#------------------------------------------------------------------------------
#$Date: 2019-05-08 01:30:27 +0300 (Wed, 08 May 2019) $
#$Revision: 214979 $
#$URL: file:///home/coder/svn-repositories/cod/cif/1/55/09/1550982.cif $
#------------------------------------------------------------------------------
#
# This file is available in the Crystallography Open Database (COD),
# http://www.crystallography.net/
#
# All data on this site have been placed in the public domain by the
# contributors.
#
data_1550982
loop_
_publ_author_name
'Kiernicki, John J.'
'Shanahan, James P.'
'Zeller, Matthias'
'Szymczak, Nathaniel K.'
_publ_section_title
;
 Tuning ligand field strength with pendent Lewis acids: access to high
 spin iron hydrides
;
_journal_name_full               'Chemical Science'
_journal_paper_doi               10.1039/C9SC00561G
_journal_year                    2019
_chemical_absolute_configuration ad
_chemical_formula_moiety         'C43 H71 B2 Fe N7, C H2 Cl2'
_chemical_formula_sum            'C44 H73 B2 Cl2 Fe N7'
_chemical_formula_weight         848.46
_chemical_properties_physical    Air-sensitive,Moisture-sensitive,Hygroscopic
_space_group_crystal_system      tetragonal
_space_group_IT_number           96
_space_group_name_Hall           'P 4nw 2abw'
_space_group_name_H-M_alt        'P 43 21 2'
_symmetry_space_group_name_Hall  'P 4nw 2abw'
_symmetry_space_group_name_H-M   'P 43 21 2'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     isomor
_atom_sites_solution_secondary   difmap
_audit_creation_method           SHELXL-2017/1
_audit_update_record
;
2018-12-10 deposited with the CCDC.    2019-04-26 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 90
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   16.4289(8)
_cell_length_b                   16.4289(8)
_cell_length_c                   16.7181(10)
_cell_measurement_reflns_used    9758
_cell_measurement_temperature    150(2)
_cell_measurement_theta_max      28.2673
_cell_measurement_theta_min      3.0056
_cell_volume                     4512.4(4)
_computing_cell_refinement       'SAINT V8.37A (Bruker, 2016)'
_computing_data_collection       'Apex3 v2016.9-0 (Bruker, 2016)'
_computing_data_reduction        'SAINT V8.37A (Bruker, 2016)'
_computing_structure_refinement
;  
SHELXL-2017/1 (Sheldrick, 2017), 
SHELXLE Rev859 (Hübschle et al., 2011)
;
_computing_structure_solution    'SHELXS-97 (Sheldrick, 2008)'
_diffrn_ambient_temperature      150(2)
_diffrn_measured_fraction_theta_full 0.982
_diffrn_measured_fraction_theta_max 0.956
_diffrn_measurement_device_type  'Bruker AXS D8 Quest CMOS diffractometer'
_diffrn_measurement_method       'omega and phi scans'
_diffrn_radiation_monochromator  'Triumph curved graphite crystal'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0798
_diffrn_reflns_av_unetI/netI     0.0438
_diffrn_reflns_Laue_measured_fraction_full 0.982
_diffrn_reflns_Laue_measured_fraction_max 0.956
_diffrn_reflns_limit_h_max       21
_diffrn_reflns_limit_h_min       -21
_diffrn_reflns_limit_k_max       21
_diffrn_reflns_limit_k_min       -21
_diffrn_reflns_limit_l_max       19
_diffrn_reflns_limit_l_min       -20
_diffrn_reflns_number            47133
_diffrn_reflns_point_group_measured_fraction_full 0.981
_diffrn_reflns_point_group_measured_fraction_max 0.951
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         28.263
_diffrn_reflns_theta_min         3.477
_diffrn_source                   'sealed tube X-ray source'
_exptl_absorpt_coefficient_mu    0.492
_exptl_absorpt_correction_T_max  0.2627
_exptl_absorpt_correction_T_min  0.1939
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
 SADABS 2016/2: Krause, L., Herbst-Irmer, R., Sheldrick G.M. & Stalke D.,
 J. Appl. Cryst. 48 (2015) 3-10
;
_exptl_crystal_colour            orange
_exptl_crystal_density_diffrn    1.249
_exptl_crystal_description       block
_exptl_crystal_F_000             1824
_exptl_crystal_recrystallization_method 'Re-crystallisation from solvent'
_exptl_crystal_size_max          0.230
_exptl_crystal_size_mid          0.210
_exptl_crystal_size_min          0.160
_refine_diff_density_max         0.585
_refine_diff_density_min         -0.461
_refine_diff_density_rms         0.073
_refine_ls_abs_structure_details
;
 Flack x determined using 1784 quotients [(I+)-(I-)]/[(I+)+(I-)]
 (Parsons, Flack and Wagner, Acta Cryst. B69 (2013) 249-259).
