# Electronic Supplementary Material (ESI) for Inorganic Chemistry Frontiers.
# This journal is © the Partner Organisations 2017

####################################################################### 
# 
# 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_1024bm152
_database_code_depnum_ccdc_archive 'CCDC 1534003'
_audit_update_record             
;
2017-02-21 deposited with the CCDC.
2017-07-04 downloaded from the CCDC.
;

_audit_creation_method           SHELXL-2014
_chemical_name_systematic        
;
 ?
;
_chemical_name_common            ?
_chemical_melting_point          ?
_chemical_formula_moiety         'C24 H22 Fe N10, 2(Cl O4)'
_chemical_formula_sum            'C24 H22 Cl2 Fe N10 O8'
_chemical_formula_weight         705.26

loop_
_atom_type_symbol
_atom_type_description
_atom_type_scat_dispersion_real
_atom_type_scat_dispersion_imag
_atom_type_scat_source
C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Cl Cl 0.1484 0.1585 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Fe Fe 0.3463 0.8444 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'

_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                   41.290(9)
_cell_length_b                   8.0448(15)
_cell_length_c                   17.843(4)
_cell_angle_alpha                90
_cell_angle_beta                 108.946(14)
_cell_angle_gamma                90
_cell_volume                     5606(2)
_cell_formula_units_Z            8
_cell_measurement_temperature    100(2)
_cell_measurement_reflns_used    1166
_cell_measurement_theta_min      2.297
_cell_measurement_theta_max      19.169

_exptl_crystal_description       plate
_exptl_crystal_colour            red
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    ?
_exptl_crystal_density_diffrn    1.671
_exptl_crystal_F_000             2880
_exptl_transmission_factor_min   ?
_exptl_transmission_factor_max   ?
_exptl_crystal_size_max          0.170
_exptl_crystal_size_mid          0.100
_exptl_crystal_size_min          0.030
_exptl_absorpt_coefficient_mu    0.798
_shelx_estimated_absorpt_T_min   0.876
_shelx_estimated_absorpt_T_max   0.976
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_correction_T_min  0.524
_exptl_absorpt_correction_T_max  0.745
_exptl_absorpt_process_details   
;
SADABS-2008/1 (Bruker,2008) was used for absorption correction.
wR2(int) was 0.1435 before and 0.0664 after correction.
The Ratio of minimum to maximum transmission is 0.7030.
The λ/2 correction factor is 0.0015.
;

_exptl_special_details           
;
 ?
;

_diffrn_ambient_temperature      100(2)
_diffrn_radiation_wavelength     0.71073
_diffrn_radiation_type           MoK\a
_diffrn_radiation_source         'multilayer monochromator ImuS'
_diffrn_measurement_device_type  'Bruker APEX II QUAZAR'
_diffrn_measurement_method       'φ and ω rotation with narrow frames'
_diffrn_detector_area_resol_mean ?
_diffrn_reflns_number            11477
_diffrn_reflns_av_unetI/netI     0.1117
_diffrn_reflns_av_R_equivalents  0.1130
_diffrn_reflns_limit_h_min       -40
_diffrn_reflns_limit_h_max       43
_diffrn_reflns_limit_k_min       -8
_diffrn_reflns_limit_k_max       8
_diffrn_reflns_limit_l_min       -18
_diffrn_reflns_limit_l_max       18
_diffrn_reflns_theta_min         2.086
_diffrn_reflns_theta_max         22.213
_diffrn_reflns_theta_full        22.210
_diffrn_measured_fraction_theta_max 0.968
_diffrn_measured_fraction_theta_full 0.968
_diffrn_reflns_Laue_measured_fraction_max 0.968
_diffrn_reflns_Laue_measured_fraction_full 0.968
_diffrn_reflns_point_group_measured_fraction_max 0.968
_diffrn_reflns_point_group_measured_fraction_full 0.968
_reflns_number_total             3428
_reflns_number_gt                2199
_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 APEX 2'
_computing_cell_refinement       'SAINT v8.34A (Bruker, 2013)'
_computing_data_reduction        'SAINT v8.34A (Bruker, 2013)'
_computing_structure_solution    'SHELXT (Sheldrick, 2015)'
_computing_structure_refinement  'SHELXL-2014 (Sheldrick, 2015)'
_computing_molecular_graphics    ?
_computing_publication_material  ?

_refine_special_details          
;
 All non-hydrogens were refined anisotropically. Both 
 perchlorates show some thermal disorder, but only required
 displacement parameters restraints. Hydrogens were placed geometrically
 on their carrier atom and refined with a riding model except those
 on the pyrazole N that were refined freely with their thermal parameter
 1.2 times that of their carrier N and a distance restraint. 
;

_vrf_THETM01_1024bm152           
;
PROBLEM:  The value of sine(theta_max)/wavelength is less than 0.550
            Calculated sin(theta_max)/wavelength =    0.5319
RESPONSE: Diffraction decreased significantly at resolutions better
than 0.95 angstrom and the present data were cut at 0.94 angstrom
where I/sigma(I) was below 2. This poor diffraction results in poor
thetamax and thetafull values, as well as a poor data over parameters ratio.
;

_vrf_PLAT027_1024bm152           
;
PROBLEM:  _diffrn_reflns_theta_full value (too) Low ......      22.21 Degree
RESPONSE: Diffraction decreased significantly at resolutions better
than 0.95 angstrom and the present data were cut at 0.94 angstrom
where I/sigma(I) was below 2. This poor diffraction results in poor
thetamax and thetafull values, as well as a poor data over parameters ratio.
;

_vrf_REFNR01_1024bm152           
;
PROBLEM:  Ratio of reflections to parameters is < 10 for a
            centrosymmetric structure
            sine(theta)/lambda                0.5319
            Proportion of unique data used    1.0000
            Ratio reflections to parameters   8.2602
RESPONSE: Diffraction decreased significantly at resolutions better
than 0.95 angstrom and the present data were cut at 0.94 angstrom
where I/sigma(I) was below 2. This poor diffraction results in poor
thetamax and thetafull values, as well as a poor data over parameters ratio.
;

_vrf_PLAT088_1024bm152           
;
PROBLEM:  Poor Data / Parameter Ratio ....................       8.26 Note  
RESPONSE: Diffraction decreased significantly at resolutions better
than 0.95 angstrom and the present data were cut at 0.94 angstrom
where I/sigma(I) was below 2. This poor diffraction results in poor
thetamax and thetafull values, as well as a poor data over parameters ratio.
;

_refine_ls_structure_factor_coef Fsqd
_refine_ls_matrix_type           full
_refine_ls_weighting_scheme      calc
_refine_ls_weighting_details     
'w=1/[σ²(Fo²)+(0.0538P)²+26.3863P] where P=(Fo²+2Fc²)/3'
_atom_sites_solution_primary     ?
_atom_sites_solution_secondary   ?
_atom_sites_solution_hydrogens   mixed
_refine_ls_hydrogen_treatment    mixed
_refine_ls_extinction_method     SHELXL
_refine_ls_extinction_coef       0.00081(11)
_refine_ls_extinction_expression Fc^*^=kFc[1+0.001xFc²λ³/sin(2θ)]^-1/4^
_refine_ls_number_reflns         3428
_refine_ls_number_parameters     415
_refine_ls_number_restraints     82
_refine_ls_R_factor_all          0.1200
_refine_ls_R_factor_gt           0.0700
_refine_ls_wR_factor_ref         0.1553
_refine_ls_wR_factor_gt          0.1355
_refine_ls_goodness_of_fit_ref   1.059
_refine_ls_restrained_S_all      1.101
_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 0.62658(3) 0.70111(13) 0.71403(6) 0.0249(4) Uani 1 1 d . . . . .
N1 N 0.61462(16) 0.4808(8) 0.6619(3) 0.0255(15) Uani 1 1 d . . . . .
N2 N 0.57985(17) 0.4610(8) 0.6290(4) 0.0331(17) Uani 1 1 d . . . . .
N3 N 0.57809(16) 0.7195(8) 0.6760(3) 0.0294(16) Uani 1 1 d . . . . .
N4 N 0.62007(17) 0.9270(7) 0.7477(3) 0.0248(15) Uani 1 1 d . . . . .
N5 N 0.63992(18) 1.0506(8) 0.7875(4) 0.0320(17) Uani 1 1 d D . . . .
H5 H 0.6626(7) 1.053(10) 0.796(4) 0.038 Uiso 1 1 d D U . . .
N6 N 0.63141(17) 0.6175(8) 0.8235(3) 0.0293(16) Uani 1 1 d . . . . .
N7 N 0.66527(17) 0.5891(8) 0.8658(3) 0.0294(16) Uani 1 1 d . . . . .
N8 N 0.67530(15) 0.6819(7) 0.7571(3) 0.0237(15) Uani 1 1 d . . . . .
N9 N 0.64037(16) 0.7809(7) 0.6244(3) 0.0238(15) Uani 1 1 d . . . . .
N10 N 0.62551(18) 0.8400(8) 0.5501(4) 0.0319(17) Uani 1 1 d D . . . .
H10 H 0.6025(6) 0.846(10) 0.530(4) 0.038 Uiso 1 1 d D U . . .
C1 C 0.6660(2) 0.3188(10) 0.6637(4) 0.036(2) Uani 1 1 d . . . . .
H1A H 0.6764 0.3993 0.6370 0.054 Uiso 1 1 calc R U . . .
H1B H 0.6705 0.2058 0.6490 0.054 Uiso 1 1 calc R U . . .
H1C H 0.6760 0.3325 0.7212 0.054 Uiso 1 1 calc R U . . .
C2 C 0.6286(2) 0.3472(10) 0.6393(4) 0.031(2) Uani 1 1 d . . . . .
C3 C 0.6024(2) 0.2438(10) 0.5912(4) 0.037(2) Uani 1 1 d . . . . .
H3 H 0.6054 0.1424 0.5669 0.045 Uiso 1 1 calc R U . . .
C4 C 0.5721(2) 0.3165(11) 0.5862(4) 0.041(2) Uani 1 1 d . . . . .
H4 H 0.5499 0.2753 0.5584 0.049 Uiso 1 1 calc R U . . .
C5 C 0.5590(2) 0.5911(10) 0.6386(4) 0.032(2) Uani 1 1 d . . . . .
C6 C 0.5237(2) 0.5898(11) 0.6154(5) 0.045(2) Uani 1 1 d . . . . .
H6 H 0.5107 0.4965 0.5895 0.054 Uiso 1 1 calc R U . . .
C7 C 0.5082(2) 0.7301(12) 0.6317(5) 0.048(3) Uani 1 1 d . . . . .
H7 H 0.4839 0.7343 0.6158 0.058 Uiso 1 1 calc R U . . .
C8 C 0.5269(2) 0.8656(11) 0.6707(5) 0.048(3) Uani 1 1 d . . . . .
H8 H 0.5158 0.9614 0.6819 0.057 Uiso 1 1 calc R U . . .
C9 C 0.5623(2) 0.8570(10) 0.6927(4) 0.033(2) Uani 1 1 d . . . . .
C10 C 0.5878(2) 0.9778(10) 0.7351(4) 0.030(2) Uani 1 1 d . . . . .
C11 C 0.5873(3) 1.1358(10) 0.7687(5) 0.037(2) Uani 1 1 d . . . . .
H11 H 0.5678 1.1988 0.7683 0.044 Uiso 1 1 calc R U . . .
C12 C 0.6208(3) 1.1787(10) 0.8019(4) 0.038(2) Uani 1 1 d . . . . .
H12 H 0.6294 1.2786 0.8297 0.046 Uiso 1 1 calc R U . . .
C13 C 0.5758(2) 0.6066(11) 0.8481(5) 0.046(2) Uani 1 1 d . . . . .
H13A H 0.5702 0.7253 0.8448 0.070 Uiso 1 1 calc R U . . .
H13B H 0.5673 0.5539 0.8876 0.070 Uiso 1 1 calc R U . . .
H13C H 0.5651 0.5545 0.7964 0.070 Uiso 1 1 calc R U . . .
C14 C 0.6135(2) 0.5855(9) 0.8720(4) 0.033(2) Uani 1 1 d . . . . .
C15 C 0.6361(2) 0.5331(9) 0.9466(5) 0.036(2) Uani 1 1 d . . . . .
H15 H 0.6299 0.5008 0.9913 0.043 Uiso 1 1 calc R U . . .
C16 C 0.6690(2) 0.5379(10) 0.9419(4) 0.038(2) Uani 1 1 d . . . . .
H16 H 0.6897 0.5114 0.9827 0.046 Uiso 1 1 calc R U . . .
C17 C 0.6898(2) 0.6248(9) 0.8304(4) 0.0264(19) Uani 1 1 d . . . . .
C18 C 0.7244(2) 0.6069(10) 0.8635(5) 0.034(2) Uani 1 1 d . . . . .
H18 H 0.7341 0.5658 0.9159 0.041 Uiso 1 1 calc R U . . .
C19 C 0.7449(2) 0.6491(10) 0.8198(5) 0.037(2) Uani 1 1 d . . . . .
H19 H 0.7690 0.6376 0.8417 0.045 Uiso 1 1 calc R U . . .
C20 C 0.7302(2) 0.7092(10) 0.7428(4) 0.0301(19) Uani 1 1 d . . . . .
H20 H 0.7441 0.7374 0.7115 0.036 Uiso 1 1 calc R U . . .
C21 C 0.6951(2) 0.7267(9) 0.7131(4) 0.030(2) Uani 1 1 d . . . . .
C22 C 0.6743(2) 0.7860(9) 0.6354(4) 0.0259(19) Uani 1 1 d . . . . .
C23 C 0.6805(2) 0.8503(9) 0.5691(4) 0.032(2) Uani 1 1 d . . . . .
H23 H 0.7022 0.8676 0.5622 0.038 Uiso 1 1 calc R U . . .
C24 C 0.6488(2) 0.8835(10) 0.5159(5) 0.038(2) Uani 1 1 d . . . . .
H24 H 0.6442 0.9289 0.4643 0.046 Uiso 1 1 calc R U . . .
Cl1 Cl 0.53659(5) 0.8151(3) 0.43116(13) 0.0442(6) Uani 1 1 d . U . . .
O1 O 0.52651(18) 0.7813(10) 0.3479(4) 0.080(2) Uani 1 1 d . U . . .
O2 O 0.50619(16) 0.8217(8) 0.4531(4) 0.0598(16) Uani 1 1 d . U . . .
O3 O 0.55783(17) 0.6754(8) 0.4708(4) 0.0638(18) Uani 1 1 d . U . . .
O4 O 0.55548(18) 0.9619(9) 0.4519(5) 0.100(2) Uani 1 1 d . U . . .
Cl2 Cl 0.72666(6) 1.0715(3) 0.90251(11) 0.0407(6) Uani 1 1 d . U . . .
O5 O 0.70978(14) 1.0279(7) 0.8196(3) 0.0392(14) Uani 1 1 d . U . . .
O6 O 0.71396(16) 0.9675(8) 0.9515(3) 0.0513(15) Uani 1 1 d . U . . .
O7 O 0.7196(2) 1.2385(8) 0.9126(4) 0.095(2) Uani 1 1 d . U . . .
O8 O 0.76243(17) 1.0417(10) 0.9202(4) 0.0742(19) Uani 1 1 d . 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 N3 1.900(6) . ?
Fe1 N8 1.913(6) . ?
Fe1 N4 1.960(6) . ?
Fe1 N9 1.972(6) . ?
Fe1 N1 1.987(6) . ?
Fe1 N6 2.013(6) . ?
N1 C2 1.344(9) . ?
N1 N2 1.373(8) . ?
N2 C4 1.370(10) . ?
N2 C5 1.400(10) . ?
N3 C5 1.339(9) . ?
N3 C9 1.366(10) . ?
N4 N5 1.337(8) . ?
N4 C10 1.340(9) . ?
N5 C12 1.371(10) . ?
N5 H5 0.90(2) . ?
N6 C14 1.332(10) . ?
N6 N7 1.375(8) . ?
N7 C16 1.380(9) . ?
N7 C17 1.386(9) . ?
N8 C17 1.332(9) . ?
N8 C21 1.352(9) . ?
N9 C22 1.351(9) . ?
N9 N10 1.353(8) . ?
N10 C24 1.344(10) . ?
N10 H10 0.90(2) . ?
C1 C2 1.480(11) . ?
C1 H1A 0.9800 . ?
C1 H1B 0.9800 . ?
C1 H1C 0.9800 . ?
C2 C3 1.414(11) . ?
C3 C4 1.355(11) . ?
C3 H3 0.9500 . ?
C4 H4 0.9500 . ?
C5 C6 1.381(11) . ?
C6 C7 1.374(12) . ?
C6 H6 0.9500 . ?
C7 C8 1.385(12) . ?
C7 H7 0.9500 . ?
C8 C9 1.385(11) . ?
C8 H8 0.9500 . ?
C9 C10 1.453(11) . ?
C10 C11 1.409(11) . ?
C11 C12 1.360(12) . ?
C11 H11 0.9500 . ?
C12 H12 0.9500 . ?
C13 C14 1.484(11) . ?
C13 H13A 0.9800 . ?
C13 H13B 0.9800 . ?
C13 H13C 0.9800 . ?
C14 C15 1.419(11) . ?
C15 C16 1.386(11) . ?
C15 H15 0.9500 . ?
C16 H16 0.9500 . ?
C17 C18 1.364(10) . ?
C18 C19 1.367(11) . ?
C18 H18 0.9500 . ?
C19 C20 1.395(10) . ?
C19 H19 0.9500 . ?
C20 C21 1.381(10) . ?
C20 H20 0.9500 . ?
C21 C22 1.454(10) . ?
C22 C23 1.389(10) . ?
C23 C24 1.371(11) . ?
C23 H23 0.9500 . ?
C24 H24 0.9500 . ?
Cl1 O4 1.397(7) . ?
Cl1 O2 1.432(6) . ?
Cl1 O1 1.432(6) . ?
Cl1 O3 1.460(6) . ?
Cl2 O7 1.399(7) . ?
Cl2 O6 1.427(6) . ?
Cl2 O8 1.427(7) . ?
Cl2 O5 1.459(5) . ?

