# Electronic Supplementary Material (ESI) for Dalton Transactions.
# This journal is © The Royal Society of Chemistry 2016

####################################################################### 
# 
# 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_1
_database_code_depnum_ccdc_archive 'CCDC 1419277'
_audit_update_record             
;
2016-09-02 deposited with the CCDC.
2016-09-26 downloaded from the CCDC.
;

_audit_creation_method           SHELXL-2014/7
_shelx_SHELXL_version_number     2014/7
_chemical_name_systematic        ?
_chemical_name_common            ?
_chemical_melting_point          ?
_chemical_formula_moiety         '(C15 H16 B Fe N9), (C19 H18 P), 0.5(C2 H3 N)'
_chemical_formula_sum            'C35 H35.50 B Fe N9.50 P'
_chemical_formula_weight         686.86

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'
P P 0.1023 0.0942 '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'

_space_group_crystal_system      monoclinic
_space_group_IT_number           15
_space_group_name_H-M_alt        'C 2/c'
_space_group_name_Hall           '-C 2yc'

_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.
;

loop_
_space_group_symop_operation_xyz
'x, y, z'
'-x, y, -z+1/2'
'x+1/2, y+1/2, z'
'-x+1/2, y+1/2, -z+1/2'
'-x, -y, -z'
'x, -y, z-1/2'
'-x+1/2, -y+1/2, -z'
'x+1/2, -y+1/2, z-1/2'

_cell_length_a                   40.799(9)
_cell_length_b                   8.793(2)
_cell_length_c                   23.324(5)
_cell_angle_alpha                90
_cell_angle_beta                 124.87
_cell_angle_gamma                90
_cell_volume                     6865(3)
_cell_formula_units_Z            8
_cell_measurement_temperature    100(2)
_cell_measurement_reflns_used    9805
_cell_measurement_theta_min      2.39
_cell_measurement_theta_max      32.22

_exptl_crystal_description       Block
_exptl_crystal_colour            Red
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    ?
_exptl_crystal_density_diffrn    1.329
_exptl_crystal_F_000             2864
_exptl_transmission_factor_min   ?
_exptl_transmission_factor_max   ?
_exptl_crystal_size_max          0.200
_exptl_crystal_size_mid          0.200
_exptl_crystal_size_min          0.100
_exptl_absorpt_coefficient_mu    0.526
_shelx_estimated_absorpt_T_min   0.902
_shelx_estimated_absorpt_T_max   0.949
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_correction_T_min  0.9020
_exptl_absorpt_correction_T_max  0.9492
_exptl_absorpt_process_details   SADABS
_exptl_absorpt_special_details   ?
_diffrn_ambient_temperature      100(2)
_diffrn_radiation_wavelength     0.71073
_diffrn_radiation_type           MoK\a
_diffrn_radiation_source         'fine-focus sealed tube'
_diffrn_radiation_monochromator  graphite
_diffrn_measurement_device_type  'Bruker APEX-II CCD'
_diffrn_measurement_method       'φ and ω scans'
_diffrn_detector_area_resol_mean ?
_diffrn_reflns_number            26708
_diffrn_reflns_av_unetI/netI     0.0218
_diffrn_reflns_av_R_equivalents  0.0259
_diffrn_reflns_limit_h_min       -49
_diffrn_reflns_limit_h_max       49
_diffrn_reflns_limit_k_min       -10
_diffrn_reflns_limit_k_max       10
_diffrn_reflns_limit_l_min       -28
_diffrn_reflns_limit_l_max       28
_diffrn_reflns_theta_min         2.128
_diffrn_reflns_theta_max         25.499
_diffrn_reflns_theta_full        25.242
_diffrn_measured_fraction_theta_max 0.998
_diffrn_measured_fraction_theta_full 0.998
_diffrn_reflns_Laue_measured_fraction_max 0.998
_diffrn_reflns_Laue_measured_fraction_full 0.998
_diffrn_reflns_point_group_measured_fraction_max 0.998
_diffrn_reflns_point_group_measured_fraction_full 0.998
_reflns_number_total             6399
_reflns_number_gt                6013
_reflns_threshold_expression     'I > 2σ(I)'
_reflns_Friedel_coverage         0.000
_reflns_Friedel_fraction_max     .
_reflns_Friedel_fraction_full    .

_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.
;

_computing_data_collection       'Bruker APEX2'
_computing_cell_refinement       'Bruker SAINT'
_computing_data_reduction        'Bruker SAINT'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_computing_structure_refinement  'SHELXL-2014/7 (Sheldrick, 2014)'
_computing_molecular_graphics    ?
_computing_publication_material  ?
_refine_special_details          ?
_refine_ls_structure_factor_coef Fsqd
_refine_ls_matrix_type           full
_refine_ls_weighting_scheme      calc
_refine_ls_weighting_details     
'w=1/[σ²(Fo²)+(0.0363P)²+8.5029P] where P=(Fo²+2Fc²)/3'
_atom_sites_solution_primary     ?
_atom_sites_solution_secondary   ?
_atom_sites_solution_hydrogens   geom
_refine_ls_hydrogen_treatment    constr
_refine_ls_extinction_method     none
_refine_ls_extinction_coef       .
_refine_ls_number_reflns         6399
_refine_ls_number_parameters     439
_refine_ls_number_restraints     1
_refine_ls_R_factor_all          0.0287
_refine_ls_R_factor_gt           0.0264
_refine_ls_wR_factor_ref         0.0713
_refine_ls_wR_factor_gt          0.0697
_refine_ls_goodness_of_fit_ref   1.018
_refine_ls_restrained_S_all      1.019
_refine_ls_shift/su_max          0.012
_refine_ls_shift/su_mean         0.000

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
B1 B 0.15525(4) 0.66737(17) 0.24673(8) 0.0133(3) Uani 1 1 d . . . . .
H1 H 0.1601 0.7766 0.2418 0.016 Uiso 1 1 calc R U . . .
C1 C 0.11855(4) 0.17353(15) 0.19028(7) 0.0147(3) Uani 1 1 d . . . . .
C2 C 0.17920(4) 0.18002(15) 0.32632(7) 0.0134(3) Uani 1 1 d . . . . .
C3 C 0.10719(4) 0.25086(15) 0.29050(7) 0.0142(3) Uani 1 1 d . . . . .
C4 C 0.19860(4) 0.33783(16) 0.21899(7) 0.0141(3) Uani 1 1 d . . . . .
H4 H 0.2024 0.2311 0.2195 0.017 Uiso 1 1 calc R U . . .
C5 C 0.21675(4) 0.44658(16) 0.20169(7) 0.0153(3) Uani 1 1 d . . . . .
C6 C 0.20243(4) 0.58429(16) 0.20798(7) 0.0149(3) Uani 1 1 d . . . . .
H6 H 0.2090 0.6816 0.1996 0.018 Uiso 1 1 calc R U . . .
C7 C 0.24574(4) 0.42173(18) 0.18225(8) 0.0210(3) Uani 1 1 d . . . . .
H7A H 0.2411 0.4980 0.1477 0.032 Uiso 1 1 calc R U . . .
H7B H 0.2418 0.3198 0.1623 0.032 Uiso 1 1 calc R U . . .
H7C H 0.2731 0.4312 0.2240 0.032 Uiso 1 1 calc R U . . .
C8 C 0.17906(4) 0.47751(16) 0.40409(7) 0.0144(3) Uani 1 1 d . . . . .
H8 H 0.1793 0.3897 0.4281 0.017 Uiso 1 1 calc R U . . .
C9 C 0.19427(4) 0.61927(16) 0.43505(7) 0.0156(3) Uani 1 1 d . . . . .
C10 C 0.18756(4) 0.71139(16) 0.38092(7) 0.0144(3) Uani 1 1 d . . . . .
H10 H 0.1946 0.8157 0.3848 0.017 Uiso 1 1 calc R U . . .
C11 C 0.21350(4) 0.65802(17) 0.51028(7) 0.0192(3) Uani 1 1 d . . . . .
H11A H 0.2227 0.7638 0.5186 0.029 Uiso 1 1 calc R U . . .
H11B H 0.2363 0.5905 0.5396 0.029 Uiso 1 1 calc R U . . .
H11C H 0.1941 0.6451 0.5219 0.029 Uiso 1 1 calc R U . . .
C12 C 0.05988(4) 0.47295(16) 0.15587(7) 0.0156(3) Uani 1 1 d . . . . .
H12 H 0.0443 0.3842 0.1465 0.019 Uiso 1 1 calc R U . . .
C13 C 0.04438(4) 0.61491(16) 0.12521(7) 0.0171(3) Uani 1 1 d . . . . .
C14 C 0.07768(4) 0.70850(16) 0.15469(7) 0.0149(3) Uani 1 1 d . . . . .
H14 H 0.0774 0.8137 0.1451 0.018 Uiso 1 1 calc R U . . .
C15 C 0.00122(4) 0.65220(18) 0.07226(9) 0.0261(3) Uani 1 1 d . . . . .
H15A H -0.0025 0.7627 0.0699 0.039 Uiso 1 1 calc R U . . .
H15B H -0.0150 0.6043 0.0859 0.039 Uiso 1 1 calc R U . . .
H15C H -0.0070 0.6140 0.0264 0.039 Uiso 1 1 calc R U . . .
C16 C 0.10551(4) 0.54184(17) 0.43230(8) 0.0198(3) Uani 1 1 d . . . . .
H16 H 0.1052 0.5518 0.3914 0.024 Uiso 1 1 calc R U . . .
C17 C 0.10887(5) 0.39896(18) 0.46048(9) 0.0265(3) Uani 1 1 d . . . . .
H17 H 0.1106 0.3110 0.4387 0.032 Uiso 1 1 calc R U . . .
C18 C 0.10969(5) 0.38474(17) 0.52064(8) 0.0256(3) Uani 1 1 d . . . . .
H18 H 0.1129 0.2873 0.5408 0.031 Uiso 1 1 calc R U . . .
C19 C 0.10587(4) 0.51263(17) 0.55144(7) 0.0205(3) Uani 1 1 d . . . . .
H19 H 0.1059 0.5019 0.5920 0.025 Uiso 1 1 calc R U . . .
C20 C 0.10196(4) 0.65576(16) 0.52325(7) 0.0160(3) Uani 1 1 d . . . . .
H20 H 0.0989 0.7427 0.5439 0.019 Uiso 1 1 calc R U . . .
C21 C 0.10256(4) 0.67152(15) 0.46408(7) 0.0141(3) Uani 1 1 d . . . . .
C22 C 0.06059(4) 0.96289(15) 0.42223(7) 0.0147(3) Uani 1 1 d . . . . .
C23 C 0.02430(4) 0.97487(18) 0.35724(8) 0.0234(3) Uani 1 1 d . . . . .
H23 H 0.0218 0.9381 0.3166 0.028 Uiso 1 1 calc R U . . .
C24 C -0.00836(5) 1.04131(19) 0.35216(8) 0.0271(3) Uani 1 1 d . . . . .
H24 H -0.0331 1.0500 0.3078 0.033 Uiso 1 1 calc R U . . .
C25 C -0.00490(4) 1.09471(17) 0.41134(8) 0.0233(3) Uani 1 1 d . . . . .
H25 H -0.0274 1.1378 0.4077 0.028 Uiso 1 1 calc R U . . .
C26 C 0.03124(4) 1.08510(17) 0.47546(8) 0.0216(3) Uani 1 1 d . . . . .
H26 H 0.0338 1.1233 0.5159 0.026 Uiso 1 1 calc R U . . .
C27 C 0.06412(4) 1.01968(16) 0.48129(7) 0.0172(3) Uani 1 1 d . . . . .
H27 H 0.0890 1.0138 0.5256 0.021 Uiso 1 1 calc R U . . .
C28 C 0.14814(4) 0.95276(15) 0.49127(7) 0.0146(3) Uani 1 1 d . . . . .
C29 C 0.16624(4) 0.94312(17) 0.56328(7) 0.0190(3) Uani 1 1 d . . . . .
H29 H 0.1536 0.8892 0.5808 0.023 Uiso 1 1 calc R U . . .
C30 C 0.20279(4) 1.01281(18) 0.60881(8) 0.0227(3) Uani 1 1 d . . . . .
H30 H 0.2150 1.0077 0.6577 0.027 Uiso 1 1 calc R U . . .
C31 C 0.22200(4) 1.09054(17) 0.58359(8) 0.0225(3) Uani 1 1 d . . . . .
H31 H 0.2472 1.1372 0.6153 0.027 Uiso 1 1 calc R U . . .
C32 C 0.20420(4) 1.09937(17) 0.51244(8) 0.0208(3) Uani 1 1 d . . . . .
H32 H 0.2173 1.1517 0.4952 0.025 Uiso 1 1 calc R U . . .
C33 C 0.16727(4) 1.03198(16) 0.46603(7) 0.0170(3) Uani 1 1 d . . . . .
H33 H 0.1549 1.0396 0.4171 0.020 Uiso 1 1 calc R U . . .
C34 C 0.09356(4) 0.84136(16) 0.34784(7) 0.0175(3) Uani 1 1 d . . . . .
H34A H 0.1165 0.7899 0.3534 0.026 Uiso 1 1 calc R U . . .
H34B H 0.0906 0.9429 0.3281 0.026 Uiso 1 1 calc R U . . .
H34C H 0.0693 0.7820 0.3164 0.026 Uiso 1 1 calc R U . . .
C36 C 0.0000 0.5292(3) 0.2500 0.0555(9) Uani 1 2 d DS T P . .
Fe1 Fe 0.14035(2) 0.32682(2) 0.26253(2) 0.01026(6) Uani 1 1 d . . . . .
N1 N 0.10614(4) 0.08439(14) 0.14629(6) 0.0210(3) Uani 1 1 d . . . . .
N2 N 0.20239(4) 0.09527(14) 0.36714(6) 0.0188(3) Uani 1 1 d . . . . .
N3 N 0.08784(4) 0.20644(14) 0.30889(6) 0.0196(3) Uani 1 1 d . . . . .
N4 N 0.17513(3) 0.40520(13) 0.23466(6) 0.0126(2) Uani 1 1 d . . . . .
N5 N 0.17766(3) 0.55791(13) 0.22804(6) 0.0132(2) Uani 1 1 d . . . . .
N6 N 0.16409(3) 0.48248(13) 0.33614(6) 0.0132(2) Uani 1 1 d . . . . .
N7 N 0.16933(3) 0.62772(13) 0.32184(6) 0.0129(2) Uani 1 1 d . . . . .
N8 N 0.09958(3) 0.47905(12) 0.20012(6) 0.0132(2) Uani 1 1 d . . . . .
N9 N 0.11047(3) 0.62511(13) 0.19925(6) 0.0126(2) Uani 1 1 d . . . . .
N10 N 0.0000 0.6551(3) 0.2500 0.0408(5) Uani 1 2 d S T P A .
P1 P 0.10124(2) 0.85828(4) 0.43103(2) 0.01236(8) Uani 1 1 d . . . . .
C35 C 0.00525(13) 0.3667(4) 0.2788(3) 0.0494(12) Uani 0.5 1 d D . P A -1
H35A H 0.0132 0.3715 0.3271 0.074 Uiso 0.5 1 calc R U P A -1
H35B H 0.0260 0.3139 0.2774 0.074 Uiso 0.5 1 calc R U P A -1
H35C H -0.0200 0.3113 0.2501 0.074 Uiso 0.5 1 calc R 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
B1 N7 1.5395(18) . ?
B1 N9 1.5457(18) . ?
B1 N5 1.5517(18) . ?
B1 H1 1.0000 . ?
C1 N1 1.1531(19) . ?
C1 Fe1 1.9322(14) . ?
C2 N2 1.1519(19) . ?
C2 Fe1 1.9224(14) . ?
C3 N3 1.1605(19) . ?
C3 Fe1 1.9266(14) . ?
C4 N4 1.3422(18) . ?
C4 C5 1.4026(19) . ?
C4 H4 0.9500 . ?
C5 C6 1.388(2) . ?
C5 C7 1.5051(19) . ?
C6 N5 1.3544(17) . ?
C6 H6 0.9500 . ?
C7 H7A 0.9800 . ?
C7 H7B 0.9800 . ?
C7 H7C 0.9800 . ?
C8 N6 1.3343(18) . ?
C8 C9 1.396(2) . ?
C8 H8 0.9500 . ?
C9 C10 1.389(2) . ?
C9 C11 1.4954(19) . ?
C10 N7 1.3495(18) . ?
C10 H10 0.9500 . ?
C11 H11A 0.9800 . ?
C11 H11B 0.9800 . ?
C11 H11C 0.9800 . ?
C12 N8 1.3344(18) . ?
C12 C13 1.397(2) . ?
C12 H12 0.9500 . ?
C13 C14 1.389(2) . ?
C13 C15 1.4989(19) . ?
C14 N9 1.3483(18) . ?
C14 H14 0.9500 . ?
C15 H15A 0.9800 . ?
C15 H15B 0.9800 . ?
C15 H15C 0.9800 . ?
C16 C17 1.388(2) . ?
C16 C21 1.402(2) . ?
C16 H16 0.9500 . ?
C17 C18 1.390(2) . ?
C17 H17 0.9500 . ?
C18 C19 1.390(2) . ?
C18 H18 0.9500 . ?
C19 C20 1.386(2) . ?
C19 H19 0.9500 . ?
C20 C21 1.401(2) . ?
C20 H20 0.9500 . ?
C21 P1 1.8018(14) . ?
C22 C23 1.391(2) . ?
C22 C27 1.393(2) . ?
C22 P1 1.8028(14) . ?
C23 C24 1.396(2) . ?
C23 H23 0.9500 . ?
C24 C25 1.387(2) . ?
C24 H24 0.9500 . ?
C25 C26 1.377(2) . ?
C25 H25 0.9500 . ?
C26 C27 1.393(2) . ?
C26 H26 0.9500 . ?
C27 H27 0.9500 . ?
C28 C29 1.3983(19) . ?
C28 C33 1.4021(19) . ?
C28 P1 1.8033(14) . ?
C29 C30 1.384(2) . ?
C29 H29 0.9500 . ?
C30 C31 1.398(2) . ?
C30 H30 0.9500 . ?
C31 C32 1.382(2) . ?
C31 H31 0.9500 . ?
C32 C33 1.389(2) . ?
C32 H32 0.9500 . ?
C33 H33 0.9500 . ?
C34 P1 1.7859(14) . ?
C34 H34A 0.9800 . ?
C34 H34B 0.9800 . ?
C34 H34C 0.9800 . ?
C36 N10 1.107(3) . ?
C36 C35 1.540(4) . ?
Fe1 N6 1.9641(12) . ?
Fe1 N8 1.9772(12) . ?
Fe1 N4 1.9911(12) . ?
N4 N5 1.3622(16) . ?
N6 N7 1.3671(16) . ?
N8 N9 1.3629(16) . ?
C35 H35A 0.9800 . ?
C35 H35B 0.9800 . ?
C35 H35C 0.9800 . ?

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
N7 B1 N9 106.27(11) . . ?
N7 B1 N5 106.42(11) . . ?
N9 B1 N5 107.12(11) . . ?
N7 B1 H1 112.2 . . ?
N9 B1 H1 112.2 . . ?
N5 B1 H1 112.2 . . ?
N1 C1 Fe1 177.77(13) . . ?
N2 C2 Fe1 176.57(12) . . ?
N3 C3 Fe1 178.42(13) . . ?
N4 C4 C5 110.71(12) . . ?
N4 C4 H4 124.6 . . ?
C5 C4 H4 124.6 . . ?
C6 C5 C4 103.94(12) . . ?
C6 C5 C7 127.53(13) . . ?
C4 C5 C7 128.52(13) . . ?
N5 C6 C5 109.23(12) . . ?
N5 C6 H6 125.4 . . ?
C5 C6 H6 125.4 . . ?
C5 C7 H7A 109.5 . . ?
C5 C7 H7B 109.5 . . ?
H7A C7 H7B 109.5 . . ?
C5 C7 H7C 109.5 . . ?
H7A C7 H7C 109.5 . . ?
H7B C7 H7C 109.5 . . ?
N6 C8 C9 110.58(12) . . ?
N6 C8 H8 124.7 . . ?
C9 C8 H8 124.7 . . ?
C10 C9 C8 104.60(12) . . ?
C10 C9 C11 129.21(13) . . ?
C8 C9 C11 126.19(13) . . ?
N7 C10 C9 108.50(12) . . ?
N7 C10 H10 125.7 . . ?
C9 C10 H10 125.7 . . ?
C9 C11 H11A 109.5 . . ?
C9 C11 H11B 109.5 . . ?
H11A C11 H11B 109.5 . . ?
C9 C11 H11C 109.5 . . ?
H11A C11 H11C 109.5 . . ?
H11B C11 H11C 109.5 . . ?
N8 C12 C13 110.73(12) . . ?
N8 C12 H12 124.6 . . ?
C13 C12 H12 124.6 . . ?
C14 C13 C12 104.34(12) . . ?
C14 C13 C15 129.37(13) . . ?
C12 C13 C15 126.29(13) . . ?
N9 C14 C13 108.55(12) . . ?
N9 C14 H14 125.7 . . ?
C13 C14 H14 125.7 . . ?
C13 C15 H15A 109.5 . . ?
C13 C15 H15B 109.5 . . ?
H15A C15 H15B 109.5 . . ?
C13 C15 H15C 109.5 . . ?
H15A C15 H15C 109.5 . . ?
H15B C15 H15C 109.5 . . ?
C17 C16 C21 120.07(13) . . ?
C17 C16 H16 120.0 . . ?
C21 C16 H16 120.0 . . ?
C16 C17 C18 119.89(14) . . ?
C16 C17 H17 120.1 . . ?
C18 C17 H17 120.1 . . ?
C19 C18 C17 120.24(14) . . ?
C19 C18 H18 119.9 . . ?
C17 C18 H18 119.9 . . ?
C20 C19 C18 120.38(14) . . ?
C20 C19 H19 119.8 . . ?
C18 C19 H19 119.8 . . ?
C19 C20 C21 119.66(13) . . ?
C19 C20 H20 120.2 . . ?
C21 C20 H20 120.2 . . ?
C20 C21 C16 119.69(13) . . ?
C20 C21 P1 119.90(10) . . ?
C16 C21 P1 120.38(11) . . ?
C23 C22 C27 119.64(13) . . ?
C23 C22 P1 119.96(11) . . ?
C27 C22 P1 120.13(10) . . ?
C22 C23 C24 119.58(14) . . ?
C22 C23 H23 120.2 . . ?
C24 C23 H23 120.2 . . ?
C25 C24 C23 120.53(14) . . ?
C25 C24 H24 119.7 . . ?
C23 C24 H24 119.7 . . ?
C26 C25 C24 119.77(14) . . ?
C26 C25 H25 120.1 . . ?
C24 C25 H25 120.1 . . ?
C25 C26 C27 120.33(14) . . ?
C25 C26 H26 119.8 . . ?
C27 C26 H26 119.8 . . ?
C26 C27 C22 120.13(13) . . ?
C26 C27 H27 119.9 . . ?
C22 C27 H27 119.9 . . ?
C29 C28 C33 119.73(13) . . ?
C29 C28 P1 120.30(10) . . ?
C33 C28 P1 119.94(10) . . ?
C30 C29 C28 119.48(13) . . ?
C30 C29 H29 120.3 . . ?
C28 C29 H29 120.3 . . ?
C29 C30 C31 120.72(14) . . ?
C29 C30 H30 119.6 . . ?
C31 C30 H30 119.6 . . ?
C32 C31 C30 119.79(13) . . ?
C32 C31 H31 120.1 . . ?
C30 C31 H31 120.1 . . ?
C31 C32 C33 120.20(13) . . ?
C31 C32 H32 119.9 . . ?
C33 C32 H32 119.9 . . ?
C32 C33 C28 120.07(13) . . ?
C32 C33 H33 120.0 . . ?
C28 C33 H33 120.0 . . ?
P1 C34 H34A 109.5 . . ?
P1 C34 H34B 109.5 . . ?
H34A C34 H34B 109.5 . . ?
P1 C34 H34C 109.5 . . ?
H34A C34 H34C 109.5 . . ?
H34B C34 H34C 109.5 . . ?
N10 C36 C35 158.03(18) . . ?
C2 Fe1 C3 86.16(6) . . ?
C2 Fe1 C1 88.36(6) . . ?
C3 Fe1 C1 89.49(6) . . ?
C2 Fe1 N6 90.86(5) . . ?
C3 Fe1 N6 92.09(5) . . ?
C1 Fe1 N6 178.19(5) . . ?
C2 Fe1 N8 177.15(5) . . ?
C3 Fe1 N8 91.48(5) . . ?
C1 Fe1 N8 93.21(5) . . ?
N6 Fe1 N8 87.63(5) . . ?
C2 Fe1 N4 93.38(5) . . ?
C3 Fe1 N4 179.39(5) . . ?
C1 Fe1 N4 90.89(5) . . ?
N6 Fe1 N4 87.52(5) . . ?
N8 Fe1 N4 88.97(5) . . ?
C4 N4 N5 106.99(11) . . ?
C4 N4 Fe1 133.51(9) . . ?
N5 N4 Fe1 119.50(8) . . ?
C6 N5 N4 109.14(11) . . ?
C6 N5 B1 131.80(12) . . ?
N4 N5 B1 118.99(11) . . ?
C8 N6 N7 106.92(11) . . ?
C8 N6 Fe1 132.66(9) . . ?
N7 N6 Fe1 120.37(8) . . ?
C10 N7 N6 109.39(11) . . ?
C10 N7 B1 131.89(12) . . ?
N6 N7 B1 118.71(11) . . ?
C12 N8 N9 106.76(11) . . ?
C12 N8 Fe1 132.89(9) . . ?
N9 N8 Fe1 120.31(8) . . ?
C14 N9 N8 109.62(11) . . ?
C14 N9 B1 131.84(11) . . ?
N8 N9 B1 118.54(11) . . ?
C34 P1 C21 109.43(7) . . ?
C34 P1 C22 109.89(7) . . ?
C21 P1 C22 108.31(6) . . ?
C34 P1 C28 109.51(7) . . ?
C21 P1 C28 109.13(6) . . ?
C22 P1 C28 110.55(7) . . ?
C36 C35 H35A 109.5 . . ?
C36 C35 H35B 109.5 . . ?
H35A C35 H35B 109.5 . . ?
C36 C35 H35C 109.5 . . ?
H35A C35 H35C 109.5 . . ?
H35B C35 H35C 109.5 . . ?

loop_
_geom_torsion_atom_site_label_1
_geom_torsion_atom_site_label_2
_geom_torsion_atom_site_label_3
_geom_torsion_atom_site_label_4
_geom_torsion
_geom_torsion_site_symmetry_1
_geom_torsion_site_symmetry_2
_geom_torsion_site_symmetry_3
_geom_torsion_site_symmetry_4
_geom_torsion_publ_flag
N4 C4 C5 C6 -0.10(15) . . . . ?
N4 C4 C5 C7 178.72(13) . . . . ?
C4 C5 C6 N5 0.31(14) . . . . ?
C7 C5 C6 N5 -178.53(13) . . . . ?
N6 C8 C9 C10 -0.12(15) . . . . ?
N6 C8 C9 C11 -179.85(12) . . . . ?
C8 C9 C10 N7 0.22(15) . . . . ?
C11 C9 C10 N7 179.94(13) . . . . ?
N8 C12 C13 C14 -0.55(16) . . . . ?
N8 C12 C13 C15 179.16(14) . . . . ?
C12 C13 C14 N9 0.50(15) . . . . ?
C15 C13 C14 N9 -179.20(14) . . . . ?
C21 C16 C17 C18 -0.6(2) . . . . ?
C16 C17 C18 C19 2.1(2) . . . . ?
C17 C18 C19 C20 -1.2(2) . . . . ?
C18 C19 C20 C21 -1.1(2) . . . . ?
C19 C20 C21 C16 2.5(2) . . . . ?
C19 C20 C21 P1 -175.38(11) . . . . ?
C17 C16 C21 C20 -1.7(2) . . . . ?
C17 C16 C21 P1 176.22(12) . . . . ?
C27 C22 C23 C24 -1.1(2) . . . . ?
P1 C22 C23 C24 172.91(12) . . . . ?
C22 C23 C24 C25 -0.3(2) . . . . ?
C23 C24 C25 C26 1.4(2) . . . . ?
C24 C25 C26 C27 -1.1(2) . . . . ?
C25 C26 C27 C22 -0.3(2) . . . . ?
C23 C22 C27 C26 1.4(2) . . . . ?
P1 C22 C27 C26 -172.63(11) . . . . ?
C33 C28 C29 C30 0.4(2) . . . . ?
P1 C28 C29 C30 178.19(12) . . . . ?
C28 C29 C30 C31 -1.0(2) . . . . ?
C29 C30 C31 C32 0.6(2) . . . . ?
C30 C31 C32 C33 0.3(2) . . . . ?
C31 C32 C33 C28 -0.9(2) . . . . ?
C29 C28 C33 C32 0.6(2) . . . . ?
P1 C28 C33 C32 -177.25(11) . . . . ?
C5 C4 N4 N5 -0.14(15) . . . . ?
C5 C4 N4 Fe1 179.36(9) . . . . ?
C5 C6 N5 N4 -0.40(15) . . . . ?
C5 C6 N5 B1 176.24(12) . . . . ?
C4 N4 N5 C6 0.33(14) . . . . ?
Fe1 N4 N5 C6 -179.25(8) . . . . ?
C4 N4 N5 B1 -176.81(11) . . . . ?
Fe1 N4 N5 B1 3.61(15) . . . . ?
N7 B1 N5 C6 -121.78(14) . . . . ?
N9 B1 N5 C6 124.86(14) . . . . ?
N7 B1 N5 N4 54.59(14) . . . . ?
N9 B1 N5 N4 -58.77(14) . . . . ?
C9 C8 N6 N7 -0.02(14) . . . . ?
C9 C8 N6 Fe1 177.16(9) . . . . ?
C9 C10 N7 N6 -0.24(14) . . . . ?
C9 C10 N7 B1 -179.13(13) . . . . ?
C8 N6 N7 C10 0.17(14) . . . . ?
Fe1 N6 N7 C10 -177.44(9) . . . . ?
C8 N6 N7 B1 179.22(11) . . . . ?
Fe1 N6 N7 B1 1.61(15) . . . . ?
N9 B1 N7 C10 -125.13(14) . . . . ?
N5 B1 N7 C10 120.93(14) . . . . ?
N9 B1 N7 N6 56.07(14) . . . . ?
N5 B1 N7 N6 -57.87(14) . . . . ?
C13 C12 N8 N9 0.39(15) . . . . ?
C13 C12 N8 Fe1 177.97(10) . . . . ?
C13 C14 N9 N8 -0.29(15) . . . . ?
C13 C14 N9 B1 -179.50(13) . . . . ?
C12 N8 N9 C14 -0.06(14) . . . . ?
Fe1 N8 N9 C14 -178.01(9) . . . . ?
C12 N8 N9 B1 179.27(11) . . . . ?
Fe1 N8 N9 B1 1.32(15) . . . . ?
N7 B1 N9 C14 121.51(14) . . . . ?
N5 B1 N9 C14 -125.03(14) . . . . ?
N7 B1 N9 N8 -57.63(14) . . . . ?
N5 B1 N9 N8 55.83(14) . . . . ?
C20 C21 P1 C34 -169.96(11) . . . . ?
C16 C21 P1 C34 12.15(13) . . . . ?
C20 C21 P1 C22 -50.18(13) . . . . ?
C16 C21 P1 C22 131.93(11) . . . . ?
C20 C21 P1 C28 70.23(12) . . . . ?
C16 C21 P1 C28 -107.66(12) . . . . ?
C23 C22 P1 C34 20.31(14) . . . . ?
C27 C22 P1 C34 -165.68(11) . . . . ?
C23 C22 P1 C21 -99.18(13) . . . . ?
C27 C22 P1 C21 74.83(12) . . . . ?
C23 C22 P1 C28 141.30(12) . . . . ?
C27 C22 P1 C28 -44.69(13) . . . . ?
C29 C28 P1 C34 -162.35(11) . . . . ?
C33 C28 P1 C34 15.47(13) . . . . ?
C29 C28 P1 C21 -42.60(13) . . . . ?
C33 C28 P1 C21 135.23(11) . . . . ?
C29 C28 P1 C22 76.43(13) . . . . ?
C33 C28 P1 C22 -105.75(12) . . . . ?

_refine_diff_density_max         0.336
_refine_diff_density_min         -0.428
_refine_diff_density_rms         0.054

####################################################################### 
# 
# 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_2_H2O-100K
_database_code_depnum_ccdc_archive 'CCDC 1419278'
_audit_update_record             
;
2016-09-02 deposited with the CCDC.
2016-09-26 downloaded from the CCDC.
;

_audit_creation_method           SHELXL-2014/7
_shelx_SHELXL_version_number     2014/7
_chemical_name_systematic        ?
_chemical_name_common            ?
_chemical_melting_point          ?
_chemical_formula_moiety         '(C66 H68 B2 Fe4 N26), 2(Cl O4), (H2 O)'
_chemical_formula_sum            'C66 H70 B2 Cl2 Fe4 N26 O9'
_chemical_formula_weight         1687.40

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'
O O 0.0106 0.0060 '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'

_space_group_crystal_system      monoclinic
_space_group_IT_number           14
_space_group_name_H-M_alt        'P 21/n'
_space_group_name_Hall           '-P 2yn'

_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.
;

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                   12.9230(12)
_cell_length_b                   17.8110(17)
_cell_length_c                   16.1986(15)
_cell_angle_alpha                90
_cell_angle_beta                 98.6780(10)
_cell_angle_gamma                90
_cell_volume                     3685.8(6)
_cell_formula_units_Z            2
_cell_measurement_temperature    100(2)
_cell_measurement_reflns_used    9944
_cell_measurement_theta_min      2.20
_cell_measurement_theta_max      31.50

_exptl_crystal_description       Block
_exptl_crystal_colour            Red
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    ?
_exptl_crystal_density_diffrn    1.520
_exptl_crystal_F_000             1736
_exptl_transmission_factor_min   ?
_exptl_transmission_factor_max   ?
_exptl_crystal_size_max          0.120
_exptl_crystal_size_mid          0.100
_exptl_crystal_size_min          0.100
_exptl_absorpt_coefficient_mu    0.919
_shelx_estimated_absorpt_T_min   0.898
_shelx_estimated_absorpt_T_max   0.914
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_correction_T_min  0.8977
_exptl_absorpt_correction_T_max  0.9137
_exptl_absorpt_process_details   sadabs
_exptl_absorpt_special_details   ?
_diffrn_ambient_temperature      100(2)
_diffrn_radiation_wavelength     0.71073
_diffrn_radiation_type           MoK\a
_diffrn_radiation_source         'fine-focus sealed tube'
_diffrn_radiation_monochromator  graphite
_diffrn_measurement_device_type  'Bruker APEX-II CCD'
_diffrn_measurement_method       'φ and ω scans'
_diffrn_detector_area_resol_mean ?
_diffrn_reflns_number            35021
_diffrn_reflns_av_unetI/netI     0.0403
_diffrn_reflns_av_R_equivalents  0.0380
_diffrn_reflns_limit_h_min       -15
_diffrn_reflns_limit_h_max       17
_diffrn_reflns_limit_k_min       -22
_diffrn_reflns_limit_k_max       24
_diffrn_reflns_limit_l_min       -22
_diffrn_reflns_limit_l_max       22
_diffrn_reflns_theta_min         1.710
_diffrn_reflns_theta_max         28.998
_diffrn_reflns_theta_full        25.242
_diffrn_measured_fraction_theta_max 0.994
_diffrn_measured_fraction_theta_full 0.993
_diffrn_reflns_Laue_measured_fraction_max 0.994
_diffrn_reflns_Laue_measured_fraction_full 0.993
_diffrn_reflns_point_group_measured_fraction_max 0.994
_diffrn_reflns_point_group_measured_fraction_full 0.993
_reflns_number_total             9734
_reflns_number_gt                7384
_reflns_threshold_expression     'I > 2σ(I)'
_reflns_Friedel_coverage         0.000
_reflns_Friedel_fraction_max     .
_reflns_Friedel_fraction_full    .

_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.
;

_computing_data_collection       'Bruker APEX2'
_computing_cell_refinement       'Bruker SAINT'
_computing_data_reduction        'Bruker SAINT'
_computing_structure_refinement  'SHELXL-2014/7 (Sheldrick, 2014)'
_computing_molecular_graphics    ?
_computing_publication_material  ?
_refine_special_details          ?
_refine_ls_structure_factor_coef Fsqd
_refine_ls_matrix_type           full
_refine_ls_weighting_scheme      calc
_refine_ls_weighting_details     
'w=1/[σ²(Fo²)+(0.0396P)²+3.4208P] where P=(Fo²+2Fc²)/3'
_atom_sites_solution_primary     ?
_atom_sites_solution_secondary   ?
_atom_sites_solution_hydrogens   mixed
_refine_ls_hydrogen_treatment    constr
_refine_ls_extinction_method     none
_refine_ls_extinction_coef       .
_refine_ls_number_reflns         9734
_refine_ls_number_parameters     545
_refine_ls_number_restraints     0
_refine_ls_R_factor_all          0.0595
_refine_ls_R_factor_gt           0.0368
_refine_ls_wR_factor_ref         0.0990
_refine_ls_wR_factor_gt          0.0858
_refine_ls_goodness_of_fit_ref   1.047
_refine_ls_restrained_S_all      1.047
_refine_ls_shift/su_max          0.000
_refine_ls_shift/su_mean         0.000

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 -0.18127(2) 0.07529(2) 0.08479(2) 0.01319(7) Uani 1 1 d . . . . .
Fe2 Fe 0.14256(2) 0.18531(2) 0.00957(2) 0.01420(7) Uani 1 1 d . . . . .
B1 B -0.1812(2) 0.07614(13) 0.27601(14) 0.0184(4) Uani 1 1 d . . . . .
H1 H -0.1822 0.0771 0.3376 0.022 Uiso 1 1 d R U . . .
N1 N -0.17844(14) -0.08082(10) 0.00511(10) 0.0164(3) Uani 1 1 d . . . . .
N2 N 0.00293(14) 0.14920(10) 0.01799(10) 0.0162(3) Uani 1 1 d . . . . .
N3 N -0.32289(16) 0.14622(12) -0.06422(12) 0.0287(4) Uani 1 1 d . . . . .
N4 N -0.07755(13) 0.02708(10) 0.17159(10) 0.0160(3) Uani 1 1 d . . . . .
N5 N -0.09049(14) 0.02909(10) 0.25333(10) 0.0178(3) Uani 1 1 d . . . . .
N6 N -0.29613(14) 0.04024(10) 0.14225(10) 0.0166(3) Uani 1 1 d . . . . .
N7 N -0.28489(14) 0.04565(10) 0.22727(10) 0.0175(3) Uani 1 1 d . . . . .
N8 N -0.17930(14) 0.16535(10) 0.15596(10) 0.0163(3) Uani 1 1 d . . . . .
N9 N -0.16943(14) 0.15543(10) 0.24042(10) 0.0184(4) Uani 1 1 d . . . . .
N10 N 0.16904(14) 0.18713(10) 0.13261(10) 0.0172(3) Uani 1 1 d . . . . .
N11 N 0.10631(14) 0.29358(10) 0.02138(11) 0.0175(3) Uani 1 1 d . . . . .
N12 N 0.28439(14) 0.22285(10) 0.00550(10) 0.0171(3) Uani 1 1 d . . . . .
N13 N 0.10057(14) 0.20721(10) -0.11092(10) 0.0179(3) Uani 1 1 d . . . . .
C1 C -0.18328(16) -0.01886(12) 0.02551(12) 0.0161(4) Uani 1 1 d . . . . .
C2 C -0.06900(16) 0.11841(11) 0.03612(12) 0.0158(4) Uani 1 1 d . . . . .
C3 C -0.27197(17) 0.11965(12) -0.00715(13) 0.0194(4) Uani 1 1 d . . . . .
C4 C 0.01171(16) -0.00989(12) 0.16740(13) 0.0184(4) Uani 1 1 d . . . . .
H4 H 0.0391 -0.0197 0.1172 0.022 Uiso 1 1 calc R U . . .
C5 C 0.05897(17) -0.03193(13) 0.24677(13) 0.0219(4) Uani 1 1 d . . . . .
C6 C -0.00821(18) -0.00579(12) 0.29927(13) 0.0219(4) Uani 1 1 d . . . . .
H6 H 0.0019 -0.0114 0.3583 0.026 Uiso 1 1 calc R U . . .
C7 C 0.15838(19) -0.07610(15) 0.26804(16) 0.0319(5) Uani 1 1 d . . . . .
H7A H 0.2076 -0.0481 0.3087 0.048 Uiso 1 1 calc R U . . .
H7B H 0.1896 -0.0844 0.2173 0.048 Uiso 1 1 calc R U . . .
H7C H 0.1428 -0.1246 0.2920 0.048 Uiso 1 1 calc R U . . .
C8 C -0.39732(17) 0.02524(12) 0.11557(14) 0.0203(4) Uani 1 1 d . . . . .
H8 H -0.4270 0.0184 0.0587 0.024 Uiso 1 1 calc R U . . .
C9 C -0.45316(17) 0.02103(12) 0.18286(15) 0.0234(5) Uani 1 1 d . . . . .
C10 C -0.37864(18) 0.03475(12) 0.25183(14) 0.0213(4) Uani 1 1 d . . . . .
H10 H -0.3916 0.0362 0.3080 0.026 Uiso 1 1 calc R U . . .
C11 C -0.5668(2) 0.00325(17) 0.18093(19) 0.0372(6) Uani 1 1 d . . . . .
H11A H -0.5794 -0.0495 0.1656 0.056 Uiso 1 1 calc R U . . .
H11B H -0.6089 0.0354 0.1397 0.056 Uiso 1 1 calc R U . . .
H11C H -0.5863 0.0123 0.2362 0.056 Uiso 1 1 calc R U . . .
C12 C -0.17215(18) 0.23890(12) 0.14241(13) 0.0208(4) Uani 1 1 d . . . . .
H12 H -0.1781 0.2616 0.0888 0.025 Uiso 1 1 calc R U . . .
C13 C -0.1546(2) 0.27783(12) 0.21810(15) 0.0253(5) Uani 1 1 d . . . . .
C14 C -0.15411(19) 0.22248(12) 0.27809(14) 0.0235(5) Uani 1 1 d . . . . .
H14 H -0.1444 0.2307 0.3367 0.028 Uiso 1 1 calc R U . . .
C15 C -0.1381(3) 0.36030(14) 0.23309(18) 0.0393(7) Uani 1 1 d . . . . .
H15A H -0.1190 0.3695 0.2931 0.059 Uiso 1 1 calc R U . . .
H15B H -0.2029 0.3874 0.2123 0.059 Uiso 1 1 calc R U . . .
H15C H -0.0818 0.3780 0.2037 0.059 Uiso 1 1 calc R U . . .
C16 C 0.21283(18) 0.13315(13) 0.18456(13) 0.0214(4) Uani 1 1 d . . . . .
H16 H 0.2346 0.0878 0.1614 0.026 Uiso 1 1 calc R U . . .
C17 C 0.2274(2) 0.14119(14) 0.27074(14) 0.0280(5) Uani 1 1 d . . . . .
H17 H 0.2577 0.1017 0.3058 0.034 Uiso 1 1 calc R U . . .
C18 C 0.1974(2) 0.20719(15) 0.30485(14) 0.0302(5) Uani 1 1 d . . . . .
H18 H 0.2082 0.2143 0.3637 0.036 Uiso 1 1 calc R U . . .
C19 C 0.1513(2) 0.26301(14) 0.25214(14) 0.0267(5) Uani 1 1 d . . . . .
H19 H 0.1300 0.3089 0.2742 0.032 Uiso 1 1 calc R U . . .
C20 C 0.13685(17) 0.25082(12) 0.16659(13) 0.0206(4) Uani 1 1 d . . . . .
C21 C 0.07563(19) 0.30374(12) 0.10546(13) 0.0226(4) Uani 1 1 d . . . . .
H21A H -0.0002 0.2938 0.1027 0.027 Uiso 1 1 calc R U . . .
H21B H 0.0894 0.3562 0.1243 0.027 Uiso 1 1 calc R U . . .
C22 C 0.19788(18) 0.34239(12) 0.01047(15) 0.0236(5) Uani 1 1 d . . . . .
H22A H 0.1819 0.3702 -0.0429 0.028 Uiso 1 1 calc R U . . .
H22B H 0.2090 0.3797 0.0563 0.028 Uiso 1 1 calc R U . . .
C23 C 0.29592(17) 0.29807(12) 0.01035(12) 0.0189(4) Uani 1 1 d . . . . .
C24 C 0.39235(18) 0.33324(13) 0.01125(13) 0.0234(5) Uani 1 1 d . . . . .
H24 H 0.3984 0.3862 0.0165 0.028 Uiso 1 1 calc R U . . .
C25 C 0.47932(19) 0.28959(15) 0.00433(15) 0.0293(5) Uani 1 1 d . . . . .
H25 H 0.5459 0.3122 0.0040 0.035 Uiso 1 1 calc R U . . .
C26 C 0.46750(19) 0.21230(15) -0.00209(15) 0.0285(5) Uani 1 1 d . . . . .
H26 H 0.5259 0.1812 -0.0074 0.034 Uiso 1 1 calc R U . . .
C27 C 0.37016(17) 0.18095(13) -0.00070(13) 0.0226(4) Uani 1 1 d . . . . .
H27 H 0.3631 0.1279 -0.0042 0.027 Uiso 1 1 calc R U . . .
C28 C 0.01764(17) 0.30861(12) -0.04705(13) 0.0219(4) Uani 1 1 d . . . . .
H28A H 0.0092 0.3633 -0.0565 0.026 Uiso 1 1 calc R U . . .
H28B H -0.0484 0.2884 -0.0319 0.026 Uiso 1 1 calc R U . . .
C29 C 0.04233(18) 0.27089(12) -0.12451(14) 0.0214(4) Uani 1 1 d . . . . .
C30 C 0.0081(2) 0.29764(14) -0.20436(15) 0.0309(5) Uani 1 1 d . . . . .
H30 H -0.0321 0.3425 -0.2124 0.037 Uiso 1 1 calc R U . . .
C31 C 0.0332(2) 0.25808(15) -0.27216(15) 0.0366(6) Uani 1 1 d . . . . .
H31 H 0.0106 0.2755 -0.3274 0.044 Uiso 1 1 calc R U . . .
C32 C 0.0914(2) 0.19322(15) -0.25871(14) 0.0314(5) Uani 1 1 d . . . . .
H32 H 0.1089 0.1651 -0.3045 0.038 Uiso 1 1 calc R U . . .
C33 C 0.12402(19) 0.16958(13) -0.17745(13) 0.0230(5) Uani 1 1 d . . . . .
H33 H 0.1646 0.1250 -0.1685 0.028 Uiso 1 1 calc R U . . .
Cl1 Cl 0.74062(9) 0.43510(6) 0.01840(7) 0.0198(2) Uani 0.5 1 d . . P A 1
O1 O 0.6866(10) 0.4816(6) -0.0477(7) 0.044(2) Uani 0.5 1 d . . P A 1
O2 O 0.6813(3) 0.4245(2) 0.0837(2) 0.0395(9) Uani 0.5 1 d . . P A 1
O3 O 0.8337(14) 0.4732(10) 0.0546(11) 0.069(4) Uani 0.5 1 d . . P A 1
O4 O 0.7747(17) 0.3602(12) -0.0132(14) 0.036(2) Uani 0.5 1 d . . P A 1
Cl1' Cl 0.78424(16) 0.45003(9) -0.01385(10) 0.0499(4) Uani 0.5 1 d . . P B 2
O1' O 0.8469(4) 0.4727(3) -0.0804(3) 0.0610(13) Uani 0.5 1 d . . P B 2
O2' O 0.774(2) 0.3748(12) -0.0096(16) 0.055(5) Uani 0.5 1 d . . P B 2
O3' O 0.8402(10) 0.4820(8) 0.0554(8) 0.035(2) Uani 0.5 1 d . . P B 2
O4' O 0.6836(13) 0.4782(8) -0.0356(10) 0.087(5) Uani 0.5 1 d . . P B 2
O1W O 0.9396(3) 0.5040(2) -0.1004(2) 0.0419(9) Uani 0.5 1 d . . P C 1
H1WA H 0.9060 0.4934 -0.0628 0.063 Uiso 0.5 1 d R U P C 1
H1WB H 1.0001 0.5134 -0.0790 0.063 Uiso 0.5 1 d R U P C 1


_geom_special_details            
;
 All esds (except the esd in the dihedral angle between two l.s. planes)
 are estimated using the full covariance matrix.  The cell esds are taken
 into account individually in the estimation of esds in distances, angles
 and torsion angles; correlations between esds in cell parameters are only
 used when they are defined by crystal symmetry.  An approximate (isotropic)
 treatment of cell esds is used for estimating esds involving l.s. planes.
;

loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
_geom_bond_publ_flag
Fe1 C2 1.914(2) . ?
Fe1 C3 1.921(2) . ?
Fe1 C1 1.931(2) . ?
Fe1 N6 1.9687(18) . ?
Fe1 N8 1.9733(17) . ?
Fe1 N4 1.9855(17) . ?
Fe2 N2 1.9397(18) . ?
Fe2 N1 1.9414(18) 3 ?
Fe2 N12 1.9615(18) . ?
Fe2 N10 1.9709(17) . ?
Fe2 N13 1.9841(17) . ?
Fe2 N11 2.0003(18) . ?
B1 N5 1.530(3) . ?
B1 N9 1.542(3) . ?
B1 N7 1.548(3) . ?
B1 H1 1.0000 . ?
N1 C1 1.156(3) . ?
N1 Fe2 1.9413(18) 3 ?
N2 C2 1.155(3) . ?
N3 C3 1.152(3) . ?
N4 C4 1.339(3) . ?
N4 N5 1.360(2) . ?
N5 C6 1.353(3) . ?
N6 C8 1.341(3) . ?
N6 N7 1.366(2) . ?
N7 C10 1.345(3) . ?
N8 C12 1.334(3) . ?
N8 N9 1.366(2) . ?
N9 C14 1.342(3) . ?
N10 C16 1.345(3) . ?
N10 C20 1.353(3) . ?
N11 C21 1.486(3) . ?
N11 C28 1.493(3) . ?
N11 C22 1.500(3) . ?
N12 C23 1.349(3) . ?
N12 C27 1.353(3) . ?
N13 C33 1.342(3) . ?
N13 C29 1.361(3) . ?
C4 C5 1.394(3) . ?
C4 H4 0.9500 . ?
C5 C6 1.384(3) . ?
C5 C7 1.501(3) . ?
C6 H6 0.9500 . ?
C7 H7A 0.9800 . ?
C7 H7B 0.9800 . ?
C7 H7C 0.9800 . ?
C8 C9 1.397(3) . ?
C8 H8 0.9500 . ?
C9 C10 1.382(3) . ?
C9 C11 1.498(3) . ?
C10 H10 0.9500 . ?
C11 H11A 0.9800 . ?
C11 H11B 0.9800 . ?
C11 H11C 0.9800 . ?
C12 C13 1.397(3) . ?
C12 H12 0.9500 . ?
C13 C14 1.383(3) . ?
C13 C15 1.499(3) . ?
C14 H14 0.9500 . ?
C15 H15A 0.9800 . ?
C15 H15B 0.9800 . ?
C15 H15C 0.9800 . ?
C16 C17 1.388(3) . ?
C16 H16 0.9500 . ?
C17 C18 1.379(4) . ?
C17 H17 0.9500 . ?
C18 C19 1.385(4) . ?
C18 H18 0.9500 . ?
C19 C20 1.387(3) . ?
C19 H19 0.9500 . ?
C20 C21 1.503(3) . ?
C21 H21A 0.9900 . ?
C21 H21B 0.9900 . ?
C22 C23 1.493(3) . ?
C22 H22A 0.9900 . ?
C22 H22B 0.9900 . ?
C23 C24 1.393(3) . ?
C24 C25 1.385(4) . ?
C24 H24 0.9500 . ?
C25 C26 1.387(4) . ?
C25 H25 0.9500 . ?
C26 C27 1.380(3) . ?
C26 H26 0.9500 . ?
C27 H27 0.9500 . ?
C28 C29 1.499(3) . ?
C28 H28A 0.9900 . ?
C28 H28B 0.9900 . ?
C29 C30 1.387(3) . ?
C30 C31 1.384(4) . ?
C30 H30 0.9500 . ?
C31 C32 1.378(4) . ?
C31 H31 0.9500 . ?
C32 C33 1.386(3) . ?
C32 H32 0.9500 . ?
C33 H33 0.9500 . ?
Cl1 O2 1.409(4) . ?
Cl1 O3 1.428(19) . ?
Cl1 O1 1.448(10) . ?
Cl1 O4 1.52(2) . ?
Cl1' O2' 1.35(2) . ?
Cl1' O3' 1.364(15) . ?
Cl1' O4' 1.389(15) . ?
Cl1' O1' 1.498(5) . ?
O1W H1WA 0.8227 . ?
O1W H1WB 0.8231 . ?

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
C2 Fe1 C3 85.83(9) . . ?
C2 Fe1 C1 95.61(8) . . ?
C3 Fe1 C1 90.62(9) . . ?
C2 Fe1 N6 174.06(8) . . ?
C3 Fe1 N6 94.68(8) . . ?
C1 Fe1 N6 90.30(8) . . ?
C2 Fe1 N8 88.32(8) . . ?
C3 Fe1 N8 94.08(8) . . ?
C1 Fe1 N8 174.09(8) . . ?
N6 Fe1 N8 85.74(7) . . ?
C2 Fe1 N4 89.57(8) . . ?
C3 Fe1 N4 174.13(8) . . ?
C1 Fe1 N4 86.19(8) . . ?
N6 Fe1 N4 90.27(7) . . ?
N8 Fe1 N4 89.43(7) . . ?
N2 Fe2 N1 86.14(7) . 3 ?
N2 Fe2 N12 177.86(7) . . ?
N1 Fe2 N12 94.64(7) 3 . ?
N2 Fe2 N10 87.47(7) . . ?
N1 Fe2 N10 97.55(7) 3 . ?
N12 Fe2 N10 90.45(7) . . ?
N2 Fe2 N13 90.86(7) . . ?
N1 Fe2 N13 95.90(7) 3 . ?
N12 Fe2 N13 91.04(7) . . ?
N10 Fe2 N13 166.30(8) . . ?
N2 Fe2 N11 94.55(7) . . ?
N1 Fe2 N11 178.37(7) 3 . ?
N12 Fe2 N11 84.73(7) . . ?
N10 Fe2 N11 83.97(7) . . ?
N13 Fe2 N11 82.61(7) . . ?
N5 B1 N9 106.84(17) . . ?
N5 B1 N7 108.73(17) . . ?
N9 B1 N7 104.91(17) . . ?
N5 B1 H1 112.0 . . ?
N9 B1 H1 112.0 . . ?
N7 B1 H1 112.0 . . ?
C1 N1 Fe2 166.94(17) . 3 ?
C2 N2 Fe2 165.56(17) . . ?
C4 N4 N5 107.21(16) . . ?
C4 N4 Fe1 132.18(14) . . ?
N5 N4 Fe1 120.60(13) . . ?
C6 N5 N4 108.75(17) . . ?
C6 N5 B1 133.33(18) . . ?
N4 N5 B1 117.35(16) . . ?
C8 N6 N7 106.81(17) . . ?
C8 N6 Fe1 132.77(14) . . ?
N7 N6 Fe1 118.76(13) . . ?
C10 N7 N6 108.93(17) . . ?
C10 N7 B1 130.48(18) . . ?
N6 N7 B1 119.42(16) . . ?
C12 N8 N9 107.06(16) . . ?
C12 N8 Fe1 134.22(14) . . ?
N9 N8 Fe1 118.10(13) . . ?
C14 N9 N8 108.99(17) . . ?
C14 N9 B1 131.39(17) . . ?
N8 N9 B1 119.56(16) . . ?
C16 N10 C20 118.08(18) . . ?
C16 N10 Fe2 127.84(15) . . ?
C20 N10 Fe2 114.07(14) . . ?
C21 N11 C28 112.18(17) . . ?
C21 N11 C22 111.21(17) . . ?
C28 N11 C22 109.83(17) . . ?
C21 N11 Fe2 107.68(13) . . ?
C28 N11 Fe2 105.45(13) . . ?
C22 N11 Fe2 110.31(13) . . ?
C23 N12 C27 117.89(19) . . ?
C23 N12 Fe2 115.61(15) . . ?
C27 N12 Fe2 126.50(15) . . ?
C33 N13 C29 118.22(19) . . ?
C33 N13 Fe2 129.09(16) . . ?
C29 N13 Fe2 112.67(14) . . ?
N1 C1 Fe1 166.86(17) . . ?
N2 C2 Fe1 170.02(17) . . ?
N3 C3 Fe1 177.1(2) . . ?
N4 C4 C5 110.65(19) . . ?
N4 C4 H4 124.7 . . ?
C5 C4 H4 124.7 . . ?
C6 C5 C4 104.11(19) . . ?
C6 C5 C7 129.0(2) . . ?
C4 C5 C7 126.9(2) . . ?
N5 C6 C5 109.27(18) . . ?
N5 C6 H6 125.4 . . ?
C5 C6 H6 125.4 . . ?
C5 C7 H7A 109.5 . . ?
C5 C7 H7B 109.5 . . ?
H7A C7 H7B 109.5 . . ?
C5 C7 H7C 109.5 . . ?
H7A C7 H7C 109.5 . . ?
H7B C7 H7C 109.5 . . ?
N6 C8 C9 110.66(19) . . ?
N6 C8 H8 124.7 . . ?
C9 C8 H8 124.7 . . ?
C10 C9 C8 104.01(19) . . ?
C10 C9 C11 128.0(2) . . ?
C8 C9 C11 128.0(2) . . ?
N7 C10 C9 109.59(19) . . ?
N7 C10 H10 125.2 . . ?
C9 C10 H10 125.2 . . ?
C9 C11 H11A 109.5 . . ?
C9 C11 H11B 109.5 . . ?
H11A C11 H11B 109.5 . . ?
C9 C11 H11C 109.5 . . ?
H11A C11 H11C 109.5 . . ?
H11B C11 H11C 109.5 . . ?
N8 C12 C13 110.43(19) . . ?
N8 C12 H12 124.8 . . ?
C13 C12 H12 124.8 . . ?
C14 C13 C12 104.23(19) . . ?
C14 C13 C15 126.8(2) . . ?
C12 C13 C15 129.0(2) . . ?
N9 C14 C13 109.26(19) . . ?
N9 C14 H14 125.4 . . ?
C13 C14 H14 125.4 . . ?
C13 C15 H15A 109.5 . . ?
C13 C15 H15B 109.5 . . ?
H15A C15 H15B 109.5 . . ?
C13 C15 H15C 109.5 . . ?
H15A C15 H15C 109.5 . . ?
H15B C15 H15C 109.5 . . ?
N10 C16 C17 122.4(2) . . ?
N10 C16 H16 118.8 . . ?
C17 C16 H16 118.8 . . ?
C18 C17 C16 119.2(2) . . ?
C18 C17 H17 120.4 . . ?
C16 C17 H17 120.4 . . ?
C17 C18 C19 119.0(2) . . ?
C17 C18 H18 120.5 . . ?
C19 C18 H18 120.5 . . ?
C18 C19 C20 119.0(2) . . ?
C18 C19 H19 120.5 . . ?
C20 C19 H19 120.5 . . ?
N10 C20 C19 122.3(2) . . ?
N10 C20 C21 114.91(18) . . ?
C19 C20 C21 122.6(2) . . ?
N11 C21 C20 109.92(17) . . ?
N11 C21 H21A 109.7 . . ?
C20 C21 H21A 109.7 . . ?
N11 C21 H21B 109.7 . . ?
C20 C21 H21B 109.7 . . ?
H21A C21 H21B 108.2 . . ?
C23 C22 N11 112.23(18) . . ?
C23 C22 H22A 109.2 . . ?
N11 C22 H22A 109.2 . . ?
C23 C22 H22B 109.2 . . ?
N11 C22 H22B 109.2 . . ?
H22A C22 H22B 107.9 . . ?
N12 C23 C24 122.6(2) . . ?
N12 C23 C22 116.03(19) . . ?
C24 C23 C22 121.4(2) . . ?
C25 C24 C23 118.8(2) . . ?
C25 C24 H24 120.6 . . ?
C23 C24 H24 120.6 . . ?
C24 C25 C26 118.8(2) . . ?
C24 C25 H25 120.6 . . ?
C26 C25 H25 120.6 . . ?
C27 C26 C25 119.4(2) . . ?
C27 C26 H26 120.3 . . ?
C25 C26 H26 120.3 . . ?
N12 C27 C26 122.5(2) . . ?
N12 C27 H27 118.7 . . ?
C26 C27 H27 118.7 . . ?
N11 C28 C29 107.72(17) . . ?
N11 C28 H28A 110.2 . . ?
C29 C28 H28A 110.2 . . ?
N11 C28 H28B 110.2 . . ?
C29 C28 H28B 110.2 . . ?
H28A C28 H28B 108.5 . . ?
N13 C29 C30 121.9(2) . . ?
N13 C29 C28 114.87(18) . . ?
C30 C29 C28 123.2(2) . . ?
C31 C30 C29 119.0(2) . . ?
C31 C30 H30 120.5 . . ?
C29 C30 H30 120.5 . . ?
C32 C31 C30 119.3(2) . . ?
C32 C31 H31 120.4 . . ?
C30 C31 H31 120.4 . . ?
C31 C32 C33 119.1(2) . . ?
C31 C32 H32 120.5 . . ?
C33 C32 H32 120.5 . . ?
N13 C33 C32 122.5(2) . . ?
N13 C33 H33 118.7 . . ?
C32 C33 H33 118.7 . . ?
O2 Cl1 O3 106.0(7) . . ?
O2 Cl1 O1 112.1(7) . . ?
O3 Cl1 O1 108.3(8) . . ?
O2 Cl1 O4 110.7(7) . . ?
O3 Cl1 O4 106.7(11) . . ?
O1 Cl1 O4 112.7(10) . . ?
O2' Cl1' O3' 114.7(13) . . ?
O2' Cl1' O4' 106.1(13) . . ?
O3' Cl1' O4' 114.6(8) . . ?
O2' Cl1' O1' 111.8(10) . . ?
O3' Cl1' O1' 101.6(6) . . ?
O4' Cl1' O1' 107.9(8) . . ?
H1WA O1W H1WB 107.9 . . ?

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
C4 N4 N5 C6 0.9(2) . . . . ?
Fe1 N4 N5 C6 -178.38(14) . . . . ?
C4 N4 N5 B1 173.35(18) . . . . ?
Fe1 N4 N5 B1 -5.9(2) . . . . ?
N9 B1 N5 C6 116.8(2) . . . . ?
N7 B1 N5 C6 -130.5(2) . . . . ?
N9 B1 N5 N4 -53.4(2) . . . . ?
N7 B1 N5 N4 59.3(2) . . . . ?
C8 N6 N7 C10 -0.6(2) . . . . ?
Fe1 N6 N7 C10 166.55(14) . . . . ?
C8 N6 N7 B1 -169.46(18) . . . . ?
Fe1 N6 N7 B1 -2.3(2) . . . . ?
N5 B1 N7 C10 138.6(2) . . . . ?
N9 B1 N7 C10 -107.4(2) . . . . ?
N5 B1 N7 N6 -55.3(2) . . . . ?
N9 B1 N7 N6 58.7(2) . . . . ?
C12 N8 N9 C14 -1.3(2) . . . . ?
Fe1 N8 N9 C14 170.93(15) . . . . ?
C12 N8 N9 B1 176.26(19) . . . . ?
Fe1 N8 N9 B1 -11.5(2) . . . . ?
N5 B1 N9 C14 -118.2(2) . . . . ?
N7 B1 N9 C14 126.5(2) . . . . ?
N5 B1 N9 N8 64.9(2) . . . . ?
N7 B1 N9 N8 -50.5(2) . . . . ?
Fe2 N1 C1 Fe1 -37.9(14) 3 . . . ?
N5 N4 C4 C5 -0.6(2) . . . . ?
Fe1 N4 C4 C5 178.51(15) . . . . ?
N4 C4 C5 C6 0.1(2) . . . . ?
N4 C4 C5 C7 178.4(2) . . . . ?
N4 N5 C6 C5 -0.8(2) . . . . ?
B1 N5 C6 C5 -171.6(2) . . . . ?
C4 C5 C6 N5 0.4(2) . . . . ?
C7 C5 C6 N5 -177.8(2) . . . . ?
N7 N6 C8 C9 0.3(2) . . . . ?
Fe1 N6 C8 C9 -164.33(15) . . . . ?
N6 C8 C9 C10 0.2(2) . . . . ?
N6 C8 C9 C11 -178.0(2) . . . . ?
N6 N7 C10 C9 0.7(2) . . . . ?
B1 N7 C10 C9 167.9(2) . . . . ?
C8 C9 C10 N7 -0.5(2) . . . . ?
C11 C9 C10 N7 177.7(2) . . . . ?
N9 N8 C12 C13 1.6(2) . . . . ?
Fe1 N8 C12 C13 -168.80(17) . . . . ?
N8 C12 C13 C14 -1.3(3) . . . . ?
N8 C12 C13 C15 177.8(3) . . . . ?
N8 N9 C14 C13 0.5(3) . . . . ?
B1 N9 C14 C13 -176.7(2) . . . . ?
C12 C13 C14 N9 0.5(3) . . . . ?
C15 C13 C14 N9 -178.7(3) . . . . ?
C20 N10 C16 C17 -1.1(3) . . . . ?
Fe2 N10 C16 C17 179.96(17) . . . . ?
N10 C16 C17 C18 -0.9(4) . . . . ?
C16 C17 C18 C19 1.4(4) . . . . ?
C17 C18 C19 C20 0.0(4) . . . . ?
C16 N10 C20 C19 2.6(3) . . . . ?
Fe2 N10 C20 C19 -178.34(18) . . . . ?
C16 N10 C20 C21 -171.9(2) . . . . ?
Fe2 N10 C20 C21 7.2(2) . . . . ?
C18 C19 C20 N10 -2.0(4) . . . . ?
C18 C19 C20 C21 172.1(2) . . . . ?
C28 N11 C21 C20 148.42(18) . . . . ?
C22 N11 C21 C20 -88.1(2) . . . . ?
Fe2 N11 C21 C20 32.8(2) . . . . ?
N10 C20 C21 N11 -27.1(3) . . . . ?
C19 C20 C21 N11 158.4(2) . . . . ?
C21 N11 C22 C23 108.4(2) . . . . ?
C28 N11 C22 C23 -126.82(19) . . . . ?
Fe2 N11 C22 C23 -11.0(2) . . . . ?
C27 N12 C23 C24 -1.6(3) . . . . ?
Fe2 N12 C23 C24 177.70(15) . . . . ?
C27 N12 C23 C22 175.45(18) . . . . ?
Fe2 N12 C23 C22 -5.2(2) . . . . ?
N11 C22 C23 N12 10.8(3) . . . . ?
N11 C22 C23 C24 -172.06(18) . . . . ?
N12 C23 C24 C25 2.0(3) . . . . ?
C22 C23 C24 C25 -174.9(2) . . . . ?
C23 C24 C25 C26 -0.9(3) . . . . ?
C24 C25 C26 C27 -0.6(3) . . . . ?
C23 N12 C27 C26 0.1(3) . . . . ?
Fe2 N12 C27 C26 -179.15(16) . . . . ?
C25 C26 C27 N12 1.0(3) . . . . ?
C21 N11 C28 C29 -159.57(17) . . . . ?
C22 N11 C28 C29 76.2(2) . . . . ?
Fe2 N11 C28 C29 -42.63(19) . . . . ?
C33 N13 C29 C30 -0.6(3) . . . . ?
Fe2 N13 C29 C30 177.74(18) . . . . ?
C33 N13 C29 C28 178.73(19) . . . . ?
Fe2 N13 C29 C28 -3.0(2) . . . . ?
N11 C28 C29 N13 30.9(2) . . . . ?
N11 C28 C29 C30 -149.8(2) . . . . ?
N13 C29 C30 C31 0.5(4) . . . . ?
C28 C29 C30 C31 -178.8(2) . . . . ?
C29 C30 C31 C32 0.1(4) . . . . ?
C30 C31 C32 C33 -0.6(4) . . . . ?
C29 N13 C33 C32 0.1(3) . . . . ?
Fe2 N13 C33 C32 -177.90(17) . . . . ?
C31 C32 C33 N13 0.5(4) . . . . ?

loop_
_geom_hbond_atom_site_label_D
_geom_hbond_atom_site_label_H
_geom_hbond_atom_site_label_A
_geom_hbond_distance_DH
_geom_hbond_distance_HA
_geom_hbond_distance_DA
_geom_hbond_angle_DHA
_geom_hbond_site_symmetry_A
C10 H10 O3 0.95 2.50 3.289(18) 140.0 2_545
C10 H10 O3' 0.95 2.41 3.227(13) 143.4 2_545
C12 H12 O4 0.95 2.43 3.31(2) 155.3 1_455
C12 H12 O2' 0.95 2.59 3.45(3) 150.9 1_455
C16 H16 N1 0.95 2.69 3.177(3) 112.6 3
C17 H17 O1' 0.95 2.42 3.346(5) 165.4 4_566
C21 H21B O1W 0.99 2.54 3.431(4) 149.6 3_665
C22 H22A O3' 0.99 2.65 3.316(13) 124.6 3_665
C26 H26 N3 0.95 2.37 3.249(3) 154.5 1_655
C27 H27 N1 0.95 2.53 3.045(3) 114.3 3
O1W H1WA Cl1 0.82 2.87 3.649(4) 159.5 .
O1W H1WA O3 0.82 2.27 3.085(18) 171.0 .
O1W H1WB O3 0.82 2.14 2.939(19) 164.6 3_765

_refine_diff_density_max         0.922
_refine_diff_density_min         -0.997
_refine_diff_density_rms         0.075

####################################################################### 
# 
# 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_2_H2O-296K
_database_code_depnum_ccdc_archive 'CCDC 1419279'
_audit_update_record             
;
2016-09-02 deposited with the CCDC.
2016-09-26 downloaded from the CCDC.
;

_audit_creation_method           SHELXL-2014/7
_shelx_SHELXL_version_number     2014/7
_chemical_name_systematic        ?
_chemical_name_common            ?
_chemical_melting_point          ?
_chemical_formula_moiety         '(C66 H68 B2 Fe4 N26), 2(Cl O4), (H2 O)'
_chemical_formula_sum            'C66 H70 B2 Cl2 Fe4 N26 O9'
_chemical_formula_weight         1687.40

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'
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'
B B 0.0013 0.0007 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Cl Cl 0.1484 0.1585 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Fe Fe 0.3463 0.8444 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'

_space_group_crystal_system      monoclinic
_space_group_IT_number           14
_space_group_name_H-M_alt        'P 21/n'
_space_group_name_Hall           '-P 2yn'

_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.
;

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                   13.065(3)
_cell_length_b                   18.047(4)
_cell_length_c                   16.373(4)
_cell_angle_alpha                90
_cell_angle_beta                 99.063(3)
_cell_angle_gamma                90
_cell_volume                     3812.2(16)
_cell_formula_units_Z            2
_cell_measurement_temperature    296(2)
_cell_measurement_reflns_used    6780
_cell_measurement_theta_min      2.17
_cell_measurement_theta_max      26.45

_exptl_crystal_description       Block
_exptl_crystal_colour            Red
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    ?
_exptl_crystal_density_diffrn    1.470
_exptl_crystal_F_000             1736
_exptl_transmission_factor_min   ?
_exptl_transmission_factor_max   ?
_exptl_crystal_size_max          0.120
_exptl_crystal_size_mid          0.100
_exptl_crystal_size_min          0.100
_exptl_absorpt_coefficient_mu    0.888
_shelx_estimated_absorpt_T_min   0.901
_shelx_estimated_absorpt_T_max   0.916
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_correction_T_min  0.9009
_exptl_absorpt_correction_T_max  0.9164
_exptl_absorpt_process_details   sadabs
_exptl_absorpt_special_details   ?
_diffrn_ambient_temperature      296(2)
_diffrn_radiation_wavelength     0.71073
_diffrn_radiation_type           MoK\a
_diffrn_radiation_source         'fine-focus sealed tube'
_diffrn_radiation_monochromator  graphite
_diffrn_measurement_device_type  'Bruker APEX-II CCD'
_diffrn_measurement_method       'φ and ω scans'
_diffrn_detector_area_resol_mean ?
_diffrn_reflns_number            26670
_diffrn_reflns_av_unetI/netI     0.0555
_diffrn_reflns_av_R_equivalents  0.0626
_diffrn_reflns_limit_h_min       -15
_diffrn_reflns_limit_h_max       15
_diffrn_reflns_limit_k_min       -21
_diffrn_reflns_limit_k_max       21
_diffrn_reflns_limit_l_min       -19
_diffrn_reflns_limit_l_max       18
_diffrn_reflns_theta_min         1.691
_diffrn_reflns_theta_max         24.999
_diffrn_reflns_theta_full        24.999
_diffrn_measured_fraction_theta_max 0.994
_diffrn_measured_fraction_theta_full 0.994
_diffrn_reflns_Laue_measured_fraction_max 0.994
_diffrn_reflns_Laue_measured_fraction_full 0.994
_diffrn_reflns_point_group_measured_fraction_max 0.994
_diffrn_reflns_point_group_measured_fraction_full 0.994
_reflns_number_total             6685
_reflns_number_gt                4662
_reflns_threshold_expression     'I > 2σ(I)'
_reflns_Friedel_coverage         0.000
_reflns_Friedel_fraction_max     .
_reflns_Friedel_fraction_full    .