;
_refine_ls_abs_structure_Flack   -0.050(6)
_refine_ls_extinction_coef       0.0023(9)
_refine_ls_extinction_expression Fc^*^=kFc[1+0.001xFc²λ³/sin(2θ)]^-1/4^
_refine_ls_extinction_method     'SHELXL-2017/1 (Sheldrick 2017)'
_refine_ls_goodness_of_fit_ref   1.079
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     420
_refine_ls_number_reflns         5321
_refine_ls_number_restraints     317
_refine_ls_restrained_S_all      1.065
_refine_ls_R_factor_all          0.0759
_refine_ls_R_factor_gt           0.0583
_refine_ls_shift/su_max          0.000
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[σ²(Fo²)+(0.0236P)²+5.4853P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1193
_refine_ls_wR_factor_ref         0.1322
_reflns_Friedel_coverage         0.737
_reflns_Friedel_fraction_full    0.978
_reflns_Friedel_fraction_max     0.944
_reflns_number_gt                4539
_reflns_number_total             5321
_reflns_threshold_expression     'I > 2σ(I)'
_cod_data_source_file            c9sc00561g2.cif
_cod_data_source_block           JK2150_0m
_cod_original_cell_volume        4512.4(5)
_cod_database_code               1550982
_shelx_shelxl_version_number     2017/1
_shelx_space_group_comment
;
The symmetry employed for this shelxl refinement is uniquely defined
by the following loop, which should always be used as a source of
symmetry information in preference to the above space-group names.
They are only intended as comments.
;
_shelx_estimated_absorpt_t_min   0.895
_shelx_estimated_absorpt_t_max   0.925
loop_
_space_group_symop_operation_xyz
'x, y, z'
'-x, -y, z+1/2'
'-y+1/2, x+1/2, z+3/4'
'y+1/2, -x+1/2, z+1/4'
'-x+1/2, y+1/2, -z+3/4'
'x+1/2, -y+1/2, -z+1/4'
'y, x, -z'
'-y, -x, -z+1/2'
loop_
_atom_site_label
_atom_site_type_symbol
_atom_site_fract_x
_atom_site_fract_y
_atom_site_fract_z
_atom_site_U_iso_or_equiv
_atom_site_adp_type
_atom_site_occupancy
_atom_site_site_symmetry_order
_atom_site_calc_flag
_atom_site_refinement_flags_posn
_atom_site_refinement_flags_adp
_atom_site_refinement_flags_occupancy
_atom_site_disorder_assembly
_atom_site_disorder_group
Fe1 Fe 0.22361(4) 0.22361(4) 0.000000 0.0352(2) Uani 1 2 d S T P . .
N1 N 0.31693(19) 0.31693(19) 0.000000 0.0331(9) Uani 1 2 d S T P A .
N2 N 0.2002(2) 0.3054(2) 0.1113(2) 0.0378(8) Uani 1 1 d . . . . .
N3 N 0.1473(2) 0.3156(2) 0.1730(2) 0.0376(8) Uani 1 1 d D . . . .
C1 C 0.3181(2) 0.3742(2) 0.0575(2) 0.0339(8) Uani 1 1 d . . . . .
C2 C 0.3777(3) 0.4348(2) 0.0598(3) 0.0388(9) Uani 1 1 d . . . . .
H2 H 0.378356 0.474263 0.101296 0.047 Uiso 1 1 calc R U . . .
C3 C 0.4357(2) 0.4357(2) 0.000000 0.0383(12) Uani 1 2 d S T P . .
H3 H 0.476625 0.476622 0.000002 0.046 Uiso 1 2 calc R U P . .
C4 C 0.2526(2) 0.3672(2) 0.1168(3) 0.0351(9) Uani 1 1 d . . . . .
C5 C 0.2338(3) 0.4173(2) 0.1821(2) 0.0360(8) Uani 1 1 d . . . . .
H5 H 0.262106 0.464741 0.198827 0.043 Uiso 1 1 calc R U . . .
C6 C 0.1657(3) 0.3833(3) 0.2170(2) 0.0369(8) Uani 1 1 d . . . . .
C7 C 0.1202(3) 0.4121(3) 0.2909(3) 0.0417(10) Uani 1 1 d . . . . .
C8 C 0.1661(4) 0.4846(3) 0.3264(3) 0.0536(12) Uani 1 1 d . . . . .
H8A H 0.167323 0.529086 0.287345 0.080 Uiso 1 1 calc R U . . .
H8AB H 0.221890 0.468177 0.339355 0.080 Uiso 1 1 calc R U . . .
H8AC H 0.138478 0.502943 0.375093 0.080 Uiso 1 1 calc R U . . .
C9 C 0.0343(3) 0.4413(4) 0.2693(3) 0.0593(15) Uani 1 1 d . . . . .
H9A H 0.002549 0.395492 0.248536 0.089 Uiso 1 1 calc R U . . .
H9AB H 0.037904 0.483901 0.228336 0.089 Uiso 1 1 calc R U . . .
H9AC H 0.007693 0.463311 0.317063 0.089 Uiso 1 1 calc R U . . .
C10 C 0.1175(4) 0.3449(3) 0.3551(3) 0.0553(13) Uani 1 1 d . . . . .
H10A H 0.086643 0.298246 0.334650 0.083 Uiso 1 1 calc R U . . .
H10B H 0.090974 0.365924 0.403365 0.083 Uiso 1 1 calc R U . . .
H10C H 0.173049 0.327719 0.368032 0.083 Uiso 1 1 calc R U . . .
