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

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

data_temp
_audit_block_doi                 10.5517/ccdc.csd.cc142wjm
_database_code_depnum_ccdc_archive 'CCDC 1045460'
_audit_update_record             
;
2015-01-24 deposited with the CCDC.
2017-10-12 downloaded from the CCDC.
;

# start Validation Reply Form
_vrf_PLAT415_temp                
;
PROBLEM: Short Inter D-H..H-X       H8B    ..  H9D     ..       1.71 Ang.  
RESPONSE: Difference electron density plots indicate two positions
which were assigned for partially occupied water molecules. The 
hydrogen atoms on these water molecules were placed only to 
satisfy the stoichiometry. No efforts were made to determine
the actual locations of these hydrogen atoms.
;
# end Validation Reply Form



_audit_creation_date             2015-01-23
_audit_creation_method           
;
Olex2 1.2-beta
(compiled 2014.10.22 svn.r3046 for OlexSys, GUI svn.r4928)
;
_shelxl_version_number           2014-3
_chemical_name_common            ?
_chemical_name_systematic        
;
 ?
;
_chemical_formula_moiety         
'C20 H39 Fe2 N8 Ni2 O4 S4, 0.36(H2 O), 2(C H2 Cl2), 1.77(B F4)'
_chemical_formula_sum            
'C22 H43.73 B1.77 Cl4 F7.08 Fe2 N8 Ni2 O4.36 S4'
_chemical_formula_weight         1143.02
_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'
B B 0.0013 0.0007 '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'
F F 0.0171 0.0103 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Fe Fe 0.3463 0.8444 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Ni Ni 0.3393 1.1124 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
S S 0.1246 0.1234 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'

_shelx_space_group_comment       
;
The symmetry employed for this shelxl refinement is uniquely defined
by the following loop, which should always be used as a source of
symmetry information in preference to the above space-group names.
They are only intended as comments.
;
_space_group_crystal_system      triclinic
_space_group_IT_number           2
_space_group_name_H-M_alt        'P -1'
_space_group_name_Hall           '-P 1'
loop_
_space_group_symop_operation_xyz
'x, y, z'
'-x, -y, -z'

_cell_length_a                   11.6249(9)
_cell_length_b                   14.1066(11)
_cell_length_c                   14.2931(11)
_cell_angle_alpha                99.860(2)
_cell_angle_beta                 104.520(3)
_cell_angle_gamma                105.715(2)
_cell_volume                     2111.1(3)
_cell_formula_units_Z            2
_cell_measurement_reflns_used    9973
_cell_measurement_temperature    110(2)
_cell_measurement_theta_max      37.148
_cell_measurement_theta_min      2.657
_shelx_estimated_absorpt_T_max   0.751
_shelx_estimated_absorpt_T_min   0.321
_exptl_absorpt_coefficient_mu    2.076
_exptl_absorpt_correction_T_max  0.8685
_exptl_absorpt_correction_T_min  0.3427
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   
;
SADABS-2012/1 (Bruker,2012) was used for absorption correction.
wR2(int) was 0.0938 before and 0.0484 after correction.
The Ratio of minimum to maximum transmission is 0.3946.
The λ/2 correction factor is 0.0015.
;
_exptl_crystal_colour            green
_exptl_crystal_colour_primary    green
_exptl_crystal_density_diffrn    1.798
_exptl_crystal_density_meas      .
_exptl_crystal_density_method    ?
_exptl_crystal_description       block
_exptl_crystal_F_000             1158
_exptl_crystal_size_max          0.708
_exptl_crystal_size_mid          0.499
_exptl_crystal_size_min          0.146
_exptl_special_details           
;
 ?
;
_exptl_transmission_factor_max   ?
_exptl_transmission_factor_min   ?
_diffrn_reflns_av_R_equivalents  0.0448
_diffrn_reflns_av_unetI/netI     0.0352
_diffrn_reflns_Laue_measured_fraction_full 0.999
_diffrn_reflns_Laue_measured_fraction_max 0.964
_diffrn_reflns_limit_h_max       20
_diffrn_reflns_limit_h_min       -20
_diffrn_reflns_limit_k_max       24
_diffrn_reflns_limit_k_min       -24
_diffrn_reflns_limit_l_max       24
_diffrn_reflns_limit_l_min       -25
_diffrn_reflns_number            120215
_diffrn_reflns_point_group_measured_fraction_full 0.999
_diffrn_reflns_point_group_measured_fraction_max 0.964
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         38.680
_diffrn_reflns_theta_min         1.523
_diffrn_ambient_temperature      110(2)
_diffrn_detector_area_resol_mean ?
_diffrn_measured_fraction_theta_full 0.999
_diffrn_measured_fraction_theta_max 0.964
_diffrn_measurement_device_type  'Bruker APEX-II CCD'
_diffrn_measurement_method       'φ and ω scans'
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_source                   ?
_diffrn_special_details          ?
_diffrn_standards_number         0
_reflns_Friedel_coverage         0.000
_reflns_Friedel_fraction_full    .
_reflns_Friedel_fraction_max     .
_reflns_number_gt                17077
_reflns_number_total             23189
_reflns_special_details          
;
 Reflections were merged by SHELXL according to the crystal
 class for the calculation of statistics and refinement.
 
