# Electronic Supplementary Material (ESI) for Chemical Communications.
# This journal is © The Royal Society of Chemistry 2017

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

data_164no2ht
_database_code_depnum_ccdc_archive 'CCDC 1428759'
_audit_update_record             
;
2015-09-30 deposited with the CCDC.
2017-11-20 downloaded from the CCDC.
;

_audit_creation_method           SHELXL-97
_chemical_name_systematic        
'Bis[4-(isopropylsulfanyl)-2,6-di(pyrazol-1-yl)pyridine]iron(II)diperchlorate nitromethane solvate'
_chemical_name_common            ?
_chemical_melting_point          ?
_chemical_formula_moiety         'C28 H30 Fe N10 S2, 2(Cl O4), C H3 N O2'
_chemical_formula_sum            'C29 H33 Cl2 Fe N11 O10 S2'
_chemical_formula_weight         886.53

loop_
_atom_type_symbol
_atom_type_description
_atom_type_scat_dispersion_real
_atom_type_scat_dispersion_imag
_atom_type_scat_source
Cl Cl 0.3639 0.7018 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
C C 0.0181 0.0091 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
O O 0.0492 0.0322 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Fe Fe -1.1336 3.1974 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
N N 0.0311 0.0180 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
S S 0.3331 0.5567 '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'

_symmetry_cell_setting           monoclinic
_symmetry_space_group_name_H-M   'P 21/c'

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

_cell_length_a                   20.4604(4)
_cell_length_b                   11.9920(3)
_cell_length_c                   16.2456(4)
_cell_angle_alpha                90.00
_cell_angle_beta                 101.666(2)
_cell_angle_gamma                90.00
_cell_volume                     3903.70(16)
_cell_formula_units_Z            4
_cell_measurement_temperature    250(2)
_cell_measurement_reflns_used    7746
_cell_measurement_theta_min      4.31
_cell_measurement_theta_max      73.42

_exptl_crystal_description       'rectangular prism'
_exptl_crystal_colour            yellow
_exptl_crystal_size_max          0.19
_exptl_crystal_size_mid          0.14
_exptl_crystal_size_min          0.09
_exptl_crystal_density_meas      ?
_exptl_crystal_density_diffrn    1.508
_exptl_crystal_density_method    'not measured'
_exptl_crystal_F_000             1824
_exptl_absorpt_coefficient_mu    5.942
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_correction_T_min  0.700
_exptl_absorpt_correction_T_max  1.000
_exptl_absorpt_process_details   
; 
CrysAlisPro, Agilent Technologies,
Version 1.171.36.24 (release 03-12-2012 CrysAlis171 .NET)
Empirical absorption correction using spherical harmonics,
 implemented in SCALE3 ABSPACK scaling algorithm.
;

_diffrn_ambient_temperature      250(2)
_diffrn_radiation_wavelength     1.54184
_diffrn_radiation_type           CuK\a
_diffrn_radiation_source         'SuperNova (Cu) X-ray Source'
_diffrn_radiation_monochromator  mirror
_diffrn_measurement_device_type  'SuperNova, Dual, Cu at zero, Atlas'
_diffrn_measurement_method       'ω scans'
_diffrn_detector_area_resol_mean 5.3095
_diffrn_standards_number         0
_diffrn_standards_interval_count 0
_diffrn_standards_interval_time  0
_diffrn_standards_decay_%        0
_diffrn_reflns_number            18206
_diffrn_reflns_av_R_equivalents  0.0377
_diffrn_reflns_av_sigmaI/netI    0.0392
_diffrn_reflns_limit_h_min       -25
_diffrn_reflns_limit_h_max       25
_diffrn_reflns_limit_k_min       -11
_diffrn_reflns_limit_k_max       14
_diffrn_reflns_limit_l_min       -20
_diffrn_reflns_limit_l_max       17
_diffrn_reflns_theta_min         4.30
_diffrn_reflns_theta_max         73.84
_reflns_number_total             7485
_reflns_number_gt                6232
_reflns_threshold_expression     >2sigma(I)

_computing_data_collection       'CrysAlisPro, Agilent Technologies'
_computing_cell_refinement       'CrysAlisPro, Agilent Technologies'
_computing_data_reduction        'CrysAlisPro, Agilent Technologies'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_molecular_graphics    'XSEED (Barbour, 2001)'
_computing_publication_material  'local program'

_refine_special_details          
; 
 Refinement of F² against ALL reflections.  The weighted R-factor wR and 
 goodness of fit S are based on F², conventional R-factors R are based 
 on F, with F set to zero for negative F². The threshold expression of 
 F² > 2sigma(F²) is used only for calculating R-factors(gt) etc. and is 
 not relevant to the choice of reflections for refinement.  R-factors based 
 on F² are statistically about twice as large as those based on F, and R- 
 factors based on ALL data will be even larger. 

 One of the isopropyl substitutents on the complex cation is disordered over 
 two equally occupied orientations, which modelled successfuly without 
 restraints. Both ClO₄⁻ ions are also disordered, over two and three 
 equally occupied orientations respectively. The refined restraints Cl---O 
 = 1.43(2) and O...O = 2.34(2) Å were applied to those residues. Finally, 
 the nitromethane molecule is also disordered and was refined with three 
 sites with occupancies of 0.50, 0.3 and 0.2. These were modelled with the 
 fixed restraints C---N = 1.45(2), N---O = 1.22(2), O...O = 2.09(2) and 
 C...O = 2.32(2) Å. 

 All fully occupied non-H atoms, plus the two half-occupied Cl atoms, were 
 refined anisotropically, and H atoms were placed in calculated positions 
 and refined using a riding model.
;

_refine_ls_structure_factor_coef Fsqd
_refine_ls_matrix_type           full
_refine_ls_weighting_scheme      calc
_refine_ls_weighting_details     
'calc w=1/[σ²(Fo²)+(0.0862P)²+2.5537P] 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         7485
_refine_ls_number_parameters     533
_refine_ls_number_restraints     76
_refine_ls_R_factor_all          0.0650
_refine_ls_R_factor_gt           0.0550
_refine_ls_wR_factor_ref         0.1575
_refine_ls_wR_factor_gt          0.1479
_refine_ls_goodness_of_fit_ref   1.049
_refine_ls_restrained_S_all      1.081
_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_symmetry_multiplicity
_atom_site_calc_flag
_atom_site_refinement_flags
_atom_site_disorder_assembly
_atom_site_disorder_group
Fe1 Fe 0.22221(2) 0.60571(4) 0.06245(3) 0.03806(16) Uani 1 1 d . . .
N2 N 0.11670(12) 0.6297(2) 0.03788(16) 0.0358(5) Uani 1 1 d . . .
C3 C 0.08830(14) 0.7064(3) -0.01768(19) 0.0345(6) Uani 1 1 d . . .
C4 C 0.02212(15) 0.7366(3) -0.0287(2) 0.0393(7) Uani 1 1 d . . .
H4 H 0.0036 0.7902 -0.0689 0.047 Uiso 1 1 calc R . .
C5 C -0.01655(15) 0.6845(3) 0.0221(2) 0.0416(7) Uani 1 1 d . . .
C6 C 0.01275(17) 0.6043(3) 0.0802(2) 0.0441(7) Uani 1 1 d . . .
H6 H -0.0121 0.5680 0.1150 0.053 Uiso 1 1 calc R . .
C7 C 0.07897(15) 0.5802(3) 0.0850(2) 0.0380(7) Uani 1 1 d . . .
N8 N 0.13324(12) 0.7548(2) -0.06195(16) 0.0356(5) Uani 1 1 d . . .
N9 N 0.19968(12) 0.7315(2) -0.03608(17) 0.0404(6) Uani 1 1 d . . .
C10 C 0.23028(17) 0.7918(3) -0.0842(3) 0.0524(9) Uani 1 1 d . . .
H10 H 0.2767 0.7929 -0.0805 0.063 Uiso 1 1 calc R . .
C11 C 0.18416(19) 0.8546(4) -0.1422(3) 0.0556(9) Uani 1 1 d . . .
H11 H 0.1935 0.9040 -0.1833 0.067 Uiso 1 1 calc R . .
C12 C 0.12349(17) 0.8286(3) -0.1261(2) 0.0468(8) Uani 1 1 d . . .
H12 H 0.0822 0.8567 -0.1545 0.056 Uiso 1 1 calc R . .
N13 N 0.11419(14) 0.5011(2) 0.14116(18) 0.0425(6) Uani 1 1 d . . .
N14 N 0.18119(13) 0.4894(2) 0.14543(18) 0.0432(6) Uani 1 1 d . . .
C15 C 0.1994(2) 0.4071(3) 0.1985(2) 0.0554(9) Uani 1 1 d . . .
H15 H 0.2435 0.3807 0.2141 0.066 Uiso 1 1 calc R . .
C16 C 0.1454(2) 0.3635(4) 0.2291(3) 0.0630(11) Uani 1 1 d . . .
H16 H 0.1459 0.3049 0.2676 0.076 Uiso 1 1 calc R . .
C17 C 0.0916(2) 0.4251(3) 0.1904(3) 0.0546(9) Uani 1 1 d . . .
H17 H 0.0473 0.4163 0.1967 0.065 Uiso 1 1 calc R . .
S18 S -0.10105(4) 0.70903(9) 0.01832(7) 0.0561(3) Uani 1 1 d . . .
C19 C -0.11980(17) 0.8399(4) -0.0381(3) 0.0530(9) Uani 1 1 d . . .
H19 H -0.1043 0.8356 -0.0919 0.064 Uiso 1 1 calc R . .
C20 C -0.0867(2) 0.9372(4) 0.0118(3) 0.0731(12) Uani 1 1 d . . .
H20A H -0.0960 1.0048 -0.0213 0.110 Uiso 1 1 calc R . .
H20B H -0.0389 0.9250 0.0259 0.110 Uiso 1 1 calc R . .
H20C H -0.1039 0.9447 0.0630 0.110 Uiso 1 1 calc R . .
C21 C -0.1958(2) 0.8502(5) -0.0565(4) 0.0807(15) Uani 1 1 d . . .
H21A H -0.2116 0.8480 -0.0041 0.121 Uiso 1 1 calc R . .
H21B H -0.2153 0.7889 -0.0921 0.121 Uiso 1 1 calc R . .
H21C H -0.2088 0.9203 -0.0849 0.121 Uiso 1 1 calc R . .
N22 N 0.32548(12) 0.5798(2) 0.11218(15) 0.0344(5) Uani 1 1 d . . .
C23 C 0.35972(15) 0.5022(3) 0.08070(19) 0.0353(6) Uani 1 1 d . . .
C24 C 0.42500(16) 0.4760(3) 0.1143(2) 0.0412(7) Uani 1 1 d . . .
H24 H 0.4475 0.4197 0.0908 0.049 Uiso 1 1 calc R . .
C25 C 0.45674(15) 0.5365(3) 0.1849(2) 0.0434(7) Uani 1 1 d . A .
C26 C 0.42233(16) 0.6207(3) 0.2175(2) 0.0430(7) Uani 1 1 d . . .
H26 H 0.4428 0.6634 0.2641 0.052 Uiso 1 1 calc R . .
C27 C 0.35683(14) 0.6384(3) 0.17816(19) 0.0348(6) Uani 1 1 d . . .
N28 N 0.32186(12) 0.4502(2) 0.00907(16) 0.0374(6) Uani 1 1 d . . .
N29 N 0.25638(12) 0.4804(2) -0.01600(17) 0.0387(6) Uani 1 1 d . . .
C30 C 0.23468(17) 0.4252(3) -0.0862(2) 0.0458(8) Uani 1 1 d . . .
H30 H 0.1908 0.4294 -0.1176 0.055 Uiso 1 1 calc R . .
C31 C 0.2848(2) 0.3598(4) -0.1080(2) 0.0554(9) Uani 1 1 d . . .
H31 H 0.2814 0.3130 -0.1551 0.066 Uiso 1 1 calc R . .
C32 C 0.3400(2) 0.3785(3) -0.0462(2) 0.0539(9) Uani 1 1 d . . .
H32 H 0.3826 0.3473 -0.0430 0.065 Uiso 1 1 calc R . .
N33 N 0.31605(13) 0.7202(2) 0.20425(17) 0.0384(6) Uani 1 1 d . . .
N34 N 0.25174(13) 0.7299(2) 0.16064(18) 0.0426(6) Uani 1 1 d . . .
C35 C 0.22635(19) 0.8151(3) 0.1953(3) 0.0529(9) Uani 1 1 d . . .
H35 H 0.1825 0.8415 0.1780 0.063 Uiso 1 1 calc R . .
C36 C 0.2736(2) 0.8604(3) 0.2610(3) 0.0562(9) Uani 1 1 d . . .
H36 H 0.2677 0.9213 0.2952 0.067 Uiso 1 1 calc R . .
C37 C 0.32974(18) 0.7982(3) 0.2654(2) 0.0466(8) Uani 1 1 d . . .
H37 H 0.3704 0.8076 0.3037 0.056 Uiso 1 1 calc R . .
S38 S 0.53860(5) 0.49603(10) 0.22705(7) 0.0674(3) Uani 1 1 d D . .
C39A C 0.5691(4) 0.5801(7) 0.3164(5) 0.0414(18) Uiso 0.50 1 d PD A 1
H39A H 0.5339 0.5886 0.3497 0.050 Uiso 0.50 1 calc PR A 1
C40A C 0.5859(5) 0.6923(9) 0.2857(7) 0.068(3) Uiso 0.50 1 d PD A 1
H40A H 0.5452 0.7303 0.2594 0.103 Uiso 0.50 1 calc PR A 1
H40B H 0.6144 0.6831 0.2452 0.103 Uiso 0.50 1 calc PR A 1
H40C H 0.6091 0.7362 0.3329 0.103 Uiso 0.50 1 calc PR A 1
C41A C 0.6291(4) 0.5228(8) 0.3695(6) 0.058(2) Uiso 0.50 1 d PD A 1
H41A H 0.6169 0.4479 0.3832 0.087 Uiso 0.50 1 calc PR A 1
H41B H 0.6441 0.5647 0.4209 0.087 Uiso 0.50 1 calc PR A 1
H41C H 0.6648 0.5191 0.3383 0.087 Uiso 0.50 1 calc PR A 1
C39B C 0.5704(4) 0.6131(7) 0.3012(5) 0.048(2) Uiso 0.50 1 d PD A 2
H39B H 0.5380 0.6270 0.3379 0.057 Uiso 0.50 1 calc PR A 2
C40B C 0.5812(6) 0.7185(9) 0.2580(7) 0.076(3) Uiso 0.50 1 d PD A 2
H40D H 0.5403 0.7396 0.2197 0.113 Uiso 0.50 1 calc PR A 2
H40E H 0.6164 0.7078 0.2266 0.113 Uiso 0.50 1 calc PR A 2
H40F H 0.5941 0.7770 0.2993 0.113 Uiso 0.50 1 calc PR A 2
C41B C 0.6343(5) 0.5654(9) 0.3545(6) 0.069(3) Uiso 0.50 1 d PD A 2
H41D H 0.6250 0.4931 0.3764 0.103 Uiso 0.50 1 calc PR A 2
H41E H 0.6510 0.6155 0.4008 0.103 Uiso 0.50 1 calc PR A 2
H41F H 0.6676 0.5571 0.3200 0.103 Uiso 0.50 1 calc PR A 2
Cl42A Cl 0.4466(4) 0.7790(9) 0.4811(6) 0.038(2) Uani 0.34 1 d PD B 1
O43A O 0.4994(4) 0.8358(8) 0.5373(7) 0.047(2) Uiso 0.34 1 d PD B 1
O44A O 0.4105(6) 0.8736(8) 0.4451(6) 0.071(3) Uiso 0.34 1 d PD B 1
O45A O 0.4071(6) 0.7048(10) 0.5188(8) 0.087(3) Uiso 0.34 1 d PD B 1
O46A O 0.4805(7) 0.7212(12) 0.4243(8) 0.081(5) Uiso 0.34 1 d PD B 1
Cl42B Cl 0.4437(6) 0.7697(12) 0.4812(8) 0.065(6) Uiso 0.33 1 d PD C 2
O43B O 0.5052(7) 0.8239(14) 0.5135(10) 0.109(6) Uiso 0.33 1 d PD C 2
O44B O 0.3916(4) 0.8467(9) 0.4543(6) 0.0406(19) Uiso 0.33 1 d PD C 2
O45B O 0.4309(6) 0.6950(9) 0.5490(7) 0.071(3) Uiso 0.33 1 d PD C 2
O46B O 0.4524(5) 0.6936(9) 0.4160(6) 0.068(3) Uiso 0.33 1 d PD C 2
Cl42C Cl 0.4484(4) 0.7543(6) 0.4892(4) 0.047(3) Uiso 0.33 1 d PD D 3
O43C O 0.4709(5) 0.7420(9) 0.4085(6) 0.050(3) Uiso 0.33 1 d PD D 3
O44C O 0.4328(9) 0.6518(12) 0.5226(11) 0.142(7) Uiso 0.33 1 d PD D 3
O45C O 0.3871(5) 0.8170(10) 0.4707(7) 0.072(4) Uiso 0.33 1 d PD D 3
O46C O 0.5010(5) 0.7978(10) 0.5507(6) 0.066(3) Uiso 0.33 1 d PD D 3
Cl47A Cl 0.0767(4) 0.9981(10) 0.2291(5) 0.0555(18) Uani 0.50 1 d PD E 1
O48A O 0.1407(4) 1.0544(7) 0.2341(5) 0.067(2) Uiso 0.50 1 d PD E 1
O49A O 0.0301(4) 1.0877(6) 0.2126(5) 0.071(2) Uiso 0.50 1 d PD E 1
O50A O 0.0716(4) 0.9380(7) 0.3060(4) 0.063(2) Uiso 0.50 1 d PD E 1
O51A O 0.0694(4) 0.9172(7) 0.1634(5) 0.073(2) Uiso 0.50 1 d PD E 1
Cl47B Cl 0.0765(4) 0.9833(10) 0.2298(6) 0.0565(19) Uani 0.50 1 d PD F 2
O48B O 0.1392(3) 1.0257(7) 0.2221(5) 0.059(2) Uiso 0.50 1 d PD F 2
O49B O 0.0184(3) 1.0509(6) 0.1993(4) 0.0674(19) Uiso 0.50 1 d PD F 2
O50B O 0.0819(4) 0.9655(6) 0.3182(4) 0.0583(19) Uiso 0.50 1 d PD F 2
O51B O 0.0646(4) 0.8809(6) 0.1810(5) 0.075(2) Uiso 0.50 1 d PD F 2
C52A C 0.5767(8) 0.568(2) 0.5899(14) 0.113(8) Uiso 0.50 1 d PD G 1
H52A H 0.5528 0.5397 0.6315 0.169 Uiso 0.50 1 calc PR G 1
H52B H 0.5676 0.5204 0.5405 0.169 Uiso 0.50 1 calc PR G 1
H52C H 0.5621 0.6432 0.5743 0.169 Uiso 0.50 1 calc PR G 1
N53A N 0.6492(10) 0.568(2) 0.6255(16) 0.200(11) Uiso 0.50 1 d PD G 1
O54A O 0.6881(6) 0.5920(10) 0.5866(7) 0.122(4) Uiso 0.50 1 d PD G 1
O55A O 0.6698(11) 0.4899(19) 0.6765(13) 0.237(11) Uiso 0.50 1 d PD G 1
C52B C 0.5831(9) 0.572(3) 0.5595(13) 0.062(6) Uiso 0.20 1 d PD H 2
H52D H 0.5492 0.5733 0.5935 0.094 Uiso 0.20 1 calc PR H 2
H52E H 0.5711 0.5165 0.5153 0.094 Uiso 0.20 1 calc PR H 2
H52F H 0.5862 0.6445 0.5346 0.094 Uiso 0.20 1 calc PR H 2
N53B N 0.6487(6) 0.5418(12) 0.6133(8) 0.027(3) Uiso 0.20 1 d PD H 2
O54B O 0.6934(9) 0.534(2) 0.5854(13) 0.104(7) Uiso 0.20 1 d PD H 2
O55B O 0.6495(11) 0.563(2) 0.6925(10) 0.093(6) Uiso 0.20 1 d PD H 2
C52C C 0.5730(8) 0.5468(19) 0.5814(15) 0.060(5) Uiso 0.30 1 d PD I 3
H52G H 0.5747 0.5024 0.5320 0.090 Uiso 0.30 1 calc PR I 3
H52H H 0.5546 0.6197 0.5642 0.090 Uiso 0.30 1 calc PR I 3
H52I H 0.5451 0.5098 0.6147 0.090 Uiso 0.30 1 calc PR I 3
N53C N 0.6401(5) 0.5596(10) 0.6313(8) 0.039(3) Uiso 0.30 1 d PD I 3
O54C O 0.6703(6) 0.4635(10) 0.6521(8) 0.077(3) Uiso 0.30 1 d PD I 3
O55C O 0.6475(7) 0.6148(12) 0.6979(8) 0.088(4) Uiso 0.30 1 d PD I 3


_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 N22 2.127(2) . ?
Fe1 N2 2.134(2) . ?
Fe1 N29 2.176(3) . ?
Fe1 N34 2.177(3) . ?
Fe1 N9 2.180(3) . ?
Fe1 N14 2.219(3) . ?
N2 C7 1.332(4) . ?
N2 C3 1.336(4) . ?
C3 C4 1.378(4) . ?
C3 N8 1.402(4) . ?
C4 C5 1.400(5) . ?
C4 H4 0.9400 . ?
C5 C6 1.395(5) . ?
C5 S18 1.743(3) . ?
C6 C7 1.372(4) . ?
C6 H6 0.9400 . ?
C7 N13 1.409(4) . ?
N8 C12 1.351(4) . ?
N8 N9 1.368(3) . ?
N9 C10 1.313(4) . ?
C10 C11 1.409(5) . ?
C10 H10 0.9400 . ?
C11 C12 1.356(5) . ?
C11 H11 0.9400 . ?
C12 H12 0.9400 . ?
N13 C17 1.354(5) . ?
N13 N14 1.366(4) . ?
N14 C15 1.315(5) . ?
C15 C16 1.403(6) . ?
C15 H15 0.9400 . ?
C16 C17 1.368(6) . ?
C16 H16 0.9400 . ?
C17 H17 0.9400 . ?
S18 C19 1.819(4) . ?
C19 C20 1.502(6) . ?
C19 C21 1.528(5) . ?
C19 H19 0.9900 . ?
C20 H20A 0.9700 . ?
C20 H20B 0.9700 . ?
C20 H20C 0.9700 . ?
C21 H21A 0.9700 . ?
C21 H21B 0.9700 . ?
C21 H21C 0.9700 . ?
N22 C23 1.328(4) . ?
N22 C27 1.332(4) . ?
C23 C24 1.373(4) . ?
C23 N28 1.407(4) . ?
C24 C25 1.400(5) . ?
C24 H24 0.9400 . ?
C25 C26 1.395(5) . ?
C25 S38 1.745(3) . ?
C26 C27 1.379(4) . ?
C26 H26 0.9400 . ?
C27 N33 1.408(4) . ?
N28 C32 1.349(4) . ?
N28 N29 1.368(3) . ?
N29 C30 1.315(4) . ?
C30 C31 1.392(5) . ?
C30 H30 0.9400 . ?
C31 C32 1.370(5) . ?
C31 H31 0.9400 . ?
C32 H32 0.9400 . ?
N33 C37 1.351(4) . ?
N33 N34 1.367(4) . ?
N34 C35 1.322(4) . ?
C35 C36 1.397(6) . ?
C35 H35 0.9400 . ?
C36 C37 1.360(5) . ?
C36 H36 0.9400 . ?
C37 H37 0.9400 . ?
S38 C39A 1.774(7) . ?
S38 C39B 1.879(8) . ?
C39A C40A 1.499(11) . ?
C39A C41A 1.516(10) . ?
C39A H39A 0.9900 . ?
C40A H40A 0.9700 . ?
C40A H40B 0.9700 . ?
C40A H40C 0.9700 . ?
C41A H41A 0.9700 . ?
C41A H41B 0.9700 . ?
C41A H41C 0.9700 . ?
C39B C40B 1.485(12) . ?
C39B C41B 1.527(11) . ?
C39B H39B 0.9900 . ?
C40B H40D 0.9700 . ?
C40B H40E 0.9700 . ?
C40B H40F 0.9700 . ?
C41B H41D 0.9700 . ?
C41B H41E 0.9700 . ?
C41B H41F 0.9700 . ?
Cl42A O44A 1.414(12) . ?
Cl42A O45A 1.423(12) . ?
Cl42A O43A 1.437(11) . ?
Cl42A O46A 1.439(11) . ?
Cl42B O44B 1.411(13) . ?
Cl42B O43B 1.420(13) . ?
Cl42B O46B 1.436(13) . ?
Cl42B O45B 1.484(14) . ?
Cl42C O44C 1.406(12) . ?
Cl42C O46C 1.411(10) . ?
Cl42C O45C 1.441(11) . ?
Cl42C O43C 1.482(10) . ?
Cl47A O49A 1.426(11) . ?
Cl47A O51A 1.426(11) . ?
Cl47A O48A 1.461(11) . ?
Cl47A O50A 1.465(11) . ?
Cl47B O48B 1.410(11) . ?
Cl47B O50B 1.433(10) . ?
Cl47B O49B 1.442(10) . ?
Cl47B O51B 1.455(12) . ?
C52A N53A 1.479(16) . ?
C52A H52A 0.9700 . ?
C52A H52B 0.9700 . ?
C52A H52C 0.9700 . ?
N53A O54A 1.149(17) . ?
N53A O55A 1.262(17) . ?
C52B N53B 1.491(15) . ?
C52B H52D 0.9700 . ?
C52B H52E 0.9700 . ?
C52B H52F 0.9700 . ?
N53B O54B 1.104(15) . ?
N53B O55B 1.309(15) . ?
C52C N53C 1.453(13) . ?
C52C H52G 0.9700 . ?
C52C H52H 0.9700 . ?
C52C H52I 0.9700 . ?
N53C O55C 1.251(15) . ?
N53C O54C 1.320(13) . ?

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
N22 Fe1 N2 168.66(10) . . ?
N22 Fe1 N29 73.10(10) . . ?
N2 Fe1 N29 114.61(10) . . ?
N22 Fe1 N34 73.41(10) . . ?
N2 Fe1 N34 99.50(10) . . ?
N29 Fe1 N34 145.86(10) . . ?
N22 Fe1 N9 115.24(10) . . ?
N2 Fe1 N9 73.35(10) . . ?
N29 Fe1 N9 95.36(11) . . ?
N34 Fe1 N9 92.90(11) . . ?
N22 Fe1 N14 98.40(10) . . ?
N2 Fe1 N14 72.90(10) . . ?
N29 Fe1 N14 97.33(11) . . ?
N34 Fe1 N14 93.89(11) . . ?
N9 Fe1 N14 146.22(10) . . ?
C7 N2 C3 118.2(3) . . ?
C7 N2 Fe1 120.9(2) . . ?
C3 N2 Fe1 120.3(2) . . ?
N2 C3 C4 123.4(3) . . ?
N2 C3 N8 113.0(2) . . ?
C4 C3 N8 123.6(3) . . ?
C3 C4 C5 117.6(3) . . ?
C3 C4 H4 121.2 . . ?
C5 C4 H4 121.2 . . ?
C6 C5 C4 119.3(3) . . ?
C6 C5 S18 115.3(3) . . ?
C4 C5 S18 125.4(3) . . ?
C7 C6 C5 117.9(3) . . ?
C7 C6 H6 121.1 . . ?
C5 C6 H6 121.1 . . ?
N2 C7 C6 123.6(3) . . ?
N2 C7 N13 113.1(3) . . ?
C6 C7 N13 123.3(3) . . ?
C12 N8 N9 110.7(3) . . ?
C12 N8 C3 131.1(3) . . ?
N9 N8 C3 118.2(2) . . ?
C10 N9 N8 105.6(3) . . ?
C10 N9 Fe1 139.7(2) . . ?
N8 N9 Fe1 114.59(19) . . ?
N9 C10 C11 110.9(3) . . ?
N9 C10 H10 124.5 . . ?
C11 C10 H10 124.5 . . ?
C12 C11 C10 105.3(3) . . ?
C12 C11 H11 127.4 . . ?
C10 C11 H11 127.4 . . ?
N8 C12 C11 107.6(3) . . ?
N8 C12 H12 126.2 . . ?
C11 C12 H12 126.2 . . ?
C17 N13 N14 111.1(3) . . ?
C17 N13 C7 130.1(3) . . ?
N14 N13 C7 118.6(3) . . ?
C15 N14 N13 105.0(3) . . ?
C15 N14 Fe1 141.1(3) . . ?
N13 N14 Fe1 113.8(2) . . ?
N14 C15 C16 111.9(4) . . ?
N14 C15 H15 124.1 . . ?
C16 C15 H15 124.1 . . ?
C17 C16 C15 104.7(3) . . ?
C17 C16 H16 127.6 . . ?
C15 C16 H16 127.6 . . ?
N13 C17 C16 107.3(4) . . ?
N13 C17 H17 126.4 . . ?
C16 C17 H17 126.4 . . ?
C5 S18 C19 105.67(17) . . ?
C20 C19 C21 111.8(4) . . ?
C20 C19 S18 111.9(3) . . ?
C21 C19 S18 105.7(3) . . ?
C20 C19 H19 109.1 . . ?
C21 C19 H19 109.1 . . ?
S18 C19 H19 109.1 . . ?
C19 C20 H20A 109.5 . . ?
C19 C20 H20B 109.5 . . ?
H20A C20 H20B 109.5 . . ?
C19 C20 H20C 109.5 . . ?
H20A C20 H20C 109.5 . . ?
H20B C20 H20C 109.5 . . ?
C19 C21 H21A 109.5 . . ?
C19 C21 H21B 109.5 . . ?
H21A C21 H21B 109.5 . . ?
C19 C21 H21C 109.5 . . ?
H21A C21 H21C 109.5 . . ?
H21B C21 H21C 109.5 . . ?
C23 N22 C27 118.3(3) . . ?
C23 N22 Fe1 121.1(2) . . ?
C27 N22 Fe1 120.5(2) . . ?
N22 C23 C24 123.7(3) . . ?
N22 C23 N28 112.6(3) . . ?
C24 C23 N28 123.8(3) . . ?
C23 C24 C25 117.3(3) . . ?
C23 C24 H24 121.3 . . ?
C25 C24 H24 121.3 . . ?
C26 C25 C24 120.0(3) . . ?
C26 C25 S38 124.7(3) . . ?
C24 C25 S38 115.3(3) . . ?
C27 C26 C25 117.0(3) . . ?
C27 C26 H26 121.5 . . ?
C25 C26 H26 121.5 . . ?
N22 C27 C26 123.8(3) . . ?
N22 C27 N33 113.0(3) . . ?
C26 C27 N33 123.2(3) . . ?
C32 N28 N29 110.8(3) . . ?
C32 N28 C23 130.8(3) . . ?
N29 N28 C23 118.1(2) . . ?
C30 N29 N28 105.3(3) . . ?
C30 N29 Fe1 139.7(2) . . ?
N28 N29 Fe1 114.82(18) . . ?
N29 C30 C31 111.6(3) . . ?
N29 C30 H30 124.2 . . ?
C31 C30 H30 124.2 . . ?
C32 C31 C30 105.2(3) . . ?
C32 C31 H31 127.4 . . ?
C30 C31 H31 127.4 . . ?
N28 C32 C31 107.1(3) . . ?
N28 C32 H32 126.4 . . ?
C31 C32 H32 126.4 . . ?
C37 N33 N34 110.9(3) . . ?
C37 N33 C27 131.0(3) . . ?
N34 N33 C27 118.0(3) . . ?
C35 N34 N33 105.4(3) . . ?
C35 N34 Fe1 140.0(2) . . ?
N33 N34 Fe1 114.63(19) . . ?
N34 C35 C36 110.8(3) . . ?
N34 C35 H35 124.6 . . ?
C36 C35 H35 124.6 . . ?
C37 C36 C35 105.9(3) . . ?
C37 C36 H36 127.1 . . ?
C35 C36 H36 127.1 . . ?
N33 C37 C36 107.1(3) . . ?
N33 C37 H37 126.5 . . ?
C36 C37 H37 126.5 . . ?
C25 S38 C39A 108.3(3) . . ?
C25 S38 C39B 103.0(3) . . ?
C40A C39A C41A 112.4(7) . . ?
C40A C39A S38 107.7(6) . . ?
C41A C39A S38 108.5(6) . . ?
C40A C39A H39A 109.4 . . ?
C41A C39A H39A 109.4 . . ?
S38 C39A H39A 109.4 . . ?
C39A C40A H40A 109.5 . . ?
C39A C40A H40B 109.5 . . ?
H40A C40A H40B 109.5 . . ?
C39A C40A H40C 109.5 . . ?
H40A C40A H40C 109.5 . . ?
H40B C40A H40C 109.5 . . ?
C39A C41A H41A 109.5 . . ?
C39A C41A H41B 109.5 . . ?
H41A C41A H41B 109.5 . . ?
C39A C41A H41C 109.5 . . ?
H41A C41A H41C 109.5 . . ?
H41B C41A H41C 109.5 . . ?
C40B C39B C41B 113.2(8) . . ?
C40B C39B S38 113.5(6) . . ?
C41B C39B S38 103.2(6) . . ?
C40B C39B H39B 108.9 . . ?
C41B C39B H39B 108.9 . . ?
S38 C39B H39B 108.9 . . ?
C39B C40B H40D 109.5 . . ?
C39B C40B H40E 109.5 . . ?
H40D C40B H40E 109.5 . . ?
C39B C40B H40F 109.5 . . ?
H40D C40B H40F 109.5 . . ?
H40E C40B H40F 109.5 . . ?
C39B C41B H41D 109.5 . . ?
C39B C41B H41E 109.5 . . ?
H41D C41B H41E 109.5 . . ?
C39B C41B H41F 109.5 . . ?
H41D C41B H41F 109.5 . . ?
H41E C41B H41F 109.5 . . ?
O44A Cl42A O45A 112.6(8) . . ?
O44A Cl42A O43A 98.4(8) . . ?
O45A Cl42A O43A 116.3(10) . . ?
O44A Cl42A O46A 113.6(9) . . ?
O45A Cl42A O46A 111.3(10) . . ?
O43A Cl42A O46A 103.8(8) . . ?
O44B Cl42B O43B 111.8(12) . . ?
O44B Cl42B O46B 112.7(10) . . ?
O43B Cl42B O46B 109.3(11) . . ?
O44B Cl42B O45B 113.0(10) . . ?
O43B Cl42B O45B 106.2(11) . . ?
O46B Cl42B O45B 103.4(10) . . ?
O44C Cl42C O46C 104.5(9) . . ?
O44C Cl42C O45C 106.3(10) . . ?
O46C Cl42C O45C 117.5(8) . . ?
O44C Cl42C O43C 113.0(10) . . ?
O46C Cl42C O43C 109.5(8) . . ?
O45C Cl42C O43C 106.3(7) . . ?
O49A Cl47A O51A 114.0(6) . . ?
O49A Cl47A O48A 102.7(9) . . ?
O51A Cl47A O48A 108.3(7) . . ?
O49A Cl47A O50A 111.8(7) . . ?
O51A Cl47A O50A 106.8(9) . . ?
O48A Cl47A O50A 113.4(6) . . ?
O48B Cl47B O50B 104.8(7) . . ?
O48B Cl47B O49B 118.0(9) . . ?
O50B Cl47B O49B 108.7(7) . . ?
O48B Cl47B O51B 108.1(7) . . ?
O50B Cl47B O51B 113.0(9) . . ?
O49B Cl47B O51B 104.6(7) . . ?
N53A C52A H52A 109.5 . . ?
N53A C52A H52B 109.5 . . ?
H52A C52A H52B 109.5 . . ?
N53A C52A H52C 109.5 . . ?
H52A C52A H52C 109.5 . . ?
H52B C52A H52C 109.5 . . ?
O54A N53A O55A 111.8(19) . . ?
O54A N53A C52A 122(2) . . ?
O55A N53A C52A 115.7(18) . . ?
N53B C52B H52D 109.5 . . ?
N53B C52B H52E 109.5 . . ?
H52D C52B H52E 109.5 . . ?
N53B C52B H52F 109.5 . . ?
H52D C52B H52F 109.5 . . ?
H52E C52B H52F 109.5 . . ?
O54B N53B O55B 125.1(16) . . ?
O54B N53B C52B 120.2(15) . . ?
O55B N53B C52B 111.1(14) . . ?
N53C C52C H52G 109.5 . . ?
N53C C52C H52H 109.5 . . ?
H52G C52C H52H 109.5 . . ?
N53C C52C H52I 109.5 . . ?
H52G C52C H52I 109.5 . . ?
H52H C52C H52I 109.5 . . ?
O55C N53C O54C 105.8(11) . . ?
O55C N53C C52C 118.3(13) . . ?
O54C N53C C52C 113.0(12) . . ?

_diffrn_measured_fraction_theta_max 0.947
_diffrn_reflns_theta_full        73.84
_diffrn_measured_fraction_theta_full 0.947
_refine_diff_density_max         0.581
_refine_diff_density_min         -0.689
_refine_diff_density_rms         0.071
_exptl_crystal_recrystallization_method 
'Re-crystallisation from solvent: Nitromethane-diethyl ether'
_exptl_crystal_preparation       'Magnetic properties'
####################################################################### 
# 
# This file contains crystal structure data downloaded from the 
# Cambridge Structural Database (CSD) hosted by the Cambridge 
# Crystallographic Data Centre (CCDC).
# 
# Full information about CCDC data access policies and citation 
# guidelines are available at http://www.ccdc.cam.ac.uk/access/V1 
# 
# Audit and citation data items may have been added by the CCDC. 
# Please retain this information to preserve the provenance of 
# this file and to allow appropriate attribution of the data. 
# 
#######################################################################

data_164no2lt
_database_code_depnum_ccdc_archive 'CCDC 1428760'
_audit_update_record             
;
2015-09-30 deposited with the CCDC.
2017-11-20 downloaded from the CCDC.
;

_audit_creation_method           SHELXL-97
_chemical_name_systematic        
'Bis[4-(isopropylsulfanyl)-2,6-di(pyrazol-1-yl)pyridine]iron(II)diperchlorate nitromethane solvate'
_chemical_name_common            ?
_chemical_melting_point          ?
_chemical_formula_moiety         'C28 H30 Fe N10 S2, 2(Cl O4), C H3 N O2'
_chemical_formula_sum            'C29 H33 Cl2 Fe N11 O10 S2'
_chemical_formula_weight         886.53

loop_
_atom_type_symbol
_atom_type_description
_atom_type_scat_dispersion_real
_atom_type_scat_dispersion_imag
_atom_type_scat_source
Cl Cl 0.3639 0.7018 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
C C 0.0181 0.0091 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
O O 0.0492 0.0322 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Fe Fe -1.1336 3.1974 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
N N 0.0311 0.0180 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
S S 0.3331 0.5567 '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'

_symmetry_cell_setting           monoclinic
_symmetry_space_group_name_H-M   'P 21/c'

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

_cell_length_a                   20.4690(2)
_cell_length_b                   11.9404(2)
_cell_length_c                   15.9241(2)
_cell_angle_alpha                90.00
_cell_angle_beta                 101.7890(10)
_cell_angle_gamma                90.00
_cell_volume                     3809.88(9)
_cell_formula_units_Z            4
_cell_measurement_temperature    150(2)
_cell_measurement_reflns_used    9367
_cell_measurement_theta_min      4.30
_cell_measurement_theta_max      73.63

_exptl_crystal_description       'rectangular prism'
_exptl_crystal_colour            yellow
_exptl_crystal_size_max          0.19
_exptl_crystal_size_mid          0.14
_exptl_crystal_size_min          0.09
_exptl_crystal_density_meas      ?
_exptl_crystal_density_diffrn    1.546
_exptl_crystal_density_method    'not measured'
_exptl_crystal_F_000             1824
_exptl_absorpt_coefficient_mu    6.089
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_correction_T_min  0.734
_exptl_absorpt_correction_T_max  1.000
_exptl_absorpt_process_details   
; 
CrysAlisPro, Agilent Technologies,
Version 1.171.36.24 (release 03-12-2012 CrysAlis171 .NET)
Empirical absorption correction using spherical harmonics,
 implemented in SCALE3 ABSPACK scaling algorithm.
;

_diffrn_ambient_temperature      150(2)
_diffrn_radiation_wavelength     1.54184
_diffrn_radiation_type           CuK\a
_diffrn_radiation_source         'SuperNova (Cu) X-ray Source'
_diffrn_radiation_monochromator  mirror
_diffrn_measurement_device_type  'SuperNova, Dual, Cu at zero, Atlas'
_diffrn_measurement_method       'ω scans'
_diffrn_detector_area_resol_mean 5.3095
_diffrn_standards_number         0
_diffrn_standards_interval_count 0
_diffrn_standards_interval_time  0
_diffrn_standards_decay_%        0
_diffrn_reflns_number            16738
_diffrn_reflns_av_R_equivalents  0.0384
_diffrn_reflns_av_sigmaI/netI    0.0391
_diffrn_reflns_limit_h_min       -24
_diffrn_reflns_limit_h_max       24
_diffrn_reflns_limit_k_min       -11
_diffrn_reflns_limit_k_max       14
_diffrn_reflns_limit_l_min       -19
_diffrn_reflns_limit_l_max       16
_diffrn_reflns_theta_min         4.31
_diffrn_reflns_theta_max         67.08
_reflns_number_total             6672
_reflns_number_gt                6049
_reflns_threshold_expression     >2sigma(I)

_computing_data_collection       'CrysAlisPro, Agilent Technologies'
_computing_cell_refinement       'CrysAlisPro, Agilent Technologies'
_computing_data_reduction        'CrysAlisPro, Agilent Technologies'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_molecular_graphics    'XSEED (Barbour, 2001)'
_computing_publication_material  'local program'

_refine_special_details          
; 
 Refinement of F² against ALL reflections.  The weighted R-factor wR and 
 goodness of fit S are based on F², conventional R-factors R are based 
 on F, with F set to zero for negative F². The threshold expression of 
 F² > 2sigma(F²) is used only for calculating R-factors(gt) etc. and is 
 not relevant to the choice of reflections for refinement.  R-factors based 
 on F² are statistically about twice as large as those based on F, and R- 
 factors based on ALL data will be even larger. 

 One ClO₄⁻ ion is disordered, over two equally occupied sites. The 
 refined restraints Cl---O = 1.42(2) and O...O = 2.32(2) Å were applied 
 to those residues. The nitromethane was disordered, and modelled over 
 three sites with occupancies of 0.40, 0.40 and 0.20. The fixed restraints 
 C---N = 1.45(2), N---O = 1.22(2), O...O = 2.09(2) and C...O = 2.32(2) Å
 were applied to those residues. 

 All wholly occupied non-H atoms, plus the two half-occupied Cl atoms, were 
 refined anisotropically, and H atoms were placed in calculated positions 
 and refined using a riding model.
;

_refine_ls_structure_factor_coef Fsqd
_refine_ls_matrix_type           full
_refine_ls_weighting_scheme      calc
_refine_ls_weighting_details     
'calc w=1/[σ²(Fo²)+(0.0719P)²+2.5680P] 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         6672
_refine_ls_number_parameters     518
_refine_ls_number_restraints     38
_refine_ls_R_factor_all          0.0488
_refine_ls_R_factor_gt           0.0445
_refine_ls_wR_factor_ref         0.1223
_refine_ls_wR_factor_gt          0.1180
_refine_ls_goodness_of_fit_ref   1.035
_refine_ls_restrained_S_all      1.065
_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_symmetry_multiplicity
_atom_site_calc_flag
_atom_site_refinement_flags
_atom_site_disorder_assembly
_atom_site_disorder_group
Fe1 Fe 0.222168(19) 0.60184(4) 0.06510(3) 0.02327(13) Uani 1 1 d . . .
N2 N 0.11709(10) 0.62748(18) 0.04006(14) 0.0220(4) Uani 1 1 d . . .
C3 C 0.08890(13) 0.7050(2) -0.01609(16) 0.0213(5) Uani 1 1 d . . .
C4 C 0.02254(13) 0.7354(2) -0.02805(17) 0.0233(5) Uani 1 1 d . . .
H4 H 0.0039 0.7901 -0.0694 0.028 Uiso 1 1 calc R . .
C5 C -0.01604(13) 0.6825(2) 0.02312(17) 0.0252(5) Uani 1 1 d . . .
C6 C 0.01289(14) 0.6014(2) 0.08253(18) 0.0271(6) Uani 1 1 d . . .
H6 H -0.0124 0.5644 0.1180 0.033 Uiso 1 1 calc R . .
C7 C 0.07899(13) 0.5771(2) 0.08772(16) 0.0234(5) Uani 1 1 d . . .
N8 N 0.13412(10) 0.75439(18) -0.06040(13) 0.0217(4) Uani 1 1 d . . .
N9 N 0.20052(11) 0.7299(2) -0.03345(14) 0.0254(5) Uani 1 1 d . . .
C10 C 0.23163(14) 0.7928(3) -0.08138(19) 0.0317(6) Uani 1 1 d . . .
H10 H 0.2786 0.7941 -0.0769 0.038 Uiso 1 1 calc R . .
C11 C 0.18613(15) 0.8573(3) -0.1397(2) 0.0344(6) Uani 1 1 d . . .
H11 H 0.1960 0.9089 -0.1808 0.041 Uiso 1 1 calc R . .
C12 C 0.12470(14) 0.8302(2) -0.12483(18) 0.0281(6) Uani 1 1 d . . .
H12 H 0.0831 0.8593 -0.1543 0.034 Uiso 1 1 calc R . .
N13 N 0.11408(11) 0.49730(19) 0.14465(14) 0.0259(5) Uani 1 1 d . . .
N14 N 0.18117(11) 0.4857(2) 0.14976(15) 0.0269(5) Uani 1 1 d . . .
C15 C 0.19939(16) 0.4024(3) 0.20384(19) 0.0351(7) Uani 1 1 d . . .
H15 H 0.2439 0.3759 0.2206 0.042 Uiso 1 1 calc R . .
C16 C 0.14473(17) 0.3580(3) 0.2335(2) 0.0387(7) Uani 1 1 d . . .
H16 H 0.1450 0.2974 0.2722 0.046 Uiso 1 1 calc R . .
C17 C 0.09126(16) 0.4207(3) 0.19483(19) 0.0330(6) Uani 1 1 d . . .
H17 H 0.0465 0.4123 0.2017 0.040 Uiso 1 1 calc R . .
S18 S -0.10086(3) 0.70689(6) 0.01884(5) 0.03211(18) Uani 1 1 d . . .
C19 C -0.11957(13) 0.8385(3) -0.03942(19) 0.0312(6) Uani 1 1 d . . .
H19 H -0.1042 0.8341 -0.0951 0.037 Uiso 1 1 calc R . .
C20 C -0.08573(16) 0.9358(3) 0.0123(2) 0.0396(7) Uani 1 1 d . . .
H20A H -0.0957 1.0051 -0.0209 0.059 Uiso 1 1 calc R . .
H20B H -0.0374 0.9235 0.0256 0.059 Uiso 1 1 calc R . .
H20C H -0.1021 0.9421 0.0658 0.059 Uiso 1 1 calc R . .
C21 C -0.19529(15) 0.8493(3) -0.0571(2) 0.0456(8) Uani 1 1 d . . .
H21A H -0.2104 0.8525 -0.0026 0.068 Uiso 1 1 calc R . .
H21B H -0.2154 0.7844 -0.0902 0.068 Uiso 1 1 calc R . .
H21C H -0.2087 0.9180 -0.0898 0.068 Uiso 1 1 calc R . .
N22 N 0.32522(10) 0.57394(19) 0.11512(14) 0.0223(4) Uani 1 1 d . . .
C23 C 0.35877(13) 0.4947(2) 0.08286(17) 0.0231(5) Uani 1 1 d . . .
C24 C 0.42365(14) 0.4666(2) 0.11699(18) 0.0270(6) Uani 1 1 d . . .
H24 H 0.4458 0.4089 0.0926 0.032 Uiso 1 1 calc R . .
C25 C 0.45613(13) 0.5263(2) 0.18937(18) 0.0284(6) Uani 1 1 d . . .
C26 C 0.42254(14) 0.6122(2) 0.22233(18) 0.0281(6) Uani 1 1 d . . .
H26 H 0.4438 0.6553 0.2703 0.034 Uiso 1 1 calc R . .
C27 C 0.35715(13) 0.6319(2) 0.18234(17) 0.0232(5) Uani 1 1 d . . .
N28 N 0.32013(11) 0.44412(19) 0.00916(14) 0.0244(5) Uani 1 1 d . . .
N29 N 0.25488(11) 0.47592(19) -0.01574(14) 0.0250(5) Uani 1 1 d . . .
C30 C 0.23243(14) 0.4226(3) -0.08872(18) 0.0309(6) Uani 1 1 d . . .
H30 H 0.1882 0.4285 -0.1213 0.037 Uiso 1 1 calc R . .
C31 C 0.28229(16) 0.3565(3) -0.1116(2) 0.0356(7) Uani 1 1 d . . .
H31 H 0.2786 0.3099 -0.1607 0.043 Uiso 1 1 calc R . .
C32 C 0.33772(15) 0.3728(3) -0.0481(2) 0.0334(6) Uani 1 1 d . . .
H32 H 0.3805 0.3402 -0.0451 0.040 Uiso 1 1 calc R . .
N33 N 0.31734(11) 0.71553(19) 0.20869(14) 0.0238(5) Uani 1 1 d . . .
N34 N 0.25292(11) 0.7269(2) 0.16400(15) 0.0267(5) Uani 1 1 d . . .
C35 C 0.22861(15) 0.8135(2) 0.19920(19) 0.0327(6) Uani 1 1 d . . .
H35 H 0.1845 0.8414 0.1816 0.039 Uiso 1 1 calc R . .
C36 C 0.27671(16) 0.8588(3) 0.2659(2) 0.0345(6) Uani 1 1 d . . .
H36 H 0.2716 0.9213 0.3010 0.041 Uiso 1 1 calc R . .
C37 C 0.33220(14) 0.7948(2) 0.27007(18) 0.0292(6) Uani 1 1 d . . .
H37 H 0.3737 0.8041 0.3089 0.035 Uiso 1 1 calc R . .
S38 S 0.53723(4) 0.48257(7) 0.23334(5) 0.0421(2) Uani 1 1 d . . .
C39 C 0.57065(15) 0.5882(3) 0.3137(2) 0.0443(9) Uani 1 1 d . . .
H39 H 0.5378 0.6022 0.3512 0.053 Uiso 1 1 calc R . .
C40 C 0.58420(19) 0.6957(4) 0.2714(3) 0.0605(11) Uani 1 1 d . . .
H40A H 0.6036 0.7503 0.3154 0.091 Uiso 1 1 calc R . .
H40B H 0.5423 0.7253 0.2376 0.091 Uiso 1 1 calc R . .
H40C H 0.6155 0.6816 0.2336 0.091 Uiso 1 1 calc R . .
C41 C 0.63417(17) 0.5363(4) 0.3673(3) 0.0605(12) Uani 1 1 d . . .
H41A H 0.6665 0.5231 0.3307 0.091 Uiso 1 1 calc R . .
H41B H 0.6232 0.4650 0.3916 0.091 Uiso 1 1 calc R . .
H41C H 0.6534 0.5876 0.4138 0.091 Uiso 1 1 calc R . .
Cl42A Cl 0.4510(5) 0.7835(7) 0.4851(6) 0.0276(11) Uani 0.50 1 d PD A 1
O43A O 0.5032(3) 0.8425(5) 0.5367(4) 0.0423(16) Uiso 0.50 1 d PD A 1
O44A O 0.4033(3) 0.8695(5) 0.4539(3) 0.0439(13) Uiso 0.50 1 d PD A 1
O45A O 0.4150(4) 0.7000(6) 0.5244(5) 0.075(2) Uiso 0.50 1 d PD A 1
O46A O 0.4764(2) 0.7388(4) 0.4164(3) 0.0291(12) Uiso 0.50 1 d PD A 1
Cl42B Cl 0.4472(5) 0.7651(7) 0.4959(6) 0.0270(11) Uani 0.50 1 d PD B 2
O43B O 0.5033(3) 0.8152(5) 0.5525(4) 0.0419(16) Uiso 0.50 1 d PD B 2
O44B O 0.3910(2) 0.8356(4) 0.4674(3) 0.0334(10) Uiso 0.50 1 d PD B 2
O45B O 0.4329(4) 0.6802(6) 0.5474(4) 0.0596(17) Uiso 0.50 1 d PD B 2
O46B O 0.4662(3) 0.7114(6) 0.4228(4) 0.054(2) Uiso 0.50 1 d PD B 2
Cl47 Cl 0.07647(3) 0.98308(6) 0.22614(4) 0.03238(17) Uani 1 1 d . . .
O48 O 0.13955(11) 1.0345(2) 0.22517(14) 0.0418(5) Uani 1 1 d . . .
O49 O 0.02360(12) 1.0629(2) 0.20025(17) 0.0536(7) Uani 1 1 d . . .
O50 O 0.07612(12) 0.9465(2) 0.31200(14) 0.0456(6) Uani 1 1 d . . .
O51 O 0.06686(13) 0.8898(2) 0.16873(17) 0.0540(7) Uani 1 1 d . . .
C52A C 0.5712(4) 0.5495(10) 0.5866(9) 0.038(4) Uiso 0.40 1 d PD C 1
H52A H 0.5504 0.5019 0.6239 0.057 Uiso 0.40 1 calc PR C 1
H52B H 0.5608 0.5202 0.5279 0.057 Uiso 0.40 1 calc PR C 1
H52C H 0.5540 0.6260 0.5871 0.057 Uiso 0.40 1 calc PR C 1
N53A N 0.6436(3) 0.5503(6) 0.6176(5) 0.0222(18) Uiso 0.40 1 d PD C 1
O54A O 0.6857(5) 0.6018(9) 0.5902(7) 0.092(3) Uiso 0.40 1 d PD C 1
O55A O 0.6693(3) 0.4602(6) 0.6555(5) 0.0454(18) Uiso 0.40 1 d PD C 1
C52B C 0.5739(5) 0.5567(11) 0.5696(7) 0.029(3) Uiso 0.40 1 d PD D 2
H52D H 0.5706 0.4870 0.5365 0.044 Uiso 0.40 1 calc PR D 2
H52E H 0.5758 0.6204 0.5314 0.044 Uiso 0.40 1 calc PR D 2
H52F H 0.5346 0.5642 0.5956 0.044 Uiso 0.40 1 calc PR D 2
N53B N 0.6353(4) 0.5545(6) 0.6383(5) 0.030(2) Uiso 0.40 1 d PD D 2
O54B O 0.6474(4) 0.6262(7) 0.6891(5) 0.0476(19) Uiso 0.40 1 d PD D 2
O55B O 0.6725(5) 0.4786(9) 0.6274(8) 0.080(3) Uiso 0.40 1 d PD D 2
C52C C 0.5823(11) 0.594(3) 0.5732(18) 0.117(16) Uiso 0.20 1 d PD E 3
H52G H 0.5855 0.5927 0.5126 0.175 Uiso 0.20 1 calc PR E 3
H52H H 0.5526 0.6553 0.5826 0.175 Uiso 0.20 1 calc PR E 3
H52I H 0.5642 0.5228 0.5885 0.175 Uiso 0.20 1 calc PR E 3
N53C N 0.6548(10) 0.6136(17) 0.6315(12) 0.081(6) Uiso 0.20 1 d PD E 3
O54C O 0.6868(8) 0.5371(16) 0.5983(10) 0.063(4) Uiso 0.20 1 d PD E 3
O55C O 0.6468(7) 0.5922(13) 0.7063(8) 0.045(4) Uiso 0.20 1 d PD E 3


_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 N22 2.123(2) . ?
Fe1 N2 2.128(2) . ?
Fe1 N34 2.168(2) . ?
Fe1 N9 2.170(2) . ?
Fe1 N29 2.172(2) . ?
Fe1 N14 2.215(2) . ?
N2 C3 1.333(3) . ?
N2 C7 1.337(4) . ?
C3 C4 1.381(4) . ?
C3 N8 1.404(3) . ?
C4 C5 1.396(4) . ?
C4 H4 0.9500 . ?
C5 C6 1.398(4) . ?
C5 S18 1.748(3) . ?
C6 C7 1.369(4) . ?
C6 H6 0.9500 . ?
C7 N13 1.407(3) . ?
N8 C12 1.352(4) . ?
N8 N9 1.371(3) . ?
N9 C10 1.323(4) . ?
C10 C11 1.403(4) . ?
C10 H10 0.9500 . ?
C11 C12 1.365(4) . ?
C11 H11 0.9500 . ?
C12 H12 0.9500 . ?
N13 C17 1.359(4) . ?
N13 N14 1.366(3) . ?
N14 C15 1.318(4) . ?
C15 C16 1.404(5) . ?
C15 H15 0.9500 . ?
C16 C17 1.364(5) . ?
C16 H16 0.9500 . ?
C17 H17 0.9500 . ?
S18 C19 1.826(3) . ?
C19 C20 1.508(5) . ?
C19 C21 1.523(4) . ?
C19 H19 1.0000 . ?
C20 H20A 0.9800 . ?
C20 H20B 0.9800 . ?
C20 H20C 0.9800 . ?
C21 H21A 0.9800 . ?
C21 H21B 0.9800 . ?
C21 H21C 0.9800 . ?
N22 C27 1.329(3) . ?
N22 C23 1.333(3) . ?
C23 C24 1.370(4) . ?
C23 N28 1.410(3) . ?
C24 C25 1.402(4) . ?
C24 H24 0.9500 . ?
C25 C26 1.396(4) . ?
C25 S38 1.745(3) . ?
C26 C27 1.380(4) . ?
C26 H26 0.9500 . ?
C27 N33 1.406(3) . ?
N28 C32 1.349(4) . ?
N28 N29 1.367(3) . ?
N29 C30 1.323(4) . ?
C30 C31 1.396(5) . ?
C30 H30 0.9500 . ?
C31 C32 1.370(4) . ?
C31 H31 0.9500 . ?
C32 H32 0.9500 . ?
N33 C37 1.350(4) . ?
N33 N34 1.371(3) . ?
N34 C35 1.322(4) . ?
C35 C36 1.401(4) . ?
C35 H35 0.9500 . ?
C36 C37 1.360(4) . ?
C36 H36 0.9500 . ?
C37 H37 0.9500 . ?
S38 C39 1.827(3) . ?
C39 C40 1.501(6) . ?
C39 C41 1.533(5) . ?
C39 H39 1.0000 . ?
C40 H40A 0.9800 . ?
C40 H40B 0.9800 . ?
C40 H40C 0.9800 . ?
C41 H41A 0.9800 . ?
C41 H41B 0.9800 . ?
C41 H41C 0.9800 . ?
Cl42A O43A 1.398(10) . ?
Cl42A O46A 1.408(10) . ?
Cl42A O44A 1.434(10) . ?
Cl42A O45A 1.456(9) . ?
Cl42B O45B 1.372(9) . ?
Cl42B O44B 1.424(10) . ?
Cl42B O43B 1.437(10) . ?
Cl42B O46B 1.450(11) . ?
Cl47 O51 1.429(3) . ?
Cl47 O48 1.433(2) . ?
Cl47 O50 1.437(2) . ?
Cl47 O49 1.438(2) . ?
C52A N53A 1.463(10) . ?
C52A H52A 0.9800 . ?
C52A H52B 0.9800 . ?
C52A H52C 0.9800 . ?
N53A O54A 1.210(10) . ?
N53A O55A 1.291(9) . ?
C52B N53B 1.489(10) . ?
C52B H52D 0.9800 . ?
C52B H52E 0.9800 . ?
C52B H52F 0.9800 . ?
N53B O54B 1.169(9) . ?
N53B O55B 1.218(10) . ?
C52C N53C 1.599(18) . ?
C52C H52G 0.9800 . ?
C52C H52H 0.9800 . ?
C52C H52I 0.9800 . ?
N53C O55C 1.262(17) . ?
N53C O54C 1.297(17) . ?

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
N22 Fe1 N2 168.95(8) . . ?
N22 Fe1 N34 73.55(8) . . ?
N2 Fe1 N34 99.75(8) . . ?
N22 Fe1 N9 114.97(8) . . ?
N2 Fe1 N9 73.38(8) . . ?
N34 Fe1 N9 91.51(9) . . ?
N22 Fe1 N29 73.19(8) . . ?
N2 Fe1 N29 114.25(8) . . ?
N34 Fe1 N29 145.92(8) . . ?
N9 Fe1 N29 95.81(9) . . ?
N22 Fe1 N14 98.30(8) . . ?
N2 Fe1 N14 73.14(8) . . ?
N34 Fe1 N14 94.53(9) . . ?
N9 Fe1 N14 146.52(8) . . ?
N29 Fe1 N14 97.36(9) . . ?
C3 N2 C7 118.0(2) . . ?
C3 N2 Fe1 120.53(18) . . ?
C7 N2 Fe1 120.90(17) . . ?
N2 C3 C4 123.6(2) . . ?
N2 C3 N8 112.9(2) . . ?
C4 C3 N8 123.4(2) . . ?
C3 C4 C5 117.2(2) . . ?
C3 C4 H4 121.4 . . ?
C5 C4 H4 121.4 . . ?
C4 C5 C6 119.8(2) . . ?
C4 C5 S18 125.3(2) . . ?
C6 C5 S18 115.0(2) . . ?
C7 C6 C5 117.6(3) . . ?
C7 C6 H6 121.2 . . ?
C5 C6 H6 121.2 . . ?
N2 C7 C6 123.7(2) . . ?
N2 C7 N13 113.0(2) . . ?
C6 C7 N13 123.4(2) . . ?
C12 N8 N9 111.1(2) . . ?
C12 N8 C3 131.0(2) . . ?
N9 N8 C3 117.8(2) . . ?
C10 N9 N8 105.1(2) . . ?
C10 N9 Fe1 139.96(19) . . ?
N8 N9 Fe1 114.83(16) . . ?
N9 C10 C11 111.1(3) . . ?
N9 C10 H10 124.4 . . ?
C11 C10 H10 124.4 . . ?
C12 C11 C10 105.4(3) . . ?
C12 C11 H11 127.3 . . ?
C10 C11 H11 127.3 . . ?
N8 C12 C11 107.2(2) . . ?
N8 C12 H12 126.4 . . ?
C11 C12 H12 126.4 . . ?
C17 N13 N14 111.0(2) . . ?
C17 N13 C7 130.0(2) . . ?
N14 N13 C7 118.8(2) . . ?
C15 N14 N13 105.2(2) . . ?
C15 N14 Fe1 141.1(2) . . ?
N13 N14 Fe1 113.66(16) . . ?
N14 C15 C16 111.5(3) . . ?
N14 C15 H15 124.3 . . ?
C16 C15 H15 124.3 . . ?
C17 C16 C15 105.2(3) . . ?
C17 C16 H16 127.4 . . ?
C15 C16 H16 127.4 . . ?
N13 C17 C16 107.1(3) . . ?
N13 C17 H17 126.4 . . ?
C16 C17 H17 126.4 . . ?
C5 S18 C19 105.47(13) . . ?
C20 C19 C21 111.9(3) . . ?
C20 C19 S18 111.1(2) . . ?
C21 C19 S18 105.5(2) . . ?
C20 C19 H19 109.4 . . ?
C21 C19 H19 109.4 . . ?
S18 C19 H19 109.4 . . ?
C19 C20 H20A 109.5 . . ?
C19 C20 H20B 109.5 . . ?
H20A C20 H20B 109.5 . . ?
C19 C20 H20C 109.5 . . ?
H20A C20 H20C 109.5 . . ?
H20B C20 H20C 109.5 . . ?
C19 C21 H21A 109.5 . . ?
C19 C21 H21B 109.5 . . ?
H21A C21 H21B 109.5 . . ?
C19 C21 H21C 109.5 . . ?
H21A C21 H21C 109.5 . . ?
H21B C21 H21C 109.5 . . ?
C27 N22 C23 118.2(2) . . ?
C27 N22 Fe1 120.51(18) . . ?
C23 N22 Fe1 121.17(17) . . ?
N22 C23 C24 123.7(2) . . ?
N22 C23 N28 112.3(2) . . ?
C24 C23 N28 124.0(2) . . ?
C23 C24 C25 117.4(2) . . ?
C23 C24 H24 121.3 . . ?
C25 C24 H24 121.3 . . ?
C26 C25 C24 119.7(2) . . ?
C26 C25 S38 124.8(2) . . ?
C24 C25 S38 115.5(2) . . ?
C27 C26 C25 117.3(3) . . ?
C27 C26 H26 121.4 . . ?
C25 C26 H26 121.4 . . ?
N22 C27 C26 123.6(3) . . ?
N22 C27 N33 113.0(2) . . ?
C26 C27 N33 123.4(2) . . ?
C32 N28 N29 111.0(2) . . ?
C32 N28 C23 130.6(2) . . ?
N29 N28 C23 118.1(2) . . ?
C30 N29 N28 105.3(2) . . ?
C30 N29 Fe1 139.5(2) . . ?
N28 N29 Fe1 114.94(16) . . ?
N29 C30 C31 111.1(3) . . ?
N29 C30 H30 124.4 . . ?
C31 C30 H30 124.4 . . ?
C32 C31 C30 105.5(3) . . ?
C32 C31 H31 127.3 . . ?
C30 C31 H31 127.3 . . ?
N28 C32 C31 107.1(3) . . ?
N28 C32 H32 126.5 . . ?
C31 C32 H32 126.5 . . ?
C37 N33 N34 110.9(2) . . ?
C37 N33 C27 130.9(2) . . ?
N34 N33 C27 118.0(2) . . ?
C35 N34 N33 105.2(2) . . ?
C35 N34 Fe1 140.2(2) . . ?
N33 N34 Fe1 114.50(16) . . ?
N34 C35 C36 110.9(3) . . ?
N34 C35 H35 124.5 . . ?
C36 C35 H35 124.5 . . ?
C37 C36 C35 105.7(3) . . ?
C37 C36 H36 127.2 . . ?
C35 C36 H36 127.2 . . ?
N33 C37 C36 107.3(3) . . ?
N33 C37 H37 126.4 . . ?
C36 C37 H37 126.4 . . ?
C25 S38 C39 105.31(14) . . ?
C40 C39 C41 112.4(3) . . ?
C40 C39 S38 110.7(3) . . ?
C41 C39 S38 105.4(3) . . ?
C40 C39 H39 109.4 . . ?
C41 C39 H39 109.4 . . ?
S38 C39 H39 109.4 . . ?
C39 C40 H40A 109.5 . . ?
C39 C40 H40B 109.5 . . ?
H40A C40 H40B 109.5 . . ?
C39 C40 H40C 109.5 . . ?
H40A C40 H40C 109.5 . . ?
H40B C40 H40C 109.5 . . ?
C39 C41 H41A 109.5 . . ?
C39 C41 H41B 109.5 . . ?
H41A C41 H41B 109.5 . . ?
C39 C41 H41C 109.5 . . ?
H41A C41 H41C 109.5 . . ?
H41B C41 H41C 109.5 . . ?
O43A Cl42A O46A 106.7(7) . . ?
O43A Cl42A O44A 103.2(7) . . ?
O46A Cl42A O44A 109.5(6) . . ?
O43A Cl42A O45A 119.1(8) . . ?
O46A Cl42A O45A 112.0(7) . . ?
O44A Cl42A O45A 105.7(7) . . ?
O45B Cl42B O44B 111.8(7) . . ?
O45B Cl42B O43B 100.0(7) . . ?
O44B Cl42B O43B 116.4(7) . . ?
O45B Cl42B O46B 106.1(7) . . ?
O44B Cl42B O46B 109.7(7) . . ?
O43B Cl42B O46B 112.0(7) . . ?
O51 Cl47 O48 109.51(16) . . ?
O51 Cl47 O50 110.20(17) . . ?
O48 Cl47 O50 108.68(14) . . ?
O51 Cl47 O49 109.64(16) . . ?
O48 Cl47 O49 109.86(16) . . ?
O50 Cl47 O49 108.94(15) . . ?
N53A C52A H52A 109.5 . . ?
N53A C52A H52B 109.5 . . ?
H52A C52A H52B 109.5 . . ?
N53A C52A H52C 109.5 . . ?
H52A C52A H52C 109.5 . . ?
H52B C52A H52C 109.5 . . ?
O54A N53A O55A 109.8(8) . . ?
O54A N53A C52A 128.9(9) . . ?
O55A N53A C52A 116.2(7) . . ?
N53B C52B H52D 109.5 . . ?
N53B C52B H52E 109.5 . . ?
H52D C52B H52E 109.5 . . ?
N53B C52B H52F 109.5 . . ?
H52D C52B H52F 109.5 . . ?
H52E C52B H52F 109.5 . . ?
O54B N53B O55B 126.4(8) . . ?
O54B N53B C52B 121.5(8) . . ?
O55B N53B C52B 111.6(8) . . ?
N53C C52C H52G 109.5 . . ?
N53C C52C H52H 109.5 . . ?
H52G C52C H52H 109.5 . . ?
N53C C52C H52I 109.5 . . ?
H52G C52C H52I 109.5 . . ?
H52H C52C H52I 109.5 . . ?
O55C N53C O54C 114.5(17) . . ?
O55C N53C C52C 103.6(16) . . ?
O54C N53C C52C 98.5(15) . . ?

_diffrn_measured_fraction_theta_max 0.980
_diffrn_reflns_theta_full        67.08
_diffrn_measured_fraction_theta_full 0.980
_refine_diff_density_max         0.696
_refine_diff_density_min         -0.516
_refine_diff_density_rms         0.072
_exptl_crystal_recrystallization_method 
'Re-crystallisation from solvent: Nitromethane-diethyl ether'
_exptl_crystal_preparation       'Magnetic properties'
####################################################################### 
# 
# This file contains crystal structure data downloaded from the 
# Cambridge Structural Database (CSD) hosted by the Cambridge 
# Crystallographic Data Centre (CCDC).
# 
# Full information about CCDC data access policies and citation 
# guidelines are available at http://www.ccdc.cam.ac.uk/access/V1 
# 
# Audit and citation data items may have been added by the CCDC. 
# Please retain this information to preserve the provenance of 
# this file and to allow appropriate attribution of the data. 
# 
#######################################################################

data_164sfht
_database_code_depnum_ccdc_archive 'CCDC 1563029'
_audit_update_record             
;
2017-07-18 deposited with the CCDC.
2017-11-20 downloaded from the CCDC.
;

_audit_creation_method           SHELXL-97
_chemical_name_systematic        
Bis[4-(isopropylsulfanyl)-2,6-di(pyrazol-1-yl)pyridine]iron(II)diperchlorate
_chemical_name_common            ?
_chemical_melting_point          ?
_chemical_formula_moiety         'C28 H30 Fe N10 S2, 2(Cl O4)'
_chemical_formula_sum            'C28 H30 Cl2 Fe N10 O8 S2'
_chemical_formula_weight         825.49

loop_
_atom_type_symbol
_atom_type_description
_atom_type_scat_dispersion_real
_atom_type_scat_dispersion_imag
_atom_type_scat_source
Cl Cl 0.3639 0.7018 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
C C 0.0181 0.0091 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Fe Fe -1.1336 3.1974 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
N N 0.0311 0.0180 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
O O 0.0492 0.0322 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
S S 0.3331 0.5567 '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'

_symmetry_cell_setting           monoclinic
_symmetry_space_group_name_H-M   'P 21/c'

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

_cell_length_a                   20.2860(6)
_cell_length_b                   11.7884(4)
_cell_length_c                   15.9103(6)
_cell_angle_alpha                90.00
_cell_angle_beta                 102.266(3)
_cell_angle_gamma                90.00
_cell_volume                     3717.9(2)
_cell_formula_units_Z            4
_cell_measurement_temperature    250(2)
_cell_measurement_reflns_used    4362
_cell_measurement_theta_min      4.36
_cell_measurement_theta_max      73.02

_exptl_crystal_description       'rectangular prism'
_exptl_crystal_colour            yellow
_exptl_crystal_size_max          0.18
_exptl_crystal_size_mid          0.14
_exptl_crystal_size_min          0.07
_exptl_crystal_density_meas      ?
_exptl_crystal_density_diffrn    1.475
_exptl_crystal_density_method    'not measured'
_exptl_crystal_F_000             1696
_exptl_absorpt_coefficient_mu    6.145
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_correction_T_min  0.537
_exptl_absorpt_correction_T_max  1.000
_exptl_absorpt_process_details   
; 
CrysAlisPro, Agilent Technologies,
Version 1.171.36.24 (release 03-12-2012 CrysAlis171 .NET)
Empirical absorption correction using spherical harmonics,
 implemented in SCALE3 ABSPACK scaling algorithm.
;

_diffrn_ambient_temperature      250(2)
_diffrn_radiation_wavelength     1.54184
_diffrn_radiation_type           CuK\a
_diffrn_radiation_source         'SuperNova (Cu) X-ray Source'
_diffrn_radiation_monochromator  mirror
_diffrn_measurement_device_type  'SuperNova, Dual, Cu at zero, Atlas'
_diffrn_measurement_method       'ω scans'
_diffrn_detector_area_resol_mean 5.3095
_diffrn_standards_number         0
_diffrn_standards_interval_count 0
_diffrn_standards_interval_time  0
_diffrn_standards_decay_%        0
_diffrn_reflns_number            14219
_diffrn_reflns_av_R_equivalents  0.0453
_diffrn_reflns_av_sigmaI/netI    0.0507
_diffrn_reflns_limit_h_min       -24
_diffrn_reflns_limit_h_max       19
_diffrn_reflns_limit_k_min       -9
_diffrn_reflns_limit_k_max       13
_diffrn_reflns_limit_l_min       -18
_diffrn_reflns_limit_l_max       19
_diffrn_reflns_theta_min         4.36
_diffrn_reflns_theta_max         67.07
_reflns_number_total             6622
_reflns_number_gt                5006
_reflns_threshold_expression     >2sigma(I)

_computing_data_collection       'CrysAlisPro, Agilent Technologies'
_computing_cell_refinement       'CrysAlisPro, Agilent Technologies'
_computing_data_reduction        'CrysAlisPro, Agilent Technologies'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_molecular_graphics    'XSEED (Barbour, 2001)'
_computing_publication_material  'local program'

_refine_special_details          
; 
 Refinement of F² against ALL reflections.  The weighted R-factor wR and 
 goodness of fit S are based on F², conventional R-factors R are based 
 on F, with F set to zero for negative F². The threshold expression of 
 F² > 2sigma(F²) is used only for calculating R-factors(gt) etc. and is 
 not relevant to the choice of reflections for refinement.  R-factors based 
 on F² are statistically about twice as large as those based on F, and R- 
 factors based on ALL data will be even larger. 

 This crystal was produced by annealing a hydrated crystal on the 
 diffractometer at 375 K. The lattice water has been removed, but the quality 
 of the crystal is significantly degraded.

 One of the isopropylsulfanyl substitutents on the complex cation is 
 disordered over three equally ovccupied orientations, which were modelled 
 with the fixed restraints C(pyridyl)---S = 1.75(2), C(alkyl)---S = 1.82(2), 
 C---C = 1.52(2), 1,3-C---C---C = 2.48(2) and 1,3-C---S---C = 2.83(2) Å. 
 Both ClO₄⁻ ions are also disordered, one over two half-occupied sites 
 and the other over four orientations. The refined restraints Cl---O = 1.44(2) 
 and O...O = 2.35(2) Å were applied to those residues.

 All fully occupied non-H atoms, plus the half-occupied disordered Cl atoms, 
 were refined anisotropically, and H atoms were placed in calculated positions 
 and refined using a riding model. 

 A SQUEEZE analysis of the final model showed 138.2 Å³ of solvent-
 accessible void space in the unit cell, containing just seven unresolved 
 electrons.
;