C11 C 0.0831(4) 0.2535(4) 0.1845(5) 0.0415(18) Uani 0.852(5) 1 d D U P A 1
H11A H 0.036493 0.278155 0.213069 0.050 Uiso 0.852(5) 1 calc R U P A 1
H11B H 0.104708 0.208679 0.217954 0.050 Uiso 0.852(5) 1 calc R U P A 1
C12 C 0.0541(3) 0.2191(3) 0.1046(3) 0.0392(10) Uani 0.852(5) 1 d D U P A 1
H12A H 0.009844 0.179581 0.115106 0.047 Uiso 0.852(5) 1 calc R U P A 1
H12B H 0.099622 0.188848 0.079702 0.047 Uiso 0.852(5) 1 calc R U P A 1
C13 C 0.0228(3) 0.2825(3) 0.0442(3) 0.0386(11) Uani 0.852(5) 1 d D U P A 1
H13A H 0.053806 0.333636 0.051874 0.046 Uiso 0.852(5) 1 calc R U P A 1
H13B H -0.034966 0.294283 0.056259 0.046 Uiso 0.852(5) 1 calc R U P A 1
B1 B 0.0299(3) 0.2557(4) -0.0492(4) 0.0403(12) Uani 0.852(5) 1 d D U P A 1
N4 N 0.1266(6) 0.2639(6) -0.0727(6) 0.0408(10) Uani 0.852(5) 1 d D U P A 1
H4 H 0.132678 0.233372 -0.124098 0.049 Uiso 0.852(5) 1 calc R U P A 1
C22 C 0.1516(6) 0.3489(5) -0.0915(6) 0.053(2) Uani 0.852(5) 1 d D U P A 1
H22A H 0.113268 0.372626 -0.129891 0.079 Uiso 0.852(5) 1 calc R U P A 1
H22B H 0.206406 0.348691 -0.114633 0.079 Uiso 0.852(5) 1 calc R U P A 1
H22C H 0.151599 0.381380 -0.042311 0.079 Uiso 0.852(5) 1 calc R U P A 1
C14 C 0.0000(4) 0.1622(4) -0.0672(5) 0.0440(14) Uani 0.852(5) 1 d D U P A 1
H14 H 0.034828 0.124374 -0.035245 0.053 Uiso 0.852(5) 1 calc R U P A 1
C15 C -0.0893(3) 0.1540(4) -0.0372(4) 0.0491(13) Uani 0.852(5) 1 d D U P A 1
H15A H -0.108504 0.098052 -0.048656 0.059 Uiso 0.852(5) 1 calc R U P A 1
H15B H -0.089916 0.161317 0.021551 0.059 Uiso 0.852(5) 1 calc R U P A 1
C16 C -0.1495(3) 0.2146(4) -0.0746(4) 0.0519(14) Uani 0.852(5) 1 d D U P A 1
H16A H -0.165257 0.194115 -0.128069 0.062 Uiso 0.852(5) 1 calc R U P A 1
H16B H -0.199262 0.215791 -0.041194 0.062 Uiso 0.852(5) 1 calc R U P A 1
C17 C -0.1181(3) 0.3017(4) -0.0837(4) 0.0503(15) Uani 0.852(5) 1 d D U P A 1
H17A H -0.126073 0.330239 -0.032118 0.060 Uiso 0.852(5) 1 calc R U P A 1
H17B H -0.152290 0.329713 -0.123971 0.060 Uiso 0.852(5) 1 calc R U P A 1
C18 C -0.0278(4) 0.3116(5) -0.1086(4) 0.0488(17) Uani 0.852(5) 1 d D U P A 1
H18 H -0.012107 0.370067 -0.102065 0.059 Uiso 0.852(5) 1 calc R U P A 1
C19 C -0.0153(4) 0.2874(5) -0.1968(4) 0.0581(17) Uani 0.852(5) 1 d D U P A 1
H19A H -0.052392 0.320709 -0.230069 0.070 Uiso 0.852(5) 1 calc R U P A 1
H19B H 0.041067 0.301653 -0.212196 0.070 Uiso 0.852(5) 1 calc R U P A 1
C20 C -0.0295(5) 0.1981(6) -0.2173(5) 0.068(2) Uani 0.852(5) 1 d D U P A 1
H20A H -0.005336 0.186704 -0.270348 0.081 Uiso 0.852(5) 1 calc R U P A 1
H20B H -0.088786 0.188242 -0.221173 0.081 Uiso 0.852(5) 1 calc R U P A 1
C21 C 0.0072(4) 0.1384(4) -0.1554(4) 0.0552(15) Uani 0.852(5) 1 d D U P A 1
H21A H -0.019466 0.084883 -0.162608 0.066 Uiso 0.852(5) 1 calc R U P A 1
H21B H 0.065604 0.131280 -0.168032 0.066 Uiso 0.852(5) 1 calc R U P A 1
C11B C 0.0725(18) 0.2665(18) 0.171(3) 0.040(5) Uani 0.148(5) 1 d D U P A 2
H11C H 0.031202 0.293353 0.136898 0.047 Uiso 0.148(5) 1 calc R U P A 2
H11D H 0.049916 0.261130 0.225669 0.047 Uiso 0.148(5) 1 calc R U P A 2
C12B C 0.0930(16) 0.1828(16) 0.1375(18) 0.041(4) Uani 0.148(5) 1 d D U P A 2
H12C H 0.042197 0.150346 0.137030 0.049 Uiso 0.148(5) 1 calc R U P A 2
H12D H 0.109791 0.190084 0.081073 0.049 Uiso 0.148(5) 1 calc R U P A 2
C13B C 0.1580(15) 0.1322(15) 0.1786(16) 0.042(5) Uani 0.148(5) 1 d D U P A 2
H13C H 0.131203 0.099507 0.220854 0.050 Uiso 0.148(5) 1 calc R U P A 2
H13D H 0.195988 0.170020 0.205696 0.050 Uiso 0.148(5) 1 calc R U P A 2
B1B B 0.2119(16) 0.0704(14) 0.1235(16) 0.046(4) Uani 0.148(5) 1 d D U P A 2
