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

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

data_Stage1_Initial
_database_code_depnum_ccdc_archive 'CCDC 1053051'
_audit_update_record             
;
2015-12-22 deposited with the CCDC.
2016-01-05 downloaded from the CCDC.
;

_audit_creation_method           SHELXL-2014/7
_shelx_SHELXL_version_number     2014/7
_chemical_name_systematic        ?
_chemical_name_common            ?
_chemical_melting_point          ?
_chemical_formula_moiety         
;
C36 H30 Fe N10 O2, 2(Cl O4), 1.35(C3 H6 O)
;
_chemical_formula_sum            'C40.05 H38.10 Cl2 Fe N10 O11.35'
_chemical_formula_weight         967.85

loop_
_atom_type_symbol
_atom_type_description
_atom_type_scat_dispersion_real
_atom_type_scat_dispersion_imag
_atom_type_scat_source
C C -0.0020 0.0020 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
N N -0.0031 0.0040 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
O O -0.0041 0.0074 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Cl Cl 0.1408 0.1896 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Fe Fe 0.2064 0.9930 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'

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

_shelx_space_group_comment       
;
The symmetry employed for this shelxl refinement is uniquely defined
by the following loop, which should always be used as a source of
symmetry information in preference to the above space-group names.
They are only intended as comments.
;

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

_cell_length_a                   14.1613(12)
_cell_length_b                   21.6112(18)
_cell_length_c                   15.3855(13)
_cell_angle_alpha                90
_cell_angle_beta                 114.3394(11)
_cell_angle_gamma                90
_cell_volume                     4290.1(6)
_cell_formula_units_Z            4
_cell_measurement_temperature    250(2)
_cell_measurement_reflns_used    9477
_cell_measurement_theta_min      2.96
_cell_measurement_theta_max      32.8

_exptl_crystal_description       block
_exptl_crystal_colour            'dark red'
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    ?
_exptl_crystal_density_diffrn    1.498
_exptl_crystal_F_000             1997
_exptl_transmission_factor_min   ?
_exptl_transmission_factor_max   ?
_exptl_crystal_size_max          0.100
_exptl_crystal_size_mid          0.070
_exptl_crystal_size_min          0.050
_exptl_absorpt_coefficient_mu    0.690
_shelx_estimated_absorpt_T_min   0.934
_shelx_estimated_absorpt_T_max   0.966
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_correction_T_min  0.626
_exptl_absorpt_correction_T_max  0.747
_exptl_absorpt_process_details   'SADABS-2012/1  (Sheldrick, 2012)'
_diffrn_ambient_temperature      250(2)
_diffrn_radiation_wavelength     0.7749
_diffrn_radiation_type           synchrotron
_diffrn_radiation_source         'Advanced Light Source Beamline 11.3.1'
_diffrn_radiation_monochromator  silicon(111)
_diffrn_measurement_device_type  'Bruker Apex2'
_diffrn_measurement_method       ω
_diffrn_detector_area_resol_mean 8.3
_diffrn_reflns_number            46488
_diffrn_reflns_av_unetI/netI     0.0655
_diffrn_reflns_av_R_equivalents  0.0631
_diffrn_reflns_limit_h_min       -20
_diffrn_reflns_limit_h_max       20
_diffrn_reflns_limit_k_min       -30
_diffrn_reflns_limit_k_max       30
_diffrn_reflns_limit_l_min       -21
_diffrn_reflns_limit_l_max       21
_diffrn_reflns_theta_min         2.963
_diffrn_reflns_theta_max         33.613
_diffrn_reflns_theta_full        27.706
_diffrn_measured_fraction_theta_max 0.995
_diffrn_measured_fraction_theta_full 0.994
_diffrn_reflns_Laue_measured_fraction_max 0.995
_diffrn_reflns_Laue_measured_fraction_full 0.994
_diffrn_reflns_point_group_measured_fraction_max 0.995
_diffrn_reflns_point_group_measured_fraction_full 0.994
_reflns_number_total             13023
_reflns_number_gt                10342
_reflns_threshold_expression     'I > 2σ(I)'
_reflns_Friedel_coverage         0.000
_reflns_Friedel_fraction_max     .
_reflns_Friedel_fraction_full    .

_reflns_special_details          
;
 Reflections were merged by SHELXL according to the crystal
 class for the calculation of statistics and refinement.
 
 _reflns_Friedel_fraction is defined as the number of unique
 Friedel pairs measured divided by the number that would be
 possible theoretically, ignoring centric projections and
 systematic absences.



The images contain diffraction patterens from two samples: The low spin
initial compound, from which this refinement was done, and  the low
spin/high spin mixed Transient.  The two
neccesary unit cells and orientation matrices were determined
using CELL_NOW and RLATT, and manually combined into an orientation matrix 
file (*.p4p).To seperate the reflections, the SAINT integration
 engine was used in command line mode, and set up with a sample mask. An 
example is shown below:
SMAP=1, 1, 2
This indicates that the first two orientation matrices belong to sample 1, and 
the third belongs to sample 2.  For all commands relating to cell or symmetry 
later on, comma-delimited lists were used to specify distinct parameters.
Listed below are most of the pertinent SAINT commands in an example from the 
SAINT manual:

FILTPOINTGP=-1, 2/m  //indicating sample 1 is triclinic and 2 is monoclinic
CRYST_SYS=1,3
PAR_MASK=TPS2, TP	//restaining the  twinned cells to be similar
GPAR_MASK=TPS2, TP    //and also restraining Detector pitch and xtal trans

 explained in the SAINT manual as
"Two-sample integration, where first sample is a two-component
twin and second component is a single crystal.  In the first sample,
constrain cell constants of the second component to those of the
first.  For both samples, constrain crystal translations and
 detector pitch"


In this case, the SAINT commands used were as follows: 
SMAP=1, 2, 
CRYST_SYS=3, 3
PAR_MASK=TP, TP
GPAR_MASK=TP, TP

This integration yielded two reflection files, both in HKLF4 format.
;

_computing_data_collection       'Apex2 v2012.10-0 (Bruker, 2012)'
_computing_cell_refinement       'SAINT V8.34A(Bruker, 2012)'
_computing_data_reduction        SAINT
_computing_structure_solution    SHELXS
_computing_structure_refinement  'SHELXL-2014/7 (Sheldrick, 2014)'
_computing_molecular_graphics    
;
     	SHELXTL 5.1, XP (Sheldrick, 1994)
	ShelXle Rev 699 (Hubschle, 2011)
;
_computing_publication_material  SHELXL-2014/7
_refine_special_details          
;
 All hydrogens were assigned geometrically and refined as riding, with 
U(H) = 1.2*U(C) for secondary and aromatic carbons, and 
U(H) = 1.5*U(C) for terminal carbons. The hydrogens on N1, N5 N6 and N10 
were found in the difference map first, then affixed geometrically, with 
U(H) = 1.2*U(N)

This stucture contains one low occupancy acetone, and two disordered 
perchlorate anions. The occupancy of the acetone molecule was determined
by fixing the thermal parameters of the atoms, and allowing their occupancies
to refine. The average of the occupancies was approximately 0.25, so the 
occupancy for the molecule was fixed at 0.25.

The disordered perchlorates were modeled as split sites, using the 
following restraints:
SADI_ClO4 0.01 Cl1 O1 Cl1 O2 Cl1 O3 Cl1 O4
SADI_ClO4 0.02 O1 O2 O1 O3 O1 O4 O2 O3 O2 O4 O3 O4

There are some large thermal parameters on some of the perchlorate oxygen
atoms, but splitting the anions further did not seem to add any
new chemical information.

The acetone molecules are not well behaved, and SADIs were used to help them.
SADI 0.01 C40 C41 C40 C42 C37 C38 C37 C39
SADI 0.01 C40 O4 C37 O3
SIMU 0.01 C41 C42 C38 C39

;

_diffrn_orient_matrix_UB_11      -0.04806
_diffrn_orient_matrix_UB_12      0.01315
_diffrn_orient_matrix_UB_13      0.02930
_diffrn_orient_matrix_UB_21      0.01128
_diffrn_orient_matrix_UB_22      -0.04045
_diffrn_orient_matrix_UB_23      0.03438
_diffrn_orient_matrix_UB_31      0.05975
_diffrn_orient_matrix_UB_32      0.01821
_diffrn_orient_matrix_UB_33      0.05521
_diffrn_orient_matrix_type       'Sparks (1982)'

_refine_ls_structure_factor_coef Fsqd
_refine_ls_matrix_type           full
_refine_ls_weighting_scheme      calc
_refine_ls_weighting_details     
'w=1/[σ²(Fo²)+(0.1307P)²+3.4646P] where P=(Fo²+2Fc²)/3'
_atom_sites_solution_primary     ?
_atom_sites_solution_secondary   ?
_atom_sites_solution_hydrogens   geom
_refine_ls_hydrogen_treatment    constr
_refine_ls_extinction_method     none
_refine_ls_extinction_coef       .
_refine_ls_number_reflns         13023
_refine_ls_number_parameters     580
_refine_ls_number_restraints     403
_refine_ls_R_factor_all          0.0902
_refine_ls_R_factor_gt           0.0767
_refine_ls_wR_factor_ref         0.2351
_refine_ls_wR_factor_gt          0.2215
_refine_ls_goodness_of_fit_ref   1.050
_refine_ls_restrained_S_all      1.201
_refine_ls_shift/su_max          0.001
_refine_ls_shift/su_mean         0.000

loop_
_atom_site_label
_atom_site_type_symbol
_atom_site_fract_x
_atom_site_fract_y
_atom_site_fract_z
_atom_site_U_iso_or_equiv
_atom_site_adp_type
_atom_site_occupancy
_atom_site_site_symmetry_order
_atom_site_calc_flag
_atom_site_refinement_flags_posn
_atom_site_refinement_flags_adp
_atom_site_refinement_flags_occupancy
_atom_site_disorder_assembly
_atom_site_disorder_group
Fe1 Fe 0.42461(2) 0.26480(2) 0.60308(2) 0.02564(11) Uani 1 1 d . . . . .
O1 O 0.2767(3) 0.34204(19) 0.9567(3) 0.0954(12) Uani 1 1 d . . . . .
O2 O 0.5041(3) 0.17642(12) 0.3220(2) 0.0670(7) Uani 1 1 d . . . . .
O3 O 0.6623(3) 0.12396(15) 0.9215(3) 0.0771(9) Uani 1 1 d D . . . .
N1 N 0.36235(19) 0.23793(12) 0.77260(17) 0.0392(5) Uani 1 1 d . . . . .
H1 H 0.3693 0.1979 0.7762 0.047 Uiso 1 1 calc R U . . .
N2 N 0.37990(17) 0.27334(11) 0.70939(15) 0.0337(4) Uani 1 1 d . . . . .
N3 N 0.40041(16) 0.35270(10) 0.59997(15) 0.0319(4) Uani 1 1 d . . . . .
N4 N 0.45707(16) 0.28944(10) 0.49630(15) 0.0326(4) Uani 1 1 d . . . . .
N5 N 0.48587(18) 0.26079(11) 0.43342(16) 0.0351(4) Uani 1 1 d . . . . .
H5 H 0.4963 0.2211 0.4331 0.042 Uiso 1 1 calc R U . . .
N6 N 0.64639(18) 0.30726(13) 0.73138(17) 0.0417(5) Uani 1 1 d . . . . .
H6 H 0.6355 0.3469 0.7308 0.050 Uiso 1 1 calc R U . . .
N7 N 0.57285(17) 0.26497(10) 0.68834(15) 0.0331(4) Uani 1 1 d . . . . .
N8 N 0.45596(18) 0.17765(10) 0.60698(15) 0.0330(4) Uani 1 1 d . . . . .
N9 N 0.28810(17) 0.23125(10) 0.51786(15) 0.0325(4) Uani 1 1 d . . . . .
N10 N 0.19169(18) 0.25247(14) 0.47045(17) 0.0413(5) Uani 1 1 d . . . . .
H10 H 0.1741 0.2913 0.4652 0.050 Uiso 1 1 calc R U . . .
C1 C 0.2490(7) 0.3805(4) 1.0188(6) 0.138(3) Uani 1 1 d . . . . .
H1A H 0.2246 0.4202 0.9886 0.208 Uiso 1 1 calc R U . . .
H1B H 0.3092 0.3866 1.0784 0.208 Uiso 1 1 calc R U . . .
H1C H 0.1946 0.3605 1.0314 0.208 Uiso 1 1 calc R U . . .
C2 C 0.2810(3) 0.2799(3) 0.9695(3) 0.0690(11) Uani 1 1 d . . . . .
C3 C 0.2580(4) 0.2509(3) 1.0392(3) 0.0858(16) Uani 1 1 d . . . . .
H3A H 0.2409 0.2748 1.0818 0.103 Uiso 1 1 calc R U . . .
C4 C 0.2602(4) 0.1882(3) 1.0461(3) 0.0881(17) Uani 1 1 d . . . . .
H4A H 0.2446 0.1693 1.0936 0.106 Uiso 1 1 calc R U . . .
C5 C 0.2846(4) 0.1520(3) 0.9851(4) 0.0831(14) Uani 1 1 d . . . . .
H5A H 0.2847 0.1086 0.9894 0.100 Uiso 1 1 calc R U . . .
C6 C 0.3095(4) 0.1812(2) 0.9164(3) 0.0675(10) Uani 1 1 d . . . . .
H6A H 0.3281 0.1567 0.8755 0.081 Uiso 1 1 calc R U . . .
C7 C 0.3079(3) 0.2446(2) 0.9061(2) 0.0536(8) Uani 1 1 d . . . . .
C8 C 0.3317(2) 0.27335(16) 0.8316(2) 0.0450(7) Uani 1 1 d . . . . .
C9 C 0.3311(2) 0.33372(17) 0.8039(2) 0.0478(7) Uani 1 1 d . . . . .
H9A H 0.3146 0.3689 0.8308 0.057 Uiso 1 1 calc R U . . .
C10 C 0.3600(2) 0.33215(14) 0.7270(2) 0.0384(5) Uani 1 1 d . . . . .
C11 C 0.3718(2) 0.37848(13) 0.6646(2) 0.0382(5) Uani 1 1 d . . . . .
C12 C 0.3560(3) 0.44185(15) 0.6649(3) 0.0508(7) Uani 1 1 d . . . . .
H12A H 0.3358 0.4601 0.7101 0.061 Uiso 1 1 calc R U . . .
C13 C 0.3709(3) 0.47776(14) 0.5960(3) 0.0542(8) Uani 1 1 d . . . . .
H13A H 0.3607 0.5208 0.5949 0.065 Uiso 1 1 calc R U . . .
C14 C 0.4000(2) 0.45133(13) 0.5303(3) 0.0475(7) Uani 1 1 d . . . . .
H14A H 0.4088 0.4755 0.4834 0.057 Uiso 1 1 calc R U . . .
C15 C 0.4163(2) 0.38784(12) 0.5345(2) 0.0364(5) Uani 1 1 d . . . . .
C16 C 0.4489(2) 0.34940(12) 0.47357(18) 0.0354(5) Uani 1 1 d . . . . .
C17 C 0.4736(2) 0.35872(14) 0.3951(2) 0.0410(6) Uani 1 1 d . . . . .
H17A H 0.4743 0.3966 0.3653 0.049 Uiso 1 1 calc R U . . .
C18 C 0.4967(2) 0.30108(14) 0.37072(19) 0.0387(5) Uani 1 1 d . . . . .
C19 C 0.5250(2) 0.28064(17) 0.2931(2) 0.0458(6) Uani 1 1 d . . . . .
C20 C 0.5496(4) 0.3267(2) 0.2411(3) 0.0662(10) Uani 1 1 d . . . . .
H20A H 0.5481 0.3686 0.2569 0.079 Uiso 1 1 calc R U . . .
C21 C 0.5760(5) 0.3104(3) 0.1662(3) 0.0858(15) Uani 1 1 d . . . . .
H21A H 0.5929 0.3412 0.1318 0.103 Uiso 1 1 calc R U . . .
C22 C 0.5770(5) 0.2487(3) 0.1432(4) 0.0870(15) Uani 1 1 d . . . . .
H22A H 0.5934 0.2375 0.0920 0.104 Uiso 1 1 calc R U . . .
C23 C 0.5541(4) 0.2033(3) 0.1948(3) 0.0776(13) Uani 1 1 d . . . . .
H23A H 0.5562 0.1613 0.1796 0.093 Uiso 1 1 calc R U . . .
C24 C 0.5282(3) 0.21984(19) 0.2686(3) 0.0533(8) Uani 1 1 d . . . . .
C25 C 0.5008(6) 0.1130(2) 0.2941(5) 0.111(2) Uani 1 1 d . . . . .
H25A H 0.4749 0.0877 0.3316 0.167 Uiso 1 1 calc R U . . .
H25B H 0.5699 0.0994 0.3046 0.167 Uiso 1 1 calc R U . . .
H25C H 0.4552 0.1089 0.2270 0.167 Uiso 1 1 calc R U . . .
C26 C 0.7398(2) 0.2800(2) 0.7757(2) 0.0543(8) Uani 1 1 d . . . . .
H26A H 0.8027 0.3004 0.8108 0.065 Uiso 1 1 calc R U . . .
C27 C 0.7274(2) 0.2185(2) 0.7612(2) 0.0517(8) Uani 1 1 d . . . . .
H27A H 0.7790 0.1879 0.7837 0.062 Uiso 1 1 calc R U . . .
C28 C 0.6211(2) 0.20991(15) 0.70524(19) 0.0389(6) Uani 1 1 d . . . . .
C29 C 0.5541(2) 0.15854(13) 0.6581(2) 0.0400(6) Uani 1 1 d . . . . .
C30 C 0.5812(3) 0.09726(16) 0.6575(3) 0.0579(9) Uani 1 1 d . . . . .
H30A H 0.6497 0.0840 0.6929 0.069 Uiso 1 1 calc R U . . .
C31 C 0.5049(4) 0.05557(15) 0.6035(3) 0.0674(11) Uani 1 1 d . . . . .
H31A H 0.5219 0.0136 0.6023 0.081 Uiso 1 1 calc R U . . .
C32 C 0.4044(3) 0.07521(15) 0.5516(3) 0.0573(9) Uani 1 1 d . . . . .
H32A H 0.3528 0.0472 0.5144 0.069 Uiso 1 1 calc R U . . .
C33 C 0.3814(2) 0.13757(12) 0.55577(19) 0.0393(6) Uani 1 1 d . . . . .
C34 C 0.2824(2) 0.16915(13) 0.50810(18) 0.0387(5) Uani 1 1 d . . . . .
C35 C 0.1797(3) 0.15127(18) 0.4544(2) 0.0522(8) Uani 1 1 d . . . . .
H35A H 0.1539 0.1109 0.4375 0.063 Uiso 1 1 calc R U . . .
C36 C 0.1256(2) 0.2051(2) 0.4320(2) 0.0530(8) Uani 1 1 d . . . . .
H36A H 0.0538 0.2088 0.3956 0.064 Uiso 1 1 calc R U . . .
C37 C 0.6190(3) 0.08181(17) 0.9396(3) 0.0581(8) Uani 1 1 d D . . . .
C38 C 0.6161(4) 0.0200(2) 0.8965(4) 0.0811(13) Uani 1 1 d D . . . .
H38A H 0.6661 0.0187 0.8683 0.122 Uiso 1 1 calc R U . . .
H38B H 0.5472 0.0123 0.8474 0.122 Uiso 1 1 calc R U . . .
H38C H 0.6332 -0.0116 0.9454 0.122 Uiso 1 1 calc R U . . .
C39 C 0.5653(5) 0.0886(3) 1.0035(4) 0.0970(17) Uani 1 1 d D . . . .
H39A H 0.5743 0.1304 1.0283 0.146 Uiso 1 1 calc R U . . .
H39B H 0.5943 0.0595 1.0560 0.146 Uiso 1 1 calc R U . . .
H39C H 0.4920 0.0801 0.9682 0.146 Uiso 1 1 calc R U . . .
O4 O -0.0351(14) 0.0709(7) 0.4516(12) 0.148(6) Uiso 0.35 1 d D . P A -1
C40 C -0.0145(13) 0.0198(7) 0.4804(10) 0.084(4) Uiso 0.35 1 d D . P A -1
C41 C 0.035(2) -0.0207(12) 0.4340(18) 0.129(10) Uiso 0.35 1 d D . P A -1
H41A H 0.0475 -0.0611 0.4643 0.193 Uiso 0.35 1 calc R U P A -1
H41B H -0.0108 -0.0251 0.3670 0.193 Uiso 0.35 1 calc R U P A -1
H41C H 0.0999 -0.0027 0.4403 0.193 Uiso 0.35 1 calc R U P A -1
C42 C -0.010(2) -0.0009(15) 0.5734(14) 0.127(8) Uiso 0.35 1 d D . P A -1
H42A H 0.0083 -0.0445 0.5823 0.190 Uiso 0.35 1 calc R U P A -1
H42B H 0.0418 0.0230 0.6241 0.190 Uiso 0.35 1 calc R U P A -1
H42C H -0.0772 0.0050 0.5750 0.190 Uiso 0.35 1 calc R U P A -1
Cl1_1 Cl 0.69667(15) 0.4664(2) 0.7453(2) 0.0535(5) Uiso 0.532(6) 1 d D . P B 1
O1_1 O 0.6133(4) 0.4344(3) 0.7618(5) 0.0592(16) Uiso 0.532(6) 1 d D . P B 1
O2_1 O 0.7873(5) 0.4607(4) 0.8294(5) 0.097(2) Uiso 0.532(6) 1 d D . P B 1
O3_1 O 0.6652(6) 0.5313(3) 0.7330(6) 0.097(2) Uiso 0.532(6) 1 d D . P B 1
O4_1 O 0.7020(8) 0.4452(4) 0.6623(5) 0.134(4) Uiso 0.532(6) 1 d D . P B 1
Cl1_2 Cl 0.69172(15) 0.4747(2) 0.7661(2) 0.0451(5) Uiso 0.468(6) 1 d D . P B 2
O1_2 O 0.6077(5) 0.4326(4) 0.7333(6) 0.082(3) Uiso 0.468(6) 1 d D . P B 2
O2_2 O 0.7213(7) 0.4996(4) 0.8575(5) 0.118(3) Uiso 0.468(6) 1 d D . P B 2
O3_2 O 0.6839(7) 0.5196(4) 0.6964(6) 0.105(3) Uiso 0.468(6) 1 d D . P B 2
O4_2 O 0.7835(6) 0.4365(4) 0.7810(7) 0.106(3) Uiso 0.468(6) 1 d D . P B 2
Cl1_3 Cl 0.3052(2) 0.05085(11) 0.7327(2) 0.0534(6) Uiso 0.502(9) 1 d D . P C 1
O1_3 O 0.2565(7) 0.0589(4) 0.7979(6) 0.105(3) Uiso 0.502(9) 1 d D . P C 1
O2_3 O 0.3678(6) -0.0028(3) 0.7627(7) 0.107(3) Uiso 0.502(9) 1 d D . P C 1
O3_3 O 0.2332(7) 0.0510(5) 0.6379(5) 0.130(4) Uiso 0.502(9) 1 d D . P C 1
O4_3 O 0.3674(5) 0.1048(3) 0.7441(5) 0.0615(18) Uiso 0.502(9) 1 d D . P C 1
Cl1_4 Cl 0.3221(3) 0.05216(12) 0.7553(3) 0.0602(7) Uiso 0.498(9) 1 d D . P C 2
O1_4 O 0.3251(8) 0.0378(4) 0.8464(5) 0.107(3) Uiso 0.498(9) 1 d D . P C 2
O2_4 O 0.3504(7) 0.0001(4) 0.7142(7) 0.108(3) Uiso 0.498(9) 1 d D . P C 2
O3_4 O 0.2175(5) 0.0676(5) 0.6961(8) 0.143(5) Uiso 0.498(9) 1 d D . P C 2
O4_4 O 0.3938(5) 0.1014(3) 0.7666(5) 0.0579(17) Uiso 0.498(9) 1 d D . P C 2


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

loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
_geom_bond_publ_flag
Fe1 N3 1.927(2) . ?
Fe1 N8 1.930(2) . ?
Fe1 N4 1.954(2) . ?
Fe1 N7 1.964(2) . ?
Fe1 N9 1.973(2) . ?
Fe1 N2 1.991(2) . ?
O1 C2 1.355(6) . ?
O1 C1 1.437(6) . ?
O2 C24 1.380(4) . ?
O2 C25 1.432(5) . ?
O3 C37 1.193(5) . ?
N1 N2 1.339(3) . ?
N1 C8 1.386(4) . ?
N1 H1 0.8700 . ?
N2 C10 1.353(4) . ?
N3 C11 1.340(3) . ?
N3 C15 1.353(3) . ?
N4 C16 1.335(3) . ?
N4 N5 1.346(3) . ?
N5 C18 1.354(3) . ?
N5 H5 0.8700 . ?
N6 N7 1.338(3) . ?
N6 C26 1.348(4) . ?
N6 H6 0.8700 . ?
N7 C28 1.343(4) . ?
N8 C33 1.341(4) . ?
N8 C29 1.349(3) . ?
N9 N10 1.336(3) . ?
N9 C34 1.349(4) . ?
N10 C36 1.348(4) . ?
N10 H10 0.8700 . ?
C1 H1A 0.9700 . ?
C1 H1B 0.9700 . ?
C1 H1C 0.9700 . ?
C2 C3 1.391(6) . ?
C2 C7 1.409(5) . ?
C3 C4 1.358(8) . ?
C3 H3A 0.9400 . ?
C4 C5 1.373(8) . ?
C4 H4A 0.9400 . ?
C5 C6 1.395(6) . ?
C5 H5A 0.9400 . ?
C6 C7 1.378(6) . ?
C6 H6A 0.9400 . ?
C7 C8 1.461(5) . ?
C8 C9 1.372(5) . ?
C9 C10 1.403(4) . ?
C9 H9A 0.9400 . ?
C10 C11 1.443(4) . ?
C11 C12 1.388(4) . ?
C12 C13 1.399(5) . ?
C12 H12A 0.9400 . ?
C13 C14 1.364(5) . ?
C13 H13A 0.9400 . ?
C14 C15 1.389(4) . ?
C14 H14A 0.9400 . ?
C15 C16 1.462(4) . ?
C16 C17 1.402(4) . ?
C17 C18 1.379(4) . ?
C17 H17A 0.9400 . ?
C18 C19 1.475(4) . ?
C19 C24 1.373(5) . ?
C19 C20 1.408(5) . ?
C20 C21 1.395(6) . ?
C20 H20A 0.9400 . ?
C21 C22 1.382(8) . ?
C21 H21A 0.9400 . ?
C22 C23 1.384(7) . ?
C22 H22A 0.9400 . ?
C23 C24 1.376(5) . ?
C23 H23A 0.9400 . ?
C25 H25A 0.9700 . ?
C25 H25B 0.9700 . ?
C25 H25C 0.9700 . ?
C26 C27 1.346(6) . ?
C26 H26A 0.9400 . ?
C27 C28 1.405(4) . ?
C27 H27A 0.9400 . ?
C28 C29 1.446(4) . ?
C29 C30 1.380(4) . ?
C30 C31 1.389(6) . ?
C30 H30A 0.9400 . ?
C31 C32 1.381(6) . ?
C31 H31A 0.9400 . ?
C32 C33 1.394(4) . ?
C32 H32A 0.9400 . ?
C33 C34 1.457(4) . ?
C34 C35 1.399(4) . ?
C35 C36 1.357(6) . ?
C35 H35A 0.9400 . ?
C36 H36A 0.9400 . ?
C37 C39 1.478(5) . ?
C37 C38 1.485(5) . ?
C38 H38A 0.9700 . ?
C38 H38B 0.9700 . ?
C38 H38C 0.9700 . ?
C39 H39A 0.9700 . ?
C39 H39B 0.9700 . ?
C39 H39C 0.9700 . ?
O4 C40 1.181(10) . ?
C40 C41 1.474(9) . ?
C40 C42 1.475(9) . ?
C41 H41A 0.9700 . ?
C41 H41B 0.9700 . ?
C41 H41C 0.9700 . ?
C42 H42A 0.9700 . ?
C42 H42B 0.9700 . ?
C42 H42C 0.9700 . ?
Cl1_1 O4_1 1.388(6) . ?
Cl1_1 O2_1 1.402(5) . ?
Cl1_1 O3_1 1.461(5) . ?
Cl1_1 O1_1 1.478(5) . ?
Cl1_2 O2_2 1.398(6) . ?
Cl1_2 O1_2 1.416(5) . ?
Cl1_2 O3_2 1.417(6) . ?
Cl1_2 O4_2 1.477(6) . ?
Cl1_3 O3_3 1.393(6) . ?
Cl1_3 O2_3 1.417(6) . ?
Cl1_3 O4_3 1.428(5) . ?
Cl1_3 O1_3 1.442(6) . ?
Cl1_4 O1_4 1.419(6) . ?
Cl1_4 O3_4 1.423(6) . ?
Cl1_4 O2_4 1.426(6) . ?
Cl1_4 O4_4 1.431(5) . ?

loop_
_geom_angle_atom_site_label_1
_geom_angle_atom_site_label_2
_geom_angle_atom_site_label_3
_geom_angle
_geom_angle_site_symmetry_1
_geom_angle_site_symmetry_3
_geom_angle_publ_flag
N3 Fe1 N8 177.09(9) . . ?
N3 Fe1 N4 79.14(9) . . ?
N8 Fe1 N4 99.28(9) . . ?
N3 Fe1 N7 98.34(9) . . ?
N8 Fe1 N7 79.18(9) . . ?
N4 Fe1 N7 90.23(9) . . ?
N3 Fe1 N9 103.31(9) . . ?
N8 Fe1 N9 79.15(9) . . ?
N4 Fe1 N9 92.69(9) . . ?
N7 Fe1 N9 158.32(9) . . ?
N3 Fe1 N2 79.37(10) . . ?
N8 Fe1 N2 102.23(9) . . ?
N4 Fe1 N2 158.49(10) . . ?
N7 Fe1 N2 93.75(9) . . ?
N9 Fe1 N2 91.36(9) . . ?
C2 O1 C1 118.9(5) . . ?
C24 O2 C25 117.2(3) . . ?
N2 N1 C8 111.2(3) . . ?
N2 N1 H1 124.4 . . ?
C8 N1 H1 124.4 . . ?
N1 N2 C10 106.0(2) . . ?
N1 N2 Fe1 139.55(19) . . ?
C10 N2 Fe1 114.46(19) . . ?
C11 N3 C15 120.9(2) . . ?
C11 N3 Fe1 119.76(19) . . ?
C15 N3 Fe1 119.29(18) . . ?
C16 N4 N5 106.1(2) . . ?
C16 N4 Fe1 117.40(18) . . ?
N5 N4 Fe1 136.49(18) . . ?
N4 N5 C18 111.9(2) . . ?
N4 N5 H5 124.1 . . ?
C18 N5 H5 124.1 . . ?
N7 N6 C26 110.7(3) . . ?
N7 N6 H6 124.7 . . ?
C26 N6 H6 124.7 . . ?
N6 N7 C28 106.2(2) . . ?
N6 N7 Fe1 137.01(19) . . ?
C28 N7 Fe1 116.51(19) . . ?
C33 N8 C29 121.1(2) . . ?
C33 N8 Fe1 119.78(19) . . ?
C29 N8 Fe1 119.03(19) . . ?
N10 N9 C34 106.2(2) . . ?
N10 N9 Fe1 137.52(19) . . ?
C34 N9 Fe1 115.92(18) . . ?
N9 N10 C36 110.3(3) . . ?
N9 N10 H10 124.8 . . ?
C36 N10 H10 124.8 . . ?
O1 C1 H1A 109.5 . . ?
O1 C1 H1B 109.5 . . ?
H1A C1 H1B 109.5 . . ?
O1 C1 H1C 109.5 . . ?
H1A C1 H1C 109.5 . . ?
H1B C1 H1C 109.5 . . ?
O1 C2 C3 123.3(4) . . ?
O1 C2 C7 116.3(4) . . ?
C3 C2 C7 120.4(5) . . ?
C4 C3 C2 120.3(5) . . ?
C4 C3 H3A 119.9 . . ?
C2 C3 H3A 119.9 . . ?
C3 C4 C5 121.3(4) . . ?
C3 C4 H4A 119.3 . . ?
C5 C4 H4A 119.3 . . ?
C4 C5 C6 118.2(5) . . ?
C4 C5 H5A 120.9 . . ?
C6 C5 H5A 120.9 . . ?
C7 C6 C5 122.7(4) . . ?
C7 C6 H6A 118.6 . . ?
C5 C6 H6A 118.6 . . ?
C6 C7 C2 117.0(4) . . ?
C6 C7 C8 121.0(3) . . ?
C2 C7 C8 122.0(4) . . ?
C9 C8 N1 106.6(3) . . ?
C9 C8 C7 132.4(3) . . ?
N1 C8 C7 121.0(3) . . ?
C8 C9 C10 105.8(3) . . ?
C8 C9 H9A 127.1 . . ?
C10 C9 H9A 127.1 . . ?
N2 C10 C9 110.4(3) . . ?
N2 C10 C11 115.4(2) . . ?
C9 C10 C11 134.2(3) . . ?
N3 C11 C12 120.7(3) . . ?
N3 C11 C10 111.0(2) . . ?
C12 C11 C10 128.3(3) . . ?
C11 C12 C13 118.0(3) . . ?
C11 C12 H12A 121.0 . . ?
C13 C12 H12A 121.0 . . ?
C14 C13 C12 121.0(3) . . ?
C14 C13 H13A 119.5 . . ?
C12 C13 H13A 119.5 . . ?
C13 C14 C15 118.4(3) . . ?
C13 C14 H14A 120.8 . . ?
C15 C14 H14A 120.8 . . ?
N3 C15 C14 120.9(3) . . ?
N3 C15 C16 110.6(2) . . ?
C14 C15 C16 128.5(3) . . ?
N4 C16 C17 109.9(3) . . ?
N4 C16 C15 113.5(2) . . ?
C17 C16 C15 136.6(3) . . ?
C18 C17 C16 106.0(2) . . ?
C18 C17 H17A 127.0 . . ?
C16 C17 H17A 127.0 . . ?
N5 C18 C17 106.1(2) . . ?
N5 C18 C19 122.2(3) . . ?
C17 C18 C19 131.7(3) . . ?
C24 C19 C20 118.5(3) . . ?
C24 C19 C18 124.0(3) . . ?
C20 C19 C18 117.5(3) . . ?
C21 C20 C19 120.3(4) . . ?
C21 C20 H20A 119.9 . . ?
C19 C20 H20A 119.9 . . ?
C22 C21 C20 119.3(4) . . ?
C22 C21 H21A 120.3 . . ?
C20 C21 H21A 120.3 . . ?
C21 C22 C23 120.5(4) . . ?
C21 C22 H22A 119.7 . . ?
C23 C22 H22A 119.7 . . ?
C24 C23 C22 119.6(5) . . ?
C24 C23 H23A 120.2 . . ?
C22 C23 H23A 120.2 . . ?
C19 C24 C23 121.7(4) . . ?
C19 C24 O2 116.3(3) . . ?
C23 C24 O2 122.0(4) . . ?
O2 C25 H25A 109.5 . . ?
O2 C25 H25B 109.5 . . ?
H25A C25 H25B 109.5 . . ?
O2 C25 H25C 109.5 . . ?
H25A C25 H25C 109.5 . . ?
H25B C25 H25C 109.5 . . ?
C27 C26 N6 108.3(3) . . ?
C27 C26 H26A 125.8 . . ?
N6 C26 H26A 125.8 . . ?
C26 C27 C28 105.4(3) . . ?
C26 C27 H27A 127.3 . . ?
C28 C27 H27A 127.3 . . ?
N7 C28 C27 109.4(3) . . ?
N7 C28 C29 114.0(2) . . ?
C27 C28 C29 136.5(3) . . ?
N8 C29 C30 120.8(3) . . ?
N8 C29 C28 111.3(2) . . ?
C30 C29 C28 127.8(3) . . ?
C29 C30 C31 118.5(3) . . ?
C29 C30 H30A 120.8 . . ?
C31 C30 H30A 120.8 . . ?
C32 C31 C30 120.6(3) . . ?
C32 C31 H31A 119.7 . . ?
C30 C31 H31A 119.7 . . ?
C31 C32 C33 118.4(3) . . ?
C31 C32 H32A 120.8 . . ?
C33 C32 H32A 120.8 . . ?
N8 C33 C32 120.6(3) . . ?
N8 C33 C34 110.8(2) . . ?
C32 C33 C34 128.6(3) . . ?
N9 C34 C35 109.9(3) . . ?
N9 C34 C33 114.1(2) . . ?
C35 C34 C33 136.0(3) . . ?
C36 C35 C34 104.7(3) . . ?
C36 C35 H35A 127.7 . . ?
C34 C35 H35A 127.7 . . ?
N10 C36 C35 108.8(3) . . ?
N10 C36 H36A 125.6 . . ?
C35 C36 H36A 125.6 . . ?
O3 C37 C39 122.3(4) . . ?
O3 C37 C38 120.3(4) . . ?
C39 C37 C38 117.3(4) . . ?
C37 C38 H38A 109.5 . . ?
C37 C38 H38B 109.5 . . ?
H38A C38 H38B 109.5 . . ?
C37 C38 H38C 109.5 . . ?
H38A C38 H38C 109.5 . . ?
H38B C38 H38C 109.5 . . ?
C37 C39 H39A 109.5 . . ?
C37 C39 H39B 109.5 . . ?
H39A C39 H39B 109.5 . . ?
C37 C39 H39C 109.5 . . ?
H39A C39 H39C 109.5 . . ?
H39B C39 H39C 109.5 . . ?
O4 C40 C41 117.8(17) . . ?
O4 C40 C42 124(2) . . ?
C41 C40 C42 116.7(17) . . ?
C40 C41 H41A 109.5 . . ?
C40 C41 H41B 109.5 . . ?
H41A C41 H41B 109.5 . . ?
C40 C41 H41C 109.5 . . ?
H41A C41 H41C 109.5 . . ?
H41B C41 H41C 109.5 . . ?
C40 C42 H42A 109.5 . . ?
C40 C42 H42B 109.5 . . ?
H42A C42 H42B 109.5 . . ?
C40 C42 H42C 109.5 . . ?
H42A C42 H42C 109.5 . . ?
H42B C42 H42C 109.5 . . ?
O4_1 Cl1_1 O2_1 116.3(5) . . ?
O4_1 Cl1_1 O3_1 109.1(5) . . ?
O2_1 Cl1_1 O3_1 108.6(5) . . ?
O4_1 Cl1_1 O1_1 110.7(5) . . ?
O2_1 Cl1_1 O1_1 107.0(4) . . ?
O3_1 Cl1_1 O1_1 104.4(4) . . ?
O2_2 Cl1_2 O1_2 117.7(6) . . ?
O2_2 Cl1_2 O3_2 113.3(6) . . ?
O1_2 Cl1_2 O3_2 112.2(5) . . ?
O2_2 Cl1_2 O4_2 100.3(5) . . ?
O1_2 Cl1_2 O4_2 104.6(5) . . ?
O3_2 Cl1_2 O4_2 106.8(5) . . ?
O3_3 Cl1_3 O2_3 115.6(6) . . ?
O3_3 Cl1_3 O4_3 106.0(5) . . ?
O2_3 Cl1_3 O4_3 110.9(5) . . ?
O3_3 Cl1_3 O1_3 112.0(5) . . ?
O2_3 Cl1_3 O1_3 106.7(5) . . ?
O4_3 Cl1_3 O1_3 105.3(4) . . ?
O1_4 Cl1_4 O3_4 106.4(6) . . ?
O1_4 Cl1_4 O2_4 111.5(5) . . ?
O3_4 Cl1_4 O2_4 108.1(6) . . ?
O1_4 Cl1_4 O4_4 108.1(5) . . ?
O3_4 Cl1_4 O4_4 113.7(5) . . ?
O2_4 Cl1_4 O4_4 109.0(5) . . ?

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
N1 H1 O4_4 0.87 2.13 2.990(6) 170.8 .
N1 H1 O4_3 0.87 2.07 2.915(6) 164.1 .
N5 H5 O2 0.87 2.01 2.587(3) 123.3 .
N6 H6 O1_2 0.87 1.90 2.767(9) 177.1 .
N6 H6 O1_1 0.87 2.01 2.858(7) 166.0 .
N6 H6 Cl1_1 0.87 2.70 3.501(4) 152.9 .
N6 H6 Cl1_2 0.87 2.86 3.676(4) 156.0 .
N10 H10 O3 0.87 1.93 2.759(4) 157.9 4_565

_refine_diff_density_max         1.215
_refine_diff_density_min         -1.414
_refine_diff_density_rms         0.091

####################################################################### 
# 
# 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_Stage1_Transient
_database_code_depnum_ccdc_archive 'CCDC 1053052'
_audit_update_record             
;
2015-12-22 deposited with the CCDC.
2016-01-05 downloaded from the CCDC.
;

_audit_creation_method           SHELXL-2014/7
_shelx_SHELXL_version_number     2014/7
_chemical_name_systematic        ?
_chemical_name_common            ?
_chemical_melting_point          ?
_chemical_formula_moiety         ?
_chemical_formula_sum            'C36 H30 Cl2 Fe N10 O10'
_chemical_formula_weight         889.45

loop_
_atom_type_symbol
_atom_type_description
_atom_type_scat_dispersion_real
_atom_type_scat_dispersion_imag
_atom_type_scat_source
C C -0.0020 0.0020 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
N N -0.0031 0.0040 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
O O -0.0041 0.0074 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Cl Cl 0.1408 0.1896 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Fe Fe 0.2064 0.9930 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'

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

_shelx_space_group_comment       
;
The symmetry employed for this shelxl refinement is uniquely defined
by the following loop, which should always be used as a source of
symmetry information in preference to the above space-group names.
They are only intended as comments.
;

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

_cell_length_a                   15.717(3)
_cell_length_b                   20.127(3)
_cell_length_c                   24.672(4)
_cell_angle_alpha                90
_cell_angle_beta                 90.353(10)
_cell_angle_gamma                90
_cell_volume                     7805(2)
_cell_formula_units_Z            8
_cell_measurement_temperature    250(2)
_cell_measurement_reflns_used    443
_cell_measurement_theta_min      3.56
_cell_measurement_theta_max      9.68

_exptl_crystal_description       block
_exptl_crystal_colour            red
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    ?
_exptl_crystal_density_diffrn    1.514
_exptl_crystal_F_000             3648
_exptl_transmission_factor_min   ?
_exptl_transmission_factor_max   ?
_exptl_crystal_size_max          0.100
_exptl_crystal_size_mid          0.070
_exptl_crystal_size_min          0.050
_exptl_absorpt_coefficient_mu    0.746
_shelx_estimated_absorpt_T_min   0.929
_shelx_estimated_absorpt_T_max   0.964
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_correction_T_min  0.321
_exptl_absorpt_correction_T_max  0.747
_exptl_absorpt_process_details   'SADABS-2012/1  (Sheldrick, 2012)'
_exptl_absorpt_special_details   ?
_diffrn_ambient_temperature      250(2)
_diffrn_radiation_wavelength     0.7749
_diffrn_radiation_type           synchrotron
_diffrn_radiation_source         'Advanced Light Source Beamline 11.3.1'
_diffrn_radiation_monochromator  silicon(111)
_diffrn_measurement_device_type  'Bruker Apex2'
_diffrn_measurement_method       ω
_diffrn_detector_area_resol_mean 8.3
_diffrn_reflns_number            15377
_diffrn_reflns_av_unetI/netI     0.1619
_diffrn_reflns_av_R_equivalents  0.1751
_diffrn_reflns_limit_h_min       -11
_diffrn_reflns_limit_h_max       11
_diffrn_reflns_limit_k_min       -14
_diffrn_reflns_limit_k_max       14
_diffrn_reflns_limit_l_min       -17
_diffrn_reflns_limit_l_max       17
_diffrn_reflns_theta_min         2.768
_diffrn_reflns_theta_max         15.947
_diffrn_reflns_theta_full        15.947
_diffrn_measured_fraction_theta_max 0.992
_diffrn_measured_fraction_theta_full 0.992
_diffrn_reflns_Laue_measured_fraction_max 0.992
_diffrn_reflns_Laue_measured_fraction_full 0.992
_diffrn_reflns_point_group_measured_fraction_max 0.992
_diffrn_reflns_point_group_measured_fraction_full 0.992
_reflns_number_total             2904
_reflns_number_gt                1715
_reflns_threshold_expression     'I > 2σ(I)'
_reflns_Friedel_coverage         0.000
_reflns_Friedel_fraction_max     .
_reflns_Friedel_fraction_full    .

_reflns_special_details          
;
 Reflections were merged by SHELXL according to the crystal
 class for the calculation of statistics and refinement.
 
 _reflns_Friedel_fraction is defined as the number of unique
 Friedel pairs measured divided by the number that would be
 possible theoretically, ignoring centric projections and
 systematic absences.


The images contain diffraction patterens from two samples: The low spin
initial compound, and  the low spin/high spin mixed Transient,
 from which this refinement was done.  The two neccesary unit cells and
 orientation matrices were determined
using CELL_NOW and RLATT, and manually combined into an orientation matrix 
file (*.p4p).To seperate the reflections, the SAINT integration
 engine was used in command line mode, and set up with a sample mask. An 
example is shown below:
SMAP=1, 1, 2
This indicates that the first two orientation matrices belong to sample 1, and 
the third belongs to sample 2.  For all commands relating to cell or symmetry 
later on, comma-delimited lists were used to specify distinct parameters.
Listed below are most of the pertinent SAINT commands in an example from the 
SAINT manual:

FILTPOINTGP=-1, 2/m  //indicating sample 1 is triclinic and 2 is monoclinic
CRYST_SYS=1,3
PAR_MASK=TPS2, TP	//restaining the  twinned cells to be similar
GPAR_MASK=TPS2, TP    //and also restraining Detector pitch and xtal trans

 explained in the SAINT manual as
"Two-sample integration, where first sample is a two-component
twin and second component is a single crystal.  In the first sample,
constrain cell constants of the second component to those of the
first.  For both samples, constrain crystal translations and
 detector pitch"


In this case, the SAINT commands used were as follows: 
SMAP=1, 2, 
CRYST_SYS=3, 3
PAR_MASK=TP, TP
GPAR_MASK=TP, TP

This integration yielded two reflection files, both in HKLF4 format.
;

_computing_data_collection       'Apex2 v2012.10-0 (Bruker, 2012)'
_computing_cell_refinement       'SAINT V8.34A(Bruker, 2012)'
_computing_data_reduction        SAINT
_computing_structure_solution    SHELXT
_computing_structure_refinement  'SHELXL-2014/7 (Sheldrick, 2014)'
_computing_molecular_graphics    
;
     	SHELXTL 5.1, XP (Sheldrick, 1994)
	ShelXle Rev 699 (Hubschle, 2011)
;
_computing_publication_material  SHELXL-2014/7
_refine_special_details          
;
 All hydrogens were assigned geometrically and refined as riding, with 
U(H) = 1.2*U(C) for secondary and aromatic carbons, and 
U(H) = 1.5*U(C) for terminal carbons. The hydrogens on N1, N5 N6 and N10 
were found in the difference map first, then affixed geometrically, with 
U(H) = 1.2*U(N)


The disordered perchlorates were modeled as split sites, using the 
following restraints:
SADI_ClO4 0.01 Cl1 O1 Cl1 O2 Cl1 O3 Cl1 O4
SADI_ClO4 0.02 O1 O2 O1 O3 O1 O4 O2 O3 O2 O4 O3 O4

There are some large thermal parameters on some of the perchlorate oxygen
atoms, but splitting the anions further did not seem to add any
new chemical information.

A RIGU command was employed to aid in refinement. 


