# Electronic Supplementary Material (ESI) for Dalton Transactions.
# This journal is © The Royal Society of Chemistry 2019

####################################################################### 
# 
# 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_fe(bpt)2
_database_code_depnum_ccdc_archive 'CCDC 1550948'
_audit_update_record             
;
2019-10-07 deposited with the CCDC.	2019-11-05 downloaded from the CCDC.
;
_audit_creation_date             2019-07-05
_audit_creation_method           
;
  Olex2 1.2
  (compiled Apr 23 2013 17:54:37, GUI svn.r4466)
;
_chemical_name_common            ?
_chemical_name_systematic        
;
Octakis[2,4-di(pyrazol-1-yl)-1,3,5-triazine]-tetrairon(II)
octa-tetrafluoroborate hemi[2-(trifluoroboryl)-1H-pyrazole]
acetonitrile (8/5.9) solvate
;
_chemical_formula_moiety         
'C72 H56 Fe4 N56, 8(B F4), 0.5(C3 H4 B F3 N2), 5.9(C2 H3 N1)'
_chemical_formula_sum            'C85.30 H75.70 B8.50 F33.50 Fe4 N62.90'
_chemical_formula_weight         2933.77
_chemical_melting_point          ?
loop_
_atom_type_symbol
_atom_type_description
_atom_type_scat_dispersion_real
_atom_type_scat_dispersion_imag
_atom_type_scat_source
C C 0.0181 0.0091 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
N N 0.0311 0.0180 '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'
F F 0.0727 0.0534 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
B B 0.0090 0.0039 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'

_space_group_crystal_system      triclinic
_space_group_IT_number           2
_space_group_name_H-M_alt        'P -1'
_space_group_name_Hall           '-P 1'
loop_
_space_group_symop_id
_space_group_symop_operation_xyz
1 'x, y, z'
2 '-x, -y, -z'

_cell_length_a                   16.1862(6)
_cell_length_b                   17.2352(5)
_cell_length_c                   23.7427(7)
_cell_angle_alpha                97.839(2)
_cell_angle_beta                 91.234(3)
_cell_angle_gamma                105.400(3)
_cell_volume                     6314.5(4)
_cell_formula_units_Z            2
_cell_measurement_reflns_used    20214
_cell_measurement_temperature    120(2)
_cell_measurement_theta_min      3.50
_cell_measurement_theta_max      73.63
_exptl_absorpt_coefficient_mu    4.676
_exptl_absorpt_correction_T_min  0.506
_exptl_absorpt_correction_T_max  1.000
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   
; 
CrysAlisPro, Agilent Technologies,
Version 1.171.36.24 (release 03-12-2012 CrysAlis171 .NET)
Empirical absorption correction using spherical harmonics,
 implemented in SCALE3 ABSPACK scaling algorithm.
;

_exptl_crystal_colour            orange
_exptl_crystal_density_diffrn    1.543
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       plate
_exptl_crystal_F_000             2952
_exptl_crystal_size_max          0.35
_exptl_crystal_size_mid          0.13
_exptl_crystal_size_min          0.06
_exptl_special_details           
;
 ? 
;
_diffrn_reflns_av_R_equivalents  0.0327
_diffrn_reflns_av_unetI/netI     0.0370
_diffrn_reflns_limit_h_max       19
_diffrn_reflns_limit_h_min       -19
_diffrn_reflns_limit_k_max       18
_diffrn_reflns_limit_k_min       -20
_diffrn_reflns_limit_l_max       29
_diffrn_reflns_limit_l_min       -26
_diffrn_reflns_number            54575
_diffrn_reflns_theta_full        72.00
_diffrn_reflns_theta_max         73.92
_diffrn_reflns_theta_min         3.31
_diffrn_ambient_temperature      120(2)
_diffrn_detector_area_resol_mean 5.3095
_diffrn_measured_fraction_theta_full 0.952
_diffrn_measured_fraction_theta_max 0.932
_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                19787
_reflns_number_total             23884
_reflns_threshold_expression     >2sigma(I)
_computing_cell_refinement       'CrysAlisPro, Agilent Technologies'
_computing_data_collection       '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         1.205
_refine_diff_density_min         -0.714
_refine_diff_density_rms         0.098
_refine_ls_extinction_coef       ?
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.022
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           fullcycle
_refine_ls_number_parameters     1754
_refine_ls_number_reflns         23884
_refine_ls_number_restraints     72
_refine_ls_R_factor_all          0.0893
_refine_ls_R_factor_gt           0.0777
_refine_ls_restrained_S_all      1.029
_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)+(0.1416P)²+9.8485P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.2221
_refine_ls_wR_factor_ref         0.2353
_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 uncoordinated pyrazole substituent is disordered over two sites, with 
 a refined occupancy ratio of 0.67:0.33. The major orientation was refined
 without restraints, but the C---C and C---N bond lengths in the minor 
 orientation were restrained to a common value of 1.38(2) Å to ensure a 
 reasonable geometry. This disorder is coupled to the presence or absence
 of a half-occupied a half-occupied pyrazole-derived fragment, positioned 
 to hydrogen bond to the major ligand disorder site. That moiety was 
 modelled as the 1H-pyrazole---BF₃ adduct, which refined acceptably
 without restraints.

 Three of the BF₄⁻ ions are also disordered over two equally occupied 
 orientations; in one case, these share a common wholly occupied B atom. 
 The refined restraints B---F = 1.39(2) and F...F = 2.27(2) Å were 
 applied to those residues. Nine acetonitrile molecules were located in
 the Fourier map, whose occupancies ranged from 0.2 to 1.0. The two 
 lowest-occupancy MeCN sites were modelled with fixed restraints 
 C---C = 1.45(2), C---N = 1.15(2) and 1,3-C...N = 2.63(2) Å to 
 ensure a reasonable geometry. The 0.2-occupied MeCN molecule is 
 co-localised with the aforementioned, half-occupied 1H-pyrazole---BF₃ 
 moiety. 

 All non-H atoms with occupancy >0.5 were refined anisotropically, while 
 H atoms were placed in calculated positions and refined using a riding 
 model. The highest residual Fourier peak of +1.2 e./%A⁻³ is 
 associated with the pyrazole---BF₃ half-molecule, and may imply 
 additional, weakly occupied solvent in this region of the lattice.
;
_olex2_refinement_description    
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups, All N(H) groups
 At 1.5 times of:
  All C(H,H,H) groups
2. Restrained distances
 B143-F44A = B143-F45A = B143-F46A = B143-F47A
 1.39455 with sigma of 0.02
 B143-F44B = B143-F45B = B143-F46B = B143-F47B
 1.39455 with sigma of 0.02
 F44A-F45A = F44A-F46A = F44A-F47A = F45A-F46A = F45A-F47A = F46A-F47A
 2.2773 with sigma of 0.02
 F44B-F45B = F44B-F46B = F44B-F47B = F45B-F46B = F45B-F47B = F46B-F47B
 2.2773 with sigma of 0.02
 B48A-F49A = B48A-F50A = B48A-F51A = B48A-F52A
 1.39455 with sigma of 0.02
 B48B-F49B = B48B-F50B = B48B-F51B = B48B-F52B
 1.39455 with sigma of 0.02
 F49A-F50A = F49A-F51A = F49A-F52A = F50A-F51A = F50A-F52A = F51A-F52A
 2.2773 with sigma of 0.02
 F49B-F50B = F49B-F51B = F49B-F52B = F50B-F51B = F50B-F52B = F51B-F52B
 2.2773 with sigma of 0.02
 B58A-F59A = B58A-F60A = B58A-F61A = B58A-F62A
 1.39455 with sigma of 0.02
 B58B-F59B = B58B-F60B = B58B-F61B = B58B-F62B
 1.39455 with sigma of 0.02
 F59A-F60A = F59A-F61A = F59A-F62A = F60A-F61A = F60A-F62A = F61A-F62A
 2.2773 with sigma of 0.02
 F59B-F60B = F59B-F61B = F59B-F62B = F60B-F61B = F60B-F62B = F61B-F62B
 2.2773 with sigma of 0.02
 C203-C204 = C206-C207
 1.48 with sigma of 0.02
 C204-N205 = C207-N208
 1.15 with sigma of 0.02
 C203-N205 = C206-N208
 2.63 with sigma of 0.02
 C106-N12B = N12B-N13B = N13B-C14B = C14B-C15B = C15B-C16B = C16B-N12B
 1.38 with sigma of 0.02
3. Others
 1(DFIX)=1(DFIX)=1(DFIX)=1(DFIX)=1(DFIX)=1(DFIX)=FVAR(1)
 1(DFIX)=1(DFIX)=1(DFIX)=1(DFIX)=1(DFIX)=1(DFIX)=1.633*FVAR(2)
 Fixed Sof: N12A(0.67) N13A(0.67) C14A(0.67) H14A(0.67) C15A(0.67) H15A(0.67)
 C16A(0.67) H16A(0.67) N12B(0.33) N13B(0.33) C14B(0.33) H14B(0.33) C15B(0.33)
 H15B(0.33) C16B(0.33) H16B(0.33) F44A(0.5) F45A(0.5) F46A(0.5) F47A(0.5)
 F44B(0.5) F45B(0.5) F46B(0.5) F47B(0.5) B48A(0.5) F49A(0.5) F50A(0.5)
 F51A(0.5) F52A(0.5) B48B(0.5) F49B(0.5) F50B(0.5) F51B(0.5) F52B(0.5)
 B58A(0.5) F59A(0.5) F60A(0.5) F61A(0.5) F62A(0.5) B58B(0.5) F59B(0.5)
 F60B(0.5) F61B(0.5) F62B(0.5) N173(0.5) N174(0.5) H174(0.5) C175(0.5)
 H175(0.5) C176(0.5) H176(0.5) C177(0.5) H177(0.5) B178(0.5) F179(0.5)
 F180(0.5) F181(0.5) C182(0.7) H18A(0.7) H18B(0.7) H18C(0.7) C183(0.7)
 N184(0.7) C185(0.8) H18D(0.8) H18E(0.8) H18F(0.8) C186(0.8) N187(0.8)
 C188(0.7) H18G(0.7) H18H(0.7) H18I(0.7) C189(0.7) N190(0.7) C194(0.9)
 H19D(0.9) H19E(0.9) H19F(0.9) C195(0.9) N196(0.9) C197(0.8) H19G(0.8)
 H19H(0.8) H19I(0.8) C198(0.8) N199(0.8) C200(0.5) H20A(0.5) H20B(0.5)
 H20C(0.5) C201(0.5) N202(0.5) C203(0.3) H20D(0.3) H20E(0.3) H20F(0.3)
 C204(0.3) N205(0.3) C206(0.2) H20G(0.2) H20H(0.2) H20I(0.2) C207(0.2) N208(0.2)
4.a Aromatic/amide H refined with riding coordinates:
 C8(H8), C13(H13), C14(H14), C15(H15), C18(H18), C19(H19), C20(H20), C24(H24),
 C29(H29), C30(H30), C31(H31), C34(H34), C35(H35), C36(H36), C40(H40), C45(H45),
  C46(H46), C47(H47), C50(H50), C51(H51), C52(H52), C56(H56), C61(H61),
 C62(H62), C63(H63), C66(H66), C67(H67), C68(H68), C72(H72), C77(H77), C78(H78),
  C79(H79), C82(H82), C83(H83), C84(H84), C88(H88), C93(H93), C94(H94),
 C95(H95), C98(H98), C99(H99), C100(H100), C104(H104), C109(H109), C110(H110),
 C111(H111), C14A(H14A), C15A(H15A), C16A(H16A), C14B(H14B), C15B(H15B),
 C16B(H16B), C120(H120), C125(H125), C126(H126), C127(H127), C130(H130),
 C131(H131), C132(H132), N174(H174), C175(H175), C176(H176), C177(H177)
4.b Idealised Me refined as rotating group:
 C182(H18A,H18B,H18C), C185(H18D,H18E,H18F), C188(H18G,H18H,H18I), C191(H19A,
 H19B,H19C), C194(H19D,H19E,H19F), C197(H19G,H19H,H19I), C200(H20A,H20B,H20C),
 C203(H20D,H20E,H20F), C206(H20G,H20H,H20I)
;
_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 0.74000(4) 0.91150(4) 0.22950(3) 0.03439(14) Uani 1 1 d . . .
Fe2 Fe 0.36769(4) 0.83855(4) 0.35011(3) 0.03712(15) Uani 1 1 d . . .
Fe3 Fe 0.33318(4) 0.43970(4) 0.30004(3) 0.03863(15) Uani 1 1 d . . .
Fe4 Fe 0.70973(4) 0.52268(4) 0.18976(3) 0.03878(16) Uani 1 1 d . . .
N5 N 0.6341(2) 0.8382(2) 0.38701(15) 0.0376(7) Uani 1 1 d . . .
C6 C 0.6773(2) 0.8666(2) 0.34412(17) 0.0351(8) Uani 1 1 d . . .
N7 N 0.6468(2) 0.8929(2) 0.29933(15) 0.0351(7) Uani 1 1 d . . .
C8 C 0.5641(3) 0.8913(2) 0.30118(19) 0.0374(9) Uani 1 1 d . . .
H8 H 0.5394 0.9104 0.2710 0.045 Uiso 1 1 calc R . .
N9 N 0.5129(2) 0.8647(2) 0.34222(15) 0.0363(7) Uani 1 1 d . . .
C10 C 0.5527(3) 0.8384(2) 0.38305(18) 0.0366(8) Uani 1 1 d . . .
N11 N 0.7631(2) 0.8681(2) 0.34479(15) 0.0365(7) Uani 1 1 d . . .
N12 N 0.8089(2) 0.8907(2) 0.29911(16) 0.0386(7) Uani 1 1 d . . .
C13 C 0.8886(3) 0.8911(3) 0.3137(2) 0.0460(10) Uani 1 1 d . . .
H13 H 0.9354 0.9035 0.2900 0.055 Uiso 1 1 calc R . .
C14 C 0.8949(3) 0.8712(4) 0.3681(2) 0.0570(13) Uani 1 1 d . . .
H14 H 0.9454 0.8683 0.3879 0.068 Uiso 1 1 calc R . .
C15 C 0.8145(3) 0.8566(3) 0.3872(2) 0.0496(11) Uani 1 1 d . . .
H15 H 0.7975 0.8413 0.4230 0.059 Uiso 1 1 calc R . .
N16 N 0.5023(2) 0.8075(2) 0.42517(15) 0.0387(7) Uani 1 1 d . . .
N17 N 0.4160(2) 0.8010(2) 0.42207(15) 0.0421(8) Uani 1 1 d . . .
C18 C 0.3869(3) 0.7681(3) 0.46811(19) 0.0500(11) Uani 1 1 d . . .
H18 H 0.3288 0.7566 0.4780 0.060 Uiso 1 1 calc R . .
C19 C 0.4536(4) 0.7525(4) 0.5002(2) 0.0580(13) Uani 1 1 d . . .
H19 H 0.4490 0.7288 0.5343 0.070 Uiso 1 1 calc R . .
C20 C 0.5264(3) 0.7787(3) 0.4719(2) 0.0504(11) Uani 1 1 d . . .
H20 H 0.5827 0.7773 0.4828 0.060 Uiso 1 1 calc R . .
N21 N 0.3195(2) 0.6403(2) 0.20614(15) 0.0360(7) Uani 1 1 d . . .
C22 C 0.3275(2) 0.7044(3) 0.24516(18) 0.0360(8) Uani 1 1 d . . .
N23 N 0.3337(2) 0.7083(2) 0.30178(15) 0.0360(7) Uani 1 1 d . . .
C24 C 0.3300(3) 0.6368(3) 0.31875(18) 0.0374(8) Uani 1 1 d . . .
H24 H 0.3340 0.6357 0.3586 0.045 Uiso 1 1 calc R . .
N25 N 0.3211(2) 0.5665(2) 0.28415(15) 0.0376(7) Uani 1 1 d . . .
C26 C 0.3162(2) 0.5738(2) 0.22898(17) 0.0349(8) Uani 1 1 d . . .
N27 N 0.3314(2) 0.7770(2) 0.22509(15) 0.0363(7) Uani 1 1 d . . .
N28 N 0.3441(2) 0.8466(2) 0.26330(16) 0.0389(7) Uani 1 1 d . . .
C29 C 0.3437(3) 0.9044(3) 0.2318(2) 0.0431(9) Uani 1 1 d . . .
H29 H 0.3507 0.9599 0.2467 0.052 Uiso 1 1 calc R . .
C30 C 0.3315(3) 0.8732(3) 0.1736(2) 0.0488(11) Uani 1 1 d . . .
H30 H 0.3290 0.9024 0.1427 0.059 Uiso 1 1 calc R . .
C31 C 0.3238(3) 0.7913(3) 0.17062(19) 0.0434(10) Uani 1 1 d . . .
H31 H 0.3148 0.7524 0.1371 0.052 Uiso 1 1 calc R . .
N32 N 0.3073(2) 0.5029(2) 0.19077(15) 0.0358(7) Uani 1 1 d . . .
N33 N 0.3060(2) 0.4325(2) 0.21193(15) 0.0388(7) Uani 1 1 d . . .
C34 C 0.2912(3) 0.3762(3) 0.1667(2) 0.0473(11) Uani 1 1 d . . .
H34 H 0.2869 0.3204 0.1677 0.057 Uiso 1 1 calc R . .
C35 C 0.2824(4) 0.4091(3) 0.1165(2) 0.0558(13) Uani 1 1 d . . .
H35 H 0.2711 0.3808 0.0787 0.067 Uiso 1 1 calc R . .
C36 C 0.2937(3) 0.4897(3) 0.13351(19) 0.0464(10) Uani 1 1 d . . .
H36 H 0.2923 0.5294 0.1097 0.056 Uiso 1 1 calc R . .
N37 N 0.6011(2) 0.5551(2) 0.35512(15) 0.0434(8) Uani 1 1 d . . .
C38 C 0.5185(3) 0.5185(3) 0.34617(18) 0.0404(9) Uani 1 1 d . . .
N39 N 0.4774(2) 0.4763(2) 0.29703(15) 0.0383(7) Uani 1 1 d . . .
C40 C 0.5288(3) 0.4717(3) 0.25467(18) 0.0395(9) Uani 1 1 d . . .
H40 H 0.5034 0.4415 0.2192 0.047 Uiso 1 1 calc R . .
N41 N 0.6135(2) 0.5063(2) 0.25788(15) 0.0388(8) Uani 1 1 d . . .
C42 C 0.6438(3) 0.5469(3) 0.30941(19) 0.0401(9) Uani 1 1 d . . .
N43 N 0.4677(2) 0.5246(2) 0.39171(16) 0.0438(8) Uani 1 1 d . . .
N44 N 0.3815(3) 0.4891(2) 0.38445(16) 0.0439(8) Uani 1 1 d . . .
C45 C 0.3523(4) 0.5019(3) 0.4354(2) 0.0556(12) Uani 1 1 d . . .
H45 H 0.2938 0.4836 0.4438 0.067 Uiso 1 1 calc R . .
C46 C 0.4190(4) 0.5462(4) 0.4755(2) 0.0624(14) Uani 1 1 d . . .
H46 H 0.4143 0.5628 0.5148 0.075 Uiso 1 1 calc R . .
C47 C 0.4908(4) 0.5602(3) 0.4468(2) 0.0539(12) Uani 1 1 d . . .
H47 H 0.5470 0.5894 0.4620 0.065 Uiso 1 1 calc R . .
N48 N 0.7315(2) 0.5843(2) 0.31507(16) 0.0442(9) Uani 1 1 d . . .
N49 N 0.7797(2) 0.5791(2) 0.26872(16) 0.0431(8) Uani 1 1 d . . .
C50 C 0.8592(3) 0.6200(3) 0.2874(2) 0.0495(11) Uani 1 1 d . . .
H50 H 0.9075 0.6266 0.2646 0.059 Uiso 1 1 calc R . .
C51 C 0.8624(3) 0.6521(3) 0.3453(2) 0.0598(13) Uani 1 1 d . . .
H51 H 0.9118 0.6838 0.3683 0.072 Uiso 1 1 calc R . .
C52 C 0.7812(3) 0.6290(3) 0.3618(2) 0.0562(13) Uani 1 1 d . . .
H52 H 0.7622 0.6414 0.3987 0.067 Uiso 1 1 calc R . .
N53 N 0.5872(2) 0.6939(2) 0.12614(14) 0.0363(7) Uani 1 1 d . . .
C54 C 0.6202(3) 0.6355(3) 0.13808(17) 0.0365(8) Uani 1 1 d . . .
N55 N 0.6902(2) 0.6432(2) 0.17197(15) 0.0368(7) Uani 1 1 d . . .
C56 C 0.7270(3) 0.7194(3) 0.19580(19) 0.0394(9) Uani 1 1 d . . .
H56 H 0.7767 0.7287 0.2205 0.047 Uiso 1 1 calc R . .
N57 N 0.6998(2) 0.7835(2) 0.18791(15) 0.0348(7) Uani 1 1 d . . .
C58 C 0.6302(2) 0.7660(2) 0.15173(17) 0.0340(8) Uani 1 1 d . . .
N59 N 0.5783(2) 0.5575(2) 0.11353(15) 0.0372(7) Uani 1 1 d . . .
N60 N 0.6107(2) 0.4945(2) 0.12454(15) 0.0389(7) Uani 1 1 d . . .
C61 C 0.5586(3) 0.4288(3) 0.09470(19) 0.0445(10) Uani 1 1 d . . .
H61 H 0.5648 0.3753 0.0938 0.053 Uiso 1 1 calc R . .
C62 C 0.4930(3) 0.4480(3) 0.0646(2) 0.0502(11) Uani 1 1 d . . .
H62 H 0.4482 0.4113 0.0401 0.060 Uiso 1 1 calc R . .
C63 C 0.5063(3) 0.5293(3) 0.07741(19) 0.0451(10) Uani 1 1 d . . .
H63 H 0.4723 0.5609 0.0639 0.054 Uiso 1 1 calc R . .
N64 N 0.6007(2) 0.8310(2) 0.14131(14) 0.0353(7) Uani 1 1 d . . .
N65 N 0.6423(2) 0.9072(2) 0.16926(15) 0.0367(7) Uani 1 1 d . . .
C66 C 0.6024(3) 0.9567(3) 0.14968(19) 0.0434(10) Uani 1 1 d . . .
H66 H 0.6171 1.0139 0.1612 0.052 Uiso 1 1 calc R . .
C67 C 0.5352(3) 0.9131(3) 0.1094(2) 0.0519(11) Uani 1 1 d . . .
H67 H 0.4971 0.9348 0.0896 0.062 Uiso 1 1 calc R . .
C68 C 0.5358(3) 0.8329(3) 0.1045(2) 0.0458(10) Uani 1 1 d . . .
H68 H 0.4986 0.7881 0.0805 0.055 Uiso 1 1 calc R . .
N69 N 0.8997(3) 1.1520(3) 0.2252(2) 0.0587(11) Uani 1 1 d . . .
C70 C 0.8587(3) 1.0740(3) 0.2218(2) 0.0486(11) Uani 1 1 d . . .
N71 N 0.7832(3) 1.0427(2) 0.24473(16) 0.0458(9) Uani 1 1 d . . .
C72 C 0.7492(4) 1.0979(3) 0.2722(2) 0.0582(13) Uani 1 1 d . . .
H72 H 0.6968 1.0793 0.2897 0.070 Uiso 1 1 calc R . .
N73 N 0.7849(4) 1.1792(3) 0.2768(2) 0.0624(12) Uani 1 1 d . . .
C74 C 0.8589(4) 1.1993(3) 0.2520(2) 0.0551(12) Uani 1 1 d . . .
N75 N 0.8949(3) 1.0190(3) 0.19144(19) 0.0536(10) Uani 1 1 d . . .
N76 N 0.8505(3) 0.9396(2) 0.18214(17) 0.0466(9) Uani 1 1 d . . .
C77 C 0.8959(3) 0.9036(3) 0.1464(2) 0.0548(12) Uani 1 1 d . . .
H77 H 0.8801 0.8471 0.1321 0.066 Uiso 1 1 calc R . .
C78 C 0.9702(4) 0.9599(4) 0.1326(3) 0.0654(14) Uani 1 1 d . . .
H78 H 1.0127 0.9493 0.1080 0.078 Uiso 1 1 calc R . .
C79 C 0.9681(3) 1.0324(4) 0.1617(3) 0.0604(13) Uani 1 1 d . . .
H79 H 1.0095 1.0831 0.1616 0.073 Uiso 1 1 calc R . .
N80 N 0.8958(3) 1.2833(3) 0.2557(2) 0.0656(12) Uani 1 1 d . . .
N81 N 0.9684(4) 1.3131(3) 0.2272(2) 0.0759(15) Uani 1 1 d . . .
C82 C 0.9818(5) 1.3934(4) 0.2371(3) 0.0786(19) Uani 1 1 d . . .
H82 H 1.0274 1.4318 0.2232 0.094 Uiso 1 1 calc R . .
C83 C 0.9177(5) 1.4130(4) 0.2717(3) 0.0760(19) Uani 1 1 d . . .
H83 H 0.9128 1.4661 0.2850 0.091 Uiso 1 1 calc R . .
C84 C 0.8661(5) 1.3439(4) 0.2820(3) 0.0762(19) Uani 1 1 d . . .
H84 H 0.8170 1.3379 0.3039 0.091 Uiso 1 1 calc R . .
N85 N 0.1693(2) 0.9106(3) 0.44242(15) 0.0440(9) Uani 1 1 d . . .
C86 C 0.2349(3) 0.9008(3) 0.41297(17) 0.0379(9) Uani 1 1 d . . .
N87 N 0.2433(2) 0.8305(2) 0.38539(16) 0.0420(8) Uani 1 1 d . . .
C88 C 0.1752(3) 0.7665(3) 0.3867(2) 0.0520(11) Uani 1 1 d . . .
H88 H 0.1774 0.7158 0.3663 0.062 Uiso 1 1 calc R . .
N89 N 0.1050(3) 0.7679(3) 0.4143(2) 0.0542(10) Uani 1 1 d . . .
C90 C 0.1077(3) 0.8408(3) 0.4419(2) 0.0466(10) Uani 1 1 d . . .
N91 N 0.3010(2) 0.9686(2) 0.40928(15) 0.0410(8) Uani 1 1 d . . .
N92 N 0.3717(2) 0.9601(2) 0.38105(16) 0.0428(8) Uani 1 1 d . . .
C93 C 0.4207(3) 1.0352(3) 0.3807(2) 0.0486(11) Uani 1 1 d . . .
H93 H 0.4749 1.0483 0.3644 0.058 Uiso 1 1 calc R . .
C94 C 0.3813(3) 1.0926(3) 0.4077(2) 0.0521(12) Uani 1 1 d . . .
H94 H 0.4031 1.1501 0.4126 0.063 Uiso 1 1 calc R . .
C95 C 0.3057(3) 1.0491(3) 0.4255(2) 0.0475(11) Uani 1 1 d . . .
H95 H 0.2643 1.0705 0.4453 0.057 Uiso 1 1 calc R . .
N96 N 0.0394(3) 0.8475(3) 0.47409(18) 0.0581(11) Uani 1 1 d . . .
N97 N -0.0290(3) 0.7795(4) 0.4765(2) 0.0729(15) Uani 1 1 d . . .
C98 C -0.0797(4) 0.8090(6) 0.5114(3) 0.086(2) Uani 1 1 d . . .
H98 H -0.1324 0.7767 0.5225 0.103 Uiso 1 1 calc R . .
C99 C -0.0484(5) 0.8908(7) 0.5300(3) 0.095(3) Uani 1 1 d . . .
H99 H -0.0749 0.9241 0.5545 0.115 Uiso 1 1 calc R . .
C100 C 0.0285(4) 0.9147(5) 0.5061(3) 0.0759(18) Uani 1 1 d . . .
H100 H 0.0666 0.9679 0.5109 0.091 Uiso 1 1 calc R . .
N101 N 0.1144(3) 0.2583(4) 0.3384(2) 0.0699(14) Uani 1 1 d . A .
C102 C 0.1862(4) 0.3058(3) 0.3254(2) 0.0585(14) Uani 1 1 d . . .
N103 N 0.2046(2) 0.3870(3) 0.32602(17) 0.0484(9) Uani 1 1 d . . .
C104 C 0.1442(3) 0.4207(4) 0.3450(2) 0.0594(13) Uani 1 1 d . . .
H104 H 0.1538 0.4776 0.3455 0.071 Uiso 1 1 calc R . .
N105 N 0.0699(3) 0.3790(4) 0.3637(2) 0.0758(16) Uani 1 1 d . A .
C106 C 0.0610(4) 0.2969(5) 0.3577(3) 0.0720(18) Uani 1 1 d D . .
N107 N 0.2494(3) 0.2689(3) 0.30960(18) 0.0567(10) Uani 1 1 d . . .
N108 N 0.3258(3) 0.3148(2) 0.29531(17) 0.0509(9) Uani 1 1 d . . .
C109 C 0.3745(4) 0.2634(3) 0.2862(2) 0.0608(14) Uani 1 1 d . . .
H109 H 0.4320 0.2787 0.2753 0.073 Uiso 1 1 calc R . .
C110 C 0.3319(5) 0.1859(4) 0.2945(3) 0.0691(16) Uani 1 1 d . . .
H110 H 0.3538 0.1396 0.2904 0.083 Uiso 1 1 calc R . .
C111 C 0.2509(6) 0.1887(3) 0.3101(3) 0.079(2) Uani 1 1 d . . .
H111 H 0.2059 0.1451 0.3193 0.095 Uiso 1 1 calc R . .
N112A N -0.0144(4) 0.2437(5) 0.3716(3) 0.0520(16) Uani 0.67 1 d P A 1
N113A N -0.0750(5) 0.2745(6) 0.3984(3) 0.066(2) Uani 0.67 1 d P A 1
C114A C -0.1346(6) 0.2118(15) 0.4093(6) 0.085(7) Uani 0.67 1 d P A 1
H114A H -0.1849 0.2152 0.4283 0.102 Uiso 0.67 1 calc PR A 1
C115A C -0.1150(5) 0.1379(7) 0.3892(4) 0.071(3) Uani 0.67 1 d P A 1
H115A H -0.1481 0.0841 0.3914 0.085 Uiso 0.67 1 calc PR A 1
C116A C -0.0360(5) 0.1625(6) 0.3656(4) 0.062(2) Uani 0.67 1 d P A 1
H116A H -0.0036 0.1280 0.3484 0.074 Uiso 0.67 1 calc PR A 1
N112B N -0.0223(11) 0.2814(11) 0.3835(8) 0.072(6) Uiso 0.33 1 d PD A 2
N113B N -0.0784(11) 0.3186(12) 0.4133(8) 0.076(5) Uiso 0.33 1 d PD A 2
C114B C -0.1499(17) 0.2648(16) 0.4287(13) 0.105(10) Uiso 0.33 1 d PD A 2
H114B H -0.1975 0.2762 0.4475 0.126 Uiso 0.33 1 calc PR A 2
C115B C -0.136(2) 0.190(2) 0.4102(19) 0.093(15) Uiso 0.33 1 d PD A 2
H115B H -0.1733 0.1393 0.4161 0.111 Uiso 0.33 1 calc PR A 2
C116B C -0.0614(15) 0.1986(12) 0.3820(9) 0.071(5) Uiso 0.33 1 d PD A 2
H116B H -0.0401 0.1554 0.3646 0.085 Uiso 0.33 1 calc PR A 2
N117 N 0.9122(2) 0.4379(2) 0.11067(16) 0.0423(8) Uani 1 1 d . . .
C118 C 0.8453(3) 0.4532(3) 0.13547(18) 0.0400(9) Uani 1 1 d . . .
N119 N 0.8267(2) 0.5248(2) 0.14552(16) 0.0418(8) Uani 1 1 d . . .
C120 C 0.8864(3) 0.5858(3) 0.1279(2) 0.0473(10) Uani 1 1 d . . .
H120 H 0.8769 0.6383 0.1340 0.057 Uiso 1 1 calc R . .
N121 N 0.9568(2) 0.5793(3) 0.10296(18) 0.0497(9) Uani 1 1 d . . .
C122 C 0.9658(3) 0.5031(3) 0.0957(2) 0.0467(10) Uani 1 1 d . . .
N123 N 0.7873(2) 0.3883(2) 0.15354(15) 0.0391(8) Uani 1 1 d . . .
N124 N 0.7177(2) 0.4006(2) 0.18133(16) 0.0423(8) Uani 1 1 d . . .
C125 C 0.6740(3) 0.3275(3) 0.1918(2) 0.0487(11) Uani 1 1 d . . .
H125 H 0.6220 0.3168 0.2108 0.058 Uiso 1 1 calc R . .
C126 C 0.7153(3) 0.2682(3) 0.1708(2) 0.0501(11) Uani 1 1 d . . .
H126 H 0.6973 0.2116 0.1731 0.060 Uiso 1 1 calc R . .
C127 C 0.7862(3) 0.3083(3) 0.1465(2) 0.0476(11) Uani 1 1 d . . .
H127 H 0.8273 0.2850 0.1280 0.057 Uiso 1 1 calc R . .
N128 N 1.0368(3) 0.4924(3) 0.06779(18) 0.0524(10) Uani 1 1 d . . .
N129 N 1.0481(3) 0.4164(3) 0.0535(2) 0.0648(12) Uani 1 1 d . . .
C130 C 1.1198(4) 0.4298(5) 0.0260(3) 0.0688(16) Uani 1 1 d . . .
H130 H 1.1445 0.3882 0.0101 0.083 Uiso 1 1 calc R . .
C131 C 1.1549(3) 0.5123(5) 0.0231(2) 0.0703(17) Uani 1 1 d . . .
H131 H 1.2062 0.5363 0.0061 0.084 Uiso 1 1 calc R . .
C132 C 1.1006(3) 0.5513(4) 0.0497(2) 0.0609(14) Uani 1 1 d . . .
H132 H 1.1060 0.6081 0.0547 0.073 Uiso 1 1 calc R . .
B133 B 0.5351(3) 0.6814(3) 0.2690(2) 0.0421(11) Uani 1 1 d . . .
F134 F 0.62410(16) 0.69900(16) 0.27985(12) 0.0477(6) Uani 1 1 d . . .
F135 F 0.50562(16) 0.60996(14) 0.23056(11) 0.0445(6) Uani 1 1 d . . .
F136 F 0.49695(16) 0.67332(15) 0.32084(11) 0.0449(5) Uani 1 1 d . . .
F137 F 0.51502(16) 0.74396(15) 0.24470(11) 0.0444(5) Uani 1 1 d . . .
B138 B 0.6950(4) 0.7016(3) 0.5313(2) 0.0474(12) Uani 1 1 d . . .
F139 F 0.6161(2) 0.6834(2) 0.55428(15) 0.0743(9) Uani 1 1 d . . .
F140 F 0.6876(3) 0.6559(3) 0.47872(15) 0.0960(14) Uani 1 1 d . . .
F141 F 0.7207(2) 0.7820(2) 0.5256(3) 0.1034(16) Uani 1 1 d . . .
F142 F 0.7559(2) 0.6810(2) 0.56338(16) 0.0782(10) Uani 1 1 d . . .
B143 B 0.1013(3) 0.5947(4) 0.2543(3) 0.0615(16) Uani 1 1 d D . .
F44A F 0.0721(6) 0.5846(5) 0.3133(3) 0.083(2) Uiso 0.50 1 d PD B 1
F45A F 0.0274(4) 0.5833(4) 0.2196(3) 0.0522(19) Uiso 0.50 1 d PD B 1
F46A F 0.1424(4) 0.5367(4) 0.2411(3) 0.0647(16) Uiso 0.50 1 d PD B 1
F47A F 0.1530(4) 0.6743(4) 0.2640(3) 0.0524(17) Uiso 0.50 1 d PD B 1
F44B F 0.1086(6) 0.5766(5) 0.3061(3) 0.080(2) Uiso 0.50 1 d PD B 2
F45B F 0.0180(4) 0.5831(5) 0.2354(3) 0.059(2) Uiso 0.50 1 d PD B 2
F46B F 0.1384(4) 0.5426(4) 0.2139(3) 0.0691(18) Uiso 0.50 1 d PD B 2
F47B F 0.1512(5) 0.6735(4) 0.2450(4) 0.070(2) Uiso 0.50 1 d PD B 2
B148A B 0.3538(9) 0.6732(9) 0.0111(5) 0.050(6) Uiso 0.50 1 d PD C 1
F149A F 0.3648(5) 0.6059(5) 0.0322(3) 0.0692(18) Uiso 0.50 1 d PD C 1
F150A F 0.3177(7) 0.7205(7) 0.0482(4) 0.109(3) Uiso 0.50 1 d PD C 1
F151A F 0.4317(6) 0.7204(6) -0.0063(4) 0.072(3) Uiso 0.50 1 d PD C 1
F152A F 0.3067(5) 0.6547(5) -0.0393(3) 0.051(2) Uiso 0.50 1 d PD C 1
B148B B 0.3606(9) 0.6861(9) 0.0103(6) 0.057(6) Uiso 0.50 1 d PD D 2
F149B F 0.3580(4) 0.6323(4) 0.0515(3) 0.0538(14) Uiso 0.50 1 d PD D 2
F150B F 0.3378(4) 0.7523(4) 0.0397(3) 0.0575(15) Uiso 0.50 1 d PD D 2
F151B F 0.4455(4) 0.7085(5) -0.0048(3) 0.050(2) Uiso 0.50 1 d PD D 2
F152B F 0.2971(5) 0.6398(6) -0.0336(3) 0.058(3) Uiso 0.50 1 d PD D 2
B153 B 0.7517(4) 0.7262(4) 0.0341(2) 0.0510(12) Uani 1 1 d . . .
F154 F 0.8066(3) 0.7177(3) 0.07782(18) 0.0946(13) Uani 1 1 d . . .
F155 F 0.7202(2) 0.79080(19) 0.05465(14) 0.0663(8) Uani 1 1 d . . .
F156 F 0.6890(3) 0.6547(2) 0.02250(16) 0.0815(11) Uani 1 1 d . . .
F157 F 0.7971(2) 0.7422(2) -0.01328(15) 0.0781(10) Uani 1 1 d . . .
B158A B 0.5126(9) 1.0999(8) 0.2324(6) 0.056(5) Uiso 0.50 1 d PD E 1
F159A F 0.4497(6) 1.0719(6) 0.1873(4) 0.100(3) Uiso 0.50 1 d PD E 1
F160A F 0.5895(5) 1.1294(5) 0.2049(4) 0.088(2) Uiso 0.50 1 d PD E 1
F161A F 0.5056(7) 1.1600(6) 0.2739(4) 0.110(3) Uiso 0.50 1 d PD E 1
F162A F 0.5213(6) 1.0331(6) 0.2560(4) 0.065(3) Uiso 0.50 1 d PD E 1
B158B B 0.5120(7) 1.1074(8) 0.2232(6) 0.046(4) Uiso 0.50 1 d PD F 2
F159B F 0.4250(4) 1.0810(4) 0.2088(3) 0.0632(16) Uiso 0.50 1 d PD F 2
F160B F 0.5571(5) 1.1156(5) 0.1746(3) 0.0739(18) Uiso 0.50 1 d PD F 2
F161B F 0.5296(5) 1.1855(4) 0.2548(3) 0.0687(17) Uiso 0.50 1 d PD F 2
F162B F 0.5364(6) 1.0528(6) 0.2544(4) 0.071(3) Uiso 0.50 1 d PD F 2
B163 B 0.6669(4) 1.0471(4) 0.4331(3) 0.0544(13) Uani 1 1 d . . .
F164 F 0.6005(3) 0.9943(2) 0.45532(18) 0.0844(11) Uani 1 1 d . . .
F165 F 0.7338(2) 1.0102(2) 0.4224(2) 0.0999(15) Uani 1 1 d . . .
F166 F 0.6386(3) 1.0610(3) 0.38185(16) 0.0987(13) Uani 1 1 d . . .
F167 F 0.6989(2) 1.1173(2) 0.47007(14) 0.0688(9) Uani 1 1 d . . .
B168 B 0.1190(3) 0.9729(4) 0.3103(2) 0.0505(13) Uani 1 1 d . . .
F169 F 0.0861(2) 0.8974(2) 0.32737(14) 0.0651(8) Uani 1 1 d . . .
F170 F 0.20495(18) 0.9826(2) 0.29853(14) 0.0663(8) Uani 1 1 d . . .
F171 F 0.0735(2) 0.9769(2) 0.26134(14) 0.0725(9) Uani 1 1 d . . .
F172 F 0.1140(2) 1.0334(2) 0.35294(16) 0.0774(10) Uani 1 1 d . . .
N173 N -0.1283(7) 0.4625(7) 0.4724(4) 0.069(2) Uiso 0.50 1 d P G 1
N174 N -0.0733(6) 0.4457(6) 0.4314(4) 0.064(2) Uiso 0.50 1 d P G 1
H174 H -0.0757 0.3968 0.4137 0.076 Uiso 0.50 1 calc PR G 1
C175 C -0.0175(8) 0.5126(7) 0.4227(5) 0.062(3) Uiso 0.50 1 d P G 1
H175 H 0.0300 0.5123 0.3998 0.074 Uiso 0.50 1 calc PR G 1
C176 C -0.0316(7) 0.5795(8) 0.4476(5) 0.062(3) Uiso 0.50 1 d P G 1
H176 H 0.0008 0.6343 0.4478 0.074 Uiso 0.50 1 calc PR G 1
C177 C -0.1091(11) 0.5484(11) 0.4745(7) 0.094(4) Uiso 0.50 1 d P G 1
H177 H -0.1435 0.5809 0.4916 0.113 Uiso 0.50 1 calc PR G 1
B178 B -0.2011(9) 0.4008(9) 0.5036(6) 0.065(3) Uiso 0.50 1 d P G 1
F179 F -0.1958(5) 0.4338(6) 0.5564(4) 0.084(2) Uiso 0.50 1 d P G 1
F180 F -0.2771(4) 0.3894(4) 0.4770(3) 0.0613(15) Uiso 0.50 1 d P G 1
F181 F -0.1759(5) 0.3313(5) 0.5008(3) 0.0748(18) Uiso 0.50 1 d P G 1
C182 C 0.6409(7) 0.2449(6) 0.3616(4) 0.079(2) Uiso 0.70 1 d P . .
H18A H 0.5880 0.2020 0.3640 0.118 Uiso 0.70 1 calc PR . .
H18B H 0.6755 0.2561 0.3976 0.118 Uiso 0.70 1 calc PR . .
H18C H 0.6736 0.2270 0.3305 0.118 Uiso 0.70 1 calc PR . .
C183 C 0.6200(5) 0.3166(5) 0.3509(4) 0.0601(18) Uiso 0.70 1 d P . .
N184 N 0.5988(6) 0.3694(6) 0.3402(4) 0.088(2) Uiso 0.70 1 d P . .
C185 C 0.3840(5) 0.1876(5) 0.0741(3) 0.080(3) Uani 0.80 1 d P . .
H18D H 0.3236 0.1872 0.0694 0.120 Uiso 0.80 1 calc PR . .
H18E H 0.3877 0.1331 0.0789 0.120 Uiso 0.80 1 calc PR . .
H18F H 0.4137 0.2039 0.0403 0.120 Uiso 0.80 1 calc PR . .
C186 C 0.4243(4) 0.2453(4) 0.1242(3) 0.0458(12) Uani 0.80 1 d P . .
N187 N 0.4546(3) 0.2915(3) 0.1622(2) 0.0468(11) Uani 0.80 1 d P . .
C188 C 0.2293(5) 0.0424(5) 0.1679(4) 0.0618(19) Uiso 0.70 1 d P . .
H18G H 0.2074 0.0217 0.2027 0.093 Uiso 0.70 1 calc PR . .
H18H H 0.2917 0.0517 0.1689 0.093 Uiso 0.70 1 calc PR . .
H18I H 0.2029 0.0024 0.1347 0.093 Uiso 0.70 1 calc PR . .
C189 C 0.2093(6) 0.1142(6) 0.1644(4) 0.065(2) Uiso 0.70 1 d P . .
N190 N 0.1883(6) 0.1734(6) 0.1653(4) 0.092(2) Uiso 0.70 1 d P . .
C191 C 1.0999(4) 0.8034(4) 0.1965(3) 0.0744(17) Uani 1 1 d . . .
H19A H 1.1153 0.7580 0.1737 0.112 Uiso 1 1 calc R . .
H19B H 1.1330 0.8173 0.2333 0.112 Uiso 1 1 calc R . .
H19C H 1.1130 0.8507 0.1763 0.112 Uiso 1 1 calc R . .
C192 C 1.0091(3) 0.7799(3) 0.2059(2) 0.0517(11) Uani 1 1 d . . .
N193 N 0.9378(3) 0.7617(3) 0.2120(2) 0.0562(10) Uani 1 1 d . . .
C194 C 0.8034(6) 0.9783(5) 0.0264(4) 0.090(2) Uiso 0.90 1 d P . .
H19D H 0.7825 0.9245 0.0381 0.135 Uiso 0.90 1 calc PR . .
H19E H 0.8645 0.9886 0.0194 0.135 Uiso 0.90 1 calc PR . .
H19F H 0.7712 0.9802 -0.0086 0.135 Uiso 0.90 1 calc PR . .
C195 C 0.7911(5) 1.0417(5) 0.0724(3) 0.0736(18) Uiso 0.90 1 d P . .
N196 N 0.7799(4) 1.0886(4) 0.1066(3) 0.0827(17) Uiso 0.90 1 d P . .
C197 C 0.4043(6) 0.8792(5) -0.0497(4) 0.085(3) Uani 0.80 1 d P . .
H19G H 0.4580 0.8665 -0.0404 0.127 Uiso 0.80 1 calc PR . .
H19H H 0.4095 0.9041 -0.0847 0.127 Uiso 0.80 1 calc PR . .
H19I H 0.3571 0.8291 -0.0554 0.127 Uiso 0.80 1 calc PR . .
C198 C 0.3869(6) 0.9349(5) -0.0039(4) 0.082(3) Uani 0.80 1 d P . .
N199 N 0.3775(6) 0.9799(5) 0.0327(4) 0.101(3) Uani 0.80 1 d P . .
C200 C 0.1461(8) 0.7588(8) -0.0063(6) 0.070(3) Uiso 0.50 1 d P . .
H20A H 0.0960 0.7447 -0.0334 0.105 Uiso 0.50 1 calc PR . .
H20B H 0.1486 0.7108 0.0108 0.105 Uiso 0.50 1 calc PR . .
H20C H 0.1985 0.7773 -0.0263 0.105 Uiso 0.50 1 calc PR . .
C201 C 0.1394(7) 0.8218(7) 0.0370(5) 0.054(2) Uiso 0.50 1 d P . .
N202 N 0.1310(8) 0.8746(8) 0.0676(6) 0.087(3) Uiso 0.50 1 d P . .
C203 C 1.0438(12) 1.2369(10) 0.1016(7) 0.061(4) Uiso 0.30 1 d PD . .
H20D H 1.0603 1.2243 0.1385 0.091 Uiso 0.30 1 calc PR . .
H20E H 0.9901 1.2529 0.1043 0.091 Uiso 0.30 1 calc PR . .
H20F H 1.0891 1.2816 0.0908 0.091 Uiso 0.30 1 calc PR . .
C204 C 1.0312(11) 1.1637(10) 0.0577(7) 0.055(4) Uiso 0.30 1 d PD . .
N205 N 1.0217(12) 1.1076(10) 0.0285(8) 0.078(5) Uiso 0.30 1 d PD . .
C206 C -0.1079(12) 0.411(2) 0.5589(15) 0.075(8) Uiso 0.20 1 d PD H 2
H20G H -0.0945 0.3972 0.5194 0.112 Uiso 0.20 1 calc PR H 2
H20H H -0.0820 0.3823 0.5837 0.112 Uiso 0.20 1 calc PR H 2
H20I H -0.0849 0.4702 0.5707 0.112 Uiso 0.20 1 calc PR H 2
C207 C -0.2016(9) 0.3885(11) 0.5630(7) 0.026(3) Uiso 0.20 1 d PD H 2
N208 N -0.2654(11) 0.3582(14) 0.5785(10) 0.058(5) Uiso 0.20 1 d PD H 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 N7 2.263(3) . ?
Fe1 N12 2.097(4) . ?
Fe1 N57 2.210(3) . ?
Fe1 N65 2.089(3) . ?
Fe1 N71 2.158(4) . ?
Fe1 N76 2.114(4) . ?
Fe2 N9 2.289(3) . ?
Fe2 N17 2.112(4) . ?
Fe2 N23 2.296(3) . ?
Fe2 N28 2.118(4) . ?
Fe2 N87 2.175(4) . ?
Fe2 N92 2.107(4) . ?
Fe3 N25 2.325(4) . ?
Fe3 N33 2.109(4) . ?
Fe3 N39 2.256(4) . ?
Fe3 N44 2.113(4) . ?
Fe3 N103 2.177(4) . ?
Fe3 N108 2.112(4) . ?
Fe4 N41 2.263(4) . ?
Fe4 N49 2.137(4) . ?
Fe4 N55 2.276(3) . ?
Fe4 N60 2.116(3) . ?
Fe4 N119 2.179(4) . ?
Fe4 N124 2.125(4) . ?
N5 C6 1.323(6) . ?
N5 C10 1.321(5) . ?
C6 N7 1.344(5) . ?
C6 N11 1.382(5) . ?
N7 C8 1.334(5) . ?
C8 H8 0.9500 . ?
C8 N9 1.342(6) . ?
N9 C10 1.344(5) . ?
C10 N16 1.378(6) . ?
N11 N12 1.368(5) . ?
N11 C15 1.360(6) . ?
N12 C13 1.326(5) . ?
C13 H13 0.9500 . ?
C13 C14 1.389(7) . ?
C14 H14 0.9500 . ?
C14 C15 1.359(7) . ?
C15 H15 0.9500 . ?
N16 N17 1.370(5) . ?
N16 C20 1.365(6) . ?
N17 C18 1.337(6) . ?
C18 H18 0.9500 . ?
C18 C19 1.411(8) . ?
C19 H19 0.9500 . ?
C19 C20 1.370(7) . ?
C20 H20 0.9500 . ?
N21 C22 1.317(5) . ?
N21 C26 1.322(5) . ?
C22 N23 1.337(5) . ?
C22 N27 1.386(6) . ?
N23 C24 1.335(6) . ?
C24 H24 0.9500 . ?
C24 N25 1.340(5) . ?
N25 C26 1.336(5) . ?
C26 N32 1.391(5) . ?
N27 N28 1.367(5) . ?
N27 C31 1.358(6) . ?
N28 C29 1.327(6) . ?
C29 H29 0.9500 . ?
C29 C30 1.402(7) . ?
C30 H30 0.9500 . ?
C30 C31 1.375(7) . ?
C31 H31 0.9500 . ?
N32 N33 1.371(5) . ?
N32 C36 1.351(6) . ?
N33 C34 1.318(5) . ?
C34 H34 0.9500 . ?
C34 C35 1.406(7) . ?
C35 H35 0.9500 . ?
C35 C36 1.356(7) . ?
C36 H36 0.9500 . ?
N37 C38 1.317(6) . ?
N37 C42 1.311(6) . ?
C38 N39 1.345(5) . ?
C38 N43 1.381(6) . ?
N39 C40 1.326(6) . ?
C40 H40 0.9500 . ?
C40 N41 1.338(6) . ?
N41 C42 1.336(5) . ?
C42 N48 1.389(6) . ?
N43 N44 1.364(5) . ?
N43 C47 1.366(6) . ?
N44 C45 1.319(6) . ?
C45 H45 0.9500 . ?
C45 C46 1.405(8) . ?
C46 H46 0.9500 . ?
C46 C47 1.342(8) . ?
C47 H47 0.9500 . ?
N48 N49 1.369(6) . ?
N48 C52 1.368(6) . ?
N49 C50 1.326(6) . ?
C50 H50 0.9500 . ?
C50 C51 1.406(8) . ?
C51 H51 0.9500 . ?
C51 C52 1.352(8) . ?
C52 H52 0.9500 . ?
N53 C54 1.318(5) . ?
N53 C58 1.310(5) . ?
C54 N55 1.341(5) . ?
C54 N59 1.376(5) . ?
N55 C56 1.329(5) . ?
C56 H56 0.9500 . ?
C56 N57 1.326(5) . ?
N57 C58 1.344(5) . ?
C58 N64 1.378(5) . ?
N59 N60 1.376(5) . ?
N59 C63 1.368(5) . ?
N60 C61 1.321(5) . ?
C61 H61 0.9500 . ?
C61 C62 1.404(7) . ?
C62 H62 0.9500 . ?
C62 C63 1.349(7) . ?
C63 H63 0.9500 . ?
N64 N65 1.375(5) . ?
N64 C68 1.362(5) . ?
N65 C66 1.322(5) . ?
C66 H66 0.9500 . ?
C66 C67 1.410(7) . ?
C67 H67 0.9500 . ?
C67 C68 1.373(7) . ?
C68 H68 0.9500 . ?
N69 C70 1.323(7) . ?
N69 C74 1.292(7) . ?
C70 N71 1.355(7) . ?
C70 N75 1.374(7) . ?
N71 C72 1.326(7) . ?
C72 H72 0.9500 . ?
C72 N73 1.356(7) . ?
N73 C74 1.329(8) . ?
C74 N80 1.402(7) . ?
N75 N76 1.352(6) . ?
N75 C79 1.375(7) . ?
N76 C77 1.331(6) . ?
C77 H77 0.9500 . ?
C77 C78 1.407(8) . ?
C78 H78 0.9500 . ?
C78 C79 1.351(8) . ?
C79 H79 0.9500 . ?
N80 N81 1.383(8) . ?
N80 C84 1.346(8) . ?
N81 C82 1.330(8) . ?
C82 H82 0.9500 . ?
C82 C83 1.419(11) . ?
C83 H83 0.9500 . ?
C83 C84 1.317(10) . ?
C84 H84 0.9500 . ?
N85 C86 1.319(5) . ?
N85 C90 1.340(7) . ?
C86 N87 1.339(5) . ?
C86 N91 1.372(6) . ?
N87 C88 1.341(6) . ?
C88 H88 0.9500 . ?
C88 N89 1.328(6) . ?
N89 C90 1.325(7) . ?
C90 N96 1.379(6) . ?
N91 N92 1.369(5) . ?
N91 C95 1.370(6) . ?
N92 C93 1.328(6) . ?
C93 H93 0.9500 . ?
C93 C94 1.405(7) . ?
C94 H94 0.9500 . ?
C94 C95 1.364(8) . ?
C95 H95 0.9500 . ?
N96 N97 1.391(7) . ?
N96 C100 1.350(8) . ?
N97 C98 1.325(9) . ?
C98 H98 0.9500 . ?
C98 C99 1.372(12) . ?
C99 H99 0.9500 . ?
C99 C100 1.365(10) . ?
C100 H100 0.9500 . ?
N101 C102 1.303(7) . ?
N101 C106 1.280(9) . ?
C102 N103 1.348(7) . ?
C102 N107 1.375(8) . ?
N103 C104 1.322(7) . ?
C104 H104 0.9500 . ?
C104 N105 1.345(7) . ?
N105 C106 1.372(10) . ?
C106 N112A 1.395(9) . ?
C106 N112B 1.469(15) . ?
N107 N108 1.357(6) . ?
N107 C111 1.392(7) . ?
N108 C109 1.332(7) . ?
C109 H109 0.9500 . ?
C109 C110 1.374(9) . ?
C110 H110 0.9500 . ?
C110 C111 1.382(10) . ?
C111 H111 0.9500 . ?
N112A N113A 1.364(11) . ?
N112A C116A 1.336(14) . ?
N113A C114A 1.304(19) . ?
C114A H114A 0.9500 . ?
C114A C115A 1.42(2) . ?
C115A H115A 0.9500 . ?
C115A C116A 1.392(12) . ?
C116A H116A 0.9500 . ?
N112B N113B 1.396(16) . ?
N112B C116B 1.394(17) . ?
N113B C114B 1.369(18) . ?
C114B H114B 0.9500 . ?
C114B C115B 1.38(2) . ?
C115B H115B 0.9500 . ?
C115B C116B 1.378(19) . ?
C116B H116B 0.9500 . ?
N117 C118 1.314(6) . ?
N117 C122 1.321(7) . ?
C118 N119 1.338(5) . ?
C118 N123 1.381(6) . ?
N119 C120 1.345(6) . ?
C120 H120 0.9500 . ?
C120 N121 1.319(6) . ?
N121 C122 1.348(6) . ?
C122 N128 1.380(6) . ?
N123 N124 1.367(5) . ?
N123 C127 1.361(6) . ?
N124 C125 1.330(6) . ?
C125 H125 0.9500 . ?
C125 C126 1.407(7) . ?
C126 H126 0.9500 . ?
C126 C127 1.358(7) . ?
C127 H127 0.9500 . ?
N128 N129 1.370(6) . ?
N128 C132 1.365(7) . ?
N129 C130 1.327(8) . ?
C130 H130 0.9500 . ?
C130 C131 1.396(10) . ?
C131 H131 0.9500 . ?
C131 C132 1.357(9) . ?
C132 H132 0.9500 . ?
B133 F134 1.401(5) . ?
B133 F135 1.394(5) . ?
B133 F136 1.395(6) . ?
B133 F137 1.396(6) . ?
B138 F139 1.375(7) . ?
B138 F140 1.366(6) . ?
B138 F141 1.364(7) . ?
B138 F142 1.381(6) . ?
B143 F44A 1.506(9) . ?
B143 F45A 1.391(8) . ?
B143 F46A 1.349(8) . ?
B143 F47A 1.389(8) . ?
B143 F44B 1.322(9) . ?
B143 F45B 1.367(8) . ?
B143 F46B 1.470(9) . ?
B143 F47B 1.433(9) . ?
B148A F149A 1.377(14) . ?
B148A F150A 1.364(13) . ?
B148A F151A 1.411(14) . ?
B148A F152A 1.358(13) . ?
B148B F149B 1.431(15) . ?
B148B F150B 1.392(14) . ?
B148B F151B 1.394(14) . ?
B148B F152B 1.438(14) . ?
B153 F154 1.401(7) . ?
B153 F155 1.380(6) . ?
B153 F156 1.362(7) . ?
B153 F157 1.375(7) . ?
B158A F159A 1.402(14) . ?
B158A F160A 1.424(14) . ?
B158A F161A 1.358(13) . ?
B158A F162A 1.385(15) . ?
B158B F159B 1.379(12) . ?
B158B F160B 1.384(13) . ?
B158B F161B 1.402(12) . ?
B158B F162B 1.403(14) . ?
B163 F164 1.377(7) . ?
B163 F165 1.405(7) . ?
B163 F166 1.363(8) . ?
B163 F167 1.365(6) . ?
B168 F169 1.388(7) . ?
B168 F170 1.395(6) . ?
B168 F171 1.381(6) . ?
B168 F172 1.371(7) . ?
N173 N174 1.386(14) . ?
N173 C177 1.42(2) . ?
N173 B178 1.629(18) . ?
N174 H174 0.8800 . ?
N174 C175 1.308(15) . ?
C175 H175 0.9500 . ?
C175 C176 1.300(16) . ?
C176 H176 0.9500 . ?
C176 C177 1.43(2) . ?
C177 H177 0.9500 . ?
B178 F179 1.296(16) . ?
B178 F180 1.325(15) . ?
B178 F181 1.358(16) . ?
C182 H18A 0.9800 . ?
C182 H18B 0.9800 . ?
C182 H18C 0.9800 . ?
C182 C183 1.418(13) . ?
C183 N184 1.112(11) . ?
C185 H18D 0.9800 . ?
C185 H18E 0.9800 . ?
C185 H18F 0.9800 . ?
C185 C186 1.459(9) . ?
C186 N187 1.125(8) . ?
C188 H18G 0.9800 . ?
C188 H18H 0.9800 . ?
C188 H18I 0.9800 . ?
C188 C189 1.373(12) . ?
C189 N190 1.155(12) . ?
C191 H19A 0.9800 . ?
C191 H19B 0.9800 . ?
C191 H19C 0.9800 . ?
C191 C192 1.448(8) . ?
C192 N193 1.131(7) . ?
C194 H19D 0.9800 . ?
C194 H19E 0.9800 . ?
C194 H19F 0.9800 . ?
C194 C195 1.491(11) . ?
C195 N196 1.117(9) . ?
C197 H19G 0.9800 . ?
C197 H19H 0.9800 . ?
C197 H19I 0.9800 . ?
C197 C198 1.432(14) . ?
C198 N199 1.126(12) . ?
C200 H20A 0.9800 . ?
C200 H20B 0.9800 . ?
C200 H20C 0.9800 . ?
C200 C201 1.418(16) . ?
C201 N202 1.124(16) . ?
C203 H20D 0.9800 . ?
C203 H20E 0.9800 . ?
C203 H20F 0.9800 . ?
C203 C204 1.488(14) . ?
C204 N205 1.082(14) . ?
C206 H20G 0.9800 . ?
C206 H20H 0.9800 . ?
C206 H20I 0.9800 . ?
C206 C207 1.471(16) . ?
C207 N208 1.121(15) . ?