 _reflns_Friedel_fraction is defined as the number of unique
 Friedel pairs measured divided by the number that would be
 possible theoretically, ignoring centric projections and
 systematic absences.
;
_reflns_threshold_expression     'I > 2σ(I)'
_computing_cell_refinement       'SAINT v8.27A (Bruker, 2012)'
_computing_data_collection       ?
_computing_data_reduction        'SAINT v8.27A (Bruker, 2012)'
_computing_molecular_graphics    'Olex2 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 (Dolomanov et al., 2009)'
_computing_structure_refinement  'XL (Sheldrick, 2008)'
_computing_structure_solution    ?
_refine_diff_density_max         1.504
_refine_diff_density_min         -0.973
_refine_diff_density_rms         0.122
_refine_ls_extinction_coef       .
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.025
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     597
_refine_ls_number_reflns         23189
_refine_ls_number_restraints     238
_refine_ls_R_factor_all          0.0651
_refine_ls_R_factor_gt           0.0410
_refine_ls_restrained_S_all      1.025
_refine_ls_shift/su_max          0.001
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details     
'w=1/[σ²(Fo²)+(0.0607P)²+1.7770P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1102
_refine_ls_wR_factor_ref         0.1255
_refine_special_details          
;
 ?
;
_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 O(H,H) groups
2. Restrained distances
 Cl3S-C1T \\sim Cl3S-C1S \\sim Cl2S-C1S \\sim Cl2T-C1T
 with sigma of 0.01
3. Uiso/Uaniso restraints and constraints
Cl3S \\sim C1S \\sim Cl2S \\sim C1T \\sim Cl2T: within 1.7A with sigma of 0.01
and sigma for terminal atoms of 0.02
B2 \\sim F5 \\sim F6 \\sim F7 \\sim F8 \\sim B2A \\sim F5A \\sim F6A \\sim F7A
\\sim F8A: within 1.7A with sigma of 0.01 and sigma for terminal atoms of 0.02
4. Rigid body (RIGU) restrains
 Cl3S, C1S, Cl2S, C1T, Cl2T
 with sigma for 1-2 distances of 0.01 and sigma for 1-3 distances of 0.01
 B2, F5, F6, F7, F8, B2A, F5A, F6A, F7A, F8A
 with sigma for 1-2 distances of 0.01 and sigma for 1-3 distances of 0.01
5. Same fragment restrains
{B2, F5, F6, F7, F8} sigma for 1-2: 0.01, 1-3: 0.04
as
{B2A, F5A, F6A, F7A, F8A}
6. Others
 Sof(C1T)=Sof(H1TA)=Sof(H1TB)=Sof(Cl2T)=1-FVAR(1)
 Sof(C1S)=Sof(H1SA)=Sof(H1SB)=Sof(Cl2S)=FVAR(1)
 Sof(B2A)=Sof(F5A)=Sof(F6A)=Sof(F7A)=Sof(F8A)=0.77*(1-FVAR(3))
 Sof(B2)=Sof(F5)=Sof(F6)=Sof(F7)=Sof(F8)=0.77*FVAR(3)
 Fixed Sof: O9(0.25) H9C(0.25) H9D(0.25) O5(0.11418) H5C(0.11418) H5D(0.11418)
7.a Free rotating group:
 O9(H9C,H9D), O5(H5C,H5D)
7.b Secondary CH2 refined with riding coordinates:
 C1(H1A,H1B), C2(H2A,H2B), C4(H4A,H4B), C5(H5A,H5B), C6(H6A,H6B), C7(H7A,H7B),
 C8(H8A,H8B), C9(H9A,H9B), C10(H10A,H10B), C11(H11A,H11B), C12(H12A,H12B),
 C13(H13A,H13B), C14(H14A,H14B), C15(H15A,H15B), C16(H16A,H16B), C17(H17A,H17B),
  C18(H18A,H18B), C19(H19A,H19B), C20(H20A,H20B), C1S(H1SA,H1SB), C5S(H5SA,
 H5SB), C1T(H1TA,H1TB)
;
_atom_sites_solution_hydrogens   mixed
_atom_sites_solution_primary     ?
_atom_sites_solution_secondary   ?
loop_
_atom_site_label
_atom_site_type_symbol
_atom_site_fract_x
_atom_site_fract_y
_atom_site_fract_z
_atom_site_U_iso_or_equiv
_atom_site_adp_type
_atom_site_occupancy
_atom_site_site_symmetry_order
_atom_site_calc_flag
_atom_site_refinement_flags_posn
_atom_site_refinement_flags_adp
_atom_site_refinement_flags_occupancy
_atom_site_disorder_assembly
_atom_site_disorder_group
Ni1 Ni 0.16439(2) 0.50519(2) 0.16047(2) 0.01477(4) Uani 1 1 d . . . . .
Ni2 Ni 0.17619(2) 0.19756(2) 0.30144(2) 0.01700(4) Uani 1 1 d . . . . .
Fe1 Fe -0.08265(2) 0.28251(2) 0.16745(2) 0.01921(5) Uani 1 1 d . . . . .
Fe2 Fe 0.24991(3) 0.28168(2) 0.08681(2) 0.01959(5) Uani 1 1 d . . . . .
S1 S -0.03905(4) 0.43243(3) 0.11796(3) 0.01740(7) Uani 1 1 d . . . . .
S2 S 0.16636(4) 0.40139(3) 0.02874(3) 0.01758(7) Uani 1 1 d . . . . .
S3 S 0.06907(5) 0.30091(3) 0.31778(3) 0.02167(8) Uani 1 1 d . . . . .
S4 S 0.30823(5) 0.31358(3) 0.26118(3) 0.02207(8) Uani 1 1 d . . . . .
O1 O -0.32675(19) 0.2312(2) 0.1869(2) 0.0586(6) Uani 1 1 d . . . . .
O2 O -0.13647(16) 0.12611(13) -0.00481(12) 0.0335(3) Uani 1 1 d . . . . .
O3 O 0.4667(2) 0.29071(17) 0.02672(17) 0.0458(5) Uani 1 1 d . . . . .
O4 O 0.08845(18) 0.08206(13) -0.01836(16) 0.0405(4) Uani 1 1 d . . . . .
N1 N -0.22209(17) 0.26193(16) 0.18988(15) 0.0303(3) Uani 1 1 d . . . . .
N2 N -0.09433(16) 0.19295(12) 0.06741(12) 0.0231(3) Uani 1 1 d . . . . .
N3 N 0.38442(17) 0.29589(13) 0.05774(14) 0.0260(3) Uani 1 1 d . . . . .
N4 N 0.14133(17) 0.16546(13) 0.03023(13) 0.0255(3) Uani 1 1 d . . . . .
N5 N 0.15857(14) 0.60107(11) 0.27593(11) 0.0181(2) Uani 1 1 d . . . . .
N6 N 0.34026(14) 0.58969(11) 0.18115(11) 0.0184(2) Uani 1 1 d . . . . .
N7 N 0.06278(16) 0.09871(12) 0.34909(12) 0.0228(3) Uani 1 1 d . . . . .
N8 N 0.28545(15) 0.11197(12) 0.30110(11) 0.0209(3) Uani 1 1 d . . . . .
C1 C -0.07249(18) 0.52327(14) 0.20597(13) 0.0211(3) Uani 1 1 d . . . . .
H1A H -0.0860 0.5796 0.1767 0.025 Uiso 1 1 calc R . . . .
H1B H -0.1495 0.4891 0.2211 0.025 Uiso 1 1 calc R . . . .
C2 C 0.03842(18) 0.56418(14) 0.30010(13) 0.0207(3) Uani 1 1 d . . . . .
H2A H 0.0285 0.6211 0.3450 0.025 Uiso 1 1 calc R . . . .
H2B H 0.0418 0.5099 0.3354 0.025 Uiso 1 1 calc R . . . .
C3 C 0.26137(18) 0.61086(14) 0.36862(13) 0.0219(3) Uani 1 1 d . . . . .
H3 H 0.246(3) 0.644(2) 0.418(2) 0.026 Uiso 1 1 d R . . . .
C4 C 0.39331(18) 0.66072(14) 0.36722(13) 0.0236(3) Uani 1 1 d . . . . .
H4A H 0.4023 0.7307 0.3600 0.028 Uiso 1 1 calc R . . . .
H4B H 0.4538 0.6661 0.4321 0.028 Uiso 1 1 calc R . . . .
C5 C 0.42673(17) 0.60396(14) 0.28432(13) 0.0218(3) Uani 1 1 d . . . . .
H5A H 0.4251 0.5362 0.2950 0.026 Uiso 1 1 calc R . . . .
H5B H 0.5138 0.6415 0.2880 0.026 Uiso 1 1 calc R . . . .
C6 C 0.17020(18) 0.70301(13) 0.25129(13) 0.0212(3) Uani 1 1 d . . . . .
H6A H 0.2315 0.7580 0.3092 0.025 Uiso 1 1 calc R . . . .
H6B H 0.0877 0.7140 0.2397 0.025 Uiso 1 1 calc R . . . .
C7 C 0.21248(18) 0.70962(13) 0.15939(13) 0.0215(3) Uani 1 1 d . . . . .
H7A H 0.2192 0.7781 0.1484 0.026 Uiso 1 1 calc R . . . .
H7B H 0.1457 0.6593 0.1008 0.026 Uiso 1 1 calc R . . . .
C8 C 0.33663(18) 0.69151(13) 0.16230(14) 0.0216(3) Uani 1 1 d . . . . .
H8A H 0.3520 0.6955 0.0978 0.026 Uiso 1 1 calc R . . . .
H8B H 0.4056 0.7466 0.2156 0.026 Uiso 1 1 calc R . . . .
C9 C 0.39792(17) 0.54285(14) 0.11078(13) 0.0209(3) Uani 1 1 d . . . . .
H9A H 0.4327 0.4931 0.1383 0.025 Uiso 1 1 calc R . . . .
H9B H 0.4679 0.5965 0.1036 0.025 Uiso 1 1 calc R . . . .
C10 C 0.30105(17) 0.49020(14) 0.01017(13) 0.0207(3) Uani 1 1 d . . . . .
H10A H 0.3368 0.4528 -0.0337 0.025 Uiso 1 1 calc R . . . .
H10B H 0.2743 0.5409 -0.0220 0.025 Uiso 1 1 calc R . . . .
C11 C -0.0164(2) 0.24000(18) 0.39456(16) 0.0310(4) Uani 1 1 d . . . . .
H11A H 0.0373 0.2613 0.4653 0.037 Uiso 1 1 calc R . . . .
H11B H -0.0929 0.2593 0.3908 0.037 Uiso 1 1 calc R . . . .
C12 C -0.0515(2) 0.12684(17) 0.35398(17) 0.0295(4) Uani 1 1 d . . . . .
H12A H -0.0909 0.0909 0.3975 0.035 Uiso 1 1 calc R . . . .
H12B H -0.1135 0.1052 0.2862 0.035 Uiso 1 1 calc R . . . .
C13 C 0.1361(2) 0.09712(17) 0.45256(15) 0.0289(4) Uani 1 1 d . . . . .
H13A H 0.1047 0.1308 0.5026 0.035 Uiso 1 1 calc R . . . .
H13B H 0.1207 0.0255 0.4561 0.035 Uiso 1 1 calc R . . . .
C14 C 0.2765(2) 0.14998(16) 0.47888(14) 0.0287(4) Uani 1 1 d . . . . .
H14A H 0.3176 0.1453 0.5467 0.034 Uiso 1 1 calc R . . . .
H14B H 0.2911 0.2231 0.4820 0.034 Uiso 1 1 calc R . . . .
C15 C 0.3416(2) 0.11004(15) 0.40883(14) 0.0268(4) Uani 1 1 d . . . . .
H15A H 0.3359 0.0391 0.4108 0.032 Uiso 1 1 calc R . . . .
H15B H 0.4318 0.1517 0.4330 0.032 Uiso 1 1 calc R . . . .
C16 C 0.0124(2) -0.00544(15) 0.27880(17) 0.0277(4) Uani 1 1 d . . . . .
H16A H -0.0314 -0.0008 0.2116 0.033 Uiso 1 1 calc R . . . .
H16B H -0.0507 -0.0502 0.3015 0.033 Uiso 1 1 calc R . . . .
C17 C 0.1115(2) -0.05436(15) 0.27020(18) 0.0303(4) Uani 1 1 d . . . . .
H17A H 0.1507 -0.0642 0.3362 0.036 Uiso 1 1 calc R . . . .
H17B H 0.0701 -0.1225 0.2226 0.036 Uiso 1 1 calc R . . . .
C18 C 0.2136(2) 0.00680(14) 0.23566(15) 0.0257(3) Uani 1 1 d . . . . .
H18A H 0.2736 -0.0307 0.2314 0.031 Uiso 1 1 calc R . . . .
H18B H 0.1749 0.0119 0.1674 0.031 Uiso 1 1 calc R . . . .
C19 C 0.39091(18) 0.15287(16) 0.26072(15) 0.0251(3) Uani 1 1 d . . . . .
H19A H 0.3600 0.1308 0.1867 0.030 Uiso 1 1 calc R . . . .
H19B H 0.4592 0.1249 0.2844 0.030 Uiso 1 1 calc R . . . .
C20 C 0.44161(19) 0.26722(17) 0.29422(16) 0.0285(4) Uani 1 1 d . . . . .
H20A H 0.5034 0.2940 0.2605 0.034 Uiso 1 1 calc R . . . .
H20B H 0.4840 0.2900 0.3674 0.034 Uiso 1 1 calc R . . . .
O9 O -0.5451(5) -0.0882(4) 0.3404(4) 0.0260(11) Uani 0.25 1 d . . P . .
H9C H -0.4724 -0.0416 0.3537 0.039 Uiso 0.25 1 d G . P . .
H9D H -0.5614 -0.1319 0.2840 0.039 Uiso 0.25 1 d G . P . .
C1S C 0.7225(6) 0.5206(6) 0.3833(5) 0.0560(16) Uani 0.527(7) 1 d D U P A 1
H1SA H 0.7647 0.5889 0.3763 0.067 Uiso 0.527(7) 1 calc R . P A 1
H1SB H 0.6670 0.4781 0.3161 0.067 Uiso 0.527(7) 1 calc R . P A 1
Cl2S Cl 0.8361(5) 0.4660(4) 0.4279(3) 0.0707(11) Uani 0.527(7) 1 d D U P A 1
Cl3S Cl 0.63123(7) 0.53227(5) 0.46147(5) 0.04247(13) Uani 1 1 d D U . . .
C5S C -0.4031(2) -0.0609(3) 0.1660(2) 0.0437(6) Uani 1 1 d . . . . .
H5SA H -0.3754 -0.0065 0.2287 0.052 Uiso 1 1 calc R . . . .
H5SB H -0.3996 -0.1249 0.1843 0.052 Uiso 1 1 calc R . . . .
Cl6S Cl -0.55925(6) -0.07672(5) 0.09851(6) 0.04325(14) Uani 1 1 d . . . . .
Cl7S Cl -0.30010(5) -0.02894(5) 0.09639(5) 0.03806(12) Uani 1 1 d . . . . .
B1 B 0.7745(2) 0.72107(18) 0.24935(18) 0.0268(4) Uani 1 1 d . . . . .
F1 F 0.70035(14) 0.61844(12) 0.21511(12) 0.0392(3) Uani 1 1 d . . . . .
F2 F 0.7014(2) 0.78014(17) 0.26539(19) 0.0653(6) Uani 1 1 d . . . . .
F3 F 0.8358(2) 0.74823(15) 0.18221(15) 0.0618(6) Uani 1 1 d . . . . .
F4 F 0.8642(2) 0.73324(15) 0.33984(14) 0.0595(5) Uani 1 1 d . . . . .
C1T C 0.7701(6) 0.5402(4) 0.4289(5) 0.0440(14) Uani 0.473(7) 1 d D U P A 2
H1TA H 0.7695 0.5739 0.3734 0.053 Uiso 0.473(7) 1 calc R . P A 2
H1TB H 0.8441 0.5829 0.4869 0.053 Uiso 0.473(7) 1 calc R . P A 2
Cl2T Cl 0.7848(2) 0.41987(19) 0.39209(17) 0.0381(5) Uani 0.473(7) 1 d D U P A 2
B2 B -0.2978(6) 0.1284(4) 0.4700(4) 0.0217(10) Uani 0.498(10) 1 d D U P B 1
F5 F -0.3705(4) 0.1141(3) 0.5328(3) 0.0244(7) Uani 0.498(10) 1 d D U P B 1
F6 F -0.1722(6) 0.1629(6) 0.5284(5) 0.0372(14) Uani 0.498(10) 1 d D U P B 1
F7 F -0.3197(7) 0.0376(4) 0.4042(5) 0.0531(16) Uani 0.498(10) 1 d D U P B 1
F8 F -0.3239(3) 0.1983(3) 0.4186(4) 0.0367(10) Uani 0.498(10) 1 d D U P B 1
B2A B -0.2886(10) 0.1325(8) 0.4589(8) 0.024(2) Uani 0.272(10) 1 d D U P B 2
F5A F -0.3786(7) 0.1367(9) 0.5060(7) 0.039(2) Uani 0.272(10) 1 d D U P B 2
F6A F -0.1711(9) 0.1893(7) 0.5278(8) 0.0220(17) Uani 0.272(10) 1 d D U P B 2
F7A F -0.2893(8) 0.0350(6) 0.4278(8) 0.0299(16) Uani 0.272(10) 1 d D U P B 2
F8A F -0.3105(6) 0.1682(7) 0.3746(8) 0.038(2) Uani 0.272(10) 1 d D U P B 2
O5 O 0.0883(15) 0.2970(10) 0.1526(9) 0.028(3) Uani 0.1142 1 d . . P . .
H5C H 0.0863 0.3567 0.1457 0.042 Uiso 0.1142 1 d G . P . .
H5D H 0.1174 0.2703 0.1080 0.042 Uiso 0.1142 1 d G . P . .


_geom_special_details            
;
 All esds (except the esd in the dihedral angle between two l.s. planes)
 are estimated using the full covariance matrix.  The cell esds are taken
 into account individually in the estimation of esds in distances, angles
 and torsion angles; correlations between esds in cell parameters are only
 used when they are defined by crystal symmetry.  An approximate (isotropic)
 treatment of cell esds is used for estimating esds involving l.s. planes.
;
loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
_geom_bond_publ_flag
Ni1 S1 2.1833(5) . ?
Ni1 S2 2.1875(5) . ?
Ni1 N5 1.9745(14) . ?
Ni1 N6 1.9860(15) . ?
Ni1 H5C 1.9950 . ?
Ni2 S3 2.1779(5) . ?
Ni2 S4 2.1842(5) . ?
Ni2 N7 1.9813(16) . ?
Ni2 N8 1.9755(15) . ?
Fe1 S1 2.3112(5) . ?
Fe1 S3 2.3357(5) . ?
Fe1 N1 1.6888(18) . ?
Fe1 N2 1.6882(16) . ?
Fe2 S2 2.3341(5) . ?
Fe2 S4 2.3404(6) . ?
Fe2 N3 1.6860(17) . ?
Fe2 N4 1.6877(17) . ?
Fe2 H5D 1.6148 . ?
S1 C1 1.8271(17) . ?
S2 C10 1.8306(18) . ?
S3 C11 1.827(2) . ?
S4 C20 1.828(2) . ?
O1 N1 1.163(3) . ?
O2 N2 1.165(2) . ?
O3 N3 1.164(2) . ?
O4 N4 1.166(2) . ?
N5 C2 1.500(2) . ?
N5 C3 1.502(2) . ?
N5 C6 1.517(2) . ?
N6 C5 1.507(2) . ?
N6 C8 1.516(2) . ?
N6 C9 1.499(2) . ?
N7 C12 1.500(3) . ?
N7 C13 1.518(3) . ?
N7 C16 1.498(3) . ?
N8 C15 1.522(2) . ?
N8 C18 1.495(2) . ?
N8 C19 1.502(3) . ?
C1 H1A 0.9900 . ?
C1 H1B 0.9900 . ?
C1 C2 1.506(3) . ?
C2 H2A 0.9900 . ?
C2 H2B 0.9900 . ?
C3 H3 0.87(3) . ?
C3 C4 1.511(3) . ?
C4 H4A 0.9900 . ?
C4 H4B 0.9900 . ?
C4 C5 1.507(3) . ?
C5 H5A 0.9900 . ?
C5 H5B 0.9900 . ?
C6 H6A 0.9900 . ?
C6 H6B 0.9900 . ?
C6 C7 1.522(3) . ?
C7 H7A 0.9900 . ?
C7 H7B 0.9900 . ?
C7 C8 1.524(3) . ?
C8 H8A 0.9900 . ?
C8 H8B 0.9900 . ?
C9 H9A 0.9900 . ?
C9 H9B 0.9900 . ?
C9 C10 1.502(3) . ?
C10 H10A 0.9900 . ?
C10 H10B 0.9900 . ?
C11 H11A 0.9900 . ?
C11 H11B 0.9900 . ?
C11 C12 1.504(3) . ?
C12 H12A 0.9900 . ?
C12 H12B 0.9900 . ?
C13 H13A 0.9900 . ?
C13 H13B 0.9900 . ?
C13 C14 1.516(3) . ?
C14 H14A 0.9900 . ?
C14 H14B 0.9900 . ?
C14 C15 1.520(3) . ?
C15 H15A 0.9900 . ?
C15 H15B 0.9900 . ?
C16 H16A 0.9900 . ?
C16 H16B 0.9900 . ?
C16 C17 1.514(3) . ?
C17 H17A 0.9900 . ?
C17 H17B 0.9900 . ?
C17 C18 1.511(3) . ?
C18 H18A 0.9900 . ?
C18 H18B 0.9900 . ?
C19 H19A 0.9900 . ?
C19 H19B 0.9900 . ?
C19 C20 1.503(3) . ?
C20 H20A 0.9900 . ?
C20 H20B 0.9900 . ?
O9 H9C 0.8702 . ?
O9 H9D 0.8699 . ?
C1S H1SA 0.9900 . ?
C1S H1SB 0.9900 . ?
C1S Cl2S 1.744(5) . ?
C1S Cl3S 1.740(5) . ?
Cl3S C1T 1.771(5) . ?
C5S H5SA 0.9900 . ?
C5S H5SB 0.9900 . ?
C5S Cl6S 1.763(3) . ?
C5S Cl7S 1.757(3) . ?
B1 F1 1.396(3) . ?
B1 F2 1.373(3) . ?
B1 F3 1.377(3) . ?
B1 F4 1.393(3) . ?
C1T H1TA 0.9900 . ?
C1T H1TB 0.9900 . ?
C1T Cl2T 1.756(5) . ?
B2 F5 1.383(6) . ?
B2 F6 1.389(6) . ?
B2 F7 1.371(5) . ?
B2 F8 1.379(6) . ?
B2A F5A 1.386(8) . ?
B2A F6A 1.393(8) . ?
B2A F7A 1.369(8) . ?
B2A F8A 1.375(8) . ?
O5 H5C 0.8700 . ?
O5 H5D 0.8701 . ?