_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.
;

_computing_data_collection       'Bruker APEX2'
_computing_cell_refinement       'Bruker SAINT'
_computing_data_reduction        'Bruker SAINT'
_computing_structure_solution    'SHELXS-2014 (Sheldrick, 2014)'
_computing_structure_refinement  'SHELXL-2014/7 (Sheldrick, 2014)'
_computing_molecular_graphics    ?
_computing_publication_material  ?
_refine_special_details          ?
_refine_ls_structure_factor_coef Fsqd
_refine_ls_matrix_type           full
_refine_ls_weighting_scheme      calc
_refine_ls_weighting_details     
'w=1/[σ²(Fo²)+(0.0992P)²+6.3582P] where P=(Fo²+2Fc²)/3'
_atom_sites_solution_primary     ?
_atom_sites_solution_secondary   ?
_atom_sites_solution_hydrogens   mixed
_refine_ls_hydrogen_treatment    constr
_refine_ls_extinction_method     none
_refine_ls_extinction_coef       .
_refine_ls_number_reflns         6685
_refine_ls_number_parameters     544
_refine_ls_number_restraints     54
_refine_ls_R_factor_all          0.0952
_refine_ls_R_factor_gt           0.0602
_refine_ls_wR_factor_ref         0.1980
_refine_ls_wR_factor_gt          0.1518
_refine_ls_goodness_of_fit_ref   1.074
_refine_ls_restrained_S_all      1.094
_refine_ls_shift/su_max          0.021
_refine_ls_shift/su_mean         0.000

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 0.31874(5) 1.07650(3) 0.08433(4) 0.0372(2) Uani 1 1 d . . . . .
Fe2 Fe 0.35701(5) 0.81863(3) -0.00916(4) 0.0393(2) Uani 1 1 d . . . . .
B1 B 0.3213(5) 1.0783(3) 0.2738(4) 0.0500(15) Uani 1 1 d . . . . .
H1 H 0.3214 1.0795 0.3336 0.060 Uiso 1 1 d R U . . .
N1 N 0.3201(3) 0.9228(2) 0.0039(3) 0.0487(10) Uani 1 1 d . . . . .
N2 N 0.5020(3) 1.1463(2) 0.0164(3) 0.0448(10) Uani 1 1 d . . . . .
N3 N 0.1754(4) 1.1467(3) -0.0623(3) 0.0781(16) Uani 1 1 d . . . . .
N4 N 0.4220(3) 1.0291(2) 0.1701(2) 0.0421(9) Uani 1 1 d . . . . .
N5 N 0.4108(3) 1.0319(2) 0.2509(3) 0.0481(10) Uani 1 1 d . . . . .
N6 N 0.2053(3) 1.0425(2) 0.1421(3) 0.0444(9) Uani 1 1 d . . . . .
N7 N 0.2179(3) 1.0474(2) 0.2261(3) 0.0462(10) Uani 1 1 d . . . . .
N8 N 0.3224(3) 1.1660(2) 0.1546(2) 0.0453(10) Uani 1 1 d . . . . .
N9 N 0.3311(4) 1.1565(2) 0.2377(3) 0.0504(11) Uani 1 1 d . . . . .
N10 N 0.3310(3) 0.8142(2) -0.1328(3) 0.0468(10) Uani 1 1 d . . . . .
N11 N 0.3916(3) 0.7089(2) -0.0214(3) 0.0495(10) Uani 1 1 d . . . . .
N12 N 0.2149(3) 0.7797(2) -0.0053(3) 0.0473(10) Uani 1 1 d . . . . .
N13 N 0.3994(3) 0.7942(2) 0.1111(3) 0.0522(11) Uani 1 1 d . . . . .
C1 C 0.3159(4) 0.9837(3) 0.0247(3) 0.0407(11) Uani 1 1 d . . . . .
C2 C 0.4298(4) 1.1175(2) 0.0348(3) 0.0402(11) Uani 1 1 d . . . . .
C3 C 0.2270(4) 1.1201(3) -0.0059(3) 0.0520(13) Uani 1 1 d . . . . .
C4 C 0.5095(4) 0.9915(3) 0.1657(3) 0.0480(12) Uani 1 1 d . . . . .
H4 H 0.5352 0.9815 0.1170 0.058 Uiso 1 1 calc R U . . .
C5 C 0.5565(4) 0.9695(3) 0.2437(4) 0.0583(15) Uani 1 1 d . . . . .
C6 C 0.4927(5) 0.9968(3) 0.2957(4) 0.0600(15) Uani 1 1 d . . . . .
H6 H 0.5040 0.9919 0.3530 0.072 Uiso 1 1 calc R U . . .
C7 C 0.6547(6) 0.9249(4) 0.2644(5) 0.094(2) Uani 1 1 d . . . . .
H7A H 0.6959 0.9449 0.3132 0.141 Uiso 1 1 calc R U . . .
H7B H 0.6931 0.9273 0.2191 0.141 Uiso 1 1 calc R U . . .
H7C H 0.6376 0.8743 0.2741 0.141 Uiso 1 1 calc R U . . .
C8 C 0.1059(4) 1.0256(3) 0.1169(4) 0.0528(13) Uani 1 1 d . . . . .
H8 H 0.0764 1.0183 0.0620 0.063 Uiso 1 1 calc R U . . .
C9 C 0.0521(5) 1.0204(3) 0.1834(4) 0.0605(15) Uani 1 1 d . . . . .
C10 C 0.1267(5) 1.0347(3) 0.2514(4) 0.0559(14) Uani 1 1 d . . . . .
H10 H 0.1154 1.0355 0.3060 0.067 Uiso 1 1 calc R U . . .
C11 C -0.0609(5) 1.0027(4) 0.1834(5) 0.091(2) Uani 1 1 d . . . . .
H11A H -0.0766 1.0077 0.2385 0.136 Uiso 1 1 calc R U . . .
H11B H -0.0748 0.9527 0.1646 0.136 Uiso 1 1 calc R U . . .
H11C H -0.1032 1.0363 0.1472 0.136 Uiso 1 1 calc R U . . .
C12 C 0.3280(5) 1.2387(3) 0.1411(4) 0.0548(14) Uani 1 1 d . . . . .
H12 H 0.3217 1.2604 0.0891 0.066 Uiso 1 1 calc R U . . .
C13 C 0.3445(6) 1.2772(3) 0.2147(4) 0.0681(18) Uani 1 1 d . . . . .
C14 C 0.3459(5) 1.2232(3) 0.2748(4) 0.0662(16) Uani 1 1 d . . . . .
H14 H 0.3554 1.2315 0.3316 0.079 Uiso 1 1 calc R U . . .
C15 C 0.3605(8) 1.3589(3) 0.2299(5) 0.099(3) Uani 1 1 d . . . . .
H15A H 0.4200 1.3751 0.2071 0.148 Uiso 1 1 calc R U . . .
H15B H 0.3714 1.3684 0.2884 0.148 Uiso 1 1 calc R U . . .
H15C H 0.3004 1.3855 0.2041 0.148 Uiso 1 1 calc R U . . .
C16 C 0.2876(5) 0.8669(3) -0.1845(4) 0.0588(14) Uani 1 1 d . . . . .
H16 H 0.2669 0.9110 -0.1625 0.071 Uiso 1 1 calc R U . . .
C17 C 0.2724(6) 0.8582(4) -0.2694(4) 0.081(2) Uani 1 1 d . . . . .
H17 H 0.2417 0.8957 -0.3039 0.097 Uiso 1 1 calc R U . . .
C18 C 0.3029(7) 0.7940(5) -0.3019(4) 0.088(2) Uani 1 1 d . . . . .
H18 H 0.2931 0.7872 -0.3589 0.106 Uiso 1 1 calc R U . . .
C19 C 0.3488(6) 0.7389(4) -0.2497(4) 0.0773(19) Uani 1 1 d . . . . .
H19 H 0.3699 0.6947 -0.2710 0.093 Uiso 1 1 calc R U . . .
C20 C 0.3626(4) 0.7511(3) -0.1646(4) 0.0551(14) Uani 1 1 d . . . . .
C21 C 0.4231(5) 0.6996(3) -0.1036(4) 0.0654(16) Uani 1 1 d . . . . .
H21A H 0.4111 0.6489 -0.1221 0.078 Uiso 1 1 calc R U . . .
H21B H 0.4965 0.7100 -0.0999 0.078 Uiso 1 1 calc R U . . .
C22 C 0.3000(5) 0.6622(3) -0.0121(5) 0.0689(17) Uani 1 1 d . . . . .
H22A H 0.3154 0.6339 0.0387 0.083 Uiso 1 1 calc R U . . .
H22B H 0.2879 0.6273 -0.0577 0.083 Uiso 1 1 calc R U . . .
C23 C 0.2035(4) 0.7061(3) -0.0103(3) 0.0498(12) Uani 1 1 d . . . . .
C24 C 0.1089(5) 0.6705(4) -0.0105(4) 0.0685(17) Uani 1 1 d . . . . .
H24 H 0.1035 0.6192 -0.0150 0.082 Uiso 1 1 calc R U . . .
C25 C 0.0233(5) 0.7137(5) -0.0038(5) 0.087(2) Uani 1 1 d . . . . .
H25 H -0.0413 0.6922 -0.0035 0.105 Uiso 1 1 calc R U . . .
C26 C 0.0359(6) 0.7896(5) 0.0024(5) 0.086(2) Uani 1 1 d . . . . .
H26 H -0.0206 0.8196 0.0077 0.103 Uiso 1 1 calc R U . . .
C27 C 0.1300(5) 0.8208(4) 0.0007(4) 0.0648(16) Uani 1 1 d . . . . .
H27 H 0.1363 0.8721 0.0039 0.078 Uiso 1 1 calc R U . . .
C28 C 0.4780(5) 0.6928(3) 0.0470(4) 0.0655(16) Uani 1 1 d . . . . .
H28A H 0.5428 0.7111 0.0330 0.079 Uiso 1 1 calc R U . . .
H28B H 0.4843 0.6397 0.0560 0.079 Uiso 1 1 calc R U . . .
C29 C 0.4553(5) 0.7301(3) 0.1233(4) 0.0600(15) Uani 1 1 d . . . . .
C30 C 0.4884(7) 0.7031(4) 0.2021(5) 0.092(2) Uani 1 1 d . . . . .
H30 H 0.5271 0.6596 0.2096 0.111 Uiso 1 1 calc R U . . .
C31 C 0.4635(8) 0.7411(5) 0.2694(5) 0.108(3) Uani 1 1 d . . . . .
H31 H 0.4829 0.7226 0.3226 0.130 Uiso 1 1 calc R U . . .
C32 C 0.4110(7) 0.8049(5) 0.2572(4) 0.092(2) Uani 1 1 d . . . . .
H32 H 0.3964 0.8320 0.3023 0.110 Uiso 1 1 calc R U . . .
C33 C 0.3786(5) 0.8306(3) 0.1780(4) 0.0627(15) Uani 1 1 d . . . . .
H33 H 0.3412 0.8745 0.1708 0.075 Uiso 1 1 calc R U . . .
Cl1 Cl 0.2617(5) 0.9371(2) 0.4874(3) 0.0755(11) Uani 0.5 1 d . U P A 1
O1 O 0.3183(16) 0.9260(10) 0.4271(11) 0.165(5) Uani 0.5 1 d . U P A 1
O2 O 0.201(2) 0.9892(16) 0.4416(18) 0.155(6) Uani 0.5 1 d . U P A 1
O3 O 0.2968(19) 0.9789(10) 0.5619(9) 0.156(6) Uani 0.5 1 d . U P A 1
O4 O 0.247(2) 0.8682(19) 0.508(3) 0.149(10) Uani 0.5 1 d . U P A 1
Cl1' Cl 0.2108(7) 0.9503(4) 0.5120(4) 0.118(2) Uani 0.5 1 d . U P B 2
O1' O 0.321(2) 0.9754(16) 0.5103(16) 0.190(6) Uani 0.5 1 d . U P B 2
O2' O 0.1439(15) 0.9761(16) 0.4485(14) 0.140(7) Uani 0.5 1 d . U P B 2
O3' O 0.163(2) 0.9737(11) 0.5811(11) 0.182(6) Uani 0.5 1 d . U P B 2
O4' O 0.197(2) 0.8776(14) 0.510(3) 0.127(8) Uani 0.5 1 d . U P B 2
O1W O 0.0561(19) 1.0033(11) 0.6030(13) 0.198(8) Uani 0.5 1 d . . P C 1
H1WA H 0.0861 1.0002 0.5607 0.238 Uiso 0.5 1 d R U P C 1
H1WB H -0.0091 1.0041 0.5870 0.238 Uiso 0.5 1 d R U P C 1


_geom_special_details            
;
 All esds (except the esd in the dihedral angle between two l.s. planes)
 are estimated using the full covariance matrix.  The cell esds are taken
 into account individually in the estimation of esds in distances, angles
 and torsion angles; correlations between esds in cell parameters are only
 used when they are defined by crystal symmetry.  An approximate (isotropic)
 treatment of cell esds is used for estimating esds involving l.s. planes.
;

loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
_geom_bond_publ_flag
Fe1 C3 1.919(5) . ?
Fe1 C2 1.918(5) . ?
Fe1 C1 1.936(5) . ?
Fe1 N6 1.977(4) . ?
Fe1 N8 1.979(4) . ?
Fe1 N4 1.981(4) . ?
Fe2 N1 1.961(4) . ?
Fe2 N2 1.969(4) 3_675 ?
Fe2 N12 1.995(4) . ?
Fe2 N10 2.000(4) . ?
Fe2 N13 2.008(4) . ?
Fe2 N11 2.048(4) . ?
B1 N5 1.532(8) . ?
B1 N9 1.544(7) . ?
B1 N7 1.553(8) . ?
B1 H1 0.9800 . ?
N1 C1 1.154(6) . ?
N2 C2 1.158(6) . ?
N2 Fe2 1.969(4) 3_675 ?
N3 C3 1.158(7) . ?
N4 C4 1.342(6) . ?
N4 N5 1.355(6) . ?
N5 C6 1.356(7) . ?
N6 C8 1.335(7) . ?
N6 N7 1.362(6) . ?
N7 C10 1.341(7) . ?
N8 C12 1.334(6) . ?
N8 N9 1.357(6) . ?
N9 C14 1.348(7) . ?
N10 C16 1.340(7) . ?
N10 C20 1.344(6) . ?
N11 C21 1.478(7) . ?
N11 C28 1.488(7) . ?
N11 C22 1.491(7) . ?
N12 C23 1.339(7) . ?
N12 C27 1.350(7) . ?
N13 C33 1.341(7) . ?
N13 C29 1.366(7) . ?
C4 C5 1.385(7) . ?
C4 H4 0.9300 . ?
C5 C6 1.373(9) . ?
C5 C7 1.507(8) . ?
C6 H6 0.9300 . ?
C7 H7A 0.9600 . ?
C7 H7B 0.9600 . ?
C7 H7C 0.9600 . ?
C8 C9 1.389(8) . ?
C8 H8 0.9300 . ?
C9 C10 1.383(9) . ?
C9 C11 1.511(9) . ?
C10 H10 0.9300 . ?
C11 H11A 0.9600 . ?
C11 H11B 0.9600 . ?
C11 H11C 0.9600 . ?
C12 C13 1.379(8) . ?
C12 H12 0.9300 . ?
C13 C14 1.383(9) . ?
C13 C15 1.505(8) . ?
C14 H14 0.9300 . ?
C15 H15A 0.9600 . ?
C15 H15B 0.9600 . ?
C15 H15C 0.9600 . ?
C16 C17 1.382(8) . ?
C16 H16 0.9300 . ?
C17 C18 1.361(11) . ?
C17 H17 0.9300 . ?
C18 C19 1.384(10) . ?
C18 H18 0.9300 . ?
C19 C20 1.394(8) . ?
C19 H19 0.9300 . ?
C20 C21 1.495(8) . ?
C21 H21A 0.9700 . ?
C21 H21B 0.9700 . ?
C22 C23 1.493(8) . ?
C22 H22A 0.9700 . ?
C22 H22B 0.9700 . ?
C23 C24 1.392(8) . ?
C24 C25 1.382(10) . ?
C24 H24 0.9300 . ?
C25 C26 1.382(11) . ?
C25 H25 0.9300 . ?
C26 C27 1.356(10) . ?
C26 H26 0.9300 . ?
C27 H27 0.9300 . ?
C28 C29 1.489(9) . ?
C28 H28A 0.9700 . ?
C28 H28B 0.9700 . ?
C29 C30 1.384(9) . ?
C30 C31 1.380(13) . ?
C30 H30 0.9300 . ?
C31 C32 1.339(12) . ?
C31 H31 0.9300 . ?
C32 C33 1.379(9) . ?
C32 H32 0.9300 . ?
C33 H33 0.9300 . ?
Cl1 O4 1.31(4) . ?
Cl1 O1 1.34(2) . ?
Cl1 O2 1.37(3) . ?
Cl1 O3 1.446(14) . ?
Cl1' O4' 1.32(3) . ?
Cl1' O2' 1.33(2) . ?
Cl1' O3' 1.44(2) . ?
Cl1' O1' 1.51(3) . ?
O1W H1WA 0.8500 . ?
O1W H1WB 0.8500 . ?

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
C3 Fe1 C2 86.5(2) . . ?
C3 Fe1 C1 90.4(2) . . ?
C2 Fe1 C1 94.3(2) . . ?
C3 Fe1 N6 94.1(2) . . ?
C2 Fe1 N6 174.68(18) . . ?
C1 Fe1 N6 90.95(18) . . ?
C3 Fe1 N8 93.9(2) . . ?
C2 Fe1 N8 88.91(18) . . ?
C1 Fe1 N8 174.80(18) . . ?
N6 Fe1 N8 85.78(17) . . ?
C3 Fe1 N4 174.7(2) . . ?
C2 Fe1 N4 89.43(18) . . ?
C1 Fe1 N4 86.59(18) . . ?
N6 Fe1 N4 90.28(17) . . ?
N8 Fe1 N4 89.39(17) . . ?
N1 Fe2 N2 86.96(17) . 3_675 ?
N1 Fe2 N12 95.05(18) . . ?
N2 Fe2 N12 177.54(17) 3_675 . ?
N1 Fe2 N10 98.26(18) . . ?
N2 Fe2 N10 87.89(17) 3_675 . ?
N12 Fe2 N10 90.42(17) . . ?
N1 Fe2 N13 97.91(18) . . ?
N2 Fe2 N13 90.75(18) 3_675 . ?
N12 Fe2 N13 90.37(17) . . ?
N10 Fe2 N13 163.67(18) . . ?
N1 Fe2 N11 178.26(18) . . ?
N2 Fe2 N11 94.69(17) 3_675 . ?
N12 Fe2 N11 83.31(17) . . ?
N10 Fe2 N11 82.35(17) . . ?
N13 Fe2 N11 81.54(18) . . ?
N5 B1 N9 107.1(4) . . ?
N5 B1 N7 108.6(4) . . ?
N9 B1 N7 104.7(4) . . ?
N5 B1 H1 112.0 . . ?
N9 B1 H1 112.0 . . ?
N7 B1 H1 112.0 . . ?
C1 N1 Fe2 165.7(4) . . ?
C2 N2 Fe2 165.5(4) . 3_675 ?
C4 N4 N5 107.2(4) . . ?
C4 N4 Fe1 132.2(4) . . ?
N5 N4 Fe1 120.6(3) . . ?
N4 N5 C6 108.3(5) . . ?
N4 N5 B1 117.6(4) . . ?
C6 N5 B1 133.7(5) . . ?
C8 N6 N7 106.5(4) . . ?
C8 N6 Fe1 133.6(4) . . ?
N7 N6 Fe1 118.8(3) . . ?
C10 N7 N6 109.2(4) . . ?
C10 N7 B1 130.6(5) . . ?
N6 N7 B1 119.2(4) . . ?
C12 N8 N9 106.9(4) . . ?
C12 N8 Fe1 134.6(4) . . ?
N9 N8 Fe1 118.1(3) . . ?
C14 N9 N8 108.9(4) . . ?
C14 N9 B1 131.1(5) . . ?
N8 N9 B1 119.9(4) . . ?
C16 N10 C20 118.9(5) . . ?
C16 N10 Fe2 126.7(4) . . ?
C20 N10 Fe2 114.4(4) . . ?
C21 N11 C28 112.1(5) . . ?
C21 N11 C22 111.9(5) . . ?
C28 N11 C22 109.8(5) . . ?
C21 N11 Fe2 107.2(3) . . ?
C28 N11 Fe2 105.5(3) . . ?
C22 N11 Fe2 110.1(3) . . ?
C23 N12 C27 117.7(5) . . ?
C23 N12 Fe2 116.3(4) . . ?
C27 N12 Fe2 126.1(4) . . ?
C33 N13 C29 117.8(5) . . ?
C33 N13 Fe2 129.3(4) . . ?
C29 N13 Fe2 112.8(4) . . ?
N1 C1 Fe1 166.9(4) . . ?
N2 C2 Fe1 169.9(4) . . ?
N3 C3 Fe1 176.8(5) . . ?
N4 C4 C5 110.7(5) . . ?
N4 C4 H4 124.7 . . ?
C5 C4 H4 124.7 . . ?
C6 C5 C4 104.2(5) . . ?
C6 C5 C7 129.1(6) . . ?
C4 C5 C7 126.7(6) . . ?
N5 C6 C5 109.6(5) . . ?
N5 C6 H6 125.2 . . ?
C5 C6 H6 125.2 . . ?
C5 C7 H7A 109.5 . . ?
C5 C7 H7B 109.5 . . ?
H7A C7 H7B 109.5 . . ?
C5 C7 H7C 109.5 . . ?
H7A C7 H7C 109.5 . . ?
H7B C7 H7C 109.5 . . ?
N6 C8 C9 111.2(5) . . ?
N6 C8 H8 124.4 . . ?
C9 C8 H8 124.4 . . ?
C10 C9 C8 103.8(5) . . ?
C10 C9 C11 127.2(6) . . ?
C8 C9 C11 129.0(6) . . ?
N7 C10 C9 109.4(5) . . ?
N7 C10 H10 125.3 . . ?
C9 C10 H10 125.3 . . ?
C9 C11 H11A 109.5 . . ?
C9 C11 H11B 109.5 . . ?
H11A C11 H11B 109.5 . . ?
C9 C11 H11C 109.5 . . ?
H11A C11 H11C 109.5 . . ?
H11B C11 H11C 109.5 . . ?
N8 C12 C13 110.9(5) . . ?
N8 C12 H12 124.6 . . ?
C13 C12 H12 124.6 . . ?
C12 C13 C14 104.4(5) . . ?
C12 C13 C15 129.6(6) . . ?
C14 C13 C15 126.0(6) . . ?
N9 C14 C13 108.8(5) . . ?
N9 C14 H14 125.6 . . ?
C13 C14 H14 125.6 . . ?
C13 C15 H15A 109.5 . . ?
C13 C15 H15B 109.5 . . ?
H15A C15 H15B 109.5 . . ?
C13 C15 H15C 109.5 . . ?
H15A C15 H15C 109.5 . . ?
H15B C15 H15C 109.5 . . ?
N10 C16 C17 122.3(6) . . ?
N10 C16 H16 118.9 . . ?
C17 C16 H16 118.9 . . ?
C18 C17 C16 119.0(7) . . ?
C18 C17 H17 120.5 . . ?
C16 C17 H17 120.5 . . ?
C17 C18 C19 119.7(6) . . ?
C17 C18 H18 120.1 . . ?
C19 C18 H18 120.1 . . ?
C18 C19 C20 118.6(6) . . ?
C18 C19 H19 120.7 . . ?
C20 C19 H19 120.7 . . ?
N10 C20 C19 121.5(6) . . ?
N10 C20 C21 115.4(5) . . ?
C19 C20 C21 122.8(5) . . ?
N11 C21 C20 110.2(4) . . ?
N11 C21 H21A 109.6 . . ?
C20 C21 H21A 109.6 . . ?
N11 C21 H21B 109.6 . . ?
C20 C21 H21B 109.6 . . ?
H21A C21 H21B 108.1 . . ?
N11 C22 C23 113.3(5) . . ?
N11 C22 H22A 108.9 . . ?
C23 C22 H22A 108.9 . . ?
N11 C22 H22B 108.9 . . ?
C23 C22 H22B 108.9 . . ?
H22A C22 H22B 107.7 . . ?
N12 C23 C24 123.2(6) . . ?
N12 C23 C22 116.2(5) . . ?
C24 C23 C22 120.5(5) . . ?
C25 C24 C23 118.0(6) . . ?
C25 C24 H24 121.0 . . ?
C23 C24 H24 121.0 . . ?
C26 C25 C24 118.5(6) . . ?
C26 C25 H25 120.8 . . ?
C24 C25 H25 120.8 . . ?
C27 C26 C25 120.5(7) . . ?
C27 C26 H26 119.7 . . ?
C25 C26 H26 119.7 . . ?
N12 C27 C26 122.1(6) . . ?
N12 C27 H27 118.9 . . ?
C26 C27 H27 118.9 . . ?
N11 C28 C29 108.4(5) . . ?
N11 C28 H28A 110.0 . . ?
C29 C28 H28A 110.0 . . ?
N11 C28 H28B 110.0 . . ?
C29 C28 H28B 110.0 . . ?
H28A C28 H28B 108.4 . . ?
N13 C29 C30 121.1(7) . . ?
N13 C29 C28 115.7(5) . . ?
C30 C29 C28 123.3(6) . . ?
C31 C30 C29 119.4(8) . . ?
C31 C30 H30 120.3 . . ?
C29 C30 H30 120.3 . . ?
C32 C31 C30 119.2(7) . . ?
C32 C31 H31 120.4 . . ?
C30 C31 H31 120.4 . . ?
C31 C32 C33 120.2(8) . . ?
C31 C32 H32 119.9 . . ?
C33 C32 H32 119.9 . . ?
N13 C33 C32 122.2(7) . . ?
N13 C33 H33 118.9 . . ?
C32 C33 H33 118.9 . . ?
O4 Cl1 O1 99.5(19) . . ?
O4 Cl1 O2 134.2(19) . . ?
O1 Cl1 O2 92.1(14) . . ?
O4 Cl1 O3 109(2) . . ?
O1 Cl1 O3 124.1(14) . . ?
O2 Cl1 O3 100.5(15) . . ?
O4' Cl1' O2' 105(2) . . ?
O4' Cl1' O3' 103.8(17) . . ?
O2' Cl1' O3' 101.6(15) . . ?
O4' Cl1' O1' 115.1(18) . . ?
O2' Cl1' O1' 112.9(15) . . ?
O3' Cl1' O1' 117.1(14) . . ?
H1WA O1W H1WB 108.5 . . ?

loop_
_geom_torsion_atom_site_label_1
_geom_torsion_atom_site_label_2
_geom_torsion_atom_site_label_3
_geom_torsion_atom_site_label_4
_geom_torsion
_geom_torsion_site_symmetry_1
_geom_torsion_site_symmetry_2
_geom_torsion_site_symmetry_3
_geom_torsion_site_symmetry_4
_geom_torsion_publ_flag
C4 N4 N5 C6 0.9(5) . . . . ?
Fe1 N4 N5 C6 -178.7(3) . . . . ?
C4 N4 N5 B1 174.5(4) . . . . ?
Fe1 N4 N5 B1 -5.1(5) . . . . ?
N9 B1 N5 N4 -53.5(6) . . . . ?
N7 B1 N5 N4 59.0(5) . . . . ?
N9 B1 N5 C6 118.1(6) . . . . ?
N7 B1 N5 C6 -129.4(6) . . . . ?
C8 N6 N7 C10 -0.8(5) . . . . ?
Fe1 N6 N7 C10 168.7(3) . . . . ?
C8 N6 N7 B1 -170.7(4) . . . . ?
Fe1 N6 N7 B1 -1.1(5) . . . . ?
N5 B1 N7 C10 136.7(5) . . . . ?
N9 B1 N7 C10 -109.2(6) . . . . ?
N5 B1 N7 N6 -56.0(5) . . . . ?
N9 B1 N7 N6 58.1(5) . . . . ?
C12 N8 N9 C14 -2.2(6) . . . . ?
Fe1 N8 N9 C14 172.0(4) . . . . ?
C12 N8 N9 B1 176.5(5) . . . . ?
Fe1 N8 N9 B1 -9.3(6) . . . . ?
N5 B1 N9 C14 -118.6(6) . . . . ?
N7 B1 N9 C14 126.3(6) . . . . ?
N5 B1 N9 N8 63.0(6) . . . . ?
N7 B1 N9 N8 -52.1(6) . . . . ?
Fe2 N1 C1 Fe1 -36(3) . . . . ?
Fe2 N2 C2 Fe1 52(3) 3_675 . . . ?
N5 N4 C4 C5 -0.1(5) . . . . ?
Fe1 N4 C4 C5 179.3(4) . . . . ?
N4 C4 C5 C6 -0.6(6) . . . . ?
N4 C4 C5 C7 178.6(6) . . . . ?
N4 N5 C6 C5 -1.3(6) . . . . ?
B1 N5 C6 C5 -173.5(5) . . . . ?
C4 C5 C6 N5 1.2(6) . . . . ?
C7 C5 C6 N5 -178.1(6) . . . . ?
N7 N6 C8 C9 0.8(5) . . . . ?
Fe1 N6 C8 C9 -166.5(4) . . . . ?
N6 C8 C9 C10 -0.5(6) . . . . ?
N6 C8 C9 C11 179.9(6) . . . . ?
N6 N7 C10 C9 0.6(5) . . . . ?
B1 N7 C10 C9 168.8(5) . . . . ?
C8 C9 C10 N7 -0.1(6) . . . . ?
C11 C9 C10 N7 179.6(6) . . . . ?
N9 N8 C12 C13 2.3(7) . . . . ?
Fe1 N8 C12 C13 -170.5(4) . . . . ?
N8 C12 C13 C14 -1.5(7) . . . . ?
N8 C12 C13 C15 177.1(7) . . . . ?
N8 N9 C14 C13 1.3(7) . . . . ?
B1 N9 C14 C13 -177.3(6) . . . . ?
C12 C13 C14 N9 0.2(8) . . . . ?
C15 C13 C14 N9 -178.5(7) . . . . ?
C20 N10 C16 C17 1.2(8) . . . . ?
Fe2 N10 C16 C17 -179.6(5) . . . . ?
N10 C16 C17 C18 -0.3(10) . . . . ?
C16 C17 C18 C19 -0.2(12) . . . . ?
C17 C18 C19 C20 -0.1(12) . . . . ?
C16 N10 C20 C19 -1.6(8) . . . . ?
Fe2 N10 C20 C19 179.1(5) . . . . ?
C16 N10 C20 C21 171.9(5) . . . . ?
Fe2 N10 C20 C21 -7.4(6) . . . . ?
C18 C19 C20 N10 1.1(10) . . . . ?
C18 C19 C20 C21 -171.9(7) . . . . ?
C28 N11 C21 C20 -150.0(5) . . . . ?
C22 N11 C21 C20 86.2(6) . . . . ?
Fe2 N11 C21 C20 -34.6(5) . . . . ?
N10 C20 C21 N11 28.8(7) . . . . ?
C19 C20 C21 N11 -157.8(6) . . . . ?
C21 N11 C22 C23 -109.8(6) . . . . ?
C28 N11 C22 C23 125.1(5) . . . . ?
Fe2 N11 C22 C23 9.3(6) . . . . ?
C27 N12 C23 C24 0.9(8) . . . . ?
Fe2 N12 C23 C24 -178.4(4) . . . . ?
C27 N12 C23 C22 -176.7(5) . . . . ?
Fe2 N12 C23 C22 4.1(6) . . . . ?
N11 C22 C23 N12 -9.1(8) . . . . ?
N11 C22 C23 C24 173.3(5) . . . . ?
N12 C23 C24 C25 -1.2(9) . . . . ?
C22 C23 C24 C25 176.3(6) . . . . ?
C23 C24 C25 C26 0.3(10) . . . . ?
C24 C25 C26 C27 0.9(11) . . . . ?
C23 N12 C27 C26 0.4(9) . . . . ?
Fe2 N12 C27 C26 179.5(5) . . . . ?
C25 C26 C27 N12 -1.3(11) . . . . ?
C21 N11 C28 C29 158.4(5) . . . . ?
C22 N11 C28 C29 -76.6(6) . . . . ?
Fe2 N11 C28 C29 42.0(5) . . . . ?
C33 N13 C29 C30 0.6(8) . . . . ?
Fe2 N13 C29 C30 -177.9(5) . . . . ?
C33 N13 C29 C28 -178.8(5) . . . . ?
Fe2 N13 C29 C28 2.7(6) . . . . ?
N11 C28 C29 N13 -30.7(7) . . . . ?
N11 C28 C29 C30 149.9(6) . . . . ?
N13 C29 C30 C31 0.8(11) . . . . ?
C28 C29 C30 C31 -179.8(7) . . . . ?
C29 C30 C31 C32 -2.5(13) . . . . ?
C30 C31 C32 C33 2.7(13) . . . . ?
C29 N13 C33 C32 -0.5(9) . . . . ?
Fe2 N13 C33 C32 177.8(5) . . . . ?
C31 C32 C33 N13 -1.2(11) . . . . ?

loop_
_geom_hbond_atom_site_label_D
_geom_hbond_atom_site_label_H
_geom_hbond_atom_site_label_A
_geom_hbond_distance_DH
_geom_hbond_distance_HA
_geom_hbond_distance_DA
_geom_hbond_angle_DHA
_geom_hbond_site_symmetry_A
O1W H1WB O2 0.85 2.48 3.33(4) 172.8 3_576
O1W H1WA O2 0.85 2.65 3.50(3) 172.9 .
O1W H1WA Cl1 0.85 2.98 3.72(2) 146.8 .
C28 H28A O4' 0.97 2.64 3.27(2) 122.7 4_675
C27 H27 N1 0.93 2.57 3.086(8) 115.4 .
C26 H26 N3 0.93 2.42 3.281(9) 154.8 3_575
C22 H22A O2 0.97 2.64 3.33(3) 128.0 2_545
C17 H17 O3' 0.93 2.44 3.36(2) 167.1 1_554
C12 H12 O4' 0.93 2.65 3.50(3) 151.9 2
C12 H12 O4 0.93 2.58 3.41(4) 148.5 2
C10 H10 O2' 0.93 2.54 3.37(2) 148.8 .
C10 H10 O2 0.93 2.47 3.22(3) 137.9 .
O1W H1WB O2 0.85 2.48 3.33(4) 172.8 3_576
O1W H1WA O2 0.85 2.65 3.50(3) 172.9 .

_refine_diff_density_max         0.809
_refine_diff_density_min         -0.592
_refine_diff_density_rms         0.093

####################################################################### 
# 
# 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_2-100K
_database_code_depnum_ccdc_archive 'CCDC 1419280'
_audit_update_record             
;
2016-09-02 deposited with the CCDC.
2016-09-26 downloaded from the CCDC.
;

_audit_creation_method           SHELXL-97
_chemical_name_systematic        
; 
 ? 
;
_chemical_name_common            ?
_chemical_melting_point          ?
_chemical_formula_moiety         '(C66 H68 B2 Fe4 N26), 2(Cl O4)'
_chemical_formula_sum            'C66 H68 B2 Cl2 Fe4 N26 O8'
_chemical_formula_weight         1669.38

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'
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'
B B 0.0013 0.0007 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Cl Cl 0.1484 0.1585 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Fe Fe 0.3463 0.8444 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'

_space_group_crystal_system      monoclinic
_space_group_IT_number           14
_space_group_name_H-M_alt        'P 21/n'
_space_group_name_Hall           '-P 2yn'

_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.
;

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                   12.820(3)
_cell_length_b                   17.772(4)
_cell_length_c                   16.154(4)
_cell_angle_alpha                90
_cell_angle_beta                 98.253(3)
_cell_angle_gamma                90
_cell_volume                     3642.4(15)
_cell_formula_units_Z            2
_cell_measurement_temperature    296(2)
_cell_measurement_reflns_used    7429
_cell_measurement_theta_min      2.22
_cell_measurement_theta_max      30.02

_exptl_crystal_description       Block
_exptl_crystal_colour            Red
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    ?
_exptl_crystal_density_diffrn    1.522
_exptl_crystal_F_000             1716
_exptl_transmission_factor_min   ?
_exptl_transmission_factor_max   ?
_exptl_crystal_size_max          0.120
_exptl_crystal_size_mid          0.100
_exptl_crystal_size_min          0.100
_exptl_absorpt_coefficient_mu    0.928
_shelx_estimated_absorpt_T_min   0.897
_shelx_estimated_absorpt_T_max   0.913
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_correction_T_min  0.8968
_exptl_absorpt_correction_T_max  0.9129
_exptl_absorpt_process_details   SADABS
_exptl_absorpt_special_details   ?
_diffrn_ambient_temperature      296(2)
_diffrn_radiation_wavelength     0.71073
_diffrn_radiation_type           MoK\a
_diffrn_radiation_source         'fine-focus sealed tube'
_diffrn_radiation_monochromator  graphite
_diffrn_measurement_device_type  'Bruker APEX-II CCD'
_diffrn_measurement_method       'φ and ω scans'
_diffrn_detector_area_resol_mean ?
_diffrn_reflns_number            30418
_diffrn_reflns_av_unetI/netI     0.0446
_diffrn_reflns_av_R_equivalents  0.0430
_diffrn_reflns_limit_h_min       -16
_diffrn_reflns_limit_h_max       16
_diffrn_reflns_limit_k_min       -23
_diffrn_reflns_limit_k_max       23
_diffrn_reflns_limit_l_min       -21
_diffrn_reflns_limit_l_max       21
_diffrn_reflns_theta_min         1.713
_diffrn_reflns_theta_max         27.999
_diffrn_reflns_theta_full        25.242
_diffrn_measured_fraction_theta_max 0.996
_diffrn_measured_fraction_theta_full 0.995
_diffrn_reflns_Laue_measured_fraction_max 0.996
_diffrn_reflns_Laue_measured_fraction_full 0.995
_diffrn_reflns_point_group_measured_fraction_max 0.996
_diffrn_reflns_point_group_measured_fraction_full 0.995
_reflns_number_total             8758
_reflns_number_gt                6964
_reflns_threshold_expression     'I > 2σ(I)'
_reflns_Friedel_coverage         0.000
_reflns_Friedel_fraction_max     .
_reflns_Friedel_fraction_full    .

_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.
;

_computing_data_collection       'Bruker APEX2'
_computing_cell_refinement       'Bruker SAINT'
_computing_data_reduction        'Bruker SAINT'
_computing_structure_solution    'SHELXS-2014 (Sheldrick, 2014)'
_computing_structure_refinement  'SHELXL-2014/7 (Sheldrick, 2014)'
_computing_molecular_graphics    ?
_computing_publication_material  ?
_refine_special_details          ?
_refine_ls_structure_factor_coef Fsqd
_refine_ls_matrix_type           full
_refine_ls_weighting_scheme      calc
_refine_ls_weighting_details     
'w=1/[σ²(Fo²)+(0.0458P)²+3.2519P] where P=(Fo²+2Fc²)/3'
_atom_sites_solution_primary     ?
_atom_sites_solution_secondary   ?
_atom_sites_solution_hydrogens   mixed
_refine_ls_hydrogen_treatment    constr
_refine_ls_extinction_method     none
_refine_ls_extinction_coef       .
_refine_ls_number_reflns         8758
_refine_ls_number_parameters     536
_refine_ls_number_restraints     155
_refine_ls_R_factor_all          0.0578
_refine_ls_R_factor_gt           0.0409
_refine_ls_wR_factor_ref         0.1037
_refine_ls_wR_factor_gt          0.0958
_refine_ls_goodness_of_fit_ref   1.019
_refine_ls_restrained_S_all      1.032
_refine_ls_shift/su_max          0.005
_refine_ls_shift/su_mean         0.000

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 0.31673(3) 1.07290(2) 0.08543(2) 0.01481(8) Uani 1 1 d . . . . .
Fe2 Fe 0.36150(3) 0.81154(2) -0.00732(2) 0.01533(8) Uani 1 1 d . . . . .
B1 B 0.3207(2) 1.07647(15) 0.27743(16) 0.0218(5) Uani 1 1 d . . . . .
H1 H 0.3208 1.0777 0.3373 0.026 Uiso 1 1 d R U . . .
N1 N 0.32266(15) 0.91592(11) 0.00684(11) 0.0179(4) Uani 1 1 d . . . . .
N2 N 0.49858(15) 1.15021(10) 0.01602(12) 0.0181(4) Uani 1 1 d . . . . .
N3 N 0.17061(18) 1.13953(14) -0.06359(13) 0.0306(5) Uani 1 1 d . . . . .
N4 N 0.42361(16) 1.02664(11) 0.17149(11) 0.0186(4) Uani 1 1 d . . . . .
N5 N 0.41242(17) 1.02972(11) 0.25394(11) 0.0212(4) Uani 1 1 d . . . . .
N6 N 0.20274(16) 1.03795(10) 0.14612(11) 0.0189(4) Uani 1 1 d . . . . .
N7 N 0.21592(17) 1.04435(11) 0.23107(12) 0.0201(4) Uani 1 1 d . . . . .
N8 N 0.31764(16) 1.16392(11) 0.15526(11) 0.0186(4) Uani 1 1 d . . . . .
N9 N 0.32987(17) 1.15550(11) 0.23997(12) 0.0209(4) Uani 1 1 d . . . . .
N10 N 0.33661(15) 0.80883(11) -0.13055(12) 0.0186(4) Uani 1 1 d . . . . .
N11 N 0.39959(16) 0.70310(11) -0.01850(12) 0.0199(4) Uani 1 1 d . . . . .
N12 N 0.21912(15) 0.77295(11) -0.00349(11) 0.0182(4) Uani 1 1 d . . . . .
N13 N 0.40394(16) 0.79035(11) 0.11329(12) 0.0205(4) Uani 1 1 d . . . . .
C1 C 0.31635(18) 0.97804(13) 0.02713(13) 0.0166(4) Uani 1 1 d . . . . .
C2 C 0.42764(18) 1.11813(12) 0.03503(13) 0.0172(4) Uani 1 1 d . . . . .
C3 C 0.22307(19) 1.11450(13) -0.00626(14) 0.0205(5) Uani 1 1 d . . . . .
C4 C 0.51304(19) 0.98926(13) 0.16611(15) 0.0211(5) Uani 1 1 d . . . . .
H4 H 0.5390 0.9790 0.1164 0.025 Uiso 1 1 calc R U . . .
C5 C 0.5618(2) 0.96779(13) 0.24534(15) 0.0247(5) Uani 1 1 d . . . . .
C6 C 0.4956(2) 0.99513(14) 0.29910(15) 0.0251(5) Uani 1 1 d . . . . .
H6 H 0.5066 0.9904 0.3570 0.030 Uiso 1 1 calc R U . . .
C7 C 0.6615(2) 0.92309(16) 0.26562(19) 0.0352(6) Uani 1 1 d . . . . .
H7A H 0.7101 0.9500 0.3058 0.053 Uiso 1 1 calc R U . . .
H7B H 0.6925 0.9154 0.2156 0.053 Uiso 1 1 calc R U . . .
H7C H 0.6458 0.8752 0.2885 0.053 Uiso 1 1 calc R U . . .
C8 C 0.1007(2) 1.02323(13) 0.12183(16) 0.0227(5) Uani 1 1 d . . . . .
H8 H 0.0701 1.0161 0.0666 0.027 Uiso 1 1 calc R U . . .
C9 C 0.0464(2) 1.02004(14) 0.19067(17) 0.0271(5) Uani 1 1 d . . . . .
C10 C 0.1227(2) 1.03422(13) 0.25794(16) 0.0247(5) Uani 1 1 d . . . . .
H10 H 0.1113 1.0364 0.3135 0.030 Uiso 1 1 calc R U . . .
C11 C -0.0681(2) 1.00318(18) 0.1922(2) 0.0398(7) Uani 1 1 d . . . . .
H11A H -0.0842 1.0100 0.2480 0.060 Uiso 1 1 calc R U . . .
H11B H -0.0826 0.9521 0.1749 0.060 Uiso 1 1 calc R U . . .
H11C H -0.1106 1.0367 0.1548 0.060 Uiso 1 1 calc R U . . .
C12 C 0.3210(2) 1.23756(13) 0.13990(15) 0.0239(5) Uani 1 1 d . . . . .
H12 H 0.3132 1.2589 0.0868 0.029 Uiso 1 1 calc R U . . .
C13 C 0.3379(2) 1.27794(14) 0.21449(17) 0.0308(6) Uani 1 1 d . . . . .
C14 C 0.3422(2) 1.22369(14) 0.27553(15) 0.0268(6) Uani 1 1 d . . . . .
H14 H 0.3520 1.2329 0.3328 0.032 Uiso 1 1 calc R U . . .
C15 C 0.3499(3) 1.36122(16) 0.2268(2) 0.0500(9) Uani 1 1 d . . . . .
H15A H 0.4073 1.3789 0.1999 0.075 Uiso 1 1 calc R U . . .
H15B H 0.3641 1.3722 0.2856 0.075 Uiso 1 1 calc R U . . .
H15C H 0.2860 1.3859 0.2030 0.075 Uiso 1 1 calc R U . . .
C16 C 0.2937(2) 0.86291(14) -0.18274(15) 0.0233(5) Uani 1 1 d . . . . .
H16 H 0.2715 0.9073 -0.1603 0.028 Uiso 1 1 calc R U . . .
C17 C 0.2813(2) 0.85476(15) -0.26894(15) 0.0302(6) Uani 1 1 d . . . . .
H17 H 0.2525 0.8936 -0.3035 0.036 Uiso 1 1 calc R U . . .
C18 C 0.3121(2) 0.78880(16) -0.30293(16) 0.0341(6) Uani 1 1 d . . . . .
H18 H 0.3025 0.7818 -0.3606 0.041 Uiso 1 1 calc R U . . .
C19 C 0.3576(2) 0.73303(15) -0.24954(16) 0.0297(6) Uani 1 1 d . . . . .
H19 H 0.3795 0.6880 -0.2708 0.036 Uiso 1 1 calc R U . . .
C20 C 0.3701(2) 0.74531(13) -0.16425(15) 0.0231(5) Uani 1 1 d . . . . .
C21 C 0.4313(2) 0.69281(14) -0.10240(16) 0.0267(5) Uani 1 1 d . . . . .
H21A H 0.4183 0.6412 -0.1205 0.032 Uiso 1 1 calc R U . . .
H21B H 0.5061 0.7027 -0.0997 0.032 Uiso 1 1 calc R U . . .
C22 C 0.3080(2) 0.65384(13) -0.00645(17) 0.0251(5) Uani 1 1 d . . . . .
H22A H 0.2986 0.6160 -0.0502 0.030 Uiso 1 1 calc R U . . .
H22B H 0.3234 0.6280 0.0468 0.030 Uiso 1 1 calc R U . . .
C23 C 0.20807(19) 0.69720(13) -0.00830(13) 0.0198(5) Uani 1 1 d . . . . .
C24 C 0.1117(2) 0.66162(15) -0.00977(14) 0.0249(5) Uani 1 1 d . . . . .
H24 H 0.1066 0.6096 -0.0151 0.030 Uiso 1 1 calc R U . . .
C25 C 0.0235(2) 0.70433(17) -0.00330(17) 0.0316(6) Uani 1 1 d . . . . .
H25 H -0.0418 0.6816 -0.0030 0.038 Uiso 1 1 calc R U . . .
C26 C 0.0340(2) 0.78217(17) 0.00285(17) 0.0314(6) Uani 1 1 d . . . . .
H26 H -0.0243 0.8122 0.0074 0.038 Uiso 1 1 calc R U . . .
C27 C 0.13160(19) 0.81405(15) 0.00205(15) 0.0241(5) Uani 1 1 d . . . . .
H27 H 0.1377 0.8661 0.0055 0.029 Uiso 1 1 calc R U . . .
C28 C 0.4885(2) 0.68897(14) 0.04969(16) 0.0265(5) Uani 1 1 d . . . . .
H28A H 0.5535 0.7088 0.0343 0.032 Uiso 1 1 calc R U . . .
H28B H 0.4971 0.6353 0.0594 0.032 Uiso 1 1 calc R U . . .
C29 C 0.4636(2) 0.72723(14) 0.12714(16) 0.0258(5) Uani 1 1 d . . . . .
C30 C 0.4993(2) 0.70196(16) 0.20719(18) 0.0368(7) Uani 1 1 d . . . . .
H30 H 0.5396 0.6584 0.2153 0.044 Uiso 1 1 calc R U . . .
C31 C 0.4746(3) 0.74198(18) 0.27484(18) 0.0468(9) Uani 1 1 d . . . . .
H31 H 0.4977 0.7256 0.3290 0.056 Uiso 1 1 calc R U . . .
C32 C 0.4154(3) 0.80621(16) 0.26118(16) 0.0382(7) Uani 1 1 d . . . . .
H32 H 0.3985 0.8342 0.3060 0.046 Uiso 1 1 calc R U . . .
C33 C 0.3810(2) 0.82892(14) 0.17959(15) 0.0268(5) Uani 1 1 d . . . . .
H33 H 0.3407 0.8724 0.1707 0.032 Uiso 1 1 calc R U . . .
Cl1 Cl 0.25129(19) 0.93592(10) 0.49126(14) 0.0296(5) Uani 0.445(4) 1 d . U P A
1
O1 O 0.3247(5) 0.9312(4) 0.4307(5) 0.078(2) Uani 0.445(4) 1 d . U P A 1
O2 O 0.1621(6) 0.9735(6) 0.4456(6) 0.0473(19) Uani 0.445(4) 1 d . U P A 1
O3 O 0.2944(6) 0.9797(3) 0.5591(4) 0.070(2) Uani 0.445(4) 1 d . U P A 1
O4 O 0.238(2) 0.8643(18) 0.515(2) 0.043(3) Uani 0.445(4) 1 d . U P A 1
Cl1' Cl 0.2000(2) 0.94856(9) 0.50954(9) 0.0401(5) Uani 0.555(4) 1 d D U P A 2
O1' O 0.2906(5) 0.9868(3) 0.4932(5) 0.092(2) Uani 0.555(4) 1 d D U P A 2
O2' O 0.1153(6) 0.9630(5) 0.4462(5) 0.067(2) Uani 0.555(4) 1 d D U P A 2
O3' O 0.1692(4) 0.9730(2) 0.5851(2) 0.0473(12) Uani 0.555(4) 1 d D U P A 2
O4' O 0.2161(17) 0.8660(13) 0.5117(17) 0.043(3) Uani 0.555(4) 1 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
Fe1 C2 1.914(2) . ?
Fe1 C3 1.916(2) . ?
Fe1 C1 1.931(2) . ?
Fe1 N8 1.9712(19) . ?
Fe1 N6 1.973(2) . ?
Fe1 N4 1.985(2) . ?
Fe2 N2 1.942(2) 3_675 ?
Fe2 N1 1.9427(19) . ?
Fe2 N12 1.959(2) . ?
Fe2 N10 1.9709(19) . ?
Fe2 N13 1.982(2) . ?
Fe2 N11 2.003(2) . ?
B1 N5 1.532(3) . ?
B1 N9 1.541(3) . ?
B1 N7 1.550(4) . ?
B1 H1 0.9670 . ?
N1 C1 1.158(3) . ?
N2 C2 1.152(3) . ?
N2 Fe2 1.942(2) 3_675 ?
N3 C3 1.153(3) . ?
N4 C4 1.339(3) . ?
N4 N5 1.361(3) . ?
N5 C6 1.350(3) . ?
N6 C8 1.336(3) . ?
N6 N7 1.363(3) . ?
N7 C10 1.341(3) . ?
N8 C12 1.334(3) . ?
N8 N9 1.363(3) . ?
N9 C14 1.341(3) . ?
N10 C16 1.343(3) . ?
N10 C20 1.350(3) . ?
N11 C21 1.481(3) . ?
N11 C28 1.488(3) . ?
N11 C22 1.500(3) . ?
N12 C27 1.352(3) . ?
N12 C23 1.355(3) . ?
N13 C33 1.339(3) . ?
N13 C29 1.358(3) . ?
C4 C5 1.395(3) . ?
C4 H4 0.9300 . ?
C5 C6 1.387(4) . ?
C5 C7 1.501(4) . ?
C6 H6 0.9300 . ?
C7 H7A 0.9600 . ?
C7 H7B 0.9600 . ?
C7 H7C 0.9600 . ?
C8 C9 1.395(3) . ?
C8 H8 0.9300 . ?
C9 C10 1.377(4) . ?
C9 C11 1.502(4) . ?
C10 H10 0.9300 . ?
C11 H11A 0.9600 . ?
C11 H11B 0.9600 . ?
C11 H11C 0.9600 . ?
C12 C13 1.392(3) . ?
C12 H12 0.9300 . ?
C13 C14 1.375(4) . ?
C13 C15 1.498(4) . ?
C14 H14 0.9300 . ?
C15 H15A 0.9600 . ?
C15 H15B 0.9600 . ?
C15 H15C 0.9600 . ?
C16 C17 1.386(3) . ?
C16 H16 0.9300 . ?
C17 C18 1.376(4) . ?
C17 H17 0.9300 . ?
C18 C19 1.387(4) . ?
C18 H18 0.9300 . ?
C19 C20 1.381(3) . ?
C19 H19 0.9300 . ?
C20 C21 1.503(4) . ?
C21 H21A 0.9700 . ?
C21 H21B 0.9700 . ?
C22 C23 1.491(3) . ?
C22 H22A 0.9700 . ?
C22 H22B 0.9700 . ?
C23 C24 1.385(3) . ?
C24 C25 1.379(4) . ?
C24 H24 0.9300 . ?
C25 C26 1.392(4) . ?
C25 H25 0.9300 . ?
C26 C27 1.376(4) . ?
C26 H26 0.9300 . ?
C27 H27 0.9300 . ?
C28 C29 1.498(4) . ?
C28 H28A 0.9700 . ?
C28 H28B 0.9700 . ?
C29 C30 1.383(4) . ?
C30 C31 1.378(5) . ?
C30 H30 0.9300 . ?
C31 C32 1.371(5) . ?
C31 H31 0.9300 . ?
C32 C33 1.388(4) . ?
C32 H32 0.9300 . ?
C33 H33 0.9300 . ?
Cl1 O4 1.35(3) . ?
Cl1 O3 1.393(6) . ?
Cl1 O2 1.433(8) . ?
Cl1 O1 1.455(7) . ?
Cl1' O3' 1.404(4) . ?
Cl1' O2' 1.404(6) . ?
Cl1' O1' 1.404(5) . ?
Cl1' O4' 1.48(2) . ?

loop_
_geom_angle_atom_site_label_1
_geom_angle_atom_site_label_2
_geom_angle_atom_site_label_3
_geom_angle
_geom_angle_site_symmetry_1
_geom_angle_site_symmetry_3
_geom_angle_publ_flag
C2 Fe1 C3 86.02(10) . . ?
C2 Fe1 C1 96.27(9) . . ?
C3 Fe1 C1 90.14(10) . . ?
C2 Fe1 N8 87.43(9) . . ?
C3 Fe1 N8 94.44(9) . . ?
C1 Fe1 N8 174.32(8) . . ?
C2 Fe1 N6 172.72(9) . . ?
C3 Fe1 N6 94.53(9) . . ?
C1 Fe1 N6 90.99(9) . . ?
N8 Fe1 N6 85.30(8) . . ?
C2 Fe1 N4 89.52(9) . . ?
C3 Fe1 N4 173.86(9) . . ?
C1 Fe1 N4 86.16(9) . . ?
N8 Fe1 N4 89.55(8) . . ?
N6 Fe1 N4 90.43(8) . . ?
N2 Fe2 N1 85.95(8) 3_675 . ?
N2 Fe2 N12 177.69(8) 3_675 . ?
N1 Fe2 N12 94.29(8) . . ?
N2 Fe2 N10 87.29(8) 3_675 . ?
N1 Fe2 N10 97.77(8) . . ?
N12 Fe2 N10 90.39(8) . . ?
N2 Fe2 N13 90.66(8) 3_675 . ?
N1 Fe2 N13 95.99(8) . . ?
N12 Fe2 N13 91.61(8) . . ?
N10 Fe2 N13 165.90(8) . . ?
N2 Fe2 N11 95.20(8) 3_675 . ?
N1 Fe2 N11 178.12(8) . . ?
N12 Fe2 N11 84.63(8) . . ?
N10 Fe2 N11 83.78(8) . . ?
N13 Fe2 N11 82.52(8) . . ?
N5 B1 N9 107.0(2) . . ?
N5 B1 N7 108.87(19) . . ?
N9 B1 N7 104.82(19) . . ?
N5 B1 H1 111.6 . . ?
N9 B1 H1 112.6 . . ?
N7 B1 H1 111.6 . . ?
C1 N1 Fe2 166.75(19) . . ?
C2 N2 Fe2 164.87(18) . 3_675 ?
C4 N4 N5 107.16(18) . . ?
C4 N4 Fe1 132.20(16) . . ?
N5 N4 Fe1 120.64(15) . . ?
C6 N5 N4 108.9(2) . . ?
C6 N5 B1 133.5(2) . . ?
N4 N5 B1 117.18(19) . . ?
C8 N6 N7 106.65(19) . . ?
C8 N6 Fe1 132.78(16) . . ?
N7 N6 Fe1 118.71(15) . . ?
C10 N7 N6 109.1(2) . . ?
C10 N7 B1 130.1(2) . . ?
N6 N7 B1 119.40(18) . . ?
C12 N8 N9 107.00(18) . . ?
C12 N8 Fe1 134.13(16) . . ?
N9 N8 Fe1 118.35(14) . . ?
C14 N9 N8 108.69(19) . . ?
C14 N9 B1 131.81(19) . . ?
N8 N9 B1 119.35(18) . . ?
C16 N10 C20 118.1(2) . . ?
C16 N10 Fe2 127.51(16) . . ?
C20 N10 Fe2 114.39(16) . . ?
C21 N11 C28 112.0(2) . . ?
C21 N11 C22 111.68(19) . . ?
C28 N11 C22 109.64(19) . . ?
C21 N11 Fe2 107.69(14) . . ?
C28 N11 Fe2 105.45(14) . . ?
C22 N11 Fe2 110.14(15) . . ?
C27 N12 C23 117.4(2) . . ?
C27 N12 Fe2 126.77(17) . . ?
C23 N12 Fe2 115.86(16) . . ?
C33 N13 C29 118.3(2) . . ?
C33 N13 Fe2 128.91(18) . . ?
C29 N13 Fe2 112.80(16) . . ?
N1 C1 Fe1 167.25(19) . . ?
N2 C2 Fe1 169.92(19) . . ?
N3 C3 Fe1 176.8(2) . . ?
N4 C4 C5 110.6(2) . . ?
N4 C4 H4 124.7 . . ?
C5 C4 H4 124.7 . . ?
C6 C5 C4 104.2(2) . . ?
C6 C5 C7 128.9(2) . . ?
C4 C5 C7 126.9(2) . . ?
N5 C6 C5 109.2(2) . . ?
N5 C6 H6 125.4 . . ?
C5 C6 H6 125.4 . . ?
C5 C7 H7A 109.5 . . ?
C5 C7 H7B 109.5 . . ?
H7A C7 H7B 109.5 . . ?
C5 C7 H7C 109.5 . . ?
H7A C7 H7C 109.5 . . ?
H7B C7 H7C 109.5 . . ?
N6 C8 C9 110.7(2) . . ?
N6 C8 H8 124.7 . . ?
C9 C8 H8 124.7 . . ?
C10 C9 C8 104.0(2) . . ?
C10 C9 C11 127.5(2) . . ?
C8 C9 C11 128.5(3) . . ?
N7 C10 C9 109.5(2) . . ?
N7 C10 H10 125.2 . . ?
C9 C10 H10 125.2 . . ?
C9 C11 H11A 109.5 . . ?
C9 C11 H11B 109.5 . . ?
H11A C11 H11B 109.5 . . ?
C9 C11 H11C 109.5 . . ?
H11A C11 H11C 109.5 . . ?
H11B C11 H11C 109.5 . . ?
N8 C12 C13 110.5(2) . . ?
N8 C12 H12 124.8 . . ?
C13 C12 H12 124.8 . . ?
C14 C13 C12 104.2(2) . . ?
C14 C13 C15 127.2(2) . . ?
C12 C13 C15 128.7(2) . . ?
N9 C14 C13 109.7(2) . . ?
N9 C14 H14 125.2 . . ?
C13 C14 H14 125.2 . . ?
C13 C15 H15A 109.5 . . ?
C13 C15 H15B 109.5 . . ?
H15A C15 H15B 109.5 . . ?
C13 C15 H15C 109.5 . . ?
H15A C15 H15C 109.5 . . ?
H15B C15 H15C 109.5 . . ?
N10 C16 C17 122.2(2) . . ?
N10 C16 H16 118.9 . . ?
C17 C16 H16 118.9 . . ?
C18 C17 C16 119.5(3) . . ?
C18 C17 H17 120.3 . . ?
C16 C17 H17 120.3 . . ?
C17 C18 C19 118.7(2) . . ?
C17 C18 H18 120.7 . . ?
C19 C18 H18 120.7 . . ?
C20 C19 C18 119.1(2) . . ?
C20 C19 H19 120.5 . . ?
C18 C19 H19 120.5 . . ?
N10 C20 C19 122.4(2) . . ?
N10 C20 C21 114.6(2) . . ?
C19 C20 C21 122.7(2) . . ?
N11 C21 C20 110.27(19) . . ?
N11 C21 H21A 109.6 . . ?
C20 C21 H21A 109.6 . . ?
N11 C21 H21B 109.6 . . ?
C20 C21 H21B 109.6 . . ?
H21A C21 H21B 108.1 . . ?
C23 C22 N11 112.46(19) . . ?
C23 C22 H22A 109.1 . . ?
N11 C22 H22A 109.1 . . ?
C23 C22 H22B 109.1 . . ?
N11 C22 H22B 109.1 . . ?
H22A C22 H22B 107.8 . . ?
N12 C23 C24 122.7(2) . . ?
N12 C23 C22 115.5(2) . . ?
C24 C23 C22 121.7(2) . . ?
C25 C24 C23 119.1(2) . . ?
C25 C24 H24 120.4 . . ?
C23 C24 H24 120.4 . . ?
C24 C25 C26 118.7(2) . . ?
C24 C25 H25 120.6 . . ?
C26 C25 H25 120.6 . . ?
C27 C26 C25 119.2(2) . . ?
C27 C26 H26 120.4 . . ?
C25 C26 H26 120.4 . . ?
N12 C27 C26 122.9(2) . . ?
N12 C27 H27 118.6 . . ?
C26 C27 H27 118.6 . . ?
N11 C28 C29 108.0(2) . . ?
N11 C28 H28A 110.1 . . ?
C29 C28 H28A 110.1 . . ?
N11 C28 H28B 110.1 . . ?
C29 C28 H28B 110.1 . . ?
H28A C28 H28B 108.4 . . ?
N13 C29 C30 121.7(3) . . ?
N13 C29 C28 114.8(2) . . ?
C30 C29 C28 123.5(2) . . ?
C31 C30 C29 119.4(3) . . ?
C31 C30 H30 120.3 . . ?
C29 C30 H30 120.3 . . ?
C32 C31 C30 119.1(3) . . ?
C32 C31 H31 120.4 . . ?
C30 C31 H31 120.4 . . ?
C31 C32 C33 119.2(3) . . ?
C31 C32 H32 120.4 . . ?
C33 C32 H32 120.4 . . ?
N13 C33 C32 122.3(3) . . ?
N13 C33 H33 118.9 . . ?
C32 C33 H33 118.9 . . ?
O4 Cl1 O3 110.6(15) . . ?
O4 Cl1 O2 117.6(12) . . ?
O3 Cl1 O2 110.0(5) . . ?
O4 Cl1 O1 105.2(16) . . ?
O3 Cl1 O1 109.9(5) . . ?
O2 Cl1 O1 103.0(5) . . ?
O3' Cl1' O2' 107.0(4) . . ?
O3' Cl1' O1' 110.9(4) . . ?
O2' Cl1' O1' 110.4(5) . . ?
O3' Cl1' O4' 110.0(11) . . ?
O2' Cl1' O4' 106.8(10) . . ?
O1' Cl1' O4' 111.5(9) . . ?

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
C4 N4 N5 C6 0.8(2) . . . . ?
Fe1 N4 N5 C6 -179.33(16) . . . . ?
C4 N4 N5 B1 174.4(2) . . . . ?
Fe1 N4 N5 B1 -5.8(3) . . . . ?
N9 B1 N5 C6 118.1(3) . . . . ?
N7 B1 N5 C6 -129.1(3) . . . . ?
N9 B1 N5 N4 -53.5(3) . . . . ?
N7 B1 N5 N4 59.3(3) . . . . ?
C8 N6 N7 C10 -0.5(2) . . . . ?
Fe1 N6 N7 C10 165.92(15) . . . . ?
C8 N6 N7 B1 -168.21(19) . . . . ?
Fe1 N6 N7 B1 -1.8(3) . . . . ?
N5 B1 N7 C10 139.5(2) . . . . ?
N9 B1 N7 C10 -106.2(3) . . . . ?
N5 B1 N7 N6 -55.7(3) . . . . ?
N9 B1 N7 N6 58.5(2) . . . . ?
C12 N8 N9 C14 -0.9(3) . . . . ?
Fe1 N8 N9 C14 171.98(17) . . . . ?
C12 N8 N9 B1 175.2(2) . . . . ?
Fe1 N8 N9 B1 -11.9(3) . . . . ?
N5 B1 N9 C14 -119.8(3) . . . . ?
N7 B1 N9 C14 124.7(3) . . . . ?
N5 B1 N9 N8 65.1(3) . . . . ?
N7 B1 N9 N8 -50.4(3) . . . . ?
Fe2 N1 C1 Fe1 -36.1(16) . . . . ?
Fe2 N2 C2 Fe1 60.7(15) 3_675 . . . ?
N5 N4 C4 C5 -0.4(3) . . . . ?
Fe1 N4 C4 C5 179.78(17) . . . . ?
N4 C4 C5 C6 -0.2(3) . . . . ?
N4 C4 C5 C7 178.0(2) . . . . ?
N4 N5 C6 C5 -0.9(3) . . . . ?
B1 N5 C6 C5 -173.0(2) . . . . ?
C4 C5 C6 N5 0.7(3) . . . . ?
C7 C5 C6 N5 -177.5(2) . . . . ?
N7 N6 C8 C9 0.1(3) . . . . ?
Fe1 N6 C8 C9 -163.58(17) . . . . ?
N6 C8 C9 C10 0.3(3) . . . . ?
N6 C8 C9 C11 -178.3(2) . . . . ?
N6 N7 C10 C9 0.7(3) . . . . ?
B1 N7 C10 C9 166.7(2) . . . . ?
C8 C9 C10 N7 -0.6(3) . . . . ?
C11 C9 C10 N7 178.0(2) . . . . ?
N9 N8 C12 C13 1.4(3) . . . . ?
Fe1 N8 C12 C13 -169.90(19) . . . . ?
N8 C12 C13 C14 -1.3(3) . . . . ?
N8 C12 C13 C15 178.3(3) . . . . ?
N8 N9 C14 C13 0.1(3) . . . . ?
B1 N9 C14 C13 -175.4(3) . . . . ?
C12 C13 C14 N9 0.7(3) . . . . ?
C15 C13 C14 N9 -178.9(3) . . . . ?
C20 N10 C16 C17 1.2(4) . . . . ?
Fe2 N10 C16 C17 179.21(19) . . . . ?
N10 C16 C17 C18 1.1(4) . . . . ?
C16 C17 C18 C19 -1.9(4) . . . . ?
C17 C18 C19 C20 0.3(4) . . . . ?
C16 N10 C20 C19 -2.9(4) . . . . ?
Fe2 N10 C20 C19 178.9(2) . . . . ?
C16 N10 C20 C21 171.4(2) . . . . ?
Fe2 N10 C20 C21 -6.9(3) . . . . ?
C18 C19 C20 N10 2.1(4) . . . . ?
C18 C19 C20 C21 -171.7(3) . . . . ?
C28 N11 C21 C20 -148.1(2) . . . . ?
C22 N11 C21 C20 88.5(2) . . . . ?
Fe2 N11 C21 C20 -32.5(2) . . . . ?
N10 C20 C21 N11 26.7(3) . . . . ?
C19 C20 C21 N11 -159.1(2) . . . . ?
C21 N11 C22 C23 -107.1(2) . . . . ?
C28 N11 C22 C23 128.2(2) . . . . ?
Fe2 N11 C22 C23 12.6(2) . . . . ?
C27 N12 C23 C24 1.6(3) . . . . ?
Fe2 N12 C23 C24 -177.36(17) . . . . ?
C27 N12 C23 C22 -174.6(2) . . . . ?
Fe2 N12 C23 C22 6.4(3) . . . . ?
N11 C22 C23 N12 -12.6(3) . . . . ?
N11 C22 C23 C24 171.1(2) . . . . ?
N12 C23 C24 C25 -2.2(3) . . . . ?
C22 C23 C24 C25 173.8(2) . . . . ?
C23 C24 C25 C26 1.3(4) . . . . ?
C24 C25 C26 C27 0.2(4) . . . . ?
C23 N12 C27 C26 -0.1(3) . . . . ?
Fe2 N12 C27 C26 178.78(19) . . . . ?
C25 C26 C27 N12 -0.8(4) . . . . ?
C21 N11 C28 C29 159.1(2) . . . . ?
C22 N11 C28 C29 -76.3(2) . . . . ?
Fe2 N11 C28 C29 42.3(2) . . . . ?
C33 N13 C29 C30 0.9(4) . . . . ?
Fe2 N13 C29 C30 -178.6(2) . . . . ?
C33 N13 C29 C28 -178.1(2) . . . . ?
Fe2 N13 C29 C28 2.4(3) . . . . ?
N11 C28 C29 N13 -30.4(3) . . . . ?
N11 C28 C29 C30 150.7(2) . . . . ?
N13 C29 C30 C31 -0.5(4) . . . . ?
C28 C29 C30 C31 178.3(3) . . . . ?
C29 C30 C31 C32 -0.3(5) . . . . ?
C30 C31 C32 C33 0.6(5) . . . . ?
C29 N13 C33 C32 -0.5(4) . . . . ?
Fe2 N13 C33 C32 178.9(2) . . . . ?
C31 C32 C33 N13 -0.3(4) . . . . ?

loop_
_geom_hbond_atom_site_label_D
_geom_hbond_atom_site_label_H
_geom_hbond_atom_site_label_A
_geom_hbond_distance_DH
_geom_hbond_distance_HA
_geom_hbond_distance_DA
_geom_hbond_angle_DHA
_geom_hbond_site_symmetry_A
C10 H10 O2 0.93 2.42 3.189(10) 140.6 .
C10 H10 O2' 0.93 2.50 3.308(8) 144.8 .
C12 H12 O4 0.93 2.52 3.38(4) 153.0 2
C12 H12 O4' 0.93 2.47 3.33(3) 153.3 2
C16 H16 N1 0.93 2.69 3.175(3) 113.3 .
C17 H17 O3' 0.93 2.41 3.327(5) 167.7 1_554
C22 H22A O3' 0.97 2.65 3.484(4) 144.4 2_545
C24 H24 O1' 0.93 2.55 3.346(6) 144.2 2_545
C26 H26 N3 0.93 2.36 3.243(4) 158.7 3_575
C27 H27 N1 0.93 2.53 3.038(3) 114.8 .
C28 H28A O4' 0.97 2.54 3.22(2) 126.8 4_675

_refine_diff_density_max         0.605
_refine_diff_density_min         -0.478
_refine_diff_density_rms         0.074

####################################################################### 
# 
# 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_2-296K
_database_code_depnum_ccdc_archive 'CCDC 1419281'
_audit_update_record             
;
2016-09-02 deposited with the CCDC.
2016-09-26 downloaded from the CCDC.
;

_audit_creation_method           SHELXL-2014/7
_shelx_SHELXL_version_number     2014/7
_chemical_name_systematic        ?
_chemical_name_common            ?
_chemical_melting_point          ?
_chemical_formula_moiety         '(C66 H68 B2 Fe4 N26), 2(Cl O4)'
_chemical_formula_sum            'C66 H68 B2 Cl2 Fe4 N26 O8'
_chemical_formula_weight         1669.38

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'
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'
B B 0.0013 0.0007 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Cl Cl 0.1484 0.1585 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Fe Fe 0.3463 0.8444 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'

_space_group_crystal_system      monoclinic
_space_group_IT_number           14
_space_group_name_H-M_alt        'P 21/n'
_space_group_name_Hall           '-P 2yn'

_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.
;

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                   12.903(3)
_cell_length_b                   18.050(4)
_cell_length_c                   16.372(4)
_cell_angle_alpha                90
_cell_angle_beta                 98.360(4)
_cell_angle_gamma                90
_cell_volume                     3772.6(15)
_cell_formula_units_Z            2
_cell_measurement_temperature    296(2)
_cell_measurement_reflns_used    9648
_cell_measurement_theta_min      2.17
_cell_measurement_theta_max      25.50

_exptl_crystal_description       Block
_exptl_crystal_colour            Red
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    ?
_exptl_crystal_density_diffrn    1.470
_exptl_crystal_F_000             1716
_exptl_transmission_factor_min   ?
_exptl_transmission_factor_max   ?
_exptl_crystal_size_max          0.120
_exptl_crystal_size_mid          0.100
_exptl_crystal_size_min          0.100
_exptl_absorpt_coefficient_mu    0.896
_shelx_estimated_absorpt_T_min   0.900
_shelx_estimated_absorpt_T_max   0.916
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_correction_T_min  0.9001
_exptl_absorpt_correction_T_max  0.9157
_exptl_absorpt_process_details   sadabs
_exptl_absorpt_special_details   ?
_diffrn_ambient_temperature      296(2)
_diffrn_radiation_wavelength     0.71073
_diffrn_radiation_type           MoK\a
_diffrn_radiation_source         'fine-focus sealed tube'
_diffrn_radiation_monochromator  graphite
_diffrn_measurement_device_type  'Bruker APEX-II CCD'
_diffrn_measurement_method       'φ and ω scans'
_diffrn_detector_area_resol_mean ?
_diffrn_reflns_number            27664
_diffrn_reflns_av_unetI/netI     0.0545
_diffrn_reflns_av_R_equivalents  0.0619
_diffrn_reflns_limit_h_min       -15
_diffrn_reflns_limit_h_max       15
_diffrn_reflns_limit_k_min       -21
_diffrn_reflns_limit_k_max       21
_diffrn_reflns_limit_l_min       -19
_diffrn_reflns_limit_l_max       19
_diffrn_reflns_theta_min         1.689
_diffrn_reflns_theta_max         24.997
_diffrn_reflns_theta_full        24.997
_diffrn_measured_fraction_theta_max 0.994
_diffrn_measured_fraction_theta_full 0.994
_diffrn_reflns_Laue_measured_fraction_max 0.994
_diffrn_reflns_Laue_measured_fraction_full 0.994
_diffrn_reflns_point_group_measured_fraction_max 0.994
_diffrn_reflns_point_group_measured_fraction_full 0.994
_reflns_number_total             6611
_reflns_number_gt                5095
_reflns_threshold_expression     'I > 2σ(I)'
_reflns_Friedel_coverage         0.000
_reflns_Friedel_fraction_max     .
_reflns_Friedel_fraction_full    .

