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Seven crystal structures of five first-row (Fe, Co, Ni, Cu, and Zn) and one second-row (Cd) transition metal–4-picoline (pic)–sulfate complexes of the form [M(pic)x]SO4 are reported. These complexes are catena-poly[[tetra­kis­(4-methyl­pyridine-κN)metal(II)]-μ-sulfato-κ2O:O′], [M(SO4)(C6H7N)4]n, where the metal/M is iron, cobalt, nickel, and cadmium, di-μ-sulfato-κ4O:O-bis­[tris­(4-methyl­pyridine-κN)copper(II)], [Cu2(SO4)2(C6H7N)6], catena-poly[[bis­(4-methyl­pyridine-κN)zinc(II)]-μ-sulfato-κ2O:O′], [Zn(SO4)(C6H7N)2]n, and catena-poly[[tris­(4-methyl­pyridine-κN)zinc(II)]-μ-sulfato-κ2O:O′], [Zn(SO4)(C6H7N)3]n. The Fe, Co, Ni, and Cd compounds are isomorphous, displaying polymeric crystal structures with infinite chains of MII ions adopting an octa­hedral N4O2 coordination environment that involves four picoline ligands and two bridging sulfate anions. The Cu compound features a dimeric crystal structure, with the CuII ions possessing square-pyramidal N3O2 coordination environments that contain three picoline ligands and two bridging sulfate anions. Zinc crystallizes in two forms, one exhibiting a polymeric crystal structure with infinite chains of ZnII ions adopting a tetra­hedral N2O2 coordination containing two picoline ligands and two bridging sulfate anions, and the other exhibiting a polymeric crystal structure with infinite chains of ZnII ions adopting a trigonal bipyramidal N3O2 coordination containing three picoline ligands and two bridging sulfate anions. The structures are compared with the analogous pyridine complexes, and the observed coordination environments are examined in relation to crystal field theory.

Supporting information

cif

Crystallographic Information File (CIF) https://doi.org/10.1107/S2053229619004625/ov3124sup1.cif
Contains datablocks umd1308_a, umd1358_a, umd1307, umd1301_a, UMD1448_a, umd1540c_a, umd1375_a, global

hkl

Structure factor file (CIF format) https://doi.org/10.1107/S2053229619004625/ov3124umd1308_asup2.hkl
Contains datablock umd1308_a

hkl

Structure factor file (CIF format) https://doi.org/10.1107/S2053229619004625/ov3124umd1358_asup3.hkl
Contains datablock umd1358_a

hkl

Structure factor file (CIF format) https://doi.org/10.1107/S2053229619004625/ov3124umd1307sup4.hkl
Contains datablock umd1307

hkl

Structure factor file (CIF format) https://doi.org/10.1107/S2053229619004625/ov3124umd1301_asup5.hkl
Contains datablock umd1301_a

hkl

Structure factor file (CIF format) https://doi.org/10.1107/S2053229619004625/ov3124UMD1448_asup6.hkl
Contains datablock UMD1448_a

hkl

Structure factor file (CIF format) https://doi.org/10.1107/S2053229619004625/ov3124umd1540c_asup7.hkl
Contains datablock umd1540c_a

hkl

Structure factor file (CIF format) https://doi.org/10.1107/S2053229619004625/ov3124umd1375_asup8.hkl
Contains datablock umd1375_a

CCDC references: 1908116; 1908115; 1908114; 1908113; 1908112; 1908111; 1908110

Computing details top

Data collection: APEX3 (Bruker, 2016) for umd1308_a, umd1358_a, umd1307, umd1301_a, UMD1448_a, umd1375_a; APEX2 (Bruker, 2015) for umd1540c_a. Cell refinement: SAINT (Bruker, 2016) for umd1308_a, umd1358_a, umd1307, umd1301_a, UMD1448_a, umd1375_a; SAINT (Bruker, 2015) for umd1540c_a. Data reduction: SAINT (Bruker, 2016) for umd1308_a, umd1358_a, umd1307, umd1301_a, UMD1448_a, umd1375_a; SAINT (Bruker, 2015) for umd1540c_a. For all structures, program(s) used to solve structure: SHELXS97 (Sheldrick, 2008); program(s) used to refine structure: SHELXL2014 (Sheldrick, 2015); molecular graphics: OLEX2 (Dolomanov et al., 2009); software used to prepare material for publication: OLEX2 (Dolomanov et al., 2009).

catena-Poly[[tetrakis(4-methylpyridine-κN)iron(II)]-sulfato-κ2O:O'] (umd1308_a) top
Crystal data top
[Fe(SO4)(C6H7N)4]F(000) = 2192
Mr = 524.41Dx = 1.364 Mg m3
Monoclinic, C2/cMo Kα radiation, λ = 0.71073 Å
a = 11.4472 (13) ÅCell parameters from 9601 reflections
b = 18.822 (2) Åθ = 3.1–25.8°
c = 24.010 (3) ŵ = 0.71 mm1
β = 99.112 (3)°T = 297 K
V = 5108.0 (11) Å3Block, yellow-brown
Z = 80.22 × 0.2 × 0.2 mm
Data collection top
Bruker D8 Venture CMOS
diffractometer
4320 reflections with I > 2σ(I)
φ and ω scansRint = 0.037
Absorption correction: multi-scan
(SADABS; Bruker, 2016)
θmax = 25.8°, θmin = 2.9°
Tmin = 0.306, Tmax = 0.332h = 1314
80351 measured reflectionsk = 2222
4895 independent reflectionsl = 2929
Refinement top
Refinement on F2Hydrogen site location: inferred from neighbouring sites
Least-squares matrix: fullH-atom parameters constrained
R[F2 > 2σ(F2)] = 0.030 w = 1/[σ2(Fo2) + (0.0378P)2 + 5.7613P]
where P = (Fo2 + 2Fc2)/3
wR(F2) = 0.083(Δ/σ)max = 0.002
S = 1.10Δρmax = 0.40 e Å3
4895 reflectionsΔρmin = 0.30 e Å3
314 parametersExtinction correction: SHELXL2014 (Sheldrick, 2015), Fc*=kFc[1+0.001xFc2λ3/sin(2θ)]-1/4
6 restraintsExtinction coefficient: 0.00300 (16)
Primary atom site location: structure-invariant direct methods
Special details top

