Crystal structures of (aceto­nitrile-κN)tris­(pyridine-4-thio­amide-κN)bis­(thio­cyanate-κN)cobalt(II) aceto­nitrile disolvate and tetra­kis­(pyridine-4-thio­amide-κN)bis­(thio­cyanate-κN)nickel(II) methanol penta­solvate

The crystal structures of the title compounds consist of discrete octa­hedral complexes that are linked by inter­molecular hydrogen bonding between the complexes and additional solvate mol­ecules into three-dimensional network structures.

Key indicators

Structure: Compound1

• Single-crystal X-ray study
• T = 200 K
• Mean [sigma](C-C) = 0.003 Å
• Disorder in solvent or counterion
• R factor = 0.032
• wR factor = 0.080
• Data-to-parameter ratio = 17.2

Structure: Compound2

• Single-crystal X-ray study
• T = 200 K
• Mean [sigma](C-C) = 0.003 Å
• R factor = 0.039
• wR factor = 0.109
• Data-to-parameter ratio = 19.0

checkCIF/PLATON results

No syntax errors found



Datablock: Compound1



Alert level C
PLAT244_ALERT_4_C Low    'Solvent' Ueq as Compared to Neighbors of         C5 Check
PLAT480_ALERT_4_C Long H...A H-Bond Reported H6C      ..S31              3.02 Ang.
PLAT480_ALERT_4_C Long H...A H-Bond Reported H12      ..S1               3.01 Ang.
PLAT480_ALERT_4_C Long H...A H-Bond Reported H25      ..S2               2.91 Ang.
PLAT480_ALERT_4_C Long H...A H-Bond Reported H34      ..S11              2.98 Ang.
PLAT480_ALERT_4_C Long H...A H-Bond Reported H35      ..S21              2.95 Ang.
PLAT906_ALERT_3_C Large K Value in the Analysis of Variance ......      4.016 Check
PLAT911_ALERT_3_C Missing FCF Refl Between Thmin & STh/L=    0.600         43 Report

Alert level G
PLAT002_ALERT_2_G Number of Distance or Angle Restraints on AtSite          9 Note
PLAT007_ALERT_5_G Number of Unrefined Donor-H Atoms ..............          6 Report
PLAT175_ALERT_4_G The CIF-Embedded .res File Contains SAME Records          2 Report
PLAT230_ALERT_2_G Hirshfeld Test Diff for   S1       --C1        .        8.7 s.u.
PLAT230_ALERT_2_G Hirshfeld Test Diff for   S2       --C2        .        6.4 s.u.
PLAT232_ALERT_2_G Hirshfeld Test Diff (M-X) Co1      --N2        .        5.0 s.u.
PLAT300_ALERT_4_G Atom Site Occupancy of N5         Constrained at       0.62 Check
PLAT300_ALERT_4_G Atom Site Occupancy of C7         Constrained at       0.62 Check
PLAT300_ALERT_4_G Atom Site Occupancy of C8         Constrained at       0.62 Check
PLAT300_ALERT_4_G Atom Site Occupancy of H8A        Constrained at       0.62 Check
PLAT300_ALERT_4_G Atom Site Occupancy of H8B        Constrained at       0.62 Check
PLAT300_ALERT_4_G Atom Site Occupancy of H8C        Constrained at       0.62 Check
PLAT300_ALERT_4_G Atom Site Occupancy of N5'        Constrained at       0.38 Check
PLAT300_ALERT_4_G Atom Site Occupancy of C7'        Constrained at       0.38 Check
PLAT300_ALERT_4_G Atom Site Occupancy of C8'        Constrained at       0.38 Check
PLAT300_ALERT_4_G Atom Site Occupancy of H8D        Constrained at       0.38 Check
PLAT300_ALERT_4_G Atom Site Occupancy of H8E        Constrained at       0.38 Check
PLAT300_ALERT_4_G Atom Site Occupancy of H8F        Constrained at       0.38 Check
PLAT302_ALERT_4_G Anion/Solvent/Minor-Residue Disorder (Resd  3  )       100% Note
PLAT302_ALERT_4_G Anion/Solvent/Minor-Residue Disorder (Resd  4  )       100% Note
PLAT304_ALERT_4_G Non-Integer Number of Atoms in ...... Resd  3          3.72 Check
PLAT304_ALERT_4_G Non-Integer Number of Atoms in ...... Resd  4          2.28 Check
PLAT432_ALERT_2_G Short Inter X...Y Contact  C3       ..C7'              3.02 Ang.
PLAT790_ALERT_4_G Centre of Gravity not Within Unit Cell: Resd.  #          4 Note
              C2 H3 N
PLAT794_ALERT_5_G Tentative Bond Valency for Co1       (II)      .       1.59 Info
PLAT860_ALERT_3_G Number of Least-Squares Restraints .............          9 Note
PLAT913_ALERT_3_G Missing # of Very Strong Reflections in FCF ....          3 Note
PLAT978_ALERT_2_G Number C-C Bonds with Positive Residual Density.          9 Info

   0 ALERT level A = Most likely a serious problem - resolve or explain
   0 ALERT level B = A potentially serious problem, consider carefully
   8 ALERT level C = Check. Ensure it is not caused by an omission or oversight
  28 ALERT level G = General information/check it is not something unexpected

   0 ALERT type 1 CIF construction/syntax error, inconsistent or missing data
   6 ALERT type 2 Indicator that the structure model may be wrong or deficient
   4 ALERT type 3 Indicator that the structure quality may be low
  24 ALERT type 4 Improvement, methodology, query or suggestion
   2 ALERT type 5 Informative message, check




Datablock: Compound2



Alert level B
PLAT420_ALERT_2_B D-H Without Acceptor       O1       --H1             Please Check

Alert level C
PLAT417_ALERT_2_C Short Inter D-H..H-D       H4       ..H5               2.11 Ang.
PLAT417_ALERT_2_C Short Inter D-H..H-D       H5       ..H5N              2.10 Ang.
PLAT420_ALERT_2_C D-H Without Acceptor       N42      --H8N            Please Check
PLAT480_ALERT_4_C Long H...A H-Bond Reported H1       ..S11              2.92 Ang.
PLAT480_ALERT_4_C Long H...A H-Bond Reported H3       ..S31              2.93 Ang.
PLAT480_ALERT_4_C Long H...A H-Bond Reported H5A      ..S31              3.03 Ang.
PLAT480_ALERT_4_C Long H...A H-Bond Reported H7A      ..S41              2.93 Ang.
PLAT480_ALERT_4_C Long H...A H-Bond Reported H12      ..S1               2.96 Ang.
PLAT480_ALERT_4_C Long H...A H-Bond Reported H21      ..N1               2.65 Ang.
PLAT480_ALERT_4_C Long H...A H-Bond Reported H25      ..N2               2.66 Ang.
PLAT480_ALERT_4_C Long H...A H-Bond Reported H25      ..S2               2.94 Ang.
PLAT480_ALERT_4_C Long H...A H-Bond Reported H45      ..S11              2.89 Ang.
PLAT906_ALERT_3_C Large K Value in the Analysis of Variance ......      3.278 Check
PLAT911_ALERT_3_C Missing FCF Refl Between Thmin & STh/L=    0.600          8 Report
PLAT913_ALERT_3_C Missing # of Very Strong Reflections in FCF ....          5 Note
PLAT976_ALERT_2_C Check Calcd Resid. Dens.  0.65A   From O4             -0.45 eA-3
PLAT977_ALERT_2_C Check Negative Difference Density on H4               -0.32 eA-3
PLAT977_ALERT_2_C Check Negative Difference Density on H5               -0.32 eA-3

