532(4) 0.55414(17) 0.0344(4) Uani 1 1 d . . . . .
N10 N 0.82106(19) 0.10766(4) 0.55399(17) 0.0343(4) Uani 1 1 d . . . . .
N11 N 0.73159(19) 0.09144(4) 0.93437(17) 0.0334(3) Uani 1 1 d . . . . .
N12 N 0.74059(18) 0.13024(4) 0.88495(17) 0.0326(3) Uani 1 1 d . . . . .
C2 C 0.7795(3) 0.31696(6) 0.6723(2) 0.0417(5) Uani 1 1 d . . . . .
C3 C 0.7776(2) 0.27029(5) 0.6722(2) 0.0361(4) Uani 1 1 d . . . . .
C4 C 0.9166(2) 0.24986(5) 0.7284(2) 0.0371(4) Uani 1 1 d . . . . .
H4 H 1.008879 0.264081 0.761007 0.045 Uiso 1 1 calc R U . . .
C5 C 0.6410(2) 0.24846(5) 0.6202(2) 0.0358(4) Uani 1 1 d . . . . .
H5 H 0.548118 0.261858 0.579638 0.043 Uiso 1 1 calc R U . . .
C6 C 0.9116(2) 0.20747(5) 0.7338(2) 0.0329(4) Uani 1 1 d . . . . .
C7 C 0.6481(2) 0.20618(5) 0.63101(19) 0.0312(4) Uani 1 1 d . . . . .
C8 C 1.1896(2) 0.18594(7) 0.8272(3) 0.0488(5) Uani 1 1 d . . . . .
H8 H 1.240898 0.210686 0.830939 0.059 Uiso 1 1 calc R U . . .
C9 C 1.2548(3) 0.14840(7) 0.8599(3) 0.0525(6) Uani 1 1 d . . . . .
H9 H 1.359073 0.142307 0.890509 0.063 Uiso 1 1 calc R U . . .
C10 C 1.1333(2) 0.12072(6) 0.8380(2) 0.0429(5) Uani 1 1 d . . . . .
H10 H 1.144946 0.092562 0.851998 0.052 Uiso 1 1 calc R U . . .
C11 C 0.3713(2) 0.18392(7) 0.5317(2) 0.0452(5) Uani 1 1 d . . . . .
H11 H 0.319857 0.208706 0.506252 0.054 Uiso 1 1 calc R U . . .
C12 C 0.3068(3) 0.14609(7) 0.5172(3) 0.0529(6) Uani 1 1 d . . . . .
H12 H 0.203123 0.139801 0.479366 0.064 Uiso 1 1 calc R U . . .
C13 C 0.4280(2) 0.11832(6) 0.5707(2) 0.0439(5) Uani 1 1 d . . . . .
H13 H 0.416357 0.090036 0.574111 0.053 Uiso 1 1 calc R U . . .
C15 C 0.7603(3) -0.05622(6) 0.8106(3) 0.0506(6) Uani 1 1 d . . . . .
C16 C 0.7679(3) -0.01024(5) 0.7921(2) 0.0404(5) Uani 1 1 d . . . . .
C17 C 0.7993(2) 0.00314(5) 0.6787(2) 0.0392(5) Uani 1 1 d . . . . .
H17 H 0.817027 -0.015267 0.618100 0.047 Uiso 1 1 calc R U . . .
C18 C 0.7442(3) 0.01715(6) 0.8840(2) 0.0405(5) Uani 1 1 d . . . . .
H18 H 0.724186 0.008165 0.960184 0.049 Uiso 1 1 calc R U . . .
C19 C 0.8030(2) 0.04498(5) 0.6605(2) 0.0325(4) Uani 1 1 d . . . . .
C20 C 0.7519(2) 0.05850(5) 0.8568(2) 0.0316(4) Uani 1 1 d . . . . .
C21 C 0.8809(3) 0.05221(6) 0.4537(2) 0.0409(5) Uani 1 1 d . . . . .
H21 H 0.896849 0.025110 0.434103 0.049 Uiso 1 1 calc R U . . .
C22 C 0.9028(3) 0.08600(7) 0.3871(2) 0.0464(5) Uani 1 1 d . . . . .
H22 H 0.936784 0.086700 0.313446 0.056 Uiso 1 1 calc R U . . .
C23 C 0.8637(3) 0.11963(6) 0.4520(2) 0.0429(5) Uani 1 1 d . . . . .
H23 H 0.867372 0.146833 0.426533 0.051 Uiso 1 1 calc R U . . .
C24 C 0.6953(3) 0.09342(7) 1.0485(2) 0.0420(5) Uani 1 1 d . . . . .
H24 H 0.682295 0.071298 1.099387 0.050 Uiso 1 1 calc R U . . .
C25 C 0.6814(3) 0.13383(7) 1.0748(2) 0.0454(5) Uani 1 1 d . . . . .
H25 H 0.657723 0.144787 1.146904 0.054 Uiso 1 1 calc R U . . .
C26 C 0.7102(2) 0.15551(6) 0.9711(2) 0.0387(4) Uani 1 1 d . . . . .
H26 H 0.708184 0.183963 0.963751 0.046 Uiso 1 1 calc R U . . .
H1N H 0.642(3) 0.3608(9) 0.660(3) 0.066(8) Uiso 1 1 d . . . . .
H2N H 0.576(3) 0.3221(8) 0.674(2) 0.049(7) Uiso 1 1 d . . . . .
H3N H 0.559(4) -0.0533(11) 0.832(3) 0.094(11) Uiso 1 1 d . . . . .
H4N H 0.627(3) -0.0943(9) 0.840(3) 0.065(8) Uiso 1 1 d . . . . .


#==============================================================================
_computing_data_collection       'RAPID AUTO (Rigaku, ????)'
_computing_cell_refinement       'RAPID AUTO'
_computing_data_reduction        'RAPID AUTO'
_computing_structure_solution    'SIR2011 (Burla, et al., 2012)'
_computing_structure_refinement  'SHELXL Version 2018/3 (Sheldrick, 2008)'
_computing_publication_material  'CrystalStructure 4.3 (Rigaku, 2019)'
_computing_molecular_graphics    'CrystalStructure 4.3'

#==============================================================================
# MOLECULAR GEOMETRY

_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 N2 1.8922(14) . ?
Fe1 N8 1.8955(14) . ?
Fe1 N4 1.9608(17) . ?
Fe1 N6 1.9622(17) . ?
Fe1 N10 1.9643(17) . ?
Fe1 N12 1.9647(17) . ?
B1 F32 1.333(4) . ?
B1 F11 1.338(3) . ?
B1 F21 1.346(4) . ?
B1 F12 1.347(5) . ?
B1 F4 1.361(3) . ?
B1 F31 1.363(4) . ?
B1 F22 1.380(4) . ?
B2 F81 1.352(4) . ?
B2 F72 1.360(5) . ?
B2 F62 1.361(4) . ?
B2 F71 1.362(4) . ?
B2 F82 1.366(5) . ?
B2 F5 1.367(3) . ?
B2 F61 1.370(4) . ?
O1 C2 1.219(3) . ?
O2 C15 1.215(3) . ?
N1 C2 1.331(3) . ?
N1 H1N 0.84(3) . ?
N1 H2N 0.84(3) . ?
N2 C7 1.333(2) . ?
N2 C6 1.338(2) . ?
N3 C8 1.356(3) . ?
N3 N4 1.377(2) . ?
N3 C6 1.402(2) . ?
N4 C10 1.318(3) . ?
N5 C11 1.358(3) . ?
N5 N6 1.383(2) . ?
N5 C7 1.397(2) . ?
N6 C13 1.320(3) . ?
N7 C15 1.310(3) . ?
N7 H3N 0.91(4) . ?
N7 H4N 0.80(3) . ?
N8 C20 1.334(2) . ?
N8 C19 1.336(2) . ?
N9 C21 1.355(3) . ?
N9 N10 1.383(2) . ?
N9 C19 1.401(2) . ?
N10 C23 1.322(3) . ?
N11 C24 1.354(3) . ?
N11 N12 1.380(2) . ?
N11 C20 1.400(2) . ?
N12 C26 1.324(2) . ?
C2 C3 1.521(2) . ?
C3 C4 1.392(3) . ?
C3 C5 1.393(3) . ?
C4 C6 1.384(2) . ?
C4 H4 0.9300 . ?
C5 C7 1.382(2) . ?
C5 H5 0.9300 . ?
C8 C9 1.357(3) . ?
C8 H8 0.9300 . ?
C9 C10 1.399(3) . ?
C9 H9 0.9300 . ?
C10 H10 0.9300 . ?
C11 C12 1.355(3) . ?
C11 H11 0.9300 . ?
C12 C13 1.404(3) . ?
C12 H12 0.9300 . ?
C13 H13 0.9300 . ?
C15 C16 1.515(3) . ?
C16 C18 1.387(3) . ?
C16 C17 1.390(3) . ?
C17 C19 1.379(2) . ?
C17 H17 0.9300 . ?
C18 C20 1.384(2) . ?
C18 H18 0.9300 . ?
C21 C22 1.357(3) . ?
C21 H21 0.9300 . ?
C22 C23 1.402(3) . ?
C22 H22 0.9300 . ?
C23 H23 0.9300 . ?
C24 C25 1.360(3) . ?
C24 H24 0.9300 . ?
C25 C26 1.399(3) . ?
C25 H25 0.9300 . ?
C26 H26 0.9300 . ?

