# Electronic Supplementary Material (ESI) for Dalton Transactions.
# This journal is © The Royal Society of Chemistry 2018

####################################################################### 
# 
# 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_ma2015-15-c
_database_code_depnum_ccdc_archive 'CCDC 1856876'
_audit_update_record             
;
2018-07-19 deposited with the CCDC.
2018-09-28 downloaded from the CCDC.
;

_audit_creation_date             2015-07-10T20:14:54-00:00
_audit_creation_method           'WinGX routine CIF_UPDATE'

#----------------------------------------------------------------------------#
#                   CHEMICAL INFORMATION                                     #
#----------------------------------------------------------------------------#

_chemical_name_systematic        
;
 ?
;
_chemical_formula_moiety         
;
        C74 H58 Fe2 N14 O8, Cl6 Fe2 O, 3(C2 H3 N)
;
_chemical_formula_sum            'C80 H67 Cl6 Fe4 N17 O9'
_chemical_formula_weight         1846.61

#----------------------------------------------------------------------------#
#                   UNIT CELL INFORMATION                                    #
#----------------------------------------------------------------------------#

_symmetry_cell_setting           monoclinic
_symmetry_space_group_name_H-M   P21/m
_symmetry_space_group_name_Hall  -P2yb
_symmetry_Int_Tables_number      11
loop_
_symmetry_equiv_pos_as_xyz
'x, y, z'
'-x, y+1/2, -z'
'-x, -y, -z'
'x, -y-1/2, z'

_cell_length_a                   12.8448(6)
_cell_length_b                   24.3450(14)
_cell_length_c                   13.5498(7)
_cell_angle_alpha                90
_cell_angle_beta                 110.800(6)
_cell_angle_gamma                90
_cell_volume                     3961.0(4)
_cell_formula_units_Z            2
_cell_measurement_temperature    170(2)
_cell_measurement_reflns_used    4147
_cell_measurement_theta_min      3.62
_cell_measurement_theta_max      24.38

#----------------------------------------------------------------------------#
#                   CRYSTAL INFORMATION                                      #
#----------------------------------------------------------------------------#

_exptl_crystal_description       'rod, axis [1 0 0]'
_exptl_crystal_colour            brown
_exptl_crystal_size_max          0.19
_exptl_crystal_size_mid          0.07
_exptl_crystal_size_min          0.06
_exptl_crystal_density_diffrn    1.548
_exptl_crystal_density_method    'not measured'
_exptl_crystal_F_000             1888
loop_
_exptl_crystal_face_index_h
_exptl_crystal_face_index_k
_exptl_crystal_face_index_l
_exptl_crystal_face_perp_dist
0 -1 0 0.03
1 5 1 0.045
-1 -2 1 0.055
1 0 -4 0.035
-1 0 0 0.08
1 0 0 0.1
0 0 -1 0.04
0 0 1 0.035
0 1 0 0.03
1 6 -2 0.04
-1 0 2 0.045

_exptl_crystal_recrystallization_method 
'from solution in acetonitrile at room temperature,by slow diffusion of diethylether??????????'
_exptl_special_details           
;
 ?
;

#----------------------------------------------------------------------------#
#                   ABSORPTION CORRECTION                                    #
#----------------------------------------------------------------------------#

_exptl_absorpt_coefficient_mu    0.990
_exptl_absorpt_correction_type   analytical
_exptl_absorpt_process_details   
;
CrysAlisPro, Agilent Technologies,
Version 1.171.37.35 (release 13-08-2014 CrysAlis171 .NET)
(compiled Aug 13 2014,18:06:01)
Analytical numeric absorption correction using a multifaceted crystal
model based on expressions derived by R.C. Clark & J.S. Reid.
(Clark, R. C. & Reid, J. S. (1995). Acta Cryst. A51, 887-897)
Empirical absorption correction using spherical harmonics,
implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_absorpt_correction_T_min  0.881
_exptl_absorpt_correction_T_max  0.948

#----------------------------------------------------------------------------#
#                   DATA COLLECTION                                          #
#----------------------------------------------------------------------------#

_diffrn_source                   'Enhance (Mo) X-ray Source'
_diffrn_ambient_temperature      170(2)
_diffrn_radiation_wavelength     0.71073
_diffrn_radiation_type           MoK\a
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_probe          x-ray
_diffrn_detector                 'CCD plate'
_diffrn_detector_area_resol_mean 8.3622
_diffrn_orient_matrix_ub_11      -0.0045842
_diffrn_orient_matrix_ub_12      0.027878
_diffrn_orient_matrix_ub_13      0.0130575
_diffrn_orient_matrix_ub_21      0.0183405
_diffrn_orient_matrix_ub_22      0.0084107
_diffrn_orient_matrix_ub_23      -0.0412408
_diffrn_orient_matrix_ub_31      -0.0559746
_diffrn_orient_matrix_ub_32      0.0004659
_diffrn_orient_matrix_ub_33      -0.0355857
_diffrn_measurement_device       'four-circle diffractometer'
_diffrn_measurement_device_type  'Xcalibur, Sapphire2, large Be window'
_diffrn_measurement_method       'ω scans'
_diffrn_reflns_av_R_equivalents  0.1044
_diffrn_reflns_av_unetI/netI     0.1216
_diffrn_reflns_number            23434
_diffrn_reflns_limit_h_min       -15
_diffrn_reflns_limit_h_max       16
_diffrn_reflns_limit_k_min       -20
_diffrn_reflns_limit_k_max       30
_diffrn_reflns_limit_l_min       -16
_diffrn_reflns_limit_l_max       16
_diffrn_reflns_theta_min         3.31
_diffrn_reflns_theta_max         26.37
_diffrn_reflns_theta_full        26.37
_diffrn_measured_fraction_theta_full 0.997
_diffrn_measured_fraction_theta_max 0.997
_reflns_number_total             8265
_reflns_number_gt                4551
_reflns_threshold_expression     >2σ(I)

#----------------------------------------------------------------------------#
#                   COMPUTER PROGRAMS USED                                   #
#----------------------------------------------------------------------------#

_computing_data_collection       
;
        CrysAlisPro, Agilent Technologies,
        Version 1.171.37.35 (release 13-08-2014 CrysAlis171 .NET)
        (compiled Aug 13 2014,18:06:01)
;
_computing_cell_refinement       
;
        CrysAlisPro, Agilent Technologies,
        Version 1.171.37.35 (release 13-08-2014 CrysAlis171 .NET)
        (compiled Aug 13 2014,18:06:01)
;
_computing_data_reduction        
;
        CrysAlisPro, Agilent Technologies,
        Version 1.171.37.35 (release 13-08-2014 CrysAlis171 .NET)
        (compiled Aug 13 2014,18:06:01)
;
_computing_structure_solution    'SIR-92 (Altomare et al., 1992)'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 2008)'
_computing_molecular_graphics    
;
        ORTEP3 for Windows (Farrugia, 1997)
        MERCURY  (Bruno et al., 2002)
;
_computing_publication_material  
;
        WinGX (Farrugia, 1999)
        PLATON (Spek, 1990-2003)
        enCIFer (Allen et al., 2004)
;

#----------------------------------------------------------------------------#
#                   STRUCTURE SOLUTION
#----------------------------------------------------------------------------#

_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_atom_sites_solution_hydrogens   geom

#----------------------------------------------------------------------------#
#                   REFINEMENT INFORMATION                                   #
#----------------------------------------------------------------------------#

_refine_special_details          
;
 Refinement of F² against ALL reflections.  The weighted R-factor wR and
 goodness of fit S are based on F², conventional R-factors R are based
 on F, with F set to zero for negative F². The threshold expression of
 F² > 2sigma(F²) is used only for calculating R-factors(gt) etc. and is
 not relevant to the choice of reflections for refinement.  R-factors based
 on F² are statistically about twice as large as those based on F, and R-
 factors based on ALL data will be even larger.
;
_refine_ls_structure_factor_coef Fsqd
_refine_ls_matrix_type           full
_refine_ls_weighting_scheme      calc
_refine_ls_weighting_details     
'calc w=1/[σ²(Fo²)+(0.0917P)²+0.0000P] where P=(Fo²+2Fc²)/3'
_refine_ls_hydrogen_treatment    mixed
_refine_ls_extinction_method     none
_refine_ls_number_reflns         8265
_refine_ls_number_parameters     591
_refine_ls_number_restraints     41
_refine_ls_R_factor_all          0.1408
_refine_ls_R_factor_gt           0.0749
_refine_ls_wR_factor_ref         0.2199
_refine_ls_wR_factor_gt          0.1736
_refine_ls_goodness_of_fit_ref   1.026
_refine_ls_restrained_S_all      1.031
_refine_ls_shift/su_max          0
_refine_ls_shift/su_mean         0
_refine_diff_density_max         1.127
_refine_diff_density_min         -0.572
_refine_diff_density_rms         0.104

#----------------------------------------------------------------------------#
#                   ATOMIC TYPES, COORDINATES AND THERMAL PARAMETERS         #
#----------------------------------------------------------------------------#

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 0 '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 0.006 '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'

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_symmetry_multiplicity
_atom_site_calc_flag
_atom_site_refinement_flags
_atom_site_disorder_assembly
_atom_site_disorder_group
C1 C 0.6145(5) 0.3949(3) 0.3973(4) 0.0487(16) Uani 1 1 d . . .
H1A H 0.6726 0.3706 0.3888 0.058 Uiso 1 1 calc R . .
H1B H 0.6207 0.4312 0.367 0.058 Uiso 1 1 calc R . .
C2 C 0.5024(5) 0.3711(2) 0.3388(4) 0.0450(15) Uani 1 1 d . . .
C3 C 0.4812(6) 0.3437(3) 0.2438(5) 0.0584(17) Uani 1 1 d . . .
H3 H 0.5394 0.336 0.2178 0.07 Uiso 1 1 calc R . .
C4 C 0.3729(6) 0.3280(3) 0.1882(5) 0.067(2) Uani 1 1 d . . .
H4 H 0.3544 0.3113 0.1208 0.081 Uiso 1 1 calc R . .
C5 C 0.2938(6) 0.3365(3) 0.2299(4) 0.0582(18) Uani 1 1 d . . .
H5 H 0.2194 0.3256 0.1912 0.07 Uiso 1 1 calc R . .
C6 C 0.3183(5) 0.3610(2) 0.3291(4) 0.0465(15) Uani 1 1 d . . .
C7 C 0.2344(4) 0.3653(2) 0.3800(4) 0.0420(14) Uani 1 1 d . . .
C8 C 0.1436(5) 0.3291(3) 0.3475(5) 0.0542(17) Uani 1 1 d . . .
H8 H 0.1385 0.3028 0.2941 0.065 Uiso 1 1 calc R . .
C9 C 0.0625(5) 0.3307(3) 0.3901(5) 0.0620(19) Uani 1 1 d . . .
H9 H 0.0025 0.3053 0.3668 0.074 Uiso 1 1 calc R . .
C10 C 0.0666(5) 0.3686(3) 0.4670(5) 0.0592(18) Uani 1 1 d . . .
H10 H 0.0095 0.3696 0.4963 0.071 Uiso 1 1 calc R . .
C11 C 0.1547(4) 0.4053(2) 0.5010(4) 0.0420(14) Uani 1 1 d D . .
C12 C 0.2397(4) 0.4031(2) 0.4592(4) 0.0403(14) Uani 1 1 d . . .
C13 C 0.0822(5) 0.4641(3) 0.6093(5) 0.0458(15) Uani 1 1 d D . .
C14 C 0.1144(5) 0.5067(3) 0.6968(5) 0.0452(15) Uani 1 1 d . . .
C15 C 0.0310(5) 0.5308(3) 0.7241(5) 0.0547(17) Uani 1 1 d . . .
H15 H -0.0443 0.5202 0.6887 0.066 Uiso 1 1 calc R . .
C16 C 0.0560(6) 0.5693(3) 0.8009(6) 0.0593(18) Uani 1 1 d . . .
H16 H -0.001 0.5863 0.8196 0.071 Uiso 1 1 calc R . .
C17 C 0.1668(6) 0.5834(3) 0.8516(5) 0.0589(18) Uani 1 1 d . . .
H17 H 0.1873 0.6106 0.9053 0.071 Uiso 1 1 calc R . .
C18 C 0.2474(5) 0.5570(3) 0.8226(5) 0.0510(16) Uani 1 1 d . . .
C19 C 0.3682(6) 0.5706(3) 0.8819(5) 0.0546(17) Uani 1 1 d D . .
C20 C 0.6130(5) 0.5046(3) 0.8552(4) 0.0453(15) Uani 1 1 d . . .
H20 H 0.571 0.4823 0.7973 0.054 Uiso 1 1 calc R . .
C21 C 0.5579(5) 0.5378(3) 0.9016(4) 0.0458(15) Uani 1 1 d D . .
C22 C 0.6205(5) 0.5702(3) 0.9884(5) 0.0585(18) Uani 1 1 d . . .
H22 H 0.5841 0.5933 1.0225 0.07 Uiso 1 1 calc R . .
C23 C 0.7342(6) 0.5680(3) 1.0232(5) 0.067(2) Uani 1 1 d . . .
H23 H 0.7763 0.5899 1.0818 0.08 Uiso 1 1 calc R . .
C24 C 0.7889(5) 0.5351(3) 0.9758(5) 0.0581(18) Uani 1 1 d . . .
H24 H 0.868 0.5344 1.0014 0.07 Uiso 1 1 calc R . .
C25 C 0.7290(5) 0.5025(2) 0.8902(4) 0.0433(14) Uani 1 1 d . . .
C26 C 0.7848(5) 0.4679(3) 0.8364(4) 0.0478(16) Uani 1 1 d . . .
C27 C 0.8839(5) 0.4388(3) 0.8908(5) 0.0548(17) Uani 1 1 d . . .
H27 H 0.9163 0.4413 0.9656 0.066 Uiso 1 1 calc R . .
C28 C 0.9332(5) 0.4073(3) 0.8369(5) 0.0540(17) Uani 1 1 d . . .
H28 H 1.0002 0.3882 0.8737 0.065 Uiso 1 1 calc R . .
C29 C 0.8857(5) 0.4034(2) 0.7294(5) 0.0478(15) Uani 1 1 d . . .
H29 H 0.9178 0.3807 0.6907 0.057 Uiso 1 1 calc R . .
C30 C 0.7893(5) 0.4333(3) 0.6781(5) 0.0467(15) Uani 1 1 d . . .
C31 C 0.7395(4) 0.4325(3) 0.5586(4) 0.0438(14) Uani 1 1 d . . .
H31A H 0.7261 0.471 0.5333 0.053 Uiso 1 1 calc R . .
H31B H 0.7952 0.4167 0.5316 0.053 Uiso 1 1 calc R . .
C32 C 0.6423(4) 0.3474(2) 0.5633(5) 0.0447(14) Uani 1 1 d . . .
H32A H 0.7212 0.3355 0.5902 0.054 Uiso 1 1 calc R . .
H32B H 0.5988 0.3199 0.5112 0.054 Uiso 1 1 calc R . .
C33 C 0.5995(4) 0.3501(2) 0.6542(4) 0.0441(14) Uani 1 1 d . . .
C34 C 0.6478(5) 0.3229(3) 0.7488(5) 0.0609(18) Uani 1 1 d . . .
H34 H 0.7149 0.3027 0.7631 0.073 Uiso 1 1 calc R . .
C35 C 0.5954(6) 0.3258(3) 0.8226(5) 0.065(2) Uani 1 1 d . . .
H35 H 0.6268 0.3075 0.8885 0.078 Uiso 1 1 calc R . .
C36 C 0.5020(6) 0.3540(3) 0.8010(5) 0.0564(17) Uani 1 1 d . . .
H36 H 0.4648 0.3549 0.8503 0.068 Uiso 1 1 calc R . .
C37 C 0.4592(5) 0.3818(3) 0.7080(4) 0.0470(15) Uani 1 1 d . . .
H37 H 0.3927 0.4024 0.6939 0.056 Uiso 1 1 calc R . .
N1 N 0.6333(4) 0.4012(2) 0.5114(4) 0.0427(12) Uani 1 1 d . . .
N2 N 0.4238(4) 0.37987(19) 0.3799(3) 0.0402(11) Uani 1 1 d . . .
N3 N 0.1645(4) 0.4449(2) 0.5801(4) 0.0427(12) Uani 1 1 d D . .
N4 N 0.2231(4) 0.5195(2) 0.7452(4) 0.0464(12) Uani 1 1 d . . .
N5 N 0.4406(4) 0.5376(2) 0.8609(4) 0.0492(13) Uani 1 1 d D . .
N6 N 0.7390(3) 0.46431(19) 0.7296(3) 0.0403(11) Uani 1 1 d . . .
N7 N 0.5093(4) 0.38080(19) 0.6351(3) 0.0389(11) Uani 1 1 d . . .
O1 O -0.0157(3) 0.44959(19) 0.5705(3) 0.0596(12) Uani 1 1 d . . .
O2 O 0.3924(4) 0.6088(2) 0.9432(4) 0.0754(15) Uani 1 1 d . . .
O3 O 0.3220(3) 0.44079(15) 0.4967(3) 0.0429(10) Uani 1 1 d . . .
O4 O 0.5326(3) 0.50119(16) 0.5991(3) 0.0397(9) Uani 1 1 d D . .
H3N H 0.229(2) 0.4609(17) 0.601(4) 0.048 Uiso 1 1 d D . .
H5N H 0.414(2) 0.5092(14) 0.823(4) 0.048 Uiso 1 1 d D . .
H4W H 0.593(3) 0.489(2) 0.640(4) 0.06 Uiso 1 1 d D . .
O5 O 0.1627(4) 0.25 0.9646(4) 0.0619(18) Uani 1 2 d S . .
Cl1 Cl 0.41589(17) 0.25 0.95963(17) 0.0613(7) Uani 1 2 d S . .
Cl2 Cl 0.18652(14) 0.17551(7) 0.76870(12) 0.0608(5) Uani 1 1 d . . .
Cl3 Cl -0.09204(18) 0.25 0.80313(17) 0.0695(8) Uani 1 2 d S . .
Cl4 Cl -0.00264(18) 0.32144(9) 1.05472(14) 0.0906(7) Uani 1 1 d . . .
Fe1 Fe 0.47186(6) 0.43880(4) 0.50547(6) 0.0395(3) Uani 1 1 d . . .
Fe2 Fe 0.23244(10) 0.25 0.87129(9) 0.0486(4) Uani 1 2 d S . .
Fe3 Fe 0.02775(9) 0.25 0.96869(9) 0.0437(3) Uani 1 2 d S . .
C38 C 0.3806(8) 0.25 0.5334(8) 0.054(2) Uani 1 2 d SD . .
C39 C 0.3027(8) 0.25 0.5906(8) 0.068(3) Uani 1 2 d SD . .
N8 N 0.4403(7) 0.25 0.4884(7) 0.072(3) Uani 1 2 d S . .
H39A H 0.279(6) 0.2880(12) 0.594(6) 0.107 Uiso 0.5 1 d PD . .
H39B H 0.343(4) 0.236(3) 0.662(3) 0.107 Uiso 0.5 1 d PD . .
H39C H 0.240(4) 0.226(3) 0.554(5) 0.107 Uiso 0.5 1 d PD . .
C40 C 0.2411(12) 0.7175(8) 0.7766(15) 0.091(6) Uani 0.5 1 d PD . .
C41 C 0.2630(12) 0.75 0.8695(13) 0.143(6) Uani 1 2 d SD . .
N9 N 0.2217(14) 0.6927(11) 0.7036(15) 0.162(9) Uani 0.5 1 d P . .
H41A H 0.239(6) 0.7878(15) 0.848(5) 0.243 Uiso 0.5 1 d PD . .
H41B H 0.344(2) 0.75 0.909(5) 0.243 Uiso 1 2 d SD . .
H41C H 0.222(6) 0.735(3) 0.912(4) 0.243 Uiso 0.5 1 d PD . .
C42 C 0.8780(16) 0.2741(8) 0.5086(17) 0.095(6) Uani 0.5 1 d PD . .
C43 C 0.8131(15) 0.2971(9) 0.4575(17) 0.132(9) Uani 0.5 1 d PD . .
N10 N 0.9642(15) 0.25 0.5701(11) 0.170(6) Uani 1 2 d S . .
H43A H 0.745(3) 0.287(2) 0.472(4) 0.254 Uiso 0.5 1 d PD . .
H43B H 0.804(5) 0.287(4) 0.385(2) 0.254 Uiso 0.5 1 d PD . .
H43C H 0.829(2) 0.3360(11) 0.471(6) 0.254 Uiso 0.5 1 d PD . .