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 (Å2) top
xyzUiso*/Ueq
Fe10.50000.50000.50000.02613 (11)
Fe20.50000.47022 (2)0.75000.02408 (11)
S10.34329 (4)0.47876 (3)0.61286 (2)0.02862 (12)
O10.42874 (11)0.48685 (8)0.57272 (5)0.0355 (3)
O20.41429 (12)0.46837 (8)0.66946 (5)0.0397 (3)
O30.27471 (15)0.54311 (10)0.61302 (7)0.0601 (5)
O40.27080 (14)0.41670 (10)0.59876 (6)0.0541 (4)
N10.51167 (14)0.38214 (9)0.49376 (6)0.0368 (4)
N20.31868 (13)0.50168 (8)0.44867 (6)0.0317 (3)
N30.61876 (13)0.55408 (8)0.72335 (6)0.0309 (3)
N40.38082 (13)0.38122 (8)0.76966 (6)0.0319 (3)
C10.4357 (2)0.33786 (12)0.51286 (10)0.0503 (5)
H10.37630.35700.53050.060*
C20.4416 (3)0.26555 (14)0.50761 (13)0.0735 (8)
H20.38600.23700.52110.088*
C30.5296 (3)0.23473 (14)0.48236 (13)0.0762 (9)
C40.6085 (3)0.28022 (14)0.46382 (11)0.0614 (7)
H40.67040.26220.44720.074*
C50.59684 (19)0.35242 (12)0.46958 (9)0.0448 (5)
H50.65100.38200.45600.054*
C60.5398 (5)0.15502 (19)0.4760 (2)0.142 (2)
H6A0.46280.13530.46330.213*
H6B0.57230.13450.51160.213*
H6C0.59070.14470.44880.213*
C70.21927 (18)0.47721 (12)0.46451 (8)0.0423 (5)
H70.22430.45550.49960.051*
C80.11013 (18)0.48259 (14)0.43148 (9)0.0480 (6)
H80.04380.46430.44440.058*
C90.09827 (17)0.51482 (12)0.37941 (9)0.0405 (5)
C100.20008 (17)0.54053 (12)0.36336 (8)0.0421 (5)
H100.19680.56320.32870.051*
C110.30687 (17)0.53292 (11)0.39820 (8)0.0381 (5)
H110.37440.55050.38600.046*
C120.0192 (2)0.52174 (19)0.34214 (12)0.0723 (9)
H12A0.07360.48790.35350.108*
H12B0.00990.51280.30370.108*
H12C0.04940.56890.34530.108*
C130.58588 (18)0.59392 (11)0.67754 (8)0.0392 (4)
H130.50890.58940.65860.047*
C140.6601 (2)0.64131 (12)0.65696 (9)0.0486 (5)
H140.63250.66790.62490.058*
C150.7746 (2)0.64959 (12)0.68349 (10)0.0492 (5)
C160.80798 (19)0.60973 (14)0.73155 (10)0.0524 (6)
H160.88400.61430.75170.063*
C170.72941 (17)0.56319 (12)0.74991 (9)0.0418 (5)
H170.75460.53680.78240.050*
C180.8597 (3)0.69965 (17)0.66174 (15)0.0827 (9)
H18A0.90710.72310.69290.124*
H18B0.81620.73440.63750.124*
H18C0.91020.67330.64090.124*
C190.40919 (17)0.34134 (11)0.81595 (8)0.0376 (4)
H190.48110.34970.83900.045*
C200.33698 (19)0.28836 (12)0.83116 (9)0.0444 (5)
H200.36090.26220.86380.053*
C210.22959 (19)0.27409 (11)0.79815 (9)0.0432 (5)
C220.20183 (19)0.31401 (12)0.74954 (9)0.0461 (5)
H220.13130.30580.72530.055*
C230.27806 (17)0.36581 (11)0.73682 (8)0.0388 (4)
H230.25720.39150.70370.047*
C240.1458 (2)0.21870 (14)0.81395 (11)0.0631 (7)
H24A0.10630.19580.78040.095*
H24B0.08830.24090.83330.095*
H24C0.18940.18400.83820.095*
Atomic displacement parameters (Å2) top
U11U22U33U12U13U23
Fe10.02428 (18)0.0346 (2)0.02019 (18)0.00324 (14)0.00571 (13)0.00115 (14)
Fe20.02236 (18)0.0318 (2)0.01830 (17)0.0000.00385 (12)0.000
S10.0230 (2)0.0449 (3)0.0184 (2)0.00246 (17)0.00465 (16)0.00322 (17)
O10.0312 (7)0.0534 (8)0.0241 (6)0.0044 (6)0.0112 (5)0.0018 (6)
O20.0411 (8)0.0563 (9)0.0203 (6)0.0082 (6)0.0000 (5)0.0051 (6)
O30.0550 (10)0.0692 (11)0.0627 (10)0.0278 (8)0.0291 (8)0.0227 (9)
O40.0518 (9)0.0755 (11)0.0356 (8)0.0345 (8)0.0090 (7)0.0054 (7)
N10.0399 (9)0.0386 (9)0.0325 (8)0.0024 (7)0.0074 (7)0.0014 (7)
N20.0285 (8)0.0402 (9)0.0262 (8)0.0036 (7)0.0039 (6)0.0017 (6)
N30.0283 (8)0.0359 (8)0.0291 (8)0.0020 (6)0.0060 (6)0.0011 (6)
N40.0309 (8)0.0348 (8)0.0314 (8)0.0005 (6)0.0093 (6)0.0015 (6)
C10.0578 (14)0.0454 (13)0.0527 (13)0.0091 (10)0.0240 (11)0.0024 (10)
C20.100 (2)0.0436 (14)0.088 (2)0.0173 (14)0.0481 (18)0.0003 (13)
C30.118 (3)0.0377 (13)0.082 (2)0.0009 (15)0.0445 (19)0.0022 (13)
C40.0807 (18)0.0494 (14)0.0609 (15)0.0148 (13)0.0320 (13)0.0041 (12)
C50.0498 (12)0.0427 (12)0.0450 (12)0.0048 (10)0.0167 (10)0.0062 (9)
C60.212 (5)0.0458 (19)0.192 (5)0.003 (2)0.110 (4)0.009 (2)
C70.0389 (11)0.0592 (13)0.0282 (10)0.0125 (10)0.0040 (8)0.0066 (9)