_refine_ls_structure_factor_coef Fsqd
_refine_ls_matrix_type           full
_refine_ls_weighting_scheme      calc
_refine_ls_weighting_details     
'calc w=1/[σ²(Fo²)+(0.1152P)²+2.8697P] 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         6622
_refine_ls_number_parameters     515
_refine_ls_number_restraints     78
_refine_ls_R_factor_all          0.0871
_refine_ls_R_factor_gt           0.0677
_refine_ls_wR_factor_ref         0.2027
_refine_ls_wR_factor_gt          0.1826
_refine_ls_goodness_of_fit_ref   1.038
_refine_ls_restrained_S_all      1.051
_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_symmetry_multiplicity
_atom_site_calc_flag
_atom_site_refinement_flags
_atom_site_disorder_assembly
_atom_site_disorder_group
Fe1 Fe 0.22918(3) 0.60339(6) 0.06518(5) 0.0444(2) Uani 1 1 d . A .
N2 N 0.12186(16) 0.6250(3) 0.0408(2) 0.0401(8) Uani 1 1 d . . .
C3 C 0.0922(2) 0.7020(3) -0.0158(3) 0.0394(9) Uani 1 1 d . . .
C4 C 0.0255(2) 0.7319(4) -0.0269(3) 0.0434(9) Uani 1 1 d . . .
H4 H 0.0060 0.7858 -0.0682 0.052 Uiso 1 1 calc R . .
C5 C -0.0119(2) 0.6793(4) 0.0255(3) 0.0433(9) Uani 1 1 d . . .
C6 C 0.0184(2) 0.5988(4) 0.0856(3) 0.0466(10) Uani 1 1 d . . .
H6 H -0.0060 0.5622 0.1218 0.056 Uiso 1 1 calc R . .
C7 C 0.0852(2) 0.5748(4) 0.0899(3) 0.0423(9) Uani 1 1 d . . .
N8 N 0.13689(16) 0.7521(3) -0.0616(2) 0.0415(8) Uani 1 1 d . . .
N9 N 0.20409(17) 0.7286(3) -0.0354(3) 0.0493(9) Uani 1 1 d . . .
C10 C 0.2339(2) 0.7910(5) -0.0855(4) 0.0626(14) Uani 1 1 d . . .
H10 H 0.2808 0.7940 -0.0813 0.075 Uiso 1 1 calc R . .
C11 C 0.1868(3) 0.8521(5) -0.1453(4) 0.0660(14) Uani 1 1 d . . .
H11 H 0.1956 0.9011 -0.1882 0.079 Uiso 1 1 calc R . .
C12 C 0.1256(2) 0.8259(4) -0.1285(3) 0.0524(11) Uani 1 1 d . . .
H12 H 0.0835 0.8537 -0.1577 0.063 Uiso 1 1 calc R . .
N13 N 0.12179(18) 0.4950(3) 0.1481(3) 0.0472(9) Uani 1 1 d . . .
N14 N 0.18923(18) 0.4848(3) 0.1518(3) 0.0493(9) Uani 1 1 d . . .
C15 C 0.2091(3) 0.4008(4) 0.2069(3) 0.0588(12) Uani 1 1 d . . .
H15 H 0.2538 0.3745 0.2229 0.071 Uiso 1 1 calc R . .
C16 C 0.1548(3) 0.3563(5) 0.2382(4) 0.0665(14) Uani 1 1 d . . .
H16 H 0.1560 0.2965 0.2775 0.080 Uiso 1 1 calc R . .
C17 C 0.1000(3) 0.4178(4) 0.1997(4) 0.0587(12) Uani 1 1 d . . .
H17 H 0.0556 0.4088 0.2073 0.070 Uiso 1 1 calc R . .
S18 S -0.09775(5) 0.70287(11) 0.02254(9) 0.0584(3) Uani 1 1 d . . .
C19 C -0.1181(2) 0.8362(4) -0.0354(3) 0.0529(11) Uani 1 1 d . . .
H19 H -0.1032 0.8322 -0.0907 0.064 Uiso 1 1 calc R . .
C20 C -0.0843(3) 0.9352(5) 0.0161(5) 0.0740(16) Uani 1 1 d . . .
H20A H -0.0934 1.0039 -0.0179 0.111 Uiso 1 1 calc R . .
H20B H -0.0360 0.9222 0.0313 0.111 Uiso 1 1 calc R . .
H20C H -0.1016 0.9432 0.0681 0.111 Uiso 1 1 calc R . .
C21 C -0.1946(3) 0.8451(6) -0.0532(5) 0.0808(18) Uani 1 1 d . . .
H21A H -0.2092 0.8514 0.0008 0.121 Uiso 1 1 calc R . .
H21B H -0.2143 0.7780 -0.0838 0.121 Uiso 1 1 calc R . .
H21C H -0.2089 0.9118 -0.0880 0.121 Uiso 1 1 calc R . .
N22 N 0.33167(16) 0.5780(3) 0.1236(2) 0.0436(8) Uani 1 1 d . A .
C23 C 0.3682(2) 0.4986(4) 0.0937(3) 0.0507(11) Uani 1 1 d . . .
C24 C 0.4327(3) 0.4735(5) 0.1317(4) 0.0716(17) Uani 1 1 d . A .
H24 H 0.4570 0.4178 0.1087 0.086 Uiso 1 1 calc R . .
C25 C 0.4622(2) 0.5328(6) 0.2063(4) 0.0739(17) Uani 1 1 d D . .
C26 C 0.4258(2) 0.6184(5) 0.2367(4) 0.0617(13) Uani 1 1 d . A .
H26 H 0.4446 0.6612 0.2858 0.074 Uiso 1 1 calc R . .
C27 C 0.3617(2) 0.6371(4) 0.1917(3) 0.0475(10) Uani 1 1 d . . .
N28 N 0.33188(18) 0.4443(3) 0.0192(3) 0.0508(9) Uani 1 1 d . . .
N29 N 0.26581(17) 0.4724(3) -0.0103(2) 0.0456(8) Uani 1 1 d . . .
C30 C 0.2460(3) 0.4121(4) -0.0810(3) 0.0549(12) Uani 1 1 d . . .
H30 H 0.2021 0.4134 -0.1152 0.066 Uiso 1 1 calc R . .
C31 C 0.2986(3) 0.3463(5) -0.0986(4) 0.0653(14) Uani 1 1 d . . .
H31 H 0.2974 0.2970 -0.1453 0.078 Uiso 1 1 calc R . .
C32 C 0.3519(3) 0.3691(5) -0.0332(4) 0.0668(14) Uani 1 1 d . . .
H32 H 0.3953 0.3376 -0.0261 0.080 Uiso 1 1 calc R . .
N33 N 0.31887(18) 0.7229(3) 0.2129(3) 0.0503(9) Uani 1 1 d . A .
N34 N 0.25571(18) 0.7319(3) 0.1648(3) 0.0517(9) Uani 1 1 d . . .
C35 C 0.2299(3) 0.8233(5) 0.1939(4) 0.0650(14) Uani 1 1 d . A .
H35 H 0.1860 0.8506 0.1727 0.078 Uiso 1 1 calc R . .
C36 C 0.2761(3) 0.8728(5) 0.2596(4) 0.0734(16) Uani 1 1 d . . .
H36 H 0.2698 0.9385 0.2906 0.088 Uiso 1 1 calc R A .
C37 C 0.3325(3) 0.8078(5) 0.2707(4) 0.0628(13) Uani 1 1 d . A .
H37 H 0.3731 0.8198 0.3109 0.075 Uiso 1 1 calc R . .
S38A S 0.5361(2) 0.4700(4) 0.2773(3) 0.0586(12) Uiso 0.34 1 d PD A 1
C39A C 0.5712(12) 0.5823(19) 0.3495(16) 0.119(19) Uiso 0.34 1 d PD A 1
H39A H 0.5438 0.6031 0.3917 0.143 Uiso 0.34 1 calc PR A 1
C40A C 0.5945(13) 0.6838(19) 0.302(2) 0.067(6) Uiso 0.34 1 d PD A 1
H40A H 0.5559 0.7305 0.2775 0.101 Uiso 0.34 1 calc PR A 1
H40B H 0.6155 0.6562 0.2566 0.101 Uiso 0.34 1 calc PR A 1
H40C H 0.6269 0.7285 0.3424 0.101 Uiso 0.34 1 calc PR A 1
C41A C 0.6357(10) 0.5125(19) 0.3877(15) 0.068(5) Uiso 0.34 1 d PD A 1
H41A H 0.6238 0.4483 0.4196 0.102 Uiso 0.34 1 calc PR A 1
H41B H 0.6677 0.5602 0.4259 0.102 Uiso 0.34 1 calc PR A 1
H41C H 0.6559 0.4854 0.3414 0.102 Uiso 0.34 1 calc PR A 1
S38B S 0.54524(18) 0.4882(4) 0.2494(3) 0.0364(7) Uiso 0.33 1 d PD A 2
C40B C 0.597(2) 0.690(3) 0.322(3) 0.14(2) Uiso 0.33 1 d PD A 2
H40D H 0.5633 0.7228 0.2765 0.205 Uiso 0.33 1 calc PR A 2
H40E H 0.6393 0.6823 0.3036 0.205 Uiso 0.33 1 calc PR A 2
H40F H 0.6035 0.7381 0.3727 0.205 Uiso 0.33 1 calc PR A 2
C41B C 0.6279(12) 0.520(2) 0.4140(16) 0.079(7) Uiso 0.33 1 d PD A 2
H41D H 0.6134 0.4456 0.4284 0.119 Uiso 0.33 1 calc PR A 2
H41E H 0.6358 0.5679 0.4648 0.119 Uiso 0.33 1 calc PR A 2
H41F H 0.6692 0.5133 0.3930 0.119 Uiso 0.33 1 calc PR A 2
C39B C 0.5734(7) 0.5729(14) 0.3447(10) 0.039(5) Uiso 0.33 1 d PD A 2
H39B H 0.5337 0.5852 0.3706 0.047 Uiso 0.33 1 calc PR A 2
S38C S 0.5518(3) 0.5255(6) 0.2312(4) 0.0831(18) Uiso 0.33 1 d PD A 3
C39C C 0.5760(6) 0.6107(15) 0.3292(9) 0.043(4) Uiso 0.33 1 d PD A 3
H39C H 0.5362 0.6378 0.3502 0.052 Uiso 0.33 1 calc PR A 3
C41C C 0.6303(11) 0.563(2) 0.4016(15) 0.077(6) Uiso 0.33 1 d PD A 3
H41G H 0.6113 0.5038 0.4312 0.116 Uiso 0.33 1 calc PR A 3
H41H H 0.6475 0.6236 0.4419 0.116 Uiso 0.33 1 calc PR A 3
H41I H 0.6669 0.5327 0.3779 0.116 Uiso 0.33 1 calc PR A 3
C40C C 0.607(2) 0.704(3) 0.284(2) 0.153(18) Uiso 0.33 1 d PD A 3
H40G H 0.5731 0.7368 0.2388 0.230 Uiso 0.33 1 calc PR A 3
H40H H 0.6434 0.6730 0.2604 0.230 Uiso 0.33 1 calc PR A 3
H40I H 0.6252 0.7630 0.3258 0.230 Uiso 0.33 1 calc PR A 3
Cl42A Cl 0.4537(4) 0.7157(7) 0.4896(6) 0.067(2) Uiso 0.25 1 d PD B 1
O43A O 0.5030(10) 0.736(2) 0.5654(11) 0.106(7) Uiso 0.25 1 d PD B 1
O44A O 0.4716(8) 0.7868(14) 0.4193(9) 0.052(4) Uiso 0.25 1 d PD B 1
O45A O 0.3905(6) 0.7726(14) 0.5052(10) 0.059(4) Uiso 0.25 1 d PD B 1
O46A O 0.4431(13) 0.6059(13) 0.4653(16) 0.137(10) Uiso 0.25 1 d PD B 1
Cl42B Cl 0.4368(3) 0.7551(6) 0.4758(4) 0.0455(13) Uiso 0.25 1 d PD C 3
O43B O 0.4550(14) 0.736(2) 0.5705(9) 0.134(9) Uiso 0.25 1 d PD C 3
O44B O 0.4959(9) 0.775(2) 0.4470(16) 0.104(8) Uiso 0.25 1 d PD C 3
O45B O 0.3885(9) 0.8449(15) 0.4646(13) 0.099(6) Uiso 0.25 1 d PD C 3
O46B O 0.4031(11) 0.6534(14) 0.4376(12) 0.088(6) Uiso 0.25 1 d PD C 3
Cl42C Cl 0.4535(4) 0.7458(9) 0.5028(5) 0.0574(19) Uiso 0.25 1 d PD D 2
O43C O 0.5168(10) 0.713(3) 0.544(2) 0.23(3) Uiso 0.25 1 d PD D 2
O44C O 0.4501(13) 0.8494(17) 0.4515(15) 0.120(8) Uiso 0.25 1 d PD D 2
O45C O 0.4022(8) 0.7466(15) 0.5492(11) 0.072(4) Uiso 0.25 1 d PD D 2
O46C O 0.4296(16) 0.657(2) 0.4319(16) 0.147(13) Uiso 0.25 1 d PD D 2
Cl42D Cl 0.4445(3) 0.7930(7) 0.4914(5) 0.0633(17) Uiso 0.25 1 d PD E 4
O43D O 0.4180(12) 0.8976(15) 0.4558(14) 0.113(7) Uiso 0.25 1 d PD E 4
O44D O 0.3920(12) 0.716(2) 0.500(2) 0.174(15) Uiso 0.25 1 d PD E 4
O45D O 0.4808(12) 0.745(2) 0.4259(13) 0.092(8) Uiso 0.25 1 d PD E 4
O46D O 0.4949(9) 0.8021(18) 0.5677(9) 0.091(5) Uiso 0.25 1 d PD E 4
Cl47A Cl 0.0761(4) 0.9839(9) 0.2307(6) 0.073(3) Uani 0.50 1 d PD F 1
O48A O 0.1392(4) 1.0378(8) 0.2215(7) 0.066(3) Uiso 0.50 1 d PD F 1
O49A O 0.0184(4) 1.0537(8) 0.1999(6) 0.064(2) Uiso 0.50 1 d PD F 1
O50A O 0.0848(4) 0.9628(7) 0.3226(5) 0.058(2) Uiso 0.50 1 d PD F 1
O51A O 0.0673(5) 0.8814(7) 0.1812(6) 0.071(2) Uiso 0.50 1 d PD F 1
Cl47B Cl 0.0769(3) 0.9936(8) 0.2308(4) 0.048(2) Uani 0.50 1 d PD G 2
O50B O 0.0669(5) 0.9309(7) 0.3041(5) 0.066(2) Uiso 0.50 1 d PD G 2
O49B O 0.0294(5) 1.0867(8) 0.2132(7) 0.079(3) Uiso 0.50 1 d PD G 2
O48B O 0.1413(5) 1.0495(9) 0.2439(7) 0.075(4) Uiso 0.50 1 d PD G 2
O51B O 0.0714(5) 0.9162(8) 0.1595(6) 0.073(3) Uiso 0.50 1 d PD G 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 N22 2.111(3) . ?
Fe1 N2 2.144(3) . ?
Fe1 N9 2.157(4) . ?
Fe1 N34 2.176(4) . ?
Fe1 N29 2.181(4) . ?
Fe1 N14 2.233(4) . ?
N2 C7 1.327(5) . ?
N2 C3 1.329(5) . ?
C3 C4 1.372(6) . ?
C3 N8 1.408(5) . ?
C4 C5 1.388(6) . ?
C4 H4 0.9400 . ?
C5 C6 1.394(6) . ?
C5 S18 1.754(4) . ?
C6 C7 1.371(6) . ?
C6 H6 0.9400 . ?
C7 N13 1.414(6) . ?
N8 C12 1.356(6) . ?
N8 N9 1.367(5) . ?
N9 C10 1.322(6) . ?
C10 C11 1.397(8) . ?
C10 H10 0.9400 . ?
C11 C12 1.360(7) . ?
C11 H11 0.9400 . ?
C12 H12 0.9400 . ?
N13 C17 1.360(6) . ?
N13 N14 1.362(5) . ?
N14 C15 1.328(6) . ?
C15 C16 1.404(8) . ?
C15 H15 0.9400 . ?
C16 C17 1.358(8) . ?
C16 H16 0.9400 . ?
C17 H17 0.9400 . ?
S18 C19 1.824(5) . ?
C19 C20 1.506(8) . ?
C19 C21 1.520(7) . ?
C19 H19 0.9900 . ?
C20 H20A 0.9700 . ?
C20 H20B 0.9700 . ?
C20 H20C 0.9700 . ?
C21 H21A 0.9700 . ?
C21 H21B 0.9700 . ?
C21 H21C 0.9700 . ?
N22 C27 1.323(6) . ?
N22 C23 1.341(6) . ?
C23 C24 1.354(7) . ?
C23 N28 1.410(6) . ?
C24 C25 1.398(8) . ?
C24 H24 0.9400 . ?
C25 C26 1.396(7) . ?
C25 S38B 1.758(5) . ?
C25 S38C 1.778(7) . ?
C25 S38A 1.830(6) . ?
C26 C27 1.363(7) . ?
C26 H26 0.9400 . ?
C27 N33 1.421(6) . ?
N28 C32 1.338(6) . ?
N28 N29 1.363(5) . ?
N29 C30 1.320(6) . ?
C30 C31 1.394(8) . ?
C30 H30 0.9400 . ?
C31 C32 1.359(8) . ?
C31 H31 0.9400 . ?
C32 H32 0.9400 . ?
N33 C37 1.347(6) . ?
N33 N34 1.350(5) . ?
N34 C35 1.323(6) . ?
C35 C36 1.376(9) . ?
C35 H35 0.9400 . ?
C36 C37 1.357(8) . ?
C36 H36 0.9400 . ?
C37 H37 0.9400 . ?
S38A C39A 1.797(17) . ?
C39A C40A 1.541(19) . ?
C39A C41A 1.556(18) . ?
C39A H39A 0.9900 . ?
C40A H40A 0.9700 . ?
C40A H40B 0.9700 . ?
C40A H40C 0.9700 . ?
C41A H41A 0.9700 . ?
C41A H41B 0.9700 . ?
C41A H41C 0.9700 . ?
S38B C39B 1.805(12) . ?
C40B C39B 1.524(18) . ?
C40B H40D 0.9700 . ?
C40B H40E 0.9700 . ?
C40B H40F 0.9700 . ?
C41B C39B 1.518(16) . ?
C41B H41D 0.9700 . ?
C41B H41E 0.9700 . ?
C41B H41F 0.9700 . ?
C39B H39B 0.9900 . ?
S38C C39C 1.832(12) . ?
C39C C41C 1.521(16) . ?
C39C C40C 1.523(19) . ?
C39C H39C 0.9900 . ?
C41C H41G 0.9700 . ?
C41C H41H 0.9700 . ?
C41C H41I 0.9700 . ?
C40C H40G 0.9700 . ?
C40C H40H 0.9700 . ?
C40C H40I 0.9700 . ?
Cl42A O46A 1.355(14) . ?
Cl42A O43A 1.416(14) . ?
Cl42A O44A 1.502(12) . ?
Cl42A O45A 1.514(12) . ?
Cl42B O44B 1.390(13) . ?
Cl42B O45B 1.428(14) . ?
Cl42B O46B 1.448(13) . ?
Cl42B O43B 1.490(14) . ?
Cl42C O43C 1.368(15) . ?
Cl42C O45C 1.397(13) . ?
Cl42C O44C 1.463(15) . ?
Cl42C O46C 1.540(16) . ?
Cl42D O43D 1.414(14) . ?
Cl42D O46D 1.415(13) . ?
Cl42D O44D 1.426(15) . ?
Cl42D O45D 1.507(14) . ?
Cl47A O49A 1.430(10) . ?
Cl47A O51A 1.432(11) . ?
Cl47A O50A 1.457(11) . ?
Cl47A O48A 1.463(11) . ?
Cl47B O50B 1.431(10) . ?
Cl47B O48B 1.438(10) . ?
Cl47B O51B 1.441(10) . ?
Cl47B O49B 1.448(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
N22 Fe1 N2 164.55(14) . . ?
N22 Fe1 N9 118.61(14) . . ?
N2 Fe1 N9 73.38(13) . . ?
N22 Fe1 N34 73.15(14) . . ?
N2 Fe1 N34 97.65(13) . . ?
N9 Fe1 N34 92.69(16) . . ?
N22 Fe1 N29 73.91(14) . . ?
N2 Fe1 N29 115.88(13) . . ?
N9 Fe1 N29 97.50(15) . . ?
N34 Fe1 N29 146.46(13) . . ?
N22 Fe1 N14 95.29(14) . . ?
N2 Fe1 N14 72.44(13) . . ?
N9 Fe1 N14 145.79(13) . . ?
N34 Fe1 N14 93.01(15) . . ?
N29 Fe1 N14 96.14(14) . . ?
C7 N2 C3 118.3(3) . . ?
C7 N2 Fe1 121.0(3) . . ?
C3 N2 Fe1 120.0(3) . . ?
N2 C3 C4 123.6(4) . . ?
N2 C3 N8 112.9(3) . . ?
C4 C3 N8 123.5(4) . . ?
C3 C4 C5 117.3(4) . . ?
C3 C4 H4 121.3 . . ?
C5 C4 H4 121.3 . . ?
C4 C5 C6 119.8(4) . . ?
C4 C5 S18 125.5(3) . . ?
C6 C5 S18 114.7(3) . . ?
C7 C6 C5 117.6(4) . . ?
C7 C6 H6 121.2 . . ?
C5 C6 H6 121.2 . . ?
N2 C7 C6 123.4(4) . . ?
N2 C7 N13 113.6(4) . . ?
C6 C7 N13 123.1(4) . . ?
C12 N8 N9 111.1(3) . . ?
C12 N8 C3 131.0(4) . . ?
N9 N8 C3 117.9(3) . . ?
C10 N9 N8 104.9(4) . . ?
C10 N9 Fe1 139.6(3) . . ?
N8 N9 Fe1 115.3(3) . . ?
N9 C10 C11 111.3(4) . . ?
N9 C10 H10 124.3 . . ?
C11 C10 H10 124.3 . . ?
C12 C11 C10 105.7(4) . . ?
C12 C11 H11 127.2 . . ?
C10 C11 H11 127.2 . . ?
N8 C12 C11 106.9(4) . . ?
N8 C12 H12 126.5 . . ?
C11 C12 H12 126.5 . . ?
C17 N13 N14 111.5(4) . . ?
C17 N13 C7 130.3(4) . . ?
N14 N13 C7 118.0(4) . . ?
C15 N14 N13 104.9(4) . . ?
C15 N14 Fe1 140.9(3) . . ?
N13 N14 Fe1 114.2(3) . . ?
N14 C15 C16 111.1(5) . . ?
N14 C15 H15 124.4 . . ?
C16 C15 H15 124.4 . . ?
C17 C16 C15 105.7(5) . . ?
C17 C16 H16 127.2 . . ?
C15 C16 H16 127.2 . . ?
C16 C17 N13 106.9(5) . . ?
C16 C17 H17 126.6 . . ?
N13 C17 H17 126.6 . . ?
C5 S18 C19 105.5(2) . . ?
C20 C19 C21 112.1(5) . . ?
C20 C19 S18 111.4(4) . . ?
C21 C19 S18 105.5(4) . . ?
C20 C19 H19 109.3 . . ?
C21 C19 H19 109.3 . . ?
S18 C19 H19 109.3 . . ?
C19 C20 H20A 109.5 . . ?
C19 C20 H20B 109.5 . . ?
H20A C20 H20B 109.5 . . ?
C19 C20 H20C 109.5 . . ?
H20A C20 H20C 109.5 . . ?
H20B C20 H20C 109.5 . . ?
C19 C21 H21A 109.5 . . ?
C19 C21 H21B 109.5 . . ?
H21A C21 H21B 109.5 . . ?
C19 C21 H21C 109.5 . . ?
H21A C21 H21C 109.5 . . ?
H21B C21 H21C 109.5 . . ?
C27 N22 C23 117.7(4) . . ?
C27 N22 Fe1 121.7(3) . . ?
C23 N22 Fe1 120.6(3) . . ?
N22 C23 C24 123.3(5) . . ?
N22 C23 N28 112.7(4) . . ?
C24 C23 N28 124.0(4) . . ?
C23 C24 C25 117.9(5) . . ?
C23 C24 H24 121.0 . . ?
C25 C24 H24 121.0 . . ?
C26 C25 C24 119.5(4) . . ?
C26 C25 S38B 127.9(4) . . ?
C24 C25 S38B 112.5(4) . . ?
C26 C25 S38C 123.3(5) . . ?
C24 C25 S38C 113.4(4) . . ?
C26 C25 S38A 120.2(4) . . ?
C24 C25 S38A 117.9(4) . . ?
C27 C26 C25 116.8(5) . . ?
C27 C26 H26 121.6 . . ?
C25 C26 H26 121.6 . . ?
N22 C27 C26 124.6(4) . . ?
N22 C27 N33 111.8(4) . . ?
C26 C27 N33 123.6(4) . . ?
C32 N28 N29 110.7(4) . . ?
C32 N28 C23 130.7(4) . . ?
N29 N28 C23 118.5(4) . . ?
C30 N29 N28 105.1(4) . . ?
C30 N29 Fe1 140.6(3) . . ?
N28 N29 Fe1 114.1(3) . . ?
N29 C30 C31 111.3(5) . . ?
N29 C30 H30 124.4 . . ?
C31 C30 H30 124.4 . . ?
C32 C31 C30 104.8(5) . . ?
C32 C31 H31 127.6 . . ?
C30 C31 H31 127.6 . . ?
N28 C32 C31 108.0(5) . . ?
N28 C32 H32 126.0 . . ?
C31 C32 H32 126.0 . . ?
C37 N33 N34 111.1(4) . . ?
C37 N33 C27 130.2(4) . . ?
N34 N33 C27 118.4(4) . . ?
C35 N34 N33 105.3(4) . . ?
C35 N34 Fe1 140.1(4) . . ?
N33 N34 Fe1 114.6(3) . . ?
N34 C35 C36 110.8(5) . . ?
N34 C35 H35 124.6 . . ?
C36 C35 H35 124.6 . . ?
C37 C36 C35 106.1(5) . . ?
C37 C36 H36 126.9 . . ?
C35 C36 H36 126.9 . . ?
N33 C37 C36 106.7(5) . . ?
N33 C37 H37 126.7 . . ?
C36 C37 H37 126.7 . . ?
C39A S38A C25 105.0(7) . . ?
C40A C39A C41A 106.4(16) . . ?
C40A C39A S38A 112.3(18) . . ?
C41A C39A S38A 92.7(14) . . ?
C40A C39A H39A 114.4 . . ?
C41A C39A H39A 114.4 . . ?
S38A C39A H39A 114.4 . . ?
C39A C40A H40A 109.5 . . ?
C39A C40A H40B 109.5 . . ?
H40A C40A H40B 109.5 . . ?
C39A C40A H40C 109.5 . . ?
H40A C40A H40C 109.5 . . ?
H40B C40A H40C 109.5 . . ?
C39A C41A H41A 109.5 . . ?
C39A C41A H41B 109.5 . . ?
H41A C41A H41B 109.5 . . ?
C39A C41A H41C 109.5 . . ?
H41A C41A H41C 109.5 . . ?
H41B C41A H41C 109.5 . . ?
C25 S38B C39B 105.5(5) . . ?
C39B C40B H40D 109.5 . . ?
C39B C40B H40E 109.5 . . ?
H40D C40B H40E 109.5 . . ?
C39B C40B H40F 109.5 . . ?
H40D C40B H40F 109.5 . . ?
H40E C40B H40F 109.5 . . ?
C39B C41B H41D 109.5 . . ?
C39B C41B H41E 109.5 . . ?
H41D C41B H41E 109.5 . . ?
C39B C41B H41F 109.5 . . ?
H41D C41B H41F 109.5 . . ?
H41E C41B H41F 109.5 . . ?
C41B C39B C40B 108.9(15) . . ?
C41B C39B S38B 115.8(15) . . ?
C40B C39B S38B 111(2) . . ?
C41B C39B H39B 106.8 . . ?
C40B C39B H39B 106.8 . . ?
S38B C39B H39B 106.8 . . ?
C25 S38C C39C 103.8(5) . . ?
C41C C39C C40C 108.2(15) . . ?
C41C C39C S38C 117.6(14) . . ?
C40C C39C S38C 93.6(19) . . ?
C41C C39C H39C 112.0 . . ?
C40C C39C H39C 112.0 . . ?
S38C C39C H39C 112.0 . . ?
C39C C41C H41G 109.5 . . ?
C39C C41C H41H 109.5 . . ?
H41G C41C H41H 109.5 . . ?
C39C C41C H41I 109.5 . . ?
H41G C41C H41I 109.5 . . ?
H41H C41C H41I 109.5 . . ?
C39C C40C H40G 109.5 . . ?
C39C C40C H40H 109.5 . . ?
H40G C40C H40H 109.5 . . ?
C39C C40C H40I 109.5 . . ?
H40G C40C H40I 109.5 . . ?
H40H C40C H40I 109.5 . . ?
O46A Cl42A O43A 116.6(13) . . ?
O46A Cl42A O44A 111.7(12) . . ?
O43A Cl42A O44A 107.4(10) . . ?
O46A Cl42A O45A 112.4(12) . . ?
O43A Cl42A O45A 104.7(12) . . ?
O44A Cl42A O45A 102.8(9) . . ?
O44B Cl42B O45B 117.0(12) . . ?
O44B Cl42B O46B 111.3(12) . . ?
O45B Cl42B O46B 108.1(11) . . ?
O44B Cl42B O43B 108.3(12) . . ?
O45B Cl42B O43B 104.7(11) . . ?
O46B Cl42B O43B 106.9(11) . . ?
O43C Cl42C O45C 118.3(15) . . ?
O43C Cl42C O44C 115.7(14) . . ?
O45C Cl42C O44C 109.7(12) . . ?
O43C Cl42C O46C 106.2(14) . . ?
O45C Cl42C O46C 103.8(12) . . ?
O44C Cl42C O46C 100.8(12) . . ?
O43D Cl42D O46D 115.0(12) . . ?
O43D Cl42D O44D 111.3(13) . . ?
O46D Cl42D O44D 112.4(13) . . ?
O43D Cl42D O45D 104.4(11) . . ?
O46D Cl42D O45D 104.6(11) . . ?
O44D Cl42D O45D 108.4(13) . . ?
O49A Cl47A O51A 107.4(8) . . ?
O49A Cl47A O50A 110.9(8) . . ?
O51A Cl47A O50A 112.5(9) . . ?
O49A Cl47A O48A 112.7(9) . . ?
O51A Cl47A O48A 108.8(8) . . ?
O50A Cl47A O48A 104.6(8) . . ?
O50B Cl47B O48B 113.6(7) . . ?
O50B Cl47B O51B 108.3(8) . . ?
O48B Cl47B O51B 108.6(7) . . ?
O50B Cl47B O49B 110.2(7) . . ?
O48B Cl47B O49B 103.1(8) . . ?
O51B Cl47B O49B 113.0(6) . . ?

_diffrn_measured_fraction_theta_max 0.998
_diffrn_reflns_theta_full        67.07
_diffrn_measured_fraction_theta_full 0.998
_refine_diff_density_max         0.989
_refine_diff_density_min         -0.943
_refine_diff_density_rms         0.083
_exptl_crystal_recrystallization_method 
'SC-SC removal of lattice water by annealing at 375 K on the diffractometer'
_exptl_crystal_preparation       'Magnetic properties'
####################################################################### 
# 
# This file contains crystal structure data downloaded from the 
# Cambridge Structural Database (CSD) hosted by the Cambridge 
# Crystallographic Data Centre (CCDC).
# 
# Full information about CCDC data access policies and citation 
# guidelines are available at http://www.ccdc.cam.ac.uk/access/V1 
# 
# Audit and citation data items may have been added by the CCDC. 
# Please retain this information to preserve the provenance of 
# this file and to allow appropriate attribution of the data. 
# 
#######################################################################

data_164h2oht
_database_code_depnum_ccdc_archive 'CCDC 1563027'
_audit_update_record             
;
2017-07-18 deposited with the CCDC.
2017-11-20 downloaded from the CCDC.
;

_audit_creation_method           SHELXL-97
_chemical_name_systematic        
'Bis[4-(isopropylsulfanyl)-2,6-di(pyrazol-1-yl)pyridine]iron(II)diperchlorate hydrate'
_chemical_name_common            ?
_chemical_melting_point          ?
_chemical_formula_moiety         'C28 H30 Fe N10 S2, 2(Cl O4), H2 O'
_chemical_formula_sum            'C28 H32 Cl2 Fe N10 O9 S2'
_chemical_formula_weight         843.51

loop_
_atom_type_symbol
_atom_type_description
_atom_type_scat_dispersion_real
_atom_type_scat_dispersion_imag
_atom_type_scat_source
Cl Cl 0.3639 0.7018 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
C C 0.0181 0.0091 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Fe Fe -1.1336 3.1974 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
N N 0.0311 0.0180 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
O O 0.0492 0.0322 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
S S 0.3331 0.5567 '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'

_symmetry_cell_setting           monoclinic
_symmetry_space_group_name_H-M   'P 21/c'

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

_cell_length_a                   20.4689(5)
_cell_length_b                   11.8194(3)
_cell_length_c                   15.6562(5)
_cell_angle_alpha                90.00
_cell_angle_beta                 103.345(3)
_cell_angle_gamma                90.00
_cell_volume                     3685.43(18)
_cell_formula_units_Z            4
_cell_measurement_temperature    250(2)
_cell_measurement_reflns_used    5776
_cell_measurement_theta_min      4.43
_cell_measurement_theta_max      72.82

_exptl_crystal_description       'rectangular prism'
_exptl_crystal_colour            yellow
_exptl_crystal_size_max          0.20
_exptl_crystal_size_mid          0.15
_exptl_crystal_size_min          0.08
_exptl_crystal_density_meas      ?
_exptl_crystal_density_diffrn    1.520
_exptl_crystal_density_method    'not measured'
_exptl_crystal_F_000             1736
_exptl_absorpt_coefficient_mu    6.233
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_correction_T_min  0.556
_exptl_absorpt_correction_T_max  1.000
_exptl_absorpt_process_details   
; 
CrysAlisPro, Agilent Technologies,
Version 1.171.36.24 (release 03-12-2012 CrysAlis171 .NET)
Empirical absorption correction using spherical harmonics,
 implemented in SCALE3 ABSPACK scaling algorithm.
;

_diffrn_ambient_temperature      250(2)
_diffrn_radiation_wavelength     1.54184
_diffrn_radiation_type           CuK\a
_diffrn_radiation_source         'SuperNova (Cu) X-ray Source'
_diffrn_radiation_monochromator  mirror
_diffrn_measurement_device_type  'SuperNova, Dual, Cu at zero, Atlas'
_diffrn_measurement_method       'ω scans'
_diffrn_detector_area_resol_mean 5.3095
_diffrn_standards_number         0
_diffrn_standards_interval_count 0
_diffrn_standards_interval_time  0
_diffrn_standards_decay_%        0
_diffrn_reflns_number            15400
_diffrn_reflns_av_R_equivalents  0.0488
_diffrn_reflns_av_sigmaI/netI    0.0512
_diffrn_reflns_limit_h_min       -17
_diffrn_reflns_limit_h_max       24
_diffrn_reflns_limit_k_min       -14
_diffrn_reflns_limit_k_max       13
_diffrn_reflns_limit_l_min       -18
_diffrn_reflns_limit_l_max       18
_diffrn_reflns_theta_min         4.35
_diffrn_reflns_theta_max         67.07
_reflns_number_total             6510
_reflns_number_gt                5170
_reflns_threshold_expression     >2sigma(I)

_computing_data_collection       'CrysAlisPro, Agilent Technologies'
_computing_cell_refinement       'CrysAlisPro, Agilent Technologies'
_computing_data_reduction        'CrysAlisPro, Agilent Technologies'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_molecular_graphics    'XSEED (Barbour, 2001)'
_computing_publication_material  'local program'

_refine_special_details          
; 
 Refinement of F² against ALL reflections.  The weighted R-factor wR and 
 goodness of fit S are based on F², conventional R-factors R are based 
 on F, with F set to zero for negative F². The threshold expression of 
 F² > 2sigma(F²) is used only for calculating R-factors(gt) etc. and is 
 not relevant to the choice of reflections for refinement.  R-factors based 
 on F² are statistically about twice as large as those based on F, and R- 
 factors based on ALL data will be even larger. 

 One of the isopropyl substitutents on the complex cation is disordered over 
 three orientations with occupancies of 0.50, 0.35 and 0.15. These were 
 modelled using the fixed restraints C---S = 1.82(2), C---C = 1.52(2), 
 1,3-C---C---C = 2.48(2) and 1,3-C---S---C = 2.83(2) Å. Both ClO₄⁻ 
 ions are also disordered, one over two sites and the other over three sites
 that shared a common wholly occupied Cl atom. The refined restraints 
 Cl---O = 1.43(2) and O...O = 2.34(2) Å were applied to those residues. 
 Finally, the water molecule is also disordered. Three partial water sites
 were identified, which were modelled with occupancies summing to 0.90 in 
 the final refinement. A whole molecule of water was included for the
 density and F(000) calculations, however, since this was clearly evident
 in a low temperature refinement from the same crystal.

 All fully occupied non-H atoms, plus the two half-occupied Cl atoms, were 
 refined anisotropically, and C-bound H atoms were placed in calculated 
 positions and refined using a riding model. The disordered water H atoms 
 were not located in the Fourier map and are not included in the refinement, 
 but are accounted for in the density and F(000) calculations.

 The disordered water molecule is positioned to hydrogen bond to the 
 disordered anion Cl42-O46, and the symmetry equivalent of the same anion 
 related by 1-x, 1-y, 1-z.
;

_refine_ls_structure_factor_coef Fsqd
_refine_ls_matrix_type           full
_refine_ls_weighting_scheme      calc
_refine_ls_weighting_details     
'calc w=1/[σ²(Fo²)+(0.1094P)²+3.8944P] 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         6510
_refine_ls_number_parameters     504
_refine_ls_number_restraints     136
_refine_ls_R_factor_all          0.0811
_refine_ls_R_factor_gt           0.0654
_refine_ls_wR_factor_ref         0.1902
_refine_ls_wR_factor_gt          0.1737
_refine_ls_goodness_of_fit_ref   1.025
_refine_ls_restrained_S_all      1.034
_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_symmetry_multiplicity
_atom_site_calc_flag
_atom_site_refinement_flags
_atom_site_disorder_assembly
_atom_site_disorder_group
Fe1 Fe 0.23115(3) 0.60466(6) 0.07556(4) 0.0373(2) Uani 1 1 d . A .
N2 N 0.12504(15) 0.6263(3) 0.0470(2) 0.0346(7) Uani 1 1 d . . .
C3 C 0.09539(19) 0.7035(3) -0.0104(3) 0.0341(8) Uani 1 1 d . . .
C4 C 0.0287(2) 0.7318(4) -0.0247(3) 0.0392(9) Uani 1 1 d . . .
H4 H 0.0093 0.7857 -0.0671 0.047 Uiso 1 1 calc R . .
C5 C -0.0090(2) 0.6767(4) 0.0269(3) 0.0406(9) Uani 1 1 d . . .
C6 C 0.0212(2) 0.5954(4) 0.0875(3) 0.0420(9) Uani 1 1 d . . .
H6 H -0.0034 0.5565 0.1220 0.050 Uiso 1 1 calc R . .
C7 C 0.0877(2) 0.5738(4) 0.0953(3) 0.0377(9) Uani 1 1 d . . .
N8 N 0.14042(16) 0.7564(3) -0.0543(2) 0.0372(7) Uani 1 1 d . . .
N9 N 0.20733(16) 0.7351(3) -0.0243(2) 0.0403(8) Uani 1 1 d . . .
C10 C 0.2370(2) 0.8003(4) -0.0720(4) 0.0543(12) Uani 1 1 d . . .
H10 H 0.2837 0.8045 -0.0658 0.065 Uiso 1 1 calc R . .
C11 C 0.1904(3) 0.8620(5) -0.1325(4) 0.0596(13) Uani 1 1 d . . .
H11 H 0.1994 0.9139 -0.1738 0.072 Uiso 1 1 calc R . .
C12 C 0.1294(2) 0.8326(4) -0.1200(3) 0.0490(11) Uani 1 1 d . . .
H12 H 0.0875 0.8601 -0.1511 0.059 Uiso 1 1 calc R . .
N13 N 0.12481(17) 0.4949(3) 0.1545(2) 0.0399(8) Uani 1 1 d . . .
N14 N 0.19212(17) 0.4866(3) 0.1617(2) 0.0419(8) Uani 1 1 d . . .
C15 C 0.2122(3) 0.4037(4) 0.2188(3) 0.0516(11) Uani 1 1 d . . .
H15 H 0.2570 0.3794 0.2374 0.062 Uiso 1 1 calc R . .
C16 C 0.1587(3) 0.3573(5) 0.2480(4) 0.0591(13) Uani 1 1 d . . .
H16 H 0.1603 0.2978 0.2883 0.071 Uiso 1 1 calc R . .
C17 C 0.1032(2) 0.4169(4) 0.2054(3) 0.0500(11) Uani 1 1 d . . .
H17 H 0.0588 0.4058 0.2104 0.060 Uiso 1 1 calc R . .
S18 S -0.09460(5) 0.69889(11) 0.01967(9) 0.0519(3) Uani 1 1 d . . .
C19 C -0.1151(2) 0.8317(4) -0.0402(3) 0.0508(11) Uani 1 1 d . . .
H19 H -0.0998 0.8280 -0.0957 0.061 Uiso 1 1 calc R . .
C20 C -0.0821(3) 0.9297(5) 0.0132(4) 0.0643(14) Uani 1 1 d . . .
H20A H -0.0931 0.9990 -0.0203 0.096 Uiso 1 1 calc R . .
H20B H -0.0338 0.9190 0.0277 0.096 Uiso 1 1 calc R . .
H20C H -0.0980 0.9347 0.0668 0.096 Uiso 1 1 calc R . .
C21 C -0.1910(3) 0.8403(6) -0.0609(4) 0.0715(16) Uani 1 1 d . . .
H21A H -0.2062 0.8412 -0.0067 0.107 Uiso 1 1 calc R . .
H21B H -0.2104 0.7758 -0.0961 0.107 Uiso 1 1 calc R . .
H21C H -0.2051 0.9095 -0.0933 0.107 Uiso 1 1 calc R . .
N22 N 0.33468(15) 0.5813(3) 0.1287(2) 0.0357(7) Uani 1 1 d . A .
C23 C 0.3697(2) 0.5058(3) 0.0935(3) 0.0387(9) Uani 1 1 d . . .
C24 C 0.4357(2) 0.4837(4) 0.1270(3) 0.0506(11) Uani 1 1 d . A .
H24 H 0.4589 0.4303 0.1006 0.061 Uiso 1 1 calc R . .
C25 C 0.46816(19) 0.5432(4) 0.2023(3) 0.0533(12) Uani 1 1 d D . .
C26 C 0.4338(2) 0.6239(4) 0.2383(3) 0.0470(10) Uani 1 1 d . A .
H26 H 0.4548 0.6660 0.2880 0.056 Uiso 1 1 calc R . .
C27 C 0.3673(2) 0.6397(4) 0.1977(3) 0.0386(9) Uani 1 1 d . . .
N28 N 0.33064(16) 0.4510(3) 0.0194(2) 0.0399(8) Uani 1 1 d . . .
N29 N 0.26414(16) 0.4765(3) -0.0063(2) 0.0380(7) Uani 1 1 d . . .
C30 C 0.2411(2) 0.4129(4) -0.0760(3) 0.0463(10) Uani 1 1 d . . .
H30 H 0.1963 0.4125 -0.1083 0.056 Uiso 1 1 calc R . .
C31 C 0.2920(3) 0.3460(5) -0.0957(3) 0.0563(12) Uani 1 1 d . . .
H31 H 0.2882 0.2938 -0.1419 0.068 Uiso 1 1 calc R . .
C32 C 0.3482(2) 0.3727(4) -0.0338(3) 0.0537(12) Uani 1 1 d . . .
H32 H 0.3913 0.3422 -0.0289 0.064 Uiso 1 1 calc R . .
N33 N 0.32550(17) 0.7213(3) 0.2249(2) 0.0421(8) Uani 1 1 d . A .
N34 N 0.26060(17) 0.7301(3) 0.1786(3) 0.0441(8) Uani 1 1 d . . .
C35 C 0.2358(3) 0.8176(4) 0.2130(4) 0.0570(12) Uani 1 1 d . A .
H35 H 0.1916 0.8442 0.1939 0.068 Uiso 1 1 calc R . .
C36 C 0.2838(3) 0.8652(4) 0.2815(4) 0.0605(13) Uani 1 1 d . . .
H36 H 0.2784 0.9277 0.3163 0.073 Uiso 1 1 calc R A .
C37 C 0.3401(3) 0.8022(4) 0.2871(3) 0.0538(12) Uani 1 1 d . A .
H37 H 0.3816 0.8129 0.3270 0.065 Uiso 1 1 calc R . .
S38A S 0.55287(12) 0.5055(3) 0.2374(2) 0.0369(6) Uiso 0.50 1 d PD A 1
C39A C 0.5832(5) 0.5866(11) 0.3380(8) 0.040(4) Uiso 0.50 1 d PD A 1
H39B H 0.5444 0.5970 0.3650 0.048 Uiso 0.50 1 calc PR A 1
C40A C 0.6008(9) 0.7025(12) 0.3087(14) 0.060(4) Uiso 0.50 1 d PD A 1
H40A H 0.5637 0.7311 0.2638 0.089 Uiso 0.50 1 calc PR A 1
H40B H 0.6406 0.6971 0.2852 0.089 Uiso 0.50 1 calc PR A 1
H40C H 0.6095 0.7537 0.3585 0.089 Uiso 0.50 1 calc PR A 1
C41A C 0.6393(7) 0.5380(15) 0.4081(10) 0.080(5) Uiso 0.50 1 d PD A 1
H41A H 0.6254 0.4656 0.4272 0.120 Uiso 0.50 1 calc PR A 1
H41B H 0.6497 0.5895 0.4576 0.120 Uiso 0.50 1 calc PR A 1
H41C H 0.6788 0.5276 0.3846 0.120 Uiso 0.50 1 calc PR A 1
S38B S 0.54629(18) 0.4870(3) 0.2631(3) 0.0466(10) Uiso 0.35 1 d PD A 2
C39B C 0.5802(9) 0.5777(16) 0.3519(12) 0.080(10) Uiso 0.35 1 d PD A 2
H39A H 0.5512 0.5812 0.3945 0.096 Uiso 0.35 1 calc PR A 2
C40B C 0.6006(17) 0.6942(19) 0.329(2) 0.099(12) Uiso 0.35 1 d PD A 2
H40D H 0.5608 0.7387 0.3048 0.148 Uiso 0.35 1 calc PR A 2
H40E H 0.6274 0.6879 0.2850 0.148 Uiso 0.35 1 calc PR A 2
H40F H 0.6268 0.7308 0.3807 0.148 Uiso 0.35 1 calc PR A 2
C41B C 0.6445(6) 0.5066(13) 0.3880(10) 0.039(3) Uiso 0.35 1 d PD A 2
H41D H 0.6318 0.4319 0.4041 0.059 Uiso 0.35 1 calc PR A 2
H41E H 0.6717 0.5437 0.4392 0.059 Uiso 0.35 1 calc PR A 2
H41F H 0.6699 0.4998 0.3431 0.059 Uiso 0.35 1 calc PR A 2
S38C S 0.5583(4) 0.5434(9) 0.2190(6) 0.048(2) Uiso 0.15 1 d PD A 3
C39C C 0.5846(8) 0.616(2) 0.3256(12) 0.028(7) Uiso 0.15 1 d PD A 3
H39C H 0.5481 0.6333 0.3556 0.033 Uiso 0.15 1 calc PR A 3
C40C C 0.612(2) 0.717(3) 0.285(3) 0.081(16) Uiso 0.15 1 d PD A 3
H40G H 0.5749 0.7625 0.2530 0.122 Uiso 0.15 1 calc PR A 3
H40H H 0.6380 0.6898 0.2441 0.122 Uiso 0.15 1 calc PR A 3
H40I H 0.6403 0.7615 0.3302 0.122 Uiso 0.15 1 calc PR A 3
C41C C 0.6439(11) 0.549(3) 0.3800(19) 0.027(6) Uiso 0.15 1 d PD A 3
H41G H 0.6272 0.4814 0.4036 0.041 Uiso 0.15 1 calc PR A 3
H41H H 0.6682 0.5952 0.4279 0.041 Uiso 0.15 1 calc PR A 3
H41I H 0.6737 0.5265 0.3429 0.041 Uiso 0.15 1 calc PR A 3
Cl42 Cl 0.45899(7) 0.72061(13) 0.50371(10) 0.0696(4) Uani 1 1 d D . .
O43A O 0.5102(5) 0.7410(9) 0.5849(5) 0.090(3) Uiso 0.50 1 d PD B 1
O44A O 0.4832(5) 0.7801(8) 0.4366(5) 0.062(2) Uiso 0.50 1 d PD B 1
O45A O 0.3969(4) 0.7629(8) 0.5126(6) 0.065(2) Uiso 0.50 1 d PD B 1
O46A O 0.4584(6) 0.6030(7) 0.4815(8) 0.104(3) Uiso 0.50 1 d PD B 1
O43B O 0.5175(8) 0.685(2) 0.5674(13) 0.139(11) Uiso 0.25 1 d PD B 2
O44B O 0.4719(10) 0.8258(12) 0.4638(13) 0.101(7) Uiso 0.25 1 d PD B 2
O45B O 0.4048(7) 0.7399(13) 0.5464(11) 0.063(4) Uiso 0.25 1 d PD B 2
O46B O 0.4396(12) 0.6350(15) 0.4376(12) 0.108(8) Uiso 0.25 1 d PD B 2
O43C O 0.5037(8) 0.7519(15) 0.4509(10) 0.074(5) Uiso 0.25 1 d PD B 3
O44C O 0.4892(8) 0.6855(15) 0.5884(7) 0.075(5) Uiso 0.25 1 d PD B 3
O45C O 0.4098(10) 0.8110(16) 0.5000(15) 0.140(11) Uiso 0.25 1 d PD B 3
O46C O 0.4181(9) 0.6256(13) 0.4546(11) 0.085(6) Uiso 0.25 1 d PD B 3
Cl7A Cl 0.0765(4) 0.9777(7) 0.2321(5) 0.061(4) Uani 0.50 1 d PD C 1
O48A O 0.1378(4) 1.0337(8) 0.2270(7) 0.059(3) Uiso 0.50 1 d PD C 1
O49A O 0.0170(4) 1.0435(9) 0.2003(7) 0.066(3) Uiso 0.50 1 d PD C 1
O50A O 0.0828(4) 0.9548(7) 0.3249(4) 0.0557(19) Uiso 0.50 1 d PD C 1
O51A O 0.0688(5) 0.8741(7) 0.1829(6) 0.068(3) Uiso 0.50 1 d PD C 1
Cl7B Cl 0.0754(2) 0.9835(7) 0.2317(4) 0.049(3) Uani 0.50 1 d PD D 2
O48B O 0.1387(5) 1.0408(10) 0.2494(8) 0.085(4) Uiso 0.50 1 d PD D 2
O49B O 0.0259(5) 1.0701(8) 0.2039(7) 0.070(4) Uiso 0.50 1 d PD D 2
O50B O 0.0647(5) 0.9237(7) 0.3065(5) 0.067(2) Uiso 0.50 1 d PD D 2
O51B O 0.0750(4) 0.9028(7) 0.1616(5) 0.065(2) Uiso 0.50 1 d PD D 2
O52A O 0.6260(9) 0.5889(18) 0.6579(12) 0.080(5) Uiso 0.35 1 d P E 1
O52B O 0.6352(18) 0.548(3) 0.626(3) 0.075(10) Uiso 0.15 1 d P F 2
O52C O 0.6320(10) 0.5910(19) 0.6320(14) 0.085(6) Uiso 0.40 1 d P G 3


_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 N22 2.108(3) . ?
Fe1 N2 2.129(3) . ?
Fe1 N9 2.169(4) . ?
Fe1 N34 2.171(4) . ?
Fe1 N29 2.189(4) . ?
Fe1 N14 2.213(4) . ?
N2 C3 1.325(5) . ?
N2 C7 1.345(5) . ?
C3 C4 1.373(5) . ?
C3 N8 1.416(5) . ?
C4 C5 1.399(6) . ?
C4 H4 0.9400 . ?
C5 C6 1.393(6) . ?
C5 S18 1.749(4) . ?
C6 C7 1.362(6) . ?
C6 H6 0.9400 . ?
C7 N13 1.406(5) . ?
N8 C12 1.347(6) . ?
N8 N9 1.365(5) . ?
N9 C10 1.315(6) . ?
C10 C11 1.386(7) . ?
C10 H10 0.9400 . ?
C11 C12 1.354(7) . ?
C11 H11 0.9400 . ?
C12 H12 0.9400 . ?
N13 C17 1.358(6) . ?
N13 N14 1.360(5) . ?
N14 C15 1.327(6) . ?
C15 C16 1.393(8) . ?
C15 H15 0.9400 . ?
C16 C17 1.371(7) . ?
C16 H16 0.9400 . ?
C17 H17 0.9400 . ?
S18 C19 1.827(5) . ?
C19 C20 1.496(7) . ?
C19 C21 1.517(6) . ?
C19 H19 0.9900 . ?
C20 H20A 0.9700 . ?
C20 H20B 0.9700 . ?
C20 H20C 0.9700 . ?
C21 H21A 0.9700 . ?
C21 H21B 0.9700 . ?
C21 H21C 0.9700 . ?
N22 C27 1.326(5) . ?
N22 C23 1.340(5) . ?
C23 C24 1.357(6) . ?
C23 N28 1.406(5) . ?
C24 C25 1.401(7) . ?
C24 H24 0.9400 . ?
C25 C26 1.381(7) . ?
C25 S38A 1.751(4) . ?
C25 S38B 1.790(5) . ?
C25 S38C 1.803(8) . ?
C26 C27 1.375(6) . ?
C26 H26 0.9400 . ?
C27 N33 1.418(5) . ?
N28 C32 1.347(6) . ?
N28 N29 1.361(5) . ?
N29 C30 1.320(6) . ?
C30 C31 1.397(7) . ?
C30 H30 0.9400 . ?
C31 C32 1.359(7) . ?
C31 H31 0.9400 . ?
C32 H32 0.9400 . ?
N33 C37 1.349(6) . ?
N33 N34 1.362(5) . ?
N34 C35 1.321(6) . ?
C35 C36 1.395(8) . ?
C35 H35 0.9400 . ?
C36 C37 1.358(7) . ?
C36 H36 0.9400 . ?
C37 H37 0.9400 . ?
S38A C39A 1.826(8) . ?
C39A C41A 1.507(11) . ?
C39A C40A 1.514(12) . ?
C39A H39B 0.9900 . ?
C40A H40A 0.9700 . ?
C40A H40B 0.9700 . ?
C40A H40C 0.9700 . ?
C41A H41A 0.9700 . ?
C41A H41B 0.9700 . ?
C41A H41C 0.9700 . ?
S38B C39B 1.766(12) . ?
C39B C40B 1.508(14) . ?
C39B C41B 1.552(13) . ?
C39B H39A 0.9900 . ?
C40B H40D 0.9700 . ?
C40B H40E 0.9700 . ?
C40B H40F 0.9700 . ?
C41B H41D 0.9700 . ?
C41B H41E 0.9700 . ?
C41B H41F 0.9700 . ?
S38C C39C 1.843(12) . ?
C39C C40C 1.518(14) . ?
C39C C41C 1.535(14) . ?
C39C H39C 0.9900 . ?
C40C H40G 0.9700 . ?
C40C H40H 0.9700 . ?
C40C H40I 0.9700 . ?
C41C H41G 0.9700 . ?
C41C H41H 0.9700 . ?
C41C H41I 0.9700 . ?
Cl42 O45A 1.403(7) . ?
Cl42 O46A 1.433(8) . ?
Cl42 O44A 1.444(6) . ?
Cl42 O43A 1.469(8) . ?
Cl42 O43B 1.432(11) . ?
Cl42 O46B 1.437(11) . ?
Cl42 O45B 1.439(10) . ?
Cl42 O44B 1.443(11) . ?
Cl42 O44C 1.390(10) . ?
Cl42 O43C 1.416(10) . ?
Cl42 O45C 1.461(11) . ?
Cl42 O46C 1.502(10) . ?
Cl7A O49A 1.433(9) . ?
Cl7A O51A 1.436(9) . ?
Cl7A O48A 1.438(9) . ?
Cl7A O50A 1.454(9) . ?
Cl7B O50B 1.429(8) . ?
Cl7B O48B 1.432(9) . ?
Cl7B O49B 1.436(8) . ?
Cl7B O51B 1.452(8) . ?

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
N22 Fe1 N2 169.20(13) . . ?
N22 Fe1 N9 114.55(13) . . ?
N2 Fe1 N9 73.40(12) . . ?
N22 Fe1 N34 73.45(13) . . ?
N2 Fe1 N34 99.72(13) . . ?
N9 Fe1 N34 91.62(15) . . ?
N22 Fe1 N29 73.88(13) . . ?
N2 Fe1 N29 113.43(13) . . ?
N9 Fe1 N29 96.77(13) . . ?
N34 Fe1 N29 146.84(13) . . ?
N22 Fe1 N14 98.54(13) . . ?
N2 Fe1 N14 73.13(13) . . ?
N9 Fe1 N14 146.52(12) . . ?
N34 Fe1 N14 93.16(15) . . ?
N29 Fe1 N14 97.13(14) . . ?
C3 N2 C7 118.0(3) . . ?
C3 N2 Fe1 120.7(3) . . ?
C7 N2 Fe1 120.7(3) . . ?
N2 C3 C4 124.1(4) . . ?
N2 C3 N8 112.7(3) . . ?
C4 C3 N8 123.2(4) . . ?
C3 C4 C5 117.0(4) . . ?
C3 C4 H4 121.5 . . ?
C5 C4 H4 121.5 . . ?
C6 C5 C4 119.8(4) . . ?
C6 C5 S18 115.4(3) . . ?
C4 C5 S18 124.8(3) . . ?
C7 C6 C5 117.9(4) . . ?
C7 C6 H6 121.0 . . ?
C5 C6 H6 121.0 . . ?
N2 C7 C6 123.3(4) . . ?
N2 C7 N13 112.7(3) . . ?
C6 C7 N13 124.0(4) . . ?
C12 N8 N9 111.4(3) . . ?
C12 N8 C3 130.7(4) . . ?
N9 N8 C3 117.7(3) . . ?
C10 N9 N8 104.7(3) . . ?
C10 N9 Fe1 140.3(3) . . ?
N8 N9 Fe1 114.8(2) . . ?
N9 C10 C11 111.3(4) . . ?
N9 C10 H10 124.4 . . ?
C11 C10 H10 124.4 . . ?
C12 C11 C10 106.2(4) . . ?
C12 C11 H11 126.9 . . ?
C10 C11 H11 126.9 . . ?
N8 C12 C11 106.5(4) . . ?
N8 C12 H12 126.8 . . ?
C11 C12 H12 126.8 . . ?
C17 N13 N14 111.3(4) . . ?
C17 N13 C7 129.6(4) . . ?
N14 N13 C7 119.0(3) . . ?
C15 N14 N13 105.0(4) . . ?
C15 N14 Fe1 141.0(3) . . ?
N13 N14 Fe1 113.9(3) . . ?
N14 C15 C16 111.6(4) . . ?
N14 C15 H15 124.2 . . ?
C16 C15 H15 124.2 . . ?
C17 C16 C15 105.3(4) . . ?
C17 C16 H16 127.4 . . ?
C15 C16 H16 127.4 . . ?
N13 C17 C16 106.8(4) . . ?
N13 C17 H17 126.6 . . ?
C16 C17 H17 126.6 . . ?
C5 S18 C19 105.6(2) . . ?
C20 C19 C21 112.1(5) . . ?
C20 C19 S18 111.0(4) . . ?
C21 C19 S18 105.7(4) . . ?
C20 C19 H19 109.4 . . ?
C21 C19 H19 109.4 . . ?
S18 C19 H19 109.4 . . ?
C19 C20 H20A 109.5 . . ?
C19 C20 H20B 109.5 . . ?
H20A C20 H20B 109.5 . . ?
C19 C20 H20C 109.5 . . ?
H20A C20 H20C 109.5 . . ?
H20B C20 H20C 109.5 . . ?
C19 C21 H21A 109.5 . . ?
C19 C21 H21B 109.5 . . ?
H21A C21 H21B 109.5 . . ?
C19 C21 H21C 109.5 . . ?
H21A C21 H21C 109.5 . . ?
H21B C21 H21C 109.5 . . ?
C27 N22 C23 117.7(3) . . ?
C27 N22 Fe1 121.6(3) . . ?
C23 N22 Fe1 120.7(3) . . ?
N22 C23 C24 123.3(4) . . ?
N22 C23 N28 112.9(3) . . ?
C24 C23 N28 123.8(4) . . ?
C23 C24 C25 117.7(4) . . ?
C23 C24 H24 121.1 . . ?
C25 C24 H24 121.1 . . ?
C26 C25 C24 120.2(4) . . ?
C26 C25 S38A 127.5(4) . . ?
C24 C25 S38A 112.3(3) . . ?
C26 C25 S38B 121.1(4) . . ?
C24 C25 S38B 116.9(4) . . ?
C26 C25 S38C 122.7(4) . . ?
C24 C25 S38C 113.2(4) . . ?
C27 C26 C25 116.6(4) . . ?
C27 C26 H26 121.7 . . ?
C25 C26 H26 121.7 . . ?
N22 C27 C26 124.4(4) . . ?
N22 C27 N33 111.9(3) . . ?
C26 C27 N33 123.7(4) . . ?
C32 N28 N29 111.1(4) . . ?
C32 N28 C23 130.1(4) . . ?
N29 N28 C23 118.8(3) . . ?
C30 N29 N28 105.0(3) . . ?
C30 N29 Fe1 141.2(3) . . ?
N28 N29 Fe1 113.8(2) . . ?
N29 C30 C31 111.3(4) . . ?
N29 C30 H30 124.3 . . ?
C31 C30 H30 124.3 . . ?
C32 C31 C30 105.2(4) . . ?
C32 C31 H31 127.4 . . ?
C30 C31 H31 127.4 . . ?
N28 C32 C31 107.4(4) . . ?
N28 C32 H32 126.3 . . ?
C31 C32 H32 126.3 . . ?
C37 N33 N34 110.9(4) . . ?
C37 N33 C27 130.5(4) . . ?
N34 N33 C27 118.3(3) . . ?
C35 N34 N33 105.2(4) . . ?
C35 N34 Fe1 140.4(3) . . ?
N33 N34 Fe1 114.3(2) . . ?
N34 C35 C36 111.1(4) . . ?
N34 C35 H35 124.4 . . ?
C36 C35 H35 124.4 . . ?
C37 C36 C35 105.4(4) . . ?
C37 C36 H36 127.3 . . ?
C35 C36 H36 127.3 . . ?
N33 C37 C36 107.4(4) . . ?
N33 C37 H37 126.3 . . ?
C36 C37 H37 126.3 . . ?
C25 S38A C39A 104.6(4) . . ?
C41A C39A C40A 111.8(9) . . ?
C41A C39A S38A 118.6(9) . . ?
C40A C39A S38A 105.8(11) . . ?
C41A C39A H39B 106.7 . . ?
C40A C39A H39B 106.7 . . ?
S38A C39A H39B 106.7 . . ?
C39A C40A H40A 109.5 . . ?
C39A C40A H40B 109.5 . . ?
H40A C40A H40B 109.5 . . ?
C39A C40A H40C 109.5 . . ?
H40A C40A H40C 109.5 . . ?
H40B C40A H40C 109.5 . . ?
C39A C41A H41A 109.5 . . ?
C39A C41A H41B 109.5 . . ?
H41A C41A H41B 109.5 . . ?
C39A C41A H41C 109.5 . . ?
H41A C41A H41C 109.5 . . ?
H41B C41A H41C 109.5 . . ?
C39B S38B C25 109.5(6) . . ?
C40B C39B C41B 108.9(12) . . ?
C40B C39B S38B 116(2) . . ?
C41B C39B S38B 96.0(10) . . ?
C40B C39B H39A 111.5 . . ?
C41B C39B H39A 111.5 . . ?
S38B C39B H39A 111.5 . . ?
C39B C40B H40D 109.5 . . ?
C39B C40B H40E 109.5 . . ?
H40D C40B H40E 109.5 . . ?
C39B C40B H40F 109.5 . . ?
H40D C40B H40F 109.5 . . ?
H40E C40B H40F 109.5 . . ?
C39B C41B H41D 109.5 . . ?
C39B C41B H41E 109.5 . . ?
H41D C41B H41E 109.5 . . ?
C39B C41B H41F 109.5 . . ?
H41D C41B H41F 109.5 . . ?
H41E C41B H41F 109.5 . . ?
C25 S38C C39C 101.9(7) . . ?
C40C C39C C41C 108.7(13) . . ?
C40C C39C S38C 92(2) . . ?
C41C C39C S38C 106.8(17) . . ?
C40C C39C H39C 115.5 . . ?
C41C C39C H39C 115.5 . . ?
S38C C39C H39C 115.5 . . ?
C39C C40C H40G 109.5 . . ?
C39C C40C H40H 109.5 . . ?
H40G C40C H40H 109.5 . . ?
C39C C40C H40I 109.5 . . ?
H40G C40C H40I 109.5 . . ?
H40H C40C H40I 109.5 . . ?
C39C C41C H41G 109.5 . . ?
C39C C41C H41H 109.5 . . ?
H41G C41C H41H 109.5 . . ?
C39C C41C H41I 109.5 . . ?
H41G C41C H41I 109.5 . . ?
H41H C41C H41I 109.5 . . ?
O45A Cl42 O46A 114.4(6) . . ?
O45A Cl42 O44A 111.7(5) . . ?
O46A Cl42 O44A 106.3(5) . . ?
O45A Cl42 O43A 109.8(5) . . ?
O46A Cl42 O44A 106.3(5) . . ?
O46A Cl42 O43A 109.5(6) . . ?
O44A Cl42 O43A 104.7(5) . . ?
O43B Cl42 O46B 110.1(10) . . ?
O43B Cl42 O45B 109.4(9) . . ?
O46B Cl42 O45B 109.4(9) . . ?
O43B Cl42 O44B 110.2(10) . . ?
O46B Cl42 O44B 110.0(9) . . ?
O45B Cl42 O44B 107.6(8) . . ?
O44C Cl42 O43C 115.5(9) . . ?
O44C Cl42 O45C 114.0(9) . . ?
O43C Cl42 O45C 108.6(9) . . ?
O44C Cl42 O46C 109.7(8) . . ?
O43C Cl42 O46C 104.8(8) . . ?
O43B Cl42 O46C 114.6(14) . . ?
O45C Cl42 O46C 103.3(9) . . ?
O49A Cl7A O51A 107.3(7) . . ?
O49A Cl7A O48A 114.4(8) . . ?
O51A Cl7A O48A 110.6(7) . . ?
O49A Cl7A O50A 108.7(7) . . ?
O51A Cl7A O50A 110.6(7) . . ?
O48A Cl7A O50A 105.3(7) . . ?
O50B Cl7B O48B 112.2(7) . . ?
O50B Cl7B O49B 111.7(6) . . ?
O48B Cl7B O49B 105.4(8) . . ?
O50B Cl7B O51B 108.6(7) . . ?
O48B Cl7B O51B 107.7(7) . . ?
O49B Cl7B O51B 111.0(6) . . ?

_diffrn_measured_fraction_theta_max 0.989
_diffrn_reflns_theta_full        67.07
_diffrn_measured_fraction_theta_full 0.989
_refine_diff_density_max         0.982
_refine_diff_density_min         -1.033
_refine_diff_density_rms         0.089
_exptl_crystal_recrystallization_method 
'SC-SC atmospheric moisture replacement of acetone solvate'
_exptl_crystal_preparation       'Magnetic properties'
####################################################################### 
# 
# This file contains crystal structure data downloaded from the 
# Cambridge Structural Database (CSD) hosted by the Cambridge 
# Crystallographic Data Centre (CCDC).
# 
# Full information about CCDC data access policies and citation 
# guidelines are available at http://www.ccdc.cam.ac.uk/access/V1 
# 
# Audit and citation data items may have been added by the CCDC. 
# Please retain this information to preserve the provenance of 
# this file and to allow appropriate attribution of the data. 
# 
#######################################################################

data_rk137MeCNPI_015K
_database_code_depnum_ccdc_archive 'CCDC 1564669'
_audit_update_record             
;
2017-07-28 deposited with the CCDC.
2017-11-20 downloaded from the CCDC.
;
_chemical_name_common            ?
_chemical_name_systematic        ?
_chemical_formula_moiety         'C28 H30 Fe N10 S2, C2 H3 N, 2(B F4)'
_chemical_formula_sum            'C30 H33 B2 F8 Fe N11 S2'
_chemical_formula_weight         841.26
_chemical_melting_point          'not measured'
loop_
_atom_type_symbol
_atom_type_description
_atom_type_scat_dispersion_real
_atom_type_scat_dispersion_imag
_atom_type_scat_source
C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
B B 0.0013 0.0007 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
F F 0.0171 0.0103 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Fe Fe 0.3463 0.8444 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
S S 0.1246 0.1234 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'

_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.
;
_space_group_crystal_system      monoclinic
_space_group_IT_number           14
_space_group_name_H-M_alt        'P 1 21/c 1'
_space_group_name_Hall           '-P 2ybc'
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                   20.2280(5)
_cell_length_b                   11.8526(4)
_cell_length_c                   15.5284(4)
_cell_angle_alpha                90
_cell_angle_beta                 99.208(2)
_cell_angle_gamma                90
_cell_volume                     3675.03(18)
_cell_formula_units_Z            4
_cell_measurement_reflns_used    4950
_cell_measurement_temperature    15(1)
_cell_measurement_theta_max      31.6220
_cell_measurement_theta_min      3.1820
_exptl_absorpt_coefficient_mu    0.605
_exptl_absorpt_correction_T_max  0.954
_exptl_absorpt_correction_T_min  0.842
_exptl_absorpt_correction_type   analytical
_exptl_absorpt_process_details   
;
CrysAlisPro, Agilent Technologies,
Version 1.171.37.35 (release 13-08-2014 CrysAlis171 .NET)
(compiled Aug 13 2014,18:06:01)
Analytical numeric absorption correction using a multifaceted crystal
			model based on expressions derived by R.C. Clark & J.S. Reid.
(Clark, R. C. & Reid, J. S. (1995). Acta Cryst. A51, 887-897)
Empirical absorption correction using spherical harmonics,
 implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_absorpt_special_details   ?
_exptl_crystal_colour            'light orange'
_exptl_crystal_density_diffrn    1.520
_exptl_crystal_density_meas      'not measured'
_exptl_crystal_density_method    none
_exptl_crystal_description       block
_exptl_crystal_F_000             1720
_exptl_crystal_size_max          0.5026
_exptl_crystal_size_mid          0.1566
_exptl_crystal_size_min          0.0797
_exptl_transmission_factor_max   ?
_exptl_transmission_factor_min   ?
_diffrn_reflns_av_R_equivalents  0.0520
_diffrn_reflns_av_unetI/netI     0.0747
_diffrn_reflns_Laue_measured_fraction_full 0.998
_diffrn_reflns_Laue_measured_fraction_max 0.998
_diffrn_reflns_limit_h_max       25
_diffrn_reflns_limit_h_min       -24
_diffrn_reflns_limit_k_max       14
_diffrn_reflns_limit_k_min       -15
_diffrn_reflns_limit_l_max       16
_diffrn_reflns_limit_l_min       -19
_diffrn_reflns_number            19748
_diffrn_reflns_point_group_measured_fraction_full 0.998
_diffrn_reflns_point_group_measured_fraction_max 0.998
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         26.999
_diffrn_reflns_theta_min         3.081
_diffrn_ambient_temperature      15(1)
_diffrn_detector                 'CCD plate'
_diffrn_detector_area_resol_mean 16.1852
_diffrn_detector_type            Sapphire3
_diffrn_measured_fraction_theta_full 0.998
_diffrn_measured_fraction_theta_max 0.998
_diffrn_measurement_details      
;
#__ type_ start__ end____ width___ exp.time_
  1 omega   12.00  105.00   1.0000    7.5000
omega____ theta____ kappa____ phi______ frames
    -       32.4262   38.0000   30.0000 93

#__ type_ start__ end____ width___ exp.time_
  2 omega  -57.00   -2.00   1.0000    7.5000
omega____ theta____ kappa____ phi______ frames
    -      -30.3949    0.0000 -180.0000 55

#__ type_ start__ end____ width___ exp.time_
  3 omega  -77.00  -37.00   1.0000    7.5000
omega____ theta____ kappa____ phi______ frames
    -      -30.3949  103.0000  156.3300 40

#__ type_ start__ end____ width___ exp.time_
  4 omega -109.00  -56.00   1.0000    7.5000
omega____ theta____ kappa____ phi______ frames
    -      -30.3949 -178.0000 -180.0000 53

#__ type_ start__ end____ width___ exp.time_
  5 omega  -90.00  -63.00   1.0000    7.5000
omega____ theta____ kappa____ phi______ frames
    -      -30.3949 -178.0000 -150.0000 27

#__ type_ start__ end____ width___ exp.time_
  6 omega -109.00  -59.00   1.0000    7.5000
omega____ theta____ kappa____ phi______ frames
    -      -30.3949 -178.0000    0.0000 50
;
_diffrn_measurement_device       'four-circle diffractometer'
_diffrn_measurement_device_type  'Xcalibur, Sapphire3'
_diffrn_measurement_method       'ω scans'
_diffrn_orient_matrix_UB_11      -0.0008170000
_diffrn_orient_matrix_UB_12      -0.0562197000
_diffrn_orient_matrix_UB_13      0.0118714000
_diffrn_orient_matrix_UB_21      -0.0055698000
_diffrn_orient_matrix_UB_22      0.0203727000
_diffrn_orient_matrix_UB_23      0.0320145000
_diffrn_orient_matrix_UB_31      -0.0459424000
_diffrn_orient_matrix_UB_32      -0.0014941000
_diffrn_orient_matrix_UB_33      -0.0098303000
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_source                   'Enhance (Mo) X-ray Source'
_reflns_Friedel_coverage         0.000
_reflns_Friedel_fraction_full    .
_reflns_Friedel_fraction_max     .
_reflns_number_gt                5813
_reflns_number_total             7998
_reflns_odcompleteness_completeness 99.80
_reflns_odcompleteness_iscentric 1
_reflns_odcompleteness_theta     26.32
_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.
;
_reflns_threshold_expression     'I > 2σ(I)'
_computing_cell_refinement       'CrysAlisPro 1.171.38.46 (Rigaku OD, 2015)'
_computing_data_collection       'CrysAlisPro 1.171.37.31c (Rigaku OD, 2014)'
_computing_data_reduction        'CrysAlisPro 1.171.38.46 (Rigaku OD, 2015)'
_computing_molecular_graphics    'Mercury3.9 (2016)'
_computing_publication_material  'Olex2 (Dolomanov et al., 2009)'
_computing_structure_refinement  'ShelXL (Sheldrick, 2015)'
_computing_structure_solution    'ShelXT (Sheldrick, 2015)'
_refine_diff_density_max         0.659
_refine_diff_density_min         -0.486
_refine_diff_density_rms         0.088
_refine_ls_extinction_coef       .
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.059
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     492
_refine_ls_number_reflns         7998
_refine_ls_number_restraints     0
_refine_ls_R_factor_all          0.0798
_refine_ls_R_factor_gt           0.0511
_refine_ls_restrained_S_all      1.059
_refine_ls_shift/su_max          0.000
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details     
'w=1/[σ²(Fo²)+(0.0530P)²+0.7738P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1133
_refine_ls_wR_factor_ref         0.1275
_refine_special_details          
;
Structure of high spin state at 15K. 
Sample was either tapped in its high spin phase or photo-exited to 
its high spin phase with the light during sample alignement.
OMIT command has been applied for not well measured Brag reflections.
;
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     dual
_atom_sites_solution_secondary   difmap
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 0.27817(2) 0.60181(4) 0.44402(3) 0.01286(12) Uani 1 1 d . . . . .
S1 S 0.60209(4) 0.71169(7) 0.47833(5) 0.01550(17) Uani 1 1 d . . . . .
S2 S -0.03972(4) 0.50187(7) 0.28154(5) 0.01649(18) Uani 1 1 d . . . . .
N7 N 0.17710(13) 0.4424(2) 0.49944(14) 0.0138(5) Uani 1 1 d . . . . .
N1 N 0.32116(13) 0.4811(2) 0.36099(15) 0.0150(5) Uani 1 1 d . . . . .
N2 N 0.38869(13) 0.4948(2) 0.36150(15) 0.0146(5) Uani 1 1 d . . . . .
N8 N 0.17584(12) 0.5755(2) 0.39326(14) 0.0128(5) Uani 1 1 d . . . . .
N6 N 0.24228(12) 0.4738(2) 0.52519(15) 0.0141(5) Uani 1 1 d . . . . .
N4 N 0.36431(12) 0.7562(2) 0.56953(14) 0.0131(5) Uani 1 1 d . . . . .
N5 N 0.29790(13) 0.7331(2) 0.54209(15) 0.0153(6) Uani 1 1 d . . . . .
N9 N 0.18740(13) 0.7183(2) 0.29899(14) 0.0141(5) Uani 1 1 d . . . . .
N10 N 0.25171(13) 0.7278(2) 0.34342(15) 0.0148(5) Uani 1 1 d . . . . .
N3 N 0.38338(13) 0.6270(2) 0.46746(15) 0.0136(5) Uani 1 1 d . . . . .
C6 C 0.51719(15) 0.6855(3) 0.47724(18) 0.0147(6) Uani 1 1 d . . . . .
C1 C 0.30451(16) 0.3926(3) 0.30978(18) 0.0170(7) Uani 1 1 d . . . . .
H1 H 0.2615 0.3631 0.2973 0.020 Uiso 1 1 calc R . . . .
C9 C 0.37301(16) 0.8346(3) 0.63371(18) 0.0170(7) Uani 1 1 d . . . . .
H9 H 0.4137 0.8627 0.6620 0.020 Uiso 1 1 calc R . . . .
C10 C 0.31078(16) 0.8645(3) 0.64889(19) 0.0187(7) Uani 1 1 d . . . . .
H10 H 0.3003 0.9166 0.6894 0.022 Uiso 1 1 calc R . . . .
C12 C 0.61874(16) 0.8473(3) 0.53329(19) 0.0166(7) Uani 1 1 d . . . . .
H12 H 0.6031 0.8449 0.5898 0.020 Uiso 1 1 calc R . . . .
C28 C -0.07641(17) 0.7228(3) 0.2409(2) 0.0227(7) Uani 1 1 d . . . . .
H28A H -0.1100 0.7162 0.2778 0.034 Uiso 1 1 calc GR . . . .
H28B H -0.0903 0.7777 0.1962 0.034 Uiso 1 1 calc GR . . . .
H28C H -0.0349 0.7460 0.2751 0.034 Uiso 1 1 calc GR . . . .
C3 C 0.41274(16) 0.4152(3) 0.31077(18) 0.0171(7) Uani 1 1 d . . . . .
H3 H 0.4568 0.4078 0.3013 0.020 Uiso 1 1 calc R . . . .
C2 C 0.36016(16) 0.3492(3) 0.27678(18) 0.0184(7) Uani 1 1 d . . . . .
H2 H 0.3608 0.2880 0.2395 0.022 Uiso 1 1 calc R . . . .
C8 C 0.41109(15) 0.7070(3) 0.52245(17) 0.0128(6) Uani 1 1 d . . . . .
C26 C -0.06709(16) 0.6100(3) 0.19919(19) 0.0173(7) Uani 1 1 d . . . . .
H26 H -0.0332 0.6176 0.1609 0.021 Uiso 1 1 calc R . . . .
C23 C 0.17370(16) 0.8026(3) 0.23895(18) 0.0162(7) Uani 1 1 d . . . . .
H23 H 0.1335 0.8143 0.2017 0.019 Uiso 1 1 calc R . . . .
C17 C 0.15849(17) 0.3612(3) 0.55252(18) 0.0182(7) Uani 1 1 d . . . . .
H17 H 0.1165 0.3278 0.5481 0.022 Uiso 1 1 calc R . . . .
C22 C 0.14512(15) 0.6362(3) 0.32623(17) 0.0136(6) Uani 1 1 d . . . . .
C16 C 0.21328(16) 0.3380(3) 0.61355(19) 0.0188(7) Uani 1 1 d . . . . .
H16 H 0.2164 0.2854 0.6585 0.023 Uiso 1 1 calc R . . . .
C19 C 0.07387(15) 0.4745(2) 0.39518(17) 0.0134(6) Uani 1 1 d . . . . .
H19 H 0.0505 0.4194 0.4206 0.016 Uiso 1 1 calc R . . . .
C20 C 0.04329(15) 0.5374(3) 0.32280(18) 0.0143(6) Uani 1 1 d . . . . .
C11 C 0.26583(16) 0.8000(3) 0.59028(18) 0.0169(7) Uani 1 1 d . . . . .
H11 H 0.2195 0.8037 0.5858 0.020 Uiso 1 1 calc R . . . .
C25 C 0.27713(16) 0.8171(3) 0.30971(18) 0.0165(7) Uani 1 1 d . . . . .
H25 H 0.3204 0.8438 0.3272 0.020 Uiso 1 1 calc R . . . .
C21 C 0.07970(15) 0.6201(3) 0.28778(18) 0.0136(6) Uani 1 1 d . . . . .
H21 H 0.0606 0.6630 0.2401 0.016 Uiso 1 1 calc R . . . .
C13 C 0.69457(16) 0.8623(3) 0.5478(2) 0.0206(7) Uani 1 1 d . . . . .
H13A H 0.7153 0.8016 0.5832 0.031 Uiso 1 1 calc GR . . . .
H13B H 0.7061 0.9328 0.5768 0.031 Uiso 1 1 calc GR . . . .
H13C H 0.7101 0.8620 0.4925 0.031 Uiso 1 1 calc GR . . . .
C24 C 0.23026(16) 0.8665(3) 0.24407(18) 0.0173(7) Uani 1 1 d . . . . .
H24 H 0.2365 0.9298 0.2109 0.021 Uiso 1 1 calc R . . . .
C5 C 0.48909(15) 0.6023(3) 0.41895(17) 0.0143(6) Uani 1 1 d . . . . .
H5 H 0.5145 0.5654 0.3827 0.017 Uiso 1 1 calc R . . . .
C14 C 0.58276(16) 0.9418(3) 0.47817(19) 0.0194(7) Uani 1 1 d . . . . .
H14A H 0.6000 0.9474 0.4243 0.029 Uiso 1 1 calc GR . . . .
H14B H 0.5899 1.0118 0.5093 0.029 Uiso 1 1 calc GR . . . .
H14C H 0.5357 0.9257 0.4662 0.029 Uiso 1 1 calc GR . . . .
C7 C 0.47735(15) 0.7391(3) 0.53178(17) 0.0142(6) Uani 1 1 d . . . . .
H7 H 0.4949 0.7936 0.5721 0.017 Uiso 1 1 calc R . . . .
C27 C -0.13202(16) 0.5661(3) 0.1457(2) 0.0241(8) Uani 1 1 d . . . . .
H27A H -0.1239 0.4945 0.1206 0.036 Uiso 1 1 calc GR . . . .
H27B H -0.1477 0.6188 0.1000 0.036 Uiso 1 1 calc GR . . . .
H27C H -0.1653 0.5575 0.1829 0.036 Uiso 1 1 calc GR . . . .
C18 C 0.13942(15) 0.4977(3) 0.42651(17) 0.0131(6) Uani 1 1 d . . . . .
C4 C 0.42281(16) 0.5770(3) 0.41710(17) 0.0140(6) Uani 1 1 d . . . . .
C15 C 0.26365(16) 0.4098(3) 0.59434(18) 0.0174(7) Uani 1 1 d . . . . .
H15 H 0.3067 0.4125 0.6260 0.021 Uiso 1 1 calc R . . . .
N11 N 0.18148(16) 0.4586(3) 0.16950(19) 0.0339(8) Uani 1 1 d . . . . .
C30 C 0.06541(18) 0.4390(3) 0.0734(2) 0.0280(8) Uani 1 1 d . . . . .
H30A H 0.0589 0.4998 0.0320 0.042 Uiso 1 1 calc GR . . . .
H30B H 0.0314 0.4420 0.1099 0.042 Uiso 1 1 calc GR . . . .
H30C H 0.0626 0.3684 0.0428 0.042 Uiso 1 1 calc GR . . . .
C29 C 0.13090(17) 0.4494(3) 0.1269(2) 0.0220(7) Uani 1 1 d . . . . .
F1 F 0.43023(9) 0.59503(16) 0.83635(11) 0.0219(4) Uani 1 1 d . . . . .
F4 F 0.47495(9) 0.43052(16) 0.79570(11) 0.0215(4) Uani 1 1 d . . . . .
F3 F 0.42615(9) 0.55457(16) 0.69185(10) 0.0212(4) Uani 1 1 d . . . . .
F2 F 0.36144(9) 0.45538(16) 0.77279(10) 0.0201(4) Uani 1 1 d . . . . .
B1 B 0.42276(19) 0.5093(3) 0.7748(2) 0.0176(8) Uani 1 1 d . . . . .
F8 F 0.11111(9) 0.66051(16) 0.54470(10) 0.0219(4) Uani 1 1 d . . . . .
F6 F 0.00320(9) 0.68609(16) 0.47493(11) 0.0213(4) Uani 1 1 d . . . . .
F7 F 0.08331(10) 0.81696(16) 0.46134(11) 0.0264(5) Uani 1 1 d . . . . .
F5 F 0.04525(10) 0.79535(18) 0.59072(11) 0.0288(5) Uani 1 1 d . . . . .
B2 B 0.06117(19) 0.7399(3) 0.5174(2) 0.0168(8) 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 N1 2.197(3) . ?
Fe1 N8 2.117(2) . ?
Fe1 N6 2.171(3) . ?
Fe1 N5 2.169(3) . ?
Fe1 N10 2.166(2) . ?
Fe1 N3 2.122(3) . ?
S1 C6 1.743(3) . ?
S1 C12 1.825(3) . ?
S2 C26 1.832(3) . ?
S2 C20 1.750(3) . ?
N7 N6 1.367(3) . ?
N7 C17 1.359(4) . ?
N7 C18 1.420(4) . ?
N1 N2 1.374(3) . ?
N1 C1 1.326(4) . ?
N2 C3 1.367(4) . ?
N2 C4 1.407(4) . ?
N8 C22 1.335(4) . ?
N8 C18 1.334(4) . ?
N6 C15 1.329(4) . ?
N4 N5 1.370(3) . ?
N4 C9 1.354(4) . ?
N4 C8 1.411(4) . ?
N5 C11 1.329(4) . ?
N9 N10 1.376(3) . ?
N9 C23 1.364(4) . ?
N9 C22 1.404(4) . ?
N10 C25 1.321(4) . ?
N3 C8 1.337(4) . ?
N3 C4 1.341(4) . ?
C6 C5 1.396(4) . ?
C6 C7 1.411(4) . ?
C1 H1 0.9300 . ?
C1 C2 1.407(4) . ?
C9 H9 0.9300 . ?
C9 C10 1.364(4) . ?
C10 H10 0.9300 . ?
C10 C11 1.405(4) . ?
C12 H12 0.9800 . ?
C12 C13 1.525(4) . ?
C12 C14 1.522(4) . ?
C28 H28A 0.9600 . ?
C28 H28B 0.9600 . ?
C28 H28C 0.9600 . ?
C28 C26 1.510(4) . ?
C3 H3 0.9300 . ?
C3 C2 1.358(4) . ?
C2 H2 0.9300 . ?
C8 C7 1.379(4) . ?
C26 H26 0.9800 . ?
C26 C27 1.529(4) . ?
C23 H23 0.9300 . ?
C23 C24 1.364(4) . ?
C17 H17 0.9300 . ?
C17 C16 1.366(4) . ?
C22 C21 1.375(4) . ?
C16 H16 0.9300 . ?
C16 C15 1.396(4) . ?
C19 H19 0.9300 . ?
C19 C20 1.407(4) . ?
C19 C18 1.365(4) . ?
C20 C21 1.389(4) . ?
C11 H11 0.9300 . ?
C25 H25 0.9300 . ?
C25 C24 1.404(4) . ?
C21 H21 0.9300 . ?
C13 H13A 0.9600 . ?
C13 H13B 0.9600 . ?
C13 H13C 0.9600 . ?
C24 H24 0.9300 . ?
C5 H5 0.9300 . ?
C5 C4 1.370(4) . ?
C14 H14A 0.9600 . ?
C14 H14B 0.9600 . ?
C14 H14C 0.9600 . ?
C7 H7 0.9300 . ?
C27 H27A 0.9600 . ?
C27 H27B 0.9600 . ?
C27 H27C 0.9600 . ?
C15 H15 0.9300 . ?
N11 C29 1.131(4) . ?
C30 H30A 0.9600 . ?
C30 H30B 0.9600 . ?
C30 H30C 0.9600 . ?
C30 C29 1.452(5) . ?
F1 B1 1.387(4) . ?
F4 B1 1.408(4) . ?
F3 B1 1.407(4) . ?
F2 B1 1.391(4) . ?
F8 B2 1.396(4) . ?
F6 B2 1.404(4) . ?
F7 B2 1.385(4) . ?
F5 B2 1.396(4) . ?

loop_
_geom_angle_atom_site_label_1
_geom_angle_atom_site_label_2
_geom_angle_atom_site_label_3
_geom_angle
_geom_angle_site_symmetry_1
_geom_angle_site_symmetry_3
_geom_angle_publ_flag
N8 Fe1 N1 98.08(9) . . ?
N8 Fe1 N6 73.45(9) . . ?
N8 Fe1 N5 115.24(10) . . ?
N8 Fe1 N10 73.69(9) . . ?
N8 Fe1 N3 168.15(9) . . ?
N6 Fe1 N1 94.93(9) . . ?
N5 Fe1 N1 146.49(10) . . ?
N5 Fe1 N6 97.75(9) . . ?
N10 Fe1 N1 95.81(9) . . ?
N10 Fe1 N6 146.51(9) . . ?
N10 Fe1 N5 90.47(9) . . ?
N3 Fe1 N1 73.26(9) . . ?
N3 Fe1 N6 114.72(9) . . ?
N3 Fe1 N5 73.25(9) . . ?
N3 Fe1 N10 98.74(9) . . ?
C6 S1 C12 105.63(15) . . ?
C20 S2 C26 104.62(14) . . ?
N6 N7 C18 118.5(2) . . ?
C17 N7 N6 111.3(2) . . ?
C17 N7 C18 130.2(3) . . ?
N2 N1 Fe1 113.95(18) . . ?
C1 N1 Fe1 141.3(2) . . ?
C1 N1 N2 104.7(2) . . ?
N1 N2 C4 118.4(2) . . ?
C3 N2 N1 111.1(2) . . ?
C3 N2 C4 130.3(3) . . ?
C22 N8 Fe1 121.1(2) . . ?
C18 N8 Fe1 121.70(19) . . ?
C18 N8 C22 117.2(3) . . ?
N7 N6 Fe1 114.65(17) . . ?
C15 N6 Fe1 140.6(2) . . ?
C15 N6 N7 104.8(2) . . ?
N5 N4 C8 117.5(2) . . ?
C9 N4 N5 111.8(2) . . ?
C9 N4 C8 130.3(3) . . ?
N4 N5 Fe1 115.00(18) . . ?
C11 N5 Fe1 140.5(2) . . ?
C11 N5 N4 104.4(2) . . ?
N10 N9 C22 118.5(2) . . ?
C23 N9 N10 110.8(2) . . ?
C23 N9 C22 130.3(3) . . ?
N9 N10 Fe1 114.21(18) . . ?
C25 N10 Fe1 140.5(2) . . ?
C25 N10 N9 105.3(2) . . ?
C8 N3 Fe1 121.0(2) . . ?
C8 N3 C4 117.2(3) . . ?
C4 N3 Fe1 120.8(2) . . ?
C5 C6 S1 115.5(2) . . ?
C5 C6 C7 119.7(3) . . ?
C7 C6 S1 124.8(2) . . ?
N1 C1 H1 124.3 . . ?
N1 C1 C2 111.5(3) . . ?
C2 C1 H1 124.3 . . ?
N4 C9 H9 126.5 . . ?
N4 C9 C10 106.9(3) . . ?
C10 C9 H9 126.5 . . ?
C9 C10 H10 127.3 . . ?
C9 C10 C11 105.4(3) . . ?
C11 C10 H10 127.3 . . ?
S1 C12 H12 109.4 . . ?
C13 C12 S1 106.1(2) . . ?
C13 C12 H12 109.4 . . ?
C14 C12 S1 110.4(2) . . ?
C14 C12 H12 109.4 . . ?
C14 C12 C13 112.1(3) . . ?
H28A C28 H28B 109.5 . . ?
H28A C28 H28C 109.5 . . ?
H28B C28 H28C 109.5 . . ?
C26 C28 H28A 109.5 . . ?
C26 C28 H28B 109.5 . . ?
C26 C28 H28C 109.5 . . ?
N2 C3 H3 126.5 . . ?
C2 C3 N2 107.0(3) . . ?
C2 C3 H3 126.5 . . ?
C1 C2 H2 127.2 . . ?
C3 C2 C1 105.7(3) . . ?
C3 C2 H2 127.2 . . ?
N3 C8 N4 112.1(3) . . ?
N3 C8 C7 124.3(3) . . ?
C7 C8 N4 123.5(3) . . ?
S2 C26 H26 109.0 . . ?
C28 C26 S2 111.4(2) . . ?
C28 C26 H26 109.0 . . ?
C28 C26 C27 112.3(3) . . ?
C27 C26 S2 106.2(2) . . ?
C27 C26 H26 109.0 . . ?
N9 C23 H23 126.6 . . ?
C24 C23 N9 106.9(3) . . ?
C24 C23 H23 126.6 . . ?
N7 C17 H17 126.6 . . ?
N7 C17 C16 106.9(3) . . ?
C16 C17 H17 126.6 . . ?
N8 C22 N9 112.3(3) . . ?
N8 C22 C21 124.0(3) . . ?
C21 C22 N9 123.7(3) . . ?
C17 C16 H16 127.2 . . ?
C17 C16 C15 105.5(3) . . ?
C15 C16 H16 127.2 . . ?
C20 C19 H19 121.5 . . ?
C18 C19 H19 121.5 . . ?
C18 C19 C20 117.1(3) . . ?
C19 C20 S2 116.0(2) . . ?
C21 C20 S2 124.4(2) . . ?
C21 C20 C19 119.6(3) . . ?
N5 C11 C10 111.5(3) . . ?
N5 C11 H11 124.3 . . ?
C10 C11 H11 124.3 . . ?
N10 C25 H25 124.4 . . ?
N10 C25 C24 111.2(3) . . ?
C24 C25 H25 124.4 . . ?
C22 C21 C20 117.5(3) . . ?
C22 C21 H21 121.2 . . ?
C20 C21 H21 121.2 . . ?
C12 C13 H13A 109.5 . . ?
C12 C13 H13B 109.5 . . ?
C12 C13 H13C 109.5 . . ?
H13A C13 H13B 109.5 . . ?
H13A C13 H13C 109.5 . . ?
H13B C13 H13C 109.5 . . ?
C23 C24 C25 105.9(3) . . ?
C23 C24 H24 127.1 . . ?
C25 C24 H24 127.1 . . ?
C6 C5 H5 121.2 . . ?
C4 C5 C6 117.6(3) . . ?
C4 C5 H5 121.2 . . ?
C12 C14 H14A 109.5 . . ?
C12 C14 H14B 109.5 . . ?
C12 C14 H14C 109.5 . . ?
H14A C14 H14B 109.5 . . ?
H14A C14 H14C 109.5 . . ?
H14B C14 H14C 109.5 . . ?
C6 C7 H7 121.6 . . ?
C8 C7 C6 116.8(3) . . ?
C8 C7 H7 121.6 . . ?
C26 C27 H27A 109.5 . . ?
C26 C27 H27B 109.5 . . ?
C26 C27 H27C 109.5 . . ?
H27A C27 H27B 109.5 . . ?
H27A C27 H27C 109.5 . . ?
H27B C27 H27C 109.5 . . ?
N8 C18 N7 111.6(3) . . ?
N8 C18 C19 124.5(3) . . ?
C19 C18 N7 123.9(3) . . ?
N3 C4 N2 112.6(3) . . ?
N3 C4 C5 124.2(3) . . ?
C5 C4 N2 123.2(3) . . ?
N6 C15 C16 111.5(3) . . ?
N6 C15 H15 124.3 . . ?
C16 C15 H15 124.3 . . ?
H30A C30 H30B 109.5 . . ?
H30A C30 H30C 109.5 . . ?
H30B C30 H30C 109.5 . . ?
C29 C30 H30A 109.5 . . ?
C29 C30 H30B 109.5 . . ?
C29 C30 H30C 109.5 . . ?
N11 C29 C30 178.9(4) . . ?
F1 B1 F4 109.4(3) . . ?
F1 B1 F3 109.6(3) . . ?
F1 B1 F2 110.5(3) . . ?
F3 B1 F4 108.7(3) . . ?
F2 B1 F4 109.5(3) . . ?
F2 B1 F3 109.2(2) . . ?
F8 B2 F6 110.2(3) . . ?
F7 B2 F8 110.1(3) . . ?
F7 B2 F6 109.5(2) . . ?
F7 B2 F5 110.0(3) . . ?
F5 B2 F8 108.7(2) . . ?
F5 B2 F6 108.2(3) . . ?


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

data_164h2olt
_database_code_depnum_ccdc_archive 'CCDC 1563028'
_audit_update_record             
;
2017-07-18 deposited with the CCDC.
2017-11-20 downloaded from the CCDC.
;

_audit_creation_method           SHELXL-97
_chemical_name_systematic        
'Bis[4-(isopropylsulfanyl)-2,6-di(pyrazol-1-yl)pyridine]iron(II)diperchlorate hydrate'
_chemical_name_common            ?
_chemical_melting_point          ?
_chemical_formula_moiety         'C28 H30 Fe N10 S2, 2(Cl O4), H2 O'
_chemical_formula_sum            'C28 H32 Cl2 Fe N10 O9 S2'
_chemical_formula_weight         843.51

loop_
_atom_type_symbol
_atom_type_description
_atom_type_scat_dispersion_real
_atom_type_scat_dispersion_imag
_atom_type_scat_source
Cl Cl 0.3639 0.7018 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
C C 0.0181 0.0091 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Fe Fe -1.1336 3.1974 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
N N 0.0311 0.0180 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
O O 0.0492 0.0322 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
S S 0.3331 0.5567 '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'

_symmetry_cell_setting           monoclinic
_symmetry_space_group_name_H-M   'P 21/c'

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

_cell_length_a                   19.9722(7)
_cell_length_b                   11.9976(6)
_cell_length_c                   15.4592(7)
_cell_angle_alpha                90.00
_cell_angle_beta                 103.466(4)
_cell_angle_gamma                90.00
_cell_volume                     3602.5(3)
_cell_formula_units_Z            4
_cell_measurement_temperature    100(2)
_cell_measurement_reflns_used    5952
_cell_measurement_theta_min      4.55
_cell_measurement_theta_max      72.46

_exptl_crystal_description       'rectangular prism'
_exptl_crystal_colour            brown
_exptl_crystal_size_max          0.20
_exptl_crystal_size_mid          0.15
_exptl_crystal_size_min          0.08
_exptl_crystal_density_meas      ?
_exptl_crystal_density_diffrn    1.555
_exptl_crystal_density_method    'not measured'
_exptl_crystal_F_000             1736
_exptl_absorpt_coefficient_mu    6.376
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_correction_T_min  0.565
_exptl_absorpt_correction_T_max  1.000
_exptl_absorpt_process_details   
; 
CrysAlisPro, Agilent Technologies,
Version 1.171.36.24 (release 03-12-2012 CrysAlis171 .NET)
Empirical absorption correction using spherical harmonics,
 implemented in SCALE3 ABSPACK scaling algorithm.
;

_diffrn_ambient_temperature      100(2)
_diffrn_radiation_wavelength     1.54184
_diffrn_radiation_type           CuK\a
_diffrn_radiation_source         'SuperNova (Cu) X-ray Source'
_diffrn_radiation_monochromator  mirror
_diffrn_measurement_device_type  'SuperNova, Dual, Cu at zero, Atlas'
_diffrn_measurement_method       'ω scans'
_diffrn_detector_area_resol_mean 5.3095
_diffrn_standards_number         0
_diffrn_standards_interval_count 0
_diffrn_standards_interval_time  0
_diffrn_standards_decay_%        0
_diffrn_reflns_number            15650
_diffrn_reflns_av_R_equivalents  0.0425
_diffrn_reflns_av_sigmaI/netI    0.0383
_diffrn_reflns_limit_h_min       -23
_diffrn_reflns_limit_h_max       18
_diffrn_reflns_limit_k_min       -14
_diffrn_reflns_limit_k_max       11
_diffrn_reflns_limit_l_min       -18
_diffrn_reflns_limit_l_max       18
_diffrn_reflns_theta_min         4.33
_diffrn_reflns_theta_max         67.08
_reflns_number_total             6385
_reflns_number_gt                5457
_reflns_threshold_expression     >2sigma(I)

_computing_data_collection       'CrysAlisPro, Agilent Technologies'
_computing_cell_refinement       'CrysAlisPro, Agilent Technologies'
_computing_data_reduction        'CrysAlisPro, Agilent Technologies'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_molecular_graphics    'XSEED (Barbour, 2001)'
_computing_publication_material  'local program'

_refine_special_details          
; 
 Refinement of F² against ALL reflections.  The weighted R-factor wR and 
 goodness of fit S are based on F², conventional R-factors R are based 
 on F, with F set to zero for negative F². The threshold expression of 
 F² > 2sigma(F²) is used only for calculating R-factors(gt) etc. and is 
 not relevant to the choice of reflections for refinement.  R-factors based 
 on F² are statistically about twice as large as those based on F, and R- 
 factors based on ALL data will be even larger. 

 The ClO₄⁻ ion Cl42-O46 is disordered over two sites with refined 
 occupancies of 0.75:0.25, which were modelled using the refined restraints 
 Cl---O = 1.43(2) and O...O = 2.34(2) Å. The water molecule is also 
 distributed over two sites with a 0.75:0.25 occupancy ratio, which appears 
 to mirror the anion disorder. All wholly occupied non-H atoms, plus the 
 0.75-occupied Cl atom Cl42A, were refined anisotropically, and C-bound H 
 atoms were placed in calculated positions and refined using a riding model.
 The disordered water H atoms were not located in the Fourier map and are 
 not included in the refinement, but are accounted for in the density and 
 F(000) calculations.