#----------------------------------------------------------------------------#
#                   MOLECULAR GEOMETRY                                       #
#----------------------------------------------------------------------------#

_geom_special_details            
;
 All esds (except the esd in the dihedral angle between two l.s. planes)
 are estimated using the full covariance matrix.  The cell esds are taken
 into account individually in the estimation of esds in distances, angles
 and torsion angles; correlations between esds in cell parameters are only
 used when they are defined by crystal symmetry.  An approximate (isotropic)
 treatment of cell esds is used for estimating esds involving l.s. planes.
;
loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
_geom_bond_publ_flag
C1 N1 1.486(6) . ?
C1 C2 1.492(8) . ?
C1 H1A 0.99 . ?
C1 H1B 0.99 . ?
C2 N2 1.333(7) . ?
C2 C3 1.389(8) . ?
C3 C4 1.380(9) . ?
C3 H3 0.95 . ?
C4 C5 1.343(9) . ?
C4 H4 0.95 . ?
C5 C6 1.400(8) . ?
C5 H5 0.95 . ?
C6 N2 1.364(7) . ?
C6 C7 1.474(8) . ?
C7 C12 1.397(8) . ?
C7 C8 1.401(8) . ?
C8 C9 1.359(9) . ?
C8 H8 0.95 . ?
C9 C10 1.379(9) . ?
C9 H9 0.95 . ?
C10 C11 1.385(8) . ?
C10 H10 0.95 . ?
C11 C12 1.398(8) . ?
C11 N3 1.415(7) . ?
C12 O3 1.356(6) . ?
C13 O1 1.230(6) . ?
C13 N3 1.338(7) . ?
C13 C14 1.519(8) . ?
C14 N4 1.352(7) . ?
C14 C15 1.381(8) . ?
C15 C16 1.353(9) . ?
C15 H15 0.95 . ?
C16 C17 1.387(9) . ?
C16 H16 0.95 . ?
C17 C18 1.388(8) . ?
C17 H17 0.95 . ?
C18 N4 1.341(8) . ?
C18 C19 1.510(9) . ?
C19 O2 1.212(7) . ?
C19 N5 1.335(8) . ?
C20 C21 1.365(8) . ?
C20 C25 1.395(7) . ?
C20 H20 0.95 . ?
C21 C22 1.407(8) . ?
C21 N5 1.408(7) . ?
C22 C23 1.368(9) . ?
C22 H22 0.95 . ?
C23 C24 1.367(9) . ?
C23 H23 0.95 . ?
C24 C25 1.389(8) . ?
C24 H24 0.95 . ?
C25 C26 1.458(8) . ?
C26 N6 1.359(7) . ?
C26 C27 1.413(8) . ?
C27 C28 1.362(9) . ?
C27 H27 0.95 . ?
C28 C29 1.367(8) . ?
C28 H28 0.95 . ?
C29 C30 1.392(8) . ?
C29 H29 0.95 . ?
C30 N6 1.340(7) . ?
C30 C31 1.516(8) . ?
C31 N1 1.494(6) . ?
C31 H31A 0.99 . ?
C31 H31B 0.99 . ?
C32 N1 1.472(7) . ?
C32 C33 1.519(8) . ?
C32 H32A 0.99 . ?
C32 H32B 0.99 . ?
C33 N7 1.325(7) . ?
C33 C34 1.379(8) . ?
C34 C35 1.391(9) . ?
C34 H34 0.95 . ?
C35 C36 1.322(9) . ?
C35 H35 0.95 . ?
C36 C37 1.362(8) . ?
C36 H36 0.95 . ?
C37 N7 1.357(7) . ?
C37 H37 0.95 . ?
N1 Fe1 2.241(5) . ?
N2 Fe1 2.142(4) . ?
N3 H3N 0.869(18) . ?
N5 H5N 0.856(18) . ?
N7 Fe1 2.170(4) . ?
O3 Fe1 1.886(4) . ?
O4 Fe1 1.955(4) . ?
O4 Fe1 2.022(4) 3_666 ?
O4 H4W 0.83(2) . ?
O5 Fe3 1.754(5) . ?
O5 Fe2 1.790(6) . ?
Cl1 Fe2 2.232(2) . ?
Cl2 Fe2 2.2330(18) . ?
Cl3 Fe3 2.225(2) . ?
Cl4 Fe3 2.204(2) . ?
Fe1 O4 2.022(4) 3_666 ?
Fe2 Cl2 2.2330(18) 4_565 ?
Fe3 Cl4 2.204(2) 4_565 ?
C38 N8 1.136(12) . ?
C38 C39 1.467(15) . ?
C39 H39A 0.98(2) . ?
C39 H39B 0.98(2) . ?
C39 H39C 0.97(2) . ?
C40 N9 1.11(2) . ?
C40 C41 1.43(2) . ?
C40 C40 1.58(4) 4_575 ?
C41 C40 1.43(2) 4_575 ?
C41 H41A 0.98(2) . ?
C41 H41B 0.98(2) . ?
C41 H41C 0.98(2) . ?
C42 C43 1.04(2) . ?
C42 C42 1.18(4) 4_565 ?
C42 N10 1.269(19) . ?
C42 C43 1.94(3) 4_565 ?
C43 C42 1.94(3) 4_565 ?
C43 H43A 0.983(19) . ?
C43 H43B 0.98(2) . ?
C43 H43C 0.97(2) . ?
N10 C42 1.269(19) 4_565 ?

loop_
_geom_angle_atom_site_label_1
_geom_angle_atom_site_label_2
_geom_angle_atom_site_label_3
_geom_angle
_geom_angle_site_symmetry_1
_geom_angle_site_symmetry_3
_geom_angle_publ_flag
N1 C1 C2 111.3(5) . . ?
N1 C1 H1A 109.4 . . ?
C2 C1 H1A 109.4 . . ?
N1 C1 H1B 109.4 . . ?
C2 C1 H1B 109.4 . . ?
H1A C1 H1B 108 . . ?
N2 C2 C3 122.5(5) . . ?
N2 C2 C1 116.6(5) . . ?
C3 C2 C1 120.9(6) . . ?
C4 C3 C2 117.8(6) . . ?
C4 C3 H3 121.1 . . ?
C2 C3 H3 121.1 . . ?
C5 C4 C3 119.7(6) . . ?
C5 C4 H4 120.2 . . ?
C3 C4 H4 120.2 . . ?
C4 C5 C6 121.6(6) . . ?
C4 C5 H5 119.2 . . ?
C6 C5 H5 119.2 . . ?
N2 C6 C5 118.2(6) . . ?
N2 C6 C7 120.1(5) . . ?
C5 C6 C7 121.7(5) . . ?
C12 C7 C8 117.6(6) . . ?
C12 C7 C6 124.1(5) . . ?
C8 C7 C6 118.3(5) . . ?
C9 C8 C7 121.8(6) . . ?
C9 C8 H8 119.1 . . ?
C7 C8 H8 119.1 . . ?
C8 C9 C10 120.7(6) . . ?
C8 C9 H9 119.7 . . ?
C10 C9 H9 119.7 . . ?
C9 C10 C11 119.4(6) . . ?
C9 C10 H10 120.3 . . ?
C11 C10 H10 120.3 . . ?
C10 C11 C12 120.2(6) . . ?
C10 C11 N3 122.3(6) . . ?
C12 C11 N3 117.4(5) . . ?
O3 C12 C7 123.6(5) . . ?
O3 C12 C11 116.1(5) . . ?
C7 C12 C11 120.3(5) . . ?
O1 C13 N3 124.7(6) . . ?
O1 C13 C14 118.9(5) . . ?
N3 C13 C14 116.4(5) . . ?
N4 C14 C15 122.6(6) . . ?
N4 C14 C13 118.9(5) . . ?
C15 C14 C13 118.4(5) . . ?
C16 C15 C14 120.4(6) . . ?
C16 C15 H15 119.8 . . ?
C14 C15 H15 119.8 . . ?
C15 C16 C17 118.3(6) . . ?
C15 C16 H16 120.9 . . ?
C17 C16 H16 120.9 . . ?
C16 C17 C18 118.9(6) . . ?
C16 C17 H17 120.6 . . ?
C18 C17 H17 120.6 . . ?
N4 C18 C17 123.2(6) . . ?
N4 C18 C19 118.4(6) . . ?
C17 C18 C19 118.5(6) . . ?
O2 C19 N5 125.5(6) . . ?
O2 C19 C18 119.9(6) . . ?
N5 C19 C18 114.6(6) . . ?
C21 C20 C25 122.1(5) . . ?
C21 C20 H20 119 . . ?
C25 C20 H20 119 . . ?
C20 C21 C22 118.7(6) . . ?
C20 C21 N5 118.4(5) . . ?
C22 C21 N5 122.9(6) . . ?
C23 C22 C21 119.3(6) . . ?
C23 C22 H22 120.3 . . ?
C21 C22 H22 120.3 . . ?
C24 C23 C22 121.6(6) . . ?
C24 C23 H23 119.2 . . ?
C22 C23 H23 119.2 . . ?
C23 C24 C25 120.2(6) . . ?
C23 C24 H24 119.9 . . ?
C25 C24 H24 119.9 . . ?
C24 C25 C20 118.1(6) . . ?
C24 C25 C26 121.5(5) . . ?
C20 C25 C26 120.4(5) . . ?
N6 C26 C27 119.5(6) . . ?
N6 C26 C25 117.8(5) . . ?
C27 C26 C25 122.7(5) . . ?
C28 C27 C26 120.4(6) . . ?
C28 C27 H27 119.8 . . ?
C26 C27 H27 119.8 . . ?
C27 C28 C29 119.7(6) . . ?
C27 C28 H28 120.2 . . ?
C29 C28 H28 120.2 . . ?
C28 C29 C30 118.4(6) . . ?
C28 C29 H29 120.8 . . ?
C30 C29 H29 120.8 . . ?
N6 C30 C29 122.9(5) . . ?
N6 C30 C31 117.7(5) . . ?
C29 C30 C31 119.4(6) . . ?
N1 C31 C30 116.0(5) . . ?
N1 C31 H31A 108.3 . . ?
C30 C31 H31A 108.3 . . ?
N1 C31 H31B 108.3 . . ?
C30 C31 H31B 108.3 . . ?
H31A C31 H31B 107.4 . . ?
N1 C32 C33 111.1(5) . . ?
N1 C32 H32A 109.4 . . ?
C33 C32 H32A 109.4 . . ?
N1 C32 H32B 109.4 . . ?
C33 C32 H32B 109.4 . . ?
H32A C32 H32B 108 . . ?
N7 C33 C34 121.8(6) . . ?
N7 C33 C32 114.1(5) . . ?
C34 C33 C32 124.1(6) . . ?
C33 C34 C35 118.1(6) . . ?
C33 C34 H34 120.9 . . ?
C35 C34 H34 120.9 . . ?
C36 C35 C34 120.0(6) . . ?
C36 C35 H35 120 . . ?
C34 C35 H35 120 . . ?
C35 C36 C37 120.0(6) . . ?
C35 C36 H36 120 . . ?
C37 C36 H36 120 . . ?
N7 C37 C36 121.6(6) . . ?
N7 C37 H37 119.2 . . ?
C36 C37 H37 119.2 . . ?
C32 N1 C1 111.1(5) . . ?
C32 N1 C31 110.2(4) . . ?
C1 N1 C31 106.5(4) . . ?
C32 N1 Fe1 107.2(3) . . ?
C1 N1 Fe1 101.4(3) . . ?
C31 N1 Fe1 120.0(4) . . ?
C2 N2 C6 120.0(5) . . ?
C2 N2 Fe1 113.1(3) . . ?
C6 N2 Fe1 125.5(4) . . ?
C13 N3 C11 126.5(5) . . ?
C13 N3 H3N 121(2) . . ?
C11 N3 H3N 112(2) . . ?
C18 N4 C14 116.7(5) . . ?
C19 N5 C21 130.1(5) . . ?
C19 N5 H5N 117(2) . . ?
C21 N5 H5N 112(2) . . ?
C30 N6 C26 118.9(5) . . ?
C33 N7 C37 118.4(5) . . ?
C33 N7 Fe1 116.9(4) . . ?
C37 N7 Fe1 123.5(4) . . ?
C12 O3 Fe1 130.4(4) . . ?
Fe1 O4 Fe1 101.60(15) . 3_666 ?
Fe1 O4 H4W 103(4) . . ?
Fe1 O4 H4W 121(4) 3_666 . ?
Fe3 O5 Fe2 140.4(3) . . ?
O3 Fe1 O4 100.60(16) . . ?
O3 Fe1 O4 99.37(15) . 3_666 ?
O4 Fe1 O4 78.40(15) . 3_666 ?
O3 Fe1 N2 88.13(17) . . ?
O4 Fe1 N2 166.38(17) . . ?
O4 Fe1 N2 89.95(16) 3_666 . ?
O3 Fe1 N7 89.73(17) . . ?
O4 Fe1 N7 93.30(16) . . ?
O4 Fe1 N7 168.63(15) 3_666 . ?
N2 Fe1 N7 97.20(17) . . ?
O3 Fe1 N1 157.35(17) . . ?
O4 Fe1 N1 98.20(16) . . ?
O4 Fe1 N1 96.66(16) 3_666 . ?
N2 Fe1 N1 75.96(17) . . ?
N7 Fe1 N1 76.65(17) . . ?
O5 Fe2 Cl1 108.59(18) . . ?
O5 Fe2 Cl2 110.61(10) . . ?
Cl1 Fe2 Cl2 109.21(6) . . ?
O5 Fe2 Cl2 110.61(10) . 4_565 ?
Cl1 Fe2 Cl2 109.21(6) . 4_565 ?
Cl2 Fe2 Cl2 108.59(9) . 4_565 ?
O5 Fe3 Cl4 112.29(12) . . ?
O5 Fe3 Cl4 112.29(12) . 4_565 ?
Cl4 Fe3 Cl4 104.18(13) . 4_565 ?
O5 Fe3 Cl3 107.80(19) . . ?
Cl4 Fe3 Cl3 110.14(7) . . ?
Cl4 Fe3 Cl3 110.14(7) 4_565 . ?
N8 C38 C39 179.5(10) . . ?
C38 C39 H39A 108(3) . . ?
C38 C39 H39B 107(3) . . ?
H39A C39 H39B 111(4) . . ?
C38 C39 H39C 109(3) . . ?
H39A C39 H39C 112(4) . . ?
H39B C39 H39C 110(4) . . ?
N9 C40 C41 178(2) . . ?
N9 C40 C40 123.0(18) . 4_575 ?
C41 C40 C40 56.4(8) . 4_575 ?
C40 C41 C40 67.3(17) . 4_575 ?
C40 C41 H41A 108(4) . . ?
C40 C41 H41A 44(4) 4_575 . ?
C40 C41 H41B 108(4) . . ?
C40 C41 H41B 108(4) 4_575 . ?
H41A C41 H41B 109(5) . . ?
C40 C41 H41C 110(4) . . ?
C40 C41 H41C 138(5) 4_575 . ?
H41A C41 H41C 110(5) . . ?
H41B C41 H41C 112(5) . . ?
C43 C42 C42 122.6(17) . 4_565 ?
C43 C42 N10 174(2) . . ?
C42 C42 N10 62.4(9) 4_565 . ?
C43 C42 C43 96(2) . 4_565 ?
C42 C42 C43 26.8(8) 4_565 4_565 ?
N10 C42 C43 89.1(12) . 4_565 ?
C42 C43 C42 30.7(14) . 4_565 ?
C42 C43 H43A 107(4) . . ?
C42 C43 H43A 91(4) 4_565 . ?
C42 C43 H43B 109(4) . . ?
C42 C43 H43B 91(4) 4_565 . ?
H43A C43 H43B 110(4) . . ?
C42 C43 H43C 109(2) . . ?
C42 C43 H43C 140(2) 4_565 . ?
H43A C43 H43C 110(4) . . ?
H43B C43 H43C 111(5) . . ?
C42 N10 C42 55.2(18) . 4_565 ?

