# Electronic Supplementary Material (ESI) for Journal of Materials Chemistry C.
# This journal is © The Royal Society of Chemistry 2020

####################################################################### 
# 
# 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_h2o220
_database_code_depnum_ccdc_archive 'CCDC 1976619'
_audit_update_record             
;
2020-01-09 deposited with the CCDC.	2020-05-26 downloaded from the CCDC.
;
_audit_creation_date             2018-06-27
_audit_creation_method           
;
  Olex2 1.2
  (compiled Apr 23 2013 17:54:37, GUI svn.r4466)
;
_chemical_name_common            ?
_chemical_name_systematic        
;
Bis[4-(isopropylsulfanyl)-2,6-di(pyrazol-1-yl)pyridine]iron(II)
ditetrafluoroborate hydrate
;
_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         818.23
_chemical_melting_point          ?
loop_
_atom_type_symbol
_atom_type_description
_atom_type_scat_dispersion_real
_atom_type_scat_dispersion_imag
_atom_type_scat_source
B B 0.0090 0.0039 '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'
F F 0.0727 0.0534 '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'

_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_id
_space_group_symop_operation_xyz
1 'x, y, z'
2 '-x, y+1/2, -z+1/2'
3 '-x, -y, -z'
4 'x, -y-1/2, z-1/2'

_cell_length_a                   20.2764(7)
_cell_length_b                   11.7156(5)
_cell_length_c                   15.6792(7)
_cell_angle_alpha                90.00
_cell_angle_beta                 102.811(4)
_cell_angle_gamma                90.00
_cell_volume                     3631.9(3)
_cell_formula_units_Z            4
_cell_measurement_reflns_used    4621
_cell_measurement_temperature    220(2)
_cell_measurement_theta_min      4.44
_cell_measurement_theta_max      72.65
_exptl_absorpt_coefficient_mu    5.130
_exptl_absorpt_correction_T_min  0.428
_exptl_absorpt_correction_T_max  1.000
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   
;
CrysAlisPro 1.171.39.46 (Rigaku Oxford Diffraction, 2018)
Empirical absorption correction using spherical harmonics,
 implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_crystal_colour            orange
_exptl_crystal_density_diffrn    1.496
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       plate
_exptl_crystal_F_000             1672
_exptl_crystal_size_max          0.35
_exptl_crystal_size_mid          0.30
_exptl_crystal_size_min          0.10
_exptl_special_details           
;
 ? 
;
_diffrn_reflns_av_R_equivalents  0.0275
_diffrn_reflns_av_unetI/netI     0.0382
_diffrn_reflns_limit_h_max       24
_diffrn_reflns_limit_h_min       -24
_diffrn_reflns_limit_k_max       14
_diffrn_reflns_limit_k_min       -10
_diffrn_reflns_limit_l_max       18
_diffrn_reflns_limit_l_min       -19
_diffrn_reflns_number            13853
_diffrn_reflns_theta_full        72.00
_diffrn_reflns_theta_max         73.74
_diffrn_reflns_theta_min         4.39
_diffrn_ambient_temperature      220(2)
_diffrn_detector_area_resol_mean 5.3095
_diffrn_measured_fraction_theta_full 0.985
_diffrn_measured_fraction_theta_max 0.968
_diffrn_measurement_device_type  'SuperNova, Dual, Cu at zero, Atlas'
_diffrn_measurement_method       'ω scans'
_diffrn_radiation_monochromator  mirror
_diffrn_radiation_type           CuK\a
_diffrn_radiation_wavelength     1.54184
_diffrn_radiation_source         'SuperNova (Cu) X-ray Source'
_diffrn_standards_number         0
_diffrn_standards_interval_count 0
_diffrn_standards_interval_time  0
_diffrn_standards_decay_%        0
_reflns_number_gt                5597
_reflns_number_total             7112
_reflns_threshold_expression     >2sigma(I)
_computing_data_collection       'CrysAlisPro, Agilent Technologies'
_computing_cell_refinement       'CrysAlisPro, Agilent Technologies'
_computing_data_reduction        'CrysAlisPro, Agilent Technologies'
_computing_molecular_graphics    'XSEED (Barbour, 2001)'
_computing_publication_material  
;
O. V. Dolomanov, L. J. Bourhis, R. J. Gildea, J. A. K. Howard and H. Puschmann,
OLEX2: a complete structure solution, refinement and analysis program.
J. Appl. Cryst. (2009). 42, 339-341.
;
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_refine_diff_density_max         0.743
_refine_diff_density_min         -0.886
_refine_diff_density_rms         0.080
_refine_ls_extinction_coef       ?
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.051
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     494
_refine_ls_number_reflns         7112
_refine_ls_number_restraints     68
_refine_ls_R_factor_all          0.0926
_refine_ls_R_factor_gt           0.0764
_refine_ls_restrained_S_all      1.064
_refine_ls_shift/su_max          0.001
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details     
'calc w=1/[σ²(Fo²)+(0.1153P)²+6.3151P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.2145
_refine_ls_wR_factor_ref         0.2276
_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 isopropylsulfanyl substitutents on the complex cation is 
 disordered over three orientations, with occupancies of 
 0.45, 0.40 and 0.15. 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. Both BF₄⁻ 
 ions are also disordered, one over two half-occupied sites and the 
 other over three orientations of occupancy 0.55, 0.30 and 0.15 which 
 share a common fully occupied B atom. The refined restraints B---F = 
 1.39(2) and F...F = 2.27(2) Å were applied to those residues. Lastly, 
 the water molecule was also refined over three different sites with a 
 0.6:0.3:0.1 occupancy ratio.

 All fully occupied non-H 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 could not be located and are not included in
 the model, but are accounted for in the density and F(000) calculations. 
 This disordered water site is positioned to hydrogen bond to anion 
 B42-F46, and to its own symmetry equivalent related by 1-x, 1-y, 1-z.
;
_olex2_refinement_description    
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups
 At 1.5 times of:
  All C(H,H,H) groups
2. Restrained distances
 B42-F43A = B42-F44A = B42-F45A = B42-F46A
 1.39295 with sigma of 0.02
 B42-F43B = B42-F44B = B42-F45B = B42-F46B
 1.39295 with sigma of 0.02
 B42-F43C = B42-F44C = B42-F45C = B42-F46C
 1.39295 with sigma of 0.02
 F43A-F44A = F43A-F45A = F43A-F46A = F44A-F45A = F44A-F46A = F45A-F46A
 2.274687 with sigma of 0.02
 F43B-F44B = F43B-F45B = F43B-F46B = F44B-F45B = F44B-F46B = F45B-F46B
 2.274687 with sigma of 0.02
 F43C-F44C = F43C-F45C = F43C-F46C = F44C-F45C = F44C-F46C = F45C-F46C
 2.274687 with sigma of 0.02
 B47A-F48A = B47A-F49A = B47A-F50A = B47A-F51A
 1.39295 with sigma of 0.02
 B47B-F48B = B47B-F49B = B47B-F50B = B47B-F51B
 1.39295 with sigma of 0.02
 F48A-F49A = F48A-F50A = F48A-F51A = F49A-F50A = F49A-F51A = F50A-F51A
 2.274687 with sigma of 0.02
 F48B-F49B = F48B-F50B = F48B-F51B = F49B-F50B = F49B-F51B = F50B-F51B
 2.274687 with sigma of 0.02
 C25-S38A = C25-S38B = C25-S38C
 1.75 with sigma of 0.02
 S38A-C39A = S38B-C39B = S38C-C39C
 1.82 with sigma of 0.02
 C39A-C40A = C39A-C41A = C39B-C40B = C39B-C41B = C39C-C40C = C39C-C41C
 1.52 with sigma of 0.02
 C40A-C41A = C40B-C41B = C40C-C41C
 2.48 with sigma of 0.02
 C25-C39A = C25-C39B = C25-C39C
 2.83 with sigma of 0.02
3. Others
 1(DFIX)=1(DFIX)=1(DFIX)=1(DFIX)=1(DFIX)=FVAR(1)
 1(DFIX)=1(DFIX)=1(DFIX)=1(DFIX)=1(DFIX)=1.633*FVAR(2)
 Fixed Sof: S38A(0.4) C39A(0.4) H39A(0.4) C40A(0.4) H40A(0.4) H40B(0.4)
 H40C(0.4) C41A(0.4) H41A(0.4) H41B(0.4) H41C(0.4) S38B(0.45) C39B(0.45)
 H39B(0.45) C40B(0.45) H40D(0.45) H40E(0.45) H40F(0.45) C41B(0.45) H41D(0.45)
 H41E(0.45) H41F(0.45) S38C(0.15) C39C(0.15) H39C(0.15) C40C(0.15) H40G(0.15)
 H40H(0.15) H40I(0.15) C41C(0.15) H41G(0.15) H41H(0.15) H41I(0.15) F43A(0.55)
 F44A(0.55) F45A(0.55) F46A(0.55) F43B(0.15) F44B(0.15) F45B(0.15) F46B(0.15)
 F43C(0.3) F44C(0.3) F45C(0.3) F46C(0.3) B47A(0.5) F48A(0.5) F49A(0.5)
 F50A(0.5) F51A(0.5) B47B(0.5) F48B(0.5) F49B(0.5) F50B(0.5) F51B(0.5)
 O52A(0.6) O52B(0.3) O52C(0.1)
4.a Ternary CH refined with riding coordinates:
 C19(H19), C39A(H39A), C39B(H39B), C39C(H39C)
4.b Me refined with riding coordinates:
 C40A(H40A,H40B,H40C), C41A(H41A,H41B,H41C), C40B(H40D,H40E,H40F), C41B(H41D,
 H41E,H41F), C40C(H40G,H40H,H40I), C41C(H41G,H41H,H41I)
4.c Aromatic/amide H refined with riding coordinates:
 C4(H4), C6(H6), C10(H10), C11(H11), C12(H12), C15(H15), C16(H16), C17(H17),
 C24(H24), C26(H26), C30(H30), C31(H31), C32(H32), C35(H35), C36(H36), C37(H37)
4.d Idealised Me refined as rotating group:
 C20(H20A,H20B,H20C), C21(H21A,H21B,H21C)
;
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_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_symmetry_multiplicity
_atom_site_calc_flag
_atom_site_refinement_flags
_atom_site_disorder_assembly
_atom_site_disorder_group
Fe1 Fe 0.23013(3) 0.60460(6) 0.07193(5) 0.0415(2) Uani 1 1 d . A .
N2 N 0.12425(18) 0.6258(3) 0.0437(2) 0.0411(8) Uani 1 1 d . . .
C3 C 0.0949(2) 0.7025(4) -0.0141(3) 0.0410(9) Uani 1 1 d . . .
C4 C 0.0271(2) 0.7327(4) -0.0281(3) 0.0453(10) Uani 1 1 d . . .
H4 H 0.0079 0.7868 -0.0707 0.054 Uiso 1 1 calc R . .
C5 C -0.0111(2) 0.6791(4) 0.0239(3) 0.0472(10) Uani 1 1 d . . .
C6 C 0.0190(2) 0.5980(4) 0.0864(3) 0.0481(11) Uani 1 1 d . . .
H6 H -0.0057 0.5614 0.1226 0.058 Uiso 1 1 calc R . .
C7 C 0.0864(2) 0.5747(4) 0.0922(3) 0.0421(9) Uani 1 1 d . . .
N8 N 0.14003(19) 0.7540(3) -0.0587(3) 0.0442(9) Uani 1 1 d . . .
N9 N 0.2078(2) 0.7322(4) -0.0283(3) 0.0489(9) Uani 1 1 d . . .
C10 C 0.2386(3) 0.7972(5) -0.0764(4) 0.0643(15) Uani 1 1 d . . .
H10 H 0.2858 0.8005 -0.0704 0.077 Uiso 1 1 calc R . .
C11 C 0.1921(3) 0.8604(6) -0.1375(4) 0.0701(17) Uani 1 1 d . . .
H11 H 0.2016 0.9124 -0.1788 0.084 Uiso 1 1 calc R . .
C12 C 0.1299(3) 0.8306(5) -0.1246(4) 0.0592(14) Uani 1 1 d . . .
H12 H 0.0879 0.8583 -0.1558 0.071 Uiso 1 1 calc R . .
N13 N 0.1239(2) 0.4951(3) 0.1524(3) 0.0465(9) Uani 1 1 d . . .
N14 N 0.1920(2) 0.4875(4) 0.1585(3) 0.0477(9) Uani 1 1 d . . .
C15 C 0.2121(3) 0.4047(5) 0.2162(4) 0.0580(13) Uani 1 1 d . . .
H15 H 0.2572 0.3803 0.2348 0.070 Uiso 1 1 calc R . .
C16 C 0.1575(3) 0.3585(5) 0.2456(4) 0.0683(16) Uani 1 1 d . . .
H16 H 0.1590 0.2985 0.2858 0.082 Uiso 1 1 calc R . .
C17 C 0.1018(3) 0.4178(5) 0.2044(4) 0.0575(13) Uani 1 1 d . . .
H17 H 0.0572 0.4074 0.2106 0.069 Uiso 1 1 calc R . .
S18 S -0.09726(6) 0.70254(12) 0.01737(10) 0.0583(4) Uani 1 1 d . . .
C19 C -0.1162(3) 0.8371(5) -0.0406(4) 0.0576(13) Uani 1 1 d . . .
H19 H -0.1000 0.8339 -0.0956 0.069 Uiso 1 1 calc R . .
C20 C -0.0825(3) 0.9356(6) 0.0142(5) 0.0725(16) Uani 1 1 d . . .
H20A H -0.0913 1.0057 -0.0193 0.109 Uiso 1 1 calc R . .
H20B H -0.0341 0.9224 0.0307 0.109 Uiso 1 1 calc R . .
H20C H -0.1004 0.9420 0.0665 0.109 Uiso 1 1 calc R . .
C21 C -0.1927(3) 0.8486(7) -0.0623(5) 0.0789(19) Uani 1 1 d . . .
H21A H -0.2086 0.8571 -0.0087 0.118 Uiso 1 1 calc R . .
H21B H -0.2127 0.7808 -0.0931 0.118 Uiso 1 1 calc R . .
H21C H -0.2057 0.9151 -0.0990 0.118 Uiso 1 1 calc R . .
N22 N 0.33357(18) 0.5854(3) 0.1245(3) 0.0431(8) Uani 1 1 d . A .
C23 C 0.3700(2) 0.5089(4) 0.0908(3) 0.0457(10) Uani 1 1 d . . .
C24 C 0.4370(2) 0.4877(5) 0.1251(4) 0.0580(13) Uani 1 1 d . A .
H24 H 0.4610 0.4337 0.0995 0.070 Uiso 1 1 calc R . .
C25 C 0.4684(2) 0.5488(6) 0.1990(4) 0.0655(15) Uani 1 1 d D . .
C26 C 0.4321(2) 0.6329(5) 0.2339(4) 0.0558(13) Uani 1 1 d . A .
H26 H 0.4526 0.6776 0.2824 0.067 Uiso 1 1 calc R . .
C27 C 0.3648(2) 0.6460(4) 0.1929(3) 0.0434(10) Uani 1 1 d . . .
N28 N 0.33152(19) 0.4509(4) 0.0178(3) 0.0465(9) Uani 1 1 d . . .
N29 N 0.2644(2) 0.4754(4) -0.0082(3) 0.0461(9) Uani 1 1 d . . .
C30 C 0.2428(3) 0.4093(5) -0.0769(3) 0.0560(13) Uani 1 1 d . . .
H30 H 0.1979 0.4074 -0.1094 0.067 Uiso 1 1 calc R . .
C31 C 0.2948(3) 0.3427(5) -0.0953(4) 0.0643(15) Uani 1 1 d . . .
H31 H 0.2918 0.2893 -0.1408 0.077 Uiso 1 1 calc R . .
C32 C 0.3505(3) 0.3710(5) -0.0342(4) 0.0616(14) Uani 1 1 d . . .
H32 H 0.3942 0.3409 -0.0288 0.074 Uiso 1 1 calc R . .
N33 N 0.3214(2) 0.7271(4) 0.2182(3) 0.0486(9) Uani 1 1 d . A .
N34 N 0.2563(2) 0.7324(4) 0.1714(3) 0.0510(10) Uani 1 1 d . . .
C35 C 0.2296(3) 0.8215(5) 0.2059(4) 0.0635(14) Uani 1 1 d . A .
H35 H 0.1847 0.8464 0.1868 0.076 Uiso 1 1 calc R . .
C36 C 0.2763(4) 0.8721(5) 0.2729(5) 0.0710(17) Uani 1 1 d . . .
H36 H 0.2692 0.9353 0.3066 0.085 Uiso 1 1 calc R A .
C37 C 0.3353(3) 0.8109(5) 0.2802(4) 0.0650(15) Uani 1 1 d . A .
H37 H 0.3767 0.8241 0.3198 0.078 Uiso 1 1 calc R . .
S38A S 0.54722(17) 0.4899(3) 0.2578(2) 0.0488(8) Uiso 0.40 1 d PD A 1
C39A C 0.5811(7) 0.6063(15) 0.3345(10) 0.052(5) Uiso 0.40 1 d PD A 1
H39A H 0.5450 0.6316 0.3636 0.063 Uiso 0.40 1 calc PR A 1
C40A C 0.6066(15) 0.709(2) 0.2943(18) 0.106(9) Uiso 0.40 1 d PD A 1
H40A H 0.5700 0.7417 0.2506 0.158 Uiso 0.40 1 calc PR A 1
H40B H 0.6430 0.6863 0.2668 0.158 Uiso 0.40 1 calc PR A 1
H40C H 0.6232 0.7651 0.3393 0.158 Uiso 0.40 1 calc PR A 1
C41A C 0.6360(11) 0.5475(18) 0.4025(13) 0.077(6) Uiso 0.40 1 d PD A 1
H41A H 0.6179 0.4782 0.4223 0.115 Uiso 0.40 1 calc PR A 1
H41B H 0.6511 0.5983 0.4519 0.115 Uiso 0.40 1 calc PR A 1
H41C H 0.6739 0.5286 0.3767 0.115 Uiso 0.40 1 calc PR A 1
S38B S 0.55445(15) 0.5168(3) 0.2341(2) 0.0487(7) Uiso 0.45 1 d PD A 2
C39B C 0.5807(7) 0.5795(13) 0.3442(9) 0.050(4) Uiso 0.45 1 d PD A 2
H39B H 0.5429 0.5838 0.3745 0.060 Uiso 0.45 1 calc PR A 2
C40B C 0.6039(9) 0.6992(13) 0.3209(13) 0.069(4) Uiso 0.45 1 d PD A 2
H40D H 0.5648 0.7439 0.2931 0.103 Uiso 0.45 1 calc PR A 2
H40E H 0.6341 0.6914 0.2812 0.103 Uiso 0.45 1 calc PR A 2
H40F H 0.6274 0.7374 0.3739 0.103 Uiso 0.45 1 calc PR A 2
C41B C 0.6398(7) 0.5124(13) 0.3958(9) 0.057(4) Uiso 0.45 1 d PD A 2
H41D H 0.6242 0.4386 0.4113 0.086 Uiso 0.45 1 calc PR A 2
H41E H 0.6601 0.5538 0.4487 0.086 Uiso 0.45 1 calc PR A 2
H41F H 0.6732 0.5016 0.3607 0.086 Uiso 0.45 1 calc PR A 2
S38C S 0.5565(4) 0.5754(10) 0.2110(6) 0.057(2) Uiso 0.15 1 d PD A 3
C39C C 0.5789(16) 0.653(4) 0.313(2) 0.11(2) Uiso 0.15 1 d PD A 3
H39C H 0.5464 0.7154 0.3168 0.134 Uiso 0.15 1 calc PR A 3
C40C C 0.650(2) 0.698(5) 0.318(4) 0.094(15) Uiso 0.15 1 d PD A 3
H40G H 0.6487 0.7540 0.2728 0.140 Uiso 0.15 1 calc PR A 3
H40H H 0.6789 0.6349 0.3105 0.140 Uiso 0.15 1 calc PR A 3
H40I H 0.6666 0.7325 0.3751 0.140 Uiso 0.15 1 calc PR A 3
C41C C 0.579(3) 0.561(5) 0.381(4) 0.094(17) Uiso 0.15 1 d PD A 3
H41G H 0.5335 0.5299 0.3734 0.141 Uiso 0.15 1 calc PR A 3
H41H H 0.5923 0.5943 0.4392 0.141 Uiso 0.15 1 calc PR A 3
H41I H 0.6100 0.5015 0.3743 0.141 Uiso 0.15 1 calc PR A 3
B42 B 0.4529(3) 0.7251(6) 0.4901(5) 0.075(2) Uani 1 1 d D . .
F43A F 0.5073(5) 0.7270(10) 0.5660(6) 0.120(3) Uiso 0.55 1 d PD B 1
F44A F 0.4750(5) 0.7900(8) 0.4257(6) 0.087(3) Uiso 0.55 1 d PD B 1
F45A F 0.3976(4) 0.7594(8) 0.5126(6) 0.084(2) Uiso 0.55 1 d PD B 1
F46A F 0.4464(6) 0.6141(8) 0.4571(7) 0.114(3) Uiso 0.55 1 d PD B 1
F43B F 0.5124(12) 0.671(3) 0.531(2) 0.163(19) Uiso 0.15 1 d PD B 2
F44B F 0.4639(13) 0.8329(16) 0.4596(17) 0.084(7) Uiso 0.15 1 d PD B 2
F45B F 0.4115(11) 0.732(2) 0.5492(15) 0.069(6) Uiso 0.15 1 d PD B 2
F46B F 0.4191(18) 0.659(3) 0.4178(17) 0.14(2) Uiso 0.15 1 d PD B 2
F43C F 0.4940(7) 0.7685(12) 0.4413(9) 0.073(4) Uiso 0.30 1 d PD B 3
F44C F 0.4819(10) 0.6901(17) 0.5703(9) 0.127(7) Uiso 0.30 1 d PD B 3
F45C F 0.3983(7) 0.8075(13) 0.4878(10) 0.097(5) Uiso 0.30 1 d PD B 3
F46C F 0.4155(7) 0.6340(12) 0.4377(10) 0.071(4) Uiso 0.30 1 d PD B 3
B47A B 0.0730(8) 0.9804(14) 0.2308(10) 0.062(8) Uiso 0.50 1 d PD C 1
F48A F 0.1356(4) 1.0355(8) 0.2313(7) 0.074(3) Uiso 0.50 1 d PD C 1
F49A F 0.0162(4) 1.0500(8) 0.2013(6) 0.069(3) Uiso 0.50 1 d PD C 1
F50A F 0.0789(4) 0.9574(7) 0.3197(5) 0.0660(19) Uiso 0.50 1 d PD C 1
F51A F 0.0683(4) 0.8874(7) 0.1785(5) 0.075(2) Uiso 0.50 1 d PD C 1
B47B B 0.0751(7) 0.9964(13) 0.2321(9) 0.049(6) Uiso 0.50 1 d PD D 2
F48B F 0.1341(5) 1.0565(10) 0.2517(8) 0.095(4) Uiso 0.50 1 d PD D 2
F49B F 0.0260(5) 1.0792(9) 0.2048(7) 0.081(3) Uiso 0.50 1 d PD D 2
F50B F 0.0588(4) 0.9270(7) 0.2989(5) 0.073(2) Uiso 0.50 1 d PD D 2
F51B F 0.0771(5) 0.9215(8) 0.1621(5) 0.077(2) Uiso 0.50 1 d PD D 2
O52A O 0.6227(7) 0.5893(11) 0.6502(8) 0.091(3) Uiso 0.60 1 d P E 1
O52B O 0.6311(12) 0.574(2) 0.6245(17) 0.093(7) Uiso 0.30 1 d P F 2
O52C O 0.591(4) 0.622(6) 0.637(5) 0.11(2) Uiso 0.10 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 N2 2.108(4) . ?
Fe1 N9 2.143(4) . ?
Fe1 N14 2.188(4) . ?
Fe1 N22 2.089(4) . ?
Fe1 N29 2.178(4) . ?
Fe1 N34 2.142(4) . ?
N2 C3 1.321(6) . ?
N2 C7 1.336(6) . ?
C3 C4 1.388(6) . ?
C3 N8 1.405(6) . ?
C4 H4 0.9400 . ?
C4 C5 1.393(7) . ?
C5 C6 1.404(7) . ?
C5 S18 1.748(5) . ?
C6 H6 0.9400 . ?
C6 C7 1.376(7) . ?
C7 N13 1.421(6) . ?
N8 N9 1.375(5) . ?
N8 C12 1.350(7) . ?
N9 C10 1.323(7) . ?
C10 H10 0.9400 . ?
C10 C11 1.398(9) . ?
C11 H11 0.9400 . ?
C11 C12 1.366(9) . ?
C12 H12 0.9400 . ?
N13 N14 1.366(5) . ?
N13 C17 1.359(6) . ?
N14 C15 1.327(7) . ?
C15 H15 0.9400 . ?
C15 C16 1.399(9) . ?
C16 H16 0.9400 . ?
C16 C17 1.361(8) . ?
C17 H17 0.9400 . ?
S18 C19 1.817(6) . ?
C19 H19 0.9900 . ?
C19 C20 1.509(9) . ?
C19 C21 1.518(7) . ?
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 1.341(6) . ?
N22 C27 1.324(6) . ?
C23 C24 1.370(7) . ?
C23 N28 1.408(6) . ?
C24 H24 0.9400 . ?
C24 C25 1.391(8) . ?
C25 C26 1.411(8) . ?
C25 S38A 1.796(6) . ?
C25 S38B 1.749(5) . ?
C25 S38C 1.780(10) . ?
C26 H26 0.9400 . ?
C26 C27 1.383(7) . ?
C27 N33 1.409(6) . ?
N28 N29 1.361(5) . ?
N28 C32 1.353(7) . ?
N29 C30 1.320(7) . ?
C30 H30 0.9400 . ?
C30 C31 1.392(9) . ?
C31 H31 0.9400 . ?
C31 C32 1.351(8) . ?
C32 H32 0.9400 . ?
N33 N34 1.363(6) . ?
N33 C37 1.367(7) . ?
N34 C35 1.343(7) . ?
C35 H35 0.9400 . ?
C35 C36 1.382(9) . ?
C36 H36 0.9400 . ?
C36 C37 1.377(9) . ?
C37 H37 0.9400 . ?
S38A C39A 1.848(13) . ?
C39A H39A 0.9900 . ?
C39A C40A 1.501(17) . ?
C39A C41A 1.525(16) . ?
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 1.842(12) . ?
C39B H39B 0.9900 . ?
C39B C40B 1.548(16) . ?
C39B C41B 1.510(14) . ?
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 1.814(19) . ?
C39C H39C 0.9900 . ?
C39C C40C 1.51(2) . ?
C39C C41C 1.51(2) . ?
C40C H40G 0.9700 . ?
C40C H40H 0.9700 . ?
C40C H40I 0.9700 . ?
C41C H41G 0.9700 . ?
C41C H41H 0.9700 . ?
C41C H41I 0.9700 . ?
B42 F43A 1.433(11) . ?
B42 F44A 1.414(10) . ?
B42 F45A 1.310(9) . ?
B42 F46A 1.395(10) . ?
B42 F43B 1.390(16) . ?
B42 F44B 1.386(15) . ?
B42 F45B 1.385(14) . ?
B42 F46B 1.414(16) . ?
B42 F43C 1.350(12) . ?
B42 F44C 1.331(13) . ?
B42 F45C 1.464(12) . ?
B42 F46C 1.454(12) . ?
B47A F48A 1.421(15) . ?
B47A F49A 1.402(15) . ?
B47A F50A 1.399(15) . ?
B47A F51A 1.355(15) . ?
B47B F48B 1.364(14) . ?
B47B F49B 1.388(14) . ?
B47B F50B 1.422(14) . ?
B47B F51B 1.413(14) . ?

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 N9 74.01(15) . . ?
N2 Fe1 N14 73.76(15) . . ?
N2 Fe1 N29 113.67(15) . . ?
N2 Fe1 N34 98.43(15) . . ?
N9 Fe1 N14 147.76(15) . . ?
N9 Fe1 N29 96.00(16) . . ?
N22 Fe1 N2 169.16(15) . . ?
N22 Fe1 N9 113.25(15) . . ?
N22 Fe1 N14 98.62(15) . . ?
N22 Fe1 N29 74.43(15) . . ?
N22 Fe1 N34 73.92(15) . . ?
N29 Fe1 N14 97.14(15) . . ?
N34 Fe1 N9 91.39(17) . . ?
N34 Fe1 N14 92.90(17) . . ?
N34 Fe1 N29 147.87(15) . . ?
C3 N2 Fe1 120.5(3) . . ?
C3 N2 C7 117.8(4) . . ?
C7 N2 Fe1 121.0(3) . . ?
N2 C3 C4 124.2(4) . . ?
N2 C3 N8 112.9(4) . . ?
C4 C3 N8 122.9(4) . . ?
C3 C4 H4 121.5 . . ?
C3 C4 C5 116.9(4) . . ?
C5 C4 H4 121.5 . . ?
C4 C5 C6 120.1(4) . . ?
C4 C5 S18 125.0(4) . . ?
C6 C5 S18 114.9(4) . . ?
C5 C6 H6 121.6 . . ?
C7 C6 C5 116.9(4) . . ?
C7 C6 H6 121.6 . . ?
N2 C7 C6 124.1(4) . . ?
N2 C7 N13 112.4(4) . . ?
C6 C7 N13 123.5(4) . . ?
N9 N8 C3 117.3(4) . . ?
C12 N8 C3 131.4(4) . . ?
C12 N8 N9 111.1(4) . . ?
N8 N9 Fe1 114.6(3) . . ?
C10 N9 Fe1 140.4(4) . . ?
C10 N9 N8 104.9(4) . . ?
N9 C10 H10 124.4 . . ?
N9 C10 C11 111.3(5) . . ?
C11 C10 H10 124.4 . . ?
C10 C11 H11 127.2 . . ?
C12 C11 C10 105.6(5) . . ?
C12 C11 H11 127.2 . . ?
N8 C12 C11 107.1(5) . . ?
N8 C12 H12 126.5 . . ?
C11 C12 H12 126.5 . . ?
N14 N13 C7 118.3(4) . . ?
C17 N13 C7 129.6(4) . . ?
C17 N13 N14 112.1(4) . . ?
N13 N14 Fe1 114.0(3) . . ?
C15 N14 Fe1 141.6(4) . . ?
C15 N14 N13 104.4(4) . . ?
N14 C15 H15 124.4 . . ?
N14 C15 C16 111.2(5) . . ?
C16 C15 H15 124.4 . . ?
C15 C16 H16 126.9 . . ?
C17 C16 C15 106.2(5) . . ?
C17 C16 H16 126.9 . . ?
N13 C17 C16 106.1(5) . . ?
N13 C17 H17 127.0 . . ?
C16 C17 H17 127.0 . . ?
C5 S18 C19 105.3(2) . . ?
S18 C19 H19 109.2 . . ?
C20 C19 S18 111.1(4) . . ?
C20 C19 H19 109.2 . . ?
C20 C19 C21 111.8(5) . . ?
C21 C19 S18 106.4(4) . . ?
C21 C19 H19 109.2 . . ?
C19 C20 H20A 109.5 . . ?
C19 C20 H20B 109.5 . . ?
C19 C20 H20C 109.5 . . ?
H20A C20 H20B 109.5 . . ?
H20A C20 H20C 109.5 . . ?
H20B C20 H20C 109.5 . . ?
C19 C21 H21A 109.5 . . ?
C19 C21 H21B 109.5 . . ?
C19 C21 H21C 109.5 . . ?
H21A C21 H21B 109.5 . . ?
H21A C21 H21C 109.5 . . ?
H21B C21 H21C 109.5 . . ?
C23 N22 Fe1 120.6(3) . . ?
C27 N22 Fe1 121.3(3) . . ?
C27 N22 C23 118.1(4) . . ?
N22 C23 C24 123.5(5) . . ?
N22 C23 N28 112.9(4) . . ?
C24 C23 N28 123.6(4) . . ?
C23 C24 H24 121.2 . . ?
C23 C24 C25 117.7(5) . . ?
C25 C24 H24 121.2 . . ?
C24 C25 C26 120.1(4) . . ?
C24 C25 S38A 114.9(4) . . ?
C24 C25 S38B 113.1(4) . . ?
C24 C25 S38C 116.1(5) . . ?
C26 C25 S38A 123.4(4) . . ?
C26 C25 S38B 126.7(4) . . ?
C26 C25 S38C 115.7(5) . . ?
C25 C26 H26 121.9 . . ?
C27 C26 C25 116.3(5) . . ?
C27 C26 H26 121.9 . . ?
N22 C27 C26 124.3(4) . . ?
N22 C27 N33 111.9(4) . . ?
C26 C27 N33 123.9(4) . . ?
N29 N28 C23 118.6(4) . . ?
C32 N28 C23 130.1(4) . . ?
C32 N28 N29 111.4(4) . . ?
N28 N29 Fe1 113.5(3) . . ?
C30 N29 Fe1 142.0(4) . . ?
C30 N29 N28 104.5(4) . . ?
N29 C30 H30 124.2 . . ?
N29 C30 C31 111.6(5) . . ?
C31 C30 H30 124.2 . . ?
C30 C31 H31 127.2 . . ?
C32 C31 C30 105.6(5) . . ?
C32 C31 H31 127.2 . . ?
N28 C32 H32 126.5 . . ?
C31 C32 N28 107.0(5) . . ?
C31 C32 H32 126.5 . . ?
N34 N33 C27 118.1(4) . . ?
N34 N33 C37 111.8(4) . . ?
C37 N33 C27 129.9(4) . . ?
N33 N34 Fe1 114.4(3) . . ?
C35 N34 Fe1 141.2(4) . . ?
C35 N34 N33 104.4(4) . . ?
N34 C35 H35 124.2 . . ?
N34 C35 C36 111.7(5) . . ?
C36 C35 H35 124.2 . . ?
C35 C36 H36 127.0 . . ?
C37 C36 C35 106.1(5) . . ?
C37 C36 H36 127.0 . . ?
N33 C37 C36 106.0(5) . . ?
N33 C37 H37 127.0 . . ?
C36 C37 H37 127.0 . . ?
C25 S38A C39A 102.1(6) . . ?
S38A C39A H39A 108.3 . . ?
C40A C39A S38A 115.5(15) . . ?
C40A C39A H39A 108.3 . . ?
C40A C39A C41A 113.0(14) . . ?
C41A C39A S38A 103.3(13) . . ?
C41A C39A H39A 108.3 . . ?
C39A C40A H40A 109.5 . . ?
C39A C40A H40B 109.5 . . ?
C39A C40A H40C 109.5 . . ?
H40A C40A H40B 109.5 . . ?
H40A C40A H40C 109.5 . . ?
H40B C40A H40C 109.5 . . ?
C39A C41A H41A 109.5 . . ?
C39A C41A H41B 109.5 . . ?
C39A C41A H41C 109.5 . . ?
H41A C41A H41B 109.5 . . ?
H41A C41A H41C 109.5 . . ?
H41B C41A H41C 109.5 . . ?
C25 S38B C39B 105.7(5) . . ?
S38B C39B H39B 112.1 . . ?
C40B C39B S38B 100.4(11) . . ?
C40B C39B H39B 112.1 . . ?
C41B C39B S38B 108.9(10) . . ?
C41B C39B H39B 112.1 . . ?
C41B C39B C40B 110.6(11) . . ?
C39B C40B H40D 109.5 . . ?
C39B C40B H40E 109.5 . . ?
C39B C40B H40F 109.5 . . ?
H40D C40B H40E 109.5 . . ?
H40D C40B H40F 109.5 . . ?
H40E C40B H40F 109.5 . . ?
C39B C41B H41D 109.5 . . ?
C39B C41B H41E 109.5 . . ?
C39B C41B H41F 109.5 . . ?
H41D C41B H41E 109.5 . . ?
H41D C41B H41F 109.5 . . ?
H41E C41B H41F 109.5 . . ?
C25 S38C C39C 103.3(11) . . ?
S38C C39C H39C 112.2 . . ?
C40C C39C S38C 106(3) . . ?
C40C C39C H39C 112.2 . . ?
C40C C39C C41C 111(2) . . ?
C41C C39C S38C 103(4) . . ?
C41C C39C H39C 112.2 . . ?
C39C C40C H40G 109.5 . . ?
C39C C40C H40H 109.5 . . ?
C39C C40C H40I 109.5 . . ?
H40G C40C H40H 109.5 . . ?
H40G C40C H40I 109.5 . . ?
H40H C40C H40I 109.5 . . ?
C39C C41C H41G 109.5 . . ?
C39C C41C H41H 109.5 . . ?
C39C C41C H41I 109.5 . . ?
H41G C41C H41H 109.5 . . ?
H41G C41C H41I 109.5 . . ?
H41H C41C H41I 109.5 . . ?
F44A B42 F43A 106.1(7) . . ?
F45A B42 F43A 108.5(8) . . ?
F45A B42 F44A 116.9(8) . . ?
F45A B42 F46A 111.7(8) . . ?
F46A B42 F43A 108.4(8) . . ?
F46A B42 F44A 104.8(7) . . ?
F43B B42 F46B 109.8(15) . . ?
F44B B42 F43B 112.9(15) . . ?
F44B B42 F46B 107.8(14) . . ?
F45B B42 F43B 108.1(14) . . ?
F45B B42 F44B 110.0(13) . . ?
F45B B42 F46B 108.2(14) . . ?
F43C B42 F45C 107.3(10) . . ?
F43C B42 F46C 105.5(9) . . ?
F44C B42 F43C 116.9(11) . . ?
F44C B42 F45C 113.6(11) . . ?
F44C B42 F46C 112.0(11) . . ?
F46C B42 F45C 100.0(9) . . ?
F49A B47A F48A 113.9(12) . . ?
F50A B47A F48A 101.7(10) . . ?
F50A B47A F49A 108.8(11) . . ?
F51A B47A F48A 108.2(11) . . ?
F51A B47A F49A 109.0(11) . . ?
F51A B47A F50A 115.3(12) . . ?
F48B B47B F49B 104.0(12) . . ?
F48B B47B F50B 117.7(11) . . ?
F48B B47B F51B 108.6(10) . . ?
F49B B47B F50B 111.1(10) . . ?
F49B B47B F51B 109.7(10) . . ?
F51B B47B F50B 105.6(11) . . ?