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
S1 Ni1 S2 89.223(17) . . ?
S1 Ni1 H5C 57.9 . . ?
S2 Ni1 H5C 63.6 . . ?
N5 Ni1 S1 89.79(5) . . ?
N5 Ni1 S2 177.80(4) . . ?
N5 Ni1 N6 90.17(6) . . ?
N5 Ni1 H5C 117.4 . . ?
N6 Ni1 S1 168.15(4) . . ?
N6 Ni1 S2 90.40(4) . . ?
N6 Ni1 H5C 131.7 . . ?
S3 Ni2 S4 88.85(2) . . ?
N7 Ni2 S3 90.09(5) . . ?
N7 Ni2 S4 175.48(5) . . ?
N8 Ni2 S3 173.89(5) . . ?
N8 Ni2 S4 90.23(5) . . ?
N8 Ni2 N7 90.36(7) . . ?
S1 Fe1 S3 109.815(19) . . ?
N1 Fe1 S1 107.49(7) . . ?
N1 Fe1 S3 107.24(7) . . ?
N2 Fe1 S1 104.18(6) . . ?
N2 Fe1 S3 117.04(6) . . ?
N2 Fe1 N1 110.72(9) . . ?
S2 Fe2 S4 112.243(18) . . ?
S2 Fe2 H5D 70.2 . . ?
S4 Fe2 H5D 77.6 . . ?
N3 Fe2 S2 106.61(6) . . ?
N3 Fe2 S4 105.77(7) . . ?
N3 Fe2 N4 112.89(9) . . ?
N3 Fe2 H5D 176.2 . . ?
N4 Fe2 S2 107.50(6) . . ?
N4 Fe2 S4 111.78(6) . . ?
N4 Fe2 H5D 66.9 . . ?
Ni1 S1 Fe1 109.573(19) . . ?
C1 S1 Ni1 98.56(6) . . ?
C1 S1 Fe1 105.68(6) . . ?
Ni1 S2 Fe2 106.442(19) . . ?
C10 S2 Ni1 95.62(6) . . ?
C10 S2 Fe2 102.77(6) . . ?
Ni2 S3 Fe1 111.98(2) . . ?
C11 S3 Ni2 97.29(7) . . ?
C11 S3 Fe1 106.05(8) . . ?
Ni2 S4 Fe2 108.95(2) . . ?
C20 S4 Ni2 96.72(7) . . ?
C20 S4 Fe2 104.32(7) . . ?
O1 N1 Fe1 165.4(2) . . ?
O2 N2 Fe1 161.61(16) . . ?
O3 N3 Fe2 169.1(2) . . ?
O4 N4 Fe2 163.78(17) . . ?
C2 N5 Ni1 112.09(11) . . ?
C2 N5 C3 105.23(13) . . ?
C2 N5 C6 109.16(13) . . ?
C3 N5 Ni1 110.51(11) . . ?
C3 N5 C6 111.47(14) . . ?
C6 N5 Ni1 108.39(10) . . ?
C5 N6 Ni1 112.67(11) . . ?
C5 N6 C8 110.75(13) . . ?
C8 N6 Ni1 107.16(11) . . ?
C9 N6 Ni1 112.50(11) . . ?
C9 N6 C5 105.19(14) . . ?
C9 N6 C8 108.55(13) . . ?
C12 N7 Ni2 111.85(12) . . ?
C12 N7 C13 109.51(16) . . ?
C13 N7 Ni2 107.96(13) . . ?
C16 N7 Ni2 111.55(12) . . ?
C16 N7 C12 104.94(16) . . ?
C16 N7 C13 111.04(15) . . ?
C15 N8 Ni2 107.53(12) . . ?
C18 N8 Ni2 111.34(12) . . ?
C18 N8 C15 111.30(15) . . ?
C18 N8 C19 105.61(15) . . ?
C19 N8 Ni2 112.44(11) . . ?
C19 N8 C15 108.64(15) . . ?
S1 C1 H1A 110.1 . . ?
S1 C1 H1B 110.1 . . ?
H1A C1 H1B 108.4 . . ?
C2 C1 S1 107.98(12) . . ?
C2 C1 H1A 110.1 . . ?
C2 C1 H1B 110.1 . . ?
N5 C2 C1 110.50(14) . . ?
N5 C2 H2A 109.6 . . ?
N5 C2 H2B 109.6 . . ?
C1 C2 H2A 109.6 . . ?
C1 C2 H2B 109.6 . . ?
H2A C2 H2B 108.1 . . ?
N5 C3 H3 106.2(19) . . ?
N5 C3 C4 114.90(14) . . ?
C4 C3 H3 111.6(19) . . ?
C3 C4 H4A 108.8 . . ?
C3 C4 H4B 108.8 . . ?
H4A C4 H4B 107.7 . . ?
C5 C4 C3 113.64(15) . . ?
C5 C4 H4A 108.8 . . ?
C5 C4 H4B 108.8 . . ?
N6 C5 H5A 108.8 . . ?
N6 C5 H5B 108.8 . . ?
C4 C5 N6 113.99(15) . . ?
C4 C5 H5A 108.8 . . ?
C4 C5 H5B 108.8 . . ?
H5A C5 H5B 107.7 . . ?
N5 C6 H6A 109.1 . . ?
N5 C6 H6B 109.1 . . ?
N5 C6 C7 112.53(13) . . ?
H6A C6 H6B 107.8 . . ?
C7 C6 H6A 109.1 . . ?
C7 C6 H6B 109.1 . . ?
C6 C7 H7A 108.1 . . ?
C6 C7 H7B 108.1 . . ?
C6 C7 C8 116.66(15) . . ?
H7A C7 H7B 107.3 . . ?
C8 C7 H7A 108.1 . . ?
C8 C7 H7B 108.1 . . ?
N6 C8 C7 113.67(14) . . ?
N6 C8 H8A 108.8 . . ?
N6 C8 H8B 108.8 . . ?
C7 C8 H8A 108.8 . . ?
C7 C8 H8B 108.8 . . ?
H8A C8 H8B 107.7 . . ?
N6 C9 H9A 109.6 . . ?
N6 C9 H9B 109.6 . . ?
N6 C9 C10 110.34(14) . . ?
H9A C9 H9B 108.1 . . ?
C10 C9 H9A 109.6 . . ?
C10 C9 H9B 109.6 . . ?
S2 C10 H10A 110.1 . . ?
S2 C10 H10B 110.1 . . ?
C9 C10 S2 108.02(12) . . ?
C9 C10 H10A 110.1 . . ?
C9 C10 H10B 110.1 . . ?
H10A C10 H10B 108.4 . . ?
S3 C11 H11A 110.3 . . ?
S3 C11 H11B 110.3 . . ?
H11A C11 H11B 108.6 . . ?
C12 C11 S3 106.88(14) . . ?
C12 C11 H11A 110.3 . . ?
C12 C11 H11B 110.3 . . ?
N7 C12 C11 110.51(18) . . ?
N7 C12 H12A 109.5 . . ?
N7 C12 H12B 109.5 . . ?
C11 C12 H12A 109.5 . . ?
C11 C12 H12B 109.5 . . ?
H12A C12 H12B 108.1 . . ?
N7 C13 H13A 109.0 . . ?
N7 C13 H13B 109.0 . . ?
H13A C13 H13B 107.8 . . ?
C14 C13 N7 112.91(16) . . ?
C14 C13 H13A 109.0 . . ?
C14 C13 H13B 109.0 . . ?
C13 C14 H14A 108.1 . . ?
C13 C14 H14B 108.1 . . ?
C13 C14 C15 116.74(18) . . ?
H14A C14 H14B 107.3 . . ?
C15 C14 H14A 108.1 . . ?
C15 C14 H14B 108.1 . . ?
N8 C15 H15A 108.9 . . ?
N8 C15 H15B 108.9 . . ?
C14 C15 N8 113.20(16) . . ?
C14 C15 H15A 108.9 . . ?
C14 C15 H15B 108.9 . . ?
H15A C15 H15B 107.8 . . ?
N7 C16 H16A 108.7 . . ?
N7 C16 H16B 108.7 . . ?
N7 C16 C17 114.32(17) . . ?
H16A C16 H16B 107.6 . . ?
C17 C16 H16A 108.7 . . ?
C17 C16 H16B 108.7 . . ?
C16 C17 H17A 108.8 . . ?
C16 C17 H17B 108.8 . . ?
H17A C17 H17B 107.7 . . ?
C18 C17 C16 113.85(17) . . ?
C18 C17 H17A 108.8 . . ?
C18 C17 H17B 108.8 . . ?
N8 C18 C17 114.86(16) . . ?
N8 C18 H18A 108.6 . . ?
N8 C18 H18B 108.6 . . ?
C17 C18 H18A 108.6 . . ?
C17 C18 H18B 108.6 . . ?
H18A C18 H18B 107.5 . . ?
N8 C19 H19A 109.5 . . ?
N8 C19 H19B 109.5 . . ?
N8 C19 C20 110.75(16) . . ?
H19A C19 H19B 108.1 . . ?
C20 C19 H19A 109.5 . . ?
C20 C19 H19B 109.5 . . ?
S4 C20 H20A 110.2 . . ?
S4 C20 H20B 110.2 . . ?
C19 C20 S4 107.38(13) . . ?
C19 C20 H20A 110.2 . . ?
C19 C20 H20B 110.2 . . ?
H20A C20 H20B 108.5 . . ?
H9C O9 H9D 109.5 . . ?
H1SA C1S H1SB 107.8 . . ?
Cl2S C1S H1SA 109.1 . . ?
Cl2S C1S H1SB 109.1 . . ?
Cl3S C1S H1SA 109.1 . . ?
Cl3S C1S H1SB 109.1 . . ?
Cl3S C1S Cl2S 112.6(3) . . ?
H5SA C5S H5SB 107.9 . . ?
Cl6S C5S H5SA 109.3 . . ?
Cl6S C5S H5SB 109.3 . . ?
Cl7S C5S H5SA 109.3 . . ?
Cl7S C5S H5SB 109.3 . . ?
Cl7S C5S Cl6S 111.72(15) . . ?
F2 B1 F1 109.9(2) . . ?
F2 B1 F3 111.8(2) . . ?
F2 B1 F4 108.9(2) . . ?
F3 B1 F1 109.96(18) . . ?
F3 B1 F4 108.5(2) . . ?
F4 B1 F1 107.62(19) . . ?
Cl3S C1T H1TA 109.2 . . ?
Cl3S C1T H1TB 109.2 . . ?
H1TA C1T H1TB 107.9 . . ?
Cl2T C1T Cl3S 112.2(3) . . ?
Cl2T C1T H1TA 109.2 . . ?
Cl2T C1T H1TB 109.2 . . ?
F5 B2 F6 107.9(5) . . ?
F7 B2 F5 110.2(5) . . ?
F7 B2 F6 107.8(5) . . ?
F7 B2 F8 110.2(5) . . ?
F8 B2 F5 110.1(4) . . ?
F8 B2 F6 110.6(5) . . ?
F5A B2A F6A 107.8(9) . . ?
F7A B2A F5A 112.1(8) . . ?
F7A B2A F6A 108.1(8) . . ?
F7A B2A F8A 106.1(8) . . ?
F8A B2A F5A 111.2(8) . . ?
F8A B2A F6A 111.6(9) . . ?
H5C O5 H5D 109.5 . . ?