Alert level G
PLAT007_ALERT_5_G Number of Unrefined Donor-H Atoms ..............         13 Report
PLAT154_ALERT_1_G The s.u.'s on the Cell Angles are Equal ..(Note)      0.002 Degree
PLAT230_ALERT_2_G Hirshfeld Test Diff for   S1       --C1        .        5.4 s.u.
PLAT230_ALERT_2_G Hirshfeld Test Diff for   S2       --C2        .        6.5 s.u.
PLAT790_ALERT_4_G Centre of Gravity not Within Unit Cell: Resd.  #          6 Note
              C H4 O
PLAT794_ALERT_5_G Tentative Bond Valency for Ni1       (II)      .       2.05 Info
PLAT910_ALERT_3_G Missing # of FCF Reflection(s) Below Theta(Min).          1 Note
PLAT933_ALERT_2_G Number of OMIT Records in Embedded .res File ...          1 Note
PLAT978_ALERT_2_G Number C-C Bonds with Positive Residual Density.          3 Info

   0 ALERT level A = Most likely a serious problem - resolve or explain
   1 ALERT level B = A potentially serious problem, consider carefully
  18 ALERT level C = Check. Ensure it is not caused by an omission or oversight
   9 ALERT level G = General information/check it is not something unexpected

   1 ALERT type 1 CIF construction/syntax error, inconsistent or missing data
  11 ALERT type 2 Indicator that the structure model may be wrong or deficient
   4 ALERT type 3 Indicator that the structure quality may be low
  10 ALERT type 4 Improvement, methodology, query or suggestion
   2 ALERT type 5 Informative message, check

---

Computing details

For both structures, data collection: X-AREA (Stoe, 2008); cell refinement: X-AREA (Stoe, 2008); data reduction: X-AREA (Stoe, 2008); program(s) used to solve structure: SHELXS97 (Sheldrick, 2008); program(s) used to refine structure: SHELXL2014 (Sheldrick, 2015); molecular graphics: Diamond (Brandenburg, 1990); software used to prepare material for publication: publCIF (Westrip, 2010).

(Acetonitrile-κN)tris(pyridine-4-thioamide-κN)bis(thiocyanato-κN)cobalt(II) acetonitrile disolvate (Compound1)

Crystal data

[Co(NCS)2(C2H3N)(C6H6N2S)3]·2C2H3N	F(000) = 1468
Mr = 712.81	Dx = 1.426 Mg m^−3
Monoclinic, P21/c	Mo Kα radiation, λ = 0.71073 Å
a = 11.3566 (4) Å	Cell parameters from 25043 reflections
b = 12.3251 (2) Å	θ = 1.7–27.0°
c = 23.7557 (8) Å	µ = 0.87 mm^−1
β = 93.273 (3)°	T = 200 K
V = 3319.69 (17) Å^3	Block, brown
Z = 4	0.12 × 0.10 × 0.08 mm

Data collection

STOE IPDS-2 diffractometer	Rint = 0.027
ω scans	θmax = 27.0°, θmin = 1.7°
25043 measured reflections	h = −14→14
7218 independent reflections	k = −14→15
6002 reflections with I > 2σ(I)	l = −30→30

Refinement

Refinement on F^2	9 restraints
Least-squares matrix: full	Hydrogen site location: mixed
R[F^2 > 2σ(F^2)] = 0.032	H-atom parameters constrained
wR(F^2) = 0.080	w = 1/[σ^2(Fo^2) + (0.0441P)^2 + 0.5907P] where P = (Fo^2 + 2Fc^2)/3
S = 1.04	(Δ/σ)max = 0.002
7218 reflections	Δρmax = 0.34 e Å^−3
419 parameters	Δρmin = −0.33 e Å^−3

Special details

Geometry. 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.

Fractional atomic coordinates and isotropic or equivalent isotropic displacement parameters (Ų)

	x	y	z	Uiso*/Ueq	Occ. (<1)
Co1	0.62828 (2)	0.49502 (2)	0.82672 (2)	0.02661 (7)
N1	0.70292 (15)	0.34698 (13)	0.80907 (7)	0.0359 (3)
C1	0.73383 (16)	0.26112 (15)	0.79702 (7)	0.0307 (4)
S1	0.77894 (5)	0.13954 (4)	0.78062 (2)	0.03821 (11)
N2	0.55051 (14)	0.64072 (13)	0.84732 (6)	0.0343 (3)
C2	0.52817 (15)	0.72538 (15)	0.86457 (7)	0.0295 (4)
S2	0.49682 (5)	0.84533 (4)	0.88860 (2)	0.04202 (12)
N3	0.61781 (15)	0.44151 (14)	0.91443 (6)	0.0387 (4)
C3	0.61548 (19)	0.40477 (17)	0.95811 (8)	0.0409 (4)
C4	0.6128 (3)	0.3573 (2)	1.01395 (10)	0.0704 (8)
H4A	0.6403	0.2820	1.0128	0.106*
H4B	0.5319	0.3589	1.0263	0.106*
H4C	0.6644	0.3989	1.0405	0.106*
N4	0.3375 (2)	0.6038 (3)	0.56403 (10)	0.0857 (9)
C5	0.2523 (3)	0.5621 (2)	0.57241 (10)	0.0576 (6)
C6	0.1421 (3)	0.5092 (3)	0.58145 (13)	0.0799 (10)
H6A	0.0807	0.5639	0.5858	0.120*
H6B	0.1505	0.4647	0.6156	0.120*
H6C	0.1200	0.4628	0.5490	0.120*
N5	−0.1359 (7)	0.5306 (5)	1.0399 (3)	0.087 (3)	0.62
C7	−0.0520 (6)	0.5785 (5)	1.04825 (19)	0.0699 (16)	0.62
C8	0.0562 (13)	0.6419 (14)	1.0603 (7)	0.082 (4)	0.62
H8A	0.0494	0.6828	1.0954	0.123*	0.62
H8B	0.0672	0.6925	1.0292	0.123*	0.62
H8C	0.1239	0.5928	1.0643	0.123*	0.62
N5'	−0.1549 (9)	0.4866 (8)	1.0254 (4)	0.063 (2)	0.38
C7'	−0.1247 (6)	0.4336 (6)	0.9894 (3)	0.0539 (16)	0.38
C8'	−0.0796 (19)	0.3668 (18)	0.9442 (9)	0.061 (4)	0.38
H8D	−0.0008	0.3922	0.9356	0.091*	0.38
H8E	−0.1328	0.3726	0.9104	0.091*	0.38
H8F	−0.0749	0.2909	0.9564	0.091*	0.38
N11	0.80040 (13)	0.56775 (12)	0.85214 (6)	0.0302 (3)
C11	0.89844 (17)	0.54836 (16)	0.82515 (8)	0.0339 (4)
H11	0.8952	0.4946	0.7964	0.041*
C12	1.00400 (17)	0.60162 (16)	0.83647 (7)	0.0340 (4)
H12	1.0706	0.5846	0.8157	0.041*
C13	1.01251 (16)	0.68036 (15)	0.87846 (7)	0.0293 (3)
C14	0.91243 (17)	0.69721 (16)	0.90835 (7)	0.0333 (4)
H14	0.9146	0.7476	0.9387	0.040*
C15	0.80988 (17)	0.64104 (16)	0.89414 (7)	0.0332 (4)
H15	0.7426	0.6548	0.9150	0.040*
C16	1.12262 (16)	0.74442 (15)	0.89216 (7)	0.0324 (4)
N12	1.21164 (14)	0.72915 (15)	0.85928 (7)	0.0397 (4)
H1N	1.2027	0.6957	0.8266	0.060*
H2N	1.2754	0.7687	0.8661	0.060*
S11	1.13309 (5)	0.83113 (5)	0.94560 (2)	0.04363 (13)
N21	0.45275 (13)	0.43047 (12)	0.80859 (6)	0.0304 (3)
C21	0.37190 (16)	0.43714 (17)	0.84752 (8)	0.0365 (4)
H21	0.3943	0.4691	0.8829	0.044*
C22	0.25792 (17)	0.39979 (17)	0.83859 (8)	0.0378 (4)
H22	0.2043	0.4034	0.8678	0.045*
C23	0.22269 (16)	0.35688 (15)	0.78638 (8)	0.0329 (4)
C24	0.30512 (17)	0.35158 (16)	0.74560 (8)	0.0341 (4)
H24	0.2837	0.3240	0.7091	0.041*
C25	0.41881 (16)	0.38689 (15)	0.75876 (7)	0.0317 (4)
H25	0.4755	0.3799	0.7311	0.038*
C26	0.09837 (16)	0.32242 (16)	0.77362 (8)	0.0362 (4)
N22	0.05589 (16)	0.25230 (17)	0.80962 (9)	0.0536 (5)
H3N	−0.0138	0.2228	0.8021	0.080*
H4N	0.0964	0.2277	0.8396	0.080*
S21	0.02293 (4)	0.37470 (4)	0.71886 (2)	0.03954 (12)
N31	0.63857 (13)	0.54138 (12)	0.73865 (6)	0.0284 (3)
C31	0.56230 (16)	0.61090 (15)	0.71318 (7)	0.0304 (4)
H31	0.5006	0.6392	0.7342	0.037*
C32	0.56864 (17)	0.64377 (15)	0.65764 (7)	0.0329 (4)
H32	0.5107	0.6910	0.6407	0.039*
C33	0.66128 (17)	0.60637 (15)	0.62729 (7)	0.0325 (4)
C34	0.73991 (17)	0.53387 (16)	0.65314 (7)	0.0334 (4)
H34	0.8040	0.5065	0.6334	0.040*
C35	0.72442 (16)	0.50179 (15)	0.70767 (7)	0.0324 (4)
H35	0.7768	0.4492	0.7243	0.039*
C36	0.67792 (19)	0.64037 (17)	0.56790 (8)	0.0399 (4)
N32	0.58298 (19)	0.63969 (19)	0.53393 (7)	0.0565 (5)
H5N	0.5843	0.6602	0.4985	0.085*
H6N	0.5141	0.6151	0.5435	0.085*
S31	0.81118 (6)	0.67528 (6)	0.54887 (2)	0.05599 (16)