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
N12 Fe1 N7 74.21(13) . . ?
N12 Fe1 N57 95.92(13) . . ?
N12 Fe1 N71 97.12(14) . . ?
N12 Fe1 N76 92.75(15) . . ?
N57 Fe1 N7 95.05(13) . . ?
N65 Fe1 N7 91.97(13) . . ?
N65 Fe1 N12 163.13(14) . . ?
N65 Fe1 N57 75.32(13) . . ?
N65 Fe1 N71 94.43(14) . . ?
N65 Fe1 N76 101.97(15) . . ?
N71 Fe1 N7 98.54(14) . . ?
N71 Fe1 N57 163.27(14) . . ?
N76 Fe1 N7 165.31(14) . . ?
N76 Fe1 N57 92.97(14) . . ?
N76 Fe1 N71 76.01(16) . . ?
N9 Fe2 N23 96.04(12) . . ?
N17 Fe2 N9 74.01(14) . . ?
N17 Fe2 N23 91.25(13) . . ?
N17 Fe2 N28 158.74(13) . . ?
N17 Fe2 N87 92.55(14) . . ?
N28 Fe2 N9 93.02(13) . . ?
N28 Fe2 N23 73.10(13) . . ?
N28 Fe2 N87 103.25(14) . . ?
N87 Fe2 N9 161.77(14) . . ?
N87 Fe2 N23 96.52(13) . . ?
N92 Fe2 N9 94.61(13) . . ?
N92 Fe2 N17 101.83(15) . . ?
N92 Fe2 N23 165.01(14) . . ?
N92 Fe2 N28 95.84(14) . . ?
N92 Fe2 N87 75.81(14) . . ?
N33 Fe3 N25 72.68(13) . . ?
N33 Fe3 N39 96.31(13) . . ?
N33 Fe3 N44 159.93(15) . . ?
N33 Fe3 N103 99.69(14) . . ?
N33 Fe3 N108 94.18(15) . . ?
N39 Fe3 N25 93.27(12) . . ?
N44 Fe3 N25 89.94(13) . . ?
N44 Fe3 N39 74.23(14) . . ?
N44 Fe3 N103 93.10(15) . . ?
N103 Fe3 N25 100.19(14) . . ?
N103 Fe3 N39 161.55(14) . . ?
N108 Fe3 N25 165.87(14) . . ?
N108 Fe3 N39 93.37(15) . . ?
N108 Fe3 N44 103.87(15) . . ?
N108 Fe3 N103 76.43(17) . . ?
N41 Fe4 N55 94.69(13) . . ?
N49 Fe4 N41 73.64(14) . . ?
N49 Fe4 N55 91.45(13) . . ?
N49 Fe4 N119 92.60(14) . . ?
N60 Fe4 N41 91.68(13) . . ?
N60 Fe4 N49 158.13(14) . . ?
N60 Fe4 N55 73.32(13) . . ?
N60 Fe4 N119 105.11(14) . . ?
N60 Fe4 N124 92.74(14) . . ?
N119 Fe4 N41 160.56(13) . . ?
N119 Fe4 N55 99.42(13) . . ?
N124 Fe4 N41 94.11(14) . . ?
N124 Fe4 N49 104.19(14) . . ?
N124 Fe4 N55 163.71(14) . . ?
N124 Fe4 N119 75.68(14) . . ?
C10 N5 C6 112.7(4) . . ?
N5 C6 N7 127.3(4) . . ?
N5 C6 N11 116.5(4) . . ?
N7 C6 N11 116.2(4) . . ?
C6 N7 Fe1 113.0(3) . . ?
C8 N7 Fe1 132.4(3) . . ?
C8 N7 C6 113.7(4) . . ?
N7 C8 H8 117.4 . . ?
N7 C8 N9 125.2(4) . . ?
N9 C8 H8 117.4 . . ?
C8 N9 Fe2 132.5(3) . . ?
C8 N9 C10 113.6(3) . . ?
C10 N9 Fe2 113.3(3) . . ?
N5 C10 N9 127.4(4) . . ?
N5 C10 N16 116.5(4) . . ?
N9 C10 N16 116.1(4) . . ?
N12 N11 C6 118.7(3) . . ?
C15 N11 C6 129.7(4) . . ?
C15 N11 N12 111.4(3) . . ?
N11 N12 Fe1 116.7(2) . . ?
C13 N12 Fe1 138.7(3) . . ?
C13 N12 N11 104.5(4) . . ?
N12 C13 H13 124.3 . . ?
N12 C13 C14 111.4(4) . . ?
C14 C13 H13 124.3 . . ?
C13 C14 H14 126.9 . . ?
C15 C14 C13 106.2(4) . . ?
C15 C14 H14 126.9 . . ?
N11 C15 H15 126.8 . . ?
C14 C15 N11 106.5(4) . . ?
C14 C15 H15 126.8 . . ?
N17 N16 C10 119.9(4) . . ?
C20 N16 C10 128.2(4) . . ?
C20 N16 N17 111.9(4) . . ?
N16 N17 Fe2 116.5(3) . . ?
C18 N17 Fe2 139.0(3) . . ?
C18 N17 N16 104.5(4) . . ?
N17 C18 H18 124.3 . . ?
N17 C18 C19 111.4(4) . . ?
C19 C18 H18 124.3 . . ?
C18 C19 H19 127.3 . . ?
C20 C19 C18 105.5(5) . . ?
C20 C19 H19 127.3 . . ?
N16 C20 C19 106.7(4) . . ?
N16 C20 H20 126.6 . . ?
C19 C20 H20 126.6 . . ?
C22 N21 C26 112.0(4) . . ?
N21 C22 N23 128.0(4) . . ?
N21 C22 N27 116.1(4) . . ?
N23 C22 N27 115.9(4) . . ?
C22 N23 Fe2 113.8(3) . . ?
C24 N23 Fe2 132.1(3) . . ?
C24 N23 C22 113.4(3) . . ?
N23 C24 H24 117.3 . . ?
N23 C24 N25 125.3(4) . . ?
N25 C24 H24 117.3 . . ?
C24 N25 Fe3 132.7(3) . . ?
C26 N25 Fe3 113.3(3) . . ?
C26 N25 C24 113.2(4) . . ?
N21 C26 N25 128.0(4) . . ?
N21 C26 N32 115.9(4) . . ?
N25 C26 N32 116.0(4) . . ?
N28 N27 C22 119.0(3) . . ?
C31 N27 C22 129.3(4) . . ?
C31 N27 N28 111.8(4) . . ?
N27 N28 Fe2 117.4(3) . . ?
C29 N28 Fe2 137.6(3) . . ?
C29 N28 N27 104.8(4) . . ?
N28 C29 H29 124.3 . . ?
N28 C29 C30 111.5(4) . . ?
C30 C29 H29 124.3 . . ?
C29 C30 H30 127.3 . . ?
C31 C30 C29 105.5(4) . . ?
C31 C30 H30 127.3 . . ?
N27 C31 C30 106.5(4) . . ?
N27 C31 H31 126.8 . . ?
C30 C31 H31 126.8 . . ?
N33 N32 C26 118.6(3) . . ?
C36 N32 C26 129.7(4) . . ?
C36 N32 N33 111.6(3) . . ?
N32 N33 Fe3 118.2(2) . . ?
C34 N33 Fe3 137.2(3) . . ?
C34 N33 N32 104.5(4) . . ?
N33 C34 H34 124.2 . . ?
N33 C34 C35 111.5(4) . . ?
C35 C34 H34 124.2 . . ?
C34 C35 H35 127.3 . . ?
C36 C35 C34 105.4(4) . . ?
C36 C35 H35 127.3 . . ?
N32 C36 C35 107.0(4) . . ?
N32 C36 H36 126.5 . . ?
C35 C36 H36 126.5 . . ?
C42 N37 C38 112.7(4) . . ?
N37 C38 N39 127.0(4) . . ?
N37 C38 N43 117.0(4) . . ?
N39 C38 N43 115.9(4) . . ?
C38 N39 Fe3 113.6(3) . . ?
C40 N39 Fe3 132.2(3) . . ?
C40 N39 C38 113.8(4) . . ?
N39 C40 H40 117.4 . . ?
N39 C40 N41 125.3(4) . . ?
N41 C40 H40 117.4 . . ?
C40 N41 Fe4 131.5(3) . . ?
C42 N41 Fe4 114.6(3) . . ?
C42 N41 C40 113.3(4) . . ?
N37 C42 N41 128.0(4) . . ?
N37 C42 N48 116.4(4) . . ?
N41 C42 N48 115.7(4) . . ?
N44 N43 C38 119.4(3) . . ?
N44 N43 C47 111.1(4) . . ?
C47 N43 C38 129.5(4) . . ?
N43 N44 Fe3 116.0(3) . . ?
C45 N44 Fe3 139.0(4) . . ?
C45 N44 N43 104.9(4) . . ?
N44 C45 H45 124.4 . . ?
N44 C45 C46 111.2(5) . . ?
C46 C45 H45 124.4 . . ?
C45 C46 H46 127.0 . . ?
C47 C46 C45 105.9(5) . . ?
C47 C46 H46 127.0 . . ?
N43 C47 H47 126.5 . . ?
C46 C47 N43 107.0(5) . . ?
C46 C47 H47 126.5 . . ?
N49 N48 C42 119.3(3) . . ?
C52 N48 C42 129.6(4) . . ?
C52 N48 N49 111.1(4) . . ?
N48 N49 Fe4 115.9(3) . . ?
C50 N49 Fe4 138.6(4) . . ?
C50 N49 N48 105.1(4) . . ?
N49 C50 H50 124.6 . . ?
N49 C50 C51 110.8(5) . . ?
C51 C50 H50 124.6 . . ?
C50 C51 H51 126.9 . . ?
C52 C51 C50 106.3(4) . . ?
C52 C51 H51 126.9 . . ?
N48 C52 H52 126.7 . . ?
C51 C52 N48 106.7(5) . . ?
C51 C52 H52 126.7 . . ?
C58 N53 C54 112.9(3) . . ?
N53 C54 N55 127.4(4) . . ?
N53 C54 N59 116.8(3) . . ?
N55 C54 N59 115.8(3) . . ?
C54 N55 Fe4 114.0(3) . . ?
C56 N55 Fe4 131.6(3) . . ?
C56 N55 C54 113.5(3) . . ?
N55 C56 H56 117.4 . . ?
N57 C56 N55 125.2(4) . . ?
N57 C56 H56 117.4 . . ?
C56 N57 Fe1 131.8(3) . . ?
C56 N57 C58 114.2(3) . . ?
C58 N57 Fe1 113.8(3) . . ?
N53 C58 N57 126.8(4) . . ?
N53 C58 N64 117.0(3) . . ?
N57 C58 N64 116.2(3) . . ?
C54 N59 N60 118.9(3) . . ?
C63 N59 C54 130.3(4) . . ?
C63 N59 N60 110.8(3) . . ?
N59 N60 Fe4 116.5(2) . . ?
C61 N60 Fe4 137.7(3) . . ?
C61 N60 N59 104.9(3) . . ?
N60 C61 H61 124.4 . . ?
N60 C61 C62 111.3(4) . . ?
C62 C61 H61 124.4 . . ?
C61 C62 H62 126.9 . . ?
C63 C62 C61 106.1(4) . . ?
C63 C62 H62 126.9 . . ?
N59 C63 H63 126.5 . . ?
C62 C63 N59 106.9(4) . . ?
C62 C63 H63 126.5 . . ?
N65 N64 C58 118.5(3) . . ?
C68 N64 C58 129.4(4) . . ?
C68 N64 N65 112.0(3) . . ?
N64 N65 Fe1 115.6(2) . . ?
C66 N65 Fe1 139.3(3) . . ?
C66 N65 N64 105.0(3) . . ?
N65 C66 H66 124.6 . . ?
N65 C66 C67 110.8(4) . . ?
C67 C66 H66 124.6 . . ?
C66 C67 H67 126.8 . . ?
C68 C67 C66 106.5(4) . . ?
C68 C67 H67 126.8 . . ?
N64 C68 C67 105.7(4) . . ?
N64 C68 H68 127.2 . . ?
C67 C68 H68 127.2 . . ?
C74 N69 C70 113.0(5) . . ?
N69 C70 N71 126.3(5) . . ?
N69 C70 N75 117.3(5) . . ?
N71 C70 N75 116.5(4) . . ?
C70 N71 Fe1 113.9(3) . . ?
C72 N71 Fe1 131.6(4) . . ?
C72 N71 C70 114.5(5) . . ?
N71 C72 H72 118.1 . . ?
N71 C72 N73 123.8(6) . . ?
N73 C72 H72 118.1 . . ?
C74 N73 C72 113.8(5) . . ?
N69 C74 N73 128.6(5) . . ?
N69 C74 N80 117.1(5) . . ?
N73 C74 N80 114.3(5) . . ?
C70 N75 C79 129.7(5) . . ?
N76 N75 C70 118.8(4) . . ?
N76 N75 C79 111.0(4) . . ?
N75 N76 Fe1 114.0(3) . . ?
C77 N76 Fe1 140.7(4) . . ?
C77 N76 N75 105.1(4) . . ?
N76 C77 H77 124.4 . . ?
N76 C77 C78 111.3(5) . . ?
C78 C77 H77 124.4 . . ?
C77 C78 H78 127.4 . . ?
C79 C78 C77 105.3(5) . . ?
C79 C78 H78 127.4 . . ?
N75 C79 H79 126.4 . . ?
C78 C79 N75 107.3(5) . . ?
C78 C79 H79 126.4 . . ?
N81 N80 C74 120.6(5) . . ?
C84 N80 C74 127.8(6) . . ?
C84 N80 N81 111.5(6) . . ?
C82 N81 N80 104.2(6) . . ?
N81 C82 H82 125.2 . . ?
N81 C82 C83 109.7(7) . . ?
C83 C82 H82 125.2 . . ?
C82 C83 H83 126.4 . . ?
C84 C83 C82 107.1(6) . . ?
C84 C83 H83 126.4 . . ?
N80 C84 H84 126.3 . . ?
C83 C84 N80 107.5(7) . . ?
C83 C84 H84 126.3 . . ?
C86 N85 C90 112.8(4) . . ?
N85 C86 N87 126.1(4) . . ?
N85 C86 N91 117.9(4) . . ?
N87 C86 N91 116.0(4) . . ?
C86 N87 Fe2 114.4(3) . . ?
C86 N87 C88 114.4(4) . . ?
C88 N87 Fe2 131.1(3) . . ?
N87 C88 H88 117.2 . . ?
N89 C88 N87 125.5(5) . . ?
N89 C88 H88 117.2 . . ?
C90 N89 C88 113.1(4) . . ?
N85 C90 N96 114.7(5) . . ?
N89 C90 N85 127.9(4) . . ?
N89 C90 N96 117.3(5) . . ?
N92 N91 C86 119.4(3) . . ?
N92 N91 C95 110.8(4) . . ?
C95 N91 C86 129.5(4) . . ?
N91 N92 Fe2 113.9(3) . . ?
C93 N92 Fe2 140.3(3) . . ?
C93 N92 N91 105.7(4) . . ?
N92 C93 H93 124.7 . . ?
N92 C93 C94 110.6(5) . . ?
C94 C93 H93 124.7 . . ?
C93 C94 H94 126.9 . . ?
C95 C94 C93 106.3(4) . . ?
C95 C94 H94 126.9 . . ?
N91 C95 H95 126.7 . . ?
C94 C95 N91 106.6(4) . . ?
C94 C95 H95 126.7 . . ?
C90 N96 N97 120.1(5) . . ?
C100 N96 C90 127.9(6) . . ?
C100 N96 N97 112.0(5) . . ?
C98 N97 N96 102.7(6) . . ?
N97 C98 H98 123.4 . . ?
N97 C98 C99 113.1(7) . . ?
C99 C98 H98 123.4 . . ?
C98 C99 H99 127.0 . . ?
C100 C99 C98 106.0(6) . . ?
C100 C99 H99 127.0 . . ?
N96 C100 C99 106.2(7) . . ?
N96 C100 H100 126.9 . . ?
C99 C100 H100 126.9 . . ?
C106 N101 C102 113.2(6) . . ?
N101 C102 N103 126.8(6) . . ?
N101 C102 N107 116.1(6) . . ?
N103 C102 N107 117.1(5) . . ?
C102 N103 Fe3 113.2(4) . . ?
C104 N103 Fe3 131.6(4) . . ?
C104 N103 C102 115.1(5) . . ?
N103 C104 H104 118.1 . . ?
N103 C104 N105 123.7(6) . . ?
N105 C104 H104 118.1 . . ?
C104 N105 C106 112.9(6) . . ?
N101 C106 N105 128.1(6) . . ?
N101 C106 N112A 111.2(7) . . ?
N105 C106 N112A 120.6(7) . . ?
N101 C106 N112B 139.6(10) . . ?
N105 C106 N112B 92.2(9) . . ?
C102 N107 C111 129.3(6) . . ?
N108 N107 C102 119.3(4) . . ?
N108 N107 C111 111.2(5) . . ?
N107 N108 Fe3 113.9(3) . . ?
C109 N108 Fe3 140.9(4) . . ?
C109 N108 N107 105.0(4) . . ?
N108 C109 H109 123.9 . . ?
N108 C109 C110 112.2(6) . . ?
C110 C109 H109 123.9 . . ?
C109 C110 H110 126.8 . . ?
C109 C110 C111 106.3(5) . . ?
C111 C110 H110 126.8 . . ?
N107 C111 H111 127.4 . . ?
C110 C111 N107 105.2(6) . . ?
C110 C111 H111 127.4 . . ?
N113A N112A C106 119.4(9) . . ?
C116A N112A C106 128.8(8) . . ?
C116A N112A N113A 111.7(7) . . ?
C114A N113A N112A 105.8(12) . . ?
N113A C114A H114A 124.3 . . ?
N113A C114A C115A 111.4(10) . . ?
C115A C114A H114A 124.3 . . ?
C114A C115A H115A 128.0 . . ?
C116A C115A C114A 104.1(10) . . ?
C116A C115A H115A 128.0 . . ?
N112A C116A C115A 107.0(9) . . ?
N112A C116A H116A 126.5 . . ?
C115A C116A H116A 126.5 . . ?
N113B N112B C106 143.9(16) . . ?
C116B N112B C106 112.5(17) . . ?
C116B N112B N113B 103.5(16) . . ?
C114B N113B N112B 114(2) . . ?
N113B C114B H114B 128.4 . . ?
N113B C114B C115B 103(3) . . ?
C115B C114B H114B 128.4 . . ?
C114B C115B H115B 124.5 . . ?
C116B C115B C114B 111(3) . . ?
C116B C115B H115B 124.5 . . ?
N112B C116B H116B 125.8 . . ?
C115B C116B N112B 108(2) . . ?
C115B C116B H116B 125.8 . . ?
C118 N117 C122 113.3(4) . . ?
N117 C118 N119 127.4(4) . . ?
N117 C118 N123 116.7(4) . . ?
N119 C118 N123 115.9(4) . . ?
C118 N119 Fe4 115.0(3) . . ?
C118 N119 C120 113.0(4) . . ?
C120 N119 Fe4 132.0(3) . . ?
N119 C120 H120 117.0 . . ?
N121 C120 N119 126.0(4) . . ?
N121 C120 H120 117.0 . . ?
C120 N121 C122 113.6(4) . . ?
N117 C122 N121 126.6(4) . . ?
N117 C122 N128 117.4(4) . . ?
N121 C122 N128 116.0(5) . . ?
N124 N123 C118 119.6(3) . . ?
C127 N123 C118 129.2(4) . . ?
C127 N123 N124 111.1(4) . . ?
N123 N124 Fe4 113.8(3) . . ?
C125 N124 Fe4 140.8(3) . . ?
C125 N124 N123 105.2(4) . . ?
N124 C125 H125 124.7 . . ?
N124 C125 C126 110.7(5) . . ?
C126 C125 H125 124.7 . . ?
C125 C126 H126 127.0 . . ?
C127 C126 C125 105.9(4) . . ?
C127 C126 H126 127.0 . . ?
N123 C127 H127 126.5 . . ?
C126 C127 N123 107.1(4) . . ?
C126 C127 H127 126.5 . . ?
N129 N128 C122 120.9(4) . . ?
C132 N128 C122 126.9(5) . . ?
C132 N128 N129 112.1(5) . . ?
C130 N129 N128 103.6(5) . . ?
N129 C130 H130 123.9 . . ?
N129 C130 C131 112.1(6) . . ?
C131 C130 H130 123.9 . . ?
C130 C131 H131 127.0 . . ?
C132 C131 C130 105.9(5) . . ?
C132 C131 H131 127.0 . . ?
N128 C132 H132 126.9 . . ?
C131 C132 N128 106.1(6) . . ?
C131 C132 H132 126.9 . . ?
F135 B133 F134 110.2(3) . . ?
F135 B133 F136 110.7(4) . . ?
F135 B133 F137 107.6(4) . . ?
F136 B133 F134 107.7(4) . . ?
F136 B133 F137 110.7(3) . . ?
F137 B133 F134 110.1(4) . . ?
F139 B138 F142 111.6(4) . . ?
F140 B138 F139 108.2(4) . . ?
F140 B138 F142 106.8(5) . . ?
F141 B138 F139 110.4(5) . . ?
F141 B138 F140 109.1(5) . . ?
F141 B138 F142 110.6(4) . . ?
F45A B143 F44A 106.2(6) . . ?
F46A B143 F44A 104.6(6) . . ?
F46A B143 F45A 113.4(6) . . ?
F46A B143 F47A 115.8(6) . . ?
F47A B143 F44A 100.4(6) . . ?
F47A B143 F45A 114.5(6) . . ?
F44B B143 F45B 112.9(7) . . ?
F44B B143 F46B 109.7(6) . . ?
F44B B143 F47B 116.2(7) . . ?
F45B B143 F46B 107.2(6) . . ?
F45B B143 F47B 109.5(6) . . ?
F47B B143 F46B 100.3(6) . . ?
F149A B148A F151A 111.4(10) . . ?
F150A B148A F149A 113.3(11) . . ?
F150A B148A F151A 110.2(12) . . ?
F152A B148A F149A 113.3(11) . . ?
F152A B148A F150A 108.3(10) . . ?
F152A B148A F151A 99.5(10) . . ?
F149B B148B F152B 104.1(10) . . ?
F150B B148B F149B 104.3(10) . . ?
F150B B148B F151B 111.1(11) . . ?
F150B B148B F152B 112.9(10) . . ?
F151B B148B F149B 105.9(10) . . ?
F151B B148B F152B 117.1(10) . . ?
F155 B153 F154 106.2(4) . . ?
F156 B153 F154 107.0(5) . . ?
F156 B153 F155 112.7(5) . . ?
F156 B153 F157 110.7(4) . . ?
F157 B153 F154 109.7(5) . . ?
F157 B153 F155 110.5(5) . . ?
F159A B158A F160A 103.6(10) . . ?
F161A B158A F159A 119.6(11) . . ?
F161A B158A F160A 107.8(11) . . ?
F161A B158A F162A 110.5(11) . . ?
F162A B158A F159A 107.9(10) . . ?
F162A B158A F160A 106.7(10) . . ?
F159B B158B F160B 109.9(10) . . ?
F159B B158B F161B 108.1(9) . . ?
F159B B158B F162B 109.9(10) . . ?
F160B B158B F161B 106.3(9) . . ?
F160B B158B F162B 111.0(9) . . ?
F161B B158B F162B 111.5(10) . . ?
F164 B163 F165 109.4(5) . . ?
F166 B163 F164 108.7(5) . . ?
F166 B163 F165 106.9(5) . . ?
F166 B163 F167 112.3(5) . . ?
F167 B163 F164 111.4(5) . . ?
F167 B163 F165 108.0(5) . . ?
F169 B168 F170 109.3(5) . . ?
F171 B168 F169 109.2(4) . . ?
F171 B168 F170 108.9(4) . . ?
F172 B168 F169 109.9(5) . . ?
F172 B168 F170 108.8(4) . . ?
F172 B168 F171 110.7(5) . . ?
N174 N173 C177 99.4(10) . . ?
N174 N173 B178 130.0(10) . . ?
C177 N173 B178 130.3(11) . . ?
N173 N174 H174 124.7 . . ?
C175 N174 N173 110.6(10) . . ?
C175 N174 H174 124.7 . . ?
N174 C175 H175 122.5 . . ?
C176 C175 N174 115.0(11) . . ?
C176 C175 H175 122.5 . . ?
C175 C176 H176 129.4 . . ?
C175 C176 C177 101.2(12) . . ?
C177 C176 H176 129.4 . . ?
N173 C177 C176 111.4(14) . . ?
N173 C177 H177 124.3 . . ?
C176 C177 H177 124.3 . . ?
F179 B178 N173 105.9(11) . . ?
F179 B178 F180 114.0(11) . . ?
F179 B178 F181 108.8(11) . . ?
F180 B178 N173 109.3(10) . . ?
F180 B178 F181 112.8(11) . . ?
F181 B178 N173 105.4(10) . . ?
H18A C182 H18B 109.5 . . ?
H18A C182 H18C 109.5 . . ?
H18B C182 H18C 109.5 . . ?
C183 C182 H18A 109.5 . . ?
C183 C182 H18B 109.5 . . ?
C183 C182 H18C 109.5 . . ?
N184 C183 C182 175.0(10) . . ?
H18D C185 H18E 109.5 . . ?
H18D C185 H18F 109.5 . . ?
H18E C185 H18F 109.5 . . ?
C186 C185 H18D 109.5 . . ?
C186 C185 H18E 109.5 . . ?
C186 C185 H18F 109.5 . . ?
N187 C186 C185 177.8(8) . . ?
H18G C188 H18H 109.5 . . ?
H18G C188 H18I 109.5 . . ?
H18H C188 H18I 109.5 . . ?
C189 C188 H18G 109.5 . . ?
C189 C188 H18H 109.5 . . ?
C189 C188 H18I 109.5 . . ?
N190 C189 C188 174.2(10) . . ?
H19A C191 H19B 109.5 . . ?
H19A C191 H19C 109.5 . . ?
H19B C191 H19C 109.5 . . ?
C192 C191 H19A 109.5 . . ?
C192 C191 H19B 109.5 . . ?
C192 C191 H19C 109.5 . . ?
N193 C192 C191 178.6(6) . . ?
H19D C194 H19E 109.5 . . ?
H19D C194 H19F 109.5 . . ?
H19E C194 H19F 109.5 . . ?
C195 C194 H19D 109.5 . . ?
C195 C194 H19E 109.5 . . ?
C195 C194 H19F 109.5 . . ?
N196 C195 C194 178.4(9) . . ?
H19G C197 H19H 109.5 . . ?
H19G C197 H19I 109.5 . . ?
H19H C197 H19I 109.5 . . ?
C198 C197 H19G 109.5 . . ?
C198 C197 H19H 109.5 . . ?
C198 C197 H19I 109.5 . . ?
N199 C198 C197 176.6(10) . . ?
H20A C200 H20B 109.5 . . ?
H20A C200 H20C 109.5 . . ?
H20B C200 H20C 109.5 . . ?
C201 C200 H20A 109.5 . . ?
C201 C200 H20B 109.5 . . ?
C201 C200 H20C 109.5 . . ?
N202 C201 C200 173.7(13) . . ?
H20D C203 H20E 109.5 . . ?
H20D C203 H20F 109.5 . . ?
H20E C203 H20F 109.5 . . ?
C204 C203 H20D 109.5 . . ?
C204 C203 H20E 109.5 . . ?
C204 C203 H20F 109.5 . . ?
N205 C204 C203 175(2) . . ?
H20G C206 H20H 109.5 . . ?
H20G C206 H20I 109.5 . . ?
H20H C206 H20I 109.5 . . ?
C207 C206 H20G 109.5 . . ?
C207 C206 H20H 109.5 . . ?
C207 C206 H20I 109.5 . . ?
N208 C207 C206 158(2) . . ?

loop_
_geom_hbond_atom_site_label_D
_geom_hbond_atom_site_label_H
_geom_hbond_atom_site_label_A
_geom_hbond_distance_DH
_geom_hbond_distance_HA
_geom_hbond_distance_DA
_geom_hbond_angle_DHA
_geom_hbond_site_symmetry_A
N174 H174 N113A 0.88 2.09 2.940(10) 161.7 .

####################################################################### 
# 
# 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_sf-15
_database_code_depnum_ccdc_archive 'CCDC 1957576'
loop_
_audit_author_name
_audit_author_address
'Malcolm Halcrow' 'University of Leeds'
_audit_update_record             
;
2019-10-04 deposited with the CCDC.	2019-11-05 downloaded from the CCDC.
;
_audit_creation_date             2019-07-05
_audit_creation_method           
;
  Olex2 1.2
  (compiled Apr 23 2013 17:54:37, GUI svn.r4466)
;
_chemical_name_common            ?
_chemical_name_systematic        
'Catena-[2,4-di(4-chloropyrazol-1-yl)-6H-1,3,5-triazine]-(acetonitrile)silver(I) perchlorate'
_chemical_formula_moiety         'C11 H8 Ag Cl3 N8 O4'
_chemical_formula_sum            'C11 H8 Ag Cl3 N8 O4'
_chemical_formula_weight         530.47
_chemical_melting_point          ?
loop_
_atom_type_symbol
_atom_type_description
_atom_type_scat_dispersion_real
_atom_type_scat_dispersion_imag
_atom_type_scat_source
C C 0.0181 0.0091 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
N N 0.0311 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'
Ag Ag 0.1306 4.2820 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Cl Cl 0.3639 0.7018 '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/n 1'
_space_group_name_Hall           '-P 2yn'
loop_
_space_group_symop_id
_space_group_symop_operation_xyz
1 'x, y, z'
2 '-x+1/2, y+1/2, -z+1/2'
3 '-x, -y, -z'
4 'x-1/2, -y-1/2, z-1/2'

_cell_length_a                   13.5601(2)
_cell_length_b                   8.2545(1)
_cell_length_c                   15.4017(3)
_cell_angle_alpha                90.00
_cell_angle_beta                 95.121(1)
_cell_angle_gamma                90.00
_cell_volume                     1717.06(5)
_cell_formula_units_Z            4
_cell_measurement_reflns_used    4157
_cell_measurement_temperature    120(2)
_cell_measurement_theta_min      4.15
_cell_measurement_theta_max      73.62
_exptl_absorpt_coefficient_mu    14.097
_exptl_absorpt_correction_T_min  0.528
_exptl_absorpt_correction_T_max  1.000
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   
; 
CrysAlisPro, Agilent Technologies,
Version 1.171.36.24 (release 03-12-2012 CrysAlis171 .NET)
Empirical absorption correction using spherical harmonics,
 implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_crystal_colour            colourless
_exptl_crystal_density_diffrn    2.052
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       fragment
_exptl_crystal_F_000             1040
_exptl_crystal_size_max          0.40
_exptl_crystal_size_mid          0.25
_exptl_crystal_size_min          0.10
_exptl_special_details           
;
 ? 
;
_diffrn_reflns_av_R_equivalents  0.0261
_diffrn_reflns_av_unetI/netI     0.0320
_diffrn_reflns_limit_h_max       15
_diffrn_reflns_limit_h_min       -16
_diffrn_reflns_limit_k_max       10
_diffrn_reflns_limit_k_min       -8
_diffrn_reflns_limit_l_max       12
_diffrn_reflns_limit_l_min       -18
_diffrn_reflns_number            6561
_diffrn_reflns_theta_full        72.00
_diffrn_reflns_theta_max         73.83
_diffrn_reflns_theta_min         4.16
_diffrn_ambient_temperature      120(2)
_diffrn_detector_area_resol_mean 5.3095
_diffrn_measured_fraction_theta_full 0.976
_diffrn_measured_fraction_theta_max 0.957
_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                3011
_reflns_number_total             3338
_reflns_threshold_expression     >2sigma(I)
_computing_cell_refinement       'CrysAlisPro, Agilent Technologies'
_computing_data_collection       '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         0.568
_refine_diff_density_min         -0.558
_refine_diff_density_rms         0.092
_refine_ls_extinction_coef       ?
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.024
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     245
_refine_ls_number_reflns         3338
_refine_ls_number_restraints     0
_refine_ls_R_factor_all          0.0322
_refine_ls_R_factor_gt           0.0284
_refine_ls_restrained_S_all      1.024
_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)+(0.0453P)²+0.2394P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0737
_refine_ls_wR_factor_ref         0.0772
_refine_special_details          
;
 Refinement of F² against ALL reflections.  The weighted R-factor wR and 
 goodness of fit S are based on F², conventional R-factors R are based 
 on F, with F set to zero for negative F². The threshold expression of 
 F² > 2sigma(F²) is used only for calculating R-factors(gt) etc. and is 
 not relevant to the choice of reflections for refinement.  R-factors based 
 on F² are statistically about twice as large as those based on F, and R- 
 factors based on ALL data will be even larger. 

 No disorder is present in the model, and no restraints were applied to the
 refinement. All non-H atoms were refined anisotropically, and H atoms were
 placed in calculated positions and refined using a riding model.
;
_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.a Aromatic/amide H refined with riding coordinates:
 C5(H5), C10(H10), C12(H12), C16(H16), C18(H18)
2.b Idealised Me refined as rotating group:
 C22(H22A,H22B,H22C)
;
_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
Ag1 Ag 0.174289(14) 0.00209(2) 0.411050(13) 0.02212(9) Uani 1 1 d . . .
N2 N 0.44544(15) 0.3281(3) 0.37015(14) 0.0176(4) Uani 1 1 d . . .
C3 C 0.37416(19) 0.2324(3) 0.39443(17) 0.0173(5) Uani 1 1 d . . .
N4 N 0.28966(16) 0.1937(3) 0.34851(15) 0.0191(5) Uani 1 1 d . . .
C5 C 0.27903(19) 0.2637(3) 0.27037(17) 0.0210(5) Uani 1 1 d . . .
H5 H 0.2194 0.2418 0.2352 0.025 Uiso 1 1 calc R . .
N6 N 0.34339(16) 0.3607(3) 0.23697(15) 0.0209(5) Uani 1 1 d . . .
C7 C 0.42489(19) 0.3877(3) 0.29021(17) 0.0174(5) Uani 1 1 d . . .
N8 N 0.39124(15) 0.1619(3) 0.47671(14) 0.0170(4) Uani 1 1 d . . .
N9 N 0.32789(17) 0.0475(3) 0.50355(16) 0.0205(5) Uani 1 1 d . . .
C10 C 0.3665(2) 0.0046(3) 0.5815(2) 0.0218(6) Uani 1 1 d . . .
H10 H 0.3388 -0.0746 0.6169 0.026 Uiso 1 1 calc R . .
C11 C 0.45423(19) 0.0914(3) 0.60565(17) 0.0184(5) Uani 1 1 d . . .
C12 C 0.46929(19) 0.1911(3) 0.53785(17) 0.0179(5) Uani 1 1 d . . .
H12 H 0.5223 0.2650 0.5337 0.021 Uiso 1 1 calc R . .
Cl13 Cl 0.52812(5) 0.07354(8) 0.70159(4) 0.02236(15) Uani 1 1 d . . .
N14 N 0.49722(19) 0.4858(3) 0.25810(16) 0.0188(5) Uani 1 1 d . . .
N15 N 0.48389(18) 0.5422(3) 0.17392(16) 0.0223(5) Uani 1 1 d . . .
C16 C 0.5636(2) 0.6275(4) 0.16328(18) 0.0225(6) Uani 1 1 d . . .
H16 H 0.5762 0.6816 0.1109 0.027 Uiso 1 1 calc R . .
C17 C 0.62806(19) 0.6277(3) 0.24065(18) 0.0206(5) Uani 1 1 d . . .
C18 C 0.5852(2) 0.5363(3) 0.29989(19) 0.0201(5) Uani 1 1 d . . .
H18 H 0.6107 0.5124 0.3579 0.024 Uiso 1 1 calc R . .
Cl19 Cl 0.73618(5) 0.73716(9) 0.25611(5) 0.02826(16) Uani 1 1 d . . .
N20 N 0.0939(2) 0.1585(4) 0.51684(19) 0.0343(6) Uani 1 1 d . . .
C21 C 0.0788(2) 0.2704(4) 0.5561(2) 0.0275(6) Uani 1 1 d . . .
C22 C 0.0589(2) 0.4130(5) 0.6067(2) 0.0394(8) Uani 1 1 d . . .
H22A H -0.0118 0.4396 0.5978 0.059 Uiso 1 1 calc R . .
H22B H 0.0979 0.5044 0.5878 0.059 Uiso 1 1 calc R . .
H22C H 0.0770 0.3915 0.6686 0.059 Uiso 1 1 calc R . .
Cl23 Cl 0.24081(4) -0.40610(8) 0.45177(4) 0.02079(14) Uani 1 1 d . . .
O24 O 0.27703(19) -0.5228(3) 0.51587(17) 0.0346(5) Uani 1 1 d . . .
O25 O 0.32291(15) -0.3301(3) 0.41473(15) 0.0344(5) Uani 1 1 d . . .
O26 O 0.18291(17) -0.2842(3) 0.49203(15) 0.0339(5) Uani 1 1 d . . .
O27 O 0.18001(17) -0.4853(3) 0.38299(18) 0.0321(5) Uani 1 1 d . . .


_geom_special_details            
;
 All esds (except the esd in the dihedral angle between two l.s. planes) 
 are estimated using the full covariance matrix.  The cell esds are taken 
 into account individually in the estimation of esds in distances, angles 
 and torsion angles; correlations between esds in cell parameters are only 
 used when they are defined by crystal symmetry.  An approximate (isotropic) 
 treatment of cell esds is used for estimating esds involving l.s. planes. 
;
loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
_geom_bond_publ_flag
Ag1 Ag1 6.9050(3) 2_545 ?
Ag1 N4 2.479(2) . ?
Ag1 N6 2.553(2) 2_545 ?
Ag1 N9 2.445(2) . ?
Ag1 N15 2.433(2) 2_545 ?
Ag1 N20 2.414(3) . ?
Ag1 O26 2.670(2) . ?
N2 C3 1.328(3) . ?
N2 C7 1.332(3) . ?
C3 N4 1.331(3) . ?
C3 N8 1.395(3) . ?
N4 C5 1.331(4) . ?
C5 H5 0.9500 . ?
C5 N6 1.322(4) . ?
N6 Ag1 2.553(2) 2 ?
N6 C7 1.335(3) . ?
C7 N14 1.396(4) . ?
N8 N9 1.365(3) . ?
N8 C12 1.374(3) . ?
N9 C10 1.314(4) . ?
C10 H10 0.9500 . ?
C10 C11 1.410(4) . ?
C11 C12 1.359(4) . ?
C11 Cl13 1.716(3) . ?
C12 H12 0.9500 . ?
N14 N15 1.374(3) . ?
N14 C18 1.369(4) . ?
N15 Ag1 2.433(2) 2 ?
N15 C16 1.313(4) . ?
C16 H16 0.9500 . ?
C16 C17 1.414(4) . ?
C17 C18 1.354(4) . ?
C17 Cl19 1.720(3) . ?
C18 H18 0.9500 . ?
N20 C21 1.132(4) . ?
C21 C22 1.451(5) . ?
C22 H22A 0.9800 . ?
C22 H22B 0.9800 . ?
C22 H22C 0.9800 . ?
Cl23 O24 1.434(2) . ?
Cl23 O25 1.439(2) . ?
Cl23 O26 1.449(2) . ?
Cl23 O27 1.440(2) . ?

loop_
_geom_angle_atom_site_label_1
_geom_angle_atom_site_label_2
_geom_angle_atom_site_label_3
_geom_angle
_geom_angle_site_symmetry_1
_geom_angle_site_symmetry_3
_geom_angle_publ_flag
N4 Ag1 N6 87.53(7) . 2_545 ?
N4 Ag1 O26 138.02(7) . . ?
N6 Ag1 O26 90.52(7) 2_545 . ?
N9 Ag1 N4 66.06(8) . . ?
N9 Ag1 N6 126.70(8) . 2_545 ?
N9 Ag1 O26 82.19(8) . . ?
N15 Ag1 N4 105.11(8) 2_545 . ?
N15 Ag1 N6 64.79(8) 2_545 2_545 ?
N15 Ag1 N9 163.04(9) 2_545 . ?
N15 Ag1 O26 111.80(8) 2_545 . ?
N20 Ag1 N4 105.04(9) . . ?
N20 Ag1 N6 146.63(8) . 2_545 ?
N20 Ag1 N9 86.39(9) . . ?
N20 Ag1 N15 82.00(9) . 2_545 ?
N20 Ag1 O26 99.32(8) . . ?
C3 N2 C7 112.5(2) . . ?
N2 C3 N4 127.4(2) . . ?
N2 C3 N8 116.0(2) . . ?
N4 C3 N8 116.6(2) . . ?
C3 N4 Ag1 119.33(18) . . ?
C3 N4 C5 113.3(2) . . ?
C5 N4 Ag1 127.37(17) . . ?
N4 C5 H5 116.8 . . ?
N6 C5 N4 126.3(2) . . ?
N6 C5 H5 116.8 . . ?
C5 N6 Ag1 127.71(17) . 2 ?
C5 N6 C7 113.6(2) . . ?
C7 N6 Ag1 118.61(18) . 2 ?
N2 C7 N6 126.8(2) . . ?
N2 C7 N14 116.5(2) . . ?
N6 C7 N14 116.6(2) . . ?
N9 N8 C3 120.4(2) . . ?
N9 N8 C12 112.4(2) . . ?
C12 N8 C3 127.2(2) . . ?
N8 N9 Ag1 117.13(16) . . ?
C10 N9 Ag1 137.7(2) . . ?
C10 N9 N8 104.7(2) . . ?
N9 C10 H10 124.4 . . ?
N9 C10 C11 111.2(2) . . ?
C11 C10 H10 124.4 . . ?
C10 C11 Cl13 126.7(2) . . ?
C12 C11 C10 106.6(2) . . ?
C12 C11 Cl13 126.7(2) . . ?
N8 C12 H12 127.4 . . ?
C11 C12 N8 105.1(2) . . ?
C11 C12 H12 127.4 . . ?
N15 N14 C7 119.6(2) . . ?
C18 N14 C7 128.3(2) . . ?
C18 N14 N15 112.1(2) . . ?
N14 N15 Ag1 119.77(17) . 2 ?
C16 N15 Ag1 134.6(2) . 2 ?
C16 N15 N14 105.0(2) . . ?
N15 C16 H16 124.8 . . ?
N15 C16 C17 110.5(3) . . ?
C17 C16 H16 124.8 . . ?
C16 C17 Cl19 124.9(2) . . ?
C18 C17 C16 107.3(2) . . ?
C18 C17 Cl19 127.6(2) . . ?
N14 C18 H18 127.4 . . ?
C17 C18 N14 105.1(2) . . ?
C17 C18 H18 127.4 . . ?
C21 N20 Ag1 155.6(3) . . ?
N20 C21 C22 179.6(4) . . ?
C21 C22 H22A 109.5 . . ?
C21 C22 H22B 109.5 . . ?
C21 C22 H22C 109.5 . . ?
H22A C22 H22B 109.5 . . ?
H22A C22 H22C 109.5 . . ?
H22B C22 H22C 109.5 . . ?
O24 Cl23 O25 109.63(15) . . ?
O24 Cl23 O26 109.69(15) . . ?
O24 Cl23 O27 109.87(15) . . ?
O25 Cl23 O26 109.57(15) . . ?
O25 Cl23 O27 108.57(15) . . ?
O27 Cl23 O26 109.48(14) . . ?
Cl23 O26 Ag1 114.67(12) . . ?

_exptl_crystal_recrystallization_method 
'Re-crystallisation from solvent: acetonitrile/diethyl ether'
####################################################################### 
# 
# 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_sf-15-2
_database_code_depnum_ccdc_archive 'CCDC 1957577'
loop_
_audit_author_name
_audit_author_address
'Malcolm Halcrow' 'University of Leeds'
_audit_update_record             
;
2019-10-04 deposited with the CCDC.	2019-11-05 downloaded from the CCDC.
;
_audit_creation_date             2019-07-05
_audit_creation_method           
;
  Olex2 1.2
  (compiled Apr 23 2013 17:54:37, GUI svn.r4466)
;
_chemical_name_common            ?
_chemical_name_systematic        
'Catena-[2,4-di(4-chloropyrazol-1-yl)-6H-1,3,5-triazine]silver(I) perchlorate'
_chemical_formula_moiety         'C9 H5 Ag Cl3 N7 O4'
_chemical_formula_sum            'C9 H5 Ag Cl3 N7 O4'
_chemical_formula_weight         489.42
_chemical_melting_point          ?
loop_
_atom_type_symbol
_atom_type_description
_atom_type_scat_dispersion_real
_atom_type_scat_dispersion_imag
_atom_type_scat_source
C C 0.0181 0.0091 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
N N 0.0311 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'
Ag Ag 0.1306 4.2820 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Cl Cl 0.3639 0.7018 '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/n 1'
_space_group_name_Hall           '-P 2yn'
loop_
_space_group_symop_id
_space_group_symop_operation_xyz
1 'x, y, z'
2 '-x+1/2, y+1/2, -z+1/2'
3 '-x, -y, -z'
4 'x-1/2, -y-1/2, z-1/2'

_cell_length_a                   8.0112(2)
_cell_length_b                   10.5868(3)
_cell_length_c                   16.9917(3)
_cell_angle_alpha                90.00
_cell_angle_beta                 95.332(2)
_cell_angle_gamma                90.00
_cell_volume                     1434.88(6)
_cell_formula_units_Z            4
_cell_measurement_reflns_used    3254
_cell_measurement_temperature    120(2)
_cell_measurement_theta_min      4.90
_cell_measurement_theta_max      73.10
_exptl_absorpt_coefficient_mu    16.771
_exptl_absorpt_correction_T_min  0.826
_exptl_absorpt_correction_T_max  1.000
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   
; 
CrysAlisPro, Agilent Technologies,
Version 1.171.36.24 (release 03-12-2012 CrysAlis171 .NET)
Empirical absorption correction using spherical harmonics,
 implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_crystal_colour            colourless
_exptl_crystal_density_diffrn    2.266
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       lath
_exptl_crystal_F_000             952
_exptl_crystal_size_max          0.35
_exptl_crystal_size_mid          0.20
_exptl_crystal_size_min          0.10
_exptl_special_details           
;
 ? 
;
_diffrn_reflns_av_R_equivalents  0.0289
_diffrn_reflns_av_unetI/netI     0.0345
_diffrn_reflns_limit_h_max       9
_diffrn_reflns_limit_h_min       -9
_diffrn_reflns_limit_k_max       9
_diffrn_reflns_limit_k_min       -12
_diffrn_reflns_limit_l_max       18
_diffrn_reflns_limit_l_min       -20
_diffrn_reflns_number            6035
_diffrn_reflns_theta_full        72.00
_diffrn_reflns_theta_max         73.76
_diffrn_reflns_theta_min         4.93
_diffrn_ambient_temperature      120(2)
_diffrn_detector_area_resol_mean 5.3095
_diffrn_measured_fraction_theta_full 0.957
_diffrn_measured_fraction_theta_max 0.941
_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                2392
_reflns_number_total             2729
_reflns_threshold_expression     >2sigma(I)
_computing_cell_refinement       'CrysAlisPro, Agilent Technologies'
_computing_data_collection       '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         1.104
_refine_diff_density_min         -0.819
_refine_diff_density_rms         0.106
_refine_ls_extinction_coef       ?
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.051
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     217
_refine_ls_number_reflns         2729
_refine_ls_number_restraints     0
_refine_ls_R_factor_all          0.0358
_refine_ls_R_factor_gt           0.0299
_refine_ls_restrained_S_all      1.051
_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)+(0.0422P)²+0.7156P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0756
_refine_ls_wR_factor_ref         0.0800
_refine_special_details          
;
 Refinement of F² against ALL reflections.  The weighted R-factor wR and 
 goodness of fit S are based on F², conventional R-factors R are based 
 on F, with F set to zero for negative F². The threshold expression of 
 F² > 2sigma(F²) is used only for calculating R-factors(gt) etc. and is 
 not relevant to the choice of reflections for refinement.  R-factors based 
 on F² are statistically about twice as large as those based on F, and R- 
 factors based on ALL data will be even larger. 

 No disorder is present in the model, and no restraints were applied to the
 refinement. All non-H atoms were refined anisotropically, and H atoms were
 placed in calculated positions and refined using a riding model.
;
_olex2_refinement_description    
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups
2.a Aromatic/amide H refined with riding coordinates:
 C5(H5), C10(H10), C12(H12), C16(H16), C18(H18)
;
_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
Ag1 Ag 0.48853(4) 0.52284(3) 0.253922(14) 0.02510(11) Uani 1 1 d . . .
N2 N 0.8815(3) 0.3296(3) 0.42262(15) 0.0143(5) Uani 1 1 d . . .
C3 C 0.7762(4) 0.4073(3) 0.38111(19) 0.0148(6) Uani 1 1 d . . .
N4 N 0.7279(4) 0.4003(3) 0.30370(16) 0.0173(6) Uani 1 1 d . . .
C5 C 0.7975(5) 0.3051(3) 0.26704(19) 0.0185(7) Uani 1 1 d . . .
H5 H 0.7673 0.2960 0.2119 0.022 Uiso 1 1 calc R . .
N6 N 0.9050(4) 0.2222(3) 0.30097(16) 0.0183(6) Uani 1 1 d . . .
C7 C 0.9387(4) 0.2386(3) 0.37818(19) 0.0143(6) Uani 1 1 d . . .
N8 N 0.7067(4) 0.5035(3) 0.42370(16) 0.0145(6) Uani 1 1 d . . .
N9 N 0.5899(4) 0.5823(3) 0.38631(17) 0.0181(6) Uani 1 1 d . . .
C10 C 0.5465(4) 0.6581(3) 0.4423(2) 0.0195(7) Uani 1 1 d . . .
H10 H 0.4661 0.7240 0.4343 0.023 Uiso 1 1 calc R . .
C11 C 0.6348(4) 0.6289(3) 0.5156(2) 0.0168(7) Uani 1 1 d . . .
C12 C 0.7368(4) 0.5293(3) 0.5025(2) 0.0163(7) Uani 1 1 d . . .
H12 H 0.8123 0.4870 0.5401 0.020 Uiso 1 1 calc R . .
Cl13 Cl 0.61052(11) 0.70367(8) 0.60316(5) 0.02045(18) Uani 1 1 d . . .
N14 N 1.0457(4) 0.1500(3) 0.41767(16) 0.0143(5) Uani 1 1 d . . .
N15 N 1.1087(4) 0.0523(3) 0.37651(16) 0.0164(6) Uani 1 1 d . . .
C16 C 1.2119(5) -0.0079(3) 0.4291(2) 0.0177(7) Uani 1 1 d . . .
H16 H 1.2754 -0.0804 0.4180 0.021 Uiso 1 1 calc R . .
C17 C 1.2149(4) 0.0501(3) 0.5041(2) 0.0167(6) Uani 1 1 d . . .
C18 C 1.1074(4) 0.1492(3) 0.49577(19) 0.0155(6) Uani 1 1 d . . .
H18 H 1.0804 0.2063 0.5358 0.019 Uiso 1 1 calc R . .
Cl19 Cl 1.33129(11) 0.00193(8) 0.58847(5) 0.02082(18) Uani 1 1 d . . .
Cl20 Cl 0.09416(11) 0.64360(8) 0.30401(4) 0.02026(18) Uani 1 1 d . . .
O21 O 0.1919(5) 0.5295(4) 0.3101(2) 0.0505(10) Uani 1 1 d . . .
O22 O -0.0127(4) 0.6424(3) 0.23220(16) 0.0340(7) Uani 1 1 d . . .
O23 O -0.0045(4) 0.6484(3) 0.37090(16) 0.0332(7) Uani 1 1 d . . .
O24 O 0.2076(5) 0.7482(4) 0.3052(2) 0.0575(11) Uani 1 1 d . . .


_geom_special_details            
;
 All esds (except the esd in the dihedral angle between two l.s. planes) 
 are estimated using the full covariance matrix.  The cell esds are taken 
 into account individually in the estimation of esds in distances, angles 
 and torsion angles; correlations between esds in cell parameters are only 
 used when they are defined by crystal symmetry.  An approximate (isotropic) 
 treatment of cell esds is used for estimating esds involving l.s. planes. 
;
loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
_geom_bond_publ_flag
Ag1 Ag1 6.7596(4) 2_655 ?
Ag1 N4 2.403(3) . ?
Ag1 N6 2.490(3) 2_655 ?
Ag1 N9 2.403(3) . ?
Ag1 N15 2.301(3) 2_655 ?
Ag1 O21 2.643(4) . ?
N2 C3 1.332(4) . ?
N2 C7 1.331(4) . ?
C3 N4 1.338(4) . ?
C3 N8 1.395(4) . ?
N4 C5 1.334(5) . ?
C5 H5 0.9500 . ?
C5 N6 1.324(5) . ?
N6 C7 1.326(4) . ?
C7 N14 1.399(4) . ?
N8 N9 1.366(4) . ?
N8 C12 1.366(4) . ?
N9 C10 1.316(5) . ?
C10 H10 0.9500 . ?
C10 C11 1.408(5) . ?
C11 C12 1.365(5) . ?
C11 Cl13 1.712(3) . ?
C12 H12 0.9500 . ?
N14 N15 1.372(4) . ?
N14 C18 1.372(4) . ?
N15 C16 1.323(5) . ?
C16 H16 0.9500 . ?
C16 C17 1.411(5) . ?
C17 C18 1.357(5) . ?
C17 Cl19 1.714(3) . ?
C18 H18 0.9500 . ?
Cl20 O21 1.438(3) . ?
Cl20 O22 1.424(3) . ?
Cl20 O23 1.444(3) . ?
Cl20 O24 1.432(4) . ?

loop_
_geom_angle_atom_site_label_1
_geom_angle_atom_site_label_2
_geom_angle_atom_site_label_3
_geom_angle
_geom_angle_site_symmetry_1
_geom_angle_site_symmetry_3
_geom_angle_publ_flag
N4 Ag1 N6 107.44(10) . 2_655 ?
N4 Ag1 N9 67.84(10) . . ?
N4 Ag1 O21 127.03(10) . . ?
N6 Ag1 O21 117.60(11) 2_655 . ?
N9 Ag1 N6 91.77(9) . 2_655 ?
N9 Ag1 O21 83.79(11) . . ?
N15 Ag1 N4 126.85(10) 2_655 . ?
N15 Ag1 N6 67.76(10) 2_655 2_655 ?
N15 Ag1 N9 157.03(10) 2_655 . ?
N15 Ag1 O21 96.25(10) 2_655 . ?
C7 N2 C3 112.4(3) . . ?
N2 C3 N4 126.7(3) . . ?
N2 C3 N8 116.1(3) . . ?
N4 C3 N8 117.2(3) . . ?
C3 N4 Ag1 117.7(2) . . ?
C5 N4 Ag1 126.7(2) . . ?
C5 N4 C3 113.9(3) . . ?
N4 C5 H5 117.2 . . ?
N6 C5 N4 125.5(3) . . ?
N6 C5 H5 117.2 . . ?
C5 N6 Ag1 129.1(2) . 2_645 ?
C5 N6 C7 114.1(3) . . ?
C7 N6 Ag1 115.9(2) . 2_645 ?
N2 C7 N14 116.2(3) . . ?
N6 C7 N2 127.4(3) . . ?
N6 C7 N14 116.5(3) . . ?
N9 N8 C3 119.6(3) . . ?
N9 N8 C12 112.6(3) . . ?
C12 N8 C3 127.8(3) . . ?
N8 N9 Ag1 115.6(2) . . ?
C10 N9 Ag1 138.4(2) . . ?
C10 N9 N8 104.6(3) . . ?
N9 C10 H10 124.4 . . ?
N9 C10 C11 111.1(3) . . ?
C11 C10 H10 124.4 . . ?
C10 C11 Cl13 125.3(3) . . ?
C12 C11 C10 106.6(3) . . ?
C12 C11 Cl13 128.1(3) . . ?
N8 C12 H12 127.4 . . ?
C11 C12 N8 105.1(3) . . ?
C11 C12 H12 127.4 . . ?
N15 N14 C7 120.0(3) . . ?
N15 N14 C18 111.8(3) . . ?
C18 N14 C7 128.1(3) . . ?
N14 N15 Ag1 119.1(2) . 2_645 ?
C16 N15 Ag1 136.1(2) . 2_645 ?
C16 N15 N14 104.8(3) . . ?
N15 C16 H16 124.5 . . ?
N15 C16 C17 111.0(3) . . ?
C17 C16 H16 124.5 . . ?
C16 C17 Cl19 126.0(3) . . ?
C18 C17 C16 106.6(3) . . ?
C18 C17 Cl19 127.4(3) . . ?
N14 C18 H18 127.1 . . ?
C17 C18 N14 105.9(3) . . ?
C17 C18 H18 127.1 . . ?
O21 Cl20 O23 107.90(19) . . ?
O22 Cl20 O21 109.5(2) . . ?
O22 Cl20 O23 110.18(18) . . ?
O22 Cl20 O24 110.5(2) . . ?
O24 Cl20 O21 107.9(3) . . ?
O24 Cl20 O23 110.8(2) . . ?
Cl20 O21 Ag1 119.9(2) . . ?

_exptl_crystal_recrystallization_method 
'Re-crystallisation from solvent: nitromethane/diethyl ether'
####################################################################### 
# 
# 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_sf16MeCN
_database_code_depnum_ccdc_archive 'CCDC 1957582'
loop_
_audit_author_name
_audit_author_address
'Malcolm Halcrow' 'University of Leeds'
_audit_update_record             
;
2019-10-04 deposited with the CCDC.	2019-11-05 downloaded from the CCDC.
;
_audit_creation_date             2019-07-08
_audit_creation_method           
;
  Olex2 1.2
  (compiled Apr 23 2013 17:54:37, GUI svn.r4466)
;
_chemical_name_common            ?
_chemical_name_systematic        
'[2,4-Di(3,5-dimethylpyrazol-1-yl)-1,3,5-triazine](acetonitrile)-silver(I) perchlorate'
_chemical_formula_moiety         'C15 H18 Ag N8, Cl O4'
_chemical_formula_sum            'C15 H18 Ag Cl N8 O4'
_chemical_formula_weight         517.69
_chemical_melting_point          ?
loop_
_atom_type_symbol
_atom_type_description
_atom_type_scat_dispersion_real
_atom_type_scat_dispersion_imag
_atom_type_scat_source
C C 0.0181 0.0091 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
N N 0.0311 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'
Ag Ag 0.1306 4.2820 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Cl Cl 0.3639 0.7018 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'

_space_group_crystal_system      triclinic
_space_group_IT_number           2
_space_group_name_H-M_alt        'P -1'
_space_group_name_Hall           '-P 1'
loop_
_space_group_symop_id
_space_group_symop_operation_xyz
1 'x, y, z'
2 '-x, -y, -z'

_cell_length_a                   7.7857(3)
_cell_length_b                   11.0383(5)
_cell_length_c                   12.5260(5)
_cell_angle_alpha                74.006(4)
_cell_angle_beta                 71.927(4)
_cell_angle_gamma                71.187(4)
_cell_volume                     950.11(7)
_cell_formula_units_Z            2
_cell_measurement_reflns_used    5009
_cell_measurement_temperature    120(2)
_cell_measurement_theta_min      3.81
_cell_measurement_theta_max      73.58
_exptl_absorpt_coefficient_mu    10.188
_exptl_absorpt_correction_T_min  0.522
_exptl_absorpt_correction_T_max  1.000
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   
; 
CrysAlisPro, Agilent Technologies,
Version 1.171.36.24 (release 03-12-2012 CrysAlis171 .NET)
Empirical absorption correction using spherical harmonics,
 implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_crystal_colour            colourless
_exptl_crystal_density_diffrn    1.810
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       fragment
_exptl_crystal_F_000             520
_exptl_crystal_size_max          0.40
_exptl_crystal_size_mid          0.25
_exptl_crystal_size_min          0.15
_exptl_special_details           
;
 ? 
;
_diffrn_reflns_av_R_equivalents  0.0262
_diffrn_reflns_av_unetI/netI     0.0318
_diffrn_reflns_limit_h_max       9
_diffrn_reflns_limit_h_min       -8
_diffrn_reflns_limit_k_max       13
_diffrn_reflns_limit_k_min       -11
_diffrn_reflns_limit_l_max       14
_diffrn_reflns_limit_l_min       -15
_diffrn_reflns_number            7034
_diffrn_reflns_theta_full        72.00
_diffrn_reflns_theta_max         73.74
_diffrn_reflns_theta_min         4.31
_diffrn_ambient_temperature      120(2)
_diffrn_detector_area_resol_mean 5.3095
_diffrn_measured_fraction_theta_full 0.939
_diffrn_measured_fraction_theta_max 0.927
_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                3405
_reflns_number_total             3554
_reflns_threshold_expression     >2sigma(I)
_computing_cell_refinement       'CrysAlisPro, Agilent Technologies'
_computing_data_collection       '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         0.905
_refine_diff_density_min         -0.810
_refine_diff_density_rms         0.091
_refine_ls_extinction_coef       ?
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.101
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     267
_refine_ls_number_reflns         3554
_refine_ls_number_restraints     0
_refine_ls_R_factor_all          0.0319
_refine_ls_R_factor_gt           0.0307
_refine_ls_restrained_S_all      1.101
_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)+(0.0364P)²+1.4244P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0783
_refine_ls_wR_factor_ref         0.0791
_refine_special_details          
;
 Refinement of F² against ALL reflections.  The weighted R-factor wR and 
 goodness of fit S are based on F², conventional R-factors R are based 
 on F, with F set to zero for negative F². The threshold expression of 
 F² > 2sigma(F²) is used only for calculating R-factors(gt) etc. and is 
 not relevant to the choice of reflections for refinement.  R-factors based 
 on F² are statistically about twice as large as those based on F, and R- 
 factors based on ALL data will be even larger. 

 No disorder is present in the model, and no restraints were applied to the
 refinement. All non-H atoms were refined anisotropically, and H atoms were
 placed in calculated positions and refined using a riding model.
;
_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.a Aromatic/amide H refined with riding coordinates:
 C5(H5), C11(H11), C18(H18)
2.b Idealised Me refined as rotating group:
 C13(H13A,H13B,H13C), C14(H14A,H14B,H14C), C20(H20A,H20B,H20C), C21(H21A,H21B,
 H21C), C24(H24A,H24B,H24C)
;
_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
Ag1 Ag 0.11913(3) 0.15007(2) 0.110635(18) 0.02208(9) Uani 1 1 d . . .
N2 N 0.2656(3) -0.0162(2) -0.0017(2) 0.0143(5) Uani 1 1 d . . .
C3 C 0.2306(4) -0.0017(3) -0.1026(2) 0.0147(5) Uani 1 1 d . . .
N4 N 0.3024(4) -0.0877(3) -0.1711(2) 0.0205(5) Uani 1 1 d . . .
C5 C 0.4273(5) -0.1927(3) -0.1328(3) 0.0233(7) Uani 1 1 d . . .
H5 H 0.4857 -0.2560 -0.1801 0.028 Uiso 1 1 calc R . .
N6 N 0.4790(4) -0.2184(2) -0.0359(2) 0.0218(6) Uani 1 1 d . . .
C7 C 0.3884(4) -0.1271(3) 0.0279(3) 0.0153(5) Uani 1 1 d . . .
N8 N 0.1063(3) 0.1153(2) -0.1373(2) 0.0152(5) Uani 1 1 d . . .
N9 N 0.0312(3) 0.2049(2) -0.0657(2) 0.0165(5) Uani 1 1 d . . .
C10 C -0.0719(4) 0.3073(3) -0.1217(3) 0.0195(6) Uani 1 1 d . . .
C11 C -0.0663(4) 0.2858(3) -0.2290(3) 0.0199(6) Uani 1 1 d . . .
H11 H -0.1297 0.3449 -0.2842 0.024 Uiso 1 1 calc R . .
C12 C 0.0472(4) 0.1643(3) -0.2383(3) 0.0172(6) Uani 1 1 d . . .
C13 C -0.1732(5) 0.4249(3) -0.0689(3) 0.0247(7) Uani 1 1 d . . .
H13A H -0.1504 0.4086 0.0071 0.037 Uiso 1 1 calc R . .
H13B H -0.3076 0.4431 -0.0618 0.037 Uiso 1 1 calc R . .
H13C H -0.1278 0.5001 -0.1174 0.037 Uiso 1 1 calc R . .
C14 C 0.1053(5) 0.0942(3) -0.3352(3) 0.0207(6) Uani 1 1 d . . .
H14A H 0.0368 0.1456 -0.3936 0.031 Uiso 1 1 calc R . .
H14B H 0.0775 0.0089 -0.3068 0.031 Uiso 1 1 calc R . .
H14C H 0.2400 0.0821 -0.3687 0.031 Uiso 1 1 calc R . .
N15 N 0.4253(3) -0.1463(2) 0.1336(2) 0.0146(5) Uani 1 1 d . . .
N16 N 0.3393(3) -0.0481(2) 0.1965(2) 0.0162(5) Uani 1 1 d . . .
C17 C 0.3917(4) -0.0950(3) 0.2936(3) 0.0185(6) Uani 1 1 d . . .
C18 C 0.5107(4) -0.2231(3) 0.2956(3) 0.0195(6) Uani 1 1 d . . .
H18 H 0.5664 -0.2764 0.3561 0.023 Uiso 1 1 calc R . .
C19 C 0.5301(4) -0.2552(3) 0.1941(3) 0.0178(6) Uani 1 1 d . . .
C20 C 0.3249(5) -0.0149(3) 0.3844(3) 0.0246(7) Uani 1 1 d . . .
H20A H 0.4115 0.0382 0.3717 0.037 Uiso 1 1 calc R . .
H20B H 0.3195 -0.0728 0.4597 0.037 Uiso 1 1 calc R . .
H20C H 0.1999 0.0423 0.3813 0.037 Uiso 1 1 calc R . .
C21 C 0.6376(5) -0.3792(3) 0.1528(3) 0.0224(6) Uani 1 1 d . . .
H21A H 0.7039 -0.4389 0.2098 0.034 Uiso 1 1 calc R . .
H21B H 0.7283 -0.3605 0.0802 0.034 Uiso 1 1 calc R . .
H21C H 0.5513 -0.4196 0.1413 0.034 Uiso 1 1 calc R . .
N22 N -0.0185(4) 0.2650(3) 0.2419(3) 0.0284(6) Uani 1 1 d . . .
C23 C -0.0817(5) 0.3124(3) 0.3189(3) 0.0243(7) Uani 1 1 d . . .
C24 C -0.1624(5) 0.3746(4) 0.4180(3) 0.0337(8) Uani 1 1 d . . .
H24A H -0.2681 0.4491 0.4036 0.051 Uiso 1 1 calc R . .
H24B H -0.0675 0.4049 0.4319 0.051 Uiso 1 1 calc R . .
H24C H -0.2060 0.3116 0.4853 0.051 Uiso 1 1 calc R . .
Cl25 Cl 0.35283(10) 0.36779(6) 0.39702(6) 0.01811(15) Uani 1 1 d . . .
O26 O 0.5162(4) 0.2599(2) 0.3926(3) 0.0383(6) Uani 1 1 d . . .
O27 O 0.2713(4) 0.3811(3) 0.3046(2) 0.0358(6) Uani 1 1 d . . .
O28 O 0.4026(4) 0.4865(2) 0.3848(2) 0.0331(6) Uani 1 1 d . . .
O29 O 0.2186(4) 0.3472(3) 0.5045(2) 0.0332(6) Uani 1 1 d . . .


_geom_special_details            
;
 All esds (except the esd in the dihedral angle between two l.s. planes) 
 are estimated using the full covariance matrix.  The cell esds are taken 
 into account individually in the estimation of esds in distances, angles 
 and torsion angles; correlations between esds in cell parameters are only 
 used when they are defined by crystal symmetry.  An approximate (isotropic) 
 treatment of cell esds is used for estimating esds involving l.s. planes. 
;
loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
_geom_bond_publ_flag
Ag1 N2 2.392(2) . ?
Ag1 N9 2.377(2) . ?
Ag1 N16 2.511(2) . ?
Ag1 N22 2.154(3) . ?
N2 C3 1.331(4) . ?
N2 C7 1.329(4) . ?
C3 N4 1.327(4) . ?
C3 N8 1.392(4) . ?
N4 C5 1.332(4) . ?
C5 H5 0.9500 . ?
C5 N6 1.326(4) . ?
N6 C7 1.337(4) . ?
C7 N15 1.387(4) . ?
N8 N9 1.384(3) . ?
N8 C12 1.388(4) . ?
N9 C10 1.320(4) . ?
C10 C11 1.414(4) . ?
C10 C13 1.495(4) . ?
C11 H11 0.9500 . ?
C11 C12 1.360(4) . ?
C12 C14 1.492(4) . ?
C13 H13A 0.9800 . ?
C13 H13B 0.9800 . ?
C13 H13C 0.9800 . ?
C14 H14A 0.9800 . ?
C14 H14B 0.9800 . ?
C14 H14C 0.9800 . ?
N15 N16 1.385(3) . ?
N15 C19 1.390(4) . ?
N16 C17 1.319(4) . ?
C17 C18 1.417(4) . ?
C17 C20 1.495(4) . ?
C18 H18 0.9500 . ?
C18 C19 1.364(4) . ?
C19 C21 1.491(4) . ?
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 1.124(4) . ?
C23 C24 1.454(4) . ?
C24 H24A 0.9800 . ?
C24 H24B 0.9800 . ?
C24 H24C 0.9800 . ?
Cl25 O26 1.433(2) . ?
Cl25 O27 1.438(2) . ?
Cl25 O28 1.439(2) . ?
Cl25 O29 1.438(3) . ?

loop_
_geom_angle_atom_site_label_1
_geom_angle_atom_site_label_2
_geom_angle_atom_site_label_3
_geom_angle
_geom_angle_site_symmetry_1
_geom_angle_site_symmetry_3
_geom_angle_publ_flag
N2 Ag1 N16 64.64(8) . . ?
N9 Ag1 N2 66.75(8) . . ?
N9 Ag1 N16 131.39(8) . . ?
N22 Ag1 N2 167.71(10) . . ?
N22 Ag1 N9 122.27(10) . . ?
N22 Ag1 N16 105.92(10) . . ?
C3 N2 Ag1 121.06(19) . . ?
C7 N2 Ag1 124.51(19) . . ?
C7 N2 C3 114.4(2) . . ?
N2 C3 N8 115.7(2) . . ?
N4 C3 N2 126.1(3) . . ?
N4 C3 N8 118.2(3) . . ?
C3 N4 C5 113.3(3) . . ?
N4 C5 H5 116.5 . . ?
N6 C5 N4 127.1(3) . . ?
N6 C5 H5 116.5 . . ?
C5 N6 C7 113.4(3) . . ?
N2 C7 N6 125.6(3) . . ?
N2 C7 N15 115.9(3) . . ?
N6 C7 N15 118.5(3) . . ?
N9 N8 C3 118.2(2) . . ?
N9 N8 C12 111.0(2) . . ?
C12 N8 C3 130.7(2) . . ?
N8 N9 Ag1 118.27(17) . . ?
C10 N9 Ag1 136.4(2) . . ?
C10 N9 N8 105.3(2) . . ?
N9 C10 C11 111.0(3) . . ?
N9 C10 C13 119.6(3) . . ?
C11 C10 C13 129.4(3) . . ?
C10 C11 H11 126.5 . . ?
C12 C11 C10 107.0(3) . . ?
C12 C11 H11 126.5 . . ?
N8 C12 C14 124.9(3) . . ?
C11 C12 N8 105.8(3) . . ?
C11 C12 C14 129.3(3) . . ?
C10 C13 H13A 109.5 . . ?
C10 C13 H13B 109.5 . . ?
C10 C13 H13C 109.5 . . ?
H13A C13 H13B 109.5 . . ?
H13A C13 H13C 109.5 . . ?
H13B C13 H13C 109.5 . . ?
C12 C14 H14A 109.5 . . ?
C12 C14 H14B 109.5 . . ?
C12 C14 H14C 109.5 . . ?
H14A C14 H14B 109.5 . . ?
H14A C14 H14C 109.5 . . ?
H14B C14 H14C 109.5 . . ?
C7 N15 C19 130.2(3) . . ?
N16 N15 C7 118.3(2) . . ?
N16 N15 C19 111.4(2) . . ?
N15 N16 Ag1 116.64(17) . . ?
C17 N16 Ag1 138.0(2) . . ?
C17 N16 N15 105.1(2) . . ?
N16 C17 C18 111.2(3) . . ?
N16 C17 C20 120.4(3) . . ?
C18 C17 C20 128.4(3) . . ?
C17 C18 H18 126.5 . . ?
C19 C18 C17 107.0(3) . . ?
C19 C18 H18 126.5 . . ?
N15 C19 C21 125.5(3) . . ?
C18 C19 N15 105.4(3) . . ?
C18 C19 C21 129.1(3) . . ?
C17 C20 H20A 109.5 . . ?
C17 C20 H20B 109.5 . . ?
C17 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 Ag1 171.9(3) . . ?
N22 C23 C24 179.5(4) . . ?
C23 C24 H24A 109.5 . . ?
C23 C24 H24B 109.5 . . ?
C23 C24 H24C 109.5 . . ?
H24A C24 H24B 109.5 . . ?
H24A C24 H24C 109.5 . . ?
H24B C24 H24C 109.5 . . ?
O26 Cl25 O27 109.33(16) . . ?
O26 Cl25 O28 110.07(16) . . ?
O26 Cl25 O29 110.26(17) . . ?
O27 Cl25 O28 108.57(17) . . ?
O27 Cl25 O29 109.61(16) . . ?
O29 Cl25 O28 108.98(15) . . ?