loop_
_geom_torsion_atom_site_label_1
_geom_torsion_atom_site_label_2
_geom_torsion_atom_site_label_3
_geom_torsion_atom_site_label_4
_geom_torsion
_geom_torsion_site_symmetry_1
_geom_torsion_site_symmetry_2
_geom_torsion_site_symmetry_3
_geom_torsion_site_symmetry_4
_geom_torsion_publ_flag
Ni1 S1 C1 C2 -33.06(13) . . . . ?
Ni1 S2 C10 C9 42.21(12) . . . . ?
Ni1 N5 C2 C1 -43.93(16) . . . . ?
Ni1 N5 C3 C4 66.66(17) . . . . ?
Ni1 N5 C6 C7 -13.21(18) . . . . ?
Ni1 N6 C5 C4 -63.20(17) . . . . ?
Ni1 N6 C8 C7 14.15(17) . . . . ?
Ni1 N6 C9 C10 36.30(16) . . . . ?
Ni2 S3 C11 C12 -39.44(15) . . . . ?
Ni2 S4 C20 C19 40.14(14) . . . . ?
Ni2 N7 C12 C11 -40.90(19) . . . . ?
Ni2 N7 C13 C14 -13.0(2) . . . . ?
Ni2 N7 C16 C17 64.6(2) . . . . ?
Ni2 N8 C15 C14 13.8(2) . . . . ?
Ni2 N8 C18 C17 -64.82(19) . . . . ?
Ni2 N8 C19 C20 38.20(18) . . . . ?
Fe1 S1 C1 C2 80.15(12) . . . . ?
Fe1 S3 C11 C12 76.00(15) . . . . ?
Fe2 S2 C10 C9 -66.09(12) . . . . ?
Fe2 S4 C20 C19 -71.43(14) . . . . ?
S1 Fe1 N1 O1 109.2(8) . . . . ?
S1 Fe1 N2 O2 -102.1(5) . . . . ?
S1 C1 C2 N5 50.68(16) . . . . ?
S2 Fe2 N3 O3 -110.0(10) . . . . ?
S2 Fe2 N4 O4 116.2(7) . . . . ?
S3 Fe1 N1 O1 -132.7(8) . . . . ?
S3 Fe1 N2 O2 136.5(5) . . . . ?
S3 C11 C12 N7 53.78(19) . . . . ?
S4 Fe2 N3 O3 130.4(9) . . . . ?
S4 Fe2 N4 O4 -120.2(7) . . . . ?
N1 Fe1 N2 O2 13.2(5) . . . . ?
N2 Fe1 N1 O1 -4.0(8) . . . . ?
N3 Fe2 N4 O4 -1.1(7) . . . . ?
N4 Fe2 N3 O3 7.8(10) . . . . ?
N5 C3 C4 C5 -60.8(2) . . . . ?
N5 C6 C7 C8 -57.1(2) . . . . ?
N6 C9 C10 S2 -53.33(16) . . . . ?
N7 C13 C14 C15 -57.5(2) . . . . ?
N7 C16 C17 C18 -58.6(2) . . . . ?
N8 C19 C20 S4 -52.71(18) . . . . ?
C2 N5 C3 C4 -172.14(15) . . . . ?
C2 N5 C6 C7 -135.55(15) . . . . ?
C3 N5 C2 C1 -164.10(14) . . . . ?
C3 N5 C6 C7 108.62(17) . . . . ?
C3 C4 C5 N6 58.0(2) . . . . ?
C5 N6 C8 C7 -109.10(17) . . . . ?
C5 N6 C9 C10 159.30(14) . . . . ?
C6 N5 C2 C1 76.15(17) . . . . ?
C6 N5 C3 C4 -53.94(19) . . . . ?
C6 C7 C8 N6 56.6(2) . . . . ?
C8 N6 C5 C4 56.81(19) . . . . ?
C8 N6 C9 C10 -82.11(17) . . . . ?
C9 N6 C5 C4 173.90(15) . . . . ?
C9 N6 C8 C7 135.89(15) . . . . ?
C12 N7 C13 C14 -134.98(18) . . . . ?
C12 N7 C16 C17 -174.14(17) . . . . ?
C13 N7 C12 C11 78.74(19) . . . . ?
C13 N7 C16 C17 -55.9(2) . . . . ?
C13 C14 C15 N8 57.2(2) . . . . ?
C15 N8 C18 C17 55.1(2) . . . . ?
C15 N8 C19 C20 -80.70(18) . . . . ?
C16 N7 C12 C11 -162.00(16) . . . . ?
C16 N7 C13 C14 109.60(19) . . . . ?
C16 C17 C18 N8 58.9(2) . . . . ?
C18 N8 C15 C14 -108.43(19) . . . . ?
C18 N8 C19 C20 159.81(15) . . . . ?
C19 N8 C15 C14 135.69(17) . . . . ?
C19 N8 C18 C17 172.87(16) . . . . ?
C1S Cl3S C1T Cl2T -72.6(7) . . . . ?
Cl2S C1S Cl3S C1T 45.5(5) . . . . ?

_olex2_submission_special_instructions 'No special instructions were received'
####################################################################### 
# 
# 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_nidacoox
_database_code_depnum_ccdc_archive 'CCDC 1565539'
_audit_update_record             
;
2017-07-28 deposited with the CCDC.
2017-10-12 downloaded from the CCDC.
;


# start Validation Reply Form
_vrf_PLAT094_nidacoox            
;
PROBLEM: Ratio of Maximum / Minimum Residual Density ....       4.51 Report
RESPONSE: A residual electron density of about 2.0 e-/A^3 was found 
probably associated with partially occupied solvent. The volume 
occupied is too small to SQUEEZE using platon. A possible hydration
with water was rejected as the compound undergoes elimination of NO
with addition of water.
;
_vrf_PLAT410_nidacoox            
;
PROBLEM: Short Intra H...H Contact  H15A   ..  H19A    ..       1.85 Ang.  
RESPONSE: DACO ligand was found disordered - Several restraints
were used to keep the bond distances, angles, and thermal
parameters meaningful. This results in shorter H-H distances.
In addition, the N4 atom shows slightly elongated ellipsoid
suggesting further disorder - no efforts were made to model the latter.

;
# end Validation Reply Form




_audit_creation_date             2016-03-07
_audit_creation_method           
;
Olex2 1.2-beta
(compiled 2015.11.10 svn.r3248 for OlexSys, GUI svn.r5133)
;
_shelxl_version_number           2014/6
_chemical_name_common            ?
_chemical_name_systematic        ?
_chemical_formula_moiety         'C20 H40 Fe N6 Ni2 O2 S4, B F4'
_chemical_formula_sum            'C20 H40 B F4 Fe N6 Ni2 O2 S4'
_chemical_formula_weight         784.90
_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'
B B 0.0013 0.0007 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
F F 0.0171 0.0103 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Fe Fe 0.3463 0.8444 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Ni Ni 0.3393 1.1124 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
S S 0.1246 0.1234 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'

_shelx_space_group_comment       
;
The symmetry employed for this shelxl refinement is uniquely defined
by the following loop, which should always be used as a source of
symmetry information in preference to the above space-group names.
They are only intended as comments.
;
_space_group_crystal_system      triclinic
_space_group_IT_number           2
_space_group_name_H-M_alt        'P -1'
_space_group_name_Hall           '-P 1'
loop_
_space_group_symop_operation_xyz
'x, y, z'
'-x, -y, -z'

_cell_length_a                   8.5324(11)
_cell_length_b                   13.8268(18)
_cell_length_c                   13.8581(18)
_cell_angle_alpha                88.197(2)
_cell_angle_beta                 72.322(2)
_cell_angle_gamma                80.263(2)
_cell_volume                     1534.9(3)
_cell_formula_units_Z            2
_cell_measurement_reflns_used    9952
_cell_measurement_temperature    150
_cell_measurement_theta_max      27.503
_cell_measurement_theta_min      2.542
_shelx_estimated_absorpt_T_max   0.972
_shelx_estimated_absorpt_T_min   0.451
_exptl_absorpt_coefficient_mu    2.008
_exptl_absorpt_correction_T_max  0.7456
_exptl_absorpt_correction_T_min  0.6362
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   
;
SADABS-2014/3 (Bruker,2014/3) was used for absorption correction.
wR2(int) was 0.0688 before and 0.0415 after correction.
The Ratio of minimum to maximum transmission is 0.8533.
The λ/2 correction factor is Not present.
;
_exptl_absorpt_special_details   ?
_exptl_crystal_colour            'dark brown'
_exptl_crystal_colour_modifier   dark
_exptl_crystal_colour_primary    brown
_exptl_crystal_density_diffrn    1.698
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    ?
_exptl_crystal_description       plate
_exptl_crystal_F_000             810
_exptl_crystal_size_max          0.471
_exptl_crystal_size_mid          0.067
_exptl_crystal_size_min          0.014
_exptl_transmission_factor_max   ?
_exptl_transmission_factor_min   ?
_diffrn_reflns_av_R_equivalents  0.0310
_diffrn_reflns_av_unetI/netI     0.0255
_diffrn_reflns_Laue_measured_fraction_full 0.998
_diffrn_reflns_Laue_measured_fraction_max 0.990
_diffrn_reflns_limit_h_max       11
_diffrn_reflns_limit_h_min       -11
_diffrn_reflns_limit_k_max       17
_diffrn_reflns_limit_k_min       -17
_diffrn_reflns_limit_l_max       18
_diffrn_reflns_limit_l_min       -17
_diffrn_reflns_number            28965
_diffrn_reflns_point_group_measured_fraction_full 0.998
_diffrn_reflns_point_group_measured_fraction_max 0.990
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         27.552
_diffrn_reflns_theta_min         1.495
_diffrn_ambient_temperature      150
_diffrn_detector_area_resol_mean ?
_diffrn_measured_fraction_theta_full 0.998
_diffrn_measured_fraction_theta_max 0.990
_diffrn_measurement_device_type  'Bruker APEX-II CCD'
_diffrn_measurement_method       'φ and ω scans'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_source                   ?
_diffrn_special_details          ?
_diffrn_standards_number         0
_reflns_Friedel_coverage         0.000
_reflns_Friedel_fraction_full    .
_reflns_Friedel_fraction_max     .
_reflns_number_gt                5842
_reflns_number_total             6997
_reflns_special_details          
;
 Reflections were merged by SHELXL according to the crystal
 class for the calculation of statistics and refinement.
 