loop_
_geom_angle_atom_site_label_1
_geom_angle_atom_site_label_2
_geom_angle_atom_site_label_3
_geom_angle
_geom_angle_site_symmetry_1
_geom_angle_site_symmetry_3
_geom_angle_publ_flag
N3 Fe1 N8 177.4(3) . . ?
N3 Fe1 N4 78.7(3) . . ?
N8 Fe1 N4 100.5(3) . . ?
N3 Fe1 N9 103.5(2) . . ?
N8 Fe1 N9 79.0(3) . . ?
N4 Fe1 N9 93.0(2) . . ?
N3 Fe1 N1 80.2(3) . . ?
N8 Fe1 N1 100.6(3) . . ?
N4 Fe1 N1 158.8(3) . . ?
N9 Fe1 N1 90.2(2) . . ?
N3 Fe1 N6 97.7(3) . . ?
N8 Fe1 N6 79.8(3) . . ?
N4 Fe1 N6 89.6(2) . . ?
N9 Fe1 N6 158.8(3) . . ?
N1 Fe1 N6 95.0(2) . . ?
C2 N1 N2 105.7(6) . . ?
C2 N1 Fe1 142.0(6) . . ?
N2 N1 Fe1 111.7(5) . . ?
C4 N2 N1 111.0(7) . . ?
C4 N2 C5 131.4(7) . . ?
N1 N2 C5 117.4(6) . . ?
C5 N3 C9 119.2(7) . . ?
C5 N3 Fe1 120.0(6) . . ?
C9 N3 Fe1 120.6(6) . . ?
N5 N4 C10 105.5(6) . . ?
N5 N4 Fe1 137.0(5) . . ?
C10 N4 Fe1 117.3(5) . . ?
N4 N5 C12 111.5(7) . . ?
N4 N5 H5 122(5) . . ?
C12 N5 H5 126(6) . . ?
C14 N6 N7 106.9(6) . . ?
C14 N6 Fe1 142.5(6) . . ?
N7 N6 Fe1 110.5(5) . . ?
N6 N7 C16 111.0(7) . . ?
N6 N7 C17 118.6(6) . . ?
C16 N7 C17 130.2(7) . . ?
C17 N8 C21 119.9(7) . . ?
C17 N8 Fe1 120.1(5) . . ?
C21 N8 Fe1 120.0(5) . . ?
C22 N9 N10 104.5(6) . . ?
C22 N9 Fe1 116.8(5) . . ?
N10 N9 Fe1 138.6(5) . . ?
C24 N10 N9 111.9(6) . . ?
C24 N10 H10 129(5) . . ?
N9 N10 H10 119(5) . . ?
C2 C1 H1A 109.5 . . ?
C2 C1 H1B 109.5 . . ?
H1A C1 H1B 109.5 . . ?
C2 C1 H1C 109.5 . . ?
H1A C1 H1C 109.5 . . ?
H1B C1 H1C 109.5 . . ?
N1 C2 C3 109.5(7) . . ?
N1 C2 C1 123.0(7) . . ?
C3 C2 C1 127.5(8) . . ?
C4 C3 C2 107.1(7) . . ?
C4 C3 H3 126.4 . . ?
C2 C3 H3 126.4 . . ?
C3 C4 N2 106.7(7) . . ?
C3 C4 H4 126.7 . . ?
N2 C4 H4 126.7 . . ?
N3 C5 C6 123.3(8) . . ?
N3 C5 N2 110.6(7) . . ?
C6 C5 N2 126.1(8) . . ?
C7 C6 C5 116.7(9) . . ?
C7 C6 H6 121.7 . . ?
C5 C6 H6 121.7 . . ?
C6 C7 C8 122.1(8) . . ?
C6 C7 H7 119.0 . . ?
C8 C7 H7 119.0 . . ?
C9 C8 C7 117.8(8) . . ?
C9 C8 H8 121.1 . . ?
C7 C8 H8 121.1 . . ?
N3 C9 C8 120.9(8) . . ?
N3 C9 C10 109.7(7) . . ?
C8 C9 C10 129.4(8) . . ?
N4 C10 C11 110.8(8) . . ?
N4 C10 C9 113.5(7) . . ?
C11 C10 C9 135.8(8) . . ?
C12 C11 C10 105.1(8) . . ?
C12 C11 H11 127.4 . . ?
C10 C11 H11 127.4 . . ?
C11 C12 N5 107.1(8) . . ?
C11 C12 H12 126.5 . . ?
N5 C12 H12 126.5 . . ?
C14 C13 H13A 109.5 . . ?
C14 C13 H13B 109.5 . . ?
H13A C13 H13B 109.5 . . ?
C14 C13 H13C 109.5 . . ?
H13A C13 H13C 109.5 . . ?
H13B C13 H13C 109.5 . . ?
N6 C14 C15 109.4(8) . . ?
N6 C14 C13 122.9(7) . . ?
C15 C14 C13 127.7(8) . . ?
C16 C15 C14 107.1(7) . . ?
C16 C15 H15 126.4 . . ?
C14 C15 H15 126.4 . . ?
N7 C16 C15 105.6(7) . . ?
N7 C16 H16 127.2 . . ?
C15 C16 H16 127.2 . . ?
N8 C17 C18 122.3(7) . . ?
N8 C17 N7 110.9(7) . . ?
C18 C17 N7 126.7(7) . . ?
C17 C18 C19 118.8(7) . . ?
C17 C18 H18 120.6 . . ?
C19 C18 H18 120.6 . . ?
C18 C19 C20 119.8(8) . . ?
C18 C19 H19 120.1 . . ?
C20 C19 H19 120.1 . . ?
C21 C20 C19 118.6(8) . . ?
C21 C20 H20 120.7 . . ?
C19 C20 H20 120.7 . . ?
N8 C21 C20 120.5(7) . . ?
N8 C21 C22 111.2(7) . . ?
C20 C21 C22 128.4(7) . . ?
N9 C22 C23 111.0(7) . . ?
N9 C22 C21 113.0(6) . . ?
C23 C22 C21 136.0(8) . . ?
C24 C23 C22 105.3(7) . . ?
C24 C23 H23 127.4 . . ?
C22 C23 H23 127.4 . . ?
N10 C24 C23 107.3(7) . . ?
N10 C24 H24 126.3 . . ?
C23 C24 H24 126.3 . . ?
O4 Cl1 O2 111.1(5) . . ?
O4 Cl1 O1 112.6(6) . . ?
O2 Cl1 O1 107.8(4) . . ?
O4 Cl1 O3 109.1(4) . . ?
O2 Cl1 O3 109.8(4) . . ?
O1 Cl1 O3 106.4(4) . . ?
O7 Cl2 O6 110.5(5) . . ?
O7 Cl2 O8 112.1(5) . . ?
O6 Cl2 O8 109.0(4) . . ?
O7 Cl2 O5 108.1(4) . . ?
O6 Cl2 O5 109.3(3) . . ?
O8 Cl2 O5 107.7(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
N5 H5 O5 0.90(2) 1.87(3) 2.759(9) 172(8) .
N10 H10 O3 0.90(2) 2.27(6) 2.999(10) 138(7) .
N10 H10 O4 0.90(2) 2.20(4) 3.017(10) 151(7) .

_refine_diff_density_max         0.881
_refine_diff_density_min         -0.412
_refine_diff_density_rms         0.098

_shelxl_version_number           2014-3



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

data_bm354
_database_code_depnum_ccdc_archive 'CCDC 1534005'
_audit_update_record             
;
2017-02-21 deposited with the CCDC.
2017-07-04 downloaded from the CCDC.
;

_audit_creation_method           SHELXL-2014
_chemical_name_systematic        
;
 ?
;
_chemical_name_common            ?
_chemical_melting_point          ?
_chemical_formula_moiety         'C24 H22 Fe N10, 2(Cl O4), H2 O'
_chemical_formula_sum            'C24 H24 Cl2 Fe N10 O9'
_chemical_formula_weight         723.28

loop_
_atom_type_symbol
_atom_type_description
_atom_type_scat_dispersion_real
_atom_type_scat_dispersion_imag
_atom_type_scat_source
C C 0.0040 0.0020
'XDisp Program in WinGX L.J. Farrugia, J.Appl.Cryst. 2012,45,849-854'
H H 0.0000 0.0000
'XDisp Program in WinGX L.J. Farrugia, J.Appl.Cryst. 2012,45,849-854'
N N 0.0076 0.0040
'XDisp Program in WinGX L.J. Farrugia, J.Appl.Cryst. 2012,45,849-854'
O O 0.0132 0.0074
'XDisp Program in WinGX L.J. Farrugia, J.Appl.Cryst. 2012,45,849-854'
Cl Cl 0.1697 0.1896
'XDisp Program in WinGX L.J. Farrugia, J.Appl.Cryst. 2012,45,849-854'
Fe Fe 0.3555 0.9930
'XDisp Program in WinGX L.J. Farrugia, J.Appl.Cryst. 2012,45,849-854'

_space_group_crystal_system      monoclinic
_space_group_IT_number           9
_space_group_name_H-M_alt        'C 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'

_cell_length_a                   11.916(6)
_cell_length_b                   11.884(6)
_cell_length_c                   19.902(15)
_cell_angle_alpha                90
_cell_angle_beta                 98.552(13)
_cell_angle_gamma                90
_cell_volume                     2787(3)
_cell_formula_units_Z            4
_cell_measurement_temperature    100(2)
_cell_measurement_reflns_used    9814
_cell_measurement_theta_min      2.65
_cell_measurement_theta_max      30.26

_exptl_crystal_description       plate
_exptl_crystal_colour            yellow
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    ?
_exptl_crystal_density_diffrn    1.724
_exptl_crystal_F_000             1480
_exptl_transmission_factor_min   ?
_exptl_transmission_factor_max   ?
_exptl_crystal_size_max          0.110
_exptl_crystal_size_mid          0.080
_exptl_crystal_size_min          0.005
_exptl_absorpt_coefficient_mu    1.015
_shelx_estimated_absorpt_T_min   0.897
_shelx_estimated_absorpt_T_max   0.995
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_correction_T_min  0.621
_exptl_absorpt_correction_T_max  0.746
_exptl_absorpt_process_details   SADABS-2014/5

_exptl_special_details           
;
 ?
;

_diffrn_ambient_temperature      100(2)
_diffrn_radiation_wavelength     0.7749
_diffrn_radiation_type           synchrotron
_diffrn_radiation_source         'Advanced Light Source station 11.3.1'
_diffrn_radiation_monochromator  'silicon 111'
_diffrn_measurement_device_type  'Bruker D8 with PHOTON 100 detector'
_diffrn_measurement_method       'shutterless /f and /w scans'
_diffrn_detector_area_resol_mean ?
_diffrn_reflns_number            16746
_diffrn_reflns_av_unetI/netI     0.0846
_diffrn_reflns_av_R_equivalents  0.0785
_diffrn_reflns_limit_h_min       -15
_diffrn_reflns_limit_h_max       15
_diffrn_reflns_limit_k_min       -15
_diffrn_reflns_limit_k_max       15
_diffrn_reflns_limit_l_min       -25
_diffrn_reflns_limit_l_max       25
_diffrn_reflns_theta_min         2.257
_diffrn_reflns_theta_max         29.793
_diffrn_reflns_theta_full        27.706
_diffrn_measured_fraction_theta_max 0.959
_diffrn_measured_fraction_theta_full 1.000
_diffrn_reflns_Laue_measured_fraction_max 0.959
_diffrn_reflns_Laue_measured_fraction_full 1.000
_diffrn_reflns_point_group_measured_fraction_max 0.953
_diffrn_reflns_point_group_measured_fraction_full 0.996
_reflns_number_total             6063
_reflns_number_gt                5438
_reflns_threshold_expression     'I > 2σ(I)'
_reflns_Friedel_coverage         0.987
_reflns_Friedel_fraction_max     0.948
_reflns_Friedel_fraction_full    0.992

_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 APEX 2'
_computing_cell_refinement       'Bruker SAINT'
_computing_data_reduction        'Bruker SAINT'
_computing_structure_solution    'SHELXT (Sheldrick, 2015)'
_computing_structure_refinement  'SHELXL-2014 (Sheldrick, 2015)'
_computing_molecular_graphics    ?
_computing_publication_material  ?