_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.
;
_computing_data_collection       'Bruker APEX2'
_computing_cell_refinement       'Bruker SAINT'
_computing_data_reduction        'Bruker SAINT'
_computing_structure_solution    'SHELXS-2014 (Sheldrick, 2014)'
_computing_structure_refinement  'SHELXL-2014/7 (Sheldrick, 2014)'
_computing_molecular_graphics    ?
_computing_publication_material  ?
_refine_special_details          ?
_refine_ls_structure_factor_coef Fsqd
_refine_ls_matrix_type           full
_refine_ls_weighting_scheme      calc
_refine_ls_weighting_details     
'w=1/[σ²(Fo²)+(0.0485P)²+14.7305P] where P=(Fo²+2Fc²)/3'
_atom_sites_solution_primary     ?
_atom_sites_solution_secondary   ?
_atom_sites_solution_hydrogens   mixed
_refine_ls_hydrogen_treatment    constr
_refine_ls_extinction_method     none
_refine_ls_extinction_coef       .
_refine_ls_number_reflns         6611
_refine_ls_number_parameters     535
_refine_ls_number_restraints     176
_refine_ls_R_factor_all          0.0812
_refine_ls_R_factor_gt           0.0612
_refine_ls_wR_factor_ref         0.1679
_refine_ls_wR_factor_gt          0.1530
_refine_ls_goodness_of_fit_ref   1.003
_refine_ls_restrained_S_all      1.026
_refine_ls_shift/su_max          0.005
_refine_ls_shift/su_mean         0.000

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 0.68479(6) -0.07410(4) 0.91384(4) 0.0374(2) Uani 1 1 d . . . . .
Fe2 Fe 0.64032(6) 0.18331(4) 1.00805(4) 0.0385(2) Uani 1 1 d . . . . .
B1 B 0.6814(5) -0.0771(3) 0.7248(4) 0.0462(14) Uani 1 1 d . . . . .
H1 H 0.6809 -0.0787 0.6649 0.055 Uiso 1 1 d R U . . .
N1 N 0.6820(4) 0.0789(3) 0.9955(3) 0.0524(11) Uani 1 1 d . . . . .
N2 N 0.5029(4) -0.1456(2) 0.9849(3) 0.0484(11) Uani 1 1 d . . . . .
N3 N 0.8305(5) -0.1415(4) 1.0593(4) 0.0870(19) Uani 1 1 d . . . . .
N4 N 0.5797(3) -0.0282(2) 0.8288(2) 0.0412(10) Uani 1 1 d . . . . .
N5 N 0.5901(4) -0.0316(2) 0.7481(2) 0.0450(10) Uani 1 1 d . . . . .
N6 N 0.7984(4) -0.0400(2) 0.8544(3) 0.0462(10) Uani 1 1 d . . . . .
N7 N 0.7846(4) -0.0458(2) 0.7704(3) 0.0476(11) Uani 1 1 d . . . . .
N8 N 0.6821(4) -0.1640(2) 0.8447(2) 0.0444(10) Uani 1 1 d . . . . .
N9 N 0.6714(4) -0.1552(2) 0.7613(3) 0.0475(11) Uani 1 1 d . . . . .
N10 N 0.6637(4) 0.1890(2) 1.1329(3) 0.0487(11) Uani 1 1 d . . . . .
N11 N 0.6037(4) 0.2947(2) 1.0207(3) 0.0501(11) Uani 1 1 d . . . . .
N12 N 0.7847(4) 0.2250(2) 1.0046(3) 0.0487(11) Uani 1 1 d . . . . .
N13 N 0.5955(4) 0.2100(3) 0.8868(3) 0.0540(12) Uani 1 1 d . . . . .
C1 C 0.6872(4) 0.0185(3) 0.9728(3) 0.0408(11) Uani 1 1 d . . . . .
C2 C 0.5746(4) -0.1159(3) 0.9651(3) 0.0403(11) Uani 1 1 d . . . . .
C3 C 0.7777(5) -0.1160(3) 1.0039(3) 0.0540(14) Uani 1 1 d . . . . .
C4 C 0.4915(4) 0.0097(3) 0.8338(3) 0.0457(12) Uani 1 1 d . . . . .
H4 H 0.4659 0.0204 0.8827 0.055 Uiso 1 1 calc R U . . .
C5 C 0.4437(5) 0.0305(3) 0.7559(4) 0.0554(15) Uani 1 1 d . . . . .
C6 C 0.5076(5) 0.0032(3) 0.7043(4) 0.0552(15) Uani 1 1 d . . . . .
H6 H 0.4962 0.0078 0.6471 0.066 Uiso 1 1 calc R U . . .
C7 C 0.3431(5) 0.0745(4) 0.7366(5) 0.083(2) Uani 1 1 d . . . . .
H7A H 0.3586 0.1231 0.7180 0.124 Uiso 1 1 calc R U . . .
H7B H 0.3103 0.0785 0.7854 0.124 Uiso 1 1 calc R U . . .
H7C H 0.2966 0.0497 0.6941 0.124 Uiso 1 1 calc R U . . .
C8 C 0.8984(4) -0.0232(3) 0.8777(4) 0.0544(14) Uani 1 1 d . . . . .
H8 H 0.9290 -0.0155 0.9321 0.065 Uiso 1 1 calc R U . . .
C9 C 0.9510(5) -0.0187(3) 0.8101(5) 0.0641(17) Uani 1 1 d . . . . .
C10 C 0.8758(5) -0.0333(3) 0.7441(4) 0.0555(15) Uani 1 1 d . . . . .
H10 H 0.8868 -0.0343 0.6892 0.067 Uiso 1 1 calc R U . . .
C11 C 1.0636(6) -0.0007(5) 0.8090(6) 0.100(3) Uani 1 1 d . . . . .
H11A H 1.0808 0.0445 0.8388 0.149 Uiso 1 1 calc R U . . .
H11B H 1.0760 0.0051 0.7530 0.149 Uiso 1 1 calc R U . . .
H11C H 1.1065 -0.0402 0.8346 0.149 Uiso 1 1 calc R U . . .
C12 C 0.6773(5) -0.2365(3) 0.8586(4) 0.0569(15) Uani 1 1 d . . . . .
H12 H 0.6836 -0.2580 0.9107 0.068 Uiso 1 1 calc R U . . .
C13 C 0.6615(6) -0.2756(3) 0.7854(4) 0.0697(19) Uani 1 1 d . . . . .
C14 C 0.6585(5) -0.2221(3) 0.7255(4) 0.0637(17) Uani 1 1 d . . . . .
H14 H 0.6491 -0.2309 0.6690 0.076 Uiso 1 1 calc R U . . .
C15 C 0.6477(8) -0.3586(3) 0.7730(6) 0.107(3) Uani 1 1 d . U . . .
H15A H 0.5859 -0.3745 0.7944 0.160 Uiso 1 1 calc R U . . .
H15B H 0.7076 -0.3839 0.8016 0.160 Uiso 1 1 calc R U . . .
H15C H 0.6408 -0.3699 0.7151 0.160 Uiso 1 1 calc R U . . .
C16 C 0.7066(5) 0.1368(3) 1.1849(4) 0.0643(16) Uani 1 1 d . . . . .
H16 H 0.7298 0.0932 1.1632 0.077 Uiso 1 1 calc R U . . .
C17 C 0.7180(7) 0.1448(5) 1.2696(4) 0.092(3) Uani 1 1 d . . . . .
H17 H 0.7451 0.1065 1.3043 0.110 Uiso 1 1 calc R U . . .
C18 C 0.6888(7) 0.2099(5) 1.3010(4) 0.095(3) Uani 1 1 d . . . . .
H18 H 0.6980 0.2173 1.3578 0.114 Uiso 1 1 calc R U . . .
C19 C 0.6456(6) 0.2646(4) 1.2489(4) 0.080(2) Uani 1 1 d . . . . .
H19 H 0.6252 0.3093 1.2699 0.096 Uiso 1 1 calc R U . . .
C20 C 0.6326(5) 0.2524(3) 1.1648(4) 0.0564(14) Uani 1 1 d . . . . .
C21 C 0.5732(6) 0.3036(4) 1.1035(4) 0.0723(19) Uani 1 1 d . . . . .
H21A H 0.4988 0.2939 1.1006 0.087 Uiso 1 1 calc R U . . .
H21B H 0.5859 0.3544 1.1217 0.087 Uiso 1 1 calc R U . . .
C22 C 0.6958(5) 0.3420(3) 1.0096(5) 0.0690(18) Uani 1 1 d . . . . .
H22A H 0.6805 0.3685 0.9577 0.083 Uiso 1 1 calc R U . . .
H22B H 0.7064 0.3783 1.0536 0.083 Uiso 1 1 calc R U . . .
C23 C 0.7931(5) 0.2995(3) 1.0097(3) 0.0510(13) Uani 1 1 d . . . . .
C24 C 0.8877(5) 0.3364(4) 1.0108(4) 0.0680(17) Uani 1 1 d . . . . .
H24 H 0.8918 0.3877 1.0145 0.082 Uiso 1 1 calc R U . . .
C25 C 0.9751(6) 0.2939(6) 1.0063(5) 0.093(3) Uani 1 1 d . . . . .
H25 H 1.0403 0.3163 1.0081 0.111 Uiso 1 1 calc R U . . .
C26 C 0.9658(7) 0.2184(6) 0.9991(5) 0.095(3) Uani 1 1 d . . . . .
H26 H 1.0244 0.1896 0.9942 0.114 Uiso 1 1 calc R U . . .
C27 C 0.8714(6) 0.1858(4) 0.9990(4) 0.0752(19) Uani 1 1 d . . . . .
H27 H 0.8666 0.1345 0.9948 0.090 Uiso 1 1 calc R U . . .
C28 C 0.5164(5) 0.3096(3) 0.9538(4) 0.0702(18) Uani 1 1 d . . . . .
H28A H 0.5087 0.3626 0.9451 0.084 Uiso 1 1 calc R U . . .
H28B H 0.4515 0.2906 0.9689 0.084 Uiso 1 1 calc R U . . .
C29 C 0.5384(5) 0.2733(3) 0.8767(4) 0.0639(17) Uani 1 1 d . . . . .
C30 C 0.5036(7) 0.3005(5) 0.7984(5) 0.098(3) Uani 1 1 d . . . . .
H30 H 0.4659 0.3445 0.7916 0.117 Uiso 1 1 calc R U . . .
C31 C 0.5254(8) 0.2616(6) 0.7312(5) 0.108(3) Uani 1 1 d . U . . .
H31 H 0.5014 0.2789 0.6783 0.130 Uiso 1 1 calc R U . . .
C32 C 0.5816(8) 0.1985(5) 0.7414(5) 0.104(3) Uani 1 1 d . . . . .
H32 H 0.5974 0.1722 0.6959 0.124 Uiso 1 1 calc R U . . .
C33 C 0.6151(6) 0.1735(4) 0.8197(4) 0.0684(18) Uani 1 1 d . . . . .
H33 H 0.6528 0.1295 0.8265 0.082 Uiso 1 1 calc R U . . .
Cl1 Cl 0.2552(7) 0.9365(5) 0.4909(5) 0.0918(19) Uani 0.5 1 d . U P A 1
O1 O 0.3159(14) 0.9348(10) 0.4268(10) 0.156(4) Uani 0.5 1 d . U P A 1
O2 O 0.1883(15) 0.9875(8) 0.4459(10) 0.128(4) Uani 0.5 1 d . U P A 1
O3 O 0.2906(16) 0.9767(9) 0.5665(9) 0.138(4) Uani 0.5 1 d . U P A 1
O4 O 0.2441(19) 0.8648(13) 0.5211(14) 0.111(4) Uani 0.5 1 d . U P A 1
Cl1' Cl 0.2165(8) 0.9460(5) 0.5130(5) 0.100(2) Uani 0.5 1 d . U P B 2
O1' O 0.3191(16) 0.9769(10) 0.5128(12) 0.149(4) Uani 0.5 1 d . U P B 2
O2' O 0.1336(14) 0.9614(9) 0.4538(10) 0.126(4) Uani 0.5 1 d . U P B 2
O3' O 0.1681(14) 0.9696(7) 0.5834(7) 0.131(4) Uani 0.5 1 d . U P B 2
O4' O 0.211(2) 0.8707(12) 0.5004(14) 0.115(4) Uani 0.5 1 d . U P B 2


_geom_special_details            
;
 All esds (except the esd in the dihedral angle between two l.s. planes)
 are estimated using the full covariance matrix.  The cell esds are taken
 into account individually in the estimation of esds in distances, angles
 and torsion angles; correlations between esds in cell parameters are only
 used when they are defined by crystal symmetry.  An approximate (isotropic)
 treatment of cell esds is used for estimating esds involving l.s. planes.
;

loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
_geom_bond_publ_flag
Fe1 C2 1.909(5) . ?
Fe1 C3 1.916(6) . ?
Fe1 C1 1.928(5) . ?
Fe1 N6 1.973(5) . ?
Fe1 N8 1.975(4) . ?
Fe1 N4 1.978(4) . ?
Fe2 N1 1.979(5) . ?
Fe2 N2 1.989(5) 3_657 ?
Fe2 N12 2.017(5) . ?
Fe2 N10 2.024(4) . ?
Fe2 N13 2.043(5) . ?
Fe2 N11 2.083(4) . ?
B1 N5 1.530(8) . ?
B1 N7 1.538(8) . ?
B1 N9 1.544(7) . ?
B1 H1 0.9800 . ?
N1 C1 1.157(6) . ?
N2 C2 1.155(6) . ?
N2 Fe2 1.989(5) 3_657 ?
N3 C3 1.149(7) . ?
N4 C4 1.341(6) . ?
N4 N5 1.349(5) . ?
N5 C6 1.349(7) . ?
N6 C8 1.327(7) . ?
N6 N7 1.364(6) . ?
N7 C10 1.330(7) . ?
N8 C12 1.332(6) . ?
N8 N9 1.362(6) . ?
N9 C14 1.341(7) . ?
N10 C16 1.336(7) . ?
N10 C20 1.343(7) . ?
N11 C21 1.474(8) . ?
N11 C28 1.477(8) . ?
N11 C22 1.496(8) . ?
N12 C27 1.338(8) . ?
N12 C23 1.351(7) . ?
N13 C33 1.336(7) . ?
N13 C29 1.355(8) . ?
C4 C5 1.385(7) . ?
C4 H4 0.9300 . ?
C5 C6 1.356(8) . ?
C5 C7 1.515(8) . ?
C6 H6 0.9300 . ?
C7 H7A 0.9600 . ?
C7 H7B 0.9600 . ?
C7 H7C 0.9600 . ?
C8 C9 1.382(9) . ?
C8 H8 0.9300 . ?
C9 C10 1.369(9) . ?
C9 C11 1.492(9) . ?
C10 H10 0.9300 . ?
C11 H11A 0.9600 . ?
C11 H11B 0.9600 . ?
C11 H11C 0.9600 . ?
C12 C13 1.380(8) . ?
C12 H12 0.9300 . ?
C13 C14 1.372(9) . ?
C13 C15 1.520(8) . ?
C14 H14 0.9300 . ?
C15 H15A 0.9600 . ?
C15 H15B 0.9600 . ?
C15 H15C 0.9600 . ?
C16 C17 1.380(9) . ?
C16 H16 0.9300 . ?
C17 C18 1.358(12) . ?
C17 H17 0.9300 . ?
C18 C19 1.370(11) . ?
C18 H18 0.9300 . ?
C19 C20 1.381(8) . ?
C19 H19 0.9300 . ?
C20 C21 1.492(9) . ?
C21 H21A 0.9700 . ?
C21 H21B 0.9700 . ?
C22 C23 1.471(9) . ?
C22 H22A 0.9700 . ?
C22 H22B 0.9700 . ?
C23 C24 1.388(8) . ?
C24 C25 1.374(11) . ?
C24 H24 0.9300 . ?
C25 C26 1.373(12) . ?
C25 H25 0.9300 . ?
C26 C27 1.353(11) . ?
C26 H26 0.9300 . ?
C27 H27 0.9300 . ?
C28 C29 1.486(10) . ?
C28 H28A 0.9700 . ?
C28 H28B 0.9700 . ?
C29 C30 1.386(9) . ?
C30 C31 1.367(13) . ?
C30 H30 0.9300 . ?
C31 C32 1.349(13) . ?
C31 H31 0.9300 . ?
C32 C33 1.368(10) . ?
C32 H32 0.9300 . ?
C33 H33 0.9300 . ?
Cl1 O2 1.395(18) . ?
Cl1 O1 1.398(18) . ?
Cl1 O4 1.40(2) . ?
Cl1 O3 1.450(16) . ?
Cl1' O2' 1.363(17) . ?
Cl1' O4' 1.38(2) . ?
Cl1' O1' 1.44(2) . ?
Cl1' O3' 1.453(16) . ?

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
C2 Fe1 C3 85.9(2) . . ?
C2 Fe1 C1 94.7(2) . . ?
C3 Fe1 C1 89.7(2) . . ?
C2 Fe1 N6 174.35(19) . . ?
C3 Fe1 N6 94.4(2) . . ?
C1 Fe1 N6 90.97(19) . . ?
C2 Fe1 N8 88.60(19) . . ?
C3 Fe1 N8 94.2(2) . . ?
C1 Fe1 N8 175.08(19) . . ?
N6 Fe1 N8 85.75(17) . . ?
C2 Fe1 N4 89.81(19) . . ?
C3 Fe1 N4 174.4(2) . . ?
C1 Fe1 N4 87.06(18) . . ?
N6 Fe1 N4 90.28(18) . . ?
N8 Fe1 N4 89.29(17) . . ?
N1 Fe2 N2 87.05(18) . 3_657 ?
N1 Fe2 N12 94.96(19) . . ?
N2 Fe2 N12 177.49(18) 3_657 . ?
N1 Fe2 N10 98.65(18) . . ?
N2 Fe2 N10 87.84(18) 3_657 . ?
N12 Fe2 N10 90.36(17) . . ?
N1 Fe2 N13 99.60(19) . . ?
N2 Fe2 N13 90.19(18) 3_657 . ?
N12 Fe2 N13 90.96(18) . . ?
N10 Fe2 N13 161.52(19) . . ?
N1 Fe2 N11 177.29(19) . . ?
N2 Fe2 N11 95.66(18) 3_657 . ?
N12 Fe2 N11 82.34(18) . . ?
N10 Fe2 N11 81.57(18) . . ?
N13 Fe2 N11 80.34(19) . . ?
N5 B1 N7 108.9(4) . . ?
N5 B1 N9 106.5(4) . . ?
N7 B1 N9 105.3(4) . . ?
N5 B1 H1 111.8 . . ?
N7 B1 H1 112.0 . . ?
N9 B1 H1 111.9 . . ?
C1 N1 Fe2 163.8(4) . . ?
C2 N2 Fe2 164.6(4) . 3_657 ?
C4 N4 N5 106.8(4) . . ?
C4 N4 Fe1 132.3(4) . . ?
N5 N4 Fe1 121.0(3) . . ?
C6 N5 N4 108.5(5) . . ?
C6 N5 B1 134.0(5) . . ?
N4 N5 B1 117.3(4) . . ?
C8 N6 N7 106.6(5) . . ?
C8 N6 Fe1 133.7(4) . . ?
N7 N6 Fe1 118.4(3) . . ?
C10 N7 N6 108.8(5) . . ?
C10 N7 B1 130.5(5) . . ?
N6 N7 B1 119.6(4) . . ?
C12 N8 N9 106.5(4) . . ?
C12 N8 Fe1 135.0(4) . . ?
N9 N8 Fe1 118.1(3) . . ?
C14 N9 N8 108.8(4) . . ?
C14 N9 B1 131.7(5) . . ?
N8 N9 B1 119.4(4) . . ?
C16 N10 C20 118.2(5) . . ?
C16 N10 Fe2 126.5(4) . . ?
C20 N10 Fe2 115.3(4) . . ?
C21 N11 C28 112.6(5) . . ?
C21 N11 C22 111.9(5) . . ?
C28 N11 C22 109.9(5) . . ?
C21 N11 Fe2 106.9(3) . . ?
C28 N11 Fe2 105.2(4) . . ?
C22 N11 Fe2 110.0(3) . . ?
C27 N12 C23 118.0(6) . . ?
C27 N12 Fe2 126.1(5) . . ?
C23 N12 Fe2 115.9(4) . . ?
C33 N13 C29 118.7(6) . . ?
C33 N13 Fe2 128.4(5) . . ?
C29 N13 Fe2 112.9(4) . . ?
N1 C1 Fe1 168.6(4) . . ?
N2 C2 Fe1 169.9(5) . . ?
N3 C3 Fe1 177.6(6) . . ?
N4 C4 C5 110.6(5) . . ?
N4 C4 H4 124.7 . . ?
C5 C4 H4 124.7 . . ?
C6 C5 C4 104.2(5) . . ?
C6 C5 C7 129.8(6) . . ?
C4 C5 C7 126.0(6) . . ?
N5 C6 C5 110.0(5) . . ?
N5 C6 H6 125.0 . . ?
C5 C6 H6 125.0 . . ?
C5 C7 H7A 109.5 . . ?
C5 C7 H7B 109.5 . . ?
H7A C7 H7B 109.5 . . ?
C5 C7 H7C 109.5 . . ?
H7A C7 H7C 109.5 . . ?
H7B C7 H7C 109.5 . . ?
N6 C8 C9 110.7(6) . . ?
N6 C8 H8 124.7 . . ?
C9 C8 H8 124.7 . . ?
C10 C9 C8 104.3(5) . . ?
C10 C9 C11 127.8(7) . . ?
C8 C9 C11 127.9(7) . . ?
N7 C10 C9 109.6(6) . . ?
N7 C10 H10 125.2 . . ?
C9 C10 H10 125.2 . . ?
C9 C11 H11A 109.5 . . ?
C9 C11 H11B 109.5 . . ?
H11A C11 H11B 109.5 . . ?
C9 C11 H11C 109.5 . . ?
H11A C11 H11C 109.5 . . ?
H11B C11 H11C 109.5 . . ?
N8 C12 C13 111.0(5) . . ?
N8 C12 H12 124.5 . . ?
C13 C12 H12 124.5 . . ?
C14 C13 C12 104.2(5) . . ?
C14 C13 C15 127.4(6) . . ?
C12 C13 C15 128.3(6) . . ?
N9 C14 C13 109.5(5) . . ?
N9 C14 H14 125.3 . . ?
C13 C14 H14 125.3 . . ?
C13 C15 H15A 109.5 . . ?
C13 C15 H15B 109.5 . . ?
H15A C15 H15B 109.5 . . ?
C13 C15 H15C 109.5 . . ?
H15A C15 H15C 109.5 . . ?
H15B C15 H15C 109.5 . . ?
N10 C16 C17 122.7(7) . . ?
N10 C16 H16 118.6 . . ?
C17 C16 H16 118.6 . . ?
C18 C17 C16 118.4(7) . . ?
C18 C17 H17 120.8 . . ?
C16 C17 H17 120.8 . . ?
C17 C18 C19 119.8(7) . . ?
C17 C18 H18 120.1 . . ?
C19 C18 H18 120.1 . . ?
C18 C19 C20 119.1(7) . . ?
C18 C19 H19 120.4 . . ?
C20 C19 H19 120.4 . . ?
N10 C20 C19 121.6(6) . . ?
N10 C20 C21 114.8(5) . . ?
C19 C20 C21 123.2(6) . . ?
N11 C21 C20 111.8(5) . . ?
N11 C21 H21A 109.3 . . ?
C20 C21 H21A 109.3 . . ?
N11 C21 H21B 109.3 . . ?
C20 C21 H21B 109.3 . . ?
H21A C21 H21B 107.9 . . ?
C23 C22 N11 113.3(5) . . ?
C23 C22 H22A 108.9 . . ?
N11 C22 H22A 108.9 . . ?
C23 C22 H22B 108.9 . . ?
N11 C22 H22B 108.9 . . ?
H22A C22 H22B 107.7 . . ?
N12 C23 C24 122.8(6) . . ?
N12 C23 C22 117.2(5) . . ?
C24 C23 C22 119.9(6) . . ?
C25 C24 C23 117.3(7) . . ?
C25 C24 H24 121.3 . . ?
C23 C24 H24 121.3 . . ?
C26 C25 C24 119.7(8) . . ?
C26 C25 H25 120.1 . . ?
C24 C25 H25 120.1 . . ?
C27 C26 C25 120.0(8) . . ?
C27 C26 H26 120.0 . . ?
C25 C26 H26 120.0 . . ?
N12 C27 C26 122.1(8) . . ?
N12 C27 H27 118.9 . . ?
C26 C27 H27 118.9 . . ?
N11 C28 C29 109.2(5) . . ?
N11 C28 H28A 109.8 . . ?
C29 C28 H28A 109.8 . . ?
N11 C28 H28B 109.8 . . ?
C29 C28 H28B 109.8 . . ?
H28A C28 H28B 108.3 . . ?
N13 C29 C30 120.5(7) . . ?
N13 C29 C28 115.9(5) . . ?
C30 C29 C28 123.6(7) . . ?
C31 C30 C29 119.1(8) . . ?
C31 C30 H30 120.5 . . ?
C29 C30 H30 120.5 . . ?
C32 C31 C30 120.2(8) . . ?
C32 C31 H31 119.9 . . ?
C30 C31 H31 119.9 . . ?
C31 C32 C33 119.1(9) . . ?
C31 C32 H32 120.5 . . ?
C33 C32 H32 120.5 . . ?
N13 C33 C32 122.4(8) . . ?
N13 C33 H33 118.8 . . ?
C32 C33 H33 118.8 . . ?
O2 Cl1 O1 89.4(11) . . ?
O2 Cl1 O4 135.2(13) . . ?
O1 Cl1 O4 110.0(15) . . ?
O2 Cl1 O3 102.4(11) . . ?
O1 Cl1 O3 120.6(13) . . ?
O4 Cl1 O3 101.3(13) . . ?
O2' Cl1' O4' 94.6(12) . . ?
O2' Cl1' O1' 123.2(12) . . ?
O4' Cl1' O1' 113.9(15) . . ?
O2' Cl1' O3' 97.0(12) . . ?
O4' Cl1' O3' 113.1(15) . . ?
O1' Cl1' O3' 113.0(11) . . ?

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
C4 N4 N5 C6 -0.9(5) . . . . ?
Fe1 N4 N5 C6 179.4(3) . . . . ?
C4 N4 N5 B1 -175.7(4) . . . . ?
Fe1 N4 N5 B1 4.6(6) . . . . ?
N7 B1 N5 C6 128.4(6) . . . . ?
N9 B1 N5 C6 -118.5(6) . . . . ?
N7 B1 N5 N4 -58.5(5) . . . . ?
N9 B1 N5 N4 54.6(6) . . . . ?
C8 N6 N7 C10 0.6(5) . . . . ?
Fe1 N6 N7 C10 -168.4(3) . . . . ?
C8 N6 N7 B1 170.0(4) . . . . ?
Fe1 N6 N7 B1 1.0(6) . . . . ?
N5 B1 N7 C10 -137.3(5) . . . . ?
N9 B1 N7 C10 108.8(6) . . . . ?
N5 B1 N7 N6 55.9(6) . . . . ?
N9 B1 N7 N6 -58.0(6) . . . . ?
C12 N8 N9 C14 1.0(6) . . . . ?
Fe1 N8 N9 C14 -172.5(4) . . . . ?
C12 N8 N9 B1 -175.8(5) . . . . ?
Fe1 N8 N9 B1 10.7(6) . . . . ?
N5 B1 N9 C14 119.5(6) . . . . ?
N7 B1 N9 C14 -124.9(6) . . . . ?
N5 B1 N9 N8 -64.6(6) . . . . ?
N7 B1 N9 N8 51.0(6) . . . . ?
Fe2 N1 C1 Fe1 28(4) . . . . ?
Fe2 N2 C2 Fe1 -50(3) 3_657 . . . ?
N5 N4 C4 C5 0.5(6) . . . . ?
Fe1 N4 C4 C5 -179.8(4) . . . . ?
N4 C4 C5 C6 0.1(6) . . . . ?
N4 C4 C5 C7 -179.5(6) . . . . ?
N4 N5 C6 C5 1.0(6) . . . . ?
B1 N5 C6 C5 174.5(5) . . . . ?
C4 C5 C6 N5 -0.6(6) . . . . ?
C7 C5 C6 N5 178.9(6) . . . . ?
N7 N6 C8 C9 -0.7(6) . . . . ?
Fe1 N6 C8 C9 165.9(4) . . . . ?
N6 C8 C9 C10 0.5(6) . . . . ?
N6 C8 C9 C11 179.5(6) . . . . ?
N6 N7 C10 C9 -0.3(6) . . . . ?
B1 N7 C10 C9 -168.2(5) . . . . ?
C8 C9 C10 N7 -0.1(6) . . . . ?
C11 C9 C10 N7 -179.1(6) . . . . ?
N9 N8 C12 C13 -1.1(7) . . . . ?
Fe1 N8 C12 C13 170.8(5) . . . . ?
N8 C12 C13 C14 0.8(8) . . . . ?
N8 C12 C13 C15 -177.7(7) . . . . ?
N8 N9 C14 C13 -0.5(7) . . . . ?
B1 N9 C14 C13 175.7(6) . . . . ?
C12 C13 C14 N9 -0.2(8) . . . . ?
C15 C13 C14 N9 178.4(7) . . . . ?
C20 N10 C16 C17 1.5(9) . . . . ?
Fe2 N10 C16 C17 -178.8(5) . . . . ?
N10 C16 C17 C18 -3.1(12) . . . . ?
C16 C17 C18 C19 2.3(13) . . . . ?
C17 C18 C19 C20 -0.1(13) . . . . ?
C16 N10 C20 C19 1.0(9) . . . . ?
Fe2 N10 C20 C19 -178.7(5) . . . . ?
C16 N10 C20 C21 -172.4(6) . . . . ?
Fe2 N10 C20 C21 7.9(7) . . . . ?
C18 C19 C20 N10 -1.7(11) . . . . ?
C18 C19 C20 C21 171.1(7) . . . . ?
C28 N11 C21 C20 148.5(5) . . . . ?
C22 N11 C21 C20 -87.1(6) . . . . ?
Fe2 N11 C21 C20 33.4(6) . . . . ?
N10 C20 C21 N11 -28.5(8) . . . . ?
C19 C20 C21 N11 158.3(6) . . . . ?
C21 N11 C22 C23 107.1(6) . . . . ?
C28 N11 C22 C23 -127.0(6) . . . . ?
Fe2 N11 C22 C23 -11.6(6) . . . . ?
C27 N12 C23 C24 -1.3(8) . . . . ?
Fe2 N12 C23 C24 177.9(4) . . . . ?
C27 N12 C23 C22 175.5(5) . . . . ?
Fe2 N12 C23 C22 -5.3(6) . . . . ?
N11 C22 C23 N12 11.5(8) . . . . ?
N11 C22 C23 C24 -171.6(5) . . . . ?
N12 C23 C24 C25 0.2(9) . . . . ?
C22 C23 C24 C25 -176.5(6) . . . . ?
C23 C24 C25 C26 1.4(11) . . . . ?
C24 C25 C26 C27 -2.0(13) . . . . ?
C23 N12 C27 C26 0.7(9) . . . . ?
Fe2 N12 C27 C26 -178.4(6) . . . . ?
C25 C26 C27 N12 0.9(12) . . . . ?
C21 N11 C28 C29 -158.7(5) . . . . ?
C22 N11 C28 C29 75.9(6) . . . . ?
Fe2 N11 C28 C29 -42.5(5) . . . . ?
C33 N13 C29 C30 -1.8(9) . . . . ?
Fe2 N13 C29 C30 178.5(5) . . . . ?
C33 N13 C29 C28 177.9(5) . . . . ?
Fe2 N13 C29 C28 -1.8(7) . . . . ?
N11 C28 C29 N13 30.8(7) . . . . ?
N11 C28 C29 C30 -149.6(6) . . . . ?
N13 C29 C30 C31 1.6(11) . . . . ?
C28 C29 C30 C31 -178.0(8) . . . . ?
C29 C30 C31 C32 -1.1(14) . . . . ?
C30 C31 C32 C33 0.8(14) . . . . ?
C29 N13 C33 C32 1.5(9) . . . . ?
Fe2 N13 C33 C32 -178.9(5) . . . . ?
C31 C32 C33 N13 -1.1(12) . . . . ?

_refine_diff_density_max         1.001
_refine_diff_density_min         -0.465
_refine_diff_density_rms         0.075

####################################################################### 
# 
# 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_2-400K
# Added during the CSD deposition process: Friday 02 September 2016 02:49 AM
# end Validation Reply Form

_database_code_depnum_ccdc_archive 'CCDC 1419282'
_audit_update_record             
;
2016-09-02 deposited with the CCDC.
2016-09-26 downloaded from the CCDC.
;
# start Validation Reply Form
_vrf_PLAT230_2-400K              
;
PROBLEM: Hirshfeld Test Diff for    C20    --  C21     ..        7.1 s.u.
RESPONSE: Due to the high temperature, 400K.
;

_audit_creation_method           SHELXL-2014/7
_shelx_SHELXL_version_number     2014/7
_chemical_name_systematic        ?
_chemical_name_common            ?
_chemical_melting_point          ?
_chemical_formula_moiety         '(C66 H68 B2 Fe4 N26), 2(Cl O4) '
_chemical_formula_sum            'C66 H68 B2 Cl2 Fe4 N26 O8'
_chemical_formula_weight         1669.38

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'
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'
B B 0.0013 0.0007 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Cl Cl 0.1484 0.1585 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Fe Fe 0.3463 0.8444 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'

_space_group_crystal_system      monoclinic
_space_group_IT_number           14
_space_group_name_H-M_alt        'P 21/n'
_space_group_name_Hall           '-P 2yn'

_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.
;

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                   12.800(7)
_cell_length_b                   18.280(10)
_cell_length_c                   16.560(9)
_cell_angle_alpha                90
_cell_angle_beta                 98.274(8)
_cell_angle_gamma                90
_cell_volume                     3834(4)
_cell_formula_units_Z            2
_cell_measurement_temperature    400(2)
_cell_measurement_reflns_used    3586
_cell_measurement_theta_min      2.44
_cell_measurement_theta_max      21.27

_exptl_crystal_description       Block
_exptl_crystal_colour            Red
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    ?
_exptl_crystal_density_diffrn    1.446
_exptl_crystal_F_000             1716
_exptl_transmission_factor_min   ?
_exptl_transmission_factor_max   ?
_exptl_crystal_size_max          0.150
_exptl_crystal_size_mid          0.100
_exptl_crystal_size_min          0.100
_exptl_absorpt_coefficient_mu    0.881
_shelx_estimated_absorpt_T_min   0.879
_shelx_estimated_absorpt_T_max   0.917
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_correction_T_min  0.8791
_exptl_absorpt_correction_T_max  0.9170
_exptl_absorpt_process_details   sadabs
_exptl_absorpt_special_details   ?
_diffrn_ambient_temperature      400(2)
_diffrn_radiation_wavelength     0.71073
_diffrn_radiation_type           MoK\a
_diffrn_radiation_source         'fine-focus sealed tube'
_diffrn_radiation_monochromator  graphite
_diffrn_measurement_device_type  'CCD area detector'
_diffrn_measurement_method       'phi and omega scans'
_diffrn_detector_area_resol_mean ?
_diffrn_reflns_number            23440
_diffrn_reflns_av_unetI/netI     0.0969
_diffrn_reflns_av_R_equivalents  0.0940
_diffrn_reflns_limit_h_min       -15
_diffrn_reflns_limit_h_max       15
_diffrn_reflns_limit_k_min       -21
_diffrn_reflns_limit_k_max       14
_diffrn_reflns_limit_l_min       -18
_diffrn_reflns_limit_l_max       19
_diffrn_reflns_theta_min         1.669
_diffrn_reflns_theta_max         24.999
_diffrn_reflns_theta_full        24.999
_diffrn_measured_fraction_theta_max 0.995
_diffrn_measured_fraction_theta_full 0.995
_diffrn_reflns_Laue_measured_fraction_max 0.995
_diffrn_reflns_Laue_measured_fraction_full 0.995
_diffrn_reflns_point_group_measured_fraction_max 0.995
_diffrn_reflns_point_group_measured_fraction_full 0.995
_reflns_number_total             6726
_reflns_number_gt                3623
_reflns_threshold_expression     'I > 2σ(I)'
_reflns_Friedel_coverage         0.000
_reflns_Friedel_fraction_max     .
_reflns_Friedel_fraction_full    .

_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.
;

_computing_data_collection       'Bruker SMART'
_computing_cell_refinement       'Bruker SMART'
_computing_data_reduction        'Bruker SAINT'
_computing_structure_solution    'SHELXS-2014 (Sheldrick, 2014)'
_computing_structure_refinement  'SHELXL-2014/7 (Sheldrick, 2014)'
_computing_molecular_graphics    ?
_computing_publication_material  ?
_refine_special_details          ?
_refine_ls_structure_factor_coef Fsqd
_refine_ls_matrix_type           full
_refine_ls_weighting_scheme      calc
_refine_ls_weighting_details     
'w=1/[σ²(Fo²)+(0.1041P)²] where P=(Fo²+2Fc²)/3'
_atom_sites_solution_primary     ?
_atom_sites_solution_secondary   ?
_atom_sites_solution_hydrogens   mixed
_refine_ls_hydrogen_treatment    constr
_refine_ls_extinction_method     none
_refine_ls_extinction_coef       .
_refine_ls_number_reflns         6726
_refine_ls_number_parameters     535
_refine_ls_number_restraints     68
_refine_ls_R_factor_all          0.1242
_refine_ls_R_factor_gt           0.0596
_refine_ls_wR_factor_ref         0.2039
_refine_ls_wR_factor_gt          0.1529
_refine_ls_goodness_of_fit_ref   1.002
_refine_ls_restrained_S_all      1.022
_refine_ls_shift/su_max          0.001
_refine_ls_shift/su_mean         0.000

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 0.30573(6) 1.07088(4) 0.09002(4) 0.0564(3) Uani 1 1 d . . . . .
Fe2 Fe 0.36254(6) 0.81753(4) -0.00711(5) 0.0641(3) Uani 1 1 d . . . . .
B1 B 0.3149(6) 1.0768(3) 0.2770(4) 0.0678(17) Uani 1 1 d . . . . .
H1 H 0.3150 1.0780 0.3369 0.081 Uiso 1 1 d R U . . .
N1 N 0.3052(4) 0.9229(2) 0.0035(3) 0.0736(12) Uani 1 1 d . . . . .
N2 N 0.4839(4) 1.1388(3) 0.0094(3) 0.0786(14) Uani 1 1 d . . . . .
N3 N 0.1492(6) 1.1303(4) -0.0524(4) 0.134(3) Uani 1 1 d . . . . .
N4 N 0.4142(3) 1.0275(2) 0.1725(3) 0.0617(11) Uani 1 1 d . . . . .
N5 N 0.4065(4) 1.0324(2) 0.2530(3) 0.0661(11) Uani 1 1 d . . . . .
N6 N 0.1937(3) 1.0378(2) 0.1534(3) 0.0640(11) Uani 1 1 d . . . . .
N7 N 0.2113(4) 1.0442(2) 0.2350(3) 0.0624(11) Uani 1 1 d . . . . .
N8 N 0.3111(4) 1.1606(2) 0.1570(3) 0.0660(11) Uani 1 1 d . . . . .
N9 N 0.3224(4) 1.1537(2) 0.2393(3) 0.0687(12) Uani 1 1 d . . . . .
N10 N 0.3467(4) 0.8041(3) -0.1371(3) 0.0761(13) Uani 1 1 d . . . . .
N11 N 0.4003(4) 0.7002(3) -0.0214(3) 0.0803(14) Uani 1 1 d . . . . .
N12 N 0.2101(4) 0.7655(3) -0.0051(3) 0.0715(12) Uani 1 1 d . . . . .
N13 N 0.4148(4) 0.7824(3) 0.1161(3) 0.0807(14) Uani 1 1 d . . . . .
C1 C 0.3032(4) 0.9804(3) 0.0310(3) 0.0611(13) Uani 1 1 d . . . . .
C2 C 0.4156(5) 1.1112(3) 0.0342(3) 0.0663(14) Uani 1 1 d . . . . .
C3 C 0.2081(5) 1.1097(3) 0.0025(4) 0.0830(17) Uani 1 1 d . . . . .
C4 C 0.5046(4) 0.9899(3) 0.1677(4) 0.0707(15) Uani 1 1 d . . . . .
H4 H 0.5291 0.9789 0.1189 0.085 Uiso 1 1 calc R U . . .
C5 C 0.5546(5) 0.9705(3) 0.2414(4) 0.0780(17) Uani 1 1 d . . . . .
C6 C 0.4886(5) 0.9984(3) 0.2951(4) 0.0826(17) Uani 1 1 d . . . . .
H6 H 0.5007 0.9937 0.3516 0.099 Uiso 1 1 calc R U . . .
C7 C 0.6544(5) 0.9286(4) 0.2616(6) 0.128(3) Uani 1 1 d . . . . .
H7A H 0.6826 0.9363 0.3179 0.193 Uiso 1 1 calc R U . . .
H7B H 0.7046 0.9449 0.2277 0.193 Uiso 1 1 calc R U . . .
H7C H 0.6406 0.8774 0.2524 0.193 Uiso 1 1 calc R U . . .
C8 C 0.0941(5) 1.0191(3) 0.1317(4) 0.0755(16) Uani 1 1 d . . . . .
H8 H 0.0622 1.0106 0.0785 0.091 Uiso 1 1 calc R U . . .
C9 C 0.0431(5) 1.0140(3) 0.2023(5) 0.0833(18) Uani 1 1 d . . . . .
C10 C 0.1202(5) 1.0304(3) 0.2637(4) 0.0769(16) Uani 1 1 d . . . . .
H10 H 0.1117 1.0321 0.3185 0.092 Uiso 1 1 calc R U . . .
C11 C -0.0687(6) 0.9954(5) 0.2063(6) 0.134(3) Uani 1 1 d . . . . .
H11A H -0.0818 0.9985 0.2619 0.201 Uiso 1 1 calc R U . . .
H11B H -0.0828 0.9465 0.1865 0.201 Uiso 1 1 calc R U . . .
H11C H -0.1138 1.0291 0.1733 0.201 Uiso 1 1 calc R U . . .
C12 C 0.3121(6) 1.2319(3) 0.1408(4) 0.0849(19) Uani 1 1 d . . . . .
H12 H 0.3052 1.2523 0.0889 0.102 Uiso 1 1 calc R U . . .
C13 C 0.3250(6) 1.2714(3) 0.2139(4) 0.099(2) Uani 1 1 d . . . . .
C14 C 0.3299(6) 1.2202(4) 0.2721(4) 0.090(2) Uani 1 1 d . . . . .
H14 H 0.3374 1.2298 0.3277 0.108 Uiso 1 1 calc R U . . .
C15 C 0.3332(8) 1.3529(4) 0.2242(6) 0.147(4) Uani 1 1 d . U . . .
H15A H 0.2777 1.3761 0.1880 0.220 Uiso 1 1 calc R U . . .
H15B H 0.4004 1.3692 0.2117 0.220 Uiso 1 1 calc R U . . .
H15C H 0.3268 1.3656 0.2796 0.220 Uiso 1 1 calc R U . . .
C16 C 0.3101(6) 0.8563(4) -0.1894(4) 0.097(2) Uani 1 1 d . . . . .
H16 H 0.2894 0.9009 -0.1697 0.117 Uiso 1 1 calc R U . . .
C17 C 0.3020(7) 0.8450(6) -0.2750(6) 0.130(3) Uani 1 1 d . . . . .
H17 H 0.2784 0.8824 -0.3112 0.156 Uiso 1 1 calc R U . . .
C18 C 0.3289(8) 0.7796(6) -0.3031(6) 0.133(3) Uani 1 1 d . . . . .
H18 H 0.3216 0.7697 -0.3587 0.160 Uiso 1 1 calc R U . . .
C19 C 0.3677(7) 0.7277(5) -0.2460(6) 0.122(3) Uani 1 1 d . . . . .
H19 H 0.3875 0.6820 -0.2631 0.147 Uiso 1 1 calc R U . . .
C20 C 0.3773(6) 0.7428(4) -0.1655(4) 0.0874(18) Uani 1 1 d . . . . .
C21 C 0.4341(7) 0.6904(4) -0.1022(5) 0.128(3) Uani 1 1 d . . . . .
H21A H 0.4200 0.6404 -0.1204 0.153 Uiso 1 1 calc R U . . .
H21B H 0.5096 0.6985 -0.0976 0.153 Uiso 1 1 calc R U . . .
C22 C 0.3103(5) 0.6537(4) -0.0074(5) 0.109(2) Uani 1 1 d . . . . .
H22A H 0.3271 0.6301 0.0454 0.131 Uiso 1 1 calc R U . . .
H22B H 0.3012 0.6155 -0.0485 0.131 Uiso 1 1 calc R U . . .
C23 C 0.2085(5) 0.6936(3) -0.0095(3) 0.0747(16) Uani 1 1 d . . . . .
C24 C 0.1183(6) 0.6526(4) -0.0110(4) 0.095(2) Uani 1 1 d . . . . .
H24 H 0.1210 0.6018 -0.0131 0.114 Uiso 1 1 calc R U . . .
C25 C 0.0255(7) 0.6873(6) -0.0092(6) 0.132(3) Uani 1 1 d . . . . .
H25 H -0.0371 0.6609 -0.0123 0.159 Uiso 1 1 calc R U . . .
C26 C 0.0253(7) 0.7614(6) -0.0028(7) 0.150(4) Uani 1 1 d . . . . .
H26 H -0.0375 0.7862 0.0002 0.180 Uiso 1 1 calc R U . . .
C27 C 0.1187(7) 0.7999(5) -0.0006(4) 0.109(2) Uani 1 1 d . . . . .
H27 H 0.1181 0.8506 0.0040 0.130 Uiso 1 1 calc R U . . .
C28 C 0.4895(5) 0.6851(4) 0.0416(5) 0.101(2) Uani 1 1 d . . . . .
H28A H 0.5535 0.7050 0.0253 0.121 Uiso 1 1 calc R U . . .
H28B H 0.4984 0.6327 0.0484 0.121 Uiso 1 1 calc R U . . .
C29 C 0.4708(6) 0.7187(4) 0.1201(5) 0.099(2) Uani 1 1 d . . . . .
C30 C 0.5134(9) 0.6900(6) 0.1949(7) 0.155(4) Uani 1 1 d . . . . .
H30 H 0.5553 0.6482 0.1986 0.186 Uiso 1 1 calc R U . . .
C31 C 0.4917(11) 0.7250(8) 0.2626(7) 0.189(6) Uani 1 1 d . . . . .
H31 H 0.5132 0.7039 0.3134 0.226 Uiso 1 1 calc R U . . .
C32 C 0.4387(9) 0.7912(7) 0.2588(5) 0.147(4) Uani 1 1 d . . . . .
H32 H 0.4296 0.8165 0.3060 0.176 Uiso 1 1 calc R U . . .
C33 C 0.4013(6) 0.8175(4) 0.1853(5) 0.096(2) Uani 1 1 d . . . . .
H33 H 0.3647 0.8616 0.1817 0.116 Uiso 1 1 calc R U . . .
Cl1 Cl 0.2423(10) 0.9367(9) 0.5010(7) 0.110(3) Uani 0.5 1 d D U P A 1
O1 O 0.3108(16) 0.9539(12) 0.4469(11) 0.212(6) Uani 0.5 1 d D U P A 1
O2 O 0.1376(12) 0.9526(12) 0.4673(14) 0.167(6) Uani 0.5 1 d D U P A 1
O3 O 0.284(2) 0.9715(10) 0.5734(10) 0.211(6) Uani 0.5 1 d D U P A 1
O4 O 0.233(4) 0.8612(11) 0.4946(18) 0.145(9) Uani 0.5 1 d D U P A 1
Cl1' Cl 0.2244(12) 0.9417(10) 0.5146(8) 0.121(3) Uani 0.5 1 d D U P B 2
O1' O 0.3228(14) 0.9729(11) 0.5113(13) 0.192(6) Uani 0.5 1 d D U P B 2
O2' O 0.168(2) 0.9773(13) 0.4479(11) 0.179(6) Uani 0.5 1 d D U P B 2
O3' O 0.1796(12) 0.9630(7) 0.5838(7) 0.138(4) Uani 0.5 1 d D U P B 2
O4' O 0.239(3) 0.8667(10) 0.5238(16) 0.118(6) Uani 0.5 1 d D U P B 2


_geom_special_details            
;
 All esds (except the esd in the dihedral angle between two l.s. planes)
 are estimated using the full covariance matrix.  The cell esds are taken
 into account individually in the estimation of esds in distances, angles
 and torsion angles; correlations between esds in cell parameters are only
 used when they are defined by crystal symmetry.  An approximate (isotropic)
 treatment of cell esds is used for estimating esds involving l.s. planes.
;

loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
_geom_bond_publ_flag
Fe1 C3 1.909(6) . ?
Fe1 C1 1.919(6) . ?
Fe1 C2 1.937(7) . ?
Fe1 N4 1.968(4) . ?
Fe1 N8 1.975(4) . ?
Fe1 N6 1.989(4) . ?
Fe2 N1 2.078(5) . ?
Fe2 N2 2.127(5) 3_675 ?
Fe2 N10 2.146(5) . ?
Fe2 N13 2.152(5) . ?
Fe2 N12 2.176(5) . ?
Fe2 N11 2.219(5) . ?
B1 N5 1.524(8) . ?
B1 N7 1.526(8) . ?
B1 N9 1.547(7) . ?
B1 H1 0.9912 . ?
N1 C1 1.146(6) . ?
N2 C2 1.135(7) . ?
N2 Fe2 2.127(5) 3_675 ?
N3 C3 1.158(7) . ?
N4 N5 1.355(6) . ?
N4 C4 1.358(6) . ?
N5 C6 1.329(7) . ?
N6 C8 1.319(7) . ?
N6 N7 1.343(6) . ?
N7 C10 1.345(7) . ?
N8 C12 1.331(6) . ?
N8 N9 1.355(6) . ?
N9 C14 1.330(7) . ?
N10 C20 1.298(7) . ?
N10 C16 1.328(8) . ?
N11 C28 1.457(8) . ?
N11 C21 1.475(9) . ?
N11 C22 1.477(8) . ?
N12 C23 1.316(7) . ?
N12 C27 1.339(8) . ?
N13 C33 1.346(8) . ?
N13 C29 1.365(9) . ?
C4 C5 1.342(7) . ?
C4 H4 0.9300 . ?
C5 C6 1.407(9) . ?
C5 C7 1.486(8) . ?
C6 H6 0.9300 . ?
C7 H7A 0.9600 . ?
C7 H7B 0.9600 . ?
C7 H7C 0.9600 . ?
C8 C9 1.421(8) . ?
C8 H8 0.9300 . ?
C9 C10 1.346(9) . ?
C9 C11 1.481(9) . ?
C10 H10 0.9300 . ?
C11 H11A 0.9600 . ?
C11 H11B 0.9600 . ?
C11 H11C 0.9600 . ?
C12 C13 1.399(8) . ?
C12 H12 0.9300 . ?
C13 C14 1.338(9) . ?
C13 C15 1.502(9) . ?
C14 H14 0.9300 . ?
C15 H15A 0.9600 . ?
C15 H15B 0.9600 . ?
C15 H15C 0.9600 . ?
C16 C17 1.422(10) . ?
C16 H16 0.9300 . ?
C17 C18 1.346(12) . ?
C17 H17 0.9300 . ?
C18 C19 1.381(12) . ?
C18 H18 0.9300 . ?
C19 C20 1.348(9) . ?
C19 H19 0.9300 . ?
C20 C21 1.525(10) . ?
C21 H21A 0.9700 . ?
C21 H21B 0.9700 . ?
C22 C23 1.489(9) . ?
C22 H22A 0.9700 . ?
C22 H22B 0.9700 . ?
C23 C24 1.374(9) . ?
C24 C25 1.350(10) . ?
C24 H24 0.9300 . ?
C25 C26 1.359(12) . ?
C25 H25 0.9300 . ?
C26 C27 1.383(12) . ?
C26 H26 0.9300 . ?
C27 H27 0.9300 . ?
C28 C29 1.487(10) . ?
C28 H28A 0.9700 . ?
C28 H28B 0.9700 . ?
C29 C30 1.384(11) . ?
C30 C31 1.353(16) . ?
C30 H30 0.9300 . ?
C31 C32 1.384(17) . ?
C31 H31 0.9300 . ?
C32 C33 1.332(11) . ?
C32 H32 0.9300 . ?
C33 H33 0.9300 . ?
Cl1 O1 1.376(9) . ?
Cl1 O4 1.388(9) . ?
Cl1 O3 1.393(9) . ?
Cl1 O2 1.407(10) . ?
Cl1' O4' 1.388(9) . ?
Cl1' O1' 1.391(9) . ?
Cl1' O2' 1.392(9) . ?
Cl1' O3' 1.408(9) . ?

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
C3 Fe1 C1 88.4(2) . . ?
C3 Fe1 C2 86.4(3) . . ?
C1 Fe1 C2 92.6(2) . . ?
C3 Fe1 N4 174.6(2) . . ?
C1 Fe1 N4 88.0(2) . . ?
C2 Fe1 N4 89.8(2) . . ?
C3 Fe1 N8 94.8(2) . . ?
C1 Fe1 N8 176.4(2) . . ?
C2 Fe1 N8 89.0(2) . . ?
N4 Fe1 N8 88.88(18) . . ?
C3 Fe1 N6 94.1(2) . . ?
C1 Fe1 N6 92.6(2) . . ?
C2 Fe1 N6 174.7(2) . . ?
N4 Fe1 N6 90.07(19) . . ?
N8 Fe1 N6 85.71(18) . . ?
N1 Fe2 N2 89.54(19) . 3_675 ?
N1 Fe2 N10 101.97(19) . . ?
N2 Fe2 N10 88.81(19) 3_675 . ?
N1 Fe2 N13 105.1(2) . . ?
N2 Fe2 N13 88.12(19) 3_675 . ?
N10 Fe2 N13 152.7(2) . . ?
N1 Fe2 N12 94.33(19) . . ?
N2 Fe2 N12 176.13(18) 3_675 . ?
N10 Fe2 N12 90.56(18) . . ?
N13 Fe2 N12 90.69(17) . . ?
N1 Fe2 N11 172.00(19) . . ?
N2 Fe2 N11 98.33(19) 3_675 . ?
N10 Fe2 N11 76.90(19) . . ?
N13 Fe2 N11 76.7(2) . . ?
N12 Fe2 N11 77.81(18) . . ?
N5 B1 N7 108.9(4) . . ?
N5 B1 N9 106.5(4) . . ?
N7 B1 N9 105.7(5) . . ?
N5 B1 H1 112.5 . . ?
N7 B1 H1 109.9 . . ?
N9 B1 H1 113.1 . . ?
C1 N1 Fe2 155.7(5) . . ?
C2 N2 Fe2 159.2(5) . 3_675 ?
N5 N4 C4 105.9(4) . . ?
N5 N4 Fe1 120.8(3) . . ?
C4 N4 Fe1 133.3(4) . . ?
C6 N5 N4 108.7(5) . . ?
C6 N5 B1 133.8(5) . . ?
N4 N5 B1 117.4(4) . . ?
C8 N6 N7 108.2(5) . . ?
C8 N6 Fe1 132.6(4) . . ?
N7 N6 Fe1 118.4(3) . . ?
N6 N7 C10 108.1(5) . . ?
N6 N7 B1 120.1(4) . . ?
C10 N7 B1 130.8(5) . . ?
C12 N8 N9 106.9(4) . . ?
C12 N8 Fe1 134.5(4) . . ?
N9 N8 Fe1 118.5(3) . . ?
C14 N9 N8 108.4(5) . . ?
C14 N9 B1 132.1(5) . . ?
N8 N9 B1 119.2(4) . . ?
C20 N10 C16 118.7(6) . . ?
C20 N10 Fe2 118.2(5) . . ?
C16 N10 Fe2 123.0(4) . . ?
C28 N11 C21 109.0(6) . . ?
C28 N11 C22 109.1(5) . . ?
C21 N11 C22 114.2(6) . . ?
C28 N11 Fe2 105.4(4) . . ?
C21 N11 Fe2 108.1(4) . . ?
C22 N11 Fe2 110.6(4) . . ?
C23 N12 C27 117.7(6) . . ?
C23 N12 Fe2 116.2(4) . . ?
C27 N12 Fe2 126.0(5) . . ?
C33 N13 C29 119.8(6) . . ?
C33 N13 Fe2 127.2(5) . . ?
C29 N13 Fe2 112.9(5) . . ?
N1 C1 Fe1 172.8(5) . . ?
N2 C2 Fe1 172.3(5) . . ?
N3 C3 Fe1 177.0(6) . . ?
C5 C4 N4 112.3(5) . . ?
C5 C4 H4 123.9 . . ?
N4 C4 H4 123.9 . . ?
C4 C5 C6 103.2(5) . . ?
C4 C5 C7 128.5(7) . . ?
C6 C5 C7 128.3(7) . . ?
N5 C6 C5 109.9(6) . . ?
N5 C6 H6 125.0 . . ?
C5 C6 H6 125.0 . . ?
C5 C7 H7A 109.5 . . ?
C5 C7 H7B 109.5 . . ?
H7A C7 H7B 109.5 . . ?
C5 C7 H7C 109.5 . . ?
H7A C7 H7C 109.5 . . ?
H7B C7 H7C 109.5 . . ?
N6 C8 C9 109.5(6) . . ?
N6 C8 H8 125.3 . . ?
C9 C8 H8 125.3 . . ?
C10 C9 C8 103.4(6) . . ?
C10 C9 C11 128.7(7) . . ?
C8 C9 C11 127.9(7) . . ?
N7 C10 C9 110.8(5) . . ?
N7 C10 H10 124.6 . . ?
C9 C10 H10 124.6 . . ?
C9 C11 H11A 109.5 . . ?
C9 C11 H11B 109.5 . . ?
H11A C11 H11B 109.5 . . ?
C9 C11 H11C 109.5 . . ?
H11A C11 H11C 109.5 . . ?
H11B C11 H11C 109.5 . . ?
N8 C12 C13 109.6(5) . . ?
N8 C12 H12 125.2 . . ?
C13 C12 H12 125.2 . . ?
C14 C13 C12 104.4(5) . . ?
C14 C13 C15 128.1(7) . . ?
C12 C13 C15 127.5(6) . . ?
N9 C14 C13 110.7(6) . . ?
N9 C14 H14 124.7 . . ?
C13 C14 H14 124.7 . . ?
C13 C15 H15A 109.5 . . ?
C13 C15 H15B 109.5 . . ?
H15A C15 H15B 109.5 . . ?
C13 C15 H15C 109.5 . . ?
H15A C15 H15C 109.5 . . ?
H15B C15 H15C 109.5 . . ?
N10 C16 C17 120.9(7) . . ?
N10 C16 H16 119.5 . . ?
C17 C16 H16 119.5 . . ?
C18 C17 C16 119.2(9) . . ?
C18 C17 H17 120.4 . . ?
C16 C17 H17 120.4 . . ?
C17 C18 C19 117.3(9) . . ?
C17 C18 H18 121.4 . . ?
C19 C18 H18 121.4 . . ?
C20 C19 C18 120.6(8) . . ?
C20 C19 H19 119.7 . . ?
C18 C19 H19 119.7 . . ?
N10 C20 C19 123.1(7) . . ?
N10 C20 C21 115.6(6) . . ?
C19 C20 C21 121.1(7) . . ?
N11 C21 C20 112.0(6) . . ?
N11 C21 H21A 109.2 . . ?
C20 C21 H21A 109.2 . . ?
N11 C21 H21B 109.2 . . ?
C20 C21 H21B 109.2 . . ?
H21A C21 H21B 107.9 . . ?
N11 C22 C23 114.5(5) . . ?
N11 C22 H22A 108.6 . . ?
C23 C22 H22A 108.6 . . ?
N11 C22 H22B 108.6 . . ?
C23 C22 H22B 108.6 . . ?
H22A C22 H22B 107.6 . . ?
N12 C23 C24 123.5(6) . . ?
N12 C23 C22 118.8(6) . . ?
C24 C23 C22 117.6(6) . . ?
C25 C24 C23 118.9(7) . . ?
C25 C24 H24 120.5 . . ?
C23 C24 H24 120.5 . . ?
C24 C25 C26 118.8(8) . . ?
C24 C25 H25 120.6 . . ?
C26 C25 H25 120.6 . . ?
C25 C26 C27 119.8(8) . . ?
C25 C26 H26 120.1 . . ?
C27 C26 H26 120.1 . . ?
N12 C27 C26 121.2(8) . . ?
N12 C27 H27 119.4 . . ?
C26 C27 H27 119.4 . . ?
N11 C28 C29 109.9(6) . . ?
N11 C28 H28A 109.7 . . ?
C29 C28 H28A 109.7 . . ?
N11 C28 H28B 109.7 . . ?
C29 C28 H28B 109.7 . . ?
H28A C28 H28B 108.2 . . ?
N13 C29 C30 120.2(9) . . ?
N13 C29 C28 117.3(6) . . ?
C30 C29 C28 122.3(9) . . ?
C31 C30 C29 117.5(11) . . ?
C31 C30 H30 121.3 . . ?
C29 C30 H30 121.3 . . ?
C30 C31 C32 122.2(10) . . ?
C30 C31 H31 118.9 . . ?
C32 C31 H31 118.9 . . ?
C33 C32 C31 117.9(10) . . ?
C33 C32 H32 121.1 . . ?
C31 C32 H32 121.1 . . ?
C32 C33 N13 122.2(9) . . ?
C32 C33 H33 118.9 . . ?
N13 C33 H33 118.9 . . ?
O1 Cl1 O4 103(2) . . ?
O1 Cl1 O3 104.9(15) . . ?
O4 Cl1 O3 122.5(16) . . ?
O1 Cl1 O2 110.8(15) . . ?
O4 Cl1 O2 96(2) . . ?
O3 Cl1 O2 118.0(19) . . ?
O4' Cl1' O1' 108(2) . . ?
O4' Cl1' O2' 126(2) . . ?
O1' Cl1' O2' 98.5(18) . . ?
O4' Cl1' O3' 104.3(18) . . ?
O1' Cl1' O3' 113.3(14) . . ?
O2' Cl1' O3' 106.9(15) . . ?

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
C4 N4 N5 C6 -0.6(5) . . . . ?
Fe1 N4 N5 C6 179.5(4) . . . . ?
C4 N4 N5 B1 176.1(4) . . . . ?
Fe1 N4 N5 B1 -3.8(6) . . . . ?
N7 B1 N5 C6 -126.0(6) . . . . ?
N9 B1 N5 C6 120.4(6) . . . . ?
N7 B1 N5 N4 58.3(6) . . . . ?
N9 B1 N5 N4 -55.3(6) . . . . ?
C8 N6 N7 C10 -1.1(6) . . . . ?
Fe1 N6 N7 C10 169.8(3) . . . . ?
C8 N6 N7 B1 -170.5(5) . . . . ?
Fe1 N6 N7 B1 0.5(6) . . . . ?
N5 B1 N7 N6 -56.9(6) . . . . ?
N9 B1 N7 N6 57.1(6) . . . . ?
N5 B1 N7 C10 136.5(5) . . . . ?
N9 B1 N7 C10 -109.5(6) . . . . ?
C12 N8 N9 C14 0.2(6) . . . . ?
Fe1 N8 N9 C14 176.7(4) . . . . ?
C12 N8 N9 B1 174.9(5) . . . . ?
Fe1 N8 N9 B1 -8.5(6) . . . . ?
N5 B1 N9 C14 -123.3(7) . . . . ?
N7 B1 N9 C14 121.0(7) . . . . ?
N5 B1 N9 N8 63.4(6) . . . . ?
N7 B1 N9 N8 -52.3(6) . . . . ?
N5 N4 C4 C5 0.2(6) . . . . ?
Fe1 N4 C4 C5 -179.9(4) . . . . ?
N4 C4 C5 C6 0.3(6) . . . . ?
N4 C4 C5 C7 179.3(6) . . . . ?
N4 N5 C6 C5 0.8(6) . . . . ?
B1 N5 C6 C5 -175.1(5) . . . . ?
C4 C5 C6 N5 -0.7(7) . . . . ?
C7 C5 C6 N5 -179.7(6) . . . . ?
N7 N6 C8 C9 0.9(6) . . . . ?
Fe1 N6 C8 C9 -168.3(4) . . . . ?
N6 C8 C9 C10 -0.3(7) . . . . ?
N6 C8 C9 C11 179.3(6) . . . . ?
N6 N7 C10 C9 0.9(6) . . . . ?
B1 N7 C10 C9 168.7(5) . . . . ?
C8 C9 C10 N7 -0.4(7) . . . . ?
C11 C9 C10 N7 -180.0(6) . . . . ?
N9 N8 C12 C13 0.4(7) . . . . ?
Fe1 N8 C12 C13 -175.3(5) . . . . ?
N8 C12 C13 C14 -0.8(8) . . . . ?
N8 C12 C13 C15 178.3(8) . . . . ?
N8 N9 C14 C13 -0.7(8) . . . . ?
B1 N9 C14 C13 -174.5(6) . . . . ?
C12 C13 C14 N9 0.9(9) . . . . ?
C15 C13 C14 N9 -178.2(8) . . . . ?
C20 N10 C16 C17 1.5(10) . . . . ?
Fe2 N10 C16 C17 179.4(6) . . . . ?
N10 C16 C17 C18 2.1(13) . . . . ?
C16 C17 C18 C19 -2.8(14) . . . . ?
C17 C18 C19 C20 0.4(14) . . . . ?
C16 N10 C20 C19 -4.2(11) . . . . ?
Fe2 N10 C20 C19 177.8(6) . . . . ?
C16 N10 C20 C21 170.7(6) . . . . ?
Fe2 N10 C20 C21 -7.3(8) . . . . ?
C18 C19 C20 N10 3.4(13) . . . . ?
C18 C19 C20 C21 -171.3(8) . . . . ?
C28 N11 C21 C20 -147.0(6) . . . . ?
C22 N11 C21 C20 90.7(7) . . . . ?
Fe2 N11 C21 C20 -32.9(8) . . . . ?
N10 C20 C21 N11 28.0(10) . . . . ?
C19 C20 C21 N11 -157.0(7) . . . . ?
C28 N11 C22 C23 131.2(6) . . . . ?
C21 N11 C22 C23 -106.6(7) . . . . ?
Fe2 N11 C22 C23 15.6(7) . . . . ?
C27 N12 C23 C24 0.9(9) . . . . ?
Fe2 N12 C23 C24 -178.4(5) . . . . ?
C27 N12 C23 C22 -174.8(6) . . . . ?
Fe2 N12 C23 C22 5.8(7) . . . . ?
N11 C22 C23 N12 -14.9(9) . . . . ?
N11 C22 C23 C24 169.1(6) . . . . ?
N12 C23 C24 C25 1.2(10) . . . . ?
C22 C23 C24 C25 177.0(7) . . . . ?
C23 C24 C25 C26 -2.6(13) . . . . ?
C24 C25 C26 C27 1.9(16) . . . . ?
C23 N12 C27 C26 -1.6(10) . . . . ?
Fe2 N12 C27 C26 177.6(7) . . . . ?
C25 C26 C27 N12 0.2(15) . . . . ?
C21 N11 C28 C29 160.3(6) . . . . ?
C22 N11 C28 C29 -74.4(7) . . . . ?
Fe2 N11 C28 C29 44.5(6) . . . . ?
C33 N13 C29 C30 0.2(10) . . . . ?
Fe2 N13 C29 C30 177.6(6) . . . . ?
C33 N13 C29 C28 -175.8(6) . . . . ?
Fe2 N13 C29 C28 1.7(7) . . . . ?
N11 C28 C29 N13 -32.6(8) . . . . ?
N11 C28 C29 C30 151.5(7) . . . . ?
N13 C29 C30 C31 4.0(14) . . . . ?
C28 C29 C30 C31 179.7(9) . . . . ?
C29 C30 C31 C32 -6.8(19) . . . . ?
C30 C31 C32 C33 5.3(19) . . . . ?
C31 C32 C33 N13 -0.9(14) . . . . ?
C29 N13 C33 C32 -1.8(10) . . . . ?
Fe2 N13 C33 C32 -178.8(6) . . . . ?