 The water molecule is positioned to hydrogen bond to the disordered anion
 Cl42-O46, and the symmetry equivalent of the same anion related by 
 1-x, 1-y, 1-z.
;

_refine_ls_structure_factor_coef Fsqd
_refine_ls_matrix_type           full
_refine_ls_weighting_scheme      calc
_refine_ls_weighting_details     
'calc w=1/[σ²(Fo²)+(0.1222P)²+0.5758P] 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         6385
_refine_ls_number_parameters     474
_refine_ls_number_restraints     20
_refine_ls_R_factor_all          0.0693
_refine_ls_R_factor_gt           0.0614
_refine_ls_wR_factor_ref         0.1707
_refine_ls_wR_factor_gt          0.1596
_refine_ls_goodness_of_fit_ref   1.031
_refine_ls_restrained_S_all      1.031
_refine_ls_shift/su_max          0.001
_refine_ls_shift/su_mean         0.000

loop_
_atom_site_label
_atom_site_type_symbol
_atom_site_fract_x
_atom_site_fract_y
_atom_site_fract_z
_atom_site_U_iso_or_equiv
_atom_site_adp_type
_atom_site_occupancy
_atom_site_symmetry_multiplicity
_atom_site_calc_flag
_atom_site_refinement_flags
_atom_site_disorder_assembly
_atom_site_disorder_group
Fe1 Fe 0.23225(2) 0.61365(4) 0.08462(3) 0.04313(18) Uani 1 1 d . . .
N2 N 0.13476(14) 0.6344(2) 0.05103(19) 0.0454(6) Uani 1 1 d . . .
C3 C 0.10665(16) 0.7115(3) -0.0079(2) 0.0444(7) Uani 1 1 d . . .
C4 C 0.03760(17) 0.7381(3) -0.0280(2) 0.0463(7) Uani 1 1 d . . .
H4 H 0.0190 0.7929 -0.0713 0.056 Uiso 1 1 calc R . .
C5 C -0.00366(17) 0.6799(3) 0.0185(2) 0.0476(7) Uani 1 1 d . . .
C6 C 0.02560(17) 0.5993(3) 0.0821(2) 0.0479(7) Uani 1 1 d . . .
H6 H -0.0016 0.5598 0.1147 0.058 Uiso 1 1 calc R . .
C7 C 0.09466(17) 0.5798(3) 0.0953(2) 0.0469(7) Uani 1 1 d . . .
N8 N 0.15743(14) 0.7632(2) -0.04338(19) 0.0459(6) Uani 1 1 d . . .
N9 N 0.22503(14) 0.7334(2) -0.00572(19) 0.0462(6) Uani 1 1 d . . .
C10 C 0.26304(18) 0.7997(3) -0.0429(3) 0.0520(8) Uani 1 1 d . . .
H10 H 0.3119 0.7982 -0.0303 0.062 Uiso 1 1 calc R . .
C11 C 0.2216(2) 0.8725(3) -0.1034(3) 0.0558(9) Uani 1 1 d . . .
H11 H 0.2368 0.9283 -0.1381 0.067 Uiso 1 1 calc R . .
C12 C 0.15485(18) 0.8471(3) -0.1025(2) 0.0513(8) Uani 1 1 d . . .
H12 H 0.1146 0.8818 -0.1367 0.062 Uiso 1 1 calc R . .
N13 N 0.13353(14) 0.5057(3) 0.1575(2) 0.0478(6) Uani 1 1 d . . .
N14 N 0.20344(14) 0.5032(2) 0.1641(2) 0.0478(6) Uani 1 1 d . . .
C15 C 0.22755(19) 0.4270(3) 0.2255(3) 0.0532(8) Uani 1 1 d . . .
H15 H 0.2747 0.4074 0.2452 0.064 Uiso 1 1 calc R . .
C16 C 0.1737(2) 0.3790(3) 0.2576(3) 0.0578(9) Uani 1 1 d . . .
H16 H 0.1776 0.3224 0.3015 0.069 Uiso 1 1 calc R . .
C17 C 0.11476(19) 0.4306(3) 0.2128(3) 0.0538(8) Uani 1 1 d . . .
H17 H 0.0694 0.4165 0.2192 0.065 Uiso 1 1 calc R . .
S18 S -0.09265(4) 0.69758(8) 0.00484(7) 0.0535(2) Uani 1 1 d . . .
C19 C -0.11412(17) 0.8276(3) -0.0569(3) 0.0503(8) Uani 1 1 d . . .
H19 H -0.0956 0.8259 -0.1116 0.060 Uiso 1 1 calc R . .
C20 C -0.08467(19) 0.9277(3) 0.0002(3) 0.0551(8) Uani 1 1 d . . .
H20A H -0.0965 0.9962 -0.0345 0.083 Uiso 1 1 calc R . .
H20B H -0.0345 0.9207 0.0189 0.083 Uiso 1 1 calc R . .
H20C H -0.1041 0.9306 0.0528 0.083 Uiso 1 1 calc R . .
C21 C -0.19259(19) 0.8313(4) -0.0831(3) 0.0628(10) Uani 1 1 d . . .
H21A H -0.2106 0.8333 -0.0293 0.094 Uiso 1 1 calc R . .
H21B H -0.2100 0.7649 -0.1180 0.094 Uiso 1 1 calc R . .
H21C H -0.2075 0.8982 -0.1187 0.094 Uiso 1 1 calc R . .
N22 N 0.32885(14) 0.5914(2) 0.1274(2) 0.0461(6) Uani 1 1 d . . .
C23 C 0.36144(18) 0.5134(3) 0.0907(2) 0.0482(7) Uani 1 1 d . . .
C24 C 0.42908(19) 0.4871(3) 0.1232(3) 0.0543(8) Uani 1 1 d . . .
H24 H 0.4511 0.4323 0.0953 0.065 Uiso 1 1 calc R . .
C25 C 0.46489(17) 0.5436(3) 0.1992(3) 0.0529(8) Uani 1 1 d . . .
C26 C 0.43199(18) 0.6260(3) 0.2383(3) 0.0516(8) Uani 1 1 d . . .
H26 H 0.4554 0.6662 0.2894 0.062 Uiso 1 1 calc R . .
C27 C 0.36393(17) 0.6456(3) 0.1988(2) 0.0471(7) Uani 1 1 d . . .
N28 N 0.31637(14) 0.4644(3) 0.0167(2) 0.0486(6) Uani 1 1 d . . .
N29 N 0.24840(14) 0.4980(2) -0.0004(2) 0.0466(6) Uani 1 1 d . . .
C30 C 0.21758(18) 0.4446(3) -0.0736(2) 0.0505(8) Uani 1 1 d . . .
H30 H 0.1702 0.4517 -0.1019 0.061 Uiso 1 1 calc R . .
C31 C 0.2642(2) 0.3759(3) -0.1040(3) 0.0543(8) Uani 1 1 d . . .
H31 H 0.2547 0.3288 -0.1548 0.065 Uiso 1 1 calc R . .
C32 C 0.3263(2) 0.3911(3) -0.0452(3) 0.0550(8) Uani 1 1 d . . .
H32 H 0.3685 0.3563 -0.0475 0.066 Uiso 1 1 calc R . .
N33 N 0.32032(14) 0.7230(3) 0.22754(19) 0.0468(6) Uani 1 1 d . . .
N34 N 0.25255(14) 0.7247(3) 0.18063(19) 0.0469(6) Uani 1 1 d . . .
C35 C 0.22383(19) 0.8085(3) 0.2144(3) 0.0512(8) Uani 1 1 d . . .
H35 H 0.1770 0.8303 0.1949 0.061 Uiso 1 1 calc R . .
C36 C 0.2725(2) 0.8610(3) 0.2832(3) 0.0553(8) Uani 1 1 d . . .
H36 H 0.2648 0.9231 0.3178 0.066 Uiso 1 1 calc R . .
C37 C 0.33276(18) 0.8044(3) 0.2901(2) 0.0502(8) Uani 1 1 d . . .
H37 H 0.3753 0.8192 0.3309 0.060 Uiso 1 1 calc R . .
S38 S 0.54980(5) 0.50014(9) 0.23944(8) 0.0633(3) Uani 1 1 d . . .
C39 C 0.58377(18) 0.5823(4) 0.3394(3) 0.0599(9) Uani 1 1 d . . .
H39 H 0.5473 0.5906 0.3736 0.072 Uiso 1 1 calc R . .
C40 C 0.6060(2) 0.6968(4) 0.3158(3) 0.0676(10) Uani 1 1 d . . .
H40A H 0.6206 0.7413 0.3701 0.101 Uiso 1 1 calc R . .
H40B H 0.5673 0.7338 0.2753 0.101 Uiso 1 1 calc R . .
H40C H 0.6445 0.6894 0.2868 0.101 Uiso 1 1 calc R . .
C41 C 0.6434(2) 0.5141(4) 0.3944(3) 0.0656(10) Uani 1 1 d . . .
H41A H 0.6803 0.5090 0.3624 0.098 Uiso 1 1 calc R . .
H41B H 0.6271 0.4391 0.4040 0.098 Uiso 1 1 calc R . .
H41C H 0.6609 0.5506 0.4519 0.098 Uiso 1 1 calc R . .
Cl42A Cl 0.47842(12) 0.7265(3) 0.50976(17) 0.0519(5) Uani 0.75 1 d PD A 1
O43A O 0.5372(2) 0.7494(4) 0.5809(3) 0.0727(10) Uiso 0.75 1 d PD A 1
O44A O 0.4903(2) 0.7776(4) 0.4301(3) 0.0692(10) Uiso 0.75 1 d PD A 1
O45A O 0.4178(3) 0.7696(4) 0.5294(3) 0.0789(12) Uiso 0.75 1 d PD A 1
O46A O 0.4722(3) 0.6095(4) 0.4933(3) 0.0822(12) Uiso 0.75 1 d PD A 1
Cl42B Cl 0.4707(5) 0.7484(8) 0.5009(6) 0.064(3) Uiso 0.25 1 d PD C 2
O43B O 0.5431(6) 0.7305(13) 0.5293(10) 0.089(4) Uiso 0.25 1 d PD C 2
O44B O 0.4407(6) 0.6585(10) 0.4425(7) 0.071(3) Uiso 0.25 1 d PD C 2
O45B O 0.4388(6) 0.7358(9) 0.5762(7) 0.059(2) Uiso 0.25 1 d PD C 2
O46B O 0.4539(6) 0.8520(9) 0.4630(8) 0.068(3) Uiso 0.25 1 d PD C 2
Cl47 Cl 0.06438(4) 0.97207(8) 0.22789(5) 0.0517(2) Uani 1 1 d . . .
O48 O 0.12896(13) 1.0269(3) 0.23288(19) 0.0616(7) Uani 1 1 d . . .
O49 O 0.00841(13) 1.0485(3) 0.19488(19) 0.0608(7) Uani 1 1 d . . .
O50 O 0.06151(14) 0.9350(3) 0.31581(19) 0.0602(6) Uani 1 1 d . . .
O51 O 0.05878(15) 0.8782(3) 0.1697(2) 0.0654(7) Uani 1 1 d . . .
O52A O 0.6290(3) 0.5470(6) 0.6227(4) 0.0840(19) Uiso 0.75 1 d P B 1
O52B O 0.6233(10) 0.5740(18) 0.6387(13) 0.080(5) Uiso 0.25 1 d P D 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 N22 1.907(3) . ?
Fe1 N2 1.911(3) . ?
Fe1 N34 1.965(3) . ?
Fe1 N14 1.982(3) . ?
Fe1 N9 1.985(3) . ?
Fe1 N29 1.988(3) . ?
N2 C3 1.327(5) . ?
N2 C7 1.340(5) . ?
C3 C4 1.379(5) . ?
C3 N8 1.405(4) . ?
C4 C5 1.400(5) . ?
C4 H4 0.9500 . ?
C5 C6 1.405(5) . ?
C5 S18 1.753(3) . ?
C6 C7 1.367(5) . ?
C6 H6 0.9500 . ?
C7 N13 1.404(5) . ?
N8 C12 1.352(5) . ?
N8 N9 1.387(4) . ?
N9 C10 1.319(5) . ?
C10 C11 1.401(6) . ?
C10 H10 0.9500 . ?
C11 C12 1.372(5) . ?
C11 H11 0.9500 . ?
C12 H12 0.9500 . ?
N13 C17 1.354(5) . ?
N13 N14 1.376(4) . ?
N14 C15 1.324(5) . ?
C15 C16 1.408(6) . ?
C15 H15 0.9500 . ?
C16 C17 1.368(6) . ?
C16 H16 0.9500 . ?
C17 H17 0.9500 . ?
S18 C19 1.826(4) . ?
C19 C20 1.525(5) . ?
C19 C21 1.525(5) . ?
C19 H19 1.0000 . ?
C20 H20A 0.9800 . ?
C20 H20B 0.9800 . ?
C20 H20C 0.9800 . ?
C21 H21A 0.9800 . ?
C21 H21B 0.9800 . ?
C21 H21C 0.9800 . ?
N22 C27 1.331(5) . ?
N22 C23 1.339(5) . ?
C23 C24 1.364(5) . ?
C23 N28 1.409(5) . ?
C24 C25 1.401(6) . ?
C24 H24 0.9500 . ?
C25 C26 1.399(5) . ?
C25 S38 1.745(3) . ?
C26 C27 1.375(5) . ?
C26 H26 0.9500 . ?
C27 N33 1.414(5) . ?
N28 C32 1.348(5) . ?
N28 N29 1.381(4) . ?
N29 C30 1.321(5) . ?
C30 C31 1.404(6) . ?
C30 H30 0.9500 . ?
C31 C32 1.368(6) . ?
C31 H31 0.9500 . ?
C32 H32 0.9500 . ?
N33 C37 1.356(5) . ?
N33 N34 1.379(4) . ?
N34 C35 1.323(5) . ?
C35 C36 1.412(6) . ?
C35 H35 0.9500 . ?
C36 C37 1.365(5) . ?
C36 H36 0.9500 . ?
C37 H37 0.9500 . ?
S38 C39 1.825(4) . ?
C39 C40 1.514(7) . ?
C39 C41 1.529(6) . ?
C39 H39 1.0000 . ?
C40 H40A 0.9800 . ?
C40 H40B 0.9800 . ?
C40 H40C 0.9800 . ?
C41 H41A 0.9800 . ?
C41 H41B 0.9800 . ?
C41 H41C 0.9800 . ?
Cl42A O45A 1.414(5) . ?
Cl42A O46A 1.427(6) . ?
Cl42A O43A 1.436(5) . ?
Cl42A O44A 1.443(5) . ?
Cl42B O44B 1.444(13) . ?
Cl42B O46B 1.382(12) . ?
Cl42B O45B 1.459(12) . ?
Cl42B O43B 1.425(13) . ?
Cl47 O51 1.430(3) . ?
Cl47 O48 1.434(3) . ?
Cl47 O50 1.444(3) . ?
Cl47 O49 1.444(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
N22 Fe1 N2 175.54(12) . . ?
N22 Fe1 N34 79.55(12) . . ?
N2 Fe1 N34 97.75(12) . . ?
N22 Fe1 N14 96.17(12) . . ?
N2 Fe1 N14 80.28(12) . . ?
N34 Fe1 N14 91.35(12) . . ?
N22 Fe1 N9 104.32(12) . . ?
N2 Fe1 N9 79.17(12) . . ?
N34 Fe1 N9 90.53(13) . . ?
N14 Fe1 N9 159.43(11) . . ?
N22 Fe1 N29 79.91(12) . . ?
N2 Fe1 N29 102.90(12) . . ?
N34 Fe1 N29 159.31(12) . . ?
N14 Fe1 N29 93.34(13) . . ?
N9 Fe1 N29 92.10(12) . . ?
C3 N2 C7 118.9(3) . . ?
C3 N2 Fe1 121.2(2) . . ?
C7 N2 Fe1 119.3(2) . . ?
N2 C3 C4 123.8(3) . . ?
N2 C3 N8 110.3(3) . . ?
C4 C3 N8 125.8(3) . . ?
C3 C4 C5 116.5(3) . . ?
C3 C4 H4 121.7 . . ?
C5 C4 H4 121.7 . . ?
C4 C5 C6 120.2(3) . . ?
C4 C5 S18 125.4(3) . . ?
C6 C5 S18 114.4(3) . . ?
C7 C6 C5 117.6(3) . . ?
C7 C6 H6 121.2 . . ?
C5 C6 H6 121.2 . . ?
N2 C7 C6 122.9(3) . . ?
N2 C7 N13 111.0(3) . . ?
C6 C7 N13 126.1(3) . . ?
C12 N8 N9 110.9(3) . . ?
C12 N8 C3 132.5(3) . . ?
N9 N8 C3 116.3(3) . . ?
C10 N9 N8 105.3(3) . . ?
C10 N9 Fe1 141.9(3) . . ?
N8 N9 Fe1 112.7(2) . . ?
N9 C10 C11 110.9(3) . . ?
N9 C10 H10 124.6 . . ?
C11 C10 H10 124.6 . . ?
C12 C11 C10 106.2(3) . . ?
C12 C11 H11 126.9 . . ?
C10 C11 H11 126.9 . . ?
N8 C12 C11 106.7(3) . . ?
N8 C12 H12 126.6 . . ?
C11 C12 H12 126.6 . . ?
C17 N13 N14 111.3(3) . . ?
C17 N13 C7 131.6(3) . . ?
N14 N13 C7 117.1(3) . . ?
C15 N14 N13 105.2(3) . . ?
C15 N14 Fe1 142.7(3) . . ?
N13 N14 Fe1 112.0(2) . . ?
N14 C15 C16 110.8(3) . . ?
N14 C15 H15 124.6 . . ?
C16 C15 H15 124.6 . . ?
C17 C16 C15 105.9(3) . . ?
C17 C16 H16 127.0 . . ?
C15 C16 H16 127.0 . . ?
N13 C17 C16 106.8(3) . . ?
N13 C17 H17 126.6 . . ?
C16 C17 H17 126.6 . . ?
C5 S18 C19 105.93(17) . . ?
C20 C19 C21 111.4(3) . . ?
C20 C19 S18 111.0(3) . . ?
C21 C19 S18 105.4(3) . . ?
C20 C19 H19 109.7 . . ?
C21 C19 H19 109.7 . . ?
S18 C19 H19 109.7 . . ?
C19 C20 H20A 109.5 . . ?
C19 C20 H20B 109.5 . . ?
H20A C20 H20B 109.5 . . ?
C19 C20 H20C 109.5 . . ?
H20A C20 H20C 109.5 . . ?
H20B C20 H20C 109.5 . . ?
C19 C21 H21A 109.5 . . ?
C19 C21 H21B 109.5 . . ?
H21A C21 H21B 109.5 . . ?
C19 C21 H21C 109.5 . . ?
H21A C21 H21C 109.5 . . ?
H21B C21 H21C 109.5 . . ?
C27 N22 C23 118.6(3) . . ?
C27 N22 Fe1 120.9(2) . . ?
C23 N22 Fe1 120.2(2) . . ?
N22 C23 C24 122.9(3) . . ?
N22 C23 N28 110.7(3) . . ?
C24 C23 N28 126.4(3) . . ?
C23 C24 C25 117.7(3) . . ?
C23 C24 H24 121.1 . . ?
C25 C24 H24 121.1 . . ?
C26 C25 C24 120.3(3) . . ?
C26 C25 S38 124.9(3) . . ?
C24 C25 S38 114.7(3) . . ?
C27 C26 C25 116.4(3) . . ?
C27 C26 H26 121.8 . . ?
C25 C26 H26 121.8 . . ?
N22 C27 C26 124.1(3) . . ?
N22 C27 N33 109.7(3) . . ?
C26 C27 N33 126.2(3) . . ?
C32 N28 N29 110.7(3) . . ?
C32 N28 C23 132.6(3) . . ?
N29 N28 C23 116.6(3) . . ?
C30 N29 N28 105.3(3) . . ?
C30 N29 Fe1 142.1(3) . . ?
N28 N29 Fe1 112.4(2) . . ?
N29 C30 C31 111.0(3) . . ?
N29 C30 H30 124.5 . . ?
C31 C30 H30 124.5 . . ?
C32 C31 C30 105.6(3) . . ?
C32 C31 H31 127.2 . . ?
C30 C31 H31 127.2 . . ?
N28 C32 C31 107.4(3) . . ?
N28 C32 H32 126.3 . . ?
C31 C32 H32 126.3 . . ?
C37 N33 N34 111.0(3) . . ?
C37 N33 C27 132.3(3) . . ?
N34 N33 C27 116.5(3) . . ?
C35 N34 N33 105.4(3) . . ?
C35 N34 Fe1 141.3(3) . . ?
N33 N34 Fe1 113.1(2) . . ?
N34 C35 C36 110.6(3) . . ?
N34 C35 H35 124.7 . . ?
C36 C35 H35 124.7 . . ?
C37 C36 C35 106.0(3) . . ?
C37 C36 H36 127.0 . . ?
C35 C36 H36 127.0 . . ?
N33 C37 C36 106.9(3) . . ?
N33 C37 H37 126.5 . . ?
C36 C37 H37 126.5 . . ?
C25 S38 C39 106.18(18) . . ?
C40 C39 C41 112.7(3) . . ?
C40 C39 S38 111.0(3) . . ?
C41 C39 S38 105.6(3) . . ?
C40 C39 H39 109.1 . . ?
C41 C39 H39 109.1 . . ?
S38 C39 H39 109.1 . . ?
C39 C40 H40A 109.5 . . ?
C39 C40 H40B 109.5 . . ?
H40A C40 H40B 109.5 . . ?
C39 C40 H40C 109.5 . . ?
H40A C40 H40C 109.5 . . ?
H40B C40 H40C 109.5 . . ?
C39 C41 H41A 109.5 . . ?
C39 C41 H41B 109.5 . . ?
H41A C41 H41B 109.5 . . ?
C39 C41 H41C 109.5 . . ?
H41A C41 H41C 109.5 . . ?
H41B C41 H41C 109.5 . . ?
O45A Cl42A O46A 110.7(3) . . ?
O45A Cl42A O43A 110.8(3) . . ?
O46A Cl42A O43A 110.3(4) . . ?
O45A Cl42A O44A 110.3(3) . . ?
O46A Cl42A O44A 106.9(3) . . ?
O43A Cl42A O44A 107.8(3) . . ?
O46B Cl42B O43B 113.3(10) . . ?
O46B Cl42B O44B 112.5(9) . . ?
O43B Cl42B O44B 108.9(9) . . ?
O46B Cl42B O45B 108.8(9) . . ?
O43B Cl42B O45B 109.8(9) . . ?
O44B Cl42B O45B 103.1(9) . . ?
O51 Cl47 O48 109.43(18) . . ?
O51 Cl47 O50 109.60(19) . . ?
O48 Cl47 O50 108.85(17) . . ?
O51 Cl47 O49 109.71(17) . . ?
O48 Cl47 O49 109.88(18) . . ?
O50 Cl47 O49 109.35(16) . . ?

_diffrn_measured_fraction_theta_max 0.992
_diffrn_reflns_theta_full        67.08
_diffrn_measured_fraction_theta_full 0.992
_refine_diff_density_max         0.761
_refine_diff_density_min         -0.683
_refine_diff_density_rms         0.101
_exptl_crystal_recrystallization_method 
'SC-SC atmospheric moisture replacement of acetone solvate'
_exptl_crystal_preparation       'Magnetic properties'
####################################################################### 
# 
# This file contains crystal structure data downloaded from the 
# Cambridge Structural Database (CSD) hosted by the Cambridge 
# Crystallographic Data Centre (CCDC).
# 
# Full information about CCDC data access policies and citation 
# guidelines are available at http://www.ccdc.cam.ac.uk/access/V1 
# 
# Audit and citation data items may have been added by the CCDC. 
# Please retain this information to preserve the provenance of 
# this file and to allow appropriate attribution of the data. 
# 
#######################################################################

data_164no2lt_CCDC1
_database_code_depnum_ccdc_archive 'CCDC 1563026'
_audit_update_record             
;
2017-07-18 deposited with the CCDC.
2017-11-20 downloaded from the CCDC.
;

_audit_creation_method           SHELXL-97
_chemical_name_systematic        
'Bis[4-(isopropylsulfanyl)-2,6-di(pyrazol-1-yl)pyridine]iron(II)diperchlorate nitromethane solvate'
_chemical_name_common            ?
_chemical_melting_point          ?
_chemical_formula_moiety         'C28 H30 Fe N10 S2, 2(Cl O4), C H3 N O2'
_chemical_formula_sum            'C29 H33 Cl2 Fe N11 O10 S2'
_chemical_formula_weight         886.53

loop_
_atom_type_symbol
_atom_type_description
_atom_type_scat_dispersion_real
_atom_type_scat_dispersion_imag
_atom_type_scat_source
Cl Cl 0.3639 0.7018 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
C C 0.0181 0.0091 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
O O 0.0492 0.0322 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Fe Fe -1.1336 3.1974 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
N N 0.0311 0.0180 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
S S 0.3331 0.5567 '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'

_symmetry_cell_setting           monoclinic
_symmetry_space_group_name_H-M   'P 21/c'

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

_cell_length_a                   20.3076(10)
_cell_length_b                   11.8848(6)
_cell_length_c                   15.9663(8)
_cell_angle_alpha                90.00
_cell_angle_beta                 102.134(4)
_cell_angle_gamma                90.00
_cell_volume                     3767.4(3)
_cell_formula_units_Z            4
_cell_measurement_temperature    100(2)
_cell_measurement_reflns_used    6377
_cell_measurement_theta_min      4.33
_cell_measurement_theta_max      73.72

_exptl_crystal_description       'rectangular prism'
_exptl_crystal_colour            brown
_exptl_crystal_size_max          0.19
_exptl_crystal_size_mid          0.14
_exptl_crystal_size_min          0.09
_exptl_crystal_density_meas      ?
_exptl_crystal_density_diffrn    1.563
_exptl_crystal_density_method    'not measured'
_exptl_crystal_F_000             1824
_exptl_absorpt_coefficient_mu    6.157
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_correction_T_min  0.578
_exptl_absorpt_correction_T_max  1.000
_exptl_absorpt_process_details   
; 
CrysAlisPro, Agilent Technologies,
Version 1.171.36.24 (release 03-12-2012 CrysAlis171 .NET)
Empirical absorption correction using spherical harmonics,
 implemented in SCALE3 ABSPACK scaling algorithm.
;

_diffrn_ambient_temperature      100(2)
_diffrn_radiation_wavelength     1.54184
_diffrn_radiation_type           CuK\a
_diffrn_radiation_source         'SuperNova (Cu) X-ray Source'
_diffrn_radiation_monochromator  mirror
_diffrn_measurement_device_type  'SuperNova, Dual, Cu at zero, Atlas'
_diffrn_measurement_method       'ω scans'
_diffrn_detector_area_resol_mean 5.3095
_diffrn_standards_number         0
_diffrn_standards_interval_count 0
_diffrn_standards_interval_time  0
_diffrn_standards_decay_%        0
_diffrn_reflns_number            14338
_diffrn_reflns_av_R_equivalents  0.0483
_diffrn_reflns_av_sigmaI/netI    0.0574
_diffrn_reflns_limit_h_min       -16
_diffrn_reflns_limit_h_max       25
_diffrn_reflns_limit_k_min       -13
_diffrn_reflns_limit_k_max       14
_diffrn_reflns_limit_l_min       -18
_diffrn_reflns_limit_l_max       19
_diffrn_reflns_theta_min         4.34
_diffrn_reflns_theta_max         73.86
_reflns_number_total             7390
_reflns_number_gt                6125
_reflns_threshold_expression     >2sigma(I)

_computing_data_collection       'CrysAlisPro, Agilent Technologies'
_computing_cell_refinement       'CrysAlisPro, Agilent Technologies'
_computing_data_reduction        'CrysAlisPro, Agilent Technologies'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_molecular_graphics    'XSEED (Barbour, 2001)'
_computing_publication_material  'local program'

_refine_special_details          
; 
 Refinement of F² against ALL reflections.  The weighted R-factor wR and 
 goodness of fit S are based on F², conventional R-factors R are based 
 on F, with F set to zero for negative F². The threshold expression of 
 F² > 2sigma(F²) is used only for calculating R-factors(gt) etc. and is 
 not relevant to the choice of reflections for refinement.  R-factors based 
 on F² are statistically about twice as large as those based on F, and R- 
 factors based on ALL data will be even larger. 

 The nitromethane was disordered, and modelled over three sites with 
 occupancies of 0.40, 0.40 and 0.20; two of these sites shared a common, 0.6-
 occupied N atom. The fixed restraints C---N = 1.45(2), N---O = 1.22(2), 
 O...O = 2.09(2) and C...O = 2.32(2) Å were applied to those residues. All 
 wholly occupied non-H atoms, plus the two half-occupied Cl atoms, were 
 refined anisotropically, and H atoms were placed in calculated positions 
 and refined using a riding model.
;

_refine_ls_structure_factor_coef Fsqd
_refine_ls_matrix_type           full
_refine_ls_weighting_scheme      calc
_refine_ls_weighting_details     
'calc w=1/[σ²(Fo²)+(0.0602P)²+13.0694P] 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         7390
_refine_ls_number_parameters     508
_refine_ls_number_restraints     18
_refine_ls_R_factor_all          0.0817
_refine_ls_R_factor_gt           0.0696
_refine_ls_wR_factor_ref         0.1692
_refine_ls_wR_factor_gt          0.1608
_refine_ls_goodness_of_fit_ref   1.031
_refine_ls_restrained_S_all      1.032
_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_symmetry_multiplicity
_atom_site_calc_flag
_atom_site_refinement_flags
_atom_site_disorder_assembly
_atom_site_disorder_group
Fe1 Fe 0.22345(3) 0.60491(6) 0.06838(4) 0.02414(17) Uani 1 1 d . A .
N2 N 0.12112(19) 0.6291(3) 0.0420(2) 0.0248(7) Uani 1 1 d . A .
C3 C 0.0931(2) 0.7067(4) -0.0150(3) 0.0247(8) Uani 1 1 d . . .
C4 C 0.0260(2) 0.7365(4) -0.0288(3) 0.0261(9) Uani 1 1 d . A 2
H4 H 0.0074 0.7912 -0.0705 0.031 Uiso 1 1 calc R . .
C5 C -0.0135(2) 0.6828(4) 0.0211(3) 0.0299(10) Uani 1 1 d . . .
C6 C 0.0155(2) 0.6009(4) 0.0816(3) 0.0284(9) Uani 1 1 d . A .
H6 H -0.0105 0.5628 0.1158 0.034 Uiso 1 1 calc R . .
C7 C 0.0827(2) 0.5785(4) 0.0889(3) 0.0268(9) Uani 1 1 d . . .
N8 N 0.1399(2) 0.7559(3) -0.0566(2) 0.0282(8) Uani 1 1 d . A .
N9 N 0.2071(2) 0.7300(3) -0.0265(2) 0.0300(8) Uani 1 1 d . . .
C10 C 0.2399(3) 0.7926(4) -0.0728(3) 0.0404(12) Uani 1 1 d . A .
H10 H 0.2875 0.7930 -0.0667 0.049 Uiso 1 1 calc R . .
C11 C 0.1951(3) 0.8585(5) -0.1321(4) 0.0501(15) Uani 1 1 d . . .
H11 H 0.2063 0.9102 -0.1722 0.060 Uiso 1 1 calc R A .
C12 C 0.1325(3) 0.8331(4) -0.1204(3) 0.0397(12) Uani 1 1 d . A .
H12 H 0.0913 0.8637 -0.1512 0.048 Uiso 1 1 calc R . .
N13 N 0.1191(2) 0.5000(3) 0.1467(2) 0.0330(9) Uani 1 1 d . A .
N14 N 0.1868(2) 0.4911(3) 0.1513(2) 0.0343(9) Uani 1 1 d . . .
C15 C 0.2063(4) 0.4075(5) 0.2070(3) 0.0518(17) Uani 1 1 d . A .
H15 H 0.2515 0.3819 0.2240 0.062 Uiso 1 1 calc R . .
C16 C 0.1525(4) 0.3625(5) 0.2369(3) 0.0548(17) Uani 1 1 d . . .
H16 H 0.1538 0.3023 0.2764 0.066 Uiso 1 1 calc R A .
C17 C 0.0970(3) 0.4230(4) 0.1977(3) 0.0458(14) Uani 1 1 d . A .
H17 H 0.0520 0.4131 0.2047 0.055 Uiso 1 1 calc R . .
S18 S -0.09936(6) 0.70479(10) 0.01431(8) 0.0343(3) Uani 1 1 d . A .
C19 C -0.1186(2) 0.8367(4) -0.0442(3) 0.0323(10) Uani 1 1 d . . .
H19 H -0.1026 0.8328 -0.0992 0.039 Uiso 1 1 calc R A .
C20 C -0.0857(3) 0.9360(4) 0.0083(3) 0.0374(11) Uani 1 1 d . A .
H20A H -0.0951 1.0050 -0.0257 0.056 Uiso 1 1 calc R . .
H20B H -0.0369 0.9241 0.0242 0.056 Uiso 1 1 calc R . .
H20C H -0.1039 0.9430 0.0603 0.056 Uiso 1 1 calc R . .
C21 C -0.1953(2) 0.8469(5) -0.0630(4) 0.0438(13) Uani 1 1 d . A .
H21A H -0.2109 0.8491 -0.0090 0.066 Uiso 1 1 calc R . .
H21B H -0.2153 0.7820 -0.0969 0.066 Uiso 1 1 calc R . .
H21C H -0.2089 0.9162 -0.0953 0.066 Uiso 1 1 calc R . .
N22 N 0.32388(18) 0.5782(3) 0.1152(2) 0.0277(8) Uani 1 1 d . . .
C23 C 0.3570(2) 0.4962(4) 0.0833(3) 0.0272(9) Uani 1 1 d . A .
C24 C 0.4217(2) 0.4670(4) 0.1180(3) 0.0307(10) Uani 1 1 d . . .
H24 H 0.4435 0.4079 0.0942 0.037 Uiso 1 1 calc R A .
C25 C 0.4555(2) 0.5272(4) 0.1904(3) 0.0309(10) Uani 1 1 d . A .
C26 C 0.4223(2) 0.6146(4) 0.2228(3) 0.0306(10) Uani 1 1 d . . .
H26 H 0.4443 0.6579 0.2706 0.037 Uiso 1 1 calc R A .
C27 C 0.3564(2) 0.6358(4) 0.1827(3) 0.0257(9) Uani 1 1 d . A .
N28 N 0.3161(2) 0.4470(4) 0.0100(2) 0.0339(9) Uani 1 1 d . . .
N29 N 0.2505(2) 0.4822(4) -0.0126(2) 0.0384(10) Uani 1 1 d . A .
C30 C 0.2270(4) 0.4285(6) -0.0865(3) 0.062(2) Uani 1 1 d . . .
H30 H 0.1822 0.4354 -0.1185 0.074 Uiso 1 1 calc R A .
C31 C 0.2757(4) 0.3614(6) -0.1110(3) 0.0591(19) Uani 1 1 d . A .
H31 H 0.2707 0.3155 -0.1606 0.071 Uiso 1 1 calc R . .
C32 C 0.3323(3) 0.3756(5) -0.0484(3) 0.0470(14) Uani 1 1 d . A .
H32 H 0.3750 0.3418 -0.0464 0.056 Uiso 1 1 calc R . .
N33 N 0.31555(19) 0.7186(3) 0.2082(2) 0.0269(8) Uani 1 1 d . . .
N34 N 0.24985(18) 0.7258(3) 0.1643(2) 0.0248(7) Uani 1 1 d . A .
C35 C 0.2240(3) 0.8126(4) 0.1991(3) 0.0315(10) Uani 1 1 d . . .
H35 H 0.1791 0.8390 0.1810 0.038 Uiso 1 1 calc R A .
C36 C 0.2717(3) 0.8596(4) 0.2657(3) 0.0384(12) Uani 1 1 d . A .
H36 H 0.2654 0.9217 0.3007 0.046 Uiso 1 1 calc R . .
C37 C 0.3292(2) 0.7984(4) 0.2703(3) 0.0322(10) Uani 1 1 d . A .
H37 H 0.3709 0.8095 0.3094 0.039 Uiso 1 1 calc R . .
S38 S 0.53644(6) 0.48096(12) 0.23576(9) 0.0430(3) Uani 1 1 d . . .
C39 C 0.5723(2) 0.5905(5) 0.3136(4) 0.0466(14) Uani 1 1 d . A .
H39 H 0.5392 0.6088 0.3500 0.056 Uiso 1 1 calc R . .
C40 C 0.5877(3) 0.6955(6) 0.2689(5) 0.0609(18) Uani 1 1 d . . .
H40A H 0.6076 0.7519 0.3116 0.091 Uiso 1 1 calc R A .
H40B H 0.5460 0.7254 0.2335 0.091 Uiso 1 1 calc R . .
H40C H 0.6196 0.6778 0.2324 0.091 Uiso 1 1 calc R . .
C41 C 0.6345(3) 0.5359(6) 0.3694(4) 0.0596(19) Uani 1 1 d . . .
H41A H 0.6674 0.5189 0.3342 0.089 Uiso 1 1 calc R A .
H41B H 0.6214 0.4660 0.3941 0.089 Uiso 1 1 calc R . .
H41C H 0.6545 0.5876 0.4155 0.089 Uiso 1 1 calc R . .
Cl42 Cl 0.45099(6) 0.78037(10) 0.48992(7) 0.0335(3) Uani 1 1 d . B 1
O43 O 0.5066(2) 0.8319(4) 0.5464(2) 0.0536(11) Uani 1 1 d . B 1
O44 O 0.40018(19) 0.8617(3) 0.4581(2) 0.0477(10) Uani 1 1 d . B 1
O45 O 0.4236(3) 0.6933(4) 0.5335(3) 0.0670(13) Uani 1 1 d . B 1
O46 O 0.47510(19) 0.7321(3) 0.4188(2) 0.0430(9) Uani 1 1 d . B 1
Cl47 Cl 0.07189(6) 0.98082(11) 0.22609(7) 0.0374(3) Uani 1 1 d . . .
O48 O 0.13584(17) 1.0330(3) 0.2265(2) 0.0407(8) Uani 1 1 d . . .
O49 O 0.0189(2) 1.0608(4) 0.1992(3) 0.0568(12) Uani 1 1 d . . .
O50 O 0.0710(2) 0.9427(3) 0.3117(2) 0.0494(10) Uani 1 1 d . . .
O51 O 0.06261(19) 0.8862(4) 0.1687(2) 0.0496(10) Uani 1 1 d . . .
C52A C 0.5611(7) 0.5516(18) 0.5837(10) 0.037(5) Uiso 0.40 1 d PD D 1
H52A H 0.5323 0.6033 0.6077 0.056 Uiso 0.40 1 calc PR D 1
H52B H 0.5437 0.4748 0.5844 0.056 Uiso 0.40 1 calc PR D 1
H52C H 0.5614 0.5736 0.5246 0.056 Uiso 0.40 1 calc PR D 1
N53A N 0.6291(6) 0.5563(10) 0.6346(8) 0.037(3) Uiso 0.40 1 d PD D 1
O54A O 0.6422(5) 0.6255(9) 0.6919(6) 0.055(3) Uiso 0.40 1 d PD D 1
O55A O 0.6747(10) 0.499(2) 0.6202(17) 0.165(12) Uiso 0.40 1 d PD D 1
C52B C 0.5732(7) 0.5470(18) 0.5726(15) 0.034(6) Uiso 0.40 1 d PD C 2
H52D H 0.5575 0.4689 0.5713 0.051 Uiso 0.40 1 calc PR C 2
H52E H 0.5694 0.5743 0.5138 0.051 Uiso 0.40 1 calc PR C 2
H52F H 0.5456 0.5940 0.6022 0.051 Uiso 0.40 1 calc PR C 2
N53B N 0.6434(4) 0.5525(7) 0.6179(6) 0.042(2) Uiso 0.60 1 d PD . .
O54B O 0.6701(6) 0.6410(9) 0.6254(8) 0.067(3) Uiso 0.40 1 d PD C 2
O55B O 0.6717(5) 0.4678(7) 0.6496(6) 0.025(2) Uiso 0.40 1 d PD C 2
C52C C 0.5739(9) 0.569(3) 0.570(2) 0.027(9) Uiso 0.20 1 d PD C 3
H52G H 0.5437 0.5190 0.5935 0.040 Uiso 0.20 1 calc PR C 3
H52H H 0.5711 0.5511 0.5096 0.040 Uiso 0.20 1 calc PR C 3
H52I H 0.5605 0.6472 0.5757 0.040 Uiso 0.20 1 calc PR C 3
O54C O 0.6556(10) 0.4568(12) 0.6500(12) 0.027(6) Uiso 0.20 1 d PD C 3
O55C O 0.6856(8) 0.6093(14) 0.5956(12) 0.038(4) Uiso 0.20 1 d PD C 3


_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 N22 2.044(4) . ?
Fe1 N2 2.052(4) . ?
Fe1 N34 2.087(3) . ?
Fe1 N29 2.097(5) . ?
Fe1 N9 2.099(4) . ?
Fe1 N14 2.134(4) . ?
N2 C7 1.333(6) . ?
N2 C3 1.336(5) . ?
C3 C4 1.381(6) . ?
C3 N8 1.396(6) . ?
C4 C5 1.398(7) . ?
C4 H4 0.9500 . ?
C5 C6 1.410(6) . ?
C5 S18 1.744(5) . ?
C6 C7 1.372(6) . ?
C6 H6 0.9500 . ?
C7 N13 1.408(5) . ?
N8 C12 1.356(6) . ?
N8 N9 1.382(5) . ?
N9 C10 1.323(6) . ?
C10 C11 1.406(8) . ?
C10 H10 0.9500 . ?
C11 C12 1.356(8) . ?
C11 H11 0.9500 . ?
C12 H12 0.9500 . ?
N13 C17 1.362(7) . ?
N13 N14 1.365(6) . ?
N14 C15 1.337(6) . ?
C15 C16 1.390(10) . ?
C15 H15 0.9500 . ?
C16 C17 1.372(8) . ?
C16 H16 0.9500 . ?
C17 H17 0.9500 . ?
S18 C19 1.824(5) . ?
C19 C20 1.518(7) . ?
C19 C21 1.529(7) . ?
C19 H19 1.0000 . ?
C20 H20A 0.9800 . ?
C20 H20B 0.9800 . ?
C20 H20C 0.9800 . ?
C21 H21A 0.9800 . ?
C21 H21B 0.9800 . ?
C21 H21C 0.9800 . ?
N22 C27 1.329(5) . ?
N22 C23 1.344(6) . ?
C23 C24 1.360(6) . ?
C23 N28 1.412(5) . ?
C24 C25 1.409(6) . ?
C24 H24 0.9500 . ?
C25 C26 1.395(7) . ?
C25 S38 1.740(5) . ?
C26 C27 1.381(6) . ?
C26 H26 0.9500 . ?
C27 N33 1.401(6) . ?
N28 C32 1.352(7) . ?
N28 N29 1.371(6) . ?
N29 C30 1.338(7) . ?
C30 C31 1.388(11) . ?
C30 H30 0.9500 . ?
C31 C32 1.366(8) . ?
C31 H31 0.9500 . ?
C32 H32 0.9500 . ?
N33 C37 1.357(6) . ?
N33 N34 1.373(5) . ?
N34 C35 1.330(6) . ?
C35 C36 1.396(7) . ?
C35 H35 0.9500 . ?
C36 C37 1.366(7) . ?
C36 H36 0.9500 . ?
C37 H37 0.9500 . ?
S38 C39 1.841(5) . ?
C39 C40 1.504(9) . ?
C39 C41 1.529(8) . ?
C39 H39 1.0000 . ?
C40 H40A 0.9800 . ?
C40 H40B 0.9800 . ?
C40 H40C 0.9800 . ?
C41 H41A 0.9800 . ?
C41 H41B 0.9800 . ?
C41 H41C 0.9800 . ?
Cl42 O45 1.424(4) . ?
Cl42 O44 1.427(4) . ?
Cl42 O43 1.427(4) . ?
Cl42 O46 1.446(4) . ?
Cl47 O49 1.432(4) . ?
Cl47 O51 1.437(4) . ?
Cl47 O48 1.438(4) . ?
Cl47 O50 1.444(4) . ?
C52A N53A 1.447(13) . ?
C52A H52A 0.9800 . ?
C52A H52B 0.9800 . ?
C52A H52C 0.9800 . ?
N53A O54A 1.217(12) . ?
N53A O55A 1.214(14) . ?
C52B N53B 1.457(12) . ?
C52B H52D 0.9800 . ?
C52B H52E 0.9800 . ?
C52B H52F 0.9800 . ?
N53B O54B 1.178(11) . ?
N53B O55B 1.215(11) . ?
C52C N53B 1.469(14) . ?
C52C H52G 0.9800 . ?
C52C H52H 0.9800 . ?
C52C H52I 0.9800 . ?
N53B O55C 1.202(13) . ?
N53B O54C 1.251(13) . ?

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
N22 Fe1 N2 170.53(14) . . ?
N22 Fe1 N34 75.85(14) . . ?
N2 Fe1 N34 98.47(14) . . ?
N22 Fe1 N29 75.36(15) . . ?
N2 Fe1 N29 110.85(14) . . ?
N34 Fe1 N29 150.60(15) . . ?
N22 Fe1 N9 111.64(16) . . ?
N2 Fe1 N9 75.67(15) . . ?
N34 Fe1 N9 91.12(15) . . ?
N29 Fe1 N9 94.02(15) . . ?
N22 Fe1 N14 97.25(15) . . ?
N2 Fe1 N14 75.26(14) . . ?
N34 Fe1 N14 92.89(15) . . ?
N29 Fe1 N14 96.44(15) . . ?
N9 Fe1 N14 150.93(15) . . ?
C7 N2 C3 118.6(4) . . ?
C7 N2 Fe1 120.6(3) . . ?
C3 N2 Fe1 120.3(3) . . ?
N2 C3 C4 123.4(4) . . ?
N2 C3 N8 112.3(4) . . ?
C4 C3 N8 124.3(4) . . ?
C3 C4 C5 117.2(4) . . ?
C3 C4 H4 121.4 . . ?
C5 C4 H4 121.4 . . ?
C4 C5 C6 119.9(4) . . ?
C4 C5 S18 125.6(3) . . ?
C6 C5 S18 114.5(4) . . ?
C7 C6 C5 117.2(4) . . ?
C7 C6 H6 121.4 . . ?
C5 C6 H6 121.4 . . ?
N2 C7 C6 123.6(4) . . ?
N2 C7 N13 112.3(4) . . ?
C6 C7 N13 124.1(4) . . ?
C12 N8 N9 110.9(4) . . ?
C12 N8 C3 131.5(4) . . ?
N9 N8 C3 117.5(3) . . ?
C10 N9 N8 104.9(4) . . ?
C10 N9 Fe1 141.2(4) . . ?
N8 N9 Fe1 113.8(3) . . ?
N9 C10 C11 111.0(5) . . ?
N9 C10 H10 124.5 . . ?
C11 C10 H10 124.5 . . ?
C12 C11 C10 106.0(5) . . ?
C12 C11 H11 127.0 . . ?
C10 C11 H11 127.0 . . ?
N8 C12 C11 107.2(5) . . ?
N8 C12 H12 126.4 . . ?
C11 C12 H12 126.4 . . ?
C17 N13 N14 111.8(4) . . ?
C17 N13 C7 130.1(5) . . ?
N14 N13 C7 118.0(4) . . ?
C15 N14 N13 104.4(5) . . ?
C15 N14 Fe1 142.2(4) . . ?
N13 N14 Fe1 113.4(3) . . ?
N14 C15 C16 111.7(5) . . ?
N14 C15 H15 124.2 . . ?
C16 C15 H15 124.2 . . ?
C17 C16 C15 105.8(5) . . ?
C17 C16 H16 127.1 . . ?
C15 C16 H16 127.1 . . ?
N13 C17 C16 106.4(6) . . ?
N13 C17 H17 126.8 . . ?
C16 C17 H17 126.8 . . ?
C5 S18 C19 105.3(2) . . ?
C20 C19 C21 111.0(4) . . ?
C20 C19 S18 111.3(3) . . ?
C21 C19 S18 105.6(4) . . ?
C20 C19 H19 109.6 . . ?
C21 C19 H19 109.6 . . ?
S18 C19 H19 109.6 . . ?
C19 C20 H20A 109.5 . . ?
C19 C20 H20B 109.5 . . ?
H20A C20 H20B 109.5 . . ?
C19 C20 H20C 109.5 . . ?
H20A C20 H20C 109.5 . . ?
H20B C20 H20C 109.5 . . ?
C19 C21 H21A 109.5 . . ?
C19 C21 H21B 109.5 . . ?
H21A C21 H21B 109.5 . . ?
C19 C21 H21C 109.5 . . ?
H21A C21 H21C 109.5 . . ?
H21B C21 H21C 109.5 . . ?
C27 N22 C23 118.5(4) . . ?
C27 N22 Fe1 120.3(3) . . ?
C23 N22 Fe1 120.9(3) . . ?
N22 C23 C24 123.3(4) . . ?
N22 C23 N28 111.2(4) . . ?
C24 C23 N28 125.5(4) . . ?
C23 C24 C25 117.8(4) . . ?
C23 C24 H24 121.1 . . ?
C25 C24 H24 121.1 . . ?
C26 C25 C24 119.5(4) . . ?
C26 C25 S38 124.6(3) . . ?
C24 C25 S38 115.8(4) . . ?
C27 C26 C25 117.4(4) . . ?
C27 C26 H26 121.3 . . ?
C25 C26 H26 121.3 . . ?
N22 C27 C26 123.4(4) . . ?
N22 C27 N33 111.9(4) . . ?
C26 C27 N33 124.7(4) . . ?
C32 N28 N29 111.9(4) . . ?
C32 N28 C23 130.3(5) . . ?
N29 N28 C23 117.4(4) . . ?
C30 N29 N28 103.5(5) . . ?
C30 N29 Fe1 141.6(5) . . ?
N28 N29 Fe1 114.6(3) . . ?
N29 C30 C31 112.3(6) . . ?
N29 C30 H30 123.9 . . ?
C31 C30 H30 123.9 . . ?
C32 C31 C30 105.3(5) . . ?
C32 C31 H31 127.4 . . ?
C30 C31 H31 127.4 . . ?
N28 C32 C31 107.0(6) . . ?
N28 C32 H32 126.5 . . ?
C31 C32 H32 126.5 . . ?
C37 N33 N34 110.9(4) . . ?
C37 N33 C27 131.3(4) . . ?
N34 N33 C27 117.8(3) . . ?
C35 N34 N33 105.2(4) . . ?
C35 N34 Fe1 141.0(3) . . ?
N33 N34 Fe1 113.8(3) . . ?
N34 C35 C36 110.9(4) . . ?
N34 C35 H35 124.6 . . ?
C36 C35 H35 124.6 . . ?
C37 C36 C35 106.1(4) . . ?
C37 C36 H36 127.0 . . ?
C35 C36 H36 127.0 . . ?
N33 C37 C36 106.9(4) . . ?
N33 C37 H37 126.5 . . ?
C36 C37 H37 126.5 . . ?
C25 S38 C39 105.2(2) . . ?
C40 C39 C41 113.6(5) . . ?
C40 C39 S38 111.0(4) . . ?
C41 C39 S38 104.7(4) . . ?
C40 C39 H39 109.1 . . ?
C41 C39 H39 109.1 . . ?
S38 C39 H39 109.1 . . ?
C39 C40 H40A 109.5 . . ?
C39 C40 H40B 109.5 . . ?
H40A C40 H40B 109.5 . . ?
C39 C40 H40C 109.5 . . ?
H40A C40 H40C 109.5 . . ?
H40B C40 H40C 109.5 . . ?
C39 C41 H41A 109.5 . . ?
C39 C41 H41B 109.5 . . ?
H41A C41 H41B 109.5 . . ?
C39 C41 H41C 109.5 . . ?
H41A C41 H41C 109.5 . . ?
H41B C41 H41C 109.5 . . ?
O45 Cl42 O44 109.7(3) . . ?
O45 Cl42 O43 110.0(3) . . ?
O44 Cl42 O43 110.6(2) . . ?
O45 Cl42 O46 109.1(3) . . ?
O44 Cl42 O46 109.2(2) . . ?
O43 Cl42 O46 108.2(2) . . ?
O49 Cl47 O51 109.8(3) . . ?
O49 Cl47 O48 109.6(3) . . ?
O51 Cl47 O48 109.7(2) . . ?
O49 Cl47 O50 109.5(2) . . ?
O51 Cl47 O50 109.4(3) . . ?
O48 Cl47 O50 108.8(2) . . ?
N53A C52A H52A 109.5 . . ?
N53A C52A H52B 109.5 . . ?
H52A C52A H52B 109.5 . . ?
N53A C52A H52C 109.5 . . ?
H52A C52A H52C 109.5 . . ?
H52B C52A H52C 109.5 . . ?
O55A N53A O54A 117.9(13) . . ?
O55A N53A C52A 123.3(14) . . ?
O54A N53A C52A 118.7(12) . . ?
N53B C52B H52D 109.5 . . ?
N53B C52B H52E 109.5 . . ?
H52D C52B H52E 109.5 . . ?
N53B C52B H52F 109.5 . . ?
H52D C52B H52F 109.5 . . ?
H52E C52B H52F 109.5 . . ?
O54B N53B O55B 122.0(10) . . ?
O54B N53B C52B 118.1(12) . . ?
O55B N53B C52B 119.8(11) . . ?
N53B C52C H52G 109.5 . . ?
N53B C52C H52H 109.5 . . ?
H52G C52C H52H 109.5 . . ?
N53B C52C H52I 109.5 . . ?
H52G C52C H52I 109.5 . . ?
H52H C52C H52I 109.5 . . ?
O55C N53B O54C 122.7(13) . . ?
O55C N53B C52C 116.0(13) . . ?
O54C N53B C52C 114.7(13) . . ?

_diffrn_measured_fraction_theta_max 0.968
_diffrn_reflns_theta_full        72.00
_diffrn_measured_fraction_theta_full 0.988
_refine_diff_density_max         0.697
_refine_diff_density_min         -0.761
_refine_diff_density_rms         0.092
_exptl_crystal_recrystallization_method 
'Re-crystallisation from solvent: Nitromethane/diethyl ether'
_exptl_crystal_preparation       'Magnetic properties'
####################################################################### 
# 
# This file contains crystal structure data downloaded from the 
# Cambridge Structural Database (CSD) hosted by the Cambridge 
# Crystallographic Data Centre (CCDC).
# 
# Full information about CCDC data access policies and citation 
# guidelines are available at http://www.ccdc.cam.ac.uk/access/V1 
# 
# Audit and citation data items may have been added by the CCDC. 
# Please retain this information to preserve the provenance of 
# this file and to allow appropriate attribution of the data. 
# 
#######################################################################

data_164melt
_database_code_depnum_ccdc_archive 'CCDC 1428762'
_audit_update_record             
;
2015-09-30 deposited with the CCDC.
2017-11-20 downloaded from the CCDC.
;

_audit_creation_method           SHELXL-97
_chemical_name_systematic        
'Bis[4-(isopropylsulfanyl)-2,6-di(pyrazol-1-yl)pyridine]iron(II)diperchlorate acetonitrile solvate'
_chemical_name_common            ?
_chemical_melting_point          ?
_chemical_formula_moiety         'C28 H30 Fe N10 S2, 2(Cl O4), C2 H3 N'
_chemical_formula_sum            'C30 H33 Cl2 Fe N11 O8 S2'
_chemical_formula_weight         866.54

loop_
_atom_type_symbol
_atom_type_description
_atom_type_scat_dispersion_real
_atom_type_scat_dispersion_imag
_atom_type_scat_source
Cl Cl 0.3639 0.7018 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
C C 0.0181 0.0091 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
O O 0.0492 0.0322 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Fe Fe -1.1336 3.1974 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
N N 0.0311 0.0180 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
S S 0.3331 0.5567 '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'

_symmetry_cell_setting           monoclinic
_symmetry_space_group_name_H-M   'P 21/c'

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

_cell_length_a                   20.4344(2)
_cell_length_b                   11.8060(1)
_cell_length_c                   15.9788(2)
_cell_angle_alpha                90.00
_cell_angle_beta                 100.5150(10)
_cell_angle_gamma                90.00
_cell_volume                     3790.13(7)
_cell_formula_units_Z            4
_cell_measurement_temperature    140(2)
_cell_measurement_reflns_used    9540
_cell_measurement_theta_min      4.39
_cell_measurement_theta_max      73.69

_exptl_crystal_description       plate
_exptl_crystal_colour            yellow
_exptl_crystal_size_max          0.28
_exptl_crystal_size_mid          0.20
_exptl_crystal_size_min          0.06
_exptl_crystal_density_meas      ?
_exptl_crystal_density_diffrn    1.519
_exptl_crystal_density_method    'not measured'
_exptl_crystal_F_000             1784
_exptl_absorpt_coefficient_mu    6.066
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_correction_T_min  0.518
_exptl_absorpt_correction_T_max  1.000
_exptl_absorpt_process_details   
; 
CrysAlisPro, Agilent Technologies,
Version 1.171.36.24 (release 03-12-2012 CrysAlis171 .NET)
Empirical absorption correction using spherical harmonics,
 implemented in SCALE3 ABSPACK scaling algorithm.
;

_diffrn_ambient_temperature      140(2)
_diffrn_radiation_wavelength     1.54184
_diffrn_radiation_type           CuK\a
_diffrn_radiation_source         'SuperNova (Cu) X-ray Source'
_diffrn_radiation_monochromator  mirror
_diffrn_measurement_device_type  'SuperNova, Dual, Cu at zero, Atlas'
_diffrn_measurement_method       'ω scans'
_diffrn_detector_area_resol_mean 5.3095
_diffrn_standards_number         0
_diffrn_standards_interval_count 0
_diffrn_standards_interval_time  0
_diffrn_standards_decay_%        0
_diffrn_reflns_number            14687
_diffrn_reflns_av_R_equivalents  0.0357
_diffrn_reflns_av_sigmaI/netI    0.0382
_diffrn_reflns_limit_h_min       -24
_diffrn_reflns_limit_h_max       24
_diffrn_reflns_limit_k_min       -14
_diffrn_reflns_limit_k_max       12
_diffrn_reflns_limit_l_min       -18
_diffrn_reflns_limit_l_max       15
_diffrn_reflns_theta_min         4.40
_diffrn_reflns_theta_max         67.08
_reflns_number_total             6727
_reflns_number_gt                6272
_reflns_threshold_expression     >2sigma(I)

_computing_data_collection       'CrysAlisPro, Agilent Technologies'
_computing_cell_refinement       'CrysAlisPro, Agilent Technologies'
_computing_data_reduction        'CrysAlisPro, Agilent Technologies'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_molecular_graphics    'XSEED (Barbour, 2001)'
_computing_publication_material  'local program'

_refine_special_details          
; 
 Refinement of F² against ALL reflections.  The weighted R-factor wR and 
 goodness of fit S are based on F², conventional R-factors R are based 
 on F, with F set to zero for negative F². The threshold expression of 
 F² > 2sigma(F²) is used only for calculating R-factors(gt) etc. and is 
 not relevant to the choice of reflections for refinement.  R-factors based 
 on F² are statistically about twice as large as those based on F, and R- 
 factors based on ALL data will be even larger. 

 No disorder is present in the model, and no restraints were applied. All 
 non-H atoms were refined anisotropically, and H atoms were placed in 
 calculated positions and refined using a riding model.
;

_refine_ls_structure_factor_coef Fsqd
_refine_ls_matrix_type           full
_refine_ls_weighting_scheme      calc
_refine_ls_weighting_details     
'calc w=1/[σ²(Fo²)+(0.0649P)²+1.3270P] 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         6727
_refine_ls_number_parameters     492
_refine_ls_number_restraints     0
_refine_ls_R_factor_all          0.0409
_refine_ls_R_factor_gt           0.0381
_refine_ls_wR_factor_ref         0.1028
_refine_ls_wR_factor_gt          0.0998
_refine_ls_goodness_of_fit_ref   1.024
_refine_ls_restrained_S_all      1.024
_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_symmetry_multiplicity
_atom_site_calc_flag
_atom_site_refinement_flags
_atom_site_disorder_assembly
_atom_site_disorder_group
Fe1 Fe 0.222047(14) 0.60120(3) 0.05937(2) 0.01902(10) Uani 1 1 d . . .
N2 N 0.11682(8) 0.62678(15) 0.03583(11) 0.0180(3) Uani 1 1 d . . .
C3 C 0.08865(9) 0.70493(17) -0.01924(12) 0.0178(4) Uani 1 1 d . . .
C4 C 0.02271(10) 0.73738(18) -0.02977(13) 0.0204(4) Uani 1 1 d . . .
H4 H 0.0044 0.7926 -0.0707 0.024 Uiso 1 1 calc R . .
C5 C -0.01589(9) 0.68440(18) 0.02315(13) 0.0213(4) Uani 1 1 d . . .
C6 C 0.01285(10) 0.60201(18) 0.08161(14) 0.0232(4) Uani 1 1 d . . .
H6 H -0.0124 0.5650 0.1179 0.028 Uiso 1 1 calc R . .
C7 C 0.07863(10) 0.57666(18) 0.08449(13) 0.0198(4) Uani 1 1 d . . .
N8 N 0.13427(8) 0.75421(15) -0.06535(11) 0.0182(3) Uani 1 1 d . . .
N9 N 0.20048(8) 0.73023(16) -0.03956(11) 0.0219(4) Uani 1 1 d . . .
C10 C 0.23155(11) 0.7934(2) -0.08833(15) 0.0275(5) Uani 1 1 d . . .
H10 H 0.2785 0.7954 -0.0846 0.033 Uiso 1 1 calc R . .
C11 C 0.18617(11) 0.8570(2) -0.14639(15) 0.0291(5) Uani 1 1 d . . .
H11 H 0.1960 0.9083 -0.1882 0.035 Uiso 1 1 calc R . .
C12 C 0.12504(10) 0.82952(19) -0.12999(14) 0.0240(4) Uani 1 1 d . . .
H12 H 0.0835 0.8581 -0.1588 0.029 Uiso 1 1 calc R . .
N13 N 0.11319(8) 0.49522(15) 0.14016(12) 0.0219(4) Uani 1 1 d . . .
N14 N 0.17997(8) 0.48201(16) 0.14229(12) 0.0229(4) Uani 1 1 d . . .
C15 C 0.19712(12) 0.3952(2) 0.19386(15) 0.0297(5) Uani 1 1 d . . .
H15 H 0.2411 0.3660 0.2079 0.036 Uiso 1 1 calc R . .
C16 C 0.14258(12) 0.3510(2) 0.22546(16) 0.0326(5) Uani 1 1 d . . .
H16 H 0.1424 0.2890 0.2633 0.039 Uiso 1 1 calc R . .
C17 C 0.08972(12) 0.4171(2) 0.18967(15) 0.0287(5) Uani 1 1 d . . .
H17 H 0.0450 0.4096 0.1979 0.034 Uiso 1 1 calc R . .
S18 S -0.10023(2) 0.70969(5) 0.02169(4) 0.02756(14) Uani 1 1 d . . .
C19 C -0.11853(10) 0.8438(2) -0.03427(15) 0.0266(5) Uani 1 1 d . . .
H19 H -0.1035 0.8402 -0.0904 0.032 Uiso 1 1 calc R . .
C20 C -0.08411(12) 0.9409(2) 0.01737(18) 0.0365(6) Uani 1 1 d . . .
H20A H -0.0925 1.0113 -0.0154 0.055 Uiso 1 1 calc R . .
H20B H -0.0361 0.9265 0.0306 0.055 Uiso 1 1 calc R . .
H20C H -0.1014 0.9481 0.0705 0.055 Uiso 1 1 calc R . .
C21 C -0.19411(11) 0.8562(3) -0.04890(19) 0.0409(6) Uani 1 1 d . . .
H21A H -0.2089 0.8575 0.0061 0.061 Uiso 1 1 calc R . .
H21B H -0.2148 0.7920 -0.0827 0.061 Uiso 1 1 calc R . .
H21C H -0.2071 0.9269 -0.0795 0.061 Uiso 1 1 calc R . .
N22 N 0.32417(8) 0.57266(15) 0.11195(11) 0.0173(3) Uani 1 1 d . . .
C23 C 0.35921(10) 0.49215(17) 0.08131(13) 0.0178(4) Uani 1 1 d . . .
C24 C 0.42416(10) 0.46627(18) 0.11521(13) 0.0206(4) Uani 1 1 d . . .
H24 H 0.4473 0.4078 0.0919 0.025 Uiso 1 1 calc R . .
C25 C 0.45490(9) 0.52951(18) 0.18553(14) 0.0213(4) Uani 1 1 d . . .
C26 C 0.41985(10) 0.61601(18) 0.21761(13) 0.0212(4) Uani 1 1 d . . .
H26 H 0.4399 0.6609 0.2647 0.025 Uiso 1 1 calc R . .
C27 C 0.35484(9) 0.63329(17) 0.17786(13) 0.0179(4) Uani 1 1 d . . .
N28 N 0.32207(8) 0.43842(15) 0.00897(11) 0.0195(3) Uani 1 1 d . . .
N29 N 0.25758(8) 0.47189(15) -0.01860(11) 0.0203(4) Uani 1 1 d . . .
C30 C 0.23657(10) 0.41206(19) -0.08854(14) 0.0233(4) Uani 1 1 d . . .
H30 H 0.1932 0.4173 -0.1220 0.028 Uiso 1 1 calc R . .
C31 C 0.28648(11) 0.3404(2) -0.10653(16) 0.0313(5) Uani 1 1 d . . .
H31 H 0.2837 0.2889 -0.1527 0.038 Uiso 1 1 calc R . .
C32 C 0.34043(11) 0.3599(2) -0.04343(15) 0.0289(5) Uani 1 1 d . . .
H32 H 0.3828 0.3247 -0.0377 0.035 Uiso 1 1 calc R . .
N33 N 0.31391(8) 0.71831(15) 0.20242(11) 0.0190(3) Uani 1 1 d . . .
N34 N 0.25051(8) 0.72819(16) 0.15774(11) 0.0225(4) Uani 1 1 d . . .
C35 C 0.22510(11) 0.8174(2) 0.19114(15) 0.0275(5) Uani 1 1 d . . .
H35 H 0.1812 0.8452 0.1728 0.033 Uiso 1 1 calc R . .
C36 C 0.27166(11) 0.8651(2) 0.25695(15) 0.0282(5) Uani 1 1 d . . .
H36 H 0.2657 0.9293 0.2906 0.034 Uiso 1 1 calc R . .
C37 C 0.32746(10) 0.79978(18) 0.26247(14) 0.0236(4) Uani 1 1 d . . .
H37 H 0.3682 0.8098 0.3013 0.028 Uiso 1 1 calc R . .
S38 S 0.53644(3) 0.49016(5) 0.22933(4) 0.03190(15) Uani 1 1 d . . .
C39 C 0.56787(11) 0.6034(2) 0.30377(16) 0.0311(5) Uani 1 1 d . . .
H39 H 0.5344 0.6194 0.3408 0.037 Uiso 1 1 calc R . .
C40 C 0.57935(14) 0.7102(2) 0.2561(2) 0.0458(7) Uani 1 1 d . . .
H40A H 0.5953 0.7705 0.2969 0.069 Uiso 1 1 calc R . .
H40B H 0.5375 0.7338 0.2201 0.069 Uiso 1 1 calc R . .
H40C H 0.6127 0.6955 0.2204 0.069 Uiso 1 1 calc R . .
C41 C 0.63128(13) 0.5576(3) 0.35884(19) 0.0496(8) Uani 1 1 d . . .
H41A H 0.6646 0.5431 0.3231 0.074 Uiso 1 1 calc R . .
H41B H 0.6213 0.4870 0.3861 0.074 Uiso 1 1 calc R . .
H41C H 0.6487 0.6135 0.4027 0.074 Uiso 1 1 calc R . .
Cl42 Cl 0.44092(2) 0.77352(5) 0.48345(3) 0.02708(13) Uani 1 1 d . . .
O43 O 0.49697(9) 0.82576(18) 0.53530(13) 0.0441(5) Uani 1 1 d . . .
O44 O 0.39054(10) 0.85562(19) 0.45411(12) 0.0487(5) Uani 1 1 d . . .
O45 O 0.41487(12) 0.6892(2) 0.53166(18) 0.0661(7) Uani 1 1 d . . .
O46 O 0.46282(11) 0.7231(2) 0.41165(12) 0.0534(6) Uani 1 1 d . . .
Cl47 Cl 0.07774(2) 0.98977(5) 0.22832(3) 0.02743(13) Uani 1 1 d . . .
O48 O 0.14112(8) 1.04158(17) 0.22691(12) 0.0374(4) Uani 1 1 d . . .
O49 O 0.02566(9) 1.07248(19) 0.20684(13) 0.0473(5) Uani 1 1 d . . .
O50 O 0.07737(10) 0.94797(18) 0.31261(12) 0.0452(5) Uani 1 1 d . . .
O51 O 0.06734(10) 0.89859(19) 0.16858(14) 0.0502(5) Uani 1 1 d . . .
C52 C 0.56607(15) 0.5589(3) 0.5765(2) 0.0514(7) Uani 1 1 d . . .
H52A H 0.5496 0.4843 0.5555 0.077 Uiso 1 1 calc R . .
H52B H 0.5661 0.6100 0.5281 0.077 Uiso 1 1 calc R . .
H52C H 0.5371 0.5899 0.6134 0.077 Uiso 1 1 calc R . .
C53 C 0.63259(15) 0.5482(3) 0.6239(2) 0.0472(7) Uani 1 1 d . . .
N54 N 0.68417(16) 0.5373(4) 0.6619(3) 0.0889(12) 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 N22 2.1295(16) . ?
Fe1 N2 2.1356(16) . ?
Fe1 N34 2.1732(18) . ?
Fe1 N29 2.1772(18) . ?
Fe1 N9 2.1815(18) . ?
Fe1 N14 2.2115(19) . ?
N2 C3 1.331(3) . ?
N2 C7 1.336(3) . ?
C3 C4 1.381(3) . ?
C3 N8 1.415(3) . ?
C4 C5 1.404(3) . ?
C4 H4 0.9500 . ?
C5 C6 1.401(3) . ?
C5 S18 1.7450(19) . ?
C6 C7 1.370(3) . ?
C6 H6 0.9500 . ?
C7 N13 1.409(3) . ?
N8 C12 1.350(3) . ?
N8 N9 1.370(2) . ?
N9 C10 1.322(3) . ?
C10 C11 1.404(3) . ?
C10 H10 0.9500 . ?
C11 C12 1.362(3) . ?
C11 H11 0.9500 . ?
C12 H12 0.9500 . ?
N13 C17 1.358(3) . ?
N13 N14 1.368(2) . ?
N14 C15 1.322(3) . ?
C15 C16 1.405(4) . ?
C15 H15 0.9500 . ?
C16 C17 1.370(3) . ?
C16 H16 0.9500 . ?
C17 H17 0.9500 . ?
S18 C19 1.823(2) . ?
C19 C20 1.510(3) . ?
C19 C21 1.526(3) . ?
C19 H19 1.0000 . ?
C20 H20A 0.9800 . ?
C20 H20B 0.9800 . ?
C20 H20C 0.9800 . ?
C21 H21A 0.9800 . ?
C21 H21B 0.9800 . ?
C21 H21C 0.9800 . ?
N22 C27 1.332(3) . ?
N22 C23 1.335(3) . ?
C23 C24 1.373(3) . ?
C23 N28 1.412(3) . ?
C24 C25 1.399(3) . ?
C24 H24 0.9500 . ?
C25 C26 1.397(3) . ?
C25 S38 1.748(2) . ?
C26 C27 1.379(3) . ?
C26 H26 0.9500 . ?
C27 N33 1.408(3) . ?
N28 C32 1.347(3) . ?
N28 N29 1.369(2) . ?
N29 C30 1.325(3) . ?
C30 C31 1.395(3) . ?
C30 H30 0.9500 . ?
C31 C32 1.371(3) . ?
C31 H31 0.9500 . ?
C32 H32 0.9500 . ?
N33 C37 1.351(3) . ?
N33 N34 1.365(2) . ?
N34 C35 1.329(3) . ?
C35 C36 1.401(3) . ?
C35 H35 0.9500 . ?
C36 C37 1.366(3) . ?
C36 H36 0.9500 . ?
C37 H37 0.9500 . ?
S38 C39 1.826(2) . ?
C39 C40 1.513(4) . ?
C39 C41 1.526(3) . ?
C39 H39 1.0000 . ?
C40 H40A 0.9800 . ?
C40 H40B 0.9800 . ?
C40 H40C 0.9800 . ?
C41 H41A 0.9800 . ?
C41 H41B 0.9800 . ?
C41 H41C 0.9800 . ?
Cl42 O45 1.421(2) . ?
Cl42 O43 1.4255(18) . ?
Cl42 O44 1.4294(19) . ?
Cl42 O46 1.4347(19) . ?
Cl47 O51 1.429(2) . ?
Cl47 O50 1.4358(19) . ?
Cl47 O48 1.4361(18) . ?
Cl47 O49 1.4390(18) . ?
C52 C53 1.436(4) . ?
C52 H52A 0.9800 . ?
C52 H52B 0.9800 . ?
C52 H52C 0.9800 . ?
C53 N54 1.124(4) . ?

loop_
_geom_angle_atom_site_label_1
_geom_angle_atom_site_label_2
_geom_angle_atom_site_label_3
_geom_angle
_geom_angle_site_symmetry_1
_geom_angle_site_symmetry_3
_geom_angle_publ_flag
N22 Fe1 N2 167.05(7) . . ?
N22 Fe1 N34 73.15(6) . . ?
N2 Fe1 N34 99.08(6) . . ?
N22 Fe1 N29 73.12(6) . . ?
N2 Fe1 N29 115.37(6) . . ?
N34 Fe1 N29 145.53(6) . . ?
N22 Fe1 N9 116.76(6) . . ?
N2 Fe1 N9 73.13(6) . . ?
N34 Fe1 N9 91.97(7) . . ?
N29 Fe1 N9 96.85(7) . . ?
N22 Fe1 N14 97.07(6) . . ?
N2 Fe1 N14 72.93(6) . . ?
N34 Fe1 N14 95.03(7) . . ?
N29 Fe1 N14 95.93(7) . . ?
N9 Fe1 N14 146.01(6) . . ?
C3 N2 C7 117.62(17) . . ?
C3 N2 Fe1 120.96(13) . . ?
C7 N2 Fe1 120.74(14) . . ?
N2 C3 C4 124.56(19) . . ?
N2 C3 N8 112.50(16) . . ?
C4 C3 N8 122.92(19) . . ?
C3 C4 C5 116.48(19) . . ?
C3 C4 H4 121.8 . . ?
C5 C4 H4 121.8 . . ?
C6 C5 C4 119.83(18) . . ?
C6 C5 S18 114.87(16) . . ?
C4 C5 S18 125.28(16) . . ?
C7 C6 C5 117.61(19) . . ?
C7 C6 H6 121.2 . . ?
C5 C6 H6 121.2 . . ?
N2 C7 C6 123.9(2) . . ?
N2 C7 N13 113.01(17) . . ?
C6 C7 N13 123.10(19) . . ?
C12 N8 N9 111.03(16) . . ?
C12 N8 C3 131.01(17) . . ?
N9 N8 C3 117.82(16) . . ?
C10 N9 N8 105.09(17) . . ?
C10 N9 Fe1 139.98(14) . . ?
N8 N9 Fe1 114.85(13) . . ?
N9 C10 C11 111.17(19) . . ?
N9 C10 H10 124.4 . . ?
C11 C10 H10 124.4 . . ?
C12 C11 C10 105.3(2) . . ?
C12 C11 H11 127.4 . . ?
C10 C11 H11 127.4 . . ?
N8 C12 C11 107.42(19) . . ?
N8 C12 H12 126.3 . . ?
C11 C12 H12 126.3 . . ?
C17 N13 N14 111.39(18) . . ?
C17 N13 C7 129.91(18) . . ?
N14 N13 C7 118.45(17) . . ?
C15 N14 N13 104.70(18) . . ?
C15 N14 Fe1 141.18(15) . . ?
N13 N14 Fe1 114.07(13) . . ?
N14 C15 C16 112.0(2) . . ?
N14 C15 H15 124.0 . . ?
C16 C15 H15 124.0 . . ?
C17 C16 C15 104.8(2) . . ?
C17 C16 H16 127.6 . . ?
C15 C16 H16 127.6 . . ?
N13 C17 C16 107.1(2) . . ?
N13 C17 H17 126.4 . . ?
C16 C17 H17 126.4 . . ?
C5 S18 C19 105.60(10) . . ?
C20 C19 C21 111.6(2) . . ?
C20 C19 S18 110.99(17) . . ?
C21 C19 S18 105.64(17) . . ?
C20 C19 H19 109.5 . . ?
C21 C19 H19 109.5 . . ?
S18 C19 H19 109.5 . . ?
C19 C20 H20A 109.5 . . ?
C19 C20 H20B 109.5 . . ?
H20A C20 H20B 109.5 . . ?
C19 C20 H20C 109.5 . . ?
H20A C20 H20C 109.5 . . ?
H20B C20 H20C 109.5 . . ?
C19 C21 H21A 109.5 . . ?
C19 C21 H21B 109.5 . . ?
H21A C21 H21B 109.5 . . ?
C19 C21 H21C 109.5 . . ?
H21A C21 H21C 109.5 . . ?
H21B C21 H21C 109.5 . . ?
C27 N22 C23 117.77(17) . . ?
C27 N22 Fe1 120.85(13) . . ?
C23 N22 Fe1 121.36(13) . . ?
N22 C23 C24 123.92(19) . . ?
N22 C23 N28 112.06(17) . . ?
C24 C23 N28 124.01(18) . . ?
C23 C24 C25 117.26(18) . . ?
C23 C24 H24 121.4 . . ?
C25 C24 H24 121.4 . . ?
C26 C25 C24 119.97(18) . . ?
C26 C25 S38 124.22(17) . . ?
C24 C25 S38 115.79(16) . . ?
C27 C26 C25 117.02(19) . . ?
C27 C26 H26 121.5 . . ?
C25 C26 H26 121.5 . . ?
N22 C27 C26 124.02(19) . . ?
N22 C27 N33 112.70(17) . . ?
C26 C27 N33 123.27(19) . . ?
C32 N28 N29 111.06(17) . . ?
C32 N28 C23 130.44(17) . . ?
N29 N28 C23 118.40(16) . . ?
C30 N29 N28 105.19(17) . . ?
C30 N29 Fe1 139.97(14) . . ?
N28 N29 Fe1 114.84(13) . . ?
N29 C30 C31 111.14(19) . . ?
N29 C30 H30 124.4 . . ?
C31 C30 H30 124.4 . . ?
C32 C31 C30 105.4(2) . . ?
C32 C31 H31 127.3 . . ?
C30 C31 H31 127.3 . . ?
N28 C32 C31 107.16(19) . . ?
N28 C32 H32 126.4 . . ?
C31 C32 H32 126.4 . . ?
C37 N33 N34 111.25(16) . . ?
C37 N33 C27 130.58(17) . . ?
N34 N33 C27 118.08(16) . . ?
C35 N34 N33 105.12(17) . . ?
C35 N34 Fe1 139.89(15) . . ?
N33 N34 Fe1 114.99(12) . . ?
N34 C35 C36 111.02(19) . . ?
N34 C35 H35 124.5 . . ?
C36 C35 H35 124.5 . . ?
C37 C36 C35 105.41(19) . . ?
C37 C36 H36 127.3 . . ?
C35 C36 H36 127.3 . . ?
N33 C37 C36 107.21(19) . . ?
N33 C37 H37 126.4 . . ?
C36 C37 H37 126.4 . . ?
C25 S38 C39 105.20(10) . . ?
C40 C39 C41 113.1(2) . . ?
C40 C39 S38 110.51(18) . . ?
C41 C39 S38 106.09(18) . . ?
C40 C39 H39 109.0 . . ?
C41 C39 H39 109.0 . . ?
S38 C39 H39 109.0 . . ?
C39 C40 H40A 109.5 . . ?
C39 C40 H40B 109.5 . . ?
H40A C40 H40B 109.5 . . ?
C39 C40 H40C 109.5 . . ?
H40A C40 H40C 109.5 . . ?
H40B C40 H40C 109.5 . . ?
C39 C41 H41A 109.5 . . ?
C39 C41 H41B 109.5 . . ?
H41A C41 H41B 109.5 . . ?
C39 C41 H41C 109.5 . . ?
H41A C41 H41C 109.5 . . ?
H41B C41 H41C 109.5 . . ?
O45 Cl42 O43 109.20(15) . . ?
O45 Cl42 O44 109.54(15) . . ?
O43 Cl42 O44 110.57(12) . . ?
O45 Cl42 O46 110.19(16) . . ?
O43 Cl42 O46 108.04(13) . . ?
O44 Cl42 O46 109.28(12) . . ?
O51 Cl47 O50 110.00(14) . . ?
O51 Cl47 O48 109.58(12) . . ?
O50 Cl47 O48 108.67(12) . . ?
O51 Cl47 O49 109.79(13) . . ?
O50 Cl47 O49 109.07(11) . . ?
O48 Cl47 O49 109.70(12) . . ?
C53 C52 H52A 109.5 . . ?
C53 C52 H52B 109.5 . . ?
H52A C52 H52B 109.5 . . ?
C53 C52 H52C 109.5 . . ?
H52A C52 H52C 109.5 . . ?
H52B C52 H52C 109.5 . . ?
N54 C53 C52 178.3(4) . . ?

_diffrn_measured_fraction_theta_max 0.995
_diffrn_reflns_theta_full        67.08
_diffrn_measured_fraction_theta_full 0.995
_refine_diff_density_max         0.495
_refine_diff_density_min         -0.359
_refine_diff_density_rms         0.067
_exptl_crystal_recrystallization_method 
'Re-crystallisation from solvent: Acetonitrile-diethyl ether'
_exptl_crystal_preparation       'Magnetic properties'
####################################################################### 
# 
# This file contains crystal structure data downloaded from the 
# Cambridge Structural Database (CSD) hosted by the Cambridge 
# Crystallographic Data Centre (CCDC).
# 
# Full information about CCDC data access policies and citation 
# guidelines are available at http://www.ccdc.cam.ac.uk/access/V1 
# 
# Audit and citation data items may have been added by the CCDC. 
# Please retain this information to preserve the provenance of 
# this file and to allow appropriate attribution of the data. 
# 
#######################################################################

data_164aclt
_database_code_depnum_ccdc_archive 'CCDC 1428764'
_audit_update_record             
;
2015-09-30 deposited with the CCDC.
2017-11-20 downloaded from the CCDC.
;

_audit_creation_method           SHELXL-97
_chemical_name_systematic        
'Bis[4-(isopropylsulfanyl)-2,6-di(pyrazol-1-yl)pyridine]iron(II)diperchlorate acetone solvate'
_chemical_name_common            ?
_chemical_melting_point          ?
_chemical_formula_moiety         'C28 H30 Fe N10 S2, 2(Cl O4), 0.7(C3 H6 O)'
_chemical_formula_sum            'C30.10 H34.20 Cl2 Fe N10 O8.70 S2'
_chemical_formula_weight         866.14

loop_
_atom_type_symbol
_atom_type_description
_atom_type_scat_dispersion_real
_atom_type_scat_dispersion_imag
_atom_type_scat_source
Cl Cl 0.3639 0.7018 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
C C 0.0181 0.0091 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Fe Fe -1.1336 3.1974 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
N N 0.0311 0.0180 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
O O 0.0492 0.0322 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
S S 0.3331 0.5567 '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'

_symmetry_cell_setting           monoclinic
_symmetry_space_group_name_H-M   'P 21/c'

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

_cell_length_a                   20.4826(3)
_cell_length_b                   11.8109(2)
_cell_length_c                   16.2096(2)
_cell_angle_alpha                90.00
_cell_angle_beta                 101.4190(10)
_cell_angle_gamma                90.00
_cell_volume                     3843.77(10)
_cell_formula_units_Z            4
_cell_measurement_temperature    150(2)
_cell_measurement_reflns_used    7932
_cell_measurement_theta_min      4.39
_cell_measurement_theta_max      73.72

_exptl_crystal_description       plate
_exptl_crystal_colour            yellow
_exptl_crystal_size_max          0.21
_exptl_crystal_size_mid          0.17
_exptl_crystal_size_min          0.05
_exptl_crystal_density_meas      ?
_exptl_crystal_density_diffrn    1.497
_exptl_crystal_density_method    'not measured'
_exptl_crystal_F_000             1786
_exptl_absorpt_coefficient_mu    5.986
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_correction_T_min  0.538
_exptl_absorpt_correction_T_max  1.000
_exptl_absorpt_process_details   
; 
CrysAlisPro, Agilent Technologies,
Version 1.171.36.24 (release 03-12-2012 CrysAlis171 .NET)
Empirical absorption correction using spherical harmonics,
 implemented in SCALE3 ABSPACK scaling algorithm.
;

_diffrn_ambient_temperature      150(2)
_diffrn_radiation_wavelength     1.54184
_diffrn_radiation_type           CuK\a
_diffrn_radiation_source         'SuperNova (Cu) X-ray Source'
_diffrn_radiation_monochromator  mirror
_diffrn_measurement_device_type  'SuperNova, Dual, Cu at zero, Atlas'
_diffrn_measurement_method       'ω scans'
_diffrn_detector_area_resol_mean 5.3095
_diffrn_standards_number         0
_diffrn_standards_interval_count 0
_diffrn_standards_interval_time  0
_diffrn_standards_decay_%        0
_diffrn_reflns_number            16056
_diffrn_reflns_av_R_equivalents  0.0375
_diffrn_reflns_av_sigmaI/netI    0.0423
_diffrn_reflns_limit_h_min       -20
_diffrn_reflns_limit_h_max       25
_diffrn_reflns_limit_k_min       -11
_diffrn_reflns_limit_k_max       14
_diffrn_reflns_limit_l_min       -17
_diffrn_reflns_limit_l_max       20
_diffrn_reflns_theta_min         4.34
_diffrn_reflns_theta_max         73.81
_reflns_number_total             7596
_reflns_number_gt                6695
_reflns_threshold_expression     >2sigma(I)

_computing_data_collection       'CrysAlisPro, Agilent Technologies'
_computing_cell_refinement       'CrysAlisPro, Agilent Technologies'
_computing_data_reduction        'CrysAlisPro, Agilent Technologies'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_molecular_graphics    'XSEED (Barbour, 2001)'
_computing_publication_material  'local program'

_refine_special_details          
; 
 Refinement of F² against ALL reflections.  The weighted R-factor wR and 
 goodness of fit S are based on F², conventional R-factors R are based 
 on F, with F set to zero for negative F². The threshold expression of 
 F² > 2sigma(F²) is used only for calculating R-factors(gt) etc. and is 
 not relevant to the choice of reflections for refinement.  R-factors based 
 on F² are statistically about twice as large as those based on F, and R- 
 factors based on ALL data will be even larger. 

 One of the isopropyl substitutents on the complex cation is disordered over 
 three equally occupied orientations, two of which share a common two-thirds 
 occupied S atom.  These were modelled with the fixed restraints 
 C(pyridyl)---S = 1.75(2), C(alkyl)---S = 1.82(2), C---C = 1.52(2), 
 1,3-C---C---C = 2.48(2) and 1,3-C---S---C = 2.83(2) Å. The ClO₄⁻ ion 
 Cl42-O46 is also disordered over three orientations with occupancies of 
 0.50, 0.30 and 0.20. The refined restraints Cl---O = 1.42(2) and O...O = 
 2.32(2) Å were applied to those residues. Finally, the acetone solvent 
 molecule is also badly disordered. Three partial solvent sites were 
 located in the Fourier map, whose occupancies sum to 0.7. The fixed 
 restraints C---O = 1.22(2), C---C = 1.51(2), 1,3-C...C = 2.62(2) and 
 1,3-C...O = 2.37(2) Å were applied to these sites.