_refine_special_details          
;Refined as a 2-component inversion twin. The structure was first
 solved in P1 on HKLF4 data, transformed to the monoclinic Cc present
 model with PLATON/ADDSYM. The used twin law was found through
 PLATON/FCF-VALIDATION. All attempts at resolving twinning
 within APEX2 in combination with CELL_NOW resulted in (very) poor
 integration of diffraction images. This is likely due to the nature
 of the available crystals that are extremely thin plates forming
 multi-stacks. Despite several attempts and efforts to separate
 these stacks, the measured crystal is likely a stack multi-crystal
 and not a true twin. This is supported by the fact various twin
 laws are in fact proposed by PLATON/FCF-VALIDATION.
 All non-hydrogens were refined anisotropically, but soft displacement
 parameters restrains (SIMU/DELU) were necessary for all atoms for the
 refinement to converge properly, likely due to the 
 twinning/multi-crystal. O1W in addition required rather strong
 isotropic displacement parameters restraints (ISOR).
 Hydrogens were placed geometrically on their 
 carrier atom and refined with a riding model, except those on the
 lattice water O1W that are omitted in the structural model but
 included in the formula., Twin
;

_vrf_DIFMN02_bm354               
;
PROBLEM:  The minimum difference density is < -0.1*ZMAX*1.00
            _refine_diff_density_min given =     -2.752
            Test value =     -2.600
RESPONSE: There remains one density hole close to O1W, that maybe
be a consequence of the twinning/multi-crystal, or to some
disorder of the lattice water molecule, since O1W required the use
of a strong isotropic displacement parameter restraint (ISOR).
;

_vrf_PLAT098_bm354               
;
PROBLEM:  Large Reported Min.  (Negative) Residual Density      -2.75 eA-3 
RESPONSE: There remains one density hole close to O1W, that maybe
be a consequence of the twinning/multi-crystal, or to some
disorder of the lattice water molecule, since O1W required the use
of a strong isotropic displacement parameter restraint (ISOR).
;

_vrf_PLAT306_bm354               
;
PROBLEM:  Isolated Oxygen Atom (H-atoms Missing ?) .......        O1W Check 
RESPONSE: Hydrogens on the lattice water molecule O1W could not
be found nor fixed and are omitted in the structural model, although
included in the formula.
;

_vrf_FORMU01_bm354               
;
PROBLEM:  There is a discrepancy between the atom counts in the
            _chemical_formula_sum and the formula from the _atom_site* data.
            Atom count from _chemical_formula_sum:C24 H24 Cl2 Fe1 N10 O9
            Atom count from the _atom_site data:  C24 H22 Cl2 Fe1 N10 O9 
RESPONSE: Hydrogens on the lattice water molecule O1W could not
be found nor fixed and are omitted in the structural model, although
included in the formula.
;

_vrf_PLAT931_bm354               
;
PROBLEM:  Found Twin Law ( 0 0  1)[       ] Estimated BASF       0.37 Check  
RESPONSE: The used twin law was found through PLATON/FCF-VALIDATION.
All attempts at resolving twinning within APEX2 in combination with 
CELL_NOW resulted in (very) poor integration of diffraction images. 
This is likely due to the nature of the available crystals that are 
extremely thin plates forming multi-stacks. Despite several attempts 
and efforts to separate these stacks, the measured crystal is likely 
a stack multi-crystal and not a true twin. Indeed, as this alert 
indicates, various twin laws are in fact proposed by 
PLATON/FCF-VALIDATION.
;

_refine_ls_structure_factor_coef Fsqd
_refine_ls_matrix_type           full
_refine_ls_weighting_scheme      calc
_refine_ls_weighting_details     
'w=1/[σ²(Fo²)+(0.1254P)²+158.4560P] 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     SHELXL
_refine_ls_extinction_coef       0.0028(9)
_refine_ls_extinction_expression Fc^*^=kFc[1+0.001xFc²λ³/sin(2θ)]^-1/4^
_refine_ls_abs_structure_details 
;
 Refined as an inversion twin.
;
_refine_ls_abs_structure_Flack   0.351(6)
_chemical_absolute_configuration ?
_refine_ls_number_reflns         6063
_refine_ls_number_parameters     419
_refine_ls_number_restraints     487
_refine_ls_R_factor_all          0.1474
_refine_ls_R_factor_gt           0.1380
_refine_ls_wR_factor_ref         0.3337
_refine_ls_wR_factor_gt          0.3254
_refine_ls_goodness_of_fit_ref   1.015
_refine_ls_restrained_S_all      0.986
_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 0.3140(3) 0.6806(2) 0.43517(18) 0.0148(6) Uani 1 1 d . U . . .
N1 N 0.4664(17) 0.6163(18) 0.4563(11) 0.023(3) Uani 1 1 d . U . . .
N2 N 0.554(2) 0.588(2) 0.4238(15) 0.037(4) Uani 1 1 d . U . . .
H2B H 0.5523 0.5926 0.3796 0.044 Uiso 1 1 calc R U . . .
N3 N 0.330(2) 0.682(2) 0.5314(11) 0.020(3) Uani 1 1 d . U . . .
N4 N 0.157(2) 0.7515(19) 0.5183(11) 0.025(3) Uani 1 1 d . U . . .
N5 N 0.1669(16) 0.7414(16) 0.4495(10) 0.017(3) Uani 1 1 d . U . . .
N6 N 0.3715(16) 0.8336(16) 0.4210(9) 0.019(3) Uani 1 1 d . U . . .
N7 N 0.4158(17) 0.9221(17) 0.4582(11) 0.024(3) Uani 1 1 d . U . . .
H7B H 0.4333 0.9217 0.5027 0.029 Uiso 1 1 calc R U . . .
N8 N 0.292(2) 0.687(2) 0.3382(11) 0.020(2) Uani 1 1 d . U . . .
N9 N 0.2269(19) 0.5108(18) 0.3448(12) 0.026(3) Uani 1 1 d . U . . .
N10 N 0.2482(18) 0.5289(17) 0.4134(11) 0.022(3) Uani 1 1 d . U . . .
C1 C 0.642(2) 0.550(3) 0.467(2) 0.047(5) Uani 1 1 d . U . . .
H1A H 0.7062 0.5115 0.4560 0.056 Uiso 1 1 calc R U . . .
C2 C 0.622(2) 0.578(3) 0.5285(19) 0.043(5) Uani 1 1 d . U . . .
H2A H 0.6752 0.5732 0.5692 0.051 Uiso 1 1 calc R U . . .
C3 C 0.511(2) 0.614(2) 0.5226(14) 0.026(3) Uani 1 1 d . U . . .
C4 C 0.436(2) 0.651(2) 0.5688(13) 0.027(4) Uani 1 1 d . U . . .
C5 C 0.451(3) 0.658(2) 0.6368(14) 0.036(4) Uani 1 1 d . U . . .
H5A H 0.5198 0.6340 0.6627 0.043 Uiso 1 1 calc R U . . .
C6 C 0.366(4) 0.700(3) 0.6688(16) 0.042(5) Uani 1 1 d . U . . .
H6A H 0.3803 0.7066 0.7169 0.050 Uiso 1 1 calc R U . . .
C7 C 0.258(3) 0.735(3) 0.6342(13) 0.035(4) Uani 1 1 d . U . . .
H7A H 0.1988 0.7646 0.6562 0.042 Uiso 1 1 calc R U . . .
C8 C 0.251(2) 0.721(2) 0.5623(12) 0.027(4) Uani 1 1 d . U . . .
C9 C 0.055(2) 0.794(2) 0.5269(14) 0.029(4) Uani 1 1 d . U . . .
H9A H 0.0314 0.8138 0.5689 0.035 Uiso 1 1 calc R U . . .
C10 C -0.006(2) 0.803(2) 0.4657(15) 0.031(4) Uani 1 1 d . U . . .
H10A H -0.0838 0.8222 0.4557 0.037 Uiso 1 1 calc R U . . .
C11 C 0.067(2) 0.7779(19) 0.4187(12) 0.022(3) Uani 1 1 d . U . . .
C12 C 0.035(3) 0.773(2) 0.3417(14) 0.032(5) Uani 1 1 d . U . . .
H12A H 0.0610 0.8420 0.3216 0.047 Uiso 1 1 calc R U . . .
H12B H -0.0482 0.7679 0.3301 0.047 Uiso 1 1 calc R U . . .
H12C H 0.0700 0.7076 0.3239 0.047 Uiso 1 1 calc R U . . .
C13 C 0.429(2) 1.007(2) 0.4204(14) 0.031(4) Uani 1 1 d . U . . .
H13A H 0.4547 1.0794 0.4359 0.038 Uiso 1 1 calc R U . . .
C14 C 0.399(2) 0.974(2) 0.3504(14) 0.029(4) Uani 1 1 d . U . . .
H14A H 0.4029 1.0166 0.3105 0.035 Uiso 1 1 calc R U . . .
C15 C 0.363(2) 0.866(2) 0.3560(13) 0.021(3) Uani 1 1 d . U . . .
C16 C 0.322(2) 0.780(2) 0.3061(13) 0.027(3) Uani 1 1 d . U . . .
C17 C 0.305(3) 0.790(3) 0.2352(14) 0.036(5) Uani 1 1 d . U . . .
H17A H 0.3212 0.8566 0.2122 0.044 Uiso 1 1 calc R U . . .
C18 C 0.260(3) 0.689(3) 0.2001(16) 0.042(5) Uani 1 1 d . U . . .
H18A H 0.2491 0.6893 0.1518 0.050 Uiso 1 1 calc R U . . .
C19 C 0.233(3) 0.597(3) 0.2313(14) 0.036(4) Uani 1 1 d . U . . .
H19A H 0.2042 0.5316 0.2068 0.043 Uiso 1 1 calc R U . . .
C20 C 0.250(2) 0.600(2) 0.3034(14) 0.028(4) Uani 1 1 d . U . . .
C21 C 0.186(2) 0.406(2) 0.3309(15) 0.030(4) Uani 1 1 d . U . . .
H21A H 0.1684 0.3724 0.2872 0.036 Uiso 1 1 calc R U . . .
C22 C 0.175(2) 0.357(2) 0.3910(16) 0.033(4) Uani 1 1 d . U . . .
H22A H 0.1446 0.2849 0.3983 0.040 Uiso 1 1 calc R U . . .
C23 C 0.2210(19) 0.440(2) 0.4424(15) 0.026(4) Uani 1 1 d . U . . .
C24 C 0.232(3) 0.421(3) 0.5170(16) 0.040(6) Uani 1 1 d . U . . .
H24A H 0.3100 0.4368 0.5379 0.060 Uiso 1 1 calc R U . . .
H24B H 0.2128 0.3430 0.5259 0.060 Uiso 1 1 calc R U . . .
H24C H 0.1799 0.4718 0.5362 0.060 Uiso 1 1 calc R U . . .
Cl1 Cl 0.4722(7) 1.0129(8) 0.6309(4) 0.046(2) Uani 1 1 d . U . . .
O1 O 0.381(3) 1.075(3) 0.5992(17) 0.084(8) Uani 1 1 d . U . . .
O2 O 0.572(3) 1.071(3) 0.626(2) 0.082(8) Uani 1 1 d . U . . .
O3 O 0.467(3) 0.988(3) 0.7008(14) 0.082(8) Uani 1 1 d . U . . .
O4 O 0.493(3) 0.908(2) 0.5966(13) 0.063(6) Uani 1 1 d . U . . .
Cl2 Cl 0.5899(8) 0.5841(8) 0.2436(5) 0.051(2) Uani 1 1 d . U . . .
O5 O 0.663(4) 0.661(3) 0.2791(19) 0.096(9) Uani 1 1 d . U . . .
O6 O 0.505(3) 0.548(3) 0.2827(15) 0.076(8) Uani 1 1 d . U . . .
O7 O 0.651(3) 0.494(4) 0.232(2) 0.095(10) Uani 1 1 d . U . . .
O8 O 0.534(3) 0.616(3) 0.1810(16) 0.091(9) Uani 1 1 d . U . . .
O1W O 0.3132(19) 0.1803(12) 0.4364(10) 0.0129(19) Uani 1 1 d . 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 N3 1.90(2) . ?
Fe1 N8 1.91(2) . ?
Fe1 N5 1.955(19) . ?
Fe1 N1 1.96(2) . ?
Fe1 N6 1.979(19) . ?
Fe1 N10 1.99(2) . ?
N1 N2 1.35(3) . ?
N1 C3 1.35(3) . ?
N2 C1 1.33(4) . ?
N2 H2B 0.8800 . ?
N3 C8 1.29(4) . ?
N3 C4 1.41(3) . ?
N4 C9 1.34(3) . ?
N4 C8 1.36(3) . ?
N4 N5 1.40(3) . ?
N5 C11 1.33(3) . ?
N6 C15 1.34(3) . ?
N6 N7 1.35(3) . ?
N7 C13 1.28(3) . ?
N7 H7B 0.8800 . ?
N8 C20 1.30(4) . ?
N8 C16 1.36(4) . ?
N9 C21 1.35(3) . ?
N9 N10 1.37(3) . ?
N9 C20 1.39(4) . ?
N10 C23 1.27(3) . ?
C1 C2 1.32(5) . ?
C1 H1A 0.9500 . ?
C2 C3 1.38(4) . ?
C2 H2A 0.9500 . ?
C3 C4 1.45(4) . ?
C4 C5 1.34(4) . ?
C5 C6 1.36(5) . ?
C5 H5A 0.9500 . ?
C6 C7 1.43(5) . ?
C6 H6A 0.9500 . ?
C7 C8 1.43(3) . ?
C7 H7A 0.9500 . ?
C9 C10 1.33(4) . ?
C9 H9A 0.9500 . ?
C10 C11 1.40(4) . ?
C10 H10A 0.9500 . ?
C11 C12 1.52(4) . ?
C12 H12A 0.9800 . ?
C12 H12B 0.9800 . ?
C12 H12C 0.9800 . ?
C13 C14 1.44(4) . ?
C13 H13A 0.9500 . ?
C14 C15 1.36(4) . ?
C14 H14A 0.9500 . ?
C15 C16 1.46(4) . ?
C16 C17 1.40(4) . ?
C17 C18 1.45(5) . ?
C17 H17A 0.9500 . ?
C18 C19 1.33(5) . ?
C18 H18A 0.9500 . ?
C19 C20 1.42(4) . ?
C19 H19A 0.9500 . ?
C21 C22 1.35(4) . ?
C21 H21A 0.9500 . ?
C22 C23 1.46(4) . ?
C22 H22A 0.9500 . ?
C23 C24 1.49(4) . ?
C24 H24A 0.9800 . ?
C24 H24B 0.9800 . ?
C24 H24C 0.9800 . ?
Cl1 O2 1.39(3) . ?
Cl1 O1 1.39(3) . ?
Cl1 O3 1.43(3) . ?
Cl1 O4 1.46(3) . ?
Cl2 O7 1.33(3) . ?
Cl2 O8 1.38(3) . ?
Cl2 O5 1.39(4) . ?
Cl2 O6 1.43(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
N3 Fe1 N8 176.6(10) . . ?
N3 Fe1 N5 79.0(10) . . ?
N8 Fe1 N5 98.2(9) . . ?
N3 Fe1 N1 80.4(10) . . ?
N8 Fe1 N1 102.5(10) . . ?
N5 Fe1 N1 159.3(8) . . ?
N3 Fe1 N6 98.7(9) . . ?
N8 Fe1 N6 79.5(9) . . ?
N5 Fe1 N6 91.0(8) . . ?
N1 Fe1 N6 93.4(9) . . ?
N3 Fe1 N10 101.9(9) . . ?
N8 Fe1 N10 79.9(10) . . ?
N5 Fe1 N10 92.0(8) . . ?
N1 Fe1 N10 91.0(9) . . ?
N6 Fe1 N10 159.4(8) . . ?
N2 N1 C3 104(2) . . ?
N2 N1 Fe1 138.8(18) . . ?
C3 N1 Fe1 116.1(17) . . ?
C1 N2 N1 111(3) . . ?
C1 N2 H2B 124.4 . . ?
N1 N2 H2B 124.4 . . ?
C8 N3 C4 120(2) . . ?
C8 N3 Fe1 120.8(19) . . ?
C4 N3 Fe1 119(2) . . ?
C9 N4 C8 133(2) . . ?
C9 N4 N5 112(2) . . ?
C8 N4 N5 115(2) . . ?
C11 N5 N4 102.7(19) . . ?
C11 N5 Fe1 144.6(17) . . ?
N4 N5 Fe1 112.7(14) . . ?
C15 N6 N7 106(2) . . ?
C15 N6 Fe1 115.3(16) . . ?
N7 N6 Fe1 139.0(16) . . ?
C13 N7 N6 111(2) . . ?
C13 N7 H7B 124.3 . . ?
N6 N7 H7B 124.3 . . ?
C20 N8 C16 121(2) . . ?
C20 N8 Fe1 119(2) . . ?
C16 N8 Fe1 120.1(19) . . ?
C21 N9 N10 111(2) . . ?
C21 N9 C20 133(2) . . ?
N10 N9 C20 117(2) . . ?
C23 N10 N9 107(2) . . ?
C23 N10 Fe1 141(2) . . ?
N9 N10 Fe1 111.7(16) . . ?
C2 C1 N2 107(3) . . ?
C2 C1 H1A 126.6 . . ?
N2 C1 H1A 126.6 . . ?
C1 C2 C3 107(3) . . ?
C1 C2 H2A 126.4 . . ?
C3 C2 H2A 126.4 . . ?
N1 C3 C2 109(3) . . ?
N1 C3 C4 115(2) . . ?
C2 C3 C4 136(3) . . ?
C5 C4 N3 119(3) . . ?
C5 C4 C3 131(3) . . ?
N3 C4 C3 109(2) . . ?
C4 C5 C6 120(3) . . ?
C4 C5 H5A 119.9 . . ?
C6 C5 H5A 119.9 . . ?
C5 C6 C7 124(3) . . ?
C5 C6 H6A 118.1 . . ?
C7 C6 H6A 118.1 . . ?
C8 C7 C6 111(3) . . ?
C8 C7 H7A 124.3 . . ?
C6 C7 H7A 124.3 . . ?
N3 C8 N4 112(2) . . ?
N3 C8 C7 125(3) . . ?
N4 C8 C7 122(2) . . ?
C10 C9 N4 107(2) . . ?
C10 C9 H9A 126.5 . . ?
N4 C9 H9A 126.5 . . ?
C9 C10 C11 107(2) . . ?
C9 C10 H10A 126.5 . . ?
C11 C10 H10A 126.5 . . ?
N5 C11 C10 111(2) . . ?
N5 C11 C12 122(2) . . ?
C10 C11 C12 126(2) . . ?
C11 C12 H12A 109.5 . . ?
C11 C12 H12B 109.5 . . ?
H12A C12 H12B 109.5 . . ?
C11 C12 H12C 109.5 . . ?
H12A C12 H12C 109.5 . . ?
H12B C12 H12C 109.5 . . ?
N7 C13 C14 109(2) . . ?
N7 C13 H13A 125.7 . . ?
C14 C13 H13A 125.7 . . ?
C15 C14 C13 102(2) . . ?
C15 C14 H14A 128.8 . . ?
C13 C14 H14A 128.8 . . ?
N6 C15 C14 112(2) . . ?
N6 C15 C16 115(2) . . ?
C14 C15 C16 133(2) . . ?
N8 C16 C17 122(3) . . ?
N8 C16 C15 110(2) . . ?
C17 C16 C15 128(3) . . ?
C16 C17 C18 114(3) . . ?
C16 C17 H17A 123.0 . . ?
C18 C17 H17A 123.0 . . ?
C19 C18 C17 124(3) . . ?
C19 C18 H18A 118.1 . . ?
C17 C18 H18A 118.1 . . ?
C18 C19 C20 116(3) . . ?
C18 C19 H19A 121.8 . . ?
C20 C19 H19A 121.8 . . ?
N8 C20 N9 113(2) . . ?
N8 C20 C19 123(3) . . ?
N9 C20 C19 124(2) . . ?
C22 C21 N9 107(2) . . ?
C22 C21 H21A 126.5 . . ?
N9 C21 H21A 126.5 . . ?
C21 C22 C23 105(2) . . ?
C21 C22 H22A 127.6 . . ?
C23 C22 H22A 127.6 . . ?
N10 C23 C22 110(3) . . ?
N10 C23 C24 126(2) . . ?
C22 C23 C24 125(2) . . ?
C23 C24 H24A 109.5 . . ?
C23 C24 H24B 109.5 . . ?
H24A C24 H24B 109.5 . . ?
C23 C24 H24C 109.5 . . ?
H24A C24 H24C 109.5 . . ?
H24B C24 H24C 109.5 . . ?
O2 Cl1 O1 109(2) . . ?
O2 Cl1 O3 109(2) . . ?
O1 Cl1 O3 114(2) . . ?
O2 Cl1 O4 101(2) . . ?
O1 Cl1 O4 115(2) . . ?
O3 Cl1 O4 108.0(19) . . ?
O7 Cl2 O8 105(3) . . ?
O7 Cl2 O5 108(3) . . ?
O8 Cl2 O5 118(3) . . ?
O7 Cl2 O6 108(3) . . ?
O8 Cl2 O6 107(2) . . ?
O5 Cl2 O6 111(2) . . ?