####################################################################### 
# 
# 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_h2o210
_database_code_depnum_ccdc_archive 'CCDC 1976620'
_audit_update_record             
;
2020-01-09 deposited with the CCDC.	2020-05-26 downloaded from the CCDC.
;
_audit_creation_date             2018-06-27
_audit_creation_method           
;
  Olex2 1.2
  (compiled Apr 23 2013 17:54:37, GUI svn.r4466)
;
_chemical_name_common            ?
_chemical_name_systematic        
;
Bis[4-(isopropylsulfanyl)-2,6-di(pyrazol-1-yl)pyridine]iron(II)
ditetrafluoroborate hydrate 
;
_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         818.23
_chemical_melting_point          ?
loop_
_atom_type_symbol
_atom_type_description
_atom_type_scat_dispersion_real
_atom_type_scat_dispersion_imag
_atom_type_scat_source
B B 0.0090 0.0039 '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'
F F 0.0727 0.0534 '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'

_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_id
_space_group_symop_operation_xyz
1 'x, y, z'
2 '-x, y+1/2, -z+1/2'
3 '-x, -y, -z'
4 'x, -y-1/2, z-1/2'

_cell_length_a                   19.983(2)
_cell_length_b                   11.8766(10)
_cell_length_c                   15.6253(14)
_cell_angle_alpha                90.00
_cell_angle_beta                 102.643(10)
_cell_angle_gamma                90.00
_cell_volume                     3618.4(6)
_cell_formula_units_Z            4
_cell_measurement_reflns_used    3037
_cell_measurement_temperature    210(2)
_cell_measurement_theta_min      4.53
_cell_measurement_theta_max      72.80
_exptl_absorpt_coefficient_mu    5.149
_exptl_absorpt_correction_T_min  0.449
_exptl_absorpt_correction_T_max  1.000
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   
;
CrysAlisPro 1.171.39.46 (Rigaku Oxford Diffraction, 2018)
Empirical absorption correction using spherical harmonics,
 implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_crystal_colour            red
_exptl_crystal_density_diffrn    1.502
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       plate
_exptl_crystal_F_000             1672
_exptl_crystal_size_max          0.35
_exptl_crystal_size_mid          0.30
_exptl_crystal_size_min          0.10
_exptl_special_details           
;
 ? 
;
_diffrn_reflns_av_R_equivalents  0.0388
_diffrn_reflns_av_unetI/netI     0.0572
_diffrn_reflns_limit_h_max       23
_diffrn_reflns_limit_h_min       -24
_diffrn_reflns_limit_k_max       14
_diffrn_reflns_limit_k_min       -10
_diffrn_reflns_limit_l_max       18
_diffrn_reflns_limit_l_min       -19
_diffrn_reflns_number            13504
_diffrn_reflns_theta_full        72.00
_diffrn_reflns_theta_max         73.62
_diffrn_reflns_theta_min         4.36
_diffrn_ambient_temperature      210(2)
_diffrn_detector_area_resol_mean 5.3095
_diffrn_measured_fraction_theta_full 0.984
_diffrn_measured_fraction_theta_max 0.966
_diffrn_measurement_device_type  'SuperNova, Dual, Cu at zero, Atlas'
_diffrn_measurement_method       'ω scans'
_diffrn_radiation_monochromator  mirror
_diffrn_radiation_type           CuK\a
_diffrn_radiation_wavelength     1.54184
_diffrn_radiation_source         'SuperNova (Cu) X-ray Source'
_diffrn_standards_number         0
_diffrn_standards_interval_count 0
_diffrn_standards_interval_time  0
_diffrn_standards_decay_%        0
_reflns_number_gt                5296
_reflns_number_total             7065
_reflns_threshold_expression     >2sigma(I)
_computing_data_collection       'CrysAlisPro, Agilent Technologies'
_computing_cell_refinement       'CrysAlisPro, Agilent Technologies'
_computing_data_reduction        'CrysAlisPro, Agilent Technologies'
_computing_molecular_graphics    'XSEED (Barbour, 2001)'
_computing_publication_material  
;
O. V. Dolomanov, L. J. Bourhis, R. J. Gildea, J. A. K. Howard and H. Puschmann,
OLEX2: a complete structure solution, refinement and analysis program.
J. Appl. Cryst. (2009). 42, 339-341.
;
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_refine_diff_density_max         0.756
_refine_diff_density_min         -0.838
_refine_diff_density_rms         0.096
_refine_ls_extinction_coef       ?
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.068
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     474
_refine_ls_number_reflns         7065
_refine_ls_number_restraints     62
_refine_ls_R_factor_all          0.1378
_refine_ls_R_factor_gt           0.1145
_refine_ls_restrained_S_all      1.073
_refine_ls_shift/su_max          0.000
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details     
'calc w=1/[σ²(Fo²)+(0.1029P)²+20.0840P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.2853
_refine_ls_wR_factor_ref         0.3016
_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 isopropylsulfanyl substituent is disordered, over two equally occupied 
 orientations. This was 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 the BF₄⁻ ions is disordered, one 
 over two equally occupied sites and the other over three sites of occupancy 
 0.5, 0.4 and 0.1 which all share a common fully occupied B atom. The anions 
 were treated with the refined restraints B---F = 1.39(2) and F...F = 
 2.27(2) Å. The water molecule was also modelled as disordered, over two 
 sites with occupancies of 0.67 and 0.33. All fully occupied non-H 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 Fouier map and could not be included in the 
 model, but are accounted for in the molecular weight and density 
 calculations.  
;
_olex2_refinement_description    
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups
 At 1.5 times of:
  All C(H,H,H) groups
2. Restrained distances
 B42-F43A = B42-F44A = B42-F45A = B42-F46A
 1.38867 with sigma of 0.02
 B42-F43B = B42-F44B = B42-F45B = B42-F46B
 1.38867 with sigma of 0.02
 B42-F43C = B42-F44C = B42-F45C = B42-F46C
 1.38867 with sigma of 0.02
 F43A-F44A = F43A-F45A = F43A-F46A = F44A-F45A = F44A-F46A = F45A-F46A
 2.267698 with sigma of 0.02
 F43B-F44B = F43B-F45B = F43B-F46B = F44B-F45B = F44B-F46B = F45B-F46B
 2.267698 with sigma of 0.02
 F43C-F44C = F43C-F45C = F43C-F46C = F44C-F45C = F44C-F46C = F45C-F46C
 2.267698 with sigma of 0.02
 B47A-F48A = B47A-F49A = B47A-F50A = B47A-F51A
 1.38867 with sigma of 0.02
 B47B-F48B = B47B-F49B = B47B-F50B = B47B-F51B
 1.38867 with sigma of 0.02
 F48A-F49A = F48A-F50A = F48A-F51A = F49A-F50A = F49A-F51A = F50A-F51A
 2.267698 with sigma of 0.02
 F48B-F49B = F48B-F50B = F48B-F51B = F49B-F50B = F49B-F51B = F50B-F51B
 2.267698 with sigma of 0.02
 C25-S38A = C25-S38B
 1.75 with sigma of 0.02
 S38A-C39A = S38B-C39B
 1.82 with sigma of 0.02
 C39A-C40A = C39A-C41A = C39B-C40B = C39B-C41B
 1.52 with sigma of 0.02
 C40A-C41A = C40B-C41B
 2.48 with sigma of 0.02
 C25-C39A = C25-C39B
 2.83 with sigma of 0.02
3. Others
 1(DFIX)=1(DFIX)=1(DFIX)=1(DFIX)=1(DFIX)=FVAR(1)
 1(DFIX)=1(DFIX)=1(DFIX)=1(DFIX)=1(DFIX)=1.633*FVAR(2)
 Fixed Sof: S38A(0.5) C39A(0.5) H39A(0.5) C40A(0.5) H40A(0.5) H40B(0.5)
 H40C(0.5) C41A(0.5) H41A(0.5) H41B(0.5) H41C(0.5) S38B(0.5) C39B(0.5)
 H39B(0.5) C40B(0.5) H40D(0.5) H40E(0.5) H40F(0.5) C41B(0.5) H41D(0.5)
 H41E(0.5) H41F(0.5) F43A(0.5) F44A(0.5) F45A(0.5) F46A(0.5) F43B(0.4)
 F44B(0.4) F45B(0.4) F46B(0.4) F43C(0.1) F44C(0.1) F45C(0.1) F46C(0.1)
 B47A(0.5) F48A(0.5) F49A(0.5) F50A(0.5) F51A(0.5) B47B(0.5) F48B(0.5)
 F49B(0.5) F50B(0.5) F51B(0.5) O52A(0.67) O52B(0.33)
4.a Ternary CH refined with riding coordinates:
 C19(H19), C39A(H39A), C39B(H39B)
4.b Me refined with riding coordinates:
 C40A(H40A,H40B,H40C), C41A(H41A,H41B,H41C), C40B(H40D,H40E,H40F), C41B(H41D,
 H41E,H41F)
4.c Aromatic/amide H refined with riding coordinates:
 C4(H4), C6(H6), C10(H10), C11(H11), C12(H12), C15(H15), C16(H16), C17(H17),
 C24(H24), C26(H26), C30(H30), C31(H31), C32(H32), C35(H35), C36(H36), C37(H37)
4.d Idealised Me refined as rotating group:
 C20(H20A,H20B,H20C), C21(H21A,H21B,H21C)
;
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_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_symmetry_multiplicity
_atom_site_calc_flag
_atom_site_refinement_flags
_atom_site_disorder_assembly
_atom_site_disorder_group
Fe1 Fe 0.23173(6) 0.60998(10) 0.07783(8) 0.0467(3) Uani 1 1 d . A .
N2 N 0.1321(3) 0.6310(5) 0.0469(4) 0.0491(14) Uani 1 1 d . . .
C3 C 0.1026(4) 0.7077(6) -0.0123(5) 0.0511(17) Uani 1 1 d . . .
C4 C 0.0340(4) 0.7358(7) -0.0287(5) 0.0567(19) Uani 1 1 d . . .
H4 H 0.0153 0.7910 -0.0713 0.068 Uiso 1 1 calc R . .
C5 C -0.0065(4) 0.6807(7) 0.0193(5) 0.0533(18) Uani 1 1 d . . .
C6 C 0.0232(4) 0.5994(7) 0.0825(5) 0.0581(19) Uani 1 1 d . . .
H6 H -0.0036 0.5614 0.1168 0.070 Uiso 1 1 calc R . .
C7 C 0.0916(4) 0.5775(6) 0.0927(5) 0.0503(17) Uani 1 1 d . . .
N8 N 0.1533(4) 0.7587(6) -0.0513(4) 0.0613(18) Uani 1 1 d . . .
N9 N 0.2212(4) 0.7329(6) -0.0148(5) 0.0620(18) Uani 1 1 d . . .
C10 C 0.2563(6) 0.8000(8) -0.0553(8) 0.088(3) Uani 1 1 d . . .
H10 H 0.3050 0.8015 -0.0447 0.106 Uiso 1 1 calc R . .
C11 C 0.2143(7) 0.8673(10) -0.1145(9) 0.106(5) Uani 1 1 d . . .
H11 H 0.2286 0.9229 -0.1504 0.127 Uiso 1 1 calc R . .
C12 C 0.1489(7) 0.8410(8) -0.1132(6) 0.081(3) Uani 1 1 d . . .
H12 H 0.1084 0.8730 -0.1479 0.098 Uiso 1 1 calc R . .
N13 N 0.1294(3) 0.5021(5) 0.1538(4) 0.0542(15) Uani 1 1 d . . .
N14 N 0.1991(3) 0.4974(6) 0.1595(4) 0.0549(15) Uani 1 1 d . . .
C15 C 0.2210(5) 0.4179(8) 0.2194(5) 0.066(2) Uani 1 1 d . . .
H15 H 0.2676 0.3963 0.2387 0.079 Uiso 1 1 calc R . .
C16 C 0.1672(6) 0.3705(8) 0.2501(6) 0.079(3) Uani 1 1 d . . .
H16 H 0.1700 0.3122 0.2924 0.095 Uiso 1 1 calc R . .
C17 C 0.1091(6) 0.4253(8) 0.2070(6) 0.070(2) Uani 1 1 d . . .
H17 H 0.0635 0.4120 0.2132 0.084 Uiso 1 1 calc R . .
S18 S -0.09434(11) 0.7014(2) 0.00911(17) 0.0689(6) Uani 1 1 d . . .
C19 C -0.1140(5) 0.8354(8) -0.0478(6) 0.066(2) Uani 1 1 d . . .
H19 H -0.0955 0.8351 -0.1023 0.079 Uiso 1 1 calc R . .
C20 C -0.0820(5) 0.9317(9) 0.0106(7) 0.080(3) Uani 1 1 d . . .
H20A H -0.0948 1.0033 -0.0198 0.120 Uiso 1 1 calc R . .
H20B H -0.0320 0.9238 0.0242 0.120 Uiso 1 1 calc R . .
H20C H -0.0987 0.9304 0.0651 0.120 Uiso 1 1 calc R . .
C21 C -0.1916(5) 0.8456(10) -0.0723(8) 0.092(3) Uani 1 1 d . . .
H21A H -0.2092 0.8567 -0.0192 0.138 Uiso 1 1 calc R . .
H21B H -0.2112 0.7767 -0.1021 0.138 Uiso 1 1 calc R . .
H21C H -0.2044 0.9101 -0.1116 0.138 Uiso 1 1 calc R . .
N22 N 0.3304(3) 0.5908(5) 0.1239(4) 0.0501(14) Uani 1 1 d . A .
C23 C 0.3657(4) 0.5137(7) 0.0893(5) 0.0521(17) Uani 1 1 d . . .
C24 C 0.4336(4) 0.4906(7) 0.1233(6) 0.059(2) Uani 1 1 d . A .
H24 H 0.4572 0.4349 0.0976 0.071 Uiso 1 1 calc R . .
C25 C 0.4671(4) 0.5513(7) 0.1968(5) 0.062(2) Uani 1 1 d D . .
C26 C 0.4314(4) 0.6340(7) 0.2325(5) 0.0562(19) Uani 1 1 d . A .
H26 H 0.4533 0.6777 0.2816 0.067 Uiso 1 1 calc R . .
C27 C 0.3633(4) 0.6494(6) 0.1935(5) 0.0484(16) Uani 1 1 d . . .
N28 N 0.3231(4) 0.4586(5) 0.0164(4) 0.0567(16) Uani 1 1 d . . .
N29 N 0.2553(4) 0.4886(6) -0.0031(4) 0.0628(19) Uani 1 1 d . . .
C30 C 0.2277(6) 0.4296(9) -0.0730(6) 0.074(3) Uani 1 1 d . . .
H30 H 0.1808 0.4327 -0.1024 0.089 Uiso 1 1 calc R . .
C31 C 0.2763(7) 0.3626(10) -0.0976(6) 0.094(4) Uani 1 1 d . . .
H31 H 0.2688 0.3116 -0.1456 0.113 Uiso 1 1 calc R . .
C32 C 0.3374(6) 0.3826(8) -0.0406(6) 0.077(3) Uani 1 1 d . . .
H32 H 0.3806 0.3498 -0.0412 0.092 Uiso 1 1 calc R . .
N33 N 0.3186(3) 0.7280(5) 0.2206(4) 0.0523(15) Uani 1 1 d . A .
N34 N 0.2518(3) 0.7289(5) 0.1741(4) 0.0508(14) Uani 1 1 d . . .
C35 C 0.2225(5) 0.8127(7) 0.2078(6) 0.061(2) Uani 1 1 d . A .
H35 H 0.1759 0.8345 0.1886 0.074 Uiso 1 1 calc R . .
C36 C 0.2704(6) 0.8657(8) 0.2766(6) 0.075(3) Uani 1 1 d . . .
H36 H 0.2625 0.9279 0.3114 0.090 Uiso 1 1 calc R A .
C37 C 0.3296(5) 0.8084(7) 0.2817(6) 0.063(2) Uani 1 1 d . A .
H37 H 0.3718 0.8229 0.3218 0.076 Uiso 1 1 calc R . .
S38A S 0.5556(3) 0.5242(5) 0.2274(3) 0.0621(13) Uiso 0.50 1 d PD A 1
C39A C 0.5835(8) 0.5978(14) 0.3325(10) 0.048(5) Uiso 0.50 1 d PD A 1
H39A H 0.5420 0.6117 0.3569 0.058 Uiso 0.50 1 calc PR A 1
C40A C 0.6117(14) 0.7114(18) 0.3132(18) 0.075(7) Uiso 0.50 1 d PD A 1
H40A H 0.5774 0.7508 0.2689 0.113 Uiso 0.50 1 calc PR A 1
H40B H 0.6535 0.7004 0.2913 0.113 Uiso 0.50 1 calc PR A 1
H40C H 0.6223 0.7563 0.3671 0.113 Uiso 0.50 1 calc PR A 1
C41A C 0.6361(15) 0.537(2) 0.4025(19) 0.096(11) Uiso 0.50 1 d PD A 1
H41A H 0.6178 0.4635 0.4147 0.144 Uiso 0.50 1 calc PR A 1
H41B H 0.6460 0.5820 0.4563 0.144 Uiso 0.50 1 calc PR A 1
H41C H 0.6785 0.5259 0.3816 0.144 Uiso 0.50 1 calc PR A 1
S38B S 0.5478(2) 0.4966(4) 0.2475(3) 0.0587(12) Uiso 0.50 1 d PD A 2
C39B C 0.5759(10) 0.5806(19) 0.3460(12) 0.085(10) Uiso 0.50 1 d PD A 2
H39B H 0.5412 0.5876 0.3831 0.102 Uiso 0.50 1 calc PR A 2
C40B C 0.597(2) 0.692(3) 0.311(3) 0.133(16) Uiso 0.50 1 d PD A 2
H40D H 0.5555 0.7348 0.2846 0.200 Uiso 0.50 1 calc PR A 2
H40E H 0.6238 0.6776 0.2674 0.200 Uiso 0.50 1 calc PR A 2
H40F H 0.6242 0.7355 0.3599 0.200 Uiso 0.50 1 calc PR A 2
C41B C 0.6404(11) 0.514(2) 0.3890(16) 0.066(7) Uiso 0.50 1 d PD A 2
H41D H 0.6269 0.4426 0.4117 0.099 Uiso 0.50 1 calc PR A 2
H41E H 0.6675 0.5581 0.4374 0.099 Uiso 0.50 1 calc PR A 2
H41F H 0.6678 0.4990 0.3454 0.099 Uiso 0.50 1 calc PR A 2
B42 B 0.4642(5) 0.7291(8) 0.4933(6) 0.080(3) Uani 1 1 d D . .
F43A F 0.5205(8) 0.7353(15) 0.5663(10) 0.129(6) Uiso 0.50 1 d PD B 1
F44A F 0.4810(6) 0.7846(10) 0.4245(7) 0.079(3) Uiso 0.50 1 d PD B 1
F45A F 0.4065(6) 0.7662(13) 0.5163(10) 0.104(4) Uiso 0.50 1 d PD B 1
F46A F 0.4566(9) 0.6150(10) 0.4675(10) 0.115(5) Uiso 0.50 1 d PD B 1
F43B F 0.5332(7) 0.721(2) 0.5271(15) 0.149(9) Uiso 0.40 1 d PD B 2
F44B F 0.4519(10) 0.8367(13) 0.4503(12) 0.119(6) Uiso 0.40 1 d PD B 2
F45B F 0.4292(8) 0.7343(14) 0.5596(9) 0.091(5) Uiso 0.40 1 d PD B 2
F46B F 0.4362(11) 0.6488(15) 0.4323(12) 0.119(9) Uiso 0.40 1 d PD B 2
F43C F 0.5128(14) 0.764(3) 0.451(2) 0.042(8) Uiso 0.10 1 d PD B 3
F44C F 0.4886(16) 0.698(3) 0.5783(12) 0.048(9) Uiso 0.10 1 d PD B 3
F45C F 0.4143(13) 0.815(2) 0.489(2) 0.044(9) Uiso 0.10 1 d PD B 3
F46C F 0.4273(15) 0.636(2) 0.447(2) 0.030(8) Uiso 0.10 1 d PD B 3
B47A B 0.0669(9) 0.9798(16) 0.2300(11) 0.066(11) Uiso 0.50 1 d PD C 1
F48A F 0.1293(6) 1.0316(12) 0.2295(9) 0.088(4) Uiso 0.50 1 d PD C 1
F49A F 0.0086(7) 1.0456(13) 0.2020(10) 0.073(5) Uiso 0.50 1 d PD C 1
F50A F 0.0740(6) 0.9528(10) 0.3193(6) 0.064(3) Uiso 0.50 1 d PD C 1
F51A F 0.0617(6) 0.8849(10) 0.1783(7) 0.079(3) Uiso 0.50 1 d PD C 1
B47B B 0.0681(9) 0.9966(16) 0.2322(11) 0.066(11) Uiso 0.50 1 d PD D 2
F48B F 0.1264(7) 1.0613(13) 0.2525(10) 0.099(5) Uiso 0.50 1 d PD D 2
F49B F 0.0148(8) 1.0717(13) 0.2021(11) 0.090(6) Uiso 0.50 1 d PD D 2
F50B F 0.0544(7) 0.9328(11) 0.3020(8) 0.078(4) Uiso 0.50 1 d PD D 2
F51B F 0.0756(6) 0.9255(11) 0.1646(7) 0.079(3) Uiso 0.50 1 d PD D 2
O52A O 0.6298(9) 0.5632(15) 0.6326(11) 0.105(5) Uiso 0.67 1 d P E 1
O52B O 0.6151(18) 0.590(3) 0.649(2) 0.106(11) Uiso 0.33 1 d P F 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 N2 1.958(6) . ?
Fe1 N9 2.034(7) . ?
Fe1 N14 2.050(7) . ?
Fe1 N22 1.958(6) . ?
Fe1 N29 2.040(8) . ?
Fe1 N34 2.038(6) . ?
N2 C3 1.340(9) . ?
N2 C7 1.352(10) . ?
C3 C4 1.379(11) . ?
C3 N8 1.426(11) . ?
C4 H4 0.9500 . ?
C4 C5 1.382(11) . ?
C5 C6 1.415(11) . ?
C5 S18 1.745(8) . ?
C6 H6 0.9500 . ?
C6 C7 1.367(11) . ?
C7 N13 1.403(10) . ?
N8 N9 1.388(10) . ?
N8 C12 1.364(11) . ?
N9 C10 1.312(11) . ?
C10 H10 0.9500 . ?
C10 C11 1.363(16) . ?
C11 H11 0.9500 . ?
C11 C12 1.348(17) . ?
C12 H12 0.9500 . ?
N13 N14 1.378(9) . ?
N13 C17 1.356(11) . ?
N14 C15 1.335(10) . ?
C15 H15 0.9500 . ?
C15 C16 1.389(14) . ?
C16 H16 0.9500 . ?
C16 C17 1.372(14) . ?
C17 H17 0.9500 . ?
S18 C19 1.823(9) . ?
C19 H19 1.0000 . ?
C19 C20 1.514(13) . ?
C19 C21 1.519(13) . ?
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 C23 1.341(10) . ?
N22 C27 1.338(9) . ?
C23 C24 1.372(11) . ?
C23 N28 1.423(10) . ?
C24 H24 0.9500 . ?
C24 C25 1.397(11) . ?
C25 C26 1.399(11) . ?
C25 S38A 1.757(8) . ?
C25 S38B 1.757(8) . ?
C26 H26 0.9500 . ?
C26 C27 1.376(11) . ?
C27 N33 1.419(10) . ?
N28 N29 1.369(10) . ?
N28 C32 1.341(11) . ?
N29 C30 1.313(11) . ?
C30 H30 0.9500 . ?
C30 C31 1.373(17) . ?
C31 H31 0.9500 . ?
C31 C32 1.364(15) . ?
C32 H32 0.9500 . ?
N33 N34 1.374(9) . ?
N33 C37 1.333(10) . ?
N34 C35 1.320(10) . ?
C35 H35 0.9500 . ?
C35 C36 1.420(13) . ?
C36 H36 0.9500 . ?
C36 C37 1.352(14) . ?
C37 H37 0.9500 . ?
S38A C39A 1.836(12) . ?
C39A H39A 1.0000 . ?
C39A C40A 1.516(17) . ?
C39A C41A 1.524(16) . ?
C40A H40A 0.9800 . ?
C40A H40B 0.9800 . ?
C40A H40C 0.9800 . ?
C41A H41A 0.9800 . ?
C41A H41B 0.9800 . ?
C41A H41C 0.9800 . ?
S38B C39B 1.816(15) . ?
C39B H39B 1.0000 . ?
C39B C40B 1.522(18) . ?
C39B C41B 1.535(17) . ?
C40B H40D 0.9800 . ?
C40B H40E 0.9800 . ?
C40B H40F 0.9800 . ?
C41B H41D 0.9800 . ?
C41B H41E 0.9800 . ?
C41B H41F 0.9800 . ?
B42 F43A 1.418(13) . ?
B42 F44A 1.364(12) . ?
B42 F45A 1.354(12) . ?
B42 F46A 1.413(13) . ?
B42 F43B 1.368(14) . ?
B42 F44B 1.439(14) . ?
B42 F45B 1.372(13) . ?
B42 F46B 1.378(14) . ?
B42 F43C 1.354(16) . ?
B42 F44C 1.362(16) . ?
B42 F45C 1.419(16) . ?
B42 F46C 1.429(16) . ?
B47A F48A 1.393(16) . ?
B47A F49A 1.392(16) . ?
B47A F50A 1.408(16) . ?
B47A F51A 1.377(17) . ?
B47B F48B 1.375(16) . ?
B47B F49B 1.390(16) . ?
B47B F50B 1.403(16) . ?
B47B F51B 1.385(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
N2 Fe1 N9 78.0(3) . . ?
N2 Fe1 N14 78.0(3) . . ?
N2 Fe1 N29 107.3(3) . . ?
N2 Fe1 N34 96.8(3) . . ?
N9 Fe1 N14 156.0(3) . . ?
N9 Fe1 N29 93.9(3) . . ?
N9 Fe1 N34 90.0(3) . . ?
N22 Fe1 N2 172.9(3) . . ?
N22 Fe1 N9 106.5(3) . . ?
N22 Fe1 N14 97.3(3) . . ?
N22 Fe1 N29 78.2(3) . . ?
N22 Fe1 N34 77.9(3) . . ?
N29 Fe1 N14 94.2(3) . . ?
N34 Fe1 N14 91.7(3) . . ?
N34 Fe1 N29 155.9(3) . . ?
C3 N2 Fe1 121.9(5) . . ?
C3 N2 C7 117.4(7) . . ?
C7 N2 Fe1 120.3(5) . . ?
N2 C3 C4 124.2(8) . . ?
N2 C3 N8 109.7(7) . . ?
C4 C3 N8 126.0(7) . . ?
C3 C4 H4 121.3 . . ?
C3 C4 C5 117.4(7) . . ?
C5 C4 H4 121.3 . . ?
C4 C5 C6 119.8(7) . . ?
C4 C5 S18 125.4(6) . . ?
C6 C5 S18 114.8(6) . . ?
C5 C6 H6 121.1 . . ?
C7 C6 C5 117.8(8) . . ?
C7 C6 H6 121.1 . . ?
N2 C7 C6 123.4(7) . . ?
N2 C7 N13 111.4(7) . . ?
C6 C7 N13 125.2(7) . . ?
N9 N8 C3 117.0(6) . . ?
C12 N8 C3 131.8(8) . . ?
C12 N8 N9 110.7(8) . . ?
N8 N9 Fe1 113.0(5) . . ?
C10 N9 Fe1 142.8(8) . . ?
C10 N9 N8 104.2(8) . . ?
N9 C10 H10 124.2 . . ?
N9 C10 C11 111.6(11) . . ?
C11 C10 H10 124.2 . . ?
C10 C11 H11 126.0 . . ?
C12 C11 C10 108.0(9) . . ?
C12 C11 H11 126.0 . . ?
N8 C12 H12 127.3 . . ?
C11 C12 N8 105.4(10) . . ?
C11 C12 H12 127.3 . . ?
N14 N13 C7 117.1(6) . . ?
C17 N13 C7 131.1(8) . . ?
C17 N13 N14 111.6(7) . . ?
N13 N14 Fe1 112.8(5) . . ?
C15 N14 Fe1 143.0(6) . . ?
C15 N14 N13 104.2(7) . . ?
N14 C15 H15 124.1 . . ?
N14 C15 C16 111.7(8) . . ?
C16 C15 H15 124.1 . . ?
C15 C16 H16 127.0 . . ?
C17 C16 C15 105.9(8) . . ?
C17 C16 H16 127.0 . . ?
N13 C17 C16 106.6(9) . . ?
N13 C17 H17 126.7 . . ?
C16 C17 H17 126.7 . . ?
C5 S18 C19 105.8(4) . . ?
S18 C19 H19 109.4 . . ?
C20 C19 S18 110.4(7) . . ?
C20 C19 H19 109.4 . . ?
C20 C19 C21 111.4(8) . . ?
C21 C19 S18 107.0(7) . . ?
C21 C19 H19 109.4 . . ?
C19 C20 H20A 109.5 . . ?
C19 C20 H20B 109.5 . . ?
C19 C20 H20C 109.5 . . ?
H20A C20 H20B 109.5 . . ?
H20A C20 H20C 109.5 . . ?
H20B C20 H20C 109.5 . . ?
C19 C21 H21A 109.5 . . ?
C19 C21 H21B 109.5 . . ?
C19 C21 H21C 109.5 . . ?
H21A C21 H21B 109.5 . . ?
H21A C21 H21C 109.5 . . ?
H21B C21 H21C 109.5 . . ?
C23 N22 Fe1 120.6(5) . . ?
C27 N22 Fe1 121.0(5) . . ?
C27 N22 C23 118.3(7) . . ?
N22 C23 C24 123.0(7) . . ?
N22 C23 N28 111.1(7) . . ?
C24 C23 N28 125.9(7) . . ?
C23 C24 H24 121.0 . . ?
C23 C24 C25 118.1(7) . . ?
C25 C24 H24 121.0 . . ?
C24 C25 C26 119.7(7) . . ?
C24 C25 S38A 113.7(6) . . ?
C24 C25 S38B 114.0(6) . . ?
C26 C25 S38A 126.2(6) . . ?
C26 C25 S38B 125.3(6) . . ?
C25 C26 H26 121.3 . . ?
C27 C26 C25 117.3(7) . . ?
C27 C26 H26 121.3 . . ?
N22 C27 C26 123.6(7) . . ?
N22 C27 N33 110.8(6) . . ?
C26 C27 N33 125.6(7) . . ?
N29 N28 C23 116.6(7) . . ?
C32 N28 C23 131.6(8) . . ?
C32 N28 N29 111.8(8) . . ?
N28 N29 Fe1 113.4(5) . . ?
C30 N29 Fe1 141.4(8) . . ?
C30 N29 N28 105.1(8) . . ?
N29 C30 H30 124.8 . . ?
N29 C30 C31 110.4(9) . . ?
C31 C30 H30 124.8 . . ?
C30 C31 H31 126.2 . . ?
C32 C31 C30 107.6(10) . . ?
C32 C31 H31 126.2 . . ?
N28 C32 C31 105.1(11) . . ?
N28 C32 H32 127.4 . . ?
C31 C32 H32 127.4 . . ?
N34 N33 C27 116.7(6) . . ?
C37 N33 C27 132.0(7) . . ?
C37 N33 N34 111.2(7) . . ?
N33 N34 Fe1 113.4(4) . . ?
C35 N34 Fe1 141.6(6) . . ?
C35 N34 N33 105.0(7) . . ?
N34 C35 H35 124.7 . . ?
N34 C35 C36 110.6(8) . . ?
C36 C35 H35 124.7 . . ?
C35 C36 H36 127.6 . . ?
C37 C36 C35 104.9(8) . . ?
C37 C36 H36 127.6 . . ?
N33 C37 C36 108.3(8) . . ?
N33 C37 H37 125.8 . . ?
C36 C37 H37 125.8 . . ?
C25 S38A C39A 104.3(6) . . ?
S38A C39A H39A 107.7 . . ?
C40A C39A S38A 107.4(15) . . ?
C40A C39A H39A 107.7 . . ?
C40A C39A C41A 109.7(14) . . ?
C41A C39A S38A 116.3(16) . . ?
C41A C39A H39A 107.7 . . ?
C39A C40A H40A 109.5 . . ?
C39A C40A H40B 109.5 . . ?
C39A C40A H40C 109.5 . . ?
H40A C40A H40B 109.5 . . ?
H40A C40A H40C 109.5 . . ?
H40B C40A H40C 109.5 . . ?
C39A C41A H41A 109.5 . . ?
C39A C41A H41B 109.5 . . ?
C39A C41A H41C 109.5 . . ?
H41A C41A H41B 109.5 . . ?
H41A C41A H41C 109.5 . . ?
H41B C41A H41C 109.5 . . ?
C25 S38B C39B 105.2(7) . . ?
S38B C39B H39B 114.3 . . ?
C40B C39B S38B 104(2) . . ?
C40B C39B H39B 114.3 . . ?
C40B C39B C41B 109.6(16) . . ?
C41B C39B S38B 99.4(15) . . ?
C41B C39B H39B 114.3 . . ?
C39B C40B H40D 109.5 . . ?
C39B C40B H40E 109.5 . . ?
C39B C40B H40F 109.5 . . ?
H40D C40B H40E 109.5 . . ?
H40D C40B H40F 109.5 . . ?
H40E C40B H40F 109.5 . . ?
C39B C41B H41D 109.5 . . ?
C39B C41B H41E 109.5 . . ?
C39B C41B H41F 109.5 . . ?
H41D C41B H41E 109.5 . . ?
H41D C41B H41F 109.5 . . ?
H41E C41B H41F 109.5 . . ?
F44A B42 F43A 108.7(10) . . ?
F44A B42 F46A 105.5(10) . . ?
F45A B42 F43A 109.9(10) . . ?
F45A B42 F44A 115.1(10) . . ?
F45A B42 F46A 110.1(11) . . ?
F46A B42 F43A 107.2(11) . . ?
F43B B42 F44B 107.2(12) . . ?
F43B B42 F45B 110.4(12) . . ?
F43B B42 F46B 116.2(13) . . ?
F45B B42 F44B 104.4(11) . . ?
F45B B42 F46B 110.9(12) . . ?
F46B B42 F44B 106.9(11) . . ?
F43C B42 F44C 114.7(15) . . ?
F43C B42 F45C 109.2(14) . . ?
F43C B42 F46C 109.7(14) . . ?
F44C B42 F45C 109.8(14) . . ?
F44C B42 F46C 108.4(14) . . ?
F45C B42 F46C 104.6(14) . . ?
F48A B47A F50A 102.1(12) . . ?
F49A B47A F48A 116.0(15) . . ?
F49A B47A F50A 109.6(13) . . ?
F51A B47A F48A 108.1(13) . . ?
F51A B47A F49A 108.9(13) . . ?
F51A B47A F50A 111.9(14) . . ?
F48B B47B F49B 105.5(14) . . ?
F48B B47B F50B 115.0(14) . . ?
F48B B47B F51B 106.8(13) . . ?
F49B B47B F50B 110.2(13) . . ?
F51B B47B F49B 109.7(14) . . ?
F51B B47B F50B 109.6(14) . . ?