;

_diffrn_orient_matrix_UB_11      -0.00442
_diffrn_orient_matrix_UB_12      -0.01419
_diffrn_orient_matrix_UB_13      -0.03876
_diffrn_orient_matrix_UB_21      0.02481
_diffrn_orient_matrix_UB_22      0.04343
_diffrn_orient_matrix_UB_23      -0.01164
_diffrn_orient_matrix_UB_31      0.05842
_diffrn_orient_matrix_UB_32      -0.01952
_diffrn_orient_matrix_UB_33      0.00228
_diffrn_orient_matrix_type       'Sparks (1982)'

_refine_ls_structure_factor_coef Fsqd
_refine_ls_matrix_type           full
_refine_ls_weighting_scheme      calc
_refine_ls_weighting_details     
'w=1/[σ²(Fo²)+(0.1724P)²+203.9031P] where P=(Fo²+2Fc²)/3'
_atom_sites_solution_primary     ?
_atom_sites_solution_secondary   ?
_atom_sites_solution_hydrogens   geom
_refine_ls_hydrogen_treatment    constr
_refine_ls_extinction_method     none
_refine_ls_extinction_coef       .
_refine_ls_number_reflns         2904
_refine_ls_number_parameters     1063
_refine_ls_number_restraints     1482
_refine_ls_R_factor_all          0.1998
_refine_ls_R_factor_gt           0.1521
_refine_ls_wR_factor_ref         0.3892
_refine_ls_wR_factor_gt          0.3468
_refine_ls_goodness_of_fit_ref   1.136
_refine_ls_restrained_S_all      0.890
_refine_ls_shift/su_max          0.000
_refine_ls_shift/su_mean         0.000

loop_
_atom_site_label
_atom_site_type_symbol
_atom_site_fract_x
_atom_site_fract_y
_atom_site_fract_z
_atom_site_U_iso_or_equiv
_atom_site_adp_type
_atom_site_occupancy
_atom_site_site_symmetry_order
_atom_site_calc_flag
_atom_site_refinement_flags_posn
_atom_site_refinement_flags_adp
_atom_site_refinement_flags_occupancy
_atom_site_disorder_assembly
_atom_site_disorder_group
Cl1_1 Cl 1.0180(9) 0.8767(7) 0.3926(5) 0.155(6) Uani 1 1 d D U . . .
O1_1 O 1.1052(11) 0.8707(13) 0.3851(10) 0.150(10) Uani 1 1 d D U . . .
O2_1 O 0.9745(16) 0.8533(14) 0.3476(9) 0.186(11) Uani 1 1 d D U . . .
O3_1 O 0.9967(17) 0.9418(9) 0.4039(12) 0.192(12) Uani 1 1 d D U . . .
O4_1 O 0.9957(17) 0.8372(12) 0.4370(9) 0.184(11) Uani 1 1 d D U . . .
Cl1_2 Cl 0.5001(8) 0.9114(7) 0.2394(5) 0.148(6) Uani 1 1 d D U . . .
O1_2 O 0.4498(14) 0.8560(10) 0.2287(9) 0.149(10) Uani 1 1 d D U . . .
O2_2 O 0.5310(16) 0.9366(13) 0.1909(8) 0.168(11) Uani 1 1 d D U . . .
O3_2 O 0.5676(13) 0.8925(12) 0.2726(9) 0.158(10) Uani 1 1 d D U . . .
O4_2 O 0.4515(16) 0.9594(11) 0.2650(10) 0.175(11) Uani 1 1 d D U . . .
Cl1_3 Cl 0.0023(9) 0.4486(7) 0.3713(5) 0.154(6) Uani 1 1 d D U . . .
O1_3 O 0.0684(14) 0.4926(12) 0.3816(11) 0.166(11) Uani 1 1 d D U . . .
O2_3 O 0.0331(17) 0.3888(10) 0.3520(11) 0.189(12) Uani 1 1 d D U . . .
O3_3 O -0.0521(16) 0.4772(13) 0.3331(10) 0.189(11) Uani 1 1 d D U . . .
O4_3 O -0.0430(18) 0.4373(14) 0.4187(9) 0.199(12) Uani 1 1 d D U . . .
Cl1_4 Cl 0.5036(9) 0.6388(7) 0.4913(5) 0.160(6) Uani 1 1 d D U . . .
O1_4 O 0.4617(15) 0.6166(12) 0.4452(8) 0.149(10) Uani 1 1 d D U . . .
O2_4 O 0.4843(19) 0.7054(9) 0.5003(11) 0.190(12) Uani 1 1 d D U . . .
O3_4 O 0.4783(19) 0.6025(13) 0.5362(9) 0.209(12) Uani 1 1 d D U . . .
O4_4 O 0.5911(12) 0.6326(15) 0.4852(11) 0.201(12) Uani 1 1 d D U . . .
Fe01 Fe 0.2238(4) 0.6848(3) 0.3474(2) 0.094(3) Uani 1 1 d . U . . .
Fe02 Fe 0.7299(4) 0.7343(3) 0.3549(2) 0.099(3) Uani 1 1 d . U . . .
O1 O 0.177(2) 0.8676(18) 0.5024(13) 0.145(11) Uani 1 1 d . U . . .
O2 O 0.330(2) 0.722(2) 0.1469(13) 0.138(11) Uani 1 1 d . U . . .
O101 O 0.840(2) 0.582(2) 0.1832(14) 0.165(14) Uani 1 1 d . U . . .
O102 O 0.632(2) 0.752(2) 0.5801(13) 0.143(11) Uani 1 1 d . U . . .
N1 N 0.1641(19) 0.7500(18) 0.4529(13) 0.099(10) Uani 1 1 d . U . . .
H1B H 0.1550 0.7898 0.4404 0.119 Uiso 1 1 calc R U . . .
N2 N 0.189(2) 0.698(2) 0.4241(14) 0.100(8) Uani 1 1 d . U . . .
N3 N 0.249(2) 0.5998(18) 0.3743(14) 0.092(7) Uani 1 1 d . U . . .
N4 N 0.274(2) 0.641(2) 0.2846(15) 0.097(7) Uani 1 1 d . U . . .
N5 N 0.289(2) 0.6541(19) 0.2330(15) 0.112(11) Uani 1 1 d . U . . .
H5A H 0.2777 0.6920 0.2178 0.135 Uiso 1 1 calc R U . . .
N6 N 0.396(2) 0.7348(19) 0.3972(12) 0.099(9) Uani 1 1 d . U . . .
H6A H 0.4098 0.7001 0.4163 0.119 Uiso 1 1 calc R U . . .
N7 N 0.326(2) 0.7378(19) 0.3619(13) 0.095(7) Uani 1 1 d . U . . .
N8 N 0.202(2) 0.7657(19) 0.3117(13) 0.102(7) Uani 1 1 d . U . . .
N9 N 0.109(2) 0.666(2) 0.3215(13) 0.098(7) Uani 1 1 d . U . . .
N10 N 0.056(2) 0.6152(18) 0.3240(12) 0.098(10) Uani 1 1 d . U . . .
H10C H 0.0657 0.5780 0.3408 0.117 Uiso 1 1 calc R U . . .
N101 N 0.787(2) 0.6893(18) 0.2312(15) 0.104(10) Uani 1 1 d . U . . .
H10D H 0.7748 0.6473 0.2351 0.124 Uiso 1 1 calc R U . . .
N102 N 0.7771(19) 0.734(2) 0.2711(14) 0.093(8) Uani 1 1 d . U . . .
N103 N 0.7653(19) 0.8311(18) 0.3360(15) 0.094(8) Uani 1 1 d . U . . .
N104 N 0.697(2) 0.7958(19) 0.4265(14) 0.097(8) Uani 1 1 d . U . . .
N105 N 0.666(2) 0.789(2) 0.4774(15) 0.115(11) Uani 1 1 d . U . . .
H10E H 0.6462 0.7520 0.4913 0.138 Uiso 1 1 calc R U . . .
N106 N 0.914(2) 0.7115(19) 0.4153(14) 0.112(11) Uani 1 1 d . U . . .
H10F H 0.9328 0.7519 0.4112 0.135 Uiso 1 1 calc R U . . .
N107 N 0.839(2) 0.692(2) 0.3931(13) 0.101(8) Uani 1 1 d . U . . .
N108 N 0.705(3) 0.6337(18) 0.3672(13) 0.097(8) Uani 1 1 d . U . . .
N109 N 0.606(2) 0.718(2) 0.3232(13) 0.099(8) Uani 1 1 d . U . . .
N110 N 0.550(2) 0.7500(19) 0.2923(13) 0.106(10) Uani 1 1 d . U . . .
H11A H 0.5533 0.7921 0.2847 0.127 Uiso 1 1 calc R U . . .
C1 C 0.189(4) 0.939(3) 0.494(2) 0.20(3) Uani 1 1 d . U . . .
H1A H 0.2146 0.9470 0.4595 0.296 Uiso 1 1 calc R U . . .
H1C H 0.1337 0.9610 0.4958 0.296 Uiso 1 1 calc R U . . .
H1D H 0.2250 0.9565 0.5230 0.296 Uiso 1 1 calc R U . . .
C2 C 0.140(3) 0.845(3) 0.551(2) 0.128(16) Uani 1 1 d . U . . .
C3 C 0.114(3) 0.887(3) 0.593(2) 0.155(19) Uani 1 1 d . U . . .
H3A H 0.1187 0.9333 0.5913 0.186 Uiso 1 1 calc R U . . .
C4 C 0.080(3) 0.854(3) 0.636(2) 0.139(18) Uani 1 1 d . U . . .
H4A H 0.0638 0.8800 0.6665 0.167 Uiso 1 1 calc R U . . .
C5 C 0.067(3) 0.786(3) 0.639(2) 0.139(18) Uani 1 1 d . U . . .
H5B H 0.0412 0.7666 0.6694 0.167 Uiso 1 1 calc R U . . .
C6 C 0.093(3) 0.749(3) 0.5956(19) 0.127(15) Uani 1 1 d . U . . .
H6B H 0.0889 0.7021 0.5978 0.152 Uiso 1 1 calc R U . . .
C7 C 0.126(3) 0.777(3) 0.549(2) 0.105(12) Uani 1 1 d . U . . .
C8 C 0.155(3) 0.731(3) 0.507(2) 0.107(13) Uani 1 1 d . U . . .
C9 C 0.178(2) 0.667(2) 0.5073(19) 0.100(12) Uani 1 1 d . U . . .
H9A H 0.1795 0.6403 0.5384 0.120 Uiso 1 1 calc R U . . .
C10 C 0.201(3) 0.646(3) 0.456(2) 0.106(14) Uani 1 1 d . U . . .
C11 C 0.234(3) 0.589(3) 0.4308(19) 0.099(12) Uani 1 1 d . U . . .
C12 C 0.252(3) 0.529(3) 0.454(2) 0.128(17) Uani 1 1 d . U . . .
H12A H 0.2413 0.5215 0.4907 0.154 Uiso 1 1 calc R U . . .
C13 C 0.285(3) 0.480(3) 0.423(2) 0.144(19) Uani 1 1 d . U . . .
H13A H 0.2961 0.4386 0.4393 0.173 Uiso 1 1 calc R U . . .
C14 C 0.303(3) 0.489(3) 0.3673(19) 0.128(16) Uani 1 1 d . U . . .
H14A H 0.3245 0.4542 0.3460 0.153 Uiso 1 1 calc R U . . .
C15 C 0.288(3) 0.550(3) 0.346(2) 0.108(13) Uani 1 1 d . U . . .
C16 C 0.294(3) 0.579(3) 0.291(2) 0.092(11) Uani 1 1 d . U . . .
C17 C 0.333(3) 0.552(2) 0.2444(17) 0.108(13) Uani 1 1 d . U . . .
H17A H 0.3589 0.5106 0.2402 0.130 Uiso 1 1 calc R U . . .
C18 C 0.326(3) 0.602(3) 0.206(2) 0.101(12) Uani 1 1 d . U . . .
C19 C 0.357(3) 0.605(3) 0.148(2) 0.116(13) Uani 1 1 d . U . . .
C20 C 0.387(3) 0.545(3) 0.126(2) 0.137(16) Uani 1 1 d . U . . .
H20A H 0.3868 0.5047 0.1450 0.164 Uiso 1 1 calc R U . . .
C21 C 0.417(3) 0.554(3) 0.071(2) 0.141(16) Uani 1 1 d . U . . .
H21A H 0.4403 0.5168 0.0533 0.170 Uiso 1 1 calc R U . . .
C22 C 0.413(4) 0.611(3) 0.046(2) 0.17(2) Uani 1 1 d . U . . .
H22A H 0.4290 0.6108 0.0090 0.202 Uiso 1 1 calc R U . . .
C23 C 0.388(3) 0.670(3) 0.067(2) 0.148(17) Uani 1 1 d . U . . .
H23A H 0.3916 0.7093 0.0465 0.177 Uiso 1 1 calc R U . . .
C24 C 0.357(3) 0.670(3) 0.121(3) 0.130(16) Uani 1 1 d . U . . .
C25 C 0.337(3) 0.786(3) 0.1215(18) 0.152(18) Uani 1 1 d . U . . .
H25A H 0.3145 0.8198 0.1457 0.228 Uiso 1 1 calc R U . . .
H25B H 0.3956 0.7956 0.1134 0.228 Uiso 1 1 calc R U . . .
H25C H 0.3036 0.7860 0.0881 0.228 Uiso 1 1 calc R U . . .
C26 C 0.438(3) 0.792(2) 0.3975(18) 0.115(15) Uani 1 1 d . U . . .
H26A H 0.4861 0.8025 0.4184 0.138 Uiso 1 1 calc R U . . .
C27 C 0.398(3) 0.833(2) 0.3625(16) 0.103(12) Uani 1 1 d . U . . .
H27A H 0.4149 0.8768 0.3534 0.124 Uiso 1 1 calc R U . . .
C28 C 0.325(3) 0.800(3) 0.3419(18) 0.103(12) Uani 1 1 d . U . . .
C29 C 0.257(3) 0.817(3) 0.3057(17) 0.091(11) Uani 1 1 d . U . . .
C30 C 0.246(3) 0.870(2) 0.2714(16) 0.099(12) Uani 1 1 d . U . . .
H30A H 0.2883 0.9023 0.2666 0.119 Uiso 1 1 calc R U . . .
C31 C 0.172(3) 0.873(2) 0.2453(17) 0.109(14) Uani 1 1 d . U . . .
H31A H 0.1614 0.9097 0.2225 0.131 Uiso 1 1 calc R U . . .
C32 C 0.110(3) 0.826(2) 0.2496(17) 0.109(13) Uani 1 1 d . U . . .
H32A H 0.0584 0.8315 0.2303 0.131 Uiso 1 1 calc R U . . .
C33 C 0.123(3) 0.769(3) 0.2838(16) 0.088(10) Uani 1 1 d . U . . .
C34 C 0.072(3) 0.710(3) 0.2915(17) 0.101(13) Uani 1 1 d . U . . .
C35 C -0.009(3) 0.690(2) 0.2757(17) 0.107(13) Uani 1 1 d . U . . .
H35A H -0.0492 0.7138 0.2550 0.128 Uiso 1 1 calc R U . . .
C36 C -0.015(3) 0.629(2) 0.2971(16) 0.102(13) Uani 1 1 d . U . . .
H36A H -0.0619 0.6011 0.2935 0.123 Uiso 1 1 calc R U . . .
C101 C 0.858(5) 0.514(3) 0.187(2) 0.24(4) Uani 1 1 d . U . . .
H10A H 0.8458 0.4990 0.2239 0.362 Uiso 1 1 calc R U . . .
H10B H 0.8229 0.4896 0.1618 0.362 Uiso 1 1 calc R U . . .
H10L H 0.9174 0.5067 0.1795 0.362 Uiso 1 1 calc R U . . .
C102 C 0.853(3) 0.611(3) 0.134(3) 0.145(18) Uani 1 1 d . U . . .
C103 C 0.884(3) 0.577(3) 0.090(2) 0.146(18) Uani 1 1 d . U . . .
H10G H 0.8974 0.5319 0.0918 0.176 Uiso 1 1 calc R U . . .
C104 C 0.893(3) 0.612(3) 0.045(2) 0.140(18) Uani 1 1 d . U . . .
H10H H 0.9088 0.5899 0.0131 0.168 Uiso 1 1 calc R U . . .
C105 C 0.880(3) 0.680(3) 0.042(2) 0.134(17) Uani 1 1 d . U . . .
H10I H 0.8891 0.7023 0.0091 0.160 Uiso 1 1 calc R U . . .
C106 C 0.852(3) 0.717(3) 0.0876(19) 0.129(15) Uani 1 1 d . U . . .
H10J H 0.8429 0.7635 0.0865 0.154 Uiso 1 1 calc R U . . .
C107 C 0.840(3) 0.679(3) 0.135(2) 0.123(14) Uani 1 1 d . U . . .
C108 C 0.817(3) 0.715(3) 0.184(2) 0.102(12) Uani 1 1 d . U . . .
C109 C 0.827(2) 0.782(2) 0.1955(17) 0.094(11) Uani 1 1 d . U . . .
H10K H 0.8496 0.8149 0.1723 0.113 Uiso 1 1 calc R U . . .
C110 C 0.798(3) 0.792(3) 0.249(2) 0.101(13) Uani 1 1 d . U . . .
C111 C 0.798(3) 0.848(3) 0.2836(18) 0.095(12) Uani 1 1 d . U . . .
C112 C 0.825(2) 0.913(2) 0.2721(18) 0.099(13) Uani 1 1 d . U . . .
H11B H 0.8466 0.9239 0.2378 0.119 Uiso 1 1 calc R U . . .
C113 C 0.819(3) 0.959(2) 0.3097(18) 0.110(14) Uani 1 1 d . U . . .
H11C H 0.8395 1.0019 0.3019 0.132 Uiso 1 1 calc R U . . .
C114 C 0.786(2) 0.947(2) 0.3603(18) 0.101(12) Uani 1 1 d . U . . .
H11D H 0.7817 0.9803 0.3868 0.121 Uiso 1 1 calc R U . . .
C115 C 0.757(3) 0.881(3) 0.3701(19) 0.097(12) Uani 1 1 d . U . . .
C116 C 0.720(3) 0.862(3) 0.422(2) 0.094(11) Uani 1 1 d . U . . .
C117 C 0.703(3) 0.893(3) 0.4689(19) 0.116(14) Uani 1 1 d . U . . .
H11E H 0.7127 0.9378 0.4767 0.139 Uiso 1 1 calc R U . . .
C118 C 0.669(3) 0.849(3) 0.503(2) 0.110(13) Uani 1 1 d . U . . .
C119 C 0.645(3) 0.860(3) 0.563(2) 0.129(15) Uani 1 1 d . U . . .
C120 C 0.641(3) 0.930(3) 0.578(2) 0.145(17) Uani 1 1 d . U . . .
H12B H 0.6513 0.9624 0.5517 0.173 Uiso 1 1 calc R U . . .
C121 C 0.623(4) 0.947(3) 0.630(2) 0.18(2) Uani 1 1 d . U . . .
H12C H 0.6252 0.9912 0.6434 0.221 Uiso 1 1 calc R U . . .
C122 C 0.601(3) 0.892(3) 0.662(2) 0.153(19) Uani 1 1 d . U . . .
H12D H 0.5828 0.9044 0.6968 0.184 Uiso 1 1 calc R U . . .
C123 C 0.598(3) 0.821(3) 0.654(2) 0.141(16) Uani 1 1 d . U . . .
H12E H 0.5842 0.7877 0.6792 0.169 Uiso 1 1 calc R U . . .
C124 C 0.621(3) 0.816(3) 0.599(2) 0.126(15) Uani 1 1 d . U . . .
C125 C 0.611(4) 0.699(3) 0.616(2) 0.18(2) Uani 1 1 d . U . . .
H12H H 0.6209 0.6566 0.5984 0.271 Uiso 1 1 calc R U . . .
H12I H 0.6473 0.7015 0.6484 0.271 Uiso 1 1 calc R U . . .
H12J H 0.5521 0.7019 0.6269 0.271 Uiso 1 1 calc R U . . .
C126 C 0.958(3) 0.666(2) 0.4440(18) 0.119(15) Uani 1 1 d . U . . .
H12F H 1.0106 0.6694 0.4623 0.143 Uiso 1 1 calc R U . . .
C127 C 0.908(3) 0.615(3) 0.4393(17) 0.109(13) Uani 1 1 d . U . . .
H12G H 0.9195 0.5735 0.4550 0.130 Uiso 1 1 calc R U . . .
C128 C 0.835(3) 0.627(3) 0.4097(17) 0.097(11) Uani 1 1 d . U . . .
C129 C 0.756(3) 0.592(3) 0.3928(16) 0.094(11) Uani 1 1 d . U . . .
C130 C 0.745(3) 0.523(2) 0.4013(16) 0.110(13) Uani 1 1 d . U . . .
H13B H 0.7874 0.4956 0.4160 0.132 Uiso 1 1 calc R U . . .
C131 C 0.666(3) 0.502(3) 0.3859(17) 0.120(15) Uani 1 1 d . U . . .
H13C H 0.6517 0.4570 0.3922 0.144 Uiso 1 1 calc R U . . .
C132 C 0.609(3) 0.540(3) 0.3628(19) 0.134(17) Uani 1 1 d . U . . .
H13D H 0.5555 0.5229 0.3525 0.161 Uiso 1 1 calc R U . . .
C133 C 0.629(3) 0.605(3) 0.3541(16) 0.096(11) Uani 1 1 d . U . . .
C134 C 0.575(3) 0.654(2) 0.3243(16) 0.089(10) Uani 1 1 d . U . . .
C135 C 0.500(3) 0.651(3) 0.2930(18) 0.115(15) Uani 1 1 d . U . . .
H13E H 0.4656 0.6132 0.2866 0.138 Uiso 1 1 calc R U . . .
C136 C 0.489(3) 0.710(3) 0.2749(18) 0.112(14) Uani 1 1 d . U . . .
H13F H 0.4441 0.7236 0.2523 0.135 Uiso 1 1 calc R U . . .


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

loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
_geom_bond_publ_flag
Cl1_1 O3_1 1.382(12) . ?
Cl1_1 O2_1 1.384(12) . ?
Cl1_1 O1_1 1.390(12) . ?
Cl1_1 O4_1 1.400(12) . ?
Cl1_2 O4_2 1.386(12) . ?
Cl1_2 O2_2 1.389(12) . ?
Cl1_2 O3_2 1.390(12) . ?
Cl1_2 O1_2 1.392(12) . ?
Cl1_3 O2_3 1.384(12) . ?
Cl1_3 O1_3 1.388(12) . ?
Cl1_3 O4_3 1.391(12) . ?
Cl1_3 O3_3 1.392(12) . ?
Cl1_4 O1_4 1.384(12) . ?
Cl1_4 O4_4 1.389(12) . ?
Cl1_4 O3_4 1.389(12) . ?
Cl1_4 O2_4 1.392(12) . ?
Fe01 N3 1.88(3) . ?
Fe01 N8 1.88(4) . ?
Fe01 N9 1.95(4) . ?
Fe01 N4 1.96(4) . ?
Fe01 N7 1.96(4) . ?
Fe01 N2 1.99(4) . ?
Fe02 N103 2.08(4) . ?
Fe02 N108 2.09(4) . ?
Fe02 N109 2.12(4) . ?
Fe02 N107 2.14(4) . ?
Fe02 N102 2.20(4) . ?
Fe02 N104 2.22(4) . ?
O1 C2 1.42(5) . ?
O1 C1 1.46(5) . ?
O2 C24 1.30(5) . ?
O2 C25 1.44(5) . ?
O101 C102 1.37(6) . ?
O101 C101 1.40(5) . ?
O102 C124 1.38(5) . ?
O102 C125 1.44(5) . ?
N1 N2 1.32(4) . ?
N1 C8 1.39(4) . ?
N1 H1B 0.8700 . ?
N2 C10 1.31(4) . ?
N3 C15 1.36(5) . ?
N3 C11 1.43(4) . ?
N4 C16 1.29(4) . ?
N4 N5 1.33(4) . ?
N5 C18 1.36(5) . ?
N5 H5A 0.8700 . ?
N6 C26 1.33(4) . ?
N6 N7 1.39(4) . ?
N6 H6A 0.8700 . ?
N7 C28 1.34(4) . ?
N8 C29 1.36(4) . ?
N8 C33 1.42(4) . ?
N9 C34 1.29(4) . ?
N9 N10 1.32(4) . ?
N10 C36 1.32(4) . ?
N10 H10C 0.8700 . ?
N101 N102 1.34(4) . ?
N101 C108 1.36(5) . ?
N101 H10D 0.8700 . ?
N102 C110 1.33(4) . ?
N103 C115 1.32(4) . ?
N103 C111 1.43(5) . ?
N104 N105 1.36(4) . ?
N104 C116 1.39(4) . ?
N105 C118 1.36(5) . ?
N105 H10E 0.8700 . ?
N106 N107 1.35(4) . ?
N106 C126 1.35(4) . ?
N106 H10F 0.8700 . ?
N107 C128 1.36(4) . ?
N108 C129 1.33(5) . ?
N108 C133 1.36(5) . ?
N109 N110 1.33(4) . ?
N109 C134 1.37(4) . ?
N110 C136 1.32(4) . ?
N110 H11A 0.8700 . ?
C1 H1A 0.9700 . ?
C1 H1C 0.9700 . ?
C1 H1D 0.9700 . ?
C2 C7 1.39(6) . ?
C2 C3 1.40(6) . ?
C3 C4 1.37(6) . ?
C3 H3A 0.9400 . ?
C4 C5 1.39(5) . ?
C4 H4A 0.9400 . ?
C5 C6 1.38(5) . ?
C5 H5B 0.9400 . ?
C6 C7 1.39(5) . ?
C6 H6B 0.9400 . ?
C7 C8 1.47(6) . ?
C8 C9 1.32(5) . ?
C9 C10 1.39(5) . ?
C9 H9A 0.9400 . ?
C10 C11 1.40(5) . ?
C11 C12 1.37(5) . ?
C12 C13 1.34(5) . ?
C12 H12A 0.9400 . ?
C13 C14 1.42(5) . ?
C13 H13A 0.9400 . ?
C14 C15 1.36(5) . ?
C14 H14A 0.9400 . ?
C15 C16 1.47(5) . ?
C16 C17 1.42(5) . ?
C17 C18 1.38(5) . ?
C17 H17A 0.9400 . ?
C18 C19 1.52(6) . ?
C19 C20 1.40(6) . ?
C19 C24 1.46(6) . ?
C20 C21 1.45(5) . ?
C20 H20A 0.9400 . ?
C21 C22 1.31(6) . ?
C21 H21A 0.9400 . ?
C22 C23 1.36(6) . ?
C22 H22A 0.9400 . ?
C23 C24 1.42(6) . ?
C23 H23A 0.9400 . ?
C25 H25A 0.9700 . ?
C25 H25B 0.9700 . ?
C25 H25C 0.9700 . ?
C26 C27 1.35(5) . ?
C26 H26A 0.9400 . ?
C27 C28 1.42(5) . ?
C27 H27A 0.9400 . ?
C28 C29 1.44(5) . ?
C29 C30 1.37(5) . ?
C30 C31 1.33(5) . ?
C30 H30A 0.9400 . ?
C31 C32 1.36(5) . ?
C31 H31A 0.9400 . ?
C32 C33 1.45(5) . ?
C32 H32A 0.9400 . ?
C33 C34 1.44(5) . ?
C34 C35 1.38(5) . ?
C35 C36 1.34(5) . ?
C35 H35A 0.9400 . ?
C36 H36A 0.9400 . ?
C101 H10A 0.9700 . ?
C101 H10B 0.9700 . ?
C101 H10L 0.9700 . ?
C102 C107 1.37(6) . ?
C102 C103 1.37(6) . ?
C103 C104 1.33(6) . ?
C103 H10G 0.9400 . ?
C104 C105 1.38(5) . ?
C104 H10H 0.9400 . ?
C105 C106 1.42(5) . ?
C105 H10I 0.9400 . ?
C106 C107 1.42(6) . ?
C106 H10J 0.9400 . ?
C107 C108 1.46(6) . ?
C108 C109 1.39(5) . ?
C109 C110 1.42(5) . ?
C109 H10K 0.9400 . ?
C110 C111 1.42(5) . ?
C111 C112 1.40(5) . ?
C112 C113 1.31(5) . ?
C112 H11B 0.9400 . ?
C113 C114 1.38(5) . ?
C113 H11C 0.9400 . ?
C114 C115 1.41(5) . ?
C114 H11D 0.9400 . ?
C115 C116 1.46(5) . ?
C116 C117 1.34(5) . ?
C117 C118 1.33(5) . ?
C117 H11E 0.9400 . ?
C118 C119 1.56(6) . ?
C119 C124 1.31(6) . ?
C119 C120 1.45(6) . ?
C120 C121 1.37(6) . ?
C120 H12B 0.9400 . ?
C121 C122 1.41(6) . ?
C121 H12C 0.9400 . ?
C122 C123 1.43(6) . ?
C122 H12D 0.9400 . ?
C123 C124 1.41(6) . ?
C123 H12E 0.9400 . ?
C125 H12H 0.9700 . ?
C125 H12I 0.9700 . ?
C125 H12J 0.9700 . ?
C126 C127 1.30(5) . ?
C126 H12F 0.9400 . ?
C127 C128 1.37(5) . ?
C127 H12G 0.9400 . ?
C128 C129 1.49(5) . ?
C129 C130 1.40(5) . ?
C130 C131 1.37(5) . ?
C130 H13B 0.9400 . ?
C131 C132 1.31(5) . ?
C131 H13C 0.9400 . ?
C132 C133 1.37(5) . ?
C132 H13D 0.9400 . ?
C133 C134 1.49(5) . ?
C134 C135 1.40(5) . ?
C135 C136 1.29(5) . ?
C135 H13E 0.9400 . ?
C136 H13F 0.9400 . ?

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
O3_1 Cl1_1 O2_1 111.4(12) . . ?
O3_1 Cl1_1 O1_1 110.5(12) . . ?
O2_1 Cl1_1 O1_1 110.3(12) . . ?
O3_1 Cl1_1 O4_1 108.5(12) . . ?
O2_1 Cl1_1 O4_1 108.1(12) . . ?
O1_1 Cl1_1 O4_1 107.9(11) . . ?
O4_2 Cl1_2 O2_2 109.6(12) . . ?
O4_2 Cl1_2 O3_2 110.0(12) . . ?
O2_2 Cl1_2 O3_2 109.6(11) . . ?
O4_2 Cl1_2 O1_2 109.4(12) . . ?
O2_2 Cl1_2 O1_2 109.3(11) . . ?
O3_2 Cl1_2 O1_2 108.9(11) . . ?
O2_3 Cl1_3 O1_3 110.8(12) . . ?
O2_3 Cl1_3 O4_3 109.1(12) . . ?
O1_3 Cl1_3 O4_3 109.7(12) . . ?
O2_3 Cl1_3 O3_3 109.9(12) . . ?
O1_3 Cl1_3 O3_3 108.5(12) . . ?
O4_3 Cl1_3 O3_3 108.7(12) . . ?
O1_4 Cl1_4 O4_4 110.4(11) . . ?
O1_4 Cl1_4 O3_4 110.4(12) . . ?
O4_4 Cl1_4 O3_4 109.1(12) . . ?
O1_4 Cl1_4 O2_4 109.8(12) . . ?
O4_4 Cl1_4 O2_4 108.8(12) . . ?
O3_4 Cl1_4 O2_4 108.4(11) . . ?
N3 Fe01 N8 172.7(15) . . ?
N3 Fe01 N9 97.6(15) . . ?
N8 Fe01 N9 81.1(17) . . ?
N3 Fe01 N4 77.3(16) . . ?
N8 Fe01 N4 95.5(15) . . ?
N9 Fe01 N4 91.6(13) . . ?
N3 Fe01 N7 105.1(15) . . ?
N8 Fe01 N7 76.4(17) . . ?
N9 Fe01 N7 157.4(17) . . ?
N4 Fe01 N7 93.4(13) . . ?
N3 Fe01 N2 81.1(16) . . ?
N8 Fe01 N2 106.1(15) . . ?
N9 Fe01 N2 94.3(13) . . ?
N4 Fe01 N2 158.2(16) . . ?
N7 Fe01 N2 89.3(13) . . ?
N103 Fe02 N108 173.4(14) . . ?
N103 Fe02 N109 108.2(14) . . ?
N108 Fe02 N109 74.0(16) . . ?
N103 Fe02 N107 105.0(14) . . ?
N108 Fe02 N107 72.5(16) . . ?
N109 Fe02 N107 146.5(16) . . ?
N103 Fe02 N102 72.7(15) . . ?
N108 Fe02 N102 101.4(13) . . ?
N109 Fe02 N102 88.1(12) . . ?
N107 Fe02 N102 97.9(12) . . ?
N103 Fe02 N104 73.7(14) . . ?
N108 Fe02 N104 112.3(13) . . ?
N109 Fe02 N104 99.7(12) . . ?
N107 Fe02 N104 93.5(12) . . ?
N102 Fe02 N104 146.3(15) . . ?
C2 O1 C1 119(4) . . ?
C24 O2 C25 119(5) . . ?
C102 O101 C101 117(5) . . ?
C124 O102 C125 117(5) . . ?
N2 N1 C8 109(4) . . ?
N2 N1 H1B 125.6 . . ?
C8 N1 H1B 125.6 . . ?
C10 N2 N1 111(4) . . ?
C10 N2 Fe01 115(4) . . ?
N1 N2 Fe01 134(3) . . ?
C15 N3 C11 118(4) . . ?
C15 N3 Fe01 125(4) . . ?
C11 N3 Fe01 116(3) . . ?
C16 N4 N5 106(4) . . ?
C16 N4 Fe01 116(4) . . ?
N5 N4 Fe01 138(3) . . ?
N4 N5 C18 113(4) . . ?
N4 N5 H5A 123.5 . . ?
C18 N5 H5A 123.5 . . ?
C26 N6 N7 111(4) . . ?
C26 N6 H6A 124.7 . . ?
N7 N6 H6A 124.7 . . ?
C28 N7 N6 106(4) . . ?
C28 N7 Fe01 115(4) . . ?
N6 N7 Fe01 137(3) . . ?
C29 N8 C33 118(5) . . ?
C29 N8 Fe01 126(4) . . ?
C33 N8 Fe01 115(4) . . ?
C34 N9 N10 106(5) . . ?
C34 N9 Fe01 118(4) . . ?
N10 N9 Fe01 136(3) . . ?
C36 N10 N9 110(4) . . ?
C36 N10 H10C 125.2 . . ?
N9 N10 H10C 125.2 . . ?
N102 N101 C108 115(4) . . ?
N102 N101 H10D 122.7 . . ?
C108 N101 H10D 122.7 . . ?
C110 N102 N101 105(4) . . ?
C110 N102 Fe02 117(4) . . ?
N101 N102 Fe02 137(3) . . ?
C115 N103 C111 115(5) . . ?
C115 N103 Fe02 123(4) . . ?
C111 N103 Fe02 122(3) . . ?
N105 N104 C116 106(4) . . ?
N105 N104 Fe02 140(3) . . ?
C116 N104 Fe02 114(3) . . ?
C118 N105 N104 108(4) . . ?
C118 N105 H10E 125.9 . . ?
N104 N105 H10E 125.9 . . ?
N107 N106 C126 117(4) . . ?
N107 N106 H10F 121.6 . . ?
C126 N106 H10F 121.6 . . ?
N106 N107 C128 102(4) . . ?
N106 N107 Fe02 139(3) . . ?
C128 N107 Fe02 118(4) . . ?
C129 N108 C133 112(5) . . ?
C129 N108 Fe02 125(4) . . ?
C133 N108 Fe02 123(4) . . ?
N110 N109 C134 103(4) . . ?
N110 N109 Fe02 137(3) . . ?
C134 N109 Fe02 118(4) . . ?
C136 N110 N109 111(4) . . ?
C136 N110 H11A 124.3 . . ?
N109 N110 H11A 124.3 . . ?
O1 C1 H1A 109.5 . . ?
O1 C1 H1C 109.5 . . ?
H1A C1 H1C 109.5 . . ?
O1 C1 H1D 109.5 . . ?
H1A C1 H1D 109.5 . . ?
H1C C1 H1D 109.5 . . ?
C7 C2 C3 126(6) . . ?
C7 C2 O1 111(6) . . ?
C3 C2 O1 124(6) . . ?
C4 C3 C2 114(6) . . ?
C4 C3 H3A 122.9 . . ?
C2 C3 H3A 122.9 . . ?
C3 C4 C5 125(6) . . ?
C3 C4 H4A 117.7 . . ?
C5 C4 H4A 117.7 . . ?
C6 C5 C4 118(5) . . ?
C6 C5 H5B 121.2 . . ?
C4 C5 H5B 121.2 . . ?
C5 C6 C7 123(5) . . ?
C5 C6 H6B 118.7 . . ?
C7 C6 H6B 118.7 . . ?
C2 C7 C6 115(6) . . ?
C2 C7 C8 127(6) . . ?
C6 C7 C8 117(6) . . ?
C9 C8 N1 105(5) . . ?
C9 C8 C7 133(5) . . ?
N1 C8 C7 122(5) . . ?
C8 C9 C10 111(5) . . ?
C8 C9 H9A 124.7 . . ?
C10 C9 H9A 124.7 . . ?
N2 C10 C9 105(5) . . ?
N2 C10 C11 116(5) . . ?
C9 C10 C11 138(5) . . ?
C12 C11 C10 128(5) . . ?
C12 C11 N3 120(5) . . ?
C10 C11 N3 112(5) . . ?
C13 C12 C11 120(5) . . ?
C13 C12 H12A 120.2 . . ?
C11 C12 H12A 120.2 . . ?
C12 C13 C14 122(5) . . ?
C12 C13 H13A 118.9 . . ?
C14 C13 H13A 118.9 . . ?
C15 C14 C13 117(5) . . ?
C15 C14 H14A 121.6 . . ?
C13 C14 H14A 121.6 . . ?
C14 C15 N3 123(5) . . ?
C14 C15 C16 134(5) . . ?
N3 C15 C16 102(5) . . ?
N4 C16 C17 111(5) . . ?
N4 C16 C15 119(5) . . ?
C17 C16 C15 129(5) . . ?
C18 C17 C16 104(5) . . ?
C18 C17 H17A 127.8 . . ?
C16 C17 H17A 127.8 . . ?
N5 C18 C17 105(5) . . ?
N5 C18 C19 125(5) . . ?
C17 C18 C19 130(5) . . ?
C20 C19 C24 126(6) . . ?
C20 C19 C18 116(5) . . ?
C24 C19 C18 118(6) . . ?
C19 C20 C21 112(5) . . ?
C19 C20 H20A 124.2 . . ?
C21 C20 H20A 124.2 . . ?
C22 C21 C20 122(6) . . ?
C22 C21 H21A 118.8 . . ?
C20 C21 H21A 118.8 . . ?
C21 C22 C23 127(6) . . ?
C21 C22 H22A 116.7 . . ?
C23 C22 H22A 116.7 . . ?
C22 C23 C24 117(6) . . ?
C22 C23 H23A 121.3 . . ?
C24 C23 H23A 121.3 . . ?
O2 C24 C23 125(6) . . ?
O2 C24 C19 119(6) . . ?
C23 C24 C19 115(6) . . ?
O2 C25 H25A 109.5 . . ?
O2 C25 H25B 109.5 . . ?
H25A C25 H25B 109.5 . . ?
O2 C25 H25C 109.5 . . ?
H25A C25 H25C 109.5 . . ?
H25B C25 H25C 109.5 . . ?
N6 C26 C27 108(5) . . ?
N6 C26 H26A 126.2 . . ?
C27 C26 H26A 126.2 . . ?
C26 C27 C28 108(5) . . ?
C26 C27 H27A 126.2 . . ?
C28 C27 H27A 126.2 . . ?
N7 C28 C27 108(5) . . ?
N7 C28 C29 118(5) . . ?
C27 C28 C29 134(5) . . ?
N8 C29 C30 126(5) . . ?
N8 C29 C28 103(5) . . ?
C30 C29 C28 131(5) . . ?
C31 C30 C29 116(5) . . ?
C31 C30 H30A 122.0 . . ?
C29 C30 H30A 122.0 . . ?
C30 C31 C32 124(5) . . ?
C30 C31 H31A 118.1 . . ?
C32 C31 H31A 118.1 . . ?
C31 C32 C33 120(5) . . ?
C31 C32 H32A 119.9 . . ?
C33 C32 H32A 119.9 . . ?
N8 C33 C34 113(5) . . ?
N8 C33 C32 116(5) . . ?
C34 C33 C32 131(5) . . ?
N9 C34 C35 112(5) . . ?
N9 C34 C33 113(6) . . ?
C35 C34 C33 135(5) . . ?
C36 C35 C34 103(5) . . ?
C36 C35 H35A 128.7 . . ?
C34 C35 H35A 128.7 . . ?
N10 C36 C35 110(5) . . ?
N10 C36 H36A 125.1 . . ?
C35 C36 H36A 125.1 . . ?
O101 C101 H10A 109.5 . . ?
O101 C101 H10B 109.5 . . ?
H10A C101 H10B 109.5 . . ?
O101 C101 H10L 109.5 . . ?
H10A C101 H10L 109.5 . . ?
H10B C101 H10L 109.5 . . ?
O101 C102 C107 113(6) . . ?
O101 C102 C103 123(6) . . ?
C107 C102 C103 124(7) . . ?
C104 C103 C102 116(6) . . ?
C104 C103 H10G 122.0 . . ?
C102 C103 H10G 122.0 . . ?
C103 C104 C105 123(6) . . ?
C103 C104 H10H 118.3 . . ?
C105 C104 H10H 118.3 . . ?
C104 C105 C106 122(5) . . ?
C104 C105 H10I 119.1 . . ?
C106 C105 H10I 119.1 . . ?
C105 C106 C107 114(5) . . ?
C105 C106 H10J 123.0 . . ?
C107 C106 H10J 123.0 . . ?
C102 C107 C106 120(6) . . ?
C102 C107 C108 124(6) . . ?
C106 C107 C108 116(6) . . ?
N101 C108 C109 104(5) . . ?
N101 C108 C107 127(5) . . ?
C109 C108 C107 129(5) . . ?
C108 C109 C110 107(5) . . ?
C108 C109 H10K 126.7 . . ?
C110 C109 H10K 126.7 . . ?
N102 C110 C109 110(5) . . ?
N102 C110 C111 118(5) . . ?
C109 C110 C111 132(5) . . ?
C112 C111 C110 129(5) . . ?
C112 C111 N103 121(5) . . ?
C110 C111 N103 110(5) . . ?
C113 C112 C111 119(5) . . ?
C113 C112 H11B 120.4 . . ?
C111 C112 H11B 120.4 . . ?
C112 C113 C114 123(5) . . ?
C112 C113 H11C 118.5 . . ?
C114 C113 H11C 118.5 . . ?
C113 C114 C115 116(5) . . ?
C113 C114 H11D 121.9 . . ?
C115 C114 H11D 121.9 . . ?
N103 C115 C114 125(5) . . ?
N103 C115 C116 113(5) . . ?
C114 C115 C116 122(5) . . ?
C117 C116 N104 108(5) . . ?
C117 C116 C115 136(6) . . ?
N104 C116 C115 116(5) . . ?
C118 C117 C116 109(6) . . ?
C118 C117 H11E 125.7 . . ?
C116 C117 H11E 125.7 . . ?
C117 C118 N105 109(5) . . ?
C117 C118 C119 127(6) . . ?
N105 C118 C119 124(5) . . ?
C124 C119 C120 118(6) . . ?
C124 C119 C118 129(6) . . ?
C120 C119 C118 113(5) . . ?
C121 C120 C119 120(5) . . ?
C121 C120 H12B 120.1 . . ?
C119 C120 H12B 120.1 . . ?
C120 C121 C122 112(6) . . ?
C120 C121 H12C 124.2 . . ?
C122 C121 H12C 124.2 . . ?
C121 C122 C123 136(6) . . ?
C121 C122 H12D 112.0 . . ?
C123 C122 H12D 112.0 . . ?
C124 C123 C122 101(5) . . ?
C124 C123 H12E 129.5 . . ?
C122 C123 H12E 129.5 . . ?
C119 C124 O102 111(6) . . ?
C119 C124 C123 133(7) . . ?
O102 C124 C123 116(6) . . ?
O102 C125 H12H 109.5 . . ?
O102 C125 H12I 109.5 . . ?
H12H C125 H12I 109.5 . . ?
O102 C125 H12J 109.5 . . ?
H12H C125 H12J 109.5 . . ?
H12I C125 H12J 109.5 . . ?
C127 C126 N106 100(5) . . ?
C127 C126 H12F 129.9 . . ?
N106 C126 H12F 129.9 . . ?
C126 C127 C128 114(5) . . ?
C126 C127 H12G 122.8 . . ?
C128 C127 H12G 122.8 . . ?
N107 C128 C127 107(5) . . ?
N107 C128 C129 114(5) . . ?
C127 C128 C129 139(5) . . ?
N108 C129 C130 128(5) . . ?
N108 C129 C128 110(5) . . ?
C130 C129 C128 122(5) . . ?
C131 C130 C129 113(5) . . ?
C131 C130 H13B 123.7 . . ?
C129 C130 H13B 123.7 . . ?
C132 C131 C130 123(6) . . ?
C132 C131 H13C 118.3 . . ?
C130 C131 H13C 118.3 . . ?
C131 C132 C133 119(6) . . ?
C131 C132 H13D 120.7 . . ?
C133 C132 H13D 120.7 . . ?
N108 C133 C132 124(5) . . ?
N108 C133 C134 110(5) . . ?
C132 C133 C134 126(5) . . ?
N109 C134 C135 110(5) . . ?
N109 C134 C133 115(5) . . ?
C135 C134 C133 135(5) . . ?
C136 C135 C134 105(5) . . ?
C136 C135 H13E 127.7 . . ?
C134 C135 H13E 127.7 . . ?
C135 C136 N110 111(5) . . ?
C135 C136 H13F 124.5 . . ?
N110 C136 H13F 124.5 . . ?

_refine_diff_density_max         0.469
_refine_diff_density_min         -0.451
_refine_diff_density_rms         0.095


# start Validation Reply Form

_vrf_ABSMU01_Stage1_Initial      
;
PROBLEM: Calculation of _exptl_absorpt_correction_mu
                not performed for this radiation type.
RESPONSE: Absorption corrections were done with SADABS that takes
 the x-ray wavelengths from the raw data. PLATON does
 not calculate these corrections for synchrotron radiation data.
;

_vrf_PLAT984_Stage1_Initial      
;
PROBLEM: The element-f Deviates from the B&C-Value
RESPONSE: DISP values for each element type present were
 calculated for the 0.7749 angstrom x-rays using XDISP
 implemented in winGX, and using the Brennan model.
;

_vrf_ABSMU01_Stage1_Transient    
;
PROBLEM: Calculation of _exptl_absorpt_correction_mu
                not performed for this radiation type.
RESPONSE: Absorption corrections were done with SADABS that takes
 the x-ray wavelengths from the raw data. PLATON does
 not calculate these corrections for synchrotron radiation data.
;

_vrf_THETM01_Stage1_Transient    
;
PROBLEM: The value of sine(theta_max)/wavelength is less than 0.550
            Calculated sin(theta_max)/wavelength =    0.3546
RESPONSE: This data set contained diffraction from two samples: an initial
compound and the intermediate transient phase. All overlapped 
reflections were omitted at the integration stage, leaving the completeness 
lower than optimal. Due to the deletion of overlapped reflections,
the number of data is low, especially for this intermediate phase, for 
which diffraction was very poor and only significant at low resolution,
resulting in very low thetamax.
;

_vrf_PLAT088_Stage1_Transient    
;
PROBLEM: Poor Data / Parameter Ratio ....................       2.73 Note  
RESPONSE: Due to the deletion of overlapped reflections,
the number of data is low. Measures have been taken to not over-refine the
structure, i.e., not attempting to refine split disordered groups 
anisotropically, etc. 
;

_vrf_RFACG01_Stage1_Transient    
;
PROBLEM: The value of the R factor is > 0.15
            R factor given   0.152
RESPONSE: This data set contained diffraction from two samples: an initial
compound and the intermediate transient phase. All overlapped 
reflections were omitted at the integration stage, leaving the completeness 
lower than optimal. Due to the deletion of overlapped reflections,
the number of data is low, especially for this intermediate phase, for 
which diffraction was very poor and only significant at low resolution,
resulting in very low thetamax. This is likely the main reason for
the rather poor R and wR factors.
;

_vrf_RFACR01_Stage1_Transient    
;
PROBLEM: The value of the weighted R factor is > 0.35
            Weighted R factor given   0.389
RESPONSE: This data set contained diffraction from two samples: an initial
compound and the intermediate transient phase. All overlapped 
reflections were omitted at the integration stage, leaving the completeness 
lower than optimal. Due to the deletion of overlapped reflections,
the number of data is low, especially for this intermediate phase, for 
which diffraction was very poor and only significant at low resolution,
resulting in very low thetamax. This is likely the main reason for
the rather poor R and wR factors.
;

_vrf_PLAT084_Stage1_Transient    
;
PROBLEM: High wR2 Value (i.e. > 0.25) ...................       0.39 Report
RESPONSE: This data set contained diffraction from two samples: an initial
compound and the intermediate transient phase. All overlapped 
reflections were omitted at the integration stage, leaving the completeness 
lower than optimal. Due to the deletion of overlapped reflections,
the number of data is low, especially for this intermediate phase, for 
which diffraction was very poor and only significant at low resolution,
resulting in very low thetamax. This is likely the main reason for
the rather poor R and wR factors.
;

_vrf_PLAT984_Stage1_Transient    
;
PROBLEM: The element-f Deviates from the B&C-Value
RESPONSE: DISP values for each element type present were
 calculated for the 0.7749 angstrom x-rays using XDISP
 implemented in winGX, and using the Brennan model.
;

_vrf_REFNR01_Stage1_Transient    
;
PROBLEM: Ratio of reflections to parameters is < 6 for a
            centrosymmetric structure 
RESPONSE: This data set contained diffraction from two samples: an initial
compound and the intermediate transient phase. All overlapped 
reflections were omitted at the integration stage, leaving the completeness 
lower than optimal. Due to the deletion of overlapped reflections,
the number of data is low, especially for this intermediate phase.
;


# end Validation Reply Form



####################################################################### 
# 
# 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_Stage2_Initial
_database_code_depnum_ccdc_archive 'CCDC 1053053'
_audit_update_record             
;
2015-12-22 deposited with the CCDC.
2016-01-05 downloaded from the CCDC.
;

_audit_creation_method           SHELXL-2014/7
_shelx_SHELXL_version_number     2014/7
_chemical_name_systematic        ?
_chemical_name_common            ?
_chemical_melting_point          ?
_chemical_formula_moiety         '(C36 H30 Fe N10 O2),2(Cl O4),1.25(C3 H6 O)'
_chemical_formula_sum            'C39.75 H37.50 Cl2 Fe N10 O11.25'
_chemical_formula_weight         962.05

loop_
_atom_type_symbol
_atom_type_description
_atom_type_scat_dispersion_real
_atom_type_scat_dispersion_imag
_atom_type_scat_source
C C -0.0020 0.0020
'WCROMER Program in WinGX L.Kissel & R.H.Pratt Acta Cryst A46 170 1990'
H H 0.0000 0.0000
'WCROMER Program in WinGX L.Kissel & R.H.Pratt Acta Cryst A46 170 1990'
N N -0.0031 0.0040
'WCROMER Program in WinGX L.Kissel & R.H.Pratt Acta Cryst A46 170 1990'
O O -0.0041 0.0074
'WCROMER Program in WinGX L.Kissel & R.H.Pratt Acta Cryst A46 170 1990'
Cl Cl 0.1408 0.1896
'WCROMER Program in WinGX L.Kissel & R.H.Pratt Acta Cryst A46 170 1990'
Fe Fe 0.2064 0.9930
'WCROMER Program in WinGX L.Kissel & R.H.Pratt Acta Cryst A46 170 1990'

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

_shelx_space_group_comment       
;
The symmetry employed for this shelxl refinement is uniquely defined
by the following loop, which should always be used as a source of
symmetry information in preference to the above space-group names.
They are only intended as comments.
;

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

_cell_length_a                   14.165(5)
_cell_length_b                   21.596(8)
_cell_length_c                   15.414(6)
_cell_angle_alpha                90
_cell_angle_beta                 114.290(4)
_cell_angle_gamma                90
_cell_volume                     4298(3)
_cell_formula_units_Z            4
_cell_measurement_temperature    250(2)
_cell_measurement_reflns_used    1221
_cell_measurement_theta_min      2.68
_cell_measurement_theta_max      24.6

_exptl_crystal_description       block
_exptl_crystal_colour            orange
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    ?
_exptl_crystal_density_diffrn    1.487
_exptl_crystal_F_000             1984
_exptl_transmission_factor_min   ?
_exptl_transmission_factor_max   ?
_exptl_crystal_size_max          0.100
_exptl_crystal_size_mid          0.070
_exptl_crystal_size_min          0.050
_exptl_absorpt_coefficient_mu    0.688
_shelx_estimated_absorpt_T_min   0.934
_shelx_estimated_absorpt_T_max   0.966
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_correction_T_min  0.6919
_exptl_absorpt_correction_T_max  0.7469
_exptl_absorpt_process_details   'SADABS-2012/1  (Sheldrick, 2012)'
_exptl_absorpt_special_details   ?
_diffrn_ambient_temperature      250(2)
_diffrn_radiation_wavelength     0.7749
_diffrn_radiation_type           synchrotron
_diffrn_radiation_source         'Advanced Light Source Beamline 11.3.1'
_diffrn_radiation_monochromator  silicon(111)
_diffrn_measurement_device_type  'Bruker Apex2'
_diffrn_measurement_method       ω
_diffrn_detector_area_resol_mean 8.3
_diffrn_reflns_number            4017
_diffrn_reflns_av_unetI/netI     0.0443
_diffrn_reflns_av_R_equivalents  0.0232
_diffrn_reflns_limit_h_min       -17
_diffrn_reflns_limit_h_max       16
_diffrn_reflns_limit_k_min       -25
_diffrn_reflns_limit_k_max       25
_diffrn_reflns_limit_l_min       -18
_diffrn_reflns_limit_l_max       18
_diffrn_reflns_theta_min         2.681
_diffrn_reflns_theta_max         28.046
_diffrn_reflns_theta_full        27.706
_diffrn_measured_fraction_theta_max 0.261
_diffrn_measured_fraction_theta_full 0.250
_diffrn_reflns_Laue_measured_fraction_max 0.261
_diffrn_reflns_Laue_measured_fraction_full 0.250
_diffrn_reflns_point_group_measured_fraction_max 0.261
_diffrn_reflns_point_group_measured_fraction_full 0.250
_reflns_number_total             2103
_reflns_number_gt                1487
_reflns_threshold_expression     'I > 2σ(I)'
_reflns_Friedel_coverage         0.000
_reflns_Friedel_fraction_max     .
_reflns_Friedel_fraction_full    .

_reflns_special_details          
;
 Reflections were merged by SHELXL according to the crystal
 class for the calculation of statistics and refinement.
 
 _reflns_Friedel_fraction is defined as the number of unique
 Friedel pairs measured divided by the number that would be
 possible theoretically, ignoring centric projections and
 systematic absences.

The images contain diffraction patterens from three samples: This low spin
initial compound, the high spin final product (which is twinned) and the low
 spin/high spin mixed Transient.  The three
neccesary unit cells and four orientation matrices were determined
using CELL_NOW and RLATT, and manually combined into an orientation matrix 
file (*.p4p).To seperate the reflections, the SAINT integration
 engine was used in command line mode, and set up with a sample mask. An 
example is shown below:
SMAP=1, 1, 2
This indicates that the first two orientation matrices belong to sample 1, and 
the third belongs to sample 2.  For all commands relating to cell or symmetry 
later on, comma-delimited lists were used to specify distinct parameters.
Listed below are most of the pertinent SAINT commands in an example from the 
SAINT manual:

FILTPOINTGP=-1, 2/m  //indicating sample 1 is triclinic and 2 is monoclinic
CRYST_SYS=1,3
PAR_MASK=TPS2, TP	//restaining the  twinned cells to be similar
GPAR_MASK=TPS2, TP    //and also restraining Detector pitch and xtal trans

 explained in the SAINT manual as
"Two-sample integration, where first sample is a two-component
twin and second component is a single crystal.  In the first sample,
constrain cell constants of the second component to those of the
first.  For both samples, constrain crystal translations and
 detector pitch"


In this case, the SAINT commands used were as follows: 
SMAP=1, 2, 3, 3
CRYST_SYS=3, 3, 1
PAR_MASK=TP, TP, TPS2
GPAR_MASK=TP, TP, TPS2

This integration yielded three reflection files; two HKLF4 and one HKLF5
;
_computing_data_collection       'Apex2 v2012.10-0 (Bruker, 2012)'
_computing_cell_refinement       'SAINT V8.27B(Bruker, 2012)'
_computing_data_reduction        SAINT
_computing_structure_solution    SHELXS
_computing_structure_refinement  'SHELXL-2014/7 (Sheldrick, 2014)'
_computing_molecular_graphics    
;
     	SHELXTL 5.1, XP (Sheldrick, 1994)
	ShelXle Rev 699 (Hubschle, 2011)
;
_computing_publication_material  SHELXL-2014/7

_refine_special_details          
;
 All hydrogens were assigned geometrically and refined as riding, with 
U(H) = 1.2*U(C) for secondary and aromatic carbons, and 
U(H) = 1.5*U(C) for terminal carbons. The hydrogens on N1, N5 N6 and N10 
were found in the difference map first, then affixed geometrically, with 
U(H) = 1.2*U(N)

This stucture contains one low occupancy acetone, and two disordered 
perchlorate anions. The occupancy of the acetone molecule was determined
by fixing the thermal parameters of the atoms, and allowing their occupancies
to refine. The average of the occupancies was approximately 0.25, so the 
occupancy for the molecule was fixed at 0.25.

The disordered perchlorates were modeled as split sites, using the 
following restraints:
SADI_ClO4 0.01 Cl1 O1 Cl1 O2 Cl1 O3 Cl1 O4
SADI_ClO4 0.02 O1 O2 O1 O3 O1 O4 O2 O3 O2 O4 O3 O4

There are some large thermal parameters on some of the perchlorate oxygen
atoms, but splitting the anions further did not seem to add any
new chemical information.

