# Electronic Supplementary Material (ESI) for Journal of Materials Chemistry C.
# This journal is © The Royal Society of Chemistry 2015

####################################################################### 
# 
# 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_as150228
_database_code_depnum_ccdc_archive 'CCDC 1058749'
_audit_update_record             
;
2015-04-09 deposited with the CCDC.
2015-05-27 downloaded from the CCDC.
;

_audit_creation_method           SHELXL-97
_chemical_name_systematic        
'Bis[2,6-di(pyrazol-1-yl)-4-(thiomorpholin-1-yl)pyridine]iron(II) di-tetrafluoroborate monohydrate'
_chemical_name_common            ?
_chemical_melting_point          ?
_chemical_formula_moiety         'C30 H32 Fe N12 S2, 2[B F4], H2 O'
_chemical_formula_sum            'C30 H34 B2 F8 Fe N12 O S2'
_chemical_formula_weight         872.28

loop_
_atom_type_symbol
_atom_type_description
_atom_type_scat_dispersion_real
_atom_type_scat_dispersion_imag
_atom_type_scat_source
C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
F F 0.0171 0.0103 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
S S 0.1246 0.1234 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
B B 0.0013 0.0007 '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'
O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'

_symmetry_cell_setting           Triclinic
_symmetry_space_group_name_H-M   'P -1'

loop_
_symmetry_equiv_pos_as_xyz
'x, y, z'
'-x, -y, -z'

_cell_length_a                   11.4182(5)
_cell_length_b                   13.3351(7)
_cell_length_c                   13.8880(8)
_cell_angle_alpha                85.289(4)
_cell_angle_beta                 68.183(4)
_cell_angle_gamma                66.115(4)
_cell_volume                     1789.21(16)
_cell_formula_units_Z            2
_cell_measurement_temperature    100(2)
_cell_measurement_reflns_used    5759
_cell_measurement_theta_min      3.95
_cell_measurement_theta_max      29.52

_exptl_crystal_description       block
_exptl_crystal_colour            yellow
_exptl_crystal_size_max          0.21
_exptl_crystal_size_mid          0.19
_exptl_crystal_size_min          0.10
_exptl_crystal_density_meas      ?
_exptl_crystal_density_diffrn    1.619
_exptl_crystal_density_method    'not measured'
_exptl_crystal_F_000             892
_exptl_absorpt_coefficient_mu    0.627
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_correction_T_min  0.914
_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     0.71073
_diffrn_radiation_type           MoK\a
_diffrn_radiation_source         'SuperNova (Mo) 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            13966
_diffrn_reflns_av_R_equivalents  0.0365
_diffrn_reflns_av_sigmaI/netI    0.0646
_diffrn_reflns_limit_h_min       -13
_diffrn_reflns_limit_h_max       15
_diffrn_reflns_limit_k_min       -17
_diffrn_reflns_limit_k_max       17
_diffrn_reflns_limit_l_min       -17
_diffrn_reflns_limit_l_max       13
_diffrn_reflns_theta_min         3.11
_diffrn_reflns_theta_max         29.83
_reflns_number_total             8281
_reflns_number_gt                6808
_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 anion B51-F55 is disordered over two sites, sharing a common wholly 
 occupied B atom, with refined occupancies of 0.67 and 0.33. These were 
 refined with the fixed restraints B---F = 1.39(2) and F...F = 2.27(2) Å.
 The minor anion site has a distorted geometry, which may reflect the
 lack of a separate B atom for this residue. Attempts to do so were 
 unsuccessful, however. 

 All wholly occupied non-H atoms were refined anisotropically, and C-bound 
 H atoms were placed in calculated positions and refined using a riding 
 model. The water H atoms were located in the Fourier map and refined 
 with the restraints O---H = 0.90(2) and H...H = 1.47(2) Å, and with 
 Uiso{H} = 1.5x Uiso{O}. There are two unfeasibly short intramolecular 
 H...H distances in the final model, H4...H19A = 1.89 Å and H4...H23B = 
 1.95 Å , which imply that the calculated positions of these H atoms 
 may differ from their true positions in the molecule.

 The highest residual Fourier peak of +1.5 e.Å⁻³ lies between the 
 disordered anion site and the water molecule. It may represent evidence 
 of minor additional disorder for one or other of those residues.
;