C80.0306 (10)0.0749 (16)0.0388 (11)0.0155 (10)0.0067 (8)0.0047 (10)
C90.0291 (10)0.0568 (13)0.0350 (10)0.0006 (9)0.0035 (8)0.0030 (9)
C100.0343 (10)0.0602 (14)0.0314 (10)0.0031 (9)0.0042 (8)0.0112 (9)
C110.0280 (9)0.0521 (12)0.0343 (10)0.0022 (8)0.0055 (8)0.0113 (9)
C120.0339 (12)0.125 (3)0.0539 (15)0.0001 (14)0.0042 (11)0.0076 (16)
C130.0411 (11)0.0383 (11)0.0360 (10)0.0047 (9)0.0002 (8)0.0016 (8)
C140.0655 (15)0.0410 (12)0.0401 (11)0.0060 (10)0.0105 (10)0.0084 (9)
C150.0484 (12)0.0482 (13)0.0561 (13)0.0122 (10)0.0237 (11)0.0008 (10)
C160.0318 (11)0.0664 (16)0.0595 (14)0.0100 (10)0.0087 (10)0.0042 (12)
C170.0312 (10)0.0545 (13)0.0396 (11)0.0036 (9)0.0049 (8)0.0061 (9)
C180.081 (2)0.078 (2)0.099 (2)0.0275 (17)0.0440 (18)0.0116 (17)
C190.0362 (10)0.0396 (11)0.0376 (10)0.0031 (8)0.0080 (8)0.0047 (8)
C200.0533 (12)0.0388 (11)0.0431 (11)0.0012 (10)0.0139 (10)0.0108 (9)
C210.0513 (12)0.0384 (11)0.0438 (11)0.0078 (9)0.0196 (10)0.0032 (9)
C220.0439 (11)0.0547 (13)0.0400 (11)0.0143 (10)0.0074 (9)0.0012 (10)
C230.0390 (11)0.0455 (12)0.0320 (10)0.0068 (9)0.0061 (8)0.0042 (8)
C240.0746 (17)0.0559 (15)0.0639 (16)0.0226 (13)0.0269 (13)0.0025 (12)
Geometric parameters (Å, º) top
Fe1—O1i2.0558 (12)C7—H70.9300
Fe1—O12.0558 (12)C7—C81.373 (3)
Fe1—N12.2289 (17)C8—H80.9300
Fe1—N1i2.2289 (17)C8—C91.377 (3)
Fe1—N2i2.2400 (15)C9—C101.372 (3)
Fe1—N22.2400 (15)C9—C121.498 (3)
Fe2—O2ii2.0254 (13)C10—H100.9300
Fe2—O22.0254 (12)C10—C111.375 (3)
Fe2—N32.2415 (15)C11—H110.9300
Fe2—N3ii2.2415 (15)C12—H12A0.9600
Fe2—N42.2570 (16)C12—H12B0.9600
Fe2—N4ii2.2570 (15)C12—H12C0.9600
S1—O11.4856 (12)C13—H130.9300
S1—O21.4819 (13)C13—C141.376 (3)
S1—O31.4437 (17)C14—H140.9300
S1—O41.4418 (16)C14—C151.373 (3)
N1—C11.337 (3)C15—C161.379 (3)
N1—C51.334 (3)C15—C181.508 (3)
N2—C71.337 (2)C16—H160.9300
N2—C111.334 (2)C16—C171.377 (3)
N3—C131.335 (2)C17—H170.9300
N3—C171.336 (2)C18—H18A0.9600
N4—C191.338 (2)C18—H18B0.9600
N4—C231.340 (2)C18—H18C0.9600
C1—H10.9300C19—H190.9300
C1—C21.370 (4)C19—C201.381 (3)
C2—H20.9300C20—H200.9300
C2—C31.384 (4)C20—C211.379 (3)
C3—C41.369 (4)C21—C221.382 (3)
C3—C61.515 (4)C21—C241.505 (3)
C4—H40.9300C22—H220.9300
C4—C51.375 (3)C22—C231.375 (3)
C5—H50.9300C23—H230.9300
C6—H6A0.9600C24—H24A0.9600
C6—H6B0.9600C24—H24B0.9600
C6—H6C0.9600C24—H24C0.9600
O1i—Fe1—O1180.0C3—C6—H6C109.5
O1—Fe1—N188.47 (6)H6A—C6—H6B109.5
O1i—Fe1—N191.53 (6)H6A—C6—H6C109.5
O1—Fe1—N1i91.53 (6)H6B—C6—H6C109.5
O1i—Fe1—N1i88.47 (6)N2—C7—H7118.4
O1i—Fe1—N289.36 (5)N2—C7—C8123.21 (18)
O1i—Fe1—N2i90.64 (5)C8—C7—H7118.4
O1—Fe1—N290.64 (5)C7—C8—H8119.8
O1—Fe1—N2i89.36 (5)C7—C8—C9120.44 (19)
N1i—Fe1—N1180.00 (8)C9—C8—H8119.8
N1—Fe1—N2i87.87 (6)C8—C9—C12122.1 (2)
N1i—Fe1—N287.87 (6)C10—C9—C8116.38 (18)
N1i—Fe1—N2i92.13 (6)C10—C9—C12121.6 (2)
N1—Fe1—N292.13 (6)C9—C10—H10119.8
N2—Fe1—N2i180.00 (11)C9—C10—C11120.33 (18)
O2ii—Fe2—O2178.03 (9)C11—C10—H10119.8
O2ii—Fe2—N3ii87.92 (5)N2—C11—C10123.43 (18)
O2—Fe2—N3ii93.47 (6)N2—C11—H11118.3
O2ii—Fe2—N393.47 (6)C10—C11—H11118.3
O2—Fe2—N387.92 (6)C9—C12—H12A109.5
O2—Fe2—N488.25 (6)C9—C12—H12B109.5
O2ii—Fe2—N4ii88.25 (6)C9—C12—H12C109.5
O2—Fe2—N4ii90.29 (6)H12A—C12—H12B109.5
O2ii—Fe2—N490.29 (6)H12A—C12—H12C109.5
N3ii—Fe2—N390.47 (8)H12B—C12—H12C109.5
N3—Fe2—N4ii92.81 (5)N3—C13—H13118.3
N3ii—Fe2—N492.81 (6)N3—C13—C14123.39 (19)
N3—Fe2—N4175.09 (5)C14—C13—H13118.3
N3ii—Fe2—N4ii175.09 (5)C13—C14—H14119.8
N4—Fe2—N4ii84.16 (8)C15—C14—C13120.3 (2)
O2—S1—O1106.66 (8)C15—C14—H14119.8
O3—S1—O1109.27 (9)C14—C15—C16116.39 (19)
O3—S1—O2109.12 (10)C14—C15—C18122.2 (2)
O4—S1—O1110.14 (9)C16—C15—C18121.4 (2)
O4—S1—O2108.67 (9)C15—C16—H16119.8
O4—S1—O3112.79 (11)C17—C16—C15120.4 (2)
S1—O1—Fe1162.52 (9)C17—C16—H16119.8
S1—O2—Fe2170.32 (11)N3—C17—C16123.2 (2)