The acetone molecules are not well behaved, and SADIs were used to help them.
SADI 0.01 C40 C41 C40 C42 C37 C38 C37 C39
SADI 0.01 C40 O4 C37 O3
SIMU 0.01 C41 C42 C38 C39

;

_diffrn_orient_matrix_UB_11      -0.04852
_diffrn_orient_matrix_UB_12      0.01369
_diffrn_orient_matrix_UB_13      0.02844
_diffrn_orient_matrix_UB_21      0.01050
_diffrn_orient_matrix_UB_22      -0.04028
_diffrn_orient_matrix_UB_23      0.03475
_diffrn_orient_matrix_UB_31      0.05945
_diffrn_orient_matrix_UB_32      0.01829
_diffrn_orient_matrix_UB_33      0.05523
_diffrn_orient_matrix_type       'Sparks (1982)'

_refine_ls_structure_factor_coef Fsqd
_refine_ls_matrix_type           full
_refine_ls_weighting_scheme      calc
_refine_ls_weighting_details     
'w=1/[σ²(Fo²)+(0.1345P)²+5.4453P] where P=(Fo²+2Fc²)/3'
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_atom_sites_solution_hydrogens   geom
_refine_ls_hydrogen_treatment    constr
_refine_ls_extinction_method     none
_refine_ls_extinction_coef       .
_refine_ls_number_reflns         2103
_refine_ls_number_parameters     580
_refine_ls_number_restraints     904
_refine_ls_R_factor_all          0.1070
_refine_ls_R_factor_gt           0.0771
_refine_ls_wR_factor_ref         0.2322
_refine_ls_wR_factor_gt          0.2095
_refine_ls_goodness_of_fit_ref   1.229
_refine_ls_restrained_S_all      1.096
_refine_ls_shift/su_max          0.000
_refine_ls_shift/su_mean         0.000

loop_
_atom_site_label
_atom_site_type_symbol
_atom_site_fract_x
_atom_site_fract_y
_atom_site_fract_z
_atom_site_U_iso_or_equiv
_atom_site_adp_type
_atom_site_occupancy
_atom_site_site_symmetry_order
_atom_site_calc_flag
_atom_site_refinement_flags_posn
_atom_site_refinement_flags_adp
_atom_site_refinement_flags_occupancy
_atom_site_disorder_assembly
_atom_site_disorder_group
Fe1 Fe 0.42434(12) 0.26513(9) 0.60267(10) 0.0255(5) Uani 1 1 d . U . . .
O1 O 0.2788(14) 0.3435(9) 0.9571(11) 0.109(6) Uani 1 1 d . U . . .
O2 O 0.5055(10) 0.1769(7) 0.3205(9) 0.067(4) Uani 1 1 d . U . . .
O3 O 0.6642(10) 0.1228(7) 0.9225(9) 0.079(4) Uani 1 1 d D U . . .
N1 N 0.3631(7) 0.2383(5) 0.7728(6) 0.033(2) Uani 1 1 d . U . . .
H1 H 0.3699 0.1982 0.7772 0.040 Uiso 1 1 calc R U . . .
N2 N 0.3794(7) 0.2736(6) 0.7091(7) 0.031(2) Uani 1 1 d . U . . .
N3 N 0.4003(8) 0.3529(5) 0.5994(7) 0.031(2) Uani 1 1 d . U . . .
N4 N 0.4580(8) 0.2892(6) 0.4960(7) 0.033(2) Uani 1 1 d . U . . .
N5 N 0.4861(8) 0.2611(5) 0.4329(7) 0.037(2) Uani 1 1 d . U . . .
H5 H 0.4965 0.2214 0.4326 0.044 Uiso 1 1 calc R U . . .
N6 N 0.6458(7) 0.3071(5) 0.7311(7) 0.035(2) Uani 1 1 d . U . . .
H6 H 0.6346 0.3468 0.7301 0.042 Uiso 1 1 calc R U . . .
N7 N 0.5727(8) 0.2649(5) 0.6870(7) 0.032(2) Uani 1 1 d . U . . .
N8 N 0.4564(8) 0.1775(5) 0.6081(7) 0.033(2) Uani 1 1 d . U . . .
N9 N 0.2859(7) 0.2302(7) 0.5176(7) 0.032(2) Uani 1 1 d . U . . .
N10 N 0.1908(7) 0.2538(6) 0.4697(8) 0.040(3) Uani 1 1 d . U . . .
H10 H 0.1744 0.2929 0.4641 0.048 Uiso 1 1 calc R U . . .
C1 C 0.253(2) 0.3793(11) 1.0221(18) 0.152(13) Uani 1 1 d . U . . .
H1A H 0.2092 0.4138 0.9886 0.228 Uiso 1 1 calc R U . . .
H1B H 0.3156 0.3949 1.0726 0.228 Uiso 1 1 calc R U . . .
H1C H 0.2158 0.3535 1.0493 0.228 Uiso 1 1 calc R U . . .
C2 C 0.2823(14) 0.2806(13) 0.9694(13) 0.068(5) Uani 1 1 d . U . . .
C3 C 0.2583(16) 0.2577(13) 1.0394(14) 0.083(6) Uani 1 1 d . U . . .
H3A H 0.2401 0.2835 1.0792 0.099 Uiso 1 1 calc R U . . .
C4 C 0.2620(14) 0.1941(13) 1.0489(14) 0.079(6) Uani 1 1 d . U . . .
H4A H 0.2500 0.1763 1.0990 0.094 Uiso 1 1 calc R U . . .
C5 C 0.2833(14) 0.1549(10) 0.9853(12) 0.074(5) Uani 1 1 d . U . . .
H5A H 0.2796 0.1116 0.9899 0.088 Uiso 1 1 calc R U . . .
C6 C 0.3097(13) 0.1810(11) 0.9168(11) 0.063(5) Uani 1 1 d . U . . .
H6A H 0.3288 0.1556 0.8771 0.076 Uiso 1 1 calc R U . . .
C7 C 0.3079(11) 0.2449(10) 0.9065(10) 0.049(4) Uani 1 1 d . U . . .
C8 C 0.3336(10) 0.2753(8) 0.8306(9) 0.040(3) Uani 1 1 d . U . . .
C9 C 0.3330(11) 0.3355(8) 0.8039(10) 0.047(3) Uani 1 1 d . U . . .
H9A H 0.3178 0.3708 0.8315 0.056 Uiso 1 1 calc R U . . .
C10 C 0.3605(9) 0.3330(7) 0.7252(9) 0.035(3) Uani 1 1 d . U . . .
C11 C 0.3725(10) 0.3799(8) 0.6629(9) 0.034(3) Uani 1 1 d . U . . .
C12 C 0.3567(10) 0.4426(8) 0.6627(11) 0.047(3) Uani 1 1 d . U . . .
H12A H 0.3373 0.4606 0.7084 0.057 Uiso 1 1 calc R U . . .
C13 C 0.3698(11) 0.4800(7) 0.5931(10) 0.051(3) Uani 1 1 d . U . . .
H13A H 0.3578 0.5229 0.5901 0.061 Uiso 1 1 calc R U . . .
C14 C 0.4001(10) 0.4514(8) 0.5312(11) 0.045(3) Uani 1 1 d . U . . .
H14A H 0.4099 0.4751 0.4844 0.054 Uiso 1 1 calc R U . . .
C15 C 0.4172(10) 0.3885(8) 0.5346(9) 0.035(3) Uani 1 1 d . U . . .
C16 C 0.4484(9) 0.3491(7) 0.4717(9) 0.033(3) Uani 1 1 d . U . . .
C17 C 0.4742(10) 0.3584(7) 0.3935(9) 0.043(3) Uani 1 1 d . U . . .
H17A H 0.4757 0.3964 0.3643 0.051 Uiso 1 1 calc R U . . .
C18 C 0.4966(9) 0.3017(7) 0.3687(8) 0.038(3) Uani 1 1 d . U . . .
C19 C 0.5249(11) 0.2805(8) 0.2928(9) 0.044(3) Uani 1 1 d . U . . .
C20 C 0.5475(13) 0.3269(8) 0.2396(11) 0.062(4) Uani 1 1 d . U . . .
H20A H 0.5428 0.3688 0.2539 0.075 Uiso 1 1 calc R U . . .
C21 C 0.5770(15) 0.3117(11) 0.1657(13) 0.079(6) Uani 1 1 d . U . . .
H21A H 0.5963 0.3424 0.1329 0.094 Uiso 1 1 calc R U . . .
C22 C 0.5763(13) 0.2515(11) 0.1440(13) 0.072(5) Uani 1 1 d . U . . .
H22A H 0.5911 0.2411 0.0917 0.086 Uiso 1 1 calc R U . . .
C23 C 0.5550(14) 0.2031(9) 0.1939(12) 0.068(5) Uani 1 1 d . U . . .
H23A H 0.5586 0.1616 0.1772 0.081 Uiso 1 1 calc R U . . .
C24 C 0.5284(12) 0.2181(10) 0.2690(11) 0.053(4) Uani 1 1 d . U . . .
C25 C 0.507(2) 0.1143(12) 0.299(2) 0.129(12) Uani 1 1 d . U . . .
H25A H 0.5178 0.0896 0.3548 0.193 Uiso 1 1 calc R U . . .
H25B H 0.5633 0.1067 0.2796 0.193 Uiso 1 1 calc R U . . .
H25C H 0.4419 0.1030 0.2476 0.193 Uiso 1 1 calc R U . . .
C26 C 0.7397(10) 0.2799(8) 0.7776(9) 0.041(3) Uani 1 1 d . U . . .
H26A H 0.8020 0.3006 0.8139 0.050 Uiso 1 1 calc R U . . .
C27 C 0.7288(10) 0.2184(9) 0.7630(10) 0.046(4) Uani 1 1 d . U . . .
H27A H 0.7802 0.1877 0.7866 0.055 Uiso 1 1 calc R U . . .
C28 C 0.6214(10) 0.2100(7) 0.7034(9) 0.034(3) Uani 1 1 d . U . . .
C29 C 0.5556(10) 0.1585(8) 0.6586(9) 0.034(3) Uani 1 1 d . U . . .
C30 C 0.5798(12) 0.0970(8) 0.6563(11) 0.052(4) Uani 1 1 d . U . . .
H30A H 0.6480 0.0835 0.6919 0.062 Uiso 1 1 calc R U . . .
C31 C 0.5048(12) 0.0544(8) 0.6020(12) 0.063(4) Uani 1 1 d . U . . .
H31A H 0.5222 0.0125 0.6001 0.076 Uiso 1 1 calc R U . . .
C32 C 0.4011(12) 0.0754(8) 0.5495(11) 0.051(4) Uani 1 1 d . U . . .
H32A H 0.3489 0.0478 0.5121 0.062 Uiso 1 1 calc R U . . .
C33 C 0.3793(10) 0.1376(8) 0.5550(9) 0.038(3) Uani 1 1 d . U . . .
C34 C 0.2812(10) 0.1686(9) 0.5083(9) 0.036(3) Uani 1 1 d . U . . .
C35 C 0.1784(11) 0.1496(9) 0.4533(10) 0.053(3) Uani 1 1 d . U . . .
H35A H 0.1525 0.1093 0.4357 0.063 Uiso 1 1 calc R U . . .
C36 C 0.1249(11) 0.2058(8) 0.4315(10) 0.050(3) Uani 1 1 d . U . . .
H36A H 0.0532 0.2098 0.3954 0.061 Uiso 1 1 calc R U . . .
C37 C 0.6196(12) 0.0823(10) 0.9401(11) 0.058(4) Uani 1 1 d D U . . .
C38 C 0.6167(14) 0.0194(9) 0.8985(13) 0.077(5) Uani 1 1 d D U . . .
H38A H 0.6865 0.0065 0.9106 0.116 Uiso 1 1 calc R U . . .
H38B H 0.5751 0.0208 0.8304 0.116 Uiso 1 1 calc R U . . .
H38C H 0.5864 -0.0098 0.9275 0.116 Uiso 1 1 calc R U . . .
C39 C 0.5654(15) 0.0864(10) 1.0051(14) 0.092(6) Uani 1 1 d D U . . .
H39A H 0.5697 0.1284 1.0285 0.138 Uiso 1 1 calc R U . . .
H39B H 0.5980 0.0584 1.0584 0.138 Uiso 1 1 calc R U . . .
H39C H 0.4932 0.0749 0.9706 0.138 Uiso 1 1 calc R U . . .
O4 O -0.050(4) 0.062(3) 0.465(5) 0.102(19) Uiso 0.25 1 d D . P A -1
C40 C -0.028(6) 0.010(3) 0.465(5) 0.08(2) Uiso 0.25 1 d D . P A -1
C41 C 0.045(7) -0.030(5) 0.442(7) 0.11(4) Uiso 0.25 1 d D . P A -1
H41A H 0.0344 -0.0731 0.4541 0.158 Uiso 0.25 1 calc R U P A -1
H41B H 0.0326 -0.0249 0.3760 0.158 Uiso 0.25 1 calc R U P A -1
H41C H 0.1159 -0.0183 0.4823 0.158 Uiso 0.25 1 calc R U P A -1
C42 C -0.020(9) -0.003(6) 0.563(5) 0.11(3) Uiso 0.25 1 d D . P A -1
H42A H -0.0022 -0.0465 0.5780 0.160 Uiso 0.25 1 calc R U P A -1
H42B H 0.0324 0.0228 0.6083 0.160 Uiso 0.25 1 calc R U P A -1
H42C H -0.0866 0.0050 0.5649 0.160 Uiso 0.25 1 calc R U P A -1
Cl1_1 Cl 0.6957(8) 0.4657(6) 0.7456(8) 0.064(3) Uiso 0.51(2) 1 d D . P B 1
O1_1 O 0.6134(15) 0.4320(11) 0.7542(16) 0.064(9) Uiso 0.51(2) 1 d D . P B 1
O2_1 O 0.7883(12) 0.4573(11) 0.8282(12) 0.079(9) Uiso 0.51(2) 1 d D . P B 1
O3_1 O 0.6692(19) 0.5301(7) 0.738(2) 0.101(11) Uiso 0.51(2) 1 d D . P B 1
O4_1 O 0.705(2) 0.4474(13) 0.6617(14) 0.142(16) Uiso 0.51(2) 1 d D . P B 1
Cl1_2 Cl 0.6939(6) 0.4747(4) 0.7650(7) 0.043(3) Uiso 0.49(2) 1 d D . P B 2
O1_2 O 0.6021(16) 0.4396(13) 0.741(2) 0.16(3) Uiso 0.49(2) 1 d D . P B 2
O2_2 O 0.723(2) 0.5034(13) 0.8548(13) 0.144(16) Uiso 0.49(2) 1 d D . P B 2
O3_2 O 0.683(2) 0.5191(12) 0.6935(17) 0.134(15) Uiso 0.49(2) 1 d D . P B 2
O4_2 O 0.7759(16) 0.4338(10) 0.771(2) 0.116(12) Uiso 0.49(2) 1 d D . P B 2
Cl1_3 Cl 0.3065(8) 0.0524(5) 0.7365(8) 0.059(3) Uiso 0.55(3) 1 d D . P C 1
O1_3 O 0.2552(17) 0.0580(10) 0.7984(15) 0.093(10) Uiso 0.55(3) 1 d D . P C 1
O2_3 O 0.3667(17) -0.0026(8) 0.7609(18) 0.100(9) Uiso 0.55(3) 1 d D . P C 1
O3_3 O 0.2329(14) 0.0504(11) 0.6406(11) 0.106(10) Uiso 0.55(3) 1 d D . P C 1
O4_3 O 0.3717(17) 0.1049(9) 0.7500(18) 0.071(10) Uiso 0.55(3) 1 d D . P C 1
Cl1_4 Cl 0.3237(11) 0.0511(6) 0.7551(11) 0.064(5) Uiso 0.45(3) 1 d D . P C 2
O1_4 O 0.331(2) 0.0353(12) 0.8470(13) 0.091(11) Uiso 0.45(3) 1 d D . P C 2
O2_4 O 0.348(2) -0.0014(10) 0.7125(18) 0.089(10) Uiso 0.45(3) 1 d D . P C 2
O3_4 O 0.2202(13) 0.0696(12) 0.698(2) 0.109(13) Uiso 0.45(3) 1 d D . P C 2
O4_4 O 0.3941(19) 0.1002(11) 0.765(2) 0.064(11) Uiso 0.45(3) 1 d D . P C 2


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

loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
_geom_bond_publ_flag
Fe1 N3 1.923(12) . ?
Fe1 N8 1.940(12) . ?
Fe1 N4 1.961(10) . ?
Fe1 N7 1.964(10) . ?
Fe1 N2 1.997(10) . ?
Fe1 N9 2.004(10) . ?
O1 C2 1.37(2) . ?
O1 C1 1.43(2) . ?
O2 C24 1.32(2) . ?
O2 C25 1.40(2) . ?
O3 C37 1.18(2) . ?
N1 N2 1.336(13) . ?
N1 C8 1.384(15) . ?
N1 H1 0.8700 . ?
N2 C10 1.354(15) . ?
N3 C11 1.330(16) . ?
N3 C15 1.358(17) . ?
N4 N5 1.337(14) . ?
N4 C16 1.339(15) . ?
N5 C18 1.375(15) . ?
N5 H5 0.8700 . ?
N6 N7 1.336(14) . ?
N6 C26 1.359(15) . ?
N6 H6 0.8700 . ?
N7 C28 1.342(16) . ?
N8 C29 1.360(16) . ?
N8 C33 1.368(17) . ?
N9 C34 1.337(16) . ?
N9 N10 1.342(14) . ?
N10 C36 1.357(18) . ?
N10 H10 0.8700 . ?
C1 H1A 0.9700 . ?
C1 H1B 0.9700 . ?
C1 H1C 0.9700 . ?
C2 C3 1.35(3) . ?
C2 C7 1.40(2) . ?
C3 C4 1.38(2) . ?
C3 H3A 0.9400 . ?
C4 C5 1.42(3) . ?
C4 H4A 0.9400 . ?
C5 C6 1.38(2) . ?
C5 H5A 0.9400 . ?
C6 C7 1.389(19) . ?
C6 H6A 0.9400 . ?
C7 C8 1.51(2) . ?
C8 C9 1.362(17) . ?
C9 C10 1.420(17) . ?
C9 H9A 0.9400 . ?
C10 C11 1.45(2) . ?
C11 C12 1.373(16) . ?
C12 C13 1.41(2) . ?
C12 H12A 0.9400 . ?
C13 C14 1.35(2) . ?
C13 H13A 0.9400 . ?
C14 C15 1.378(16) . ?
C14 H14A 0.9400 . ?
C15 C16 1.486(19) . ?
C16 C17 1.411(17) . ?
C17 C18 1.359(18) . ?
C17 H17A 0.9400 . ?
C18 C19 1.458(18) . ?
C19 C24 1.40(2) . ?
C19 C20 1.41(2) . ?
C20 C21 1.40(2) . ?
C20 H20A 0.9400 . ?
C21 C22 1.34(2) . ?
C21 H21A 0.9400 . ?
C22 C23 1.40(2) . ?
C22 H22A 0.9400 . ?
C23 C24 1.40(2) . ?
C23 H23A 0.9400 . ?
C25 H25A 0.9700 . ?
C25 H25B 0.9700 . ?
C25 H25C 0.9700 . ?
C26 C27 1.347(17) . ?
C26 H26A 0.9400 . ?
C27 C28 1.427(17) . ?
C27 H27A 0.9400 . ?
C28 C29 1.434(19) . ?
C29 C30 1.375(17) . ?
C30 C31 1.39(2) . ?
C30 H30A 0.9400 . ?
C31 C32 1.43(2) . ?
C31 H31A 0.9400 . ?
C32 C33 1.390(17) . ?
C32 H32A 0.9400 . ?
C33 C34 1.440(19) . ?
C34 C35 1.412(18) . ?
C35 C36 1.40(2) . ?
C35 H35A 0.9400 . ?
C36 H36A 0.9400 . ?
C37 C38 1.494(16) . ?
C37 C39 1.495(16) . ?
C38 H38A 0.9700 . ?
C38 H38B 0.9700 . ?
C38 H38C 0.9700 . ?
C39 H39A 0.9700 . ?
C39 H39B 0.9700 . ?
C39 H39C 0.9700 . ?
O4 C40 1.17(2) . ?
C40 C41 1.493(18) . ?
C40 C42 1.494(18) . ?
C41 H41A 0.9700 . ?
C41 H41B 0.9700 . ?
C41 H41C 0.9700 . ?
C42 H42A 0.9700 . ?
C42 H42B 0.9700 . ?
C42 H42C 0.9700 . ?
Cl1_1 O4_1 1.410(10) . ?
Cl1_1 O2_1 1.414(9) . ?
Cl1_1 O1_1 1.427(9) . ?
Cl1_1 O3_1 1.432(10) . ?
Cl1_2 O2_2 1.413(10) . ?
Cl1_2 O1_2 1.415(10) . ?
Cl1_2 O3_2 1.420(10) . ?
Cl1_2 O4_2 1.434(10) . ?
Cl1_3 O3_3 1.417(9) . ?
Cl1_3 O2_3 1.420(9) . ?
Cl1_3 O1_3 1.422(9) . ?
Cl1_3 O4_3 1.423(9) . ?
Cl1_4 O1_4 1.420(10) . ?
Cl1_4 O2_4 1.420(9) . ?
Cl1_4 O4_4 1.422(9) . ?
Cl1_4 O3_4 1.422(10) . ?

loop_
_geom_angle_atom_site_label_1
_geom_angle_atom_site_label_2
_geom_angle_atom_site_label_3
_geom_angle
_geom_angle_site_symmetry_1
_geom_angle_site_symmetry_3
_geom_angle_publ_flag
N3 Fe1 N8 176.9(4) . . ?
N3 Fe1 N4 79.6(4) . . ?
N8 Fe1 N4 99.3(5) . . ?
N3 Fe1 N7 98.6(4) . . ?
N8 Fe1 N7 78.5(5) . . ?
N4 Fe1 N7 89.6(4) . . ?
N3 Fe1 N2 79.5(4) . . ?
N8 Fe1 N2 101.6(4) . . ?
N4 Fe1 N2 159.1(5) . . ?
N7 Fe1 N2 94.1(4) . . ?
N3 Fe1 N9 103.8(5) . . ?
N8 Fe1 N9 79.1(5) . . ?
N4 Fe1 N9 93.5(4) . . ?
N7 Fe1 N9 157.6(5) . . ?
N2 Fe1 N9 90.9(4) . . ?
C2 O1 C1 116.4(15) . . ?
C24 O2 C25 118.6(14) . . ?
N2 N1 C8 109.4(12) . . ?
N2 N1 H1 125.3 . . ?
C8 N1 H1 125.3 . . ?
N1 N2 C10 107.4(11) . . ?
N1 N2 Fe1 139.6(9) . . ?
C10 N2 Fe1 113.0(9) . . ?
C11 N3 C15 119.2(13) . . ?
C11 N3 Fe1 121.1(10) . . ?
C15 N3 Fe1 119.6(9) . . ?
N5 N4 C16 105.2(10) . . ?
N5 N4 Fe1 137.5(10) . . ?
C16 N4 Fe1 117.3(8) . . ?
N4 N5 C18 112.7(12) . . ?
N4 N5 H5 123.6 . . ?
C18 N5 H5 123.6 . . ?
N7 N6 C26 111.1(13) . . ?
N7 N6 H6 124.5 . . ?
C26 N6 H6 124.5 . . ?
N6 N7 C28 106.0(12) . . ?
N6 N7 Fe1 136.8(9) . . ?
C28 N7 Fe1 117.0(10) . . ?
C29 N8 C33 122.3(13) . . ?
C29 N8 Fe1 119.2(10) . . ?
C33 N8 Fe1 118.3(10) . . ?
C34 N9 N10 108.9(10) . . ?
C34 N9 Fe1 115.9(8) . . ?
N10 N9 Fe1 135.1(11) . . ?
N9 N10 C36 107.8(13) . . ?
N9 N10 H10 126.1 . . ?
C36 N10 H10 126.1 . . ?
O1 C1 H1A 109.5 . . ?
O1 C1 H1B 109.5 . . ?
H1A C1 H1B 109.5 . . ?
O1 C1 H1C 109.5 . . ?
H1A C1 H1C 109.5 . . ?
H1B C1 H1C 109.5 . . ?
C3 C2 O1 118(2) . . ?
C3 C2 C7 125(3) . . ?
O1 C2 C7 117.1(16) . . ?
C2 C3 C4 116(2) . . ?
C2 C3 H3A 122.0 . . ?
C4 C3 H3A 122.0 . . ?
C3 C4 C5 122.1(18) . . ?
C3 C4 H4A 119.0 . . ?
C5 C4 H4A 119.0 . . ?
C6 C5 C4 119(2) . . ?
C6 C5 H5A 120.4 . . ?
C4 C5 H5A 120.4 . . ?
C5 C6 C7 119.8(17) . . ?
C5 C6 H6A 120.1 . . ?
C7 C6 H6A 120.1 . . ?
C6 C7 C2 117.8(16) . . ?
C6 C7 C8 121.4(13) . . ?
C2 C7 C8 120.8(19) . . ?
C9 C8 N1 108.8(12) . . ?
C9 C8 C7 132.4(15) . . ?
N1 C8 C7 118.7(15) . . ?
C8 C9 C10 104.6(13) . . ?
C8 C9 H9A 127.7 . . ?
C10 C9 H9A 127.7 . . ?
N2 C10 C9 109.8(13) . . ?
N2 C10 C11 117.0(12) . . ?
C9 C10 C11 133.3(14) . . ?
N3 C11 C12 121.9(13) . . ?
N3 C11 C10 109.3(14) . . ?
C12 C11 C10 128.8(12) . . ?
C11 C12 C13 119.5(14) . . ?
C11 C12 H12A 120.3 . . ?
C13 C12 H12A 120.3 . . ?
C14 C13 C12 117.1(16) . . ?
C14 C13 H13A 121.4 . . ?
C12 C13 H13A 121.4 . . ?
C13 C14 C15 121.9(14) . . ?
C13 C14 H14A 119.1 . . ?
C15 C14 H14A 119.1 . . ?
N3 C15 C14 120.3(12) . . ?
N3 C15 C16 110.2(13) . . ?
C14 C15 C16 129.4(12) . . ?
N4 C16 C17 110.1(13) . . ?
N4 C16 C15 113.2(11) . . ?
C17 C16 C15 136.7(14) . . ?
C18 C17 C16 106.5(14) . . ?
C18 C17 H17A 126.7 . . ?
C16 C17 H17A 126.7 . . ?
C17 C18 N5 105.4(12) . . ?
C17 C18 C19 132.9(15) . . ?
N5 C18 C19 121.7(14) . . ?
C24 C19 C20 119.2(15) . . ?
C24 C19 C18 124.1(15) . . ?
C20 C19 C18 116.6(16) . . ?
C21 C20 C19 121.4(18) . . ?
C21 C20 H20A 119.3 . . ?
C19 C20 H20A 119.3 . . ?
C22 C21 C20 117.1(18) . . ?
C22 C21 H21A 121.5 . . ?
C20 C21 H21A 121.5 . . ?
C21 C22 C23 124.5(17) . . ?
C21 C22 H22A 117.7 . . ?
C23 C22 H22A 117.7 . . ?
C24 C23 C22 118.3(19) . . ?
C24 C23 H23A 120.9 . . ?
C22 C23 H23A 120.9 . . ?
O2 C24 C23 124.0(18) . . ?
O2 C24 C19 116.6(14) . . ?
C23 C24 C19 119.4(17) . . ?
O2 C25 H25A 109.5 . . ?
O2 C25 H25B 109.5 . . ?
H25A C25 H25B 109.5 . . ?
O2 C25 H25C 109.5 . . ?
H25A C25 H25C 109.5 . . ?
H25B C25 H25C 109.5 . . ?
C27 C26 N6 108.5(12) . . ?
C27 C26 H26A 125.7 . . ?
N6 C26 H26A 125.7 . . ?
C26 C27 C28 104.6(13) . . ?
C26 C27 H27A 127.7 . . ?
C28 C27 H27A 127.7 . . ?
N7 C28 C27 109.8(14) . . ?
N7 C28 C29 114.4(13) . . ?
C27 C28 C29 135.8(15) . . ?
N8 C29 C30 119.2(14) . . ?
N8 C29 C28 110.8(13) . . ?
C30 C29 C28 130.0(13) . . ?
C29 C30 C31 121.1(15) . . ?
C29 C30 H30A 119.5 . . ?
C31 C30 H30A 119.5 . . ?
C30 C31 C32 118.8(16) . . ?
C30 C31 H31A 120.6 . . ?
C32 C31 H31A 120.6 . . ?
C33 C32 C31 118.4(15) . . ?
C33 C32 H32A 120.8 . . ?
C31 C32 H32A 120.8 . . ?
N8 C33 C32 120.2(13) . . ?
N8 C33 C34 112.0(15) . . ?
C32 C33 C34 127.8(14) . . ?
N9 C34 C35 110.3(13) . . ?
N9 C34 C33 114.5(12) . . ?
C35 C34 C33 135.2(17) . . ?
C36 C35 C34 102.4(16) . . ?
C36 C35 H35A 128.8 . . ?
C34 C35 H35A 128.8 . . ?
N10 C36 C35 110.5(14) . . ?
N10 C36 H36A 124.7 . . ?
C35 C36 H36A 124.7 . . ?
O3 C37 C38 120.0(18) . . ?
O3 C37 C39 125.7(18) . . ?
C38 C37 C39 114.2(18) . . ?
C37 C38 H38A 109.5 . . ?
C37 C38 H38B 109.5 . . ?
H38A C38 H38B 109.5 . . ?
C37 C38 H38C 109.5 . . ?
H38A C38 H38C 109.5 . . ?
H38B C38 H38C 109.5 . . ?
C37 C39 H39A 109.5 . . ?
C37 C39 H39B 109.5 . . ?
H39A C39 H39B 109.5 . . ?
C37 C39 H39C 109.5 . . ?
H39A C39 H39C 109.5 . . ?
H39B C39 H39C 109.5 . . ?
O4 C40 C41 140(7) . . ?
O4 C40 C42 96(7) . . ?
C41 C40 C42 111(7) . . ?
C40 C41 H41A 109.5 . . ?
C40 C41 H41B 109.5 . . ?
H41A C41 H41B 109.5 . . ?
C40 C41 H41C 109.5 . . ?
H41A C41 H41C 109.5 . . ?
H41B C41 H41C 109.5 . . ?
C40 C42 H42A 109.5 . . ?
C40 C42 H42B 109.5 . . ?
H42A C42 H42B 109.5 . . ?
C40 C42 H42C 109.5 . . ?
H42A C42 H42C 109.5 . . ?
H42B C42 H42C 109.5 . . ?
O4_1 Cl1_1 O2_1 112.8(10) . . ?
O4_1 Cl1_1 O1_1 109.3(10) . . ?
O2_1 Cl1_1 O1_1 110.0(10) . . ?
O4_1 Cl1_1 O3_1 108.4(10) . . ?
O2_1 Cl1_1 O3_1 108.4(10) . . ?
O1_1 Cl1_1 O3_1 107.9(10) . . ?
O2_2 Cl1_2 O1_2 111.4(11) . . ?
O2_2 Cl1_2 O3_2 110.9(11) . . ?
O1_2 Cl1_2 O3_2 111.0(11) . . ?
O2_2 Cl1_2 O4_2 107.8(10) . . ?
O1_2 Cl1_2 O4_2 108.6(11) . . ?
O3_2 Cl1_2 O4_2 107.0(10) . . ?
O3_3 Cl1_3 O2_3 110.8(10) . . ?
O3_3 Cl1_3 O1_3 110.1(10) . . ?
O2_3 Cl1_3 O1_3 108.1(10) . . ?
O3_3 Cl1_3 O4_3 109.3(10) . . ?
O2_3 Cl1_3 O4_3 110.2(10) . . ?
O1_3 Cl1_3 O4_3 108.3(10) . . ?
O1_4 Cl1_4 O2_4 109.7(10) . . ?
O1_4 Cl1_4 O4_4 108.4(10) . . ?
O2_4 Cl1_4 O4_4 110.6(10) . . ?
O1_4 Cl1_4 O3_4 108.6(10) . . ?
O2_4 Cl1_4 O3_4 108.5(10) . . ?
O4_4 Cl1_4 O3_4 110.9(11) . . ?

loop_
_geom_hbond_atom_site_label_D
_geom_hbond_atom_site_label_H
_geom_hbond_atom_site_label_A
_geom_hbond_distance_DH
_geom_hbond_distance_HA
_geom_hbond_distance_DA
_geom_hbond_angle_DHA
_geom_hbond_site_symmetry_A
N1 H1 O4_4 0.87 2.16 3.02(3) 169.0 .
N1 H1 O4_3 0.87 2.06 2.91(2) 165.2 .
N5 H5 O2 0.87 2.03 2.603(16) 122.9 .
N6 H6 O1_2 0.87 2.08 2.94(3) 173.1 .
N6 H6 O1_1 0.87 1.93 2.78(3) 168.3 .
N6 H6 Cl1_1 0.87 2.69 3.486(17) 152.8 .
N6 H6 Cl1_2 0.87 2.87 3.681(15) 155.0 .
N10 H10 O3 0.87 1.92 2.75(2) 159.2 4_565

_refine_diff_density_max         0.309
_refine_diff_density_min         -0.327
_refine_diff_density_rms         0.057

# start Validation Reply Form

_vrf_PLAT028_Stage2_Initial      
;
PROBLEM: _diffrn_measured_fraction_theta_max  Low .......      0.261       
RESPONSE: This is one sample in a multi-sample integration. To avoid bias
in the intensity values, any overlaps were omitted, and not included in the
raw intensity file. This has decreased the completeness. 
;

_vrf_PLAT088_Stage2_Initial      
;
PROBLEM: Poor Data / Parameter Ratio ....................       3.63 Note  
RESPONSE: As stated above, the completeness is low. Due to this, measures were
taken to avoid over-modelling the structure. Disordered anions were refined
isotropically, and SADI were used to input chemical knowledge, to assist the
refinement. 
;

_vrf_PLAT412_Stage2_Initial      
;
PROBLEM: Short Intra XH3 .. XHn     H1C    ..  H3A     ..       1.58 Ang.  
RESPONSE: An AFIX 137 was employed in this case(C1), but this probably didn't  
take into consideration the large size of the displacement elipsoid. C1 was 
recommended for splitting, but since no chemical knowledge would have been 
gained, it was not. If the data:parameter ratio had not been so low, splitting
this atom would have probably yielded better hydrogen positions.
;

_vrf_ABSMU01_Stage2_Initial      
;
PROBLEM: Calculation of _exptl_absorpt_correction_mu
                not performed for this radiation type.
RESPONSE: Absorption corrections were done with SADABS that takes
 the x-ray wavelengths from the raw data. PLATON does
 not calculate these corrections for synchrotron radiation data.
;

_vrf_PLAT984_Stage2_Initial      
;
PROBLEM: The element-f Deviates from the B&C-Value
RESPONSE: DISP values for each element type present were
 calculated for the 0.7749 angstrom x-rays using XDISP
 implemented in winGX, and using the Brennan model.
;
####################################################################### 
# 
# 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_Stage2_Transient
_database_code_depnum_ccdc_archive 'CCDC 1053054'
_audit_update_record             
;
2015-12-22 deposited with the CCDC.
2016-01-05 downloaded from the CCDC.
;

_audit_creation_method           SHELXL-2014/7
_shelx_SHELXL_version_number     2014/7
_chemical_name_systematic        ?
_chemical_name_common            ?
_chemical_melting_point          ?
_chemical_formula_moiety         '(C36 H30 Fe N10 O2),2(Cl O4)'
_chemical_formula_sum            'C36 H30 Cl2 Fe N10 O10'
_chemical_formula_weight         889.45

loop_
_atom_type_symbol
_atom_type_description
_atom_type_scat_dispersion_real
_atom_type_scat_dispersion_imag
_atom_type_scat_source
C C -0.0020 0.0020
'WCROMER Program in WinGX L.Kissel & R.H.Pratt Acta Cryst A46 170 1990'
H H 0.0000 0.0000
'WCROMER Program in WinGX L.Kissel & R.H.Pratt Acta Cryst A46 170 1990'
N N -0.0031 0.0040
'WCROMER Program in WinGX L.Kissel & R.H.Pratt Acta Cryst A46 170 1990'
O O -0.0041 0.0074
'WCROMER Program in WinGX L.Kissel & R.H.Pratt Acta Cryst A46 170 1990'
Cl Cl 0.1408 0.1896
'WCROMER Program in WinGX L.Kissel & R.H.Pratt Acta Cryst A46 170 1990'
Fe Fe 0.2064 0.9930
'WCROMER Program in WinGX L.Kissel & R.H.Pratt Acta Cryst A46 170 1990'

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

_shelx_space_group_comment       
;
The symmetry employed for this shelxl refinement is uniquely defined
by the following loop, which should always be used as a source of
symmetry information in preference to the above space-group names.
They are only intended as comments.
;

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

_cell_length_a                   15.679(12)
_cell_length_b                   20.102(15)
_cell_length_c                   24.601(18)
_cell_angle_alpha                90
_cell_angle_beta                 90.221(8)
_cell_angle_gamma                90
_cell_volume                     7754(10)
_cell_formula_units_Z            8
_cell_measurement_temperature    250(2)
_cell_measurement_reflns_used    1179
_cell_measurement_theta_min      2.78
_cell_measurement_theta_max      24.64

_exptl_crystal_description       block
_exptl_crystal_colour            orange
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    ?
_exptl_crystal_density_diffrn    1.524
_exptl_crystal_F_000             3648
_exptl_transmission_factor_min   ?
_exptl_transmission_factor_max   ?
_exptl_crystal_size_max          0.100
_exptl_crystal_size_mid          0.070
_exptl_crystal_size_min          0.050
_exptl_absorpt_coefficient_mu    0.751
_shelx_estimated_absorpt_T_min   0.929
_shelx_estimated_absorpt_T_max   0.963
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_correction_T_min  0.5205
_exptl_absorpt_correction_T_max  0.7445
_exptl_absorpt_process_details   'SADABS-2012/1  (Sheldrick, 2012)'
_exptl_absorpt_special_details   ?
_diffrn_ambient_temperature      250(2)
_diffrn_radiation_wavelength     0.7749
_diffrn_radiation_type           synchrotron
_diffrn_radiation_source         'Advanced Light Source Beamline 11.3.1'
_diffrn_radiation_monochromator  silicon(111)
_diffrn_measurement_device_type  'Bruker Apex2'
_diffrn_measurement_method       ω
_diffrn_detector_area_resol_mean 8.3
_diffrn_reflns_number            11377
_diffrn_reflns_av_unetI/netI     0.0723
_diffrn_reflns_av_R_equivalents  0.0857
_diffrn_reflns_limit_h_min       -13
_diffrn_reflns_limit_h_max       13
_diffrn_reflns_limit_k_min       -16
_diffrn_reflns_limit_k_max       16
_diffrn_reflns_limit_l_min       -20
_diffrn_reflns_limit_l_max       20
_diffrn_reflns_theta_min         2.777
_diffrn_reflns_theta_max         18.835
_diffrn_reflns_theta_full        18.835
_diffrn_measured_fraction_theta_max 0.594
_diffrn_measured_fraction_theta_full 0.594
_diffrn_reflns_Laue_measured_fraction_max 0.594
_diffrn_reflns_Laue_measured_fraction_full 0.594
_diffrn_reflns_point_group_measured_fraction_max 0.594
_diffrn_reflns_point_group_measured_fraction_full 0.594
_reflns_number_total             2792
_reflns_number_gt                1625
_reflns_threshold_expression     'I > 2σ(I)'
_reflns_Friedel_coverage         0.000
_reflns_Friedel_fraction_max     .
_reflns_Friedel_fraction_full    .

_reflns_special_details          
;
 Reflections were merged by SHELXL according to the crystal
 class for the calculation of statistics and refinement.
 
 _reflns_Friedel_fraction is defined as the number of unique
 Friedel pairs measured divided by the number that would be
 possible theoretically, ignoring centric projections and
 systematic absences.

The images contain diffraction patterens from three samples: The low spin
initial compound, the high spin final product (which is twinned) and the low
 spin/high spin mixed Transient, which is shown in this file.  The three
neccesary unit cells and four orientation matrices were determined
using CELL_NOW and RLATT, and manually combined into an orientation matrix 
file (*.p4p).To seperate the reflections, the SAINT integration
 engine was used in command line mode, and set up with a sample mask. An 
example is shown below:
SMAP=1, 1, 2
This indicates that the first two orientation matrices belong to sample 1, and 
the third belongs to sample 2.  For all commands relating to cell or symmetry 
later on, comma-delimited lists were used to specify distinct parameters.
Listed below are most of the pertinent SAINT commands in an example from the 
SAINT manual:

FILTPOINTGP=-1, 2/m  //indicating sample 1 is triclinic and 2 is monoclinic
CRYST_SYS=1,3
PAR_MASK=TPS2, TP	//restaining the  twinned cells to be similar
GPAR_MASK=TPS2, TP    //and also restraining Detector pitch and xtal trans

 explained in the SAINT manual as
"Two-sample integration, where first sample is a two-component
twin and second component is a single crystal.  In the first sample,
constrain cell constants of the second component to those of the
first.  For both samples, constrain crystal translations and
 detector pitch"


In this case, the SAINT commands used were as follows: 
SMAP=1, 2, 3, 3
CRYST_SYS=3, 3, 1
PAR_MASK=TP, TP, TPS2
GPAR_MASK=TP, TP, TPS2

This integration yielded three reflection files; two HKLF4 and one HKLF5
;

_computing_data_collection       'Apex2 v2012.10-0 (Bruker, 2012)'
_computing_cell_refinement       'SAINT V8.27B(Bruker, 2012)'
_computing_data_reduction        SAINT
_computing_structure_solution    'SHELXT (Sheldrick, 2012)'
_computing_structure_refinement  'SHELXL-2014/7 (Sheldrick, 2014)'
_computing_molecular_graphics    
;
     	SHELXTL 5.1, XP (Sheldrick, 1994)
	ShelXle Rev 699 (Hubschle, 2011)
;
_computing_publication_material  SHELXL-2014/7
_refine_special_details          
;
  This is the intermediate in a conversion from low spin to high spin. 
This conversion requires the loss of a solvent molecule (acetone in this case)
and creates a horrible sample from a nearly perfect crystal.The diffraction of
the intermediate was not useable past 1.26A. This has resulted in very few
data per parameter.

The solvent molecule that is present in the final high spin sample can not be
found in this structure. SQUEEZE was uesd to look for unmodelled electron 
density, and all that was found was 3 electrons in a void measuring 125.3 A³
This leads us to conclude that the acetone molecules are so disordered during 
this meta-stable state, that their scattering contribution is not detected in
the Bragg scattering, and these molecules may only contribute diffuse scatter.

All hydrogens  were assigned geometrically and refined
as riding, with U(H) = 1.2*U(C) for aromatic carbons, U(H) = 1.2*U(N) for 
nitrogens and U(H) = 1.5*U(C) for terminal carbons. 

The perchlorates were not modeled as split sites even though 
splitting could have been called for, due to the low data to parameter ratio.
The following similarity restraints were employed:

SADI_ClO4 0.01 Cl1 O1 Cl1 O2 Cl1 O3 Cl1 O4
SADI_ClO4 0.02 O1 O2 O1 O3 O1 O4 O2 O3 O2 O4 O3 O4

To aide in the refinement of the structure, a RIGU command was used.

The high second weighting term is probably due to the weak data which
was deconvoluted from images with three discrete patterns, and
 all overlapped reflections were discarded.
;

_diffrn_orient_matrix_UB_11      0.00511
_diffrn_orient_matrix_UB_12      -0.01474
_diffrn_orient_matrix_UB_13      0.03870
_diffrn_orient_matrix_UB_21      -0.02480
_diffrn_orient_matrix_UB_22      0.04327
_diffrn_orient_matrix_UB_23      0.01228
_diffrn_orient_matrix_UB_31      -0.05854
_diffrn_orient_matrix_UB_32      -0.01962
_diffrn_orient_matrix_UB_33      -0.00199
_diffrn_orient_matrix_type       'Sparks (1982)'

_refine_ls_structure_factor_coef Fsqd
_refine_ls_matrix_type           full
_refine_ls_weighting_scheme      calc
_refine_ls_weighting_details     
'w=1/[σ²(Fo²)+(0.0953P)²+57.0043P] where P=(Fo²+2Fc²)/3'
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_atom_sites_solution_hydrogens   geom
_refine_ls_hydrogen_treatment    constr
_refine_ls_extinction_method     none
_refine_ls_extinction_coef       .
_refine_ls_number_reflns         2792
_refine_ls_number_parameters     1063
_refine_ls_number_restraints     1482
_refine_ls_R_factor_all          0.1349
_refine_ls_R_factor_gt           0.0696
_refine_ls_wR_factor_ref         0.2093
_refine_ls_wR_factor_gt          0.1604
_refine_ls_goodness_of_fit_ref   1.090
_refine_ls_restrained_S_all      0.958
_refine_ls_shift/su_max          0.000
_refine_ls_shift/su_mean         0.000