loop_
_geom_angle_atom_site_label_1
_geom_angle_atom_site_label_2
_geom_angle_atom_site_label_3
_geom_angle
_geom_angle_site_symmetry_1
_geom_angle_site_symmetry_3
_geom_angle_publ_flag
N2 Fe1 N8 177.33(7) . . ?
N2 Fe1 N4 80.35(6) . . ?
N8 Fe1 N4 99.57(7) . . ?
N2 Fe1 N6 80.30(6) . . ?
N8 Fe1 N6 99.86(6) . . ?
N4 Fe1 N6 160.53(6) . . ?
N2 Fe1 N10 102.43(6) . . ?
N8 Fe1 N10 80.22(6) . . ?
N4 Fe1 N10 88.24(7) . . ?
N6 Fe1 N10 93.86(7) . . ?
N2 Fe1 N12 97.00(6) . . ?
N8 Fe1 N12 80.35(6) . . ?
N4 Fe1 N12 94.41(7) . . ?
N6 Fe1 N12 90.02(7) . . ?
N10 Fe1 N12 160.56(6) . . ?
F11 B1 F21 109.5(4) . . ?
F32 B1 F12 107.1(7) . . ?
F32 B1 F4 114.5(3) . . ?
F11 B1 F4 113.3(3) . . ?
F21 B1 F4 111.8(3) . . ?
F12 B1 F4 120.0(6) . . ?
F11 B1 F31 108.2(4) . . ?
F21 B1 F31 109.6(6) . . ?
F4 B1 F31 104.2(4) . . ?
F32 B1 F22 103.8(5) . . ?
F12 B1 F22 108.2(8) . . ?
F4 B1 F22 101.7(4) . . ?
F72 B2 F62 113.9(8) . . ?
F81 B2 F71 109.5(5) . . ?
F72 B2 F82 103.8(9) . . ?
F62 B2 F82 101.5(8) . . ?
F81 B2 F5 113.2(3) . . ?
F72 B2 F5 118.2(7) . . ?
F62 B2 F5 110.2(4) . . ?
F71 B2 F5 108.1(4) . . ?
F82 B2 F5 107.5(6) . . ?
F81 B2 F61 113.1(4) . . ?
F71 B2 F61 104.8(5) . . ?
F5 B2 F61 107.7(3) . . ?
C2 N1 H1N 119(2) . . ?
C2 N1 H2N 119.6(17) . . ?
H1N N1 H2N 116(3) . . ?
C7 N2 C6 119.96(15) . . ?
C7 N2 Fe1 119.83(12) . . ?
C6 N2 Fe1 120.02(12) . . ?
C8 N3 N4 110.55(16) . . ?
C8 N3 C6 132.59(17) . . ?
N4 N3 C6 116.60(15) . . ?
C10 N4 N3 105.28(16) . . ?
C10 N4 Fe1 141.21(14) . . ?
N3 N4 Fe1 112.45(12) . . ?
C11 N5 N6 110.68(16) . . ?
C11 N5 C7 133.13(16) . . ?
N6 N5 C7 116.18(15) . . ?
C13 N6 N5 105.09(16) . . ?
C13 N6 Fe1 142.33(14) . . ?
N5 N6 Fe1 112.37(11) . . ?
C15 N7 H3N 122(2) . . ?
C15 N7 H4N 120(2) . . ?
H3N N7 H4N 118(3) . . ?
C20 N8 C19 120.08(15) . . ?
C20 N8 Fe1 119.86(12) . . ?
C19 N8 Fe1 120.05(12) . . ?
C21 N9 N10 110.82(15) . . ?
C21 N9 C19 132.74(16) . . ?
N10 N9 C19 116.18(15) . . ?
C23 N10 N9 104.79(16) . . ?
C23 N10 Fe1 141.76(14) . . ?
N9 N10 Fe1 112.61(12) . . ?
C24 N11 N12 110.83(16) . . ?
C24 N11 C20 132.62(16) . . ?
N12 N11 C20 116.44(15) . . ?
C26 N12 N11 104.91(16) . . ?
C26 N12 Fe1 142.54(14) . . ?
N11 N12 Fe1 112.41(11) . . ?
O1 C2 N1 124.05(18) . . ?
O1 C2 C3 120.37(19) . . ?
N1 C2 C3 115.56(19) . . ?
C4 C3 C5 120.68(17) . . ?
C4 C3 C2 117.98(18) . . ?
C5 C3 C2 121.33(18) . . ?
C6 C4 C3 117.14(18) . . ?
C6 C4 H4 121.4 . . ?
C3 C4 H4 121.4 . . ?
C7 C5 C3 117.68(18) . . ?
C7 C5 H5 121.2 . . ?
C3 C5 H5 121.2 . . ?
N2 C6 C4 122.43(18) . . ?
N2 C6 N3 110.32(15) . . ?
C4 C6 N3 127.25(18) . . ?
N2 C7 C5 122.07(17) . . ?
N2 C7 N5 111.06(15) . . ?
C5 C7 N5 126.85(18) . . ?
N3 C8 C9 107.19(19) . . ?
N3 C8 H8 126.4 . . ?
C9 C8 H8 126.4 . . ?
C8 C9 C10 105.9(2) . . ?
C8 C9 H9 127.0 . . ?
C10 C9 H9 127.0 . . ?
N4 C10 C9 111.05(19) . . ?
N4 C10 H10 124.5 . . ?
C9 C10 H10 124.5 . . ?
C12 C11 N5 107.09(19) . . ?
C12 C11 H11 126.5 . . ?
N5 C11 H11 126.5 . . ?
C11 C12 C13 106.2(2) . . ?
C11 C12 H12 126.9 . . ?
C13 C12 H12 126.9 . . ?
N6 C13 C12 110.94(18) . . ?
N6 C13 H13 124.5 . . ?
C12 C13 H13 124.5 . . ?
O2 C15 N7 124.0(2) . . ?
O2 C15 C16 119.6(2) . . ?
N7 C15 C16 116.4(2) . . ?
C18 C16 C17 121.67(17) . . ?
C18 C16 C15 121.39(19) . . ?
C17 C16 C15 116.94(18) . . ?
C19 C17 C16 116.86(18) . . ?
C19 C17 H17 121.6 . . ?
C16 C17 H17 121.6 . . ?
C20 C18 C16 116.80(18) . . ?
C20 C18 H18 121.6 . . ?
C16 C18 H18 121.6 . . ?
N8 C19 C17 122.33(18) . . ?
N8 C19 N9 110.84(15) . . ?
C17 C19 N9 126.83(17) . . ?
N8 C20 C18 122.23(17) . . ?
N8 C20 N11 110.93(15) . . ?
C18 C20 N11 126.83(18) . . ?
N9 C21 C22 107.23(18) . . ?
N9 C21 H21 126.4 . . ?
C22 C21 H21 126.4 . . ?
C21 C22 C23 105.92(19) . . ?
C21 C22 H22 127.0 . . ?
C23 C22 H22 127.0 . . ?
N10 C23 C22 111.24(18) . . ?
N10 C23 H23 124.4 . . ?
C22 C23 H23 124.4 . . ?
N11 C24 C25 107.18(19) . . ?
N11 C24 H24 126.4 . . ?
C25 C24 H24 126.4 . . ?
C24 C25 C26 105.92(19) . . ?
C24 C25 H25 127.0 . . ?
C26 C25 H25 127.0 . . ?
N12 C26 C25 111.15(17) . . ?
N12 C26 H26 124.4 . . ?
C25 C26 H26 124.4 . . ?

loop_
_geom_torsion_atom_site_label_1
_geom_torsion_atom_site_label_2
_geom_torsion_atom_site_label_3
_geom_torsion_atom_site_label_4
_geom_torsion
_geom_torsion_site_symmetry_1
_geom_torsion_site_symmetry_2
_geom_torsion_site_symmetry_3
_geom_torsion_site_symmetry_4
_geom_torsion_publ_flag
N4 Fe1 N2 C7 -177.32(16) . . . . ?
N6 Fe1 N2 C7 4.82(15) . . . . ?
N10 Fe1 N2 C7 96.66(15) . . . . ?
N12 Fe1 N2 C7 -84.01(15) . . . . ?
N4 Fe1 N2 C6 -2.32(15) . . . . ?
N6 Fe1 N2 C6 179.81(16) . . . . ?
N10 Fe1 N2 C6 -88.34(15) . . . . ?
N12 Fe1 N2 C6 90.99(15) . . . . ?
C8 N3 N4 C10 0.0(2) . . . . ?
C6 N3 N4 C10 174.82(18) . . . . ?
C8 N3 N4 Fe1 -170.87(15) . . . . ?
C6 N3 N4 Fe1 4.0(2) . . . . ?
C11 N5 N6 C13 0.4(2) . . . . ?
C7 N5 N6 C13 179.21(18) . . . . ?
C11 N5 N6 Fe1 -175.59(14) . . . . ?
C7 N5 N6 Fe1 3.2(2) . . . . ?
N4 Fe1 N8 C20 94.16(15) . . . . ?
N6 Fe1 N8 C20 -87.06(15) . . . . ?
N10 Fe1 N8 C20 -179.32(16) . . . . ?
N12 Fe1 N8 C20 1.27(15) . . . . ?
N4 Fe1 N8 C19 -86.47(16) . . . . ?
N6 Fe1 N8 C19 92.31(15) . . . . ?
N10 Fe1 N8 C19 0.05(15) . . . . ?
N12 Fe1 N8 C19 -179.36(16) . . . . ?
C21 N9 N10 C23 0.4(2) . . . . ?
C19 N9 N10 C23 175.32(18) . . . . ?
C21 N9 N10 Fe1 -171.42(14) . . . . ?
C19 N9 N10 Fe1 3.5(2) . . . . ?
C24 N11 N12 C26 0.4(2) . . . . ?
C20 N11 N12 C26 176.93(17) . . . . ?
C24 N11 N12 Fe1 -176.32(14) . . . . ?
C20 N11 N12 Fe1 0.3(2) . . . . ?
O1 C2 C3 C4 20.2(3) . . . . ?
N1 C2 C3 C4 -161.3(2) . . . . ?
O1 C2 C3 C5 -161.2(2) . . . . ?
N1 C2 C3 C5 17.4(3) . . . . ?
C5 C3 C4 C6 -1.9(3) . . . . ?
C2 C3 C4 C6 176.72(18) . . . . ?
C4 C3 C5 C7 2.3(3) . . . . ?
C2 C3 C5 C7 -176.33(18) . . . . ?
C7 N2 C6 C4 1.0(3) . . . . ?
Fe1 N2 C6 C4 -174.02(15) . . . . ?
C7 N2 C6 N3 179.90(17) . . . . ?
Fe1 N2 C6 N3 4.9(2) . . . . ?
C3 C4 C6 N2 0.3(3) . . . . ?
C3 C4 C6 N3 -178.45(19) . . . . ?
C8 N3 C6 N2 167.8(2) . . . . ?
N4 N3 C6 N2 -5.6(2) . . . . ?
C8 N3 C6 C4 -13.3(4) . . . . ?
N4 N3 C6 C4 173.24(19) . . . . ?
C6 N2 C7 C5 -0.6(3) . . . . ?
Fe1 N2 C7 C5 174.40(15) . . . . ?
C6 N2 C7 N5 -179.24(17) . . . . ?
Fe1 N2 C7 N5 -4.2(2) . . . . ?
C3 C5 C7 N2 -1.0(3) . . . . ?
C3 C5 C7 N5 177.41(19) . . . . ?
C11 N5 C7 N2 178.9(2) . . . . ?
N6 N5 C7 N2 0.4(2) . . . . ?
C11 N5 C7 C5 0.3(4) . . . . ?
N6 N5 C7 C5 -178.14(19) . . . . ?
N4 N3 C8 C9 -0.2(3) . . . . ?
C6 N3 C8 C9 -173.9(2) . . . . ?
N3 C8 C9 C10 0.3(3) . . . . ?
N3 N4 C10 C9 0.2(3) . . . . ?
Fe1 N4 C10 C9 166.61(19) . . . . ?
C8 C9 C10 N4 -0.3(3) . . . . ?
N6 N5 C11 C12 -0.6(3) . . . . ?
C7 N5 C11 C12 -179.1(2) . . . . ?
N5 C11 C12 C13 0.5(3) . . . . ?
N5 N6 C13 C12 -0.1(3) . . . . ?
Fe1 N6 C13 C12 173.89(19) . . . . ?
C11 C12 C13 N6 -0.3(3) . . . . ?
O2 C15 C16 C18 -128.1(3) . . . . ?
N7 C15 C16 C18 51.8(4) . . . . ?
O2 C15 C16 C17 52.0(4) . . . . ?
N7 C15 C16 C17 -128.1(3) . . . . ?
C18 C16 C17 C19 -1.2(3) . . . . ?
C15 C16 C17 C19 178.7(2) . . . . ?
C17 C16 C18 C20 0.6(3) . . . . ?
C15 C16 C18 C20 -179.3(2) . . . . ?
C20 N8 C19 C17 1.1(3) . . . . ?
Fe1 N8 C19 C17 -178.28(16) . . . . ?
C20 N8 C19 N9 -178.86(17) . . . . ?
Fe1 N8 C19 N9 1.8(2) . . . . ?
C16 C17 C19 N8 0.4(3) . . . . ?
C16 C17 C19 N9 -179.7(2) . . . . ?
C21 N9 C19 N8 170.1(2) . . . . ?
N10 N9 C19 N8 -3.4(2) . . . . ?
C21 N9 C19 C17 -9.8(4) . . . . ?
N10 N9 C19 C17 176.7(2) . . . . ?
C19 N8 C20 C18 -1.7(3) . . . . ?
Fe1 N8 C20 C18 177.63(16) . . . . ?
C19 N8 C20 N11 179.20(17) . . . . ?
Fe1 N8 C20 N11 -1.4(2) . . . . ?
C16 C18 C20 N8 0.9(3) . . . . ?
C16 C18 C20 N11 179.8(2) . . . . ?
C24 N11 C20 N8 176.3(2) . . . . ?
N12 N11 C20 N8 0.7(2) . . . . ?
C24 N11 C20 C18 -2.7(4) . . . . ?
N12 N11 C20 C18 -178.31(19) . . . . ?
N10 N9 C21 C22 -0.1(2) . . . . ?
C19 N9 C21 C22 -173.9(2) . . . . ?
N9 C21 C22 C23 -0.2(3) . . . . ?
N9 N10 C23 C22 -0.5(2) . . . . ?
Fe1 N10 C23 C22 167.21(18) . . . . ?
C21 C22 C23 N10 0.5(3) . . . . ?
N12 N11 C24 C25 -0.4(2) . . . . ?
C20 N11 C24 C25 -176.3(2) . . . . ?
N11 C24 C25 C26 0.3(3) . . . . ?
N11 N12 C26 C25 -0.1(2) . . . . ?
Fe1 N12 C26 C25 174.80(18) . . . . ?
C24 C25 C26 N12 -0.1(3) . . . . ?

loop_
_geom_hbond_atom_site_label_D
_geom_hbond_atom_site_label_H
_geom_hbond_atom_site_label_A
_geom_hbond_site_symmetry_D
_geom_hbond_site_symmetry_H
_geom_hbond_site_symmetry_A
_geom_hbond_distance_DA
_geom_hbond_distance_DH
_geom_hbond_distance_HA
_geom_hbond_angle_DHA
_geom_hbond_publ_flag
N1 H1N O2 . . 2_656 2.879(3) 0.84(3) 2.04(3) 174(3) no
N1 H2N F32 . . 4_566 2.786(10) 0.84(3) 2.07(3) 143(2) no
N7 H3N F72 . . . 2.845(12) 0.91(4) 1.96(4) 164(4) no

#==============================================================================
# Additional structures and associated data_? identifiers
# should be added at this point if there is more than one 
# structure analysis in the CIF.