_exptl_crystal_recrystallization_method 
'Re-crystallisation from solvent: acetonitrile/diethyl ether'
####################################################################### 
# 
# 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_sf-16
_database_code_depnum_ccdc_archive 'CCDC 1957579'
loop_
_audit_author_name
_audit_author_address
'Malcolm Halcrow' 'University of Leeds'
_audit_update_record             
;
2019-10-04 deposited with the CCDC.	2019-11-05 downloaded from the CCDC.
;
_audit_creation_date             2019-07-08
_audit_creation_method           
;
  Olex2 1.2
  (compiled Apr 23 2013 17:54:37, GUI svn.r4466)
;
_chemical_name_common            ?
_chemical_name_systematic        
'Tetrakis-[2,4-di(3,5-dimethylpyrazol-1-yl)-1,3,5-triazine]-tetrasilver(I) tetraperchlorate hydrate nitromethane solvate'
_chemical_formula_moiety         
'C52 H60 Ag4 N28, 4(Cl O4), 3.2(C H3 N O2), 1.2(H2 O)'
_chemical_formula_sum            'C55.20 H72 Ag4 Cl4 N31.20 O23.60'
_chemical_formula_weight         2123.52
_chemical_melting_point          ?
loop_
_atom_type_symbol
_atom_type_description
_atom_type_scat_dispersion_real
_atom_type_scat_dispersion_imag
_atom_type_scat_source
C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Ag Ag -0.8971 1.1015 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Cl Cl 0.1484 0.1585 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'

_space_group_crystal_system      monoclinic
_space_group_IT_number           15
_space_group_name_H-M_alt        'C 1 2/c 1'
_space_group_name_Hall           '-C 2yc'
loop_
_space_group_symop_id
_space_group_symop_operation_xyz
1 'x, y, z'
2 '-x, y, -z+1/2'
3 'x+1/2, y+1/2, z'
4 '-x+1/2, y+1/2, -z+1/2'
5 '-x, -y, -z'
6 'x, -y, z-1/2'
7 '-x+1/2, -y+1/2, -z'
8 'x+1/2, -y+1/2, z-1/2'

_cell_length_a                   20.8911(9)
_cell_length_b                   27.7398(10)
_cell_length_c                   15.8143(7)
_cell_angle_alpha                90.00
_cell_angle_beta                 107.315(5)
_cell_angle_gamma                90.00
_cell_volume                     8749.3(6)
_cell_formula_units_Z            4
_cell_measurement_reflns_used    8937
_cell_measurement_temperature    120(2)
_cell_measurement_theta_min      3.21
_cell_measurement_theta_max      26.40
_exptl_absorpt_coefficient_mu    1.089
_exptl_absorpt_correction_T_min  0.591
_exptl_absorpt_correction_T_max  1.000
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   
; 
CrysAlisPro, Agilent Technologies,
Version 1.171.36.24 (release 03-12-2012 CrysAlis171 .NET)
Empirical absorption correction using spherical harmonics,
 implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_crystal_colour            colourless
_exptl_crystal_density_diffrn    1.612
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       needle
_exptl_crystal_F_000             4266
_exptl_crystal_size_max          0.35
_exptl_crystal_size_mid          0.10
_exptl_crystal_size_min          0.05
_exptl_special_details           
;
 ? 
;
_diffrn_reflns_av_R_equivalents  0.0607
_diffrn_reflns_av_unetI/netI     0.0823
_diffrn_reflns_limit_h_max       28
_diffrn_reflns_limit_h_min       -23
_diffrn_reflns_limit_k_max       37
_diffrn_reflns_limit_k_min       -35
_diffrn_reflns_limit_l_max       14
_diffrn_reflns_limit_l_min       -21
_diffrn_reflns_number            31510
_diffrn_reflns_theta_full        26.00
_diffrn_reflns_theta_max         29.54
_diffrn_reflns_theta_min         3.05
_diffrn_ambient_temperature      120(2)
_diffrn_detector_area_resol_mean 5.3095
_diffrn_measured_fraction_theta_full 0.997
_diffrn_measured_fraction_theta_max 0.862
_diffrn_measurement_device_type  'SuperNova, Dual, Mo at zero, Atlas'
_diffrn_measurement_method       'ω scans'
_diffrn_radiation_monochromator  mirror
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_radiation_source         'SuperNova (Mo) X-ray Source'
_diffrn_standards_number         0
_diffrn_standards_interval_count 0
_diffrn_standards_interval_time  0
_diffrn_standards_decay_%        0
_reflns_number_gt                6979
_reflns_number_total             10539
_reflns_threshold_expression     >2sigma(I)
_computing_cell_refinement       'CrysAlisPro, Agilent Technologies'
_computing_data_collection       '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         2.372
_refine_diff_density_min         -1.160
_refine_diff_density_rms         0.172
_refine_ls_extinction_coef       ?
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.038
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     578
_refine_ls_number_reflns         10539
_refine_ls_number_restraints     37
_refine_ls_R_factor_all          0.1197
_refine_ls_R_factor_gt           0.0742
_refine_ls_restrained_S_all      1.039
_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)+(0.0978P)²+86.2927P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1827
_refine_ls_wR_factor_ref         0.2109
_refine_special_details          
;
 Refinement of F² against ALL reflections.  The weighted R-factor wR and 
 goodness of fit S are based on F², conventional R-factors R are based 
 on F, with F set to zero for negative F². The threshold expression of 
 F² > 2sigma(F²) is used only for calculating R-factors(gt) etc. and is 
 not relevant to the choice of reflections for refinement.  R-factors based 
 on F² are statistically about twice as large as those based on F, and R- 
 factors based on ALL data will be even larger. 

 The asymmetric unit contains half a formula unit. That is, half a cyclic
 tetrameric complex, spanning the crystallographic C₂ axis 1/2, y, 3/4;
 two half anions, also on crystallographic C₂ axes; another whole
 perchlorate ion on a general crystallographic position; and three partially
 occupied or disordered solvent sites, one of which is also close to a 
 crystallographic C₂ axis. While all the perchlorate ions are ordered, all 
 the partial nitromethane molecules required fixed restraints to refine to 
 reasonable geometries. The were C---N = 1.45(2), N---O = 1.22(2), O...O = 
 2.09(2) and C...O = 2.30(2) Å. An antibumping restraint between two O
 atoms, including a disordered solvent atom, was also added to deal with
 a CheckCif alert. 

 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.
 H atoms associated with the partially occupied water molecule are not 
 included in the model, but are accounted for in the molecular weight and 
 density calculations.

 The highest residual Fourier peak of +2.4 e.Å⁻³ is 0.9 Å from Cl44. 
;
_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
 C54A-N55A = C58A-N59A = C58B-N59B
 1.45 with sigma of 0.02
 N55A-O56A = N55A-O57A = N59A-O60A = N59A-O61A = N59B-O60B = N59B-O61B
 1.22 with sigma of 0.02
 O56A-O57A = O60A-O61A = O60B-O61B
 2.09 with sigma of 0.02
 C54A-O56A = C54A-O57A = C58A-O60A = C58A-O61A = C58B-O60B = C58B-O61B
 2.3 with sigma of 0.02
 C62A-N63A = C62B-N63B = C62C-N63C
 1.45 with sigma of 0.02
 N63A-O64A = N63A-O65A = N63B-O64B = N63B-O65B = N63C-O64C = N63C-O65C
 1.22 with sigma of 0.02
 O64A-O65A = O64B-O65B = O64C-O65C
 2.09 with sigma of 0.02
 C62A-O64A = C62A-O65A = C62B-O64B = C62B-O65B = C62C-O64C = C62C-O65C
 2.3 with sigma of 0.02
 O53-O65B_$1
 -2.8 with sigma of 0.02
3. Others
 Fixed Sof: C54A(0.4) H54A(0.4) H54B(0.4) H54C(0.4) N55A(0.4) O56A(0.4)
 O57A(0.4) O57B(0.6) C58A(0.25) H58A(0.25) H58B(0.25) H58C(0.25) N59A(0.25)
 O60A(0.25) O61A(0.25) C58B(0.25) H58D(0.25) H58E(0.25) H58F(0.25) N59B(0.25)
 O60B(0.25) O61B(0.25) C62A(0.25) H62A(0.25) H62B(0.25) H62C(0.25) N63A(0.25)
 O64A(0.25) O65A(0.25) C62B(0.25) H62D(0.25) H62E(0.25) H62F(0.25) N63B(0.25)
 O64B(0.25) O65B(0.25) C62C(0.2) H62G(0.2) H62H(0.2) H62I(0.2) N63C(0.2)
 O64C(0.2) O65C(0.2)
4.a Me refined with riding coordinates:
 C54A(H54A,H54B,H54C), C58A(H58A,H58B,H58C), C58B(H58D,H58E,H58F), C62A(H62A,
 H62B,H62C), C62B(H62D,H62E,H62F), C62C(H62G,H62H,H62I)
4.b Aromatic/amide H refined with riding coordinates:
 C4(H4), C12(H12), C19(H19), C24(H24), C32(H32), C39(H39)
4.c Idealised Me refined as rotating group:
 C14(H14A,H14B,H14C), C15(H15A,H15B,H15C), C21(H21A,H21B,H21C), C22(H22A,H22B,
 H22C), C34(H34A,H34B,H34C), C35(H35A,H35B,H35C), C41(H41A,H41B,H41C), C42(H42A,
 H42B,H42C)
;
_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
Ag1 Ag 0.39558(3) 0.648330(18) 0.53245(3) 0.02888(16) Uani 1 1 d . . .
Ag2 Ag 0.73618(3) 0.662677(19) 0.62497(4) 0.03116(16) Uani 1 1 d . . .
N3 N 0.5040(3) 0.63085(19) 0.5067(4) 0.0261(12) Uani 1 1 d . . .
C4 C 0.5614(4) 0.6546(2) 0.5369(5) 0.0296(15) Uani 1 1 d . . .
H4 H 0.5604 0.6839 0.5673 0.036 Uiso 1 1 calc R . .
N5 N 0.6202(3) 0.64108(19) 0.5284(4) 0.0264(12) Uani 1 1 d . . .
C6 C 0.6175(3) 0.5996(2) 0.4846(4) 0.0218(13) Uani 1 1 d . . .
N7 N 0.5639(3) 0.57162(17) 0.4522(3) 0.0194(10) Uani 1 1 d . . .
C8 C 0.5086(3) 0.5892(2) 0.4665(4) 0.0219(13) Uani 1 1 d . . .
N9 N 0.4500(3) 0.56190(18) 0.4402(3) 0.0199(10) Uani 1 1 d . . .
N10 N 0.3941(3) 0.57759(19) 0.4627(4) 0.0240(11) Uani 1 1 d . . .
C11 C 0.3479(3) 0.5446(2) 0.4312(4) 0.0223(13) Uani 1 1 d . . .
C12 C 0.3715(3) 0.5081(2) 0.3867(4) 0.0248(14) Uani 1 1 d . . .
H12 H 0.3472 0.4808 0.3578 0.030 Uiso 1 1 calc R . .
C13 C 0.4365(3) 0.5195(2) 0.3928(4) 0.0237(13) Uani 1 1 d . . .
C14 C 0.2793(3) 0.5495(2) 0.4426(5) 0.0315(15) Uani 1 1 d . . .
H14A H 0.2828 0.5660 0.4986 0.047 Uiso 1 1 calc R . .
H14B H 0.2599 0.5174 0.4435 0.047 Uiso 1 1 calc R . .
H14C H 0.2505 0.5682 0.3933 0.047 Uiso 1 1 calc R . .
C15 C 0.4834(3) 0.4931(2) 0.3557(4) 0.0274(14) Uani 1 1 d . . .
H15A H 0.4961 0.5136 0.3129 0.041 Uiso 1 1 calc R . .
H15B H 0.4616 0.4638 0.3260 0.041 Uiso 1 1 calc R . .
H15C H 0.5236 0.4843 0.4036 0.041 Uiso 1 1 calc R . .
N16 N 0.6788(3) 0.58498(19) 0.4731(3) 0.0223(11) Uani 1 1 d . . .
N17 N 0.7367(3) 0.6069(2) 0.5234(4) 0.0288(12) Uani 1 1 d . . .
C18 C 0.7852(4) 0.5891(3) 0.4955(5) 0.0345(16) Uani 1 1 d . . .
C19 C 0.7598(4) 0.5553(3) 0.4275(5) 0.0334(16) Uani 1 1 d . . .
H19 H 0.7852 0.5377 0.3971 0.040 Uiso 1 1 calc R . .
C20 C 0.6928(3) 0.5522(2) 0.4132(4) 0.0265(14) Uani 1 1 d . . .
C21 C 0.8563(4) 0.6053(3) 0.5381(7) 0.055(2) Uani 1 1 d . . .
H21A H 0.8697 0.6275 0.4983 0.083 Uiso 1 1 calc R . .
H21B H 0.8860 0.5772 0.5497 0.083 Uiso 1 1 calc R . .
H21C H 0.8593 0.6217 0.5940 0.083 Uiso 1 1 calc R . .
C22 C 0.6426(4) 0.5225(3) 0.3489(5) 0.0339(16) Uani 1 1 d . . .
H22A H 0.6639 0.5061 0.3094 0.051 Uiso 1 1 calc R . .
H22B H 0.6063 0.5432 0.3140 0.051 Uiso 1 1 calc R . .
H22C H 0.6243 0.4984 0.3807 0.051 Uiso 1 1 calc R . .
N23 N 0.3399(3) 0.6891(2) 0.6258(4) 0.0323(13) Uani 1 1 d . . .
C24 C 0.3246(4) 0.6700(3) 0.6943(5) 0.0331(16) Uani 1 1 d . . .
H24 H 0.3362 0.6372 0.7078 0.040 Uiso 1 1 calc R . .
N25 N 0.2946(3) 0.6929(2) 0.7451(4) 0.0321(13) Uani 1 1 d . . .
C26 C 0.2774(3) 0.7383(2) 0.7212(4) 0.0267(14) Uani 1 1 d . . .
N27 N 0.2895(3) 0.7618(2) 0.6540(4) 0.0268(12) Uani 1 1 d . . .
C28 C 0.3216(3) 0.7349(2) 0.6094(4) 0.0257(14) Uani 1 1 d . . .
N29 N 0.3388(3) 0.7559(2) 0.5385(4) 0.0269(12) Uani 1 1 d . . .
N30 N 0.3696(3) 0.7271(2) 0.4915(4) 0.0298(13) Uani 1 1 d . . .
C31 C 0.3827(4) 0.7557(3) 0.4317(5) 0.0314(16) Uani 1 1 d . . .
C32 C 0.3595(4) 0.8028(3) 0.4383(5) 0.0364(17) Uani 1 1 d . . .
H32 H 0.3624 0.8296 0.4021 0.044 Uiso 1 1 calc R . .
C33 C 0.3323(4) 0.8027(2) 0.5060(5) 0.0308(15) Uani 1 1 d . . .
C34 C 0.4199(4) 0.7367(3) 0.3702(5) 0.0388(18) Uani 1 1 d . . .
H34A H 0.4669 0.7468 0.3914 0.058 Uiso 1 1 calc R . .
H34B H 0.3993 0.7494 0.3104 0.058 Uiso 1 1 calc R . .
H34C H 0.4175 0.7014 0.3687 0.058 Uiso 1 1 calc R . .
C35 C 0.3026(5) 0.8434(3) 0.5427(6) 0.042(2) Uani 1 1 d . . .
H35A H 0.3032 0.8726 0.5080 0.064 Uiso 1 1 calc R . .
H35B H 0.3287 0.8489 0.6045 0.064 Uiso 1 1 calc R . .
H35C H 0.2562 0.8355 0.5396 0.064 Uiso 1 1 calc R . .
N36 N 0.2429(3) 0.76251(19) 0.7716(3) 0.0259(12) Uani 1 1 d . . .
N37 N 0.2217(3) 0.7360(2) 0.8329(4) 0.0290(12) Uani 1 1 d . . .
C38 C 0.1892(4) 0.7666(3) 0.8687(4) 0.0304(15) Uani 1 1 d . . .
C39 C 0.1897(4) 0.8137(2) 0.8341(5) 0.0308(15) Uani 1 1 d . . .
H39 H 0.1705 0.8417 0.8509 0.037 Uiso 1 1 calc R . .
C40 C 0.2229(3) 0.8109(2) 0.7725(4) 0.0269(14) Uani 1 1 d . . .
C41 C 0.1574(4) 0.7494(3) 0.9369(5) 0.0391(18) Uani 1 1 d . . .
H41A H 0.1687 0.7154 0.9505 0.059 Uiso 1 1 calc R . .
H41B H 0.1086 0.7529 0.9137 0.059 Uiso 1 1 calc R . .
H41C H 0.1741 0.7687 0.9909 0.059 Uiso 1 1 calc R . .
C42 C 0.2357(4) 0.8499(3) 0.7156(5) 0.0400(18) Uani 1 1 d . . .
H42A H 0.2208 0.8808 0.7334 0.060 Uiso 1 1 calc R . .
H42B H 0.2109 0.8433 0.6536 0.060 Uiso 1 1 calc R . .
H42C H 0.2838 0.8515 0.7221 0.060 Uiso 1 1 calc R . .
Cl43 Cl 0.5000 0.63634(11) 0.7500 0.0417(6) Uani 1 2 d S . .
O44 O 0.4486(3) 0.6052(2) 0.6945(4) 0.0502(15) Uani 1 1 d . . .
O45 O 0.5271(4) 0.6657(3) 0.6968(4) 0.076(2) Uani 1 1 d . . .
Cl46 Cl 0.5000 0.64333(8) 0.2500 0.0253(5) Uani 1 2 d S . .
O47 O 0.4660(3) 0.6729(2) 0.1752(4) 0.0407(13) Uani 1 1 d . . .
O48 O 0.4515(3) 0.6135(2) 0.2739(3) 0.0436(14) Uani 1 1 d . . .
Cl49 Cl 0.78320(13) 0.56941(8) 0.78141(16) 0.0545(6) Uani 1 1 d . . .
O50 O 0.7959(5) 0.5202(3) 0.7716(6) 0.091(3) Uani 1 1 d . . .
O51 O 0.7817(4) 0.5786(3) 0.8687(4) 0.078(2) Uani 1 1 d . . .
O52 O 0.7189(4) 0.5809(2) 0.7198(5) 0.0642(18) Uani 1 1 d . . .
O53 O 0.8323(4) 0.5991(3) 0.7618(6) 0.089(3) Uani 1 1 d D . .
C54A C 0.0937(16) 0.5052(9) 0.3113(16) 0.090(9) Uiso 0.40 1 d PD A 1
H54A H 0.0583 0.4818 0.2841 0.135 Uiso 0.40 1 calc PR A 1
H54B H 0.0863 0.5182 0.3652 0.135 Uiso 0.40 1 calc PR A 1
H54C H 0.1374 0.4891 0.3264 0.135 Uiso 0.40 1 calc PR A 1
N55A N 0.0922(8) 0.5438(6) 0.2500(10) 0.044(4) Uiso 0.40 1 d PD A 1
O56A O 0.1309(8) 0.5759(5) 0.2700(11) 0.062(4) Uiso 0.40 1 d PD A 1
O57A O 0.0616(9) 0.5381(7) 0.1710(10) 0.084(6) Uiso 0.40 1 d PD A 1
O57B O 0.0843(7) 0.5829(5) 0.2160(9) 0.076(3) Uiso 0.60 1 d P B 2
C58A C 0.5227(14) 0.8434(8) 0.6008(19) 0.035(7) Uiso 0.25 1 d PD C 1
H58A H 0.5079 0.8516 0.6524 0.053 Uiso 0.25 1 calc PR C 1
H58B H 0.4834 0.8385 0.5491 0.053 Uiso 0.25 1 calc PR C 1
H58C H 0.5500 0.8697 0.5889 0.053 Uiso 0.25 1 calc PR C 1
N59A N 0.5623(13) 0.7993(8) 0.6187(16) 0.042(6) Uiso 0.25 1 d PD C 1
O60A O 0.5743(19) 0.7765(12) 0.564(2) 0.112(13) Uiso 0.25 1 d PD C 1
O61A O 0.581(2) 0.7844(15) 0.695(2) 0.102(13) Uiso 0.25 1 d PD C 1
C58B C 0.503(3) 0.807(4) 0.605(3) 0.20(4) Uiso 0.25 1 d PD D 2
H58D H 0.4790 0.8218 0.6420 0.303 Uiso 0.25 1 calc PR D 2
H58E H 0.4762 0.7812 0.5690 0.303 Uiso 0.25 1 calc PR D 2
H58F H 0.5131 0.8314 0.5653 0.303 Uiso 0.25 1 calc PR D 2
N59B N 0.5665(18) 0.7867(18) 0.661(2) 0.086(13) Uiso 0.25 1 d PD D 2
O60B O 0.6052(9) 0.7695(7) 0.6268(13) 0.033(4) Uiso 0.25 1 d PD D 2
O61B O 0.5727(19) 0.7847(15) 0.740(2) 0.104(12) Uiso 0.25 1 d PD D 2
C62A C 1.033(4) 0.6687(14) 0.793(2) 0.12(2) Uiso 0.25 1 d PD E 1
H62A H 1.0671 0.6891 0.7798 0.187 Uiso 0.25 1 calc PR E 1
H62B H 1.0531 0.6503 0.8470 0.187 Uiso 0.25 1 calc PR E 1
H62C H 0.9968 0.6890 0.8009 0.187 Uiso 0.25 1 calc PR E 1
N63A N 1.0059(16) 0.6359(9) 0.7200(15) 0.059(8) Uiso 0.25 1 d PD . 1
O64A O 1.0032(19) 0.6492(10) 0.6453(15) 0.056(11) Uiso 0.25 1 d PD . 1
O65A O 1.002(2) 0.5933(8) 0.734(2) 0.068(8) Uiso 0.25 1 d PD . 1
C62B C 0.9777(15) 0.6965(17) 0.742(3) 0.087(16) Uiso 0.25 1 d PD F 2
H62D H 0.9329 0.6820 0.7241 0.131 Uiso 0.25 1 calc PR F 2
H62E H 0.9766 0.7269 0.7098 0.131 Uiso 0.25 1 calc PR F 2
H62F H 0.9915 0.7029 0.8058 0.131 Uiso 0.25 1 calc PR F 2
N63B N 1.0255(14) 0.6634(12) 0.721(2) 0.060(8) Uiso 0.25 1 d PD . 2
O64B O 1.014(3) 0.649(2) 0.646(3) 0.15(4) Uiso 0.25 1 d PD G 2
O65B O 1.0825(14) 0.6665(13) 0.769(3) 0.120(14) Uiso 0.25 1 d PD . 2
C62C C 1.0478(15) 0.5623(9) 0.5443(19) 0.020(6) Uiso 0.20 1 d PD H 3
H62G H 1.0540 0.5332 0.5809 0.030 Uiso 0.20 1 calc PR H 3
H62H H 1.0902 0.5706 0.5330 0.030 Uiso 0.20 1 calc PR H 3
H62I H 1.0133 0.5564 0.4878 0.030 Uiso 0.20 1 calc PR H 3
N63C N 1.027(2) 0.6015(10) 0.590(2) 0.068(11) Uiso 0.20 1 d PD H 3
O64C O 1.009(2) 0.5928(14) 0.656(2) 0.109(15) Uiso 0.20 1 d PD H 3
O65C O 1.016(2) 0.6415(9) 0.557(3) 0.090(13) Uiso 0.20 1 d PD H 3


_geom_special_details            
;
 All esds (except the esd in the dihedral angle between two l.s. planes) 
 are estimated using the full covariance matrix.  The cell esds are taken 
 into account individually in the estimation of esds in distances, angles 
 and torsion angles; correlations between esds in cell parameters are only 
 used when they are defined by crystal symmetry.  An approximate (isotropic) 
 treatment of cell esds is used for estimating esds involving l.s. planes. 
;
loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
_geom_bond_publ_flag
Ag1 N3 2.466(5) . ?
Ag1 N10 2.246(5) . ?
Ag1 N23 2.415(6) . ?
Ag1 N30 2.296(6) . ?
Ag1 O44 2.745(6) . ?
Ag2 N5 2.522(6) . ?
Ag2 N17 2.231(6) . ?
Ag2 N25 2.474(6) 2_656 ?
Ag2 N37 2.238(6) 2_656 ?
Ag2 O52 2.802(7) . ?
N3 C4 1.327(9) . ?
N3 C8 1.335(8) . ?
C4 H4 0.9500 . ?
C4 N5 1.328(9) . ?
N5 C6 1.334(8) . ?
C6 N7 1.333(8) . ?
C6 N16 1.407(8) . ?
N7 C8 1.335(8) . ?
C8 N9 1.394(8) . ?
N9 N10 1.389(7) . ?
N9 C13 1.376(8) . ?
N10 C11 1.315(8) . ?
C11 C12 1.403(9) . ?
C11 C14 1.503(9) . ?
C12 H12 0.9500 . ?
C12 C13 1.368(9) . ?
C13 C15 1.479(9) . ?
C14 H14A 0.9800 . ?
C14 H14B 0.9800 . ?
C14 H14C 0.9800 . ?
C15 H15A 0.9800 . ?
C15 H15B 0.9800 . ?
C15 H15C 0.9800 . ?
N16 N17 1.376(8) . ?
N16 C20 1.405(8) . ?
N17 C18 1.318(9) . ?
C18 C19 1.406(11) . ?
C18 C21 1.505(11) . ?
C19 H19 0.9500 . ?
C19 C20 1.354(10) . ?
C20 C22 1.475(10) . ?
C21 H21A 0.9800 . ?
C21 H21B 0.9800 . ?
C21 H21C 0.9800 . ?
C22 H22A 0.9800 . ?
C22 H22B 0.9800 . ?
C22 H22C 0.9800 . ?
N23 C24 1.326(9) . ?
N23 C28 1.329(8) . ?
C24 H24 0.9500 . ?
C24 N25 1.321(9) . ?
N25 C26 1.333(9) . ?
C26 N27 1.334(9) . ?
C26 N36 1.395(8) . ?
N27 C28 1.336(8) . ?
C28 N29 1.401(8) . ?
N29 N30 1.376(7) . ?
N29 C33 1.388(9) . ?
N30 C31 1.325(9) . ?
C31 C32 1.407(10) . ?
C31 C34 1.510(10) . ?
C32 H32 0.9500 . ?
C32 C33 1.354(10) . ?
C33 C35 1.487(9) . ?
C34 H34A 0.9800 . ?
C34 H34B 0.9800 . ?
C34 H34C 0.9800 . ?
C35 H35A 0.9800 . ?
C35 H35B 0.9800 . ?
C35 H35C 0.9800 . ?
N36 N37 1.390(8) . ?
N36 C40 1.408(8) . ?
N37 C38 1.316(8) . ?
C38 C39 1.417(10) . ?
C38 C41 1.501(10) . ?
C39 H39 0.9500 . ?
C39 C40 1.356(9) . ?
C40 C42 1.482(10) . ?
C41 H41A 0.9800 . ?
C41 H41B 0.9800 . ?
C41 H41C 0.9800 . ?
C42 H42A 0.9800 . ?
C42 H42B 0.9800 . ?
C42 H42C 0.9800 . ?
Cl43 O44 1.452(6) . ?
Cl43 O45 1.406(7) . ?
Cl46 O47 1.441(5) . ?
Cl46 O48 1.443(5) . ?
Cl49 O50 1.407(8) . ?
Cl49 O51 1.414(7) . ?
Cl49 O52 1.440(7) . ?
Cl49 O53 1.419(8) . ?
C54A H54A 0.9800 . ?
C54A H54B 0.9800 . ?
C54A H54C 0.9800 . ?
C54A N55A 1.440(15) . ?
N55A O56A 1.181(14) . ?
N55A O57A 1.233(14) . ?
C58A H58A 0.9800 . ?
C58A H58B 0.9800 . ?
C58A H58C 0.9800 . ?
C58A N59A 1.456(16) . ?
N59A O60A 1.162(16) . ?
N59A O61A 1.226(17) . ?
C58B H58D 0.9800 . ?
C58B H58E 0.9800 . ?
C58B H58F 0.9800 . ?
C58B N59B 1.462(18) . ?
N59B O60B 1.196(17) . ?
N59B O61B 1.216(18) . ?
C62A H62A 0.9800 . ?
C62A H62B 0.9800 . ?
C62A H62C 0.9800 . ?
C62A N63A 1.443(17) . ?
N63A O64A 1.221(17) . ?
N63A O65A 1.210(16) . ?
C62B H62D 0.9800 . ?
C62B H62E 0.9800 . ?
C62B H62F 0.9800 . ?
C62B N63B 1.467(18) . ?
N63B O64B 1.201(18) . ?
N63B O65B 1.209(18) . ?
C62C H62G 0.9800 . ?
C62C H62H 0.9800 . ?
C62C H62I 0.9800 . ?
C62C N63C 1.440(17) . ?
N63C O64C 1.236(17) . ?
N63C O65C 1.217(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
N3 Ag1 O44 86.20(19) . . ?
N10 Ag1 N3 68.07(18) . . ?
N10 Ag1 N23 140.3(2) . . ?
N10 Ag1 N30 136.43(19) . . ?
N10 Ag1 O44 91.17(18) . . ?
N23 Ag1 N3 145.7(2) . . ?
N23 Ag1 O44 76.52(19) . . ?
N30 Ag1 N3 107.0(2) . . ?
N30 Ag1 N23 67.11(19) . . ?
N30 Ag1 O44 132.34(19) . . ?
N5 Ag2 O52 83.00(19) . . ?
N17 Ag2 N5 66.98(19) . . ?
N17 Ag2 N25 152.9(2) . 2_656 ?
N17 Ag2 N37 139.3(2) . 2_656 ?
N17 Ag2 O52 81.5(2) . . ?
N25 Ag2 N5 98.23(19) 2_656 . ?
N25 Ag2 O52 74.0(2) 2_656 . ?
N37 Ag2 N5 128.2(2) 2_656 . ?
N37 Ag2 N25 67.71(19) 2_656 2_656 ?
N37 Ag2 O52 132.74(19) 2_656 . ?
C4 N3 Ag1 128.3(4) . . ?
C4 N3 C8 114.5(6) . . ?
C8 N3 Ag1 116.6(4) . . ?
N3 C4 H4 117.0 . . ?
N3 C4 N5 126.0(6) . . ?
N5 C4 H4 117.0 . . ?
C4 N5 Ag2 128.5(4) . . ?
C4 N5 C6 113.4(6) . . ?
C6 N5 Ag2 113.8(4) . . ?
N5 C6 N16 114.6(6) . . ?
N7 C6 N5 127.1(6) . . ?
N7 C6 N16 118.3(5) . . ?
C6 N7 C8 113.0(5) . . ?
N3 C8 N7 125.9(6) . . ?
N3 C8 N9 115.6(5) . . ?
N7 C8 N9 118.5(5) . . ?
N10 N9 C8 118.9(5) . . ?
C13 N9 C8 130.3(5) . . ?
C13 N9 N10 110.8(5) . . ?
N9 N10 Ag1 120.6(4) . . ?
C11 N10 Ag1 134.1(4) . . ?
C11 N10 N9 105.2(5) . . ?
N10 C11 C12 111.4(6) . . ?
N10 C11 C14 120.6(6) . . ?
C12 C11 C14 128.0(6) . . ?
C11 C12 H12 126.7 . . ?
C13 C12 C11 106.6(6) . . ?
C13 C12 H12 126.7 . . ?
N9 C13 C15 125.9(6) . . ?
C12 C13 N9 106.0(6) . . ?
C12 C13 C15 128.1(6) . . ?
C11 C14 H14A 109.5 . . ?
C11 C14 H14B 109.5 . . ?
C11 C14 H14C 109.5 . . ?
H14A C14 H14B 109.5 . . ?
H14A C14 H14C 109.5 . . ?
H14B C14 H14C 109.5 . . ?
C13 C15 H15A 109.5 . . ?
C13 C15 H15B 109.5 . . ?
C13 C15 H15C 109.5 . . ?
H15A C15 H15B 109.5 . . ?
H15A C15 H15C 109.5 . . ?
H15B C15 H15C 109.5 . . ?
N17 N16 C6 118.3(5) . . ?
N17 N16 C20 110.7(5) . . ?
C20 N16 C6 130.9(5) . . ?
N16 N17 Ag2 122.1(4) . . ?
C18 N17 Ag2 132.1(5) . . ?
C18 N17 N16 105.7(6) . . ?
N17 C18 C19 110.7(6) . . ?
N17 C18 C21 119.5(7) . . ?
C19 C18 C21 129.7(7) . . ?
C18 C19 H19 126.1 . . ?
C20 C19 C18 107.8(6) . . ?
C20 C19 H19 126.1 . . ?
N16 C20 C22 125.4(6) . . ?
C19 C20 N16 105.0(6) . . ?
C19 C20 C22 129.6(6) . . ?
C18 C21 H21A 109.5 . . ?
C18 C21 H21B 109.5 . . ?
C18 C21 H21C 109.5 . . ?
H21A C21 H21B 109.5 . . ?
H21A C21 H21C 109.5 . . ?
H21B C21 H21C 109.5 . . ?
C20 C22 H22A 109.5 . . ?
C20 C22 H22B 109.5 . . ?
C20 C22 H22C 109.5 . . ?
H22A C22 H22B 109.5 . . ?
H22A C22 H22C 109.5 . . ?
H22B C22 H22C 109.5 . . ?
C24 N23 Ag1 126.1(4) . . ?
C24 N23 C28 114.5(6) . . ?
C28 N23 Ag1 119.4(4) . . ?
N23 C24 H24 117.3 . . ?
N25 C24 N23 125.4(6) . . ?
N25 C24 H24 117.3 . . ?
C24 N25 Ag2 129.1(5) . 2_656 ?
C24 N25 C26 114.6(6) . . ?
C26 N25 Ag2 116.2(4) . 2_656 ?
N25 C26 N27 126.1(6) . . ?
N25 C26 N36 115.7(6) . . ?
N27 C26 N36 118.2(6) . . ?
C26 N27 C28 113.0(5) . . ?
N23 C28 N27 126.3(6) . . ?
N23 C28 N29 115.2(6) . . ?
N27 C28 N29 118.5(6) . . ?
N30 N29 C28 117.6(5) . . ?
N30 N29 C33 110.6(5) . . ?
C33 N29 C28 131.7(5) . . ?
N29 N30 Ag1 120.6(4) . . ?
C31 N30 Ag1 133.7(4) . . ?
C31 N30 N29 105.4(5) . . ?
N30 C31 C32 110.9(6) . . ?
N30 C31 C34 120.3(6) . . ?
C32 C31 C34 128.8(7) . . ?
C31 C32 H32 126.6 . . ?
C33 C32 C31 106.9(7) . . ?
C33 C32 H32 126.6 . . ?
N29 C33 C35 124.9(6) . . ?
C32 C33 N29 106.2(6) . . ?
C32 C33 C35 128.9(7) . . ?
C31 C34 H34A 109.5 . . ?
C31 C34 H34B 109.5 . . ?
C31 C34 H34C 109.5 . . ?
H34A C34 H34B 109.5 . . ?
H34A C34 H34C 109.5 . . ?
H34B C34 H34C 109.5 . . ?
C33 C35 H35A 109.5 . . ?
C33 C35 H35B 109.5 . . ?
C33 C35 H35C 109.5 . . ?
H35A C35 H35B 109.5 . . ?
H35A C35 H35C 109.5 . . ?
H35B C35 H35C 109.5 . . ?
C26 N36 C40 132.1(6) . . ?
N37 N36 C26 118.0(5) . . ?
N37 N36 C40 109.9(5) . . ?
N36 N37 Ag2 120.6(4) . 2_656 ?
C38 N37 Ag2 131.7(5) . 2_656 ?
C38 N37 N36 105.8(5) . . ?
N37 C38 C39 111.3(6) . . ?
N37 C38 C41 120.0(6) . . ?
C39 C38 C41 128.7(6) . . ?
C38 C39 H39 126.5 . . ?
C40 C39 C38 106.9(6) . . ?
C40 C39 H39 126.5 . . ?
N36 C40 C42 125.6(6) . . ?
C39 C40 N36 106.1(6) . . ?
C39 C40 C42 128.2(6) . . ?
C38 C41 H41A 109.5 . . ?
C38 C41 H41B 109.5 . . ?
C38 C41 H41C 109.5 . . ?
H41A C41 H41B 109.5 . . ?
H41A C41 H41C 109.5 . . ?
H41B C41 H41C 109.5 . . ?
C40 C42 H42A 109.5 . . ?
C40 C42 H42B 109.5 . . ?
C40 C42 H42C 109.5 . . ?
H42A C42 H42B 109.5 . . ?
H42A C42 H42C 109.5 . . ?
H42B C42 H42C 109.5 . . ?
O44 Cl43 O44 107.0(5) . 2_656 ?
O45 Cl43 O44 110.4(4) . 2_656 ?
O45 Cl43 O44 109.9(4) . . ?
O45 Cl43 O45 109.1(7) . 2_656 ?
Cl43 O44 Ag1 109.0(3) . . ?
O47 Cl46 O47 110.7(5) . 2_655 ?
O47 Cl46 O48 109.2(3) . . ?
O47 Cl46 O48 108.9(3) . 2_655 ?
O48 Cl46 O48 110.0(5) 2_655 . ?
O50 Cl49 O51 110.0(5) . . ?
O50 Cl49 O52 107.9(5) . . ?
O50 Cl49 O53 111.5(6) . . ?
O51 Cl49 O52 109.5(5) . . ?
O51 Cl49 O53 109.6(5) . . ?
O53 Cl49 O52 108.3(5) . . ?
Cl49 O52 Ag2 107.4(3) . . ?
H54A C54A H54B 109.5 . . ?
H54A C54A H54C 109.5 . . ?
H54B C54A H54C 109.5 . . ?
N55A C54A H54A 109.5 . . ?
N55A C54A H54B 109.5 . . ?
N55A C54A H54C 109.5 . . ?
O56A N55A C54A 120.4(15) . . ?
O56A N55A O57A 118.3(15) . . ?
O57A N55A C54A 119.2(15) . . ?
H58A C58A H58B 109.5 . . ?
H58A C58A H58C 109.5 . . ?
H58B C58A H58C 109.5 . . ?
N59A C58A H58A 109.5 . . ?
N59A C58A H58B 109.5 . . ?
N59A C58A H58C 109.5 . . ?
O60A N59A C58A 123.3(18) . . ?
O60A N59A O61A 118.3(19) . . ?
O61A N59A C58A 118.3(17) . . ?
H58D C58B H58E 109.5 . . ?
H58D C58B H58F 109.5 . . ?
H58E C58B H58F 109.5 . . ?
N59B C58B H58D 109.5 . . ?
N59B C58B H58E 109.5 . . ?
N59B C58B H58F 109.5 . . ?
O60B N59B C58B 119.2(19) . . ?
O60B N59B O61B 124(2) . . ?
O61B N59B C58B 116.2(18) . . ?
H62A C62A H62B 109.5 . . ?
H62A C62A H62C 109.5 . . ?
H62B C62A H62C 109.5 . . ?
N63A C62A H62A 109.5 . . ?
N63A C62A H62B 109.5 . . ?
N63A C62A H62C 109.5 . . ?
O64A N63A C62A 118.5(19) . . ?
O65A N63A C62A 120.3(19) . . ?
O65A N63A O64A 118.7(18) . . ?
H62D C62B H62E 109.5 . . ?
H62D C62B H62F 109.5 . . ?
H62E C62B H62F 109.5 . . ?
N63B C62B H62D 109.5 . . ?
N63B C62B H62E 109.5 . . ?
N63B C62B H62F 109.5 . . ?
O64B N63B C62B 118(2) . . ?
O64B N63B O65B 121(2) . . ?
O65B N63B C62B 115.0(18) . . ?
H62G C62C H62H 109.5 . . ?
H62G C62C H62I 109.5 . . ?
H62H C62C H62I 109.5 . . ?
N63C C62C H62G 109.5 . . ?
N63C C62C H62H 109.5 . . ?
N63C C62C H62I 109.5 . . ?
O64C N63C C62C 119.2(18) . . ?
O65C N63C C62C 122.2(19) . . ?
O65C N63C O64C 117.3(19) . . ?

_exptl_crystal_recrystallization_method 
'Re-crystallisation from solvent: nitromethane/diethyl ether'
####################################################################### 
# 
# 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_150ncs-2
_database_code_depnum_ccdc_archive 'CCDC 1957583'
loop_
_audit_author_name
_audit_author_address
'Malcolm Halcrow' 'University of Leeds'
_audit_update_record             
;
2019-10-04 deposited with the CCDC.	2019-11-05 downloaded from the CCDC.
;
_audit_creation_date             2019-07-05
_audit_creation_method           
;
  Olex2 1.2
  (compiled Apr 23 2013 17:54:37, GUI svn.r4466)
;
_chemical_name_common            ?
_chemical_name_systematic        
;
Bis-[4,6-di(pyrazol-1-yl)pyrimidine]-di[isothiocyanato]iron(II)
;
_chemical_formula_moiety         'C22 H16 Fe N14 S2'
_chemical_formula_sum            'C22 H16 Fe N14 S2'
_chemical_formula_weight         596.46
_chemical_melting_point          ?
loop_
_atom_type_symbol
_atom_type_description
_atom_type_scat_dispersion_real
_atom_type_scat_dispersion_imag
_atom_type_scat_source
C C 0.0181 0.0091 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
N N 0.0311 0.0180 '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'
S S 0.3331 0.5567 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'

_space_group_crystal_system      triclinic
_space_group_IT_number           2
_space_group_name_H-M_alt        'P -1'
_space_group_name_Hall           '-P 1'
loop_
_space_group_symop_id
_space_group_symop_operation_xyz
1 'x, y, z'
2 '-x, -y, -z'

_cell_length_a                   8.1002(4)
_cell_length_b                   11.5650(6)
_cell_length_c                   14.0754(7)
_cell_angle_alpha                101.393(4)
_cell_angle_beta                 93.048(4)
_cell_angle_gamma                91.065(4)
_cell_volume                     1290.19(11)
_cell_formula_units_Z            2
_cell_measurement_reflns_used    5745
_cell_measurement_temperature    120(2)
_cell_measurement_theta_min      3.88
_cell_measurement_theta_max      73.38
_exptl_absorpt_coefficient_mu    6.565
_exptl_absorpt_correction_T_min  0.799
_exptl_absorpt_correction_T_max  1.000
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   
; 
CrysAlisPro, Agilent Technologies,
Version 1.171.36.24 (release 03-12-2012 CrysAlis171 .NET)
Empirical absorption correction using spherical harmonics,
 implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_crystal_colour            red
_exptl_crystal_density_diffrn    1.535
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       'rectangular prism'
_exptl_crystal_F_000             608
_exptl_crystal_size_max          0.35
_exptl_crystal_size_mid          0.25
_exptl_crystal_size_min          0.10
_exptl_special_details           
;
 ? 
;
_diffrn_reflns_av_R_equivalents  0.0260
_diffrn_reflns_av_unetI/netI     0.0354
_diffrn_reflns_limit_h_max       8
_diffrn_reflns_limit_h_min       -10
_diffrn_reflns_limit_k_max       14
_diffrn_reflns_limit_k_min       -14
_diffrn_reflns_limit_l_max       17
_diffrn_reflns_limit_l_min       -16
_diffrn_reflns_number            9319
_diffrn_reflns_theta_full        72.00
_diffrn_reflns_theta_max         73.82
_diffrn_reflns_theta_min         3.90
_diffrn_ambient_temperature      120(2)
_diffrn_detector_area_resol_mean 5.3095
_diffrn_measured_fraction_theta_full 0.947
_diffrn_measured_fraction_theta_max 0.929
_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                4552
_reflns_number_total             4858
_reflns_threshold_expression     >2sigma(I)
_computing_cell_refinement       'CrysAlisPro, Agilent Technologies'
_computing_data_collection       '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         0.259
_refine_diff_density_min         -0.301
_refine_diff_density_rms         0.052
_refine_ls_extinction_coef       ?
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.018
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     352
_refine_ls_number_reflns         4858
_refine_ls_number_restraints     0
_refine_ls_R_factor_all          0.0324
_refine_ls_R_factor_gt           0.0295
_refine_ls_restrained_S_all      1.018
_refine_ls_shift/su_max          0.002
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details     
'calc w=1/[σ²(Fo²)+(0.0375P)²+0.4165P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0731
_refine_ls_wR_factor_ref         0.0753
_refine_special_details          
;
 Refinement of F² against ALL reflections.  The weighted R-factor wR and 
 goodness of fit S are based on F², conventional R-factors R are based 
 on F, with F set to zero for negative F². The threshold expression of 
 F² > 2sigma(F²) is used only for calculating R-factors(gt) etc. and is 
 not relevant to the choice of reflections for refinement.  R-factors based 
 on F² are statistically about twice as large as those based on F, and R- 
 factors based on ALL data will be even larger. 

 No disorder is present in the model and no restraints are included in the
 refinement. All non-H atoms were refined anisotropically and H atoms
 were placed in calculated positions and refined using a riding model.
;
_olex2_refinement_description    
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups
2.a Aromatic/amide H refined with riding coordinates:
 C8(H8), C11(H11), C16(H16), C17(H17), C18(H18), C21(H21), C22(H22), C23(H23),
 C24(H24), C27(H27), C32(H32), C33(H33), C34(H34), C37(H37), C38(H38), C39(H39)
;
_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 0.45637(3) 0.28193(2) 0.734327(19) 0.01644(8) Uani 1 1 d . . .
N2 N 0.55194(18) 0.45448(13) 0.78763(12) 0.0236(3) Uani 1 1 d . . .
C3 C 0.6010(2) 0.55029(16) 0.81896(12) 0.0196(3) Uani 1 1 d . . .
S4 S 0.67326(6) 0.68403(4) 0.86315(3) 0.02748(11) Uani 1 1 d . . .
N5 N 0.65089(19) 0.23415(15) 0.64679(12) 0.0266(3) Uani 1 1 d . . .
C6 C 0.7476(2) 0.16029(16) 0.62920(12) 0.0213(4) Uani 1 1 d . . .
S7 S 0.88479(6) 0.06034(5) 0.60483(4) 0.03217(12) Uani 1 1 d . . .
C8 C 0.6412(2) 0.27553(16) 0.93760(13) 0.0213(4) Uani 1 1 d . . .
H8 H 0.6384 0.3590 0.9455 0.026 Uiso 1 1 calc R . .
N9 N 0.55359(17) 0.21313(13) 0.86126(10) 0.0188(3) Uani 1 1 d . . .
C10 C 0.5530(2) 0.09547(15) 0.85277(12) 0.0175(3) Uani 1 1 d . . .
C11 C 0.6373(2) 0.04043(16) 0.91874(12) 0.0190(3) Uani 1 1 d . . .
H11 H 0.6329 -0.0427 0.9139 0.023 Uiso 1 1 calc R . .
C12 C 0.7289(2) 0.11607(16) 0.99249(12) 0.0186(3) Uani 1 1 d . . .
N13 N 0.73187(18) 0.23380(13) 1.00367(11) 0.0209(3) Uani 1 1 d . . .
N14 N 0.46437(17) 0.03223(13) 0.77062(11) 0.0183(3) Uani 1 1 d . . .
N15 N 0.38508(17) 0.09414(13) 0.70896(11) 0.0191(3) Uani 1 1 d . . .
C16 C 0.3179(2) 0.01289(16) 0.63752(13) 0.0224(4) Uani 1 1 d . . .
H16 H 0.2545 0.0296 0.5834 0.027 Uiso 1 1 calc R . .
C17 C 0.3520(2) -0.10152(17) 0.65158(14) 0.0264(4) Uani 1 1 d . . .
H17 H 0.3173 -0.1741 0.6103 0.032 Uiso 1 1 calc R . .
C18 C 0.4452(2) -0.08654(16) 0.73694(14) 0.0239(4) Uani 1 1 d . . .
H18 H 0.4884 -0.1470 0.7671 0.029 Uiso 1 1 calc R . .
N19 N 0.82720(18) 0.07220(13) 1.06072(10) 0.0193(3) Uani 1 1 d . . .
N20 N 0.81031(19) -0.04219(14) 1.07165(11) 0.0237(3) Uani 1 1 d . . .
C21 C 0.9200(2) -0.04912(17) 1.14350(13) 0.0248(4) Uani 1 1 d . . .
H21 H 0.9368 -0.1186 1.1687 0.030 Uiso 1 1 calc R . .
C22 C 1.0089(2) 0.05811(18) 1.17830(13) 0.0244(4) Uani 1 1 d . . .
H22 H 1.0936 0.0739 1.2289 0.029 Uiso 1 1 calc R . .
C23 C 0.9475(2) 0.13389(17) 1.12391(13) 0.0235(4) Uani 1 1 d . . .
H23 H 0.9812 0.2140 1.1287 0.028 Uiso 1 1 calc R . .
C24 C 0.2994(2) 0.29070(16) 0.52285(13) 0.0231(4) Uani 1 1 d . . .
H24 H 0.4057 0.2663 0.5030 0.028 Uiso 1 1 calc R . .
N25 N 0.27497(18) 0.30379(13) 0.61790(10) 0.0187(3) Uani 1 1 d . . .
C26 C 0.1231(2) 0.33684(14) 0.64395(12) 0.0177(3) Uani 1 1 d . . .
C27 C -0.0013(2) 0.35799(15) 0.57942(13) 0.0197(3) Uani 1 1 d . . .
H27 H -0.1082 0.3817 0.5988 0.024 Uiso 1 1 calc R . .
C28 C 0.0425(2) 0.34181(15) 0.48394(13) 0.0207(3) Uani 1 1 d . . .
N29 N 0.1905(2) 0.30833(14) 0.45372(11) 0.0245(3) Uani 1 1 d . . .
N30 N 0.09910(17) 0.34984(13) 0.74330(11) 0.0183(3) Uani 1 1 d . . .
N31 N 0.22801(18) 0.33017(13) 0.80386(10) 0.0194(3) Uani 1 1 d . . .
C32 C 0.1726(2) 0.35542(17) 0.89238(13) 0.0243(4) Uani 1 1 d . . .
H32 H 0.2358 0.3500 0.9501 0.029 Uiso 1 1 calc R . .
C33 C 0.0078(2) 0.39130(18) 0.88947(14) 0.0283(4) Uani 1 1 d . . .
H33 H -0.0593 0.4139 0.9430 0.034 Uiso 1 1 calc R . .
C34 C -0.0354(2) 0.38682(17) 0.79377(14) 0.0246(4) Uani 1 1 d . . .
H34 H -0.1394 0.4059 0.7674 0.030 Uiso 1 1 calc R . .
N35 N -0.07455(19) 0.36161(13) 0.41205(11) 0.0225(3) Uani 1 1 d . . .
N36 N -0.2305(2) 0.39517(14) 0.43715(12) 0.0258(3) Uani 1 1 d . . .
C37 C -0.3064(3) 0.40468(17) 0.35341(15) 0.0297(4) Uani 1 1 d . . .
H37 H -0.4182 0.4268 0.3468 0.036 Uiso 1 1 calc R . .
C38 C -0.2027(3) 0.37828(18) 0.27522(15) 0.0324(5) Uani 1 1 d . . .
H38 H -0.2303 0.3790 0.2089 0.039 Uiso 1 1 calc R . .
C39 C -0.0543(3) 0.35149(17) 0.31491(14) 0.0278(4) Uani 1 1 d . . .
H39 H 0.0431 0.3301 0.2818 0.033 Uiso 1 1 calc R . .


_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 2.1056(16) . ?
Fe1 N5 2.0679(16) . ?
Fe1 N9 2.2092(15) . ?
Fe1 N15 2.1916(15) . ?
Fe1 N25 2.1976(14) . ?
Fe1 N31 2.1693(15) . ?
N2 C3 1.163(2) . ?
C3 S4 1.6337(18) . ?
N5 C6 1.169(3) . ?
C6 S7 1.6190(19) . ?
C8 H8 0.9500 . ?
C8 N9 1.331(2) . ?
C8 N13 1.325(2) . ?
N9 C10 1.342(2) . ?
C10 C11 1.384(2) . ?
C10 N14 1.395(2) . ?
C11 H11 0.9500 . ?
C11 C12 1.389(2) . ?
C12 N13 1.339(2) . ?
C12 N19 1.393(2) . ?
N14 N15 1.372(2) . ?
N14 C18 1.365(2) . ?
N15 C16 1.319(2) . ?
C16 H16 0.9500 . ?
C16 C17 1.406(3) . ?
C17 H17 0.9500 . ?
C17 C18 1.364(3) . ?
C18 H18 0.9500 . ?
N19 N20 1.367(2) . ?
N19 C23 1.371(2) . ?
N20 C21 1.326(2) . ?
C21 H21 0.9500 . ?
C21 C22 1.409(3) . ?
C22 H22 0.9500 . ?
C22 C23 1.358(3) . ?
C23 H23 0.9500 . ?
C24 H24 0.9500 . ?
C24 N25 1.342(2) . ?
C24 N29 1.327(2) . ?
N25 C26 1.343(2) . ?
C26 C27 1.378(2) . ?
C26 N30 1.401(2) . ?
C27 H27 0.9500 . ?
C27 C28 1.386(3) . ?
C28 N29 1.332(2) . ?
C28 N35 1.405(2) . ?
N30 N31 1.364(2) . ?
N30 C34 1.362(2) . ?
N31 C32 1.327(2) . ?
C32 H32 0.9500 . ?
C32 C33 1.406(3) . ?
C33 H33 0.9500 . ?
C33 C34 1.364(3) . ?
C34 H34 0.9500 . ?
N35 N36 1.372(2) . ?
N35 C39 1.368(2) . ?
N36 C37 1.325(2) . ?
C37 H37 0.9500 . ?
C37 C38 1.409(3) . ?
C38 H38 0.9500 . ?
C38 C39 1.365(3) . ?
C39 H39 0.9500 . ?

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 94.28(6) . . ?
N2 Fe1 N15 166.98(6) . . ?
N2 Fe1 N25 103.46(6) . . ?
N2 Fe1 N31 89.48(6) . . ?
N5 Fe1 N2 93.98(6) . . ?
N5 Fe1 N9 97.37(6) . . ?
N5 Fe1 N15 87.31(6) . . ?
N5 Fe1 N25 96.75(6) . . ?
N5 Fe1 N31 170.53(6) . . ?
N15 Fe1 N9 72.71(5) . . ?
N15 Fe1 N25 89.23(5) . . ?
N25 Fe1 N9 156.43(6) . . ?
N31 Fe1 N9 91.15(5) . . ?
N31 Fe1 N15 91.30(6) . . ?
N31 Fe1 N25 73.85(5) . . ?
C3 N2 Fe1 177.98(16) . . ?
N2 C3 S4 178.99(16) . . ?
C6 N5 Fe1 141.10(15) . . ?
N5 C6 S7 178.65(17) . . ?
N9 C8 H8 116.5 . . ?
N13 C8 H8 116.5 . . ?
N13 C8 N9 127.01(17) . . ?
C8 N9 Fe1 125.46(12) . . ?
C8 N9 C10 116.06(15) . . ?
C10 N9 Fe1 117.14(11) . . ?
N9 C10 C11 122.87(15) . . ?
N9 C10 N14 114.81(15) . . ?
C11 C10 N14 122.29(16) . . ?
C10 C11 H11 122.6 . . ?
C10 C11 C12 114.83(16) . . ?
C12 C11 H11 122.6 . . ?
C11 C12 N19 120.93(16) . . ?
N13 C12 C11 123.97(16) . . ?
N13 C12 N19 115.10(15) . . ?
C8 N13 C12 115.15(15) . . ?
N15 N14 C10 118.31(14) . . ?
C18 N14 C10 130.41(15) . . ?
C18 N14 N15 111.24(14) . . ?
N14 N15 Fe1 114.64(10) . . ?
C16 N15 Fe1 137.86(13) . . ?
C16 N15 N14 104.96(14) . . ?
N15 C16 H16 124.2 . . ?
N15 C16 C17 111.51(16) . . ?
C17 C16 H16 124.2 . . ?
C16 C17 H17 127.2 . . ?
C18 C17 C16 105.62(16) . . ?
C18 C17 H17 127.2 . . ?
N14 C18 H18 126.7 . . ?
C17 C18 N14 106.67(16) . . ?
C17 C18 H18 126.7 . . ?
N20 N19 C12 121.52(14) . . ?
N20 N19 C23 112.11(15) . . ?
C23 N19 C12 126.37(16) . . ?
C21 N20 N19 103.68(15) . . ?
N20 C21 H21 123.8 . . ?
N20 C21 C22 112.49(16) . . ?
C22 C21 H21 123.8 . . ?
C21 C22 H22 127.5 . . ?
C23 C22 C21 105.09(16) . . ?
C23 C22 H22 127.5 . . ?
N19 C23 H23 126.7 . . ?
C22 C23 N19 106.62(17) . . ?
C22 C23 H23 126.7 . . ?
N25 C24 H24 116.6 . . ?
N29 C24 H24 116.6 . . ?
N29 C24 N25 126.73(17) . . ?
C24 N25 Fe1 127.32(12) . . ?
C24 N25 C26 115.51(15) . . ?
C26 N25 Fe1 117.14(11) . . ?
N25 C26 C27 123.58(16) . . ?
N25 C26 N30 114.91(14) . . ?
C27 C26 N30 121.50(16) . . ?
C26 C27 H27 122.8 . . ?
C26 C27 C28 114.37(16) . . ?
C28 C27 H27 122.8 . . ?
C27 C28 N35 119.20(16) . . ?
N29 C28 C27 124.73(16) . . ?
N29 C28 N35 116.06(16) . . ?
C24 N29 C28 115.07(16) . . ?
N31 N30 C26 118.78(14) . . ?
C34 N30 C26 129.87(15) . . ?
C34 N30 N31 111.24(14) . . ?
N30 N31 Fe1 115.28(11) . . ?
C32 N31 Fe1 139.25(12) . . ?
C32 N31 N30 105.28(14) . . ?
N31 C32 H32 124.5 . . ?
N31 C32 C33 110.99(16) . . ?
C33 C32 H32 124.5 . . ?
C32 C33 H33 127.2 . . ?
C34 C33 C32 105.61(17) . . ?
C34 C33 H33 127.2 . . ?
N30 C34 C33 106.88(16) . . ?
N30 C34 H34 126.6 . . ?
C33 C34 H34 126.6 . . ?
N36 N35 C28 119.64(16) . . ?
C39 N35 C28 127.77(17) . . ?
C39 N35 N36 112.60(15) . . ?
C37 N36 N35 103.53(17) . . ?
N36 C37 H37 123.8 . . ?
N36 C37 C38 112.38(18) . . ?
C38 C37 H37 123.8 . . ?
C37 C38 H38 127.3 . . ?
C39 C38 C37 105.47(17) . . ?
C39 C38 H38 127.3 . . ?
N35 C39 H39 127.0 . . ?
C38 C39 N35 106.02(19) . . ?
C38 C39 H39 127.0 . . ?

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

data_sf-16c
_database_code_depnum_ccdc_archive 'CCDC 1957578'
loop_
_audit_author_name
_audit_author_address
'Malcolm Halcrow' 'University of Leeds'
_audit_update_record             
;
2019-11-03 deposited with the CCDC.	2019-11-05 downloaded from the CCDC.
;
_audit_creation_date             2019-07-08
_audit_creation_method           
;
  Olex2 1.2
  (compiled Apr 23 2013 17:54:37, GUI svn.r4466)
;
_chemical_name_common            ?
_chemical_name_systematic        
'Tetrakis-[2,4-di(3,5-dimethylpyrazol-1-yl)-6H-1,3,5-triazine)]-tetrasilver(I) tetra-perchlorate'
_chemical_formula_moiety         'C52 H60 Ag4 N28, 4(Cl O4)'
_chemical_formula_sum            'C52 H60 Ag4 Cl4 N28 O16'
_chemical_formula_weight         1906.56
_chemical_absolute_configuration ad
_chemical_melting_point          ?
loop_
_atom_type_symbol
_atom_type_description
_atom_type_scat_dispersion_real
_atom_type_scat_dispersion_imag
_atom_type_scat_source
C C 0.0181 0.0091 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
N N 0.0311 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'
Ag Ag 0.1306 4.2820 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Cl Cl 0.3639 0.7018 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'

_space_group_crystal_system      tetragonal
_space_group_IT_number           114
_space_group_name_H-M_alt        'P -4 21 c'
_space_group_name_Hall           'P -4 2n'
loop_
_space_group_symop_id
_space_group_symop_operation_xyz
1 'x, y, z'
2 'y, -x, -z'
3 '-x, -y, z'
4 '-y, x, -z'
5 'x+1/2, -y+1/2, -z+1/2'
6 '-x+1/2, y+1/2, -z+1/2'
7 '-y+1/2, -x+1/2, z+1/2'
8 'y+1/2, x+1/2, z+1/2'

_cell_length_a                   13.9144(2)
_cell_length_b                   13.9144(2)
_cell_length_c                   17.8688(3)
_cell_angle_alpha                90.00
_cell_angle_beta                 90.00
_cell_angle_gamma                90.00
_cell_volume                     3459.59(9)
_cell_formula_units_Z            2
_cell_measurement_reflns_used    5077
_cell_measurement_temperature    120(2)
_cell_measurement_theta_min      4.48
_cell_measurement_theta_max      73.67
_exptl_absorpt_coefficient_mu    11.110
_exptl_absorpt_correction_T_min  0.555
_exptl_absorpt_correction_T_max  1.000
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   
; 
CrysAlisPro, Agilent Technologies,
Version 1.171.36.24 (release 03-12-2012 CrysAlis171 .NET)
Empirical absorption correction using spherical harmonics,
 implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_crystal_colour            colourless
_exptl_crystal_density_diffrn    1.830
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       'cubic prism'
_exptl_crystal_F_000             1904
_exptl_crystal_size_max          0.40
_exptl_crystal_size_mid          0.30
_exptl_crystal_size_min          0.30
_exptl_special_details           
;
 ? 
;
_diffrn_reflns_av_R_equivalents  0.0282
_diffrn_reflns_av_unetI/netI     0.0365
_diffrn_reflns_limit_h_max       14
_diffrn_reflns_limit_h_min       -17
_diffrn_reflns_limit_k_max       14
_diffrn_reflns_limit_k_min       -16
_diffrn_reflns_limit_l_max       20
_diffrn_reflns_limit_l_min       -21
_diffrn_reflns_number            6825
_diffrn_reflns_theta_full        72.00
_diffrn_reflns_theta_max         73.42
_diffrn_reflns_theta_min         4.03
_diffrn_ambient_temperature      120(2)
_diffrn_detector_area_resol_mean 5.3095
_diffrn_measured_fraction_theta_full 0.988
_diffrn_measured_fraction_theta_max 0.979
_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                3125
_reflns_number_total             3221
_reflns_threshold_expression     >2sigma(I)
_computing_cell_refinement       'CrysAlisPro, Agilent Technologies'
_computing_data_collection       '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         1.174
_refine_diff_density_min         -0.927
_refine_diff_density_rms         0.102
_refine_ls_abs_structure_details 'Flack H D (1983), Acta Cryst. A39, 876-881'
_refine_ls_abs_structure_Flack   0.170(10)
_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     241
_refine_ls_number_reflns         3221
_refine_ls_number_restraints     0
_refine_ls_R_factor_all          0.0370
_refine_ls_R_factor_gt           0.0358
_refine_ls_restrained_S_all      1.051
_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)+(0.0579P)²+2.2352P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0906
_refine_ls_wR_factor_ref         0.0919
_refine_special_details          
;
 Refinement of F² against ALL reflections.  The weighted R-factor wR and 
 goodness of fit S are based on F², conventional R-factors R are based 
 on F, with F set to zero for negative F². The threshold expression of 
 F² > 2sigma(F²) is used only for calculating R-factors(gt) etc. and is 
 not relevant to the choice of reflections for refinement.  R-factors based 
 on F² are statistically about twice as large as those based on F, and R- 
 factors based on ALL data will be even larger. 

 The crystal was refined as a racemic twin.

 The asymmetric unit contains one-quarter of a formula unit, with a quarter
 of the cyclic tetramer encircling the -4 site 1/2, 1/2, 1/2 and two 
 complete ClO₄⁻ half-anions spanning C₂ axes 1/2, 0, z and 1/2, 1/2, z.
 No restraints were applied to the model in the final least squares cycles.
 All fully occupied non-H atoms plus the Cl half-atoms were refined 
 anisotropically, and H atoms were placed in calculated positions and 
 refined using a riding model.
;
_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. Others
 Fixed Sof: O23(0.5) O24(0.5) O25(0.5) O26(0.5) Cl27(0.5) O28(0.5) O29(0.5)
 O30(0.5) O31(0.5)
3.a Aromatic/amide H refined with riding coordinates:
 C5(H5), C11(H11), C18(H18)
3.b Idealised Me refined as rotating group:
 C13(H13A,H13B,H13C), C14(H14A,H14B,H14C), 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
Ag1 Ag 0.68675(2) 0.22373(3) 0.46100(2) 0.02727(12) Uani 1 1 d . . .
N2 N 0.4009(2) 0.1932(2) 0.34602(18) 0.0126(7) Uani 1 1 d . . .
C3 C 0.4920(3) 0.2082(3) 0.3658(2) 0.0125(8) Uani 1 1 d . . .
N4 N 0.5217(3) 0.2488(3) 0.4299(2) 0.0218(8) Uani 1 1 d . . .
C5 C 0.4517(3) 0.2779(4) 0.4747(2) 0.0247(10) Uani 1 1 d . . .
H5 H 0.4696 0.3121 0.5186 0.030 Uiso 1 1 calc R . .
N6 N 0.3586(3) 0.2633(3) 0.4634(2) 0.0220(8) Uani 1 1 d . . .
C7 C 0.3376(3) 0.2195(3) 0.3986(2) 0.0130(8) Uani 1 1 d . . .
N8 N 0.5649(2) 0.1769(3) 0.31799(18) 0.0114(7) Uani 1 1 d . . .
N9 N 0.6579(2) 0.1781(3) 0.3438(2) 0.0146(7) Uani 1 1 d . . .
C10 C 0.7115(3) 0.1420(3) 0.2903(2) 0.0145(8) Uani 1 1 d . . .
C11 C 0.6546(3) 0.1182(3) 0.2269(3) 0.0154(8) Uani 1 1 d . . .
H11 H 0.6766 0.0922 0.1809 0.018 Uiso 1 1 calc R . .
C12 C 0.5615(3) 0.1402(3) 0.2456(2) 0.0116(8) Uani 1 1 d . . .
C13 C 0.8172(3) 0.1306(3) 0.3005(3) 0.0225(9) Uani 1 1 d . . .
H13A H 0.8320 0.0632 0.3116 0.034 Uiso 1 1 calc R . .
H13B H 0.8387 0.1711 0.3421 0.034 Uiso 1 1 calc R . .
H13C H 0.8504 0.1500 0.2546 0.034 Uiso 1 1 calc R . .
C14 C 0.4743(3) 0.1297(3) 0.1996(2) 0.0194(9) Uani 1 1 d . . .
H14A H 0.4924 0.1126 0.1483 0.029 Uiso 1 1 calc R . .
H14B H 0.4387 0.1904 0.1992 0.029 Uiso 1 1 calc R . .
H14C H 0.4336 0.0789 0.2206 0.029 Uiso 1 1 calc R . .
N15 N 0.2410(2) 0.1999(2) 0.38686(19) 0.0129(7) Uani 1 1 d . . .
N16 N 0.1766(3) 0.2236(3) 0.44233(18) 0.0163(7) Uani 1 1 d . . .
C17 C 0.0923(3) 0.1895(4) 0.4212(2) 0.0189(9) Uani 1 1 d . . .
C18 C 0.1004(3) 0.1432(3) 0.3502(2) 0.0170(8) Uani 1 1 d . . .
H18 H 0.0502 0.1133 0.3227 0.020 Uiso 1 1 calc R . .
C19 C 0.1944(3) 0.1502(3) 0.3298(2) 0.0128(8) Uani 1 1 d . . .
C20 C 0.0056(3) 0.2014(4) 0.4698(3) 0.0304(11) Uani 1 1 d . . .
H20A H -0.0401 0.2450 0.4454 0.046 Uiso 1 1 calc R . .
H20B H 0.0249 0.2284 0.5181 0.046 Uiso 1 1 calc R . .
H20C H -0.0249 0.1387 0.4776 0.046 Uiso 1 1 calc R . .
C21 C 0.2405(3) 0.1145(3) 0.2603(2) 0.0176(8) Uani 1 1 d . . .
H21A H 0.1914 0.0873 0.2272 0.026 Uiso 1 1 calc R . .
H21B H 0.2877 0.0647 0.2730 0.026 Uiso 1 1 calc R . .
H21C H 0.2730 0.1678 0.2349 0.026 Uiso 1 1 calc R . .
Cl22 Cl 0.5000 0.0000 0.49844(10) 0.0344(4) Uani 1 2 d S . .
O23 O 0.4103(8) 0.0450(8) 0.4723(6) 0.057(3) Uiso 0.50 1 d P . .
O24 O 0.5518(6) 0.0801(5) 0.5402(5) 0.0303(17) Uiso 0.50 1 d P . .
O25 O 0.5616(8) -0.0130(8) 0.4367(6) 0.059(3) Uiso 0.50 1 d P . .
O26 O 0.4878(7) -0.0775(6) 0.5452(5) 0.0312(17) Uiso 0.50 1 d P . .
Cl27 Cl 0.492(2) 0.492(2) 0.35097(11) 0.027(3) Uani 0.50 1 d P . .
O28 O 0.5186(8) 0.4060(8) 0.3137(6) 0.035(3) Uiso 0.50 1 d P A -1
O29 O 0.5505(8) 0.5065(10) 0.4135(6) 0.066(3) Uiso 0.50 1 d P A -1
O30 O 0.4893(10) 0.5723(9) 0.3000(7) 0.051(3) Uiso 0.50 1 d P A -1
O31 O 0.3959(7) 0.4755(7) 0.3785(5) 0.046(2) Uiso 0.50 1 d P A -1


_geom_special_details            
;
 All esds (except the esd in the dihedral angle between two l.s. planes) 
 are estimated using the full covariance matrix.  The cell esds are taken 
 into account individually in the estimation of esds in distances, angles 
 and torsion angles; correlations between esds in cell parameters are only 
 used when they are defined by crystal symmetry.  An approximate (isotropic) 
 treatment of cell esds is used for estimating esds involving l.s. planes. 
;
loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
_geom_bond_publ_flag
Ag1 N4 2.388(4) . ?
Ag1 N6 2.414(4) 4_656 ?
Ag1 N9 2.225(4) . ?
Ag1 N16 2.230(3) 4_656 ?
Ag1 Ag1 6.7083(5) 4_656 ?
N2 C3 1.333(5) . ?
N2 C7 1.338(5) . ?
C3 N4 1.343(5) . ?
C3 N8 1.396(5) . ?
N4 C5 1.324(6) . ?
C5 H5 0.9500 . ?
C5 N6 1.328(6) . ?
N6 C7 1.340(5) . ?
C7 N15 1.387(5) . ?
N8 N9 1.373(5) . ?
N8 C12 1.392(5) . ?
N9 C10 1.312(6) . ?
C10 C11 1.421(6) . ?
C10 C13 1.491(6) . ?
C11 H11 0.9500 . ?
C11 C12 1.372(6) . ?
C12 C14 1.473(6) . ?
C13 H13A 0.9800 . ?
C13 H13B 0.9800 . ?
C13 H13C 0.9800 . ?
C14 H14A 0.9800 . ?
C14 H14B 0.9800 . ?
C14 H14C 0.9800 . ?
N15 N16 1.377(5) . ?
N15 C19 1.393(5) . ?
N16 C17 1.321(6) . ?
C17 C18 1.427(6) . ?
C17 C20 1.495(6) . ?
C18 H18 0.9500 . ?
C18 C19 1.361(6) . ?
C19 C21 1.484(6) . ?
C20 H20A 0.9800 . ?
C20 H20B 0.9800 . ?
C20 H20C 0.9800 . ?
C21 H21A 0.9800 . ?
C21 H21B 0.9800 . ?
C21 H21C 0.9800 . ?
Cl22 O23 1.473(11) . ?
Cl22 O24 1.522(8) . ?
Cl22 O25 1.409(11) . ?
Cl22 O26 1.374(8) . ?
Cl27 O28 1.42(3) . ?
Cl27 O29 1.401(19) . ?
Cl27 O30 1.44(3) . ?
Cl27 O31 1.44(3) . ?

loop_
_geom_angle_atom_site_label_1
_geom_angle_atom_site_label_2
_geom_angle_atom_site_label_3
_geom_angle
_geom_angle_site_symmetry_1
_geom_angle_site_symmetry_3
_geom_angle_publ_flag
N4 Ag1 N6 107.06(13) . 4_656 ?
N9 Ag1 N4 69.48(13) . . ?
N9 Ag1 N6 143.17(13) . 4_656 ?
N9 Ag1 N16 138.27(13) . 4_656 ?
N16 Ag1 N4 139.56(13) 4_656 . ?
N16 Ag1 N6 68.53(13) 4_656 4_656 ?
C3 N2 C7 113.4(3) . . ?
N2 C3 N4 125.8(4) . . ?
N2 C3 N8 118.7(3) . . ?
N4 C3 N8 115.5(4) . . ?
C3 N4 Ag1 115.6(3) . . ?
C5 N4 Ag1 127.7(3) . . ?
C5 N4 C3 114.7(4) . . ?
N4 C5 H5 117.3 . . ?
N4 C5 N6 125.4(4) . . ?
N6 C5 H5 117.3 . . ?
C5 N6 Ag1 129.0(3) . 2_566 ?
C5 N6 C7 114.4(4) . . ?
C7 N6 Ag1 116.4(3) . 2_566 ?
N2 C7 N6 126.0(4) . . ?
N2 C7 N15 118.5(3) . . ?
N6 C7 N15 115.5(4) . . ?
N9 N8 C3 118.4(3) . . ?
N9 N8 C12 110.4(3) . . ?
C12 N8 C3 131.2(3) . . ?
N8 N9 Ag1 119.3(3) . . ?
C10 N9 Ag1 133.8(3) . . ?
C10 N9 N8 106.6(3) . . ?
N9 C10 C11 110.7(4) . . ?
N9 C10 C13 120.8(4) . . ?
C11 C10 C13 128.5(4) . . ?
C10 C11 H11 126.9 . . ?
C12 C11 C10 106.3(4) . . ?
C12 C11 H11 126.9 . . ?
N8 C12 C14 125.7(4) . . ?
C11 C12 N8 106.0(4) . . ?
C11 C12 C14 128.3(4) . . ?
C10 C13 H13A 109.5 . . ?
C10 C13 H13B 109.5 . . ?
C10 C13 H13C 109.5 . . ?
H13A C13 H13B 109.5 . . ?
H13A C13 H13C 109.5 . . ?
H13B C13 H13C 109.5 . . ?
C12 C14 H14A 109.5 . . ?
C12 C14 H14B 109.5 . . ?
C12 C14 H14C 109.5 . . ?
H14A C14 H14B 109.5 . . ?
H14A C14 H14C 109.5 . . ?
H14B C14 H14C 109.5 . . ?
C7 N15 C19 131.3(3) . . ?
N16 N15 C7 118.4(3) . . ?
N16 N15 C19 110.0(3) . . ?
N15 N16 Ag1 120.0(3) . 2_566 ?
C17 N16 Ag1 133.2(3) . 2_566 ?
C17 N16 N15 106.7(3) . . ?
N16 C17 C18 110.3(4) . . ?
N16 C17 C20 120.7(4) . . ?
C18 C17 C20 129.1(4) . . ?
C17 C18 H18 126.8 . . ?
C19 C18 C17 106.4(4) . . ?
C19 C18 H18 126.8 . . ?
N15 C19 C21 125.3(4) . . ?
C18 C19 N15 106.7(4) . . ?
C18 C19 C21 128.0(4) . . ?
C17 C20 H20A 109.5 . . ?
C17 C20 H20B 109.5 . . ?
C17 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 . . ?
O23 Cl22 O24 104.2(5) . . ?
O25 Cl22 O23 108.8(8) . . ?
O25 Cl22 O24 100.9(6) . . ?
O26 Cl22 O23 115.0(6) . . ?
O26 Cl22 O24 109.6(4) . . ?
O26 Cl22 O25 116.7(6) . . ?
O28 Cl27 O30 111.2(9) . . ?
O28 Cl27 O31 105.6(16) . . ?
O29 Cl27 O28 110(2) . . ?
O29 Cl27 O30 114.0(18) . . ?
O29 Cl27 O31 107.0(9) . . ?
O31 Cl27 O30 109(2) . . ?