_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)+(0.0493P)²+3.6348P] where P=(Fo²+2Fc²)/3'
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_atom_sites_solution_hydrogens   geom
_refine_ls_hydrogen_treatment    mixed
_refine_ls_extinction_method     none
_refine_ls_extinction_coef       ?
_refine_ls_number_reflns         8281
_refine_ls_number_parameters     508
_refine_ls_number_restraints     23
_refine_ls_R_factor_all          0.0691
_refine_ls_R_factor_gt           0.0564
_refine_ls_wR_factor_ref         0.1421
_refine_ls_wR_factor_gt          0.1313
_refine_ls_goodness_of_fit_ref   1.035
_refine_ls_restrained_S_all      1.054
_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 0.85966(4) 0.28573(3) 0.25104(3) 0.01195(11) Uani 1 1 d . . .
N2 N 0.8540(2) 0.16428(19) 0.35858(18) 0.0121(5) Uani 1 1 d . . .
C3 C 0.8625(3) 0.1757(2) 0.4499(2) 0.0133(5) Uani 1 1 d . . .
C4 C 0.8369(3) 0.1120(2) 0.5308(2) 0.0149(6) Uani 1 1 d . . .
H4 H 0.8436 0.1248 0.5945 0.018 Uiso 1 1 calc R . .
C5 C 0.7998(3) 0.0259(2) 0.5168(2) 0.0149(6) Uani 1 1 d . . .
C6 C 0.7869(3) 0.0152(2) 0.4209(2) 0.0147(6) Uani 1 1 d . . .
H6 H 0.7584 -0.0386 0.4084 0.018 Uiso 1 1 calc R . .
C7 C 0.8168(3) 0.0848(2) 0.3468(2) 0.0128(5) Uani 1 1 d . . .
N8 N 0.9038(2) 0.26144(19) 0.45436(18) 0.0124(5) Uani 1 1 d . . .
N9 N 0.9232(2) 0.3231(2) 0.37078(19) 0.0146(5) Uani 1 1 d . . .
C10 C 0.9643(3) 0.3937(2) 0.3964(2) 0.0159(6) Uani 1 1 d . . .
H10 H 0.9845 0.4485 0.3537 0.019 Uiso 1 1 calc R . .
C11 C 0.9740(3) 0.3767(3) 0.4946(2) 0.0202(6) Uani 1 1 d . . .
H11 H 1.0019 0.4159 0.5296 0.024 Uiso 1 1 calc R . .
C12 C 0.9351(3) 0.2918(2) 0.5295(2) 0.0178(6) Uani 1 1 d . . .
H12 H 0.9308 0.2602 0.5939 0.021 Uiso 1 1 calc R . .
N13 N 0.8156(2) 0.0782(2) 0.24625(19) 0.0133(5) Uani 1 1 d . . .
N14 N 0.8461(2) 0.1539(2) 0.18038(19) 0.0141(5) Uani 1 1 d . . .
C15 C 0.8513(3) 0.1237(2) 0.0900(2) 0.0160(6) Uani 1 1 d . . .
H15 H 0.8709 0.1612 0.0287 0.019 Uiso 1 1 calc R . .
C16 C 0.8240(3) 0.0294(3) 0.0963(2) 0.0192(6) Uani 1 1 d . . .
H16 H 0.8208 -0.0076 0.0423 0.023 Uiso 1 1 calc R . .
C17 C 0.8030(3) 0.0018(2) 0.1966(2) 0.0173(6) Uani 1 1 d . . .
H17 H 0.7834 -0.0592 0.2259 0.021 Uiso 1 1 calc R . .
N18 N 0.7829(3) -0.0453(2) 0.5912(2) 0.0182(5) Uani 1 1 d . . .
C19 C 0.7897(3) -0.0302(3) 0.6917(2) 0.0185(6) Uani 1 1 d . . .
H19A H 0.8495 0.0094 0.6833 0.022 Uiso 1 1 calc R . .
H19B H 0.8315 -0.1030 0.7164 0.022 Uiso 1 1 calc R . .
C20 C 0.6477(3) 0.0345(3) 0.7720(3) 0.0205(6) Uani 1 1 d . . .
H20A H 0.6037 0.1060 0.7462 0.025 Uiso 1 1 calc R . .
H20B H 0.6561 0.0492 0.8373 0.025 Uiso 1 1 calc R . .
S21 S 0.54110(8) -0.04252(7) 0.79751(6) 0.02230(18) Uani 1 1 d . . .
C22 C 0.5630(3) -0.0680(3) 0.6645(3) 0.0222(7) Uani 1 1 d . . .
H22A H 0.5196 -0.1185 0.6628 0.027 Uiso 1 1 calc R . .
H22B H 0.5153 0.0022 0.6385 0.027 Uiso 1 1 calc R . .
C23 C 0.7139(3) -0.1181(3) 0.5932(2) 0.0204(6) Uani 1 1 d . . .
H23A H 0.7611 -0.1896 0.6175 0.025 Uiso 1 1 calc R . .
H23B H 0.7210 -0.1318 0.5219 0.025 Uiso 1 1 calc R . .
N24 N 0.8028(2) 0.41471(19) 0.15685(18) 0.0124(5) Uani 1 1 d . . .
C25 C 0.6741(3) 0.4927(2) 0.1860(2) 0.0123(5) Uani 1 1 d . . .
C26 C 0.6256(3) 0.5698(2) 0.1229(2) 0.0150(6) Uani 1 1 d . . .
H26 H 0.5336 0.6239 0.1483 0.018 Uiso 1 1 calc R . .
C27 C 0.7148(3) 0.5672(2) 0.0194(2) 0.0143(6) Uani 1 1 d . . .
C28 C 0.8501(3) 0.4820(2) -0.0132(2) 0.0138(6) Uani 1 1 d . . .
H28 H 0.9139 0.4744 -0.0825 0.017 Uiso 1 1 calc R . .
C29 C 0.8858(3) 0.4112(2) 0.0583(2) 0.0131(5) Uani 1 1 d . . .
N30 N 0.5900(2) 0.48370(19) 0.28701(18) 0.0129(5) Uani 1 1 d . . .
N31 N 0.6417(2) 0.3906(2) 0.33402(19) 0.0136(5) Uani 1 1 d . . .
C32 C 0.5348(3) 0.3909(3) 0.4163(2) 0.0166(6) Uani 1 1 d . . .
H32 H 0.5394 0.3358 0.4644 0.020 Uiso 1 1 calc R . .
C33 C 0.4140(3) 0.4829(3) 0.4233(2) 0.0191(6) Uani 1 1 d . . .
H33 H 0.3244 0.5013 0.4751 0.023 Uiso 1 1 calc R . .
C34 C 0.4520(3) 0.5406(3) 0.3397(2) 0.0170(6) Uani 1 1 d . . .
H34 H 0.3935 0.6072 0.3219 0.020 Uiso 1 1 calc R . .
N35 N 1.0173(2) 0.3240(2) 0.03288(18) 0.0133(5) Uani 1 1 d . . .
N36 N 1.0479(2) 0.2611(2) 0.11013(19) 0.0144(5) Uani 1 1 d . . .
C37 C 1.1750(3) 0.1856(2) 0.0622(2) 0.0168(6) Uani 1 1 d . . .
H37 H 1.2247 0.1292 0.0961 0.020 Uiso 1 1 calc R . .
C38 C 1.2268(3) 0.1994(3) -0.0443(2) 0.0181(6) Uani 1 1 d . . .
H38 H 1.3147 0.1562 -0.0945 0.022 Uiso 1 1 calc R . .
C39 C 1.1238(3) 0.2882(3) -0.0607(2) 0.0170(6) Uani 1 1 d . . .
H39 H 1.1261 0.3191 -0.1251 0.020 Uiso 1 1 calc R . .
N40 N 0.6743(3) 0.6426(2) -0.04547(19) 0.0163(5) Uani 1 1 d . . .
C41 C 0.5341(3) 0.7267(3) -0.0149(2) 0.0195(6) Uani 1 1 d . . .
H41A H 0.5359 0.7956 -0.0464 0.023 Uiso 1 1 calc R . .
H41B H 0.4932 0.7418 0.0617 0.023 Uiso 1 1 calc R . .
C42 C 0.4459(3) 0.6898(3) -0.0497(3) 0.0224(7) Uani 1 1 d . . .
H42A H 0.3497 0.7458 -0.0236 0.027 Uiso 1 1 calc R . .
H42B H 0.4459 0.6200 -0.0193 0.027 Uiso 1 1 calc R . .
S43 S 0.50845(8) 0.66977(7) -0.18969(6) 0.02325(18) Uani 1 1 d . . .
C44 C 0.6862(3) 0.5790(3) -0.2119(3) 0.0218(6) Uani 1 1 d . . .
H44A H 0.6905 0.5070 -0.1852 0.026 Uiso 1 1 calc R . .
H44B H 0.7410 0.5667 -0.2876 0.026 Uiso 1 1 calc R . .
C45 C 0.7483(3) 0.6275(3) -0.1581(2) 0.0182(6) Uani 1 1 d . . .
H45A H 0.8464 0.5778 -0.1743 0.022 Uiso 1 1 calc R . .
H45B H 0.7446 0.6993 -0.1852 0.022 Uiso 1 1 calc R . .
B46 B 0.1650(4) 0.8038(3) 0.1871(3) 0.0213(7) Uani 1 1 d . . .
F47 F 0.1916(2) 0.88443(17) 0.12449(15) 0.0295(5) Uani 1 1 d . . .
F48 F 0.1329(2) 0.73909(19) 0.13691(17) 0.0364(5) Uani 1 1 d . . .
F49 F 0.2812(2) 0.73815(18) 0.21052(17) 0.0345(5) Uani 1 1 d . . .
F50 F 0.0564(2) 0.85265(18) 0.28018(15) 0.0333(5) Uani 1 1 d . . .
B51 B 0.6364(4) 0.7569(4) 0.3716(4) 0.0369(10) Uani 1 1 d D . .
F52A F 0.5967(5) 0.7502(4) 0.2892(4) 0.0714(14) Uiso 0.67 1 d PD A 1
F53A F 0.5210(5) 0.8122(4) 0.4532(4) 0.0630(14) Uiso 0.67 1 d PD A 1
F54A F 0.7270(4) 0.8119(3) 0.3401(3) 0.0338(9) Uiso 0.67 1 d PD A 1
F55A F 0.7106(3) 0.6508(3) 0.3858(3) 0.0344(8) Uiso 0.67 1 d PD A 1
F52B F 0.5500(11) 0.7433(9) 0.3399(9) 0.083(3) Uiso 0.33 1 d PD A 2
F53B F 0.5503(8) 0.8200(6) 0.4737(6) 0.0383(18) Uiso 0.33 1 d PD A 2
F54B F 0.7143(8) 0.8087(6) 0.3106(6) 0.037(2) Uiso 0.33 1 d PD A 2
F55B F 0.7243(8) 0.6701(6) 0.4208(7) 0.049(2) Uiso 0.33 1 d PD A 2
O56 O 0.9935(3) 0.6089(2) 0.2660(2) 0.0388(6) Uani 1 1 d D . .
H56A H 0.894(2) 0.628(4) 0.277(4) 0.058 Uiso 1 1 d D . .
H56B H 1.012(4) 0.665(3) 0.235(4) 0.058 Uiso 1 1 d 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 N24 2.109(2) . ?
Fe1 N2 2.115(2) . ?
Fe1 N14 2.167(2) . ?
Fe1 N31 2.189(2) . ?
Fe1 N9 2.206(2) . ?
Fe1 N36 2.228(2) . ?
N2 C3 1.333(4) . ?
N2 C7 1.333(4) . ?
C3 C4 1.367(4) . ?
C3 N8 1.415(4) . ?
C4 C5 1.424(4) . ?
C5 N18 1.358(4) . ?
C5 C6 1.418(4) . ?
C6 C7 1.369(4) . ?
C7 N13 1.412(4) . ?
N8 C12 1.358(4) . ?
N8 N9 1.368(3) . ?
N9 C10 1.331(4) . ?
C10 C11 1.402(4) . ?
C11 C12 1.368(4) . ?
N13 C17 1.357(4) . ?
N13 N14 1.369(3) . ?
N14 C15 1.323(4) . ?
C15 C16 1.402(4) . ?
C16 C17 1.369(4) . ?
N18 C19 1.462(4) . ?
N18 C23 1.469(4) . ?
C19 C20 1.517(4) . ?
C20 S21 1.814(3) . ?
S21 C22 1.812(3) . ?
C22 C23 1.518(4) . ?
N24 C29 1.336(4) . ?
N24 C25 1.340(4) . ?
C25 C26 1.372(4) . ?
C25 N30 1.403(4) . ?
C26 C27 1.412(4) . ?
C27 N40 1.349(4) . ?
C27 C28 1.423(4) . ?
C28 C29 1.370(4) . ?
C29 N35 1.411(4) . ?
N30 C34 1.364(4) . ?
N30 N31 1.369(3) . ?
N31 C32 1.325(4) . ?
C32 C33 1.403(4) . ?
C33 C34 1.370(4) . ?
N35 C39 1.361(4) . ?
N35 N36 1.367(3) . ?
N36 C37 1.332(4) . ?
C37 C38 1.403(4) . ?
C38 C39 1.364(4) . ?
N40 C41 1.457(4) . ?
N40 C45 1.461(4) . ?
C41 C42 1.513(4) . ?
C42 S43 1.806(3) . ?
S43 C44 1.813(3) . ?
C44 C45 1.523(4) . ?
B46 F48 1.381(4) . ?
B46 F47 1.385(4) . ?
B46 F50 1.388(4) . ?
B46 F49 1.402(4) . ?
B51 F53A 1.343(6) . ?
B51 F55A 1.366(5) . ?
B51 F52A 1.399(7) . ?
B51 F54A 1.424(6) . ?
B51 F52B 1.295(9) . ?
B51 F54B 1.352(8) . ?
B51 F53B 1.475(8) . ?
B51 F55B 1.502(8) . ?
O56 H56A 1.006(19) . ?
O56 H56B 0.897(19) . ?