_refine_diff_density_max         0.424
_refine_diff_density_min         -0.488
_refine_diff_density_rms         0.096

####################################################################### 
# 
# 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_2_H2O-re-100K
_database_code_depnum_ccdc_archive 'CCDC 1419283'
_audit_update_record             
;
2016-09-02 deposited with the CCDC.
2016-09-26 downloaded from the CCDC.
;

_audit_creation_method           SHELXL-2014/7
_shelx_SHELXL_version_number     2014/7
_chemical_name_systematic        ?
_chemical_name_common            ?
_chemical_melting_point          ?
_chemical_formula_moiety         ?
_chemical_formula_sum            'C66 H70 B2 Cl2 Fe4 N26 O9'
_chemical_formula_weight         1687.40

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'
O O 0.0106 0.0060 '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'

_space_group_crystal_system      monoclinic
_space_group_IT_number           14
_space_group_name_H-M_alt        'P 21/n'
_space_group_name_Hall           '-P 2yn'

_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.
;

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                   12.9229(12)
_cell_length_b                   17.8121(17)
_cell_length_c                   16.2091(15)
_cell_angle_alpha                90
_cell_angle_beta                 98.7200(10)
_cell_angle_gamma                90
_cell_volume                     3687.9(6)
_cell_formula_units_Z            2
_cell_measurement_temperature    100(2)
_cell_measurement_reflns_used    8514
_cell_measurement_theta_min      2.20
_cell_measurement_theta_max      31.22

_exptl_crystal_description       Block
_exptl_crystal_colour            Red
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    ?
_exptl_crystal_density_diffrn    1.520
_exptl_crystal_F_000             1736
_exptl_transmission_factor_min   ?
_exptl_transmission_factor_max   ?
_exptl_crystal_size_max          0.120
_exptl_crystal_size_mid          0.100
_exptl_crystal_size_min          0.100
_exptl_absorpt_coefficient_mu    0.918
_shelx_estimated_absorpt_T_min   0.898
_shelx_estimated_absorpt_T_max   0.914
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_correction_T_min  0.8978
_exptl_absorpt_correction_T_max  0.9138
_exptl_absorpt_process_details   sadabs
_exptl_absorpt_special_details   ?
_diffrn_ambient_temperature      100(2)
_diffrn_radiation_wavelength     0.71073
_diffrn_radiation_type           MoK\a
_diffrn_radiation_source         'fine-focus sealed tube'
_diffrn_radiation_monochromator  graphite
_diffrn_measurement_device_type  'Bruker APEX-II CCD'
_diffrn_measurement_method       'φ and ω scans'
_diffrn_detector_area_resol_mean ?
_diffrn_reflns_number            27393
_diffrn_reflns_av_unetI/netI     0.0456
_diffrn_reflns_av_R_equivalents  0.0522
_diffrn_reflns_limit_h_min       -15
_diffrn_reflns_limit_h_max       15
_diffrn_reflns_limit_k_min       -20
_diffrn_reflns_limit_k_max       21
_diffrn_reflns_limit_l_min       -19
_diffrn_reflns_limit_l_max       19
_diffrn_reflns_theta_min         1.710
_diffrn_reflns_theta_max         25.499
_diffrn_reflns_theta_full        25.242
_diffrn_measured_fraction_theta_max 0.995
_diffrn_measured_fraction_theta_full 0.995
_diffrn_reflns_Laue_measured_fraction_max 0.995
_diffrn_reflns_Laue_measured_fraction_full 0.995
_diffrn_reflns_point_group_measured_fraction_max 0.995
_diffrn_reflns_point_group_measured_fraction_full 0.995
_reflns_number_total             6838
_reflns_number_gt                5306
_reflns_threshold_expression     'I > 2σ(I)'
_reflns_Friedel_coverage         0.000
_reflns_Friedel_fraction_max     .
_reflns_Friedel_fraction_full    .

_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.
;

_computing_data_collection       'Bruker APEX2'
_computing_cell_refinement       'Bruker SAINT'
_computing_data_reduction        'Bruker SAINT'
_computing_structure_solution    'SHELXS-2014 (Sheldrick, 2014)'
_computing_structure_refinement  'SHELXL-2014/7 (Sheldrick, 2014)'
_computing_molecular_graphics    ?
_computing_publication_material  ?
_refine_special_details          ?
_refine_ls_structure_factor_coef Fsqd
_refine_ls_matrix_type           full
_refine_ls_weighting_scheme      calc
_refine_ls_weighting_details     
'w=1/[σ²(Fo²)+(0.0306P)²+3.3692P] where P=(Fo²+2Fc²)/3'
_atom_sites_solution_primary     ?
_atom_sites_solution_secondary   ?
_atom_sites_solution_hydrogens   mixed
_refine_ls_hydrogen_treatment    constr
_refine_ls_extinction_method     none
_refine_ls_extinction_coef       .
_refine_ls_number_reflns         6838
_refine_ls_number_parameters     545
_refine_ls_number_restraints     136
_refine_ls_R_factor_all          0.0523
_refine_ls_R_factor_gt           0.0331
_refine_ls_wR_factor_ref         0.0857
_refine_ls_wR_factor_gt          0.0754
_refine_ls_goodness_of_fit_ref   1.029
_refine_ls_restrained_S_all      1.035
_refine_ls_shift/su_max          0.001
_refine_ls_shift/su_mean         0.000

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 -0.18130(3) 0.07511(2) 0.08488(2) 0.01431(9) Uani 1 1 d . . . . .
Fe2 Fe 0.14250(3) 0.18544(2) 0.00964(2) 0.01524(9) Uani 1 1 d . . . . .
B1 B -0.1813(2) 0.07587(16) 0.27593(17) 0.0195(6) Uani 1 1 d . . . . .
H1 H -0.1823 0.0768 0.3375 0.023 Uiso 1 1 d R U . . .
N1 N -0.17849(16) -0.08101(12) 0.00491(12) 0.0175(4) Uani 1 1 d . . . . .
N2 N 0.00294(16) 0.14930(11) 0.01799(12) 0.0171(4) Uani 1 1 d . . . . .
N3 N -0.32326(18) 0.14615(14) -0.06409(14) 0.0296(5) Uani 1 1 d . . . . .
N4 N -0.07780(16) 0.02684(11) 0.17142(12) 0.0166(4) Uani 1 1 d . . . . .
N5 N -0.09020(16) 0.02870(11) 0.25334(12) 0.0184(4) Uani 1 1 d . . . . .
N6 N -0.29633(16) 0.04009(11) 0.14243(12) 0.0178(4) Uani 1 1 d . . . . .
N7 N -0.28480(16) 0.04548(11) 0.22720(12) 0.0183(4) Uani 1 1 d . . . . .
N8 N -0.17918(16) 0.16500(11) 0.15610(12) 0.0177(4) Uani 1 1 d . . . . .
N9 N -0.16932(16) 0.15516(12) 0.24067(12) 0.0191(5) Uani 1 1 d . . . . .
N10 N 0.16875(16) 0.18721(11) 0.13281(12) 0.0183(4) Uani 1 1 d . . . . .
N11 N 0.10600(16) 0.29360(12) 0.02120(13) 0.0189(5) Uani 1 1 d . . . . .
N12 N 0.28421(16) 0.22320(11) 0.00558(12) 0.0171(4) Uani 1 1 d . . . . .
N13 N 0.10023(16) 0.20751(11) -0.11088(12) 0.0181(4) Uani 1 1 d . . . . .
C1 C -0.18327(19) -0.01883(14) 0.02554(14) 0.0165(5) Uani 1 1 d . . . . .
C2 C -0.0692(2) 0.11827(13) 0.03639(14) 0.0164(5) Uani 1 1 d . . . . .
C3 C -0.2721(2) 0.11935(14) -0.00686(16) 0.0200(5) Uani 1 1 d . . . . .
C4 C 0.01155(19) -0.01007(14) 0.16755(16) 0.0192(5) Uani 1 1 d . . . . .
H4 H 0.0390 -0.0199 0.1175 0.023 Uiso 1 1 calc R U . . .
C5 C 0.0590(2) -0.03216(14) 0.24680(16) 0.0218(6) Uani 1 1 d . . . . .
C6 C -0.0083(2) -0.00579(14) 0.29923(16) 0.0225(6) Uani 1 1 d . . . . .
H6 H 0.0019 -0.0112 0.3582 0.027 Uiso 1 1 calc R U . . .
C7 C 0.1586(2) -0.07603(17) 0.26795(19) 0.0327(7) Uani 1 1 d . . . . .
H7A H 0.2072 -0.0483 0.3093 0.049 Uiso 1 1 calc R U . . .
H7B H 0.1904 -0.0835 0.2174 0.049 Uiso 1 1 calc R U . . .
H7C H 0.1432 -0.1249 0.2910 0.049 Uiso 1 1 calc R U . . .
C8 C -0.39740(19) 0.02513(14) 0.11571(16) 0.0206(5) Uani 1 1 d . . . . .
H8 H -0.4269 0.0182 0.0589 0.025 Uiso 1 1 calc R U . . .
C9 C -0.4535(2) 0.02117(15) 0.18260(17) 0.0241(6) Uani 1 1 d . . . . .
C10 C -0.3789(2) 0.03467(14) 0.25183(17) 0.0221(6) Uani 1 1 d . . . . .
H10 H -0.3920 0.0361 0.3079 0.027 Uiso 1 1 calc R U . . .
C11 C -0.5673(2) 0.00336(19) 0.1811(2) 0.0373(7) Uani 1 1 d . . . . .
H11A H -0.5802 -0.0493 0.1652 0.056 Uiso 1 1 calc R U . . .
H11B H -0.6098 0.0359 0.1405 0.056 Uiso 1 1 calc R U . . .
H11C H -0.5863 0.0118 0.2367 0.056 Uiso 1 1 calc R U . . .
C12 C -0.1721(2) 0.23870(14) 0.14259(16) 0.0211(6) Uani 1 1 d . . . . .
H12 H -0.1780 0.2614 0.0891 0.025 Uiso 1 1 calc R U . . .
C13 C -0.1548(2) 0.27763(15) 0.21822(17) 0.0263(6) Uani 1 1 d . . . . .
C14 C -0.1543(2) 0.22238(15) 0.27807(17) 0.0245(6) Uani 1 1 d . . . . .
H14 H -0.1448 0.2307 0.3366 0.029 Uiso 1 1 calc R U . . .
C15 C -0.1385(3) 0.35999(15) 0.23271(19) 0.0383(8) Uani 1 1 d . . . . .
H15A H -0.1246 0.3699 0.2928 0.057 Uiso 1 1 calc R U . . .
H15B H -0.2016 0.3872 0.2080 0.057 Uiso 1 1 calc R U . . .
H15C H -0.0788 0.3768 0.2068 0.057 Uiso 1 1 calc R U . . .
C16 C 0.2128(2) 0.13338(15) 0.18483(16) 0.0221(6) Uani 1 1 d . . . . .
H16 H 0.2348 0.0882 0.1617 0.027 Uiso 1 1 calc R U . . .
C17 C 0.2272(2) 0.14120(16) 0.27073(17) 0.0289(6) Uani 1 1 d . . . . .
H17 H 0.2575 0.1017 0.3058 0.035 Uiso 1 1 calc R U . . .
C18 C 0.1968(2) 0.20733(17) 0.30480(17) 0.0311(7) Uani 1 1 d . . . . .
H18 H 0.2073 0.2144 0.3636 0.037 Uiso 1 1 calc R U . . .
C19 C 0.1510(2) 0.26308(16) 0.25214(16) 0.0274(6) Uani 1 1 d . . . . .
H19 H 0.1295 0.3090 0.2742 0.033 Uiso 1 1 calc R U . . .
C20 C 0.1367(2) 0.25093(14) 0.16663(16) 0.0205(6) Uani 1 1 d . . . . .
C21 C 0.0754(2) 0.30380(14) 0.10550(16) 0.0232(6) Uani 1 1 d . . . . .
H21A H -0.0004 0.2939 0.1028 0.028 Uiso 1 1 calc R U . . .
H21B H 0.0891 0.3562 0.1243 0.028 Uiso 1 1 calc R U . . .
C22 C 0.1975(2) 0.34248(15) 0.01034(17) 0.0243(6) Uani 1 1 d . . . . .
H22A H 0.1815 0.3700 -0.0431 0.029 Uiso 1 1 calc R U . . .
H22B H 0.2082 0.3799 0.0560 0.029 Uiso 1 1 calc R U . . .
C23 C 0.2960(2) 0.29847(14) 0.01072(14) 0.0197(5) Uani 1 1 d . . . . .
C24 C 0.3924(2) 0.33357(16) 0.01135(15) 0.0249(6) Uani 1 1 d . . . . .
H24 H 0.3984 0.3866 0.0163 0.030 Uiso 1 1 calc R U . . .
C25 C 0.4793(2) 0.28989(17) 0.00465(17) 0.0296(7) Uani 1 1 d . . . . .
H25 H 0.5459 0.3124 0.0046 0.036 Uiso 1 1 calc R U . . .
C26 C 0.4674(2) 0.21269(17) -0.00197(17) 0.0289(6) Uani 1 1 d . . . . .
H26 H 0.5258 0.1816 -0.0074 0.035 Uiso 1 1 calc R U . . .
C27 C 0.3702(2) 0.18148(15) -0.00062(15) 0.0228(6) Uani 1 1 d . . . . .
H27 H 0.3632 0.1284 -0.0042 0.027 Uiso 1 1 calc R U . . .
C28 C 0.0171(2) 0.30865(15) -0.04693(16) 0.0233(6) Uani 1 1 d . . . . .
H28A H 0.0085 0.3634 -0.0562 0.028 Uiso 1 1 calc R U . . .
H28B H -0.0488 0.2883 -0.0318 0.028 Uiso 1 1 calc R U . . .
C29 C 0.0421(2) 0.27109(14) -0.12437(16) 0.0210(6) Uani 1 1 d . . . . .
C30 C 0.0079(2) 0.29758(16) -0.20400(17) 0.0312(7) Uani 1 1 d . . . . .
H30 H -0.0323 0.3424 -0.2120 0.037 Uiso 1 1 calc R U . . .
C31 C 0.0328(3) 0.25817(17) -0.27196(18) 0.0357(7) Uani 1 1 d . . . . .
H31 H 0.0097 0.2754 -0.3271 0.043 Uiso 1 1 calc R U . . .
C32 C 0.0915(2) 0.19373(17) -0.25844(17) 0.0314(7) Uani 1 1 d . . . . .
H32 H 0.1096 0.1659 -0.3042 0.038 Uiso 1 1 calc R U . . .
C33 C 0.1238(2) 0.16994(15) -0.17743(16) 0.0236(6) Uani 1 1 d . . . . .
H33 H 0.1643 0.1253 -0.1685 0.028 Uiso 1 1 calc R U . . .
Cl1 Cl 0.74075(11) 0.43476(8) 0.01863(9) 0.0205(3) Uani 0.5 1 d D U P A 1
O1 O 0.6843(12) 0.4738(9) -0.0503(8) 0.051(3) Uani 0.5 1 d D U P A 1
O2 O 0.6814(3) 0.4251(2) 0.0834(3) 0.0387(10) Uani 0.5 1 d D U P A 1
O3 O 0.8341(13) 0.4702(12) 0.0535(11) 0.045(3) Uani 0.5 1 d D U P A 1
O4 O 0.7613(13) 0.3631(5) -0.0116(14) 0.039(3) Uani 0.5 1 d D U P A 1
Cl1' Cl 0.78306(18) 0.44972(10) -0.01338(12) 0.0497(5) Uani 0.5 1 d D U P B 2
O1' O 0.8460(5) 0.4714(3) -0.0793(3) 0.0628(14) Uani 0.5 1 d D U P B 2
O2' O 0.7875(13) 0.3706(5) -0.0115(14) 0.039(3) Uani 0.5 1 d D U P B 2
O3' O 0.8410(13) 0.4850(12) 0.0565(11) 0.043(2) Uani 0.5 1 d D U P B 2
O4' O 0.6857(10) 0.4864(9) -0.0344(9) 0.056(3) Uani 0.5 1 d D U P B 2
O1W O 0.9398(4) 0.5037(2) -0.1003(3) 0.0401(11) Uani 0.5 1 d . . P C 1
H1WA H 0.9061 0.4931 -0.0627 0.060 Uiso 0.5 1 d R U P C 1
H1WB H 1.0002 0.5130 -0.0789 0.060 Uiso 0.5 1 d R U P C 1


_geom_special_details            
;
 All esds (except the esd in the dihedral angle between two l.s. planes)
 are estimated using the full covariance matrix.  The cell esds are taken
 into account individually in the estimation of esds in distances, angles
 and torsion angles; correlations between esds in cell parameters are only
 used when they are defined by crystal symmetry.  An approximate (isotropic)
 treatment of cell esds is used for estimating esds involving l.s. planes.
;

loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
_geom_bond_publ_flag
Fe1 C2 1.911(3) . ?
Fe1 C3 1.918(3) . ?
Fe1 C1 1.928(3) . ?
Fe1 N8 1.972(2) . ?
Fe1 N6 1.972(2) . ?
Fe1 N4 1.982(2) . ?
Fe2 N2 1.939(2) . ?
Fe2 N1 1.940(2) 3 ?
Fe2 N12 1.961(2) . ?
Fe2 N10 1.974(2) . ?
Fe2 N13 1.986(2) . ?
Fe2 N11 1.999(2) . ?
B1 N5 1.535(4) . ?
B1 N9 1.540(3) . ?
B1 N7 1.544(4) . ?
B1 H1 1.0007 . ?
N1 C1 1.161(3) . ?
N1 Fe2 1.940(2) 3 ?
N2 C2 1.161(3) . ?
N3 C3 1.157(3) . ?
N4 C4 1.338(3) . ?
N4 N5 1.362(3) . ?
N5 C6 1.347(3) . ?
N6 C8 1.339(3) . ?
N6 N7 1.363(3) . ?
N7 C10 1.351(3) . ?
N8 C12 1.336(3) . ?
N8 N9 1.369(3) . ?
N9 C14 1.343(3) . ?
N10 C16 1.345(3) . ?
N10 C20 1.352(3) . ?
N11 C21 1.490(3) . ?
N11 C28 1.492(3) . ?
N11 C22 1.500(3) . ?
N12 C23 1.351(3) . ?
N12 C27 1.353(3) . ?
N13 C33 1.343(3) . ?
N13 C29 1.358(3) . ?
C4 C5 1.394(3) . ?
C4 H4 0.9500 . ?
C5 C6 1.386(4) . ?
C5 C7 1.500(4) . ?
C6 H6 0.9500 . ?
C7 H7A 0.9800 . ?
C7 H7B 0.9800 . ?
C7 H7C 0.9800 . ?
C8 C9 1.394(4) . ?
C8 H8 0.9500 . ?
C9 C10 1.385(4) . ?
C9 C11 1.501(4) . ?
C10 H10 0.9500 . ?
C11 H11A 0.9800 . ?
C11 H11B 0.9800 . ?
C11 H11C 0.9800 . ?
C12 C13 1.397(4) . ?
C12 H12 0.9500 . ?
C13 C14 1.381(4) . ?
C13 C15 1.495(4) . ?
C14 H14 0.9500 . ?
C15 H15A 0.9800 . ?
C15 H15B 0.9800 . ?
C15 H15C 0.9800 . ?
C16 C17 1.383(4) . ?
C16 H16 0.9500 . ?
C17 C18 1.383(4) . ?
C17 H17 0.9500 . ?
C18 C19 1.383(4) . ?
C18 H18 0.9500 . ?
C19 C20 1.387(4) . ?
C19 H19 0.9500 . ?
C20 C21 1.503(4) . ?
C21 H21A 0.9900 . ?
C21 H21B 0.9900 . ?
C22 C23 1.494(4) . ?
C22 H22A 0.9900 . ?
C22 H22B 0.9900 . ?
C23 C24 1.392(4) . ?
C24 C25 1.383(4) . ?
C24 H24 0.9500 . ?
C25 C26 1.386(4) . ?
C25 H25 0.9500 . ?
C26 C27 1.377(4) . ?
C26 H26 0.9500 . ?
C27 H27 0.9500 . ?
C28 C29 1.500(4) . ?
C28 H28A 0.9900 . ?
C28 H28B 0.9900 . ?
C29 C30 1.382(4) . ?
C30 C31 1.385(4) . ?
C30 H30 0.9500 . ?
C31 C32 1.375(4) . ?
C31 H31 0.9500 . ?
C32 C33 1.383(4) . ?
C32 H32 0.9500 . ?
C33 H33 0.9500 . ?
Cl1 O2 1.401(4) . ?
Cl1 O3 1.402(9) . ?
Cl1 O4 1.408(8) . ?
Cl1 O1 1.421(8) . ?
Cl1' O3' 1.408(9) . ?
Cl1' O2' 1.411(8) . ?
Cl1' O4' 1.412(9) . ?
Cl1' O1' 1.489(5) . ?
O1W H1WA 0.8232 . ?
O1W H1WB 0.8230 . ?

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
C2 Fe1 C3 85.91(10) . . ?
C2 Fe1 C1 95.59(10) . . ?
C3 Fe1 C1 90.55(10) . . ?
C2 Fe1 N8 88.28(9) . . ?
C3 Fe1 N8 94.17(10) . . ?
C1 Fe1 N8 174.10(9) . . ?
C2 Fe1 N6 173.95(9) . . ?
C3 Fe1 N6 94.60(9) . . ?
C1 Fe1 N6 90.44(9) . . ?
N8 Fe1 N6 85.67(8) . . ?
C2 Fe1 N4 89.61(9) . . ?
C3 Fe1 N4 174.17(9) . . ?
C1 Fe1 N4 86.17(9) . . ?
N8 Fe1 N4 89.42(8) . . ?
N6 Fe1 N4 90.24(8) . . ?
N2 Fe2 N1 86.15(8) . 3 ?
N2 Fe2 N12 177.85(8) . . ?
N1 Fe2 N12 94.72(9) 3 . ?
N2 Fe2 N10 87.35(8) . . ?
N1 Fe2 N10 97.50(8) 3 . ?
N12 Fe2 N10 90.59(8) . . ?
N2 Fe2 N13 90.82(8) . . ?
N1 Fe2 N13 96.05(8) 3 . ?
N12 Fe2 N13 91.04(8) . . ?
N10 Fe2 N13 166.17(9) . . ?
N2 Fe2 N11 94.49(8) . . ?
N1 Fe2 N11 178.34(8) 3 . ?
N12 Fe2 N11 84.69(8) . . ?
N10 Fe2 N11 84.06(8) . . ?
N13 Fe2 N11 82.41(8) . . ?
N5 B1 N9 106.8(2) . . ?
N5 B1 N7 108.8(2) . . ?
N9 B1 N7 105.1(2) . . ?
N5 B1 H1 111.9 . . ?
N9 B1 H1 111.9 . . ?
N7 B1 H1 112.0 . . ?
C1 N1 Fe2 166.8(2) . 3 ?
C2 N2 Fe2 165.38(19) . . ?
C4 N4 N5 106.71(19) . . ?
C4 N4 Fe1 132.41(16) . . ?
N5 N4 Fe1 120.87(15) . . ?
C6 N5 N4 109.2(2) . . ?
C6 N5 B1 133.3(2) . . ?
N4 N5 B1 116.98(19) . . ?
C8 N6 N7 107.0(2) . . ?
C8 N6 Fe1 132.70(17) . . ?
N7 N6 Fe1 118.66(15) . . ?
C10 N7 N6 108.8(2) . . ?
C10 N7 B1 130.4(2) . . ?
N6 N7 B1 119.62(19) . . ?
C12 N8 N9 107.0(2) . . ?
C12 N8 Fe1 134.19(17) . . ?
N9 N8 Fe1 118.25(15) . . ?
C14 N9 N8 108.8(2) . . ?
C14 N9 B1 131.8(2) . . ?
N8 N9 B1 119.33(19) . . ?
C16 N10 C20 118.1(2) . . ?
C16 N10 Fe2 127.90(17) . . ?
C20 N10 Fe2 114.03(17) . . ?
C21 N11 C28 112.0(2) . . ?
C21 N11 C22 111.1(2) . . ?
C28 N11 C22 109.9(2) . . ?
C21 N11 Fe2 107.62(15) . . ?
C28 N11 Fe2 105.65(15) . . ?
C22 N11 Fe2 110.31(15) . . ?
C23 N12 C27 117.6(2) . . ?
C23 N12 Fe2 115.82(17) . . ?
C27 N12 Fe2 126.56(17) . . ?
C33 N13 C29 118.3(2) . . ?
C33 N13 Fe2 128.99(18) . . ?
C29 N13 Fe2 112.72(16) . . ?
N1 C1 Fe1 166.9(2) . . ?
N2 C2 Fe1 170.2(2) . . ?
N3 C3 Fe1 177.1(2) . . ?
N4 C4 C5 110.9(2) . . ?
N4 C4 H4 124.5 . . ?
C5 C4 H4 124.5 . . ?
C6 C5 C4 103.9(2) . . ?
C6 C5 C7 129.2(2) . . ?
C4 C5 C7 126.9(2) . . ?
N5 C6 C5 109.2(2) . . ?
N5 C6 H6 125.4 . . ?
C5 C6 H6 125.4 . . ?
C5 C7 H7A 109.5 . . ?
C5 C7 H7B 109.5 . . ?
H7A C7 H7B 109.5 . . ?
C5 C7 H7C 109.5 . . ?
H7A C7 H7C 109.5 . . ?
H7B C7 H7C 109.5 . . ?
N6 C8 C9 110.8(2) . . ?
N6 C8 H8 124.6 . . ?
C9 C8 H8 124.6 . . ?
C10 C9 C8 104.0(2) . . ?
C10 C9 C11 127.5(2) . . ?
C8 C9 C11 128.4(3) . . ?
N7 C10 C9 109.4(2) . . ?
N7 C10 H10 125.3 . . ?
C9 C10 H10 125.3 . . ?
C9 C11 H11A 109.5 . . ?
C9 C11 H11B 109.5 . . ?
H11A C11 H11B 109.5 . . ?
C9 C11 H11C 109.5 . . ?
H11A C11 H11C 109.5 . . ?
H11B C11 H11C 109.5 . . ?
N8 C12 C13 110.5(2) . . ?
N8 C12 H12 124.8 . . ?
C13 C12 H12 124.8 . . ?
C14 C13 C12 104.2(2) . . ?
C14 C13 C15 127.1(3) . . ?
C12 C13 C15 128.7(3) . . ?
N9 C14 C13 109.5(2) . . ?
N9 C14 H14 125.3 . . ?
C13 C14 H14 125.3 . . ?
C13 C15 H15A 109.5 . . ?
C13 C15 H15B 109.5 . . ?
H15A C15 H15B 109.5 . . ?
C13 C15 H15C 109.5 . . ?
H15A C15 H15C 109.5 . . ?
H15B C15 H15C 109.5 . . ?
N10 C16 C17 122.6(2) . . ?
N10 C16 H16 118.7 . . ?
C17 C16 H16 118.7 . . ?
C18 C17 C16 119.0(3) . . ?
C18 C17 H17 120.5 . . ?
C16 C17 H17 120.5 . . ?
C17 C18 C19 119.1(3) . . ?
C17 C18 H18 120.5 . . ?
C19 C18 H18 120.5 . . ?
C18 C19 C20 119.0(3) . . ?
C18 C19 H19 120.5 . . ?
C20 C19 H19 120.5 . . ?
N10 C20 C19 122.3(2) . . ?
N10 C20 C21 114.9(2) . . ?
C19 C20 C21 122.5(2) . . ?
N11 C21 C20 109.9(2) . . ?
N11 C21 H21A 109.7 . . ?
C20 C21 H21A 109.7 . . ?
N11 C21 H21B 109.7 . . ?
C20 C21 H21B 109.7 . . ?
H21A C21 H21B 108.2 . . ?
C23 C22 N11 112.4(2) . . ?
C23 C22 H22A 109.1 . . ?
N11 C22 H22A 109.1 . . ?
C23 C22 H22B 109.1 . . ?
N11 C22 H22B 109.1 . . ?
H22A C22 H22B 107.9 . . ?
N12 C23 C24 122.6(2) . . ?
N12 C23 C22 115.6(2) . . ?
C24 C23 C22 121.7(2) . . ?
C25 C24 C23 118.9(3) . . ?
C25 C24 H24 120.6 . . ?
C23 C24 H24 120.6 . . ?
C24 C25 C26 118.9(3) . . ?
C24 C25 H25 120.6 . . ?
C26 C25 H25 120.6 . . ?
C27 C26 C25 119.3(3) . . ?
C27 C26 H26 120.3 . . ?
C25 C26 H26 120.3 . . ?
N12 C27 C26 122.7(3) . . ?
N12 C27 H27 118.6 . . ?
C26 C27 H27 118.6 . . ?
N11 C28 C29 107.5(2) . . ?
N11 C28 H28A 110.2 . . ?
C29 C28 H28A 110.2 . . ?
N11 C28 H28B 110.2 . . ?
C29 C28 H28B 110.2 . . ?
H28A C28 H28B 108.5 . . ?
N13 C29 C30 121.7(2) . . ?
N13 C29 C28 114.9(2) . . ?
C30 C29 C28 123.4(2) . . ?
C29 C30 C31 119.3(3) . . ?
C29 C30 H30 120.3 . . ?
C31 C30 H30 120.3 . . ?
C32 C31 C30 119.0(3) . . ?
C32 C31 H31 120.5 . . ?
C30 C31 H31 120.5 . . ?
C31 C32 C33 119.2(3) . . ?
C31 C32 H32 120.4 . . ?
C33 C32 H32 120.4 . . ?
N13 C33 C32 122.5(3) . . ?
N13 C33 H33 118.8 . . ?
C32 C33 H33 118.8 . . ?
O2 Cl1 O3 106.8(9) . . ?
O2 Cl1 O4 107.7(8) . . ?
O3 Cl1 O4 110.6(11) . . ?
O2 Cl1 O1 112.0(7) . . ?
O3 Cl1 O1 113.9(12) . . ?
O4 Cl1 O1 105.8(11) . . ?
O3' Cl1' O2' 114.4(12) . . ?
O3' Cl1' O4' 109.5(11) . . ?
O2' Cl1' O4' 120.0(11) . . ?
O3' Cl1' O1' 100.4(9) . . ?
O2' Cl1' O1' 104.5(8) . . ?
O4' Cl1' O1' 105.7(7) . . ?
H1WA O1W H1WB 107.9 . . ?

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
C4 N4 N5 C6 0.9(3) . . . . ?
Fe1 N4 N5 C6 -178.11(16) . . . . ?
C4 N4 N5 B1 173.4(2) . . . . ?
Fe1 N4 N5 B1 -5.7(3) . . . . ?
N9 B1 N5 C6 116.4(3) . . . . ?
N7 B1 N5 C6 -130.7(3) . . . . ?
N9 B1 N5 N4 -53.8(3) . . . . ?
N7 B1 N5 N4 59.1(3) . . . . ?
C8 N6 N7 C10 -0.7(3) . . . . ?
Fe1 N6 N7 C10 166.51(16) . . . . ?
C8 N6 N7 B1 -169.4(2) . . . . ?
Fe1 N6 N7 B1 -2.2(3) . . . . ?
N5 B1 N7 C10 138.7(2) . . . . ?
N9 B1 N7 C10 -107.3(3) . . . . ?
N5 B1 N7 N6 -55.4(3) . . . . ?
N9 B1 N7 N6 58.7(3) . . . . ?
C12 N8 N9 C14 -1.2(3) . . . . ?
Fe1 N8 N9 C14 171.16(17) . . . . ?
C12 N8 N9 B1 176.1(2) . . . . ?
Fe1 N8 N9 B1 -11.5(3) . . . . ?
N5 B1 N9 C14 -118.4(3) . . . . ?
N7 B1 N9 C14 126.2(3) . . . . ?
N5 B1 N9 N8 65.1(3) . . . . ?
N7 B1 N9 N8 -50.4(3) . . . . ?
Fe2 N1 C1 Fe1 -37.9(16) 3 . . . ?
N5 N4 C4 C5 -0.5(3) . . . . ?
Fe1 N4 C4 C5 178.36(17) . . . . ?
N4 C4 C5 C6 -0.1(3) . . . . ?
N4 C4 C5 C7 178.6(2) . . . . ?
N4 N5 C6 C5 -1.0(3) . . . . ?
B1 N5 C6 C5 -171.8(2) . . . . ?
C4 C5 C6 N5 0.6(3) . . . . ?
C7 C5 C6 N5 -178.0(3) . . . . ?
N7 N6 C8 C9 0.5(3) . . . . ?
Fe1 N6 C8 C9 -164.16(18) . . . . ?
N6 C8 C9 C10 -0.1(3) . . . . ?
N6 C8 C9 C11 -177.9(3) . . . . ?
N6 N7 C10 C9 0.6(3) . . . . ?
B1 N7 C10 C9 167.8(2) . . . . ?
C8 C9 C10 N7 -0.3(3) . . . . ?
C11 C9 C10 N7 177.5(3) . . . . ?
N9 N8 C12 C13 1.6(3) . . . . ?
Fe1 N8 C12 C13 -169.04(19) . . . . ?
N8 C12 C13 C14 -1.3(3) . . . . ?
N8 C12 C13 C15 177.8(3) . . . . ?
N8 N9 C14 C13 0.4(3) . . . . ?
B1 N9 C14 C13 -176.4(3) . . . . ?
C12 C13 C14 N9 0.5(3) . . . . ?
C15 C13 C14 N9 -178.6(3) . . . . ?
C20 N10 C16 C17 -0.6(4) . . . . ?
Fe2 N10 C16 C17 179.9(2) . . . . ?
N10 C16 C17 C18 -1.1(4) . . . . ?
C16 C17 C18 C19 1.3(4) . . . . ?
C17 C18 C19 C20 0.0(4) . . . . ?
C16 N10 C20 C19 2.1(4) . . . . ?
Fe2 N10 C20 C19 -178.4(2) . . . . ?
C16 N10 C20 C21 -172.0(2) . . . . ?
Fe2 N10 C20 C21 7.5(3) . . . . ?
C18 C19 C20 N10 -1.8(4) . . . . ?
C18 C19 C20 C21 171.9(3) . . . . ?
C28 N11 C21 C20 148.4(2) . . . . ?
C22 N11 C21 C20 -88.1(2) . . . . ?
Fe2 N11 C21 C20 32.7(2) . . . . ?
N10 C20 C21 N11 -27.2(3) . . . . ?
C19 C20 C21 N11 158.7(2) . . . . ?
C21 N11 C22 C23 108.1(2) . . . . ?
C28 N11 C22 C23 -127.3(2) . . . . ?
Fe2 N11 C22 C23 -11.2(3) . . . . ?
C27 N12 C23 C24 -1.2(3) . . . . ?
Fe2 N12 C23 C24 177.93(18) . . . . ?
C27 N12 C23 C22 175.1(2) . . . . ?
Fe2 N12 C23 C22 -5.7(3) . . . . ?
N11 C22 C23 N12 11.3(3) . . . . ?
N11 C22 C23 C24 -172.3(2) . . . . ?
N12 C23 C24 C25 1.4(4) . . . . ?
C22 C23 C24 C25 -174.7(2) . . . . ?
C23 C24 C25 C26 -0.4(4) . . . . ?
C24 C25 C26 C27 -0.8(4) . . . . ?
C23 N12 C27 C26 -0.1(3) . . . . ?
Fe2 N12 C27 C26 -179.12(19) . . . . ?
C25 C26 C27 N12 1.1(4) . . . . ?
C21 N11 C28 C29 -159.8(2) . . . . ?
C22 N11 C28 C29 76.1(2) . . . . ?
Fe2 N11 C28 C29 -42.9(2) . . . . ?
C33 N13 C29 C30 -0.4(4) . . . . ?
Fe2 N13 C29 C30 177.8(2) . . . . ?
C33 N13 C29 C28 178.6(2) . . . . ?
Fe2 N13 C29 C28 -3.2(3) . . . . ?
N11 C28 C29 N13 31.2(3) . . . . ?
N11 C28 C29 C30 -149.8(2) . . . . ?
N13 C29 C30 C31 0.4(4) . . . . ?
C28 C29 C30 C31 -178.5(3) . . . . ?
C29 C30 C31 C32 -0.3(4) . . . . ?
C30 C31 C32 C33 0.1(4) . . . . ?
C29 N13 C33 C32 0.2(4) . . . . ?
Fe2 N13 C33 C32 -177.63(19) . . . . ?
C31 C32 C33 N13 -0.1(4) . . . . ?

loop_
_geom_hbond_atom_site_label_D
_geom_hbond_atom_site_label_H
_geom_hbond_atom_site_label_A
_geom_hbond_distance_DH
_geom_hbond_distance_HA
_geom_hbond_distance_DA
_geom_hbond_angle_DHA
_geom_hbond_site_symmetry_A
C10 H10 O3 0.95 2.54 3.326(16) 139.6 2_545
C10 H10 O3' 0.95 2.38 3.195(15) 144.1 2_545
C12 H12 O4 0.95 2.48 3.35(2) 152.2 1_455
C12 H12 O2' 0.95 2.53 3.411(19) 153.7 1_455
C16 H16 N1 0.95 2.69 3.180(3) 112.6 3
C17 H17 O1' 0.95 2.41 3.340(6) 164.7 4_566
C21 H21B O1W 0.99 2.54 3.436(5) 149.7 3_665
C22 H22A O3' 0.99 2.60 3.27(2) 124.8 3_665
C24 H24 O4' 0.95 2.55 3.400(15) 149.5 3_665
C26 H26 N3 0.95 2.37 3.250(4) 154.8 1_655
C27 H27 N1 0.95 2.53 3.049(3) 114.4 3
C28 H28B O2' 0.99 2.64 3.297(15) 124.3 1_455
O1W H1WA Cl1 0.82 2.87 3.653(4) 159.6 .
O1W H1WA O3 0.82 2.26 3.08(2) 171.7 .
O1W H1WB O3 0.82 2.14 2.943(14) 165.6 3_765
C10 H10 O3 0.95 2.54 3.326(16) 139.6 2_545
C10 H10 O3' 0.95 2.38 3.195(15) 144.1 2_545
C12 H12 O4 0.95 2.48 3.35(2) 152.2 1_455
C12 H12 O2' 0.95 2.53 3.411(19) 153.7 1_455
C16 H16 N1 0.95 2.69 3.180(3) 112.6 3
C17 H17 O1' 0.95 2.41 3.340(6) 164.7 4_566
C21 H21B O1W 0.99 2.54 3.436(5) 149.7 3_665
C22 H22A O3' 0.99 2.60 3.27(2) 124.8 3_665
C24 H24 O4' 0.95 2.55 3.400(15) 149.5 3_665
C26 H26 N3 0.95 2.37 3.250(4) 154.8 1_655
C27 H27 N1 0.95 2.53 3.049(3) 114.4 3
C28 H28B O2' 0.99 2.64 3.297(15) 124.3 1_455
O1W H1WA Cl1 0.82 2.87 3.653(4) 159.6 .
O1W H1WA O3 0.82 2.26 3.08(2) 171.7 .
O1W H1WB O3 0.82 2.14 2.943(14) 165.6 3_765

_refine_diff_density_max         0.466
_refine_diff_density_min         -0.594
_refine_diff_density_rms         0.065

####################################################################### 
# 
# 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_2_H2O-re-296K
_database_code_depnum_ccdc_archive 'CCDC 1419284'
_audit_update_record             
;
2016-09-02 deposited with the CCDC.
2016-09-26 downloaded from the CCDC.
;

_audit_creation_method           SHELXL-2014/7
_shelx_SHELXL_version_number     2014/7
_chemical_name_systematic        ?
_chemical_name_common            ?
_chemical_melting_point          ?
_chemical_formula_moiety         '(C66 H68 B2 Fe4 N26), 2(Cl O4), (H2 O)'
_chemical_formula_sum            'C66 H70 B2 Cl2 Fe4 N26 O9'
_chemical_formula_weight         1687.40

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'
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'
B B 0.0013 0.0007 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Cl Cl 0.1484 0.1585 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Fe Fe 0.3463 0.8444 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'

_space_group_crystal_system      monoclinic
_space_group_IT_number           14
_space_group_name_H-M_alt        'P 21/n'
_space_group_name_Hall           '-P 2yn'

_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.
;

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                   13.0316(18)
_cell_length_b                   18.007(3)
_cell_length_c                   16.368(2)
_cell_angle_alpha                90
_cell_angle_beta                 99.188(2)
_cell_angle_gamma                90
_cell_volume                     3791.7(9)
_cell_formula_units_Z            2
_cell_measurement_temperature    296(2)
_cell_measurement_reflns_used    7051
_cell_measurement_theta_min      2.45
_cell_measurement_theta_max      28.32

_exptl_crystal_description       Block
_exptl_crystal_colour            Red
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    ?
_exptl_crystal_density_diffrn    1.478
_exptl_crystal_F_000             1736
_exptl_transmission_factor_min   ?
_exptl_transmission_factor_max   ?
_exptl_crystal_size_max          0.120
_exptl_crystal_size_mid          0.100
_exptl_crystal_size_min          0.100
_exptl_absorpt_coefficient_mu    0.893
_shelx_estimated_absorpt_T_min   0.900
_shelx_estimated_absorpt_T_max   0.916
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_correction_T_min  0.9004
_exptl_absorpt_correction_T_max  0.9160
_exptl_absorpt_process_details   sadabs
_exptl_absorpt_special_details   ?
_diffrn_ambient_temperature      296(2)
_diffrn_radiation_wavelength     0.71073
_diffrn_radiation_type           MoK\a
_diffrn_radiation_source         'fine-focus sealed tube'
_diffrn_radiation_monochromator  graphite
_diffrn_measurement_device_type  'Bruker APEX-II CCD'
_diffrn_measurement_method       'φ and ω scans'
_diffrn_detector_area_resol_mean ?
_diffrn_reflns_number            26221
_diffrn_reflns_av_unetI/netI     0.0438
_diffrn_reflns_av_R_equivalents  0.0495
_diffrn_reflns_limit_h_min       -15
_diffrn_reflns_limit_h_max       13
_diffrn_reflns_limit_k_min       -21
_diffrn_reflns_limit_k_max       21
_diffrn_reflns_limit_l_min       -19
_diffrn_reflns_limit_l_max       19
_diffrn_reflns_theta_min         1.693
_diffrn_reflns_theta_max         25.000
_diffrn_reflns_theta_full        25.000
_diffrn_measured_fraction_theta_max 0.993
_diffrn_measured_fraction_theta_full 0.993
_diffrn_reflns_Laue_measured_fraction_max 0.993
_diffrn_reflns_Laue_measured_fraction_full 0.993
_diffrn_reflns_point_group_measured_fraction_max 0.993
_diffrn_reflns_point_group_measured_fraction_full 0.993
_reflns_number_total             6639
_reflns_number_gt                5127
_reflns_threshold_expression     'I > 2σ(I)'
_reflns_Friedel_coverage         0.000
_reflns_Friedel_fraction_max     .
_reflns_Friedel_fraction_full    .

_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.
;

_computing_data_collection       'Bruker APEX2'
_computing_cell_refinement       'Bruker SAINT'
_computing_data_reduction        'Bruker SAINT'
_computing_structure_solution    'SHELXS-2014 (Sheldrick, 2014)'
_computing_structure_refinement  'SHELXL-2014/7 (Sheldrick, 2014)'
_computing_molecular_graphics    ?
_computing_publication_material  ?
_refine_special_details          ?
_refine_ls_structure_factor_coef Fsqd
_refine_ls_matrix_type           full
_refine_ls_weighting_scheme      calc
_refine_ls_weighting_details     
'w=1/[σ²(Fo²)+(0.0774P)²+1.5162P] where P=(Fo²+2Fc²)/3'
_atom_sites_solution_primary     ?
_atom_sites_solution_secondary   ?
_atom_sites_solution_hydrogens   mixed
_refine_ls_hydrogen_treatment    constr
_refine_ls_extinction_method     none
_refine_ls_extinction_coef       .
_refine_ls_number_reflns         6639
_refine_ls_number_parameters     543
_refine_ls_number_restraints     54
_refine_ls_R_factor_all          0.0591
_refine_ls_R_factor_gt           0.0422
_refine_ls_wR_factor_ref         0.1311
_refine_ls_wR_factor_gt          0.1154
_refine_ls_goodness_of_fit_ref   1.021
_refine_ls_restrained_S_all      1.066
_refine_ls_shift/su_max          0.002
_refine_ls_shift/su_mean         0.000

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 0.31913(3) 1.07673(2) 0.08401(2) 0.03320(14) Uani 1 1 d . . . . .
Fe2 Fe 0.35657(3) 0.81884(2) -0.00941(2) 0.03537(14) Uani 1 1 d . . . . .
B1 B 0.3216(3) 1.07826(19) 0.2731(2) 0.0474(9) Uani 1 1 d . . . . .
H1 H 0.3216 1.0793 0.3330 0.057 Uiso 1 1 d R U . . .
N1 N 0.3200(2) 0.92303(14) 0.00372(16) 0.0449(6) Uani 1 1 d . . . . .
N2 N 0.5021(2) 1.14603(13) 0.01619(16) 0.0418(6) Uani 1 1 d . . . . .
N3 N 0.1762(3) 1.1473(2) -0.0623(2) 0.0755(10) Uani 1 1 d . . . . .
N4 N 0.4225(2) 1.02912(13) 0.16983(14) 0.0391(6) Uani 1 1 d . . . . .
N5 N 0.4110(2) 1.03161(14) 0.25050(15) 0.0450(6) Uani 1 1 d . . . . .
N6 N 0.2059(2) 1.04265(13) 0.14141(15) 0.0418(6) Uani 1 1 d . . . . .
N7 N 0.2182(2) 1.04749(13) 0.22511(16) 0.0440(6) Uani 1 1 d . . . . .
N8 N 0.3225(2) 1.16597(13) 0.15467(15) 0.0413(6) Uani 1 1 d . . . . .
N9 N 0.3323(2) 1.15647(14) 0.23772(16) 0.0471(7) Uani 1 1 d . . . . .
N10 N 0.3305(2) 0.81449(13) -0.13283(16) 0.0427(6) Uani 1 1 d . . . . .
N11 N 0.3910(2) 0.70933(14) -0.02180(17) 0.0467(6) Uani 1 1 d . . . . .
N12 N 0.2140(2) 0.77998(14) -0.00580(15) 0.0433(6) Uani 1 1 d . . . . .
N13 N 0.3989(2) 0.79424(15) 0.11073(16) 0.0471(7) Uani 1 1 d . . . . .
C1 C 0.3159(2) 0.98432(16) 0.02469(17) 0.0373(7) Uani 1 1 d . . . . .
C2 C 0.4302(2) 1.11739(15) 0.03518(17) 0.0366(7) Uani 1 1 d . . . . .
C3 C 0.2274(3) 1.12046(19) -0.0067(2) 0.0472(8) Uani 1 1 d . . . . .
C4 C 0.5096(3) 0.99170(17) 0.1655(2) 0.0466(8) Uani 1 1 d . . . . .
H4 H 0.5354 0.9819 0.1168 0.056 Uiso 1 1 calc R U . . .
C5 C 0.5566(3) 0.96942(19) 0.2438(2) 0.0554(9) Uani 1 1 d . . . . .
C6 C 0.4925(3) 0.99640(19) 0.2954(2) 0.0560(9) Uani 1 1 d . . . . .
H6 H 0.5034 0.9912 0.3527 0.067 Uiso 1 1 calc R U . . .
C7 C 0.6545(4) 0.9243(3) 0.2640(3) 0.0874(15) Uani 1 1 d . . . . .
H7A H 0.6818 0.9139 0.2141 0.131 Uiso 1 1 calc R U . . .
H7B H 0.7050 0.9517 0.3014 0.131 Uiso 1 1 calc R U . . .
H7C H 0.6393 0.8784 0.2895 0.131 Uiso 1 1 calc R U . . .
C8 C 0.1066(3) 1.02589(17) 0.1156(2) 0.0480(8) Uani 1 1 d . . . . .
H8 H 0.0775 1.0188 0.0605 0.058 Uiso 1 1 calc R U . . .
C9 C 0.0520(3) 1.02037(18) 0.1817(3) 0.0564(9) Uani 1 1 d . . . . .
C10 C 0.1261(3) 1.03461(17) 0.2495(2) 0.0525(9) Uani 1 1 d . . . . .
H10 H 0.1143 1.0352 0.3041 0.063 Uiso 1 1 calc R U . . .
C11 C -0.0604(3) 1.0029(3) 0.1810(3) 0.0888(14) Uani 1 1 d . . . . .
H11A H -0.0752 1.0037 0.2366 0.133 Uiso 1 1 calc R U . . .
H11B H -0.0757 0.9545 0.1574 0.133 Uiso 1 1 calc R U . . .
H11C H -0.1026 1.0393 0.1484 0.133 Uiso 1 1 calc R U . . .
C12 C 0.3288(3) 1.23865(16) 0.1412(2) 0.0523(9) Uani 1 1 d . . . . .
H12 H 0.3230 1.2606 0.0892 0.063 Uiso 1 1 calc R U . . .
C13 C 0.3452(3) 1.27677(18) 0.2153(2) 0.0635(11) Uani 1 1 d . . . . .
C14 C 0.3463(3) 1.22281(19) 0.2746(2) 0.0595(10) Uani 1 1 d . . . . .
H14 H 0.3554 1.2310 0.3314 0.071 Uiso 1 1 calc R U . . .
C15 C 0.3616(5) 1.3586(2) 0.2304(3) 0.1010(18) Uani 1 1 d . . . . .
H15A H 0.4180 1.3754 0.2039 0.152 Uiso 1 1 calc R U . . .
H15B H 0.3778 1.3676 0.2888 0.152 Uiso 1 1 calc R U . . .
H15C H 0.2994 1.3850 0.2080 0.152 Uiso 1 1 calc R U . . .
C16 C 0.2865(3) 0.8672(2) -0.1850(2) 0.0559(9) Uani 1 1 d . . . . .
H16 H 0.2650 0.9111 -0.1630 0.067 Uiso 1 1 calc R U . . .
C17 C 0.2721(4) 0.8588(3) -0.2692(2) 0.0788(13) Uani 1 1 d . . . . .
H17 H 0.2424 0.8967 -0.3037 0.095 Uiso 1 1 calc R U . . .
C18 C 0.3022(4) 0.7938(3) -0.3021(3) 0.0867(14) Uani 1 1 d . . . . .
H18 H 0.2921 0.7868 -0.3591 0.104 Uiso 1 1 calc R U . . .
C19 C 0.3473(4) 0.7395(3) -0.2500(3) 0.0736(12) Uani 1 1 d . . . . .
H19 H 0.3678 0.6949 -0.2711 0.088 Uiso 1 1 calc R U . . .
C20 C 0.3620(3) 0.75167(19) -0.1656(2) 0.0517(8) Uani 1 1 d . . . . .
C21 C 0.4223(3) 0.69950(19) -0.1039(2) 0.0611(10) Uani 1 1 d . . . . .
H21A H 0.4094 0.6486 -0.1223 0.073 Uiso 1 1 calc R U . . .
H21B H 0.4961 0.7093 -0.1001 0.073 Uiso 1 1 calc R U . . .
C22 C 0.2990(3) 0.66238(19) -0.0124(3) 0.0648(11) Uani 1 1 d . . . . .
H22A H 0.2867 0.6274 -0.0580 0.078 Uiso 1 1 calc R U . . .
H22B H 0.3146 0.6340 0.0384 0.078 Uiso 1 1 calc R U . . .
C23 C 0.2030(3) 0.70623(18) -0.01055(19) 0.0469(8) Uani 1 1 d . . . . .
C24 C 0.1087(3) 0.6712(2) -0.0110(2) 0.0642(10) Uani 1 1 d . . . . .
H24 H 0.1032 0.6199 -0.0158 0.077 Uiso 1 1 calc R U . . .
C25 C 0.0224(4) 0.7142(3) -0.0041(3) 0.0837(14) Uani 1 1 d . . . . .
H25 H -0.0423 0.6925 -0.0039 0.100 Uiso 1 1 calc R U . . .
C26 C 0.0350(4) 0.7901(3) 0.0023(3) 0.0808(13) Uani 1 1 d . . . . .
H26 H -0.0216 0.8202 0.0076 0.097 Uiso 1 1 calc R U . . .
C27 C 0.1296(3) 0.8209(2) 0.0010(2) 0.0617(10) Uani 1 1 d . . . . .
H27 H 0.1364 0.8722 0.0050 0.074 Uiso 1 1 calc R U . . .
C28 C 0.4774(3) 0.69327(19) 0.0464(3) 0.0602(10) Uani 1 1 d . . . . .
H28A H 0.5423 0.7121 0.0327 0.072 Uiso 1 1 calc R U . . .
H28B H 0.4843 0.6401 0.0549 0.072 Uiso 1 1 calc R U . . .
C29 C 0.4541(3) 0.73000(19) 0.1235(2) 0.0575(9) Uani 1 1 d . . . . .
C30 C 0.4868(4) 0.7024(3) 0.2013(3) 0.0859(15) Uani 1 1 d . . . . .
H30 H 0.5246 0.6584 0.2086 0.103 Uiso 1 1 calc R U . . .
C31 C 0.4628(5) 0.7410(3) 0.2688(3) 0.107(2) Uani 1 1 d . . . . .
H31 H 0.4835 0.7229 0.3221 0.128 Uiso 1 1 calc R U . . .
C32 C 0.4091(5) 0.8053(3) 0.2565(3) 0.0894(16) Uani 1 1 d . . . . .
H32 H 0.3936 0.8322 0.3015 0.107 Uiso 1 1 calc R U . . .
C33 C 0.3776(3) 0.8305(2) 0.1774(2) 0.0606(10) Uani 1 1 d . . . . .
H33 H 0.3401 0.8746 0.1697 0.073 Uiso 1 1 calc R U . . .
Cl1 Cl 0.2606(3) 0.93719(17) 0.48700(18) 0.0705(8) Uani 0.5 1 d . U P A 1
O1 O 0.3144(9) 0.9245(7) 0.4245(7) 0.161(4) Uani 0.5 1 d . U P A 1
O2 O 0.1967(18) 0.9904(9) 0.4454(14) 0.159(6) Uani 0.5 1 d . U P A 1
O3 O 0.2929(14) 0.9810(6) 0.5610(6) 0.154(5) Uani 0.5 1 d . U P A 1
O4 O 0.2509(14) 0.8687(12) 0.5073(15) 0.157(6) Uani 0.5 1 d . U P A 1
Cl1' Cl 0.2126(5) 0.9503(3) 0.5096(3) 0.1218(16) Uani 0.5 1 d . U P B 2
O1' O 0.3222(18) 0.9725(12) 0.5128(12) 0.211(6) Uani 0.5 1 d . U P B 2
O2' O 0.1464(14) 0.9720(11) 0.4463(12) 0.151(6) Uani 0.5 1 d . U P B 2
O3' O 0.1576(17) 0.9749(8) 0.5808(8) 0.204(5) Uani 0.5 1 d . U P B 2
O4' O 0.1986(11) 0.8762(8) 0.5101(12) 0.112(4) Uani 0.5 1 d . U P B 2
O1W O 0.0532(11) 1.0049(6) 0.6053(7) 0.161(4) Uani 0.5 1 d . . P C 1
H1WA H -0.0119 1.0058 0.5884 0.193 Uiso 0.5 1 d R U P C 1
H1WB H 0.0842 1.0016 0.5635 0.193 Uiso 0.5 1 d R U P C 1


_geom_special_details            
;
 All esds (except the esd in the dihedral angle between two l.s. planes)
 are estimated using the full covariance matrix.  The cell esds are taken
 into account individually in the estimation of esds in distances, angles
 and torsion angles; correlations between esds in cell parameters are only
 used when they are defined by crystal symmetry.  An approximate (isotropic)
 treatment of cell esds is used for estimating esds involving l.s. planes.
;

loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
_geom_bond_publ_flag
Fe1 C2 1.908(3) . ?
Fe1 C3 1.920(3) . ?
Fe1 C1 1.924(3) . ?
Fe1 N6 1.970(3) . ?
Fe1 N8 1.976(2) . ?
Fe1 N4 1.980(2) . ?
Fe2 N1 1.956(3) . ?
Fe2 N2 1.967(3) 3_675 ?
Fe2 N12 1.995(3) . ?
Fe2 N10 1.996(3) . ?
Fe2 N13 2.005(3) . ?
Fe2 N11 2.040(2) . ?
B1 N5 1.529(5) . ?
B1 N9 1.538(4) . ?
B1 N7 1.550(5) . ?
B1 H1 0.9801 . ?
N1 C1 1.160(4) . ?
N2 C2 1.155(4) . ?
N2 Fe2 1.967(3) 3_675 ?
N3 C3 1.146(4) . ?
N4 C4 1.332(4) . ?
N4 N5 1.353(3) . ?
N5 C6 1.350(4) . ?
N6 C8 1.330(4) . ?
N6 N7 1.356(3) . ?
N7 C10 1.344(4) . ?
N8 C12 1.332(4) . ?
N8 N9 1.356(3) . ?
N9 C14 1.338(4) . ?
N10 C16 1.342(4) . ?
N10 C20 1.345(4) . ?
N11 C21 1.476(5) . ?
N11 C28 1.483(5) . ?
N11 C22 1.494(5) . ?
N12 C23 1.337(4) . ?
N12 C27 1.342(5) . ?
N13 C33 1.338(5) . ?
N13 C29 1.360(4) . ?
C4 C5 1.387(5) . ?
C4 H4 0.9300 . ?
C5 C6 1.370(6) . ?
C5 C7 1.504(5) . ?
C6 H6 0.9300 . ?
C7 H7A 0.9600 . ?
C7 H7B 0.9600 . ?
C7 H7C 0.9600 . ?
C8 C9 1.390(5) . ?
C8 H8 0.9300 . ?
C9 C10 1.374(5) . ?
C9 C11 1.497(6) . ?
C10 H10 0.9300 . ?
C11 H11A 0.9600 . ?
C11 H11B 0.9600 . ?
C11 H11C 0.9600 . ?
C12 C13 1.380(5) . ?
C12 H12 0.9300 . ?
C13 C14 1.373(5) . ?
C13 C15 1.503(5) . ?
C14 H14 0.9300 . ?
C15 H15A 0.9600 . ?
C15 H15B 0.9600 . ?
C15 H15C 0.9600 . ?
C16 C17 1.371(5) . ?
C16 H16 0.9300 . ?
C17 C18 1.371(7) . ?
C17 H17 0.9300 . ?
C18 C19 1.367(7) . ?
C18 H18 0.9300 . ?
C19 C20 1.380(5) . ?
C19 H19 0.9300 . ?
C20 C21 1.506(5) . ?
C21 H21A 0.9700 . ?
C21 H21B 0.9700 . ?
C22 C23 1.484(5) . ?
C22 H22A 0.9700 . ?
C22 H22B 0.9700 . ?
C23 C24 1.381(5) . ?
C24 C25 1.385(7) . ?
C24 H24 0.9300 . ?
C25 C26 1.377(7) . ?
C25 H25 0.9300 . ?
C26 C27 1.356(6) . ?
C26 H26 0.9300 . ?
C27 H27 0.9300 . ?
C28 C29 1.497(6) . ?
C28 H28A 0.9700 . ?
C28 H28B 0.9700 . ?
C29 C30 1.371(6) . ?
C30 C31 1.383(8) . ?
C30 H30 0.9300 . ?
C31 C32 1.351(8) . ?
C31 H31 0.9300 . ?
C32 C33 1.373(6) . ?
C32 H32 0.9300 . ?
C33 H33 0.9300 . ?
Cl1 O4 1.29(2) . ?
Cl1 O1 1.348(11) . ?
Cl1 O2 1.38(2) . ?
Cl1 O3 1.451(9) . ?
Cl1' O2' 1.298(18) . ?
Cl1' O4' 1.346(15) . ?
Cl1' O1' 1.48(2) . ?
Cl1' O3' 1.529(19) . ?
O1W H1WA 0.8501 . ?
O1W H1WB 0.8500 . ?

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
C2 Fe1 C3 86.50(13) . . ?
C2 Fe1 C1 94.44(12) . . ?
C3 Fe1 C1 90.21(13) . . ?
C2 Fe1 N6 174.72(11) . . ?
C3 Fe1 N6 94.33(13) . . ?
C1 Fe1 N6 90.77(11) . . ?
C2 Fe1 N8 89.19(11) . . ?
C3 Fe1 N8 94.12(13) . . ?
C1 Fe1 N8 174.51(11) . . ?
N6 Fe1 N8 85.55(10) . . ?
C2 Fe1 N4 89.27(11) . . ?
C3 Fe1 N4 174.51(12) . . ?
C1 Fe1 N4 86.62(11) . . ?
N6 Fe1 N4 90.19(11) . . ?
N8 Fe1 N4 89.32(10) . . ?
N1 Fe2 N2 86.82(11) . 3_675 ?
N1 Fe2 N12 95.09(11) . . ?
N2 Fe2 N12 177.68(10) 3_675 . ?
N1 Fe2 N10 98.26(11) . . ?
N2 Fe2 N10 88.02(11) 3_675 . ?
N12 Fe2 N10 90.40(11) . . ?
N1 Fe2 N13 97.93(11) . . ?
N2 Fe2 N13 90.73(11) 3_675 . ?
N12 Fe2 N13 90.31(11) . . ?
N10 Fe2 N13 163.67(11) . . ?
N1 Fe2 N11 178.37(11) . . ?
N2 Fe2 N11 94.74(11) 3_675 . ?
N12 Fe2 N11 83.36(11) . . ?
N10 Fe2 N11 82.30(11) . . ?
N13 Fe2 N11 81.57(11) . . ?
N5 B1 N9 107.1(3) . . ?
N5 B1 N7 108.4(3) . . ?
N9 B1 N7 105.1(3) . . ?
N5 B1 H1 111.9 . . ?
N9 B1 H1 112.0 . . ?
N7 B1 H1 112.0 . . ?
C1 N1 Fe2 165.7(3) . . ?
C2 N2 Fe2 165.0(2) . 3_675 ?
C4 N4 N5 107.3(2) . . ?
C4 N4 Fe1 132.1(2) . . ?
N5 N4 Fe1 120.6(2) . . ?
C6 N5 N4 108.4(3) . . ?
C6 N5 B1 133.6(3) . . ?
N4 N5 B1 117.5(2) . . ?
C8 N6 N7 106.7(3) . . ?
C8 N6 Fe1 133.2(2) . . ?
N7 N6 Fe1 119.0(2) . . ?
C10 N7 N6 108.8(3) . . ?
C10 N7 B1 131.0(3) . . ?
N6 N7 B1 119.2(3) . . ?
C12 N8 N9 106.9(2) . . ?
C12 N8 Fe1 134.3(2) . . ?
N9 N8 Fe1 118.29(18) . . ?
C14 N9 N8 108.9(3) . . ?
C14 N9 B1 131.4(3) . . ?
N8 N9 B1 119.6(2) . . ?
C16 N10 C20 117.9(3) . . ?
C16 N10 Fe2 127.0(2) . . ?
C20 N10 Fe2 115.1(2) . . ?
C21 N11 C28 112.1(3) . . ?
C21 N11 C22 111.6(3) . . ?
C28 N11 C22 109.7(3) . . ?
C21 N11 Fe2 107.7(2) . . ?
C28 N11 Fe2 105.44(19) . . ?
C22 N11 Fe2 110.1(2) . . ?
C23 N12 C27 117.9(3) . . ?
C23 N12 Fe2 116.0(2) . . ?
C27 N12 Fe2 126.1(2) . . ?
C33 N13 C29 117.6(3) . . ?
C33 N13 Fe2 129.1(3) . . ?
C29 N13 Fe2 113.2(2) . . ?
N1 C1 Fe1 167.0(3) . . ?
N2 C2 Fe1 170.6(3) . . ?
N3 C3 Fe1 177.2(3) . . ?
N4 C4 C5 110.6(3) . . ?
N4 C4 H4 124.7 . . ?
C5 C4 H4 124.7 . . ?
C6 C5 C4 104.1(3) . . ?
C6 C5 C7 129.4(4) . . ?
C4 C5 C7 126.4(4) . . ?
N5 C6 C5 109.6(3) . . ?
N5 C6 H6 125.2 . . ?
C5 C6 H6 125.2 . . ?
C5 C7 H7A 109.5 . . ?
C5 C7 H7B 109.5 . . ?
H7A C7 H7B 109.5 . . ?
C5 C7 H7C 109.5 . . ?
H7A C7 H7C 109.5 . . ?
H7B C7 H7C 109.5 . . ?
N6 C8 C9 111.2(3) . . ?
N6 C8 H8 124.4 . . ?
C9 C8 H8 124.4 . . ?
C10 C9 C8 103.6(3) . . ?
C10 C9 C11 127.3(4) . . ?
C8 C9 C11 129.1(4) . . ?
N7 C10 C9 109.7(3) . . ?
N7 C10 H10 125.1 . . ?
C9 C10 H10 125.1 . . ?
C9 C11 H11A 109.5 . . ?
C9 C11 H11B 109.5 . . ?
H11A C11 H11B 109.5 . . ?
C9 C11 H11C 109.5 . . ?
H11A C11 H11C 109.5 . . ?
H11B C11 H11C 109.5 . . ?
N8 C12 C13 110.4(3) . . ?
N8 C12 H12 124.8 . . ?
C13 C12 H12 124.8 . . ?
C14 C13 C12 104.6(3) . . ?
C14 C13 C15 126.3(4) . . ?
C12 C13 C15 129.1(4) . . ?
N9 C14 C13 109.1(3) . . ?
N9 C14 H14 125.4 . . ?
C13 C14 H14 125.4 . . ?
C13 C15 H15A 109.5 . . ?
C13 C15 H15B 109.5 . . ?
H15A C15 H15B 109.5 . . ?
C13 C15 H15C 109.5 . . ?
H15A C15 H15C 109.5 . . ?
H15B C15 H15C 109.5 . . ?
N10 C16 C17 122.5(4) . . ?
N10 C16 H16 118.7 . . ?
C17 C16 H16 118.7 . . ?
C16 C17 C18 119.1(4) . . ?
C16 C17 H17 120.4 . . ?
C18 C17 H17 120.4 . . ?
C19 C18 C17 119.2(4) . . ?
C19 C18 H18 120.4 . . ?
C17 C18 H18 120.4 . . ?
C18 C19 C20 119.2(4) . . ?
C18 C19 H19 120.4 . . ?
C20 C19 H19 120.4 . . ?
N10 C20 C19 122.0(4) . . ?
N10 C20 C21 114.6(3) . . ?
C19 C20 C21 123.1(3) . . ?
N11 C21 C20 110.2(3) . . ?
N11 C21 H21A 109.6 . . ?
C20 C21 H21A 109.6 . . ?
N11 C21 H21B 109.6 . . ?
C20 C21 H21B 109.6 . . ?
H21A C21 H21B 108.1 . . ?
C23 C22 N11 113.2(3) . . ?
C23 C22 H22A 108.9 . . ?
N11 C22 H22A 108.9 . . ?
C23 C22 H22B 108.9 . . ?
N11 C22 H22B 108.9 . . ?
H22A C22 H22B 107.8 . . ?
N12 C23 C24 122.7(4) . . ?
N12 C23 C22 116.6(3) . . ?
C24 C23 C22 120.7(3) . . ?
C23 C24 C25 118.6(4) . . ?
C23 C24 H24 120.7 . . ?
C25 C24 H24 120.7 . . ?
C26 C25 C24 118.2(4) . . ?
C26 C25 H25 120.9 . . ?
C24 C25 H25 120.9 . . ?
C27 C26 C25 120.1(4) . . ?
C27 C26 H26 119.9 . . ?
C25 C26 H26 119.9 . . ?
N12 C27 C26 122.4(4) . . ?
N12 C27 H27 118.8 . . ?
C26 C27 H27 118.8 . . ?
N11 C28 C29 108.4(3) . . ?
N11 C28 H28A 110.0 . . ?
C29 C28 H28A 110.0 . . ?
N11 C28 H28B 110.0 . . ?
C29 C28 H28B 110.0 . . ?
H28A C28 H28B 108.4 . . ?
N13 C29 C30 121.9(4) . . ?
N13 C29 C28 114.8(3) . . ?
C30 C29 C28 123.2(4) . . ?
C29 C30 C31 119.0(5) . . ?
C29 C30 H30 120.5 . . ?
C31 C30 H30 120.5 . . ?
C32 C31 C30 119.3(4) . . ?
C32 C31 H31 120.3 . . ?
C30 C31 H31 120.3 . . ?
C31 C32 C33 119.6(5) . . ?
C31 C32 H32 120.2 . . ?
C33 C32 H32 120.2 . . ?
N13 C33 C32 122.5(4) . . ?
N13 C33 H33 118.7 . . ?
C32 C33 H33 118.7 . . ?
O4 Cl1 O1 96.7(11) . . ?
O4 Cl1 O2 135.8(12) . . ?
O1 Cl1 O2 95.2(11) . . ?
O4 Cl1 O3 109.4(12) . . ?
O1 Cl1 O3 127.5(10) . . ?
O2 Cl1 O3 96.1(11) . . ?
O2' Cl1' O4' 103.3(12) . . ?
O2' Cl1' O1' 117.6(12) . . ?
O4' Cl1' O1' 113.6(12) . . ?
O2' Cl1' O3' 100.9(12) . . ?
O4' Cl1' O3' 101.6(9) . . ?
O1' Cl1' O3' 117.6(10) . . ?
H1WA O1W H1WB 108.5 . . ?

loop_
_geom_torsion_atom_site_label_1
_geom_torsion_atom_site_label_2
_geom_torsion_atom_site_label_3
_geom_torsion_atom_site_label_4
_geom_torsion
_geom_torsion_site_symmetry_1
_geom_torsion_site_symmetry_2
_geom_torsion_site_symmetry_3
_geom_torsion_site_symmetry_4
_geom_torsion_publ_flag
C4 N4 N5 C6 0.9(3) . . . . ?
Fe1 N4 N5 C6 -178.9(2) . . . . ?
C4 N4 N5 B1 174.3(3) . . . . ?
Fe1 N4 N5 B1 -5.5(3) . . . . ?
N9 B1 N5 C6 117.7(4) . . . . ?
N7 B1 N5 C6 -129.3(4) . . . . ?
N9 B1 N5 N4 -53.6(4) . . . . ?
N7 B1 N5 N4 59.4(3) . . . . ?
C8 N6 N7 C10 -0.8(3) . . . . ?
Fe1 N6 N7 C10 168.67(19) . . . . ?
C8 N6 N7 B1 -170.6(3) . . . . ?
Fe1 N6 N7 B1 -1.2(3) . . . . ?
N5 B1 N7 C10 136.7(3) . . . . ?
N9 B1 N7 C10 -109.1(3) . . . . ?
N5 B1 N7 N6 -56.1(3) . . . . ?
N9 B1 N7 N6 58.1(3) . . . . ?
C12 N8 N9 C14 -1.0(4) . . . . ?
Fe1 N8 N9 C14 172.2(2) . . . . ?
C12 N8 N9 B1 176.3(3) . . . . ?
Fe1 N8 N9 B1 -10.5(4) . . . . ?
N5 B1 N9 C14 -119.4(4) . . . . ?
N7 B1 N9 C14 125.5(4) . . . . ?
N5 B1 N9 N8 64.0(4) . . . . ?
N7 B1 N9 N8 -51.1(4) . . . . ?
Fe2 N1 C1 Fe1 -36(2) . . . . ?
N5 N4 C4 C5 -0.3(3) . . . . ?
Fe1 N4 C4 C5 179.5(2) . . . . ?
N4 C4 C5 C6 -0.5(4) . . . . ?
N4 C4 C5 C7 178.2(4) . . . . ?
N4 N5 C6 C5 -1.2(4) . . . . ?
B1 N5 C6 C5 -173.1(3) . . . . ?
C4 C5 C6 N5 1.0(4) . . . . ?
C7 C5 C6 N5 -177.6(4) . . . . ?
N7 N6 C8 C9 0.7(3) . . . . ?
Fe1 N6 C8 C9 -166.6(2) . . . . ?
N6 C8 C9 C10 -0.4(4) . . . . ?
N6 C8 C9 C11 179.8(4) . . . . ?
N6 N7 C10 C9 0.6(3) . . . . ?
B1 N7 C10 C9 168.8(3) . . . . ?
C8 C9 C10 N7 -0.1(3) . . . . ?
C11 C9 C10 N7 179.7(4) . . . . ?
N9 N8 C12 C13 1.4(4) . . . . ?
Fe1 N8 C12 C13 -170.2(3) . . . . ?
N8 C12 C13 C14 -1.2(5) . . . . ?
N8 C12 C13 C15 177.3(5) . . . . ?
N8 N9 C14 C13 0.3(4) . . . . ?
B1 N9 C14 C13 -176.6(4) . . . . ?
C12 C13 C14 N9 0.5(5) . . . . ?
C15 C13 C14 N9 -178.0(4) . . . . ?
C20 N10 C16 C17 0.6(5) . . . . ?
Fe2 N10 C16 C17 179.9(3) . . . . ?
N10 C16 C17 C18 1.0(7) . . . . ?
C16 C17 C18 C19 -1.0(8) . . . . ?
C17 C18 C19 C20 -0.4(8) . . . . ?
C16 N10 C20 C19 -2.2(5) . . . . ?
Fe2 N10 C20 C19 178.5(3) . . . . ?
C16 N10 C20 C21 172.7(3) . . . . ?
Fe2 N10 C20 C21 -6.6(4) . . . . ?
C18 C19 C20 N10 2.1(7) . . . . ?
C18 C19 C20 C21 -172.3(4) . . . . ?
C28 N11 C21 C20 -149.5(3) . . . . ?
C22 N11 C21 C20 86.9(3) . . . . ?
Fe2 N11 C21 C20 -34.0(3) . . . . ?
N10 C20 C21 N11 27.7(4) . . . . ?
C19 C20 C21 N11 -157.5(4) . . . . ?
C21 N11 C22 C23 -110.1(3) . . . . ?
C28 N11 C22 C23 125.1(3) . . . . ?
Fe2 N11 C22 C23 9.4(4) . . . . ?
C27 N12 C23 C24 1.8(5) . . . . ?
Fe2 N12 C23 C24 -178.3(3) . . . . ?
C27 N12 C23 C22 -176.1(3) . . . . ?
Fe2 N12 C23 C22 3.8(4) . . . . ?
N11 C22 C23 N12 -8.9(5) . . . . ?
N11 C22 C23 C24 173.1(3) . . . . ?
N12 C23 C24 C25 -1.7(5) . . . . ?
C22 C23 C24 C25 176.1(4) . . . . ?
C23 C24 C25 C26 0.4(6) . . . . ?
C24 C25 C26 C27 0.7(7) . . . . ?
C23 N12 C27 C26 -0.7(5) . . . . ?
Fe2 N12 C27 C26 179.4(3) . . . . ?
C25 C26 C27 N12 -0.5(7) . . . . ?
C21 N11 C28 C29 159.5(3) . . . . ?
C22 N11 C28 C29 -75.9(3) . . . . ?
Fe2 N11 C28 C29 42.6(3) . . . . ?
C33 N13 C29 C30 0.4(5) . . . . ?
Fe2 N13 C29 C30 -177.6(3) . . . . ?
C33 N13 C29 C28 -178.6(3) . . . . ?
Fe2 N13 C29 C28 3.5(4) . . . . ?
N11 C28 C29 N13 -31.6(4) . . . . ?
N11 C28 C29 C30 149.5(4) . . . . ?
N13 C29 C30 C31 0.1(7) . . . . ?
C28 C29 C30 C31 178.9(4) . . . . ?
C29 C30 C31 C32 -0.9(8) . . . . ?
C30 C31 C32 C33 1.2(8) . . . . ?
C29 N13 C33 C32 -0.1(5) . . . . ?
Fe2 N13 C33 C32 177.5(3) . . . . ?
C31 C32 C33 N13 -0.7(7) . . . . ?

loop_
_geom_hbond_atom_site_label_D
_geom_hbond_atom_site_label_H
_geom_hbond_atom_site_label_A
_geom_hbond_distance_DH
_geom_hbond_distance_HA
_geom_hbond_distance_DA
_geom_hbond_angle_DHA
_geom_hbond_site_symmetry_A
O1W H1WB O2 0.85 2.61 3.46(3) 174.3 .
O1W H1WA O2 0.85 2.38 3.23(3) 174.5 3_576
C28 H28A O4' 0.97 2.66 3.283(12) 122.6 4_675
C27 H27 N1 0.93 2.56 3.083(5) 115.6 .
C26 H26 N3 0.93 2.41 3.267(6) 154.1 3_575
C22 H22B O2 0.97 2.61 3.28(2) 127.0 2_545
C21 H21A O1W 0.97 2.64 3.520(11) 150.8 2_545
C17 H17 O3' 0.93 2.47 3.383(14) 167.0 1_554
C12 H12 O4' 0.93 2.63 3.481(17) 152.5 2
C12 H12 O4 0.93 2.59 3.42(2) 147.6 2
C10 H10 O2' 0.93 2.57 3.38(2) 146.9 .
C10 H10 O2 0.93 2.52 3.29(2) 139.9 .
O1W H1WB O2 0.85 2.61 3.46(3) 174.3 .
O1W H1WA O2 0.85 2.38 3.23(3) 174.5 3_576
C27 H27 N1 0.93 2.56 3.083(5) 115.6 .
C26 H26 N3 0.93 2.41 3.267(6) 154.1 3_575
C22 H22B O2 0.97 2.61 3.28(2) 127.0 2_545
C21 H21A O1W 0.97 2.64 3.520(11) 150.8 2_545
C17 H17 O3' 0.93 2.47 3.383(14) 167.0 1_554
C12 H12 O4' 0.93 2.63 3.481(17) 152.5 2
C12 H12 O4 0.93 2.59 3.42(2) 147.6 2
C10 H10 O2' 0.93 2.57 3.38(2) 146.9 .
C10 H10 O2 0.93 2.52 3.29(2) 139.9 .