#==============================================================================
#     End of CIF
#==============================================================================
_chemical_name_systematic        
'bis[2,6-bis(1H-pyrazol-1-yl)pyridine-4-carboxamide]-iron bis[tetrafluoridoborate]'
_exptl_crystal_recrystallization_method 
'Re-crystallisation from solvent: CH3NO2 and Et2O'
_exptl_crystal_preparation       'Magnetic properties'
####################################################################### 
# 
# 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_M171020B
_database_code_depnum_ccdc_archive 'CCDC 2085820'
loop_
_audit_author_name
_audit_author_address
'Hiroki Akutsu'
;Osaka University
Japan
;
_audit_update_record             
;
2021-07-05 deposited with the CCDC.	2021-07-28 downloaded from the CCDC.
;

#==============================================================================
# CHEMICAL DATA

_chemical_formula_sum            'C24 H20 B2 F8 Fe N12 O2'
_chemical_formula_moiety         '(C12 H10 N6 O)2 Fe, 2(B F4)'
_chemical_formula_weight         737.96
_chemical_melting_point          ?

#==============================================================================
# CRYSTAL DATA
_space_group_crystal_system      monoclinic
_space_group_name_H-M_alt        'P 1 21/n 1'
_space_group_name_Hall           '-P 2yn'
_space_group_IT_number           14
loop_
_space_group_symop_id
_space_group_symop_operation_xyz
1 +X,+Y,+Z
2 1/2-X,1/2+Y,1/2-Z
3 -X,-Y,-Z
4 -1/2+X,-1/2-Y,-1/2+Z
#------------------------------------------------------------------------------
_cell_length_a                   9.24860(19)
_cell_length_b                   32.5567(8)
_cell_length_c                   10.3344(2)
_cell_angle_alpha                90.0000
_cell_angle_beta                 109.892(8)
_cell_angle_gamma                90.0000
_cell_volume                     2926.06(18)
_cell_formula_units_Z            4
_cell_measurement_reflns_used    24538
_cell_measurement_theta_min      2.10
_cell_measurement_theta_max      27.46
_cell_measurement_temperature    101
#------------------------------------------------------------------------------
_exptl_crystal_description       block
_exptl_crystal_colour            brown
_exptl_crystal_size_max          0.180
_exptl_crystal_size_mid          0.180
_exptl_crystal_size_min          0.130
_exptl_crystal_density_diffrn    1.675
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    'not measured'
_exptl_crystal_F_000             1488.00
_exptl_absorpt_coefficient_mu    0.615
_exptl_absorpt_correction_type   none

#==============================================================================
# EXPERIMENTAL DATA

_diffrn_ambient_temperature      101
_diffrn_radiation_type           'Mo K\a'
_diffrn_radiation_wavelength     0.71075
_diffrn_measurement_device_type  'Rigaku R-AXIS RAPID'
_diffrn_measurement_method       ω
_diffrn_detector_area_resol_mean 10.000
_diffrn_reflns_number            27553
_diffrn_reflns_av_unetI/netI     0.0319
_diffrn_reflns_av_R_equivalents  0.0370
_diffrn_reflns_theta_max         27.465
_diffrn_reflns_theta_min         2.187
_diffrn_reflns_theta_full        25.242
_diffrn_measured_fraction_theta_max 0.991
_diffrn_measured_fraction_theta_full 0.992
_diffrn_reflns_Laue_measured_fraction_max 0.991
_diffrn_reflns_Laue_measured_fraction_full 0.992
_diffrn_reflns_point_group_measured_fraction_max 0.991
_diffrn_reflns_point_group_measured_fraction_full 0.992
_diffrn_reflns_limit_h_min       -11
_diffrn_reflns_limit_h_max       11
_diffrn_reflns_limit_k_min       -42
_diffrn_reflns_limit_k_max       42
_diffrn_reflns_limit_l_min       -13
_diffrn_reflns_limit_l_max       13
_diffrn_standards_number         0
_diffrn_standards_interval_count .
_diffrn_standards_decay_%        ?
_reflns_number_total             6630
_reflns_number_gt                5575
_reflns_threshold_expression     F²>2.0σ(F²)
_reflns_Friedel_coverage         0.000
_reflns_Friedel_fraction_max     .
_reflns_Friedel_fraction_full    .

#==============================================================================
# REFINEMENT DATA

_refine_special_details          
;
    Refinement was performed using all reflections. The weighted 
    R-factor (wR) and goodness of fit (S) are based on F².
    R-factor (gt) are based on F. The threshold expression of
    F² > 2.0 sigma(F²) is used only for calculating R-factor (gt).
;
_refine_ls_structure_factor_coef Fsqd
_refine_ls_R_factor_all          0.0583
_refine_ls_R_factor_gt           0.0489
_refine_ls_wR_factor_ref         0.1374
_refine_ls_wR_factor_gt          0.1300
_refine_ls_number_restraints     4
_refine_ls_hydrogen_treatment    mixed
_refine_ls_number_reflns         6630
_refine_ls_number_parameters     464
_refine_ls_goodness_of_fit_ref   1.056
_refine_ls_weighting_scheme      calc
_refine_ls_weighting_details     
'w = 1/[σ²(Fo²)+(0.0674P)²+3.9292P] where P=(Fo²+2Fc²)/3'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_refine_ls_shift/su_max          0.001
_refine_diff_density_max         0.69
_refine_diff_density_min         -0.89
_refine_ls_extinction_method     none
_refine_ls_extinction_coef       ?

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 for Crystallography
(Vol. C, Tables 4.2.6.8 and 6.1.1.4)
;
H H 0.0000 0.0000
;
International Tables for Crystallography
(Vol. C, Table 6.1.1.4)
;
B B 0.0013 0.0007
;
International Tables for Crystallography
(Vol. C, Tables 4.2.6.8 and 6.1.1.4)
;
F F 0.0171 0.0103
;
International Tables for Crystallography
(Vol. C, Tables 4.2.6.8 and 6.1.1.4)
;
Fe Fe 0.3463 0.8444
;
International Tables for Crystallography
(Vol. C, Tables 4.2.6.8 and 6.1.1.4)
;
O O 0.0106 0.0060
;
International Tables for Crystallography
(Vol. C, Tables 4.2.6.8 and 6.1.1.4)
;
N N 0.0061 0.0033
;
International Tables for Crystallography
(Vol. C, Tables 4.2.6.8 and 6.1.1.4)
;

#==============================================================================
# ATOMIC COORDINATES AND THERMAL PARAMETERS

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 0.78184(4) 0.12851(2) 0.71079(4) 0.02090(11) Uani 1 1 d . . . . .
F1 F 0.9883(2) 0.26455(6) 0.3571(2) 0.0521(5) Uani 1 1 d . . . . .
F21 F 0.8806(6) 0.21545(16) 0.1940(4) 0.0731(15) Uani 0.6441 1 d D . P A 1
F31 F 1.0428(3) 0.19932(10) 0.3977(8) 0.099(2) Uani 0.7339 1 d D . P A 1
F4 F 0.8061(2) 0.22140(5) 0.38543(19) 0.0365(4) Uani 1 1 d . . . . .
F5 F 0.40706(19) 0.05811(5) 0.84182(19) 0.0365(4) Uani 1 1 d . . . . .
F6 F 0.3355(3) 0.02587(6) 0.6353(2) 0.0620(7) Uani 1 1 d . . . . .
F7 F 0.3949(2) -0.01172(5) 0.8293(2) 0.0433(5) Uani 1 1 d . . . . .
F8 F 0.1762(2) 0.02499(5) 0.7617(2) 0.0517(6) Uani 1 1 d . . . . .
F22 F 0.8450(11) 0.2313(3) 0.1942(5) 0.0731(15) Uani 0.3559 1 d D . P A 2
F32 F 0.9983(14) 0.1896(2) 0.338(3) 0.099(2) Uani 0.2661 1 d D . P A 2
O1 O 0.8958(2) 0.33581(5) 0.6841(2) 0.0305(4) Uani 1 1 d . . . . .
O2 O 0.8725(3) -0.07807(5) 0.8158(3) 0.0414(5) Uani 1 1 d . . . . .
N1 N 0.6391(3) 0.33464(7) 0.6478(3) 0.0311(5) Uani 1 1 d . . . . .
N2 N 0.7809(2) 0.18598(6) 0.6821(2) 0.0228(4) Uani 1 1 d . . . . .
N3 N 1.0373(2) 0.18067(6) 0.7865(2) 0.0239(4) Uani 1 1 d . . . . .
N4 N 1.0022(3) 0.13963(6) 0.7944(2) 0.0238(4) Uani 1 1 d . . . . .
N5 N 0.5246(2) 0.17792(6) 0.5850(2) 0.0248(4) Uani 1 1 d . . . . .
N6 N 0.5627(3) 0.13671(6) 0.6111(2) 0.0240(4) Uani 1 1 d . . . . .
N7 N 0.6404(3) -0.07052(7) 0.8413(3) 0.0363(6) Uani 1 1 d . . . . .
N8 N 0.7804(2) 0.07147(6) 0.7485(2) 0.0220(4) Uani 1 1 d . . . . .
N9 N 0.8341(2) 0.06409(6) 0.5526(2) 0.0233(4) Uani 1 1 d . . . . .
N10 N 0.8238(2) 0.10658(6) 0.5503(2) 0.0232(4) Uani 1 1 d . . . . .
N11 N 0.7318(2) 0.09214(6) 0.9377(2) 0.0231(4) Uani 1 1 d . . . . .
N12 N 0.7418(2) 0.13074(6) 0.8853(2) 0.0229(4) Uani 1 1 d . . . . .
C2 C 0.7758(3) 0.31684(7) 0.6680(3) 0.0265(5) Uani 1 1 d . . . . .
C3 C 0.7758(3) 0.27010(7) 0.6678(3) 0.0244(5) Uani 1 1 d . . . . .
C4 C 0.9168(3) 0.24992(7) 0.7253(3) 0.0250(5) Uani 1 1 d . . . . .
H4 H 1.010918 0.264637 0.759229 0.030 Uiso 1 1 calc R U . . .
C5 C 0.6383(3) 0.24798(7) 0.6144(3) 0.0245(5) Uani 1 1 d . . . . .
H5 H 0.542732 0.261479 0.572116 0.029 Uiso 1 1 calc R U . . .
C6 C 0.9125(3) 0.20736(7) 0.7303(3) 0.0232(5) Uani 1 1 d . . . . .
C7 C 0.6475(3) 0.20560(7) 0.6258(3) 0.0238(5) Uani 1 1 d . . . . .
C8 C 1.1924(3) 0.18627(8) 0.8243(3) 0.0284(5) Uani 1 1 d . . . . .
H8 H 1.244121 0.211644 0.827163 0.034 Uiso 1 1 calc R U . . .
C9 C 1.2595(3) 0.14838(8) 0.8574(3) 0.0298(6) Uani 1 1 d . . . . .
H9 H 1.366238 0.142209 0.887482 0.036 Uiso 1 1 calc R U . . .
C10 C 1.1373(3) 0.12049(7) 0.8375(3) 0.0269(5) Uani 1 1 d . . . . .
H10 H 1.149815 0.091731 0.852806 0.032 Uiso 1 1 calc R U . . .
C11 C 0.3691(3) 0.18280(8) 0.5258(3) 0.0282(6) Uani 1 1 d . . . . .
H11 H 0.315624 0.208037 0.499269 0.034 Uiso 1 1 calc R U . . .
C12 C 0.3052(3) 0.14443(8) 0.5119(3) 0.0304(6) Uani 1 1 d . . . . .
H12 H 0.199122 0.137697 0.473472 0.037 Uiso 1 1 calc R U . . .
C13 C 0.4287(3) 0.11695(7) 0.5661(3) 0.0270(5) Uani 1 1 d . . . . .
H13 H 0.417835 0.088006 0.570144 0.032 Uiso 1 1 calc R U . . .
C15 C 0.7653(3) -0.05653(7) 0.8202(3) 0.0281(6) Uani 1 1 d . . . . .
C16 C 0.7711(3) -0.01061(7) 0.7983(3) 0.0254(5) Uani 1 1 d . . . . .
C17 C 0.8035(3) 0.00226(7) 0.6828(3) 0.0251(5) Uani 1 1 d . . . . .
H17 H 0.823125 -0.016869 0.621381 0.030 Uiso 1 1 calc R U . . .
C18 C 0.7451(3) 0.01734(7) 0.8909(3) 0.0255(5) Uani 1 1 d . . . . .
H18 H 0.723534 0.008588 0.970106 0.031 Uiso 1 1 calc R U . . .
C19 C 0.8059(3) 0.04419(7) 0.6613(3) 0.0221(5) Uani 1 1 d . . . . .
C20 C 0.7528(3) 0.05875(7) 0.8601(3) 0.0222(5) Uani 1 1 d . . . . .
C21 C 0.8863(3) 0.05043(7) 0.4517(3) 0.0257(5) Uani 1 1 d . . . . .
H21 H 0.902925 0.022601 0.432905 0.031 Uiso 1 1 calc R U . . .
C22 C 0.9104(3) 0.08413(8) 0.3827(3) 0.0279(5) Uani 1 1 d . . . . .
H22 H 0.947394 0.084528 0.307466 0.033 Uiso 1 1 calc R U . . .
C23 C 0.8687(3) 0.11824(7) 0.4469(3) 0.0269(5) Uani 1 1 d . . . . .
H23 H 0.872400 0.145974 0.419604 0.032 Uiso 1 1 calc R U . . .
C24 C 0.6941(3) 0.09466(7) 1.0533(3) 0.0260(5) Uani 1 1 d . . . . .
H24 H 0.680440 0.072300 1.107119 0.031 Uiso 1 1 calc R U . . .
C25 C 0.6793(3) 0.13558(7) 1.0780(3) 0.0268(5) Uani 1 1 d . . . . .
H25 H 0.654068 0.147224 1.151904 0.032 Uiso 1 1 calc R U . . .
C26 C 0.7094(3) 0.15671(7) 0.9711(3) 0.0256(5) Uani 1 1 d . . . . .
H26 H 0.706870 0.185747 0.961470 0.031 Uiso 1 1 calc R U . . .
B1 B 0.9256(3) 0.22614(8) 0.3322(3) 0.0329(7) Uani 1 1 d D . . . .
B2 B 0.3281(4) 0.02496(8) 0.7662(3) 0.0274(6) Uani 1 1 d . . . . .
H1N H 0.633(4) 0.3615(12) 0.655(4) 0.045(10) Uiso 1 1 d . . . . .
H2N H 0.569(4) 0.3208(11) 0.660(3) 0.033(9) Uiso 1 1 d . . . . .
H3N H 0.567(4) -0.0533(12) 0.839(4) 0.048(10) Uiso 1 1 d . . . . .
H4N H 0.626(4) -0.0957(13) 0.845(4) 0.051(11) Uiso 1 1 d . . . . .