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
N2 H2B O6 0.88 2.00 2.82(4) 155.1 .
N7 H7B O4 0.88 1.90 2.78(3) 170.6 .

_refine_diff_density_max         1.997
_refine_diff_density_min         -2.752
_refine_diff_density_rms         0.235

_shelxl_version_number           2014-3



####################################################################### 
# 
# 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_1012bm167
_database_code_depnum_ccdc_archive 'CCDC 1534006'
_audit_update_record             
;
2017-02-21 deposited with the CCDC.
2017-07-04 downloaded from the CCDC.
;

_audit_creation_method           SHELXL-2014
_chemical_name_systematic        
;
 ?
;
_chemical_name_common            ?
_chemical_melting_point          ?
_chemical_formula_moiety         'C26 H26 Fe N10, 2(Cl O4)'
_chemical_formula_sum            'C26 H26 Cl2 Fe N10 O8'
_chemical_formula_weight         733.32

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'
Cl Cl 0.1484 0.1585 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Fe Fe 0.3463 0.8444 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'

_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                   8.3260(5)
_cell_length_b                   38.4690(19)
_cell_length_c                   9.6130(5)
_cell_angle_alpha                90
_cell_angle_beta                 95.768(3)
_cell_angle_gamma                90
_cell_volume                     3063.4(3)
_cell_formula_units_Z            4
_cell_measurement_temperature    298(2)
_cell_measurement_reflns_used    1140
_cell_measurement_theta_min      2.515
_cell_measurement_theta_max      18.779

_exptl_crystal_description       plate
_exptl_crystal_colour            red
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    ?
_exptl_crystal_density_diffrn    1.590
_exptl_crystal_F_000             1504
_exptl_transmission_factor_min   ?
_exptl_transmission_factor_max   ?
_exptl_crystal_size_max          0.151
_exptl_crystal_size_mid          0.103
_exptl_crystal_size_min          0.015
_exptl_absorpt_coefficient_mu    0.733
_shelx_estimated_absorpt_T_min   0.897
_shelx_estimated_absorpt_T_max   0.989
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_correction_T_min  0.653
_exptl_absorpt_correction_T_max  0.745
_exptl_absorpt_process_details   
;
SADABS-2008/1 (Bruker,2008) was used for absorption correction.
wR2(int) was 0.0877 before and 0.0650 after correction.
The Ratio of minimum to maximum transmission is 0.8764.
The λ/2 correction factor is 0.0015.
;

_exptl_special_details           
;
 ?
;

_diffrn_ambient_temperature      298(2)
_diffrn_radiation_wavelength     0.71073
_diffrn_radiation_type           MoK\a
_diffrn_radiation_source         'multilayer monochromator ImuS'
_diffrn_measurement_device_type  'Bruker APEX II QUAZAR'
_diffrn_measurement_method       'φ and ω rotation with narrow frames'
_diffrn_detector_area_resol_mean ?
_diffrn_reflns_number            16899
_diffrn_reflns_av_unetI/netI     0.0766
_diffrn_reflns_av_R_equivalents  0.0902
_diffrn_reflns_limit_h_min       -8
_diffrn_reflns_limit_h_max       8
_diffrn_reflns_limit_k_min       -41
_diffrn_reflns_limit_k_max       38
_diffrn_reflns_limit_l_min       -10
_diffrn_reflns_limit_l_max       10
_diffrn_reflns_theta_min         2.927
_diffrn_reflns_theta_max         22.462
_diffrn_reflns_theta_full        22.465
_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             3964
_reflns_number_gt                2572
_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 APEX 2'
_computing_cell_refinement       'SAINT v8.34A (Bruker, 2013)'
_computing_data_reduction        'SAINT v8.34A (Bruker, 2013)'
_computing_structure_solution    'SHELXT (Sheldrick, 2015)'
_computing_structure_refinement  'SHELXL-2014 (Sheldrick, 2015)'
_computing_molecular_graphics    ?
_computing_publication_material  ?

_refine_special_details          
;
 All non-hydrogens were refined anisotropically. One of the perchlorate
 has 3 of its oxygens disordered over two positions with relative 
 occupancies 0.553:0.447. These were refine with 1,2 and 1,3 distance
 restraints as well as displacement parameters restraints. The other 
 perchlorate also shows some thermal disorder, but only required
 displacement parameters restraints. Hydrogens were placed geometrically
 on their carrier atom and refined with a riding model except those
 on the pyrazole N that were refined freely with their thermal parameter
 1.2 times that of their carrier N and a distance restraint. 
;

_vrf_THETM01_1012bm167           
;
PROBLEM:  The value of sine(theta_max)/wavelength is less than 0.550
            Calculated sin(theta_max)/wavelength =    0.5376
RESPONSE: Diffraction decreased significantly at resolutions better
than 0.95 angstrom and the present data were cut at 0.93 angstrom
where I/sigma(I) was below 2. This poor diffraction results in poor
thetamax and thetafull values, as well as a poor data over parameters ratio.
;

_vrf_REFNR01_1012bm167           
;
PROBLEM:  Ratio of reflections to parameters is < 10 for a
            centrosymmetric structure
            sine(theta)/lambda                0.5376
            Proportion of unique data used    1.0000
            Ratio reflections to parameters   8.4161
RESPONSE: Diffraction decreased significantly at resolutions better
than 0.95 angstrom and the present data were cut at 0.93 angstrom
where I/sigma(I) was below 2. This poor diffraction results in poor
thetamax and thetafull values, as well as a poor data over parameters ratio.
;

_vrf_PLAT088_1012bm167           
;
PROBLEM:  Poor Data / Parameter Ratio ....................       8.42 Note  
RESPONSE: Diffraction decreased significantly at resolutions better
than 0.95 angstrom and the present data were cut at 0.93 angstrom
where I/sigma(I) was below 2. This poor diffraction results in poor
thetamax and thetafull values, as well as a poor data over parameters ratio.
;