Atomic displacement parameters (Ų)

	U^11	U^22	U^33	U^12	U^13	U^23
Co1	0.02609 (12)	0.02759 (12)	0.02615 (11)	−0.00033 (9)	0.00155 (8)	−0.00024 (9)
N1	0.0378 (9)	0.0323 (8)	0.0376 (8)	0.0035 (7)	0.0024 (6)	0.0008 (6)
C1	0.0272 (8)	0.0343 (10)	0.0306 (8)	−0.0027 (7)	0.0019 (6)	0.0036 (7)
S1	0.0420 (3)	0.0280 (2)	0.0453 (2)	0.0007 (2)	0.0089 (2)	−0.00051 (19)
N2	0.0336 (8)	0.0337 (8)	0.0356 (7)	0.0017 (7)	0.0027 (6)	−0.0023 (6)
C2	0.0281 (9)	0.0343 (10)	0.0260 (7)	−0.0013 (7)	0.0008 (6)	0.0017 (7)
S2	0.0581 (3)	0.0324 (2)	0.0357 (2)	0.0065 (2)	0.0041 (2)	−0.00340 (19)
N3	0.0387 (9)	0.0450 (10)	0.0323 (8)	−0.0007 (8)	0.0018 (6)	0.0051 (7)
C3	0.0459 (11)	0.0408 (11)	0.0365 (10)	0.0055 (9)	0.0063 (8)	0.0020 (8)
C4	0.106 (2)	0.0678 (17)	0.0391 (11)	0.0193 (16)	0.0174 (13)	0.0178 (12)
N4	0.0587 (15)	0.141 (3)	0.0563 (13)	−0.0153 (16)	−0.0072 (11)	0.0269 (15)
C5	0.0606 (16)	0.0687 (17)	0.0430 (12)	−0.0035 (13)	−0.0019 (11)	0.0062 (11)
C6	0.099 (2)	0.081 (2)	0.0614 (16)	−0.0387 (19)	0.0166 (16)	−0.0124 (14)
N5	0.129 (7)	0.067 (4)	0.072 (4)	0.025 (4)	0.055 (4)	0.004 (3)
C7	0.101 (4)	0.062 (3)	0.051 (2)	0.038 (3)	0.041 (3)	0.021 (2)
C8	0.103 (9)	0.084 (6)	0.061 (4)	0.041 (6)	0.026 (5)	0.020 (4)
N5'	0.061 (4)	0.070 (7)	0.059 (5)	0.013 (4)	0.006 (4)	0.004 (4)
C7'	0.044 (3)	0.061 (4)	0.054 (4)	−0.002 (3)	−0.010 (3)	0.026 (3)
C8'	0.061 (7)	0.064 (8)	0.057 (9)	0.006 (7)	−0.003 (6)	0.016 (5)
N11	0.0289 (7)	0.0315 (8)	0.0300 (7)	−0.0015 (6)	0.0009 (6)	−0.0007 (6)
C11	0.0320 (9)	0.0357 (10)	0.0342 (9)	−0.0019 (8)	0.0031 (7)	−0.0070 (7)
C12	0.0300 (9)	0.0388 (10)	0.0335 (9)	−0.0020 (8)	0.0047 (7)	−0.0044 (7)
C13	0.0301 (9)	0.0312 (9)	0.0264 (8)	−0.0012 (7)	−0.0012 (6)	0.0033 (6)
C14	0.0342 (9)	0.0360 (10)	0.0296 (8)	−0.0003 (8)	0.0004 (7)	−0.0056 (7)
C15	0.0302 (9)	0.0392 (10)	0.0304 (8)	−0.0014 (8)	0.0035 (7)	−0.0039 (7)
C16	0.0333 (9)	0.0330 (9)	0.0304 (8)	−0.0019 (8)	−0.0027 (7)	0.0054 (7)
N12	0.0305 (8)	0.0489 (10)	0.0397 (8)	−0.0079 (7)	0.0009 (6)	−0.0052 (7)
S11	0.0460 (3)	0.0464 (3)	0.0382 (2)	−0.0120 (2)	0.0000 (2)	−0.0079 (2)
N21	0.0278 (7)	0.0309 (8)	0.0325 (7)	−0.0026 (6)	0.0015 (6)	−0.0017 (6)
C21	0.0308 (9)	0.0469 (11)	0.0319 (9)	−0.0028 (8)	0.0026 (7)	−0.0053 (8)
C22	0.0297 (9)	0.0481 (11)	0.0359 (9)	−0.0017 (8)	0.0046 (7)	−0.0020 (8)
C23	0.0292 (9)	0.0297 (9)	0.0395 (9)	−0.0006 (7)	−0.0004 (7)	0.0018 (7)
C24	0.0325 (9)	0.0348 (10)	0.0349 (9)	−0.0010 (8)	0.0008 (7)	−0.0032 (7)
C25	0.0307 (9)	0.0331 (9)	0.0315 (8)	−0.0023 (7)	0.0029 (7)	−0.0026 (7)
C26	0.0289 (9)	0.0351 (10)	0.0446 (10)	0.0002 (8)	0.0019 (7)	−0.0040 (8)
N22	0.0319 (9)	0.0620 (13)	0.0661 (12)	−0.0109 (9)	−0.0058 (8)	0.0201 (10)
S21	0.0325 (2)	0.0461 (3)	0.0393 (2)	0.0015 (2)	−0.00403 (18)	−0.0051 (2)
N31	0.0294 (7)	0.0308 (7)	0.0253 (6)	−0.0011 (6)	0.0026 (5)	0.0001 (5)
C31	0.0299 (9)	0.0317 (9)	0.0298 (8)	0.0007 (7)	0.0027 (7)	0.0004 (7)
C32	0.0344 (9)	0.0327 (9)	0.0313 (8)	0.0004 (8)	−0.0005 (7)	0.0017 (7)
C33	0.0373 (10)	0.0324 (9)	0.0279 (8)	−0.0075 (8)	0.0011 (7)	−0.0014 (7)
C34	0.0327 (9)	0.0382 (10)	0.0299 (8)	−0.0014 (8)	0.0051 (7)	−0.0032 (7)
C35	0.0305 (9)	0.0363 (10)	0.0304 (8)	0.0017 (8)	0.0024 (7)	−0.0001 (7)
C36	0.0496 (12)	0.0416 (11)	0.0288 (8)	−0.0045 (9)	0.0054 (8)	0.0012 (8)
N32	0.0536 (12)	0.0857 (15)	0.0298 (8)	−0.0040 (11)	−0.0003 (8)	0.0136 (9)
S31	0.0562 (3)	0.0740 (4)	0.0391 (3)	−0.0196 (3)	0.0143 (2)	0.0030 (3)