#==============================================================================
_computing_data_collection       'RAPID AUTO (Rigaku, ????)'
_computing_cell_refinement       'RAPID AUTO'
_computing_data_reduction        'RAPID AUTO'
_computing_structure_solution    ?
_computing_structure_refinement  'SHELXL Version 2018/3 (Sheldrick, 2008)'
_computing_publication_material  'CrystalStructure 4.3 (Rigaku, 2019)'
_computing_molecular_graphics    'CrystalStructure 4.3'

#==============================================================================
# MOLECULAR GEOMETRY

_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 N2 1.894(2) . ?
Fe1 N8 1.8983(19) . ?
Fe1 N6 1.955(2) . ?
Fe1 N4 1.958(2) . ?
Fe1 N10 1.961(2) . ?
Fe1 N12 1.962(2) . ?
F1 B1 1.365(3) . ?
F21 B1 1.389(4) . ?
F31 B1 1.377(4) . ?
F4 B1 1.401(4) . ?
F5 B2 1.386(3) . ?
F6 B2 1.377(4) . ?
F7 B2 1.400(3) . ?
F8 B2 1.389(4) . ?
F22 B1 1.376(5) . ?
F32 B1 1.357(5) . ?
O1 C2 1.231(3) . ?
O2 C15 1.228(3) . ?
N1 C2 1.341(3) . ?
N1 H1N 0.88(4) . ?
N1 H2N 0.83(4) . ?
N2 C7 1.334(3) . ?
N2 C6 1.342(3) . ?
N3 C8 1.364(3) . ?
N3 N4 1.384(3) . ?
N3 C6 1.403(3) . ?
N4 C10 1.330(3) . ?
N5 C11 1.367(3) . ?
N5 N6 1.390(3) . ?
N5 C7 1.398(3) . ?
N6 C13 1.332(3) . ?
N7 C15 1.327(4) . ?
N7 H3N 0.87(4) . ?
N7 H4N 0.83(4) . ?
N8 C20 1.330(3) . ?
N8 C19 1.342(3) . ?
N9 C21 1.363(3) . ?
N9 N10 1.386(3) . ?
N9 C19 1.397(3) . ?
N10 C23 1.327(3) . ?
N11 C24 1.357(3) . ?
N11 N12 1.384(3) . ?
N11 C20 1.403(3) . ?
N12 C26 1.332(3) . ?
C2 C3 1.521(3) . ?
C3 C4 1.400(4) . ?
C3 C5 1.401(4) . ?
C4 C6 1.387(3) . ?
C4 H4 0.9500 . ?
C5 C7 1.385(3) . ?
C5 H5 0.9500 . ?
C8 C9 1.371(4) . ?
C8 H8 0.9500 . ?
C9 C10 1.409(4) . ?
C9 H9 0.9500 . ?
C10 H10 0.9500 . ?
C11 C12 1.369(3) . ?
C11 H11 0.9500 . ?
C12 C13 1.409(4) . ?
C12 H12 0.9500 . ?
C13 H13 0.9500 . ?
C15 C16 1.516(3) . ?
C16 C17 1.391(4) . ?
C16 C18 1.399(4) . ?
C17 C19 1.384(3) . ?
C17 H17 0.9500 . ?
C18 C20 1.392(3) . ?
C18 H18 0.9500 . ?
C21 C22 1.368(4) . ?
C21 H21 0.9500 . ?
C22 C23 1.413(4) . ?
C22 H22 0.9500 . ?
C23 H23 0.9500 . ?
C24 C25 1.372(3) . ?
C24 H24 0.9500 . ?
C25 C26 1.407(4) . ?
C25 H25 0.9500 . ?
C26 H26 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
N2 Fe1 N8 176.88(10) . . ?
N2 Fe1 N6 80.43(8) . . ?
N8 Fe1 N6 99.42(9) . . ?
N2 Fe1 N4 80.50(8) . . ?
N8 Fe1 N4 99.74(9) . . ?
N6 Fe1 N4 160.81(8) . . ?
N2 Fe1 N10 102.65(9) . . ?
N8 Fe1 N10 80.47(9) . . ?
N6 Fe1 N10 94.13(9) . . ?
N4 Fe1 N10 87.97(9) . . ?
N2 Fe1 N12 96.60(9) . . ?
N8 Fe1 N12 80.28(9) . . ?
N6 Fe1 N12 89.61(9) . . ?
N4 Fe1 N12 94.68(9) . . ?
N10 Fe1 N12 160.75(8) . . ?
C2 N1 H1N 120(2) . . ?
C2 N1 H2N 119(2) . . ?
H1N N1 H2N 117(3) . . ?
C7 N2 C6 120.0(2) . . ?
C7 N2 Fe1 119.71(16) . . ?
C6 N2 Fe1 119.93(16) . . ?
C8 N3 N4 110.9(2) . . ?
C8 N3 C6 132.3(2) . . ?
N4 N3 C6 116.4(2) . . ?
C10 N4 N3 105.0(2) . . ?
C10 N4 Fe1 141.20(17) . . ?
N3 N4 Fe1 112.51(15) . . ?
C11 N5 N6 110.9(2) . . ?
C11 N5 C7 133.1(2) . . ?
N6 N5 C7 115.9(2) . . ?
C13 N6 N5 104.8(2) . . ?
C13 N6 Fe1 142.44(17) . . ?
N5 N6 Fe1 112.50(15) . . ?
C15 N7 H3N 119(3) . . ?
C15 N7 H4N 120(3) . . ?
H3N N7 H4N 120(4) . . ?
C20 N8 C19 120.4(2) . . ?
C20 N8 Fe1 119.95(16) . . ?
C19 N8 Fe1 119.67(17) . . ?
C21 N9 N10 110.7(2) . . ?
C21 N9 C19 132.5(2) . . ?
N10 N9 C19 116.5(2) . . ?
C23 N10 N9 105.1(2) . . ?
C23 N10 Fe1 141.52(17) . . ?
N9 N10 Fe1 112.42(16) . . ?
C24 N11 N12 111.2(2) . . ?
C24 N11 C20 132.6(2) . . ?
N12 N11 C20 116.1(2) . . ?
C26 N12 N11 104.8(2) . . ?
C26 N12 Fe1 142.35(17) . . ?
N11 N12 Fe1 112.63(15) . . ?
O1 C2 N1 124.3(2) . . ?
O1 C2 C3 120.1(2) . . ?
N1 C2 C3 115.6(2) . . ?
C4 C3 C5 121.0(2) . . ?
C4 C3 C2 118.0(2) . . ?
C5 C3 C2 121.0(2) . . ?
C6 C4 C3 116.7(2) . . ?
C6 C4 H4 121.6 . . ?
C3 C4 H4 121.6 . . ?
C7 C5 C3 117.2(2) . . ?
C7 C5 H5 121.4 . . ?
C3 C5 H5 121.4 . . ?
N2 C6 C4 122.6(2) . . ?
N2 C6 N3 110.30(19) . . ?
C4 C6 N3 127.1(2) . . ?
N2 C7 C5 122.4(2) . . ?
N2 C7 N5 111.0(2) . . ?
C5 C7 N5 126.6(2) . . ?
N3 C8 C9 107.1(2) . . ?
N3 C8 H8 126.5 . . ?
C9 C8 H8 126.5 . . ?
C8 C9 C10 105.7(2) . . ?
C8 C9 H9 127.1 . . ?
C10 C9 H9 127.1 . . ?
N4 C10 C9 111.2(2) . . ?
N4 C10 H10 124.4 . . ?
C9 C10 H10 124.4 . . ?
N5 C11 C12 107.0(2) . . ?
N5 C11 H11 126.5 . . ?
C12 C11 H11 126.5 . . ?
C11 C12 C13 106.0(2) . . ?
C11 C12 H12 127.0 . . ?
C13 C12 H12 127.0 . . ?
N6 C13 C12 111.4(2) . . ?
N6 C13 H13 124.3 . . ?
C12 C13 H13 124.3 . . ?
O2 C15 N7 124.7(2) . . ?
O2 C15 C16 119.2(2) . . ?
N7 C15 C16 116.1(2) . . ?
C17 C16 C18 121.9(2) . . ?
C17 C16 C15 117.0(2) . . ?
C18 C16 C15 121.1(2) . . ?
C19 C17 C16 117.1(2) . . ?
C19 C17 H17 121.5 . . ?
C16 C17 H17 121.5 . . ?
C20 C18 C16 116.1(2) . . ?
C20 C18 H18 122.0 . . ?
C16 C18 H18 122.0 . . ?
N8 C19 C17 121.9(2) . . ?
N8 C19 N9 110.9(2) . . ?
C17 C19 N9 127.2(2) . . ?
N8 C20 C18 122.6(2) . . ?
N8 C20 N11 111.1(2) . . ?
C18 C20 N11 126.3(2) . . ?
N9 C21 C22 107.4(2) . . ?
N9 C21 H21 126.3 . . ?
C22 C21 H21 126.3 . . ?
C21 C22 C23 105.5(2) . . ?
C21 C22 H22 127.3 . . ?
C23 C22 H22 127.3 . . ?
N10 C23 C22 111.3(2) . . ?
N10 C23 H23 124.3 . . ?
C22 C23 H23 124.3 . . ?
N11 C24 C25 107.1(2) . . ?
N11 C24 H24 126.4 . . ?
C25 C24 H24 126.4 . . ?
C24 C25 C26 105.7(2) . . ?
C24 C25 H25 127.2 . . ?
C26 C25 H25 127.2 . . ?
N12 C26 C25 111.2(2) . . ?
N12 C26 H26 124.4 . . ?
C25 C26 H26 124.4 . . ?
F22 B1 F32 103.7(11) . . ?
F22 B1 F1 97.4(5) . . ?
F32 B1 F1 128.4(6) . . ?
F1 B1 F21 112.5(3) . . ?
F1 B1 F31 106.0(3) . . ?
F21 B1 F31 104.9(4) . . ?
F22 B1 F4 101.5(5) . . ?
F32 B1 F4 109.4(9) . . ?
F1 B1 F4 111.6(2) . . ?
F21 B1 F4 112.1(3) . . ?
F31 B1 F4 109.3(3) . . ?
F6 B2 F5 110.1(2) . . ?
F6 B2 F8 110.8(3) . . ?
F5 B2 F8 110.6(2) . . ?
F6 B2 F7 108.3(2) . . ?
F5 B2 F7 109.7(2) . . ?
F8 B2 F7 107.3(2) . . ?