_refine_diff_density_max         0.473
_refine_diff_density_min         -0.470
_refine_diff_density_rms         0.070

####################################################################### 
# 
# 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_3_MeOH-100K
_database_code_depnum_ccdc_archive 'CCDC 1419285'
_audit_update_record             
;
2016-09-02 deposited with the CCDC.
2016-09-26 downloaded from the CCDC.
;

_audit_creation_method           SHELXL-2014/7
_shelx_SHELXL_version_number     2014/7
_chemical_name_systematic        ?
_chemical_name_common            ?
_chemical_melting_point          ?
_chemical_formula_moiety         'C62 H60 B2 Fe4 N26, 2(Cl O4), C H4 O '
_chemical_formula_sum            'C63 H64 B2 Cl2 Fe4 N26 O9'
_chemical_formula_weight         1645.32

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'
N N 0.0061 0.0033 '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'
O O 0.0106 0.0060 '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'

_space_group_crystal_system      monoclinic
_space_group_IT_number           14
_space_group_name_H-M_alt        'P 21/c'
_space_group_name_Hall           '-P 2ybc'

_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.
;

loop_
_space_group_symop_operation_xyz
'x, y, z'
'-x, y+1/2, -z+1/2'
'-x, -y, -z'
'x, -y-1/2, z-1/2'

_cell_length_a                   12.858(3)
_cell_length_b                   17.264(4)
_cell_length_c                   16.783(4)
_cell_angle_alpha                90
_cell_angle_beta                 109.315(4)
_cell_angle_gamma                90
_cell_volume                     3515.9(13)
_cell_formula_units_Z            2
_cell_measurement_temperature    100(2)
_cell_measurement_reflns_used    5263
_cell_measurement_theta_min      2.56
_cell_measurement_theta_max      26.71

_exptl_crystal_description       block
_exptl_crystal_colour            red
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    'not measured'
_exptl_crystal_density_diffrn    1.554
_exptl_crystal_F_000             1688
_exptl_transmission_factor_min   ?
_exptl_transmission_factor_max   ?
_exptl_crystal_size_max          0.100
_exptl_crystal_size_mid          0.050
_exptl_crystal_size_min          0.050
_exptl_absorpt_coefficient_mu    0.961
_shelx_estimated_absorpt_T_min   0.910
_shelx_estimated_absorpt_T_max   0.954
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_correction_T_min  0.9100
_exptl_absorpt_correction_T_max  0.9535
_exptl_absorpt_process_details   sadabs
_exptl_absorpt_special_details   ?
_diffrn_ambient_temperature      100(2)
_diffrn_radiation_wavelength     0.71073
_diffrn_radiation_type           MoK\a
_diffrn_source                   ?
_diffrn_measurement_device_type  'Bruker APEX-II CCD'
_diffrn_measurement_method       'φ and ω scans'
_diffrn_detector_area_resol_mean ?
_diffrn_reflns_number            26447
_diffrn_reflns_av_unetI/netI     0.0750
_diffrn_reflns_av_R_equivalents  0.0918
_diffrn_reflns_limit_h_min       -15
_diffrn_reflns_limit_h_max       15
_diffrn_reflns_limit_k_min       -20
_diffrn_reflns_limit_k_max       20
_diffrn_reflns_limit_l_min       -19
_diffrn_reflns_limit_l_max       19
_diffrn_reflns_theta_min         1.678
_diffrn_reflns_theta_max         24.997
_diffrn_reflns_theta_full        24.997
_diffrn_measured_fraction_theta_max 0.998
_diffrn_measured_fraction_theta_full 0.998
_diffrn_reflns_Laue_measured_fraction_max 0.998
_diffrn_reflns_Laue_measured_fraction_full 0.998
_diffrn_reflns_point_group_measured_fraction_max 0.998
_diffrn_reflns_point_group_measured_fraction_full 0.998
_reflns_number_total             6184
_reflns_number_gt                4541
_reflns_threshold_expression     'I > 2σ(I)'
_reflns_Friedel_coverage         0.000
_reflns_Friedel_fraction_max     .
_reflns_Friedel_fraction_full    .

_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.
;

_computing_data_collection       'Bruker APEX2'
_computing_cell_refinement       'Bruker SAINT'
_computing_data_reduction        'Bruker SAINT'
_computing_structure_solution    'SHELXS-2014 (Sheldrick, 2014)'
_computing_structure_refinement  'SHELXL-2014/7 (Sheldrick, 2014)'
_computing_molecular_graphics    'Bruker SHELXTL'
_computing_publication_material  'Bruker SHELXTL'
_refine_special_details          ?
_refine_ls_structure_factor_coef Fsqd
_refine_ls_matrix_type           full
_refine_ls_weighting_scheme      calc
_refine_ls_weighting_details     
'w=1/[σ²(Fo²)+(0.0827P)²+10.5120P] where P=(Fo²+2Fc²)/3'
_atom_sites_solution_primary     ?
_atom_sites_solution_secondary   ?
_atom_sites_solution_hydrogens   mixed
_refine_ls_hydrogen_treatment    constr
_refine_ls_extinction_method     none
_refine_ls_extinction_coef       .
_refine_ls_number_reflns         6184
_refine_ls_number_parameters     534
_refine_ls_number_restraints     182
_refine_ls_R_factor_all          0.0949
_refine_ls_R_factor_gt           0.0636
_refine_ls_wR_factor_ref         0.1782
_refine_ls_wR_factor_gt          0.1522
_refine_ls_goodness_of_fit_ref   1.079
_refine_ls_restrained_S_all      1.103
_refine_ls_shift/su_max          0.001
_refine_ls_shift/su_mean         0.000

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 0.25961(6) 0.57781(4) 0.92889(4) 0.0200(2) Uani 1 1 d . . . . .
Fe2 Fe 0.37590(5) 0.31776(4) 1.04028(4) 0.0181(2) Uani 1 1 d . . . . .
B1 B 0.1246(6) 0.5703(5) 0.7351(5) 0.0444(19) Uani 1 1 d . . . . .
N1 N 0.3332(4) 0.4257(2) 1.0250(3) 0.0229(9) Uani 1 1 d . . . . .
N2 N 0.4880(3) 0.6526(2) 0.9783(2) 0.0206(9) Uani 1 1 d . . . . .
N3 N 0.2066(4) 0.6525(3) 1.0774(3) 0.0333(11) Uani 1 1 d . . . . .
N4 N 0.3040(4) 0.5268(2) 0.8395(3) 0.0297(11) Uani 1 1 d . . . . .
N5 N 0.2368(4) 0.5287(3) 0.7574(3) 0.0445(14) Uani 1 1 d . . . . .
N6 N 0.2022(3) 0.6667(2) 0.8536(2) 0.0226(9) Uani 1 1 d . . . . .
N7 N 0.1496(4) 0.6550(3) 0.7695(3) 0.0340(11) Uani 1 1 d . . . . .
N8 N 0.1126(4) 0.5315(2) 0.8771(3) 0.0302(11) Uani 1 1 d . . . . .
N9 N 0.0646(4) 0.5321(3) 0.7924(3) 0.0405(13) Uani 1 1 d . . . . .
N10 N 0.4609(4) 0.3184(3) 1.1630(3) 0.0335(12) Uani 1 1 d . . . . .
N11 N 0.4173(3) 0.2061(2) 1.0529(3) 0.0280(10) Uani 1 1 d . . . . .
N12 N 0.2382(3) 0.2833(2) 1.0573(2) 0.0210(9) Uani 1 1 d . . . . .
N13 N 0.3004(3) 0.2892(2) 0.9199(2) 0.0201(9) Uani 1 1 d . . . . .
C1 C 0.3088(4) 0.4865(3) 0.9970(3) 0.0252(11) Uani 1 1 d . . . . .
C2 C 0.4026(4) 0.6249(3) 0.9686(3) 0.0215(11) Uani 1 1 d . . . . .
C3 C 0.2250(4) 0.6244(3) 1.0212(3) 0.0219(11) Uani 1 1 d . . . . .
C4 C 0.3937(5) 0.4858(3) 0.8427(4) 0.0408(15) Uani 1 1 d . . . . .
H4 H 0.4540 0.4755 0.8925 0.049 Uiso 1 1 calc R U . . .
C5 C 0.3854(6) 0.4605(5) 0.7624(5) 0.070(3) Uani 1 1 d . . . . .
H5 H 0.4373 0.4304 0.7467 0.084 Uiso 1 1 calc R U . . .
C6 C 0.2869(6) 0.4881(5) 0.7109(5) 0.069(2) Uani 1 1 d . U . . .
H6 H 0.2577 0.4802 0.6516 0.083 Uiso 1 1 calc R U . . .
C7 C 0.2039(4) 0.7425(3) 0.8671(3) 0.0241(11) Uani 1 1 d . . . . .
H7 H 0.2350 0.7667 0.9206 0.029 Uiso 1 1 calc R U . . .
C8 C 0.1533(5) 0.7813(4) 0.7914(4) 0.0395(15) Uani 1 1 d . . . . .
H8 H 0.1435 0.8356 0.7830 0.047 Uiso 1 1 calc R U . . .
C9 C 0.1208(5) 0.7237(4) 0.7315(4) 0.0462(17) Uani 1 1 d . . . . .
H9 H 0.0839 0.7314 0.6729 0.055 Uiso 1 1 calc R U . . .
C10 C 0.0433(5) 0.4947(3) 0.9091(4) 0.0399(16) Uani 1 1 d . . . . .
H10 H 0.0570 0.4857 0.9675 0.048 Uiso 1 1 calc R U . . .
C11 C -0.0507(6) 0.4719(4) 0.8452(5) 0.064(2) Uani 1 1 d . . . . .
H11 H -0.1128 0.4452 0.8503 0.076 Uiso 1 1 calc R U . . .
C12 C -0.0343(6) 0.4964(4) 0.7731(5) 0.061(2) Uani 1 1 d . . . . .
H12 H -0.0847 0.4894 0.7176 0.074 Uiso 1 1 calc R U . . .
C13 C 0.0561(6) 0.5663(6) 0.6377(4) 0.074(3) Uani 1 1 d . . . . .
H13A H 0.0972 0.5921 0.6054 0.111 Uiso 1 1 calc R U . . .
H13B H -0.0150 0.5923 0.6272 0.111 Uiso 1 1 calc R U . . .
H13C H 0.0435 0.5120 0.6201 0.111 Uiso 1 1 calc R U . . .
C14 C 0.4611(6) 0.3727(5) 1.2199(4) 0.054(2) Uani 1 1 d . . . . .
H14 H 0.4132 0.4161 1.2036 0.065 Uiso 1 1 calc R U . . .
C15 C 0.5330(7) 0.3655(6) 1.3045(4) 0.071(3) Uani 1 1 d . U . . .
H15 H 0.5348 0.4048 1.3446 0.085 Uiso 1 1 calc R U . . .
C16 C 0.5986(7) 0.3029(7) 1.3277(5) 0.081(3) Uani 1 1 d . U . . .
H16 H 0.6450 0.2974 1.3847 0.097 Uiso 1 1 calc R U . . .
C17 C 0.5990(6) 0.2469(6) 1.2696(5) 0.071(2) Uani 1 1 d . U . . .
H17 H 0.6458 0.2030 1.2854 0.085 Uiso 1 1 calc R U . . .
C18 C 0.5292(5) 0.2564(5) 1.1878(4) 0.050(2) Uani 1 1 d . . . . .
C19 C 0.5276(4) 0.2009(4) 1.1194(4) 0.0408(16) Uani 1 1 d . . . . .
H19A H 0.5861 0.2142 1.0954 0.049 Uiso 1 1 calc R U . . .
H19B H 0.5407 0.1475 1.1421 0.049 Uiso 1 1 calc R U . . .
C20 C 0.3346(4) 0.1618(3) 1.0801(5) 0.0411(16) Uani 1 1 d . . . . .
H20A H 0.3655 0.1510 1.1414 0.049 Uiso 1 1 calc R U . . .
H20B H 0.3194 0.1116 1.0501 0.049 Uiso 1 1 calc R U . . .
C21 C 0.2285(4) 0.2062(3) 1.0620(4) 0.0287(12) Uani 1 1 d . . . . .
C22 C 0.1285(5) 0.1704(3) 1.0540(5) 0.0431(16) Uani 1 1 d . . . . .
H22 H 0.1231 0.1156 1.0550 0.052 Uiso 1 1 calc R U . . .
C23 C 0.0374(4) 0.2165(4) 1.0445(4) 0.0424(16) Uani 1 1 d . . . . .
H23 H -0.0320 0.1938 1.0388 0.051 Uiso 1 1 calc R U . . .
C24 C 0.0486(4) 0.2958(3) 1.0434(4) 0.0325(13) Uani 1 1 d . . . . .
H24 H -0.0125 0.3286 1.0388 0.039 Uiso 1 1 calc R U . . .
C25 C 0.1493(4) 0.3270(3) 1.0491(3) 0.0267(11) Uani 1 1 d . . . . .
H25 H 0.1560 0.3817 1.0471 0.032 Uiso 1 1 calc R U . . .
C26 C 0.4191(5) 0.1802(3) 0.9687(4) 0.0355(14) Uani 1 1 d . . . . .
H26A H 0.4134 0.1230 0.9646 0.043 Uiso 1 1 calc R U . . .
H26B H 0.4891 0.1960 0.9609 0.043 Uiso 1 1 calc R U . . .
C27 C 0.3239(4) 0.2165(3) 0.9023(4) 0.0277(12) Uani 1 1 d . . . . .
C28 C 0.2641(5) 0.1799(4) 0.8282(4) 0.0466(17) Uani 1 1 d . . . . .
H28 H 0.2804 0.1280 0.8177 0.056 Uiso 1 1 calc R U . . .
C29 C 0.1797(5) 0.2202(4) 0.7689(4) 0.0509(19) Uani 1 1 d . . . . .
H29 H 0.1383 0.1963 0.7172 0.061 Uiso 1 1 calc R U . . .
C30 C 0.1567(5) 0.2947(4) 0.7859(4) 0.0407(15) Uani 1 1 d . . . . .
H30 H 0.0997 0.3232 0.7461 0.049 Uiso 1 1 calc R U . . .
C31 C 0.2189(4) 0.3279(3) 0.8629(3) 0.0245(11) Uani 1 1 d . . . . .
H31 H 0.2029 0.3793 0.8752 0.029 Uiso 1 1 calc R U . . .
Cl1 Cl 0.2457(3) 0.55236(17) 0.45474(19) 0.0196(6) Uani 0.5 1 d . U P A 1
O1 O 0.1437(6) 0.5928(4) 0.4177(5) 0.0371(18) Uani 0.5 1 d . U P A 1
O2 O 0.2452(7) 0.4839(5) 0.4047(5) 0.0399(19) Uani 0.5 1 d . U P A 1
O3 O 0.2564(8) 0.5280(5) 0.5379(5) 0.046(2) Uani 0.5 1 d . U P A 1
O4 O 0.3355(7) 0.6021(5) 0.4563(6) 0.045(2) Uani 0.5 1 d . U P A 1
Cl1' Cl 0.3010(3) 0.53902(19) 0.4655(2) 0.0344(8) Uani 0.5 1 d . U P B 2
O1' O 0.2226(7) 0.4851(5) 0.4752(6) 0.047(2) Uani 0.5 1 d . U P B 2
O2' O 0.2907(8) 0.5418(5) 0.3783(5) 0.048(2) Uani 0.5 1 d . U P B 2
O3' O 0.4067(8) 0.5148(5) 0.5160(6) 0.062(3) Uani 0.5 1 d . U P B 2
O4' O 0.2817(9) 0.6146(5) 0.4938(6) 0.054(2) Uani 0.5 1 d . U P B 2
C1S C 0.3219(9) 0.5370(6) 0.2439(7) 0.034(3) Uani 0.5 1 d . . P C 1
H1SA H 0.2867 0.5835 0.2567 0.051 Uiso 0.5 1 calc R U P C 1
H1SB H 0.2689 0.4942 0.2303 0.051 Uiso 0.5 1 calc R U P C 1
H1SC H 0.3465 0.5472 0.1955 0.051 Uiso 0.5 1 calc R U P C 1
O1S O 0.4135(6) 0.5169(5) 0.3147(5) 0.0351(18) Uani 0.5 1 d . . P C 1
H1S H 0.3968 0.5285 0.3664 0.053 Uiso 0.5 1 d R U P C 1


_geom_special_details            
;
 All esds (except the esd in the dihedral angle between two l.s. planes)
 are estimated using the full covariance matrix.  The cell esds are taken
 into account individually in the estimation of esds in distances, angles
 and torsion angles; correlations between esds in cell parameters are only
 used when they are defined by crystal symmetry.  An approximate (isotropic)
 treatment of cell esds is used for estimating esds involving l.s. planes.
;

loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
_geom_bond_publ_flag
Fe1 C2 1.917(5) . ?
Fe1 C3 1.924(5) . ?
Fe1 C1 1.927(5) . ?
Fe1 N6 1.970(4) . ?
Fe1 N8 1.970(5) . ?
Fe1 N4 1.979(4) . ?
Fe2 N1 1.935(4) . ?
Fe2 N2 1.945(4) 3_667 ?
Fe2 N12 1.977(4) . ?
Fe2 N10 1.987(4) . ?
Fe2 N13 1.992(4) . ?
Fe2 N11 1.993(4) . ?
B1 N5 1.543(10) . ?
B1 N9 1.563(8) . ?
B1 N7 1.566(9) . ?
B1 C13 1.582(10) . ?
N1 C1 1.151(6) . ?
N2 C2 1.159(6) . ?
N2 Fe2 1.945(4) 3_667 ?
N3 C3 1.152(6) . ?
N4 C4 1.340(7) . ?
N4 N5 1.362(7) . ?
N5 C6 1.359(8) . ?
N6 C7 1.327(6) . ?
N6 N7 1.363(6) . ?
N7 C9 1.340(8) . ?
N8 C10 1.342(7) . ?
N8 N9 1.350(7) . ?
N9 C12 1.353(7) . ?
N10 C14 1.337(9) . ?
N10 C18 1.360(9) . ?
N11 C19 1.489(7) . ?
N11 C26 1.489(8) . ?
N11 C20 1.500(6) . ?
N12 C25 1.338(7) . ?
N12 C21 1.341(7) . ?
N13 C31 1.340(6) . ?
N13 C27 1.348(7) . ?
C4 C5 1.387(9) . ?
C4 H4 0.9500 . ?
C5 C6 1.361(12) . ?
C5 H5 0.9500 . ?
C6 H6 0.9500 . ?
C7 C8 1.392(8) . ?
C7 H7 0.9500 . ?
C8 C9 1.378(10) . ?
C8 H8 0.9500 . ?
C9 H9 0.9500 . ?
C10 C11 1.382(10) . ?
C10 H10 0.9500 . ?
C11 C12 1.362(11) . ?
C11 H11 0.9500 . ?
C12 H12 0.9500 . ?
C13 H13A 0.9800 . ?
C13 H13B 0.9800 . ?
C13 H13C 0.9800 . ?
C14 C15 1.421(10) . ?
C14 H14 0.9500 . ?
C15 C16 1.347(13) . ?
C15 H15 0.9500 . ?
C16 C17 1.374(14) . ?
C16 H16 0.9500 . ?
C17 C18 1.379(9) . ?
C17 H17 0.9500 . ?
C18 C19 1.491(10) . ?
C19 H19A 0.9900 . ?
C19 H19B 0.9900 . ?
C20 C21 1.505(7) . ?
C20 H20A 0.9900 . ?
C20 H20B 0.9900 . ?
C21 C22 1.392(7) . ?
C22 C23 1.382(8) . ?
C22 H22 0.9500 . ?
C23 C24 1.377(8) . ?
C23 H23 0.9500 . ?
C24 C25 1.377(7) . ?
C24 H24 0.9500 . ?
C25 H25 0.9500 . ?
C26 C27 1.494(8) . ?
C26 H26A 0.9900 . ?
C26 H26B 0.9900 . ?
C27 C28 1.380(8) . ?
C28 C29 1.392(10) . ?
C28 H28 0.9500 . ?
C29 C30 1.370(10) . ?
C29 H29 0.9500 . ?
C30 C31 1.398(8) . ?
C30 H30 0.9500 . ?
C31 H31 0.9500 . ?
Cl1 O3 1.421(8) . ?
Cl1 O4 1.433(9) . ?
Cl1 O1 1.433(8) . ?
Cl1 O2 1.449(8) . ?
Cl1' O3' 1.407(10) . ?
Cl1' O1' 1.420(9) . ?
Cl1' O2' 1.427(9) . ?
Cl1' O4' 1.439(10) . ?
C1S O1S 1.412(13) . ?
C1S H1SA 0.9800 . ?
C1S H1SB 0.9800 . ?
C1S H1SC 0.9800 . ?
O1S H1S 0.9799 . ?

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
C2 Fe1 C3 89.6(2) . . ?
C2 Fe1 C1 93.0(2) . . ?
C3 Fe1 C1 89.0(2) . . ?
C2 Fe1 N6 90.34(18) . . ?
C3 Fe1 N6 93.05(19) . . ?
C1 Fe1 N6 176.13(19) . . ?
C2 Fe1 N8 174.5(2) . . ?
C3 Fe1 N8 94.67(19) . . ?
C1 Fe1 N8 90.5(2) . . ?
N6 Fe1 N8 86.08(18) . . ?
C2 Fe1 N4 88.16(19) . . ?
C3 Fe1 N4 176.2(2) . . ?
C1 Fe1 N4 88.0(2) . . ?
N6 Fe1 N4 90.06(19) . . ?
N8 Fe1 N4 87.70(18) . . ?
N1 Fe2 N2 87.50(17) . 3_667 ?
N1 Fe2 N12 94.62(17) . . ?
N2 Fe2 N12 177.61(17) 3_667 . ?
N1 Fe2 N10 99.6(2) . . ?
N2 Fe2 N10 87.11(17) 3_667 . ?
N12 Fe2 N10 93.62(17) . . ?
N1 Fe2 N13 94.72(17) . . ?
N2 Fe2 N13 93.73(17) 3_667 . ?
N12 Fe2 N13 85.01(17) . . ?
N10 Fe2 N13 165.7(2) . . ?
N1 Fe2 N11 178.49(19) . . ?
N2 Fe2 N11 92.77(17) 3_667 . ?
N12 Fe2 N11 85.08(17) . . ?
N10 Fe2 N11 81.9(2) . . ?
N13 Fe2 N11 83.78(18) . . ?
N5 B1 N9 105.4(6) . . ?
N5 B1 N7 106.5(5) . . ?
N9 B1 N7 104.4(5) . . ?
N5 B1 C13 112.8(5) . . ?
N9 B1 C13 113.5(5) . . ?
N7 B1 C13 113.5(7) . . ?
C1 N1 Fe2 163.6(4) . . ?
C2 N2 Fe2 161.2(4) . 3_667 ?
C4 N4 N5 107.6(5) . . ?
C4 N4 Fe1 131.7(4) . . ?
N5 N4 Fe1 120.7(4) . . ?
C6 N5 N4 107.8(6) . . ?
C6 N5 B1 133.1(6) . . ?
N4 N5 B1 119.1(4) . . ?
C7 N6 N7 107.3(4) . . ?
C7 N6 Fe1 132.6(3) . . ?
N7 N6 Fe1 120.1(3) . . ?
C9 N7 N6 109.0(5) . . ?
C9 N7 B1 131.3(5) . . ?
N6 N7 B1 119.5(5) . . ?
C10 N8 N9 107.0(5) . . ?
C10 N8 Fe1 133.1(5) . . ?
N9 N8 Fe1 119.9(3) . . ?
N8 N9 C12 108.4(5) . . ?
N8 N9 B1 120.3(4) . . ?
C12 N9 B1 131.3(6) . . ?
C14 N10 C18 119.1(6) . . ?
C14 N10 Fe2 127.9(5) . . ?
C18 N10 Fe2 113.0(4) . . ?
C19 N11 C26 112.6(4) . . ?
C19 N11 C20 109.6(4) . . ?
C26 N11 C20 111.8(5) . . ?
C19 N11 Fe2 107.0(4) . . ?
C26 N11 Fe2 106.1(3) . . ?
C20 N11 Fe2 109.5(3) . . ?
C25 N12 C21 118.2(4) . . ?
C25 N12 Fe2 126.2(3) . . ?
C21 N12 Fe2 114.4(3) . . ?
C31 N13 C27 119.1(4) . . ?
C31 N13 Fe2 127.2(3) . . ?
C27 N13 Fe2 112.6(3) . . ?
N1 C1 Fe1 168.6(4) . . ?
N2 C2 Fe1 168.4(4) . . ?
N3 C3 Fe1 178.6(5) . . ?
N4 C4 C5 109.8(6) . . ?
N4 C4 H4 125.1 . . ?
C5 C4 H4 125.1 . . ?
C6 C5 C4 105.3(6) . . ?
C6 C5 H5 127.4 . . ?
C4 C5 H5 127.4 . . ?
N5 C6 C5 109.5(6) . . ?
N5 C6 H6 125.3 . . ?
C5 C6 H6 125.3 . . ?
N6 C7 C8 110.0(5) . . ?
N6 C7 H7 125.0 . . ?
C8 C7 H7 125.0 . . ?
C9 C8 C7 104.8(6) . . ?
C9 C8 H8 127.6 . . ?
C7 C8 H8 127.6 . . ?
N7 C9 C8 108.9(5) . . ?
N7 C9 H9 125.6 . . ?
C8 C9 H9 125.6 . . ?
N8 C10 C11 110.5(6) . . ?
N8 C10 H10 124.7 . . ?
C11 C10 H10 124.7 . . ?
C12 C11 C10 104.3(5) . . ?
C12 C11 H11 127.8 . . ?
C10 C11 H11 127.8 . . ?
N9 C12 C11 109.8(7) . . ?
N9 C12 H12 125.1 . . ?
C11 C12 H12 125.1 . . ?
B1 C13 H13A 109.5 . . ?
B1 C13 H13B 109.5 . . ?
H13A C13 H13B 109.5 . . ?
B1 C13 H13C 109.5 . . ?
H13A C13 H13C 109.5 . . ?
H13B C13 H13C 109.5 . . ?
N10 C14 C15 120.0(8) . . ?
N10 C14 H14 120.0 . . ?
C15 C14 H14 120.0 . . ?
C16 C15 C14 119.8(8) . . ?
C16 C15 H15 120.1 . . ?
C14 C15 H15 120.1 . . ?
C15 C16 C17 120.6(8) . . ?
C15 C16 H16 119.7 . . ?
C17 C16 H16 119.7 . . ?
C16 C17 C18 118.0(9) . . ?
C16 C17 H17 121.0 . . ?
C18 C17 H17 121.0 . . ?
N10 C18 C17 122.6(8) . . ?
N10 C18 C19 115.3(5) . . ?
C17 C18 C19 122.0(7) . . ?
N11 C19 C18 107.8(5) . . ?
N11 C19 H19A 110.1 . . ?
C18 C19 H19A 110.1 . . ?
N11 C19 H19B 110.1 . . ?
C18 C19 H19B 110.1 . . ?
H19A C19 H19B 108.5 . . ?
N11 C20 C21 111.5(4) . . ?
N11 C20 H20A 109.3 . . ?
C21 C20 H20A 109.3 . . ?
N11 C20 H20B 109.3 . . ?
C21 C20 H20B 109.3 . . ?
H20A C20 H20B 108.0 . . ?
N12 C21 C22 122.4(5) . . ?
N12 C21 C20 114.9(4) . . ?
C22 C21 C20 122.6(5) . . ?
C23 C22 C21 118.4(5) . . ?
C23 C22 H22 120.8 . . ?
C21 C22 H22 120.8 . . ?
C24 C23 C22 119.1(5) . . ?
C24 C23 H23 120.5 . . ?
C22 C23 H23 120.5 . . ?
C23 C24 C25 119.2(5) . . ?
C23 C24 H24 120.4 . . ?
C25 C24 H24 120.4 . . ?
N12 C25 C24 122.6(5) . . ?
N12 C25 H25 118.7 . . ?
C24 C25 H25 118.7 . . ?
N11 C26 C27 108.4(4) . . ?
N11 C26 H26A 110.0 . . ?
C27 C26 H26A 110.0 . . ?
N11 C26 H26B 110.0 . . ?
C27 C26 H26B 110.0 . . ?
H26A C26 H26B 108.4 . . ?
N13 C27 C28 121.7(5) . . ?
N13 C27 C26 114.5(5) . . ?
C28 C27 C26 123.8(5) . . ?
C27 C28 C29 119.1(6) . . ?
C27 C28 H28 120.5 . . ?
C29 C28 H28 120.5 . . ?
C30 C29 C28 119.4(5) . . ?
C30 C29 H29 120.3 . . ?
C28 C29 H29 120.3 . . ?
C29 C30 C31 118.8(6) . . ?
C29 C30 H30 120.6 . . ?
C31 C30 H30 120.6 . . ?
N13 C31 C30 121.9(5) . . ?
N13 C31 H31 119.0 . . ?
C30 C31 H31 119.0 . . ?
O3 Cl1 O4 110.1(6) . . ?
O3 Cl1 O1 110.3(5) . . ?
O4 Cl1 O1 109.4(5) . . ?
O3 Cl1 O2 108.0(5) . . ?
O4 Cl1 O2 110.4(6) . . ?
O1 Cl1 O2 108.6(5) . . ?
O3' Cl1' O1' 108.5(6) . . ?
O3' Cl1' O2' 111.8(7) . . ?
O1' Cl1' O2' 108.1(5) . . ?
O3' Cl1' O4' 108.0(6) . . ?
O1' Cl1' O4' 110.5(7) . . ?
O2' Cl1' O4' 109.9(6) . . ?
O1S C1S H1SA 109.5 . . ?
O1S C1S H1SB 109.5 . . ?
H1SA C1S H1SB 109.5 . . ?
O1S C1S H1SC 109.5 . . ?
H1SA C1S H1SC 109.5 . . ?
H1SB C1S H1SC 109.5 . . ?
C1S O1S H1S 109.2 . . ?

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
C4 N4 N5 C6 0.1(6) . . . . ?
Fe1 N4 N5 C6 -178.8(4) . . . . ?
C4 N4 N5 B1 178.1(5) . . . . ?
Fe1 N4 N5 B1 -0.8(6) . . . . ?
N9 B1 N5 C6 122.5(7) . . . . ?
N7 B1 N5 C6 -126.9(7) . . . . ?
C13 B1 N5 C6 -1.9(10) . . . . ?
N9 B1 N5 N4 -54.9(6) . . . . ?
N7 B1 N5 N4 55.7(7) . . . . ?
C13 B1 N5 N4 -179.3(5) . . . . ?
C7 N6 N7 C9 0.9(5) . . . . ?
Fe1 N6 N7 C9 -178.5(3) . . . . ?
C7 N6 N7 B1 -174.3(4) . . . . ?
Fe1 N6 N7 B1 6.3(6) . . . . ?
N5 B1 N7 C9 126.7(6) . . . . ?
N9 B1 N7 C9 -122.1(6) . . . . ?
C13 B1 N7 C9 2.0(8) . . . . ?
N5 B1 N7 N6 -59.4(6) . . . . ?
N9 B1 N7 N6 51.9(7) . . . . ?
C13 B1 N7 N6 176.0(5) . . . . ?
C10 N8 N9 C12 0.6(6) . . . . ?
Fe1 N8 N9 C12 179.3(4) . . . . ?
C10 N8 N9 B1 -179.5(5) . . . . ?
Fe1 N8 N9 B1 -0.7(7) . . . . ?
N5 B1 N9 N8 56.5(6) . . . . ?
N7 B1 N9 N8 -55.5(7) . . . . ?
C13 B1 N9 N8 -179.6(6) . . . . ?
N5 B1 N9 C12 -123.5(7) . . . . ?
N7 B1 N9 C12 124.5(7) . . . . ?
C13 B1 N9 C12 0.4(11) . . . . ?
Fe2 N1 C1 Fe1 22(3) . . . . ?
Fe2 N2 C2 Fe1 -20(3) 3_667 . . . ?
N5 N4 C4 C5 0.0(7) . . . . ?
Fe1 N4 C4 C5 178.7(4) . . . . ?
N4 C4 C5 C6 0.0(8) . . . . ?
N4 N5 C6 C5 -0.1(8) . . . . ?
B1 N5 C6 C5 -177.7(7) . . . . ?
C4 C5 C6 N5 0.1(9) . . . . ?
N7 N6 C7 C8 -0.7(6) . . . . ?
Fe1 N6 C7 C8 178.6(4) . . . . ?
N6 C7 C8 C9 0.2(6) . . . . ?
N6 N7 C9 C8 -0.8(6) . . . . ?
B1 N7 C9 C8 173.6(5) . . . . ?
C7 C8 C9 N7 0.4(6) . . . . ?
N9 N8 C10 C11 -0.6(7) . . . . ?
Fe1 N8 C10 C11 -179.1(4) . . . . ?
N8 C10 C11 C12 0.3(8) . . . . ?
N8 N9 C12 C11 -0.4(8) . . . . ?
B1 N9 C12 C11 179.7(7) . . . . ?
C10 C11 C12 N9 0.0(8) . . . . ?
C18 N10 C14 C15 0.7(8) . . . . ?
Fe2 N10 C14 C15 -175.9(4) . . . . ?
N10 C14 C15 C16 -1.8(9) . . . . ?
C14 C15 C16 C17 1.9(11) . . . . ?
C15 C16 C17 C18 -0.9(11) . . . . ?
C14 N10 C18 C17 0.3(8) . . . . ?
Fe2 N10 C18 C17 177.4(5) . . . . ?
C14 N10 C18 C19 -177.0(5) . . . . ?
Fe2 N10 C18 C19 0.1(6) . . . . ?
C16 C17 C18 N10 -0.2(9) . . . . ?
C16 C17 C18 C19 176.9(6) . . . . ?
C26 N11 C19 C18 156.4(4) . . . . ?
C20 N11 C19 C18 -78.5(6) . . . . ?
Fe2 N11 C19 C18 40.2(5) . . . . ?
N10 C18 C19 N11 -27.0(6) . . . . ?
C17 C18 C19 N11 155.7(5) . . . . ?
C19 N11 C20 C21 136.3(6) . . . . ?
C26 N11 C20 C21 -98.2(6) . . . . ?
Fe2 N11 C20 C21 19.1(6) . . . . ?
C25 N12 C21 C22 3.6(8) . . . . ?
Fe2 N12 C21 C22 -164.5(5) . . . . ?
C25 N12 C21 C20 -174.0(5) . . . . ?
Fe2 N12 C21 C20 17.8(6) . . . . ?
N11 C20 C21 N12 -24.6(8) . . . . ?
N11 C20 C21 C22 157.7(6) . . . . ?
N12 C21 C22 C23 -2.9(10) . . . . ?
C20 C21 C22 C23 174.6(6) . . . . ?
C21 C22 C23 C24 -0.1(10) . . . . ?
C22 C23 C24 C25 2.1(9) . . . . ?
C21 N12 C25 C24 -1.5(8) . . . . ?
Fe2 N12 C25 C24 165.1(4) . . . . ?
C23 C24 C25 N12 -1.3(8) . . . . ?
C19 N11 C26 C27 -156.9(4) . . . . ?
C20 N11 C26 C27 79.2(5) . . . . ?
Fe2 N11 C26 C27 -40.1(5) . . . . ?
C31 N13 C27 C28 -1.9(8) . . . . ?
Fe2 N13 C27 C28 166.9(5) . . . . ?
C31 N13 C27 C26 177.6(5) . . . . ?
Fe2 N13 C27 C26 -13.6(6) . . . . ?
N11 C26 C27 N13 36.5(6) . . . . ?
N11 C26 C27 C28 -144.0(6) . . . . ?
N13 C27 C28 C29 2.1(9) . . . . ?
C26 C27 C28 C29 -177.4(6) . . . . ?
C27 C28 C29 C30 -0.9(10) . . . . ?
C28 C29 C30 C31 -0.4(10) . . . . ?
C27 N13 C31 C30 0.6(8) . . . . ?
Fe2 N13 C31 C30 -166.3(4) . . . . ?
C29 C30 C31 N13 0.5(9) . . . . ?

loop_
_geom_hbond_atom_site_label_D
_geom_hbond_atom_site_label_H
_geom_hbond_atom_site_label_A
_geom_hbond_distance_DH
_geom_hbond_distance_HA
_geom_hbond_distance_DA
_geom_hbond_angle_DHA
_geom_hbond_site_symmetry_A
O1S H1S O4 0.98 2.30 3.223(13) 156.2 .
O1S H1S O2 0.98 2.37 3.073(12) 127.9 .
O1S H1S Cl1 0.98 2.84 3.729(8) 151.7 .
C31 H31 N1 0.95 2.64 3.125(7) 112.0 .
C28 H28 O2 0.95 2.55 3.149(10) 121.2 4_566
C26 H26A O3' 0.99 2.54 3.474(11) 156.7 4_566
C25 H25 N1 0.95 2.54 3.047(7) 113.4 .
C24 H24 N3 0.95 2.63 3.357(7) 133.7 3_567
C20 H20B O3' 0.99 2.60 3.460(12) 145.1 4_566
C20 H20B O1' 0.99 2.21 3.151(11) 158.6 4_566
C20 H20B Cl1' 0.99 2.93 3.919(7) 173.7 4_566
C20 H20B O3 0.99 2.53 3.432(10) 151.6 4_566
C19 H19B O1S 0.99 2.38 3.365(10) 172.6 2_646
C19 H19A O4 0.99 2.47 3.016(11) 114.5 2_646
C17 H17 N3 0.95 2.60 3.355(9) 136.3 2_647
C15 H15 O1S 0.95 2.43 3.065(14) 123.9 1_556
C15 H15 O3' 0.95 2.61 3.521(13) 161.4 3_667
C14 H14 O1S 0.95 2.55 3.124(11) 119.0 1_556
C12 H12 O2 0.95 2.43 3.320(12) 156.7 3_566
C12 H12 O1 0.95 2.57 3.409(10) 147.4 3_566
C11 H11 N3 0.95 2.60 3.471(8) 153.1 3_567
C8 H8 O1 0.95 2.58 3.067(11) 112.4 4_576
C7 H7 O4' 0.95 2.36 3.194(10) 145.9 4_576
C7 H7 O4 0.95 2.58 3.260(10) 129.0 4_576
C6 H6 O3 0.95 2.07 2.881(11) 141.9 .
C5 H5 O1S 0.95 2.62 3.275(9) 126.3 3_666
O1S H1S O4 0.98 2.30 3.223(13) 156.2 .
O1S H1S O2 0.98 2.37 3.073(12) 127.9 .

_refine_diff_density_max         0.926
_refine_diff_density_min         -0.721
_refine_diff_density_rms         0.121

####################################################################### 
# 
# 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_3_MeOH-296K
_database_code_depnum_ccdc_archive 'CCDC 1419286'
_audit_update_record             
;
2016-09-02 deposited with the CCDC.
2016-09-26 downloaded from the CCDC.
;

_audit_creation_method           SHELXL-2014/7
_shelx_SHELXL_version_number     2014/7
_chemical_name_systematic        ?
_chemical_name_common            ?
_chemical_melting_point          ?
_chemical_formula_moiety         'C62 H60 B2 Fe4 N26, 2(Cl O4), C H4 O '
_chemical_formula_sum            'C63 H64 B2 Cl2 Fe4 N26 O9'
_chemical_formula_weight         1645.32

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'
O O 0.0106 0.0060 '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'

_space_group_crystal_system      monoclinic
_space_group_IT_number           14
_space_group_name_H-M_alt        'P 21/c'
_space_group_name_Hall           '-P 2ybc'

_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.
;

loop_
_space_group_symop_operation_xyz
'x, y, z'
'-x, y+1/2, -z+1/2'
'-x, -y, -z'
'x, -y-1/2, z-1/2'

_cell_length_a                   13.0293(14)
_cell_length_b                   17.5910(19)
_cell_length_c                   16.8823(18)
_cell_angle_alpha                90
_cell_angle_beta                 108.685(2)
_cell_angle_gamma                90
_cell_volume                     3665.5(7)
_cell_formula_units_Z            2
_cell_measurement_temperature    296(2)
_cell_measurement_reflns_used    7027
_cell_measurement_theta_min      2.32
_cell_measurement_theta_max      24.33

_exptl_crystal_description       block
_exptl_crystal_colour            red
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    'not measured'
_exptl_crystal_density_diffrn    1.491
_exptl_crystal_F_000             1688
_exptl_transmission_factor_min   ?
_exptl_transmission_factor_max   ?
_exptl_crystal_size_max          0.100
_exptl_crystal_size_mid          0.050
_exptl_crystal_size_min          0.050
_exptl_absorpt_coefficient_mu    0.922
_shelx_estimated_absorpt_T_min   0.913
_shelx_estimated_absorpt_T_max   0.955
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_correction_T_min  0.9135
_exptl_absorpt_correction_T_max  0.9554
_exptl_absorpt_process_details   sadabs
_exptl_absorpt_special_details   ?
_diffrn_ambient_temperature      296(2)
_diffrn_radiation_wavelength     0.71073
_diffrn_radiation_type           MoK\a
_diffrn_source                   ?
_diffrn_measurement_device_type  'Bruker APEX-II CCD'
_diffrn_measurement_method       'φ and ω scans'
_diffrn_detector_area_resol_mean ?
_diffrn_reflns_number            35928
_diffrn_reflns_av_unetI/netI     0.0452
_diffrn_reflns_av_R_equivalents  0.0428
_diffrn_reflns_limit_h_min       -17
_diffrn_reflns_limit_h_max       17
_diffrn_reflns_limit_k_min       -23
_diffrn_reflns_limit_k_max       23
_diffrn_reflns_limit_l_min       -19
_diffrn_reflns_limit_l_max       22
_diffrn_reflns_theta_min         1.650
_diffrn_reflns_theta_max         28.989
_diffrn_reflns_theta_full        25.242
_diffrn_measured_fraction_theta_max 0.991
_diffrn_measured_fraction_theta_full 0.996
_diffrn_reflns_Laue_measured_fraction_max 0.991
_diffrn_reflns_Laue_measured_fraction_full 0.996
_diffrn_reflns_point_group_measured_fraction_max 0.991
_diffrn_reflns_point_group_measured_fraction_full 0.996
_reflns_number_total             9644
_reflns_number_gt                6423
_reflns_threshold_expression     'I > 2σ(I)'
_reflns_Friedel_coverage         0.000
_reflns_Friedel_fraction_max     .
_reflns_Friedel_fraction_full    .

_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.
;

_computing_data_collection       'Bruker APEX2'
_computing_cell_refinement       'Bruker SAINT'
_computing_data_reduction        'Bruker SAINT'
_computing_structure_solution    'SHELXS-2014 (Sheldrick, 2014)'
_computing_structure_refinement  'SHELXL-2014/7 (Sheldrick, 2014)'
_computing_molecular_graphics    'Bruker SHELXTL'
_computing_publication_material  'Bruker SHELXTL'
_refine_special_details          ?
_refine_ls_structure_factor_coef Fsqd
_refine_ls_matrix_type           full
_refine_ls_weighting_scheme      calc
_refine_ls_weighting_details     
'w=1/[σ²(Fo²)+(0.0746P)²+0.5992P] where P=(Fo²+2Fc²)/3'
_atom_sites_solution_primary     ?
_atom_sites_solution_secondary   ?
_atom_sites_solution_hydrogens   mixed
_refine_ls_hydrogen_treatment    constr
_refine_ls_extinction_method     none
_refine_ls_extinction_coef       .
_refine_ls_number_reflns         9644
_refine_ls_number_parameters     534
_refine_ls_number_restraints     200
_refine_ls_R_factor_all          0.0776
_refine_ls_R_factor_gt           0.0441
_refine_ls_wR_factor_ref         0.1378
_refine_ls_wR_factor_gt          0.1175
_refine_ls_goodness_of_fit_ref   1.011
_refine_ls_restrained_S_all      1.075
_refine_ls_shift/su_max          0.001
_refine_ls_shift/su_mean         0.000

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 0.25976(3) 0.57779(2) 0.92839(2) 0.03618(11) Uani 1 1 d . . . . .
Fe2 Fe 0.37599(3) 0.32148(2) 1.03975(2) 0.03601(11) Uani 1 1 d . . . . .
B1 B 0.1263(3) 0.5720(2) 0.7375(2) 0.0571(8) Uani 1 1 d . . . . .
N1 N 0.33310(19) 0.43114(14) 1.02747(16) 0.0540(6) Uani 1 1 d . . . . .
N2 N 0.48411(18) 0.65073(12) 0.98284(15) 0.0493(5) Uani 1 1 d . . . . .
N3 N 0.2067(2) 0.6478(2) 1.07708(18) 0.0757(8) Uani 1 1 d . . . . .
N4 N 0.30376(17) 0.52885(12) 0.83883(13) 0.0425(5) Uani 1 1 d . . . . .
N5 N 0.23769(19) 0.53133(13) 0.75852(15) 0.0523(6) Uani 1 1 d . . . . .
N6 N 0.20386(17) 0.66533(11) 0.85488(13) 0.0418(5) Uani 1 1 d . . . . .
N7 N 0.15109(19) 0.65406(14) 0.77200(14) 0.0522(6) Uani 1 1 d . . . . .
N8 N 0.11525(17) 0.53200(12) 0.87820(14) 0.0458(5) Uani 1 1 d . . . . .
N9 N 0.06776(18) 0.53326(14) 0.79391(15) 0.0532(6) Uani 1 1 d . . . . .
N10 N 0.4646(2) 0.31406(15) 1.16493(15) 0.0571(6) Uani 1 1 d . . . . .
N11 N 0.41095(18) 0.20478(12) 1.05248(14) 0.0459(5) Uani 1 1 d . . . . .
N12 N 0.23364(17) 0.28460(12) 1.05862(13) 0.0441(5) Uani 1 1 d . . . . .
N13 N 0.29900(18) 0.28745(13) 0.91730(14) 0.0467(5) Uani 1 1 d . . . . .
C1 C 0.3083(2) 0.48927(15) 0.99615(17) 0.0436(6) Uani 1 1 d . . . . .
C2 C 0.4006(2) 0.62363(13) 0.96941(15) 0.0386(5) Uani 1 1 d . . . . .
C3 C 0.2252(2) 0.62240(16) 1.02063(18) 0.0486(6) Uani 1 1 d . . . . .
C4 C 0.3910(2) 0.48902(16) 0.8403(2) 0.0546(7) Uani 1 1 d . . . . .
H4 H 0.4489 0.4785 0.8881 0.065 Uiso 1 1 calc R U . . .
C5 C 0.3833(3) 0.4657(2) 0.7613(2) 0.0759(10) Uani 1 1 d . . . . .
H5 H 0.4332 0.4371 0.7452 0.091 Uiso 1 1 calc R U . . .
C6 C 0.2866(3) 0.4934(2) 0.7113(2) 0.0726(10) Uani 1 1 d . . . . .
H6 H 0.2588 0.4872 0.6537 0.087 Uiso 1 1 calc R U . . .
C7 C 0.2069(2) 0.73991(14) 0.8678(2) 0.0525(7) Uani 1 1 d . . . . .
H7 H 0.2379 0.7631 0.9195 0.063 Uiso 1 1 calc R U . . .
C8 C 0.1580(3) 0.77782(18) 0.7948(2) 0.0724(10) Uani 1 1 d . . . . .
H8 H 0.1498 0.8301 0.7871 0.087 Uiso 1 1 calc R U . . .
C9 C 0.1236(3) 0.7221(2) 0.7351(2) 0.0716(10) Uani 1 1 d . . . . .
H9 H 0.0874 0.7301 0.6785 0.086 Uiso 1 1 calc R U . . .
C10 C 0.0486(2) 0.49513(17) 0.9104(2) 0.0608(8) Uani 1 1 d . . . . .
H10 H 0.0618 0.4863 0.9671 0.073 Uiso 1 1 calc R U . . .
C11 C -0.0424(3) 0.4719(2) 0.8479(3) 0.0814(11) Uani 1 1 d . . . . .
H11 H -0.1012 0.4451 0.8535 0.098 Uiso 1 1 calc R U . . .
C12 C -0.0280(3) 0.4966(2) 0.7761(3) 0.0746(10) Uani 1 1 d . . . . .
H12 H -0.0766 0.4894 0.7227 0.089 Uiso 1 1 calc R U . . .
C13 C 0.0582(3) 0.5697(3) 0.6406(2) 0.0876(12) Uani 1 1 d . . . . .
H13A H -0.0095 0.5954 0.6316 0.131 Uiso 1 1 calc R U . . .
H13B H 0.0448 0.5178 0.6227 0.131 Uiso 1 1 calc R U . . .
H13C H 0.0983 0.5944 0.6092 0.131 Uiso 1 1 calc R U . . .
C14 C 0.4699(4) 0.3663(2) 1.2234(2) 0.0904(14) Uani 1 1 d . . . . .
H14 H 0.4271 0.4097 1.2098 0.108 Uiso 1 1 calc R U . . .
C15 C 0.5408(5) 0.3557(4) 1.3067(3) 0.1159(19) Uani 1 1 d . U . . .
H15 H 0.5454 0.3922 1.3475 0.139 Uiso 1 1 calc R U . . .
C16 C 0.6006(5) 0.2924(4) 1.3250(3) 0.124(2) Uani 1 1 d . U . . .
H16 H 0.6470 0.2851 1.3792 0.149 Uiso 1 1 calc R U . . .
C17 C 0.5949(3) 0.2396(3) 1.2671(3) 0.1020(16) Uani 1 1 d . . . . .
H17 H 0.6364 0.1957 1.2809 0.122 Uiso 1 1 calc R U . . .
C18 C 0.5263(2) 0.2508(2) 1.1859(2) 0.0643(9) Uani 1 1 d . . . . .
C19 C 0.5188(2) 0.19760(19) 1.1162(2) 0.0625(8) Uani 1 1 d . . . . .
H19A H 0.5747 0.2093 1.0915 0.075 Uiso 1 1 calc R U . . .
H19B H 0.5297 0.1459 1.1371 0.075 Uiso 1 1 calc R U . . .
C20 C 0.3284(2) 0.16514(15) 1.0811(2) 0.0583(8) Uani 1 1 d . . . . .
H20A H 0.3576 0.1568 1.1409 0.070 Uiso 1 1 calc R U . . .
H20B H 0.3133 0.1158 1.0541 0.070 Uiso 1 1 calc R U . . .
C21 C 0.2243(2) 0.20906(15) 1.06209(16) 0.0451(6) Uani 1 1 d . . . . .
C22 C 0.1258(3) 0.17397(19) 1.0533(2) 0.0632(8) Uani 1 1 d . . . . .
H22 H 0.1207 0.1213 1.0543 0.076 Uiso 1 1 calc R U . . .
C23 C 0.0361(3) 0.2187(2) 1.0431(2) 0.0748(10) Uani 1 1 d . . . . .
H23 H -0.0311 0.1966 1.0362 0.090 Uiso 1 1 calc R U . . .
C24 C 0.0467(3) 0.2960(2) 1.0431(2) 0.0769(10) Uani 1 1 d . . . . .
H24 H -0.0127 0.3271 1.0386 0.092 Uiso 1 1 calc R U . . .
C25 C 0.1455(3) 0.32742(19) 1.0500(2) 0.0632(8) Uani 1 1 d . . . . .
H25 H 0.1517 0.3800 1.0486 0.076 Uiso 1 1 calc R U . . .
C26 C 0.4098(3) 0.17818(17) 0.9687(2) 0.0641(8) Uani 1 1 d . . . . .
H26A H 0.4017 0.1233 0.9653 0.077 Uiso 1 1 calc R U . . .
H26B H 0.4779 0.1911 0.9602 0.077 Uiso 1 1 calc R U . . .
C27 C 0.3183(3) 0.21458(18) 0.90256(19) 0.0589(7) Uani 1 1 d . . . . .
C28 C 0.2571(4) 0.1767(3) 0.8310(3) 0.0976(14) Uani 1 1 d . . . . .
H28 H 0.2685 0.1255 0.8228 0.117 Uiso 1 1 calc R U . . .
C29 C 0.1774(4) 0.2185(3) 0.7717(3) 0.1104(16) Uani 1 1 d . . . . .
H29 H 0.1370 0.1956 0.7219 0.132 Uiso 1 1 calc R U . . .
C30 C 0.1585(4) 0.2919(3) 0.7860(2) 0.0874(12) Uani 1 1 d . . . . .
H30 H 0.1045 0.3193 0.7470 0.105 Uiso 1 1 calc R U . . .
C31 C 0.2206(3) 0.32531(19) 0.85909(19) 0.0605(8) Uani 1 1 d . . . . .
H31 H 0.2081 0.3760 0.8687 0.073 Uiso 1 1 calc R U . . .
Cl1 Cl 0.2797(6) 0.9545(4) 0.9632(5) 0.1030(18) Uani 0.5 1 d . U P A 1
O1 O 0.2486(9) 0.8820(4) 0.9977(5) 0.138(3) Uani 0.5 1 d . U P A 1
O2 O 0.3781(6) 0.9791(4) 1.0178(5) 0.140(3) Uani 0.5 1 d . U P A 1
O3 O 0.2040(8) 1.0093(5) 0.9734(7) 0.143(3) Uani 0.5 1 d . U P A 1
O4 O 0.2653(9) 0.9463(5) 0.8815(5) 0.137(3) Uani 0.5 1 d . U P A 1
Cl1' Cl 0.2552(5) 0.9472(4) 0.9625(4) 0.0661(9) Uani 0.5 1 d . U P B 2
O1' O 0.3284(7) 0.8914(5) 0.9753(6) 0.136(3) Uani 0.5 1 d . U P B 2
O2' O 0.2490(11) 0.9923(6) 1.0209(6) 0.164(3) Uani 0.5 1 d . U P B 2
O3' O 0.2544(10) 0.9992(7) 0.8991(7) 0.177(4) Uani 0.5 1 d . U P B 2
O4' O 0.1490(7) 0.9126(5) 0.9264(7) 0.154(3) Uani 0.5 1 d . U P B 2
C1S C 0.3296(7) 0.9674(5) 0.7394(5) 0.088(3) Uani 0.5 1 d . . P C 1
H1SA H 0.2818 1.0096 0.7188 0.131 Uiso 0.5 1 calc R U P C 1
H1SB H 0.2890 0.9251 0.7495 0.131 Uiso 0.5 1 calc R U P C 1
H1SC H 0.3635 0.9534 0.6986 0.131 Uiso 0.5 1 calc R U P C 1
O1S O 0.4051(7) 0.9870(5) 0.8101(6) 0.141(3) Uani 0.5 1 d . . P C 1
H1S H 0.3736 0.9874 0.8543 0.211 Uiso 0.5 1 d R U P C 1


_geom_special_details            
;
 All esds (except the esd in the dihedral angle between two l.s. planes)
 are estimated using the full covariance matrix.  The cell esds are taken
 into account individually in the estimation of esds in distances, angles
 and torsion angles; correlations between esds in cell parameters are only
 used when they are defined by crystal symmetry.  An approximate (isotropic)
 treatment of cell esds is used for estimating esds involving l.s. planes.
;

loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
_geom_bond_publ_flag
Fe1 C1 1.916(3) . ?
Fe1 C2 1.919(3) . ?
Fe1 C3 1.921(3) . ?
Fe1 N6 1.965(2) . ?
Fe1 N8 1.972(2) . ?
Fe1 N4 1.978(2) . ?
Fe2 N1 2.000(2) . ?
Fe2 N2 2.038(2) 3_667 ?
Fe2 N10 2.062(3) . ?
Fe2 N13 2.076(2) . ?
Fe2 N12 2.084(2) . ?
Fe2 N11 2.099(2) . ?
B1 N7 1.552(4) . ?
B1 N5 1.554(5) . ?
B1 N9 1.555(4) . ?
B1 C13 1.591(5) . ?
N1 C1 1.149(3) . ?
N2 C2 1.143(3) . ?
N2 Fe2 2.038(2) 3_667 ?
N3 C3 1.146(4) . ?
N4 C4 1.329(3) . ?
N4 N5 1.354(3) . ?
N5 C6 1.345(4) . ?
N6 C7 1.329(3) . ?
N6 N7 1.361(3) . ?
N7 C9 1.344(4) . ?
N8 C10 1.331(4) . ?
N8 N9 1.358(3) . ?
N9 C12 1.350(4) . ?
N10 C14 1.333(4) . ?
N10 C18 1.352(4) . ?
N11 C19 1.476(4) . ?
N11 C26 1.485(4) . ?
N11 C20 1.486(4) . ?
N12 C21 1.337(3) . ?
N12 C25 1.341(4) . ?
N13 C27 1.345(4) . ?
N13 C31 1.345(4) . ?
C4 C5 1.367(4) . ?
C4 H4 0.9300 . ?
C5 C6 1.362(5) . ?
C5 H5 0.9300 . ?
C6 H6 0.9300 . ?
C7 C8 1.367(4) . ?
C7 H7 0.9300 . ?
C8 C9 1.374(5) . ?
C8 H8 0.9300 . ?
C9 H9 0.9300 . ?
C10 C11 1.373(5) . ?
C10 H10 0.9300 . ?
C11 C12 1.356(5) . ?
C11 H11 0.9300 . ?
C12 H12 0.9300 . ?
C13 H13A 0.9600 . ?
C13 H13B 0.9600 . ?
C13 H13C 0.9600 . ?
C14 C15 1.426(7) . ?
C14 H14 0.9300 . ?
C15 C16 1.336(8) . ?
C15 H15 0.9300 . ?
C16 C17 1.334(8) . ?
C16 H16 0.9300 . ?
C17 C18 1.390(5) . ?
C17 H17 0.9300 . ?
C18 C19 1.482(5) . ?
C19 H19A 0.9700 . ?
C19 H19B 0.9700 . ?
C20 C21 1.503(4) . ?
C20 H20A 0.9700 . ?
C20 H20B 0.9700 . ?
C21 C22 1.389(4) . ?
C22 C23 1.374(5) . ?
C22 H22 0.9300 . ?
C23 C24 1.367(6) . ?
C23 H23 0.9300 . ?
C24 C25 1.372(5) . ?
C24 H24 0.9300 . ?
C25 H25 0.9300 . ?
C26 C27 1.492(4) . ?
C26 H26A 0.9700 . ?
C26 H26B 0.9700 . ?
C27 C28 1.387(5) . ?
C28 C29 1.398(7) . ?
C28 H28 0.9300 . ?
C29 C30 1.351(7) . ?
C29 H29 0.9300 . ?
C30 C31 1.372(5) . ?
C30 H30 0.9300 . ?
C31 H31 0.9300 . ?
Cl1 O4 1.338(10) . ?
Cl1 O2 1.386(10) . ?
Cl1 O3 1.428(12) . ?
Cl1 O1 1.512(10) . ?
Cl1' O2' 1.287(12) . ?
Cl1' O1' 1.337(9) . ?
Cl1' O3' 1.405(11) . ?
Cl1' O4' 1.456(11) . ?
C1S O1S 1.327(10) . ?
C1S H1SA 0.9600 . ?
C1S H1SB 0.9600 . ?
C1S H1SC 0.9600 . ?
O1S H1S 0.9599 . ?

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
C1 Fe1 C2 91.79(10) . . ?
C1 Fe1 C3 88.07(12) . . ?
C2 Fe1 C3 88.90(11) . . ?
C1 Fe1 N6 176.99(10) . . ?
C2 Fe1 N6 90.95(9) . . ?
C3 Fe1 N6 93.22(11) . . ?
C1 Fe1 N8 90.68(10) . . ?
C2 Fe1 N8 175.98(10) . . ?
C3 Fe1 N8 94.35(11) . . ?
N6 Fe1 N8 86.51(9) . . ?
C1 Fe1 N4 88.94(10) . . ?
C2 Fe1 N4 88.92(9) . . ?
C3 Fe1 N4 176.24(11) . . ?
N6 Fe1 N4 89.88(9) . . ?
N8 Fe1 N4 87.96(9) . . ?
N1 Fe2 N2 89.21(9) . 3_667 ?
N1 Fe2 N10 102.31(11) . . ?
N2 Fe2 N10 88.08(10) 3_667 . ?
N1 Fe2 N13 98.34(10) . . ?
N2 Fe2 N13 93.37(9) 3_667 . ?
N10 Fe2 N13 159.31(10) . . ?
N1 Fe2 N12 94.77(9) . . ?
N2 Fe2 N12 175.42(9) 3_667 . ?
N10 Fe2 N12 93.26(9) . . ?
N13 Fe2 N12 83.84(9) . . ?
N1 Fe2 N11 176.36(9) . . ?
N2 Fe2 N11 94.36(9) 3_667 . ?
N10 Fe2 N11 78.54(10) . . ?
N13 Fe2 N11 80.78(9) . . ?
N12 Fe2 N11 81.63(9) . . ?
N7 B1 N5 106.0(2) . . ?
N7 B1 N9 105.1(3) . . ?
N5 B1 N9 105.3(3) . . ?
N7 B1 C13 112.9(3) . . ?
N5 B1 C13 113.3(3) . . ?
N9 B1 C13 113.4(3) . . ?
C1 N1 Fe2 159.0(2) . . ?
C2 N2 Fe2 156.3(2) . 3_667 ?
C4 N4 N5 107.5(2) . . ?
C4 N4 Fe1 132.2(2) . . ?
N5 N4 Fe1 120.30(17) . . ?
C6 N5 N4 107.9(3) . . ?
C6 N5 B1 132.6(3) . . ?
N4 N5 B1 119.5(2) . . ?
C7 N6 N7 107.0(2) . . ?
C7 N6 Fe1 133.2(2) . . ?
N7 N6 Fe1 119.86(16) . . ?
C9 N7 N6 108.6(3) . . ?
C9 N7 B1 131.4(3) . . ?
N6 N7 B1 119.8(2) . . ?
C10 N8 N9 107.3(2) . . ?
C10 N8 Fe1 133.0(2) . . ?
N9 N8 Fe1 119.69(17) . . ?
C12 N9 N8 107.7(3) . . ?
C12 N9 B1 132.2(3) . . ?
N8 N9 B1 120.1(2) . . ?
C14 N10 C18 119.2(3) . . ?
C14 N10 Fe2 126.5(3) . . ?
C18 N10 Fe2 114.2(2) . . ?
C19 N11 C26 112.6(2) . . ?
C19 N11 C20 110.0(2) . . ?
C26 N11 C20 112.0(2) . . ?
C19 N11 Fe2 106.44(18) . . ?
C26 N11 Fe2 105.96(17) . . ?
C20 N11 Fe2 109.65(16) . . ?
C21 N12 C25 118.4(2) . . ?
C21 N12 Fe2 114.44(18) . . ?
C25 N12 Fe2 125.5(2) . . ?
C27 N13 C31 118.7(3) . . ?
C27 N13 Fe2 113.56(19) . . ?
C31 N13 Fe2 126.6(2) . . ?
N1 C1 Fe1 171.3(3) . . ?
N2 C2 Fe1 170.7(2) . . ?
N3 C3 Fe1 178.2(3) . . ?
N4 C4 C5 110.2(3) . . ?
N4 C4 H4 124.9 . . ?
C5 C4 H4 124.9 . . ?
C6 C5 C4 105.2(3) . . ?
C6 C5 H5 127.4 . . ?
C4 C5 H5 127.4 . . ?
N5 C6 C5 109.2(3) . . ?
N5 C6 H6 125.4 . . ?
C5 C6 H6 125.4 . . ?
N6 C7 C8 110.6(3) . . ?
N6 C7 H7 124.7 . . ?
C8 C7 H7 124.7 . . ?
C7 C8 C9 105.2(3) . . ?
C7 C8 H8 127.4 . . ?
C9 C8 H8 127.4 . . ?
N7 C9 C8 108.6(3) . . ?
N7 C9 H9 125.7 . . ?
C8 C9 H9 125.7 . . ?
N8 C10 C11 110.3(3) . . ?
N8 C10 H10 124.8 . . ?
C11 C10 H10 124.8 . . ?
C12 C11 C10 105.0(3) . . ?
C12 C11 H11 127.5 . . ?
C10 C11 H11 127.5 . . ?
N9 C12 C11 109.7(3) . . ?
N9 C12 H12 125.2 . . ?
C11 C12 H12 125.2 . . ?
B1 C13 H13A 109.5 . . ?
B1 C13 H13B 109.5 . . ?
H13A C13 H13B 109.5 . . ?
B1 C13 H13C 109.5 . . ?
H13A C13 H13C 109.5 . . ?
H13B C13 H13C 109.5 . . ?
N10 C14 C15 120.2(5) . . ?
N10 C14 H14 119.9 . . ?
C15 C14 H14 119.9 . . ?
C16 C15 C14 118.9(5) . . ?
C16 C15 H15 120.6 . . ?
C14 C15 H15 120.6 . . ?
C17 C16 C15 121.2(5) . . ?
C17 C16 H16 119.4 . . ?
C15 C16 H16 119.4 . . ?
C16 C17 C18 119.5(5) . . ?
C16 C17 H17 120.3 . . ?
C18 C17 H17 120.3 . . ?
N10 C18 C17 121.0(4) . . ?
N10 C18 C19 115.5(3) . . ?
C17 C18 C19 123.5(4) . . ?
N11 C19 C18 109.2(2) . . ?
N11 C19 H19A 109.8 . . ?
C18 C19 H19A 109.8 . . ?
N11 C19 H19B 109.8 . . ?
C18 C19 H19B 109.8 . . ?
H19A C19 H19B 108.3 . . ?
N11 C20 C21 112.8(2) . . ?
N11 C20 H20A 109.0 . . ?
C21 C20 H20A 109.0 . . ?
N11 C20 H20B 109.0 . . ?
C21 C20 H20B 109.0 . . ?
H20A C20 H20B 107.8 . . ?
N12 C21 C22 122.1(3) . . ?
N12 C21 C20 115.6(2) . . ?
C22 C21 C20 122.3(3) . . ?
C23 C22 C21 118.6(3) . . ?
C23 C22 H22 120.7 . . ?
C21 C22 H22 120.7 . . ?
C24 C23 C22 119.2(3) . . ?
C24 C23 H23 120.4 . . ?
C22 C23 H23 120.4 . . ?
C23 C24 C25 119.5(3) . . ?
C23 C24 H24 120.2 . . ?
C25 C24 H24 120.2 . . ?
N12 C25 C24 122.0(3) . . ?
N12 C25 H25 119.0 . . ?
C24 C25 H25 119.0 . . ?
N11 C26 C27 109.8(2) . . ?
N11 C26 H26A 109.7 . . ?
C27 C26 H26A 109.7 . . ?
N11 C26 H26B 109.7 . . ?
C27 C26 H26B 109.7 . . ?
H26A C26 H26B 108.2 . . ?
N13 C27 C28 122.0(3) . . ?
N13 C27 C26 115.0(3) . . ?
C28 C27 C26 123.0(3) . . ?
C27 C28 C29 117.3(4) . . ?
C27 C28 H28 121.4 . . ?
C29 C28 H28 121.4 . . ?
C30 C29 C28 120.8(4) . . ?
C30 C29 H29 119.6 . . ?
C28 C29 H29 119.6 . . ?
C29 C30 C31 118.8(4) . . ?
C29 C30 H30 120.6 . . ?
C31 C30 H30 120.6 . . ?
N13 C31 C30 122.4(3) . . ?
N13 C31 H31 118.8 . . ?
C30 C31 H31 118.8 . . ?
O4 Cl1 O2 120.9(9) . . ?
O4 Cl1 O3 108.9(7) . . ?
O2 Cl1 O3 103.7(8) . . ?
O4 Cl1 O1 109.8(8) . . ?
O2 Cl1 O1 108.1(7) . . ?
O3 Cl1 O1 103.9(8) . . ?
O2' Cl1' O1' 123.1(9) . . ?
O2' Cl1' O3' 101.3(9) . . ?
O1' Cl1' O3' 115.5(9) . . ?
O2' Cl1' O4' 107.1(8) . . ?
O1' Cl1' O4' 107.1(7) . . ?
O3' Cl1' O4' 100.3(8) . . ?
O1S C1S H1SA 109.5 . . ?
O1S C1S H1SB 109.5 . . ?
H1SA C1S H1SB 109.5 . . ?
O1S C1S H1SC 109.5 . . ?
H1SA C1S H1SC 109.5 . . ?
H1SB C1S H1SC 109.5 . . ?
C1S O1S H1S 108.9 . . ?