Geometric parameters (Å, º)

Co1—N1	2.0650 (16)	C14—C15	1.380 (3)
Co1—N2	2.0720 (16)	C14—H14	0.9500
Co1—N21	2.1666 (15)	C15—H15	0.9500
Co1—N31	2.1785 (14)	C16—N12	1.326 (2)
Co1—N3	2.1950 (15)	C16—S11	1.6583 (19)
Co1—N11	2.2032 (15)	N12—H1N	0.8799
N1—C1	1.156 (2)	N12—H2N	0.8800
C1—S1	1.6378 (19)	N21—C25	1.336 (2)
N2—C2	1.155 (2)	N21—C21	1.342 (2)
C2—S2	1.6314 (19)	C21—C22	1.379 (3)
N3—C3	1.134 (2)	C21—H21	0.9500
C3—C4	1.451 (3)	C22—C23	1.386 (3)
C4—H4A	0.9800	C22—H22	0.9500
C4—H4B	0.9800	C23—C24	1.387 (3)
C4—H4C	0.9800	C23—C26	1.489 (3)
N4—C5	1.123 (4)	C24—C25	1.381 (3)
C5—C6	1.439 (4)	C24—H24	0.9500
C6—H6A	0.9800	C25—H25	0.9500
C6—H6B	0.9800	C26—N22	1.326 (3)
C6—H6C	0.9800	C26—S21	1.647 (2)
N5—C7	1.129 (8)	N22—H3N	0.8799
C7—C8	1.470 (14)	N22—H4N	0.8800
C8—H8A	0.9800	N31—C31	1.338 (2)
C8—H8B	0.9800	N31—C35	1.346 (2)
C8—H8C	0.9800	C31—C32	1.386 (2)
N5'—C7'	1.144 (9)	C31—H31	0.9500
C7'—C8'	1.469 (15)	C32—C33	1.388 (3)
C8'—H8D	0.9800	C32—H32	0.9500
C8'—H8E	0.9800	C33—C34	1.382 (3)
C8'—H8F	0.9800	C33—C36	1.494 (2)
N11—C11	1.338 (2)	C34—C35	1.375 (2)
N11—C15	1.346 (2)	C34—H34	0.9500
C11—C12	1.380 (3)	C35—H35	0.9500
C11—H11	0.9500	C36—N32	1.309 (3)
C12—C13	1.391 (3)	C36—S31	1.661 (2)
C12—H12	0.9500	N32—H5N	0.8800
C13—C14	1.390 (2)	N32—H6N	0.8799
C13—C16	1.499 (3)
N1—Co1—N2	177.65 (6)	C15—C14—C13	120.22 (16)
N1—Co1—N21	91.08 (6)	C15—C14—H14	119.9
N2—Co1—N21	88.02 (6)	C13—C14—H14	119.9
N1—Co1—N31	89.52 (6)	N11—C15—C14	123.29 (16)
N2—Co1—N31	92.66 (6)	N11—C15—H15	118.4
N21—Co1—N31	90.26 (6)	C14—C15—H15	118.4
N1—Co1—N3	88.41 (6)	N12—C16—C13	116.87 (16)
N2—Co1—N3	89.39 (6)	N12—C16—S11	121.24 (15)
N21—Co1—N3	88.82 (6)	C13—C16—S11	121.88 (13)
N31—Co1—N3	177.72 (6)	C16—N12—H1N	122.2
N1—Co1—N11	92.70 (6)	C16—N12—H2N	117.4
N2—Co1—N11	88.06 (6)	H1N—N12—H2N	118.3
N21—Co1—N11	174.69 (5)	C25—N21—C21	117.44 (16)
N31—Co1—N11	93.50 (5)	C25—N21—Co1	122.63 (12)
N3—Co1—N11	87.56 (6)	C21—N21—Co1	119.88 (12)
C1—N1—Co1	173.25 (16)	N21—C21—C22	123.13 (17)
N1—C1—S1	179.26 (19)	N21—C21—H21	118.4
C2—N2—Co1	166.49 (16)	C22—C21—H21	118.4
N2—C2—S2	179.66 (17)	C21—C22—C23	119.05 (17)
C3—N3—Co1	173.73 (17)	C21—C22—H22	120.5
N3—C3—C4	179.7 (3)	C23—C22—H22	120.5
C3—C4—H4A	109.5	C22—C23—C24	118.11 (17)
C3—C4—H4B	109.5	C22—C23—C26	120.86 (16)
H4A—C4—H4B	109.5	C24—C23—C26	120.96 (16)
C3—C4—H4C	109.5	C25—C24—C23	119.13 (17)
H4A—C4—H4C	109.5	C25—C24—H24	120.4
H4B—C4—H4C	109.5	C23—C24—H24	120.4
N4—C5—C6	178.3 (3)	N21—C25—C24	123.06 (16)
C5—C6—H6A	109.5	N21—C25—H25	118.5
C5—C6—H6B	109.5	C24—C25—H25	118.5
H6A—C6—H6B	109.5	N22—C26—C23	115.48 (17)
C5—C6—H6C	109.5	N22—C26—S21	124.91 (16)
H6A—C6—H6C	109.5	C23—C26—S21	119.58 (14)
H6B—C6—H6C	109.5	C26—N22—H3N	119.6
N5—C7—C8	178.7 (8)	C26—N22—H4N	123.7
C7—C8—H8A	109.5	H3N—N22—H4N	116.4
C7—C8—H8B	109.5	C31—N31—C35	117.08 (14)
H8A—C8—H8B	109.5	C31—N31—Co1	122.23 (11)
C7—C8—H8C	109.5	C35—N31—Co1	120.68 (12)
H8A—C8—H8C	109.5	N31—C31—C32	123.38 (16)
H8B—C8—H8C	109.5	N31—C31—H31	118.3
N5'—C7'—C8'	177.0 (11)	C32—C31—H31	118.3
C7'—C8'—H8D	109.5	C31—C32—C33	118.66 (17)
C7'—C8'—H8E	109.5	C31—C32—H32	120.7
H8D—C8'—H8E	109.5	C33—C32—H32	120.7
C7'—C8'—H8F	109.5	C34—C33—C32	118.28 (16)
H8D—C8'—H8F	109.5	C34—C33—C36	119.17 (17)
H8E—C8'—H8F	109.5	C32—C33—C36	122.54 (18)
C11—N11—C15	116.21 (16)	C35—C34—C33	119.35 (17)
C11—N11—Co1	123.08 (12)	C35—C34—H34	120.3
C15—N11—Co1	120.56 (12)	C33—C34—H34	120.3
N11—C11—C12	124.01 (17)	N31—C35—C34	123.11 (17)
N11—C11—H11	118.0	N31—C35—H35	118.4
C12—C11—H11	118.0	C34—C35—H35	118.4
C11—C12—C13	119.72 (17)	N32—C36—C33	115.85 (18)
C11—C12—H12	120.1	N32—C36—S31	124.40 (15)
C13—C12—H12	120.1	C33—C36—S31	119.75 (15)
C14—C13—C12	116.44 (17)	C36—N32—H5N	121.9
C14—C13—C16	120.45 (16)	C36—N32—H6N	123.8
C12—C13—C16	123.11 (16)	H5N—N32—H6N	114.2