_refine_ls_structure_factor_coef Fsqd
_refine_ls_matrix_type           full
_refine_ls_weighting_scheme      calc
_refine_ls_weighting_details     
'w=1/[σ²(Fo²)+(0.0884P)²+2.3311P] where P=(Fo²+2Fc²)/3'
_atom_sites_solution_primary     ?
_atom_sites_solution_secondary   ?
_atom_sites_solution_hydrogens   mixed
_refine_ls_hydrogen_treatment    mixed
_refine_ls_extinction_method     none
_refine_ls_extinction_coef       .
_refine_ls_number_reflns         3964
_refine_ls_number_parameters     471
_refine_ls_number_restraints     197
_refine_ls_R_factor_all          0.1004
_refine_ls_R_factor_gt           0.0591
_refine_ls_wR_factor_ref         0.1749
_refine_ls_wR_factor_gt          0.1483
_refine_ls_goodness_of_fit_ref   1.019
_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 0.26758(10) 0.62525(2) 0.41146(9) 0.0391(3) Uani 1 1 d . . . . .
N1 N 0.0604(6) 0.63215(13) 0.4935(5) 0.0425(13) Uani 1 1 d . . . . .
N2 N 0.0368(6) 0.66615(13) 0.5328(5) 0.0437(13) Uani 1 1 d . . . . .
N3 N 0.2770(6) 0.67417(12) 0.4468(5) 0.0394(12) Uani 1 1 d . . . . .
N4 N 0.4751(6) 0.63665(13) 0.3408(5) 0.0420(13) Uani 1 1 d . . . . .
N5 N 0.5885(6) 0.62068(14) 0.2765(6) 0.0505(14) Uani 1 1 d D . . . .
H5 H 0.579(8) 0.5973(6) 0.265(7) 0.061 Uiso 1 1 d D U . . .
N6 N 0.1625(6) 0.62455(13) 0.2188(5) 0.0440(13) Uani 1 1 d . . . . .
N7 N 0.1597(6) 0.59138(14) 0.1585(5) 0.0494(14) Uani 1 1 d . . . . .
N8 N 0.2655(6) 0.57646(12) 0.3753(6) 0.0439(13) Uani 1 1 d . . . . .
N9 N 0.3670(6) 0.60806(14) 0.5924(5) 0.0479(13) Uani 1 1 d . . . . .
N10 N 0.4265(7) 0.62114(16) 0.7166(6) 0.0561(15) Uani 1 1 d D . . . .
H10 H 0.425(8) 0.6440(6) 0.731(7) 0.067 Uiso 1 1 d D U . . .
C1 C -0.0830(8) 0.57594(17) 0.5129(8) 0.065(2) Uani 1 1 d . . . . .
H1A H -0.0748 0.5708 0.4161 0.098 Uiso 1 1 calc R U . . .
H1B H -0.1870 0.5689 0.5374 0.098 Uiso 1 1 calc R U . . .
H1C H -0.0003 0.5636 0.5697 0.098 Uiso 1 1 calc R U . . .
C2 C -0.0623(7) 0.61439(17) 0.5371(6) 0.0476(17) Uani 1 1 d . . . . .
C3 C -0.1636(8) 0.6368(2) 0.6023(7) 0.0593(19) Uani 1 1 d . . . . .
H3 H -0.2578 0.6305 0.6404 0.071 Uiso 1 1 calc R U . . .
C4 C -0.1003(8) 0.6690(2) 0.5999(7) 0.0550(18) Uani 1 1 d . . . . .
C5 C -0.1614(9) 0.7025(2) 0.6540(8) 0.078(2) Uani 1 1 d . . . . .
H5A H -0.0798 0.7126 0.7192 0.117 Uiso 1 1 calc R U . . .
H5B H -0.2565 0.6981 0.7000 0.117 Uiso 1 1 calc R U . . .
H5C H -0.1872 0.7182 0.5774 0.117 Uiso 1 1 calc R U . . .
C6 C 0.1564(7) 0.69030(16) 0.5019(6) 0.0413(15) Uani 1 1 d . . . . .
C7 C 0.1542(8) 0.72549(17) 0.5196(7) 0.0528(17) Uani 1 1 d . . . . .
H7 H 0.0685 0.7364 0.5567 0.063 Uiso 1 1 calc R U . . .
C8 C 0.2822(8) 0.74411(17) 0.4808(7) 0.0580(18) Uani 1 1 d . . . . .
H8 H 0.2828 0.7681 0.4913 0.070 Uiso 1 1 calc R U . . .
C9 C 0.4110(8) 0.72809(17) 0.4263(7) 0.0535(18) Uani 1 1 d . . . . .
H9 H 0.4988 0.7409 0.4019 0.064 Uiso 1 1 calc R U . . .
C10 C 0.4047(7) 0.69283(16) 0.4097(6) 0.0413(15) Uani 1 1 d . . . . .
C11 C 0.5177(7) 0.67042(16) 0.3474(6) 0.0417(15) Uani 1 1 d . . . . .
C12 C 0.6589(8) 0.67527(18) 0.2830(7) 0.0557(18) Uani 1 1 d . . . . .
H12 H 0.7129 0.6961 0.2716 0.067 Uiso 1 1 calc R U . . .
C13 C 0.7007(8) 0.6432(2) 0.2404(7) 0.062(2) Uani 1 1 d . . . . .
H13 H 0.7906 0.6377 0.1946 0.074 Uiso 1 1 calc R U . . .
C14 C 0.0860(9) 0.68375(18) 0.1389(7) 0.064(2) Uani 1 1 d . . . . .
H14A H 0.0243 0.6875 0.2167 0.097 Uiso 1 1 calc R U . . .
H14B H 0.0310 0.6940 0.0564 0.097 Uiso 1 1 calc R U . . .
H14C H 0.1905 0.6942 0.1580 0.097 Uiso 1 1 calc R U . . .
C15 C 0.1049(7) 0.64538(18) 0.1163(7) 0.0473(17) Uani 1 1 d . . . . .
C16 C 0.0672(8) 0.6266(2) -0.0073(7) 0.063(2) Uani 1 1 d . . . . .
H16 H 0.0257 0.6357 -0.0931 0.076 Uiso 1 1 calc R U . . .
C17 C 0.1022(9) 0.5927(2) 0.0205(7) 0.063(2) Uani 1 1 d . . . . .
C18 C 0.0865(11) 0.5619(2) -0.0742(8) 0.089(3) Uani 1 1 d . . . . .
H18A H 0.1885 0.5501 -0.0711 0.134 Uiso 1 1 calc R U . . .
H18B H 0.0544 0.5694 -0.1681 0.134 Uiso 1 1 calc R U . . .
H18C H 0.0067 0.5463 -0.0442 0.134 Uiso 1 1 calc R U . . .
C19 C 0.2097(8) 0.56447(17) 0.2503(7) 0.0481(16) Uani 1 1 d . . . . .
C20 C 0.1997(9) 0.5292(2) 0.2227(9) 0.071(2) Uani 1 1 d . . . . .
H20 H 0.1602 0.5210 0.1349 0.085 Uiso 1 1 calc R U . . .
C21 C 0.2496(10) 0.5068(2) 0.3282(10) 0.076(2) Uani 1 1 d . . . . .
H21 H 0.2423 0.4830 0.3123 0.091 Uiso 1 1 calc R U . . .
C22 C 0.3097(9) 0.51858(19) 0.4562(9) 0.072(2) Uani 1 1 d . . . . .
H22 H 0.3433 0.5031 0.5274 0.086 Uiso 1 1 calc R U . . .
C23 C 0.3203(8) 0.55431(17) 0.4791(8) 0.0535(18) Uani 1 1 d . . . . .
C24 C 0.3806(7) 0.57294(17) 0.6049(7) 0.0505(17) Uani 1 1 d . . . . .
C25 C 0.4477(9) 0.5647(2) 0.7397(8) 0.072(2) Uani 1 1 d . . . . .
H25 H 0.4689 0.5426 0.7764 0.087 Uiso 1 1 calc R U . . .
C26 C 0.4755(9) 0.5954(2) 0.8057(8) 0.073(2) Uani 1 1 d . . . . .
H26 H 0.5208 0.5983 0.8974 0.088 Uiso 1 1 calc R U . . .
Cl1 Cl 0.3629(2) 0.70964(5) 0.86078(19) 0.0657(5) Uani 1 1 d . U . . .
O1 O 0.3404(9) 0.74524(16) 0.8315(7) 0.129(2) Uani 1 1 d . U . . .
O2 O 0.4646(8) 0.69567(18) 0.7694(7) 0.122(2) Uani 1 1 d . U . . .
O3 O 0.2131(8) 0.69177(19) 0.8317(6) 0.121(2) Uani 1 1 d . U . . .
O4 O 0.4264(7) 0.70468(16) 1.0001(6) 0.1043(18) Uani 1 1 d . U . . .
Cl2 Cl 0.7009(2) 0.53892(5) 0.1425(2) 0.0735(6) Uani 1 1 d D U . . .
O5 O 0.7833(17) 0.5697(3) 0.1224(15) 0.099(4) Uani 0.553(10) 1 d D U P A 1
O6 O 0.6246(18) 0.5243(4) 0.0237(12) 0.142(4) Uani 0.553(10) 1 d D U P A 1
O7 O 0.8184(14) 0.5136(3) 0.2033(14) 0.118(3) Uani 0.553(10) 1 d D U P A 1
O8 O 0.5957(12) 0.5438(2) 0.2517(12) 0.086(3) Uani 0.553(10) 1 d D U P A 1
O55 O 0.8252(17) 0.5656(4) 0.1784(16) 0.081(4) Uani 0.447(10) 1 d D U P A 2
O66 O 0.7164(17) 0.5285(4) -0.0012(11) 0.106(4) Uani 0.447(10) 1 d D U P A 2
O77 O 0.730(2) 0.5108(3) 0.2288(16) 0.121(4) Uani 0.447(10) 1 d D U P A 2
O88 O 0.5454(12) 0.5543(3) 0.1438(17) 0.101(3) Uani 0.447(10) 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 N8 1.909(5) . ?
Fe1 N3 1.912(5) . ?
Fe1 N9 1.965(5) . ?
Fe1 N6 1.968(5) . ?
Fe1 N4 1.968(5) . ?
Fe1 N1 1.985(5) . ?
N1 C2 1.331(7) . ?
N1 N2 1.381(6) . ?
N2 C4 1.371(8) . ?
N2 C6 1.415(7) . ?
N3 C6 1.335(7) . ?
N3 C10 1.359(7) . ?
N4 N5 1.330(7) . ?
N4 C11 1.347(7) . ?
N5 C13 1.343(8) . ?
N5 H5 0.91(2) . ?
N6 C15 1.322(7) . ?
N6 N7 1.401(7) . ?
N7 C17 1.365(8) . ?
N7 C19 1.396(8) . ?
N8 C19 1.327(8) . ?
N8 C23 1.356(8) . ?
N9 N10 1.343(7) . ?
N9 C24 1.360(8) . ?
N10 C26 1.345(9) . ?
N10 H10 0.89(2) . ?
C1 C2 1.505(9) . ?
C1 H1A 0.9600 . ?
C1 H1B 0.9600 . ?
C1 H1C 0.9600 . ?
C2 C3 1.396(9) . ?
C3 C4 1.348(9) . ?
C3 H3 0.9300 . ?
C4 C5 1.497(9) . ?
C5 H5A 0.9600 . ?
C5 H5B 0.9600 . ?
C5 H5C 0.9600 . ?
C6 C7 1.364(8) . ?
C7 C8 1.367(9) . ?
C7 H7 0.9300 . ?
C8 C9 1.385(9) . ?
C8 H8 0.9300 . ?
C9 C10 1.366(8) . ?
C9 H9 0.9300 . ?
C10 C11 1.450(8) . ?
C11 C12 1.395(8) . ?
C12 C13 1.357(9) . ?
C12 H12 0.9300 . ?
C13 H13 0.9300 . ?
C14 C15 1.502(9) . ?
C14 H14A 0.9600 . ?
C14 H14B 0.9600 . ?
C14 H14C 0.9600 . ?
C15 C16 1.399(9) . ?
C16 C17 1.357(9) . ?
C16 H16 0.9300 . ?
C17 C18 1.493(10) . ?
C18 H18A 0.9600 . ?
C18 H18B 0.9600 . ?
C18 H18C 0.9600 . ?
C19 C20 1.385(9) . ?
C20 C21 1.363(10) . ?
C20 H20 0.9300 . ?
C21 C22 1.359(10) . ?
C21 H21 0.9300 . ?
C22 C23 1.393(9) . ?
C22 H22 0.9300 . ?
C23 C24 1.451(9) . ?
C24 C25 1.395(9) . ?
C25 C26 1.351(10) . ?
C25 H25 0.9300 . ?
C26 H26 0.9300 . ?
Cl1 O2 1.388(6) . ?
Cl1 O4 1.403(5) . ?
Cl1 O1 1.407(6) . ?
Cl1 O3 1.427(6) . ?
Cl2 O77 1.370(10) . ?
Cl2 O6 1.371(9) . ?
Cl2 O5 1.392(9) . ?
Cl2 O88 1.425(9) . ?
Cl2 O8 1.446(8) . ?
Cl2 O66 1.457(10) . ?
Cl2 O7 1.460(9) . ?
Cl2 O55 1.475(12) . ?

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
N8 Fe1 N3 178.1(2) . . ?
N8 Fe1 N9 79.9(2) . . ?
N3 Fe1 N9 99.7(2) . . ?
N8 Fe1 N6 79.6(2) . . ?
N3 Fe1 N6 100.8(2) . . ?
N9 Fe1 N6 159.5(2) . . ?
N8 Fe1 N4 98.5(2) . . ?
N3 Fe1 N4 79.6(2) . . ?
N9 Fe1 N4 94.2(2) . . ?
N6 Fe1 N4 90.04(19) . . ?
N8 Fe1 N1 102.2(2) . . ?
N3 Fe1 N1 79.6(2) . . ?
N9 Fe1 N1 89.9(2) . . ?
N6 Fe1 N1 93.11(19) . . ?
N4 Fe1 N1 159.3(2) . . ?
C2 N1 N2 105.4(5) . . ?
C2 N1 Fe1 141.4(5) . . ?
N2 N1 Fe1 112.8(3) . . ?
C4 N2 N1 110.6(5) . . ?
C4 N2 C6 133.1(6) . . ?
N1 N2 C6 116.2(5) . . ?
C6 N3 C10 119.8(5) . . ?
C6 N3 Fe1 120.6(4) . . ?
C10 N3 Fe1 119.5(4) . . ?
N5 N4 C11 105.7(5) . . ?
N5 N4 Fe1 138.3(4) . . ?
C11 N4 Fe1 115.8(4) . . ?
N4 N5 C13 111.5(6) . . ?
N4 N5 H5 117(4) . . ?
C13 N5 H5 132(4) . . ?
C15 N6 N7 104.7(5) . . ?
C15 N6 Fe1 141.9(5) . . ?
N7 N6 Fe1 112.9(4) . . ?
C17 N7 C19 134.0(6) . . ?
C17 N7 N6 110.9(6) . . ?
C19 N7 N6 115.0(5) . . ?
C19 N8 C23 120.6(6) . . ?
C19 N8 Fe1 120.2(4) . . ?
C23 N8 Fe1 119.2(5) . . ?
N10 N9 C24 105.9(5) . . ?
N10 N9 Fe1 138.2(4) . . ?
C24 N9 Fe1 115.9(4) . . ?
N9 N10 C26 110.6(6) . . ?
N9 N10 H10 120(5) . . ?
C26 N10 H10 129(5) . . ?
C2 C1 H1A 109.5 . . ?
C2 C1 H1B 109.5 . . ?
H1A C1 H1B 109.5 . . ?
C2 C1 H1C 109.5 . . ?
H1A C1 H1C 109.5 . . ?
H1B C1 H1C 109.5 . . ?
N1 C2 C3 110.0(6) . . ?
N1 C2 C1 122.4(6) . . ?
C3 C2 C1 127.6(6) . . ?
C4 C3 C2 107.7(6) . . ?
C4 C3 H3 126.1 . . ?
C2 C3 H3 126.1 . . ?
C3 C4 N2 106.2(6) . . ?
C3 C4 C5 129.7(6) . . ?
N2 C4 C5 124.1(7) . . ?
C4 C5 H5A 109.5 . . ?
C4 C5 H5B 109.5 . . ?
H5A C5 H5B 109.5 . . ?
C4 C5 H5C 109.5 . . ?
H5A C5 H5C 109.5 . . ?
H5B C5 H5C 109.5 . . ?
N3 C6 C7 122.1(6) . . ?
N3 C6 N2 110.6(5) . . ?
C7 C6 N2 127.3(6) . . ?
C6 C7 C8 117.7(6) . . ?
C6 C7 H7 121.1 . . ?
C8 C7 H7 121.1 . . ?
C7 C8 C9 121.6(6) . . ?
C7 C8 H8 119.2 . . ?
C9 C8 H8 119.2 . . ?
C10 C9 C8 117.6(6) . . ?
C10 C9 H9 121.2 . . ?
C8 C9 H9 121.2 . . ?
N3 C10 C9 121.1(6) . . ?
N3 C10 C11 110.6(5) . . ?
C9 C10 C11 128.3(6) . . ?
N4 C11 C12 109.8(6) . . ?
N4 C11 C10 114.5(5) . . ?
C12 C11 C10 135.7(6) . . ?
C13 C12 C11 105.4(6) . . ?
C13 C12 H12 127.3 . . ?
C11 C12 H12 127.3 . . ?
N5 C13 C12 107.6(6) . . ?
N5 C13 H13 126.2 . . ?
C12 C13 H13 126.2 . . ?
C15 C14 H14A 109.5 . . ?
C15 C14 H14B 109.5 . . ?
H14A C14 H14B 109.5 . . ?
C15 C14 H14C 109.5 . . ?
H14A C14 H14C 109.5 . . ?
H14B C14 H14C 109.5 . . ?
N6 C15 C16 110.7(6) . . ?
N6 C15 C14 121.5(6) . . ?
C16 C15 C14 127.7(6) . . ?
C17 C16 C15 107.7(6) . . ?
C17 C16 H16 126.2 . . ?
C15 C16 H16 126.2 . . ?
C16 C17 N7 106.0(6) . . ?
C16 C17 C18 129.8(7) . . ?
N7 C17 C18 124.3(7) . . ?
C17 C18 H18A 109.5 . . ?
C17 C18 H18B 109.5 . . ?
H18A C18 H18B 109.5 . . ?
C17 C18 H18C 109.5 . . ?
H18A C18 H18C 109.5 . . ?
H18B C18 H18C 109.5 . . ?
N8 C19 C20 121.5(7) . . ?
N8 C19 N7 111.7(6) . . ?
C20 C19 N7 126.7(7) . . ?
C21 C20 C19 118.0(7) . . ?
C21 C20 H20 121.0 . . ?
C19 C20 H20 121.0 . . ?
C22 C21 C20 121.4(7) . . ?
C22 C21 H21 119.3 . . ?
C20 C21 H21 119.3 . . ?
C21 C22 C23 119.0(7) . . ?
C21 C22 H22 120.5 . . ?
C23 C22 H22 120.5 . . ?
N8 C23 C22 119.5(7) . . ?
N8 C23 C24 111.5(6) . . ?
C22 C23 C24 129.0(7) . . ?
N9 C24 C25 109.3(7) . . ?
N9 C24 C23 113.4(6) . . ?
C25 C24 C23 137.2(7) . . ?
C26 C25 C24 105.7(7) . . ?
C26 C25 H25 127.2 . . ?
C24 C25 H25 127.2 . . ?
N10 C26 C25 108.6(7) . . ?
N10 C26 H26 125.7 . . ?
C25 C26 H26 125.7 . . ?
O2 Cl1 O4 110.9(4) . . ?
O2 Cl1 O1 109.1(5) . . ?
O4 Cl1 O1 110.7(4) . . ?
O2 Cl1 O3 105.5(4) . . ?
O4 Cl1 O3 111.1(4) . . ?
O1 Cl1 O3 109.5(5) . . ?
O6 Cl2 O5 115.3(7) . . ?
O77 Cl2 O88 115.4(7) . . ?
O6 Cl2 O8 113.2(7) . . ?
O5 Cl2 O8 109.4(6) . . ?
O77 Cl2 O66 109.2(8) . . ?
O88 Cl2 O66 106.9(7) . . ?
O6 Cl2 O7 107.1(7) . . ?
O5 Cl2 O7 107.7(7) . . ?
O8 Cl2 O7 103.1(6) . . ?
O77 Cl2 O55 109.2(8) . . ?
O88 Cl2 O55 109.0(7) . . ?
O66 Cl2 O55 106.7(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
N10 H10 O2 0.89(2) 2.04(3) 2.924(9) 170(6) .
N5 H5 O8 0.91(2) 2.07(3) 2.967(11) 171(6) .
N5 H5 O88 0.91(2) 2.03(4) 2.861(13) 152(6) .