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
N3 H3N O3 0.869(18) 2.20(3) 2.646(6) 111(2) .
O4 H4W N6 0.83(2) 1.93(2) 2.762(5) 175(6) .

#----------------------------------------------------------------------------#
#                   SHELXL.RES FILE                                          #
#----------------------------------------------------------------------------#

_iucr_refine_instruction_details 
;
TITL Compound-4' at 170 K in P2(1)/m (#11 in standard setting)
CELL  0.71073  12.8448  24.3450  13.5498   90.000  110.800   90.000
ZERR     2.00   0.0006   0.0014   0.0007    0.000    0.006    0.000
LATT   1
SYMM  - X, 1/2 + Y, - Z
SFAC  C    H    N    O    CL   FE
UNIT  160  134  34   18   12   8
MERG   2
OMIT    -2   3   2
SHEL  13 0.8
DFIX  0.88 N3 H3N N5 H5N
SADI  0.04 C11 H3N C13 H3N C19 H5N C21 H5N
DFIX  0.98 C39 H39A C39 H39B C39 H39C
DFIX  0.98 C41 H41A C41 H41B C41 H41C
DFIX  0.98 C43 H43A C43 H43B C43 H43C
DANG  1.60 H39A H39B H39A H39C H39B H39C
DANG  1.60 H41A H41B H41A H41C H41B H41C
DANG  1.60 H43A H43B H43A H43C H43B H43C
SADI  0.04 C38 H39A C38 H39B C38 H39C
SADI  0.04 C40 H41A C40 H41B C40 H41C
SADI  0.04 C42 H43A C42 H43B C42 H43C
DFIX  0.85 O4 H4W
HTAB N3  O3
HTAB O4  N6
FMAP   2
PLAN   25
SIZE     0.06   0.07   0.19
ACTA
BOND   $H
BUMP    0.02000
L.S.   4
TEMP  -103.00
WGHT    0.091700
FVAR       0.34416
MOLE    1
C1    1    0.614475    0.394896    0.397293    11.00000    0.05525    0.05976 =
         0.04005   -0.00804    0.02793   -0.00603
AFIX  23
H1A   2    0.672595    0.370635    0.388833    11.00000   -1.20000
H1B   2    0.620747    0.431211    0.366998    11.00000   -1.20000
AFIX   0
C2    1    0.502420    0.371099    0.338806    11.00000    0.05811    0.04154 =
         0.03602   -0.00350    0.01768   -0.00857
C3    1    0.481229    0.343683    0.243751    11.00000    0.07010    0.06425 =
         0.04748   -0.01042    0.02919   -0.00679
AFIX  43
H3    2    0.539375    0.335965    0.217847    11.00000   -1.20000
AFIX   0
C4    1    0.372899    0.328032    0.188207    11.00000    0.09299    0.06552 =
         0.04547   -0.01638    0.02776   -0.01842
AFIX  43
H4    2    0.354381    0.311337    0.120764    11.00000   -1.20000
AFIX   0
C5    1    0.293776    0.336509    0.229928    11.00000    0.06502    0.06271 =
         0.04035   -0.01233    0.01061   -0.01977
AFIX  43
H5    2    0.219383    0.325627    0.191206    11.00000   -1.20000
AFIX   0
C6    1    0.318260    0.361001    0.329124    11.00000    0.05755    0.04181 =
         0.03428   -0.00245    0.00894   -0.00626
C7    1    0.234377    0.365258    0.379968    11.00000    0.03866    0.04778 =
         0.03274    0.00587    0.00443   -0.00079
C8    1    0.143577    0.329126    0.347461    11.00000    0.05324    0.04586 =
         0.05379   -0.01048    0.00718   -0.00772
AFIX  43
H8    2    0.138522    0.302835    0.294141    11.00000   -1.20000
AFIX   0
C9    1    0.062538    0.330674    0.390149    11.00000    0.04858    0.06193 =
         0.06445   -0.00740    0.00632   -0.01739
AFIX  43
H9    2    0.002465    0.305339    0.366832    11.00000   -1.20000
AFIX   0
C10   1    0.066614    0.368638    0.466956    11.00000    0.03976    0.06234 =
         0.07282   -0.01152    0.01683   -0.01596
AFIX  43
H10   2    0.009546    0.369642    0.496271    11.00000   -1.20000
AFIX   0
C11   1    0.154676    0.405291    0.500963    11.00000    0.03453    0.04259 =
         0.04438    0.00219    0.00861   -0.00145
C12   1    0.239678    0.403099    0.459154    11.00000    0.04089    0.04122 =
         0.03287    0.00334    0.00581   -0.00562
C13   1    0.082161    0.464057    0.609300    11.00000    0.04192    0.04980 =
         0.05233    0.00556    0.02480   -0.00390
C14   1    0.114385    0.506725    0.696832    11.00000    0.04668    0.04716 =
         0.04915    0.00494    0.02627   -0.00262
C15   1    0.031019    0.530752    0.724078    11.00000    0.04247    0.06606 =
         0.06330    0.00784    0.02812    0.00611
AFIX  43
H15   2   -0.044275    0.520153    0.688689    11.00000   -1.20000
AFIX   0
C16   1    0.055952    0.569298    0.800882    11.00000    0.06376    0.05637 =
         0.07322   -0.00154    0.04345    0.01003
AFIX  43
H16   2   -0.001026    0.586280    0.819585    11.00000   -1.20000
AFIX   0
C17   1    0.166802    0.583393    0.851618    11.00000    0.07169    0.05685 =
         0.06262   -0.00481    0.04147    0.00673
AFIX  43
H17   2    0.187265    0.610639    0.905309    11.00000   -1.20000
AFIX   0
C18   1    0.247353    0.557009    0.822610    11.00000    0.05793    0.06165 =
         0.03947   -0.00135    0.02462   -0.00374
C19   1    0.368183    0.570640    0.881880    11.00000    0.06604    0.06051 =
         0.04766   -0.01093    0.03304   -0.00786
C20   1    0.612985    0.504636    0.855213    11.00000    0.05195    0.05052 =
         0.03135   -0.00240    0.01209   -0.01205
AFIX  43
H20   2    0.571008    0.482280    0.797283    11.00000   -1.20000
AFIX   0
C21   1    0.557863    0.537823    0.901551    11.00000    0.04836    0.05347 =
         0.03601   -0.00357    0.01543   -0.00549
C22   1    0.620465    0.570201    0.988409    11.00000    0.06693    0.06451 =
         0.04152   -0.01631    0.01596   -0.00670
AFIX  43
H22   2    0.584084    0.593342    1.022504    11.00000   -1.20000
AFIX   0
C23   1    0.734246    0.568006    1.023234    11.00000    0.06697    0.07959 =
         0.03457   -0.02168   -0.00536   -0.01525
AFIX  43
H23   2    0.776344    0.589922    1.081827    11.00000   -1.20000
AFIX   0
C24   1    0.788857    0.535058    0.975807    11.00000    0.05380    0.06688 =
         0.04330   -0.01196    0.00463   -0.00737
AFIX  43
H24   2    0.867954    0.534414    1.001436    11.00000   -1.20000
AFIX   0
C25   1    0.729028    0.502514    0.890244    11.00000    0.04679    0.04495 =
         0.03324    0.00126    0.00802   -0.00246
C26   1    0.784847    0.467917    0.836435    11.00000    0.04734    0.05287 =
         0.03849   -0.00288    0.00949   -0.00858
C27   1    0.883885    0.438840    0.890837    11.00000    0.04435    0.06999 =
         0.04301    0.00646    0.00687   -0.00821
AFIX  43
H27   2    0.916273    0.441304    0.965554    11.00000   -1.20000
AFIX   0
C28   1    0.933198    0.407315    0.836871    11.00000    0.03762    0.06067 =
         0.06269    0.01137    0.01662    0.00394
AFIX  43
H28   2    1.000237    0.388166    0.873671    11.00000   -1.20000
AFIX   0
C29   1    0.885740    0.403357    0.729438    11.00000    0.04567    0.04467 =
         0.05756    0.00516    0.02393   -0.00756
AFIX  43
H29   2    0.917823    0.380702    0.690736    11.00000   -1.20000
AFIX   0
C30   1    0.789343    0.433296    0.678132    11.00000    0.04778    0.04678 =
         0.04996   -0.00659    0.02272   -0.01513
C31   1    0.739548    0.432544    0.558591    11.00000    0.03972    0.04920 =
         0.04750   -0.00094    0.02176   -0.01016
AFIX  23
H31A  2    0.726142    0.470968    0.533312    11.00000   -1.20000
H31B  2    0.795246    0.416738    0.531563    11.00000   -1.20000
AFIX   0
C32   1    0.642335    0.347418    0.563305    11.00000    0.04043    0.04210 =
         0.05385   -0.00854    0.01936   -0.00392
AFIX  23
H32A  2    0.721184    0.335537    0.590151    11.00000   -1.20000
H32B  2    0.598796    0.319905    0.511151    11.00000   -1.20000
AFIX   0
C33   1    0.599494    0.350099    0.654235    11.00000    0.04032    0.04857 =
         0.04370   -0.00366    0.01524   -0.00874
C34   1    0.647757    0.322878    0.748780    11.00000    0.05470    0.06430 =
         0.05950    0.01342    0.01523    0.00484
AFIX  43
H34   2    0.714852    0.302717    0.763108    11.00000   -1.20000
AFIX   0
C35   1    0.595428    0.325772    0.822588    11.00000    0.08569    0.07197 =
         0.04031    0.01756    0.02624    0.00534
AFIX  43
H35   2    0.626794    0.307474    0.888483    11.00000   -1.20000
AFIX   0
C36   1    0.502045    0.353988    0.801029    11.00000    0.07116    0.05959 =
         0.04650    0.00181    0.03087    0.00077
AFIX  43
H36   2    0.464814    0.354876    0.850338    11.00000   -1.20000
AFIX   0
C37   1    0.459223    0.381796    0.708038    11.00000    0.05183    0.05000 =
         0.04298   -0.00349    0.02147   -0.00774
AFIX  43
H37   2    0.392680    0.402396    0.693911    11.00000   -1.20000
AFIX   0
N1    3    0.633283    0.401228    0.511438    11.00000    0.04429    0.04407 =
         0.04609   -0.00530    0.02397   -0.01060
N2    3    0.423799    0.379866    0.379938    11.00000    0.04278    0.04618 =
         0.03011   -0.00504    0.01124   -0.00917
N3    3    0.164504    0.444945    0.580100    11.00000    0.03266    0.04936 =
         0.04938   -0.00285    0.01870   -0.00991
N4    3    0.223122    0.519524    0.745151    11.00000    0.04859    0.05217 =
         0.04349   -0.00053    0.02254   -0.00039
N5    3    0.440622    0.537576    0.860900    11.00000    0.05291    0.05751 =
         0.04005   -0.01952    0.02020   -0.00642
N6    3    0.738961    0.464309    0.729556    11.00000    0.03344    0.04259 =
         0.04222   -0.00416    0.01025   -0.01188
N7    3    0.509261    0.380803    0.635078    11.00000    0.04045    0.04087 =
         0.03482    0.00086    0.01257   -0.00243
O1    4   -0.015735    0.449585    0.570482    11.00000    0.03858    0.07850 =
         0.06703   -0.00939    0.02540   -0.01012
O2    4    0.392376    0.608827    0.943226    11.00000    0.06958    0.08685 =
         0.07750   -0.03344    0.03575   -0.00631
O3    4    0.322022    0.440794    0.496722    11.00000    0.04163    0.04676 =
         0.04045   -0.00555    0.01462   -0.01285
O4    4    0.532618    0.501185    0.599109    11.00000    0.04578    0.04519 =
         0.02519   -0.00216    0.00896   -0.00062
H3N   2    0.229146    0.460948    0.601071    11.00000   -1.20000
H5N   2    0.413969    0.509175    0.823191    11.00000   -1.20000
H4W   2    0.592782    0.489003    0.639924    11.00000   -1.50000
FE1   6    0.471865    0.438801    0.505470    11.00000    0.04050    0.04804 =
         0.03061   -0.00423    0.01336   -0.00736
MOLE    2
O5    4    0.162740    0.250000    0.964609    10.50000    0.03344    0.10948 =
         0.04038    0.00000    0.01024    0.00000
CL1   5    0.415891    0.250000    0.959626    10.50000    0.04323    0.09300 =
         0.05569    0.00000    0.02732    0.00000
CL2   5    0.186517    0.175515    0.768696    11.00000    0.08031    0.05300 =
         0.04797    0.00169    0.02125   -0.00427
CL3   5   -0.092035    0.250000    0.803128    10.50000    0.04721    0.11339 =
         0.04047    0.00000    0.00660    0.00000
CL4   5   -0.002637    0.321444    1.054722    11.00000    0.10788    0.09895 =
         0.05704   -0.01475    0.01948    0.03670
FE2   6    0.232440    0.250000    0.871294    10.50000    0.04695    0.06673 =
         0.03662    0.00000    0.02055    0.00000
FE3   6    0.027751    0.250000    0.968688    10.50000    0.03402    0.06020 =
         0.03668    0.00000    0.01247    0.00000
MOLE    3
C38   1    0.380572    0.250000    0.533392    10.50000    0.05007    0.03565 =
         0.06115    0.00000    0.00144    0.00000
C39   1    0.302735    0.250000    0.590606    10.50000    0.06299    0.08858 =
         0.05584    0.00000    0.02473    0.00000
N8    3    0.440259    0.250000    0.488444    10.50000    0.05914    0.06623 =
         0.09246    0.00000    0.03086    0.00000
H39A  2    0.279377    0.287963    0.594369    10.50000   -1.50000
H39B  2    0.343157    0.235574    0.661571    10.50000   -1.50000
H39C  2    0.239793    0.226415    0.553875    10.50000   -1.50000
MOLE    4
C40   1    0.241087    0.717513    0.776574    10.50000    0.04684    0.14616 =
         0.07349    0.00254    0.01231    0.00654
C41   1    0.263048    0.750000    0.869491    10.50000    0.11723    0.17284 =
         0.11603    0.00000    0.01438    0.00000
N9    3    0.221748    0.692729    0.703563    10.50000    0.09175    0.29220 =
         0.09941   -0.05934    0.03147    0.01678
H41A  2    0.238716    0.787772    0.848188    10.50000   -1.50000
H41B  2    0.343655    0.750000    0.908504    10.50000   -1.50000
H41C  2    0.222147    0.735317    0.912124    10.50000   -1.50000
MOLE    5
C42   1    0.877994    0.274135    0.508631    10.50000    0.07316    0.10553 =
         0.10191    0.01049    0.02666    0.01299
C43   1    0.813099    0.297089    0.457510    10.50000    0.07801    0.20346 =
         0.13082    0.03564    0.05808    0.04034
N10   3    0.964232    0.250000    0.570116    10.50000    0.18875    0.19739 =
         0.10023    0.00000    0.02348    0.00000
H43A  2    0.745395    0.287365    0.471621    10.50000   -1.50000
H43B  2    0.804066    0.287362    0.384811    10.50000   -1.50000
H43C  2    0.829307    0.336050    0.470936    10.50000   -1.50000
HKLF    4
 
REM  MA2015-15-c at 170 K in P2(1)/m (#11 in standard setting)
REM R1 =  0.0749 for   4551 Fo > 4sig(Fo)  and  0.1408 for all   8265 data
REM    591 parameters refined using     41 restraints
 