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
C4 N4 N5 C6 -0.8(3) . . . . ?
Fe1 N4 N5 C6 -179.5(2) . . . . ?
C4 N4 N5 B1 177.8(2) . . . . ?
Fe1 N4 N5 B1 -0.9(3) . . . . ?
N7 B1 N5 C6 -126.0(3) . . . . ?
N9 B1 N5 C6 122.9(3) . . . . ?
C13 B1 N5 C6 -1.6(5) . . . . ?
N7 B1 N5 N4 55.8(3) . . . . ?
N9 B1 N5 N4 -55.3(3) . . . . ?
C13 B1 N5 N4 -179.8(3) . . . . ?
C7 N6 N7 C9 0.8(3) . . . . ?
Fe1 N6 N7 C9 -178.4(2) . . . . ?
C7 N6 N7 B1 -175.4(3) . . . . ?
Fe1 N6 N7 B1 5.5(3) . . . . ?
N5 B1 N7 C9 126.1(3) . . . . ?
N9 B1 N7 C9 -122.7(4) . . . . ?
C13 B1 N7 C9 1.4(5) . . . . ?
N5 B1 N7 N6 -58.8(3) . . . . ?
N9 B1 N7 N6 52.4(3) . . . . ?
C13 B1 N7 N6 176.6(3) . . . . ?
C10 N8 N9 C12 -0.1(3) . . . . ?
Fe1 N8 N9 C12 178.2(2) . . . . ?
C10 N8 N9 B1 -179.4(3) . . . . ?
Fe1 N8 N9 B1 -1.1(3) . . . . ?
N7 B1 N9 C12 125.9(3) . . . . ?
N5 B1 N9 C12 -122.4(3) . . . . ?
C13 B1 N9 C12 2.0(5) . . . . ?
N7 B1 N9 N8 -55.0(3) . . . . ?
N5 B1 N9 N8 56.7(3) . . . . ?
C13 B1 N9 N8 -178.8(3) . . . . ?
N5 N4 C4 C5 0.5(3) . . . . ?
Fe1 N4 C4 C5 178.9(2) . . . . ?
N4 C4 C5 C6 0.1(4) . . . . ?
N4 N5 C6 C5 0.9(4) . . . . ?
B1 N5 C6 C5 -177.5(3) . . . . ?
C4 C5 C6 N5 -0.6(4) . . . . ?
N7 N6 C7 C8 -0.6(3) . . . . ?
Fe1 N6 C7 C8 178.3(2) . . . . ?
N6 C7 C8 C9 0.3(4) . . . . ?
N6 N7 C9 C8 -0.6(4) . . . . ?
B1 N7 C9 C8 175.0(3) . . . . ?
C7 C8 C9 N7 0.2(4) . . . . ?
N9 N8 C10 C11 0.1(4) . . . . ?
Fe1 N8 C10 C11 -177.8(2) . . . . ?
N8 C10 C11 C12 -0.1(4) . . . . ?
N8 N9 C12 C11 0.0(4) . . . . ?
B1 N9 C12 C11 179.2(3) . . . . ?
C10 C11 C12 N9 0.1(4) . . . . ?
C18 N10 C14 C15 0.7(5) . . . . ?
Fe2 N10 C14 C15 -175.5(3) . . . . ?
N10 C14 C15 C16 -0.7(7) . . . . ?
C14 C15 C16 C17 0.0(8) . . . . ?
C15 C16 C17 C18 0.6(8) . . . . ?
C14 N10 C18 C17 0.0(5) . . . . ?
Fe2 N10 C18 C17 176.6(3) . . . . ?
C14 N10 C18 C19 -177.4(3) . . . . ?
Fe2 N10 C18 C19 -0.7(3) . . . . ?
C16 C17 C18 N10 -0.6(6) . . . . ?
C16 C17 C18 C19 176.5(4) . . . . ?
C26 N11 C19 C18 157.7(3) . . . . ?
C20 N11 C19 C18 -76.7(3) . . . . ?
Fe2 N11 C19 C18 42.0(3) . . . . ?
N10 C18 C19 N11 -28.3(4) . . . . ?
C17 C18 C19 N11 154.4(3) . . . . ?
C19 N11 C20 C21 138.6(3) . . . . ?
C26 N11 C20 C21 -95.4(3) . . . . ?
Fe2 N11 C20 C21 21.9(3) . . . . ?
C25 N12 C21 C22 2.9(4) . . . . ?
Fe2 N12 C21 C22 -163.5(2) . . . . ?
C25 N12 C21 C20 -173.7(3) . . . . ?
Fe2 N12 C21 C20 19.9(3) . . . . ?
N11 C20 C21 N12 -28.2(4) . . . . ?
N11 C20 C21 C22 155.2(3) . . . . ?
N12 C21 C22 C23 -1.9(5) . . . . ?
C20 C21 C22 C23 174.5(3) . . . . ?
C21 C22 C23 C24 -0.9(5) . . . . ?
C22 C23 C24 C25 2.6(6) . . . . ?
C21 N12 C25 C24 -1.2(5) . . . . ?
Fe2 N12 C25 C24 163.7(3) . . . . ?
C23 C24 C25 N12 -1.6(6) . . . . ?
C19 N11 C26 C27 -156.7(3) . . . . ?
C20 N11 C26 C27 78.7(3) . . . . ?
Fe2 N11 C26 C27 -40.7(3) . . . . ?
C31 N13 C27 C28 -2.7(5) . . . . ?
Fe2 N13 C27 C28 165.9(3) . . . . ?
C31 N13 C27 C26 177.4(3) . . . . ?
Fe2 N13 C27 C26 -14.0(3) . . . . ?
N11 C26 C27 N13 37.7(4) . . . . ?
N11 C26 C27 C28 -142.2(4) . . . . ?
N13 C27 C28 C29 3.6(7) . . . . ?
C26 C27 C28 C29 -176.6(4) . . . . ?
C27 C28 C29 C30 -2.9(8) . . . . ?
C28 C29 C30 C31 1.4(8) . . . . ?
C27 N13 C31 C30 1.2(5) . . . . ?
Fe2 N13 C31 C30 -165.8(3) . . . . ?
C29 C30 C31 N13 -0.5(6) . . . . ?

loop_
_geom_hbond_atom_site_label_D
_geom_hbond_atom_site_label_H
_geom_hbond_atom_site_label_A
_geom_hbond_distance_DH
_geom_hbond_distance_HA
_geom_hbond_distance_DA
_geom_hbond_angle_DHA
_geom_hbond_site_symmetry_A
O1S H1S O4 0.96 1.77 2.586(13) 140.6 .
O1S H1S Cl1 0.96 2.58 3.518(10) 166.2 .
C28 H28 O3' 0.93 2.60 3.331(11) 135.4 1_545
C25 H25 N1 0.93 2.66 3.169(4) 115.3 .
C24 H24 N3 0.93 2.69 3.421(5) 136.0 3_567
C20 H20B O2' 0.97 2.33 3.267(11) 161.7 1_545
C20 H20B O3 0.97 2.48 3.400(10) 158.1 1_545
C19 H19B O1S 0.97 2.55 3.505(9) 168.9 3_667
C19 H19A O1' 0.97 2.63 3.281(9) 124.8 3_667
C15 H15 O2 0.93 2.66 3.551(9) 161.8 2_647
C14 H14 O1S 0.93 2.56 3.211(9) 127.2 4_576
C12 H12 O3' 0.93 2.56 3.444(11) 158.2 2_546
C12 H12 O4 0.93 2.63 3.486(10) 152.5 2_546
C11 H11 N3 0.93 2.64 3.516(5) 157.4 3_567
C7 H7 O1' 0.93 2.58 3.325(9) 137.5 .
C7 H7 O1 0.93 2.45 3.254(8) 144.3 .
C6 H6 O2' 0.93 2.23 3.104(10) 155.4 4_575
O1S H1S O4 0.96 1.77 2.586(13) 140.6 .

_refine_diff_density_max         0.468
_refine_diff_density_min         -0.362
_refine_diff_density_rms         0.064

####################################################################### 
# 
# 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_3-100K
_database_code_depnum_ccdc_archive 'CCDC 1419287'
_audit_update_record             
;
2016-09-02 deposited with the CCDC.
2016-09-26 downloaded from the CCDC.
;

_audit_creation_method           SHELXL-2014/7
_shelx_SHELXL_version_number     2014/7
_chemical_name_systematic        ?
_chemical_name_common            ?
_chemical_melting_point          ?
_chemical_formula_moiety         'C62 H60 B2 Fe4 N26, 2(Cl O4) '
_chemical_formula_sum            'C62 H60 B2 Cl2 Fe4 N26 O8'
_chemical_formula_weight         1613.28

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'
N N 0.0061 0.0033 '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'
O O 0.0106 0.0060 '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'

_space_group_crystal_system      monoclinic
_space_group_IT_number           14
_space_group_name_H-M_alt        'P 21/c'
_space_group_name_Hall           '-P 2ybc'

_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.
;

loop_
_space_group_symop_operation_xyz
'x, y, z'
'-x, y+1/2, -z+1/2'
'-x, -y, -z'
'x, -y-1/2, z-1/2'

_cell_length_a                   12.6962(11)
_cell_length_b                   17.2719(15)
_cell_length_c                   16.5706(15)
_cell_angle_alpha                90
_cell_angle_beta                 108.5880(10)
_cell_angle_gamma                90
_cell_volume                     3444.2(5)
_cell_formula_units_Z            2
_cell_measurement_temperature    100(2)
_cell_measurement_reflns_used    7063
_cell_measurement_theta_min      2.36
_cell_measurement_theta_max      29.42

_exptl_crystal_description       block
_exptl_crystal_colour            red
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    'not measured'
_exptl_crystal_density_diffrn    1.556
_exptl_crystal_F_000             1652
_exptl_transmission_factor_min   ?
_exptl_transmission_factor_max   ?
_exptl_crystal_size_max          0.200
_exptl_crystal_size_mid          0.100
_exptl_crystal_size_min          0.070
_exptl_absorpt_coefficient_mu    0.978
_shelx_estimated_absorpt_T_min   0.828
_shelx_estimated_absorpt_T_max   0.935
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_correction_T_min  0.8284
_exptl_absorpt_correction_T_max  0.9347
_exptl_absorpt_process_details   sadabs
_exptl_absorpt_special_details   ?
_diffrn_ambient_temperature      100(2)
_diffrn_radiation_wavelength     0.71073
_diffrn_radiation_type           MoK\a
_diffrn_source                   ?
_diffrn_measurement_device_type  'Bruker APEX-II CCD'
_diffrn_measurement_method       'φ and ω scans'
_diffrn_detector_area_resol_mean ?
_diffrn_reflns_number            24676
_diffrn_reflns_av_unetI/netI     0.0354
_diffrn_reflns_av_R_equivalents  0.0393
_diffrn_reflns_limit_h_min       -15
_diffrn_reflns_limit_h_max       15
_diffrn_reflns_limit_k_min       -20
_diffrn_reflns_limit_k_max       19
_diffrn_reflns_limit_l_min       -19
_diffrn_reflns_limit_l_max       19
_diffrn_reflns_theta_min         1.692
_diffrn_reflns_theta_max         24.999
_diffrn_reflns_theta_full        24.999
_diffrn_measured_fraction_theta_max 0.993
_diffrn_measured_fraction_theta_full 0.993
_diffrn_reflns_Laue_measured_fraction_max 0.993
_diffrn_reflns_Laue_measured_fraction_full 0.993
_diffrn_reflns_point_group_measured_fraction_max 0.993
_diffrn_reflns_point_group_measured_fraction_full 0.993
_reflns_number_total             6027
_reflns_number_gt                5040
_reflns_threshold_expression     'I > 2σ(I)'
_reflns_Friedel_coverage         0.000
_reflns_Friedel_fraction_max     .
_reflns_Friedel_fraction_full    .

_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.
;

_computing_data_collection       'Bruker APEX2'
_computing_cell_refinement       'Bruker SAINT'
_computing_data_reduction        'Bruker SAINT'
_computing_structure_solution    'SHELXS-2014 (Sheldrick, 2014)'
_computing_structure_refinement  'SHELXL-2014/7 (Sheldrick, 2014)'
_computing_molecular_graphics    'Bruker SHELXTL'
_computing_publication_material  'Bruker SHELXTL'
_refine_special_details          ?
_refine_ls_structure_factor_coef Fsqd
_refine_ls_matrix_type           full
_refine_ls_weighting_scheme      calc
_refine_ls_weighting_details     
'w=1/[σ²(Fo²)+(0.0437P)²+4.1541P] where P=(Fo²+2Fc²)/3'
_atom_sites_solution_primary     ?
_atom_sites_solution_secondary   ?
_atom_sites_solution_hydrogens   geom
_refine_ls_hydrogen_treatment    constr
_refine_ls_extinction_method     none
_refine_ls_extinction_coef       .
_refine_ls_number_reflns         6027
_refine_ls_number_parameters     516
_refine_ls_number_restraints     196
_refine_ls_R_factor_all          0.0459
_refine_ls_R_factor_gt           0.0354
_refine_ls_wR_factor_ref         0.0956
_refine_ls_wR_factor_gt          0.0893
_refine_ls_goodness_of_fit_ref   1.042
_refine_ls_restrained_S_all      1.046
_refine_ls_shift/su_max          0.003
_refine_ls_shift/su_mean         0.000

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 0.26079(3) 0.57735(2) 0.92755(2) 0.01414(11) Uani 1 1 d . . . . .
Fe2 Fe 0.37196(3) 0.31588(2) 1.03770(2) 0.01467(11) Uani 1 1 d . . . . .
B1 B 0.1310(3) 0.5753(2) 0.7311(2) 0.0219(7) Uani 1 1 d . . . . .
N1 N 0.33073(18) 0.42403(13) 1.02222(14) 0.0180(5) Uani 1 1 d . . . . .
N2 N 0.48951(19) 0.65434(13) 0.98103(13) 0.0176(5) Uani 1 1 d . . . . .
N3 N 0.2100(2) 0.64640(16) 1.08182(16) 0.0286(6) Uani 1 1 d . . . . .
N4 N 0.30909(18) 0.52815(13) 0.83707(13) 0.0170(5) Uani 1 1 d . . . . .
N5 N 0.24398(19) 0.53231(13) 0.75378(13) 0.0192(5) Uani 1 1 d . . . . .
N6 N 0.20602(18) 0.66746(13) 0.85398(13) 0.0174(5) Uani 1 1 d . . . . .
N7 N 0.15673(19) 0.65794(14) 0.76838(14) 0.0201(5) Uani 1 1 d . . . . .
N8 N 0.11220(19) 0.53220(13) 0.87222(14) 0.0182(5) Uani 1 1 d . . . . .
N9 N 0.06616(19) 0.53568(13) 0.78610(14) 0.0194(5) Uani 1 1 d . . . . .
N10 N 0.45543(19) 0.31631(13) 1.16077(14) 0.0203(5) Uani 1 1 d . . . . .
N11 N 0.41089(19) 0.20412(13) 1.05134(14) 0.0196(5) Uani 1 1 d . . . . .
N12 N 0.23244(18) 0.28357(13) 1.05571(13) 0.0167(5) Uani 1 1 d . . . . .
N13 N 0.29607(19) 0.28694(14) 0.91673(14) 0.0196(5) Uani 1 1 d . . . . .
C1 C 0.3074(2) 0.48497(16) 0.99387(16) 0.0171(6) Uani 1 1 d . . . . .
C2 C 0.4044(2) 0.62536(15) 0.96998(16) 0.0162(6) Uani 1 1 d . . . . .
C3 C 0.2271(2) 0.62105(16) 1.02303(17) 0.0200(6) Uani 1 1 d . . . . .
C4 C 0.3981(2) 0.48650(16) 0.83974(18) 0.0208(6) Uani 1 1 d . . . . .
H4 H 0.4569 0.4743 0.8901 0.025 Uiso 1 1 calc R U . . .
C5 C 0.3928(2) 0.46349(18) 0.75858(19) 0.0265(7) Uani 1 1 d . . . . .
H5 H 0.4454 0.4333 0.7425 0.032 Uiso 1 1 calc R U . . .
C6 C 0.2947(3) 0.49388(18) 0.70616(19) 0.0266(7) Uani 1 1 d . . . . .
H6 H 0.2672 0.4885 0.6460 0.032 Uiso 1 1 calc R U . . .
C7 C 0.2096(2) 0.74313(16) 0.86982(18) 0.0205(6) Uani 1 1 d . . . . .
H7 H 0.2393 0.7660 0.9245 0.025 Uiso 1 1 calc R U . . .
C8 C 0.1634(2) 0.78364(18) 0.79435(19) 0.0262(7) Uani 1 1 d . . . . .
H8 H 0.1555 0.8382 0.7874 0.031 Uiso 1 1 calc R U . . .
C9 C 0.1315(2) 0.72834(17) 0.73204(19) 0.0248(7) Uani 1 1 d . . . . .
H9 H 0.0972 0.7380 0.6730 0.030 Uiso 1 1 calc R U . . .
C10 C 0.0390(2) 0.49599(16) 0.90172(19) 0.0228(6) Uani 1 1 d . . . . .
H10 H 0.0500 0.4852 0.9600 0.027 Uiso 1 1 calc R U . . .
C11 C -0.0554(2) 0.47644(18) 0.8351(2) 0.0298(7) Uani 1 1 d . . . . .
H11 H -0.1198 0.4505 0.8384 0.036 Uiso 1 1 calc R U . . .
C12 C -0.0354(2) 0.50270(17) 0.76349(19) 0.0264(7) Uani 1 1 d . . . . .
H12 H -0.0850 0.4984 0.7070 0.032 Uiso 1 1 calc R U . . .
C13 C 0.0648(3) 0.57439(19) 0.63215(18) 0.0309(7) Uani 1 1 d . . . . .
H13A H 0.1109 0.5971 0.6008 0.046 Uiso 1 1 calc R U . . .
H13B H -0.0037 0.6046 0.6212 0.046 Uiso 1 1 calc R U . . .
H13C H 0.0462 0.5209 0.6133 0.046 Uiso 1 1 calc R U . . .
C14 C 0.4547(3) 0.37032(18) 1.21821(18) 0.0264(7) Uani 1 1 d . . . . .
H14 H 0.4065 0.4135 1.2009 0.032 Uiso 1 1 calc R U . . .
C15 C 0.5221(3) 0.3654(2) 1.30251(19) 0.0368(8) Uani 1 1 d . . . . .
H15 H 0.5203 0.4047 1.3422 0.044 Uiso 1 1 calc R U . . .
C16 C 0.5919(3) 0.3024(2) 1.3275(2) 0.0413(9) Uani 1 1 d . . . . .
H16 H 0.6394 0.2981 1.3847 0.050 Uiso 1 1 calc R U . . .
C17 C 0.5923(3) 0.2459(2) 1.2693(2) 0.0333(8) Uani 1 1 d . . . . .
H17 H 0.6389 0.2017 1.2859 0.040 Uiso 1 1 calc R U . . .
C18 C 0.5240(2) 0.25420(18) 1.18623(18) 0.0243(7) Uani 1 1 d . . . . .
C19 C 0.5218(2) 0.19797(17) 1.11662(19) 0.0251(7) Uani 1 1 d . . . . .
H19A H 0.5807 0.2108 1.0915 0.030 Uiso 1 1 calc R U . . .
H19B H 0.5344 0.1446 1.1395 0.030 Uiso 1 1 calc R U . . .
C20 C 0.3271(2) 0.16191(17) 1.08085(19) 0.0238(6) Uani 1 1 d . . . . .
H20A H 0.3579 0.1527 1.1429 0.029 Uiso 1 1 calc R U . . .
H20B H 0.3114 0.1109 1.0522 0.029 Uiso 1 1 calc R U . . .
C21 C 0.2210(2) 0.20699(16) 1.06187(16) 0.0188(6) Uani 1 1 d . . . . .
C22 C 0.1201(2) 0.17238(18) 1.05570(17) 0.0240(6) Uani 1 1 d . . . . .
H22 H 0.1141 0.1177 1.0584 0.029 Uiso 1 1 calc R U . . .
C23 C 0.0283(2) 0.21917(19) 1.04551(18) 0.0285(7) Uani 1 1 d . . . . .
H23 H -0.0420 0.1971 1.0404 0.034 Uiso 1 1 calc R U . . .
C24 C 0.0404(2) 0.29813(19) 1.04285(19) 0.0284(7) Uani 1 1 d . . . . .
H24 H -0.0208 0.3315 1.0381 0.034 Uiso 1 1 calc R U . . .
C25 C 0.1428(2) 0.32826(17) 1.04721(18) 0.0237(6) Uani 1 1 d . . . . .
H25 H 0.1502 0.3828 1.0441 0.028 Uiso 1 1 calc R U . . .
C26 C 0.4113(2) 0.17569(17) 0.96664(18) 0.0241(6) Uani 1 1 d . . . . .
H26A H 0.4036 0.1186 0.9638 0.029 Uiso 1 1 calc R U . . .
H26B H 0.4821 0.1897 0.9573 0.029 Uiso 1 1 calc R U . . .
C27 C 0.3155(2) 0.21255(17) 0.89972(18) 0.0228(6) Uani 1 1 d . . . . .
C28 C 0.2517(3) 0.1751(2) 0.8272(2) 0.0342(8) Uani 1 1 d . . . . .
H28 H 0.2652 0.1223 0.8176 0.041 Uiso 1 1 calc R U . . .
C29 C 0.1674(3) 0.2158(2) 0.7683(2) 0.0415(9) Uani 1 1 d . . . . .
H29 H 0.1222 0.1912 0.7179 0.050 Uiso 1 1 calc R U . . .
C30 C 0.1500(3) 0.2924(2) 0.78397(19) 0.0340(8) Uani 1 1 d . . . . .
H30 H 0.0939 0.3216 0.7438 0.041 Uiso 1 1 calc R U . . .
C31 C 0.2151(2) 0.32605(18) 0.85849(17) 0.0242(6) Uani 1 1 d . . . . .
H31 H 0.2024 0.3787 0.8692 0.029 Uiso 1 1 calc R U . . .
Cl1 Cl 0.2575(10) 0.5527(7) 0.4511(8) 0.035(2) Uani 0.143(4) 1 d D U P A 1
O1 O 0.1476(10) 0.5877(8) 0.4243(10) 0.043(3) Uani 0.143(4) 1 d D U P A 1
O2 O 0.275(2) 0.5148(12) 0.3794(12) 0.056(5) Uani 0.143(4) 1 d D U P A 1
O3 O 0.2591(18) 0.4949(11) 0.5132(12) 0.073(4) Uani 0.143(4) 1 d D U P A 1
O4 O 0.3358(12) 0.6133(8) 0.4829(10) 0.040(3) Uani 0.143(4) 1 d D U P A 1
Cl1' Cl 0.28325(18) 0.54256(11) 0.46428(13) 0.0361(5) Uani 0.857(4) 1 d D U P A
2
O1' O 0.1997(3) 0.48814(18) 0.4662(2) 0.0505(9) Uani 0.857(4) 1 d D U P A 2
O2' O 0.2908(4) 0.5461(2) 0.3803(2) 0.0558(11) Uani 0.857(4) 1 d D U P A 2
O3' O 0.3874(2) 0.51743(17) 0.52374(17) 0.0441(8) Uani 0.857(4) 1 d D U P A 2
O4' O 0.2552(4) 0.61705(18) 0.4897(2) 0.0715(12) Uani 0.857(4) 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
Fe1 C3 1.921(3) . ?
Fe1 C1 1.921(3) . ?
Fe1 C2 1.921(3) . ?
Fe1 N6 1.962(2) . ?
Fe1 N8 1.976(2) . ?
Fe1 N4 1.983(2) . ?
Fe2 N1 1.935(2) . ?
Fe2 N2 1.950(2) 3_667 ?
Fe2 N12 1.969(2) . ?
Fe2 N10 1.976(2) . ?
Fe2 N11 1.987(2) . ?
Fe2 N13 1.991(2) . ?
B1 N7 1.548(4) . ?
B1 N5 1.551(4) . ?
B1 N9 1.568(4) . ?
B1 C13 1.586(4) . ?
N1 C1 1.152(3) . ?
N2 C2 1.151(3) . ?
N2 Fe2 1.950(2) 3_667 ?
N3 C3 1.150(4) . ?
N4 C4 1.328(4) . ?
N4 N5 1.366(3) . ?
N5 C6 1.342(4) . ?
N6 C7 1.331(4) . ?
N6 N7 1.366(3) . ?
N7 C9 1.349(4) . ?
N8 C10 1.336(4) . ?
N8 N9 1.360(3) . ?
N9 C12 1.349(4) . ?
N10 C14 1.335(4) . ?
N10 C18 1.361(4) . ?
N11 C19 1.481(4) . ?
N11 C26 1.488(4) . ?
N11 C20 1.495(3) . ?
N12 C21 1.338(4) . ?
N12 C25 1.345(4) . ?
N13 C31 1.346(4) . ?
N13 C27 1.355(4) . ?
C4 C5 1.383(4) . ?
C4 H4 0.9500 . ?
C5 C6 1.376(4) . ?
C5 H5 0.9500 . ?
C6 H6 0.9500 . ?
C7 C8 1.389(4) . ?
C7 H7 0.9500 . ?
C8 C9 1.370(4) . ?
C8 H8 0.9500 . ?
C9 H9 0.9500 . ?
C10 C11 1.388(4) . ?
C10 H10 0.9500 . ?
C11 C12 1.367(4) . ?
C11 H11 0.9500 . ?
C12 H12 0.9500 . ?
C13 H13A 0.9800 . ?
C13 H13B 0.9800 . ?
C13 H13C 0.9800 . ?
C14 C15 1.389(4) . ?
C14 H14 0.9500 . ?
C15 C16 1.381(5) . ?
C15 H15 0.9500 . ?
C16 C17 1.374(5) . ?
C16 H16 0.9500 . ?
C17 C18 1.381(4) . ?
C17 H17 0.9500 . ?
C18 C19 1.501(4) . ?
C19 H19A 0.9900 . ?
C19 H19B 0.9900 . ?
C20 C21 1.500(4) . ?
C20 H20A 0.9900 . ?
C20 H20B 0.9900 . ?
C21 C22 1.388(4) . ?
C22 C23 1.383(4) . ?
C22 H22 0.9500 . ?
C23 C24 1.375(5) . ?
C23 H23 0.9500 . ?
C24 C25 1.380(4) . ?
C24 H24 0.9500 . ?
C25 H25 0.9500 . ?
C26 C27 1.501(4) . ?
C26 H26A 0.9900 . ?
C26 H26B 0.9900 . ?
C27 C28 1.378(4) . ?
C28 C29 1.388(5) . ?
C28 H28 0.9500 . ?
C29 C30 1.381(5) . ?
C29 H29 0.9500 . ?
C30 C31 1.376(4) . ?
C30 H30 0.9500 . ?
C31 H31 0.9500 . ?
Cl1 O4 1.424(9) . ?
Cl1 O3 1.430(9) . ?
Cl1 O2 1.437(9) . ?
Cl1 O1 1.454(9) . ?
Cl1' O2' 1.426(3) . ?
Cl1' O1' 1.425(3) . ?
Cl1' O4' 1.433(4) . ?
Cl1' O3' 1.441(3) . ?

loop_
_geom_angle_atom_site_label_1
_geom_angle_atom_site_label_2
_geom_angle_atom_site_label_3
_geom_angle
_geom_angle_site_symmetry_1
_geom_angle_site_symmetry_3
_geom_angle_publ_flag
C3 Fe1 C1 87.95(11) . . ?
C3 Fe1 C2 87.92(11) . . ?
C1 Fe1 C2 93.76(11) . . ?
C3 Fe1 N6 94.14(11) . . ?
C1 Fe1 N6 176.16(10) . . ?
C2 Fe1 N6 89.55(10) . . ?
C3 Fe1 N8 96.13(10) . . ?
C1 Fe1 N8 90.70(10) . . ?
C2 Fe1 N8 174.09(10) . . ?
N6 Fe1 N8 85.87(9) . . ?
C3 Fe1 N4 174.39(11) . . ?
C1 Fe1 N4 87.90(10) . . ?
C2 Fe1 N4 88.60(10) . . ?
N6 Fe1 N4 90.23(9) . . ?
N8 Fe1 N4 87.69(9) . . ?
N1 Fe2 N2 86.79(9) . 3_667 ?
N1 Fe2 N12 94.31(9) . . ?
N2 Fe2 N12 178.77(9) 3_667 . ?
N1 Fe2 N10 99.59(10) . . ?
N2 Fe2 N10 87.08(9) 3_667 . ?
N12 Fe2 N10 93.27(9) . . ?
N1 Fe2 N11 178.59(10) . . ?
N2 Fe2 N11 94.02(9) 3_667 . ?
N12 Fe2 N11 84.87(9) . . ?
N10 Fe2 N11 81.61(10) . . ?
N1 Fe2 N13 94.89(10) . . ?
N2 Fe2 N13 94.45(9) 3_667 . ?
N12 Fe2 N13 84.91(9) . . ?
N10 Fe2 N13 165.50(10) . . ?
N11 Fe2 N13 83.90(10) . . ?
N7 B1 N5 106.5(2) . . ?
N7 B1 N9 104.7(2) . . ?
N5 B1 N9 105.4(2) . . ?
N7 B1 C13 113.4(2) . . ?
N5 B1 C13 113.0(2) . . ?
N9 B1 C13 113.1(2) . . ?
C1 N1 Fe2 163.6(2) . . ?
C2 N2 Fe2 159.7(2) . 3_667 ?
C4 N4 N5 107.2(2) . . ?
C4 N4 Fe1 132.20(19) . . ?
N5 N4 Fe1 120.53(17) . . ?
C6 N5 N4 108.6(2) . . ?
C6 N5 B1 132.4(2) . . ?
N4 N5 B1 119.0(2) . . ?
C7 N6 N7 107.4(2) . . ?
C7 N6 Fe1 132.32(19) . . ?
N7 N6 Fe1 120.27(17) . . ?
C9 N7 N6 108.7(2) . . ?
C9 N7 B1 131.5(2) . . ?
N6 N7 B1 119.6(2) . . ?
C10 N8 N9 106.8(2) . . ?
C10 N8 Fe1 133.5(2) . . ?
N9 N8 Fe1 119.79(17) . . ?
C12 N9 N8 109.0(2) . . ?
C12 N9 B1 131.0(2) . . ?
N8 N9 B1 120.0(2) . . ?
C14 N10 C18 118.6(2) . . ?
C14 N10 Fe2 128.0(2) . . ?
C18 N10 Fe2 113.37(19) . . ?
C19 N11 C26 112.1(2) . . ?
C19 N11 C20 109.7(2) . . ?
C26 N11 C20 111.4(2) . . ?
C19 N11 Fe2 107.26(17) . . ?
C26 N11 Fe2 106.77(17) . . ?
C20 N11 Fe2 109.50(17) . . ?
C21 N12 C25 117.8(2) . . ?
C21 N12 Fe2 114.64(18) . . ?
C25 N12 Fe2 126.43(19) . . ?
C31 N13 C27 118.4(2) . . ?
C31 N13 Fe2 127.6(2) . . ?
C27 N13 Fe2 112.68(18) . . ?
N1 C1 Fe1 169.9(2) . . ?
N2 C2 Fe1 168.3(2) . . ?
N3 C3 Fe1 177.9(3) . . ?
N4 C4 C5 110.3(3) . . ?
N4 C4 H4 124.9 . . ?
C5 C4 H4 124.9 . . ?
C6 C5 C4 104.9(3) . . ?
C6 C5 H5 127.5 . . ?
C4 C5 H5 127.5 . . ?
N5 C6 C5 109.0(3) . . ?
N5 C6 H6 125.5 . . ?
C5 C6 H6 125.5 . . ?
N6 C7 C8 109.8(3) . . ?
N6 C7 H7 125.1 . . ?
C8 C7 H7 125.1 . . ?
C9 C8 C7 105.4(3) . . ?
C9 C8 H8 127.3 . . ?
C7 C8 H8 127.3 . . ?
N7 C9 C8 108.7(3) . . ?
N7 C9 H9 125.6 . . ?
C8 C9 H9 125.6 . . ?
N8 C10 C11 110.3(3) . . ?
N8 C10 H10 124.8 . . ?
C11 C10 H10 124.8 . . ?
C12 C11 C10 104.9(3) . . ?
C12 C11 H11 127.5 . . ?
C10 C11 H11 127.5 . . ?
N9 C12 C11 108.9(3) . . ?
N9 C12 H12 125.5 . . ?
C11 C12 H12 125.5 . . ?
B1 C13 H13A 109.5 . . ?
B1 C13 H13B 109.5 . . ?
H13A C13 H13B 109.5 . . ?
B1 C13 H13C 109.5 . . ?
H13A C13 H13C 109.5 . . ?
H13B C13 H13C 109.5 . . ?
N10 C14 C15 122.2(3) . . ?
N10 C14 H14 118.9 . . ?
C15 C14 H14 118.9 . . ?
C16 C15 C14 118.7(3) . . ?
C16 C15 H15 120.6 . . ?
C14 C15 H15 120.6 . . ?
C17 C16 C15 119.7(3) . . ?
C17 C16 H16 120.2 . . ?
C15 C16 H16 120.2 . . ?
C16 C17 C18 119.0(3) . . ?
C16 C17 H17 120.5 . . ?
C18 C17 H17 120.5 . . ?
N10 C18 C17 121.8(3) . . ?
N10 C18 C19 114.7(2) . . ?
C17 C18 C19 123.4(3) . . ?
N11 C19 C18 107.2(2) . . ?
N11 C19 H19A 110.3 . . ?
C18 C19 H19A 110.3 . . ?
N11 C19 H19B 110.3 . . ?
C18 C19 H19B 110.3 . . ?
H19A C19 H19B 108.5 . . ?
N11 C20 C21 111.3(2) . . ?
N11 C20 H20A 109.4 . . ?
C21 C20 H20A 109.4 . . ?
N11 C20 H20B 109.4 . . ?
C21 C20 H20B 109.4 . . ?
H20A C20 H20B 108.0 . . ?
N12 C21 C22 122.7(3) . . ?
N12 C21 C20 114.6(2) . . ?
C22 C21 C20 122.6(3) . . ?
C23 C22 C21 118.6(3) . . ?
C23 C22 H22 120.7 . . ?
C21 C22 H22 120.7 . . ?
C24 C23 C22 119.0(3) . . ?
C24 C23 H23 120.5 . . ?
C22 C23 H23 120.5 . . ?
C23 C24 C25 119.0(3) . . ?
C23 C24 H24 120.5 . . ?
C25 C24 H24 120.5 . . ?
N12 C25 C24 122.7(3) . . ?
N12 C25 H25 118.6 . . ?
C24 C25 H25 118.6 . . ?
N11 C26 C27 108.1(2) . . ?
N11 C26 H26A 110.1 . . ?
C27 C26 H26A 110.1 . . ?
N11 C26 H26B 110.1 . . ?
C27 C26 H26B 110.1 . . ?
H26A C26 H26B 108.4 . . ?
N13 C27 C28 122.1(3) . . ?
N13 C27 C26 114.0(2) . . ?
C28 C27 C26 123.9(3) . . ?
C27 C28 C29 118.8(3) . . ?
C27 C28 H28 120.6 . . ?
C29 C28 H28 120.6 . . ?
C30 C29 C28 119.2(3) . . ?
C30 C29 H29 120.4 . . ?
C28 C29 H29 120.4 . . ?
C31 C30 C29 119.1(3) . . ?
C31 C30 H30 120.4 . . ?
C29 C30 H30 120.4 . . ?
N13 C31 C30 122.3(3) . . ?
N13 C31 H31 118.8 . . ?
C30 C31 H31 118.8 . . ?
O4 Cl1 O3 113.4(11) . . ?
O4 Cl1 O2 111.4(11) . . ?
O3 Cl1 O2 108.0(12) . . ?
O4 Cl1 O1 107.2(10) . . ?
O3 Cl1 O1 107.6(11) . . ?
O2 Cl1 O1 109.1(11) . . ?
O2' Cl1' O1' 109.4(2) . . ?
O2' Cl1' O4' 110.4(3) . . ?
O1' Cl1' O4' 109.2(3) . . ?
O2' Cl1' O3' 110.3(3) . . ?
O1' Cl1' O3' 108.3(2) . . ?
O4' Cl1' O3' 109.2(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
C4 N4 N5 C6 -0.8(3) . . . . ?
Fe1 N4 N5 C6 -179.26(19) . . . . ?
C4 N4 N5 B1 177.8(2) . . . . ?
Fe1 N4 N5 B1 -0.7(3) . . . . ?
N7 B1 N5 C6 -126.3(3) . . . . ?
N9 B1 N5 C6 122.8(3) . . . . ?
C13 B1 N5 C6 -1.2(4) . . . . ?
N7 B1 N5 N4 55.5(3) . . . . ?
N9 B1 N5 N4 -55.4(3) . . . . ?
C13 B1 N5 N4 -179.4(2) . . . . ?
C7 N6 N7 C9 0.7(3) . . . . ?
Fe1 N6 N7 C9 -177.17(18) . . . . ?
C7 N6 N7 B1 -174.6(2) . . . . ?
Fe1 N6 N7 B1 7.6(3) . . . . ?
N5 B1 N7 C9 126.0(3) . . . . ?
N9 B1 N7 C9 -122.7(3) . . . . ?
C13 B1 N7 C9 1.1(4) . . . . ?
N5 B1 N7 N6 -60.0(3) . . . . ?
N9 B1 N7 N6 51.4(3) . . . . ?
C13 B1 N7 N6 175.1(2) . . . . ?
C10 N8 N9 C12 0.9(3) . . . . ?
Fe1 N8 N9 C12 -178.83(19) . . . . ?
C10 N8 N9 B1 179.8(2) . . . . ?
Fe1 N8 N9 B1 0.1(3) . . . . ?
N7 B1 N9 C12 122.8(3) . . . . ?
N5 B1 N9 C12 -125.1(3) . . . . ?
C13 B1 N9 C12 -1.2(4) . . . . ?
N7 B1 N9 N8 -55.9(3) . . . . ?
N5 B1 N9 N8 56.3(3) . . . . ?
C13 B1 N9 N8 -179.8(2) . . . . ?
Fe2 N1 C1 Fe1 23(2) . . . . ?
Fe2 N2 C2 Fe1 -25.6(17) 3_667 . . . ?
N5 N4 C4 C5 0.5(3) . . . . ?
Fe1 N4 C4 C5 178.7(2) . . . . ?
N4 C4 C5 C6 0.0(3) . . . . ?
N4 N5 C6 C5 0.8(3) . . . . ?
B1 N5 C6 C5 -177.5(3) . . . . ?
C4 C5 C6 N5 -0.5(3) . . . . ?
N7 N6 C7 C8 -0.5(3) . . . . ?
Fe1 N6 C7 C8 177.0(2) . . . . ?
N6 C7 C8 C9 0.1(3) . . . . ?
N6 N7 C9 C8 -0.6(3) . . . . ?
B1 N7 C9 C8 173.9(3) . . . . ?
C7 C8 C9 N7 0.3(3) . . . . ?
N9 N8 C10 C11 -0.6(3) . . . . ?
Fe1 N8 C10 C11 179.1(2) . . . . ?
N8 C10 C11 C12 0.1(3) . . . . ?
N8 N9 C12 C11 -0.9(3) . . . . ?
B1 N9 C12 C11 -179.6(3) . . . . ?
C10 C11 C12 N9 0.5(3) . . . . ?
C18 N10 C14 C15 0.6(4) . . . . ?
Fe2 N10 C14 C15 -176.6(2) . . . . ?
N10 C14 C15 C16 -0.2(5) . . . . ?
C14 C15 C16 C17 -0.7(5) . . . . ?
C15 C16 C17 C18 1.2(5) . . . . ?
C14 N10 C18 C17 -0.1(4) . . . . ?
Fe2 N10 C18 C17 177.5(2) . . . . ?
C14 N10 C18 C19 -178.1(2) . . . . ?
Fe2 N10 C18 C19 -0.5(3) . . . . ?
C16 C17 C18 N10 -0.8(4) . . . . ?
C16 C17 C18 C19 177.0(3) . . . . ?
C26 N11 C19 C18 158.2(2) . . . . ?
C20 N11 C19 C18 -77.5(3) . . . . ?
Fe2 N11 C19 C18 41.3(2) . . . . ?
N10 C18 C19 N11 -27.2(3) . . . . ?
C17 C18 C19 N11 154.8(3) . . . . ?
C19 N11 C20 C21 137.8(2) . . . . ?
C26 N11 C20 C21 -97.5(3) . . . . ?
Fe2 N11 C20 C21 20.3(3) . . . . ?
C25 N12 C21 C22 3.2(4) . . . . ?
Fe2 N12 C21 C22 -165.4(2) . . . . ?
C25 N12 C21 C20 -173.5(2) . . . . ?
Fe2 N12 C21 C20 17.9(3) . . . . ?
N11 C20 C21 N12 -25.4(3) . . . . ?
N11 C20 C21 C22 157.8(2) . . . . ?
N12 C21 C22 C23 -2.1(4) . . . . ?
C20 C21 C22 C23 174.3(3) . . . . ?
C21 C22 C23 C24 -0.8(4) . . . . ?
C22 C23 C24 C25 2.4(4) . . . . ?
C21 N12 C25 C24 -1.4(4) . . . . ?
Fe2 N12 C25 C24 165.6(2) . . . . ?
C23 C24 C25 N12 -1.4(4) . . . . ?
C19 N11 C26 C27 -157.0(2) . . . . ?
C20 N11 C26 C27 79.7(3) . . . . ?
Fe2 N11 C26 C27 -39.8(2) . . . . ?
C31 N13 C27 C28 -3.3(4) . . . . ?
Fe2 N13 C27 C28 164.2(2) . . . . ?
C31 N13 C27 C26 177.0(2) . . . . ?
Fe2 N13 C27 C26 -15.5(3) . . . . ?
N11 C26 C27 N13 37.2(3) . . . . ?
N11 C26 C27 C28 -142.5(3) . . . . ?
N13 C27 C28 C29 2.4(5) . . . . ?
C26 C27 C28 C29 -178.0(3) . . . . ?
C27 C28 C29 C30 0.1(5) . . . . ?
C28 C29 C30 C31 -1.5(5) . . . . ?
C27 N13 C31 C30 1.8(4) . . . . ?
Fe2 N13 C31 C30 -163.6(2) . . . . ?
C29 C30 C31 N13 0.6(5) . . . . ?

_refine_diff_density_max         1.509
_refine_diff_density_min         -0.389
_refine_diff_density_rms         0.068

####################################################################### 
# 
# 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_3-296K
# Added during the CSD deposition process: Friday 02 September 2016 02:49 AM
# end Validation Reply Form

_database_code_depnum_ccdc_archive 'CCDC 1419288'
_audit_update_record             
;
2016-09-02 deposited with the CCDC.
2016-09-26 downloaded from the CCDC.
;
# start Validation Reply Form
_vrf_PLAT232_3-296K              
;
PROBLEM: Hirshfeld Test Diff (M-X)  Fe2    --  N1      ..       12.2 s.u.
RESPONSE: At 296 K, the Fe(II) atom of the complex is in the middle of spin \ transition process. So, there will be a rather obvious variation of Fe-N bond length and it cann't to be treated well as a disordered model.
;
_vrf_PLAT232_3-296K_2            
;
PROBLEM: Hirshfeld Test Diff (M-X)  Fe2    --  N2_a    ..       11.4 s.u.
RESPONSE: At 296 K, the Fe(II) atom of the complex is in the middle of spin \ transition process. So, there will be a rather obvious variation of Fe-N bond length and it cann't to be treated well as a disordered model.
;

_audit_creation_method           SHELXL-2014/7
_shelx_SHELXL_version_number     2014/7
_chemical_name_systematic        ?
_chemical_name_common            ?
_chemical_melting_point          ?
_chemical_formula_moiety         'C62 H60 B2 Fe4 N26, 2(Cl O4) '
_chemical_formula_sum            'C62 H60 B2 Cl2 Fe4 N26 O8'
_chemical_formula_weight         1613.28

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'
N N 0.0061 0.0033 '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'
O O 0.0106 0.0060 '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'

_space_group_crystal_system      monoclinic
_space_group_IT_number           14
_space_group_name_H-M_alt        'P 21/c'
_space_group_name_Hall           '-P 2ybc'

_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.
;

loop_
_space_group_symop_operation_xyz
'x, y, z'
'-x, y+1/2, -z+1/2'
'-x, -y, -z'
'x, -y-1/2, z-1/2'

_cell_length_a                   12.9011(17)
_cell_length_b                   17.554(2)
_cell_length_c                   16.696(2)
_cell_angle_alpha                90
_cell_angle_beta                 108.167(2)
_cell_angle_gamma                90
_cell_volume                     3592.6(8)
_cell_formula_units_Z            2
_cell_measurement_temperature    296(2)
_cell_measurement_reflns_used    8937
_cell_measurement_theta_min      2.32
_cell_measurement_theta_max      25.96

_exptl_crystal_description       block
_exptl_crystal_colour            red
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    'not measured'
_exptl_crystal_density_diffrn    1.491
_exptl_crystal_F_000             1652
_exptl_transmission_factor_min   ?
_exptl_transmission_factor_max   ?
_exptl_crystal_size_max          0.200
_exptl_crystal_size_mid          0.100
_exptl_crystal_size_min          0.070
_exptl_absorpt_coefficient_mu    0.938
_shelx_estimated_absorpt_T_min   0.835
_shelx_estimated_absorpt_T_max   0.937
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_correction_T_min  0.8346
_exptl_absorpt_correction_T_max  0.9372
_exptl_absorpt_process_details   sadabs
_exptl_absorpt_special_details   ?
_diffrn_ambient_temperature      296(2)
_diffrn_radiation_wavelength     0.71073
_diffrn_radiation_type           MoK\a
_diffrn_source                   ?
_diffrn_measurement_device_type  'Bruker APEX-II CCD'
_diffrn_measurement_method       'φ and ω scans'
_diffrn_detector_area_resol_mean ?
_diffrn_reflns_number            26111
_diffrn_reflns_av_unetI/netI     0.0350
_diffrn_reflns_av_R_equivalents  0.0357
_diffrn_reflns_limit_h_min       -15
_diffrn_reflns_limit_h_max       15
_diffrn_reflns_limit_k_min       -20
_diffrn_reflns_limit_k_max       20
_diffrn_reflns_limit_l_min       -19
_diffrn_reflns_limit_l_max       19
_diffrn_reflns_theta_min         1.661
_diffrn_reflns_theta_max         24.999
_diffrn_reflns_theta_full        24.999
_diffrn_measured_fraction_theta_max 0.994
_diffrn_measured_fraction_theta_full 0.994
_diffrn_reflns_Laue_measured_fraction_max 0.994
_diffrn_reflns_Laue_measured_fraction_full 0.994
_diffrn_reflns_point_group_measured_fraction_max 0.994
_diffrn_reflns_point_group_measured_fraction_full 0.994
_reflns_number_total             6295
_reflns_number_gt                5216
_reflns_threshold_expression     'I > 2σ(I)'
_reflns_Friedel_coverage         0.000
_reflns_Friedel_fraction_max     .
_reflns_Friedel_fraction_full    .

_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.
;

_computing_data_collection       'Bruker APEX2'
_computing_cell_refinement       'Bruker SAINT'
_computing_data_reduction        'Bruker SAINT'
_computing_structure_solution    'SHELXS-2014 (Sheldrick, 2014)'
_computing_structure_refinement  'SHELXL-2014/7 (Sheldrick, 2014)'
_computing_molecular_graphics    'Bruker SHELXTL'
_computing_publication_material  'Bruker SHELXTL'
_refine_special_details          ?
_refine_ls_structure_factor_coef Fsqd
_refine_ls_matrix_type           full
_refine_ls_weighting_scheme      calc
_refine_ls_weighting_details     
'w=1/[σ²(Fo²)+(0.0593P)²+1.9922P] where P=(Fo²+2Fc²)/3'
_atom_sites_solution_primary     ?
_atom_sites_solution_secondary   ?
_atom_sites_solution_hydrogens   geom
_refine_ls_hydrogen_treatment    constr
_refine_ls_extinction_method     none
_refine_ls_extinction_coef       .
_refine_ls_number_reflns         6295
_refine_ls_number_parameters     516
_refine_ls_number_restraints     176
_refine_ls_R_factor_all          0.0490
_refine_ls_R_factor_gt           0.0380
_refine_ls_wR_factor_ref         0.1140
_refine_ls_wR_factor_gt          0.1041
_refine_ls_goodness_of_fit_ref   1.069
_refine_ls_restrained_S_all      1.110
_refine_ls_shift/su_max          0.002
_refine_ls_shift/su_mean         0.000

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 0.25880(3) 0.57706(2) 0.92691(2) 0.03257(12) Uani 1 1 d . . . . .
Fe2 Fe 0.37451(3) 0.32014(2) 1.03911(2) 0.03434(13) Uani 1 1 d . . . . .
B1 B 0.1309(3) 0.5736(2) 0.7337(2) 0.0489(8) Uani 1 1 d . . . . .
N1 N 0.3311(2) 0.43017(15) 1.02705(17) 0.0506(6) Uani 1 1 d . . . . .
N2 N 0.4839(2) 0.65133(14) 0.98454(16) 0.0461(6) Uani 1 1 d . . . . .
N3 N 0.2045(3) 0.6458(2) 1.0776(2) 0.0707(9) Uani 1 1 d . . . . .
N4 N 0.30625(18) 0.52878(12) 0.83712(14) 0.0383(5) Uani 1 1 d . . . . .
N5 N 0.2427(2) 0.53225(14) 0.75564(15) 0.0455(6) Uani 1 1 d . . . . .
N6 N 0.20503(18) 0.66539(12) 0.85356(15) 0.0390(5) Uani 1 1 d . . . . .
N7 N 0.1554(2) 0.65531(14) 0.76941(15) 0.0450(6) Uani 1 1 d . . . . .
N8 N 0.11340(19) 0.53177(13) 0.87380(15) 0.0406(5) Uani 1 1 d . . . . .
N9 N 0.06844(19) 0.53449(14) 0.78870(15) 0.0462(6) Uani 1 1 d . . . . .
N10 N 0.4629(2) 0.31243(15) 1.16566(16) 0.0504(6) Uani 1 1 d . . . . .
N11 N 0.40945(19) 0.20302(13) 1.05207(15) 0.0411(5) Uani 1 1 d . . . . .
N12 N 0.23077(19) 0.28307(13) 1.05909(15) 0.0428(6) Uani 1 1 d . . . . .
N13 N 0.2969(2) 0.28495(15) 0.91532(16) 0.0478(6) Uani 1 1 d . . . . .
C1 C 0.3061(2) 0.48815(16) 0.99468(18) 0.0387(6) Uani 1 1 d . . . . .
C2 C 0.3998(2) 0.62322(15) 0.96969(16) 0.0360(6) Uani 1 1 d . . . . .
C3 C 0.2231(2) 0.62058(17) 1.0205(2) 0.0447(7) Uani 1 1 d . . . . .
C4 C 0.3946(2) 0.48863(17) 0.8396(2) 0.0482(7) Uani 1 1 d . . . . .
H4 H 0.4516 0.4774 0.8882 0.058 Uiso 1 1 calc R U . . .
C5 C 0.3891(3) 0.4662(2) 0.7592(2) 0.0624(9) Uani 1 1 d . . . . .
H5 H 0.4401 0.4375 0.7433 0.075 Uiso 1 1 calc R U . . .
C6 C 0.2935(3) 0.4949(2) 0.7083(2) 0.0605(9) Uani 1 1 d . . . . .
H6 H 0.2674 0.4896 0.6500 0.073 Uiso 1 1 calc R U . . .
C7 C 0.2090(2) 0.74029(16) 0.8681(2) 0.0474(7) Uani 1 1 d . . . . .
H7 H 0.2387 0.7630 0.9206 0.057 Uiso 1 1 calc R U . . .
C8 C 0.1627(3) 0.77879(19) 0.7937(3) 0.0637(10) Uani 1 1 d . . . . .
H8 H 0.1553 0.8312 0.7862 0.076 Uiso 1 1 calc R U . . .
C9 C 0.1300(3) 0.7240(2) 0.7331(2) 0.0618(9) Uani 1 1 d . . . . .
H9 H 0.0958 0.7327 0.6760 0.074 Uiso 1 1 calc R U . . .
C10 C 0.0434(3) 0.49499(18) 0.9046(2) 0.0530(8) Uani 1 1 d . . . . .
H10 H 0.0544 0.4850 0.9613 0.064 Uiso 1 1 calc R U . . .
C11 C -0.0479(3) 0.4741(2) 0.8391(3) 0.0695(10) Uani 1 1 d . . . . .
H11 H -0.1090 0.4482 0.8429 0.083 Uiso 1 1 calc R U . . .
C12 C -0.0291(3) 0.4996(2) 0.7685(3) 0.0644(10) Uani 1 1 d . . . . .
H12 H -0.0767 0.4938 0.7141 0.077 Uiso 1 1 calc R U . . .
C13 C 0.0655(4) 0.5720(2) 0.6359(2) 0.0756(12) Uani 1 1 d . . . . .
H13A H 0.1051 0.6000 0.6056 0.113 Uiso 1 1 calc R U . . .
H13B H -0.0050 0.5947 0.6265 0.113 Uiso 1 1 calc R U . . .
H13C H 0.0568 0.5202 0.6164 0.113 Uiso 1 1 calc R U . . .
C14 C 0.4684(4) 0.3644(2) 1.2251(2) 0.0747(12) Uani 1 1 d . . . . .
H14 H 0.4255 0.4080 1.2116 0.090 Uiso 1 1 calc R U . . .
C15 C 0.5383(5) 0.3542(3) 1.3079(3) 0.0981(17) Uani 1 1 d . U . . .
H15 H 0.5427 0.3910 1.3489 0.118 Uiso 1 1 calc R U . . .
C16 C 0.5991(5) 0.2902(4) 1.3268(3) 0.1056(18) Uani 1 1 d . U . . .
H16 H 0.6457 0.2828 1.3813 0.127 Uiso 1 1 calc R U . . .
C17 C 0.5928(3) 0.2371(3) 1.2676(3) 0.0849(14) Uani 1 1 d . . . . .
H17 H 0.6340 0.1927 1.2810 0.102 Uiso 1 1 calc R U . . .
C18 C 0.5248(3) 0.2491(2) 1.1868(2) 0.0557(9) Uani 1 1 d . . . . .
C19 C 0.5178(3) 0.19557(19) 1.1158(2) 0.0556(8) Uani 1 1 d . . . . .
H19A H 0.5743 0.2075 1.0907 0.067 Uiso 1 1 calc R U . . .
H19B H 0.5287 0.1437 1.1366 0.067 Uiso 1 1 calc R U . . .
C20 C 0.3259(3) 0.16386(17) 1.0822(2) 0.0512(8) Uani 1 1 d . . . . .
H20A H 0.3551 0.1564 1.1427 0.061 Uiso 1 1 calc R U . . .
H20B H 0.3110 0.1140 1.0561 0.061 Uiso 1 1 calc R U . . .
C21 C 0.2214(2) 0.20760(17) 1.06278(18) 0.0417(6) Uani 1 1 d . . . . .
C22 C 0.1227(3) 0.1721(2) 1.0549(2) 0.0575(9) Uani 1 1 d . . . . .
H22 H 0.1180 0.1193 1.0562 0.069 Uiso 1 1 calc R U . . .
C23 C 0.0320(3) 0.2169(3) 1.0450(2) 0.0707(11) Uani 1 1 d . . . . .
H23 H -0.0354 0.1946 1.0390 0.085 Uiso 1 1 calc R U . . .
C24 C 0.0419(3) 0.2943(3) 1.0441(3) 0.0742(11) Uani 1 1 d . . . . .
H24 H -0.0182 0.3254 1.0393 0.089 Uiso 1 1 calc R U . . .
C25 C 0.1409(3) 0.3255(2) 1.0504(2) 0.0604(9) Uani 1 1 d . . . . .
H25 H 0.1467 0.3782 1.0487 0.072 Uiso 1 1 calc R U . . .
C26 C 0.4079(3) 0.17544(19) 0.9682(2) 0.0589(9) Uani 1 1 d . . . . .
H26A H 0.4000 0.1205 0.9656 0.071 Uiso 1 1 calc R U . . .
H26B H 0.4761 0.1884 0.9584 0.071 Uiso 1 1 calc R U . . .
C27 C 0.3150(3) 0.2114(2) 0.9022(2) 0.0555(8) Uani 1 1 d . . . . .
C28 C 0.2516(4) 0.1728(3) 0.8313(3) 0.0883(14) Uani 1 1 d . . . . .
H28 H 0.2630 0.1214 0.8236 0.106 Uiso 1 1 calc R U . . .
C29 C 0.1714(4) 0.2130(4) 0.7729(3) 0.1050(17) Uani 1 1 d . . . . .
H29 H 0.1288 0.1887 0.7243 0.126 Uiso 1 1 calc R U . . .
C30 C 0.1534(4) 0.2886(3) 0.7850(3) 0.0883(14) Uani 1 1 d . . . . .
H30 H 0.0990 0.3157 0.7455 0.106 Uiso 1 1 calc R U . . .
C31 C 0.2176(3) 0.3228(2) 0.8570(2) 0.0600(9) Uani 1 1 d . . . . .
H31 H 0.2062 0.3740 0.8659 0.072 Uiso 1 1 calc R U . . .
Cl1 Cl 0.2685(11) 0.5538(8) 0.4603(9) 0.073(2) Uani 0.327(6) 1 d . U P A 1
O1 O 0.1507(10) 0.5864(7) 0.4273(8) 0.117(3) Uani 0.327(6) 1 d . U P A 1
O2 O 0.2984(19) 0.5177(9) 0.3886(11) 0.124(4) Uani 0.327(6) 1 d . U P A 1
O3 O 0.2535(15) 0.4953(8) 0.5054(9) 0.124(4) Uani 0.327(6) 1 d . U P A 1
O4 O 0.3308(11) 0.6140(7) 0.4832(9) 0.102(3) Uani 0.327(6) 1 d . U P A 1
Cl1' Cl 0.2753(6) 0.5459(4) 0.4597(4) 0.0830(14) Uani 0.673(6) 1 d . U P A 2
O1' O 0.2006(6) 0.4926(4) 0.4651(5) 0.130(2) Uani 0.673(6) 1 d . U P A 2
O2' O 0.2744(8) 0.5514(5) 0.3782(5) 0.120(2) Uani 0.673(6) 1 d . U P A 2
O3' O 0.3778(5) 0.5199(3) 0.5215(3) 0.116(2) Uani 0.673(6) 1 d . U P A 2
O4' O 0.2559(8) 0.6189(4) 0.4914(5) 0.136(3) Uani 0.673(6) 1 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
Fe1 C1 1.913(3) . ?
Fe1 C2 1.915(3) . ?
Fe1 C3 1.920(3) . ?
Fe1 N6 1.964(2) . ?
Fe1 N8 1.975(2) . ?
Fe1 N4 1.978(2) . ?
Fe2 N1 2.004(3) . ?
Fe2 N2 2.048(3) 3_667 ?
Fe2 N10 2.069(3) . ?
Fe2 N12 2.088(2) . ?
Fe2 N13 2.089(3) . ?
Fe2 N11 2.101(2) . ?
B1 N7 1.548(4) . ?
B1 N5 1.553(5) . ?
B1 N9 1.557(5) . ?
B1 C13 1.587(5) . ?
N1 C1 1.150(4) . ?
N2 C2 1.146(4) . ?
N2 Fe2 2.048(3) 3_667 ?
N3 C3 1.143(4) . ?
N4 C4 1.330(4) . ?
N4 N5 1.353(3) . ?
N5 C6 1.345(4) . ?
N6 C7 1.335(4) . ?
N6 N7 1.362(3) . ?
N7 C9 1.343(4) . ?
N8 C10 1.336(4) . ?
N8 N9 1.358(3) . ?
N9 C12 1.345(4) . ?
N10 C14 1.334(4) . ?
N10 C18 1.349(4) . ?
N11 C19 1.475(4) . ?
N11 C26 1.476(4) . ?
N11 C20 1.492(4) . ?
N12 C21 1.333(4) . ?
N12 C25 1.347(4) . ?
N13 C27 1.343(4) . ?
N13 C31 1.347(4) . ?
C4 C5 1.379(5) . ?
C4 H4 0.9300 . ?
C5 C6 1.359(5) . ?
C5 H5 0.9300 . ?
C6 H6 0.9300 . ?
C7 C8 1.376(5) . ?
C7 H7 0.9300 . ?
C8 C9 1.364(5) . ?
C8 H8 0.9300 . ?
C9 H9 0.9300 . ?
C10 C11 1.383(5) . ?
C10 H10 0.9300 . ?
C11 C12 1.351(5) . ?
C11 H11 0.9300 . ?
C12 H12 0.9300 . ?
C13 H13A 0.9600 . ?
C13 H13B 0.9600 . ?
C13 H13C 0.9600 . ?
C14 C15 1.407(6) . ?
C14 H14 0.9300 . ?
C15 C16 1.350(8) . ?
C15 H15 0.9300 . ?
C16 C17 1.342(8) . ?
C16 H16 0.9300 . ?
C17 C18 1.377(5) . ?
C17 H17 0.9300 . ?
C18 C19 1.494(5) . ?
C19 H19A 0.9700 . ?
C19 H19B 0.9700 . ?
C20 C21 1.497(4) . ?
C20 H20A 0.9700 . ?
C20 H20B 0.9700 . ?
C21 C22 1.386(4) . ?
C22 C23 1.377(5) . ?
C22 H22 0.9300 . ?
C23 C24 1.366(6) . ?
C23 H23 0.9300 . ?
C24 C25 1.364(5) . ?
C24 H24 0.9300 . ?
C25 H25 0.9300 . ?
C26 C27 1.492(5) . ?
C26 H26A 0.9700 . ?
C26 H26B 0.9700 . ?
C27 C28 1.386(5) . ?
C28 C29 1.375(7) . ?
C28 H28 0.9300 . ?
C29 C30 1.373(7) . ?
C29 H29 0.9300 . ?
C30 C31 1.367(6) . ?
C30 H30 0.9300 . ?
C31 H31 0.9300 . ?
Cl1 O4 1.311(18) . ?
Cl1 O3 1.323(17) . ?
Cl1 O2 1.51(2) . ?
Cl1 O1 1.555(19) . ?
Cl1' O2' 1.360(11) . ?
Cl1' O1' 1.366(9) . ?
Cl1' O4' 1.439(10) . ?
Cl1' O3' 1.473(9) . ?

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
C1 Fe1 C2 91.95(11) . . ?
C1 Fe1 C3 87.51(12) . . ?
C2 Fe1 C3 88.25(12) . . ?
C1 Fe1 N6 177.30(11) . . ?
C2 Fe1 N6 90.47(10) . . ?
C3 Fe1 N6 93.76(12) . . ?
C1 Fe1 N8 91.15(11) . . ?
C2 Fe1 N8 175.48(11) . . ?
C3 Fe1 N8 95.17(11) . . ?
N6 Fe1 N8 86.36(9) . . ?
C1 Fe1 N4 88.96(11) . . ?
C2 Fe1 N4 88.93(10) . . ?
C3 Fe1 N4 175.40(11) . . ?
N6 Fe1 N4 89.90(10) . . ?
N8 Fe1 N4 87.84(10) . . ?
N1 Fe2 N2 89.02(10) . 3_667 ?
N1 Fe2 N10 102.33(11) . . ?
N2 Fe2 N10 88.41(10) 3_667 . ?
N1 Fe2 N12 94.71(10) . . ?
N2 Fe2 N12 175.68(10) 3_667 . ?
N10 Fe2 N12 92.91(10) . . ?
N1 Fe2 N13 98.79(11) . . ?
N2 Fe2 N13 93.60(10) 3_667 . ?
N10 Fe2 N13 158.82(11) . . ?
N12 Fe2 N13 83.69(10) . . ?
N1 Fe2 N11 176.15(10) . . ?
N2 Fe2 N11 94.79(9) 3_667 . ?
N10 Fe2 N11 78.38(10) . . ?
N12 Fe2 N11 81.45(9) . . ?
N13 Fe2 N11 80.44(10) . . ?
N7 B1 N5 106.2(2) . . ?
N7 B1 N9 105.2(3) . . ?
N5 B1 N9 105.6(3) . . ?
N7 B1 C13 113.1(3) . . ?
N5 B1 C13 113.0(3) . . ?
N9 B1 C13 113.1(3) . . ?
C1 N1 Fe2 158.3(3) . . ?
C2 N2 Fe2 154.7(2) . 3_667 ?
C4 N4 N5 107.5(2) . . ?
C4 N4 Fe1 131.9(2) . . ?
N5 N4 Fe1 120.59(18) . . ?
C6 N5 N4 108.4(3) . . ?
C6 N5 B1 132.5(3) . . ?
N4 N5 B1 119.0(2) . . ?
C7 N6 N7 107.1(2) . . ?
C7 N6 Fe1 132.7(2) . . ?
N7 N6 Fe1 120.12(17) . . ?
C9 N7 N6 108.6(3) . . ?
C9 N7 B1 131.8(3) . . ?
N6 N7 B1 119.5(2) . . ?
C10 N8 N9 107.4(2) . . ?
C10 N8 Fe1 133.1(2) . . ?
N9 N8 Fe1 119.46(18) . . ?
C12 N9 N8 107.9(3) . . ?
C12 N9 B1 132.0(3) . . ?
N8 N9 B1 120.1(2) . . ?
C14 N10 C18 118.6(3) . . ?
C14 N10 Fe2 126.8(3) . . ?
C18 N10 Fe2 114.5(2) . . ?
C19 N11 C26 112.6(3) . . ?
C19 N11 C20 109.7(2) . . ?
C26 N11 C20 111.8(3) . . ?
C19 N11 Fe2 106.60(19) . . ?
C26 N11 Fe2 106.51(18) . . ?
C20 N11 Fe2 109.34(17) . . ?
C21 N12 C25 117.8(3) . . ?
C21 N12 Fe2 114.50(19) . . ?
C25 N12 Fe2 126.0(2) . . ?
C27 N13 C31 119.2(3) . . ?
C27 N13 Fe2 113.1(2) . . ?
C31 N13 Fe2 126.2(2) . . ?
N1 C1 Fe1 172.3(3) . . ?
N2 C2 Fe1 171.1(2) . . ?
N3 C3 Fe1 178.1(3) . . ?
N4 C4 C5 109.7(3) . . ?
N4 C4 H4 125.1 . . ?
C5 C4 H4 125.1 . . ?
C6 C5 C4 105.4(3) . . ?
C6 C5 H5 127.3 . . ?
C4 C5 H5 127.3 . . ?
N5 C6 C5 109.0(3) . . ?
N5 C6 H6 125.5 . . ?
C5 C6 H6 125.5 . . ?
N6 C7 C8 109.8(3) . . ?
N6 C7 H7 125.1 . . ?
C8 C7 H7 125.1 . . ?
C9 C8 C7 105.6(3) . . ?
C9 C8 H8 127.2 . . ?
C7 C8 H8 127.2 . . ?
N7 C9 C8 108.9(3) . . ?
N7 C9 H9 125.6 . . ?
C8 C9 H9 125.6 . . ?
N8 C10 C11 109.6(3) . . ?
N8 C10 H10 125.2 . . ?
C11 C10 H10 125.2 . . ?
C12 C11 C10 105.2(3) . . ?
C12 C11 H11 127.4 . . ?
C10 C11 H11 127.4 . . ?
N9 C12 C11 109.9(3) . . ?
N9 C12 H12 125.1 . . ?
C11 C12 H12 125.1 . . ?
B1 C13 H13A 109.5 . . ?
B1 C13 H13B 109.5 . . ?
H13A C13 H13B 109.5 . . ?
B1 C13 H13C 109.5 . . ?
H13A C13 H13C 109.5 . . ?
H13B C13 H13C 109.5 . . ?
N10 C14 C15 120.9(5) . . ?
N10 C14 H14 119.6 . . ?
C15 C14 H14 119.6 . . ?
C16 C15 C14 118.9(5) . . ?
C16 C15 H15 120.6 . . ?
C14 C15 H15 120.6 . . ?
C17 C16 C15 120.6(5) . . ?
C17 C16 H16 119.7 . . ?
C15 C16 H16 119.7 . . ?
C16 C17 C18 119.3(5) . . ?
C16 C17 H17 120.4 . . ?
C18 C17 H17 120.4 . . ?
N10 C18 C17 121.8(4) . . ?
N10 C18 C19 115.2(3) . . ?
C17 C18 C19 122.9(4) . . ?
N11 C19 C18 109.0(3) . . ?
N11 C19 H19A 109.9 . . ?
C18 C19 H19A 109.9 . . ?
N11 C19 H19B 109.9 . . ?
C18 C19 H19B 109.9 . . ?
H19A C19 H19B 108.3 . . ?
N11 C20 C21 112.8(2) . . ?
N11 C20 H20A 109.0 . . ?
C21 C20 H20A 109.0 . . ?
N11 C20 H20B 109.0 . . ?
C21 C20 H20B 109.0 . . ?
H20A C20 H20B 107.8 . . ?
N12 C21 C22 122.4(3) . . ?
N12 C21 C20 115.5(2) . . ?
C22 C21 C20 121.9(3) . . ?
C23 C22 C21 118.4(3) . . ?
C23 C22 H22 120.8 . . ?
C21 C22 H22 120.8 . . ?
C24 C23 C22 119.4(3) . . ?
C24 C23 H23 120.3 . . ?
C22 C23 H23 120.3 . . ?
C25 C24 C23 119.1(4) . . ?
C25 C24 H24 120.4 . . ?
C23 C24 H24 120.4 . . ?
N12 C25 C24 122.7(3) . . ?
N12 C25 H25 118.6 . . ?
C24 C25 H25 118.6 . . ?
N11 C26 C27 109.4(3) . . ?
N11 C26 H26A 109.8 . . ?
C27 C26 H26A 109.8 . . ?
N11 C26 H26B 109.8 . . ?
C27 C26 H26B 109.8 . . ?
H26A C26 H26B 108.2 . . ?
N13 C27 C28 121.5(4) . . ?
N13 C27 C26 115.2(3) . . ?
C28 C27 C26 123.3(4) . . ?
C29 C28 C27 117.9(4) . . ?
C29 C28 H28 121.1 . . ?
C27 C28 H28 121.1 . . ?
C30 C29 C28 121.1(4) . . ?
C30 C29 H29 119.5 . . ?
C28 C29 H29 119.5 . . ?
C31 C30 C29 118.0(4) . . ?
C31 C30 H30 121.0 . . ?
C29 C30 H30 121.0 . . ?
N13 C31 C30 122.3(4) . . ?
N13 C31 H31 118.8 . . ?
C30 C31 H31 118.8 . . ?
O4 Cl1 O3 130.2(15) . . ?
O4 Cl1 O2 106.6(13) . . ?
O3 Cl1 O2 104.1(14) . . ?
O4 Cl1 O1 104.5(12) . . ?
O3 Cl1 O1 100.8(12) . . ?
O2 Cl1 O1 109.7(13) . . ?
O2' Cl1' O1' 109.2(7) . . ?
O2' Cl1' O4' 110.8(6) . . ?
O1' Cl1' O4' 112.3(8) . . ?
O2' Cl1' O3' 116.7(7) . . ?
O1' Cl1' O3' 103.9(6) . . ?
O4' Cl1' O3' 103.8(6) . . ?

loop_
_geom_torsion_atom_site_label_1
_geom_torsion_atom_site_label_2
_geom_torsion_atom_site_label_3
_geom_torsion_atom_site_label_4
_geom_torsion
_geom_torsion_site_symmetry_1
_geom_torsion_site_symmetry_2
_geom_torsion_site_symmetry_3
_geom_torsion_site_symmetry_4
_geom_torsion_publ_flag
C4 N4 N5 C6 -0.9(3) . . . . ?
Fe1 N4 N5 C6 -179.7(2) . . . . ?
C4 N4 N5 B1 177.8(3) . . . . ?
Fe1 N4 N5 B1 -1.0(3) . . . . ?
N7 B1 N5 C6 -125.5(3) . . . . ?
N9 B1 N5 C6 123.1(4) . . . . ?
C13 B1 N5 C6 -1.1(5) . . . . ?
N7 B1 N5 N4 56.2(3) . . . . ?
N9 B1 N5 N4 -55.2(3) . . . . ?
C13 B1 N5 N4 -179.3(3) . . . . ?
C7 N6 N7 C9 0.3(3) . . . . ?
Fe1 N6 N7 C9 -177.8(2) . . . . ?
C7 N6 N7 B1 -175.5(3) . . . . ?
Fe1 N6 N7 B1 6.4(4) . . . . ?
N5 B1 N7 C9 125.7(4) . . . . ?
N9 B1 N7 C9 -122.7(4) . . . . ?
C13 B1 N7 C9 1.2(5) . . . . ?
N5 B1 N7 N6 -59.6(4) . . . . ?
N9 B1 N7 N6 52.0(3) . . . . ?
C13 B1 N7 N6 175.9(3) . . . . ?
C10 N8 N9 C12 0.3(3) . . . . ?
Fe1 N8 N9 C12 179.5(2) . . . . ?
C10 N8 N9 B1 -179.6(3) . . . . ?
Fe1 N8 N9 B1 -0.4(3) . . . . ?
N7 B1 N9 C12 124.5(4) . . . . ?
N5 B1 N9 C12 -123.5(4) . . . . ?
C13 B1 N9 C12 0.6(5) . . . . ?
N7 B1 N9 N8 -55.6(3) . . . . ?
N5 B1 N9 N8 56.4(3) . . . . ?
C13 B1 N9 N8 -179.5(3) . . . . ?
N5 N4 C4 C5 0.4(3) . . . . ?
Fe1 N4 C4 C5 179.1(2) . . . . ?
N4 C4 C5 C6 0.2(4) . . . . ?
N4 N5 C6 C5 1.0(4) . . . . ?
B1 N5 C6 C5 -177.4(3) . . . . ?
C4 C5 C6 N5 -0.7(4) . . . . ?
N7 N6 C7 C8 -0.3(4) . . . . ?
Fe1 N6 C7 C8 177.4(2) . . . . ?
N6 C7 C8 C9 0.2(4) . . . . ?
N6 N7 C9 C8 -0.2(4) . . . . ?
B1 N7 C9 C8 174.9(3) . . . . ?
C7 C8 C9 N7 0.1(4) . . . . ?
N9 N8 C10 C11 -0.4(4) . . . . ?
Fe1 N8 C10 C11 -179.4(2) . . . . ?
N8 C10 C11 C12 0.3(4) . . . . ?
N8 N9 C12 C11 -0.2(4) . . . . ?
B1 N9 C12 C11 179.7(3) . . . . ?
C10 C11 C12 N9 -0.1(4) . . . . ?
C18 N10 C14 C15 0.9(5) . . . . ?
Fe2 N10 C14 C15 -175.2(3) . . . . ?
N10 C14 C15 C16 -0.9(6) . . . . ?
C14 C15 C16 C17 0.0(8) . . . . ?
C15 C16 C17 C18 0.9(8) . . . . ?
C14 N10 C18 C17 0.0(5) . . . . ?
Fe2 N10 C18 C17 176.6(3) . . . . ?
C14 N10 C18 C19 -177.2(3) . . . . ?
Fe2 N10 C18 C19 -0.6(3) . . . . ?
C16 C17 C18 N10 -1.0(6) . . . . ?
C16 C17 C18 C19 176.1(4) . . . . ?
C26 N11 C19 C18 158.8(3) . . . . ?
C20 N11 C19 C18 -75.9(3) . . . . ?
Fe2 N11 C19 C18 42.4(3) . . . . ?
N10 C18 C19 N11 -28.6(4) . . . . ?
C17 C18 C19 N11 154.2(3) . . . . ?
C19 N11 C20 C21 139.3(3) . . . . ?
C26 N11 C20 C21 -94.9(3) . . . . ?
Fe2 N11 C20 C21 22.8(3) . . . . ?
C25 N12 C21 C22 2.5(4) . . . . ?
Fe2 N12 C21 C22 -163.8(2) . . . . ?
C25 N12 C21 C20 -173.3(3) . . . . ?
Fe2 N12 C21 C20 20.4(3) . . . . ?
N11 C20 C21 N12 -29.3(4) . . . . ?
N11 C20 C21 C22 154.9(3) . . . . ?
N12 C21 C22 C23 -1.7(5) . . . . ?
C20 C21 C22 C23 173.8(3) . . . . ?
C21 C22 C23 C24 -0.6(6) . . . . ?
C22 C23 C24 C25 2.0(6) . . . . ?
C21 N12 C25 C24 -1.0(5) . . . . ?
Fe2 N12 C25 C24 163.5(3) . . . . ?
C23 C24 C25 N12 -1.2(6) . . . . ?
C19 N11 C26 C27 -157.6(3) . . . . ?
C20 N11 C26 C27 78.2(3) . . . . ?
Fe2 N11 C26 C27 -41.1(3) . . . . ?
C31 N13 C27 C28 -2.2(5) . . . . ?
Fe2 N13 C27 C28 164.7(3) . . . . ?
C31 N13 C27 C26 177.1(3) . . . . ?
Fe2 N13 C27 C26 -16.0(4) . . . . ?
N11 C26 C27 N13 39.3(4) . . . . ?
N11 C26 C27 C28 -141.5(4) . . . . ?
N13 C27 C28 C29 2.2(7) . . . . ?
C26 C27 C28 C29 -177.0(4) . . . . ?
C27 C28 C29 C30 -1.2(8) . . . . ?
C28 C29 C30 C31 0.1(8) . . . . ?
C27 N13 C31 C30 1.1(5) . . . . ?
Fe2 N13 C31 C30 -164.0(3) . . . . ?
C29 C30 C31 N13 0.0(7) . . . . ?