_refine_diff_density_max         0.406
_refine_diff_density_min         -0.523
_refine_diff_density_rms         0.072

_shelxl_version_number           2014-3



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

data_1097bm246
_database_code_depnum_ccdc_archive 'CCDC 1534004'
_audit_update_record             
;
2017-02-21 deposited with the CCDC.
2017-07-04 downloaded from the CCDC.
;

_audit_creation_method           SHELXL-2014
_chemical_name_systematic        
;
 ?
;
_chemical_name_common            ?
_chemical_melting_point          ?
_chemical_formula_moiety         'C24 H22 Fe N10, 2(Cl O4)'
_chemical_formula_sum            'C24 H22 Cl2 Fe N10 O8'
_chemical_formula_weight         705.26

loop_
_atom_type_symbol
_atom_type_description
_atom_type_scat_dispersion_real
_atom_type_scat_dispersion_imag
_atom_type_scat_source
C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Cl Cl 0.1484 0.1585 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Fe Fe 0.3463 0.8444 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'

_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                   42.2075(12)
_cell_length_b                   8.1769(3)
_cell_length_c                   18.2952(5)
_cell_angle_alpha                90
_cell_angle_beta                 111.307(2)
_cell_angle_gamma                90
_cell_volume                     5882.6(3)
_cell_formula_units_Z            8
_cell_measurement_temperature    300(2)
_cell_measurement_reflns_used    3884
_cell_measurement_theta_min      2.232
_cell_measurement_theta_max      22.902

_exptl_crystal_description       plate
_exptl_crystal_colour            yellow
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    ?
_exptl_crystal_density_diffrn    1.593
_exptl_crystal_F_000             2880
_exptl_transmission_factor_min   ?
_exptl_transmission_factor_max   ?
_exptl_crystal_size_max          0.344
_exptl_crystal_size_mid          0.077
_exptl_crystal_size_min          0.018
_exptl_absorpt_coefficient_mu    0.760
_shelx_estimated_absorpt_T_min   0.780
_shelx_estimated_absorpt_T_max   0.986
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_correction_T_min  0.628
_exptl_absorpt_correction_T_max  0.745
_exptl_absorpt_process_details   
;
SADABS-2008/1 (Bruker,2008) was used for absorption correction.
wR2(int) was 0.1537 before and 0.0498 after correction.
The Ratio of minimum to maximum transmission is 0.8423.
The λ/2 correction factor is 0.0015.
;

_exptl_special_details           
;
 ?
;

_diffrn_ambient_temperature      300(2)
_diffrn_radiation_wavelength     0.71073
_diffrn_radiation_type           MoK\a
_diffrn_radiation_source         'multilayer monochromator ImuS'
_diffrn_measurement_device_type  'Bruker APEX II QUAZAR'
_diffrn_measurement_method       'φ and ω rotation with narrow frames'
_diffrn_detector_area_resol_mean ?
_diffrn_reflns_number            18876
_diffrn_reflns_av_unetI/netI     0.0427
_diffrn_reflns_av_R_equivalents  0.0453
_diffrn_reflns_limit_h_min       -48
_diffrn_reflns_limit_h_max       48
_diffrn_reflns_limit_k_min       -9
_diffrn_reflns_limit_k_max       9
_diffrn_reflns_limit_l_min       -21
_diffrn_reflns_limit_l_max       21
_diffrn_reflns_theta_min         2.233
_diffrn_reflns_theta_max         24.406
_diffrn_reflns_theta_full        24.405
_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             4843
_reflns_number_gt                3391
_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 APEX 2'
_computing_cell_refinement       'SAINT v8.34A (Bruker, 2013)'
_computing_data_reduction        'SAINT v8.34A (Bruker, 2013)'
_computing_structure_solution    'SHELXT (Sheldrick, 2015)'
_computing_structure_refinement  'SHELXL-2014 (Sheldrick, 2015)'
_computing_molecular_graphics    ?
_computing_publication_material  ?

_refine_special_details          
;
 All non-hydrogens were refined anisotropically. Both 
 perchlorates show some thermal disorder, but only required
 displacement parameters restraints. Hydrogens were placed geometrically
 on their carrier atom and refined with a riding model except those
 on the pyrazole N that were refined freely with their thermal parameter
 1.2 times that of their carrier N and a distance restraint.
;

_vrf_THETM01_1097bm246           
;
PROBLEM:  The value of sine(theta_max)/wavelength is less than 0.590
            Calculated sin(theta_max)/wavelength =    0.5814
RESPONSE: Diffraction decreased significantly at resolutions better
than 0.85 angstrom and the present data were cut at 0.86 angstrom
where I/sigma(I) was below 2. This poor diffraction results in poor
thetamax and thetafull values.
;

_vrf_PLAT027_1097bm246           
;
PROBLEM:  _diffrn_reflns_theta_full value (too) Low ......      24.41 Degree
RESPONSE: Diffraction decreased significantly at resolutions better
than 0.85 angstrom and the present data were cut at 0.86 angstrom
where I/sigma(I) was below 2. This poor diffraction results in poor
thetamax and thetafull values.
;


_refine_ls_structure_factor_coef Fsqd
_refine_ls_matrix_type           full
_refine_ls_weighting_scheme      calc
_refine_ls_weighting_details     
'w=1/[σ²(Fo²)+(0.0969P)²+9.2836P] where P=(Fo²+2Fc²)/3'
_atom_sites_solution_primary     ?
_atom_sites_solution_secondary   ?
_atom_sites_solution_hydrogens   mixed
_refine_ls_hydrogen_treatment    mixed
_refine_ls_extinction_method     none
_refine_ls_extinction_coef       .
_refine_ls_number_reflns         4843
_refine_ls_number_parameters     414
_refine_ls_number_restraints     82
_refine_ls_R_factor_all          0.0838
_refine_ls_R_factor_gt           0.0579
_refine_ls_wR_factor_ref         0.1806
_refine_ls_wR_factor_gt          0.1610
_refine_ls_goodness_of_fit_ref   1.051
_refine_ls_restrained_S_all      1.156
_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 0.62581(2) 0.69623(8) 0.71319(3) 0.0465(2) Uani 1 1 d . . . . .
N1 N 0.60879(10) 0.4617(5) 0.6540(2) 0.0619(11) Uani 1 1 d . . . . .
N2 N 0.57425(12) 0.4471(6) 0.6241(2) 0.0703(12) Uani 1 1 d . . . . .
N3 N 0.57189(9) 0.7015(5) 0.6700(2) 0.0567(10) Uani 1 1 d . . . . .
N4 N 0.61181(9) 0.9373(5) 0.7416(2) 0.0543(9) Uani 1 1 d . . . . .
N5 N 0.62787(12) 1.0690(6) 0.7819(2) 0.0731(12) Uani 1 1 d D . . . .
H5 H 0.6507(5) 1.060(8) 0.800(3) 0.088 Uiso 1 1 d D U . . .
N6 N 0.63761(9) 0.6195(5) 0.8354(2) 0.0533(9) Uani 1 1 d . . . . .
N7 N 0.67140(9) 0.5896(5) 0.8743(2) 0.0556(10) Uani 1 1 d . . . . .
N8 N 0.67935(9) 0.6725(5) 0.7637(2) 0.0489(9) Uani 1 1 d . . . . .
N9 N 0.64488(9) 0.7771(5) 0.6230(2) 0.0547(10) Uani 1 1 d . . . . .
N10 N 0.63282(10) 0.8400(6) 0.5498(2) 0.0632(11) Uani 1 1 d D . . . .
H10 H 0.6103(5) 0.847(7) 0.529(3) 0.076 Uiso 1 1 d D U . . .
C1 C 0.65784(19) 0.3018(8) 0.6549(4) 0.095(2) Uani 1 1 d . . . . .
H1A H 0.6665 0.3658 0.6223 0.143 Uiso 1 1 calc R U . . .
H1B H 0.6620 0.1880 0.6491 0.143 Uiso 1 1 calc R U . . .
H1C H 0.6690 0.3335 0.7087 0.143 Uiso 1 1 calc R U . . .
C2 C 0.62096(17) 0.3294(7) 0.6313(3) 0.0747(16) Uani 1 1 d . . . . .
C3 C 0.5941(2) 0.2292(9) 0.5863(4) 0.099(2) Uani 1 1 d . . . . .
H3 H 0.5960 0.1294 0.5639 0.119 Uiso 1 1 calc R U . . .
C4 C 0.5647(2) 0.3050(9) 0.5817(4) 0.094(2) Uani 1 1 d . . . . .
H4 H 0.5427 0.2681 0.5551 0.113 Uiso 1 1 calc R U . . .
C5 C 0.55435(12) 0.5723(8) 0.6353(3) 0.0667(14) Uani 1 1 d . . . . .
C6 C 0.51922(16) 0.5634(11) 0.6128(4) 0.106(3) Uani 1 1 d . . . . .
H6A H 0.5072 0.4707 0.5885 0.128 Uiso 1 1 calc R U . . .
C7 C 0.50299(16) 0.6976(13) 0.6279(5) 0.113(3) Uani 1 1 d . . . . .
H7 H 0.4794 0.6966 0.6131 0.136 Uiso 1 1 calc R U . . .
C8 C 0.52103(14) 0.8332(9) 0.6646(4) 0.089(2) Uani 1 1 d . . . . .
H8 H 0.5100 0.9234 0.6753 0.107 Uiso 1 1 calc R U . . .
C9 C 0.55587(12) 0.8327(7) 0.6852(3) 0.0608(14) Uani 1 1 d . . . . .
C10 C 0.57926(12) 0.9631(7) 0.7270(3) 0.0587(13) Uani 1 1 d . . . . .
C11 C 0.57430(19) 1.1115(9) 0.7573(4) 0.0871(19) Uani 1 1 d . . . . .
H11 H 0.5538 1.1579 0.7545 0.105 Uiso 1 1 calc R U . . .
C12 C 0.6055(2) 1.1738(9) 0.7915(4) 0.095(2) Uani 1 1 d . . . . .
H12 H 0.6108 1.2735 0.8175 0.114 Uiso 1 1 calc R U . . .
C13 C 0.58548(14) 0.6102(9) 0.8660(3) 0.0879(19) Uani 1 1 d . . . . .
H13A H 0.5790 0.7199 0.8480 0.132 Uiso 1 1 calc R U . . .
H13B H 0.5800 0.5897 0.9116 0.132 Uiso 1 1 calc R U . . .
H13C H 0.5734 0.5344 0.8253 0.132 Uiso 1 1 calc R U . . .
C14 C 0.62236(13) 0.5898(7) 0.8859(3) 0.0615(13) Uani 1 1 d . . . . .
C15 C 0.64685(15) 0.5366(8) 0.9580(3) 0.0785(17) Uani 1 1 d . . . . .
H15 H 0.6429 0.5066 1.0029 0.094 Uiso 1 1 calc R U . . .
C16 C 0.67693(15) 0.5378(8) 0.9487(3) 0.0769(16) Uani 1 1 d . . . . .
H16 H 0.6978 0.5087 0.9863 0.092 Uiso 1 1 calc R U . . .
C17 C 0.69419(11) 0.6202(6) 0.8366(3) 0.0530(11) Uani 1 1 d . . . . .
C18 C 0.72907(12) 0.6024(8) 0.8721(3) 0.0731(15) Uani 1 1 d . . . . .
H18 H 0.7391 0.5662 0.9236 0.088 Uiso 1 1 calc R U . . .
C19 C 0.74805(13) 0.6406(8) 0.8279(4) 0.0820(18) Uani 1 1 d . . . . .
H19 H 0.7715 0.6283 0.8495 0.098 Uiso 1 1 calc R U . . .
C20 C 0.73326(12) 0.6971(7) 0.7517(3) 0.0707(15) Uani 1 1 d . . . . .
H20 H 0.7465 0.7240 0.7223 0.085 Uiso 1 1 calc R U . . .
C21 C 0.69871(11) 0.7120(6) 0.7209(3) 0.0537(11) Uani 1 1 d . . . . .
C22 C 0.67852(11) 0.7741(6) 0.6426(3) 0.0539(12) Uani 1 1 d . . . . .
C23 C 0.68763(13) 0.8290(7) 0.5814(3) 0.0644(14) Uani 1 1 d . . . . .
H23 H 0.7094 0.8360 0.5800 0.077 Uiso 1 1 calc R U . . .
C24 C 0.65768(14) 0.8707(7) 0.5235(3) 0.0699(15) Uani 1 1 d . . . . .
H24 H 0.6552 0.9129 0.4745 0.084 Uiso 1 1 calc R U . . .
Cl1 Cl 0.54170(3) 0.8177(2) 0.43537(8) 0.0775(4) Uani 1 1 d . U . . .
O1 O 0.52395(14) 0.7813(8) 0.3571(3) 0.1317(18) Uani 1 1 d . U . . .
O2 O 0.56205(14) 0.9532(8) 0.4411(4) 0.1442(19) Uani 1 1 d . U . . .
O3 O 0.56183(16) 0.6823(8) 0.4733(4) 0.148(2) Uani 1 1 d . U . . .
O4 O 0.51738(15) 0.8424(9) 0.4692(4) 0.155(2) Uani 1 1 d . U . . .
Cl2 Cl 0.71700(3) 1.07855(19) 0.89232(7) 0.0737(4) Uani 1 1 d . U . . .
O5 O 0.70116(11) 1.0342(7) 0.8135(2) 0.1060(14) Uani 1 1 d . U . . .
O6 O 0.70745(15) 0.9719(8) 0.9402(3) 0.1364(18) Uani 1 1 d . U . . .
O7 O 0.75164(12) 1.0514(11) 0.9099(3) 0.179(3) Uani 1 1 d . U . . .
O8 O 0.7074(3) 1.2308(9) 0.9016(5) 0.228(3) Uani 1 1 d . 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 N8 2.117(3) . ?
Fe1 N3 2.121(4) . ?
Fe1 N4 2.175(4) . ?
Fe1 N9 2.184(4) . ?
Fe1 N1 2.191(4) . ?
Fe1 N6 2.197(3) . ?
N1 C2 1.327(7) . ?
N1 N2 1.363(6) . ?
N2 C4 1.374(7) . ?
N2 C5 1.386(7) . ?
N3 C5 1.313(7) . ?
N3 C9 1.350(6) . ?
N4 C10 1.318(6) . ?
N4 N5 1.341(6) . ?
N5 C12 1.331(8) . ?
N5 H5 0.90(2) . ?
N6 C14 1.327(5) . ?
N6 N7 1.365(5) . ?
N7 C16 1.362(6) . ?
N7 C17 1.395(6) . ?
N8 C17 1.323(6) . ?
N8 C21 1.359(6) . ?
N9 C22 1.332(5) . ?
N9 N10 1.351(5) . ?
N10 C24 1.327(6) . ?
N10 H10 0.89(2) . ?
C1 C2 1.474(9) . ?
C1 H1A 0.9600 . ?
C1 H1B 0.9600 . ?
C1 H1C 0.9600 . ?
C2 C3 1.398(9) . ?
C3 C4 1.360(10) . ?
C3 H3 0.9300 . ?
C4 H4 0.9300 . ?
C5 C6 1.389(8) . ?
C6 C7 1.374(11) . ?
C6 H6A 0.9300 . ?
C7 C8 1.374(10) . ?
C7 H7 0.9300 . ?
C8 C9 1.379(7) . ?
C8 H8 0.9300 . ?
C9 C10 1.465(7) . ?
C10 C11 1.381(8) . ?
C11 C12 1.338(9) . ?
C11 H11 0.9300 . ?
C12 H12 0.9300 . ?
C13 C14 1.474(7) . ?
C13 H13A 0.9600 . ?
C13 H13B 0.9600 . ?
C13 H13C 0.9600 . ?
C14 C15 1.416(7) . ?
C15 C16 1.341(8) . ?
C15 H15 0.9300 . ?
C16 H16 0.9300 . ?
C17 C18 1.384(6) . ?
C18 C19 1.366(8) . ?
C18 H18 0.9300 . ?
C19 C20 1.383(8) . ?
C19 H19 0.9300 . ?
C20 C21 1.365(6) . ?
C20 H20 0.9300 . ?
C21 C22 1.466(6) . ?
C22 C23 1.385(6) . ?
C23 C24 1.365(7) . ?
C23 H23 0.9300 . ?
C24 H24 0.9300 . ?
Cl1 O2 1.382(6) . ?
Cl1 O1 1.385(5) . ?
Cl1 O4 1.393(5) . ?
Cl1 O3 1.414(6) . ?
Cl2 O8 1.338(7) . ?
Cl2 O6 1.396(5) . ?
Cl2 O7 1.396(5) . ?
Cl2 O5 1.399(4) . ?