loop_
_geom_torsion_atom_site_label_1
_geom_torsion_atom_site_label_2
_geom_torsion_atom_site_label_3
_geom_torsion_atom_site_label_4
_geom_torsion
_geom_torsion_site_symmetry_1
_geom_torsion_site_symmetry_2
_geom_torsion_site_symmetry_3
_geom_torsion_site_symmetry_4
_geom_torsion_publ_flag
N6 Fe1 N2 C7 5.8(2) . . . . ?
N4 Fe1 N2 C7 -176.4(2) . . . . ?
N10 Fe1 N2 C7 97.9(2) . . . . ?
N12 Fe1 N2 C7 -82.7(2) . . . . ?
N6 Fe1 N2 C6 179.4(2) . . . . ?
N4 Fe1 N2 C6 -2.8(2) . . . . ?
N10 Fe1 N2 C6 -88.5(2) . . . . ?
N12 Fe1 N2 C6 90.9(2) . . . . ?
C8 N3 N4 C10 0.1(3) . . . . ?
C6 N3 N4 C10 174.1(2) . . . . ?
C8 N3 N4 Fe1 -169.86(18) . . . . ?
C6 N3 N4 Fe1 4.2(3) . . . . ?
C11 N5 N6 C13 0.4(3) . . . . ?
C7 N5 N6 C13 178.9(2) . . . . ?
C11 N5 N6 Fe1 -174.83(18) . . . . ?
C7 N5 N6 Fe1 3.7(3) . . . . ?
N6 Fe1 N8 C20 -86.5(2) . . . . ?
N4 Fe1 N8 C20 94.64(19) . . . . ?
N10 Fe1 N8 C20 -179.1(2) . . . . ?
N12 Fe1 N8 C20 1.52(19) . . . . ?
N6 Fe1 N8 C19 92.9(2) . . . . ?
N4 Fe1 N8 C19 -86.0(2) . . . . ?
N10 Fe1 N8 C19 0.22(19) . . . . ?
N12 Fe1 N8 C19 -179.2(2) . . . . ?
C21 N9 N10 C23 0.5(3) . . . . ?
C19 N9 N10 C23 174.4(2) . . . . ?
C21 N9 N10 Fe1 -170.67(16) . . . . ?
C19 N9 N10 Fe1 3.2(3) . . . . ?
C24 N11 N12 C26 0.0(3) . . . . ?
C20 N11 N12 C26 176.5(2) . . . . ?
C24 N11 N12 Fe1 -175.98(16) . . . . ?
C20 N11 N12 Fe1 0.5(3) . . . . ?
O1 C2 C3 C4 18.5(4) . . . . ?
N1 C2 C3 C4 -162.5(3) . . . . ?
O1 C2 C3 C5 -162.9(3) . . . . ?
N1 C2 C3 C5 16.2(4) . . . . ?
C5 C3 C4 C6 -1.9(4) . . . . ?
C2 C3 C4 C6 176.7(2) . . . . ?
C4 C3 C5 C7 2.4(4) . . . . ?
C2 C3 C5 C7 -176.2(2) . . . . ?
C7 N2 C6 C4 0.5(4) . . . . ?
Fe1 N2 C6 C4 -173.1(2) . . . . ?
C7 N2 C6 N3 179.1(2) . . . . ?
Fe1 N2 C6 N3 5.6(3) . . . . ?
C3 C4 C6 N2 0.5(4) . . . . ?
C3 C4 C6 N3 -178.0(3) . . . . ?
C8 N3 C6 N2 166.3(3) . . . . ?
N4 N3 C6 N2 -6.1(3) . . . . ?
C8 N3 C6 C4 -15.1(5) . . . . ?
N4 N3 C6 C4 172.4(3) . . . . ?
C6 N2 C7 C5 0.0(4) . . . . ?
Fe1 N2 C7 C5 173.6(2) . . . . ?
C6 N2 C7 N5 -178.7(2) . . . . ?
Fe1 N2 C7 N5 -5.1(3) . . . . ?
C3 C5 C7 N2 -1.5(4) . . . . ?
C3 C5 C7 N5 177.1(3) . . . . ?
C11 N5 C7 N2 178.8(3) . . . . ?
N6 N5 C7 N2 0.7(3) . . . . ?
C11 N5 C7 C5 0.1(5) . . . . ?
N6 N5 C7 C5 -178.1(3) . . . . ?
N4 N3 C8 C9 0.0(3) . . . . ?
C6 N3 C8 C9 -172.8(3) . . . . ?
N3 C8 C9 C10 -0.1(3) . . . . ?
N3 N4 C10 C9 -0.1(3) . . . . ?
Fe1 N4 C10 C9 164.9(2) . . . . ?
C8 C9 C10 N4 0.1(3) . . . . ?
N6 N5 C11 C12 -0.6(3) . . . . ?
C7 N5 C11 C12 -178.7(3) . . . . ?
N5 C11 C12 C13 0.5(3) . . . . ?
N5 N6 C13 C12 -0.1(3) . . . . ?
Fe1 N6 C13 C12 172.7(2) . . . . ?
C11 C12 C13 N6 -0.2(3) . . . . ?
O2 C15 C16 C17 50.6(4) . . . . ?
N7 C15 C16 C17 -128.6(3) . . . . ?
O2 C15 C16 C18 -129.3(3) . . . . ?
N7 C15 C16 C18 51.5(4) . . . . ?
C18 C16 C17 C19 -1.3(4) . . . . ?
C15 C16 C17 C19 178.8(2) . . . . ?
C17 C16 C18 C20 0.4(4) . . . . ?
C15 C16 C18 C20 -179.8(2) . . . . ?
C20 N8 C19 C17 0.4(4) . . . . ?
Fe1 N8 C19 C17 -178.88(19) . . . . ?
C20 N8 C19 N9 -179.3(2) . . . . ?
Fe1 N8 C19 N9 1.4(3) . . . . ?
C16 C17 C19 N8 1.0(4) . . . . ?
C16 C17 C19 N9 -179.4(2) . . . . ?
C21 N9 C19 N8 169.2(2) . . . . ?
N10 N9 C19 N8 -3.0(3) . . . . ?
C21 N9 C19 C17 -10.5(4) . . . . ?
N10 N9 C19 C17 177.3(2) . . . . ?
C19 N8 C20 C18 -1.5(4) . . . . ?
Fe1 N8 C20 C18 177.8(2) . . . . ?
C19 N8 C20 N11 179.1(2) . . . . ?
Fe1 N8 C20 N11 -1.6(3) . . . . ?
C16 C18 C20 N8 1.1(4) . . . . ?
C16 C18 C20 N11 -179.6(2) . . . . ?
C24 N11 C20 N8 176.2(2) . . . . ?
N12 N11 C20 N8 0.6(3) . . . . ?
C24 N11 C20 C18 -3.2(5) . . . . ?
N12 N11 C20 C18 -178.7(2) . . . . ?
N10 N9 C21 C22 0.0(3) . . . . ?
C19 N9 C21 C22 -172.6(3) . . . . ?
N9 C21 C22 C23 -0.5(3) . . . . ?
N9 N10 C23 C22 -0.8(3) . . . . ?
Fe1 N10 C23 C22 166.0(2) . . . . ?
C21 C22 C23 N10 0.8(3) . . . . ?
N12 N11 C24 C25 -0.2(3) . . . . ?
C20 N11 C24 C25 -175.9(3) . . . . ?
N11 C24 C25 C26 0.3(3) . . . . ?
N11 N12 C26 C25 0.2(3) . . . . ?
Fe1 N12 C26 C25 174.1(2) . . . . ?
C24 C25 C26 N12 -0.3(3) . . . . ?

loop_
_geom_hbond_atom_site_label_D
_geom_hbond_atom_site_label_H
_geom_hbond_atom_site_label_A
_geom_hbond_site_symmetry_D
_geom_hbond_site_symmetry_H
_geom_hbond_site_symmetry_A
_geom_hbond_distance_DA
_geom_hbond_distance_DH
_geom_hbond_distance_HA
_geom_hbond_angle_DHA
_geom_hbond_publ_flag
N1 H1N O2 . . 2_656 2.874(3) 0.88(4) 1.99(4) 176(3) no
N1 H2N F32 . . 4_566 2.81(3) 0.83(4) 2.18(5) 134(3) no
N7 H3N F7 . . . 2.940(3) 0.87(4) 2.07(4) 179(4) no
N7 H4N O1 . . 2_646 3.069(3) 0.83(4) 2.25(4) 168(4) no

#==============================================================================
# Additional structures and associated data_? identifiers
# should be added at this point if there is more than one 
# structure analysis in the CIF.





#==============================================================================
#     End of CIF
#==============================================================================
_chemical_name_systematic        
'bis[2,6-bis(1H-pyrazol-1-yl)pyridine-4-carboxamide]-iron bis[tetrafluoridoborate]'
_exptl_crystal_recrystallization_method 
'Re-crystallisation from solvent: CH3NO2 and Et2O'
_exptl_crystal_preparation       'Magnetic properties'
####################################################################### 
# 
# 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_c-bppconh2mecn
_database_code_depnum_ccdc_archive 'CCDC 2085826'
loop_
_audit_author_name
_audit_author_address
'Lee Martin'
;Nottingham Trent University
United Kingdom
;
_audit_update_record             
;
2021-05-25 deposited with the CCDC.	2021-07-28 downloaded from the CCDC.
;
_audit_creation_date             2019-08-14
_audit_creation_method           
;
Olex2 1.2
(compiled 2018.05.29 svn.r3508 for OlexSys, GUI svn.r5506)
;
_shelx_SHELXL_version_number     2018/3
_chemical_name_common            ?
_chemical_name_systematic        ?
_chemical_formula_moiety         'C24 H20 Fe N12 O2, 2(Cl O4)'
_chemical_formula_sum            'C24 H20 Cl2 Fe N12 O10'
_chemical_formula_weight         763.27
_chemical_melting_point          ?
_chemical_oxdiff_formula         'C24 H20 Cl2 O10 Fe1 N12'
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'
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           14
_space_group_name_H-M_alt        'P 1 21/n 1'
_space_group_name_Hall           '-P 2yn'
loop_
_space_group_symop_operation_xyz
'x, y, z'
'-x+1/2, y+1/2, -z+1/2'
'-x, -y, -z'
'x-1/2, -y-1/2, z-1/2'

_cell_length_a                   9.4886(4)
_cell_length_b                   32.6089(8)
_cell_length_c                   10.5004(4)
_cell_angle_alpha                90
_cell_angle_beta                 109.721(4)
_cell_angle_gamma                90
_cell_volume                     3058.4(2)
_cell_formula_units_Z            4
_cell_measurement_reflns_used    4558
_cell_measurement_temperature    293(1)
_cell_measurement_theta_max      27.4560
_cell_measurement_theta_min      3.1320
_shelx_estimated_absorpt_T_max   ?
_shelx_estimated_absorpt_T_min   ?
_exptl_absorpt_coefficient_mu    0.745
_exptl_absorpt_correction_T_max  0.961
_exptl_absorpt_correction_T_min  0.891
_exptl_absorpt_correction_type   analytical
_exptl_absorpt_process_details   
;
CrysAlisPro 1.171.38.46 (Rigaku Oxford Diffraction, 2015)
Analytical numeric absorption correction using a multifaceted crystal
			model based on expressions derived by R.C. Clark & J.S. Reid.
(Clark, R. C. & Reid, J. S. (1995). Acta Cryst. A51, 887-897)
Empirical absorption correction using spherical harmonics,
 implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_absorpt_special_details   ?
_exptl_crystal_colour            ?
_exptl_crystal_density_diffrn    1.658
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    ?
_exptl_crystal_description       block
_exptl_crystal_F_000             1552
loop_
_exptl_crystal_face_index_h
_exptl_crystal_face_index_k
_exptl_crystal_face_index_l
_exptl_crystal_face_perp_dist
-3 -45 3 0.0448
10 -13 -12 0.0462
-10 13 12 0.0462
-1 42 -5 0.0235
0 -41 6 0.0691
5 42 -4 0.0132
9 -3 7 0.1035
-9 3 -7 0.1035