_refine_diff_density_max         0.667
_refine_diff_density_min         -0.242
_refine_diff_density_rms         0.059

####################################################################### 
# 
# 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_3-370K
_database_code_depnum_ccdc_archive 'CCDC 1419289'
_audit_update_record             
;
2016-09-02 deposited with the CCDC.
2016-09-26 downloaded from the CCDC.
;

_audit_creation_method           SHELXL-2014/7
_shelx_SHELXL_version_number     2014/7
_chemical_name_systematic        ?
_chemical_name_common            ?
_chemical_melting_point          ?
_chemical_formula_moiety         'C62 H60 B2 Fe4 N26, 2(Cl O4) '
_chemical_formula_sum            'C62 H60 B2 Cl2 Fe4 N26 O8'
_chemical_formula_weight         1613.28

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'
O O 0.0106 0.0060 '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'

_space_group_crystal_system      monoclinic
_space_group_IT_number           14
_space_group_name_H-M_alt        'P 21/c'
_space_group_name_Hall           '-P 2ybc'

_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.
;

loop_
_space_group_symop_operation_xyz
'x, y, z'
'-x, y+1/2, -z+1/2'
'-x, -y, -z'
'x, -y-1/2, z-1/2'

_cell_length_a                   12.962(2)
_cell_length_b                   17.700(3)
_cell_length_c                   16.746(3)
_cell_angle_alpha                90
_cell_angle_beta                 107.707(3)
_cell_angle_gamma                90
_cell_volume                     3660.0(9)
_cell_formula_units_Z            2
_cell_measurement_temperature    370(2)
_cell_measurement_reflns_used    2497
_cell_measurement_theta_min      2.30
_cell_measurement_theta_max      21.80

_exptl_crystal_description       block
_exptl_crystal_colour            red
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    'not measured'
_exptl_crystal_density_diffrn    1.464
_exptl_crystal_F_000             1652
_exptl_transmission_factor_min   ?
_exptl_transmission_factor_max   ?
_exptl_crystal_size_max          0.100
_exptl_crystal_size_mid          0.050
_exptl_crystal_size_min          0.050
_exptl_absorpt_coefficient_mu    0.921
_shelx_estimated_absorpt_T_min   0.914
_shelx_estimated_absorpt_T_max   0.955
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_correction_T_min  0.9136
_exptl_absorpt_correction_T_max  0.9554
_exptl_absorpt_process_details   sadabs
_exptl_absorpt_special_details   ?
_diffrn_ambient_temperature      370(2)
_diffrn_radiation_wavelength     0.71073
_diffrn_radiation_type           MoK\a
_diffrn_source                   ?
_diffrn_measurement_device_type  'Bruker APEX-II CCD'
_diffrn_measurement_method       'φ and ω scans'
_diffrn_detector_area_resol_mean ?
_diffrn_reflns_number            19989
_diffrn_reflns_av_unetI/netI     0.0857
_diffrn_reflns_av_R_equivalents  0.0724
_diffrn_reflns_limit_h_min       -15
_diffrn_reflns_limit_h_max       13
_diffrn_reflns_limit_k_min       -21
_diffrn_reflns_limit_k_max       20
_diffrn_reflns_limit_l_min       -10
_diffrn_reflns_limit_l_max       19
_diffrn_reflns_theta_min         1.718
_diffrn_reflns_theta_max         25.000
_diffrn_reflns_theta_full        25.000
_diffrn_measured_fraction_theta_max 0.999
_diffrn_measured_fraction_theta_full 0.999
_diffrn_reflns_Laue_measured_fraction_max 0.999
_diffrn_reflns_Laue_measured_fraction_full 0.999
_diffrn_reflns_point_group_measured_fraction_max 0.999
_diffrn_reflns_point_group_measured_fraction_full 0.999
_reflns_number_total             6427
_reflns_number_gt                3477
_reflns_threshold_expression     'I > 2σ(I)'
_reflns_Friedel_coverage         0.000
_reflns_Friedel_fraction_max     .
_reflns_Friedel_fraction_full    .

_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.
;

_computing_data_collection       'Bruker APEX2'
_computing_cell_refinement       'Bruker SAINT'
_computing_data_reduction        'Bruker SAINT'
_computing_structure_solution    'SHELXS-2014 (Sheldrick, 2014)'
_computing_structure_refinement  'SHELXL-2014/7 (Sheldrick, 2014)'
_computing_molecular_graphics    'Bruker SHELXTL'
_computing_publication_material  'Bruker SHELXTL'
_refine_special_details          ?
_refine_ls_structure_factor_coef Fsqd
_refine_ls_matrix_type           full
_refine_ls_weighting_scheme      calc
_refine_ls_weighting_details     
'w=1/[σ²(Fo²)+(0.0429P)²] where P=(Fo²+2Fc²)/3'
_atom_sites_solution_primary     ?
_atom_sites_solution_secondary   ?
_atom_sites_solution_hydrogens   geom
_refine_ls_hydrogen_treatment    constr
_refine_ls_extinction_method     none
_refine_ls_extinction_coef       .
_refine_ls_number_reflns         6427
_refine_ls_number_parameters     516
_refine_ls_number_restraints     184
_refine_ls_R_factor_all          0.1144
_refine_ls_R_factor_gt           0.0471
_refine_ls_wR_factor_ref         0.1103
_refine_ls_wR_factor_gt          0.0878
_refine_ls_goodness_of_fit_ref   0.974
_refine_ls_restrained_S_all      1.005
_refine_ls_shift/su_max          0.010
_refine_ls_shift/su_mean         0.000

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 0.25641(5) 0.57616(3) 0.92589(4) 0.04484(18) Uani 1 1 d . . . . .
Fe2 Fe 0.37642(5) 0.32092(3) 1.03931(4) 0.0489(2) Uani 1 1 d . . . . .
B1 B 0.1316(4) 0.5729(3) 0.7336(3) 0.0613(15) Uani 1 1 d . . . . .
N1 N 0.3298(3) 0.4330(2) 1.0291(2) 0.0641(11) Uani 1 1 d . . . . .
N2 N 0.4800(3) 0.65009(18) 0.9873(2) 0.0591(10) Uani 1 1 d . . . . .
N3 N 0.1997(4) 0.6442(2) 1.0749(3) 0.0840(14) Uani 1 1 d . . . . .
N4 N 0.3047(3) 0.52879(17) 0.8373(2) 0.0501(9) Uani 1 1 d . . . . .
N5 N 0.2426(3) 0.53266(19) 0.7553(2) 0.0588(10) Uani 1 1 d . . . . .
N6 N 0.2039(3) 0.66427(17) 0.8533(2) 0.0487(9) Uani 1 1 d . . . . .
N7 N 0.1541(3) 0.65418(19) 0.7695(2) 0.0573(10) Uani 1 1 d . . . . .
N8 N 0.1128(3) 0.53095(17) 0.8725(2) 0.0526(9) Uani 1 1 d . . . . .
N9 N 0.0690(3) 0.53335(19) 0.7879(2) 0.0610(10) Uani 1 1 d . . . . .
N10 N 0.4697(3) 0.3072(2) 1.1680(2) 0.0594(10) Uani 1 1 d . . . . .
N11 N 0.4091(3) 0.19993(17) 1.0526(2) 0.0536(10) Uani 1 1 d . . . . .
N12 N 0.2289(3) 0.28073(18) 1.0602(2) 0.0556(10) Uani 1 1 d . . . . .
N13 N 0.2975(3) 0.2819(2) 0.9133(2) 0.0627(10) Uani 1 1 d . . . . .
C1 C 0.3037(3) 0.4889(2) 0.9945(3) 0.0487(11) Uani 1 1 d . . . . .
C2 C 0.3963(4) 0.6224(2) 0.9698(3) 0.0473(11) Uani 1 1 d . . . . .
C3 C 0.2180(4) 0.6191(2) 1.0181(3) 0.0555(12) Uani 1 1 d . . . . .
C4 C 0.3933(4) 0.4900(2) 0.8388(3) 0.0632(13) Uani 1 1 d . . . . .
H4 H 0.4497 0.4791 0.8870 0.076 Uiso 1 1 calc R U . . .
C5 C 0.3896(5) 0.4686(3) 0.7596(4) 0.0833(16) Uani 1 1 d . . . . .
H5 H 0.4411 0.4407 0.7440 0.100 Uiso 1 1 calc R U . . .
C6 C 0.2951(5) 0.4964(3) 0.7084(3) 0.0808(16) Uani 1 1 d . . . . .
H6 H 0.2704 0.4912 0.6504 0.097 Uiso 1 1 calc R U . . .
C7 C 0.2080(3) 0.7381(2) 0.8681(3) 0.0582(12) Uani 1 1 d . . . . .
H7 H 0.2377 0.7607 0.9201 0.070 Uiso 1 1 calc R U . . .
C8 C 0.1612(4) 0.7757(3) 0.7936(4) 0.0813(17) Uani 1 1 d . . . . .
H8 H 0.1533 0.8277 0.7860 0.098 Uiso 1 1 calc R U . . .
C9 C 0.1289(4) 0.7218(3) 0.7338(3) 0.0770(16) Uani 1 1 d . . . . .
H9 H 0.0948 0.7305 0.6771 0.092 Uiso 1 1 calc R U . . .
C10 C 0.0439(4) 0.4944(2) 0.9027(3) 0.0675(13) Uani 1 1 d . . . . .
H10 H 0.0546 0.4844 0.9592 0.081 Uiso 1 1 calc R U . . .
C11 C -0.0470(4) 0.4731(3) 0.8379(4) 0.0898(18) Uani 1 1 d . . . . .
H11 H -0.1073 0.4468 0.8420 0.108 Uiso 1 1 calc R U . . .
C12 C -0.0285(4) 0.4991(3) 0.7669(4) 0.0808(16) Uani 1 1 d . . . . .
H12 H -0.0755 0.4941 0.7128 0.097 Uiso 1 1 calc R U . . .
C13 C 0.0680(4) 0.5707(3) 0.6362(3) 0.0931(18) Uani 1 1 d . . . . .
H13A H -0.0007 0.5956 0.6261 0.140 Uiso 1 1 calc R U . . .
H13B H 0.0565 0.5192 0.6178 0.140 Uiso 1 1 calc R U . . .
H13C H 0.1097 0.5962 0.6058 0.140 Uiso 1 1 calc R U . . .
C14 C 0.4794(4) 0.3577(3) 1.2298(3) 0.0821(16) Uani 1 1 d . . . . .
H14 H 0.4389 0.4020 1.2179 0.098 Uiso 1 1 calc R U . . .
C15 C 0.5474(6) 0.3463(4) 1.3104(4) 0.102(2) Uani 1 1 d . . . . .
H15 H 0.5533 0.3825 1.3519 0.122 Uiso 1 1 calc R U . . .
C16 C 0.6051(6) 0.2812(5) 1.3275(5) 0.119(3) Uani 1 1 d . . . . .
H16 H 0.6516 0.2724 1.3811 0.143 Uiso 1 1 calc R U . . .
C17 C 0.5949(4) 0.2292(4) 1.2664(4) 0.0969(19) Uani 1 1 d . . . . .
H17 H 0.6336 0.1842 1.2780 0.116 Uiso 1 1 calc R U . . .
C18 C 0.5268(4) 0.2435(3) 1.1867(3) 0.0641(13) Uani 1 1 d . . . . .
C19 C 0.5169(4) 0.1920(3) 1.1145(3) 0.0717(15) Uani 1 1 d . . . . .
H19A H 0.5722 0.2042 1.0884 0.086 Uiso 1 1 calc R U . . .
H19B H 0.5277 0.1402 1.1340 0.086 Uiso 1 1 calc R U . . .
C20 C 0.3257(4) 0.1627(2) 1.0822(3) 0.0681(14) Uani 1 1 d . . . . .
H20A H 0.3542 0.1552 1.1423 0.082 Uiso 1 1 calc R U . . .
H20B H 0.3104 0.1133 1.0562 0.082 Uiso 1 1 calc R U . . .
C21 C 0.2220(4) 0.2061(3) 1.0636(3) 0.0550(12) Uani 1 1 d . . . . .
C22 C 0.1248(4) 0.1696(3) 1.0546(3) 0.0777(15) Uani 1 1 d . . . . .
H22 H 0.1216 0.1172 1.0553 0.093 Uiso 1 1 calc R U . . .
C23 C 0.0342(5) 0.2115(4) 1.0449(3) 0.101(2) Uani 1 1 d . . . . .
H23 H -0.0321 0.1880 1.0382 0.122 Uiso 1 1 calc R U . . .
C24 C 0.0413(5) 0.2893(4) 1.0448(4) 0.103(2) Uani 1 1 d . . . . .
H24 H -0.0192 0.3192 1.0404 0.123 Uiso 1 1 calc R U . . .
C25 C 0.1391(5) 0.3212(3) 1.0515(3) 0.0820(16) Uani 1 1 d . . . . .
H25 H 0.1437 0.3736 1.0501 0.098 Uiso 1 1 calc R U . . .
C26 C 0.4058(4) 0.1730(3) 0.9687(3) 0.0770(15) Uani 1 1 d . . . . .
H26A H 0.3977 0.1185 0.9664 0.092 Uiso 1 1 calc R U . . .
H26B H 0.4735 0.1853 0.9584 0.092 Uiso 1 1 calc R U . . .
C27 C 0.3143(4) 0.2080(3) 0.9023(3) 0.0718(14) Uani 1 1 d . . . . .
C28 C 0.2508(5) 0.1686(4) 0.8334(4) 0.105(2) Uani 1 1 d . . . . .
H28 H 0.2624 0.1174 0.8270 0.126 Uiso 1 1 calc R U . . .
C29 C 0.1700(6) 0.2069(5) 0.7745(4) 0.128(3) Uani 1 1 d . . . . .
H29 H 0.1261 0.1817 0.7278 0.154 Uiso 1 1 calc R U . . .
C30 C 0.1547(5) 0.2830(5) 0.7853(4) 0.116(2) Uani 1 1 d . . . . .
H30 H 0.1015 0.3098 0.7455 0.140 Uiso 1 1 calc R U . . .
C31 C 0.2189(4) 0.3180(3) 0.8555(3) 0.0851(17) Uani 1 1 d . . . . .
H31 H 0.2075 0.3690 0.8634 0.102 Uiso 1 1 calc R U . . .
Cl1 Cl 0.2747(4) 0.9505(3) 0.9625(3) 0.0880(12) Uani 0.690(5) 1 d D U P A 1
O1 O 0.3733(6) 0.9765(4) 1.0189(4) 0.145(3) Uani 0.690(5) 1 d D U P A 1
O2 O 0.2669(8) 0.9518(6) 0.8755(4) 0.149(3) Uani 0.690(5) 1 d D U P A 1
O3 O 0.1993(6) 1.0052(4) 0.9663(6) 0.159(3) Uani 0.690(5) 1 d D U P A 1
O4 O 0.2611(8) 0.8776(4) 0.9905(6) 0.158(3) Uani 0.690(5) 1 d D U P A 1
Cl1' Cl 0.2587(11) 0.9442(9) 0.9511(10) 0.118(3) Uani 0.310(5) 1 d D U P A 2
O1' O 0.1519(12) 0.9156(8) 0.9261(10) 0.138(4) Uani 0.310(5) 1 d D U P A 2
O2' O 0.3237(16) 0.9677(13) 0.9012(13) 0.141(4) Uani 0.310(5) 1 d D U P A 2
O3' O 0.2652(18) 1.0014(10) 1.0098(11) 0.139(4) Uani 0.310(5) 1 d D U P A 2
O4' O 0.3350(14) 0.8885(10) 0.9868(13) 0.137(4) Uani 0.310(5) 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
Fe1 C1 1.912(4) . ?
Fe1 C3 1.917(5) . ?
Fe1 C2 1.921(4) . ?
Fe1 N4 1.964(4) . ?
Fe1 N6 1.967(3) . ?
Fe1 N8 1.973(3) . ?
Fe2 N1 2.065(4) . ?
Fe2 N2 2.104(4) 3_667 ?
Fe2 N10 2.141(4) . ?
Fe2 N13 2.160(4) . ?
Fe2 N12 2.166(4) . ?
Fe2 N11 2.181(3) . ?
B1 N5 1.547(6) . ?
B1 N7 1.552(6) . ?
B1 N9 1.558(7) . ?
B1 C13 1.589(6) . ?
N1 C1 1.144(4) . ?
N2 C2 1.144(5) . ?
N2 Fe2 2.104(4) 3_667 ?
N3 C3 1.138(5) . ?
N4 C4 1.331(5) . ?
N4 N5 1.367(4) . ?
N5 C6 1.347(6) . ?
N6 C7 1.327(4) . ?
N6 N7 1.366(4) . ?
N7 C9 1.334(5) . ?
N8 C10 1.322(5) . ?
N8 N9 1.357(4) . ?
N9 C12 1.347(6) . ?
N10 C18 1.333(5) . ?
N10 C14 1.344(6) . ?
N11 C19 1.471(5) . ?
N11 C26 1.472(6) . ?
N11 C20 1.475(5) . ?
N12 C21 1.326(5) . ?
N12 C25 1.337(6) . ?
N13 C31 1.335(5) . ?
N13 C27 1.347(6) . ?
C4 C5 1.367(6) . ?
C4 H4 0.9300 . ?
C5 C6 1.356(6) . ?
C5 H5 0.9300 . ?
C6 H6 0.9300 . ?
C7 C8 1.382(6) . ?
C7 H7 0.9300 . ?
C8 C9 1.354(6) . ?
C8 H8 0.9300 . ?
C9 H9 0.9300 . ?
C10 C11 1.389(6) . ?
C10 H10 0.9300 . ?
C11 C12 1.363(7) . ?
C11 H11 0.9300 . ?
C12 H12 0.9300 . ?
C13 H13A 0.9600 . ?
C13 H13B 0.9600 . ?
C13 H13C 0.9600 . ?
C14 C15 1.385(7) . ?
C14 H14 0.9300 . ?
C15 C16 1.356(8) . ?
C15 H15 0.9300 . ?
C16 C17 1.352(8) . ?
C16 H16 0.9300 . ?
C17 C18 1.381(6) . ?
C17 H17 0.9300 . ?
C18 C19 1.488(6) . ?
C19 H19A 0.9700 . ?
C19 H19B 0.9700 . ?
C20 C21 1.496(6) . ?
C20 H20A 0.9700 . ?
C20 H20B 0.9700 . ?
C21 C22 1.383(6) . ?
C22 C23 1.355(7) . ?
C22 H22 0.9300 . ?
C23 C24 1.381(8) . ?
C23 H23 0.9300 . ?
C24 C25 1.360(7) . ?
C24 H24 0.9300 . ?
C25 H25 0.9300 . ?
C26 C27 1.492(6) . ?
C26 H26A 0.9700 . ?
C26 H26B 0.9700 . ?
C27 C28 1.385(7) . ?
C28 C29 1.378(8) . ?
C28 H28 0.9300 . ?
C29 C30 1.381(8) . ?
C29 H29 0.9300 . ?
C30 C31 1.366(7) . ?
C30 H30 0.9300 . ?
C31 H31 0.9300 . ?
Cl1 O3 1.391(6) . ?
Cl1 O4 1.402(7) . ?
Cl1 O1 1.416(6) . ?
Cl1 O2 1.429(7) . ?
Cl1' O3' 1.396(9) . ?
Cl1' O4' 1.396(9) . ?
Cl1' O1' 1.413(9) . ?
Cl1' O2' 1.417(10) . ?

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
C1 Fe1 C3 87.18(18) . . ?
C1 Fe1 C2 91.24(16) . . ?
C3 Fe1 C2 88.21(18) . . ?
C1 Fe1 N4 89.48(16) . . ?
C3 Fe1 N4 175.88(16) . . ?
C2 Fe1 N4 89.44(16) . . ?
C1 Fe1 N6 178.27(15) . . ?
C3 Fe1 N6 93.30(16) . . ?
C2 Fe1 N6 90.43(14) . . ?
N4 Fe1 N6 90.10(14) . . ?
C1 Fe1 N8 91.74(15) . . ?
C3 Fe1 N8 94.91(17) . . ?
C2 Fe1 N8 175.79(17) . . ?
N4 Fe1 N8 87.61(15) . . ?
N6 Fe1 N8 86.57(13) . . ?
N1 Fe2 N2 90.19(14) . 3_667 ?
N1 Fe2 N10 104.72(15) . . ?
N2 Fe2 N10 88.59(14) 3_667 . ?
N1 Fe2 N13 100.75(15) . . ?
N2 Fe2 N13 93.31(14) 3_667 . ?
N10 Fe2 N13 154.45(15) . . ?
N1 Fe2 N12 94.52(14) . . ?
N2 Fe2 N12 174.35(13) 3_667 . ?
N10 Fe2 N12 93.23(13) . . ?
N13 Fe2 N12 82.75(14) . . ?
N1 Fe2 N11 173.82(15) . . ?
N2 Fe2 N11 95.98(13) 3_667 . ?
N10 Fe2 N11 75.68(14) . . ?
N13 Fe2 N11 78.79(14) . . ?
N12 Fe2 N11 79.31(13) . . ?
N5 B1 N7 106.5(4) . . ?
N5 B1 N9 105.6(4) . . ?
N7 B1 N9 105.1(4) . . ?
N5 B1 C13 112.7(4) . . ?
N7 B1 C13 113.5(4) . . ?
N9 B1 C13 112.9(4) . . ?
C1 N1 Fe2 155.0(4) . . ?
C2 N2 Fe2 151.8(4) . 3_667 ?
C4 N4 N5 106.6(4) . . ?
C4 N4 Fe1 132.6(3) . . ?
N5 N4 Fe1 120.8(3) . . ?
C6 N5 N4 108.3(4) . . ?
C6 N5 B1 132.9(4) . . ?
N4 N5 B1 118.7(4) . . ?
C7 N6 N7 107.4(3) . . ?
C7 N6 Fe1 132.7(3) . . ?
N7 N6 Fe1 119.8(2) . . ?
C9 N7 N6 108.6(4) . . ?
C9 N7 B1 131.8(4) . . ?
N6 N7 B1 119.6(3) . . ?
C10 N8 N9 107.3(3) . . ?
C10 N8 Fe1 132.8(3) . . ?
N9 N8 Fe1 119.9(3) . . ?
C12 N9 N8 108.7(4) . . ?
C12 N9 B1 131.6(4) . . ?
N8 N9 B1 119.8(3) . . ?
C18 N10 C14 117.9(4) . . ?
C18 N10 Fe2 115.8(3) . . ?
C14 N10 Fe2 126.2(3) . . ?
C19 N11 C26 112.8(4) . . ?
C19 N11 C20 111.0(4) . . ?
C26 N11 C20 111.4(4) . . ?
C19 N11 Fe2 106.2(2) . . ?
C26 N11 Fe2 105.8(3) . . ?
C20 N11 Fe2 109.5(3) . . ?
C21 N12 C25 118.1(4) . . ?
C21 N12 Fe2 114.1(3) . . ?
C25 N12 Fe2 126.1(3) . . ?
C31 N13 C27 119.0(4) . . ?
C31 N13 Fe2 125.8(4) . . ?
C27 N13 Fe2 113.3(3) . . ?
N1 C1 Fe1 173.9(4) . . ?
N2 C2 Fe1 172.6(4) . . ?
N3 C3 Fe1 177.1(4) . . ?
N4 C4 C5 110.5(4) . . ?
N4 C4 H4 124.8 . . ?
C5 C4 H4 124.8 . . ?
C6 C5 C4 105.7(5) . . ?
C6 C5 H5 127.2 . . ?
C4 C5 H5 127.2 . . ?
N5 C6 C5 108.9(5) . . ?
N5 C6 H6 125.5 . . ?
C5 C6 H6 125.5 . . ?
N6 C7 C8 109.0(4) . . ?
N6 C7 H7 125.5 . . ?
C8 C7 H7 125.5 . . ?
C9 C8 C7 106.2(4) . . ?
C9 C8 H8 126.9 . . ?
C7 C8 H8 126.9 . . ?
N7 C9 C8 108.8(4) . . ?
N7 C9 H9 125.6 . . ?
C8 C9 H9 125.6 . . ?
N8 C10 C11 110.2(5) . . ?
N8 C10 H10 124.9 . . ?
C11 C10 H10 124.9 . . ?
C12 C11 C10 105.0(5) . . ?
C12 C11 H11 127.5 . . ?
C10 C11 H11 127.5 . . ?
N9 C12 C11 108.9(5) . . ?
N9 C12 H12 125.6 . . ?
C11 C12 H12 125.6 . . ?
B1 C13 H13A 109.5 . . ?
B1 C13 H13B 109.5 . . ?
H13A C13 H13B 109.5 . . ?
B1 C13 H13C 109.5 . . ?
H13A C13 H13C 109.5 . . ?
H13B C13 H13C 109.5 . . ?
N10 C14 C15 122.4(5) . . ?
N10 C14 H14 118.8 . . ?
C15 C14 H14 118.8 . . ?
C16 C15 C14 118.4(6) . . ?
C16 C15 H15 120.8 . . ?
C14 C15 H15 120.8 . . ?
C17 C16 C15 119.9(7) . . ?
C17 C16 H16 120.1 . . ?
C15 C16 H16 120.1 . . ?
C16 C17 C18 119.5(6) . . ?
C16 C17 H17 120.2 . . ?
C18 C17 H17 120.2 . . ?
N10 C18 C17 121.8(5) . . ?
N10 C18 C19 115.0(4) . . ?
C17 C18 C19 123.0(5) . . ?
N11 C19 C18 110.0(4) . . ?
N11 C19 H19A 109.7 . . ?
C18 C19 H19A 109.7 . . ?
N11 C19 H19B 109.7 . . ?
C18 C19 H19B 109.7 . . ?
H19A C19 H19B 108.2 . . ?
N11 C20 C21 113.8(4) . . ?
N11 C20 H20A 108.8 . . ?
C21 C20 H20A 108.8 . . ?
N11 C20 H20B 108.8 . . ?
C21 C20 H20B 108.8 . . ?
H20A C20 H20B 107.7 . . ?
N12 C21 C22 122.1(4) . . ?
N12 C21 C20 116.9(4) . . ?
C22 C21 C20 120.9(4) . . ?
C23 C22 C21 119.1(5) . . ?
C23 C22 H22 120.5 . . ?
C21 C22 H22 120.5 . . ?
C22 C23 C24 119.3(6) . . ?
C22 C23 H23 120.3 . . ?
C24 C23 H23 120.3 . . ?
C25 C24 C23 118.3(6) . . ?
C25 C24 H24 120.8 . . ?
C23 C24 H24 120.8 . . ?
N12 C25 C24 123.1(5) . . ?
N12 C25 H25 118.5 . . ?
C24 C25 H25 118.5 . . ?
N11 C26 C27 111.3(4) . . ?
N11 C26 H26A 109.4 . . ?
C27 C26 H26A 109.4 . . ?
N11 C26 H26B 109.4 . . ?
C27 C26 H26B 109.4 . . ?
H26A C26 H26B 108.0 . . ?
N13 C27 C28 121.5(5) . . ?
N13 C27 C26 115.2(4) . . ?
C28 C27 C26 123.2(5) . . ?
C29 C28 C27 118.5(6) . . ?
C29 C28 H28 120.7 . . ?
C27 C28 H28 120.7 . . ?
C28 C29 C30 119.6(6) . . ?
C28 C29 H29 120.2 . . ?
C30 C29 H29 120.2 . . ?
C31 C30 C29 118.8(6) . . ?
C31 C30 H30 120.6 . . ?
C29 C30 H30 120.6 . . ?
N13 C31 C30 122.5(6) . . ?
N13 C31 H31 118.8 . . ?
C30 C31 H31 118.8 . . ?
O3 Cl1 O4 117.6(7) . . ?
O3 Cl1 O1 104.3(5) . . ?
O4 Cl1 O1 104.8(6) . . ?
O3 Cl1 O2 101.7(7) . . ?
O4 Cl1 O2 112.3(7) . . ?
O1 Cl1 O2 116.4(6) . . ?
O3' Cl1' O4' 109.2(17) . . ?
O3' Cl1' O1' 108.2(15) . . ?
O4' Cl1' O1' 112.1(15) . . ?
O3' Cl1' O2' 106.5(17) . . ?
O4' Cl1' O2' 89.3(16) . . ?
O1' Cl1' O2' 129.4(16) . . ?

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
C4 N4 N5 C6 -0.3(5) . . . . ?
Fe1 N4 N5 C6 179.5(3) . . . . ?
C4 N4 N5 B1 178.3(4) . . . . ?
Fe1 N4 N5 B1 -2.0(5) . . . . ?
N7 B1 N5 C6 -125.3(5) . . . . ?
N9 B1 N5 C6 123.3(5) . . . . ?
C13 B1 N5 C6 -0.3(7) . . . . ?
N7 B1 N5 N4 56.6(5) . . . . ?
N9 B1 N5 N4 -54.8(5) . . . . ?
C13 B1 N5 N4 -178.4(4) . . . . ?
C7 N6 N7 C9 0.4(5) . . . . ?
Fe1 N6 N7 C9 -178.3(3) . . . . ?
C7 N6 N7 B1 -176.7(4) . . . . ?
Fe1 N6 N7 B1 4.7(5) . . . . ?
N5 B1 N7 C9 125.3(5) . . . . ?
N9 B1 N7 C9 -123.0(5) . . . . ?
C13 B1 N7 C9 0.8(8) . . . . ?
N5 B1 N7 N6 -58.5(5) . . . . ?
N9 B1 N7 N6 53.3(5) . . . . ?
C13 B1 N7 N6 177.0(4) . . . . ?
C10 N8 N9 C12 1.2(5) . . . . ?
Fe1 N8 N9 C12 -179.9(3) . . . . ?
C10 N8 N9 B1 -179.8(4) . . . . ?
Fe1 N8 N9 B1 -0.9(5) . . . . ?
N5 B1 N9 C12 -124.4(5) . . . . ?
N7 B1 N9 C12 123.2(5) . . . . ?
C13 B1 N9 C12 -0.9(7) . . . . ?
N5 B1 N9 N8 56.8(5) . . . . ?
N7 B1 N9 N8 -55.5(5) . . . . ?
C13 B1 N9 N8 -179.7(4) . . . . ?
N5 N4 C4 C5 -0.2(5) . . . . ?
Fe1 N4 C4 C5 -179.9(3) . . . . ?
N4 C4 C5 C6 0.6(6) . . . . ?
N4 N5 C6 C5 0.6(6) . . . . ?
B1 N5 C6 C5 -177.7(5) . . . . ?
C4 C5 C6 N5 -0.7(6) . . . . ?
N7 N6 C7 C8 -0.2(5) . . . . ?
Fe1 N6 C7 C8 178.2(3) . . . . ?
N6 C7 C8 C9 0.0(6) . . . . ?
N6 N7 C9 C8 -0.4(6) . . . . ?
B1 N7 C9 C8 176.2(5) . . . . ?
C7 C8 C9 N7 0.3(6) . . . . ?
N9 N8 C10 C11 -0.7(5) . . . . ?
Fe1 N8 C10 C11 -179.4(3) . . . . ?
N8 C10 C11 C12 0.0(6) . . . . ?
N8 N9 C12 C11 -1.2(6) . . . . ?
B1 N9 C12 C11 179.9(5) . . . . ?
C10 C11 C12 N9 0.8(6) . . . . ?
C18 N10 C14 C15 1.3(7) . . . . ?
Fe2 N10 C14 C15 -175.6(4) . . . . ?
N10 C14 C15 C16 -0.8(9) . . . . ?
C14 C15 C16 C17 -0.3(10) . . . . ?
C15 C16 C17 C18 0.9(10) . . . . ?
C14 N10 C18 C17 -0.7(7) . . . . ?
Fe2 N10 C18 C17 176.5(4) . . . . ?
C14 N10 C18 C19 -176.8(4) . . . . ?
Fe2 N10 C18 C19 0.4(5) . . . . ?
C16 C17 C18 N10 -0.4(8) . . . . ?
C16 C17 C18 C19 175.4(6) . . . . ?
C26 N11 C19 C18 159.6(4) . . . . ?
C20 N11 C19 C18 -74.7(4) . . . . ?
Fe2 N11 C19 C18 44.2(4) . . . . ?
N10 C18 C19 N11 -30.9(6) . . . . ?
C17 C18 C19 N11 153.1(4) . . . . ?
C19 N11 C20 C21 139.7(4) . . . . ?
C26 N11 C20 C21 -93.8(4) . . . . ?
Fe2 N11 C20 C21 22.8(4) . . . . ?
C25 N12 C21 C22 3.1(7) . . . . ?
Fe2 N12 C21 C22 -162.9(4) . . . . ?
C25 N12 C21 C20 -173.8(4) . . . . ?
Fe2 N12 C21 C20 20.3(5) . . . . ?
N11 C20 C21 N12 -29.7(6) . . . . ?
N11 C20 C21 C22 153.4(4) . . . . ?
N12 C21 C22 C23 -2.3(7) . . . . ?
C20 C21 C22 C23 174.5(5) . . . . ?
C21 C22 C23 C24 -0.6(8) . . . . ?
C22 C23 C24 C25 2.5(9) . . . . ?
C21 N12 C25 C24 -1.1(7) . . . . ?
Fe2 N12 C25 C24 163.0(4) . . . . ?
C23 C24 C25 N12 -1.7(9) . . . . ?
C19 N11 C26 C27 -157.4(4) . . . . ?
C20 N11 C26 C27 77.1(5) . . . . ?
Fe2 N11 C26 C27 -41.8(4) . . . . ?
C31 N13 C27 C28 -1.1(8) . . . . ?
Fe2 N13 C27 C28 164.2(4) . . . . ?
C31 N13 C27 C26 178.3(5) . . . . ?
Fe2 N13 C27 C26 -16.4(6) . . . . ?
N11 C26 C27 N13 40.6(6) . . . . ?
N11 C26 C27 C28 -140.0(5) . . . . ?
N13 C27 C28 C29 1.1(9) . . . . ?
C26 C27 C28 C29 -178.3(6) . . . . ?
C27 C28 C29 C30 0.2(11) . . . . ?
C28 C29 C30 C31 -1.4(11) . . . . ?
C27 N13 C31 C30 -0.2(8) . . . . ?
Fe2 N13 C31 C30 -163.5(5) . . . . ?
C29 C30 C31 N13 1.4(10) . . . . ?

_refine_diff_density_max         0.295
_refine_diff_density_min         -0.245
_refine_diff_density_rms         0.055

####################################################################### 
# 
# 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_3-400K
# Added during the CSD deposition process: Friday 02 September 2016 02:49 AM
# end Validation Reply Form

_database_code_depnum_ccdc_archive 'CCDC 1419290'
_audit_update_record             
;
2016-09-02 deposited with the CCDC.
2016-09-26 downloaded from the CCDC.
;
# start Validation Reply Form
_vrf_PLAT341_3-400K              
;
PROBLEM: Low Bond Precision on  C-C Bonds ...............    0.01576 Ang.
RESPONSE: Due to the high temperature, 400K.
;
_vrf_PLAT939_3-400K              
;
PROBLEM: Large Value of Not (SHELXL) Weight Optimized S .     123.18 Check
RESPONSE: Due to the high temperature, 400K.
;

_audit_creation_method           SHELXL-2014/7
_shelx_SHELXL_version_number     2014/7
_chemical_name_systematic        ?
_chemical_name_common            ?
_chemical_melting_point          ?
_chemical_formula_moiety         'C62 H60 B2 Fe4 N26, 2(Cl O4) '
_chemical_formula_sum            'C62 H60 B2 Cl2 Fe4 N26 O8'
_chemical_formula_weight         1613.28

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'
O O 0.0106 0.0060 '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'

_space_group_crystal_system      monoclinic
_space_group_IT_number           14
_space_group_name_H-M_alt        'P 21/c'
_space_group_name_Hall           '-P 2ybc'

_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.
;

loop_
_space_group_symop_operation_xyz
'x, y, z'
'-x, y+1/2, -z+1/2'
'-x, -y, -z'
'x, -y-1/2, z-1/2'

_cell_length_a                   12.976(2)
_cell_length_b                   17.688(3)
_cell_length_c                   16.754(3)
_cell_angle_alpha                90
_cell_angle_beta                 107.769(3)
_cell_angle_gamma                90
_cell_volume                     3661.8(10)
_cell_formula_units_Z            2
_cell_measurement_temperature    400(2)
_cell_measurement_reflns_used    1953
_cell_measurement_theta_min      2.30
_cell_measurement_theta_max      19.64

_exptl_crystal_description       block
_exptl_crystal_colour            red
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    'not measured'
_exptl_crystal_density_diffrn    1.463
_exptl_crystal_F_000             1652
_exptl_transmission_factor_min   ?
_exptl_transmission_factor_max   ?
_exptl_crystal_size_max          0.100
_exptl_crystal_size_mid          0.050
_exptl_crystal_size_min          0.050
_exptl_absorpt_coefficient_mu    0.920
_shelx_estimated_absorpt_T_min   0.914
_shelx_estimated_absorpt_T_max   0.955
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_correction_T_min  0.9136
_exptl_absorpt_correction_T_max  0.9554
_exptl_absorpt_process_details   sadabs
_exptl_absorpt_special_details   ?
_diffrn_ambient_temperature      400(2)
_diffrn_radiation_wavelength     0.71073
_diffrn_radiation_type           MoK\a
_diffrn_source                   ?
_diffrn_measurement_device_type  'Bruker APEX-II CCD'
_diffrn_measurement_method       'φ and ω scans'
_diffrn_detector_area_resol_mean ?
_diffrn_reflns_number            16388
_diffrn_reflns_av_unetI/netI     0.0706
_diffrn_reflns_av_R_equivalents  0.0557
_diffrn_reflns_limit_h_min       -15
_diffrn_reflns_limit_h_max       10
_diffrn_reflns_limit_k_min       -15
_diffrn_reflns_limit_k_max       21
_diffrn_reflns_limit_l_min       -16
_diffrn_reflns_limit_l_max       19
_diffrn_reflns_theta_min         1.719
_diffrn_reflns_theta_max         24.999
_diffrn_reflns_theta_full        24.999
_diffrn_measured_fraction_theta_max 0.981
_diffrn_measured_fraction_theta_full 0.981
_diffrn_reflns_Laue_measured_fraction_max 0.981
_diffrn_reflns_Laue_measured_fraction_full 0.981
_diffrn_reflns_point_group_measured_fraction_max 0.981
_diffrn_reflns_point_group_measured_fraction_full 0.981
_reflns_number_total             6311
_reflns_number_gt                3758
_reflns_threshold_expression     'I > 2σ(I)'
_reflns_Friedel_coverage         0.000
_reflns_Friedel_fraction_max     .
_reflns_Friedel_fraction_full    .

_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.
;

_computing_data_collection       'Bruker APEX2'
_computing_cell_refinement       'Bruker SAINT'
_computing_data_reduction        'Bruker SAINT'
_computing_structure_solution    'SHELXS-2014 (Sheldrick, 2014)'
_computing_structure_refinement  'SHELXL-2014/7 (Sheldrick, 2014)'
_computing_molecular_graphics    'Bruker SHELXTL'
_computing_publication_material  'Bruker SHELXTL'
_refine_special_details          ?
_refine_ls_structure_factor_coef Fsqd
_refine_ls_matrix_type           full
_refine_ls_weighting_scheme      calc
_refine_ls_weighting_details     
'w=1/[σ²(Fo²)+(0.2000P)²] where P=(Fo²+2Fc²)/3'
_atom_sites_solution_primary     ?
_atom_sites_solution_secondary   ?
_atom_sites_solution_hydrogens   geom
_refine_ls_hydrogen_treatment    constr
_refine_ls_extinction_method     none
_refine_ls_extinction_coef       .
_refine_ls_number_reflns         6311
_refine_ls_number_parameters     516
_refine_ls_number_restraints     178
_refine_ls_R_factor_all          0.1252
_refine_ls_R_factor_gt           0.0694
_refine_ls_wR_factor_ref         0.3016
_refine_ls_wR_factor_gt          0.2109
_refine_ls_goodness_of_fit_ref   1.031
_refine_ls_restrained_S_all      1.041
_refine_ls_shift/su_max          0.001
_refine_ls_shift/su_mean         0.000

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 0.25603(8) 0.57600(5) 0.92591(6) 0.0486(4) Uani 1 1 d . . . . .
Fe2 Fe 0.37658(8) 0.32125(5) 1.03934(6) 0.0540(4) Uani 1 1 d . . . . .
B1 B 0.1301(8) 0.5727(5) 0.7330(6) 0.069(3) Uani 1 1 d . . . . .
N1 N 0.3301(6) 0.4331(4) 1.0288(5) 0.0697(18) Uani 1 1 d . . . . .
N2 N 0.4793(6) 0.6494(4) 0.9886(4) 0.0671(17) Uani 1 1 d . . . . .
N3 N 0.1984(7) 0.6447(5) 1.0733(5) 0.095(2) Uani 1 1 d . . . . .
N4 N 0.3044(5) 0.5290(3) 0.8365(4) 0.0541(14) Uani 1 1 d . . . . .
N5 N 0.2436(6) 0.5328(3) 0.7568(4) 0.0664(17) Uani 1 1 d . . . . .
N6 N 0.2027(5) 0.6636(3) 0.8526(4) 0.0549(14) Uani 1 1 d . . . . .
N7 N 0.1539(5) 0.6532(4) 0.7697(4) 0.0654(16) Uani 1 1 d . . . . .
N8 N 0.1127(5) 0.5300(3) 0.8727(4) 0.0550(14) Uani 1 1 d . . . . .
N9 N 0.0680(5) 0.5341(4) 0.7883(4) 0.0671(17) Uani 1 1 d . . . . .
N10 N 0.4692(6) 0.3068(4) 1.1676(4) 0.0668(17) Uani 1 1 d . . . . .
N11 N 0.4082(5) 0.1991(3) 1.0512(4) 0.0588(15) Uani 1 1 d . . . . .
N12 N 0.2277(5) 0.2796(4) 1.0600(4) 0.0651(17) Uani 1 1 d . . . . .
N13 N 0.2960(6) 0.2813(4) 0.9118(4) 0.0732(19) Uani 1 1 d . . . . .
C1 C 0.3029(6) 0.4892(4) 0.9930(4) 0.0526(16) Uani 1 1 d . . . . .
C2 C 0.3961(6) 0.6222(4) 0.9710(4) 0.0503(16) Uani 1 1 d . . . . .
C3 C 0.2173(6) 0.6195(4) 1.0179(6) 0.0605(19) Uani 1 1 d . . . . .
C4 C 0.3930(7) 0.4889(4) 0.8387(6) 0.070(2) Uani 1 1 d . . . . .
H4 H 0.4483 0.4771 0.8874 0.084 Uiso 1 1 calc R U . . .
C5 C 0.3911(9) 0.4680(6) 0.7609(7) 0.090(3) Uani 1 1 d . . . . .
H5 H 0.4435 0.4409 0.7455 0.108 Uiso 1 1 calc R U . . .
C6 C 0.2940(9) 0.4957(6) 0.7088(6) 0.094(3) Uani 1 1 d . . . . .
H6 H 0.2681 0.4899 0.6509 0.113 Uiso 1 1 calc R U . . .
C7 C 0.2095(7) 0.7384(4) 0.8681(6) 0.069(2) Uani 1 1 d . . . . .
H7 H 0.2409 0.7615 0.9197 0.083 Uiso 1 1 calc R U . . .
C8 C 0.1617(8) 0.7741(5) 0.7937(7) 0.088(3) Uani 1 1 d . . . . .
H8 H 0.1537 0.8262 0.7865 0.106 Uiso 1 1 calc R U . . .
C9 C 0.1280(8) 0.7220(5) 0.7323(6) 0.083(3) Uani 1 1 d . . . . .
H9 H 0.0938 0.7313 0.6757 0.099 Uiso 1 1 calc R U . . .
C10 C 0.0442(7) 0.4932(4) 0.9024(6) 0.073(2) Uani 1 1 d . . . . .
H10 H 0.0555 0.4821 0.9586 0.088 Uiso 1 1 calc R U . . .
C11 C -0.0477(8) 0.4735(5) 0.8374(7) 0.094(3) Uani 1 1 d . . . . .
H11 H -0.1090 0.4485 0.8412 0.113 Uiso 1 1 calc R U . . .
C12 C -0.0278(8) 0.4987(6) 0.7676(8) 0.097(3) Uani 1 1 d . . . . .
H12 H -0.0737 0.4925 0.7133 0.116 Uiso 1 1 calc R U . . .
C13 C 0.0674(9) 0.5683(6) 0.6375(6) 0.099(3) Uani 1 1 d . . . . .
H13A H 0.0028 0.5983 0.6256 0.149 Uiso 1 1 calc R U . . .
H13B H 0.0484 0.5167 0.6220 0.149 Uiso 1 1 calc R U . . .
H13C H 0.1124 0.5873 0.6059 0.149 Uiso 1 1 calc R U . . .
C14 C 0.4773(7) 0.3593(6) 1.2285(5) 0.081(2) Uani 1 1 d . . . . .
H14 H 0.4371 0.4037 1.2168 0.097 Uiso 1 1 calc R U . . .
C15 C 0.5507(9) 0.3447(8) 1.3130(6) 0.101(3) Uani 1 1 d . . . . .
H15 H 0.5589 0.3798 1.3558 0.122 Uiso 1 1 calc R U . . .
C16 C 0.6057(10) 0.2793(7) 1.3266(7) 0.107(4) Uani 1 1 d . . . . .
H16 H 0.6525 0.2694 1.3798 0.128 Uiso 1 1 calc R U . . .
C17 C 0.5954(10) 0.2285(7) 1.2667(7) 0.103(3) Uani 1 1 d . . . . .
H17 H 0.6329 0.1830 1.2786 0.123 Uiso 1 1 calc R U . . .
C18 C 0.5291(7) 0.2430(5) 1.1868(5) 0.072(2) Uani 1 1 d . . . . .
C19 C 0.5165(7) 0.1903(5) 1.1145(6) 0.073(2) Uani 1 1 d . . . . .
H19A H 0.5723 0.2008 1.0885 0.087 Uiso 1 1 calc R U . . .
H19B H 0.5254 0.1386 1.1346 0.087 Uiso 1 1 calc R U . . .
C20 C 0.3268(7) 0.1625(5) 1.0820(6) 0.074(2) Uani 1 1 d . . . . .
H20A H 0.3564 0.1556 1.1421 0.089 Uiso 1 1 calc R U . . .
H20B H 0.3112 0.1128 1.0566 0.089 Uiso 1 1 calc R U . . .
C21 C 0.2235(6) 0.2063(5) 1.0636(5) 0.065(2) Uani 1 1 d . . . . .
C22 C 0.1252(8) 0.1707(6) 1.0547(6) 0.084(3) Uani 1 1 d . . . . .
H22 H 0.1225 0.1182 1.0559 0.101 Uiso 1 1 calc R U . . .
C23 C 0.0338(10) 0.2107(9) 1.0445(8) 0.119(4) Uani 1 1 d . . . . .
H23 H -0.0321 0.1865 1.0375 0.143 Uiso 1 1 calc R U . . .
C24 C 0.0406(8) 0.2864(8) 1.0447(7) 0.108(4) Uani 1 1 d . . . . .
H24 H -0.0208 0.3154 1.0396 0.130 Uiso 1 1 calc R U . . .
C25 C 0.1397(8) 0.3219(6) 1.0525(7) 0.091(3) Uani 1 1 d . . . . .
H25 H 0.1443 0.3744 1.0524 0.110 Uiso 1 1 calc R U . . .
C26 C 0.4060(8) 0.1734(5) 0.9691(6) 0.084(3) Uani 1 1 d . . . . .
H26A H 0.3981 0.1188 0.9664 0.101 Uiso 1 1 calc R U . . .
H26B H 0.4742 0.1859 0.9597 0.101 Uiso 1 1 calc R U . . .
C27 C 0.3162(8) 0.2081(6) 0.9026(5) 0.079(2) Uani 1 1 d . . . . .
C28 C 0.2542(10) 0.1684(8) 0.8350(7) 0.110(4) Uani 1 1 d . . . . .
H28 H 0.2641 0.1169 0.8287 0.132 Uiso 1 1 calc R U . . .
C29 C 0.1742(13) 0.2101(11) 0.7757(8) 0.149(6) Uani 1 1 d . . . . .
H29 H 0.1330 0.1861 0.7270 0.179 Uiso 1 1 calc R U . . .
C30 C 0.1550(12) 0.2846(9) 0.7868(8) 0.126(4) Uani 1 1 d . . . . .
H30 H 0.0992 0.3106 0.7484 0.152 Uiso 1 1 calc R U . . .
C31 C 0.2193(8) 0.3185(6) 0.8550(6) 0.092(3) Uani 1 1 d . . . . .
H31 H 0.2100 0.3698 0.8628 0.110 Uiso 1 1 calc R U . . .
Cl1 Cl 0.2738(8) 0.9495(5) 0.9616(6) 0.0972(17) Uani 0.651(11) 1 d D U P A 1
O1 O 0.3705(10) 0.9758(8) 1.0190(8) 0.145(4) Uani 0.651(11) 1 d D U P A 1
O2 O 0.2679(15) 0.9475(10) 0.8762(7) 0.138(4) Uani 0.651(11) 1 d D U P A 1
O3 O 0.1937(13) 0.9996(11) 0.9667(11) 0.158(4) Uani 0.651(11) 1 d D U P A 1
O4 O 0.2620(17) 0.8773(7) 0.9924(10) 0.150(4) Uani 0.651(11) 1 d D U P A 1
Cl1' Cl 0.2623(17) 0.9458(12) 0.9568(15) 0.113(3) Uani 0.349(11) 1 d D U P A 2
O1' O 0.1570(19) 0.9158(15) 0.9313(18) 0.143(5) Uani 0.349(11) 1 d D U P A 2
O2' O 0.310(3) 0.9753(18) 0.8989(17) 0.137(5) Uani 0.349(11) 1 d D U P A 2
O3' O 0.244(3) 1.0110(16) 0.9972(19) 0.140(5) Uani 0.349(11) 1 d D U P A 2
O4' O 0.332(2) 0.8841(14) 0.9836(19) 0.129(5) Uani 0.349(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
Fe1 C1 1.891(7) . ?
Fe1 C3 1.922(9) . ?
Fe1 C2 1.925(7) . ?
Fe1 N6 1.967(6) . ?
Fe1 N8 1.976(6) . ?
Fe1 N4 1.976(6) . ?
Fe2 N1 2.061(6) . ?
Fe2 N2 2.127(7) 3_667 ?
Fe2 N10 2.133(7) . ?
Fe2 N13 2.189(7) . ?
Fe2 N12 2.191(6) . ?
Fe2 N11 2.197(6) . ?
B1 N7 1.546(11) . ?
B1 N9 1.559(12) . ?
B1 C13 1.560(13) . ?
B1 N5 1.571(12) . ?
N1 C1 1.157(9) . ?
N2 C2 1.135(9) . ?
N2 Fe2 2.127(7) 3_667 ?
N3 C3 1.121(9) . ?
N4 N5 1.328(8) . ?
N4 C4 1.342(10) . ?
N5 C6 1.352(11) . ?
N6 C7 1.346(9) . ?
N6 N7 1.352(8) . ?
N7 C9 1.363(10) . ?
N8 C10 1.315(9) . ?
N8 N9 1.356(8) . ?
N9 C12 1.340(11) . ?
N10 C18 1.352(10) . ?
N10 C14 1.361(11) . ?
N11 C26 1.440(11) . ?
N11 C20 1.461(10) . ?
N11 C19 1.487(10) . ?
N12 C21 1.301(10) . ?
N12 C25 1.339(11) . ?
N13 C31 1.324(11) . ?
N13 C27 1.339(12) . ?
C4 C5 1.348(11) . ?
C4 H4 0.9300 . ?
C5 C6 1.385(14) . ?
C5 H5 0.9300 . ?
C6 H6 0.9300 . ?
C7 C8 1.366(12) . ?
C7 H7 0.9300 . ?
C8 C9 1.351(14) . ?
C8 H8 0.9300 . ?
C9 H9 0.9300 . ?
C10 C11 1.392(13) . ?
C10 H10 0.9300 . ?
C11 C12 1.347(13) . ?
C11 H11 0.9300 . ?
C12 H12 0.9300 . ?
C13 H13A 0.9600 . ?
C13 H13B 0.9600 . ?
C13 H13C 0.9600 . ?
C14 C15 1.468(13) . ?
C14 H14 0.9300 . ?
C15 C16 1.342(16) . ?
C15 H15 0.9300 . ?
C16 C17 1.324(16) . ?
C16 H16 0.9300 . ?
C17 C18 1.376(13) . ?
C17 H17 0.9300 . ?
C18 C19 1.497(12) . ?
C19 H19A 0.9700 . ?
C19 H19B 0.9700 . ?
C20 C21 1.497(12) . ?
C20 H20A 0.9700 . ?
C20 H20B 0.9700 . ?
C21 C22 1.389(11) . ?
C22 C23 1.346(16) . ?
C22 H22 0.9300 . ?
C23 C24 1.342(17) . ?
C23 H23 0.9300 . ?
C24 C25 1.401(14) . ?
C24 H24 0.9300 . ?
C25 H25 0.9300 . ?
C26 C27 1.478(14) . ?
C26 H26A 0.9700 . ?
C26 H26B 0.9700 . ?
C27 C28 1.366(13) . ?
C28 C29 1.408(19) . ?
C28 H28 0.9300 . ?
C29 C30 1.36(2) . ?
C29 H29 0.9300 . ?
C30 C31 1.334(15) . ?
C30 H30 0.9300 . ?
C31 H31 0.9300 . ?
Cl1 O3 1.387(9) . ?
Cl1 O4 1.403(9) . ?
Cl1 O1 1.406(9) . ?
Cl1 O2 1.410(9) . ?
Cl1' O3' 1.394(10) . ?
Cl1' O4' 1.400(10) . ?
Cl1' O2' 1.404(10) . ?
Cl1' O1' 1.404(10) . ?

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
C1 Fe1 C3 87.9(3) . . ?
C1 Fe1 C2 91.0(3) . . ?
C3 Fe1 C2 87.8(3) . . ?
C1 Fe1 N6 177.5(3) . . ?
C3 Fe1 N6 93.3(3) . . ?
C2 Fe1 N6 91.2(3) . . ?
C1 Fe1 N8 91.2(3) . . ?
C3 Fe1 N8 94.9(3) . . ?
C2 Fe1 N8 176.5(3) . . ?
N6 Fe1 N8 86.5(2) . . ?
C1 Fe1 N4 89.4(3) . . ?
C3 Fe1 N4 176.4(3) . . ?
C2 Fe1 N4 89.8(3) . . ?
N6 Fe1 N4 89.5(2) . . ?
N8 Fe1 N4 87.6(2) . . ?
N1 Fe2 N2 90.1(3) . 3_667 ?
N1 Fe2 N10 105.2(3) . . ?
N2 Fe2 N10 89.3(3) 3_667 . ?
N1 Fe2 N13 100.7(3) . . ?
N2 Fe2 N13 93.1(3) 3_667 . ?
N10 Fe2 N13 154.0(3) . . ?
N1 Fe2 N12 95.0(3) . . ?
N2 Fe2 N12 173.7(3) 3_667 . ?
N10 Fe2 N12 93.1(3) . . ?
N13 Fe2 N12 82.2(3) . . ?
N1 Fe2 N11 173.7(2) . . ?
N2 Fe2 N11 96.1(2) 3_667 . ?
N10 Fe2 N11 76.0(2) . . ?
N13 Fe2 N11 77.9(3) . . ?
N12 Fe2 N11 78.7(2) . . ?
N7 B1 N9 104.1(7) . . ?
N7 B1 C13 115.6(8) . . ?
N9 B1 C13 112.7(8) . . ?
N7 B1 N5 104.7(7) . . ?
N9 B1 N5 105.4(6) . . ?
C13 B1 N5 113.2(8) . . ?
C1 N1 Fe2 154.5(7) . . ?
C2 N2 Fe2 151.3(6) . 3_667 ?
N5 N4 C4 107.2(6) . . ?
N5 N4 Fe1 120.8(5) . . ?
C4 N4 Fe1 132.0(6) . . ?
N4 N5 C6 109.1(7) . . ?
N4 N5 B1 120.1(6) . . ?
C6 N5 B1 130.8(8) . . ?
C7 N6 N7 108.3(6) . . ?
C7 N6 Fe1 131.6(5) . . ?
N7 N6 Fe1 120.0(4) . . ?
N6 N7 C9 108.9(7) . . ?
N6 N7 B1 120.6(6) . . ?
C9 N7 B1 130.4(8) . . ?
C10 N8 N9 107.3(7) . . ?
C10 N8 Fe1 133.2(6) . . ?
N9 N8 Fe1 119.5(4) . . ?
C12 N9 N8 108.2(8) . . ?
C12 N9 B1 131.2(8) . . ?
N8 N9 B1 120.6(6) . . ?
C18 N10 C14 118.9(8) . . ?
C18 N10 Fe2 116.5(6) . . ?
C14 N10 Fe2 124.4(6) . . ?
C26 N11 C20 113.0(7) . . ?
C26 N11 C19 112.8(7) . . ?
C20 N11 C19 109.2(6) . . ?
C26 N11 Fe2 106.0(5) . . ?
C20 N11 Fe2 109.4(5) . . ?
C19 N11 Fe2 106.1(5) . . ?
C21 N12 C25 121.0(8) . . ?
C21 N12 Fe2 113.2(5) . . ?
C25 N12 Fe2 124.4(6) . . ?
C31 N13 C27 121.9(8) . . ?
C31 N13 Fe2 124.9(7) . . ?
C27 N13 Fe2 111.9(6) . . ?
N1 C1 Fe1 175.1(7) . . ?
N2 C2 Fe1 172.2(6) . . ?
N3 C3 Fe1 177.5(8) . . ?
N4 C4 C5 110.8(8) . . ?
N4 C4 H4 124.6 . . ?
C5 C4 H4 124.6 . . ?
C4 C5 C6 104.9(8) . . ?
C4 C5 H5 127.5 . . ?
C6 C5 H5 127.5 . . ?
N5 C6 C5 108.0(8) . . ?
N5 C6 H6 126.0 . . ?
C5 C6 H6 126.0 . . ?
N6 C7 C8 107.1(8) . . ?
N6 C7 H7 126.4 . . ?
C8 C7 H7 126.4 . . ?
C9 C8 C7 109.3(8) . . ?
C9 C8 H8 125.3 . . ?
C7 C8 H8 125.3 . . ?
C8 C9 N7 106.4(8) . . ?
C8 C9 H9 126.8 . . ?
N7 C9 H9 126.8 . . ?
N8 C10 C11 110.2(8) . . ?
N8 C10 H10 124.9 . . ?
C11 C10 H10 124.9 . . ?
C12 C11 C10 104.5(8) . . ?
C12 C11 H11 127.7 . . ?
C10 C11 H11 127.7 . . ?
N9 C12 C11 109.8(9) . . ?
N9 C12 H12 125.1 . . ?
C11 C12 H12 125.1 . . ?
B1 C13 H13A 109.5 . . ?
B1 C13 H13B 109.5 . . ?
H13A C13 H13B 109.5 . . ?
B1 C13 H13C 109.5 . . ?
H13A C13 H13C 109.5 . . ?
H13B C13 H13C 109.5 . . ?
N10 C14 C15 118.8(10) . . ?
N10 C14 H14 120.6 . . ?
C15 C14 H14 120.6 . . ?
C16 C15 C14 118.1(11) . . ?
C16 C15 H15 121.0 . . ?
C14 C15 H15 121.0 . . ?
C17 C16 C15 122.1(11) . . ?
C17 C16 H16 119.0 . . ?
C15 C16 H16 119.0 . . ?
C16 C17 C18 120.0(12) . . ?
C16 C17 H17 120.0 . . ?
C18 C17 H17 120.0 . . ?
N10 C18 C17 122.0(10) . . ?
N10 C18 C19 114.4(7) . . ?
C17 C18 C19 123.6(9) . . ?
N11 C19 C18 111.0(7) . . ?
N11 C19 H19A 109.4 . . ?
C18 C19 H19A 109.4 . . ?
N11 C19 H19B 109.4 . . ?
C18 C19 H19B 109.4 . . ?
H19A C19 H19B 108.0 . . ?
N11 C20 C21 113.4(6) . . ?
N11 C20 H20A 108.9 . . ?
C21 C20 H20A 108.9 . . ?
N11 C20 H20B 108.9 . . ?
C21 C20 H20B 108.9 . . ?
H20A C20 H20B 107.7 . . ?
N12 C21 C22 119.8(9) . . ?
N12 C21 C20 118.5(7) . . ?
C22 C21 C20 121.6(8) . . ?
C23 C22 C21 121.4(10) . . ?
C23 C22 H22 119.3 . . ?
C21 C22 H22 119.3 . . ?
C24 C23 C22 117.9(10) . . ?
C24 C23 H23 121.0 . . ?
C22 C23 H23 121.0 . . ?
C23 C24 C25 120.4(10) . . ?
C23 C24 H24 119.8 . . ?
C25 C24 H24 119.8 . . ?
N12 C25 C24 119.4(10) . . ?
N12 C25 H25 120.3 . . ?
C24 C25 H25 120.3 . . ?
N11 C26 C27 111.7(7) . . ?
N11 C26 H26A 109.3 . . ?
C27 C26 H26A 109.3 . . ?
N11 C26 H26B 109.3 . . ?
C27 C26 H26B 109.3 . . ?
H26A C26 H26B 107.9 . . ?
N13 C27 C28 120.4(10) . . ?
N13 C27 C26 116.8(8) . . ?
C28 C27 C26 122.7(10) . . ?
C27 C28 C29 115.9(13) . . ?
C27 C28 H28 122.1 . . ?
C29 C28 H28 122.1 . . ?
C30 C29 C28 122.5(12) . . ?
C30 C29 H29 118.8 . . ?
C28 C29 H29 118.8 . . ?
C31 C30 C29 117.3(13) . . ?
C31 C30 H30 121.4 . . ?
C29 C30 H30 121.4 . . ?
N13 C31 C30 121.9(12) . . ?
N13 C31 H31 119.0 . . ?
C30 C31 H31 119.0 . . ?
O3 Cl1 O4 113.0(15) . . ?
O3 Cl1 O1 106.0(11) . . ?
O4 Cl1 O1 102.9(12) . . ?
O3 Cl1 O2 105.6(13) . . ?
O4 Cl1 O2 111.8(11) . . ?
O1 Cl1 O2 117.6(12) . . ?
O3' Cl1' O4' 133(3) . . ?
O3' Cl1' O2' 102(3) . . ?
O4' Cl1' O2' 98(2) . . ?
O3' Cl1' O1' 100(2) . . ?
O4' Cl1' O1' 106(2) . . ?
O2' Cl1' O1' 122(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
C4 N4 N5 C6 -0.6(9) . . . . ?
Fe1 N4 N5 C6 -179.3(6) . . . . ?
C4 N4 N5 B1 176.8(7) . . . . ?
Fe1 N4 N5 B1 -1.9(9) . . . . ?
N7 B1 N5 N4 56.0(9) . . . . ?
N9 B1 N5 N4 -53.5(8) . . . . ?
C13 B1 N5 N4 -177.1(7) . . . . ?
N7 B1 N5 C6 -127.2(9) . . . . ?
N9 B1 N5 C6 123.2(9) . . . . ?
C13 B1 N5 C6 -0.4(13) . . . . ?
C7 N6 N7 C9 -1.0(9) . . . . ?
Fe1 N6 N7 C9 -177.8(6) . . . . ?
C7 N6 N7 B1 -177.5(7) . . . . ?
Fe1 N6 N7 B1 5.7(10) . . . . ?
N9 B1 N7 N6 52.2(9) . . . . ?
C13 B1 N7 N6 176.4(8) . . . . ?
N5 B1 N7 N6 -58.2(10) . . . . ?
N9 B1 N7 C9 -123.3(9) . . . . ?
C13 B1 N7 C9 0.9(14) . . . . ?
N5 B1 N7 C9 126.2(9) . . . . ?
C10 N8 N9 C12 -0.6(9) . . . . ?
Fe1 N8 N9 C12 179.6(6) . . . . ?
C10 N8 N9 B1 -178.4(7) . . . . ?
Fe1 N8 N9 B1 1.8(9) . . . . ?
N7 B1 N9 C12 126.1(9) . . . . ?
C13 B1 N9 C12 0.1(13) . . . . ?
N5 B1 N9 C12 -123.9(9) . . . . ?
N7 B1 N9 N8 -56.6(9) . . . . ?
C13 B1 N9 N8 177.4(7) . . . . ?
N5 B1 N9 N8 53.4(9) . . . . ?
N5 N4 C4 C5 1.4(9) . . . . ?
Fe1 N4 C4 C5 179.8(6) . . . . ?
N4 C4 C5 C6 -1.5(11) . . . . ?
N4 N5 C6 C5 -0.4(10) . . . . ?
B1 N5 C6 C5 -177.4(8) . . . . ?
C4 C5 C6 N5 1.1(11) . . . . ?
N7 N6 C7 C8 1.5(9) . . . . ?
Fe1 N6 C7 C8 177.9(6) . . . . ?
N6 C7 C8 C9 -1.5(11) . . . . ?
C7 C8 C9 N7 0.9(11) . . . . ?
N6 N7 C9 C8 0.1(10) . . . . ?
B1 N7 C9 C8 176.0(9) . . . . ?
N9 N8 C10 C11 -0.8(9) . . . . ?
Fe1 N8 C10 C11 179.0(6) . . . . ?
N8 C10 C11 C12 1.8(11) . . . . ?
N8 N9 C12 C11 1.7(11) . . . . ?
B1 N9 C12 C11 179.3(9) . . . . ?
C10 C11 C12 N9 -2.1(11) . . . . ?
C18 N10 C14 C15 -0.1(12) . . . . ?
Fe2 N10 C14 C15 -175.2(6) . . . . ?
N10 C14 C15 C16 -0.9(14) . . . . ?
C14 C15 C16 C17 0.0(18) . . . . ?
C15 C16 C17 C18 2.0(19) . . . . ?
C14 N10 C18 C17 2.1(12) . . . . ?
Fe2 N10 C18 C17 177.5(7) . . . . ?
C14 N10 C18 C19 -178.1(7) . . . . ?
Fe2 N10 C18 C19 -2.7(9) . . . . ?
C16 C17 C18 N10 -3.0(15) . . . . ?
C16 C17 C18 C19 177.2(10) . . . . ?
C26 N11 C19 C18 157.6(7) . . . . ?
C20 N11 C19 C18 -75.8(8) . . . . ?
Fe2 N11 C19 C18 42.0(7) . . . . ?
N10 C18 C19 N11 -27.5(9) . . . . ?
C17 C18 C19 N11 152.3(8) . . . . ?
C26 N11 C20 C21 -93.8(9) . . . . ?
C19 N11 C20 C21 139.8(7) . . . . ?
Fe2 N11 C20 C21 24.1(9) . . . . ?
C25 N12 C21 C22 3.7(12) . . . . ?
Fe2 N12 C21 C22 -163.5(6) . . . . ?
C25 N12 C21 C20 -173.0(8) . . . . ?
Fe2 N12 C21 C20 19.8(9) . . . . ?
N11 C20 C21 N12 -30.7(11) . . . . ?
N11 C20 C21 C22 152.7(8) . . . . ?
N12 C21 C22 C23 -1.7(14) . . . . ?
C20 C21 C22 C23 174.9(10) . . . . ?
C21 C22 C23 C24 -1.2(17) . . . . ?
C22 C23 C24 C25 2.1(19) . . . . ?
C21 N12 C25 C24 -2.8(14) . . . . ?
Fe2 N12 C25 C24 162.9(8) . . . . ?
C23 C24 C25 N12 -0.2(18) . . . . ?
C20 N11 C26 C27 77.6(9) . . . . ?
C19 N11 C26 C27 -157.9(7) . . . . ?
Fe2 N11 C26 C27 -42.2(8) . . . . ?
C31 N13 C27 C28 -2.9(13) . . . . ?
Fe2 N13 C27 C28 164.4(8) . . . . ?
C31 N13 C27 C26 178.2(8) . . . . ?
Fe2 N13 C27 C26 -14.4(9) . . . . ?
N11 C26 C27 N13 40.0(11) . . . . ?
N11 C26 C27 C28 -138.8(9) . . . . ?
N13 C27 C28 C29 3.4(16) . . . . ?
C26 C27 C28 C29 -177.8(11) . . . . ?
C27 C28 C29 C30 -4(2) . . . . ?
C28 C29 C30 C31 4(2) . . . . ?
C27 N13 C31 C30 2.6(15) . . . . ?
Fe2 N13 C31 C30 -163.0(9) . . . . ?
C29 C30 C31 N13 -3(2) . . . . ?