_exptl_crystal_recrystallization_method 
'Re-crystallisation from solvent: nitromethane-diethyl ether'
####################################################################### 
# 
# 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_sf26-3
_database_code_depnum_ccdc_archive 'CCDC 1957581'
loop_
_audit_author_name
_audit_author_address
'Malcolm Halcrow' 'University of Leeds'
_audit_update_record             
;
2019-11-03 deposited with the CCDC.	2019-11-05 downloaded from the CCDC.
;
_audit_creation_date             2019-07-09
_audit_creation_method           
;
  Olex2 1.2
  (compiled Apr 23 2013 17:54:37, GUI svn.r4466)
;
_chemical_name_common            ?
_chemical_name_systematic        
'Tetrakis-[2,4-di(4,5,6,7-tetrahydroindazol-2-yl)-6H-1,3,5-triazine]-tetrasilver(I) tetraperchlorate nitromethane solvate'
_chemical_formula_moiety         'C68 H76 Ag4 N28, 4(Cl O4), C H3 N O2'
_chemical_formula_sum            'C69 H79 Ag4 Cl4 N29 O18'
_chemical_formula_weight         2175.89
_chemical_melting_point          ?
loop_
_atom_type_symbol
_atom_type_description
_atom_type_scat_dispersion_real
_atom_type_scat_dispersion_imag
_atom_type_scat_source
C C 0.0181 0.0091 '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'
Ag Ag 0.1306 4.2820 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Cl Cl 0.3639 0.7018 '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'

_space_group_crystal_system      monoclinic
_space_group_IT_number           15
_space_group_name_H-M_alt        'C 1 2/c 1'
_space_group_name_Hall           '-C 2yc'
loop_
_space_group_symop_id
_space_group_symop_operation_xyz
1 'x, y, z'
2 '-x, y, -z+1/2'
3 'x+1/2, y+1/2, z'
4 '-x+1/2, y+1/2, -z+1/2'
5 '-x, -y, -z'
6 'x, -y, z-1/2'
7 '-x+1/2, -y+1/2, -z'
8 'x+1/2, -y+1/2, z-1/2'

_cell_length_a                   20.7165(11)
_cell_length_b                   33.8226(13)
_cell_length_c                   15.6449(6)
_cell_angle_alpha                90.00
_cell_angle_beta                 131.404(3)
_cell_angle_gamma                90.00
_cell_volume                     8222.3(6)
_cell_formula_units_Z            4
_cell_measurement_reflns_used    3162
_cell_measurement_temperature    120(2)
_cell_measurement_theta_min      4.83
_cell_measurement_theta_max      73.40
_exptl_absorpt_coefficient_mu    9.462
_exptl_absorpt_correction_T_min  0.714
_exptl_absorpt_correction_T_max  1.000
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   
; 
CrysAlisPro, Agilent Technologies,
Version 1.171.36.24 (release 03-12-2012 CrysAlis171 .NET)
Empirical absorption correction using spherical harmonics,
 implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_crystal_colour            colourless
_exptl_crystal_density_diffrn    1.758
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       needle
_exptl_crystal_F_000             4384
_exptl_crystal_size_max          0.30
_exptl_crystal_size_mid          0.10
_exptl_crystal_size_min          0.05
_exptl_special_details           
;
 ? 
;
_diffrn_reflns_av_R_equivalents  0.0554
_diffrn_reflns_av_unetI/netI     0.0764
_diffrn_reflns_limit_h_max       24
_diffrn_reflns_limit_h_min       -25
_diffrn_reflns_limit_k_max       41
_diffrn_reflns_limit_k_min       -29
_diffrn_reflns_limit_l_max       14
_diffrn_reflns_limit_l_min       -19
_diffrn_reflns_number            10874
_diffrn_reflns_theta_full        72.00
_diffrn_reflns_theta_max         73.85
_diffrn_reflns_theta_min         4.59
_diffrn_ambient_temperature      120(2)
_diffrn_detector_area_resol_mean 5.3095
_diffrn_measured_fraction_theta_full 0.841
_diffrn_measured_fraction_theta_max 0.824
_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                4861
_reflns_number_total             6881
_reflns_threshold_expression     >2sigma(I)
_computing_cell_refinement       'CrysAlisPro, Agilent Technologies'
_computing_data_collection       '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         1.288
_refine_diff_density_min         -0.883
_refine_diff_density_rms         0.115
_refine_ls_extinction_coef       ?
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.062
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     580
_refine_ls_number_reflns         6881
_refine_ls_number_restraints     26
_refine_ls_R_factor_all          0.0964
_refine_ls_R_factor_gt           0.0635
_refine_ls_restrained_S_all      1.062
_refine_ls_shift/su_max          0.002
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details     
'calc w=1/[σ²(Fo²)+(0.0684P)²+43.6977P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1500
_refine_ls_wR_factor_ref         0.1682
_refine_special_details          
;
 Refinement of F² against ALL reflections.  The weighted R-factor wR and 
 goodness of fit S are based on F², conventional R-factors R are based 
 on F, with F set to zero for negative F². The threshold expression of 
 F² > 2sigma(F²) is used only for calculating R-factors(gt) etc. and is 
 not relevant to the choice of reflections for refinement.  R-factors based 
 on F² are statistically about twice as large as those based on F, and R- 
 factors based on ALL data will be even larger. 

 The structure was originally solved in I2/a, then transformed to the 
 standard space group setting C2/c using PLATON.

 The asymmetric unit contains half a formula unit, that is: half a tetrameric
 complex molecule surrounding the crystallographic C₂ axis 1/2, y, 3/4;
 four ClO₄⁻ half-anions, either ordered or disordered about C₂ axes;
 and one nitromethane half-molecule, also spanning a C₂ axis. One
 half-anion is further disordered over two orientations, whose occupancy ratio
 refined to 0.33:0.17. The disordered half-anion was refined using the fixed 
 restraints Cl---O = 1.43(2) and O...O = 2.34(2) Å, while the solvent half-
 molecule also required the following fixed restraints to achieve a sensible
 geometry: C---N = 1.45(2), N---O = 1.22(2), O...O = 2.09(2) and C...O = 
 2.30(2) Å. 

 All crystallographically ordered non-H atoms, plus disordered half-occupied 
 Cl atoms, were refined anisotropically and H atoms were placed in calculated 
 positions and refined using a riding model. The highest residual Fourier peak
 of +1.3 e.Å⁻³ lies on the C₂ axis within the disordered half-anion. 
;
_olex2_refinement_description    
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups, All C(H,H) groups
 At 1.5 times of:
  All C(H,H,H) groups
2. Restrained distances
 Cl5A-O57A = Cl5A-O58A = Cl5A-O59A = Cl5A-O60A
 1.43 with sigma of 0.02
 Cl5B-O57B = Cl5B-O58B = Cl5B-O59B = Cl5B-O60B
 1.43 with sigma of 0.02
 O57A-O58A = O57A-O59A = O57A-O60A = O58A-O59A = O58A-O60A = O59A-O60A
 2.34 with sigma of 0.02
 O57B-O58B = O57B-O59B = O57B-O60B = O58B-O59B = O58B-O60B = O59B-O60B
 2.34 with sigma of 0.02
 C69-N70
 1.45 with sigma of 0.02
 N70-O71 = N70-O72
 1.22 with sigma of 0.02
 O71-O72
 2.09 with sigma of 0.02
 C69-O71 = C69-O72
 2.34 with sigma of 0.02
3. Others
 Fixed Sof: Cl51(0.5) O52(0.5) O53(0.5) O54(0.5) O55(0.5) Cl5A(0.33)
 O57A(0.33) O58A(0.33) O59A(0.33) O60A(0.33) Cl5B(0.17) O57B(0.17) O58B(0.17)
 O59B(0.17) O60B(0.17) Cl61(0.5) O62(0.5) O63(0.5) O64(0.5) O65(0.5) C69(0.5)
 H69A(0.5) H69B(0.5) H69C(0.5) N70(0.5) O71(0.5) O72(0.5)
4.a Secondary CH2 refined with riding coordinates:
 C12(H12A,H12B), C13(H13A,H13B), C14(H14A,H14B), C15(H15A,H15B), C21(H21A,
 H21B), C22(H22A,H22B), C23(H23A,H23B), C24(H24A,H24B), C36(H36A,H36B),
 C37(H37A,H37B), C38(H38A,H38B), C39(H39A,H39B), C45(H45A,H45B), C46(H46A,H46B),
  C47(H47A,H47B), C48(H48A,H48B)
4.b Me refined with riding coordinates:
 C69(H69A,H69B,H69C)
4.c Aromatic/amide H refined with riding coordinates:
 C6(H6), C17(H17), C26(H26), C30(H30), C41(H41), C50(H50)
;
_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
Ag1 Ag 0.36816(5) 0.661058(16) 0.34709(6) 0.04427(19) Uani 1 1 d . . .
Ag2 Ag 0.75245(5) 0.592135(16) 0.85173(6) 0.0466(2) Uani 1 1 d . . .
N3 N 0.5360(4) 0.55096(15) 0.4917(5) 0.0241(12) Uani 1 1 d . . .
C4 C 0.4810(5) 0.58090(19) 0.4393(6) 0.0262(15) Uani 1 1 d . . .
N5 N 0.4791(4) 0.61289(16) 0.4874(6) 0.0311(14) Uani 1 1 d . . .
C6 C 0.5456(5) 0.61564(19) 0.5982(7) 0.0321(17) Uani 1 1 d . . .
H6 H 0.5475 0.6380 0.6366 0.038 Uiso 1 1 calc R B .
N7 N 0.6099(4) 0.58991(16) 0.6605(5) 0.0286(13) Uani 1 1 d . . .
C8 C 0.5990(5) 0.55772(18) 0.6032(6) 0.0248(14) Uani 1 1 d . . .
N9 N 0.4171(4) 0.57747(16) 0.3213(5) 0.0260(12) Uani 1 1 d . B .
N10 N 0.3600(4) 0.60778(16) 0.2576(5) 0.0273(13) Uani 1 1 d . B .
C11 C 0.3145(5) 0.5965(2) 0.1522(7) 0.0308(16) Uani 1 1 d . . .
C12 C 0.2475(5) 0.6215(2) 0.0511(7) 0.0356(18) Uani 1 1 d . . .
H12A H 0.2756 0.6431 0.0432 0.043 Uiso 1 1 calc R . .
H12B H 0.2099 0.6336 0.0620 0.043 Uiso 1 1 calc R . .
C13 C 0.1942(6) 0.5965(3) -0.0553(8) 0.043(2) Uani 1 1 d . . .
H13A H 0.1592 0.6141 -0.1227 0.052 Uiso 1 1 calc R B .
H13B H 0.1542 0.5802 -0.0562 0.052 Uiso 1 1 calc R . .
C14 C 0.2476(6) 0.5698(3) -0.0648(7) 0.044(2) Uani 1 1 d . . .
H14A H 0.2888 0.5859 -0.0622 0.053 Uiso 1 1 calc R . .
H14B H 0.2095 0.5558 -0.1389 0.053 Uiso 1 1 calc R . .
C15 C 0.2975(5) 0.5393(2) 0.0324(7) 0.0382(18) Uani 1 1 d . . .
H15A H 0.2573 0.5187 0.0182 0.046 Uiso 1 1 calc R B .
H15B H 0.3413 0.5262 0.0345 0.046 Uiso 1 1 calc R . .
C16 C 0.3403(5) 0.5585(2) 0.1437(7) 0.0288(15) Uani 1 1 d . . .
C17 C 0.4065(5) 0.5477(2) 0.2536(7) 0.0289(16) Uani 1 1 d . . .
H17 H 0.4392 0.5241 0.2786 0.035 Uiso 1 1 calc R B .
N18 N 0.6604(4) 0.52811(16) 0.6620(5) 0.0250(12) Uani 1 1 d . B .
N19 N 0.7345(4) 0.53352(16) 0.7740(5) 0.0285(13) Uani 1 1 d . . .
C20 C 0.7807(5) 0.5015(2) 0.7978(7) 0.0309(16) Uani 1 1 d . . .
C21 C 0.8677(5) 0.4947(2) 0.9117(7) 0.0388(18) Uani 1 1 d . . .
H21A H 0.8620 0.4864 0.9672 0.047 Uiso 1 1 calc R B .
H21B H 0.9016 0.5194 0.9396 0.047 Uiso 1 1 calc R . .
C22 C 0.9138(6) 0.4623(3) 0.9009(8) 0.044(2) Uani 1 1 d . . .
H22A H 0.9330 0.4733 0.8623 0.053 Uiso 1 1 calc R . .
H22B H 0.9655 0.4536 0.9780 0.053 Uiso 1 1 calc R . .
C23 C 0.8563(5) 0.4267(2) 0.8340(8) 0.043(2) Uani 1 1 d . . .
H23A H 0.8355 0.4160 0.8710 0.051 Uiso 1 1 calc R B .
H23B H 0.8903 0.4057 0.8352 0.051 Uiso 1 1 calc R . .
C24 C 0.7781(5) 0.4376(2) 0.7088(7) 0.0342(17) Uani 1 1 d . . .
H24A H 0.7970 0.4408 0.6653 0.041 Uiso 1 1 calc R . .
H24B H 0.7349 0.4161 0.6730 0.041 Uiso 1 1 calc R . .
C25 C 0.7384(4) 0.47541(19) 0.7052(6) 0.0252(15) Uani 1 1 d . . .
C26 C 0.6623(5) 0.49293(18) 0.6204(6) 0.0239(14) Uani 1 1 d . B .
H26 H 0.6184 0.4827 0.5459 0.029 Uiso 1 1 calc R . .
N27 N 0.2093(4) 0.69739(17) 0.4445(6) 0.0335(14) Uani 1 1 d . . .
C28 C 0.2569(5) 0.6909(2) 0.4165(7) 0.0319(16) Uani 1 1 d . . .
N29 N 0.3078(5) 0.65931(17) 0.4468(6) 0.0382(16) Uani 1 1 d . . .
C30 C 0.3070(6) 0.6336(2) 0.5102(7) 0.0394(19) Uani 1 1 d . . .
H30 H 0.3454 0.6119 0.5393 0.047 Uiso 1 1 calc R B .
N31 N 0.2579(4) 0.63506(18) 0.5374(6) 0.0361(15) Uani 1 1 d . . .
C32 C 0.2096(5) 0.6678(2) 0.4997(7) 0.0336(17) Uani 1 1 d . . .
N33 N 0.2540(4) 0.71937(16) 0.3517(6) 0.0311(14) Uani 1 1 d . B .
N34 N 0.2965(4) 0.71542(17) 0.3126(6) 0.0338(14) Uani 1 1 d . B .
C35 C 0.2718(5) 0.74586(19) 0.2440(7) 0.0326(17) Uani 1 1 d . . .
C36 C 0.3020(6) 0.7539(2) 0.1820(7) 0.0393(19) Uani 1 1 d . . .
H36A H 0.3026 0.7292 0.1487 0.047 Uiso 1 1 calc R . .
H36B H 0.3612 0.7648 0.2351 0.047 Uiso 1 1 calc R . .
C37 C 0.2399(7) 0.7842(3) 0.0865(9) 0.052(2) Uani 1 1 d . . .
H37A H 0.2664 0.7943 0.0564 0.062 Uiso 1 1 calc R B .
H37B H 0.1861 0.7704 0.0234 0.062 Uiso 1 1 calc R . .
C38 C 0.2179(7) 0.8183(3) 0.1230(9) 0.052(2) Uani 1 1 d . . .
H38A H 0.1815 0.8369 0.0585 0.062 Uiso 1 1 calc R . .
H38B H 0.2716 0.8323 0.1857 0.062 Uiso 1 1 calc R . .
C39 C 0.1711(6) 0.8064(2) 0.1627(8) 0.0375(18) Uani 1 1 d . . .
H39A H 0.1101 0.8008 0.0958 0.045 Uiso 1 1 calc R B .
H39B H 0.1729 0.8285 0.2058 0.045 Uiso 1 1 calc R . .
C40 C 0.2126(5) 0.76979(19) 0.2383(7) 0.0292(16) Uani 1 1 d . . .
C41 C 0.2020(5) 0.75238(19) 0.3061(7) 0.0311(16) Uani 1 1 d . . .
H41 H 0.1658 0.7612 0.3196 0.037 Uiso 1 1 calc R B .
N42 N 0.1550(4) 0.67161(17) 0.5207(6) 0.0322(14) Uani 1 1 d . B .
N43 N 0.1483(4) 0.64168(17) 0.5744(6) 0.0349(14) Uani 1 1 d . . .
C44 C 0.0858(5) 0.6543(2) 0.5715(6) 0.0326(16) Uani 1 1 d . . .
C45 C 0.0534(6) 0.6309(2) 0.6178(8) 0.043(2) Uani 1 1 d . . .
H45A H 0.1027 0.6207 0.6943 0.051 Uiso 1 1 calc R B .
H45B H 0.0194 0.6081 0.5673 0.051 Uiso 1 1 calc R . .
C46 C -0.0021(7) 0.6569(3) 0.6255(10) 0.057(3) Uani 1 1 d . . .
H46A H -0.0364 0.6398 0.6339 0.069 Uiso 1 1 calc R . .
H46B H 0.0357 0.6735 0.6946 0.069 Uiso 1 1 calc R . .
C47 C -0.0620(7) 0.6831(3) 0.5238(11) 0.065(3) Uani 1 1 d . . .
H47A H -0.0978 0.6981 0.5335 0.077 Uiso 1 1 calc R B .
H47B H -0.1010 0.6663 0.4553 0.077 Uiso 1 1 calc R . .
C48 C -0.0178(6) 0.7123(3) 0.5032(9) 0.050(2) Uani 1 1 d . . .
H48A H -0.0599 0.7231 0.4249 0.060 Uiso 1 1 calc R . .
H48B H 0.0061 0.7346 0.5576 0.060 Uiso 1 1 calc R . .
C49 C 0.0537(5) 0.6912(2) 0.5189(7) 0.0370(17) Uani 1 1 d . . .
C50 C 0.0974(5) 0.7015(2) 0.4852(7) 0.0358(18) Uani 1 1 d . B .
H50 H 0.0896 0.7247 0.4451 0.043 Uiso 1 1 calc R . .
Cl51 Cl 0.4738(2) 0.55355(9) 0.7203(3) 0.0315(10) Uani 0.50 1 d P A -1
O52 O 0.3819(8) 0.5494(3) 0.6529(11) 0.045(3) Uiso 0.50 1 d P A -1
O53 O 0.4980(7) 0.5360(3) 0.6610(10) 0.030(2) Uiso 0.50 1 d P A -1
O54 O 0.5209(9) 0.5342(4) 0.8288(12) 0.046(3) Uiso 0.50 1 d P A -1
O55 O 0.4897(11) 0.5948(2) 0.7335(13) 0.036(2) Uiso 0.50 1 d P A -1
Cl5A Cl 0.5104(5) 0.66895(17) 0.2845(5) 0.0465(14) Uiso 0.33 1 d PD B -1
O57A O 0.4733(18) 0.6924(7) 0.316(3) 0.107(11) Uiso 0.33 1 d PD B -1
O58A O 0.5441(9) 0.6337(3) 0.3482(12) 0.031(3) Uiso 0.33 1 d PD B -1
O59A O 0.5747(11) 0.6902(5) 0.2923(18) 0.046(5) Uiso 0.33 1 d PD B -1
O60A O 0.4452(17) 0.6568(9) 0.1652(14) 0.164(19) Uiso 0.33 1 d PD B -1
Cl5B Cl 0.5035(11) 0.6972(5) 0.2796(13) 0.078(5) Uiso 0.17 1 d PD B -2
O57B O 0.4984(17) 0.6945(7) 0.367(2) 0.025(6) Uiso 0.17 1 d PD B -2
O58B O 0.518(3) 0.7385(6) 0.271(4) 0.104(18) Uiso 0.17 1 d PD B -2
O59B O 0.5730(17) 0.6737(10) 0.310(3) 0.043(10) Uiso 0.17 1 d PD B -2
O60B O 0.4227(15) 0.6855(10) 0.1726(19) 0.037(9) Uiso 0.17 1 d PD B -2
Cl61 Cl 0.5062(5) 0.70558(10) 0.7766(5) 0.0442(13) Uani 0.50 1 d P C -1
O62 O 0.4208(16) 0.6891(7) 0.693(2) 0.089(8) Uiso 0.50 1 d P C -1
O63 O 0.5265(12) 0.7065(5) 0.8828(15) 0.082(5) Uiso 0.50 1 d P C -1
O64 O 0.5656(9) 0.6822(4) 0.7749(12) 0.031(3) Uiso 0.50 1 d P C -1
O65 O 0.5138(11) 0.7460(3) 0.758(2) 0.055(3) Uiso 0.50 1 d P C -1
Cl66 Cl 0.0000 0.52630(8) 0.7500 0.0460(7) Uani 1 2 d S . .
O67 O 0.0751(5) 0.5016(2) 0.8249(6) 0.0606(18) Uani 1 1 d . . .
O68 O 0.0102(5) 0.5502(2) 0.6846(6) 0.0640(19) Uani 1 1 d . . .
C69 C 0.0349(15) 0.5836(5) 0.315(2) 0.075(6) Uiso 0.50 1 d PD D -1
H69A H 0.0375 0.5827 0.3800 0.112 Uiso 0.50 1 calc PR D -1
H69B H 0.0929 0.5805 0.3424 0.112 Uiso 0.50 1 calc PR D -1
H69C H -0.0019 0.5621 0.2620 0.112 Uiso 0.50 1 calc PR D -1
N70 N -0.0007(18) 0.6215(4) 0.257(3) 0.068(4) Uiso 0.50 1 d PD D -1
O71 O -0.0696(11) 0.6332(5) 0.2267(18) 0.082(6) Uiso 0.50 1 d PD D -1
O72 O 0.0399(13) 0.6437(5) 0.2450(19) 0.088(6) Uiso 0.50 1 d PD D -1


_geom_special_details            
;
 All esds (except the esd in the dihedral angle between two l.s. planes) 
 are estimated using the full covariance matrix.  The cell esds are taken 
 into account individually in the estimation of esds in distances, angles 
 and torsion angles; correlations between esds in cell parameters are only 
 used when they are defined by crystal symmetry.  An approximate (isotropic) 
 treatment of cell esds is used for estimating esds involving l.s. planes. 
;
loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
_geom_bond_publ_flag
Ag1 Ag2 7.0322(9) 2_656 ?
Ag1 Ag2 6.9287(11) . ?
Ag1 N5 2.466(7) . ?
Ag1 N10 2.219(6) . ?
Ag1 N29 2.566(7) . ?
Ag1 N34 2.195(6) . ?
Ag1 O57A 2.74(2) . ?
Ag1 O57B 2.75(2) . ?
Ag2 N7 2.447(6) . ?
Ag2 N19 2.225(6) . ?
Ag2 N31 2.378(6) 2_656 ?
Ag2 N43 2.287(6) 2_656 ?
N3 C4 1.327(9) . ?
N3 C8 1.336(10) . ?
C4 N5 1.333(9) . ?
C4 N9 1.394(10) . ?
N5 C6 1.323(11) . ?
C6 H6 0.9500 . ?
C6 N7 1.329(10) . ?
N7 C8 1.331(9) . ?
C8 N18 1.385(9) . ?
N9 N10 1.372(8) . ?
N9 C17 1.369(9) . ?
N10 C11 1.302(10) . ?
C11 C12 1.496(11) . ?
C11 C16 1.431(9) . ?
C12 H12A 0.9900 . ?
C12 H12B 0.9900 . ?
C12 C13 1.508(12) . ?
C13 H13A 0.9900 . ?
C13 H13B 0.9900 . ?
C13 C14 1.511(11) . ?
C14 H14A 0.9900 . ?
C14 H14B 0.9900 . ?
C14 C15 1.538(12) . ?
C15 H15A 0.9900 . ?
C15 H15B 0.9900 . ?
C15 C16 1.483(11) . ?
C16 C17 1.360(11) . ?
C17 H17 0.9500 . ?
N18 N19 1.380(9) . ?
N18 C26 1.369(8) . ?
N19 C20 1.325(9) . ?
C20 C21 1.493(12) . ?
C20 C25 1.402(11) . ?
C21 H21A 0.9900 . ?
C21 H21B 0.9900 . ?
C21 C22 1.535(12) . ?
C22 H22A 0.9900 . ?
C22 H22B 0.9900 . ?
C22 C23 1.521(12) . ?
C23 H23A 0.9900 . ?
C23 H23B 0.9900 . ?
C23 C24 1.550(12) . ?
C24 H24A 0.9900 . ?
C24 H24B 0.9900 . ?
C24 C25 1.501(10) . ?
C25 C26 1.352(10) . ?
C26 H26 0.9500 . ?
N27 C28 1.336(9) . ?
N27 C32 1.320(9) . ?
C28 N29 1.346(9) . ?
C28 N33 1.371(9) . ?
N29 C30 1.326(10) . ?
C30 H30 0.9500 . ?
C30 N31 1.338(10) . ?
N31 C32 1.339(9) . ?
C32 N42 1.377(10) . ?
N33 N34 1.370(8) . ?
N33 C41 1.378(9) . ?
N34 C35 1.323(10) . ?
C35 C36 1.486(10) . ?
C35 C40 1.422(9) . ?
C36 H36A 0.9900 . ?
C36 H36B 0.9900 . ?
C36 C37 1.547(12) . ?
C37 H37A 0.9900 . ?
C37 H37B 0.9900 . ?
C37 C38 1.485(12) . ?
C38 H38A 0.9900 . ?
C38 H38B 0.9900 . ?
C38 C39 1.511(11) . ?
C39 H39A 0.9900 . ?
C39 H39B 0.9900 . ?
C39 C40 1.526(10) . ?
C40 C41 1.353(10) . ?
C41 H41 0.9500 . ?
N42 N43 1.380(8) . ?
N42 C50 1.369(9) . ?
N43 C44 1.335(10) . ?
C44 C45 1.498(10) . ?
C44 C49 1.398(11) . ?
C45 H45A 0.9900 . ?
C45 H45B 0.9900 . ?
C45 C46 1.513(13) . ?
C46 H46A 0.9900 . ?
C46 H46B 0.9900 . ?
C46 C47 1.499(15) . ?
C47 H47A 0.9900 . ?
C47 H47B 0.9900 . ?
C47 C48 1.518(12) . ?
C48 H48A 0.9900 . ?
C48 H48B 0.9900 . ?
C48 C49 1.510(11) . ?
C49 C50 1.359(11) . ?
C50 H50 0.9500 . ?
Cl51 O52 1.448(13) . ?
Cl51 O53 1.441(13) . ?
Cl51 O54 1.439(15) . ?
Cl51 O55 1.416(9) . ?
Cl5A O57A 1.404(14) . ?
Cl5A O58A 1.409(12) . ?
Cl5A O59A 1.446(13) . ?
Cl5A O60A 1.464(15) . ?
Cl5B O57B 1.435(16) . ?
Cl5B O58B 1.454(16) . ?
Cl5B O59B 1.421(17) . ?
Cl5B O60B 1.433(17) . ?
Cl61 O62 1.45(3) . ?
Cl61 O63 1.419(19) . ?
Cl61 O64 1.477(14) . ?
Cl61 O65 1.427(12) . ?
Cl66 O67 1.441(7) . ?
Cl66 O68 1.426(7) . ?
C69 H69A 0.9800 . ?
C69 H69B 0.9800 . ?
C69 H69C 0.9800 . ?
C69 N70 1.458(16) . ?
N70 O71 1.236(17) . ?
N70 O72 1.231(16) . ?

loop_
_geom_angle_atom_site_label_1
_geom_angle_atom_site_label_2
_geom_angle_atom_site_label_3
_geom_angle
_geom_angle_site_symmetry_1
_geom_angle_site_symmetry_3
_geom_angle_publ_flag
N5 Ag1 N29 89.18(19) . . ?
N5 Ag1 O57A 91.8(6) . . ?
N5 Ag1 O57B 84.5(5) . . ?
N10 Ag1 N5 70.3(2) . . ?
N10 Ag1 N29 120.1(2) . . ?
N10 Ag1 O57A 86.6(5) . . ?
N10 Ag1 O57B 93.6(5) . . ?
N29 Ag1 O57A 151.8(6) . . ?
N29 Ag1 O57B 141.2(5) . . ?
N34 Ag1 N5 148.5(2) . . ?
N34 Ag1 N10 140.2(2) . . ?
N34 Ag1 N29 69.3(2) . . ?
N34 Ag1 O57A 96.9(4) . . ?
N34 Ag1 O57B 97.9(5) . . ?
N19 Ag2 N7 71.0(2) . . ?
N19 Ag2 N31 151.6(2) . 2_656 ?
N19 Ag2 N43 134.3(2) . 2_656 ?
N31 Ag2 N7 107.0(2) 2_656 . ?
N43 Ag2 N7 126.5(2) 2_656 . ?
N43 Ag2 N31 70.7(2) 2_656 2_656 ?
C4 N3 C8 112.0(6) . . ?
N3 C4 N5 127.2(7) . . ?
N3 C4 N9 115.5(6) . . ?
N5 C4 N9 117.3(6) . . ?
C4 N5 Ag1 113.1(5) . . ?
C6 N5 Ag1 132.0(4) . . ?
C6 N5 C4 113.7(6) . . ?
N5 C6 H6 117.1 . . ?
N5 C6 N7 125.8(6) . . ?
N7 C6 H6 117.1 . . ?
C6 N7 Ag2 133.7(5) . . ?
C6 N7 C8 113.6(6) . . ?
C8 N7 Ag2 112.3(5) . . ?
N3 C8 N18 114.7(6) . . ?
N7 C8 N3 127.1(6) . . ?
N7 C8 N18 118.1(6) . . ?
N10 N9 C4 120.5(5) . . ?
C17 N9 C4 127.7(6) . . ?
C17 N9 N10 111.5(6) . . ?
N9 N10 Ag1 118.6(4) . . ?
C11 N10 Ag1 136.5(5) . . ?
C11 N10 N9 104.9(5) . . ?
N10 C11 C12 124.2(6) . . ?
N10 C11 C16 112.2(7) . . ?
C16 C11 C12 123.5(7) . . ?
C11 C12 H12A 109.7 . . ?
C11 C12 H12B 109.7 . . ?
C11 C12 C13 109.9(6) . . ?
H12A C12 H12B 108.2 . . ?
C13 C12 H12A 109.7 . . ?
C13 C12 H12B 109.7 . . ?
C12 C13 H13A 108.9 . . ?
C12 C13 H13B 108.9 . . ?
C12 C13 C14 113.3(7) . . ?
H13A C13 H13B 107.7 . . ?
C14 C13 H13A 108.9 . . ?
C14 C13 H13B 108.9 . . ?
C13 C14 H14A 109.4 . . ?
C13 C14 H14B 109.4 . . ?
C13 C14 C15 111.2(7) . . ?
H14A C14 H14B 108.0 . . ?
C15 C14 H14A 109.4 . . ?
C15 C14 H14B 109.4 . . ?
C14 C15 H15A 109.5 . . ?
C14 C15 H15B 109.5 . . ?
H15A C15 H15B 108.1 . . ?
C16 C15 C14 110.8(7) . . ?
C16 C15 H15A 109.5 . . ?
C16 C15 H15B 109.5 . . ?
C11 C16 C15 122.2(7) . . ?
C17 C16 C11 104.5(7) . . ?
C17 C16 C15 133.3(6) . . ?
N9 C17 H17 126.5 . . ?
C16 C17 N9 107.0(6) . . ?
C16 C17 H17 126.5 . . ?
N19 N18 C8 120.6(5) . . ?
C26 N18 C8 128.0(6) . . ?
C26 N18 N19 111.1(6) . . ?
N18 N19 Ag2 117.1(4) . . ?
C20 N19 Ag2 138.3(5) . . ?
C20 N19 N18 103.8(6) . . ?
N19 C20 C21 122.6(7) . . ?
N19 C20 C25 112.5(7) . . ?
C25 C20 C21 124.9(7) . . ?
C20 C21 H21A 109.9 . . ?
C20 C21 H21B 109.9 . . ?
C20 C21 C22 109.1(7) . . ?
H21A C21 H21B 108.3 . . ?
C22 C21 H21A 109.9 . . ?
C22 C21 H21B 109.9 . . ?
C21 C22 H22A 109.1 . . ?
C21 C22 H22B 109.1 . . ?
H22A C22 H22B 107.9 . . ?
C23 C22 C21 112.3(7) . . ?
C23 C22 H22A 109.1 . . ?
C23 C22 H22B 109.1 . . ?
C22 C23 H23A 109.3 . . ?
C22 C23 H23B 109.3 . . ?
C22 C23 C24 111.6(7) . . ?
H23A C23 H23B 108.0 . . ?
C24 C23 H23A 109.3 . . ?
C24 C23 H23B 109.3 . . ?
C23 C24 H24A 109.7 . . ?
C23 C24 H24B 109.7 . . ?
H24A C24 H24B 108.2 . . ?
C25 C24 C23 109.9(7) . . ?
C25 C24 H24A 109.7 . . ?
C25 C24 H24B 109.7 . . ?
C20 C25 C24 123.0(7) . . ?
C26 C25 C20 105.3(6) . . ?
C26 C25 C24 131.6(7) . . ?
N18 C26 H26 126.4 . . ?
C25 C26 N18 107.2(6) . . ?
C25 C26 H26 126.4 . . ?
C32 N27 C28 113.8(6) . . ?
N27 C28 N29 126.2(7) . . ?
N27 C28 N33 116.4(6) . . ?
N29 C28 N33 117.4(6) . . ?
C28 N29 Ag1 110.5(5) . . ?
C30 N29 Ag1 136.2(5) . . ?
C30 N29 C28 112.9(7) . . ?
N29 C30 H30 116.5 . . ?
N29 C30 N31 127.0(7) . . ?
N31 C30 H30 116.5 . . ?
C30 N31 Ag2 131.6(5) . 2_656 ?
C30 N31 C32 113.2(6) . . ?
C32 N31 Ag2 115.1(5) . 2_656 ?
N27 C32 N31 126.4(7) . . ?
N27 C32 N42 115.8(7) . . ?
N31 C32 N42 117.8(6) . . ?
C28 N33 C41 126.1(6) . . ?
N34 N33 C28 122.3(6) . . ?
N34 N33 C41 111.2(6) . . ?
N33 N34 Ag1 120.1(4) . . ?
C35 N34 Ag1 133.4(5) . . ?
C35 N34 N33 105.6(6) . . ?
N34 C35 C36 124.7(7) . . ?
N34 C35 C40 110.3(6) . . ?
C40 C35 C36 125.0(7) . . ?
C35 C36 H36A 110.1 . . ?
C35 C36 H36B 110.1 . . ?
C35 C36 C37 108.1(7) . . ?
H36A C36 H36B 108.4 . . ?
C37 C36 H36A 110.1 . . ?
C37 C36 H36B 110.1 . . ?
C36 C37 H37A 108.7 . . ?
C36 C37 H37B 108.7 . . ?
H37A C37 H37B 107.6 . . ?
C38 C37 C36 114.4(8) . . ?
C38 C37 H37A 108.7 . . ?
C38 C37 H37B 108.7 . . ?
C37 C38 H38A 108.9 . . ?
C37 C38 H38B 108.9 . . ?
C37 C38 C39 113.3(8) . . ?
H38A C38 H38B 107.7 . . ?
C39 C38 H38A 108.9 . . ?
C39 C38 H38B 108.9 . . ?
C38 C39 H39A 109.6 . . ?
C38 C39 H39B 109.6 . . ?
C38 C39 C40 110.4(7) . . ?
H39A C39 H39B 108.1 . . ?
C40 C39 H39A 109.6 . . ?
C40 C39 H39B 109.6 . . ?
C35 C40 C39 122.0(6) . . ?
C41 C40 C35 106.5(6) . . ?
C41 C40 C39 131.4(6) . . ?
N33 C41 H41 126.8 . . ?
C40 C41 N33 106.3(6) . . ?
C40 C41 H41 126.8 . . ?
C32 N42 N43 120.4(6) . . ?
C50 N42 C32 127.3(6) . . ?
C50 N42 N43 112.1(6) . . ?
N42 N43 Ag2 115.2(5) . 2_656 ?
C44 N43 Ag2 141.3(5) . 2_656 ?
C44 N43 N42 103.3(6) . . ?
N43 C44 C45 123.2(7) . . ?
N43 C44 C49 112.3(6) . . ?
C49 C44 C45 124.4(7) . . ?
C44 C45 H45A 109.7 . . ?
C44 C45 H45B 109.7 . . ?
C44 C45 C46 109.8(7) . . ?
H45A C45 H45B 108.2 . . ?
C46 C45 H45A 109.7 . . ?
C46 C45 H45B 109.7 . . ?
C45 C46 H46A 108.9 . . ?
C45 C46 H46B 108.9 . . ?
H46A C46 H46B 107.7 . . ?
C47 C46 C45 113.5(8) . . ?
C47 C46 H46A 108.9 . . ?
C47 C46 H46B 108.9 . . ?
C46 C47 H47A 108.6 . . ?
C46 C47 H47B 108.6 . . ?
C46 C47 C48 114.7(9) . . ?
H47A C47 H47B 107.6 . . ?
C48 C47 H47A 108.6 . . ?
C48 C47 H47B 108.6 . . ?
C47 C48 H48A 109.9 . . ?
C47 C48 H48B 109.9 . . ?
H48A C48 H48B 108.3 . . ?
C49 C48 C47 108.9(7) . . ?
C49 C48 H48A 109.9 . . ?
C49 C48 H48B 109.9 . . ?
C44 C49 C48 123.4(7) . . ?
C50 C49 C44 106.0(7) . . ?
C50 C49 C48 130.6(7) . . ?
N42 C50 H50 126.9 . . ?
C49 C50 N42 106.3(7) . . ?
C49 C50 H50 126.9 . . ?
O53 Cl51 O52 109.9(7) . . ?
O54 Cl51 O52 110.8(8) . . ?
O54 Cl51 O53 108.6(7) . . ?
O55 Cl51 O52 105.6(8) . . ?
O55 Cl51 O53 110.6(9) . . ?
O55 Cl51 O54 111.4(8) . . ?
O57A Cl5A O58A 111.1(12) . . ?
O57A Cl5A O59A 112.3(12) . . ?
O57A Cl5A O60A 110.5(14) . . ?
O58A Cl5A O59A 111.4(10) . . ?
O58A Cl5A O60A 105.7(13) . . ?
O59A Cl5A O60A 105.6(12) . . ?
Cl5A O57A Ag1 122.0(15) . . ?
O57B Cl5B O58B 107.5(15) . . ?
O59B Cl5B O57B 109.7(14) . . ?
O59B Cl5B O58B 109.8(16) . . ?
O59B Cl5B O60B 112.4(15) . . ?
O60B Cl5B O57B 109.2(15) . . ?
O60B Cl5B O58B 108.1(15) . . ?
Cl5B O57B Ag1 127.1(15) . . ?
O62 Cl61 O64 108.2(10) . . ?
O63 Cl61 O62 107.7(13) . . ?
O63 Cl61 O64 115.2(10) . . ?
O63 Cl61 O65 103.2(12) . . ?
O65 Cl61 O62 114.8(13) . . ?
O65 Cl61 O64 107.9(9) . . ?
O67 Cl66 O67 109.3(6) . 2_556 ?
O68 Cl66 O67 108.6(4) 2_556 2_556 ?
O68 Cl66 O67 109.7(4) . 2_556 ?
O68 Cl66 O67 109.7(4) 2_556 . ?
O68 Cl66 O67 108.6(4) . . ?
O68 Cl66 O68 110.8(6) . 2_556 ?
H69A C69 H69B 109.5 . . ?
H69A C69 H69C 109.5 . . ?
H69B C69 H69C 109.5 . . ?
N70 C69 H69A 109.5 . . ?
N70 C69 H69B 109.5 . . ?
N70 C69 H69C 109.5 . . ?
O71 N70 C69 120.0(17) . . ?
O72 N70 C69 121.0(17) . . ?
O72 N70 O71 118.7(16) . . ?

_exptl_crystal_recrystallization_method 
'Re-crystallisation from solvent: nitromethane-diethyl ether'
####################################################################### 
# 
# 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_sf-23
_database_code_depnum_ccdc_archive 'CCDC 1957580'
loop_
_audit_author_name
_audit_author_address
'Malcolm Halcrow' 'University of Leeds'
_audit_update_record             
;
2019-10-04 deposited with the CCDC.	2019-11-05 downloaded from the CCDC.
;
_audit_creation_date             2019-08-11
_audit_creation_method           
;
  Olex2 1.2
  (compiled Apr 23 2013 17:54:37, GUI svn.r4466)
;
_chemical_name_common            ?
_chemical_name_systematic        
'Tetrakis-[2,4-di(3,5-dimethylpyrazol-1-yl)-6H-1,3,5-triazine)]-tetrasilver(I) tetra-hexafluoroantimonate nitromethane solvate'
_chemical_formula_moiety         'C52 H60 Ag4 N28, 4(F6 Sb), C H3 N O2'
_chemical_formula_sum            'C53 H63 Ag4 F24 N29 O2 Sb4'
_chemical_formula_weight         2512.80
_chemical_melting_point          ?
loop_
_atom_type_symbol
_atom_type_description
_atom_type_scat_dispersion_real
_atom_type_scat_dispersion_imag
_atom_type_scat_source
C C 0.0181 0.0091 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
N N 0.0311 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'
Sb Sb -0.0562 5.8946 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Ag Ag 0.1306 4.2820 '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'

_space_group_crystal_system      monoclinic
_space_group_IT_number           14
_space_group_name_H-M_alt        'P 1 21/n 1'
_space_group_name_Hall           '-P 2yn'
loop_
_space_group_symop_id
_space_group_symop_operation_xyz
1 'x, y, z'
2 '-x+1/2, y+1/2, -z+1/2'
3 '-x, -y, -z'
4 'x-1/2, -y-1/2, z-1/2'

_cell_length_a                   22.9855(3)
_cell_length_b                   14.9629(3)
_cell_length_c                   23.3614(3)
_cell_angle_alpha                90.00
_cell_angle_beta                 95.028(1)
_cell_angle_gamma                90.00
_cell_volume                     8003.8(2)
_cell_formula_units_Z            4
_cell_measurement_reflns_used    17247
_cell_measurement_temperature    120(2)
_cell_measurement_theta_min      3.49
_cell_measurement_theta_max      73.73
_exptl_absorpt_coefficient_mu    19.250
_exptl_absorpt_correction_T_min  0.142
_exptl_absorpt_correction_T_max  1.000
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   
; 
CrysAlisPro, Agilent Technologies,
Version 1.171.36.24 (release 03-12-2012 CrysAlis171 .NET)
Empirical absorption correction using spherical harmonics,
 implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_crystal_colour            colourless
_exptl_crystal_density_diffrn    2.085
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       needle
_exptl_crystal_F_000             4832
_exptl_crystal_size_max          0.45
_exptl_crystal_size_mid          0.15
_exptl_crystal_size_min          0.05
_exptl_special_details           
;
 ? 
;
_diffrn_reflns_av_R_equivalents  0.0462
_diffrn_reflns_av_unetI/netI     0.0544
_diffrn_reflns_limit_h_max       28
_diffrn_reflns_limit_h_min       -27
_diffrn_reflns_limit_k_max       16
_diffrn_reflns_limit_k_min       -18
_diffrn_reflns_limit_l_max       29
_diffrn_reflns_limit_l_min       -26
_diffrn_reflns_number            33503
_diffrn_reflns_theta_full        72.00
_diffrn_reflns_theta_max         73.83
_diffrn_reflns_theta_min         3.51
_diffrn_ambient_temperature      120(2)
_diffrn_detector_area_resol_mean 5.3095
_diffrn_measured_fraction_theta_full 0.989
_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                13737
_reflns_number_total             15778
_reflns_threshold_expression     >2sigma(I)
_computing_cell_refinement       'CrysAlisPro, Agilent Technologies'
_computing_data_collection       '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         1.703
_refine_diff_density_min         -1.703
_refine_diff_density_rms         0.175
_refine_ls_extinction_coef       ?
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.044
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     1062
_refine_ls_number_reflns         15778
_refine_ls_number_restraints     0
_refine_ls_R_factor_all          0.0512
_refine_ls_R_factor_gt           0.0444
_refine_ls_restrained_S_all      1.044
_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)+(0.0631P)²+14.3568P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1143
_refine_ls_wR_factor_ref         0.1201
_refine_special_details          
;
 Refinement of F² against ALL reflections.  The weighted R-factor wR and 
 goodness of fit S are based on F², conventional R-factors R are based 
 on F, with F set to zero for negative F². The threshold expression of 
 F² > 2sigma(F²) is used only for calculating R-factors(gt) etc. and is 
 not relevant to the choice of reflections for refinement.  R-factors based 
 on F² are statistically about twice as large as those based on F, and R- 
 factors based on ALL data will be even larger. 

 No disorder is present in the model, and no restraints were applied to the
 refinement. All non-H atoms were refined anisotropically, and H atoms were
 placed in calculated positions and refined using a riding model. The 
 highest residual peak (+1.7 eÅ⁻³) and hole (-1.7 eÅ⁻³) are 0.9 Å 
 from Ag2 and Sb99, respectively.
;
_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.a Aromatic/amide H refined with riding coordinates:
 C8(H8), C14(H14), C21(H21), C28(H28), C34(H34), C41(H41), C48(H48), C54(H54),
 C61(H61), C68(H68), C74(H74), C81(H81)
2.b Idealised Me refined as rotating group:
 C16(H16A,H16B,H16C), C17(H17A,H17B,H17C), C23(H23A,H23B,H23C), C24(H24A,H24B,
 H24C), C36(H36A,H36B,H36C), C37(H37A,H37B,H37C), C43(H43A,H43B,H43C), C44(H44A,
 H44B,H44C), C56(H56A,H56B,H56C), C57(H57A,H57B,H57C), C63(H63A,H63B,H63C),
 C64(H64A,H64B,H64C), C76(H76A,H76B,H76C), C77(H77A,H77B,H77C), C83(H83A,H83B,
 H83C), C84(H84A,H84B,H84C), C113(H11A,H11B,H11C)
;
_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
Ag1 Ag 0.386320(16) 0.50342(3) 0.609940(17) 0.02175(10) Uani 1 1 d . . .
Ag2 Ag 0.327088(16) 0.06456(3) 0.609525(18) 0.02529(10) Uani 1 1 d . . .
Ag3 Ag 0.127990(16) -0.01371(3) 0.395042(15) 0.01886(9) Uani 1 1 d . . .
Ag4 Ag 0.157061(19) 0.43477(3) 0.418044(17) 0.02837(11) Uani 1 1 d . . .
N5 N 0.47594(17) 0.2428(3) 0.56961(17) 0.0138(8) Uani 1 1 d . . .
C6 C 0.4542(2) 0.3246(4) 0.5718(2) 0.0161(10) Uani 1 1 d . . .
N7 N 0.39867(18) 0.3462(3) 0.57882(19) 0.0177(9) Uani 1 1 d . . .
C8 C 0.3649(2) 0.2764(4) 0.5871(2) 0.0210(11) Uani 1 1 d . . .
H8 H 0.3251 0.2882 0.5923 0.025 Uiso 1 1 calc R . .
N9 N 0.38165(18) 0.1922(3) 0.58857(19) 0.0174(9) Uani 1 1 d . . .
C10 C 0.4378(2) 0.1788(4) 0.57840(19) 0.0136(9) Uani 1 1 d . . .
N11 N 0.49231(18) 0.3979(3) 0.56768(19) 0.0178(9) Uani 1 1 d . . .
N12 N 0.47612(18) 0.4790(3) 0.5886(2) 0.0194(9) Uani 1 1 d . . .
C13 C 0.5194(2) 0.5338(4) 0.5828(3) 0.0229(12) Uani 1 1 d . . .
C14 C 0.5643(2) 0.4894(4) 0.5566(3) 0.0264(13) Uani 1 1 d . . .
H14 H 0.6002 0.5148 0.5473 0.032 Uiso 1 1 calc R . .
C15 C 0.5467(2) 0.4030(4) 0.5471(2) 0.0227(11) Uani 1 1 d . . .
C16 C 0.5180(3) 0.6270(4) 0.6041(3) 0.0322(14) Uani 1 1 d . . .
H16A H 0.4776 0.6436 0.6098 0.048 Uiso 1 1 calc R . .
H16B H 0.5333 0.6673 0.5760 0.048 Uiso 1 1 calc R . .
H16C H 0.5420 0.6317 0.6408 0.048 Uiso 1 1 calc R . .
C17 C 0.5773(2) 0.3289(5) 0.5209(3) 0.0338(15) Uani 1 1 d . . .
H17A H 0.6060 0.3533 0.4965 0.051 Uiso 1 1 calc R . .
H17B H 0.5489 0.2923 0.4975 0.051 Uiso 1 1 calc R . .
H17C H 0.5972 0.2920 0.5512 0.051 Uiso 1 1 calc R . .
N18 N 0.45606(17) 0.0907(3) 0.57751(18) 0.0167(9) Uani 1 1 d . . .
N19 N 0.41534(19) 0.0249(3) 0.5846(2) 0.0186(9) Uani 1 1 d . . .
C20 C 0.4433(3) -0.0514(4) 0.5842(2) 0.0243(12) Uani 1 1 d . . .
C21 C 0.5031(2) -0.0361(4) 0.5773(3) 0.0248(12) Uani 1 1 d . . .
H21 H 0.5324 -0.0806 0.5755 0.030 Uiso 1 1 calc R . .
C22 C 0.5110(2) 0.0525(4) 0.5738(2) 0.0181(10) Uani 1 1 d . . .
C23 C 0.4115(3) -0.1370(4) 0.5915(3) 0.0339(14) Uani 1 1 d . . .
H23A H 0.3883 -0.1322 0.6247 0.051 Uiso 1 1 calc R . .
H23B H 0.4397 -0.1859 0.5979 0.051 Uiso 1 1 calc R . .
H23C H 0.3855 -0.1492 0.5569 0.051 Uiso 1 1 calc R . .
C24 C 0.5661(2) 0.1042(4) 0.5683(3) 0.0259(12) Uani 1 1 d . . .
H24A H 0.5987 0.0626 0.5659 0.039 Uiso 1 1 calc R . .
H24B H 0.5740 0.1429 0.6020 0.039 Uiso 1 1 calc R . .
H24C H 0.5617 0.1409 0.5335 0.039 Uiso 1 1 calc R . .
N25 N 0.14175(18) -0.0317(3) 0.59108(18) 0.0143(8) Uani 1 1 d . . .
C26 C 0.1946(2) 0.0011(4) 0.6073(2) 0.0139(9) Uani 1 1 d . . .
N27 N 0.23119(18) 0.0385(3) 0.57265(19) 0.0182(9) Uani 1 1 d . . .
C28 C 0.2100(2) 0.0455(4) 0.5183(2) 0.0174(10) Uani 1 1 d . . .
H28 H 0.2337 0.0749 0.4928 0.021 Uiso 1 1 calc R . .
N29 N 0.15845(19) 0.0149(3) 0.49641(19) 0.0178(9) Uani 1 1 d . . .
C30 C 0.1275(2) -0.0253(3) 0.5351(2) 0.0149(10) Uani 1 1 d . . .
N31 N 0.21597(17) -0.0067(3) 0.66479(17) 0.0140(8) Uani 1 1 d . . .
N32 N 0.27419(18) 0.0107(3) 0.67915(19) 0.0170(9) Uani 1 1 d . . .
C33 C 0.2844(2) -0.0081(4) 0.7343(2) 0.0207(11) Uani 1 1 d . . .
C34 C 0.2326(2) -0.0383(4) 0.7566(2) 0.0207(11) Uani 1 1 d . . .
H34 H 0.2286 -0.0566 0.7950 0.025 Uiso 1 1 calc R . .
C35 C 0.1898(2) -0.0362(4) 0.7128(2) 0.0167(10) Uani 1 1 d . . .
C36 C 0.3438(3) 0.0012(5) 0.7641(3) 0.0327(15) Uani 1 1 d . . .
H36A H 0.3622 -0.0578 0.7683 0.049 Uiso 1 1 calc R . .
H36B H 0.3410 0.0276 0.8022 0.049 Uiso 1 1 calc R . .
H36C H 0.3674 0.0401 0.7416 0.049 Uiso 1 1 calc R . .
C37 C 0.1273(2) -0.0616(5) 0.7138(2) 0.0255(13) Uani 1 1 d . . .
H37A H 0.1201 -0.1179 0.6929 0.038 Uiso 1 1 calc R . .
H37B H 0.1026 -0.0146 0.6953 0.038 Uiso 1 1 calc R . .
H37C H 0.1181 -0.0690 0.7537 0.038 Uiso 1 1 calc R . .
N38 N 0.07572(17) -0.0655(3) 0.51221(18) 0.0155(9) Uani 1 1 d . . .
N39 N 0.06900(19) -0.0811(3) 0.45359(18) 0.0188(9) Uani 1 1 d . . .
C40 C 0.0201(2) -0.1258(4) 0.4439(2) 0.0207(11) Uani 1 1 d . . .
C41 C -0.0065(2) -0.1391(4) 0.4956(2) 0.0214(11) Uani 1 1 d . . .
H41 H -0.0424 -0.1690 0.4996 0.026 Uiso 1 1 calc R . .
C42 C 0.0289(2) -0.1009(4) 0.5384(2) 0.0184(11) Uani 1 1 d . . .
C43 C 0.0002(3) -0.1577(5) 0.3845(2) 0.0315(14) Uani 1 1 d . . .
H43A H 0.0260 -0.1333 0.3571 0.047 Uiso 1 1 calc R . .
H43B H -0.0399 -0.1376 0.3742 0.047 Uiso 1 1 calc R . .
H43C H 0.0016 -0.2232 0.3835 0.047 Uiso 1 1 calc R . .
C44 C 0.0207(2) -0.0951(4) 0.6007(2) 0.0216(11) Uani 1 1 d . . .
H44A H -0.0196 -0.1114 0.6070 0.032 Uiso 1 1 calc R . .
H44B H 0.0285 -0.0339 0.6142 0.032 Uiso 1 1 calc R . .
H44C H 0.0477 -0.1363 0.6221 0.032 Uiso 1 1 calc R . .
N45 N 0.16581(17) 0.2283(3) 0.28038(17) 0.0124(8) Uani 1 1 d . . .
C46 C 0.15495(19) 0.1524(3) 0.3073(2) 0.0116(9) Uani 1 1 d . . .
N47 N 0.14797(18) 0.1426(3) 0.36312(17) 0.0157(8) Uani 1 1 d . . .
C48 C 0.1519(2) 0.2187(4) 0.3921(2) 0.0182(10) Uani 1 1 d . . .
H48 H 0.1479 0.2151 0.4322 0.022 Uiso 1 1 calc R . .
N49 N 0.16078(19) 0.2996(3) 0.37100(17) 0.0151(8) Uani 1 1 d . . .
C50 C 0.16804(19) 0.2997(3) 0.3149(2) 0.0113(9) Uani 1 1 d . . .
N51 N 0.15067(18) 0.0743(3) 0.27506(17) 0.0138(8) Uani 1 1 d . . .
N52 N 0.14613(19) -0.0061(3) 0.30328(18) 0.0161(9) Uani 1 1 d . . .
C53 C 0.1431(2) -0.0689(4) 0.2633(2) 0.0195(11) Uani 1 1 d . . .
C54 C 0.1458(2) -0.0297(4) 0.2085(2) 0.0216(11) Uani 1 1 d . . .
H54 H 0.1450 -0.0604 0.1729 0.026 Uiso 1 1 calc R . .
C55 C 0.1498(2) 0.0598(4) 0.2162(2) 0.0206(11) Uani 1 1 d . . .
C56 C 0.1373(4) -0.1650(4) 0.2776(3) 0.0365(16) Uani 1 1 d . . .
H56A H 0.1494 -0.1743 0.3184 0.055 Uiso 1 1 calc R . .
H56B H 0.1621 -0.2007 0.2543 0.055 Uiso 1 1 calc R . .
H56C H 0.0965 -0.1835 0.2695 0.055 Uiso 1 1 calc R . .
C57 C 0.1513(4) 0.1301(5) 0.1721(2) 0.0368(16) Uani 1 1 d . . .
H57A H 0.1468 0.1028 0.1338 0.055 Uiso 1 1 calc R . .
H57B H 0.1887 0.1617 0.1772 0.055 Uiso 1 1 calc R . .
H57C H 0.1193 0.1724 0.1760 0.055 Uiso 1 1 calc R . .
N58 N 0.17995(18) 0.3821(3) 0.29109(17) 0.0152(8) Uani 1 1 d . . .
N59 N 0.1784(2) 0.4567(3) 0.3262(2) 0.0208(9) Uani 1 1 d . . .
C60 C 0.1902(3) 0.5261(4) 0.2945(3) 0.0268(12) Uani 1 1 d . . .
C61 C 0.1998(3) 0.4978(4) 0.2382(3) 0.0256(12) Uani 1 1 d . . .
H61 H 0.2094 0.5351 0.2074 0.031 Uiso 1 1 calc R . .
C62 C 0.1928(2) 0.4076(4) 0.2361(2) 0.0177(10) Uani 1 1 d . . .
C63 C 0.1891(4) 0.6180(5) 0.3181(3) 0.0471(19) Uani 1 1 d . . .
H63A H 0.1485 0.6366 0.3206 0.071 Uiso 1 1 calc R . .
H63B H 0.2080 0.6591 0.2928 0.071 Uiso 1 1 calc R . .
H63C H 0.2099 0.6191 0.3565 0.071 Uiso 1 1 calc R . .
C64 C 0.1973(3) 0.3471(4) 0.1869(2) 0.0284(13) Uani 1 1 d . . .
H64A H 0.2049 0.3822 0.1529 0.043 Uiso 1 1 calc R . .
H64B H 0.1606 0.3141 0.1792 0.043 Uiso 1 1 calc R . .
H64C H 0.2294 0.3049 0.1958 0.043 Uiso 1 1 calc R . .
N65 N 0.19706(18) 0.5949(3) 0.57927(17) 0.0143(8) Uani 1 1 d . . .
C66 C 0.1750(2) 0.5518(3) 0.5319(2) 0.0137(9) Uani 1 1 d . . .
N67 N 0.20442(19) 0.4938(3) 0.50157(18) 0.0163(9) Uani 1 1 d . . .
C68 C 0.2597(2) 0.4817(4) 0.5217(2) 0.0182(10) Uani 1 1 d . . .
H68 H 0.2816 0.4398 0.5019 0.022 Uiso 1 1 calc R . .
N69 N 0.28731(18) 0.5220(3) 0.56658(19) 0.0174(9) Uani 1 1 d . . .
C70 C 0.2528(2) 0.5780(3) 0.5937(2) 0.0139(9) Uani 1 1 d . . .
N71 N 0.11769(19) 0.5677(3) 0.51156(18) 0.0171(9) Uani 1 1 d . . .
N72 N 0.09635(19) 0.5259(3) 0.46072(19) 0.0197(9) Uani 1 1 d . . .
C73 C 0.0436(2) 0.5582(4) 0.4486(2) 0.0208(11) Uani 1 1 d . . .
C74 C 0.0289(2) 0.6186(4) 0.4906(2) 0.0247(12) Uani 1 1 d . . .
H74 H -0.0070 0.6499 0.4912 0.030 Uiso 1 1 calc R . .
C75 C 0.0755(2) 0.6244(4) 0.5303(2) 0.0199(11) Uani 1 1 d . . .
C76 C 0.0078(3) 0.5293(5) 0.3946(3) 0.0309(14) Uani 1 1 d . . .
H76A H 0.0038 0.5795 0.3676 0.046 Uiso 1 1 calc R . .
H76B H -0.0310 0.5103 0.4042 0.046 Uiso 1 1 calc R . .
H76C H 0.0273 0.4794 0.3770 0.046 Uiso 1 1 calc R . .
C77 C 0.0817(2) 0.6786(5) 0.5835(3) 0.0298(14) Uani 1 1 d . . .
H77A H 0.0448 0.7092 0.5885 0.045 Uiso 1 1 calc R . .
H77B H 0.1127 0.7230 0.5808 0.045 Uiso 1 1 calc R . .
H77C H 0.0918 0.6395 0.6166 0.045 Uiso 1 1 calc R . .
N78 N 0.28080(18) 0.6213(3) 0.64160(17) 0.0158(9) Uani 1 1 d . . .
N79 N 0.33798(18) 0.6001(3) 0.65867(19) 0.0187(9) Uani 1 1 d . . .
C80 C 0.3542(2) 0.6540(4) 0.7020(2) 0.0223(11) Uani 1 1 d . . .
C81 C 0.3087(3) 0.7109(4) 0.7134(3) 0.0282(13) Uani 1 1 d . . .
H81 H 0.3098 0.7554 0.7425 0.034 Uiso 1 1 calc R . .
C82 C 0.2624(2) 0.6910(4) 0.6753(2) 0.0210(11) Uani 1 1 d . . .
C83 C 0.4147(3) 0.6503(5) 0.7309(3) 0.0342(15) Uani 1 1 d . . .
H83A H 0.4355 0.5992 0.7162 0.051 Uiso 1 1 calc R . .
H83B H 0.4129 0.6437 0.7725 0.051 Uiso 1 1 calc R . .
H83C H 0.4355 0.7056 0.7231 0.051 Uiso 1 1 calc R . .
C84 C 0.2037(3) 0.7345(5) 0.6688(3) 0.0353(16) Uani 1 1 d . . .
H84A H 0.2015 0.7799 0.6987 0.053 Uiso 1 1 calc R . .
H84B H 0.1734 0.6893 0.6724 0.053 Uiso 1 1 calc R . .
H84C H 0.1978 0.7629 0.6309 0.053 Uiso 1 1 calc R . .
Sb85 Sb 0.167175(14) 0.28649(2) 0.598849(15) 0.01874(9) Uani 1 1 d . . .
F86 F 0.2279(2) 0.2290(3) 0.6432(2) 0.0559(13) Uani 1 1 d . . .
F87 F 0.13332(18) 0.1759(3) 0.5778(2) 0.0511(12) Uani 1 1 d . . .
F88 F 0.20136(19) 0.3968(3) 0.61900(17) 0.0395(9) Uani 1 1 d . . .
F89 F 0.1238(2) 0.2922(3) 0.66241(19) 0.0457(11) Uani 1 1 d . . .
F90 F 0.2117(2) 0.2806(3) 0.5358(2) 0.0513(12) Uani 1 1 d . . .
F91 F 0.10804(19) 0.3439(4) 0.5533(2) 0.0534(13) Uani 1 1 d . . .
Sb92 Sb 0.249895(14) -0.21234(2) 0.476028(14) 0.01800(9) Uani 1 1 d . . .
F93 F 0.2086(2) -0.3169(3) 0.45933(18) 0.0483(11) Uani 1 1 d . . .
F94 F 0.3042(2) -0.2457(4) 0.42520(17) 0.0491(12) Uani 1 1 d . . .
F95 F 0.2914(2) -0.1070(3) 0.4927(2) 0.0516(12) Uani 1 1 d . . .
F96 F 0.1957(2) -0.1795(3) 0.52788(18) 0.0463(11) Uani 1 1 d . . .
F97 F 0.29476(16) -0.2709(3) 0.53619(15) 0.0323(8) Uani 1 1 d . . .
F98 F 0.20528(16) -0.1533(3) 0.41638(16) 0.0359(9) Uani 1 1 d . . .
Sb99 Sb 0.339502(13) 0.20632(2) 0.399671(14) 0.01818(9) Uani 1 1 d . . .
F100 F 0.3446(2) 0.0829(3) 0.3938(2) 0.0488(11) Uani 1 1 d . . .
F101 F 0.39578(17) 0.2156(3) 0.34674(16) 0.0424(11) Uani 1 1 d . . .
F102 F 0.33650(19) 0.3300(3) 0.4053(2) 0.0438(10) Uani 1 1 d . . .
F103 F 0.2833(2) 0.1949(3) 0.4511(2) 0.0496(11) Uani 1 1 d . . .
F104 F 0.28146(18) 0.2074(4) 0.3380(2) 0.0523(12) Uani 1 1 d . . .
F105 F 0.40003(17) 0.2054(3) 0.45880(15) 0.0369(9) Uani 1 1 d . . .
Sb106 Sb -0.007363(14) 0.27319(3) 0.246448(14) 0.02132(9) Uani 1 1 d . . .
F107 F 0.05173(19) 0.2865(5) 0.1971(2) 0.0681(18) Uani 1 1 d . . .
F108 F -0.04682(17) 0.3684(3) 0.20798(17) 0.0383(9) Uani 1 1 d . . .
F109 F 0.0337(2) 0.3498(4) 0.2984(2) 0.0602(15) Uani 1 1 d . . .
F110 F -0.0470(2) 0.1931(3) 0.19470(16) 0.0409(10) Uani 1 1 d . . .
F111 F -0.06738(17) 0.2612(3) 0.29452(16) 0.0363(9) Uani 1 1 d . . .
F112 F 0.03207(16) 0.1769(3) 0.28311(18) 0.0449(11) Uani 1 1 d . . .
C113 C 0.5458(3) -0.0411(5) 0.7273(3) 0.0430(17) Uani 1 1 d . . .
H11A H 0.5779 -0.0562 0.7040 0.064 Uiso 1 1 calc R . .
H11B H 0.5615 -0.0112 0.7627 0.064 Uiso 1 1 calc R . .
H11C H 0.5183 -0.0012 0.7055 0.064 Uiso 1 1 calc R . .
N114 N 0.5153(3) -0.1233(5) 0.7420(3) 0.0505(17) Uani 1 1 d . . .
O115 O 0.5367(3) -0.1711(5) 0.7796(3) 0.0632(17) Uani 1 1 d . . .
O116 O 0.4680(5) -0.1349(8) 0.7179(5) 0.126(5) Uani 1 1 d . . .