Hydrogen-bond geometry (Å, º)

D—H···A	D—H	H···A	D···A	D—H···A
C4—H4C···N5′^i	0.98	2.37	3.081 (12)	129
C6—H6C···S31^ii	0.98	3.02	3.901 (3)	150
C11—H11···S21^i	0.95	2.83	3.6556 (18)	146
C12—H12···S1^iii	0.95	3.01	3.8491 (18)	148
N12—H1N···S1^iii	0.88	2.66	3.5097 (17)	163
N12—H2N···S2^i	0.88	2.71	3.5731 (17)	167
C21—H21···N3	0.95	2.63	3.134 (3)	114
C22—H22···N5^iv	0.95	2.50	3.384 (7)	154
C25—H25···S2^v	0.95	2.91	3.7172 (18)	144
N22—H3N···S1^vi	0.88	2.59	3.4715 (19)	179
N22—H4N···S31^v	0.88	2.87	3.729 (2)	167
C34—H34···S11^vii	0.95	2.98	3.7698 (19)	142
C35—H35···N1	0.95	2.56	3.094 (2)	116
C35—H35···S21^i	0.95	2.95	3.7301 (19)	140
N32—H5N···S2^viii	0.88	2.74	3.5390 (18)	152
N32—H6N···N4	0.88	2.10	2.951 (3)	164
C8—H8B···S11^vi	0.98	2.76	3.728 (19)	172
C8′—H8D···N5′^iv	0.98	2.46	3.26 (2)	140
C8′—H8F···S11^ix	0.98	2.88	3.65 (3)	137

Symmetry codes: (i) x+1, y, z; (ii) −x+1, −y+1, −z+1; (iii) −x+2, y+1/2, −z+3/2; (iv) −x, −y+1, −z+2; (v) −x+1, y−1/2, −z+3/2; (vi) x−1, y, z; (vii) −x+2, y−1/2, −z+3/2; (viii) x, −y+3/2, z−1/2; (ix) −x+1, −y+1, −z+2.

Tetrakis(pyridine-4-thioamide-κN)bis(thiocyanato-κN)nickel(II) methanol pentasolvate (Compound2)

Crystal data

[Ni(NCS)2(C6H6N2S)4]·5CH4O	Z = 2
Mr = 887.83	F(000) = 928
Triclinic, P1	Dx = 1.392 Mg m^−3
a = 10.4520 (3) Å	Mo Kα radiation, λ = 0.71073 Å
b = 14.5934 (4) Å	Cell parameters from 30865 reflections
c = 15.0580 (5) Å	θ = 1.5–27.0°
α = 101.553 (2)°	µ = 0.80 mm^−1
β = 97.105 (2)°	T = 200 K
γ = 106.417 (2)°	Block, yellow
V = 2118.43 (11) Å^3	0.30 × 0.18 × 0.10 mm

Data collection

STOE IPDS-2 diffractometer	7895 reflections with I > 2σ(I)
ω scans	Rint = 0.031
Absorption correction: numerical (X-Red and X-Shape; Stoe, 2008)	θmax = 27.0°, θmin = 1.5°
Tmin = 0.622, Tmax = 0.889	h = −13→13
30865 measured reflections	k = −18→18
9253 independent reflections	l = −19→19

Refinement

Refinement on F^2	0 restraints
Least-squares matrix: full	Hydrogen site location: mixed
R[F^2 > 2σ(F^2)] = 0.039	H-atom parameters constrained
wR(F^2) = 0.109	w = 1/[σ^2(Fo^2) + (0.0575P)^2 + 1.0537P] where P = (Fo^2 + 2Fc^2)/3
S = 1.06	(Δ/σ)max = 0.026
9253 reflections	Δρmax = 0.62 e Å^−3
486 parameters	Δρmin = −0.57 e Å^−3

Special details

Geometry. 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.

Fractional atomic coordinates and isotropic or equivalent isotropic displacement parameters (Ų)