####################################################################### 
# 
# 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_h2o250
_database_code_depnum_ccdc_archive 'CCDC 1976621'
_audit_update_record             
;
2020-01-09 deposited with the CCDC.	2020-05-26 downloaded from the CCDC.
;
_audit_creation_date             2018-06-23
_audit_creation_method           
;
  Olex2 1.2
  (compiled Apr 23 2013 17:54:37, GUI svn.r4466)
;
_chemical_name_common            ?
_chemical_name_systematic        
;
Bis[4-(isopropylsulfanyl)-2,6-di(pyrazol-1-yl)pyridine]iron(II)
ditetrafluoroborate hydrate
;
_chemical_formula_moiety         'C28 H29.55 Fe N10 S2, 2(B F4), H2 O'
_chemical_formula_sum            'C28 H32 B2 F8 Fe N10 O S2'
_chemical_formula_weight         818.23
_chemical_melting_point          ?
loop_
_atom_type_symbol
_atom_type_description
_atom_type_scat_dispersion_real
_atom_type_scat_dispersion_imag
_atom_type_scat_source
B B 0.0090 0.0039 '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'
F F 0.0727 0.0534 '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'

_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_id
_space_group_symop_operation_xyz
1 'x, y, z'
2 '-x, y+1/2, -z+1/2'
3 '-x, -y, -z'
4 'x, -y-1/2, z-1/2'

_cell_length_a                   20.3054(8)
_cell_length_b                   11.6878(6)
_cell_length_c                   15.8081(8)
_cell_angle_alpha                90.00
_cell_angle_beta                 102.737(5)
_cell_angle_gamma                90.00
_cell_volume                     3659.3(3)
_cell_formula_units_Z            4
_cell_measurement_reflns_used    4100
_cell_measurement_temperature    250(2)
_cell_measurement_theta_min      4.44
_cell_measurement_theta_max      70.90
_exptl_absorpt_coefficient_mu    5.092
_exptl_absorpt_correction_T_min  0.435
_exptl_absorpt_correction_T_max  1.000
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   
;
CrysAlisPro 1.171.39.46 (Rigaku Oxford Diffraction, 2018)
Empirical absorption correction using spherical harmonics,
 implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_crystal_colour            yellow
_exptl_crystal_density_diffrn    1.485
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       plate
_exptl_crystal_F_000             1672
_exptl_crystal_size_max          0.35
_exptl_crystal_size_mid          0.30
_exptl_crystal_size_min          0.10
_exptl_special_details           
;
 ? 
;
_diffrn_reflns_av_R_equivalents  0.0319
_diffrn_reflns_av_unetI/netI     0.0433
_diffrn_reflns_limit_h_max       24
_diffrn_reflns_limit_h_min       -23
_diffrn_reflns_limit_k_max       14
_diffrn_reflns_limit_k_min       -10
_diffrn_reflns_limit_l_max       19
_diffrn_reflns_limit_l_min       -19
_diffrn_reflns_number            13962
_diffrn_reflns_theta_full        72.00
_diffrn_reflns_theta_max         73.38
_diffrn_reflns_theta_min         4.39
_diffrn_ambient_temperature      250(2)
_diffrn_detector_area_resol_mean 5.3095
_diffrn_measured_fraction_theta_full 0.985
_diffrn_measured_fraction_theta_max 0.973
_diffrn_measurement_device_type  'SuperNova, Dual, Cu at zero, Atlas'
_diffrn_measurement_method       'ω scans'
_diffrn_radiation_monochromator  mirror
_diffrn_radiation_type           CuK\a
_diffrn_radiation_wavelength     1.54184
_diffrn_radiation_source         'SuperNova (Cu) X-ray Source'
_diffrn_standards_number         0
_diffrn_standards_interval_count 0
_diffrn_standards_interval_time  0
_diffrn_standards_decay_%        0
_reflns_number_gt                5342
_reflns_number_total             7161
_reflns_threshold_expression     >2sigma(I)
_computing_data_collection       'CrysAlisPro, Agilent Technologies'
_computing_cell_refinement       'CrysAlisPro, Agilent Technologies'
_computing_data_reduction        'CrysAlisPro, Agilent Technologies'
_computing_molecular_graphics    'XSEED (Barbour, 2001)'
_computing_publication_material  
;
O. V. Dolomanov, L. J. Bourhis, R. J. Gildea, J. A. K. Howard and H. Puschmann,
OLEX2: a complete structure solution, refinement and analysis program.
J. Appl. Cryst. (2009). 42, 339-341.
;
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_refine_diff_density_max         0.591
_refine_diff_density_min         -1.057
_refine_diff_density_rms         0.082
_refine_ls_extinction_coef       ?
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.060
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     494
_refine_ls_number_reflns         7161
_refine_ls_number_restraints     68
_refine_ls_R_factor_all          0.1030
_refine_ls_R_factor_gt           0.0826
_refine_ls_restrained_S_all      1.074
_refine_ls_shift/su_max          0.005
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details     
'calc w=1/[σ²(Fo²)+(0.1280P)²+5.4858P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.2322
_refine_ls_wR_factor_ref         0.2495
_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 isopropylsulfanyl substitutents on the complex cation is 
 disordered over three orientations, with occupancies of 0.50, 0.35 and 0.15.
 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. Both BF₄⁻ ions are also disordered, one 
 over two half-occupied sites and the other over three orientations of
 occupancy 0.5, 0.25 and 0;25 which share a common fully occupied B atom. 
 The refined restraints B---F = 1.39(2) and F...F = 2.27(2) Å were applied 
 to those residues. Lastly, the water molecule was also refined over three 
 different sites with a 0.6:0.3:0.1 occupancy ratio.

 All fully occupied non-H 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 could not be located and are not included in
 the model, but are accounted for in the density and F(000) calculations. 
 This disordered water site is positioned to hydrogen bond to anion 
 B42-F46, and to its own symmetry equivalent related by 1-x, 1-y, 1-z.

 The deepest residual Fourier peak of -1.0 e.Å⁻³ is associated with the 
 disordered S atom S38.
;
_olex2_refinement_description    
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups
 At 1.5 times of:
  All C(H,H,H) groups
2. Restrained distances
 B42-F43A = B42-F44A = B42-F45A = B42-F46A
 1.38922 with sigma of 0.02
 B42-F43B = B42-F44B = B42-F45B = B42-F46B
 1.38922 with sigma of 0.02
 B42-F43C = B42-F44C = B42-F45C = B42-F46C
 1.38922 with sigma of 0.02
 F43A-F44A = F43A-F45A = F43A-F46A = F44A-F45A = F44A-F46A = F45A-F46A
 2.268596 with sigma of 0.02
 F43B-F44B = F43B-F45B = F43B-F46B = F44B-F45B = F44B-F46B = F45B-F46B
 2.268596 with sigma of 0.02
 F43C-F44C = F43C-F45C = F43C-F46C = F44C-F45C = F44C-F46C = F45C-F46C
 2.268596 with sigma of 0.02
 B47A-F48A = B47A-F49A = B47A-F50A = B47A-F51A
 1.38922 with sigma of 0.02
 B47B-F48B = B47B-F49B = B47B-F50B = B47B-F51B
 1.38922 with sigma of 0.02
 F48A-F49A = F48A-F50A = F48A-F51A = F49A-F50A = F49A-F51A = F50A-F51A
 2.268596 with sigma of 0.02
 F48B-F49B = F48B-F50B = F48B-F51B = F49B-F50B = F49B-F51B = F50B-F51B
 2.268596 with sigma of 0.02
 C25-S38A = C25-S38B = C25-S38C
 1.75 with sigma of 0.02
 S38A-C39A = S38B-C39B = S38C-C39C
 1.82 with sigma of 0.02
 C39A-C40A = C39A-C41A = C39B-C40B = C39B-C41B = C39C-C40C = C39C-C41C
 1.52 with sigma of 0.02
 C40A-C41A = C40B-C41B = C40C-C41C
 2.48 with sigma of 0.02
 C25-C39A = C25-C39B = C25-C39C
 2.83 with sigma of 0.02
3. Others
 1(DFIX)=1(DFIX)=1(DFIX)=1(DFIX)=1(DFIX)=FVAR(1)
 1(DFIX)=1(DFIX)=1(DFIX)=1(DFIX)=1(DFIX)=1.633*FVAR(2)
 Fixed Sof: S38B(0.5) C39B(0.5) H39B(0.5) C40B(0.5) H40A(0.5) H40B(0.5)
 H40C(0.5) C41B(0.5) H41A(0.5) H41B(0.5) H41C(0.5) S38A(0.35) C39A(0.35)
 H39A(0.35) C40A(0.35) H40D(0.35) H40E(0.35) H40F(0.35) C41A(0.35) H41D(0.35)
 H41E(0.35) H41F(0.35) S38C(0.15) C39C(0.15) H39C(0.15) C40C(0.15) H40G(0.15)
 H40H(0.15) H40I(0.15) C41C(0.15) H41G(0.15) H41H(0.15) H41I(0.15) F43A(0.5)
 F44A(0.5) F45A(0.5) F46A(0.5) F43B(0.25) F44B(0.25) F45B(0.25) F46B(0.25)
 F43C(0.25) F44C(0.25) F45C(0.25) F46C(0.25) B47A(0.5) F48A(0.5) F49A(0.5)
 F50A(0.5) F51A(0.5) B47B(0.5) F48B(0.5) F49B(0.5) F50B(0.5) F51B(0.5)
 O52A(0.6) O52B(0.3) O52C(0.1)
4.a Ternary CH refined with riding coordinates:
 C19(H19), C39B(H39B), C39A(H39A), C39C(H39C)
4.b Me refined with riding coordinates:
 C40B(H40A,H40B,H40C), C41B(H41A,H41B,H41C), C40A(H40D,H40E,H40F), C41A(H41D,
 H41E,H41F), C40C(H40G,H40H,H40I), C41C(H41G,H41H,H41I)
4.c Aromatic/amide H refined with riding coordinates:
 C4(H4), C6(H6), C10(H10), C11(H11), C12(H12), C15(H15), C16(H16), C17(H17),
 C24(H24), C26(H26), C30(H30), C31(H31), C32(H32), C35(H35), C36(H36), C37(H37)
4.d Idealised Me refined as rotating group:
 C20(H20A,H20B,H20C), C21(H21A,H21B,H21C)
;
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_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_symmetry_multiplicity
_atom_site_calc_flag
_atom_site_refinement_flags
_atom_site_disorder_assembly
_atom_site_disorder_group
Fe1 Fe 0.22956(3) 0.60432(7) 0.06966(5) 0.0471(2) Uani 1 1 d . A .
N2 N 0.12273(19) 0.6259(3) 0.0425(3) 0.0456(9) Uani 1 1 d . . .
C3 C 0.0934(2) 0.7022(4) -0.0154(3) 0.0439(10) Uani 1 1 d . . .
C4 C 0.0261(2) 0.7321(5) -0.0281(3) 0.0496(11) Uani 1 1 d . . .
H4 H 0.0067 0.7860 -0.0705 0.059 Uiso 1 1 calc R . .
C5 C -0.0118(2) 0.6797(5) 0.0239(4) 0.0523(12) Uani 1 1 d . . .
C6 C 0.0187(3) 0.5983(5) 0.0861(4) 0.0539(12) Uani 1 1 d . . .
H6 H -0.0059 0.5617 0.1223 0.065 Uiso 1 1 calc R . .
C7 C 0.0854(2) 0.5749(4) 0.0915(3) 0.0467(11) Uani 1 1 d . . .
N8 N 0.1382(2) 0.7531(4) -0.0608(3) 0.0483(9) Uani 1 1 d . . .
N9 N 0.2058(2) 0.7313(4) -0.0313(3) 0.0525(10) Uani 1 1 d . . .
C10 C 0.2365(3) 0.7951(6) -0.0802(4) 0.0691(16) Uani 1 1 d . . .
H10 H 0.2835 0.7982 -0.0746 0.083 Uiso 1 1 calc R . .
C11 C 0.1898(4) 0.8575(6) -0.1416(5) 0.0763(19) Uani 1 1 d . . .
H11 H 0.1989 0.9084 -0.1836 0.092 Uiso 1 1 calc R . .
C12 C 0.1276(3) 0.8277(5) -0.1268(4) 0.0626(14) Uani 1 1 d . . .
H12 H 0.0854 0.8549 -0.1573 0.075 Uiso 1 1 calc R . .
N13 N 0.1228(2) 0.4952(4) 0.1509(3) 0.0519(10) Uani 1 1 d . . .
N14 N 0.1907(2) 0.4869(4) 0.1567(3) 0.0536(10) Uani 1 1 d . . .
C15 C 0.2111(3) 0.4039(5) 0.2137(4) 0.0644(15) Uani 1 1 d . . .
H15 H 0.2560 0.3789 0.2317 0.077 Uiso 1 1 calc R . .
C16 C 0.1562(4) 0.3586(6) 0.2435(5) 0.0730(17) Uani 1 1 d . . .
H16 H 0.1575 0.2991 0.2838 0.088 Uiso 1 1 calc R . .
C17 C 0.1008(3) 0.4182(5) 0.2020(4) 0.0631(14) Uani 1 1 d . . .
H17 H 0.0562 0.4078 0.2079 0.076 Uiso 1 1 calc R . .
S18 S -0.09766(6) 0.70371(14) 0.01851(12) 0.0653(4) Uani 1 1 d . . .
C19 C -0.1165(3) 0.8391(6) -0.0386(4) 0.0630(14) Uani 1 1 d . . .
H19 H -0.1004 0.8358 -0.0932 0.076 Uiso 1 1 calc R . .
C20 C -0.0831(4) 0.9368(6) 0.0144(5) 0.0823(19) Uani 1 1 d . . .
H20A H -0.0911 1.0065 -0.0196 0.123 Uiso 1 1 calc R . .
H20B H -0.0350 0.9226 0.0316 0.123 Uiso 1 1 calc R . .
H20C H -0.1016 0.9449 0.0657 0.123 Uiso 1 1 calc R . .
C21 C -0.1930(3) 0.8497(8) -0.0604(6) 0.092(2) Uani 1 1 d . . .
H21A H -0.2093 0.8531 -0.0072 0.137 Uiso 1 1 calc R . .
H21B H -0.2125 0.7839 -0.0942 0.137 Uiso 1 1 calc R . .
H21C H -0.2060 0.9190 -0.0937 0.137 Uiso 1 1 calc R . .
N22 N 0.33338(19) 0.5854(4) 0.1234(3) 0.0469(9) Uani 1 1 d . A .
C23 C 0.3696(2) 0.5089(5) 0.0903(4) 0.0507(11) Uani 1 1 d . . .
C24 C 0.4370(3) 0.4875(6) 0.1249(4) 0.0670(16) Uani 1 1 d . A .
H24 H 0.4613 0.4333 0.1001 0.080 Uiso 1 1 calc R . .
C25 C 0.4675(3) 0.5498(7) 0.1982(5) 0.077(2) Uani 1 1 d D . .
C26 C 0.4307(3) 0.6339(6) 0.2322(4) 0.0644(15) Uani 1 1 d . A .
H26 H 0.4506 0.6784 0.2806 0.077 Uiso 1 1 calc R . .
C27 C 0.3638(2) 0.6473(5) 0.1902(3) 0.0500(11) Uani 1 1 d . . .
N28 N 0.3323(2) 0.4493(4) 0.0181(3) 0.0513(10) Uani 1 1 d . . .
N29 N 0.2653(2) 0.4742(4) -0.0088(3) 0.0490(9) Uani 1 1 d . . .
C30 C 0.2440(3) 0.4089(5) -0.0768(4) 0.0586(13) Uani 1 1 d . . .
H30 H 0.1992 0.4075 -0.1094 0.070 Uiso 1 1 calc R . .
C31 C 0.2962(3) 0.3413(6) -0.0948(4) 0.0696(16) Uani 1 1 d . . .
H31 H 0.2936 0.2876 -0.1397 0.083 Uiso 1 1 calc R . .
C32 C 0.3514(3) 0.3708(6) -0.0330(4) 0.0669(16) Uani 1 1 d . . .
H32 H 0.3952 0.3412 -0.0272 0.080 Uiso 1 1 calc R . .
N33 N 0.3206(2) 0.7285(4) 0.2147(3) 0.0548(10) Uani 1 1 d . A .
N34 N 0.2556(2) 0.7342(4) 0.1681(3) 0.0571(11) Uani 1 1 d . . .
C35 C 0.2285(3) 0.8233(5) 0.2018(5) 0.0688(16) Uani 1 1 d . A .
H35 H 0.1837 0.8480 0.1828 0.083 Uiso 1 1 calc R . .
C36 C 0.2754(4) 0.8740(6) 0.2684(5) 0.080(2) Uani 1 1 d . . .
H36 H 0.2683 0.9379 0.3013 0.096 Uiso 1 1 calc R A .
C37 C 0.3339(3) 0.8132(6) 0.2768(5) 0.0725(17) Uani 1 1 d . A .
H37 H 0.3749 0.8263 0.3168 0.087 Uiso 1 1 calc R . .
S38A S 0.5455(2) 0.4867(4) 0.2595(3) 0.0511(9) Uiso 0.35 1 d PD A 2
C39A C 0.5774(10) 0.5807(16) 0.3480(13) 0.065(7) Uiso 0.35 1 d PD A 2
H39A H 0.5450 0.5911 0.3858 0.077 Uiso 0.35 1 calc PR A 2
C40A C 0.6025(13) 0.6970(17) 0.3191(17) 0.073(6) Uiso 0.35 1 d PD A 2
H40D H 0.5640 0.7451 0.2950 0.109 Uiso 0.35 1 calc PR A 2
H40E H 0.6286 0.6837 0.2756 0.109 Uiso 0.35 1 calc PR A 2
H40F H 0.6306 0.7349 0.3689 0.109 Uiso 0.35 1 calc PR A 2
C41A C 0.6382(9) 0.5096(17) 0.3917(13) 0.061(5) Uiso 0.35 1 d PD A 2
H41D H 0.6231 0.4352 0.4068 0.091 Uiso 0.35 1 calc PR A 2
H41E H 0.6619 0.5483 0.4438 0.091 Uiso 0.35 1 calc PR A 2
H41F H 0.6683 0.5001 0.3523 0.091 Uiso 0.35 1 calc PR A 2
S38B S 0.55350(17) 0.5176(4) 0.2343(2) 0.0631(8) Uiso 0.50 1 d PD A 1
C39B C 0.5808(7) 0.6010(16) 0.3335(9) 0.066(5) Uiso 0.50 1 d PD A 1
H39B H 0.5410 0.6216 0.3570 0.079 Uiso 0.50 1 calc PR A 1
C40B C 0.6057(17) 0.706(2) 0.2941(19) 0.147(13) Uiso 0.50 1 d PD A 1
H40A H 0.5694 0.7368 0.2497 0.221 Uiso 0.50 1 calc PR A 1
H40B H 0.6431 0.6845 0.2684 0.221 Uiso 0.50 1 calc PR A 1
H40C H 0.6205 0.7625 0.3388 0.221 Uiso 0.50 1 calc PR A 1
C41B C 0.6334(11) 0.5458(18) 0.4037(13) 0.100(6) Uiso 0.50 1 d PD A 1
H41A H 0.6164 0.4736 0.4202 0.149 Uiso 0.50 1 calc PR A 1
H41B H 0.6438 0.5960 0.4538 0.149 Uiso 0.50 1 calc PR A 1
H41C H 0.6741 0.5324 0.3824 0.149 Uiso 0.50 1 calc PR A 1
S38C S 0.5565(4) 0.5785(8) 0.2122(5) 0.0477(17) Uiso 0.15 1 d PD A 3
C39C C 0.5769(14) 0.649(4) 0.3174(19) 0.071(12) Uiso 0.15 1 d PD A 3
H39C H 0.5463 0.7147 0.3189 0.085 Uiso 0.15 1 calc PR A 3
C40C C 0.572(3) 0.563(6) 0.387(5) 0.13(3) Uiso 0.15 1 d PD A 3
H40G H 0.5248 0.5417 0.3819 0.194 Uiso 0.15 1 calc PR A 3
H40H H 0.5894 0.5958 0.4436 0.194 Uiso 0.15 1 calc PR A 3
H40I H 0.5976 0.4950 0.3797 0.194 Uiso 0.15 1 calc PR A 3
C41C C 0.6485(18) 0.689(4) 0.325(3) 0.082(13) Uiso 0.15 1 d PD A 3
H41G H 0.6793 0.6358 0.3605 0.123 Uiso 0.15 1 calc PR A 3
H41H H 0.6540 0.7644 0.3523 0.123 Uiso 0.15 1 calc PR A 3
H41I H 0.6583 0.6941 0.2680 0.123 Uiso 0.15 1 calc PR A 3
B42 B 0.4505(4) 0.7286(8) 0.4865(5) 0.095(3) Uani 1 1 d D . .
F43A F 0.5035(7) 0.7342(13) 0.5624(7) 0.134(4) Uiso 0.50 1 d PD B 1
F44A F 0.4738(5) 0.7879(9) 0.4216(6) 0.086(3) Uiso 0.50 1 d PD B 1
F45A F 0.3939(5) 0.7665(11) 0.5035(8) 0.097(3) Uiso 0.50 1 d PD B 1
F46A F 0.4441(8) 0.6148(9) 0.4567(9) 0.137(5) Uiso 0.50 1 d PD B 1
F43B F 0.5082(10) 0.676(2) 0.5382(17) 0.164(12) Uiso 0.25 1 d PD B 2
F44B F 0.4651(12) 0.8341(16) 0.4567(15) 0.130(8) Uiso 0.25 1 d PD B 2
F45B F 0.4051(8) 0.7357(16) 0.5381(11) 0.083(5) Uiso 0.25 1 d PD B 2
F46B F 0.4239(15) 0.658(2) 0.4155(15) 0.175(16) Uiso 0.25 1 d PD B 2
F43C F 0.4954(8) 0.7643(14) 0.4417(11) 0.075(5) Uiso 0.25 1 d PD B 3
F44C F 0.4731(13) 0.701(2) 0.5693(10) 0.145(10) Uiso 0.25 1 d PD B 3
F45C F 0.3986(9) 0.8194(16) 0.4778(14) 0.114(7) Uiso 0.25 1 d PD B 3
F46C F 0.4117(8) 0.6381(13) 0.4378(11) 0.074(4) Uiso 0.25 1 d PD B 3
B47A B 0.0732(7) 0.9807(14) 0.2322(9) 0.060(7) Uiso 0.50 1 d PD C 1
F48A F 0.1353(5) 1.0393(9) 0.2306(7) 0.083(3) Uiso 0.50 1 d PD C 1
F49A F 0.0168(5) 1.0510(9) 0.2019(6) 0.078(3) Uiso 0.50 1 d PD C 1
F50A F 0.0803(4) 0.9602(8) 0.3202(5) 0.075(2) Uiso 0.50 1 d PD C 1
F51A F 0.0689(5) 0.8887(8) 0.1807(6) 0.089(3) Uiso 0.50 1 d PD C 1
B47B B 0.0758(7) 1.0002(13) 0.2320(9) 0.055(6) Uiso 0.50 1 d PD D 2
F48B F 0.1359(6) 1.0554(12) 0.2533(9) 0.112(5) Uiso 0.50 1 d PD D 2
F49B F 0.0281(5) 1.0849(9) 0.2076(7) 0.090(3) Uiso 0.50 1 d PD D 2
F50B F 0.0595(5) 0.9291(8) 0.2967(6) 0.084(2) Uiso 0.50 1 d PD D 2
F51B F 0.0769(5) 0.9262(9) 0.1620(6) 0.087(3) Uiso 0.50 1 d PD D 2
O52A O 0.6222(8) 0.5910(13) 0.6499(10) 0.109(4) Uiso 0.60 1 d P E 1
O52B O 0.6324(18) 0.574(3) 0.623(2) 0.136(12) Uiso 0.30 1 d P F 2
O52C O 0.585(4) 0.617(6) 0.617(5) 0.11(2) Uiso 0.10 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 N2 2.131(4) . ?
Fe1 N9 2.154(4) . ?
Fe1 N14 2.208(5) . ?
Fe1 N22 2.104(4) . ?
Fe1 N29 2.185(4) . ?
Fe1 N34 2.155(5) . ?
N2 C3 1.322(6) . ?
N2 C7 1.337(6) . ?
C3 C4 1.383(6) . ?
C3 N8 1.408(6) . ?
C4 H4 0.9400 . ?
C4 C5 1.386(7) . ?
C5 C6 1.410(8) . ?
C5 S18 1.749(5) . ?
C6 H6 0.9400 . ?
C6 C7 1.367(7) . ?
C7 N13 1.418(7) . ?
N8 N9 1.373(6) . ?
N8 C12 1.341(7) . ?
N9 C10 1.324(7) . ?
C10 H10 0.9400 . ?
C10 C11 1.401(9) . ?
C11 H11 0.9400 . ?
C11 C12 1.379(9) . ?
C12 H12 0.9400 . ?
N13 N14 1.366(6) . ?
N13 C17 1.349(7) . ?
N14 C15 1.326(7) . ?
C15 H15 0.9400 . ?
C15 C16 1.405(9) . ?
C16 H16 0.9400 . ?
C16 C17 1.362(9) . ?
C17 H17 0.9400 . ?
S18 C19 1.821(6) . ?
C19 H19 0.9900 . ?
C19 C20 1.488(10) . ?
C19 C21 1.520(8) . ?
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 1.336(6) . ?
N22 C27 1.316(7) . ?
C23 C24 1.381(7) . ?
C23 N28 1.407(7) . ?
C24 H24 0.9400 . ?
C24 C25 1.392(9) . ?
C25 C26 1.411(8) . ?
C25 S38B 1.754(6) . ?
C25 S38A 1.820(7) . ?
C25 S38C 1.802(9) . ?
C26 H26 0.9400 . ?
C26 C27 1.384(7) . ?
C27 N33 1.403(7) . ?
N28 N29 1.364(6) . ?
N28 C32 1.336(7) . ?
N29 C30 1.311(7) . ?
C30 H30 0.9400 . ?
C30 C31 1.401(9) . ?
C31 H31 0.9400 . ?
C31 C32 1.359(9) . ?
C32 H32 0.9400 . ?
N33 N34 1.364(6) . ?
N33 C37 1.378(8) . ?
N34 C35 1.341(7) . ?
C35 H35 0.9400 . ?
C35 C36 1.387(10) . ?
C36 H36 0.9400 . ?
C36 C37 1.365(10) . ?
C37 H37 0.9400 . ?
S38A C39A 1.784(14) . ?
C39A H39A 0.9900 . ?
C39A C40A 1.555(18) . ?
C39A C41A 1.521(16) . ?
C40A H40D 0.9700 . ?
C40A H40E 0.9700 . ?
C40A H40F 0.9700 . ?
C41A H41D 0.9700 . ?
C41A H41E 0.9700 . ?
C41A H41F 0.9700 . ?
S38B C39B 1.826(12) . ?
C39B H39B 0.9900 . ?
C39B C40B 1.508(18) . ?
C39B C41B 1.506(15) . ?
C40B H40A 0.9700 . ?
C40B H40B 0.9700 . ?
C40B H40C 0.9700 . ?
C41B H41A 0.9700 . ?
C41B H41B 0.9700 . ?
C41B H41C 0.9700 . ?
S38C C39C 1.821(18) . ?
C39C H39C 0.9900 . ?
C39C C40C 1.51(2) . ?
C39C C41C 1.508(19) . ?
C40C H40G 0.9700 . ?
C40C H40H 0.9700 . ?
C40C H40I 0.9700 . ?
C41C H41G 0.9700 . ?
C41C H41H 0.9700 . ?
C41C H41I 0.9700 . ?
B42 F43A 1.425(12) . ?
B42 F44A 1.403(11) . ?
B42 F45A 1.315(11) . ?
B42 F46A 1.407(12) . ?
B42 F43B 1.411(15) . ?
B42 F44B 1.376(15) . ?
B42 F45B 1.362(13) . ?
B42 F46B 1.398(15) . ?
B42 F43C 1.339(13) . ?
B42 F44C 1.330(14) . ?
B42 F45C 1.480(14) . ?
B42 F46C 1.437(13) . ?
B47A F48A 1.441(15) . ?
B47A F49A 1.405(14) . ?
B47A F50A 1.388(14) . ?
B47A F51A 1.340(15) . ?
B47B F48B 1.356(14) . ?
B47B F49B 1.379(14) . ?
B47B F50B 1.412(14) . ?
B47B F51B 1.409(14) . ?

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 N9 73.62(15) . . ?
N2 Fe1 N14 73.25(16) . . ?
N2 Fe1 N29 114.73(16) . . ?
N2 Fe1 N34 98.00(16) . . ?
N9 Fe1 N14 146.86(16) . . ?
N9 Fe1 N29 96.13(17) . . ?
N9 Fe1 N34 91.67(19) . . ?
N22 Fe1 N2 168.12(16) . . ?
N22 Fe1 N9 114.33(16) . . ?
N22 Fe1 N14 98.43(16) . . ?
N22 Fe1 N29 74.20(16) . . ?
N22 Fe1 N34 73.60(16) . . ?
N29 Fe1 N14 97.46(16) . . ?
N34 Fe1 N14 93.00(18) . . ?
N34 Fe1 N29 147.25(16) . . ?
C3 N2 Fe1 120.1(3) . . ?
C3 N2 C7 118.4(4) . . ?
C7 N2 Fe1 120.8(3) . . ?
N2 C3 C4 123.5(5) . . ?
N2 C3 N8 113.3(4) . . ?
C4 C3 N8 123.2(4) . . ?
C3 C4 H4 121.2 . . ?
C3 C4 C5 117.5(5) . . ?
C5 C4 H4 121.2 . . ?
C4 C5 C6 119.8(5) . . ?
C4 C5 S18 125.3(4) . . ?
C6 C5 S18 114.9(4) . . ?
C5 C6 H6 121.5 . . ?
C7 C6 C5 117.1(5) . . ?
C7 C6 H6 121.5 . . ?
N2 C7 C6 123.7(5) . . ?
N2 C7 N13 112.8(4) . . ?
C6 C7 N13 123.4(5) . . ?
N9 N8 C3 117.3(4) . . ?
C12 N8 C3 131.3(4) . . ?
C12 N8 N9 111.3(4) . . ?
N8 N9 Fe1 115.0(3) . . ?
C10 N9 Fe1 139.8(4) . . ?
C10 N9 N8 105.1(4) . . ?
N9 C10 H10 124.3 . . ?
N9 C10 C11 111.4(5) . . ?
C11 C10 H10 124.3 . . ?
C10 C11 H11 127.6 . . ?
C12 C11 C10 104.9(5) . . ?
C12 C11 H11 127.6 . . ?
N8 C12 C11 107.4(5) . . ?
N8 C12 H12 126.3 . . ?
C11 C12 H12 126.3 . . ?
N14 N13 C7 118.4(4) . . ?
C17 N13 C7 129.5(5) . . ?
C17 N13 N14 112.0(5) . . ?
N13 N14 Fe1 114.1(3) . . ?
C15 N14 Fe1 141.1(4) . . ?
C15 N14 N13 104.8(5) . . ?
N14 C15 H15 124.7 . . ?
N14 C15 C16 110.6(5) . . ?
C16 C15 H15 124.7 . . ?
C15 C16 H16 127.0 . . ?
C17 C16 C15 106.1(5) . . ?
C17 C16 H16 127.0 . . ?
N13 C17 C16 106.4(5) . . ?
N13 C17 H17 126.8 . . ?
C16 C17 H17 126.8 . . ?
C5 S18 C19 105.2(3) . . ?
S18 C19 H19 108.9 . . ?
C20 C19 S18 111.6(5) . . ?
C20 C19 H19 108.9 . . ?
C20 C19 C21 112.4(6) . . ?
C21 C19 S18 106.0(5) . . ?
C21 C19 H19 108.9 . . ?
C19 C20 H20A 109.5 . . ?
C19 C20 H20B 109.5 . . ?
C19 C20 H20C 109.5 . . ?
H20A C20 H20B 109.5 . . ?
H20A C20 H20C 109.5 . . ?
H20B C20 H20C 109.5 . . ?
C19 C21 H21A 109.5 . . ?
C19 C21 H21B 109.5 . . ?
C19 C21 H21C 109.5 . . ?
H21A C21 H21B 109.5 . . ?
H21A C21 H21C 109.5 . . ?
H21B C21 H21C 109.5 . . ?
C23 N22 Fe1 120.1(3) . . ?
C27 N22 Fe1 121.1(3) . . ?
C27 N22 C23 118.8(4) . . ?
N22 C23 C24 123.3(5) . . ?
N22 C23 N28 113.9(4) . . ?
C24 C23 N28 122.8(5) . . ?
C23 C24 H24 121.4 . . ?
C23 C24 C25 117.1(5) . . ?
C25 C24 H24 121.4 . . ?
C24 C25 C26 120.3(5) . . ?
C24 C25 S38B 112.8(5) . . ?
C24 C25 S38A 114.0(5) . . ?
C24 C25 S38C 116.7(5) . . ?
C26 C25 S38B 126.8(5) . . ?
C26 C25 S38A 123.4(5) . . ?
C26 C25 S38C 115.1(6) . . ?
C25 C26 H26 121.8 . . ?
C27 C26 C25 116.3(5) . . ?
C27 C26 H26 121.8 . . ?
N22 C27 C26 124.0(5) . . ?
N22 C27 N33 112.5(4) . . ?
C26 C27 N33 123.5(5) . . ?
N29 N28 C23 118.0(4) . . ?
C32 N28 C23 130.9(5) . . ?
C32 N28 N29 111.1(5) . . ?
N28 N29 Fe1 113.8(3) . . ?
C30 N29 Fe1 141.2(4) . . ?
C30 N29 N28 105.0(4) . . ?
N29 C30 H30 124.2 . . ?
N29 C30 C31 111.5(5) . . ?
C31 C30 H30 124.2 . . ?
C30 C31 H31 127.7 . . ?
C32 C31 C30 104.6(5) . . ?
C32 C31 H31 127.7 . . ?
N28 C32 C31 107.8(5) . . ?
N28 C32 H32 126.1 . . ?
C31 C32 H32 126.1 . . ?
N34 N33 C27 118.3(4) . . ?
N34 N33 C37 111.4(5) . . ?
C37 N33 C27 130.2(5) . . ?
N33 N34 Fe1 114.2(3) . . ?
C35 N34 Fe1 141.0(4) . . ?
C35 N34 N33 104.9(5) . . ?
N34 C35 H35 124.4 . . ?
N34 C35 C36 111.1(6) . . ?
C36 C35 H35 124.4 . . ?
C35 C36 H36 126.6 . . ?
C37 C36 C35 106.7(6) . . ?
C37 C36 H36 126.6 . . ?
N33 C37 H37 127.0 . . ?
C36 C37 N33 105.9(6) . . ?
C36 C37 H37 127.0 . . ?
C39A S38A C25 107.0(6) . . ?
S38A C39A H39A 111.9 . . ?
C40A C39A S38A 113.3(17) . . ?
C40A C39A H39A 111.9 . . ?
C41A C39A S38A 97.9(13) . . ?
C41A C39A H39A 111.9 . . ?
C41A C39A C40A 109.0(14) . . ?
C39A C40A H40D 109.5 . . ?
C39A C40A H40E 109.5 . . ?
C39A C40A H40F 109.5 . . ?
H40D C40A H40E 109.5 . . ?
H40D C40A H40F 109.5 . . ?
H40E C40A H40F 109.5 . . ?
C39A C41A H41D 109.5 . . ?
C39A C41A H41E 109.5 . . ?
C39A C41A H41F 109.5 . . ?
H41D C41A H41E 109.5 . . ?
H41D C41A H41F 109.5 . . ?
H41E C41A H41F 109.5 . . ?
C25 S38B C39B 104.9(6) . . ?
S38B C39B H39B 109.5 . . ?
C40B C39B S38B 98.3(16) . . ?
C40B C39B H39B 109.5 . . ?
C41B C39B S38B 115.8(14) . . ?
C41B C39B H39B 109.5 . . ?
C41B C39B C40B 113.8(14) . . ?
C39B C40B H40A 109.5 . . ?
C39B C40B H40B 109.5 . . ?
C39B C40B H40C 109.5 . . ?
H40A C40B H40B 109.5 . . ?
H40A C40B H40C 109.5 . . ?
H40B C40B H40C 109.5 . . ?
C39B C41B H41A 109.5 . . ?
C39B C41B H41B 109.5 . . ?
C39B C41B H41C 109.5 . . ?
H41A C41B H41B 109.5 . . ?
H41A C41B H41C 109.5 . . ?
H41B C41B H41C 109.5 . . ?
C25 S38C C39C 102.5(10) . . ?
S38C C39C H39C 110.8 . . ?
C40C C39C S38C 109(4) . . ?
C40C C39C H39C 110.8 . . ?
C41C C39C S38C 104(3) . . ?
C41C C39C H39C 110.8 . . ?
C41C C39C C40C 112(2) . . ?
C39C C40C H40G 109.5 . . ?
C39C C40C H40H 109.5 . . ?
C39C C40C H40I 109.5 . . ?
H40G C40C H40H 109.5 . . ?
H40G C40C H40I 109.5 . . ?
H40H C40C H40I 109.5 . . ?
C39C C41C H41G 109.5 . . ?
C39C C41C H41H 109.5 . . ?
C39C C41C H41I 109.5 . . ?
H41G C41C H41H 109.5 . . ?
H41G C41C H41I 109.5 . . ?
H41H C41C H41I 109.5 . . ?
F44A B42 F43A 106.2(9) . . ?
F44A B42 F46A 104.1(9) . . ?
F45A B42 F43A 110.1(9) . . ?
F45A B42 F44A 115.7(10) . . ?
F45A B42 F46A 111.5(9) . . ?
F46A B42 F43A 108.8(10) . . ?
F44B B42 F43B 111.8(13) . . ?
F44B B42 F46B 109.0(13) . . ?
F45B B42 F43B 105.3(12) . . ?
F45B B42 F44B 112.0(12) . . ?
F45B B42 F46B 108.9(13) . . ?
F46B B42 F43B 109.6(14) . . ?
F43C B42 F45C 106.3(11) . . ?
F43C B42 F46C 107.7(10) . . ?
F44C B42 F43C 118.0(13) . . ?
F44C B42 F45C 110.6(13) . . ?
F44C B42 F46C 112.1(13) . . ?
F46C B42 F45C 100.5(10) . . ?
F49A B47A F48A 111.6(12) . . ?
F50A B47A F48A 101.7(10) . . ?
F50A B47A F49A 109.8(11) . . ?
F51A B47A F48A 108.1(11) . . ?
F51A B47A F49A 108.9(11) . . ?
F51A B47A F50A 116.6(13) . . ?
F48B B47B F49B 105.4(12) . . ?
F48B B47B F50B 116.1(12) . . ?
F48B B47B F51B 108.5(11) . . ?
F49B B47B F50B 111.3(11) . . ?
F49B B47B F51B 110.7(11) . . ?
F51B B47B F50B 104.8(11) . . ?