 _reflns_Friedel_fraction is defined as the number of unique
 Friedel pairs measured divided by the number that would be
 possible theoretically, ignoring centric projections and
 systematic absences.
;
_reflns_threshold_expression     'I > 2σ(I)'
_computing_cell_refinement       'SAINT v8.34A (Bruker, 2013)'
_computing_data_collection       ?
_computing_data_reduction        'SAINT v8.34A (Bruker, 2013)'
_computing_molecular_graphics    'Olex2 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 (Dolomanov et al., 2009)'
_computing_structure_refinement  'ShelXL (Sheldrick, 2015)'
_computing_structure_solution    'ShelXT (Sheldrick, 2015)'
_refine_diff_density_max         2.025
_refine_diff_density_min         -0.449
_refine_diff_density_rms         0.076
_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     445
_refine_ls_number_reflns         6997
_refine_ls_number_restraints     503
_refine_ls_R_factor_all          0.0451
_refine_ls_R_factor_gt           0.0359
_refine_ls_restrained_S_all      1.061
_refine_ls_shift/su_max          0.001
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details     
'w=1/[σ²(Fo²)+(0.0556P)²+1.3483P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0981
_refine_ls_wR_factor_ref         0.1050
_refine_special_details          ?
_olex2_refinement_description    
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H,H) groups, All C(H,H,H,H) groups
2. Restrained distances
 C20A-C19A \\sim C20-C19
 with sigma of 0.02
 S4-C20A \\sim S4-C20
 with sigma of 0.02
 N4-C19 \\sim N4-C19A
 with sigma of 0.02
 C5-C4A \\sim C5-C4 \\sim C4A-C3 \\sim C4-C3 \\sim C8-C7A \\sim C7A-C6 \\sim
C7-C6 \\sim C8-C7
 with sigma of 0.02
 B1-F1 \\sim B1-F2 \\sim B1-F3 \\sim B1-F4 \\sim B1A-F1A \\sim B1A-F2A \\sim
B1A-F3A \\sim B1A-F4A
 with sigma of 0.02
 F1-F2 \\sim F1-F3 \\sim F1-F4 \\sim F2-F3 \\sim F2-F4 \\sim F3-F4 \\sim
F1A-F2A \\sim F1A-F3A \\sim F1A-F4A ~
 F2A-F3A \\sim F2A-F4A \\sim F3A-F4A
 with sigma of 0.02
3. Uiso/Uaniso restraints and constraints
B1 \\sim F1 \\sim F2 \\sim F3 \\sim F4 \\sim B1A \\sim F1A \\sim F2A \\sim F3A
\\sim F4A: within 2A with sigma of 0.04 and sigma for terminal atoms of 0.08
C3 \\sim C4 \\sim C4A \\sim C5 \\sim C6 \\sim C7 \\sim C7A \\sim C8: within 2A
with sigma of 0.005 and sigma for terminal atoms of 0.01
S4 \\sim N4 \\sim C20 \\sim C20A \\sim C19 \\sim C19A: within 2A with sigma of
0.04 and sigma for terminal atoms of 0.08
4. Rigid body (RIGU) restrains
 B1, F1, F2, F3, F4, B1A, F1A, F2A, F3A, F4A
 with sigma for 1-2 distances of 0.004 and sigma for 1-3 distances of 0.004
 C3, C4, C4A, C5, C6, C7, C7A, C8
 with sigma for 1-2 distances of 0.005 and sigma for 1-3 distances of 0.005
 S4, N4, C20, C20A, C19, C19A
 with sigma for 1-2 distances of 0.004 and sigma for 1-3 distances of 0.004
5. Others
 Sof(H3AA)=Sof(H3AB)=Sof(C4A)=Sof(H4AA)=Sof(H4AB)=Sof(H5AA)=Sof(H5AB)=
 Sof(H6BC)=Sof(H6BD)=Sof(C7A)=Sof(H7AA)=Sof(H7AB)=Sof(H8BC)=Sof(H8BD)=1-FVAR(1)
 Sof(H3BC)=Sof(H3BD)=Sof(C4)=Sof(H4A)=Sof(H4B)=Sof(H5BC)=Sof(H5BD)=Sof(H6AA)=
 Sof(H6AB)=Sof(C7)=Sof(H7A)=Sof(H7B)=Sof(H8AA)=Sof(H8AB)=FVAR(1)
 Sof(C19A)=Sof(H19C)=Sof(H19D)=Sof(C20A)=Sof(H20C)=Sof(H20D)=1-FVAR(2)
 Sof(C19)=Sof(H19A)=Sof(H19B)=Sof(C20)=Sof(H20A)=Sof(H20B)=FVAR(2)
 Sof(B1A)=Sof(F1A)=Sof(F2A)=Sof(F3A)=Sof(F4A)=1-FVAR(3)
 Sof(B1)=Sof(F1)=Sof(F2)=Sof(F3)=Sof(F4)=FVAR(3)
6.a Secondary CH2 refined with riding coordinates:
 C1(H1A,H1B), C2(H2A,H2B), C3(H3AA,H3AB), C3(H3BC,H3BD), C4A(H4AA,H4AB),
 C4(H4A,H4B), C5(H5AA,H5AB), C5(H5BC,H5BD), C6(H6AA,H6AB), C6(H6BC,H6BD),
 C7(H7A,H7B), C7A(H7AA,H7AB), C8(H8AA,H8AB), C8(H8BC,H8BD), C9(H9A,H9B),
 C10(H10A,H10B), C11(H11A,H11B), C12(H12A,H12B), C13(H13A,H13B), C14(H14A,H14B),
  C15(H15A,H15B), C16(H16A,H16B), C17(H17A,H17B), C18(H18A,H18B), C19(H19A,
 H19B), C20(H20A,H20B), C19A(H19C,H19D), C20A(H20C,H20D)
;
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     ?
_atom_sites_solution_secondary   ?
loop_
_atom_site_label
_atom_site_type_symbol
_atom_site_fract_x
_atom_site_fract_y
_atom_site_fract_z
_atom_site_U_iso_or_equiv
_atom_site_adp_type
_atom_site_occupancy
_atom_site_site_symmetry_order
_atom_site_calc_flag
_atom_site_refinement_flags_posn
_atom_site_refinement_flags_adp
_atom_site_refinement_flags_occupancy
_atom_site_disorder_assembly
_atom_site_disorder_group
Ni1 Ni 0.44294(4) 0.13812(2) 0.86334(3) 0.03115(10) Uani 1 1 d . . . . .
S1 S 0.39264(10) 0.22605(5) 0.99967(5) 0.03736(16) Uani 1 1 d . . . . .
S2 S 0.19282(11) 0.10427(7) 0.92114(7) 0.0507(2) Uani 1 1 d . . . . .
N1 N 0.6753(3) 0.16701(18) 0.8149(2) 0.0432(6) Uani 1 1 d . . . . .
N2 N 0.4981(4) 0.04048(19) 0.7529(2) 0.0461(6) Uani 1 1 d . . . . .
C1 C 0.6018(4) 0.2490(2) 0.9837(3) 0.0505(8) Uani 1 1 d . . . . .
H1A H 0.5964 0.3123 1.0172 0.061 Uiso 1 1 calc R . . . .
H1B H 0.6619 0.1963 1.0156 0.061 Uiso 1 1 calc R . . . .
C2 C 0.6920(4) 0.2523(2) 0.8741(3) 0.0526(9) Uani 1 1 d . . . . .
H2A H 0.8117 0.2521 0.8652 0.063 Uiso 1 1 calc R . . . .
H2B H 0.6479 0.3144 0.8465 0.063 Uiso 1 1 calc R . . . .
C3 C 0.7839(5) 0.0758(2) 0.8347(4) 0.0630(9) Uani 1 1 d D U . . .
H3AA H 0.7508 0.0657 0.9088 0.076 Uiso 0.272(7) 1 calc R . P A 1
H3AB H 0.9004 0.0881 0.8140 0.076 Uiso 0.272(7) 1 calc R . P A 1
H3BC H 0.8940 0.0694 0.7823 0.076 Uiso 0.728(7) 1 calc R . P A 2
H3BD H 0.8021 0.0842 0.9010 0.076 Uiso 0.728(7) 1 calc R . P A 2
C4A C 0.7822(17) -0.0187(8) 0.7839(14) 0.0586(17) Uani 0.272(7) 1 d D U P A 1
H4AA H 0.8584 -0.0194 0.7138 0.070 Uiso 0.272(7) 1 calc R . P A 1
H4AB H 0.8310 -0.0733 0.8194 0.070 Uiso 0.272(7) 1 calc R . P A 1
C4 C 0.7191(9) -0.0153(4) 0.8357(6) 0.0650(12) Uani 0.728(7) 1 d D U P A 2
H4A H 0.8182 -0.0678 0.8209 0.078 Uiso 0.728(7) 1 calc R . P A 2
H4B H 0.6547 -0.0234 0.9072 0.078 Uiso 0.728(7) 1 calc R . P A 2
C5 C 0.6197(5) -0.0416(2) 0.7777(3) 0.0590(9) Uani 1 1 d D U . . .
H5AA H 0.5622 -0.0685 0.8435 0.071 Uiso 0.272(7) 1 calc R . P A 1
H5AB H 0.6454 -0.0945 0.7259 0.071 Uiso 0.272(7) 1 calc R . P A 1
H5BC H 0.5559 -0.0918 0.8151 0.071 Uiso 0.728(7) 1 calc R . P A 2
H5BD H 0.6955 -0.0727 0.7132 0.071 Uiso 0.728(7) 1 calc R . P A 2
C6 C 0.7323(5) 0.1931(3) 0.7060(3) 0.0650(10) Uani 1 1 d D U . . .
H6AA H 0.6597 0.2541 0.6962 0.078 Uiso 0.728(7) 1 calc R . P A 1
H6AB H 0.8469 0.2079 0.6903 0.078 Uiso 0.728(7) 1 calc R . P A 1
H6BC H 0.7280 0.2650 0.7014 0.078 Uiso 0.272(7) 1 calc R . P A 2
H6BD H 0.8500 0.1617 0.6761 0.078 Uiso 0.272(7) 1 calc R . P A 2
C7 C 0.7330(7) 0.1189(4) 0.6325(4) 0.0611(12) Uani 0.728(7) 1 d D U P A 1
H7A H 0.8218 0.0627 0.6330 0.073 Uiso 0.728(7) 1 calc R . P A 1
H7B H 0.7633 0.1473 0.5642 0.073 Uiso 0.728(7) 1 calc R . P A 1
C7A C 0.637(2) 0.1643(10) 0.6483(10) 0.0710(18) Uani 0.272(7) 1 d D U P A 2
H7AA H 0.5394 0.2179 0.6597 0.085 Uiso 0.272(7) 1 calc R . P A 2
H7AB H 0.7045 0.1699 0.5770 0.085 Uiso 0.272(7) 1 calc R . P A 2
C8 C 0.5709(6) 0.0796(3) 0.6491(3) 0.0699(10) Uani 1 1 d D U . . .
H8AA H 0.4871 0.1330 0.6360 0.084 Uiso 0.728(7) 1 calc R . P A 1
H8AB H 0.5906 0.0265 0.5985 0.084 Uiso 0.728(7) 1 calc R . P A 1
H8BC H 0.6600 0.0283 0.6086 0.084 Uiso 0.272(7) 1 calc R . P A 2
H8BD H 0.4826 0.0925 0.6154 0.084 Uiso 0.272(7) 1 calc R . P A 2
C9 C 0.3466(6) 0.0027(3) 0.7481(3) 0.0642(11) Uani 1 1 d . . . . .
H9A H 0.2864 0.0492 0.7104 0.077 Uiso 1 1 calc R . . . .
H9B H 0.3811 -0.0612 0.7108 0.077 Uiso 1 1 calc R . . . .
C10 C 0.2326(5) -0.0102(3) 0.8514(4) 0.0650(11) Uani 1 1 d . . . . .
H10A H 0.2851 -0.0640 0.8860 0.078 Uiso 1 1 calc R . . . .
H10B H 0.1267 -0.0269 0.8467 0.078 Uiso 1 1 calc R . . . .
Ni2 Ni 0.29319(4) 0.53122(2) 0.72317(3) 0.03087(10) Uani 1 1 d . . . . .
S3 S 0.34242(9) 0.38032(5) 0.76807(5) 0.03626(16) Uani 1 1 d . . . . .
S4 S 0.50839(11) 0.55873(7) 0.76097(7) 0.0531(2) Uani 1 1 d D U . . .
N3 N 0.0834(3) 0.50827(16) 0.70120(17) 0.0321(5) Uani 1 1 d . . . . .
N4 N 0.2697(3) 0.66147(19) 0.6609(2) 0.0497(7) Uani 1 1 d D U . . .
C11 C 0.1905(4) 0.3337(2) 0.7217(2) 0.0452(7) Uani 1 1 d . . . . .
H11A H 0.2370 0.3189 0.6481 0.054 Uiso 1 1 calc R . . . .
H11B H 0.1618 0.2727 0.7568 0.054 Uiso 1 1 calc R . . . .
C12 C 0.0378(4) 0.4118(2) 0.7428(2) 0.0418(7) Uani 1 1 d . . . . .
H12A H -0.0421 0.3920 0.7114 0.050 Uiso 1 1 calc R . . . .
H12B H -0.0170 0.4189 0.8168 0.050 Uiso 1 1 calc R . . . .
C13 C 0.0954(4) 0.5117(2) 0.5911(2) 0.0460(7) Uani 1 1 d . . . . .
H13A H -0.0058 0.5538 0.5830 0.055 Uiso 1 1 calc R . . . .
H13B H 0.0982 0.4448 0.5666 0.055 Uiso 1 1 calc R . . . .
C14 C 0.2469(5) 0.5506(3) 0.5265(3) 0.0617(10) Uani 1 1 d . . . . .
H14A H 0.2455 0.5505 0.4553 0.074 Uiso 1 1 calc R . . . .
H14B H 0.3472 0.5044 0.5300 0.074 Uiso 1 1 calc R . . . .
C15 C 0.2647(5) 0.6524(3) 0.5537(3) 0.0635(11) Uani 1 1 d . . . . .
H15A H 0.3685 0.6697 0.5064 0.076 Uiso 1 1 calc R . . . .
H15B H 0.1698 0.7001 0.5448 0.076 Uiso 1 1 calc R . . . .
C16 C -0.0548(4) 0.5858(2) 0.7615(2) 0.0411(7) Uani 1 1 d . . . . .
H16A H -0.1628 0.5701 0.7597 0.049 Uiso 1 1 calc R . . . .
H16B H -0.0548 0.5833 0.8330 0.049 Uiso 1 1 calc R . . . .
C17 C -0.0425(4) 0.6887(2) 0.7250(3) 0.0457(7) Uani 1 1 d . . . . .
H17A H -0.0525 0.6923 0.6556 0.055 Uiso 1 1 calc R . . . .
H17B H -0.1389 0.7337 0.7689 0.055 Uiso 1 1 calc R . . . .
C18 C 0.1134(5) 0.7250(2) 0.7234(3) 0.0514(8) Uani 1 1 d . . . . .
H18A H 0.1176 0.7289 0.7937 0.062 Uiso 1 1 calc R . . . .
H18B H 0.1094 0.7921 0.6962 0.062 Uiso 1 1 calc R . . . .
C19 C 0.4271(8) 0.7055(5) 0.6396(6) 0.0525(17) Uani 0.647(11) 1 d D U P B 1
H19A H 0.5152 0.6717 0.5808 0.063 Uiso 0.647(11) 1 calc R . P B 1
H19B H 0.4051 0.7761 0.6249 0.063 Uiso 0.647(11) 1 calc R . P B 1
C20 C 0.4800(10) 0.6913(5) 0.7338(6) 0.0574(18) Uani 0.647(11) 1 d D U P B 1
H20A H 0.3939 0.7281 0.7915 0.069 Uiso 0.647(11) 1 calc R . P B 1
H20B H 0.5859 0.7163 0.7237 0.069 Uiso 0.647(11) 1 calc R . P B 1
C19A C 0.3843(13) 0.7231(8) 0.6967(12) 0.053(3) Uani 0.353(11) 1 d D U P B 2
H19C H 0.3941 0.7843 0.6579 0.063 Uiso 0.353(11) 1 calc R . P B 2
H19D H 0.3345 0.7409 0.7695 0.063 Uiso 0.353(11) 1 calc R . P B 2
C20A C 0.5534(13) 0.6608(9) 0.6785(12) 0.060(3) Uani 0.353(11) 1 d D U P B 2
H20C H 0.6312 0.6969 0.6971 0.072 Uiso 0.353(11) 1 calc R . P B 2
H20D H 0.6019 0.6386 0.6067 0.072 Uiso 0.353(11) 1 calc R . P B 2
Fe1 Fe 0.25603(5) 0.36404(3) 0.94255(3) 0.03292(11) Uani 1 1 d . . . . .
O1 O 0.3148(3) 0.52308(16) 1.04274(18) 0.0487(5) Uani 1 1 d . . . . .
O2 O -0.0788(3) 0.3358(2) 1.0245(2) 0.0643(7) Uani 1 1 d . . . . .
N5 N 0.3070(3) 0.45837(17) 0.99364(18) 0.0368(5) Uani 1 1 d . . . . .
N6 N 0.0584(3) 0.34414(19) 0.98358(19) 0.0399(6) Uani 1 1 d . . . . .
B1 B 0.827(3) 0.8200(14) 0.4853(13) 0.064(5) Uani 0.172(14) 1 d D U P C 1
F1 F 0.942(2) 0.7361(13) 0.4558(14) 0.056(5) Uani 0.172(14) 1 d D U P C 1
F2 F 0.6700(18) 0.8011(16) 0.4964(17) 0.079(5) Uani 0.172(14) 1 d D U P C 1
F3 F 0.863(3) 0.8909(15) 0.4144(17) 0.073(6) Uani 0.172(14) 1 d D U P C 1
F4 F 0.833(4) 0.8537(17) 0.5755(14) 0.088(6) Uani 0.172(14) 1 d D U P C 1
B1A B 0.8341(7) 0.8206(4) 0.4921(4) 0.0458(12) Uani 0.828(14) 1 d D U P C 2
F1A F 0.8957(10) 0.7218(3) 0.4836(5) 0.095(2) Uani 0.828(14) 1 d D U P C 2
F2A F 0.6674(5) 0.8377(5) 0.5387(5) 0.1056(17) Uani 0.828(14) 1 d D U P C 2
F3A F 0.8637(7) 0.8578(5) 0.3959(3) 0.0728(13) Uani 0.828(14) 1 d D U P C 2
F4A F 0.9144(7) 0.8640(3) 0.5467(4) 0.0706(12) Uani 0.828(14) 1 d D U P C 2