	x	y	z	Uiso*/Ueq
Ni1	0.51341 (2)	0.75649 (2)	0.25835 (2)	0.02541 (8)
N1	0.54979 (18)	0.69614 (13)	0.13314 (13)	0.0327 (4)
C1	0.55335 (19)	0.66218 (14)	0.05750 (14)	0.0274 (4)
S1	0.55930 (7)	0.61468 (4)	−0.04898 (4)	0.03984 (14)
N2	0.47316 (17)	0.81774 (12)	0.38258 (12)	0.0312 (4)
C2	0.45784 (19)	0.84815 (14)	0.45634 (14)	0.0270 (4)
S2	0.43803 (5)	0.89172 (4)	0.56086 (4)	0.03231 (12)
O1	1.11056 (19)	0.76700 (17)	0.45151 (19)	0.0685 (6)
H1	1.1714	0.7529	0.4827	0.103*
C3	0.9826 (3)	0.7028 (2)	0.4528 (3)	0.0619 (8)
H3A	0.9932	0.6612	0.4951	0.093*
H3B	0.9412	0.6610	0.3905	0.093*
H3C	0.9240	0.7413	0.4737	0.093*
O2	0.2866 (3)	0.29719 (16)	0.25572 (19)	0.0746 (7)
H2	0.2560	0.2466	0.2117	0.112*
C4	0.2076 (4)	0.3592 (3)	0.2485 (3)	0.0869 (11)
H4A	0.2268	0.4087	0.3071	0.130*
H4B	0.1111	0.3202	0.2341	0.130*
H4C	0.2294	0.3923	0.1991	0.130*
O3	−0.1063 (2)	0.74182 (19)	0.0459 (2)	0.0769 (7)
H3	−0.1766	0.7415	0.0120	0.115*
C5	0.0077 (4)	0.7993 (3)	0.0215 (4)	0.0954 (14)
H5A	−0.0007	0.8647	0.0224	0.143*
H5B	0.0151	0.7679	−0.0407	0.143*
H5C	0.0891	0.8060	0.0655	0.143*
O4	0.9917 (4)	1.1226 (3)	0.1994 (3)	0.1172 (11)
H4	0.9255	1.1374	0.2174	0.176*
C6	0.9483 (5)	1.0242 (3)	0.1498 (3)	0.0990 (14)
H6A	1.0269	1.0004	0.1471	0.149*
H6B	0.9032	1.0186	0.0869	0.149*
H6C	0.8843	0.9844	0.1804	0.149*
O5	0.7792 (3)	1.1926 (2)	0.2133 (2)	0.0917 (9)
H5	0.8183	1.2328	0.1847	0.138*
C7	0.8085 (7)	1.2391 (5)	0.3032 (4)	0.138 (2)
H7A	0.8012	1.3054	0.3079	0.208*
H7B	0.9017	1.2459	0.3307	0.208*
H7C	0.7455	1.2058	0.3385	0.208*
N11	0.55562 (17)	0.64292 (12)	0.31467 (12)	0.0292 (3)
C11	0.5353 (3)	0.55466 (16)	0.25963 (16)	0.0399 (5)
H11	0.5032	0.5446	0.1955	0.048*
C12	0.5581 (3)	0.47683 (17)	0.29056 (16)	0.0428 (5)
H12	0.5421	0.4151	0.2483	0.051*
C13	0.6048 (2)	0.48958 (16)	0.38378 (15)	0.0336 (4)
C14	0.6301 (2)	0.58205 (16)	0.44148 (15)	0.0355 (5)
H14	0.6653	0.5947	0.5055	0.043*
C15	0.6037 (2)	0.65570 (16)	0.40479 (15)	0.0340 (4)
H15	0.6202	0.7185	0.4452	0.041*
C16	0.6263 (3)	0.40563 (17)	0.41981 (16)	0.0398 (5)
N12	0.5319 (2)	0.31979 (15)	0.38285 (15)	0.0457 (5)
H1N	0.4568	0.3147	0.3458	0.069*
H2N	0.5292	0.2622	0.3934	0.069*
S11	0.76130 (8)	0.42440 (6)	0.50051 (6)	0.0593 (2)
N21	0.72138 (16)	0.84055 (12)	0.30150 (12)	0.0286 (3)
C21	0.8184 (2)	0.80324 (16)	0.27672 (16)	0.0342 (4)
H21	0.7920	0.7383	0.2383	0.041*
C22	0.9556 (2)	0.85515 (16)	0.30453 (16)	0.0363 (5)
H22	1.0218	0.8256	0.2868	0.044*
C23	0.9951 (2)	0.95123 (16)	0.35878 (15)	0.0315 (4)
C24	0.8945 (2)	0.99054 (15)	0.38322 (15)	0.0329 (4)
H24	0.9178	1.0564	0.4192	0.040*
C25	0.7602 (2)	0.93304 (15)	0.35472 (15)	0.0315 (4)
H25	0.6922	0.9599	0.3735	0.038*
C26	1.1412 (2)	1.01136 (16)	0.38800 (15)	0.0344 (4)
N22	1.22398 (18)	0.96366 (15)	0.41365 (14)	0.0385 (4)
H4N	1.3129	0.9904	0.4262	0.058*
H3N	1.1961	0.9051	0.4250	0.058*
S21	1.19199 (6)	1.12876 (4)	0.38386 (5)	0.04608 (15)
N31	0.47817 (17)	0.87293 (12)	0.20441 (12)	0.0288 (3)
C31	0.5552 (2)	0.91431 (15)	0.14905 (15)	0.0324 (4)
H31	0.6224	0.8868	0.1296	0.039*
C32	0.5413 (2)	0.99481 (16)	0.11913 (16)	0.0359 (5)
H32	0.5997	1.0230	0.0814	0.043*
C33	0.4415 (2)	1.03440 (16)	0.14444 (16)	0.0345 (4)
C34	0.3592 (2)	0.99038 (17)	0.20028 (16)	0.0374 (5)
H34	0.2884	1.0144	0.2183	0.045*
C35	0.3820 (2)	0.91149 (16)	0.22892 (15)	0.0339 (4)
H35	0.3266	0.8830	0.2681	0.041*
C36	0.4190 (2)	1.11957 (17)	0.11202 (17)	0.0403 (5)
N32	0.5284 (2)	1.19414 (15)	0.11852 (18)	0.0520 (6)
H5N	0.6061	1.1934	0.1481	0.078*
H6N	0.5270	1.2440	0.0943	0.078*
S31	0.26248 (7)	1.11340 (5)	0.06808 (6)	0.0578 (2)
N41	0.30423 (17)	0.67290 (13)	0.21366 (12)	0.0310 (4)
C41	0.2366 (2)	0.66188 (16)	0.12907 (15)	0.0342 (4)
H41	0.2852	0.6901	0.0866	0.041*
C42	0.0993 (2)	0.61148 (16)	0.10008 (16)	0.0370 (5)
H42	0.0543	0.6076	0.0400	0.044*
C43	0.0283 (2)	0.56666 (16)	0.15998 (17)	0.0361 (5)
C44	0.0988 (2)	0.57619 (17)	0.24755 (17)	0.0398 (5)
H44	0.0540	0.5457	0.2902	0.048*
C45	0.2346 (2)	0.63047 (16)	0.27168 (16)	0.0363 (5)
H45	0.2812	0.6382	0.3324	0.044*
C46	−0.1192 (2)	0.50686 (18)	0.13038 (19)	0.0437 (5)
N42	−0.1973 (2)	0.54523 (17)	0.08483 (17)	0.0515 (5)
H7N	−0.1699	0.6010	0.0683	0.077*
H8N	−0.2852	0.5139	0.0721	0.077*
S41	−0.17085 (7)	0.39687 (6)	0.15227 (7)	0.0666 (2)

Atomic displacement parameters (Ų)