loop_
_geom_angle_atom_site_label_1
_geom_angle_atom_site_label_2
_geom_angle_atom_site_label_3
_geom_angle
_geom_angle_site_symmetry_1
_geom_angle_site_symmetry_3
_geom_angle_publ_flag
N24 Fe1 N2 162.78(9) . . ?
N24 Fe1 N14 101.65(9) . . ?
N2 Fe1 N14 72.33(9) . . ?
N24 Fe1 N31 72.91(9) . . ?
N2 Fe1 N31 92.22(9) . . ?
N14 Fe1 N31 101.65(9) . . ?
N24 Fe1 N9 115.30(9) . . ?
N2 Fe1 N9 73.25(9) . . ?
N14 Fe1 N9 142.82(9) . . ?
N31 Fe1 N9 93.25(9) . . ?
N24 Fe1 N36 73.06(9) . . ?
N2 Fe1 N36 121.61(9) . . ?
N14 Fe1 N36 86.52(9) . . ?
N31 Fe1 N36 145.93(9) . . ?
N9 Fe1 N36 99.90(9) . . ?
C3 N2 C7 116.6(2) . . ?
C3 N2 Fe1 120.90(19) . . ?
C7 N2 Fe1 121.33(19) . . ?
N2 C3 C4 125.0(3) . . ?
N2 C3 N8 112.3(2) . . ?
C4 C3 N8 122.7(3) . . ?
C3 C4 C5 118.0(3) . . ?
N18 C5 C6 121.7(3) . . ?
N18 C5 C4 120.9(3) . . ?
C6 C5 C4 117.3(3) . . ?
C7 C6 C5 118.0(3) . . ?
N2 C7 C6 125.0(3) . . ?
N2 C7 N13 111.6(2) . . ?
C6 C7 N13 123.3(3) . . ?
C12 N8 N9 111.4(2) . . ?
C12 N8 C3 129.8(2) . . ?
N9 N8 C3 118.7(2) . . ?
C10 N9 N8 104.9(2) . . ?
C10 N9 Fe1 141.6(2) . . ?
N8 N9 Fe1 113.10(17) . . ?
N9 C10 C11 111.2(3) . . ?
C12 C11 C10 105.7(3) . . ?
N8 C12 C11 106.8(3) . . ?
C17 N13 N14 111.2(2) . . ?
C17 N13 C7 131.3(2) . . ?
N14 N13 C7 117.1(2) . . ?
C15 N14 N13 105.2(2) . . ?
C15 N14 Fe1 139.4(2) . . ?
N13 N14 Fe1 115.26(17) . . ?
N14 C15 C16 111.2(3) . . ?
C17 C16 C15 105.5(3) . . ?
N13 C17 C16 106.9(3) . . ?
C5 N18 C19 121.1(3) . . ?
C5 N18 C23 123.2(3) . . ?
C19 N18 C23 112.8(2) . . ?
N18 C19 C20 111.4(3) . . ?
H19A C19 H19B 108.0 . . ?
C19 C20 S21 110.1(2) . . ?
C22 S21 C20 98.20(15) . . ?
C23 C22 S21 112.1(2) . . ?
N18 C23 C22 111.5(3) . . ?
C29 N24 C25 116.4(2) . . ?
C29 N24 Fe1 120.96(19) . . ?
C25 N24 Fe1 121.56(19) . . ?
N24 C25 C26 124.4(3) . . ?
N24 C25 N30 112.7(2) . . ?
C26 C25 N30 122.8(3) . . ?
C25 C26 C27 118.9(3) . . ?
N40 C27 C26 121.6(3) . . ?
N40 C27 C28 121.4(3) . . ?
C26 C27 C28 117.0(3) . . ?
C29 C28 C27 118.1(3) . . ?
N24 C29 C28 125.2(3) . . ?
N24 C29 N35 112.7(2) . . ?
C28 C29 N35 122.1(3) . . ?
C34 N30 N31 111.2(2) . . ?
C34 N30 C25 129.9(2) . . ?
N31 N30 C25 117.2(2) . . ?
C32 N31 N30 105.1(2) . . ?
C32 N31 Fe1 139.8(2) . . ?
N30 N31 Fe1 114.90(17) . . ?
N31 C32 C33 111.3(3) . . ?
C34 C33 C32 105.6(3) . . ?
N30 C34 C33 106.7(3) . . ?
C39 N35 N36 111.6(2) . . ?
C39 N35 C29 129.8(2) . . ?
N36 N35 C29 118.5(2) . . ?
C37 N36 N35 104.4(2) . . ?
C37 N36 Fe1 140.1(2) . . ?
N35 N36 Fe1 111.98(17) . . ?
N36 C37 C38 111.7(3) . . ?
C39 C38 C37 105.3(3) . . ?
N35 C39 C38 107.0(3) . . ?
C27 N40 C41 121.9(2) . . ?
C27 N40 C45 122.9(3) . . ?
C41 N40 C45 112.5(2) . . ?
N40 C41 C42 110.8(3) . . ?
C41 C42 S43 111.6(2) . . ?
C42 S43 C44 97.96(15) . . ?
C45 C44 S43 111.3(2) . . ?
N40 C45 C44 111.3(2) . . ?
F48 B46 F47 110.1(3) . . ?
F48 B46 F50 110.0(3) . . ?
F47 B46 F50 109.6(3) . . ?
F48 B46 F49 109.7(3) . . ?
F47 B46 F49 109.6(3) . . ?
F50 B46 F49 107.8(3) . . ?
F53A B51 F55A 115.4(4) . . ?
F53A B51 F52A 107.4(4) . . ?
F55A B51 F52A 105.6(4) . . ?
F53A B51 F54A 111.7(4) . . ?
F55A B51 F54A 107.6(3) . . ?
F52A B51 F54A 108.7(4) . . ?
F52B B51 F54B 117.9(7) . . ?
F52B B51 F53B 104.6(7) . . ?
F54B B51 F53B 109.5(6) . . ?
F52B B51 F55B 123.5(7) . . ?
F54B B51 F55B 107.0(5) . . ?
F53B B51 F55B 89.9(5) . . ?
H56A O56 H56B 106(2) . . ?

loop_
_geom_hbond_atom_site_label_D
_geom_hbond_atom_site_label_H
_geom_hbond_atom_site_label_A
_geom_hbond_distance_DH
_geom_hbond_distance_HA
_geom_hbond_distance_DA
_geom_hbond_angle_DHA
_geom_hbond_site_symmetry_A
O56 H56A F55A 1.006(19) 1.99(3) 2.866(4) 144(4) .
O56 H56A F55B 1.006(19) 2.12(4) 2.843(9) 127(4) .
O56 H56B F48 0.897(19) 2.05(2) 2.892(4) 156(4) 1_655

_diffrn_measured_fraction_theta_max 0.807
_diffrn_reflns_theta_full        29.83
_diffrn_measured_fraction_theta_full 0.807
_refine_diff_density_max         1.511
_refine_diff_density_min         -1.062
_refine_diff_density_rms         0.095
_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_as148226
_database_code_depnum_ccdc_archive 'CCDC 1058750'
_audit_update_record             
;
2015-04-09 deposited with the CCDC.
2015-05-27 downloaded from the CCDC.
;

_audit_creation_method           SHELXL-97
_chemical_name_systematic        
'Bis[2,6-di(pyrazol-1-yl)-4-(thiomorpholin-1-yl)pyridine]iron(II) diperchlorate hydrate (1/0.33)'
_chemical_name_common            ?
_chemical_melting_point          ?
_chemical_formula_moiety         'C30 H32 Fe N12 S2, 2[Cl O4], 0.33[H2 O]'
_chemical_formula_sum            'C30 H32.66 Cl2 Fe N12 O8.33 S2'
_chemical_formula_weight         885.49

loop_
_atom_type_symbol
_atom_type_description
_atom_type_scat_dispersion_real
_atom_type_scat_dispersion_imag
_atom_type_scat_source
C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
S S 0.1246 0.1234 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Cl Cl 0.1484 0.1585 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Fe Fe 0.3463 0.8444 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'

_symmetry_cell_setting           Triclinic
_symmetry_space_group_name_H-M   'P -1'

loop_
_symmetry_equiv_pos_as_xyz
'x, y, z'
'-x, -y, -z'

_cell_length_a                   11.5334(6)
_cell_length_b                   13.2237(7)
_cell_length_c                   14.0842(8)
_cell_angle_alpha                85.594(4)
_cell_angle_beta                 68.230(5)
_cell_angle_gamma                65.418(5)
_cell_volume                     1806.40(17)
_cell_formula_units_Z            2
_cell_measurement_temperature    100(2)
_cell_measurement_reflns_used    4850
_cell_measurement_theta_min      3.30
_cell_measurement_theta_max      27.86