loop_
_geom_angle_atom_site_label_1
_geom_angle_atom_site_label_2
_geom_angle_atom_site_label_3
_geom_angle
_geom_angle_site_symmetry_1
_geom_angle_site_symmetry_3
_geom_angle_publ_flag
N8 Fe1 N3 174.45(15) . . ?
N8 Fe1 N4 108.56(14) . . ?
N3 Fe1 N4 73.91(16) . . ?
N8 Fe1 N9 74.28(13) . . ?
N3 Fe1 N9 110.63(14) . . ?
N4 Fe1 N9 96.48(15) . . ?
N8 Fe1 N1 104.00(15) . . ?
N3 Fe1 N1 73.67(17) . . ?
N4 Fe1 N1 147.45(15) . . ?
N9 Fe1 N1 92.09(15) . . ?
N8 Fe1 N6 73.65(13) . . ?
N3 Fe1 N6 101.59(13) . . ?
N4 Fe1 N6 89.80(14) . . ?
N9 Fe1 N6 147.67(13) . . ?
N1 Fe1 N6 99.50(15) . . ?
C2 N1 N2 106.4(5) . . ?
C2 N1 Fe1 140.6(4) . . ?
N2 N1 Fe1 112.7(3) . . ?
N1 N2 C4 110.6(6) . . ?
N1 N2 C5 119.5(4) . . ?
C4 N2 C5 129.8(6) . . ?
C5 N3 C9 120.1(4) . . ?
C5 N3 Fe1 120.3(4) . . ?
C9 N3 Fe1 119.3(3) . . ?
C10 N4 N5 105.4(4) . . ?
C10 N4 Fe1 116.7(3) . . ?
N5 N4 Fe1 137.1(3) . . ?
C12 N5 N4 110.4(5) . . ?
C12 N5 H5 136(4) . . ?
N4 N5 H5 114(4) . . ?
C14 N6 N7 106.4(4) . . ?
C14 N6 Fe1 140.6(3) . . ?
N7 N6 Fe1 112.9(2) . . ?
C16 N7 N6 110.2(4) . . ?
C16 N7 C17 130.6(4) . . ?
N6 N7 C17 119.2(3) . . ?
C17 N8 C21 119.6(4) . . ?
C17 N8 Fe1 120.6(3) . . ?
C21 N8 Fe1 119.8(3) . . ?
C22 N9 N10 104.7(4) . . ?
C22 N9 Fe1 116.1(3) . . ?
N10 N9 Fe1 139.0(3) . . ?
C24 N10 N9 111.6(4) . . ?
C24 N10 H10 134(3) . . ?
N9 N10 H10 114(3) . . ?
C2 C1 H1A 109.5 . . ?
C2 C1 H1B 109.5 . . ?
H1A C1 H1B 109.5 . . ?
C2 C1 H1C 109.5 . . ?
H1A C1 H1C 109.5 . . ?
H1B C1 H1C 109.5 . . ?
N1 C2 C3 109.8(6) . . ?
N1 C2 C1 121.4(6) . . ?
C3 C2 C1 128.8(6) . . ?
C4 C3 C2 107.2(6) . . ?
C4 C3 H3 126.4 . . ?
C2 C3 H3 126.4 . . ?
C3 C4 N2 106.1(6) . . ?
C3 C4 H4 126.9 . . ?
N2 C4 H4 126.9 . . ?
N3 C5 N2 113.6(4) . . ?
N3 C5 C6 122.6(7) . . ?
N2 C5 C6 123.8(6) . . ?
C7 C6 C5 117.1(7) . . ?
C7 C6 H6A 121.5 . . ?
C5 C6 H6A 121.5 . . ?
C6 C7 C8 121.0(6) . . ?
C6 C7 H7 119.5 . . ?
C8 C7 H7 119.5 . . ?
C7 C8 C9 118.5(6) . . ?
C7 C8 H8 120.7 . . ?
C9 C8 H8 120.7 . . ?
N3 C9 C8 120.7(6) . . ?
N3 C9 C10 113.1(4) . . ?
C8 C9 C10 126.1(6) . . ?
N4 C10 C11 111.0(5) . . ?
N4 C10 C9 116.4(5) . . ?
C11 C10 C9 132.6(5) . . ?
C12 C11 C10 104.8(6) . . ?
C12 C11 H11 127.6 . . ?
C10 C11 H11 127.6 . . ?
N5 C12 C11 108.6(6) . . ?
N5 C12 H12 125.7 . . ?
C11 C12 H12 125.7 . . ?
C14 C13 H13A 109.5 . . ?
C14 C13 H13B 109.5 . . ?
H13A C13 H13B 109.5 . . ?
C14 C13 H13C 109.5 . . ?
H13A C13 H13C 109.5 . . ?
H13B C13 H13C 109.5 . . ?
N6 C14 C15 109.3(4) . . ?
N6 C14 C13 122.9(4) . . ?
C15 C14 C13 127.8(5) . . ?
C16 C15 C14 106.5(5) . . ?
C16 C15 H15 126.7 . . ?
C14 C15 H15 126.7 . . ?
C15 C16 N7 107.6(5) . . ?
C15 C16 H16 126.2 . . ?
N7 C16 H16 126.2 . . ?
N8 C17 C18 122.7(5) . . ?
N8 C17 N7 113.5(4) . . ?
C18 C17 N7 123.8(4) . . ?
C19 C18 C17 116.8(5) . . ?
C19 C18 H18 121.6 . . ?
C17 C18 H18 121.6 . . ?
C18 C19 C20 121.8(5) . . ?
C18 C19 H19 119.1 . . ?
C20 C19 H19 119.1 . . ?
C21 C20 C19 118.0(5) . . ?
C21 C20 H20 121.0 . . ?
C19 C20 H20 121.0 . . ?
N8 C21 C20 121.2(4) . . ?
N8 C21 C22 112.8(4) . . ?
C20 C21 C22 126.1(4) . . ?
N9 C22 C23 111.0(4) . . ?
N9 C22 C21 117.0(4) . . ?
C23 C22 C21 132.0(4) . . ?
C24 C23 C22 104.9(4) . . ?
C24 C23 H23 127.5 . . ?
C22 C23 H23 127.5 . . ?
N10 C24 C23 107.6(5) . . ?
N10 C24 H24 126.2 . . ?
C23 C24 H24 126.2 . . ?
O2 Cl1 O1 109.8(4) . . ?
O2 Cl1 O4 112.8(4) . . ?
O1 Cl1 O4 106.3(4) . . ?
O2 Cl1 O3 110.1(4) . . ?
O1 Cl1 O3 109.9(4) . . ?
O4 Cl1 O3 107.7(4) . . ?
O8 Cl2 O6 109.4(5) . . ?
O8 Cl2 O7 117.3(6) . . ?
O6 Cl2 O7 105.8(4) . . ?
O8 Cl2 O5 108.6(4) . . ?
O6 Cl2 O5 110.3(4) . . ?
O7 Cl2 O5 105.3(3) . . ?

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
N5 H5 O5 0.90(2) 2.06(2) 2.947(7) 166(5) .
N10 H10 O2 0.89(2) 2.26(3) 3.068(7) 151(5) .

_refine_diff_density_max         0.640
_refine_diff_density_min         -0.599
_refine_diff_density_rms         0.069

_shelxl_version_number           2014-3



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

data_1105bm247
_database_code_depnum_ccdc_archive 'CCDC 1534007'
_audit_update_record             
;
2017-02-21 deposited with the CCDC.
2017-07-04 downloaded from the CCDC.
;

_audit_creation_method           SHELXL-2014
_chemical_name_systematic        
;
 ?
;
_chemical_name_common            ?
_chemical_melting_point          ?
_chemical_formula_moiety         'C26 H26 Fe N10, 2(Cl O4)'
_chemical_formula_sum            'C26 H26 Cl2 Fe N10 O8'
_chemical_formula_weight         733.32

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'
Cl Cl 0.1484 0.1585 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Fe Fe 0.3463 0.8444 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'

_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                   8.2654(3)
_cell_length_b                   37.8383(12)
_cell_length_c                   9.5096(3)
_cell_angle_alpha                90
_cell_angle_beta                 96.203(2)
_cell_angle_gamma                90
_cell_volume                     2956.70(17)
_cell_formula_units_Z            4
_cell_measurement_temperature    100(2)
_cell_measurement_reflns_used    5577
_cell_measurement_theta_min      2.409
_cell_measurement_theta_max      28.328

_exptl_crystal_description       plate
_exptl_crystal_colour            red
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    ?
_exptl_crystal_density_diffrn    1.647
_exptl_crystal_F_000             1504
_exptl_transmission_factor_min   ?
_exptl_transmission_factor_max   ?
_exptl_crystal_size_max          0.155
_exptl_crystal_size_mid          0.141
_exptl_crystal_size_min          0.042
_exptl_absorpt_coefficient_mu    0.760
_shelx_estimated_absorpt_T_min   0.891
_shelx_estimated_absorpt_T_max   0.969
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_correction_T_min  0.632
_exptl_absorpt_correction_T_max  0.746
_exptl_absorpt_process_details   
;
SADABS-2008/1 (Bruker,2008) was used for absorption correction.
wR2(int) was 0.0966 before and 0.0567 after correction.
The Ratio of minimum to maximum transmission is 0.8470.
The λ/2 correction factor is 0.0015.
;

_exptl_special_details           
;
 ?
;

_diffrn_ambient_temperature      100(2)
_diffrn_radiation_wavelength     0.71073
_diffrn_radiation_type           MoK\a
_diffrn_radiation_source         'multilayer monochromator ImuS'
_diffrn_measurement_device_type  'Bruker APEX II QUAZAR'
_diffrn_measurement_method       'φ and ω rotation with narrow frames'
_diffrn_detector_area_resol_mean ?
_diffrn_reflns_number            29162
_diffrn_reflns_av_unetI/netI     0.0564
_diffrn_reflns_av_R_equivalents  0.0584
_diffrn_reflns_limit_h_min       -10
_diffrn_reflns_limit_h_max       11
_diffrn_reflns_limit_k_min       -50
_diffrn_reflns_limit_k_max       49
_diffrn_reflns_limit_l_min       -12
_diffrn_reflns_limit_l_max       12
_diffrn_reflns_theta_min         1.076
_diffrn_reflns_theta_max         28.421
_diffrn_reflns_theta_full        27.780
_diffrn_measured_fraction_theta_max 0.994
_diffrn_measured_fraction_theta_full 0.999
_diffrn_reflns_Laue_measured_fraction_max 0.994
_diffrn_reflns_Laue_measured_fraction_full 0.999
_diffrn_reflns_point_group_measured_fraction_max 0.994
_diffrn_reflns_point_group_measured_fraction_full 0.999
_reflns_number_total             7392
_reflns_number_gt                5642
_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 APEX 2'
_computing_cell_refinement       'SAINT v8.34A (Bruker, 2013)'
_computing_data_reduction        'SAINT v8.34A (Bruker, 2013)'
_computing_structure_solution    'SHELXT (Sheldrick, 2015)'
_computing_structure_refinement  'SHELXL-2014 (Sheldrick, 2015)'
_computing_molecular_graphics    ?
_computing_publication_material  ?