 All fully occupied non-H atoms, plus the two-thirds occupied S atom, were 
 refined anisotropically, and H atoms were placed in calculated positions 
 and refined using a riding model.
;

_refine_ls_structure_factor_coef Fsqd
_refine_ls_matrix_type           full
_refine_ls_weighting_scheme      calc
_refine_ls_weighting_details     
'calc w=1/[σ²(Fo²)+(0.0967P)²+3.9305P] 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         7596
_refine_ls_number_parameters     539
_refine_ls_number_restraints     65
_refine_ls_R_factor_all          0.0655
_refine_ls_R_factor_gt           0.0589
_refine_ls_wR_factor_ref         0.1670
_refine_ls_wR_factor_gt          0.1595
_refine_ls_goodness_of_fit_ref   1.042
_refine_ls_restrained_S_all      1.052
_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_symmetry_multiplicity
_atom_site_calc_flag
_atom_site_refinement_flags
_atom_site_disorder_assembly
_atom_site_disorder_group
Fe1 Fe 0.22311(2) 0.60118(4) 0.05618(3) 0.02404(15) Uani 1 1 d . B .
N2 N 0.11798(12) 0.6265(2) 0.03419(15) 0.0228(5) Uani 1 1 d . . .
C3 C 0.08884(14) 0.7023(2) -0.02209(17) 0.0221(5) Uani 1 1 d . . .
C4 C 0.02290(14) 0.7350(3) -0.03192(19) 0.0258(6) Uani 1 1 d . . .
H4 H 0.0038 0.7891 -0.0731 0.031 Uiso 1 1 calc R . .
C5 C -0.01428(14) 0.6844(3) 0.02165(19) 0.0266(6) Uani 1 1 d . . .
C6 C 0.01533(16) 0.6040(3) 0.0810(2) 0.0293(6) Uani 1 1 d . . .
H6 H -0.0092 0.5684 0.1178 0.035 Uiso 1 1 calc R . .
C7 C 0.08110(15) 0.5789(3) 0.08403(18) 0.0242(6) Uani 1 1 d . . .
N8 N 0.13285(12) 0.7465(2) -0.07058(15) 0.0237(5) Uani 1 1 d . . .
N9 N 0.19799(13) 0.7141(3) -0.05122(18) 0.0343(6) Uani 1 1 d . . .
C10 C 0.22685(18) 0.7678(4) -0.1054(3) 0.0516(11) Uani 1 1 d . . .
H10 H 0.2730 0.7631 -0.1064 0.062 Uiso 1 1 calc R . .
C11 C 0.18097(19) 0.8329(4) -0.1615(3) 0.0488(10) Uani 1 1 d . . .
H11 H 0.1895 0.8779 -0.2067 0.059 Uiso 1 1 calc R . .
C12 C 0.12150(17) 0.8179(3) -0.1375(2) 0.0326(7) Uani 1 1 d . . .
H12 H 0.0801 0.8510 -0.1627 0.039 Uiso 1 1 calc R . .
N13 N 0.11695(13) 0.5004(2) 0.14103(17) 0.0287(5) Uani 1 1 d . . .
N14 N 0.18399(13) 0.4895(2) 0.14442(17) 0.0303(6) Uani 1 1 d . . .
C15 C 0.2026(2) 0.4067(3) 0.1990(2) 0.0433(9) Uani 1 1 d . . .
H15 H 0.2471 0.3800 0.2147 0.052 Uiso 1 1 calc R . .
C16 C 0.1488(2) 0.3631(4) 0.2308(3) 0.0494(10) Uani 1 1 d . . .
H16 H 0.1497 0.3032 0.2702 0.059 Uiso 1 1 calc R . .
C17 C 0.09481(19) 0.4253(3) 0.1929(2) 0.0375(7) Uani 1 1 d . . .
H17 H 0.0504 0.4175 0.2011 0.045 Uiso 1 1 calc R . .
S18 S -0.09879(4) 0.70890(7) 0.01916(6) 0.0357(2) Uani 1 1 d . . .
C19 C -0.11793(15) 0.8418(3) -0.0382(2) 0.0330(7) Uani 1 1 d . . .
H19 H -0.1012 0.8385 -0.0921 0.040 Uiso 1 1 calc R . .
C20 C -0.0863(2) 0.9406(3) 0.0140(3) 0.0452(9) Uani 1 1 d . . .
H20A H -0.0956 1.0107 -0.0186 0.068 Uiso 1 1 calc R . .
H20B H -0.0380 0.9290 0.0293 0.068 Uiso 1 1 calc R . .
H20C H -0.1047 0.9464 0.0652 0.068 Uiso 1 1 calc R . .
C21 C -0.19359(18) 0.8496(4) -0.0573(3) 0.0519(10) Uani 1 1 d . . .
H21A H -0.2098 0.8543 -0.0044 0.078 Uiso 1 1 calc R . .
H21B H -0.2123 0.7821 -0.0885 0.078 Uiso 1 1 calc R . .
H21C H -0.2074 0.9173 -0.0912 0.078 Uiso 1 1 calc R . .
N22 N 0.32671(12) 0.5893(2) 0.10638(16) 0.0256(5) Uani 1 1 d . B .
C23 C 0.36438(15) 0.5116(3) 0.0781(2) 0.0286(6) Uani 1 1 d . . .
C24 C 0.43141(17) 0.4994(3) 0.1082(2) 0.0381(8) Uani 1 1 d . B .
H24 H 0.4567 0.4434 0.0864 0.046 Uiso 1 1 calc R . .
C25 C 0.46107(17) 0.5730(4) 0.1727(2) 0.0436(9) Uani 1 1 d D . .
C26 C 0.42294(16) 0.6546(4) 0.2030(2) 0.0389(8) Uani 1 1 d . B .
H26 H 0.4420 0.7048 0.2470 0.047 Uiso 1 1 calc R . .
C27 C 0.35637(15) 0.6592(3) 0.16646(19) 0.0280(6) Uani 1 1 d . . .
N28 N 0.32763(13) 0.4467(2) 0.01137(17) 0.0293(5) Uani 1 1 d . . .
N29 N 0.26190(12) 0.4715(2) -0.01641(16) 0.0278(5) Uani 1 1 d . . .
C30 C 0.24220(18) 0.4073(3) -0.0833(2) 0.0345(7) Uani 1 1 d . . .
H30 H 0.1983 0.4065 -0.1160 0.041 Uiso 1 1 calc R . .
C31 C 0.2945(2) 0.3408(4) -0.0996(3) 0.0454(9) Uani 1 1 d . . .
H31 H 0.2932 0.2875 -0.1438 0.055 Uiso 1 1 calc R . .
C32 C 0.34820(19) 0.3688(4) -0.0384(3) 0.0430(8) Uani 1 1 d . . .
H32 H 0.3919 0.3388 -0.0321 0.052 Uiso 1 1 calc R . .
N33 N 0.31221(13) 0.7410(2) 0.18744(17) 0.0323(6) Uani 1 1 d . B .
N34 N 0.24746(13) 0.7388(2) 0.14627(17) 0.0293(5) Uani 1 1 d . . .
C35 C 0.21974(18) 0.8283(3) 0.1749(2) 0.0382(8) Uani 1 1 d . B .
H35 H 0.1743 0.8490 0.1575 0.046 Uiso 1 1 calc R . .
C36 C 0.2656(2) 0.8881(4) 0.2334(3) 0.0505(10) Uani 1 1 d . . .
H36 H 0.2578 0.9548 0.2628 0.061 Uiso 1 1 calc R B .
C37 C 0.3241(2) 0.8309(4) 0.2397(3) 0.0490(10) Uani 1 1 d . B .
H37 H 0.3655 0.8507 0.2745 0.059 Uiso 1 1 calc R . .
S38A S 0.54829(5) 0.56565(17) 0.20669(9) 0.0389(3) Uani 0.67 1 d PD A .
C39A C 0.5699(6) 0.6976(11) 0.2680(8) 0.049(4) Uiso 0.34 1 d PD A 1
H39A H 0.5402 0.7067 0.3096 0.058 Uiso 0.34 1 calc PR A 1
C40A C 0.5650(6) 0.8040(10) 0.2109(7) 0.049(3) Uiso 0.34 1 d PD A 1
H40A H 0.5184 0.8168 0.1839 0.074 Uiso 0.34 1 calc PR A 1
H40B H 0.5917 0.7923 0.1676 0.074 Uiso 0.34 1 calc PR A 1
H40C H 0.5820 0.8701 0.2451 0.074 Uiso 0.34 1 calc PR A 1
C41A C 0.6420(5) 0.6889(10) 0.3141(7) 0.039(2) Uiso 0.34 1 d PD A 1
H41A H 0.6474 0.6222 0.3507 0.059 Uiso 0.34 1 calc PR A 1
H41B H 0.6541 0.7571 0.3481 0.059 Uiso 0.34 1 calc PR A 1
H41C H 0.6711 0.6819 0.2730 0.059 Uiso 0.34 1 calc PR A 1
C39B C 0.5677(6) 0.6367(13) 0.3049(7) 0.039(4) Uiso 0.33 1 d PD A 2
H39B H 0.5494 0.7154 0.3009 0.047 Uiso 0.33 1 calc PR A 2
C40B C 0.5392(6) 0.5634(11) 0.3722(8) 0.051(3) Uiso 0.33 1 d PD A 2
H40D H 0.4904 0.5665 0.3595 0.076 Uiso 0.33 1 calc PR A 2
H40E H 0.5558 0.5939 0.4287 0.076 Uiso 0.33 1 calc PR A 2
H40F H 0.5538 0.4847 0.3698 0.076 Uiso 0.33 1 calc PR A 2
C41B C 0.6416(5) 0.6364(11) 0.3326(7) 0.040(2) Uiso 0.33 1 d PD A 2
H41D H 0.6560 0.5634 0.3587 0.060 Uiso 0.33 1 calc PR A 2
H41E H 0.6549 0.6973 0.3735 0.060 Uiso 0.33 1 calc PR A 2
H41F H 0.6623 0.6483 0.2838 0.060 Uiso 0.33 1 calc PR A 2
S38C S 0.5396(2) 0.5126(4) 0.2213(3) 0.0536(10) Uiso 0.33 1 d PD B 3
C39C C 0.5639(6) 0.6086(11) 0.3122(7) 0.034(3) Uiso 0.33 1 d PD B 3
H39C H 0.5267 0.6143 0.3438 0.041 Uiso 0.33 1 calc PR B 3
C40C C 0.5773(10) 0.7260(14) 0.2770(12) 0.063(5) Uiso 0.33 1 d PD B 3
H40G H 0.5353 0.7579 0.2460 0.095 Uiso 0.33 1 calc PR B 3
H40H H 0.6087 0.7181 0.2390 0.095 Uiso 0.33 1 calc PR B 3
H40I H 0.5962 0.7765 0.3235 0.095 Uiso 0.33 1 calc PR B 3
C41C C 0.6227(9) 0.5585(16) 0.3667(12) 0.087(5) Uiso 0.33 1 d PD B 3
H41G H 0.6135 0.4792 0.3781 0.131 Uiso 0.33 1 calc PR B 3
H41H H 0.6330 0.6005 0.4198 0.131 Uiso 0.33 1 calc PR B 3
H41I H 0.6607 0.5625 0.3384 0.131 Uiso 0.33 1 calc PR B 3
Cl42A Cl 0.43407(16) 0.7588(3) 0.4576(2) 0.0429(10) Uiso 0.50 1 d PD C 1
O43A O 0.5028(5) 0.7718(10) 0.4769(8) 0.116(4) Uiso 0.50 1 d PD C 1
O44A O 0.4090(5) 0.8742(6) 0.4297(5) 0.070(2) Uiso 0.50 1 d PD C 1
O45A O 0.4048(4) 0.7235(8) 0.5240(5) 0.056(2) Uiso 0.50 1 d PD C 1
O46A O 0.4136(5) 0.6848(7) 0.3890(5) 0.073(2) Uiso 0.50 1 d PD C 1
Cl42B Cl 0.4307(2) 0.7770(4) 0.4627(3) 0.0350(14) Uiso 0.30 1 d PD D 2
O43B O 0.4931(4) 0.8175(7) 0.5105(5) 0.0394(18) Uiso 0.30 1 d PD D 2
O44B O 0.3800(5) 0.8522(9) 0.4388(6) 0.039(3) Uiso 0.30 1 d PD D 2
O45B O 0.4094(8) 0.6957(13) 0.5211(9) 0.073(6) Uiso 0.30 1 d PD D 2
O46B O 0.4478(6) 0.7067(9) 0.3957(6) 0.055(2) Uiso 0.30 1 d PD D 2
Cl42C Cl 0.4200(2) 0.7835(4) 0.4268(3) 0.0294(8) Uiso 0.20 1 d PD E 3
O43C O 0.4693(6) 0.8102(11) 0.3798(8) 0.047(3) Uiso 0.20 1 d PD E 3
O44C O 0.4488(8) 0.7537(14) 0.5122(8) 0.067(4) Uiso 0.20 1 d PD E 3
O45C O 0.3845(6) 0.6895(8) 0.3839(6) 0.028(2) Uiso 0.20 1 d PD E 3
O46C O 0.3780(6) 0.8790(10) 0.4259(8) 0.022(3) Uiso 0.20 1 d PD E 3
Cl47 Cl 0.07576(4) 0.99764(8) 0.23168(5) 0.0384(2) Uani 1 1 d . . .
O48 O 0.13922(14) 1.0485(3) 0.2323(2) 0.0540(7) Uani 1 1 d . . .
O49 O 0.02435(16) 1.0808(3) 0.2105(2) 0.0671(10) Uani 1 1 d . . .
O50 O 0.07424(16) 0.9536(3) 0.31325(18) 0.0554(8) Uani 1 1 d . . .
O51 O 0.06542(16) 0.9079(3) 0.1713(2) 0.0681(10) Uani 1 1 d . . .
O52A O 0.6967(8) 0.5606(17) 0.6081(11) 0.047(4) Uiso 0.15 1 d PD F 1
C53A C 0.6364(11) 0.558(6) 0.5999(16) 0.098(18) Uiso 0.15 1 d PD F 1
C54A C 0.6071(13) 0.596(3) 0.6752(13) 0.050(7) Uiso 0.15 1 d PD F 1
H54A H 0.6424 0.5982 0.7258 0.075 Uiso 0.15 1 calc PR F 1
H54B H 0.5723 0.5432 0.6836 0.075 Uiso 0.15 1 calc PR F 1
H54C H 0.5879 0.6722 0.6644 0.075 Uiso 0.15 1 calc PR F 1
C55A C 0.5941(8) 0.5470(16) 0.5137(9) 0.022(4) Uiso 0.15 1 d PD F 1
H55A H 0.6215 0.5206 0.4745 0.034 Uiso 0.15 1 calc PR F 1
H55B H 0.5746 0.6207 0.4951 0.034 Uiso 0.15 1 calc PR F 1
H55C H 0.5583 0.4923 0.5152 0.034 Uiso 0.15 1 calc PR F 1
O52B O 0.6595(9) 0.5505(17) 0.7003(9) 0.091(5) Uiso 0.25 1 d PD G 2
C53B C 0.6338(8) 0.549(2) 0.6262(11) 0.058(5) Uiso 0.25 1 d PD G 2
C54B C 0.6692(6) 0.5297(12) 0.5537(8) 0.032(3) Uiso 0.25 1 d PD G 2
H54D H 0.7164 0.5142 0.5758 0.048 Uiso 0.25 1 calc PR G 2
H54E H 0.6650 0.5974 0.5180 0.048 Uiso 0.25 1 calc PR G 2
H54F H 0.6490 0.4649 0.5203 0.048 Uiso 0.25 1 calc PR G 2
C55B C 0.5594(7) 0.575(2) 0.5999(13) 0.067(5) Uiso 0.25 1 d PD G 2
H55D H 0.5405 0.5869 0.6502 0.100 Uiso 0.25 1 calc PR G 2
H55E H 0.5369 0.5103 0.5679 0.100 Uiso 0.25 1 calc PR G 2
H55F H 0.5530 0.6427 0.5647 0.100 Uiso 0.25 1 calc PR G 2
O52C O 0.6454(7) 0.6150(12) 0.7299(8) 0.079(4) Uiso 0.30 1 d PD H 3
C53C C 0.6239(8) 0.5802(18) 0.6558(11) 0.066(5) Uiso 0.30 1 d PD H 3
C54C C 0.6686(11) 0.538(2) 0.6026(13) 0.083(6) Uiso 0.30 1 d PD H 3
H54G H 0.7148 0.5432 0.6332 0.125 Uiso 0.30 1 calc PR H 3
H54H H 0.6631 0.5836 0.5512 0.125 Uiso 0.30 1 calc PR H 3
H54I H 0.6578 0.4588 0.5877 0.125 Uiso 0.30 1 calc PR H 3
C55C C 0.5480(8) 0.585(2) 0.6307(14) 0.087(6) Uiso 0.30 1 d PD H 3
H55G H 0.5296 0.6154 0.6774 0.131 Uiso 0.30 1 calc PR H 3
H55H H 0.5306 0.5082 0.6173 0.131 Uiso 0.30 1 calc PR H 3
H55I H 0.5351 0.6334 0.5811 0.131 Uiso 0.30 1 calc PR H 3


_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 N22 2.121(2) . ?
Fe1 N2 2.133(2) . ?
Fe1 N9 2.172(3) . ?
Fe1 N29 2.175(3) . ?
Fe1 N34 2.176(3) . ?
Fe1 N14 2.210(3) . ?
N2 C3 1.332(4) . ?
N2 C7 1.335(4) . ?
C3 C4 1.383(4) . ?
C3 N8 1.408(4) . ?
C4 C5 1.397(4) . ?
C4 H4 0.9500 . ?
C5 C6 1.402(4) . ?
C5 S18 1.748(3) . ?
C6 C7 1.371(4) . ?
C6 H6 0.9500 . ?
C7 N13 1.408(4) . ?
N8 C12 1.357(4) . ?
N8 N9 1.364(3) . ?
N9 C10 1.315(5) . ?
C10 C11 1.400(5) . ?
C10 H10 0.9500 . ?
C11 C12 1.362(5) . ?
C11 H11 0.9500 . ?
C12 H12 0.9500 . ?
N13 C17 1.360(4) . ?
N13 N14 1.370(4) . ?
N14 C15 1.322(4) . ?
C15 C16 1.404(6) . ?
C15 H15 0.9500 . ?
C16 C17 1.368(5) . ?
C16 H16 0.9500 . ?
C17 H17 0.9500 . ?
S18 C19 1.827(3) . ?
C19 C20 1.511(5) . ?
C19 C21 1.522(4) . ?
C19 H19 1.0000 . ?
C20 H20A 0.9800 . ?
C20 H20B 0.9800 . ?
C20 H20C 0.9800 . ?
C21 H21A 0.9800 . ?
C21 H21B 0.9800 . ?
C21 H21C 0.9800 . ?
N22 C27 1.329(4) . ?
N22 C23 1.337(4) . ?
C23 C24 1.371(4) . ?
C23 N28 1.415(4) . ?
C24 C25 1.402(5) . ?
C24 H24 0.9500 . ?
C25 C26 1.390(5) . ?
C25 S38A 1.764(3) . ?
C25 S38C 1.793(5) . ?
C26 C27 1.376(4) . ?
C26 H26 0.9500 . ?
C27 N33 1.410(4) . ?
N28 C32 1.345(4) . ?
N28 N29 1.364(4) . ?
N29 C30 1.319(4) . ?
C30 C31 1.395(5) . ?
C30 H30 0.9500 . ?
C31 C32 1.368(6) . ?
C31 H31 0.9500 . ?
C32 H32 0.9500 . ?
N33 C37 1.351(5) . ?
N33 N34 1.362(4) . ?
N34 C35 1.326(4) . ?
C35 C36 1.388(5) . ?
C35 H35 0.9500 . ?
C36 C37 1.362(6) . ?
C36 H36 0.9500 . ?
C37 H37 0.9500 . ?
S38A C39B 1.774(11) . ?
S38A C39A 1.854(12) . ?
C39A C41A 1.521(13) . ?
C39A C40A 1.552(14) . ?
C39A H39A 1.0000 . ?
C40A H40A 0.9800 . ?
C40A H40B 0.9800 . ?
C40A H40C 0.9800 . ?
C41A H41A 0.9800 . ?
C41A H41B 0.9800 . ?
C41A H41C 0.9800 . ?
C39B C41B 1.491(13) . ?
C39B C40B 1.591(15) . ?
C39B H39B 1.0000 . ?
C40B H40D 0.9800 . ?
C40B H40E 0.9800 . ?
C40B H40F 0.9800 . ?
C41B H41D 0.9800 . ?
C41B H41E 0.9800 . ?
C41B H41F 0.9800 . ?
S38C C39C 1.847(11) . ?
C39C C41C 1.468(15) . ?
C39C C40C 1.545(15) . ?
C39C H39C 1.0000 . ?
C40C H40G 0.9800 . ?
C40C H40H 0.9800 . ?
C40C H40I 0.9800 . ?
C41C H41G 0.9800 . ?
C41C H41H 0.9800 . ?
C41C H41I 0.9800 . ?
Cl42A O43A 1.389(10) . ?
Cl42A O45A 1.397(7) . ?
Cl42A O46A 1.411(8) . ?
Cl42A O44A 1.494(8) . ?
Cl42B O44B 1.364(10) . ?
Cl42B O43B 1.438(9) . ?
Cl42B O46B 1.463(9) . ?
Cl42B O45B 1.474(11) . ?
Cl42C O43C 1.416(11) . ?
Cl42C O46C 1.417(11) . ?
Cl42C O45C 1.431(10) . ?
Cl42C O44C 1.436(12) . ?
Cl47 O50 1.427(3) . ?
Cl47 O51 1.430(3) . ?
Cl47 O48 1.430(3) . ?
Cl47 O49 1.431(3) . ?
O52A C53A 1.217(18) . ?
C53A C55A 1.497(18) . ?
C53A C54A 1.531(18) . ?
C54A H54A 0.9800 . ?
C54A H54B 0.9800 . ?
C54A H54C 0.9800 . ?
C55A H55A 0.9800 . ?
C55A H55B 0.9800 . ?
C55A H55C 0.9800 . ?
O52B C53B 1.213(16) . ?
C53B C54B 1.515(16) . ?
C53B C55B 1.529(16) . ?
C54B H54D 0.9800 . ?
C54B H54E 0.9800 . ?
C54B H54F 0.9800 . ?
C55B H55D 0.9800 . ?
C55B H55E 0.9800 . ?
C55B H55F 0.9800 . ?
O52C C53C 1.263(15) . ?
C53C C54C 1.464(16) . ?
C53C C55C 1.527(15) . ?
C54C H54G 0.9800 . ?
C54C H54H 0.9800 . ?
C54C H54I 0.9800 . ?
C55C H55G 0.9800 . ?
C55C H55H 0.9800 . ?
C55C H55I 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
N22 Fe1 N2 166.76(10) . . ?
N22 Fe1 N9 114.09(10) . . ?
N2 Fe1 N9 73.07(10) . . ?
N22 Fe1 N29 73.51(10) . . ?
N2 Fe1 N29 118.24(10) . . ?
N9 Fe1 N29 93.01(11) . . ?
N22 Fe1 N34 73.33(10) . . ?
N2 Fe1 N34 95.57(10) . . ?
N9 Fe1 N34 93.76(11) . . ?
N29 Fe1 N34 146.02(10) . . ?
N22 Fe1 N14 100.11(10) . . ?
N2 Fe1 N14 73.05(10) . . ?
N9 Fe1 N14 145.75(10) . . ?
N29 Fe1 N14 98.51(10) . . ?
N34 Fe1 N14 94.36(11) . . ?
C3 N2 C7 117.9(2) . . ?
C3 N2 Fe1 120.63(19) . . ?
C7 N2 Fe1 120.89(19) . . ?
N2 C3 C4 124.1(3) . . ?
N2 C3 N8 112.4(2) . . ?
C4 C3 N8 123.4(3) . . ?
C3 C4 C5 116.7(3) . . ?
C3 C4 H4 121.7 . . ?
C5 C4 H4 121.7 . . ?
C4 C5 C6 120.1(3) . . ?
C4 C5 S18 125.0(2) . . ?
C6 C5 S18 114.8(2) . . ?
C7 C6 C5 117.4(3) . . ?
C7 C6 H6 121.3 . . ?
C5 C6 H6 121.3 . . ?
N2 C7 C6 123.9(3) . . ?
N2 C7 N13 113.0(3) . . ?
C6 C7 N13 123.2(3) . . ?
C12 N8 N9 111.3(2) . . ?
C12 N8 C3 130.5(2) . . ?
N9 N8 C3 118.2(2) . . ?
C10 N9 N8 105.1(3) . . ?
C10 N9 Fe1 139.9(2) . . ?
N8 N9 Fe1 114.98(19) . . ?
N9 C10 C11 111.4(3) . . ?
N9 C10 H10 124.3 . . ?
C11 C10 H10 124.3 . . ?
C12 C11 C10 105.4(3) . . ?
C12 C11 H11 127.3 . . ?
C10 C11 H11 127.3 . . ?
N8 C12 C11 106.7(3) . . ?
N8 C12 H12 126.6 . . ?
C11 C12 H12 126.6 . . ?
C17 N13 N14 111.6(3) . . ?
C17 N13 C7 129.8(3) . . ?
N14 N13 C7 118.5(3) . . ?
C15 N14 N13 104.5(3) . . ?
C15 N14 Fe1 141.3(2) . . ?
N13 N14 Fe1 114.02(19) . . ?
N14 C15 C16 112.0(3) . . ?
N14 C15 H15 124.0 . . ?
C16 C15 H15 124.0 . . ?
C17 C16 C15 105.1(3) . . ?
C17 C16 H16 127.4 . . ?
C15 C16 H16 127.4 . . ?
N13 C17 C16 106.8(3) . . ?
N13 C17 H17 126.6 . . ?
C16 C17 H17 126.6 . . ?
C5 S18 C19 105.42(15) . . ?
C20 C19 C21 112.0(3) . . ?
C20 C19 S18 110.7(3) . . ?
C21 C19 S18 105.2(3) . . ?
C20 C19 H19 109.6 . . ?
C21 C19 H19 109.6 . . ?
S18 C19 H19 109.6 . . ?
C19 C20 H20A 109.5 . . ?
C19 C20 H20B 109.5 . . ?
H20A C20 H20B 109.5 . . ?
C19 C20 H20C 109.5 . . ?
H20A C20 H20C 109.5 . . ?
H20B C20 H20C 109.5 . . ?
C19 C21 H21A 109.5 . . ?
C19 C21 H21B 109.5 . . ?
H21A C21 H21B 109.5 . . ?
C19 C21 H21C 109.5 . . ?
H21A C21 H21C 109.5 . . ?
H21B C21 H21C 109.5 . . ?
C27 N22 C23 117.8(3) . . ?
C27 N22 Fe1 121.2(2) . . ?
C23 N22 Fe1 121.0(2) . . ?
N22 C23 C24 123.8(3) . . ?
N22 C23 N28 112.2(3) . . ?
C24 C23 N28 124.0(3) . . ?
C23 C24 C25 117.1(3) . . ?
C23 C24 H24 121.4 . . ?
C25 C24 H24 121.4 . . ?
C26 C25 C24 120.2(3) . . ?
C26 C25 S38A 121.9(3) . . ?
C24 C25 S38A 117.7(3) . . ?
C26 C25 S38C 129.7(3) . . ?
C24 C25 S38C 107.4(3) . . ?
C27 C26 C25 117.0(3) . . ?
C27 C26 H26 121.5 . . ?
C25 C26 H26 121.5 . . ?
N22 C27 C26 124.1(3) . . ?
N22 C27 N33 112.4(3) . . ?
C26 C27 N33 123.5(3) . . ?
C32 N28 N29 110.8(3) . . ?
C32 N28 C23 130.3(3) . . ?
N29 N28 C23 118.5(2) . . ?
C30 N29 N28 105.6(3) . . ?
C30 N29 Fe1 139.8(2) . . ?
N28 N29 Fe1 114.53(19) . . ?
N29 C30 C31 111.0(3) . . ?
N29 C30 H30 124.5 . . ?
C31 C30 H30 124.5 . . ?
C32 C31 C30 105.3(3) . . ?
C32 C31 H31 127.4 . . ?
C30 C31 H31 127.4 . . ?
N28 C32 C31 107.3(3) . . ?
N28 C32 H32 126.3 . . ?
C31 C32 H32 126.3 . . ?
C37 N33 N34 111.1(3) . . ?
C37 N33 C27 130.2(3) . . ?
N34 N33 C27 118.6(3) . . ?
C35 N34 N33 104.9(3) . . ?
C35 N34 Fe1 140.6(2) . . ?
N33 N34 Fe1 114.48(19) . . ?
N34 C35 C36 111.5(3) . . ?
N34 C35 H35 124.3 . . ?
C36 C35 H35 124.3 . . ?
C37 C36 C35 105.4(3) . . ?
C37 C36 H36 127.3 . . ?
C35 C36 H36 127.3 . . ?
N33 C37 C36 107.2(3) . . ?
N33 C37 H37 126.4 . . ?
C36 C37 H37 126.4 . . ?
C25 S38A C39B 106.9(4) . . ?
C25 S38A C39A 104.2(4) . . ?
C41A C39A C40A 106.8(10) . . ?
C41A C39A S38A 108.2(9) . . ?
C40A C39A S38A 112.4(9) . . ?
C41A C39A H39A 109.8 . . ?
C40A C39A H39A 109.8 . . ?
S38A C39A H39A 109.8 . . ?
C39A C40A H40A 109.5 . . ?
C39A C40A H40B 109.5 . . ?
H40A C40A H40B 109.5 . . ?
C39A C40A H40C 109.5 . . ?
H40A C40A H40C 109.5 . . ?
H40B C40A H40C 109.5 . . ?
C39A C41A H41A 109.5 . . ?
C39A C41A H41B 109.5 . . ?
H41A C41A H41B 109.5 . . ?
C39A C41A H41C 109.5 . . ?
H41A C41A H41C 109.5 . . ?
H41B C41A H41C 109.5 . . ?
C41B C39B C40B 106.3(10) . . ?
C41B C39B S38A 107.6(8) . . ?
C40B C39B S38A 108.1(9) . . ?
C41B C39B H39B 111.5 . . ?
C40B C39B H39B 111.5 . . ?
S38A C39B H39B 111.5 . . ?
C39B C40B H40D 109.5 . . ?
C39B C40B H40E 109.5 . . ?
H40D C40B H40E 109.5 . . ?
C39B C40B H40F 109.5 . . ?
H40D C40B H40F 109.5 . . ?
H40E C40B H40F 109.5 . . ?
C39B C41B H41D 109.5 . . ?
C39B C41B H41E 109.5 . . ?
H41D C41B H41E 109.5 . . ?
C39B C41B H41F 109.5 . . ?
H41D C41B H41F 109.5 . . ?
H41E C41B H41F 109.5 . . ?
C25 S38C C39C 100.6(4) . . ?
C41C C39C C40C 113.5(12) . . ?
C41C C39C S38C 107.0(11) . . ?
C40C C39C S38C 107.1(11) . . ?
C41C C39C H39C 109.7 . . ?
C40C C39C H39C 109.7 . . ?
S38C C39C H39C 109.7 . . ?
C39C C40C H40G 109.5 . . ?
C39C C40C H40H 109.5 . . ?
H40G C40C H40H 109.5 . . ?
C39C C40C H40I 109.5 . . ?
H40G C40C H40I 109.5 . . ?
H40H C40C H40I 109.5 . . ?
C39C C41C H41G 109.5 . . ?
C39C C41C H41H 109.5 . . ?
H41G C41C H41H 109.5 . . ?
C39C C41C H41I 109.5 . . ?
H41G C41C H41I 109.5 . . ?
H41H C41C H41I 109.5 . . ?
O43A Cl42A O45A 115.5(6) . . ?
O43A Cl42A O46A 112.1(7) . . ?
O45A Cl42A O46A 108.5(6) . . ?
O43A Cl42A O44A 103.8(6) . . ?
O45A Cl42A O44A 109.3(6) . . ?
O46A Cl42A O44A 107.2(5) . . ?
O44B Cl42B O43B 118.9(7) . . ?
O44B Cl42B O46B 116.1(7) . . ?
O43B Cl42B O46B 105.8(6) . . ?
O44B Cl42B O45B 107.5(8) . . ?
O43B Cl42B O45B 102.4(8) . . ?
O46B Cl42B O45B 104.5(8) . . ?
O43C Cl42C O46C 108.2(8) . . ?
O43C Cl42C O45C 105.1(7) . . ?
O46C Cl42C O45C 111.3(7) . . ?
O43C Cl42C O44C 111.9(9) . . ?
O46C Cl42C O44C 109.7(8) . . ?
O45C Cl42C O44C 110.5(8) . . ?
O50 Cl47 O51 109.7(2) . . ?
O50 Cl47 O48 109.45(19) . . ?
O51 Cl47 O48 109.1(2) . . ?
O50 Cl47 O49 108.78(19) . . ?
O51 Cl47 O49 110.1(2) . . ?
O48 Cl47 O49 109.8(2) . . ?
O52A C53A C55A 119.5(18) . . ?
O52A C53A C54A 117.2(18) . . ?
C55A C53A C54A 121.6(17) . . ?
C53A C54A H54A 109.5 . . ?
C53A C54A H54B 109.5 . . ?
H54A C54A H54B 109.5 . . ?
C53A C54A H54C 109.5 . . ?
H54A C54A H54C 109.5 . . ?
H54B C54A H54C 109.5 . . ?
C53A C55A H55A 109.5 . . ?
C53A C55A H55B 109.5 . . ?
H55A C55A H55B 109.5 . . ?
C53A C55A H55C 109.5 . . ?
H55A C55A H55C 109.5 . . ?
H55B C55A H55C 109.5 . . ?
O52B C53B C54B 126.1(14) . . ?
O52B C53B C55B 119.2(15) . . ?
C54B C53B C55B 114.6(13) . . ?
C53B C54B H54D 109.5 . . ?
C53B C54B H54E 109.5 . . ?
H54D C54B H54E 109.5 . . ?
C53B C54B H54F 109.5 . . ?
H54D C54B H54F 109.5 . . ?
H54E C54B H54F 109.5 . . ?
C53B C55B H55D 109.5 . . ?
C53B C55B H55E 109.5 . . ?
H55D C55B H55E 109.5 . . ?
C53B C55B H55F 109.5 . . ?
H55D C55B H55F 109.5 . . ?
H55E C55B H55F 109.5 . . ?
O52C C53C C54C 121.9(14) . . ?
O52C C53C C55C 112.9(14) . . ?
C54C C53C C55C 125.2(14) . . ?
C53C C54C H54G 109.5 . . ?
C53C C54C H54H 109.5 . . ?
H54G C54C H54H 109.5 . . ?
C53C C54C H54I 109.5 . . ?
H54G C54C H54I 109.5 . . ?
H54H C54C H54I 109.5 . . ?
C53C C55C H55G 109.5 . . ?
C53C C55C H55H 109.5 . . ?
H55G C55C H55H 109.5 . . ?
C53C C55C H55I 109.5 . . ?
H55G C55C H55I 109.5 . . ?
H55H C55C H55I 109.5 . . ?

_diffrn_measured_fraction_theta_max 0.977
_diffrn_reflns_theta_full        72.00
_diffrn_measured_fraction_theta_full 0.989
_refine_diff_density_max         1.218
_refine_diff_density_min         -0.820
_refine_diff_density_rms         0.088
_exptl_crystal_recrystallization_method 
'Re-crystallisation from solvent: Acetone-diethyl ether'
_exptl_crystal_preparation       'Magnetic properties'
####################################################################### 
# 
# This file contains crystal structure data downloaded from the 
# Cambridge Structural Database (CSD) hosted by the Cambridge 
# Crystallographic Data Centre (CCDC).
# 
# Full information about CCDC data access policies and citation 
# guidelines are available at http://www.ccdc.cam.ac.uk/access/V1 
# 
# Audit and citation data items may have been added by the CCDC. 
# Please retain this information to preserve the provenance of 
# this file and to allow appropriate attribution of the data. 
# 
#######################################################################

data_rk137H2OPI_020K
_database_code_depnum_ccdc_archive 'CCDC 1564666'
_audit_update_record             
;
2017-07-28 deposited with the CCDC.
2017-11-20 downloaded from the CCDC.
;
_chemical_name_common            ?
_chemical_name_systematic        ?
_chemical_formula_moiety         'C28 H30 Fe N10 S2, 2(B F4), H2 O'
_chemical_formula_sum            'C28 H32 B2 F8 Fe N10 O S2'
_chemical_formula_weight         818.22
_chemical_melting_point          'not measured'
loop_
_atom_type_symbol
_atom_type_description
_atom_type_scat_dispersion_real
_atom_type_scat_dispersion_imag
_atom_type_scat_source
C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
B B 0.0013 0.0007 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
F F 0.0171 0.0103 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Fe Fe 0.3463 0.8444 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
S S 0.1246 0.1234 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'

_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.
;
_space_group_crystal_system      monoclinic
_space_group_IT_number           14
_space_group_name_H-M_alt        'P 1 21/c 1'
_space_group_name_Hall           '-P 2ybc'
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                   20.2276(5)
_cell_length_b                   11.8791(3)
_cell_length_c                   15.0082(4)
_cell_angle_alpha                90
_cell_angle_beta                 102.531(2)
_cell_angle_gamma                90
_cell_volume                     3520.35(16)
_cell_formula_units_Z            4
_cell_measurement_reflns_used    6163
_cell_measurement_temperature    20
_cell_measurement_theta_max      31.0630
_cell_measurement_theta_min      3.2620
_exptl_absorpt_coefficient_mu    0.631
_exptl_absorpt_correction_T_max  0.951
_exptl_absorpt_correction_T_min  0.917
_exptl_absorpt_correction_type   analytical
_exptl_absorpt_process_details   
;
CrysAlisPro 1.171.38.41 (Rigaku Oxford Diffraction, 2015)
Analytical numeric absorption correction using a multifaceted crystal
			model based on expressions derived by R.C. Clark & J.S. Reid.
(Clark, R. C. & Reid, J. S. (1995). Acta Cryst. A51, 887-897)
Empirical absorption correction using spherical harmonics,
 implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_absorpt_special_details   ?
_exptl_crystal_colour            'light orange'
_exptl_crystal_density_diffrn    1.544
_exptl_crystal_density_meas      'not measured'
_exptl_crystal_density_method    none
_exptl_crystal_description       block
_exptl_crystal_F_000             1672
loop_
_exptl_crystal_face_index_h
_exptl_crystal_face_index_k
_exptl_crystal_face_index_l
_exptl_crystal_face_perp_dist
-19 13 -1 0.0697
-18 -13 1 0.0368
-2 -5 20 0.0806
-10 -6 19 0.0746
18 13 0 0.0633
14 12 -13 0.0625
20 -12 -1 0.0323
-8 -3 -18 0.0897

_exptl_crystal_size_max          0.225
_exptl_crystal_size_mid          0.111
_exptl_crystal_size_min          0.101
loop_
_exptl_oxdiff_crystal_face_indexfrac_h
_exptl_oxdiff_crystal_face_indexfrac_k
_exptl_oxdiff_crystal_face_indexfrac_l
_exptl_oxdiff_crystal_face_x
_exptl_oxdiff_crystal_face_y
_exptl_oxdiff_crystal_face_z
-18.5549 12.5638 -1.0576 -0.9489 0.0211 -0.3518
-17.9856 -12.8814 0.8719 -0.0265 -0.8969 0.4407
-1.9499 -4.8695 19.9307 0.0315 0.2746 0.9568
-10.0465 -5.9210 18.8893 -0.1447 0.0172 0.9631
17.9841 12.8835 0.1258 0.0218 0.9224 -0.3999
13.9655 11.8419 -12.8673 0.0101 0.4566 -0.8925
19.5509 -11.5804 -0.9301 0.9495 -0.0105 0.2405
-8.0272 -3.0451 -18.0072 -0.0251 -0.7651 -0.6318

_exptl_transmission_factor_max   ?
_exptl_transmission_factor_min   ?
_diffrn_reflns_av_R_equivalents  0.0837
_diffrn_reflns_av_unetI/netI     0.0810
_diffrn_reflns_Laue_measured_fraction_full 0.998
_diffrn_reflns_Laue_measured_fraction_max 0.999
_diffrn_reflns_limit_h_max       25
_diffrn_reflns_limit_h_min       -25
_diffrn_reflns_limit_k_max       14
_diffrn_reflns_limit_k_min       -15
_diffrn_reflns_limit_l_max       19
_diffrn_reflns_limit_l_min       -16
_diffrn_reflns_number            36302
_diffrn_reflns_point_group_measured_fraction_full 0.998
_diffrn_reflns_point_group_measured_fraction_max 0.999
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         26.998
_diffrn_reflns_theta_min         3.082
_diffrn_ambient_temperature      20.0
_diffrn_detector                 'CCD plate'
_diffrn_detector_area_resol_mean 16.1852
_diffrn_detector_type            Sapphire3
_diffrn_measured_fraction_theta_full 0.998
_diffrn_measured_fraction_theta_max 0.999
_diffrn_measurement_details      
;
List of Runs (angles in degrees, time in seconds):

  # Type    Start    End  Width  tₑₓₚ   ω     θ     κ     φ   Frames
#--------------------------------------------------------------------------
  1  ω      0.00  38.00   1.00    7.50    --  -33.81   0.00  90.00   38
  2  ω    -55.00 -11.00   1.00    7.50    --  -33.81  38.00 150.00   44
  3  ω    -73.00 -29.00   1.00    7.50    --  -33.81 -38.00 -30.00   44
  4  ω     58.00 109.00   1.00    7.50    --   35.69 178.00 -30.00   51
  5  ω     57.00 107.00   1.00    7.50    --   35.69 178.00-120.00   50
  6  ω   -109.00 -33.00   1.00    7.50    --  -33.81   0.00  90.00   76
  7  ω      0.00  38.00   1.00    7.50    --  -33.81   0.00  90.00   38
  8  ω    -55.00 -11.00   1.00    7.50    --  -33.81  38.00 150.00   44
  9  ω    -73.00 -29.00   1.00    7.50    --  -33.81 -38.00 -30.00   44
 10  ω     58.00 109.00   1.00    7.50    --   35.69 178.00 -30.00   51
 11  ω     57.00 107.00   1.00    7.50    --   35.69 178.00-120.00   50
 12  ω   -109.00 -33.00   1.00    7.50    --  -33.81   0.00  90.00   76
;
_diffrn_measurement_device       'four-circle diffractometer'
_diffrn_measurement_device_type  'Xcalibur, Sapphire3'
_diffrn_measurement_method       'ω scans'
_diffrn_orient_matrix_type       
'CrysAlisPro convention (1999,Acta A55,543-557)'
_diffrn_orient_matrix_UB_11      0.0270299000
_diffrn_orient_matrix_UB_12      -0.0359913000
_diffrn_orient_matrix_UB_13      -0.0045677000
_diffrn_orient_matrix_UB_21      0.0235032000
_diffrn_orient_matrix_UB_22      0.0385384000
_diffrn_orient_matrix_UB_23      0.0254935000
_diffrn_orient_matrix_UB_31      -0.0023965000
_diffrn_orient_matrix_UB_32      -0.0280961000
_diffrn_orient_matrix_UB_33      0.0409061000
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_source                   'fine-focus sealed X-ray tube'
_diffrn_source_type              'Enhance (Mo) X-ray Source'
_reflns_Friedel_coverage         0.000
_reflns_Friedel_fraction_full    .
_reflns_Friedel_fraction_max     .
_reflns_number_gt                5325
_reflns_number_total             7685
_reflns_odcompleteness_completeness 99.79
_reflns_odcompleteness_iscentric 1
_reflns_odcompleteness_theta     26.32
_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.
;
_reflns_threshold_expression     'I > 2σ(I)'
_computing_cell_refinement       'CrysAlisPro 1.171.38.41 (Rigaku OD, 2015)'
_computing_data_collection       'CrysAlisPro 1.171.37.31c (Rigaku OD, 2014)'
_computing_data_reduction        'CrysAlisPro 1.171.38.41 (Rigaku OD, 2015)'
_computing_molecular_graphics    'Mercury3.9 (2016)'
_computing_publication_material  'Olex2 (Dolomanov et al., 2009)'
_computing_structure_refinement  'ShelXL (Sheldrick, 2015)'
_computing_structure_solution    'ShelXT (Sheldrick, 2015)'
_refine_diff_density_max         0.429
_refine_diff_density_min         -0.413
_refine_diff_density_rms         0.083
_refine_ls_extinction_coef       .
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.027
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     486
_refine_ls_number_reflns         7685
_refine_ls_number_restraints     27
_refine_ls_R_factor_all          0.0821
_refine_ls_R_factor_gt           0.0470
_refine_ls_restrained_S_all      1.025
_refine_ls_shift/su_max          0.001
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details     
'w=1/[σ²(Fo²)+(0.0303P)²+0.5219P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0877
_refine_ls_wR_factor_ref         0.1007
_refine_special_details          
;
 Structure of photo-excited high spin state at 20K. 
Excitation with 660nm laser. Laser power delivered on the crystal was ~3.5mW.
 Three DFIX and four ISOR restrains, and also three EADP constrains 
have been applied for BF4-ion at B2 atom site to model respectively 
geometry of B-F bonds and ADP's for diordered F-sites.
;
_atom_sites_solution_hydrogens   mixed
_atom_sites_solution_primary     dual
_atom_sites_solution_secondary   difmap
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 0.26972(2) 0.60124(3) 0.42885(3) 0.01299(11) Uani 1 1 d . . . . .
S1 S 0.59783(3) 0.70031(6) 0.48033(5) 0.01509(16) Uani 1 1 d . . . . .
S2 S -0.05351(4) 0.50648(7) 0.25595(5) 0.02000(18) Uani 1 1 d . . . . .
N2 N 0.36029(11) 0.75710(19) 0.55891(14) 0.0121(5) Uani 1 1 d . . . . .
N3 N 0.37632(11) 0.62386(19) 0.45591(14) 0.0123(5) Uani 1 1 d . . . . .
N9 N 0.16789(11) 0.44933(19) 0.48741(15) 0.0130(5) Uani 1 1 d . . . . .
N6 N 0.24145(11) 0.7284(2) 0.32319(14) 0.0140(5) Uani 1 1 d . . . . .
N4 N 0.37729(11) 0.49154(19) 0.34512(15) 0.0132(5) Uani 1 1 d . . . . .
N5 N 0.30919(11) 0.4830(2) 0.34006(15) 0.0140(5) Uani 1 1 d . . . . .
N10 N 0.23564(11) 0.4726(2) 0.51336(14) 0.0131(5) Uani 1 1 d . . . . .
N8 N 0.16554(11) 0.58145(19) 0.37584(14) 0.0126(5) Uani 1 1 d . . . . .
N1 N 0.29256(11) 0.7337(2) 0.52882(15) 0.0147(5) Uani 1 1 d . . . . .
N7 N 0.17566(11) 0.72141(19) 0.27554(15) 0.0130(5) Uani 1 1 d . . . . .
C28 C -0.14244(14) 0.5281(3) 0.0971(2) 0.0220(7) Uani 1 1 d . . . . .
H28A H -0.1269 0.4541 0.0811 0.033 Uiso 1 1 calc GR . . . .
H28B H -0.1609 0.5705 0.0412 0.033 Uiso 1 1 calc GR . . . .
H28C H -0.1777 0.5182 0.1320 0.033 Uiso 1 1 calc GR . . . .
C10 C 0.34357(15) 0.3525(2) 0.25069(18) 0.0173(6) Uani 1 1 d . . . . .
H10 H 0.3423 0.2918 0.2091 0.021 Uiso 1 1 calc R . . . .
C4 C 0.40598(14) 0.7029(2) 0.51425(17) 0.0117(6) Uani 1 1 d . . . . .
C26 C -0.08293(14) 0.5926(3) 0.15474(19) 0.0185(7) Uani 1 1 d . . . . .
H26 H -0.0460 0.5997 0.1202 0.022 Uiso 1 1 calc R . . . .
C11 C 0.28888(15) 0.3992(2) 0.28229(18) 0.0165(6) Uani 1 1 d . . . . .
H11 H 0.2434 0.3739 0.2645 0.020 Uiso 1 1 calc R . . . .
C18 C 0.12902(14) 0.5066(2) 0.41122(18) 0.0124(6) Uani 1 1 d . . . . .
C20 C 0.02982(14) 0.5463(2) 0.30003(18) 0.0152(6) Uani 1 1 d . . . . .
C22 C 0.13317(14) 0.6410(2) 0.30437(17) 0.0120(6) Uani 1 1 d . . . . .
C2 C 0.30799(14) 0.8708(2) 0.63455(19) 0.0165(6) Uani 1 1 d . . . . .
H2 H 0.2982 0.9268 0.6750 0.020 Uiso 1 1 calc R . . . .
C1 C 0.26129(14) 0.8041(2) 0.57425(18) 0.0153(6) Uani 1 1 d . . . . .
H1 H 0.2135 0.8089 0.5670 0.018 Uiso 1 1 calc R . . . .
C19 C 0.06200(14) 0.4865(2) 0.37772(18) 0.0157(6) Uani 1 1 d . . . . .
H19 H 0.0379 0.4338 0.4061 0.019 Uiso 1 1 calc R . . . .
C6 C 0.51198(14) 0.6766(2) 0.47412(18) 0.0143(6) Uani 1 1 d . . . . .
C13 C 0.58119(15) 0.9302(2) 0.48611(19) 0.0182(7) Uani 1 1 d . . . . .
H13A H 0.5971 0.9359 0.4291 0.027 Uiso 1 1 calc GR . . . .
H13B H 0.5914 1.0003 0.5208 0.027 Uiso 1 1 calc GR . . . .
H13C H 0.5322 0.9173 0.4722 0.027 Uiso 1 1 calc GR . . . .
C15 C 0.25829(14) 0.4055(2) 0.58392(17) 0.0133(6) Uani 1 1 d . . . . .
H15 H 0.3040 0.4031 0.6169 0.016 Uiso 1 1 calc R . . . .
C3 C 0.37015(14) 0.8388(2) 0.62323(18) 0.0157(6) Uani 1 1 d . . . . .
H3 H 0.4125 0.8682 0.6546 0.019 Uiso 1 1 calc R . . . .
C12 C 0.61661(14) 0.8329(2) 0.54228(18) 0.0148(6) Uani 1 1 d . . . . .
H12 H 0.6013 0.8283 0.6012 0.018 Uiso 1 1 calc R . . . .
C21 C 0.06579(14) 0.6277(2) 0.26312(19) 0.0152(6) Uani 1 1 d . . . . .
H21 H 0.0448 0.6718 0.2120 0.018 Uiso 1 1 calc R . . . .
C14 C 0.69326(14) 0.8459(3) 0.56183(19) 0.0199(7) Uani 1 1 d . . . . .
H14A H 0.7146 0.7795 0.5948 0.030 Uiso 1 1 calc GR . . . .
H14B H 0.7065 0.9133 0.5991 0.030 Uiso 1 1 calc GR . . . .
H14C H 0.7081 0.8533 0.5041 0.030 Uiso 1 1 calc GR . . . .
C9 C 0.39913(14) 0.4136(2) 0.29278(17) 0.0146(6) Uani 1 1 d . . . . .
H9 H 0.4444 0.4031 0.2863 0.018 Uiso 1 1 calc R . . . .
C16 C 0.20630(14) 0.3384(2) 0.60386(18) 0.0157(6) Uani 1 1 d . . . . .
H16 H 0.2099 0.2838 0.6509 0.019 Uiso 1 1 calc R . . . .
C17 C 0.14936(15) 0.3686(2) 0.54101(18) 0.0168(6) Uani 1 1 d . . . . .
H17 H 0.1052 0.3386 0.5359 0.020 Uiso 1 1 calc R . . . .
C27 C -0.10347(15) 0.7082(3) 0.1808(2) 0.0223(7) Uani 1 1 d . . . . .
H27A H -0.1396 0.7011 0.2146 0.033 Uiso 1 1 calc GR . . . .
H27B H -0.1198 0.7528 0.1254 0.033 Uiso 1 1 calc GR . . . .
H27C H -0.0643 0.7458 0.2191 0.033 Uiso 1 1 calc GR . . . .
C24 C 0.21777(15) 0.8683(2) 0.21998(19) 0.0178(6) Uani 1 1 d . . . . .
H24 H 0.2232 0.9333 0.1853 0.021 Uiso 1 1 calc R . . . .
C25 C 0.26676(14) 0.8172(2) 0.28864(18) 0.0161(6) Uani 1 1 d . . . . .
H25 H 0.3121 0.8428 0.3079 0.019 Uiso 1 1 calc R . . . .
C7 C 0.48142(14) 0.5946(2) 0.41181(18) 0.0133(6) Uani 1 1 d . . . . .
H7 H 0.5064 0.5558 0.3746 0.016 Uiso 1 1 calc R . . . .
C8 C 0.41433(14) 0.5719(2) 0.40617(18) 0.0140(6) Uani 1 1 d . . . . .
C23 C 0.16054(15) 0.8048(2) 0.21351(18) 0.0165(6) Uani 1 1 d . . . . .
H23 H 0.1181 0.8172 0.1729 0.020 Uiso 1 1 calc R . . . .
C5 C 0.47351(14) 0.7325(2) 0.52795(18) 0.0135(6) Uani 1 1 d . . . . .
H5 H 0.4929 0.7879 0.5715 0.016 Uiso 1 1 calc R . . . .
F7 F -0.00471(10) 0.78827(17) 0.41817(11) 0.0347(5) Uani 0.978(2) 1 d . U P A 2
F8 F 0.10229(8) 0.73726(15) 0.48678(11) 0.0243(5) Uani 0.978(2) 1 d . . P A 2
F6 F 0.01676(8) 0.71962(14) 0.56243(11) 0.0217(4) Uani 1 1 d . . . . .
F5 F 0.05609(11) 0.89190(16) 0.53718(13) 0.0335(6) Uani 0.978(2) 1 d . U P A 2
B2 B 0.04302(18) 0.7844(3) 0.5003(2) 0.0213(8) Uani 1 1 d D . . . .
F4 F 0.43189(9) 0.56606(15) 0.68975(11) 0.0255(4) Uani 1 1 d . . . . .
F3 F 0.36388(8) 0.46565(14) 0.76351(10) 0.0211(4) Uani 1 1 d . . . . .
F2 F 0.47870(8) 0.44753(14) 0.80576(10) 0.0202(4) Uani 1 1 d . . . . .
F1 F 0.42719(8) 0.61061(14) 0.83555(11) 0.0202(4) Uani 1 1 d . . . . .
B1 B 0.42498(17) 0.5229(3) 0.7743(2) 0.0178(7) Uani 1 1 d . . . . .
O1W O 0.12763(11) 0.41499(19) 0.14644(15) 0.0278(5) Uani 1 1 d . . . . .
H1WA H 0.0914 0.3735 0.1346 0.042 Uiso 1 1 d G . . . .
H1WB H 0.1195 0.4789 0.1178 0.042 Uiso 1 1 d G . . . .
F8A F 0.057(4) 0.774(7) 0.413(2) 0.0243(5) Uani 0.022(2) 1 d D . P A 1
F5A F 0.097(3) 0.832(7) 0.563(4) 0.0335(6) Uani 0.022(2) 1 d D U P A 1
F7A F 0.008(4) 0.887(4) 0.484(5) 0.0347(5) Uani 0.022(2) 1 d D U P A 1


_geom_special_details            
;
 All esds (except the esd in the dihedral angle between two l.s. planes)
 are estimated using the full covariance matrix.  The cell esds are taken
 into account individually in the estimation of esds in distances, angles
 and torsion angles; correlations between esds in cell parameters are only
 used when they are defined by crystal symmetry.  An approximate (isotropic)
 treatment of cell esds is used for estimating esds involving l.s. planes.
;
loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
_geom_bond_publ_flag
Fe1 N3 2.123(2) . ?
Fe1 N6 2.175(2) . ?
Fe1 N5 2.202(2) . ?
Fe1 N10 2.190(2) . ?
Fe1 N8 2.098(2) . ?
Fe1 N1 2.154(2) . ?
S1 C6 1.742(3) . ?
S1 C12 1.826(3) . ?
S2 C26 1.821(3) . ?
S2 C20 1.737(3) . ?
N2 N1 1.375(3) . ?
N2 C4 1.409(3) . ?
N2 C3 1.353(3) . ?
N3 C4 1.334(3) . ?
N3 C8 1.334(3) . ?
N9 N10 1.369(3) . ?
N9 C18 1.413(3) . ?
N9 C17 1.356(3) . ?
N6 N7 1.370(3) . ?
N6 C25 1.326(3) . ?
N4 N5 1.367(3) . ?
N4 C9 1.349(3) . ?
N4 C8 1.419(3) . ?
N5 C11 1.325(3) . ?
N10 C15 1.325(3) . ?
N8 C18 1.338(3) . ?
N8 C22 1.332(3) . ?
N1 C1 1.324(3) . ?
N7 C22 1.414(3) . ?
N7 C23 1.349(3) . ?
C28 H28A 0.9800 . ?
C28 H28B 0.9800 . ?
C28 H28C 0.9800 . ?
C28 C26 1.527(4) . ?
C10 H10 0.9500 . ?
C10 C11 1.408(4) . ?
C10 C9 1.371(4) . ?
C4 C5 1.382(4) . ?
C26 H26 1.0000 . ?
C26 C27 1.511(4) . ?
C11 H11 0.9500 . ?
C18 C19 1.361(4) . ?
C20 C19 1.399(4) . ?
C20 C21 1.395(4) . ?
C22 C21 1.378(4) . ?
C2 H2 0.9500 . ?
C2 C1 1.402(4) . ?
C2 C3 1.359(4) . ?
C1 H1 0.9500 . ?
C19 H19 0.9500 . ?
C6 C7 1.398(4) . ?
C6 C5 1.404(4) . ?
C13 H13A 0.9800 . ?
C13 H13B 0.9800 . ?
C13 H13C 0.9800 . ?
C13 C12 1.516(4) . ?
C15 H15 0.9500 . ?
C15 C16 1.402(4) . ?
C3 H3 0.9500 . ?
C12 H12 1.0000 . ?
C12 C14 1.522(4) . ?
C21 H21 0.9500 . ?
C14 H14A 0.9800 . ?
C14 H14B 0.9800 . ?
C14 H14C 0.9800 . ?
C9 H9 0.9500 . ?
C16 H16 0.9500 . ?
C16 C17 1.369(4) . ?
C17 H17 0.9500 . ?
C27 H27A 0.9800 . ?
C27 H27B 0.9800 . ?
C27 H27C 0.9800 . ?
C24 H24 0.9500 . ?
C24 C25 1.403(4) . ?
C24 C23 1.367(4) . ?
C25 H25 0.9500 . ?
C7 H7 0.9500 . ?
C7 C8 1.368(4) . ?
C23 H23 0.9500 . ?
C5 H5 0.9500 . ?
F7 B2 1.392(4) . ?
F8 B2 1.378(4) . ?
F6 B2 1.399(4) . ?
F5 B2 1.394(4) . ?
B2 F8A 1.396(10) . ?
B2 F5A 1.402(10) . ?
B2 F7A 1.402(10) . ?
F4 B1 1.404(3) . ?
F3 B1 1.389(4) . ?
F2 B1 1.408(4) . ?
F1 B1 1.384(4) . ?
O1W H1WA 0.8697 . ?
O1W H1WB 0.8703 . ?

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 N6 98.45(8) . . ?
N3 Fe1 N5 73.14(8) . . ?
N3 Fe1 N10 114.32(8) . . ?
N3 Fe1 N1 73.67(8) . . ?
N6 Fe1 N5 94.26(8) . . ?
N6 Fe1 N10 147.21(9) . . ?
N10 Fe1 N5 96.11(8) . . ?
N8 Fe1 N3 169.02(8) . . ?
N8 Fe1 N6 73.60(9) . . ?
N8 Fe1 N5 99.51(9) . . ?
N8 Fe1 N10 74.04(9) . . ?
N8 Fe1 N1 113.08(9) . . ?
N1 Fe1 N6 89.04(9) . . ?
N1 Fe1 N5 146.77(9) . . ?
N1 Fe1 N10 98.81(8) . . ?
C6 S1 C12 105.16(13) . . ?
C20 S2 C26 106.21(13) . . ?
N1 N2 C4 117.4(2) . . ?
C3 N2 N1 111.2(2) . . ?
C3 N2 C4 131.1(2) . . ?
C4 N3 Fe1 120.53(17) . . ?
C8 N3 Fe1 121.29(18) . . ?
C8 N3 C4 117.5(2) . . ?
N10 N9 C18 118.7(2) . . ?
C17 N9 N10 111.3(2) . . ?
C17 N9 C18 130.0(2) . . ?
N7 N6 Fe1 114.25(16) . . ?
C25 N6 Fe1 140.8(2) . . ?
C25 N6 N7 104.9(2) . . ?
N5 N4 C8 118.1(2) . . ?
C9 N4 N5 111.7(2) . . ?
C9 N4 C8 130.1(2) . . ?
N4 N5 Fe1 114.35(16) . . ?
C11 N5 Fe1 140.66(19) . . ?
C11 N5 N4 104.9(2) . . ?
N9 N10 Fe1 113.43(16) . . ?
C15 N10 Fe1 141.68(19) . . ?
C15 N10 N9 104.9(2) . . ?
C18 N8 Fe1 121.32(18) . . ?
C22 N8 Fe1 121.57(18) . . ?
C22 N8 C18 117.1(2) . . ?
N2 N1 Fe1 115.10(16) . . ?
C1 N1 Fe1 140.03(19) . . ?
C1 N1 N2 104.9(2) . . ?
N6 N7 C22 117.8(2) . . ?
C23 N7 N6 111.4(2) . . ?
C23 N7 C22 130.2(2) . . ?
H28A C28 H28B 109.5 . . ?
H28A C28 H28C 109.5 . . ?
H28B C28 H28C 109.5 . . ?
C26 C28 H28A 109.5 . . ?
C26 C28 H28B 109.5 . . ?
C26 C28 H28C 109.5 . . ?
C11 C10 H10 127.4 . . ?
C9 C10 H10 127.4 . . ?
C9 C10 C11 105.2(2) . . ?
N3 C4 N2 112.7(2) . . ?
N3 C4 C5 124.5(2) . . ?
C5 C4 N2 122.8(2) . . ?
S2 C26 H26 109.5 . . ?
C28 C26 S2 105.4(2) . . ?
C28 C26 H26 109.5 . . ?
C27 C26 S2 110.7(2) . . ?
C27 C26 C28 112.0(2) . . ?
C27 C26 H26 109.5 . . ?
N5 C11 C10 111.2(3) . . ?
N5 C11 H11 124.4 . . ?
C10 C11 H11 124.4 . . ?
N8 C18 N9 112.5(2) . . ?
N8 C18 C19 124.1(3) . . ?
C19 C18 N9 123.3(2) . . ?
C19 C20 S2 114.6(2) . . ?
C21 C20 S2 125.7(2) . . ?
C21 C20 C19 119.6(3) . . ?
N8 C22 N7 112.3(2) . . ?
N8 C22 C21 124.5(2) . . ?
C21 C22 N7 123.2(3) . . ?
C1 C2 H2 127.1 . . ?
C3 C2 H2 127.1 . . ?
C3 C2 C1 105.9(2) . . ?
N1 C1 C2 111.0(2) . . ?
N1 C1 H1 124.5 . . ?
C2 C1 H1 124.5 . . ?
C18 C19 C20 117.7(3) . . ?
C18 C19 H19 121.1 . . ?
C20 C19 H19 121.1 . . ?
C7 C6 S1 116.1(2) . . ?
C7 C6 C5 119.7(3) . . ?
C5 C6 S1 124.3(2) . . ?
H13A C13 H13B 109.5 . . ?
H13A C13 H13C 109.5 . . ?
H13B C13 H13C 109.5 . . ?
C12 C13 H13A 109.5 . . ?
C12 C13 H13B 109.5 . . ?
C12 C13 H13C 109.5 . . ?
N10 C15 H15 124.2 . . ?
N10 C15 C16 111.5(3) . . ?
C16 C15 H15 124.2 . . ?
N2 C3 C2 107.0(3) . . ?
N2 C3 H3 126.5 . . ?
C2 C3 H3 126.5 . . ?
S1 C12 H12 109.5 . . ?
C13 C12 S1 110.70(19) . . ?
C13 C12 H12 109.5 . . ?
C13 C12 C14 111.6(2) . . ?
C14 C12 S1 106.1(2) . . ?
C14 C12 H12 109.5 . . ?
C20 C21 H21 121.6 . . ?
C22 C21 C20 116.8(3) . . ?
C22 C21 H21 121.6 . . ?
C12 C14 H14A 109.5 . . ?
C12 C14 H14B 109.5 . . ?
C12 C14 H14C 109.5 . . ?
H14A C14 H14B 109.5 . . ?
H14A C14 H14C 109.5 . . ?
H14B C14 H14C 109.5 . . ?
N4 C9 C10 107.0(2) . . ?
N4 C9 H9 126.5 . . ?
C10 C9 H9 126.5 . . ?
C15 C16 H16 127.4 . . ?
C17 C16 C15 105.2(2) . . ?
C17 C16 H16 127.4 . . ?
N9 C17 C16 107.1(2) . . ?
N9 C17 H17 126.4 . . ?
C16 C17 H17 126.4 . . ?
C26 C27 H27A 109.5 . . ?
C26 C27 H27B 109.5 . . ?
C26 C27 H27C 109.5 . . ?
H27A C27 H27B 109.5 . . ?
H27A C27 H27C 109.5 . . ?
H27B C27 H27C 109.5 . . ?
C25 C24 H24 127.3 . . ?
C23 C24 H24 127.3 . . ?
C23 C24 C25 105.4(3) . . ?
N6 C25 C24 111.1(3) . . ?
N6 C25 H25 124.4 . . ?
C24 C25 H25 124.4 . . ?
C6 C7 H7 121.1 . . ?
C8 C7 C6 117.8(2) . . ?
C8 C7 H7 121.1 . . ?
N3 C8 N4 112.6(2) . . ?
N3 C8 C7 124.0(3) . . ?
C7 C8 N4 123.4(2) . . ?
N7 C23 C24 107.1(3) . . ?
N7 C23 H23 126.4 . . ?
C24 C23 H23 126.4 . . ?
C4 C5 C6 116.5(3) . . ?
C4 C5 H5 121.7 . . ?
C6 C5 H5 121.7 . . ?
F7 B2 F6 108.5(3) . . ?
F7 B2 F5 110.9(3) . . ?
F8 B2 F7 109.9(3) . . ?
F8 B2 F6 110.1(3) . . ?
F8 B2 F5 109.6(3) . . ?
F6 B2 F5A 97(3) . . ?
F6 B2 F7A 110(3) . . ?
F5 B2 F6 107.9(2) . . ?
F8A B2 F6 139(3) . . ?
F8A B2 F5A 112(4) . . ?
F8A B2 F7A 96(5) . . ?
F7A B2 F5A 94(6) . . ?
F4 B1 F2 108.3(2) . . ?
F3 B1 F4 109.5(2) . . ?
F3 B1 F2 109.3(3) . . ?
F1 B1 F4 109.2(3) . . ?
F1 B1 F3 110.3(2) . . ?
F1 B1 F2 110.2(2) . . ?
H1WA O1W H1WB 109.4 . . ?

loop_
_geom_torsion_atom_site_label_1
_geom_torsion_atom_site_label_2
_geom_torsion_atom_site_label_3
_geom_torsion_atom_site_label_4
_geom_torsion
_geom_torsion_site_symmetry_1
_geom_torsion_site_symmetry_2
_geom_torsion_site_symmetry_3
_geom_torsion_site_symmetry_4
_geom_torsion_publ_flag
Fe1 N3 C4 N2 5.7(3) . . . . ?
Fe1 N3 C4 C5 -172.0(2) . . . . ?
Fe1 N3 C8 N4 -8.2(3) . . . . ?
Fe1 N3 C8 C7 170.7(2) . . . . ?
Fe1 N6 N7 C22 5.0(3) . . . . ?
Fe1 N6 N7 C23 177.67(16) . . . . ?
Fe1 N6 C25 C24 -176.8(2) . . . . ?
Fe1 N5 C11 C10 -176.4(2) . . . . ?
Fe1 N10 C15 C16 -179.2(2) . . . . ?
Fe1 N8 C18 N9 2.3(3) . . . . ?
Fe1 N8 C18 C19 -177.3(2) . . . . ?
Fe1 N8 C22 N7 -4.5(3) . . . . ?
Fe1 N8 C22 C21 176.2(2) . . . . ?
Fe1 N1 C1 C2 178.2(2) . . . . ?
S1 C6 C7 C8 178.8(2) . . . . ?
S1 C6 C5 C4 -179.7(2) . . . . ?
S2 C20 C19 C18 174.5(2) . . . . ?
S2 C20 C21 C22 -175.1(2) . . . . ?
N2 N1 C1 C2 -1.3(3) . . . . ?
N2 C4 C5 C6 -175.7(2) . . . . ?
N3 C4 C5 C6 1.8(4) . . . . ?
N9 N10 C15 C16 0.3(3) . . . . ?
N9 C18 C19 C20 -177.9(2) . . . . ?
N6 N7 C22 N8 -0.7(3) . . . . ?
N6 N7 C22 C21 178.6(2) . . . . ?
N6 N7 C23 C24 0.2(3) . . . . ?
N4 N5 C11 C10 0.7(3) . . . . ?
N5 N4 C9 C10 0.9(3) . . . . ?
N5 N4 C8 N3 4.4(3) . . . . ?
N5 N4 C8 C7 -174.5(3) . . . . ?
N10 N9 C18 N8 -2.2(3) . . . . ?
N10 N9 C18 C19 177.4(2) . . . . ?
N10 N9 C17 C16 0.2(3) . . . . ?
N10 C15 C16 C17 -0.2(3) . . . . ?
N8 C18 C19 C20 1.6(4) . . . . ?
N8 C22 C21 C20 0.4(4) . . . . ?
N1 N2 C4 N3 -8.5(3) . . . . ?
N1 N2 C4 C5 169.3(2) . . . . ?
N1 N2 C3 C2 -0.9(3) . . . . ?
N7 N6 C25 C24 0.7(3) . . . . ?
N7 C22 C21 C20 -178.9(2) . . . . ?
C4 N2 N1 Fe1 7.4(3) . . . . ?
C4 N2 N1 C1 -173.0(2) . . . . ?
C4 N2 C3 C2 172.4(3) . . . . ?
C4 N3 C8 N4 -178.6(2) . . . . ?
C4 N3 C8 C7 0.3(4) . . . . ?
C26 S2 C20 C19 -178.4(2) . . . . ?
C26 S2 C20 C21 -0.5(3) . . . . ?
C11 C10 C9 N4 -0.4(3) . . . . ?
C18 N9 N10 Fe1 1.1(3) . . . . ?
C18 N9 N10 C15 -178.6(2) . . . . ?
C18 N9 C17 C16 178.2(3) . . . . ?
C18 N8 C22 N7 176.9(2) . . . . ?
C18 N8 C22 C21 -2.4(4) . . . . ?
C20 S2 C26 C28 158.03(19) . . . . ?
C20 S2 C26 C27 -80.6(2) . . . . ?
C22 N8 C18 N9 -179.1(2) . . . . ?
C22 N8 C18 C19 1.3(4) . . . . ?
C22 N7 C23 C24 171.7(3) . . . . ?
C1 C2 C3 N2 0.1(3) . . . . ?
C19 C20 C21 C22 2.7(4) . . . . ?
C6 S1 C12 C13 -67.6(2) . . . . ?
C6 S1 C12 C14 171.19(18) . . . . ?
C6 C7 C8 N3 0.5(4) . . . . ?
C6 C7 C8 N4 179.3(2) . . . . ?
C15 C16 C17 N9 0.0(3) . . . . ?
C3 N2 N1 Fe1 -178.24(17) . . . . ?
C3 N2 N1 C1 1.4(3) . . . . ?
C3 N2 C4 N3 178.5(3) . . . . ?
C3 N2 C4 C5 -3.7(4) . . . . ?
C3 C2 C1 N1 0.8(3) . . . . ?
C12 S1 C6 C7 165.5(2) . . . . ?
C12 S1 C6 C5 -15.6(3) . . . . ?
C21 C20 C19 C18 -3.6(4) . . . . ?
C9 N4 N5 Fe1 177.00(17) . . . . ?
C9 N4 N5 C11 -1.0(3) . . . . ?
C9 N4 C8 N3 -170.8(3) . . . . ?
C9 N4 C8 C7 10.3(4) . . . . ?
C9 C10 C11 N5 -0.2(3) . . . . ?
C17 N9 N10 Fe1 179.37(17) . . . . ?
C17 N9 N10 C15 -0.3(3) . . . . ?
C17 N9 C18 N8 179.9(3) . . . . ?
C17 N9 C18 C19 -0.5(4) . . . . ?
C25 N6 N7 C22 -173.2(2) . . . . ?
C25 N6 N7 C23 -0.6(3) . . . . ?
C25 C24 C23 N7 0.2(3) . . . . ?
C7 C6 C5 C4 -0.9(4) . . . . ?
C8 N3 C4 N2 176.2(2) . . . . ?
C8 N3 C4 C5 -1.5(4) . . . . ?
C8 N4 N5 Fe1 1.0(3) . . . . ?
C8 N4 N5 C11 -177.0(2) . . . . ?
C8 N4 C9 C10 176.3(3) . . . . ?
C23 N7 C22 N8 -171.7(2) . . . . ?
C23 N7 C22 C21 7.6(4) . . . . ?
C23 C24 C25 N6 -0.6(3) . . . . ?
C5 C6 C7 C8 -0.2(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_rk137MeNO2PI_015K
_database_code_depnum_ccdc_archive 'CCDC 1564672'
_audit_update_record             
;
2017-07-28 deposited with the CCDC.
2017-11-20 downloaded from the CCDC.
;
_chemical_name_common            ?
_chemical_name_systematic        ?
_chemical_formula_moiety         'C28 H30 Fe N10 S2, 2(B F4), C H3 N O2'
_chemical_formula_sum            'C29 H33 B2 F8 Fe N11 O2 S2'
_chemical_formula_weight         861.25
_chemical_absolute_configuration ?
_chemical_melting_point          'not measured'
loop_
_atom_type_symbol
_atom_type_description
_atom_type_scat_dispersion_real
_atom_type_scat_dispersion_imag
_atom_type_scat_source
C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
B B 0.0013 0.0007 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
F F 0.0171 0.0103 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Fe Fe 0.3463 0.8444 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
S S 0.1246 0.1234 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'

_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.
;
_space_group_crystal_system      monoclinic
_space_group_IT_number           4
_space_group_name_H-M_alt        'P 1 21 1'
_space_group_name_Hall           'P 2yb'
loop_
_space_group_symop_operation_xyz
'x, y, z'
'-x, y+1/2, -z'

_cell_length_a                   20.2896(5)
_cell_length_b                   12.0942(3)
_cell_length_c                   15.3831(4)
_cell_angle_alpha                90
_cell_angle_beta                 101.088(2)
_cell_angle_gamma                90
_cell_volume                     3704.34(16)
_cell_special_details            
;
In comparison to high temperature high spin phase for this system where
space group is P2(1)/n, at 15 K after light irradiation with 660nm laser
and ~3.5mW power, the reflection conditions for n-glide plane are no longer
valid. New symmetry at 15K for high spin phase is P2(1).
;
_cell_formula_units_Z            4
_cell_measurement_reflns_used    9484
_cell_measurement_temperature    15(1)
_cell_measurement_theta_max      32.9910
_cell_measurement_theta_min      3.4860
_exptl_absorpt_coefficient_mu    0.606
_exptl_absorpt_correction_T_max  0.978
_exptl_absorpt_correction_T_min  0.960
_exptl_absorpt_correction_type   analytical
_exptl_absorpt_process_details   
;
CrysAlisPro 1.171.38.41 (Rigaku Oxford Diffraction, 2015)
Analytical numeric absorption correction using a multifaceted crystal
			model based on expressions derived by R.C. Clark & J.S. Reid.
(Clark, R. C. & Reid, J. S. (1995). Acta Cryst. A51, 887-897)
Empirical absorption correction using spherical harmonics,
 implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_absorpt_special_details   ?
_exptl_crystal_colour            orange
_exptl_crystal_density_diffrn    1.544
_exptl_crystal_density_meas      'not measured'
_exptl_crystal_density_method    none
_exptl_crystal_description       block
_exptl_crystal_F_000             1760
loop_
_exptl_crystal_face_index_h
_exptl_crystal_face_index_k
_exptl_crystal_face_index_l
_exptl_crystal_face_perp_dist
1 15 12 0.1127
-1 8 -24 0.1139
3 -9 23 0.0451
1 -15 -12 0.0147
-21 -3 2 0.0421
20 5 -1 0.2197
13 2 -25 0.1857

_exptl_crystal_size_max          0.329
_exptl_crystal_size_mid          0.169
_exptl_crystal_size_min          0.132
loop_
_exptl_oxdiff_crystal_face_indexfrac_h
_exptl_oxdiff_crystal_face_indexfrac_k
_exptl_oxdiff_crystal_face_indexfrac_l
_exptl_oxdiff_crystal_face_x
_exptl_oxdiff_crystal_face_y
_exptl_oxdiff_crystal_face_z
1.1210 14.9914 12.4927 0.3951 0.8300 0.3712
-1.3206 8.3912 -23.6902 -0.8874 0.4222 0.1062
3.2256 -9.0989 22.6970 0.8853 -0.4257 -0.2051
0.7841 -15.0197 -12.4505 -0.3636 -0.7967 -0.4485
-21.0733 -3.1274 1.5736 -0.2626 -0.5536 0.7877
20.1375 4.5063 -0.5546 0.2781 0.6109 -0.7124
12.8503 2.0227 -25.4776 -0.7017 0.3384 -0.6216

_exptl_transmission_factor_max   ?
_exptl_transmission_factor_min   ?
_diffrn_reflns_av_R_equivalents  0.0265
_diffrn_reflns_av_unetI/netI     0.0512
_diffrn_reflns_Laue_measured_fraction_full 0.997
_diffrn_reflns_Laue_measured_fraction_max 0.997
_diffrn_reflns_limit_h_max       22
_diffrn_reflns_limit_h_min       -24
_diffrn_reflns_limit_k_max       14
_diffrn_reflns_limit_k_min       -13
_diffrn_reflns_limit_l_max       18
_diffrn_reflns_limit_l_min       -18
_diffrn_reflns_number            16837
_diffrn_reflns_point_group_measured_fraction_full 0.998
_diffrn_reflns_point_group_measured_fraction_max 0.998
_diffrn_reflns_theta_full        24.999
_diffrn_reflns_theta_max         24.999
_diffrn_reflns_theta_min         3.065
_diffrn_ambient_temperature      15(1)
_diffrn_detector                 'CCD plate'
_diffrn_detector_area_resol_mean 16.1852
_diffrn_detector_type            Sapphire3
_diffrn_measured_fraction_theta_full 0.997
_diffrn_measured_fraction_theta_max 0.997
_diffrn_measurement_details      
;
List of Runs (angles in degrees, time in seconds):

  # Type    Start    End  Width  tₑₓₚ   ω     θ     κ     φ   Frames
#--------------------------------------------------------------------------
  1  ω      2.00 106.00   1.00   10.00    --   32.43  38.00   0.00  104
  2  ω      8.00  95.00   1.00   10.00    --   32.43  77.00 120.00   87
  3  ω    -97.00 -35.00   1.00   10.00    --  -30.39-178.00 120.00   62
  4  ω   -108.00 -60.00   1.00   10.00    --  -30.39-178.00-180.00   48
;
_diffrn_measurement_device       'four-circle diffractometer'
_diffrn_measurement_device_type  'Xcalibur, Sapphire3'
_diffrn_measurement_method       'ω scans'
_diffrn_orient_matrix_type       
'CrysAlisPro convention (1999,Acta A55,543-557)'
_diffrn_orient_matrix_UB_11      0.0156950000
_diffrn_orient_matrix_UB_12      -0.0040966000
_diffrn_orient_matrix_UB_13      0.0351333000
_diffrn_orient_matrix_UB_21      0.0182990000
_diffrn_orient_matrix_UB_22      0.0538162000
_diffrn_orient_matrix_UB_23      0.0002193000
_diffrn_orient_matrix_UB_31      -0.0403358000
_diffrn_orient_matrix_UB_32      0.0228857000
_diffrn_orient_matrix_UB_33      0.0058703000
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_source                   'fine-focus sealed X-ray tube'
_diffrn_source_type              'Enhance (Mo) X-ray Source'
_reflns_Friedel_coverage         0.902
_reflns_Friedel_fraction_full    0.999
_reflns_Friedel_fraction_max     0.999
_reflns_number_gt                10472
_reflns_number_total             11529
_reflns_odcompleteness_completeness 99.77
_reflns_odcompleteness_iscentric 1
_reflns_odcompleteness_theta     26.32
_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.
;
_reflns_threshold_expression     'I > 2σ(I)'
_computing_cell_refinement       'CrysAlisPro 1.171.38.41 (Rigaku OD, 2015)'
_computing_data_collection       'CrysAlisPro 1.171.37.31c (Rigaku OD, 2014)'
_computing_data_reduction        'CrysAlisPro 1.171.38.41 (Rigaku OD, 2015)'
_computing_molecular_graphics    'Mercury3.9 (2016)'
_computing_publication_material  'Olex2 (Dolomanov et al., 2009)'
_computing_structure_refinement  'ShelXL (Sheldrick, 2015)'
_computing_structure_solution    'ShelXT (Sheldrick, 2015)'
_refine_diff_density_max         0.288
_refine_diff_density_min         -0.287
_refine_diff_density_rms         0.059
_refine_ls_abs_structure_details 
;
 Refined as an inversion twin with 50%/50% ratio.
;
_refine_ls_abs_structure_Flack   0.483(15)
_refine_ls_extinction_coef       .
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.010
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     1012
_refine_ls_number_reflns         11529
_refine_ls_number_restraints     1
_refine_ls_R_factor_all          0.0398
_refine_ls_R_factor_gt           0.0334
_refine_ls_restrained_S_all      1.010
_refine_ls_shift/su_max          0.001
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details     
'w=1/[σ²(Fo²)+(0.0308P)²+0.3569P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0696
_refine_ls_wR_factor_ref         0.0732
_refine_special_details          
;
Structure of photoincuded high spin state at 15K.
Excitation with 660nm laser. Laser power delivered on the crystal was ~3.5mW.
Refined as a 2-component inversion twin with (-1 0 0 0 -1 0 0 0 -1)
twin matrix due to either domains formation or crystal breaking.
Five reflections have been treated with OMIT ShelXL instruction.
;
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     dual
_atom_sites_solution_secondary   difmap
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
Fe1B Fe 0.72097(3) 0.82363(5) 0.81166(4) 0.00872(15) Uani 1 1 d . . . . .
Fe1 Fe 0.72093(3) 0.12475(5) 0.30596(4) 0.00861(15) Uani 1 1 d . . . . .
S1B S 0.39695(6) 0.93878(10) 0.77052(8) 0.0109(3) Uani 1 1 d . . . . .
S1 S 0.39650(6) 0.02116(10) 0.27177(8) 0.0112(3) Uani 1 1 d . . . . .
S2B S 1.03751(5) 0.69652(10) 0.97868(7) 0.0140(2) Uani 1 1 d . . . . .
S2 S 1.04521(5) 0.20353(11) 0.46131(7) 0.0158(3) Uani 1 1 d . . . . .
F2 F 0.57732(13) 0.1754(2) 0.05883(16) 0.0160(6) Uani 1 1 d . . . . .
F4 F 0.64115(12) 0.2564(2) -0.03049(16) 0.0147(6) Uani 1 1 d . . . . .
F7B F 0.89347(12) 0.8670(2) 0.70394(16) 0.0209(6) Uani 1 1 d . . . . .
F5B F 0.99849(12) 0.8895(2) 0.78869(16) 0.0176(6) Uani 1 1 d . . . . .
F3B F 0.56336(12) 0.8414(2) 0.41376(16) 0.0156(6) Uani 1 1 d . . . . .
F1 F 0.52782(12) 0.2847(2) -0.05645(16) 0.0165(6) Uani 1 1 d . . . . .
F3 F 0.57019(13) 0.1152(2) -0.08323(16) 0.0175(6) Uani 1 1 d . . . . .
F2B F 0.57083(12) 0.7851(2) 0.55744(16) 0.0154(6) Uani 1 1 d . . . . .
F8B F 0.97004(12) 0.9779(2) 0.65648(15) 0.0184(6) Uani 1 1 d . . . . .
F8 F 0.93795(12) -0.1174(2) 0.31469(16) 0.0199(6) Uani 1 1 d . . . . .
F5 F 0.89374(12) 0.0249(2) 0.22506(16) 0.0185(6) Uani 1 1 d . . . . .
F4B F 0.52073(12) 0.6737(2) 0.44351(16) 0.0163(6) Uani 1 1 d . . . . .
F1B F 0.63430(12) 0.7012(2) 0.46894(16) 0.0148(6) Uani 1 1 d . . . . .
F6B F 0.92237(13) 1.0301(2) 0.77355(18) 0.0255(7) Uani 1 1 d . . . . .
F7 F 1.00717(12) 0.0158(2) 0.27727(18) 0.0234(7) Uani 1 1 d . . . . .
F6 F 0.95633(13) -0.1062(3) 0.17317(16) 0.0293(7) Uani 1 1 d . . . . .
O1 O 0.82952(15) 0.1792(3) 0.5814(2) 0.0222(8) Uani 1 1 d . . . . .
N8B N 0.82371(18) 0.7911(3) 0.8626(2) 0.0097(8) Uani 1 1 d . . . . .
N9 N 0.82319(17) 0.2724(3) 0.2438(2) 0.0098(8) Uani 1 1 d . . . . .
N1 N 0.68164(17) 0.2409(3) 0.3945(2) 0.0093(8) Uani 1 1 d . . . . .
N3 N 0.61517(18) 0.1008(3) 0.2831(2) 0.0085(8) Uani 1 1 d . . . . .
N3B N 0.61547(18) 0.8534(3) 0.7894(2) 0.0085(8) Uani 1 1 d . . . . .
N4B N 0.63424(17) 0.9810(3) 0.6869(2) 0.0097(8) Uani 1 1 d . . . . .
O1B O 1.14328(14) 1.1034(3) 0.94791(19) 0.0204(8) Uani 1 1 d . . . . .
N10 N 0.75566(18) 0.2495(3) 0.2227(2) 0.0099(8) Uani 1 1 d . . . . .
N8 N 0.82575(17) 0.1423(3) 0.3521(2) 0.0085(8) Uani 1 1 d . . . . .
N6B N 0.75273(17) 0.7032(3) 0.7247(2) 0.0092(8) Uani 1 1 d . . . . .
N5 N 0.69883(17) -0.0076(3) 0.2098(2) 0.0096(8) Uani 1 1 d . . . . .
N2 N 0.61385(18) 0.2307(3) 0.3917(2) 0.0100(9) Uani 1 1 d . . . . .
N9B N 0.81739(17) 0.9293(3) 0.9618(2) 0.0095(8) Uani 1 1 d . . . . .
N6 N 0.74925(17) -0.0012(3) 0.4069(2) 0.0112(9) Uani 1 1 d . . . . .
N2B N 0.61078(17) 0.7224(3) 0.8958(2) 0.0090(9) Uani 1 1 d . . . . .
N7B N 0.81758(18) 0.6664(3) 0.7504(2) 0.0099(8) Uani 1 1 d . . . . .
N7 N 0.81598(17) 0.0013(3) 0.4472(2) 0.0095(8) Uani 1 1 d . . . . .
N11 N 0.85406(19) 0.2584(3) 0.6252(2) 0.0149(9) Uani 1 1 d . . . . .
N5B N 0.70090(17) 0.9521(3) 0.7120(2) 0.0109(9) Uani 1 1 d . . . . .
N4 N 0.63159(17) -0.0289(3) 0.1816(2) 0.0085(8) Uani 1 1 d . . . . .
N10B N 0.75298(18) 0.9452(3) 0.9145(2) 0.0103(8) Uani 1 1 d . . . . .
N1B N 0.67849(17) 0.7100(3) 0.8995(2) 0.0101(8) Uani 1 1 d . . . . .
O2 O 0.82125(16) 0.3379(3) 0.6416(2) 0.0274(8) Uani 1 1 d . . . . .
C5B C 0.5103(2) 0.8298(4) 0.8344(3) 0.0102(10) Uani 1 1 d . . . . .
H5B H 0.4851 0.7945 0.8707 0.012 Uiso 1 1 calc R . . . .
C22B C 0.8569(2) 0.8458(4) 0.9331(3) 0.0091(10) Uani 1 1 d . . . . .
C22 C 0.8622(2) 0.2166(4) 0.3175(3) 0.0091(10) Uani 1 1 d . . . . .
C6 C 0.4814(2) 0.0457(4) 0.2724(3) 0.0097(10) Uani 1 1 d . . . . .
C15B C 0.7290(2) 0.6505(4) 0.6495(3) 0.0119(11) Uani 1 1 d . . . . .
H15B H 0.6859 0.6594 0.6165 0.014 Uiso 1 1 calc R . . . .
C8B C 0.5881(2) 0.9319(4) 0.7330(3) 0.0087(10) Uani 1 1 d . . . . .
C16 C 0.7729(2) -0.1404(4) 0.5052(3) 0.0134(10) Uani 1 1 d . . . . .
H16 H 0.7671 -0.2023 0.5388 0.016 Uiso 1 1 calc R . . . .
C10 C 0.6840(2) -0.1420(4) 0.1065(3) 0.0124(11) Uani 1 1 d . . . . .
H10 H 0.6937 -0.1954 0.0673 0.015 Uiso 1 1 calc R . . . .
C7 C 0.5193(2) -0.0081(4) 0.2184(3) 0.0068(10) Uani 1 1 d . . . . .
H7 H 0.5006 -0.0621 0.1782 0.008 Uiso 1 1 calc R . . . .
C19 C 0.9246(2) 0.0924(4) 0.4563(3) 0.0125(10) Uani 1 1 d . . . . .
H19 H 0.9447 0.0488 0.5039 0.015 Uiso 1 1 calc R . . . .
N11B N 1.13778(19) 1.1517(4) 0.8775(3) 0.0210(10) Uani 1 1 d . . . . .
C11 C 0.7295(2) -0.0776(4) 0.1644(3) 0.0122(11) Uani 1 1 d . . . . .
H11 H 0.7759 -0.0830 0.1706 0.015 Uiso 1 1 calc R . . . .
C18B C 0.8570(2) 0.7133(4) 0.8269(3) 0.0088(10) Uani 1 1 d . . . . .
C9 C 0.6217(2) -0.1099(4) 0.1198(3) 0.0118(10) Uani 1 1 d . . . . .
H9 H 0.5806 -0.1384 0.0916 0.014 Uiso 1 1 calc R . . . .
C4B C 0.5765(2) 0.8038(4) 0.8382(3) 0.0095(10) Uani 1 1 d . . . . .
C15 C 0.7238(2) -0.0874(4) 0.4424(3) 0.0108(10) Uani 1 1 d . . . . .
H15 H 0.6791 -0.1097 0.4275 0.013 Uiso 1 1 calc R . . . .
C20 C 0.9608(2) 0.1724(4) 0.4206(3) 0.0111(10) Uani 1 1 d . . . . .
C8 C 0.5857(2) 0.0227(4) 0.2274(3) 0.0086(10) Uani 1 1 d . . . . .
C21 C 0.9289(2) 0.2370(4) 0.3480(3) 0.0123(10) Uani 1 1 d . . . . .
H21 H 0.9520 0.2905 0.3225 0.015 Uiso 1 1 calc R . . . .
C23B C 0.8340(2) 1.0081(4) 1.0252(3) 0.0112(10) Uani 1 1 d . . . . .
H23B H 0.8747 1.0145 1.0647 0.013 Uiso 1 1 calc R . . . .
C3 C 0.5923(2) 0.3059(4) 0.4456(3) 0.0109(10) Uani 1 1 d . . . . .
H3 H 0.5485 0.3148 0.4540 0.013 Uiso 1 1 calc R . . . .
C17B C 0.8336(2) 0.5919(4) 0.6918(3) 0.0126(10) Uani 1 1 d . . . . .
H17B H 0.8745 0.5560 0.6953 0.015 Uiso 1 1 calc R . . . .
C13B C 0.4171(2) 1.1643(4) 0.7643(3) 0.0136(11) Uani 1 1 d . . . . .
H13A H 0.4009 1.1714 0.8187 0.020 Uiso 1 1 calc GR . . . .
H13B H 0.4088 1.2318 0.7311 0.020 Uiso 1 1 calc GR . . . .
H13C H 0.4644 1.1496 0.7771 0.020 Uiso 1 1 calc GR . . . .
C4 C 0.5774(2) 0.1508(4) 0.3343(3) 0.0094(10) Uani 1 1 d . . . . .
C5 C 0.5112(2) 0.1275(4) 0.3319(3) 0.0089(10) Uani 1 1 d . . . . .
H5 H 0.4868 0.1645 0.3684 0.011 Uiso 1 1 calc R . . . .
C6B C 0.4818(2) 0.9109(4) 0.7743(3) 0.0096(10) Uani 1 1 d . . . . .
C1B C 0.6959(2) 0.6257(4) 0.9539(3) 0.0121(10) Uani 1 1 d . . . . .
H1B H 0.7393 0.5978 0.9690 0.015 Uiso 1 1 calc R . . . .
C18 C 0.8573(2) 0.0803(4) 0.4183(3) 0.0095(10) Uani 1 1 d . . . . .
C19B C 0.9224(2) 0.6851(4) 0.8596(3) 0.0094(10) Uani 1 1 d . . . . .
H19B H 0.9441 0.6315 0.8321 0.011 Uiso 1 1 calc R . . . .
C16B C 0.7776(2) 0.5798(4) 0.6263(3) 0.0111(10) Uani 1 1 d . . . . .
H16B H 0.7729 0.5341 0.5769 0.013 Uiso 1 1 calc R . . . .
C1 C 0.7010(2) 0.3219(4) 0.4513(3) 0.0108(10) Uani 1 1 d . . . . .
H1 H 0.7450 0.3470 0.4670 0.013 Uiso 1 1 calc R . . . .
C21B C 0.9223(2) 0.8236(4) 0.9731(3) 0.0113(10) Uani 1 1 d . . . . .
H21B H 0.9435 0.8628 1.0227 0.014 Uiso 1 1 calc R . . . .
C2 C 0.6467(2) 0.3655(4) 0.4850(3) 0.0116(10) Uani 1 1 d . . . . .
H2 H 0.6478 0.4228 0.5255 0.014 Uiso 1 1 calc R . . . .
C9B C 0.6258(2) 1.0604(4) 0.6231(3) 0.0110(10) Uani 1 1 d . . . . .
H9B H 0.5853 1.0921 0.5959 0.013 Uiso 1 1 calc R . . . .
C25 C 0.7334(2) 0.3097(4) 0.1505(3) 0.0098(10) Uani 1 1 d . . . . .
H25 H 0.6889 0.3116 0.1209 0.012 Uiso 1 1 calc R . . . .
C3B C 0.5875(2) 0.6473(4) 0.9477(3) 0.0108(10) Uani 1 1 d . . . . .
H3B H 0.5434 0.6403 0.9557 0.013 Uiso 1 1 calc R . . . .
C26 C 1.0720(2) 0.1005(4) 0.5475(3) 0.0152(11) Uani 1 1 d . . . . .
H26 H 1.0384 0.0962 0.5856 0.018 Uiso 1 1 calc R . . . .
C7B C 0.5216(2) 0.9637(4) 0.7209(3) 0.0106(10) Uani 1 1 d . . . . .
H7B H 0.5040 1.0173 0.6795 0.013 Uiso 1 1 calc R . . . .
C12B C 0.3809(2) 1.0700(4) 0.7104(3) 0.0108(10) Uani 1 1 d . . . . .
H12B H 0.3962 1.0645 0.6539 0.013 Uiso 1 1 calc R . . . .
C17 C 0.8308(2) -0.0826(4) 0.5068(3) 0.0136(11) Uani 1 1 d . . . . .
H17 H 0.8725 -0.0976 0.5419 0.016 Uiso 1 1 calc R . . . .
C14B C 0.3051(2) 1.0856(4) 0.6931(3) 0.0166(11) Uani 1 1 d . . . . .
H14A H 0.2839 1.0255 0.6576 0.025 Uiso 1 1 calc GR . . . .
H14B H 0.2937 1.1541 0.6623 0.025 Uiso 1 1 calc GR . . . .
H14C H 0.2899 1.0871 0.7485 0.025 Uiso 1 1 calc GR . . . .
C26B C 1.0688(2) 0.7922(4) 1.0699(3) 0.0135(10) Uani 1 1 d . . . . .
H26B H 1.0354 0.7986 1.1080 0.016 Uiso 1 1 calc R . . . .
C2B C 0.6408(2) 0.5835(4) 0.9860(3) 0.0134(11) Uani 1 1 d . . . . .
H2B H 0.6406 0.5248 1.0249 0.016 Uiso 1 1 calc R . . . .
C23 C 0.8418(2) 0.3433(4) 0.1848(3) 0.0131(10) Uani 1 1 d . . . . .
H23 H 0.8850 0.3693 0.1852 0.016 Uiso 1 1 calc R . . . .
C24 C 0.7854(2) 0.3696(4) 0.1248(3) 0.0121(10) Uani 1 1 d . . . . .
H24 H 0.7822 0.4174 0.0768 0.015 Uiso 1 1 calc R . . . .
C12 C 0.3766(2) -0.1078(4) 0.2107(3) 0.0122(10) Uani 1 1 d . . . . .
H12 H 0.3912 -0.1028 0.1537 0.015 Uiso 1 1 calc R . . . .
C20B C 0.9556(2) 0.7398(4) 0.9361(3) 0.0125(10) Uani 1 1 d . . . . .
C27 C 1.1380(2) 0.1442(4) 0.6020(3) 0.0222(12) Uani 1 1 d . . . . .
H27D H 1.1706 0.1511 0.5646 0.033 Uiso 1 1 calc GR . . . .
H27E H 1.1543 0.0937 0.6494 0.033 Uiso 1 1 calc GR . . . .
H27F H 1.1305 0.2153 0.6261 0.033 Uiso 1 1 calc GR . . . .
C28B C 1.0821(2) 0.9056(4) 1.0353(3) 0.0185(11) Uani 1 1 d . . . . .
H28A H 1.1166 0.9003 1.0006 0.028 Uiso 1 1 calc GR . . . .
H28B H 1.0966 0.9547 1.0843 0.028 Uiso 1 1 calc GR . . . .
H28C H 1.0417 0.9337 0.9992 0.028 Uiso 1 1 calc GR . . . .
C11B C 0.7325(2) 1.0159(4) 0.6630(3) 0.0102(10) Uani 1 1 d . . . . .
H11B H 0.7787 1.0150 0.6658 0.012 Uiso 1 1 calc R . . . .
C14 C 0.3002(2) -0.1196(4) 0.1949(3) 0.0158(11) Uani 1 1 d . . . . .
H14D H 0.2863 -0.1309 0.2505 0.024 Uiso 1 1 calc GR . . . .
H14E H 0.2866 -0.1817 0.1568 0.024 Uiso 1 1 calc GR . . . .
H14F H 0.2796 -0.0536 0.1675 0.024 Uiso 1 1 calc GR . . . .
C24B C 0.7800(2) 1.0757(4) 1.0200(3) 0.0128(10) Uani 1 1 d . . . . .
H24B H 0.7764 1.1371 1.0551 0.015 Uiso 1 1 calc R . . . .
C29 C 0.9274(2) 0.2576(4) 0.6614(3) 0.0205(11) Uani 1 1 d . . . . .
H29D H 0.9401 0.1871 0.6881 0.031 Uiso 1 1 calc GR . . . .
H29E H 0.9381 0.3147 0.7052 0.031 Uiso 1 1 calc GR . . . .
H29F H 0.9514 0.2705 0.6143 0.031 Uiso 1 1 calc GR . . . .
C25B C 0.7309(2) 1.0339(4) 0.9512(3) 0.0118(10) Uani 1 1 d . . . . .
H25B H 0.6884 1.0644 0.9334 0.014 Uiso 1 1 calc R . . . .
C27B C 1.1327(2) 0.7402(4) 1.1226(3) 0.0180(11) Uani 1 1 d . . . . .
H27A H 1.1227 0.6681 1.1427 0.027 Uiso 1 1 calc GR . . . .
H27B H 1.1502 0.7860 1.1728 0.027 Uiso 1 1 calc GR . . . .
H27C H 1.1656 0.7338 1.0856 0.027 Uiso 1 1 calc GR . . . .
B2B B 0.9453(3) 0.9414(5) 0.7313(3) 0.0149(12) Uani 1 1 d . . . . .
C13 C 0.4112(2) -0.2055(4) 0.2630(3) 0.0158(11) Uani 1 1 d . . . . .
H13D H 0.4588 -0.1927 0.2769 0.024 Uiso 1 1 calc GR . . . .
H13E H 0.4022 -0.2716 0.2281 0.024 Uiso 1 1 calc GR . . . .
H13F H 0.3944 -0.2139 0.3168 0.024 Uiso 1 1 calc GR . . . .
C28 C 1.0801(2) -0.0138(4) 0.5087(3) 0.0219(11) Uani 1 1 d . . . . .
H28D H 1.0386 -0.0357 0.4716 0.033 Uiso 1 1 calc GR . . . .
H28E H 1.0922 -0.0663 0.5559 0.033 Uiso 1 1 calc GR . . . .
H28F H 1.1148 -0.0112 0.4742 0.033 Uiso 1 1 calc GR . . . .
C10B C 0.6878(2) 1.0849(4) 0.6064(3) 0.0131(11) Uani 1 1 d . . . . .
H10B H 0.6983 1.1362 0.5662 0.016 Uiso 1 1 calc R . . . .
B1 B 0.5794(3) 0.2078(5) -0.0286(3) 0.0108(11) Uani 1 1 d . . . . .
C29B C 1.0733(2) 1.1388(5) 0.8126(3) 0.0235(12) Uani 1 1 d . . . . .
H29A H 1.0760 1.0753 0.7760 0.035 Uiso 1 1 calc GR . . . .
H29B H 1.0652 1.2036 0.7761 0.035 Uiso 1 1 calc GR . . . .
H29C H 1.0371 1.1291 0.8440 0.035 Uiso 1 1 calc GR . . . .
B1B B 0.5724(3) 0.7513(5) 0.4700(3) 0.0125(12) Uani 1 1 d . . . . .
B2 B 0.9480(3) -0.0452(5) 0.2484(3) 0.0177(13) Uani 1 1 d . . . . .
O2B O 1.1773(10) 1.226(3) 0.871(3) 0.031(8) Uani 0.54(10) 1 d . . P A 2
O2A O 1.1860(11) 1.185(5) 0.843(2) 0.029(7) Uani 0.46(10) 1 d . . P A 1