_exptl_crystal_description       block
_exptl_crystal_colour            yellow
_exptl_crystal_size_max          0.28
_exptl_crystal_size_mid          0.23
_exptl_crystal_size_min          0.12
_exptl_crystal_density_meas      ?
_exptl_crystal_density_diffrn    1.628
_exptl_crystal_density_method    'not measured'
_exptl_crystal_F_000             911
_exptl_absorpt_coefficient_mu    0.751
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_correction_T_min  0.961
_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     0.71073
_diffrn_radiation_type           MoK\a
_diffrn_radiation_source         'SuperNova (Mo) 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            21938
_diffrn_reflns_av_R_equivalents  0.0648
_diffrn_reflns_av_sigmaI/netI    0.0985
_diffrn_reflns_limit_h_min       -16
_diffrn_reflns_limit_h_max       12
_diffrn_reflns_limit_k_min       -17
_diffrn_reflns_limit_k_max       18
_diffrn_reflns_limit_l_min       -19
_diffrn_reflns_limit_l_max       19
_diffrn_reflns_theta_min         3.13
_diffrn_reflns_theta_max         29.70
_reflns_number_total             8768
_reflns_number_gt                6122
_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 two perchlorate ions, Cl51-O55, is disordered over two sites, 
 whose occupancies refined to 0.67 and 0.33. These were refined without 
 restraints. Another significant Fourier peak that is not bonded to 
 any other residue was modelled as a partial water molecule (O56) whose 
 occupancy refined to approximately 0.33. This partial water site lies 
 within hydrogen bonding distance of the disordered anion, and of the 
 symmetry equivalent of the other, ordered anion Cl46-O50 related by 
 1+x, y, z. The anion disorder  clearly correlates with the presence or 
 absence of O56, so O56 was refined with the same occupancy as the minor 
 disorder residue in the final least squares cycles. 

 All non-H atoms except the minor anion disorder site were refined 
 anisotropically, and C-bound H atoms were placed in calculated positions 
 and refined using a riding model. Although the partial H atoms associated 
 with this water site could not be located or refined, the water H content 
 is included in the density and F000 calculations. There are two unfeasibly 
 short intramolecular H...H distances in the final model, H4...H19A = 1.88 Å 
 and H4...H23B = 1.95 Å , which imply that the calculated positions of 
 these H atoms may differ from their true positions in the molecule.
;

_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)+(0.0318P)²+0.2723P] 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         8768
_refine_ls_number_parameters     521
_refine_ls_number_restraints     0
_refine_ls_R_factor_all          0.0948
_refine_ls_R_factor_gt           0.0584
_refine_ls_wR_factor_ref         0.1158
_refine_ls_wR_factor_gt          0.0994
_refine_ls_goodness_of_fit_ref   1.046
_refine_ls_restrained_S_all      1.046
_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 0.85767(4) 0.28789(3) 0.25305(3) 0.01288(11) Uani 1 1 d . . .
N2 N 0.8530(2) 0.16510(19) 0.35857(18) 0.0137(5) Uani 1 1 d . . .
C3 C 0.8607(3) 0.1759(2) 0.4492(2) 0.0128(6) Uani 1 1 d . . .
C4 C 0.8351(3) 0.1122(2) 0.5285(2) 0.0153(6) Uani 1 1 d . . .
H4 H 0.8423 0.1244 0.5913 0.018 Uiso 1 1 calc R . .
C5 C 0.7969(3) 0.0264(2) 0.5137(2) 0.0153(6) Uani 1 1 d . . .
C6 C 0.7844(3) 0.0161(2) 0.4190(2) 0.0165(6) Uani 1 1 d . . .
H6 H 0.7551 -0.0372 0.4065 0.020 Uiso 1 1 calc R . .
C7 C 0.8157(3) 0.0852(2) 0.3461(2) 0.0137(6) Uani 1 1 d . . .
N8 N 0.9029(2) 0.26171(19) 0.45374(18) 0.0138(5) Uani 1 1 d . . .
N9 N 0.9177(2) 0.32588(19) 0.37293(18) 0.0140(5) Uani 1 1 d . . .
C10 C 0.9604(3) 0.3953(2) 0.3983(2) 0.0165(6) Uani 1 1 d . . .
H10 H 0.9785 0.4514 0.3572 0.020 Uiso 1 1 calc R . .
C11 C 0.9753(3) 0.3754(2) 0.4931(2) 0.0189(7) Uani 1 1 d . . .
H11 H 1.0053 0.4134 0.5269 0.023 Uiso 1 1 calc R . .
C12 C 0.9379(3) 0.2900(2) 0.5267(2) 0.0183(7) Uani 1 1 d . . .
H12 H 0.9364 0.2567 0.5892 0.022 Uiso 1 1 calc R . .
N13 N 0.8149(2) 0.0782(2) 0.24704(18) 0.0145(5) Uani 1 1 d . . .
N14 N 0.8429(2) 0.1560(2) 0.18258(18) 0.0155(5) Uani 1 1 d . . .
C15 C 0.8495(3) 0.1237(2) 0.0934(2) 0.0172(6) Uani 1 1 d . . .
H15 H 0.8678 0.1616 0.0334 0.021 Uiso 1 1 calc R . .
C16 C 0.8264(3) 0.0277(3) 0.0977(2) 0.0196(7) Uani 1 1 d . . .
H16 H 0.8251 -0.0103 0.0437 0.023 Uiso 1 1 calc R . .
C17 C 0.8060(3) -0.0001(3) 0.1963(2) 0.0186(7) Uani 1 1 d . . .
H17 H 0.7888 -0.0625 0.2242 0.022 Uiso 1 1 calc R . .
N18 N 0.7798(2) -0.0455(2) 0.58709(18) 0.0185(6) Uani 1 1 d . . .
C19 C 0.7847(3) -0.0299(3) 0.6868(2) 0.0180(7) Uani 1 1 d . . .
H19A H 0.8429 0.0101 0.6798 0.022 Uiso 1 1 calc R . .
H19B H 0.8266 -0.1037 0.7109 0.022 Uiso 1 1 calc R . .
C20 C 0.6410(3) 0.0365(2) 0.7655(2) 0.0225(7) Uani 1 1 d . . .
H20A H 0.5968 0.1086 0.7398 0.027 Uiso 1 1 calc R . .
H20B H 0.6473 0.0524 0.8305 0.027 Uiso 1 1 calc R . .
S21 S 0.53773(8) -0.04189(7) 0.78888(6) 0.0245(2) Uani 1 1 d . . .
C22 C 0.5615(3) -0.0678(3) 0.6568(2) 0.0229(7) Uani 1 1 d . . .
H22A H 0.5194 -0.1187 0.6539 0.028 Uiso 1 1 calc R . .
H22B H 0.5137 0.0035 0.6316 0.028 Uiso 1 1 calc R . .
C23 C 0.7128(3) -0.1192(2) 0.5869(2) 0.0208(7) Uani 1 1 d . . .
H23A H 0.7601 -0.1920 0.6103 0.025 Uiso 1 1 calc R . .
H23B H 0.7211 -0.1329 0.5160 0.025 Uiso 1 1 calc R . .
N24 N 0.8047(2) 0.41343(19) 0.15567(18) 0.0131(5) Uani 1 1 d . . .
C25 C 0.6764(3) 0.4928(2) 0.1801(2) 0.0144(6) Uani 1 1 d . . .
C26 C 0.6304(3) 0.5682(2) 0.1158(2) 0.0161(6) Uani 1 1 d . . .
H26 H 0.5385 0.6238 0.1387 0.019 Uiso 1 1 calc R . .
C27 C 0.7241(3) 0.5610(2) 0.0135(2) 0.0163(6) Uani 1 1 d . . .
C28 C 0.8587(3) 0.4752(2) -0.0140(2) 0.0174(7) Uani 1 1 d . . .
H28 H 0.9250 0.4655 -0.0815 0.021 Uiso 1 1 calc R . .
C29 C 0.8909(3) 0.4070(2) 0.0582(2) 0.0145(6) Uani 1 1 d . . .
N30 N 0.5899(2) 0.48794(19) 0.28088(17) 0.0132(5) Uani 1 1 d . . .
N31 N 0.6402(2) 0.39645(19) 0.33025(18) 0.0136(5) Uani 1 1 d . . .
C32 C 0.5316(3) 0.4018(2) 0.4123(2) 0.0172(7) Uani 1 1 d . . .
H32 H 0.5345 0.3488 0.4618 0.021 Uiso 1 1 calc R . .
C33 C 0.4129(3) 0.4952(3) 0.4163(2) 0.0192(7) Uani 1 1 d . . .
H33 H 0.3233 0.5171 0.4675 0.023 Uiso 1 1 calc R . .
C34 C 0.4522(3) 0.5485(3) 0.3318(2) 0.0194(7) Uani 1 1 d . . .
H34 H 0.3948 0.6149 0.3121 0.023 Uiso 1 1 calc R . .
N35 N 1.0227(2) 0.3179(2) 0.03799(18) 0.0154(5) Uani 1 1 d . . .
N36 N 1.0488(2) 0.2579(2) 0.11662(18) 0.0160(5) Uani 1 1 d . . .
C37 C 1.1765(3) 0.1803(3) 0.0728(2) 0.0212(7) Uani 1 1 d . . .
H37 H 1.2240 0.1252 0.1086 0.025 Uiso 1 1 calc R . .
C38 C 1.2326(3) 0.1897(3) -0.0327(2) 0.0223(7) Uani 1 1 d . . .
H38 H 1.3216 0.1441 -0.0802 0.027 Uiso 1 1 calc R . .
C39 C 1.1318(3) 0.2782(3) -0.0523(2) 0.0205(7) Uani 1 1 d . . .
H39 H 1.1369 0.3069 -0.1169 0.025 Uiso 1 1 calc R . .
N40 N 0.6868(3) 0.6340(2) -0.05336(19) 0.0208(6) Uani 1 1 d . . .
C41 C 0.5492(3) 0.7237(3) -0.0261(2) 0.0240(7) Uani 1 1 d . . .
H41A H 0.5557 0.7909 -0.0593 0.029 Uiso 1 1 calc R . .
H41B H 0.5076 0.7427 0.0491 0.029 Uiso 1 1 calc R . .
C42 C 0.4575(3) 0.6916(3) -0.0589(2) 0.0257(8) Uani 1 1 d . . .
H42A H 0.3636 0.7524 -0.0347 0.031 Uiso 1 1 calc R . .
H42B H 0.4521 0.6236 -0.0268 0.031 Uiso 1 1 calc R . .
S43 S 0.52196(9) 0.66557(7) -0.19694(6) 0.0269(2) Uani 1 1 d . . .
C44 C 0.6968(3) 0.5682(3) -0.2158(2) 0.0248(7) Uani 1 1 d . . .
H44A H 0.6965 0.4974 -0.1874 0.030 Uiso 1 1 calc R . .
H44B H 0.7524 0.5515 -0.2903 0.030 Uiso 1 1 calc R . .
C45 C 0.7627(3) 0.6128(3) -0.1652(2) 0.0260(8) Uani 1 1 d . . .
H45A H 0.8588 0.5582 -0.1800 0.031 Uiso 1 1 calc R . .
H45B H 0.7644 0.6831 -0.1940 0.031 Uiso 1 1 calc R . .
Cl46 Cl 0.16867(7) 0.80771(6) 0.18263(6) 0.02124(18) Uani 1 1 d . . .
O47 O 0.1884(2) 0.89590(19) 0.12167(17) 0.0294(6) Uani 1 1 d . . .
O48 O 0.1393(3) 0.7394(2) 0.12858(18) 0.0348(6) Uani 1 1 d . . .
O49 O 0.2909(2) 0.7407(2) 0.20284(19) 0.0376(6) Uani 1 1 d . . .
O50 O 0.0567(2) 0.8557(2) 0.27945(17) 0.0322(6) Uani 1 1 d . . .
Cl51A Cl 0.72895(14) 0.69802(10) 0.35002(9) 0.0257(3) Uani 0.67 1 d P A 1
O52A O 0.8406(4) 0.6145(3) 0.2689(3) 0.0495(11) Uani 0.67 1 d P A 1
O53A O 0.7379(4) 0.6648(3) 0.4464(3) 0.0388(10) Uani 0.67 1 d P A 1
O54A O 0.7247(9) 0.8064(8) 0.3338(8) 0.0336(18) Uani 0.67 1 d P A 1
O55A O 0.5990(5) 0.7080(5) 0.3498(4) 0.0660(14) Uani 0.67 1 d P A 1
Cl51B Cl 0.6365(3) 0.7468(2) 0.36689(19) 0.0205(5) Uiso 0.33 1 d P B 2
O52B O 0.6081(9) 0.7420(7) 0.2792(7) 0.047(2) Uiso 0.33 1 d P B 2
O53B O 0.5161(8) 0.8076(7) 0.4511(6) 0.044(2) Uiso 0.33 1 d P B 2
O54B O 0.7514(19) 0.798(2) 0.3395(17) 0.028(4) Uiso 0.33 1 d P B 2
O55B O 0.7058(7) 0.6345(7) 0.3913(6) 0.0344(18) Uiso 0.33 1 d P B 2
O56 O 1.0005(7) 0.6143(6) 0.2652(5) 0.0279(16) Uiso 0.33 1 d P . .