_geom_special_details            
;
 All esds (except the esd in the dihedral angle between two l.s. planes)
 are estimated using the full covariance matrix.  The cell esds are taken
 into account individually in the estimation of esds in distances, angles
 and torsion angles; correlations between esds in cell parameters are only
 used when they are defined by crystal symmetry.  An approximate (isotropic)
 treatment of cell esds is used for estimating esds involving l.s. planes.
;
loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
_geom_bond_publ_flag
Ni1 S1 2.1696(8) . ?
Ni1 S2 2.1659(9) . ?
Ni1 N1 1.996(3) . ?
Ni1 N2 1.966(3) . ?
S1 C1 1.811(3) . ?
S1 Fe1 2.3105(8) . ?
S2 C10 1.808(4) . ?
N1 C2 1.508(4) . ?
N1 C3 1.505(4) . ?
N1 C6 1.492(4) . ?
N2 C5 1.509(4) . ?
N2 C8 1.506(5) . ?
N2 C9 1.494(5) . ?
C1 H1A 0.9900 . ?
C1 H1B 0.9900 . ?
C1 C2 1.484(5) . ?
C2 H2A 0.9900 . ?
C2 H2B 0.9900 . ?
C3 H3AA 0.9900 . ?
C3 H3AB 0.9900 . ?
C3 H3BC 0.9900 . ?
C3 H3BD 0.9900 . ?
C3 C4A 1.508(11) . ?
C3 C4 1.456(6) . ?
C4A H4AA 0.9900 . ?
C4A H4AB 0.9900 . ?
C4A C5 1.501(11) . ?
C4 H4A 0.9900 . ?
C4 H4B 0.9900 . ?
C4 C5 1.427(6) . ?
C5 H5AA 0.9900 . ?
C5 H5AB 0.9900 . ?
C5 H5BC 0.9900 . ?
C5 H5BD 0.9900 . ?
C6 H6AA 0.9900 . ?
C6 H6AB 0.9900 . ?
C6 H6BC 0.9900 . ?
C6 H6BD 0.9900 . ?
C6 C7 1.466(6) . ?
C6 C7A 1.411(11) . ?
C7 H7A 0.9900 . ?
C7 H7B 0.9900 . ?
C7 C8 1.520(7) . ?
C7A H7AA 0.9900 . ?
C7A H7AB 0.9900 . ?
C7A C8 1.379(11) . ?
C8 H8AA 0.9900 . ?
C8 H8AB 0.9900 . ?
C8 H8BC 0.9900 . ?
C8 H8BD 0.9900 . ?
C9 H9A 0.9900 . ?
C9 H9B 0.9900 . ?
C9 C10 1.491(6) . ?
C10 H10A 0.9900 . ?
C10 H10B 0.9900 . ?
Ni2 S3 2.1674(8) . ?
Ni2 S4 2.1503(8) . ?
Ni2 N3 1.982(2) . ?
Ni2 N4 1.978(3) . ?
S3 C11 1.823(3) . ?
S3 Fe1 2.3195(8) . ?
S4 C20 1.851(6) . ?
S4 C20A 1.806(10) . ?
N3 C12 1.501(4) . ?
N3 C13 1.498(4) . ?
N3 C16 1.506(4) . ?
N4 C15 1.510(5) . ?
N4 C18 1.500(5) . ?
N4 C19 1.512(6) . ?
N4 C19A 1.590(10) . ?
C11 H11A 0.9900 . ?
C11 H11B 0.9900 . ?
C11 C12 1.504(5) . ?
C12 H12A 0.9900 . ?
C12 H12B 0.9900 . ?
C13 H13A 0.9900 . ?
C13 H13B 0.9900 . ?
C13 C14 1.504(5) . ?
C14 H14A 0.9900 . ?
C14 H14B 0.9900 . ?
C14 C15 1.513(6) . ?
C15 H15A 0.9900 . ?
C15 H15B 0.9900 . ?
C16 H16A 0.9900 . ?
C16 H16B 0.9900 . ?
C16 C17 1.504(4) . ?
C17 H17A 0.9900 . ?
C17 H17B 0.9900 . ?
C17 C18 1.493(5) . ?
C18 H18A 0.9900 . ?
C18 H18B 0.9900 . ?
C19 H19A 0.9900 . ?
C19 H19B 0.9900 . ?
C19 C20 1.502(8) . ?
C20 H20A 0.9900 . ?
C20 H20B 0.9900 . ?
C19A H19C 0.9900 . ?
C19A H19D 0.9900 . ?
C19A C20A 1.504(14) . ?
C20A H20C 0.9900 . ?
C20A H20D 0.9900 . ?
Fe1 N5 1.682(2) . ?
Fe1 N6 1.676(3) . ?
O1 N5 1.164(3) . ?
O2 N6 1.159(3) . ?
B1 F1 1.370(13) . ?
B1 F2 1.370(13) . ?
B1 F3 1.371(13) . ?
B1 F4 1.366(13) . ?
B1A F1A 1.374(5) . ?
B1A F2A 1.354(6) . ?
B1A F3A 1.379(5) . ?
B1A F4A 1.372(5) . ?

loop_
_geom_angle_atom_site_label_1
_geom_angle_atom_site_label_2
_geom_angle_atom_site_label_3
_geom_angle
_geom_angle_site_symmetry_1
_geom_angle_site_symmetry_3
_geom_angle_publ_flag
S2 Ni1 S1 88.42(3) . . ?
N1 Ni1 S1 90.42(9) . . ?
N1 Ni1 S2 177.77(8) . . ?
N2 Ni1 S1 170.76(8) . . ?
N2 Ni1 S2 90.72(9) . . ?
N2 Ni1 N1 90.11(12) . . ?
Ni1 S1 Fe1 95.31(3) . . ?
C1 S1 Ni1 98.94(12) . . ?
C1 S1 Fe1 106.05(10) . . ?
C10 S2 Ni1 96.89(14) . . ?
C2 N1 Ni1 110.6(2) . . ?
C3 N1 Ni1 105.4(2) . . ?
C3 N1 C2 109.5(3) . . ?
C6 N1 Ni1 114.6(2) . . ?
C6 N1 C2 106.2(3) . . ?
C6 N1 C3 110.6(3) . . ?
C5 N2 Ni1 105.1(2) . . ?
C8 N2 Ni1 114.0(2) . . ?
C8 N2 C5 111.1(3) . . ?
C9 N2 Ni1 111.4(2) . . ?
C9 N2 C5 110.0(3) . . ?
C9 N2 C8 105.2(3) . . ?
S1 C1 H1A 109.8 . . ?
S1 C1 H1B 109.8 . . ?
H1A C1 H1B 108.3 . . ?
C2 C1 S1 109.3(2) . . ?
C2 C1 H1A 109.8 . . ?
C2 C1 H1B 109.8 . . ?
N1 C2 H2A 109.1 . . ?
N1 C2 H2B 109.1 . . ?
C1 C2 N1 112.5(3) . . ?
C1 C2 H2A 109.1 . . ?
C1 C2 H2B 109.1 . . ?
H2A C2 H2B 107.8 . . ?
N1 C3 H3AA 107.9 . . ?
N1 C3 H3AB 107.9 . . ?
N1 C3 H3BC 108.4 . . ?
N1 C3 H3BD 108.4 . . ?
N1 C3 C4A 117.7(6) . . ?
H3AA C3 H3AB 107.2 . . ?
H3BC C3 H3BD 107.4 . . ?
C4A C3 H3AA 107.9 . . ?
C4A C3 H3AB 107.9 . . ?
C4 C3 N1 115.6(3) . . ?
C4 C3 H3BC 108.4 . . ?
C4 C3 H3BD 108.4 . . ?
C3 C4A H4AA 107.5 . . ?
C3 C4A H4AB 107.5 . . ?
H4AA C4A H4AB 107.0 . . ?
C5 C4A C3 119.3(9) . . ?
C5 C4A H4AA 107.5 . . ?
C5 C4A H4AB 107.5 . . ?
C3 C4 H4A 105.2 . . ?
C3 C4 H4B 105.2 . . ?
H4A C4 H4B 105.9 . . ?
C5 C4 C3 128.5(4) . . ?
C5 C4 H4A 105.2 . . ?
C5 C4 H4B 105.2 . . ?
N2 C5 H5AA 107.8 . . ?
N2 C5 H5AB 107.8 . . ?
N2 C5 H5BC 108.2 . . ?
N2 C5 H5BD 108.2 . . ?
C4A C5 N2 118.2(6) . . ?
C4A C5 H5AA 107.8 . . ?
C4A C5 H5AB 107.8 . . ?
C4 C5 N2 116.5(3) . . ?
C4 C5 H5BC 108.2 . . ?
C4 C5 H5BD 108.2 . . ?
H5AA C5 H5AB 107.1 . . ?
H5BC C5 H5BD 107.3 . . ?
N1 C6 H6AA 108.2 . . ?
N1 C6 H6AB 108.2 . . ?
N1 C6 H6BC 108.8 . . ?
N1 C6 H6BD 108.8 . . ?
H6AA C6 H6AB 107.4 . . ?
H6BC C6 H6BD 107.7 . . ?
C7 C6 N1 116.3(3) . . ?
C7 C6 H6AA 108.2 . . ?
C7 C6 H6AB 108.2 . . ?
C7A C6 N1 113.8(6) . . ?
C7A C6 H6BC 108.8 . . ?
C7A C6 H6BD 108.8 . . ?
C6 C7 H7A 108.2 . . ?
C6 C7 H7B 108.2 . . ?
C6 C7 C8 116.4(4) . . ?
H7A C7 H7B 107.3 . . ?
C8 C7 H7A 108.2 . . ?
C8 C7 H7B 108.2 . . ?
C6 C7A H7AA 104.5 . . ?
C6 C7A H7AB 104.5 . . ?
H7AA C7A H7AB 105.7 . . ?
C8 C7A C6 131.0(11) . . ?
C8 C7A H7AA 104.5 . . ?
C8 C7A H7AB 104.5 . . ?
N2 C8 C7 115.6(4) . . ?
N2 C8 H8AA 108.4 . . ?
N2 C8 H8AB 108.4 . . ?
N2 C8 H8BC 108.6 . . ?
N2 C8 H8BD 108.6 . . ?
C7 C8 H8AA 108.4 . . ?
C7 C8 H8AB 108.4 . . ?
C7A C8 N2 114.9(6) . . ?
C7A C8 H8BC 108.6 . . ?
C7A C8 H8BD 108.6 . . ?
H8AA C8 H8AB 107.4 . . ?
H8BC C8 H8BD 107.5 . . ?
N2 C9 H9A 109.3 . . ?
N2 C9 H9B 109.3 . . ?
H9A C9 H9B 108.0 . . ?
C10 C9 N2 111.5(3) . . ?
C10 C9 H9A 109.3 . . ?
C10 C9 H9B 109.3 . . ?
S2 C10 H10A 110.2 . . ?
S2 C10 H10B 110.2 . . ?
C9 C10 S2 107.6(3) . . ?
C9 C10 H10A 110.2 . . ?
C9 C10 H10B 110.2 . . ?
H10A C10 H10B 108.5 . . ?
S4 Ni2 S3 89.14(3) . . ?
N3 Ni2 S3 90.45(7) . . ?
N3 Ni2 S4 174.90(7) . . ?
N4 Ni2 S3 171.12(10) . . ?
N4 Ni2 S4 91.09(8) . . ?
N4 Ni2 N3 90.10(10) . . ?
Ni2 S3 Fe1 112.38(3) . . ?
C11 S3 Ni2 97.50(10) . . ?
C11 S3 Fe1 106.14(11) . . ?
C20 S4 Ni2 95.58(19) . . ?
C20A S4 Ni2 98.0(4) . . ?
C12 N3 Ni2 111.65(17) . . ?
C12 N3 C16 105.8(2) . . ?
C13 N3 Ni2 111.36(19) . . ?
C13 N3 C12 109.4(2) . . ?
C13 N3 C16 111.2(2) . . ?
C16 N3 Ni2 107.33(17) . . ?
C15 N4 Ni2 111.2(2) . . ?
C15 N4 C19 99.0(4) . . ?
C15 N4 C19A 125.7(6) . . ?
C18 N4 Ni2 109.5(2) . . ?
C18 N4 C15 109.9(3) . . ?
C18 N4 C19 115.3(4) . . ?
C18 N4 C19A 91.9(5) . . ?
C19 N4 Ni2 111.7(3) . . ?
C19A N4 Ni2 106.6(4) . . ?
S3 C11 H11A 110.2 . . ?
S3 C11 H11B 110.2 . . ?
H11A C11 H11B 108.5 . . ?
C12 C11 S3 107.4(2) . . ?
C12 C11 H11A 110.2 . . ?
C12 C11 H11B 110.2 . . ?
N3 C12 C11 110.7(3) . . ?
N3 C12 H12A 109.5 . . ?
N3 C12 H12B 109.5 . . ?
C11 C12 H12A 109.5 . . ?
C11 C12 H12B 109.5 . . ?
H12A C12 H12B 108.1 . . ?
N3 C13 H13A 108.9 . . ?
N3 C13 H13B 108.9 . . ?
N3 C13 C14 113.2(3) . . ?
H13A C13 H13B 107.7 . . ?
C14 C13 H13A 108.9 . . ?
C14 C13 H13B 108.9 . . ?
C13 C14 H14A 108.2 . . ?
C13 C14 H14B 108.2 . . ?
C13 C14 C15 116.4(3) . . ?
H14A C14 H14B 107.3 . . ?
C15 C14 H14A 108.2 . . ?
C15 C14 H14B 108.2 . . ?
N4 C15 C14 113.1(3) . . ?
N4 C15 H15A 109.0 . . ?
N4 C15 H15B 109.0 . . ?
C14 C15 H15A 109.0 . . ?
C14 C15 H15B 109.0 . . ?
H15A C15 H15B 107.8 . . ?
N3 C16 H16A 108.6 . . ?
N3 C16 H16B 108.6 . . ?
H16A C16 H16B 107.6 . . ?
C17 C16 N3 114.6(2) . . ?
C17 C16 H16A 108.6 . . ?
C17 C16 H16B 108.6 . . ?
C16 C17 H17A 108.3 . . ?
C16 C17 H17B 108.3 . . ?
H17A C17 H17B 107.4 . . ?
C18 C17 C16 115.9(3) . . ?
C18 C17 H17A 108.3 . . ?
C18 C17 H17B 108.3 . . ?
N4 C18 H18A 108.8 . . ?
N4 C18 H18B 108.8 . . ?
C17 C18 N4 113.7(3) . . ?
C17 C18 H18A 108.8 . . ?
C17 C18 H18B 108.8 . . ?
H18A C18 H18B 107.7 . . ?
N4 C19 H19A 110.6 . . ?
N4 C19 H19B 110.6 . . ?
H19A C19 H19B 108.7 . . ?
C20 C19 N4 105.9(5) . . ?
C20 C19 H19A 110.6 . . ?
C20 C19 H19B 110.6 . . ?
S4 C20 H20A 110.0 . . ?
S4 C20 H20B 110.0 . . ?
C19 C20 S4 108.5(5) . . ?
C19 C20 H20A 110.0 . . ?
C19 C20 H20B 110.0 . . ?
H20A C20 H20B 108.4 . . ?
N4 C19A H19C 110.1 . . ?
N4 C19A H19D 110.1 . . ?
H19C C19A H19D 108.4 . . ?
C20A C19A N4 108.0(9) . . ?
C20A C19A H19C 110.1 . . ?
C20A C19A H19D 110.1 . . ?
S4 C20A H20C 111.2 . . ?
S4 C20A H20D 111.2 . . ?
C19A C20A S4 102.7(8) . . ?
C19A C20A H20C 111.2 . . ?
C19A C20A H20D 111.2 . . ?
H20C C20A H20D 109.1 . . ?
S1 Fe1 S3 114.30(3) . . ?
N5 Fe1 S1 104.30(8) . . ?
N5 Fe1 S3 107.51(9) . . ?
N6 Fe1 S1 101.11(9) . . ?
N6 Fe1 S3 110.92(9) . . ?
N6 Fe1 N5 118.67(12) . . ?
O1 N5 Fe1 167.5(2) . . ?
O2 N6 Fe1 170.6(2) . . ?
F1 B1 F2 110.0(12) . . ?
F1 B1 F3 109.9(12) . . ?
F2 B1 F3 109.6(12) . . ?
F4 B1 F1 109.4(12) . . ?
F4 B1 F2 109.4(12) . . ?
F4 B1 F3 108.6(12) . . ?
F1A B1A F3A 108.2(4) . . ?
F2A B1A F1A 111.2(5) . . ?
F2A B1A F3A 108.3(4) . . ?
F2A B1A F4A 110.0(4) . . ?
F4A B1A F1A 108.3(4) . . ?
F4A B1A F3A 110.8(4) . . ?