END
 
WGHT      0.0917      0.0000
REM Highest difference peak  1.127,  deepest hole -0.572,  1-sigma level  0.104
Q1    1   0.0580  0.2500  0.7625  10.50000  0.05    1.13
Q2    1   0.0039  0.2500  1.0267  10.50000  0.05    0.80
Q3    1   0.4380  0.5045  0.5966  11.00000  0.05    0.61
Q4    1  -0.0571  0.2500  0.9616  10.50000  0.05    0.61
Q5    1   0.5000  0.5000  0.5000  10.50000  0.05    0.58
Q6    1   0.0965  0.3233  1.0673  11.00000  0.05    0.56
Q7    1   0.3497  0.2500  0.8820  10.50000  0.05    0.55
Q8    1   0.9209  0.2500  0.6466  10.50000  0.05    0.51
Q9    1   0.0966  0.2500  1.0488  10.50000  0.05    0.51
Q10   1   0.5647  0.4313  0.5044  11.00000  0.05    0.49
Q11   1   0.4738  0.2500  0.9113  10.50000  0.05    0.48
Q12   1   0.0245  0.3001  0.9730  11.00000  0.05    0.45
Q13   1   0.2689  0.1752  0.7703  11.00000  0.05    0.41
Q14   1   0.4407  0.2500  1.0360  10.50000  0.05    0.40
Q15   1   0.4003  0.2881  0.9639  11.00000  0.05    0.38
Q16   1   0.2409  0.1866  0.8563  11.00000  0.05    0.38
Q17   1   0.5801  0.4936  0.8842  11.00000  0.05    0.37
Q18   1  -0.0783  0.2993  0.9972  11.00000  0.05    0.37
Q19   1   0.4952  0.3786  0.4941  11.00000  0.05    0.36
Q20   1  -0.1349  0.2500  0.8694  10.50000  0.05    0.36
Q21   1   0.2213  0.5086  0.6832  11.00000  0.05    0.35
Q22   1   0.2852  0.3634  0.3674  11.00000  0.05    0.34
Q23   1  -0.0916  0.2500  0.7081  10.50000  0.05    0.34
Q24   1   0.3103  0.5630  0.8606  11.00000  0.05    0.34
Q25   1   0.1228  0.2752  0.9499  11.00000  0.05    0.34
;
####################################################################### 
# 
# 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_ma7fecl2-b
_database_code_depnum_ccdc_archive 'CCDC 1856877'
_audit_update_record             
;
2018-07-19 deposited with the CCDC.
2018-09-28 downloaded from the CCDC.
;

_audit_creation_date             2014-06-17T16:54:20-00:00
_audit_creation_method           'WinGX routine CIF_UPDATE'

#----------------------------------------------------------------------------#
#                   CHEMICAL INFORMATION                                     #
#----------------------------------------------------------------------------#


_chemical_name_systematic        
;
 ?
;
_chemical_formula_moiety         'C37 H29 Cl2 Fe N7 O2'
_chemical_formula_sum            'C37 H29 Cl2 Fe N7 O2'
_chemical_formula_weight         730.42
_chemical_absolute_configuration unk

#----------------------------------------------------------------------------#
#                   UNIT CELL INFORMATION                                    #
#----------------------------------------------------------------------------#

_symmetry_cell_setting           monoclinic
_symmetry_space_group_name_H-M   Cc
_symmetry_space_group_name_Hall  C-2yc
_symmetry_Int_Tables_number      9
loop_
_symmetry_equiv_pos_as_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                   15.153(3)
_cell_length_b                   13.630(2)
_cell_length_c                   16.654(3)
_cell_angle_alpha                90
_cell_angle_beta                 107.23(2)
_cell_angle_gamma                90
_cell_volume                     3285.3(10)
_cell_formula_units_Z            4
_cell_measurement_temperature    170(2)
_cell_measurement_reflns_used    1206
_cell_measurement_theta_min      2.8086
_cell_measurement_theta_max      31.6256

#----------------------------------------------------------------------------#
#                   CRYSTAL INFORMATION                                      #
#----------------------------------------------------------------------------#

_exptl_crystal_description       
;
prismatic triangular rod, axis [1 0 0]
;
_exptl_crystal_colour            colourless
_exptl_crystal_size_max          0.17
_exptl_crystal_size_mid          0.06
_exptl_crystal_size_min          0.03
_exptl_crystal_density_diffrn    1.477
_exptl_crystal_density_method    'not measured'
_exptl_crystal_F_000             1504
loop_
_exptl_crystal_face_index_h
_exptl_crystal_face_index_k
_exptl_crystal_face_index_l
_exptl_crystal_face_perp_dist
0 0 -1 0
1 0 0 0.07
-1 0 0 0.09
0 1 0 0.03
0 -1 0 0.03
1 0 -10 0
-1 6 9 0.02
-1 -6 9 0.02

_exptl_crystal_recrystallization_method 
'from solution in dichloromethane at room temperature,by slow diffusion of diethylether'
_exptl_special_details           
;
 ?
;

#----------------------------------------------------------------------------#
#                   ABSORPTION CORRECTION                                    #
#----------------------------------------------------------------------------#

_exptl_absorpt_coefficient_mu    0.669
_exptl_absorpt_correction_type   analytical
_exptl_absorpt_process_details   
;
CrysAlis RED, Oxford Diffraction Ltd.,
Version 1.171.33.52 (release 06-11-2009 CrysAlis171 .NET)
(compiled Nov  6 2009,16:24:50)
Analytical numeric absorption correction using a multifaceted crystal
model based on expressions derived by R.C. Clark & J.S. Reid.
(Clark, R. C. & Reid, J. S. (1995). Acta Cryst. A51, 887-897)
;
_exptl_absorpt_correction_T_min  0.940
_exptl_absorpt_correction_T_max  0.989

#----------------------------------------------------------------------------#
#                   DATA COLLECTION                                          #
#----------------------------------------------------------------------------#

_diffrn_source                   'sealed X-ray tube'
_diffrn_ambient_temperature      170(2)
_diffrn_radiation_wavelength     0.71073
_diffrn_radiation_type           MoK\a
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_probe          X-ray
_diffrn_detector                 'CCD plate'
_diffrn_detector_area_resol_mean 8.3622
_diffrn_orient_matrix_ub_11      0.0102022429
_diffrn_orient_matrix_ub_12      -0.0474240662
_diffrn_orient_matrix_ub_13      0.0182913976
_diffrn_orient_matrix_ub_21      -0.0004261651
_diffrn_orient_matrix_ub_22      -0.0195419029
_diffrn_orient_matrix_ub_23      -0.0397748977
_diffrn_orient_matrix_ub_31      0.0481285025
_diffrn_orient_matrix_ub_32      0.0098606439
_diffrn_orient_matrix_ub_33      0.0093578789
_diffrn_measurement_device       'Kappa-geometry diffractometer'
_diffrn_measurement_device_type  'Xcalibur, Sapphire2, large Be window'
_diffrn_measurement_method       'ω scans'
_diffrn_reflns_av_R_equivalents  0.2004
_diffrn_reflns_av_unetI/netI     0.33
_diffrn_reflns_number            12174
_diffrn_reflns_limit_h_min       -14
_diffrn_reflns_limit_h_max       18
_diffrn_reflns_limit_k_min       -16
_diffrn_reflns_limit_k_max       17
_diffrn_reflns_limit_l_min       -20
_diffrn_reflns_limit_l_max       20
_diffrn_reflns_theta_min         2.81
_diffrn_reflns_theta_max         26.37
_diffrn_reflns_theta_full        26.37
_diffrn_measured_fraction_theta_full 0.998
_diffrn_measured_fraction_theta_max 0.998
_reflns_number_total             4852
_reflns_number_gt                2079
_reflns_threshold_expression     >2sigma(I)

#----------------------------------------------------------------------------#
#                   COMPUTER PROGRAMS USED                                   #
#----------------------------------------------------------------------------#

_computing_data_collection       
;
CrysAlis CCD, Oxford Diffraction Ltd.,
Version 1.171.33.52 (release 06-11-2009 CrysAlis171 .NET)
(compiled Nov  6 2009,16:24:50)
;
_computing_cell_refinement       
;
CrysAlis RED, Oxford Diffraction Ltd.,
Version 1.171.33.52 (release 06-11-2009 CrysAlis171 .NET)
(compiled Nov  6 2009,16:24:50)
;
_computing_data_reduction        
;
CrysAlis RED, Oxford Diffraction Ltd.,
Version 1.171.33.52 (release 06-11-2009 CrysAlis171 .NET)
(compiled Nov  6 2009,16:24:50)
;
_computing_structure_solution    'SIR-92 (Altomare et al., 1992)'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_molecular_graphics    
;
ORTEP3 for Windows (Farrugia, 1997)
MERCURY  (Bruno et al., 2002)
;
_computing_publication_material  
;
WinGX (Farrugia, 1999)
PLATON (Spek, 1990-2003)
enCIFer (Allen et al., 2004)
;

#----------------------------------------------------------------------------#
#                   STRUCTURE SOLUTION
#----------------------------------------------------------------------------#

_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_atom_sites_solution_hydrogens   geom

#----------------------------------------------------------------------------#
#                   REFINEMENT INFORMATION                                   #
#----------------------------------------------------------------------------#

_refine_special_details          
;
 Refinement of F² against ALL reflections.  The weighted R-factor wR and
 goodness of fit S are based on F², conventional R-factors R are based
 on F, with F set to zero for negative F². The threshold expression of
 F² > 2sigma(F²) is used only for calculating R-factors(gt) etc. and is
 not relevant to the choice of reflections for refinement.  R-factors based
 on F² are statistically about twice as large as those based on F, and R-
 factors based on ALL data will be even larger.
;
_refine_ls_structure_factor_coef Fsqd
_refine_ls_matrix_type           full
_refine_ls_weighting_scheme      calc
_refine_ls_weighting_details     
'calc w=1/[σ²(Fo²)+(0.0000P)²+0.0000P] where P=(Fo²+2Fc²)/3'
_refine_ls_hydrogen_treatment    constr
_refine_ls_extinction_method     none
_refine_ls_number_reflns         4852
_refine_ls_number_parameters     432
_refine_ls_number_restraints     134
_refine_ls_R_factor_all          0.1888
_refine_ls_R_factor_gt           0.0769
_refine_ls_wR_factor_ref         0.0969
_refine_ls_wR_factor_gt          0.0771
_refine_ls_goodness_of_fit_ref   0.822
_refine_ls_restrained_S_all      0.813
_refine_ls_shift/su_max          0
_refine_ls_shift/su_mean         0
_refine_ls_abs_structure_details 'Flack H D (1983), Acta Cryst. A39, 876-881'
_refine_ls_abs_structure_Flack   0.03(3)
_refine_diff_density_max         0.37
_refine_diff_density_min         -0.392
_refine_diff_density_rms         0.082

#----------------------------------------------------------------------------#
#                   ATOMIC TYPES, COORDINATES AND THERMAL PARAMETERS         #
#----------------------------------------------------------------------------#

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 0 '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 0.006 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Fe Fe 0.3463 0.8444 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Cl Cl 0.1484 0.1585 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'

loop_
_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_symmetry_multiplicity
_atom_site_calc_flag
_atom_site_refinement_flags
_atom_site_disorder_assembly
_atom_site_disorder_group
C1 C 0.5071(6) 0.8517(7) 0.2867(6) 0.030(3) Uani 1 1 d U . .
H1A H 0.5505 0.8169 0.3345 0.036 Uiso 1 1 calc R . .
H1B H 0.5445 0.8871 0.2563 0.036 Uiso 1 1 calc R . .
C2 C 0.4558(6) 0.9239(8) 0.3202(6) 0.026(2) Uani 1 1 d U . .
C3 C 0.4807(7) 1.0221(7) 0.3287(6) 0.028(3) Uani 1 1 d U . .
H3 H 0.5304 1.0458 0.3104 0.034 Uiso 1 1 calc R . .
C4 C 0.4308(7) 1.0849(8) 0.3647(7) 0.035(3) Uani 1 1 d U . .
H4 H 0.4471 1.1523 0.3721 0.042 Uiso 1 1 calc R . .
C5 C 0.3603(7) 1.0513(7) 0.3889(6) 0.029(3) Uani 1 1 d U . .
H5 H 0.3261 1.095 0.4126 0.035 Uiso 1 1 calc R . .
C6 C 0.3360(7) 0.9516(7) 0.3797(6) 0.024(2) Uani 1 1 d U . .
C7 C 0.2526(6) 0.9131(7) 0.3970(6) 0.017(2) Uiso 1 1 d U . .
C8 C 0.1728(7) 0.9696(7) 0.3781(6) 0.030(3) Uani 1 1 d U . .
H8 H 0.1737 1.0345 0.3577 0.036 Uiso 1 1 calc R . .
C9 C 0.0920(7) 0.9324(8) 0.3887(6) 0.037(3) Uani 1 1 d U . .
H9 H 0.038 0.972 0.3763 0.045 Uiso 1 1 calc R . .
C10 C 0.0901(7) 0.8373(8) 0.4175(6) 0.029(3) Uani 1 1 d U . .
H10 H 0.034 0.8107 0.4224 0.035 Uiso 1 1 calc R . .
C11 C 0.1703(7) 0.7800(7) 0.4395(5) 0.022(2) Uani 1 1 d U . .
C12 C 0.2520(7) 0.8188(7) 0.4309(5) 0.023(2) Uani 1 1 d U . .
H12 H 0.3074 0.7815 0.4479 0.028 Uiso 1 1 calc R . .
C13 C 0.1278(6) 0.6400(7) 0.5158(6) 0.022(2) Uani 1 1 d U . .
C14 C 0.1373(7) 0.5306(7) 0.5240(6) 0.021(2) Uani 1 1 d U . .
C15 C 0.1000(7) 0.4843(8) 0.5781(7) 0.037(3) Uani 1 1 d U . .
H15 H 0.0713 0.5213 0.6117 0.044 Uiso 1 1 calc R . .
C16 C 0.1039(7) 0.3803(8) 0.5847(6) 0.040(3) Uani 1 1 d U . .
H16 H 0.0772 0.3455 0.6212 0.048 Uiso 1 1 calc R . .
C17 C 0.1495(6) 0.3325(7) 0.5341(6) 0.027(2) Uani 1 1 d U . .
H17 H 0.1553 0.2631 0.5363 0.033 Uiso 1 1 calc R . .
C18 C 0.1864(6) 0.3861(6) 0.4806(6) 0.018(2) Uani 1 1 d U . .
C19 C 0.2346(7) 0.3307(8) 0.4268(6) 0.025(3) Uani 1 1 d U . .
C20 C 0.3259(6) 0.4181(7) 0.2593(6) 0.024(2) Uani 1 1 d U . .
H20 H 0.3353 0.4834 0.28 0.029 Uiso 1 1 calc R . .
C21 C 0.2850(6) 0.3512(7) 0.2989(6) 0.021(2) Uani 1 1 d U . .
C22 C 0.2695(6) 0.2537(7) 0.2694(6) 0.027(3) Uani 1 1 d U . .
H22 H 0.2404 0.2072 0.2958 0.033 Uiso 1 1 calc R . .
C23 C 0.2984(6) 0.2280(8) 0.1998(6) 0.035(3) Uani 1 1 d U . .
H23 H 0.2894 0.1628 0.1788 0.042 Uiso 1 1 calc R . .
C24 C 0.3402(6) 0.2965(7) 0.1611(6) 0.027(3) Uani 1 1 d U . .
H24 H 0.3599 0.2776 0.1143 0.032 Uiso 1 1 calc R . .
C25 C 0.3536(7) 0.3931(7) 0.1905(6) 0.023(2) Uani 1 1 d U . .
C26 C 0.3934(6) 0.4682(7) 0.1485(6) 0.020(3) Uiso 1 1 d U . .
C27 C 0.3921(6) 0.4598(7) 0.0647(6) 0.022(2) Uani 1 1 d U . .
H27 H 0.3646 0.4039 0.0332 0.027 Uiso 1 1 calc R . .
C28 C 0.4296(6) 0.5308(8) 0.0277(6) 0.029(3) Uani 1 1 d U . .
H28 H 0.4299 0.5246 -0.0291 0.035 Uiso 1 1 calc R . .
C29 C 0.4674(6) 0.6123(7) 0.0749(6) 0.023(2) Uani 1 1 d U . .
H29 H 0.4929 0.6637 0.0504 0.028 Uiso 1 1 calc R . .
C30 C 0.4678(7) 0.6187(7) 0.1595(7) 0.025(2) Uani 1 1 d U . .
C31 C 0.5125(6) 0.7016(7) 0.2141(6) 0.027(2) Uani 1 1 d U . .
H31A H 0.5489 0.6747 0.2692 0.033 Uiso 1 1 calc R . .
H31B H 0.5564 0.7335 0.1886 0.033 Uiso 1 1 calc R . .
C32 C 0.3992(6) 0.8222(7) 0.1478(6) 0.025(2) Uani 1 1 d U . .
H32A H 0.3888 0.7721 0.1029 0.03 Uiso 1 1 calc R . .
H32B H 0.4375 0.875 0.1345 0.03 Uiso 1 1 calc R . .
C33 C 0.3059(6) 0.8651(7) 0.1487(6) 0.019(2) Uani 1 1 d U . .
C34 C 0.2669(7) 0.9441(7) 0.1005(6) 0.035(3) Uani 1 1 d U . .
H34 H 0.2988 0.9767 0.067 0.042 Uiso 1 1 calc R . .
C35 C 0.1838(7) 0.9748(9) 0.1013(6) 0.048(3) Uani 1 1 d U . .
H35 H 0.1564 1.0301 0.0686 0.057 Uiso 1 1 calc R . .
C36 C 0.1368(7) 0.9261(8) 0.1502(6) 0.038(3) Uani 1 1 d U . .
H36 H 0.0771 0.9464 0.1511 0.046 Uiso 1 1 calc R . .
C37 C 0.1806(6) 0.8476(7) 0.1966(6) 0.027(2) Uani 1 1 d U . .
H37 H 0.1497 0.8136 0.2302 0.032 Uiso 1 1 calc R . .
N1 N 0.4496(5) 0.7772(6) 0.2288(4) 0.0217(17) Uani 1 1 d U . .
N2 N 0.3841(5) 0.8901(6) 0.3445(5) 0.0244(19) Uani 1 1 d U . .
N3 N 0.1701(6) 0.6799(6) 0.4639(5) 0.029(2) Uani 1 1 d U . .
H3A H 0.2019 0.6392 0.4421 0.035 Uiso 1 1 calc R . .
N4 N 0.1801(5) 0.4842(6) 0.4753(5) 0.026(2) Uani 1 1 d U . .
N5 N 0.2502(5) 0.3854(6) 0.3640(4) 0.021(2) Uani 1 1 d U . .
H5A H 0.2375 0.4484 0.3638 0.026 Uiso 1 1 calc R . .
N6 N 0.4280(5) 0.5478(6) 0.1938(5) 0.025(2) Uani 1 1 d U . .
N7 N 0.2643(5) 0.8163(5) 0.1974(5) 0.0244(19) Uani 1 1 d U . .
O1 O 0.0821(4) 0.6867(5) 0.5520(5) 0.036(2) Uani 1 1 d U . .
O2 O 0.2494(4) 0.2448(5) 0.4370(4) 0.038(2) Uani 1 1 d U . .
Fe1 Fe 0.35137(10) 0.73114(9) 0.29921(9) 0.0248(4) Uani 1 1 d U . .
Cl1 Cl 0.22490(17) 0.62802(17) 0.29638(16) 0.0289(7) Uani 1 1 d U . .
Cl2 Cl 0.46517(17) 0.66792(18) 0.41200(15) 0.0347(7) Uani 1 1 d U . .