_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 N24 2.107(2) . ?
Fe1 N2 2.119(2) . ?
Fe1 N14 2.167(2) . ?
Fe1 N31 2.180(2) . ?
Fe1 N9 2.207(2) . ?
Fe1 N36 2.227(2) . ?
N2 C3 1.334(4) . ?
N2 C7 1.340(4) . ?
C3 C4 1.365(4) . ?
C3 N8 1.423(4) . ?
C4 C5 1.431(4) . ?
C5 N18 1.365(4) . ?
C5 C6 1.416(4) . ?
C6 C7 1.370(4) . ?
C7 N13 1.409(4) . ?
N8 C12 1.361(4) . ?
N8 N9 1.369(3) . ?
N9 C10 1.331(4) . ?
C10 C11 1.399(4) . ?
C11 C12 1.363(4) . ?
N13 C17 1.360(4) . ?
N13 N14 1.379(3) . ?
N14 C15 1.322(4) . ?
C15 C16 1.394(4) . ?
C16 C17 1.368(4) . ?
N18 C19 1.459(4) . ?
N18 C23 1.476(4) . ?
C19 C20 1.524(4) . ?
C20 S21 1.812(3) . ?
S21 C22 1.816(3) . ?
C22 C23 1.522(4) . ?
N24 C25 1.340(4) . ?
N24 C29 1.348(4) . ?
C25 C26 1.368(4) . ?
C25 N30 1.415(3) . ?
C26 C27 1.426(4) . ?
C27 N40 1.349(4) . ?
C27 C28 1.415(4) . ?
C28 C29 1.359(4) . ?
C29 N35 1.422(4) . ?
N30 C34 1.365(3) . ?
N30 N31 1.368(3) . ?
N31 C32 1.332(3) . ?
C32 C33 1.396(4) . ?
C33 C34 1.362(4) . ?
N35 C39 1.357(4) . ?
N35 N36 1.364(3) . ?
N36 C37 1.330(4) . ?
C37 C38 1.402(4) . ?
C38 C39 1.362(4) . ?
N40 C41 1.458(4) . ?
N40 C45 1.472(4) . ?
C41 C42 1.508(4) . ?
C42 S43 1.808(3) . ?
S43 C44 1.814(3) . ?
C44 C45 1.508(4) . ?
Cl46 O48 1.436(2) . ?
Cl46 O47 1.439(2) . ?
Cl46 O49 1.440(2) . ?
Cl46 O50 1.440(2) . ?
Cl51A O54A 1.417(10) . ?
Cl51A O53A 1.422(4) . ?
Cl51A O52A 1.450(4) . ?
Cl51A O55A 1.450(5) . ?
Cl51B O52B 1.403(10) . ?
Cl51B O53B 1.406(8) . ?
Cl51B O55B 1.450(8) . ?
Cl51B O54B 1.64(2) . ?