_exptl_crystal_size_max          0.216
_exptl_crystal_size_mid          0.092
_exptl_crystal_size_min          0.065
loop_
_exptl_oxdiff_crystal_face_indexfrac_h
_exptl_oxdiff_crystal_face_indexfrac_k
_exptl_oxdiff_crystal_face_indexfrac_l
_exptl_oxdiff_crystal_face_x
_exptl_oxdiff_crystal_face_y
_exptl_oxdiff_crystal_face_z
-2.9976 -44.9147 3.0042 -0.0968 -0.4054 -0.9213
10.0038 -13.1156 -12.0083 -0.9882 -0.0775 0.1044
-10.0038 13.1156 12.0083 0.9882 0.0775 -0.1044
-0.9950 41.9079 -5.0031 0.1888 0.0248 0.9739
-0.0051 -40.8978 6.0038 -0.0993 -0.0296 -0.9827
4.9967 41.9049 -4.0053 -0.0542 0.4576 0.8838
8.9810 -2.9505 6.9988 -0.1924 0.9037 -0.3912
-8.9810 2.9505 -6.9988 0.1924 -0.9037 0.3912

_exptl_transmission_factor_max   ?
_exptl_transmission_factor_min   ?
_diffrn_reflns_av_R_equivalents  0.0349
_diffrn_reflns_av_unetI/netI     0.0579
_diffrn_reflns_Laue_measured_fraction_full 0.998
_diffrn_reflns_Laue_measured_fraction_max 0.843
_diffrn_reflns_limit_h_max       9
_diffrn_reflns_limit_h_min       -13
_diffrn_reflns_limit_k_max       21
_diffrn_reflns_limit_k_min       -43
_diffrn_reflns_limit_l_max       13
_diffrn_reflns_limit_l_min       -14
_diffrn_reflns_number            15661
_diffrn_reflns_point_group_measured_fraction_full 0.998
_diffrn_reflns_point_group_measured_fraction_max 0.843
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         29.302
_diffrn_reflns_theta_min         3.129
_diffrn_ambient_environment      air
_diffrn_ambient_temperature      293(1)
_diffrn_detector                 'CCD plate'
_diffrn_detector_area_resol_mean 15.9832
_diffrn_detector_type            Sapphire3
_diffrn_measured_fraction_theta_full 0.998
_diffrn_measured_fraction_theta_max 0.843
_diffrn_measurement_details      
;
List of Runs (angles in degrees, time in seconds):

  # Type    Start    End  Width  tₑₓₚ   ω     θ     κ     φ   Frames
#--------------------------------------------------------------------------
  1  ω    -51.00  20.00   1.00  325.00    --   16.00 -57.00-120.00   71
  2  ω     -1.00  79.00   1.00  325.00    --   16.00  57.00  90.00   80
  3  ω     44.00  70.00   1.00  325.00    --   16.00  57.00-180.00   26
  4  ω      9.00  64.00   1.00  325.00    --   16.00  37.00-180.00   55
;
_diffrn_measurement_device       'four-circle diffractometer'
_diffrn_measurement_device_type  'Xcalibur, Sapphire3, Gemini'
_diffrn_measurement_method       'ω scans'
_diffrn_orient_matrix_type       
'CrysAlisPro convention (1999,Acta A55,543-557)'
_diffrn_orient_matrix_UB_11      -0.0464302000
_diffrn_orient_matrix_UB_12      0.0076159000
_diffrn_orient_matrix_UB_13      0.0352984000
_diffrn_orient_matrix_UB_21      0.0637995000
_diffrn_orient_matrix_UB_22      0.0081581000
_diffrn_orient_matrix_UB_23      0.0506895000
_diffrn_orient_matrix_UB_31      -0.0089543000
_diffrn_orient_matrix_UB_32      0.0186657000
_diffrn_orient_matrix_UB_33      -0.0365370000
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_source                   'fine-focus sealed X-ray tube'
_diffrn_source_type              'Enhance (Mo) X-ray Source'
_reflns_Friedel_coverage         0.000
_reflns_Friedel_fraction_full    .
_reflns_Friedel_fraction_max     .
_reflns_number_gt                5152
_reflns_number_total             7053
_reflns_odcompleteness_completeness 99.67
_reflns_odcompleteness_iscentric 1
_reflns_odcompleteness_theta     26.32
_reflns_special_details          
;
 Reflections were merged by SHELXL according to the crystal
 class for the calculation of statistics and refinement.
 
 _reflns_Friedel_fraction is defined as the number of unique
 Friedel pairs measured divided by the number that would be
 possible theoretically, ignoring centric projections and
 systematic absences.
;
_reflns_threshold_expression     'I > 2σ(I)'
_computing_cell_refinement       'CrysAlisPro 1.171.38.46 (Rigaku OD, 2015)'
_computing_data_collection       'CrysAlisPro 1.171.38.46 (Rigaku OD, 2015)'
_computing_data_reduction        'CrysAlisPro 1.171.38.46 (Rigaku OD, 2015)'
_computing_molecular_graphics    'Olex2 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 (Dolomanov et al., 2009)'
_computing_structure_refinement  'ShelXL (Sheldrick, 2015)'
_computing_structure_solution    'ShelXT (Sheldrick, 2015)'
_refine_diff_density_max         0.483
_refine_diff_density_min         -0.439
_refine_diff_density_rms         0.065
_refine_ls_extinction_coef       .
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.090
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     498
_refine_ls_number_reflns         7053
_refine_ls_number_restraints     347
_refine_ls_R_factor_all          0.0963
_refine_ls_R_factor_gt           0.0633
_refine_ls_restrained_S_all      1.110
_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)+(0.0261P)²+3.6544P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1055
_refine_ls_wR_factor_ref         0.1164
_refine_special_details          ?
_olex2_refinement_description    
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups, All N(H,H) groups
2. Restrained distances
 Cl03-O10 \\sim Cl03-O1AA \\sim Cl03-O7 \\sim Cl03-O0AA \\sim Cl03-O9 \\sim
Cl03-O2AA \\sim Cl03-O8 ~
 Cl02-O4B \\sim Cl02-O5 \\sim Cl02-O3B \\sim Cl02-O3 \\sim Cl02-O5B \\sim
Cl02-O4 \\sim Cl02-O6
 with sigma of 0.02
3. Uiso/Uaniso restraints and constraints
Cl02 \\sim Cl02 \\sim Cl02 \\sim Cl02 \\sim Cl02 \\sim Cl02 \\sim Cl02 \\sim O6
\\sim O3B \\sim O4B \\sim O5B \\sim Cl03 \\sim Cl03 \\sim Cl03 \\sim Cl03 \\sim
Cl03 \\sim Cl03 \\sim Cl03 \\sim Cl03 \\sim O8 \\sim O7 \\sim O9 \\sim O10
\\sim O0AA \\sim O1AA \\sim O2AA \\sim O3 \\sim O4 \\sim O5: within 2A with
sigma of 0.04 and sigma for terminal atoms of 0.08
4. Rigid body (RIGU) restrains
 Cl02, Cl02, Cl02, Cl02, Cl02, Cl02, Cl02, O6, O3B, O4B, O5B, Cl03, Cl03, Cl03,
  Cl03, Cl03, Cl03, Cl03, Cl03, O8, O7, O9, O10, O0AA, O1AA, O2AA, O3, O4, O5
 with sigma for 1-2 distances of 0.004 and sigma for 1-3 distances of 0.004
5. Others
 Sof(O7)=Sof(O9)=Sof(O10)=1-FVAR(1)
 Sof(O0AA)=Sof(O1AA)=Sof(O2AA)=FVAR(1)
 Sof(O3B)=Sof(O4B)=Sof(O5B)=1-FVAR(2)
 Sof(O3)=Sof(O4)=Sof(O5)=FVAR(2)
6.a Aromatic/amide H refined with riding coordinates:
 C1(H1), C2(H2), C3(H3), C5(H5), C7(H7), C9(H9), C10(H10), C11(H11), C13(H13),
 C14(H14), C15(H15), C17(H17), C19(H19), C21(H21), C22(H22), C23(H23)
6.b X=CH2 refined with riding coordinates:
 N11(H11A,H11B), N12(H12A,H12B)
;
_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 0.28531(5) 0.62912(2) 0.71545(4) 0.02630(12) Uani 1 1 d . . . . .
O1 O 0.3638(4) 0.42240(8) 0.8053(4) 0.0853(12) Uani 1 1 d . . . . .
O2 O 0.3976(3) 0.83561(7) 0.6851(3) 0.0540(7) Uani 1 1 d . . . . .
N1 N 0.2454(3) 0.63036(8) 0.8872(3) 0.0307(6) Uani 1 1 d . . . . .
N2 N 0.2353(3) 0.59178(8) 0.9360(3) 0.0315(6) Uani 1 1 d . . . . .
N3 N 0.2847(3) 0.57218(7) 0.7501(2) 0.0266(6) Uani 1 1 d . . . . .
N4 N 0.3385(3) 0.56566(8) 0.5581(3) 0.0314(6) Uani 1 1 d . . . . .
N5 N 0.3271(3) 0.60771(8) 0.5566(3) 0.0320(6) Uani 1 1 d . . . . .
N6 N 0.4999(3) 0.64025(8) 0.7982(3) 0.0323(6) Uani 1 1 d . . . . .
N7 N 0.5337(3) 0.68106(8) 0.7902(3) 0.0351(6) Uani 1 1 d . . . . .
N8 N 0.2847(3) 0.68645(7) 0.6891(2) 0.0263(6) Uani 1 1 d . . . . .
N9 N 0.0351(3) 0.67874(8) 0.5922(3) 0.0319(6) Uani 1 1 d . . . . .
N10 N 0.0708(3) 0.63773(7) 0.6160(3) 0.0315(6) Uani 1 1 d . . . . .
N11 N 0.1440(4) 0.43073(10) 0.8346(4) 0.0740(12) Uani 1 1 d . . . . .
H11A H 0.132420 0.404866 0.843697 0.089 Uiso 1 1 calc R . . . .
H11B H 0.076680 0.447726 0.839341 0.089 Uiso 1 1 calc R . . . .
N12 N 0.1523(4) 0.83484(8) 0.6590(3) 0.0540(9) Uani 1 1 d . . . . .
H12A H 0.145553 0.861143 0.656735 0.065 Uiso 1 1 calc R . . . .
H12B H 0.074726 0.820126 0.651535 0.065 Uiso 1 1 calc R . . . .
C1 C 0.2128(4) 0.65545(10) 0.9724(3) 0.0383(8) Uani 1 1 d . . . . .
H1 H 0.210898 0.683882 0.965149 0.046 Uiso 1 1 calc R . . . .
C2 C 0.1817(4) 0.63394(12) 1.0740(4) 0.0462(9) Uani 1 1 d . . . . .
H2 H 0.156061 0.644896 1.144946 0.055 Uiso 1 1 calc R . . . .
C3 C 0.1965(4) 0.59376(11) 1.0486(3) 0.0412(9) Uani 1 1 d . . . . .
H3 H 0.182603 0.571662 1.099100 0.049 Uiso 1 1 calc R . . . .
C4 C 0.2564(4) 0.55889(9) 0.8591(3) 0.0294(7) Uani 1 1 d . . . . .
C5 C 0.2480(4) 0.51769(10) 0.8862(3) 0.0365(8) Uani 1 1 d . . . . .
H5 H 0.226842 0.508829 0.962044 0.044 Uiso 1 1 calc R . . . .
C6 C 0.2726(4) 0.49002(9) 0.7948(4) 0.0358(8) Uani 1 1 d . . . . .
C7 C 0.3062(4) 0.50358(9) 0.6829(3) 0.0363(8) Uani 1 1 d . . . . .
H7 H 0.325668 0.485194 0.623211 0.044 Uiso 1 1 calc R . . . .
C8 C 0.3097(4) 0.54518(9) 0.6640(3) 0.0287(7) Uani 1 1 d . . . . .
C9 C 0.3879(4) 0.55238(11) 0.4584(3) 0.0382(8) Uani 1 1 d . . . . .
H9 H 0.404139 0.525261 0.439690 0.046 Uiso 1 1 calc R . . . .
C10 C 0.4091(4) 0.58588(12) 0.3913(4) 0.0445(9) Uani 1 1 d . . . . .
H10 H 0.443095 0.586458 0.317933 0.053 Uiso 1 1 calc R . . . .
C11 C 0.3693(4) 0.61953(11) 0.4548(3) 0.0425(9) Uani 1 1 d . . . . .
H11 H 0.372254 0.646679 0.428645 0.051 Uiso 1 1 calc R . . . .
C12 C 0.2640(5) 0.44421(10) 0.8134(4) 0.0473(10) Uani 1 1 d . . . . .
C13 C 0.6304(4) 0.62137(11) 0.8398(4) 0.0409(8) Uani 1 1 d . . . . .
H13 H 0.642774 0.593281 0.854832 0.049 Uiso 1 1 calc R . . . .
C14 C 0.7472(4) 0.64905(12) 0.8582(4) 0.0510(10) Uani 1 1 d . . . . .
H14 H 0.848915 0.643027 0.886757 0.061 Uiso 1 1 calc R . . . .
C15 C 0.6833(4) 0.68657(12) 0.8262(4) 0.0495(10) Uani 1 1 d . . . . .
H15 H 0.732846 0.711317 0.828528 0.059 Uiso 1 1 calc R . . . .
C16 C 0.4126(4) 0.70771(9) 0.7363(3) 0.0304(7) Uani 1 1 d . . . . .
C17 C 0.4165(4) 0.75003(9) 0.7311(3) 0.0341(8) Uani 1 1 d . . . . .
H17 H 0.506299 0.764346 0.763952 0.041 Uiso 1 1 calc R . . . .
C18 C 0.2810(4) 0.77032(9) 0.6747(3) 0.0325(8) Uani 1 1 d . . . . .
C19 C 0.1475(4) 0.74836(9) 0.6222(3) 0.0334(7) Uani 1 1 d . . . . .
H19 H 0.056740 0.761692 0.581636 0.040 Uiso 1 1 calc R . . . .
C20 C 0.1551(4) 0.70602(9) 0.6326(3) 0.0287(7) Uani 1 1 d . . . . .
C21 C -0.1145(4) 0.68368(11) 0.5346(4) 0.0419(9) Uani 1 1 d . . . . .
H21 H -0.165131 0.708422 0.509943 0.050 Uiso 1 1 calc R . . . .
C22 C -0.1768(4) 0.64575(12) 0.5195(4) 0.0509(10) Uani 1 1 d . . . . .
H22 H -0.278065 0.639389 0.482300 0.061 Uiso 1 1 calc R . . . .
C23 C -0.0585(4) 0.61818(11) 0.5711(4) 0.0410(9) Uani 1 1 d . . . . .
H23 H -0.069338 0.589875 0.573370 0.049 Uiso 1 1 calc R . . . .
C24 C 0.2823(5) 0.81697(10) 0.6739(4) 0.0402(9) Uani 1 1 d . . . . .
Cl02 Cl -0.17162(11) 0.52533(3) 0.76353(10) 0.0473(2) Uani 1 1 d D U . . .
O6 O -0.0925(3) 0.55923(9) 0.8386(3) 0.0747(9) Uani 1 1 d D U . . .
O3B O -0.1047(19) 0.4872(5) 0.762(3) 0.101(8) Uani 0.305(19) 1 d D U P A 2
O4B O -0.242(3) 0.5401(5) 0.6292(11) 0.077(6) Uani 0.305(19) 1 d D U P A 2
O5B O -0.299(2) 0.5167(8) 0.801(2) 0.089(7) Uani 0.305(19) 1 d D U P A 2
Cl03 Cl 0.94353(12) 0.77227(3) 0.85627(13) 0.0570(3) Uani 1 1 d D U . . .
O8 O 0.8207(3) 0.77730(9) 0.9031(3) 0.0682(9) Uani 1 1 d D U . . .
O7 O 0.921(3) 0.7400(8) 0.769(3) 0.157(11) Uani 0.282(12) 1 d D U P B 2
O9 O 1.0707(17) 0.7581(7) 0.964(2) 0.150(8) Uani 0.282(12) 1 d D U P B 2
O10 O 1.002(2) 0.8070(3) 0.8277(19) 0.072(6) Uani 0.282(12) 1 d D U P B 2
O0AA O 0.9823(8) 0.73194(16) 0.8529(8) 0.076(2) Uani 0.718(12) 1 d D U P B 1
O1AA O 0.8977(10) 0.7878(3) 0.7197(8) 0.145(5) Uani 0.718(12) 1 d D U P B 1
O2AA O 1.0597(7) 0.7952(3) 0.9372(13) 0.172(5) Uani 0.718(12) 1 d D U P B 1
O3 O -0.1067(9) 0.4897(2) 0.8389(9) 0.077(2) Uani 0.695(19) 1 d D U P A 1
O4 O -0.3244(8) 0.5260(3) 0.7478(14) 0.103(4) Uani 0.695(19) 1 d D U P A 1
O5 O -0.1418(15) 0.5226(3) 0.6409(8) 0.097(4) Uani 0.695(19) 1 d D U P A 1