loop_
_atom_site_label
_atom_site_type_symbol
_atom_site_fract_x
_atom_site_fract_y
_atom_site_fract_z
_atom_site_U_iso_or_equiv
_atom_site_adp_type
_atom_site_occupancy
_atom_site_site_symmetry_order
_atom_site_calc_flag
_atom_site_refinement_flags_posn
_atom_site_refinement_flags_adp
_atom_site_refinement_flags_occupancy
_atom_site_disorder_assembly
_atom_site_disorder_group
Cl1_1 Cl 1.0174(5) 0.8780(4) 0.3926(3) 0.104(3) Uani 1 1 d D U . . .
O1_1 O 1.1058(7) 0.8719(8) 0.3854(6) 0.107(6) Uani 1 1 d D U . . .
O2_1 O 0.9738(11) 0.8522(9) 0.3479(6) 0.157(8) Uani 1 1 d D U . . .
O3_1 O 0.9945(11) 0.9425(6) 0.4054(8) 0.159(8) Uani 1 1 d D U . . .
O4_1 O 0.9964(11) 0.8368(8) 0.4377(6) 0.154(7) Uani 1 1 d D U . . .
Cl1_2 Cl 0.5001(5) 0.9113(4) 0.2395(3) 0.108(3) Uani 1 1 d D U . . .
O1_2 O 0.4500(9) 0.8551(6) 0.2283(6) 0.114(6) Uani 1 1 d D U . . .
O2_2 O 0.5328(10) 0.9378(8) 0.1912(5) 0.139(7) Uani 1 1 d D U . . .
O3_2 O 0.5683(8) 0.8923(8) 0.2735(6) 0.127(7) Uani 1 1 d D U . . .
O4_2 O 0.4510(10) 0.9598(7) 0.2656(7) 0.145(7) Uani 1 1 d D U . . .
Cl1_3 Cl 0.0031(5) 0.4491(4) 0.3714(4) 0.113(3) Uani 1 1 d D U . . .
O1_3 O 0.0696(9) 0.4935(7) 0.3824(7) 0.136(7) Uani 1 1 d D U . . .
O2_3 O 0.0327(11) 0.3886(7) 0.3524(8) 0.166(8) Uani 1 1 d D U . . .
O3_3 O -0.0520(11) 0.4785(8) 0.3331(7) 0.174(8) Uani 1 1 d D U . . .
O4_3 O -0.0447(13) 0.4393(9) 0.4188(6) 0.174(9) Uani 1 1 d D U . . .
Cl1_4 Cl 0.5036(5) 0.6390(4) 0.4909(3) 0.114(3) Uani 1 1 d D U . . .
O1_4 O 0.4597(10) 0.6169(7) 0.4449(5) 0.110(6) Uani 1 1 d D U . . .
O2_4 O 0.4823(12) 0.7059(7) 0.5011(7) 0.167(8) Uani 1 1 d D U . . .
O3_4 O 0.4826(13) 0.6021(9) 0.5370(6) 0.193(9) Uani 1 1 d D U . . .
O4_4 O 0.5924(7) 0.6364(10) 0.4836(8) 0.176(8) Uani 1 1 d D U . . .
Fe01 Fe 0.2241(2) 0.6851(2) 0.34747(13) 0.0644(14) Uani 1 1 d . U . . .
Fe02 Fe 0.7300(2) 0.7345(2) 0.35494(15) 0.0672(14) Uani 1 1 d . U . . .
O1 O 0.1778(12) 0.8676(10) 0.5014(8) 0.115(7) Uani 1 1 d . U . . .
O2 O 0.3305(11) 0.7252(12) 0.1483(8) 0.105(6) Uani 1 1 d . U . . .
O101 O 0.8395(13) 0.5819(11) 0.1853(8) 0.126(7) Uani 1 1 d . U . . .
O102 O 0.6319(11) 0.7512(12) 0.5796(8) 0.112(6) Uani 1 1 d . U . . .
N1 N 0.1653(10) 0.7508(10) 0.4526(8) 0.063(5) Uani 1 1 d . U . . .
H1B H 0.1575 0.7910 0.4405 0.076 Uiso 1 1 calc R U . . .
N2 N 0.1890(12) 0.6992(11) 0.4225(8) 0.073(5) Uani 1 1 d . U . . .
N3 N 0.2508(12) 0.5986(10) 0.3784(9) 0.068(5) Uani 1 1 d . U . . .
N4 N 0.2726(12) 0.6393(11) 0.2838(8) 0.068(5) Uani 1 1 d . U . . .
N5 N 0.2921(11) 0.6542(10) 0.2323(8) 0.076(5) Uani 1 1 d . U . . .
H5A H 0.2836 0.6926 0.2169 0.091 Uiso 1 1 calc R U . . .
N6 N 0.3956(12) 0.7330(10) 0.3975(7) 0.072(6) Uani 1 1 d . U . . .
H6A H 0.4092 0.6986 0.4172 0.086 Uiso 1 1 calc R U . . .
N7 N 0.3266(11) 0.7374(10) 0.3623(7) 0.060(5) Uani 1 1 d . U . . .
N8 N 0.1954(13) 0.7666(10) 0.3087(8) 0.069(5) Uani 1 1 d . U . . .
N9 N 0.1083(12) 0.6652(11) 0.3216(8) 0.074(5) Uani 1 1 d . U . . .
N10 N 0.0549(12) 0.6145(10) 0.3247(7) 0.072(6) Uani 1 1 d . U . . .
H10C H 0.0639 0.5773 0.3418 0.087 Uiso 1 1 calc R U . . .
N101 N 0.7872(11) 0.6890(10) 0.2298(8) 0.072(5) Uani 1 1 d . U . . .
H10D H 0.7756 0.6468 0.2327 0.086 Uiso 1 1 calc R U . . .
N102 N 0.7752(10) 0.7332(11) 0.2709(8) 0.062(5) Uani 1 1 d . U . . .
N103 N 0.7630(11) 0.8336(10) 0.3346(9) 0.060(5) Uani 1 1 d . U . . .
N104 N 0.6975(12) 0.7962(12) 0.4272(8) 0.074(5) Uani 1 1 d . U . . .
N105 N 0.6654(12) 0.7897(11) 0.4780(8) 0.084(6) Uani 1 1 d . U . . .
H10E H 0.6441 0.7535 0.4916 0.101 Uiso 1 1 calc R U . . .
N106 N 0.9158(12) 0.7119(10) 0.4149(8) 0.082(6) Uani 1 1 d . U . . .
H10F H 0.9364 0.7519 0.4120 0.098 Uiso 1 1 calc R U . . .
N107 N 0.8421(12) 0.6947(11) 0.3917(8) 0.076(6) Uani 1 1 d . U . . .
N108 N 0.7045(12) 0.6316(10) 0.3682(8) 0.068(5) Uani 1 1 d . U . . .
N109 N 0.6037(12) 0.7181(11) 0.3230(8) 0.067(5) Uani 1 1 d . U . . .
N110 N 0.5502(12) 0.7507(11) 0.2907(8) 0.082(7) Uani 1 1 d . U . . .
H11A H 0.5553 0.7921 0.2811 0.099 Uiso 1 1 calc R U . . .
C1 C 0.192(2) 0.9382(15) 0.4962(12) 0.153(13) Uani 1 1 d . U . . .
H1A H 0.2196 0.9473 0.4618 0.229 Uiso 1 1 calc R U . . .
H1C H 0.1375 0.9612 0.4974 0.229 Uiso 1 1 calc R U . . .
H1D H 0.2277 0.9535 0.5258 0.229 Uiso 1 1 calc R U . . .
C2 C 0.1382(17) 0.8436(17) 0.5483(13) 0.097(8) Uani 1 1 d . U . . .
C3 C 0.1114(19) 0.8850(16) 0.5928(12) 0.121(10) Uani 1 1 d . U . . .
H3A H 0.1156 0.9316 0.5919 0.146 Uiso 1 1 calc R U . . .
C4 C 0.0803(18) 0.8521(17) 0.6351(13) 0.114(10) Uani 1 1 d . U . . .
H4A H 0.0667 0.8779 0.6658 0.137 Uiso 1 1 calc R U . . .
C5 C 0.066(2) 0.7868(17) 0.6393(13) 0.125(12) Uani 1 1 d . U . . .
H5B H 0.0406 0.7684 0.6704 0.150 Uiso 1 1 calc R U . . .
C6 C 0.0907(15) 0.7475(14) 0.5962(11) 0.085(8) Uani 1 1 d . U . . .
H6B H 0.0833 0.7012 0.5987 0.102 Uiso 1 1 calc R U . . .
C7 C 0.1266(15) 0.7745(16) 0.5487(11) 0.080(7) Uani 1 1 d . U . . .
C8 C 0.1546(14) 0.7311(16) 0.5067(11) 0.073(7) Uani 1 1 d . U . . .
C9 C 0.1744(15) 0.6662(14) 0.5073(11) 0.082(8) Uani 1 1 d . U . . .
H9A H 0.1720 0.6385 0.5380 0.098 Uiso 1 1 calc R U . . .
C10 C 0.1990(16) 0.6461(14) 0.4556(11) 0.076(7) Uani 1 1 d . U . . .
C11 C 0.2334(14) 0.5891(14) 0.4302(11) 0.070(6) Uani 1 1 d . U . . .
C12 C 0.2525(16) 0.5276(13) 0.4532(11) 0.096(9) Uani 1 1 d . U . . .
H12A H 0.2421 0.5193 0.4902 0.116 Uiso 1 1 calc R U . . .
C13 C 0.2868(18) 0.4796(14) 0.4207(12) 0.113(10) Uani 1 1 d . U . . .
H13A H 0.3008 0.4379 0.4355 0.136 Uiso 1 1 calc R U . . .
C14 C 0.3005(16) 0.4913(14) 0.3684(11) 0.100(9) Uani 1 1 d . U . . .
H14A H 0.3201 0.4567 0.3460 0.120 Uiso 1 1 calc R U . . .
C15 C 0.2863(16) 0.5534(15) 0.3466(11) 0.075(7) Uani 1 1 d . U . . .
C16 C 0.2957(15) 0.5776(14) 0.2914(11) 0.069(7) Uani 1 1 d . U . . .
C17 C 0.3306(14) 0.5501(13) 0.2441(10) 0.079(7) Uani 1 1 d . U . . .
H17A H 0.3515 0.5067 0.2391 0.094 Uiso 1 1 calc R U . . .
C18 C 0.3276(13) 0.5997(14) 0.2076(11) 0.068(6) Uani 1 1 d . U . . .
C19 C 0.3593(14) 0.6088(16) 0.1499(11) 0.080(7) Uani 1 1 d . U . . .
C20 C 0.3857(18) 0.5485(16) 0.1259(12) 0.112(9) Uani 1 1 d . U . . .
H20A H 0.3816 0.5083 0.1453 0.135 Uiso 1 1 calc R U . . .
C21 C 0.418(2) 0.5492(17) 0.0726(13) 0.130(11) Uani 1 1 d . U . . .
H21A H 0.4422 0.5113 0.0561 0.156 Uiso 1 1 calc R U . . .
C22 C 0.4128(19) 0.6105(18) 0.0460(14) 0.129(11) Uani 1 1 d . U . . .
H22A H 0.4295 0.6121 0.0094 0.155 Uiso 1 1 calc R U . . .
C23 C 0.3853(17) 0.6678(16) 0.0689(12) 0.110(9) Uani 1 1 d . U . . .
H23A H 0.3851 0.7068 0.0478 0.133 Uiso 1 1 calc R U . . .
C24 C 0.3568(17) 0.6713(18) 0.1238(14) 0.093(8) Uani 1 1 d . U . . .
C25 C 0.3372(18) 0.7858(15) 0.1218(11) 0.124(11) Uani 1 1 d . U . . .
H25A H 0.3153 0.8209 0.1449 0.187 Uiso 1 1 calc R U . . .
H25B H 0.3966 0.7946 0.1135 0.187 Uiso 1 1 calc R U . . .
H25C H 0.3044 0.7844 0.0883 0.187 Uiso 1 1 calc R U . . .
C26 C 0.4378(16) 0.7911(13) 0.3959(10) 0.071(8) Uani 1 1 d . U . . .
H26A H 0.4876 0.8000 0.4161 0.086 Uiso 1 1 calc R U . . .
C27 C 0.4001(16) 0.8358(14) 0.3617(10) 0.084(8) Uani 1 1 d . U . . .
H27A H 0.4176 0.8790 0.3523 0.101 Uiso 1 1 calc R U . . .
C28 C 0.3281(16) 0.7998(14) 0.3442(10) 0.066(7) Uani 1 1 d . U . . .
C29 C 0.2580(15) 0.8133(13) 0.3077(9) 0.060(6) Uani 1 1 d . U . . .
C30 C 0.2475(16) 0.8685(12) 0.2747(10) 0.083(8) Uani 1 1 d . U . . .
H30A H 0.2895 0.9018 0.2729 0.100 Uiso 1 1 calc R U . . .
C31 C 0.1730(17) 0.8732(14) 0.2443(11) 0.103(9) Uani 1 1 d . U . . .
H31A H 0.1659 0.9086 0.2198 0.123 Uiso 1 1 calc R U . . .
C32 C 0.1091(17) 0.8263(13) 0.2497(9) 0.080(7) Uani 1 1 d . U . . .
H32A H 0.0564 0.8327 0.2321 0.096 Uiso 1 1 calc R U . . .
C33 C 0.1229(16) 0.7700(14) 0.2808(10) 0.066(7) Uani 1 1 d . U . . .
C34 C 0.0722(17) 0.7133(14) 0.2921(10) 0.072(7) Uani 1 1 d . U . . .
C35 C -0.0078(15) 0.6913(13) 0.2743(9) 0.078(7) Uani 1 1 d . U . . .
H35A H -0.0473 0.7135 0.2519 0.094 Uiso 1 1 calc R U . . .
C36 C -0.0147(16) 0.6305(14) 0.2969(10) 0.083(8) Uani 1 1 d . U . . .
H36A H -0.0629 0.6030 0.2934 0.099 Uiso 1 1 calc R U . . .
C101 C 0.862(3) 0.5111(19) 0.1896(14) 0.26(3) Uani 1 1 d . U . . .
H10A H 0.8486 0.4952 0.2258 0.383 Uiso 1 1 calc R U . . .
H10B H 0.8292 0.4859 0.1630 0.383 Uiso 1 1 calc R U . . .
H10L H 0.9222 0.5054 0.1827 0.383 Uiso 1 1 calc R U . . .
C102 C 0.8546(17) 0.6118(17) 0.1360(13) 0.096(8) Uani 1 1 d . U . . .
C103 C 0.8813(18) 0.5800(15) 0.0883(12) 0.115(10) Uani 1 1 d . U . . .
H10G H 0.8900 0.5337 0.0889 0.138 Uiso 1 1 calc R U . . .
C104 C 0.8948(18) 0.6129(17) 0.0423(13) 0.111(10) Uani 1 1 d . U . . .
H10H H 0.9137 0.5902 0.0112 0.134 Uiso 1 1 calc R U . . .
C105 C 0.8808(17) 0.6809(17) 0.0407(12) 0.106(9) Uani 1 1 d . U . . .
H10I H 0.8886 0.7042 0.0080 0.127 Uiso 1 1 calc R U . . .
C106 C 0.8550(16) 0.7155(15) 0.0876(11) 0.101(8) Uani 1 1 d . U . . .
H10J H 0.8475 0.7619 0.0868 0.121 Uiso 1 1 calc R U . . .
C107 C 0.8405(14) 0.6797(16) 0.1357(11) 0.076(6) Uani 1 1 d . U . . .
C108 C 0.8184(13) 0.7161(14) 0.1846(10) 0.064(6) Uani 1 1 d . U . . .
C109 C 0.8270(12) 0.7835(13) 0.1949(9) 0.060(6) Uani 1 1 d . U . . .
H10K H 0.8472 0.8164 0.1711 0.072 Uiso 1 1 calc R U . . .
C110 C 0.7984(13) 0.7921(13) 0.2499(10) 0.061(6) Uani 1 1 d . U . . .
C111 C 0.7970(14) 0.8498(14) 0.2853(10) 0.057(6) Uani 1 1 d . U . . .
C112 C 0.8236(15) 0.9110(14) 0.2723(11) 0.075(7) Uani 1 1 d . U . . .
H11B H 0.8458 0.9201 0.2376 0.089 Uiso 1 1 calc R U . . .
C113 C 0.8174(14) 0.9611(13) 0.3117(10) 0.073(7) Uani 1 1 d . U . . .
H11C H 0.8359 1.0044 0.3034 0.087 Uiso 1 1 calc R U . . .
C114 C 0.7850(15) 0.9480(13) 0.3618(11) 0.074(7) Uani 1 1 d . U . . .
H11D H 0.7808 0.9812 0.3885 0.089 Uiso 1 1 calc R U . . .
C115 C 0.7584(15) 0.8828(15) 0.3718(11) 0.070(7) Uani 1 1 d . U . . .
C116 C 0.7197(15) 0.8595(15) 0.4211(11) 0.075(7) Uani 1 1 d . U . . .
C117 C 0.7050(16) 0.8948(14) 0.4701(10) 0.092(8) Uani 1 1 d . U . . .
H11E H 0.7159 0.9399 0.4774 0.111 Uiso 1 1 calc R U . . .
C118 C 0.6717(16) 0.8485(15) 0.5039(12) 0.082(7) Uani 1 1 d . U . . .
C119 C 0.6434(16) 0.8635(18) 0.5635(12) 0.099(7) Uani 1 1 d . U . . .
C120 C 0.6400(19) 0.9318(18) 0.5776(12) 0.129(11) Uani 1 1 d . U . . .
H12B H 0.6510 0.9654 0.5519 0.155 Uiso 1 1 calc R U . . .
C121 C 0.619(2) 0.9474(19) 0.6325(14) 0.153(13) Uani 1 1 d . U . . .
H12C H 0.6157 0.9917 0.6445 0.184 Uiso 1 1 calc R U . . .
C122 C 0.604(2) 0.8955(19) 0.6670(14) 0.140(12) Uani 1 1 d . U . . .
H12D H 0.5944 0.9062 0.7037 0.168 Uiso 1 1 calc R U . . .
C123 C 0.6014(16) 0.8289(17) 0.6534(12) 0.110(8) Uani 1 1 d . U . . .
H12E H 0.5863 0.7955 0.6784 0.132 Uiso 1 1 calc R U . . .
C124 C 0.6234(17) 0.815(2) 0.5986(14) 0.109(9) Uani 1 1 d . U . . .
C125 C 0.6088(19) 0.6983(16) 0.6168(12) 0.139(11) Uani 1 1 d . U . . .
H12H H 0.6173 0.6556 0.5993 0.209 Uiso 1 1 calc R U . . .
H12I H 0.6444 0.7009 0.6491 0.209 Uiso 1 1 calc R U . . .
H12J H 0.5494 0.7029 0.6270 0.209 Uiso 1 1 calc R U . . .
C126 C 0.9560(16) 0.6648(13) 0.4425(10) 0.080(8) Uani 1 1 d . U . . .
H12F H 1.0086 0.6693 0.4606 0.097 Uiso 1 1 calc R U . . .
C127 C 0.9085(15) 0.6101(13) 0.4401(9) 0.082(8) Uani 1 1 d . U . . .
H12G H 0.9198 0.5678 0.4548 0.099 Uiso 1 1 calc R U . . .
C128 C 0.8376(15) 0.6312(14) 0.4101(10) 0.071(7) Uani 1 1 d . U . . .
C129 C 0.7613(15) 0.5919(14) 0.3940(8) 0.060(6) Uani 1 1 d . U . . .
C130 C 0.7467(17) 0.5249(14) 0.4020(10) 0.092(8) Uani 1 1 d . U . . .
H13B H 0.7882 0.4969 0.4174 0.110 Uiso 1 1 calc R U . . .
C131 C 0.6669(17) 0.5009(14) 0.3858(11) 0.102(9) Uani 1 1 d . U . . .
H13C H 0.6531 0.4559 0.3915 0.123 Uiso 1 1 calc R U . . .
C132 C 0.6117(17) 0.5400(15) 0.3630(10) 0.092(8) Uani 1 1 d . U . . .
H13D H 0.5582 0.5229 0.3526 0.110 Uiso 1 1 calc R U . . .
C133 C 0.6300(16) 0.6066(15) 0.3537(9) 0.069(7) Uani 1 1 d . U . . .
C134 C 0.5751(15) 0.6539(14) 0.3244(9) 0.065(6) Uani 1 1 d . U . . .
C135 C 0.5013(16) 0.6485(14) 0.2952(10) 0.090(8) Uani 1 1 d . U . . .
H13E H 0.4677 0.6102 0.2901 0.108 Uiso 1 1 calc R U . . .
C136 C 0.4873(16) 0.7102(14) 0.2752(10) 0.083(8) Uani 1 1 d . U . . .
H13F H 0.4403 0.7226 0.2536 0.100 Uiso 1 1 calc R U . . .


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

loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
_geom_bond_publ_flag
Cl1_1 O3_1 1.383(9) . ?
Cl1_1 O2_1 1.394(9) . ?
Cl1_1 O1_1 1.403(9) . ?
Cl1_1 O4_1 1.422(9) . ?
Cl1_2 O4_2 1.400(9) . ?
Cl1_2 O2_2 1.401(9) . ?
Cl1_2 O1_2 1.404(9) . ?
Cl1_2 O3_2 1.408(9) . ?
Cl1_3 O2_3 1.383(9) . ?
Cl1_3 O1_3 1.399(9) . ?
Cl1_3 O4_3 1.402(9) . ?
Cl1_3 O3_3 1.405(9) . ?
Cl1_4 O3_4 1.394(9) . ?
Cl1_4 O1_4 1.396(9) . ?
Cl1_4 O4_4 1.405(9) . ?
Cl1_4 O2_4 1.408(9) . ?
Fe01 N3 1.943(19) . ?
Fe01 N8 1.947(19) . ?
Fe01 N2 1.95(2) . ?
Fe01 N7 1.954(19) . ?
Fe01 N9 1.96(2) . ?
Fe01 N4 1.97(2) . ?
Fe02 N103 2.12(2) . ?
Fe02 N107 2.13(2) . ?
Fe02 N108 2.13(2) . ?
Fe02 N109 2.153(19) . ?
Fe02 N102 2.19(2) . ?
Fe02 N104 2.23(2) . ?
O1 C2 1.40(3) . ?
O1 C1 1.44(3) . ?
O2 C24 1.31(3) . ?
O2 C25 1.39(3) . ?
O101 C102 1.37(3) . ?
O101 C101 1.47(3) . ?
O102 C124 1.36(3) . ?
O102 C125 1.45(3) . ?
N1 N2 1.33(2) . ?
N1 C8 1.40(3) . ?
N1 H1B 0.8700 . ?
N2 C10 1.35(3) . ?
N3 C11 1.32(3) . ?
N3 C15 1.32(3) . ?
N4 C16 1.31(2) . ?
N4 N5 1.34(2) . ?
N5 C18 1.37(3) . ?
N5 H5A 0.8700 . ?
N6 C26 1.34(2) . ?
N6 N7 1.39(2) . ?
N6 H6A 0.8700 . ?
N7 C28 1.33(2) . ?
N8 C33 1.33(3) . ?
N8 C29 1.36(3) . ?
N9 N10 1.32(2) . ?
N9 C34 1.33(3) . ?
N10 C36 1.33(2) . ?
N10 H10C 0.8700 . ?
N101 C108 1.33(3) . ?
N101 N102 1.36(2) . ?
N101 H10D 0.8700 . ?
N102 C110 1.34(2) . ?
N103 C115 1.35(3) . ?
N103 C111 1.37(3) . ?
N104 C116 1.33(3) . ?
N104 N105 1.35(2) . ?
N105 C118 1.35(3) . ?
N105 H10E 0.8700 . ?
N106 C126 1.32(2) . ?
N106 N107 1.33(2) . ?
N106 H10F 0.8700 . ?
N107 C128 1.36(3) . ?
N108 C133 1.32(3) . ?
N108 C129 1.35(3) . ?
N109 N110 1.33(2) . ?
N109 C134 1.37(2) . ?
N110 C136 1.33(3) . ?
N110 H11A 0.8700 . ?
C1 H1A 0.9700 . ?
C1 H1C 0.9700 . ?
C1 H1D 0.9700 . ?
C2 C7 1.40(3) . ?
C2 C3 1.44(4) . ?
C3 C4 1.33(3) . ?
C3 H3A 0.9400 . ?
C4 C5 1.34(3) . ?
C4 H4A 0.9400 . ?
C5 C6 1.38(3) . ?
C5 H5B 0.9400 . ?
C6 C7 1.41(3) . ?
C6 H6B 0.9400 . ?
C7 C8 1.42(3) . ?
C8 C9 1.34(3) . ?
C9 C10 1.39(3) . ?
C9 H9A 0.9400 . ?
C10 C11 1.41(3) . ?
C11 C12 1.39(3) . ?
C12 C13 1.36(3) . ?
C12 H12A 0.9400 . ?
C13 C14 1.33(3) . ?
C13 H13A 0.9400 . ?
C14 C15 1.38(3) . ?
C14 H14A 0.9400 . ?
C15 C16 1.45(3) . ?
C16 C17 1.40(3) . ?
C17 C18 1.34(3) . ?
C17 H17A 0.9400 . ?
C18 C19 1.52(3) . ?
C19 C20 1.41(3) . ?
C19 C24 1.41(4) . ?
C20 C21 1.41(4) . ?
C20 H20A 0.9400 . ?
C21 C22 1.40(3) . ?
C21 H21A 0.9400 . ?
C22 C23 1.35(3) . ?
C22 H22A 0.9400 . ?
C23 C24 1.43(4) . ?
C23 H23A 0.9400 . ?
C25 H25A 0.9700 . ?
C25 H25B 0.9700 . ?
C25 H25C 0.9700 . ?
C26 C27 1.36(3) . ?
C26 H26A 0.9400 . ?
C27 C28 1.41(3) . ?
C27 H27A 0.9400 . ?
C28 C29 1.44(3) . ?
C29 C30 1.39(3) . ?
C30 C31 1.39(3) . ?
C30 H30A 0.9400 . ?
C31 C32 1.38(3) . ?
C31 H31A 0.9400 . ?
C32 C33 1.38(3) . ?
C32 H32A 0.9400 . ?
C33 C34 1.42(3) . ?
C34 C35 1.40(3) . ?
C35 C36 1.35(3) . ?
C35 H35A 0.9400 . ?
C36 H36A 0.9400 . ?
C101 H10A 0.9700 . ?
C101 H10B 0.9700 . ?
C101 H10L 0.9700 . ?
C102 C107 1.38(3) . ?
C102 C103 1.40(3) . ?
C103 C104 1.33(3) . ?
C103 H10G 0.9400 . ?
C104 C105 1.38(3) . ?
C104 H10H 0.9400 . ?
C105 C106 1.41(3) . ?
C105 H10I 0.9400 . ?
C106 C107 1.40(3) . ?
C106 H10J 0.9400 . ?
C107 C108 1.45(3) . ?
C108 C109 1.38(3) . ?
C109 C110 1.44(3) . ?
C109 H10K 0.9400 . ?
C110 C111 1.45(3) . ?
C111 C112 1.34(3) . ?
C112 C113 1.40(3) . ?
C112 H11B 0.9400 . ?
C113 C114 1.36(3) . ?
C113 H11C 0.9400 . ?
C114 C115 1.40(3) . ?
C114 H11D 0.9400 . ?
C115 C116 1.44(3) . ?
C116 C117 1.42(3) . ?
C117 C118 1.35(3) . ?
C117 H11E 0.9400 . ?
C118 C119 1.56(4) . ?
C119 C124 1.35(4) . ?
C119 C120 1.42(3) . ?
C120 C121 1.43(4) . ?
C120 H12B 0.9400 . ?
C121 C122 1.37(4) . ?
C121 H12C 0.9400 . ?
C122 C123 1.38(4) . ?
C122 H12D 0.9400 . ?
C123 C124 1.42(4) . ?
C123 H12E 0.9400 . ?
C125 H12H 0.9700 . ?
C125 H12I 0.9700 . ?
C125 H12J 0.9700 . ?
C126 C127 1.33(3) . ?
C126 H12F 0.9400 . ?
C127 C128 1.40(3) . ?
C127 H12G 0.9400 . ?
C128 C129 1.49(3) . ?
C129 C130 1.38(3) . ?
C130 C131 1.40(3) . ?
C130 H13B 0.9400 . ?
C131 C132 1.30(3) . ?
C131 H13C 0.9400 . ?
C132 C133 1.39(3) . ?
C132 H13D 0.9400 . ?
C133 C134 1.47(3) . ?
C134 C135 1.36(3) . ?
C135 C136 1.35(3) . ?
C135 H13E 0.9400 . ?
C136 H13F 0.9400 . ?

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
O3_1 Cl1_1 O2_1 113.7(10) . . ?
O3_1 Cl1_1 O1_1 111.6(9) . . ?
O2_1 Cl1_1 O1_1 110.4(9) . . ?
O3_1 Cl1_1 O4_1 108.0(10) . . ?
O2_1 Cl1_1 O4_1 106.5(10) . . ?
O1_1 Cl1_1 O4_1 106.2(9) . . ?
O4_2 Cl1_2 O2_2 109.2(10) . . ?
O4_2 Cl1_2 O1_2 110.0(10) . . ?
O2_2 Cl1_2 O1_2 110.3(9) . . ?
O4_2 Cl1_2 O3_2 109.5(10) . . ?
O2_2 Cl1_2 O3_2 109.2(9) . . ?
O1_2 Cl1_2 O3_2 108.7(9) . . ?
O2_3 Cl1_3 O1_3 112.0(10) . . ?
O2_3 Cl1_3 O4_3 109.7(10) . . ?
O1_3 Cl1_3 O4_3 109.2(10) . . ?
O2_3 Cl1_3 O3_3 110.5(10) . . ?
O1_3 Cl1_3 O3_3 108.5(10) . . ?
O4_3 Cl1_3 O3_3 106.7(10) . . ?
O3_4 Cl1_4 O1_4 111.9(10) . . ?
O3_4 Cl1_4 O4_4 108.8(10) . . ?
O1_4 Cl1_4 O4_4 111.7(9) . . ?
O3_4 Cl1_4 O2_4 107.9(10) . . ?
O1_4 Cl1_4 O2_4 109.3(9) . . ?
O4_4 Cl1_4 O2_4 107.1(10) . . ?
N3 Fe01 N8 173.6(9) . . ?
N3 Fe01 N2 79.7(9) . . ?
N8 Fe01 N2 106.0(9) . . ?
N3 Fe01 N7 103.4(8) . . ?
N8 Fe01 N7 80.0(9) . . ?
N2 Fe01 N7 88.9(8) . . ?
N3 Fe01 N9 98.2(8) . . ?
N8 Fe01 N9 78.5(9) . . ?
N2 Fe01 N9 94.2(8) . . ?
N7 Fe01 N9 158.3(9) . . ?
N3 Fe01 N4 79.1(9) . . ?
N8 Fe01 N4 95.3(9) . . ?
N2 Fe01 N4 158.7(9) . . ?
N7 Fe01 N4 94.5(8) . . ?
N9 Fe01 N4 90.4(8) . . ?
N103 Fe02 N107 104.6(8) . . ?
N103 Fe02 N108 173.9(8) . . ?
N107 Fe02 N108 74.1(8) . . ?
N103 Fe02 N109 106.5(8) . . ?
N107 Fe02 N109 148.6(9) . . ?
N108 Fe02 N109 74.6(8) . . ?
N103 Fe02 N102 73.0(8) . . ?
N107 Fe02 N102 97.3(7) . . ?
N108 Fe02 N102 101.2(8) . . ?
N109 Fe02 N102 87.4(7) . . ?
N103 Fe02 N104 73.9(9) . . ?
N107 Fe02 N104 93.5(8) . . ?
N108 Fe02 N104 112.0(8) . . ?
N109 Fe02 N104 99.5(7) . . ?
N102 Fe02 N104 146.8(8) . . ?
C2 O1 C1 119(3) . . ?
C24 O2 C25 119(3) . . ?
C102 O101 C101 116(3) . . ?
C124 O102 C125 116(3) . . ?
N2 N1 C8 110(2) . . ?
N2 N1 H1B 124.9 . . ?
C8 N1 H1B 124.9 . . ?
N1 N2 C10 108(2) . . ?
N1 N2 Fe01 136.3(18) . . ?
C10 N2 Fe01 115(2) . . ?
C11 N3 C15 124(3) . . ?
C11 N3 Fe01 118(2) . . ?
C15 N3 Fe01 118(2) . . ?
C16 N4 N5 107(2) . . ?
C16 N4 Fe01 115.9(19) . . ?
N5 N4 Fe01 137.5(18) . . ?
N4 N5 C18 110(2) . . ?
N4 N5 H5A 125.2 . . ?
C18 N5 H5A 125.2 . . ?
C26 N6 N7 108(2) . . ?
C26 N6 H6A 126.0 . . ?
N7 N6 H6A 126.0 . . ?
C28 N7 N6 105(2) . . ?
C28 N7 Fe01 117.4(17) . . ?
N6 N7 Fe01 136.1(16) . . ?
C33 N8 C29 125(2) . . ?
C33 N8 Fe01 119.5(19) . . ?
C29 N8 Fe01 115.1(18) . . ?
N10 N9 C34 109(2) . . ?
N10 N9 Fe01 136.3(17) . . ?
C34 N9 Fe01 114.8(19) . . ?
N9 N10 C36 108(2) . . ?
N9 N10 H10C 126.2 . . ?
C36 N10 H10C 126.2 . . ?
C108 N101 N102 114(2) . . ?
C108 N101 H10D 123.1 . . ?
N102 N101 H10D 123.1 . . ?
C110 N102 N101 105(2) . . ?
C110 N102 Fe02 116.2(18) . . ?
N101 N102 Fe02 139.2(17) . . ?
C115 N103 C111 117(2) . . ?
C115 N103 Fe02 121(2) . . ?
C111 N103 Fe02 122.0(19) . . ?
C116 N104 N105 107(2) . . ?
C116 N104 Fe02 112.5(19) . . ?
N105 N104 Fe02 140.3(19) . . ?
C118 N105 N104 109(2) . . ?
C118 N105 H10E 125.5 . . ?
N104 N105 H10E 125.5 . . ?
C126 N106 N107 116(2) . . ?
C126 N106 H10F 121.8 . . ?
N107 N106 H10F 121.8 . . ?
N106 N107 C128 98(2) . . ?
N106 N107 Fe02 142.9(18) . . ?
C128 N107 Fe02 116.8(17) . . ?
C133 N108 C129 119(2) . . ?
C133 N108 Fe02 119.6(19) . . ?
C129 N108 Fe02 121.3(17) . . ?
N110 N109 C134 106(2) . . ?
N110 N109 Fe02 136.2(18) . . ?
C134 N109 Fe02 115.9(17) . . ?
N109 N110 C136 110(2) . . ?
N109 N110 H11A 125.2 . . ?
C136 N110 H11A 125.2 . . ?
O1 C1 H1A 109.5 . . ?
O1 C1 H1C 109.5 . . ?
H1A C1 H1C 109.5 . . ?
O1 C1 H1D 109.5 . . ?
H1A C1 H1D 109.5 . . ?
H1C C1 H1D 109.5 . . ?
O1 C2 C7 114(3) . . ?
O1 C2 C3 124(3) . . ?
C7 C2 C3 122(3) . . ?
C4 C3 C2 115(3) . . ?
C4 C3 H3A 122.6 . . ?
C2 C3 H3A 122.6 . . ?
C3 C4 C5 128(4) . . ?
C3 C4 H4A 116.1 . . ?
C5 C4 H4A 116.1 . . ?
C4 C5 C6 117(3) . . ?
C4 C5 H5B 121.4 . . ?
C6 C5 H5B 121.4 . . ?
C5 C6 C7 122(3) . . ?
C5 C6 H6B 119.0 . . ?
C7 C6 H6B 119.0 . . ?
C2 C7 C6 116(3) . . ?
C2 C7 C8 124(3) . . ?
C6 C7 C8 119(3) . . ?
C9 C8 N1 105(3) . . ?
C9 C8 C7 131(3) . . ?
N1 C8 C7 124(3) . . ?
C8 C9 C10 110(3) . . ?
C8 C9 H9A 125.1 . . ?
C10 C9 H9A 125.1 . . ?
N2 C10 C9 107(3) . . ?
N2 C10 C11 115(3) . . ?
C9 C10 C11 138(3) . . ?
N3 C11 C12 119(3) . . ?
N3 C11 C10 113(3) . . ?
C12 C11 C10 128(3) . . ?
C13 C12 C11 118(3) . . ?
C13 C12 H12A 120.9 . . ?
C11 C12 H12A 120.9 . . ?
C14 C13 C12 121(3) . . ?
C14 C13 H13A 119.7 . . ?
C12 C13 H13A 119.7 . . ?
C13 C14 C15 121(3) . . ?
C13 C14 H14A 119.6 . . ?
C15 C14 H14A 119.6 . . ?
N3 C15 C14 117(3) . . ?
N3 C15 C16 112(3) . . ?
C14 C15 C16 131(3) . . ?
N4 C16 C17 111(3) . . ?
N4 C16 C15 115(3) . . ?
C17 C16 C15 133(3) . . ?
C18 C17 C16 104(3) . . ?
C18 C17 H17A 127.8 . . ?
C16 C17 H17A 127.8 . . ?
C17 C18 N5 108(3) . . ?
C17 C18 C19 135(3) . . ?
N5 C18 C19 117(3) . . ?
C20 C19 C24 126(3) . . ?
C20 C19 C18 113(3) . . ?
C24 C19 C18 122(3) . . ?
C19 C20 C21 119(3) . . ?
C19 C20 H20A 120.3 . . ?
C21 C20 H20A 120.3 . . ?
C22 C21 C20 115(3) . . ?
C22 C21 H21A 122.6 . . ?
C20 C21 H21A 122.6 . . ?
C23 C22 C21 125(4) . . ?
C23 C22 H22A 117.4 . . ?
C21 C22 H22A 117.4 . . ?
C22 C23 C24 123(3) . . ?
C22 C23 H23A 118.7 . . ?
C24 C23 H23A 118.7 . . ?
O2 C24 C19 122(4) . . ?
O2 C24 C23 125(3) . . ?
C19 C24 C23 112(3) . . ?
O2 C25 H25A 109.5 . . ?
O2 C25 H25B 109.5 . . ?
H25A C25 H25B 109.5 . . ?
O2 C25 H25C 109.5 . . ?
H25A C25 H25C 109.5 . . ?
H25B C25 H25C 109.5 . . ?
N6 C26 C27 112(3) . . ?
N6 C26 H26A 123.9 . . ?
C27 C26 H26A 123.9 . . ?
C26 C27 C28 101(3) . . ?
C26 C27 H27A 129.4 . . ?
C28 C27 H27A 129.4 . . ?
N7 C28 C27 113(2) . . ?
N7 C28 C29 112(2) . . ?
C27 C28 C29 135(3) . . ?
N8 C29 C30 119(2) . . ?
N8 C29 C28 114(2) . . ?
C30 C29 C28 127(3) . . ?
C31 C30 C29 118(3) . . ?
C31 C30 H30A 121.1 . . ?
C29 C30 H30A 121.1 . . ?
C32 C31 C30 121(3) . . ?
C32 C31 H31A 119.6 . . ?
C30 C31 H31A 119.6 . . ?
C31 C32 C33 120(3) . . ?
C31 C32 H32A 120.0 . . ?
C33 C32 H32A 120.0 . . ?
N8 C33 C32 117(3) . . ?
N8 C33 C34 110(3) . . ?
C32 C33 C34 133(3) . . ?
N9 C34 C35 109(3) . . ?
N9 C34 C33 117(3) . . ?
C35 C34 C33 134(3) . . ?
C36 C35 C34 103(2) . . ?
C36 C35 H35A 128.3 . . ?
C34 C35 H35A 128.3 . . ?
N10 C36 C35 111(3) . . ?
N10 C36 H36A 124.3 . . ?
C35 C36 H36A 124.3 . . ?
O101 C101 H10A 109.5 . . ?
O101 C101 H10B 109.5 . . ?
H10A C101 H10B 109.5 . . ?
O101 C101 H10L 109.5 . . ?
H10A C101 H10L 109.5 . . ?
H10B C101 H10L 109.5 . . ?
O101 C102 C107 114(3) . . ?
O101 C102 C103 126(3) . . ?
C107 C102 C103 120(3) . . ?
C104 C103 C102 122(3) . . ?
C104 C103 H10G 118.8 . . ?
C102 C103 H10G 118.8 . . ?
C103 C104 C105 119(3) . . ?
C103 C104 H10H 120.3 . . ?
C105 C104 H10H 120.3 . . ?
C104 C105 C106 121(3) . . ?
C104 C105 H10I 119.6 . . ?
C106 C105 H10I 119.6 . . ?
C107 C106 C105 119(3) . . ?
C107 C106 H10J 120.5 . . ?
C105 C106 H10J 120.5 . . ?
C102 C107 C106 119(3) . . ?
C102 C107 C108 122(3) . . ?
C106 C107 C108 119(3) . . ?
N101 C108 C109 107(2) . . ?
N101 C108 C107 125(3) . . ?
C109 C108 C107 128(3) . . ?
C108 C109 C110 105(2) . . ?
C108 C109 H10K 127.5 . . ?
C110 C109 H10K 127.5 . . ?
N102 C110 C109 110(2) . . ?
N102 C110 C111 118(3) . . ?
C109 C110 C111 132(3) . . ?
C112 C111 N103 124(3) . . ?
C112 C111 C110 126(3) . . ?
N103 C111 C110 110(3) . . ?
C111 C112 C113 118(3) . . ?
C111 C112 H11B 120.9 . . ?
C113 C112 H11B 120.9 . . ?
C114 C113 C112 121(3) . . ?
C114 C113 H11C 119.5 . . ?
C112 C113 H11C 119.5 . . ?
C113 C114 C115 117(3) . . ?
C113 C114 H11D 121.5 . . ?
C115 C114 H11D 121.5 . . ?
N103 C115 C114 123(3) . . ?
N103 C115 C116 111(3) . . ?
C114 C115 C116 126(3) . . ?
N104 C116 C117 110(3) . . ?
N104 C116 C115 121(3) . . ?
C117 C116 C115 129(3) . . ?
C118 C117 C116 104(3) . . ?
C118 C117 H11E 128.0 . . ?
C116 C117 H11E 128.0 . . ?
N105 C118 C117 110(3) . . ?
N105 C118 C119 126(3) . . ?
C117 C118 C119 124(3) . . ?
C124 C119 C120 123(3) . . ?
C124 C119 C118 122(3) . . ?
C120 C119 C118 115(3) . . ?
C119 C120 C121 117(3) . . ?
C119 C120 H12B 121.5 . . ?
C121 C120 H12B 121.5 . . ?
C122 C121 C120 118(4) . . ?
C122 C121 H12C 121.2 . . ?
C120 C121 H12C 121.2 . . ?
C121 C122 C123 126(4) . . ?
C121 C122 H12D 116.8 . . ?
C123 C122 H12D 116.8 . . ?
C122 C123 C124 115(4) . . ?
C122 C123 H12E 122.6 . . ?
C124 C123 H12E 122.6 . . ?
C119 C124 O102 116(3) . . ?
C119 C124 C123 121(4) . . ?
O102 C124 C123 122(4) . . ?
O102 C125 H12H 109.5 . . ?
O102 C125 H12I 109.5 . . ?
H12H C125 H12I 109.5 . . ?
O102 C125 H12J 109.5 . . ?
H12H C125 H12J 109.5 . . ?
H12I C125 H12J 109.5 . . ?
N106 C126 C127 108(3) . . ?
N106 C126 H12F 126.2 . . ?
C127 C126 H12F 126.2 . . ?
C126 C127 C128 102(3) . . ?
C126 C127 H12G 128.8 . . ?
C128 C127 H12G 128.8 . . ?
N107 C128 C127 115(2) . . ?
N107 C128 C129 117(2) . . ?
C127 C128 C129 128(3) . . ?
N108 C129 C130 122(2) . . ?
N108 C129 C128 110(3) . . ?
C130 C129 C128 128(3) . . ?
C129 C130 C131 116(3) . . ?
C129 C130 H13B 121.8 . . ?
C131 C130 H13B 121.8 . . ?
C132 C131 C130 121(3) . . ?
C132 C131 H13C 119.7 . . ?
C130 C131 H13C 119.7 . . ?
C131 C132 C133 121(3) . . ?
C131 C132 H13D 119.4 . . ?
C133 C132 H13D 119.4 . . ?
N108 C133 C132 120(3) . . ?
N108 C133 C134 114(3) . . ?
C132 C133 C134 126(3) . . ?
C135 C134 N109 110(3) . . ?
C135 C134 C133 134(3) . . ?
N109 C134 C133 116(2) . . ?
C136 C135 C134 105(3) . . ?
C136 C135 H13E 127.6 . . ?
C134 C135 H13E 127.6 . . ?
N110 C136 C135 110(3) . . ?
N110 C136 H13F 125.2 . . ?
C135 C136 H13F 125.2 . . ?

_refine_diff_density_max         0.290
_refine_diff_density_min         -0.208
_refine_diff_density_rms         0.050


# start Validation Reply Form

_vrf_REFNR01_Stage2_Transient    
;
PROBLEM: Ratio of reflections to parameters is < 6 for a
RESPONSE: This data set contained diffraction from three samples: an initial
compound, this Transient and a final, twinned compound. All overlapped 
reflections were omitted at the integration stage. The diffraction data for
the Transient were cut at 1.26\%A, due to poor statistics, leaving a
poor data to parameter ratio.
;

_vrf_THETM01_Stage2_Transient    
;
PROBLEM: The value of sine(theta_max)/wavelength is less than 0.550
RESPONSE: Mean I/\s dropped below 2.0 at 1.23\%A, but R(merge) went 
above 30% at 1.31\%A, so the compromise was to cut the data at 1.26\%A.
;

_vrf_PLAT023_Stage2_Transient    
;
PROBLEM: Resolution (too) Low [sin(theta)/Lambda < 0.6]..      18.83 Degree
RESPONSE: As stated above, the data quality declined precipitously into noise
with increasing resolution.
;

_vrf_PLAT029_Stage2_Transient    
;
PROBLEM: _diffrn_measured_fraction_theta_full Low .......      0.594 Note  
RESPONSE: See above comments.
;

_vrf_PLAT088_Stage2_Transient    
;
PROBLEM: Poor Data / Parameter Ratio ....................       2.63 Note  
RESPONSE: See above comments.
;

_vrf_ABSMU01_Stage2_Transient    
;
PROBLEM: Calculation of _exptl_absorpt_correction_mu
                not performed for this radiation type.
RESPONSE: Absorption corrections were done with SADABS that takes
 the x-ray wavelengths from the raw data. PLATON does
 not calculate these corrections for synchrotron radiation data.
;

_vrf_PLAT984_Stage2_Transient    
;
PROBLEM: The element-f Deviates from the B&C-Value
RESPONSE: DISP values for each element type present were
 calculated for the 0.7749 angstrom x-rays using XDISP
 implemented in winGX, and using the Brennan model.
;
####################################################################### 
# 
# 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_Stage2_Final
_database_code_depnum_ccdc_archive 'CCDC 1053055'
_audit_update_record             
;
2015-12-22 deposited with the CCDC.
2016-01-05 downloaded from the CCDC.
;

_audit_creation_method           SHELXL-2014/7
_shelx_SHELXL_version_number     2014/7
_chemical_name_systematic        ?
_chemical_name_common            ?
_chemical_melting_point          ?
_chemical_formula_moiety         
;
C36 H30 Fe N10 O2, C3 H6 O, 2(Cl O4) 
;
_chemical_formula_sum            'C39 H36 Cl2 Fe N10 O11'
_chemical_formula_weight         947.53

loop_
_atom_type_symbol
_atom_type_description
_atom_type_scat_dispersion_real
_atom_type_scat_dispersion_imag
_atom_type_scat_source
C C -0.0020 0.0020
'WCROMER Program in WinGX L.Kissel & R.H.Pratt Acta Cryst A46 170 1990'
H H 0.0000 0.0000
'WCROMER Program in WinGX L.Kissel & R.H.Pratt Acta Cryst A46 170 1990'
N N -0.0031 0.0040
'WCROMER Program in WinGX L.Kissel & R.H.Pratt Acta Cryst A46 170 1990'
O O -0.0041 0.0074
'WCROMER Program in WinGX L.Kissel & R.H.Pratt Acta Cryst A46 170 1990'
Cl Cl 0.1408 0.1896
'WCROMER Program in WinGX L.Kissel & R.H.Pratt Acta Cryst A46 170 1990'
Fe Fe 0.2064 0.9930
'WCROMER Program in WinGX L.Kissel & R.H.Pratt Acta Cryst A46 170 1990'

_space_group_crystal_system      triclinic
_space_group_IT_number           2
_space_group_name_H-M_alt        'P -1'
_space_group_name_Hall           '-P 1'

_shelx_space_group_comment       
;
The symmetry employed for this shelxl refinement is uniquely defined
by the following loop, which should always be used as a source of
symmetry information in preference to the above space-group names.
They are only intended as comments.
;

loop_
_space_group_symop_operation_xyz
'x, y, z'
'-x, -y, -z'

_cell_length_a                   13.073(3)
_cell_length_b                   13.356(3)
_cell_length_c                   14.075(3)
_cell_angle_alpha                71.88(3)
_cell_angle_beta                 69.89(3)
_cell_angle_gamma                70.65(3)
_cell_volume                     2123.0(10)
_cell_formula_units_Z            2
_cell_measurement_temperature    250(2)
_cell_measurement_reflns_used    1378
_cell_measurement_theta_min      3.27
_cell_measurement_theta_max      22.7

_exptl_crystal_description       block
_exptl_crystal_colour            orange
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    ?
_exptl_crystal_density_diffrn    1.482
_exptl_crystal_F_000             976
_exptl_transmission_factor_min   ?
_exptl_transmission_factor_max   ?
_exptl_crystal_size_max          0.100
_exptl_crystal_size_mid          0.070
_exptl_crystal_size_min          0.050
_exptl_absorpt_coefficient_mu    0.694
_shelx_estimated_absorpt_T_min   0.934
_shelx_estimated_absorpt_T_max   0.966
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_correction_T_min  0.524839
_exptl_absorpt_correction_T_max  0.745584
_exptl_absorpt_process_details   'TWINABS 2012/1  (Sheldrick, 2012)'
_exptl_absorpt_special_details   ?
_diffrn_ambient_temperature      250(2)
_diffrn_radiation_wavelength     0.7749
_diffrn_radiation_type           synchrotron
_diffrn_radiation_source         'Advanced Light Source Beamline 11.3.1'
_diffrn_radiation_monochromator  silicon(111)
_diffrn_measurement_device_type  'Bruker Apex2'
_diffrn_measurement_method       ω
_diffrn_detector_area_resol_mean 8.3
_diffrn_reflns_number            2413
_diffrn_reflns_av_unetI/netI     0.0595
_diffrn_reflns_av_R_equivalents  ?
_diffrn_reflns_limit_h_min       -14
_diffrn_reflns_limit_h_max       15
_diffrn_reflns_limit_k_min       -14
_diffrn_reflns_limit_k_max       16
_diffrn_reflns_limit_l_min       0
_diffrn_reflns_limit_l_max       15
_diffrn_reflns_theta_min         3.273
_diffrn_reflns_theta_max         27.719
_diffrn_reflns_theta_full        27.706
_diffrn_measured_fraction_theta_max 0.346
_diffrn_measured_fraction_theta_full 0.346
_diffrn_reflns_Laue_measured_fraction_max 0.346
_diffrn_reflns_Laue_measured_fraction_full 0.346
_diffrn_reflns_point_group_measured_fraction_max 0.346
_diffrn_reflns_point_group_measured_fraction_full 0.346
_reflns_number_total             2413
_reflns_number_gt                1516
_reflns_threshold_expression     'I > 2σ(I)'
_reflns_Friedel_coverage         0.000
_reflns_Friedel_fraction_max     .
_reflns_Friedel_fraction_full    .

_reflns_special_details          
;
 _reflns_Friedel_fraction is defined as the number of unique
 Friedel pairs measured divided by the number that would be
 possible theoretically, ignoring centric projections and
 systematic absences.

The images contain diffraction patterens from three samples:The low spin 
initial compound, the low spin/high spin mixed Transient and the high spin final
product (which is twinned) which is shown in this file.  The three
neccesary unit cells and four orientation matrices were determined
using CELL_NOW and RLATT, and manually combined into an orientation matrix 
file (*.p4p).To seperate the reflections, the SAINT integration
 engine was used in command line mode, and set up with a sample mask. An 
example is shown below:
SMAP=1, 1, 2
This indicates that the first two orientation matrices belong to sample 1, and 
the third belongs to sample 2.  For all commands relating to cell or symmetry 
later on, comma-delimited lists were used to specify distinct parameters.
Listed below are most of the pertinent SAINT commands in an example from the 
SAINT manual:

FILTPOINTGP=-1, 2/m  //indicating sample 1 is triclinic and 2 is monoclinic
CRYST_SYS=1,3
PAR_MASK=TPS2, TP	//restaining the  twinned cells to be similar
GPAR_MASK=TPS2, TP    //and also restraining Detector pitch and xtal trans

 explained in the SAINT manual as
"Two-sample integration, where first sample is a two-component
twin and second component is a single crystal.  In the first sample,
constrain cell constants of the second component to those of the
first.  For both samples, constrain crystal translations and
 detector pitch"


In this case, the SAINT commands used were as follows: 
SMAP=1, 2, 3, 3
CRYST_SYS=3, 3, 1
PAR_MASK=TP, TP, TPS2
GPAR_MASK=TP, TP, TPS2

This integration yielded three reflection files; two HKLF4 and one HKLF5
;

_computing_data_collection       'Apex2 v2012.10-0 (Bruker, 2012)'
_computing_cell_refinement       'SAINT V8.27B(Bruker, 2012)'
_computing_data_reduction        SAINT
_computing_structure_solution    'SHELXT (Sheldrick, 2012)'
_computing_structure_refinement  'SHELXL-2014/7 (Sheldrick, 2014)'
_computing_molecular_graphics    
;
     	SHELXTL 5.1, XP (Sheldrick, 1994)
	ShelXle Rev 699 (Hubschle, 2011)
;
_computing_publication_material  SHELXL-2014/7
_refine_special_details          
;
 Refined as a 2-component twin.
All hydrogens were assigned geometrically and refined as riding, with 
U(H) = 1.2*U(C) for secondary and aromatic carbons, and 
U(H) = 1.5*U(C) for terminal carbons. The hydrogens on N1, N5 N6 and N10 
were found in the difference map first, then affixed geometrically, with 
U(H) = 1.2*U(N)


This stucture contains two disordered perchlorate anions.The disordered 
perchlorates were modeled as split sites, using the 
following restraints:

SADI_ClO4 0.01 Cl1 O1 Cl1 O2 Cl1 O3 Cl1 O4
SADI_ClO4 0.02 O1 O2 O1 O3 O1 O4 O2 O3 O2 O4 O3 O4
EADP O3_4 O3_2
EADP Cl1_1 Cl1_3

The orientation matrices for the two domains are listed below, due
to the cif format not being able to take dupicate entries:

Domain 1:
ORT13	-0.06170	0.05424	 	0.03660
ORT23	-0.05501	-0.04209	0.01026
ORT33	0.01581		-0.04372	0.06765

Domain 2:
ORT14	0.08289		-0.03334	-0.01972
ORT24	-0.00744	-0.01956	-0.05995
ORT34	0.01250		0.07163		-0.04515



;
_refine_ls_structure_factor_coef Fsqd
_refine_ls_matrix_type           full
_refine_ls_weighting_scheme      calc
_refine_ls_weighting_details     
'w=1/[σ²(Fo²)+(0.1561P)²+0.0246P] where P=(Fo²+2Fc²)/3'
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_atom_sites_solution_hydrogens   geom
_refine_ls_hydrogen_treatment    constr
_refine_ls_extinction_method     none
_refine_ls_extinction_coef       .
_refine_ls_number_reflns         2413
_refine_ls_number_parameters     561
_refine_ls_number_restraints     897
_refine_ls_R_factor_all          0.1147
_refine_ls_R_factor_gt           0.0685
_refine_ls_wR_factor_ref         0.2212
_refine_ls_wR_factor_gt          0.1821
_refine_ls_goodness_of_fit_ref   1.045
_refine_ls_restrained_S_all      0.923
_refine_ls_shift/su_max          0.000
_refine_ls_shift/su_mean         0.000

loop_
_atom_site_label
_atom_site_type_symbol
_atom_site_fract_x
_atom_site_fract_y
_atom_site_fract_z
_atom_site_U_iso_or_equiv
_atom_site_adp_type
_atom_site_occupancy
_atom_site_site_symmetry_order
_atom_site_calc_flag
_atom_site_refinement_flags_posn
_atom_site_refinement_flags_adp
_atom_site_refinement_flags_occupancy
_atom_site_disorder_assembly
_atom_site_disorder_group
Fe1 Fe 0.49810(13) 0.75244(11) 0.24953(15) 0.0421(6) Uani 1 1 d . U . . .
O1 O 0.1327(10) 0.9156(11) 0.7021(11) 0.103(4) Uani 1 1 d . U . . .
O2 O 0.8359(7) 0.6400(8) -0.1022(8) 0.072(3) Uani 1 1 d . U . . .
N1 N 0.2506(8) 0.8082(7) 0.4256(9) 0.054(3) Uani 1 1 d . U . . .
H1D H 0.2094 0.7879 0.4016 0.065 Uiso 1 1 calc R U . . .
N2 N 0.3623(8) 0.8040(7) 0.3805(9) 0.047(2) Uani 1 1 d . U . . .
N3 N 0.5714(7) 0.8079(6) 0.3287(8) 0.042(2) Uani 1 1 d . U . . .
N4 N 0.6762(7) 0.7378(7) 0.1598(9) 0.048(2) Uani 1 1 d . U . . .
N5 N 0.7499(8) 0.6979(7) 0.0743(9) 0.046(2) Uani 1 1 d . U . . .
H5B H 0.7320 0.6754 0.0319 0.055 Uiso 1 1 calc R U . . .
N6 N 0.3981(9) 0.9878(8) 0.1130(10) 0.063(3) Uani 1 1 d . U . . .
H6B H 0.4212 1.0272 0.1362 0.076 Uiso 1 1 calc R U . . .
N7 N 0.4223(9) 0.8797(7) 0.1393(10) 0.054(3) Uani 1 1 d . U . . .
N8 N 0.4415(7) 0.6755(7) 0.1723(9) 0.047(2) Uani 1 1 d . U . . .
N9 N 0.5410(8) 0.5795(7) 0.3182(10) 0.049(2) Uani 1 1 d . U . . .
N10 N 0.5971(8) 0.5137(7) 0.3865(9) 0.059(3) Uani 1 1 d . U . . .
H10A H 0.6240 0.5358 0.4228 0.071 Uiso 1 1 calc R U . . .
C1 C 0.1035(18) 0.9331(14) 0.8042(16) 0.107(6) Uani 1 1 d . U . . .
H1A H 0.1550 0.8793 0.8420 0.161 Uiso 1 1 calc R U . . .
H1B H 0.0273 0.9266 0.8402 0.161 Uiso 1 1 calc R U . . .
H1C H 0.1084 1.0054 0.7998 0.161 Uiso 1 1 calc R U . . .
C2 C -0.0605(14) 0.9149(14) 0.7212(16) 0.098(5) Uani 1 1 d . U . . .
H2A H -0.0856 0.9370 0.7844 0.118 Uiso 1 1 calc R U . . .
C3 C 0.0533(13) 0.8979(11) 0.6674(14) 0.078(4) Uani 1 1 d . U . . .
C4 C -0.1352(15) 0.8997(14) 0.6829(17) 0.102(5) Uani 1 1 d . U . . .
H4A H -0.2116 0.9115 0.7201 0.123 Uiso 1 1 calc R U . . .
C5 C -0.1005(12) 0.8665(12) 0.5887(15) 0.089(4) Uani 1 1 d . U . . .
H5A H -0.1515 0.8554 0.5618 0.106 Uiso 1 1 calc R U . . .
C6 C 0.0147(12) 0.8509(13) 0.5373(15) 0.085(4) Uani 1 1 d . U . . .
H6A H 0.0406 0.8297 0.4736 0.102 Uiso 1 1 calc R U . . .
C7 C 0.0912(11) 0.8649(10) 0.5751(13) 0.069(3) Uani 1 1 d . U . . .
C8 C 0.2114(10) 0.8490(9) 0.5146(12) 0.057(3) Uani 1 1 d . U . . .
C9 C 0.2997(10) 0.8679(9) 0.5282(12) 0.057(3) Uani 1 1 d . U . . .
H9A H 0.2998 0.8943 0.5828 0.068 Uiso 1 1 calc R U . . .
C10 C 0.3941(10) 0.8400(8) 0.4425(11) 0.046(2) Uani 1 1 d . U . . .
C11 C 0.5103(9) 0.8411(7) 0.4167(10) 0.042(2) Uani 1 1 d . U . . .
C12 C 0.5575(10) 0.8729(9) 0.4700(11) 0.057(3) Uani 1 1 d . U . . .
H12A H 0.5120 0.8962 0.5312 0.068 Uiso 1 1 calc R U . . .
C13 C 0.6708(10) 0.8727(10) 0.4384(12) 0.061(3) Uani 1 1 d . U . . .
H13A H 0.7033 0.8926 0.4776 0.073 Uiso 1 1 calc R U . . .
C14 C 0.7330(10) 0.8415(9) 0.3457(11) 0.058(3) Uani 1 1 d . U . . .
H14A H 0.8088 0.8439 0.3170 0.070 Uiso 1 1 calc R U . . .
C15 C 0.6797(9) 0.8067(8) 0.2964(10) 0.044(2) Uani 1 1 d . U . . .
C16 C 0.7385(10) 0.7635(8) 0.1993(11) 0.044(2) Uani 1 1 d . U . . .
C17 C 0.8525(10) 0.7443(9) 0.1408(11) 0.053(3) Uani 1 1 d . U . . .
H17A H 0.9125 0.7595 0.1514 0.064 Uiso 1 1 calc R U . . .
C18 C 0.8552(9) 0.7003(10) 0.0682(11) 0.051(3) Uani 1 1 d . U . . .
C19 C 0.9529(10) 0.6638(10) -0.0210(12) 0.058(3) Uani 1 1 d . U . . .
C20 C 1.0587(10) 0.6552(11) -0.0148(12) 0.066(4) Uani 1 1 d . U . . .
H20A H 1.0664 0.6735 0.0412 0.079 Uiso 1 1 calc R U . . .
C21 C 1.1551(13) 0.6192(15) -0.0918(15) 0.091(5) Uani 1 1 d . U . . .
H21A H 1.2271 0.6160 -0.0893 0.109 Uiso 1 1 calc R U . . .
C22 C 1.1416(13) 0.5888(14) -0.1706(15) 0.089(5) Uani 1 1 d . U . . .
H22A H 1.2056 0.5645 -0.2223 0.106 Uiso 1 1 calc R U . . .
C23 C 1.0353(13) 0.5932(14) -0.1761(15) 0.086(4) Uani 1 1 d . U . . .
H23A H 1.0268 0.5710 -0.2295 0.104 Uiso 1 1 calc R U . . .
C24 C 0.9432(11) 0.6316(11) -0.0997(13) 0.063(3) Uani 1 1 d . U . . .
C25 C 0.8215(14) 0.6164(14) -0.1859(15) 0.088(5) Uani 1 1 d . U . . .
H25A H 0.7421 0.6378 -0.1827 0.132 Uiso 1 1 calc R U . . .
H25B H 0.8504 0.5389 -0.1830 0.132 Uiso 1 1 calc R U . . .
H25C H 0.8620 0.6562 -0.2503 0.132 Uiso 1 1 calc R U . . .
C26 C 0.3351(13) 1.0283(11) 0.0477(14) 0.078(4) Uani 1 1 d . U . . .
H26A H 0.3071 1.1024 0.0202 0.094 Uiso 1 1 calc R U . . .
C27 C 0.3185(14) 0.9440(11) 0.0277(14) 0.084(5) Uani 1 1 d . U . . .
H27A H 0.2776 0.9467 -0.0169 0.101 Uiso 1 1 calc R U . . .
C28 C 0.3743(11) 0.8520(10) 0.0868(12) 0.056(3) Uani 1 1 d . U . . .
C29 C 0.3862(11) 0.7366(10) 0.1004(13) 0.060(3) Uani 1 1 d . U . . .
C30 C 0.3477(11) 0.6858(12) 0.0539(13) 0.069(4) Uani 1 1 d . U . . .
H30A H 0.3068 0.7277 0.0052 0.083 Uiso 1 1 calc R U . . .
C31 C 0.3673(13) 0.5782(12) 0.0765(15) 0.078(4) Uani 1 1 d . U . . .
H31A H 0.3418 0.5450 0.0421 0.094 Uiso 1 1 calc R U . . .
C32 C 0.4234(11) 0.5152(10) 0.1483(14) 0.071(4) Uani 1 1 d . U . . .
H32A H 0.4369 0.4389 0.1644 0.085 Uiso 1 1 calc R U . . .
C33 C 0.4593(10) 0.5657(9) 0.1960(12) 0.052(3) Uani 1 1 d . U . . .
C34 C 0.5179(10) 0.5151(9) 0.2757(12) 0.049(3) Uani 1 1 d . U . . .
C35 C 0.5586(11) 0.4041(9) 0.3254(12) 0.066(4) Uani 1 1 d . U . . .
H35A H 0.5527 0.3409 0.3139 0.079 Uiso 1 1 calc R U . . .
C36 C 0.6067(12) 0.4113(10) 0.3920(13) 0.068(4) Uani 1 1 d . U . . .
H36A H 0.6422 0.3517 0.4364 0.082 Uiso 1 1 calc R U . . .
Cl1_1 Cl 0.4827(10) 1.1569(8) 0.2306(10) 0.0696(14) Uiso 0.50(3) 1 d D . P A 1
O1_1 O 0.5717(19) 1.190(2) 0.234(3) 0.20(2) Uiso 0.50(3) 1 d D . P A 1
O2_1 O 0.445(2) 1.2210(18) 0.1447(18) 0.107(10) Uiso 0.50(3) 1 d D . P A 1
O3_1 O 0.394(2) 1.167(3) 0.3191(18) 0.22(2) Uiso 0.50(3) 1 d D . P A 1
O4_1 O 0.521(2) 1.0498(10) 0.2213(19) 0.082(8) Uiso 0.50(3) 1 d D . P A 1
Cl1_2 Cl 0.0913(9) 0.7395(11) 0.2640(11) 0.066(3) Uiso 0.45(3) 1 d D . P B 1
O1_2 O 0.1830(14) 0.740(2) 0.292(2) 0.098(9) Uiso 0.45(3) 1 d D . P B 1
O2_2 O 0.096(2) 0.7960(19) 0.1628(16) 0.113(11) Uiso 0.45(3) 1 d D . P B 1
O3_2 O 0.092(2) 0.6327(13) 0.272(3) 0.144(5) Uiso 0.45(3) 1 d D . P B 1
O4_2 O -0.0070(14) 0.785(2) 0.3312(19) 0.095(10) Uiso 0.45(3) 1 d D . P B 1
Cl1_4 Cl 0.0866(8) 0.7146(10) 0.2893(11) 0.066(3) Uiso 0.55(3) 1 d D . P B 2
O1_4 O 0.1813(12) 0.6878(19) 0.3251(18) 0.091(7) Uiso 0.55(3) 1 d D . P B 2
O2_4 O 0.081(2) 0.8138(13) 0.219(2) 0.169(14) Uiso 0.55(3) 1 d D . P B 2
O3_4 O 0.095(2) 0.6359(15) 0.2397(19) 0.144(5) Uiso 0.55(3) 1 d D . P B 2
O4_4 O -0.0083(12) 0.721(2) 0.3724(15) 0.105(9) Uiso 0.55(3) 1 d D . P B 2
Cl1_3 Cl 0.4638(10) 1.1695(8) 0.2145(9) 0.0696(14) Uiso 0.50(3) 1 d D . P A 2
O1_3 O 0.451(3) 1.0648(13) 0.265(2) 0.129(12) Uiso 0.50(3) 1 d D . P A 2
O2_3 O 0.429(3) 1.201(2) 0.1248(16) 0.138(14) Uiso 0.50(3) 1 d D . P A 2
O3_3 O 0.5778(12) 1.165(2) 0.189(3) 0.24(3) Uiso 0.50(3) 1 d D . P A 2
O4_3 O 0.4023(17) 1.2387(17) 0.2806(17) 0.094(9) Uiso 0.50(3) 1 d D . P A 2
C39 C 0.8083(13) 0.6071(13) 0.5680(16) 0.092(6) Uani 1 1 d . U . . .
H39A H 0.8878 0.5751 0.5624 0.139 Uiso 1 1 calc R U . . .
H39B H 0.7949 0.6855 0.5442 0.139 Uiso 1 1 calc R U . . .
H39C H 0.7655 0.5892 0.6398 0.139 Uiso 1 1 calc R U . . .
C37 C 0.8683(12) 0.4973(17) 0.4344(18) 0.116(8) Uani 1 1 d . U . . .
H37A H 0.9382 0.4842 0.4513 0.174 Uiso 1 1 calc R U . . .
H37B H 0.8522 0.4283 0.4441 0.174 Uiso 1 1 calc R U . . .
H37C H 0.8751 0.5363 0.3626 0.174 Uiso 1 1 calc R U . . .
C38 C 0.7733(12) 0.5646(12) 0.5047(13) 0.064(4) Uani 1 1 d . U . . .
O3 O 0.6803(8) 0.5901(9) 0.4974(9) 0.084(4) Uani 1 1 d . U . . .