N4B N 0.269(3) 0.129(4) 0.068(3) 0.0408(10) Uani 0.148(5) 1 d D U P A 2
H4B H 0.291799 0.090714 0.026839 0.049 Uiso 0.148(5) 1 calc R U P A 2
C22B C 0.343(3) 0.161(4) 0.109(4) 0.053(2) Uani 0.148(5) 1 d D U P A 2
H22D H 0.370373 0.116650 0.137216 0.079 Uiso 0.148(5) 1 calc R U P A 2
H22E H 0.326743 0.203112 0.147493 0.079 Uiso 0.148(5) 1 calc R U P A 2
H22F H 0.380018 0.184733 0.069415 0.079 Uiso 0.148(5) 1 calc R U P A 2
C14B C 0.161(2) 0.0083(19) 0.066(2) 0.049(6) Uani 0.148(5) 1 d D U P A 2
H14B H 0.128521 0.042023 0.027248 0.059 Uiso 0.148(5) 1 calc R U P A 2
C15B C 0.0998(17) -0.040(2) 0.1187(18) 0.057(6) Uani 0.148(5) 1 d D U P A 2
H15C H 0.060878 -0.001008 0.142884 0.068 Uiso 0.148(5) 1 calc R U P A 2
H15D H 0.068304 -0.077331 0.084094 0.068 Uiso 0.148(5) 1 calc R U P A 2
C16B C 0.140(2) -0.090(2) 0.186(2) 0.063(6) Uani 0.148(5) 1 d D U P A 2
H16C H 0.098010 -0.102969 0.226862 0.076 Uiso 0.148(5) 1 calc R U P A 2
H16D H 0.159254 -0.142224 0.163611 0.076 Uiso 0.148(5) 1 calc R U P A 2
C17B C 0.211(2) -0.050(3) 0.229(2) 0.065(7) Uani 0.148(5) 1 d D U P A 2
H17C H 0.246400 -0.093183 0.250829 0.078 Uiso 0.148(5) 1 calc R U P A 2
H17D H 0.189326 -0.018721 0.274845 0.078 Uiso 0.148(5) 1 calc R U P A 2
C18B C 0.2663(18) 0.0089(18) 0.1800(19) 0.059(6) Uani 0.148(5) 1 d D U P A 2
H18B H 0.300465 0.041766 0.217521 0.071 Uiso 0.148(5) 1 calc R U P A 2
C19B C 0.322(2) -0.042(3) 0.126(2) 0.059(7) Uani 0.148(5) 1 d D U P A 2
H19C H 0.359276 -0.004828 0.097130 0.070 Uiso 0.148(5) 1 calc R U P A 2
H19D H 0.356238 -0.077480 0.160235 0.070 Uiso 0.148(5) 1 calc R U P A 2
C20B C 0.281(2) -0.097(2) 0.063(2) 0.061(7) Uani 0.148(5) 1 d D U P A 2
H20C H 0.256692 -0.144695 0.089889 0.073 Uiso 0.148(5) 1 calc R U P A 2
H20D H 0.322743 -0.116943 0.024821 0.073 Uiso 0.148(5) 1 calc R U P A 2
C21B C 0.2143(17) -0.0491(18) 0.0171(16) 0.050(6) Uani 0.148(5) 1 d D U P A 2
H21C H 0.241198 -0.016867 -0.025401 0.060 Uiso 0.148(5) 1 calc R U P A 2
H21D H 0.178444 -0.089123 -0.009675 0.060 Uiso 0.148(5) 1 calc R U P A 2
C23 C 0.439(2) 0.561(2) 0.250000 0.119(9) Uani 0.072(4) 2 d DS TU P B 1
H23A H 0.432587 0.504432 0.230781 0.143 Uiso 0.0359(19) 1 calc R U P B 1
H23B H 0.495568 0.567413 0.269219 0.143 Uiso 0.0359(19) 1 calc R U P B 1
Cl1 Cl 0.423(3) 0.627(2) 0.1697(10) 0.122(8) Uani 0.072(4) 1 d D U P B 1
C23B C 0.3223(6) 0.6777(6) 0.250000 0.112(5) Uani 0.770(4) 2 d DS TU P C 2
H23C H 0.330905 0.736667 0.258612 0.134 Uiso 0.385(2) 1 calc R U P C 2
H23D H 0.263333 0.669095 0.241388 0.134 Uiso 0.385(2) 1 calc R U P C 2
Cl1B Cl 0.3738(3) 0.6492(2) 0.1631(3) 0.1405(17) Uani 0.770(4) 1 d D U P C 2
C24 C 0.388(4) 0.662(4) 0.220(5) 0.120(7) Uani 0.0791(19) 1 d D U P D -33
H24A H 0.436718 0.696448 0.227759 0.144 Uiso 0.0791(19) 1 calc R U P D -33
H24B H 0.386079 0.645524 0.163261 0.144 Uiso 0.0791(19) 1 calc R U P D -33
Cl2 Cl 0.301(2) 0.719(2) 0.242(4) 0.127(10) Uani 0.0791(19) 1 d D U P D -33
Cl3 Cl 0.3982(19) 0.5745(17) 0.279(2) 0.115(9) Uani 0.0791(19) 1 d D U P D -33
loop_
_atom_type_symbol
_atom_type_description
_atom_type_scat_dispersion_real
_atom_type_scat_dispersion_imag
_atom_type_scat_source
C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
B B 0.0013 0.0007 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
N N 0.0061 0.0033 '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'
Cl Cl 0.1484 0.1585 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
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
N4B Fe1 N4B 148(2) . 7
N4B Fe1 N4 3.2(17) . 7
N4B Fe1 N4 145.6(10) 7 7
N4 Fe1 N4 143.6(4) . 7
N4B Fe1 N1 106.1(11) . .