_refine_special_details          
;
 All non-hydrogens were refined anisotropically. Hydrogens were 
 placed geometrically on their carrier atom and refined with a 
 riding model. 
;
_refine_ls_structure_factor_coef Fsqd
_refine_ls_matrix_type           full
_refine_ls_weighting_scheme      calc
_refine_ls_weighting_details     
'w=1/[σ²(Fo²)+(0.0370P)²+3.0519P] 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         7392
_refine_ls_number_parameters     428
_refine_ls_number_restraints     0
_refine_ls_R_factor_all          0.0669
_refine_ls_R_factor_gt           0.0462
_refine_ls_wR_factor_ref         0.1066
_refine_ls_wR_factor_gt          0.0969
_refine_ls_goodness_of_fit_ref   1.031
_refine_ls_restrained_S_all      1.031
_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 0.72058(4) 0.37552(2) 0.58219(3) 0.01404(9) Uani 1 1 d . . . . .
N1 N 0.8263(2) 0.37501(5) 0.7778(2) 0.0157(4) Uani 1 1 d . . . . .
N2 N 0.8315(2) 0.40809(5) 0.8408(2) 0.0180(4) Uani 1 1 d . . . . .
N3 N 0.7269(2) 0.42499(5) 0.6212(2) 0.0168(4) Uani 1 1 d . . . . .
N4 N 0.6218(2) 0.39417(5) 0.4000(2) 0.0182(4) Uani 1 1 d . . . . .
N5 N 0.5609(3) 0.38148(6) 0.2731(2) 0.0213(5) Uani 1 1 d . . . . .
H5 H 0.5530 0.3589 0.2515 0.026 Uiso 1 1 calc R U . . .
N6 N 0.9286(2) 0.36872(5) 0.5013(2) 0.0160(4) Uani 1 1 d . . . . .
N7 N 0.9525(2) 0.33398(5) 0.4613(2) 0.0166(4) Uani 1 1 d . . . . .
N8 N 0.7095(2) 0.32598(5) 0.5454(2) 0.0140(4) Uani 1 1 d . . . . .
N9 N 0.5109(2) 0.36428(5) 0.6514(2) 0.0157(4) Uani 1 1 d . . . . .
N10 N 0.3984(2) 0.38081(5) 0.7185(2) 0.0180(4) Uani 1 1 d . . . . .
H10 H 0.3979 0.4037 0.7356 0.022 Uiso 1 1 calc R U . . .
C1 C 0.9023(3) 0.31391(7) 0.8510(3) 0.0216(5) Uani 1 1 d . . . . .
H1A H 0.7942 0.3033 0.8290 0.032 Uiso 1 1 calc R U . . .
H1B H 0.9582 0.3025 0.9352 0.032 Uiso 1 1 calc R U . . .
H1C H 0.9658 0.3105 0.7708 0.032 Uiso 1 1 calc R U . . .
C2 C 0.8847(3) 0.35256(6) 0.8783(3) 0.0179(5) Uani 1 1 d . . . . .
C3 C 0.9261(3) 0.37113(7) 1.0055(3) 0.0245(6) Uani 1 1 d . . . . .
H3 H 0.9696 0.3612 1.0932 0.029 Uiso 1 1 calc R U . . .
C4 C 0.9150(4) 0.43670(8) 1.0783(3) 0.0310(7) Uani 1 1 d . . . . .
H4A H 1.0039 0.4516 1.0518 0.047 Uiso 1 1 calc R U . . .
H4B H 0.9416 0.4282 1.1754 0.047 Uiso 1 1 calc R U . . .
H4C H 0.8143 0.4505 1.0722 0.047 Uiso 1 1 calc R U . . .
C5 C 0.8926(3) 0.40588(7) 0.9800(3) 0.0229(6) Uani 1 1 d . . . . .
C6 C 0.7854(3) 0.43648(6) 0.7502(3) 0.0183(5) Uani 1 1 d . . . . .
C6AA C 0.8339(3) 0.27330(6) 0.4712(3) 0.0185(5) Uani 1 1 d . . . . .
H6AA H 0.9218 0.2619 0.4330 0.022 Uiso 1 1 calc R U . . .
C7 C 0.8004(3) 0.47216(7) 0.7811(3) 0.0227(5) Uani 1 1 d . . . . .
H7 H 0.8416 0.4801 0.8727 0.027 Uiso 1 1 calc R U . . .
C8 C 0.7533(3) 0.49566(7) 0.6740(3) 0.0253(6) Uani 1 1 d . . . . .
H8 H 0.7646 0.5203 0.6919 0.030 Uiso 1 1 calc R U . . .
C9 C 0.6900(3) 0.48429(7) 0.5410(3) 0.0244(6) Uani 1 1 d . . . . .
H9 H 0.6572 0.5007 0.4679 0.029 Uiso 1 1 calc R U . . .
C10 C 0.6760(3) 0.44849(7) 0.5177(3) 0.0206(5) Uani 1 1 d . . . . .
C11 C 0.6131(3) 0.42967(7) 0.3894(3) 0.0195(5) Uani 1 1 d . . . . .
C12 C 0.5443(3) 0.43945(7) 0.2533(3) 0.0248(6) Uani 1 1 d . . . . .
H12 H 0.5238 0.4627 0.2178 0.030 Uiso 1 1 calc R U . . .
C13 C 0.5132(3) 0.40814(7) 0.1831(3) 0.0248(6) Uani 1 1 d . . . . .
H13 H 0.4664 0.4056 0.0880 0.030 Uiso 1 1 calc R U . . .
C14 C 1.0748(3) 0.42548(7) 0.4902(3) 0.0231(6) Uani 1 1 d . . . . .
H14A H 0.9958 0.4387 0.4264 0.035 Uiso 1 1 calc R U . . .
H14B H 1.1853 0.4326 0.4741 0.035 Uiso 1 1 calc R U . . .
H14C H 1.0572 0.4305 0.5885 0.035 Uiso 1 1 calc R U . . .
C15 C 1.0536(3) 0.38687(7) 0.4622(2) 0.0177(5) Uani 1 1 d . . . . .
C16 C 1.1570(3) 0.36417(7) 0.3958(3) 0.0204(5) Uani 1 1 d . . . . .
H16 H 1.2540 0.3708 0.3572 0.024 Uiso 1 1 calc R U . . .
C17 C 1.1567(3) 0.29714(7) 0.3442(3) 0.0259(6) Uani 1 1 d . . . . .
H17A H 1.1804 0.2807 0.4235 0.039 Uiso 1 1 calc R U . . .
H17B H 1.2565 0.3018 0.3004 0.039 Uiso 1 1 calc R U . . .
H17C H 1.0750 0.2867 0.2741 0.039 Uiso 1 1 calc R U . . .
C18 C 1.0928(3) 0.33098(7) 0.3969(3) 0.0190(5) Uani 1 1 d . . . . .
C19 C 0.8315(3) 0.30973(6) 0.4899(2) 0.0154(5) Uani 1 1 d . . . . .
C20 C 0.7033(3) 0.25436(7) 0.5103(3) 0.0208(5) Uani 1 1 d . . . . .
H20 H 0.7017 0.2294 0.4990 0.025 Uiso 1 1 calc R U . . .
C21 C 0.5744(3) 0.27075(7) 0.5658(3) 0.0198(5) Uani 1 1 d . . . . .
H21 H 0.4842 0.2575 0.5910 0.024 Uiso 1 1 calc R U . . .
C22 C 0.5818(3) 0.30698(6) 0.5831(2) 0.0163(5) Uani 1 1 d . . . . .
C23 C 0.4681(3) 0.32987(6) 0.6472(2) 0.0164(5) Uani 1 1 d . . . . .
C24 C 0.3265(3) 0.32482(7) 0.7126(3) 0.0193(5) Uani 1 1 d . . . . .
H24 H 0.2707 0.3032 0.7241 0.023 Uiso 1 1 calc R U . . .
C25 C 0.2858(3) 0.35785(7) 0.7566(3) 0.0201(5) Uani 1 1 d . . . . .
H25 H 0.1947 0.3636 0.8052 0.024 Uiso 1 1 calc R U . . .
Cl1 Cl 0.27887(8) 0.46389(2) 0.84479(7) 0.02571(15) Uani 1 1 d . . . . .
O1 O 0.1833(3) 0.43221(5) 0.8513(3) 0.0414(6) Uani 1 1 d . . . . .
O2 O 0.1824(3) 0.48996(6) 0.7646(3) 0.0478(6) Uani 1 1 d . . . . .
O3 O 0.3264(4) 0.47751(7) 0.9804(3) 0.0696(9) Uani 1 1 d . . . . .
O4 O 0.4149(3) 0.45586(6) 0.7672(3) 0.0516(7) Uani 1 1 d . . . . .
Cl2 Cl 0.63154(7) 0.29019(2) 0.13443(6) 0.02062(14) Uani 1 1 d . . . . .
O5 O 0.7930(2) 0.30454(6) 0.1586(2) 0.0352(5) Uani 1 1 d . . . . .
O6 O 0.5646(2) 0.29604(5) -0.00907(19) 0.0288(4) Uani 1 1 d . . . . .
O7 O 0.6364(3) 0.25319(5) 0.1646(2) 0.0364(5) Uani 1 1 d . . . . .
O8 O 0.5306(2) 0.30766(5) 0.2286(2) 0.0316(5) Uani 1 1 d . . . . .


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

loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
_geom_bond_publ_flag
Fe1 N8 1.907(2) . ?
Fe1 N3 1.908(2) . ?
Fe1 N4 1.965(2) . ?
Fe1 N9 1.966(2) . ?
Fe1 N1 1.9682(19) . ?
Fe1 N6 1.975(2) . ?
N1 C2 1.330(3) . ?
N1 N2 1.386(3) . ?
N2 C5 1.368(3) . ?
N2 C6 1.403(3) . ?
N3 C6 1.341(3) . ?
N3 C10 1.359(3) . ?
N4 N5 1.345(3) . ?
N4 C11 1.348(3) . ?
N5 C13 1.354(3) . ?
N5 H5 0.8800 . ?
N6 C15 1.327(3) . ?
N6 N7 1.389(3) . ?
N7 C18 1.373(3) . ?
N7 C19 1.405(3) . ?
N8 C19 1.337(3) . ?
N8 C22 1.357(3) . ?
N9 N10 1.339(3) . ?
N9 C23 1.348(3) . ?
N10 C25 1.351(3) . ?
N10 H10 0.8800 . ?
C1 C2 1.495(3) . ?
C1 H1A 0.9800 . ?
C1 H1B 0.9800 . ?
C1 H1C 0.9800 . ?
C2 C3 1.408(3) . ?
C3 C5 1.360(4) . ?
C3 H3 0.9500 . ?
C4 C5 1.494(4) . ?
C4 H4A 0.9800 . ?
C4 H4B 0.9800 . ?
C4 H4C 0.9800 . ?
C6 C7 1.384(3) . ?
C6AA C20 1.380(4) . ?
C6AA C19 1.390(3) . ?
C6AA H6AA 0.9500 . ?
C7 C8 1.376(4) . ?
C7 H7 0.9500 . ?
C8 C9 1.385(4) . ?
C8 H8 0.9500 . ?
C9 C10 1.375(3) . ?
C9 H9 0.9500 . ?
C10 C11 1.459(3) . ?
C11 C12 1.406(3) . ?
C12 C13 1.370(4) . ?
C12 H12 0.9500 . ?
C13 H13 0.9500 . ?
C14 C15 1.492(3) . ?
C14 H14A 0.9800 . ?
C14 H14B 0.9800 . ?
C14 H14C 0.9800 . ?
C15 C16 1.409(4) . ?
C16 C18 1.364(4) . ?
C16 H16 0.9500 . ?
C17 C18 1.492(4) . ?
C17 H17A 0.9800 . ?
C17 H17B 0.9800 . ?
C17 H17C 0.9800 . ?
C20 C21 1.385(4) . ?
C20 H20 0.9500 . ?
C21 C22 1.382(3) . ?
C21 H21 0.9500 . ?
C22 C23 1.459(3) . ?
C23 C24 1.396(3) . ?
C24 C25 1.372(4) . ?
C24 H24 0.9500 . ?
C25 H25 0.9500 . ?
Cl1 O3 1.405(2) . ?
Cl1 O2 1.435(2) . ?
Cl1 O1 1.440(2) . ?
Cl1 O4 1.443(2) . ?
Cl2 O7 1.429(2) . ?
Cl2 O6 1.4332(18) . ?
Cl2 O5 1.4362(19) . ?
Cl2 O8 1.448(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
N8 Fe1 N3 178.60(9) . . ?
N8 Fe1 N4 100.61(8) . . ?
N3 Fe1 N4 79.60(8) . . ?
N8 Fe1 N9 79.74(9) . . ?
N3 Fe1 N9 98.86(9) . . ?
N4 Fe1 N9 94.34(8) . . ?
N8 Fe1 N1 99.86(8) . . ?
N3 Fe1 N1 79.96(8) . . ?
N4 Fe1 N1 159.52(8) . . ?
N9 Fe1 N1 89.94(8) . . ?
N8 Fe1 N6 80.04(8) . . ?
N3 Fe1 N6 101.36(9) . . ?
N4 Fe1 N6 89.96(8) . . ?
N9 Fe1 N6 159.77(8) . . ?
N1 Fe1 N6 92.91(8) . . ?
C2 N1 N2 105.94(19) . . ?
C2 N1 Fe1 140.83(17) . . ?
N2 N1 Fe1 112.90(14) . . ?
C5 N2 N1 110.7(2) . . ?
C5 N2 C6 133.5(2) . . ?
N1 N2 C6 115.63(19) . . ?
C6 N3 C10 120.2(2) . . ?
C6 N3 Fe1 119.71(16) . . ?
C10 N3 Fe1 120.05(16) . . ?
N5 N4 C11 106.09(19) . . ?
N5 N4 Fe1 137.95(16) . . ?
C11 N4 Fe1 115.92(16) . . ?
N4 N5 C13 110.9(2) . . ?
N4 N5 H5 124.6 . . ?
C13 N5 H5 124.6 . . ?
C15 N6 N7 106.0(2) . . ?
C15 N6 Fe1 141.14(18) . . ?
N7 N6 Fe1 112.69(15) . . ?
C18 N7 N6 110.62(19) . . ?
C18 N7 C19 133.3(2) . . ?
N6 N7 C19 116.1(2) . . ?
C19 N8 C22 120.1(2) . . ?
C19 N8 Fe1 120.06(16) . . ?
C22 N8 Fe1 119.71(16) . . ?
N10 N9 C23 105.8(2) . . ?
N10 N9 Fe1 137.85(16) . . ?
C23 N9 Fe1 115.93(16) . . ?
N9 N10 C25 111.2(2) . . ?
N9 N10 H10 124.4 . . ?
C25 N10 H10 124.4 . . ?
C2 C1 H1A 109.5 . . ?
C2 C1 H1B 109.5 . . ?
H1A C1 H1B 109.5 . . ?
C2 C1 H1C 109.5 . . ?
H1A C1 H1C 109.5 . . ?
H1B C1 H1C 109.5 . . ?
N1 C2 C3 109.5(2) . . ?
N1 C2 C1 122.3(2) . . ?
C3 C2 C1 128.2(2) . . ?
C5 C3 C2 107.7(2) . . ?
C5 C3 H3 126.2 . . ?
C2 C3 H3 126.2 . . ?
C5 C4 H4A 109.5 . . ?
C5 C4 H4B 109.5 . . ?
H4A C4 H4B 109.5 . . ?
C5 C4 H4C 109.5 . . ?
H4A C4 H4C 109.5 . . ?
H4B C4 H4C 109.5 . . ?
C3 C5 N2 106.1(2) . . ?
C3 C5 C4 129.4(2) . . ?
N2 C5 C4 124.4(2) . . ?
N3 C6 C7 121.7(2) . . ?
N3 C6 N2 111.1(2) . . ?
C7 C6 N2 127.2(2) . . ?
C20 C6AA C19 117.2(2) . . ?
C20 C6AA H6AA 121.4 . . ?
C19 C6AA H6AA 121.4 . . ?
C8 C7 C6 117.5(2) . . ?
C8 C7 H7 121.2 . . ?
C6 C7 H7 121.2 . . ?
C7 C8 C9 121.6(2) . . ?
C7 C8 H8 119.2 . . ?
C9 C8 H8 119.2 . . ?
C10 C9 C8 118.0(2) . . ?
C10 C9 H9 121.0 . . ?
C8 C9 H9 121.0 . . ?
N3 C10 C9 120.9(2) . . ?
N3 C10 C11 109.9(2) . . ?
C9 C10 C11 129.1(2) . . ?
N4 C11 C12 110.1(2) . . ?
N4 C11 C10 114.4(2) . . ?
C12 C11 C10 135.5(2) . . ?
C13 C12 C11 104.9(2) . . ?
C13 C12 H12 127.6 . . ?
C11 C12 H12 127.6 . . ?
N5 C13 C12 108.1(2) . . ?
N5 C13 H13 126.0 . . ?
C12 C13 H13 126.0 . . ?
C15 C14 H14A 109.5 . . ?
C15 C14 H14B 109.5 . . ?
H14A C14 H14B 109.5 . . ?
C15 C14 H14C 109.5 . . ?
H14A C14 H14C 109.5 . . ?
H14B C14 H14C 109.5 . . ?
N6 C15 C16 109.8(2) . . ?
N6 C15 C14 122.5(2) . . ?
C16 C15 C14 127.7(2) . . ?
C18 C16 C15 107.6(2) . . ?
C18 C16 H16 126.2 . . ?
C15 C16 H16 126.2 . . ?
C18 C17 H17A 109.5 . . ?
C18 C17 H17B 109.5 . . ?
H17A C17 H17B 109.5 . . ?
C18 C17 H17C 109.5 . . ?
H17A C17 H17C 109.5 . . ?
H17B C17 H17C 109.5 . . ?
C16 C18 N7 106.0(2) . . ?
C16 C18 C17 129.4(2) . . ?
N7 C18 C17 124.5(2) . . ?
N8 C19 C6AA 121.9(2) . . ?
N8 C19 N7 111.0(2) . . ?
C6AA C19 N7 127.0(2) . . ?
C6AA C20 C21 121.8(2) . . ?
C6AA C20 H20 119.1 . . ?
C21 C20 H20 119.1 . . ?
C22 C21 C20 117.6(2) . . ?
C22 C21 H21 121.2 . . ?
C20 C21 H21 121.2 . . ?
N8 C22 C21 121.3(2) . . ?
N8 C22 C23 110.5(2) . . ?
C21 C22 C23 128.1(2) . . ?
N9 C23 C24 110.4(2) . . ?
N9 C23 C22 114.0(2) . . ?
C24 C23 C22 135.5(2) . . ?
C25 C24 C23 104.8(2) . . ?
C25 C24 H24 127.6 . . ?
C23 C24 H24 127.6 . . ?
N10 C25 C24 107.8(2) . . ?
N10 C25 H25 126.1 . . ?
C24 C25 H25 126.1 . . ?
O3 Cl1 O2 108.67(15) . . ?
O3 Cl1 O1 111.46(17) . . ?
O2 Cl1 O1 108.60(15) . . ?
O3 Cl1 O4 113.01(18) . . ?
O2 Cl1 O4 106.97(16) . . ?
O1 Cl1 O4 107.95(13) . . ?
O7 Cl2 O6 109.99(12) . . ?
O7 Cl2 O5 109.46(13) . . ?
O6 Cl2 O5 110.52(12) . . ?
O7 Cl2 O8 109.18(13) . . ?
O6 Cl2 O8 109.26(12) . . ?
O5 Cl2 O8 108.40(13) . . ?

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
N10 H10 O4 0.88 2.00 2.878(3) 175.0 .
N5 H5 O8 0.88 1.96 2.832(3) 172.7 .

_refine_diff_density_max         0.948
_refine_diff_density_min         -0.555
_refine_diff_density_rms         0.084

_shelxl_version_number           2014-3



_exptl_crystal_preparation       ', Magnetic properties'