loop_
_geom_angle_atom_site_label_1
_geom_angle_atom_site_label_2
_geom_angle_atom_site_label_3
_geom_angle
_geom_angle_site_symmetry_1
_geom_angle_site_symmetry_3
_geom_angle_publ_flag
N24 Fe1 N2 163.22(9) . . ?
N24 Fe1 N14 99.27(9) . . ?
N2 Fe1 N14 72.63(9) . . ?
N24 Fe1 N31 72.98(9) . . ?
N2 Fe1 N31 93.65(9) . . ?
N14 Fe1 N31 100.22(9) . . ?
N24 Fe1 N9 117.23(9) . . ?
N2 Fe1 N9 72.93(9) . . ?
N14 Fe1 N9 143.31(9) . . ?
N31 Fe1 N9 94.21(9) . . ?
N24 Fe1 N36 73.10(9) . . ?
N2 Fe1 N36 120.05(9) . . ?
N14 Fe1 N36 87.05(9) . . ?
N31 Fe1 N36 146.02(9) . . ?
N9 Fe1 N36 99.47(9) . . ?
C3 N2 C7 116.3(2) . . ?
C3 N2 Fe1 121.53(19) . . ?
C7 N2 Fe1 120.9(2) . . ?
N2 C3 C4 125.5(3) . . ?
N2 C3 N8 111.7(2) . . ?
C4 C3 N8 122.7(3) . . ?
C3 C4 C5 117.5(3) . . ?
N18 C5 C6 122.0(3) . . ?
N18 C5 C4 120.4(3) . . ?
C6 C5 C4 117.6(3) . . ?
C7 C6 C5 118.0(3) . . ?
N2 C7 C6 124.9(3) . . ?
N2 C7 N13 111.9(2) . . ?
C6 C7 N13 123.1(3) . . ?
C12 N8 N9 111.6(2) . . ?
C12 N8 C3 129.8(2) . . ?
N9 N8 C3 118.5(2) . . ?
C10 N9 N8 104.4(2) . . ?
C10 N9 Fe1 141.8(2) . . ?
N8 N9 Fe1 113.76(17) . . ?
N9 C10 C11 111.6(3) . . ?
C12 C11 C10 105.6(3) . . ?
N8 C12 C11 106.8(3) . . ?
C17 N13 N14 110.8(2) . . ?
C17 N13 C7 131.6(2) . . ?
N14 N13 C7 117.1(2) . . ?
C15 N14 N13 104.5(2) . . ?
C15 N14 Fe1 140.3(2) . . ?
N13 N14 Fe1 115.21(18) . . ?
N14 C15 C16 112.3(3) . . ?
C17 C16 C15 105.1(3) . . ?
N13 C17 C16 107.3(3) . . ?
C5 N18 C19 121.4(2) . . ?
C5 N18 C23 122.7(3) . . ?
C19 N18 C23 113.1(2) . . ?
N18 C19 C20 111.0(3) . . ?
C19 C20 S21 110.1(2) . . ?
C20 S21 C22 98.07(14) . . ?
C23 C22 S21 112.0(2) . . ?
N18 C23 C22 111.3(2) . . ?
C25 N24 C29 115.6(3) . . ?
C25 N24 Fe1 121.97(18) . . ?
C29 N24 Fe1 121.46(19) . . ?
N24 C25 C26 125.2(3) . . ?
N24 C25 N30 111.9(3) . . ?
C26 C25 N30 122.8(3) . . ?
C25 C26 C27 118.2(3) . . ?
N40 C27 C28 121.5(3) . . ?
N40 C27 C26 121.5(3) . . ?
C28 C27 C26 117.0(3) . . ?
C29 C28 C27 118.5(3) . . ?
N24 C29 C28 125.4(3) . . ?
N24 C29 N35 111.7(3) . . ?
C28 C29 N35 122.9(3) . . ?
C34 N30 N31 111.3(2) . . ?
C34 N30 C25 130.1(3) . . ?
N31 N30 C25 117.2(2) . . ?
C32 N31 N30 104.6(2) . . ?
C32 N31 Fe1 140.2(2) . . ?
N30 N31 Fe1 115.10(16) . . ?
N31 C32 C33 111.5(3) . . ?
C34 C33 C32 105.8(3) . . ?
C33 C34 N30 106.8(3) . . ?
C39 N35 N36 111.8(2) . . ?
C39 N35 C29 129.3(3) . . ?
N36 N35 C29 118.9(2) . . ?
C37 N36 N35 104.2(2) . . ?
C37 N36 Fe1 140.1(2) . . ?
N35 N36 Fe1 112.30(16) . . ?
N36 C37 C38 111.9(3) . . ?
C39 C38 C37 105.0(3) . . ?
N35 C39 C38 107.1(3) . . ?
C27 N40 C41 122.4(2) . . ?
C27 N40 C45 123.2(3) . . ?
C41 N40 C45 112.2(3) . . ?
N40 C41 C42 112.0(3) . . ?
C41 C42 S43 111.3(2) . . ?
C42 S43 C44 97.77(15) . . ?
C45 C44 S43 112.5(2) . . ?
N40 C45 C44 111.0(2) . . ?
O48 Cl46 O47 109.58(14) . . ?
O48 Cl46 O49 109.76(16) . . ?
O47 Cl46 O49 109.69(14) . . ?
O48 Cl46 O50 110.29(15) . . ?
O47 Cl46 O50 109.28(14) . . ?
O49 Cl46 O50 108.22(14) . . ?
O54A Cl51A O53A 111.9(4) . . ?
O54A Cl51A O52A 112.6(4) . . ?
O53A Cl51A O52A 109.5(2) . . ?
O54A Cl51A O55A 104.4(4) . . ?
O53A Cl51A O55A 109.2(3) . . ?
O52A Cl51A O55A 109.2(3) . . ?
O52B Cl51B O53B 111.5(5) . . ?
O52B Cl51B O55B 109.5(5) . . ?
O53B Cl51B O55B 110.4(5) . . ?
O52B Cl51B O54B 109.1(8) . . ?
O53B Cl51B O54B 112.6(9) . . ?
O55B Cl51B O54B 103.5(8) . . ?

_diffrn_measured_fraction_theta_max 0.854
_diffrn_reflns_theta_full        29.70
_diffrn_measured_fraction_theta_full 0.854
_refine_diff_density_max         0.583
_refine_diff_density_min         -0.509
_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_as149227
_database_code_depnum_ccdc_archive 'CCDC 1058751'
_audit_update_record             
;
2015-04-09 deposited with the CCDC.
2015-05-27 downloaded from the CCDC.
;

_audit_creation_method           SHELXL-97
_chemical_name_systematic        
'Bis[2,6-di(pyrazol-1-yl)-4-(thiomorpholin-1-yl)pyridine]iron(II) bis-trifluoromethanesulfonate'
_chemical_name_common            ?
_chemical_melting_point          ?
_chemical_formula_moiety         'C30 H32 Fe N12 S2, 2[C F3 O3 S]'
_chemical_formula_sum            'C32 H32 F6 Fe N12 O6 S4'
_chemical_formula_weight         978.79

loop_
_atom_type_symbol
_atom_type_description
_atom_type_scat_dispersion_real
_atom_type_scat_dispersion_imag
_atom_type_scat_source
C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
F F 0.0171 0.0103 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
S S 0.1246 0.1234 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Fe Fe 0.3463 0.8444 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'

_symmetry_cell_setting           Triclinic
_symmetry_space_group_name_H-M   'P -1'

loop_
_symmetry_equiv_pos_as_xyz
'x, y, z'
'-x, -y, -z'

_cell_length_a                   12.4186(7)
_cell_length_b                   13.3433(7)
_cell_length_c                   14.2652(6)
_cell_angle_alpha                75.472(4)
_cell_angle_beta                 67.419(5)
_cell_angle_gamma                64.190(5)
_cell_volume                     1954.89(17)
_cell_formula_units_Z            2
_cell_measurement_temperature    100(2)
_cell_measurement_reflns_used    4330
_cell_measurement_theta_min      3.69
_cell_measurement_theta_max      28.11

_exptl_crystal_description       block
_exptl_crystal_colour            yellow
_exptl_crystal_size_max          0.26
_exptl_crystal_size_mid          0.20
_exptl_crystal_size_min          0.14
_exptl_crystal_density_meas      ?
_exptl_crystal_density_diffrn    1.663
_exptl_crystal_density_method    'not measured'
_exptl_crystal_F_000             1000
_exptl_absorpt_coefficient_mu    0.690
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_correction_T_min  0.953
_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     0.71073
_diffrn_radiation_type           MoK\a
_diffrn_radiation_source         'SuperNova (Mo) 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            11920
_diffrn_reflns_av_R_equivalents  0.0326
_diffrn_reflns_av_sigmaI/netI    0.0789
_diffrn_reflns_limit_h_min       -14
_diffrn_reflns_limit_h_max       15
_diffrn_reflns_limit_k_min       -9
_diffrn_reflns_limit_k_max       18
_diffrn_reflns_limit_l_min       -19
_diffrn_reflns_limit_l_max       18
_diffrn_reflns_theta_min         3.13
_diffrn_reflns_theta_max         28.94
_reflns_number_total             8652
_reflns_number_gt                6663
_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 was detected during refinement, and no restraints were applied.
 All non-H atoms were refined anisotropically, while H atoms were placed in 
 calculated positions and refined using a riding model. The highest residual 
 Fourier peak of +1.1 e.Å⁻³ lies near the centroid of one of the triflate 
 anions.
;