loop_
_geom_torsion_atom_site_label_1
_geom_torsion_atom_site_label_2
_geom_torsion_atom_site_label_3
_geom_torsion_atom_site_label_4
_geom_torsion
_geom_torsion_site_symmetry_1
_geom_torsion_site_symmetry_2
_geom_torsion_site_symmetry_3
_geom_torsion_site_symmetry_4
_geom_torsion_publ_flag
Ni1 S1 C1 C2 31.0(2) . . . . ?
Ni1 S2 C10 C9 -39.0(3) . . . . ?
Ni1 N1 C2 C1 40.7(3) . . . . ?
Ni1 N1 C3 C4A 59.9(9) . . . . ?
Ni1 N1 C3 C4 27.0(5) . . . . ?
Ni1 N1 C6 C7 -59.7(4) . . . . ?
Ni1 N1 C6 C7A -18.5(8) . . . . ?
Ni1 N2 C5 C4A -61.1(9) . . . . ?
Ni1 N2 C5 C4 -27.7(5) . . . . ?
Ni1 N2 C8 C7 60.3(4) . . . . ?
Ni1 N2 C8 C7A 19.7(9) . . . . ?
Ni1 N2 C9 C10 -38.5(3) . . . . ?
S1 C1 C2 N1 -48.0(3) . . . . ?
S1 Fe1 N5 O1 -95.0(10) . . . . ?
N1 C3 C4A C5 -40.9(16) . . . . ?
N1 C3 C4 C5 33.0(9) . . . . ?
N1 C6 C7 C8 53.0(5) . . . . ?
N1 C6 C7A C8 -41.0(18) . . . . ?
N2 C9 C10 S2 52.4(4) . . . . ?
C2 N1 C3 C4A 178.8(8) . . . . ?
C2 N1 C3 C4 146.0(5) . . . . ?
C2 N1 C6 C7 177.9(4) . . . . ?
C2 N1 C6 C7A -141.0(8) . . . . ?
C3 N1 C2 C1 -74.9(3) . . . . ?
C3 N1 C6 C7 59.2(5) . . . . ?
C3 N1 C6 C7A 100.4(8) . . . . ?
C3 C4A C5 N2 41.3(16) . . . . ?
C3 C4 C5 N2 -33.0(9) . . . . ?
C5 N2 C8 C7 -58.3(4) . . . . ?
C5 N2 C8 C7A -98.9(8) . . . . ?
C5 N2 C9 C10 77.7(4) . . . . ?
C6 N1 C2 C1 165.7(3) . . . . ?
C6 N1 C3 C4A -64.5(9) . . . . ?
C6 N1 C3 C4 -97.4(5) . . . . ?
C6 C7 C8 N2 -53.4(5) . . . . ?
C6 C7A C8 N2 40.6(18) . . . . ?
C8 N2 C5 C4A 62.7(9) . . . . ?
C8 N2 C5 C4 96.1(5) . . . . ?
C8 N2 C9 C10 -162.5(3) . . . . ?
C9 N2 C5 C4A 178.8(8) . . . . ?
C9 N2 C5 C4 -147.8(5) . . . . ?
C9 N2 C8 C7 -177.4(3) . . . . ?
C9 N2 C8 C7A 142.1(8) . . . . ?
Ni2 S3 C11 C12 -38.4(2) . . . . ?
Ni2 S4 C20 C19 -40.5(6) . . . . ?
Ni2 S4 C20A C19A 45.6(11) . . . . ?
Ni2 N3 C12 C11 -40.1(3) . . . . ?
Ni2 N3 C13 C14 -11.2(3) . . . . ?
Ni2 N3 C16 C17 66.5(3) . . . . ?
Ni2 N4 C15 C14 10.5(4) . . . . ?
Ni2 N4 C18 C17 -65.0(3) . . . . ?
Ni2 N4 C19 C20 -46.1(7) . . . . ?
Ni2 N4 C19A C20A 49.2(11) . . . . ?
S3 C11 C12 N3 52.6(3) . . . . ?
S3 Fe1 N5 O1 143.3(10) . . . . ?
N3 C13 C14 C15 -58.0(4) . . . . ?
N3 C16 C17 C18 -58.6(4) . . . . ?
N4 C19 C20 S4 57.2(8) . . . . ?
N4 C19A C20A S4 -63.1(13) . . . . ?
C12 N3 C13 C14 -135.1(3) . . . . ?
C12 N3 C16 C17 -174.2(3) . . . . ?
C13 N3 C12 C11 83.6(3) . . . . ?
C13 N3 C16 C17 -55.5(3) . . . . ?
C13 C14 C15 N4 58.5(4) . . . . ?
C15 N4 C18 C17 57.3(4) . . . . ?
C15 N4 C19 C20 -163.2(6) . . . . ?
C15 N4 C19A C20A -83.5(11) . . . . ?
C16 N3 C12 C11 -156.6(2) . . . . ?
C16 N3 C13 C14 108.4(3) . . . . ?
C16 C17 C18 N4 56.8(4) . . . . ?
C18 N4 C15 C14 -110.8(3) . . . . ?
C18 N4 C19 C20 79.7(6) . . . . ?
C18 N4 C19A C20A 160.2(10) . . . . ?
C19 N4 C15 C14 128.0(4) . . . . ?
C19 N4 C18 C17 168.1(4) . . . . ?
C19A N4 C15 C14 141.5(6) . . . . ?
C19A N4 C18 C17 -173.4(5) . . . . ?
Fe1 S1 C1 C2 -67.2(2) . . . . ?
Fe1 S3 C11 C12 77.6(2) . . . . ?
N6 Fe1 N5 O1 16.5(11) . . . . ?

_olex2_submission_special_instructions 'No special instructions were received'
####################################################################### 
# 
# 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_feni
_audit_block_doi                 10.5517/ccdc.csd.cc142wkn
_database_code_depnum_ccdc_archive 'CCDC 1045461'
_audit_update_record             
;
2015-01-24 deposited with the CCDC.
2017-10-12 downloaded from the CCDC.
;

_audit_creation_method           SHELXL-2013
_chemical_name_systematic        
;
 ?
;
_chemical_name_common            ?
_chemical_melting_point          ?
_chemical_formula_moiety         ?
_chemical_formula_sum            'C10.50 H21 Cl Fe N4 Ni O2 S2'
_chemical_formula_weight         449.44

loop_
_atom_type_symbol
_atom_type_description
_atom_type_scat_dispersion_real
_atom_type_scat_dispersion_imag
_atom_type_scat_source
C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
S S 0.1246 0.1234 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Cl Cl 0.1484 0.1585 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Fe Fe 0.3463 0.8444 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Ni Ni 0.3393 1.1124 '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 2/c'
_space_group_name_Hall           '-C 2yc'

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

No pseudo-merohedral twinning detected by TwinRotMat
;

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

_cell_length_a                   12.318(8)
_cell_length_b                   11.116(7)
_cell_length_c                   24.241(15)
_cell_angle_alpha                90
_cell_angle_beta                 90.062(7)
_cell_angle_gamma                90
_cell_volume                     3319(4)
_cell_formula_units_Z            8
_cell_measurement_temperature    110(2)
_cell_measurement_reflns_used    5268
_cell_measurement_theta_min      2.47
_cell_measurement_theta_max      29.13

_exptl_crystal_description       'plate     '
_exptl_crystal_colour            'dark brown       '
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    ?
_exptl_crystal_density_diffrn    1.799
_exptl_crystal_F_000             1848
_exptl_transmission_factor_min   ?
_exptl_transmission_factor_max   ?
_exptl_crystal_size_max          0.400
_exptl_crystal_size_mid          0.200
_exptl_crystal_size_min          0.050
_exptl_absorpt_coefficient_mu    2.429
_shelx_estimated_absorpt_T_min   0.443
_shelx_estimated_absorpt_T_max   0.888
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_correction_T_min  0.6617
_exptl_absorpt_correction_T_max  0.7459
_exptl_absorpt_process_details   
;
SADABS-2009/1 (Bruker,2009) was employed for absorption correction.
wR2(int) was   0.0718 before and   0.0550 after correction.
The ratio of minimum to maximum transmission factors was   0.8871.
Additional spherical absorption correction applied with mu*r =  0.2000.
The λ/2 correction factor of 0.0015 was applied.
;

_exptl_special_details           
;
 ?
;

_diffrn_ambient_temperature      110(2)
_diffrn_radiation_wavelength     0.71073
_diffrn_radiation_type           MoK\a
_diffrn_source                   ?
_diffrn_measurement_method       'phi and omega scans'
_diffrn_detector_area_resol_mean ?
_diffrn_reflns_number            20288
_diffrn_reflns_av_unetI/netI     0.0422
_diffrn_reflns_av_R_equivalents  0.0487
_diffrn_reflns_limit_h_min       -16
_diffrn_reflns_limit_h_max       16
_diffrn_reflns_limit_k_min       -15
_diffrn_reflns_limit_k_max       15
_diffrn_reflns_limit_l_min       -33
_diffrn_reflns_limit_l_max       33
_diffrn_reflns_theta_min         2.468
_diffrn_reflns_theta_max         29.638
_diffrn_reflns_theta_full        25.242
_diffrn_measured_fraction_theta_max 0.932
_diffrn_measured_fraction_theta_full 0.999
_diffrn_reflns_Laue_measured_fraction_max 0.932
_diffrn_reflns_Laue_measured_fraction_full 0.999
_diffrn_reflns_point_group_measured_fraction_max 0.932
_diffrn_reflns_point_group_measured_fraction_full 0.999
_reflns_number_total             4376
_reflns_number_gt                3564
_reflns_threshold_expression     'I > 2σ(I)'
_reflns_Friedel_coverage         0.000
_reflns_Friedel_fraction_max     .
_reflns_Friedel_fraction_full    .

_reflns_special_details          
;
 Reflections were merged by SHELXL according to the crystal
 class for the calculation of statistics and refinement.

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

_computing_data_collection       'APEXII (Bruker, 2012a)'
_computing_cell_refinement       'APEXII (Bruker, 2012a)'
_computing_data_reduction        'SAINT (Bruker, 2012b)'
_computing_structure_solution    'SHELXS (Sheldrick 2008)'
_computing_structure_refinement  'SHELXL-2013 (Sheldrick, 2013)'
_computing_molecular_graphics    'shelXLe (Hübschle 2011)'
_computing_publication_material  'Ciftab (Sheldrick, 2008)'