N4B Fe1 N1 106.1(11) 7 .
N4 Fe1 N1 108.2(2) . .
N4 Fe1 N1 108.2(2) 7 .
N4B Fe1 N2 96.0(18) . 7
N4B Fe1 N2 93(2) 7 7
N4 Fe1 N2 91.6(3) . 7
N4 Fe1 N2 98.9(3) 7 7
N1 Fe1 N2 73.05(9) . 7
N4B Fe1 N2 93(2) . .
N4B Fe1 N2 96.0(18) 7 .
N4 Fe1 N2 98.9(3) . .
N4 Fe1 N2 91.6(3) 7 .
N1 Fe1 N2 73.04(9) . .
N2 Fe1 N2 146.09(17) 7 .
C1 N1 C1 119.4(5) 7 .
C1 N1 Fe1 120.3(2) 7 .
C1 N1 Fe1 120.3(2) . .
C4 N2 N3 105.4(3) . .
C4 N2 Fe1 112.8(3) . .
N3 N2 Fe1 141.6(3) . .
N2 N3 C6 111.6(3) . .
N2 N3 C11B 116.7(18) . .
C6 N3 C11B 130.0(16) . .
N2 N3 C11 117.9(4) . .
C6 N3 C11 130.4(4) . .
N1 C1 C2 121.9(4) . .
N1 C1 C4 114.7(4) . .
C2 C1 C4 123.4(4) . .
C3 C2 C1 118.1(4) . .
C3 C2 H2 120.9 . .
C1 C2 H2 120.9 . .
C2 C3 C2 120.6(5) . 7
C2 C3 H3 119.7 . .
C2 C3 H3 119.7 7 .
N2 C4 C5 111.0(4) . .
N2 C4 C1 119.1(4) . .
C5 C4 C1 129.9(4) . .
C6 C5 C4 105.7(4) . .
C6 C5 H5 127.1 . .
C4 C5 H5 127.1 . .
N3 C6 C5 106.2(3) . .
N3 C6 C7 125.7(4) . .
C5 C6 C7 128.1(4) . .
C6 C7 C8 108.4(4) . .
C6 C7 C9 111.0(4) . .
C8 C7 C9 107.6(4) . .
C6 C7 C10 110.9(4) . .
C8 C7 C10 107.7(4) . .
C9 C7 C10 111.2(4) . .
C7 C8 H8A 109.5 . .
C7 C8 H8AB 109.5 . .
H8A C8 H8AB 109.5 . .
C7 C8 H8AC 109.5 . .
H8A C8 H8AC 109.5 . .
H8AB C8 H8AC 109.5 . .
C7 C9 H9A 109.5 . .
C7 C9 H9AB 109.5 . .
H9A C9 H9AB 109.5 . .
C7 C9 H9AC 109.5 . .
H9A C9 H9AC 109.5 . .
H9AB C9 H9AC 109.5 . .
C7 C10 H10A 109.5 . .
C7 C10 H10B 109.5 . .
H10A C10 H10B 109.5 . .
C7 C10 H10C 109.5 . .
H10A C10 H10C 109.5 . .
H10B C10 H10C 109.5 . .
N3 C11 C12 111.4(5) . .
N3 C11 H11A 109.4 . .
C12 C11 H11A 109.4 . .
N3 C11 H11B 109.4 . .
C12 C11 H11B 109.4 . .
H11A C11 H11B 108.0 . .
C11 C12 C13 115.3(5) . .
C11 C12 H12A 108.4 . .
C13 C12 H12A 108.4 . .
C11 C12 H12B 108.4 . .
C13 C12 H12B 108.4 . .
H12A C12 H12B 107.5 . .
C12 C13 B1 115.0(4) . .
C12 C13 H13A 108.5 . .
B1 C13 H13A 108.5 . .
C12 C13 H13B 108.5 . .
B1 C13 H13B 108.5 . .
H13A C13 H13B 107.5 . .
C13 B1 N4 106.1(5) . .
C13 B1 C14 114.1(5) . .
N4 B1 C14 108.8(6) . .
C13 B1 C18 112.6(5) . .
N4 B1 C18 111.5(5) . .
C14 B1 C18 103.8(5) . .
C22 N4 B1 113.2(8) . .
C22 N4 Fe1 101.9(5) . .
B1 N4 Fe1 124.6(6) . .
C22 N4 H4 105.2 . .
B1 N4 H4 105.2 . .
Fe1 N4 H4 105.2 . .
N4 C22 H22A 109.5 . .
N4 C22 H22B 109.5 . .
H22A C22 H22B 109.5 . .
N4 C22 H22C 109.5 . .
H22A C22 H22C 109.5 . .
H22B C22 H22C 109.5 . .
C21 C14 C15 111.1(6) . .
C21 C14 B1 113.1(6) . .
C15 C14 B1 107.7(6) . .
C21 C14 H14 108.2 . .
C15 C14 H14 108.2 . .
B1 C14 H14 108.2 . .
C16 C15 C14 114.8(5) . .
C16 C15 H15A 108.6 . .
C14 C15 H15A 108.6 . .
C16 C15 H15B 108.6 . .
C14 C15 H15B 108.6 . .
H15A C15 H15B 107.5 . .
C17 C16 C15 115.5(5) . .
C17 C16 H16A 108.4 . .
C15 C16 H16A 108.4 . .
C17 C16 H16B 108.4 . .
C15 C16 H16B 108.4 . .