_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)+(0.0323P)²+1.3457P] 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         8652
_refine_ls_number_parameters     550
_refine_ls_number_restraints     0
_refine_ls_R_factor_all          0.0719
_refine_ls_R_factor_gt           0.0520
_refine_ls_wR_factor_ref         0.1189
_refine_ls_wR_factor_gt          0.1037
_refine_ls_goodness_of_fit_ref   1.038
_refine_ls_restrained_S_all      1.038
_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 0.37852(4) 0.77413(3) 0.75622(3) 0.01201(11) Uani 1 1 d . . .
N2 N 0.5056(2) 0.65558(19) 0.64874(18) 0.0123(5) Uani 1 1 d . . .
C3 C 0.4886(3) 0.6621(2) 0.5607(2) 0.0119(6) Uani 1 1 d . . .
C4 C 0.5753(3) 0.5999(2) 0.4812(2) 0.0156(6) Uani 1 1 d . . .
H4 H 0.5579 0.6091 0.4196 0.019 Uiso 1 1 calc R . .
C5 C 0.6923(3) 0.5211(2) 0.4944(2) 0.0143(6) Uani 1 1 d . . .
C6 C 0.7116(3) 0.5145(2) 0.5877(2) 0.0138(6) Uani 1 1 d . . .
H6 H 0.7889 0.4651 0.5996 0.017 Uiso 1 1 calc R . .
C7 C 0.6159(3) 0.5809(2) 0.6604(2) 0.0135(6) Uani 1 1 d . . .
N8 N 0.3685(2) 0.7415(2) 0.55705(18) 0.0124(5) Uani 1 1 d . . .
N9 N 0.2926(2) 0.8059(2) 0.63717(19) 0.0144(5) Uani 1 1 d . . .
C10 C 0.1863(3) 0.8690(2) 0.6150(2) 0.0159(6) Uani 1 1 d . . .
H10 H 0.1157 0.9229 0.6565 0.019 Uiso 1 1 calc R . .
C11 C 0.1925(3) 0.8454(2) 0.5214(2) 0.0167(6) Uani 1 1 d . . .
H11 H 0.1290 0.8792 0.4891 0.020 Uiso 1 1 calc R . .
C12 C 0.3094(3) 0.7633(3) 0.4872(2) 0.0158(6) Uani 1 1 d . . .
H12 H 0.3426 0.7284 0.4263 0.019 Uiso 1 1 calc R . .
N13 N 0.6203(2) 0.5759(2) 0.75848(19) 0.0141(5) Uani 1 1 d . . .
N14 N 0.5169(2) 0.6456(2) 0.82527(19) 0.0148(5) Uani 1 1 d . . .
C15 C 0.5408(3) 0.6163(2) 0.9132(2) 0.0162(6) Uani 1 1 d . . .
H15 H 0.4855 0.6506 0.9740 0.019 Uiso 1 1 calc R . .
C16 C 0.6580(3) 0.5280(3) 0.9052(2) 0.0206(7) Uani 1 1 d . . .
H16 H 0.6962 0.4926 0.9574 0.025 Uiso 1 1 calc R . .
C17 C 0.7057(3) 0.5038(2) 0.8060(2) 0.0178(7) Uani 1 1 d . . .
H17 H 0.7840 0.4472 0.7759 0.021 Uiso 1 1 calc R . .
N18 N 0.7792(2) 0.4514(2) 0.42169(19) 0.0173(6) Uani 1 1 d . . .
C19 C 0.7612(3) 0.4585(3) 0.3249(2) 0.0181(7) Uani 1 1 d . . .
H19A H 0.6699 0.4903 0.3336 0.022 Uiso 1 1 calc R . .
H19B H 0.7974 0.3825 0.3032 0.022 Uiso 1 1 calc R . .
C20 C 0.8242(3) 0.5316(3) 0.2426(2) 0.0195(7) Uani 1 1 d . . .
H20A H 0.7921 0.6063 0.2659 0.023 Uiso 1 1 calc R . .
H20B H 0.8035 0.5417 0.1796 0.023 Uiso 1 1 calc R . .
S21 S 0.99362(8) 0.46697(7) 0.21596(7) 0.0246(2) Uani 1 1 d . . .
C22 C 0.9974(3) 0.4458(3) 0.3452(3) 0.0231(7) Uani 1 1 d . . .
H22A H 1.0848 0.4004 0.3460 0.028 Uiso 1 1 calc R . .
H22B H 0.9717 0.5192 0.3683 0.028 Uiso 1 1 calc R . .
C23 C 0.9109(3) 0.3871(3) 0.4196(2) 0.0195(7) Uani 1 1 d . . .
H23A H 0.9393 0.3118 0.3991 0.023 Uiso 1 1 calc R . .
H23B H 0.9163 0.3778 0.4889 0.023 Uiso 1 1 calc R . .
N24 N 0.3030(2) 0.9032(2) 0.85344(18) 0.0123(5) Uani 1 1 d . . .
C25 C 0.3502(3) 0.9827(2) 0.8315(2) 0.0120(6) Uani 1 1 d . . .
C26 C 0.3137(3) 1.0616(2) 0.8950(2) 0.0146(6) Uani 1 1 d . . .
H26 H 0.3508 1.1158 0.8751 0.018 Uiso 1 1 calc R . .
C27 C 0.2192(3) 1.0609(2) 0.9911(2) 0.0151(6) Uani 1 1 d . . .
C28 C 0.1692(3) 0.9765(2) 1.0151(2) 0.0143(6) Uani 1 1 d . . .
H28 H 0.1063 0.9712 1.0783 0.017 Uiso 1 1 calc R . .
C29 C 0.2147(3) 0.9030(2) 0.9440(2) 0.0124(6) Uani 1 1 d . . .
N30 N 0.4445(2) 0.9747(2) 0.73548(19) 0.0140(5) Uani 1 1 d . . .
N31 N 0.4773(2) 0.8883(2) 0.68235(19) 0.0136(5) Uani 1 1 d . . .
C32 C 0.5651(3) 0.9014(3) 0.5960(2) 0.0170(7) Uani 1 1 d . . .
H32 H 0.6064 0.8529 0.5434 0.020 Uiso 1 1 calc R . .
C33 C 0.5890(3) 0.9960(3) 0.5923(2) 0.0201(7) Uani 1 1 d . . .
H33 H 0.6472 1.0232 0.5389 0.024 Uiso 1 1 calc R . .
C34 C 0.5105(3) 1.0407(3) 0.6821(2) 0.0169(7) Uani 1 1 d . . .
H34 H 0.5035 1.1059 0.7033 0.020 Uiso 1 1 calc R . .
N35 N 0.1713(2) 0.8157(2) 0.96038(18) 0.0129(5) Uani 1 1 d . . .
N36 N 0.2184(2) 0.7490(2) 0.88407(19) 0.0154(5) Uani 1 1 d . . .
C37 C 0.1627(3) 0.6760(3) 0.9217(2) 0.0185(7) Uani 1 1 d . . .
H37 H 0.1776 0.6178 0.8856 0.022 Uiso 1 1 calc R . .
C38 C 0.0799(3) 0.6945(3) 1.0201(2) 0.0190(7) Uani 1 1 d . . .
H38 H 0.0289 0.6538 1.0622 0.023 Uiso 1 1 calc R . .
C39 C 0.0878(3) 0.7842(2) 1.0433(2) 0.0152(6) Uani 1 1 d . . .
H39 H 0.0432 0.8179 1.1055 0.018 Uiso 1 1 calc R . .
N40 N 0.1782(2) 1.1387(2) 1.0556(2) 0.0189(6) Uani 1 1 d . . .
C41 C 0.2248(3) 1.2291(3) 1.0293(3) 0.0220(7) Uani 1 1 d . . .
H41A H 0.1541 1.2991 1.0539 0.026 Uiso 1 1 calc R . .
H41B H 0.2595 1.2417 0.9542 0.026 Uiso 1 1 calc R . .
C42 C 0.3264(3) 1.2005(3) 1.0767(3) 0.0296(8) Uani 1 1 d . . .
H42A H 0.3621 1.2592 1.0524 0.036 Uiso 1 1 calc R . .
H42B H 0.3952 1.1287 1.0543 0.036 Uiso 1 1 calc R . .
S43 S 0.26513(9) 1.18906(8) 1.21407(7) 0.0310(2) Uani 1 1 d . . .
C44 C 0.1917(4) 1.0916(3) 1.2301(3) 0.0336(9) Uani 1 1 d . . .
H44A H 0.2586 1.0172 1.2134 0.040 Uiso 1 1 calc R . .
H44B H 0.1409 1.0840 1.3027 0.040 Uiso 1 1 calc R . .
C45 C 0.1078(3) 1.1265(3) 1.1645(3) 0.0266(8) Uani 1 1 d . . .
H45A H 0.0714 1.0698 1.1768 0.032 Uiso 1 1 calc R . .
H45B H 0.0375 1.1986 1.1838 0.032 Uiso 1 1 calc R . .
C46 C 0.1565(3) 0.1901(3) 0.6485(3) 0.0200(7) Uani 1 1 d . . .
F47 F 0.15044(19) 0.22050(17) 0.73387(16) 0.0334(5) Uani 1 1 d . . .
F48 F 0.18414(18) 0.26553(16) 0.57221(16) 0.0341(5) Uani 1 1 d . . .
F49 F 0.25291(16) 0.09142(15) 0.63105(15) 0.0266(5) Uani 1 1 d . . .
S50 S 0.00886(7) 0.18110(6) 0.66177(6) 0.01664(17) Uani 1 1 d . . .
O51 O -0.0794(2) 0.29458(18) 0.67761(18) 0.0266(5) Uani 1 1 d . . .
O52 O -0.0046(2) 0.10001(18) 0.74994(17) 0.0221(5) Uani 1 1 d . . .
O53 O 0.0335(2) 0.14332(19) 0.56687(17) 0.0260(5) Uani 1 1 d . . .
C54 C 0.6209(3) 0.2343(3) 0.8282(3) 0.0211(7) Uani 1 1 d . . .
F55 F 0.67382(18) 0.28289(17) 0.85814(16) 0.0329(5) Uani 1 1 d . . .
F56 F 0.70742(18) 0.18165(16) 0.74600(15) 0.0290(5) Uani 1 1 d . . .
F57 F 0.59666(19) 0.15568(17) 0.90217(16) 0.0347(5) Uani 1 1 d . . .
S58 S 0.47919(7) 0.33278(6) 0.79866(6) 0.01667(17) Uani 1 1 d . . .
O59 O 0.5258(2) 0.39773(19) 0.70709(17) 0.0242(5) Uani 1 1 d . . .
O60 O 0.4305(2) 0.25994(18) 0.78269(18) 0.0233(5) Uani 1 1 d . . .
O61 O 0.4031(2) 0.39309(18) 0.88683(17) 0.0239(5) Uani 1 1 d . . .