_geom_special_details            
;
 All esds (except the esd in the dihedral angle between two l.s. planes)
 are estimated using the full covariance matrix.  The cell esds are taken
 into account individually in the estimation of esds in distances, angles
 and torsion angles; correlations between esds in cell parameters are only
 used when they are defined by crystal symmetry.  An approximate (isotropic)
 treatment of cell esds is used for estimating esds involving l.s. planes.
;
loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
_geom_bond_publ_flag
Fe1B N8B 2.118(4) . ?
Fe1B N3B 2.132(4) . ?
Fe1B N6B 2.158(4) . ?
Fe1B N5B 2.166(4) . ?
Fe1B N10B 2.166(4) . ?
Fe1B N1B 2.215(4) . ?
Fe1 N1 2.210(4) . ?
Fe1 N3 2.126(4) . ?
Fe1 N10 2.182(4) . ?
Fe1 N8 2.119(4) . ?
Fe1 N5 2.167(4) . ?
Fe1 N6 2.172(4) . ?
S1B C6B 1.744(4) . ?
S1B C12B 1.834(5) . ?
S1 C6 1.747(4) . ?
S1 C12 1.825(5) . ?
S2B C26B 1.836(4) . ?
S2B C20B 1.745(4) . ?
S2 C20 1.747(4) . ?
S2 C26 1.825(5) . ?
F2 B1 1.409(5) . ?
F4 B1 1.389(6) . ?
F7B B2B 1.386(6) . ?
F5B B2B 1.404(6) . ?
F3B B1B 1.381(6) . ?
F1 B1 1.405(6) . ?
F3 B1 1.391(6) . ?
F2B B1B 1.413(5) . ?
F8B B2B 1.412(5) . ?
F8 B2 1.388(6) . ?
F5 B2 1.382(6) . ?
F4B B1B 1.407(6) . ?
F1B B1B 1.398(6) . ?
F6B B2B 1.381(6) . ?
F7 B2 1.406(6) . ?
F6 B2 1.409(6) . ?
O1 N11 1.220(5) . ?
N8B C22B 1.337(6) . ?
N8B C18B 1.336(5) . ?
N9 N10 1.374(5) . ?
N9 C22 1.421(5) . ?
N9 C23 1.354(6) . ?
N1 N2 1.373(5) . ?
N1 C1 1.321(6) . ?
N3 C8 1.337(6) . ?
N3 C4 1.344(5) . ?
N3B C8B 1.333(6) . ?
N3B C4B 1.333(5) . ?
N4B N5B 1.378(5) . ?
N4B C8B 1.409(5) . ?
N4B C9B 1.361(6) . ?
O1B N11B 1.217(5) . ?
N10 C25 1.332(6) . ?
N8 C22 1.338(5) . ?
N8 C18 1.325(6) . ?
N6B N7B 1.373(5) . ?
N6B C15B 1.327(6) . ?
N5 N4 1.374(5) . ?
N5 C11 1.327(6) . ?
N2 C3 1.358(5) . ?
N2 C4 1.417(6) . ?
N9B N10B 1.381(5) . ?
N9B C22B 1.412(5) . ?
N9B C23B 1.358(6) . ?
N6 N7 1.377(5) . ?
N6 C15 1.327(6) . ?
N2B N1B 1.372(5) . ?
N2B C4B 1.414(6) . ?
N2B C3B 1.353(5) . ?
N7B C18B 1.409(5) . ?
N7B C17B 1.357(5) . ?
N7 C18 1.400(5) . ?
N7 C17 1.362(6) . ?
N11 O2 1.223(5) . ?
N11 C29 1.485(5) . ?
N5B C11B 1.326(6) . ?
N4 C9 1.354(6) . ?
N4 C8 1.416(5) . ?
N10B C25B 1.329(6) . ?
N1B C1B 1.323(6) . ?
C5B H5B 0.9300 . ?
C5B C4B 1.371(6) . ?
C5B C6B 1.394(6) . ?
C22B C21B 1.378(6) . ?
C22 C21 1.367(6) . ?
C6 C7 1.397(6) . ?
C6 C5 1.403(6) . ?
C15B H15B 0.9300 . ?
C15B C16B 1.402(6) . ?
C8B C7B 1.381(6) . ?
C16 H16 0.9300 . ?
C16 C15 1.402(6) . ?
C16 C17 1.363(6) . ?
C10 H10 0.9300 . ?
C10 C11 1.391(7) . ?
C10 C9 1.374(6) . ?
C7 H7 0.9300 . ?
C7 C8 1.378(6) . ?
C19 H19 0.9300 . ?
C19 C20 1.391(6) . ?
C19 C18 1.386(6) . ?
N11B C29B 1.494(6) . ?
N11B O2B 1.219(14) . ?
N11B O2A 1.27(2) . ?
C11 H11 0.9300 . ?
C18B C19B 1.368(6) . ?
C9 H9 0.9300 . ?
C15 H15 0.9300 . ?
C20 C21 1.413(6) . ?
C21 H21 0.9300 . ?
C23B H23B 0.9300 . ?
C23B C24B 1.356(6) . ?
C3 H3 0.9300 . ?
C3 C2 1.359(6) . ?
C17B H17B 0.9300 . ?
C17B C16B 1.374(6) . ?
C13B H13A 0.9600 . ?
C13B H13B 0.9600 . ?
C13B H13C 0.9600 . ?
C13B C12B 1.514(7) . ?
C4 C5 1.367(6) . ?
C5 H5 0.9300 . ?
C6B C7B 1.413(6) . ?
C1B H1B 0.9300 . ?
C1B C2B 1.401(6) . ?
C19B H19B 0.9300 . ?
C19B C20B 1.404(6) . ?
C16B H16B 0.9300 . ?
C1 H1 0.9300 . ?
C1 C2 1.408(6) . ?
C21B H21B 0.9300 . ?
C21B C20B 1.397(6) . ?
C2 H2 0.9300 . ?
C9B H9B 0.9300 . ?
C9B C10B 1.363(6) . ?
C25 H25 0.9300 . ?
C25 C24 1.399(6) . ?
C3B H3B 0.9300 . ?
C3B C2B 1.366(6) . ?
C26 H26 0.9800 . ?
C26 C27 1.532(6) . ?
C26 C28 1.527(7) . ?
C7B H7B 0.9300 . ?
C12B H12B 0.9800 . ?
C12B C14B 1.522(6) . ?
C17 H17 0.9300 . ?
C14B H14A 0.9600 . ?
C14B H14B 0.9600 . ?
C14B H14C 0.9600 . ?
C26B H26B 0.9800 . ?
C26B C28B 1.514(7) . ?
C26B C27B 1.527(6) . ?
C2B H2B 0.9300 . ?
C23 H23 0.9300 . ?
C23 C24 1.361(6) . ?
C24 H24 0.9300 . ?
C12 H12 0.9800 . ?
C12 C14 1.530(6) . ?
C12 C13 1.522(7) . ?
C27 H27D 0.9600 . ?
C27 H27E 0.9600 . ?
C27 H27F 0.9600 . ?
C28B H28A 0.9600 . ?
C28B H28B 0.9600 . ?
C28B H28C 0.9600 . ?
C11B H11B 0.9300 . ?
C11B C10B 1.405(6) . ?
C14 H14D 0.9600 . ?
C14 H14E 0.9600 . ?
C14 H14F 0.9600 . ?
C24B H24B 0.9300 . ?
C24B C25B 1.401(6) . ?
C29 H29D 0.9600 . ?
C29 H29E 0.9600 . ?
C29 H29F 0.9600 . ?
C25B H25B 0.9300 . ?
C27B H27A 0.9600 . ?
C27B H27B 0.9600 . ?
C27B H27C 0.9600 . ?
C13 H13D 0.9600 . ?
C13 H13E 0.9600 . ?
C13 H13F 0.9600 . ?
C28 H28D 0.9600 . ?
C28 H28E 0.9600 . ?
C28 H28F 0.9600 . ?
C10B H10B 0.9300 . ?
C29B H29A 0.9600 . ?
C29B H29B 0.9600 . ?
C29B H29C 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
N8B Fe1B N3B 167.67(14) . . ?
N8B Fe1B N6B 73.38(13) . . ?
N8B Fe1B N5B 115.64(13) . . ?
N8B Fe1B N10B 73.76(14) . . ?
N8B Fe1B N1B 97.47(13) . . ?
N3B Fe1B N6B 115.14(14) . . ?
N3B Fe1B N5B 73.68(13) . . ?
N3B Fe1B N10B 98.81(14) . . ?
N3B Fe1B N1B 72.92(14) . . ?
N6B Fe1B N5B 94.79(14) . . ?
N6B Fe1B N10B 145.84(13) . . ?
N6B Fe1B N1B 99.06(14) . . ?
N5B Fe1B N10B 91.10(15) . . ?
N5B Fe1B N1B 146.60(13) . . ?
N10B Fe1B N1B 94.15(14) . . ?
N3 Fe1 N1 73.52(13) . . ?
N3 Fe1 N10 115.25(14) . . ?
N3 Fe1 N5 73.54(13) . . ?
N3 Fe1 N6 98.20(14) . . ?
N10 Fe1 N1 96.78(14) . . ?
N8 Fe1 N1 100.81(13) . . ?
N8 Fe1 N3 169.97(13) . . ?
N8 Fe1 N10 73.21(14) . . ?
N8 Fe1 N5 111.42(14) . . ?
N8 Fe1 N6 73.74(14) . . ?
N5 Fe1 N1 146.99(13) . . ?
N5 Fe1 N10 99.09(14) . . ?
N5 Fe1 N6 87.78(15) . . ?
N6 Fe1 N1 94.72(14) . . ?
N6 Fe1 N10 146.47(13) . . ?
C6B S1B C12B 105.2(2) . . ?
C6 S1 C12 105.6(2) . . ?
C20B S2B C26B 105.2(2) . . ?
C20 S2 C26 104.3(2) . . ?
C22B N8B Fe1B 121.0(3) . . ?
C18B N8B Fe1B 121.2(3) . . ?
C18B N8B C22B 117.8(4) . . ?
N10 N9 C22 118.0(3) . . ?
C23 N9 N10 111.2(3) . . ?
C23 N9 C22 130.7(4) . . ?
N2 N1 Fe1 113.7(3) . . ?
C1 N1 Fe1 141.5(3) . . ?
C1 N1 N2 104.9(3) . . ?
C8 N3 Fe1 121.0(3) . . ?
C8 N3 C4 117.3(4) . . ?
C4 N3 Fe1 120.8(3) . . ?
C8B N3B Fe1B 120.2(3) . . ?
C4B N3B Fe1B 121.3(3) . . ?
C4B N3B C8B 118.1(4) . . ?
N5B N4B C8B 117.6(4) . . ?
C9B N4B N5B 111.2(3) . . ?
C9B N4B C8B 131.1(4) . . ?
N9 N10 Fe1 114.9(3) . . ?
C25 N10 Fe1 140.5(3) . . ?
C25 N10 N9 104.5(4) . . ?
C22 N8 Fe1 121.9(3) . . ?
C18 N8 Fe1 120.5(3) . . ?
C18 N8 C22 117.6(4) . . ?
N7B N6B Fe1B 115.1(3) . . ?
C15B N6B Fe1B 139.7(3) . . ?
C15B N6B N7B 105.2(3) . . ?
N4 N5 Fe1 114.6(3) . . ?
C11 N5 Fe1 140.8(3) . . ?
C11 N5 N4 104.6(3) . . ?
N1 N2 C4 118.7(3) . . ?
C3 N2 N1 111.0(4) . . ?
C3 N2 C4 130.2(4) . . ?
N10B N9B C22B 118.1(4) . . ?
C23B N9B N10B 111.1(4) . . ?
C23B N9B C22B 130.4(4) . . ?
N7 N6 Fe1 114.1(3) . . ?
C15 N6 Fe1 140.8(3) . . ?
C15 N6 N7 105.0(4) . . ?
N1B N2B C4B 118.0(3) . . ?
C3B N2B N1B 111.2(4) . . ?
C3B N2B C4B 130.7(4) . . ?
N6B N7B C18B 117.9(3) . . ?
C17B N7B N6B 111.2(3) . . ?
C17B N7B C18B 130.7(4) . . ?
N6 N7 C18 118.0(4) . . ?
C17 N7 N6 110.9(4) . . ?
C17 N7 C18 130.9(4) . . ?
O1 N11 O2 123.4(4) . . ?
O1 N11 C29 118.3(4) . . ?
O2 N11 C29 118.3(4) . . ?
N4B N5B Fe1B 114.9(3) . . ?
C11B N5B Fe1B 140.7(3) . . ?
C11B N5B N4B 104.4(4) . . ?
N5 N4 C8 118.0(3) . . ?
C9 N4 N5 111.1(3) . . ?
C9 N4 C8 130.2(4) . . ?
N9B N10B Fe1B 114.2(3) . . ?
C25B N10B Fe1B 141.2(3) . . ?
C25B N10B N9B 104.5(4) . . ?
N2B N1B Fe1B 114.3(3) . . ?
C1B N1B Fe1B 140.9(3) . . ?
C1B N1B N2B 104.7(3) . . ?
C4B C5B H5B 121.0 . . ?
C4B C5B C6B 118.0(4) . . ?
C6B C5B H5B 121.0 . . ?
N8B C22B N9B 112.3(4) . . ?
N8B C22B C21B 123.9(4) . . ?
C21B C22B N9B 123.8(4) . . ?
N8 C22 N9 111.8(4) . . ?
N8 C22 C21 124.8(4) . . ?
C21 C22 N9 123.4(4) . . ?
C7 C6 S1 124.9(4) . . ?
C7 C6 C5 120.0(4) . . ?
C5 C6 S1 115.1(3) . . ?
N6B C15B H15B 124.4 . . ?
N6B C15B C16B 111.1(4) . . ?
C16B C15B H15B 124.4 . . ?
N3B C8B N4B 113.2(4) . . ?
N3B C8B C7B 124.0(4) . . ?
C7B C8B N4B 122.7(4) . . ?
C15 C16 H16 127.0 . . ?
C17 C16 H16 127.0 . . ?
C17 C16 C15 105.9(4) . . ?
C11 C10 H10 127.4 . . ?
C9 C10 H10 127.4 . . ?
C9 C10 C11 105.2(4) . . ?
C6 C7 H7 121.5 . . ?
C8 C7 C6 117.0(4) . . ?
C8 C7 H7 121.5 . . ?
C20 C19 H19 121.3 . . ?
C18 C19 H19 121.3 . . ?
C18 C19 C20 117.3(4) . . ?
O1B N11B C29B 117.6(4) . . ?
O1B N11B O2B 118.7(17) . . ?
O1B N11B O2A 125.6(9) . . ?
O2B N11B C29B 121.7(10) . . ?
O2A N11B C29B 113.6(10) . . ?
N5 C11 C10 112.0(4) . . ?
N5 C11 H11 124.0 . . ?
C10 C11 H11 124.0 . . ?
N8B C18B N7B 112.1(4) . . ?
N8B C18B C19B 123.8(4) . . ?
C19B C18B N7B 124.1(4) . . ?
N4 C9 C10 107.1(4) . . ?
N4 C9 H9 126.5 . . ?
C10 C9 H9 126.5 . . ?
N3B C4B N2B 113.2(4) . . ?
N3B C4B C5B 123.7(4) . . ?
C5B C4B N2B 123.1(4) . . ?
N6 C15 C16 111.1(4) . . ?
N6 C15 H15 124.4 . . ?
C16 C15 H15 124.4 . . ?
C19 C20 S2 124.3(3) . . ?
C19 C20 C21 120.0(4) . . ?
C21 C20 S2 115.7(3) . . ?
N3 C8 N4 111.9(4) . . ?
N3 C8 C7 124.3(4) . . ?
C7 C8 N4 123.7(4) . . ?
C22 C21 C20 116.5(4) . . ?
C22 C21 H21 121.8 . . ?
C20 C21 H21 121.8 . . ?
N9B C23B H23B 126.4 . . ?
C24B C23B N9B 107.2(4) . . ?
C24B C23B H23B 126.4 . . ?
N2 C3 H3 126.3 . . ?
N2 C3 C2 107.4(4) . . ?
C2 C3 H3 126.3 . . ?
N7B C17B H17B 126.6 . . ?
N7B C17B C16B 106.8(4) . . ?
C16B C17B H17B 126.6 . . ?
H13A C13B H13B 109.5 . . ?
H13A C13B H13C 109.5 . . ?
H13B C13B H13C 109.5 . . ?
C12B C13B H13A 109.5 . . ?
C12B C13B H13B 109.5 . . ?
C12B C13B H13C 109.5 . . ?
N3 C4 N2 112.6(4) . . ?
N3 C4 C5 124.1(4) . . ?
C5 C4 N2 123.4(4) . . ?
C6 C5 H5 121.3 . . ?
C4 C5 C6 117.4(4) . . ?
C4 C5 H5 121.3 . . ?
C5B C6B S1B 116.1(3) . . ?
C5B C6B C7B 119.5(4) . . ?
C7B C6B S1B 124.4(4) . . ?
N1B C1B H1B 124.2 . . ?
N1B C1B C2B 111.6(4) . . ?
C2B C1B H1B 124.2 . . ?
N8 C18 N7 113.5(4) . . ?
N8 C18 C19 123.8(4) . . ?
C19 C18 N7 122.7(4) . . ?
C18B C19B H19B 121.1 . . ?
C18B C19B C20B 117.8(4) . . ?
C20B C19B H19B 121.1 . . ?
C15B C16B H16B 127.1 . . ?
C17B C16B C15B 105.7(4) . . ?
C17B C16B H16B 127.1 . . ?
N1 C1 H1 124.2 . . ?
N1 C1 C2 111.5(4) . . ?
C2 C1 H1 124.2 . . ?
C22B C21B H21B 121.3 . . ?
C22B C21B C20B 117.4(4) . . ?
C20B C21B H21B 121.3 . . ?
C3 C2 C1 105.2(4) . . ?
C3 C2 H2 127.4 . . ?
C1 C2 H2 127.4 . . ?
N4B C9B H9B 126.4 . . ?
N4B C9B C10B 107.3(4) . . ?
C10B C9B H9B 126.4 . . ?
N10 C25 H25 124.3 . . ?
N10 C25 C24 111.4(4) . . ?
C24 C25 H25 124.3 . . ?
N2B C3B H3B 126.4 . . ?
N2B C3B C2B 107.2(4) . . ?
C2B C3B H3B 126.4 . . ?
S2 C26 H26 109.0 . . ?
C27 C26 S2 105.6(3) . . ?
C27 C26 H26 109.0 . . ?
C28 C26 S2 111.9(3) . . ?
C28 C26 H26 109.0 . . ?
C28 C26 C27 112.1(4) . . ?
C8B C7B C6B 116.7(4) . . ?
C8B C7B H7B 121.6 . . ?
C6B C7B H7B 121.6 . . ?
S1B C12B H12B 109.5 . . ?
C13B C12B S1B 110.9(3) . . ?
C13B C12B H12B 109.5 . . ?
C13B C12B C14B 111.7(4) . . ?
C14B C12B S1B 105.7(3) . . ?
C14B C12B H12B 109.5 . . ?
N7 C17 C16 107.0(4) . . ?
N7 C17 H17 126.5 . . ?
C16 C17 H17 126.5 . . ?
C12B C14B H14A 109.5 . . ?
C12B C14B H14B 109.5 . . ?
C12B C14B H14C 109.5 . . ?
H14A C14B H14B 109.5 . . ?
H14A C14B H14C 109.5 . . ?
H14B C14B H14C 109.5 . . ?
S2B C26B H26B 109.2 . . ?
C28B C26B S2B 111.2(3) . . ?
C28B C26B H26B 109.2 . . ?
C28B C26B C27B 111.6(4) . . ?
C27B C26B S2B 106.3(3) . . ?
C27B C26B H26B 109.2 . . ?
C1B C2B H2B 127.4 . . ?
C3B C2B C1B 105.2(4) . . ?
C3B C2B H2B 127.4 . . ?
N9 C23 H23 126.4 . . ?
N9 C23 C24 107.3(4) . . ?
C24 C23 H23 126.4 . . ?
C25 C24 H24 127.2 . . ?
C23 C24 C25 105.5(4) . . ?
C23 C24 H24 127.2 . . ?
S1 C12 H12 109.5 . . ?
C14 C12 S1 106.2(3) . . ?
C14 C12 H12 109.5 . . ?
C13 C12 S1 111.0(3) . . ?
C13 C12 H12 109.5 . . ?
C13 C12 C14 111.2(4) . . ?
C19B C20B S2B 116.2(3) . . ?
C21B C20B S2B 124.4(3) . . ?
C21B C20B C19B 119.3(4) . . ?
C26 C27 H27D 109.5 . . ?
C26 C27 H27E 109.5 . . ?
C26 C27 H27F 109.5 . . ?
H27D C27 H27E 109.5 . . ?
H27D C27 H27F 109.5 . . ?
H27E C27 H27F 109.5 . . ?
C26B C28B H28A 109.5 . . ?
C26B C28B H28B 109.5 . . ?
C26B C28B H28C 109.5 . . ?
H28A C28B H28B 109.5 . . ?
H28A C28B H28C 109.5 . . ?
H28B C28B H28C 109.5 . . ?
N5B C11B H11B 124.1 . . ?
N5B C11B C10B 111.9(4) . . ?
C10B C11B H11B 124.1 . . ?
C12 C14 H14D 109.5 . . ?
C12 C14 H14E 109.5 . . ?
C12 C14 H14F 109.5 . . ?
H14D C14 H14E 109.5 . . ?
H14D C14 H14F 109.5 . . ?
H14E C14 H14F 109.5 . . ?
C23B C24B H24B 127.0 . . ?
C23B C24B C25B 106.0(4) . . ?
C25B C24B H24B 127.0 . . ?
N11 C29 H29D 109.5 . . ?
N11 C29 H29E 109.5 . . ?
N11 C29 H29F 109.5 . . ?
H29D C29 H29E 109.5 . . ?
H29D C29 H29F 109.5 . . ?
H29E C29 H29F 109.5 . . ?
N10B C25B C24B 111.3(4) . . ?
N10B C25B H25B 124.3 . . ?
C24B C25B H25B 124.3 . . ?
C26B C27B H27A 109.5 . . ?
C26B C27B H27B 109.5 . . ?
C26B C27B H27C 109.5 . . ?
H27A C27B H27B 109.5 . . ?
H27A C27B H27C 109.5 . . ?
H27B C27B H27C 109.5 . . ?
F7B B2B F5B 110.3(4) . . ?
F7B B2B F8B 108.9(4) . . ?
F5B B2B F8B 107.5(4) . . ?
F6B B2B F7B 110.1(4) . . ?
F6B B2B F5B 109.8(4) . . ?
F6B B2B F8B 110.2(4) . . ?
C12 C13 H13D 109.5 . . ?
C12 C13 H13E 109.5 . . ?
C12 C13 H13F 109.5 . . ?
H13D C13 H13E 109.5 . . ?
H13D C13 H13F 109.5 . . ?
H13E C13 H13F 109.5 . . ?
C26 C28 H28D 109.5 . . ?
C26 C28 H28E 109.5 . . ?
C26 C28 H28F 109.5 . . ?
H28D C28 H28E 109.5 . . ?
H28D C28 H28F 109.5 . . ?
H28E C28 H28F 109.5 . . ?
C9B C10B C11B 105.3(4) . . ?
C9B C10B H10B 127.4 . . ?
C11B C10B H10B 127.4 . . ?
F4 B1 F2 109.3(4) . . ?
F4 B1 F1 109.6(4) . . ?
F4 B1 F3 110.2(4) . . ?
F1 B1 F2 108.5(3) . . ?
F3 B1 F2 109.1(4) . . ?
F3 B1 F1 110.1(4) . . ?
N11B C29B H29A 109.5 . . ?
N11B C29B H29B 109.5 . . ?
N11B C29B H29C 109.5 . . ?
H29A C29B H29B 109.5 . . ?
H29A C29B H29C 109.5 . . ?
H29B C29B H29C 109.5 . . ?
F3B B1B F2B 110.1(4) . . ?
F3B B1B F4B 110.1(4) . . ?
F3B B1B F1B 110.3(4) . . ?
F4B B1B F2B 108.5(3) . . ?
F1B B1B F2B 108.7(4) . . ?
F1B B1B F4B 109.2(4) . . ?
F8 B2 F7 109.6(4) . . ?
F8 B2 F6 109.4(4) . . ?
F5 B2 F8 110.7(4) . . ?
F5 B2 F7 110.5(5) . . ?
F5 B2 F6 108.9(4) . . ?
F7 B2 F6 107.8(4) . . ?


loop_
_twin_individual_id
_twin_individual_mass_fraction_refined
1 0.517(15)
2 0.483(15)

####################################################################### 
# 
# 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_164sflt
_database_code_depnum_ccdc_archive 'CCDC 1563030'
_audit_update_record             
;
2017-07-18 deposited with the CCDC.
2017-11-20 downloaded from the CCDC.
;

_audit_creation_method           SHELXL-97
_chemical_name_systematic        
Bis[4-(isopropylsulfanyl)-2,6-di(pyrazol-1-yl)pyridine]iron(II)diperchlorate
_chemical_name_common            ?
_chemical_melting_point          ?
_chemical_formula_moiety         'C28 H30 Fe N10 S2, 2(Cl O4)'
_chemical_formula_sum            'C28 H30 Cl2 Fe N10 O8 S2'
_chemical_formula_weight         825.49

loop_
_atom_type_symbol
_atom_type_description
_atom_type_scat_dispersion_real
_atom_type_scat_dispersion_imag
_atom_type_scat_source
Cl Cl 0.3639 0.7018 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
C C 0.0181 0.0091 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Fe Fe -1.1336 3.1974 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
N N 0.0311 0.0180 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
O O 0.0492 0.0322 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
S S 0.3331 0.5567 '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'

_symmetry_cell_setting           monoclinic
_symmetry_space_group_name_H-M   'P 21/c'

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

_cell_length_a                   19.8888(8)
_cell_length_b                   12.0560(5)
_cell_length_c                   15.4109(8)
_cell_angle_alpha                90.00
_cell_angle_beta                 104.145(4)
_cell_angle_gamma                90.00
_cell_volume                     3583.2(3)
_cell_formula_units_Z            4
_cell_measurement_temperature    118(2)
_cell_measurement_reflns_used    6498
_cell_measurement_theta_min      4.33
_cell_measurement_theta_max      73.32

_exptl_crystal_description       'rectangular prism'
_exptl_crystal_colour            brown
_exptl_crystal_size_max          0.18
_exptl_crystal_size_mid          0.14
_exptl_crystal_size_min          0.07
_exptl_crystal_density_meas      ?
_exptl_crystal_density_diffrn    1.530
_exptl_crystal_density_method    'not measured'
_exptl_crystal_F_000             1696
_exptl_absorpt_coefficient_mu    6.376
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_correction_T_min  0.481
_exptl_absorpt_correction_T_max  1.000
_exptl_absorpt_process_details   
; 
CrysAlisPro, Agilent Technologies,
Version 1.171.36.24 (release 03-12-2012 CrysAlis171 .NET)
Empirical absorption correction using spherical harmonics,
 implemented in SCALE3 ABSPACK scaling algorithm.
;

_diffrn_ambient_temperature      118(2)
_diffrn_radiation_wavelength     1.54184
_diffrn_radiation_type           CuK\a
_diffrn_radiation_source         'SuperNova (Cu) X-ray Source'
_diffrn_radiation_monochromator  mirror
_diffrn_measurement_device_type  'SuperNova, Dual, Cu at zero, Atlas'
_diffrn_measurement_method       'ω scans'
_diffrn_detector_area_resol_mean 5.3095
_diffrn_standards_number         0
_diffrn_standards_interval_count 0
_diffrn_standards_interval_time  0
_diffrn_standards_decay_%        0
_diffrn_reflns_number            13667
_diffrn_reflns_av_R_equivalents  0.0422
_diffrn_reflns_av_sigmaI/netI    0.0458
_diffrn_reflns_limit_h_min       -23
_diffrn_reflns_limit_h_max       18
_diffrn_reflns_limit_k_min       -9
_diffrn_reflns_limit_k_max       14
_diffrn_reflns_limit_l_min       -18
_diffrn_reflns_limit_l_max       18
_diffrn_reflns_theta_min         4.32
_diffrn_reflns_theta_max         67.05
_reflns_number_total             6343
_reflns_number_gt                5552
_reflns_threshold_expression     >2sigma(I)

_computing_data_collection       'CrysAlisPro, Agilent Technologies'
_computing_cell_refinement       'CrysAlisPro, Agilent Technologies'
_computing_data_reduction        'CrysAlisPro, Agilent Technologies'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_molecular_graphics    'XSEED (Barbour, 2001)'
_computing_publication_material  'local program'

_refine_special_details          
; 
 Refinement of F² against ALL reflections.  The weighted R-factor wR and 
 goodness of fit S are based on F², conventional R-factors R are based 
 on F, with F set to zero for negative F². The threshold expression of 
 F² > 2sigma(F²) is used only for calculating R-factors(gt) etc. and is 
 not relevant to the choice of reflections for refinement.  R-factors based 
 on F² are statistically about twice as large as those based on F, and R- 
 factors based on ALL data will be even larger. 

 This crystal was produced by heating the acetone solvate of the complex at 
 370 K on the diffractometer for 1 hr.

 One of the ClO₄⁻ ions are disordered over two sites, whose occupancies
 refined to 0.65:0.35. The refined restraints Cl---O = 1.43(2) and O...O = 
 2.34(2) Å were applied to that residue. All fully occupied non-H atoms, 
 plus the major disordered Cl atom, were refined anisotropically, and H atoms 
 were placed in calculated positions and refined using a riding model. The 
 largest residual Fourier peak (+0.95 e.Å⁻³) and hole (-1.12 e.Å⁻³) 
 are both associated with the disordered anion.

 A SQUEEZE analysis of the final model showed 89.6 Å³ of solvent-
 accessible void space in the unit cell, containing just four unresolved 
 electrons.
;

_refine_ls_structure_factor_coef Fsqd
_refine_ls_matrix_type           full
_refine_ls_weighting_scheme      calc
_refine_ls_weighting_details     
'calc w=1/[σ²(Fo²)+(0.1174P)²+3.5325P] 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         6343
_refine_ls_number_parameters     466
_refine_ls_number_restraints     20
_refine_ls_R_factor_all          0.0699
_refine_ls_R_factor_gt           0.0629
_refine_ls_wR_factor_ref         0.1757
_refine_ls_wR_factor_gt          0.1674
_refine_ls_goodness_of_fit_ref   1.020
_refine_ls_restrained_S_all      1.024
_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_symmetry_multiplicity
_atom_site_calc_flag
_atom_site_refinement_flags
_atom_site_disorder_assembly
_atom_site_disorder_group
Fe1 Fe 0.23245(3) 0.61214(5) 0.08473(4) 0.02263(18) Uani 1 1 d . . .
N2 N 0.13465(15) 0.6331(3) 0.0516(2) 0.0249(6) Uani 1 1 d . . .
C3 C 0.10559(19) 0.7095(3) -0.0080(3) 0.0252(7) Uani 1 1 d . . .
C4 C 0.03606(18) 0.7368(3) -0.0275(3) 0.0249(7) Uani 1 1 d . . .
H4 H 0.0170 0.7916 -0.0708 0.030 Uiso 1 1 calc R . .
C5 C -0.00465(18) 0.6802(3) 0.0195(3) 0.0274(8) Uani 1 1 d . . .
C6 C 0.0250(2) 0.5996(3) 0.0837(3) 0.0296(8) Uani 1 1 d . . .
H6 H -0.0021 0.5607 0.1166 0.035 Uiso 1 1 calc R . .
C7 C 0.09453(18) 0.5796(3) 0.0968(3) 0.0257(7) Uani 1 1 d . . .
N8 N 0.15643(15) 0.7607(3) -0.0440(2) 0.0252(6) Uani 1 1 d . . .
N9 N 0.22440(15) 0.7303(2) -0.0072(2) 0.0245(6) Uani 1 1 d . . .
C10 C 0.26215(19) 0.7935(3) -0.0464(3) 0.0283(8) Uani 1 1 d . . .
H10 H 0.3113 0.7911 -0.0344 0.034 Uiso 1 1 calc R . .
C11 C 0.2197(2) 0.8652(3) -0.1085(3) 0.0332(9) Uani 1 1 d . . .
H11 H 0.2344 0.9186 -0.1453 0.040 Uiso 1 1 calc R . .
C12 C 0.1530(2) 0.8423(3) -0.1053(3) 0.0293(8) Uani 1 1 d . . .
H12 H 0.1121 0.8770 -0.1394 0.035 Uiso 1 1 calc R . .
N13 N 0.13411(16) 0.5057(3) 0.1593(2) 0.0278(7) Uani 1 1 d . . .
N14 N 0.20408(16) 0.5023(3) 0.1647(2) 0.0272(7) Uani 1 1 d . . .
C15 C 0.2288(2) 0.4240(3) 0.2247(3) 0.0327(8) Uani 1 1 d . . .
H15 H 0.2761 0.4026 0.2429 0.039 Uiso 1 1 calc R . .
C16 C 0.1751(2) 0.3772(3) 0.2577(3) 0.0361(9) Uani 1 1 d . . .
H16 H 0.1793 0.3204 0.3014 0.043 Uiso 1 1 calc R . .
C17 C 0.1158(2) 0.4301(3) 0.2140(3) 0.0343(9) Uani 1 1 d . . .
H17 H 0.0704 0.4164 0.2208 0.041 Uiso 1 1 calc R . .
S18 S -0.09403(4) 0.69825(8) 0.00589(7) 0.0324(2) Uani 1 1 d . . .
C19 C -0.11601(19) 0.8270(3) -0.0568(3) 0.0302(8) Uani 1 1 d . . .
H19 H -0.0980 0.8248 -0.1119 0.036 Uiso 1 1 calc R . .
C20 C -0.0859(2) 0.9263(3) -0.0001(3) 0.0326(8) Uani 1 1 d . . .
H20A H -0.0973 0.9943 -0.0355 0.049 Uiso 1 1 calc R . .
H20B H -0.0354 0.9185 0.0196 0.049 Uiso 1 1 calc R . .
H20C H -0.1055 0.9304 0.0523 0.049 Uiso 1 1 calc R . .
C21 C -0.1948(2) 0.8316(4) -0.0828(3) 0.0408(10) Uani 1 1 d . . .
H21A H -0.2122 0.8346 -0.0286 0.061 Uiso 1 1 calc R . .
H21B H -0.2130 0.7652 -0.1174 0.061 Uiso 1 1 calc R . .
H21C H -0.2100 0.8978 -0.1192 0.061 Uiso 1 1 calc R . .
N22 N 0.32948(15) 0.5898(3) 0.1294(2) 0.0260(6) Uani 1 1 d . . .
C23 C 0.36264(19) 0.5113(3) 0.0944(3) 0.0274(8) Uani 1 1 d . . .
C24 C 0.4301(2) 0.4823(3) 0.1301(3) 0.0326(9) Uani 1 1 d . . .
H24 H 0.4524 0.4278 0.1025 0.039 Uiso 1 1 calc R . .
C25 C 0.4652(2) 0.5362(3) 0.2089(3) 0.0332(9) Uani 1 1 d . . .
C26 C 0.4316(2) 0.6200(3) 0.2466(3) 0.0315(8) Uani 1 1 d . . .
H26 H 0.4545 0.6589 0.2991 0.038 Uiso 1 1 calc R . .
C27 C 0.36382(19) 0.6425(3) 0.2033(3) 0.0263(7) Uani 1 1 d . . .
N28 N 0.31786(16) 0.4642(3) 0.0188(2) 0.0291(7) Uani 1 1 d . . .
N29 N 0.24930(15) 0.4968(3) 0.0000(2) 0.0266(7) Uani 1 1 d . . .
C30 C 0.2188(2) 0.4445(3) -0.0745(3) 0.0288(8) Uani 1 1 d . . .
H30 H 0.1711 0.4511 -0.1038 0.035 Uiso 1 1 calc R . .
C31 C 0.2662(2) 0.3781(3) -0.1045(3) 0.0335(9) Uani 1 1 d . . .
H31 H 0.2569 0.3325 -0.1563 0.040 Uiso 1 1 calc R . .
C32 C 0.3287(2) 0.3920(3) -0.0441(3) 0.0328(9) Uani 1 1 d . . .
H32 H 0.3714 0.3577 -0.0458 0.039 Uiso 1 1 calc R . .
N33 N 0.32072(15) 0.7210(3) 0.2296(2) 0.0264(6) Uani 1 1 d . . .
N34 N 0.25294(15) 0.7240(3) 0.1803(2) 0.0255(6) Uani 1 1 d . . .
C35 C 0.2246(2) 0.8105(3) 0.2109(3) 0.0299(8) Uani 1 1 d . . .
H35 H 0.1777 0.8333 0.1895 0.036 Uiso 1 1 calc R . .
C36 C 0.2734(2) 0.8636(3) 0.2794(3) 0.0320(8) Uani 1 1 d . . .
H36 H 0.2660 0.9274 0.3120 0.038 Uiso 1 1 calc R . .
C37 C 0.3337(2) 0.8053(3) 0.2897(3) 0.0287(8) Uani 1 1 d . . .
H37 H 0.3766 0.8209 0.3310 0.034 Uiso 1 1 calc R . .
S38 S 0.54902(5) 0.49031(9) 0.25452(9) 0.0448(3) Uani 1 1 d . . .
C39 C 0.5830(2) 0.5774(4) 0.3527(3) 0.0383(9) Uani 1 1 d . . .
H39 H 0.5462 0.5884 0.3858 0.046 Uiso 1 1 calc R . .
C40 C 0.6053(2) 0.6890(4) 0.3246(3) 0.0448(11) Uani 1 1 d . . .
H40A H 0.6233 0.7346 0.3778 0.067 Uiso 1 1 calc R . .
H40B H 0.5654 0.7261 0.2854 0.067 Uiso 1 1 calc R . .
H40C H 0.6416 0.6784 0.2923 0.067 Uiso 1 1 calc R . .
C41 C 0.6420(2) 0.5118(4) 0.4103(4) 0.0466(11) Uani 1 1 d . . .
H41A H 0.6783 0.5010 0.3780 0.070 Uiso 1 1 calc R . .
H41B H 0.6249 0.4395 0.4244 0.070 Uiso 1 1 calc R . .
H41C H 0.6612 0.5525 0.4659 0.070 Uiso 1 1 calc R . .
Cl42A Cl 0.48129(11) 0.7349(2) 0.51749(14) 0.0303(4) Uani 0.65 1 d PD A 1
O43A O 0.5382(4) 0.7719(7) 0.5884(5) 0.083(2) Uiso 0.65 1 d PD A 1
O44A O 0.4910(3) 0.7788(4) 0.4349(3) 0.0432(11) Uiso 0.65 1 d PD A 1
O45A O 0.4184(3) 0.7669(5) 0.5358(4) 0.0512(13) Uiso 0.65 1 d PD A 1
O46A O 0.4838(5) 0.6171(6) 0.5110(6) 0.096(3) Uiso 0.65 1 d PD A 1
Cl42B Cl 0.4686(4) 0.7612(6) 0.5040(5) 0.064(2) Uiso 0.35 1 d PD B 2
O43B O 0.5424(6) 0.7269(13) 0.5362(10) 0.096(5) Uiso 0.35 1 d PD B 2
O44B O 0.4562(6) 0.8587(9) 0.4663(8) 0.069(3) Uiso 0.35 1 d PD B 2
O45B O 0.4397(5) 0.7493(8) 0.5824(6) 0.046(2) Uiso 0.35 1 d PD B 2
O46B O 0.4381(5) 0.6672(8) 0.4483(6) 0.055(2) Uiso 0.35 1 d PD B 2
Cl47 Cl 0.06417(4) 0.97119(8) 0.22698(6) 0.0292(2) Uani 1 1 d . . .
O48 O 0.12906(14) 1.0259(3) 0.2314(2) 0.0366(7) Uani 1 1 d . . .
O49 O 0.00758(14) 1.0478(3) 0.1938(2) 0.0370(7) Uani 1 1 d . . .
O50 O 0.06157(15) 0.9353(3) 0.3156(2) 0.0365(6) Uani 1 1 d . . .
O51 O 0.05765(16) 0.8773(3) 0.1687(2) 0.0416(7) 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 N22 1.903(3) . ?
Fe1 N2 1.903(3) . ?
Fe1 N34 1.965(3) . ?
Fe1 N14 1.983(3) . ?
Fe1 N9 1.987(3) . ?
Fe1 N29 1.991(3) . ?
N2 C3 1.329(5) . ?
N2 C7 1.345(5) . ?
C3 C4 1.381(5) . ?
C3 N8 1.409(5) . ?
C4 C5 1.390(5) . ?
C4 H4 0.9500 . ?
C5 C6 1.409(6) . ?
C5 S18 1.752(4) . ?
C6 C7 1.369(5) . ?
C6 H6 0.9500 . ?
C7 N13 1.404(5) . ?
N8 C12 1.354(5) . ?
N8 N9 1.382(4) . ?
N9 C10 1.316(5) . ?
C10 C11 1.408(6) . ?
C10 H10 0.9500 . ?
C11 C12 1.368(6) . ?
C11 H11 0.9500 . ?
C12 H12 0.9500 . ?
N13 C17 1.350(5) . ?
N13 N14 1.374(4) . ?
N14 C15 1.328(5) . ?
C15 C16 1.407(6) . ?
C15 H15 0.9500 . ?
C16 C17 1.365(6) . ?
C16 H16 0.9500 . ?
C17 H17 0.9500 . ?
S18 C19 1.825(4) . ?
C19 C20 1.517(6) . ?
C19 C21 1.521(5) . ?
C19 H19 1.0000 . ?
C20 H20A 0.9800 . ?
C20 H20B 0.9800 . ?
C20 H20C 0.9800 . ?
C21 H21A 0.9800 . ?
C21 H21B 0.9800 . ?
C21 H21C 0.9800 . ?
N22 C27 1.337(5) . ?
N22 C23 1.340(5) . ?
C23 C24 1.364(5) . ?
C23 N28 1.403(5) . ?
C24 C25 1.404(6) . ?
C24 H24 0.9500 . ?
C25 C26 1.412(6) . ?
C25 S38 1.735(4) . ?
C26 C27 1.376(6) . ?
C26 H26 0.9500 . ?
C27 N33 1.402(5) . ?
N28 C32 1.358(5) . ?
N28 N29 1.380(4) . ?
N29 C30 1.321(5) . ?
C30 C31 1.398(6) . ?
C30 H30 0.9500 . ?
C31 C32 1.369(6) . ?
C31 H31 0.9500 . ?
C32 H32 0.9500 . ?
N33 C37 1.357(5) . ?
N33 N34 1.377(4) . ?
N34 C35 1.327(5) . ?
C35 C36 1.401(6) . ?
C35 H35 0.9500 . ?
C36 C37 1.365(6) . ?
C36 H36 0.9500 . ?
C37 H37 0.9500 . ?
S38 C39 1.829(5) . ?
C39 C41 1.510(6) . ?
C39 C40 1.513(7) . ?
C39 H39 1.0000 . ?
C40 H40A 0.9800 . ?
C40 H40B 0.9800 . ?
C40 H40C 0.9800 . ?
C41 H41A 0.9800 . ?
C41 H41B 0.9800 . ?
C41 H41C 0.9800 . ?
Cl42A O45A 1.402(6) . ?
Cl42A O46A 1.426(8) . ?
Cl42A O44A 1.435(5) . ?
Cl42A O43A 1.439(8) . ?
Cl42B O44B 1.308(11) . ?
Cl42B O46B 1.461(11) . ?
Cl42B O45B 1.466(10) . ?
Cl42B O43B 1.489(12) . ?
Cl47 O51 1.431(3) . ?
Cl47 O48 1.436(3) . ?
Cl47 O50 1.445(3) . ?
Cl47 O49 1.449(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
N22 Fe1 N2 174.47(14) . . ?
N22 Fe1 N34 79.61(13) . . ?
N2 Fe1 N34 96.95(13) . . ?
N22 Fe1 N14 95.60(13) . . ?
N2 Fe1 N14 80.11(13) . . ?
N34 Fe1 N14 91.78(13) . . ?
N22 Fe1 N9 104.92(13) . . ?
N2 Fe1 N9 79.31(13) . . ?
N34 Fe1 N9 90.45(13) . . ?
N14 Fe1 N9 159.42(13) . . ?
N22 Fe1 N29 79.64(13) . . ?
N2 Fe1 N29 103.99(13) . . ?
N34 Fe1 N29 158.99(13) . . ?
N14 Fe1 N29 93.45(13) . . ?
N9 Fe1 N29 91.74(13) . . ?
C3 N2 C7 118.5(3) . . ?
C3 N2 Fe1 121.4(2) . . ?
C7 N2 Fe1 119.6(3) . . ?
N2 C3 C4 123.9(3) . . ?
N2 C3 N8 110.1(3) . . ?
C4 C3 N8 126.0(3) . . ?
C3 C4 C5 116.7(3) . . ?
C3 C4 H4 121.6 . . ?
C5 C4 H4 121.6 . . ?
C4 C5 C6 120.4(3) . . ?
C4 C5 S18 125.4(3) . . ?
C6 C5 S18 114.1(3) . . ?
C7 C6 C5 117.3(3) . . ?
C7 C6 H6 121.3 . . ?
C5 C6 H6 121.3 . . ?
N2 C7 C6 123.0(4) . . ?
N2 C7 N13 110.8(3) . . ?
C6 C7 N13 126.1(3) . . ?
C12 N8 N9 110.9(3) . . ?
C12 N8 C3 132.4(3) . . ?
N9 N8 C3 116.5(3) . . ?
C10 N9 N8 105.6(3) . . ?
C10 N9 Fe1 141.9(3) . . ?
N8 N9 Fe1 112.5(2) . . ?
N9 C10 C11 110.7(3) . . ?
N9 C10 H10 124.7 . . ?
C11 C10 H10 124.7 . . ?
C12 C11 C10 106.1(3) . . ?
C12 C11 H11 126.9 . . ?
C10 C11 H11 126.9 . . ?
N8 C12 C11 106.7(3) . . ?
N8 C12 H12 126.6 . . ?
C11 C12 H12 126.6 . . ?
C17 N13 N14 111.4(3) . . ?
C17 N13 C7 131.7(3) . . ?
N14 N13 C7 116.8(3) . . ?
C15 N14 N13 105.1(3) . . ?
C15 N14 Fe1 142.6(3) . . ?
N13 N14 Fe1 112.3(2) . . ?
N14 C15 C16 110.6(4) . . ?
N14 C15 H15 124.7 . . ?
C16 C15 H15 124.7 . . ?
C17 C16 C15 105.9(4) . . ?
C17 C16 H16 127.0 . . ?
C15 C16 H16 127.0 . . ?
N13 C17 C16 106.9(3) . . ?
N13 C17 H17 126.5 . . ?
C16 C17 H17 126.5 . . ?
C5 S18 C19 105.89(18) . . ?
C20 C19 C21 111.1(3) . . ?
C20 C19 S18 110.9(3) . . ?
C21 C19 S18 105.6(3) . . ?
C20 C19 H19 109.7 . . ?
C21 C19 H19 109.7 . . ?
S18 C19 H19 109.7 . . ?
C19 C20 H20A 109.5 . . ?
C19 C20 H20B 109.5 . . ?
H20A C20 H20B 109.5 . . ?
C19 C20 H20C 109.5 . . ?
H20A C20 H20C 109.5 . . ?
H20B C20 H20C 109.5 . . ?
C19 C21 H21A 109.5 . . ?
C19 C21 H21B 109.5 . . ?
H21A C21 H21B 109.5 . . ?
C19 C21 H21C 109.5 . . ?
H21A C21 H21C 109.5 . . ?
H21B C21 H21C 109.5 . . ?
C27 N22 C23 118.6(3) . . ?
C27 N22 Fe1 120.2(2) . . ?
C23 N22 Fe1 120.6(3) . . ?
N22 C23 C24 123.4(4) . . ?
N22 C23 N28 110.2(3) . . ?
C24 C23 N28 126.3(3) . . ?
C23 C24 C25 117.5(3) . . ?
C23 C24 H24 121.3 . . ?
C25 C24 H24 121.3 . . ?
C24 C25 C26 120.1(4) . . ?
C24 C25 S38 115.4(3) . . ?
C26 C25 S38 124.5(3) . . ?
C27 C26 C25 116.6(4) . . ?
C27 C26 H26 121.7 . . ?
C25 C26 H26 121.7 . . ?
N22 C27 C26 123.7(3) . . ?
N22 C27 N33 110.2(3) . . ?
C26 C27 N33 126.0(4) . . ?
C32 N28 N29 110.7(3) . . ?
C32 N28 C23 132.3(3) . . ?
N29 N28 C23 116.9(3) . . ?
C30 N29 N28 105.4(3) . . ?
C30 N29 Fe1 142.1(3) . . ?
N28 N29 Fe1 112.2(2) . . ?
N29 C30 C31 111.0(4) . . ?
N29 C30 H30 124.5 . . ?
C31 C30 H30 124.5 . . ?
C32 C31 C30 106.2(4) . . ?
C32 C31 H31 126.9 . . ?
C30 C31 H31 126.9 . . ?
N28 C32 C31 106.7(3) . . ?
N28 C32 H32 126.7 . . ?
C31 C32 H32 126.7 . . ?
C37 N33 N34 110.7(3) . . ?
C37 N33 C27 132.5(3) . . ?
N34 N33 C27 116.3(3) . . ?
C35 N34 N33 105.6(3) . . ?
C35 N34 Fe1 141.1(3) . . ?
N33 N34 Fe1 113.0(2) . . ?
N34 C35 C36 110.5(3) . . ?
N34 C35 H35 124.8 . . ?
C36 C35 H35 124.8 . . ?
C37 C36 C35 106.3(3) . . ?
C37 C36 H36 126.9 . . ?
C35 C36 H36 126.9 . . ?
N33 C37 C36 106.9(4) . . ?
N33 C37 H37 126.5 . . ?
C36 C37 H37 126.5 . . ?
C25 S38 C39 106.0(2) . . ?
C41 C39 C40 113.2(4) . . ?
C41 C39 S38 105.3(3) . . ?
C40 C39 S38 110.4(3) . . ?
C41 C39 H39 109.3 . . ?
C40 C39 H39 109.3 . . ?
S38 C39 H39 109.3 . . ?
C39 C40 H40A 109.5 . . ?
C39 C40 H40B 109.5 . . ?
H40A C40 H40B 109.5 . . ?
C39 C40 H40C 109.5 . . ?
H40A C40 H40C 109.5 . . ?
H40B C40 H40C 109.5 . . ?
C39 C41 H41A 109.5 . . ?
C39 C41 H41B 109.5 . . ?
H41A C41 H41B 109.5 . . ?
C39 C41 H41C 109.5 . . ?
H41A C41 H41C 109.5 . . ?
H41B C41 H41C 109.5 . . ?
O45A Cl42A O46A 109.6(4) . . ?
O45A Cl42A O44A 113.4(4) . . ?
O46A Cl42A O44A 106.9(4) . . ?
O45A Cl42A O43A 109.7(4) . . ?
O46A Cl42A O43A 109.1(5) . . ?
O44A Cl42A O43A 108.0(4) . . ?
O44B Cl42B O46B 115.5(8) . . ?
O44B Cl42B O45B 112.7(8) . . ?
O46B Cl42B O45B 102.6(7) . . ?
O44B Cl42B O43B 117.5(9) . . ?
O46B Cl42B O43B 102.4(8) . . ?
O45B Cl42B O43B 104.5(8) . . ?
O51 Cl47 O48 109.64(19) . . ?
O51 Cl47 O50 109.7(2) . . ?
O48 Cl47 O50 109.37(18) . . ?
O51 Cl47 O49 109.84(18) . . ?
O48 Cl47 O49 109.60(18) . . ?
O50 Cl47 O49 108.66(17) . . ?

_diffrn_measured_fraction_theta_max 0.989
_diffrn_reflns_theta_full        67.05
_diffrn_measured_fraction_theta_full 0.989
_refine_diff_density_max         0.946
_refine_diff_density_min         -1.117
_refine_diff_density_rms         0.111
_exptl_crystal_recrystallization_method 
'SC-SC removal of lattice water by annealing at 375 K on the diffractometer'
_exptl_crystal_preparation       'Magnetic properties'
####################################################################### 
# 
# This file contains crystal structure data downloaded from the 
# Cambridge Structural Database (CSD) hosted by the Cambridge 
# Crystallographic Data Centre (CCDC).
# 
# Full information about CCDC data access policies and citation 
# guidelines are available at http://www.ccdc.cam.ac.uk/access/V1 
# 
# Audit and citation data items may have been added by the CCDC. 
# Please retain this information to preserve the provenance of 
# this file and to allow appropriate attribution of the data. 
# 
#######################################################################

data_164meht
_database_code_depnum_ccdc_archive 'CCDC 1428761'
_audit_update_record             
;
2015-09-30 deposited with the CCDC.
2017-11-20 downloaded from the CCDC.
;

_audit_creation_method           SHELXL-97
_chemical_name_systematic        
'Bis[4-(isopropylsulfanyl)-2,6-di(pyrazol-1-yl)pyridine]iron(II)diperchlorate acetonitrile solvate'
_chemical_name_common            ?
_chemical_melting_point          ?
_chemical_formula_moiety         'C28 H30 Fe N10 S2, 2(Cl O4), C2 H3 N'
_chemical_formula_sum            'C30 H33 Cl2 Fe N11 O8 S2'
_chemical_formula_weight         866.54

loop_
_atom_type_symbol
_atom_type_description
_atom_type_scat_dispersion_real
_atom_type_scat_dispersion_imag
_atom_type_scat_source
Cl Cl 0.3639 0.7018 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
C C 0.0181 0.0091 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
O O 0.0492 0.0322 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Fe Fe -1.1336 3.1974 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
N N 0.0311 0.0180 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
S S 0.3331 0.5567 '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'

_symmetry_cell_setting           monoclinic
_symmetry_space_group_name_H-M   'P 21/c'

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

_cell_length_a                   20.4279(4)
_cell_length_b                   11.9512(3)
_cell_length_c                   16.1688(5)
_cell_angle_alpha                90.00
_cell_angle_beta                 100.738(2)
_cell_angle_gamma                90.00
_cell_volume                     3878.29(17)
_cell_formula_units_Z            4
_cell_measurement_temperature    250(2)
_cell_measurement_reflns_used    7745
_cell_measurement_theta_min      3.83
_cell_measurement_theta_max      73.74

_exptl_crystal_description       plate
_exptl_crystal_colour            yellow
_exptl_crystal_size_max          0.28
_exptl_crystal_size_mid          0.20
_exptl_crystal_size_min          0.06
_exptl_crystal_density_meas      ?
_exptl_crystal_density_diffrn    1.484
_exptl_crystal_density_method    'not measured'
_exptl_crystal_F_000             1784
_exptl_absorpt_coefficient_mu    5.928
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_correction_T_min  0.463
_exptl_absorpt_correction_T_max  1.000
_exptl_absorpt_process_details   
; 
CrysAlisPro, Agilent Technologies,
Version 1.171.36.24 (release 03-12-2012 CrysAlis171 .NET)
Empirical absorption correction using spherical harmonics,
 implemented in SCALE3 ABSPACK scaling algorithm.
;

_diffrn_ambient_temperature      250(2)
_diffrn_radiation_wavelength     1.54184
_diffrn_radiation_type           CuK\a
_diffrn_radiation_source         'SuperNova (Cu) X-ray Source'
_diffrn_radiation_monochromator  mirror
_diffrn_measurement_device_type  'SuperNova, Dual, Cu at zero, Atlas'
_diffrn_measurement_method       'ω scans'
_diffrn_detector_area_resol_mean 5.3095
_diffrn_standards_number         0
_diffrn_standards_interval_count 0
_diffrn_standards_interval_time  0
_diffrn_standards_decay_%        0
_diffrn_reflns_number            15386
_diffrn_reflns_av_R_equivalents  0.0365
_diffrn_reflns_av_sigmaI/netI    0.0415
_diffrn_reflns_limit_h_min       -24
_diffrn_reflns_limit_h_max       25
_diffrn_reflns_limit_k_min       -14
_diffrn_reflns_limit_k_max       13
_diffrn_reflns_limit_l_min       -19
_diffrn_reflns_limit_l_max       15
_diffrn_reflns_theta_min         4.41
_diffrn_reflns_theta_max         74.93
_reflns_number_total             7395
_reflns_number_gt                6262
_reflns_threshold_expression     >2sigma(I)

_computing_data_collection       'CrysAlisPro, Agilent Technologies'
_computing_cell_refinement       'CrysAlisPro, Agilent Technologies'
_computing_data_reduction        'CrysAlisPro, Agilent Technologies'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_molecular_graphics    'XSEED (Barbour, 2001)'
_computing_publication_material  'local program'

_refine_special_details          
; 
 Refinement of F² against ALL reflections.  The weighted R-factor wR and 
 goodness of fit S are based on F², conventional R-factors R are based 
 on F, with F set to zero for negative F². The threshold expression of 
 F² > 2sigma(F²) is used only for calculating R-factors(gt) etc. and is 
 not relevant to the choice of reflections for refinement.  R-factors based 
 on F² are statistically about twice as large as those based on F, and R- 
 factors based on ALL data will be even larger. 

 One of the isopropyl substitutents on the complex cation is disordered over 
 two equally occupied orientations, which were modelled using the fixed 
 restraints C---S = 1.82(2), C---C = 1.52(2), 1,3-C---C---C = 2.48(2) and 
 1,3-C---S---C = 2.83(2) Å. Both ClO₄⁻ ions are also disordered, one 
 over two sites and the other over three. The refined restraints Cl---O = 
 1.43(2) and O...O = 2.34(2) Å were applied to those residues. Finally, 
 the acetonitrile molecule is also disordered and was refined with three 
 sites with occupancies of 0.40, 0.40 and 0.20. These were modelled with 
 the fixed restraints C---C = 1.48(2), C---N = 1.15(2) and 1,3-C...N = 
 2.63(2) Å. 

 All fully occupied non-H atoms, plus the two half-occupied Cl atoms, 
 were refined anisotropically, and H atoms were placed in calculated 
 positions and refined using a riding model. 
;

_refine_ls_structure_factor_coef Fsqd
_refine_ls_matrix_type           full
_refine_ls_weighting_scheme      calc
_refine_ls_weighting_details     
'calc w=1/[σ²(Fo²)+(0.0720P)²+2.9770P] 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         7395
_refine_ls_number_parameters     519
_refine_ls_number_restraints     67
_refine_ls_R_factor_all          0.0627
_refine_ls_R_factor_gt           0.0528
_refine_ls_wR_factor_ref         0.1485
_refine_ls_wR_factor_gt          0.1361
_refine_ls_goodness_of_fit_ref   1.082
_refine_ls_restrained_S_all      1.101
_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_symmetry_multiplicity
_atom_site_calc_flag
_atom_site_refinement_flags
_atom_site_disorder_assembly
_atom_site_disorder_group
Fe1 Fe 0.22200(2) 0.60447(4) 0.05897(3) 0.03628(15) Uani 1 1 d . . .
N2 N 0.11641(11) 0.6286(2) 0.03500(16) 0.0337(5) Uani 1 1 d . . .
C3 C 0.08851(13) 0.7058(3) -0.01936(18) 0.0316(6) Uani 1 1 d . . .
C4 C 0.02196(14) 0.7376(3) -0.0297(2) 0.0385(7) Uani 1 1 d . . .
H4 H 0.0036 0.7913 -0.0699 0.046 Uiso 1 1 calc R . .
C5 C -0.01608(14) 0.6860(3) 0.0224(2) 0.0391(7) Uani 1 1 d . . .
C6 C 0.01261(15) 0.6048(3) 0.0797(2) 0.0421(7) Uani 1 1 d . . .
H6 H -0.0125 0.5684 0.1149 0.051 Uiso 1 1 calc R . .
C7 C 0.07850(14) 0.5796(3) 0.0832(2) 0.0364(6) Uani 1 1 d . . .
N8 N 0.13367(11) 0.7542(2) -0.06492(16) 0.0343(5) Uani 1 1 d . . .
N9 N 0.19985(12) 0.7300(2) -0.03989(17) 0.0389(6) Uani 1 1 d . . .
C10 C 0.23059(16) 0.7924(3) -0.0888(2) 0.0500(9) Uani 1 1 d . . .
H10 H 0.2770 0.7945 -0.0853 0.060 Uiso 1 1 calc R . .
C11 C 0.18520(18) 0.8542(4) -0.1459(2) 0.0536(9) Uani 1 1 d . . .
H11 H 0.1948 0.9037 -0.1872 0.064 Uiso 1 1 calc R . .
C12 C 0.12408(16) 0.8280(3) -0.1295(2) 0.0435(7) Uani 1 1 d . . .
H12 H 0.0829 0.8560 -0.1577 0.052 Uiso 1 1 calc R . .
N13 N 0.11287(13) 0.4992(2) 0.13841(17) 0.0401(6) Uani 1 1 d . . .
N14 N 0.17993(13) 0.4866(3) 0.14104(18) 0.0420(6) Uani 1 1 d . . .
C15 C 0.19733(19) 0.4022(3) 0.1927(2) 0.0531(9) Uani 1 1 d . . .
H15 H 0.2411 0.3746 0.2070 0.064 Uiso 1 1 calc R . .
C16 C 0.1434(2) 0.3586(4) 0.2238(3) 0.0603(10) Uani 1 1 d . . .
H16 H 0.1436 0.2985 0.2614 0.072 Uiso 1 1 calc R . .
C17 C 0.09004(19) 0.4228(3) 0.1876(2) 0.0521(9) Uani 1 1 d . . .
H17 H 0.0458 0.4149 0.1955 0.063 Uiso 1 1 calc R . .
S18 S -0.10073(4) 0.71080(9) 0.02050(7) 0.0529(2) Uani 1 1 d . . .
C19 C -0.11939(16) 0.8430(3) -0.0346(2) 0.0496(8) Uani 1 1 d . . .
H19 H -0.1040 0.8396 -0.0891 0.060 Uiso 1 1 calc R . .
C20 C -0.0859(2) 0.9394(4) 0.0160(3) 0.0689(12) Uani 1 1 d . . .
H20A H -0.0955 1.0082 -0.0158 0.103 Uiso 1 1 calc R . .
H20B H -0.0381 0.9271 0.0282 0.103 Uiso 1 1 calc R . .
H20C H -0.1024 0.9452 0.0684 0.103 Uiso 1 1 calc R . .
C21 C -0.19491(19) 0.8538(5) -0.0511(4) 0.0758(14) Uani 1 1 d . . .
H21A H -0.2102 0.8587 0.0021 0.114 Uiso 1 1 calc R . .
H21B H -0.2147 0.7889 -0.0820 0.114 Uiso 1 1 calc R . .
H21C H -0.2080 0.9209 -0.0838 0.114 Uiso 1 1 calc R . .
N22 N 0.32439(11) 0.5778(2) 0.11141(15) 0.0306(5) Uani 1 1 d . . .
C23 C 0.35952(14) 0.4985(3) 0.08130(19) 0.0339(6) Uani 1 1 d . . .
C24 C 0.42465(15) 0.4737(3) 0.1155(2) 0.0380(7) Uani 1 1 d . . .
H24 H 0.4479 0.4169 0.0930 0.046 Uiso 1 1 calc R . .
C25 C 0.45484(14) 0.5365(3) 0.1852(2) 0.0390(7) Uani 1 1 d . A .
C26 C 0.41963(15) 0.6204(3) 0.2170(2) 0.0386(7) Uani 1 1 d . . .
H26 H 0.4391 0.6636 0.2637 0.046 Uiso 1 1 calc R . .
C27 C 0.35474(14) 0.6374(3) 0.17695(18) 0.0323(6) Uani 1 1 d . . .
N28 N 0.32271(11) 0.4445(2) 0.01019(16) 0.0351(5) Uani 1 1 d . . .
N29 N 0.25832(11) 0.4767(2) -0.01740(16) 0.0355(6) Uani 1 1 d . . .
C30 C 0.23762(16) 0.4174(3) -0.0863(2) 0.0432(7) Uani 1 1 d . . .
H30 H 0.1946 0.4217 -0.1190 0.052 Uiso 1 1 calc R . .
C31 C 0.28761(18) 0.3480(4) -0.1039(2) 0.0558(10) Uani 1 1 d . . .
H31 H 0.2851 0.2979 -0.1491 0.067 Uiso 1 1 calc R . .
C32 C 0.34160(18) 0.3682(3) -0.0412(2) 0.0508(9) Uani 1 1 d . . .
H32 H 0.3838 0.3347 -0.0354 0.061 Uiso 1 1 calc R . .
N33 N 0.31337(12) 0.7210(2) 0.20094(16) 0.0349(5) Uani 1 1 d . . .
N34 N 0.24969(12) 0.7297(2) 0.15662(17) 0.0403(6) Uani 1 1 d . . .
C35 C 0.22436(17) 0.8176(3) 0.1895(2) 0.0498(9) Uani 1 1 d . . .
H35 H 0.1808 0.8446 0.1714 0.060 Uiso 1 1 calc R . .
C36 C 0.27057(19) 0.8650(3) 0.2546(3) 0.0538(9) Uani 1 1 d . . .
H36 H 0.2643 0.9274 0.2876 0.065 Uiso 1 1 calc R . .
C37 C 0.32664(17) 0.8017(3) 0.2601(2) 0.0429(7) Uani 1 1 d . . .
H37 H 0.3670 0.8123 0.2981 0.052 Uiso 1 1 calc R . .
S38 S 0.53683(4) 0.49725(9) 0.22844(7) 0.0615(3) Uani 1 1 d D . .
C39A C 0.5688(4) 0.6207(7) 0.2971(5) 0.0406(18) Uiso 0.50 1 d PD A 1
H39A H 0.5373 0.6372 0.3352 0.049 Uiso 0.50 1 calc PR A 1
C40A C 0.5780(5) 0.7232(9) 0.2484(7) 0.066(3) Uiso 0.50 1 d PD A 1
H40A H 0.5353 0.7470 0.2166 0.099 Uiso 0.50 1 calc PR A 1
H40B H 0.6081 0.7071 0.2101 0.099 Uiso 0.50 1 calc PR A 1
H40C H 0.5967 0.7822 0.2868 0.099 Uiso 0.50 1 calc PR A 1
C41A C 0.6338(5) 0.5772(9) 0.3489(6) 0.067(2) Uiso 0.50 1 d PD A 1
H41A H 0.6250 0.5104 0.3791 0.100 Uiso 0.50 1 calc PR A 1
H41B H 0.6533 0.6341 0.3888 0.100 Uiso 0.50 1 calc PR A 1
H41C H 0.6645 0.5594 0.3117 0.100 Uiso 0.50 1 calc PR A 1
C39B C 0.5664(3) 0.5896(7) 0.3131(5) 0.0373(17) Uiso 0.50 1 d PD A 2
H39B H 0.5310 0.6025 0.3462 0.045 Uiso 0.50 1 calc PR A 2
C40B C 0.5833(5) 0.6986(9) 0.2743(7) 0.069(3) Uiso 0.50 1 d PD A 2
H40D H 0.5435 0.7290 0.2393 0.104 Uiso 0.50 1 calc PR A 2
H40E H 0.6169 0.6853 0.2403 0.104 Uiso 0.50 1 calc PR A 2
H40F H 0.6002 0.7516 0.3187 0.104 Uiso 0.50 1 calc PR A 2
C41B C 0.6264(4) 0.5394(8) 0.3687(5) 0.0517(18) Uiso 0.50 1 d PD A 2
H41D H 0.6138 0.4700 0.3926 0.078 Uiso 0.50 1 calc PR A 2
H41E H 0.6435 0.5913 0.4136 0.078 Uiso 0.50 1 calc PR A 2
H41F H 0.6605 0.5244 0.3356 0.078 Uiso 0.50 1 calc PR A 2
Cl42A Cl 0.4404(5) 0.7726(10) 0.4780(7) 0.045(5) Uiso 0.34 1 d PD B 1
O43A O 0.4945(4) 0.8054(9) 0.5458(6) 0.054(2) Uiso 0.34 1 d PD B 1
O44A O 0.3926(6) 0.8603(10) 0.4499(7) 0.042(2) Uiso 0.34 1 d PD B 1
O45A O 0.4082(6) 0.6807(11) 0.5064(8) 0.091(4) Uiso 0.34 1 d PD B 1
O46A O 0.4721(6) 0.7481(10) 0.4065(7) 0.068(4) Uiso 0.34 1 d PD B 1
Cl42B Cl 0.4414(3) 0.7872(6) 0.4762(5) 0.043(3) Uiso 0.33 1 d PD C 2
O43B O 0.4641(6) 0.7193(11) 0.4148(6) 0.050(3) Uiso 0.33 1 d PD C 2
O44B O 0.4961(4) 0.8417(9) 0.5307(7) 0.048(2) Uiso 0.33 1 d PD C 2
O45B O 0.4058(6) 0.8800(9) 0.4409(8) 0.075(5) Uiso 0.33 1 d PD C 2
O46B O 0.4063(6) 0.7202(10) 0.5302(8) 0.071(3) Uiso 0.33 1 d PD C 2
Cl42C Cl 0.4408(3) 0.7596(6) 0.4844(4) 0.041(2) Uiso 0.33 1 d PD D 3
O43C O 0.4442(6) 0.6933(10) 0.4113(7) 0.082(4) Uiso 0.33 1 d PD D 3
O44C O 0.5017(5) 0.8157(13) 0.5123(9) 0.084(4) Uiso 0.33 1 d PD D 3
O45C O 0.4258(5) 0.6880(10) 0.5463(7) 0.070(3) Uiso 0.33 1 d PD D 3
O46C O 0.3830(5) 0.8334(9) 0.4592(7) 0.059(4) Uiso 0.33 1 d PD D 3
Cl47A Cl 0.0776(3) 0.9878(9) 0.2310(4) 0.0520(17) Uani 0.50 1 d PD E 1
O48A O 0.1404(3) 1.0309(6) 0.2213(5) 0.056(2) Uiso 0.50 1 d PD E 1
O49A O 0.0201(3) 1.0566(6) 0.2032(5) 0.067(2) Uiso 0.50 1 d PD E 1
O50A O 0.0835(3) 0.9672(6) 0.3190(4) 0.0520(16) Uiso 0.50 1 d PD E 1
O51A O 0.0648(4) 0.8869(6) 0.1811(5) 0.070(2) Uiso 0.50 1 d PD E 1
Cl47B Cl 0.0778(3) 1.0009(9) 0.2295(4) 0.0534(18) Uani 0.50 1 d PD F 2
O48B O 0.1410(3) 1.0583(7) 0.2352(5) 0.061(2) Uiso 0.50 1 d PD F 2
O49B O 0.0309(3) 1.0916(6) 0.2157(5) 0.0626(18) Uiso 0.50 1 d PD F 2
O50B O 0.0725(4) 0.9373(6) 0.3055(4) 0.064(2) Uiso 0.50 1 d PD F 2
O51B O 0.0698(4) 0.9221(6) 0.1618(4) 0.070(2) Uiso 0.50 1 d PD F 2
C52A C 0.5649(7) 0.5607(14) 0.5845(11) 0.053(3) Uiso 0.40 1 d PD G 1
H52A H 0.5533 0.6114 0.5371 0.080 Uiso 0.40 1 calc PR G 1
H52B H 0.5450 0.5871 0.6309 0.080 Uiso 0.40 1 calc PR G 1
H52C H 0.5482 0.4865 0.5680 0.080 Uiso 0.40 1 calc PR G 1
C53A C 0.6382(6) 0.5565(16) 0.6110(10) 0.065(4) Uiso 0.40 1 d PD G 1
N54A N 0.6927(6) 0.5622(15) 0.6408(10) 0.104(4) Uiso 0.40 1 d PD G 1
C52B C 0.5749(7) 0.5621(16) 0.5604(10) 0.084(6) Uiso 0.40 1 d PD H 2
H52G H 0.5565 0.4916 0.5371 0.126 Uiso 0.40 1 calc PR H 2
H52H H 0.5901 0.6053 0.5168 0.126 Uiso 0.40 1 calc PR H 2
H52I H 0.5409 0.6038 0.5818 0.126 Uiso 0.40 1 calc PR H 2
C53B C 0.6317(7) 0.5401(16) 0.6299(11) 0.064(5) Uiso 0.40 1 d PD H 2
N54B N 0.6822(6) 0.5192(11) 0.6689(8) 0.080(3) Uiso 0.40 1 d PD H 2
C52C C 0.5519(15) 0.549(5) 0.591(3) 0.12(2) Uiso 0.20 1 d PD I 3
H52D H 0.5348 0.4875 0.6202 0.174 Uiso 0.20 1 calc PR I 3
H52E H 0.5529 0.5276 0.5338 0.174 Uiso 0.20 1 calc PR I 3
H52F H 0.5233 0.6138 0.5915 0.174 Uiso 0.20 1 calc PR I 3
C53C C 0.6209(11) 0.577(3) 0.6356(16) 0.059(6) Uiso 0.20 1 d PD I 3
N54C N 0.6676(10) 0.582(2) 0.6861(14) 0.079(6) Uiso 0.20 1 d PD I 3


_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 N22 2.129(2) . ?
Fe1 N2 2.139(2) . ?
Fe1 N34 2.173(3) . ?
Fe1 N9 2.178(3) . ?
Fe1 N29 2.179(3) . ?
Fe1 N14 2.215(3) . ?
N2 C3 1.327(4) . ?
N2 C7 1.333(4) . ?
C3 C4 1.391(4) . ?
C3 N8 1.408(4) . ?
C4 C5 1.393(5) . ?
C4 H4 0.9400 . ?
C5 C6 1.393(5) . ?
C5 S18 1.749(3) . ?
C6 C7 1.370(4) . ?
C6 H6 0.9400 . ?
C7 N13 1.407(4) . ?
N8 C12 1.353(4) . ?
N8 N9 1.368(3) . ?
N9 C10 1.326(4) . ?
C10 C11 1.393(5) . ?
C10 H10 0.9400 . ?
C11 C12 1.360(5) . ?
C11 H11 0.9400 . ?
C12 H12 0.9400 . ?
N13 C17 1.350(5) . ?
N13 N14 1.371(4) . ?
N14 C15 1.316(5) . ?
C15 C16 1.394(6) . ?
C15 H15 0.9400 . ?
C16 C17 1.372(6) . ?
C16 H16 0.9400 . ?
C17 H17 0.9400 . ?
S18 C19 1.819(4) . ?
C19 C20 1.502(6) . ?
C19 C21 1.521(5) . ?
C19 H19 0.9900 . ?
C20 H20A 0.9700 . ?
C20 H20B 0.9700 . ?
C20 H20C 0.9700 . ?
C21 H21A 0.9700 . ?
C21 H21B 0.9700 . ?
C21 H21C 0.9700 . ?
N22 C27 1.330(4) . ?
N22 C23 1.335(4) . ?
C23 C24 1.375(4) . ?
C23 N28 1.408(4) . ?
C24 C25 1.398(5) . ?
C24 H24 0.9400 . ?
C25 C26 1.387(5) . ?
C25 S38 1.755(3) . ?
C26 C27 1.378(4) . ?
C26 H26 0.9400 . ?
C27 N33 1.409(4) . ?
N28 C32 1.338(4) . ?
N28 N29 1.363(3) . ?
N29 C30 1.321(4) . ?
C30 C31 1.385(5) . ?
C30 H30 0.9400 . ?
C31 C32 1.373(5) . ?
C31 H31 0.9400 . ?
C32 H32 0.9400 . ?
N33 C37 1.351(4) . ?
N33 N34 1.367(3) . ?
N34 C35 1.326(4) . ?
C35 C36 1.395(5) . ?
C35 H35 0.9400 . ?
C36 C37 1.361(5) . ?
C36 H36 0.9400 . ?
C37 H37 0.9400 . ?
S38 C39B 1.774(7) . ?
S38 C39A 1.889(7) . ?
C39A C40A 1.486(11) . ?
C39A C41A 1.523(10) . ?
C39A H39A 0.9900 . ?
C40A H40A 0.9700 . ?
C40A H40B 0.9700 . ?
C40A H40C 0.9700 . ?
C41A H41A 0.9700 . ?
C41A H41B 0.9700 . ?
C41A H41C 0.9700 . ?
C39B C41B 1.502(9) . ?
C39B C40B 1.514(11) . ?
C39B H39B 0.9900 . ?
C40B H40D 0.9700 . ?
C40B H40E 0.9700 . ?
C40B H40F 0.9700 . ?
C41B H41D 0.9700 . ?
C41B H41E 0.9700 . ?
C41B H41F 0.9700 . ?
Cl42A O45A 1.401(13) . ?
Cl42A O44A 1.447(12) . ?
Cl42A O43A 1.457(12) . ?
Cl42A O46A 1.457(12) . ?
Cl42B O45B 1.389(11) . ?
Cl42B O43B 1.425(10) . ?
Cl42B O44B 1.443(10) . ?
Cl42B O46B 1.466(11) . ?
Cl42C O45C 1.394(11) . ?
Cl42C O44C 1.412(11) . ?
Cl42C O43C 1.434(11) . ?
Cl42C O46C 1.470(10) . ?
Cl47A O48A 1.417(9) . ?
Cl47A O50A 1.427(8) . ?
Cl47A O49A 1.436(9) . ?
Cl47A O51A 1.447(10) . ?
Cl47B O51B 1.431(9) . ?
Cl47B O49B 1.436(10) . ?
Cl47B O48B 1.449(9) . ?
Cl47B O50B 1.466(10) . ?
C52A C53A 1.481(13) . ?
C52A H52A 0.9700 . ?
C52A H52B 0.9700 . ?
C52A H52C 0.9700 . ?
C53A N54A 1.130(13) . ?
C52B C53B 1.480(14) . ?
C52B H52G 0.9700 . ?
C52B H52H 0.9700 . ?
C52B H52I 0.9700 . ?
C53B N54B 1.133(13) . ?
C52C C53C 1.495(17) . ?
C52C H52D 0.9700 . ?
C52C H52E 0.9700 . ?
C52C H52F 0.9700 . ?
C53C N54C 1.138(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
N22 Fe1 N2 167.15(10) . . ?
N22 Fe1 N34 73.15(9) . . ?
N2 Fe1 N34 98.97(10) . . ?
N22 Fe1 N9 116.72(9) . . ?
N2 Fe1 N9 73.10(9) . . ?
N34 Fe1 N9 92.81(11) . . ?
N22 Fe1 N29 73.02(9) . . ?
N2 Fe1 N29 115.49(10) . . ?
N34 Fe1 N29 145.54(9) . . ?
N9 Fe1 N29 96.49(10) . . ?
N22 Fe1 N14 97.37(9) . . ?
N2 Fe1 N14 72.77(10) . . ?
N34 Fe1 N14 94.60(11) . . ?
N9 Fe1 N14 145.79(9) . . ?
N29 Fe1 N14 96.04(11) . . ?
C3 N2 C7 117.9(2) . . ?
C3 N2 Fe1 120.54(19) . . ?
C7 N2 Fe1 120.7(2) . . ?
N2 C3 C4 124.0(3) . . ?
N2 C3 N8 112.9(2) . . ?
C4 C3 N8 123.1(3) . . ?
C3 C4 C5 116.7(3) . . ?
C3 C4 H4 121.7 . . ?
C5 C4 H4 121.7 . . ?
C4 C5 C6 119.9(3) . . ?
C4 C5 S18 125.1(3) . . ?
C6 C5 S18 115.0(2) . . ?
C7 C6 C5 118.0(3) . . ?
C7 C6 H6 121.0 . . ?
C5 C6 H6 121.0 . . ?
N2 C7 C6 123.6(3) . . ?
N2 C7 N13 113.3(3) . . ?
C6 C7 N13 123.1(3) . . ?
C12 N8 N9 111.0(2) . . ?
C12 N8 C3 131.1(2) . . ?
N9 N8 C3 117.8(2) . . ?
C10 N9 N8 104.9(3) . . ?
C10 N9 Fe1 140.2(2) . . ?
N8 N9 Fe1 114.91(19) . . ?
N9 C10 C11 111.3(3) . . ?
N9 C10 H10 124.4 . . ?
C11 C10 H10 124.4 . . ?
C12 C11 C10 105.7(3) . . ?
C12 C11 H11 127.2 . . ?
C10 C11 H11 127.2 . . ?
N8 C12 C11 107.1(3) . . ?
N8 C12 H12 126.4 . . ?
C11 C12 H12 126.4 . . ?
C17 N13 N14 111.1(3) . . ?
C17 N13 C7 130.5(3) . . ?
N14 N13 C7 118.2(3) . . ?
C15 N14 N13 104.7(3) . . ?
C15 N14 Fe1 141.1(2) . . ?
N13 N14 Fe1 114.1(2) . . ?
N14 C15 C16 112.2(3) . . ?
N14 C15 H15 123.9 . . ?
C16 C15 H15 123.9 . . ?
C17 C16 C15 104.8(3) . . ?
C17 C16 H16 127.6 . . ?
C15 C16 H16 127.6 . . ?
N13 C17 C16 107.2(3) . . ?
N13 C17 H17 126.4 . . ?
C16 C17 H17 126.4 . . ?
C5 S18 C19 105.80(16) . . ?
C20 C19 C21 112.0(4) . . ?
C20 C19 S18 111.5(3) . . ?
C21 C19 S18 105.8(3) . . ?
C20 C19 H19 109.2 . . ?
C21 C19 H19 109.2 . . ?
S18 C19 H19 109.2 . . ?
C19 C20 H20A 109.5 . . ?
C19 C20 H20B 109.5 . . ?
H20A C20 H20B 109.5 . . ?
C19 C20 H20C 109.5 . . ?
H20A C20 H20C 109.5 . . ?
H20B C20 H20C 109.5 . . ?
C19 C21 H21A 109.5 . . ?
C19 C21 H21B 109.5 . . ?
H21A C21 H21B 109.5 . . ?
C19 C21 H21C 109.5 . . ?
H21A C21 H21C 109.5 . . ?
H21B C21 H21C 109.5 . . ?
C27 N22 C23 117.9(2) . . ?
C27 N22 Fe1 120.99(19) . . ?
C23 N22 Fe1 121.06(19) . . ?
N22 C23 C24 123.5(3) . . ?
N22 C23 N28 112.5(2) . . ?
C24 C23 N28 124.0(3) . . ?
C23 C24 C25 117.2(3) . . ?
C23 C24 H24 121.4 . . ?
C25 C24 H24 121.4 . . ?
C26 C25 C24 120.4(3) . . ?
C26 C25 S38 124.6(2) . . ?
C24 C25 S38 115.0(2) . . ?
C27 C26 C25 116.9(3) . . ?
C27 C26 H26 121.6 . . ?
C25 C26 H26 121.6 . . ?
N22 C27 C26 124.1(3) . . ?
N22 C27 N33 112.6(2) . . ?
C26 C27 N33 123.3(3) . . ?
C32 N28 N29 111.2(3) . . ?
C32 N28 C23 130.4(3) . . ?
N29 N28 C23 118.3(2) . . ?
C30 N29 N28 105.2(3) . . ?
C30 N29 Fe1 139.8(2) . . ?
N28 N29 Fe1 114.96(18) . . ?
N29 C30 C31 111.2(3) . . ?
N29 C30 H30 124.4 . . ?
C31 C30 H30 124.4 . . ?
C32 C31 C30 105.4(3) . . ?
C32 C31 H31 127.3 . . ?
C30 C31 H31 127.3 . . ?
N28 C32 C31 107.0(3) . . ?
N28 C32 H32 126.5 . . ?
C31 C32 H32 126.5 . . ?
C37 N33 N34 111.3(2) . . ?
C37 N33 C27 130.6(3) . . ?
N34 N33 C27 118.1(2) . . ?
C35 N34 N33 104.7(3) . . ?
C35 N34 Fe1 140.3(2) . . ?
N33 N34 Fe1 114.94(19) . . ?
N34 C35 C36 111.3(3) . . ?
N34 C35 H35 124.3 . . ?
C36 C35 H35 124.3 . . ?
C37 C36 C35 105.5(3) . . ?
C37 C36 H36 127.2 . . ?
C35 C36 H36 127.2 . . ?
N33 C37 C36 107.1(3) . . ?
N33 C37 H37 126.4 . . ?
C36 C37 H37 126.4 . . ?
C25 S38 C39B 107.7(3) . . ?
C25 S38 C39A 103.0(3) . . ?
C40A C39A C41A 112.9(8) . . ?
C40A C39A S38 113.3(6) . . ?
C41A C39A S38 103.1(6) . . ?
C40A C39A H39A 109.1 . . ?
C41A C39A H39A 109.1 . . ?
S38 C39A H39A 109.1 . . ?
C39A C40A H40A 109.5 . . ?
C39A C40A H40B 109.5 . . ?
H40A C40A H40B 109.5 . . ?
C39A C40A H40C 109.5 . . ?
H40A C40A H40C 109.5 . . ?
H40B C40A H40C 109.5 . . ?
C39A C41A H41A 109.5 . . ?
C39A C41A H41B 109.5 . . ?
H41A C41A H41B 109.5 . . ?
C39A C41A H41C 109.5 . . ?
H41A C41A H41C 109.5 . . ?
H41B C41A H41C 109.5 . . ?
C41B C39B C40B 111.6(7) . . ?
C41B C39B S38 109.6(5) . . ?
C40B C39B S38 106.7(6) . . ?
C41B C39B H39B 109.6 . . ?
C40B C39B H39B 109.6 . . ?
S38 C39B H39B 109.6 . . ?
C39B C40B H40D 109.5 . . ?
C39B C40B H40E 109.5 . . ?
H40D C40B H40E 109.5 . . ?
C39B C40B H40F 109.5 . . ?
H40D C40B H40F 109.5 . . ?
H40E C40B H40F 109.5 . . ?
C39B C41B H41D 109.5 . . ?
C39B C41B H41E 109.5 . . ?
H41D C41B H41E 109.5 . . ?
C39B C41B H41F 109.5 . . ?
H41D C41B H41F 109.5 . . ?
H41E C41B H41F 109.5 . . ?
O45A Cl42A O44A 109.9(10) . . ?
O45A Cl42A O43A 107.5(10) . . ?
O44A Cl42A O43A 114.5(9) . . ?
O45A Cl42A O46A 114.1(10) . . ?
O44A Cl42A O46A 105.6(9) . . ?
O43A Cl42A O46A 105.3(9) . . ?
O45B Cl42B O43B 112.5(8) . . ?
O45B Cl42B O44B 100.1(8) . . ?
O43B Cl42B O44B 111.5(8) . . ?
O45B Cl42B O46B 113.8(8) . . ?
O43B Cl42B O46B 111.3(9) . . ?
O44B Cl42B O46B 107.0(8) . . ?
O45C Cl42C O44C 111.2(8) . . ?
O45C Cl42C O43C 107.7(8) . . ?
O44C Cl42C O43C 110.6(8) . . ?
O45C Cl42C O46C 107.1(7) . . ?
O44C Cl42C O46C 114.7(9) . . ?
O43C Cl42C O46C 105.2(7) . . ?
O48A Cl47A O50A 105.3(6) . . ?
O48A Cl47A O49A 117.5(8) . . ?
O50A Cl47A O49A 108.8(5) . . ?
O48A Cl47A O51A 108.4(6) . . ?
O50A Cl47A O51A 112.6(8) . . ?
O49A Cl47A O51A 104.5(6) . . ?
O51B Cl47B O49B 113.5(6) . . ?
O51B Cl47B O48B 109.5(6) . . ?
O49B Cl47B O48B 102.3(8) . . ?
O51B Cl47B O50B 106.6(8) . . ?
O49B Cl47B O50B 111.8(6) . . ?
O48B Cl47B O50B 113.3(6) . . ?
C53A C52A H52A 109.5 . . ?
C53A C52A H52B 109.5 . . ?
H52A C52A H52B 109.5 . . ?
C53A C52A H52C 109.5 . . ?
H52A C52A H52C 109.5 . . ?
H52B C52A H52C 109.5 . . ?
N54A C53A C52A 170.1(19) . . ?
C53B C52B H52G 109.5 . . ?
C53B C52B H52H 109.5 . . ?
H52G C52B H52H 109.5 . . ?
C53B C52B H52I 109.5 . . ?
H52G C52B H52I 109.5 . . ?
H52H C52B H52I 109.5 . . ?
N54B C53B C52B 165(2) . . ?
C53C C52C H52D 109.5 . . ?
C53C C52C H52E 109.5 . . ?
H52D C52C H52E 109.5 . . ?
C53C C52C H52F 109.5 . . ?
H52D C52C H52F 109.5 . . ?
H52E C52C H52F 109.5 . . ?
N54C C53C C52C 161(3) . . ?