_geom_special_details            
;
 All esds (except the esd in the dihedral angle between two l.s. planes)
 are estimated using the full covariance matrix.  The cell esds are taken
 into account individually in the estimation of esds in distances, angles
 and torsion angles; correlations between esds in cell parameters are only
 used when they are defined by crystal symmetry.  An approximate (isotropic)
 treatment of cell esds is used for estimating esds involving l.s. planes.
;
loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
_geom_bond_publ_flag
Fe1 N1 1.964(3) . ?
Fe1 N3 1.892(2) . ?
Fe1 N5 1.968(3) . ?
Fe1 N6 1.959(3) . ?
Fe1 N8 1.889(2) . ?
Fe1 N10 1.969(3) . ?
O1 C12 1.210(4) . ?
O2 C24 1.222(4) . ?
N1 N2 1.374(3) . ?
N1 C1 1.324(4) . ?
N2 C3 1.353(4) . ?
N2 C4 1.397(4) . ?
N3 C4 1.333(4) . ?
N3 C8 1.339(4) . ?
N4 N5 1.375(3) . ?
N4 C8 1.401(4) . ?
N4 C9 1.354(4) . ?
N5 C11 1.319(4) . ?
N6 N7 1.378(3) . ?
N6 C13 1.319(4) . ?
N7 C15 1.352(4) . ?
N7 C16 1.399(4) . ?
N8 C16 1.339(4) . ?
N8 C20 1.334(4) . ?
N9 N10 1.382(3) . ?
N9 C20 1.394(4) . ?
N9 C21 1.351(4) . ?
N10 C23 1.321(4) . ?
N11 H11A 0.8600 . ?
N11 H11B 0.8600 . ?
N11 C12 1.308(5) . ?
N12 H12A 0.8600 . ?
N12 H12B 0.8600 . ?
N12 C24 1.324(5) . ?
C1 H1 0.9300 . ?
C1 C2 1.389(5) . ?
C2 H2 0.9300 . ?
C2 C3 1.354(5) . ?
C3 H3 0.9300 . ?
C4 C5 1.381(4) . ?
C5 H5 0.9300 . ?
C5 C6 1.394(4) . ?
C6 C7 1.389(4) . ?
C6 C12 1.512(4) . ?
C7 H7 0.9300 . ?
C7 C8 1.373(4) . ?
C9 H9 0.9300 . ?
C9 C10 1.352(5) . ?
C10 H10 0.9300 . ?
C10 C11 1.401(5) . ?
C11 H11 0.9300 . ?
C13 H13 0.9300 . ?
C13 C14 1.391(5) . ?
C14 H14 0.9300 . ?
C14 C15 1.356(5) . ?
C15 H15 0.9300 . ?
C16 C17 1.382(4) . ?
C17 H17 0.9300 . ?
C17 C18 1.388(5) . ?
C18 C19 1.397(5) . ?
C18 C24 1.521(4) . ?
C19 H19 0.9300 . ?
C19 C20 1.385(4) . ?
C21 H21 0.9300 . ?
C21 C22 1.357(5) . ?
C22 H22 0.9300 . ?
C22 C23 1.397(5) . ?
C23 H23 0.9300 . ?
Cl02 O6 1.417(3) . ?
Cl02 O3B 1.399(10) . ?
Cl02 O4B 1.426(9) . ?
Cl02 O5B 1.421(11) . ?
Cl02 O3 1.422(5) . ?
Cl02 O4 1.402(7) . ?
Cl02 O5 1.411(5) . ?
Cl03 O8 1.419(3) . ?
Cl03 O7 1.363(11) . ?
Cl03 O9 1.422(12) . ?
Cl03 O10 1.336(9) . ?
Cl03 O0AA 1.369(5) . ?
Cl03 O1AA 1.442(6) . ?
Cl03 O2AA 1.366(6) . ?