_geom_special_details            
;
 All esds (except the esd in the dihedral angle between two l.s. planes) 
 are estimated using the full covariance matrix.  The cell esds are taken 
 into account individually in the estimation of esds in distances, angles 
 and torsion angles; correlations between esds in cell parameters are only 
 used when they are defined by crystal symmetry.  An approximate (isotropic) 
 treatment of cell esds is used for estimating esds involving l.s. planes. 
;
loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
_geom_bond_publ_flag
Ag1 N7 2.486(5) . ?
Ag1 N12 2.196(4) . ?
Ag1 N69 2.425(4) . ?
Ag1 N79 2.201(5) . ?
Ag2 N9 2.360(5) . ?
Ag2 N19 2.239(4) . ?
Ag2 N27 2.328(4) . ?
Ag2 N32 2.263(4) . ?
Ag3 N29 2.448(4) . ?
Ag3 N39 2.247(5) . ?
Ag3 N47 2.510(5) . ?
Ag3 N52 2.222(4) . ?
Ag3 F98 2.759(4) . ?
Ag4 N49 2.307(4) . ?
Ag4 N59 2.267(5) . ?
Ag4 N67 2.324(4) . ?
Ag4 N72 2.246(5) . ?
N5 C6 1.324(7) . ?
N5 C10 1.326(7) . ?
C6 N7 1.340(7) . ?
C6 N11 1.413(7) . ?
N7 C8 1.325(8) . ?
C8 H8 0.9500 . ?
C8 N9 1.317(8) . ?
N9 C10 1.348(6) . ?
C10 N18 1.385(7) . ?
N11 N12 1.372(7) . ?
N11 C15 1.379(7) . ?
N12 C13 1.306(7) . ?
C13 C14 1.411(9) . ?
C13 C16 1.482(9) . ?
C14 H14 0.9500 . ?
C14 C15 1.367(9) . ?
C15 C17 1.475(9) . ?
C16 H16A 0.9800 . ?
C16 H16B 0.9800 . ?
C16 H16C 0.9800 . ?
C17 H17A 0.9800 . ?
C17 H17B 0.9800 . ?
C17 H17C 0.9800 . ?
N18 N19 1.377(7) . ?
N18 C22 1.395(7) . ?
N19 C20 1.312(8) . ?
C20 C21 1.417(9) . ?
C20 C23 1.492(9) . ?
C21 H21 0.9500 . ?
C21 C22 1.341(9) . ?
C22 C24 1.499(8) . ?
C23 H23A 0.9800 . ?
C23 H23B 0.9800 . ?
C23 H23C 0.9800 . ?
C24 H24A 0.9800 . ?
C24 H24B 0.9800 . ?
C24 H24C 0.9800 . ?
N25 C26 1.334(7) . ?
N25 C30 1.323(7) . ?
C26 N27 1.340(7) . ?
C26 N31 1.394(6) . ?
N27 C28 1.323(7) . ?
C28 H28 0.9500 . ?
C28 N29 1.331(7) . ?
N29 C30 1.341(7) . ?
C30 N38 1.398(6) . ?
N31 N32 1.376(6) . ?
N31 C35 1.391(7) . ?
N32 C33 1.320(7) . ?
C33 C34 1.415(8) . ?
C33 C36 1.483(7) . ?
C34 H34 0.9500 . ?
C34 C35 1.357(7) . ?
C35 C37 1.487(7) . ?
C36 H36A 0.9800 . ?
C36 H36B 0.9800 . ?
C36 H36C 0.9800 . ?
C37 H37A 0.9800 . ?
C37 H37B 0.9800 . ?
C37 H37C 0.9800 . ?
N38 N39 1.384(6) . ?
N38 C42 1.390(7) . ?
N39 C40 1.310(7) . ?
C40 C41 1.414(8) . ?
C40 C43 1.501(7) . ?
C41 H41 0.9500 . ?
C41 C42 1.358(7) . ?
C42 C44 1.487(7) . ?
C43 H43A 0.9800 . ?
C43 H43B 0.9800 . ?
C43 H43C 0.9800 . ?
C44 H44A 0.9800 . ?
C44 H44B 0.9800 . ?
C44 H44C 0.9800 . ?
N45 C46 1.332(6) . ?
N45 C50 1.336(6) . ?
C46 N47 1.336(6) . ?
C46 N51 1.389(6) . ?
N47 C48 1.323(7) . ?
C48 H48 0.9500 . ?
C48 N49 1.329(7) . ?
N49 C50 1.337(6) . ?
C50 N58 1.390(7) . ?
N51 N52 1.380(6) . ?
N51 C55 1.391(6) . ?
N52 C53 1.324(7) . ?
C53 C54 1.415(8) . ?
C53 C56 1.485(8) . ?
C54 H54 0.9500 . ?
C54 C55 1.352(8) . ?
C55 C57 1.474(8) . ?
C56 H56A 0.9800 . ?
C56 H56B 0.9800 . ?
C56 H56C 0.9800 . ?
C57 H57A 0.9800 . ?
C57 H57B 0.9800 . ?
C57 H57C 0.9800 . ?
N58 N59 1.387(6) . ?
N58 C62 1.395(7) . ?
N59 C60 1.317(8) . ?
C60 C61 1.417(9) . ?
C60 C63 1.483(9) . ?
C61 H61 0.9500 . ?
C61 C62 1.360(8) . ?
C62 C64 1.475(8) . ?
C63 H63A 0.9800 . ?
C63 H63B 0.9800 . ?
C63 H63C 0.9800 . ?
C64 H64A 0.9800 . ?
C64 H64B 0.9800 . ?
C64 H64C 0.9800 . ?
N65 C66 1.341(6) . ?
N65 C70 1.319(7) . ?
C66 N67 1.340(7) . ?
C66 N71 1.382(6) . ?
N67 C68 1.328(7) . ?
C68 H68 0.9500 . ?
C68 N69 1.323(7) . ?
N69 C70 1.349(7) . ?
C70 N78 1.401(6) . ?
N71 N72 1.393(6) . ?
N71 C75 1.389(7) . ?
N72 C73 1.314(7) . ?
C73 C74 1.398(8) . ?
C73 C76 1.505(7) . ?
C74 H74 0.9500 . ?
C74 C75 1.356(7) . ?
C75 C77 1.480(8) . ?
C76 H76A 0.9800 . ?
C76 H76B 0.9800 . ?
C76 H76C 0.9800 . ?
C77 H77A 0.9800 . ?
C77 H77B 0.9800 . ?
C77 H77C 0.9800 . ?
N78 N79 1.377(6) . ?
N78 C82 1.395(7) . ?
N79 C80 1.322(7) . ?
C80 C81 1.392(9) . ?
C80 C83 1.495(7) . ?
C81 H81 0.9500 . ?
C81 C82 1.359(8) . ?
C82 C84 1.493(8) . ?
C83 H83A 0.9800 . ?
C83 H83B 0.9800 . ?
C83 H83C 0.9800 . ?
C84 H84A 0.9800 . ?
C84 H84B 0.9800 . ?
C84 H84C 0.9800 . ?
Sb85 F86 1.873(4) . ?
Sb85 F87 1.875(4) . ?
Sb85 F88 1.871(4) . ?
Sb85 F89 1.861(4) . ?
Sb85 F90 1.867(4) . ?
Sb85 F91 1.862(4) . ?
Sb92 F93 1.854(4) . ?
Sb92 F94 1.865(4) . ?
Sb92 F95 1.866(4) . ?
Sb92 F96 1.877(4) . ?
Sb92 F97 1.885(3) . ?
Sb92 F98 1.877(3) . ?
Sb99 F100 1.857(5) . ?
Sb99 F101 1.871(4) . ?
Sb99 F102 1.857(4) . ?
Sb99 F103 1.847(4) . ?
Sb99 F104 1.876(4) . ?
Sb99 F105 1.873(3) . ?
Sb106 F107 1.867(4) . ?
Sb106 F108 1.876(4) . ?
Sb106 F109 1.864(4) . ?
Sb106 F110 1.880(4) . ?
Sb106 F111 1.862(4) . ?
Sb106 F112 1.869(4) . ?
C113 H11A 0.9800 . ?
C113 H11B 0.9800 . ?
C113 H11C 0.9800 . ?
C113 N114 1.470(11) . ?
N114 O115 1.203(9) . ?
N114 O116 1.194(11) . ?

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
N12 Ag1 N7 69.06(16) . . ?
N12 Ag1 N69 142.28(16) . . ?
N12 Ag1 N79 138.91(17) . . ?
N69 Ag1 N7 96.53(14) . . ?
N79 Ag1 N7 148.09(16) . . ?
N79 Ag1 N69 69.06(15) . . ?
N19 Ag2 N9 69.53(17) . . ?
N19 Ag2 N27 135.19(16) . . ?
N19 Ag2 N32 130.46(17) . . ?
N27 Ag2 N9 124.18(15) . . ?
N32 Ag2 N9 140.01(16) . . ?
N32 Ag2 N27 69.84(15) . . ?
N29 Ag3 N47 94.60(15) . . ?
N29 Ag3 F98 80.37(14) . . ?
N39 Ag3 N29 68.05(15) . . ?
N39 Ag3 N47 137.28(16) . . ?
N39 Ag3 F98 87.92(14) . . ?
N47 Ag3 F98 128.88(13) . . ?
N52 Ag3 N29 149.58(15) . . ?
N52 Ag3 N39 141.66(16) . . ?
N52 Ag3 N47 67.09(15) . . ?
N52 Ag3 F98 92.35(14) . . ?
N49 Ag4 N67 134.36(15) . . ?
N59 Ag4 N49 69.86(16) . . ?
N59 Ag4 N67 127.97(16) . . ?
N72 Ag4 N49 142.57(16) . . ?
N72 Ag4 N59 121.81(17) . . ?
N72 Ag4 N67 70.12(15) . . ?
C6 N5 C10 113.8(4) . . ?
N5 C6 N7 126.5(5) . . ?
N5 C6 N11 118.5(4) . . ?
N7 C6 N11 115.0(5) . . ?
C6 N7 Ag1 113.5(4) . . ?
C8 N7 Ag1 128.3(4) . . ?
C8 N7 C6 113.8(5) . . ?
N7 C8 H8 117.1 . . ?
N9 C8 N7 125.8(5) . . ?
N9 C8 H8 117.1 . . ?
C8 N9 Ag2 128.4(3) . . ?
C8 N9 C10 114.8(5) . . ?
C10 N9 Ag2 116.8(4) . . ?
N5 C10 N9 125.1(5) . . ?
N5 C10 N18 118.7(4) . . ?
N9 C10 N18 116.1(5) . . ?
N12 N11 C6 118.3(4) . . ?
N12 N11 C15 111.0(5) . . ?
C15 N11 C6 130.7(5) . . ?
N11 N12 Ag1 121.2(3) . . ?
C13 N12 Ag1 131.2(4) . . ?
C13 N12 N11 106.6(5) . . ?
N12 C13 C14 110.0(5) . . ?
N12 C13 C16 121.1(5) . . ?
C14 C13 C16 128.9(5) . . ?
C13 C14 H14 126.3 . . ?
C15 C14 C13 107.3(5) . . ?
C15 C14 H14 126.3 . . ?
N11 C15 C17 125.7(5) . . ?
C14 C15 N11 105.1(5) . . ?
C14 C15 C17 129.2(5) . . ?
C13 C16 H16A 109.5 . . ?
C13 C16 H16B 109.5 . . ?
C13 C16 H16C 109.5 . . ?
H16A C16 H16B 109.5 . . ?
H16A C16 H16C 109.5 . . ?
H16B C16 H16C 109.5 . . ?
C15 C17 H17A 109.5 . . ?
C15 C17 H17B 109.5 . . ?
C15 C17 H17C 109.5 . . ?
H17A C17 H17B 109.5 . . ?
H17A C17 H17C 109.5 . . ?
H17B C17 H17C 109.5 . . ?
C10 N18 C22 131.9(5) . . ?
N19 N18 C10 117.9(4) . . ?
N19 N18 C22 110.1(5) . . ?
N18 N19 Ag2 118.9(3) . . ?
C20 N19 Ag2 133.5(4) . . ?
C20 N19 N18 106.4(4) . . ?
N19 C20 C21 109.9(5) . . ?
N19 C20 C23 120.1(5) . . ?
C21 C20 C23 130.0(6) . . ?
C20 C21 H21 126.1 . . ?
C22 C21 C20 107.7(5) . . ?
C22 C21 H21 126.1 . . ?
N18 C22 C24 124.8(5) . . ?
C21 C22 N18 105.9(5) . . ?
C21 C22 C24 129.4(5) . . ?
C20 C23 H23A 109.5 . . ?
C20 C23 H23B 109.5 . . ?
C20 C23 H23C 109.5 . . ?
H23A C23 H23B 109.5 . . ?
H23A C23 H23C 109.5 . . ?
H23B C23 H23C 109.5 . . ?
C22 C24 H24A 109.5 . . ?
C22 C24 H24B 109.5 . . ?
C22 C24 H24C 109.5 . . ?
H24A C24 H24B 109.5 . . ?
H24A C24 H24C 109.5 . . ?
H24B C24 H24C 109.5 . . ?
C30 N25 C26 113.2(4) . . ?
N25 C26 N27 125.9(5) . . ?
N25 C26 N31 118.6(4) . . ?
N27 C26 N31 115.4(4) . . ?
C26 N27 Ag2 118.1(3) . . ?
C28 N27 Ag2 126.8(3) . . ?
C28 N27 C26 114.5(4) . . ?
N27 C28 H28 117.2 . . ?
N27 C28 N29 125.6(5) . . ?
N29 C28 H28 117.2 . . ?
C28 N29 Ag3 127.0(3) . . ?
C28 N29 C30 113.7(4) . . ?
C30 N29 Ag3 116.8(3) . . ?
N25 C30 N29 126.8(5) . . ?
N25 C30 N38 118.4(5) . . ?
N29 C30 N38 114.8(4) . . ?
N32 N31 C26 118.2(4) . . ?
N32 N31 C35 110.1(4) . . ?
C35 N31 C26 131.5(4) . . ?
N31 N32 Ag2 117.7(3) . . ?
C33 N32 Ag2 135.8(4) . . ?
C33 N32 N31 106.5(4) . . ?
N32 C33 C34 110.1(4) . . ?
N32 C33 C36 121.1(5) . . ?
C34 C33 C36 128.8(5) . . ?
C33 C34 H34 126.4 . . ?
C35 C34 C33 107.1(5) . . ?
C35 C34 H34 126.4 . . ?
N31 C35 C37 125.5(4) . . ?
C34 C35 N31 106.2(5) . . ?
C34 C35 C37 128.4(5) . . ?
C33 C36 H36A 109.5 . . ?
C33 C36 H36B 109.5 . . ?
C33 C36 H36C 109.5 . . ?
H36A C36 H36B 109.5 . . ?
H36A C36 H36C 109.5 . . ?
H36B C36 H36C 109.5 . . ?
C35 C37 H37A 109.5 . . ?
C35 C37 H37B 109.5 . . ?
C35 C37 H37C 109.5 . . ?
H37A C37 H37B 109.5 . . ?
H37A C37 H37C 109.5 . . ?
H37B C37 H37C 109.5 . . ?
N39 N38 C30 118.0(4) . . ?
N39 N38 C42 110.3(4) . . ?
C42 N38 C30 131.5(4) . . ?
N38 N39 Ag3 120.4(3) . . ?
C40 N39 Ag3 132.7(4) . . ?
C40 N39 N38 106.0(4) . . ?
N39 C40 C41 110.7(5) . . ?
N39 C40 C43 120.6(5) . . ?
C41 C40 C43 128.7(5) . . ?
C40 C41 H41 126.5 . . ?
C42 C41 C40 107.0(5) . . ?
C42 C41 H41 126.5 . . ?
N38 C42 C44 125.4(5) . . ?
C41 C42 N38 105.9(5) . . ?
C41 C42 C44 128.8(5) . . ?
C40 C43 H43A 109.5 . . ?
C40 C43 H43B 109.5 . . ?
C40 C43 H43C 109.5 . . ?
H43A C43 H43B 109.5 . . ?
H43A C43 H43C 109.5 . . ?
H43B C43 H43C 109.5 . . ?
C42 C44 H44A 109.5 . . ?
C42 C44 H44B 109.5 . . ?
C42 C44 H44C 109.5 . . ?
H44A C44 H44B 109.5 . . ?
H44A C44 H44C 109.5 . . ?
H44B C44 H44C 109.5 . . ?
C46 N45 C50 113.3(4) . . ?
N45 C46 N47 126.7(5) . . ?
N45 C46 N51 117.9(4) . . ?
N47 C46 N51 115.4(4) . . ?
C46 N47 Ag3 115.6(3) . . ?
C48 N47 Ag3 131.0(3) . . ?
C48 N47 C46 113.4(5) . . ?
N47 C48 H48 116.6 . . ?
N47 C48 N49 126.8(5) . . ?
N49 C48 H48 116.6 . . ?
C48 N49 Ag4 127.5(3) . . ?
C48 N49 C50 113.6(4) . . ?
C50 N49 Ag4 118.7(3) . . ?
N45 C50 N49 126.1(5) . . ?
N45 C50 N58 117.9(4) . . ?
N49 C50 N58 116.0(4) . . ?
C46 N51 C55 131.4(4) . . ?
N52 N51 C46 118.6(4) . . ?
N52 N51 C55 110.0(4) . . ?
N51 N52 Ag3 122.3(3) . . ?
C53 N52 Ag3 129.9(4) . . ?
C53 N52 N51 106.5(4) . . ?
N52 C53 C54 109.9(5) . . ?
N52 C53 C56 121.9(5) . . ?
C54 C53 C56 128.2(5) . . ?
C53 C54 H54 126.3 . . ?
C55 C54 C53 107.4(5) . . ?
C55 C54 H54 126.3 . . ?
N51 C55 C57 125.5(5) . . ?
C54 C55 N51 106.3(5) . . ?
C54 C55 C57 128.2(5) . . ?
C53 C56 H56A 109.5 . . ?
C53 C56 H56B 109.5 . . ?
C53 C56 H56C 109.5 . . ?
H56A C56 H56B 109.5 . . ?
H56A C56 H56C 109.5 . . ?
H56B C56 H56C 109.5 . . ?
C55 C57 H57A 109.5 . . ?
C55 C57 H57B 109.5 . . ?
C55 C57 H57C 109.5 . . ?
H57A C57 H57B 109.5 . . ?
H57A C57 H57C 109.5 . . ?
H57B C57 H57C 109.5 . . ?
C50 N58 C62 132.5(4) . . ?
N59 N58 C50 117.5(4) . . ?
N59 N58 C62 110.0(4) . . ?
N58 N59 Ag4 117.5(3) . . ?
C60 N59 Ag4 136.0(4) . . ?
C60 N59 N58 106.6(5) . . ?
N59 C60 C61 110.1(5) . . ?
N59 C60 C63 120.7(6) . . ?
C61 C60 C63 129.2(6) . . ?
C60 C61 H61 126.2 . . ?
C62 C61 C60 107.5(5) . . ?
C62 C61 H61 126.2 . . ?
N58 C62 C64 125.8(5) . . ?
C61 C62 N58 105.9(5) . . ?
C61 C62 C64 128.3(5) . . ?
C60 C63 H63A 109.5 . . ?
C60 C63 H63B 109.5 . . ?
C60 C63 H63C 109.5 . . ?
H63A C63 H63B 109.5 . . ?
H63A C63 H63C 109.5 . . ?
H63B C63 H63C 109.5 . . ?
C62 C64 H64A 109.5 . . ?
C62 C64 H64B 109.5 . . ?
C62 C64 H64C 109.5 . . ?
H64A C64 H64B 109.5 . . ?
H64A C64 H64C 109.5 . . ?
H64B C64 H64C 109.5 . . ?
C70 N65 C66 113.9(4) . . ?
N65 C66 N71 118.8(4) . . ?
N67 C66 N65 125.2(4) . . ?
N67 C66 N71 116.0(4) . . ?
C66 N67 Ag4 118.0(3) . . ?
C68 N67 Ag4 127.5(4) . . ?
C68 N67 C66 114.3(4) . . ?
N67 C68 H68 116.7 . . ?
N69 C68 N67 126.6(5) . . ?
N69 C68 H68 116.7 . . ?
C68 N69 Ag1 130.2(4) . . ?
C68 N69 C70 113.2(4) . . ?
C70 N69 Ag1 116.4(3) . . ?
N65 C70 N69 126.7(5) . . ?
N65 C70 N78 118.9(4) . . ?
N69 C70 N78 114.4(4) . . ?
C66 N71 N72 118.0(4) . . ?
C66 N71 C75 131.9(4) . . ?
C75 N71 N72 109.9(4) . . ?
N71 N72 Ag4 117.7(3) . . ?
C73 N72 Ag4 136.5(4) . . ?
C73 N72 N71 105.6(4) . . ?
N72 C73 C74 111.1(5) . . ?
N72 C73 C76 120.1(5) . . ?
C74 C73 C76 128.8(5) . . ?
C73 C74 H74 126.3 . . ?
C75 C74 C73 107.4(5) . . ?
C75 C74 H74 126.3 . . ?
N71 C75 C77 125.4(5) . . ?
C74 C75 N71 106.0(5) . . ?
C74 C75 C77 128.5(5) . . ?
C73 C76 H76A 109.5 . . ?
C73 C76 H76B 109.5 . . ?
C73 C76 H76C 109.5 . . ?
H76A C76 H76B 109.5 . . ?
H76A C76 H76C 109.5 . . ?
H76B C76 H76C 109.5 . . ?
C75 C77 H77A 109.5 . . ?
C75 C77 H77B 109.5 . . ?
C75 C77 H77C 109.5 . . ?
H77A C77 H77B 109.5 . . ?
H77A C77 H77C 109.5 . . ?
H77B C77 H77C 109.5 . . ?
N79 N78 C70 119.1(4) . . ?
N79 N78 C82 109.7(4) . . ?
C82 N78 C70 131.0(4) . . ?
N78 N79 Ag1 120.9(3) . . ?
C80 N79 Ag1 132.5(4) . . ?
C80 N79 N78 106.2(4) . . ?
N79 C80 C81 110.8(5) . . ?
N79 C80 C83 120.9(6) . . ?
C81 C80 C83 128.4(6) . . ?
C80 C81 H81 126.3 . . ?
C82 C81 C80 107.3(5) . . ?
C82 C81 H81 126.3 . . ?
N78 C82 C84 125.7(5) . . ?
C81 C82 N78 106.0(5) . . ?
C81 C82 C84 128.3(5) . . ?
C80 C83 H83A 109.5 . . ?
C80 C83 H83B 109.5 . . ?
C80 C83 H83C 109.5 . . ?
H83A C83 H83B 109.5 . . ?
H83A C83 H83C 109.5 . . ?
H83B C83 H83C 109.5 . . ?
C82 C84 H84A 109.5 . . ?
C82 C84 H84B 109.5 . . ?
C82 C84 H84C 109.5 . . ?
H84A C84 H84B 109.5 . . ?
H84A C84 H84C 109.5 . . ?
H84B C84 H84C 109.5 . . ?
F86 Sb85 F87 90.7(2) . . ?
F88 Sb85 F86 89.4(2) . . ?
F88 Sb85 F87 179.3(2) . . ?
F89 Sb85 F86 90.3(2) . . ?
F89 Sb85 F87 90.6(2) . . ?
F89 Sb85 F88 90.08(19) . . ?
F89 Sb85 F90 179.1(2) . . ?
F89 Sb85 F91 91.1(2) . . ?
F90 Sb85 F86 88.9(2) . . ?
F90 Sb85 F87 89.7(2) . . ?
F90 Sb85 F88 89.6(2) . . ?
F91 Sb85 F86 178.6(2) . . ?
F91 Sb85 F87 89.5(2) . . ?
F91 Sb85 F88 90.3(2) . . ?
F91 Sb85 F90 89.7(2) . . ?
F93 Sb92 F94 90.0(2) . . ?
F93 Sb92 F95 179.9(3) . . ?
F93 Sb92 F96 90.0(2) . . ?
F93 Sb92 F97 90.07(19) . . ?
F93 Sb92 F98 90.2(2) . . ?
F94 Sb92 F95 90.0(2) . . ?
F94 Sb92 F96 179.32(19) . . ?
F94 Sb92 F97 89.83(17) . . ?
F94 Sb92 F98 90.36(17) . . ?
F95 Sb92 F96 90.0(2) . . ?
F95 Sb92 F97 90.1(2) . . ?
F95 Sb92 F98 89.6(2) . . ?
F96 Sb92 F97 89.49(18) . . ?
F96 Sb92 F98 90.32(18) . . ?
F98 Sb92 F97 179.6(2) . . ?
Sb92 F98 Ag3 142.3(2) . . ?
F100 Sb99 F101 88.4(2) . . ?
F100 Sb99 F104 89.9(2) . . ?
F100 Sb99 F105 89.93(19) . . ?
F101 Sb99 F104 88.7(2) . . ?
F101 Sb99 F105 88.63(17) . . ?
F102 Sb99 F100 178.5(2) . . ?
F102 Sb99 F101 90.3(2) . . ?
F102 Sb99 F104 91.0(2) . . ?
F102 Sb99 F105 89.16(19) . . ?
F103 Sb99 F100 90.5(2) . . ?
F103 Sb99 F101 178.7(2) . . ?
F103 Sb99 F102 90.8(2) . . ?
F103 Sb99 F104 90.6(2) . . ?
F103 Sb99 F105 92.0(2) . . ?
F105 Sb99 F104 177.4(2) . . ?
F107 Sb106 F108 88.3(2) . . ?
F107 Sb106 F110 90.5(2) . . ?
F107 Sb106 F112 90.9(2) . . ?
F108 Sb106 F110 89.40(19) . . ?
F109 Sb106 F107 89.0(3) . . ?
F109 Sb106 F108 92.3(2) . . ?
F109 Sb106 F110 178.2(2) . . ?
F109 Sb106 F112 88.8(2) . . ?
F111 Sb106 F107 178.8(2) . . ?
F111 Sb106 F108 90.55(19) . . ?
F111 Sb106 F109 91.5(2) . . ?
F111 Sb106 F110 89.06(19) . . ?
F111 Sb106 F112 90.24(18) . . ?
F112 Sb106 F108 178.6(2) . . ?
F112 Sb106 F110 89.5(2) . . ?
H11A C113 H11B 109.5 . . ?
H11A C113 H11C 109.5 . . ?
H11B C113 H11C 109.5 . . ?
N114 C113 H11A 109.5 . . ?
N114 C113 H11B 109.5 . . ?
N114 C113 H11C 109.5 . . ?
O115 N114 C113 119.7(7) . . ?
O116 N114 C113 116.4(8) . . ?
O116 N114 O115 123.7(9) . . ?

_exptl_crystal_recrystallization_method 
'Re-crystallisation from solvent: nitromethane/diethyl ether'
####################################################################### 
# 
# 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_150-ncse
_database_code_depnum_ccdc_archive 'CCDC 1957585'
loop_
_audit_author_name
_audit_author_address
'Malcolm Halcrow' 'University of Leeds'
_audit_update_record             
;
2019-10-04 deposited with the CCDC.	2019-11-05 downloaded from the CCDC.
;
_audit_creation_date             2019-07-05
_audit_creation_method           
;
  Olex2 1.2
  (compiled Apr 23 2013 17:54:37, GUI svn.r4466)
;
_chemical_name_common            ?
_chemical_name_systematic        
'Bis-[4,6-di(pyrazol-1-yl)pyrimidine]-di[isoselenocyanato]iron(II)methanol solvate'
_chemical_formula_moiety         'C22 H16 Fe N14 Se2, C H4 O'
_chemical_formula_sum            'C23 H20 Fe N14 O Se2'
_chemical_formula_weight         722.30
_chemical_melting_point          ?
loop_
_atom_type_symbol
_atom_type_description
_atom_type_scat_dispersion_real
_atom_type_scat_dispersion_imag
_atom_type_scat_source
C C 0.0181 0.0091 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
N N 0.0311 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'
Se Se -0.7943 1.1372 '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'

_space_group_crystal_system      monoclinic
_space_group_IT_number           14
_space_group_name_H-M_alt        'P 1 21/n 1'
_space_group_name_Hall           '-P 2yn'
loop_
_space_group_symop_id
_space_group_symop_operation_xyz
1 'x, y, z'
2 '-x+1/2, y+1/2, -z+1/2'
3 '-x, -y, -z'
4 'x-1/2, -y-1/2, z-1/2'

_cell_length_a                   12.9026(2)
_cell_length_b                   14.5475(2)
_cell_length_c                   16.1511(2)
_cell_angle_alpha                90.00
_cell_angle_beta                 109.427(2)
_cell_angle_gamma                90.00
_cell_volume                     2858.97(7)
_cell_formula_units_Z            4
_cell_measurement_reflns_used    7979
_cell_measurement_temperature    120(2)
_cell_measurement_theta_min      4.21
_cell_measurement_theta_max      73.55
_exptl_absorpt_coefficient_mu    7.528
_exptl_absorpt_correction_T_min  0.503
_exptl_absorpt_correction_T_max  1.000
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   
; 
CrysAlisPro, Agilent Technologies,
Version 1.171.36.24 (release 03-12-2012 CrysAlis171 .NET)
Empirical absorption correction using spherical harmonics,
 implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_crystal_colour            yellow
_exptl_crystal_density_diffrn    1.678
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       plate
_exptl_crystal_F_000             1432
_exptl_crystal_size_max          0.40
_exptl_crystal_size_mid          0.20
_exptl_crystal_size_min          0.08
_exptl_special_details           
;
 ? 
;
_diffrn_reflns_av_R_equivalents  0.0253
_diffrn_reflns_av_unetI/netI     0.0281
_diffrn_reflns_limit_h_max       8
_diffrn_reflns_limit_h_min       -16
_diffrn_reflns_limit_k_max       15
_diffrn_reflns_limit_k_min       -17
_diffrn_reflns_limit_l_max       19
_diffrn_reflns_limit_l_min       -16
_diffrn_reflns_number            14817
_diffrn_reflns_theta_full        72.00
_diffrn_reflns_theta_max         73.71
_diffrn_reflns_theta_min         3.82
_diffrn_ambient_temperature      120(2)
_diffrn_detector_area_resol_mean 5.3095
_diffrn_measured_fraction_theta_full 0.973
_diffrn_measured_fraction_theta_max 0.959
_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                5063
_reflns_number_total             5531
_reflns_threshold_expression     >2sigma(I)
_computing_cell_refinement       'CrysAlisPro, Agilent Technologies'
_computing_data_collection       '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         0.587
_refine_diff_density_min         -0.415
_refine_diff_density_rms         0.064
_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     383
_refine_ls_number_reflns         5531
_refine_ls_number_restraints     1
_refine_ls_R_factor_all          0.0341
_refine_ls_R_factor_gt           0.0300
_refine_ls_restrained_S_all      1.051
_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)+(0.0420P)²+1.3464P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0760
_refine_ls_wR_factor_ref         0.0788
_refine_special_details          
;
 Refinement of F² against ALL reflections.  The weighted R-factor wR and 
 goodness of fit S are based on F², conventional R-factors R are based 
 on F, with F set to zero for negative F². The threshold expression of 
 F² > 2sigma(F²) is used only for calculating R-factors(gt) etc. and is 
 not relevant to the choice of reflections for refinement.  R-factors based 
 on F² are statistically about twice as large as those based on F, and R- 
 factors based on ALL data will be even larger. 

 No disorder is present in the model and no restraints are included in the
 refinement. All non-H atoms were refined anisotropically and C-bound H 
 atoms were placed in calculated positions and refined using a riding model.
 The methanol hydroxyl H atom was located in the Fourier map and refined,
 subject to the restraint O---H = 0.90(2) /%A and the constrain Uiso =
 1.5x Ueq{O}.
;
_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, All O(H) groups
2. Restrained distances
 O41-H41
 0.9 with sigma of 0.02
3. Others
 Fixed Sof: Se7A(0.57) Se7B(0.43)
4.a Aromatic/amide H refined with riding coordinates:
 C8(H8), C11(H11), C16(H16), C17(H17), C18(H18), C21(H21), C22(H22), C23(H23),
 C24(H24), C27(H27), C32(H32), C33(H33), C34(H34), C37(H37), C38(H38), C39(H39)
4.b Idealised Me refined as rotating group:
 C40(H40A,H40B,H40C)
;
_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 0.41172(3) 0.74855(2) 0.73556(2) 0.02176(9) Uani 1 1 d . . .
N2 N 0.54911(16) 0.66425(14) 0.79454(13) 0.0302(4) Uani 1 1 d . . .
C3 C 0.61487(18) 0.61925(16) 0.84402(14) 0.0259(4) Uani 1 1 d . . .
Se4 Se 0.71280(2) 0.548876(18) 0.924015(16) 0.03305(8) Uani 1 1 d . . .
N5 N 0.31279(18) 0.64137(15) 0.67314(14) 0.0339(4) Uani 1 1 d . A .
C6 C 0.2360(2) 0.60028(17) 0.63366(15) 0.0296(5) Uani 1 1 d . . .
Se7A Se 0.1228(3) 0.5316(2) 0.5721(3) 0.0434(6) Uani 0.57 1 d P A 1
Se7B Se 0.1090(4) 0.5448(3) 0.5747(4) 0.0540(9) Uani 0.43 1 d P A 2
C8 C 0.42532(19) 0.70921(18) 0.93391(15) 0.0310(5) Uani 1 1 d . . .
H8 H 0.4880 0.6741 0.9354 0.037 Uiso 1 1 calc R . .
N9 N 0.37468(16) 0.75532(13) 0.85931(12) 0.0266(4) Uani 1 1 d . . .
C10 C 0.28741(18) 0.80539(16) 0.85887(14) 0.0253(4) Uani 1 1 d . . .
C11 C 0.25173(19) 0.81191(16) 0.93045(15) 0.0282(5) Uani 1 1 d . . .
H11 H 0.1913 0.8494 0.9303 0.034 Uiso 1 1 calc R . .
C12 C 0.31040(19) 0.75994(16) 1.00215(15) 0.0257(4) Uani 1 1 d . . .
N13 N 0.39702(16) 0.70761(15) 1.00549(13) 0.0303(4) Uani 1 1 d . . .
N14 N 0.23179(16) 0.84920(14) 0.77932(12) 0.0272(4) Uani 1 1 d . . .
N15 N 0.26768(15) 0.83632(14) 0.70937(12) 0.0259(4) Uani 1 1 d . . .
C16 C 0.19513(19) 0.87937(17) 0.64333(15) 0.0304(5) Uani 1 1 d . . .
H16 H 0.1986 0.8823 0.5856 0.036 Uiso 1 1 calc R . .
C17 C 0.1118(2) 0.92044(18) 0.66930(17) 0.0358(5) Uani 1 1 d . . .
H17 H 0.0507 0.9550 0.6339 0.043 Uiso 1 1 calc R . .
C18 C 0.1378(2) 0.89993(18) 0.75596(17) 0.0346(5) Uani 1 1 d . . .
H18 H 0.0978 0.9177 0.7933 0.041 Uiso 1 1 calc R . .
N19 N 0.28027(16) 0.75814(13) 1.07791(12) 0.0268(4) Uani 1 1 d . . .
N20 N 0.20379(17) 0.81811(14) 1.08665(14) 0.0317(4) Uani 1 1 d . . .
C21 C 0.1968(2) 0.79758(18) 1.16468(16) 0.0354(6) Uani 1 1 d . . .
H21 H 0.1500 0.8287 1.1900 0.043 Uiso 1 1 calc R . .
C22 C 0.2661(2) 0.72500(19) 1.20549(15) 0.0341(5) Uani 1 1 d . . .
H22 H 0.2746 0.6984 1.2611 0.041 Uiso 1 1 calc R . .
C23 C 0.31892(19) 0.70051(18) 1.14838(15) 0.0315(5) Uani 1 1 d . . .
H23 H 0.3718 0.6530 1.1560 0.038 Uiso 1 1 calc R . .
C24 C 0.41211(19) 0.74442(15) 0.53642(15) 0.0254(4) Uani 1 1 d . . .
H24 H 0.3617 0.6953 0.5306 0.030 Uiso 1 1 calc R . .
N25 N 0.44339(14) 0.79000(13) 0.61304(11) 0.0217(3) Uani 1 1 d . . .
C26 C 0.51126(16) 0.86098(14) 0.61861(13) 0.0207(4) Uani 1 1 d . . .
C27 C 0.54726(17) 0.88840(15) 0.55083(13) 0.0221(4) Uani 1 1 d . . .
H27 H 0.5925 0.9409 0.5548 0.026 Uiso 1 1 calc R . .
C28 C 0.51208(17) 0.83312(15) 0.47623(13) 0.0214(4) Uani 1 1 d . . .
N29 N 0.44450(16) 0.76112(13) 0.46797(12) 0.0256(4) Uani 1 1 d . . .
N30 N 0.54797(14) 0.90443(12) 0.70042(11) 0.0212(3) Uani 1 1 d . . .
N31 N 0.51575(15) 0.86960(13) 0.76683(12) 0.0249(4) Uani 1 1 d . . .
C32 C 0.5687(2) 0.91919(17) 0.83676(15) 0.0296(5) Uani 1 1 d . . .
H32 H 0.5626 0.9107 0.8933 0.036 Uiso 1 1 calc R . .
C33 C 0.6352(2) 0.98605(18) 0.81664(16) 0.0323(5) Uani 1 1 d . . .
H33 H 0.6810 1.0298 0.8556 0.039 Uiso 1 1 calc R . .
C34 C 0.62048(19) 0.97523(16) 0.72966(15) 0.0280(5) Uani 1 1 d . . .
H34 H 0.6541 1.0102 0.6959 0.034 Uiso 1 1 calc R . .
N35 N 0.54813(15) 0.85055(13) 0.40557(11) 0.0239(4) Uani 1 1 d . . .
N36 N 0.62133(17) 0.91987(14) 0.40968(13) 0.0308(4) Uani 1 1 d . . .
C37 C 0.6373(2) 0.91553(18) 0.33320(16) 0.0348(5) Uani 1 1 d . . .
H37 H 0.6848 0.9559 0.3166 0.042 Uiso 1 1 calc R . .
C38 C 0.5767(2) 0.84498(19) 0.27888(15) 0.0340(5) Uani 1 1 d . . .
H38 H 0.5751 0.8292 0.2214 0.041 Uiso 1 1 calc R . .
C39 C 0.5206(2) 0.80439(17) 0.32732(14) 0.0306(5) Uani 1 1 d . . .
H39 H 0.4717 0.7537 0.3100 0.037 Uiso 1 1 calc R . .
C40 C 0.4457(4) 0.5129(3) 0.3753(3) 0.0777(12) Uani 1 1 d . . .
H40A H 0.4968 0.4620 0.3793 0.117 Uiso 1 1 calc R . .
H40B H 0.3886 0.5125 0.3174 0.117 Uiso 1 1 calc R . .
H40C H 0.4116 0.5060 0.4209 0.117 Uiso 1 1 calc R . .
O41 O 0.4993(3) 0.5908(2) 0.3866(2) 0.0914(12) Uani 1 1 d D . .
H41 H 0.480(5) 0.636(3) 0.420(4) 0.137 Uiso 1 1 d D . .


_geom_special_details            
;
 All esds (except the esd in the dihedral angle between two l.s. planes) 
 are estimated using the full covariance matrix.  The cell esds are taken 
 into account individually in the estimation of esds in distances, angles 
 and torsion angles; correlations between esds in cell parameters are only 
 used when they are defined by crystal symmetry.  An approximate (isotropic) 
 treatment of cell esds is used for estimating esds involving l.s. planes. 
;
loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
_geom_bond_publ_flag
Fe1 N2 2.105(2) . ?
Fe1 N5 2.055(2) . ?
Fe1 N9 2.2064(19) . ?
Fe1 N15 2.1772(19) . ?
Fe1 N25 2.2325(17) . ?
Fe1 N31 2.1695(19) . ?
N2 C3 1.156(3) . ?
C3 Se4 1.797(2) . ?
N5 C6 1.151(3) . ?
C6 Se7A 1.776(5) . ?
C6 Se7B 1.790(6) . ?
C8 H8 0.9500 . ?
C8 N9 1.343(3) . ?
C8 N13 1.323(3) . ?
N9 C10 1.339(3) . ?
C10 C11 1.383(3) . ?
C10 N14 1.399(3) . ?
C11 H11 0.9500 . ?
C11 C12 1.379(3) . ?
C12 N13 1.338(3) . ?
C12 N19 1.402(3) . ?
N14 N15 1.369(3) . ?
N14 C18 1.361(3) . ?
N15 C16 1.320(3) . ?
C16 H16 0.9500 . ?
C16 C17 1.410(4) . ?
C17 H17 0.9500 . ?
C17 C18 1.360(4) . ?
C18 H18 0.9500 . ?
N19 N20 1.359(3) . ?
N19 C23 1.367(3) . ?
N20 C21 1.327(3) . ?
C21 H21 0.9500 . ?
C21 C22 1.399(4) . ?
C22 H22 0.9500 . ?
C22 C23 1.364(4) . ?
C23 H23 0.9500 . ?
C24 H24 0.9500 . ?
C24 N25 1.342(3) . ?
C24 N29 1.328(3) . ?
N25 C26 1.337(3) . ?
C26 C27 1.383(3) . ?
C26 N30 1.398(3) . ?
C27 H27 0.9500 . ?
C27 C28 1.393(3) . ?
C28 N29 1.341(3) . ?
C28 N35 1.391(3) . ?
N30 N31 1.370(3) . ?
N30 C34 1.366(3) . ?
N31 C32 1.323(3) . ?
C32 H32 0.9500 . ?
C32 C33 1.405(4) . ?
C33 H33 0.9500 . ?
C33 C34 1.363(3) . ?
C34 H34 0.9500 . ?
N35 N36 1.368(3) . ?
N35 C39 1.370(3) . ?
N36 C37 1.319(3) . ?
C37 H37 0.9500 . ?
C37 C38 1.407(4) . ?
C38 H38 0.9500 . ?
C38 C39 1.364(3) . ?
C39 H39 0.9500 . ?
C40 H40A 0.9800 . ?
C40 H40B 0.9800 . ?
C40 H40C 0.9800 . ?
C40 O41 1.308(5) . ?
O41 H41 0.93(2) . ?

loop_
_geom_angle_atom_site_label_1
_geom_angle_atom_site_label_2
_geom_angle_atom_site_label_3
_geom_angle
_geom_angle_site_symmetry_1
_geom_angle_site_symmetry_3
_geom_angle_publ_flag
N2 Fe1 N9 91.12(7) . . ?
N2 Fe1 N15 164.92(7) . . ?
N2 Fe1 N25 100.58(7) . . ?
N2 Fe1 N31 90.28(8) . . ?
N5 Fe1 N2 94.14(9) . . ?
N5 Fe1 N9 101.07(8) . . ?
N5 Fe1 N15 89.93(8) . . ?
N5 Fe1 N25 92.12(7) . . ?
N5 Fe1 N31 164.92(8) . . ?
N9 Fe1 N25 161.72(7) . . ?
N15 Fe1 N9 73.85(7) . . ?
N15 Fe1 N25 93.75(7) . . ?
N31 Fe1 N9 93.24(7) . . ?
N31 Fe1 N15 89.50(7) . . ?
N31 Fe1 N25 72.88(7) . . ?
C3 N2 Fe1 163.12(17) . . ?
N2 C3 Se4 177.25(19) . . ?
C6 N5 Fe1 161.0(2) . . ?
N5 C6 Se7A 176.6(3) . . ?
N5 C6 Se7B 174.6(3) . . ?
N9 C8 H8 116.6 . . ?
N13 C8 H8 116.6 . . ?
N13 C8 N9 126.8(2) . . ?
C8 N9 Fe1 127.07(16) . . ?
C10 N9 Fe1 117.03(15) . . ?
C10 N9 C8 115.70(19) . . ?
N9 C10 C11 123.1(2) . . ?
N9 C10 N14 115.22(19) . . ?
C11 C10 N14 121.7(2) . . ?
C10 C11 H11 122.5 . . ?
C12 C11 C10 115.0(2) . . ?
C12 C11 H11 122.5 . . ?
C11 C12 N19 120.6(2) . . ?
N13 C12 C11 124.3(2) . . ?
N13 C12 N19 115.1(2) . . ?
C8 N13 C12 115.1(2) . . ?
N15 N14 C10 118.98(18) . . ?
C18 N14 C10 129.7(2) . . ?
C18 N14 N15 111.10(19) . . ?
N14 N15 Fe1 114.90(13) . . ?
C16 N15 Fe1 139.94(16) . . ?
C16 N15 N14 104.98(18) . . ?
N15 C16 H16 124.2 . . ?
N15 C16 C17 111.5(2) . . ?
C17 C16 H16 124.2 . . ?
C16 C17 H17 127.4 . . ?
C18 C17 C16 105.2(2) . . ?
C18 C17 H17 127.4 . . ?
N14 C18 H18 126.4 . . ?
C17 C18 N14 107.2(2) . . ?
C17 C18 H18 126.4 . . ?
N20 N19 C12 120.0(2) . . ?
N20 N19 C23 112.55(19) . . ?
C23 N19 C12 127.4(2) . . ?
C21 N20 N19 103.6(2) . . ?
N20 C21 H21 123.7 . . ?
N20 C21 C22 112.5(2) . . ?
C22 C21 H21 123.7 . . ?
C21 C22 H22 127.4 . . ?
C23 C22 C21 105.3(2) . . ?
C23 C22 H22 127.4 . . ?
N19 C23 H23 127.0 . . ?
C22 C23 N19 106.1(2) . . ?
C22 C23 H23 127.0 . . ?
N25 C24 H24 116.7 . . ?
N29 C24 H24 116.7 . . ?
N29 C24 N25 126.6(2) . . ?
C24 N25 Fe1 126.60(15) . . ?
C26 N25 Fe1 117.23(13) . . ?
C26 N25 C24 115.65(18) . . ?
N25 C26 C27 123.66(19) . . ?
N25 C26 N30 114.91(18) . . ?
C27 C26 N30 121.38(19) . . ?
C26 C27 H27 122.6 . . ?
C26 C27 C28 114.81(19) . . ?
C28 C27 H27 122.6 . . ?
N29 C28 C27 123.44(19) . . ?
N29 C28 N35 116.39(18) . . ?
N35 C28 C27 120.17(19) . . ?
C24 N29 C28 115.74(18) . . ?
N31 N30 C26 118.51(17) . . ?
C34 N30 C26 130.22(18) . . ?
C34 N30 N31 111.08(17) . . ?
N30 N31 Fe1 116.32(13) . . ?
C32 N31 Fe1 138.19(16) . . ?
C32 N31 N30 105.17(18) . . ?
N31 C32 H32 124.4 . . ?
N31 C32 C33 111.2(2) . . ?
C33 C32 H32 124.4 . . ?
C32 C33 H33 127.1 . . ?
C34 C33 C32 105.8(2) . . ?
C34 C33 H33 127.1 . . ?
N30 C34 H34 126.6 . . ?
C33 C34 N30 106.8(2) . . ?
C33 C34 H34 126.6 . . ?
N36 N35 C28 120.55(18) . . ?
N36 N35 C39 111.65(18) . . ?
C39 N35 C28 127.79(19) . . ?
C37 N36 N35 103.86(19) . . ?
N36 C37 H37 123.5 . . ?
N36 C37 C38 113.0(2) . . ?
C38 C37 H37 123.5 . . ?
C37 C38 H38 127.8 . . ?
C39 C38 C37 104.4(2) . . ?
C39 C38 H38 127.8 . . ?
N35 C39 H39 126.5 . . ?
C38 C39 N35 107.0(2) . . ?
C38 C39 H39 126.5 . . ?
H40A C40 H40B 109.5 . . ?
H40A C40 H40C 109.5 . . ?
H40B C40 H40C 109.5 . . ?
O41 C40 H40A 109.5 . . ?
O41 C40 H40B 109.5 . . ?
O41 C40 H40C 109.5 . . ?
C40 O41 H41 117(4) . . ?

loop_
_geom_hbond_atom_site_label_D
_geom_hbond_atom_site_label_H
_geom_hbond_atom_site_label_A
_geom_hbond_distance_DH
_geom_hbond_distance_HA
_geom_hbond_distance_DA
_geom_hbond_angle_DHA
_geom_hbond_site_symmetry_A
O41 H41 N29 0.93(2) 2.09(3) 2.998(3) 164(5) .

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

data_icb-90l
_database_code_depnum_ccdc_archive 'CCDC 1957575'
loop_
_audit_author_name
_audit_author_address
'Malcolm Halcrow' 'University of Leeds'
_audit_update_record             
;
2019-10-04 deposited with the CCDC.	2019-11-05 downloaded from the CCDC.
;
_audit_creation_date             2018-06-05
_audit_creation_method           
;
  Olex2 1.2
  (compiled Apr 23 2013 17:54:37, GUI svn.r4466)
;
_chemical_name_common            ?
_chemical_name_systematic        
;
2-Amino-4,6-(pyrazol-1-yl)pyrimidine
;
_chemical_formula_moiety         'C10 H9 N7'
_chemical_formula_sum            'C10 H9 N7'
_chemical_formula_weight         227.24
_chemical_melting_point          ?
loop_
_atom_type_symbol
_atom_type_description
_atom_type_scat_dispersion_real
_atom_type_scat_dispersion_imag
_atom_type_scat_source
C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'

_space_group_crystal_system      monoclinic
_space_group_IT_number           15
_space_group_name_H-M_alt        'C 1 2/c 1'
_space_group_name_Hall           '-C 2yc'
loop_
_space_group_symop_id
_space_group_symop_operation_xyz
1 'x, y, z'
2 '-x, y, -z+1/2'
3 'x+1/2, y+1/2, z'
4 '-x+1/2, y+1/2, -z+1/2'
5 '-x, -y, -z'
6 'x, -y, z-1/2'
7 '-x+1/2, -y+1/2, -z'
8 'x+1/2, -y+1/2, z-1/2'

_cell_length_a                   17.0960(11)
_cell_length_b                   10.5273(4)
_cell_length_c                   13.4500(6)
_cell_angle_alpha                90.00
_cell_angle_beta                 121.235(4)
_cell_angle_gamma                90.00
_cell_volume                     2069.78(18)
_cell_formula_units_Z            8
_cell_measurement_reflns_used    3135
_cell_measurement_temperature    120(2)
_cell_measurement_theta_min      4.25
_cell_measurement_theta_max      29.44
_exptl_absorpt_coefficient_mu    0.100
_exptl_absorpt_correction_T_min  0.818
_exptl_absorpt_correction_T_max  1.000
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   
; 
CrysAlisPro, Agilent Technologies,
Version 1.171.36.24 (release 03-12-2012 CrysAlis171 .NET)
Empirical absorption correction using spherical harmonics,
 implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_crystal_colour            colourless
_exptl_crystal_density_diffrn    1.458
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       lath
_exptl_crystal_F_000             944
_exptl_crystal_size_max          0.30
_exptl_crystal_size_mid          0.25
_exptl_crystal_size_min          0.10
_exptl_special_details           
;
 ? 
;
_diffrn_reflns_av_R_equivalents  0.0188
_diffrn_reflns_av_unetI/netI     0.0272
_diffrn_reflns_limit_h_max       17
_diffrn_reflns_limit_h_min       -21
_diffrn_reflns_limit_k_max       10
_diffrn_reflns_limit_k_min       -14
_diffrn_reflns_limit_l_max       18
_diffrn_reflns_limit_l_min       -16
_diffrn_reflns_number            5264
_diffrn_reflns_theta_full        26.00
_diffrn_reflns_theta_max         29.61
_diffrn_reflns_theta_min         3.37
_diffrn_ambient_temperature      120(2)
_diffrn_detector_area_resol_mean 5.3095
_diffrn_measured_fraction_theta_full 0.988
_diffrn_measured_fraction_theta_max 0.847
_diffrn_measurement_device_type  'SuperNova, Dual, Cu at zero, Atlas'
_diffrn_measurement_method       'ω scans'
_diffrn_radiation_monochromator  mirror
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_radiation_source         'SuperNova (Mo) X-ray Source'
_diffrn_standards_number         0
_diffrn_standards_interval_count 0
_diffrn_standards_interval_time  0
_diffrn_standards_decay_%        0
_reflns_number_gt                2192
_reflns_number_total             2471
_reflns_threshold_expression     >2sigma(I)
_computing_cell_refinement       'CrysAlisPro, Agilent Technologies'
_computing_data_collection       '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         0.311
_refine_diff_density_min         -0.224
_refine_diff_density_rms         0.042
_refine_ls_extinction_coef       ?
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.099
_refine_ls_hydrogen_treatment    refxyz
_refine_ls_matrix_type           full
_refine_ls_number_parameters     181
_refine_ls_number_reflns         2471
_refine_ls_number_restraints     0
_refine_ls_R_factor_all          0.0455
_refine_ls_R_factor_gt           0.0403
_refine_ls_restrained_S_all      1.099
_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)+(0.0430P)²+1.8029P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1024
_refine_ls_wR_factor_ref         0.1061
_refine_special_details          
;
 Refinement of F² against ALL reflections.  The weighted R-factor wR and 
 goodness of fit S are based on F², conventional R-factors R are based 
 on F, with F set to zero for negative F². The threshold expression of 
 F² > 2sigma(F²) is used only for calculating R-factors(gt) etc. and is 
 not relevant to the choice of reflections for refinement.  R-factors based 
 on F² are statistically about twice as large as those based on F, and R- 
 factors based on ALL data will be even larger. 

 No disorder is present in the model, and no restraints were applied to the
 refinement. All non-H atoms were refined anisotropically. The H atoms were 
 all located in the Fourier map and allowed to refine, with Uiso constrained 
 to 1.2x Ueq for the corresponding C atom, or 1.5x Ueq(N) for the amino
 H atoms. 
;
_olex2_refinement_description    
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups
 At 1.5 times of:
  All N(H,H) groups
;
_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
C1 C 0.12996(8) 0.36326(12) 0.41730(10) 0.0173(3) Uani 1 1 d . . .
N2 N 0.05397(7) 0.32849(10) 0.41806(9) 0.0166(2) Uani 1 1 d . . .
C3 C 0.05570(8) 0.35375(11) 0.51615(10) 0.0157(2) Uani 1 1 d . . .
C4 C 0.12853(8) 0.40971(12) 0.61363(10) 0.0173(3) Uani 1 1 d . . .
H4 H 0.1268(10) 0.4271(15) 0.6822(13) 0.021 Uiso 1 1 d . . .
C5 C 0.20319(8) 0.43453(11) 0.60252(10) 0.0168(3) Uani 1 1 d . . .
N6 N 0.20707(7) 0.41253(10) 0.50799(9) 0.0176(2) Uani 1 1 d . . .
N7 N -0.02195(7) 0.31669(10) 0.51960(9) 0.0163(2) Uani 1 1 d . . .
N8 N -0.02876(7) 0.35094(10) 0.61276(9) 0.0195(2) Uani 1 1 d . . .
C9 C -0.10559(9) 0.29694(13) 0.59232(12) 0.0214(3) Uani 1 1 d . . .
H9 H -0.1254(11) 0.3065(15) 0.6498(14) 0.026 Uiso 1 1 d . . .
C10 C -0.14834(9) 0.22720(13) 0.48779(12) 0.0225(3) Uani 1 1 d . . .
H10 H -0.2045(11) 0.1775(16) 0.4540(14) 0.027 Uiso 1 1 d . . .
C11 C -0.09337(8) 0.24159(12) 0.44305(11) 0.0189(3) Uani 1 1 d . . .
H11 H -0.0967(10) 0.2119(15) 0.3731(14) 0.023 Uiso 1 1 d . . .
N12 N 0.28335(7) 0.48648(10) 0.69727(9) 0.0177(2) Uani 1 1 d . . .
N13 N 0.28330(7) 0.52888(10) 0.79317(9) 0.0194(2) Uani 1 1 d . . .
C14 C 0.36809(9) 0.57012(12) 0.86358(11) 0.0209(3) Uani 1 1 d . . .
H14 H 0.3855(11) 0.6046(15) 0.9407(14) 0.025 Uiso 1 1 d . . .
C15 C 0.42277(9) 0.55492(13) 0.81469(12) 0.0242(3) Uani 1 1 d . . .
H15 H 0.4857(12) 0.5783(16) 0.8490(15) 0.029 Uiso 1 1 d . . .
C16 C 0.36669(9) 0.50105(13) 0.70818(12) 0.0214(3) Uani 1 1 d . . .
H16 H 0.3753(11) 0.4731(16) 0.6466(14) 0.026 Uiso 1 1 d . . .
N17 N 0.12932(8) 0.34626(12) 0.31764(9) 0.0214(3) Uani 1 1 d . . .
H17A H 0.0771(13) 0.3350(17) 0.2532(16) 0.032 Uiso 1 1 d . . .
H17B H 0.1760(12) 0.3783(17) 0.3127(15) 0.032 Uiso 1 1 d . . .


_geom_special_details            
;
 All esds (except the esd in the dihedral angle between two l.s. planes) 
 are estimated using the full covariance matrix.  The cell esds are taken 
 into account individually in the estimation of esds in distances, angles 
 and torsion angles; correlations between esds in cell parameters are only 
 used when they are defined by crystal symmetry.  An approximate (isotropic) 
 treatment of cell esds is used for estimating esds involving l.s. planes. 
;
loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
_geom_bond_publ_flag
C1 N2 1.3547(16) . ?
C1 N6 1.3518(15) . ?
C1 N17 1.3468(16) . ?
N2 C3 1.3311(16) . ?
C3 C4 1.3868(17) . ?
C3 N7 1.4073(15) . ?
C4 C5 1.3848(17) . ?
C5 N6 1.3274(16) . ?
C5 N12 1.4107(15) . ?
N7 N8 1.3656(14) . ?
N7 C11 1.3683(16) . ?
N8 C9 1.3227(17) . ?
C9 C10 1.4086(19) . ?
C10 C11 1.3619(18) . ?
N12 N13 1.3652(14) . ?
N12 C16 1.3633(16) . ?
N13 C14 1.3277(16) . ?
C14 C15 1.4033(19) . ?
C15 C16 1.3670(19) . ?

loop_
_geom_angle_atom_site_label_1
_geom_angle_atom_site_label_2
_geom_angle_atom_site_label_3
_geom_angle
_geom_angle_site_symmetry_1
_geom_angle_site_symmetry_3
_geom_angle_publ_flag
N6 C1 N2 125.96(11) . . ?
N17 C1 N2 117.30(11) . . ?
N17 C1 N6 116.73(11) . . ?
C3 N2 C1 115.15(10) . . ?
N2 C3 C4 124.71(11) . . ?
N2 C3 N7 116.16(10) . . ?
C4 C3 N7 119.10(11) . . ?
C5 C4 C3 113.83(11) . . ?
C4 C5 N12 119.58(11) . . ?
N6 C5 C4 125.25(11) . . ?
N6 C5 N12 115.17(11) . . ?
C5 N6 C1 114.92(10) . . ?
N8 N7 C3 119.19(10) . . ?
N8 N7 C11 112.06(10) . . ?
C11 N7 C3 128.63(11) . . ?
C9 N8 N7 104.11(10) . . ?
N8 C9 C10 112.13(12) . . ?
C11 C10 C9 105.27(11) . . ?
C10 C11 N7 106.42(11) . . ?
N13 N12 C5 120.27(10) . . ?
C16 N12 C5 127.76(11) . . ?
C16 N12 N13 111.97(10) . . ?
C14 N13 N12 104.21(10) . . ?
N13 C14 C15 112.00(12) . . ?
C16 C15 C14 105.23(11) . . ?
N12 C16 C15 106.58(12) . . ?

loop_
_geom_hbond_atom_site_label_D
_geom_hbond_atom_site_label_H
_geom_hbond_atom_site_label_A
_geom_hbond_distance_DH
_geom_hbond_distance_HA
_geom_hbond_distance_DA
_geom_hbond_angle_DHA
_geom_hbond_site_symmetry_A
N17 H17A N2 0.872(18) 2.231(19) 3.0986(15) 173.2(17) 2
N17 H17B N13 0.901(19) 2.210(19) 3.1088(16) 175.1(16) 6_565

_exptl_crystal_recrystallization_method 
'Re-crystallisation from solvent: chloroform'
####################################################################### 
# 
# 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_90-ncse
_database_code_depnum_ccdc_archive 'CCDC 1957591'
loop_
_audit_author_name
_audit_author_address
'Malcolm Halcrow' 'University of Leeds'
_audit_update_record             
;
2019-10-04 deposited with the CCDC.	2019-11-05 downloaded from the CCDC.
;
_audit_creation_date             2019-07-05
_audit_creation_method           
;
  Olex2 1.2
  (compiled Apr 23 2013 17:54:37, GUI svn.r4466)
;
_chemical_name_common            ?
_chemical_name_systematic        
'Catena-[2-amino-4,6-(pyrazol-1-yl)pyrimidine]-di-isoselenocyanato iron(II)'
_chemical_formula_moiety         'C12 H9 Fe N9 Se2'
_chemical_formula_sum            'C12 H9 Fe N9 Se2'
_chemical_formula_weight         493.05
_chemical_melting_point          ?
loop_
_atom_type_symbol
_atom_type_description
_atom_type_scat_dispersion_real
_atom_type_scat_dispersion_imag
_atom_type_scat_source
C C 0.0181 0.0091 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
N N 0.0311 0.0180 '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'
Se Se -0.7943 1.1372 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'

_space_group_crystal_system      tetragonal
_space_group_IT_number           88
_space_group_name_H-M_alt        'I 41/a'
_space_group_name_Hall           '-I 4ad'
loop_
_space_group_symop_id
_space_group_symop_operation_xyz
1 'x, y, z'
2 '-y+3/4, x+1/4, z+1/4'
3 '-x, -y+1/2, z'
4 'y+1/4, -x+1/4, z+1/4'
5 'x+1/2, y+1/2, z+1/2'
6 '-y+5/4, x+3/4, z+3/4'
7 '-x+1/2, -y+1, z+1/2'
8 'y+3/4, -x+3/4, z+3/4'
9 '-x, -y, -z'
10 'y-3/4, -x-1/4, -z-1/4'
11 'x, y-1/2, -z'
12 '-y-1/4, x-1/4, -z-1/4'
13 '-x+1/2, -y+1/2, -z+1/2'
14 'y-1/4, -x+1/4, -z+1/4'
15 'x+1/2, y, -z+1/2'
16 '-y+1/4, x+1/4, -z+1/4'

_cell_length_a                   16.4591(3)
_cell_length_b                   16.4591(3)
_cell_length_c                   25.0804(6)
_cell_angle_alpha                90.00
_cell_angle_beta                 90.00
_cell_angle_gamma                90.00
_cell_volume                     6794.3(2)
_cell_formula_units_Z            16
_cell_measurement_reflns_used    2507
_cell_measurement_temperature    120(2)
_cell_measurement_theta_min      5.37
_cell_measurement_theta_max      72.49
_exptl_absorpt_coefficient_mu    12.161
_exptl_absorpt_correction_T_min  0.923
_exptl_absorpt_correction_T_max  1.000
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   
; 
CrysAlisPro, Agilent Technologies,
Version 1.171.36.24 (release 03-12-2012 CrysAlis171 .NET)
Empirical absorption correction using spherical harmonics,
 implemented in SCALE3 ABSPACK scaling algorithm.
;

_exptl_crystal_colour            yellow
_exptl_crystal_density_diffrn    1.928
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       fragment
_exptl_crystal_F_000             3808
_exptl_crystal_size_max          0.20
_exptl_crystal_size_mid          0.20
_exptl_crystal_size_min          0.10
_exptl_special_details           
;
 ? 
;
_diffrn_reflns_av_R_equivalents  0.0311
_diffrn_reflns_av_unetI/netI     0.0423
_diffrn_reflns_limit_h_max       17
_diffrn_reflns_limit_h_min       -20
_diffrn_reflns_limit_k_max       17
_diffrn_reflns_limit_k_min       -19
_diffrn_reflns_limit_l_max       30
_diffrn_reflns_limit_l_min       -20
_diffrn_reflns_number            7393
_diffrn_reflns_theta_full        72.00
_diffrn_reflns_theta_max         73.64
_diffrn_reflns_theta_min         3.21
_diffrn_ambient_temperature      120(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                2489
_reflns_number_total             3326
_reflns_threshold_expression     >2sigma(I)
_computing_cell_refinement       'CrysAlisPro, Agilent Technologies'
_computing_data_collection       '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         0.840
_refine_diff_density_min         -0.856
_refine_diff_density_rms         0.091
_refine_ls_extinction_coef       ?
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.012
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     223
_refine_ls_number_reflns         3326
_refine_ls_number_restraints     2
_refine_ls_R_factor_all          0.0671
_refine_ls_R_factor_gt           0.0462
_refine_ls_restrained_S_all      1.011
_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)+(0.0609P)²+16.2324P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1146
_refine_ls_wR_factor_ref         0.1276
_refine_special_details          
;
 Refinement of F² against ALL reflections.  The weighted R-factor wR and 
 goodness of fit S are based on F², conventional R-factors R are based 
 on F, with F set to zero for negative F². The threshold expression of 
 F² > 2sigma(F²) is used only for calculating R-factors(gt) etc. and is 
 not relevant to the choice of reflections for refinement.  R-factors based 
 on F² are statistically about twice as large as those based on F, and R- 
 factors based on ALL data will be even larger. 