#----------------------------------------------------------------------------#
#                   MOLECULAR GEOMETRY                                       #
#----------------------------------------------------------------------------#

_geom_special_details            
;
 All s.u.'s (except the s.u. in the dihedral angle between two l.s. planes)
 are estimated using the full covariance matrix.  The cell s.u.'s are taken
 into account individually in the estimation of s.u.'s in distances, angles
 and torsion angles; correlations between s.u.'s in cell parameters are only
 used when they are defined by crystal symmetry.  An approximate (isotropic)
 treatment of cell s.u.'s is used for estimating s.u.'s 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
C1 C2 1.464(12) . ?
C1 N1 1.489(10) . ?
C2 N2 1.348(11) . ?
C2 C3 1.386(13) . ?
C3 C4 1.391(13) . ?
C4 C5 1.329(12) . ?
C5 C6 1.405(12) . ?
C6 N2 1.353(11) . ?
C6 C7 1.473(12) . ?
C7 C8 1.388(12) . ?
C7 C12 1.405(12) . ?
C8 C9 1.385(13) . ?
C9 C10 1.386(13) . ?
C10 C11 1.399(12) . ?
C11 C12 1.391(11) . ?
C11 N3 1.425(11) . ?
C13 O1 1.223(10) . ?
C13 N3 1.334(10) . ?
C13 C14 1.502(12) . ?
C14 N4 1.338(11) . ?
C14 C15 1.352(12) . ?
C15 C16 1.421(14) . ?
C16 C17 1.399(12) . ?
C17 C18 1.391(11) . ?
C18 N4 1.342(10) . ?
C18 C19 1.514(12) . ?
C19 O2 1.196(10) . ?
C19 N5 1.362(11) . ?
C20 C25 1.374(12) . ?
C20 C21 1.376(12) . ?
C21 C22 1.413(13) . ?
C21 N5 1.416(11) . ?
C22 C23 1.400(12) . ?
C23 C24 1.390(12) . ?
C24 C25 1.398(12) . ?
C25 C26 1.465(12) . ?
C26 N6 1.337(11) . ?
C26 C27 1.394(11) . ?
C27 C28 1.359(12) . ?
C28 C29 1.383(12) . ?
C29 C30 1.409(12) . ?
C30 N6 1.353(11) . ?
C30 C31 1.482(13) . ?
C31 N1 1.473(10) . ?
C32 N1 1.473(10) . ?
C32 C33 1.535(11) . ?
C33 N7 1.341(11) . ?
C33 C34 1.368(12) . ?
C34 C35 1.331(12) . ?
C35 C36 1.398(13) . ?
C36 C37 1.370(12) . ?
C37 N7 1.334(10) . ?
N1 Fe1 2.240(7) . ?
N2 Fe1 2.299(8) . ?
N7 Fe1 2.154(8) . ?
Fe1 Cl2 2.308(3) . ?
Fe1 Cl1 2.366(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
C2 C1 N1 115.5(8) . . ?
N2 C2 C3 121.3(9) . . ?
N2 C2 C1 116.8(9) . . ?
C3 C2 C1 122.0(9) . . ?
C2 C3 C4 118.2(10) . . ?
C5 C4 C3 120.4(10) . . ?
C4 C5 C6 120.6(10) . . ?
N2 C6 C5 119.3(10) . . ?
N2 C6 C7 117.9(9) . . ?
C5 C6 C7 122.3(9) . . ?
C8 C7 C12 119.3(9) . . ?
C8 C7 C6 119.9(9) . . ?
C12 C7 C6 120.8(9) . . ?
C9 C8 C7 120.8(10) . . ?
C8 C9 C10 119.7(10) . . ?
C9 C10 C11 120.5(10) . . ?
C12 C11 C10 119.5(10) . . ?
C12 C11 N3 118.1(9) . . ?
C10 C11 N3 122.3(10) . . ?
C11 C12 C7 120.0(9) . . ?
O1 C13 N3 124.0(9) . . ?
O1 C13 C14 121.6(9) . . ?
N3 C13 C14 114.3(9) . . ?
N4 C14 C15 123.8(9) . . ?
N4 C14 C13 117.6(9) . . ?
C15 C14 C13 118.5(10) . . ?
C14 C15 C16 120.1(10) . . ?
C17 C16 C15 115.7(10) . . ?
C18 C17 C16 120.4(10) . . ?
N4 C18 C17 122.1(9) . . ?
N4 C18 C19 119.6(9) . . ?
C17 C18 C19 118.3(8) . . ?
O2 C19 N5 125.2(10) . . ?
O2 C19 C18 120.5(9) . . ?
N5 C19 C18 114.0(8) . . ?
C25 C20 C21 121.9(10) . . ?
C20 C21 C22 120.5(9) . . ?
C20 C21 N5 118.2(9) . . ?
C22 C21 N5 120.9(8) . . ?
C23 C22 C21 117.6(9) . . ?
C24 C23 C22 120.9(10) . . ?
C23 C24 C25 120.7(10) . . ?
C20 C25 C24 118.4(10) . . ?
C20 C25 C26 119.7(9) . . ?
C24 C25 C26 121.9(9) . . ?
N6 C26 C27 121.2(9) . . ?
N6 C26 C25 116.5(9) . . ?
C27 C26 C25 122.3(9) . . ?
C28 C27 C26 120.8(9) . . ?
C27 C28 C29 118.1(10) . . ?
C28 C29 C30 119.9(9) . . ?
N6 C30 C29 120.4(9) . . ?
N6 C30 C31 117.7(9) . . ?
C29 C30 C31 121.8(9) . . ?
N1 C31 C30 115.8(8) . . ?
N1 C32 C33 112.2(8) . . ?
N7 C33 C34 123.1(9) . . ?
N7 C33 C32 114.6(8) . . ?
C34 C33 C32 122.2(9) . . ?
C35 C34 C33 119.2(11) . . ?
C34 C35 C36 120.2(11) . . ?
C37 C36 C35 117.0(10) . . ?
N7 C37 C36 123.7(10) . . ?
C31 N1 C32 108.9(7) . . ?
C31 N1 C1 107.5(7) . . ?
C32 N1 C1 110.7(8) . . ?
C31 N1 Fe1 117.0(6) . . ?
C32 N1 Fe1 110.6(5) . . ?
C1 N1 Fe1 101.8(5) . . ?
C2 N2 C6 120.2(9) . . ?
C2 N2 Fe1 109.8(7) . . ?
C6 N2 Fe1 129.4(7) . . ?
C13 N3 C11 128.1(8) . . ?
C14 N4 C18 117.9(9) . . ?
C19 N5 C21 126.7(8) . . ?
C26 N6 C30 119.4(9) . . ?
C37 N7 C33 116.8(8) . . ?
C37 N7 Fe1 122.6(6) . . ?
C33 N7 Fe1 117.1(6) . . ?
N7 Fe1 N1 77.5(3) . . ?
N7 Fe1 N2 76.9(3) . . ?
N1 Fe1 N2 78.2(3) . . ?
N7 Fe1 Cl2 167.9(2) . . ?
N1 Fe1 Cl2 94.5(2) . . ?
N2 Fe1 Cl2 92.8(2) . . ?
N7 Fe1 Cl1 90.1(2) . . ?
N1 Fe1 Cl1 144.70(19) . . ?
N2 Fe1 Cl1 131.4(2) . . ?
Cl2 Fe1 Cl1 101.54(10) . . ?

#----------------------------------------------------------------------------#
#                   SHELXL.RES FILE                                          #
#----------------------------------------------------------------------------#

_iucr_refine_instruction_details 
;
TITL Compound-4 at 170 K in Cc (#9)
CELL  0.71073  15.1530  13.6300  16.6540   90.000  107.230   90.000
ZERR     4.00   0.0030   0.0020   0.0030    0.000    0.020    0.000
LATT  -7
SYMM    X, - Y, 1/2 + Z
SFAC  C    H    N    O    FE   CL
UNIT  148  116  28   8    4    8
MERG   2
OMIT    -3   7   6
DELU
SHEL   13  0.8
FMAP   2
PLAN   25
SIZE     0.03   0.06   0.17
ACTA
L.S.   4
TEMP  -103.00
WGHT    0.000000
FVAR       0.07179
MOLE    1
C1    1    0.507109    0.851656    0.286658    11.00000    0.03041    0.03189 =
         0.02595   -0.00687    0.00491   -0.00553
AFIX  23
H1A   2    0.550456    0.816912    0.334481    11.00000   -1.20000
H1B   2    0.544539    0.887074    0.256306    11.00000   -1.20000
AFIX   0
C2    1    0.455789    0.923946    0.320184    11.00000    0.00912    0.02524 =
         0.03370   -0.00383   -0.00944    0.00572
C3    1    0.480661    1.022084    0.328681    11.00000    0.02262    0.02777 =
         0.03052    0.00401    0.00296    0.00002
AFIX  43
H3    2    0.530432    1.045811    0.310376    11.00000   -1.20000
AFIX   0
C4    1    0.430766    1.084920    0.364743    11.00000    0.04548    0.02139 =
         0.04034   -0.00428    0.01489   -0.00390
AFIX  43
H4    2    0.447142    1.152317    0.372142    11.00000   -1.20000
AFIX   0
C5    1    0.360336    1.051264    0.388909    11.00000    0.03869    0.01343 =
         0.03726    0.00283    0.01417    0.00142
AFIX  43
H5    2    0.326119    1.095046    0.412639    11.00000   -1.20000
AFIX   0
C6    1    0.336017    0.951551    0.379691    11.00000    0.02772    0.02154 =
         0.01451   -0.00338   -0.00780    0.00670
C7    1    0.252616    0.913148    0.397043    11.00000    0.01744
C8    1    0.172843    0.969558    0.378150    11.00000    0.04480    0.01554 =
         0.02656    0.00069    0.00506    0.00491
AFIX  43
H8    2    0.173733    1.034501    0.357693    11.00000   -1.20000
AFIX   0
C9    1    0.091982    0.932400    0.388732    11.00000    0.05131    0.03399 =
         0.02882    0.00115    0.01547    0.01323
AFIX  43
H9    2    0.037996    0.971962    0.376294    11.00000   -1.20000
AFIX   0
C10   1    0.090110    0.837252    0.417544    11.00000    0.03095    0.03706 =
         0.02221    0.00858    0.01249    0.00996
AFIX  43
H10   2    0.033955    0.810719    0.422429    11.00000   -1.20000
AFIX   0
C11   1    0.170326    0.780030    0.439476    11.00000    0.03062    0.02373 =
         0.00815    0.00400   -0.00019    0.00521
C12   1    0.251990    0.818800    0.430888    11.00000    0.03469    0.01832 =
         0.01722    0.00026    0.00876    0.01150
AFIX  43
H12   2    0.307364    0.781462    0.447916    11.00000   -1.20000
AFIX   0
C13   1    0.127805    0.640046    0.515761    11.00000    0.02407    0.02547 =
         0.01418    0.00192    0.00438    0.00728
C14   1    0.137273    0.530556    0.523996    11.00000    0.02892    0.01350 =
         0.01427   -0.00191   -0.00108    0.00051
C15   1    0.100038    0.484294    0.578093    11.00000    0.04398    0.03927 =
         0.02994    0.00284    0.01523    0.00191
AFIX  43
H15   2    0.071279    0.521324    0.611704    11.00000   -1.20000
AFIX   0
C16   1    0.103892    0.380337    0.584706    11.00000    0.04827    0.04964 =
         0.02680    0.00975    0.01868    0.00178
AFIX  43
H16   2    0.077211    0.345527    0.621157    11.00000   -1.20000
AFIX   0
C17   1    0.149487    0.332547    0.534107    11.00000    0.03292    0.03045 =
         0.01949    0.00435    0.00847   -0.00189
AFIX  43
H17   2    0.155284    0.263125    0.536303    11.00000   -1.20000
AFIX   0
C18   1    0.186380    0.386084    0.480604    11.00000    0.02461    0.01397 =
         0.01237    0.00379    0.00107    0.00534
C19   1    0.234562    0.330738    0.426835    11.00000    0.02872    0.02145 =
         0.02459    0.01004    0.00768    0.01431
C20   1    0.325935    0.418076    0.259251    11.00000    0.02275    0.02121 =
         0.02857   -0.00577    0.00712   -0.00393
AFIX  43
H20   2    0.335312    0.483366    0.280007    11.00000   -1.20000
AFIX   0
C21   1    0.284996    0.351243    0.298925    11.00000    0.01681    0.02245 =
         0.02424    0.00429    0.00581    0.00109
C22   1    0.269467    0.253685    0.269410    11.00000    0.02469    0.02057 =
         0.03995    0.00105    0.01467   -0.00273
AFIX  43
H22   2    0.240433    0.207239    0.295824    11.00000   -1.20000
AFIX   0
C23   1    0.298426    0.227979    0.199834    11.00000    0.03606    0.02947 =
         0.03678   -0.00545    0.00498   -0.00306
AFIX  43
H23   2    0.289384    0.162801    0.178778    11.00000   -1.20000
AFIX   0
C24   1    0.340228    0.296535    0.161147    11.00000    0.03136    0.02808 =
         0.02471   -0.00854    0.01359    0.00430
AFIX  43
H24   2    0.359888    0.277568    0.114282    11.00000   -1.20000
AFIX   0
C25   1    0.353646    0.393113    0.190483    11.00000    0.02408    0.02756 =
         0.01862   -0.00482    0.00924    0.00504
C26   1    0.393412    0.468179    0.148538    11.00000    0.02003
C27   1    0.392097    0.459844    0.064745    11.00000    0.01399    0.02362 =
         0.02835   -0.01101    0.00462   -0.00336
AFIX  43
H27   2    0.364629    0.403857    0.033164    11.00000   -1.20000
AFIX   0
C28   1    0.429595    0.530768    0.027680    11.00000    0.01911    0.04522 =
         0.02707   -0.00092    0.01271   -0.01547
AFIX  43
H28   2    0.429869    0.524576   -0.029064    11.00000   -1.20000
AFIX   0
C29   1    0.467362    0.612250    0.074940    11.00000    0.02498    0.01616 =
         0.03198    0.00497    0.01323    0.00936
AFIX  43
H29   2    0.492942    0.663716    0.050440    11.00000   -1.20000
AFIX   0
C30   1    0.467805    0.618741    0.159497    11.00000    0.02349    0.02147 =
         0.03155   -0.00090    0.00847    0.00371
C31   1    0.512513    0.701607    0.214093    11.00000    0.02271    0.02738 =
         0.02807    0.00160    0.00176    0.00257
AFIX  23
H31A  2    0.548911    0.674743    0.269178    11.00000   -1.20000
H31B  2    0.556431    0.733508    0.188574    11.00000   -1.20000
AFIX   0
C32   1    0.399247    0.822211    0.147785    11.00000    0.01843    0.03341 =
         0.02836    0.01144    0.01457   -0.00331
AFIX  23
H32A  2    0.388783    0.772089    0.102914    11.00000   -1.20000
H32B  2    0.437549    0.875042    0.134522    11.00000   -1.20000
AFIX   0
C33   1    0.305901    0.865088    0.148681    11.00000    0.02314    0.01876 =
         0.01637   -0.00569    0.00749    0.00070
C34   1    0.266933    0.944119    0.100547    11.00000    0.05293    0.03141 =
         0.02490    0.01106    0.01797    0.01732
AFIX  43
H34   2    0.298792    0.976668    0.066970    11.00000   -1.20000
AFIX   0
C35   1    0.183816    0.974842    0.101346    11.00000    0.04902    0.06643 =
         0.02435    0.03031    0.00630    0.02759
AFIX  43
H35   2    0.156361    1.030079    0.068629    11.00000   -1.20000
AFIX   0
C36   1    0.136800    0.926064    0.150187    11.00000    0.02906    0.04000 =
         0.04445   -0.00562    0.01048    0.01108
AFIX  43
H36   2    0.077147    0.946376    0.151143    11.00000   -1.20000
AFIX   0
C37   1    0.180642    0.847633    0.196619    11.00000    0.02632    0.02951 =
         0.02477   -0.00442    0.00772   -0.00680
AFIX  43
H37   2    0.149705    0.813618    0.230187    11.00000   -1.20000
AFIX   0
N1    3    0.449640    0.777228    0.228849    11.00000    0.01960    0.02023 =
         0.02457   -0.00234    0.00527   -0.00021
N2    3    0.384089    0.890086    0.344481    11.00000    0.02372    0.02172 =
         0.02306   -0.00145   -0.00029    0.00473
N3    3    0.170137    0.679856    0.463911    11.00000    0.04132    0.02341 =
         0.03234    0.00284    0.02636    0.00928
AFIX  43
H3A   2    0.201892    0.639198    0.442084    11.00000   -1.20000
AFIX   0
N4    3    0.180094    0.484224    0.475262    11.00000    0.02360    0.02068 =
         0.02747    0.00572    0.00022    0.00740
N5    3    0.250238    0.385376    0.363988    11.00000    0.02540    0.02108 =
         0.01448    0.00620    0.00111    0.00882
AFIX  43
H5A   2    0.237460    0.448375    0.363771    11.00000   -1.20000
AFIX   0
N6    3    0.427954    0.547827    0.193800    11.00000    0.03033    0.01900 =
         0.02555   -0.00377    0.00885    0.00182
N7    3    0.264294    0.816325    0.197367    11.00000    0.01655    0.02380 =
         0.03528    0.00127    0.01162    0.00094
O1    4    0.082063    0.686713    0.551960    11.00000    0.05343    0.02867 =
         0.03783   -0.00275    0.03284    0.00408
O2    4    0.249437    0.244751    0.437025    11.00000    0.05289    0.02116 =
         0.04933    0.00260    0.03184    0.00962
FE1   5    0.351368    0.731135    0.299210    11.00000    0.03075    0.02074 =
         0.02333    0.00519    0.00874    0.00278
CL1   6    0.224902    0.628016    0.296376    11.00000    0.03641    0.02038 =
         0.03189   -0.00119    0.01333   -0.00308
CL2   6    0.465174    0.667919    0.411999    11.00000    0.04041    0.03242 =
         0.02914    0.00965    0.00694    0.00791
HKLF    4
 