####################################################################### 
# 
# 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_h2o180
_database_code_depnum_ccdc_archive 'CCDC 1976623'
_audit_update_record             
;
2020-01-09 deposited with the CCDC.	2020-05-26 downloaded from the CCDC.
;
_audit_creation_date             2018-06-23
_audit_creation_method           
;
  Olex2 1.2
  (compiled Apr 23 2013 17:54:37, GUI svn.r4466)
;
_chemical_name_common            ?
_chemical_name_systematic        
;
Bis[4-(isopropylsulfanyl)-2,6-di(pyrazol-1-yl)pyridine]iron(II)
ditetrafluoroborate hydrate
;
_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         818.23
_chemical_melting_point          ?
loop_
_atom_type_symbol
_atom_type_description
_atom_type_scat_dispersion_real
_atom_type_scat_dispersion_imag
_atom_type_scat_source
B B 0.0090 0.0039 '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'
F F 0.0727 0.0534 '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'

_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_id
_space_group_symop_operation_xyz
1 'x, y, z'
2 '-x, y+1/2, -z+1/2'
3 '-x, -y, -z'
4 'x, -y-1/2, z-1/2'

_cell_length_a                   19.8157(5)
_cell_length_b                   11.9288(4)
_cell_length_c                   15.5408(6)
_cell_angle_alpha                90.00
_cell_angle_beta                 102.457(3)
_cell_angle_gamma                90.00
_cell_volume                     3587.0(2)
_cell_formula_units_Z            4
_cell_measurement_reflns_used    4100
_cell_measurement_temperature    180(2)
_cell_measurement_theta_min      4.35
_cell_measurement_theta_max      73.03
_exptl_absorpt_coefficient_mu    5.194
_exptl_absorpt_correction_T_min  0.358
_exptl_absorpt_correction_T_max  1.000
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   
;
CrysAlisPro 1.171.39.46 (Rigaku Oxford Diffraction, 2018)
Empirical absorption correction using spherical harmonics,
 implemented in SCALE3 ABSPACK scaling algorithm.
;

_exptl_crystal_colour            brown
_exptl_crystal_density_diffrn    1.515
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       plate
_exptl_crystal_F_000             1672
_exptl_crystal_size_max          0.35
_exptl_crystal_size_mid          0.30
_exptl_crystal_size_min          0.10
_exptl_special_details           
;
 ? 
;
_diffrn_reflns_av_R_equivalents  0.0327
_diffrn_reflns_av_unetI/netI     0.0487
_diffrn_reflns_limit_h_max       23
_diffrn_reflns_limit_h_min       -23
_diffrn_reflns_limit_k_max       14
_diffrn_reflns_limit_k_min       -10
_diffrn_reflns_limit_l_max       18
_diffrn_reflns_limit_l_min       -19
_diffrn_reflns_number            13498
_diffrn_reflns_theta_full        72.00
_diffrn_reflns_theta_max         73.60
_diffrn_reflns_theta_min         4.35
_diffrn_ambient_temperature      180(2)
_diffrn_detector_area_resol_mean 5.3095
_diffrn_measured_fraction_theta_full 0.985
_diffrn_measured_fraction_theta_max 0.970
_diffrn_measurement_device_type  'SuperNova, Dual, Cu at zero, Atlas'
_diffrn_measurement_method       'ω scans'
_diffrn_radiation_monochromator  mirror
_diffrn_radiation_type           CuK\a
_diffrn_radiation_wavelength     1.54184
_diffrn_radiation_source         'SuperNova (Cu) X-ray Source'
_diffrn_standards_number         0
_diffrn_standards_interval_count 0
_diffrn_standards_interval_time  0
_diffrn_standards_decay_%        0
_reflns_number_gt                5440
_reflns_number_total             7028
_reflns_threshold_expression     >2sigma(I)
_computing_data_collection       'CrysAlisPro, Agilent Technologies'
_computing_cell_refinement       'CrysAlisPro, Agilent Technologies'
_computing_data_reduction        'CrysAlisPro, Agilent Technologies'
_computing_molecular_graphics    'XSEED (Barbour, 2001)'
_computing_publication_material  
;
O. V. Dolomanov, L. J. Bourhis, R. J. Gildea, J. A. K. Howard and H. Puschmann,
OLEX2: a complete structure solution, refinement and analysis program.
J. Appl. Cryst. (2009). 42, 339-341.
;
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_refine_diff_density_max         0.859
_refine_diff_density_min         -0.719
_refine_diff_density_rms         0.080
_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     463
_refine_ls_number_reflns         7028
_refine_ls_number_restraints     40
_refine_ls_R_factor_all          0.0891
_refine_ls_R_factor_gt           0.0696
_refine_ls_restrained_S_all      1.070
_refine_ls_shift/su_max          0.000
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details     
'calc w=1/[σ²(Fo²)+(0.0971P)²+4.7856P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1827
_refine_ls_wR_factor_ref         0.1967
_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. 

 Both the BF₄⁻ ions is disordered over two equally occupied sites, which
 were treated with the refined restraints B---F = 1.39(2) and F...F = 
 2.27(2) Å. The water molecule was also modelled as disordered, over two 
 sites with occupancies of 0.67 and 0.33. All fully occupied non-H 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 Fouier map and could not be included in the model, 
 but are accounted for in the molecular weight and density calculations.

;
_olex2_refinement_description    
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups
 At 1.5 times of:
  All C(H,H,H) groups
2. Restrained distances
 B42A-F43A = B42A-F44A = B42A-F45A = B42A-F46A
 1.39396 with sigma of 0.02
 B42B-F43B = B42B-F44B = B42B-F45B = B42B-F46B
 1.39396 with sigma of 0.02
 F43A-F44A = F43A-F45A = F43A-F46A = F44A-F45A = F44A-F46A = F45A-F46A
 2.276337 with sigma of 0.02
 F43B-F44B = F43B-F45B = F43B-F46B = F44B-F45B = F44B-F46B = F45B-F46B
 2.276337 with sigma of 0.02
 B47A-F48A = B47A-F49A = B47A-F50A = B47A-F51A
 1.39396 with sigma of 0.02
 B47B-F48B = B47B-F49B = B47B-F50B = B47B-F51B
 1.39396 with sigma of 0.02
 F48A-F49A = F48A-F50A = F48A-F51A = F49A-F50A = F49A-F51A = F50A-F51A
 2.276337 with sigma of 0.02
 F48B-F49B = F48B-F50B = F48B-F51B = F49B-F50B = F49B-F51B = F50B-F51B
 2.276337 with sigma of 0.02
3. Others
 1(DFIX)=1(DFIX)=1(DFIX)=1(DFIX)=FVAR(1)
 1(DFIX)=1(DFIX)=1(DFIX)=1(DFIX)=1.633*FVAR(2)
 Fixed Sof: B42A(0.5) F43A(0.5) F44A(0.5) F45A(0.5) F46A(0.5) B42B(0.5)
 F43B(0.5) F44B(0.5) F45B(0.5) F46B(0.5) B47A(0.5) F48A(0.5) F49A(0.5)
 F50A(0.5) F51A(0.5) B47B(0.5) F48B(0.5) F49B(0.5) F50B(0.5) F51B(0.5)
 O52A(0.67) O52B(0.33)
4.a Ternary CH refined with riding coordinates:
 C19(H19), C39(H39)
4.b Aromatic/amide H refined with riding coordinates:
 C4(H4), C6(H6), C10(H10), C11(H11), C12(H12), C15(H15), C16(H16), C17(H17),
 C24(H24), C26(H26), C30(H30), C31(H31), C32(H32), C35(H35), C36(H36), C37(H37)
4.c Idealised Me refined as rotating group:
 C20(H20A,H20B,H20C), C21(H21A,H21B,H21C), C40(H40A,H40B,H40C), C41(H41A,H41B,
 H41C)
;
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_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_symmetry_multiplicity
_atom_site_calc_flag
_atom_site_refinement_flags
_atom_site_disorder_assembly
_atom_site_disorder_group
Fe1 Fe 0.23205(3) 0.61339(6) 0.08106(4) 0.03390(19) Uani 1 1 d . . .
N2 N 0.13435(18) 0.6332(3) 0.0477(2) 0.0374(8) Uani 1 1 d . . .
C3 C 0.1069(2) 0.7103(4) -0.0111(3) 0.0346(8) Uani 1 1 d . . .
C4 C 0.0374(2) 0.7380(4) -0.0302(3) 0.0390(9) Uani 1 1 d . . .
H4 H 0.0191 0.7930 -0.0732 0.047 Uiso 1 1 calc R . .
C5 C -0.0044(2) 0.6816(4) 0.0166(3) 0.0411(10) Uani 1 1 d . . .
C6 C 0.0243(2) 0.6003(4) 0.0802(3) 0.0442(10) Uani 1 1 d . . .
H6 H -0.0035 0.5610 0.1129 0.053 Uiso 1 1 calc R . .
C7 C 0.0933(2) 0.5804(4) 0.0928(3) 0.0391(9) Uani 1 1 d . . .
N8 N 0.15852(18) 0.7616(3) -0.0468(2) 0.0382(8) Uani 1 1 d . . .
N9 N 0.22605(17) 0.7329(3) -0.0088(2) 0.0370(8) Uani 1 1 d . . .
C10 C 0.2647(2) 0.8012(4) -0.0445(3) 0.0447(10) Uani 1 1 d . . .
H10 H 0.3138 0.8016 -0.0309 0.054 Uiso 1 1 calc R . .
C11 C 0.2235(3) 0.8730(4) -0.1052(4) 0.0521(12) Uani 1 1 d . . .
H11 H 0.2391 0.9292 -0.1396 0.063 Uiso 1 1 calc R . .
C12 C 0.1569(3) 0.8469(4) -0.1055(3) 0.0453(10) Uani 1 1 d . . .
H12 H 0.1169 0.8814 -0.1399 0.054 Uiso 1 1 calc R . .
N13 N 0.13167(18) 0.5060(3) 0.1547(3) 0.0407(8) Uani 1 1 d . . .
N14 N 0.20199(18) 0.5027(3) 0.1604(3) 0.0390(8) Uani 1 1 d . . .
C15 C 0.2254(3) 0.4257(4) 0.2213(3) 0.0480(11) Uani 1 1 d . . .
H15 H 0.2726 0.4056 0.2405 0.058 Uiso 1 1 calc R . .
C16 C 0.1710(3) 0.3781(5) 0.2533(4) 0.0524(12) Uani 1 1 d . . .
H16 H 0.1743 0.3211 0.2967 0.063 Uiso 1 1 calc R . .
C17 C 0.1123(3) 0.4303(4) 0.2096(3) 0.0493(11) Uani 1 1 d . . .
H17 H 0.0665 0.4162 0.2163 0.059 Uiso 1 1 calc R . .
S18 S -0.09372(5) 0.70036(11) 0.00321(9) 0.0497(3) Uani 1 1 d . . .
C19 C -0.1128(2) 0.8342(4) -0.0527(4) 0.0474(11) Uani 1 1 d . . .
H19 H -0.0928 0.8353 -0.1065 0.057 Uiso 1 1 calc R . .
C20 C -0.0827(3) 0.9295(5) 0.0076(4) 0.0607(14) Uani 1 1 d . . .
H20A H -0.0946 1.0010 -0.0230 0.091 Uiso 1 1 calc R . .
H20B H -0.0323 0.9218 0.0239 0.091 Uiso 1 1 calc R . .
H20C H -0.1017 0.9275 0.0608 0.091 Uiso 1 1 calc R . .
C21 C -0.1910(3) 0.8413(6) -0.0798(5) 0.0659(16) Uani 1 1 d . . .
H21A H -0.2108 0.8375 -0.0272 0.099 Uiso 1 1 calc R . .
H21B H -0.2086 0.7786 -0.1191 0.099 Uiso 1 1 calc R . .
H21C H -0.2043 0.9122 -0.1106 0.099 Uiso 1 1 calc R . .
N22 N 0.32883(17) 0.5935(3) 0.1235(2) 0.0358(8) Uani 1 1 d . . .
C23 C 0.3637(2) 0.5171(4) 0.0872(3) 0.0378(9) Uani 1 1 d . . .
C24 C 0.4320(2) 0.4926(4) 0.1199(3) 0.0419(10) Uani 1 1 d . . .
H24 H 0.4553 0.4374 0.0931 0.050 Uiso 1 1 calc R . .
C25 C 0.4660(2) 0.5519(4) 0.1940(3) 0.0447(10) Uani 1 1 d . . .
C26 C 0.4308(2) 0.6343(4) 0.2318(3) 0.0424(10) Uani 1 1 d . . .
H26 H 0.4535 0.6770 0.2812 0.051 Uiso 1 1 calc R . .
C27 C 0.3624(2) 0.6504(4) 0.1942(3) 0.0359(9) Uani 1 1 d . . .
N28 N 0.31945(18) 0.4650(3) 0.0152(3) 0.0394(8) Uani 1 1 d . . .
N29 N 0.25094(18) 0.4969(3) -0.0020(2) 0.0384(8) Uani 1 1 d . . .
C30 C 0.2214(2) 0.4388(4) -0.0730(3) 0.0423(10) Uani 1 1 d . . .
H30 H 0.1737 0.4426 -0.1006 0.051 Uiso 1 1 calc R . .
C31 C 0.2699(3) 0.3710(4) -0.1016(3) 0.0493(11) Uani 1 1 d . . .
H31 H 0.2616 0.3222 -0.1510 0.059 Uiso 1 1 calc R . .
C32 C 0.3315(3) 0.3891(4) -0.0444(4) 0.0486(11) Uani 1 1 d . . .
H32 H 0.3745 0.3550 -0.0460 0.058 Uiso 1 1 calc R . .
N33 N 0.31706(18) 0.7271(3) 0.2218(2) 0.0379(8) Uani 1 1 d . . .
N34 N 0.24952(18) 0.7267(3) 0.1756(2) 0.0371(8) Uani 1 1 d . . .
C35 C 0.2188(2) 0.8089(4) 0.2091(3) 0.0441(10) Uani 1 1 d . . .
H35 H 0.1715 0.8286 0.1903 0.053 Uiso 1 1 calc R . .
C36 C 0.2662(3) 0.8632(4) 0.2766(4) 0.0517(12) Uani 1 1 d . . .
H36 H 0.2572 0.9254 0.3106 0.062 Uiso 1 1 calc R . .
C37 C 0.3276(3) 0.8090(4) 0.2835(3) 0.0455(10) Uani 1 1 d . . .
H37 H 0.3697 0.8254 0.3238 0.055 Uiso 1 1 calc R . .
S38 S 0.55154(6) 0.51158(13) 0.23460(10) 0.0614(4) Uani 1 1 d . . .
C39 C 0.5819(2) 0.5912(5) 0.3352(4) 0.0532(13) Uani 1 1 d . . .
H39 H 0.5432 0.6003 0.3666 0.064 Uiso 1 1 calc R . .
C40 C 0.6065(4) 0.7057(6) 0.3134(5) 0.0789(19) Uani 1 1 d . . .
H40A H 0.6159 0.7522 0.3667 0.118 Uiso 1 1 calc R . .
H40B H 0.5707 0.7415 0.2684 0.118 Uiso 1 1 calc R . .
H40C H 0.6489 0.6977 0.2911 0.118 Uiso 1 1 calc R . .
C41 C 0.6391(3) 0.5212(6) 0.3921(4) 0.0703(17) Uani 1 1 d . . .
H41A H 0.6767 0.5107 0.3610 0.106 Uiso 1 1 calc R . .
H41B H 0.6206 0.4480 0.4038 0.106 Uiso 1 1 calc R . .
H41C H 0.6568 0.5601 0.4480 0.106 Uiso 1 1 calc R . .
B42A B 0.4730(7) 0.7245(12) 0.4984(9) 0.044(6) Uiso 0.50 1 d PD A 1
F43A F 0.5315(4) 0.7388(8) 0.5638(6) 0.083(2) Uiso 0.50 1 d PD A 1
F44A F 0.4827(4) 0.7838(7) 0.4221(5) 0.0747(19) Uiso 0.50 1 d PD A 1
F45A F 0.4162(4) 0.7728(8) 0.5203(6) 0.087(2) Uiso 0.50 1 d PD A 1
F46A F 0.4607(4) 0.6143(6) 0.4699(6) 0.079(2) Uiso 0.50 1 d PD A 1
B42B B 0.4668(7) 0.7375(12) 0.4922(9) 0.049(6) Uiso 0.50 1 d PD B 2
F43B F 0.5375(4) 0.7224(9) 0.5267(7) 0.094(3) Uiso 0.50 1 d PD B 2
F44B F 0.4527(5) 0.8378(8) 0.4501(6) 0.101(3) Uiso 0.50 1 d PD B 2
F45B F 0.4309(3) 0.7349(6) 0.5601(5) 0.0634(16) Uiso 0.50 1 d PD B 2
F46B F 0.4390(4) 0.6482(7) 0.4363(5) 0.075(2) Uiso 0.50 1 d PD B 2
B47A B 0.0629(6) 0.9749(11) 0.2285(7) 0.039(3) Uiso 0.50 1 d PD C 1
F48A F 0.1277(3) 1.0269(6) 0.2330(4) 0.0496(14) Uiso 0.50 1 d PD C 1
F49A F 0.0064(4) 1.0466(7) 0.1961(6) 0.051(2) Uiso 0.50 1 d PD C 1
F50A F 0.0667(4) 0.9530(7) 0.3190(5) 0.050(2) Uiso 0.50 1 d PD C 1
F51A F 0.0585(3) 0.8836(6) 0.1756(4) 0.0552(15) Uiso 0.50 1 d PD C 1
B47B B 0.0677(6) 1.0018(11) 0.2337(8) 0.049(4) Uiso 0.50 1 d PD D 2
F48B F 0.1231(4) 1.0700(8) 0.2495(6) 0.079(2) Uiso 0.50 1 d PD D 2
F49B F 0.0094(5) 1.0676(9) 0.2070(7) 0.070(4) Uiso 0.50 1 d PD D 2
F50B F 0.0552(5) 0.9322(7) 0.3052(5) 0.062(3) Uiso 0.50 1 d PD D 2
F51B F 0.0730(4) 0.9265(7) 0.1659(5) 0.074(2) Uiso 0.50 1 d PD D 2
O52A O 0.6294(5) 0.5557(8) 0.6269(6) 0.078(3) Uiso 0.67 1 d P E 1
O52B O 0.6185(10) 0.5761(16) 0.6479(12) 0.078(5) Uiso 0.33 1 d P F 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 N2 1.908(4) . ?
Fe1 N9 1.982(4) . ?
Fe1 N14 1.983(4) . ?
Fe1 N22 1.903(3) . ?
Fe1 N29 1.987(4) . ?
Fe1 N34 1.971(4) . ?
N2 C3 1.328(6) . ?
N2 C7 1.340(6) . ?
C3 C4 1.385(6) . ?
C3 N8 1.405(5) . ?
C4 H4 0.9500 . ?
C4 C5 1.388(6) . ?
C5 C6 1.413(7) . ?
C5 S18 1.752(4) . ?
C6 H6 0.9500 . ?
C6 C7 1.359(6) . ?
C7 N13 1.407(6) . ?
N8 N9 1.384(5) . ?
N8 C12 1.362(6) . ?
N9 C10 1.320(6) . ?
C10 H10 0.9500 . ?
C10 C11 1.400(7) . ?
C11 H11 0.9500 . ?
C11 C12 1.354(7) . ?
C12 H12 0.9500 . ?
N13 N14 1.378(5) . ?
N13 C17 1.352(6) . ?
N14 C15 1.329(6) . ?
C15 H15 0.9500 . ?
C15 C16 1.400(7) . ?
C16 H16 0.9500 . ?
C16 C17 1.365(7) . ?
C17 H17 0.9500 . ?
S18 C19 1.818(5) . ?
C19 H19 1.0000 . ?
C19 C20 1.512(8) . ?
C19 C21 1.519(7) . ?
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 C23 1.339(6) . ?
N22 C27 1.341(6) . ?
C23 C24 1.371(6) . ?
C23 N28 1.408(6) . ?
C24 H24 0.9500 . ?
C24 C25 1.395(7) . ?
C25 C26 1.405(7) . ?
C25 S38 1.743(4) . ?
C26 H26 0.9500 . ?
C26 C27 1.370(6) . ?
C27 N33 1.412(5) . ?
N28 N29 1.379(5) . ?
N28 C32 1.352(6) . ?
N29 C30 1.327(6) . ?
C30 H30 0.9500 . ?
C30 C31 1.400(7) . ?
C31 H31 0.9500 . ?
C31 C32 1.362(7) . ?
C32 H32 0.9500 . ?
N33 N34 1.376(5) . ?
N33 C37 1.352(6) . ?
N34 C35 1.319(6) . ?
C35 H35 0.9500 . ?
C35 C36 1.406(7) . ?
C36 H36 0.9500 . ?
C36 C37 1.362(7) . ?
C37 H37 0.9500 . ?
S38 C39 1.818(5) . ?
C39 H39 1.0000 . ?
C39 C40 1.514(9) . ?
C39 C41 1.527(8) . ?
C40 H40A 0.9800 . ?
C40 H40B 0.9800 . ?
C40 H40C 0.9800 . ?
C41 H41A 0.9800 . ?
C41 H41B 0.9800 . ?
C41 H41C 0.9800 . ?
B42A F43A 1.378(13) . ?
B42A F44A 1.429(14) . ?
B42A F45A 1.372(14) . ?
B42A F46A 1.392(13) . ?
B42B F43B 1.399(14) . ?
B42B F44B 1.364(15) . ?
B42B F45B 1.395(14) . ?
B42B F46B 1.409(14) . ?
B47A F48A 1.414(12) . ?
B47A F49A 1.411(12) . ?
B47A F50A 1.416(11) . ?
B47A F51A 1.357(13) . ?
B47B F48B 1.346(13) . ?
B47B F49B 1.384(13) . ?
B47B F50B 1.449(13) . ?
B47B F51B 1.406(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
N2 Fe1 N9 79.42(15) . . ?
N2 Fe1 N14 80.10(15) . . ?
N2 Fe1 N29 103.46(15) . . ?
N2 Fe1 N34 97.01(15) . . ?
N9 Fe1 N14 159.49(14) . . ?
N9 Fe1 N29 92.08(15) . . ?
N14 Fe1 N29 93.55(15) . . ?
N22 Fe1 N2 175.60(16) . . ?
N22 Fe1 N9 103.68(15) . . ?
N22 Fe1 N14 96.73(15) . . ?
N22 Fe1 N29 79.69(15) . . ?
N22 Fe1 N34 79.94(15) . . ?
N34 Fe1 N9 90.37(15) . . ?
N34 Fe1 N14 91.22(16) . . ?
N34 Fe1 N29 159.48(15) . . ?
C3 N2 Fe1 120.9(3) . . ?
C3 N2 C7 118.7(4) . . ?
C7 N2 Fe1 119.7(3) . . ?
N2 C3 C4 123.6(4) . . ?
N2 C3 N8 110.4(3) . . ?
C4 C3 N8 125.9(4) . . ?
C3 C4 H4 121.6 . . ?
C3 C4 C5 116.7(4) . . ?
C5 C4 H4 121.6 . . ?
C4 C5 C6 120.3(4) . . ?
C4 C5 S18 125.2(4) . . ?
C6 C5 S18 114.5(3) . . ?
C5 C6 H6 121.3 . . ?
C7 C6 C5 117.4(4) . . ?
C7 C6 H6 121.3 . . ?
N2 C7 C6 123.3(4) . . ?
N2 C7 N13 110.8(4) . . ?
C6 C7 N13 126.0(4) . . ?
N9 N8 C3 116.3(3) . . ?
C12 N8 C3 132.5(4) . . ?
C12 N8 N9 110.5(4) . . ?
N8 N9 Fe1 112.6(3) . . ?
C10 N9 Fe1 142.0(3) . . ?
C10 N9 N8 105.3(4) . . ?
N9 C10 H10 124.7 . . ?
N9 C10 C11 110.7(4) . . ?
C11 C10 H10 124.7 . . ?
C10 C11 H11 126.6 . . ?
C12 C11 C10 106.8(4) . . ?
C12 C11 H11 126.6 . . ?
N8 C12 H12 126.6 . . ?
C11 C12 N8 106.7(4) . . ?
C11 C12 H12 126.6 . . ?
N14 N13 C7 116.9(4) . . ?
C17 N13 C7 131.9(4) . . ?
C17 N13 N14 111.2(4) . . ?
N13 N14 Fe1 112.1(3) . . ?
C15 N14 Fe1 142.9(3) . . ?
C15 N14 N13 104.9(4) . . ?
N14 C15 H15 124.5 . . ?
N14 C15 C16 110.9(4) . . ?
C16 C15 H15 124.5 . . ?
C15 C16 H16 127.0 . . ?
C17 C16 C15 106.1(4) . . ?
C17 C16 H16 127.0 . . ?
N13 C17 C16 106.9(4) . . ?
N13 C17 H17 126.5 . . ?
C16 C17 H17 126.5 . . ?
C5 S18 C19 105.7(2) . . ?
S18 C19 H19 109.5 . . ?
C20 C19 S18 110.5(4) . . ?
C20 C19 H19 109.5 . . ?
C20 C19 C21 111.9(5) . . ?
C21 C19 S18 106.0(4) . . ?
C21 C19 H19 109.5 . . ?
C19 C20 H20A 109.5 . . ?
C19 C20 H20B 109.5 . . ?
C19 C20 H20C 109.5 . . ?
H20A C20 H20B 109.5 . . ?
H20A C20 H20C 109.5 . . ?
H20B C20 H20C 109.5 . . ?
C19 C21 H21A 109.5 . . ?
C19 C21 H21B 109.5 . . ?
C19 C21 H21C 109.5 . . ?
H21A C21 H21B 109.5 . . ?
H21A C21 H21C 109.5 . . ?
H21B C21 H21C 109.5 . . ?
C23 N22 Fe1 120.8(3) . . ?
C23 N22 C27 118.7(4) . . ?
C27 N22 Fe1 120.4(3) . . ?
N22 C23 C24 123.1(4) . . ?
N22 C23 N28 110.3(4) . . ?
C24 C23 N28 126.6(4) . . ?
C23 C24 H24 121.3 . . ?
C23 C24 C25 117.5(4) . . ?
C25 C24 H24 121.3 . . ?
C24 C25 C26 120.3(4) . . ?
C24 C25 S38 114.7(4) . . ?
C26 C25 S38 124.9(4) . . ?
C25 C26 H26 121.5 . . ?
C27 C26 C25 117.1(4) . . ?
C27 C26 H26 121.5 . . ?
N22 C27 C26 123.3(4) . . ?
N22 C27 N33 110.0(4) . . ?
C26 C27 N33 126.7(4) . . ?
N29 N28 C23 116.8(3) . . ?
C32 N28 C23 131.9(4) . . ?
C32 N28 N29 111.3(4) . . ?
N28 N29 Fe1 112.5(3) . . ?
C30 N29 Fe1 142.5(3) . . ?
C30 N29 N28 104.9(4) . . ?
N29 C30 H30 124.6 . . ?
N29 C30 C31 110.7(4) . . ?
C31 C30 H30 124.6 . . ?
C30 C31 H31 126.8 . . ?
C32 C31 C30 106.4(4) . . ?
C32 C31 H31 126.8 . . ?
N28 C32 C31 106.7(4) . . ?
N28 C32 H32 126.6 . . ?
C31 C32 H32 126.6 . . ?
N34 N33 C27 116.7(3) . . ?
C37 N33 C27 132.2(4) . . ?
C37 N33 N34 110.9(4) . . ?
N33 N34 Fe1 112.8(3) . . ?
C35 N34 Fe1 141.5(3) . . ?
C35 N34 N33 105.7(4) . . ?
N34 C35 H35 124.9 . . ?
N34 C35 C36 110.3(4) . . ?
C36 C35 H35 124.9 . . ?
C35 C36 H36 126.8 . . ?
C37 C36 C35 106.3(4) . . ?
C37 C36 H36 126.8 . . ?
N33 C37 C36 106.8(4) . . ?
N33 C37 H37 126.6 . . ?
C36 C37 H37 126.6 . . ?
C25 S38 C39 106.4(2) . . ?
S38 C39 H39 109.2 . . ?
C40 C39 S38 110.0(5) . . ?
C40 C39 H39 109.2 . . ?
C40 C39 C41 112.8(5) . . ?
C41 C39 S38 106.2(4) . . ?
C41 C39 H39 109.2 . . ?
C39 C40 H40A 109.5 . . ?
C39 C40 H40B 109.5 . . ?
C39 C40 H40C 109.5 . . ?
H40A C40 H40B 109.5 . . ?
H40A C40 H40C 109.5 . . ?
H40B C40 H40C 109.5 . . ?
C39 C41 H41A 109.5 . . ?
C39 C41 H41B 109.5 . . ?
C39 C41 H41C 109.5 . . ?
H41A C41 H41B 109.5 . . ?
H41A C41 H41C 109.5 . . ?
H41B C41 H41C 109.5 . . ?
F43A B42A F44A 108.0(10) . . ?
F43A B42A F46A 114.5(12) . . ?
F45A B42A F43A 111.7(10) . . ?
F45A B42A F44A 105.2(11) . . ?
F45A B42A F46A 112.2(10) . . ?
F46A B42A F44A 104.5(9) . . ?
F43B B42B F46B 111.4(11) . . ?
F44B B42B F43B 112.4(11) . . ?
F44B B42B F45B 107.3(11) . . ?
F44B B42B F46B 110.8(11) . . ?
F45B B42B F43B 109.8(11) . . ?
F45B B42B F46B 104.8(10) . . ?
F48A B47A F50A 100.2(8) . . ?
F49A B47A F48A 113.2(10) . . ?
F49A B47A F50A 109.6(8) . . ?
F51A B47A F48A 108.7(8) . . ?
F51A B47A F49A 109.1(9) . . ?
F51A B47A F50A 115.9(10) . . ?
F48B B47B F49B 107.9(11) . . ?
F48B B47B F50B 118.3(10) . . ?
F48B B47B F51B 109.5(10) . . ?
F49B B47B F50B 106.5(9) . . ?
F49B B47B F51B 109.2(10) . . ?
F51B B47B F50B 105.2(10) . . ?