H16A C16 H16B 107.5 . .
C16 C17 C18 116.6(5) . .
C16 C17 H17A 108.1 . .
C18 C17 H17A 108.1 . .
C16 C17 H17B 108.1 . .
C18 C17 H17B 108.1 . .
H17A C17 H17B 107.3 . .
C19 C18 C17 111.0(6) . .
C19 C18 B1 110.7(5) . .
C17 C18 B1 109.3(5) . .
C19 C18 H18 108.6 . .
C17 C18 H18 108.6 . .
B1 C18 H18 108.6 . .
C20 C19 C18 116.3(6) . .
C20 C19 H19A 108.2 . .
C18 C19 H19A 108.2 . .
C20 C19 H19B 108.2 . .
C18 C19 H19B 108.2 . .
H19A C19 H19B 107.4 . .
C19 C20 C21 113.6(6) . .
C19 C20 H20A 108.8 . .
C21 C20 H20A 108.8 . .
C19 C20 H20B 108.8 . .
C21 C20 H20B 108.8 . .
H20A C20 H20B 107.7 . .
C14 C21 C20 116.9(6) . .
C14 C21 H21A 108.1 . .
C20 C21 H21A 108.1 . .
C14 C21 H21B 108.1 . .
C20 C21 H21B 108.1 . .
H21A C21 H21B 107.3 . .
N3 C11B C12B 109(2) . .
N3 C11B H11C 110.0 . .
C12B C11B H11C 110.0 . .
N3 C11B H11D 110.0 . .
C12B C11B H11D 110.0 . .
H11C C11B H11D 108.3 . .
C13B C12B C11B 119(3) . .
C13B C12B H12C 107.6 . .
C11B C12B H12C 107.6 . .
C13B C12B H12D 107.6 . .
C11B C12B H12D 107.6 . .
H12C C12B H12D 107.0 . .
C12B C13B B1B 118(2) . .
C12B C13B H13C 107.9 . .
B1B C13B H13C 107.9 . .
C12B C13B H13D 107.9 . .
B1B C13B H13D 107.9 . .
H13C C13B H13D 107.2 . .
C13B B1B N4B 106(3) . .
C13B B1B C14B 116(2) . .
N4B B1B C14B 109(2) . .
C13B B1B C18B 110.6(19) . .
N4B B1B C18B 112(2) . .
C14B B1B C18B 103.6(19) . .
C22B N4B B1B 114(3) . .
C22B N4B Fe1 106(4) . .
B1B N4B Fe1 123(3) . .
C22B N4B H4B 103.6 . .
B1B N4B H4B 103.6 . .
Fe1 N4B H4B 103.6 . .
N4B C22B H22D 109.5 . .
N4B C22B H22E 109.5 . .
H22D C22B H22E 109.5 . .
N4B C22B H22F 109.5 . .
H22D C22B H22F 109.5 . .
H22E C22B H22F 109.5 . .
C21B C14B C15B 111(2) . .
C21B C14B B1B 114(2) . .
C15B C14B B1B 108(2) . .
C21B C14B H14B 107.8 . .
C15B C14B H14B 107.8 . .
B1B C14B H14B 107.8 . .
C16B C15B C14B 114(2) . .
C16B C15B H15C 108.7 . .
C14B C15B H15C 108.7 . .
C16B C15B H15D 108.7 . .
C14B C15B H15D 108.7 . .
H15C C15B H15D 107.6 . .
C17B C16B C15B 116(2) . .
C17B C16B H16C 108.3 . .
C15B C16B H16C 108.3 . .
C17B C16B H16D 108.3 . .
C15B C16B H16D 108.3 . .
H16C C16B H16D 107.4 . .
C16B C17B C18B 118(3) . .
C16B C17B H17C 107.7 . .
C18B C17B H17C 107.7 . .
C16B C17B H17D 107.7 . .
C18B C17B H17D 107.7 . .
H17C C17B H17D 107.1 . .
C19B C18B C17B 109(3) . .
C19B C18B B1B 109(2) . .
C17B C18B B1B 111(2) . .
C19B C18B H18B 109.4 . .
C17B C18B H18B 109.4 . .
B1B C18B H18B 109.4 . .
C20B C19B C18B 117(3) . .
C20B C19B H19C 107.9 . .
C18B C19B H19C 107.9 . .
C20B C19B H19D 107.9 . .
C18B C19B H19D 107.9 . .
H19C C19B H19D 107.2 . .
C19B C20B C21B 111(2) . .
C19B C20B H20C 109.5 . .
C21B C20B H20C 109.5 . .
C19B C20B H20D 109.5 . .
C21B C20B H20D 109.5 . .
H20C C20B H20D 108.1 . .
C14B C21B C20B 117(2) . .
C14B C21B H21C 108.0 . .
C20B C21B H21C 108.0 . .
C14B C21B H21D 108.0 . .
C20B C21B H21D 108.0 . .
H21C C21B H21D 107.2 . .
Cl1 C23 Cl1 114.1(18) 8_665 .
Cl1 C23 H23A 108.7 8_665 .
Cl1 C23 H23A 108.7 . .
Cl1 C23 H23B 108.7 8_665 .
Cl1 C23 H23B 108.7 . .
H23A C23 H23B 107.6 . .
Cl1B C23B Cl1B 115.6(8) 8_665 .
Cl1B C23B H23C 108.4 8_665 .
Cl1B C23B H23C 108.4 . .
Cl1B C23B H23D 108.4 8_665 .
Cl1B C23B H23D 108.4 . .
H23C C23B H23D 107.4 . .