_diffrn_measured_fraction_theta_max 0.926
_diffrn_reflns_theta_full        72.00
_diffrn_measured_fraction_theta_full 0.957
_refine_diff_density_max         0.584
_refine_diff_density_min         -0.644
_refine_diff_density_rms         0.067
_exptl_crystal_recrystallization_method 
'Re-crystallisation from solvent: Acetonitrile-diethyl ether'
_exptl_crystal_preparation       'Magnetic properties'
####################################################################### 
# 
# This file contains crystal structure data downloaded from the 
# Cambridge Structural Database (CSD) hosted by the Cambridge 
# Crystallographic Data Centre (CCDC).
# 
# Full information about CCDC data access policies and citation 
# guidelines are available at http://www.ccdc.cam.ac.uk/access/V1 
# 
# Audit and citation data items may have been added by the CCDC. 
# Please retain this information to preserve the provenance of 
# this file and to allow appropriate attribution of the data. 
# 
#######################################################################

data_rk137MeNO2_100K
_database_code_depnum_ccdc_archive 'CCDC 1564670'
_audit_update_record             
;
2017-07-28 deposited with the CCDC.
2017-11-20 downloaded from the CCDC.
;
_chemical_name_common            ?
_chemical_name_systematic        ?
_chemical_formula_moiety         'C28 H30 Fe N10 S2, 2(B F4), C H3 N O2'
_chemical_formula_sum            'C29 H33 B2 F8 Fe N11 O2 S2'
_chemical_formula_weight         861.25
_chemical_melting_point          'not measured'
loop_
_atom_type_symbol
_atom_type_description
_atom_type_scat_dispersion_real
_atom_type_scat_dispersion_imag
_atom_type_scat_source
C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
B B 0.0013 0.0007 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
F F 0.0171 0.0103 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Fe Fe 0.3463 0.8444 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
S S 0.1246 0.1234 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'

_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.
;
_space_group_crystal_system      monoclinic
_space_group_IT_number           14
_space_group_name_H-M_alt        'P 1 21/c 1'
_space_group_name_Hall           '-P 2ybc'
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                   19.7391(7)
_cell_length_b                   11.9252(4)
_cell_length_c                   16.0160(5)
_cell_angle_alpha                90
_cell_angle_beta                 100.942(3)
_cell_angle_gamma                90
_cell_volume                     3701.5(2)
_cell_formula_units_Z            4
_cell_measurement_reflns_used    2416
_cell_measurement_temperature    100(2)
_cell_measurement_theta_max      25.3170
_cell_measurement_theta_min      3.0060
_exptl_absorpt_coefficient_mu    0.607
_exptl_absorpt_correction_T_max  0.963
_exptl_absorpt_correction_T_min  0.918
_exptl_absorpt_correction_type   analytical
_exptl_absorpt_process_details   
;
CrysAlisPro 1.171.38.41 (Rigaku Oxford Diffraction, 2015)
Analytical numeric absorption correction using a multifaceted crystal
			model based on expressions derived by R.C. Clark & J.S. Reid.
(Clark, R. C. & Reid, J. S. (1995). Acta Cryst. A51, 887-897)
Empirical absorption correction using spherical harmonics,
 implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_absorpt_special_details   ?
_exptl_crystal_colour            'dark orange'
_exptl_crystal_colour_modifier   dark
_exptl_crystal_colour_primary    orange
_exptl_crystal_density_diffrn    1.545
_exptl_crystal_density_meas      'not measured'
_exptl_crystal_density_method    none
_exptl_crystal_description       block
_exptl_crystal_F_000             1760
loop_
_exptl_crystal_face_index_h
_exptl_crystal_face_index_k
_exptl_crystal_face_index_l
_exptl_crystal_face_perp_dist
1 16 10 0.0247
0 -16 -10 0.0411
-21 -4 0 0.0906
22 -3 -5 0.1225
0 -6 26 0.0346
1 6 -26 0.0526

_exptl_crystal_size_max          0.238
_exptl_crystal_size_mid          0.091
_exptl_crystal_size_min          0.07
loop_
_exptl_oxdiff_crystal_face_indexfrac_h
_exptl_oxdiff_crystal_face_indexfrac_k
_exptl_oxdiff_crystal_face_indexfrac_l
_exptl_oxdiff_crystal_face_x
_exptl_oxdiff_crystal_face_y
_exptl_oxdiff_crystal_face_z
1.0172 15.9896 10.0335 -0.9581 0.3504 -0.0903
-0.0173 -15.9901 -10.0331 0.9588 -0.3452 0.0455
-21.0015 -3.9894 -0.0146 0.2234 -0.1035 0.9451
21.9937 -3.0063 -4.9998 0.1972 -0.0652 -0.9683
0.0015 -6.0193 25.9963 0.3372 0.9562 -0.0667
0.9984 6.0188 -25.9960 -0.3365 -0.9511 0.0219

_exptl_transmission_factor_max   ?
_exptl_transmission_factor_min   ?
_diffrn_reflns_av_R_equivalents  0.0692
_diffrn_reflns_av_unetI/netI     0.1385
_diffrn_reflns_Laue_measured_fraction_full 0.998
_diffrn_reflns_Laue_measured_fraction_max 0.999
_diffrn_reflns_limit_h_max       25
_diffrn_reflns_limit_h_min       -15
_diffrn_reflns_limit_k_max       15
_diffrn_reflns_limit_k_min       -13
_diffrn_reflns_limit_l_max       20
_diffrn_reflns_limit_l_min       -20
_diffrn_reflns_number            16453
_diffrn_reflns_point_group_measured_fraction_full 0.998
_diffrn_reflns_point_group_measured_fraction_max 0.999
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         26.998
_diffrn_reflns_theta_min         2.975
_diffrn_ambient_temperature      100(2)
_diffrn_detector                 'CCD plate'
_diffrn_detector_area_resol_mean 16.1852
_diffrn_detector_type            Sapphire3
_diffrn_measured_fraction_theta_full 0.998
_diffrn_measured_fraction_theta_max 0.999
_diffrn_measurement_details      
;
List of Runs (angles in degrees, time in seconds):

  # Type    Start    End  Width  tₑₓₚ   ω     θ     κ     φ   Frames
#--------------------------------------------------------------------------
  1  ω     -4.00  97.00   1.00   10.00    --   23.49  38.00-120.00  101
  2  ω    -21.00  22.00   1.00   10.00    --  -21.46 -99.00-150.00   43
  3  ω    -83.00 -34.00   1.00   10.00    --  -21.46 -19.00-120.00   49
  4  ω   -104.00 -45.00   1.00   10.00    --  -21.46 178.00  30.00   59
;
_diffrn_measurement_device       'four-circle diffractometer'
_diffrn_measurement_device_type  'Xcalibur, Sapphire3'
_diffrn_measurement_method       'ω scans'
_diffrn_orient_matrix_type       
'CrysAlisPro convention (1999,Acta A55,543-557)'
_diffrn_orient_matrix_UB_11      0.0006578000
_diffrn_orient_matrix_UB_12      -0.0594618000
_diffrn_orient_matrix_UB_13      -0.0007965000
_diffrn_orient_matrix_UB_21      0.0051500000
_diffrn_orient_matrix_UB_22      -0.0013067000
_diffrn_orient_matrix_UB_23      0.0364809000
_diffrn_orient_matrix_UB_31      -0.0448031000
_diffrn_orient_matrix_UB_32      -0.0010378000
_diffrn_orient_matrix_UB_33      -0.0028020000
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_source                   'fine-focus sealed X-ray tube'
_diffrn_source_type              'Enhance (Mo) X-ray Source'
_reflns_Friedel_coverage         0.000
_reflns_Friedel_fraction_full    .
_reflns_Friedel_fraction_max     .
_reflns_number_gt                4550
_reflns_number_total             8083
_reflns_odcompleteness_completeness 99.79
_reflns_odcompleteness_iscentric 1
_reflns_odcompleteness_theta     26.32
_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.
;
_reflns_threshold_expression     'I > 2σ(I)'
_computing_cell_refinement       'CrysAlisPro 1.171.38.41 (Rigaku OD, 2015)'
_computing_data_collection       'CrysAlisPro 1.171.37.31c (Rigaku OD, 2014)'
_computing_data_reduction        'CrysAlisPro 1.171.38.41 (Rigaku OD, 2015)'
_computing_molecular_graphics    'Mercury3.9 (2016)'
_computing_publication_material  'Olex2 (Dolomanov et al., 2009)'
_computing_structure_refinement  'ShelXL (Sheldrick, 2015)'
_computing_structure_solution    'ShelXT (Sheldrick, 2015)'
_refine_diff_density_max         0.446
_refine_diff_density_min         -0.412
_refine_diff_density_rms         0.090
_refine_ls_extinction_coef       .
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.008
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     558
_refine_ls_number_reflns         8083
_refine_ls_number_restraints     6
_refine_ls_R_factor_all          0.1363
_refine_ls_R_factor_gt           0.0636
_refine_ls_restrained_S_all      1.008
_refine_ls_shift/su_max          0.001
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details     
'w=1/[σ²(Fo²)+(0.0076P)²] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0696
_refine_ls_wR_factor_ref         0.0888
_refine_special_details          
;
Structure of higher symmetry low spin state at 100K.
ISOR restrain for ADP of F1B site has been applied.
;
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     dual
_atom_sites_solution_secondary   difmap
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 0.27649(3) 0.61672(5) 0.43402(3) 0.01793(14) Uani 1 1 d . . . . .
S2 S 0.60082(5) 0.70865(9) 0.49583(6) 0.0252(2) Uani 1 1 d . . . . .
S1 S -0.04113(5) 0.51489(10) 0.28472(6) 0.0349(3) Uani 1 1 d . . . . .
N10 N 0.30663(15) 0.5053(3) 0.35724(16) 0.0189(7) Uani 1 1 d . . . . .
N5 N 0.25581(15) 0.5013(3) 0.51420(16) 0.0187(7) Uani 1 1 d . . . . .
N6 N 0.28266(15) 0.7347(3) 0.52245(16) 0.0187(7) Uani 1 1 d . . . . .
N9 N 0.37650(15) 0.5093(3) 0.35923(16) 0.0195(7) Uani 1 1 d . . . . .
N7 N 0.35023(15) 0.7620(3) 0.55776(16) 0.0167(7) Uani 1 1 d . . . . .
N4 N 0.18791(15) 0.4673(3) 0.49663(17) 0.0177(7) Uani 1 1 d . . . . .
N1 N 0.26071(15) 0.7290(3) 0.34321(16) 0.0188(7) Uani 1 1 d . . . . .
N3 N 0.18057(15) 0.5976(3) 0.39413(16) 0.0174(7) Uani 1 1 d . . . . .
N2 N 0.19314(15) 0.7311(3) 0.29927(17) 0.0195(7) Uani 1 1 d . . . . .
N8 N 0.37337(14) 0.6358(2) 0.46279(16) 0.0158(7) Uani 1 1 d . . . . .
C15 C 0.24498(19) 0.7979(3) 0.5636(2) 0.0242(9) Uani 1 1 d . . . . .
H15 H 0.1970 0.7974 0.5536 0.029 Uiso 1 1 calc R . . . .
C28 C 0.5862(2) 0.9383(3) 0.4898(2) 0.0355(11) Uani 1 1 d . . . . .
H28A H 0.6078 0.9410 0.4409 0.053 Uiso 1 1 calc GR . . . .
H28B H 0.5934 1.0082 0.5199 0.053 Uiso 1 1 calc GR . . . .
H28C H 0.5376 0.9255 0.4718 0.053 Uiso 1 1 calc GR . . . .
C10 C 0.23444(19) 0.3779(3) 0.6115(2) 0.0225(9) Uani 1 1 d . . . . .
H10 H 0.2416 0.3311 0.6589 0.027 Uiso 1 1 calc R . . . .
C7 C 0.07765(18) 0.4946(3) 0.3962(2) 0.0228(9) Uani 1 1 d . . . . .
H7 H 0.0545 0.4398 0.4211 0.027 Uiso 1 1 calc R . . . .
C18 C 0.40130(18) 0.7132(3) 0.5200(2) 0.0163(8) Uani 1 1 d . . . . .
C3 C 0.1849(2) 0.8116(3) 0.2387(2) 0.0252(10) Uani 1 1 d . . . . .
H3 H 0.1444 0.8280 0.2006 0.030 Uiso 1 1 calc R . . . .
C2 C 0.2458(2) 0.8633(3) 0.2436(2) 0.0299(11) Uani 1 1 d . . . . .
H2 H 0.2556 0.9225 0.2101 0.036 Uiso 1 1 calc R . . . .
C5 C 0.07968(18) 0.6381(3) 0.2901(2) 0.0218(9) Uani 1 1 d . . . . .
H5 H 0.0583 0.6806 0.2438 0.026 Uiso 1 1 calc R . . . .
C13 C -0.1322(2) 0.5462(5) 0.1408(3) 0.079(2) Uani 1 1 d . . . . .
H13A H -0.1176 0.4744 0.1238 0.118 Uiso 1 1 calc GR . . . .
H13B H -0.1496 0.5903 0.0912 0.118 Uiso 1 1 calc GR . . . .
H13C H -0.1679 0.5362 0.1734 0.118 Uiso 1 1 calc GR . . . .
C1 C 0.2916(2) 0.8108(3) 0.3088(2) 0.0235(9) Uani 1 1 d . . . . .
H1 H 0.3377 0.8307 0.3260 0.028 Uiso 1 1 calc R . . . .
C4 C 0.14781(18) 0.6548(3) 0.3269(2) 0.0187(9) Uani 1 1 d . . . . .
C22 C 0.41468(19) 0.5846(3) 0.4177(2) 0.0170(9) Uani 1 1 d . . . . .
C19 C 0.47036(18) 0.7405(3) 0.5352(2) 0.0195(9) Uani 1 1 d . . . . .
H19 H 0.4884 0.7930 0.5764 0.023 Uiso 1 1 calc R . . . .
C20 C 0.51225(18) 0.6869(3) 0.4868(2) 0.0187(9) Uani 1 1 d . . . . .
C27 C 0.69615(19) 0.8546(3) 0.5712(2) 0.0359(11) Uani 1 1 d . . . . .
H27A H 0.7145 0.7951 0.6092 0.054 Uiso 1 1 calc GR . . . .
H27B H 0.7079 0.9255 0.5984 0.054 Uiso 1 1 calc GR . . . .
H27C H 0.7153 0.8501 0.5205 0.054 Uiso 1 1 calc GR . . . .
C17 C 0.3529(2) 0.8416(3) 0.6193(2) 0.0239(10) Uani 1 1 d . . . . .
H17 H 0.3925 0.8730 0.6517 0.029 Uiso 1 1 calc R . . . .
C11 C 0.2839(2) 0.4467(3) 0.5838(2) 0.0219(9) Uani 1 1 d . . . . .
H11 H 0.3298 0.4527 0.6108 0.026 Uiso 1 1 calc R . . . .
C6 C 0.04434(19) 0.5553(3) 0.3251(2) 0.0227(9) Uani 1 1 d . . . . .
C16 C 0.2866(2) 0.8662(3) 0.6244(2) 0.0260(10) Uani 1 1 d . . . . .
H16 H 0.2717 0.9177 0.6607 0.031 Uiso 1 1 calc R . . . .
C14 C -0.0883(3) 0.7208(4) 0.2247(3) 0.086(2) Uani 1 1 d . . . . .
H14A H -0.1270 0.7149 0.2528 0.129 Uiso 1 1 calc GR . . . .
H14B H -0.0998 0.7699 0.1766 0.129 Uiso 1 1 calc GR . . . .
H14C H -0.0494 0.7505 0.2635 0.129 Uiso 1 1 calc GR . . . .
C26 C 0.61760(19) 0.8435(3) 0.5480(2) 0.0270(10) Uani 1 1 d . . . . .
H26 H 0.5982 0.8444 0.6000 0.032 Uiso 1 1 calc R . . . .
C8 C 0.14536(19) 0.5187(3) 0.4275(2) 0.0176(9) Uani 1 1 d . . . . .
C25 C 0.2843(2) 0.4240(3) 0.3033(2) 0.0245(10) Uani 1 1 d . . . . .
H25 H 0.2385 0.4011 0.2895 0.029 Uiso 1 1 calc R . . . .
C24 C 0.3378(2) 0.3768(3) 0.2694(2) 0.0282(10) Uani 1 1 d . . . . .
H24 H 0.3342 0.3193 0.2295 0.034 Uiso 1 1 calc R . . . .
C23 C 0.3962(2) 0.4318(3) 0.3064(2) 0.0239(10) Uani 1 1 d . . . . .
H23 H 0.4407 0.4189 0.2974 0.029 Uiso 1 1 calc R . . . .
C21 C 0.48327(18) 0.6064(3) 0.4262(2) 0.0194(9) Uani 1 1 d . . . . .
H21 H 0.5101 0.5692 0.3931 0.023 Uiso 1 1 calc R . . . .
C9 C 0.17437(19) 0.3933(3) 0.5557(2) 0.0216(9) Uani 1 1 d . . . . .
H9 H 0.1321 0.3598 0.5575 0.026 Uiso 1 1 calc R . . . .
C12 C -0.0707(2) 0.6066(4) 0.1951(3) 0.0485(14) Uani 1 1 d . . . . .
H12 H -0.0340 0.6143 0.1621 0.058 Uiso 1 1 calc R . . . .
F4B F -0.0200(9) 0.718(3) 0.512(3) 0.042(9) Uani 0.26(4) 1 d . . P A 3
F1 F 0.0754(8) 0.8004(16) 0.4692(7) 0.056(3) Uani 0.74(4) 1 d . . P A 4
F3 F 0.0346(10) 0.7872(15) 0.5926(5) 0.059(3) Uani 0.74(4) 1 d . . P A 4
F4 F -0.0108(6) 0.6816(10) 0.4794(7) 0.037(2) Uani 0.74(4) 1 d . . P A 4
F2 F 0.09407(12) 0.6424(2) 0.55596(12) 0.0415(7) Uani 1 1 d . . . . .
F3B F 0.066(2) 0.817(2) 0.5942(14) 0.046(7) Uani 0.26(4) 1 d . . P A 3
F1B F 0.079(2) 0.773(3) 0.4665(15) 0.025(6) Uani 0.26(4) 1 d . U P A 3
B1 B 0.0501(3) 0.7303(5) 0.5258(3) 0.0300(12) Uani 1 1 d . . . . .
O1 O 0.18104(19) 0.3801(3) 0.1008(2) 0.0818(13) Uani 1 1 d . . . . .
O2 O 0.1315(7) 0.4450(18) 0.1941(7) 0.082(6) Uani 0.55(2) 1 d . . P B 1
O2B O 0.1558(5) 0.5164(13) 0.1695(7) 0.042(4) Uani 0.45(2) 1 d . . P B 2
N11 N 0.1350(2) 0.4296(4) 0.1211(3) 0.0500(12) Uani 1 1 d . . . . .
C29 C 0.0671(2) 0.4372(4) 0.0655(3) 0.0740(18) Uani 1 1 d . . . . .
H29A H 0.0616 0.5101 0.0396 0.111 Uiso 1 1 calc GR . . . .
H29B H 0.0318 0.4256 0.0983 0.111 Uiso 1 1 calc GR . . . .
H29C H 0.0634 0.3809 0.0220 0.111 Uiso 1 1 calc GR . . . .
F7 F 0.4432(6) 0.5938(19) 0.8307(5) 0.046(3) Uani 0.82(5) 1 d . . P C 6
F5 F 0.43808(11) 0.54923(19) 0.69156(12) 0.0324(6) Uani 1 1 d . . . . .
F7B F 0.427(2) 0.549(4) 0.833(2) 0.021(7) Uani 0.18(5) 1 d . . P C 5
F6 F 0.49114(12) 0.4286(2) 0.79361(13) 0.0437(7) Uani 1 1 d . . . . .
F8 F 0.3727(4) 0.4522(16) 0.7685(8) 0.043(3) Uani 0.82(5) 1 d . . P C 6
F8B F 0.383(2) 0.411(4) 0.750(3) 0.025(8) Uani 0.18(5) 1 d . . P C 5
B2 B 0.4355(2) 0.5023(5) 0.7705(3) 0.0323(13) 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 N10 1.978(3) . ?
Fe1 N5 1.977(3) . ?
Fe1 N6 1.984(3) . ?
Fe1 N1 1.958(3) . ?
Fe1 N3 1.894(3) . ?
Fe1 N8 1.894(3) . ?
S2 C20 1.746(4) . ?
S2 C26 1.814(4) . ?
S1 C6 1.756(4) . ?
S1 C12 1.811(4) . ?
N10 N9 1.374(4) . ?
N10 C25 1.317(4) . ?
N5 N4 1.377(4) . ?
N5 C11 1.319(4) . ?
N6 N7 1.385(4) . ?
N6 C15 1.319(4) . ?
N9 C22 1.408(4) . ?
N9 C23 1.359(4) . ?
N7 C18 1.397(4) . ?
N7 C17 1.363(4) . ?
N4 C8 1.398(4) . ?
N4 C9 1.357(4) . ?
N1 N2 1.385(4) . ?
N1 C1 1.325(4) . ?
N3 C4 1.334(4) . ?
N3 C8 1.339(4) . ?
N2 C3 1.353(4) . ?
N2 C4 1.405(4) . ?
N8 C18 1.343(4) . ?
N8 C22 1.335(4) . ?
C15 H15 0.9300 . ?
C15 C16 1.409(5) . ?
C28 H28A 0.9600 . ?
C28 H28B 0.9600 . ?
C28 H28C 0.9600 . ?
C28 C26 1.520(5) . ?
C10 H10 0.9300 . ?
C10 C11 1.410(5) . ?
C10 C9 1.355(5) . ?
C7 H7 0.9300 . ?
C7 C6 1.403(5) . ?
C7 C8 1.366(5) . ?
C18 C19 1.378(5) . ?
C3 H3 0.9300 . ?
C3 C2 1.341(5) . ?
C2 H2 0.9300 . ?
C2 C1 1.392(5) . ?
C5 H5 0.9300 . ?
C5 C4 1.376(5) . ?
C5 C6 1.388(5) . ?
C13 H13A 0.9600 . ?
C13 H13B 0.9600 . ?
C13 H13C 0.9600 . ?
C13 C12 1.533(6) . ?
C1 H1 0.9300 . ?
C22 C21 1.360(5) . ?
C19 H19 0.9300 . ?
C19 C20 1.392(5) . ?
C20 C21 1.407(5) . ?
C27 H27A 0.9600 . ?
C27 H27B 0.9600 . ?
C27 H27C 0.9600 . ?
C27 C26 1.530(5) . ?
C17 H17 0.9300 . ?
C17 C16 1.359(5) . ?
C11 H11 0.9300 . ?
C16 H16 0.9300 . ?
C14 H14A 0.9600 . ?
C14 H14B 0.9600 . ?
C14 H14C 0.9600 . ?
C14 C12 1.504(7) . ?
C26 H26 0.9800 . ?
C25 H25 0.9300 . ?
C25 C24 1.395(5) . ?
C24 H24 0.9300 . ?
C24 C23 1.361(5) . ?
C23 H23 0.9300 . ?
C21 H21 0.9300 . ?
C9 H9 0.9300 . ?
C12 H12 0.9800 . ?
F4B B1 1.368(17) . ?
F1 B1 1.394(14) . ?
F3 B1 1.351(9) . ?
F4 B1 1.413(8) . ?
F2 B1 1.388(5) . ?
F3B B1 1.49(3) . ?
F1B B1 1.30(3) . ?
O1 N11 1.180(4) . ?
O2 N11 1.198(11) . ?
O2B N11 1.311(12) . ?
N11 C29 1.465(5) . ?
C29 H29A 0.9600 . ?
C29 H29B 0.9600 . ?
C29 H29C 0.9600 . ?
F7 B2 1.444(15) . ?
F5 B2 1.393(5) . ?
F7B B2 1.18(3) . ?
F6 B2 1.401(5) . ?
F8 B2 1.371(8) . ?
F8B B2 1.50(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
N10 Fe1 N6 159.36(12) . . ?
N5 Fe1 N10 93.41(12) . . ?
N5 Fe1 N6 91.29(11) . . ?
N1 Fe1 N10 91.26(11) . . ?
N1 Fe1 N5 159.26(12) . . ?
N1 Fe1 N6 91.42(12) . . ?
N3 Fe1 N10 96.24(12) . . ?
N3 Fe1 N5 79.56(12) . . ?
N3 Fe1 N6 104.39(12) . . ?
N3 Fe1 N1 79.86(12) . . ?
N3 Fe1 N8 174.47(12) . . ?
N8 Fe1 N10 79.79(12) . . ?
N8 Fe1 N5 104.41(12) . . ?
N8 Fe1 N6 79.57(12) . . ?
N8 Fe1 N1 96.30(12) . . ?
C20 S2 C26 105.20(18) . . ?
C6 S1 C12 105.59(19) . . ?
N9 N10 Fe1 112.4(2) . . ?
C25 N10 Fe1 143.1(3) . . ?
C25 N10 N9 104.5(3) . . ?
N4 N5 Fe1 112.6(2) . . ?
C11 N5 Fe1 141.9(3) . . ?
C11 N5 N4 105.3(3) . . ?
N7 N6 Fe1 112.4(2) . . ?
C15 N6 Fe1 142.9(3) . . ?
C15 N6 N7 104.6(3) . . ?
N10 N9 C22 116.5(3) . . ?
C23 N9 N10 111.5(3) . . ?
C23 N9 C22 131.9(3) . . ?
N6 N7 C18 116.3(3) . . ?
C17 N7 N6 111.2(3) . . ?
C17 N7 C18 132.2(3) . . ?
N5 N4 C8 116.6(3) . . ?
C9 N4 N5 111.2(3) . . ?
C9 N4 C8 132.0(3) . . ?
N2 N1 Fe1 113.1(2) . . ?
C1 N1 Fe1 142.3(3) . . ?
C1 N1 N2 104.5(3) . . ?
C4 N3 Fe1 120.7(2) . . ?
C4 N3 C8 118.2(3) . . ?
C8 N3 Fe1 120.8(2) . . ?
N1 N2 C4 116.0(3) . . ?
C3 N2 N1 110.5(3) . . ?
C3 N2 C4 133.5(3) . . ?
C18 N8 Fe1 120.9(2) . . ?
C22 N8 Fe1 120.4(2) . . ?
C22 N8 C18 118.0(3) . . ?
N6 C15 H15 124.3 . . ?
N6 C15 C16 111.4(3) . . ?
C16 C15 H15 124.3 . . ?
H28A C28 H28B 109.5 . . ?
H28A C28 H28C 109.5 . . ?
H28B C28 H28C 109.5 . . ?
C26 C28 H28A 109.5 . . ?
C26 C28 H28B 109.5 . . ?
C26 C28 H28C 109.5 . . ?
C11 C10 H10 126.7 . . ?
C9 C10 H10 126.7 . . ?
C9 C10 C11 106.5(3) . . ?
C6 C7 H7 121.2 . . ?
C8 C7 H7 121.2 . . ?
C8 C7 C6 117.7(4) . . ?
N8 C18 N7 110.2(3) . . ?
N8 C18 C19 123.2(3) . . ?
C19 C18 N7 126.6(3) . . ?
N2 C3 H3 126.3 . . ?
C2 C3 N2 107.4(3) . . ?
C2 C3 H3 126.3 . . ?
C3 C2 H2 126.7 . . ?
C3 C2 C1 106.6(3) . . ?
C1 C2 H2 126.7 . . ?
C4 C5 H5 121.5 . . ?
C4 C5 C6 117.1(3) . . ?
C6 C5 H5 121.5 . . ?
H13A C13 H13B 109.5 . . ?
H13A C13 H13C 109.5 . . ?
H13B C13 H13C 109.5 . . ?
C12 C13 H13A 109.5 . . ?
C12 C13 H13B 109.5 . . ?
C12 C13 H13C 109.5 . . ?
N1 C1 C2 111.0(4) . . ?
N1 C1 H1 124.5 . . ?
C2 C1 H1 124.5 . . ?
N3 C4 N2 110.2(3) . . ?
N3 C4 C5 123.8(4) . . ?
C5 C4 N2 126.0(3) . . ?
N8 C22 N9 110.3(3) . . ?
N8 C22 C21 123.9(3) . . ?
C21 C22 N9 125.8(3) . . ?
C18 C19 H19 121.1 . . ?
C18 C19 C20 117.7(3) . . ?
C20 C19 H19 121.1 . . ?
C19 C20 S2 125.2(3) . . ?
C19 C20 C21 119.4(3) . . ?
C21 C20 S2 115.4(3) . . ?
H27A C27 H27B 109.5 . . ?
H27A C27 H27C 109.5 . . ?
H27B C27 H27C 109.5 . . ?
C26 C27 H27A 109.5 . . ?
C26 C27 H27B 109.5 . . ?
C26 C27 H27C 109.5 . . ?
N7 C17 H17 126.6 . . ?
C16 C17 N7 106.8(3) . . ?
C16 C17 H17 126.6 . . ?
N5 C11 C10 110.4(3) . . ?
N5 C11 H11 124.8 . . ?
C10 C11 H11 124.8 . . ?
C7 C6 S1 115.3(3) . . ?
C5 C6 S1 124.6(3) . . ?
C5 C6 C7 120.1(3) . . ?
C15 C16 H16 127.0 . . ?
C17 C16 C15 106.0(3) . . ?
C17 C16 H16 127.0 . . ?
H14A C14 H14B 109.5 . . ?
H14A C14 H14C 109.5 . . ?
H14B C14 H14C 109.5 . . ?
C12 C14 H14A 109.5 . . ?
C12 C14 H14B 109.5 . . ?
C12 C14 H14C 109.5 . . ?
S2 C26 H26 109.5 . . ?
C28 C26 S2 111.0(3) . . ?
C28 C26 C27 111.2(3) . . ?
C28 C26 H26 109.5 . . ?
C27 C26 S2 106.0(3) . . ?
C27 C26 H26 109.5 . . ?
N3 C8 N4 110.2(3) . . ?
N3 C8 C7 123.2(3) . . ?
C7 C8 N4 126.7(3) . . ?
N10 C25 H25 124.2 . . ?
N10 C25 C24 111.6(3) . . ?
C24 C25 H25 124.2 . . ?
C25 C24 H24 127.0 . . ?
C23 C24 C25 106.1(3) . . ?
C23 C24 H24 127.0 . . ?
N9 C23 C24 106.2(3) . . ?
N9 C23 H23 126.9 . . ?
C24 C23 H23 126.9 . . ?
C22 C21 C20 117.8(3) . . ?
C22 C21 H21 121.1 . . ?
C20 C21 H21 121.1 . . ?
N4 C9 H9 126.7 . . ?
C10 C9 N4 106.6(3) . . ?
C10 C9 H9 126.7 . . ?
S1 C12 H12 108.9 . . ?
C13 C12 S1 105.5(3) . . ?
C13 C12 H12 108.9 . . ?
C14 C12 S1 110.9(3) . . ?
C14 C12 C13 113.5(4) . . ?
C14 C12 H12 108.9 . . ?
F4B B1 F2 121.4(12) . . ?
F4B B1 F3B 105.2(13) . . ?
F1 B1 F4 106.2(7) . . ?
F3 B1 F1 112.2(8) . . ?
F3 B1 F4 109.0(5) . . ?
F3 B1 F2 108.9(5) . . ?
F2 B1 F1 113.7(8) . . ?
F2 B1 F4 106.6(7) . . ?
F2 B1 F3B 103.6(12) . . ?
F1B B1 F4B 119(2) . . ?
F1B B1 F2 102.9(19) . . ?
F1B B1 F3B 101.8(18) . . ?
O1 N11 O2 122.4(5) . . ?
O1 N11 O2B 112.8(6) . . ?
O1 N11 C29 121.8(4) . . ?
O2 N11 C29 111.6(7) . . ?
O2B N11 C29 117.3(5) . . ?
N11 C29 H29A 109.5 . . ?
N11 C29 H29B 109.5 . . ?
N11 C29 H29C 109.5 . . ?
H29A C29 H29B 109.5 . . ?
H29A C29 H29C 109.5 . . ?
H29B C29 H29C 109.5 . . ?
F5 B2 F7 106.6(9) . . ?
F5 B2 F6 109.2(4) . . ?
F5 B2 F8B 103.6(14) . . ?
F7B B2 F5 128.0(18) . . ?
F7B B2 F6 107.2(15) . . ?
F7B B2 F8B 109.2(14) . . ?
F6 B2 F7 108.7(4) . . ?
F6 B2 F8B 94(2) . . ?
F8 B2 F7 109.0(5) . . ?
F8 B2 F5 110.0(5) . . ?
F8 B2 F6 113.1(8) . . ?


####################################################################### 
# 
# 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_164acht
_database_code_depnum_ccdc_archive 'CCDC 1428763'
_audit_update_record             
;
2015-09-30 deposited with the CCDC.
2017-11-20 downloaded from the CCDC.
;

_audit_creation_method           SHELXL-97
_chemical_name_systematic        
'Bis[4-(isopropylsulfanyl)-2,6-di(pyrazol-1-yl)pyridine]iron(II)diperchlorate acetone solvate'
_chemical_name_common            ?
_chemical_melting_point          ?
_chemical_formula_moiety         'C28 H30 Fe N10 S2, 2(Cl O4), 0.7(C3 H6 O)'
_chemical_formula_sum            'C30.10 H34.20 Cl2 Fe N10 O8.70 S2'
_chemical_formula_weight         866.14

loop_
_atom_type_symbol
_atom_type_description
_atom_type_scat_dispersion_real
_atom_type_scat_dispersion_imag
_atom_type_scat_source
Cl Cl 0.3639 0.7018 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
C C 0.0181 0.0091 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Fe Fe -1.1336 3.1974 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
N N 0.0311 0.0180 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
O O 0.0492 0.0322 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
S S 0.3331 0.5567 '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'

_symmetry_cell_setting           monoclinic
_symmetry_space_group_name_H-M   'P 21/c'

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

_cell_length_a                   20.4915(4)
_cell_length_b                   11.9029(3)
_cell_length_c                   16.4898(4)
_cell_angle_alpha                90.00
_cell_angle_beta                 101.531(2)
_cell_angle_gamma                90.00
_cell_volume                     3940.82(16)
_cell_formula_units_Z            4
_cell_measurement_temperature    250(2)
_cell_measurement_reflns_used    6357
_cell_measurement_theta_min      4.40
_cell_measurement_theta_max      73.69

_exptl_crystal_description       plate
_exptl_crystal_colour            yellow
_exptl_crystal_size_max          0.21
_exptl_crystal_size_mid          0.17
_exptl_crystal_size_min          0.05
_exptl_crystal_density_meas      ?
_exptl_crystal_density_diffrn    1.460
_exptl_crystal_density_method    'not measured'
_exptl_crystal_F_000             1786
_exptl_absorpt_coefficient_mu    5.839
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_correction_T_min  0.506
_exptl_absorpt_correction_T_max  1.000
_exptl_absorpt_process_details   
; 
CrysAlisPro, Agilent Technologies,
Version 1.171.36.24 (release 03-12-2012 CrysAlis171 .NET)
Empirical absorption correction using spherical harmonics,
 implemented in SCALE3 ABSPACK scaling algorithm.
;

_diffrn_ambient_temperature      250(2)
_diffrn_radiation_wavelength     1.54184
_diffrn_radiation_type           CuK\a
_diffrn_radiation_source         'SuperNova (Cu) X-ray Source'
_diffrn_radiation_monochromator  mirror
_diffrn_measurement_device_type  'SuperNova, Dual, Cu at zero, Atlas'
_diffrn_measurement_method       'ω scans'
_diffrn_detector_area_resol_mean 5.3095
_diffrn_standards_number         0
_diffrn_standards_interval_count 0
_diffrn_standards_interval_time  0
_diffrn_standards_decay_%        0
_diffrn_reflns_number            16507
_diffrn_reflns_av_R_equivalents  0.0371
_diffrn_reflns_av_sigmaI/netI    0.0424
_diffrn_reflns_limit_h_min       -21
_diffrn_reflns_limit_h_max       25
_diffrn_reflns_limit_k_min       -11
_diffrn_reflns_limit_k_max       14
_diffrn_reflns_limit_l_min       -17
_diffrn_reflns_limit_l_max       20
_diffrn_reflns_theta_min         4.32
_diffrn_reflns_theta_max         73.90
_reflns_number_total             7746
_reflns_number_gt                6098
_reflns_threshold_expression     >2sigma(I)

_computing_data_collection       'CrysAlisPro, Agilent Technologies'
_computing_cell_refinement       'CrysAlisPro, Agilent Technologies'
_computing_data_reduction        'CrysAlisPro, Agilent Technologies'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_molecular_graphics    'XSEED (Barbour, 2001)'
_computing_publication_material  'local program'

_refine_special_details          
; 
 Refinement of F² against ALL reflections.  The weighted R-factor wR and 
 goodness of fit S are based on F², conventional R-factors R are based 
 on F, with F set to zero for negative F². The threshold expression of 
 F² > 2sigma(F²) is used only for calculating R-factors(gt) etc. and is 
 not relevant to the choice of reflections for refinement.  R-factors based 
 on F² are statistically about twice as large as those based on F, and R- 
 factors based on ALL data will be even larger. 

 One of the isopropyl substitutents on the complex cation is disordered over 
 three equally occupied orientations, which were modelled with the fixed 
 restraints C(pyridyl)---S = 1.75(2), C(alkyl)---S = 1.82(2), C---C = 1.52(2), 
 1,3-C---C---C = 2.48(2) and 1,3-C---S---C = 2.83(2) Å. Both ClO₄⁻ ions 
 are also disordered, one over two equally occupied sites and the other over 
 three orientations with occupancies of 0.50, 0.30 and 0.20. The refined 
 restraints Cl---O = 1.43(2) and O...O = 2.34(2) Å were applied to those 
 residues. Finally, the acetone solvent molecule is also badly disordered. 
 Three partial solvent sites were located in the Fourier map, whose 
 occupancies sum to 0.7. The fixed restraints C---O = 1.22(2), C---C = 
 1.51(2), 1,3-C...C = 2.62(2) and 1,3-C...O = 2.37(2) Å were applied to 
 these sites. An anti-bumping restraint was also required between H15 and
 the disordered solvent methyl group C54Aⁱ (related by 1-x, 1-y, 1-z).

 All fully occupied non-H atoms, plus the two half-Cl atoms Cl47A and Cl47B, 
 were refined anisotropically, and H atoms were placed in calculated 
 positions and refined using a riding model.
;

_refine_ls_structure_factor_coef Fsqd
_refine_ls_matrix_type           full
_refine_ls_weighting_scheme      calc
_refine_ls_weighting_details     
'calc w=1/[σ²(Fo²)+(0.1290P)²+3.7003P] 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         7746
_refine_ls_number_parameters     543
_refine_ls_number_restraints     87
_refine_ls_R_factor_all          0.0872
_refine_ls_R_factor_gt           0.0728
_refine_ls_wR_factor_ref         0.2213
_refine_ls_wR_factor_gt          0.2041
_refine_ls_goodness_of_fit_ref   1.053
_refine_ls_restrained_S_all      1.065
_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_symmetry_multiplicity
_atom_site_calc_flag
_atom_site_refinement_flags
_atom_site_disorder_assembly
_atom_site_disorder_group
Fe1 Fe 0.22193(3) 0.60130(6) 0.05464(4) 0.0404(2) Uani 1 1 d . A .
N2 N 0.11658(15) 0.6272(3) 0.0333(2) 0.0378(7) Uani 1 1 d . . .
C3 C 0.08732(17) 0.7021(3) -0.0226(2) 0.0366(8) Uani 1 1 d . . .
C4 C 0.02133(19) 0.7347(4) -0.0319(3) 0.0432(9) Uani 1 1 d . . .
H4 H 0.0024 0.7876 -0.0720 0.052 Uiso 1 1 calc R . .
C5 C -0.01554(19) 0.6857(4) 0.0208(3) 0.0454(9) Uani 1 1 d . . .
C6 C 0.0142(2) 0.6065(4) 0.0793(3) 0.0485(10) Uani 1 1 d . . .
H6 H -0.0100 0.5725 0.1155 0.058 Uiso 1 1 calc R . .
C7 C 0.07969(19) 0.5801(3) 0.0821(3) 0.0407(8) Uani 1 1 d . . .
N8 N 0.13098(15) 0.7460(3) -0.07018(19) 0.0384(7) Uani 1 1 d . . .
N9 N 0.19646(16) 0.7159(3) -0.0501(2) 0.0485(8) Uani 1 1 d . . .
C10 C 0.2253(2) 0.7681(5) -0.1042(3) 0.0632(14) Uani 1 1 d . . .
H10 H 0.2708 0.7633 -0.1054 0.076 Uiso 1 1 calc R . .
C11 C 0.1791(3) 0.8313(5) -0.1595(3) 0.0673(14) Uani 1 1 d . . .
H11 H 0.1873 0.8755 -0.2036 0.081 Uiso 1 1 calc R . .
C12 C 0.1197(2) 0.8156(4) -0.1362(3) 0.0516(10) Uani 1 1 d . . .
H12 H 0.0785 0.8471 -0.1614 0.062 Uiso 1 1 calc R . .
N13 N 0.11530(17) 0.5022(3) 0.1382(2) 0.0451(8) Uani 1 1 d . . .
N14 N 0.18235(17) 0.4903(3) 0.1412(2) 0.0463(8) Uani 1 1 d . . .
C15 C 0.2011(3) 0.4092(4) 0.1950(3) 0.0602(12) Uani 1 1 d . . .
H15 H 0.2451 0.3825 0.2099 0.072 Uiso 1 1 calc RD . .
C16 C 0.1479(3) 0.3673(5) 0.2272(4) 0.0680(14) Uani 1 1 d . . .
H16 H 0.1490 0.3096 0.2665 0.082 Uiso 1 1 calc R . .
C17 C 0.0936(3) 0.4288(4) 0.1891(3) 0.0569(11) Uani 1 1 d . . .
H17 H 0.0496 0.4211 0.1971 0.068 Uiso 1 1 calc R . .
S18 S -0.09984(5) 0.71100(12) 0.01874(9) 0.0621(4) Uani 1 1 d . . .
C19 C -0.1190(2) 0.8433(4) -0.0376(3) 0.0566(11) Uani 1 1 d . . .
H19 H -0.1025 0.8396 -0.0901 0.068 Uiso 1 1 calc R . .
C20 C -0.0876(3) 0.9407(6) 0.0121(4) 0.0793(16) Uani 1 1 d . . .
H20A H -0.0982 1.0093 -0.0196 0.119 Uiso 1 1 calc R . .
H20B H -0.0396 0.9306 0.0252 0.119 Uiso 1 1 calc R . .
H20C H -0.1044 0.9457 0.0629 0.119 Uiso 1 1 calc R . .
C21 C -0.1948(3) 0.8514(6) -0.0571(5) 0.0840(19) Uani 1 1 d . . .
H21A H -0.2112 0.8516 -0.0059 0.126 Uiso 1 1 calc R . .
H21B H -0.2131 0.7875 -0.0905 0.126 Uiso 1 1 calc R . .
H21C H -0.2082 0.9202 -0.0873 0.126 Uiso 1 1 calc R . .
N22 N 0.32527(15) 0.5858(3) 0.1058(2) 0.0382(7) Uani 1 1 d . A .
C23 C 0.36258(19) 0.5088(4) 0.0773(2) 0.0422(9) Uani 1 1 d . . .
C24 C 0.4286(2) 0.4929(4) 0.1087(3) 0.0531(11) Uani 1 1 d . A .
H24 H 0.4533 0.4384 0.0867 0.064 Uiso 1 1 calc R . .
C25 C 0.4580(2) 0.5607(5) 0.1748(3) 0.0632(14) Uani 1 1 d D . .
C26 C 0.4208(2) 0.6427(5) 0.2047(3) 0.0550(12) Uani 1 1 d . A .
H26 H 0.4398 0.6900 0.2488 0.066 Uiso 1 1 calc R . .
C27 C 0.35472(18) 0.6517(4) 0.1669(2) 0.0394(8) Uani 1 1 d . . .
N28 N 0.32607(16) 0.4480(3) 0.0093(2) 0.0428(7) Uani 1 1 d . . .
N29 N 0.26044(16) 0.4728(3) -0.0175(2) 0.0441(8) Uani 1 1 d . . .
C30 C 0.2410(2) 0.4126(4) -0.0851(3) 0.0511(10) Uani 1 1 d . . .
H30 H 0.1974 0.4125 -0.1169 0.061 Uiso 1 1 calc R . .
C31 C 0.2932(3) 0.3494(5) -0.1032(3) 0.0645(13) Uani 1 1 d . . .
H31 H 0.2921 0.3002 -0.1481 0.077 Uiso 1 1 calc R . .
C32 C 0.3470(2) 0.3745(5) -0.0414(3) 0.0595(12) Uani 1 1 d . . .
H32 H 0.3903 0.3454 -0.0358 0.071 Uiso 1 1 calc R . .
N33 N 0.31133(16) 0.7340(3) 0.1879(2) 0.0439(8) Uani 1 1 d . A .
N34 N 0.24754(16) 0.7363(3) 0.1456(2) 0.0456(8) Uani 1 1 d . . .
C35 C 0.2201(2) 0.8244(4) 0.1748(3) 0.0565(11) Uani 1 1 d . A .
H35 H 0.1756 0.8471 0.1569 0.068 Uiso 1 1 calc R . .
C36 C 0.2661(3) 0.8787(5) 0.2355(4) 0.0642(13) Uani 1 1 d . . .
H36 H 0.2591 0.9433 0.2654 0.077 Uiso 1 1 calc R A .
C37 C 0.3229(2) 0.8194(4) 0.2426(3) 0.0594(12) Uani 1 1 d . A .
H37 H 0.3634 0.8348 0.2791 0.071 Uiso 1 1 calc R . .
S38A S 0.54350(15) 0.5354(4) 0.2131(2) 0.0316(6) Uiso 0.34 1 d PD A 1
C39A C 0.5687(13) 0.648(2) 0.2869(18) 0.23(3) Uiso 0.34 1 d PD A 1
H39A H 0.5357 0.6553 0.3229 0.281 Uiso 0.34 1 calc PR A 1
C40A C 0.5725(14) 0.756(2) 0.2423(16) 0.115(8) Uiso 0.34 1 d PD A 1
H40A H 0.5283 0.7776 0.2131 0.172 Uiso 0.34 1 calc PR A 1
H40B H 0.6015 0.7474 0.2029 0.172 Uiso 0.34 1 calc PR A 1
H40C H 0.5902 0.8146 0.2818 0.172 Uiso 0.34 1 calc PR A 1
C41A C 0.6348(10) 0.6115(19) 0.3386(13) 0.086(6) Uiso 0.34 1 d PD A 1
H41A H 0.6288 0.5425 0.3676 0.129 Uiso 0.34 1 calc PR A 1
H41B H 0.6516 0.6697 0.3785 0.129 Uiso 0.34 1 calc PR A 1
H41C H 0.6664 0.5987 0.3029 0.129 Uiso 0.34 1 calc PR A 1
S38B S 0.54894(18) 0.5762(4) 0.2012(2) 0.0499(10) Uiso 0.33 1 d PD A 2
C39B C 0.5671(6) 0.6376(16) 0.2997(8) 0.048(4) Uiso 0.33 1 d PD A 2
H39B H 0.5400 0.7067 0.2987 0.058 Uiso 0.33 1 calc PR A 2
C40B C 0.5499(16) 0.559(3) 0.364(2) 0.155(13) Uiso 0.33 1 d PD A 2
H40D H 0.5019 0.5544 0.3581 0.232 Uiso 0.33 1 calc PR A 2
H40E H 0.5691 0.5874 0.4191 0.232 Uiso 0.33 1 calc PR A 2
H40F H 0.5677 0.4849 0.3575 0.232 Uiso 0.33 1 calc PR A 2
C41B C 0.6401(9) 0.670(2) 0.3168(14) 0.087(6) Uiso 0.33 1 d PD A 2
H41D H 0.6668 0.6081 0.3431 0.130 Uiso 0.33 1 calc PR A 2
H41E H 0.6469 0.7352 0.3533 0.130 Uiso 0.33 1 calc PR A 2
H41F H 0.6534 0.6889 0.2652 0.130 Uiso 0.33 1 calc PR A 2
S38C S 0.53510(19) 0.5002(4) 0.2273(2) 0.0486(10) Uiso 0.33 1 d PD A 3
C39C C 0.5618(5) 0.5992(11) 0.3120(7) 0.035(3) Uiso 0.33 1 d PD A 3
H39C H 0.5256 0.6078 0.3433 0.043 Uiso 0.33 1 calc PR A 3
C40C C 0.5752(8) 0.7113(13) 0.2765(9) 0.058(3) Uiso 0.33 1 d PD A 3
H40G H 0.5338 0.7426 0.2461 0.087 Uiso 0.33 1 calc PR A 3
H40H H 0.6061 0.7018 0.2395 0.087 Uiso 0.33 1 calc PR A 3
H40I H 0.5943 0.7619 0.3211 0.087 Uiso 0.33 1 calc PR A 3
C41C C 0.6205(8) 0.5472(15) 0.3670(10) 0.072(4) Uiso 0.33 1 d PD A 3
H41G H 0.6106 0.4695 0.3775 0.109 Uiso 0.33 1 calc PR A 3
H41H H 0.6305 0.5879 0.4190 0.109 Uiso 0.33 1 calc PR A 3
H41I H 0.6586 0.5504 0.3403 0.109 Uiso 0.33 1 calc PR A 3
Cl42A Cl 0.4342(2) 0.7601(4) 0.4623(3) 0.0622(14) Uiso 0.50 1 d PD B 1
O43A O 0.4984(6) 0.7989(12) 0.4992(9) 0.119(5) Uiso 0.50 1 d PD B 1
O44A O 0.3948(10) 0.8645(14) 0.4323(13) 0.177(12) Uiso 0.50 1 d PD B 1
O45A O 0.4028(6) 0.7169(10) 0.5231(6) 0.074(3) Uiso 0.50 1 d PD B 1
O46A O 0.4330(6) 0.6923(9) 0.3954(6) 0.093(3) Uiso 0.50 1 d PD B 1
Cl42B Cl 0.4321(3) 0.7845(6) 0.4636(5) 0.0466(16) Uiso 0.30 1 d PD C 2
O43B O 0.4888(6) 0.8361(12) 0.5168(8) 0.068(4) Uiso 0.30 1 d PD C 2
O44B O 0.3794(5) 0.8572(9) 0.4374(6) 0.042(2) Uiso 0.30 1 d PD C 2
O45B O 0.4142(12) 0.6882(16) 0.5064(14) 0.161(13) Uiso 0.30 1 d PD C 2
O46B O 0.4580(8) 0.7459(14) 0.3921(8) 0.089(4) Uiso 0.30 1 d PD C 2
Cl42C Cl 0.4296(5) 0.7766(11) 0.4459(6) 0.061(3) Uiso 0.20 1 d PD D 3
O43C O 0.5015(7) 0.7655(19) 0.4521(16) 0.096(7) Uiso 0.20 1 d PD D 3
O44C O 0.4215(16) 0.740(2) 0.5301(11) 0.126(15) Uiso 0.20 1 d PD D 3
O45C O 0.3990(9) 0.6891(12) 0.3913(9) 0.053(4) Uiso 0.20 1 d PD D 3
O46C O 0.4074(10) 0.8824(12) 0.4300(11) 0.052(5) Uiso 0.20 1 d PD D 3
Cl47A Cl 0.0736(6) 0.9897(10) 0.2294(7) 0.0528(17) Uani 0.50 1 d PD E 1
O48A O 0.1377(4) 1.0325(8) 0.2263(6) 0.066(2) Uiso 0.50 1 d PD E 1
O49A O 0.0199(4) 1.0634(8) 0.2018(6) 0.078(3) Uiso 0.50 1 d PD E 1
O50A O 0.0687(5) 0.9443(9) 0.3078(5) 0.072(3) Uiso 0.50 1 d PD E 1
O51A O 0.0640(5) 0.8901(9) 0.1781(6) 0.085(3) Uiso 0.50 1 d PD E 1
Cl47B Cl 0.0788(6) 1.0138(10) 0.2360(8) 0.058(2) Uani 0.50 1 d PD F 2
O48B O 0.1421(5) 1.0681(9) 0.2362(6) 0.079(3) Uiso 0.50 1 d PD F 2
O49B O 0.0306(5) 1.1010(8) 0.2217(6) 0.081(3) Uiso 0.50 1 d PD F 2
O50B O 0.0829(5) 0.9731(8) 0.3174(5) 0.062(2) Uiso 0.50 1 d PD F 2
O51B O 0.0682(5) 0.9346(9) 0.1689(6) 0.091(3) Uiso 0.50 1 d PD F 2
O52A O 0.6860(19) 0.518(4) 0.622(3) 0.122(15) Uiso 0.15 1 d PD G 1
C53A C 0.633(2) 0.565(6) 0.611(3) 0.09(2) Uiso 0.15 1 d PD G 1
C54A C 0.6112(14) 0.620(8) 0.685(3) 0.19(4) Uiso 0.15 1 d PD G 1
H54A H 0.6496 0.6286 0.7299 0.283 Uiso 0.15 1 calc PR G 1
H54B H 0.5785 0.5722 0.7037 0.283 Uiso 0.15 1 calc PR G 1
H54C H 0.5918 0.6925 0.6692 0.283 Uiso 0.15 1 calc PR G 1
C55A C 0.584(3) 0.556(7) 0.531(3) 0.14(2) Uiso 0.15 1 d PD G 1
H55A H 0.6067 0.5328 0.4875 0.212 Uiso 0.15 1 calc PR G 1
H55B H 0.5630 0.6288 0.5165 0.212 Uiso 0.15 1 calc PR G 1
H55C H 0.5498 0.5014 0.5358 0.212 Uiso 0.15 1 calc PR G 1
O52B O 0.6607(12) 0.541(2) 0.6980(13) 0.116(8) Uiso 0.25 1 d PD H 2
C53B C 0.6407(11) 0.540(3) 0.6240(14) 0.072(8) Uiso 0.25 1 d PD H 2
C54B C 0.6850(14) 0.524(4) 0.5628(18) 0.105(10) Uiso 0.25 1 d PD H 2
H54D H 0.7303 0.5109 0.5922 0.158 Uiso 0.25 1 calc PR H 2
H54E H 0.6838 0.5911 0.5289 0.158 Uiso 0.25 1 calc PR H 2
H54F H 0.6697 0.4602 0.5278 0.158 Uiso 0.25 1 calc PR H 2
C55B C 0.5676(10) 0.569(3) 0.5892(15) 0.072(6) Uiso 0.25 1 d PD H 2
H55D H 0.5447 0.5818 0.6346 0.108 Uiso 0.25 1 calc PR H 2
H55E H 0.5466 0.5077 0.5553 0.108 Uiso 0.25 1 calc PR H 2
H55F H 0.5652 0.6369 0.5559 0.108 Uiso 0.25 1 calc PR H 2
O52C O 0.6500(9) 0.5951(16) 0.7168(9) 0.091(5) Uiso 0.30 1 d PD I 3
C53C C 0.6289(8) 0.5717(17) 0.6461(10) 0.060(4) Uiso 0.30 1 d PD I 3
C54C C 0.6723(12) 0.542(3) 0.5858(15) 0.094(8) Uiso 0.30 1 d PD I 3
H54G H 0.7187 0.5460 0.6133 0.141 Uiso 0.30 1 calc PR I 3
H54H H 0.6640 0.5940 0.5397 0.141 Uiso 0.30 1 calc PR I 3
H54I H 0.6621 0.4660 0.5655 0.141 Uiso 0.30 1 calc PR I 3
C55C C 0.5546(9) 0.588(3) 0.6130(16) 0.099(8) Uiso 0.30 1 d PD I 3
H55G H 0.5339 0.6175 0.6566 0.148 Uiso 0.30 1 calc PR I 3
H55H H 0.5345 0.5166 0.5940 0.148 Uiso 0.30 1 calc PR I 3
H55I H 0.5481 0.6408 0.5671 0.148 Uiso 0.30 1 calc PR I 3


_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 N22 2.125(3) . ?
Fe1 N2 2.139(3) . ?
Fe1 N29 2.180(3) . ?
Fe1 N9 2.181(4) . ?
Fe1 N34 2.188(4) . ?
Fe1 N14 2.215(4) . ?
N2 C7 1.333(5) . ?
N2 C3 1.335(5) . ?
C3 C4 1.386(5) . ?
C3 N8 1.404(5) . ?
C4 C5 1.388(6) . ?
C4 H4 0.9400 . ?
C5 C6 1.398(6) . ?
C5 S18 1.747(4) . ?
C6 C7 1.371(6) . ?
C6 H6 0.9400 . ?
C7 N13 1.407(5) . ?
N8 C12 1.350(6) . ?
N8 N9 1.364(4) . ?
N9 C10 1.319(6) . ?
C10 C11 1.396(7) . ?
C10 H10 0.9400 . ?
C11 C12 1.361(7) . ?
C11 H11 0.9400 . ?
C12 H12 0.9400 . ?
N13 C17 1.347(6) . ?
N13 N14 1.372(5) . ?
N14 C15 1.315(6) . ?
C15 C16 1.398(8) . ?
C15 H15 0.9400 . ?
C16 C17 1.376(7) . ?
C16 H16 0.9400 . ?
C17 H17 0.9400 . ?
S18 C19 1.831(5) . ?
C19 C20 1.490(8) . ?
C19 C21 1.525(6) . ?
C19 H19 0.9900 . ?
C20 H20A 0.9700 . ?
C20 H20B 0.9700 . ?
C20 H20C 0.9700 . ?
C21 H21A 0.9700 . ?
C21 H21B 0.9700 . ?
C21 H21C 0.9700 . ?
N22 C27 1.324(5) . ?
N22 C23 1.338(5) . ?
C23 C24 1.362(5) . ?
C23 N28 1.415(5) . ?
C24 C25 1.393(7) . ?
C24 H24 0.9400 . ?
C25 C26 1.388(7) . ?
C25 S38A 1.766(5) . ?
C25 S38C 1.794(5) . ?
C25 S38B 1.837(5) . ?
C26 C27 1.377(5) . ?
C26 H26 0.9400 . ?
C27 N33 1.412(5) . ?
N28 C32 1.339(6) . ?
N28 N29 1.361(4) . ?
N29 C30 1.319(6) . ?
C30 C31 1.390(7) . ?
C30 H30 0.9400 . ?
C31 C32 1.376(7) . ?
C31 H31 0.9400 . ?
C32 H32 0.9400 . ?
N33 C37 1.348(6) . ?
N33 N34 1.354(5) . ?
N34 C35 1.326(6) . ?
C35 C36 1.390(7) . ?
C35 H35 0.9400 . ?
C36 C37 1.346(7) . ?
C36 H36 0.9400 . ?
C37 H37 0.9400 . ?
S38A C39A 1.815(19) . ?
C39A C40A 1.49(2) . ?
C39A C41A 1.513(18) . ?
C39A H39A 0.9900 . ?
C40A H40A 0.9700 . ?
C40A H40B 0.9700 . ?
C40A H40C 0.9700 . ?
C41A H41A 0.9700 . ?
C41A H41B 0.9700 . ?
C41A H41C 0.9700 . ?
S38B C39B 1.752(11) . ?
C39B C40B 1.512(18) . ?
C39B C41B 1.518(16) . ?
C39B H39B 0.9900 . ?
C40B H40D 0.9700 . ?
C40B H40E 0.9700 . ?
C40B H40F 0.9700 . ?
C41B H41D 0.9700 . ?
C41B H41E 0.9700 . ?
C41B H41F 0.9700 . ?
S38C C39C 1.826(10) . ?
C39C C41C 1.488(14) . ?
C39C C40C 1.504(15) . ?
C39C H39C 0.9900 . ?
C40C H40G 0.9700 . ?
C40C H40H 0.9700 . ?
C40C H40I 0.9700 . ?
C41C H41G 0.9700 . ?
C41C H41H 0.9700 . ?
C41C H41I 0.9700 . ?
Cl42A O46A 1.363(10) . ?
Cl42A O45A 1.393(9) . ?
Cl42A O43A 1.412(11) . ?
Cl42A O44A 1.511(12) . ?
Cl42B O44B 1.385(10) . ?
Cl42B O45B 1.432(14) . ?
Cl42B O43B 1.445(11) . ?
Cl42B O46B 1.461(12) . ?
Cl42C O46C 1.346(14) . ?
Cl42C O45C 1.437(14) . ?
Cl42C O43C 1.461(14) . ?
Cl42C O44C 1.497(15) . ?
Cl47A O49A 1.410(13) . ?
Cl47A O48A 1.420(12) . ?
Cl47A O50A 1.422(12) . ?
Cl47A O51A 1.447(13) . ?
Cl47B O50B 1.415(13) . ?
Cl47B O49B 1.418(13) . ?
Cl47B O51B 1.436(12) . ?
Cl47B O48B 1.449(13) . ?
O52A C53A 1.211(18) . ?
C53A C55A 1.504(18) . ?
C53A C54A 1.519(18) . ?
C54A H54A 0.9700 . ?
C54A H54B 0.9700 . ?
C54A H54C 0.9700 . ?
C55A H55A 0.9700 . ?
C55A H55B 0.9700 . ?
C55A H55C 0.9700 . ?
O52B C53B 1.207(17) . ?
C53B C54B 1.500(17) . ?
C53B C55B 1.532(17) . ?
C54B H54D 0.9700 . ?
C54B H54E 0.9700 . ?
C54B H54F 0.9700 . ?
C55B H55D 0.9700 . ?
C55B H55E 0.9700 . ?
C55B H55F 0.9700 . ?
O52C C53C 1.194(15) . ?
C53C C54C 1.503(16) . ?
C53C C55C 1.523(16) . ?
C54C H54G 0.9700 . ?
C54C H54H 0.9700 . ?
C54C H54I 0.9700 . ?
C55C H55G 0.9700 . ?
C55C H55H 0.9700 . ?
C55C H55I 0.9700 . ?

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
N22 Fe1 N2 166.08(13) . . ?
N22 Fe1 N29 73.44(12) . . ?
N2 Fe1 N29 118.34(13) . . ?
N22 Fe1 N9 115.51(13) . . ?
N2 Fe1 N9 72.89(12) . . ?
N29 Fe1 N9 93.55(14) . . ?
N22 Fe1 N34 73.04(12) . . ?
N2 Fe1 N34 95.92(12) . . ?
N29 Fe1 N34 145.63(12) . . ?
N9 Fe1 N34 94.02(15) . . ?
N22 Fe1 N14 98.98(13) . . ?
N2 Fe1 N14 72.81(13) . . ?
N29 Fe1 N14 98.77(14) . . ?
N9 Fe1 N14 145.42(12) . . ?
N34 Fe1 N14 93.72(14) . . ?
C7 N2 C3 117.8(3) . . ?
C7 N2 Fe1 121.0(3) . . ?
C3 N2 Fe1 120.6(2) . . ?
N2 C3 C4 123.8(4) . . ?
N2 C3 N8 112.7(3) . . ?
C4 C3 N8 123.5(3) . . ?
C3 C4 C5 117.1(4) . . ?
C3 C4 H4 121.5 . . ?
C5 C4 H4 121.5 . . ?
C4 C5 C6 119.9(4) . . ?
C4 C5 S18 125.1(3) . . ?
C6 C5 S18 115.0(3) . . ?
C7 C6 C5 117.8(4) . . ?
C7 C6 H6 121.1 . . ?
C5 C6 H6 121.1 . . ?
N2 C7 C6 123.5(4) . . ?
N2 C7 N13 113.1(3) . . ?
C6 C7 N13 123.3(4) . . ?
C12 N8 N9 111.0(3) . . ?
C12 N8 C3 130.8(3) . . ?
N9 N8 C3 118.2(3) . . ?
C10 N9 N8 105.3(3) . . ?
C10 N9 Fe1 139.6(3) . . ?
N8 N9 Fe1 115.1(2) . . ?
N9 C10 C11 111.0(4) . . ?
N9 C10 H10 124.5 . . ?
C11 C10 H10 124.5 . . ?
C12 C11 C10 105.6(4) . . ?
C12 C11 H11 127.2 . . ?
C10 C11 H11 127.2 . . ?
N8 C12 C11 107.0(4) . . ?
N8 C12 H12 126.5 . . ?
C11 C12 H12 126.5 . . ?
C17 N13 N14 111.4(4) . . ?
C17 N13 C7 130.1(4) . . ?
N14 N13 C7 118.4(3) . . ?
C15 N14 N13 104.8(4) . . ?
C15 N14 Fe1 141.0(3) . . ?
N13 N14 Fe1 114.1(2) . . ?
N14 C15 C16 111.9(4) . . ?
N14 C15 H15 124.1 . . ?
C16 C15 H15 124.1 . . ?
C17 C16 C15 105.0(4) . . ?
C17 C16 H16 127.5 . . ?
C15 C16 H16 127.5 . . ?
N13 C17 C16 106.9(4) . . ?
N13 C17 H17 126.5 . . ?
C16 C17 H17 126.5 . . ?
C5 S18 C19 105.6(2) . . ?
C20 C19 C21 112.1(5) . . ?
C20 C19 S18 111.4(4) . . ?
C21 C19 S18 105.5(4) . . ?
C20 C19 H19 109.2 . . ?
C21 C19 H19 109.2 . . ?
S18 C19 H19 109.2 . . ?
C19 C20 H20A 109.5 . . ?
C19 C20 H20B 109.5 . . ?
H20A C20 H20B 109.5 . . ?
C19 C20 H20C 109.5 . . ?
H20A C20 H20C 109.5 . . ?
H20B C20 H20C 109.5 . . ?
C19 C21 H21A 109.5 . . ?
C19 C21 H21B 109.5 . . ?
H21A C21 H21B 109.5 . . ?
C19 C21 H21C 109.5 . . ?
H21A C21 H21C 109.5 . . ?
H21B C21 H21C 109.5 . . ?
C27 N22 C23 117.9(3) . . ?
C27 N22 Fe1 121.2(2) . . ?
C23 N22 Fe1 120.9(3) . . ?
N22 C23 C24 123.7(4) . . ?
N22 C23 N28 112.3(3) . . ?
C24 C23 N28 123.9(4) . . ?
C23 C24 C25 117.3(4) . . ?
C23 C24 H24 121.3 . . ?
C25 C24 H24 121.3 . . ?
C26 C25 C24 120.2(4) . . ?
C26 C25 S38A 124.7(4) . . ?
C24 C25 S38A 115.1(4) . . ?
C26 C25 S38C 127.2(4) . . ?
C24 C25 S38C 110.3(4) . . ?
C26 C25 S38B 116.7(4) . . ?
C24 C25 S38B 120.2(3) . . ?
C27 C26 C25 117.0(4) . . ?
C27 C26 H26 121.5 . . ?
C25 C26 H26 121.5 . . ?
N22 C27 C26 123.8(4) . . ?
N22 C27 N33 112.6(3) . . ?
C26 C27 N33 123.6(4) . . ?
C32 N28 N29 111.0(4) . . ?
C32 N28 C23 130.1(4) . . ?
N29 N28 C23 118.5(3) . . ?
C30 N29 N28 105.6(3) . . ?
C30 N29 Fe1 139.6(3) . . ?
N28 N29 Fe1 114.6(2) . . ?
N29 C30 C31 111.1(4) . . ?
N29 C30 H30 124.4 . . ?
C31 C30 H30 124.4 . . ?
C32 C31 C30 105.1(4) . . ?
C32 C31 H31 127.5 . . ?
C30 C31 H31 127.5 . . ?
N28 C32 C31 107.2(4) . . ?
N28 C32 H32 126.4 . . ?
C31 C32 H32 126.4 . . ?
C37 N33 N34 110.7(3) . . ?
C37 N33 C27 130.7(4) . . ?
N34 N33 C27 118.5(3) . . ?
C35 N34 N33 105.3(4) . . ?
C35 N34 Fe1 140.3(3) . . ?
N33 N34 Fe1 114.5(2) . . ?
N34 C35 C36 110.7(4) . . ?
N34 C35 H35 124.6 . . ?
C36 C35 H35 124.6 . . ?
C37 C36 C35 105.6(4) . . ?
C37 C36 H36 127.2 . . ?
C35 C36 H36 127.2 . . ?
C36 C37 N33 107.7(4) . . ?
C36 C37 H37 126.2 . . ?
N33 C37 H37 126.2 . . ?
C25 S38A C39A 104.0(9) . . ?
C40A C39A C41A 113.4(18) . . ?
C40A C39A S38A 110(2) . . ?
C41A C39A S38A 105.5(17) . . ?
C40A C39A H39A 109.2 . . ?
C41A C39A H39A 109.2 . . ?
S38A C39A H39A 109.2 . . ?
C39A C40A H40A 109.5 . . ?
C39A C40A H40B 109.5 . . ?
H40A C40A H40B 109.5 . . ?
C39A C40A H40C 109.5 . . ?
H40A C40A H40C 109.5 . . ?
H40B C40A H40C 109.5 . . ?
C39A C41A H41A 109.5 . . ?
C39A C41A H41B 109.5 . . ?
H41A C41A H41B 109.5 . . ?
C39A C41A H41C 109.5 . . ?
H41A C41A H41C 109.5 . . ?
H41B C41A H41C 109.5 . . ?
C39B S38B C25 106.1(5) . . ?
C40B C39B C41B 112.8(14) . . ?
C40B C39B S38B 111.1(19) . . ?
C41B C39B S38B 107.4(12) . . ?
C40B C39B H39B 108.5 . . ?
C41B C39B H39B 108.5 . . ?
S38B C39B H39B 108.5 . . ?
C39B C40B H40D 109.5 . . ?
C39B C40B H40E 109.5 . . ?
H40D C40B H40E 109.5 . . ?
C39B C40B H40F 109.5 . . ?
H40D C40B H40F 109.5 . . ?
H40E C40B H40F 109.5 . . ?
C39B C41B H41D 109.5 . . ?
C39B C41B H41E 109.5 . . ?
H41D C41B H41E 109.5 . . ?
C39B C41B H41F 109.5 . . ?
H41D C41B H41F 109.5 . . ?
H41E C41B H41F 109.5 . . ?
C25 S38C C39C 102.2(4) . . ?
C41C C39C C40C 114.7(11) . . ?
C41C C39C S38C 106.3(10) . . ?
C40C C39C S38C 109.0(9) . . ?
C41C C39C H39C 108.9 . . ?
C40C C39C H39C 108.9 . . ?
S38C C39C H39C 108.9 . . ?
C39C C40C H40G 109.5 . . ?
C39C C40C H40H 109.5 . . ?
H40G C40C H40H 109.5 . . ?
C39C C40C H40I 109.5 . . ?
H40G C40C H40I 109.5 . . ?
H40H C40C H40I 109.5 . . ?
C39C C41C H41G 109.5 . . ?
C39C C41C H41H 109.5 . . ?
H41G C41C H41H 109.5 . . ?
C39C C41C H41I 109.5 . . ?
H41G C41C H41I 109.5 . . ?
H41H C41C H41I 109.5 . . ?
O46A Cl42A O45A 115.4(8) . . ?
O46A Cl42A O43A 114.0(8) . . ?
O45A Cl42A O43A 109.6(8) . . ?
O46A Cl42A O44A 107.5(9) . . ?
O45A Cl42A O44A 104.2(9) . . ?
O43A Cl42A O44A 105.2(10) . . ?
O44B Cl42B O45B 113.2(11) . . ?
O44B Cl42B O43B 114.0(8) . . ?
O45B Cl42B O43B 107.2(11) . . ?
O44B Cl42B O46B 109.3(9) . . ?
O45B Cl42B O46B 108.5(11) . . ?
O43B Cl42B O46B 104.2(9) . . ?
O46C Cl42C O45C 117.9(11) . . ?
O46C Cl42C O43C 113.3(12) . . ?
O45C Cl42C O43C 106.6(12) . . ?
O46C Cl42C O44C 111.1(13) . . ?
O45C Cl42C O44C 104.6(12) . . ?
O43C Cl42C O44C 101.9(12) . . ?
O49A Cl47A O48A 115.7(10) . . ?
O49A Cl47A O50A 109.7(9) . . ?
O48A Cl47A O50A 113.7(9) . . ?
O49A Cl47A O51A 108.4(9) . . ?
O48A Cl47A O51A 106.9(9) . . ?
O50A Cl47A O51A 101.2(9) . . ?
O50B Cl47B O49B 108.4(9) . . ?
O50B Cl47B O51B 118.5(10) . . ?
O49B Cl47B O51B 111.1(10) . . ?
O50B Cl47B O48B 105.4(9) . . ?
O49B Cl47B O48B 105.5(9) . . ?
O51B Cl47B O48B 106.9(10) . . ?
O52A C53A C55A 121(2) . . ?
O52A C53A C54A 118.9(19) . . ?
C55A C53A C54A 119.3(17) . . ?
C53A C54A H54A 109.5 . . ?
C53A C54A H54B 109.5 . . ?
H54A C54A H54B 109.5 . . ?
C53A C54A H54C 109.5 . . ?
H54A C54A H54C 109.5 . . ?
H54B C54A H54C 109.5 . . ?
C53A C55A H55A 109.5 . . ?
C53A C55A H55B 109.5 . . ?
H55A C55A H55B 109.5 . . ?
C53A C55A H55C 109.5 . . ?
H55A C55A H55C 109.5 . . ?
H55B C55A H55C 109.5 . . ?
O52B C53B C54B 123.5(17) . . ?
O52B C53B C55B 119.1(16) . . ?
C54B C53B C55B 117.1(15) . . ?
C53B C54B H54D 109.5 . . ?
C53B C54B H54E 109.5 . . ?
H54D C54B H54E 109.5 . . ?
C53B C54B H54F 109.5 . . ?
H54D C54B H54F 109.5 . . ?
H54E C54B H54F 109.5 . . ?
C53B C55B H55D 109.5 . . ?
C53B C55B H55E 109.5 . . ?
H55D C55B H55E 109.5 . . ?
C53B C55B H55F 109.5 . . ?
H55D C55B H55F 109.5 . . ?
H55E C55B H55F 109.5 . . ?
O52C C53C C54C 123.7(15) . . ?
O52C C53C C55C 117.5(15) . . ?
C54C C53C C55C 118.3(14) . . ?
C53C C54C H54G 109.5 . . ?
C53C C54C H54H 109.5 . . ?
H54G C54C H54H 109.5 . . ?
C53C C54C H54I 109.5 . . ?
H54G C54C H54I 109.5 . . ?
H54H C54C H54I 109.5 . . ?
C53C C55C H55G 109.5 . . ?
C53C C55C H55H 109.5 . . ?
H55G C55C H55H 109.5 . . ?
C53C C55C H55I 109.5 . . ?
H55G C55C H55I 109.5 . . ?
H55H C55C H55I 109.5 . . ?