C1—N1—Fe1123.25 (14)N3—C17—H17118.4
C5—N1—Fe1120.15 (14)C16—C17—H17118.4
C5—N1—C1116.59 (19)C15—C18—H18A109.5
C7—N2—Fe1126.50 (13)C15—C18—H18B109.5
C11—N2—Fe1117.23 (12)C15—C18—H18C109.5
C11—N2—C7116.20 (16)H18A—C18—H18B109.5
C13—N3—Fe2121.74 (13)H18A—C18—H18C109.5
C13—N3—C17116.32 (17)H18B—C18—H18C109.5
C17—N3—Fe2121.75 (13)N4—C19—H19118.4
C19—N4—Fe2120.99 (13)N4—C19—C20123.25 (19)
C19—N4—C23116.25 (17)C20—C19—H19118.4
C23—N4—Fe2122.75 (13)C19—C20—H20119.8
N1—C1—H1118.5C21—C20—C19120.33 (19)
N1—C1—C2123.0 (2)C21—C20—H20119.8
C2—C1—H1118.5C20—C21—C22116.37 (19)
C1—C2—H2119.8C20—C21—C24122.4 (2)
C1—C2—C3120.4 (2)C22—C21—C24121.3 (2)
C3—C2—H2119.8C21—C22—H22119.9
C2—C3—C6122.2 (3)C23—C22—C21120.3 (2)
C4—C3—C2116.4 (2)C23—C22—H22119.9
C4—C3—C6121.4 (3)N4—C23—C22123.49 (19)
C3—C4—H4119.8N4—C23—H23118.3
C3—C4—C5120.4 (2)C22—C23—H23118.3
C5—C4—H4119.8C21—C24—H24A109.5
N1—C5—C4123.2 (2)C21—C24—H24B109.5
N1—C5—H5118.4C21—C24—H24C109.5
C4—C5—H5118.4H24A—C24—H24B109.5
C3—C6—H6A109.5H24A—C24—H24C109.5
C3—C6—H6B109.5H24B—C24—H24C109.5
Fe1—N1—C1—C2178.3 (2)C7—N2—C11—C100.1 (3)
Fe1—N1—C5—C4179.33 (19)C7—C8—C9—C100.1 (4)
Fe1—N2—C7—C8177.35 (18)C7—C8—C9—C12180.0 (2)
Fe1—N2—C11—C10177.06 (17)C8—C9—C10—C110.7 (3)
Fe2—N3—C13—C14173.88 (16)C9—C10—C11—N20.7 (4)
Fe2—N3—C17—C16173.95 (18)C11—N2—C7—C80.5 (3)
Fe2—N4—C19—C20177.08 (15)C12—C9—C10—C11179.5 (2)
Fe2—N4—C23—C22176.84 (16)C13—N3—C17—C161.1 (3)
O2—S1—O1—Fe1178.2 (3)C13—C14—C15—C161.6 (3)
O3—S1—O1—Fe164.0 (3)C13—C14—C15—C18178.6 (2)
O4—S1—O1—Fe160.4 (3)C14—C15—C16—C171.7 (4)
N1—C1—C2—C30.9 (5)C15—C16—C17—N30.3 (4)
N2—C7—C8—C90.5 (4)C17—N3—C13—C141.2 (3)
N3—C13—C14—C150.2 (3)C18—C15—C16—C17178.6 (2)
N4—C19—C20—C210.1 (3)C19—N4—C23—C222.2 (3)
C1—N1—C5—C40.1 (3)C19—C20—C21—C221.7 (3)
C1—C2—C3—C40.3 (5)C19—C20—C21—C24177.8 (2)
C1—C2—C3—C6179.7 (4)C20—C21—C22—C231.5 (3)
C2—C3—C4—C51.3 (5)C21—C22—C23—N40.5 (3)
C3—C4—C5—N11.1 (4)C23—N4—C19—C202.0 (3)
C5—N1—C1—C21.1 (4)C24—C21—C22—C23178.0 (2)
C6—C3—C4—C5179.3 (3)
Symmetry codes: (i) x+1, y+1, z+1; (ii) x+1, y, z+3/2.
Hydrogen-bond geometry (Å, º) top
D—H···AD—HH···AD···AD—H···A
C1—H1···O40.932.463.355 (3)163
C5—H5···O3i0.932.433.299 (3)156
C7—H7···S10.932.883.620 (2)138
C7—H7···O40.932.473.381 (3)168
C11—H11···O1i0.932.423.019 (2)122
C13—H13···O20.932.553.059 (2)115
C17—H17···O3ii0.932.593.320 (3)136
C19—H19···O2ii0.932.563.114 (3)119
C23—H23···O20.932.543.094 (2)118
C23—H23···O40.932.593.439 (2)152
Symmetry codes: (i) x+1, y+1, z+1; (ii) x+1, y, z+3/2.
catena-Poly[[tetrakis(4-methylpyridine-κN)cobalt(II)]-sulfato-κ2O:O'] (umd1358_a) top
Crystal data top
[Co(SO4)(C6H7N)4]F(000) = 2200
Mr = 527.49Dx = 1.380 Mg m3
Monoclinic, C2/cMo Kα radiation, λ = 0.71073 Å
a = 11.3904 (10) ÅCell parameters from 9954 reflections
b = 18.7098 (16) Åθ = 3.1–25.7°
c = 24.145 (2) ŵ = 0.80 mm1
β = 99.324 (3)°T = 297 K
V = 5077.6 (8) Å3BLOCK, pink
Z = 80.36 × 0.3 × 0.24 mm
Data collection top
Bruker D8 Venture CMOS
diffractometer
3999 reflections with I > 2σ(I)
φ and ω scansRint = 0.039
Absorption correction: multi-scan
(SADABS; Bruker, 2016)
θmax = 25.8°, θmin = 3.1°
Tmin = 0.518, Tmax = 0.562h = 1313
58263 measured reflectionsk = 2222
4853 independent reflectionsl = 2929
Refinement top
Refinement on F2Hydrogen site location: inferred from neighbouring sites
Least-squares matrix: fullH-atom parameters constrained
R[F2 > 2σ(F2)] = 0.031 w = 1/[σ2(Fo2) + (0.0387P)2 + 6.6062P]
where P = (Fo2 + 2Fc2)/3
wR(F2) = 0.084(Δ/σ)max = 0.002
S = 1.06Δρmax = 0.55 e Å3
4853 reflectionsΔρmin = 0.29 e Å3
314 parametersExtinction correction: SHELXL2014 (Sheldrick, 2015), Fc*=kFc[1+0.001xFc2λ3/sin(2θ)]-1/4
6 restraintsExtinction coefficient: 0.00134 (11)
Primary atom site location: structure-invariant direct methods
Special details top

