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Supporting information
![]() | Crystallographic Information File (CIF) https://doi.org/10.1107/S2056989022010362/mw2191sup1.cif |
![]() | Structure factor file (CIF format) https://doi.org/10.1107/S2056989022010362/mw2191Isup2.hkl |
![]() | Chemdraw file https://doi.org/10.1107/S2056989022010362/mw2191Isup3.cdx |
![]() | Text file https://doi.org/10.1107/S2056989022010362/mw2191sup4.txt |
![]() | Text file https://doi.org/10.1107/S2056989022010362/mw2191sup5.txt |
![]() | Joint Photographic Experts Group (JPEG) image https://doi.org/10.1107/S2056989022010362/mw2191sup6.jpg |
![]() | Joint Photographic Experts Group (JPEG) image https://doi.org/10.1107/S2056989022010362/mw2191sup7.jpg |
CCDC reference: 2215549
Data collection: CrysAlis PRO (Rigaku OD, 2021); cell refinement: CrysAlis PRO (Rigaku OD, 2021); data reduction: CrysAlis PRO (Rigaku OD, 2021); program(s) used to solve structure: SHELXT2018/2 (Sheldrick, 2015a); program(s) used to refine structure: SHELXL2018/3 (Sheldrick, 2015b); molecular graphics: OLEX2 (Dolomanov et al., 2009); software used to prepare material for publication: OLEX2 (Dolomanov et al., 2009).
[NiCl2(C4H6N2)4]·2C2H3N | Z = 1 |
Mr = 540.15 | F(000) = 282 |
Triclinic, P1 | Dx = 1.296 Mg m−3 |
a = 6.9625 (4) Å | Mo Kα radiation, λ = 0.71073 Å |
b = 9.8482 (8) Å | Cell parameters from 1586 reflections |
c = 11.0920 (12) Å | θ = 2.3–29.1° |
α = 74.417 (8)° | µ = 0.92 mm−1 |
β = 81.495 (6)° | T = 293 K |
γ = 71.191 (6)° | Plate, clear light blue |
V = 691.92 (10) Å3 | 0.2 × 0.15 × 0.03 mm |
Xcalibur, Eos diffractometer | 3161 independent reflections |
Radiation source: fine-focus sealed X-ray tube, Enhance (Mo) X-ray Source | 2500 reflections with I > 2σ(I) |
Graphite monochromator | Rint = 0.031 |
Detector resolution: 16.1593 pixels mm-1 | θmax = 29.4°, θmin = 1.9° |
ω scans | h = −8→9 |
Absorption correction: multi-scan (CrysAlisPro; Rigaku OD, 2021) | k = −13→12 |
Tmin = 0.795, Tmax = 1.000 | l = −14→15 |
5491 measured reflections |
Refinement on F2 | Primary atom site location: dual |
Least-squares matrix: full | Hydrogen site location: inferred from neighbouring sites |
R[F2 > 2σ(F2)] = 0.047 | H-atom parameters constrained |