_refine_diff_density_max         0.569
_refine_diff_density_min         -0.700
_refine_diff_density_rms         0.168

####################################################################### 
# 
# 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_3_H2O-100K
_database_code_depnum_ccdc_archive 'CCDC 1419291'
_audit_update_record             
;
2016-09-02 deposited with the CCDC.
2016-09-26 downloaded from the CCDC.
;

_audit_creation_method           SHELXL-2014/7
_shelx_SHELXL_version_number     2014/7
_chemical_name_systematic        ?
_chemical_name_common            ?
_chemical_melting_point          ?
_chemical_formula_moiety         'C62 H60 B2 Fe4 N26, 2(Cl O4), 2(H2 O)'
_chemical_formula_sum            'C62 H64 B2 Cl2 Fe4 N26 O10'
_chemical_formula_weight         1649.31

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'
O O 0.0106 0.0060 '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'

_space_group_crystal_system      monoclinic
_space_group_IT_number           14
_space_group_name_H-M_alt        'P 21/c'
_space_group_name_Hall           '-P 2ybc'

_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.
;

loop_
_space_group_symop_operation_xyz
'x, y, z'
'-x, y+1/2, -z+1/2'
'-x, -y, -z'
'x, -y-1/2, z-1/2'

_cell_length_a                   12.8450(11)
_cell_length_b                   17.4067(15)
_cell_length_c                   16.5485(14)
_cell_angle_alpha                90
_cell_angle_beta                 108.7210(10)
_cell_angle_gamma                90
_cell_volume                     3504.3(5)
_cell_formula_units_Z            2
_cell_measurement_temperature    100(2)
_cell_measurement_reflns_used    4893
_cell_measurement_theta_min      2.34
_cell_measurement_theta_max      28.36

_exptl_crystal_description       block
_exptl_crystal_colour            red
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    'not measured'
_exptl_crystal_density_diffrn    1.563
_exptl_crystal_F_000             1692
_exptl_transmission_factor_min   ?
_exptl_transmission_factor_max   ?
_exptl_crystal_size_max          0.100
_exptl_crystal_size_mid          0.050
_exptl_crystal_size_min          0.050
_exptl_absorpt_coefficient_mu    0.965
_shelx_estimated_absorpt_T_min   0.910
_shelx_estimated_absorpt_T_max   0.953
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_correction_T_min  0.9096
_exptl_absorpt_correction_T_max  0.9533
_exptl_absorpt_process_details   sadabs
_exptl_absorpt_special_details   ?
_diffrn_ambient_temperature      100(2)
_diffrn_radiation_wavelength     0.71073
_diffrn_radiation_type           MoK\a
_diffrn_source                   ?
_diffrn_measurement_device_type  'Bruker APEX-II CCD'
_diffrn_measurement_method       'φ and ω scans'
_diffrn_detector_area_resol_mean ?
_diffrn_reflns_number            20986
_diffrn_reflns_av_unetI/netI     0.0485
_diffrn_reflns_av_R_equivalents  0.0434
_diffrn_reflns_limit_h_min       -15
_diffrn_reflns_limit_h_max       15
_diffrn_reflns_limit_k_min       -21
_diffrn_reflns_limit_k_max       15
_diffrn_reflns_limit_l_min       -19
_diffrn_reflns_limit_l_max       20
_diffrn_reflns_theta_min         1.748
_diffrn_reflns_theta_max         25.500
_diffrn_reflns_theta_full        25.242
_diffrn_measured_fraction_theta_max 0.994
_diffrn_measured_fraction_theta_full 0.994
_diffrn_reflns_Laue_measured_fraction_max 0.994
_diffrn_reflns_Laue_measured_fraction_full 0.994
_diffrn_reflns_point_group_measured_fraction_max 0.994
_diffrn_reflns_point_group_measured_fraction_full 0.994
_reflns_number_total             6476
_reflns_number_gt                5033
_reflns_threshold_expression     'I > 2σ(I)'
_reflns_Friedel_coverage         0.000
_reflns_Friedel_fraction_max     .
_reflns_Friedel_fraction_full    .

_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.
;

_computing_data_collection       'Bruker APEX2'
_computing_cell_refinement       'Bruker SAINT'
_computing_data_reduction        'Bruker SAINT'
_computing_structure_solution    'SHELXS-2014 (Sheldrick, 2014)'
_computing_structure_refinement  'SHELXL-2014/7 (Sheldrick, 2014)'
_computing_molecular_graphics    'Bruker SHELXTL'
_computing_publication_material  'Bruker SHELXTL'
_refine_special_details          ?
_refine_ls_structure_factor_coef Fsqd
_refine_ls_matrix_type           full
_refine_ls_weighting_scheme      calc
_refine_ls_weighting_details     
'w=1/[σ²(Fo²)+(0.0465P)²+2.8474P] where P=(Fo²+2Fc²)/3'
_atom_sites_solution_primary     ?
_atom_sites_solution_secondary   ?
_atom_sites_solution_hydrogens   mixed
_refine_ls_hydrogen_treatment    constr
_refine_ls_extinction_method     none
_refine_ls_extinction_coef       .
_refine_ls_number_reflns         6476
_refine_ls_number_parameters     524
_refine_ls_number_restraints     184
_refine_ls_R_factor_all          0.0554
_refine_ls_R_factor_gt           0.0372
_refine_ls_wR_factor_ref         0.1016
_refine_ls_wR_factor_gt          0.0915
_refine_ls_goodness_of_fit_ref   1.021
_refine_ls_restrained_S_all      1.062
_refine_ls_shift/su_max          0.005
_refine_ls_shift/su_mean         0.000

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 0.73591(3) 1.08050(2) 0.57105(2) 0.01495(11) Uani 1 1 d . . . . .
Fe2 Fe 0.63107(3) 0.82042(2) 0.46023(2) 0.01676(11) Uani 1 1 d . . . . .
B1 B 0.8724(3) 1.0769(2) 0.7664(2) 0.0246(7) Uani 1 1 d . . . . .
N1 N 0.67061(18) 0.92770(14) 0.47723(14) 0.0194(5) Uani 1 1 d . . . . .
N2 N 0.50695(19) 1.15219(13) 0.52169(14) 0.0188(5) Uani 1 1 d . . . . .
N3 N 0.7814(2) 1.14591(17) 0.41338(17) 0.0308(6) Uani 1 1 d . . . . .
N4 N 0.69351(18) 1.03086(13) 0.66333(14) 0.0183(5) Uani 1 1 d . . . . .
N5 N 0.76080(19) 1.03379(14) 0.74573(14) 0.0212(5) Uani 1 1 d . . . . .
N6 N 0.79154(18) 1.16951(13) 0.64524(14) 0.0179(5) Uani 1 1 d . . . . .
N7 N 0.84488(19) 1.15943(14) 0.73022(15) 0.0216(5) Uani 1 1 d . . . . .
N8 N 0.88397(18) 1.03672(13) 0.62247(14) 0.0177(5) Uani 1 1 d . . . . .
N9 N 0.93316(18) 1.03865(14) 0.70844(15) 0.0217(5) Uani 1 1 d . . . . .
N10 N 0.55008(19) 0.82341(14) 0.33679(15) 0.0221(5) Uani 1 1 d . . . . .
N11 N 0.59253(19) 0.70952(14) 0.44461(15) 0.0210(5) Uani 1 1 d . . . . .
N12 N 0.76996(18) 0.78878(14) 0.44358(14) 0.0185(5) Uani 1 1 d . . . . .
N13 N 0.70468(18) 0.79061(14) 0.58096(14) 0.0194(5) Uani 1 1 d . . . . .
C1 C 0.6907(2) 0.98866(17) 0.50504(17) 0.0178(6) Uani 1 1 d . . . . .
C2 C 0.5922(2) 1.12566(16) 0.53140(17) 0.0180(6) Uani 1 1 d . . . . .
C3 C 0.7660(2) 1.12350(17) 0.47439(18) 0.0209(6) Uani 1 1 d . . . . .
C4 C 0.6061(2) 0.98973(17) 0.66227(19) 0.0225(6) Uani 1 1 d . . . . .
H4 H 0.5461 0.9783 0.6126 0.027 Uiso 1 1 calc R U . . .
C5 C 0.6152(2) 0.96581(19) 0.7443(2) 0.0289(7) Uani 1 1 d . . . . .
H5 H 0.5642 0.9358 0.7615 0.035 Uiso 1 1 calc R U . . .
C6 C 0.7141(3) 0.99503(19) 0.7952(2) 0.0286(7) Uani 1 1 d . . . . .
H6 H 0.7442 0.9888 0.8553 0.034 Uiso 1 1 calc R U . . .
C7 C 0.7876(2) 1.24499(16) 0.6307(2) 0.0224(6) Uani 1 1 d . . . . .
H7 H 0.7557 1.2683 0.5764 0.027 Uiso 1 1 calc R U . . .
C8 C 0.8368(2) 1.28445(19) 0.7060(2) 0.0284(7) Uani 1 1 d . . . . .
H8 H 0.8445 1.3385 0.7136 0.034 Uiso 1 1 calc R U . . .
C9 C 0.8719(3) 1.22881(19) 0.7671(2) 0.0293(7) Uani 1 1 d . . . . .
H9 H 0.9092 1.2376 0.8260 0.035 Uiso 1 1 calc R U . . .
C10 C 0.9526(2) 1.00146(17) 0.5893(2) 0.0238(7) Uani 1 1 d . . . . .
H10 H 0.9387 0.9923 0.5302 0.029 Uiso 1 1 calc R U . . .
C11 C 1.0478(2) 0.97998(19) 0.6537(2) 0.0328(8) Uani 1 1 d . . . . .
H11 H 1.1100 0.9539 0.6478 0.039 Uiso 1 1 calc R U . . .
C12 C 1.0320(2) 1.00486(19) 0.7281(2) 0.0301(7) Uani 1 1 d . . . . .
H12 H 1.0827 0.9990 0.7839 0.036 Uiso 1 1 calc R U . . .
C13 C 0.9416(3) 1.0747(2) 0.86458(19) 0.0359(8) Uani 1 1 d . . . . .
H13A H 1.0083 1.1057 0.8747 0.054 Uiso 1 1 calc R U . . .
H13B H 0.9620 1.0215 0.8820 0.054 Uiso 1 1 calc R U . . .
H13C H 0.8974 1.0955 0.8979 0.054 Uiso 1 1 calc R U . . .
C14 C 0.5520(2) 0.87818(18) 0.28052(19) 0.0258(7) Uani 1 1 d . . . . .
H14 H 0.6006 0.9204 0.2992 0.031 Uiso 1 1 calc R U . . .
C15 C 0.4860(3) 0.8756(2) 0.1965(2) 0.0360(8) Uani 1 1 d . . . . .
H15 H 0.4893 0.9154 0.1581 0.043 Uiso 1 1 calc R U . . .
C16 C 0.4157(3) 0.8148(2) 0.1690(2) 0.0405(9) Uani 1 1 d . . . . .
H16 H 0.3688 0.8124 0.1115 0.049 Uiso 1 1 calc R U . . .
C17 C 0.4137(3) 0.7567(2) 0.2258(2) 0.0369(9) Uani 1 1 d . . . . .
H17 H 0.3665 0.7136 0.2077 0.044 Uiso 1 1 calc R U . . .
C18 C 0.4818(2) 0.76278(18) 0.30969(19) 0.0258(7) Uani 1 1 d . . . . .
C19 C 0.4831(2) 0.70486(18) 0.3775(2) 0.0263(7) Uani 1 1 d . . . . .
H19A H 0.4242 0.7164 0.4021 0.032 Uiso 1 1 calc R U . . .
H19B H 0.4710 0.6526 0.3527 0.032 Uiso 1 1 calc R U . . .
C20 C 0.6758(2) 0.66866(17) 0.4149(2) 0.0259(7) Uani 1 1 d . . . . .
H20A H 0.6903 0.6174 0.4421 0.031 Uiso 1 1 calc R U . . .
H20B H 0.6461 0.6611 0.3524 0.031 Uiso 1 1 calc R U . . .
C21 C 0.7809(2) 0.71237(17) 0.43615(17) 0.0202(6) Uani 1 1 d . . . . .
C22 C 0.8812(2) 0.67859(18) 0.44328(19) 0.0246(7) Uani 1 1 d . . . . .
H22 H 0.8869 0.6244 0.4396 0.030 Uiso 1 1 calc R U . . .
C23 C 0.9726(2) 0.72439(19) 0.45583(19) 0.0284(7) Uani 1 1 d . . . . .
H23 H 1.0422 0.7023 0.4617 0.034 Uiso 1 1 calc R U . . .
C24 C 0.9608(2) 0.80309(19) 0.4598(2) 0.0287(7) Uani 1 1 d . . . . .
H24 H 1.0218 0.8361 0.4664 0.034 Uiso 1 1 calc R U . . .
C25 C 0.8594(2) 0.83288(18) 0.45387(18) 0.0240(7) Uani 1 1 d . . . . .
H25 H 0.8521 0.8870 0.4572 0.029 Uiso 1 1 calc R U . . .
C26 C 0.5914(2) 0.68016(18) 0.52848(19) 0.0255(7) Uani 1 1 d . . . . .
H26A H 0.5999 0.6236 0.5307 0.031 Uiso 1 1 calc R U . . .
H26B H 0.5206 0.6930 0.5371 0.031 Uiso 1 1 calc R U . . .
C27 C 0.6847(2) 0.71686(18) 0.59695(19) 0.0238(7) Uani 1 1 d . . . . .
C28 C 0.7461(3) 0.6795(2) 0.6707(2) 0.0334(8) Uani 1 1 d . . . . .
H28 H 0.7325 0.6271 0.6800 0.040 Uiso 1 1 calc R U . . .
C29 C 0.8279(3) 0.7203(2) 0.7307(2) 0.0388(9) Uani 1 1 d . . . . .
H29 H 0.8711 0.6961 0.7820 0.047 Uiso 1 1 calc R U . . .
C30 C 0.8461(3) 0.7957(2) 0.7156(2) 0.0335(8) Uani 1 1 d . . . . .
H30 H 0.9013 0.8244 0.7566 0.040 Uiso 1 1 calc R U . . .
C31 C 0.7836(2) 0.82940(19) 0.64072(19) 0.0251(7) Uani 1 1 d . . . . .
H31 H 0.7965 0.8817 0.6306 0.030 Uiso 1 1 calc R U . . .
Cl1 Cl 0.2798(5) 0.9606(3) 0.9629(4) 0.0547(15) Uani 0.5 1 d D U P A 1
O1 O 0.2438(7) 0.8884(3) 0.9921(4) 0.0733(19) Uani 0.5 1 d D U P A 1
O2 O 0.3838(4) 0.9826(3) 1.0171(3) 0.0536(14) Uani 0.5 1 d D U P A 1
O3 O 0.2020(5) 1.0150(3) 0.9728(4) 0.0557(15) Uani 0.5 1 d D U P A 1
O4 O 0.2650(11) 0.9550(5) 0.8747(5) 0.070(3) Uani 0.5 1 d D U P A 1
Cl1' Cl 0.2656(4) 0.9506(3) 0.9543(3) 0.0340(10) Uani 0.5 1 d D U P B 2
O1' O 0.3432(5) 0.8906(3) 0.9707(4) 0.0649(17) Uani 0.5 1 d D U P B 2
O2' O 0.2906(11) 1.0042(5) 1.0183(5) 0.114(3) Uani 0.5 1 d D U P B 2
O3' O 0.2693(10) 0.9906(4) 0.8788(5) 0.054(2) Uani 0.5 1 d D U P B 2
O4' O 0.1593(5) 0.9156(4) 0.9374(5) 0.0836(19) Uani 0.5 1 d D U P B 2
O1W O 0.6444(2) 0.05192(18) 0.25749(18) 0.0598(8) Uani 1 1 d . . . . .
H1WA H 0.6845 0.0710 0.3045 0.072 Uiso 1 1 d R U . . .
H1WB H 0.6831 0.0474 0.2246 0.072 Uiso 1 1 d R U . . .


_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 C3 1.915(3) . ?
Fe1 C2 1.917(3) . ?
Fe1 C1 1.918(3) . ?
Fe1 N6 1.963(2) . ?
Fe1 N8 1.971(2) . ?
Fe1 N4 1.977(2) . ?
Fe2 N1 1.932(3) . ?
Fe2 N2 1.950(2) 3_676 ?
Fe2 N12 1.969(2) . ?
Fe2 N10 1.973(2) . ?
Fe2 N13 1.985(2) . ?
Fe2 N11 1.989(2) . ?
B1 N7 1.553(4) . ?
B1 N5 1.556(4) . ?
B1 N9 1.565(4) . ?
B1 C13 1.583(4) . ?
N1 C1 1.152(4) . ?
N2 C2 1.152(4) . ?
N2 Fe2 1.949(2) 3_676 ?
N3 C3 1.157(4) . ?
N4 C4 1.327(4) . ?
N4 N5 1.361(3) . ?
N5 C6 1.342(4) . ?
N6 C7 1.334(4) . ?
N6 N7 1.364(3) . ?
N7 C9 1.348(4) . ?
N8 C10 1.329(4) . ?
N8 N9 1.359(3) . ?
N9 C12 1.341(4) . ?
N10 C14 1.338(4) . ?
N10 C18 1.353(4) . ?
N11 C26 1.484(4) . ?
N11 C19 1.488(4) . ?
N11 C20 1.493(4) . ?
N12 C25 1.346(4) . ?
N12 C21 1.347(4) . ?
N13 C31 1.348(4) . ?
N13 C27 1.352(4) . ?
C4 C5 1.389(4) . ?
C4 H4 0.9500 . ?
C5 C6 1.377(5) . ?
C5 H5 0.9500 . ?
C6 H6 0.9500 . ?
C7 C8 1.386(4) . ?
C7 H7 0.9500 . ?
C8 C9 1.368(5) . ?
C8 H8 0.9500 . ?
C9 H9 0.9500 . ?
C10 C11 1.391(4) . ?
C10 H10 0.9500 . ?
C11 C12 1.380(5) . ?
C11 H11 0.9500 . ?
C12 H12 0.9500 . ?
C13 H13A 0.9800 . ?
C13 H13B 0.9800 . ?
C13 H13C 0.9800 . ?
C14 C15 1.378(4) . ?
C14 H14 0.9500 . ?
C15 C16 1.371(5) . ?
C15 H15 0.9500 . ?
C16 C17 1.387(5) . ?
C16 H16 0.9500 . ?
C17 C18 1.387(4) . ?
C17 H17 0.9500 . ?
C18 C19 1.504(5) . ?
C19 H19A 0.9900 . ?
C19 H19B 0.9900 . ?
C20 C21 1.490(4) . ?
C20 H20A 0.9900 . ?
C20 H20B 0.9900 . ?
C21 C22 1.386(4) . ?
C22 C23 1.378(4) . ?
C22 H22 0.9500 . ?
C23 C24 1.382(5) . ?
C23 H23 0.9500 . ?
C24 C25 1.376(4) . ?
C24 H24 0.9500 . ?
C25 H25 0.9500 . ?
C26 C27 1.503(4) . ?
C26 H26A 0.9900 . ?
C26 H26B 0.9900 . ?
C27 C28 1.384(4) . ?
C28 C29 1.388(5) . ?
C28 H28 0.9500 . ?
C29 C30 1.371(5) . ?
C29 H29 0.9500 . ?
C30 C31 1.373(4) . ?
C30 H30 0.9500 . ?
C31 H31 0.9500 . ?
Cl1 O2 1.403(7) . ?
Cl1 O4 1.413(7) . ?
Cl1 O3 1.425(7) . ?
Cl1 O1 1.474(7) . ?
Cl1' O2' 1.371(7) . ?
Cl1' O1' 1.408(6) . ?
Cl1' O4' 1.438(7) . ?
Cl1' O3' 1.445(7) . ?
O1W H1WA 0.8499 . ?
O1W H1WB 0.8501 . ?

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
C3 Fe1 C2 89.09(11) . . ?
C3 Fe1 C1 87.45(12) . . ?
C2 Fe1 C1 93.70(11) . . ?
C3 Fe1 N6 94.78(11) . . ?
C2 Fe1 N6 90.43(10) . . ?
C1 Fe1 N6 175.34(11) . . ?
C3 Fe1 N8 94.94(11) . . ?
C2 Fe1 N8 174.74(11) . . ?
C1 Fe1 N8 89.86(10) . . ?
N6 Fe1 N8 85.87(9) . . ?
C3 Fe1 N4 174.71(11) . . ?
C2 Fe1 N4 88.29(10) . . ?
C1 Fe1 N4 88.14(11) . . ?
N6 Fe1 N4 89.84(10) . . ?
N8 Fe1 N4 87.96(9) . . ?
N1 Fe2 N2 87.17(10) . 3_676 ?
N1 Fe2 N12 94.77(10) . . ?
N2 Fe2 N12 177.82(10) 3_676 . ?
N1 Fe2 N10 98.73(10) . . ?
N2 Fe2 N10 87.08(10) 3_676 . ?
N12 Fe2 N10 93.60(9) . . ?
N1 Fe2 N13 95.05(10) . . ?
N2 Fe2 N13 94.14(9) 3_676 . ?
N12 Fe2 N13 84.70(9) . . ?
N10 Fe2 N13 166.21(10) . . ?
N1 Fe2 N11 178.98(10) . . ?
N2 Fe2 N11 93.25(10) 3_676 . ?
N12 Fe2 N11 84.79(10) . . ?
N10 Fe2 N11 82.22(10) . . ?
N13 Fe2 N11 84.00(10) . . ?
N7 B1 N5 106.3(2) . . ?
N7 B1 N9 104.7(2) . . ?
N5 B1 N9 105.4(2) . . ?
N7 B1 C13 113.6(3) . . ?
N5 B1 C13 112.8(3) . . ?
N9 B1 C13 113.1(3) . . ?
C1 N1 Fe2 164.3(2) . . ?
C2 N2 Fe2 161.4(2) . 3_676 ?
C4 N4 N5 107.2(2) . . ?
C4 N4 Fe1 131.8(2) . . ?
N5 N4 Fe1 120.91(17) . . ?
C6 N5 N4 109.1(2) . . ?
C6 N5 B1 132.0(3) . . ?
N4 N5 B1 118.8(2) . . ?
C7 N6 N7 106.9(2) . . ?
C7 N6 Fe1 132.8(2) . . ?
N7 N6 Fe1 120.32(17) . . ?
C9 N7 N6 108.9(2) . . ?
C9 N7 B1 131.4(3) . . ?
N6 N7 B1 119.5(2) . . ?
C10 N8 N9 107.2(2) . . ?
C10 N8 Fe1 132.6(2) . . ?
N9 N8 Fe1 120.16(17) . . ?
C12 N9 N8 109.2(2) . . ?
C12 N9 B1 131.1(3) . . ?
N8 N9 B1 119.7(2) . . ?
C14 N10 C18 118.7(3) . . ?
C14 N10 Fe2 128.2(2) . . ?
C18 N10 Fe2 113.1(2) . . ?
C26 N11 C19 112.9(2) . . ?
C26 N11 C20 111.5(2) . . ?
C19 N11 C20 109.5(2) . . ?
C26 N11 Fe2 106.84(17) . . ?
C19 N11 Fe2 106.62(18) . . ?
C20 N11 Fe2 109.29(18) . . ?
C25 N12 C21 117.7(2) . . ?
C25 N12 Fe2 126.7(2) . . ?
C21 N12 Fe2 114.52(19) . . ?
C31 N13 C27 118.5(3) . . ?
C31 N13 Fe2 127.6(2) . . ?
C27 N13 Fe2 112.71(19) . . ?
N1 C1 Fe1 169.4(2) . . ?
N2 C2 Fe1 168.6(2) . . ?
N3 C3 Fe1 176.2(3) . . ?
N4 C4 C5 110.1(3) . . ?
N4 C4 H4 124.9 . . ?
C5 C4 H4 124.9 . . ?
C6 C5 C4 105.0(3) . . ?
C6 C5 H5 127.5 . . ?
C4 C5 H5 127.5 . . ?
N5 C6 C5 108.5(3) . . ?
N5 C6 H6 125.7 . . ?
C5 C6 H6 125.7 . . ?
N6 C7 C8 110.2(3) . . ?
N6 C7 H7 124.9 . . ?
C8 C7 H7 124.9 . . ?
C9 C8 C7 105.1(3) . . ?
C9 C8 H8 127.4 . . ?
C7 C8 H8 127.4 . . ?
N7 C9 C8 108.9(3) . . ?
N7 C9 H9 125.6 . . ?
C8 C9 H9 125.6 . . ?
N8 C10 C11 110.2(3) . . ?
N8 C10 H10 124.9 . . ?
C11 C10 H10 124.9 . . ?
C12 C11 C10 104.7(3) . . ?
C12 C11 H11 127.6 . . ?
C10 C11 H11 127.6 . . ?
N9 C12 C11 108.7(3) . . ?
N9 C12 H12 125.7 . . ?
C11 C12 H12 125.7 . . ?
B1 C13 H13A 109.5 . . ?
B1 C13 H13B 109.5 . . ?
H13A C13 H13B 109.5 . . ?
B1 C13 H13C 109.5 . . ?
H13A C13 H13C 109.5 . . ?
H13B C13 H13C 109.5 . . ?
N10 C14 C15 122.5(3) . . ?
N10 C14 H14 118.8 . . ?
C15 C14 H14 118.8 . . ?
C16 C15 C14 119.1(3) . . ?
C16 C15 H15 120.5 . . ?
C14 C15 H15 120.5 . . ?
C15 C16 C17 119.4(3) . . ?
C15 C16 H16 120.3 . . ?
C17 C16 H16 120.3 . . ?
C16 C17 C18 118.7(3) . . ?
C16 C17 H17 120.7 . . ?
C18 C17 H17 120.7 . . ?
N10 C18 C17 121.7(3) . . ?
N10 C18 C19 115.1(3) . . ?
C17 C18 C19 123.2(3) . . ?
N11 C19 C18 107.6(2) . . ?
N11 C19 H19A 110.2 . . ?
C18 C19 H19A 110.2 . . ?
N11 C19 H19B 110.2 . . ?
C18 C19 H19B 110.2 . . ?
H19A C19 H19B 108.5 . . ?
C21 C20 N11 111.7(2) . . ?
C21 C20 H20A 109.3 . . ?
N11 C20 H20A 109.3 . . ?
C21 C20 H20B 109.3 . . ?
N11 C20 H20B 109.3 . . ?
H20A C20 H20B 107.9 . . ?
N12 C21 C22 122.2(3) . . ?
N12 C21 C20 114.3(2) . . ?
C22 C21 C20 123.4(3) . . ?
C23 C22 C21 119.4(3) . . ?
C23 C22 H22 120.3 . . ?
C21 C22 H22 120.3 . . ?
C22 C23 C24 118.7(3) . . ?
C22 C23 H23 120.7 . . ?
C24 C23 H23 120.7 . . ?
C25 C24 C23 119.1(3) . . ?
C25 C24 H24 120.5 . . ?
C23 C24 H24 120.5 . . ?
N12 C25 C24 122.9(3) . . ?
N12 C25 H25 118.5 . . ?
C24 C25 H25 118.5 . . ?
N11 C26 C27 108.3(2) . . ?
N11 C26 H26A 110.0 . . ?
C27 C26 H26A 110.0 . . ?
N11 C26 H26B 110.0 . . ?
C27 C26 H26B 110.0 . . ?
H26A C26 H26B 108.4 . . ?
N13 C27 C28 121.9(3) . . ?
N13 C27 C26 114.3(3) . . ?
C28 C27 C26 123.8(3) . . ?
C27 C28 C29 118.4(3) . . ?
C27 C28 H28 120.8 . . ?
C29 C28 H28 120.8 . . ?
C30 C29 C28 119.6(3) . . ?
C30 C29 H29 120.2 . . ?
C28 C29 H29 120.2 . . ?
C29 C30 C31 119.3(3) . . ?
C29 C30 H30 120.4 . . ?
C31 C30 H30 120.4 . . ?
N13 C31 C30 122.2(3) . . ?
N13 C31 H31 118.9 . . ?
C30 C31 H31 118.9 . . ?
O2 Cl1 O4 117.7(7) . . ?
O2 Cl1 O3 107.6(5) . . ?
O4 Cl1 O3 107.4(7) . . ?
O2 Cl1 O1 111.0(6) . . ?
O4 Cl1 O1 109.2(6) . . ?
O3 Cl1 O1 102.9(6) . . ?
O2' Cl1' O1' 112.4(7) . . ?
O2' Cl1' O4' 114.2(7) . . ?
O1' Cl1' O4' 107.0(5) . . ?
O2' Cl1' O3' 105.9(6) . . ?
O1' Cl1' O3' 107.9(6) . . ?
O4' Cl1' O3' 109.2(7) . . ?
H1WA O1W H1WB 108.3 . . ?

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
C4 N4 N5 C6 -0.6(3) . . . . ?
Fe1 N4 N5 C6 -179.1(2) . . . . ?
C4 N4 N5 B1 178.4(2) . . . . ?
Fe1 N4 N5 B1 -0.2(3) . . . . ?
N7 B1 N5 C6 -126.1(3) . . . . ?
N9 B1 N5 C6 123.0(3) . . . . ?
C13 B1 N5 C6 -0.9(5) . . . . ?
N7 B1 N5 N4 55.2(3) . . . . ?
N9 B1 N5 N4 -55.6(3) . . . . ?
C13 B1 N5 N4 -179.6(2) . . . . ?
C7 N6 N7 C9 0.8(3) . . . . ?
Fe1 N6 N7 C9 -178.31(19) . . . . ?
C7 N6 N7 B1 -174.4(2) . . . . ?
Fe1 N6 N7 B1 6.5(3) . . . . ?
N5 B1 N7 C9 126.7(3) . . . . ?
N9 B1 N7 C9 -121.9(3) . . . . ?
C13 B1 N7 C9 2.0(5) . . . . ?
N5 B1 N7 N6 -59.3(3) . . . . ?
N9 B1 N7 N6 52.0(3) . . . . ?
C13 B1 N7 N6 175.9(2) . . . . ?
C10 N8 N9 C12 0.2(3) . . . . ?
Fe1 N8 N9 C12 179.3(2) . . . . ?
C10 N8 N9 B1 -180.0(3) . . . . ?
Fe1 N8 N9 B1 -0.9(3) . . . . ?
N7 B1 N9 C12 124.5(3) . . . . ?
N5 B1 N9 C12 -123.5(3) . . . . ?
C13 B1 N9 C12 0.2(5) . . . . ?
N7 B1 N9 N8 -55.3(3) . . . . ?
N5 B1 N9 N8 56.7(3) . . . . ?
C13 B1 N9 N8 -179.6(3) . . . . ?
Fe2 N1 C1 Fe1 35.7(19) . . . . ?
Fe2 N2 C2 Fe1 -22.3(19) 3_676 . . . ?
N5 N4 C4 C5 0.4(3) . . . . ?
Fe1 N4 C4 C5 178.7(2) . . . . ?
N4 C4 C5 C6 -0.1(3) . . . . ?
N4 N5 C6 C5 0.5(3) . . . . ?
B1 N5 C6 C5 -178.3(3) . . . . ?
C4 C5 C6 N5 -0.2(3) . . . . ?
N7 N6 C7 C8 -0.9(3) . . . . ?
Fe1 N6 C7 C8 178.1(2) . . . . ?
N6 C7 C8 C9 0.6(3) . . . . ?
N6 N7 C9 C8 -0.4(3) . . . . ?
B1 N7 C9 C8 174.0(3) . . . . ?
C7 C8 C9 N7 -0.1(3) . . . . ?
N9 N8 C10 C11 0.0(3) . . . . ?
Fe1 N8 C10 C11 -179.0(2) . . . . ?
N8 C10 C11 C12 -0.1(4) . . . . ?
N8 N9 C12 C11 -0.3(4) . . . . ?
B1 N9 C12 C11 179.9(3) . . . . ?
C10 C11 C12 N9 0.2(4) . . . . ?
C18 N10 C14 C15 0.9(4) . . . . ?
Fe2 N10 C14 C15 -175.9(2) . . . . ?
N10 C14 C15 C16 0.0(5) . . . . ?
C14 C15 C16 C17 -1.0(5) . . . . ?
C15 C16 C17 C18 1.2(5) . . . . ?
C14 N10 C18 C17 -0.7(4) . . . . ?
Fe2 N10 C18 C17 176.6(2) . . . . ?
C14 N10 C18 C19 -178.7(2) . . . . ?
Fe2 N10 C18 C19 -1.5(3) . . . . ?
C16 C17 C18 N10 -0.4(5) . . . . ?
C16 C17 C18 C19 177.5(3) . . . . ?
C26 N11 C19 C18 157.2(2) . . . . ?
C20 N11 C19 C18 -77.9(3) . . . . ?
Fe2 N11 C19 C18 40.2(2) . . . . ?
N10 C18 C19 N11 -26.2(3) . . . . ?
C17 C18 C19 N11 155.8(3) . . . . ?
C26 N11 C20 C21 -96.7(3) . . . . ?
C19 N11 C20 C21 137.7(3) . . . . ?
Fe2 N11 C20 C21 21.2(3) . . . . ?
C25 N12 C21 C22 3.5(4) . . . . ?
Fe2 N12 C21 C22 -165.2(2) . . . . ?
C25 N12 C21 C20 -173.3(3) . . . . ?
Fe2 N12 C21 C20 18.0(3) . . . . ?
N11 C20 C21 N12 -26.2(4) . . . . ?
N11 C20 C21 C22 157.2(3) . . . . ?
N12 C21 C22 C23 -2.0(4) . . . . ?
C20 C21 C22 C23 174.4(3) . . . . ?
C21 C22 C23 C24 -0.9(4) . . . . ?
C22 C23 C24 C25 2.1(5) . . . . ?
C21 N12 C25 C24 -2.1(4) . . . . ?
Fe2 N12 C25 C24 165.0(2) . . . . ?
C23 C24 C25 N12 -0.6(5) . . . . ?
C19 N11 C26 C27 -155.8(2) . . . . ?
C20 N11 C26 C27 80.4(3) . . . . ?
Fe2 N11 C26 C27 -39.0(3) . . . . ?
C31 N13 C27 C28 -3.0(4) . . . . ?
Fe2 N13 C27 C28 165.6(2) . . . . ?
C31 N13 C27 C26 176.9(2) . . . . ?
Fe2 N13 C27 C26 -14.5(3) . . . . ?
N11 C26 C27 N13 36.1(3) . . . . ?
N11 C26 C27 C28 -144.0(3) . . . . ?
N13 C27 C28 C29 2.1(5) . . . . ?
C26 C27 C28 C29 -177.8(3) . . . . ?
C27 C28 C29 C30 -0.2(5) . . . . ?
C28 C29 C30 C31 -0.7(5) . . . . ?
C27 N13 C31 C30 2.0(4) . . . . ?
Fe2 N13 C31 C30 -164.6(2) . . . . ?
C29 C30 C31 N13 -0.1(5) . . . . ?

_refine_diff_density_max         0.471
_refine_diff_density_min         -0.551
_refine_diff_density_rms         0.072

####################################################################### 
# 
# 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_3_H2O-296K
_database_code_depnum_ccdc_archive 'CCDC 1419292'
_audit_update_record             
;
2016-09-02 deposited with the CCDC.
2016-09-26 downloaded from the CCDC.
;

_audit_creation_method           SHELXL-2014/7
_shelx_SHELXL_version_number     2014/7
_chemical_name_systematic        ?
_chemical_name_common            ?
_chemical_melting_point          ?
_chemical_formula_moiety         'C62 H60 B2 Fe4 N26, 2(Cl O4), 2(H2 O)'
_chemical_formula_sum            'C62 H64 B2 Cl2 Fe4 N26 O10'
_chemical_formula_weight         1649.31

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'
O O 0.0106 0.0060 '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'

_space_group_crystal_system      monoclinic
_space_group_IT_number           14
_space_group_name_H-M_alt        'P 21/c'
_space_group_name_Hall           '-P 2ybc'

_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.
;

loop_
_space_group_symop_operation_xyz
'x, y, z'
'-x, y+1/2, -z+1/2'
'-x, -y, -z'
'x, -y-1/2, z-1/2'

_cell_length_a                   12.9516(12)
_cell_length_b                   17.5832(16)
_cell_length_c                   16.7140(15)
_cell_angle_alpha                90
_cell_angle_beta                 108.4290(10)
_cell_angle_gamma                90
_cell_volume                     3611.1(6)
_cell_formula_units_Z            2
_cell_measurement_temperature    296(2)
_cell_measurement_reflns_used    6294
_cell_measurement_theta_min      2.32
_cell_measurement_theta_max      24.99

_exptl_crystal_description       block
_exptl_crystal_colour            red
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    'not measured'
_exptl_crystal_density_diffrn    1.517
_exptl_crystal_F_000             1692
_exptl_transmission_factor_min   ?
_exptl_transmission_factor_max   ?
_exptl_crystal_size_max          0.100
_exptl_crystal_size_mid          0.050
_exptl_crystal_size_min          0.050
_exptl_absorpt_coefficient_mu    0.937
_shelx_estimated_absorpt_T_min   0.912
_shelx_estimated_absorpt_T_max   0.955
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_correction_T_min  0.9121
_exptl_absorpt_correction_T_max  0.9546
_exptl_absorpt_process_details   sadabs
_exptl_absorpt_special_details   ?
_diffrn_ambient_temperature      296(2)
_diffrn_radiation_wavelength     0.71073
_diffrn_radiation_type           MoK\a
_diffrn_source                   ?
_diffrn_measurement_device_type  'Bruker APEX-II CCD'
_diffrn_measurement_method       'φ and ω scans'
_diffrn_detector_area_resol_mean ?
_diffrn_reflns_number            25140
_diffrn_reflns_av_unetI/netI     0.0380
_diffrn_reflns_av_R_equivalents  0.0408
_diffrn_reflns_limit_h_min       -15
_diffrn_reflns_limit_h_max       15
_diffrn_reflns_limit_k_min       -20
_diffrn_reflns_limit_k_max       20
_diffrn_reflns_limit_l_min       -19
_diffrn_reflns_limit_l_max       18
_diffrn_reflns_theta_min         1.657
_diffrn_reflns_theta_max         24.998
_diffrn_reflns_theta_full        24.998
_diffrn_measured_fraction_theta_max 0.996
_diffrn_measured_fraction_theta_full 0.996
_diffrn_reflns_Laue_measured_fraction_max 0.996
_diffrn_reflns_Laue_measured_fraction_full 0.996
_diffrn_reflns_point_group_measured_fraction_max 0.996
_diffrn_reflns_point_group_measured_fraction_full 0.996
_reflns_number_total             6330
_reflns_number_gt                4901
_reflns_threshold_expression     'I > 2σ(I)'
_reflns_Friedel_coverage         0.000
_reflns_Friedel_fraction_max     .
_reflns_Friedel_fraction_full    .

_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.
;

_computing_data_collection       'Bruker APEX2'
_computing_cell_refinement       'Bruker SAINT'
_computing_data_reduction        'Bruker SAINT'
_computing_structure_solution    'SHELXS-2014 (Sheldrick, 2014)'
_computing_structure_refinement  'SHELXL-2014/7 (Sheldrick, 2014)'
_computing_molecular_graphics    'Bruker SHELXTL'
_computing_publication_material  'Bruker SHELXTL'
_refine_special_details          ?
_refine_ls_structure_factor_coef Fsqd
_refine_ls_matrix_type           full
_refine_ls_weighting_scheme      calc
_refine_ls_weighting_details     
'w=1/[σ²(Fo²)+(0.0637P)²+2.5141P] where P=(Fo²+2Fc²)/3'
_atom_sites_solution_primary     ?
_atom_sites_solution_secondary   ?
_atom_sites_solution_hydrogens   mixed
_refine_ls_hydrogen_treatment    constr
_refine_ls_extinction_method     none
_refine_ls_extinction_coef       .
_refine_ls_number_reflns         6330
_refine_ls_number_parameters     525
_refine_ls_number_restraints     194
_refine_ls_R_factor_all          0.0586
_refine_ls_R_factor_gt           0.0409
_refine_ls_wR_factor_ref         0.1238
_refine_ls_wR_factor_gt          0.1093
_refine_ls_goodness_of_fit_ref   1.048
_refine_ls_restrained_S_all      1.097
_refine_ls_shift/su_max          0.001
_refine_ls_shift/su_mean         0.000

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 0.73810(3) 1.07862(2) 0.57163(3) 0.03194(14) Uani 1 1 d . . . . .
Fe2 Fe 0.62749(4) 0.82140(2) 0.46074(3) 0.03364(14) Uani 1 1 d . . . . .
B1 B 0.8710(4) 1.0744(2) 0.7642(3) 0.0511(10) Uani 1 1 d . . . . .
N1 N 0.6691(2) 0.93004(17) 0.47414(18) 0.0467(7) Uani 1 1 d . . . . .
N2 N 0.5126(2) 1.15116(15) 0.51797(18) 0.0444(7) Uani 1 1 d . . . . .
N3 N 0.7876(3) 1.1450(2) 0.4183(2) 0.0689(10) Uani 1 1 d . . . . .
N4 N 0.6942(2) 1.02984(15) 0.66250(16) 0.0380(6) Uani 1 1 d . . . . .
N5 N 0.7593(2) 1.03296(16) 0.74367(17) 0.0446(7) Uani 1 1 d . . . . .
N6 N 0.7932(2) 1.16683(15) 0.64560(17) 0.0396(6) Uani 1 1 d . . . . .
N7 N 0.8453(2) 1.15604(17) 0.72924(18) 0.0464(7) Uani 1 1 d . . . . .
N8 N 0.8840(2) 1.03398(15) 0.62265(17) 0.0395(6) Uani 1 1 d . . . . .
N9 N 0.9315(2) 1.03595(17) 0.70775(18) 0.0469(7) Uani 1 1 d . . . . .
N10 N 0.5422(2) 0.81727(17) 0.33542(18) 0.0476(7) Uani 1 1 d . . . . .
N11 N 0.5920(2) 0.70639(15) 0.44681(18) 0.0414(6) Uani 1 1 d . . . . .
N12 N 0.7693(2) 0.78631(15) 0.44262(17) 0.0409(6) Uani 1 1 d . . . . .
N13 N 0.7033(2) 0.78823(17) 0.58323(18) 0.0448(7) Uani 1 1 d . . . . .
C1 C 0.6913(2) 0.98887(19) 0.5046(2) 0.0378(7) Uani 1 1 d . . . . .
C2 C 0.5970(3) 1.12409(17) 0.53066(19) 0.0358(7) Uani 1 1 d . . . . .
C3 C 0.7710(3) 1.1218(2) 0.4766(2) 0.0435(8) Uani 1 1 d . . . . .
C4 C 0.6068(3) 0.98992(19) 0.6618(2) 0.0466(8) Uani 1 1 d . . . . .
H4 H 0.5486 0.9792 0.6138 0.056 Uiso 1 1 calc R U . . .
C5 C 0.6142(4) 0.9670(2) 0.7413(3) 0.0631(11) Uani 1 1 d . . . . .
H5 H 0.5640 0.9383 0.7577 0.076 Uiso 1 1 calc R U . . .
C6 C 0.7114(4) 0.9951(2) 0.7917(3) 0.0598(11) Uani 1 1 d . . . . .
H6 H 0.7395 0.9890 0.8499 0.072 Uiso 1 1 calc R U . . .
C7 C 0.7893(3) 1.24156(19) 0.6315(3) 0.0507(9) Uani 1 1 d . . . . .
H7 H 0.7583 1.2644 0.5792 0.061 Uiso 1 1 calc R U . . .
C8 C 0.8377(4) 1.2798(2) 0.7056(3) 0.0663(12) Uani 1 1 d . . . . .
H8 H 0.8457 1.3321 0.7134 0.080 Uiso 1 1 calc R U . . .
C9 C 0.8713(4) 1.2244(2) 0.7652(3) 0.0635(11) Uani 1 1 d . . . . .
H9 H 0.9069 1.2328 0.8222 0.076 Uiso 1 1 calc R U . . .
C10 C 0.9519(3) 0.9983(2) 0.5905(3) 0.0518(9) Uani 1 1 d . . . . .
H10 H 0.9392 0.9895 0.5334 0.062 Uiso 1 1 calc R U . . .
C11 C 1.0441(4) 0.9761(3) 0.6539(3) 0.0744(13) Uani 1 1 d . . . . .
H11 H 1.1038 0.9498 0.6484 0.089 Uiso 1 1 calc R U . . .
C12 C 1.0282(3) 1.0014(2) 0.7271(3) 0.0658(12) Uani 1 1 d . . . . .
H12 H 1.0769 0.9954 0.7811 0.079 Uiso 1 1 calc R U . . .
C13 C 0.9391(4) 1.0718(3) 0.8618(3) 0.0771(14) Uani 1 1 d . . . . .
H13A H 1.0037 1.1020 0.8719 0.116 Uiso 1 1 calc R U . . .
H13B H 0.9589 1.0202 0.8784 0.116 Uiso 1 1 calc R U . . .
H13C H 0.8957 1.0917 0.8942 0.116 Uiso 1 1 calc R U . . .
C14 C 0.5391(4) 0.8700(3) 0.2779(3) 0.0676(12) Uani 1 1 d . . . . .
H14 H 0.5828 0.9129 0.2935 0.081 Uiso 1 1 calc R U . . .
C15 C 0.4719(5) 0.8627(4) 0.1948(3) 0.0960(18) Uani 1 1 d . U . . .
H15 H 0.4707 0.9003 0.1554 0.115 Uiso 1 1 calc R U . . .
C16 C 0.4098(5) 0.8014(5) 0.1724(3) 0.106(2) Uani 1 1 d . U . . .
H16 H 0.3642 0.7964 0.1171 0.127 Uiso 1 1 calc R U . . .
C17 C 0.4119(4) 0.7446(3) 0.2305(3) 0.0848(16) Uani 1 1 d . . . . .
H17 H 0.3696 0.7010 0.2149 0.102 Uiso 1 1 calc R U . . .
C18 C 0.4792(3) 0.7550(2) 0.3121(2) 0.0555(10) Uani 1 1 d . . . . .
C19 C 0.4838(3) 0.7001(2) 0.3812(3) 0.0550(10) Uani 1 1 d . . . . .
H19A H 0.4267 0.7115 0.4056 0.066 Uiso 1 1 calc R U . . .
H19B H 0.4728 0.6487 0.3590 0.066 Uiso 1 1 calc R U . . .
C20 C 0.6760(3) 0.66682(19) 0.4180(3) 0.0517(9) Uani 1 1 d . . . . .
H20A H 0.6909 0.6174 0.4449 0.062 Uiso 1 1 calc R U . . .
H20B H 0.6474 0.6587 0.3576 0.062 Uiso 1 1 calc R U . . .
C21 C 0.7797(3) 0.71062(19) 0.4377(2) 0.0410(8) Uani 1 1 d . . . . .
C22 C 0.8783(3) 0.6763(2) 0.4459(2) 0.0556(10) Uani 1 1 d . . . . .
H22 H 0.8836 0.6237 0.4439 0.067 Uiso 1 1 calc R U . . .
C23 C 0.9685(3) 0.7213(3) 0.4570(3) 0.0700(12) Uani 1 1 d . . . . .
H23 H 1.0361 0.6996 0.4630 0.084 Uiso 1 1 calc R U . . .
C24 C 0.9573(4) 0.7985(3) 0.4589(3) 0.0718(12) Uani 1 1 d . . . . .
H24 H 1.0169 0.8300 0.4649 0.086 Uiso 1 1 calc R U . . .
C25 C 0.8582(3) 0.8291(2) 0.4521(3) 0.0580(10) Uani 1 1 d . . . . .
H25 H 0.8519 0.8817 0.4540 0.070 Uiso 1 1 calc R U . . .
C26 C 0.5923(4) 0.6787(2) 0.5306(2) 0.0578(10) Uani 1 1 d . . . . .
H26A H 0.6008 0.6239 0.5335 0.069 Uiso 1 1 calc R U . . .
H26B H 0.5238 0.6913 0.5394 0.069 Uiso 1 1 calc R U . . .
C27 C 0.6842(3) 0.7152(2) 0.5976(2) 0.0555(10) Uani 1 1 d . . . . .
C28 C 0.7456(5) 0.6777(3) 0.6704(3) 0.0868(16) Uani 1 1 d . . . . .
H28 H 0.7333 0.6267 0.6792 0.104 Uiso 1 1 calc R U . . .
C29 C 0.8255(5) 0.7188(4) 0.7291(3) 0.0986(18) Uani 1 1 d . . . . .
H29 H 0.8670 0.6954 0.7788 0.118 Uiso 1 1 calc R U . . .
C30 C 0.8441(4) 0.7923(3) 0.7154(3) 0.0800(14) Uani 1 1 d . . . . .
H30 H 0.8981 0.8198 0.7548 0.096 Uiso 1 1 calc R U . . .
C31 C 0.7815(3) 0.8255(2) 0.6421(2) 0.0580(10) Uani 1 1 d . . . . .
H31 H 0.7939 0.8763 0.6327 0.070 Uiso 1 1 calc R U . . .
Cl1 Cl 0.2743(8) 0.9553(5) 0.9590(6) 0.0970(19) Uani 0.587(6) 1 d . U P A 1
O1 O 0.3746(7) 0.9822(5) 1.0198(5) 0.129(3) Uani 0.587(6) 1 d . U P A 1
O2 O 0.2632(11) 0.9462(6) 0.8777(6) 0.132(3) Uani 0.587(6) 1 d . U P A 1
O3 O 0.1997(8) 1.0093(6) 0.9675(7) 0.141(3) Uani 0.587(6) 1 d . U P A 1
O4 O 0.2530(11) 0.8837(5) 0.9946(6) 0.143(3) Uani 0.587(6) 1 d . U P A 1
Cl1' Cl 0.2630(10) 0.9484(7) 0.9594(8) 0.0718(17) Uani 0.413(6) 1 d . U P A 2
O1' O 0.1504(10) 0.9138(7) 0.9333(9) 0.132(3) Uani 0.413(6) 1 d . U P A 2
O2' O 0.2709(15) 0.9900(8) 0.8848(9) 0.128(4) Uani 0.413(6) 1 d . U P A 2
O3' O 0.2531(15) 1.0023(8) 1.0092(8) 0.136(4) Uani 0.413(6) 1 d . U P A 2
O4' O 0.3350(11) 0.8900(6) 0.9767(8) 0.115(3) Uani 0.413(6) 1 d . U P A 2
O1W O 0.3450(6) 0.9585(5) 0.7396(5) 0.226(3) Uani 1 1 d . . . . .
H1WA H 0.3431 0.9616 0.7886 0.339 Uiso 1 1 d R U . . .
H1WB H 0.2977 0.9284 0.7117 0.339 Uiso 1 1 d R U . . .


_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 C2 1.913(3) . ?
Fe1 C1 1.920(3) . ?
Fe1 C3 1.926(4) . ?
Fe1 N6 1.971(3) . ?
Fe1 N8 1.973(3) . ?
Fe1 N4 1.977(3) . ?
Fe2 N1 1.978(3) . ?
Fe2 N2 2.015(3) 3_676 ?
Fe2 N10 2.037(3) . ?
Fe2 N12 2.049(3) . ?
Fe2 N13 2.055(3) . ?
Fe2 N11 2.071(3) . ?
B1 N7 1.545(5) . ?
B1 N9 1.558(5) . ?
B1 N5 1.559(5) . ?
B1 C13 1.592(6) . ?
N1 C1 1.148(4) . ?
N2 C2 1.149(4) . ?
N2 Fe2 2.015(3) 3_676 ?
N3 C3 1.137(4) . ?
N4 C4 1.330(4) . ?
N4 N5 1.353(4) . ?
N5 C6 1.337(5) . ?
N6 C7 1.333(4) . ?
N6 N7 1.360(4) . ?
N7 C9 1.338(5) . ?
N8 C10 1.325(4) . ?
N8 N9 1.360(4) . ?
N9 C12 1.337(5) . ?
N10 C14 1.326(5) . ?
N10 C18 1.347(5) . ?
N11 C26 1.482(5) . ?
N11 C19 1.485(5) . ?
N11 C20 1.493(4) . ?
N12 C25 1.342(5) . ?
N12 C21 1.343(4) . ?
N13 C31 1.339(5) . ?
N13 C27 1.343(5) . ?
C4 C5 1.363(5) . ?
C4 H4 0.9300 . ?
C5 C6 1.367(6) . ?
C5 H5 0.9300 . ?
C6 H6 0.9300 . ?
C7 C8 1.374(6) . ?
C7 H7 0.9300 . ?
C8 C9 1.362(6) . ?
C8 H8 0.9300 . ?
C9 H9 0.9300 . ?
C10 C11 1.378(6) . ?
C10 H10 0.9300 . ?
C11 C12 1.377(6) . ?
C11 H11 0.9300 . ?
C12 H12 0.9300 . ?
C13 H13A 0.9600 . ?
C13 H13B 0.9600 . ?
C13 H13C 0.9600 . ?
C14 C15 1.393(7) . ?
C14 H14 0.9300 . ?
C15 C16 1.326(9) . ?
C15 H15 0.9300 . ?
C16 C17 1.387(9) . ?
C16 H16 0.9300 . ?
C17 C18 1.380(6) . ?
C17 H17 0.9300 . ?
C18 C19 1.492(6) . ?
C19 H19A 0.9700 . ?
C19 H19B 0.9700 . ?
C20 C21 1.493(5) . ?
C20 H20A 0.9700 . ?
C20 H20B 0.9700 . ?
C21 C22 1.379(5) . ?
C22 C23 1.374(6) . ?
C22 H22 0.9300 . ?
C23 C24 1.367(6) . ?
C23 H23 0.9300 . ?
C24 C25 1.362(6) . ?
C24 H24 0.9300 . ?
C25 H25 0.9300 . ?
C26 C27 1.495(6) . ?
C26 H26A 0.9700 . ?
C26 H26B 0.9700 . ?
C27 C28 1.392(6) . ?
C28 C29 1.385(8) . ?
C28 H28 0.9300 . ?
C29 C30 1.347(8) . ?
C29 H29 0.9300 . ?
C30 C31 1.368(6) . ?
C30 H30 0.9300 . ?
C31 H31 0.9300 . ?
Cl1 O2 1.329(13) . ?
Cl1 O3 1.394(14) . ?
Cl1 O1 1.452(13) . ?
Cl1 O4 1.456(12) . ?
Cl1' O3' 1.293(18) . ?
Cl1' O4' 1.356(16) . ?
Cl1' O2' 1.477(17) . ?
Cl1' O1' 1.513(18) . ?
O1W H1WA 0.8282 . ?
O1W H1WB 0.8326 . ?

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
C2 Fe1 C1 92.58(13) . . ?
C2 Fe1 C3 88.59(14) . . ?
C1 Fe1 C3 87.35(14) . . ?
C2 Fe1 N6 90.65(12) . . ?
C1 Fe1 N6 176.38(12) . . ?
C3 Fe1 N6 94.39(13) . . ?
C2 Fe1 N8 175.62(12) . . ?
C1 Fe1 N8 90.44(12) . . ?
C3 Fe1 N8 94.72(13) . . ?
N6 Fe1 N8 86.25(11) . . ?
C2 Fe1 N4 88.98(12) . . ?
C1 Fe1 N4 88.71(12) . . ?
C3 Fe1 N4 175.28(13) . . ?
N6 Fe1 N4 89.69(11) . . ?
N8 Fe1 N4 87.92(11) . . ?
N1 Fe2 N2 88.69(11) . 3_676 ?
N1 Fe2 N10 100.98(12) . . ?
N2 Fe2 N10 87.97(12) 3_676 . ?
N1 Fe2 N12 94.74(11) . . ?
N2 Fe2 N12 176.06(11) 3_676 . ?
N10 Fe2 N12 93.28(11) . . ?
N1 Fe2 N13 97.71(12) . . ?
N2 Fe2 N13 93.73(11) 3_676 . ?
N10 Fe2 N13 161.27(12) . . ?
N12 Fe2 N13 83.90(11) . . ?
N1 Fe2 N11 177.06(11) . . ?
N2 Fe2 N11 94.21(11) 3_676 . ?
N10 Fe2 N11 79.67(12) . . ?
N12 Fe2 N11 82.35(11) . . ?
N13 Fe2 N11 81.61(11) . . ?
N7 B1 N9 105.3(3) . . ?
N7 B1 N5 106.1(3) . . ?
N9 B1 N5 105.9(3) . . ?
N7 B1 C13 113.4(3) . . ?
N9 B1 C13 112.7(3) . . ?
N5 B1 C13 112.7(4) . . ?
C1 N1 Fe2 160.2(3) . . ?
C2 N2 Fe2 157.5(3) . 3_676 ?
C4 N4 N5 106.8(3) . . ?
C4 N4 Fe1 132.3(2) . . ?
N5 N4 Fe1 120.9(2) . . ?
C6 N5 N4 108.8(3) . . ?
C6 N5 B1 132.5(3) . . ?
N4 N5 B1 118.7(3) . . ?
C7 N6 N7 107.4(3) . . ?
C7 N6 Fe1 132.7(3) . . ?
N7 N6 Fe1 119.9(2) . . ?
C9 N7 N6 108.0(3) . . ?
C9 N7 B1 132.1(3) . . ?
N6 N7 B1 119.7(3) . . ?
C10 N8 N9 107.3(3) . . ?
C10 N8 Fe1 132.9(3) . . ?
N9 N8 Fe1 119.8(2) . . ?
C12 N9 N8 108.7(3) . . ?
C12 N9 B1 131.6(3) . . ?
N8 N9 B1 119.7(3) . . ?
C14 N10 C18 118.8(4) . . ?
C14 N10 Fe2 127.0(3) . . ?
C18 N10 Fe2 114.1(2) . . ?
C26 N11 C19 113.2(3) . . ?
C26 N11 C20 111.5(3) . . ?
C19 N11 C20 109.9(3) . . ?
C26 N11 Fe2 106.3(2) . . ?
C19 N11 Fe2 106.3(2) . . ?
C20 N11 Fe2 109.4(2) . . ?
C25 N12 C21 117.7(3) . . ?
C25 N12 Fe2 126.1(2) . . ?
C21 N12 Fe2 114.8(2) . . ?
C31 N13 C27 118.4(3) . . ?
C31 N13 Fe2 127.2(3) . . ?
C27 N13 Fe2 113.1(2) . . ?
N1 C1 Fe1 171.0(3) . . ?
N2 C2 Fe1 170.1(3) . . ?
N3 C3 Fe1 177.0(4) . . ?
N4 C4 C5 110.5(4) . . ?
N4 C4 H4 124.8 . . ?
C5 C4 H4 124.8 . . ?
C4 C5 C6 105.1(4) . . ?
C4 C5 H5 127.4 . . ?
C6 C5 H5 127.4 . . ?
N5 C6 C5 108.8(3) . . ?
N5 C6 H6 125.6 . . ?
C5 C6 H6 125.6 . . ?
N6 C7 C8 110.0(4) . . ?
N6 C7 H7 125.0 . . ?
C8 C7 H7 125.0 . . ?
C9 C8 C7 105.0(3) . . ?
C9 C8 H8 127.5 . . ?
C7 C8 H8 127.5 . . ?
N7 C9 C8 109.7(4) . . ?
N7 C9 H9 125.1 . . ?
C8 C9 H9 125.1 . . ?
N8 C10 C11 110.4(4) . . ?
N8 C10 H10 124.8 . . ?
C11 C10 H10 124.8 . . ?
C12 C11 C10 104.8(4) . . ?
C12 C11 H11 127.6 . . ?
C10 C11 H11 127.6 . . ?
N9 C12 C11 108.9(4) . . ?
N9 C12 H12 125.5 . . ?
C11 C12 H12 125.5 . . ?
B1 C13 H13A 109.5 . . ?
B1 C13 H13B 109.5 . . ?
H13A C13 H13B 109.5 . . ?
B1 C13 H13C 109.5 . . ?
H13A C13 H13C 109.5 . . ?
H13B C13 H13C 109.5 . . ?
N10 C14 C15 121.6(5) . . ?
N10 C14 H14 119.2 . . ?
C15 C14 H14 119.2 . . ?
C16 C15 C14 119.3(5) . . ?
C16 C15 H15 120.4 . . ?
C14 C15 H15 120.4 . . ?
C15 C16 C17 120.7(5) . . ?
C15 C16 H16 119.6 . . ?
C17 C16 H16 119.6 . . ?
C18 C17 C16 117.6(5) . . ?
C18 C17 H17 121.2 . . ?
C16 C17 H17 121.2 . . ?
N10 C18 C17 121.9(4) . . ?
N10 C18 C19 115.5(3) . . ?
C17 C18 C19 122.5(4) . . ?
N11 C19 C18 108.7(3) . . ?
N11 C19 H19A 110.0 . . ?
C18 C19 H19A 110.0 . . ?
N11 C19 H19B 110.0 . . ?
C18 C19 H19B 110.0 . . ?
H19A C19 H19B 108.3 . . ?
C21 C20 N11 112.7(3) . . ?
C21 C20 H20A 109.1 . . ?
N11 C20 H20A 109.1 . . ?
C21 C20 H20B 109.1 . . ?
N11 C20 H20B 109.1 . . ?
H20A C20 H20B 107.8 . . ?
N12 C21 C22 122.3(3) . . ?
N12 C21 C20 115.1(3) . . ?
C22 C21 C20 122.5(3) . . ?
C23 C22 C21 118.9(4) . . ?
C23 C22 H22 120.6 . . ?
C21 C22 H22 120.6 . . ?
C24 C23 C22 118.8(4) . . ?
C24 C23 H23 120.6 . . ?
C22 C23 H23 120.6 . . ?
C25 C24 C23 119.7(4) . . ?
C25 C24 H24 120.2 . . ?
C23 C24 H24 120.2 . . ?
N12 C25 C24 122.5(4) . . ?
N12 C25 H25 118.7 . . ?
C24 C25 H25 118.7 . . ?
N11 C26 C27 109.3(3) . . ?
N11 C26 H26A 109.8 . . ?
C27 C26 H26A 109.8 . . ?
N11 C26 H26B 109.8 . . ?
C27 C26 H26B 109.8 . . ?
H26A C26 H26B 108.3 . . ?
N13 C27 C28 121.5(4) . . ?
N13 C27 C26 115.1(3) . . ?
C28 C27 C26 123.4(4) . . ?
C29 C28 C27 117.7(5) . . ?
C29 C28 H28 121.1 . . ?
C27 C28 H28 121.1 . . ?
C30 C29 C28 120.9(5) . . ?
C30 C29 H29 119.5 . . ?
C28 C29 H29 119.5 . . ?
C29 C30 C31 118.4(5) . . ?
C29 C30 H30 120.8 . . ?
C31 C30 H30 120.8 . . ?
N13 C31 C30 123.1(4) . . ?
N13 C31 H31 118.5 . . ?
C30 C31 H31 118.5 . . ?
O2 Cl1 O3 109.3(9) . . ?
O2 Cl1 O1 122.6(10) . . ?
O3 Cl1 O1 101.7(9) . . ?
O2 Cl1 O4 109.9(9) . . ?
O3 Cl1 O4 108.7(10) . . ?
O1 Cl1 O4 103.8(8) . . ?
O3' Cl1' O4' 128.3(14) . . ?
O3' Cl1' O2' 103.2(12) . . ?
O4' Cl1' O2' 109.2(11) . . ?
O3' Cl1' O1' 101.4(12) . . ?
O4' Cl1' O1' 106.9(11) . . ?
O2' Cl1' O1' 105.9(12) . . ?
H1WA O1W H1WB 110.4 . . ?

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
C4 N4 N5 C6 0.0(4) . . . . ?
Fe1 N4 N5 C6 -179.3(2) . . . . ?
C4 N4 N5 B1 178.1(3) . . . . ?
Fe1 N4 N5 B1 -1.3(4) . . . . ?
N7 B1 N5 C6 -126.0(4) . . . . ?
N9 B1 N5 C6 122.4(4) . . . . ?
C13 B1 N5 C6 -1.3(6) . . . . ?
N7 B1 N5 N4 56.5(4) . . . . ?
N9 B1 N5 N4 -55.1(4) . . . . ?
C13 B1 N5 N4 -178.8(3) . . . . ?
C7 N6 N7 C9 0.7(4) . . . . ?
Fe1 N6 N7 C9 -178.2(3) . . . . ?
C7 N6 N7 B1 -175.1(3) . . . . ?
Fe1 N6 N7 B1 6.0(4) . . . . ?
N9 B1 N7 C9 -122.2(4) . . . . ?
N5 B1 N7 C9 125.8(4) . . . . ?
C13 B1 N7 C9 1.5(6) . . . . ?
N9 B1 N7 N6 52.4(4) . . . . ?
N5 B1 N7 N6 -59.6(4) . . . . ?
C13 B1 N7 N6 176.1(3) . . . . ?
C10 N8 N9 C12 0.0(4) . . . . ?
Fe1 N8 N9 C12 179.0(3) . . . . ?
C10 N8 N9 B1 -179.8(3) . . . . ?
Fe1 N8 N9 B1 -0.8(4) . . . . ?
N7 B1 N9 C12 124.8(4) . . . . ?
N5 B1 N9 C12 -123.1(4) . . . . ?
C13 B1 N9 C12 0.6(6) . . . . ?
N7 B1 N9 N8 -55.5(4) . . . . ?
N5 B1 N9 N8 56.7(4) . . . . ?
C13 B1 N9 N8 -179.6(3) . . . . ?
N5 N4 C4 C5 -0.1(4) . . . . ?
Fe1 N4 C4 C5 179.1(3) . . . . ?
N4 C4 C5 C6 0.2(5) . . . . ?
N4 N5 C6 C5 0.1(4) . . . . ?
B1 N5 C6 C5 -177.6(4) . . . . ?
C4 C5 C6 N5 -0.2(5) . . . . ?
N7 N6 C7 C8 -0.5(4) . . . . ?
Fe1 N6 C7 C8 178.2(3) . . . . ?
N6 C7 C8 C9 0.1(5) . . . . ?
N6 N7 C9 C8 -0.7(5) . . . . ?
B1 N7 C9 C8 174.4(4) . . . . ?
C7 C8 C9 N7 0.3(5) . . . . ?
N9 N8 C10 C11 0.4(4) . . . . ?
Fe1 N8 C10 C11 -178.5(3) . . . . ?
N8 C10 C11 C12 -0.5(5) . . . . ?
N8 N9 C12 C11 -0.3(5) . . . . ?
B1 N9 C12 C11 179.5(4) . . . . ?
C10 C11 C12 N9 0.5(5) . . . . ?
C18 N10 C14 C15 0.4(6) . . . . ?
Fe2 N10 C14 C15 -175.8(3) . . . . ?
N10 C14 C15 C16 -0.2(7) . . . . ?
C14 C15 C16 C17 -0.7(9) . . . . ?
C15 C16 C17 C18 1.2(8) . . . . ?
C14 N10 C18 C17 0.2(6) . . . . ?
Fe2 N10 C18 C17 176.9(3) . . . . ?
C14 N10 C18 C19 -177.4(3) . . . . ?
Fe2 N10 C18 C19 -0.7(4) . . . . ?
C16 C17 C18 N10 -1.0(7) . . . . ?
C16 C17 C18 C19 176.4(4) . . . . ?
C26 N11 C19 C18 157.7(3) . . . . ?
C20 N11 C19 C18 -76.9(4) . . . . ?
Fe2 N11 C19 C18 41.5(3) . . . . ?
N10 C18 C19 N11 -27.9(4) . . . . ?
C17 C18 C19 N11 154.5(4) . . . . ?
C26 N11 C20 C21 -95.7(4) . . . . ?
C19 N11 C20 C21 137.9(3) . . . . ?
Fe2 N11 C20 C21 21.5(4) . . . . ?
C25 N12 C21 C22 3.0(5) . . . . ?
Fe2 N12 C21 C22 -164.1(3) . . . . ?
C25 N12 C21 C20 -173.7(3) . . . . ?
Fe2 N12 C21 C20 19.1(4) . . . . ?
N11 C20 C21 N12 -27.3(4) . . . . ?
N11 C20 C21 C22 155.9(3) . . . . ?
N12 C21 C22 C23 -1.9(6) . . . . ?
C20 C21 C22 C23 174.5(4) . . . . ?
C21 C22 C23 C24 -0.4(6) . . . . ?
C22 C23 C24 C25 1.6(7) . . . . ?
C21 N12 C25 C24 -1.8(6) . . . . ?
Fe2 N12 C25 C24 163.8(3) . . . . ?
C23 C24 C25 N12 -0.6(7) . . . . ?
C19 N11 C26 C27 -156.5(3) . . . . ?
C20 N11 C26 C27 78.9(4) . . . . ?
Fe2 N11 C26 C27 -40.3(4) . . . . ?
C31 N13 C27 C28 -1.8(6) . . . . ?
Fe2 N13 C27 C28 166.2(4) . . . . ?
C31 N13 C27 C26 177.4(3) . . . . ?
Fe2 N13 C27 C26 -14.6(4) . . . . ?
N11 C26 C27 N13 37.6(5) . . . . ?
N11 C26 C27 C28 -143.1(4) . . . . ?
N13 C27 C28 C29 1.8(7) . . . . ?
C26 C27 C28 C29 -177.4(5) . . . . ?
C27 C28 C29 C30 -1.0(9) . . . . ?
C28 C29 C30 C31 0.4(9) . . . . ?
C27 N13 C31 C30 1.1(6) . . . . ?
Fe2 N13 C31 C30 -165.0(3) . . . . ?
C29 C30 C31 N13 -0.4(7) . . . . ?

loop_
_geom_hbond_atom_site_label_D
_geom_hbond_atom_site_label_H
_geom_hbond_atom_site_label_A
_geom_hbond_distance_DH
_geom_hbond_distance_HA
_geom_hbond_distance_DA
_geom_hbond_angle_DHA
_geom_hbond_site_symmetry_A
O1W H1WB N3 0.83 2.47 3.219(9) 150.6 3_676
O1W H1WA O2' 0.83 2.16 2.930(19) 155.0 .
O1W H1WA O2 0.83 2.08 2.837(13) 151.0 .
C28 H28 O2' 0.93 2.63 3.416(14) 143.2 2_646
C25 H25 N1 0.93 2.64 3.139(5) 114.7 .
C24 H24 N3 0.93 2.70 3.440(6) 137.1 3_776
C20 H20A O3' 0.97 2.20 3.161(14) 168.5 2_646
C20 H20A O3 0.97 2.54 3.461(11) 158.6 2_646
C20 H20A O1 0.97 2.65 3.533(9) 151.1 2_646
C19 H19A O4' 0.97 2.63 3.273(13) 124.2 4_575
C17 H17 N3 0.93 2.68 3.445(6) 139.4 2_645
C15 H15 O1 0.93 2.64 3.496(9) 153.3 1_554
C14 H14 O1W 0.93 2.57 3.421(9) 152.0 3_676
C12 H12 O2' 0.93 2.56 3.410(16) 151.5 1_655
C12 H12 O2 0.93 2.59 3.421(13) 148.7 1_655
C11 H11 N3 0.93 2.64 3.522(6) 157.6 3_776
C8 H8 O2 0.93 2.64 3.325(11) 130.9 2_656
C7 H7 O4' 0.93 2.55 3.291(13) 137.1 2_656
C7 H7 O4 0.93 2.41 3.203(10) 142.6 2_656
C6 H6 O3' 0.93 2.33 3.213(14) 157.7 3_677
O1W H1WB N3 0.83 2.47 3.219(9) 150.6 3_676
O1W H1WA O2 0.83 2.08 2.837(13) 151.0 .
O1W H1WA O2' 0.83 2.16 2.930(19) 155.0 .

_refine_diff_density_max         0.520
_refine_diff_density_min         -0.489
_refine_diff_density_rms         0.066