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

loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
_geom_bond_publ_flag
Fe1 N3 2.104(10) . ?
Fe1 N8 2.130(11) . ?
Fe1 N7 2.140(10) . ?
Fe1 N9 2.170(9) . ?
Fe1 N2 2.181(10) . ?
Fe1 N4 2.210(10) . ?
O1 C3 1.40(2) . ?
O1 C1 1.43(2) . ?
O2 C24 1.381(18) . ?
O2 C25 1.39(2) . ?
N1 N2 1.367(15) . ?
N1 C8 1.389(18) . ?
N1 H1D 0.8700 . ?
N2 C10 1.344(16) . ?
N3 C15 1.326(15) . ?
N3 C11 1.341(15) . ?
N4 C16 1.308(17) . ?
N4 N5 1.386(14) . ?
N5 C18 1.360(17) . ?
N5 H5B 0.8700 . ?
N6 C26 1.31(2) . ?
N6 N7 1.329(14) . ?
N6 H6B 0.8700 . ?
N7 C28 1.311(19) . ?
N8 C29 1.346(17) . ?
N8 C33 1.356(15) . ?
N9 N10 1.329(15) . ?
N9 C34 1.343(18) . ?
N10 C36 1.312(18) . ?
N10 H10A 0.8700 . ?
C1 H1A 0.9700 . ?
C1 H1B 0.9700 . ?
C1 H1C 0.9700 . ?
C2 C4 1.36(3) . ?
C2 C3 1.40(2) . ?
C2 H2A 0.9400 . ?
C3 C7 1.38(2) . ?
C4 C5 1.41(3) . ?
C4 H4A 0.9400 . ?
C5 C6 1.40(2) . ?
C5 H5A 0.9400 . ?
C6 C7 1.37(2) . ?
C6 H6A 0.9400 . ?
C7 C8 1.487(19) . ?
C8 C9 1.35(2) . ?
C9 C10 1.438(19) . ?
C9 H9A 0.9400 . ?
C10 C11 1.439(17) . ?
C11 C12 1.346(17) . ?
C12 C13 1.392(19) . ?
C12 H12A 0.9400 . ?
C13 C14 1.386(19) . ?
C13 H13A 0.9400 . ?
C14 C15 1.389(18) . ?
C14 H14A 0.9400 . ?
C15 C16 1.505(18) . ?
C16 C17 1.414(18) . ?
C17 C18 1.314(19) . ?
C17 H17A 0.9400 . ?
C18 C19 1.520(19) . ?
C19 C24 1.36(2) . ?
C19 C20 1.38(2) . ?
C20 C21 1.41(2) . ?
C20 H20A 0.9400 . ?
C21 C22 1.37(3) . ?
C21 H21A 0.9400 . ?
C22 C23 1.40(3) . ?
C22 H22A 0.9400 . ?
C23 C24 1.38(2) . ?
C23 H23A 0.9400 . ?
C25 H25A 0.9700 . ?
C25 H25B 0.9700 . ?
C25 H25C 0.9700 . ?
C26 C27 1.34(3) . ?
C26 H26A 0.9400 . ?
C27 C28 1.386(19) . ?
C27 H27A 0.9400 . ?
C28 C29 1.45(2) . ?
C29 C30 1.37(2) . ?
C30 C31 1.33(2) . ?
C30 H30A 0.9400 . ?
C31 C32 1.36(2) . ?
C31 H31A 0.9400 . ?
C32 C33 1.36(2) . ?
C32 H32A 0.9400 . ?
C33 C34 1.441(19) . ?
C34 C35 1.435(17) . ?
C35 C36 1.34(2) . ?
C35 H35A 0.9400 . ?
C36 H36A 0.9400 . ?
Cl1_1 O4_1 1.382(8) . ?
Cl1_1 O3_1 1.385(9) . ?
Cl1_1 O1_1 1.388(9) . ?
Cl1_1 O2_1 1.390(9) . ?
Cl1_2 O2_2 1.381(9) . ?
Cl1_2 O4_2 1.385(9) . ?
Cl1_2 O1_2 1.387(9) . ?
Cl1_2 O3_2 1.393(9) . ?
Cl1_4 O4_4 1.381(9) . ?
Cl1_4 O2_4 1.385(9) . ?
Cl1_4 O3_4 1.389(9) . ?
Cl1_4 O1_4 1.392(8) . ?
Cl1_3 O4_3 1.377(9) . ?
Cl1_3 O2_3 1.383(9) . ?
Cl1_3 O3_3 1.393(9) . ?
Cl1_3 O1_3 1.393(9) . ?
C39 C38 1.45(2) . ?
C39 H39A 0.9700 . ?
C39 H39B 0.9700 . ?
C39 H39C 0.9700 . ?
C37 C38 1.52(2) . ?
C37 H37A 0.9700 . ?
C37 H37B 0.9700 . ?
C37 H37C 0.9700 . ?
C38 O3 1.180(16) . ?

loop_
_geom_angle_atom_site_label_1
_geom_angle_atom_site_label_2
_geom_angle_atom_site_label_3
_geom_angle
_geom_angle_site_symmetry_1
_geom_angle_site_symmetry_3
_geom_angle_publ_flag
N3 Fe1 N8 172.0(3) . . ?
N3 Fe1 N7 113.3(4) . . ?
N8 Fe1 N7 73.7(4) . . ?
N3 Fe1 N9 99.3(4) . . ?
N8 Fe1 N9 73.6(4) . . ?
N7 Fe1 N9 147.3(4) . . ?
N3 Fe1 N2 74.4(4) . . ?
N8 Fe1 N2 110.0(4) . . ?
N7 Fe1 N2 92.4(4) . . ?
N9 Fe1 N2 98.1(4) . . ?
N3 Fe1 N4 73.7(4) . . ?
N8 Fe1 N4 101.9(4) . . ?
N7 Fe1 N4 98.4(4) . . ?
N9 Fe1 N4 88.8(4) . . ?
N2 Fe1 N4 148.0(4) . . ?
C3 O1 C1 120.1(16) . . ?
C24 O2 C25 119.3(12) . . ?
N2 N1 C8 111.3(12) . . ?
N2 N1 H1D 124.4 . . ?
C8 N1 H1D 124.4 . . ?
C10 N2 N1 105.5(11) . . ?
C10 N2 Fe1 114.3(8) . . ?
N1 N2 Fe1 140.1(9) . . ?
C15 N3 C11 117.8(11) . . ?
C15 N3 Fe1 121.6(8) . . ?
C11 N3 Fe1 120.5(8) . . ?
C16 N4 N5 105.2(10) . . ?
C16 N4 Fe1 115.9(9) . . ?
N5 N4 Fe1 138.6(8) . . ?
C18 N5 N4 108.1(11) . . ?
C18 N5 H5B 125.9 . . ?
N4 N5 H5B 125.9 . . ?
C26 N6 N7 112.2(14) . . ?
C26 N6 H6B 123.9 . . ?
N7 N6 H6B 123.9 . . ?
C28 N7 N6 105.0(10) . . ?
C28 N7 Fe1 117.2(8) . . ?
N6 N7 Fe1 137.4(10) . . ?
C29 N8 C33 119.8(12) . . ?
C29 N8 Fe1 119.6(8) . . ?
C33 N8 Fe1 120.6(8) . . ?
N10 N9 C34 106.5(9) . . ?
N10 N9 Fe1 137.3(9) . . ?
C34 N9 Fe1 115.8(8) . . ?
C36 N10 N9 111.2(13) . . ?
C36 N10 H10A 124.4 . . ?
N9 N10 H10A 124.4 . . ?
O1 C1 H1A 109.5 . . ?
O1 C1 H1B 109.5 . . ?
H1A C1 H1B 109.5 . . ?
O1 C1 H1C 109.5 . . ?
H1A C1 H1C 109.5 . . ?
H1B C1 H1C 109.5 . . ?
C4 C2 C3 120.5(19) . . ?
C4 C2 H2A 119.8 . . ?
C3 C2 H2A 119.8 . . ?
C7 C3 C2 120.3(18) . . ?
C7 C3 O1 117.2(15) . . ?
C2 C3 O1 122.5(16) . . ?
C2 C4 C5 121.3(17) . . ?
C2 C4 H4A 119.3 . . ?
C5 C4 H4A 119.3 . . ?
C6 C5 C4 116.1(18) . . ?
C6 C5 H5A 122.0 . . ?
C4 C5 H5A 122.0 . . ?
C7 C6 C5 123.3(17) . . ?
C7 C6 H6A 118.3 . . ?
C5 C6 H6A 118.3 . . ?
C6 C7 C3 118.5(15) . . ?
C6 C7 C8 119.9(15) . . ?
C3 C7 C8 121.5(16) . . ?
C9 C8 N1 107.0(12) . . ?
C9 C8 C7 131.8(15) . . ?
N1 C8 C7 121.2(13) . . ?
C8 C9 C10 106.4(14) . . ?
C8 C9 H9A 126.8 . . ?
C10 C9 H9A 126.8 . . ?
N2 C10 C9 109.9(12) . . ?
N2 C10 C11 118.4(11) . . ?
C9 C10 C11 131.7(13) . . ?
N3 C11 C12 120.9(12) . . ?
N3 C11 C10 112.4(11) . . ?
C12 C11 C10 126.7(12) . . ?
C11 C12 C13 122.8(13) . . ?
C11 C12 H12A 118.6 . . ?
C13 C12 H12A 118.6 . . ?
C14 C13 C12 116.1(14) . . ?
C14 C13 H13A 121.9 . . ?
C12 C13 H13A 121.9 . . ?
C13 C14 C15 117.9(14) . . ?
C13 C14 H14A 121.0 . . ?
C15 C14 H14A 121.0 . . ?
N3 C15 C14 124.3(12) . . ?
N3 C15 C16 112.0(11) . . ?
C14 C15 C16 123.8(12) . . ?
N4 C16 C17 111.9(12) . . ?
N4 C16 C15 116.6(12) . . ?
C17 C16 C15 131.4(12) . . ?
C18 C17 C16 104.1(12) . . ?
C18 C17 H17A 128.0 . . ?
C16 C17 H17A 128.0 . . ?
C17 C18 N5 110.5(11) . . ?
C17 C18 C19 129.9(13) . . ?
N5 C18 C19 119.3(12) . . ?
C24 C19 C20 119.2(12) . . ?
C24 C19 C18 124.7(12) . . ?
C20 C19 C18 115.9(14) . . ?
C19 C20 C21 120.5(16) . . ?
C19 C20 H20A 119.7 . . ?
C21 C20 H20A 119.7 . . ?
C22 C21 C20 118.5(16) . . ?
C22 C21 H21A 120.8 . . ?
C20 C21 H21A 120.8 . . ?
C21 C22 C23 121.8(15) . . ?
C21 C22 H22A 119.1 . . ?
C23 C22 H22A 119.1 . . ?
C24 C23 C22 117.3(18) . . ?
C24 C23 H23A 121.4 . . ?
C22 C23 H23A 121.4 . . ?
C19 C24 O2 117.4(12) . . ?
C19 C24 C23 122.7(15) . . ?
O2 C24 C23 120.0(16) . . ?
O2 C25 H25A 109.5 . . ?
O2 C25 H25B 109.5 . . ?
H25A C25 H25B 109.5 . . ?
O2 C25 H25C 109.5 . . ?
H25A C25 H25C 109.5 . . ?
H25B C25 H25C 109.5 . . ?
N6 C26 C27 107.1(12) . . ?
N6 C26 H26A 126.4 . . ?
C27 C26 H26A 126.4 . . ?
C26 C27 C28 105.3(16) . . ?
C26 C27 H27A 127.4 . . ?
C28 C27 H27A 127.4 . . ?
N7 C28 C27 110.3(13) . . ?
N7 C28 C29 117.6(11) . . ?
C27 C28 C29 132.1(16) . . ?
N8 C29 C30 118.6(12) . . ?
N8 C29 C28 111.7(14) . . ?
C30 C29 C28 129.6(13) . . ?
C31 C30 C29 120.9(13) . . ?
C31 C30 H30A 119.5 . . ?
C29 C30 H30A 119.5 . . ?
C30 C31 C32 121.2(18) . . ?
C30 C31 H31A 119.4 . . ?
C32 C31 H31A 119.4 . . ?
C33 C32 C31 117.8(13) . . ?
C33 C32 H32A 121.1 . . ?
C31 C32 H32A 121.1 . . ?
C32 C33 N8 121.5(12) . . ?
C32 C33 C34 127.0(11) . . ?
N8 C33 C34 111.5(12) . . ?
N9 C34 C35 108.1(12) . . ?
N9 C34 C33 118.3(10) . . ?
C35 C34 C33 133.5(13) . . ?
C36 C35 C34 104.2(12) . . ?
C36 C35 H35A 127.9 . . ?
C34 C35 H35A 127.9 . . ?
N10 C36 C35 110.0(12) . . ?
N10 C36 H36A 125.0 . . ?
C35 C36 H36A 125.0 . . ?
O4_1 Cl1_1 O3_1 110.3(10) . . ?
O4_1 Cl1_1 O1_1 108.3(10) . . ?
O3_1 Cl1_1 O1_1 111.3(10) . . ?
O4_1 Cl1_1 O2_1 108.9(9) . . ?
O3_1 Cl1_1 O2_1 108.6(10) . . ?
O1_1 Cl1_1 O2_1 109.5(10) . . ?
O2_2 Cl1_2 O4_2 110.6(9) . . ?
O2_2 Cl1_2 O1_2 110.5(10) . . ?
O4_2 Cl1_2 O1_2 109.3(9) . . ?
O2_2 Cl1_2 O3_2 108.5(10) . . ?
O4_2 Cl1_2 O3_2 108.0(10) . . ?
O1_2 Cl1_2 O3_2 109.8(10) . . ?
O4_4 Cl1_4 O2_4 110.1(9) . . ?
O4_4 Cl1_4 O3_4 110.2(10) . . ?
O2_4 Cl1_4 O3_4 108.5(10) . . ?
O4_4 Cl1_4 O1_4 109.1(9) . . ?
O2_4 Cl1_4 O1_4 109.4(10) . . ?
O3_4 Cl1_4 O1_4 109.5(9) . . ?
O4_3 Cl1_3 O2_3 111.7(10) . . ?
O4_3 Cl1_3 O3_3 110.1(10) . . ?
O2_3 Cl1_3 O3_3 109.5(10) . . ?
O4_3 Cl1_3 O1_3 109.2(9) . . ?
O2_3 Cl1_3 O1_3 108.8(10) . . ?
O3_3 Cl1_3 O1_3 107.4(10) . . ?
C38 C39 H39A 109.5 . . ?
C38 C39 H39B 109.5 . . ?
H39A C39 H39B 109.5 . . ?
C38 C39 H39C 109.5 . . ?
H39A C39 H39C 109.5 . . ?
H39B C39 H39C 109.5 . . ?
C38 C37 H37A 109.5 . . ?
C38 C37 H37B 109.5 . . ?
H37A C37 H37B 109.5 . . ?
C38 C37 H37C 109.5 . . ?
H37A C37 H37C 109.5 . . ?
H37B C37 H37C 109.5 . . ?
O3 C38 C39 123.5(14) . . ?
O3 C38 C37 120.9(16) . . ?
C39 C38 C37 115.0(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
N1 H1D O1_2 0.87 2.01 2.81(2) 152.4 .
N1 H1D O1_4 0.87 2.14 2.94(2) 153.8 .
N5 H5B O2 0.87 2.00 2.595(15) 124.6 .
N6 H6B Cl1_1 0.87 2.92 3.783(19) 175.0 .
N6 H6B O2_1 0.87 2.75 3.55(3) 153.4 .
N6 H6B O4_1 0.87 2.19 2.99(2) 153.4 .
N6 H6B Cl1_3 0.87 2.75 3.613(19) 172.0 .
N6 H6B O1_3 0.87 2.20 2.99(3) 150.7 .
N6 H6B O2_3 0.87 2.32 3.07(3) 145.5 .
N10 H10A O3 0.87 1.88 2.749(18) 177.3 .
C25 H25A O2_1 0.97 2.55 3.40(3) 146.6 2_675
C25 H25A O2_3 0.97 2.63 3.39(3) 134.8 2_675
C25 H25A O4_3 0.97 2.55 3.38(2) 143.4 2_675
C26 H26A N4 0.94 2.75 3.554(17) 143.4 2_675
C26 H26A N5 0.94 2.57 3.503(15) 173.1 2_675

_refine_diff_density_max         0.301
_refine_diff_density_min         -0.308
_refine_diff_density_rms         0.057


# start Validation Reply Form

_vrf_PLAT029_Stage2_Final        
;
PROBLEM: _diffrn_measured_fraction_theta_full Low .......      0.346 Note  
RESPONSE: This data set contained diffraction from three samples: an initial
compound, the intermediate and this final, twinned compound. All overlapped 
reflections were omitted at the integration stage, leaving the completeness 
lower than optimal.
;
_vrf_PLAT088_Stage2_Final        
;
PROBLEM: Poor Data / Parameter Ratio ....................       4.30 Note  
RESPONSE: Due to the deletion of overlapped reflections,
the number of data is low. Measures have been taken to not over-refine the
structure, i.e., not attempting to refine split disordered groups 
anisotropically, etc. 
;

_vrf_ABSMU01_Stage2_Final        
;
PROBLEM: Calculation of _exptl_absorpt_correction_mu
                not performed for this radiation type.
RESPONSE: Absorption corrections were done with SADABS that takes
 the x-ray wavelengths from the raw data. PLATON does
 not calculate these corrections for synchrotron radiation data.
;

_vrf_PLAT984_Stage2_Final        
;
PROBLEM: The element-f Deviates from the B&C-Value
RESPONSE: DISP values for each element type present were
 calculated for the 0.7749 angstrom x-rays using XDISP
 implemented in winGX, and using the Brennan model.
;

# end Validation Reply Form


####################################################################### 
# 
# 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_Stage3_Transient
_database_code_depnum_ccdc_archive 'CCDC 1053056'
_audit_update_record             
;
2015-12-22 deposited with the CCDC.
2016-01-05 downloaded from the CCDC.
;

_audit_creation_method           SHELXL-2014/7
_shelx_SHELXL_version_number     2014/7
_chemical_name_systematic        ?
_chemical_name_common            ?
_chemical_melting_point          ?
_chemical_formula_moiety         '(C36 H30 N10 Fe)2, (Cl O4)4'
_chemical_formula_sum            'C72 H60 Cl4 Fe2 N20 O20'
_chemical_formula_weight         1778.90

loop_
_atom_type_symbol
_atom_type_description
_atom_type_scat_dispersion_real
_atom_type_scat_dispersion_imag
_atom_type_scat_source
C C -0.0020 0.0020
'WCROMER Program in WinGX L.Kissel & R.H.Pratt Acta Cryst A46 170 1990'
H H 0.0000 0.0000
'WCROMER Program in WinGX L.Kissel & R.H.Pratt Acta Cryst A46 170 1990'
N N -0.0031 0.0040
'WCROMER Program in WinGX L.Kissel & R.H.Pratt Acta Cryst A46 170 1990'
O O -0.0041 0.0074
'WCROMER Program in WinGX L.Kissel & R.H.Pratt Acta Cryst A46 170 1990'
Cl Cl 0.1408 0.1896
'WCROMER Program in WinGX L.Kissel & R.H.Pratt Acta Cryst A46 170 1990'
Fe Fe 0.2064 0.9930
'WCROMER Program in WinGX L.Kissel & R.H.Pratt Acta Cryst A46 170 1990'

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

_shelx_space_group_comment       
;
The symmetry employed for this shelxl refinement is uniquely defined
by the following loop, which should always be used as a source of
symmetry information in preference to the above space-group names.
They are only intended as comments.
;

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

_cell_length_a                   15.700(3)
_cell_length_b                   20.035(4)
_cell_length_c                   24.638(5)
_cell_angle_alpha                90
_cell_angle_beta                 90.45(3)
_cell_angle_gamma                90
_cell_volume                     7750(3)
_cell_formula_units_Z            4
_cell_measurement_temperature    250(2)
_cell_measurement_reflns_used    4552
_cell_measurement_theta_min      2.30
_cell_measurement_theta_max      20.6

_exptl_crystal_description       block
_exptl_crystal_colour            orange
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    ?
_exptl_crystal_density_diffrn    1.525
_exptl_crystal_F_000             3648
_exptl_transmission_factor_min   ?
_exptl_transmission_factor_max   ?
_exptl_crystal_size_max          0.500
_exptl_crystal_size_mid          0.400
_exptl_crystal_size_min          0.300
_exptl_absorpt_coefficient_mu    0.752
_shelx_estimated_absorpt_T_min   0.705
_shelx_estimated_absorpt_T_max   0.806
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_correction_T_min  0.5205
_exptl_absorpt_correction_T_max  0.7443
_exptl_absorpt_process_details   'SADABS-2012/1  (Sheldrick, 2012)'
_exptl_absorpt_special_details   ?
_diffrn_ambient_temperature      250(2)
_diffrn_radiation_wavelength     0.7749
_diffrn_radiation_type           synchrotron
_diffrn_radiation_source         'Advanced Light Source Beamline 11.3.1'
_diffrn_radiation_monochromator  silicon(111)
_diffrn_measurement_device_type  'Bruker Apex2'
_diffrn_measurement_method       ω
_diffrn_detector_area_resol_mean 8.3
_diffrn_reflns_number            14414
_diffrn_reflns_av_unetI/netI     0.0475
_diffrn_reflns_av_R_equivalents  0.0566
_diffrn_reflns_limit_h_min       -12
_diffrn_reflns_limit_h_max       12
_diffrn_reflns_limit_k_min       -15
_diffrn_reflns_limit_k_max       15
_diffrn_reflns_limit_l_min       -19
_diffrn_reflns_limit_l_max       19
_diffrn_reflns_theta_min         2.015
_diffrn_reflns_theta_max         17.908
_diffrn_reflns_theta_full        17.908
_diffrn_measured_fraction_theta_max 0.694
_diffrn_measured_fraction_theta_full 0.694
_diffrn_reflns_Laue_measured_fraction_max 0.694
_diffrn_reflns_Laue_measured_fraction_full 0.694
_diffrn_reflns_point_group_measured_fraction_max 0.694
_diffrn_reflns_point_group_measured_fraction_full 0.694
_reflns_number_total             2811
_reflns_number_gt                1770
_reflns_threshold_expression     'I > 2σ(I)'
_reflns_Friedel_coverage         0.000
_reflns_Friedel_fraction_max     .
_reflns_Friedel_fraction_full    .

_reflns_special_details          
;
 Reflections were merged by SHELXL according to the crystal
 class for the calculation of statistics and refinement.
 
 _reflns_Friedel_fraction is defined as the number of unique
 Friedel pairs measured divided by the number that would be
 possible theoretically, ignoring centric projections and
 systematic absences.

 The images contain diffraction patterens from two samples: the high spin final
product (which is twinned) and the low spin/high spin mixed Transient, 
which is shown in this file.  The three neccesary unit cells were determined
using CELL_NOW and RLATT, and manually combined into an orientation matrix 
file (*.p4p).To seperate the reflections, the SAINT integration
 engine was used in command line mode, and set up with a sample mask, which is 
shown below:
SMAP=1, 1, 2
This indicates that the first two orientation matrices belong to sample 1, and 
the third belongs to sample 2.  For all commands relating to cell or symmetry 
later on, comma-delimited lists were used to specify distinct parameters.
Listed below are most of the pertinent SAINT commands:

FILTPOINTGP=-1, 2/m  //indicating sample 1 is triclinic and 2 is monoclinic
CRYST_SYS=1,3
PAR_MASK=TPS2, TP	//restaining the  twinned cells to be similar
GPAR_MASK=TPS2, TP    //and also restraining Detector pitch and xtal trans

 explained in the SAINT manual as
"Two-sample integration, where first sample is a two-component
twin and second component is a single crystal.  In the first sample,
constrain cell constants of the second component to those of the
first.  For both samples, constrain crystal translations and
 detector pitch"
;

_computing_data_collection       'Apex2 v2012.10-0 (Bruker, 2012)'
_computing_cell_refinement       'SAINT V8.27B(Bruker, 2012)'
_computing_data_reduction        SAINT
_computing_structure_solution    SHELXS
_computing_structure_refinement  'SHELXL-2014/7 (Sheldrick, 2014)'
_computing_molecular_graphics    
;
     	SHELXTL 5.1, XP (Sheldrick, 1994)
	ShelXle Rev 699 (Hubschle, 2011)
;
_computing_publication_material  SHELXL-2014/7

_refine_special_details          
;
 This is the intermediate in a conversion from low spin to high spin. 
This conversion requires the loss of a solvent molecule (acetone in this case)
and creates a horrible sample from a nearly perfect crystal.The diffraction of
the intermediate was not useable past 1.26A. This has resulted in very few
data per parameter.

The solvent molecule that is present in the final high spin sample can not be
found in this structure. SQUEEZE was uesd to look for unmodelled electron 
density, and all that was found was 3 electrons in a void measuring 125.3 A³
This leads us to conclude that the acetone molecules are so disordered during 
this meta-stable state, that their scattering contribution is not detected in
the Bragg scattering, and these molecules may only contribute diffuse scatter.

All hydrogens  were assigned geometrically and refined
as riding, with U(H) = 1.2*U(C) for aromatic carbons, U(H) = 1.2*U(N) for 
nitrogens and U(H) = 1.5*U(C) for terminal carbons. 

The disordered perchlorates were modeled as split sites, using the 
following restraints:

SADI_ClO4 0.01 Cl1 O1 Cl1 O2 Cl1 O3 Cl1 O4
SADI_ClO4 0.02 O1 O2 O1 O3 O1 O4 O2 O3 O2 O4 O3 O4

A RIGU command was employed. 

The high weighting term is probably due to the weak data and
the fact that it was deconvoluted from images with three discrete patterns.
;
_refine_ls_structure_factor_coef Fsqd
_refine_ls_matrix_type           full
_refine_ls_weighting_scheme      calc
_refine_ls_weighting_details     
'w=1/[σ²(Fo²)+(0.0945P)²+85.7635P] where P=(Fo²+2Fc²)/3'
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_atom_sites_solution_hydrogens   geom
_refine_ls_hydrogen_treatment    constr
_refine_ls_extinction_method     none
_refine_ls_extinction_coef       .
_refine_ls_number_reflns         2811
_refine_ls_number_parameters     679
_refine_ls_number_restraints     1380
_refine_ls_R_factor_all          0.1344
_refine_ls_R_factor_gt           0.0809
_refine_ls_wR_factor_ref         0.2456
_refine_ls_wR_factor_gt          0.1908
_refine_ls_goodness_of_fit_ref   1.065
_refine_ls_restrained_S_all      0.859
_refine_ls_shift/su_max          0.000
_refine_ls_shift/su_mean         0.000

loop_
_atom_site_label
_atom_site_type_symbol
_atom_site_fract_x
_atom_site_fract_y
_atom_site_fract_z
_atom_site_U_iso_or_equiv
_atom_site_adp_type
_atom_site_occupancy
_atom_site_site_symmetry_order
_atom_site_calc_flag
_atom_site_refinement_flags_posn
_atom_site_refinement_flags_adp
_atom_site_refinement_flags_occupancy
_atom_site_disorder_assembly
_atom_site_disorder_group
Fe1 Fe 0.2696(2) 1.2670(2) 0.64517(13) 0.0877(16) Uani 1 1 d . U . . .
O1 O 0.3683(12) 1.2503(11) 0.4208(7) 0.135(7) Uani 1 1 d . . . . .
O2 O 0.1598(14) 1.4162(10) 0.8167(8) 0.150(7) Uani 1 1 d . . . . .
N1 N 0.3352(13) 1.2125(11) 0.5215(9) 0.093(7) Uani 1 1 d . U . . .
H1A H 0.3552 1.2487 0.5079 0.112 Uiso 1 1 calc R U . . .
N2 N 0.3039(13) 1.2045(11) 0.5719(9) 0.093(6) Uani 1 1 d . U . . .
N3 N 0.2360(12) 1.1659(9) 0.6666(8) 0.076(5) Uani 1 1 d . U . . .
N4 N 0.2244(11) 1.2688(10) 0.7290(7) 0.084(5) Uani 1 1 d . U . . .
N5 N 0.2099(11) 1.3109(9) 0.7716(8) 0.088(6) Uani 1 1 d . U . . .
H5B H 0.2195 1.3531 0.7699 0.105 Uiso 1 1 calc R U . . .
N6 N 0.0835(14) 1.2862(10) 0.5861(8) 0.101(7) Uani 1 1 d . U . . .
H6A H 0.0663 1.2455 0.5879 0.121 Uiso 1 1 calc R U . . .
N7 N 0.1558(14) 1.3086(11) 0.6068(8) 0.088(6) Uani 1 1 d . U . . .
N8 N 0.2953(14) 1.3687(9) 0.6322(7) 0.085(5) Uani 1 1 d . U . . .
N9 N 0.3959(13) 1.2831(11) 0.6786(8) 0.088(6) Uani 1 1 d . U . . .
N10 N 0.4513(13) 1.2495(10) 0.7084(8) 0.098(7) Uani 1 1 d . U . . .
H10A H 0.4481 1.2079 0.7167 0.118 Uiso 1 1 calc R U . . .
C1 C 0.375(2) 1.184(2) 0.4019(16) 0.162(14) Uiso 1 1 d . . . . .
C2 C 0.4002(17) 1.1741(15) 0.3465(12) 0.131(10) Uiso 1 1 d . . . . .
H2A H 0.4162 1.2070 0.3220 0.158 Uiso 1 1 calc R U . . .
C3 C 0.3960(19) 1.1065(17) 0.3366(13) 0.154(12) Uiso 1 1 d . . . . .
H3A H 0.4081 1.0951 0.3009 0.185 Uiso 1 1 calc R U . . .
C4 C 0.377(2) 1.052(2) 0.3690(15) 0.193(15) Uiso 1 1 d . . . . .
H4A H 0.3778 1.0080 0.3568 0.232 Uiso 1 1 calc R U . . .
C5 C 0.3577(16) 1.0706(14) 0.4226(10) 0.112(9) Uiso 1 1 d . . . . .
H5A H 0.3458 1.0376 0.4480 0.135 Uiso 1 1 calc R U . . .
C6 C 0.3556(18) 1.1391(16) 0.4387(13) 0.129(10) Uiso 1 1 d . . . . .
C7 C 0.3289(17) 1.1507(14) 0.4956(12) 0.104(9) Uiso 1 1 d . . . . .
C8 C 0.2954(15) 1.1065(13) 0.5299(10) 0.101(9) Uiso 1 1 d . . . . .
H8A H 0.2837 1.0619 0.5225 0.122 Uiso 1 1 calc R U . . .
C9 C 0.2812(15) 1.1392(13) 0.5781(10) 0.075(8) Uiso 1 1 d . . . . .
C10 C 0.2450(16) 1.1196(14) 0.6275(11) 0.095(8) Uiso 1 1 d . . . . .
C11 C 0.2163(15) 1.0543(13) 0.6397(10) 0.096(8) Uiso 1 1 d . . . . .
H11A H 0.2213 1.0202 0.6143 0.115 Uiso 1 1 calc R U . . .
C12 C 0.1825(16) 1.0426(13) 0.6877(11) 0.109(9) Uiso 1 1 d . . . . .
H12A H 0.1622 0.9998 0.6943 0.130 Uiso 1 1 calc R U . . .
C13 C 0.1752(15) 1.0883(13) 0.7281(10) 0.100(8) Uiso 1 1 d . . . . .
H13A H 0.1527 1.0781 0.7619 0.119 Uiso 1 1 calc R U . . .
C14 C 0.2042(17) 1.1516(13) 0.7147(11) 0.089(8) Uiso 1 1 d . . . . .
C15 C 0.2015(15) 1.2087(13) 0.7500(10) 0.085(8) Uiso 1 1 d . . . . .
C16 C 0.1744(15) 1.2163(13) 0.8026(9) 0.082(8) Uiso 1 1 d . . . . .
H16A H 0.1556 1.1822 0.8252 0.099 Uiso 1 1 calc R U . . .
C17 C 0.1799(15) 1.2815(13) 0.8159(11) 0.088(8) Uiso 1 1 d . . . . .
C18 C 0.1587(14) 1.3190(13) 0.8648(9) 0.083(7) Uiso 1 1 d . . . . .
C19 C 0.1409(18) 1.2844(16) 0.9097(12) 0.134(11) Uiso 1 1 d . . . . .
H19A H 0.1440 1.2381 0.9091 0.161 Uiso 1 1 calc R U . . .
C30 C 0.2534(19) 1.4760(15) 0.5987(10) 0.128(10) Uiso 1 1 d . . . . .
H30A H 0.2104 1.5032 0.5850 0.154 Uiso 1 1 calc R U . . .
C20 C 0.1176(16) 1.3170(14) 0.9580(11) 0.118(9) Uiso 1 1 d . . . . .
H20A H 0.1106 1.2940 0.9904 0.142 Uiso 1 1 calc R U . . .
C21 C 0.1058(16) 1.3841(14) 0.9545(11) 0.117(9) Uiso 1 1 d . . . . .
H21A H 0.0879 1.4058 0.9858 0.140 Uiso 1 1 calc R U . . .
C22 C 0.1174(16) 1.4220(14) 0.9104(11) 0.118(9) Uiso 1 1 d . . . . .
H22A H 0.1082 1.4678 0.9100 0.141 Uiso 1 1 calc R U . . .
C23 C 0.1453(16) 1.3857(15) 0.8640(12) 0.099(9) Uiso 1 1 d . . . . .
C24 C 0.394(2) 1.3006(17) 0.3809(13) 0.173(14) Uiso 1 1 d . . . . .
H24A H 0.3873 1.3443 0.3964 0.259 Uiso 1 1 calc R U . . .
H24B H 0.4519 1.2936 0.3710 0.259 Uiso 1 1 calc R U . . .
H24C H 0.3579 1.2968 0.3492 0.259 Uiso 1 1 calc R U . . .
C25 C 0.132(3) 1.485(2) 0.8145(15) 0.225(18) Uiso 1 1 d . . . . .
H25A H 0.1447 1.5030 0.7795 0.337 Uiso 1 1 calc R U . . .
H25B H 0.0719 1.4868 0.8206 0.337 Uiso 1 1 calc R U . . .
H25C H 0.1614 1.5099 0.8420 0.337 Uiso 1 1 calc R U . . .
C26 C 0.0413(19) 1.3354(14) 0.5620(10) 0.115(10) Uiso 1 1 d . . . . .
H26A H -0.0142 1.3326 0.5485 0.138 Uiso 1 1 calc R U . . .
C27 C 0.0912(17) 1.3902(14) 0.5600(9) 0.107(9) Uiso 1 1 d . . . . .
H27A H 0.0804 1.4303 0.5423 0.128 Uiso 1 1 calc R U . . .
C28 C 0.1622(17) 1.3727(14) 0.5904(10) 0.087(8) Uiso 1 1 d . . . . .
C29 C 0.2413(18) 1.4068(14) 0.6069(10) 0.092(8) Uiso 1 1 d . . . . .
C31 C 0.3340(19) 1.5010(15) 0.6123(10) 0.126(10) Uiso 1 1 d . . . . .
H31A H 0.3493 1.5448 0.6047 0.151 Uiso 1 1 calc R U . . .
C32 C 0.3885(17) 1.4584(14) 0.6371(9) 0.111(9) Uiso 1 1 d . . . . .
H32A H 0.4410 1.4747 0.6488 0.133 Uiso 1 1 calc R U . . .
C33 C 0.3704(18) 1.3921(14) 0.6459(9) 0.091(8) Uiso 1 1 d . . . . .
C34 C 0.4239(18) 1.3443(14) 0.6733(10) 0.091(8) Uiso 1 1 d . . . . .
C35 C 0.4985(16) 1.3531(13) 0.7051(9) 0.098(8) Uiso 1 1 d . . . . .
H35A H 0.5289 1.3922 0.7113 0.118 Uiso 1 1 calc R U . . .
C36 C 0.5149(18) 1.2928(13) 0.7237(9) 0.101(9) Uiso 1 1 d . . . . .
H36A H 0.5626 1.2812 0.7443 0.121 Uiso 1 1 calc R U . . .
Fe2 Fe 0.2250(2) 0.6855(2) 0.34735(12) 0.0869(16) Uani 1 1 d . U . . .
O3 O 0.3289(13) 0.7233(10) 0.1483(7) 0.130(7) Uani 1 1 d . . . . .
O4 O 0.1769(13) 0.8650(9) 0.5025(7) 0.138(7) Uani 1 1 d . . . . .
N11 N 0.2909(12) 0.6537(11) 0.2326(8) 0.092(7) Uani 1 1 d . U . . .
H11B H 0.2795 0.6920 0.2185 0.111 Uiso 1 1 calc R U . . .
N12 N 0.2740(11) 0.6401(10) 0.2848(8) 0.081(6) Uani 1 1 d . U . . .
N13 N 0.2506(11) 0.5990(8) 0.3778(7) 0.074(5) Uiso 1 1 d . . . . .
N14 N 0.1880(13) 0.7000(11) 0.4230(8) 0.088(6) Uani 1 1 d . U . . .
N15 N 0.1623(11) 0.7497(10) 0.4532(8) 0.088(6) Uani 1 1 d . U . . .
H15A H 0.1517 0.7893 0.4415 0.105 Uiso 1 1 calc R U . . .
N16 N 0.0537(14) 0.6163(10) 0.3229(7) 0.096(6) Uani 1 1 d . U . . .
H16B H 0.0601 0.5794 0.3403 0.115 Uiso 1 1 calc R U . . .
N17 N 0.1099(12) 0.6658(10) 0.3215(7) 0.081(5) Uani 1 1 d . U . . .
N18 N 0.1989(14) 0.7678(10) 0.3102(7) 0.084(6) Uiso 1 1 d . . . . .
N19 N 0.3282(12) 0.7382(10) 0.3636(7) 0.083(6) Uani 1 1 d . U . . .
N20 N 0.3963(13) 0.7337(11) 0.3968(8) 0.099(7) Uani 1 1 d . U . . .
H20B H 0.4107 0.6993 0.4156 0.118 Uiso 1 1 calc R U . . .
C37 C 0.3572(16) 0.6682(16) 0.1232(11) 0.101(9) Uiso 1 1 d . . . . .
C38 C 0.3882(17) 0.6685(15) 0.0686(11) 0.129(10) Uiso 1 1 d . . . . .
H38A H 0.3908 0.7082 0.0491 0.155 Uiso 1 1 calc R U . . .
C39 C 0.4135(18) 0.6108(16) 0.0459(12) 0.138(11) Uiso 1 1 d . . . . .
H39A H 0.4327 0.6122 0.0103 0.166 Uiso 1 1 calc R U . . .
C40 C 0.4131(17) 0.5516(15) 0.0709(11) 0.129(10) Uiso 1 1 d . . . . .
H40A H 0.4309 0.5126 0.0538 0.155 Uiso 1 1 calc R U . . .
C41 C 0.3830(16) 0.5523(14) 0.1267(11) 0.118(9) Uiso 1 1 d . . . . .
H41A H 0.3816 0.5129 0.1465 0.142 Uiso 1 1 calc R U . . .
C42 C 0.3576(15) 0.6087(13) 0.1493(10) 0.087(8) Uiso 1 1 d . . . . .
C43 C 0.3273(16) 0.6032(13) 0.2025(11) 0.094(8) Uiso 1 1 d . . . . .
C44 C 0.3305(13) 0.5536(11) 0.2423(9) 0.084(7) Uiso 1 1 d . . . . .
H44A H 0.3525 0.5110 0.2368 0.101 Uiso 1 1 calc R U . . .
C45 C 0.2967(15) 0.5754(13) 0.2907(10) 0.086(8) Uiso 1 1 d . . . . .
C46 C 0.2839(16) 0.5551(12) 0.3452(10) 0.087(8) Uiso 1 1 d . . . . .
C47 C 0.3021(16) 0.4908(14) 0.3675(11) 0.122(9) Uiso 1 1 d . . . . .
H47A H 0.3230 0.4568 0.3457 0.147 Uiso 1 1 calc R U . . .
C48 C 0.2883(18) 0.4799(16) 0.4219(12) 0.141(11) Uiso 1 1 d . . . . .
H48A H 0.3039 0.4396 0.4379 0.170 Uiso 1 1 calc R U . . .
C49 C 0.2520(18) 0.5280(15) 0.4516(12) 0.133(10) Uiso 1 1 d . . . . .
H49A H 0.2395 0.5192 0.4878 0.160 Uiso 1 1 calc R U . . .
C50 C 0.2324(15) 0.5898(13) 0.4310(10) 0.088(8) Uiso 1 1 d . . . . .
C51 C 0.1988(16) 0.6440(14) 0.4566(11) 0.083(9) Uiso 1 1 d . . . . .
C52 C 0.1805(15) 0.6640(12) 0.5073(11) 0.097(8) Uiso 1 1 d . . . . .
H52A H 0.1847 0.6373 0.5381 0.116 Uiso 1 1 calc R U . . .
C53 C 0.1546(16) 0.7295(13) 0.5070(11) 0.089(8) Uiso 1 1 d . . . . .
C54 C 0.1267(16) 0.7764(14) 0.5477(10) 0.094(9) Uiso 1 1 d . . . . .
C55 C 0.0950(15) 0.7476(14) 0.5939(10) 0.110(9) Uiso 1 1 d . . . . .
H55A H 0.0902 0.7013 0.5953 0.132 Uiso 1 1 calc R U . . .
C56 C 0.0692(17) 0.7854(15) 0.6396(11) 0.121(10) Uiso 1 1 d . . . . .
H56A H 0.0443 0.7660 0.6699 0.145 Uiso 1 1 calc R U . . .
C57 C 0.0836(19) 0.8508(16) 0.6357(13) 0.145(11) Uiso 1 1 d . . . . .
H57A H 0.0715 0.8771 0.6658 0.174 Uiso 1 1 calc R U . . .
C58 C 0.1142(18) 0.8817(16) 0.5914(12) 0.134(10) Uiso 1 1 d . . . . .
H58A H 0.1163 0.9280 0.5898 0.160 Uiso 1 1 calc R U . . .
C59 C 0.1416(17) 0.8449(15) 0.5498(13) 0.105(9) Uiso 1 1 d . . . . .
C60 C 0.3413(19) 0.7859(16) 0.1230(12) 0.146(12) Uiso 1 1 d . . . . .
H60A H 0.3180 0.8205 0.1454 0.219 Uiso 1 1 calc R U . . .
H60B H 0.4012 0.7935 0.1183 0.219 Uiso 1 1 calc R U . . .
H60C H 0.3133 0.7862 0.0883 0.219 Uiso 1 1 calc R U . . .
C61 C 0.189(2) 0.9338(16) 0.4983(12) 0.155(12) Uiso 1 1 d . . . . .
H61A H 0.2141 0.9440 0.4639 0.232 Uiso 1 1 calc R U . . .
H61B H 0.1350 0.9560 0.5012 0.232 Uiso 1 1 calc R U . . .
H61C H 0.2261 0.9486 0.5271 0.232 Uiso 1 1 calc R U . . .
C62 C -0.014(2) 0.6327(15) 0.2936(11) 0.125(10) Uiso 1 1 d . . . . .
H62A H -0.0593 0.6046 0.2859 0.150 Uiso 1 1 calc R U . . .
C63 C -0.0064(16) 0.6950(13) 0.2768(9) 0.099(8) Uiso 1 1 d . . . . .
H63A H -0.0470 0.7205 0.2585 0.119 Uiso 1 1 calc R U . . .
C64 C 0.0757(18) 0.7143(14) 0.2925(9) 0.084(8) Uiso 1 1 d . . . . .
C65 C 0.1233(17) 0.7716(14) 0.2825(10) 0.096(8) Uiso 1 1 d . . . . .
C66 C 0.1112(17) 0.8258(13) 0.2493(10) 0.113(9) Uiso 1 1 d . . . . .
H66A H 0.0609 0.8302 0.2294 0.135 Uiso 1 1 calc R U . . .
C67 C 0.1733(18) 0.8735(13) 0.2455(10) 0.112(9) Uiso 1 1 d . . . . .
H67A H 0.1654 0.9096 0.2223 0.135 Uiso 1 1 calc R U . . .
C68 C 0.2487(17) 0.8686(13) 0.2762(10) 0.110(9) Uiso 1 1 d . . . . .
H68A H 0.2904 0.9016 0.2744 0.132 Uiso 1 1 calc R U . . .
C69 C 0.2591(16) 0.8136(13) 0.3090(9) 0.085(8) Uiso 1 1 d . . . . .
C70 C 0.3311(18) 0.8006(15) 0.3444(11) 0.092(9) Uiso 1 1 d . . . . .
C71 C 0.3995(17) 0.8369(14) 0.3618(10) 0.100(8) Uiso 1 1 d . . . . .
H71A H 0.4154 0.8803 0.3529 0.120 Uiso 1 1 calc R U . . .
C72 C 0.4381(18) 0.7925(13) 0.3955(10) 0.097(9) Uiso 1 1 d . . . . .
H72A H 0.4874 0.8015 0.4154 0.116 Uiso 1 1 calc R U . . .
Cl1_1 Cl 0.4996(5) 0.9116(4) 0.2406(3) 0.130(3) Uani 1 1 d D . . . .
O1_1 O 0.5692(8) 0.8910(8) 0.2754(6) 0.150(7) Uiso 1 1 d D . . . .
O2_1 O 0.4484(10) 0.8535(7) 0.2283(6) 0.151(7) Uiso 1 1 d D . . . .
O3_1 O 0.4483(10) 0.9603(7) 0.2681(7) 0.176(9) Uiso 1 1 d D . . . .
O4_1 O 0.5321(10) 0.9392(8) 0.1911(5) 0.152(7) Uiso 1 1 d D . . . .
Cl1_2 Cl 0.5117(14) 0.6431(11) 0.4925(7) 0.219(18) Uani 0.64(3) 1 d D . P A 1
O1_2 O 0.472(3) 0.6172(18) 0.4439(10) 0.15(2) Uiso 0.64(3) 1 d D . P A 1
O2_2 O 0.4889(17) 0.7123(11) 0.4996(10) 0.125(16) Uiso 0.64(3) 1 d D . P A 1
O3_2 O 0.6027(16) 0.6377(15) 0.4871(12) 0.140(16) Uiso 0.64(3) 1 d D . P A 1
O4_2 O 0.4830(17) 0.6058(13) 0.5388(9) 0.113(12) Uiso 0.64(3) 1 d D . P A 1
Cl1_3 Cl 0.4965(18) 0.6339(12) 0.4899(8) 0.052(11) Uani 0.36(3) 1 d D . P A 2
O1_3 O 0.450(3) 0.613(2) 0.4420(14) 0.08(3) Uiso 0.36(3) 1 d D . P A 2
O2_3 O 0.560(4) 0.682(3) 0.475(2) 0.25(5) Uiso 0.36(3) 1 d D . P A 2
O3_3 O 0.537(4) 0.5766(18) 0.514(2) 0.18(3) Uiso 0.36(3) 1 d D . P A 2
O4_3 O 0.438(3) 0.663(4) 0.528(2) 0.32(7) Uiso 0.36(3) 1 d D . P A 2
Cl1_4 Cl 0.0188(8) 0.8755(7) 0.3952(5) 0.119(3) Uani 0.79(3) 1 d D . P B 1
O1_4 O 0.1096(10) 0.8739(13) 0.3874(11) 0.134(19) Uiso 0.79(3) 1 d D . P B 1
O2_4 O -0.0246(14) 0.8515(11) 0.3472(7) 0.141(11) Uiso 0.79(3) 1 d D . P B 1
O3_4 O -0.0080(14) 0.9430(8) 0.4061(9) 0.139(11) Uiso 0.79(3) 1 d D . P B 1
O4_4 O -0.0037(13) 0.8337(9) 0.4407(7) 0.126(10) Uiso 0.79(3) 1 d D . P B 1
Cl1_5 Cl 0.018(3) 0.889(2) 0.384(2) 0.119(3) Uani 0.21(3) 1 d D . P B 2
O1_5 O 0.101(4) 0.858(4) 0.382(3) 0.05(4) Uiso 0.21(3) 1 d D . P B 2
O2_5 O -0.046(5) 0.838(4) 0.378(4) 0.19(6) Uiso 0.21(3) 1 d D . P B 2
O3_5 O 0.008(5) 0.922(4) 0.436(2) 0.13(4) Uiso 0.21(3) 1 d D . P B 2
O4_5 O 0.009(5) 0.937(4) 0.341(3) 0.19(5) Uiso 0.21(3) 1 d D . P B 2
Cl1_6 Cl 0.0017(9) 0.4507(7) 0.3696(5) 0.124(3) Uani 0.73(3) 1 d D . P C 1
O1_6 O 0.0735(12) 0.4947(10) 0.3772(10) 0.125(11) Uiso 0.73(3) 1 d D . P C 1
O2_6 O -0.0597(13) 0.4823(10) 0.3340(9) 0.142(12) Uiso 0.73(3) 1 d D . P C 1
O3_6 O 0.0304(14) 0.3892(9) 0.3456(9) 0.133(11) Uiso 0.73(3) 1 d D . P C 1
O4_6 O -0.0360(17) 0.4369(12) 0.4215(7) 0.152(13) Uiso 0.73(3) 1 d D . P C 1
Cl1_7 Cl 0.005(2) 0.4434(18) 0.3710(13) 0.124(3) Uani 0.27(3) 1 d D . P C 2
O1_7 O 0.047(3) 0.497(2) 0.400(2) 0.12(3) Uiso 0.27(3) 1 d D . P C 2
O2_7 O 0.007(4) 0.457(3) 0.3136(14) 0.15(4) Uiso 0.27(3) 1 d D . P C 2
O3_7 O 0.048(3) 0.381(2) 0.382(3) 0.14(3) Uiso 0.27(3) 1 d D . P C 2
O4_7 O -0.082(2) 0.438(3) 0.388(2) 0.12(3) Uiso 0.27(3) 1 d D . P C 2