REM  MA7FeCl2-b at 170 K in Cc (#9)
REM R1 =  0.0769 for   2079 Fo > 4sig(Fo)  and  0.1888 for all   4852 data
REM    432 parameters refined using    134 restraints
 
END
 
WGHT      0.0000      0.0000
REM Highest difference peak  0.370,  deepest hole -0.392,  1-sigma level  0.082
Q1    1  -0.0193  0.7770  0.4225  11.00000  0.05    0.37
Q2    1   0.3018  0.7376  0.2182  11.00000  0.05    0.34
Q3    1   0.4293  0.7925  0.0199  11.00000  0.05    0.31
Q4    1   0.4560  0.9029  0.4790  11.00000  0.05    0.31
Q5    1   0.3136  0.6260  0.3307  11.00000  0.05    0.31
Q6    1   0.3322  0.6568  0.2684  11.00000  0.05    0.30
Q7    1   0.0565  0.7320  0.3272  11.00000  0.05    0.30
Q8    1   0.3946  0.6733  0.3377  11.00000  0.05    0.30
Q9    1   0.2678  0.7379  0.2883  11.00000  0.05    0.30
Q10   1   0.4565  0.7621  0.4406  11.00000  0.05    0.30
Q11   1   0.2411  0.7513  0.1609  11.00000  0.05    0.30
Q12   1   0.3993  0.3408 -0.0050  11.00000  0.05    0.29
Q13   1   0.1794  0.9468  0.3207  11.00000  0.05    0.29
Q14   1   0.5276  0.6240  0.2695  11.00000  0.05    0.28
Q15   1   0.2594  0.2490  0.1304  11.00000  0.05    0.28
Q16   1   0.3173  0.4683 -0.0032  11.00000  0.05    0.28
Q17   1   0.2726  0.2278  0.4478  11.00000  0.05    0.28
Q18   1   0.3692  0.5405 -0.0744  11.00000  0.05    0.28
Q19   1   0.1509  1.1604  0.0659  11.00000  0.05    0.28
Q20   1   0.1365  1.0309  0.3444  11.00000  0.05    0.27
Q21   1   0.4584  0.7249 -0.0221  11.00000  0.05    0.27
Q22   1   0.3510  0.6026  0.1282  11.00000  0.05    0.27
Q23   1   0.4081  0.7409  0.3844  11.00000  0.05    0.27
Q24   1   0.4507  0.2809  0.0932  11.00000  0.05    0.27
Q25   1   0.1682  0.2398  0.4318  11.00000  0.05    0.26
;
####################################################################### 
# 
# 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_ma2016-37-a
_database_code_depnum_ccdc_archive 'CCDC 1856878'
_audit_update_record             
;
2018-07-19 deposited with the CCDC.
2018-09-28 downloaded from the CCDC.
;

_audit_creation_date             2016-07-22T20:06:30-00:00
_audit_creation_method           'WinGX routine CIF_UPDATE'

#----------------------------------------------------------------------------#
#                   CHEMICAL INFORMATION                                     #
#----------------------------------------------------------------------------#

_chemical_name_systematic        
;
 ?
;
_chemical_formula_moiety         
;
        C32 H31 Fe N7 2+, (C F3 O3 S 1-)2
;
_chemical_formula_sum            'C34 H31 F6 Fe N7 O6 S2'
_chemical_formula_weight         867.63

#----------------------------------------------------------------------------#
#                   UNIT CELL INFORMATION                                    #
#----------------------------------------------------------------------------#

_symmetry_cell_setting           triclinic
_symmetry_space_group_name_H-M   'P -1'
_symmetry_space_group_name_Hall  '-P 1'
_symmetry_Int_Tables_number      2
loop_
_symmetry_equiv_pos_as_xyz
'x, y, z'
'-x, -y, -z'

_cell_length_a                   11.6048(4)
_cell_length_b                   13.6563(6)
_cell_length_c                   14.1144(4)
_cell_angle_alpha                116.401(4)
_cell_angle_beta                 92.178(3)
_cell_angle_gamma                109.682(4)
_cell_volume                     1839.14(12)
_cell_formula_units_Z            2
_cell_measurement_temperature    170(2)
_cell_measurement_reflns_used    7461
_cell_measurement_theta_min      3.646
_cell_measurement_theta_max      29.194

#----------------------------------------------------------------------------#
#                   CRYSTAL INFORMATION                                      #
#----------------------------------------------------------------------------#

_exptl_crystal_description       'fragment of plate'
_exptl_crystal_colour            yellow
_exptl_crystal_size_max          0.33
_exptl_crystal_size_mid          0.18
_exptl_crystal_size_min          0.13
_exptl_crystal_density_diffrn    1.567
_exptl_crystal_density_method    'not measured'
_exptl_crystal_F_000             888
loop_
_exptl_crystal_face_index_h
_exptl_crystal_face_index_k
_exptl_crystal_face_index_l
_exptl_crystal_face_perp_dist
0 0 1 0.07
5 -3 -2 0.15
-1 -1 0 0.08
3 -4 5 0.12
-1 -2 3 0.075
-1 0 5 0.09
1 3 -4 0.08
-1 -9 -9 0.06
2 -1 1 0.12
-8 1 -1 0.135
-3 -4 3 0.07
0 2 -1 0.095
0 1 -1 0.085
0 -1 -3 0.055
1 0 5 0.04
2 -2 1 0.155
-2 2 -1 0.155
1 4 -10 0.075
1 1 -1 0.115
-1 -1 1 0.085
0 0 -1 0.07
-4 6 -1 0.15
5 3 -2 0.115

_exptl_crystal_recrystallization_method 
'from solution in dichloromethane at room temperature,by slow diffusion of diethylether'
_exptl_special_details           
;
 ?
;

#----------------------------------------------------------------------------#
#                   ABSORPTION CORRECTION                                    #
#----------------------------------------------------------------------------#

_exptl_absorpt_coefficient_mu    0.61
_exptl_absorpt_correction_type   analytical
_exptl_absorpt_process_details   
;
CrysAlisPro, Agilent Technologies,
Version 1.171.37.35 (release 13-08-2014 CrysAlis171 .NET)
(compiled Aug 13 2014,18:06:01)
Analytical numeric absorption correction using a multifaceted crystal
model based on expressions derived by R.C. Clark & J.S. Reid.
(Clark, R. C. & Reid, J. S. (1995). Acta Cryst. A51, 887-897)
Empirical absorption correction using spherical harmonics,
implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_absorpt_correction_T_min  0.865
_exptl_absorpt_correction_T_max  0.946

#----------------------------------------------------------------------------#
#                   DATA COLLECTION                                          #
#----------------------------------------------------------------------------#

_diffrn_source                   'Enhance (Mo) X-ray Source'
_diffrn_ambient_temperature      170(2)
_diffrn_radiation_wavelength     0.71073
_diffrn_radiation_type           MoK\a
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_probe          x-ray
_diffrn_detector                 'CCD plate'
_diffrn_detector_area_resol_mean 8.3622
_diffrn_orient_matrix_ub_11      0.0172897
_diffrn_orient_matrix_ub_12      0.0331179
_diffrn_orient_matrix_ub_13      0.0574741
_diffrn_orient_matrix_ub_21      0.0007132
_diffrn_orient_matrix_ub_22      0.0511893
_diffrn_orient_matrix_ub_23      -0.001989
_diffrn_orient_matrix_ub_31      -0.0642971
_diffrn_orient_matrix_ub_32      -0.016359
_diffrn_orient_matrix_ub_33      0.0021648
_diffrn_measurement_device       'four-circle diffractometer'
_diffrn_measurement_device_type  'Xcalibur, Sapphire2, large Be window'
_diffrn_measurement_method       'ω scans'
_diffrn_reflns_av_R_equivalents  0.0326
_diffrn_reflns_av_unetI/netI     0.0424
_diffrn_reflns_number            15152
_diffrn_reflns_limit_h_min       -12
_diffrn_reflns_limit_h_max       14
_diffrn_reflns_limit_k_min       -17
_diffrn_reflns_limit_k_max       10
_diffrn_reflns_limit_l_min       -17
_diffrn_reflns_limit_l_max       17
_diffrn_reflns_theta_min         3.43
_diffrn_reflns_theta_max         26.37
_diffrn_reflns_theta_full        26.37
_diffrn_measured_fraction_theta_full 0.997
_diffrn_measured_fraction_theta_max 0.997
_reflns_number_total             7511
_reflns_number_gt                6167
_reflns_threshold_expression     >2σ(I)

#----------------------------------------------------------------------------#
#                   COMPUTER PROGRAMS USED                                   #
#----------------------------------------------------------------------------#

_computing_data_collection       
;
        CrysAlisPro, Agilent Technologies,
        Version 1.171.37.35 (release 13-08-2014 CrysAlis171 .NET)
        (compiled Aug 13 2014,18:06:01)
;
_computing_cell_refinement       
;
        CrysAlisPro, Agilent Technologies,
        Version 1.171.37.35 (release 13-08-2014 CrysAlis171 .NET)
        (compiled Aug 13 2014,18:06:01)
;
_computing_data_reduction        
;
        CrysAlisPro, Agilent Technologies,
        Version 1.171.37.35 (release 13-08-2014 CrysAlis171 .NET)
        (compiled Aug 13 2014,18:06:01)
;
_computing_structure_solution    'SIR-92 (Altomare et al., 1992)'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 2008)'
_computing_molecular_graphics    
;
        ORTEP3 for Windows (Farrugia, 1997)
        MERCURY  (Bruno et al., 2002)
;
_computing_publication_material  
;
        WinGX (Farrugia, 1999)
        PLATON (Spek, 1990-2003)
        enCIFer (Allen et al., 2004)
;

#----------------------------------------------------------------------------#
#                   STRUCTURE SOLUTION
#----------------------------------------------------------------------------#

_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_atom_sites_solution_hydrogens   geom

#----------------------------------------------------------------------------#
#                   REFINEMENT INFORMATION                                   #
#----------------------------------------------------------------------------#

_refine_special_details          
;
 Refinement of F² against ALL reflections.  The weighted R-factor wR and
 goodness of fit S are based on F², conventional R-factors R are based
 on F, with F set to zero for negative F². The threshold expression of
 F² > 2σ(F²) is used only for calculating R-factors(gt) etc. and is
 not relevant to the choice of reflections for refinement.  R-factors based
 on F² are statistically about twice as large as those based on F, and R-
 factors based on ALL data will be even larger.
;
_refine_ls_structure_factor_coef Fsqd
_refine_ls_matrix_type           full
_refine_ls_weighting_scheme      calc
_refine_ls_weighting_details     
'calc w=1/[σ²(Fo²)+(0.0539P)²+0.6440P] where P=(Fo²+2Fc²)/3'
_refine_ls_hydrogen_treatment    mixed
_refine_ls_extinction_method     none
_refine_ls_number_reflns         7511
_refine_ls_number_parameters     506
_refine_ls_number_restraints     14
_refine_ls_R_factor_all          0.0524
_refine_ls_R_factor_gt           0.0396
_refine_ls_wR_factor_ref         0.106
_refine_ls_wR_factor_gt          0.0982
_refine_ls_goodness_of_fit_ref   1.054
_refine_ls_restrained_S_all      1.053
_refine_ls_shift/su_max          0
_refine_ls_shift/su_mean         0
_refine_diff_density_max         0.471
_refine_diff_density_min         -0.458
_refine_diff_density_rms         0.072

#----------------------------------------------------------------------------#
#                   ATOMIC TYPES, COORDINATES AND THERMAL PARAMETERS         #
#----------------------------------------------------------------------------#

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 0 '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 0.006 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
F F 0.0171 0.0103 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
S S 0.1246 0.1234 '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'