 No disorder is present in the model, and no restraints were applied to the
 refinement. All non-H atoms were refined anisotropically, and C-bound H 
 atoms were placed in calculated positions and refined using a riding model.
 The amino H atoms H14A and H14B were located in the Fourier map and 
 refined, with the restraint N---H = 0.90(2) Å and the constraint
 Uiso = 1.5xUeq{N14}. 

;
_olex2_refinement_description    
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups
 At 1.5 times of:
  All N(H,H) groups
2. Restrained distances
 N14-H14A = N14-H14B
 0.9 with sigma of 0.02
3.a Aromatic/amide H refined with riding coordinates:
 C11(H11), C17(H17), C18(H18), C19(H19), C22(H22), C23(H23), C24(H24)
;
_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 0.71603(5) 0.52508(5) 0.81005(3) 0.0403(2) Uani 1 1 d . . .
N2 N 0.8337(3) 0.5616(3) 0.79304(16) 0.0517(12) Uani 1 1 d . . .
C3 C 0.8929(4) 0.5805(3) 0.81356(18) 0.0454(12) Uani 1 1 d . . .
Se4 Se 0.98323(4) 0.61539(4) 0.84560(2) 0.04898(19) Uani 1 1 d . . .
N5 N 0.7678(3) 0.4075(3) 0.82043(16) 0.0480(11) Uani 1 1 d . . .
C6 C 0.8074(4) 0.3528(4) 0.8093(2) 0.0465(13) Uani 1 1 d . . .
Se7 Se 0.87034(4) 0.26746(4) 0.79249(3) 0.0649(2) Uani 1 1 d . . .
C8 C 0.7016(3) 0.4910(3) 0.68573(16) 0.0405(12) Uani 1 1 d . . .
N9 N 0.6651(3) 0.4854(3) 0.73345(13) 0.0377(9) Uani 1 1 d . . .
C10 C 0.5928(3) 0.4482(3) 0.73461(17) 0.0368(11) Uani 1 1 d . . .
C11 C 0.5536(3) 0.4182(3) 0.69051(18) 0.0392(11) Uani 1 1 d . . .
H11 H 0.5020 0.3924 0.6923 0.047 Uiso 1 1 calc R . .
C12 C 0.5957(3) 0.4286(3) 0.64317(17) 0.0381(11) Uani 1 1 d . . .
N13 N 0.6685(3) 0.4626(3) 0.63960(14) 0.0388(9) Uani 1 1 d . . .
N14 N 0.7740(3) 0.5258(4) 0.68312(16) 0.0632(16) Uani 1 1 d D . .
H14A H 0.801(5) 0.535(5) 0.7132(19) 0.095 Uiso 1 1 d D . .
H14B H 0.798(5) 0.529(5) 0.6510(17) 0.095 Uiso 1 1 d D . .
N15 N 0.5580(3) 0.4411(3) 0.78557(15) 0.0423(10) Uani 1 1 d . . .
N16 N 0.5982(3) 0.4743(3) 0.82822(15) 0.0434(10) Uani 1 1 d . . .
C17 C 0.5522(4) 0.4570(4) 0.8702(2) 0.0518(15) Uani 1 1 d . . .
H17 H 0.5644 0.4725 0.9058 0.062 Uiso 1 1 calc R . .
C18 C 0.4839(4) 0.4132(5) 0.8550(3) 0.0655(18) Uani 1 1 d . . .
H18 H 0.4418 0.3938 0.8776 0.079 Uiso 1 1 calc R . .
C19 C 0.4891(4) 0.4036(4) 0.8012(2) 0.0590(16) Uani 1 1 d . . .
H19 H 0.4516 0.3758 0.7790 0.071 Uiso 1 1 calc R . .
N20 N 0.5629(3) 0.4027(3) 0.59496(16) 0.0433(10) Uani 1 1 d . . .
N21 N 0.6050(3) 0.4152(3) 0.54877(15) 0.0492(12) Uani 1 1 d . . .
C22 C 0.5579(4) 0.3863(4) 0.5103(2) 0.0623(18) Uani 1 1 d . . .
H22 H 0.5713 0.3872 0.4734 0.075 Uiso 1 1 calc R . .
C23 C 0.4863(5) 0.3547(5) 0.5311(3) 0.075(2) Uani 1 1 d . . .
H23 H 0.4434 0.3301 0.5116 0.090 Uiso 1 1 calc R . .
C24 C 0.4894(4) 0.3657(5) 0.5852(3) 0.0650(18) Uani 1 1 d . . .
H24 H 0.4492 0.3508 0.6107 0.078 Uiso 1 1 calc R . .


_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 2.073(5) . ?
Fe1 N5 2.131(5) . ?
Fe1 N9 2.195(4) . ?
Fe1 N13 2.201(4) 4_565 ?
Fe1 N16 2.160(5) . ?
Fe1 N21 2.162(5) 4_565 ?
N2 C3 1.145(7) . ?
C3 Se4 1.784(6) . ?
N5 C6 1.146(8) . ?
C6 Se7 1.795(7) . ?
C8 N9 1.342(6) . ?
C8 N13 1.361(6) . ?
C8 N14 1.323(7) . ?
N9 C10 1.339(7) . ?
C10 C11 1.373(7) . ?
C10 N15 1.406(6) . ?
C11 H11 0.9500 . ?
C11 C12 1.385(7) . ?
C12 N13 1.326(7) . ?
C12 N20 1.391(6) . ?
N14 H14A 0.89(2) . ?
N14 H14B 0.90(2) . ?
N15 N16 1.371(6) . ?
N15 C19 1.350(8) . ?
N16 C17 1.328(7) . ?
C17 H17 0.9500 . ?
C17 C18 1.390(9) . ?
C18 H18 0.9500 . ?
C18 C19 1.361(8) . ?
C19 H19 0.9500 . ?
N20 N21 1.366(6) . ?
N20 C24 1.376(8) . ?
N21 C22 1.326(7) . ?
C22 H22 0.9500 . ?
C22 C23 1.392(11) . ?
C23 H23 0.9500 . ?
C23 C24 1.370(9) . ?
C24 H24 0.9500 . ?

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 N5 85.1(2) . . ?
N2 Fe1 N9 105.23(16) . . ?
N2 Fe1 N13 95.06(17) . 4_565 ?
N2 Fe1 N16 174.0(2) . . ?
N2 Fe1 N21 94.0(2) . 4_565 ?
N5 Fe1 N9 89.38(16) . . ?
N5 Fe1 N13 106.41(16) . 4_565 ?
N5 Fe1 N16 88.97(19) . . ?
N5 Fe1 N21 179.1(2) . 4_565 ?
N9 Fe1 N13 155.37(17) . 4_565 ?
N16 Fe1 N9 74.15(15) . . ?
N16 Fe1 N13 87.08(16) . 4_565 ?
N16 Fe1 N21 91.91(19) . 4_565 ?
N21 Fe1 N9 90.55(16) 4_565 . ?
N21 Fe1 N13 73.96(15) 4_565 4_565 ?
C3 N2 Fe1 141.4(4) . . ?
N2 C3 Se4 176.9(6) . . ?
C6 N5 Fe1 155.7(4) . . ?
N5 C6 Se7 179.2(5) . . ?
N9 C8 N13 123.7(5) . . ?
N14 C8 N9 118.4(4) . . ?
N14 C8 N13 117.8(4) . . ?
C8 N9 Fe1 126.1(3) . . ?
C10 N9 Fe1 117.2(3) . . ?
C10 N9 C8 116.6(4) . . ?
N9 C10 C11 124.4(4) . . ?
N9 C10 N15 114.8(4) . . ?
C11 C10 N15 120.8(5) . . ?
C10 C11 H11 122.9 . . ?
C10 C11 C12 114.3(5) . . ?
C12 C11 H11 122.9 . . ?
C11 C12 N20 120.9(5) . . ?
N13 C12 C11 124.2(4) . . ?
N13 C12 N20 114.9(4) . . ?
C8 N13 Fe1 126.4(4) . 6_544 ?
C12 N13 Fe1 116.9(3) . 6_544 ?
C12 N13 C8 116.7(4) . . ?
C8 N14 H14A 119(6) . . ?
C8 N14 H14B 117(6) . . ?
H14A N14 H14B 122(8) . . ?
N16 N15 C10 118.7(4) . . ?
C19 N15 C10 130.1(5) . . ?
C19 N15 N16 111.1(4) . . ?
N15 N16 Fe1 115.0(3) . . ?
C17 N16 Fe1 139.7(4) . . ?
C17 N16 N15 105.0(4) . . ?
N16 C17 H17 124.6 . . ?
N16 C17 C18 110.8(5) . . ?
C18 C17 H17 124.6 . . ?
C17 C18 H18 126.8 . . ?
C19 C18 C17 106.3(5) . . ?
C19 C18 H18 126.8 . . ?
N15 C19 C18 106.8(6) . . ?
N15 C19 H19 126.6 . . ?
C18 C19 H19 126.6 . . ?
N21 N20 C12 119.6(5) . . ?
N21 N20 C24 111.3(4) . . ?
C24 N20 C12 129.1(5) . . ?
N20 N21 Fe1 114.3(3) . 6_544 ?
C22 N21 Fe1 140.1(4) . 6_544 ?
C22 N21 N20 105.5(5) . . ?
N21 C22 H22 124.6 . . ?
N21 C22 C23 110.8(5) . . ?
C23 C22 H22 124.6 . . ?
C22 C23 H23 126.5 . . ?
C24 C23 C22 107.0(6) . . ?
C24 C23 H23 126.5 . . ?
N20 C24 H24 127.3 . . ?
C23 C24 N20 105.5(6) . . ?
C23 C24 H24 127.3 . . ?

loop_
_geom_hbond_atom_site_label_D
_geom_hbond_atom_site_label_H
_geom_hbond_atom_site_label_A
_geom_hbond_distance_DH
_geom_hbond_distance_HA
_geom_hbond_distance_DA
_geom_hbond_angle_DHA
_geom_hbond_site_symmetry_A
N14 H14A N2 0.89(2) 2.12(3) 2.986(6) 164(8) .
N14 H14B N5 0.90(2) 2.16(3) 3.046(6) 170(8) 6_544

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

data_sf-6
_database_code_depnum_ccdc_archive 'CCDC 1957574'
loop_
_audit_author_name
_audit_author_address
'Malcolm Halcrow' 'University of Leeds'
_audit_update_record             
;
2019-10-04 deposited with the CCDC.	2019-11-05 downloaded from the CCDC.
;
_audit_creation_date             2019-07-05
_audit_creation_method           
;
  Olex2 1.2
  (compiled Apr 23 2013 17:54:37, GUI svn.r4466)
;
_chemical_name_common            ?
_chemical_name_systematic        
;
2,4-Bis(4-chloropyrazol-1-yl)-6H-1,3,5-triazine acetonitrile solvate
;
_chemical_formula_moiety         'C9 H5 Cl2 N7, C2 H3 N'
_chemical_formula_sum            'C11 H8 Cl2 N8'
_chemical_formula_weight         323.15
_chemical_absolute_configuration ad
_chemical_melting_point          ?
loop_
_atom_type_symbol
_atom_type_description
_atom_type_scat_dispersion_real
_atom_type_scat_dispersion_imag
_atom_type_scat_source
C C 0.0181 0.0091 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
N N 0.0311 0.0180 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Cl Cl 0.3639 0.7018 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'

_space_group_crystal_system      orthorhombic
_space_group_IT_number           19
_space_group_name_H-M_alt        'P 21 21 21'
_space_group_name_Hall           'P 2ac 2ab'
loop_
_space_group_symop_id
_space_group_symop_operation_xyz
1 'x, y, z'
2 '-x+1/2, -y, z+1/2'
3 'x+1/2, -y+1/2, -z'
4 '-x, y+1/2, -z+1/2'

_cell_length_a                   3.9058(4)
_cell_length_b                   16.7955(15)
_cell_length_c                   20.5409(9)
_cell_angle_alpha                90.00
_cell_angle_beta                 90.00
_cell_angle_gamma                90.00
_cell_volume                     1347.48(19)
_cell_formula_units_Z            4
_cell_measurement_reflns_used    2008
_cell_measurement_temperature    120(2)
_cell_measurement_theta_min      4.29
_cell_measurement_theta_max      73.57
_exptl_absorpt_coefficient_mu    4.411
_exptl_absorpt_correction_T_min  0.834
_exptl_absorpt_correction_T_max  1.000
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   
; 
CrysAlisPro, Agilent Technologies,
Version 1.171.36.24 (release 03-12-2012 CrysAlis171 .NET)
Empirical absorption correction using spherical harmonics,
 implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_crystal_colour            colourless
_exptl_crystal_density_diffrn    1.593
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       needle
_exptl_crystal_F_000             656
_exptl_crystal_size_max          0.40
_exptl_crystal_size_mid          0.10
_exptl_crystal_size_min          0.05
_exptl_special_details           
;
 ? 
;
_diffrn_reflns_av_R_equivalents  0.0255
_diffrn_reflns_av_unetI/netI     0.0413
_diffrn_reflns_limit_h_max       4
_diffrn_reflns_limit_h_min       -3
_diffrn_reflns_limit_k_max       20
_diffrn_reflns_limit_k_min       -15
_diffrn_reflns_limit_l_max       24
_diffrn_reflns_limit_l_min       -24
_diffrn_reflns_number            3249
_diffrn_reflns_theta_full        72.00
_diffrn_reflns_theta_max         74.04
_diffrn_reflns_theta_min         3.40
_diffrn_ambient_temperature      120(2)
_diffrn_detector_area_resol_mean 5.3095
_diffrn_measured_fraction_theta_full 0.988
_diffrn_measured_fraction_theta_max 0.971
_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                2142
_reflns_number_total             2346
_reflns_threshold_expression     >2sigma(I)
_computing_cell_refinement       'CrysAlisPro, Agilent Technologies'
_computing_data_collection       '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         0.254
_refine_diff_density_min         -0.286
_refine_diff_density_rms         0.055
_refine_ls_abs_structure_details 'Flack H D (1983), Acta Cryst. A39, 876-881'
_refine_ls_abs_structure_Flack   0.346(19)
_refine_ls_extinction_coef       ?
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.065
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     192
_refine_ls_number_reflns         2346
_refine_ls_number_restraints     0
_refine_ls_R_factor_all          0.0375
_refine_ls_R_factor_gt           0.0332
_refine_ls_restrained_S_all      1.065
_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)+(0.0485P)²+0.1533P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0856
_refine_ls_wR_factor_ref         0.0879
_refine_special_details          
;
 Refinement of F² against ALL reflections.  The weighted R-factor wR and 
 goodness of fit S are based on F², conventional R-factors R are based 
 on F, with F set to zero for negative F². The threshold expression of 
 F² > 2sigma(F²) is used only for calculating R-factors(gt) etc. and is 
 not relevant to the choice of reflections for refinement.  R-factors based 
 on F² are statistically about twice as large as those based on F, and R- 
 factors based on ALL data will be even larger. 

 The crystal was refined as a racemic twin. All non-H atoms were refined 
 anisotropically. While all the H atoms were located in the Fourier map, they
 didn't all refine to chemically reasonable positions. Hence, H atoms were
 placed in calculated positions and refined using a riding model in the final
 least squares cycles.
;
_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.a Aromatic/amide H refined with riding coordinates:
 C4(H4), C9(H9), C11(H11), C15(H15), C17(H17)
2.b Idealised Me refined as rotating group:
 C19(H19A,H19B,H19C)
;
_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
N1 N 0.4968(6) 0.55804(12) 0.60154(11) 0.0192(5) Uani 1 1 d . . .
C2 C 0.3336(8) 0.62711(15) 0.60721(12) 0.0195(5) Uani 1 1 d . . .
N3 N 0.3017(7) 0.68314(12) 0.56167(11) 0.0229(5) Uani 1 1 d . . .
C4 C 0.4501(8) 0.66280(16) 0.50589(13) 0.0234(6) Uani 1 1 d . . .
H4 H 0.4313 0.7002 0.4714 0.028 Uiso 1 1 calc R . .
N5 N 0.6217(7) 0.59641(13) 0.49253(11) 0.0223(5) Uani 1 1 d . . .
C6 C 0.6342(7) 0.54687(15) 0.54322(12) 0.0182(5) Uani 1 1 d . . .
N7 N 0.1770(7) 0.64029(12) 0.66709(10) 0.0198(4) Uani 1 1 d . . .
N8 N 0.0247(7) 0.71180(14) 0.68114(12) 0.0261(5) Uani 1 1 d . . .
C9 C -0.0973(8) 0.70238(17) 0.74043(15) 0.0275(7) Uani 1 1 d . . .
H9 H -0.2163 0.7424 0.7640 0.033 Uiso 1 1 calc R . .
C10 C -0.0286(8) 0.62521(16) 0.76449(13) 0.0226(6) Uani 1 1 d . . .
C11 C 0.1466(7) 0.58658(15) 0.71717(12) 0.0203(5) Uani 1 1 d . . .
H11 H 0.2306 0.5335 0.7184 0.024 Uiso 1 1 calc R . .
Cl12 Cl -0.1532(2) 0.58705(4) 0.83842(3) 0.02634(17) Uani 1 1 d . . .
N13 N 0.8160(6) 0.47598(12) 0.53551(10) 0.0192(4) Uani 1 1 d . . .
N14 N 0.9681(7) 0.45754(14) 0.47744(11) 0.0218(5) Uani 1 1 d . . .
C15 C 1.1121(8) 0.38790(16) 0.48811(13) 0.0232(6) Uani 1 1 d . . .
H15 H 1.2414 0.3593 0.4567 0.028 Uiso 1 1 calc R . .
C16 C 1.0499(8) 0.36113(16) 0.55213(13) 0.0213(6) Uani 1 1 d . . .
C17 C 0.8604(7) 0.41850(15) 0.58192(12) 0.0203(5) Uani 1 1 d . . .
H17 H 0.7772 0.4186 0.6254 0.024 Uiso 1 1 calc R . .
Cl18 Cl 1.1836(2) 0.27318(4) 0.58587(3) 0.02734(17) Uani 1 1 d . . .
C19 C 0.3997(10) 0.3857(2) 0.85431(15) 0.0353(8) Uani 1 1 d . . .
H19A H 0.4424 0.3305 0.8676 0.053 Uiso 1 1 calc R . .
H19B H 0.1536 0.3968 0.8565 0.053 Uiso 1 1 calc R . .
H19C H 0.5224 0.4219 0.8835 0.053 Uiso 1 1 calc R . .
C20 C 0.5193(9) 0.39730(17) 0.78792(15) 0.0288(6) Uani 1 1 d . . .
N21 N 0.6105(9) 0.40605(18) 0.73620(13) 0.0425(8) Uani 1 1 d . . .


_geom_special_details            
;
 All esds (except the esd in the dihedral angle between two l.s. planes) 
 are estimated using the full covariance matrix.  The cell esds are taken 
 into account individually in the estimation of esds in distances, angles 
 and torsion angles; correlations between esds in cell parameters are only 
 used when they are defined by crystal symmetry.  An approximate (isotropic) 
 treatment of cell esds is used for estimating esds involving l.s. planes. 
;
loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
_geom_bond_publ_flag
N1 C2 1.329(3) . ?
N1 C6 1.326(3) . ?
C2 N3 1.333(3) . ?
C2 N7 1.391(3) . ?
N3 C4 1.329(4) . ?
C4 H4 0.9500 . ?
C4 N5 1.330(4) . ?
N5 C6 1.334(3) . ?
C6 N13 1.395(3) . ?
N7 N8 1.371(3) . ?
N7 C11 1.373(3) . ?
N8 C9 1.317(4) . ?
C9 H9 0.9500 . ?
C9 C10 1.413(4) . ?
C10 C11 1.354(4) . ?
C10 Cl12 1.719(3) . ?
C11 H11 0.9500 . ?
N13 N14 1.368(3) . ?
N13 C17 1.368(3) . ?
N14 C15 1.316(4) . ?
C15 H15 0.9500 . ?
C15 C16 1.411(4) . ?
C16 C17 1.360(4) . ?
C16 Cl18 1.713(3) . ?
C17 H17 0.9500 . ?
C19 H19A 0.9800 . ?
C19 H19B 0.9800 . ?
C19 H19C 0.9800 . ?
C19 C20 1.455(4) . ?
C20 N21 1.130(4) . ?

loop_
_geom_angle_atom_site_label_1
_geom_angle_atom_site_label_2
_geom_angle_atom_site_label_3
_geom_angle
_geom_angle_site_symmetry_1
_geom_angle_site_symmetry_3
_geom_angle_publ_flag
C6 N1 C2 113.4(2) . . ?
N1 C2 N3 126.9(2) . . ?
N1 C2 N7 115.3(2) . . ?
N3 C2 N7 117.8(2) . . ?
C4 N3 C2 112.5(2) . . ?
N3 C4 H4 116.1 . . ?
N3 C4 N5 127.9(2) . . ?
N5 C4 H4 116.1 . . ?
C4 N5 C6 112.4(2) . . ?
N1 C6 N5 127.0(2) . . ?
N1 C6 N13 115.4(2) . . ?
N5 C6 N13 117.5(2) . . ?
N8 N7 C2 121.1(2) . . ?
N8 N7 C11 112.3(2) . . ?
C11 N7 C2 126.6(2) . . ?
C9 N8 N7 104.3(2) . . ?
N8 C9 H9 124.3 . . ?
N8 C9 C10 111.4(3) . . ?
C10 C9 H9 124.3 . . ?
C9 C10 Cl12 126.7(2) . . ?
C11 C10 C9 106.5(2) . . ?
C11 C10 Cl12 126.8(2) . . ?
N7 C11 H11 127.3 . . ?
C10 C11 N7 105.5(2) . . ?
C10 C11 H11 127.3 . . ?
N14 N13 C6 120.9(2) . . ?
C17 N13 C6 126.0(2) . . ?
C17 N13 N14 113.1(2) . . ?
C15 N14 N13 104.0(2) . . ?
N14 C15 H15 124.3 . . ?
N14 C15 C16 111.4(2) . . ?
C16 C15 H15 124.3 . . ?
C15 C16 Cl18 126.8(2) . . ?
C17 C16 C15 106.7(2) . . ?
C17 C16 Cl18 126.5(2) . . ?
N13 C17 H17 127.6 . . ?
C16 C17 N13 104.8(2) . . ?
C16 C17 H17 127.6 . . ?
H19A C19 H19B 109.5 . . ?
H19A C19 H19C 109.5 . . ?
H19B C19 H19C 109.5 . . ?
C20 C19 H19A 109.5 . . ?
C20 C19 H19B 109.5 . . ?
C20 C19 H19C 109.5 . . ?
N21 C20 C19 179.6(4) . . ?

loop_
_geom_hbond_atom_site_label_D
_geom_hbond_atom_site_label_H
_geom_hbond_atom_site_label_A
_geom_hbond_distance_DH
_geom_hbond_distance_HA
_geom_hbond_distance_DA
_geom_hbond_angle_DHA
_geom_hbond_site_symmetry_A
C17 H17 N21 0.95 2.38 3.322(4) 173.4 .

_exptl_crystal_recrystallization_method 
'Re-crystallisation from solvent: acetonitrile/diethyl ether'
####################################################################### 
# 
# 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_89-scn
_database_code_depnum_ccdc_archive 'CCDC 1957588'
loop_
_audit_author_name
_audit_author_address
'Malcolm Halcrow' 'University of Leeds'
_audit_update_record             
;
2019-10-04 deposited with the CCDC.	2019-11-05 downloaded from the CCDC.
;
_audit_creation_date             2019-07-05
_audit_creation_method           
;
  Olex2 1.2
  (compiled Apr 23 2013 17:54:37, GUI svn.r4466)
;
_chemical_name_common            ?
_chemical_name_systematic        
'Catena-[2-methyl-4,6-(pyrazol-1-yl)pyrimidine]-di-isothiocyanato iron(II)'
_chemical_formula_moiety         'C13 H10 Fe N8 S2'
_chemical_formula_sum            'C13 H10 Fe N8 S2'
_chemical_formula_weight         398.26
_chemical_melting_point          ?
loop_
_atom_type_symbol
_atom_type_description
_atom_type_scat_dispersion_real
_atom_type_scat_dispersion_imag
_atom_type_scat_source
C C 0.0181 0.0091 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
N N 0.0311 0.0180 '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'
S S 0.3331 0.5567 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'

_space_group_crystal_system      tetragonal
_space_group_IT_number           88
_space_group_name_H-M_alt        'I 41/a'
_space_group_name_Hall           '-I 4ad'
loop_
_space_group_symop_id
_space_group_symop_operation_xyz
1 'x, y, z'
2 '-y+3/4, x+1/4, z+1/4'
3 '-x, -y+1/2, z'
4 'y+1/4, -x+1/4, z+1/4'
5 'x+1/2, y+1/2, z+1/2'
6 '-y+5/4, x+3/4, z+3/4'
7 '-x+1/2, -y+1, z+1/2'
8 'y+3/4, -x+3/4, z+3/4'
9 '-x, -y, -z'
10 'y-3/4, -x-1/4, -z-1/4'
11 'x, y-1/2, -z'
12 '-y-1/4, x-1/4, -z-1/4'
13 '-x+1/2, -y+1/2, -z+1/2'
14 'y-1/4, -x+1/4, -z+1/4'
15 'x+1/2, y, -z+1/2'
16 '-y+1/4, x+1/4, -z+1/4'

_cell_length_a                   16.1912(6)
_cell_length_b                   16.1912(6)
_cell_length_c                   25.146(3)
_cell_angle_alpha                90.00
_cell_angle_beta                 90.00
_cell_angle_gamma                90.00
_cell_volume                     6592.1(8)
_cell_formula_units_Z            16
_cell_measurement_reflns_used    3153
_cell_measurement_temperature    120(2)
_cell_measurement_theta_min      5.22
_cell_measurement_theta_max      71.88
_exptl_absorpt_coefficient_mu    9.830
_exptl_absorpt_correction_T_min  0.528
_exptl_absorpt_correction_T_max  1.000
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   
; 
CrysAlisPro, Agilent Technologies,
Version 1.171.36.24 (release 03-12-2012 CrysAlis171 .NET)
Empirical absorption correction using spherical harmonics,
 implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_crystal_colour            red
_exptl_crystal_density_diffrn    1.605
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       plate
_exptl_crystal_F_000             3232
_exptl_crystal_size_max          0.40
_exptl_crystal_size_mid          0.35
_exptl_crystal_size_min          0.10
_exptl_special_details           
;
 ? 
;
_diffrn_reflns_av_R_equivalents  0.0219
_diffrn_reflns_av_unetI/netI     0.0263
_diffrn_reflns_limit_h_max       19
_diffrn_reflns_limit_h_min       -19
_diffrn_reflns_limit_k_max       19
_diffrn_reflns_limit_k_min       -14
_diffrn_reflns_limit_l_max       29
_diffrn_reflns_limit_l_min       -23
_diffrn_reflns_number            7784
_diffrn_reflns_theta_full        72.00
_diffrn_reflns_theta_max         73.39
_diffrn_reflns_theta_min         3.25
_diffrn_ambient_temperature      120(2)
_diffrn_detector_area_resol_mean 5.3095
_diffrn_measured_fraction_theta_full 0.985
_diffrn_measured_fraction_theta_max 0.974
_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                2786
_reflns_number_total             3232
_reflns_threshold_expression     >2sigma(I)
_computing_cell_refinement       'CrysAlisPro, Agilent Technologies'
_computing_data_collection       '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         0.635
_refine_diff_density_min         -0.399
_refine_diff_density_rms         0.066
_refine_ls_extinction_coef       ?
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.076
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     218
_refine_ls_number_reflns         3232
_refine_ls_number_restraints     0
_refine_ls_R_factor_all          0.0633
_refine_ls_R_factor_gt           0.0558
_refine_ls_restrained_S_all      1.076
_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)+(0.0849P)²+10.8593P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1506
_refine_ls_wR_factor_ref         0.1565
_refine_special_details          
;
 Refinement of F² against ALL reflections.  The weighted R-factor wR and 
 goodness of fit S are based on F², conventional R-factors R are based 
 on F, with F set to zero for negative F². The threshold expression of 
 F² > 2sigma(F²) is used only for calculating R-factors(gt) etc. and is 
 not relevant to the choice of reflections for refinement.  R-factors based 
 on F² are statistically about twice as large as those based on F, and R- 
 factors based on ALL data will be even larger. 

 No disorder is present in the model, and no restraints were applied to the
 refinement. All non-H atoms were refined anisotropically, and H atoms were
 placed in calculated positions and refined using a riding model.
;
_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.a Aromatic/amide H refined with riding coordinates:
 C11(H11), C17(H17), C18(H18), C19(H19), C22(H22), C23(H23), C24(H24)
2.b Idealised Me refined as rotating group:
 C14(H14A,H14B,H14C)
;
_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 0.72116(4) 0.53027(4) 0.809934(19) 0.0482(2) Uani 1 1 d . . .
N2 N 0.8408(2) 0.5706(3) 0.80327(13) 0.0616(9) Uani 1 1 d . . .
C3 C 0.9051(3) 0.5855(2) 0.82083(15) 0.0516(9) Uani 1 1 d . . .
S4 S 0.99332(8) 0.61108(8) 0.84436(6) 0.0789(4) Uani 1 1 d . . .
N5 N 0.7678(2) 0.4067(2) 0.80854(12) 0.0571(8) Uani 1 1 d . . .
C6 C 0.8086(2) 0.3497(3) 0.79720(15) 0.0509(9) Uani 1 1 d . . .
S7 S 0.86780(7) 0.27189(7) 0.78509(6) 0.0740(4) Uani 1 1 d . . .
C8 C 0.6955(2) 0.4996(3) 0.68567(13) 0.0501(9) Uani 1 1 d . . .
N9 N 0.66123(18) 0.49257(19) 0.73380(10) 0.0445(7) Uani 1 1 d . . .
C10 C 0.5916(2) 0.4497(2) 0.73747(13) 0.0431(7) Uani 1 1 d . . .
C11 C 0.5522(2) 0.4145(2) 0.69455(13) 0.0452(8) Uani 1 1 d . . .
H11 H 0.5020 0.3844 0.6977 0.054 Uiso 1 1 calc R . .
C12 C 0.5921(2) 0.4268(2) 0.64628(13) 0.0435(8) Uani 1 1 d . . .
N13 N 0.66375(19) 0.4653(2) 0.64151(10) 0.0463(7) Uani 1 1 d . . .
C14 C 0.7726(3) 0.5484(4) 0.68019(16) 0.0744(14) Uani 1 1 d . . .
H14A H 0.8156 0.5140 0.6641 0.112 Uiso 1 1 calc R . .
H14B H 0.7908 0.5669 0.7154 0.112 Uiso 1 1 calc R . .
H14C H 0.7622 0.5965 0.6575 0.112 Uiso 1 1 calc R . .
N15 N 0.55877(19) 0.44208(19) 0.78880(11) 0.0464(7) Uani 1 1 d . . .
N16 N 0.59965(19) 0.47903(19) 0.83001(11) 0.0469(7) Uani 1 1 d . . .
C17 C 0.5545(3) 0.4618(3) 0.87284(14) 0.0543(9) Uani 1 1 d . . .
H17 H 0.5676 0.4797 0.9078 0.065 Uiso 1 1 calc R . .
C18 C 0.4859(3) 0.4146(3) 0.86009(17) 0.0663(12) Uani 1 1 d . . .
H18 H 0.4448 0.3949 0.8839 0.080 Uiso 1 1 calc R . .
C19 C 0.4894(3) 0.4021(3) 0.80648(16) 0.0594(10) Uani 1 1 d . . .
H19 H 0.4512 0.3717 0.7855 0.071 Uiso 1 1 calc R . .
N20 N 0.55766(19) 0.3978(2) 0.59901(11) 0.0507(7) Uani 1 1 d . . .
N21 N 0.5983(2) 0.4137(2) 0.55184(11) 0.0552(8) Uani 1 1 d . . .
C22 C 0.5480(3) 0.3842(3) 0.51461(16) 0.0685(13) Uani 1 1 d . . .
H22 H 0.5593 0.3861 0.4776 0.082 Uiso 1 1 calc R . .
C23 C 0.4767(3) 0.3502(4) 0.5366(2) 0.0774(14) Uani 1 1 d . . .
H23 H 0.4320 0.3256 0.5179 0.093 Uiso 1 1 calc R . .
C24 C 0.4837(3) 0.3591(3) 0.59053(18) 0.0674(12) Uani 1 1 d . . .
H24 H 0.4451 0.3419 0.6167 0.081 Uiso 1 1 calc R . .


_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 2.051(4) . ?
Fe1 N5 2.139(4) . ?
Fe1 N9 2.231(3) . ?
Fe1 N13 2.245(3) 4_565 ?
Fe1 N16 2.194(3) . ?
Fe1 N21 2.184(4) 4_565 ?
N2 C3 1.157(5) . ?
C3 S4 1.601(4) . ?
N5 C6 1.171(5) . ?
C6 S7 1.611(5) . ?
C8 N9 1.336(4) . ?
C8 N13 1.344(4) . ?
C8 C14 1.483(6) . ?
N9 C10 1.326(5) . ?
C10 C11 1.379(5) . ?
C10 N15 1.402(4) . ?
C11 H11 0.9500 . ?
C11 C12 1.390(5) . ?
C12 N13 1.322(5) . ?
C12 N20 1.394(4) . ?
C14 H14A 0.9800 . ?
C14 H14B 0.9800 . ?
C14 H14C 0.9800 . ?
N15 N16 1.367(4) . ?
N15 C19 1.370(5) . ?
N16 C17 1.332(5) . ?
C17 H17 0.9500 . ?
C17 C18 1.384(6) . ?
C18 H18 0.9500 . ?
C18 C19 1.364(6) . ?
C19 H19 0.9500 . ?
N20 N21 1.381(5) . ?
N20 C24 1.368(6) . ?
N21 C22 1.329(5) . ?
C22 H22 0.9500 . ?
C22 C23 1.395(8) . ?
C23 H23 0.9500 . ?
C23 C24 1.368(7) . ?
C24 H24 0.9500 . ?

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 N5 87.87(15) . . ?
N2 Fe1 N9 115.32(12) . . ?
N2 Fe1 N13 89.18(13) . 4_565 ?
N2 Fe1 N16 170.43(12) . . ?
N2 Fe1 N21 96.21(15) . 4_565 ?
N5 Fe1 N9 83.32(12) . . ?
N5 Fe1 N13 114.05(11) . 4_565 ?
N5 Fe1 N16 88.10(13) . . ?
N5 Fe1 N21 172.19(12) . 4_565 ?
N9 Fe1 N13 151.19(12) . 4_565 ?
N16 Fe1 N9 72.78(11) . . ?
N16 Fe1 N13 84.53(11) . 4_565 ?
N21 Fe1 N9 88.91(11) 4_565 . ?
N21 Fe1 N13 72.77(11) 4_565 4_565 ?
N21 Fe1 N16 88.84(13) 4_565 . ?
C3 N2 Fe1 152.3(3) . . ?
N2 C3 S4 177.0(4) . . ?
C6 N5 Fe1 160.2(3) . . ?
N5 C6 S7 176.4(4) . . ?
N9 C8 N13 123.7(3) . . ?
N9 C8 C14 118.6(3) . . ?
N13 C8 C14 117.7(3) . . ?
C8 N9 Fe1 125.0(2) . . ?
C10 N9 Fe1 116.9(2) . . ?
C10 N9 C8 117.4(3) . . ?
N9 C10 C11 123.8(3) . . ?
N9 C10 N15 115.7(3) . . ?
C11 C10 N15 120.5(3) . . ?
C10 C11 H11 123.0 . . ?
C10 C11 C12 114.1(3) . . ?
C12 C11 H11 123.0 . . ?
C11 C12 N20 120.6(3) . . ?
N13 C12 C11 123.7(3) . . ?
N13 C12 N20 115.6(3) . . ?
C8 N13 Fe1 125.7(3) . 6_544 ?
C12 N13 Fe1 117.2(2) . 6_544 ?
C12 N13 C8 117.1(3) . . ?
C8 C14 H14A 109.5 . . ?
C8 C14 H14B 109.5 . . ?
C8 C14 H14C 109.5 . . ?
H14A C14 H14B 109.5 . . ?
H14A C14 H14C 109.5 . . ?
H14B C14 H14C 109.5 . . ?
N16 N15 C10 118.4(3) . . ?
N16 N15 C19 110.9(3) . . ?
C19 N15 C10 130.7(3) . . ?
N15 N16 Fe1 115.2(2) . . ?
C17 N16 Fe1 139.3(3) . . ?
C17 N16 N15 104.8(3) . . ?
N16 C17 H17 124.2 . . ?
N16 C17 C18 111.6(3) . . ?
C18 C17 H17 124.2 . . ?
C17 C18 H18 126.9 . . ?
C19 C18 C17 106.1(4) . . ?
C19 C18 H18 126.9 . . ?
N15 C19 H19 126.7 . . ?
C18 C19 N15 106.5(4) . . ?
C18 C19 H19 126.7 . . ?
N21 N20 C12 118.6(3) . . ?
C24 N20 C12 129.6(3) . . ?
C24 N20 N21 111.6(3) . . ?
N20 N21 Fe1 115.4(2) . 6_544 ?
C22 N21 Fe1 140.3(3) . 6_544 ?
C22 N21 N20 104.2(4) . . ?
N21 C22 H22 124.1 . . ?
N21 C22 C23 111.7(4) . . ?
C23 C22 H22 124.1 . . ?
C22 C23 H23 126.8 . . ?
C24 C23 C22 106.4(4) . . ?
C24 C23 H23 126.8 . . ?
N20 C24 H24 127.0 . . ?
C23 C24 N20 106.0(5) . . ?
C23 C24 H24 127.0 . . ?

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

data_icb15nm
_database_code_depnum_ccdc_archive 'CCDC 1957592'
loop_
_audit_author_name
_audit_author_address
'Malcolm Halcrow' 'University of Leeds'
_audit_update_record             
;
2019-10-04 deposited with the CCDC.	2019-11-05 downloaded from the CCDC.
;
_audit_creation_date             2019-07-05
_audit_creation_method           
;
  Olex2 1.2
  (compiled Apr 23 2013 17:54:37, GUI svn.r4466)
;
_chemical_name_common            ?
_chemical_name_systematic        
;
Catena-[4,6-(pyrazol-1-yl)pyrimidine]-diaquairon(II) diperchlorate
;
_chemical_formula_moiety         'C10 H11 Fe N6 O2, 2(Cl O4)'
_chemical_formula_sum            'C10 H12 Cl2 Fe N6 O10'
_chemical_formula_weight         503.01
_chemical_melting_point          ?
loop_
_atom_type_symbol
_atom_type_description
_atom_type_scat_dispersion_real
_atom_type_scat_dispersion_imag
_atom_type_scat_source
C C 0.0181 0.0091 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
N N 0.0311 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'
Cl Cl 0.3639 0.7018 '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'

_space_group_crystal_system      monoclinic
_space_group_IT_number           15
_space_group_name_H-M_alt        'C 1 2/c 1'
_space_group_name_Hall           '-C 2yc'
loop_
_space_group_symop_id
_space_group_symop_operation_xyz
1 'x, y, z'
2 '-x, y, -z+1/2'
3 'x+1/2, y+1/2, z'
4 '-x+1/2, y+1/2, -z+1/2'
5 '-x, -y, -z'
6 'x, -y, z-1/2'
7 '-x+1/2, -y+1/2, -z'
8 'x+1/2, -y+1/2, z-1/2'

_cell_length_a                   20.888(2)
_cell_length_b                   9.323(2)
_cell_length_c                   19.916(2)
_cell_angle_alpha                90.00
_cell_angle_beta                 113.519(13)
_cell_angle_gamma                90.00
_cell_volume                     3556.3(10)
_cell_formula_units_Z            8
_cell_measurement_reflns_used    1585
_cell_measurement_temperature    125(2)
_cell_measurement_theta_min      5.17
_cell_measurement_theta_max      73.34
_exptl_absorpt_coefficient_mu    10.228
_exptl_absorpt_correction_T_min  0.557
_exptl_absorpt_correction_T_max  1.000
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   
; 
CrysAlisPro, Agilent Technologies,
Version 1.171.36.24 (release 03-12-2012 CrysAlis171 .NET)
Empirical absorption correction using spherical harmonics,
 implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_crystal_colour            yellow
_exptl_crystal_density_diffrn    1.879
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       needle
_exptl_crystal_F_000             2032
_exptl_crystal_size_max          0.40
_exptl_crystal_size_mid          0.15
_exptl_crystal_size_min          0.05
_exptl_special_details           
;
 ? 
;
_diffrn_reflns_av_R_equivalents  0.0387
_diffrn_reflns_av_unetI/netI     0.0535
_diffrn_reflns_limit_h_max       25
_diffrn_reflns_limit_h_min       -25
_diffrn_reflns_limit_k_max       11
_diffrn_reflns_limit_k_min       -7
_diffrn_reflns_limit_l_max       24
_diffrn_reflns_limit_l_min       -20
_diffrn_reflns_number            6362
_diffrn_reflns_theta_full        72.00
_diffrn_reflns_theta_max         73.24
_diffrn_reflns_theta_min         4.62
_diffrn_ambient_temperature      125(2)
_diffrn_detector_area_resol_mean 5.3095
_diffrn_measured_fraction_theta_full 0.979
_diffrn_measured_fraction_theta_max 0.965
_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                2515
_reflns_number_total             3454
_reflns_threshold_expression     >2sigma(I)
_computing_cell_refinement       'CrysAlisPro, Agilent Technologies'
_computing_data_collection       '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         0.670
_refine_diff_density_min         -0.936
_refine_diff_density_rms         0.106
_refine_ls_extinction_coef       ?
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.036
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     284
_refine_ls_number_reflns         3454
_refine_ls_number_restraints     44
_refine_ls_R_factor_all          0.1128
_refine_ls_R_factor_gt           0.0881
_refine_ls_restrained_S_all      1.038
_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)+(0.1130P)²+27.6726P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.2258
_refine_ls_wR_factor_ref         0.2503
_refine_special_details          
;
 Refinement of F² against ALL reflections.  The weighted R-factor wR and 
 goodness of fit S are based on F², conventional R-factors R are based 
 on F, with F set to zero for negative F². The threshold expression of 
 F² > 2sigma(F²) is used only for calculating R-factors(gt) etc. and is 
 not relevant to the choice of reflections for refinement.  R-factors based 
 on F² are statistically about twice as large as those based on F, and R- 
 factors based on ALL data will be even larger.

 The asymmetric unit contains two iron half-atoms lying on special positions:
 Fe1, lying on the crystallographic C₂ axis 1/2, y, 1/4; and Fe2, on the
 inversion centre 1/2, 1, 1/2. There is also one whole organic bridging ligand,
 one aqua ligand per iron atom, and two disordered perchlorate anions which
 were modelled over two orientations with the refined restraints Cl---O = 
 1.43(2) Å and O...O = 2.34(2) Å. Fully occupied non-H atoms plus the
 partial Cl atoms were refined anisotropically, and C-bound H atoms were
 placed in calculated positions and refined using a riding model. 

 Three of the four H atoms on the two aqua ligands were located in the Fourier 
 map and refined positionally, with the fixed restraints O---H = 0.90(2) and
 H...H = 1.37(2) Å and the constraint Uiso{H} = 1.5xUeq{O}. The fourth H 
 atom, bound to O20, was not located but is accounted for in the molecular 
 weight and density calculations. Potential H-bond acceptors for this H atom 
 are disordered anion O28Aⁱ/O29Bⁱ or o27Aⁱⁱ (symmetry codes: 
 (i) x, 2-y, 1/2+z; (ii) 1-x, 1+y, 1/2-z).  
;
_olex2_refinement_description    
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups
 At 1.5 times of:
  All O(H) groups, All O(H,H) groups
2. Restrained distances
 Cl1A-O22A = Cl1A-O23A = Cl1A-O24A = Cl1A-O25A
 1.4318 with sigma of 0.02
 Cl1B-O22B = Cl1B-O23B = Cl1B-O24B = Cl1B-O25B
 1.4318 with sigma of 0.02
 O22A-O23A = O22A-O24A = O22A-O25A = O23A-O24A = O23A-O25A = O24A-O25A
 2.338129 with sigma of 0.02
 O22B-O23B = O22B-O24B = O22B-O25B = O23B-O24B = O23B-O25B = O24B-O25B
 2.338129 with sigma of 0.02
 Cl6A-O27A = Cl6A-O28A = Cl6A-O29A = Cl6A-O30A
 1.4318 with sigma of 0.02
 Cl6B-O27B = Cl6B-O28B = Cl6B-O29B = Cl6B-O30B
 1.4318 with sigma of 0.02
 O27A-O28A = O27A-O29A = O27A-O30A = O28A-O29A = O28A-O30A = O29A-O30A
 2.338129 with sigma of 0.02
 O27B-O28B = O27B-O29B = O27B-O30B = O28B-O29B = O28B-O30B = O29B-O30B
 2.338129 with sigma of 0.02
 O19-H19A = O19-H19B = O20-H20
 0.9 with sigma of 0.02
 H19A-H19B
 1.37 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: Cl1A(0.5) O22A(0.5) O23A(0.5) O24A(0.5) O25A(0.5) Cl1B(0.5)
 O22B(0.5) O23B(0.5) O24B(0.5) O25B(0.5) Cl6A(0.6) O27A(0.6) O28A(0.6)
 O29A(0.6) O30A(0.6) Cl6B(0.4) O27B(0.4) O28B(0.4) O29B(0.4) O30B(0.4)
4.a Aromatic/amide H refined with riding coordinates:
 C3(H3), C6(H6), C11(H11), C12(H12), C13(H13), C16(H16), C17(H17), C18(H18)
;
_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 0.5000 0.57234(19) 0.2500 0.0490(4) Uani 1 2 d S . .
Fe2 Fe 0.5000 1.0000 0.5000 0.0454(4) Uani 1 2 d S . .
C3 C 0.5157(4) 0.8009(9) 0.3764(3) 0.0523(17) Uani 1 1 d . . .
H3 H 0.4681 0.7784 0.3648 0.063 Uiso 1 1 calc R . .
N4 N 0.5456(3) 0.7369(8) 0.3366(3) 0.0524(15) Uani 1 1 d . . .
C5 C 0.6124(4) 0.7711(10) 0.3539(4) 0.0557(19) Uani 1 1 d . . .
C6 C 0.6493(4) 0.8647(11) 0.4087(4) 0.063(2) Uani 1 1 d . . .
H6 H 0.6967 0.8882 0.4196 0.076 Uiso 1 1 calc R . .
C7 C 0.6132(4) 0.9228(10) 0.4472(4) 0.0569(19) Uani 1 1 d . . .
N8 N 0.5459(3) 0.8932(7) 0.4307(3) 0.0519(14) Uani 1 1 d . . .
N9 N 0.6435(3) 0.7011(8) 0.3121(3) 0.0541(15) Uani 1 1 d . . .
N10 N 0.6038(3) 0.6051(8) 0.2598(3) 0.0553(15) Uani 1 1 d . . .
C11 C 0.6452(4) 0.5588(10) 0.2292(4) 0.0579(19) Uani 1 1 d . . .
H11 H 0.6320 0.4906 0.1906 0.070 Uiso 1 1 calc R . .
C12 C 0.7112(4) 0.6225(12) 0.2606(4) 0.067(2) Uani 1 1 d . . .
H12 H 0.7499 0.6054 0.2479 0.080 Uiso 1 1 calc R . .
C13 C 0.7091(4) 0.7129(11) 0.3125(4) 0.062(2) Uani 1 1 d . . .
H13 H 0.7458 0.7730 0.3432 0.075 Uiso 1 1 calc R . .
N14 N 0.6456(3) 1.0127(8) 0.5061(4) 0.0581(16) Uani 1 1 d . . .
N15 N 0.6114(3) 1.0455(7) 0.5510(3) 0.0552(15) Uani 1 1 d . . .
C16 C 0.6572(4) 1.1196(9) 0.6048(5) 0.062(2) Uani 1 1 d . . .
H16 H 0.6486 1.1565 0.6448 0.074 Uiso 1 1 calc R . .
C17 C 0.7208(4) 1.1383(10) 0.5964(5) 0.068(2) Uani 1 1 d . . .
H17 H 0.7610 1.1891 0.6279 0.081 Uiso 1 1 calc R . .
C18 C 0.7120(4) 1.0676(12) 0.5334(5) 0.073(3) Uani 1 1 d . . .
H18 H 0.7454 1.0582 0.5125 0.088 Uiso 1 1 calc R . .
O19 O 0.4792(3) 0.4152(7) 0.1695(3) 0.0627(14) Uani 1 1 d D . .
H19A H 0.475(5) 0.321(3) 0.174(5) 0.094 Uiso 1 1 d D . .
H19B H 0.448(4) 0.430(9) 0.124(2) 0.094 Uiso 1 1 d D . .
O20 O 0.4899(3) 1.1883(7) 0.4400(3) 0.0727(17) Uani 1 1 d D . .
H20A H 0.453(4) 1.196(14) 0.397(3) 0.109 Uiso 1 1 d D . .
Cl21A Cl 0.3902(3) 1.0924(6) 0.2293(3) 0.0616(14) Uani 0.50 1 d PD A 1
O22A O 0.3185(5) 1.0738(13) 0.1861(6) 0.069(3) Uiso 0.50 1 d PD A 1
O23A O 0.3990(7) 1.2071(14) 0.2817(7) 0.078(4) Uiso 0.50 1 d PD A 1
O24A O 0.4235(7) 1.1340(16) 0.1812(7) 0.088(4) Uiso 0.50 1 d PD A 1
O25A O 0.4205(5) 0.9652(10) 0.2675(5) 0.055(2) Uiso 0.50 1 d PD A 1
Cl21B Cl 0.3934(3) 1.1346(6) 0.2580(3) 0.0639(14) Uani 0.50 1 d PD B 2
O22B O 0.3722(8) 0.9898(13) 0.2587(8) 0.090(4) Uiso 0.50 1 d PD B 2
O23B O 0.4685(6) 1.1427(16) 0.3013(7) 0.091(4) Uiso 0.50 1 d PD B 2
O24B O 0.3790(8) 1.1844(17) 0.1866(7) 0.101(5) Uiso 0.50 1 d PD B 2
O25B O 0.3629(9) 1.2215(17) 0.2969(9) 0.112(5) Uiso 0.50 1 d PD B 2
Cl26A Cl 0.3716(5) 0.5083(9) -0.0332(5) 0.0547(17) Uani 0.60 1 d PD C 1
O27A O 0.4183(5) 0.4086(10) -0.0440(5) 0.066(2) Uiso 0.60 1 d PD C 1
O28A O 0.3867(7) 0.6506(13) -0.0481(8) 0.115(5) Uiso 0.60 1 d PD C 1
O29A O 0.3704(5) 0.5030(13) 0.0391(5) 0.070(3) Uiso 0.60 1 d PD C 1
O30A O 0.3011(4) 0.4791(9) -0.0851(4) 0.0516(19) Uiso 0.60 1 d PD C 1
Cl26B Cl 0.3709(8) 0.5322(16) -0.0185(8) 0.066(4) Uani 0.40 1 d PD D 2
O27B O 0.3618(14) 0.460(3) -0.0828(10) 0.158(11) Uiso 0.40 1 d PD D 2
O28B O 0.3240(10) 0.6474(19) -0.0290(11) 0.114(7) Uiso 0.40 1 d PD D 2
O29B O 0.4409(8) 0.592(2) 0.0148(10) 0.099(6) Uiso 0.40 1 d PD D 2
O30B O 0.3674(6) 0.4304(14) 0.0358(6) 0.050(3) Uiso 0.40 1 d PD D 2


_geom_special_details            
;
 All esds (except the esd in the dihedral angle between two l.s. planes) 
 are estimated using the full covariance matrix.  The cell esds are taken 
 into account individually in the estimation of esds in distances, angles 
 and torsion angles; correlations between esds in cell parameters are only 
 used when they are defined by crystal symmetry.  An approximate (isotropic) 
 treatment of cell esds is used for estimating esds involving l.s. planes. 
;
loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
_geom_bond_publ_flag
Fe1 N4 2.219(6) . ?
Fe1 N10 2.119(6) . ?
Fe1 O19 2.086(6) . ?
Fe2 N8 2.207(6) . ?
Fe2 N15 2.178(6) . ?
Fe2 O20 2.086(6) . ?
C3 H3 0.9500 . ?
C3 N4 1.329(9) . ?
C3 N8 1.328(9) . ?
N4 C5 1.337(9) . ?
C5 C6 1.369(11) . ?
C5 N9 1.404(10) . ?
C6 H6 0.9500 . ?
C6 C7 1.383(11) . ?
C7 N8 1.338(9) . ?
C7 N14 1.380(10) . ?
N9 N10 1.373(9) . ?
N9 C13 1.373(9) . ?
N10 C11 1.314(10) . ?
C11 H11 0.9500 . ?
C11 C12 1.399(12) . ?
C12 H12 0.9500 . ?
C12 C13 1.347(12) . ?
C13 H13 0.9500 . ?
N14 N15 1.381(9) . ?
N14 C18 1.371(10) . ?
N15 C16 1.312(10) . ?
C16 H16 0.9500 . ?
C16 C17 1.414(12) . ?
C17 H17 0.9500 . ?
C17 C18 1.363(12) . ?
C18 H18 0.9500 . ?
O19 H19A 0.89(2) . ?
O19 H19B 0.89(2) . ?
O20 H20A 0.89(2) . ?
Cl21A O22A 1.408(11) . ?
Cl21A O23A 1.454(11) . ?
Cl21A O24A 1.445(11) . ?
Cl21A O25A 1.415(10) . ?
Cl21B O22B 1.422(12) . ?
Cl21B O23B 1.460(11) . ?
Cl21B O24B 1.411(12) . ?
Cl21B O25B 1.435(13) . ?
Cl26A O27A 1.423(11) . ?
Cl26A O28A 1.422(13) . ?
Cl26A O29A 1.452(10) . ?
Cl26A O30A 1.449(11) . ?
Cl26B O27B 1.394(15) . ?
Cl26B O28B 1.412(16) . ?
Cl26B O29B 1.456(16) . ?
Cl26B O30B 1.462(15) . ?

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
N4 Fe1 N4 92.6(3) . 2_655 ?
N10 Fe1 N4 74.0(2) . . ?
N10 Fe1 N4 94.4(2) . 2_655 ?
N10 Fe1 N10 163.4(4) . 2_655 ?
O19 Fe1 N4 89.7(2) . 2_655 ?
O19 Fe1 N4 167.5(2) . . ?
O19 Fe1 N10 93.7(3) . . ?
O19 Fe1 N10 98.0(3) . 2_655 ?
O19 Fe1 O19 90.7(3) . 2_655 ?
N8 Fe2 N8 180.00 . 5_676 ?
N15 Fe2 N8 74.3(2) . . ?
N15 Fe2 N8 105.7(2) . 5_676 ?
N15 Fe2 N15 180.00 5_676 . ?
O20 Fe2 N8 90.5(3) . 5_676 ?
O20 Fe2 N8 89.5(3) . . ?
O20 Fe2 N15 93.0(3) . 5_676 ?
O20 Fe2 N15 87.0(3) . . ?
O20 Fe2 O20 180.00 5_676 . ?
N4 C3 H3 116.8 . . ?
N8 C3 H3 116.8 . . ?
N8 C3 N4 126.3(7) . . ?
C3 N4 Fe1 128.0(5) . . ?
C3 N4 C5 115.5(6) . . ?
C5 N4 Fe1 116.4(5) . . ?
N4 C5 C6 123.7(7) . . ?
N4 C5 N9 114.7(7) . . ?
C6 C5 N9 121.5(7) . . ?
C5 C6 H6 122.2 . . ?
C5 C6 C7 115.7(7) . . ?
C7 C6 H6 122.2 . . ?
N8 C7 C6 122.4(7) . . ?
N8 C7 N14 116.4(7) . . ?
N14 C7 C6 121.2(7) . . ?
C3 N8 Fe2 128.2(5) . . ?
C3 N8 C7 116.4(6) . . ?
C7 N8 Fe2 115.4(5) . . ?
N10 N9 C5 118.1(6) . . ?
C13 N9 C5 131.0(7) . . ?
C13 N9 N10 110.8(6) . . ?
N9 N10 Fe1 116.7(5) . . ?
C11 N10 Fe1 138.5(6) . . ?
C11 N10 N9 104.8(6) . . ?
N10 C11 H11 124.2 . . ?
N10 C11 C12 111.6(7) . . ?
C12 C11 H11 124.2 . . ?
C11 C12 H12 126.9 . . ?
C13 C12 C11 106.3(7) . . ?
C13 C12 H12 126.9 . . ?
N9 C13 H13 126.7 . . ?
C12 C13 N9 106.5(8) . . ?
C12 C13 H13 126.7 . . ?
C7 N14 N15 118.7(6) . . ?
C18 N14 C7 129.8(7) . . ?
C18 N14 N15 111.2(7) . . ?
N14 N15 Fe2 112.7(4) . . ?
C16 N15 Fe2 141.1(6) . . ?
C16 N15 N14 104.4(7) . . ?
N15 C16 H16 123.8 . . ?
N15 C16 C17 112.4(7) . . ?
C17 C16 H16 123.8 . . ?
C16 C17 H17 127.5 . . ?
C18 C17 C16 105.1(7) . . ?
C18 C17 H17 127.5 . . ?
N14 C18 H18 126.6 . . ?
C17 C18 N14 106.8(8) . . ?
C17 C18 H18 126.6 . . ?
Fe1 O19 H19A 128(6) . . ?
Fe1 O19 H19B 121(6) . . ?
H19A O19 H19B 102(3) . . ?
Fe2 O20 H20A 117(8) . . ?
O22A Cl21A O23A 109.2(8) . . ?
O22A Cl21A O24A 107.7(8) . . ?
O22A Cl21A O25A 111.4(7) . . ?
O24A Cl21A O23A 108.8(8) . . ?
O25A Cl21A O23A 109.2(8) . . ?
O25A Cl21A O24A 110.5(8) . . ?
O22B Cl21B O23B 108.0(8) . . ?
O22B Cl21B O25B 108.9(9) . . ?
O24B Cl21B O22B 112.4(9) . . ?
O24B Cl21B O23B 108.9(9) . . ?
O24B Cl21B O25B 113.4(9) . . ?
O25B Cl21B O23B 104.9(9) . . ?
O27A Cl26A O29A 114.3(8) . . ?
O27A Cl26A O30A 109.4(7) . . ?
O28A Cl26A O27A 110.8(9) . . ?
O28A Cl26A O29A 109.4(9) . . ?
O28A Cl26A O30A 105.9(8) . . ?
O30A Cl26A O29A 106.7(8) . . ?
O27B Cl26B O28B 113.7(14) . . ?
O27B Cl26B O29B 110.5(14) . . ?
O27B Cl26B O30B 109.6(13) . . ?
O28B Cl26B O29B 106.6(12) . . ?
O28B Cl26B O30B 111.5(12) . . ?
O29B Cl26B O30B 104.5(11) . . ?

loop_
_geom_hbond_atom_site_label_D
_geom_hbond_atom_site_label_H
_geom_hbond_atom_site_label_A
_geom_hbond_distance_DH
_geom_hbond_distance_HA
_geom_hbond_distance_DA
_geom_hbond_angle_DHA
_geom_hbond_site_symmetry_A
O19 H19A O24A 0.89(2) 2.09(5) 2.913(15) 154(10) 1_545
O19 H19A O23B 0.89(2) 1.98(7) 2.735(16) 142(9) 2_645
O19 H19B O29A 0.89(2) 1.94(4) 2.804(11) 163(10) .
O19 H19B O30B 0.89(2) 1.89(4) 2.757(13) 164(9) .
O20 H20A O23A 0.89(2) 2.13(5) 2.967(15) 156(11) .
O20 H20A O23B 0.89(2) 2.13(11) 2.651(15) 117(9) .
O20 H20A O25B 0.89(2) 2.14(3) 3.037(18) 178(12) .

_exptl_crystal_recrystallization_method 
'Re-crystallisation from solvent: nitromethane'
####################################################################### 
# 
# 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_sf-3
_database_code_depnum_ccdc_archive 'CCDC 1957573'
loop_
_audit_author_name
_audit_author_address
'Malcolm Halcrow' 'University of Leeds'
_audit_update_record             
;
2019-10-04 deposited with the CCDC.	2019-11-05 downloaded from the CCDC.
;
_audit_creation_date             2019-07-09
_audit_creation_method           
;
  Olex2 1.2
  (compiled Apr 23 2013 17:54:37, GUI svn.r4466)
;
_chemical_name_common            ?
_chemical_name_systematic        
'2,4-Bis(4,5,6,7-tetrahydroindazol-2-yl)-6H-1,3,5-triazinedichloroform solvate'
_chemical_formula_moiety         'C17 H19 N7, 2(C H Cl3)'
_chemical_formula_sum            'C19 H21 Cl6 N7'
_chemical_formula_weight         560.13
_chemical_melting_point          ?
loop_
_atom_type_symbol
_atom_type_description
_atom_type_scat_dispersion_real
_atom_type_scat_dispersion_imag
_atom_type_scat_source
C C 0.0181 0.0091 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
N N 0.0311 0.0180 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Cl Cl 0.3639 0.7018 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'

_space_group_crystal_system      triclinic
_space_group_IT_number           2
_space_group_name_H-M_alt        'P -1'
_space_group_name_Hall           '-P 1'
loop_
_space_group_symop_id
_space_group_symop_operation_xyz
1 'x, y, z'
2 '-x, -y, -z'

_cell_length_a                   9.3073(3)
_cell_length_b                   11.3030(3)
_cell_length_c                   23.5856(8)
_cell_angle_alpha                88.648(2)
_cell_angle_beta                 86.046(3)
_cell_angle_gamma                87.961(2)
_cell_volume                     2473.19(13)
_cell_formula_units_Z            4
_cell_measurement_reflns_used    6346
_cell_measurement_temperature    120(2)
_cell_measurement_theta_min      3.73
_cell_measurement_theta_max      73.19
_exptl_absorpt_coefficient_mu    6.530
_exptl_absorpt_correction_T_min  0.421
_exptl_absorpt_correction_T_max  1.000
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   
; 
CrysAlisPro, Agilent Technologies,
Version 1.171.36.24 (release 03-12-2012 CrysAlis171 .NET)
Empirical absorption correction using spherical harmonics,
 implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_crystal_colour            colourless
_exptl_crystal_density_diffrn    1.504
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       fragment
_exptl_crystal_F_000             1144
_exptl_crystal_size_max          0.20
_exptl_crystal_size_mid          0.10
_exptl_crystal_size_min          0.10
_exptl_special_details           
;
 ? 
;
_diffrn_reflns_av_R_equivalents  0.0524
_diffrn_reflns_av_unetI/netI     0.0602
_diffrn_reflns_limit_h_max       8
_diffrn_reflns_limit_h_min       -11
_diffrn_reflns_limit_k_max       14
_diffrn_reflns_limit_k_min       -12
_diffrn_reflns_limit_l_max       27
_diffrn_reflns_limit_l_min       -29
_diffrn_reflns_number            19525
_diffrn_reflns_theta_full        72.00
_diffrn_reflns_theta_max         73.79
_diffrn_reflns_theta_min         3.76
_diffrn_ambient_temperature      120(2)
_diffrn_detector_area_resol_mean 5.3095
_diffrn_measured_fraction_theta_full 0.945
_diffrn_measured_fraction_theta_max 0.932
_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                6794
_reflns_number_total             9320
_reflns_threshold_expression     >2sigma(I)
_computing_cell_refinement       'CrysAlisPro, Agilent Technologies'
_computing_data_collection       '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         1.077
_refine_diff_density_min         -0.832
_refine_diff_density_rms         0.112
_refine_ls_extinction_coef       ?
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.029
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     609
_refine_ls_number_reflns         9320
_refine_ls_number_restraints     24
_refine_ls_R_factor_all          0.1008
_refine_ls_R_factor_gt           0.0766
_refine_ls_restrained_S_all      1.819
_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)+(0.1155P)²+3.3688P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1950
_refine_ls_wR_factor_ref         0.2201
_refine_special_details          
;
 Refinement of F² against ALL reflections.  The weighted R-factor wR and 
 goodness of fit S are based on F², conventional R-factors R are based 
 on F, with F set to zero for negative F². The threshold expression of 
 F² > 2sigma(F²) is used only for calculating R-factors(gt) etc. and is 
 not relevant to the choice of reflections for refinement.  R-factors based 
 on F² are statistically about twice as large as those based on F, and R- 
 factors based on ALL data will be even larger. 