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

loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
_geom_bond_publ_flag
Fe1 N8 2.103(19) . ?
Fe1 N3 2.16(2) . ?
Fe1 N9 2.17(2) . ?
Fe1 N7 2.18(2) . ?
Fe1 N4 2.190(19) . ?
Fe1 N2 2.26(2) . ?
O1 C1 1.41(4) . ?
O1 C24 1.46(3) . ?
O2 C23 1.34(3) . ?
O2 C25 1.44(4) . ?
N1 N2 1.35(2) . ?
N1 C7 1.40(3) . ?
N1 H1A 0.8600 . ?
N2 C9 1.36(3) . ?
N3 C14 1.32(3) . ?
N3 C10 1.35(3) . ?
N4 C15 1.36(2) . ?
N4 N5 1.37(2) . ?
N5 C17 1.33(2) . ?
N5 H5B 0.8600 . ?
N6 N7 1.32(2) . ?
N6 C26 1.33(3) . ?
N6 H6A 0.8600 . ?
N7 C28 1.35(3) . ?
N8 C29 1.30(3) . ?
N8 C33 1.31(3) . ?
N9 C34 1.31(3) . ?
N9 N10 1.32(2) . ?
N10 C36 1.37(3) . ?
N10 H10A 0.8600 . ?
C1 C6 1.31(4) . ?
C1 C2 1.44(4) . ?
C2 C3 1.38(3) . ?
C2 H2A 0.9300 . ?
C3 C4 1.39(4) . ?
C3 H3A 0.9300 . ?
C4 C5 1.41(3) . ?
C4 H4A 0.9300 . ?
C5 C6 1.43(3) . ?
C5 H5A 0.9300 . ?
C6 C7 1.49(3) . ?
C7 C8 1.33(3) . ?
C8 C9 1.38(3) . ?
C8 H8A 0.9300 . ?
C9 C10 1.40(3) . ?
C10 C11 1.42(3) . ?
C11 C12 1.32(3) . ?
C11 H11A 0.9300 . ?
C12 C13 1.36(3) . ?
C12 H12A 0.9300 . ?
C13 C14 1.39(3) . ?
C13 H13A 0.9300 . ?
C14 C15 1.44(3) . ?
C15 C16 1.38(3) . ?
C16 C17 1.35(3) . ?
C16 H16A 0.9300 . ?
C17 C18 1.46(3) . ?
C18 C19 1.34(3) . ?
C18 C23 1.35(3) . ?
C19 C20 1.41(3) . ?
C19 H19A 0.9300 . ?
C30 C31 1.40(3) . ?
C30 C29 1.41(3) . ?
C30 H30A 0.9300 . ?
C20 C21 1.36(3) . ?
C20 H20A 0.9300 . ?
C21 C22 1.34(3) . ?
C21 H21A 0.9300 . ?
C22 C23 1.43(3) . ?
C22 H22A 0.9300 . ?
C24 H24A 0.9600 . ?
C24 H24B 0.9600 . ?
C24 H24C 0.9600 . ?
C25 H25A 0.9600 . ?
C25 H25B 0.9600 . ?
C25 H25C 0.9600 . ?
C26 C27 1.35(3) . ?
C26 H26A 0.9300 . ?
C27 C28 1.38(3) . ?
C27 H27A 0.9300 . ?
C28 C29 1.47(3) . ?
C31 C32 1.35(3) . ?
C31 H31A 0.9300 . ?
C32 C33 1.37(3) . ?
C32 H32A 0.9300 . ?
C33 C34 1.44(3) . ?
C34 C35 1.41(3) . ?
C35 C36 1.32(3) . ?
C35 H35A 0.9300 . ?
C36 H36A 0.9300 . ?
Fe2 N18 1.929(19) . ?
Fe2 N13 1.931(17) . ?
Fe2 N17 1.95(2) . ?
Fe2 N12 1.95(2) . ?
Fe2 N19 1.97(2) . ?
Fe2 N14 1.98(2) . ?
O3 C37 1.34(3) . ?
O3 C60 1.41(3) . ?
O4 C59 1.36(3) . ?
O4 C61 1.40(3) . ?
N11 N12 1.35(2) . ?
N11 C43 1.38(3) . ?
N11 H11B 0.8600 . ?
N12 C45 1.35(2) . ?
N13 C46 1.30(2) . ?
N13 C50 1.35(2) . ?
N14 N15 1.31(2) . ?
N14 C51 1.40(3) . ?
N15 C53 1.39(3) . ?
N15 H15A 0.8600 . ?
N16 C62 1.32(3) . ?
N16 N17 1.33(2) . ?
N16 H16B 0.8600 . ?
N17 C64 1.32(3) . ?
N18 C69 1.32(3) . ?
N18 C65 1.37(3) . ?
N19 C70 1.34(3) . ?
N19 N20 1.34(2) . ?
N20 C72 1.35(3) . ?
N20 H20B 0.8600 . ?
C37 C42 1.36(3) . ?
C37 C38 1.43(3) . ?
C38 C39 1.35(3) . ?
C38 H38A 0.9300 . ?
C39 C40 1.34(3) . ?
C39 H39A 0.9300 . ?
C40 C41 1.46(3) . ?
C40 H40A 0.9300 . ?
C41 C42 1.32(3) . ?
C41 H41A 0.9300 . ?
C42 C43 1.40(3) . ?
C43 C44 1.40(3) . ?
C44 C45 1.38(3) . ?
C44 H44A 0.9300 . ?
C45 C46 1.42(3) . ?
C46 C47 1.43(3) . ?
C47 C48 1.38(3) . ?
C47 H47A 0.9300 . ?
C48 C49 1.34(3) . ?
C48 H48A 0.9300 . ?
C49 C50 1.37(3) . ?
C49 H49A 0.9300 . ?
C50 C51 1.36(3) . ?
C51 C52 1.34(3) . ?
C52 C53 1.37(3) . ?
C52 H52A 0.9300 . ?
C53 C54 1.44(3) . ?
C54 C55 1.37(3) . ?
C54 C59 1.39(3) . ?
C55 C56 1.42(3) . ?
C55 H55A 0.9300 . ?
C56 C57 1.33(3) . ?
C56 H56A 0.9300 . ?
C57 C58 1.35(3) . ?
C57 H57A 0.9300 . ?
C58 C59 1.34(3) . ?
C58 H58A 0.9300 . ?
C60 H60A 0.9600 . ?
C60 H60B 0.9600 . ?
C60 H60C 0.9600 . ?
C61 H61A 0.9600 . ?
C61 H61B 0.9600 . ?
C61 H61C 0.9600 . ?
C62 C63 1.32(3) . ?
C62 H62A 0.9300 . ?
C63 C64 1.40(3) . ?
C63 H63A 0.9300 . ?
C64 C65 1.39(3) . ?
C65 C66 1.37(3) . ?
C66 C67 1.37(3) . ?
C66 H66A 0.9300 . ?
C67 C68 1.40(3) . ?
C67 H67A 0.9300 . ?
C68 C69 1.38(3) . ?
C68 H68A 0.9300 . ?
C69 C70 1.45(3) . ?
C70 C71 1.36(3) . ?
C71 C72 1.36(3) . ?
C71 H71A 0.9300 . ?
C72 H72A 0.9300 . ?
Cl1_1 O4_1 1.436(9) . ?
Cl1_1 O3_1 1.438(9) . ?
Cl1_1 O1_1 1.444(9) . ?
Cl1_1 O2_1 1.444(9) . ?
Cl1_2 O4_2 1.439(9) . ?
Cl1_2 O3_2 1.440(9) . ?
Cl1_2 O2_2 1.442(9) . ?
Cl1_2 O1_2 1.444(9) . ?
Cl1_3 O4_3 1.440(9) . ?
Cl1_3 O2_3 1.441(10) . ?
Cl1_3 O3_3 1.442(9) . ?
Cl1_3 O1_3 1.443(9) . ?
Cl1_4 O1_4 1.441(9) . ?
Cl1_4 O2_4 1.443(9) . ?
Cl1_4 O4_4 1.444(9) . ?
Cl1_4 O3_4 1.444(9) . ?
Cl1_5 O4_5 1.441(9) . ?
Cl1_5 O1_5 1.442(9) . ?
Cl1_5 O2_5 1.442(9) . ?
Cl1_5 O3_5 1.442(9) . ?
Cl1_6 O3_6 1.440(9) . ?
Cl1_6 O4_6 1.441(9) . ?
Cl1_6 O1_6 1.442(9) . ?
Cl1_6 O2_6 1.444(9) . ?
Cl1_7 O3_7 1.441(9) . ?
Cl1_7 O4_7 1.442(9) . ?
Cl1_7 O1_7 1.442(9) . ?
Cl1_7 O2_7 1.442(9) . ?

loop_
_geom_angle_atom_site_label_1
_geom_angle_atom_site_label_2
_geom_angle_atom_site_label_3
_geom_angle
_geom_angle_site_symmetry_1
_geom_angle_site_symmetry_3
_geom_angle_publ_flag
N8 Fe1 N3 173.7(8) . . ?
N8 Fe1 N9 74.8(8) . . ?
N3 Fe1 N9 105.8(8) . . ?
N8 Fe1 N7 73.8(8) . . ?
N3 Fe1 N7 105.3(8) . . ?
N9 Fe1 N7 148.5(9) . . ?
N8 Fe1 N4 101.1(7) . . ?
N3 Fe1 N4 72.7(8) . . ?
N9 Fe1 N4 86.6(7) . . ?
N7 Fe1 N4 97.6(7) . . ?
N8 Fe1 N2 111.6(8) . . ?
N3 Fe1 N2 74.7(8) . . ?
N9 Fe1 N2 99.3(7) . . ?
N7 Fe1 N2 93.7(7) . . ?
N4 Fe1 N2 147.3(8) . . ?
C1 O1 C24 114(3) . . ?
C23 O2 C25 114(3) . . ?
N2 N1 C7 107(2) . . ?
N2 N1 H1A 126.5 . . ?
C7 N1 H1A 126.5 . . ?
N1 N2 C9 108(2) . . ?
N1 N2 Fe1 139.4(18) . . ?
C9 N2 Fe1 112.2(17) . . ?
C14 N3 C10 122(2) . . ?
C14 N3 Fe1 121.1(17) . . ?
C10 N3 Fe1 116.4(18) . . ?
C15 N4 N5 102.0(19) . . ?
C15 N4 Fe1 115.7(17) . . ?
N5 N4 Fe1 142.3(16) . . ?
C17 N5 N4 115(2) . . ?
C17 N5 H5B 122.6 . . ?
N4 N5 H5B 122.6 . . ?
N7 N6 C26 110(2) . . ?
N7 N6 H6A 124.9 . . ?
C26 N6 H6A 124.9 . . ?
N6 N7 C28 106(2) . . ?
N6 N7 Fe1 137.5(19) . . ?
C28 N7 Fe1 115.5(19) . . ?
C29 N8 C33 120(2) . . ?
C29 N8 Fe1 121.2(18) . . ?
C33 N8 Fe1 118.8(18) . . ?
C34 N9 N10 108(2) . . ?
C34 N9 Fe1 114(2) . . ?
N10 N9 Fe1 137.2(18) . . ?
N9 N10 C36 108(2) . . ?
N9 N10 H10A 126.1 . . ?
C36 N10 H10A 126.1 . . ?
C6 C1 O1 113(4) . . ?
C6 C1 C2 129(4) . . ?
O1 C1 C2 118(3) . . ?
C3 C2 C1 107(3) . . ?
C3 C2 H2A 126.6 . . ?
C1 C2 H2A 126.6 . . ?
C2 C3 C4 133(3) . . ?
C2 C3 H3A 113.5 . . ?
C4 C3 H3A 113.5 . . ?
C3 C4 C5 112(3) . . ?
C3 C4 H4A 123.8 . . ?
C5 C4 H4A 123.8 . . ?
C4 C5 C6 121(3) . . ?
C4 C5 H5A 119.3 . . ?
C6 C5 H5A 119.3 . . ?
C1 C6 C5 117(3) . . ?
C1 C6 C7 128(3) . . ?
C5 C6 C7 115(3) . . ?
C8 C7 N1 109(3) . . ?
C8 C7 C6 128(3) . . ?
N1 C7 C6 123(3) . . ?
C7 C8 C9 107(3) . . ?
C7 C8 H8A 126.3 . . ?
C9 C8 H8A 126.3 . . ?
N2 C9 C8 108(2) . . ?
N2 C9 C10 118(2) . . ?
C8 C9 C10 133(3) . . ?
N3 C10 C9 118(3) . . ?
N3 C10 C11 117(3) . . ?
C9 C10 C11 125(3) . . ?
C12 C11 C10 119(3) . . ?
C12 C11 H11A 120.5 . . ?
C10 C11 H11A 120.5 . . ?
C11 C12 C13 125(3) . . ?
C11 C12 H12A 117.5 . . ?
C13 C12 H12A 117.5 . . ?
C12 C13 C14 114(3) . . ?
C12 C13 H13A 122.8 . . ?
C14 C13 H13A 122.8 . . ?
N3 C14 C13 123(3) . . ?
N3 C14 C15 113(3) . . ?
C13 C14 C15 125(3) . . ?
N4 C15 C16 110(2) . . ?
N4 C15 C14 118(2) . . ?
C16 C15 C14 132(3) . . ?
C17 C16 C15 108(2) . . ?
C17 C16 H16A 125.8 . . ?
C15 C16 H16A 125.8 . . ?
N5 C17 C16 105(2) . . ?
N5 C17 C18 122(2) . . ?
C16 C17 C18 133(3) . . ?
C19 C18 C23 119(3) . . ?
C19 C18 C17 118(3) . . ?
C23 C18 C17 122(2) . . ?
C18 C19 C20 121(3) . . ?
C18 C19 H19A 119.5 . . ?
C20 C19 H19A 119.5 . . ?
C31 C30 C29 116(3) . . ?
C31 C30 H30A 122.0 . . ?
C29 C30 H30A 122.0 . . ?
C21 C20 C19 116(3) . . ?
C21 C20 H20A 121.9 . . ?
C19 C20 H20A 121.9 . . ?
C22 C21 C20 126(3) . . ?
C22 C21 H21A 116.9 . . ?
C20 C21 H21A 116.9 . . ?
C21 C22 C23 114(3) . . ?
C21 C22 H22A 123.0 . . ?
C23 C22 H22A 123.0 . . ?
O2 C23 C18 116(3) . . ?
O2 C23 C22 121(3) . . ?
C18 C23 C22 123(3) . . ?
O1 C24 H24A 109.5 . . ?
O1 C24 H24B 109.5 . . ?
H24A C24 H24B 109.5 . . ?
O1 C24 H24C 109.5 . . ?
H24A C24 H24C 109.5 . . ?
H24B C24 H24C 109.5 . . ?
O2 C25 H25A 109.5 . . ?
O2 C25 H25B 109.5 . . ?
H25A C25 H25B 109.5 . . ?
O2 C25 H25C 109.5 . . ?
H25A C25 H25C 109.5 . . ?
H25B C25 H25C 109.5 . . ?
N6 C26 C27 109(3) . . ?
N6 C26 H26A 125.3 . . ?
C27 C26 H26A 125.3 . . ?
C26 C27 C28 104(3) . . ?
C26 C27 H27A 128.0 . . ?
C28 C27 H27A 128.0 . . ?
N7 C28 C27 110(3) . . ?
N7 C28 C29 115(3) . . ?
C27 C28 C29 135(3) . . ?
N8 C29 C30 124(3) . . ?
N8 C29 C28 114(3) . . ?
C30 C29 C28 122(3) . . ?
C32 C31 C30 117(3) . . ?
C32 C31 H31A 121.6 . . ?
C30 C31 H31A 121.6 . . ?
C31 C32 C33 123(3) . . ?
C31 C32 H32A 118.3 . . ?
C33 C32 H32A 118.3 . . ?
N8 C33 C32 119(3) . . ?
N8 C33 C34 114(3) . . ?
C32 C33 C34 127(3) . . ?
N9 C34 C35 110(3) . . ?
N9 C34 C33 118(3) . . ?
C35 C34 C33 131(3) . . ?
C36 C35 C34 104(3) . . ?
C36 C35 H35A 128.1 . . ?
C34 C35 H35A 128.1 . . ?
C35 C36 N10 110(3) . . ?
C35 C36 H36A 125.0 . . ?
N10 C36 H36A 125.0 . . ?
N18 Fe2 N13 174.5(8) . . ?
N18 Fe2 N17 79.9(9) . . ?
N13 Fe2 N17 97.7(8) . . ?
N18 Fe2 N12 96.2(8) . . ?
N13 Fe2 N12 78.8(8) . . ?
N17 Fe2 N12 91.0(7) . . ?
N18 Fe2 N19 79.1(9) . . ?
N13 Fe2 N19 103.5(8) . . ?
N17 Fe2 N19 158.7(9) . . ?
N12 Fe2 N19 94.7(7) . . ?
N18 Fe2 N14 105.0(8) . . ?
N13 Fe2 N14 80.0(8) . . ?
N17 Fe2 N14 93.4(8) . . ?
N12 Fe2 N14 158.8(8) . . ?
N19 Fe2 N14 88.7(8) . . ?
C37 O3 C60 119(2) . . ?
C59 O4 C61 114(2) . . ?
N12 N11 C43 117(2) . . ?
N12 N11 H11B 121.6 . . ?
C43 N11 H11B 121.6 . . ?
N11 N12 C45 104(2) . . ?
N11 N12 Fe2 138.0(17) . . ?
C45 N12 Fe2 117.9(17) . . ?
C46 N13 C50 126(2) . . ?
C46 N13 Fe2 116.7(16) . . ?
C50 N13 Fe2 116.9(16) . . ?
N15 N14 C51 108(2) . . ?
N15 N14 Fe2 137.9(18) . . ?
C51 N14 Fe2 113.8(19) . . ?
N14 N15 C53 110(2) . . ?
N14 N15 H15A 124.8 . . ?
C53 N15 H15A 124.8 . . ?
C62 N16 N17 109(2) . . ?
C62 N16 H16B 125.4 . . ?
N17 N16 H16B 125.4 . . ?
C64 N17 N16 107(2) . . ?
C64 N17 Fe2 113.6(19) . . ?
N16 N17 Fe2 139.2(17) . . ?
C69 N18 C65 125(2) . . ?
C69 N18 Fe2 117.1(19) . . ?
C65 N18 Fe2 117.7(19) . . ?
C70 N19 N20 104(2) . . ?
C70 N19 Fe2 117.3(19) . . ?
N20 N19 Fe2 137.4(18) . . ?
N19 N20 C72 108(2) . . ?
N19 N20 H20B 125.9 . . ?
C72 N20 H20B 125.9 . . ?
O3 C37 C42 120(3) . . ?
O3 C37 C38 123(3) . . ?
C42 C37 C38 117(3) . . ?
C39 C38 C37 119(3) . . ?
C39 C38 H38A 120.3 . . ?
C37 C38 H38A 120.3 . . ?
C40 C39 C38 125(3) . . ?
C40 C39 H39A 117.7 . . ?
C38 C39 H39A 117.7 . . ?
C39 C40 C41 115(3) . . ?
C39 C40 H40A 122.3 . . ?
C41 C40 H40A 122.3 . . ?
C42 C41 C40 121(3) . . ?
C42 C41 H41A 119.7 . . ?
C40 C41 H41A 119.7 . . ?
C41 C42 C37 123(3) . . ?
C41 C42 C43 116(3) . . ?
C37 C42 C43 121(3) . . ?
N11 C43 C44 99(2) . . ?
N11 C43 C42 126(2) . . ?
C44 C43 C42 134(3) . . ?
C45 C44 C43 112(2) . . ?
C45 C44 H44A 124.2 . . ?
C43 C44 H44A 124.2 . . ?
N12 C45 C44 108(2) . . ?
N12 C45 C46 110(2) . . ?
C44 C45 C46 142(3) . . ?
N13 C46 C45 117(2) . . ?
N13 C46 C47 117(2) . . ?
C45 C46 C47 126(2) . . ?
C48 C47 C46 119(3) . . ?
C48 C47 H47A 120.5 . . ?
C46 C47 H47A 120.5 . . ?
C49 C48 C47 119(3) . . ?
C49 C48 H48A 120.4 . . ?
C47 C48 H48A 120.4 . . ?
C48 C49 C50 123(3) . . ?
C48 C49 H49A 118.6 . . ?
C50 C49 H49A 118.6 . . ?
N13 C50 C51 115(2) . . ?
N13 C50 C49 116(2) . . ?
C51 C50 C49 129(3) . . ?
C52 C51 C50 139(3) . . ?
C52 C51 N14 106(3) . . ?
C50 C51 N14 114(3) . . ?
C51 C52 C53 110(3) . . ?
C51 C52 H52A 124.9 . . ?
C53 C52 H52A 124.9 . . ?
C52 C53 N15 105(2) . . ?
C52 C53 C54 135(3) . . ?
N15 C53 C54 120(2) . . ?
C55 C54 C59 116(3) . . ?
C55 C54 C53 115(3) . . ?
C59 C54 C53 128(3) . . ?
C54 C55 C56 123(3) . . ?
C54 C55 H55A 118.6 . . ?
C56 C55 H55A 118.6 . . ?
C57 C56 C55 115(3) . . ?
C57 C56 H56A 122.7 . . ?
C55 C56 H56A 122.7 . . ?
C56 C57 C58 125(3) . . ?
C56 C57 H57A 117.6 . . ?
C58 C57 H57A 117.6 . . ?
C59 C58 C57 119(3) . . ?
C59 C58 H58A 120.4 . . ?
C57 C58 H58A 120.4 . . ?
C58 C59 O4 129(3) . . ?
C58 C59 C54 121(3) . . ?
O4 C59 C54 109(3) . . ?
O3 C60 H60A 109.5 . . ?
O3 C60 H60B 109.5 . . ?
H60A C60 H60B 109.5 . . ?
O3 C60 H60C 109.5 . . ?
H60A C60 H60C 109.5 . . ?
H60B C60 H60C 109.5 . . ?
O4 C61 H61A 109.5 . . ?
O4 C61 H61B 109.5 . . ?
H61A C61 H61B 109.5 . . ?
O4 C61 H61C 109.5 . . ?
H61A C61 H61C 109.5 . . ?
H61B C61 H61C 109.5 . . ?
N16 C62 C63 110(3) . . ?
N16 C62 H62A 125.2 . . ?
C63 C62 H62A 125.2 . . ?
C62 C63 C64 105(3) . . ?
C62 C63 H63A 127.6 . . ?
C64 C63 H63A 127.6 . . ?
N17 C64 C65 119(3) . . ?
N17 C64 C63 108(3) . . ?
C65 C64 C63 132(3) . . ?
N18 C65 C66 117(3) . . ?
N18 C65 C64 109(3) . . ?
C66 C65 C64 133(3) . . ?
C67 C66 C65 120(3) . . ?
C67 C66 H66A 120.1 . . ?
C65 C66 H66A 120.1 . . ?
C66 C67 C68 121(3) . . ?
C66 C67 H67A 119.5 . . ?
C68 C67 H67A 119.5 . . ?
C69 C68 C67 118(3) . . ?
C69 C68 H68A 121.0 . . ?
C67 C68 H68A 121.0 . . ?
N18 C69 C68 119(3) . . ?
N18 C69 C70 115(3) . . ?
C68 C69 C70 126(3) . . ?
N19 C70 C71 115(3) . . ?
N19 C70 C69 111(3) . . ?
C71 C70 C69 135(3) . . ?
C72 C71 C70 101(3) . . ?
C72 C71 H71A 129.6 . . ?
C70 C71 H71A 129.6 . . ?
N20 C72 C71 112(3) . . ?
N20 C72 H72A 124.1 . . ?
C71 C72 H72A 124.1 . . ?
O4_1 Cl1_1 O3_1 110.1(9) . . ?
O4_1 Cl1_1 O1_1 110.0(9) . . ?
O3_1 Cl1_1 O1_1 109.7(9) . . ?
O4_1 Cl1_1 O2_1 109.5(8) . . ?
O3_1 Cl1_1 O2_1 109.4(9) . . ?
O1_1 Cl1_1 O2_1 108.1(8) . . ?
O4_2 Cl1_2 O3_2 110.6(11) . . ?
O4_2 Cl1_2 O2_2 108.9(10) . . ?
O3_2 Cl1_2 O2_2 109.3(10) . . ?
O4_2 Cl1_2 O1_2 109.5(11) . . ?
O3_2 Cl1_2 O1_2 108.7(11) . . ?
O2_2 Cl1_2 O1_2 109.9(11) . . ?
O4_3 Cl1_3 O2_3 109.9(11) . . ?
O4_3 Cl1_3 O3_3 109.4(11) . . ?
O2_3 Cl1_3 O3_3 109.4(11) . . ?
O4_3 Cl1_3 O1_3 109.6(11) . . ?
O2_3 Cl1_3 O1_3 109.4(11) . . ?
O3_3 Cl1_3 O1_3 109.1(11) . . ?
O1_4 Cl1_4 O2_4 110.2(10) . . ?
O1_4 Cl1_4 O4_4 109.8(10) . . ?
O2_4 Cl1_4 O4_4 109.1(10) . . ?
O1_4 Cl1_4 O3_4 109.6(10) . . ?
O2_4 Cl1_4 O3_4 109.2(10) . . ?
O4_4 Cl1_4 O3_4 109.0(10) . . ?
O4_5 Cl1_5 O1_5 109.7(11) . . ?
O4_5 Cl1_5 O2_5 109.4(11) . . ?
O1_5 Cl1_5 O2_5 109.5(11) . . ?
O4_5 Cl1_5 O3_5 109.2(11) . . ?
O1_5 Cl1_5 O3_5 109.6(11) . . ?
O2_5 Cl1_5 O3_5 109.4(11) . . ?
O3_6 Cl1_6 O4_6 109.3(10) . . ?
O3_6 Cl1_6 O1_6 109.3(10) . . ?
O4_6 Cl1_6 O1_6 109.1(10) . . ?
O3_6 Cl1_6 O2_6 109.6(10) . . ?
O4_6 Cl1_6 O2_6 110.3(10) . . ?
O1_6 Cl1_6 O2_6 109.2(9) . . ?
O3_7 Cl1_7 O4_7 109.2(11) . . ?
O3_7 Cl1_7 O1_7 109.7(11) . . ?
O4_7 Cl1_7 O1_7 109.5(11) . . ?
O3_7 Cl1_7 O2_7 109.7(11) . . ?
O4_7 Cl1_7 O2_7 109.4(11) . . ?
O1_7 Cl1_7 O2_7 109.3(11) . . ?

loop_
_geom_torsion_atom_site_label_1
_geom_torsion_atom_site_label_2
_geom_torsion_atom_site_label_3
_geom_torsion_atom_site_label_4
_geom_torsion
_geom_torsion_site_symmetry_1
_geom_torsion_site_symmetry_2
_geom_torsion_site_symmetry_3
_geom_torsion_site_symmetry_4
_geom_torsion_publ_flag
C7 N1 N2 C9 2(3) . . . . ?
C7 N1 N2 Fe1 -172.2(19) . . . . ?
C15 N4 N5 C17 0(2) . . . . ?
Fe1 N4 N5 C17 -180.0(17) . . . . ?
C26 N6 N7 C28 -6(3) . . . . ?
C26 N6 N7 Fe1 -172.6(18) . . . . ?
C34 N9 N10 C36 2(3) . . . . ?
Fe1 N9 N10 C36 -169.5(16) . . . . ?
C24 O1 C1 C6 178(3) . . . . ?
C24 O1 C1 C2 -4(4) . . . . ?
C6 C1 C2 C3 3(5) . . . . ?
O1 C1 C2 C3 -175(3) . . . . ?
C1 C2 C3 C4 -3(5) . . . . ?
C2 C3 C4 C5 1(6) . . . . ?
C3 C4 C5 C6 2(4) . . . . ?
O1 C1 C6 C5 178(2) . . . . ?
C2 C1 C6 C5 -1(6) . . . . ?
O1 C1 C6 C7 -1(5) . . . . ?
C2 C1 C6 C7 -179(3) . . . . ?
C4 C5 C6 C1 -2(5) . . . . ?
C4 C5 C6 C7 177(3) . . . . ?
N2 N1 C7 C8 -1(3) . . . . ?
N2 N1 C7 C6 179(2) . . . . ?
C1 C6 C7 C8 168(3) . . . . ?
C5 C6 C7 C8 -11(4) . . . . ?
C1 C6 C7 N1 -12(5) . . . . ?
C5 C6 C7 N1 170(2) . . . . ?
N1 C7 C8 C9 -1(3) . . . . ?
C6 C7 C8 C9 180(3) . . . . ?
N1 N2 C9 C8 -2(3) . . . . ?
Fe1 N2 C9 C8 173.3(15) . . . . ?
N1 N2 C9 C10 -179(2) . . . . ?
Fe1 N2 C9 C10 -3(3) . . . . ?
C7 C8 C9 N2 2(3) . . . . ?
C7 C8 C9 C10 177(3) . . . . ?
C14 N3 C10 C9 -179(2) . . . . ?
Fe1 N3 C10 C9 5(3) . . . . ?
C14 N3 C10 C11 2(3) . . . . ?
Fe1 N3 C10 C11 -174.8(17) . . . . ?
N2 C9 C10 N3 -1(4) . . . . ?
C8 C9 C10 N3 -176(2) . . . . ?
N2 C9 C10 C11 178(2) . . . . ?
C8 C9 C10 C11 3(5) . . . . ?
N3 C10 C11 C12 0(4) . . . . ?
C9 C10 C11 C12 -179(2) . . . . ?
C10 C11 C12 C13 -2(4) . . . . ?
C11 C12 C13 C14 2(4) . . . . ?
C10 N3 C14 C13 -2(4) . . . . ?
Fe1 N3 C14 C13 174.4(18) . . . . ?
C10 N3 C14 C15 179(2) . . . . ?
Fe1 N3 C14 C15 -4(3) . . . . ?
C12 C13 C14 N3 0(4) . . . . ?
C12 C13 C14 C15 179(2) . . . . ?
N5 N4 C15 C16 0(3) . . . . ?
Fe1 N4 C15 C16 180.0(15) . . . . ?
N5 N4 C15 C14 177(2) . . . . ?
Fe1 N4 C15 C14 -4(3) . . . . ?
N3 C14 C15 N4 5(3) . . . . ?
C13 C14 C15 N4 -174(2) . . . . ?
N3 C14 C15 C16 -179(3) . . . . ?
C13 C14 C15 C16 2(5) . . . . ?
N4 C15 C16 C17 0(3) . . . . ?
C14 C15 C16 C17 -176(3) . . . . ?
N4 N5 C17 C16 0(3) . . . . ?
N4 N5 C17 C18 -178.5(19) . . . . ?
C15 C16 C17 N5 0(3) . . . . ?
C15 C16 C17 C18 178(2) . . . . ?
N5 C17 C18 C19 -170(2) . . . . ?
C16 C17 C18 C19 11(4) . . . . ?
N5 C17 C18 C23 19(4) . . . . ?
C16 C17 C18 C23 -160(3) . . . . ?
C23 C18 C19 C20 -7(4) . . . . ?
C17 C18 C19 C20 -178(2) . . . . ?
C18 C19 C20 C21 7(4) . . . . ?
C19 C20 C21 C22 -3(4) . . . . ?
C20 C21 C22 C23 0(4) . . . . ?
C25 O2 C23 C18 171(3) . . . . ?
C25 O2 C23 C22 -9(4) . . . . ?
C19 C18 C23 O2 -176(2) . . . . ?
C17 C18 C23 O2 -6(4) . . . . ?
C19 C18 C23 C22 4(4) . . . . ?
C17 C18 C23 C22 174(2) . . . . ?
C21 C22 C23 O2 180(2) . . . . ?
C21 C22 C23 C18 0(4) . . . . ?
N7 N6 C26 C27 8(3) . . . . ?
N6 C26 C27 C28 -7(3) . . . . ?
N6 N7 C28 C27 1(3) . . . . ?
Fe1 N7 C28 C27 171.4(15) . . . . ?
N6 N7 C28 C29 -177(2) . . . . ?
Fe1 N7 C28 C29 -7(3) . . . . ?
C26 C27 C28 N7 3(3) . . . . ?
C26 C27 C28 C29 -178(3) . . . . ?
C33 N8 C29 C30 -8(4) . . . . ?
Fe1 N8 C29 C30 177.6(18) . . . . ?
C33 N8 C29 C28 176(2) . . . . ?
Fe1 N8 C29 C28 2(3) . . . . ?
C31 C30 C29 N8 9(4) . . . . ?
C31 C30 C29 C28 -175(2) . . . . ?
N7 C28 C29 N8 4(3) . . . . ?
C27 C28 C29 N8 -174(3) . . . . ?
N7 C28 C29 C30 -172(2) . . . . ?
C27 C28 C29 C30 10(4) . . . . ?
C29 C30 C31 C32 -7(4) . . . . ?
C30 C31 C32 C33 4(4) . . . . ?
C29 N8 C33 C32 5(4) . . . . ?
Fe1 N8 C33 C32 179.3(16) . . . . ?
C29 N8 C33 C34 -180(2) . . . . ?
Fe1 N8 C33 C34 -6(3) . . . . ?
C31 C32 C33 N8 -3(4) . . . . ?
C31 C32 C33 C34 -178(2) . . . . ?
N10 N9 C34 C35 -5(3) . . . . ?
Fe1 N9 C34 C35 168.8(15) . . . . ?
N10 N9 C34 C33 -175(2) . . . . ?
Fe1 N9 C34 C33 -1(3) . . . . ?
N8 C33 C34 N9 4(3) . . . . ?
C32 C33 C34 N9 179(2) . . . . ?
N8 C33 C34 C35 -163(2) . . . . ?
C32 C33 C34 C35 12(4) . . . . ?
N9 C34 C35 C36 6(3) . . . . ?
C33 C34 C35 C36 174(3) . . . . ?
C34 C35 C36 N10 -4(3) . . . . ?
N9 N10 C36 C35 2(3) . . . . ?
C43 N11 N12 C45 -3(3) . . . . ?
C43 N11 N12 Fe2 -179.7(17) . . . . ?
C51 N14 N15 C53 0(3) . . . . ?
Fe2 N14 N15 C53 -172.8(18) . . . . ?
C62 N16 N17 C64 2(3) . . . . ?
C62 N16 N17 Fe2 -175.8(18) . . . . ?
C70 N19 N20 C72 -1(2) . . . . ?
Fe2 N19 N20 C72 -169.3(16) . . . . ?
C60 O3 C37 C42 171(2) . . . . ?
C60 O3 C37 C38 -9(4) . . . . ?
O3 C37 C38 C39 -178(3) . . . . ?
C42 C37 C38 C39 2(4) . . . . ?
C37 C38 C39 C40 -1(5) . . . . ?
C38 C39 C40 C41 0(4) . . . . ?
C39 C40 C41 C42 1(4) . . . . ?
C40 C41 C42 C37 0(4) . . . . ?
C40 C41 C42 C43 178(2) . . . . ?
O3 C37 C42 C41 179(2) . . . . ?
C38 C37 C42 C41 -1(4) . . . . ?
O3 C37 C42 C43 1(4) . . . . ?
C38 C37 C42 C43 -179(2) . . . . ?
N12 N11 C43 C44 1(3) . . . . ?
N12 N11 C43 C42 -173(2) . . . . ?
C41 C42 C43 N11 -174(2) . . . . ?
C37 C42 C43 N11 4(4) . . . . ?
C41 C42 C43 C44 14(4) . . . . ?
C37 C42 C43 C44 -169(3) . . . . ?
N11 C43 C44 C45 1(3) . . . . ?
C42 C43 C44 C45 175(3) . . . . ?
N11 N12 C45 C44 3(2) . . . . ?
Fe2 N12 C45 C44 -179.3(14) . . . . ?
N11 N12 C45 C46 178.5(18) . . . . ?
Fe2 N12 C45 C46 -4(3) . . . . ?
C43 C44 C45 N12 -2(3) . . . . ?
C43 C44 C45 C46 -176(3) . . . . ?
C50 N13 C46 C45 179(2) . . . . ?
Fe2 N13 C46 C45 -1(3) . . . . ?
C50 N13 C46 C47 1(4) . . . . ?
Fe2 N13 C46 C47 -179.4(17) . . . . ?
N12 C45 C46 N13 3(3) . . . . ?
C44 C45 C46 N13 176(3) . . . . ?
N12 C45 C46 C47 -179(2) . . . . ?
C44 C45 C46 C47 -5(5) . . . . ?
N13 C46 C47 C48 -4(4) . . . . ?
C45 C46 C47 C48 178(3) . . . . ?
C46 C47 C48 C49 5(4) . . . . ?
C47 C48 C49 C50 -4(5) . . . . ?
C46 N13 C50 C51 179(2) . . . . ?
Fe2 N13 C50 C51 -1(3) . . . . ?
C46 N13 C50 C49 0(4) . . . . ?
Fe2 N13 C50 C49 -179.4(18) . . . . ?
C48 C49 C50 N13 1(4) . . . . ?
C48 C49 C50 C51 -177(3) . . . . ?
N13 C50 C51 C52 -169(3) . . . . ?
C49 C50 C51 C52 9(6) . . . . ?
N13 C50 C51 N14 1(3) . . . . ?
C49 C50 C51 N14 179(3) . . . . ?
N15 N14 C51 C52 -2(3) . . . . ?
Fe2 N14 C51 C52 173.0(16) . . . . ?
N15 N14 C51 C50 -175(2) . . . . ?
Fe2 N14 C51 C50 0(3) . . . . ?
C50 C51 C52 C53 173(3) . . . . ?
N14 C51 C52 C53 3(3) . . . . ?
C51 C52 C53 N15 -3(3) . . . . ?
C51 C52 C53 C54 179(3) . . . . ?
N14 N15 C53 C52 2(3) . . . . ?
N14 N15 C53 C54 -180(2) . . . . ?
C52 C53 C54 C55 -23(4) . . . . ?
N15 C53 C54 C55 160(2) . . . . ?
C52 C53 C54 C59 145(3) . . . . ?
N15 C53 C54 C59 -33(4) . . . . ?
C59 C54 C55 C56 7(4) . . . . ?
C53 C54 C55 C56 176(2) . . . . ?
C54 C55 C56 C57 -4(4) . . . . ?
C55 C56 C57 C58 5(5) . . . . ?
C56 C57 C58 C59 -8(5) . . . . ?
C57 C58 C59 O4 -178(3) . . . . ?
C57 C58 C59 C54 10(5) . . . . ?
C61 O4 C59 C58 3(4) . . . . ?
C61 O4 C59 C54 175(2) . . . . ?
C55 C54 C59 C58 -10(4) . . . . ?
C53 C54 C59 C58 -177(3) . . . . ?
C55 C54 C59 O4 177(2) . . . . ?
C53 C54 C59 O4 9(4) . . . . ?
N17 N16 C62 C63 -6(3) . . . . ?
N16 C62 C63 C64 7(3) . . . . ?
N16 N17 C64 C65 -177(2) . . . . ?
Fe2 N17 C64 C65 1(3) . . . . ?
N16 N17 C64 C63 2(3) . . . . ?
Fe2 N17 C64 C63 -179.4(14) . . . . ?
C62 C63 C64 N17 -5(3) . . . . ?
C62 C63 C64 C65 174(3) . . . . ?
C69 N18 C65 C66 3(4) . . . . ?
Fe2 N18 C65 C66 -169.9(17) . . . . ?
C69 N18 C65 C64 179(2) . . . . ?
Fe2 N18 C65 C64 6(3) . . . . ?
N17 C64 C65 N18 -5(3) . . . . ?
C63 C64 C65 N18 176(2) . . . . ?
N17 C64 C65 C66 170(3) . . . . ?
C63 C64 C65 C66 -9(5) . . . . ?
N18 C65 C66 C67 -1(4) . . . . ?
C64 C65 C66 C67 -176(3) . . . . ?
C65 C66 C67 C68 -2(4) . . . . ?
C66 C67 C68 C69 2(4) . . . . ?
C65 N18 C69 C68 -3(4) . . . . ?
Fe2 N18 C69 C68 170.1(16) . . . . ?
C65 N18 C69 C70 176(2) . . . . ?
Fe2 N18 C69 C70 -11(3) . . . . ?
C67 C68 C69 N18 0(3) . . . . ?
C67 C68 C69 C70 -178(2) . . . . ?
N20 N19 C70 C71 2(3) . . . . ?
Fe2 N19 C70 C71 173.2(17) . . . . ?
N20 N19 C70 C69 -178.1(19) . . . . ?
Fe2 N19 C70 C69 -7(3) . . . . ?
N18 C69 C70 N19 11(3) . . . . ?
C68 C69 C70 N19 -170(2) . . . . ?
N18 C69 C70 C71 -169(3) . . . . ?
C68 C69 C70 C71 10(5) . . . . ?
N19 C70 C71 C72 -2(3) . . . . ?
C69 C70 C71 C72 178(3) . . . . ?
N19 N20 C72 C71 0(3) . . . . ?
C70 C71 C72 N20 1(3) . . . . ?

loop_
_geom_hbond_atom_site_label_D
_geom_hbond_atom_site_label_H
_geom_hbond_atom_site_label_A
_geom_hbond_distance_DH
_geom_hbond_distance_HA
_geom_hbond_distance_DA
_geom_hbond_angle_DHA
_geom_hbond_site_symmetry_A
N1 H1A O1 0.86 2.16 2.65(3) 116.0 .
N1 H1A O2_2 0.86 2.58 3.19(4) 129.3 3_676
N1 H1A O3_2 0.86 2.37 3.16(4) 153.2 3_676
N1 H1A O2_3 0.86 1.96 2.68(4) 139.7 3_676
N5 H5B O2 0.86 1.95 2.51(3) 121.5 .
N6 H6A Cl1_4 0.86 2.80 3.65(2) 168.2 3_576
N6 H6A O2_4 0.86 2.60 3.35(3) 145.1 3_576
N6 H6A O4_4 0.86 1.99 2.79(3) 152.9 3_576
N6 H6A O2_5 0.86 1.89 2.70(7) 155.8 3_576
N10 H10A Cl1_1 0.86 2.74 3.55(2) 157.2 3_676
N10 H10A O1_1 0.86 2.01 2.86(3) 170.7 3_676
N10 H10A O2_1 0.86 2.44 3.02(3) 125.6 3_676
C16 H16A O3_6 0.93 2.49 3.28(3) 143.0 4_576
C16 H16A O3_7 0.93 2.54 3.41(6) 155.8 4_576
C30 H30A O4_7 0.93 2.42 3.21(5) 142.1 3_576
C22 H22A O3_4 0.93 2.55 3.35(3) 143.3 4_586
C25 H25B O4_5 0.96 1.89 2.58(9) 126.3 4_586
C32 H32A O4_1 0.93 2.47 3.32(3) 152.4 4_586
N11 H11B O3 0.86 2.00 2.58(3) 123.2 .
N15 H15A O4 0.86 2.17 2.62(3) 112.2 .
N15 H15A Cl1_4 0.86 2.93 3.66(2) 144.0 .
N15 H15A O1_4 0.86 2.25 3.08(3) 161.5 .
N15 H15A O4_4 0.86 2.60 3.12(3) 119.9 .
N15 H15A O1_5 0.86 2.15 2.94(6) 152.6 .
N16 H16B Cl1_6 0.86 2.83 3.61(2) 150.7 .
N16 H16B O1_6 0.86 1.94 2.79(3) 178.0 .
N16 H16B Cl1_7 0.86 2.96 3.74(4) 152.3 .
N16 H16B O1_7 0.86 2.22 3.06(6) 163.1 .
N20 H20B Cl1_2 0.86 2.71 3.47(3) 149.4 .
N20 H20B O1_2 0.86 2.02 2.86(4) 163.4 .
N20 H20B O2_2 0.86 2.41 2.94(3) 120.4 .
N20 H20B Cl1_3 0.86 2.62 3.42(3) 155.6 .
N20 H20B O1_3 0.86 1.95 2.79(5) 166.8 .
C38 H38A O2_2 0.93 2.53 3.34(4) 144.6 4_575
C47 H47A O4_1 0.93 2.48 3.16(3) 130.1 2_645
C60 H60B O4_3 0.96 2.46 2.98(4) 113.9 4_575
C61 H61B O3_5 0.96 2.65 3.23(8) 119.8 .
C66 H66A O3_6 0.93 2.61 3.45(4) 150.9 2

_refine_diff_density_max         0.275
_refine_diff_density_min         -0.235
_refine_diff_density_rms         0.065


# start Validation Reply Form

_vrf_REFNR01_Stage3_Transient    
;
PROBLEM: Ratio of reflections to parameters is < 6 for a
RESPONSE: This is the intermediate in a conversion from low spin to high spin. 
This conversion requires the loss of a solvent molecule (acetone in this case)
and creates a horrible sample from a nearly perfect crystal.The diffraction of
the intermediate was not useable past 1.26A. This has resulted in very few
data per parameter.
;

_vrf_THETM01_Stage3_Transient    
;
PROBLEM: The value of sine(theta_max)/wavelength is less than 0.550
RESPONSE: As stated above, the data were poor to non-existent beyond 1.26\%A
;

_vrf_PLAT023_Stage3_Transient    
;
PROBLEM: Resolution (too) Low [sin(theta)/Lambda < 0.6]..      17.91 Degree
RESPONSE:  R(int)went higher than 30% and I/\s went lower than 2 at d=1.26\%A, 
so the data were cut at that point. 
;

_vrf_PLAT029_Stage3_Transient    
;
PROBLEM: _diffrn_measured_fraction_theta_full Low .......      0.694 Note  
RESPONSE: Due to the diffraction images containing diffraction from three 
crystallographic domains, there was a great deal of overlap. Any overlapped
reflections were omitted. This has led to low completeness. 
;

_vrf_PLAT088_Stage3_Transient    
;
PROBLEM: Poor Data / Parameter Ratio ....................       4.14 Note  
RESPONSE: As explained above.
;

_vrf_PLAT201_Stage3_Transient    
;
PROBLEM: Isotropic non-H Atoms in Main Residue(s) .......         74 Report
RESPONSE: To account for the low data/parameter ratio, light atoms were 
refined isotropically. 
;

_vrf_ABSMU01_Stage3_Transient    
;
PROBLEM: Calculation of _exptl_absorpt_correction_mu
                not performed for this radiation type.
RESPONSE: Absorption corrections were done with SADABS that takes
 the x-ray wavelengths from the raw data. PLATON does
 not calculate these corrections for synchrotron radiation data.
;

_vrf_PLAT984_Stage3_Transient    
;
PROBLEM: The element-f Deviates from the B&C-Value
RESPONSE: DISP values for each element type present were
 calculated for the 0.7749 angstrom x-rays using XDISP
 implemented in winGX, and using the Brennan model.
;
####################################################################### 
# 
# 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_Stage3_Final
_database_code_depnum_ccdc_archive 'CCDC 1053057'
_audit_update_record             
;
2015-12-22 deposited with the CCDC.
2016-01-05 downloaded from the CCDC.
;

_audit_creation_method           SHELXL-2014/7
_shelx_SHELXL_version_number     2014/7
_chemical_name_systematic        ?
_chemical_name_common            ?
_chemical_melting_point          ?
_chemical_formula_moiety         'C36 H30 N10 Fe, C3 H6 O, (Cl O4)2'
_chemical_formula_sum            'C39 H36 Cl2 Fe N10 O11'
_chemical_formula_weight         947.53

loop_
_atom_type_symbol
_atom_type_description
_atom_type_scat_dispersion_real
_atom_type_scat_dispersion_imag
_atom_type_scat_source
C C -0.0020 0.0020
'WCROMER Program in WinGX L.Kissel & R.H.Pratt Acta Cryst A46 170 1990'
H H 0.0000 0.0000
'WCROMER Program in WinGX L.Kissel & R.H.Pratt Acta Cryst A46 170 1990'
N N -0.0031 0.0040
'WCROMER Program in WinGX L.Kissel & R.H.Pratt Acta Cryst A46 170 1990'
O O -0.0041 0.0074
'WCROMER Program in WinGX L.Kissel & R.H.Pratt Acta Cryst A46 170 1990'
Cl Cl 0.1408 0.1896
'WCROMER Program in WinGX L.Kissel & R.H.Pratt Acta Cryst A46 170 1990'
Fe Fe 0.2064 0.9930
'WCROMER Program in WinGX L.Kissel & R.H.Pratt Acta Cryst A46 170 1990'

_space_group_crystal_system      triclinic
_space_group_IT_number           2
_space_group_name_H-M_alt        'P -1'
_space_group_name_Hall           '-P 1'

_shelx_space_group_comment       
;
The symmetry employed for this shelxl refinement is uniquely defined
by the following loop, which should always be used as a source of
symmetry information in preference to the above space-group names.
They are only intended as comments.
;

loop_
_space_group_symop_operation_xyz
'x, y, z'
'-x, -y, -z'

_cell_length_a                   13.0297(8)
_cell_length_b                   13.2995(9)
_cell_length_c                   14.0177(9)
_cell_angle_alpha                71.801(5)
_cell_angle_beta                 69.822(4)
_cell_angle_gamma                70.752(4)
_cell_volume                     2097.8(3)
_cell_formula_units_Z            2
_cell_measurement_temperature    250(2)
_cell_measurement_reflns_used    4773
_cell_measurement_theta_min      2.26
_cell_measurement_theta_max      25.38

_exptl_crystal_description       block
_exptl_crystal_colour            orange
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    ?
_exptl_crystal_density_diffrn    1.500
_exptl_crystal_F_000             976
_exptl_transmission_factor_min   ?
_exptl_transmission_factor_max   ?
_exptl_crystal_size_max          0.500
_exptl_crystal_size_mid          0.400
_exptl_crystal_size_min          0.300
_exptl_absorpt_coefficient_mu    0.702
_shelx_estimated_absorpt_T_min   0.720
_shelx_estimated_absorpt_T_max   0.817
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_correction_T_min  0.542430
_exptl_absorpt_correction_T_max  0.745232
_exptl_absorpt_process_details   'TWINABS 2012/1  (Sheldrick, 2012)'

_diffrn_ambient_temperature      250(2)
_diffrn_radiation_wavelength     0.7749
_diffrn_radiation_type           synchrotron
_diffrn_radiation_source         'Advanced Light Source Beamline 11.3.1'
_diffrn_radiation_monochromator  silicon(111)
_diffrn_measurement_device_type  'Bruker Apex2'
_diffrn_measurement_method       ω
_diffrn_detector_area_resol_mean 8.3
_diffrn_reflns_number            2709
_diffrn_reflns_av_unetI/netI     0.0451
_diffrn_reflns_av_R_equivalents  ?
_diffrn_reflns_limit_h_min       -10
_diffrn_reflns_limit_h_max       11
_diffrn_reflns_limit_k_min       -11
_diffrn_reflns_limit_k_max       11
_diffrn_reflns_limit_l_min       0
_diffrn_reflns_limit_l_max       12
_diffrn_reflns_theta_min         2.210
_diffrn_reflns_theta_max         20.425
_diffrn_reflns_theta_full        20.425
_diffrn_measured_fraction_theta_max 0.927
_diffrn_measured_fraction_theta_full 0.927
_diffrn_reflns_Laue_measured_fraction_max 0.927
_diffrn_reflns_Laue_measured_fraction_full 0.927
_diffrn_reflns_point_group_measured_fraction_max 0.927
_diffrn_reflns_point_group_measured_fraction_full 0.927
_reflns_number_total             2709
_reflns_number_gt                2265
_reflns_threshold_expression     'I > 2σ(I)'
_reflns_Friedel_coverage         0.000
_reflns_Friedel_fraction_max     .
_reflns_Friedel_fraction_full    .