wR(F2) = 0.130 | w = 1/[σ2(Fo2) + (0.0597P)2 + 0.1286P] where P = (Fo2 + 2Fc2)/3 |
S = 1.03 | (Δ/σ)max < 0.001 |
3161 reflections | Δρmax = 0.57 e Å−3 |
154 parameters | Δρmin = −0.45 e Å−3 |
0 restraints |
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. |
x | y | z | Uiso*/Ueq | ||
Ni1 | 0.500000 | 0.500000 | 1.000000 | 0.03038 (17) | |
C3 | 0.7595 (4) | 0.6698 (3) | 0.7894 (3) | 0.0418 (7) | |
H3 | 0.885178 | 0.600521 | 0.807503 | 0.050* | |
N2 | 0.4458 (4) | 0.7836 (3) | 0.7985 (2) | 0.0433 (6) | |
H2 | 0.318650 | 0.807118 | 0.822630 | 0.052* | |
N3 | 0.4456 (3) | 0.4131 (2) | 0.8602 (2) | 0.0357 (5) | |
C5 | 0.2833 (5) | 0.3210 (4) | 0.7604 (3) | 0.0509 (8) | |
H5 | 0.184629 | 0.285430 | 0.742681 | 0.061* | |
C2 | 0.7297 (5) | 0.7927 (4) | 0.6882 (3) | 0.0451 (7) | |
C7 | 0.5519 (4) | 0.3886 (3) | 0.7546 (3) | 0.0423 (7) | |
H7 | 0.676277 | 0.406895 | 0.728729 | 0.051* | |
C6 | 0.4560 (5) | 0.3325 (3) | 0.6874 (3) | 0.0464 (7) | |
C1 | 0.5283 (5) | 0.8623 (4) | 0.6981 (3) | 0.0522 (8) | |
H1 | 0.458925 | 0.949441 | 0.644659 | 0.063* | |
C8 | 0.5300 (7) | 0.2883 (5) | 0.5643 (4) | 0.0789 (12) | |
H8A | 0.602413 | 0.184814 | 0.580475 | 0.118* | |
H8B | 0.618933 | 0.343879 | 0.517855 | 0.118* | |
H8C | 0.415733 | 0.308009 | 0.516557 | 0.118* | |
N1 | 0.5870 (3) | 0.6636 (2) | 0.8565 (2) | 0.0354 (5) | |
Cl1 | 0.14603 (9) | 0.65951 (7) | 0.99696 (7) | 0.0397 (2) | |
N4 | 0.2819 (3) | 0.3701 (3) | 0.8618 (3) | 0.0433 (6) | |
H4 | 0.186829 | 0.373560 | 0.921075 | 0.052* | |
C4 | 0.8908 (6) | 0.8343 (5) | 0.5915 (4) | 0.0752 (12) | |
H4A | 1.021370 | 0.791110 | 0.626254 | 0.113* | |
H4B | 0.861116 | 0.939785 | 0.568022 | 0.113* | |
H4C | 0.892391 | 0.798492 | 0.518891 | 0.113* | |
C9 | 0.9065 (6) | 0.0384 (4) | 0.8290 (4) | 0.0599 (9) | |
N5 | 1.0344 (5) | 0.0551 (4) | 0.7595 (4) | 0.0803 (11) | |
C10 | 0.7409 (5) | 0.0148 (4) | 0.9202 (4) | 0.0674 (11) | |
H10A | 0.620906 | 0.035123 | 0.877485 | 0.101* | |
H10B | 0.714797 | 0.079430 | 0.975807 | 0.101* | |
H10C | 0.777646 | −0.085902 | 0.967767 | 0.101* |
U11 | U22 | U33 | U12 | U13 | U23 | |
Ni1 | 0.0233 (2) | 0.0330 (3) | 0.0342 (3) | −0.01078 (19) | 0.00342 (19) | −0.0069 (2) |