_diffrn_measured_fraction_theta_max 0.968
_diffrn_reflns_theta_full        73.90
_diffrn_measured_fraction_theta_full 0.968
_refine_diff_density_max         1.091
_refine_diff_density_min         -0.972
_refine_diff_density_rms         0.086
_exptl_crystal_recrystallization_method 
'Re-crystallisation from solvent: Acetone-diethyl ether'
_exptl_crystal_preparation       'Magnetic properties'
####################################################################### 
# 
# This file contains crystal structure data downloaded from the 
# Cambridge Structural Database (CSD) hosted by the Cambridge 
# Crystallographic Data Centre (CCDC).
# 
# Full information about CCDC data access policies and citation 
# guidelines are available at http://www.ccdc.cam.ac.uk/access/V1 
# 
# Audit and citation data items may have been added by the CCDC. 
# Please retain this information to preserve the provenance of 
# this file and to allow appropriate attribution of the data. 
# 
#######################################################################

data_rk137H2O_020K
_database_code_depnum_ccdc_archive 'CCDC 1564665'
_audit_update_record             
;
2017-07-28 deposited with the CCDC.
2017-11-20 downloaded from the CCDC.
;
_chemical_name_common            ?
_chemical_name_systematic        ?
_chemical_formula_moiety         'C28 H30 Fe N10 S2, 2(B F4), H2 O'
_chemical_formula_sum            'C28 H32 B2 F8 Fe N10 O S2'
_chemical_formula_weight         818.22
_chemical_melting_point          'not measured'
loop_
_atom_type_symbol
_atom_type_description
_atom_type_scat_dispersion_real
_atom_type_scat_dispersion_imag
_atom_type_scat_source
C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
B B 0.0013 0.0007 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
F F 0.0171 0.0103 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Fe Fe 0.3463 0.8444 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
S S 0.1246 0.1234 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'

_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.
;
_space_group_crystal_system      monoclinic
_space_group_IT_number           14
_space_group_name_H-M_alt        'P 1 21/c 1'
_space_group_name_Hall           '-P 2ybc'
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                   19.7442(10)
_cell_length_b                   12.1364(5)
_cell_length_c                   15.0558(9)
_cell_angle_alpha                90
_cell_angle_beta                 103.004(5)
_cell_angle_gamma                90
_cell_volume                     3515.2(3)
_cell_formula_units_Z            4
_cell_measurement_reflns_used    3428
_cell_measurement_temperature    20
_cell_measurement_theta_max      31.0800
_cell_measurement_theta_min      3.2360
_exptl_absorpt_coefficient_mu    0.632
_exptl_absorpt_correction_T_max  0.951
_exptl_absorpt_correction_T_min  0.917
_exptl_absorpt_correction_type   analytical
_exptl_absorpt_process_details   
;
CrysAlisPro 1.171.38.41 (Rigaku Oxford Diffraction, 2015)
Analytical numeric absorption correction using a multifaceted crystal
			model based on expressions derived by R.C. Clark & J.S. Reid.
(Clark, R. C. & Reid, J. S. (1995). Acta Cryst. A51, 887-897)
Empirical absorption correction using spherical harmonics,
 implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_absorpt_special_details   ?
_exptl_crystal_colour            'dark orange'
_exptl_crystal_colour_modifier   dark
_exptl_crystal_colour_primary    orange
_exptl_crystal_density_diffrn    1.546
_exptl_crystal_density_meas      'not measured'
_exptl_crystal_density_method    none
_exptl_crystal_description       block
_exptl_crystal_F_000             1672
loop_
_exptl_crystal_face_index_h
_exptl_crystal_face_index_k
_exptl_crystal_face_index_l
_exptl_crystal_face_perp_dist
-17 13 -1 0.0697
-18 -13 1 0.0368
-2 -5 20 0.0806
-10 -6 19 0.0746
18 13 0 0.0633
14 12 -13 0.0625
18 -12 -1 0.0323
-8 -3 -18 0.0897

_exptl_crystal_size_max          0.225
_exptl_crystal_size_mid          0.111
_exptl_crystal_size_min          0.101
loop_
_exptl_oxdiff_crystal_face_indexfrac_h
_exptl_oxdiff_crystal_face_indexfrac_k
_exptl_oxdiff_crystal_face_indexfrac_l
_exptl_oxdiff_crystal_face_x
_exptl_oxdiff_crystal_face_y
_exptl_oxdiff_crystal_face_z
-17.4717 13.2200 -0.8557 -0.9489 0.0211 -0.3518
-18.2113 -12.8004 1.0756 -0.0265 -0.8969 0.4407
-1.9952 -5.0625 19.9579 0.0315 0.2746 0.9568
-9.9604 -5.9656 19.0063 -0.1447 0.0172 0.9631
18.2179 12.7962 -0.0777 0.0218 0.9224 -0.3999
14.1385 11.8966 -13.0285 0.0101 0.4566 -0.8925
18.4786 -12.2228 -1.1437 0.9495 -0.0105 0.2405
-8.1352 -2.8330 -17.9208 -0.0251 -0.7651 -0.6318

_exptl_transmission_factor_max   ?
_exptl_transmission_factor_min   ?
_diffrn_reflns_av_R_equivalents  0.0703
_diffrn_reflns_av_unetI/netI     0.1103
_diffrn_reflns_Laue_measured_fraction_full 0.998
_diffrn_reflns_Laue_measured_fraction_max 0.999
_diffrn_reflns_limit_h_max       25
_diffrn_reflns_limit_h_min       -24
_diffrn_reflns_limit_k_max       14
_diffrn_reflns_limit_k_min       -15
_diffrn_reflns_limit_l_max       19
_diffrn_reflns_limit_l_min       -16
_diffrn_reflns_number            18249
_diffrn_reflns_point_group_measured_fraction_full 0.998
_diffrn_reflns_point_group_measured_fraction_max 0.999
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         27.000
_diffrn_reflns_theta_min         3.091
_diffrn_ambient_temperature      20.0
_diffrn_detector                 'CCD plate'
_diffrn_detector_area_resol_mean 16.1852
_diffrn_detector_type            Sapphire3
_diffrn_measured_fraction_theta_full 0.998
_diffrn_measured_fraction_theta_max 0.999
_diffrn_measurement_details      
;
List of Runs (angles in degrees, time in seconds):

  # Type    Start    End  Width  tₑₓₚ   ω     θ     κ     φ   Frames
#--------------------------------------------------------------------------
  1  ω      0.00  38.00   1.00    7.50    --  -33.81   0.00  90.00   38
  2  ω    -55.00 -11.00   1.00    7.50    --  -33.81  38.00 150.00   44
  3  ω    -73.00 -29.00   1.00    7.50    --  -33.81 -38.00 -30.00   44
  4  ω     58.00 109.00   1.00    7.50    --   35.69 178.00 -30.00   51
  5  ω     57.00 107.00   1.00    7.50    --   35.69 178.00-120.00   50
  6  ω   -109.00 -33.00   1.00    7.50    --  -33.81   0.00  90.00   76
;
_diffrn_measurement_device       'four-circle diffractometer'
_diffrn_measurement_device_type  'Xcalibur, Sapphire3'
_diffrn_measurement_method       'ω scans'
_diffrn_orient_matrix_type       
'CrysAlisPro convention (1999,Acta A55,543-557)'
_diffrn_orient_matrix_UB_11      0.0268742000
_diffrn_orient_matrix_UB_12      -0.0365844000
_diffrn_orient_matrix_UB_13      -0.0050142000
_diffrn_orient_matrix_UB_21      0.0251297000
_diffrn_orient_matrix_UB_22      0.0364618000
_diffrn_orient_matrix_UB_23      0.0255209000
_diffrn_orient_matrix_UB_31      -0.0025620000
_diffrn_orient_matrix_UB_32      -0.0273588000
_diffrn_orient_matrix_UB_33      0.0407438000
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_source                   'fine-focus sealed X-ray tube'
_diffrn_source_type              'Enhance (Mo) X-ray Source'
_reflns_Friedel_coverage         0.000
_reflns_Friedel_fraction_full    .
_reflns_Friedel_fraction_max     .
_reflns_number_gt                5047
_reflns_number_total             7671
_reflns_odcompleteness_completeness 99.79
_reflns_odcompleteness_iscentric 1
_reflns_odcompleteness_theta     26.32
_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.
;
_reflns_threshold_expression     'I > 2σ(I)'
_computing_cell_refinement       'CrysAlisPro 1.171.38.41 (Rigaku OD, 2015)'
_computing_data_collection       'CrysAlisPro 1.171.37.31c (Rigaku OD, 2014)'
_computing_data_reduction        'CrysAlisPro 1.171.38.41 (Rigaku OD, 2015)'
_computing_molecular_graphics    'Mercury3.9 (2016)'
_computing_publication_material  'Olex2 (Dolomanov et al., 2009)'
_computing_structure_refinement  'ShelXL (Sheldrick, 2015)'
_computing_structure_solution    'ShelXT (Sheldrick, 2015)'
_refine_diff_density_max         0.474
_refine_diff_density_min         -0.479
_refine_diff_density_rms         0.093
_refine_ls_extinction_coef       .
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   0.991
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     489
_refine_ls_number_reflns         7671
_refine_ls_number_restraints     4
_refine_ls_R_factor_all          0.0957
_refine_ls_R_factor_gt           0.0523
_refine_ls_restrained_S_all      0.991
_refine_ls_shift/su_max          0.000
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details     
'w=1/[σ²(Fo²)+(0.0162P)²] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0817
_refine_ls_wR_factor_ref         0.0981
_refine_special_details          
;
 Structure of low spin state at 20K.  
 Four DFIX restrains and four EADP constrains have been applied for BF4-ion
at B2 atom site to model respectively geometry of B-F bonds 
and ADP's for diordered F-sites.
;
_atom_sites_solution_hydrogens   mixed
_atom_sites_solution_primary     dual
_atom_sites_solution_secondary   difmap
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 0.26985(2) 0.61192(4) 0.41858(3) 0.01208(12) Uani 1 1 d . . . . .
S1 S 0.59642(4) 0.70202(7) 0.49756(6) 0.01545(19) Uani 1 1 d . . . . .
S2 S -0.05082(4) 0.50353(7) 0.26253(6) 0.0176(2) Uani 1 1 d . . . . .
N2 N 0.34300(13) 0.7628(2) 0.54713(17) 0.0127(6) Uani 1 1 d . . . . .
N3 N 0.36723(13) 0.6342(2) 0.45181(17) 0.0119(6) Uani 1 1 d . . . . .
N9 N 0.18500(13) 0.4633(2) 0.48781(17) 0.0122(6) Uani 1 1 d . . . . .
N6 N 0.25001(13) 0.7221(2) 0.32131(17) 0.0132(6) Uani 1 1 d . . . . .
N4 N 0.37036(13) 0.5062(2) 0.34409(17) 0.0129(6) Uani 1 1 d . . . . .
N5 N 0.29958(14) 0.5031(2) 0.33743(17) 0.0136(6) Uani 1 1 d . . . . .
N10 N 0.25364(13) 0.4975(2) 0.50565(17) 0.0126(6) Uani 1 1 d . . . . .
N8 N 0.17301(13) 0.5904(2) 0.37616(16) 0.0114(6) Uani 1 1 d . . . . .
N1 N 0.27536(13) 0.7307(2) 0.50974(17) 0.0128(6) Uani 1 1 d . . . . .
N7 N 0.18132(13) 0.7225(2) 0.27466(17) 0.0122(6) Uani 1 1 d . . . . .
C28 C -0.14157(17) 0.5140(3) 0.1019(2) 0.0202(8) Uani 1 1 d . . . . .
H28A H -0.1227 0.4427 0.0886 0.030 Uiso 1 1 calc GR . . . .
H28B H -0.1613 0.5523 0.0447 0.030 Uiso 1 1 calc GR . . . .
H28C H -0.1779 0.5021 0.1358 0.030 Uiso 1 1 calc GR . . . .
C10 C 0.33008(17) 0.3805(3) 0.2416(2) 0.0158(7) Uani 1 1 d . . . . .
H10 H 0.3264 0.3246 0.1965 0.019 Uiso 1 1 calc R . . . .
C4 C 0.39559(17) 0.7119(3) 0.5117(2) 0.0134(7) Uani 1 1 d . . . . .
C26 C -0.08363(17) 0.5835(3) 0.1591(2) 0.0163(8) Uani 1 1 d . . . . .
H26 H -0.0457 0.5920 0.1254 0.020 Uiso 1 1 calc R . . . .
C11 C 0.27561(17) 0.4269(3) 0.2750(2) 0.0150(7) Uani 1 1 d . . . . .
H11 H 0.2281 0.4065 0.2557 0.018 Uiso 1 1 calc R . . . .
C18 C 0.13909(16) 0.5135(3) 0.4134(2) 0.0111(7) Uani 1 1 d . . . . .
C20 C 0.03466(16) 0.5462(3) 0.3038(2) 0.0145(7) Uani 1 1 d . . . . .
C22 C 0.13756(16) 0.6455(3) 0.3039(2) 0.0121(7) Uani 1 1 d . . . . .
C2 C 0.27678(16) 0.8748(3) 0.6034(2) 0.0142(7) Uani 1 1 d . . . . .
H2 H 0.2605 0.9321 0.6363 0.017 Uiso 1 1 calc R . . . .
C1 C 0.23645(17) 0.7986(3) 0.5443(2) 0.0139(7) Uani 1 1 d . . . . .
H1 H 0.1871 0.7963 0.5309 0.017 Uiso 1 1 calc R . . . .
C19 C 0.07107(16) 0.4872(3) 0.3803(2) 0.0128(7) Uani 1 1 d . . . . .
H19 H 0.0490 0.4312 0.4077 0.015 Uiso 1 1 calc R . . . .
C6 C 0.50734(16) 0.6823(3) 0.4835(2) 0.0129(7) Uani 1 1 d . . . . .
C13 C 0.58539(17) 0.9285(3) 0.5011(2) 0.0169(8) Uani 1 1 d . . . . .
H13A H 0.6051 0.9313 0.4469 0.025 Uiso 1 1 calc GR . . . .
H13B H 0.5966 0.9969 0.5359 0.025 Uiso 1 1 calc GR . . . .
H13C H 0.5348 0.9202 0.4824 0.025 Uiso 1 1 calc GR . . . .
C15 C 0.28437(17) 0.4427(3) 0.5794(2) 0.0146(7) Uani 1 1 d . . . . .
H15 H 0.3322 0.4489 0.6081 0.017 Uiso 1 1 calc R . . . .
C3 C 0.34456(17) 0.8497(3) 0.6042(2) 0.0152(7) Uani 1 1 d . . . . .
H3 H 0.3848 0.8861 0.6380 0.018 Uiso 1 1 calc R . . . .
C12 C 0.61605(16) 0.8310(3) 0.5602(2) 0.0149(7) Uani 1 1 d . . . . .
H12 H 0.5966 0.8288 0.6160 0.018 Uiso 1 1 calc R . . . .
C21 C 0.06836(16) 0.6282(3) 0.2654(2) 0.0123(7) Uani 1 1 d . . . . .
H21 H 0.0446 0.6704 0.2147 0.015 Uiso 1 1 calc R . . . .
C14 C 0.69525(16) 0.8375(3) 0.5879(2) 0.0180(8) Uani 1 1 d . . . . .
H14A H 0.7132 0.7745 0.6268 0.027 Uiso 1 1 calc GR . . . .
H14B H 0.7090 0.9061 0.6214 0.027 Uiso 1 1 calc GR . . . .
H14C H 0.7143 0.8361 0.5332 0.027 Uiso 1 1 calc GR . . . .
C9 C 0.38948(17) 0.4318(3) 0.2867(2) 0.0149(7) Uani 1 1 d . . . . .
H9 H 0.4353 0.4182 0.2794 0.018 Uiso 1 1 calc R . . . .
C16 C 0.23696(17) 0.3738(3) 0.6099(2) 0.0155(7) Uani 1 1 d . . . . .
H16 H 0.2466 0.3264 0.6614 0.019 Uiso 1 1 calc R . . . .
C17 C 0.17431(17) 0.3889(3) 0.5505(2) 0.0144(7) Uani 1 1 d . . . . .
H17 H 0.1316 0.3540 0.5527 0.017 Uiso 1 1 calc R . . . .
C27 C -0.10761(18) 0.6972(3) 0.1812(2) 0.0217(8) Uani 1 1 d . . . . .
H27A H -0.1446 0.6898 0.2146 0.033 Uiso 1 1 calc GR . . . .
H27B H -0.1253 0.7379 0.1244 0.033 Uiso 1 1 calc GR . . . .
H27C H -0.0684 0.7374 0.2187 0.033 Uiso 1 1 calc GR . . . .
C24 C 0.23009(17) 0.8603(3) 0.2203(2) 0.0167(8) Uani 1 1 d . . . . .
H24 H 0.2380 0.9230 0.1861 0.020 Uiso 1 1 calc R . . . .
C25 C 0.27871(17) 0.8068(3) 0.2873(2) 0.0146(7) Uani 1 1 d . . . . .
H25 H 0.3261 0.8278 0.3064 0.018 Uiso 1 1 calc R . . . .
C7 C 0.47822(16) 0.6013(3) 0.4200(2) 0.0137(7) Uani 1 1 d . . . . .
H7 H 0.5061 0.5622 0.3868 0.016 Uiso 1 1 calc R . . . .
C8 C 0.40891(17) 0.5799(3) 0.4070(2) 0.0132(7) Uani 1 1 d . . . . .
C23 C 0.16885(17) 0.8055(3) 0.2130(2) 0.0149(7) Uani 1 1 d . . . . .
H23 H 0.1258 0.8223 0.1725 0.018 Uiso 1 1 calc R . . . .
C5 C 0.46486(16) 0.7392(3) 0.5317(2) 0.0142(7) Uani 1 1 d . . . . .
H5 H 0.4832 0.7937 0.5759 0.017 Uiso 1 1 calc R . . . .
F7 F -0.03703(10) 0.75665(17) 0.43113(13) 0.0232(5) Uani 0.9599(19) 1 d . . P A
2
F8 F 0.08016(10) 0.72843(18) 0.47020(14) 0.0237(5) Uani 0.9599(19) 1 d . . P A
2
F6 F 0.01565(10) 0.71775(17) 0.57788(12) 0.0210(5) Uani 0.9599(19) 1 d . . P A
2
F5 F 0.03448(11) 0.88335(17) 0.51784(14) 0.0238(5) Uani 0.9599(19) 1 d . . P A
2
B2 B 0.0239(2) 0.7704(3) 0.4990(3) 0.0170(9) Uani 1 1 d D . . . .
F4 F 0.43937(9) 0.56192(15) 0.68596(11) 0.0173(4) Uani 1 1 d . . . . .
F3 F 0.37208(9) 0.47893(16) 0.77099(12) 0.0177(4) Uani 1 1 d . . . . .
F2 F 0.48990(9) 0.45516(15) 0.80769(11) 0.0175(4) Uani 1 1 d . . . . .
F1 F 0.44239(9) 0.62246(15) 0.83062(11) 0.0189(4) Uani 1 1 d . . . . .
B1 B 0.4358(2) 0.5301(3) 0.7747(3) 0.0150(8) Uani 1 1 d . . . . .
O1W O 0.12456(13) 0.4462(2) 0.12980(17) 0.0284(6) Uani 1 1 d . . . . .
H1WA H 0.0995 0.3887 0.1185 0.043 Uiso 1 1 d G . . . .
H1WB H 0.1037 0.5001 0.0995 0.043 Uiso 1 1 d G . . . .
F5A F 0.065(2) 0.827(4) 0.573(2) 0.0238(5) Uani 0.0401(19) 1 d D . P A 1
F7A F -0.0417(12) 0.738(4) 0.508(3) 0.0232(5) Uani 0.0401(19) 1 d D . P A 1
F8A F 0.055(3) 0.771(5) 0.424(2) 0.0237(5) Uani 0.0401(19) 1 d D . P A 1
F6A F 0.055(2) 0.672(2) 0.539(3) 0.0210(5) Uani 0.0401(19) 1 d D . P A 1


_geom_special_details            
;
 All esds (except the esd in the dihedral angle between two l.s. planes)
 are estimated using the full covariance matrix.  The cell esds are taken
 into account individually in the estimation of esds in distances, angles
 and torsion angles; correlations between esds in cell parameters are only
 used when they are defined by crystal symmetry.  An approximate (isotropic)
 treatment of cell esds is used for estimating esds involving l.s. planes.
;
loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
_geom_bond_publ_flag
Fe1 N3 1.894(3) . ?
Fe1 N6 1.957(3) . ?
Fe1 N5 1.975(3) . ?
Fe1 N10 1.984(3) . ?
Fe1 N8 1.893(3) . ?
Fe1 N1 1.976(3) . ?
S1 C6 1.740(3) . ?
S1 C12 1.823(3) . ?
S2 C26 1.826(3) . ?
S2 C20 1.741(3) . ?
N2 N1 1.384(3) . ?
N2 C4 1.412(4) . ?
N2 C3 1.356(4) . ?
N3 C4 1.338(4) . ?
N3 C8 1.347(4) . ?
N9 N10 1.385(3) . ?
N9 C18 1.411(4) . ?
N9 C17 1.357(4) . ?
N6 N7 1.380(3) . ?
N6 C25 1.330(4) . ?
N4 N5 1.379(3) . ?
N4 C9 1.360(4) . ?
N4 C8 1.397(4) . ?
N5 C11 1.327(4) . ?
N10 C15 1.320(4) . ?
N8 C18 1.343(4) . ?
N8 C22 1.333(4) . ?
N1 C1 1.311(4) . ?
N7 C22 1.409(4) . ?
N7 C23 1.354(4) . ?
C28 H28A 0.9800 . ?
C28 H28B 0.9800 . ?
C28 H28C 0.9800 . ?
C28 C26 1.523(4) . ?
C10 H10 0.9500 . ?
C10 C11 1.404(4) . ?
C10 C9 1.366(4) . ?
C4 C5 1.373(4) . ?
C26 H26 1.0000 . ?
C26 C27 1.520(4) . ?
C11 H11 0.9500 . ?
C18 C19 1.361(4) . ?
C20 C19 1.408(4) . ?
C20 C21 1.394(4) . ?
C22 C21 1.375(4) . ?
C2 H2 0.9500 . ?
C2 C1 1.402(4) . ?
C2 C3 1.370(4) . ?
C1 H1 0.9500 . ?
C19 H19 0.9500 . ?
C6 C7 1.401(4) . ?
C6 C5 1.408(4) . ?
C13 H13A 0.9800 . ?
C13 H13B 0.9800 . ?
C13 H13C 0.9800 . ?
C13 C12 1.522(4) . ?
C15 H15 0.9500 . ?
C15 C16 1.407(4) . ?
C3 H3 0.9500 . ?
C12 H12 1.0000 . ?
C12 C14 1.527(4) . ?
C21 H21 0.9500 . ?
C14 H14A 0.9800 . ?
C14 H14B 0.9800 . ?
C14 H14C 0.9800 . ?
C9 H9 0.9500 . ?
C16 H16 0.9500 . ?
C16 C17 1.366(4) . ?
C17 H17 0.9500 . ?
C27 H27A 0.9800 . ?
C27 H27B 0.9800 . ?
C27 H27C 0.9800 . ?
C24 H24 0.9500 . ?
C24 C25 1.388(4) . ?
C24 C23 1.363(4) . ?
C25 H25 0.9500 . ?
C7 H7 0.9500 . ?
C7 C8 1.363(4) . ?
C23 H23 0.9500 . ?
C5 H5 0.9500 . ?
F7 B2 1.402(4) . ?
F8 B2 1.377(4) . ?
F6 B2 1.391(4) . ?
F5 B2 1.406(4) . ?
B2 F5A 1.400(10) . ?
B2 F7A 1.392(10) . ?
B2 F8A 1.402(10) . ?
B2 F6A 1.412(10) . ?
F4 B1 1.408(4) . ?
F3 B1 1.392(4) . ?
F2 B1 1.406(4) . ?
F1 B1 1.390(4) . ?
O1W H1WA 0.8502 . ?
O1W H1WB 0.8495 . ?

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 N6 96.93(11) . . ?
N3 Fe1 N5 80.41(11) . . ?
N3 Fe1 N10 103.31(11) . . ?
N3 Fe1 N1 79.55(11) . . ?
N6 Fe1 N5 91.79(11) . . ?
N6 Fe1 N10 159.68(11) . . ?
N6 Fe1 N1 89.52(11) . . ?
N5 Fe1 N10 93.19(10) . . ?
N5 Fe1 N1 159.93(11) . . ?
N8 Fe1 N3 175.72(11) . . ?
N8 Fe1 N6 79.92(11) . . ?
N8 Fe1 N5 96.73(11) . . ?
N8 Fe1 N10 79.94(11) . . ?
N8 Fe1 N1 103.22(11) . . ?
N1 Fe1 N10 92.47(10) . . ?
C6 S1 C12 105.82(15) . . ?
C20 S2 C26 106.00(15) . . ?
N1 N2 C4 116.6(3) . . ?
C3 N2 N1 111.1(2) . . ?
C3 N2 C4 131.7(3) . . ?
C4 N3 Fe1 121.6(2) . . ?
C4 N3 C8 118.2(3) . . ?
C8 N3 Fe1 119.7(2) . . ?
N10 N9 C18 116.8(2) . . ?
C17 N9 N10 111.3(3) . . ?
C17 N9 C18 131.8(3) . . ?
N7 N6 Fe1 113.04(19) . . ?
C25 N6 Fe1 141.7(2) . . ?
C25 N6 N7 104.9(3) . . ?
N5 N4 C8 117.1(2) . . ?
C9 N4 N5 110.9(3) . . ?
C9 N4 C8 132.0(3) . . ?
N4 N5 Fe1 112.0(2) . . ?
C11 N5 Fe1 142.7(2) . . ?
C11 N5 N4 105.3(2) . . ?
N9 N10 Fe1 112.23(19) . . ?
C15 N10 Fe1 142.8(2) . . ?
C15 N10 N9 104.8(2) . . ?
C18 N8 Fe1 121.1(2) . . ?
C22 N8 Fe1 120.7(2) . . ?
C22 N8 C18 118.0(3) . . ?
N2 N1 Fe1 112.66(18) . . ?
C1 N1 Fe1 142.0(2) . . ?
C1 N1 N2 105.0(3) . . ?
N6 N7 C22 116.1(3) . . ?
C23 N7 N6 110.9(3) . . ?
C23 N7 C22 132.7(3) . . ?
H28A C28 H28B 109.5 . . ?
H28A C28 H28C 109.5 . . ?
H28B C28 H28C 109.5 . . ?
C26 C28 H28A 109.5 . . ?
C26 C28 H28B 109.5 . . ?
C26 C28 H28C 109.5 . . ?
C11 C10 H10 126.9 . . ?
C9 C10 H10 126.9 . . ?
C9 C10 C11 106.2(3) . . ?
N3 C4 N2 109.4(3) . . ?
N3 C4 C5 124.3(3) . . ?
C5 C4 N2 126.3(3) . . ?
S2 C26 H26 108.9 . . ?
C28 C26 S2 105.3(2) . . ?
C28 C26 H26 108.9 . . ?
C27 C26 S2 111.4(2) . . ?
C27 C26 C28 113.3(3) . . ?
C27 C26 H26 108.9 . . ?
N5 C11 C10 110.7(3) . . ?
N5 C11 H11 124.6 . . ?
C10 C11 H11 124.6 . . ?
N8 C18 N9 109.9(3) . . ?
N8 C18 C19 123.6(3) . . ?
C19 C18 N9 126.5(3) . . ?
C19 C20 S2 114.6(2) . . ?
C21 C20 S2 125.4(3) . . ?
C21 C20 C19 120.0(3) . . ?
N8 C22 N7 110.0(3) . . ?
N8 C22 C21 123.9(3) . . ?
C21 C22 N7 126.1(3) . . ?
C1 C2 H2 127.1 . . ?
C3 C2 H2 127.1 . . ?
C3 C2 C1 105.8(3) . . ?
N1 C1 C2 111.5(3) . . ?
N1 C1 H1 124.2 . . ?
C2 C1 H1 124.2 . . ?
C18 C19 C20 117.4(3) . . ?
C18 C19 H19 121.3 . . ?
C20 C19 H19 121.3 . . ?
C7 C6 S1 115.3(2) . . ?
C7 C6 C5 119.7(3) . . ?
C5 C6 S1 125.0(3) . . ?
H13A C13 H13B 109.5 . . ?
H13A C13 H13C 109.5 . . ?
H13B C13 H13C 109.5 . . ?
C12 C13 H13A 109.5 . . ?
C12 C13 H13B 109.5 . . ?
C12 C13 H13C 109.5 . . ?
N10 C15 H15 124.4 . . ?
N10 C15 C16 111.1(3) . . ?
C16 C15 H15 124.4 . . ?
N2 C3 C2 106.6(3) . . ?
N2 C3 H3 126.7 . . ?
C2 C3 H3 126.7 . . ?
S1 C12 H12 109.6 . . ?
C13 C12 S1 110.8(2) . . ?
C13 C12 H12 109.6 . . ?
C13 C12 C14 111.6(3) . . ?
C14 C12 S1 105.7(2) . . ?
C14 C12 H12 109.6 . . ?
C20 C21 H21 121.5 . . ?
C22 C21 C20 117.1(3) . . ?
C22 C21 H21 121.5 . . ?
C12 C14 H14A 109.5 . . ?
C12 C14 H14B 109.5 . . ?
C12 C14 H14C 109.5 . . ?
H14A C14 H14B 109.5 . . ?
H14A C14 H14C 109.5 . . ?
H14B C14 H14C 109.5 . . ?
N4 C9 C10 106.8(3) . . ?
N4 C9 H9 126.6 . . ?
C10 C9 H9 126.6 . . ?
C15 C16 H16 126.9 . . ?
C17 C16 C15 106.2(3) . . ?
C17 C16 H16 126.9 . . ?
N9 C17 C16 106.5(3) . . ?
N9 C17 H17 126.7 . . ?
C16 C17 H17 126.7 . . ?
C26 C27 H27A 109.5 . . ?
C26 C27 H27B 109.5 . . ?
C26 C27 H27C 109.5 . . ?
H27A C27 H27B 109.5 . . ?
H27A C27 H27C 109.5 . . ?
H27B C27 H27C 109.5 . . ?
C25 C24 H24 126.7 . . ?
C23 C24 H24 126.7 . . ?
C23 C24 C25 106.6(3) . . ?
N6 C25 C24 110.9(3) . . ?
N6 C25 H25 124.6 . . ?
C24 C25 H25 124.6 . . ?
C6 C7 H7 120.8 . . ?
C8 C7 C6 118.4(3) . . ?
C8 C7 H7 120.8 . . ?
N3 C8 N4 110.6(3) . . ?
N3 C8 C7 122.8(3) . . ?
C7 C8 N4 126.5(3) . . ?
N7 C23 C24 106.7(3) . . ?
N7 C23 H23 126.7 . . ?
C24 C23 H23 126.7 . . ?
C4 C5 C6 116.6(3) . . ?
C4 C5 H5 121.7 . . ?
C6 C5 H5 121.7 . . ?
F7 B2 F5 109.1(3) . . ?
F8 B2 F7 110.4(3) . . ?
F8 B2 F6 110.9(3) . . ?
F8 B2 F5 109.3(3) . . ?
F6 B2 F7 108.7(3) . . ?
F6 B2 F5 108.4(3) . . ?
F5A B2 F8A 111(3) . . ?
F5A B2 F6A 87(3) . . ?
F7A B2 F5A 117(3) . . ?
F7A B2 F8A 132(3) . . ?
F7A B2 F6A 92(3) . . ?
F8A B2 F6A 97(3) . . ?
F3 B1 F4 108.8(3) . . ?
F3 B1 F2 109.5(3) . . ?
F2 B1 F4 108.4(3) . . ?
F1 B1 F4 109.6(3) . . ?
F1 B1 F3 110.2(3) . . ?
F1 B1 F2 110.3(3) . . ?
H1WA O1W H1WB 109.5 . . ?

loop_
_geom_torsion_atom_site_label_1
_geom_torsion_atom_site_label_2
_geom_torsion_atom_site_label_3
_geom_torsion_atom_site_label_4
_geom_torsion
_geom_torsion_site_symmetry_1
_geom_torsion_site_symmetry_2
_geom_torsion_site_symmetry_3
_geom_torsion_site_symmetry_4
_geom_torsion_publ_flag
Fe1 N3 C4 N2 4.4(3) . . . . ?
Fe1 N3 C4 C5 -173.3(2) . . . . ?
Fe1 N3 C8 N4 -4.4(3) . . . . ?
Fe1 N3 C8 C7 172.2(2) . . . . ?
Fe1 N6 N7 C22 0.1(3) . . . . ?
Fe1 N6 N7 C23 175.19(19) . . . . ?
Fe1 N6 C25 C24 -172.4(3) . . . . ?
Fe1 N5 C11 C10 178.1(3) . . . . ?
Fe1 N10 C15 C16 176.0(3) . . . . ?
Fe1 N8 C18 N9 4.2(3) . . . . ?
Fe1 N8 C18 C19 -173.6(2) . . . . ?
Fe1 N8 C22 N7 -5.2(3) . . . . ?
Fe1 N8 C22 C21 175.1(2) . . . . ?
Fe1 N1 C1 C2 -172.8(3) . . . . ?
S1 C6 C7 C8 178.6(2) . . . . ?
S1 C6 C5 C4 -179.7(2) . . . . ?
S2 C20 C19 C18 177.2(2) . . . . ?
S2 C20 C21 C22 -175.7(2) . . . . ?
N2 N1 C1 C2 0.1(3) . . . . ?
N2 C4 C5 C6 -175.8(3) . . . . ?
N3 C4 C5 C6 1.6(5) . . . . ?
N9 N10 C15 C16 -0.2(3) . . . . ?
N9 C18 C19 C20 -178.7(3) . . . . ?
N6 Fe1 N3 C4 86.0(2) . . . . ?
N6 Fe1 N3 C8 -86.1(2) . . . . ?
N6 Fe1 N8 C18 179.2(2) . . . . ?
N6 Fe1 N8 C22 4.3(2) . . . . ?
N6 N7 C22 N8 3.0(4) . . . . ?
N6 N7 C22 C21 -177.2(3) . . . . ?
N6 N7 C23 C24 -0.5(3) . . . . ?
N4 N5 C11 C10 0.2(3) . . . . ?
N5 Fe1 N3 C4 176.7(2) . . . . ?
N5 Fe1 N3 C8 4.5(2) . . . . ?
N5 Fe1 N8 C18 88.6(2) . . . . ?
N5 Fe1 N8 C22 -86.3(2) . . . . ?
N5 N4 C9 C10 0.6(4) . . . . ?
N5 N4 C8 N3 1.2(4) . . . . ?
N5 N4 C8 C7 -175.2(3) . . . . ?
N10 Fe1 N3 C4 -92.3(2) . . . . ?
N10 Fe1 N3 C8 95.5(2) . . . . ?
N10 Fe1 N8 C18 -3.5(2) . . . . ?
N10 Fe1 N8 C22 -178.4(2) . . . . ?
N10 N9 C18 N8 -2.4(4) . . . . ?
N10 N9 C18 C19 175.3(3) . . . . ?
N10 N9 C17 C16 -0.3(3) . . . . ?
N10 C15 C16 C17 0.0(4) . . . . ?
N8 C18 C19 C20 -1.3(5) . . . . ?
N8 C22 C21 C20 -1.5(5) . . . . ?
N1 Fe1 N3 C4 -2.2(2) . . . . ?
N1 Fe1 N3 C8 -174.4(2) . . . . ?
N1 Fe1 N8 C18 -93.7(2) . . . . ?
N1 Fe1 N8 C22 91.4(2) . . . . ?
N1 N2 C4 N3 -4.9(4) . . . . ?
N1 N2 C4 C5 172.8(3) . . . . ?
N1 N2 C3 C2 -0.3(3) . . . . ?
N7 N6 C25 C24 -0.2(3) . . . . ?
N7 C22 C21 C20 178.8(3) . . . . ?
C4 N2 N1 Fe1 3.5(3) . . . . ?
C4 N2 N1 C1 -171.8(3) . . . . ?
C4 N2 C3 C2 170.0(3) . . . . ?
C4 N3 C8 N4 -176.8(3) . . . . ?
C4 N3 C8 C7 -0.3(5) . . . . ?
C26 S2 C20 C19 -175.2(2) . . . . ?
C26 S2 C20 C21 2.2(3) . . . . ?
C11 C10 C9 N4 -0.4(4) . . . . ?
C18 N9 N10 Fe1 -0.1(3) . . . . ?
C18 N9 N10 C15 177.4(3) . . . . ?
C18 N9 C17 C16 -176.8(3) . . . . ?
C18 N8 C22 N7 179.8(2) . . . . ?
C18 N8 C22 C21 0.0(5) . . . . ?
C20 S2 C26 C28 154.7(2) . . . . ?
C20 S2 C26 C27 -82.1(3) . . . . ?
C22 N8 C18 N9 179.3(3) . . . . ?
C22 N8 C18 C19 1.4(5) . . . . ?
C22 N7 C23 C24 173.5(3) . . . . ?
C1 C2 C3 N2 0.4(3) . . . . ?
C19 C20 C21 C22 1.6(4) . . . . ?
C6 S1 C12 C13 -69.2(2) . . . . ?
C6 S1 C12 C14 169.7(2) . . . . ?
C6 C7 C8 N3 0.9(5) . . . . ?
C6 C7 C8 N4 176.8(3) . . . . ?
C15 C16 C17 N9 0.2(4) . . . . ?
C3 N2 N1 Fe1 175.43(19) . . . . ?
C3 N2 N1 C1 0.1(3) . . . . ?
C3 N2 C4 N3 -174.9(3) . . . . ?
C3 N2 C4 C5 2.8(5) . . . . ?
C3 C2 C1 N1 -0.3(4) . . . . ?
C12 S1 C6 C7 166.4(2) . . . . ?
C12 S1 C6 C5 -14.9(3) . . . . ?
C21 C20 C19 C18 -0.3(5) . . . . ?
C9 N4 N5 Fe1 -179.1(2) . . . . ?
C9 N4 N5 C11 -0.5(3) . . . . ?
C9 N4 C8 N3 -177.2(3) . . . . ?
C9 N4 C8 C7 6.4(5) . . . . ?
C9 C10 C11 N5 0.2(4) . . . . ?
C17 N9 N10 Fe1 -177.19(19) . . . . ?
C17 N9 N10 C15 0.3(3) . . . . ?
C17 N9 C18 N8 173.9(3) . . . . ?
C17 N9 C18 C19 -8.3(5) . . . . ?
C25 N6 N7 C22 -174.6(2) . . . . ?
C25 N6 N7 C23 0.5(3) . . . . ?
C25 C24 C23 N7 0.4(3) . . . . ?
C7 C6 C5 C4 -1.0(4) . . . . ?
C8 N3 C4 N2 176.7(3) . . . . ?
C8 N3 C4 C5 -1.0(5) . . . . ?
C8 N4 N5 Fe1 2.2(3) . . . . ?
C8 N4 N5 C11 -179.1(3) . . . . ?
C8 N4 C9 C10 179.0(3) . . . . ?
C23 N7 C22 N8 -170.7(3) . . . . ?
C23 N7 C22 C21 9.0(5) . . . . ?
C23 C24 C25 N6 -0.1(4) . . . . ?
C5 C6 C7 C8 -0.2(5) . . . . ?


####################################################################### 
# 
# This file contains crystal structure data downloaded from the 
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# Crystallographic Data Centre (CCDC).
# 
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# guidelines are available at http://www.ccdc.cam.ac.uk/access/V1 
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# 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_rk137MeNO2_015K
_database_code_depnum_ccdc_archive 'CCDC 1564671'
_audit_update_record             
;
2017-07-28 deposited with the CCDC.
2017-11-20 downloaded from the CCDC.
;
_chemical_name_common            ?
_chemical_name_systematic        ?
_chemical_formula_moiety         'C28 H30 Fe N10 S2, 2(B F4), C H3 N O2'
_chemical_formula_sum            'C29 H33 B2 F8 Fe N11 O2 S2'
_chemical_formula_weight         861.25
_chemical_melting_point          'not measured'
loop_
_atom_type_symbol
_atom_type_description
_atom_type_scat_dispersion_real
_atom_type_scat_dispersion_imag
_atom_type_scat_source
C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
B B 0.0013 0.0007 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
F F 0.0171 0.0103 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Fe Fe 0.3463 0.8444 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
S S 0.1246 0.1234 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'

_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.
;
_space_group_crystal_system      monoclinic
_space_group_IT_number           14
_space_group_name_H-M_alt        'P 1 21/c 1'
_space_group_name_Hall           '-P 2ybc'
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                   19.7255(5)
_cell_length_b                   35.2106(8)
_cell_length_c                   16.0710(4)
_cell_angle_alpha                90
_cell_angle_beta                 100.706(2)
_cell_angle_gamma                90
_cell_volume                     10967.8(5)
_cell_special_details            
;
In comparison to 100K data, new satellite reflections along b-axis appear at 15K. 
Although the symmetry remains valid, the tripling of the b-cell parameter has been
applied for final processing of 15K data.
;
_cell_formula_units_Z            12
_cell_measurement_reflns_used    8965
_cell_measurement_temperature    15
_cell_measurement_theta_max      32.4840
_cell_measurement_theta_min      3.6050
_exptl_absorpt_coefficient_mu    0.614
_exptl_absorpt_correction_T_max  0.978
_exptl_absorpt_correction_T_min  0.957
_exptl_absorpt_correction_type   analytical
_exptl_absorpt_process_details   
;
CrysAlisPro 1.171.38.41 (Rigaku Oxford Diffraction, 2015)
Analytical numeric absorption correction using a multifaceted crystal
			model based on expressions derived by R.C. Clark & J.S. Reid.
(Clark, R. C. & Reid, J. S. (1995). Acta Cryst. A51, 887-897)
Empirical absorption correction using spherical harmonics,
 implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_absorpt_special_details   ?
_exptl_crystal_colour            'dark orange'
_exptl_crystal_density_diffrn    1.565
_exptl_crystal_density_meas      'not measured'
_exptl_crystal_density_method    none
_exptl_crystal_description       block
_exptl_crystal_F_000             5280
loop_
_exptl_crystal_face_index_h
_exptl_crystal_face_index_k
_exptl_crystal_face_index_l
_exptl_crystal_face_perp_dist
-1 44 -12 0.1127
-1 -44 12 0.0147
22 -10 -2 0.0421
-21 14 1 0.2197
-4 -26 -22 0.0451
2 24 23 0.1139
-13 6 25 0.1857

_exptl_crystal_size_max          0.329
_exptl_crystal_size_mid          0.169
_exptl_crystal_size_min          0.132
loop_
_exptl_oxdiff_crystal_face_indexfrac_h
_exptl_oxdiff_crystal_face_indexfrac_k
_exptl_oxdiff_crystal_face_indexfrac_l
_exptl_oxdiff_crystal_face_x
_exptl_oxdiff_crystal_face_y
_exptl_oxdiff_crystal_face_z
-1.0427 43.8927 -11.9630 0.3951 0.8300 0.3712
-0.9573 -43.8975 11.9627 -0.3636 -0.7967 -0.4485
22.0084 -9.9276 -2.0001 -0.2626 -0.5536 0.7877
-21.0122 13.9206 1.0036 0.2781 0.6109 -0.7124
-3.9839 -25.9721 -21.9928 0.8853 -0.4257 -0.2051
1.9860 23.9725 22.9903 -0.8874 0.4222 0.1062
-12.9975 5.9772 24.9757 -0.7017 0.3384 -0.6216

_exptl_transmission_factor_max   ?
_exptl_transmission_factor_min   ?
_diffrn_reflns_av_R_equivalents  0.0594
_diffrn_reflns_av_unetI/netI     0.0957
_diffrn_reflns_Laue_measured_fraction_full 0.998
_diffrn_reflns_Laue_measured_fraction_max 0.998
_diffrn_reflns_limit_h_max       25
_diffrn_reflns_limit_h_min       -24
_diffrn_reflns_limit_k_max       44
_diffrn_reflns_limit_k_min       -38
_diffrn_reflns_limit_l_max       20
_diffrn_reflns_limit_l_min       -20
_diffrn_reflns_number            53607
_diffrn_reflns_point_group_measured_fraction_full 0.998
_diffrn_reflns_point_group_measured_fraction_max 0.998
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         27.000
_diffrn_reflns_theta_min         2.961
_diffrn_ambient_temperature      15
_diffrn_detector                 'CCD plate'
_diffrn_detector_area_resol_mean 16.1852
_diffrn_detector_type            Sapphire3
_diffrn_measured_fraction_theta_full 0.998
_diffrn_measured_fraction_theta_max 0.998
_diffrn_measurement_details      
;
List of Runs (angles in degrees, time in seconds):

  # Type    Start    End  Width  tₑₓₚ   ω     θ     κ     φ   Frames
#--------------------------------------------------------------------------
  1  ω     56.00 103.00   1.00    7.50    --   32.27  57.00 -30.00   47
  2  ω    -16.00  64.00   1.00    7.50    --   32.27  19.00 150.00   80
  3  ω    -94.00 -16.00   1.00    7.50    --  -30.39 -57.00-180.00   78
  4  ω   -107.00 -35.00   1.00    7.50    --  -30.39-178.00-180.00   72
;
_diffrn_measurement_device       'four-circle diffractometer'
_diffrn_measurement_device_type  'Xcalibur, Sapphire3'
_diffrn_measurement_method       'ω scans'
_diffrn_orient_matrix_type       
'CrysAlisPro convention (1999,Acta A55,543-557)'
_diffrn_orient_matrix_UB_11      -0.0157407000
_diffrn_orient_matrix_UB_12      -0.0011855000
_diffrn_orient_matrix_UB_13      -0.0360036000
_diffrn_orient_matrix_UB_21      -0.0167180000
_diffrn_orient_matrix_UB_22      0.0186206000
_diffrn_orient_matrix_UB_23      0.0003934000
_diffrn_orient_matrix_UB_31      0.0386048000
_diffrn_orient_matrix_UB_32      0.0075727000
_diffrn_orient_matrix_UB_33      -0.0066101000
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_source                   'fine-focus sealed X-ray tube'
_diffrn_source_type              'Enhance (Mo) X-ray Source'
_reflns_Friedel_coverage         0.000
_reflns_Friedel_fraction_full    .
_reflns_Friedel_fraction_max     .
_reflns_number_gt                15924
_reflns_number_total             23910
_reflns_odcompleteness_completeness 99.78
_reflns_odcompleteness_iscentric 1
_reflns_odcompleteness_theta     26.32
_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.
;
_reflns_threshold_expression     'I > 2σ(I)'
_computing_cell_refinement       'CrysAlisPro 1.171.38.41 (Rigaku OD, 2015)'
_computing_data_collection       'CrysAlisPro 1.171.37.31c (Rigaku OD, 2014)'
_computing_data_reduction        'CrysAlisPro 1.171.38.41 (Rigaku OD, 2015)'
_computing_molecular_graphics    'Mercury3.9 (2016)'
_computing_publication_material  'Olex2 (Dolomanov et al., 2009)'
_computing_structure_refinement  'ShelXL (Sheldrick, 2015)'
_computing_structure_solution    'ShelXT (Sheldrick, 2015)'
_refine_diff_density_max         0.845
_refine_diff_density_min         -0.623
_refine_diff_density_rms         0.098
_refine_ls_extinction_coef       .
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.017
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     1501
_refine_ls_number_reflns         23910
_refine_ls_number_restraints     0
_refine_ls_R_factor_all          0.0974
_refine_ls_R_factor_gt           0.0566
_refine_ls_restrained_S_all      1.017
_refine_ls_shift/su_max          0.001
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details     
'w=1/[σ²(Fo²)+(0.0363P)²+1.4286P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1060
_refine_ls_wR_factor_ref         0.1243
_refine_special_details          
;
Structure of lower symmetry low spin state at 15K.
Five reflections have been treated with OMIT ShelXL instruction.
;
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     dual
_atom_sites_solution_secondary   difmap
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 0.22117(2) 0.20670(2) 0.55142(3) 0.00766(11) Uani 1 1 d . . . . .
S1 S -0.10254(4) 0.23927(2) 0.49801(5) 0.01074(18) Uani 1 1 d . . . . .
S2 S 0.54141(4) 0.17806(3) 0.69860(6) 0.0184(2) Uani 1 1 d . . . . .
N7 N 0.31099(12) 0.15479(7) 0.49351(16) 0.0084(6) Uani 1 1 d . . . . .
N5 N 0.21379(12) 0.24432(7) 0.45806(16) 0.0089(6) Uani 1 1 d . . . . .
N3 N 0.12371(13) 0.21327(7) 0.52410(16) 0.0076(6) Uani 1 1 d . . . . .
N9 N 0.30368(13) 0.24902(7) 0.67950(16) 0.0096(6) Uani 1 1 d . . . . .
N4 N 0.14628(12) 0.25403(7) 0.42526(16) 0.0084(6) Uani 1 1 d . . . . .
N8 N 0.31776(13) 0.20116(7) 0.59133(16) 0.0088(6) Uani 1 1 d . . . . .
N2 N 0.12203(12) 0.17194(7) 0.63147(16) 0.0080(6) Uani 1 1 d . . . . .
N6 N 0.24269(12) 0.16640(7) 0.47464(16) 0.0080(6) Uani 1 1 d . . . . .
N1 N 0.19205(12) 0.17001(7) 0.63110(16) 0.0083(6) Uani 1 1 d . . . . .
N10 N 0.23637(13) 0.24696(7) 0.63727(16) 0.0097(6) Uani 1 1 d . . . . .
C5 C 0.01487(15) 0.20509(9) 0.56615(19) 0.0082(7) Uani 1 1 d . . . . .
H5 H -0.0120 0.1934 0.6022 0.010 Uiso 1 1 calc R . . . .
C10 C 0.20880(16) 0.28459(9) 0.3480(2) 0.0130(7) Uani 1 1 d . . . . .
H10 H 0.2233 0.3003 0.3066 0.016 Uiso 1 1 calc R . . . .
C9 C 0.14271(16) 0.27830(9) 0.3584(2) 0.0103(7) Uani 1 1 d . . . . .
H9 H 0.1020 0.2888 0.3254 0.012 Uiso 1 1 calc R . . . .
C23 C 0.31287(17) 0.27883(9) 0.7343(2) 0.0115(7) Uani 1 1 d . . . . .
H23 H 0.3547 0.2861 0.7703 0.014 Uiso 1 1 calc R . . . .
C19 C 0.42182(16) 0.16678(9) 0.5911(2) 0.0105(7) Uani 1 1 d . . . . .
H19 H 0.4460 0.1474 0.5675 0.013 Uiso 1 1 calc R . . . .
C28 C 0.61540(18) 0.17452(11) 0.8579(2) 0.0232(9) Uani 1 1 d . . . . .
H28A H 0.5966 0.1489 0.8607 0.035 Uiso 1 1 calc GR . . . .
H28B H 0.6273 0.1851 0.9151 0.035 Uiso 1 1 calc GR . . . .
H28C H 0.6569 0.1734 0.8325 0.035 Uiso 1 1 calc GR . . . .
C2 C 0.16141(16) 0.12631(9) 0.7201(2) 0.0128(7) Uani 1 1 d . . . . .
H2 H 0.1650 0.1062 0.7602 0.015 Uiso 1 1 calc R . . . .
C8 C 0.09555(15) 0.23851(9) 0.4659(2) 0.0094(7) Uani 1 1 d . . . . .
C14 C -0.08623(17) 0.31668(9) 0.4929(2) 0.0166(8) Uani 1 1 d . . . . .
H14A H -0.1039 0.3183 0.5459 0.025 Uiso 1 1 calc GR . . . .
H14B H -0.0963 0.3404 0.4611 0.025 Uiso 1 1 calc GR . . . .
H14C H -0.0362 0.3126 0.5057 0.025 Uiso 1 1 calc GR . . . .
C16 C 0.26549(16) 0.12420(9) 0.3785(2) 0.0109(7) Uani 1 1 d . . . . .
H16 H 0.2589 0.1079 0.3305 0.013 Uiso 1 1 calc R . . . .
C6 C -0.01424(15) 0.23150(9) 0.5040(2) 0.0098(7) Uani 1 1 d . . . . .
C3 C 0.10289(16) 0.14551(9) 0.68416(19) 0.0104(7) Uani 1 1 d . . . . .
H3 H 0.0576 0.1412 0.6942 0.012 Uiso 1 1 calc R . . . .
C11 C 0.25108(16) 0.26314(9) 0.4106(2) 0.0108(7) Uani 1 1 d . . . . .
H11 H 0.3000 0.2622 0.4182 0.013 Uiso 1 1 calc R . . . .
C22 C 0.34971(15) 0.22239(9) 0.65563(19) 0.0084(7) Uani 1 1 d . . . . .
C7 C 0.02659(15) 0.24866(9) 0.4526(2) 0.0093(7) Uani 1 1 d . . . . .
H7 H 0.0079 0.2665 0.4102 0.011 Uiso 1 1 calc R . . . .
C24 C 0.25026(16) 0.29629(9) 0.7276(2) 0.0120(7) Uani 1 1 d . . . . .
H24 H 0.2397 0.3180 0.7579 0.014 Uiso 1 1 calc R . . . .
C21 C 0.41796(15) 0.21788(9) 0.6919(2) 0.0111(7) Uani 1 1 d . . . . .
H21 H 0.4394 0.2336 0.7373 0.013 Uiso 1 1 calc R . . . .
C20 C 0.45452(16) 0.18928(10) 0.6596(2) 0.0123(7) Uani 1 1 d . . . . .
C15 C 0.21578(16) 0.14739(9) 0.40503(19) 0.0098(7) Uani 1 1 d . . . . .
H15 H 0.1691 0.1493 0.3769 0.012 Uiso 1 1 calc R . . . .
C1 C 0.21503(16) 0.14252(9) 0.6853(2) 0.0104(7) Uani 1 1 d . . . . .
H1 H 0.2619 0.1347 0.6989 0.012 Uiso 1 1 calc R . . . .
C25 C 0.20453(16) 0.27552(9) 0.6666(2) 0.0109(7) Uani 1 1 d . . . . .
H25 H 0.1570 0.2813 0.6489 0.013 Uiso 1 1 calc R . . . .
C13 C -0.19942(16) 0.28783(10) 0.4219(2) 0.0165(8) Uani 1 1 d . . . . .
H13A H -0.2201 0.2660 0.3888 0.025 Uiso 1 1 calc GR . . . .
H13B H -0.2122 0.3112 0.3899 0.025 Uiso 1 1 calc GR . . . .
H13C H -0.2163 0.2889 0.4755 0.025 Uiso 1 1 calc GR . . . .
C12 C -0.12072(16) 0.28367(9) 0.4401(2) 0.0120(7) Uani 1 1 d . . . . .
H12 H -0.1034 0.2822 0.3855 0.014 Uiso 1 1 calc R . . . .
C17 C 0.32544(16) 0.12969(9) 0.4356(2) 0.0114(7) Uani 1 1 d . . . . .
H17 H 0.3688 0.1181 0.4347 0.014 Uiso 1 1 calc R . . . .
C26 C 0.56149(16) 0.19975(9) 0.8037(2) 0.0133(7) Uani 1 1 d . . . . .
H26 H 0.5188 0.2000 0.8289 0.016 Uiso 1 1 calc R . . . .
C4 C 0.08359(15) 0.19696(9) 0.57253(19) 0.0078(7) Uani 1 1 d . . . . .
C27 C 0.58700(19) 0.24002(10) 0.7996(3) 0.0262(9) Uani 1 1 d . . . . .
H27A H 0.6281 0.2402 0.7734 0.039 Uiso 1 1 calc GR . . . .
H27B H 0.5987 0.2505 0.8570 0.039 Uiso 1 1 calc GR . . . .
H27C H 0.5508 0.2555 0.7657 0.039 Uiso 1 1 calc GR . . . .
C18 C 0.35336(16) 0.17410(9) 0.56012(19) 0.0084(7) Uani 1 1 d . . . . .
Fe1B Fe 0.77999(2) 0.37055(2) 0.92298(3) 0.00798(11) Uani 1 1 d . . . . .
S2B S 1.10380(4) 0.40224(2) 0.99110(5) 0.01075(18) Uani 1 1 d . . . . .
S1B S 0.46074(4) 0.35368(2) 0.75862(5) 0.01373(19) Uani 1 1 d . . . . .
N5B N 0.77392(13) 0.40963(8) 0.83516(17) 0.0109(6) Uani 1 1 d . . . . .
N3B N 0.68422(13) 0.36826(7) 0.87745(16) 0.0092(6) Uani 1 1 d . . . . .
N10B N 0.78458(13) 0.40932(8) 1.01361(17) 0.0107(6) Uani 1 1 d . . . . .
N1B N 0.75101(12) 0.33167(7) 0.99793(16) 0.0090(6) Uani 1 1 d . . . . .
N9B N 0.85199(12) 0.41759(7) 1.05094(16) 0.0091(6) Uani 1 1 d . . . . .
N4B N 0.70810(13) 0.41398(8) 0.78931(17) 0.0106(6) Uani 1 1 d . . . . .
N7B N 0.88145(13) 0.33309(7) 0.85181(16) 0.0087(6) Uani 1 1 d . . . . .
N8B N 0.87734(12) 0.37507(7) 0.95678(16) 0.0085(6) Uani 1 1 d . . . . .
N6B N 0.81098(13) 0.33218(8) 0.84793(17) 0.0106(6) Uani 1 1 d . . . . .
N2B N 0.68145(12) 0.32300(7) 0.97544(16) 0.0086(6) Uani 1 1 d . . . . .
C15B C 0.78857(17) 0.30473(9) 0.7937(2) 0.0120(7) Uani 1 1 d . . . . .
H15B H 0.7415 0.2976 0.7775 0.014 Uiso 1 1 calc R . . . .
C20B C 1.01531(15) 0.39326(9) 0.9813(2) 0.0097(7) Uani 1 1 d . . . . .
C13B C 0.35959(17) 0.39013(11) 0.6549(2) 0.0199(8) Uani 1 1 d . . . . .
H13D H 0.3617 0.3686 0.6169 0.030 Uiso 1 1 calc GR . . . .
H13E H 0.3423 0.4125 0.6214 0.030 Uiso 1 1 calc GR . . . .
H13F H 0.3285 0.3840 0.6940 0.030 Uiso 1 1 calc GR . . . .
C10B C 0.77118(17) 0.45704(10) 0.7410(2) 0.0145(7) Uani 1 1 d . . . . .
H10B H 0.7862 0.4773 0.7097 0.017 Uiso 1 1 calc R . . . .
C5B C 0.57462(16) 0.33891(9) 0.8737(2) 0.0109(7) Uani 1 1 d . . . . .
H5B H 0.5469 0.3211 0.8966 0.013 Uiso 1 1 calc R . . . .
C6B C 0.54709(16) 0.36219(9) 0.8043(2) 0.0111(7) Uani 1 1 d . . . . .
C18B C 0.91874(16) 0.35794(9) 0.9114(2) 0.0102(7) Uani 1 1 d . . . . .
C4B C 0.64340(16) 0.34326(9) 0.9066(2) 0.0093(7) Uani 1 1 d . . . . .
C9B C 0.70623(17) 0.44257(9) 0.7317(2) 0.0117(7) Uani 1 1 d . . . . .
H9B H 0.6669 0.4508 0.6924 0.014 Uiso 1 1 calc R . . . .
C26B C 1.11635(16) 0.44885(9) 1.0412(2) 0.0113(7) Uani 1 1 d . . . . .
H26B H 1.0951 0.4491 1.0931 0.014 Uiso 1 1 calc R . . . .
C25B C 0.74606(16) 0.43005(9) 1.0550(2) 0.0116(7) Uani 1 1 d . . . . .
H25B H 0.6971 0.4306 1.0428 0.014 Uiso 1 1 calc R . . . .
C14B C 0.43005(17) 0.42945(10) 0.7698(2) 0.0160(8) Uani 1 1 d . . . . .
H14D H 0.3983 0.4224 0.8074 0.024 Uiso 1 1 calc GR . . . .
H14E H 0.4147 0.4533 0.7407 0.024 Uiso 1 1 calc GR . . . .
H14F H 0.4766 0.4328 0.8032 0.024 Uiso 1 1 calc GR . . . .
C11B C 0.81145(17) 0.43599(9) 0.8063(2) 0.0129(7) Uani 1 1 d . . . . .
H11B H 0.8592 0.4401 0.8269 0.016 Uiso 1 1 calc R . . . .
C7B C 0.58879(15) 0.38898(9) 0.7731(2) 0.0113(7) Uani 1 1 d . . . . .
H7B H 0.5707 0.4053 0.7273 0.014 Uiso 1 1 calc R . . . .
C2B C 0.71987(15) 0.29001(9) 1.0901(2) 0.0115(7) Uani 1 1 d . . . . .
H2B H 0.7229 0.2734 1.1372 0.014 Uiso 1 1 calc R . . . .
C8B C 0.65699(16) 0.39042(9) 0.8117(2) 0.0103(7) Uani 1 1 d . . . . .
C3B C 0.66242(16) 0.29791(9) 1.0307(2) 0.0134(7) Uani 1 1 d . . . . .
H3B H 0.6176 0.2877 1.0285 0.016 Uiso 1 1 calc R . . . .
C17B C 0.90145(16) 0.30605(9) 0.8013(2) 0.0122(7) Uani 1 1 d . . . . .
H17B H 0.9473 0.3010 0.7940 0.015 Uiso 1 1 calc R . . . .
C21B C 0.97292(15) 0.41116(9) 1.0302(2) 0.0100(7) Uani 1 1 d . . . . .
H21B H 0.9906 0.4294 1.0722 0.012 Uiso 1 1 calc R . . . .
C1B C 0.77355(16) 0.31155(9) 1.0669(2) 0.0099(7) Uani 1 1 d . . . . .
H1B H 0.8198 0.3116 1.0969 0.012 Uiso 1 1 calc R . . . .
C23B C 0.85384(16) 0.44293(9) 1.1152(2) 0.0104(7) Uani 1 1 d . . . . .
H23B H 0.8939 0.4529 1.1504 0.012 Uiso 1 1 calc R . . . .
C28B C 1.19403(16) 0.45449(10) 1.0665(2) 0.0160(8) Uani 1 1 d . . . . .
H28D H 1.2134 0.4346 1.1067 0.024 Uiso 1 1 calc GR . . . .
H28E H 1.2035 0.4795 1.0931 0.024 Uiso 1 1 calc GR . . . .
H28F H 1.2152 0.4530 1.0160 0.024 Uiso 1 1 calc GR . . . .
C16B C 0.84323(16) 0.28745(9) 0.7630(2) 0.0133(7) Uani 1 1 d . . . . .
H16B H 0.8403 0.2671 0.7237 0.016 Uiso 1 1 calc R . . . .
C12B C 0.43099(16) 0.39825(9) 0.7047(2) 0.0130(7) Uani 1 1 d . . . . .
H12B H 0.4624 0.4056 0.6652 0.016 Uiso 1 1 calc R . . . .
C24B C 0.78712(16) 0.45117(9) 1.1195(2) 0.0120(7) Uani 1 1 d . . . . .
H24B H 0.7715 0.4679 1.1583 0.014 Uiso 1 1 calc R . . . .
C27B C 1.08329(16) 0.47970(10) 0.9804(2) 0.0149(8) Uani 1 1 d . . . . .
H27D H 1.1054 0.4802 0.9307 0.022 Uiso 1 1 calc GR . . . .
H27E H 1.0892 0.5044 1.0090 0.022 Uiso 1 1 calc GR . . . .
H27F H 1.0340 0.4743 0.9626 0.022 Uiso 1 1 calc GR . . . .
C19B C 0.98827(15) 0.36594(9) 0.9206(2) 0.0110(7) Uani 1 1 d . . . . .
H19B H 1.0166 0.3535 0.8872 0.013 Uiso 1 1 calc R . . . .
C22B C 0.90410(16) 0.40103(9) 1.01436(19) 0.0087(7) Uani 1 1 d . . . . .
Fe1C Fe 0.76952(2) 0.45862(2) 0.42742(3) 0.00761(11) Uani 1 1 d . . . . .
S1C S 0.44949(4) 0.49225(2) 0.29211(5) 0.01176(18) Uani 1 1 d . . . . .
S2C S 1.09581(4) 0.43230(2) 0.50186(5) 0.01155(18) Uani 1 1 d . . . . .
N6C N 0.77414(12) 0.41817(7) 0.51495(16) 0.0089(6) Uani 1 1 d . . . . .
N3C N 0.67293(13) 0.46522(7) 0.39077(16) 0.0086(6) Uani 1 1 d . . . . .
N5C N 0.75234(12) 0.42130(7) 0.33496(16) 0.0083(6) Uani 1 1 d . . . . .
N1C N 0.75117(12) 0.49738(7) 0.50884(16) 0.0082(6) Uani 1 1 d . . . . .
N8C N 0.86661(13) 0.45216(7) 0.45749(16) 0.0087(6) Uani 1 1 d . . . . .
N4C N 0.68469(12) 0.42194(7) 0.29164(16) 0.0081(6) Uani 1 1 d . . . . .
N7C N 0.84194(12) 0.40971(7) 0.55213(16) 0.0087(6) Uani 1 1 d . . . . .
N10C N 0.80034(12) 0.49689(7) 0.35197(17) 0.0093(6) Uani 1 1 d . . . . .
N9C N 0.87081(12) 0.49498(7) 0.35406(16) 0.0088(6) Uani 1 1 d . . . . .
N2C N 0.68232(13) 0.50805(8) 0.49649(17) 0.0104(6) Uani 1 1 d . . . . .
C13C C 0.40409(18) 0.42534(10) 0.2106(3) 0.0283(10) Uani 1 1 d . . . . .
H13G H 0.4437 0.4128 0.2459 0.042 Uiso 1 1 calc GR . . . .
H13H H 0.3917 0.4118 0.1567 0.042 Uiso 1 1 calc GR . . . .
H13I H 0.3648 0.4251 0.2400 0.042 Uiso 1 1 calc GR . . . .
C22C C 0.90835(16) 0.47042(9) 0.4141(2) 0.0093(7) Uani 1 1 d . . . . .
C25C C 0.77837(16) 0.52382(9) 0.2957(2) 0.0119(7) Uani 1 1 d . . . . .
H25C H 0.7316 0.5316 0.2803 0.014 Uiso 1 1 calc R . . . .
C10C C 0.73591(16) 0.37759(9) 0.2307(2) 0.0115(7) Uani 1 1 d . . . . .
H10C H 0.7453 0.3578 0.1944 0.014 Uiso 1 1 calc R . . . .
C26C C 1.11234(16) 0.38324(9) 0.5362(2) 0.0108(7) Uani 1 1 d . . . . .
H26C H 1.0882 0.3777 0.5843 0.013 Uiso 1 1 calc R . . . .
C1C C 0.78156(16) 0.51758(9) 0.5747(2) 0.0098(7) Uani 1 1 d . . . . .
H1C H 0.8294 0.5164 0.5982 0.012 Uiso 1 1 calc R . . . .
C27C C 1.19012(15) 0.38062(10) 0.5667(2) 0.0151(8) Uani 1 1 d . . . . .
H27G H 1.2138 0.3880 0.5208 0.023 Uiso 1 1 calc GR . . . .
H27H H 1.2026 0.3545 0.5840 0.023 Uiso 1 1 calc GR . . . .
H27I H 1.2039 0.3977 0.6151 0.023 Uiso 1 1 calc GR . . . .
C18C C 0.89393(16) 0.42673(9) 0.5164(2) 0.0094(7) Uani 1 1 d . . . . .
C28C C 1.08658(17) 0.35599(10) 0.4634(2) 0.0186(8) Uani 1 1 d . . . . .
H28G H 1.0376 0.3608 0.4414 0.028 Uiso 1 1 calc GR . . . .
H28H H 1.0925 0.3298 0.4838 0.028 Uiso 1 1 calc GR . . . .
H28I H 1.1130 0.3599 0.4181 0.028 Uiso 1 1 calc GR . . . .
C5C C 0.56913(16) 0.49856(9) 0.4006(2) 0.0107(7) Uani 1 1 d . . . . .
H5C H 0.5453 0.5163 0.4293 0.013 Uiso 1 1 calc R . . . .
C15C C 0.73595(16) 0.39591(9) 0.5527(2) 0.0109(7) Uani 1 1 d . . . . .
H15C H 0.6870 0.3951 0.5395 0.013 Uiso 1 1 calc R . . . .
C21C C 0.97820(15) 0.46415(9) 0.4262(2) 0.0105(7) Uani 1 1 d . . . . .
H21C H 1.0065 0.4773 0.3940 0.013 Uiso 1 1 calc R . . . .
C9C C 0.67450(16) 0.39574(9) 0.2288(2) 0.0115(7) Uani 1 1 d . . . . .
H9C H 0.6325 0.3909 0.1907 0.014 Uiso 1 1 calc R . . . .
C8C C 0.64001(16) 0.44695(9) 0.3224(2) 0.0090(7) Uani 1 1 d . . . . .
C23C C 0.89091(16) 0.52081(9) 0.3006(2) 0.0119(7) Uani 1 1 d . . . . .
H23C H 0.9367 0.5251 0.2920 0.014 Uiso 1 1 calc R . . . .
C16C C 0.77661(16) 0.37344(9) 0.6151(2) 0.0120(7) Uani 1 1 d . . . . .
H16C H 0.7608 0.3553 0.6510 0.014 Uiso 1 1 calc R . . . .
C20C C 1.00617(15) 0.43756(9) 0.4880(2) 0.0099(7) Uani 1 1 d . . . . .
C11C C 0.78262(16) 0.39437(9) 0.2978(2) 0.0108(7) Uani 1 1 d . . . . .
H11C H 0.8297 0.3872 0.3140 0.013 Uiso 1 1 calc R . . . .
C24C C 0.83293(16) 0.53938(9) 0.2616(2) 0.0125(7) Uani 1 1 d . . . . .
H24C H 0.8300 0.5588 0.2200 0.015 Uiso 1 1 calc R . . . .
C2C C 0.73430(16) 0.54089(9) 0.6052(2) 0.0119(7) Uani 1 1 d . . . . .
H2C H 0.7436 0.5579 0.6519 0.014 Uiso 1 1 calc R . . . .
C7C C 0.57145(15) 0.45286(9) 0.2878(2) 0.0094(7) Uani 1 1 d . . . . .
H7C H 0.5495 0.4395 0.2388 0.011 Uiso 1 1 calc R . . . .
C3C C 0.67163(17) 0.53418(9) 0.5541(2) 0.0116(7) Uani 1 1 d . . . . .
H3C H 0.6289 0.5457 0.5583 0.014 Uiso 1 1 calc R . . . .
C17C C 0.84346(16) 0.38292(9) 0.6137(2) 0.0103(7) Uani 1 1 d . . . . .
H17C H 0.8834 0.3728 0.6489 0.012 Uiso 1 1 calc R . . . .
C6C C 0.53596(15) 0.47920(9) 0.3281(2) 0.0097(7) Uani 1 1 d . . . . .
C14C C 0.36045(17) 0.48804(11) 0.1451(2) 0.0223(9) Uani 1 1 d . . . . .
H14G H 0.3241 0.4894 0.1791 0.033 Uiso 1 1 calc GR . . . .
H14H H 0.3427 0.4751 0.0915 0.033 Uiso 1 1 calc GR . . . .
H14I H 0.3751 0.5138 0.1334 0.033 Uiso 1 1 calc GR . . . .
C4C C 0.63823(16) 0.49055(9) 0.4283(2) 0.0102(7) Uani 1 1 d . . . . .
C12C C 0.42262(17) 0.46576(10) 0.1942(2) 0.0176(8) Uani 1 1 d . . . . .
H12C H 0.4608 0.4659 0.1611 0.021 Uiso 1 1 calc R . . . .
C19C C 0.96368(16) 0.41847(9) 0.5348(2) 0.0111(7) Uani 1 1 d . . . . .
H19C H 0.9819 0.4006 0.5774 0.013 Uiso 1 1 calc R . . . .
F1C F 0.93527(9) 0.48794(5) 0.83368(12) 0.0175(4) Uani 1 1 d . . . . .
F4C F 0.99538(9) 0.53378(5) 0.77914(12) 0.0172(4) Uani 1 1 d . . . . .
F3C F 0.93699(9) 0.48837(5) 0.69175(11) 0.0130(4) Uani 1 1 d . . . . .
F2C F 0.87735(9) 0.53414(5) 0.74919(12) 0.0175(5) Uani 1 1 d . . . . .
B1C B 0.93588(19) 0.51108(11) 0.7638(2) 0.0125(8) Uani 1 1 d . . . . .
F6C F 0.47595(9) 0.42716(6) 0.49889(13) 0.0237(5) Uani 1 1 d . . . . .
F7C F 0.57243(9) 0.40639(5) 0.45378(12) 0.0184(5) Uani 1 1 d . . . . .
F5C F 0.54414(10) 0.38126(6) 0.57209(12) 0.0226(5) Uani 1 1 d . . . . .
F8C F 0.58257(11) 0.44259(6) 0.57197(13) 0.0308(6) Uani 1 1 d . . . . .
B2C B 0.5434(2) 0.41433(11) 0.5237(2) 0.0146(9) Uani 1 1 d . . . . .
F2 F 0.00203(9) 0.14140(5) 0.20853(12) 0.0162(4) Uani 1 1 d . . . . .
F4 F 0.11991(9) 0.14186(6) 0.23037(12) 0.0191(5) Uani 1 1 d . . . . .
F3 F 0.06294(9) 0.18586(5) 0.29615(11) 0.0140(4) Uani 1 1 d . . . . .
F1 F 0.05778(9) 0.18864(6) 0.15261(12) 0.0192(5) Uani 1 1 d . . . . .
B1 B 0.06051(19) 0.16448(12) 0.2215(2) 0.0136(8) Uani 1 1 d . . . . .
F8B F 0.48466(9) 0.39460(5) 0.97084(11) 0.0141(4) Uani 1 1 d . . . . .
F7B F 0.59175(9) 0.37998(5) 1.04583(11) 0.0148(4) Uani 1 1 d . . . . .
F5B F 0.57607(9) 0.43330(5) 0.96367(12) 0.0155(4) Uani 1 1 d . . . . .
F6B F 0.53199(9) 0.42994(5) 1.08549(11) 0.0163(4) Uani 1 1 d . . . . .
B2B B 0.54666(18) 0.40928(11) 1.0165(2) 0.0125(8) Uani 1 1 d . . . . .
F7 F 0.41288(9) 0.25470(5) 0.50967(11) 0.0146(4) Uani 1 1 d . . . . .
F5 F 0.44003(13) 0.26161(6) 0.38007(13) 0.0398(7) Uani 1 1 d . . . . .
F6 F 0.39702(10) 0.20575(5) 0.41456(12) 0.0189(5) Uani 1 1 d . . . . .
F8 F 0.50450(10) 0.22291(7) 0.47840(15) 0.0438(7) Uani 1 1 d . . . . .
B2 B 0.4384(2) 0.23626(12) 0.4446(2) 0.0155(9) Uani 1 1 d . . . . .
F4B F 0.98332(9) 0.30737(5) 1.27773(12) 0.0168(4) Uani 1 1 d . . . . .
F2B F 0.86582(9) 0.31437(6) 1.24879(12) 0.0194(5) Uani 1 1 d . . . . .
F3B F 0.93433(9) 0.36240(6) 1.31346(12) 0.0200(5) Uani 1 1 d . . . . .
F1B F 0.93280(9) 0.34842(5) 1.17449(11) 0.0143(4) Uani 1 1 d . . . . .
B1B B 0.92852(19) 0.33318(12) 1.2540(2) 0.0142(9) Uani 1 1 d . . . . .
O1C O 0.65170(12) 0.49087(7) 0.16221(15) 0.0180(6) Uani 1 1 d . . . . .
O2C O 0.69058(11) 0.53554(7) 0.09143(15) 0.0184(6) Uani 1 1 d . . . . .
N11C N 0.64432(14) 0.51435(8) 0.10534(18) 0.0140(6) Uani 1 1 d . . . . .
C29C C 0.57551(16) 0.51694(10) 0.0490(2) 0.0194(8) Uani 1 1 d . . . . .
H29A H 0.5693 0.4953 0.0101 0.029 Uiso 1 1 calc GR . . . .
H29B H 0.5726 0.5406 0.0165 0.029 Uiso 1 1 calc GR . . . .
H29C H 0.5394 0.5166 0.0834 0.029 Uiso 1 1 calc GR . . . .
O1B O 0.66222(13) 0.30034(8) 0.57959(19) 0.0317(7) Uani 1 1 d . . . . .
O2B O 0.63154(13) 0.31499(8) 0.69589(17) 0.0307(7) Uani 1 1 d . . . . .
N11B N 0.61830(15) 0.30440(8) 0.6233(2) 0.0207(7) Uani 1 1 d . . . . .
C29B C 0.54543(17) 0.29502(10) 0.5873(2) 0.0210(8) Uani 1 1 d . . . . .
H29D H 0.5364 0.2684 0.5995 0.031 Uiso 1 1 calc GR . . . .
H29E H 0.5369 0.2990 0.5259 0.031 Uiso 1 1 calc GR . . . .
H29F H 0.5148 0.3115 0.6128 0.031 Uiso 1 1 calc GR . . . .
O2 O 0.37287(15) 0.15390(8) 0.79949(18) 0.0385(8) Uani 1 1 d . . . . .
O1 O 0.30948(13) 0.12915(8) 0.88118(17) 0.0313(7) Uani 1 1 d . . . . .
N11 N 0.36160(17) 0.14490(9) 0.8693(2) 0.0260(8) Uani 1 1 d . . . . .
C29 C 0.4167(2) 0.15322(12) 0.9434(2) 0.0365(11) Uani 1 1 d . . . . .
H29G H 0.4096 0.1786 0.9651 0.055 Uiso 1 1 calc GR . . . .
H29H H 0.4618 0.1521 0.9262 0.055 Uiso 1 1 calc GR . . . .
H29I H 0.4151 0.1344 0.9879 0.055 Uiso 1 1 calc GR . . . .


_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 N5 1.986(3) . ?
Fe1 N3 1.905(2) . ?
Fe1 N8 1.904(2) . ?
Fe1 N6 1.978(3) . ?
Fe1 N1 1.978(3) . ?
Fe1 N10 1.962(3) . ?
S1 C6 1.748(3) . ?
S1 C12 1.821(3) . ?
S2 C20 1.757(3) . ?
S2 C26 1.829(3) . ?
N7 N6 1.387(3) . ?
N7 C17 1.351(4) . ?
N7 C18 1.405(4) . ?
N5 N4 1.381(3) . ?
N5 C11 1.330(4) . ?
N3 C8 1.334(4) . ?
N3 C4 1.338(4) . ?
N9 N10 1.376(3) . ?
N9 C23 1.361(4) . ?
N9 C22 1.407(4) . ?
N4 C9 1.365(4) . ?
N4 C8 1.404(4) . ?
N8 C22 1.335(4) . ?
N8 C18 1.336(4) . ?
N2 N1 1.384(3) . ?
N2 C3 1.358(4) . ?
N2 C4 1.408(4) . ?
N6 C15 1.327(4) . ?
N1 C1 1.324(4) . ?
N10 C25 1.319(4) . ?
C5 H5 0.9500 . ?
C5 C6 1.407(4) . ?
C5 C4 1.370(4) . ?
C10 H10 0.9500 . ?
C10 C9 1.363(4) . ?
C10 C11 1.403(4) . ?
C9 H9 0.9500 . ?
C23 H23 0.9500 . ?
C23 C24 1.366(4) . ?
C19 H19 0.9500 . ?
C19 C20 1.411(4) . ?
C19 C18 1.374(4) . ?
C28 H28A 0.9800 . ?
C28 H28B 0.9800 . ?
C28 H28C 0.9800 . ?
C28 C26 1.528(4) . ?
C2 H2 0.9500 . ?
C2 C3 1.369(4) . ?
C2 C1 1.407(4) . ?
C8 C7 1.384(4) . ?
C14 H14A 0.9800 . ?
C14 H14B 0.9800 . ?
C14 H14C 0.9800 . ?
C14 C12 1.523(4) . ?
C16 H16 0.9500 . ?
C16 C15 1.402(4) . ?
C16 C17 1.369(4) . ?
C6 C7 1.394(4) . ?
C3 H3 0.9500 . ?
C11 H11 0.9500 . ?
C22 C21 1.374(4) . ?
C7 H7 0.9500 . ?
C24 H24 0.9500 . ?
C24 C25 1.407(4) . ?
C21 H21 0.9500 . ?
C21 C20 1.394(5) . ?
C15 H15 0.9500 . ?
C1 H1 0.9500 . ?
C25 H25 0.9500 . ?
C13 H13A 0.9800 . ?
C13 H13B 0.9800 . ?
C13 H13C 0.9800 . ?
C13 C12 1.532(4) . ?
C12 H12 1.0000 . ?
C17 H17 0.9500 . ?
C26 H26 1.0000 . ?
C26 C27 1.510(5) . ?
C27 H27A 0.9800 . ?
C27 H27B 0.9800 . ?
C27 H27C 0.9800 . ?
Fe1B N5B 1.959(3) . ?
Fe1B N3B 1.896(2) . ?
Fe1B N10B 1.986(3) . ?
Fe1B N1B 1.977(3) . ?
Fe1B N8B 1.903(2) . ?
Fe1B N6B 1.982(3) . ?
S2B C20B 1.752(3) . ?
S2B C26B 1.824(3) . ?
S1B C6B 1.751(3) . ?
S1B C12B 1.835(3) . ?
N5B N4B 1.377(3) . ?
N5B C11B 1.324(4) . ?
N3B C4B 1.335(4) . ?
N3B C8B 1.342(4) . ?
N10B N9B 1.384(3) . ?
N10B C25B 1.319(4) . ?
N1B N2B 1.386(3) . ?
N1B C1B 1.321(4) . ?
N9B C23B 1.361(4) . ?
N9B C22B 1.402(4) . ?
N4B C9B 1.363(4) . ?
N4B C8B 1.403(4) . ?
N7B N6B 1.380(3) . ?
N7B C18B 1.400(4) . ?
N7B C17B 1.356(4) . ?
N8B C18B 1.336(4) . ?
N8B C22B 1.337(4) . ?
N6B C15B 1.321(4) . ?
N2B C4B 1.410(4) . ?
N2B C3B 1.354(4) . ?
C15B H15B 0.9500 . ?
C15B C16B 1.405(5) . ?
C20B C21B 1.399(4) . ?
C20B C19B 1.404(4) . ?
C13B H13D 0.9800 . ?
C13B H13E 0.9800 . ?
C13B H13F 0.9800 . ?
C13B C12B 1.513(4) . ?
C10B H10B 0.9500 . ?
C10B C9B 1.361(4) . ?
C10B C11B 1.404(4) . ?
C5B H5B 0.9500 . ?
C5B C6B 1.409(4) . ?
C5B C4B 1.370(4) . ?
C6B C7B 1.404(5) . ?
C18B C19B 1.381(4) . ?
C9B H9B 0.9500 . ?
C26B H26B 1.0000 . ?
C26B C28B 1.523(4) . ?
C26B C27B 1.524(4) . ?
C25B H25B 0.9500 . ?
C25B C24B 1.404(4) . ?
C14B H14D 0.9800 . ?
C14B H14E 0.9800 . ?
C14B H14F 0.9800 . ?
C14B C12B 1.518(5) . ?
C11B H11B 0.9500 . ?
C7B H7B 0.9500 . ?
C7B C8B 1.374(4) . ?
C2B H2B 0.9500 . ?
C2B C3B 1.368(4) . ?
C2B C1B 1.408(4) . ?
C3B H3B 0.9500 . ?
C17B H17B 0.9500 . ?
C17B C16B 1.366(4) . ?
C21B H21B 0.9500 . ?
C21B C22B 1.381(4) . ?
C1B H1B 0.9500 . ?
C23B H23B 0.9500 . ?
C23B C24B 1.362(4) . ?
C28B H28D 0.9800 . ?
C28B H28E 0.9800 . ?
C28B H28F 0.9800 . ?
C16B H16B 0.9500 . ?
C12B H12B 1.0000 . ?
C24B H24B 0.9500 . ?
C27B H27D 0.9800 . ?
C27B H27E 0.9800 . ?
C27B H27F 0.9800 . ?
C19B H19B 0.9500 . ?
Fe1C N6C 1.992(3) . ?
Fe1C N3C 1.901(2) . ?
Fe1C N5C 1.965(3) . ?
Fe1C N1C 1.970(3) . ?
Fe1C N8C 1.900(3) . ?
Fe1C N10C 1.982(3) . ?
S1C C6C 1.757(3) . ?
S1C C12C 1.821(3) . ?
S2C C26C 1.824(3) . ?
S2C C20C 1.751(3) . ?
N6C N7C 1.392(3) . ?
N6C C15C 1.311(4) . ?
N3C C8C 1.333(4) . ?
N3C C4C 1.334(4) . ?
N5C N4C 1.386(3) . ?
N5C C11C 1.321(4) . ?
N1C N2C 1.387(3) . ?
N1C C1C 1.323(4) . ?
N8C C22C 1.338(4) . ?
N8C C18C 1.341(4) . ?
N4C C9C 1.355(4) . ?
N4C C8C 1.400(4) . ?
N7C C18C 1.400(4) . ?
N7C C17C 1.363(4) . ?
N10C N9C 1.386(3) . ?
N10C C25C 1.327(4) . ?
N9C C22C 1.401(4) . ?
N9C C23C 1.360(4) . ?
N2C C3C 1.349(4) . ?
N2C C4C 1.408(4) . ?
C13C H13G 0.9800 . ?
C13C H13H 0.9800 . ?
C13C H13I 0.9800 . ?
C13C C12C 1.505(5) . ?
C22C C21C 1.373(4) . ?
C25C H25C 0.9500 . ?
C25C C24C 1.407(5) . ?
C10C H10C 0.9500 . ?
C10C C9C 1.365(4) . ?
C10C C11C 1.411(4) . ?
C26C H26C 1.0000 . ?
C26C C27C 1.524(4) . ?
C26C C28C 1.525(4) . ?
C1C H1C 0.9500 . ?
C1C C2C 1.398(4) . ?
C27C H27G 0.9800 . ?
C27C H27H 0.9800 . ?
C27C H27I 0.9800 . ?
C18C C19C 1.383(4) . ?
C28C H28G 0.9800 . ?
C28C H28H 0.9800 . ?
C28C H28I 0.9800 . ?
C5C H5C 0.9500 . ?
C5C C6C 1.404(4) . ?
C5C C4C 1.382(4) . ?
C15C H15C 0.9500 . ?
C15C C16C 1.406(4) . ?
C21C H21C 0.9500 . ?
C21C C20C 1.401(4) . ?
C9C H9C 0.9500 . ?
C8C C7C 1.379(4) . ?
C23C H23C 0.9500 . ?
C23C C24C 1.365(4) . ?
C16C H16C 0.9500 . ?
C16C C17C 1.364(4) . ?
C20C C19C 1.397(5) . ?
C11C H11C 0.9500 . ?
C24C H24C 0.9500 . ?
C2C H2C 0.9500 . ?
C2C C3C 1.372(4) . ?
C7C H7C 0.9500 . ?
C7C C6C 1.391(4) . ?
C3C H3C 0.9500 . ?
C17C H17C 0.9500 . ?
C14C H14G 0.9800 . ?
C14C H14H 0.9800 . ?
C14C H14I 0.9800 . ?
C14C C12C 1.544(4) . ?
C12C H12C 1.0000 . ?
C19C H19C 0.9500 . ?
F1C B1C 1.389(4) . ?
F4C B1C 1.403(4) . ?
F3C B1C 1.411(4) . ?
F2C B1C 1.395(4) . ?
F6C B2C 1.392(4) . ?
F7C B2C 1.381(4) . ?
F5C B2C 1.399(4) . ?
F8C B2C 1.402(4) . ?
F2 B1 1.395(4) . ?
F4 B1 1.402(4) . ?
F3 B1 1.410(4) . ?
F1 B1 1.389(4) . ?
F8B B2B 1.403(4) . ?
F7B B2B 1.386(4) . ?
F5B B2B 1.399(4) . ?
F6B B2B 1.400(4) . ?
F7 B2 1.401(4) . ?
F5 B2 1.374(5) . ?
F6 B2 1.381(4) . ?
F8 B2 1.397(4) . ?
F4B B1B 1.410(4) . ?
F2B B1B 1.392(4) . ?
F3B B1B 1.395(4) . ?
F1B B1B 1.402(4) . ?
O1C N11C 1.221(3) . ?
O2C N11C 1.231(3) . ?
N11C C29C 1.488(4) . ?
C29C H29A 0.9800 . ?
C29C H29B 0.9800 . ?
C29C H29C 0.9800 . ?
O1B N11B 1.221(4) . ?
O2B N11B 1.206(4) . ?
N11B C29B 1.484(4) . ?
C29B H29D 0.9800 . ?
C29B H29E 0.9800 . ?
C29B H29F 0.9800 . ?
O2 N11 1.225(4) . ?
O1 N11 1.214(4) . ?
N11 C29 1.485(4) . ?
C29 H29G 0.9800 . ?
C29 H29H 0.9800 . ?
C29 H29I 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
N3 Fe1 N5 79.38(11) . . ?
N3 Fe1 N6 105.53(10) . . ?
N3 Fe1 N1 80.00(11) . . ?
N3 Fe1 N10 95.17(11) . . ?
N8 Fe1 N5 104.54(11) . . ?
N8 Fe1 N3 173.69(11) . . ?
N8 Fe1 N6 79.60(10) . . ?
N8 Fe1 N1 96.19(11) . . ?
N8 Fe1 N10 79.89(11) . . ?
N6 Fe1 N5 90.09(11) . . ?
N6 Fe1 N1 93.27(11) . . ?
N1 Fe1 N5 159.26(10) . . ?
N10 Fe1 N5 91.69(11) . . ?
N10 Fe1 N6 159.19(10) . . ?
N10 Fe1 N1 92.37(11) . . ?
C6 S1 C12 105.19(15) . . ?
C20 S2 C26 105.37(16) . . ?
N6 N7 C18 116.1(2) . . ?
C17 N7 N6 111.3(2) . . ?
C17 N7 C18 132.0(3) . . ?
N4 N5 Fe1 112.55(19) . . ?
C11 N5 Fe1 142.6(2) . . ?
C11 N5 N4 104.7(2) . . ?
C8 N3 Fe1 120.9(2) . . ?
C8 N3 C4 118.6(3) . . ?
C4 N3 Fe1 119.6(2) . . ?
N10 N9 C22 116.3(2) . . ?
C23 N9 N10 111.1(3) . . ?
C23 N9 C22 132.5(3) . . ?
N5 N4 C8 116.5(2) . . ?
C9 N4 N5 111.1(3) . . ?
C9 N4 C8 132.3(3) . . ?
C22 N8 Fe1 120.2(2) . . ?
C22 N8 C18 119.0(3) . . ?
C18 N8 Fe1 120.6(2) . . ?
N1 N2 C4 116.2(3) . . ?
C3 N2 N1 111.2(2) . . ?
C3 N2 C4 132.1(3) . . ?
N7 N6 Fe1 112.80(18) . . ?
C15 N6 Fe1 142.1(2) . . ?
C15 N6 N7 104.8(3) . . ?
N2 N1 Fe1 112.38(19) . . ?
C1 N1 Fe1 142.9(2) . . ?
C1 N1 N2 104.7(3) . . ?
N9 N10 Fe1 113.10(19) . . ?
C25 N10 Fe1 141.4(2) . . ?
C25 N10 N9 105.3(2) . . ?
C6 C5 H5 121.3 . . ?
C4 C5 H5 121.3 . . ?
C4 C5 C6 117.3(3) . . ?
C9 C10 H10 126.9 . . ?
C9 C10 C11 106.2(3) . . ?
C11 C10 H10 126.9 . . ?
N4 C9 H9 126.6 . . ?
C10 C9 N4 106.7(3) . . ?
C10 C9 H9 126.6 . . ?
N9 C23 H23 126.7 . . ?
N9 C23 C24 106.6(3) . . ?
C24 C23 H23 126.7 . . ?
C20 C19 H19 121.5 . . ?
C18 C19 H19 121.5 . . ?
C18 C19 C20 116.9(3) . . ?
H28A C28 H28B 109.5 . . ?
H28A C28 H28C 109.5 . . ?
H28B C28 H28C 109.5 . . ?
C26 C28 H28A 109.5 . . ?
C26 C28 H28B 109.5 . . ?
C26 C28 H28C 109.5 . . ?
C3 C2 H2 127.2 . . ?
C3 C2 C1 105.6(3) . . ?
C1 C2 H2 127.2 . . ?
N3 C8 N4 110.2(3) . . ?
N3 C8 C7 123.4(3) . . ?
C7 C8 N4 126.3(3) . . ?
H14A C14 H14B 109.5 . . ?
H14A C14 H14C 109.5 . . ?
H14B C14 H14C 109.5 . . ?
C12 C14 H14A 109.5 . . ?
C12 C14 H14B 109.5 . . ?
C12 C14 H14C 109.5 . . ?
C15 C16 H16 126.9 . . ?
C17 C16 H16 126.9 . . ?
C17 C16 C15 106.2(3) . . ?
C5 C6 S1 114.4(2) . . ?
C7 C6 S1 125.4(2) . . ?
C7 C6 C5 120.2(3) . . ?
N2 C3 C2 106.9(3) . . ?
N2 C3 H3 126.5 . . ?
C2 C3 H3 126.5 . . ?
N5 C11 C10 111.2(3) . . ?
N5 C11 H11 124.4 . . ?
C10 C11 H11 124.4 . . ?
N8 C22 N9 110.4(3) . . ?
N8 C22 C21 123.3(3) . . ?
C21 C22 N9 126.3(3) . . ?
C8 C7 C6 117.1(3) . . ?
C8 C7 H7 121.5 . . ?
C6 C7 H7 121.5 . . ?
C23 C24 H24 127.0 . . ?
C23 C24 C25 105.9(3) . . ?
C25 C24 H24 127.0 . . ?
C22 C21 H21 121.3 . . ?
C22 C21 C20 117.3(3) . . ?
C20 C21 H21 121.3 . . ?
C19 C20 S2 115.2(3) . . ?
C21 C20 S2 124.6(2) . . ?
C21 C20 C19 120.2(3) . . ?
N6 C15 C16 110.9(3) . . ?
N6 C15 H15 124.5 . . ?
C16 C15 H15 124.5 . . ?
N1 C1 C2 111.6(3) . . ?
N1 C1 H1 124.2 . . ?
C2 C1 H1 124.2 . . ?
N10 C25 C24 111.1(3) . . ?
N10 C25 H25 124.5 . . ?
C24 C25 H25 124.5 . . ?
H13A C13 H13B 109.5 . . ?
H13A C13 H13C 109.5 . . ?
H13B C13 H13C 109.5 . . ?
C12 C13 H13A 109.5 . . ?
C12 C13 H13B 109.5 . . ?
C12 C13 H13C 109.5 . . ?
S1 C12 H12 109.7 . . ?
C14 C12 S1 110.2(2) . . ?
C14 C12 C13 111.4(3) . . ?
C14 C12 H12 109.7 . . ?
C13 C12 S1 106.0(2) . . ?
C13 C12 H12 109.7 . . ?
N7 C17 C16 106.7(3) . . ?
N7 C17 H17 126.6 . . ?
C16 C17 H17 126.6 . . ?
S2 C26 H26 108.8 . . ?
C28 C26 S2 107.0(2) . . ?
C28 C26 H26 108.8 . . ?
C27 C26 S2 111.7(2) . . ?
C27 C26 C28 111.6(3) . . ?
C27 C26 H26 108.8 . . ?
N3 C4 N2 110.9(3) . . ?
N3 C4 C5 123.4(3) . . ?
C5 C4 N2 125.6(3) . . ?
C26 C27 H27A 109.5 . . ?
C26 C27 H27B 109.5 . . ?
C26 C27 H27C 109.5 . . ?
H27A C27 H27B 109.5 . . ?
H27A C27 H27C 109.5 . . ?
H27B C27 H27C 109.5 . . ?
N8 C18 N7 110.6(3) . . ?
N8 C18 C19 123.2(3) . . ?
C19 C18 N7 126.2(3) . . ?
N5B Fe1B N10B 91.95(11) . . ?
N5B Fe1B N1B 160.00(10) . . ?
N5B Fe1B N6B 91.43(11) . . ?
N3B Fe1B N5B 80.14(11) . . ?
N3B Fe1B N10B 102.63(11) . . ?
N3B Fe1B N1B 79.96(11) . . ?
N3B Fe1B N8B 173.61(12) . . ?
N3B Fe1B N6B 97.70(11) . . ?
N1B Fe1B N10B 90.46(11) . . ?
N1B Fe1B N6B 93.18(11) . . ?
N8B Fe1B N5B 94.03(11) . . ?
N8B Fe1B N10B 80.04(11) . . ?
N8B Fe1B N1B 105.94(11) . . ?
N8B Fe1B N6B 79.73(11) . . ?
N6B Fe1B N10B 159.67(10) . . ?
C20B S2B C26B 104.66(15) . . ?
C6B S1B C12B 104.61(15) . . ?
N4B N5B Fe1B 112.9(2) . . ?
C11B N5B Fe1B 141.4(2) . . ?
C11B N5B N4B 105.5(3) . . ?
C4B N3B Fe1B 121.0(2) . . ?
C4B N3B C8B 118.7(3) . . ?
C8B N3B Fe1B 120.2(2) . . ?
N9B N10B Fe1B 111.82(19) . . ?
C25B N10B Fe1B 142.9(2) . . ?
C25B N10B N9B 105.2(2) . . ?
N2B N1B Fe1B 112.19(18) . . ?
C1B N1B Fe1B 142.4(2) . . ?
C1B N1B N2B 105.3(3) . . ?
N10B N9B C22B 116.8(2) . . ?
C23B N9B N10B 110.8(3) . . ?
C23B N9B C22B 132.3(3) . . ?
N5B N4B C8B 116.6(3) . . ?
C9B N4B N5B 110.5(3) . . ?
C9B N4B C8B 132.9(3) . . ?
N6B N7B C18B 116.2(3) . . ?
C17B N7B N6B 111.0(2) . . ?
C17B N7B C18B 132.3(3) . . ?
C18B N8B Fe1B 119.5(2) . . ?
C18B N8B C22B 118.9(3) . . ?
C22B N8B Fe1B 120.2(2) . . ?
N7B N6B Fe1B 112.24(19) . . ?
C15B N6B Fe1B 142.8(2) . . ?
C15B N6B N7B 104.9(3) . . ?
N1B N2B C4B 116.7(3) . . ?
C3B N2B N1B 110.7(2) . . ?
C3B N2B C4B 132.3(3) . . ?
N6B C15B H15B 124.3 . . ?
N6B C15B C16B 111.3(3) . . ?
C16B C15B H15B 124.3 . . ?
C21B C20B S2B 123.9(2) . . ?
C21B C20B C19B 120.7(3) . . ?
C19B C20B S2B 115.4(2) . . ?
H13D C13B H13E 109.5 . . ?
H13D C13B H13F 109.5 . . ?
H13E C13B H13F 109.5 . . ?
C12B C13B H13D 109.5 . . ?
C12B C13B H13E 109.5 . . ?
C12B C13B H13F 109.5 . . ?
C9B C10B H10B 127.0 . . ?
C9B C10B C11B 105.9(3) . . ?
C11B C10B H10B 127.0 . . ?
C6B C5B H5B 121.7 . . ?
C4B C5B H5B 121.7 . . ?
C4B C5B C6B 116.6(3) . . ?
C5B C6B S1B 115.7(3) . . ?
C7B C6B S1B 123.6(2) . . ?
C7B C6B C5B 120.6(3) . . ?
N8B C18B N7B 111.0(3) . . ?
N8B C18B C19B 123.0(3) . . ?
C19B C18B N7B 125.9(3) . . ?
N3B C4B N2B 109.9(3) . . ?
N3B C4B C5B 123.9(3) . . ?
C5B C4B N2B 126.2(3) . . ?
N4B C9B H9B 126.4 . . ?
C10B C9B N4B 107.2(3) . . ?
C10B C9B H9B 126.4 . . ?
S2B C26B H26B 109.4 . . ?
C28B C26B S2B 106.4(2) . . ?
C28B C26B H26B 109.4 . . ?
C27B C26B S2B 110.6(2) . . ?
C27B C26B H26B 109.4 . . ?
C27B C26B C28B 111.6(3) . . ?
N10B C25B H25B 124.5 . . ?
N10B C25B C24B 111.0(3) . . ?
C24B C25B H25B 124.5 . . ?
H14D C14B H14E 109.5 . . ?
H14D C14B H14F 109.5 . . ?
H14E C14B H14F 109.5 . . ?
C12B C14B H14D 109.5 . . ?
C12B C14B H14E 109.5 . . ?
C12B C14B H14F 109.5 . . ?
N5B C11B C10B 110.9(3) . . ?
N5B C11B H11B 124.6 . . ?
C10B C11B H11B 124.6 . . ?
C6B C7B H7B 121.6 . . ?
C8B C7B C6B 116.9(3) . . ?
C8B C7B H7B 121.6 . . ?
C3B C2B H2B 127.1 . . ?
C3B C2B C1B 105.8(3) . . ?
C1B C2B H2B 127.1 . . ?
N3B C8B N4B 110.1(3) . . ?
N3B C8B C7B 123.3(3) . . ?
C7B C8B N4B 126.5(3) . . ?
N2B C3B C2B 107.2(3) . . ?
N2B C3B H3B 126.4 . . ?
C2B C3B H3B 126.4 . . ?
N7B C17B H17B 126.5 . . ?
N7B C17B C16B 107.0(3) . . ?
C16B C17B H17B 126.5 . . ?
C20B C21B H21B 121.6 . . ?
C22B C21B C20B 116.7(3) . . ?
C22B C21B H21B 121.6 . . ?
N1B C1B C2B 111.0(3) . . ?
N1B C1B H1B 124.5 . . ?
C2B C1B H1B 124.5 . . ?
N9B C23B H23B 126.6 . . ?
N9B C23B C24B 106.7(3) . . ?
C24B C23B H23B 126.6 . . ?
C26B C28B H28D 109.5 . . ?
C26B C28B H28E 109.5 . . ?
C26B C28B H28F 109.5 . . ?
H28D C28B H28E 109.5 . . ?
H28D C28B H28F 109.5 . . ?
H28E C28B H28F 109.5 . . ?
C15B C16B H16B 127.2 . . ?
C17B C16B C15B 105.6(3) . . ?
C17B C16B H16B 127.2 . . ?
S1B C12B H12B 109.8 . . ?
C13B C12B S1B 105.8(2) . . ?
C13B C12B C14B 111.9(3) . . ?
C13B C12B H12B 109.8 . . ?
C14B C12B S1B 109.7(2) . . ?
C14B C12B H12B 109.8 . . ?
C25B C24B H24B 126.8 . . ?
C23B C24B C25B 106.3(3) . . ?
C23B C24B H24B 126.8 . . ?
C26B C27B H27D 109.5 . . ?
C26B C27B H27E 109.5 . . ?
C26B C27B H27F 109.5 . . ?
H27D C27B H27E 109.5 . . ?
H27D C27B H27F 109.5 . . ?
H27E C27B H27F 109.5 . . ?
C20B C19B H19B 121.4 . . ?
C18B C19B C20B 117.1(3) . . ?
C18B C19B H19B 121.4 . . ?
N8B C22B N9B 110.4(3) . . ?
N8B C22B C21B 123.5(3) . . ?
C21B C22B N9B 126.0(3) . . ?
N3C Fe1C N6C 102.59(11) . . ?
N3C Fe1C N5C 79.95(11) . . ?
N3C Fe1C N1C 79.85(11) . . ?
N3C Fe1C N10C 97.52(11) . . ?
N5C Fe1C N6C 92.00(11) . . ?
N5C Fe1C N1C 159.74(10) . . ?
N5C Fe1C N10C 91.22(11) . . ?
N1C Fe1C N6C 90.93(11) . . ?
N1C Fe1C N10C 92.89(11) . . ?
N8C Fe1C N6C 79.81(11) . . ?
N8C Fe1C N3C 176.74(12) . . ?
N8C Fe1C N5C 97.84(11) . . ?
N8C Fe1C N1C 102.41(11) . . ?
N8C Fe1C N10C 80.08(11) . . ?
N10C Fe1C N6C 159.88(10) . . ?
C6C S1C C12C 105.02(16) . . ?
C20C S2C C26C 104.97(15) . . ?
N7C N6C Fe1C 111.75(19) . . ?
C15C N6C Fe1C 143.1(2) . . ?
C15C N6C N7C 105.2(2) . . ?
C8C N3C Fe1C 120.2(2) . . ?
C8C N3C C4C 118.8(3) . . ?
C4C N3C Fe1C 120.7(2) . . ?
N4C N5C Fe1C 112.56(19) . . ?
C11C N5C Fe1C 142.5(2) . . ?
C11C N5C N4C 105.0(2) . . ?
N2C N1C Fe1C 112.84(18) . . ?
C1C N1C Fe1C 142.4(2) . . ?
C1C N1C N2C 104.8(3) . . ?
C22C N8C Fe1C 119.9(2) . . ?
C22C N8C C18C 118.9(3) . . ?
C18C N8C Fe1C 120.9(2) . . ?
N5C N4C C8C 116.3(2) . . ?
C9C N4C N5C 111.0(3) . . ?
C9C N4C C8C 132.5(3) . . ?
N6C N7C C18C 116.8(2) . . ?
C17C N7C N6C 110.5(3) . . ?
C17C N7C C18C 132.5(3) . . ?
N9C N10C Fe1C 111.87(19) . . ?
C25C N10C Fe1C 143.6(2) . . ?
C25C N10C N9C 104.5(3) . . ?
N10C N9C C22C 116.5(3) . . ?
C23C N9C N10C 111.2(2) . . ?
C23C N9C C22C 132.0(3) . . ?
N1C N2C C4C 116.1(3) . . ?
C3C N2C N1C 111.1(2) . . ?
C3C N2C C4C 132.8(3) . . ?
H13G C13C H13H 109.5 . . ?
H13G C13C H13I 109.5 . . ?
H13H C13C H13I 109.5 . . ?
C12C C13C H13G 109.5 . . ?
C12C C13C H13H 109.5 . . ?
C12C C13C H13I 109.5 . . ?
N8C C22C N9C 111.0(3) . . ?
N8C C22C C21C 123.2(3) . . ?
C21C C22C N9C 125.8(3) . . ?
N10C C25C H25C 124.2 . . ?
N10C C25C C24C 111.6(3) . . ?
C24C C25C H25C 124.2 . . ?
C9C C10C H10C 127.1 . . ?
C9C C10C C11C 105.8(3) . . ?
C11C C10C H10C 127.1 . . ?
S2C C26C H26C 109.5 . . ?
C27C C26C S2C 105.5(2) . . ?
C27C C26C H26C 109.5 . . ?
C27C C26C C28C 112.4(3) . . ?
C28C C26C S2C 110.4(2) . . ?
C28C C26C H26C 109.5 . . ?
N1C C1C H1C 124.3 . . ?
N1C C1C C2C 111.3(3) . . ?
C2C C1C H1C 124.3 . . ?
C26C C27C H27G 109.5 . . ?
C26C C27C H27H 109.5 . . ?
C26C C27C H27I 109.5 . . ?
H27G C27C H27H 109.5 . . ?
H27G C27C H27I 109.5 . . ?
H27H C27C H27I 109.5 . . ?
N8C C18C N7C 110.3(3) . . ?
N8C C18C C19C 123.0(3) . . ?
C19C C18C N7C 126.7(3) . . ?
C26C C28C H28G 109.5 . . ?
C26C C28C H28H 109.5 . . ?
C26C C28C H28I 109.5 . . ?
H28G C28C H28H 109.5 . . ?
H28G C28C H28I 109.5 . . ?
H28H C28C H28I 109.5 . . ?
C6C C5C H5C 121.7 . . ?
C4C C5C H5C 121.7 . . ?
C4C C5C C6C 116.6(3) . . ?
N6C C15C H15C 124.3 . . ?
N6C C15C C16C 111.5(3) . . ?
C16C C15C H15C 124.3 . . ?
C22C C21C H21C 121.3 . . ?
C22C C21C C20C 117.4(3) . . ?
C20C C21C H21C 121.3 . . ?
N4C C9C C10C 107.1(3) . . ?
N4C C9C H9C 126.4 . . ?
C10C C9C H9C 126.4 . . ?
N3C C8C N4C 110.7(3) . . ?
N3C C8C C7C 123.4(3) . . ?
C7C C8C N4C 125.9(3) . . ?
N9C C23C H23C 126.5 . . ?
N9C C23C C24C 107.0(3) . . ?
C24C C23C H23C 126.5 . . ?
C15C C16C H16C 127.0 . . ?
C17C C16C C15C 106.0(3) . . ?
C17C C16C H16C 127.0 . . ?
C21C C20C S2C 114.6(2) . . ?
C19C C20C S2C 125.0(2) . . ?
C19C C20C C21C 120.4(3) . . ?
N5C C11C C10C 111.1(3) . . ?
N5C C11C H11C 124.4 . . ?
C10C C11C H11C 124.4 . . ?
C25C C24C H24C 127.1 . . ?
C23C C24C C25C 105.7(3) . . ?
C23C C24C H24C 127.1 . . ?
C1C C2C H2C 127.1 . . ?
C3C C2C C1C 105.9(3) . . ?
C3C C2C H2C 127.1 . . ?
C8C C7C H7C 121.5 . . ?
C8C C7C C6C 117.0(3) . . ?
C6C C7C H7C 121.5 . . ?
N2C C3C C2C 106.9(3) . . ?
N2C C3C H3C 126.6 . . ?
C2C C3C H3C 126.6 . . ?
N7C C17C C16C 106.9(3) . . ?
N7C C17C H17C 126.6 . . ?
C16C C17C H17C 126.6 . . ?
C5C C6C S1C 114.9(2) . . ?
C7C C6C S1C 124.3(2) . . ?
C7C C6C C5C 120.9(3) . . ?
H14G C14C H14H 109.5 . . ?
H14G C14C H14I 109.5 . . ?
H14H C14C H14I 109.5 . . ?
C12C C14C H14G 109.5 . . ?
C12C C14C H14H 109.5 . . ?
C12C C14C H14I 109.5 . . ?
N3C C4C N2C 110.5(3) . . ?
N3C C4C C5C 123.3(3) . . ?
C5C C4C N2C 126.2(3) . . ?
S1C C12C H12C 109.3 . . ?
C13C C12C S1C 112.0(3) . . ?
C13C C12C C14C 112.0(3) . . ?
C13C C12C H12C 109.3 . . ?
C14C C12C S1C 104.9(2) . . ?
C14C C12C H12C 109.3 . . ?
C18C C19C C20C 117.1(3) . . ?
C18C C19C H19C 121.4 . . ?
C20C C19C H19C 121.4 . . ?
F1C B1C F4C 109.0(3) . . ?
F1C B1C F3C 109.5(3) . . ?
F1C B1C F2C 110.3(3) . . ?
F4C B1C F3C 109.1(3) . . ?
F2C B1C F4C 109.7(3) . . ?
F2C B1C F3C 109.3(3) . . ?
F6C B2C F5C 109.9(3) . . ?
F6C B2C F8C 109.1(3) . . ?
F7C B2C F6C 110.5(3) . . ?
F7C B2C F5C 108.7(3) . . ?
F7C B2C F8C 109.0(3) . . ?
F5C B2C F8C 109.6(3) . . ?
F2 B1 F4 109.7(3) . . ?
F2 B1 F3 109.5(3) . . ?
F4 B1 F3 108.7(3) . . ?
F1 B1 F2 109.3(3) . . ?
F1 B1 F4 109.7(3) . . ?
F1 B1 F3 110.0(3) . . ?
F7B B2B F8B 110.2(3) . . ?
F7B B2B F5B 110.1(3) . . ?
F7B B2B F6B 109.4(3) . . ?
F5B B2B F8B 108.9(3) . . ?
F5B B2B F6B 109.7(3) . . ?
F6B B2B F8B 108.5(3) . . ?
F5 B2 F7 108.9(3) . . ?
F5 B2 F6 109.6(3) . . ?
F5 B2 F8 111.2(3) . . ?
F6 B2 F7 110.5(3) . . ?
F6 B2 F8 108.8(3) . . ?
F8 B2 F7 107.8(3) . . ?
F2B B1B F4B 109.7(3) . . ?
F2B B1B F3B 110.5(3) . . ?
F2B B1B F1B 109.3(3) . . ?
F3B B1B F4B 109.2(3) . . ?
F3B B1B F1B 109.3(3) . . ?
F1B B1B F4B 108.7(3) . . ?
O1C N11C O2C 123.9(3) . . ?
O1C N11C C29C 117.7(3) . . ?
O2C N11C C29C 118.4(3) . . ?
N11C C29C H29A 109.5 . . ?
N11C C29C H29B 109.5 . . ?
N11C C29C H29C 109.5 . . ?
H29A C29C H29B 109.5 . . ?
H29A C29C H29C 109.5 . . ?
H29B C29C H29C 109.5 . . ?
O1B N11B C29B 119.3(3) . . ?
O2B N11B O1B 122.9(3) . . ?
O2B N11B C29B 117.8(3) . . ?
N11B C29B H29D 109.5 . . ?
N11B C29B H29E 109.5 . . ?
N11B C29B H29F 109.5 . . ?
H29D C29B H29E 109.5 . . ?
H29D C29B H29F 109.5 . . ?
H29E C29B H29F 109.5 . . ?
O2 N11 C29 116.9(3) . . ?
O1 N11 O2 124.4(3) . . ?
O1 N11 C29 118.6(3) . . ?
N11 C29 H29G 109.5 . . ?
N11 C29 H29H 109.5 . . ?
N11 C29 H29I 109.5 . . ?
H29G C29 H29H 109.5 . . ?
H29G C29 H29I 109.5 . . ?
H29H C29 H29I 109.5 . . ?