Cl2 C24 Cl3 113.9(16) . .
Cl2 C24 H24A 108.8 . .
Cl3 C24 H24A 108.8 . .
Cl2 C24 H24B 108.8 . .
Cl3 C24 H24B 108.8 . .
H24A C24 H24B 107.7 . .
C24 Cl2 H23C 93(3) . 8_665
C24 Cl2 H23D 73(5) . 8_665
H23C Cl2 H23D 146.3 8_665 8_665
C24 Cl3 H23A 96(3) . 8_665
C24 Cl3 H23B 111(3) . 8_665
H23A Cl3 H23B 61.4 8_665 8_665
loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
Fe1 N4B 2.06(5) .
Fe1 N4B 2.06(5) 7
Fe1 N4 2.111(9) .
Fe1 N4 2.111(9) 7
Fe1 N1 2.168(5) .
Fe1 N2 2.327(4) 7
Fe1 N2 2.327(3) .
N1 C1 1.345(4) 7
N1 C1 1.345(4) .
N2 C4 1.334(5) .
N2 N3 1.360(5) .
N3 C6 1.367(5) .
N3 C11B 1.47(2) .
N3 C11 1.480(7) .
C1 C2 1.398(6) .
C1 C4 1.468(6) .
C2 C3 1.381(5) .
C2 H2 0.9500 .
C3 H3 0.9500 .
C4 C5 1.401(6) .
C5 C6 1.381(6) .
C5 H5 0.9500 .
C6 C7 1.520(6) .
C7 C8 1.528(7) .
C7 C9 1.533(7) .
C7 C10 1.540(7) .
C8 H8A 0.9800 .
C8 H8AB 0.9800 .
C8 H8AC 0.9800 .
C9 H9A 0.9800 .
C9 H9AB 0.9800 .
C9 H9AC 0.9800 .
C10 H10A 0.9800 .
C10 H10B 0.9800 .
C10 H10C 0.9800 .
C11 C12 1.527(8) .
C11 H11A 0.9900 .
C11 H11B 0.9900 .
C12 C13 1.539(7) .
C12 H12A 0.9900 .
C12 H12B 0.9900 .
C13 B1 1.627(8) .
C13 H13A 0.9900 .
C13 H13B 0.9900 .
B1 N4 1.641(11) .
B1 C14 1.641(9) .
B1 C18 1.653(9) .
N4 C22 1.489(8) .
N4 H4 1.0000 .
C22 H22A 0.9800 .
C22 H22B 0.9800 .
C22 H22C 0.9800 .
C14 C21 1.530(11) .
C14 C15 1.557(9) .
C14 H14 1.0000 .
C15 C16 1.535(8) .
C15 H15A 0.9900 .
C15 H15B 0.9900 .
C16 C17 1.530(9) .
C16 H16A 0.9900 .
C16 H16B 0.9900 .
C17 C18 1.549(9) .
C17 H17A 0.9900 .
C17 H17B 0.9900 .
C18 C19 1.541(9) .
C18 H18 1.0000 .
C19 C20 1.523(12) .
C19 H19A 0.9900 .
C19 H19B 0.9900 .
C20 C21 1.547(10) .
C20 H20A 0.9900 .
C20 H20B 0.9900 .
C21 H21A 0.9900 .
C21 H21B 0.9900 .
C11B C12B 1.52(2) .
C11B H11C 0.9900 .
C11B H11D 0.9900 .
C12B C13B 1.52(2) .
C12B H12C 0.9900 .
C12B H12D 0.9900 .
C13B B1B 1.63(2) .
C13B H13C 0.9900 .
C13B H13D 0.9900 .
B1B N4B 1.64(3) .
B1B C14B 1.64(2) .
B1B C18B 1.65(2) .
N4B C22B 1.49(3) .
N4B H4B 1.0000 .
C22B H22D 0.9800 .
C22B H22E 0.9800 .
C22B H22F 0.9800 .
C14B C21B 1.52(3) .
C14B C15B 1.56(3) .
C14B H14B 1.0000 .
C15B C16B 1.55(2) .
C15B H15C 0.9900 .
C15B H15D 0.9900 .
C16B C17B 1.52(3) .
C16B H16C 0.9900 .
C16B H16D 0.9900 .
C17B C18B 1.55(3) .
C17B H17C 0.9900 .
C17B H17D 0.9900 .
C18B C19B 1.54(2) .
C18B H18B 1.0000 .
C19B C20B 1.53(3) .
C19B H19C 0.9900 .
C19B H19D 0.9900 .
C20B C21B 1.56(3) .
C20B H20C 0.9900 .
C20B H20D 0.9900 .
C21B H21C 0.9900 .
C21B H21D 0.9900 .
C23 Cl1 1.747(16) 8_665
C23 Cl1 1.747(16) .
C23 H23A 0.9900 .
C23 H23B 0.9900 .
C23B Cl1B 1.744(8) 8_665
C23B Cl1B 1.744(8) .
C23B H23C 0.9900 .
C23B H23D 0.9900 .
C24 Cl2 1.746(16) .
C24 Cl3 1.747(16) .
C24 H24A 0.9900 .
C24 H24B 0.9900 .
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_4
C4 N2 N3 C6 0.2(5) . .
Fe1 N2 N3 C6 -174.9(3) . .
C4 N2 N3 C11B 167(2) . .
Fe1 N2 N3 C11B -8(2) . .
C4 N2 N3 C11 -177.6(5) . .
Fe1 N2 N3 C11 7.4(7) . .