 The asymmetric unit contains two formula units of the compound. That is,
 two molecules of interest and four chloroform solvent molecules. Two of
 the solvent molecules are disordered over two sites, whose occupancies
 refined to 0.61:0.39 and 0.64:0.36. These were modelled using the fixed
 restraints C---Cl = 1.72(2) and Cl...Cl = 2.81(2) Å. All non-H atoms
 except the minor disorder sites were refined anisotropically, and H atoms
 were placed in calculated positions and refined using a riding model.
;
_olex2_refinement_description    
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups, All C(H,H) groups
2. Restrained distances
 C57A-Cl8A = C57A-Cl9A = C57A-Cl0A = C57B-Cl8B = C57B-Cl9B = C57B-Cl0B
 1.72 with sigma of 0.02
 Cl8A-Cl9A = Cl8A-Cl0A = Cl9A-Cl0A = Cl8B-Cl9B = Cl8B-Cl0B = Cl9B-Cl0B
 2.81 with sigma of 0.02
 C61A-Cl2A = C61A-Cl3A = C61A-Cl4A = C61B-Cl2B = C61B-Cl3B = C61B-Cl4B
 1.72 with sigma of 0.02
 Cl2A-Cl2A = Cl2A-Cl4A = Cl3A-Cl4A = Cl2B-Cl3B = Cl2B-Cl4B = Cl3B-Cl4B
 2.81 with sigma of 0.02
3. Others
 Fixed Sof: C57A(0.61) H57A(0.61) Cl8A(0.61) Cl9A(0.61) Cl0A(0.61) C57B(0.39)
 H57B(0.39) Cl8B(0.39) Cl9B(0.39) Cl0B(0.39) C61A(0.64) H61A(0.64) Cl2A(0.64)
 Cl3A(0.64) Cl4A(0.64) C61B(0.36) H61B(0.36) Cl2B(0.36) Cl3B(0.36) Cl4B(0.36)
4.a Ternary CH refined with riding coordinates:
 C49(H49), C53(H53), C57A(H57A), C57B(H57B), C61A(H61A), C61B(H61B)
4.b Secondary CH2 refined with riding coordinates:
 C10(H10A,H10B), C11(H11A,H11B), C12(H12A,H12B), C13(H13A,H13B), C19(H19A,
 H19B), C20(H20A,H20B), C21(H21A,H21B), C22(H22A,H22B), C34(H34A,H34B),
 C35(H35A,H35B), C36(H36A,H36B), C37(H37A,H37B), C43(H43A,H43B), C44(H44A,H44B),
  C45(H45A,H45B), C46(H46A,H46B)
4.c Aromatic/amide H refined with riding coordinates:
 C4(H4), C15(H15), C24(H24), C28(H28), C39(H39), C48(H48)
;
_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
N1 N 0.7336(6) 0.2821(5) 0.2495(2) 0.0257(12) Uani 1 1 d . . .
C2 C 0.8073(7) 0.3389(6) 0.2863(3) 0.0264(14) Uani 1 1 d . . .
N3 N 0.8026(7) 0.4552(5) 0.2952(3) 0.0294(12) Uani 1 1 d . . .
C4 C 0.7143(8) 0.5158(6) 0.2620(3) 0.0315(15) Uani 1 1 d . . .
H4 H 0.7072 0.5992 0.2666 0.038 Uiso 1 1 calc R . .
N5 N 0.6348(7) 0.4714(5) 0.2229(3) 0.0293(13) Uani 1 1 d . . .
C6 C 0.6503(7) 0.3542(6) 0.2196(3) 0.0241(13) Uani 1 1 d . . .
N7 N 0.8949(6) 0.2675(5) 0.3192(2) 0.0264(12) Uani 1 1 d . . .
N8 N 0.9727(6) 0.3160(5) 0.3602(2) 0.0289(12) Uani 1 1 d . . .
C9 C 1.0346(8) 0.2237(7) 0.3847(3) 0.0292(14) Uani 1 1 d . . .
C10 C 1.1285(8) 0.2314(7) 0.4337(3) 0.0339(16) Uani 1 1 d . . .
H10A H 1.0878 0.2922 0.4603 0.041 Uiso 1 1 calc R . .
H10B H 1.2263 0.2548 0.4196 0.041 Uiso 1 1 calc R . .
C11 C 1.1369(9) 0.1108(8) 0.4644(3) 0.0410(19) Uani 1 1 d . . .
H11A H 1.2121 0.1114 0.4920 0.049 Uiso 1 1 calc R . .
H11B H 1.0436 0.0963 0.4857 0.049 Uiso 1 1 calc R . .
C12 C 1.1721(9) 0.0108(8) 0.4226(4) 0.0404(18) Uani 1 1 d . . .
H12A H 1.1886 -0.0641 0.4441 0.048 Uiso 1 1 calc R . .
H12B H 1.2621 0.0282 0.3995 0.048 Uiso 1 1 calc R . .
C13 C 1.0502(9) -0.0049(7) 0.3827(3) 0.0366(17) Uani 1 1 d . . .
H13A H 1.0855 -0.0554 0.3505 0.044 Uiso 1 1 calc R . .
H13B H 0.9688 -0.0444 0.4036 0.044 Uiso 1 1 calc R . .
C14 C 0.9997(8) 0.1148(6) 0.3602(3) 0.0296(14) Uani 1 1 d . . .
C15 C 0.9099(8) 0.1466(6) 0.3189(3) 0.0294(14) Uani 1 1 d . . .
H15 H 0.8660 0.0949 0.2946 0.035 Uiso 1 1 calc R . .
N16 N 0.5724(6) 0.2984(5) 0.1802(2) 0.0256(12) Uani 1 1 d . . .
N17 N 0.4870(7) 0.3635(5) 0.1448(3) 0.0284(12) Uani 1 1 d . . .
C18 C 0.4368(7) 0.2830(6) 0.1119(3) 0.0251(13) Uani 1 1 d . . .
C19 C 0.3415(9) 0.3118(6) 0.0643(3) 0.0340(16) Uani 1 1 d . . .
H19A H 0.3980 0.3500 0.0323 0.041 Uiso 1 1 calc R . .
H19B H 0.2625 0.3677 0.0775 0.041 Uiso 1 1 calc R . .
C20 C 0.2779(11) 0.1967(8) 0.0444(4) 0.046(2) Uani 1 1 d . . .
H20A H 0.2007 0.1713 0.0726 0.055 Uiso 1 1 calc R . .
H20B H 0.2343 0.2124 0.0077 0.055 Uiso 1 1 calc R . .
C21 C 0.3905(11) 0.0987(8) 0.0372(4) 0.046(2) Uani 1 1 d . . .
H21A H 0.4708 0.1261 0.0111 0.055 Uiso 1 1 calc R . .
H21B H 0.3482 0.0304 0.0198 0.055 Uiso 1 1 calc R . .
C22 C 0.4498(8) 0.0585(6) 0.0939(3) 0.0312(15) Uani 1 1 d . . .
H22A H 0.3762 0.0139 0.1170 0.037 Uiso 1 1 calc R . .
H22B H 0.5361 0.0058 0.0869 0.037 Uiso 1 1 calc R . .
C23 C 0.4888(8) 0.1660(6) 0.1254(3) 0.0257(13) Uani 1 1 d . . .
C24 C 0.5747(8) 0.1803(6) 0.1690(3) 0.0272(14) Uani 1 1 d . . .
H24 H 0.6266 0.1194 0.1882 0.033 Uiso 1 1 calc R . .
N25 N 0.2475(6) 0.2636(5) 0.2537(2) 0.0270(12) Uani 1 1 d . . .
C26 C 0.3274(7) 0.1872(6) 0.2827(3) 0.0240(13) Uani 1 1 d . . .
N27 N 0.3355(6) 0.0695(5) 0.2774(2) 0.0274(12) Uani 1 1 d . . .
C28 C 0.2510(8) 0.0315(6) 0.2390(3) 0.0303(15) Uani 1 1 d . . .
H28 H 0.2516 -0.0517 0.2341 0.036 Uiso 1 1 calc R . .
N29 N 0.1658(7) 0.0963(5) 0.2067(3) 0.0291(12) Uani 1 1 d . . .
C30 C 0.1692(8) 0.2120(6) 0.2167(3) 0.0259(13) Uani 1 1 d . . .
N31 N 0.4103(6) 0.2374(5) 0.3218(2) 0.0264(12) Uani 1 1 d . . .
N32 N 0.4883(6) 0.1677(5) 0.3581(2) 0.0273(12) Uani 1 1 d . . .
C33 C 0.5426(8) 0.2443(6) 0.3916(3) 0.0279(14) Uani 1 1 d . . .
C34 C 0.6333(8) 0.2098(7) 0.4396(3) 0.0317(15) Uani 1 1 d . . .
H34A H 0.7332 0.1901 0.4247 0.038 Uiso 1 1 calc R . .
H34B H 0.5943 0.1391 0.4600 0.038 Uiso 1 1 calc R . .
C35 C 0.6330(10) 0.3140(7) 0.4807(3) 0.0391(18) Uani 1 1 d . . .
H35A H 0.5372 0.3223 0.5015 0.047 Uiso 1 1 calc R . .
H35B H 0.7055 0.2974 0.5089 0.047 Uiso 1 1 calc R . .
C36 C 0.6671(9) 0.4296(7) 0.4485(3) 0.0352(16) Uani 1 1 d . . .
H36A H 0.7591 0.4190 0.4252 0.042 Uiso 1 1 calc R . .
H36B H 0.6792 0.4925 0.4761 0.042 Uiso 1 1 calc R . .
C37 C 0.5467(9) 0.4680(6) 0.4098(3) 0.0327(15) Uani 1 1 d . . .
H37A H 0.4626 0.5007 0.4331 0.039 Uiso 1 1 calc R . .
H37B H 0.5813 0.5307 0.3828 0.039 Uiso 1 1 calc R . .
C38 C 0.5027(8) 0.3637(6) 0.3776(3) 0.0289(14) Uani 1 1 d . . .
C39 C 0.4175(8) 0.3563(6) 0.3328(3) 0.0284(14) Uani 1 1 d . . .
H39 H 0.3723 0.4202 0.3132 0.034 Uiso 1 1 calc R . .
N40 N 0.0839(6) 0.2891(5) 0.1856(2) 0.0280(12) Uani 1 1 d . . .
N41 N 0.0009(7) 0.2503(5) 0.1445(3) 0.0292(12) Uani 1 1 d . . .
C42 C -0.0550(8) 0.3482(6) 0.1224(3) 0.0296(14) Uani 1 1 d . . .
C43 C -0.1483(9) 0.3508(7) 0.0727(3) 0.0361(17) Uani 1 1 d . . .
H43A H -0.2268 0.2943 0.0798 0.043 Uiso 1 1 calc R . .
H43B H -0.0901 0.3266 0.0379 0.043 Uiso 1 1 calc R . .
C44 C -0.2132(10) 0.4775(8) 0.0641(4) 0.044(2) Uani 1 1 d . . .
H44A H -0.2501 0.4850 0.0258 0.053 Uiso 1 1 calc R . .
H44B H -0.2955 0.4907 0.0924 0.053 Uiso 1 1 calc R . .
C45 C -0.1026(10) 0.5726(8) 0.0704(4) 0.0441(19) Uani 1 1 d . . .
H45A H -0.0173 0.5567 0.0439 0.053 Uiso 1 1 calc R . .
H45B H -0.1452 0.6511 0.0601 0.053 Uiso 1 1 calc R . .
C46 C -0.0557(9) 0.5750(7) 0.1310(4) 0.0381(17) Uani 1 1 d . . .
H46A H 0.0257 0.6285 0.1328 0.046 Uiso 1 1 calc R . .
H46B H -0.1365 0.6048 0.1569 0.046 Uiso 1 1 calc R . .
C47 C -0.0106(8) 0.4516(6) 0.1488(3) 0.0305(15) Uani 1 1 d . . .
C48 C 0.0776(8) 0.4111(6) 0.1889(3) 0.0301(15) Uani 1 1 d . . .
H48 H 0.1257 0.4574 0.2143 0.036 Uiso 1 1 calc R . .
C49 C 0.5343(9) -0.1105(7) 0.3485(3) 0.0350(16) Uani 1 1 d . . .
H49 H 0.4860 -0.0316 0.3414 0.042 Uiso 1 1 calc R . .
Cl50 Cl 0.4104(3) -0.22057(19) 0.34064(13) 0.0591(7) Uani 1 1 d . . .
Cl51 Cl 0.6843(3) -0.1266(2) 0.30013(13) 0.0722(8) Uani 1 1 d . . .
Cl52 Cl 0.5887(3) -0.1159(2) 0.41884(10) 0.0549(6) Uani 1 1 d . . .
C53 C 0.4435(9) 0.6451(7) 0.1431(4) 0.0365(17) Uani 1 1 d . . .
H53 H 0.4872 0.5645 0.1502 0.044 Uiso 1 1 calc R . .
Cl54 Cl 0.3080(3) 0.6748(2) 0.19711(10) 0.0533(6) Uani 1 1 d . . .
Cl55 Cl 0.3678(3) 0.6468(2) 0.07634(10) 0.0543(6) Uani 1 1 d . . .
Cl56 Cl 0.5788(3) 0.74896(19) 0.14336(14) 0.0612(7) Uani 1 1 d . . .
C57A C 1.0094(15) 0.6028(15) 0.3653(7) 0.033(4) Uani 0.61 1 d PD A 1
H57A H 0.9652 0.5264 0.3567 0.040 Uiso 0.61 1 calc PR A 1
Cl58A Cl 1.0449(4) 0.6801(4) 0.30157(15) 0.0522(9) Uani 0.61 1 d PD A 1
Cl59A Cl 1.1685(5) 0.5702(4) 0.3998(3) 0.0752(17) Uani 0.61 1 d PD A 1
Cl60A Cl 0.8857(5) 0.6838(3) 0.4115(2) 0.0508(11) Uani 0.61 1 d PD A 1
C57B C 1.012(3) 0.580(3) 0.3777(10) 0.037(9) Uiso 0.39 1 d PD B 2
H57B H 0.9661 0.5037 0.3695 0.044 Uiso 0.39 1 calc PR B 2
Cl58B Cl 1.1215(9) 0.6207(8) 0.3177(3) 0.0721(19) Uiso 0.39 1 d PD B 2
Cl59B Cl 1.1100(10) 0.5562(8) 0.4366(4) 0.0694(19) Uiso 0.39 1 d PD B 2
Cl60B Cl 0.8757(8) 0.6871(7) 0.3901(3) 0.048(2) Uiso 0.39 1 d PD B 2
C61A C -0.0324(14) -0.0235(17) 0.1183(8) 0.027(4) Uani 0.64 1 d PD C 1
H61A H 0.0115 0.0504 0.1305 0.033 Uiso 0.64 1 calc PR C 1
Cl62A Cl -0.1403(5) -0.0806(3) 0.17605(19) 0.0511(9) Uani 0.64 1 d PD C 1
Cl63A Cl -0.1371(5) 0.0125(5) 0.0611(2) 0.0510(10) Uani 0.64 1 d PD C 1
Cl64A Cl 0.1068(11) -0.1250(10) 0.0981(5) 0.067(4) Uani 0.64 1 d PD C 1
C61B C -0.026(4) -0.038(4) 0.1257(14) 0.058(18) Uiso 0.36 1 d PD D 2
H61B H 0.0081 0.0412 0.1358 0.070 Uiso 0.36 1 calc PR D 2
Cl62B Cl -0.0884(12) -0.1111(10) 0.1868(4) 0.071(3) Uiso 0.36 1 d PD D 2
Cl63B Cl -0.1632(14) -0.0179(12) 0.0801(5) 0.081(4) Uiso 0.36 1 d PD D 2
Cl64B Cl 0.1159(16) -0.1200(15) 0.0936(5) 0.034(3) Uiso 0.36 1 d PD D 2


_geom_special_details            
;
 All esds (except the esd in the dihedral angle between two l.s. planes) 
 are estimated using the full covariance matrix.  The cell esds are taken 
 into account individually in the estimation of esds in distances, angles 
 and torsion angles; correlations between esds in cell parameters are only 
 used when they are defined by crystal symmetry.  An approximate (isotropic) 
 treatment of cell esds is used for estimating esds involving l.s. planes. 
;
loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
_geom_bond_publ_flag
N1 C2 1.334(9) . ?
N1 C6 1.329(9) . ?
C2 N3 1.335(9) . ?
C2 N7 1.389(9) . ?
N3 C4 1.334(9) . ?
C4 H4 0.9500 . ?
C4 N5 1.338(9) . ?
N5 C6 1.331(9) . ?
C6 N16 1.392(8) . ?
N7 N8 1.381(8) . ?
N7 C15 1.369(9) . ?
N8 C9 1.316(10) . ?
C9 C10 1.502(10) . ?
C9 C14 1.428(10) . ?
C10 H10A 0.9900 . ?
C10 H10B 0.9900 . ?
C10 C11 1.531(12) . ?
C11 H11A 0.9900 . ?
C11 H11B 0.9900 . ?
C11 C12 1.529(13) . ?
C12 H12A 0.9900 . ?
C12 H12B 0.9900 . ?
C12 C13 1.541(11) . ?
C13 H13A 0.9900 . ?
C13 H13B 0.9900 . ?
C13 C14 1.512(10) . ?
C14 C15 1.361(10) . ?
C15 H15 0.9500 . ?
N16 N17 1.376(8) . ?
N16 C24 1.366(9) . ?
N17 C18 1.326(9) . ?
C18 C19 1.501(9) . ?
C18 C23 1.429(9) . ?
C19 H19A 0.9900 . ?
C19 H19B 0.9900 . ?
C19 C20 1.545(11) . ?
C20 H20A 0.9900 . ?
C20 H20B 0.9900 . ?
C20 C21 1.501(13) . ?
C21 H21A 0.9900 . ?
C21 H21B 0.9900 . ?
C21 C22 1.534(11) . ?
C22 H22A 0.9900 . ?
C22 H22B 0.9900 . ?
C22 C23 1.506(9) . ?
C23 C24 1.362(10) . ?
C24 H24 0.9500 . ?
N25 C26 1.328(9) . ?
N25 C30 1.332(9) . ?
C26 N27 1.339(9) . ?
C26 N31 1.387(8) . ?
N27 C28 1.329(9) . ?
C28 H28 0.9500 . ?
C28 N29 1.327(9) . ?
N29 C30 1.335(9) . ?
C30 N40 1.389(9) . ?
N31 N32 1.377(8) . ?
N31 C39 1.379(9) . ?
N32 C33 1.320(9) . ?
C33 C34 1.495(10) . ?
C33 C38 1.425(10) . ?
C34 H34A 0.9900 . ?
C34 H34B 0.9900 . ?
C34 C35 1.542(10) . ?
C35 H35A 0.9900 . ?
C35 H35B 0.9900 . ?
C35 C36 1.526(11) . ?
C36 H36A 0.9900 . ?
C36 H36B 0.9900 . ?
C36 C37 1.539(11) . ?
C37 H37A 0.9900 . ?
C37 H37B 0.9900 . ?
C37 C38 1.502(9) . ?
C38 C39 1.370(10) . ?
C39 H39 0.9500 . ?
N40 N41 1.370(8) . ?
N40 C48 1.381(9) . ?
N41 C42 1.317(10) . ?
C42 C43 1.505(10) . ?
C42 C47 1.426(10) . ?
C43 H43A 0.9900 . ?
C43 H43B 0.9900 . ?
C43 C44 1.549(11) . ?
C44 H44A 0.9900 . ?
C44 H44B 0.9900 . ?
C44 C45 1.531(13) . ?
C45 H45A 0.9900 . ?
C45 H45B 0.9900 . ?
C45 C46 1.524(12) . ?
C46 H46A 0.9900 . ?
C46 H46B 0.9900 . ?
C46 C47 1.501(10) . ?
C47 C48 1.356(10) . ?
C48 H48 0.9500 . ?
C49 H49 1.0000 . ?
C49 Cl50 1.748(8) . ?
C49 Cl51 1.747(9) . ?
C49 Cl52 1.767(8) . ?
C53 H53 1.0000 . ?
C53 Cl54 1.759(9) . ?
C53 Cl55 1.768(8) . ?
C53 Cl56 1.752(8) . ?
C57A H57A 1.0000 . ?
C57A Cl58A 1.738(19) . ?
C57A Cl59A 1.763(15) . ?
C57A Cl60A 1.774(15) . ?
C57B H57B 1.0000 . ?
C57B Cl58B 1.75(3) . ?
C57B Cl59B 1.72(2) . ?
C57B Cl60B 1.74(3) . ?
C61A H61A 1.0000 . ?
C61A Cl62A 1.760(18) . ?
C61A Cl63A 1.749(19) . ?
C61A Cl64A 1.747(16) . ?
C61B H61B 1.0000 . ?
C61B Cl62B 1.72(3) . ?
C61B Cl63B 1.73(3) . ?
C61B Cl64B 1.73(3) . ?

loop_
_geom_angle_atom_site_label_1
_geom_angle_atom_site_label_2
_geom_angle_atom_site_label_3
_geom_angle
_geom_angle_site_symmetry_1
_geom_angle_site_symmetry_3
_geom_angle_publ_flag
C6 N1 C2 113.0(6) . . ?
N1 C2 N3 126.7(6) . . ?
N1 C2 N7 115.4(6) . . ?
N3 C2 N7 117.9(6) . . ?
C4 N3 C2 113.3(6) . . ?
N3 C4 H4 116.6 . . ?
N3 C4 N5 126.7(6) . . ?
N5 C4 H4 116.6 . . ?
C6 N5 C4 112.8(6) . . ?
N1 C6 N5 127.5(6) . . ?
N1 C6 N16 114.8(6) . . ?
N5 C6 N16 117.7(6) . . ?
N8 N7 C2 120.6(6) . . ?
C15 N7 C2 127.2(6) . . ?
C15 N7 N8 112.1(6) . . ?
C9 N8 N7 103.9(6) . . ?
N8 C9 C10 123.9(7) . . ?
N8 C9 C14 112.3(6) . . ?
C14 C9 C10 123.8(7) . . ?
C9 C10 H10A 109.8 . . ?
C9 C10 H10B 109.8 . . ?
C9 C10 C11 109.2(6) . . ?
H10A C10 H10B 108.3 . . ?
C11 C10 H10A 109.8 . . ?
C11 C10 H10B 109.8 . . ?
C10 C11 H11A 109.3 . . ?
C10 C11 H11B 109.3 . . ?
H11A C11 H11B 108.0 . . ?
C12 C11 C10 111.5(7) . . ?
C12 C11 H11A 109.3 . . ?
C12 C11 H11B 109.3 . . ?
C11 C12 H12A 109.2 . . ?
C11 C12 H12B 109.2 . . ?
C11 C12 C13 112.1(7) . . ?
H12A C12 H12B 107.9 . . ?
C13 C12 H12A 109.2 . . ?
C13 C12 H12B 109.2 . . ?
C12 C13 H13A 109.7 . . ?
C12 C13 H13B 109.7 . . ?
H13A C13 H13B 108.2 . . ?
C14 C13 C12 109.6(6) . . ?
C14 C13 H13A 109.7 . . ?
C14 C13 H13B 109.7 . . ?
C9 C14 C13 123.0(6) . . ?
C15 C14 C9 105.0(6) . . ?
C15 C14 C13 131.9(7) . . ?
N7 C15 H15 126.6 . . ?
C14 C15 N7 106.7(6) . . ?
C14 C15 H15 126.6 . . ?
N17 N16 C6 120.6(5) . . ?
C24 N16 C6 127.2(6) . . ?
C24 N16 N17 112.1(5) . . ?
C18 N17 N16 103.8(5) . . ?
N17 C18 C19 124.0(6) . . ?
N17 C18 C23 112.3(6) . . ?
C23 C18 C19 123.6(6) . . ?
C18 C19 H19A 109.8 . . ?
C18 C19 H19B 109.8 . . ?
C18 C19 C20 109.4(6) . . ?
H19A C19 H19B 108.2 . . ?
C20 C19 H19A 109.8 . . ?
C20 C19 H19B 109.8 . . ?
C19 C20 H20A 109.2 . . ?
C19 C20 H20B 109.2 . . ?
H20A C20 H20B 107.9 . . ?
C21 C20 C19 111.9(7) . . ?
C21 C20 H20A 109.2 . . ?
C21 C20 H20B 109.2 . . ?
C20 C21 H21A 109.1 . . ?
C20 C21 H21B 109.1 . . ?
C20 C21 C22 112.3(7) . . ?
H21A C21 H21B 107.9 . . ?
C22 C21 H21A 109.1 . . ?
C22 C21 H21B 109.1 . . ?
C21 C22 H22A 109.9 . . ?
C21 C22 H22B 109.9 . . ?
H22A C22 H22B 108.3 . . ?
C23 C22 C21 109.0(6) . . ?
C23 C22 H22A 109.9 . . ?
C23 C22 H22B 109.9 . . ?
C18 C23 C22 123.0(6) . . ?
C24 C23 C18 104.4(6) . . ?
C24 C23 C22 132.5(6) . . ?
N16 C24 H24 126.3 . . ?
C23 C24 N16 107.3(6) . . ?
C23 C24 H24 126.3 . . ?
C26 N25 C30 113.3(6) . . ?
N25 C26 N27 126.7(6) . . ?
N25 C26 N31 115.1(6) . . ?
N27 C26 N31 118.2(6) . . ?
C28 N27 C26 112.9(6) . . ?
N27 C28 H28 116.3 . . ?
N29 C28 N27 127.5(6) . . ?
N29 C28 H28 116.3 . . ?
C28 N29 C30 112.7(6) . . ?
N25 C30 N29 126.9(6) . . ?
N25 C30 N40 114.9(6) . . ?
N29 C30 N40 118.1(6) . . ?
N32 N31 C26 121.0(5) . . ?
N32 N31 C39 112.2(5) . . ?
C39 N31 C26 126.6(6) . . ?
C33 N32 N31 104.1(5) . . ?
N32 C33 C34 124.0(6) . . ?
N32 C33 C38 112.5(6) . . ?
C38 C33 C34 123.5(6) . . ?
C33 C34 H34A 109.9 . . ?
C33 C34 H34B 109.9 . . ?
C33 C34 C35 109.0(6) . . ?
H34A C34 H34B 108.3 . . ?
C35 C34 H34A 109.9 . . ?
C35 C34 H34B 109.9 . . ?
C34 C35 H35A 109.4 . . ?
C34 C35 H35B 109.4 . . ?
H35A C35 H35B 108.0 . . ?
C36 C35 C34 111.1(6) . . ?
C36 C35 H35A 109.4 . . ?
C36 C35 H35B 109.4 . . ?
C35 C36 H36A 109.3 . . ?
C35 C36 H36B 109.3 . . ?
C35 C36 C37 111.5(6) . . ?
H36A C36 H36B 108.0 . . ?
C37 C36 H36A 109.3 . . ?
C37 C36 H36B 109.3 . . ?
C36 C37 H37A 109.7 . . ?
C36 C37 H37B 109.7 . . ?
H37A C37 H37B 108.2 . . ?
C38 C37 C36 109.8(6) . . ?
C38 C37 H37A 109.7 . . ?
C38 C37 H37B 109.7 . . ?
C33 C38 C37 123.4(6) . . ?
C39 C38 C33 105.0(6) . . ?
C39 C38 C37 131.5(7) . . ?
N31 C39 H39 126.9 . . ?
C38 C39 N31 106.3(6) . . ?
C38 C39 H39 126.9 . . ?
N41 N40 C30 122.1(6) . . ?
N41 N40 C48 111.9(6) . . ?
C48 N40 C30 125.9(6) . . ?
C42 N41 N40 104.2(6) . . ?
N41 C42 C43 123.8(7) . . ?
N41 C42 C47 112.3(6) . . ?
C47 C42 C43 123.8(7) . . ?
C42 C43 H43A 109.8 . . ?
C42 C43 H43B 109.8 . . ?
C42 C43 C44 109.5(7) . . ?
H43A C43 H43B 108.2 . . ?
C44 C43 H43A 109.8 . . ?
C44 C43 H43B 109.8 . . ?
C43 C44 H44A 109.2 . . ?
C43 C44 H44B 109.2 . . ?
H44A C44 H44B 107.9 . . ?
C45 C44 C43 112.2(7) . . ?
C45 C44 H44A 109.2 . . ?
C45 C44 H44B 109.2 . . ?
C44 C45 H45A 109.4 . . ?
C44 C45 H45B 109.4 . . ?
H45A C45 H45B 108.0 . . ?
C46 C45 C44 111.3(7) . . ?
C46 C45 H45A 109.4 . . ?
C46 C45 H45B 109.4 . . ?
C45 C46 H46A 109.9 . . ?
C45 C46 H46B 109.9 . . ?
H46A C46 H46B 108.3 . . ?
C47 C46 C45 108.7(7) . . ?
C47 C46 H46A 109.9 . . ?
C47 C46 H46B 109.9 . . ?
C42 C47 C46 123.3(7) . . ?
C48 C47 C42 105.1(6) . . ?
C48 C47 C46 131.6(7) . . ?
N40 C48 H48 126.7 . . ?
C47 C48 N40 106.6(6) . . ?
C47 C48 H48 126.7 . . ?
Cl50 C49 H49 108.6 . . ?
Cl50 C49 Cl52 109.3(5) . . ?
Cl51 C49 H49 108.6 . . ?
Cl51 C49 Cl50 111.5(4) . . ?
Cl51 C49 Cl52 110.2(4) . . ?
Cl52 C49 H49 108.6 . . ?
Cl54 C53 H53 108.6 . . ?
Cl54 C53 Cl55 109.9(4) . . ?
Cl55 C53 H53 108.6 . . ?
Cl56 C53 H53 108.6 . . ?
Cl56 C53 Cl54 110.5(4) . . ?
Cl56 C53 Cl55 110.5(5) . . ?
Cl58A C57A H57A 108.3 . . ?
Cl58A C57A Cl59A 111.4(9) . . ?
Cl58A C57A Cl60A 111.1(9) . . ?
Cl59A C57A H57A 108.3 . . ?
Cl59A C57A Cl60A 109.4(9) . . ?
Cl60A C57A H57A 108.3 . . ?
Cl58B C57B H57B 108.1 . . ?
Cl59B C57B H57B 108.1 . . ?
Cl59B C57B Cl58B 111.8(16) . . ?
Cl59B C57B Cl60B 111.2(16) . . ?
Cl60B C57B H57B 108.1 . . ?
Cl60B C57B Cl58B 109.4(15) . . ?
Cl62A C61A H61A 108.3 . . ?
Cl63A C61A H61A 108.3 . . ?
Cl63A C61A Cl62A 110.5(8) . . ?
Cl64A C61A H61A 108.3 . . ?
Cl64A C61A Cl62A 110.4(12) . . ?
Cl64A C61A Cl63A 110.9(10) . . ?
Cl62B C61B H61B 109.1 . . ?
Cl62B C61B Cl63B 110(2) . . ?
Cl62B C61B Cl64B 109(2) . . ?
Cl63B C61B H61B 109.1 . . ?
Cl63B C61B Cl64B 110(2) . . ?
Cl64B C61B H61B 109.1 . . ?

loop_
_geom_hbond_atom_site_label_D
_geom_hbond_atom_site_label_H
_geom_hbond_atom_site_label_A
_geom_hbond_distance_DH
_geom_hbond_distance_HA
_geom_hbond_distance_DA
_geom_hbond_angle_DHA
_geom_hbond_site_symmetry_A
C49 H49 N27 1.00 2.38 3.220(9) 141.7 .
C49 H49 N32 1.00 2.30 3.170(9) 145.2 .
C53 H53 N5 1.00 2.46 3.258(10) 135.9 .
C53 H53 N17 1.00 2.28 3.194(9) 151.6 .
C57A H57A N3 1.00 2.34 3.165(16) 138.8 .
C57A H57A N8 1.00 2.38 3.277(18) 149.5 .
C57B H57B N3 1.00 2.48 3.23(3) 130.8 .
C57B H57B N8 1.00 2.14 3.05(3) 152.0 .
C61A H61A N29 1.00 2.45 3.230(17) 134.1 .
C61A H61A N41 1.00 2.29 3.200(19) 151.0 .
C61B H61B N29 1.00 2.41 3.16(5) 131.0 .
C61B H61B N41 1.00 2.38 3.32(5) 157.0 .

_exptl_crystal_recrystallization_method 
'Re-crystallisation from solvent: chloroform'
####################################################################### 
# 
# 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_90-ncs
_database_code_depnum_ccdc_archive 'CCDC 1957590'
loop_
_audit_author_name
_audit_author_address
'Malcolm Halcrow' 'University of Leeds'
_audit_update_record             
;
2019-10-04 deposited with the CCDC.	2019-11-05 downloaded from the CCDC.
;
_audit_creation_date             2019-07-05
_audit_creation_method           
;
  Olex2 1.2
  (compiled Apr 23 2013 17:54:37, GUI svn.r4466)
;
_chemical_name_common            ?
_chemical_name_systematic        
'Catena-[2-amino-4,6-(pyrazol-1-yl)pyrimidine]-di-isothiocyanato iron(II)'
_chemical_formula_moiety         'C12 H9 Fe N9 S2'
_chemical_formula_sum            'C12 H9 Fe N9 S2'
_chemical_formula_weight         399.25
_chemical_melting_point          ?
loop_
_atom_type_symbol
_atom_type_description
_atom_type_scat_dispersion_real
_atom_type_scat_dispersion_imag
_atom_type_scat_source
C C 0.0032 0.0015 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
N N 0.0060 0.0030 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Fe Fe 0.3525 0.8017 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
S S 0.1181 0.1169 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'

_space_group_crystal_system      tetragonal
_space_group_IT_number           88
_space_group_name_H-M_alt        'I 41/a'
_space_group_name_Hall           '-I 4ad'
loop_
_space_group_symop_id
_space_group_symop_operation_xyz
1 'x, y, z'
2 '-y+3/4, x+1/4, z+1/4'
3 '-x, -y+1/2, z'
4 'y+1/4, -x+1/4, z+1/4'
5 'x+1/2, y+1/2, z+1/2'
6 '-y+5/4, x+3/4, z+3/4'
7 '-x+1/2, -y+1, z+1/2'
8 'y+3/4, -x+3/4, z+3/4'
9 '-x, -y, -z'
10 'y-3/4, -x-1/4, -z-1/4'
11 'x, y-1/2, -z'
12 '-y-1/4, x-1/4, -z-1/4'
13 '-x+1/2, -y+1/2, -z+1/2'
14 'y-1/4, -x+1/4, -z+1/4'
15 'x+1/2, y, -z+1/2'
16 '-y+1/4, x+1/4, -z+1/4'

_cell_length_a                   16.0404(2)
_cell_length_b                   16.0404(2)
_cell_length_c                   25.1086(3)
_cell_angle_alpha                90.00
_cell_angle_beta                 90.00
_cell_angle_gamma                90.00
_cell_volume                     6460.30(14)
_cell_formula_units_Z            16
_cell_measurement_reflns_used    2639

_cell_measurement_temperature    100(2)
_cell_measurement_theta_max      20.86
_cell_measurement_theta_min      1.46
_exptl_absorpt_coefficient_mu    1.114
_exptl_absorpt_correction_T_max  1.000
_exptl_absorpt_correction_T_min  0.994
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   
;
SADABS (Sheldrick, 2002).  University of Gottingen, Germany.
;
_exptl_crystal_colour            red
_exptl_crystal_density_diffrn    1.642
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       plate
_exptl_crystal_F_000             3232
_exptl_crystal_size_max          0.10
_exptl_crystal_size_mid          0.10
_exptl_crystal_size_min          0.03
_exptl_special_details           
;
 
;
_diffrn_reflns_av_R_equivalents  0.0681
_diffrn_reflns_av_unetI/netI     0.0628
_diffrn_reflns_limit_h_max       19
_diffrn_reflns_limit_h_min       -19
_diffrn_reflns_limit_k_max       18
_diffrn_reflns_limit_k_min       -16
_diffrn_reflns_limit_l_max       25
_diffrn_reflns_limit_l_min       -28
_diffrn_reflns_number            13505
_diffrn_reflns_theta_full        24.82
_diffrn_reflns_theta_max         24.91
_diffrn_reflns_theta_min         1.46
_diffrn_ambient_temperature      100(2)
_diffrn_detector_area_resol_mean ?
_diffrn_measured_fraction_theta_full 0.855
_diffrn_measured_fraction_theta_max 0.849
_diffrn_measurement_device       'Fixed χ 3-circle diffractometer'
_diffrn_measurement_device_type  'Fluid Film Devices'
_diffrn_measurement_method       'shutterless scans'
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_type           synchrotron
_diffrn_radiation_wavelength     0.68890
_diffrn_source                   'fine-focus sealed tube'
_diffrn_standards_decay_%        0
_diffrn_standards_interval_count 0
_diffrn_standards_interval_time  0
_diffrn_standards_number         0
_reflns_number_gt                1383
_reflns_number_total             2629
_reflns_threshold_expression     >2sigma(I)
_computing_cell_refinement       'CrysAlisPro, Agilent Technologies'
_computing_data_collection       '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         0.327
_refine_diff_density_min         -0.412
_refine_diff_density_rms         0.062
_refine_ls_extinction_coef       ?
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   0.904
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     223
_refine_ls_number_reflns         2629
_refine_ls_number_restraints     2
_refine_ls_R_factor_all          0.1067
_refine_ls_R_factor_gt           0.0558
_refine_ls_restrained_S_all      0.904
_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)+(0.1050P)²+0.0000P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1533
_refine_ls_wR_factor_ref         0.1753
_refine_special_details          
;
 Refinement of F² against ALL reflections.  The weighted R-factor wR and 
 goodness of fit S are based on F², conventional R-factors R are based 
 on F, with F set to zero for negative F². The threshold expression of 
 F² > 2sigma(F²) is used only for calculating R-factors(gt) etc. and is 
 not relevant to the choice of reflections for refinement.  R-factors based 
 on F² are statistically about twice as large as those based on F, and R- 
 factors based on ALL data will be even larger. 

 No disorder is present in the model, and no restraints were applied to the
 refinement. All non-H atoms were refined anisotropically, and C-bound H 
 atoms were placed in calculated positions and refined using a riding model.
 The amino H atoms H14A and H14B were located in the Fourier map and 
 refined, with the restraint N---H = 0.90(2) Å and the constraint
 Uiso = 1.5xUeq{N14}.
;
_olex2_refinement_description    
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups
 At 1.5 times of:
  All N(H,H) groups
2. Restrained distances
 N14-H14A = N14-H14B
 0.9 with sigma of 0.02
3.a Aromatic/amide H refined with riding coordinates:
 C11(H11), C17(H17), C18(H18), C19(H19), C22(H22), C23(H23), C24(H24)
;
_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 0.72162(6) 0.52868(6) 0.81256(2) 0.0878(4) Uani 1 1 d . . .
N2 N 0.8387(4) 0.5679(4) 0.79378(16) 0.1036(18) Uani 1 1 d . . .
C3 C 0.9001(5) 0.5862(4) 0.8141(2) 0.0957(19) Uani 1 1 d . . .
S4 S 0.98794(12) 0.61592(12) 0.84133(7) 0.1089(6) Uani 1 1 d . . .
N5 N 0.7751(4) 0.4091(4) 0.82184(17) 0.0975(16) Uani 1 1 d . . .
C6 C 0.8116(4) 0.3525(5) 0.8068(2) 0.0908(19) Uani 1 1 d . . .
S7 S 0.86593(12) 0.27174(12) 0.78528(8) 0.1164(7) Uani 1 1 d . . .
C8 C 0.7008(4) 0.4960(4) 0.68826(16) 0.0796(16) Uani 1 1 d . . .
N9 N 0.6652(3) 0.4882(3) 0.73688(13) 0.0745(12) Uani 1 1 d . . .
C10 C 0.5927(4) 0.4490(4) 0.73896(17) 0.0782(15) Uani 1 1 d . . .
C11 C 0.5513(3) 0.4173(4) 0.69533(17) 0.0779(15) Uani 1 1 d . . .
H11 H 0.4994 0.3891 0.6979 0.093 Uiso 1 1 calc R . .
C12 C 0.5918(4) 0.4300(4) 0.64759(18) 0.0797(15) Uani 1 1 d . . .
N13 N 0.6659(3) 0.4672(3) 0.64291(13) 0.0801(13) Uani 1 1 d . . .
N14 N 0.7738(4) 0.5329(4) 0.68492(14) 0.1038(18) Uani 1 1 d D . .
H14A H 0.802(4) 0.549(4) 0.7142(18) 0.156 Uiso 1 1 d D . .
H14B H 0.798(4) 0.528(5) 0.6534(15) 0.156 Uiso 1 1 d D . .
N15 N 0.5590(3) 0.4415(3) 0.79033(15) 0.0794(13) Uani 1 1 d . . .
N16 N 0.5998(3) 0.4771(3) 0.83192(15) 0.0821(13) Uani 1 1 d . . .
C17 C 0.5537(4) 0.4584(4) 0.8742(2) 0.0894(18) Uani 1 1 d . . .
H17 H 0.5672 0.4744 0.9096 0.107 Uiso 1 1 calc R . .
C18 C 0.4844(4) 0.4132(4) 0.8606(2) 0.105(2) Uani 1 1 d . . .
H18 H 0.4420 0.3938 0.8839 0.126 Uiso 1 1 calc R . .
C19 C 0.4883(4) 0.4017(4) 0.8067(2) 0.0942(18) Uani 1 1 d . . .
H19 H 0.4497 0.3720 0.7851 0.113 Uiso 1 1 calc R . .
N20 N 0.5559(3) 0.4024(3) 0.59983(15) 0.0870(14) Uani 1 1 d . . .
N21 N 0.5984(3) 0.4155(3) 0.55322(16) 0.0955(15) Uani 1 1 d . . .
C22 C 0.5486(5) 0.3855(5) 0.5160(2) 0.115(2) Uani 1 1 d . . .
H22 H 0.5614 0.3859 0.4790 0.138 Uiso 1 1 calc R . .
C23 C 0.4766(5) 0.3539(6) 0.5368(3) 0.134(3) Uani 1 1 d . . .
H23 H 0.4312 0.3305 0.5176 0.161 Uiso 1 1 calc R . .
C24 C 0.4831(4) 0.3629(5) 0.5923(3) 0.111(2) Uani 1 1 d . . .
H24 H 0.4445 0.3450 0.6187 0.133 Uiso 1 1 calc R . .


_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 2.036(6) . ?
Fe1 N5 2.113(6) . ?
Fe1 N9 2.202(4) . ?
Fe1 N13 2.206(4) 4_565 ?
Fe1 N16 2.178(5) . ?
Fe1 N21 2.181(5) 4_565 ?
N2 C3 1.146(8) . ?
C3 S4 1.638(8) . ?
N5 C6 1.146(8) . ?
C6 S7 1.651(8) . ?
C8 N9 1.354(6) . ?
C8 N13 1.350(6) . ?
C8 N14 1.315(8) . ?
N9 C10 1.323(6) . ?
C10 C11 1.378(7) . ?
C10 N15 1.404(6) . ?
C11 H11 0.9500 . ?
C11 C12 1.378(7) . ?
C12 N13 1.335(7) . ?
C12 N20 1.402(6) . ?
N14 H14A 0.90(2) . ?
N14 H14B 0.89(2) . ?
N15 N16 1.358(6) . ?
N15 C19 1.365(7) . ?
N16 C17 1.327(6) . ?
C17 H17 0.9500 . ?
C17 C18 1.371(8) . ?
C18 H18 0.9500 . ?
C18 C19 1.366(7) . ?
C19 H19 0.9500 . ?
N20 N21 1.370(6) . ?
N20 C24 1.342(8) . ?
N21 C22 1.320(7) . ?
C22 H22 0.9500 . ?
C22 C23 1.366(10) . ?
C23 H23 0.9500 . ?
C23 C24 1.405(9) . ?
C24 H24 0.9500 . ?

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 N5 86.1(2) . . ?
N2 Fe1 N9 105.67(17) . . ?
N2 Fe1 N13 96.73(18) . 4_565 ?
N2 Fe1 N16 175.6(2) . . ?
N2 Fe1 N21 94.4(2) . 4_565 ?
N5 Fe1 N9 89.68(17) . . ?
N5 Fe1 N13 106.14(17) . 4_565 ?
N5 Fe1 N16 89.69(19) . . ?
N5 Fe1 N21 179.5(2) . 4_565 ?
N9 Fe1 N13 153.46(18) . 4_565 ?
N16 Fe1 N9 73.25(15) . . ?
N16 Fe1 N13 85.42(15) . 4_565 ?
N16 Fe1 N21 89.83(18) . 4_565 ?
N21 Fe1 N9 90.23(16) 4_565 . ?
N21 Fe1 N13 73.77(17) 4_565 4_565 ?
C3 N2 Fe1 140.2(4) . . ?
N2 C3 S4 177.6(6) . . ?
C6 N5 Fe1 153.0(5) . . ?
N5 C6 S7 179.0(6) . . ?
N13 C8 N9 123.6(5) . . ?
N14 C8 N9 118.3(4) . . ?
N14 C8 N13 118.0(4) . . ?
C8 N9 Fe1 125.3(4) . . ?
C10 N9 Fe1 117.8(3) . . ?
C10 N9 C8 116.7(4) . . ?
N9 C10 C11 124.6(4) . . ?
N9 C10 N15 114.6(4) . . ?
C11 C10 N15 120.8(5) . . ?
C10 C11 H11 122.9 . . ?
C12 C11 C10 114.2(5) . . ?
C12 C11 H11 122.9 . . ?
C11 C12 N20 120.2(5) . . ?
N13 C12 C11 124.2(5) . . ?
N13 C12 N20 115.6(5) . . ?
C8 N13 Fe1 126.4(4) . 6_544 ?
C12 N13 Fe1 117.0(3) . 6_544 ?
C12 N13 C8 116.6(4) . . ?
C8 N14 H14A 121(5) . . ?
C8 N14 H14B 114(5) . . ?
H14A N14 H14B 122(7) . . ?
N16 N15 C10 119.0(5) . . ?
N16 N15 C19 111.4(4) . . ?
C19 N15 C10 129.6(5) . . ?
N15 N16 Fe1 114.9(3) . . ?
C17 N16 Fe1 139.8(4) . . ?
C17 N16 N15 104.6(4) . . ?
N16 C17 H17 124.1 . . ?
N16 C17 C18 111.8(5) . . ?
C18 C17 H17 124.1 . . ?
C17 C18 H18 126.9 . . ?
C19 C18 C17 106.3(5) . . ?
C19 C18 H18 126.9 . . ?
N15 C19 C18 105.9(5) . . ?
N15 C19 H19 127.1 . . ?
C18 C19 H19 127.1 . . ?
N21 N20 C12 118.6(5) . . ?
C24 N20 C12 128.8(5) . . ?
C24 N20 N21 112.6(4) . . ?
N20 N21 Fe1 114.9(3) . 6_544 ?
C22 N21 Fe1 140.7(5) . 6_544 ?
C22 N21 N20 104.4(5) . . ?
N21 C22 H22 124.0 . . ?
N21 C22 C23 112.0(6) . . ?
C23 C22 H22 124.0 . . ?
C22 C23 H23 126.9 . . ?
C22 C23 C24 106.2(6) . . ?
C24 C23 H23 126.9 . . ?
N20 C24 C23 104.7(6) . . ?
N20 C24 H24 127.7 . . ?
C23 C24 H24 127.7 . . ?

loop_
_geom_hbond_atom_site_label_D
_geom_hbond_atom_site_label_H
_geom_hbond_atom_site_label_A
_geom_hbond_distance_DH
_geom_hbond_distance_HA
_geom_hbond_distance_DA
_geom_hbond_angle_DHA
_geom_hbond_site_symmetry_A
N14 H14A N2 0.90(2) 2.11(3) 2.978(6) 164(7) .
N14 H14B N5 0.89(2) 2.16(2) 3.038(6) 171(7) 6_544

_olex2_submission_special_instructions 'No special instructions were received'

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

data_150-se
_database_code_depnum_ccdc_archive 'CCDC 1957586'
loop_
_audit_author_name
_audit_author_address
'Malcolm Halcrow' 'University of Leeds'
_audit_update_record             
;
2019-10-04 deposited with the CCDC.	2019-11-05 downloaded from the CCDC.
;
_audit_creation_date             2019-07-05
_audit_creation_method           
;
  Olex2 1.2
  (compiled Apr 23 2013 17:54:37, GUI svn.r4466)
;
_chemical_name_common            ?
_chemical_name_systematic        
'Bis-[4,6-di(pyrazol-1-yl)pyrimidine]-di[isoselenocyanato]iron(II)hemi-ethanol solvate'
_chemical_formula_moiety         'C22 H16 Fe N14 Se2, 0.5(C2 H6 O)'
_chemical_formula_sum            'C23 H19 Fe N14 O0.50 Se2'
_chemical_formula_weight         713.29
_chemical_melting_point          ?
loop_
_atom_type_symbol
_atom_type_description
_atom_type_scat_dispersion_real
_atom_type_scat_dispersion_imag
_atom_type_scat_source
C C 0.0181 0.0091 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
N N 0.0311 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'
Se Se -0.7943 1.1372 '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'

_space_group_crystal_system      monoclinic
_space_group_IT_number           14
_space_group_name_H-M_alt        'P 1 21/n 1'
_space_group_name_Hall           '-P 2yn'
loop_
_space_group_symop_id
_space_group_symop_operation_xyz
1 'x, y, z'
2 '-x+1/2, y+1/2, -z+1/2'
3 '-x, -y, -z'
4 'x-1/2, -y-1/2, z-1/2'

_cell_length_a                   12.6992(7)
_cell_length_b                   14.4699(6)
_cell_length_c                   16.2226(9)
_cell_angle_alpha                90.00
_cell_angle_beta                 108.645(6)
_cell_angle_gamma                90.00
_cell_volume                     2824.6(3)
_cell_formula_units_Z            4
_cell_measurement_reflns_used    4661
_cell_measurement_temperature    120(2)
_cell_measurement_theta_min      4.18
_cell_measurement_theta_max      72.15
_exptl_absorpt_coefficient_mu    7.598
_exptl_absorpt_correction_T_min  0.868
_exptl_absorpt_correction_T_max  1.000
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   
; 
CrysAlisPro, Agilent Technologies,
Version 1.171.36.24 (release 03-12-2012 CrysAlis171 .NET)
Empirical absorption correction using spherical harmonics,
 implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_crystal_colour            yellow
_exptl_crystal_density_diffrn    1.677
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       lath
_exptl_crystal_F_000             1412
_exptl_crystal_size_max          0.30
_exptl_crystal_size_mid          0.20
_exptl_crystal_size_min          0.10
_exptl_special_details           
;
 ? 
;
_diffrn_reflns_av_R_equivalents  0.0261
_diffrn_reflns_av_unetI/netI     0.0367
_diffrn_reflns_limit_h_max       13
_diffrn_reflns_limit_h_min       -15
_diffrn_reflns_limit_k_max       15
_diffrn_reflns_limit_k_min       -17
_diffrn_reflns_limit_l_max       19
_diffrn_reflns_limit_l_min       -19
_diffrn_reflns_number            11028
_diffrn_reflns_theta_full        72.00
_diffrn_reflns_theta_max         73.42
_diffrn_reflns_theta_min         3.87
_diffrn_ambient_temperature      120(2)
_diffrn_detector_area_resol_mean 5.3095
_diffrn_measured_fraction_theta_full 0.990
_diffrn_measured_fraction_theta_max 0.975
_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                4736
_reflns_number_total             5540
_reflns_threshold_expression     >2sigma(I)
_computing_cell_refinement       'CrysAlisPro, Agilent Technologies'
_computing_data_collection       '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         0.363
_refine_diff_density_min         -0.377
_refine_diff_density_rms         0.060
_refine_ls_extinction_coef       ?
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.030
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     387
_refine_ls_number_reflns         5540
_refine_ls_number_restraints     6
_refine_ls_R_factor_all          0.0410
_refine_ls_R_factor_gt           0.0322
_refine_ls_restrained_S_all      1.031
_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)+(0.0315P)²+1.1180P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0727
_refine_ls_wR_factor_ref         0.0773
_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 Se atoms in the model had a larger displacement ellipsoid than
 the other atoms in the molecule, and was refined without restraints over 
 two half-occupied disorder sites. The solvent half-molecule occupies a 
 cavity spanning the crystallographic inversion centre, and is disordered 
 over two sites with occupancies of 0.30 and 0.20. These were treated with
 the fixed restraints C---C = 1.5(2), C---O = 1.40(2) and 1,3-C...O = 
 2.37(2) Å. 

 All non-H atoms except the disordered solvent were refined anisotropically 
 and H atoms were placed in calculated positions and refined using a
 riding model. 
;
_olex2_refinement_description    
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups, All C(H,H) groups, All O(H) groups
 At 1.5 times of:
  All C(H,H,H) groups
2. Restrained distances
 C40A-C41A = C40B-C41B
 1.5 with sigma of 0.02
 C41A-O42A = C41B-O42B
 1.4 with sigma of 0.02
 C40A-O42A = C40B-O42B
 2.37 with sigma of 0.02
3. Others
 Fixed Sof: Se7A(0.57) Se7B(0.43) C40A(0.3) H40A(0.3) H40B(0.3) H40C(0.3)
 C41A(0.3) H41A(0.3) H41B(0.3) O42A(0.3) H42A(0.3) C40B(0.2) H40E(0.2)
 H40F(0.2) H40D(0.2) C41B(0.2) H41C(0.2) H41D(0.2) O42B(0.2) H42B(0.2)
4.a Secondary CH2 refined with riding coordinates:
 C41A(H41A,H41B), C41B(H41C,H41D)
4.b Me refined with riding coordinates:
 C40A(H40A,H40B,H40C), C40B(H40E,H40F,H40D)
4.c Aromatic/amide H refined with riding coordinates:
 C8(H8), C11(H11), C16(H16), C17(H17), C18(H18), C21(H21), C22(H22), C23(H23),
 C24(H24), C27(H27), C32(H32), C33(H33), C34(H34), C37(H37), C38(H38), C39(H39)
4.d Idealised tetrahedral OH refined as rotating group:
 O42A(H42A), O42B(H42B)
;
_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 0.40961(3) 0.75129(3) 0.73876(2) 0.02515(9) Uani 1 1 d . . .
N2 N 0.54519(18) 0.66396(17) 0.79699(15) 0.0331(5) Uani 1 1 d . . .
C3 C 0.6103(2) 0.61826(18) 0.84636(17) 0.0292(5) Uani 1 1 d . . .
Se4 Se 0.70671(2) 0.54709(2) 0.926621(19) 0.03482(9) Uani 1 1 d . . .
N5 N 0.3073(2) 0.64446(17) 0.67780(16) 0.0370(5) Uani 1 1 d . A .
C6 C 0.2319(2) 0.6036(2) 0.63619(17) 0.0341(6) Uani 1 1 d . . .
Se7A Se 0.1212(3) 0.5332(2) 0.5701(2) 0.0458(5) Uani 0.57 1 d P A 1
Se7B Se 0.1034(4) 0.5507(3) 0.5758(3) 0.0544(9) Uani 0.43 1 d P A 2
C8 C 0.4236(2) 0.7137(2) 0.93669(17) 0.0351(6) Uani 1 1 d . . .
H8 H 0.4874 0.6788 0.9380 0.042 Uiso 1 1 calc R . .
N9 N 0.37243(18) 0.75973(16) 0.86261(14) 0.0300(5) Uani 1 1 d . . .
C10 C 0.2837(2) 0.80957(18) 0.86226(17) 0.0291(5) Uani 1 1 d . . .
C11 C 0.2465(2) 0.81549(19) 0.93362(18) 0.0328(6) Uani 1 1 d . . .
H11 H 0.1847 0.8525 0.9336 0.039 Uiso 1 1 calc R . .
C12 C 0.3058(2) 0.76378(19) 1.00469(17) 0.0322(6) Uani 1 1 d . . .
N13 N 0.39410(19) 0.71211(18) 1.00781(15) 0.0358(5) Uani 1 1 d . . .
N14 N 0.22780(18) 0.85368(16) 0.78399(15) 0.0318(5) Uani 1 1 d . . .
N15 N 0.26419(18) 0.84073(16) 0.71409(14) 0.0303(5) Uani 1 1 d . . .
C16 C 0.1908(2) 0.8835(2) 0.64869(18) 0.0364(6) Uani 1 1 d . . .
H16 H 0.1941 0.8856 0.5910 0.044 Uiso 1 1 calc R . .
C17 C 0.1072(2) 0.9256(2) 0.6752(2) 0.0423(7) Uani 1 1 d . . .
H17 H 0.0458 0.9607 0.6405 0.051 Uiso 1 1 calc R . .
C18 C 0.1330(2) 0.9053(2) 0.7612(2) 0.0408(7) Uani 1 1 d . . .
H18 H 0.0925 0.9237 0.7985 0.049 Uiso 1 1 calc R . .
N19 N 0.2742(2) 0.76257(17) 1.07963(15) 0.0351(5) Uani 1 1 d . . .
N20 N 0.1951(2) 0.82320(18) 1.08732(18) 0.0444(6) Uani 1 1 d . . .
C21 C 0.1879(3) 0.8041(2) 1.1652(2) 0.0508(9) Uani 1 1 d . . .
H21 H 0.1398 0.8357 1.1900 0.061 Uiso 1 1 calc R . .
C22 C 0.2589(3) 0.7320(3) 1.2073(2) 0.0510(9) Uani 1 1 d . . .
H22 H 0.2671 0.7065 1.2629 0.061 Uiso 1 1 calc R . .
C23 C 0.3138(2) 0.7065(3) 1.15052(18) 0.0444(7) Uani 1 1 d . . .
H23 H 0.3683 0.6593 1.1588 0.053 Uiso 1 1 calc R . .
C24 C 0.4041(2) 0.74921(18) 0.53861(17) 0.0295(5) Uani 1 1 d . . .
H24 H 0.3505 0.7018 0.5329 0.035 Uiso 1 1 calc R . .
N25 N 0.43920(16) 0.79390(15) 0.61562(13) 0.0254(4) Uani 1 1 d . . .
C26 C 0.51053(19) 0.86304(16) 0.62042(16) 0.0240(5) Uani 1 1 d . . .
C27 C 0.5473(2) 0.88914(17) 0.55245(16) 0.0253(5) Uani 1 1 d . . .
H27 H 0.5956 0.9402 0.5561 0.030 Uiso 1 1 calc R . .
C28 C 0.50847(19) 0.83507(17) 0.47865(15) 0.0246(5) Uani 1 1 d . . .
N29 N 0.43705(17) 0.76502(16) 0.47016(14) 0.0292(4) Uani 1 1 d . . .
N30 N 0.54991(17) 0.90565(14) 0.70179(13) 0.0259(4) Uani 1 1 d . . .
N31 N 0.51785(17) 0.87094(15) 0.76872(14) 0.0288(4) Uani 1 1 d . . .
C32 C 0.5750(2) 0.9186(2) 0.83771(17) 0.0354(6) Uani 1 1 d . . .
H32 H 0.5700 0.9096 0.8944 0.042 Uiso 1 1 calc R . .
C33 C 0.6437(3) 0.9839(2) 0.81712(19) 0.0385(6) Uani 1 1 d . . .
H33 H 0.6922 1.0264 0.8556 0.046 Uiso 1 1 calc R . .
C34 C 0.6267(2) 0.97387(18) 0.73043(18) 0.0331(6) Uani 1 1 d . . .
H34 H 0.6617 1.0080 0.6964 0.040 Uiso 1 1 calc R . .
N35 N 0.54523(17) 0.85043(15) 0.40728(14) 0.0270(4) Uani 1 1 d . . .
N36 N 0.6216(2) 0.91815(16) 0.40968(15) 0.0347(5) Uani 1 1 d . . .
C37 C 0.6366(2) 0.9116(2) 0.33286(19) 0.0372(6) Uani 1 1 d . . .
H37 H 0.6858 0.9501 0.3149 0.045 Uiso 1 1 calc R . .
C38 C 0.5723(2) 0.8421(2) 0.28091(18) 0.0389(6) Uani 1 1 d . . .
H38 H 0.5693 0.8252 0.2236 0.047 Uiso 1 1 calc R . .
C39 C 0.5148(2) 0.8037(2) 0.33022(17) 0.0346(6) Uani 1 1 d . . .
H39 H 0.4635 0.7539 0.3141 0.041 Uiso 1 1 calc R . .
C40A C 0.4575(13) 0.4987(10) 0.5167(10) 0.049(4) Uiso 0.30 1 d PD B 1
H40A H 0.4789 0.4424 0.5516 0.074 Uiso 0.30 1 calc PR B 1
H40B H 0.3772 0.4983 0.4867 0.074 Uiso 0.30 1 calc PR B 1
H40C H 0.4771 0.5529 0.5548 0.074 Uiso 0.30 1 calc PR B 1
C41A C 0.5179(12) 0.5028(7) 0.4507(9) 0.036(2) Uiso 0.30 1 d PD B 1
H41A H 0.5989 0.5008 0.4812 0.044 Uiso 0.30 1 calc PR B 1
H41B H 0.4978 0.4479 0.4124 0.044 Uiso 0.30 1 calc PR B 1
O42A O 0.4928(8) 0.5808(6) 0.4011(6) 0.042(2) Uiso 0.30 1 d PD B 1
H42A H 0.4918 0.6263 0.4329 0.051 Uiso 0.30 1 calc PR B 1
C40B C 0.494(7) 0.501(4) 0.510(2) 0.099(10) Uiso 0.20 1 d PD C 2
H40E H 0.5137 0.4371 0.5304 0.148 Uiso 0.20 1 calc PR C 2
H40F H 0.4242 0.5177 0.5203 0.148 Uiso 0.20 1 calc PR C 2
H40D H 0.5531 0.5427 0.5426 0.148 Uiso 0.20 1 calc PR C 2
C41B C 0.479(2) 0.5067(13) 0.4168(16) 0.073(7) Uiso 0.20 1 d PD C 2
H41C H 0.5457 0.4788 0.4071 0.087 Uiso 0.20 1 calc PR C 2
H41D H 0.4148 0.4680 0.3853 0.087 Uiso 0.20 1 calc PR C 2
O42B O 0.4643(12) 0.5921(9) 0.3796(9) 0.045(3) Uiso 0.20 1 d PD C 2
H42B H 0.4177 0.6216 0.3962 0.054 Uiso 0.20 1 calc PR C 2


_geom_special_details            
;
 All esds (except the esd in the dihedral angle between two l.s. planes) 
 are estimated using the full covariance matrix.  The cell esds are taken 
 into account individually in the estimation of esds in distances, angles 
 and torsion angles; correlations between esds in cell parameters are only 
 used when they are defined by crystal symmetry.  An approximate (isotropic) 
 treatment of cell esds is used for estimating esds involving l.s. planes. 
;
loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
_geom_bond_publ_flag
Fe1 N2 2.101(2) . ?
Fe1 N5 2.057(2) . ?
Fe1 N9 2.209(2) . ?
Fe1 N15 2.185(2) . ?
Fe1 N25 2.234(2) . ?
Fe1 N31 2.167(2) . ?
N2 C3 1.157(4) . ?
C3 Se4 1.799(3) . ?
N5 C6 1.144(4) . ?
C6 Se7A 1.790(5) . ?
C6 Se7B 1.785(6) . ?
C8 H8 0.9500 . ?
C8 N9 1.345(4) . ?
C8 N13 1.322(3) . ?
N9 C10 1.337(3) . ?
C10 C11 1.385(3) . ?
C10 N14 1.395(3) . ?
C11 H11 0.9500 . ?
C11 C12 1.379(4) . ?
C12 N13 1.336(4) . ?
C12 N19 1.396(3) . ?
N14 N15 1.367(3) . ?
N14 C18 1.363(4) . ?
N15 C16 1.321(4) . ?
C16 H16 0.9500 . ?
C16 C17 1.405(4) . ?
C17 H17 0.9500 . ?
C17 C18 1.359(4) . ?
C18 H18 0.9500 . ?
N19 N20 1.369(4) . ?
N19 C23 1.365(4) . ?
N20 C21 1.325(4) . ?
C21 H21 0.9500 . ?
C21 C22 1.405(6) . ?
C22 H22 0.9500 . ?
C22 C23 1.371(4) . ?
C23 H23 0.9500 . ?
C24 H24 0.9500 . ?
C24 N25 1.350(3) . ?
C24 N29 1.326(3) . ?
N25 C26 1.335(3) . ?
C26 C27 1.381(3) . ?
C26 N30 1.397(3) . ?
C27 H27 0.9500 . ?
C27 C28 1.383(4) . ?
C28 N29 1.338(3) . ?
C28 N35 1.398(3) . ?
N30 N31 1.371(3) . ?
N30 C34 1.361(3) . ?
N31 C32 1.317(4) . ?
C32 H32 0.9500 . ?
C32 C33 1.397(4) . ?
C33 H33 0.9500 . ?
C33 C34 1.361(4) . ?
C34 H34 0.9500 . ?
N35 N36 1.370(3) . ?
N35 C39 1.364(3) . ?
N36 C37 1.323(4) . ?
C37 H37 0.9500 . ?
C37 C38 1.396(4) . ?
C38 H38 0.9500 . ?
C38 C39 1.362(4) . ?
C39 H39 0.9500 . ?
C40A H40A 0.9800 . ?
C40A H40B 0.9800 . ?
C40A H40C 0.9800 . ?
C40A C41A 1.504(12) . ?
C41A H41A 0.9900 . ?
C41A H41B 0.9900 . ?
C41A O42A 1.363(12) . ?
O42A H42A 0.8400 . ?
C40B H40E 0.9800 . ?
C40B H40F 0.9800 . ?
C40B H40D 0.9800 . ?
C40B C41B 1.472(19) . ?
C41B H41C 0.9900 . ?
C41B H41D 0.9900 . ?
C41B O42B 1.362(17) . ?
O42B H42B 0.8400 . ?

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 90.40(8) . . ?
N2 Fe1 N15 164.14(8) . . ?
N2 Fe1 N25 102.72(8) . . ?
N2 Fe1 N31 90.56(9) . . ?
N5 Fe1 N2 93.72(10) . . ?
N5 Fe1 N9 101.13(9) . . ?
N5 Fe1 N15 89.44(9) . . ?
N5 Fe1 N25 92.20(9) . . ?
N5 Fe1 N31 164.96(9) . . ?
N9 Fe1 N25 160.69(8) . . ?
N15 Fe1 N9 73.73(8) . . ?
N15 Fe1 N25 92.68(8) . . ?
N31 Fe1 N9 93.24(8) . . ?
N31 Fe1 N15 90.35(8) . . ?
N31 Fe1 N25 72.79(8) . . ?
C3 N2 Fe1 163.05(19) . . ?
N2 C3 Se4 176.9(2) . . ?
C6 N5 Fe1 162.3(2) . . ?
N5 C6 Se7A 175.6(3) . . ?
N5 C6 Se7B 172.5(3) . . ?
N9 C8 H8 116.6 . . ?
N13 C8 H8 116.6 . . ?
N13 C8 N9 126.7(2) . . ?
C8 N9 Fe1 127.06(17) . . ?
C10 N9 Fe1 116.82(17) . . ?
C10 N9 C8 115.9(2) . . ?
N9 C10 C11 122.8(2) . . ?
N9 C10 N14 115.7(2) . . ?
C11 C10 N14 121.5(2) . . ?
C10 C11 H11 122.4 . . ?
C12 C11 C10 115.1(2) . . ?
C12 C11 H11 122.4 . . ?
C11 C12 N19 120.2(2) . . ?
N13 C12 C11 124.2(2) . . ?
N13 C12 N19 115.5(3) . . ?
C8 N13 C12 115.2(2) . . ?
N15 N14 C10 118.9(2) . . ?
C18 N14 C10 130.2(2) . . ?
C18 N14 N15 110.7(2) . . ?
N14 N15 Fe1 114.79(16) . . ?
C16 N15 Fe1 139.70(19) . . ?
C16 N15 N14 105.3(2) . . ?
N15 C16 H16 124.3 . . ?
N15 C16 C17 111.4(3) . . ?
C17 C16 H16 124.3 . . ?
C16 C17 H17 127.4 . . ?
C18 C17 C16 105.2(3) . . ?
C18 C17 H17 127.4 . . ?
N14 C18 H18 126.3 . . ?
C17 C18 N14 107.4(2) . . ?
C17 C18 H18 126.3 . . ?
N20 N19 C12 119.6(3) . . ?
C23 N19 C12 127.6(3) . . ?
C23 N19 N20 112.8(2) . . ?
C21 N20 N19 103.3(3) . . ?
N20 C21 H21 123.6 . . ?
N20 C21 C22 112.9(3) . . ?
C22 C21 H21 123.6 . . ?
C21 C22 H22 127.5 . . ?
C23 C22 C21 105.0(3) . . ?
C23 C22 H22 127.5 . . ?
N19 C23 C22 106.0(3) . . ?
N19 C23 H23 127.0 . . ?
C22 C23 H23 127.0 . . ?
N25 C24 H24 116.8 . . ?
N29 C24 H24 116.8 . . ?
N29 C24 N25 126.4(2) . . ?
C24 N25 Fe1 126.52(17) . . ?
C26 N25 Fe1 117.36(16) . . ?
C26 N25 C24 115.5(2) . . ?
N25 C26 C27 123.7(2) . . ?
N25 C26 N30 114.7(2) . . ?
C27 C26 N30 121.6(2) . . ?
C26 C27 H27 122.6 . . ?
C26 C27 C28 114.8(2) . . ?
C28 C27 H27 122.6 . . ?
C27 C28 N35 120.4(2) . . ?
N29 C28 C27 124.1(2) . . ?
N29 C28 N35 115.5(2) . . ?
C24 N29 C28 115.5(2) . . ?
N31 N30 C26 118.7(2) . . ?
C34 N30 C26 130.1(2) . . ?
C34 N30 N31 110.9(2) . . ?
N30 N31 Fe1 116.28(15) . . ?
C32 N31 Fe1 138.26(18) . . ?
C32 N31 N30 105.0(2) . . ?
N31 C32 H32 124.2 . . ?
N31 C32 C33 111.5(2) . . ?
C33 C32 H32 124.2 . . ?
C32 C33 H33 127.2 . . ?
C34 C33 C32 105.7(2) . . ?
C34 C33 H33 127.2 . . ?
N30 C34 H34 126.6 . . ?
C33 C34 N30 106.8(2) . . ?
C33 C34 H34 126.6 . . ?
N36 N35 C28 120.7(2) . . ?
C39 N35 C28 127.5(2) . . ?
C39 N35 N36 111.8(2) . . ?
C37 N36 N35 103.6(2) . . ?
N36 C37 H37 123.6 . . ?
N36 C37 C38 112.8(2) . . ?
C38 C37 H37 123.6 . . ?
C37 C38 H38 127.5 . . ?
C39 C38 C37 105.0(2) . . ?
C39 C38 H38 127.5 . . ?
N35 C39 H39 126.6 . . ?
C38 C39 N35 106.7(2) . . ?
C38 C39 H39 126.6 . . ?
H40A C40A H40B 109.5 . . ?
H40A C40A H40C 109.5 . . ?
H40B C40A H40C 109.5 . . ?
C41A C40A H40A 109.5 . . ?
C41A C40A H40B 109.5 . . ?
C41A C40A H40C 109.5 . . ?
C40A C41A H41A 109.2 . . ?
C40A C41A H41B 109.2 . . ?
H41A C41A H41B 107.9 . . ?
O42A C41A C40A 112.2(8) . . ?
O42A C41A H41A 109.2 . . ?
O42A C41A H41B 109.2 . . ?
H40E C40B H40F 109.5 . . ?
H40E C40B H40D 109.5 . . ?
H40F C40B H40D 109.5 . . ?
C41B C40B H40E 109.5 . . ?
C41B C40B H40F 109.5 . . ?
C41B C40B H40D 109.5 . . ?
C40B C41B H41C 107.9 . . ?
C40B C41B H41D 107.9 . . ?
H41C C41B H41D 107.2 . . ?
O42B C41B C40B 118(2) . . ?
O42B C41B H41C 107.9 . . ?
O42B C41B H41D 107.9 . . ?
C41B O42B H42B 109.5 . . ?

loop_
_geom_hbond_atom_site_label_D
_geom_hbond_atom_site_label_H
_geom_hbond_atom_site_label_A
_geom_hbond_distance_DH
_geom_hbond_distance_HA
_geom_hbond_distance_DA
_geom_hbond_angle_DHA
_geom_hbond_site_symmetry_A
O42A H42A N29 0.84 2.27 3.062(9) 157.6 .
O42B H42B N29 0.84 2.37 2.977(13) 129.6 .