C3 | 0.0322 (14) | 0.0492 (18) | 0.0462 (18) | −0.0196 (13) | 0.0066 (13) | −0.0110 (15) |
N2 | 0.0338 (12) | 0.0407 (15) | 0.0471 (15) | −0.0084 (11) | 0.0012 (11) | −0.0019 (12) |
N3 | 0.0285 (11) | 0.0391 (13) | 0.0412 (14) | −0.0139 (10) | 0.0028 (10) | −0.0105 (11) |
C5 | 0.0442 (17) | 0.057 (2) | 0.061 (2) | −0.0219 (15) | −0.0078 (16) | −0.0199 (17) |
C2 | 0.0520 (18) | 0.056 (2) | 0.0330 (16) | −0.0293 (16) | 0.0077 (14) | −0.0092 (14) |
C7 | 0.0400 (15) | 0.0505 (18) | 0.0417 (17) | −0.0208 (13) | 0.0078 (13) | −0.0160 (14) |
C6 | 0.0565 (19) | 0.0449 (19) | 0.0390 (17) | −0.0168 (15) | −0.0018 (14) | −0.0104 (14) |
C1 | 0.057 (2) | 0.052 (2) | 0.0391 (18) | −0.0174 (16) | −0.0001 (15) | 0.0031 (15) |
C8 | 0.109 (3) | 0.085 (3) | 0.056 (3) | −0.038 (3) | 0.008 (2) | −0.034 (2) |
N1 | 0.0320 (11) | 0.0358 (13) | 0.0383 (13) | −0.0136 (10) | 0.0027 (10) | −0.0072 (11) |
Cl1 | 0.0231 (3) | 0.0415 (4) | 0.0513 (5) | −0.0089 (3) | 0.0037 (3) | −0.0101 (3) |
N4 | 0.0299 (12) | 0.0513 (15) | 0.0537 (16) | −0.0178 (11) | 0.0060 (11) | −0.0181 (13) |
C4 | 0.079 (3) | 0.092 (3) | 0.056 (2) | −0.047 (2) | 0.023 (2) | −0.007 (2) |
C9 | 0.057 (2) | 0.052 (2) | 0.067 (3) | −0.0080 (17) | −0.011 (2) | −0.0142 (19) |
N5 | 0.066 (2) | 0.081 (3) | 0.091 (3) | −0.0224 (18) | 0.009 (2) | −0.022 (2) |
C10 | 0.059 (2) | 0.065 (3) | 0.071 (3) | −0.0125 (19) | −0.002 (2) | −0.014 (2) |
Ni1—N3 | 2.091 (2) | C2—C4 | 1.511 (4) |
Ni1—N3i | 2.092 (2) | C7—H7 | 0.9300 |
Ni1—N1 | 2.112 (2) | C7—C6 | 1.383 (4) |
Ni1—N1i | 2.112 (2) | C6—C8 | 1.512 (5) |
Ni1—Cl1i | 2.4581 (6) | C1—H1 | 0.9300 |
Ni1—Cl1 | 2.4581 (6) | C8—H8A | 0.9600 |
C3—H3 | 0.9300 | C8—H8B | 0.9600 |
C3—C2 | 1.394 (4) | C8—H8C | 0.9600 |
C3—N1 | 1.326 (3) | N4—H4 | 0.8600 |
N2—H2 | 0.8600 | C4—H4A | 0.9600 |
N2—C1 | 1.344 (4) | C4—H4B | 0.9600 |
N2—N1 | 1.345 (3) | C4—H4C | 0.9600 |
N3—C7 | 1.327 (4) | C9—N5 | 1.113 (5) |
N3—N4 | 1.334 (3) | C9—C10 | 1.452 (5) |
C5—H5 | 0.9300 | C10—H10A | 0.9600 |
C5—C6 | 1.365 (4) | C10—H10B | 0.9600 |
C5—N4 | 1.337 (4) | C10—H10C | 0.9600 |
C2—C1 | 1.350 (5) | ||
N3—Ni1—N3i | 180.0 | C6—C7—H7 | 124.0 |
N3i—Ni1—N1i | 88.18 (9) | C5—C6—C7 | 104.0 (3) |
N3i—Ni1—N1 | 91.82 (9) | C5—C6—C8 | 128.1 (3) |