####################################################################### 
# 
# 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_rk137MeCN_085K
_database_code_depnum_ccdc_archive 'CCDC 1564667'
_audit_update_record             
;
2017-07-28 deposited with the CCDC.
2017-11-20 downloaded from the CCDC.
;
_chemical_name_common            ?
_chemical_name_systematic        ?
_chemical_formula_moiety         'C28 H30 Fe N10 S2, 2(B F4), C2 H3 N'
_chemical_formula_sum            'C30 H33 B2 F8 Fe N11 S2'
_chemical_formula_weight         841.26
_chemical_melting_point          'not measured'
loop_
_atom_type_symbol
_atom_type_description
_atom_type_scat_dispersion_real
_atom_type_scat_dispersion_imag
_atom_type_scat_source
C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
B B 0.0013 0.0007 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
F F 0.0171 0.0103 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Fe Fe 0.3463 0.8444 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
S S 0.1246 0.1234 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'

_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.
;
_space_group_crystal_system      monoclinic
_space_group_IT_number           14
_space_group_name_H-M_alt        'P 1 21/c 1'
_space_group_name_Hall           '-P 2ybc'
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                   19.5906(3)
_cell_length_b                   12.3086(2)
_cell_length_c                   15.6311(2)
_cell_angle_alpha                90
_cell_angle_beta                 100.6220(10)
_cell_angle_gamma                90
_cell_volume                     3704.59(10)
_cell_formula_units_Z            4
_cell_measurement_reflns_used    10817
_cell_measurement_temperature    85
_cell_measurement_theta_max      32.8780
_cell_measurement_theta_min      3.2150
_exptl_absorpt_coefficient_mu    0.600
_exptl_absorpt_correction_T_max  0.951
_exptl_absorpt_correction_T_min  0.816
_exptl_absorpt_correction_type   analytical
_exptl_absorpt_process_details   
;
CrysAlisPro 1.171.38.46 (Rigaku Oxford Diffraction, 2015)
Analytical numeric absorption correction using a multifaceted crystal
			model based on expressions derived by R.C. Clark & J.S. Reid.
(Clark, R. C. & Reid, J. S. (1995). Acta Cryst. A51, 887-897)
Empirical absorption correction using spherical harmonics,
 implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_absorpt_special_details   ?
_exptl_crystal_colour            'dark orange'
_exptl_crystal_density_diffrn    1.508
_exptl_crystal_density_meas      'not measured'
_exptl_crystal_density_method    none
_exptl_crystal_description       block
_exptl_crystal_F_000             1720
loop_
_exptl_crystal_face_index_h
_exptl_crystal_face_index_k
_exptl_crystal_face_index_l
_exptl_crystal_face_perp_dist
0 13 19 0.0406
1 -8 24 0.0296
-19 -9 4 0.2116
16 2 14 0.1760
-14 -5 -17 0.1774
0 -13 -19 0.0598
-1 8 -24 0.0739
-19 7 -2 0.2306
19 9 -4 0.1976
9 8 19 0.1207
19 -8 1 0.2081

_exptl_crystal_size_max          0.508
_exptl_crystal_size_mid          0.138
_exptl_crystal_size_min          0.1
loop_
_exptl_oxdiff_crystal_face_indexfrac_h
_exptl_oxdiff_crystal_face_indexfrac_k
_exptl_oxdiff_crystal_face_indexfrac_l
_exptl_oxdiff_crystal_face_x
_exptl_oxdiff_crystal_face_y
_exptl_oxdiff_crystal_face_z
-0.2380 12.5496 19.1456 -0.8349 0.1970 0.5314
0.7934 -8.1489 24.2633 -0.1896 -0.8260 0.5608
-18.9884 -9.3755 4.2140 -0.1576 -0.7091 -0.7115
15.8377 2.2150 14.2824 -0.0330 -0.0038 0.9842
-13.7987 -5.3339 -17.1590 0.2441 -0.0600 -0.9928
0.2380 -12.5496 -19.1456 0.8349 -0.1970 -0.5314
-0.7934 8.1489 -24.2633 0.1896 0.8260 -0.5608
-18.9951 7.1751 -1.8216 -0.6169 0.1550 -0.7493
18.9884 9.3755 -4.2140 0.1576 0.7091 0.7115
8.7714 8.4364 19.1033 -0.4989 0.1088 0.8605
19.0086 -8.2172 0.8703 0.6731 -0.1837 0.7203

_exptl_transmission_factor_max   ?
_exptl_transmission_factor_min   ?
_diffrn_reflns_av_R_equivalents  0.0334
_diffrn_reflns_av_unetI/netI     0.0286
_diffrn_reflns_Laue_measured_fraction_full 0.998
_diffrn_reflns_Laue_measured_fraction_max 0.998
_diffrn_reflns_limit_h_max       24
_diffrn_reflns_limit_h_min       -25
_diffrn_reflns_limit_k_max       15
_diffrn_reflns_limit_k_min       -15
_diffrn_reflns_limit_l_max       19
_diffrn_reflns_limit_l_min       -19
_diffrn_reflns_number            34450
_diffrn_reflns_point_group_measured_fraction_full 0.998
_diffrn_reflns_point_group_measured_fraction_max 0.998
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         26.995
_diffrn_reflns_theta_min         3.073
_diffrn_ambient_temperature      85.0
_diffrn_detector                 'CCD plate'
_diffrn_detector_area_resol_mean 16.1852
_diffrn_detector_type            Sapphire3
_diffrn_measured_fraction_theta_full 0.998
_diffrn_measured_fraction_theta_max 0.998
_diffrn_measurement_details      
;
List of Runs (angles in degrees, time in seconds):

  # Type    Start    End  Width  tₑₓₚ   ω     θ     κ     φ   Frames
#--------------------------------------------------------------------------
  1  ω   -103.00 -70.00   1.00   30.00    --  -30.39 -77.00 -30.00   33
  2  ω   -113.00 -87.00   1.00   30.00    --  -30.39 178.00 150.00   26
  3  ω     50.00 110.00   1.00   30.00    --   32.43 178.00  30.00   60
  4  ω    -25.00  71.00   1.00   30.00    --   32.43 -99.00   0.00   96
  5  ω     27.00  77.00   1.00   30.00    --   32.43 -99.00 120.00   50
  6  ω     20.00 100.00   1.00   30.00    --   32.43  57.00-120.00   80
  7  ω     33.00 102.00   1.00   30.00    --   32.43  57.00-180.00   69
  8  ω     15.00 102.00   1.00   30.00    --   32.43  38.00 120.00   87
  9  ω    -38.00   5.00   1.00   30.00    --   32.43 -57.00  30.00   43
;
_diffrn_measurement_device       'four-circle diffractometer'
_diffrn_measurement_device_type  'Xcalibur, Sapphire3'
_diffrn_measurement_method       'ω scans'
_diffrn_orient_matrix_type       
'CrysAlisPro convention (1999,Acta A55,543-557)'
_diffrn_orient_matrix_UB_11      0.0211473000
_diffrn_orient_matrix_UB_12      -0.0351437000
_diffrn_orient_matrix_UB_13      -0.0203076000
_diffrn_orient_matrix_UB_21      0.0107594000
_diffrn_orient_matrix_UB_22      0.0452121000
_diffrn_orient_matrix_UB_23      -0.0192119000
_diffrn_orient_matrix_UB_31      0.0395960000
_diffrn_orient_matrix_UB_32      0.0064860000
_diffrn_orient_matrix_UB_33      0.0239988000
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_source                   'fine-focus sealed X-ray tube'
_diffrn_source_type              'Enhance (Mo) X-ray Source'
_reflns_Friedel_coverage         0.000
_reflns_Friedel_fraction_full    .
_reflns_Friedel_fraction_max     .
_reflns_number_gt                6739
_reflns_number_total             8066
_reflns_odcompleteness_completeness 99.85
_reflns_odcompleteness_iscentric 1
_reflns_odcompleteness_theta     31.44
_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.
;
_reflns_threshold_expression     'I > 2σ(I)'
_computing_cell_refinement       'CrysAlisPro 1.171.38.46 (Rigaku OD, 2015)'
_computing_data_collection       'CrysAlisPro 1.171.37.31c (Rigaku OD, 2014)'
_computing_data_reduction        'CrysAlisPro 1.171.38.46 (Rigaku OD, 2015)'
_computing_molecular_graphics    'Mercury3.9 (2016)'
_computing_publication_material  'Olex2 (Dolomanov et al., 2009)'
_computing_structure_refinement  'ShelXL (Sheldrick, 2015)'
_computing_structure_solution    'ShelXT (Sheldrick, 2015)'
_refine_diff_density_max         0.490
_refine_diff_density_min         -0.410
_refine_diff_density_rms         0.056
_refine_ls_extinction_coef       .
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.035
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     520
_refine_ls_number_reflns         8066
_refine_ls_number_restraints     0
_refine_ls_R_factor_all          0.0456
_refine_ls_R_factor_gt           0.0336
_refine_ls_restrained_S_all      1.035
_refine_ls_shift/su_max          0.001
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details     
'w=1/[σ²(Fo²)+(0.0308P)²+2.5668P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0737
_refine_ls_wR_factor_ref         0.0791
_refine_special_details          
;
Structure of low temperature low spin state.
;
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     dual
_atom_sites_solution_secondary   difmap
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 0.72421(2) 0.38032(2) 0.56686(2) 0.01476(7) Uani 1 1 d . . . . .
S1 S 0.39775(2) 0.29184(4) 0.50363(3) 0.02130(11) Uani 1 1 d . . . . .
S2 S 1.04005(2) 0.49719(4) 0.72392(3) 0.02672(12) Uani 1 1 d . . . . .
F1 F 0.62744(5) 0.52929(11) 0.22463(7) 0.0314(3) Uani 1 1 d . . . . .
F4 F 0.56045(5) 0.44648(10) 0.30877(7) 0.0259(2) Uani 1 1 d . . . . .
F3 F 0.51007(6) 0.55821(10) 0.19832(8) 0.0318(3) Uani 1 1 d . . . . .
F2 F 0.55393(6) 0.39380(11) 0.16781(8) 0.0353(3) Uani 1 1 d . . . . .
F8 F 0.91688(7) 0.36644(11) 0.44630(8) 0.0387(3) Uani 1 1 d . . . . .
F6 F 1.0244(4) 0.2859(15) 0.4997(15) 0.051(4) Uani 0.52(4) 1 d . . P A 2
F7 F 0.9271(8) 0.2359(14) 0.5503(10) 0.037(2) Uani 0.52(4) 1 d . . P A 2
N7 N 0.81114(7) 0.52873(13) 0.50201(9) 0.0167(3) Uani 1 1 d . . . . .
N8 N 0.82048(7) 0.40341(12) 0.60807(9) 0.0156(3) Uani 1 1 d . . . . .
N2 N 0.65150(7) 0.23375(13) 0.44404(9) 0.0168(3) Uani 1 1 d . . . . .
N3 N 0.62661(7) 0.36038(12) 0.53713(9) 0.0153(3) Uani 1 1 d . . . . .
F5 F 0.9397(9) 0.1918(7) 0.4151(5) 0.0382(19) Uani 0.52(4) 1 d . . P A 2
N9 N 0.80868(7) 0.27432(13) 0.70615(9) 0.0176(3) Uani 1 1 d . . . . .
N6 N 0.74319(7) 0.49191(12) 0.48391(9) 0.0161(3) Uani 1 1 d . . . . .
N4 N 0.62286(7) 0.48725(12) 0.64069(10) 0.0176(3) Uani 1 1 d . . . . .
N1 N 0.71939(7) 0.26276(12) 0.47907(9) 0.0165(3) Uani 1 1 d . . . . .
N5 N 0.69347(7) 0.49012(12) 0.64301(9) 0.0171(3) Uani 1 1 d . . . . .
N10 N 0.74092(7) 0.27279(13) 0.66105(9) 0.0177(3) Uani 1 1 d . . . . .
C22 C 0.85302(9) 0.35095(15) 0.67867(11) 0.0164(3) Uani 1 1 d . . . . .
C7 C 0.51514(9) 0.39293(15) 0.57282(11) 0.0185(4) Uani 1 1 d . . . . .
H7 H 0.4869 0.4314 0.6058 0.022 Uiso 1 1 calc R . . . .
C8 C 0.58471(9) 0.41345(15) 0.58213(11) 0.0166(4) Uani 1 1 d . . . . .
C4 C 0.59927(9) 0.28405(15) 0.48051(11) 0.0163(4) Uani 1 1 d . . . . .
C18 C 0.85444(9) 0.48160(15) 0.57391(11) 0.0163(4) Uani 1 1 d . . . . .
C6 C 0.48707(9) 0.31260(15) 0.51245(11) 0.0180(4) Uani 1 1 d . . . . .
C3 C 0.65000(9) 0.15146(15) 0.38607(11) 0.0199(4) Uani 1 1 d . . . . .
H3 H 0.6097 0.1179 0.3537 0.024 Uiso 1 1 calc R . . . .
C5 C 0.52966(8) 0.25701(15) 0.46426(11) 0.0174(4) Uani 1 1 d . . . . .
H5 H 0.5115 0.2034 0.4225 0.021 Uiso 1 1 calc R . . . .
C21 C 0.92045(9) 0.37258(16) 0.71848(11) 0.0191(4) Uani 1 1 d . . . . .
H21 H 0.9422 0.3338 0.7687 0.023 Uiso 1 1 calc R . . . .
C1 C 0.75831(9) 0.19710(15) 0.44157(12) 0.0193(4) Uani 1 1 d . . . . .
H1 H 0.8076 0.1978 0.4527 0.023 Uiso 1 1 calc R . . . .
C23 C 0.81940(9) 0.19391(16) 0.76669(12) 0.0208(4) Uani 1 1 d . . . . .
H23 H 0.8616 0.1785 0.8056 0.025 Uiso 1 1 calc R . . . .
C19 C 0.92194(9) 0.51029(15) 0.60735(11) 0.0191(4) Uani 1 1 d . . . . .
H19 H 0.9449 0.5658 0.5813 0.023 Uiso 1 1 calc R . . . .
C15 C 0.71372(9) 0.54623(15) 0.41376(11) 0.0176(4) Uani 1 1 d . . . . .
H15 H 0.6666 0.5381 0.3859 0.021 Uiso 1 1 calc R . . . .
C9 C 0.60360(9) 0.56279(16) 0.69505(12) 0.0214(4) Uani 1 1 d . . . . .
H9 H 0.5577 0.5766 0.7041 0.026 Uiso 1 1 calc R . . . .
C17 C 0.82262(9) 0.60462(15) 0.44318(12) 0.0201(4) Uani 1 1 d . . . . .
H17 H 0.8650 0.6416 0.4419 0.024 Uiso 1 1 calc R . . . .
C20 C 0.95549(9) 0.45418(16) 0.68153(11) 0.0194(4) Uani 1 1 d . . . . .
C12 C 0.38006(9) 0.16309(16) 0.44622(12) 0.0215(4) Uani 1 1 d . . . . .
H12 H 0.3998 0.1648 0.3917 0.026 Uiso 1 1 calc R . . . .
C11 C 0.71698(9) 0.56737(16) 0.69936(12) 0.0209(4) Uani 1 1 d . . . . .
H11 H 0.7644 0.5882 0.7145 0.025 Uiso 1 1 calc R . . . .
C2 C 0.71735(9) 0.12592(16) 0.38301(12) 0.0223(4) Uani 1 1 d . . . . .
H2 H 0.7333 0.0713 0.3485 0.027 Uiso 1 1 calc R . . . .
C24 C 0.75816(10) 0.13959(16) 0.76097(12) 0.0235(4) Uani 1 1 d . . . . .
H24 H 0.7492 0.0790 0.7949 0.028 Uiso 1 1 calc R . . . .
C25 C 0.71080(9) 0.19109(16) 0.69476(12) 0.0201(4) Uani 1 1 d . . . . .
H25 H 0.6637 0.1701 0.6767 0.024 Uiso 1 1 calc R . . . .
C10 C 0.66255(10) 0.61501(16) 0.73413(12) 0.0237(4) Uani 1 1 d . . . . .
H10 H 0.6662 0.6716 0.7760 0.028 Uiso 1 1 calc R . . . .
C16 C 0.76117(9) 0.61735(16) 0.38596(12) 0.0207(4) Uani 1 1 d . . . . .
H16 H 0.7524 0.6648 0.3372 0.025 Uiso 1 1 calc R . . . .
C26 C 1.07086(9) 0.40687(17) 0.81556(12) 0.0246(4) Uani 1 1 d . . . . .
H26 H 1.0327 0.3959 0.8493 0.029 Uiso 1 1 calc R . . . .
C14 C 0.30108(10) 0.15436(18) 0.42295(14) 0.0299(5) Uani 1 1 d . . . . .
H14A H 0.2816 0.1551 0.4764 0.045 Uiso 1 1 calc GR . . . .
H14B H 0.2883 0.0864 0.3914 0.045 Uiso 1 1 calc GR . . . .
H14C H 0.2826 0.2160 0.3862 0.045 Uiso 1 1 calc GR . . . .
C13 C 0.41132(10) 0.06868(17) 0.50261(13) 0.0276(4) Uani 1 1 d . . . . .
H13A H 0.4614 0.0799 0.5205 0.041 Uiso 1 1 calc GR . . . .
H13B H 0.4029 0.0009 0.4694 0.041 Uiso 1 1 calc GR . . . .
H13C H 0.3898 0.0642 0.5544 0.041 Uiso 1 1 calc GR . . . .
C29 C 0.86877(12) 0.60297(18) 0.89059(14) 0.0330(5) Uani 1 1 d . . . . .
C27 C 1.09284(12) 0.2974(2) 0.78582(17) 0.0403(6) Uani 1 1 d . . . . .
H27A H 1.0534 0.2630 0.7479 0.060 Uiso 1 1 calc GR . . . .
H27B H 1.1085 0.2511 0.8366 0.060 Uiso 1 1 calc GR . . . .
H27C H 1.1309 0.3073 0.7537 0.060 Uiso 1 1 calc GR . . . .
N11 N 0.81312(11) 0.63407(18) 0.87219(14) 0.0483(6) Uani 1 1 d . . . . .
C28 C 1.13059(10) 0.4677(2) 0.87254(14) 0.0333(5) Uani 1 1 d . . . . .
H28A H 1.1668 0.4834 0.8386 0.050 Uiso 1 1 calc GR . . . .
H28B H 1.1500 0.4228 0.9229 0.050 Uiso 1 1 calc GR . . . .
H28C H 1.1132 0.5360 0.8926 0.050 Uiso 1 1 calc GR . . . .
B1 B 0.56311(11) 0.4822(2) 0.22380(14) 0.0239(5) Uani 1 1 d . . . . .
B2 B 0.95352(11) 0.2752(2) 0.48068(14) 0.0251(5) Uani 1 1 d . . . . .
C30 C 0.93887(12) 0.5624(2) 0.91575(18) 0.0456(6) Uani 1 1 d . . . . .
H30A H 0.9664 0.5842 0.8722 0.068 Uiso 1 1 calc GR . . . .
H30B H 0.9379 0.4829 0.9195 0.068 Uiso 1 1 calc GR . . . .
H30C H 0.9598 0.5926 0.9726 0.068 Uiso 1 1 calc GR . . . .
F6A F 1.0170(5) 0.3161(10) 0.5263(6) 0.0343(16) Uani 0.48(4) 1 d . . P A 1
F5A F 0.9640(10) 0.2132(16) 0.4140(6) 0.050(3) Uani 0.48(4) 1 d . . P A 1
F7A F 0.9217(8) 0.2224(17) 0.5385(13) 0.043(3) Uani 0.48(4) 1 d . . P A 1


_geom_special_details            
;
 All esds (except the esd in the dihedral angle between two l.s. planes)
 are estimated using the full covariance matrix.  The cell esds are taken
 into account individually in the estimation of esds in distances, angles
 and torsion angles; correlations between esds in cell parameters are only
 used when they are defined by crystal symmetry.  An approximate (isotropic)
 treatment of cell esds is used for estimating esds involving l.s. planes.
;
loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
_geom_bond_publ_flag
Fe1 N8 1.8986(14) . ?
Fe1 N3 1.8987(14) . ?
Fe1 N6 1.9706(15) . ?
Fe1 N1 1.9845(15) . ?
Fe1 N5 1.9673(15) . ?
Fe1 N10 1.9619(15) . ?
S1 C6 1.7486(17) . ?
S1 C12 1.8226(19) . ?
S2 C20 1.7491(17) . ?
S2 C26 1.8257(19) . ?
F1 B1 1.385(2) . ?
F4 B1 1.409(2) . ?
F3 B1 1.400(2) . ?
F2 B1 1.388(3) . ?
F8 B2 1.386(3) . ?
F6 B2 1.372(7) . ?
F7 B2 1.377(17) . ?
N7 N6 1.3852(19) . ?
N7 C18 1.403(2) . ?
N7 C17 1.358(2) . ?
N8 C22 1.335(2) . ?
N8 C18 1.336(2) . ?
N2 N1 1.3885(19) . ?
N2 C4 1.404(2) . ?
N2 C3 1.356(2) . ?
N3 C8 1.345(2) . ?
N3 C4 1.333(2) . ?
F5 B2 1.441(9) . ?
N9 N10 1.3835(19) . ?
N9 C22 1.402(2) . ?
N9 C23 1.359(2) . ?
N6 C15 1.323(2) . ?
N4 N5 1.3775(19) . ?
N4 C8 1.403(2) . ?
N4 C9 1.359(2) . ?
N1 C1 1.320(2) . ?
N5 C11 1.320(2) . ?
N10 C25 1.324(2) . ?
C22 C21 1.378(2) . ?
C7 H7 0.9500 . ?
C7 C8 1.367(2) . ?
C7 C6 1.407(3) . ?
C4 C5 1.381(2) . ?
C18 C19 1.375(2) . ?
C6 C5 1.401(2) . ?
C3 H3 0.9500 . ?
C3 C2 1.366(3) . ?
C5 H5 0.9500 . ?
C21 H21 0.9500 . ?
C21 C20 1.400(3) . ?
C1 H1 0.9500 . ?
C1 C2 1.407(3) . ?
C23 H23 0.9500 . ?
C23 C24 1.362(3) . ?
C19 H19 0.9500 . ?
C19 C20 1.404(3) . ?
C15 H15 0.9500 . ?
C15 C16 1.403(3) . ?
C9 H9 0.9500 . ?
C9 C10 1.364(3) . ?
C17 H17 0.9500 . ?
C17 C16 1.370(2) . ?
C12 H12 1.0000 . ?
C12 C14 1.526(2) . ?
C12 C13 1.518(3) . ?
C11 H11 0.9500 . ?
C11 C10 1.411(3) . ?
C2 H2 0.9500 . ?
C24 H24 0.9500 . ?
C24 C25 1.407(3) . ?
C25 H25 0.9500 . ?
C10 H10 0.9500 . ?
C16 H16 0.9500 . ?
C26 H26 1.0000 . ?
C26 C27 1.513(3) . ?
C26 C28 1.530(3) . ?
C14 H14A 0.9800 . ?
C14 H14B 0.9800 . ?
C14 H14C 0.9800 . ?
C13 H13A 0.9800 . ?
C13 H13B 0.9800 . ?
C13 H13C 0.9800 . ?
C29 N11 1.141(3) . ?
C29 C30 1.446(3) . ?
C27 H27A 0.9800 . ?
C27 H27B 0.9800 . ?
C27 H27C 0.9800 . ?
C28 H28A 0.9800 . ?
C28 H28B 0.9800 . ?
C28 H28C 0.9800 . ?
B2 F6A 1.408(7) . ?
B2 F5A 1.339(10) . ?
B2 F7A 1.355(19) . ?
C30 H30A 0.9800 . ?
C30 H30B 0.9800 . ?
C30 H30C 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 N6 79.80(6) . . ?
N8 Fe1 N1 105.15(6) . . ?
N8 Fe1 N5 95.03(6) . . ?
N8 Fe1 N10 80.12(6) . . ?
N3 Fe1 N8 174.26(6) . . ?
N3 Fe1 N6 103.46(6) . . ?
N3 Fe1 N1 79.57(6) . . ?
N3 Fe1 N5 80.22(6) . . ?
N3 Fe1 N10 96.76(6) . . ?
N6 Fe1 N1 92.52(6) . . ?
N5 Fe1 N6 92.02(6) . . ?
N5 Fe1 N1 159.79(6) . . ?
N10 Fe1 N6 159.78(6) . . ?
N10 Fe1 N1 90.41(6) . . ?
N10 Fe1 N5 92.10(6) . . ?
C6 S1 C12 105.23(9) . . ?
C20 S2 C26 105.43(9) . . ?
N6 N7 C18 116.41(14) . . ?
C17 N7 N6 111.07(14) . . ?
C17 N7 C18 132.51(15) . . ?
C22 N8 Fe1 120.08(12) . . ?
C22 N8 C18 118.80(14) . . ?
C18 N8 Fe1 120.59(12) . . ?
N1 N2 C4 116.32(14) . . ?
C3 N2 N1 110.91(14) . . ?
C3 N2 C4 132.33(15) . . ?
C8 N3 Fe1 119.57(11) . . ?
C4 N3 Fe1 121.11(12) . . ?
C4 N3 C8 118.70(14) . . ?
N10 N9 C22 116.32(14) . . ?
C23 N9 N10 110.84(14) . . ?
C23 N9 C22 132.71(15) . . ?
N7 N6 Fe1 112.61(10) . . ?
C15 N6 Fe1 142.31(12) . . ?
C15 N6 N7 105.08(14) . . ?
N5 N4 C8 116.44(14) . . ?
C9 N4 N5 111.05(14) . . ?
C9 N4 C8 132.43(15) . . ?
N2 N1 Fe1 112.35(10) . . ?
C1 N1 Fe1 142.72(12) . . ?
C1 N1 N2 104.90(14) . . ?
N4 N5 Fe1 112.60(11) . . ?
C11 N5 Fe1 142.23(12) . . ?
C11 N5 N4 105.15(14) . . ?
N9 N10 Fe1 112.64(11) . . ?
C25 N10 Fe1 141.84(12) . . ?
C25 N10 N9 105.30(14) . . ?
N8 C22 N9 110.50(14) . . ?
N8 C22 C21 123.48(16) . . ?
C21 C22 N9 126.00(16) . . ?
C8 C7 H7 121.3 . . ?
C8 C7 C6 117.38(16) . . ?
C6 C7 H7 121.3 . . ?
N3 C8 N4 110.64(14) . . ?
N3 C8 C7 123.18(16) . . ?
C7 C8 N4 126.13(16) . . ?
N3 C4 N2 110.29(14) . . ?
N3 C4 C5 123.64(16) . . ?
C5 C4 N2 126.02(16) . . ?
N8 C18 N7 110.24(14) . . ?
N8 C18 C19 123.22(16) . . ?
C19 C18 N7 126.54(16) . . ?
C7 C6 S1 114.67(13) . . ?
C5 C6 S1 124.93(14) . . ?
C5 C6 C7 120.39(15) . . ?
N2 C3 H3 126.5 . . ?
N2 C3 C2 107.05(16) . . ?
C2 C3 H3 126.5 . . ?
C4 C5 C6 116.68(16) . . ?
C4 C5 H5 121.7 . . ?
C6 C5 H5 121.7 . . ?
C22 C21 H21 121.5 . . ?
C22 C21 C20 117.02(16) . . ?
C20 C21 H21 121.5 . . ?
N1 C1 H1 124.3 . . ?
N1 C1 C2 111.31(15) . . ?
C2 C1 H1 124.3 . . ?
N9 C23 H23 126.6 . . ?
N9 C23 C24 106.89(16) . . ?
C24 C23 H23 126.6 . . ?
C18 C19 H19 121.4 . . ?
C18 C19 C20 117.28(17) . . ?
C20 C19 H19 121.4 . . ?
N6 C15 H15 124.5 . . ?
N6 C15 C16 111.06(15) . . ?
C16 C15 H15 124.5 . . ?
N4 C9 H9 126.5 . . ?
N4 C9 C10 107.02(16) . . ?
C10 C9 H9 126.5 . . ?
N7 C17 H17 126.7 . . ?
N7 C17 C16 106.59(16) . . ?
C16 C17 H17 126.7 . . ?
C21 C20 S2 124.27(14) . . ?
C21 C20 C19 120.19(16) . . ?
C19 C20 S2 115.49(14) . . ?
S1 C12 H12 109.5 . . ?
C14 C12 S1 105.71(13) . . ?
C14 C12 H12 109.5 . . ?
C13 C12 S1 111.10(13) . . ?
C13 C12 H12 109.5 . . ?
C13 C12 C14 111.55(16) . . ?
N5 C11 H11 124.4 . . ?
N5 C11 C10 111.15(16) . . ?
C10 C11 H11 124.4 . . ?
C3 C2 C1 105.83(16) . . ?
C3 C2 H2 127.1 . . ?
C1 C2 H2 127.1 . . ?
C23 C24 H24 126.8 . . ?
C23 C24 C25 106.30(17) . . ?
C25 C24 H24 126.8 . . ?
N10 C25 C24 110.68(16) . . ?
N10 C25 H25 124.7 . . ?
C24 C25 H25 124.7 . . ?
C9 C10 C11 105.62(17) . . ?
C9 C10 H10 127.2 . . ?
C11 C10 H10 127.2 . . ?
C15 C16 H16 126.9 . . ?
C17 C16 C15 106.20(16) . . ?
C17 C16 H16 126.9 . . ?
S2 C26 H26 108.9 . . ?
C27 C26 S2 111.88(15) . . ?
C27 C26 H26 108.9 . . ?
C27 C26 C28 112.60(17) . . ?
C28 C26 S2 105.39(14) . . ?
C28 C26 H26 108.9 . . ?
C12 C14 H14A 109.5 . . ?
C12 C14 H14B 109.5 . . ?
C12 C14 H14C 109.5 . . ?
H14A C14 H14B 109.5 . . ?
H14A C14 H14C 109.5 . . ?
H14B C14 H14C 109.5 . . ?
C12 C13 H13A 109.5 . . ?
C12 C13 H13B 109.5 . . ?
C12 C13 H13C 109.5 . . ?
H13A C13 H13B 109.5 . . ?
H13A C13 H13C 109.5 . . ?
H13B C13 H13C 109.5 . . ?
N11 C29 C30 178.6(3) . . ?
C26 C27 H27A 109.5 . . ?
C26 C27 H27B 109.5 . . ?
C26 C27 H27C 109.5 . . ?
H27A C27 H27B 109.5 . . ?
H27A C27 H27C 109.5 . . ?
H27B C27 H27C 109.5 . . ?
C26 C28 H28A 109.5 . . ?
C26 C28 H28B 109.5 . . ?
C26 C28 H28C 109.5 . . ?
H28A C28 H28B 109.5 . . ?
H28A C28 H28C 109.5 . . ?
H28B C28 H28C 109.5 . . ?
F1 B1 F4 108.27(15) . . ?
F1 B1 F3 110.48(18) . . ?
F1 B1 F2 110.24(16) . . ?
F3 B1 F4 108.80(16) . . ?
F2 B1 F4 109.05(18) . . ?
F2 B1 F3 109.96(16) . . ?
F8 B2 F5 106.6(5) . . ?
F8 B2 F6A 104.7(5) . . ?
F6 B2 F8 116.0(5) . . ?
F6 B2 F7 112.1(8) . . ?
F6 B2 F5 105.8(6) . . ?
F7 B2 F8 110.4(7) . . ?
F7 B2 F5 105.3(7) . . ?
F5A B2 F8 107.6(5) . . ?
F5A B2 F6A 110.4(5) . . ?
F5A B2 F7A 113.7(9) . . ?
F7A B2 F8 112.2(8) . . ?
F7A B2 F6A 107.9(8) . . ?
C29 C30 H30A 109.5 . . ?
C29 C30 H30B 109.5 . . ?
C29 C30 H30C 109.5 . . ?
H30A C30 H30B 109.5 . . ?
H30A C30 H30C 109.5 . . ?
H30B C30 H30C 109.5 . . ?

loop_
_geom_torsion_atom_site_label_1
_geom_torsion_atom_site_label_2
_geom_torsion_atom_site_label_3
_geom_torsion_atom_site_label_4
_geom_torsion
_geom_torsion_site_symmetry_1
_geom_torsion_site_symmetry_2
_geom_torsion_site_symmetry_3
_geom_torsion_site_symmetry_4
_geom_torsion_publ_flag
Fe1 N8 C22 N9 6.7(2) . . . . ?
Fe1 N8 C22 C21 -172.12(14) . . . . ?
Fe1 N8 C18 N7 -6.7(2) . . . . ?
Fe1 N8 C18 C19 172.44(14) . . . . ?
Fe1 N3 C8 N4 6.5(2) . . . . ?
Fe1 N3 C8 C7 -171.03(14) . . . . ?
Fe1 N3 C4 N2 -5.5(2) . . . . ?
Fe1 N3 C4 C5 171.92(14) . . . . ?
Fe1 N6 C15 C16 -179.07(15) . . . . ?
Fe1 N1 C1 C2 177.44(15) . . . . ?
Fe1 N5 C11 C10 -177.86(15) . . . . ?
Fe1 N10 C25 C24 173.65(15) . . . . ?
S1 C6 C5 C4 -179.65(14) . . . . ?
N7 N6 C15 C16 0.08(19) . . . . ?
N7 C18 C19 C20 178.36(17) . . . . ?
N7 C17 C16 C15 0.0(2) . . . . ?
N8 C22 C21 C20 -0.1(3) . . . . ?
N8 C18 C19 C20 -0.6(3) . . . . ?
N2 N1 C1 C2 -0.1(2) . . . . ?
N2 C4 C5 C6 175.53(16) . . . . ?
N2 C3 C2 C1 -0.2(2) . . . . ?
N3 C4 C5 C6 -1.5(3) . . . . ?
N9 N10 C25 C24 -0.1(2) . . . . ?
N9 C22 C21 C20 -178.69(17) . . . . ?
N9 C23 C24 C25 -0.1(2) . . . . ?
N6 Fe1 N8 C22 177.22(14) . . . . ?
N6 Fe1 N8 C18 5.64(13) . . . . ?
N6 Fe1 N3 C8 -96.66(13) . . . . ?
N6 Fe1 N3 C4 92.45(14) . . . . ?
N6 N7 C18 N8 3.7(2) . . . . ?
N6 N7 C18 C19 -175.38(17) . . . . ?
N6 N7 C17 C16 0.0(2) . . . . ?
N6 C15 C16 C17 -0.1(2) . . . . ?
N4 N5 C11 C10 0.1(2) . . . . ?
N4 C9 C10 C11 0.7(2) . . . . ?
N1 Fe1 N8 C22 -92.92(14) . . . . ?
N1 Fe1 N8 C18 95.50(14) . . . . ?
N1 Fe1 N3 C8 173.22(14) . . . . ?
N1 Fe1 N3 C4 2.34(13) . . . . ?
N1 N2 C4 N3 6.7(2) . . . . ?
N1 N2 C4 C5 -170.68(16) . . . . ?
N1 N2 C3 C2 0.1(2) . . . . ?
N1 C1 C2 C3 0.1(2) . . . . ?
N5 Fe1 N8 C22 86.07(14) . . . . ?
N5 Fe1 N8 C18 -85.51(14) . . . . ?
N5 Fe1 N3 C8 -6.92(13) . . . . ?
N5 Fe1 N3 C4 -177.81(14) . . . . ?
N5 N4 C8 N3 -1.5(2) . . . . ?
N5 N4 C8 C7 176.03(17) . . . . ?
N5 N4 C9 C10 -0.6(2) . . . . ?
N5 C11 C10 C9 -0.5(2) . . . . ?
N10 Fe1 N8 C22 -5.19(13) . . . . ?
N10 Fe1 N8 C18 -176.77(14) . . . . ?
N10 Fe1 N3 C8 84.06(14) . . . . ?
N10 Fe1 N3 C4 -86.83(14) . . . . ?
N10 N9 C22 N8 -4.4(2) . . . . ?
N10 N9 C22 C21 174.34(17) . . . . ?
N10 N9 C23 C24 0.0(2) . . . . ?
C22 N8 C18 N7 -178.37(15) . . . . ?
C22 N8 C18 C19 0.8(3) . . . . ?
C22 N9 N10 Fe1 0.60(18) . . . . ?
C22 N9 N10 C25 176.42(15) . . . . ?
C22 N9 C23 C24 -175.55(18) . . . . ?
C22 C21 C20 S2 177.78(14) . . . . ?
C22 C21 C20 C19 0.2(3) . . . . ?
C7 C6 C5 C4 1.1(3) . . . . ?
C8 N3 C4 N2 -176.50(15) . . . . ?
C8 N3 C4 C5 1.0(3) . . . . ?
C8 N4 N5 Fe1 -3.77(18) . . . . ?
C8 N4 N5 C11 177.57(15) . . . . ?
C8 N4 C9 C10 -177.31(18) . . . . ?
C8 C7 C6 S1 -179.51(14) . . . . ?
C8 C7 C6 C5 -0.2(3) . . . . ?
C4 N2 N1 Fe1 -5.09(18) . . . . ?
C4 N2 N1 C1 173.28(15) . . . . ?
C4 N2 C3 C2 -171.76(18) . . . . ?
C4 N3 C8 N4 177.66(15) . . . . ?
C4 N3 C8 C7 0.1(3) . . . . ?
C18 N7 N6 Fe1 0.44(18) . . . . ?
C18 N7 N6 C15 -179.00(15) . . . . ?
C18 N7 C17 C16 178.73(18) . . . . ?
C18 N8 C22 N9 178.41(15) . . . . ?
C18 N8 C22 C21 -0.4(3) . . . . ?
C18 C19 C20 S2 -177.66(14) . . . . ?
C18 C19 C20 C21 0.1(3) . . . . ?
C6 S1 C12 C14 -169.60(13) . . . . ?
C6 S1 C12 C13 69.22(15) . . . . ?
C6 C7 C8 N3 -0.4(3) . . . . ?
C6 C7 C8 N4 -177.63(17) . . . . ?
C3 N2 N1 Fe1 -178.41(12) . . . . ?
C3 N2 N1 C1 -0.04(19) . . . . ?
C3 N2 C4 N3 178.24(17) . . . . ?
C3 N2 C4 C5 0.9(3) . . . . ?
C23 N9 N10 Fe1 -175.76(12) . . . . ?
C23 N9 N10 C25 0.06(19) . . . . ?
C23 N9 C22 N8 170.94(18) . . . . ?
C23 N9 C22 C21 -10.3(3) . . . . ?
C23 C24 C25 N10 0.1(2) . . . . ?
C9 N4 N5 Fe1 178.97(12) . . . . ?
C9 N4 N5 C11 0.3(2) . . . . ?
C9 N4 C8 N3 175.08(18) . . . . ?
C9 N4 C8 C7 -7.4(3) . . . . ?
C17 N7 N6 Fe1 179.38(12) . . . . ?
C17 N7 N6 C15 -0.06(19) . . . . ?
C17 N7 C18 N8 -174.95(18) . . . . ?
C17 N7 C18 C19 6.0(3) . . . . ?
C20 S2 C26 C27 78.28(16) . . . . ?
C20 S2 C26 C28 -159.02(14) . . . . ?
C12 S1 C6 C7 -165.02(14) . . . . ?
C12 S1 C6 C5 15.68(18) . . . . ?
C26 S2 C20 C21 4.64(19) . . . . ?
C26 S2 C20 C19 -177.68(15) . . . . ?


####################################################################### 
# 
# 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_rk137MeCNPI_085K
_database_code_depnum_ccdc_archive 'CCDC 1564668'
_audit_update_record             
;
2017-07-28 deposited with the CCDC.
2017-11-20 downloaded from the CCDC.
;
_chemical_name_common            ?
_chemical_name_systematic        ?
_chemical_formula_moiety         'C28 H30 Fe N10 S2, 2(B F4), C2 H3 N'
_chemical_formula_sum            'C30 H33 B2 F8 Fe N11 S2'
_chemical_formula_weight         841.26
_chemical_melting_point          'not measured'
loop_
_atom_type_symbol
_atom_type_description
_atom_type_scat_dispersion_real
_atom_type_scat_dispersion_imag
_atom_type_scat_source
C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
B B 0.0013 0.0007 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
F F 0.0171 0.0103 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Fe Fe 0.3463 0.8444 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
S S 0.1246 0.1234 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'

_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.
;
_space_group_crystal_system      monoclinic
_space_group_IT_number           14
_space_group_name_H-M_alt        'P 1 21/c 1'
_space_group_name_Hall           '-P 2ybc'
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                   20.2089(3)
_cell_length_b                   11.8753(2)
_cell_length_c                   15.6161(3)
_cell_angle_alpha                90
_cell_angle_beta                 99.4110(10)
_cell_angle_gamma                90
_cell_volume                     3697.22(11)
_cell_formula_units_Z            4
_cell_measurement_reflns_used    10752
_cell_measurement_temperature    85
_cell_measurement_theta_max      33.0440
_cell_measurement_theta_min      3.1760
_shelx_estimated_absorpt_T_max   ?
_shelx_estimated_absorpt_T_min   ?
_exptl_absorpt_coefficient_mu    0.602
_exptl_absorpt_correction_T_max  0.951
_exptl_absorpt_correction_T_min  0.823
_exptl_absorpt_correction_type   analytical
_exptl_absorpt_process_details   
;
CrysAlisPro 1.171.38.46 (Rigaku Oxford Diffraction, 2015)
Analytical numeric absorption correction using a multifaceted crystal
			model based on expressions derived by R.C. Clark & J.S. Reid.
(Clark, R. C. & Reid, J. S. (1995). Acta Cryst. A51, 887-897)
Empirical absorption correction using spherical harmonics,
 implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_absorpt_special_details   ?
_exptl_crystal_colour            'light orange'
_exptl_crystal_density_diffrn    1.511
_exptl_crystal_density_meas      'not measured'
_exptl_crystal_density_method    none
_exptl_crystal_description       block
_exptl_crystal_F_000             1720
loop_
_exptl_crystal_face_index_h
_exptl_crystal_face_index_k
_exptl_crystal_face_index_l
_exptl_crystal_face_perp_dist
0 12 20 0.0406
0 -12 -20 0.0598
16 2 15 0.1760
19 -8 1 0.2081
9 8 20 0.1207
-19 7 -2 0.2306
-14 -5 -18 0.1774
-1 8 -25 0.0739
1 -8 25 0.0296
19 9 -4 0.1976
-19 -9 4 0.2116

_exptl_crystal_size_max          0.508
_exptl_crystal_size_mid          0.138
_exptl_crystal_size_min          0.1
loop_
_exptl_oxdiff_crystal_face_indexfrac_h
_exptl_oxdiff_crystal_face_indexfrac_k
_exptl_oxdiff_crystal_face_indexfrac_l
_exptl_oxdiff_crystal_face_x
_exptl_oxdiff_crystal_face_y
_exptl_oxdiff_crystal_face_z
0.0012 12.0161 19.9408 -0.8349 0.1970 0.5314
-0.0012 -12.0161 -19.9408 0.8349 -0.1970 -0.5314
16.0018 2.0157 14.9817 -0.0330 -0.0038 0.9842
19.0011 -7.9948 1.0289 0.6731 -0.1837 0.7203
9.0017 8.0182 19.9557 -0.4989 0.1088 0.8605
-19.0011 6.9941 -2.0247 -0.6169 0.1550 -0.7493
-14.0019 -5.0176 -17.9685 0.2441 -0.0600 -0.9928
-1.0027 7.9759 -24.9972 0.1896 0.8260 -0.5608
1.0027 -7.9759 24.9972 -0.1896 -0.8260 0.5608
18.9998 8.9978 -4.0180 0.1576 0.7091 0.7115
-18.9998 -8.9978 4.0180 -0.1576 -0.7091 -0.7115

_exptl_transmission_factor_max   ?
_exptl_transmission_factor_min   ?
_diffrn_reflns_av_R_equivalents  0.0337
_diffrn_reflns_av_unetI/netI     0.0296
_diffrn_reflns_Laue_measured_fraction_full 0.998
_diffrn_reflns_Laue_measured_fraction_max 0.998
_diffrn_reflns_limit_h_max       25
_diffrn_reflns_limit_h_min       -21
_diffrn_reflns_limit_k_max       15
_diffrn_reflns_limit_k_min       -14
_diffrn_reflns_limit_l_max       19
_diffrn_reflns_limit_l_min       -19
_diffrn_reflns_number            34512
_diffrn_reflns_point_group_measured_fraction_full 0.998
_diffrn_reflns_point_group_measured_fraction_max 0.998
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         26.999
_diffrn_reflns_theta_min         3.066
_diffrn_ambient_temperature      85
_diffrn_detector                 'CCD plate'
_diffrn_detector_area_resol_mean 16.1852
_diffrn_detector_type            Sapphire3
_diffrn_measured_fraction_theta_full 0.998
_diffrn_measured_fraction_theta_max 0.998
_diffrn_measurement_details      
;
List of Runs (angles in degrees, time in seconds):

  # Type    Start    End  Width  tₑₓₚ   ω     θ     κ     φ   Frames
#--------------------------------------------------------------------------
  1  ω    -89.00 -62.00   1.00   30.00    --  -30.39-178.00 -30.00   27
  2  ω   -113.00 -73.00   1.00   30.00    --  -30.39 178.00 -60.00   40
  3  ω    -37.00  50.00   1.00   30.00    --   32.43 -57.00-180.00   87
  4  ω    -12.00  70.00   1.00   30.00    --   32.43 -99.00 -60.00   82
  5  ω     11.00 100.00   1.00   30.00    --   32.43  57.00  30.00   89
  6  ω    -33.00 103.00   1.00   30.00    --   32.43  19.00-180.00  136
  7  ω     17.00  76.00   1.00   30.00    --   32.43 -99.00 150.00   59
  8  ω     40.00  65.00   1.00   30.00    --   32.43  57.00 -30.00   25
;
_diffrn_measurement_device       'four-circle diffractometer'
_diffrn_measurement_device_type  'Xcalibur, Sapphire3'
_diffrn_measurement_method       'ω scans'
_diffrn_orient_matrix_type       
'CrysAlisPro convention (1999,Acta A55,543-557)'
_diffrn_orient_matrix_UB_11      0.0212442000
_diffrn_orient_matrix_UB_12      -0.0362750000
_diffrn_orient_matrix_UB_13      -0.0200100000
_diffrn_orient_matrix_UB_21      0.0111314000
_diffrn_orient_matrix_UB_22      0.0470570000
_diffrn_orient_matrix_UB_23      -0.0184771000
_diffrn_orient_matrix_UB_31      0.0393106000
_diffrn_orient_matrix_UB_32      0.0062810000
_diffrn_orient_matrix_UB_33      0.0228637000
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_source                   'fine-focus sealed X-ray tube'
_diffrn_source_type              'Enhance (Mo) X-ray Source'
_diffrn_special_details          
'under light exposure, laser 660nm 2mW on the sample'
_reflns_Friedel_coverage         0.000
_reflns_Friedel_fraction_full    .
_reflns_Friedel_fraction_max     .
_reflns_number_gt                6640
_reflns_number_total             8048
_reflns_odcompleteness_completeness 99.84
_reflns_odcompleteness_iscentric 1
_reflns_odcompleteness_theta     31.44
_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.
;
_reflns_threshold_expression     'I > 2σ(I)'
_computing_cell_refinement       'CrysAlisPro 1.171.38.46 (Rigaku OD, 2015)'
_computing_data_collection       'CrysAlisPro 1.171.37.31c (Rigaku OD, 2014)'
_computing_data_reduction        'CrysAlisPro 1.171.38.46 (Rigaku OD, 2015)'
_computing_molecular_graphics    'Mercury3.9 (2016)'
_computing_publication_material  'Olex2 (Dolomanov et al., 2009)'
_computing_structure_refinement  'ShelXL (Sheldrick, 2015)'
_computing_structure_solution    'ShelXT (Sheldrick, 2015)'
_refine_diff_density_max         0.503
_refine_diff_density_min         -0.329
_refine_diff_density_rms         0.061
_refine_ls_extinction_coef       .
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.058
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     492
_refine_ls_number_reflns         8048
_refine_ls_number_restraints     0
_refine_ls_R_factor_all          0.0506
_refine_ls_R_factor_gt           0.0376
_refine_ls_restrained_S_all      1.058
_refine_ls_shift/su_max          0.001
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details     
'w=1/[σ²(Fo²)+(0.0382P)²+2.7729P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0860
_refine_ls_wR_factor_ref         0.0919
_refine_special_details          
;
Structure of photo-excited high spin state at 85K. 
Excitation with 660nm laser. Laser power delivered on the crystal was ~2mW.
;
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     dual
_atom_sites_solution_secondary   difmap
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 0.72202(2) 0.39757(2) 0.55592(2) 0.01773(8) Uani 1 1 d . . . . .
S1 S 0.39757(2) 0.28787(4) 0.52147(3) 0.02205(12) Uani 1 1 d . . . . .
S2 S 1.04001(3) 0.49771(5) 0.72044(4) 0.02660(13) Uani 1 1 d . . . . .
F1 F 0.63882(6) 0.54616(12) 0.22818(8) 0.0328(3) Uani 1 1 d . . . . .
F4 F 0.57470(7) 0.44753(12) 0.30831(8) 0.0340(3) Uani 1 1 d . . . . .
F3 F 0.52542(6) 0.57116(12) 0.20566(9) 0.0348(3) Uani 1 1 d . . . . .
F2 F 0.57008(7) 0.40780(13) 0.16496(9) 0.0376(3) Uani 1 1 d . . . . .
F8 F 0.89015(7) 0.34268(13) 0.45375(9) 0.0390(3) Uani 1 1 d . . . . .
F6 F 0.99641(6) 0.31372(12) 0.52530(9) 0.0377(3) Uani 1 1 d . U . . .
F7 F 0.91543(8) 0.18698(15) 0.53568(11) 0.0529(4) Uani 1 1 d . . . . .
N7 N 0.82393(8) 0.55688(14) 0.50213(10) 0.0178(3) Uani 1 1 d . . . . .
N8 N 0.82486(8) 0.42356(14) 0.60733(10) 0.0165(3) Uani 1 1 d . . . . .
N2 N 0.63502(8) 0.24466(14) 0.43072(10) 0.0171(3) Uani 1 1 d . . . . .
N3 N 0.61628(8) 0.37256(14) 0.53270(10) 0.0168(3) Uani 1 1 d . . . . .
F5 F 0.95522(9) 0.20824(16) 0.40880(9) 0.0582(5) Uani 1 1 d . U . . .
N9 N 0.81287(8) 0.28012(14) 0.70059(10) 0.0180(3) Uani 1 1 d . . . . .
N6 N 0.75856(8) 0.52542(14) 0.47581(10) 0.0179(3) Uani 1 1 d . . . . .
N4 N 0.61143(8) 0.50427(14) 0.63840(11) 0.0192(3) Uani 1 1 d . . . . .
N1 N 0.70184(8) 0.26710(15) 0.45740(10) 0.0195(4) Uani 1 1 d . . . . .
N5 N 0.67878(8) 0.51791(14) 0.63927(10) 0.0199(4) Uani 1 1 d . . . . .
N10 N 0.74868(8) 0.27134(14) 0.65635(10) 0.0197(4) Uani 1 1 d . . . . .
C22 C 0.85485(10) 0.36296(17) 0.67414(12) 0.0173(4) Uani 1 1 d . . . . .
C7 C 0.51077(10) 0.39700(17) 0.58088(13) 0.0200(4) Uani 1 1 d . . . . .
H7 H 0.4849 0.4340 0.6181 0.024 Uiso 1 1 calc R . . . .
C8 C 0.57722(10) 0.42245(17) 0.58257(12) 0.0186(4) Uani 1 1 d . . . . .
C4 C 0.58859(9) 0.29353(16) 0.47739(12) 0.0170(4) Uani 1 1 d . . . . .
C18 C 0.86098(9) 0.50121(16) 0.57449(12) 0.0167(4) Uani 1 1 d . . . . .
C6 C 0.48258(9) 0.31415(17) 0.52205(12) 0.0186(4) Uani 1 1 d . . . . .
C3 C 0.62621(10) 0.16655(17) 0.36582(12) 0.0203(4) Uani 1 1 d . . . . .
H3 H 0.5846 0.1381 0.3366 0.024 Uiso 1 1 calc R . . . .
C5 C 0.52207(9) 0.26127(17) 0.46826(12) 0.0180(4) Uani 1 1 d . . . . .
H5 H 0.5040 0.2057 0.4273 0.022 Uiso 1 1 calc R . . . .
C21 C 0.92063(10) 0.37849(17) 0.71322(12) 0.0195(4) Uani 1 1 d . . . . .
H21 H 0.9401 0.3343 0.7615 0.023 Uiso 1 1 calc R . . . .
C1 C 0.73373(10) 0.20134(18) 0.40942(13) 0.0226(4) Uani 1 1 d . . . . .
H1 H 0.7811 0.1979 0.4139 0.027 Uiso 1 1 calc R . . . .
C23 C 0.82630(10) 0.19698(18) 0.76082(13) 0.0220(4) Uani 1 1 d . . . . .
H23 H 0.8673 0.1855 0.7992 0.026 Uiso 1 1 calc R . . . .
C19 C 0.92690(10) 0.52434(17) 0.60643(13) 0.0196(4) Uani 1 1 d . . . . .
H19 H 0.9510 0.5802 0.5808 0.024 Uiso 1 1 calc R . . . .
C15 C 0.73718(10) 0.58883(17) 0.40670(12) 0.0200(4) Uani 1 1 d . . . . .
H15 H 0.6932 0.5859 0.3742 0.024 Uiso 1 1 calc R . . . .
C9 C 0.58718(11) 0.58284(18) 0.68890(13) 0.0234(4) Uani 1 1 d . . . . .
H9 H 0.5421 0.5901 0.6982 0.028 Uiso 1 1 calc R . . . .
C17 C 0.84261(11) 0.63735(18) 0.44987(13) 0.0240(4) Uani 1 1 d . . . . .
H17 H 0.8856 0.6715 0.4550 0.029 Uiso 1 1 calc R . . . .
C20 C 0.95719(10) 0.46183(17) 0.67880(13) 0.0203(4) Uani 1 1 d . . . . .
C12 C 0.38100(10) 0.15289(18) 0.46643(13) 0.0225(4) Uani 1 1 d . . . . .
H12 H 0.3968 0.1555 0.4091 0.027 Uiso 1 1 calc R . . . .
C11 C 0.69579(11) 0.60547(18) 0.69067(13) 0.0238(4) Uani 1 1 d . . . . .
H11 H 0.7399 0.6351 0.7038 0.029 Uiso 1 1 calc R . . . .
C2 C 0.68852(10) 0.13709(18) 0.35091(13) 0.0237(4) Uani 1 1 d . . . . .
H2 H 0.6992 0.0842 0.3096 0.028 Uiso 1 1 calc R . . . .
C24 C 0.76958(11) 0.13320(18) 0.75556(14) 0.0249(4) Uani 1 1 d . . . . .
H24 H 0.7631 0.0688 0.7893 0.030 Uiso 1 1 calc R . . . .
C25 C 0.72286(10) 0.18238(18) 0.68997(13) 0.0231(4) Uani 1 1 d . . . . .
H25 H 0.6785 0.1554 0.6720 0.028 Uiso 1 1 calc R . . . .
C10 C 0.64012(11) 0.64906(19) 0.72348(14) 0.0266(5) Uani 1 1 d . . . . .
H10 H 0.6395 0.7113 0.7616 0.032 Uiso 1 1 calc R . . . .
C16 C 0.78793(11) 0.66052(19) 0.38810(13) 0.0250(5) Uani 1 1 d . . . . .
H16 H 0.7851 0.7139 0.3424 0.030 Uiso 1 1 calc R . . . .
C26 C 1.06735(11) 0.3910(2) 0.80284(14) 0.0285(5) Uani 1 1 d . . . . .
H26 H 1.0324 0.3824 0.8409 0.034 Uiso 1 1 calc R . . . .
C14 C 0.30505(11) 0.1377(2) 0.45202(16) 0.0318(5) Uani 1 1 d . . . . .
H14A H 0.2894 0.1368 0.5082 0.048 Uiso 1 1 calc GR . . . .
H14B H 0.2932 0.0665 0.4217 0.048 Uiso 1 1 calc GR . . . .
H14C H 0.2837 0.2002 0.4169 0.048 Uiso 1 1 calc GR . . . .
C13 C 0.41666(11) 0.0584(2) 0.52093(15) 0.0290(5) Uani 1 1 d . . . . .
H13A H 0.4649 0.0740 0.5328 0.044 Uiso 1 1 calc GR . . . .
H13B H 0.4088 -0.0129 0.4893 0.044 Uiso 1 1 calc GR . . . .
H13C H 0.3993 0.0531 0.5759 0.044 Uiso 1 1 calc GR . . . .
C29 C 0.86975(12) 0.5523(2) 0.87275(16) 0.0355(6) Uani 1 1 d . . . . .
C27 C 1.07816(12) 0.2786(2) 0.76146(18) 0.0391(6) Uani 1 1 d . . . . .
H27A H 1.0360 0.2534 0.7265 0.059 Uiso 1 1 calc GR . . . .
H27B H 1.0930 0.2230 0.8069 0.059 Uiso 1 1 calc GR . . . .
H27C H 1.1124 0.2866 0.7241 0.059 Uiso 1 1 calc GR . . . .
N11 N 0.81856(13) 0.5430(2) 0.83184(18) 0.0615(7) Uani 1 1 d . . . . .
C28 C 1.13173(12) 0.4369(3) 0.85693(17) 0.0434(7) Uani 1 1 d . . . . .
H28A H 1.1660 0.4466 0.8197 0.065 Uiso 1 1 calc GR . . . .
H28B H 1.1480 0.3838 0.9037 0.065 Uiso 1 1 calc GR . . . .
H28C H 1.1224 0.5097 0.8820 0.065 Uiso 1 1 calc GR . . . .
B1 B 0.57744(12) 0.4928(2) 0.22608(15) 0.0246(5) Uani 1 1 d . . . . .
B2 B 0.93876(13) 0.2625(2) 0.48129(16) 0.0270(5) Uani 1 1 d . . . . .
C30 C 0.93562(14) 0.5612(2) 0.9248(2) 0.0485(7) Uani 1 1 d . . . . .
H30A H 0.9694 0.5681 0.8867 0.073 Uiso 1 1 calc GR . . . .
H30B H 0.9448 0.4937 0.9609 0.073 Uiso 1 1 calc GR . . . .
H30C H 0.9373 0.6279 0.9622 0.073 Uiso 1 1 calc GR . . . .


_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 2.1246(16) . ?
Fe1 N3 2.1289(16) . ?
Fe1 N6 2.1721(17) . ?
Fe1 N1 2.1745(17) . ?
Fe1 N5 2.2073(17) . ?
Fe1 N10 2.1726(17) . ?
S1 C6 1.7446(19) . ?
S1 C12 1.824(2) . ?
S2 C20 1.746(2) . ?
S2 C26 1.826(2) . ?
F1 B1 1.389(3) . ?
F4 B1 1.402(3) . ?
F3 B1 1.401(3) . ?
F2 B1 1.381(3) . ?
F8 B2 1.385(3) . ?
F6 B2 1.392(3) . ?
F7 B2 1.371(3) . ?
N7 N6 1.370(2) . ?
N7 C18 1.413(2) . ?
N7 C17 1.350(3) . ?
N8 C22 1.329(2) . ?
N8 C18 1.330(2) . ?
N2 N1 1.373(2) . ?
N2 C4 1.404(2) . ?
N2 C3 1.364(2) . ?
N3 C8 1.335(3) . ?
N3 C4 1.335(2) . ?
F5 B2 1.390(3) . ?
N9 N10 1.370(2) . ?
N9 C22 1.405(3) . ?
N9 C23 1.360(3) . ?
N6 C15 1.329(3) . ?
N4 N5 1.369(2) . ?
N4 C8 1.409(3) . ?
N4 C9 1.363(3) . ?
N1 C1 1.321(3) . ?
N5 C11 1.324(3) . ?
N10 C25 1.324(3) . ?
C22 C21 1.381(3) . ?
C7 H7 0.9500 . ?
C7 C8 1.372(3) . ?
C7 C6 1.402(3) . ?
C4 C5 1.383(3) . ?
C18 C19 1.372(3) . ?
C6 C5 1.398(3) . ?
C3 H3 0.9500 . ?
C3 C2 1.363(3) . ?
C5 H5 0.9500 . ?
C21 H21 0.9500 . ?
C21 C20 1.394(3) . ?
C1 H1 0.9500 . ?
C1 C2 1.407(3) . ?
C23 H23 0.9500 . ?
C23 C24 1.365(3) . ?
C19 H19 0.9500 . ?
C19 C20 1.406(3) . ?
C15 H15 0.9500 . ?
C15 C16 1.400(3) . ?
C9 H9 0.9500 . ?
C9 C10 1.366(3) . ?
C17 H17 0.9500 . ?
C17 C16 1.371(3) . ?
C12 H12 1.0000 . ?
C12 C14 1.525(3) . ?
C12 C13 1.517(3) . ?
C11 H11 0.9500 . ?
C11 C10 1.409(3) . ?
C2 H2 0.9500 . ?
C24 H24 0.9500 . ?
C24 C25 1.402(3) . ?
C25 H25 0.9500 . ?
C10 H10 0.9500 . ?
C16 H16 0.9500 . ?
C26 H26 1.0000 . ?
C26 C27 1.515(4) . ?
C26 C28 1.531(3) . ?
C14 H14A 0.9800 . ?
C14 H14B 0.9800 . ?
C14 H14C 0.9800 . ?
C13 H13A 0.9800 . ?
C13 H13B 0.9800 . ?
C13 H13C 0.9800 . ?
C29 N11 1.129(3) . ?
C29 C30 1.446(3) . ?
C27 H27A 0.9800 . ?
C27 H27B 0.9800 . ?
C27 H27C 0.9800 . ?
C28 H28A 0.9800 . ?
C28 H28B 0.9800 . ?
C28 H28C 0.9800 . ?
C30 H30A 0.9800 . ?
C30 H30B 0.9800 . ?
C30 H30C 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 167.76(6) . . ?
N8 Fe1 N6 73.28(6) . . ?
N8 Fe1 N1 115.44(6) . . ?
N8 Fe1 N5 98.06(6) . . ?
N8 Fe1 N10 73.48(6) . . ?
N3 Fe1 N6 115.20(6) . . ?
N3 Fe1 N1 73.33(6) . . ?
N3 Fe1 N5 73.00(6) . . ?
N3 Fe1 N10 98.65(6) . . ?
N6 Fe1 N1 97.62(6) . . ?
N6 Fe1 N5 95.26(6) . . ?
N6 Fe1 N10 146.14(6) . . ?
N1 Fe1 N5 146.31(6) . . ?
N10 Fe1 N1 90.85(6) . . ?
N10 Fe1 N5 95.53(6) . . ?
C6 S1 C12 105.34(10) . . ?
C20 S2 C26 104.73(10) . . ?
N6 N7 C18 118.11(16) . . ?
C17 N7 N6 111.28(16) . . ?
C17 N7 C18 130.58(17) . . ?
C22 N8 Fe1 120.68(13) . . ?
C22 N8 C18 118.01(16) . . ?
C18 N8 Fe1 121.31(13) . . ?
N1 N2 C4 118.03(15) . . ?
C3 N2 N1 111.10(15) . . ?
C3 N2 C4 130.51(16) . . ?
C8 N3 Fe1 120.77(13) . . ?
C8 N3 C4 117.66(17) . . ?
C4 N3 Fe1 120.74(13) . . ?
N10 N9 C22 118.19(15) . . ?
C23 N9 N10 111.03(16) . . ?
C23 N9 C22 130.55(17) . . ?
N7 N6 Fe1 114.83(11) . . ?
C15 N6 Fe1 140.16(14) . . ?
C15 N6 N7 105.00(16) . . ?
N5 N4 C8 118.31(16) . . ?
C9 N4 N5 111.35(16) . . ?
C9 N4 C8 130.06(18) . . ?
N2 N1 Fe1 114.49(12) . . ?
C1 N1 Fe1 140.37(14) . . ?
C1 N1 N2 105.08(16) . . ?
N4 N5 Fe1 113.98(12) . . ?
C11 N5 Fe1 141.02(14) . . ?
C11 N5 N4 104.96(16) . . ?
N9 N10 Fe1 114.46(12) . . ?
C25 N10 Fe1 140.29(14) . . ?
C25 N10 N9 105.22(16) . . ?
N8 C22 N9 112.98(16) . . ?
N8 C22 C21 123.83(18) . . ?
C21 C22 N9 123.19(17) . . ?
C8 C7 H7 121.3 . . ?
C8 C7 C6 117.30(18) . . ?
C6 C7 H7 121.3 . . ?
N3 C8 N4 112.96(17) . . ?
N3 C8 C7 124.13(18) . . ?
C7 C8 N4 122.91(18) . . ?
N3 C4 N2 112.42(16) . . ?
N3 C4 C5 123.99(18) . . ?
C5 C4 N2 123.57(17) . . ?
N8 C18 N7 112.35(16) . . ?
N8 C18 C19 124.07(18) . . ?
C19 C18 N7 123.58(18) . . ?
C7 C6 S1 115.04(15) . . ?
C5 C6 S1 125.08(15) . . ?
C5 C6 C7 119.87(18) . . ?
N2 C3 H3 126.6 . . ?
C2 C3 N2 106.82(17) . . ?
C2 C3 H3 126.6 . . ?
C4 C5 C6 117.03(18) . . ?
C4 C5 H5 121.5 . . ?
C6 C5 H5 121.5 . . ?
C22 C21 H21 121.4 . . ?
C22 C21 C20 117.18(18) . . ?
C20 C21 H21 121.4 . . ?
N1 C1 H1 124.3 . . ?
N1 C1 C2 111.34(18) . . ?
C2 C1 H1 124.3 . . ?
N9 C23 H23 126.6 . . ?
N9 C23 C24 106.89(18) . . ?
C24 C23 H23 126.6 . . ?
C18 C19 H19 121.4 . . ?
C18 C19 C20 117.12(18) . . ?
C20 C19 H19 121.4 . . ?
N6 C15 H15 124.4 . . ?
N6 C15 C16 111.17(18) . . ?
C16 C15 H15 124.4 . . ?
N4 C9 H9 126.6 . . ?
N4 C9 C10 106.88(19) . . ?
C10 C9 H9 126.6 . . ?
N7 C17 H17 126.4 . . ?
N7 C17 C16 107.14(18) . . ?
C16 C17 H17 126.4 . . ?
C21 C20 S2 124.44(15) . . ?
C21 C20 C19 119.75(18) . . ?
C19 C20 S2 115.80(15) . . ?
S1 C12 H12 109.5 . . ?
C14 C12 S1 106.03(15) . . ?
C14 C12 H12 109.5 . . ?
C13 C12 S1 110.60(15) . . ?
C13 C12 H12 109.5 . . ?
C13 C12 C14 111.70(18) . . ?
N5 C11 H11 124.3 . . ?
N5 C11 C10 111.43(19) . . ?
C10 C11 H11 124.3 . . ?
C3 C2 C1 105.66(18) . . ?
C3 C2 H2 127.2 . . ?
C1 C2 H2 127.2 . . ?
C23 C24 H24 127.1 . . ?
C23 C24 C25 105.74(18) . . ?
C25 C24 H24 127.1 . . ?
N10 C25 C24 111.11(18) . . ?
N10 C25 H25 124.4 . . ?
C24 C25 H25 124.4 . . ?
C9 C10 C11 105.37(19) . . ?
C9 C10 H10 127.3 . . ?
C11 C10 H10 127.3 . . ?
C15 C16 H16 127.3 . . ?
C17 C16 C15 105.41(18) . . ?
C17 C16 H16 127.3 . . ?
S2 C26 H26 109.2 . . ?
C27 C26 S2 111.05(16) . . ?
C27 C26 H26 109.2 . . ?
C27 C26 C28 112.3(2) . . ?
C28 C26 S2 105.90(16) . . ?
C28 C26 H26 109.2 . . ?
C12 C14 H14A 109.5 . . ?
C12 C14 H14B 109.5 . . ?
C12 C14 H14C 109.5 . . ?
H14A C14 H14B 109.5 . . ?
H14A C14 H14C 109.5 . . ?
H14B C14 H14C 109.5 . . ?
C12 C13 H13A 109.5 . . ?
C12 C13 H13B 109.5 . . ?
C12 C13 H13C 109.5 . . ?
H13A C13 H13B 109.5 . . ?
H13A C13 H13C 109.5 . . ?
H13B C13 H13C 109.5 . . ?
N11 C29 C30 178.5(3) . . ?
C26 C27 H27A 109.5 . . ?
C26 C27 H27B 109.5 . . ?
C26 C27 H27C 109.5 . . ?
H27A C27 H27B 109.5 . . ?
H27A C27 H27C 109.5 . . ?
H27B C27 H27C 109.5 . . ?
C26 C28 H28A 109.5 . . ?
C26 C28 H28B 109.5 . . ?
C26 C28 H28C 109.5 . . ?
H28A C28 H28B 109.5 . . ?
H28A C28 H28C 109.5 . . ?
H28B C28 H28C 109.5 . . ?
F1 B1 F4 108.80(17) . . ?
F1 B1 F3 109.7(2) . . ?
F3 B1 F4 108.83(18) . . ?
F2 B1 F1 110.17(18) . . ?
F2 B1 F4 109.7(2) . . ?
F2 B1 F3 109.66(18) . . ?
F8 B2 F6 110.3(2) . . ?
F8 B2 F5 108.54(19) . . ?
F7 B2 F8 110.1(2) . . ?
F7 B2 F6 108.96(19) . . ?
F7 B2 F5 110.7(2) . . ?
F5 B2 F6 108.2(2) . . ?
C29 C30 H30A 109.5 . . ?
C29 C30 H30B 109.5 . . ?
C29 C30 H30C 109.5 . . ?
H30A C30 H30B 109.5 . . ?
H30A C30 H30C 109.5 . . ?
H30B C30 H30C 109.5 . . ?

loop_
_geom_torsion_atom_site_label_1
_geom_torsion_atom_site_label_2
_geom_torsion_atom_site_label_3
_geom_torsion_atom_site_label_4
_geom_torsion
_geom_torsion_site_symmetry_1
_geom_torsion_site_symmetry_2
_geom_torsion_site_symmetry_3
_geom_torsion_site_symmetry_4
_geom_torsion_publ_flag
Fe1 N8 C22 N9 3.5(2) . . . . ?
Fe1 N8 C22 C21 -177.14(15) . . . . ?
Fe1 N8 C18 N7 -2.6(2) . . . . ?
Fe1 N8 C18 C19 177.94(15) . . . . ?
Fe1 N3 C8 N4 10.3(2) . . . . ?
Fe1 N3 C8 C7 -169.19(15) . . . . ?
Fe1 N3 C4 N2 -8.3(2) . . . . ?
Fe1 N3 C4 C5 170.27(15) . . . . ?
Fe1 N6 C15 C16 178.30(16) . . . . ?
Fe1 N1 C1 C2 -175.84(16) . . . . ?
Fe1 N5 C11 C10 177.43(16) . . . . ?
Fe1 N10 C25 C24 178.12(16) . . . . ?
S1 C6 C5 C4 179.50(15) . . . . ?
N7 N6 C15 C16 0.1(2) . . . . ?
N7 C18 C19 C20 -179.88(18) . . . . ?
N7 C17 C16 C15 -0.6(2) . . . . ?
N8 C22 C21 C20 -1.0(3) . . . . ?
N8 C18 C19 C20 -0.5(3) . . . . ?
N2 N1 C1 C2 0.7(2) . . . . ?
N2 C4 C5 C6 177.16(17) . . . . ?
N2 C3 C2 C1 -0.2(2) . . . . ?
N3 C4 C5 C6 -1.3(3) . . . . ?
N9 N10 C25 C24 0.0(2) . . . . ?
N9 C22 C21 C20 178.23(18) . . . . ?
N9 C23 C24 C25 0.1(2) . . . . ?
N6 N7 C18 N8 -0.1(2) . . . . ?
N6 N7 C18 C19 179.31(18) . . . . ?
N6 N7 C17 C16 0.7(2) . . . . ?
N6 C15 C16 C17 0.3(2) . . . . ?
N4 N5 C11 C10 0.1(2) . . . . ?
N4 C9 C10 C11 0.1(2) . . . . ?
N1 N2 C4 N3 11.5(2) . . . . ?
N1 N2 C4 C5 -167.11(18) . . . . ?
N1 N2 C3 C2 0.6(2) . . . . ?
N1 C1 C2 C3 -0.3(2) . . . . ?
N5 N4 C8 N3 -3.9(2) . . . . ?
N5 N4 C8 C7 175.61(18) . . . . ?
N5 N4 C9 C10 -0.1(2) . . . . ?
N5 C11 C10 C9 -0.1(3) . . . . ?
N10 N9 C22 N8 0.2(2) . . . . ?
N10 N9 C22 C21 -179.16(18) . . . . ?
N10 N9 C23 C24 -0.1(2) . . . . ?
C22 N8 C18 N7 178.00(16) . . . . ?
C22 N8 C18 C19 -1.4(3) . . . . ?
C22 N9 N10 Fe1 -3.5(2) . . . . ?
C22 N9 N10 C25 175.19(17) . . . . ?
C22 N9 C23 C24 -174.42(19) . . . . ?
C22 C21 C20 S2 178.01(15) . . . . ?
C22 C21 C20 C19 -1.0(3) . . . . ?
C7 C6 C5 C4 0.9(3) . . . . ?
C8 N3 C4 N2 -177.99(16) . . . . ?
C8 N3 C4 C5 0.6(3) . . . . ?
C8 N4 N5 Fe1 -3.6(2) . . . . ?
C8 N4 N5 C11 174.57(17) . . . . ?
C8 N4 C9 C10 -173.82(19) . . . . ?
C8 C7 C6 S1 -178.70(15) . . . . ?
C8 C7 C6 C5 0.0(3) . . . . ?
C4 N2 N1 Fe1 -9.4(2) . . . . ?
C4 N2 N1 C1 172.99(17) . . . . ?
C4 N2 C3 C2 -172.19(19) . . . . ?
C4 N3 C8 N4 179.98(16) . . . . ?
C4 N3 C8 C7 0.5(3) . . . . ?
C18 N7 N6 Fe1 2.6(2) . . . . ?
C18 N7 N6 C15 -178.66(17) . . . . ?
C18 N7 C17 C16 178.56(19) . . . . ?
C18 N8 C22 N9 -177.08(16) . . . . ?
C18 N8 C22 C21 2.2(3) . . . . ?
C18 C19 C20 S2 -177.39(15) . . . . ?
C18 C19 C20 C21 1.7(3) . . . . ?
C6 S1 C12 C14 -170.91(15) . . . . ?
C6 S1 C12 C13 67.82(16) . . . . ?
C6 C7 C8 N3 -0.8(3) . . . . ?
C6 C7 C8 N4 179.77(18) . . . . ?
C3 N2 N1 Fe1 176.74(12) . . . . ?
C3 N2 N1 C1 -0.8(2) . . . . ?
C3 N2 C4 N3 -176.08(18) . . . . ?
C3 N2 C4 C5 5.3(3) . . . . ?
C23 N9 N10 Fe1 -178.61(13) . . . . ?
C23 N9 N10 C25 0.1(2) . . . . ?
C23 N9 C22 N8 174.14(19) . . . . ?
C23 N9 C22 C21 -5.2(3) . . . . ?
C23 C24 C25 N10 0.0(2) . . . . ?
C9 N4 N5 Fe1 -178.19(13) . . . . ?
C9 N4 N5 C11 0.0(2) . . . . ?
C9 N4 C8 N3 169.48(19) . . . . ?
C9 N4 C8 C7 -11.0(3) . . . . ?
C17 N7 N6 Fe1 -179.24(14) . . . . ?
C17 N7 N6 C15 -0.5(2) . . . . ?
C17 N7 C18 N8 -177.9(2) . . . . ?
C17 N7 C18 C19 1.6(3) . . . . ?
C20 S2 C26 C27 72.67(17) . . . . ?
C20 S2 C26 C28 -165.12(17) . . . . ?
C12 S1 C6 C7 -163.41(15) . . . . ?
C12 S1 C6 C5 18.0(2) . . . . ?
C26 S2 C20 C21 8.1(2) . . . . ?
C26 S2 C20 C19 -172.88(16) . . . . ?