_refine_special_details          
;
 ?
;
_refine_ls_structure_factor_coef Fsqd
_refine_ls_matrix_type           full
_refine_ls_weighting_scheme      calc
_refine_ls_weighting_details     
'w=1/[σ²(Fo²)+(0.0296P)²] where P=(Fo²+2Fc²)/3'
_atom_sites_solution_primary     ?
_atom_sites_solution_secondary   ?
_atom_sites_solution_hydrogens   geom
_refine_ls_hydrogen_treatment    constr
_refine_ls_extinction_method     none
_refine_ls_extinction_coef       .
_refine_ls_number_reflns         4376
_refine_ls_number_parameters     195
_refine_ls_number_restraints     0
_refine_ls_R_factor_all          0.0437
_refine_ls_R_factor_gt           0.0314
_refine_ls_wR_factor_ref         0.0708
_refine_ls_wR_factor_gt          0.0671
_refine_ls_goodness_of_fit_ref   1.085
_refine_ls_restrained_S_all      1.085
_refine_ls_shift/su_max          0.001
_refine_ls_shift/su_mean         0.000

loop_
_atom_site_label
_atom_site_type_symbol
_atom_site_fract_x
_atom_site_fract_y
_atom_site_fract_z
_atom_site_U_iso_or_equiv
_atom_site_adp_type
_atom_site_occupancy
_atom_site_site_symmetry_order
_atom_site_calc_flag
_atom_site_refinement_flags_posn
_atom_site_refinement_flags_adp
_atom_site_refinement_flags_occupancy
_atom_site_disorder_assembly
_atom_site_disorder_group
Ni1 Ni 0.02484(2) 0.94311(2) 0.91384(2) 0.01066(7) Uani 1 1 d . . . . .
Fe1 Fe 0.26016(2) 0.91025(3) 0.88570(2) 0.01478(9) Uani 1 1 d . . . . .
Cl1 Cl 0.10525(6) 0.54041(7) 0.77700(3) 0.03998(18) Uani 1 1 d . . . . .
S1 S 0.14676(4) 1.07995(5) 0.89919(2) 0.01458(12) Uani 1 1 d . . . . .
S2 S 0.14947(4) 0.85277(5) 0.96110(2) 0.01542(12) Uani 1 1 d . . . . .
O1 O 0.48639(14) 0.92586(16) 0.90571(8) 0.0333(5) Uani 1 1 d . . . . .
O2 O 0.24822(14) 0.79086(16) 0.78192(7) 0.0278(4) Uani 1 1 d . . . . .
N1 N 0.38869(16) 0.92880(17) 0.90458(8) 0.0201(4) Uani 1 1 d . . . . .
N2 N 0.24538(14) 0.84120(17) 0.82579(8) 0.0181(4) Uani 1 1 d . . . . .
N3 N -0.07804(14) 1.02236(16) 0.86268(7) 0.0119(4) Uani 1 1 d . . . . .
N4 N -0.07596(14) 0.80750(15) 0.92402(7) 0.0118(4) Uani 1 1 d . . . . .
C1 C 0.08761(17) 1.1339(2) 0.83429(9) 0.0179(5) Uani 1 1 d . . . . .
H1A H 0.1174 1.2138 0.8245 0.021 Uiso 1 1 calc R U . . .
H1B H 0.1034 1.0771 0.8039 0.021 Uiso 1 1 calc R U . . .
C2 C -0.03339(17) 1.14188(19) 0.84442(9) 0.0170(5) Uani 1 1 d . . . . .
H2A H -0.0479 1.2031 0.8732 0.020 Uiso 1 1 calc R U . . .
H2B H -0.0704 1.1675 0.8101 0.020 Uiso 1 1 calc R U . . .
C3 C -0.09537(18) 0.94218(19) 0.81330(8) 0.0153(4) Uani 1 1 d . . . . .
H3A H -0.0601 0.9795 0.7809 0.018 Uiso 1 1 calc R U . . .
H3B H -0.1742 0.9373 0.8056 0.018 Uiso 1 1 calc R U . . .
C4 C -0.05148(17) 0.8159(2) 0.82027(9) 0.0160(5) Uani 1 1 d . . . . .
H4A H 0.0286 0.8211 0.8228 0.019 Uiso 1 1 calc R U . . .
H4B H -0.0689 0.7700 0.7864 0.019 Uiso 1 1 calc R U . . .
C5 C -0.09166(17) 0.74382(19) 0.86945(8) 0.0149(4) Uani 1 1 d . . . . .
H5A H -0.1698 0.7264 0.8644 0.018 Uiso 1 1 calc R U . . .
H5B H -0.0526 0.6660 0.8706 0.018 Uiso 1 1 calc R U . . .
C6 C -0.18421(17) 1.0469(2) 0.89081(9) 0.0155(4) Uani 1 1 d . . . . .
H6A H -0.2309 1.0945 0.8657 0.019 Uiso 1 1 calc R U . . .
H6B H -0.1705 1.0962 0.9241 0.019 Uiso 1 1 calc R U . . .
C7 C -0.24458(17) 0.9336(2) 0.90757(9) 0.0166(5) Uani 1 1 d . . . . .
H7A H -0.3135 0.9572 0.9256 0.020 Uiso 1 1 calc R U . . .
H7B H -0.2633 0.8878 0.8738 0.020 Uiso 1 1 calc R U . . .
C8 C -0.18251(17) 0.8519(2) 0.94615(9) 0.0153(4) Uani 1 1 d . . . . .
H8A H -0.1688 0.8957 0.9810 0.018 Uiso 1 1 calc R U . . .
H8B H -0.2286 0.7815 0.9550 0.018 Uiso 1 1 calc R U . . .
C9 C -0.03140(17) 0.7201(2) 0.96565(9) 0.0167(5) Uani 1 1 d . . . . .
H9A H -0.0692 0.6419 0.9620 0.020 Uiso 1 1 calc R U . . .
H9B H -0.0444 0.7510 1.0034 0.020 Uiso 1 1 calc R U . . .
C10 C 0.08910(17) 0.70267(19) 0.95678(9) 0.0174(5) Uani 1 1 d . . . . .
H10A H 0.1031 0.6665 0.9202 0.021 Uiso 1 1 calc R U . . .
H10B H 0.1198 0.6493 0.9855 0.021 Uiso 1 1 calc R U . . .
C11 C 0.0000 0.4511(3) 0.7500 0.0418(11) Uani 1 2 d S T P . .
H11A H -0.0293 0.3988 0.7795 0.050 Uiso 0.5 1 calc R U P . .
H11B H 0.0293 0.3988 0.7205 0.050 Uiso 0.5 1 calc R U P . .


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

loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
_geom_bond_publ_flag
Ni1 N4 1.9688(19) . ?
Ni1 N3 1.9791(19) . ?
Ni1 S2 2.1620(10) . ?
Ni1 S1 2.1671(11) . ?
Fe1 N2 1.652(2) . ?
Fe1 N1 1.660(2) . ?
Fe1 S2 2.3694(12) . ?
Fe1 S1 2.3702(12) . ?
Cl1 C11 1.759(2) . ?
S1 C1 1.834(2) . ?
S2 C10 1.830(2) . ?
O1 N1 1.204(3) . ?
O2 N2 1.202(2) . ?
N3 C6 1.501(3) . ?
N3 C2 1.505(3) . ?
N3 C3 1.507(3) . ?
N4 C8 1.502(3) . ?
N4 C9 1.504(3) . ?
N4 C5 1.513(3) . ?
C1 C2 1.513(3) . ?
C1 H1A 0.9900 . ?
C1 H1B 0.9900 . ?
C2 H2A 0.9900 . ?
C2 H2B 0.9900 . ?
C3 C4 1.514(3) . ?
C3 H3A 0.9900 . ?
C3 H3B 0.9900 . ?
C4 C5 1.519(3) . ?
C4 H4A 0.9900 . ?
C4 H4B 0.9900 . ?
C5 H5A 0.9900 . ?
C5 H5B 0.9900 . ?
C6 C7 1.518(3) . ?
C6 H6A 0.9900 . ?
C6 H6B 0.9900 . ?
C7 C8 1.511(3) . ?
C7 H7A 0.9900 . ?
C7 H7B 0.9900 . ?
C8 H8A 0.9900 . ?
C8 H8B 0.9900 . ?
C9 C10 1.513(3) . ?
C9 H9A 0.9900 . ?
C9 H9B 0.9900 . ?
C10 H10A 0.9900 . ?
C10 H10B 0.9900 . ?
C11 Cl1 1.759(2) 2_556 ?
C11 H11A 0.9900 . ?
C11 H11B 0.9900 . ?

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 Ni1 N3 90.91(8) . . ?
N4 Ni1 S2 91.46(7) . . ?
N3 Ni1 S2 173.07(5) . . ?
N4 Ni1 S1 174.43(5) . . ?
N3 Ni1 S1 91.63(7) . . ?
S2 Ni1 S1 85.47(5) . . ?
N2 Fe1 N1 113.84(9) . . ?
N2 Fe1 S2 119.33(8) . . ?
N1 Fe1 S2 111.72(8) . . ?
N2 Fe1 S1 115.25(7) . . ?
N1 Fe1 S1 115.15(7) . . ?
S2 Fe1 S1 76.61(4) . . ?
C1 S1 Ni1 95.47(8) . . ?
C1 S1 Fe1 112.06(8) . . ?
Ni1 S1 Fe1 82.68(5) . . ?
C10 S2 Ni1 96.02(8) . . ?
C10 S2 Fe1 115.84(8) . . ?
Ni1 S2 Fe1 82.81(5) . . ?
O1 N1 Fe1 162.84(19) . . ?
O2 N2 Fe1 172.00(17) . . ?
C6 N3 C2 106.98(16) . . ?
C6 N3 C3 110.22(16) . . ?
C2 N3 C3 109.88(16) . . ?
C6 N3 Ni1 110.73(13) . . ?
C2 N3 Ni1 110.07(13) . . ?
C3 N3 Ni1 108.94(13) . . ?
C8 N4 C9 106.93(16) . . ?
C8 N4 C5 110.81(16) . . ?
C9 N4 C5 109.31(16) . . ?
C8 N4 Ni1 110.16(13) . . ?
C9 N4 Ni1 110.42(13) . . ?
C5 N4 Ni1 109.19(12) . . ?
C2 C1 S1 105.69(15) . . ?
C2 C1 H1A 110.6 . . ?
S1 C1 H1A 110.6 . . ?
C2 C1 H1B 110.6 . . ?
S1 C1 H1B 110.6 . . ?
H1A C1 H1B 108.7 . . ?
N3 C2 C1 110.88(17) . . ?
N3 C2 H2A 109.5 . . ?
C1 C2 H2A 109.5 . . ?
N3 C2 H2B 109.5 . . ?
C1 C2 H2B 109.5 . . ?
H2A C2 H2B 108.1 . . ?
N3 C3 C4 114.17(17) . . ?
N3 C3 H3A 108.7 . . ?
C4 C3 H3A 108.7 . . ?
N3 C3 H3B 108.7 . . ?
C4 C3 H3B 108.7 . . ?
H3A C3 H3B 107.6 . . ?
C3 C4 C5 117.37(18) . . ?
C3 C4 H4A 108.0 . . ?
C5 C4 H4A 108.0 . . ?
C3 C4 H4B 108.0 . . ?
C5 C4 H4B 108.0 . . ?
H4A C4 H4B 107.2 . . ?
N4 C5 C4 113.46(17) . . ?
N4 C5 H5A 108.9 . . ?
C4 C5 H5A 108.9 . . ?
N4 C5 H5B 108.9 . . ?
C4 C5 H5B 108.9 . . ?
H5A C5 H5B 107.7 . . ?
N3 C6 C7 113.47(18) . . ?
N3 C6 H6A 108.9 . . ?
C7 C6 H6A 108.9 . . ?
N3 C6 H6B 108.9 . . ?
C7 C6 H6B 108.9 . . ?
H6A C6 H6B 107.7 . . ?
C8 C7 C6 114.62(19) . . ?
C8 C7 H7A 108.6 . . ?
C6 C7 H7A 108.6 . . ?
C8 C7 H7B 108.6 . . ?
C6 C7 H7B 108.6 . . ?
H7A C7 H7B 107.6 . . ?
N4 C8 C7 114.74(17) . . ?
N4 C8 H8A 108.6 . . ?
C7 C8 H8A 108.6 . . ?
N4 C8 H8B 108.6 . . ?
C7 C8 H8B 108.6 . . ?
H8A C8 H8B 107.6 . . ?
N4 C9 C10 110.17(17) . . ?
N4 C9 H9A 109.6 . . ?
C10 C9 H9A 109.6 . . ?
N4 C9 H9B 109.6 . . ?
C10 C9 H9B 109.6 . . ?
H9A C9 H9B 108.1 . . ?
C9 C10 S2 105.90(15) . . ?
C9 C10 H10A 110.6 . . ?
S2 C10 H10A 110.6 . . ?
C9 C10 H10B 110.6 . . ?
S2 C10 H10B 110.6 . . ?
H10A C10 H10B 108.7 . . ?
Cl1 C11 Cl1 111.3(2) . 2_556 ?
Cl1 C11 H11A 109.4 . . ?
Cl1 C11 H11A 109.4 2_556 . ?
Cl1 C11 H11B 109.4 . . ?
Cl1 C11 H11B 109.4 2_556 . ?
H11A C11 H11B 108.0 . . ?

loop_
_geom_torsion_atom_site_label_1
_geom_torsion_atom_site_label_2
_geom_torsion_atom_site_label_3
_geom_torsion_atom_site_label_4
_geom_torsion
_geom_torsion_site_symmetry_1
_geom_torsion_site_symmetry_2
_geom_torsion_site_symmetry_3
_geom_torsion_site_symmetry_4
_geom_torsion_publ_flag
N2 Fe1 N1 O1 -2.7(6) . . . . ?
S2 Fe1 N1 O1 136.1(6) . . . . ?
S1 Fe1 N1 O1 -139.0(6) . . . . ?
Ni1 S1 C1 C2 43.59(15) . . . . ?
Fe1 S1 C1 C2 127.90(13) . . . . ?
C6 N3 C2 C1 159.91(18) . . . . ?
C3 N3 C2 C1 -80.4(2) . . . . ?
Ni1 N3 C2 C1 39.5(2) . . . . ?
S1 C1 C2 N3 -56.8(2) . . . . ?
C6 N3 C3 C4 -109.6(2) . . . . ?
C2 N3 C3 C4 132.70(19) . . . . ?
Ni1 N3 C3 C4 12.0(2) . . . . ?
N3 C3 C4 C5 55.9(3) . . . . ?
C8 N4 C5 C4 107.0(2) . . . . ?
C9 N4 C5 C4 -135.38(18) . . . . ?
Ni1 N4 C5 C4 -14.5(2) . . . . ?
C3 C4 C5 N4 -54.4(3) . . . . ?
C2 N3 C6 C7 175.17(18) . . . . ?
C3 N3 C6 C7 55.7(2) . . . . ?
Ni1 N3 C6 C7 -64.9(2) . . . . ?
N3 C6 C7 C8 58.6(2) . . . . ?
C9 N4 C8 C7 -175.20(18) . . . . ?
C5 N4 C8 C7 -56.2(2) . . . . ?
Ni1 N4 C8 C7 64.8(2) . . . . ?
C6 C7 C8 N4 -59.0(2) . . . . ?
C8 N4 C9 C10 -161.30(18) . . . . ?
C5 N4 C9 C10 78.7(2) . . . . ?
Ni1 N4 C9 C10 -41.5(2) . . . . ?
N4 C9 C10 S2 56.6(2) . . . . ?
Ni1 S2 C10 C9 -42.13(15) . . . . ?
Fe1 S2 C10 C9 -127.04(13) . . . . ?

_refine_diff_density_max         0.809
_refine_diff_density_min         -0.733
_refine_diff_density_rms         0.095

_shelxl_version_number           2013-4