####################################################################### 
# 
# 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_h2o240
_database_code_depnum_ccdc_archive 'CCDC 1976626'
_audit_update_record             
;
2020-01-09 deposited with the CCDC.	2020-05-26 downloaded from the CCDC.
;
_audit_creation_date             2018-06-23
_audit_creation_method           
;
  Olex2 1.2
  (compiled Apr 23 2013 17:54:37, GUI svn.r4466)
;
_chemical_name_common            ?
_chemical_name_systematic        
;
Bis[4-(isopropylsulfanyl)-2,6-di(pyrazol-1-yl)pyridine]iron(II)
ditetrafluoroborate hydrate
;
_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         818.23
_chemical_melting_point          ?
loop_
_atom_type_symbol
_atom_type_description
_atom_type_scat_dispersion_real
_atom_type_scat_dispersion_imag
_atom_type_scat_source
B B 0.0090 0.0039 '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'
F F 0.0727 0.0534 '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'

_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_id
_space_group_symop_operation_xyz
1 'x, y, z'
2 '-x, y+1/2, -z+1/2'
3 '-x, -y, -z'
4 'x, -y-1/2, z-1/2'

_cell_length_a                   20.3115(7)
_cell_length_b                   11.7055(5)
_cell_length_c                   15.7741(8)
_cell_angle_alpha                90.00
_cell_angle_beta                 102.832(4)
_cell_angle_gamma                90.00
_cell_volume                     3656.7(3)
_cell_formula_units_Z            4
_cell_measurement_reflns_used    4346
_cell_measurement_temperature    240(2)
_cell_measurement_theta_min      4.38
_cell_measurement_theta_max      72.51
_exptl_absorpt_coefficient_mu    5.095
_exptl_absorpt_correction_T_min  0.414
_exptl_absorpt_correction_T_max  1.000
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   
;
CrysAlisPro 1.171.39.46 (Rigaku Oxford Diffraction, 2018)
Empirical absorption correction using spherical harmonics,
 implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_crystal_colour            yellow
_exptl_crystal_density_diffrn    1.486
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       plate
_exptl_crystal_F_000             1672
_exptl_crystal_size_max          0.35
_exptl_crystal_size_mid          0.30
_exptl_crystal_size_min          0.10
_exptl_special_details           
;
 ? 
;
_diffrn_reflns_av_R_equivalents  0.0304
_diffrn_reflns_av_unetI/netI     0.0415
_diffrn_reflns_limit_h_max       24
_diffrn_reflns_limit_h_min       -24
_diffrn_reflns_limit_k_max       14
_diffrn_reflns_limit_k_min       -10
_diffrn_reflns_limit_l_max       18
_diffrn_reflns_limit_l_min       -19
_diffrn_reflns_number            13972
_diffrn_reflns_theta_full        72.00
_diffrn_reflns_theta_max         73.48
_diffrn_reflns_theta_min         4.39
_diffrn_ambient_temperature      240(2)
_diffrn_detector_area_resol_mean 5.3095
_diffrn_measured_fraction_theta_full 0.984
_diffrn_measured_fraction_theta_max 0.970
_diffrn_measurement_device_type  'SuperNova, Dual, Cu at zero, Atlas'
_diffrn_measurement_method       'ω scans'
_diffrn_radiation_monochromator  mirror
_diffrn_radiation_type           CuK\a
_diffrn_radiation_wavelength     1.54184
_diffrn_radiation_source         'SuperNova (Cu) X-ray Source'
_diffrn_standards_number         0
_diffrn_standards_interval_count 0
_diffrn_standards_interval_time  0
_diffrn_standards_decay_%        0
_reflns_number_gt                5471
_reflns_number_total             7146
_reflns_threshold_expression     >2sigma(I)
_computing_data_collection       'CrysAlisPro, Agilent Technologies'
_computing_cell_refinement       'CrysAlisPro, Agilent Technologies'
_computing_data_reduction        'CrysAlisPro, Agilent Technologies'
_computing_molecular_graphics    'XSEED (Barbour, 2001)'
_computing_publication_material  
;
O. V. Dolomanov, L. J. Bourhis, R. J. Gildea, J. A. K. Howard and H. Puschmann,
OLEX2: a complete structure solution, refinement and analysis program.
J. Appl. Cryst. (2009). 42, 339-341.
;
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_refine_diff_density_max         0.715
_refine_diff_density_min         -1.135
_refine_diff_density_rms         0.082
_refine_ls_extinction_coef       ?
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.031
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     494
_refine_ls_number_reflns         7146
_refine_ls_number_restraints     68
_refine_ls_R_factor_all          0.0995
_refine_ls_R_factor_gt           0.0804
_refine_ls_restrained_S_all      1.044
_refine_ls_shift/su_max          0.000
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details     
'calc w=1/[σ²(Fo²)+(0.1199P)²+7.1242P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.2226
_refine_ls_wR_factor_ref         0.2390
_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 isopropylsulfanyl substitutents on the complex cation is 
 disordered over three orientations, with occupancies of 0.50, 0.35 and 0.15.
 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. Both BF₄⁻ ions are also disordered, one 
 over two half-occupied sites and the other over three orientations of
 occupancy 0.5, 0.25 and 0;25 which share a common fully occupied B atom. 
 The refined restraints B---F = 1.39(2) and F...F = 2.27(2) Å were applied 
 to those residues. Lastly, the water molecule was also refined over three 
 different sites with a 0.6:0.3:0.1 occupancy ratio.

 All fully occupied non-H 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 could not be located and are not included in
 the model, but are accounted for in the density and F(000) calculations. 
 This disordered water site is positioned to hydrogen bond to anion 
 B42-F46, and to its own symmetry equivalent related by 1-x, 1-y, 1-z.

 The deepest residual Fourier peak of -1.0 e.Å⁻³ is associated with the 
 disordered S atom S38.
;
_olex2_refinement_description    
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups
 At 1.5 times of:
  All C(H,H,H) groups
2. Restrained distances
 B42-F43A = B42-F44A = B42-F45A = B42-F46A
 1.39098 with sigma of 0.02
 B42-F43B = B42-F44B = B42-F45B = B42-F46B
 1.39098 with sigma of 0.02
 B42-F43C = B42-F44C = B42-F45C = B42-F46C
 1.39098 with sigma of 0.02
 F43A-F44A = F43A-F45A = F43A-F46A = F44A-F45A = F44A-F46A = F45A-F46A
 2.27147 with sigma of 0.02
 F43B-F44B = F43B-F45B = F43B-F46B = F44B-F45B = F44B-F46B = F45B-F46B
 2.27147 with sigma of 0.02
 F43C-F44C = F43C-F45C = F43C-F46C = F44C-F45C = F44C-F46C = F45C-F46C
 2.27147 with sigma of 0.02
 B47A-F48A = B47A-F49A = B47A-F50A = B47A-F51A
 1.39098 with sigma of 0.02
 B47B-F48B = B47B-F49B = B47B-F50B = B47B-F51B
 1.39098 with sigma of 0.02
 F48A-F49A = F48A-F50A = F48A-F51A = F49A-F50A = F49A-F51A = F50A-F51A
 2.27147 with sigma of 0.02
 F48B-F49B = F48B-F50B = F48B-F51B = F49B-F50B = F49B-F51B = F50B-F51B
 2.27147 with sigma of 0.02
 C25-S38A = C25-S38B = C25-S38C
 1.75 with sigma of 0.02
 S38A-C39A = S38B-C39B = S38C-C39C
 1.82 with sigma of 0.02
 C39A-C40A = C39A-C41A = C39B-C40B = C39B-C41B = C39C-C40C = C39C-C41C
 1.52 with sigma of 0.02
 C40A-C41A = C40B-C41B = C40C-C41C
 2.48 with sigma of 0.02
 C25-C39A = C25-C39B = C25-C39C
 2.83 with sigma of 0.02
3. Others
 1(DFIX)=1(DFIX)=1(DFIX)=1(DFIX)=1(DFIX)=FVAR(1)
 1(DFIX)=1(DFIX)=1(DFIX)=1(DFIX)=1(DFIX)=1.633*FVAR(2)
 Fixed Sof: S38B(0.35) C39B(0.35) H39B(0.35) C40B(0.35) H40A(0.35) H40B(0.35)
 H40C(0.35) C41B(0.35) H41A(0.35) H41B(0.35) H41C(0.35) S38A(0.5) C39A(0.5)
 H39A(0.5) C40A(0.5) H40D(0.5) H40E(0.5) H40F(0.5) C41A(0.5) H41D(0.5)
 H41E(0.5) H41F(0.5) S38C(0.15) C39C(0.15) H39C(0.15) C40C(0.15) H40G(0.15)
 H40H(0.15) H40I(0.15) C41C(0.15) H41G(0.15) H41H(0.15) H41I(0.15) F43A(0.5)
 F44A(0.5) F45A(0.5) F46A(0.5) F43B(0.25) F44B(0.25) F45B(0.25) F46B(0.25)
 F43C(0.25) F44C(0.25) F45C(0.25) F46C(0.25) B47A(0.5) F48A(0.5) F49A(0.5)
 F50A(0.5) F51A(0.5) B47B(0.5) F48B(0.5) F49B(0.5) F50B(0.5) F51B(0.5)
 O52A(0.6) O52B(0.3) O52C(0.1)
4.a Ternary CH refined with riding coordinates:
 C19(H19), C39B(H39B), C39A(H39A), C39C(H39C)
4.b Me refined with riding coordinates:
 C40B(H40A,H40B,H40C), C41B(H41A,H41B,H41C), C40A(H40D,H40E,H40F), C41A(H41D,
 H41E,H41F), C40C(H40G,H40H,H40I), C41C(H41G,H41H,H41I)
4.c Aromatic/amide H refined with riding coordinates:
 C4(H4), C6(H6), C10(H10), C11(H11), C12(H12), C15(H15), C16(H16), C17(H17),
 C24(H24), C26(H26), C30(H30), C31(H31), C32(H32), C35(H35), C36(H36), C37(H37)
4.d Idealised Me refined as rotating group:
 C20(H20A,H20B,H20C), C21(H21A,H21B,H21C)
;
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_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_symmetry_multiplicity
_atom_site_calc_flag
_atom_site_refinement_flags
_atom_site_disorder_assembly
_atom_site_disorder_group
Fe1 Fe 0.22979(3) 0.60434(7) 0.07047(5) 0.0449(2) Uani 1 1 d . A .
N2 N 0.12301(19) 0.6258(3) 0.0429(3) 0.0435(9) Uani 1 1 d . . .
C3 C 0.0936(2) 0.7021(4) -0.0148(3) 0.0427(10) Uani 1 1 d . . .
C4 C 0.0264(2) 0.7324(4) -0.0280(3) 0.0472(11) Uani 1 1 d . . .
H4 H 0.0072 0.7866 -0.0702 0.057 Uiso 1 1 calc R . .
C5 C -0.0115(2) 0.6794(5) 0.0238(4) 0.0505(11) Uani 1 1 d . . .
C6 C 0.0189(3) 0.5984(5) 0.0865(4) 0.0528(12) Uani 1 1 d . . .
H6 H -0.0054 0.5627 0.1233 0.063 Uiso 1 1 calc R . .
C7 C 0.0856(2) 0.5744(4) 0.0914(3) 0.0455(10) Uani 1 1 d . . .
N8 N 0.13877(19) 0.7535(4) -0.0601(3) 0.0463(9) Uani 1 1 d . . .
N9 N 0.2063(2) 0.7316(4) -0.0302(3) 0.0515(10) Uani 1 1 d . . .
C10 C 0.2371(3) 0.7956(5) -0.0790(4) 0.0649(15) Uani 1 1 d . . .
H10 H 0.2841 0.7987 -0.0732 0.078 Uiso 1 1 calc R . .
C11 C 0.1902(3) 0.8584(6) -0.1406(5) 0.0742(18) Uani 1 1 d . . .
H11 H 0.1992 0.9094 -0.1826 0.089 Uiso 1 1 calc R . .
C12 C 0.1283(3) 0.8287(5) -0.1258(4) 0.0603(14) Uani 1 1 d . . .
H12 H 0.0862 0.8562 -0.1562 0.072 Uiso 1 1 calc R . .
N13 N 0.1231(2) 0.4951(4) 0.1514(3) 0.0491(9) Uani 1 1 d . . .
N14 N 0.1911(2) 0.4870(4) 0.1574(3) 0.0513(10) Uani 1 1 d . . .
C15 C 0.2115(3) 0.4039(5) 0.2145(4) 0.0610(14) Uani 1 1 d . . .
H15 H 0.2564 0.3790 0.2327 0.073 Uiso 1 1 calc R . .
C16 C 0.1566(3) 0.3585(6) 0.2441(4) 0.0703(16) Uani 1 1 d . . .
H16 H 0.1579 0.2990 0.2844 0.084 Uiso 1 1 calc R . .
C17 C 0.1012(3) 0.4177(5) 0.2026(4) 0.0608(14) Uani 1 1 d . . .
H17 H 0.0566 0.4070 0.2084 0.073 Uiso 1 1 calc R . .
S18 S -0.09745(6) 0.70333(13) 0.01818(11) 0.0621(4) Uani 1 1 d . . .
C19 C -0.1165(3) 0.8381(5) -0.0392(4) 0.0602(14) Uani 1 1 d . . .
H19 H -0.1003 0.8346 -0.0938 0.072 Uiso 1 1 calc R . .
C20 C -0.0828(4) 0.9362(6) 0.0142(5) 0.0789(19) Uani 1 1 d . . .
H20A H -0.0910 1.0059 -0.0197 0.118 Uiso 1 1 calc R . .
H20B H -0.0345 0.9222 0.0312 0.118 Uiso 1 1 calc R . .
H20C H -0.1009 0.9440 0.0659 0.118 Uiso 1 1 calc R . .
C21 C -0.1926(3) 0.8496(7) -0.0613(6) 0.086(2) Uani 1 1 d . . .
H21A H -0.2089 0.8541 -0.0080 0.129 Uiso 1 1 calc R . .
H21B H -0.2123 0.7836 -0.0946 0.129 Uiso 1 1 calc R . .
H21C H -0.2052 0.9184 -0.0953 0.129 Uiso 1 1 calc R . .
N22 N 0.33345(19) 0.5855(4) 0.1239(3) 0.0451(9) Uani 1 1 d . A .
C23 C 0.3700(2) 0.5087(4) 0.0907(4) 0.0493(11) Uani 1 1 d . . .
C24 C 0.4370(3) 0.4887(6) 0.1255(4) 0.0645(15) Uani 1 1 d . A .
H24 H 0.4613 0.4347 0.1005 0.077 Uiso 1 1 calc R . .
C25 C 0.4680(2) 0.5502(6) 0.1986(4) 0.0722(18) Uani 1 1 d D . .
C26 C 0.4313(3) 0.6331(6) 0.2325(4) 0.0624(15) Uani 1 1 d . A .
H26 H 0.4513 0.6774 0.2812 0.075 Uiso 1 1 calc R . .
C27 C 0.3641(2) 0.6466(5) 0.1910(3) 0.0487(11) Uani 1 1 d . . .
N28 N 0.3322(2) 0.4500(4) 0.0181(3) 0.0490(9) Uani 1 1 d . . .
N29 N 0.2650(2) 0.4745(4) -0.0087(3) 0.0475(9) Uani 1 1 d . . .
C30 C 0.2438(3) 0.4086(5) -0.0766(4) 0.0570(13) Uani 1 1 d . . .
H30 H 0.1991 0.4070 -0.1091 0.068 Uiso 1 1 calc R . .
C31 C 0.2959(3) 0.3411(6) -0.0948(4) 0.0665(15) Uani 1 1 d . . .
H31 H 0.2931 0.2874 -0.1398 0.080 Uiso 1 1 calc R . .
C32 C 0.3512(3) 0.3702(5) -0.0334(4) 0.0640(15) Uani 1 1 d . . .
H32 H 0.3949 0.3403 -0.0276 0.077 Uiso 1 1 calc R . .
N33 N 0.3213(2) 0.7280(4) 0.2161(3) 0.0521(10) Uani 1 1 d . A .
N34 N 0.2561(2) 0.7338(4) 0.1694(3) 0.0543(10) Uani 1 1 d . . .
C35 C 0.2292(3) 0.8226(5) 0.2034(4) 0.0658(15) Uani 1 1 d . A .
H35 H 0.1843 0.8473 0.1843 0.079 Uiso 1 1 calc R . .
C36 C 0.2758(4) 0.8734(6) 0.2701(5) 0.0761(18) Uani 1 1 d . . .
H36 H 0.2686 0.9370 0.3032 0.091 Uiso 1 1 calc R A .
C37 C 0.3343(3) 0.8128(5) 0.2782(4) 0.0685(16) Uani 1 1 d . A .
H37 H 0.3754 0.8263 0.3182 0.082 Uiso 1 1 calc R . .
S38A S 0.54720(16) 0.4913(3) 0.2557(2) 0.0609(8) Uiso 0.50 1 d PD A 2
C39A C 0.5798(7) 0.5834(12) 0.3452(9) 0.057(4) Uiso 0.50 1 d PD A 2
H39A H 0.5458 0.5947 0.3807 0.069 Uiso 0.50 1 calc PR A 2
C40A C 0.6032(10) 0.7002(13) 0.3164(13) 0.077(4) Uiso 0.50 1 d PD A 2
H40D H 0.5640 0.7469 0.2924 0.116 Uiso 0.50 1 calc PR A 2
H40E H 0.6292 0.6883 0.2725 0.116 Uiso 0.50 1 calc PR A 2
H40F H 0.6310 0.7386 0.3662 0.116 Uiso 0.50 1 calc PR A 2
C41A C 0.6384(7) 0.5149(13) 0.3951(9) 0.065(4) Uiso 0.50 1 d PD A 2
H41D H 0.6224 0.4410 0.4098 0.097 Uiso 0.50 1 calc PR A 2
H41E H 0.6591 0.5553 0.4480 0.097 Uiso 0.50 1 calc PR A 2
H41F H 0.6713 0.5044 0.3597 0.097 Uiso 0.50 1 calc PR A 2
S38B S 0.55477(18) 0.5219(4) 0.2314(3) 0.0455(8) Uiso 0.35 1 d PD A 1
C39B C 0.5811(9) 0.606(2) 0.3314(12) 0.060(7) Uiso 0.35 1 d PD A 1
H39B H 0.5409 0.6289 0.3531 0.073 Uiso 0.35 1 calc PR A 1
C40B C 0.608(2) 0.708(3) 0.291(3) 0.148(18) Uiso 0.35 1 d PD A 1
H40A H 0.5719 0.7404 0.2465 0.222 Uiso 0.35 1 calc PR A 1
H40B H 0.6447 0.6844 0.2654 0.222 Uiso 0.35 1 calc PR A 1
H40C H 0.6237 0.7651 0.3356 0.222 Uiso 0.35 1 calc PR A 1
C41B C 0.6336(13) 0.554(2) 0.4049(16) 0.087(7) Uiso 0.35 1 d PD A 1
H41A H 0.6170 0.4820 0.4218 0.131 Uiso 0.35 1 calc PR A 1
H41B H 0.6421 0.6059 0.4542 0.131 Uiso 0.35 1 calc PR A 1
H41C H 0.6751 0.5417 0.3856 0.131 Uiso 0.35 1 calc PR A 1
S38C S 0.5563(4) 0.5802(9) 0.2108(6) 0.0508(18) Uiso 0.15 1 d PD A 3
C39C C 0.5786(14) 0.645(4) 0.3182(18) 0.070(14) Uiso 0.15 1 d PD A 3
H39C H 0.5485 0.7105 0.3208 0.084 Uiso 0.15 1 calc PR A 3
C40C C 0.575(3) 0.562(5) 0.391(4) 0.12(2) Uiso 0.15 1 d PD A 3
H40G H 0.5289 0.5400 0.3874 0.175 Uiso 0.15 1 calc PR A 3
H40H H 0.5931 0.5989 0.4465 0.175 Uiso 0.15 1 calc PR A 3
H40I H 0.6021 0.4951 0.3857 0.175 Uiso 0.15 1 calc PR A 3
C41C C 0.6493(18) 0.687(4) 0.323(3) 0.080(13) Uiso 0.15 1 d PD A 3
H41G H 0.6814 0.6350 0.3581 0.120 Uiso 0.15 1 calc PR A 3
H41H H 0.6545 0.7625 0.3492 0.120 Uiso 0.15 1 calc PR A 3
H41I H 0.6577 0.6912 0.2649 0.120 Uiso 0.15 1 calc PR A 3
B42 B 0.4515(4) 0.7265(7) 0.4879(5) 0.085(2) Uani 1 1 d D . .
F43A F 0.5045(6) 0.7327(12) 0.5642(7) 0.126(4) Uiso 0.50 1 d PD B 1
F44A F 0.4746(5) 0.7879(9) 0.4231(6) 0.084(3) Uiso 0.50 1 d PD B 1
F45A F 0.3950(4) 0.7639(10) 0.5060(7) 0.089(3) Uiso 0.50 1 d PD B 1
F46A F 0.4450(7) 0.6139(9) 0.4575(8) 0.126(4) Uiso 0.50 1 d PD B 1
F43B F 0.5091(10) 0.675(2) 0.5402(16) 0.156(11) Uiso 0.25 1 d PD B 2
F44B F 0.4650(11) 0.8300(15) 0.4547(14) 0.121(8) Uiso 0.25 1 d PD B 2
F45B F 0.4064(8) 0.7365(16) 0.5404(12) 0.088(5) Uiso 0.25 1 d PD B 2
F46B F 0.4228(14) 0.653(2) 0.4189(14) 0.143(13) Uiso 0.25 1 d PD B 2
F43C F 0.4948(7) 0.7645(13) 0.4418(10) 0.068(4) Uiso 0.25 1 d PD B 3
F44C F 0.4760(11) 0.697(2) 0.5704(9) 0.124(8) Uiso 0.25 1 d PD B 3
F45C F 0.3983(8) 0.8150(15) 0.4826(12) 0.099(6) Uiso 0.25 1 d PD B 3
F46C F 0.4126(8) 0.6360(13) 0.4388(12) 0.073(4) Uiso 0.25 1 d PD B 3
B47A B 0.0735(8) 0.9810(14) 0.2325(10) 0.066(8) Uiso 0.50 1 d PD C 1
F48A F 0.1352(5) 1.0380(9) 0.2302(7) 0.083(3) Uiso 0.50 1 d PD C 1
F49A F 0.0169(4) 1.0510(8) 0.2019(6) 0.073(3) Uiso 0.50 1 d PD C 1
F50A F 0.0798(4) 0.9598(7) 0.3203(5) 0.072(2) Uiso 0.50 1 d PD C 1
F51A F 0.0684(5) 0.8882(8) 0.1804(6) 0.083(3) Uiso 0.50 1 d PD C 1
B47B B 0.0753(7) 0.9980(13) 0.2318(9) 0.051(6) Uiso 0.50 1 d PD D 2
F48B F 0.1353(5) 1.0545(11) 0.2528(8) 0.100(4) Uiso 0.50 1 d PD D 2
F49B F 0.0276(5) 1.0833(9) 0.2064(7) 0.089(3) Uiso 0.50 1 d PD D 2
F50B F 0.0592(5) 0.9282(8) 0.2977(5) 0.079(2) Uiso 0.50 1 d PD D 2
F51B F 0.0772(5) 0.9243(8) 0.1623(6) 0.082(3) Uiso 0.50 1 d PD D 2
O52A O 0.6217(9) 0.5912(13) 0.6504(10) 0.108(4) Uiso 0.60 1 d P E 1
O52B O 0.6318(15) 0.574(3) 0.627(2) 0.111(9) Uiso 0.30 1 d P F 2
O52C O 0.583(5) 0.618(8) 0.625(6) 0.14(3) Uiso 0.10 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 N2 2.130(4) . ?
Fe1 N9 2.152(4) . ?
Fe1 N14 2.205(5) . ?
Fe1 N22 2.099(4) . ?
Fe1 N29 2.185(4) . ?
Fe1 N34 2.156(5) . ?
N2 C3 1.319(6) . ?
N2 C7 1.335(6) . ?
C3 C4 1.380(6) . ?
C3 N8 1.416(6) . ?
C4 H4 0.9400 . ?
C4 C5 1.388(7) . ?
C5 C6 1.411(8) . ?
C5 S18 1.750(5) . ?
C6 H6 0.9400 . ?
C6 C7 1.369(7) . ?
C7 N13 1.419(7) . ?
N8 N9 1.372(5) . ?
N8 C12 1.340(7) . ?
N9 C10 1.326(7) . ?
C10 H10 0.9400 . ?
C10 C11 1.408(9) . ?
C11 H11 0.9400 . ?
C11 C12 1.372(9) . ?
C12 H12 0.9400 . ?
N13 N14 1.368(6) . ?
N13 C17 1.353(7) . ?
N14 C15 1.328(7) . ?
C15 H15 0.9400 . ?
C15 C16 1.404(9) . ?
C16 H16 0.9400 . ?
C16 C17 1.359(9) . ?
C17 H17 0.9400 . ?
S18 C19 1.817(6) . ?
C19 H19 0.9900 . ?
C19 C20 1.497(9) . ?
C19 C21 1.513(8) . ?
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 1.343(6) . ?
N22 C27 1.314(6) . ?
C23 C24 1.370(7) . ?
C23 N28 1.408(7) . ?
C24 H24 0.9400 . ?
C24 C25 1.387(8) . ?
C25 C26 1.400(8) . ?
C25 S38B 1.755(6) . ?
C25 S38A 1.797(6) . ?
C25 S38C 1.796(9) . ?
C26 H26 0.9400 . ?
C26 C27 1.385(7) . ?
C27 N33 1.405(6) . ?
N28 N29 1.365(6) . ?
N28 C32 1.349(7) . ?
N29 C30 1.313(7) . ?
C30 H30 0.9400 . ?
C30 C31 1.400(9) . ?
C31 H31 0.9400 . ?
C31 C32 1.354(9) . ?
C32 H32 0.9400 . ?
N33 N34 1.368(6) . ?
N33 C37 1.378(7) . ?
N34 C35 1.339(7) . ?
C35 H35 0.9400 . ?
C35 C36 1.383(10) . ?
C36 H36 0.9400 . ?
C36 C37 1.365(9) . ?
C37 H37 0.9400 . ?
S38A C39A 1.782(11) . ?
C39A H39A 0.9900 . ?
C39A C40A 1.549(15) . ?
C39A C41A 1.504(14) . ?
C40A H40D 0.9700 . ?
C40A H40E 0.9700 . ?
C40A H40F 0.9700 . ?
C41A H41D 0.9700 . ?
C41A H41E 0.9700 . ?
C41A H41F 0.9700 . ?
S38B C39B 1.837(14) . ?
C39B H39B 0.9900 . ?
C39B C40B 1.506(19) . ?
C39B C41B 1.517(17) . ?
C40B H40A 0.9700 . ?
C40B H40B 0.9700 . ?
C40B H40C 0.9700 . ?
C41B H41A 0.9700 . ?
C41B H41B 0.9700 . ?
C41B H41C 0.9700 . ?
S38C C39C 1.818(18) . ?
C39C H39C 0.9900 . ?
C39C C40C 1.51(2) . ?
C39C C41C 1.506(19) . ?
C40C H40G 0.9700 . ?
C40C H40H 0.9700 . ?
C40C H40I 0.9700 . ?
C41C H41G 0.9700 . ?
C41C H41H 0.9700 . ?
C41C H41I 0.9700 . ?
B42 F43A 1.426(11) . ?
B42 F44A 1.413(11) . ?
B42 F45A 1.319(10) . ?
B42 F46A 1.398(11) . ?
B42 F43B 1.406(15) . ?
B42 F44B 1.372(14) . ?
B42 F45B 1.370(13) . ?
B42 F46B 1.407(15) . ?
B42 F43C 1.336(12) . ?
B42 F44C 1.333(13) . ?
B42 F45C 1.487(13) . ?
B42 F46C 1.440(13) . ?
B47A F48A 1.428(15) . ?
B47A F49A 1.405(15) . ?
B47A F50A 1.386(15) . ?
B47A F51A 1.352(15) . ?
B47B F48B 1.362(14) . ?
B47B F49B 1.388(14) . ?
B47B F50B 1.415(14) . ?
B47B F51B 1.403(14) . ?

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 N9 73.68(15) . . ?
N2 Fe1 N14 73.35(15) . . ?
N2 Fe1 N29 114.41(15) . . ?
N2 Fe1 N34 98.16(16) . . ?
N9 Fe1 N14 147.04(15) . . ?
N9 Fe1 N29 96.11(17) . . ?
N9 Fe1 N34 91.54(18) . . ?
N22 Fe1 N2 168.40(16) . . ?
N22 Fe1 N9 114.05(16) . . ?
N22 Fe1 N14 98.53(16) . . ?
N22 Fe1 N29 74.33(15) . . ?
N22 Fe1 N34 73.62(16) . . ?
N29 Fe1 N14 97.41(16) . . ?
N34 Fe1 N14 93.02(18) . . ?
N34 Fe1 N29 147.40(15) . . ?
C3 N2 Fe1 120.3(3) . . ?
C3 N2 C7 118.2(4) . . ?
C7 N2 Fe1 120.8(3) . . ?
N2 C3 C4 123.9(4) . . ?
N2 C3 N8 113.0(4) . . ?
C4 C3 N8 123.0(4) . . ?
C3 C4 H4 121.4 . . ?
C3 C4 C5 117.2(5) . . ?
C5 C4 H4 121.4 . . ?
C4 C5 C6 119.9(4) . . ?
C4 C5 S18 125.2(4) . . ?
C6 C5 S18 114.8(4) . . ?
C5 C6 H6 121.5 . . ?
C7 C6 C5 116.9(5) . . ?
C7 C6 H6 121.5 . . ?
N2 C7 C6 123.8(5) . . ?
N2 C7 N13 112.8(4) . . ?
C6 C7 N13 123.3(5) . . ?
N9 N8 C3 117.2(4) . . ?
C12 N8 C3 131.3(4) . . ?
C12 N8 N9 111.3(4) . . ?
N8 N9 Fe1 115.1(3) . . ?
C10 N9 Fe1 139.8(4) . . ?
C10 N9 N8 105.0(4) . . ?
N9 C10 H10 124.4 . . ?
N9 C10 C11 111.2(5) . . ?
C11 C10 H10 124.4 . . ?
C10 C11 H11 127.6 . . ?
C12 C11 C10 104.8(5) . . ?
C12 C11 H11 127.6 . . ?
N8 C12 C11 107.7(5) . . ?
N8 C12 H12 126.1 . . ?
C11 C12 H12 126.1 . . ?
N14 N13 C7 118.4(4) . . ?
C17 N13 C7 129.6(5) . . ?
C17 N13 N14 111.9(4) . . ?
N13 N14 Fe1 114.1(3) . . ?
C15 N14 Fe1 141.1(4) . . ?
C15 N14 N13 104.8(4) . . ?
N14 C15 H15 124.7 . . ?
N14 C15 C16 110.7(5) . . ?
C16 C15 H15 124.7 . . ?
C15 C16 H16 126.9 . . ?
C17 C16 C15 106.3(5) . . ?
C17 C16 H16 126.9 . . ?
N13 C17 C16 106.4(5) . . ?
N13 C17 H17 126.8 . . ?
C16 C17 H17 126.8 . . ?
C5 S18 C19 105.3(3) . . ?
S18 C19 H19 108.9 . . ?
C20 C19 S18 111.5(5) . . ?
C20 C19 H19 108.9 . . ?
C20 C19 C21 112.2(6) . . ?
C21 C19 S18 106.6(5) . . ?
C21 C19 H19 108.9 . . ?
C19 C20 H20A 109.5 . . ?
C19 C20 H20B 109.5 . . ?
C19 C20 H20C 109.5 . . ?
H20A C20 H20B 109.5 . . ?
H20A C20 H20C 109.5 . . ?
H20B C20 H20C 109.5 . . ?
C19 C21 H21A 109.5 . . ?
C19 C21 H21B 109.5 . . ?
C19 C21 H21C 109.5 . . ?
H21A C21 H21B 109.5 . . ?
H21A C21 H21C 109.5 . . ?
H21B C21 H21C 109.5 . . ?
C23 N22 Fe1 120.4(3) . . ?
C27 N22 Fe1 121.3(3) . . ?
C27 N22 C23 118.3(4) . . ?
N22 C23 C24 123.0(5) . . ?
N22 C23 N28 113.3(4) . . ?
C24 C23 N28 123.7(5) . . ?
C23 C24 H24 121.0 . . ?
C23 C24 C25 118.1(5) . . ?
C25 C24 H24 121.0 . . ?
C24 C25 C26 119.7(5) . . ?
C24 C25 S38B 112.8(5) . . ?
C24 C25 S38A 114.1(5) . . ?
C24 C25 S38C 116.7(5) . . ?
C26 C25 S38B 127.1(5) . . ?
C26 C25 S38A 124.6(5) . . ?
C26 C25 S38C 115.3(6) . . ?
C25 C26 H26 121.6 . . ?
C27 C26 C25 116.8(5) . . ?
C27 C26 H26 121.6 . . ?
N22 C27 C26 124.0(5) . . ?
N22 C27 N33 112.6(4) . . ?
C26 C27 N33 123.4(5) . . ?
N29 N28 C23 118.4(4) . . ?
C32 N28 C23 130.5(5) . . ?
C32 N28 N29 111.0(4) . . ?
N28 N29 Fe1 113.6(3) . . ?
C30 N29 Fe1 141.7(4) . . ?
C30 N29 N28 104.6(4) . . ?
N29 C30 H30 124.0 . . ?
N29 C30 C31 112.0(5) . . ?
C31 C30 H30 124.0 . . ?
C30 C31 H31 127.6 . . ?
C32 C31 C30 104.8(5) . . ?
C32 C31 H31 127.6 . . ?
N28 C32 C31 107.6(5) . . ?
N28 C32 H32 126.2 . . ?
C31 C32 H32 126.2 . . ?
N34 N33 C27 117.9(4) . . ?
N34 N33 C37 110.9(4) . . ?
C37 N33 C27 131.0(5) . . ?
N33 N34 Fe1 114.2(3) . . ?
C35 N34 Fe1 141.0(4) . . ?
C35 N34 N33 104.8(5) . . ?
N34 C35 H35 124.2 . . ?
N34 C35 C36 111.5(6) . . ?
C36 C35 H35 124.2 . . ?
C35 C36 H36 126.8 . . ?
C37 C36 C35 106.4(6) . . ?
C37 C36 H36 126.8 . . ?
N33 C37 H37 126.8 . . ?
C36 C37 N33 106.4(6) . . ?
C36 C37 H37 126.8 . . ?
C39A S38A C25 107.4(5) . . ?
S38A C39A H39A 110.2 . . ?
C40A C39A S38A 112.7(12) . . ?
C40A C39A H39A 110.2 . . ?
C41A C39A S38A 101.8(9) . . ?
C41A C39A H39A 110.2 . . ?
C41A C39A C40A 111.4(11) . . ?
C39A C40A H40D 109.5 . . ?
C39A C40A H40E 109.5 . . ?
C39A C40A H40F 109.5 . . ?
H40D C40A H40E 109.5 . . ?
H40D C40A H40F 109.5 . . ?
H40E C40A H40F 109.5 . . ?
C39A C41A H41D 109.5 . . ?
C39A C41A H41E 109.5 . . ?
C39A C41A H41F 109.5 . . ?
H41D C41A H41E 109.5 . . ?
H41D C41A H41F 109.5 . . ?
H41E C41A H41F 109.5 . . ?
C25 S38B C39B 103.5(7) . . ?
S38B C39B H39B 109.6 . . ?
C40B C39B S38B 97(2) . . ?
C40B C39B H39B 109.6 . . ?
C40B C39B C41B 112.6(16) . . ?
C41B C39B S38B 117.5(18) . . ?
C41B C39B H39B 109.6 . . ?
C39B C40B H40A 109.5 . . ?
C39B C40B H40B 109.5 . . ?
C39B C40B H40C 109.5 . . ?
H40A C40B H40B 109.5 . . ?
H40A C40B H40C 109.5 . . ?
H40B C40B H40C 109.5 . . ?
C39B C41B H41A 109.5 . . ?
C39B C41B H41B 109.5 . . ?
C39B C41B H41C 109.5 . . ?
H41A C41B H41B 109.5 . . ?
H41A C41B H41C 109.5 . . ?
H41B C41B H41C 109.5 . . ?
C25 S38C C39C 102.6(10) . . ?
S38C C39C H39C 109.5 . . ?
C40C C39C S38C 113(4) . . ?
C40C C39C H39C 109.5 . . ?
C41C C39C S38C 103(3) . . ?
C41C C39C H39C 109.5 . . ?
C41C C39C C40C 112(2) . . ?
C39C C40C H40G 109.5 . . ?
C39C C40C H40H 109.5 . . ?
C39C C40C H40I 109.5 . . ?
H40G C40C H40H 109.5 . . ?
H40G C40C H40I 109.5 . . ?
H40H C40C H40I 109.5 . . ?
C39C C41C H41G 109.5 . . ?
C39C C41C H41H 109.5 . . ?
C39C C41C H41I 109.5 . . ?
H41G C41C H41H 109.5 . . ?
H41G C41C H41I 109.5 . . ?
H41H C41C H41I 109.5 . . ?
F44A B42 F43A 106.0(8) . . ?
F45A B42 F43A 109.3(9) . . ?
F45A B42 F44A 115.6(9) . . ?
F45A B42 F46A 111.5(9) . . ?
F46A B42 F43A 109.5(9) . . ?
F46A B42 F44A 104.6(8) . . ?
F43B B42 F46B 110.1(14) . . ?
F44B B42 F43B 112.9(13) . . ?
F44B B42 F46B 109.1(13) . . ?
F45B B42 F43B 105.2(12) . . ?
F45B B42 F44B 111.8(12) . . ?
F45B B42 F46B 107.6(13) . . ?
F43C B42 F45C 107.1(11) . . ?
F43C B42 F46C 107.5(10) . . ?
F44C B42 F43C 118.1(12) . . ?
F44C B42 F45C 110.4(12) . . ?
F44C B42 F46C 111.9(12) . . ?
F46C B42 F45C 100.1(10) . . ?
F49A B47A F48A 112.0(13) . . ?
F50A B47A F48A 102.8(11) . . ?
F50A B47A F49A 109.6(11) . . ?
F51A B47A F48A 108.0(12) . . ?
F51A B47A F49A 108.3(11) . . ?
F51A B47A F50A 116.2(13) . . ?
F48B B47B F49B 104.6(12) . . ?
F48B B47B F50B 116.2(11) . . ?
F48B B47B F51B 108.1(11) . . ?
F49B B47B F50B 111.6(10) . . ?
F49B B47B F51B 110.8(10) . . ?
F51B B47B F50B 105.6(11) . . ?