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 (Å2) top
xyzUiso*/Ueq
Co10.50000.50000.50000.02482 (11)
Co20.50000.46925 (2)0.25000.02267 (11)
S10.65907 (4)0.47838 (3)0.38723 (2)0.02747 (13)
O10.57321 (12)0.48643 (8)0.42671 (6)0.0340 (3)
O20.58914 (14)0.46684 (9)0.33098 (6)0.0402 (4)
O30.72749 (16)0.54361 (11)0.38679 (8)0.0605 (5)
O40.73364 (15)0.41659 (11)0.40208 (7)0.0539 (5)
N10.51127 (16)0.61564 (10)0.49367 (7)0.0345 (4)
N20.32237 (14)0.49777 (9)0.44950 (7)0.0296 (4)
N30.61651 (14)0.55148 (9)0.22427 (7)0.0288 (4)
N40.38306 (14)0.38189 (9)0.26959 (7)0.0294 (4)
C10.5965 (2)0.64537 (13)0.46927 (10)0.0417 (6)
H10.65020.61560.45530.050*
C20.6082 (3)0.71812 (14)0.46383 (12)0.0570 (7)
H20.66980.73630.44700.068*
C30.5299 (3)0.76398 (15)0.48299 (14)0.0728 (9)
C40.4420 (3)0.73299 (15)0.50832 (14)0.0711 (9)
H40.38670.76170.52200.085*
C50.4360 (2)0.66030 (14)0.51334 (11)0.0487 (6)
H50.37690.64100.53120.058*
C60.5409 (5)0.8442 (2)0.4769 (2)0.1310 (19)
H6A0.59040.85450.44930.197*
H6B0.57580.86440.51230.197*
H6C0.46340.86450.46530.197*
C70.2222 (2)0.52253 (13)0.46490 (9)0.0407 (6)
H70.22700.54450.49970.049*
C80.1127 (2)0.51696 (15)0.43170 (10)0.0462 (6)
H80.04580.53530.44430.055*
C90.10114 (19)0.48443 (13)0.38004 (9)0.0386 (5)
C100.20364 (19)0.45862 (13)0.36442 (9)0.0398 (5)
H100.20050.43570.33000.048*
C110.31084 (19)0.46640 (12)0.39919 (9)0.0357 (5)
H110.37890.44900.38710.043*
C120.0170 (2)0.4774 (2)0.34265 (13)0.0703 (9)
H12A0.06910.51470.35120.105*
H12B0.05120.43180.34870.105*
H12C0.00620.48130.30410.105*
C130.72826 (18)0.56053 (13)0.25047 (10)0.0398 (5)
H130.75420.53400.28270.048*
C140.8065 (2)0.60716 (15)0.23192 (11)0.0498 (6)
H140.88340.61150.25170.060*
C150.7721 (2)0.64756 (14)0.18426 (11)0.0473 (6)
C160.6566 (2)0.63943 (13)0.15825 (10)0.0465 (6)
H160.62830.66630.12650.056*
C170.5824 (2)0.59176 (12)0.17893 (9)0.0367 (5)
H170.50460.58740.16030.044*
C180.8571 (3)0.69786 (18)0.16216 (16)0.0785 (10)
H18A0.90360.72270.19290.118*
H18B0.81290.73180.13720.118*
H18C0.90890.67110.14230.118*
C190.27944 (19)0.36630 (12)0.23693 (9)0.0364 (5)
H190.25800.39210.20390.044*
C200.2033 (2)0.31420 (13)0.24978 (10)0.0440 (6)
H200.13220.30580.22580.053*
C210.2319 (2)0.27413 (12)0.29823 (10)0.0410 (5)
C220.3401 (2)0.28864 (13)0.33079 (10)0.0427 (6)
H220.36470.26240.36330.051*
C230.41222 (19)0.34187 (12)0.31547 (9)0.0358 (5)
H230.48490.35030.33830.043*
C240.1476 (3)0.21859 (15)0.31421 (12)0.0604 (8)
H24A0.10860.19480.28100.091*
H24B0.08910.24130.33280.091*
H24C0.19120.18430.33900.091*
Atomic displacement parameters (Å2) top
U11U22U33U12U13U23
Co10.0230 (2)0.0323 (2)0.01965 (19)0.00332 (15)0.00493 (14)0.00122 (15)
Co20.02097 (19)0.0293 (2)0.01818 (19)0.0000.00437 (14)0.000
S10.0219 (2)0.0430 (3)0.0179 (2)0.0022 (2)0.00470 (18)0.0034 (2)
O10.0300 (8)0.0511 (9)0.0232 (7)0.0045 (7)0.0114 (6)0.0013 (6)
O20.0418 (9)0.0573 (10)0.0197 (7)0.0091 (7)0.0004 (6)0.0053 (7)
O30.0550 (11)0.0675 (13)0.0665 (12)0.0288 (9)0.0323 (10)0.0246 (10)
O40.0510 (10)0.0762 (13)0.0357 (9)0.0358 (9)0.0102 (8)0.0066 (9)
N10.0375 (10)0.0366 (10)0.0304 (10)0.0040 (8)0.0082 (8)0.0012 (8)
N20.0278 (9)0.0376 (10)0.0236 (9)0.0035 (7)0.0043 (7)0.0017 (7)
N30.0265 (9)0.0327 (9)0.0274 (9)0.0010 (7)0.0054 (7)0.0014 (7)
N40.0299 (9)0.0325 (9)0.0274 (9)0.0006 (7)0.0097 (7)0.0011 (7)
C10.0470 (14)0.0417 (14)0.0390 (13)0.0039 (11)0.0151 (11)0.0060 (10)
C20.0749 (19)0.0454 (16)0.0568 (17)0.0128 (14)0.0294 (14)0.0019 (13)
C30.108 (3)0.0367 (15)0.083 (2)0.0006 (16)0.043 (2)0.0013 (15)
C40.095 (2)0.0425 (16)0.087 (2)0.0183 (16)0.0480 (19)0.0014 (15)
C50.0561 (15)0.0430 (14)0.0526 (15)0.0107 (12)0.0254 (13)0.0039 (12)
C60.189 (5)0.047 (2)0.178 (5)0.003 (3)0.094 (4)0.010 (2)
C70.0359 (12)0.0581 (15)0.0277 (11)0.0127 (11)0.0037 (9)0.0084 (10)
C80.0308 (12)0.0720 (18)0.0363 (13)0.0163 (11)0.0072 (10)0.0037 (12)
C90.0286 (11)0.0539 (15)0.0327 (12)0.0011 (10)0.0031 (9)0.0033 (10)
C100.0333 (12)0.0569 (15)0.0290 (11)0.0043 (10)0.0042 (9)0.0114 (10)
C110.0264 (11)0.0491 (14)0.0319 (12)0.0022 (9)0.0058 (9)0.0104 (10)
C120.0318 (14)0.126 (3)0.0502 (17)0.0003 (15)0.0022 (12)0.0057 (17)
C130.0277 (11)0.0537 (15)0.0377 (12)0.0029 (10)0.0044 (9)0.0065 (11)
C140.0298 (12)0.0625 (17)0.0574 (16)0.0097 (11)0.0082 (11)0.0049 (13)
C150.0483 (15)0.0452 (14)0.0537 (15)0.0120 (11)0.0245 (12)0.0028 (12)
C160.0638 (16)0.0392 (14)0.0372 (13)0.0069 (12)0.0101 (12)0.0081 (11)
C170.0389 (12)0.0351 (12)0.0346 (12)0.0032 (10)0.0013 (10)0.0010 (10)
C180.077 (2)0.073 (2)0.095 (3)0.0234 (18)0.0439 (19)0.0115 (19)
C190.0365 (12)0.0437 (13)0.0290 (11)0.0068 (10)0.0049 (9)0.0040 (9)
C200.0419 (13)0.0519 (15)0.0383 (13)0.0137 (11)0.0069 (10)0.0015 (11)
C210.0500 (14)0.0356 (13)0.0413 (13)0.0071 (10)0.0186 (11)0.0031 (10)
C220.0527 (15)0.0371 (13)0.0407 (13)0.0027 (11)0.0151 (11)0.0107 (10)
C230.0361 (12)0.0379 (12)0.0340 (12)0.0034 (10)0.0073 (9)0.0043 (10)
C240.0732 (19)0.0528 (17)0.0601 (17)0.0211 (14)0.0253 (15)0.0035 (14)
Geometric parameters (Å, º) top
Co1—O1i2.0903 (13)C7—H70.9300
Co1—O12.0903 (13)C7—C81.373 (3)
Co1—N12.1743 (19)C8—H80.9300
Co1—N1i2.1743 (19)C8—C91.375 (3)
Co1—N22.1869 (17)C9—C101.372 (3)
Co1—N2i2.1869 (17)C9—C121.500 (3)
Co2—O2ii2.0525 (14)C10—H100.9300
Co2—O22.0525 (14)C10—C111.373 (3)
Co2—N32.1866 (17)C11—H110.9300
Co2—N3ii2.1866 (17)C12—H12A0.9600
Co2—N42.2077 (17)C12—H12B0.9600
Co2—N4ii2.2078 (17)C12—H12C0.9600
S1—O11.4799 (14)C13—H130.9300
S1—O21.4748 (15)C13—C141.373 (3)
S1—O31.4490 (18)C14—H140.9300
S1—O41.4449 (17)C14—C151.380 (4)
N1—C11.335 (3)C15—C161.371 (4)
N1—C51.338 (3)C15—C181.508 (3)
N2—C71.339 (3)C16—H160.9300
N2—C111.336 (3)C16—C171.377 (3)
N3—C131.337 (3)C17—H170.9300