_reflns_special_details          
;
 _reflns_Friedel_fraction is defined as the number of unique
 Friedel pairs measured divided by the number that would be
 possible theoretically, ignoring centric projections and
 systematic absences.


The images contain diffraction patterens from two samples: the low spin/high
spin mixed Transient and the high spin final product (which is twinned)
which is shown in this file.  The two neccesary unit cells and three 
orientation matrices were determined using CELL_NOW and RLATT, and manually
 combined into an orientation matrix file (*.p4p).To seperate the reflections,
 the SAINT integration engine was used in command line mode, and set up with a
 sample mask. An example is shown below:
SMAP=1, 1, 2
This indicates that the first two orientation matrices belong to sample 1, and 
the third belongs to sample 2.  For all commands relating to cell or symmetry 
later on, comma-delimited lists were used to specify distinct parameters.
Listed below are most of the pertinent SAINT commands in an example from the 
SAINT manual:

FILTPOINTGP=-1, 2/m  //indicating sample 1 is triclinic and 2 is monoclinic
CRYST_SYS=1,3
PAR_MASK=TPS2, TP	//restaining the  twinned cells to be similar
GPAR_MASK=TPS2, TP    //and also restraining Detector pitch and xtal trans

 explained in the SAINT manual as
"Two-sample integration, where first sample is a two-component
twin and second component is a single crystal.  In the first sample,
constrain cell constants of the second component to those of the
first.  For both samples, constrain crystal translations and
 detector pitch"


In this case, the SAINT commands used were as follows: 
SMAP=1, 1, 2
CRYST_SYS=1, 3
PAR_MASK=TPS2, TP
GPAR_MASK=TPS2, TP 

This integration yielded three reflection files; one HKLF4 and one HKLF5
;

_computing_data_collection       'Apex2 v2012.10-0 (Bruker, 2012)'
_computing_cell_refinement       'SAINT V8.27B(Bruker, 2012)'
_computing_data_reduction        SAINT
_computing_structure_solution    SHELXS
_computing_structure_refinement  'SHELXL-2014/7 (Sheldrick, 2014)'
_computing_molecular_graphics    
;
     	SHELXTL 5.1, XP (Sheldrick, 1994)
	ShelXle Rev 699 (Hubschle, 2011)
;
_computing_publication_material  SHELXL-2014/7
_refine_special_details          
;
 Refined as a 2-component twin.

All hydrogens were assigned geometrically and refined as riding, with 
U(H) = 1.2*U(C) for secondary and aromatic carbons, and 
U(H) = 1.5*U(C) for terminal carbons. The hydrogens on N1, N5 N6 and N10 
were found in the difference map first, then affixed geometrically, with 
U(H) = 1.2*U(N)


This stucture contains two disordered perchlorate anions.The disordered 
perchlorates were modeled as split sites, using the 
following restraints:

SADI_ClO4 0.01 Cl1 O1 Cl1 O2 Cl1 O3 Cl1 O4
SADI_ClO4 0.02 O1 O2 O1 O3 O1 O4 O2 O3 O2 O4 O3 O4

A RIGU was employed.

;
_refine_ls_structure_factor_coef Fsqd
_refine_ls_matrix_type           full
_refine_ls_weighting_scheme      calc
_refine_ls_weighting_details     
'w=1/[σ²(Fo²)+(0.1912P)²+14.0134P] where P=(Fo²+2Fc²)/3'
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_atom_sites_solution_hydrogens   geom
_refine_ls_hydrogen_treatment    constr
_refine_ls_extinction_method     none
_refine_ls_extinction_coef       .
_refine_ls_number_reflns         2709
_refine_ls_number_parameters     563
_refine_ls_number_restraints     897
_refine_ls_R_factor_all          0.1228
_refine_ls_R_factor_gt           0.1052
_refine_ls_wR_factor_ref         0.3116
_refine_ls_wR_factor_gt          0.2974
_refine_ls_goodness_of_fit_ref   1.174
_refine_ls_restrained_S_all      1.019
_refine_ls_shift/su_max          0.000
_refine_ls_shift/su_mean         0.000

loop_
_atom_site_label
_atom_site_type_symbol
_atom_site_fract_x
_atom_site_fract_y
_atom_site_fract_z
_atom_site_U_iso_or_equiv
_atom_site_adp_type
_atom_site_occupancy
_atom_site_site_symmetry_order
_atom_site_calc_flag
_atom_site_refinement_flags_posn
_atom_site_refinement_flags_adp
_atom_site_refinement_flags_occupancy
_atom_site_disorder_assembly
_atom_site_disorder_group
Fe1 Fe 0.4980(2) 0.7520(2) 0.2493(2) 0.0535(11) Uani 1 1 d . U . . .
O1 O 0.1312(13) 0.9146(13) 0.7015(13) 0.093(5) Uani 1 1 d . U . . .
O2 O 0.8348(11) 0.6385(14) -0.1026(11) 0.084(5) Uani 1 1 d . U . . .
N1 N 0.2513(13) 0.8127(13) 0.4293(13) 0.064(4) Uani 1 1 d . U . . .
H1D H 0.2087 0.7948 0.4045 0.077 Uiso 1 1 calc R U . . .
N2 N 0.3584(12) 0.8035(12) 0.3817(12) 0.054(4) Uani 1 1 d . U . . .
N3 N 0.5700(14) 0.8066(12) 0.3288(13) 0.058(4) Uani 1 1 d . U . . .
N4 N 0.6744(12) 0.7373(11) 0.1580(11) 0.045(3) Uani 1 1 d . U . . .
N5 N 0.7497(12) 0.6991(12) 0.0756(12) 0.057(4) Uani 1 1 d . U . . .
H5B H 0.7305 0.6768 0.0336 0.068 Uiso 1 1 calc R U . . .
N6 N 0.3914(14) 0.9910(14) 0.1156(13) 0.070(4) Uani 1 1 d . U . . .
H6B H 0.4092 1.0319 0.1421 0.084 Uiso 1 1 calc R U . . .
N7 N 0.4201(12) 0.8822(13) 0.1409(12) 0.053(4) Uani 1 1 d . U . . .
N8 N 0.4426(12) 0.6713(14) 0.1720(13) 0.057(4) Uani 1 1 d . U . . .
N9 N 0.5427(12) 0.5794(12) 0.3191(12) 0.054(3) Uani 1 1 d . U . . .
N10 N 0.5969(12) 0.5137(13) 0.3863(12) 0.058(4) Uani 1 1 d . U . . .
H10A H 0.6216 0.5360 0.4244 0.070 Uiso 1 1 calc R U . . .
C1 C 0.103(3) 0.936(3) 0.809(2) 0.130(10) Uani 1 1 d . U . . .
H1A H 0.1611 0.8889 0.8428 0.195 Uiso 1 1 calc R U . . .
H1B H 0.0307 0.9216 0.8500 0.195 Uiso 1 1 calc R U . . .
H1C H 0.1002 1.0120 0.8018 0.195 Uiso 1 1 calc R U . . .
C2 C -0.061(2) 0.918(2) 0.725(2) 0.101(8) Uani 1 1 d . U . . .
H2A H -0.0885 0.9421 0.7878 0.121 Uiso 1 1 calc R U . . .
C3 C 0.050(2) 0.9001(19) 0.6728(18) 0.079(6) Uani 1 1 d . U . . .
C4 C -0.131(2) 0.900(2) 0.683(2) 0.091(7) Uani 1 1 d . U . . .
H4A H -0.2087 0.9134 0.7169 0.109 Uiso 1 1 calc R U . . .
C5 C -0.0953(19) 0.865(2) 0.595(2) 0.094(7) Uani 1 1 d . U . . .
H5A H -0.1464 0.8510 0.5695 0.113 Uiso 1 1 calc R U . . .
C6 C 0.0178(17) 0.8484(17) 0.5404(18) 0.073(6) Uani 1 1 d . U . . .
H6A H 0.0434 0.8233 0.4785 0.087 Uiso 1 1 calc R U . . .
C7 C 0.0931(17) 0.8687(17) 0.5766(17) 0.069(5) Uani 1 1 d . U . . .
C8 C 0.2101(17) 0.8484(16) 0.5128(17) 0.058(5) Uani 1 1 d . U . . .
C9 C 0.3023(16) 0.8734(16) 0.5243(16) 0.063(5) Uani 1 1 d . U . . .
H9A H 0.3012 0.9062 0.5752 0.075 Uiso 1 1 calc R U . . .
C10 C 0.3942(16) 0.8394(14) 0.4450(15) 0.052(4) Uani 1 1 d . U . . .
C11 C 0.5070(17) 0.8418(16) 0.4135(17) 0.062(5) Uani 1 1 d . U . . .
C12 C 0.5578(17) 0.8701(15) 0.4748(17) 0.062(5) Uani 1 1 d . U . . .
H12A H 0.5171 0.8861 0.5404 0.075 Uiso 1 1 calc R U . . .
C13 C 0.6666(18) 0.8721(17) 0.4327(18) 0.075(6) Uani 1 1 d . U . . .
H13A H 0.6997 0.8971 0.4679 0.089 Uiso 1 1 calc R U . . .
C14 C 0.7297(18) 0.8419(15) 0.3468(17) 0.063(5) Uani 1 1 d . U . . .
H14A H 0.8064 0.8426 0.3226 0.075 Uiso 1 1 calc R U . . .
C15 C 0.6807(16) 0.8083(16) 0.2910(16) 0.056(5) Uani 1 1 d . U . . .
C16 C 0.7399(16) 0.7687(15) 0.1955(16) 0.052(5) Uani 1 1 d . U . . .
C17 C 0.8499(16) 0.7454(16) 0.1445(16) 0.063(6) Uani 1 1 d . U . . .
H17A H 0.9099 0.7573 0.1587 0.076 Uiso 1 1 calc R U . . .
C18 C 0.8551(15) 0.6983(15) 0.0637(15) 0.052(5) Uani 1 1 d . U . . .
C19 C 0.9554(17) 0.6587(18) -0.0214(17) 0.066(6) Uani 1 1 d . U . . .
C20 C 1.0609(16) 0.6548(17) -0.0185(17) 0.067(6) Uani 1 1 d . U . . .
H20A H 1.0679 0.6767 0.0361 0.081 Uiso 1 1 calc R U . . .
C21 C 1.1559(18) 0.620(2) -0.0926(19) 0.085(7) Uani 1 1 d . U . . .
H21A H 1.2275 0.6185 -0.0899 0.102 Uiso 1 1 calc R U . . .
C22 C 1.144(2) 0.587(2) -0.174(2) 0.097(8) Uani 1 1 d . U . . .
H22A H 1.2065 0.5594 -0.2253 0.117 Uiso 1 1 calc R U . . .
C23 C 1.0407(19) 0.5951(19) -0.1740(18) 0.085(6) Uani 1 1 d . U . . .
H23A H 1.0305 0.5791 -0.2305 0.102 Uiso 1 1 calc R U . . .
C24 C 0.9452(17) 0.6266(17) -0.0947(17) 0.065(5) Uani 1 1 d . U . . .
C25 C 0.821(2) 0.617(2) -0.1912(18) 0.100(9) Uani 1 1 d . U . . .
H25A H 0.7447 0.6102 -0.1757 0.150 Uiso 1 1 calc R U . . .
H25B H 0.8746 0.5503 -0.2070 0.150 Uiso 1 1 calc R U . . .
H25C H 0.8335 0.6776 -0.2509 0.150 Uiso 1 1 calc R U . . .
C26 C 0.3324(17) 1.030(2) 0.0452(17) 0.070(5) Uani 1 1 d . U . . .
H26A H 0.3070 1.1041 0.0140 0.084 Uiso 1 1 calc R U . . .
C27 C 0.3159(16) 0.9423(18) 0.0274(16) 0.064(5) Uani 1 1 d . U . . .
H27A H 0.2734 0.9426 -0.0149 0.077 Uiso 1 1 calc R U . . .
C28 C 0.3750(16) 0.8539(18) 0.0849(17) 0.063(5) Uani 1 1 d . U . . .
C29 C 0.3848(15) 0.7393(17) 0.1001(16) 0.061(4) Uani 1 1 d . U . . .
C30 C 0.3479(19) 0.687(2) 0.0475(19) 0.084(6) Uani 1 1 d . U . . .
H30A H 0.3085 0.7283 -0.0027 0.101 Uiso 1 1 calc R U . . .
C31 C 0.3701(19) 0.582(2) 0.071(2) 0.088(6) Uani 1 1 d . U . . .
H31A H 0.3452 0.5497 0.0350 0.105 Uiso 1 1 calc R U . . .
C32 C 0.4244(18) 0.5147(19) 0.1401(19) 0.082(6) Uani 1 1 d . U . . .
H32A H 0.4407 0.4384 0.1505 0.099 Uiso 1 1 calc R U . . .
C33 C 0.4568(17) 0.5650(18) 0.1979(17) 0.065(5) Uani 1 1 d . U . . .
C34 C 0.5158(14) 0.5117(15) 0.2730(15) 0.051(4) Uani 1 1 d . U . . .
C35 C 0.5609(16) 0.4027(17) 0.3179(17) 0.068(5) Uani 1 1 d . U . . .
H35A H 0.5594 0.3386 0.3040 0.082 Uiso 1 1 calc R U . . .
C36 C 0.6101(17) 0.4133(18) 0.3904(18) 0.066(5) Uani 1 1 d . U . . .
H36A H 0.6468 0.3543 0.4347 0.079 Uiso 1 1 calc R U . . .
Cl1_1 Cl 0.4735(7) 1.1638(7) 0.2219(7) 0.038(7) Uiso 0.54(5) 1 d D . P A 1
O1_1 O 0.567(2) 1.201(3) 0.208(3) 0.19(3) Uiso 0.54(5) 1 d D . P A 1
O2_1 O 0.431(4) 1.214(3) 0.134(2) 0.22(5) Uiso 0.54(5) 1 d D . P A 1
O3_1 O 0.389(2) 1.190(4) 0.310(2) 0.17(2) Uiso 0.54(5) 1 d D . P A 1
O4_1 O 0.504(3) 1.0510(12) 0.231(3) 0.130(17) Uiso 0.54(5) 1 d D . P A 1
Cl1_2 Cl 0.0898(11) 0.7394(18) 0.2631(16) 0.089(6) Uiso 0.58(4) 1 d D . P B 1
O1_2 O 0.1823(18) 0.745(3) 0.289(3) 0.152(16) Uiso 0.58(4) 1 d D . P B 1
O2_2 O 0.083(2) 0.806(2) 0.166(2) 0.103(13) Uiso 0.58(4) 1 d D . P B 1
O3_2 O 0.099(3) 0.631(2) 0.265(3) 0.144(19) Uiso 0.58(4) 1 d D . P B 1
O4_2 O -0.0085(16) 0.775(3) 0.339(2) 0.113(12) Uiso 0.58(4) 1 d D . P B 1
Cl1_4 Cl 0.0888(12) 0.7122(15) 0.2916(17) 0.058(7) Uiso 0.42(4) 1 d D . P B 2
O1_4 O 0.1878(16) 0.679(3) 0.323(2) 0.061(13) Uiso 0.42(4) 1 d D . P B 2
O2_4 O 0.074(4) 0.821(2) 0.236(5) 0.25(4) Uiso 0.42(4) 1 d D . P B 2
O3_4 O 0.097(3) 0.647(4) 0.227(3) 0.19(4) Uiso 0.42(4) 1 d D . P B 2
O4_4 O -0.0035(18) 0.703(4) 0.379(2) 0.094(16) Uiso 0.42(4) 1 d D . P B 2
Cl1_3 Cl 0.469(2) 1.168(2) 0.229(2) 0.29(4) Uiso 0.46(5) 1 d D . P A 2
O1_3 O 0.433(5) 1.076(3) 0.294(4) 0.21(3) Uiso 0.46(5) 1 d D . P A 2
O2_3 O 0.441(3) 1.195(3) 0.136(2) 0.080(19) Uiso 0.46(5) 1 d D . P A 2
O3_3 O 0.586(2) 1.146(5) 0.210(4) 0.20(3) Uiso 0.46(5) 1 d D . P A 2
O4_3 O 0.417(3) 1.255(3) 0.279(3) 0.12(2) Uiso 0.46(5) 1 d D . P A 2
C39 C 0.809(2) 0.597(2) 0.570(2) 0.100(8) Uani 1 1 d . U . . .
H39A H 0.8900 0.5722 0.5571 0.151 Uiso 1 1 calc R U . . .
H39B H 0.7862 0.6763 0.5587 0.151 Uiso 1 1 calc R U . . .
H39C H 0.7728 0.5651 0.6408 0.151 Uiso 1 1 calc R U . . .
C37 C 0.8646(19) 0.496(2) 0.441(2) 0.114(10) Uani 1 1 d . U . . .
H37A H 0.9366 0.4883 0.4515 0.171 Uiso 1 1 calc R U . . .
H37B H 0.8488 0.4245 0.4609 0.171 Uiso 1 1 calc R U . . .
H37C H 0.8675 0.5269 0.3676 0.171 Uiso 1 1 calc R U . . .
C38 C 0.777(2) 0.567(2) 0.5030(19) 0.083(7) Uani 1 1 d . U . . .
O3 O 0.6795(13) 0.5868(15) 0.5004(13) 0.100(5) Uani 1 1 d . U . . .


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

loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
_geom_bond_publ_flag
Fe1 N3 2.080(16) . ?
Fe1 N7 2.145(16) . ?
Fe1 N9 2.162(16) . ?
Fe1 N8 2.149(16) . ?
Fe1 N4 2.189(14) . ?
Fe1 N2 2.206(15) . ?
O1 C3 1.35(3) . ?
O1 C1 1.51(3) . ?
O2 C24 1.43(2) . ?
O2 C25 1.44(2) . ?
N1 C8 1.28(2) . ?
N1 N2 1.305(19) . ?
N1 H1D 0.8700 . ?
N2 C10 1.39(2) . ?
N3 C11 1.31(2) . ?
N3 C15 1.36(2) . ?
N4 C16 1.36(2) . ?
N4 N5 1.345(19) . ?
N5 C18 1.32(2) . ?
N5 H5B 0.8700 . ?
N6 C26 1.33(2) . ?
N6 N7 1.33(2) . ?
N6 H6B 0.8700 . ?
N7 C28 1.32(2) . ?
N8 C33 1.31(2) . ?
N8 C29 1.38(2) . ?
N9 N10 1.299(19) . ?
N9 C34 1.44(2) . ?
N10 C36 1.28(2) . ?
N10 H10A 0.8700 . ?
C1 H1A 0.9700 . ?
C1 H1B 0.9700 . ?
C1 H1C 0.9700 . ?
C2 C4 1.36(3) . ?
C2 C3 1.35(3) . ?
C2 H2A 0.9400 . ?
C3 C7 1.41(3) . ?
C4 C5 1.34(3) . ?
C4 H4A 0.9400 . ?
C5 C6 1.38(3) . ?
C5 H5A 0.9400 . ?
C6 C7 1.38(3) . ?
C6 H6A 0.9400 . ?
C7 C8 1.46(3) . ?
C8 C9 1.42(3) . ?
C9 C10 1.38(3) . ?
C9 H9A 0.9400 . ?
C10 C11 1.39(3) . ?
C11 C12 1.44(3) . ?
C12 C13 1.34(3) . ?
C12 H12A 0.9400 . ?
C13 C14 1.30(3) . ?
C13 H13A 0.9400 . ?
C14 C15 1.40(3) . ?
C14 H14A 0.9400 . ?
C15 C16 1.46(3) . ?
C16 C17 1.34(3) . ?
C17 C18 1.43(3) . ?
C17 H17A 0.9400 . ?
C18 C19 1.51(3) . ?
C19 C24 1.29(3) . ?
C19 C20 1.37(3) . ?
C20 C21 1.36(3) . ?
C20 H20A 0.9400 . ?
C21 C22 1.42(3) . ?
C21 H21A 0.9400 . ?
C22 C23 1.31(3) . ?
C22 H22A 0.9400 . ?
C23 C24 1.40(3) . ?
C23 H23A 0.9400 . ?
C25 H25A 0.9700 . ?
C25 H25B 0.9700 . ?
C25 H25C 0.9700 . ?
C26 C27 1.36(3) . ?
C26 H26A 0.9400 . ?
C27 C28 1.36(3) . ?
C27 H27A 0.9400 . ?
C28 C29 1.44(3) . ?
C29 C30 1.43(3) . ?
C30 C31 1.29(3) . ?
C30 H30A 0.9400 . ?
C31 C32 1.33(3) . ?
C31 H31A 0.9400 . ?
C32 C33 1.43(3) . ?
C32 H32A 0.9400 . ?
C33 C34 1.39(3) . ?
C34 C35 1.40(3) . ?
C35 C36 1.43(3) . ?
C35 H35A 0.9400 . ?
C36 H36A 0.9400 . ?
Cl1_1 O1_1 1.392(12) . ?
Cl1_1 O4_1 1.394(12) . ?
Cl1_1 O3_1 1.397(12) . ?
Cl1_1 O2_1 1.402(12) . ?
Cl1_2 O2_2 1.385(12) . ?
Cl1_2 O3_2 1.397(12) . ?
Cl1_2 O1_2 1.399(12) . ?
Cl1_2 O4_2 1.407(12) . ?
Cl1_4 O3_4 1.397(12) . ?
Cl1_4 O1_4 1.396(12) . ?
Cl1_4 O4_4 1.397(12) . ?
Cl1_4 O2_4 1.399(12) . ?
Cl1_3 O3_3 1.395(12) . ?
Cl1_3 O4_3 1.397(12) . ?
Cl1_3 O2_3 1.397(12) . ?
Cl1_3 O1_3 1.398(12) . ?
C39 C38 1.35(3) . ?
C39 H39A 0.9700 . ?
C39 H39B 0.9700 . ?
C39 H39C 0.9700 . ?
C37 C38 1.44(3) . ?
C37 H37A 0.9700 . ?
C37 H37B 0.9700 . ?
C37 H37C 0.9700 . ?
C38 O3 1.22(3) . ?

loop_
_geom_angle_atom_site_label_1
_geom_angle_atom_site_label_2
_geom_angle_atom_site_label_3
_geom_angle
_geom_angle_site_symmetry_1
_geom_angle_site_symmetry_3
_geom_angle_publ_flag
N3 Fe1 N7 112.7(6) . . ?
N3 Fe1 N9 98.1(6) . . ?
N7 Fe1 N9 149.2(6) . . ?
N3 Fe1 N8 170.9(6) . . ?
N7 Fe1 N8 75.6(7) . . ?
N9 Fe1 N8 73.6(7) . . ?
N3 Fe1 N4 74.9(6) . . ?
N7 Fe1 N4 98.7(5) . . ?
N9 Fe1 N4 88.4(5) . . ?
N8 Fe1 N4 100.7(6) . . ?
N3 Fe1 N2 74.9(6) . . ?
N7 Fe1 N2 90.9(6) . . ?
N9 Fe1 N2 98.1(5) . . ?
N8 Fe1 N2 109.6(6) . . ?
N4 Fe1 N2 149.6(6) . . ?
C3 O1 C1 118.7(19) . . ?
C24 O2 C25 120.7(16) . . ?
C8 N1 N2 118.9(18) . . ?
C8 N1 H1D 120.5 . . ?
N2 N1 H1D 120.5 . . ?
N1 N2 C10 102.3(15) . . ?
N1 N2 Fe1 145.6(13) . . ?
C10 N2 Fe1 112.1(11) . . ?
C11 N3 C15 120.8(17) . . ?
C11 N3 Fe1 119.5(14) . . ?
C15 N3 Fe1 119.7(13) . . ?
C16 N4 N5 102.2(15) . . ?
C16 N4 Fe1 116.0(12) . . ?
N5 N4 Fe1 141.6(12) . . ?
C18 N5 N4 114.5(16) . . ?
C18 N5 H5B 122.7 . . ?
N4 N5 H5B 122.7 . . ?
C26 N6 N7 113(2) . . ?
C26 N6 H6B 123.7 . . ?
N7 N6 H6B 123.7 . . ?
C28 N7 N6 103.8(18) . . ?
C28 N7 Fe1 116.5(14) . . ?
N6 N7 Fe1 139.4(14) . . ?
C33 N8 C29 123.1(18) . . ?
C33 N8 Fe1 121.2(16) . . ?
C29 N8 Fe1 115.6(13) . . ?
N10 N9 C34 106.8(15) . . ?
N10 N9 Fe1 139.0(13) . . ?
C34 N9 Fe1 113.9(12) . . ?
C36 N10 N9 113(2) . . ?
C36 N10 H10A 123.6 . . ?
N9 N10 H10A 123.6 . . ?
O1 C1 H1A 109.5 . . ?
O1 C1 H1B 109.5 . . ?
H1A C1 H1B 109.5 . . ?
O1 C1 H1C 109.5 . . ?
H1A C1 H1C 109.5 . . ?
H1B C1 H1C 109.5 . . ?
C4 C2 C3 117(2) . . ?
C4 C2 H2A 121.7 . . ?
C3 C2 H2A 121.7 . . ?
O1 C3 C2 125(2) . . ?
O1 C3 C7 111(2) . . ?
C2 C3 C7 123(2) . . ?
C5 C4 C2 123(2) . . ?
C5 C4 H4A 118.3 . . ?
C2 C4 H4A 118.3 . . ?
C4 C5 C6 120(2) . . ?
C4 C5 H5A 120.2 . . ?
C6 C5 H5A 120.2 . . ?
C7 C6 C5 120(2) . . ?
C7 C6 H6A 119.8 . . ?
C5 C6 H6A 119.8 . . ?
C3 C7 C6 116(2) . . ?
C3 C7 C8 128(2) . . ?
C6 C7 C8 115(2) . . ?
N1 C8 C9 103.8(18) . . ?
N1 C8 C7 128(2) . . ?
C9 C8 C7 128(2) . . ?
C10 C9 C8 105.6(19) . . ?
C10 C9 H9A 127.2 . . ?
C8 C9 H9A 127.2 . . ?
N2 C10 C9 109.1(17) . . ?
N2 C10 C11 116.7(17) . . ?
C9 C10 C11 134(2) . . ?
N3 C11 C10 117(2) . . ?
N3 C11 C12 120.1(19) . . ?
C10 C11 C12 122.8(19) . . ?
C13 C12 C11 116(2) . . ?
C13 C12 H12A 122.0 . . ?
C11 C12 H12A 122.0 . . ?
C14 C13 C12 125(2) . . ?
C14 C13 H13A 117.6 . . ?
C12 C13 H13A 117.6 . . ?
C13 C14 C15 118(2) . . ?
C13 C14 H14A 120.8 . . ?
C15 C14 H14A 120.8 . . ?
N3 C15 C14 119.5(18) . . ?
N3 C15 C16 115.0(18) . . ?
C14 C15 C16 125.5(19) . . ?
N4 C16 C17 113.6(18) . . ?
N4 C16 C15 114.4(17) . . ?
C17 C16 C15 131.4(19) . . ?
C16 C17 C18 104.2(17) . . ?
C16 C17 H17A 127.9 . . ?
C18 C17 H17A 127.9 . . ?
N5 C18 C17 105.3(16) . . ?
N5 C18 C19 125.1(18) . . ?
C17 C18 C19 129.5(17) . . ?
C24 C19 C20 120(2) . . ?
C24 C19 C18 122.3(19) . . ?
C20 C19 C18 118(2) . . ?
C21 C20 C19 122(2) . . ?
C21 C20 H20A 119.1 . . ?
C19 C20 H20A 119.1 . . ?
C20 C21 C22 118(2) . . ?
C20 C21 H21A 120.9 . . ?
C22 C21 H21A 120.9 . . ?
C23 C22 C21 117(2) . . ?
C23 C22 H22A 121.4 . . ?
C21 C22 H22A 121.4 . . ?
C22 C23 C24 123(2) . . ?
C22 C23 H23A 118.3 . . ?
C24 C23 H23A 118.3 . . ?
C19 C24 C23 120(2) . . ?
C19 C24 O2 119.5(19) . . ?
C23 C24 O2 120(2) . . ?
O2 C25 H25A 109.5 . . ?
O2 C25 H25B 109.5 . . ?
H25A C25 H25B 109.5 . . ?
O2 C25 H25C 109.5 . . ?
H25A C25 H25C 109.5 . . ?
H25B C25 H25C 109.5 . . ?
N6 C26 C27 107(2) . . ?
N6 C26 H26A 126.7 . . ?
C27 C26 H26A 126.7 . . ?
C26 C27 C28 105(2) . . ?
C26 C27 H27A 127.7 . . ?
C28 C27 H27A 127.7 . . ?
N7 C28 C27 112(2) . . ?
N7 C28 C29 118(2) . . ?
C27 C28 C29 130(2) . . ?
N8 C29 C30 116.3(19) . . ?
N8 C29 C28 114.8(19) . . ?
C30 C29 C28 129(2) . . ?
C31 C30 C29 118(2) . . ?
C31 C30 H30A 120.9 . . ?
C29 C30 H30A 120.9 . . ?
C30 C31 C32 127(3) . . ?
C30 C31 H31A 116.5 . . ?
C32 C31 H31A 116.5 . . ?
C31 C32 C33 116(2) . . ?
C31 C32 H32A 122.0 . . ?
C33 C32 H32A 122.0 . . ?
N8 C33 C32 119(2) . . ?
N8 C33 C34 114(2) . . ?
C32 C33 C34 127(2) . . ?
C35 C34 C33 136(2) . . ?
C35 C34 N9 107.1(18) . . ?
C33 C34 N9 117.0(17) . . ?
C36 C35 C34 102.8(19) . . ?
C36 C35 H35A 128.6 . . ?
C34 C35 H35A 128.6 . . ?
N10 C36 C35 111(2) . . ?
N10 C36 H36A 124.7 . . ?
C35 C36 H36A 124.7 . . ?
O1_1 Cl1_1 O4_1 110.3(10) . . ?
O1_1 Cl1_1 O3_1 110.5(10) . . ?
O4_1 Cl1_1 O3_1 109.9(10) . . ?
O1_1 Cl1_1 O2_1 108.9(10) . . ?
O4_1 Cl1_1 O2_1 108.6(10) . . ?
O3_1 Cl1_1 O2_1 108.6(10) . . ?
O2_2 Cl1_2 O3_2 110.5(10) . . ?
O2_2 Cl1_2 O1_2 110.8(10) . . ?
O3_2 Cl1_2 O1_2 109.6(10) . . ?
O2_2 Cl1_2 O4_2 109.5(10) . . ?
O3_2 Cl1_2 O4_2 108.5(10) . . ?
O1_2 Cl1_2 O4_2 107.9(10) . . ?
O3_4 Cl1_4 O1_4 109.5(10) . . ?
O3_4 Cl1_4 O4_4 109.9(10) . . ?
O1_4 Cl1_4 O4_4 109.8(10) . . ?
O3_4 Cl1_4 O2_4 109.0(10) . . ?
O1_4 Cl1_4 O2_4 109.3(10) . . ?
O4_4 Cl1_4 O2_4 109.3(10) . . ?
O3_3 Cl1_3 O4_3 109.9(10) . . ?
O3_3 Cl1_3 O2_3 109.8(10) . . ?
O4_3 Cl1_3 O2_3 109.6(10) . . ?
O3_3 Cl1_3 O1_3 109.2(11) . . ?
O4_3 Cl1_3 O1_3 109.1(10) . . ?
O2_3 Cl1_3 O1_3 109.3(10) . . ?
C38 C39 H39A 109.5 . . ?
C38 C39 H39B 109.5 . . ?
H39A C39 H39B 109.5 . . ?
C38 C39 H39C 109.5 . . ?
H39A C39 H39C 109.5 . . ?
H39B C39 H39C 109.5 . . ?
C38 C37 H37A 109.5 . . ?
C38 C37 H37B 109.5 . . ?
H37A C37 H37B 109.5 . . ?
C38 C37 H37C 109.5 . . ?
H37A C37 H37C 109.5 . . ?
H37B C37 H37C 109.5 . . ?
O3 C38 C39 124(2) . . ?
O3 C38 C37 120(2) . . ?
C39 C38 C37 115(2) . . ?

loop_
_geom_hbond_atom_site_label_D
_geom_hbond_atom_site_label_H
_geom_hbond_atom_site_label_A
_geom_hbond_distance_DH
_geom_hbond_distance_HA
_geom_hbond_distance_DA
_geom_hbond_angle_DHA
_geom_hbond_site_symmetry_A
N1 H1D O1_2 0.87 2.10 2.89(3) 151.6 .
N1 H1D O1_4 0.87 2.31 3.08(3) 148.9 .
N5 H5B O2 0.87 2.03 2.62(2) 124.7 .
N6 H6B Cl1_1 0.87 2.80 3.67(2) 178.0 .
N6 H6B O2_1 0.87 2.50 3.28(5) 149.5 .
N6 H6B O4_1 0.87 2.16 2.95(4) 150.6 .
N6 H6B Cl1_3 0.87 2.89 3.76(3) 179.7 .
N6 H6B O1_3 0.87 2.51 3.30(6) 151.3 .
N6 H6B O2_3 0.87 2.30 3.10(4) 151.4 .
N10 H10A O3 0.87 1.87 2.74(2) 177.2 .
C25 H25A O2_1 0.97 2.73 3.30(5) 118.3 2_675
C25 H25A O2_3 0.97 2.95 3.50(5) 116.6 2_675
C25 H25A O4_3 0.97 2.78 3.44(5) 125.9 2_675
C26 H26A N4 0.94 2.66 3.49(3) 147.4 2_675
C26 H26A N5 0.94 2.51 3.45(3) 176.8 2_675

_refine_diff_density_max         0.482
_refine_diff_density_min         -0.489
_refine_diff_density_rms         0.116


# start Validation Reply Form

_vrf_REFNR01_Stage3_Final        
;
PROBLEM: Ratio of reflections to parameters is < 6 for a
RESPONSE: Due to the deletion of overlapped reflections,
the number of data is low. Measures have been taken to not over-refine the
structure, i.e., not attempting to refine split disordered groups 
anisotropically, etc. 
;

_vrf_THETM01_Stage3_Final        
;
PROBLEM: The value of sine(theta_max)/wavelength is less than 0.550
RESPONSE: Mean I/\s dropped below 2.0 at 1.1\%A, so the data was cut
at 1.26\%A.
;

_vrf_PLAT023_Stage3_Final        
;
PROBLEM: Resolution (too) Low [sin(theta)/Lambda < 0.6]..      20.42 Degree
RESPONSE: See above
;

_vrf_PLAT029_Stage3_Final        
;
PROBLEM: _diffrn_measured_fraction_theta_full Low .......      0.927 Note  
RESPONSE: This data set contained diffraction from two samples: an intermediate
and this final, twinned compound. All overlapped reflections were omitted at
 the integration stage, leaving the completeness lower than optimal.
;

_vrf_PLAT088_Stage3_Final        
;
PROBLEM: Poor Data / Parameter Ratio ....................       4.81 Note  
RESPONSE: Due to the deletion of overlapped reflections and cutting the data,
the number of data is low. Measures have been taken to not over-refine the
structure, i.e., not attempting to refine split disordered groups 
anisotropically, etc.
;

_vrf_ABSMU01_Stage3_Final        
;
PROBLEM: Calculation of _exptl_absorpt_correction_mu
                not performed for this radiation type.
RESPONSE: Absorption corrections were done with SADABS that takes
 the x-ray wavelengths from the raw data. PLATON does
 not calculate these corrections for synchrotron radiation data.
;

_vrf_PLAT984_Stage3_Final        
;
PROBLEM: The element-f Deviates from the B&C-Value
RESPONSE: DISP values for each element type present were
 calculated for the 0.7749 angstrom x-rays using XDISP
 implemented in winGX, and using the Brennan model.
;

# end Validation Reply Form

####################################################################### 
# 
# 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_srj31_Final_LS
_database_code_depnum_ccdc_archive 'CCDC 1053058'
_audit_update_record             
;
2015-03-10 deposited with the CCDC.
2016-01-05 downloaded from the CCDC.
;

_audit_creation_method           SHELXL-2013
_chemical_name_systematic        
;
 ?
;
_chemical_name_common            ?
_chemical_melting_point          ?
_chemical_formula_moiety         'C36 H30 Fe N10 O2, 2(Cl O4), C3 H6 O'
_chemical_formula_sum            'C39 H36 Cl2 Fe N10 O11'
_chemical_formula_weight         947.53

loop_
_atom_type_symbol
_atom_type_description
_atom_type_scat_dispersion_real
_atom_type_scat_dispersion_imag
_atom_type_scat_source
C C -0.0020 0.0020
'WCROMER Program in WinGX L.Kissel & R.H.Pratt Acta Cryst A46 170 1990'
H H 0.0000 0.0000
'WCROMER Program in WinGX L.Kissel & R.H.Pratt Acta Cryst A46 170 1990'
N N -0.0031 0.0040
'WCROMER Program in WinGX L.Kissel & R.H.Pratt Acta Cryst A46 170 1990'
O O -0.0041 0.0074
'WCROMER Program in WinGX L.Kissel & R.H.Pratt Acta Cryst A46 170 1990'
Cl Cl 0.1408 0.1896
'WCROMER Program in WinGX L.Kissel & R.H.Pratt Acta Cryst A46 170 1990'
Fe Fe 0.2064 0.9930
'WCROMER Program in WinGX L.Kissel & R.H.Pratt Acta Cryst A46 170 1990'

_space_group_crystal_system      triclinic
_space_group_IT_number           2
_space_group_name_H-M_alt        'P -1'
_space_group_name_Hall           '-P 1'

_shelx_space_group_comment       
;
The symmetry employed for this shelxl refinement is uniquely defined
by the following loop, which should always be used as a source of
symmetry information in preference to the above space-group names.
They are only intended as comments.
;

loop_
_space_group_symop_operation_xyz
'x, y, z'
'-x, -y, -z'

_cell_length_a                   12.906(9)
_cell_length_b                   13.199(9)
_cell_length_c                   14.759(10)
_cell_angle_alpha                71.402(8)
_cell_angle_beta                 68.242(8)
_cell_angle_gamma                67.214(8)
_cell_volume                     2107(3)
_cell_formula_units_Z            2
_cell_measurement_temperature    150(2)
_cell_measurement_reflns_used    3947
_cell_measurement_theta_min      3.08
_cell_measurement_theta_max      24.73

_exptl_crystal_description       block
_exptl_crystal_colour            orange
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    ?
_exptl_crystal_density_diffrn    1.493
_exptl_crystal_F_000             976
_exptl_transmission_factor_min   ?
_exptl_transmission_factor_max   ?
_exptl_crystal_size_max          0.18
_exptl_crystal_size_mid          0.14
_exptl_crystal_size_min          0.08
_exptl_absorpt_coefficient_mu    0.699
_shelx_estimated_absorpt_T_min   0.884
_shelx_estimated_absorpt_T_max   0.946
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_correction_T_min  0.520
_exptl_absorpt_correction_T_max  0.745
_exptl_absorpt_process_details   'SADABS Bruker AXS Madison WI US'

_exptl_special_details           
;
 ?
;

_diffrn_ambient_temperature      150(2)
_diffrn_radiation_wavelength     0.7749
_diffrn_radiation_type           synchrotron
_diffrn_radiation_source         'Advanced Light Source station 11.3.1'
_diffrn_radiation_monochromator  'silicon 111'
_diffrn_measurement_device_type  'Bruker APEX II CCD diffractometer'
_diffrn_measurement_method       'π and ω rotation with narrow frames'
_diffrn_detector_area_resol_mean ?
_diffrn_reflns_number            15425
_diffrn_reflns_av_unetI/netI     0.0891
_diffrn_reflns_av_R_equivalents  0.0779
_diffrn_reflns_limit_h_min       -13
_diffrn_reflns_limit_h_max       14
_diffrn_reflns_limit_k_min       -14
_diffrn_reflns_limit_k_max       14
_diffrn_reflns_limit_l_min       -16
_diffrn_reflns_limit_l_max       16
_diffrn_reflns_theta_min         2.889
_diffrn_reflns_theta_max         25.087
_diffrn_reflns_theta_full        24.900
_diffrn_measured_fraction_theta_max 0.977
_diffrn_measured_fraction_theta_full 0.993
_diffrn_reflns_Laue_measured_fraction_max 0.977
_diffrn_reflns_Laue_measured_fraction_full 0.993
_diffrn_reflns_point_group_measured_fraction_max 0.977
_diffrn_reflns_point_group_measured_fraction_full 0.993
_reflns_number_total             5640
_reflns_number_gt                3580
_reflns_threshold_expression     'I > 2σ(I)'
_reflns_Friedel_coverage         0.000
_reflns_Friedel_fraction_max     .
_reflns_Friedel_fraction_full    .

_reflns_special_details          
;
 Reflections were merged by SHELXL according to the crystal
 class for the calculation of statistics and refinement.
 
 _reflns_Friedel_fraction is defined as the number of unique
 Friedel pairs measured divided by the number that would be
 possible theoretically, ignoring centric projections and
 systematic absences.
;

_vrf_THETM01_srj31_Final_LS      
;
PROBLEM:  The value of sine(theta_max)/wavelength is less than 0.550
RESPONSE: The crystal has suffered a transformation upon losing acetone
through a thermal treatment at 120 degrees C. This results in an
increased mosaicity and diffraction decreasing quickly. Indeed there
was significant diffraction only to 0.95 ansgtrom resolution, and
the present data were cut at 0.93 angstrom. All this leads to
rather low values of thetamax, thetafull, high wR2 and a poor though 
acceptable reflections to parameters ratio of 9.6.
;

_vrf_PLAT027_srj31_Final_LS      
;
PROBLEM:  _diffrn_reflns_theta_full (too) Low ............      24.90 Degree
RESPONSE: The crystal has suffered a transformation upon losing acetone
through a thermal treatment at 120 degrees C. This results in an
increased mosaicity and diffraction decreasing quickly. Indeed there
was significant diffraction only to 0.95 ansgtrom resolution, and
the present data were cut at 0.93 angstrom. All this leads to
rather low values of thetamax, thetafull, high wR2 and a poor though 
acceptable reflections to parameters ratio of 9.6.
;

_vrf_REFNR01_srj31_Final_LS      
;
PROBLEM:  Ratio of reflections to parameters is < 10 for a
            centrosymmetric structure
RESPONSE: The crystal has suffered a transformation upon losing acetone
through a thermal treatment at 120 degrees C. This results in an
increased mosaicity and diffraction decreasing quickly. Indeed there
was significant diffraction only to 0.95 ansgtrom resolution, and
the present data were cut at 0.93 angstrom. All this leads to
rather low values of thetamax, thetafull, high wR2 and a poor though 
acceptable reflections to parameters ratio of 9.6.
;

_vrf_RFACR01_srj31_Final_LS      
;
PROBLEM:  The value of the weighted R factor is > 0.25
RESPONSE: The crystal has suffered a transformation upon losing acetone
through a thermal treatment at 120 degrees C. This results in an
increased mosaicity and diffraction decreasing quickly. Indeed there
was significant diffraction only to 0.95 ansgtrom resolution, and
the present data were cut at 0.93 angstrom. All this leads to
rather low values of thetamax, thetafull, high wR2 and a poor though 
acceptable reflections to parameters ratio of 9.6.
;

_computing_data_collection       'Bruker APEX 2'
_computing_cell_refinement       'Bruker SAINT'
_computing_data_reduction        'Bruker SAINT'
_computing_structure_solution    'SIR97 (Altomare, 1999)'
_computing_structure_refinement  'SHELXL-2013 (Sheldrick, 2013)'
_computing_molecular_graphics    ?
_computing_publication_material  ?

_refine_special_details          
;
 All non-hydrogens were refined anisotropically. Hydrogens were placed
 geometrically on their carrier atom and refined with a riding model,
 except those on the pyrazole nitrogens N1, N5, N6 and N10, that were
 refined freely with their thermal parameter 1.2 times that of their
 carrier N.
;
_refine_ls_structure_factor_coef Fsqd
_refine_ls_matrix_type           full
_refine_ls_weighting_scheme      calc
_refine_ls_weighting_details     
'w=1/[σ²(Fo²)+(0.1684P)²+0.9250P] where P=(Fo²+2Fc²)/3'
_atom_sites_solution_primary     ?
_atom_sites_solution_secondary   ?
_atom_sites_solution_hydrogens   mixed
_refine_ls_hydrogen_treatment    mixed
_refine_ls_extinction_method     none
_refine_ls_extinction_coef       .
_refine_ls_number_reflns         5640
_refine_ls_number_parameters     584
_refine_ls_number_restraints     0
_refine_ls_R_factor_all          0.1252
_refine_ls_R_factor_gt           0.0819
_refine_ls_wR_factor_ref         0.2632
_refine_ls_wR_factor_gt          0.2314
_refine_ls_goodness_of_fit_ref   1.033
_refine_ls_restrained_S_all      1.033
_refine_ls_shift/su_max          0.000
_refine_ls_shift/su_mean         0.000

loop_
_atom_site_label
_atom_site_type_symbol
_atom_site_fract_x
_atom_site_fract_y
_atom_site_fract_z
_atom_site_U_iso_or_equiv
_atom_site_adp_type
_atom_site_occupancy
_atom_site_site_symmetry_order
_atom_site_calc_flag
_atom_site_refinement_flags_posn
_atom_site_refinement_flags_adp
_atom_site_refinement_flags_occupancy
_atom_site_disorder_assembly
_atom_site_disorder_group
Fe1 Fe 0.49013(9) 0.74110(9) 0.24218(8) 0.0448(4) Uani 1 1 d . . . . .
O1 O 0.9011(6) 0.6021(6) -0.1825(5) 0.086(2) Uani 1 1 d . . . . .
O2 O 0.2016(5) 0.8544(5) 0.5833(4) 0.0697(17) Uani 1 1 d . . . . .
N1 N 0.7410(6) 0.6998(5) 0.0893(5) 0.0503(16) Uani 1 1 d . . . . .
H1A H 0.778(7) 0.722(7) 0.118(6) 0.060 Uiso 1 1 d . U . . .
N2 N 0.6285(5) 0.7020(5) 0.1253(4) 0.0435(14) Uani 1 1 d . . . . .
N3 N 0.4233(5) 0.6894(5) 0.1740(4) 0.0455(15) Uani 1 1 d . . . . .
N4 N 0.3309(5) 0.7588(5) 0.3312(5) 0.0497(16) Uani 1 1 d . . . . .
N5 N 0.2648(6) 0.7990(5) 0.4138(4) 0.0473(15) Uani 1 1 d . . . . .
H5B H 0.306(7) 0.828(6) 0.438(6) 0.057 Uiso 1 1 d . U . . .
N6 N 0.5765(6) 0.4914(5) 0.3396(5) 0.0505(16) Uani 1 1 d . . . . .
H6B H 0.540(7) 0.470(7) 0.308(6) 0.061 Uiso 1 1 d . U . . .
N7 N 0.5571(5) 0.6017(5) 0.3277(4) 0.0487(16) Uani 1 1 d . . . . .
N8 N 0.5451(5) 0.7963(5) 0.3148(5) 0.0478(15) Uani 1 1 d . . . . .
N9 N 0.4471(5) 0.9025(5) 0.1811(4) 0.0453(15) Uani 1 1 d . . . . .
N10 N 0.3970(6) 0.9678(5) 0.1112(5) 0.0523(16) Uani 1 1 d . . . . .
H10A H 0.368(7) 0.926(7) 0.078(6) 0.063 Uiso 1 1 d . U . . .
C1 C 0.9480(11) 0.5755(11) -0.2786(8) 0.102(4) Uani 1 1 d . . . . .
H1B H 0.8869 0.5662 -0.2968 0.154 Uiso 1 1 calc R U . . .
H1C H 1.0133 0.5055 -0.2779 0.154 Uiso 1 1 calc R U . . .
H1D H 0.9762 0.6363 -0.3275 0.154 Uiso 1 1 calc R U . . .
C2 C 0.9722(8) 0.6164(8) -0.1406(7) 0.073(3) Uani 1 1 d . . . . .
C3 C 1.0904(9) 0.6038(9) -0.1895(8) 0.085(3) Uani 1 1 d . . . . .
H3A H 1.1240 0.5845 -0.2533 0.102 Uiso 1 1 calc R U . . .
C4 C 1.1570(9) 0.6191(9) -0.1455(9) 0.087(3) Uani 1 1 d . . . . .
H4A H 1.2384 0.6075 -0.1774 0.104 Uiso 1 1 calc R U . . .
C5 C 1.1076(9) 0.6516(10) -0.0546(9) 0.091(3) Uani 1 1 d . . . . .
H5A H 1.1535 0.6657 -0.0250 0.110 Uiso 1 1 calc R U . . .
C6 C 0.9874(7) 0.6634(8) -0.0063(8) 0.071(3) Uani 1 1 d . . . . .
H6A H 0.9538 0.6821 0.0576 0.086 Uiso 1 1 calc R U . . .
C7 C 0.9189(7) 0.6488(6) -0.0492(6) 0.054(2) Uani 1 1 d . . . . .
C8 C 0.7951(7) 0.6602(6) 0.0027(6) 0.052(2) Uani 1 1 d . . . . .
C9 C 0.7126(7) 0.6377(6) -0.0169(6) 0.054(2) Uani 1 1 d . . . . .
H9A H 0.7227 0.6096 -0.0724 0.065 Uiso 1 1 calc R U . . .
C10 C 0.6077(7) 0.6642(6) 0.0618(6) 0.0479(18) Uani 1 1 d . . . . .
C11 C 0.4912(7) 0.6566(6) 0.0871(6) 0.0494(19) Uani 1 1 d . . . . .
C12 C 0.4470(8) 0.6225(6) 0.0338(6) 0.059(2) Uani 1 1 d . . . . .
H12A H 0.4929 0.6031 -0.0290 0.071 Uiso 1 1 calc R U . . .
C13 C 0.3334(8) 0.6174(7) 0.0752(7) 0.062(2) Uani 1 1 d . . . . .
H13A H 0.3016 0.5915 0.0414 0.074 Uiso 1 1 calc R U . . .
C14 C 0.2660(7) 0.6491(7) 0.1641(7) 0.058(2) Uani 1 1 d . . . . .
H14A H 0.1882 0.6451 0.1919 0.070 Uiso 1 1 calc R U . . .
C15 C 0.3128(7) 0.6873(6) 0.2131(6) 0.0467(18) Uani 1 1 d . . . . .
C16 C 0.2596(7) 0.7287(6) 0.3036(6) 0.0499(19) Uani 1 1 d . . . . .
C17 C 0.1480(7) 0.7492(7) 0.3697(6) 0.058(2) Uani 1 1 d . . . . .
H17A H 0.0829 0.7342 0.3674 0.069 Uiso 1 1 calc R U . . .
C18 C 0.1512(7) 0.7974(7) 0.4416(6) 0.055(2) Uani 1 1 d . . . . .
C19 C 0.0602(8) 0.8401(7) 0.5268(6) 0.061(2) Uani 1 1 d . . . . .
C20 C -0.0576(8) 0.8545(8) 0.5374(8) 0.077(3) Uani 1 1 d . . . . .
H20A H -0.0763 0.8370 0.4888 0.092 Uiso 1 1 calc R U . . .
C21 C -0.1453(9) 0.8936(9) 0.6171(9) 0.092(3) Uani 1 1 d . . . . .
H21A H -0.2245 0.9034 0.6236 0.110 Uiso 1 1 calc R U . . .
C22 C -0.1183(10) 0.9185(9) 0.6871(8) 0.085(3) Uani 1 1 d . . . . .
H22A H -0.1791 0.9419 0.7438 0.102 Uiso 1 1 calc R U . . .
C23 C -0.0066(10) 0.9108(9) 0.6779(8) 0.087(3) Uani 1 1 d . . . . .
H23A H 0.0094 0.9331 0.7253 0.104 Uiso 1 1 calc R U . . .
C24 C 0.0845(7) 0.8694(7) 0.5974(7) 0.062(2) Uani 1 1 d . . . . .
C25 C 0.2339(10) 0.8779(9) 0.6569(8) 0.090(3) Uani 1 1 d . . . . .
H25A H 0.3193 0.8601 0.6382 0.135 Uiso 1 1 calc R U . . .
H25B H 0.2072 0.8320 0.7223 0.135 Uiso 1 1 calc R U . . .
H25C H 0.1971 0.9576 0.6599 0.135 Uiso 1 1 calc R U . . .
C26 C 0.6364(7) 0.4303(7) 0.4074(6) 0.055(2) Uani 1 1 d . . . . .
H26A H 0.6590 0.3508 0.4279 0.066 Uiso 1 1 calc R U . . .
C27 C 0.6588(7) 0.5018(7) 0.4412(5) 0.056(2) Uani 1 1 d . . . . .
H27A H 0.6996 0.4834 0.4891 0.067 Uiso 1 1 calc R U . . .
C28 C 0.6078(7) 0.6104(7) 0.3891(5) 0.0491(19) Uani 1 1 d . . . . .
C29 C 0.5959(7) 0.7264(7) 0.3858(6) 0.0514(19) Uani 1 1 d . . . . .
C30 C 0.6304(7) 0.7634(7) 0.4444(6) 0.059(2) Uani 1 1 d . . . . .
H30A H 0.6665 0.7120 0.4939 0.071 Uiso 1 1 calc R U . . .
C31 C 0.6106(8) 0.8780(8) 0.4286(7) 0.066(2) Uani 1 1 d . . . . .
H31A H 0.6340 0.9060 0.4673 0.079 Uiso 1 1 calc R U . . .
C32 C 0.5569(8) 0.9517(7) 0.3565(7) 0.061(2) Uani 1 1 d . . . . .
H32A H 0.5420 1.0303 0.3463 0.073 Uiso 1 1 calc R U . . .
C33 C 0.5252(7) 0.9089(6) 0.2991(6) 0.0493(19) Uani 1 1 d . . . . .
C34 C 0.4697(7) 0.9678(7) 0.2206(6) 0.051(2) Uani 1 1 d . . . . .
C35 C 0.4306(7) 1.0801(7) 0.1722(6) 0.060(2) Uani 1 1 d . . . . .
H35A H 0.4352 1.1444 0.1844 0.072 Uiso 1 1 calc R U . . .
C36 C 0.3850(7) 1.0771(7) 0.1045(7) 0.062(2) Uani 1 1 d . . . . .
H36A H 0.3507 1.1401 0.0599 0.074 Uiso 1 1 calc R U . . .
Cl1 Cl 0.5630(2) 0.65412(19) -0.27076(16) 0.0688(7) Uani 1 1 d . . . . .
Cl2 Cl 0.9049(2) 0.7898(2) 0.2311(2) 0.0800(8) Uani 1 1 d . . . . .
O3 O 0.6219(6) 0.6480(6) -0.2028(5) 0.0820(19) Uani 1 1 d . . . . .
O4 O 0.5274(7) 0.7647(5) -0.3217(5) 0.094(2) Uani 1 1 d . . . . .
O5 O 0.4649(7) 0.6148(7) -0.2167(6) 0.103(2) Uani 1 1 d . . . . .
O6 O 0.6380(8) 0.5841(6) -0.3403(5) 0.100(2) Uani 1 1 d . . . . .
O7 O 0.8777(7) 0.8751(7) 0.2795(7) 0.121(3) Uani 1 1 d . . . . .
O8 O 0.8088(6) 0.7996(7) 0.2020(5) 0.096(2) Uani 1 1 d . . . . .
O9 O 1.0024(7) 0.7941(10) 0.1461(7) 0.139(4) Uani 1 1 d . . . . .
O10 O 0.9344(10) 0.6926(8) 0.3007(10) 0.166(5) Uani 1 1 d . . . . .
O1S O 0.6689(6) 0.1028(5) 0.0067(5) 0.0750(17) Uani 1 1 d . . . . .
C1S C 0.7655(9) 0.0731(8) 0.0174(7) 0.070(2) Uani 1 1 d . . . . .
C2S C 0.8664(9) -0.0024(11) -0.0410(9) 0.098(4) Uani 1 1 d . . . . .
H2SA H 0.8392 -0.0354 -0.0753 0.147 Uiso 1 1 calc R U . . .
H2SB H 0.9092 -0.0623 0.0034 0.147 Uiso 1 1 calc R U . . .
H2SC H 0.9183 0.0400 -0.0903 0.147 Uiso 1 1 calc R U . . .
C3S C 0.7821(11) 0.1103(10) 0.0960(9) 0.099(4) Uani 1 1 d . . . . .
H3SA H 0.7087 0.1636 0.1260 0.149 Uiso 1 1 calc R U . . .
H3SB H 0.8439 0.1466 0.0655 0.149 Uiso 1 1 calc R U . . .
H3SC H 0.8046 0.0449 0.1476 0.149 Uiso 1 1 calc R U . . .