####################################################################### 
# 
# 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_h2o190
_database_code_depnum_ccdc_archive 'CCDC 1976624'
_audit_update_record             
;
2020-01-09 deposited with the CCDC.	2020-05-26 downloaded from the CCDC.
;
_audit_creation_date             2018-06-23
_audit_creation_method           
;
  Olex2 1.2
  (compiled Apr 23 2013 17:54:37, GUI svn.r4466)
;
_chemical_name_common            ?
_chemical_name_systematic        
;
Bis[4-(isopropylsulfanyl)-2,6-di(pyrazol-1-yl)pyridine]iron(II)
ditetrafluoroborate hydrate
;
_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         818.23
_chemical_melting_point          ?
loop_
_atom_type_symbol
_atom_type_description
_atom_type_scat_dispersion_real
_atom_type_scat_dispersion_imag
_atom_type_scat_source
B B 0.0090 0.0039 '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'
F F 0.0727 0.0534 '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'

_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_id
_space_group_symop_operation_xyz
1 'x, y, z'
2 '-x, y+1/2, -z+1/2'
3 '-x, -y, -z'
4 'x, -y-1/2, z-1/2'

_cell_length_a                   19.8308(5)
_cell_length_b                   11.9218(3)
_cell_length_c                   15.5604(5)
_cell_angle_alpha                90.00
_cell_angle_beta                 102.502(3)
_cell_angle_gamma                90.00
_cell_volume                     3591.52(18)
_cell_formula_units_Z            4
_cell_measurement_reflns_used    4096
_cell_measurement_temperature    190(2)
_cell_measurement_theta_min      4.34
_cell_measurement_theta_max      72.22
_exptl_absorpt_coefficient_mu    5.188
_exptl_absorpt_correction_T_min  0.394
_exptl_absorpt_correction_T_max  1.000
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   
;
CrysAlisPro 1.171.39.46 (Rigaku Oxford Diffraction, 2018)
Empirical absorption correction using spherical harmonics,
 implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_crystal_colour            brown
_exptl_crystal_density_diffrn    1.513
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       plate
_exptl_crystal_F_000             1672
_exptl_crystal_size_max          0.35
_exptl_crystal_size_mid          0.30
_exptl_crystal_size_min          0.10
_exptl_special_details           
;
 ? 
;
_diffrn_reflns_av_R_equivalents  0.0318
_diffrn_reflns_av_unetI/netI     0.0476
_diffrn_reflns_limit_h_max       23
_diffrn_reflns_limit_h_min       -24
_diffrn_reflns_limit_k_max       14
_diffrn_reflns_limit_k_min       -10
_diffrn_reflns_limit_l_max       18
_diffrn_reflns_limit_l_min       -19
_diffrn_reflns_number            13580
_diffrn_reflns_theta_full        72.00
_diffrn_reflns_theta_max         73.48
_diffrn_reflns_theta_min         4.36
_diffrn_ambient_temperature      190(2)
_diffrn_detector_area_resol_mean 5.3095
_diffrn_measured_fraction_theta_full 0.985
_diffrn_measured_fraction_theta_max 0.972
_diffrn_measurement_device_type  'SuperNova, Dual, Cu at zero, Atlas'
_diffrn_measurement_method       'ω scans'
_diffrn_radiation_monochromator  mirror
_diffrn_radiation_type           CuK\a
_diffrn_radiation_wavelength     1.54184
_diffrn_radiation_source         'SuperNova (Cu) X-ray Source'
_diffrn_standards_number         0
_diffrn_standards_interval_count 0
_diffrn_standards_interval_time  0
_diffrn_standards_decay_%        0
_reflns_number_gt                5328
_reflns_number_total             7040
_reflns_threshold_expression     >2sigma(I)
_computing_data_collection       'CrysAlisPro, Agilent Technologies'
_computing_cell_refinement       'CrysAlisPro, Agilent Technologies'
_computing_data_reduction        'CrysAlisPro, Agilent Technologies'
_computing_molecular_graphics    'XSEED (Barbour, 2001)'
_computing_publication_material  
;
O. V. Dolomanov, L. J. Bourhis, R. J. Gildea, J. A. K. Howard and H. Puschmann,
OLEX2: a complete structure solution, refinement and analysis program.
J. Appl. Cryst. (2009). 42, 339-341.
;
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_refine_diff_density_max         0.550
_refine_diff_density_min         -0.572
_refine_diff_density_rms         0.074
_refine_ls_extinction_coef       ?
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.052
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     479
_refine_ls_number_reflns         7040
_refine_ls_number_restraints     50
_refine_ls_R_factor_all          0.0866
_refine_ls_R_factor_gt           0.0659
_refine_ls_restrained_S_all      1.065
_refine_ls_shift/su_max          0.000
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details     
'calc w=1/[σ²(Fo²)+(0.0858P)²+4.8624P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1721
_refine_ls_wR_factor_ref         0.1855
_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. 

 Both the BF₄⁻ ions is disordered, one over two equally occupied sites and
 the other over three sites of occupancy 0.5, 0.4 and 0.1, two of which share
 a common B atom. The anions were treated with the refined restraints B---F = 
 1.39(2) and F...F = 2.27(2) Å. The water molecule was also modelled as 
 disordered, over two sites with occupancies of 0.67 and 0.33. All fully 
 occupied non-H 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 Fouier map and could not be included in 
 the model, but are accounted for in the molecular weight and density 
 calculations. 
;
_olex2_refinement_description    
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups
 At 1.5 times of:
  All C(H,H,H) groups
2. Restrained distances
 B42A-F43A = B42A-F44A = B42A-F45A = B42A-F46A
 1.3936 with sigma of 0.02
 B42B-F43B = B42B-F44B = B42B-F45B = B42B-F46B
 1.3936 with sigma of 0.02
 B42A-F43C = B42A-F44C = B42A-F45C = B42A-F46C
 1.3936 with sigma of 0.02
 F43A-F44A = F43A-F45A = F43A-F46A = F44A-F45A = F44A-F46A = F45A-F46A
 2.275749 with sigma of 0.02
 F43B-F44B = F43B-F45B = F43B-F46B = F44B-F45B = F44B-F46B = F45B-F46B
 2.275749 with sigma of 0.02
 F43C-F44C = F43C-F45C = F43C-F46C = F44C-F45C = F44C-F46C = F45C-F46C
 2.275749 with sigma of 0.02
 B47A-F48A = B47A-F49A = B47A-F50A = B47A-F51A
 1.3936 with sigma of 0.02
 B47B-F48B = B47B-F49B = B47B-F50B = B47B-F51B
 1.3936 with sigma of 0.02
 F48A-F49A = F48A-F50A = F48A-F51A = F49A-F50A = F49A-F51A = F50A-F51A
 2.275749 with sigma of 0.02
 F48B-F49B = F48B-F50B = F48B-F51B = F49B-F50B = F49B-F51B = F50B-F51B
 2.275749 with sigma of 0.02
3. Others
 1(DFIX)=1(DFIX)=1(DFIX)=1(DFIX)=1(DFIX)=FVAR(1)
 1(DFIX)=1(DFIX)=1(DFIX)=1(DFIX)=1(DFIX)=1.633*FVAR(2)
 Fixed Sof: B42A(0.6) F43A(0.5) F44A(0.5) F45A(0.5) F46A(0.5) B42B(0.4)
 F43B(0.4) F44B(0.4) F45B(0.4) F46B(0.4) F43C(0.1) F44C(0.1) F45C(0.1)
 F46C(0.1) B47A(0.5) F48A(0.5) F49A(0.5) F50A(0.5) F51A(0.5) B47B(0.5)
 F48B(0.5) F49B(0.5) F50B(0.5) F51B(0.5) O52A(0.67) O52B(0.33)
4.a Ternary CH refined with riding coordinates:
 C19(H19), C39(H39)
4.b Aromatic/amide H refined with riding coordinates:
 C4(H4), C6(H6), C10(H10), C11(H11), C12(H12), C15(H15), C16(H16), C17(H17),
 C24(H24), C26(H26), C30(H30), C31(H31), C32(H32), C35(H35), C36(H36), C37(H37)
4.c Idealised Me refined as rotating group:
 C20(H20A,H20B,H20C), C21(H21A,H21B,H21C), C40(H40A,H40B,H40C), C41(H41A,H41B,
 H41C)
;
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_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_symmetry_multiplicity
_atom_site_calc_flag
_atom_site_refinement_flags
_atom_site_disorder_assembly
_atom_site_disorder_group
Fe1 Fe 0.23213(3) 0.61331(5) 0.08098(4) 0.03520(18) Uani 1 1 d . . .
N2 N 0.13446(17) 0.6333(3) 0.0478(2) 0.0376(7) Uani 1 1 d . . .
C3 C 0.1067(2) 0.7106(4) -0.0110(3) 0.0381(9) Uani 1 1 d . . .
C4 C 0.0375(2) 0.7379(4) -0.0300(3) 0.0403(9) Uani 1 1 d . . .
H4 H 0.0192 0.7926 -0.0731 0.048 Uiso 1 1 calc R . .
C5 C -0.0042(2) 0.6816(4) 0.0171(3) 0.0431(10) Uani 1 1 d . . .
C6 C 0.0245(2) 0.5998(4) 0.0803(3) 0.0450(10) Uani 1 1 d . . .
H6 H -0.0033 0.5604 0.1129 0.054 Uiso 1 1 calc R . .
C7 C 0.0933(2) 0.5799(4) 0.0926(3) 0.0417(9) Uani 1 1 d . . .
N8 N 0.15853(17) 0.7613(3) -0.0469(2) 0.0397(8) Uani 1 1 d . . .
N9 N 0.22593(17) 0.7331(3) -0.0089(2) 0.0395(8) Uani 1 1 d . . .
C10 C 0.2646(2) 0.8009(4) -0.0449(3) 0.0467(10) Uani 1 1 d . . .
H10 H 0.3137 0.8012 -0.0316 0.056 Uiso 1 1 calc R . .
C11 C 0.2229(3) 0.8721(4) -0.1055(4) 0.0553(12) Uani 1 1 d . . .
H11 H 0.2384 0.9283 -0.1399 0.066 Uiso 1 1 calc R . .
C12 C 0.1569(3) 0.8463(4) -0.1059(3) 0.0497(11) Uani 1 1 d . . .
H12 H 0.1169 0.8806 -0.1406 0.060 Uiso 1 1 calc R . .
N13 N 0.13186(18) 0.5059(3) 0.1546(3) 0.0415(8) Uani 1 1 d . . .
N14 N 0.20178(18) 0.5024(3) 0.1606(3) 0.0412(8) Uani 1 1 d . . .
C15 C 0.2253(3) 0.4250(4) 0.2207(3) 0.0497(11) Uani 1 1 d . . .
H15 H 0.2725 0.4042 0.2393 0.060 Uiso 1 1 calc R . .
C16 C 0.1712(3) 0.3781(5) 0.2531(4) 0.0567(13) Uani 1 1 d . . .
H16 H 0.1747 0.3216 0.2969 0.068 Uiso 1 1 calc R . .
C17 C 0.1126(3) 0.4294(4) 0.2095(3) 0.0509(11) Uani 1 1 d . . .
H17 H 0.0669 0.4146 0.2161 0.061 Uiso 1 1 calc R . .
S18 S -0.09356(5) 0.70034(11) 0.00346(9) 0.0527(3) Uani 1 1 d . . .
C19 C -0.1127(2) 0.8348(4) -0.0523(3) 0.0490(11) Uani 1 1 d . . .
H19 H -0.0928 0.8361 -0.1061 0.059 Uiso 1 1 calc R . .
C20 C -0.0828(3) 0.9296(5) 0.0077(4) 0.0655(15) Uani 1 1 d . . .
H20A H -0.0943 1.0011 -0.0230 0.098 Uiso 1 1 calc R . .
H20B H -0.0325 0.9214 0.0245 0.098 Uiso 1 1 calc R . .
H20C H -0.1021 0.9279 0.0606 0.098 Uiso 1 1 calc R . .
C21 C -0.1908(3) 0.8415(5) -0.0791(5) 0.0697(16) Uani 1 1 d . . .
H21A H -0.2102 0.8420 -0.0263 0.105 Uiso 1 1 calc R . .
H21B H -0.2085 0.7763 -0.1155 0.105 Uiso 1 1 calc R . .
H21C H -0.2042 0.9104 -0.1128 0.105 Uiso 1 1 calc R . .
N22 N 0.32908(17) 0.5940(3) 0.1235(2) 0.0376(7) Uani 1 1 d . . .
C23 C 0.3636(2) 0.5167(4) 0.0876(3) 0.0395(9) Uani 1 1 d . . .
C24 C 0.4318(2) 0.4927(4) 0.1202(3) 0.0445(10) Uani 1 1 d . . .
H24 H 0.4551 0.4377 0.0933 0.053 Uiso 1 1 calc R . .
C25 C 0.4660(2) 0.5518(4) 0.1943(3) 0.0463(10) Uani 1 1 d . . .
C26 C 0.4308(2) 0.6346(4) 0.2319(3) 0.0447(10) Uani 1 1 d . . .
H26 H 0.4535 0.6776 0.2812 0.054 Uiso 1 1 calc R . .
C27 C 0.3624(2) 0.6506(4) 0.1943(3) 0.0375(9) Uani 1 1 d . . .
N28 N 0.31957(18) 0.4649(3) 0.0156(2) 0.0407(8) Uani 1 1 d . . .
N29 N 0.25117(18) 0.4962(3) -0.0019(2) 0.0396(8) Uani 1 1 d . . .
C30 C 0.2219(2) 0.4386(4) -0.0724(3) 0.0434(10) Uani 1 1 d . . .
H30 H 0.1743 0.4426 -0.1001 0.052 Uiso 1 1 calc R . .
C31 C 0.2703(3) 0.3708(4) -0.1009(3) 0.0521(12) Uani 1 1 d . . .
H31 H 0.2619 0.3218 -0.1502 0.062 Uiso 1 1 calc R . .
C32 C 0.3317(3) 0.3891(4) -0.0441(3) 0.0511(11) Uani 1 1 d . . .
H32 H 0.3747 0.3552 -0.0458 0.061 Uiso 1 1 calc R . .
N33 N 0.31711(17) 0.7271(3) 0.2219(2) 0.0398(8) Uani 1 1 d . . .
N34 N 0.24966(17) 0.7269(3) 0.1756(2) 0.0391(8) Uani 1 1 d . . .
C35 C 0.2193(2) 0.8093(4) 0.2090(3) 0.0480(11) Uani 1 1 d . . .
H35 H 0.1720 0.8292 0.1901 0.058 Uiso 1 1 calc R . .
C36 C 0.2663(3) 0.8636(4) 0.2763(4) 0.0528(12) Uani 1 1 d . . .
H36 H 0.2572 0.9257 0.3104 0.063 Uiso 1 1 calc R . .
C37 C 0.3279(3) 0.8089(4) 0.2829(3) 0.0473(10) Uani 1 1 d . . .
H37 H 0.3701 0.8255 0.3229 0.057 Uiso 1 1 calc R . .
S38 S 0.55150(6) 0.51175(13) 0.23460(10) 0.0647(4) Uani 1 1 d . . .
C39 C 0.5818(2) 0.5919(5) 0.3345(4) 0.0563(13) Uani 1 1 d . . .
H39 H 0.5430 0.6015 0.3657 0.068 Uiso 1 1 calc R . .
C40 C 0.6067(4) 0.7053(6) 0.3130(6) 0.085(2) Uani 1 1 d . . .
H40A H 0.6146 0.7527 0.3656 0.127 Uiso 1 1 calc R . .
H40B H 0.5718 0.7401 0.2664 0.127 Uiso 1 1 calc R . .
H40C H 0.6500 0.6970 0.2928 0.127 Uiso 1 1 calc R . .
C41 C 0.6389(3) 0.5212(6) 0.3919(4) 0.0726(17) Uani 1 1 d . . .
H41A H 0.6779 0.5144 0.3629 0.109 Uiso 1 1 calc R . .
H41B H 0.6208 0.4463 0.4002 0.109 Uiso 1 1 calc R . .
H41C H 0.6543 0.5575 0.4493 0.109 Uiso 1 1 calc R . .
B42A B 0.4710(6) 0.7257(10) 0.4968(7) 0.051(5) Uiso 0.60 1 d PD . .
F43A F 0.5322(4) 0.7387(7) 0.5610(6) 0.082(2) Uiso 0.50 1 d PD A 1
F44A F 0.4799(4) 0.7851(6) 0.4221(4) 0.0741(18) Uiso 0.50 1 d PD A 1
F45A F 0.4171(4) 0.7638(8) 0.5280(6) 0.081(2) Uiso 0.50 1 d PD A 1
F46A F 0.4620(5) 0.6146(7) 0.4690(6) 0.087(3) Uiso 0.50 1 d PD A 1
B42B B 0.4663(8) 0.7401(14) 0.4929(10) 0.053(8) Uiso 0.40 1 d PD A 2
F43B F 0.5372(5) 0.7202(9) 0.5235(8) 0.083(3) Uiso 0.40 1 d PD A 2
F44B F 0.4515(5) 0.8403(8) 0.4513(6) 0.082(3) Uiso 0.40 1 d PD A 2
F45B F 0.4334(4) 0.7320(7) 0.5635(5) 0.060(2) Uiso 0.40 1 d PD A 2
F46B F 0.4378(6) 0.6548(9) 0.4318(7) 0.080(4) Uiso 0.40 1 d PD A 2
F43C F 0.5188(11) 0.764(2) 0.4535(17) 0.058(7) Uiso 0.10 1 d PD A 3
F44C F 0.4947(17) 0.700(3) 0.5835(12) 0.108(14) Uiso 0.10 1 d PD A 3
F45C F 0.4169(9) 0.8088(15) 0.4909(14) 0.032(5) Uiso 0.10 1 d PD A 3
F46C F 0.4382(11) 0.6303(16) 0.4504(16) 0.021(5) Uiso 0.10 1 d PD A 3
B47A B 0.0629(6) 0.9744(11) 0.2288(7) 0.043(3) Uiso 0.50 1 d PD B 1
F48A F 0.1277(3) 1.0277(6) 0.2332(4) 0.0539(15) Uiso 0.50 1 d PD B 1
F49A F 0.0057(4) 1.0457(7) 0.1970(6) 0.056(3) Uiso 0.50 1 d PD B 1
F50A F 0.0675(4) 0.9537(7) 0.3189(4) 0.054(2) Uiso 0.50 1 d PD B 1
F51A F 0.0588(3) 0.8842(6) 0.1758(4) 0.0587(16) Uiso 0.50 1 d PD B 1
B47B B 0.0679(6) 1.0032(11) 0.2334(8) 0.047(3) Uiso 0.50 1 d PD C 2
F48B F 0.1227(4) 1.0721(8) 0.2504(6) 0.086(2) Uiso 0.50 1 d PD C 2
F49B F 0.0101(5) 1.0688(8) 0.2064(7) 0.071(3) Uiso 0.50 1 d PD C 2
F50B F 0.0549(4) 0.9331(7) 0.3050(5) 0.064(3) Uiso 0.50 1 d PD C 2
F51B F 0.0740(4) 0.9281(7) 0.1665(5) 0.075(2) Uiso 0.50 1 d PD C 2
O52A O 0.6290(5) 0.5564(8) 0.6266(6) 0.082(3) Uiso 0.67 1 d P D 1
O52B O 0.6182(10) 0.5757(17) 0.6468(13) 0.084(6) Uiso 0.33 1 d P E 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 N2 1.908(3) . ?
Fe1 N9 1.983(4) . ?
Fe1 N14 1.991(4) . ?
Fe1 N22 1.907(3) . ?
Fe1 N29 1.992(4) . ?
Fe1 N34 1.975(4) . ?
N2 C3 1.330(5) . ?
N2 C7 1.344(6) . ?
C3 C4 1.379(6) . ?
C3 N8 1.407(5) . ?
C4 H4 0.9500 . ?
C4 C5 1.390(6) . ?
C5 C6 1.414(7) . ?
C5 S18 1.754(4) . ?
C6 H6 0.9500 . ?
C6 C7 1.357(6) . ?
C7 N13 1.405(6) . ?
N8 N9 1.381(5) . ?
N8 C12 1.363(6) . ?
N9 C10 1.320(6) . ?
C10 H10 0.9500 . ?
C10 C11 1.399(7) . ?
C11 H11 0.9500 . ?
C11 C12 1.343(7) . ?
C12 H12 0.9500 . ?
N13 N14 1.370(5) . ?
N13 C17 1.360(6) . ?
N14 C15 1.326(6) . ?
C15 H15 0.9500 . ?
C15 C16 1.397(7) . ?
C16 H16 0.9500 . ?
C16 C17 1.357(7) . ?
C17 H17 0.9500 . ?
S18 C19 1.823(5) . ?
C19 H19 1.0000 . ?
C19 C20 1.503(8) . ?
C19 C21 1.517(7) . ?
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 C23 1.339(5) . ?
N22 C27 1.338(5) . ?
C23 C24 1.369(6) . ?
C23 N28 1.405(6) . ?
C24 H24 0.9500 . ?
C24 C25 1.395(7) . ?
C25 C26 1.408(6) . ?
C25 S38 1.742(4) . ?
C26 H26 0.9500 . ?
C26 C27 1.369(6) . ?
C27 N33 1.411(5) . ?
N28 N29 1.376(5) . ?
N28 C32 1.354(6) . ?
N29 C30 1.317(6) . ?
C30 H30 0.9500 . ?
C30 C31 1.399(7) . ?
C31 H31 0.9500 . ?
C31 C32 1.358(7) . ?
C32 H32 0.9500 . ?
N33 N34 1.375(5) . ?
N33 C37 1.346(6) . ?
N34 C35 1.317(6) . ?
C35 H35 0.9500 . ?
C35 C36 1.400(7) . ?
C36 H36 0.9500 . ?
C36 C37 1.368(7) . ?
C37 H37 0.9500 . ?
S38 C39 1.813(5) . ?
C39 H39 1.0000 . ?
C39 C40 1.502(9) . ?
C39 C41 1.533(8) . ?
C40 H40A 0.9800 . ?
C40 H40B 0.9800 . ?
C40 H40C 0.9800 . ?
C41 H41A 0.9800 . ?
C41 H41B 0.9800 . ?
C41 H41C 0.9800 . ?
B42A F43A 1.403(12) . ?
B42A F44A 1.403(12) . ?
B42A F45A 1.347(12) . ?
B42A F46A 1.393(12) . ?
B42A F43C 1.354(15) . ?
B42A F44C 1.362(15) . ?
B42A F45C 1.449(15) . ?
B42A F46C 1.426(14) . ?
B42B F43B 1.404(15) . ?
B42B F44B 1.360(16) . ?
B42B F45B 1.395(15) . ?
B42B F46B 1.423(15) . ?
B47A F48A 1.422(12) . ?
B47A F49A 1.418(12) . ?
B47A F50A 1.407(12) . ?
B47A F51A 1.347(12) . ?
B47B F48B 1.342(13) . ?
B47B F49B 1.378(12) . ?
B47B F50B 1.459(12) . ?
B47B F51B 1.398(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
N2 Fe1 N9 79.32(14) . . ?
N2 Fe1 N14 79.97(15) . . ?
N2 Fe1 N29 103.63(15) . . ?
N2 Fe1 N34 96.94(15) . . ?
N9 Fe1 N14 159.26(14) . . ?
N9 Fe1 N29 92.26(15) . . ?
N14 Fe1 N29 93.60(15) . . ?
N22 Fe1 N2 175.51(16) . . ?
N22 Fe1 N9 103.64(15) . . ?
N22 Fe1 N14 96.98(15) . . ?
N22 Fe1 N29 79.75(15) . . ?
N22 Fe1 N34 79.77(14) . . ?
N34 Fe1 N9 90.35(15) . . ?
N34 Fe1 N14 91.12(16) . . ?
N34 Fe1 N29 159.40(14) . . ?
C3 N2 Fe1 121.1(3) . . ?
C3 N2 C7 118.6(4) . . ?
C7 N2 Fe1 119.7(3) . . ?
N2 C3 C4 123.7(4) . . ?
N2 C3 N8 110.0(3) . . ?
C4 C3 N8 126.3(4) . . ?
C3 C4 H4 121.6 . . ?
C3 C4 C5 116.8(4) . . ?
C5 C4 H4 121.6 . . ?
C4 C5 C6 120.3(4) . . ?
C4 C5 S18 125.1(4) . . ?
C6 C5 S18 114.6(3) . . ?
C5 C6 H6 121.3 . . ?
C7 C6 C5 117.3(4) . . ?
C7 C6 H6 121.3 . . ?
N2 C7 C6 123.3(4) . . ?
N2 C7 N13 110.7(4) . . ?
C6 C7 N13 126.0(4) . . ?
N9 N8 C3 116.6(3) . . ?
C12 N8 C3 132.4(4) . . ?
C12 N8 N9 110.4(4) . . ?
N8 N9 Fe1 112.6(3) . . ?
C10 N9 Fe1 141.9(3) . . ?
C10 N9 N8 105.5(4) . . ?
N9 C10 H10 124.9 . . ?
N9 C10 C11 110.2(4) . . ?
C11 C10 H10 124.9 . . ?
C10 C11 H11 126.4 . . ?
C12 C11 C10 107.3(4) . . ?
C12 C11 H11 126.4 . . ?
N8 C12 H12 126.7 . . ?
C11 C12 N8 106.7(4) . . ?
C11 C12 H12 126.7 . . ?
N14 N13 C7 117.3(4) . . ?
C17 N13 C7 131.9(4) . . ?
C17 N13 N14 110.8(4) . . ?
N13 N14 Fe1 112.0(3) . . ?
C15 N14 Fe1 142.5(3) . . ?
C15 N14 N13 105.4(4) . . ?
N14 C15 H15 124.7 . . ?
N14 C15 C16 110.6(4) . . ?
C16 C15 H15 124.7 . . ?
C15 C16 H16 126.8 . . ?
C17 C16 C15 106.4(4) . . ?
C17 C16 H16 126.8 . . ?
N13 C17 H17 126.6 . . ?
C16 C17 N13 106.8(4) . . ?
C16 C17 H17 126.6 . . ?
C5 S18 C19 105.7(2) . . ?
S18 C19 H19 109.5 . . ?
C20 C19 S18 110.6(4) . . ?
C20 C19 H19 109.5 . . ?
C20 C19 C21 111.9(5) . . ?
C21 C19 S18 105.8(4) . . ?
C21 C19 H19 109.5 . . ?
C19 C20 H20A 109.5 . . ?
C19 C20 H20B 109.5 . . ?
C19 C20 H20C 109.5 . . ?
H20A C20 H20B 109.5 . . ?
H20A C20 H20C 109.5 . . ?
H20B C20 H20C 109.5 . . ?
C19 C21 H21A 109.5 . . ?
C19 C21 H21B 109.5 . . ?
C19 C21 H21C 109.5 . . ?
H21A C21 H21B 109.5 . . ?
H21A C21 H21C 109.5 . . ?
H21B C21 H21C 109.5 . . ?
C23 N22 Fe1 120.4(3) . . ?
C27 N22 Fe1 120.4(3) . . ?
C27 N22 C23 119.0(4) . . ?
N22 C23 C24 122.8(4) . . ?
N22 C23 N28 110.5(4) . . ?
C24 C23 N28 126.7(4) . . ?
C23 C24 H24 121.1 . . ?
C23 C24 C25 117.8(4) . . ?
C25 C24 H24 121.1 . . ?
C24 C25 C26 120.1(4) . . ?
C24 C25 S38 114.9(3) . . ?
C26 C25 S38 125.0(4) . . ?
C25 C26 H26 121.5 . . ?
C27 C26 C25 117.0(4) . . ?
C27 C26 H26 121.5 . . ?
N22 C27 C26 123.3(4) . . ?
N22 C27 N33 110.0(3) . . ?
C26 C27 N33 126.7(4) . . ?
N29 N28 C23 117.0(3) . . ?
C32 N28 C23 132.0(4) . . ?
C32 N28 N29 111.0(4) . . ?
N28 N29 Fe1 112.2(3) . . ?
C30 N29 Fe1 142.5(3) . . ?
C30 N29 N28 105.2(4) . . ?
N29 C30 H30 124.6 . . ?
N29 C30 C31 110.8(4) . . ?
C31 C30 H30 124.6 . . ?
C30 C31 H31 126.8 . . ?
C32 C31 C30 106.3(4) . . ?
C32 C31 H31 126.8 . . ?
N28 C32 C31 106.7(4) . . ?
N28 C32 H32 126.7 . . ?
C31 C32 H32 126.7 . . ?
N34 N33 C27 116.8(3) . . ?
C37 N33 C27 132.0(4) . . ?
C37 N33 N34 111.0(4) . . ?
N33 N34 Fe1 112.7(2) . . ?
C35 N34 Fe1 141.7(3) . . ?
C35 N34 N33 105.5(4) . . ?
N34 C35 H35 124.7 . . ?
N34 C35 C36 110.7(4) . . ?
C36 C35 H35 124.7 . . ?
C35 C36 H36 127.0 . . ?
C37 C36 C35 106.0(4) . . ?
C37 C36 H36 127.0 . . ?
N33 C37 C36 106.8(4) . . ?
N33 C37 H37 126.6 . . ?
C36 C37 H37 126.6 . . ?
C25 S38 C39 106.3(2) . . ?
S38 C39 H39 109.2 . . ?
C40 C39 S38 110.3(5) . . ?
C40 C39 H39 109.2 . . ?
C40 C39 C41 112.9(5) . . ?
C41 C39 S38 106.0(4) . . ?
C41 C39 H39 109.2 . . ?
C39 C40 H40A 109.5 . . ?
C39 C40 H40B 109.5 . . ?
C39 C40 H40C 109.5 . . ?
H40A C40 H40B 109.5 . . ?
H40A C40 H40C 109.5 . . ?
H40B C40 H40C 109.5 . . ?
C39 C41 H41A 109.5 . . ?
C39 C41 H41B 109.5 . . ?
C39 C41 H41C 109.5 . . ?
H41A C41 H41B 109.5 . . ?
H41A C41 H41C 109.5 . . ?
H41B C41 H41C 109.5 . . ?
F43A B42A F44A 106.9(8) . . ?
F45A B42A F43A 109.7(9) . . ?
F45A B42A F44A 112.3(10) . . ?
F45A B42A F46A 111.9(9) . . ?
F46A B42A F43A 111.1(10) . . ?
F46A B42A F44A 104.7(8) . . ?
F43C B42A F44C 116.0(15) . . ?
F43C B42A F45C 109.1(13) . . ?
F43C B42A F46C 108.0(13) . . ?
F44C B42A F45C 107.8(14) . . ?
F44C B42A F46C 110.3(15) . . ?
F46C B42A F45C 105.2(12) . . ?
F43B B42B F46B 109.2(12) . . ?
F44B B42B F43B 113.9(12) . . ?
F44B B42B F45B 110.3(12) . . ?
F44B B42B F46B 107.2(12) . . ?
F45B B42B F43B 109.0(12) . . ?
F45B B42B F46B 106.9(11) . . ?
F49A B47A F48A 113.2(10) . . ?
F50A B47A F48A 99.6(8) . . ?
F50A B47A F49A 109.1(8) . . ?
F51A B47A F48A 108.7(8) . . ?
F51A B47A F49A 109.1(9) . . ?
F51A B47A F50A 116.9(10) . . ?
F48B B47B F49B 107.3(10) . . ?
F48B B47B F50B 118.1(10) . . ?
F48B B47B F51B 110.0(9) . . ?
F49B B47B F50B 106.5(9) . . ?
F49B B47B F51B 109.7(9) . . ?
F51B B47B F50B 105.1(9) . . ?

####################################################################### 
# 
# 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_h2o260c
_database_code_depnum_ccdc_archive 'CCDC 1976622'
_audit_update_record             
;
2020-01-09 deposited with the CCDC.	2020-05-26 downloaded from the CCDC.
;
_audit_creation_date             2018-06-27
_audit_creation_method           
;
  Olex2 1.2
  (compiled Apr 23 2013 17:54:37, GUI svn.r4466)
;
_chemical_name_common            ?
_chemical_name_systematic        
;
Bis[4-(isopropylsulfanyl)-2,6-di(pyrazol-1-yl)pyridine]iron(II)
ditetrafluoroborate hydrate
;
_chemical_formula_moiety         'C28 H29.55 Fe N10 S2, 2(B F4), H2 O'
_chemical_formula_sum            'C28 H32 B2 F8 Fe N10 O S2'
_chemical_formula_weight         818.23
_chemical_melting_point          ?
loop_
_atom_type_symbol
_atom_type_description
_atom_type_scat_dispersion_real
_atom_type_scat_dispersion_imag
_atom_type_scat_source
B B 0.0090 0.0039 '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'
F F 0.0727 0.0534 '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'

_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_id
_space_group_symop_operation_xyz
1 'x, y, z'
2 '-x, y+1/2, -z+1/2'
3 '-x, -y, -z'
4 'x, -y-1/2, z-1/2'

_cell_length_a                   20.2922(10)
_cell_length_b                   11.6992(6)
_cell_length_c                   15.8171(9)
_cell_angle_alpha                90.00
_cell_angle_beta                 102.687(6)
_cell_angle_gamma                90.00
_cell_volume                     3663.3(3)
_cell_formula_units_Z            4
_cell_measurement_reflns_used    3214
_cell_measurement_temperature    260(2)
_cell_measurement_theta_min      4.47
_cell_measurement_theta_max      72.90
_exptl_absorpt_coefficient_mu    5.086
_exptl_absorpt_correction_T_min  0.631
_exptl_absorpt_correction_T_max  1.000
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   
;
CrysAlisPro 1.171.39.46 (Rigaku Oxford Diffraction, 2018)
Empirical absorption correction using spherical harmonics,
 implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_crystal_colour            yellow
_exptl_crystal_density_diffrn    1.484
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       plate
_exptl_crystal_F_000             1672
_exptl_crystal_size_max          0.35
_exptl_crystal_size_mid          0.30
_exptl_crystal_size_min          0.10
_exptl_special_details           
;
 ? 
;
_diffrn_reflns_av_R_equivalents  0.0391
_diffrn_reflns_av_unetI/netI     0.0503
_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       19
_diffrn_reflns_limit_l_min       -19
_diffrn_reflns_number            14184
_diffrn_reflns_theta_full        72.00
_diffrn_reflns_theta_max         73.40
_diffrn_reflns_theta_min         4.39
_diffrn_ambient_temperature      260(2)
_diffrn_detector_area_resol_mean 5.3095
_diffrn_measured_fraction_theta_full 0.983
_diffrn_measured_fraction_theta_max 0.968
_diffrn_measurement_device_type  'SuperNova, Dual, Cu at zero, Atlas'
_diffrn_measurement_method       'ω scans'
_diffrn_radiation_monochromator  mirror
_diffrn_radiation_type           CuK\a
_diffrn_radiation_wavelength     1.54184
_diffrn_radiation_source         'SuperNova (Cu) X-ray Source'
_diffrn_standards_number         0
_diffrn_standards_interval_count 0
_diffrn_standards_interval_time  0
_diffrn_standards_decay_%        0
_reflns_number_gt                4880
_reflns_number_total             7142
_reflns_threshold_expression     >2sigma(I)
_computing_data_collection       'CrysAlisPro, Agilent Technologies'
_computing_cell_refinement       'CrysAlisPro, Agilent Technologies'
_computing_data_reduction        'CrysAlisPro, Agilent Technologies'
_computing_molecular_graphics    'XSEED (Barbour, 2001)'
_computing_publication_material  
;
O. V. Dolomanov, L. J. Bourhis, R. J. Gildea, J. A. K. Howard and H. Puschmann,
OLEX2: a complete structure solution, refinement and analysis program.
J. Appl. Cryst. (2009). 42, 339-341.
;
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_refine_diff_density_max         0.539
_refine_diff_density_min         -0.982
_refine_diff_density_rms         0.077
_refine_ls_extinction_coef       ?
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.046
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     494
_refine_ls_number_reflns         7142
_refine_ls_number_restraints     68
_refine_ls_R_factor_all          0.1124
_refine_ls_R_factor_gt           0.0809
_refine_ls_restrained_S_all      1.056
_refine_ls_shift/su_max          0.000
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details     
'calc w=1/[σ²(Fo²)+(0.1188P)²+5.2792P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.2177
_refine_ls_wR_factor_ref         0.2423
_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 isopropylsulfanyl substitutents on the complex cation is 
 disordered over three orientations, with occupancies of 0.50, 0.35 and 0.15.
 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. Both BF₄⁻ ions are also disordered, one 
 over two half-occupied sites and the other over three orientations of
 occupancy 0.5, 0.25 and 0;25 which share a common fully occupied B atom. 
 The refined restraints B---F = 1.39(2) and F...F = 2.27(2) Å were applied 
 to those residues. Lastly, the water molecule was also refined over three 
 different sites with a 0.6:0.3:0.1 occupancy ratio.