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

data_ic150ncs
_database_code_depnum_ccdc_archive 'CCDC 1957584'
loop_
_audit_author_name
_audit_author_address
'Malcolm Halcrow' 'University of Leeds'
_audit_update_record             
;
2019-10-04 deposited with the CCDC.	2019-11-05 downloaded from the CCDC.
;
_audit_creation_date             2019-07-05
_audit_creation_method           
;
  Olex2 1.2
  (compiled Apr 23 2013 17:54:37, GUI svn.r4466)
;
_chemical_name_common            ?
_chemical_name_systematic        
'Bis-[4,6-di(pyrazol-1-yl)pyrimidine]-di[isothiocyanato]iron(II)methanol solvate'
_chemical_formula_moiety         'C22 H16 Fe N14 S2, C H4 O'
_chemical_formula_sum            'C23 H20 Fe N14 O S2'
_chemical_formula_weight         628.50
_chemical_melting_point          ?
loop_
_atom_type_symbol
_atom_type_description
_atom_type_scat_dispersion_real
_atom_type_scat_dispersion_imag
_atom_type_scat_source
C C 0.0181 0.0091 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
N N 0.0311 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'
Fe Fe -1.1336 3.1974 '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/n 1'
_space_group_name_Hall           '-P 2yn'
loop_
_space_group_symop_id
_space_group_symop_operation_xyz
1 'x, y, z'
2 '-x+1/2, y+1/2, -z+1/2'
3 '-x, -y, -z'
4 'x-1/2, -y-1/2, z-1/2'

_cell_length_a                   13.1916(3)
_cell_length_b                   14.3276(3)
_cell_length_c                   15.8098(4)
_cell_angle_alpha                90.00
_cell_angle_beta                 110.841(2)
_cell_angle_gamma                90.00
_cell_volume                     2792.61(11)
_cell_formula_units_Z            4
_cell_measurement_reflns_used    4646
_cell_measurement_temperature    120(2)
_cell_measurement_theta_min      4.27
_cell_measurement_theta_max      72.62
_exptl_absorpt_coefficient_mu    6.123
_exptl_absorpt_correction_T_min  0.768
_exptl_absorpt_correction_T_max  1.000
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   
; 
CrysAlisPro, Agilent Technologies,
Version 1.171.36.24 (release 03-12-2012 CrysAlis171 .NET)
Empirical absorption correction using spherical harmonics,
 implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_crystal_colour            red
_exptl_crystal_density_diffrn    1.495
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       lath
_exptl_crystal_F_000             1288
_exptl_crystal_size_max          0.38
_exptl_crystal_size_mid          0.20
_exptl_crystal_size_min          0.10
_exptl_special_details           
;
 ? 
;
_diffrn_reflns_av_R_equivalents  0.0269
_diffrn_reflns_av_unetI/netI     0.0346
_diffrn_reflns_limit_h_max       15
_diffrn_reflns_limit_h_min       -16
_diffrn_reflns_limit_k_max       17
_diffrn_reflns_limit_k_min       -11
_diffrn_reflns_limit_l_max       19
_diffrn_reflns_limit_l_min       -17
_diffrn_reflns_number            11284
_diffrn_reflns_theta_full        72.00
_diffrn_reflns_theta_max         73.42
_diffrn_reflns_theta_min         3.76
_diffrn_ambient_temperature      120(2)
_diffrn_detector_area_resol_mean 5.3095
_diffrn_measured_fraction_theta_full 0.986
_diffrn_measured_fraction_theta_max 0.974
_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                4796
_reflns_number_total             5480
_reflns_threshold_expression     >2sigma(I)
_computing_cell_refinement       'CrysAlisPro, Agilent Technologies'
_computing_data_collection       '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         0.657
_refine_diff_density_min         -0.477
_refine_diff_density_rms         0.057
_refine_ls_extinction_coef       ?
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.027
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     374
_refine_ls_number_reflns         5480
_refine_ls_number_restraints     1
_refine_ls_R_factor_all          0.0448
_refine_ls_R_factor_gt           0.0375
_refine_ls_restrained_S_all      1.029
_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)+(0.0548P)²+1.1122P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0958
_refine_ls_wR_factor_ref         0.1007
_refine_special_details          
;
 Refinement of F² against ALL reflections.  The weighted R-factor wR and 
 goodness of fit S are based on F², conventional R-factors R are based 
 on F, with F set to zero for negative F². The threshold expression of 
 F² > 2sigma(F²) is used only for calculating R-factors(gt) etc. and is 
 not relevant to the choice of reflections for refinement.  R-factors based 
 on F² are statistically about twice as large as those based on F, and R- 
 factors based on ALL data will be even larger. 

 No disorder is present in the model and no restraints are included in the
 refinement. All non-H atoms were refined anisotropically and C-bound H 
 atoms were placed in calculated positions and refined using a riding model.
 The methanol hydroxyl H atom was located in the Fourier map and refined,
 subject to the restraint O---H = 0.90(2) /%A and the constrain Uiso =
 1.5x Ueq{O}.
;
_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, All O(H) groups
2. Restrained distances
 O41-H41
 0.9 with sigma of 0.02
3.a Aromatic/amide H refined with riding coordinates:
 C8(H8), C11(H11), C16(H16), C17(H17), C18(H18), C21(H21), C22(H22), C23(H23),
 C24(H24), C27(H27), C32(H32), C33(H33), C34(H34), C37(H37), C38(H38), C39(H39)
3.b Idealised Me refined as rotating group:
 C40(H40A,H40B,H40C)
;
_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 0.40244(3) 0.75645(2) 0.72251(2) 0.02429(10) Uani 1 1 d . . .
N2 N 0.53536(16) 0.66841(15) 0.78628(13) 0.0322(4) Uani 1 1 d . . .
C3 C 0.59963(18) 0.61605(16) 0.83035(14) 0.0274(5) Uani 1 1 d . . .
S4 S 0.68754(5) 0.54057(5) 0.89242(4) 0.03748(15) Uani 1 1 d . . .
N5 N 0.30333(17) 0.64833(16) 0.65706(14) 0.0375(5) Uani 1 1 d . . .
C6 C 0.22815(19) 0.60163(16) 0.62188(15) 0.0295(5) Uani 1 1 d . . .
S7 S 0.12319(5) 0.53624(5) 0.57333(4) 0.04007(16) Uani 1 1 d . . .
C8 C 0.41305(19) 0.72302(19) 0.92513(16) 0.0331(5) Uani 1 1 d . . .
H8 H 0.4765 0.6887 0.9300 0.040 Uiso 1 1 calc R . .
N9 N 0.36323(14) 0.76764(14) 0.84639(12) 0.0274(4) Uani 1 1 d . . .
C10 C 0.27528(16) 0.81716(16) 0.84128(14) 0.0250(4) Uani 1 1 d . . .
C11 C 0.23687(17) 0.82321(16) 0.91172(14) 0.0267(4) Uani 1 1 d . . .
H11 H 0.1753 0.8597 0.9080 0.032 Uiso 1 1 calc R . .
C12 C 0.29458(17) 0.77232(16) 0.98814(14) 0.0251(4) Uani 1 1 d . . .
N13 N 0.38297(15) 0.72197(15) 0.99617(13) 0.0315(4) Uani 1 1 d . . .
N14 N 0.22254(14) 0.86071(14) 0.75813(12) 0.0266(4) Uani 1 1 d . . .
N15 N 0.26288(14) 0.84977(14) 0.69050(12) 0.0274(4) Uani 1 1 d . . .
C16 C 0.19340(19) 0.89346(18) 0.61983(15) 0.0332(5) Uani 1 1 d . . .
H16 H 0.2007 0.8979 0.5623 0.040 Uiso 1 1 calc R . .
C17 C 0.1073(2) 0.93250(19) 0.64079(17) 0.0376(5) Uani 1 1 d . . .
H17 H 0.0474 0.9668 0.6016 0.045 Uiso 1 1 calc R . .
C18 C 0.12799(19) 0.91061(18) 0.72930(16) 0.0347(5) Uani 1 1 d . . .
H18 H 0.0850 0.9269 0.7642 0.042 Uiso 1 1 calc R . .
N19 N 0.26253(14) 0.77124(13) 1.06334(12) 0.0257(4) Uani 1 1 d . . .
N20 N 0.18011(15) 0.82817(13) 1.06595(13) 0.0282(4) Uani 1 1 d . . .
C21 C 0.17439(18) 0.81060(17) 1.14637(15) 0.0303(5) Uani 1 1 d . . .
H21 H 0.1242 0.8399 1.1685 0.036 Uiso 1 1 calc R . .
C22 C 0.25074(19) 0.74384(18) 1.19528(15) 0.0319(5) Uani 1 1 d . . .
H22 H 0.2615 0.7206 1.2541 0.038 Uiso 1 1 calc R . .
C23 C 0.30597(18) 0.71946(18) 1.14056(15) 0.0314(5) Uani 1 1 d . . .
H23 H 0.3632 0.6753 1.1534 0.038 Uiso 1 1 calc R . .
C24 C 0.40049(18) 0.75718(16) 0.52017(15) 0.0280(5) Uani 1 1 d . . .
H24 H 0.3460 0.7111 0.5116 0.034 Uiso 1 1 calc R . .
N25 N 0.43669(13) 0.79951(13) 0.60088(11) 0.0240(4) Uani 1 1 d . . .
C26 C 0.51115(15) 0.86671(14) 0.61050(13) 0.0221(4) Uani 1 1 d . . .
C27 C 0.55018(16) 0.89106(15) 0.54330(13) 0.0232(4) Uani 1 1 d . . .
H27 H 0.6015 0.9397 0.5504 0.028 Uiso 1 1 calc R . .
C28 C 0.50868(16) 0.83889(15) 0.46445(13) 0.0228(4) Uani 1 1 d . . .
N29 N 0.43249(15) 0.77266(14) 0.45120(12) 0.0272(4) Uani 1 1 d . . .
N30 N 0.54976(13) 0.90815(13) 0.69616(11) 0.0231(3) Uani 1 1 d . . .
N31 N 0.51121(14) 0.87665(13) 0.76070(12) 0.0254(4) Uani 1 1 d . . .
C32 C 0.56382(18) 0.92509(17) 0.83404(15) 0.0297(5) Uani 1 1 d . . .
H32 H 0.5538 0.9181 0.8903 0.036 Uiso 1 1 calc R . .
C33 C 0.63662(19) 0.98847(18) 0.81842(16) 0.0329(5) Uani 1 1 d . . .
H33 H 0.6834 1.0310 0.8605 0.039 Uiso 1 1 calc R . .
C34 C 0.62593(17) 0.97610(16) 0.73024(15) 0.0291(4) Uani 1 1 d . . .
H34 H 0.6642 1.0086 0.6985 0.035 Uiso 1 1 calc R . .
N35 N 0.54562(14) 0.85148(13) 0.39294(12) 0.0249(4) Uani 1 1 d . . .
N36 N 0.61864(16) 0.92088(14) 0.39562(13) 0.0317(4) Uani 1 1 d . . .
C37 C 0.6329(2) 0.91170(18) 0.31734(16) 0.0343(5) Uani 1 1 d . . .
H37 H 0.6795 0.9506 0.2988 0.041 Uiso 1 1 calc R . .
C38 C 0.57205(19) 0.83849(18) 0.26473(15) 0.0327(5) Uani 1 1 d . . .
H38 H 0.5696 0.8194 0.2065 0.039 Uiso 1 1 calc R . .
C39 C 0.51705(18) 0.80049(17) 0.31488(14) 0.0295(5) Uani 1 1 d . . .
H39 H 0.4686 0.7489 0.2988 0.035 Uiso 1 1 calc R . .
C40 C 0.5389(3) 0.4635(2) 0.6115(2) 0.0547(8) Uani 1 1 d . . .
H40A H 0.4953 0.5190 0.6112 0.082 Uiso 1 1 calc R . .
H40B H 0.4968 0.4208 0.5633 0.082 Uiso 1 1 calc R . .
H40C H 0.6051 0.4821 0.6012 0.082 Uiso 1 1 calc R . .
O41 O 0.56656(19) 0.41862(16) 0.69516(15) 0.0550(5) Uani 1 1 d D . .
H41 H 0.607(3) 0.460(3) 0.747(2) 0.083 Uiso 1 1 d D . .


_geom_special_details            
;
 All esds (except the esd in the dihedral angle between two l.s. planes) 
 are estimated using the full covariance matrix.  The cell esds are taken 
 into account individually in the estimation of esds in distances, angles 
 and torsion angles; correlations between esds in cell parameters are only 
 used when they are defined by crystal symmetry.  An approximate (isotropic) 
 treatment of cell esds is used for estimating esds involving l.s. planes. 
;
loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
_geom_bond_publ_flag
Fe1 N2 2.103(2) . ?
Fe1 N5 2.054(2) . ?
Fe1 N9 2.2023(18) . ?
Fe1 N15 2.1841(19) . ?
Fe1 N25 2.2138(17) . ?
Fe1 N31 2.1847(19) . ?
N2 C3 1.160(3) . ?
C3 S4 1.633(2) . ?
N5 C6 1.161(3) . ?
C6 S7 1.621(2) . ?
C8 H8 0.9500 . ?
C8 N9 1.345(3) . ?
C8 N13 1.318(3) . ?
N9 C10 1.338(3) . ?
C10 C11 1.381(3) . ?
C10 N14 1.397(3) . ?
C11 H11 0.9500 . ?
C11 C12 1.384(3) . ?
C12 N13 1.338(3) . ?
C12 N19 1.397(3) . ?
N14 N15 1.362(2) . ?
N14 C18 1.368(3) . ?
N15 C16 1.323(3) . ?
C16 H16 0.9500 . ?
C16 C17 1.408(3) . ?
C17 H17 0.9500 . ?
C17 C18 1.363(3) . ?
C18 H18 0.9500 . ?
N19 N20 1.371(3) . ?
N19 C23 1.368(3) . ?
N20 C21 1.324(3) . ?
C21 H21 0.9500 . ?
C21 C22 1.405(4) . ?
C22 H22 0.9500 . ?
C22 C23 1.360(3) . ?
C23 H23 0.9500 . ?
C24 H24 0.9500 . ?
C24 N25 1.338(3) . ?
C24 N29 1.321(3) . ?
N25 C26 1.345(3) . ?
C26 C27 1.380(3) . ?
C26 N30 1.398(3) . ?
C27 H27 0.9500 . ?
C27 C28 1.388(3) . ?
C28 N29 1.343(3) . ?
C28 N35 1.393(3) . ?
N30 N31 1.369(2) . ?
N30 C34 1.365(3) . ?
N31 C32 1.317(3) . ?
C32 H32 0.9500 . ?
C32 C33 1.406(3) . ?
C33 H33 0.9500 . ?
C33 C34 1.362(3) . ?
C34 H34 0.9500 . ?
N35 N36 1.374(3) . ?
N35 C39 1.367(3) . ?
N36 C37 1.323(3) . ?
C37 H37 0.9500 . ?
C37 C38 1.400(4) . ?
C38 H38 0.9500 . ?
C38 C39 1.364(3) . ?
C39 H39 0.9500 . ?
C40 H40A 0.9800 . ?
C40 H40B 0.9800 . ?
C40 H40C 0.9800 . ?
C40 O41 1.398(4) . ?
O41 H41 0.999(19) . ?

loop_
_geom_angle_atom_site_label_1
_geom_angle_atom_site_label_2
_geom_angle_atom_site_label_3
_geom_angle
_geom_angle_site_symmetry_1
_geom_angle_site_symmetry_3
_geom_angle_publ_flag
N2 Fe1 N9 92.12(7) . . ?
N2 Fe1 N15 165.56(7) . . ?
N2 Fe1 N25 100.98(7) . . ?
N2 Fe1 N31 89.24(8) . . ?
N5 Fe1 N2 93.55(9) . . ?
N5 Fe1 N9 101.20(8) . . ?
N5 Fe1 N15 90.69(8) . . ?
N5 Fe1 N25 93.59(8) . . ?
N5 Fe1 N31 166.34(8) . . ?
N9 Fe1 N25 159.60(7) . . ?
N15 Fe1 N9 73.51(7) . . ?
N15 Fe1 N25 92.51(7) . . ?
N15 Fe1 N31 89.88(7) . . ?
N31 Fe1 N9 92.05(7) . . ?
N31 Fe1 N25 72.75(6) . . ?
C3 N2 Fe1 169.06(18) . . ?
N2 C3 S4 178.5(2) . . ?
C6 N5 Fe1 163.4(2) . . ?
N5 C6 S7 179.7(2) . . ?
N9 C8 H8 116.6 . . ?
N13 C8 H8 116.6 . . ?
N13 C8 N9 126.7(2) . . ?
C8 N9 Fe1 126.62(15) . . ?
C10 N9 Fe1 117.25(14) . . ?
C10 N9 C8 115.85(19) . . ?
N9 C10 C11 122.94(19) . . ?
N9 C10 N14 115.13(18) . . ?
C11 C10 N14 121.90(19) . . ?
C10 C11 H11 122.4 . . ?
C10 C11 C12 115.2(2) . . ?
C12 C11 H11 122.4 . . ?
C11 C12 N19 120.65(19) . . ?
N13 C12 C11 123.84(19) . . ?
N13 C12 N19 115.51(19) . . ?
C8 N13 C12 115.43(19) . . ?
N15 N14 C10 118.98(17) . . ?
N15 N14 C18 111.29(18) . . ?
C18 N14 C10 129.58(18) . . ?
N14 N15 Fe1 114.89(13) . . ?
C16 N15 Fe1 139.35(16) . . ?
C16 N15 N14 105.16(18) . . ?
N15 C16 H16 124.3 . . ?
N15 C16 C17 111.3(2) . . ?
C17 C16 H16 124.3 . . ?
C16 C17 H17 127.3 . . ?
C18 C17 C16 105.4(2) . . ?
C18 C17 H17 127.3 . . ?
N14 C18 H18 126.6 . . ?
C17 C18 N14 106.8(2) . . ?
C17 C18 H18 126.6 . . ?
N20 N19 C12 120.16(18) . . ?
C23 N19 C12 127.46(19) . . ?
C23 N19 N20 112.37(18) . . ?
C21 N20 N19 103.44(18) . . ?
N20 C21 H21 123.7 . . ?
N20 C21 C22 112.5(2) . . ?
C22 C21 H21 123.7 . . ?
C21 C22 H22 127.3 . . ?
C23 C22 C21 105.4(2) . . ?
C23 C22 H22 127.3 . . ?
N19 C23 H23 126.9 . . ?
C22 C23 N19 106.2(2) . . ?
C22 C23 H23 126.9 . . ?
N25 C24 H24 116.5 . . ?
N29 C24 H24 116.5 . . ?
N29 C24 N25 126.9(2) . . ?
C24 N25 Fe1 126.03(15) . . ?
C24 N25 C26 115.53(18) . . ?
C26 N25 Fe1 117.89(13) . . ?
N25 C26 C27 123.45(19) . . ?
N25 C26 N30 114.42(17) . . ?
C27 C26 N30 122.08(19) . . ?
C26 C27 H27 122.6 . . ?
C26 C27 C28 114.79(19) . . ?
C28 C27 H27 122.6 . . ?
C27 C28 N35 121.27(19) . . ?
N29 C28 C27 123.68(19) . . ?
N29 C28 N35 115.04(18) . . ?
C24 N29 C28 115.53(18) . . ?
N31 N30 C26 118.56(17) . . ?
C34 N30 C26 130.45(18) . . ?
C34 N30 N31 110.95(17) . . ?
N30 N31 Fe1 115.83(13) . . ?
C32 N31 Fe1 138.34(15) . . ?
C32 N31 N30 105.27(18) . . ?
N31 C32 H32 124.3 . . ?
N31 C32 C33 111.38(19) . . ?
C33 C32 H32 124.3 . . ?
C32 C33 H33 127.2 . . ?
C34 C33 C32 105.5(2) . . ?
C34 C33 H33 127.2 . . ?
N30 C34 H34 126.6 . . ?
C33 C34 N30 106.9(2) . . ?
C33 C34 H34 126.6 . . ?
N36 N35 C28 120.82(17) . . ?
C39 N35 C28 126.87(19) . . ?
C39 N35 N36 112.31(18) . . ?
C37 N36 N35 103.33(19) . . ?
N36 C37 H37 123.6 . . ?
N36 C37 C38 112.8(2) . . ?
C38 C37 H37 123.6 . . ?
C37 C38 H38 127.3 . . ?
C39 C38 C37 105.4(2) . . ?
C39 C38 H38 127.3 . . ?
N35 C39 H39 126.9 . . ?
C38 C39 N35 106.2(2) . . ?
C38 C39 H39 126.9 . . ?
H40A C40 H40B 109.5 . . ?
H40A C40 H40C 109.5 . . ?
H40B C40 H40C 109.5 . . ?
O41 C40 H40A 109.5 . . ?
O41 C40 H40B 109.5 . . ?
O41 C40 H40C 109.5 . . ?
C40 O41 H41 112(2) . . ?

loop_
_geom_hbond_atom_site_label_D
_geom_hbond_atom_site_label_H
_geom_hbond_atom_site_label_A
_geom_hbond_distance_DH
_geom_hbond_distance_HA
_geom_hbond_distance_DA
_geom_hbond_angle_DHA
_geom_hbond_site_symmetry_A
O41 H41 S4 0.999(19) 2.45(2) 3.433(2) 167(3) .

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

data_89-ncse
_database_code_depnum_ccdc_archive 'CCDC 1957589'
loop_
_audit_author_name
_audit_author_address
'Malcolm Halcrow' 'University of Leeds'
_audit_update_record             
;
2019-10-04 deposited with the CCDC.	2019-11-05 downloaded from the CCDC.
;
_audit_creation_date             2019-07-05
_audit_creation_method           
;
  Olex2 1.2
  (compiled Apr 23 2013 17:54:37, GUI svn.r4466)
;
_chemical_name_common            ?
_chemical_name_systematic        
'Bis-[2-methyl-4,6-(pyrazol-1-yl)pyrimidine]-di-isoselenocyanato iron(II)'
_chemical_formula_moiety         'C24 H20 Fe N14 Se2'
_chemical_formula_sum            'C24 H20 Fe N14 Se2'
_chemical_formula_weight         718.31
_chemical_melting_point          ?
loop_
_atom_type_symbol
_atom_type_description
_atom_type_scat_dispersion_real
_atom_type_scat_dispersion_imag
_atom_type_scat_source
C C 0.0181 0.0091 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
N N 0.0311 0.0180 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Se Se -0.7943 1.1372 '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'

_space_group_crystal_system      triclinic
_space_group_IT_number           2
_space_group_name_H-M_alt        'P -1'
_space_group_name_Hall           '-P 1'
loop_
_space_group_symop_id
_space_group_symop_operation_xyz
1 'x, y, z'
2 '-x, -y, -z'

_cell_length_a                   8.1773(4)
_cell_length_b                   12.1684(6)
_cell_length_c                   14.1965(8)
_cell_angle_alpha                77.437(4)
_cell_angle_beta                 83.062(4)
_cell_angle_gamma                89.966(4)
_cell_volume                     1368.22(12)
_cell_formula_units_Z            2
_cell_measurement_reflns_used    5267
_cell_measurement_temperature    120(2)
_cell_measurement_theta_min      3.71
_cell_measurement_theta_max      73.45
_exptl_absorpt_coefficient_mu    7.834
_exptl_absorpt_correction_T_min  0.633
_exptl_absorpt_correction_T_max  1.000
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   
; 
CrysAlisPro, Agilent Technologies,
Version 1.171.36.24 (release 03-12-2012 CrysAlis171 .NET)
Empirical absorption correction using spherical harmonics,
 implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_crystal_colour            yellow
_exptl_crystal_density_diffrn    1.744
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       'rectangular prism'
_exptl_crystal_F_000             712
_exptl_crystal_size_max          0.32
_exptl_crystal_size_mid          0.25
_exptl_crystal_size_min          0.10
_exptl_special_details           
;
 ? 
;
_diffrn_reflns_av_R_equivalents  0.0343
_diffrn_reflns_av_unetI/netI     0.0427
_diffrn_reflns_limit_h_max       8
_diffrn_reflns_limit_h_min       -10
_diffrn_reflns_limit_k_max       15
_diffrn_reflns_limit_k_min       -12
_diffrn_reflns_limit_l_max       17
_diffrn_reflns_limit_l_min       -17
_diffrn_reflns_number            10627
_diffrn_reflns_theta_full        72.00
_diffrn_reflns_theta_max         73.72
_diffrn_reflns_theta_min         3.21
_diffrn_ambient_temperature      120(2)
_diffrn_detector_area_resol_mean 5.3095
_diffrn_measured_fraction_theta_full 0.945
_diffrn_measured_fraction_theta_max 0.929
_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                4584
_reflns_number_total             5148
_reflns_threshold_expression     >2sigma(I)
_computing_cell_refinement       'CrysAlisPro, Agilent Technologies'
_computing_data_collection       '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         1.251
_refine_diff_density_min         -0.677
_refine_diff_density_rms         0.117
_refine_ls_extinction_coef       ?
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.032
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     372
_refine_ls_number_reflns         5148
_refine_ls_number_restraints     0
_refine_ls_R_factor_all          0.0474
_refine_ls_R_factor_gt           0.0420
_refine_ls_restrained_S_all      1.032
_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)+(0.0808P)²+0.1384P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1119
_refine_ls_wR_factor_ref         0.1173
_refine_special_details          
;
 Refinement of F² against ALL reflections.  The weighted R-factor wR and 
 goodness of fit S are based on F², conventional R-factors R are based 
 on F, with F set to zero for negative F². The threshold expression of 
 F² > 2sigma(F²) is used only for calculating R-factors(gt) etc. and is 
 not relevant to the choice of reflections for refinement.  R-factors based 
 on F² are statistically about twice as large as those based on F, and R- 
 factors based on ALL data will be even larger. 

 No disorder is present in the model, and no restraints were appplied to the
 refinement. All non-H atoms were refined anisotropically, and H atoms were
 placed in calculated positions and refined using a riding model.
;
_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.a Aromatic/amide H refined with riding coordinates:
 C11(H11), C16(H16), C17(H17), C18(H18), C21(H21), C22(H22), C23(H23),
 C28(H28), C33(H33), C34(H34), C35(H35), C38(H38), C39(H39), C40(H40)
2.b Idealised Me refined as rotating group:
 C24(H24A,H24B,H24C), 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 0.46063(6) 0.26465(4) 0.72741(4) 0.01761(14) Uani 1 1 d . . .
N2 N 0.5492(3) 0.4317(2) 0.7119(2) 0.0237(6) Uani 1 1 d . . .
C3 C 0.6147(4) 0.5162(3) 0.7101(2) 0.0207(6) Uani 1 1 d . . .
Se4 Se 0.71985(4) 0.64718(3) 0.70496(3) 0.02804(12) Uani 1 1 d . . .
N5 N 0.6705(3) 0.2078(2) 0.7913(2) 0.0256(6) Uani 1 1 d . . .
C6 C 0.7503(4) 0.1566(3) 0.8476(2) 0.0216(6) Uani 1 1 d . . .
Se7 Se 0.87060(4) 0.08006(3) 0.93437(3) 0.02966(13) Uani 1 1 d . . .
C8 C 0.6616(4) 0.2654(3) 0.5088(2) 0.0211(6) Uani 1 1 d . . .
N9 N 0.5744(3) 0.2060(2) 0.5906(2) 0.0196(5) Uani 1 1 d . . .
C10 C 0.5839(4) 0.0930(3) 0.6048(2) 0.0193(6) Uani 1 1 d . . .
C11 C 0.6801(4) 0.0390(3) 0.5432(2) 0.0224(6) Uani 1 1 d . . .
H11 H 0.6841 -0.0407 0.5538 0.027 Uiso 1 1 calc R . .
C12 C 0.7710(4) 0.1103(3) 0.4641(2) 0.0216(6) Uani 1 1 d . . .
N13 N 0.7609(3) 0.2221(2) 0.4455(2) 0.0214(5) Uani 1 1 d . . .
N14 N 0.4887(3) 0.0325(2) 0.6884(2) 0.0211(5) Uani 1 1 d . . .
N15 N 0.3946(3) 0.0888(2) 0.7468(2) 0.0223(6) Uani 1 1 d . . .
C16 C 0.3166(4) 0.0110(3) 0.8172(3) 0.0262(7) Uani 1 1 d . . .
H16 H 0.2413 0.0263 0.8689 0.031 Uiso 1 1 calc R . .
C17 C 0.3598(5) -0.0982(3) 0.8057(3) 0.0290(7) Uani 1 1 d . . .
H17 H 0.3215 -0.1682 0.8467 0.035 Uiso 1 1 calc R . .
C18 C 0.4686(4) -0.0812(3) 0.7228(3) 0.0253(7) Uani 1 1 d . . .
H18 H 0.5207 -0.1379 0.6942 0.030 Uiso 1 1 calc R . .
N19 N 0.8795(3) 0.0681(2) 0.3987(2) 0.0229(6) Uani 1 1 d . . .
N20 N 0.8904(4) -0.0457(2) 0.4056(2) 0.0263(6) Uani 1 1 d . . .
C21 C 1.0010(4) -0.0528(3) 0.3307(3) 0.0290(7) Uani 1 1 d . . .
H21 H 1.0346 -0.1221 0.3151 0.035 Uiso 1 1 calc R . .
C22 C 1.0636(4) 0.0537(3) 0.2766(3) 0.0308(8) Uani 1 1 d . . .
H22 H 1.1442 0.0692 0.2210 0.037 Uiso 1 1 calc R . .
C23 C 0.9828(4) 0.1283(3) 0.3220(3) 0.0269(7) Uani 1 1 d . . .
H23 H 0.9956 0.2080 0.3039 0.032 Uiso 1 1 calc R . .
C24 C 0.6438(4) 0.3901(3) 0.4850(3) 0.0248(7) Uani 1 1 d . . .
H24A H 0.5347 0.4079 0.4647 0.037 Uiso 1 1 calc R . .
H24B H 0.7290 0.4241 0.4320 0.037 Uiso 1 1 calc R . .
H24C H 0.6559 0.4201 0.5425 0.037 Uiso 1 1 calc R . .
C25 C 0.2563(4) 0.2798(3) 0.9391(2) 0.0229(7) Uani 1 1 d . . .
N26 N 0.2542(3) 0.2917(2) 0.8417(2) 0.0198(5) Uani 1 1 d . . .
C27 C 0.1170(4) 0.3366(3) 0.8074(2) 0.0203(6) Uani 1 1 d . . .
C28 C -0.0142(4) 0.3706(3) 0.8634(3) 0.0234(6) Uani 1 1 d . . .
H28 H -0.1088 0.4035 0.8371 0.028 Uiso 1 1 calc R . .
C29 C 0.0036(4) 0.3528(3) 0.9617(3) 0.0220(6) Uani 1 1 d . . .
N30 N 0.1365(3) 0.3083(2) 0.9993(2) 0.0248(6) Uani 1 1 d . . .
N31 N 0.1148(3) 0.3449(2) 0.7070(2) 0.0201(5) Uani 1 1 d . . .
N32 N 0.2481(3) 0.3127(2) 0.6537(2) 0.0193(5) Uani 1 1 d . . .
C33 C 0.2061(4) 0.3214(3) 0.5654(2) 0.0209(6) Uani 1 1 d . . .
H33 H 0.2760 0.3040 0.5124 0.025 Uiso 1 1 calc R . .
C34 C 0.0451(4) 0.3593(3) 0.5601(3) 0.0254(7) Uani 1 1 d . . .
H34 H -0.0133 0.3722 0.5050 0.031 Uiso 1 1 calc R . .
C35 C -0.0106(4) 0.3741(3) 0.6516(3) 0.0250(7) Uani 1 1 d . . .
H35 H -0.1158 0.3997 0.6724 0.030 Uiso 1 1 calc R . .
N36 N -0.1203(3) 0.3799(2) 1.0291(2) 0.0246(6) Uani 1 1 d . . .
N37 N -0.2708(4) 0.4154(3) 1.0025(2) 0.0301(6) Uani 1 1 d . . .
C38 C -0.3545(5) 0.4284(3) 1.0847(3) 0.0320(8) Uani 1 1 d . . .
H38 H -0.4651 0.4524 1.0899 0.038 Uiso 1 1 calc R . .
C39 C -0.2619(5) 0.4027(3) 1.1641(3) 0.0304(8) Uani 1 1 d . . .
H39 H -0.2965 0.4062 1.2297 0.037 Uiso 1 1 calc R . .
C40 C -0.1118(5) 0.3717(3) 1.1262(3) 0.0290(7) Uani 1 1 d . . .
H40 H -0.0201 0.3490 1.1603 0.035 Uiso 1 1 calc R . .
C41 C 0.4056(4) 0.2289(4) 0.9813(3) 0.0315(8) Uani 1 1 d . . .
H41A H 0.3915 0.2241 1.0516 0.047 Uiso 1 1 calc R . .
H41B H 0.5031 0.2761 0.9511 0.047 Uiso 1 1 calc R . .
H41C H 0.4197 0.1533 0.9686 0.047 Uiso 1 1 calc R . .


_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 2.115(3) . ?
Fe1 N5 2.085(3) . ?
Fe1 N9 2.305(3) . ?
Fe1 N15 2.157(3) . ?
Fe1 N26 2.271(3) . ?
Fe1 N32 2.151(3) . ?
N2 C3 1.154(4) . ?
C3 Se4 1.795(3) . ?
N5 C6 1.167(5) . ?
C6 Se7 1.774(3) . ?
C8 N9 1.347(4) . ?
C8 N13 1.332(5) . ?
C8 C24 1.491(5) . ?
N9 C10 1.349(4) . ?
C10 C11 1.378(5) . ?
C10 N14 1.398(4) . ?
C11 H11 0.9500 . ?
C11 C12 1.393(5) . ?
C12 N13 1.333(4) . ?
C12 N19 1.386(5) . ?
N14 N15 1.357(4) . ?
N14 C18 1.366(4) . ?
N15 C16 1.318(5) . ?
C16 H16 0.9500 . ?
C16 C17 1.413(5) . ?
C17 H17 0.9500 . ?
C17 C18 1.365(5) . ?
C18 H18 0.9500 . ?
N19 N20 1.371(4) . ?
N19 C23 1.366(5) . ?
N20 C21 1.327(5) . ?
C21 H21 0.9500 . ?
C21 C22 1.415(6) . ?
C22 H22 0.9500 . ?
C22 C23 1.352(5) . ?
C23 H23 0.9500 . ?
C24 H24A 0.9800 . ?
C24 H24B 0.9800 . ?
C24 H24C 0.9800 . ?
C25 N26 1.362(4) . ?
C25 N30 1.317(5) . ?
C25 C41 1.498(5) . ?
N26 C27 1.345(4) . ?
C27 C28 1.375(5) . ?
C27 N31 1.409(4) . ?
C28 H28 0.9500 . ?
C28 C29 1.391(5) . ?
C29 N30 1.331(5) . ?
C29 N36 1.398(4) . ?
N31 N32 1.357(4) . ?
N31 C35 1.367(4) . ?
N32 C33 1.323(4) . ?
C33 H33 0.9500 . ?
C33 C34 1.400(5) . ?
C34 H34 0.9500 . ?
C34 C35 1.373(5) . ?
C35 H35 0.9500 . ?
N36 N37 1.373(4) . ?
N36 C40 1.371(5) . ?
N37 C38 1.320(5) . ?
C38 H38 0.9500 . ?
C38 C39 1.412(6) . ?
C39 H39 0.9500 . ?
C39 C40 1.366(5) . ?
C40 H40 0.9500 . ?
C41 H41A 0.9800 . ?
C41 H41B 0.9800 . ?
C41 H41C 0.9800 . ?

loop_
_geom_angle_atom_site_label_1
_geom_angle_atom_site_label_2
_geom_angle_atom_site_label_3
_geom_angle
_geom_angle_site_symmetry_1
_geom_angle_site_symmetry_3
_geom_angle_publ_flag
N2 Fe1 N9 106.30(10) . . ?
N2 Fe1 N15 174.19(11) . . ?
N2 Fe1 N26 90.30(10) . . ?
N2 Fe1 N32 94.76(10) . . ?
N5 Fe1 N2 88.59(11) . . ?
N5 Fe1 N9 87.88(10) . . ?
N5 Fe1 N15 85.72(11) . . ?
N5 Fe1 N26 110.77(11) . . ?
N5 Fe1 N32 175.03(11) . . ?
N15 Fe1 N9 72.35(10) . . ?
N15 Fe1 N26 92.82(10) . . ?
N26 Fe1 N9 155.59(9) . . ?
N32 Fe1 N9 87.65(10) . . ?
N32 Fe1 N15 90.84(10) . . ?
N32 Fe1 N26 72.95(10) . . ?
C3 N2 Fe1 170.7(3) . . ?
N2 C3 Se4 178.6(3) . . ?
C6 N5 Fe1 158.8(3) . . ?
N5 C6 Se7 179.1(3) . . ?
N9 C8 C24 117.9(3) . . ?
N13 C8 N9 125.5(3) . . ?
N13 C8 C24 116.6(3) . . ?
C8 N9 Fe1 129.6(2) . . ?
C8 N9 C10 115.7(3) . . ?
C10 N9 Fe1 113.0(2) . . ?
N9 C10 C11 123.7(3) . . ?
N9 C10 N14 115.0(3) . . ?
C11 C10 N14 121.3(3) . . ?
C10 C11 H11 122.6 . . ?
C10 C11 C12 114.8(3) . . ?
C12 C11 H11 122.6 . . ?
N13 C12 C11 123.4(3) . . ?
N13 C12 N19 115.3(3) . . ?
N19 C12 C11 121.3(3) . . ?
C8 N13 C12 116.7(3) . . ?
N15 N14 C10 119.5(3) . . ?
N15 N14 C18 110.7(3) . . ?
C18 N14 C10 129.8(3) . . ?
N14 N15 Fe1 115.2(2) . . ?
C16 N15 Fe1 135.8(2) . . ?
C16 N15 N14 106.0(3) . . ?
N15 C16 H16 124.4 . . ?
N15 C16 C17 111.1(3) . . ?
C17 C16 H16 124.4 . . ?
C16 C17 H17 127.6 . . ?
C18 C17 C16 104.9(3) . . ?
C18 C17 H17 127.6 . . ?
N14 C18 H18 126.3 . . ?
C17 C18 N14 107.3(3) . . ?
C17 C18 H18 126.3 . . ?
N20 N19 C12 120.6(3) . . ?
C23 N19 C12 127.3(3) . . ?
C23 N19 N20 112.1(3) . . ?
C21 N20 N19 103.1(3) . . ?
N20 C21 H21 123.5 . . ?
N20 C21 C22 113.0(3) . . ?
C22 C21 H21 123.5 . . ?
C21 C22 H22 127.8 . . ?
C23 C22 C21 104.3(3) . . ?
C23 C22 H22 127.8 . . ?
N19 C23 H23 126.3 . . ?
C22 C23 N19 107.5(3) . . ?
C22 C23 H23 126.3 . . ?
C8 C24 H24A 109.5 . . ?
C8 C24 H24B 109.5 . . ?
C8 C24 H24C 109.5 . . ?
H24A C24 H24B 109.5 . . ?
H24A C24 H24C 109.5 . . ?
H24B C24 H24C 109.5 . . ?
N26 C25 C41 117.4(3) . . ?
N30 C25 N26 125.0(3) . . ?
N30 C25 C41 117.6(3) . . ?
C25 N26 Fe1 128.8(2) . . ?
C27 N26 Fe1 115.6(2) . . ?
C27 N26 C25 115.2(3) . . ?
N26 C27 C28 124.5(3) . . ?
N26 C27 N31 114.4(3) . . ?
C28 C27 N31 121.1(3) . . ?
C27 C28 H28 122.9 . . ?
C27 C28 C29 114.2(3) . . ?
C29 C28 H28 122.9 . . ?
C28 C29 N36 121.6(3) . . ?
N30 C29 C28 123.6(3) . . ?
N30 C29 N36 114.8(3) . . ?
C25 N30 C29 117.4(3) . . ?
N32 N31 C27 119.3(3) . . ?
N32 N31 C35 111.0(3) . . ?
C35 N31 C27 129.5(3) . . ?
N31 N32 Fe1 116.83(19) . . ?
C33 N32 Fe1 137.4(2) . . ?
C33 N32 N31 105.8(2) . . ?
N32 C33 H33 124.4 . . ?
N32 C33 C34 111.2(3) . . ?
C34 C33 H33 124.4 . . ?
C33 C34 H34 127.3 . . ?
C35 C34 C33 105.4(3) . . ?
C35 C34 H34 127.3 . . ?
N31 C35 C34 106.7(3) . . ?
N31 C35 H35 126.7 . . ?
C34 C35 H35 126.7 . . ?
N37 N36 C29 121.2(3) . . ?
C40 N36 C29 126.3(3) . . ?
C40 N36 N37 112.5(3) . . ?
C38 N37 N36 103.5(3) . . ?
N37 C38 H38 123.6 . . ?
N37 C38 C39 112.8(3) . . ?
C39 C38 H38 123.6 . . ?
C38 C39 H39 127.4 . . ?
C40 C39 C38 105.1(3) . . ?
C40 C39 H39 127.4 . . ?
N36 C40 H40 126.9 . . ?
C39 C40 N36 106.1(3) . . ?
C39 C40 H40 126.9 . . ?
C25 C41 H41A 109.5 . . ?
C25 C41 H41B 109.5 . . ?
C25 C41 H41C 109.5 . . ?
H41A C41 H41B 109.5 . . ?
H41A C41 H41C 109.5 . . ?
H41B C41 H41C 109.5 . . ?

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

data_150seac
_database_code_depnum_ccdc_archive 'CCDC 1957587'
loop_
_audit_author_name
_audit_author_address
'Malcolm Halcrow' 'University of Leeds'
_audit_update_record             
;
2019-10-04 deposited with the CCDC.	2019-11-05 downloaded from the CCDC.
;
_audit_creation_date             2019-07-05
_audit_creation_method           
;
  Olex2 1.2
  (compiled Apr 23 2013 17:54:37, GUI svn.r4466)
;
_chemical_name_common            ?
_chemical_name_systematic        
'Bis-[4,6-di(pyrazol-1-yl)pyrimidine]-di[isoselenocyanato]iron(II)hemi-acetone solvate'
_chemical_formula_moiety         'C22 H16 Fe N14 Se2, 0.5(C3 H6 O)'
_chemical_formula_sum            'C23.50 H19 Fe N14 O0.50 Se2'
_chemical_formula_weight         719.30
_chemical_melting_point          ?
loop_
_atom_type_symbol
_atom_type_description
_atom_type_scat_dispersion_real
_atom_type_scat_dispersion_imag
_atom_type_scat_source
C C 0.0181 0.0091 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
N N 0.0311 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'
Se Se -0.7943 1.1372 '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'

_space_group_crystal_system      monoclinic
_space_group_IT_number           14
_space_group_name_H-M_alt        'P 1 21/n 1'
_space_group_name_Hall           '-P 2yn'
loop_
_space_group_symop_id
_space_group_symop_operation_xyz
1 'x, y, z'
2 '-x+1/2, y+1/2, -z+1/2'
3 '-x, -y, -z'
4 'x-1/2, -y-1/2, z-1/2'

_cell_length_a                   12.7269(5)
_cell_length_b                   14.6440(6)
_cell_length_c                   16.1908(7)
_cell_angle_alpha                90.00
_cell_angle_beta                 109.447(4)
_cell_angle_gamma                90.00
_cell_volume                     2845.4(2)
_cell_formula_units_Z            4
_cell_measurement_reflns_used    3443
_cell_measurement_temperature    120(2)
_cell_measurement_theta_min      3.84
_cell_measurement_theta_max      73.32
_exptl_absorpt_coefficient_mu    7.549
_exptl_absorpt_correction_T_min  0.481
_exptl_absorpt_correction_T_max  1.000
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   
; 
CrysAlisPro, Agilent Technologies,
Version 1.171.36.24 (release 03-12-2012 CrysAlis171 .NET)
Empirical absorption correction using spherical harmonics,
 implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_crystal_colour            yellow
_exptl_crystal_density_diffrn    1.679
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       plate
_exptl_crystal_F_000             1424
_exptl_crystal_size_max          0.30
_exptl_crystal_size_mid          0.25
_exptl_crystal_size_min          0.05
_exptl_special_details           
;
 ? 
;
_diffrn_reflns_av_R_equivalents  0.0321
_diffrn_reflns_av_unetI/netI     0.0432
_diffrn_reflns_limit_h_max       15
_diffrn_reflns_limit_h_min       -14
_diffrn_reflns_limit_k_max       17
_diffrn_reflns_limit_k_min       -10
_diffrn_reflns_limit_l_max       19
_diffrn_reflns_limit_l_min       -18
_diffrn_reflns_number            10897
_diffrn_reflns_theta_full        72.00
_diffrn_reflns_theta_max         73.54
_diffrn_reflns_theta_min         3.85
_diffrn_ambient_temperature      120(2)
_diffrn_detector_area_resol_mean 5.3095
_diffrn_measured_fraction_theta_full 0.983
_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                4193
_reflns_number_total             5537
_reflns_threshold_expression     >2sigma(I)
_computing_cell_refinement       'CrysAlisPro, Agilent Technologies'
_computing_data_collection       '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         0.642
_refine_diff_density_min         -0.631
_refine_diff_density_rms         0.076
_refine_ls_extinction_coef       ?
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.024
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     393
_refine_ls_number_reflns         5537
_refine_ls_number_restraints     18
_refine_ls_R_factor_all          0.0680
_refine_ls_R_factor_gt           0.0489
_refine_ls_restrained_S_all      1.041
_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)+(0.0636P)²+2.4629P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1220
_refine_ls_wR_factor_ref         0.1356
_refine_special_details          
;
 Refinement of F² against ALL reflections.  The weighted R-factor wR and 
 goodness of fit S are based on F², conventional R-factors R are based 
 on F, with F set to zero for negative F². The threshold expression of 
 F² > 2sigma(F²) is used only for calculating R-factors(gt) etc. and is 
 not relevant to the choice of reflections for refinement.  R-factors based 
 on F² are statistically about twice as large as those based on F, and R- 
 factors based on ALL data will be even larger. 

 The asymmetric unit contains one molecule of the complex, and half a 
 molecule of acetone near the crystallographic inversion centre. 
 One of the Se atoms in the model had a larger displacement ellipsoid than
 the other atoms in the molecule, and was refined without restraints over 
 two disorder sites with refined occupancies of 0.57 and 0.43. The acetone
 half-molecule is also disordered over two 0.25-occupied sites, which were
 treated with SIMU displacement ellipsoid restraints, and with the following 
 fixed distance restraints: C---O = 1.22(2), C---C = 1.51(2), 1,3-C...C = 
 2.62(2) and 1,3-C...O = 2.37(2) Å. 

 All crystallographically ordered non-H atoms, plus the disordered Se atoms, 
 were refined anisotropically and all H atoms were placed in calculated positions   and refined using a riding model. 
;
_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
 O40A-C41A = O40B-C41B
 1.22 with sigma of 0.02
 C41A-C42A = C41A-C43A = C41B-C42B = C41B-C43B
 1.51 with sigma of 0.02
 C42A-C43A = C42B-C43B
 2.62 with sigma of 0.02
 O40A-C42A = O40A-C43A = O40B-C42B = O40B-C43B
 2.37 with sigma of 0.02
3. Uiso/Uaniso restraints and constraints
O40A \\sim C41A \\sim C42A \\sim C43A: within 1.7A with sigma of 0.005 and sigma for terminal atoms of 0.01
O40B \\sim C41B \\sim C42B \\sim C43B: within 1.7A with sigma of 0.005 and sigma for terminal atoms of 0.01
4. Others
 Fixed Sof: Se7A(0.57) Se7B(0.43) O40A(0.25) C41A(0.25) C42A(0.25) H42A(0.25)
 H42B(0.25) H42C(0.25) C43A(0.25) H43A(0.25) H43B(0.25) H43C(0.25) O40B(0.25)
 C41B(0.25) C42B(0.25) H42D(0.25) H42E(0.25) H42F(0.25) C43B(0.25) H43D(0.25)
 H43E(0.25) H43F(0.25)
5.a Me refined with riding coordinates:
 C42A(H42A,H42B,H42C), C43A(H43A,H43B,H43C), C42B(H42D,H42E,H42F), C43B(H43D,
 H43E,H43F)
5.b Aromatic/amide H refined with riding coordinates:
 C8(H8), C11(H11), C16(H16), C17(H17), C18(H18), C21(H21), C22(H22), C23(H23),
 C24(H24), C27(H27), C32(H32), C33(H33), C34(H34), C37(H37), C38(H38), C39(H39)
;
_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 0.40889(5) 0.76081(5) 0.73840(4) 0.04282(19) Uani 1 1 d . . .
N2 N 0.5431(3) 0.6714(3) 0.7959(2) 0.0528(10) Uani 1 1 d . . .
C3 C 0.6062(4) 0.6233(4) 0.8435(3) 0.0493(11) Uani 1 1 d . . .
Se4 Se 0.69861(5) 0.54666(5) 0.92011(3) 0.06049(19) Uani 1 1 d . . .
N5 N 0.3028(3) 0.6569(3) 0.6770(2) 0.0518(9) Uani 1 1 d . A .
C6 C 0.2278(4) 0.6151(3) 0.6368(3) 0.0490(11) Uani 1 1 d . . .
Se7A Se 0.1211(4) 0.5428(4) 0.5742(3) 0.0636(9) Uani 0.57 1 d P A 1
Se7B Se 0.0934(5) 0.5599(5) 0.5740(4) 0.0611(11) Uani 0.43 1 d P A 2
C8 C 0.4223(4) 0.7229(4) 0.9367(3) 0.0536(12) Uani 1 1 d . . .
H8 H 0.4866 0.6887 0.9386 0.064 Uiso 1 1 calc R . .
N9 N 0.3729(3) 0.7692(3) 0.8630(2) 0.0460(9) Uani 1 1 d . . .
C10 C 0.2838(4) 0.8180(3) 0.8620(3) 0.0456(10) Uani 1 1 d . . .
C11 C 0.2450(5) 0.8226(3) 0.9319(3) 0.0553(12) Uani 1 1 d . . .
H11 H 0.1831 0.8592 0.9312 0.066 Uiso 1 1 calc R . .
C12 C 0.3034(4) 0.7697(4) 1.0032(3) 0.0518(12) Uani 1 1 d . . .
N13 N 0.3924(3) 0.7189(3) 1.0074(2) 0.0559(11) Uani 1 1 d . . .
N14 N 0.2288(3) 0.8632(3) 0.7830(2) 0.0472(9) Uani 1 1 d . . .
N15 N 0.2654(3) 0.8514(3) 0.7142(2) 0.0452(8) Uani 1 1 d . . .
C16 C 0.1934(4) 0.8950(4) 0.6490(3) 0.0521(11) Uani 1 1 d . . .
H16 H 0.1975 0.8976 0.5915 0.062 Uiso 1 1 calc R . .
C17 C 0.1099(4) 0.9371(4) 0.6738(4) 0.0601(13) Uani 1 1 d . . .
H17 H 0.0493 0.9728 0.6384 0.072 Uiso 1 1 calc R . .
C18 C 0.1347(5) 0.9156(4) 0.7597(4) 0.0636(14) Uani 1 1 d . . .
H18 H 0.0941 0.9336 0.7967 0.076 Uiso 1 1 calc R . .
N19 N 0.2696(4) 0.7661(3) 1.0773(3) 0.0615(12) Uani 1 1 d . . .
N20 N 0.1871(5) 0.8234(3) 1.0825(3) 0.0746(15) Uani 1 1 d . . .
C21 C 0.1782(6) 0.8039(5) 1.1595(4) 0.082(2) Uani 1 1 d . . .
H21 H 0.1274 0.8331 1.1826 0.098 Uiso 1 1 calc R . .
C22 C 0.2513(6) 0.7361(6) 1.2024(4) 0.091(3) Uani 1 1 d . . .
H22 H 0.2597 0.7115 1.2586 0.110 Uiso 1 1 calc R . .
C23 C 0.3097(5) 0.7107(5) 1.1483(3) 0.076(2) Uani 1 1 d . . .
H23 H 0.3654 0.6649 1.1583 0.091 Uiso 1 1 calc R . .
C24 C 0.3954(4) 0.7599(5) 0.5370(3) 0.0674(17) Uani 1 1 d . . .
H24 H 0.3376 0.7166 0.5308 0.081 Uiso 1 1 calc R . .
N25 N 0.4348(3) 0.8024(3) 0.6139(2) 0.0502(10) Uani 1 1 d . . .
C26 C 0.5093(3) 0.8685(3) 0.6193(3) 0.0425(10) Uani 1 1 d . . .
C27 C 0.5471(3) 0.8906(3) 0.5509(3) 0.0406(9) Uani 1 1 d . . .
H27 H 0.5982 0.9390 0.5548 0.049 Uiso 1 1 calc R . .
C28 C 0.5057(3) 0.8380(3) 0.4775(3) 0.0461(10) Uani 1 1 d . . .
N29 N 0.4286(3) 0.7718(4) 0.4677(2) 0.0624(12) Uani 1 1 d . . .
N30 N 0.5507(3) 0.9112(3) 0.7009(2) 0.0412(8) Uani 1 1 d . . .
N31 N 0.5193(3) 0.8778(3) 0.7683(2) 0.0446(8) Uani 1 1 d . . .
C32 C 0.5750(4) 0.9277(3) 0.8366(3) 0.0506(11) Uani 1 1 d . . .
H32 H 0.5697 0.9203 0.8934 0.061 Uiso 1 1 calc R . .
C33 C 0.6422(5) 0.9922(4) 0.8160(3) 0.0608(13) Uani 1 1 d . . .
H33 H 0.6900 1.0353 0.8543 0.073 Uiso 1 1 calc R . .
C34 C 0.6251(4) 0.9804(3) 0.7281(3) 0.0538(12) Uani 1 1 d . . .
H34 H 0.6586 1.0141 0.6934 0.065 Uiso 1 1 calc R . .
N35 N 0.5437(3) 0.8478(3) 0.4059(2) 0.0450(8) Uani 1 1 d . . .
N36 N 0.6216(3) 0.9127(3) 0.4077(2) 0.0495(9) Uani 1 1 d . . .
C37 C 0.6367(4) 0.9016(3) 0.3311(3) 0.0516(11) Uani 1 1 d . . .
H37 H 0.6871 0.9373 0.3125 0.062 Uiso 1 1 calc R . .
C38 C 0.5713(4) 0.8325(4) 0.2809(3) 0.0554(12) Uani 1 1 d . . .
H38 H 0.5683 0.8128 0.2243 0.067 Uiso 1 1 calc R . .
C39 C 0.5125(4) 0.7989(4) 0.3307(3) 0.0560(12) Uani 1 1 d . . .
H39 H 0.4598 0.7505 0.3156 0.067 Uiso 1 1 calc R . .
O40A O 0.4428(15) 0.5234(15) 0.5025(12) 0.091(4) Uiso 0.25 1 d PDU . 1
C41A C 0.4913(14) 0.5250(15) 0.4502(11) 0.056(4) Uiso 0.25 1 d PDU . 1
C42A C 0.4586(13) 0.5812(12) 0.3699(9) 0.042(3) Uiso 0.25 1 d PDU B 1
H42A H 0.5082 0.5679 0.3363 0.063 Uiso 0.25 1 calc PR B 1
H42B H 0.4643 0.6460 0.3858 0.063 Uiso 0.25 1 calc PR B 1
H42C H 0.3816 0.5669 0.3343 0.063 Uiso 0.25 1 calc PR B 1
C43A C 0.6155(14) 0.4969(16) 0.4717(14) 0.068(5) Uiso 0.25 1 d PDU C 1
H43A H 0.6341 0.4960 0.4177 0.102 Uiso 0.25 1 calc PR C 1
H43B H 0.6271 0.4359 0.4983 0.102 Uiso 0.25 1 calc PR C 1
H43C H 0.6634 0.5410 0.5128 0.102 Uiso 0.25 1 calc PR C 1
O40B O 0.5309(18) 0.4822(16) 0.4483(15) 0.108(5) Uiso 0.25 1 d PDU . 2
C41B C 0.452(2) 0.536(2) 0.4227(15) 0.088(5) Uiso 0.25 1 d PDU D 2
C42B C 0.3864(15) 0.5591(13) 0.4817(12) 0.051(4) Uiso 0.25 1 d PDU D 2
H42D H 0.4158 0.5249 0.5366 0.076 Uiso 0.25 1 calc PR D 2
H42E H 0.3080 0.5431 0.4526 0.076 Uiso 0.25 1 calc PR D 2
H42F H 0.3926 0.6248 0.4943 0.076 Uiso 0.25 1 calc PR D 2
C43B C 0.425(3) 0.573(3) 0.3340(15) 0.133(9) Uiso 0.25 1 d PDU D 2
H43D H 0.4791 0.5503 0.3074 0.200 Uiso 0.25 1 calc PR D 2
H43E H 0.4287 0.6398 0.3369 0.200 Uiso 0.25 1 calc PR D 2
H43F H 0.3501 0.5538 0.2984 0.200 Uiso 0.25 1 calc PR D 2


_geom_special_details            
;
 All esds (except the esd in the dihedral angle between two l.s. planes) 
 are estimated using the full covariance matrix.  The cell esds are taken 
 into account individually in the estimation of esds in distances, angles 
 and torsion angles; correlations between esds in cell parameters are only 
 used when they are defined by crystal symmetry.  An approximate (isotropic) 
 treatment of cell esds is used for estimating esds involving l.s. planes. 
;
loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
_geom_bond_publ_flag
Fe1 N2 2.108(4) . ?
Fe1 N5 2.057(4) . ?
Fe1 N9 2.216(3) . ?
Fe1 N15 2.185(4) . ?
Fe1 N25 2.233(3) . ?
Fe1 N31 2.166(4) . ?
N2 C3 1.150(6) . ?
C3 Se4 1.791(5) . ?
N5 C6 1.138(6) . ?
C6 Se7A 1.754(8) . ?
C6 Se7B 1.860(9) . ?
C8 H8 0.9500 . ?
C8 N9 1.335(6) . ?
C8 N13 1.323(5) . ?
N9 C10 1.335(6) . ?
C10 C11 1.380(6) . ?
C10 N14 1.402(6) . ?
C11 H11 0.9500 . ?
C11 C12 1.383(8) . ?
C12 N13 1.338(7) . ?
C12 N19 1.404(5) . ?
N14 N15 1.355(4) . ?
N14 C18 1.366(7) . ?
N15 C16 1.310(6) . ?
C16 H16 0.9500 . ?
C16 C17 1.399(7) . ?
C17 H17 0.9500 . ?
C17 C18 1.357(8) . ?
C18 H18 0.9500 . ?
N19 N20 1.368(7) . ?
N19 C23 1.360(8) . ?
N20 C21 1.321(7) . ?
C21 H21 0.9500 . ?
C21 C22 1.380(11) . ?
C22 H22 0.9500 . ?
C22 C23 1.375(9) . ?
C23 H23 0.9500 . ?
C24 H24 0.9500 . ?
C24 N25 1.331(6) . ?
C24 N29 1.336(6) . ?
N25 C26 1.337(6) . ?
C26 C27 1.385(5) . ?
C26 N30 1.397(5) . ?
C27 H27 0.9500 . ?
C27 C28 1.367(6) . ?
C28 N29 1.350(6) . ?
C28 N35 1.403(5) . ?
N30 N31 1.370(5) . ?
N30 C34 1.357(6) . ?
N31 C32 1.318(6) . ?
C32 H32 0.9500 . ?
C32 C33 1.388(7) . ?
C33 H33 0.9500 . ?
C33 C34 1.376(7) . ?
C34 H34 0.9500 . ?
N35 N36 1.367(5) . ?
N35 C39 1.353(6) . ?
N36 C37 1.327(5) . ?
C37 H37 0.9500 . ?
C37 C38 1.388(7) . ?
C38 H38 0.9500 . ?
C38 C39 1.362(6) . ?
C39 H39 0.9500 . ?
O40A C41A 1.202(15) . ?
C41A C42A 1.477(16) . ?
C41A C43A 1.556(16) . ?
C42A H42A 0.9800 . ?
C42A H42B 0.9800 . ?
C42A H42C 0.9800 . ?
C43A H43A 0.9800 . ?
C43A H43B 0.9800 . ?
C43A H43C 0.9800 . ?
O40B C41B 1.228(17) . ?
C41B C42B 1.506(16) . ?
C41B C43B 1.466(17) . ?
C42B H42D 0.9800 . ?
C42B H42E 0.9800 . ?
C42B H42F 0.9800 . ?
C43B H43D 0.9800 . ?
C43B H43E 0.9800 . ?
C43B H43F 0.9800 . ?

loop_
_geom_angle_atom_site_label_1
_geom_angle_atom_site_label_2
_geom_angle_atom_site_label_3
_geom_angle
_geom_angle_site_symmetry_1
_geom_angle_site_symmetry_3
_geom_angle_publ_flag
N2 Fe1 N9 90.87(14) . . ?
N2 Fe1 N15 164.35(13) . . ?
N2 Fe1 N25 103.12(14) . . ?
N2 Fe1 N31 91.30(16) . . ?
N5 Fe1 N2 93.38(17) . . ?
N5 Fe1 N9 100.34(14) . . ?
N5 Fe1 N15 89.30(16) . . ?
N5 Fe1 N25 92.07(15) . . ?
N5 Fe1 N31 164.93(14) . . ?
N9 Fe1 N25 160.75(17) . . ?
N15 Fe1 N9 73.48(14) . . ?
N15 Fe1 N25 92.17(14) . . ?
N31 Fe1 N9 93.90(13) . . ?
N31 Fe1 N15 90.04(15) . . ?
N31 Fe1 N25 72.91(14) . . ?
C3 N2 Fe1 163.6(3) . . ?
N2 C3 Se4 176.8(4) . . ?
C6 N5 Fe1 164.6(4) . . ?
N5 C6 Se7A 174.6(5) . . ?
N5 C6 Se7B 172.1(5) . . ?
N9 C8 H8 116.2 . . ?
N13 C8 H8 116.2 . . ?
N13 C8 N9 127.6(5) . . ?
C8 N9 Fe1 127.3(3) . . ?
C8 N9 C10 115.4(4) . . ?
C10 N9 Fe1 116.8(3) . . ?
N9 C10 C11 123.4(5) . . ?
N9 C10 N14 115.4(3) . . ?
C11 C10 N14 121.2(4) . . ?
C10 C11 H11 122.7 . . ?
C10 C11 C12 114.7(5) . . ?
C12 C11 H11 122.7 . . ?
C11 C12 N19 120.1(5) . . ?
N13 C12 C11 124.4(4) . . ?
N13 C12 N19 115.6(5) . . ?
C8 N13 C12 114.5(4) . . ?
N15 N14 C10 119.1(4) . . ?
N15 N14 C18 110.7(4) . . ?
C18 N14 C10 130.1(4) . . ?
N14 N15 Fe1 115.2(3) . . ?
C16 N15 Fe1 139.4(3) . . ?
C16 N15 N14 105.2(4) . . ?
N15 C16 H16 123.9 . . ?
N15 C16 C17 112.2(4) . . ?
C17 C16 H16 123.9 . . ?
C16 C17 H17 127.7 . . ?
C18 C17 C16 104.6(5) . . ?
C18 C17 H17 127.7 . . ?
N14 C18 H18 126.4 . . ?
C17 C18 N14 107.3(4) . . ?
C17 C18 H18 126.4 . . ?
N20 N19 C12 119.3(5) . . ?
C23 N19 C12 127.5(5) . . ?
C23 N19 N20 113.2(4) . . ?
C21 N20 N19 103.6(6) . . ?
N20 C21 H21 124.0 . . ?
N20 C21 C22 112.0(6) . . ?
C22 C21 H21 124.0 . . ?
C21 C22 H22 126.6 . . ?
C23 C22 C21 106.9(6) . . ?
C23 C22 H22 126.6 . . ?
N19 C23 C22 104.3(7) . . ?
N19 C23 H23 127.8 . . ?
C22 C23 H23 127.8 . . ?
N25 C24 H24 116.6 . . ?
N25 C24 N29 126.7(5) . . ?
N29 C24 H24 116.6 . . ?
C24 N25 Fe1 126.4(3) . . ?
C24 N25 C26 116.0(4) . . ?
C26 N25 Fe1 116.9(3) . . ?
N25 C26 C27 123.0(4) . . ?
N25 C26 N30 115.0(3) . . ?
C27 C26 N30 122.0(4) . . ?
C26 C27 H27 122.4 . . ?
C28 C27 C26 115.3(4) . . ?
C28 C27 H27 122.4 . . ?
C27 C28 N35 121.4(4) . . ?
N29 C28 C27 124.1(4) . . ?
N29 C28 N35 114.4(4) . . ?
C24 N29 C28 114.6(4) . . ?
N31 N30 C26 118.4(4) . . ?
C34 N30 C26 130.1(3) . . ?
C34 N30 N31 111.4(3) . . ?
N30 N31 Fe1 116.3(3) . . ?
C32 N31 Fe1 138.9(3) . . ?
C32 N31 N30 104.6(4) . . ?
N31 C32 H32 123.9 . . ?
N31 C32 C33 112.2(4) . . ?
C33 C32 H32 123.9 . . ?
C32 C33 H33 127.3 . . ?
C34 C33 C32 105.3(5) . . ?
C34 C33 H33 127.3 . . ?
N30 C34 C33 106.4(4) . . ?
N30 C34 H34 126.8 . . ?
C33 C34 H34 126.8 . . ?
N36 N35 C28 120.1(4) . . ?
C39 N35 C28 127.6(4) . . ?
C39 N35 N36 112.3(3) . . ?
C37 N36 N35 103.0(4) . . ?
N36 C37 H37 123.5 . . ?
N36 C37 C38 113.0(4) . . ?
C38 C37 H37 123.5 . . ?
C37 C38 H38 127.5 . . ?
C39 C38 C37 104.9(4) . . ?
C39 C38 H38 127.5 . . ?
N35 C39 C38 106.7(4) . . ?
N35 C39 H39 126.6 . . ?
C38 C39 H39 126.6 . . ?
O40A C41A C42A 124.8(16) . . ?
O40A C41A C43A 124.0(16) . . ?
C42A C41A C43A 108.2(12) . . ?
C41A C42A H42A 109.5 . . ?
C41A C42A H42B 109.5 . . ?
C41A C42A H42C 109.5 . . ?
H42A C42A H42B 109.5 . . ?
H42A C42A H42C 109.5 . . ?
H42B C42A H42C 109.5 . . ?
C41A C43A H43A 109.5 . . ?
C41A C43A H43B 109.5 . . ?
C41A C43A H43C 109.5 . . ?
H43A C43A H43B 109.5 . . ?
H43A C43A H43C 109.5 . . ?
H43B C43A H43C 109.5 . . ?
C41B C42B H42D 109.5 . . ?
C41B C42B H42E 109.5 . . ?
C41B C42B H42F 109.5 . . ?
H42D C42B H42E 109.5 . . ?
H42D C42B H42F 109.5 . . ?
H42E C42B H42F 109.5 . . ?
C41B C43B H43D 109.5 . . ?
C41B C43B H43E 109.5 . . ?
C41B C43B H43F 109.5 . . ?
H43D C43B H43E 109.5 . . ?
H43D C43B H43F 109.5 . . ?
H43E C43B H43F 109.5 . . ?

_exptl_crystal_recrystallization_method 
'Re-crystallisation from solvent: acetone'
_exptl_crystal_preparation       'Magnetic properties'