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 N5 160.36(11) . . ?
N1 Fe1 N10 89.94(11) . . ?
N3 Fe1 N1 80.19(10) . . ?
N3 Fe1 N5 80.18(10) . . ?
N3 Fe1 N6 99.60(11) . . ?
N3 Fe1 N10 99.91(11) . . ?
N5 Fe1 N10 93.97(11) . . ?
N6 Fe1 N1 94.72(11) . . ?
N6 Fe1 N5 88.00(11) . . ?
N6 Fe1 N10 160.44(10) . . ?
N8 Fe1 N1 97.00(10) . . ?
N8 Fe1 N3 177.19(11) . . ?
N8 Fe1 N5 102.62(10) . . ?
N8 Fe1 N6 80.40(11) . . ?
N8 Fe1 N10 80.18(11) . . ?
N2 N1 Fe1 112.55(19) . . ?
C1 N1 Fe1 142.6(2) . . ?
C1 N1 N2 104.6(3) . . ?
N1 N2 C4 116.4(2) . . ?
C3 N2 N1 110.9(3) . . ?
C3 N2 C4 132.5(3) . . ?
C4 N3 Fe1 119.9(2) . . ?
C4 N3 C8 119.9(3) . . ?
C8 N3 Fe1 120.2(2) . . ?
N5 N4 C8 116.7(2) . . ?
C9 N4 N5 110.9(3) . . ?
C9 N4 C8 132.2(3) . . ?
N4 N5 Fe1 112.43(18) . . ?
C11 N5 Fe1 141.8(2) . . ?
C11 N5 N4 104.9(3) . . ?
N7 N6 Fe1 112.37(19) . . ?
C13 N6 Fe1 141.2(2) . . ?
C13 N6 N7 105.0(3) . . ?
N6 N7 C16 116.6(3) . . ?
C15 N7 N6 110.8(3) . . ?
C15 N7 C16 132.2(3) . . ?
C16 N8 Fe1 120.0(2) . . ?
C20 N8 Fe1 119.7(2) . . ?
C20 N8 C16 120.1(3) . . ?
N10 N9 C20 115.9(3) . . ?
C21 N9 N10 110.7(3) . . ?
C21 N9 C20 133.4(3) . . ?
N9 N10 Fe1 112.39(19) . . ?
C23 N10 Fe1 142.2(2) . . ?
C23 N10 N9 105.1(3) . . ?
H11A N11 H11B 120.0 . . ?
C12 N11 H11A 120.0 . . ?
C12 N11 H11B 120.0 . . ?
H12A N12 H12B 120.0 . . ?
C24 N12 H12A 120.0 . . ?
C24 N12 H12B 120.0 . . ?
N1 C1 H1 124.3 . . ?
N1 C1 C2 111.5(3) . . ?
C2 C1 H1 124.3 . . ?
C1 C2 H2 127.0 . . ?
C3 C2 C1 106.0(3) . . ?
C3 C2 H2 127.0 . . ?
N2 C3 C2 107.2(3) . . ?
N2 C3 H3 126.4 . . ?
C2 C3 H3 126.4 . . ?
N3 C4 N2 110.9(3) . . ?
N3 C4 C5 122.4(3) . . ?
C5 C4 N2 126.7(3) . . ?
C4 C5 H5 121.5 . . ?
C4 C5 C6 116.9(3) . . ?
C6 C5 H5 121.5 . . ?
C5 C6 C12 121.4(3) . . ?
C7 C6 C5 121.1(3) . . ?
C7 C6 C12 117.5(3) . . ?
C6 C7 H7 121.3 . . ?
C8 C7 C6 117.4(3) . . ?
C8 C7 H7 121.3 . . ?
N3 C8 N4 110.4(3) . . ?
N3 C8 C7 122.2(3) . . ?
C7 C8 N4 127.3(3) . . ?
N4 C9 H9 126.4 . . ?
C10 C9 N4 107.2(3) . . ?
C10 C9 H9 126.4 . . ?
C9 C10 H10 127.1 . . ?
C9 C10 C11 105.8(3) . . ?
C11 C10 H10 127.1 . . ?
N5 C11 C10 111.2(3) . . ?
N5 C11 H11 124.4 . . ?
C10 C11 H11 124.4 . . ?
O1 C12 N11 124.1(3) . . ?
O1 C12 C6 119.6(3) . . ?
N11 C12 C6 116.2(3) . . ?
N6 C13 H13 124.5 . . ?
N6 C13 C14 111.0(3) . . ?
C14 C13 H13 124.5 . . ?
C13 C14 H14 126.8 . . ?
C15 C14 C13 106.4(3) . . ?
C15 C14 H14 126.8 . . ?
N7 C15 C14 106.8(3) . . ?
N7 C15 H15 126.6 . . ?
C14 C15 H15 126.6 . . ?
N8 C16 N7 110.3(3) . . ?
N8 C16 C17 122.4(3) . . ?
C17 C16 N7 127.4(3) . . ?
C16 C17 H17 121.3 . . ?
C16 C17 C18 117.4(3) . . ?
C18 C17 H17 121.3 . . ?
C17 C18 C19 120.7(3) . . ?
C17 C18 C24 118.1(3) . . ?
C19 C18 C24 121.2(3) . . ?
C18 C19 H19 121.2 . . ?
C20 C19 C18 117.6(3) . . ?
C20 C19 H19 121.2 . . ?
N8 C20 N9 111.5(3) . . ?
N8 C20 C19 121.9(3) . . ?
C19 C20 N9 126.6(3) . . ?
N9 C21 H21 126.4 . . ?
N9 C21 C22 107.1(3) . . ?
C22 C21 H21 126.4 . . ?
C21 C22 H22 126.9 . . ?
C21 C22 C23 106.2(3) . . ?
C23 C22 H22 126.9 . . ?
N10 C23 C22 110.9(3) . . ?
N10 C23 H23 124.6 . . ?
C22 C23 H23 124.6 . . ?
O2 C24 N12 124.1(3) . . ?
O2 C24 C18 120.4(3) . . ?
N12 C24 C18 115.6(3) . . ?
O6 Cl02 O4B 105.7(6) . . ?
O6 Cl02 O5B 110.0(11) . . ?
O6 Cl02 O3 106.2(5) . . ?
O3B Cl02 O6 122.9(8) . . ?
O3B Cl02 O4B 110.5(10) . . ?
O3B Cl02 O5B 105.1(14) . . ?
O5B Cl02 O4B 100.4(11) . . ?
O4 Cl02 O6 112.7(4) . . ?
O4 Cl02 O3 108.4(6) . . ?
O4 Cl02 O5 114.2(5) . . ?
O5 Cl02 O6 109.0(3) . . ?
O5 Cl02 O3 105.9(4) . . ?
O8 Cl03 O9 109.9(9) . . ?
O8 Cl03 O1AA 107.2(3) . . ?
O7 Cl03 O8 111.0(9) . . ?
O7 Cl03 O9 100.5(17) . . ?
O10 Cl03 O8 115.4(6) . . ?
O10 Cl03 O7 119.1(12) . . ?
O10 Cl03 O9 98.6(11) . . ?
O0AA Cl03 O8 112.3(3) . . ?
O0AA Cl03 O1AA 107.8(5) . . ?
O2AA Cl03 O8 107.8(4) . . ?
O2AA Cl03 O0AA 112.0(5) . . ?
O2AA Cl03 O1AA 109.6(7) . . ?

loop_
_geom_torsion_atom_site_label_1
_geom_torsion_atom_site_label_2
_geom_torsion_atom_site_label_3
_geom_torsion_atom_site_label_4
_geom_torsion
_geom_torsion_site_symmetry_1
_geom_torsion_site_symmetry_2
_geom_torsion_site_symmetry_3
_geom_torsion_site_symmetry_4
_geom_torsion_publ_flag
Fe1 N1 N2 C3 -175.3(2) . . . . ?
Fe1 N1 N2 C4 0.8(3) . . . . ?
Fe1 N1 C1 C2 173.1(3) . . . . ?
Fe1 N3 C4 N2 -2.0(4) . . . . ?
Fe1 N3 C4 C5 177.1(3) . . . . ?
Fe1 N3 C8 N4 2.0(4) . . . . ?
Fe1 N3 C8 C7 -178.2(3) . . . . ?
Fe1 N5 C11 C10 166.9(3) . . . . ?
Fe1 N6 N7 C15 -169.3(2) . . . . ?
Fe1 N6 N7 C16 5.0(3) . . . . ?
Fe1 N6 C13 C14 164.2(3) . . . . ?
Fe1 N8 C16 N7 5.4(3) . . . . ?
Fe1 N8 C16 C17 -173.8(2) . . . . ?
Fe1 N8 C20 N9 -4.0(3) . . . . ?
Fe1 N8 C20 C19 174.1(2) . . . . ?
Fe1 N10 C23 C22 172.3(3) . . . . ?
N1 Fe1 N3 C4 2.0(2) . . . . ?
N1 Fe1 N3 C8 -179.4(3) . . . . ?
N1 Fe1 N8 C16 91.3(2) . . . . ?
N1 Fe1 N8 C20 -83.6(2) . . . . ?
N1 N2 C3 C2 -0.3(4) . . . . ?
N1 N2 C4 N3 0.7(4) . . . . ?
N1 N2 C4 C5 -178.4(3) . . . . ?
N1 C1 C2 C3 0.0(4) . . . . ?
N2 N1 C1 C2 -0.2(4) . . . . ?
N2 C4 C5 C6 179.8(3) . . . . ?
N3 C4 C5 C6 0.8(5) . . . . ?
N4 N5 C11 C10 -0.5(4) . . . . ?
N4 C9 C10 C11 -0.4(4) . . . . ?
N5 Fe1 N3 C4 -178.6(3) . . . . ?
N5 Fe1 N3 C8 0.1(2) . . . . ?
N5 Fe1 N8 C16 -88.0(2) . . . . ?
N5 Fe1 N8 C20 97.0(2) . . . . ?
N5 N4 C8 N3 -3.9(4) . . . . ?
N5 N4 C8 C7 176.3(3) . . . . ?
N5 N4 C9 C10 0.1(4) . . . . ?
N6 Fe1 N3 C4 95.1(2) . . . . ?
N6 Fe1 N3 C8 -86.2(2) . . . . ?
N6 Fe1 N8 C16 -2.3(2) . . . . ?
N6 Fe1 N8 C20 -177.2(2) . . . . ?
N6 N7 C15 C14 -0.2(4) . . . . ?
N6 N7 C16 N8 -6.6(4) . . . . ?
N6 N7 C16 C17 172.6(3) . . . . ?
N6 C13 C14 C15 0.1(5) . . . . ?
N7 N6 C13 C14 -0.2(4) . . . . ?
N7 C16 C17 C18 -178.8(3) . . . . ?
N8 C16 C17 C18 0.3(5) . . . . ?
N9 N10 C23 C22 -0.3(4) . . . . ?
N9 C21 C22 C23 0.3(4) . . . . ?
N10 Fe1 N3 C4 -86.2(2) . . . . ?
N10 Fe1 N3 C8 92.4(2) . . . . ?
N10 Fe1 N8 C16 -180.0(2) . . . . ?
N10 Fe1 N8 C20 5.1(2) . . . . ?
N10 N9 C20 N8 -0.6(4) . . . . ?
N10 N9 C20 C19 -178.6(3) . . . . ?
N10 N9 C21 C22 -0.5(4) . . . . ?
C1 N1 N2 C3 0.3(4) . . . . ?
C1 N1 N2 C4 176.4(3) . . . . ?
C1 C2 C3 N2 0.1(4) . . . . ?
C3 N2 C4 N3 175.7(3) . . . . ?
C3 N2 C4 C5 -3.3(6) . . . . ?
C4 N2 C3 C2 -175.5(3) . . . . ?
C4 N3 C8 N4 -179.3(3) . . . . ?
C4 N3 C8 C7 0.5(5) . . . . ?
C4 C5 C6 C7 1.0(5) . . . . ?
C4 C5 C6 C12 -179.1(3) . . . . ?
C5 C6 C7 C8 -1.9(5) . . . . ?
C5 C6 C12 O1 -131.2(4) . . . . ?
C5 C6 C12 N11 50.4(6) . . . . ?
C6 C7 C8 N3 1.2(5) . . . . ?
C6 C7 C8 N4 -179.0(3) . . . . ?
C7 C6 C12 O1 48.7(6) . . . . ?
C7 C6 C12 N11 -129.7(4) . . . . ?
C8 N3 C4 N2 179.3(3) . . . . ?
C8 N3 C4 C5 -1.6(5) . . . . ?
C8 N4 N5 Fe1 4.0(3) . . . . ?
C8 N4 N5 C11 175.7(3) . . . . ?
C8 N4 C9 C10 -174.4(3) . . . . ?
C9 N4 N5 Fe1 -171.4(2) . . . . ?
C9 N4 N5 C11 0.3(4) . . . . ?
C9 N4 C8 N3 170.3(3) . . . . ?
C9 N4 C8 C7 -9.5(6) . . . . ?
C9 C10 C11 N5 0.6(4) . . . . ?
C12 C6 C7 C8 178.1(3) . . . . ?
C13 N6 N7 C15 0.3(4) . . . . ?
C13 N6 N7 C16 174.5(3) . . . . ?
C13 C14 C15 N7 0.0(4) . . . . ?
C15 N7 C16 N8 166.1(3) . . . . ?
C15 N7 C16 C17 -14.7(6) . . . . ?
C16 N7 C15 C14 -173.2(3) . . . . ?
C16 N8 C20 N9 -178.9(3) . . . . ?
C16 N8 C20 C19 -0.8(4) . . . . ?
C16 C17 C18 C19 -1.9(5) . . . . ?
C16 C17 C18 C24 177.3(3) . . . . ?
C17 C18 C19 C20 2.1(5) . . . . ?
C17 C18 C24 O2 20.6(5) . . . . ?
C17 C18 C24 N12 -160.1(3) . . . . ?
C18 C19 C20 N8 -0.8(5) . . . . ?
C18 C19 C20 N9 177.0(3) . . . . ?
C19 C18 C24 O2 -160.2(3) . . . . ?
C19 C18 C24 N12 19.1(5) . . . . ?
C20 N8 C16 N7 -179.7(3) . . . . ?
C20 N8 C16 C17 1.1(5) . . . . ?
C20 N9 N10 Fe1 4.5(3) . . . . ?
C20 N9 N10 C23 179.6(3) . . . . ?
C20 N9 C21 C22 -179.4(3) . . . . ?
C21 N9 N10 Fe1 -174.6(2) . . . . ?
C21 N9 N10 C23 0.5(4) . . . . ?
C21 N9 C20 N8 178.2(3) . . . . ?
C21 N9 C20 C19 0.3(6) . . . . ?
C21 C22 C23 N10 0.0(4) . . . . ?
C24 C18 C19 C20 -177.0(3) . . . . ?


_olex2_submission_special_instructions 'No special instructions were received'
_oxdiff_exptl_absorpt_empirical_details 
;
Empirical correction (ABSPACK) includes:
- Absorption correction using spherical harmonics
- Frame scaling
;
_oxdiff_exptl_absorpt_empirical_full_max 1.018
_oxdiff_exptl_absorpt_empirical_full_min 0.981