 All fully occupied non-H 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 could not be located and are not included in
 the model, but are accounted for in the density and F(000) calculations. 
 This disordered water site is positioned to hydrogen bond to anion 
 B42-F46, and to its own symmetry equivalent related by 1-x, 1-y, 1-z.
;
_olex2_refinement_description    
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups
 At 1.5 times of:
  All C(H,H,H) groups
2. Restrained distances
 B42-F43A = B42-F44A = B42-F45A = B42-F46A
 1.38888 with sigma of 0.02
 B42-F43B = B42-F44B = B42-F45B = B42-F46B
 1.38888 with sigma of 0.02
 B42-F43C = B42-F44C = B42-F45C = B42-F46C
 1.38888 with sigma of 0.02
 F43A-F44A = F43A-F45A = F43A-F46A = F44A-F45A = F44A-F46A = F45A-F46A
 2.268041 with sigma of 0.02
 F43B-F44B = F43B-F45B = F43B-F46B = F44B-F45B = F44B-F46B = F45B-F46B
 2.268041 with sigma of 0.02
 F43C-F44C = F43C-F45C = F43C-F46C = F44C-F45C = F44C-F46C = F45C-F46C
 2.268041 with sigma of 0.02
 B47A-F48A = B47A-F49A = B47A-F50A = B47A-F51A
 1.38888 with sigma of 0.02
 B47B-F48B = B47B-F49B = B47B-F50B = B47B-F51B
 1.38888 with sigma of 0.02
 F48A-F49A = F48A-F50A = F48A-F51A = F49A-F50A = F49A-F51A = F50A-F51A
 2.268041 with sigma of 0.02
 F48B-F49B = F48B-F50B = F48B-F51B = F49B-F50B = F49B-F51B = F50B-F51B
 2.268041 with sigma of 0.02
 C25-S38A = C25-S38B = C25-S38C
 1.75 with sigma of 0.02
 S38A-C39A = S38B-C39B = S38C-C39C
 1.82 with sigma of 0.02
 C39A-C40A = C39A-C41A = C39B-C40B = C39B-C41B = C39C-C40C = C39C-C41C
 1.52 with sigma of 0.02
 C40A-C41A = C40B-C41B = C40C-C41C
 2.48 with sigma of 0.02
 C25-C39A = C25-C39B = C25-C39C
 2.83 with sigma of 0.02
3. Others
 1(DFIX)=1(DFIX)=1(DFIX)=1(DFIX)=1(DFIX)=FVAR(1)
 1(DFIX)=1(DFIX)=1(DFIX)=1(DFIX)=1(DFIX)=1.633*FVAR(2)
 Fixed Sof: S38A(0.35) C39A(0.35) H39A(0.35) C40A(0.35) H40A(0.35) H40B(0.35)
 H40C(0.35) C41A(0.35) H41A(0.35) H41B(0.35) H41C(0.35) S38B(0.5) C39B(0.5)
 H39B(0.5) C40B(0.5) H40D(0.5) H40E(0.5) H40F(0.5) C41B(0.5) H41D(0.5)
 H41E(0.5) H41F(0.5) S38C(0.15) C39C(0.15) H39C(0.15) C40C(0.15) H40G(0.15)
 H40H(0.15) H40I(0.15) C41C(0.15) H41G(0.15) H41H(0.15) H41I(0.15) F43A(0.5)
 F44A(0.5) F45A(0.5) F46A(0.5) F43B(0.25) F44B(0.25) F45B(0.25) F46B(0.25)
 F43C(0.25) F44C(0.25) F45C(0.25) F46C(0.25) B47A(0.5) F48A(0.5) F49A(0.5)
 F50A(0.5) F51A(0.5) B47B(0.5) F48B(0.5) F49B(0.5) F50B(0.5) F51B(0.5)
 O52A(0.6) O52B(0.3) O52C(0.1)
4.a Ternary CH refined with riding coordinates:
 C19(H19), C39A(H39A), C39B(H39B), C39C(H39C)
4.b Me refined with riding coordinates:
 C40A(H40A,H40B,H40C), C41A(H41A,H41B,H41C), C40B(H40D,H40E,H40F), C41B(H41D,
 H41E,H41F), C40C(H40G,H40H,H40I), C41C(H41G,H41H,H41I)
4.c Aromatic/amide H refined with riding coordinates:
 C4(H4), C6(H6), C10(H10), C11(H11), C12(H12), C15(H15), C16(H16), C17(H17),
 C24(H24), C26(H26), C30(H30), C31(H31), C32(H32), C35(H35), C36(H36), C37(H37)
4.d Idealised Me refined as rotating group:
 C20(H20A,H20B,H20C), C21(H21A,H21B,H21C)
;
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_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_symmetry_multiplicity
_atom_site_calc_flag
_atom_site_refinement_flags
_atom_site_disorder_assembly
_atom_site_disorder_group
Fe1 Fe 0.22981(4) 0.60411(7) 0.06918(6) 0.0479(3) Uani 1 1 d . A .
N2 N 0.1231(2) 0.6250(4) 0.0423(3) 0.0453(9) Uani 1 1 d . . .
C3 C 0.0932(2) 0.7024(4) -0.0160(3) 0.0447(11) Uani 1 1 d . . .
C4 C 0.0264(2) 0.7313(5) -0.0282(4) 0.0496(12) Uani 1 1 d . . .
H4 H 0.0068 0.7849 -0.0706 0.060 Uiso 1 1 calc R . .
C5 C -0.0115(3) 0.6785(5) 0.0241(4) 0.0532(12) Uani 1 1 d . . .
C6 C 0.0194(3) 0.5985(5) 0.0865(4) 0.0535(13) Uani 1 1 d . . .
H6 H -0.0048 0.5629 0.1236 0.064 Uiso 1 1 calc R . .
C7 C 0.0855(2) 0.5743(4) 0.0911(3) 0.0474(11) Uani 1 1 d . . .
N8 N 0.1382(2) 0.7525(4) -0.0610(3) 0.0474(10) Uani 1 1 d . . .
N9 N 0.2058(2) 0.7311(4) -0.0318(3) 0.0541(11) Uani 1 1 d . . .
C10 C 0.2358(3) 0.7947(6) -0.0811(5) 0.0702(17) Uani 1 1 d . . .
H10 H 0.2828 0.7977 -0.0760 0.084 Uiso 1 1 calc R . .
C11 C 0.1891(3) 0.8572(6) -0.1418(5) 0.0716(18) Uani 1 1 d . . .
H11 H 0.1981 0.9087 -0.1834 0.086 Uiso 1 1 calc R . .
C12 C 0.1268(3) 0.8268(5) -0.1272(4) 0.0630(15) Uani 1 1 d . . .
H12 H 0.0845 0.8530 -0.1578 0.076 Uiso 1 1 calc R . .
N13 N 0.1231(2) 0.4947(4) 0.1510(3) 0.0507(10) Uani 1 1 d . . .
N14 N 0.1907(2) 0.4868(4) 0.1566(3) 0.0526(10) Uani 1 1 d . . .
C15 C 0.2113(3) 0.4041(5) 0.2131(4) 0.0631(15) Uani 1 1 d . . .
H15 H 0.2562 0.3790 0.2305 0.076 Uiso 1 1 calc R . .
C16 C 0.1567(4) 0.3586(6) 0.2436(5) 0.0755(18) Uani 1 1 d . . .
H16 H 0.1582 0.2999 0.2846 0.091 Uiso 1 1 calc R . .
C17 C 0.1012(3) 0.4170(5) 0.2018(4) 0.0622(15) Uani 1 1 d . . .
H17 H 0.0564 0.4057 0.2071 0.075 Uiso 1 1 calc R . .
S18 S -0.09750(6) 0.70325(14) 0.01905(12) 0.0651(4) Uani 1 1 d . . .
C19 C -0.1162(3) 0.8381(5) -0.0375(4) 0.0620(15) Uani 1 1 d . . .
H19 H -0.1001 0.8349 -0.0922 0.074 Uiso 1 1 calc R . .
C20 C -0.0825(4) 0.9361(6) 0.0160(5) 0.082(2) Uani 1 1 d . . .
H20A H -0.0883 1.0051 -0.0189 0.123 Uiso 1 1 calc R . .
H20B H -0.0347 0.9200 0.0359 0.123 Uiso 1 1 calc R . .
H20C H -0.1028 0.9468 0.0656 0.123 Uiso 1 1 calc R . .
C21 C -0.1929(3) 0.8501(8) -0.0588(6) 0.092(2) Uani 1 1 d . . .
H21A H -0.2094 0.8464 -0.0058 0.137 Uiso 1 1 calc R . .
H21B H -0.2128 0.7886 -0.0972 0.137 Uiso 1 1 calc R . .
H21C H -0.2054 0.9230 -0.0871 0.137 Uiso 1 1 calc R . .
N22 N 0.3334(2) 0.5852(4) 0.1229(3) 0.0476(10) Uani 1 1 d . A .
C23 C 0.3702(3) 0.5087(5) 0.0905(4) 0.0511(12) Uani 1 1 d . . .
C24 C 0.4374(3) 0.4888(6) 0.1252(4) 0.0663(16) Uani 1 1 d . A .
H24 H 0.4620 0.4356 0.1000 0.080 Uiso 1 1 calc R . .
C25 C 0.4679(3) 0.5497(7) 0.1987(5) 0.077(2) Uani 1 1 d D . .
C26 C 0.4304(3) 0.6346(6) 0.2321(4) 0.0667(17) Uani 1 1 d . A .
H26 H 0.4501 0.6799 0.2802 0.080 Uiso 1 1 calc R . .
C27 C 0.3637(3) 0.6472(5) 0.1904(4) 0.0521(12) Uani 1 1 d . . .
N28 N 0.3331(2) 0.4499(4) 0.0184(3) 0.0503(10) Uani 1 1 d . . .
N29 N 0.2658(2) 0.4744(4) -0.0086(3) 0.0513(10) Uani 1 1 d . . .
C30 C 0.2449(3) 0.4089(5) -0.0771(4) 0.0583(14) Uani 1 1 d . . .
H30 H 0.2003 0.4077 -0.1100 0.070 Uiso 1 1 calc R . .
C31 C 0.2975(3) 0.3412(6) -0.0948(4) 0.0676(16) Uani 1 1 d . . .
H31 H 0.2949 0.2874 -0.1396 0.081 Uiso 1 1 calc R . .
C32 C 0.3524(3) 0.3702(6) -0.0336(4) 0.0655(16) Uani 1 1 d . . .
H32 H 0.3962 0.3406 -0.0281 0.079 Uiso 1 1 calc R . .
N33 N 0.3205(2) 0.7281(4) 0.2144(3) 0.0533(11) Uani 1 1 d . A .
N34 N 0.2558(2) 0.7346(4) 0.1680(3) 0.0571(11) Uani 1 1 d . . .
C35 C 0.2287(3) 0.8238(5) 0.2011(5) 0.0687(17) Uani 1 1 d . A .
H35 H 0.1839 0.8491 0.1817 0.082 Uiso 1 1 calc R . .
C36 C 0.2757(4) 0.8739(6) 0.2678(5) 0.080(2) Uani 1 1 d . . .
H36 H 0.2686 0.9377 0.3009 0.096 Uiso 1 1 calc R A .
C37 C 0.3337(3) 0.8137(6) 0.2764(5) 0.0696(17) Uani 1 1 d . A .
H37 H 0.3747 0.8271 0.3163 0.083 Uiso 1 1 calc R . .
S38A S 0.5456(2) 0.4863(4) 0.2602(3) 0.0521(10) Uiso 0.35 1 d PD A 1
C39A C 0.5775(10) 0.5827(17) 0.3469(13) 0.063(8) Uiso 0.35 1 d PD A 1
H39A H 0.5449 0.5918 0.3846 0.076 Uiso 0.35 1 calc PR A 1
C40A C 0.6011(12) 0.7005(16) 0.3208(16) 0.069(5) Uiso 0.35 1 d PD A 1
H40A H 0.5620 0.7473 0.2969 0.103 Uiso 0.35 1 calc PR A 1
H40B H 0.6280 0.6903 0.2776 0.103 Uiso 0.35 1 calc PR A 1
H40C H 0.6281 0.7379 0.3714 0.103 Uiso 0.35 1 calc PR A 1
C41A C 0.6378(9) 0.5119(17) 0.3920(13) 0.059(5) Uiso 0.35 1 d PD A 1
H41A H 0.6224 0.4377 0.4070 0.089 Uiso 0.35 1 calc PR A 1
H41B H 0.6609 0.5508 0.4443 0.089 Uiso 0.35 1 calc PR A 1
H41C H 0.6686 0.5021 0.3536 0.089 Uiso 0.35 1 calc PR A 1
S38B S 0.55364(17) 0.5182(4) 0.2347(2) 0.0622(8) Uiso 0.50 1 d PD A 2
C39B C 0.5799(8) 0.6008(17) 0.3341(10) 0.067(6) Uiso 0.50 1 d PD A 2
H39B H 0.5401 0.6240 0.3566 0.081 Uiso 0.50 1 calc PR A 2
C40B C 0.6086(17) 0.703(2) 0.2947(19) 0.159(13) Uiso 0.50 1 d PD A 2
H40D H 0.5737 0.7366 0.2498 0.238 Uiso 0.50 1 calc PR A 2
H40E H 0.6458 0.6779 0.2697 0.238 Uiso 0.50 1 calc PR A 2
H40F H 0.6248 0.7593 0.3394 0.238 Uiso 0.50 1 calc PR A 2
C41B C 0.6326(10) 0.5457(17) 0.4050(12) 0.092(6) Uiso 0.50 1 d PD A 2
H41D H 0.6155 0.4735 0.4214 0.138 Uiso 0.50 1 calc PR A 2
H41E H 0.6427 0.5959 0.4549 0.138 Uiso 0.50 1 calc PR A 2
H41F H 0.6734 0.5323 0.3840 0.138 Uiso 0.50 1 calc PR A 2
S38C S 0.5566(4) 0.5787(8) 0.2116(5) 0.0439(17) Uiso 0.15 1 d PD A 3
C39C C 0.5781(13) 0.646(3) 0.3182(16) 0.053(10) Uiso 0.15 1 d PD A 3
H39C H 0.5464 0.7088 0.3222 0.064 Uiso 0.15 1 calc PR A 3
C40C C 0.572(3) 0.552(4) 0.382(4) 0.097(18) Uiso 0.15 1 d PD A 3
H40G H 0.5253 0.5316 0.3761 0.145 Uiso 0.15 1 calc PR A 3
H40H H 0.5909 0.5784 0.4403 0.145 Uiso 0.15 1 calc PR A 3
H40I H 0.5975 0.4855 0.3699 0.145 Uiso 0.15 1 calc PR A 3
C41C C 0.6489(18) 0.690(4) 0.330(4) 0.087(15) Uiso 0.15 1 d PD A 3
H41G H 0.6800 0.6371 0.3650 0.131 Uiso 0.15 1 calc PR A 3
H41H H 0.6523 0.7641 0.3578 0.131 Uiso 0.15 1 calc PR A 3
H41I H 0.6601 0.6976 0.2733 0.131 Uiso 0.15 1 calc PR A 3
B42 B 0.4497(4) 0.7289(8) 0.4859(5) 0.090(3) Uani 1 1 d D . .
F43A F 0.5024(6) 0.7298(13) 0.5624(7) 0.130(4) Uiso 0.50 1 d PD B 1
F44A F 0.4740(5) 0.7874(9) 0.4223(6) 0.084(3) Uiso 0.50 1 d PD B 1
F45A F 0.3933(5) 0.7656(10) 0.5035(8) 0.096(3) Uiso 0.50 1 d PD B 1
F46A F 0.4438(8) 0.6145(9) 0.4564(9) 0.135(5) Uiso 0.50 1 d PD B 1
F43B F 0.5089(10) 0.681(2) 0.5345(16) 0.159(12) Uiso 0.25 1 d PD B 2
F44B F 0.4613(11) 0.8356(15) 0.4536(14) 0.123(8) Uiso 0.25 1 d PD B 2
F45B F 0.4055(9) 0.7384(16) 0.5392(12) 0.086(5) Uiso 0.25 1 d PD B 2
F46B F 0.4212(14) 0.656(2) 0.4169(13) 0.131(11) Uiso 0.25 1 d PD B 2
F43C F 0.4964(8) 0.7667(16) 0.4453(12) 0.087(6) Uiso 0.25 1 d PD B 3
F44C F 0.4716(14) 0.701(2) 0.5700(10) 0.158(12) Uiso 0.25 1 d PD B 3
F45C F 0.3977(9) 0.8192(16) 0.4777(14) 0.113(7) Uiso 0.25 1 d PD B 3
F46C F 0.4118(9) 0.6377(14) 0.4381(13) 0.077(5) Uiso 0.25 1 d PD B 3
B47A B 0.0741(8) 0.9828(15) 0.2334(10) 0.071(10) Uiso 0.50 1 d PD C 1
F48A F 0.1350(5) 1.0423(9) 0.2309(7) 0.082(3) Uiso 0.50 1 d PD C 1
F49A F 0.0166(5) 1.0504(9) 0.2026(7) 0.083(3) Uiso 0.50 1 d PD C 1
F50A F 0.0803(4) 0.9593(8) 0.3201(5) 0.076(2) Uiso 0.50 1 d PD C 1
F51A F 0.0696(5) 0.8898(8) 0.1803(6) 0.088(3) Uiso 0.50 1 d PD C 1
B47B B 0.0752(7) 0.9988(14) 0.2318(9) 0.054(7) Uiso 0.50 1 d PD D 2
F48B F 0.1354(6) 1.0533(12) 0.2555(9) 0.119(6) Uiso 0.50 1 d PD D 2
F49B F 0.0279(5) 1.0849(9) 0.2072(7) 0.087(3) Uiso 0.50 1 d PD D 2
F50B F 0.0584(5) 0.9287(8) 0.2955(6) 0.087(3) Uiso 0.50 1 d PD D 2
F51B F 0.0774(5) 0.9272(9) 0.1609(6) 0.089(3) Uiso 0.50 1 d PD D 2
O52A O 0.6212(8) 0.5913(13) 0.6488(10) 0.109(4) Uiso 0.60 1 d P E 1
O52B O 0.6296(18) 0.575(3) 0.621(2) 0.137(13) Uiso 0.30 1 d P F 2
O52C O 0.577(5) 0.632(8) 0.642(6) 0.15(3) Uiso 0.10 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 N2 2.126(4) . ?
Fe1 N9 2.157(5) . ?
Fe1 N14 2.215(5) . ?
Fe1 N22 2.099(4) . ?
Fe1 N29 2.178(5) . ?
Fe1 N34 2.165(5) . ?
N2 C3 1.339(6) . ?
N2 C7 1.338(6) . ?
C3 C4 1.369(7) . ?
C3 N8 1.404(6) . ?
C4 H4 0.9400 . ?
C4 C5 1.392(7) . ?
C5 C6 1.404(8) . ?
C5 S18 1.753(5) . ?
C6 H6 0.9400 . ?
C6 C7 1.357(7) . ?
C7 N13 1.425(7) . ?
N8 N9 1.371(6) . ?
N8 C12 1.341(7) . ?
N9 C10 1.319(7) . ?
C10 H10 0.9400 . ?
C10 C11 1.398(9) . ?
C11 H11 0.9400 . ?
C11 C12 1.380(9) . ?
C12 H12 0.9400 . ?
N13 N14 1.358(6) . ?
N13 C17 1.351(7) . ?
N14 C15 1.321(7) . ?
C15 H15 0.9400 . ?
C15 C16 1.406(9) . ?
C16 H16 0.9400 . ?
C16 C17 1.358(9) . ?
C17 H17 0.9400 . ?
S18 C19 1.812(6) . ?
C19 H19 0.9900 . ?
C19 C20 1.497(10) . ?
C19 C21 1.526(8) . ?
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 1.336(6) . ?
N22 C27 1.325(7) . ?
C23 C24 1.374(7) . ?
C23 N28 1.402(7) . ?
C24 H24 0.9400 . ?
C24 C25 1.388(9) . ?
C25 C26 1.423(8) . ?
C25 S38A 1.819(7) . ?
C25 S38B 1.746(6) . ?
C25 S38C 1.798(9) . ?
C26 H26 0.9400 . ?
C26 C27 1.377(8) . ?
C27 N33 1.398(7) . ?
N28 N29 1.369(6) . ?
N28 C32 1.357(7) . ?
N29 C30 1.318(7) . ?
C30 H30 0.9400 . ?
C30 C31 1.406(9) . ?
C31 H31 0.9400 . ?
C31 C32 1.349(9) . ?
C32 H32 0.9400 . ?
N33 N34 1.359(6) . ?
N33 C37 1.385(8) . ?
N34 C35 1.339(7) . ?
C35 H35 0.9400 . ?
C35 C36 1.388(10) . ?
C36 H36 0.9400 . ?
C36 C37 1.353(9) . ?
C37 H37 0.9400 . ?
S38A C39A 1.784(14) . ?
C39A H39A 0.9900 . ?
C39A C40A 1.545(18) . ?
C39A C41A 1.518(16) . ?
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 1.823(12) . ?
C39B H39B 0.9900 . ?
C39B C40B 1.522(17) . ?
C39B C41B 1.514(15) . ?
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 1.824(17) . ?
C39C H39C 0.9900 . ?
C39C C40C 1.51(2) . ?
C39C C41C 1.500(19) . ?
C40C H40G 0.9700 . ?
C40C H40H 0.9700 . ?
C40C H40I 0.9700 . ?
C41C H41G 0.9700 . ?
C41C H41H 0.9700 . ?
C41C H41I 0.9700 . ?
B42 F43A 1.427(12) . ?
B42 F44A 1.393(10) . ?
B42 F45A 1.308(11) . ?
B42 F46A 1.414(12) . ?
B42 F43B 1.392(15) . ?
B42 F44B 1.389(14) . ?
B42 F45B 1.364(13) . ?
B42 F46B 1.404(14) . ?
B42 F43C 1.332(13) . ?
B42 F44C 1.345(14) . ?
B42 F45C 1.478(14) . ?
B42 F46C 1.431(13) . ?
B47A F48A 1.426(16) . ?
B47A F49A 1.405(15) . ?
B47A F50A 1.377(15) . ?
B47A F51A 1.364(15) . ?
B47B F48B 1.355(14) . ?
B47B F49B 1.387(14) . ?
B47B F50B 1.399(15) . ?
B47B F51B 1.409(14) . ?

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 N9 73.67(16) . . ?
N2 Fe1 N14 72.99(16) . . ?
N2 Fe1 N29 114.81(16) . . ?
N2 Fe1 N34 98.01(16) . . ?
N9 Fe1 N14 146.66(16) . . ?
N9 Fe1 N29 96.37(17) . . ?
N9 Fe1 N34 91.64(19) . . ?
N22 Fe1 N2 168.01(17) . . ?
N22 Fe1 N9 114.52(17) . . ?
N22 Fe1 N14 98.42(17) . . ?
N22 Fe1 N29 74.03(17) . . ?
N22 Fe1 N34 73.67(17) . . ?
N29 Fe1 N14 97.54(17) . . ?
N34 Fe1 N14 92.85(18) . . ?
N34 Fe1 N29 147.17(16) . . ?
C3 N2 Fe1 120.2(3) . . ?
C7 N2 Fe1 121.3(3) . . ?
C7 N2 C3 117.8(4) . . ?
N2 C3 C4 123.4(5) . . ?
N2 C3 N8 112.6(4) . . ?
C4 C3 N8 124.0(5) . . ?
C3 C4 H4 121.1 . . ?
C3 C4 C5 117.8(5) . . ?
C5 C4 H4 121.1 . . ?
C4 C5 C6 119.6(5) . . ?
C4 C5 S18 125.1(4) . . ?
C6 C5 S18 115.4(4) . . ?
C5 C6 H6 121.3 . . ?
C7 C6 C5 117.4(5) . . ?
C7 C6 H6 121.3 . . ?
N2 C7 C6 124.1(5) . . ?
N2 C7 N13 112.5(4) . . ?
C6 C7 N13 123.4(5) . . ?
N9 N8 C3 117.9(4) . . ?
C12 N8 C3 130.3(5) . . ?
C12 N8 N9 111.7(4) . . ?
N8 N9 Fe1 114.9(3) . . ?
C10 N9 Fe1 140.2(4) . . ?
C10 N9 N8 104.7(5) . . ?
N9 C10 H10 124.1 . . ?
N9 C10 C11 111.8(5) . . ?
C11 C10 H10 124.1 . . ?
C10 C11 H11 127.6 . . ?
C12 C11 C10 104.9(5) . . ?
C12 C11 H11 127.6 . . ?
N8 C12 C11 106.9(5) . . ?
N8 C12 H12 126.6 . . ?
C11 C12 H12 126.6 . . ?
N14 N13 C7 118.3(4) . . ?
C17 N13 C7 129.6(5) . . ?
C17 N13 N14 112.0(5) . . ?
N13 N14 Fe1 114.3(3) . . ?
C15 N14 Fe1 140.6(4) . . ?
C15 N14 N13 105.0(5) . . ?
N14 C15 H15 124.6 . . ?
N14 C15 C16 110.7(6) . . ?
C16 C15 H15 124.6 . . ?
C15 C16 H16 127.1 . . ?
C17 C16 C15 105.9(6) . . ?
C17 C16 H16 127.1 . . ?
N13 C17 C16 106.4(5) . . ?
N13 C17 H17 126.8 . . ?
C16 C17 H17 126.8 . . ?
C5 S18 C19 105.3(3) . . ?
S18 C19 H19 109.0 . . ?
C20 C19 S18 111.6(5) . . ?
C20 C19 H19 109.0 . . ?
C20 C19 C21 111.8(6) . . ?
C21 C19 S18 106.4(5) . . ?
C21 C19 H19 109.0 . . ?
C19 C20 H20A 109.5 . . ?
C19 C20 H20B 109.5 . . ?
C19 C20 H20C 109.5 . . ?
H20A C20 H20B 109.5 . . ?
H20A C20 H20C 109.5 . . ?
H20B C20 H20C 109.5 . . ?
C19 C21 H21A 109.5 . . ?
C19 C21 H21B 109.5 . . ?
C19 C21 H21C 109.5 . . ?
H21A C21 H21B 109.5 . . ?
H21A C21 H21C 109.5 . . ?
H21B C21 H21C 109.5 . . ?
C23 N22 Fe1 120.6(4) . . ?
C27 N22 Fe1 120.9(3) . . ?
C27 N22 C23 118.4(4) . . ?
N22 C23 C24 123.3(5) . . ?
N22 C23 N28 113.3(4) . . ?
C24 C23 N28 123.4(5) . . ?
C23 C24 H24 121.0 . . ?
C23 C24 C25 118.0(5) . . ?
C25 C24 H24 121.0 . . ?
C24 C25 C26 119.5(5) . . ?
C24 C25 S38A 114.4(5) . . ?
C24 C25 S38B 113.2(5) . . ?
C24 C25 S38C 116.3(5) . . ?
C26 C25 S38A 123.9(5) . . ?
C26 C25 S38B 127.1(5) . . ?
C26 C25 S38C 115.5(6) . . ?
C25 C26 H26 121.7 . . ?
C27 C26 C25 116.5(5) . . ?
C27 C26 H26 121.7 . . ?
N22 C27 C26 124.1(5) . . ?
N22 C27 N33 112.5(5) . . ?
C26 C27 N33 123.4(5) . . ?
N29 N28 C23 118.2(4) . . ?
C32 N28 C23 131.0(5) . . ?
C32 N28 N29 110.9(5) . . ?
N28 N29 Fe1 113.9(3) . . ?
C30 N29 Fe1 141.4(4) . . ?
C30 N29 N28 104.7(4) . . ?
N29 C30 H30 124.1 . . ?
N29 C30 C31 111.8(5) . . ?
C31 C30 H30 124.1 . . ?
C30 C31 H31 127.5 . . ?
C32 C31 C30 105.0(5) . . ?
C32 C31 H31 127.5 . . ?
N28 C32 H32 126.1 . . ?
C31 C32 N28 107.8(5) . . ?
C31 C32 H32 126.1 . . ?
N34 N33 C27 118.7(4) . . ?
N34 N33 C37 110.8(5) . . ?
C37 N33 C27 130.2(5) . . ?
N33 N34 Fe1 113.8(3) . . ?
C35 N34 Fe1 140.9(5) . . ?
C35 N34 N33 105.3(5) . . ?
N34 C35 H35 124.6 . . ?
N34 C35 C36 110.7(6) . . ?
C36 C35 H35 124.6 . . ?
C35 C36 H36 126.5 . . ?
C37 C36 C35 107.1(6) . . ?
C37 C36 H36 126.5 . . ?
N33 C37 H37 127.0 . . ?
C36 C37 N33 106.1(6) . . ?
C36 C37 H37 127.0 . . ?
C39A S38A C25 106.2(7) . . ?
S38A C39A H39A 110.6 . . ?
C40A C39A S38A 116.1(17) . . ?
C40A C39A H39A 110.6 . . ?
C41A C39A S38A 97.8(13) . . ?
C41A C39A H39A 110.6 . . ?
C41A C39A C40A 110.3(14) . . ?
C39A C40A H40A 109.5 . . ?
C39A C40A H40B 109.5 . . ?
C39A C40A H40C 109.5 . . ?
H40A C40A H40B 109.5 . . ?
H40A C40A H40C 109.5 . . ?
H40B C40A H40C 109.5 . . ?
C39A C41A H41A 109.5 . . ?
C39A C41A H41B 109.5 . . ?
C39A C41A H41C 109.5 . . ?
H41A C41A H41B 109.5 . . ?
H41A C41A H41C 109.5 . . ?
H41B C41A H41C 109.5 . . ?
C25 S38B C39B 104.5(6) . . ?
S38B C39B H39B 110.5 . . ?
C40B C39B S38B 97.4(16) . . ?
C40B C39B H39B 110.5 . . ?
C41B C39B S38B 116.0(14) . . ?
C41B C39B H39B 110.5 . . ?
C41B C39B C40B 111.4(14) . . ?
C39B C40B H40D 109.5 . . ?
C39B C40B H40E 109.5 . . ?
C39B C40B H40F 109.5 . . ?
H40D C40B H40E 109.5 . . ?
H40D C40B H40F 109.5 . . ?
H40E C40B H40F 109.5 . . ?
C39B C41B H41D 109.5 . . ?
C39B C41B H41E 109.5 . . ?
C39B C41B H41F 109.5 . . ?
H41D C41B H41E 109.5 . . ?
H41D C41B H41F 109.5 . . ?
H41E C41B H41F 109.5 . . ?
C25 S38C C39C 102.5(9) . . ?
S38C C39C H39C 110.7 . . ?
C40C C39C S38C 105(3) . . ?
C40C C39C H39C 110.7 . . ?
C41C C39C S38C 107(3) . . ?
C41C C39C H39C 110.7 . . ?
C41C C39C C40C 112.4(19) . . ?
C39C C40C H40G 109.5 . . ?
C39C C40C H40H 109.5 . . ?
C39C C40C H40I 109.5 . . ?
H40G C40C H40H 109.5 . . ?
H40G C40C H40I 109.5 . . ?
H40H C40C H40I 109.5 . . ?
C39C C41C H41G 109.5 . . ?
C39C C41C H41H 109.5 . . ?
C39C C41C H41I 109.5 . . ?
H41G C41C H41H 109.5 . . ?
H41G C41C H41I 109.5 . . ?
H41H C41C H41I 109.5 . . ?
F44A B42 F43A 106.8(9) . . ?
F44A B42 F46A 104.2(8) . . ?
F45A B42 F43A 110.2(9) . . ?
F45A B42 F44A 117.1(9) . . ?
F45A B42 F46A 111.4(9) . . ?
F46A B42 F43A 106.3(10) . . ?
F43B B42 F46B 110.2(13) . . ?
F44B B42 F43B 111.6(13) . . ?
F44B B42 F46B 109.4(13) . . ?
F45B B42 F43B 107.3(12) . . ?
F45B B42 F44B 110.0(12) . . ?
F45B B42 F46B 108.4(12) . . ?
F43C B42 F44C 116.3(13) . . ?
F43C B42 F45C 106.8(11) . . ?
F43C B42 F46C 110.4(11) . . ?
F44C B42 F45C 109.5(13) . . ?
F44C B42 F46C 111.4(13) . . ?
F46C B42 F45C 101.3(11) . . ?
F49A B47A F48A 112.0(13) . . ?
F50A B47A F48A 103.6(11) . . ?
F50A B47A F49A 110.1(12) . . ?
F51A B47A F48A 108.3(12) . . ?
F51A B47A F49A 107.3(12) . . ?
F51A B47A F50A 115.6(13) . . ?
F48B B47B F49B 105.2(13) . . ?
F48B B47B F50B 115.1(12) . . ?
F48B B47B F51B 108.4(11) . . ?
F49B B47B F50B 111.4(11) . . ?
F49B B47B F51B 110.4(11) . . ?
F50B B47B F51B 106.3(12) . . ?