N3—C171.334 (3)C18—H18A0.9600
N4—C191.341 (3)C18—H18B0.9600
N4—C231.334 (3)C18—H18C0.9600
C1—H10.9300C19—H190.9300
C1—C21.376 (4)C19—C201.373 (3)
C2—H20.9300C20—H200.9300
C2—C31.371 (4)C20—C211.383 (3)
C3—C41.382 (4)C21—C221.377 (3)
C3—C61.515 (5)C21—C241.507 (3)
C4—H40.9300C22—H220.9300
C4—C51.368 (4)C22—C231.379 (3)
C5—H50.9300C23—H230.9300
C6—H6A0.9600C24—H24A0.9600
C6—H6B0.9600C24—H24B0.9600
C6—H6C0.9600C24—H24C0.9600
O1i—Co1—O1180.00 (3)C3—C6—H6C109.5
O1i—Co1—N188.56 (6)H6A—C6—H6B109.5
O1i—Co1—N1i91.44 (6)H6A—C6—H6C109.5
O1—Co1—N191.44 (6)H6B—C6—H6C109.5
O1—Co1—N1i88.56 (6)N2—C7—H7118.4
O1i—Co1—N2i89.18 (6)N2—C7—C8123.1 (2)
O1—Co1—N289.18 (6)C8—C7—H7118.4
O1i—Co1—N290.82 (6)C7—C8—H8119.8
O1—Co1—N2i90.82 (6)C7—C8—C9120.5 (2)
N1i—Co1—N1180.0C9—C8—H8119.8
N1i—Co1—N287.73 (7)C8—C9—C12122.0 (2)
N1—Co1—N2i87.73 (7)C10—C9—C8116.4 (2)
N1—Co1—N292.27 (7)C10—C9—C12121.6 (2)
N1i—Co1—N2i92.27 (7)C9—C10—H10119.8
N2i—Co1—N2180.0C9—C10—C11120.5 (2)
O2ii—Co2—O2177.48 (10)C11—C10—H10119.8
O2ii—Co2—N3ii93.26 (6)N2—C11—C10123.3 (2)
O2ii—Co2—N388.52 (6)N2—C11—H11118.3
O2—Co2—N3ii88.52 (6)C10—C11—H11118.3
O2—Co2—N393.26 (6)C9—C12—H12A109.5
O2—Co2—N490.12 (7)C9—C12—H12B109.5
O2—Co2—N4ii88.01 (6)C9—C12—H12C109.5
O2ii—Co2—N4ii90.12 (7)H12A—C12—H12B109.5
O2ii—Co2—N488.01 (6)H12A—C12—H12C109.5
N3ii—Co2—N390.57 (9)H12B—C12—H12C109.5
N3ii—Co2—N492.58 (6)N3—C13—H13118.5
N3ii—Co2—N4ii175.44 (6)N3—C13—C14123.0 (2)
N3—Co2—N4ii92.58 (6)C14—C13—H13118.5
N3—Co2—N4175.43 (6)C13—C14—H14119.7
N4—Co2—N4ii84.47 (9)C13—C14—C15120.5 (2)
O2—S1—O1107.06 (9)C15—C14—H14119.7
O3—S1—O1109.36 (10)C14—C15—C18121.7 (3)
O3—S1—O2109.11 (11)C16—C15—C14116.3 (2)
O4—S1—O1110.17 (9)C16—C15—C18122.0 (3)
O4—S1—O2108.63 (10)C15—C16—H16119.8
O4—S1—O3112.36 (12)C15—C16—C17120.4 (2)
S1—O1—Co1162.48 (10)C17—C16—H16119.8
S1—O2—Co2169.75 (12)N3—C17—C16123.3 (2)
C1—N1—Co1120.06 (15)N3—C17—H17118.3
C1—N1—C5116.7 (2)C16—C17—H17118.3
C5—N1—Co1123.22 (16)C15—C18—H18A109.5
C7—N2—Co1126.28 (14)C15—C18—H18B109.5
C11—N2—Co1117.45 (13)C15—C18—H18C109.5
C11—N2—C7116.22 (18)H18A—C18—H18B109.5
C13—N3—Co2121.99 (15)H18A—C18—H18C109.5
C17—N3—Co2121.42 (14)H18B—C18—H18C109.5
C17—N3—C13116.42 (19)N4—C19—H19118.3
C19—N4—Co2122.63 (14)N4—C19—C20123.3 (2)
C23—N4—Co2121.05 (14)C20—C19—H19118.3
C23—N4—C19116.32 (18)C19—C20—H20119.8
N1—C1—H1118.6C19—C20—C21120.3 (2)
N1—C1—C2122.9 (2)C21—C20—H20119.8
C2—C1—H1118.6C20—C21—C24121.2 (2)
C1—C2—H2119.7C22—C21—C20116.3 (2)
C3—C2—C1120.5 (3)C22—C21—C24122.6 (2)
C3—C2—H2119.7C21—C22—H22119.8
C2—C3—C4116.4 (3)C21—C22—C23120.4 (2)
C2—C3—C6121.2 (3)C23—C22—H22119.8
C4—C3—C6122.4 (3)N4—C23—C22123.3 (2)
C3—C4—H4119.8N4—C23—H23118.3
C5—C4—C3120.4 (3)C22—C23—H23118.3
C5—C4—H4119.8C21—C24—H24A109.5
N1—C5—C4123.0 (2)C21—C24—H24B109.5
N1—C5—H5118.5C21—C24—H24C109.5
C4—C5—H5118.5H24A—C24—H24B109.5
C3—C6—H6A109.5H24A—C24—H24C109.5
C3—C6—H6B109.5H24B—C24—H24C109.5
Co1—N1—C1—C2179.9 (2)C5—N1—C1—C20.2 (4)
Co1—N1—C5—C4178.7 (2)C6—C3—C4—C5179.4 (4)
Co1—N2—C7—C8177.52 (19)C7—N2—C11—C100.5 (3)
Co1—N2—C11—C10177.07 (19)C7—C8—C9—C100.0 (4)
Co2—N3—C13—C14173.74 (19)C7—C8—C9—C12180.0 (3)
Co2—N3—C17—C16173.79 (18)C8—C9—C10—C110.7 (4)
Co2—N4—C19—C20177.09 (18)C9—C10—C11—N21.0 (4)
Co2—N4—C23—C22177.27 (17)C11—N2—C7—C80.2 (4)
O1—S1—O2—Co2105.8 (6)C12—C9—C10—C11179.3 (3)
O2—S1—O1—Co1177.7 (3)C13—N3—C17—C161.5 (3)
O3—S1—O1—Co164.3 (4)C13—C14—C15—C161.5 (4)
O3—S1—O2—Co212.5 (6)C13—C14—C15—C18178.5 (3)
O4—S1—O1—Co159.7 (4)C14—C15—C16—C171.5 (4)
O4—S1—O2—Co2135.3 (6)C15—C16—C17—N30.0 (4)
N1—C1—C2—C31.0 (4)C17—N3—C13—C141.5 (3)
N2—C7—C8—C90.4 (4)C18—C15—C16—C17178.5 (3)
N3—C13—C14—C150.0 (4)C19—N4—C23—C222.2 (3)
N4—C19—C20—C210.5 (4)C19—C20—C21—C221.5 (3)
C1—N1—C5—C41.4 (4)C19—C20—C21—C24177.7 (2)
C1—C2—C3—C41.1 (5)C20—C21—C22—C231.7 (3)
C1—C2—C3—C6179.5 (4)C21—C22—C23—N40.2 (4)
C2—C3—C4—C50.0 (5)C23—N4—C19—C202.4 (3)
C3—C4—C5—N11.3 (5)C24—C21—C22—C23177.5 (2)
Symmetry codes: (i) x+1, y+1, z+1; (ii) x+1, y, z+1/2.
Hydrogen-bond geometry (Å, º) top
D—H···AD—HH···AD···AD—H···A
C1—H1···O30.932.413.284 (3)157
C5—H5···O4i0.932.453.355 (3)165
C7—H7···S1i0.932.863.607 (2)138
C7—H7···O4i0.932.453.368 (3)169
C11—H11···O10.932.372.978 (3)123
C13—H13···O30.932.593.308 (3)135
C17—H17···S1ii0.932.873.632 (2)140
C17—H17···O2ii0.932.523.031 (3)115
C19—H19···O2ii0.932.483.044 (3)119
C23—H23···O20.932.503.070 (3)120
Symmetry codes: (i) x+1, y+1, z+1; (ii) x+1, y, z+1/2.
catena-Poly[[tetrakis(4-methylpyridine-κN)nickel(II)]-sulfato-κ2O:O'] (umd1307) top
Crystal data top
[Ni(SO4)(C6H7N)4]F(000) = 2208
Mr = 527.27Dx = 1.394 Mg m3
Monoclinic, C2/cMo Kα radiation, λ = 0.71073 Å
a = 11.3610 (17) ÅCell parameters from 9925 reflections
b = 18.546 (3) Åθ = 3.1–25.7°
c = 24.178 (4) ŵ = 0.89 mm1
β = 99.459 (5)°T = 297 K
V = 5025.1 (13) Å3PRISM, green
Z = 80.25 × 0.19 × 0.12 mm
Data collection top
Bruker D8 Venture CMOS
diffractometer
4037 reflections with I > 2σ(I)
φ and ω scansRint = 0.044
Absorption correction: multi-scan
(SADABS; Bruker, 2016)
θmax = 25.7°, θmin = 2.9°
Tmin = 0.289, Tmax = 0.332h = 1313
62062 measured reflectionsk = 2222
4798 independent reflectionsl = 2929
Refinement top
Refinement on F2Hydrogen site location: inferred from neighbouring sites
Least-squares matrix: fullH-atom parameters constrained
R[F2 > 2σ(F2)] = 0.029 w = 1/[σ2(Fo2) + (0.0338P)2 + 6.8591P]
where P = (Fo2 + 2Fc2)/3
wR(F2) = 0.077(Δ/σ)max = 0.001
S = 1.05Δρmax = 0.53 e Å3
4798 reflectionsΔρmin = 0.29 e Å3
314 parametersExtinction correction: SHELXL2014 (Sheldrick, 2015), Fc*=kFc[1+0.001xFc2λ3/sin(2θ)]-1/4
0 restraintsExtinction coefficient: 0.00116 (10)
Primary atom site location: structure-invariant direct methods
Special details top