	U^11	U^22	U^33	U^12	U^13	U^23
Ni1	0.02585 (13)	0.02370 (13)	0.02562 (13)	0.00738 (9)	0.00263 (9)	0.00581 (9)
N1	0.0353 (9)	0.0315 (9)	0.0308 (9)	0.0112 (7)	0.0047 (7)	0.0065 (7)
C1	0.0274 (9)	0.0241 (9)	0.0301 (10)	0.0079 (7)	0.0012 (7)	0.0087 (8)
S1	0.0564 (3)	0.0380 (3)	0.0263 (3)	0.0188 (3)	0.0059 (2)	0.0062 (2)
N2	0.0327 (9)	0.0288 (8)	0.0318 (9)	0.0103 (7)	0.0055 (7)	0.0063 (7)
C2	0.0243 (8)	0.0228 (9)	0.0337 (11)	0.0073 (7)	0.0023 (7)	0.0089 (8)
S2	0.0369 (3)	0.0324 (3)	0.0302 (3)	0.0145 (2)	0.0078 (2)	0.0076 (2)
O1	0.0363 (9)	0.0662 (13)	0.1032 (18)	0.0093 (9)	−0.0012 (10)	0.0403 (13)
C3	0.0440 (14)	0.0586 (17)	0.082 (2)	0.0114 (13)	0.0091 (14)	0.0225 (16)
O2	0.0758 (15)	0.0506 (12)	0.0884 (18)	0.0191 (11)	−0.0121 (12)	0.0152 (11)
C4	0.072 (2)	0.080 (3)	0.110 (3)	0.029 (2)	0.010 (2)	0.021 (2)
O3	0.0504 (11)	0.0750 (15)	0.109 (2)	0.0153 (11)	−0.0006 (12)	0.0485 (15)
C5	0.062 (2)	0.088 (3)	0.153 (4)	0.0253 (19)	0.014 (2)	0.070 (3)
O4	0.109 (2)	0.115 (3)	0.120 (3)	0.049 (2)	−0.005 (2)	0.008 (2)
C6	0.087 (3)	0.101 (3)	0.083 (3)	0.001 (2)	0.006 (2)	0.014 (2)
O5	0.0716 (16)	0.0709 (16)	0.119 (2)	0.0153 (13)	−0.0155 (15)	0.0239 (16)
C7	0.186 (6)	0.197 (6)	0.094 (4)	0.101 (5)	0.082 (4)	0.079 (4)
N11	0.0326 (8)	0.0260 (8)	0.0280 (8)	0.0093 (7)	0.0016 (7)	0.0069 (6)
C11	0.0605 (14)	0.0289 (10)	0.0282 (11)	0.0141 (10)	0.0019 (10)	0.0063 (8)
C12	0.0683 (16)	0.0283 (10)	0.0330 (11)	0.0187 (10)	0.0061 (11)	0.0076 (9)
C13	0.0369 (10)	0.0334 (10)	0.0347 (11)	0.0141 (8)	0.0067 (9)	0.0134 (9)
C14	0.0408 (11)	0.0382 (11)	0.0278 (10)	0.0151 (9)	0.0003 (8)	0.0087 (8)
C15	0.0387 (11)	0.0307 (10)	0.0303 (10)	0.0126 (8)	−0.0010 (8)	0.0046 (8)
C16	0.0509 (13)	0.0387 (12)	0.0380 (12)	0.0216 (10)	0.0107 (10)	0.0160 (9)
N12	0.0586 (13)	0.0343 (10)	0.0495 (12)	0.0189 (9)	0.0064 (10)	0.0182 (9)
S11	0.0673 (4)	0.0537 (4)	0.0597 (4)	0.0251 (3)	−0.0083 (3)	0.0239 (3)
N21	0.0260 (8)	0.0273 (8)	0.0307 (9)	0.0077 (6)	0.0030 (6)	0.0053 (7)
C21	0.0310 (10)	0.0297 (10)	0.0386 (11)	0.0114 (8)	0.0024 (8)	0.0009 (8)
C22	0.0291 (10)	0.0355 (11)	0.0428 (12)	0.0138 (8)	0.0054 (9)	0.0026 (9)
C23	0.0276 (9)	0.0341 (10)	0.0306 (10)	0.0084 (8)	0.0034 (8)	0.0063 (8)
C24	0.0305 (10)	0.0293 (10)	0.0354 (11)	0.0080 (8)	0.0053 (8)	0.0029 (8)
C25	0.0281 (9)	0.0289 (10)	0.0363 (11)	0.0098 (8)	0.0057 (8)	0.0042 (8)
C26	0.0286 (10)	0.0387 (11)	0.0317 (11)	0.0087 (8)	0.0053 (8)	0.0023 (9)
N22	0.0256 (8)	0.0417 (10)	0.0452 (11)	0.0101 (7)	0.0023 (7)	0.0076 (8)
S21	0.0317 (3)	0.0354 (3)	0.0643 (4)	0.0052 (2)	0.0027 (3)	0.0088 (3)
N31	0.0300 (8)	0.0277 (8)	0.0301 (9)	0.0096 (7)	0.0044 (7)	0.0106 (7)
C31	0.0306 (10)	0.0330 (10)	0.0375 (11)	0.0123 (8)	0.0091 (8)	0.0123 (9)
C32	0.0358 (10)	0.0336 (11)	0.0411 (12)	0.0100 (8)	0.0091 (9)	0.0157 (9)
C33	0.0357 (10)	0.0299 (10)	0.0372 (11)	0.0105 (8)	0.0011 (9)	0.0101 (8)
C34	0.0391 (11)	0.0384 (11)	0.0412 (12)	0.0199 (9)	0.0099 (9)	0.0116 (9)
C35	0.0352 (10)	0.0368 (11)	0.0354 (11)	0.0159 (9)	0.0104 (9)	0.0127 (9)
C36	0.0462 (12)	0.0348 (11)	0.0432 (13)	0.0171 (10)	0.0038 (10)	0.0139 (10)
N32	0.0485 (12)	0.0370 (11)	0.0726 (16)	0.0118 (9)	0.0008 (11)	0.0269 (10)
S31	0.0447 (3)	0.0499 (4)	0.0843 (5)	0.0191 (3)	−0.0010 (3)	0.0312 (4)
N41	0.0283 (8)	0.0304 (8)	0.0317 (9)	0.0061 (7)	0.0020 (7)	0.0088 (7)
C41	0.0316 (10)	0.0360 (11)	0.0325 (11)	0.0070 (8)	0.0020 (8)	0.0106 (9)
C42	0.0326 (10)	0.0377 (11)	0.0368 (11)	0.0081 (9)	−0.0022 (9)	0.0105 (9)
C43	0.0287 (10)	0.0315 (10)	0.0452 (13)	0.0075 (8)	0.0027 (9)	0.0087 (9)
C44	0.0349 (11)	0.0414 (12)	0.0410 (12)	0.0057 (9)	0.0070 (9)	0.0150 (10)
C45	0.0338 (10)	0.0383 (11)	0.0333 (11)	0.0056 (9)	0.0016 (8)	0.0129 (9)
C46	0.0311 (11)	0.0405 (12)	0.0548 (15)	0.0066 (9)	0.0026 (10)	0.0116 (11)
N42	0.0308 (10)	0.0495 (12)	0.0692 (15)	0.0080 (9)	−0.0023 (10)	0.0176 (11)
S41	0.0384 (3)	0.0507 (4)	0.1036 (7)	−0.0017 (3)	−0.0032 (4)	0.0362 (4)

Geometric parameters (Å, º)