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_symmetry_multiplicity
_atom_site_calc_flag
_atom_site_refinement_flags
_atom_site_disorder_assembly
_atom_site_disorder_group
C1 C 0.1475(2) 0.12286(19) 0.28689(17) 0.0259(5) Uani 1 1 d . . .
H1A H 0.0709 0.0678 0.2932 0.031 Uiso 1 1 calc R . .
H1B H 0.1348 0.1101 0.2119 0.031 Uiso 1 1 calc R . .
C2 C 0.16845(19) 0.24979(19) 0.36582(17) 0.0236(4) Uani 1 1 d . . .
C3 C 0.0931(2) 0.3018(2) 0.34671(18) 0.0278(5) Uani 1 1 d . . .
H3 H 0.0294 0.2595 0.2822 0.033 Uiso 1 1 calc R . .
C4 C 0.1121(2) 0.4160(2) 0.42301(19) 0.0326(5) Uani 1 1 d . . .
H4 H 0.0595 0.4525 0.4132 0.039 Uiso 1 1 calc R . .
C5 C 0.2088(2) 0.4768(2) 0.51403(19) 0.0310(5) Uani 1 1 d . . .
H5 H 0.2238 0.5561 0.5666 0.037 Uiso 1 1 calc R . .
C6 C 0.2838(2) 0.42180(19) 0.52851(17) 0.0238(4) Uani 1 1 d . . .
C7 C 0.39421(19) 0.48614(18) 0.62042(17) 0.0228(4) Uani 1 1 d . . .
C8 C 0.3880(2) 0.56913(19) 0.72072(17) 0.0255(5) Uani 1 1 d . . .
H8 H 0.3144 0.5852 0.7286 0.031 Uiso 1 1 calc R . .
C9 C 0.4891(2) 0.6296(2) 0.81061(18) 0.0301(5) Uani 1 1 d D . .
C10 C 0.5973(2) 0.6053(2) 0.79672(19) 0.0316(5) Uani 1 1 d . . .
H10 H 0.6664 0.6445 0.8567 0.038 Uiso 1 1 calc R . .
C11 C 0.6041(2) 0.5245(2) 0.69596(19) 0.0302(5) Uani 1 1 d . . .
H11 H 0.6784 0.5098 0.6874 0.036 Uiso 1 1 calc R . .
C12 C 0.5035(2) 0.46436(19) 0.60696(18) 0.0257(5) Uani 1 1 d . . .
H12 H 0.509 0.4093 0.5381 0.031 Uiso 1 1 calc R . .
C13 C 0.3621(2) 0.1468(2) 0.26745(17) 0.0278(5) Uani 1 1 d . . .
H13A H 0.3659 0.224 0.2762 0.033 Uiso 1 1 calc R . .
H13B H 0.3491 0.0922 0.1891 0.033 Uiso 1 1 calc R . .
C14 C 0.4840(2) 0.16485(19) 0.32707(17) 0.0251(5) Uani 1 1 d . . .
C15 C 0.5886(2) 0.1722(2) 0.28240(18) 0.0284(5) Uani 1 1 d . . .
H15 H 0.5839 0.161 0.2107 0.034 Uiso 1 1 calc R . .
C16 C 0.7001(2) 0.1960(2) 0.3439(2) 0.0317(5) Uani 1 1 d . . .
H16 H 0.7738 0.2034 0.3157 0.038 Uiso 1 1 calc R . .
C17 C 0.7030(2) 0.2090(2) 0.44709(19) 0.0297(5) Uani 1 1 d . . .
H17 H 0.7791 0.2259 0.4903 0.036 Uiso 1 1 calc R . .
C18 C 0.5949(2) 0.19758(18) 0.48740(17) 0.0238(4) Uani 1 1 d . . .
C19 C 0.5903(2) 0.20160(19) 0.59380(17) 0.0239(4) Uani 1 1 d . . .
C20 C 0.6889(2) 0.2837(2) 0.68268(18) 0.0293(5) Uani 1 1 d . . .
H20 H 0.7604 0.3374 0.6752 0.035 Uiso 1 1 calc R . .
C21 C 0.6842(2) 0.2882(2) 0.78375(19) 0.0333(5) Uani 1 1 d D . .
C22 C 0.5780(2) 0.2079(2) 0.79218(19) 0.0330(5) Uani 1 1 d . . .
H22 H 0.5729 0.2106 0.8603 0.04 Uiso 1 1 calc R . .
C23 C 0.4803(2) 0.1245(2) 0.70312(19) 0.0295(5) Uani 1 1 d . . .
H23 H 0.4095 0.0699 0.7102 0.035 Uiso 1 1 calc R . .
C24 C 0.4854(2) 0.1203(2) 0.60324(18) 0.0265(5) Uani 1 1 d . . .
H24 H 0.4185 0.0629 0.5419 0.032 Uiso 1 1 calc R . .
C25 C 0.2188(2) -0.03165(19) 0.26704(17) 0.0285(5) Uani 1 1 d . . .
H25A H 0.2942 -0.0506 0.2598 0.034 Uiso 1 1 calc R . .
H25B H 0.1622 -0.0762 0.1943 0.034 Uiso 1 1 calc R . .
C26 C 0.1528(2) -0.06932(19) 0.34286(17) 0.0247(4) Uani 1 1 d . . .
C27 C 0.0669(2) -0.1843(2) 0.30687(19) 0.0327(5) Uani 1 1 d . . .
H27 H 0.0427 -0.2411 0.2318 0.039 Uiso 1 1 calc R . .
C28 C 0.0171(2) -0.2153(2) 0.3816(2) 0.0326(5) Uani 1 1 d . . .
H28 H -0.0414 -0.2939 0.3589 0.039 Uiso 1 1 calc R . .
C29 C 0.0535(2) -0.1300(2) 0.49026(19) 0.0292(5) Uani 1 1 d . . .
H29 H 0.0209 -0.1494 0.5433 0.035 Uiso 1 1 calc R . .
C30 C 0.1378(2) -0.0166(2) 0.52030(17) 0.0253(5) Uani 1 1 d . . .
H30 H 0.1618 0.0419 0.5948 0.03 Uiso 1 1 calc R . .
C31 C 0.3036(4) 0.3875(3) 0.8516(2) 0.0590(9) Uani 1 1 d . . .
H31A H 0.2786 0.4518 0.8588 0.089 Uiso 1 1 calc R . .
H31B H 0.3865 0.4215 0.8988 0.089 Uiso 1 1 calc R . .
H31C H 0.2422 0.3358 0.8728 0.089 Uiso 1 1 calc R . .
C32 C 0.3088(3) 0.3181(2) 0.7392(2) 0.0354(6) Uani 1 1 d . . .
N1 N 0.25592(16) 0.09685(15) 0.30892(13) 0.0233(4) Uani 1 1 d . . .
N2 N 0.26001(16) 0.30679(15) 0.45634(13) 0.0213(4) Uani 1 1 d . . .
N3 N 0.4818(2) 0.7131(2) 0.90858(16) 0.0463(6) Uani 1 1 d D . .
H3A H 0.5461 0.7528 0.9644 0.056 Uiso 1 1 calc RD . .
H3B H 0.4129 0.7269 0.9154 0.056 Uiso 1 1 calc RD . .
N4 N 0.7816(2) 0.3696(2) 0.87114(19) 0.0643(8) Uani 1 1 d D . .
H4A H 0.7782 0.3722 0.9344 0.077 Uiso 1 1 calc RD . .
H4B H 0.8477 0.4195 0.8643 0.077 Uiso 1 1 calc RD . .
N5 N 0.48689(16) 0.17889(15) 0.42872(14) 0.0225(4) Uani 1 1 d . . .
N6 N 0.18744(16) 0.01435(15) 0.44824(14) 0.0229(4) Uani 1 1 d . . .
N7 N 0.30935(18) 0.26401(16) 0.65169(15) 0.0270(4) Uani 1 1 d . . .
Fe1 Fe 0.32262(3) 0.18782(3) 0.48732(2) 0.02101(9) Uani 1 1 d . . .
C33 C 0.1799(2) 0.0282(2) 0.9407(2) 0.0411(6) Uani 1 1 d . . .
O1 O 0.16813(18) -0.00867(16) 0.74624(13) 0.0436(4) Uani 1 1 d . . .
O2 O 0.31832(16) 0.18044(16) 0.89127(14) 0.0426(4) Uani 1 1 d . . .
O3 O 0.09581(18) 0.13775(17) 0.86526(16) 0.0476(5) Uani 1 1 d . . .
F1 F 0.19909(18) 0.10962(18) 1.04326(12) 0.0702(6) Uani 1 1 d . . .
F2 F 0.06688(15) -0.05730(15) 0.91486(14) 0.0598(5) Uani 1 1 d . . .
F3 F 0.26523(18) -0.01811(18) 0.93600(18) 0.0724(6) Uani 1 1 d . . .
S1 S 0.19170(5) 0.09178(5) 0.85095(4) 0.02769(14) Uani 1 1 d . . .
C34 C 0.0192(2) 0.6833(2) 0.9335(2) 0.0349(5) Uani 1 1 d . . .
O4 O 0.12478(17) 0.65378(18) 0.77006(14) 0.0429(4) Uani 1 1 d . . .
O5 O 0.0008(2) 0.48037(17) 0.78350(18) 0.0662(7) Uani 1 1 d . . .
O6 O 0.20222(18) 0.6163(2) 0.90635(16) 0.0527(5) Uani 1 1 d . . .
F4 F -0.01728(15) 0.63889(14) 0.99944(12) 0.0463(4) Uani 1 1 d . . .
F5 F 0.09868(18) 0.79524(14) 0.99543(13) 0.0609(5) Uani 1 1 d . . .
F6 F -0.07992(17) 0.68180(19) 0.88336(14) 0.0661(5) Uani 1 1 d . . .
S2 S 0.09507(5) 0.59881(5) 0.83704(5) 0.02963(14) Uani 1 1 d . . .



#----------------------------------------------------------------------------#
#                   MOLECULAR GEOMETRY                                       #
#----------------------------------------------------------------------------#

_geom_special_details            
;
 All s.u.'s (except the s.u. in the dihedral angle between two l.s. planes)
 are estimated using the full covariance matrix.  The cell s.u.'s are taken
 into account individually in the estimation of s.u.'s in distances, angles
 and torsion angles; correlations between s.u.'s in cell parameters are only
 used when they are defined by crystal symmetry.  An approximate (isotropic)
 treatment of cell s.u.'s is used for estimating s.u.'s 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
C1 N1 1.474(3) . ?
C1 C2 1.511(3) . ?
C1 H1A 0.99 . ?
C1 H1B 0.99 . ?
C2 N2 1.350(3) . ?
C2 C3 1.383(3) . ?
C3 C4 1.377(3) . ?
C3 H3 0.95 . ?
C4 C5 1.383(3) . ?
C4 H4 0.95 . ?
C5 C6 1.389(3) . ?
C5 H5 0.95 . ?
C6 N2 1.358(3) . ?
C6 C7 1.482(3) . ?
C7 C8 1.389(3) . ?
C7 C12 1.398(3) . ?
C8 C9 1.403(3) . ?
C8 H8 0.95 . ?
C9 N3 1.375(3) . ?
C9 C10 1.403(3) . ?
C10 C11 1.385(3) . ?
C10 H10 0.95 . ?
C11 C12 1.393(3) . ?
C11 H11 0.95 . ?
C12 H12 0.95 . ?
C13 N1 1.473(3) . ?
C13 C14 1.503(3) . ?
C13 H13A 0.99 . ?
C13 H13B 0.99 . ?
C14 N5 1.358(3) . ?
C14 C15 1.384(3) . ?
C15 C16 1.383(3) . ?
C15 H15 0.95 . ?
C16 C17 1.384(3) . ?
C16 H16 0.95 . ?
C17 C18 1.386(3) . ?
C17 H17 0.95 . ?
C18 N5 1.357(3) . ?
C18 C19 1.482(3) . ?
C19 C20 1.384(3) . ?
C19 C24 1.401(3) . ?
C20 C21 1.404(3) . ?
C20 H20 0.95 . ?
C21 N4 1.364(3) . ?
C21 C22 1.397(3) . ?
C22 C23 1.382(3) . ?
C22 H22 0.95 . ?
C23 C24 1.390(3) . ?
C23 H23 0.95 . ?
C24 H24 0.95 . ?
C25 N1 1.471(3) . ?
C25 C26 1.511(3) . ?
C25 H25A 0.99 . ?
C25 H25B 0.99 . ?
C26 N6 1.347(3) . ?
C26 C27 1.384(3) . ?
C27 C28 1.380(3) . ?
C27 H27 0.95 . ?
C28 C29 1.384(3) . ?
C28 H28 0.95 . ?
C29 C30 1.378(3) . ?
C29 H29 0.95 . ?
C30 N6 1.345(3) . ?
C30 H30 0.95 . ?
C31 C32 1.459(3) . ?
C31 H31A 0.98 . ?
C31 H31B 0.98 . ?
C31 H31C 0.98 . ?
C32 N7 1.124(3) . ?
N1 Fe1 2.2147(17) . ?
N2 Fe1 2.1819(18) . ?
N3 H3A 0.88 . ?
N3 H3B 0.88 . ?
N4 H4A 0.88 . ?
N4 H4B 0.88 . ?
N5 Fe1 2.1260(18) . ?
N6 Fe1 2.1555(18) . ?
N7 Fe1 2.1159(19) . ?
C33 F1 1.326(3) . ?
C33 F2 1.330(3) . ?
C33 F3 1.332(3) . ?
C33 S1 1.813(3) . ?
O1 S1 1.4333(17) . ?
O2 S1 1.4402(17) . ?
O3 S1 1.4312(19) . ?
C34 F6 1.317(3) . ?
C34 F5 1.324(3) . ?
C34 F4 1.331(3) . ?
C34 S2 1.828(3) . ?
O4 S2 1.4345(18) . ?
O5 S2 1.429(2) . ?
O6 S2 1.4354(19) . ?

loop_
_geom_angle_atom_site_label_1
_geom_angle_atom_site_label_2
_geom_angle_atom_site_label_3
_geom_angle
_geom_angle_site_symmetry_1
_geom_angle_site_symmetry_3
_geom_angle_publ_flag
N1 C1 C2 110.74(17) . . ?
N1 C1 H1A 109.5 . . ?
C2 C1 H1A 109.5 . . ?
N1 C1 H1B 109.5 . . ?
C2 C1 H1B 109.5 . . ?
H1A C1 H1B 108.1 . . ?
N2 C2 C3 122.5(2) . . ?
N2 C2 C1 116.78(18) . . ?
C3 C2 C1 120.68(19) . . ?
C4 C3 C2 118.7(2) . . ?
C4 C3 H3 120.7 . . ?
C2 C3 H3 120.7 . . ?
C3 C4 C5 119.3(2) . . ?
C3 C4 H4 120.4 . . ?
C5 C4 H4 120.4 . . ?
C4 C5 C6 119.9(2) . . ?
C4 C5 H5 120 . . ?
C6 C5 H5 120 . . ?
N2 C6 C5 120.60(19) . . ?
N2 C6 C7 117.48(18) . . ?
C5 C6 C7 121.90(19) . . ?
C8 C7 C12 120.10(19) . . ?
C8 C7 C6 119.07(19) . . ?
C12 C7 C6 120.83(19) . . ?
C7 C8 C9 120.9(2) . . ?
C7 C8 H8 119.5 . . ?
C9 C8 H8 119.5 . . ?
N3 C9 C10 121.6(2) . . ?
N3 C9 C8 119.9(2) . . ?
C10 C9 C8 118.5(2) . . ?
C11 C10 C9 120.3(2) . . ?
C11 C10 H10 119.8 . . ?
C9 C10 H10 119.8 . . ?
C10 C11 C12 121.0(2) . . ?
C10 C11 H11 119.5 . . ?
C12 C11 H11 119.5 . . ?
C11 C12 C7 119.1(2) . . ?
C11 C12 H12 120.5 . . ?
C7 C12 H12 120.5 . . ?
N1 C13 C14 110.95(17) . . ?
N1 C13 H13A 109.4 . . ?
C14 C13 H13A 109.4 . . ?
N1 C13 H13B 109.4 . . ?
C14 C13 H13B 109.4 . . ?
H13A C13 H13B 108 . . ?
N5 C14 C15 122.1(2) . . ?
N5 C14 C13 116.21(18) . . ?
C15 C14 C13 121.60(19) . . ?
C16 C15 C14 118.9(2) . . ?
C16 C15 H15 120.6 . . ?
C14 C15 H15 120.6 . . ?
C15 C16 C17 119.1(2) . . ?
C15 C16 H16 120.4 . . ?
C17 C16 H16 120.4 . . ?
C16 C17 C18 120.1(2) . . ?
C16 C17 H17 120 . . ?
C18 C17 H17 120 . . ?
N5 C18 C17 120.7(2) . . ?
N5 C18 C19 116.96(18) . . ?
C17 C18 C19 122.27(19) . . ?
C20 C19 C24 120.3(2) . . ?
C20 C19 C18 120.5(2) . . ?
C24 C19 C18 119.24(19) . . ?
C19 C20 C21 120.6(2) . . ?
C19 C20 H20 119.7 . . ?
C21 C20 H20 119.7 . . ?
N4 C21 C22 121.3(2) . . ?
N4 C21 C20 120.3(2) . . ?
C22 C21 C20 118.4(2) . . ?
C23 C22 C21 121.1(2) . . ?
C23 C22 H22 119.4 . . ?
C21 C22 H22 119.4 . . ?
C22 C23 C24 120.2(2) . . ?
C22 C23 H23 119.9 . . ?
C24 C23 H23 119.9 . . ?
C23 C24 C19 119.4(2) . . ?
C23 C24 H24 120.3 . . ?
C19 C24 H24 120.3 . . ?
N1 C25 C26 110.34(17) . . ?
N1 C25 H25A 109.6 . . ?
C26 C25 H25A 109.6 . . ?
N1 C25 H25B 109.6 . . ?
C26 C25 H25B 109.6 . . ?
H25A C25 H25B 108.1 . . ?
N6 C26 C27 122.2(2) . . ?
N6 C26 C25 115.74(18) . . ?
C27 C26 C25 121.9(2) . . ?
C28 C27 C26 119.0(2) . . ?
C28 C27 H27 120.5 . . ?
C26 C27 H27 120.5 . . ?
C27 C28 C29 119.0(2) . . ?
C27 C28 H28 120.5 . . ?
C29 C28 H28 120.5 . . ?
C30 C29 C28 119.0(2) . . ?
C30 C29 H29 120.5 . . ?
C28 C29 H29 120.5 . . ?
N6 C30 C29 122.5(2) . . ?
N6 C30 H30 118.7 . . ?
C29 C30 H30 118.7 . . ?
C32 C31 H31A 109.5 . . ?
C32 C31 H31B 109.5 . . ?
H31A C31 H31B 109.5 . . ?
C32 C31 H31C 109.5 . . ?
H31A C31 H31C 109.5 . . ?
H31B C31 H31C 109.5 . . ?
N7 C32 C31 178.0(3) . . ?
C25 N1 C13 112.07(17) . . ?
C25 N1 C1 110.86(17) . . ?
C13 N1 C1 111.91(17) . . ?
C25 N1 Fe1 108.14(12) . . ?
C13 N1 Fe1 106.14(12) . . ?
C1 N1 Fe1 107.43(12) . . ?
C2 N2 C6 118.81(18) . . ?
C2 N2 Fe1 113.53(14) . . ?
C6 N2 Fe1 125.98(13) . . ?
C9 N3 H3A 120 . . ?
C9 N3 H3B 120 . . ?
H3A N3 H3B 120 . . ?
C21 N4 H4A 120 . . ?
C21 N4 H4B 120 . . ?
H4A N4 H4B 120 . . ?
C18 N5 C14 119.00(18) . . ?
C18 N5 Fe1 125.61(14) . . ?
C14 N5 Fe1 115.03(14) . . ?
C30 N6 C26 118.24(18) . . ?
C30 N6 Fe1 125.37(14) . . ?
C26 N6 Fe1 116.38(14) . . ?
C32 N7 Fe1 171.13(19) . . ?
N7 Fe1 N5 126.54(7) . . ?
N7 Fe1 N6 93.04(7) . . ?
N5 Fe1 N6 111.77(7) . . ?
N7 Fe1 N2 93.55(7) . . ?
N5 Fe1 N2 111.66(7) . . ?
N6 Fe1 N2 119.17(6) . . ?
N7 Fe1 N1 156.83(7) . . ?
N5 Fe1 N1 76.63(7) . . ?
N6 Fe1 N1 76.07(6) . . ?
N2 Fe1 N1 74.89(6) . . ?
F1 C33 F2 107.5(2) . . ?
F1 C33 F3 107.0(2) . . ?
F2 C33 F3 108.1(2) . . ?
F1 C33 S1 111.58(19) . . ?
F2 C33 S1 111.22(17) . . ?
F3 C33 S1 111.19(19) . . ?
O3 S1 O1 114.06(12) . . ?
O3 S1 O2 115.02(12) . . ?
O1 S1 O2 115.30(11) . . ?
O3 S1 C33 104.60(13) . . ?
O1 S1 C33 102.88(12) . . ?
O2 S1 C33 102.75(11) . . ?
F6 C34 F5 108.7(2) . . ?
F6 C34 F4 108.3(2) . . ?
F5 C34 F4 106.9(2) . . ?
F6 C34 S2 111.39(17) . . ?
F5 C34 S2 110.40(18) . . ?
F4 C34 S2 110.90(17) . . ?
O5 S2 O4 115.11(13) . . ?
O5 S2 O6 114.77(15) . . ?
O4 S2 O6 114.49(11) . . ?
O5 S2 C34 103.02(12) . . ?
O4 S2 C34 104.48(11) . . ?
O6 S2 C34 102.73(12) . . ?