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

loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
_geom_bond_publ_flag
Fe1 N8 1.909(6) . ?
Fe1 N3 1.940(6) . ?
Fe1 N7 1.955(6) . ?
Fe1 N4 1.956(6) . ?
Fe1 N9 1.972(6) . ?
Fe1 N2 2.000(6) . ?
O1 C2 1.374(12) . ?
O1 C1 1.421(11) . ?
O2 C24 1.389(10) . ?
O2 C25 1.449(11) . ?
N1 N2 1.341(8) . ?
N1 C8 1.370(10) . ?
N1 H1A 0.91(8) . ?
N2 C10 1.336(9) . ?
N3 C15 1.334(9) . ?
N3 C11 1.352(9) . ?
N4 N5 1.337(8) . ?
N4 C16 1.355(9) . ?
N5 C18 1.375(10) . ?
N5 H5B 0.97(8) . ?
N6 N7 1.341(8) . ?
N6 C26 1.351(10) . ?
N6 H6B 0.93(8) . ?
N7 C28 1.351(9) . ?
N8 C29 1.342(10) . ?
N8 C33 1.363(10) . ?
N9 N10 1.312(8) . ?
N9 C34 1.346(9) . ?
N10 C36 1.364(10) . ?
N10 H10A 1.06(8) . ?
C1 H1B 0.9800 . ?
C1 H1C 0.9800 . ?
C1 H1D 0.9800 . ?
C2 C7 1.389(13) . ?
C2 C3 1.393(14) . ?
C3 C4 1.355(15) . ?
C3 H3A 0.9500 . ?
C4 C5 1.383(16) . ?
C4 H4A 0.9500 . ?
C5 C6 1.415(13) . ?
C5 H5A 0.9500 . ?
C6 C7 1.358(12) . ?
C6 H6A 0.9500 . ?
C7 C8 1.464(11) . ?
C8 C9 1.354(11) . ?
C9 C10 1.425(11) . ?
C9 H9A 0.9500 . ?
C10 C11 1.444(11) . ?
C11 C12 1.381(11) . ?
C12 C13 1.382(12) . ?
C12 H12A 0.9500 . ?
C13 C14 1.369(12) . ?
C13 H13A 0.9500 . ?
C14 C15 1.390(10) . ?
C14 H14A 0.9500 . ?
C15 C16 1.431(11) . ?
C16 C17 1.387(11) . ?
C17 C18 1.419(12) . ?
C17 H17A 0.9500 . ?
C18 C19 1.457(11) . ?
C19 C24 1.389(12) . ?
C19 C20 1.411(13) . ?
C20 C21 1.371(14) . ?
C20 H20A 0.9500 . ?
C21 C22 1.368(15) . ?
C21 H21A 0.9500 . ?
C22 C23 1.362(15) . ?
C22 H22A 0.9500 . ?
C23 C24 1.405(13) . ?
C23 H23A 0.9500 . ?
C25 H25A 0.9800 . ?
C25 H25B 0.9800 . ?
C25 H25C 0.9800 . ?
C26 C27 1.357(11) . ?
C26 H26A 0.9500 . ?
C27 C28 1.421(11) . ?
C27 H27A 0.9500 . ?
C28 C29 1.466(11) . ?
C29 C30 1.380(11) . ?
C30 C31 1.389(12) . ?
C30 H30A 0.9500 . ?
C31 C32 1.387(12) . ?
C31 H31A 0.9500 . ?
C32 C33 1.395(11) . ?
C32 H32A 0.9500 . ?
C33 C34 1.438(11) . ?
C34 C35 1.405(12) . ?
C35 C36 1.351(12) . ?
C35 H35A 0.9500 . ?
C36 H36A 0.9500 . ?
Cl1 O4 1.394(7) . ?
Cl1 O5 1.416(7) . ?
Cl1 O6 1.421(7) . ?
Cl1 O3 1.435(6) . ?
Cl2 O10 1.384(10) . ?
Cl2 O7 1.386(8) . ?
Cl2 O8 1.406(7) . ?
Cl2 O9 1.414(9) . ?
O1S C1S 1.209(10) . ?
C1S C2S 1.464(14) . ?
C1S C3S 1.503(14) . ?
C2S H2SA 0.9800 . ?
C2S H2SB 0.9800 . ?
C2S H2SC 0.9800 . ?
C3S H3SA 0.9800 . ?
C3S H3SB 0.9800 . ?
C3S H3SC 0.9800 . ?

loop_
_geom_angle_atom_site_label_1
_geom_angle_atom_site_label_2
_geom_angle_atom_site_label_3
_geom_angle
_geom_angle_site_symmetry_1
_geom_angle_site_symmetry_3
_geom_angle_publ_flag
N8 Fe1 N3 176.0(3) . . ?
N8 Fe1 N7 79.1(3) . . ?
N3 Fe1 N7 101.9(3) . . ?
N8 Fe1 N4 97.4(3) . . ?
N3 Fe1 N4 78.7(3) . . ?
N7 Fe1 N4 93.4(3) . . ?
N8 Fe1 N9 79.6(3) . . ?
N3 Fe1 N9 99.4(3) . . ?
N7 Fe1 N9 158.7(3) . . ?
N4 Fe1 N9 90.7(2) . . ?
N8 Fe1 N2 103.9(3) . . ?
N3 Fe1 N2 79.9(3) . . ?
N7 Fe1 N2 90.6(2) . . ?
N4 Fe1 N2 158.7(3) . . ?
N9 Fe1 N2 93.2(2) . . ?
C2 O1 C1 119.6(8) . . ?
C24 O2 C25 119.1(7) . . ?
N2 N1 C8 111.7(7) . . ?
N2 N1 H1A 125(5) . . ?
C8 N1 H1A 123(5) . . ?
C10 N2 N1 106.7(6) . . ?
C10 N2 Fe1 113.9(5) . . ?
N1 N2 Fe1 139.4(5) . . ?
C15 N3 C11 121.9(6) . . ?
C15 N3 Fe1 119.8(5) . . ?
C11 N3 Fe1 118.3(5) . . ?
N5 N4 C16 105.7(6) . . ?
N5 N4 Fe1 138.2(5) . . ?
C16 N4 Fe1 116.0(5) . . ?
N4 N5 C18 112.9(7) . . ?
N4 N5 H5B 113(5) . . ?
C18 N5 H5B 134(5) . . ?
N7 N6 C26 111.5(7) . . ?
N7 N6 H6B 118(5) . . ?
C26 N6 H6B 130(5) . . ?
N6 N7 C28 105.6(6) . . ?
N6 N7 Fe1 137.6(5) . . ?
C28 N7 Fe1 116.6(5) . . ?
C29 N8 C33 119.6(7) . . ?
C29 N8 Fe1 120.8(5) . . ?
C33 N8 Fe1 119.4(5) . . ?
N10 N9 C34 107.8(6) . . ?
N10 N9 Fe1 136.9(5) . . ?
C34 N9 Fe1 115.3(5) . . ?
N9 N10 C36 110.1(7) . . ?
N9 N10 H10A 115(4) . . ?
C36 N10 H10A 135(4) . . ?
O1 C1 H1B 109.5 . . ?
O1 C1 H1C 109.5 . . ?
H1B C1 H1C 109.5 . . ?
O1 C1 H1D 109.5 . . ?
H1B C1 H1D 109.5 . . ?
H1C C1 H1D 109.5 . . ?
O1 C2 C7 116.5(8) . . ?
O1 C2 C3 121.6(9) . . ?
C7 C2 C3 121.8(10) . . ?
C4 C3 C2 119.5(10) . . ?
C4 C3 H3A 120.2 . . ?
C2 C3 H3A 120.2 . . ?
C3 C4 C5 120.6(9) . . ?
C3 C4 H4A 119.7 . . ?
C5 C4 H4A 119.7 . . ?
C4 C5 C6 118.7(11) . . ?
C4 C5 H5A 120.7 . . ?
C6 C5 H5A 120.7 . . ?
C7 C6 C5 121.7(9) . . ?
C7 C6 H6A 119.2 . . ?
C5 C6 H6A 119.2 . . ?
C6 C7 C2 117.6(8) . . ?
C6 C7 C8 120.6(8) . . ?
C2 C7 C8 121.7(8) . . ?
C9 C8 N1 106.2(7) . . ?
C9 C8 C7 132.5(7) . . ?
N1 C8 C7 121.4(7) . . ?
C8 C9 C10 106.8(7) . . ?
C8 C9 H9A 126.6 . . ?
C10 C9 H9A 126.6 . . ?
N2 C10 C9 108.7(7) . . ?
N2 C10 C11 116.5(6) . . ?
C9 C10 C11 134.9(7) . . ?
N3 C11 C12 120.7(7) . . ?
N3 C11 C10 111.3(6) . . ?
C12 C11 C10 127.9(7) . . ?
C11 C12 C13 117.6(8) . . ?
C11 C12 H12A 121.2 . . ?
C13 C12 H12A 121.2 . . ?
C14 C13 C12 121.1(8) . . ?
C14 C13 H13A 119.5 . . ?
C12 C13 H13A 119.5 . . ?
C13 C14 C15 119.3(8) . . ?
C13 C14 H14A 120.4 . . ?
C15 C14 H14A 120.4 . . ?
N3 C15 C14 119.3(7) . . ?
N3 C15 C16 110.8(6) . . ?
C14 C15 C16 129.9(7) . . ?
N4 C16 C17 110.9(7) . . ?
N4 C16 C15 114.7(7) . . ?
C17 C16 C15 134.4(7) . . ?
C16 C17 C18 105.8(7) . . ?
C16 C17 H17A 127.1 . . ?
C18 C17 H17A 127.1 . . ?
N5 C18 C17 104.7(7) . . ?
N5 C18 C19 124.0(8) . . ?
C17 C18 C19 131.3(8) . . ?
C24 C19 C20 118.3(8) . . ?
C24 C19 C18 122.5(8) . . ?
C20 C19 C18 119.1(8) . . ?
C21 C20 C19 120.6(10) . . ?
C21 C20 H20A 119.7 . . ?
C19 C20 H20A 119.7 . . ?
C22 C21 C20 119.6(10) . . ?
C22 C21 H21A 120.2 . . ?
C20 C21 H21A 120.2 . . ?
C23 C22 C21 122.0(10) . . ?
C23 C22 H22A 119.0 . . ?
C21 C22 H22A 119.0 . . ?
C22 C23 C24 119.0(11) . . ?
C22 C23 H23A 120.5 . . ?
C24 C23 H23A 120.5 . . ?
C19 C24 O2 116.2(7) . . ?
C19 C24 C23 120.3(9) . . ?
O2 C24 C23 123.5(9) . . ?
O2 C25 H25A 109.5 . . ?
O2 C25 H25B 109.5 . . ?
H25A C25 H25B 109.5 . . ?
O2 C25 H25C 109.5 . . ?
H25A C25 H25C 109.5 . . ?
H25B C25 H25C 109.5 . . ?
N6 C26 C27 108.3(7) . . ?
N6 C26 H26A 125.8 . . ?
C27 C26 H26A 125.8 . . ?
C26 C27 C28 104.7(7) . . ?
C26 C27 H27A 127.6 . . ?
C28 C27 H27A 127.6 . . ?
N7 C28 C27 109.8(7) . . ?
N7 C28 C29 113.5(7) . . ?
C27 C28 C29 136.7(7) . . ?
N8 C29 C30 122.8(7) . . ?
N8 C29 C28 109.8(6) . . ?
C30 C29 C28 127.4(8) . . ?
C29 C30 C31 117.9(8) . . ?
C29 C30 H30A 121.1 . . ?
C31 C30 H30A 121.1 . . ?
C32 C31 C30 120.2(8) . . ?
C32 C31 H31A 119.9 . . ?
C30 C31 H31A 119.9 . . ?
C31 C32 C33 119.1(8) . . ?
C31 C32 H32A 120.4 . . ?
C33 C32 H32A 120.4 . . ?
N8 C33 C32 120.4(7) . . ?
N8 C33 C34 110.4(7) . . ?
C32 C33 C34 129.2(7) . . ?
N9 C34 C35 108.6(7) . . ?
N9 C34 C33 115.1(7) . . ?
C35 C34 C33 136.3(7) . . ?
C36 C35 C34 105.4(7) . . ?
C36 C35 H35A 127.3 . . ?
C34 C35 H35A 127.3 . . ?
C35 C36 N10 108.1(8) . . ?
C35 C36 H36A 126.0 . . ?
N10 C36 H36A 126.0 . . ?
O4 Cl1 O5 110.3(5) . . ?
O4 Cl1 O6 109.5(4) . . ?
O5 Cl1 O6 107.5(5) . . ?
O4 Cl1 O3 109.7(4) . . ?
O5 Cl1 O3 109.1(4) . . ?
O6 Cl1 O3 110.7(5) . . ?
O10 Cl2 O7 103.9(7) . . ?
O10 Cl2 O8 113.0(6) . . ?
O7 Cl2 O8 110.5(5) . . ?
O10 Cl2 O9 109.9(7) . . ?
O7 Cl2 O9 110.1(6) . . ?
O8 Cl2 O9 109.4(5) . . ?
O1S C1S C2S 121.8(9) . . ?
O1S C1S C3S 119.4(9) . . ?
C2S C1S C3S 118.7(9) . . ?
C1S C2S H2SA 109.5 . . ?
C1S C2S H2SB 109.5 . . ?
H2SA C2S H2SB 109.5 . . ?
C1S C2S H2SC 109.5 . . ?
H2SA C2S H2SC 109.5 . . ?
H2SB C2S H2SC 109.5 . . ?
C1S C3S H3SA 109.5 . . ?
C1S C3S H3SB 109.5 . . ?
H3SA C3S H3SB 109.5 . . ?
C1S C3S H3SC 109.5 . . ?
H3SA C3S H3SC 109.5 . . ?
H3SB C3S H3SC 109.5 . . ?

_refine_diff_density_max         0.729
_refine_diff_density_min         -0.424
_refine_diff_density_rms         0.112

_shelxl_version_number           2013-4

####################################################################### 
# 
# 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_srj31a260_Final_HS
_database_code_depnum_ccdc_archive 'CCDC 1053059'
_audit_update_record             
;
2015-03-10 deposited with the CCDC.
2016-01-05 downloaded from the CCDC.
;

_audit_creation_method           SHELXL-2013
_chemical_name_systematic        
;
 ?
;
_chemical_name_common            ?
_chemical_melting_point          ?
_chemical_formula_moiety         'C36 H30 Fe N10 O2, 2(Cl O4), C3 H6 O'
_chemical_formula_sum            'C39 H36 Cl2 Fe N10 O11'
_chemical_formula_weight         947.53

loop_
_atom_type_symbol
_atom_type_description
_atom_type_scat_dispersion_real
_atom_type_scat_dispersion_imag
_atom_type_scat_source
C C -0.0020 0.0020
'WCROMER Program in WinGX L.Kissel & R.H.Pratt Acta Cryst A46 170 1990'
H H 0.0000 0.0000
'WCROMER Program in WinGX L.Kissel & R.H.Pratt Acta Cryst A46 170 1990'
N N -0.0031 0.0040
'WCROMER Program in WinGX L.Kissel & R.H.Pratt Acta Cryst A46 170 1990'
O O -0.0041 0.0074
'WCROMER Program in WinGX L.Kissel & R.H.Pratt Acta Cryst A46 170 1990'
Cl Cl 0.1408 0.1896
'WCROMER Program in WinGX L.Kissel & R.H.Pratt Acta Cryst A46 170 1990'
Fe Fe 0.2064 0.9930
'WCROMER Program in WinGX L.Kissel & R.H.Pratt Acta Cryst A46 170 1990'

_space_group_crystal_system      triclinic
_space_group_IT_number           2
_space_group_name_H-M_alt        'P -1'
_space_group_name_Hall           '-P 1'

_shelx_space_group_comment       
;
The symmetry employed for this shelxl refinement is uniquely defined
by the following loop, which should always be used as a source of
symmetry information in preference to the above space-group names.
They are only intended as comments.
;

loop_
_space_group_symop_operation_xyz
'x, y, z'
'-x, -y, -z'

_cell_length_a                   13.085(6)
_cell_length_b                   13.381(6)
_cell_length_c                   14.139(7)
_cell_angle_alpha                72.092(6)
_cell_angle_beta                 69.882(7)
_cell_angle_gamma                70.219(6)
_cell_volume                     2135.6(17)
_cell_formula_units_Z            2
_cell_measurement_temperature    260(2)
_cell_measurement_reflns_used    3026
_cell_measurement_theta_min      3.26
_cell_measurement_theta_max      22.76

_exptl_crystal_description       block
_exptl_crystal_colour            orange
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    ?
_exptl_crystal_density_diffrn    1.473
_exptl_crystal_F_000             976
_exptl_transmission_factor_min   ?
_exptl_transmission_factor_max   ?
_exptl_crystal_size_max          0.180
_exptl_crystal_size_mid          0.140
_exptl_crystal_size_min          0.080
_exptl_absorpt_coefficient_mu    0.690
_shelx_estimated_absorpt_T_min   0.886
_shelx_estimated_absorpt_T_max   0.947
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_correction_T_min  0.519
_exptl_absorpt_correction_T_max  0.745
_exptl_absorpt_process_details   'SADABS Bruker AXS Madison WI US'

_exptl_special_details           
;
 ?
;

_diffrn_ambient_temperature      260(2)
_diffrn_radiation_wavelength     0.7749
_diffrn_radiation_type           synchrotron
_diffrn_radiation_source         'Advanced Light Source station 11.3.1'
_diffrn_radiation_monochromator  'silicon 111'
_diffrn_measurement_device_type  'Bruker APEX II CCD diffractometer'
_diffrn_measurement_method       'π and ω rotation with narrow frames'
_diffrn_detector_area_resol_mean ?
_diffrn_reflns_number            14966
_diffrn_reflns_av_unetI/netI     0.0856
_diffrn_reflns_av_R_equivalents  0.0788
_diffrn_reflns_limit_h_min       -13
_diffrn_reflns_limit_h_max       13
_diffrn_reflns_limit_k_min       -13
_diffrn_reflns_limit_k_max       13
_diffrn_reflns_limit_l_min       -14
_diffrn_reflns_limit_l_max       14
_diffrn_reflns_theta_min         2.856
_diffrn_reflns_theta_max         23.880
_diffrn_reflns_theta_full        23.800
_diffrn_measured_fraction_theta_max 0.990
_diffrn_measured_fraction_theta_full 0.994
_diffrn_reflns_Laue_measured_fraction_max 0.990
_diffrn_reflns_Laue_measured_fraction_full 0.994
_diffrn_reflns_point_group_measured_fraction_max 0.990
_diffrn_reflns_point_group_measured_fraction_full 0.994
_reflns_number_total             5051
_reflns_number_gt                3040
_reflns_threshold_expression     'I > 2σ(I)'
_reflns_Friedel_coverage         0.000
_reflns_Friedel_fraction_max     .
_reflns_Friedel_fraction_full    .

_reflns_special_details          
;
 Reflections were merged by SHELXL according to the crystal
 class for the calculation of statistics and refinement.
 
 _reflns_Friedel_fraction is defined as the number of unique
 Friedel pairs measured divided by the number that would be
 possible theoretically, ignoring centric projections and
 systematic absences.
;

_vrf_THETM01_srj31a260_Final_HS  
;
PROBLEM:  The value of sine(theta_max)/wavelength is less than 0.550
RESPONSE: The crystal has suffered a transformation upon losing acetone
through a thermal treatment at 120 degrees C. This results in an
increased mosaicity and diffraction decreasing quickly. Indeed there
was significant diffraction only to 0.95 ansgtrom resolution, and
the present data were cut at 0.96 angstrom. All this leads to
rather low values of thetamax, thetafull, high wR2 and a poor though 
acceptable reflections to parameters ratio of 8.4.
;

_vrf_PLAT027_srj31a260_Final_HS  
;
PROBLEM:  _diffrn_reflns_theta_full (too) Low ............      24.90 Degree
RESPONSE: The crystal has suffered a transformation upon losing acetone
through a thermal treatment at 120 degrees C. This results in an
increased mosaicity and diffraction decreasing quickly. Indeed there
was significant diffraction only to 0.95 ansgtrom resolution, and
the present data were cut at 0.96 angstrom. All this leads to
rather low values of thetamax, thetafull, high wR2 and a poor though 
acceptable reflections to parameters ratio of 8.4.
;

_vrf_REFNR01_srj31a260_Final_HS  
;
PROBLEM:  Ratio of reflections to parameters is < 10 for a
            centrosymmetric structure
RESPONSE: The crystal has suffered a transformation upon losing acetone
through a thermal treatment at 120 degrees C. This results in an
increased mosaicity and diffraction decreasing quickly. Indeed there
was significant diffraction only to 0.95 ansgtrom resolution, and
the present data were cut at 0.96 angstrom. All this leads to
rather low values of thetamax, thetafull, high wR2 and a poor though 
acceptable reflections to parameters ratio of 8.4.
;

_vrf_RFACR01_srj31a260_Final_HS  
;
PROBLEM:  The value of the weighted R factor is > 0.25
RESPONSE: The crystal has suffered a transformation upon losing acetone
through a thermal treatment at 120 degrees C. This results in an
increased mosaicity and diffraction decreasing quickly. Indeed there
was significant diffraction only to 0.95 angstrom resolution, and
the present data were cut at 0.96 angstrom. All this leads to
rather low values of thetamax, thetafull, high wR2 and a poor though 
acceptable reflections to parameters ratio of 8.4.
;

_computing_data_collection       'Bruker APEX 2'
_computing_cell_refinement       'Bruker SAINT'
_computing_data_reduction        'Bruker SAINT'
_computing_structure_solution    'SIR97 (Altomare, 1999)'
_computing_structure_refinement  'SHELXL-2013 (Sheldrick, 2013)'
_computing_molecular_graphics    ?
_computing_publication_material  ?

_refine_special_details          
;
 All non-hydrogens were refined anisotropically. Both perchlorates showed
 some disorder, mostly of two of their oxygens, O3 and O6 on one hand
 and O6 and O10 on the other. O3 and O6 were split over two positions,
 with relative occupancies of 0.478:0.522. O8 and O10 were first splt
 but as this did not improve the model, they were kept as full
 occupancy sites. Both perchlorates were refined with distance and 
 displacement parameters restraints. Hydrogens were placed
 geometrically on their carrier atom and refined with a riding model,
 except those on the pyrazole nitrogens N1, N5, N6 and N10, that were
 refined freely with their thermal parameter 1.2 times that of their
 carrier N.
;

_refine_ls_structure_factor_coef Fsqd
_refine_ls_matrix_type           full
_refine_ls_weighting_scheme      calc
_refine_ls_weighting_details     
'w=1/[σ²(Fo²)+(0.1619P)²+2.2416P] where P=(Fo²+2Fc²)/3'
_atom_sites_solution_primary     ?
_atom_sites_solution_secondary   ?
_atom_sites_solution_hydrogens   mixed
_refine_ls_hydrogen_treatment    mixed
_refine_ls_extinction_method     none
_refine_ls_extinction_coef       .
_refine_ls_number_reflns         5051
_refine_ls_number_parameters     603
_refine_ls_number_restraints     220
_refine_ls_R_factor_all          0.1404
_refine_ls_R_factor_gt           0.0911
_refine_ls_wR_factor_ref         0.2849
_refine_ls_wR_factor_gt          0.2534
_refine_ls_goodness_of_fit_ref   1.077
_refine_ls_restrained_S_all      1.259
_refine_ls_shift/su_max          0.000
_refine_ls_shift/su_mean         0.000

loop_
_atom_site_label
_atom_site_type_symbol
_atom_site_fract_x
_atom_site_fract_y
_atom_site_fract_z
_atom_site_U_iso_or_equiv
_atom_site_adp_type
_atom_site_occupancy
_atom_site_site_symmetry_order
_atom_site_calc_flag
_atom_site_refinement_flags_posn
_atom_site_refinement_flags_adp
_atom_site_refinement_flags_occupancy
_atom_site_disorder_assembly
_atom_site_disorder_group
Fe1 Fe 0.50126(10) 0.74689(10) 0.25025(10) 0.0598(5) Uani 1 1 d . . . . .
O1 O 0.8678(7) 0.5891(7) -0.2022(6) 0.110(3) Uani 1 1 d . . . . .
O2 O 0.1646(6) 0.8594(6) 0.6000(5) 0.092(2) Uani 1 1 d . . . . .
N1 N 0.7481(7) 0.6895(6) 0.0731(6) 0.065(2) Uani 1 1 d . . . . .
H1A H 0.793(8) 0.679(7) 0.119(7) 0.078 Uiso 1 1 d . U . . .
N2 N 0.6394(6) 0.6952(5) 0.1183(6) 0.0609(19) Uani 1 1 d . . . . .
N3 N 0.4259(6) 0.6926(5) 0.1723(6) 0.0591(18) Uani 1 1 d . . . . .
N4 N 0.3232(6) 0.7628(6) 0.3417(6) 0.0617(19) Uani 1 1 d . . . . .
N5 N 0.2503(6) 0.8012(6) 0.4233(6) 0.063(2) Uani 1 1 d . . . . .
H5B H 0.272(7) 0.821(7) 0.471(7) 0.075 Uiso 1 1 d . U . . .
N6 N 0.6037(9) 0.5086(8) 0.3838(9) 0.097(3) Uani 1 1 d . . . . .
H6B H 0.563(10) 0.497(9) 0.335(9) 0.117 Uiso 1 1 d . U . . .
N7 N 0.5774(7) 0.6177(6) 0.3586(6) 0.072(2) Uani 1 1 d . . . . .
N8 N 0.5588(6) 0.8225(7) 0.3288(6) 0.070(2) Uani 1 1 d . . . . .
N9 N 0.4589(6) 0.9175(6) 0.1821(6) 0.0595(18) Uani 1 1 d . . . . .
N10 N 0.4048(7) 0.9846(7) 0.1140(7) 0.077(2) Uani 1 1 d . . . . .
H10A H 0.365(8) 0.955(8) 0.084(8) 0.092 Uiso 1 1 d . U . . .
C1 C 0.8979(12) 0.5658(12) -0.2997(10) 0.123(5) Uani 1 1 d . . . . .
H1B H 0.8310 0.5756 -0.3189 0.185 Uiso 1 1 calc R U . . .
H1C H 0.9424 0.4920 -0.2977 0.185 Uiso 1 1 calc R U . . .
H1D H 0.9409 0.6141 -0.3494 0.185 Uiso 1 1 calc R U . . .
C2 C 0.9476(10) 0.6007(9) -0.1670(9) 0.086(3) Uani 1 1 d . . . . .
C3 C 1.0588(12) 0.5851(11) -0.2181(11) 0.119(5) Uani 1 1 d . . . . .
H3A H 1.0841 0.5630 -0.2804 0.143 Uiso 1 1 calc R U . . .
C4 C 1.1369(12) 0.6012(10) -0.1807(13) 0.115(4) Uani 1 1 d . . . . .
H4A H 1.2130 0.5878 -0.2158 0.138 Uiso 1 1 calc R U . . .
C5 C 1.0986(10) 0.6362(10) -0.0934(12) 0.107(4) Uani 1 1 d . . . . .
H5A H 1.1482 0.6517 -0.0694 0.129 Uiso 1 1 calc R U . . .
C6 C 0.9859(9) 0.6503(9) -0.0369(9) 0.090(3) Uani 1 1 d . . . . .
H6A H 0.9630 0.6695 0.0266 0.108 Uiso 1 1 calc R U . . .
C7 C 0.9078(8) 0.6361(8) -0.0735(8) 0.072(3) Uani 1 1 d . . . . .
C8 C 0.7893(8) 0.6504(7) -0.0144(8) 0.066(2) Uani 1 1 d . . . . .
C9 C 0.6987(8) 0.6315(7) -0.0272(8) 0.069(3) Uani 1 1 d . . . . .
H9A H 0.6982 0.6054 -0.0808 0.083 Uiso 1 1 calc R U . . .
C10 C 0.6066(7) 0.6595(7) 0.0565(7) 0.060(2) Uani 1 1 d . . . . .
C11 C 0.4902(8) 0.6576(6) 0.0850(7) 0.063(2) Uani 1 1 d . . . . .
C12 C 0.4432(9) 0.6261(7) 0.0267(8) 0.072(3) Uani 1 1 d . . . . .
H12A H 0.4863 0.6057 -0.0354 0.087 Uiso 1 1 calc R U . . .
C13 C 0.3299(9) 0.6263(8) 0.0652(9) 0.084(3) Uani 1 1 d . . . . .
H13A H 0.2966 0.6040 0.0296 0.100 Uiso 1 1 calc R U . . .
C14 C 0.2665(9) 0.6597(8) 0.1563(9) 0.079(3) Uani 1 1 d . . . . .
H14A H 0.1907 0.6603 0.1822 0.094 Uiso 1 1 calc R U . . .
C15 C 0.3180(8) 0.6922(7) 0.2082(8) 0.066(2) Uani 1 1 d . . . . .
C16 C 0.2604(8) 0.7341(7) 0.3013(7) 0.061(2) Uani 1 1 d . . . . .
C17 C 0.1482(8) 0.7551(8) 0.3579(8) 0.073(3) Uani 1 1 d . . . . .
H17A H 0.0888 0.7423 0.3456 0.087 Uiso 1 1 calc R U . . .
C18 C 0.1435(8) 0.7997(7) 0.4376(7) 0.068(2) Uani 1 1 d . . . . .
C19 C 0.0462(8) 0.8379(8) 0.5203(8) 0.073(3) Uani 1 1 d . . . . .
C20 C -0.0620(9) 0.8464(9) 0.5195(8) 0.085(3) Uani 1 1 d . . . . .
H20A H -0.0703 0.8269 0.4654 0.102 Uiso 1 1 calc R U . . .
C21 C -0.1561(10) 0.8808(11) 0.5919(10) 0.101(4) Uani 1 1 d . . . . .
H21A H -0.2274 0.8844 0.5894 0.121 Uiso 1 1 calc R U . . .
C22 C -0.1398(12) 0.9108(12) 0.6709(11) 0.122(5) Uani 1 1 d . . . . .
H22A H -0.2021 0.9344 0.7231 0.146 Uiso 1 1 calc R U . . .
C23 C -0.0373(11) 0.9067(10) 0.6739(9) 0.094(3) Uani 1 1 d . . . . .
H23A H -0.0296 0.9296 0.7263 0.113 Uiso 1 1 calc R U . . .
C24 C 0.0564(9) 0.8687(8) 0.5998(8) 0.079(3) Uani 1 1 d . . . . .
C25 C 0.1787(12) 0.8851(12) 0.6857(10) 0.122(4) Uani 1 1 d . . . . .
H25A H 0.2554 0.8865 0.6717 0.184 Uiso 1 1 calc R U . . .
H25B H 0.1605 0.8309 0.7469 0.184 Uiso 1 1 calc R U . . .
H25C H 0.1294 0.9551 0.6956 0.184 Uiso 1 1 calc R U . . .
C26 C 0.6673(12) 0.4708(11) 0.4505(11) 0.108(4) Uani 1 1 d . . . . .
H26A H 0.6976 0.3979 0.4769 0.130 Uiso 1 1 calc R U . . .
C27 C 0.6796(11) 0.5548(13) 0.4724(9) 0.105(4) Uani 1 1 d . . . . .
H27A H 0.7172 0.5526 0.5184 0.126 Uiso 1 1 calc R U . . .
C28 C 0.6255(9) 0.6457(9) 0.4132(8) 0.082(3) Uani 1 1 d . . . . .
C29 C 0.6105(9) 0.7616(9) 0.3999(8) 0.079(3) Uani 1 1 d . . . . .
C30 C 0.6489(10) 0.8132(12) 0.4495(9) 0.100(4) Uani 1 1 d . . . . .
H30A H 0.6868 0.7722 0.4996 0.120 Uiso 1 1 calc R U . . .
C31 C 0.6297(12) 0.9251(13) 0.4231(12) 0.113(4) Uani 1 1 d . . . . .
H31A H 0.6544 0.9594 0.4560 0.136 Uiso 1 1 calc R U . . .
C32 C 0.5759(9) 0.9845(10) 0.3506(10) 0.090(3) Uani 1 1 d . . . . .
H32A H 0.5629 1.0598 0.3328 0.108 Uiso 1 1 calc R U . . .
C33 C 0.5402(8) 0.9317(9) 0.3029(8) 0.074(3) Uani 1 1 d . . . . .
C34 C 0.4822(8) 0.9844(8) 0.2226(8) 0.072(3) Uani 1 1 d . . . . .
C35 C 0.4423(8) 1.0917(9) 0.1743(10) 0.085(3) Uani 1 1 d . . . . .
H35A H 0.4486 1.1537 0.1864 0.102 Uiso 1 1 calc R U . . .
C36 C 0.3931(10) 1.0879(9) 0.1070(10) 0.091(3) Uani 1 1 d . . . . .
H36A H 0.3576 1.1469 0.0637 0.110 Uiso 1 1 calc R U . . .
Cl1 Cl 0.5235(3) 0.3372(3) 0.2765(3) 0.1088(10) Uani 1 1 d D U . . .
O3 O 0.6033(12) 0.323(2) 0.1940(10) 0.150(6) Uani 0.478(19) 1 d D U P A 1
O3B O 0.5918(14) 0.2523(15) 0.2203(14) 0.161(6) Uani 0.522(19) 1 d D U P A 2
O4 O 0.4234(8) 0.3254(11) 0.2892(10) 0.207(4) Uani 1 1 d D U . . .
O5 O 0.5590(9) 0.2952(8) 0.3647(7) 0.160(4) Uani 1 1 d D U . . .
O6 O 0.4918(19) 0.4509(9) 0.2762(18) 0.172(6) Uani 0.478(19) 1 d D U P A 1
O6B O 0.5513(18) 0.4235(13) 0.2188(15) 0.159(6) Uani 0.522(19) 1 d D U P A 2
Cl2 Cl 0.0905(3) 0.2247(3) 0.7778(3) 0.1099(11) Uani 1 1 d D U . . .
O7 O 0.1004(10) 0.1318(9) 0.7505(10) 0.193(4) Uani 1 1 d D U . . .
O8 O 0.1804(7) 0.2135(10) 0.8089(8) 0.162(4) Uani 1 1 d D U . . .
O9 O 0.0814(10) 0.3027(10) 0.6901(9) 0.214(5) Uani 1 1 d D U . . .
O10 O -0.0052(7) 0.2448(10) 0.8536(8) 0.179(4) Uani 1 1 d D U . . .
O1S O 0.3197(8) 0.9115(7) 0.0007(7) 0.109(3) Uani 1 1 d . . . . .
C2S C 0.1970(13) 0.8918(11) -0.0725(10) 0.127(5) Uani 1 1 d . . . . .
H2SA H 0.2647 0.8521 -0.1136 0.190 Uiso 1 1 calc R U . . .
H2SB H 0.1583 0.9513 -0.1169 0.190 Uiso 1 1 calc R U . . .
H2SC H 0.1490 0.8444 -0.0322 0.190 Uiso 1 1 calc R U . . .
C3S C 0.1338(12) 0.9998(15) 0.0644(13) 0.157(6) Uani 1 1 d . . . . .
H3SA H 0.1532 1.0645 0.0599 0.235 Uiso 1 1 calc R U . . .
H3SB H 0.1225 0.9585 0.1342 0.235 Uiso 1 1 calc R U . . .
H3SC H 0.0658 1.0194 0.0437 0.235 Uiso 1 1 calc R U . . .
C1S C 0.2258(11) 0.9339(10) -0.0039(9) 0.088(3) Uani 1 1 d . . . . .


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

loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
_geom_bond_publ_flag
Fe1 N3 2.107(7) . ?
Fe1 N7 2.141(8) . ?
Fe1 N9 2.146(7) . ?
Fe1 N8 2.147(8) . ?
Fe1 N2 2.203(8) . ?
Fe1 N4 2.216(7) . ?
O1 C2 1.369(14) . ?
O1 C1 1.400(14) . ?
O2 C24 1.380(12) . ?
O2 C25 1.439(13) . ?
N1 N2 1.329(10) . ?
N1 C8 1.357(12) . ?
N1 H1A 0.96(9) . ?
N2 C10 1.352(11) . ?
N3 C15 1.328(11) . ?
N3 C11 1.350(11) . ?
N4 N5 1.334(10) . ?
N4 C16 1.348(11) . ?
N5 C18 1.347(11) . ?
N5 H5B 0.95(10) . ?
N6 N7 1.342(11) . ?
N6 C26 1.342(16) . ?
N6 H6B 1.08(13) . ?
N7 C28 1.344(13) . ?
N8 C29 1.312(12) . ?
N8 C33 1.349(12) . ?
N9 N10 1.319(10) . ?
N9 C34 1.358(12) . ?
N10 C36 1.315(13) . ?
N10 H10A 1.01(11) . ?
C1 H1B 0.9600 . ?
C1 H1C 0.9600 . ?
C1 H1D 0.9600 . ?
C2 C3 1.360(16) . ?
C2 C7 1.410(15) . ?
C3 C4 1.399(19) . ?
C3 H3A 0.9300 . ?
C4 C5 1.330(18) . ?
C4 H4A 0.9300 . ?
C5 C6 1.394(15) . ?
C5 H5A 0.9300 . ?
C6 C7 1.380(14) . ?
C6 H6A 0.9300 . ?
C7 C8 1.466(13) . ?
C8 C9 1.371(13) . ?
C9 C10 1.407(12) . ?
C9 H9A 0.9300 . ?
C10 C11 1.442(12) . ?
C11 C12 1.406(13) . ?
C12 C13 1.393(13) . ?
C12 H12A 0.9300 . ?
C13 C14 1.384(14) . ?
C13 H13A 0.9300 . ?
C14 C15 1.383(13) . ?
C14 H14A 0.9300 . ?
C15 C16 1.450(13) . ?
C16 C17 1.388(12) . ?
C17 C18 1.404(13) . ?
C17 H17A 0.9300 . ?
C18 C19 1.468(13) . ?
C19 C24 1.370(14) . ?
C19 C20 1.386(14) . ?
C20 C21 1.347(14) . ?
C20 H20A 0.9300 . ?
C21 C22 1.398(18) . ?
C21 H21A 0.9300 . ?
C22 C23 1.338(17) . ?
C22 H22A 0.9300 . ?
C23 C24 1.372(14) . ?
C23 H23A 0.9300 . ?
C25 H25A 0.9600 . ?
C25 H25B 0.9600 . ?
C25 H25C 0.9600 . ?
C26 C27 1.326(18) . ?
C26 H26A 0.9300 . ?
C27 C28 1.371(15) . ?
C27 H27A 0.9300 . ?
C28 C29 1.456(15) . ?
C29 C30 1.413(15) . ?
C30 C31 1.382(17) . ?
C30 H30A 0.9300 . ?
C31 C32 1.339(16) . ?
C31 H31A 0.9300 . ?
C32 C33 1.381(14) . ?
C32 H32A 0.9300 . ?
C33 C34 1.449(14) . ?
C34 C35 1.391(14) . ?
C35 C36 1.341(15) . ?
C35 H35A 0.9300 . ?
C36 H36A 0.9300 . ?
Cl1 O6B 1.278(11) . ?
Cl1 O3 1.285(11) . ?
Cl1 O4 1.316(9) . ?
Cl1 O5 1.370(9) . ?
Cl1 O6 1.434(12) . ?
Cl1 O3B 1.449(11) . ?
Cl2 O8 1.340(8) . ?
Cl2 O10 1.347(8) . ?
Cl2 O9 1.365(10) . ?
Cl2 O7 1.366(9) . ?
O1S C1S 1.182(12) . ?
C2S C1S 1.460(16) . ?
C2S H2SA 0.9600 . ?
C2S H2SB 0.9600 . ?
C2S H2SC 0.9600 . ?
C3S C1S 1.471(16) . ?
C3S H3SA 0.9600 . ?
C3S H3SB 0.9600 . ?
C3S H3SC 0.9600 . ?

loop_
_geom_angle_atom_site_label_1
_geom_angle_atom_site_label_2
_geom_angle_atom_site_label_3
_geom_angle
_geom_angle_site_symmetry_1
_geom_angle_site_symmetry_3
_geom_angle_publ_flag
N3 Fe1 N7 112.6(3) . . ?
N3 Fe1 N9 98.8(3) . . ?
N7 Fe1 N9 148.5(3) . . ?
N3 Fe1 N8 172.0(3) . . ?
N7 Fe1 N8 74.0(3) . . ?
N9 Fe1 N8 74.5(3) . . ?
N3 Fe1 N2 75.5(3) . . ?
N7 Fe1 N2 92.1(3) . . ?
N9 Fe1 N2 97.3(3) . . ?
N8 Fe1 N2 109.5(3) . . ?
N3 Fe1 N4 73.8(3) . . ?
N7 Fe1 N4 97.8(3) . . ?
N9 Fe1 N4 89.2(3) . . ?
N8 Fe1 N4 101.3(3) . . ?
N2 Fe1 N4 149.2(3) . . ?
C2 O1 C1 119.8(10) . . ?
C24 O2 C25 117.7(9) . . ?
N2 N1 C8 114.2(8) . . ?
N2 N1 H1A 115(5) . . ?
C8 N1 H1A 123(5) . . ?
N1 N2 C10 104.6(7) . . ?
N1 N2 Fe1 141.9(6) . . ?
C10 N2 Fe1 113.4(6) . . ?
C15 N3 C11 120.7(8) . . ?
C15 N3 Fe1 120.9(6) . . ?
C11 N3 Fe1 118.4(6) . . ?
N5 N4 C16 104.7(7) . . ?
N5 N4 Fe1 140.5(6) . . ?
C16 N4 Fe1 114.5(6) . . ?
N4 N5 C18 113.7(8) . . ?
N4 N5 H5B 124(5) . . ?
C18 N5 H5B 123(5) . . ?
N7 N6 C26 110.3(12) . . ?
N7 N6 H6B 98(6) . . ?
C26 N6 H6B 152(6) . . ?
N6 N7 C28 104.8(9) . . ?
N6 N7 Fe1 138.3(8) . . ?
C28 N7 Fe1 116.5(7) . . ?
C29 N8 C33 122.4(9) . . ?
C29 N8 Fe1 119.3(7) . . ?
C33 N8 Fe1 118.3(7) . . ?
N10 N9 C34 103.9(8) . . ?
N10 N9 Fe1 138.9(6) . . ?
C34 N9 Fe1 116.8(6) . . ?
C36 N10 N9 114.0(10) . . ?
C36 N10 H10A 126(6) . . ?
N9 N10 H10A 119(6) . . ?
O1 C1 H1B 109.5 . . ?
O1 C1 H1C 109.5 . . ?
H1B C1 H1C 109.5 . . ?
O1 C1 H1D 109.5 . . ?
H1B C1 H1D 109.5 . . ?
H1C C1 H1D 109.5 . . ?
C3 C2 O1 124.5(12) . . ?
C3 C2 C7 119.3(13) . . ?
O1 C2 C7 116.1(9) . . ?
C2 C3 C4 122.5(14) . . ?
C2 C3 H3A 118.7 . . ?
C4 C3 H3A 118.7 . . ?
C5 C4 C3 117.9(13) . . ?
C5 C4 H4A 121.1 . . ?
C3 C4 H4A 121.1 . . ?
C4 C5 C6 121.6(13) . . ?
C4 C5 H5A 119.2 . . ?
C6 C5 H5A 119.2 . . ?
C7 C6 C5 121.1(12) . . ?
C7 C6 H6A 119.5 . . ?
C5 C6 H6A 119.5 . . ?
C6 C7 C2 117.5(10) . . ?
C6 C7 C8 121.4(10) . . ?
C2 C7 C8 121.0(10) . . ?
N1 C8 C9 104.9(8) . . ?
N1 C8 C7 122.0(9) . . ?
C9 C8 C7 133.2(9) . . ?
C8 C9 C10 106.6(8) . . ?
C8 C9 H9A 126.7 . . ?
C10 C9 H9A 126.7 . . ?
N2 C10 C9 109.8(8) . . ?
N2 C10 C11 117.8(8) . . ?
C9 C10 C11 132.5(9) . . ?
N3 C11 C12 120.9(8) . . ?
N3 C11 C10 114.9(8) . . ?
C12 C11 C10 124.2(9) . . ?
C13 C12 C11 117.6(9) . . ?
C13 C12 H12A 121.2 . . ?
C11 C12 H12A 121.2 . . ?
C14 C13 C12 120.3(9) . . ?
C14 C13 H13A 119.9 . . ?
C12 C13 H13A 119.9 . . ?
C15 C14 C13 118.8(9) . . ?
C15 C14 H14A 120.6 . . ?
C13 C14 H14A 120.6 . . ?
N3 C15 C14 121.6(9) . . ?
N3 C15 C16 113.8(8) . . ?
C14 C15 C16 124.5(9) . . ?
N4 C16 C17 111.1(8) . . ?
N4 C16 C15 116.9(8) . . ?
C17 C16 C15 131.9(9) . . ?
C16 C17 C18 105.3(9) . . ?
C16 C17 H17A 127.4 . . ?
C18 C17 H17A 127.4 . . ?
N5 C18 C17 105.2(8) . . ?
N5 C18 C19 125.4(9) . . ?
C17 C18 C19 129.4(9) . . ?
C24 C19 C20 116.8(10) . . ?
C24 C19 C18 122.8(10) . . ?
C20 C19 C18 120.4(10) . . ?
C21 C20 C19 124.5(11) . . ?
C21 C20 H20A 117.8 . . ?
C19 C20 H20A 117.8 . . ?
C20 C21 C22 115.8(11) . . ?
C20 C21 H21A 122.1 . . ?
C22 C21 H21A 122.1 . . ?
C23 C22 C21 122.1(12) . . ?
C23 C22 H22A 118.9 . . ?
C21 C22 H22A 118.9 . . ?
C22 C23 C24 120.1(12) . . ?
C22 C23 H23A 120.0 . . ?
C24 C23 H23A 120.0 . . ?
C19 C24 C23 120.6(11) . . ?
C19 C24 O2 116.3(9) . . ?
C23 C24 O2 123.1(10) . . ?
O2 C25 H25A 109.5 . . ?
O2 C25 H25B 109.5 . . ?
H25A C25 H25B 109.5 . . ?
O2 C25 H25C 109.5 . . ?
H25A C25 H25C 109.5 . . ?
H25B C25 H25C 109.5 . . ?
C27 C26 N6 108.6(12) . . ?
C27 C26 H26A 125.7 . . ?
N6 C26 H26A 125.7 . . ?
C26 C27 C28 105.8(12) . . ?
C26 C27 H27A 127.1 . . ?
C28 C27 H27A 127.1 . . ?
N7 C28 C27 110.4(11) . . ?
N7 C28 C29 116.5(10) . . ?
C27 C28 C29 133.1(13) . . ?
N8 C29 C30 118.2(11) . . ?
N8 C29 C28 113.5(10) . . ?
C30 C29 C28 128.2(11) . . ?
C31 C30 C29 119.4(11) . . ?
C31 C30 H30A 120.3 . . ?
C29 C30 H30A 120.3 . . ?
C32 C31 C30 120.6(11) . . ?
C32 C31 H31A 119.7 . . ?
C30 C31 H31A 119.7 . . ?
C31 C32 C33 118.6(11) . . ?
C31 C32 H32A 120.7 . . ?
C33 C32 H32A 120.7 . . ?
N8 C33 C32 120.7(10) . . ?
N8 C33 C34 114.1(9) . . ?
C32 C33 C34 125.1(10) . . ?
N9 C34 C35 109.1(9) . . ?
N9 C34 C33 116.1(9) . . ?
C35 C34 C33 134.9(10) . . ?
C36 C35 C34 106.2(10) . . ?
C36 C35 H35A 126.9 . . ?
C34 C35 H35A 126.9 . . ?
N10 C36 C35 106.7(10) . . ?
N10 C36 H36A 126.6 . . ?
C35 C36 H36A 126.6 . . ?
O6B Cl1 O4 120.0(9) . . ?
O3 Cl1 O4 121.5(10) . . ?
O6B Cl1 O5 116.3(9) . . ?
O3 Cl1 O5 113.5(9) . . ?
O4 Cl1 O5 112.7(7) . . ?
O3 Cl1 O6 106.6(9) . . ?
O4 Cl1 O6 98.8(8) . . ?
O5 Cl1 O6 99.6(8) . . ?
O6B Cl1 O3B 104.9(9) . . ?
O4 Cl1 O3B 98.7(8) . . ?
O5 Cl1 O3B 99.5(7) . . ?
O8 Cl2 O10 110.8(6) . . ?
O8 Cl2 O9 113.9(7) . . ?
O10 Cl2 O9 109.8(7) . . ?
O8 Cl2 O7 109.8(7) . . ?
O10 Cl2 O7 109.0(7) . . ?
O9 Cl2 O7 103.2(7) . . ?
C1S C2S H2SA 109.5 . . ?
C1S C2S H2SB 109.5 . . ?
H2SA C2S H2SB 109.5 . . ?
C1S C2S H2SC 109.5 . . ?
H2SA C2S H2SC 109.5 . . ?
H2SB C2S H2SC 109.5 . . ?
C1S C3S H3SA 109.5 . . ?
C1S C3S H3SB 109.5 . . ?
H3SA C3S H3SB 109.5 . . ?
C1S C3S H3SC 109.5 . . ?
H3SA C3S H3SC 109.5 . . ?
H3SB C3S H3SC 109.5 . . ?
O1S C1S C2S 121.1(12) . . ?
O1S C1S C3S 120.5(12) . . ?
C2S C1S C3S 118.3(12) . . ?

_refine_diff_density_max         0.773
_refine_diff_density_min         -0.448
_refine_diff_density_rms         0.101

_shelxl_version_number           2013-4