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

loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
_geom_bond_publ_flag
Fe1 N2 2.128(2) . ?
Fe1 N24 2.135(2) . ?
Fe1 N14 2.180(3) . ?
Fe1 N31 2.182(2) . ?
Fe1 N9 2.200(3) . ?
Fe1 N36 2.209(2) . ?
N2 C3 1.328(4) . ?
N2 C7 1.341(4) . ?
C3 C4 1.376(4) . ?
C3 N8 1.417(4) . ?
C4 C5 1.426(4) . ?
C5 N18 1.363(4) . ?
C5 C6 1.415(4) . ?
C6 C7 1.368(4) . ?
C7 N13 1.405(4) . ?
N8 C12 1.359(4) . ?
N8 N9 1.376(3) . ?
N9 C10 1.330(4) . ?
C10 C11 1.413(4) . ?
C11 C12 1.373(4) . ?
N13 C17 1.359(4) . ?
N13 N14 1.373(3) . ?
N14 C15 1.323(4) . ?
C15 C16 1.402(4) . ?
C16 C17 1.370(4) . ?
N18 C19 1.455(4) . ?
N18 C23 1.472(4) . ?
C19 C20 1.525(4) . ?
C20 S21 1.812(3) . ?
S21 C22 1.809(3) . ?
C22 C23 1.527(4) . ?
N24 C29 1.336(4) . ?
N24 C25 1.343(4) . ?
C25 C26 1.372(4) . ?
C25 N30 1.411(4) . ?
C26 C27 1.423(4) . ?
C27 N40 1.358(4) . ?
C27 C28 1.422(4) . ?
C28 C29 1.374(4) . ?
C29 N35 1.419(3) . ?
N30 C34 1.356(4) . ?
N30 N31 1.365(3) . ?
N31 C32 1.328(4) . ?
C32 C33 1.402(4) . ?
C33 C34 1.365(4) . ?
N35 C39 1.357(4) . ?
N35 N36 1.365(3) . ?
N36 C37 1.325(4) . ?
C37 C38 1.391(4) . ?
C38 C39 1.370(4) . ?
N40 C41 1.464(4) . ?
N40 C45 1.469(4) . ?
C41 C42 1.517(5) . ?
C42 S43 1.803(4) . ?
S43 C44 1.816(4) . ?
C44 C45 1.513(5) . ?
C46 F48 1.335(4) . ?
C46 F49 1.339(4) . ?
C46 F47 1.343(4) . ?
C46 S50 1.823(3) . ?
S50 O53 1.439(2) . ?
S50 O51 1.443(2) . ?
S50 O52 1.447(2) . ?
C54 F55 1.327(4) . ?
C54 F57 1.334(4) . ?
C54 F56 1.346(4) . ?
C54 S58 1.811(3) . ?
S58 O61 1.434(2) . ?
S58 O59 1.442(2) . ?
S58 O60 1.446(2) . ?

loop_
_geom_angle_atom_site_label_1
_geom_angle_atom_site_label_2
_geom_angle_atom_site_label_3
_geom_angle
_geom_angle_site_symmetry_1
_geom_angle_site_symmetry_3
_geom_angle_publ_flag
N2 Fe1 N24 161.95(9) . . ?
N2 Fe1 N14 72.34(9) . . ?
N24 Fe1 N14 100.14(9) . . ?
N2 Fe1 N31 92.27(9) . . ?
N24 Fe1 N31 72.32(9) . . ?
N14 Fe1 N31 98.70(9) . . ?
N2 Fe1 N9 72.80(9) . . ?
N24 Fe1 N9 117.11(9) . . ?
N14 Fe1 N9 142.59(9) . . ?
N31 Fe1 N9 95.80(9) . . ?
N2 Fe1 N36 123.36(9) . . ?
N24 Fe1 N36 72.49(9) . . ?
N14 Fe1 N36 92.71(9) . . ?
N31 Fe1 N36 144.38(9) . . ?
N9 Fe1 N36 95.23(9) . . ?
C3 N2 C7 116.6(2) . . ?
C3 N2 Fe1 121.77(19) . . ?
C7 N2 Fe1 120.92(19) . . ?
N2 C3 C4 125.2(3) . . ?
N2 C3 N8 112.1(2) . . ?
C4 C3 N8 122.7(3) . . ?
C3 C4 C5 117.6(3) . . ?
N18 C5 C6 121.6(3) . . ?
N18 C5 C4 120.8(3) . . ?
C6 C5 C4 117.5(3) . . ?
C7 C6 C5 118.3(3) . . ?
N2 C7 C6 124.8(3) . . ?
N2 C7 N13 111.7(2) . . ?
C6 C7 N13 123.5(3) . . ?
C12 N8 N9 111.4(2) . . ?
C12 N8 C3 130.3(2) . . ?
N9 N8 C3 118.2(2) . . ?
C10 N9 N8 105.0(2) . . ?
C10 N9 Fe1 140.7(2) . . ?
N8 N9 Fe1 114.23(17) . . ?
N9 C10 C11 111.0(3) . . ?
C12 C11 C10 105.5(3) . . ?
N8 C12 C11 106.9(3) . . ?
C17 N13 N14 110.8(2) . . ?
C17 N13 C7 131.0(3) . . ?
N14 N13 C7 117.9(2) . . ?
C15 N14 N13 105.2(2) . . ?
C15 N14 Fe1 139.9(2) . . ?
N13 N14 Fe1 114.57(18) . . ?
N14 C15 C16 111.5(3) . . ?
C17 C16 C15 105.3(3) . . ?
N13 C17 C16 107.3(3) . . ?
C5 N18 C19 122.1(3) . . ?
C5 N18 C23 123.0(3) . . ?
C19 N18 C23 112.6(2) . . ?
N18 C19 C20 111.0(2) . . ?
C19 C20 S21 110.1(2) . . ?
C22 S21 C20 98.31(15) . . ?
C23 C22 S21 112.7(2) . . ?
N18 C23 C22 111.3(3) . . ?
C29 N24 C25 116.2(2) . . ?
C29 N24 Fe1 121.77(19) . . ?
C25 N24 Fe1 121.74(19) . . ?
N24 C25 C26 124.5(3) . . ?
N24 C25 N30 112.0(2) . . ?
C26 C25 N30 123.4(3) . . ?
C25 C26 C27 118.8(3) . . ?
N40 C27 C28 122.1(3) . . ?
N40 C27 C26 120.9(3) . . ?
C28 C27 C26 116.9(3) . . ?
C29 C28 C27 117.9(3) . . ?
N24 C29 C28 125.6(3) . . ?
N24 C29 N35 112.0(2) . . ?
C28 C29 N35 122.4(3) . . ?
C34 N30 N31 111.1(2) . . ?
C34 N30 C25 131.3(2) . . ?
N31 N30 C25 117.6(2) . . ?
C32 N31 N30 105.1(2) . . ?
C32 N31 Fe1 138.8(2) . . ?
N30 N31 Fe1 116.11(18) . . ?
N31 C32 C33 111.3(3) . . ?
C34 C33 C32 105.2(3) . . ?
N30 C34 C33 107.4(3) . . ?
C39 N35 N36 111.4(2) . . ?
C39 N35 C29 130.2(2) . . ?
N36 N35 C29 118.4(2) . . ?
C37 N36 N35 104.6(2) . . ?
C37 N36 Fe1 139.9(2) . . ?
N35 N36 Fe1 114.30(17) . . ?
N36 C37 C38 112.0(3) . . ?
C39 C38 C37 105.2(3) . . ?
N35 C39 C38 106.8(3) . . ?
C27 N40 C41 122.4(3) . . ?
C27 N40 C45 123.5(3) . . ?
C41 N40 C45 112.7(2) . . ?
N40 C41 C42 110.8(3) . . ?
C41 C42 S43 111.5(2) . . ?
C42 S43 C44 97.57(16) . . ?
C45 C44 S43 113.7(2) . . ?
N40 C45 C44 111.4(3) . . ?
F48 C46 F49 108.0(2) . . ?
F48 C46 F47 107.1(3) . . ?
F49 C46 F47 107.3(3) . . ?
F48 C46 S50 111.9(2) . . ?
F49 C46 S50 111.4(2) . . ?
F47 C46 S50 111.1(2) . . ?
O53 S50 O51 115.95(14) . . ?
O53 S50 O52 114.79(14) . . ?
O51 S50 O52 115.31(14) . . ?
O53 S50 C46 103.72(15) . . ?
O51 S50 C46 101.98(14) . . ?
O52 S50 C46 102.22(14) . . ?
F55 C54 F57 107.7(3) . . ?
F55 C54 F56 107.4(3) . . ?
F57 C54 F56 107.1(3) . . ?
F55 C54 S58 112.7(2) . . ?
F57 C54 S58 111.1(2) . . ?
F56 C54 S58 110.7(2) . . ?
O61 S58 O59 115.28(14) . . ?
O61 S58 O60 114.86(14) . . ?
O59 S58 O60 113.92(14) . . ?
O61 S58 C54 104.84(15) . . ?
O59 S58 C54 103.41(15) . . ?
O60 S58 C54 102.38(14) . . ?

_diffrn_measured_fraction_theta_max 0.837
_diffrn_reflns_theta_full        28.94
_diffrn_measured_fraction_theta_full 0.837
_refine_diff_density_max         1.079
_refine_diff_density_min         -0.625
_refine_diff_density_rms         0.091
_exptl_crystal_recrystallization_method 
'Re-crystallisation from solvent: nitromethane-diethyl ether'
_exptl_crystal_preparation       'Magnetic properties'