C1 N1 C1 C2 -0.6(3) 7 .
Fe1 N1 C1 C2 179.4(3) . .
C1 N1 C1 C4 179.8(4) 7 .
Fe1 N1 C1 C4 -0.2(4) . .
N1 C1 C2 C3 1.2(6) . .
C4 C1 C2 C3 -179.2(3) . .
C1 C2 C3 C2 -0.5(3) . 7
N3 N2 C4 C5 0.2(5) . .
Fe1 N2 C4 C5 176.9(3) . .
N3 N2 C4 C1 -179.5(4) . .
Fe1 N2 C4 C1 -2.8(5) . .
N1 C1 C4 N2 2.2(6) . .
C2 C1 C4 N2 -177.5(4) . .
N1 C1 C4 C5 -177.5(4) . .
C2 C1 C4 C5 2.9(7) . .
N2 C4 C5 C6 -0.5(5) . .
C1 C4 C5 C6 179.2(4) . .
N2 N3 C6 C5 -0.5(5) . .
C11B N3 C6 C5 -165(3) . .
C11 N3 C6 C5 176.9(5) . .
N2 N3 C6 C7 -178.9(4) . .
C11B N3 C6 C7 17(3) . .
C11 N3 C6 C7 -1.5(8) . .
C4 C5 C6 N3 0.6(5) . .
C4 C5 C6 C7 178.9(4) . .
N3 C6 C7 C8 174.1(4) . .
C5 C6 C7 C8 -3.9(6) . .
N3 C6 C7 C9 -68.0(6) . .
C5 C6 C7 C9 114.0(5) . .
N3 C6 C7 C10 56.2(6) . .
C5 C6 C7 C10 -121.9(5) . .
N2 N3 C11 C12 -34.2(7) . .
C6 N3 C11 C12 148.5(5) . .
N3 C11 C12 C13 -56.0(6) . .
C11 C12 C13 B1 154.1(5) . .
C12 C13 B1 N4 -74.9(6) . .
C12 C13 B1 C14 44.9(6) . .
C12 C13 B1 C18 162.9(5) . .
C13 B1 N4 C22 -80.8(7) . .
C14 B1 N4 C22 156.0(7) . .
C18 B1 N4 C22 42.1(9) . .
C13 B1 N4 Fe1 43.9(8) . .
C14 B1 N4 Fe1 -79.3(8) . .
C18 B1 N4 Fe1 166.8(6) . .
C13 B1 C14 C21 179.9(5) . .
N4 B1 C14 C21 -61.8(7) . .
C18 B1 C14 C21 57.0(6) . .
C13 B1 C14 C15 56.7(6) . .
N4 B1 C14 C15 174.9(5) . .
C18 B1 C14 C15 -66.3(6) . .
C21 C14 C15 C16 -67.2(7) . .
B1 C14 C15 C16 57.3(7) . .
C14 C15 C16 C17 -41.7(8) . .
C15 C16 C17 C18 38.5(9) . .
C16 C17 C18 C19 71.7(8) . .
C16 C17 C18 B1 -50.7(8) . .
C13 B1 C18 C19 176.7(5) . .
N4 B1 C18 C19 57.6(8) . .
C14 B1 C18 C19 -59.4(7) . .
C13 B1 C18 C17 -60.8(7) . .
N4 B1 C18 C17 -179.9(6) . .
C14 B1 C18 C17 63.1(7) . .
C17 C18 C19 C20 -65.6(8) . .
B1 C18 C19 C20 55.9(8) . .
C18 C19 C20 C21 -42.9(9) . .
C15 C14 C21 C20 71.8(8) . .
B1 C14 C21 C20 -49.6(8) . .
C19 C20 C21 C14 39.3(9) . .
N2 N3 C11B C12B 37(4) . .
C6 N3 C11B C12B -159.2(18) . .
N3 C11B C12B C13B 57(4) . .
C11B C12B C13B B1B -149(3) . .
C12B C13B B1B N4B 69(3) . .
C12B C13B B1B C14B -52(3) . .
C12B C13B B1B C18B -169(2) . .
C13B B1B N4B C22B 80(6) . .
C14B B1B N4B C22B -154(5) . .
C18B B1B N4B C22B -40(6) . .
C13B B1B N4B Fe1 -51(4) . .
C14B B1B N4B Fe1 74(5) . .
C18B B1B N4B Fe1 -172(3) . .
C13B B1B C14B C21B -179(2) . .
N4B B1B C14B C21B 62(4) . .
C18B B1B C14B C21B -57(3) . .
C13B B1B C14B C15B -55(3) . .
N4B B1B C14B C15B -174(3) . .
C18B B1B C14B C15B 67(3) . .
C21B C14B C15B C16B 67(3) . .
B1B C14B C15B C16B -59(3) . .
C14B C15B C16B C17B 39(5) . .
C15B C16B C17B C18B -32(5) . .
C16B C17B C18B C19B -76(4) . .
C16B C17B C18B B1B 44(5) . .
C13B B1B C18B C19B -175(3) . .
N4B B1B C18B C19B -57(4) . .
C14B B1B C18B C19B 60(3) . .
C13B B1B C18B C17B 66(3) . .
N4B B1B C18B C17B -177(3) . .
C14B B1B C18B C17B -59(3) . .
C17B C18B C19B C20B 61(4) . .
B1B C18B C19B C20B -60(4) . .
C18B C19B C20B C21B 47(5) . .
C15B C14B C21B C20B -73(3) . .
B1B C14B C21B C20B 50(4) . .
C19B C20B C21B C14B -40(4) . .