N3—Ni1—N1i | 91.83 (9) | C7—C6—C8 | 127.9 (3) |
N3—Ni1—N1 | 88.17 (9) | N2—C1—C2 | 108.0 (3) |
N3i—Ni1—Cl1i | 89.43 (6) | N2—C1—H1 | 126.0 |
N3i—Ni1—Cl1 | 90.57 (6) | C2—C1—H1 | 126.0 |
N3—Ni1—Cl1 | 89.43 (6) | C6—C8—H8A | 109.5 |
N3—Ni1—Cl1i | 90.57 (6) | C6—C8—H8B | 109.5 |
N1i—Ni1—N1 | 180.0 | C6—C8—H8C | 109.5 |
N1—Ni1—Cl1 | 89.91 (6) | H8A—C8—H8B | 109.5 |
N1i—Ni1—Cl1 | 90.09 (6) | H8A—C8—H8C | 109.5 |
N1—Ni1—Cl1i | 90.09 (6) | H8B—C8—H8C | 109.5 |
N1i—Ni1—Cl1i | 89.91 (6) | C3—N1—Ni1 | 134.1 (2) |
Cl1i—Ni1—Cl1 | 180.0 | C3—N1—N2 | 104.4 (2) |
C2—C3—H3 | 124.1 | N2—N1—Ni1 | 120.53 (17) |
N1—C3—H3 | 124.1 | N3—N4—C5 | 111.9 (3) |
N1—C3—C2 | 111.8 (3) | N3—N4—H4 | 124.0 |
C1—N2—H2 | 124.3 | C5—N4—H4 | 124.0 |
C1—N2—N1 | 111.4 (2) | C2—C4—H4A | 109.5 |
N1—N2—H2 | 124.3 | C2—C4—H4B | 109.5 |
C7—N3—Ni1 | 131.41 (19) | C2—C4—H4C | 109.5 |
C7—N3—N4 | 104.5 (2) | H4A—C4—H4B | 109.5 |
N4—N3—Ni1 | 124.12 (18) | H4A—C4—H4C | 109.5 |
C6—C5—H5 | 126.2 | H4B—C4—H4C | 109.5 |
N4—C5—H5 | 126.2 | N5—C9—C10 | 179.3 (5) |
N4—C5—C6 | 107.6 (3) | C9—C10—H10A | 109.5 |
C3—C2—C4 | 126.4 (3) | C9—C10—H10B | 109.5 |
C1—C2—C3 | 104.3 (3) | C9—C10—H10C | 109.5 |
C1—C2—C4 | 129.3 (3) | H10A—C10—H10B | 109.5 |
N3—C7—H7 | 124.0 | H10A—C10—H10C | 109.5 |
N3—C7—C6 | 112.1 (3) | H10B—C10—H10C | 109.5 |
Ni1—N3—C7—C6 | −178.4 (2) | C1—N2—N1—Ni1 | −170.4 (2) |
Ni1—N3—N4—C5 | 179.1 (2) | C1—N2—N1—C3 | 0.0 (3) |
C3—C2—C1—N2 | −0.5 (4) | N1—C3—C2—C1 | 0.5 (4) |
N3—C7—C6—C5 | −1.2 (4) | N1—C3—C2—C4 | −179.4 (3) |
N3—C7—C6—C8 | −178.9 (3) | N1—N2—C1—C2 | 0.3 (4) |
C2—C3—N1—Ni1 | 168.1 (2) | N4—N3—C7—C6 | 1.0 (3) |
C2—C3—N1—N2 | −0.3 (3) | N4—C5—C6—C7 | 0.8 (4) |
C7—N3—N4—C5 | −0.5 (3) | N4—C5—C6—C8 | 178.5 (3) |
C6—C5—N4—N3 | −0.3 (4) | C4—C2—C1—N2 | 179.4 (3) |
Symmetry code: (i) −x+1, −y+1, −z+2. |
D—H···A | D—H | H···A | D···A | D—H···A |
N2—H2···N5ii | 0.86 | 2.60 | 3.217 (4) | 130 |
C10ii—H10Cii···Cl1 | 0.96 | 2.94 | 3.697 (3) | 137 |
N2—H2···Cl1 | 0.86 | 2.50 | 3.088 (3) | 127 |
N4—H4···Cl1iii | 0.86 | 2.45 | 3.217 (2) | 149 |
C10i—H10Bi···Cl1 | 0.96 | 3.12 | 3.8958 (3) | 139 |
C5—H5···N5iv | 0.93 | 2.74 | 3.5785 (2) | 150 |
Symmetry codes: (i) −x+1, −y+1, −z+2; (ii) x−1, y+1, z; (iii) −x, −y+1, −z+2; (iv) x−1, y, z. |