Ni1—N1	2.0435 (18)	N12—H1N	0.8800
Ni1—N2	2.0526 (18)	N12—H2N	0.8801
Ni1—N21	2.1157 (16)	N21—C21	1.337 (3)
Ni1—N31	2.1250 (17)	N21—C25	1.344 (3)
Ni1—N41	2.1262 (17)	C21—C22	1.384 (3)
Ni1—N11	2.1316 (17)	C21—H21	0.9500
N1—C1	1.157 (3)	C22—C23	1.391 (3)
C1—S1	1.631 (2)	C22—H22	0.9500
N2—C2	1.159 (3)	C23—C24	1.387 (3)
C2—S2	1.636 (2)	C23—C26	1.490 (3)
O1—C3	1.405 (3)	C24—C25	1.378 (3)
O1—H1	0.8400	C24—H24	0.9500
C3—H3A	0.9800	C25—H25	0.9500
C3—H3B	0.9800	C26—N22	1.322 (3)
C3—H3C	0.9800	C26—S21	1.661 (2)
O2—C4	1.398 (4)	N22—H4N	0.8800
O2—H2	0.8400	N22—H3N	0.8801
C4—H4A	0.9800	N31—C35	1.339 (3)
C4—H4B	0.9800	N31—C31	1.342 (3)
C4—H4C	0.9800	C31—C32	1.377 (3)
O3—C5	1.388 (4)	C31—H31	0.9500
O3—H3	0.8400	C32—C33	1.385 (3)
C5—H5A	0.9800	C32—H32	0.9500
C5—H5B	0.9800	C33—C34	1.394 (3)
C5—H5C	0.9800	C33—C36	1.489 (3)
O4—C6	1.395 (5)	C34—C35	1.377 (3)
O4—H4	0.8400	C34—H34	0.9500
C6—H6A	0.9800	C35—H35	0.9500
C6—H6B	0.9800	C36—N32	1.315 (3)
C6—H6C	0.9800	C36—S31	1.657 (2)
O5—C7	1.341 (6)	N32—H5N	0.8801
O5—H5	0.8401	N32—H6N	0.8799
C7—H7A	0.9800	N41—C41	1.334 (3)
C7—H7B	0.9800	N41—C45	1.340 (3)
C7—H7C	0.9800	C41—C42	1.383 (3)
N11—C11	1.329 (3)	C41—H41	0.9500
N11—C15	1.344 (3)	C42—C43	1.385 (3)
C11—C12	1.379 (3)	C42—H42	0.9500
C11—H11	0.9500	C43—C44	1.389 (3)
C12—C13	1.385 (3)	C43—C46	1.501 (3)
C12—H12	0.9500	C44—C45	1.377 (3)
C13—C14	1.385 (3)	C44—H44	0.9500
C13—C16	1.496 (3)	C45—H45	0.9500
C14—C15	1.380 (3)	C46—N42	1.313 (3)
C14—H14	0.9500	C46—S41	1.656 (3)
C15—H15	0.9500	N42—H7N	0.8799
C16—N12	1.319 (3)	N42—H8N	0.8800
C16—S11	1.663 (3)
N1—Ni1—N2	178.69 (7)	C16—N12—H1N	121.7
N1—Ni1—N21	90.21 (7)	C16—N12—H2N	127.8
N2—Ni1—N21	90.67 (7)	H1N—N12—H2N	110.4
N1—Ni1—N31	89.06 (7)	C21—N21—C25	117.90 (17)
N2—Ni1—N31	89.98 (7)	C21—N21—Ni1	121.02 (13)
N21—Ni1—N31	89.16 (6)	C25—N21—Ni1	121.08 (13)
N1—Ni1—N41	89.46 (7)	N21—C21—C22	122.89 (19)
N2—Ni1—N41	89.65 (7)	N21—C21—H21	118.6
N21—Ni1—N41	179.30 (7)	C22—C21—H21	118.6
N31—Ni1—N41	90.22 (7)	C21—C22—C23	118.92 (19)
N1—Ni1—N11	91.28 (7)	C21—C22—H22	120.5
N2—Ni1—N11	89.71 (7)	C23—C22—H22	120.5
N21—Ni1—N11	88.91 (6)	C24—C23—C22	118.20 (19)
N31—Ni1—N11	178.04 (6)	C24—C23—C26	120.74 (19)
N41—Ni1—N11	91.72 (7)	C22—C23—C26	121.04 (19)
C1—N1—Ni1	170.85 (17)	C25—C24—C23	119.27 (19)
N1—C1—S1	179.7 (2)	C25—C24—H24	120.4
C2—N2—Ni1	173.81 (17)	C23—C24—H24	120.4
N2—C2—S2	179.4 (2)	N21—C25—C24	122.78 (19)
C3—O1—H1	109.5	N21—C25—H25	118.6
O1—C3—H3A	109.5	C24—C25—H25	118.6
O1—C3—H3B	109.5	N22—C26—C23	115.3 (2)
H3A—C3—H3B	109.5	N22—C26—S21	124.16 (17)
O1—C3—H3C	109.5	C23—C26—S21	120.56 (17)
H3A—C3—H3C	109.5	C26—N22—H4N	122.5
H3B—C3—H3C	109.5	C26—N22—H3N	123.7
C4—O2—H2	109.5	H4N—N22—H3N	113.5
O2—C4—H4A	109.5	C35—N31—C31	117.33 (18)
O2—C4—H4B	109.5	C35—N31—Ni1	120.65 (14)
H4A—C4—H4B	109.5	C31—N31—Ni1	121.92 (14)
O2—C4—H4C	109.5	N31—C31—C32	123.0 (2)
H4A—C4—H4C	109.5	N31—C31—H31	118.5
H4B—C4—H4C	109.5	C32—C31—H31	118.5
C5—O3—H3	109.5	C31—C32—C33	119.5 (2)
O3—C5—H5A	109.5	C31—C32—H32	120.2
O3—C5—H5B	109.5	C33—C32—H32	120.2
H5A—C5—H5B	109.5	C32—C33—C34	117.7 (2)
O3—C5—H5C	109.5	C32—C33—C36	122.0 (2)
H5A—C5—H5C	109.5	C34—C33—C36	120.3 (2)
H5B—C5—H5C	109.5	C35—C34—C33	119.0 (2)
C6—O4—H4	109.5	C35—C34—H34	120.5
O4—C6—H6A	109.5	C33—C34—H34	120.5
O4—C6—H6B	109.5	N31—C35—C34	123.4 (2)
H6A—C6—H6B	109.5	N31—C35—H35	118.3
O4—C6—H6C	109.5	C34—C35—H35	118.3
H6A—C6—H6C	109.5	N32—C36—C33	116.1 (2)
H6B—C6—H6C	109.5	N32—C36—S31	124.75 (19)
C7—O5—H5	107.6	C33—C36—S31	119.16 (17)
O5—C7—H7A	107.6	C36—N32—H5N	118.1
O5—C7—H7B	110.9	C36—N32—H6N	122.8
H7A—C7—H7B	108.2	H5N—N32—H6N	119.1
O5—C7—H7C	112.6	C41—N41—C45	117.46 (18)
H7A—C7—H7C	108.2	C41—N41—Ni1	122.39 (14)
H7B—C7—H7C	109.3	C45—N41—Ni1	120.14 (14)
C11—N11—C15	116.96 (18)	N41—C41—C42	123.2 (2)
C11—N11—Ni1	119.87 (14)	N41—C41—H41	118.4
C15—N11—Ni1	123.18 (14)	C42—C41—H41	118.4
N11—C11—C12	123.6 (2)	C41—C42—C43	119.0 (2)
N11—C11—H11	118.2	C41—C42—H42	120.5
C12—C11—H11	118.2	C43—C42—H42	120.5
C11—C12—C13	119.3 (2)	C42—C43—C44	118.0 (2)
C11—C12—H12	120.3	C42—C43—C46	121.1 (2)
C13—C12—H12	120.3	C44—C43—C46	120.8 (2)
C14—C13—C12	117.7 (2)	C45—C44—C43	119.1 (2)
C14—C13—C16	121.8 (2)	C45—C44—H44	120.4
C12—C13—C16	120.5 (2)	C43—C44—H44	120.4
C15—C14—C13	119.2 (2)	N41—C45—C44	123.1 (2)
C15—C14—H14	120.4	N41—C45—H45	118.4
C13—C14—H14	120.4	C44—C45—H45	118.4
N11—C15—C14	123.3 (2)	N42—C46—C43	116.3 (2)
N11—C15—H15	118.4	N42—C46—S41	124.76 (18)
C14—C15—H15	118.4	C43—C46—S41	118.88 (18)
N12—C16—C13	114.9 (2)	C46—N42—H7N	125.7
N12—C16—S11	124.92 (18)	C46—N42—H8N	117.1
C13—C16—S11	120.23 (18)	H7N—N42—H8N	117.1

Hydrogen-bond geometry (Å, º)

D—H···A	D—H	H···A	D···A	D—H···A
O1—H1···S2^i	0.84	2.88	3.409 (2)	123
O1—H1···S11^ii	0.84	2.92	3.578 (2)	137
O2—H2···S31^iii	0.84	2.62	3.413 (3)	157
O3—H3···S1^iv	0.84	2.77	3.427 (2)	136
O3—H3···S31^v	0.84	2.93	3.576 (2)	135
C5—H5A···S31^v	0.98	3.03	3.632 (4)	121
O4—H4···O5	0.84	1.92	2.708 (5)	156
C6—H6B···S31^vi	0.98	2.73	3.566 (4)	143
O5—H5···S41^vii	0.84	2.51	3.216 (3)	142
C7—H7A···S41^vii	0.98	2.93	3.528 (5)	121
C11—H11···N1	0.95	2.52	3.063 (3)	117
C11—H11···S1^viii	0.95	2.73	3.442 (2)	133
C12—H12···S1^viii	0.95	2.96	3.542 (2)	121
C15—H15···N2	0.95	2.61	3.097 (3)	113
N12—H1N···O2	0.88	2.02	2.898 (3)	177
N12—H2N···S2^ix	0.88	2.58	3.446 (2)	171
C21—H21···N1	0.95	2.65	3.109 (3)	110
C25—H25···N2	0.95	2.66	3.122 (3)	111
C25—H25···S2^x	0.95	2.94	3.846 (2)	159
N22—H4N···S2^xi	0.88	2.64	3.4939 (19)	163
N22—H3N···O1	0.88	2.10	2.978 (3)	174
N32—H5N···O5	0.88	1.95	2.833 (3)	180
N32—H6N···S1^vi	0.88	2.64	3.478 (2)	159
C45—H45···S11^ix	0.95	2.89	3.673 (2)	141
N42—H7N···O3	0.88	2.08	2.957 (3)	173
N42—H8N···S1^xii	0.88	2.88	3.749 (2)	169

Symmetry codes: (i) x+1, y, z; (ii) −x+2, −y+1, −z+1; (iii) x, y−1, z; (iv) x−1, y, z; (v) −x, −y+2, −z; (vi) −x+1, −y+2, −z; (vii) x+1, y+1, z; (viii) −x+1, −y+1, −z; (ix) −x+1, −y+1, −z+1; (x) −x+1, −y+2, −z+1; (xi) −x+2, −y+2, −z+1; (xii) −x, −y+1, −z.