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 (Å2) top
xyzUiso*/Ueq
Ni10.50000.50000.50000.02536 (11)
Ni20.50000.46852 (2)0.75000.02357 (10)
S10.34019 (4)0.47765 (3)0.61271 (2)0.02773 (13)
O10.42614 (12)0.48641 (8)0.57336 (6)0.0335 (3)
O20.40988 (14)0.46594 (9)0.66890 (6)0.0414 (4)
O30.27061 (16)0.54326 (10)0.61312 (8)0.0602 (5)
O40.26541 (15)0.41507 (10)0.59764 (6)0.0519 (5)
N10.48860 (15)0.61365 (9)0.50649 (7)0.0334 (4)
N20.67325 (14)0.49832 (9)0.54977 (7)0.0299 (4)
N30.38519 (14)0.38311 (9)0.76961 (7)0.0300 (4)
N40.61420 (14)0.54921 (9)0.72508 (7)0.0288 (4)
C10.5636 (2)0.65898 (13)0.48683 (10)0.0480 (6)
H10.62310.63980.46900.058*
C20.5565 (3)0.73261 (15)0.49175 (13)0.0664 (8)
H20.61130.76190.47780.080*
C30.4685 (3)0.76356 (14)0.51732 (13)0.0640 (8)
C40.3904 (2)0.71672 (14)0.53641 (11)0.0528 (6)
H40.32850.73480.55310.063*
C50.4031 (2)0.64333 (12)0.53101 (9)0.0401 (5)
H50.34970.61310.54500.048*
C60.4574 (4)0.84444 (18)0.5235 (2)0.1170 (17)
H6A0.40790.85470.55110.176*
H6B0.42220.86490.48820.176*
H6C0.53510.86490.53510.176*
C70.7735 (2)0.52382 (14)0.53425 (9)0.0426 (6)
H70.76830.54600.49940.051*
C80.8838 (2)0.51860 (15)0.56761 (10)0.0482 (6)
H80.95030.53790.55520.058*
C90.89660 (19)0.48533 (13)0.61890 (9)0.0406 (5)
C100.79391 (19)0.45863 (13)0.63449 (9)0.0403 (5)
H100.79750.43530.66880.048*
C110.68613 (18)0.46613 (12)0.59981 (9)0.0351 (5)
H110.61840.44780.61180.042*
C121.0162 (2)0.4780 (2)0.65665 (13)0.0706 (9)
H12A1.06910.51500.64780.106*
H12B1.04970.43160.65110.106*
H12C1.00570.48270.69510.106*
C130.41554 (19)0.34230 (12)0.81550 (9)0.0369 (5)
H130.48870.35060.83820.044*
C140.3429 (2)0.28850 (12)0.83055 (10)0.0436 (5)
H140.36790.26170.86280.052*
C150.2339 (2)0.27407 (12)0.79831 (10)0.0425 (5)
C160.2046 (2)0.31492 (13)0.75013 (10)0.0445 (6)
H160.13290.30670.72630.053*
C170.28103 (19)0.36763 (12)0.73722 (9)0.0372 (5)
H170.25920.39380.70430.045*
C180.1496 (3)0.21803 (15)0.81438 (12)0.0628 (8)
H18A0.19370.18320.83890.094*
H18B0.10980.19430.78120.094*
H18C0.09150.24090.83320.094*
C190.57846 (19)0.59043 (12)0.68007 (9)0.0365 (5)
H190.50000.58640.66190.044*
C200.6525 (2)0.63862 (13)0.65933 (10)0.0450 (6)
H200.62330.66610.62790.054*
C210.7689 (2)0.64654 (13)0.68459 (10)0.0460 (6)
C220.8049 (2)0.60531 (14)0.73190 (11)0.0496 (6)
H220.88250.60950.75120.060*
C230.72652 (18)0.55802 (13)0.75068 (9)0.0393 (5)
H230.75320.53100.78270.047*
C240.8539 (3)0.69725 (18)0.66225 (15)0.0769 (9)
H24A0.80920.73290.63880.115*
H24B0.90290.67050.64080.115*
H24C0.90350.72070.69300.115*
Atomic displacement parameters (Å2) top
U11U22U33U12U13U23
Ni10.02605 (19)0.0310 (2)0.01982 (17)0.00419 (14)0.00613 (13)0.00076 (14)
Ni20.02264 (18)0.0295 (2)0.01939 (17)0.0000.00592 (13)0.000
S10.0242 (2)0.0410 (3)0.0189 (2)0.0030 (2)0.00638 (18)0.00281 (19)
O10.0305 (7)0.0491 (9)0.0233 (7)0.0041 (6)0.0120 (6)0.0016 (6)
O20.0447 (9)0.0575 (10)0.0203 (7)0.0109 (7)0.0003 (6)0.0057 (6)
O30.0561 (11)0.0625 (12)0.0703 (12)0.0262 (9)0.0347 (9)0.0239 (10)
O40.0513 (10)0.0692 (12)0.0363 (9)0.0343 (9)0.0103 (7)0.0053 (8)
N10.0380 (10)0.0358 (10)0.0274 (9)0.0045 (8)0.0080 (7)0.0007 (7)
N20.0303 (9)0.0363 (9)0.0237 (8)0.0044 (7)0.0063 (7)0.0000 (7)
N30.0312 (9)0.0333 (9)0.0275 (8)0.0010 (7)0.0109 (7)0.0012 (7)
N40.0274 (8)0.0322 (9)0.0274 (8)0.0005 (7)0.0066 (7)0.0019 (7)
C10.0565 (15)0.0409 (13)0.0527 (14)0.0096 (11)0.0272 (12)0.0030 (11)
C20.088 (2)0.0405 (14)0.081 (2)0.0174 (14)0.0443 (17)0.0010 (14)
C30.095 (2)0.0347 (14)0.0683 (18)0.0012 (14)0.0320 (17)0.0005 (13)
C40.0682 (17)0.0431 (14)0.0522 (15)0.0121 (12)0.0248 (13)0.0024 (11)
C50.0431 (12)0.0412 (13)0.0378 (12)0.0015 (10)0.0126 (10)0.0053 (10)
C60.168 (4)0.0375 (17)0.166 (4)0.002 (2)0.087 (4)0.008 (2)
C70.0413 (13)0.0602 (15)0.0267 (11)0.0148 (11)0.0064 (9)0.0049 (10)
C80.0338 (12)0.0726 (17)0.0394 (13)0.0201 (12)0.0098 (10)0.0004 (12)
C90.0299 (11)0.0570 (15)0.0347 (12)0.0019 (10)0.0048 (9)0.0059 (10)
C100.0333 (11)0.0581 (15)0.0299 (11)0.0037 (10)0.0060 (9)0.0090 (10)
C110.0275 (10)0.0476 (13)0.0308 (11)0.0019 (9)0.0068 (8)0.0084 (9)
C120.0308 (13)0.121 (3)0.0581 (18)0.0025 (15)0.0028 (12)0.0044 (17)
C130.0388 (12)0.0383 (12)0.0350 (11)0.0057 (9)0.0100 (9)0.0056 (9)
C140.0571 (15)0.0367 (12)0.0403 (13)0.0051 (11)0.0180 (11)0.0110 (10)
C150.0560 (14)0.0352 (12)0.0413 (13)0.0092 (10)0.0225 (11)0.0050 (10)
C160.0444 (13)0.0507 (14)0.0393 (12)0.0146 (11)0.0096 (10)0.0013 (11)
C170.0389 (12)0.0432 (13)0.0301 (11)0.0060 (10)0.0073 (9)0.0038 (9)
C180.081 (2)0.0537 (16)0.0601 (17)0.0204 (15)0.0295 (15)0.0030 (13)
C190.0380 (12)0.0347 (12)0.0353 (11)0.0024 (9)0.0017 (9)0.0008 (9)
C200.0606 (15)0.0385 (13)0.0368 (12)0.0052 (11)0.0106 (11)0.0053 (10)