####################################################################### 
# 
# 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_h2o230
_database_code_depnum_ccdc_archive 'CCDC 1976625'
_audit_update_record             
;
2020-01-09 deposited with the CCDC.	2020-05-26 downloaded from the CCDC.
;
_audit_creation_date             2018-06-27
_audit_creation_method           
;
  Olex2 1.2
  (compiled Apr 23 2013 17:54:37, GUI svn.r4466)
;
_chemical_name_common            ?
_chemical_name_systematic        
;
Bis[4-(isopropylsulfanyl)-2,6-di(pyrazol-1-yl)pyridine]iron(II)
ditetrafluoroborate hydrate
;
_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         818.23
_chemical_melting_point          ?
loop_
_atom_type_symbol
_atom_type_description
_atom_type_scat_dispersion_real
_atom_type_scat_dispersion_imag
_atom_type_scat_source
B B 0.0090 0.0039 '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'
F F 0.0727 0.0534 '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'

_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_id
_space_group_symop_operation_xyz
1 'x, y, z'
2 '-x, y+1/2, -z+1/2'
3 '-x, -y, -z'
4 'x, -y-1/2, z-1/2'

_cell_length_a                   20.2949(7)
_cell_length_b                   11.7133(5)
_cell_length_c                   15.7287(7)
_cell_angle_alpha                90.00
_cell_angle_beta                 102.837(4)
_cell_angle_gamma                90.00
_cell_volume                     3645.6(3)
_cell_formula_units_Z            4
_cell_measurement_reflns_used    4423
_cell_measurement_temperature    230(2)
_cell_measurement_theta_min      4.45
_cell_measurement_theta_max      71.62
_exptl_absorpt_coefficient_mu    5.111
_exptl_absorpt_correction_T_min  0.448
_exptl_absorpt_correction_T_max  1.000
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   
;
CrysAlisPro 1.171.39.46 (Rigaku Oxford Diffraction, 2018)
Empirical absorption correction using spherical harmonics,
 implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_crystal_colour            yellow
_exptl_crystal_density_diffrn    1.491
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       plate
_exptl_crystal_F_000             1672
_exptl_crystal_size_max          0.35
_exptl_crystal_size_mid          0.30
_exptl_crystal_size_min          0.10
_exptl_special_details           
;
 ? 
;
_diffrn_reflns_av_R_equivalents  0.0270
_diffrn_reflns_av_unetI/netI     0.0371
_diffrn_reflns_limit_h_max       24
_diffrn_reflns_limit_h_min       -24
_diffrn_reflns_limit_k_max       14
_diffrn_reflns_limit_k_min       -10
_diffrn_reflns_limit_l_max       18
_diffrn_reflns_limit_l_min       -19
_diffrn_reflns_number            13921
_diffrn_reflns_theta_full        72.00
_diffrn_reflns_theta_max         73.58
_diffrn_reflns_theta_min         4.39
_diffrn_ambient_temperature      230(2)
_diffrn_detector_area_resol_mean 5.3095
_diffrn_measured_fraction_theta_full 0.984
_diffrn_measured_fraction_theta_max 0.969
_diffrn_measurement_device_type  'SuperNova, Dual, Cu at zero, Atlas'
_diffrn_measurement_method       'ω scans'
_diffrn_radiation_monochromator  mirror
_diffrn_radiation_type           CuK\a
_diffrn_radiation_wavelength     1.54184
_diffrn_radiation_source         'SuperNova (Cu) X-ray Source'
_diffrn_standards_number         0
_diffrn_standards_interval_count 0
_diffrn_standards_interval_time  0
_diffrn_standards_decay_%        0
_reflns_number_gt                5510
_reflns_number_total             7128
_reflns_threshold_expression     >2sigma(I)
_computing_data_collection       'CrysAlisPro, Agilent Technologies'
_computing_cell_refinement       'CrysAlisPro, Agilent Technologies'
_computing_data_reduction        'CrysAlisPro, Agilent Technologies'
_computing_molecular_graphics    'XSEED (Barbour, 2001)'
_computing_publication_material  
;
O. V. Dolomanov, L. J. Bourhis, R. J. Gildea, J. A. K. Howard and H. Puschmann,
OLEX2: a complete structure solution, refinement and analysis program.
J. Appl. Cryst. (2009). 42, 339-341.
;
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_refine_diff_density_max         0.734
_refine_diff_density_min         -1.152
_refine_diff_density_rms         0.084
_refine_ls_extinction_coef       ?
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.042
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     494
_refine_ls_number_reflns         7128
_refine_ls_number_restraints     70
_refine_ls_R_factor_all          0.0990
_refine_ls_R_factor_gt           0.0804
_refine_ls_restrained_S_all      1.055
_refine_ls_shift/su_max          0.000
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details     
'calc w=1/[σ²(Fo²)+(0.1240P)²+7.1296P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.2245
_refine_ls_wR_factor_ref         0.2404
_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 isopropylsulfanyl substitutents on the complex cation is 
 disordered over three orientations, with occupancies of 0.5, 0.4 and 0.1. 
 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. SIMU displacement ellipsoid restraints were
 also applied to the 0.1-occupied isopropyl disorder site. Both BF₄⁻ 
 ions are also disordered, one over two half-occupied sites and the other 
 over three orientations of occupancy 0.55, 0.30 and 0.15 which share a 
 common fully occupied B atom. The refined restraints B---F = 1.39(2) and 
 F...F = 2.27(2) Å were applied to those residues. Lastly, the water 
 molecule was also refined over three different sites with a 0.6:0.3:0.1 
 occupancy ratio.

 All fully occupied non-H 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 could not be located and are not included in
 the model, but are accounted for in the density and F(000) calculations. 
 This disordered water site is positioned to hydrogen bond to anion 
 B42-F46, and to its own symmetry equivalent related by 1-x, 1-y, 1-z.

 The deepest residual Fourier peak of -1.1 e.Å⁻³ is associated with the 
 disordered S atom S38.
;
_olex2_refinement_description    
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups
 At 1.5 times of:
  All C(H,H,H) groups
2. Restrained distances
 B42-F43A = B42-F44A = B42-F45A = B42-F46A
 1.39248 with sigma of 0.02
 B42-F43B = B42-F44B = B42-F45B = B42-F46B
 1.39248 with sigma of 0.02
 B42-F43C = B42-F44C = B42-F45C = B42-F46C
 1.39248 with sigma of 0.02
 F43A-F44A = F43A-F45A = F43A-F46A = F44A-F45A = F44A-F46A = F45A-F46A
 2.27392 with sigma of 0.02
 F43B-F44B = F43B-F45B = F43B-F46B = F44B-F45B = F44B-F46B = F45B-F46B
 2.27392 with sigma of 0.02
 F43C-F44C = F43C-F45C = F43C-F46C = F44C-F45C = F44C-F46C = F45C-F46C
 2.27392 with sigma of 0.02
 B47A-F48A = B47A-F49A = B47A-F50A = B47A-F51A
 1.39248 with sigma of 0.02
 B47B-F48B = B47B-F49B = B47B-F50B = B47B-F51B
 1.39248 with sigma of 0.02
 F48A-F49A = F48A-F50A = F48A-F51A = F49A-F50A = F49A-F51A = F50A-F51A
 2.27392 with sigma of 0.02
 F48B-F49B = F48B-F50B = F48B-F51B = F49B-F50B = F49B-F51B = F50B-F51B
 2.27392 with sigma of 0.02
 C25-S38A = C25-S38B = C25-S38C
 1.75 with sigma of 0.02
 S38A-C39A = S38B-C39B = S38C-C39C
 1.82 with sigma of 0.02
 C39A-C40A = C39A-C41A = C39B-C40B = C39B-C41B = C39C-C40C = C39C-C41C
 1.52 with sigma of 0.02
 C40A-C41A = C40B-C41B = C40C-C41C
 2.48 with sigma of 0.02
 C25-C39A = C25-C39B = C25-C39C
 2.83 with sigma of 0.02
3. Uiso/Uaniso restraints and constraints
S38C \\sim C39C \\sim C40C \\sim C41C: within 1.7A with sigma of 0.04 and sigma for terminal atoms of 0.08
4. Others
 1(DFIX)=1(DFIX)=1(DFIX)=1(DFIX)=1(DFIX)=FVAR(1)
 1(DFIX)=1(DFIX)=1(DFIX)=1(DFIX)=1(DFIX)=1.633*FVAR(2)
 Fixed Sof: S38A(0.5) C39A(0.5) H39A(0.5) C40A(0.5) H40A(0.5) H40B(0.5)
 H40C(0.5) C41A(0.5) H41A(0.5) H41B(0.5) H41C(0.5) S38B(0.4) C39B(0.4)
 H39B(0.4) C40B(0.4) H40D(0.4) H40E(0.4) H40F(0.4) C41B(0.4) H41D(0.4)
 H41E(0.4) H41F(0.4) S38C(0.1) C40C(0.1) H40G(0.1) H40H(0.1) H40I(0.1)
 C39C(0.1) H39C(0.1) C41C(0.1) H41G(0.1) H41H(0.1) H41I(0.1) F43A(0.55)
 F44A(0.55) F45A(0.55) F46A(0.55) F43B(0.15) F44B(0.15) F45B(0.15) F46B(0.15)
 F43C(0.3) F44C(0.3) F45C(0.3) F46C(0.3) B47A(0.5) F48A(0.5) F49A(0.5)
 F50A(0.5) F51A(0.5) B47B(0.5) F48B(0.5) F49B(0.5) F50B(0.5) F51B(0.5)
 O52A(0.6) O52B(0.3) O52C(0.1)
5.a Ternary CH refined with riding coordinates:
 C19(H19), C39A(H39A), C39B(H39B), C39C(H39C)
5.b Me refined with riding coordinates:
 C40A(H40A,H40B,H40C), C41A(H41A,H41B,H41C), C40B(H40D,H40E,H40F), C41B(H41D,
 H41E,H41F), C40C(H40G,H40H,H40I), C41C(H41G,H41H,H41I)
5.c Aromatic/amide H refined with riding coordinates:
 C4(H4), C6(H6), C10(H10), C11(H11), C12(H12), C15(H15), C16(H16), C17(H17),
 C24(H24), C26(H26), C30(H30), C31(H31), C32(H32), C35(H35), C36(H36), C37(H37)
5.d Idealised Me refined as rotating group:
 C20(H20A,H20B,H20C), C21(H21A,H21B,H21C)
;
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_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_symmetry_multiplicity
_atom_site_calc_flag
_atom_site_refinement_flags
_atom_site_disorder_assembly
_atom_site_disorder_group
Fe1 Fe 0.22994(3) 0.60439(7) 0.07115(5) 0.0427(2) Uani 1 1 d . A .
N2 N 0.12360(19) 0.6258(3) 0.0435(3) 0.0419(8) Uani 1 1 d . . .
C3 C 0.0940(2) 0.7022(4) -0.0144(3) 0.0412(10) Uani 1 1 d . . .
C4 C 0.0266(2) 0.7323(4) -0.0279(3) 0.0457(11) Uani 1 1 d . . .
H4 H 0.0074 0.7865 -0.0703 0.055 Uiso 1 1 calc R . .
C5 C -0.0115(2) 0.6791(5) 0.0241(4) 0.0482(11) Uani 1 1 d . . .
C6 C 0.0190(2) 0.5977(4) 0.0867(4) 0.0493(11) Uani 1 1 d . . .
H6 H -0.0054 0.5611 0.1231 0.059 Uiso 1 1 calc R . .
C7 C 0.0859(2) 0.5745(4) 0.0918(3) 0.0434(10) Uani 1 1 d . . .
N8 N 0.1392(2) 0.7536(4) -0.0595(3) 0.0451(9) Uani 1 1 d . . .
N9 N 0.2069(2) 0.7318(4) -0.0292(3) 0.0502(10) Uani 1 1 d . . .
C10 C 0.2376(3) 0.7968(5) -0.0779(4) 0.0642(16) Uani 1 1 d . . .
H10 H 0.2846 0.8003 -0.0721 0.077 Uiso 1 1 calc R . .
C11 C 0.1907(3) 0.8592(6) -0.1391(5) 0.0708(18) Uani 1 1 d . . .
H11 H 0.1998 0.9108 -0.1807 0.085 Uiso 1 1 calc R . .
C12 C 0.1289(3) 0.8295(5) -0.1253(4) 0.0592(14) Uani 1 1 d . . .
H12 H 0.0869 0.8569 -0.1562 0.071 Uiso 1 1 calc R . .
N13 N 0.1234(2) 0.4950(4) 0.1516(3) 0.0475(9) Uani 1 1 d . . .
N14 N 0.1915(2) 0.4871(4) 0.1580(3) 0.0489(10) Uani 1 1 d . . .
C15 C 0.2120(3) 0.4044(5) 0.2153(4) 0.0586(14) Uani 1 1 d . . .
H15 H 0.2570 0.3796 0.2334 0.070 Uiso 1 1 calc R . .
C16 C 0.1572(4) 0.3586(6) 0.2452(4) 0.0677(16) Uani 1 1 d . . .
H16 H 0.1587 0.2993 0.2858 0.081 Uiso 1 1 calc R . .
C17 C 0.1014(3) 0.4177(5) 0.2035(4) 0.0593(14) Uani 1 1 d . . .
H17 H 0.0567 0.4071 0.2095 0.071 Uiso 1 1 calc R . .
S18 S -0.09735(6) 0.70301(13) 0.01790(11) 0.0596(4) Uani 1 1 d . . .
C19 C -0.1163(3) 0.8379(5) -0.0400(4) 0.0573(13) Uani 1 1 d . . .
H19 H -0.1002 0.8347 -0.0949 0.069 Uiso 1 1 calc R . .
C20 C -0.0824(4) 0.9354(6) 0.0144(5) 0.0762(18) Uani 1 1 d . . .
H20A H -0.0897 1.0052 -0.0197 0.114 Uiso 1 1 calc R . .
H20B H -0.0343 0.9204 0.0324 0.114 Uiso 1 1 calc R . .
H20C H -0.1013 0.9437 0.0655 0.114 Uiso 1 1 calc R . .
C21 C -0.1929(3) 0.8488(7) -0.0615(6) 0.082(2) Uani 1 1 d . . .
H21A H -0.2088 0.8545 -0.0079 0.124 Uiso 1 1 calc R . .
H21B H -0.2127 0.7821 -0.0940 0.124 Uiso 1 1 calc R . .
H21C H -0.2060 0.9167 -0.0965 0.124 Uiso 1 1 calc R . .
N22 N 0.33360(19) 0.5858(4) 0.1244(3) 0.0441(9) Uani 1 1 d . A .
C23 C 0.3700(2) 0.5087(4) 0.0906(4) 0.0479(11) Uani 1 1 d . . .
C24 C 0.4371(3) 0.4881(6) 0.1250(4) 0.0610(15) Uani 1 1 d . A .
H24 H 0.4613 0.4342 0.0997 0.073 Uiso 1 1 calc R . .
C25 C 0.4682(2) 0.5498(6) 0.1984(4) 0.0688(17) Uani 1 1 d D . .
C26 C 0.4317(3) 0.6332(6) 0.2336(4) 0.0593(14) Uani 1 1 d . A .
H26 H 0.4519 0.6771 0.2825 0.071 Uiso 1 1 calc R . .
C27 C 0.3645(2) 0.6468(4) 0.1917(3) 0.0449(10) Uani 1 1 d . . .
N28 N 0.3322(2) 0.4502(4) 0.0180(3) 0.0465(9) Uani 1 1 d . . .
N29 N 0.2648(2) 0.4747(4) -0.0084(3) 0.0471(9) Uani 1 1 d . . .
C30 C 0.2434(3) 0.4091(5) -0.0770(4) 0.0547(13) Uani 1 1 d . . .
H30 H 0.1986 0.4075 -0.1097 0.066 Uiso 1 1 calc R . .
C31 C 0.2957(3) 0.3423(6) -0.0951(4) 0.0648(15) Uani 1 1 d . . .
H31 H 0.2930 0.2888 -0.1403 0.078 Uiso 1 1 calc R . .
C32 C 0.3509(3) 0.3710(5) -0.0337(4) 0.0629(15) Uani 1 1 d . . .
H32 H 0.3946 0.3409 -0.0281 0.075 Uiso 1 1 calc R . .
N33 N 0.3215(2) 0.7278(4) 0.2170(3) 0.0497(10) Uani 1 1 d . A .
N34 N 0.2562(2) 0.7332(4) 0.1704(3) 0.0519(10) Uani 1 1 d . . .
C35 C 0.2296(3) 0.8226(5) 0.2045(5) 0.0647(15) Uani 1 1 d . A .
H35 H 0.1848 0.8480 0.1852 0.078 Uiso 1 1 calc R . .
C36 C 0.2763(4) 0.8726(6) 0.2716(5) 0.0739(18) Uani 1 1 d . . .
H36 H 0.2692 0.9358 0.3053 0.089 Uiso 1 1 calc R A .
C37 C 0.3348(3) 0.8116(5) 0.2791(4) 0.0653(15) Uani 1 1 d . A .
H37 H 0.3760 0.8246 0.3191 0.078 Uiso 1 1 calc R . .
S38A S 0.54766(16) 0.4916(3) 0.2556(2) 0.0581(8) Uiso 0.50 1 d PD A 1
C39A C 0.5803(7) 0.5815(12) 0.3462(9) 0.057(4) Uiso 0.50 1 d PD A 1
H39A H 0.5464 0.5922 0.3820 0.068 Uiso 0.50 1 calc PR A 1
C40A C 0.6037(10) 0.6987(13) 0.3177(13) 0.076(4) Uiso 0.50 1 d PD A 1
H40A H 0.5648 0.7414 0.2867 0.114 Uiso 0.50 1 calc PR A 1
H40B H 0.6348 0.6868 0.2797 0.114 Uiso 0.50 1 calc PR A 1
H40C H 0.6263 0.7412 0.3688 0.114 Uiso 0.50 1 calc PR A 1
C41A C 0.6394(7) 0.5144(13) 0.3957(10) 0.066(4) Uiso 0.50 1 d PD A 1
H41A H 0.6239 0.4411 0.4124 0.099 Uiso 0.50 1 calc PR A 1
H41B H 0.6611 0.5562 0.4476 0.099 Uiso 0.50 1 calc PR A 1
H41C H 0.6715 0.5024 0.3591 0.099 Uiso 0.50 1 calc PR A 1
S38B S 0.55506(18) 0.5220(4) 0.2312(3) 0.0508(8) Uiso 0.40 1 d PD A 2
C39B C 0.5810(8) 0.6087(17) 0.3311(10) 0.056(5) Uiso 0.40 1 d PD A 2
H39B H 0.5410 0.6309 0.3536 0.068 Uiso 0.40 1 calc PR A 2
C40B C 0.609(2) 0.710(3) 0.293(2) 0.148(16) Uiso 0.40 1 d PD A 2
H40D H 0.5738 0.7438 0.2476 0.223 Uiso 0.40 1 calc PR A 2
H40E H 0.6463 0.6866 0.2679 0.223 Uiso 0.40 1 calc PR A 2
H40F H 0.6246 0.7665 0.3382 0.223 Uiso 0.40 1 calc PR A 2
C41B C 0.6338(13) 0.552(2) 0.4030(16) 0.097(8) Uiso 0.40 1 d PD A 2
H41D H 0.6144 0.4850 0.4240 0.146 Uiso 0.40 1 calc PR A 2
H41E H 0.6482 0.6055 0.4507 0.146 Uiso 0.40 1 calc PR A 2
H41F H 0.6725 0.5298 0.3799 0.146 Uiso 0.40 1 calc PR A 2
S38C S 0.5562(4) 0.5814(9) 0.2094(6) 0.0306(18) Uiso 0.10 1 d PD A 3
C40C C 0.6504(19) 0.695(5) 0.321(3) 0.052(12) Uiso 0.10 1 d PDU A 3
H40G H 0.6524 0.7453 0.2726 0.078 Uiso 0.10 1 calc PR A 3
H40H H 0.6790 0.6289 0.3190 0.078 Uiso 0.10 1 calc PR A 3
H40I H 0.6659 0.7351 0.3754 0.078 Uiso 0.10 1 calc PR A 3
C39C C 0.5781(17) 0.656(5) 0.314(2) 0.10(3) Uiso 0.10 1 d PDU A 3
H39C H 0.5472 0.7201 0.3166 0.122 Uiso 0.10 1 calc PR A 3
C41C C 0.575(4) 0.565(7) 0.382(6) 0.09(2) Uiso 0.10 1 d PDU A 3
H41G H 0.5288 0.5432 0.3787 0.130 Uiso 0.10 1 calc PR A 3
H41H H 0.5949 0.5950 0.4393 0.130 Uiso 0.10 1 calc PR A 3
H41I H 0.6009 0.4984 0.3710 0.130 Uiso 0.10 1 calc PR A 3
B42 B 0.4520(4) 0.7256(7) 0.4886(5) 0.078(2) Uani 1 1 d D . .
F43A F 0.5063(6) 0.7281(11) 0.5646(7) 0.124(4) Uiso 0.55 1 d PD B 1
F44A F 0.4741(5) 0.7908(9) 0.4249(6) 0.092(3) Uiso 0.55 1 d PD B 1
F45A F 0.3965(4) 0.7592(9) 0.5109(7) 0.088(2) Uiso 0.55 1 d PD B 1
F46A F 0.4457(6) 0.6146(8) 0.4558(7) 0.122(4) Uiso 0.55 1 d PD B 1
F43B F 0.5116(12) 0.671(3) 0.530(2) 0.155(18) Uiso 0.15 1 d PD B 2
F44B F 0.4632(14) 0.8338(17) 0.4588(17) 0.088(8) Uiso 0.15 1 d PD B 2
F45B F 0.4107(11) 0.731(2) 0.5475(14) 0.067(6) Uiso 0.15 1 d PD B 2
F46B F 0.4187(18) 0.660(3) 0.4164(16) 0.124(18) Uiso 0.15 1 d PD B 2
F43C F 0.4935(7) 0.7676(13) 0.4403(9) 0.073(4) Uiso 0.30 1 d PD B 3
F44C F 0.4801(11) 0.6911(18) 0.5692(9) 0.135(8) Uiso 0.30 1 d PD B 3
F45C F 0.3977(7) 0.8091(13) 0.4864(11) 0.099(5) Uiso 0.30 1 d PD B 3
F46C F 0.4140(8) 0.6350(12) 0.4369(11) 0.076(4) Uiso 0.30 1 d PD B 3
B47A B 0.0735(8) 0.9812(15) 0.2314(10) 0.065(9) Uiso 0.50 1 d PD C 1
F48A F 0.1356(5) 1.0370(9) 0.2308(7) 0.077(3) Uiso 0.50 1 d PD C 1
F49A F 0.0163(4) 1.0497(8) 0.2013(6) 0.070(3) Uiso 0.50 1 d PD C 1
F50A F 0.0795(4) 0.9592(7) 0.3201(5) 0.070(2) Uiso 0.50 1 d PD C 1
F51A F 0.0687(5) 0.8878(8) 0.1795(6) 0.077(2) Uiso 0.50 1 d PD C 1
B47B B 0.0750(7) 0.9968(14) 0.2319(9) 0.052(7) Uiso 0.50 1 d PD D 2
F48B F 0.1349(5) 1.0550(11) 0.2522(8) 0.099(4) Uiso 0.50 1 d PD D 2
F49B F 0.0268(5) 1.0817(9) 0.2062(7) 0.082(3) Uiso 0.50 1 d PD D 2
F50B F 0.0594(5) 0.9278(7) 0.2985(5) 0.075(2) Uiso 0.50 1 d PD D 2
F51B F 0.0773(5) 0.9231(8) 0.1622(5) 0.078(3) Uiso 0.50 1 d PD D 2
O52A O 0.6227(8) 0.5903(13) 0.6500(9) 0.098(4) Uiso 0.60 1 d P E 1
O52B O 0.6306(15) 0.574(3) 0.626(2) 0.104(9) Uiso 0.30 1 d P F 2
O52C O 0.586(4) 0.619(6) 0.626(5) 0.11(2) Uiso 0.10 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 N2 2.120(4) . ?
Fe1 N9 2.146(4) . ?
Fe1 N14 2.199(4) . ?
Fe1 N22 2.096(4) . ?
Fe1 N29 2.183(4) . ?
Fe1 N34 2.151(5) . ?
N2 C3 1.322(6) . ?
N2 C7 1.335(6) . ?
C3 C4 1.382(6) . ?
C3 N8 1.413(6) . ?
C4 H4 0.9400 . ?
C4 C5 1.391(7) . ?
C5 C6 1.411(7) . ?
C5 S18 1.747(5) . ?
C6 H6 0.9400 . ?
C6 C7 1.370(7) . ?
C7 N13 1.419(6) . ?
N8 N9 1.374(6) . ?
N8 C12 1.346(7) . ?
N9 C10 1.330(7) . ?
C10 H10 0.9400 . ?
C10 C11 1.399(9) . ?
C11 H11 0.9400 . ?
C11 C12 1.364(9) . ?
C12 H12 0.9400 . ?
N13 N14 1.366(6) . ?
N13 C17 1.359(7) . ?
N14 C15 1.326(7) . ?
C15 H15 0.9400 . ?
C15 C16 1.406(9) . ?
C16 H16 0.9400 . ?
C16 C17 1.365(9) . ?
C17 H17 0.9400 . ?
S18 C19 1.822(6) . ?
C19 H19 0.9900 . ?
C19 C20 1.499(9) . ?
C19 C21 1.520(8) . ?
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 1.348(6) . ?
N22 C27 1.316(6) . ?
C23 C24 1.370(7) . ?
C23 N28 1.406(7) . ?
C24 H24 0.9400 . ?
C24 C25 1.389(8) . ?
C25 C26 1.411(8) . ?
C25 S38A 1.797(6) . ?
C25 S38B 1.754(6) . ?
C25 S38C 1.795(10) . ?
C26 H26 0.9400 . ?
C26 C27 1.386(7) . ?
C27 N33 1.405(6) . ?
N28 N29 1.368(6) . ?
N28 C32 1.343(7) . ?
N29 C30 1.317(7) . ?
C30 H30 0.9400 . ?
C30 C31 1.398(9) . ?
C31 H31 0.9400 . ?
C31 C32 1.348(9) . ?
C32 H32 0.9400 . ?
N33 N34 1.366(6) . ?
N33 C37 1.369(7) . ?
N34 C35 1.344(7) . ?
C35 H35 0.9400 . ?
C35 C36 1.382(10) . ?
C36 H36 0.9400 . ?
C36 C37 1.369(9) . ?
C37 H37 0.9400 . ?
S38A C39A 1.778(11) . ?
C39A H39A 0.9900 . ?
C39A C40A 1.551(16) . ?
C39A C41A 1.499(14) . ?
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 1.847(13) . ?
C39B H39B 0.9900 . ?
C39B C40B 1.501(18) . ?
C39B C41B 1.526(17) . ?
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 1.82(2) . ?
C40C H40G 0.9700 . ?
C40C H40H 0.9700 . ?
C40C H40I 0.9700 . ?
C40C C39C 1.52(2) . ?
C39C H39C 0.9900 . ?
C39C C41C 1.52(2) . ?
C41C H41G 0.9700 . ?
C41C H41H 0.9700 . ?
C41C H41I 0.9700 . ?
B42 F43A 1.434(11) . ?
B42 F44A 1.409(10) . ?
B42 F45A 1.313(10) . ?
B42 F46A 1.394(11) . ?
B42 F43B 1.391(16) . ?
B42 F44B 1.388(15) . ?
B42 F45B 1.383(14) . ?
B42 F46B 1.413(16) . ?
B42 F43C 1.345(12) . ?
B42 F44C 1.332(13) . ?
B42 F45C 1.469(13) . ?
B42 F46C 1.451(12) . ?
B47A F48A 1.423(15) . ?
B47A F49A 1.403(15) . ?
B47A F50A 1.397(15) . ?
B47A F51A 1.356(15) . ?
B47B F48B 1.369(14) . ?
B47B F49B 1.391(14) . ?
B47B F50B 1.413(14) . ?
B47B F51B 1.404(14) . ?

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 N9 73.82(15) . . ?
N2 Fe1 N14 73.49(15) . . ?
N2 Fe1 N29 114.16(15) . . ?
N2 Fe1 N34 98.22(16) . . ?
N9 Fe1 N14 147.30(15) . . ?
N9 Fe1 N29 96.19(17) . . ?
N9 Fe1 N34 91.39(18) . . ?
N22 Fe1 N2 168.63(16) . . ?
N22 Fe1 N9 113.65(16) . . ?
N22 Fe1 N14 98.64(16) . . ?
N22 Fe1 N29 74.46(16) . . ?
N22 Fe1 N34 73.64(16) . . ?
N29 Fe1 N14 97.27(16) . . ?
N34 Fe1 N14 92.97(17) . . ?
N34 Fe1 N29 147.60(15) . . ?
C3 N2 Fe1 120.5(3) . . ?
C3 N2 C7 117.8(4) . . ?
C7 N2 Fe1 121.1(3) . . ?
N2 C3 C4 124.1(4) . . ?
N2 C3 N8 112.8(4) . . ?
C4 C3 N8 123.1(4) . . ?
C3 C4 H4 121.4 . . ?
C3 C4 C5 117.1(5) . . ?
C5 C4 H4 121.4 . . ?
C4 C5 C6 119.9(4) . . ?
C4 C5 S18 125.0(4) . . ?
C6 C5 S18 115.1(4) . . ?
C5 C6 H6 121.7 . . ?
C7 C6 C5 116.7(5) . . ?
C7 C6 H6 121.7 . . ?
N2 C7 C6 124.3(5) . . ?
N2 C7 N13 112.5(4) . . ?
C6 C7 N13 123.2(4) . . ?
N9 N8 C3 117.2(4) . . ?
C12 N8 C3 131.3(4) . . ?
C12 N8 N9 111.2(4) . . ?
N8 N9 Fe1 115.0(3) . . ?
C10 N9 Fe1 140.3(4) . . ?
C10 N9 N8 104.7(4) . . ?
N9 C10 H10 124.4 . . ?
N9 C10 C11 111.2(5) . . ?
C11 C10 H10 124.4 . . ?
C10 C11 H11 127.3 . . ?
C12 C11 C10 105.4(5) . . ?
C12 C11 H11 127.3 . . ?
N8 C12 C11 107.4(5) . . ?
N8 C12 H12 126.3 . . ?
C11 C12 H12 126.3 . . ?
N14 N13 C7 118.5(4) . . ?
C17 N13 C7 129.5(5) . . ?
C17 N13 N14 111.9(4) . . ?
N13 N14 Fe1 113.9(3) . . ?
C15 N14 Fe1 141.1(4) . . ?
C15 N14 N13 105.0(4) . . ?
N14 C15 H15 124.6 . . ?
N14 C15 C16 110.7(5) . . ?
C16 C15 H15 124.6 . . ?
C15 C16 H16 126.9 . . ?
C17 C16 C15 106.2(5) . . ?
C17 C16 H16 126.9 . . ?
N13 C17 C16 106.1(5) . . ?
N13 C17 H17 126.9 . . ?
C16 C17 H17 126.9 . . ?
C5 S18 C19 105.3(3) . . ?
S18 C19 H19 109.2 . . ?
C20 C19 S18 110.9(5) . . ?
C20 C19 H19 109.2 . . ?
C20 C19 C21 112.4(6) . . ?
C21 C19 S18 106.0(5) . . ?
C21 C19 H19 109.2 . . ?
C19 C20 H20A 109.5 . . ?
C19 C20 H20B 109.5 . . ?
C19 C20 H20C 109.5 . . ?
H20A C20 H20B 109.5 . . ?
H20A C20 H20C 109.5 . . ?
H20B C20 H20C 109.5 . . ?
C19 C21 H21A 109.5 . . ?
C19 C21 H21B 109.5 . . ?
C19 C21 H21C 109.5 . . ?
H21A C21 H21B 109.5 . . ?
H21A C21 H21C 109.5 . . ?
H21B C21 H21C 109.5 . . ?
C23 N22 Fe1 120.1(3) . . ?
C27 N22 Fe1 121.4(3) . . ?
C27 N22 C23 118.4(4) . . ?
N22 C23 C24 123.1(5) . . ?
N22 C23 N28 113.5(4) . . ?
C24 C23 N28 123.4(5) . . ?
C23 C24 H24 121.2 . . ?
C23 C24 C25 117.6(5) . . ?
C25 C24 H24 121.2 . . ?
C24 C25 C26 120.4(5) . . ?
C24 C25 S38A 114.2(5) . . ?
C24 C25 S38B 112.9(4) . . ?
C24 C25 S38C 116.4(5) . . ?
C26 C25 S38A 123.9(5) . . ?
C26 C25 S38B 126.4(4) . . ?
C26 C25 S38C 114.7(6) . . ?
C25 C26 H26 122.0 . . ?
C27 C26 C25 116.1(5) . . ?
C27 C26 H26 122.0 . . ?
N22 C27 C26 124.3(5) . . ?
N22 C27 N33 112.3(4) . . ?
C26 C27 N33 123.4(5) . . ?
N29 N28 C23 118.2(4) . . ?
C32 N28 C23 130.7(5) . . ?
C32 N28 N29 111.0(4) . . ?
N28 N29 Fe1 113.7(3) . . ?
C30 N29 Fe1 141.7(4) . . ?
C30 N29 N28 104.6(4) . . ?
N29 C30 H30 124.3 . . ?
N29 C30 C31 111.5(5) . . ?
C31 C30 H30 124.3 . . ?
C30 C31 H31 127.4 . . ?
C32 C31 C30 105.2(5) . . ?
C32 C31 H31 127.4 . . ?
N28 C32 C31 107.7(5) . . ?
N28 C32 H32 126.1 . . ?
C31 C32 H32 126.1 . . ?
N34 N33 C27 118.0(4) . . ?
N34 N33 C37 111.4(4) . . ?
C37 N33 C27 130.5(5) . . ?
N33 N34 Fe1 114.3(3) . . ?
C35 N34 Fe1 141.3(4) . . ?
C35 N34 N33 104.4(5) . . ?
N34 C35 H35 124.2 . . ?
N34 C35 C36 111.6(6) . . ?
C36 C35 H35 124.2 . . ?
C35 C36 H36 126.9 . . ?
C37 C36 C35 106.2(5) . . ?
C37 C36 H36 126.9 . . ?
N33 C37 H37 126.8 . . ?
C36 C37 N33 106.4(6) . . ?
C36 C37 H37 126.8 . . ?
C39A S38A C25 108.0(5) . . ?
S38A C39A H39A 110.4 . . ?
C40A C39A S38A 112.1(12) . . ?
C40A C39A H39A 110.4 . . ?
C41A C39A S38A 102.6(10) . . ?
C41A C39A H39A 110.4 . . ?
C41A C39A C40A 110.7(11) . . ?
C39A C40A H40A 109.5 . . ?
C39A C40A H40B 109.5 . . ?
C39A C40A H40C 109.5 . . ?
H40A C40A H40B 109.5 . . ?
H40A C40A H40C 109.5 . . ?
H40B C40A H40C 109.5 . . ?
C39A C41A H41A 109.5 . . ?
C39A C41A H41B 109.5 . . ?
C39A C41A H41C 109.5 . . ?
H41A C41A H41B 109.5 . . ?
H41A C41A H41C 109.5 . . ?
H41B C41A H41C 109.5 . . ?
C25 S38B C39B 103.1(6) . . ?
S38B C39B H39B 110.3 . . ?
C40B C39B S38B 99.0(19) . . ?
C40B C39B H39B 110.3 . . ?
C40B C39B C41B 112.2(16) . . ?
C41B C39B S38B 114.3(15) . . ?
C41B C39B H39B 110.3 . . ?
C39B C40B H40D 109.5 . . ?
C39B C40B H40E 109.5 . . ?
C39B C40B H40F 109.5 . . ?
H40D C40B H40E 109.5 . . ?
H40D C40B H40F 109.5 . . ?
H40E C40B H40F 109.5 . . ?
C39B C41B H41D 109.5 . . ?
C39B C41B H41E 109.5 . . ?
C39B C41B H41F 109.5 . . ?
H41D C41B H41E 109.5 . . ?
H41D C41B H41F 109.5 . . ?
H41E C41B H41F 109.5 . . ?
C25 S38C C39C 102.9(11) . . ?
H40G C40C H40H 109.5 . . ?
H40G C40C H40I 109.5 . . ?
H40H C40C H40I 109.5 . . ?
C39C C40C H40G 109.5 . . ?
C39C C40C H40H 109.5 . . ?
C39C C40C H40I 109.5 . . ?
S38C C39C H39C 112.2 . . ?
C40C C39C S38C 104(3) . . ?
C40C C39C H39C 112.2 . . ?
C40C C39C C41C 110(2) . . ?
C41C C39C S38C 105(5) . . ?
C41C C39C H39C 112.2 . . ?
C39C C41C H41G 109.5 . . ?
C39C C41C H41H 109.5 . . ?
C39C C41C H41I 109.5 . . ?
H41G C41C H41H 109.5 . . ?
H41G C41C H41I 109.5 . . ?
H41H C41C H41I 109.5 . . ?
F44A B42 F43A 106.0(8) . . ?
F45A B42 F43A 108.5(8) . . ?
F45A B42 F44A 117.0(9) . . ?
F45A B42 F46A 111.4(8) . . ?
F46A B42 F43A 108.6(9) . . ?
F46A B42 F44A 105.1(8) . . ?
F43B B42 F46B 109.7(15) . . ?
F44B B42 F43B 112.5(15) . . ?
F44B B42 F46B 108.1(14) . . ?
F45B B42 F43B 107.7(14) . . ?
F45B B42 F44B 110.6(13) . . ?
F45B B42 F46B 108.2(14) . . ?
F43C B42 F45C 107.6(10) . . ?
F43C B42 F46C 105.8(10) . . ?
F44C B42 F43C 117.4(12) . . ?
F44C B42 F45C 112.6(11) . . ?
F44C B42 F46C 111.9(12) . . ?
F46C B42 F45C 99.8(9) . . ?
F49A B47A F48A 113.7(13) . . ?
F50A B47A F48A 102.1(11) . . ?
F50A B47A F49A 108.9(11) . . ?
F51A B47A F48A 108.1(12) . . ?
F51A B47A F49A 108.4(11) . . ?
F51A B47A F50A 115.6(13) . . ?
F48B B47B F49B 104.0(12) . . ?
F48B B47B F50B 116.5(11) . . ?
F48B B47B F51B 107.9(11) . . ?
F49B B47B F50B 111.4(10) . . ?
F49B B47B F51B 110.8(11) . . ?
F51B B47B F50B 106.2(12) . . ?