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
N3 H3A O2 0.88 2.14 3.009(3) 167.5 2_667
N3 H3B O6 0.88 2.37 3.057(3) 135.6 .
N4 H4A O6 0.88 2.18 3.054(3) 172 2_667
N4 H4B O5 0.88 2.27 3.099(3) 157 1_655

#----------------------------------------------------------------------------#
#                   SHELXL.RES FILE                                          #
#----------------------------------------------------------------------------#

_iucr_refine_instruction_details 
;
TITL Compound-2 at 170 K in P-1
CELL  0.71073  11.6048  13.6563  14.1144  116.401   92.178  109.682
ZERR     2.00   0.0004   0.0006   0.0004    0.004    0.003    0.004
LATT   1
SFAC  C    H    N    O    F    S    FE
UNIT  68   62   14   12   12   4    2
MERG   2
OMIT     0  -2   2
OMIT    -2   1   1
SHEL   13 0.8
DFIX   0.88  N3 H3A  N3 H3B  N4 H4A  N4 H4B
DANG   1.524 H3A H3B  H4A H4B
SADI  0.04  C9 H3A  C9 H3B  C21 H4A  C21 H4B
FLAT  C9 N3 H3A H3B
FLAT  C21 N4 H4A H4B
EQIV  $1    -x+1, -y+1, -z+2
EQIV  $2     x+1, y, z
HTAB   N3  O2_$1
HTAB   N3  O6
HTAB   N4  O6_$1
HTAB   N4  O5_$2
FMAP   2
PLAN   25
SIZE     0.13   0.18   0.33
ACTA
BOND   $H
L.S.   4
TEMP  -103.00
WGHT    0.053900    0.644000
FVAR       1.64340
MOLE    1
C1    1    0.147534    0.122858    0.286891    11.00000    0.02284    0.03110 =
         0.01882    0.00940    0.00048    0.00948
AFIX  23
H1A   2    0.070882    0.067756    0.293195    11.00000   -1.20000
H1B   2    0.134820    0.110062    0.211857    11.00000   -1.20000
AFIX   0
C2    1    0.168446    0.249794    0.365824    11.00000    0.01967    0.02915 =
         0.02077    0.01351    0.00364    0.00660
C3    1    0.093052    0.301784    0.346708    11.00000    0.02238    0.03671 =
         0.02452    0.01622    0.00140    0.01049
AFIX  43
H3    2    0.029358    0.259550    0.282210    11.00000   -1.20000
AFIX   0
C4    1    0.112139    0.415958    0.423006    11.00000    0.02973    0.03948 =
         0.03466    0.01921    0.00545    0.01905
AFIX  43
H4    2    0.059491    0.452538    0.413212    11.00000   -1.20000
AFIX   0
C5    1    0.208751    0.476794    0.514025    11.00000    0.03452    0.02952 =
         0.02768    0.01207    0.00362    0.01424
AFIX  43
H5    2    0.223757    0.556111    0.566590    11.00000   -1.20000
AFIX   0
C6    1    0.283835    0.421798    0.528511    11.00000    0.02253    0.02635 =
         0.02150    0.01244    0.00490    0.00749
C7    1    0.394214    0.486138    0.620425    11.00000    0.02238    0.02082 =
         0.02329    0.01223    0.00227    0.00469
C8    1    0.388045    0.569129    0.720716    11.00000    0.02093    0.02617 =
         0.02549    0.01167    0.00338    0.00628
AFIX  43
H8    2    0.314406    0.585189    0.728567    11.00000   -1.20000
AFIX   0
C9    1    0.489061    0.629589    0.810609    11.00000    0.02559    0.02850 =
         0.02627    0.01107    0.00253    0.00295
C10   1    0.597324    0.605298    0.796719    11.00000    0.02242    0.03414 =
         0.02862    0.01410   -0.00218    0.00284
AFIX  43
H10   2    0.666366    0.644500    0.856747    11.00000   -1.20000
AFIX   0
C11   1    0.604051    0.524477    0.695964    11.00000    0.02042    0.03263 =
         0.03760    0.01859    0.00441    0.00859
AFIX  43
H11   2    0.678417    0.509797    0.687400    11.00000   -1.20000
AFIX   0
C12   1    0.503468    0.464364    0.606965    11.00000    0.02596    0.02400 =
         0.02706    0.01321    0.00711    0.00841
AFIX  43
H12   2    0.509044    0.409319    0.538060    11.00000   -1.20000
AFIX   0
C13   1    0.362117    0.146834    0.267454    11.00000    0.02826    0.03850 =
         0.02082    0.01662    0.00711    0.01472
AFIX  23
H13A  2    0.365929    0.224005    0.276222    11.00000   -1.20000
H13B  2    0.349080    0.092173    0.189106    11.00000   -1.20000
AFIX   0
C14   1    0.483965    0.164850    0.327066    11.00000    0.02678    0.02701 =
         0.02359    0.01274    0.00697    0.01237
C15   1    0.588610    0.172186    0.282402    11.00000    0.03222    0.03272 =
         0.02855    0.01847    0.01332    0.01635
AFIX  43
H15   2    0.583947    0.161036    0.210740    11.00000   -1.20000
AFIX   0
C16   1    0.700125    0.196034    0.343886    11.00000    0.02826    0.03374 =
         0.04284    0.02277    0.01754    0.01627
AFIX  43
H16   2    0.773763    0.203383    0.315675    11.00000   -1.20000
AFIX   0
C17   1    0.702978    0.209050    0.447091    11.00000    0.02197    0.03392 =
         0.03902    0.02079    0.00677    0.01328
AFIX  43
H17   2    0.779053    0.225854    0.490327    11.00000   -1.20000
AFIX   0
C18   1    0.594912    0.197581    0.487400    11.00000    0.02263    0.02144 =
         0.02710    0.01140    0.00349    0.00927
C19   1    0.590289    0.201602    0.593803    11.00000    0.02227    0.02637 =
         0.02775    0.01381    0.00529    0.01397
C20   1    0.688910    0.283672    0.682677    11.00000    0.02181    0.03446 =
         0.03308    0.02028    0.00248    0.00767
AFIX  43
H20   2    0.760377    0.337388    0.675221    11.00000   -1.20000
AFIX   0
C21   1    0.684228    0.288212    0.783752    11.00000    0.02881    0.03622 =
         0.03061    0.01714   -0.00074    0.00756
C22   1    0.578032    0.207875    0.792179    11.00000    0.03564    0.04169 =
         0.02915    0.02151    0.00844    0.01755
AFIX  43
H22   2    0.572887    0.210600    0.860265    11.00000   -1.20000
AFIX   0
C23   1    0.480343    0.124510    0.703121    11.00000    0.02666    0.03007 =
         0.03444    0.01769    0.00949    0.01104
AFIX  43
H23   2    0.409471    0.069878    0.710221    11.00000   -1.20000
AFIX   0
C24   1    0.485447    0.120340    0.603242    11.00000    0.02262    0.02735 =
         0.02790    0.01219    0.00372    0.00992
AFIX  43
H24   2    0.418484    0.062934    0.541933    11.00000   -1.20000
AFIX   0
C25   1    0.218806   -0.031654    0.267042    11.00000    0.03222    0.02629 =
         0.02043    0.00595    0.00520    0.01170
AFIX  23
H25A  2    0.294242   -0.050635    0.259765    11.00000   -1.20000
H25B  2    0.162166   -0.076198    0.194304    11.00000   -1.20000
AFIX   0
C26   1    0.152768   -0.069319    0.342863    11.00000    0.02342    0.02534 =
         0.02373    0.00971    0.00257    0.01116
C27   1    0.066920   -0.184335    0.306867    11.00000    0.03256    0.02819 =
         0.03070    0.00897    0.00128    0.01272
AFIX  43
H27   2    0.042669   -0.241138    0.231820    11.00000   -1.20000
AFIX   0
C28   1    0.017058   -0.215280    0.381642    11.00000    0.02786    0.02342 =
         0.04346    0.01597    0.00361    0.00771
AFIX  43
H28   2   -0.041377   -0.293916    0.358905    11.00000   -1.20000
AFIX   0
C29   1    0.053480   -0.130008    0.490261    11.00000    0.02609    0.03289 =
         0.03613    0.02174    0.01058    0.01280
AFIX  43
H29   2    0.020850   -0.149352    0.543255    11.00000   -1.20000
AFIX   0
C30   1    0.137814   -0.016623    0.520296    11.00000    0.02472    0.03099 =
         0.02342    0.01446    0.00650    0.01264
AFIX  43
H30   2    0.161819    0.041921    0.594791    11.00000   -1.20000
AFIX   0
C31   1    0.303586    0.387494    0.851636    11.00000    0.11031    0.03683 =
         0.03084    0.01505    0.02601    0.03097
AFIX 137
H31A  2    0.278611    0.451814    0.858811    11.00000   -1.50000
H31B  2    0.386501    0.421513    0.898834    11.00000   -1.50000
H31C  2    0.242156    0.335791    0.872784    11.00000   -1.50000
AFIX   0
C32   1    0.308785    0.318058    0.739189    11.00000    0.05154    0.02816 =
         0.03050    0.01708    0.01019    0.01606
N1    3    0.255916    0.096853    0.308923    11.00000    0.02316    0.02802 =
         0.01946    0.01171    0.00530    0.01069
N2    3    0.260015    0.306785    0.456341    11.00000    0.01914    0.02421 =
         0.01867    0.01068    0.00284    0.00611
N3    3    0.481820    0.713111    0.908579    11.00000    0.03083    0.05405 =
         0.02445   -0.00084   -0.00224    0.01214
AFIX  93
H3A   2    0.546063    0.752801    0.964446    11.00000   -1.20000
H3B   2    0.412944    0.726871    0.915409    11.00000   -1.20000
AFIX   0
N4    3    0.781566    0.369594    0.871137    11.00000    0.04602    0.08010 =
         0.03607    0.03293   -0.01194   -0.01370
AFIX  93
H4A   2    0.778228    0.372197    0.934360    11.00000   -1.20000
H4B   2    0.847680    0.419477    0.864272    11.00000   -1.20000
AFIX   0
N5    3    0.486890    0.178887    0.428718    11.00000    0.02273    0.02378 =
         0.02163    0.01118    0.00410    0.00997
N6    3    0.187440    0.014351    0.448239    11.00000    0.02205    0.02440 =
         0.02034    0.00935    0.00221    0.00944
N7    3    0.309351    0.264008    0.651688    11.00000    0.03373    0.02510 =
         0.02134    0.01039    0.00359    0.01227
FE1   7    0.322622    0.187823    0.487315    11.00000    0.02004    0.02475 =
         0.01704    0.00997    0.00308    0.00789
MOLE    2
C33   1    0.179883    0.028215    0.940669    11.00000    0.03350    0.04646 =
         0.03672    0.02481   -0.00305    0.00326
O1    4    0.168126   -0.008675    0.746243    11.00000    0.04724    0.04869 =
         0.02437    0.01025    0.00540    0.01786
O2    4    0.318322    0.180439    0.891267    11.00000    0.03177    0.04609 =
         0.03976    0.02384    0.00010    0.00064
O3    4    0.095806    0.137749    0.865257    11.00000    0.04107    0.04392 =
         0.05797    0.02136    0.00551    0.02216
F1    5    0.199086    0.109619    1.043256    11.00000    0.06593    0.08762 =
         0.02497    0.02640    0.00104   -0.00323
F2    5    0.066880   -0.057299    0.914861    11.00000    0.04654    0.06106 =
         0.05985    0.04341   -0.00686   -0.00971
F3    5    0.265232   -0.018107    0.936002    11.00000    0.06160    0.08179 =
         0.09749    0.06399   -0.00060    0.02837
S1    6    0.191701    0.091777    0.850949    11.00000    0.02654    0.03020 =
         0.02291    0.01280    0.00211    0.00790
MOLE    3
C34   1    0.019157    0.683287    0.933520    11.00000    0.03730    0.03875 =
         0.03190    0.01777    0.01000    0.01745
O4    4    0.124779    0.653785    0.770060    11.00000    0.04457    0.06556 =
         0.03714    0.03407    0.01648    0.02919
O5    4    0.000840    0.480370    0.783504    11.00000    0.06525    0.03370 =
         0.06045    0.00131    0.02990    0.00379
O6    4    0.202222    0.616280    0.906351    11.00000    0.04321    0.09686 =
         0.04990    0.05021    0.02105    0.04195
F4    5   -0.017283    0.638892    0.999440    11.00000    0.05355    0.05745 =
         0.03856    0.02817    0.02330    0.02597
F5    5    0.098678    0.795239    0.995434    11.00000    0.08584    0.03433 =
         0.04515    0.00926    0.02028    0.01772
F6    5   -0.079922    0.681799    0.883363    11.00000    0.06065    0.11700 =
         0.05480    0.04775    0.02424    0.06397
S2    6    0.095070    0.598811    0.837039    11.00000    0.02833    0.03395 =
         0.02674    0.01376    0.00839    0.01356
HKLF    4
 
REM  MA2016-37-a_170K_proffit in P-1
REM R1 =  0.0396 for   6167 Fo > 4sig(Fo)  and  0.0524 for all   7511 data
REM    506 parameters refined using     14 restraints
 
END
 
WGHT      0.0538      0.6527
REM Highest difference peak  0.471,  deepest hole -0.458,  1-sigma level  0.072
Q1    1  -0.1177  0.5930  0.8351  11.00000  0.05    0.47
Q2    1   0.0235  0.7680  0.9383  11.00000  0.05    0.47
Q3    1   0.1797 -0.0496  0.3044  11.00000  0.05    0.38
Q4    1   0.2403  0.0419  0.2970  11.00000  0.05    0.36
Q5    1   0.3938  0.6861  0.9211  11.00000  0.05    0.34
Q6    1   0.3012  0.1098  0.2804  11.00000  0.05    0.34
Q7    1   0.5536  0.5080  0.6544  11.00000  0.05    0.33
Q8    1   0.1982  0.1080  0.2888  11.00000  0.05    0.32
Q9    1   0.5003  0.1390  0.6599  11.00000  0.05    0.32
Q10   1   0.4348  0.9328  1.0494  11.00000  0.05    0.32
Q11   1   0.0256 -0.1638  0.4349  11.00000  0.05    0.32
Q12   1   0.4654  0.6555  0.9323  11.00000  0.05    0.31
Q13   1   0.0568  0.6458  0.8909  11.00000  0.05    0.31
Q14   1   0.1615  0.1923  0.3356  11.00000  0.05    0.31
Q15   1   0.5379  0.1638  0.6097  11.00000  0.05    0.31
Q16   1   0.5432  0.1561  0.7362  11.00000  0.05    0.30
Q17   1   0.0961  0.5853  0.7553  11.00000  0.05    0.29
Q18   1   0.2792  0.2438  0.6860  11.00000  0.05    0.29
Q19   1   0.3753  0.4726  0.8896  11.00000  0.05    0.28
Q20   1   0.2206  0.0883  0.4605  11.00000  0.05    0.27
Q21   1   0.4844  0.0763  0.6313  11.00000  0.05    0.27
Q22   1   0.5844  0.5435  0.7485  11.00000  0.05    0.26
Q23   1  -0.0102  0.4422  0.7425  11.00000  0.05    0.26
Q24   1   0.3808  0.5100  0.6731  11.00000  0.05    0.26
Q25   1   0.4007  0.1891  0.5046  11.00000  0.05    0.26
;