C210.0497 (14)0.0419 (13)0.0522 (14)0.0115 (11)0.0254 (12)0.0024 (11)
C220.0311 (12)0.0606 (16)0.0582 (15)0.0091 (11)0.0102 (11)0.0040 (13)
C230.0296 (11)0.0516 (14)0.0368 (11)0.0036 (10)0.0058 (9)0.0065 (10)
C240.078 (2)0.072 (2)0.090 (2)0.0243 (17)0.0430 (19)0.0097 (17)
Geometric parameters (Å, º) top
Ni1—O1i2.0984 (13)C7—H70.9300
Ni1—O12.0984 (13)C7—C81.377 (3)
Ni1—N12.1191 (18)C8—H80.9300
Ni1—N1i2.1190 (18)C8—C91.371 (3)
Ni1—N22.1318 (16)C9—C101.376 (3)
Ni1—N2i2.1318 (16)C9—C121.513 (3)
Ni2—O2ii2.0581 (14)C10—H100.9300
Ni2—O22.0581 (14)C10—C111.373 (3)
Ni2—N32.1537 (17)C11—H110.9300
Ni2—N3ii2.1537 (17)C12—H12A0.9600
Ni2—N4ii2.1313 (16)C12—H12B0.9600
Ni2—N42.1313 (17)C12—H12C0.9600
S1—O11.4800 (13)C13—H130.9300
S1—O21.4719 (15)C13—C141.381 (3)
S1—O31.4520 (18)C14—H140.9300
S1—O41.4491 (16)C14—C151.377 (3)
N1—C11.338 (3)C15—C161.384 (3)
N1—C51.337 (3)C15—C181.507 (3)
N2—C71.342 (3)C16—H160.9300
N2—C111.335 (3)C16—C171.377 (3)
N3—C131.341 (3)C17—H170.9300
N3—C171.338 (3)C18—H18A0.9600
N4—C191.337 (3)C18—H18B0.9600
N4—C231.334 (3)C18—H18C0.9600
C1—H10.9300C19—H190.9300
C1—C21.374 (4)C19—C201.377 (3)
C2—H20.9300C20—H200.9300
C2—C31.384 (4)C20—C211.370 (3)
C3—C41.374 (4)C21—C221.381 (4)
C3—C61.515 (4)C21—C241.510 (3)
C4—H40.9300C22—H220.9300
C4—C51.377 (3)C22—C231.379 (3)
C5—H50.9300C23—H230.9300
C6—H6A0.9600C24—H24A0.9600
C6—H6B0.9600C24—H24B0.9600
C6—H6C0.9600C24—H24C0.9600
O1i—Ni1—O1180.0C3—C6—H6C109.5
O1—Ni1—N191.10 (6)H6A—C6—H6B109.5
O1i—Ni1—N188.90 (6)H6A—C6—H6C109.5
O1—Ni1—N1i88.90 (6)H6B—C6—H6C109.5
O1i—Ni1—N1i91.10 (6)N2—C7—H7118.5
O1i—Ni1—N2i88.94 (6)N2—C7—C8122.9 (2)
O1i—Ni1—N291.06 (6)C8—C7—H7118.5
O1—Ni1—N2i91.06 (6)C7—C8—H8119.6
O1—Ni1—N288.94 (6)C9—C8—C7120.8 (2)
N1i—Ni1—N1180.00 (9)C9—C8—H8119.6
N1—Ni1—N291.99 (7)C8—C9—C10116.2 (2)
N1i—Ni1—N2i91.99 (7)C8—C9—C12122.5 (2)
N1i—Ni1—N288.01 (7)C10—C9—C12121.3 (2)
N1—Ni1—N2i88.01 (7)C9—C10—H10119.7
N2i—Ni1—N2180.0C11—C10—C9120.5 (2)
O2ii—Ni2—O2177.34 (9)C11—C10—H10119.7
O2ii—Ni2—N3ii88.18 (6)N2—C11—C10123.55 (19)
O2ii—Ni2—N389.86 (7)N2—C11—H11118.2
O2—Ni2—N388.18 (6)C10—C11—H11118.2
O2—Ni2—N3ii89.86 (7)C9—C12—H12A109.5
O2ii—Ni2—N4ii88.72 (6)C9—C12—H12B109.5
O2—Ni2—N488.72 (6)C9—C12—H12C109.5
O2ii—Ni2—N493.16 (6)H12A—C12—H12B109.5
O2—Ni2—N4ii93.15 (6)H12A—C12—H12C109.5
N3ii—Ni2—N385.30 (9)H12B—C12—H12C109.5
N4—Ni2—N3ii92.02 (6)N3—C13—H13118.6
N4ii—Ni2—N3ii175.91 (6)N3—C13—C14122.8 (2)
N4—Ni2—N3175.91 (6)C14—C13—H13118.6
N4ii—Ni2—N392.02 (6)C13—C14—H14119.6
N4ii—Ni2—N490.81 (9)C15—C14—C13120.8 (2)
O2—S1—O1107.33 (9)C15—C14—H14119.6
O3—S1—O1109.26 (9)C14—C15—C16116.1 (2)
O3—S1—O2109.15 (11)C14—C15—C18122.6 (2)
O4—S1—O1110.35 (9)C16—C15—C18121.3 (2)
O4—S1—O2108.55 (10)C15—C16—H16119.8
O4—S1—O3112.06 (12)C17—C16—C15120.4 (2)
S1—O1—Ni1162.62 (9)C17—C16—H16119.8
S1—O2—Ni2169.73 (12)N3—C17—C16123.3 (2)
C1—N1—Ni1123.25 (15)N3—C17—H17118.3
C5—N1—Ni1119.99 (14)C16—C17—H17118.3
C5—N1—C1116.8 (2)C15—C18—H18A109.5
C7—N2—Ni1125.74 (14)C15—C18—H18B109.5
C11—N2—Ni1118.13 (13)C15—C18—H18C109.5
C11—N2—C7116.04 (18)H18A—C18—H18B109.5
C13—N3—Ni2120.98 (14)H18A—C18—H18C109.5
C17—N3—Ni2122.56 (14)H18B—C18—H18C109.5
C17—N3—C13116.46 (18)N4—C19—H19118.5
C19—N4—Ni2120.92 (14)N4—C19—C20123.0 (2)
C23—N4—Ni2122.36 (14)C20—C19—H19118.5
C23—N4—C19116.56 (18)C19—C20—H20119.7
N1—C1—H1118.5C21—C20—C19120.7 (2)
N1—C1—C2123.0 (2)C21—C20—H20119.7
C2—C1—H1118.5C20—C21—C22116.2 (2)
C1—C2—H2119.8C20—C21—C24122.3 (2)
C1—C2—C3120.5 (2)C22—C21—C24121.5 (2)
C3—C2—H2119.8C21—C22—H22119.8
C2—C3—C6122.2 (3)C23—C22—C21120.4 (2)
C4—C3—C2116.2 (2)C23—C22—H22119.8
C4—C3—C6121.6 (3)N4—C23—C22123.1 (2)
C3—C4—H4119.7N4—C23—H23118.5
C3—C4—C5120.7 (2)C22—C23—H23118.5
C5—C4—H4119.7C21—C24—H24A109.5
N1—C5—C4122.9 (2)C21—C24—H24B109.5
N1—C5—H5118.5C21—C24—H24C109.5
C4—C5—H5118.5H24A—C24—H24B109.5
C3—C6—H6A109.5H24A—C24—H24C109.5
C3—C6—H6B109.5H24B—C24—H24C109.5
Ni1—N1—C1—C2179.2 (2)C5—N1—C1—C21.0 (4)
Ni1—N1—C5—C4179.76 (19)C6—C3—C4—C5179.2 (3)
Ni1—N2—C7—C8177.41 (19)C7—N2—C11—C100.1 (3)
Ni1—N2—C11—C10176.88 (18)C7—C8—C9—C100.4 (4)
Ni2—N3—C13—C14177.94 (16)C7—C8—C9—C12179.6 (3)
Ni2—N3—C17—C16177.65 (17)C8—C9—C10—C110.3 (4)
Ni2—N4—C19—C20173.89 (17)C9—C10—C11—N20.5 (4)
Ni2—N4—C23—C22173.78 (19)C11—N2—C7—C80.9 (3)
O1—S1—O2—Ni2103.4 (6)C12—C9—C10—C11179.7 (2)
O2—S1—O1—Ni1176.0 (3)C13—N3—C17—C162.5 (3)
O3—S1—O1—Ni165.7 (4)C13—C14—C15—C161.7 (3)
O3—S1—O2—Ni215.0 (6)C13—C14—C15—C18177.4 (2)
O4—S1—O1—Ni157.9 (4)C14—C15—C16—C171.5 (3)
O4—S1—O2—Ni2137.4 (5)C15—C16—C17—N30.7 (4)
N1—C1—C2—C30.8 (5)C17—N3—C13—C142.2 (3)
N2—C7—C8—C91.1 (4)C18—C15—C16—C17177.7 (2)
N3—C13—C14—C150.1 (3)C19—N4—C23—C221.7 (3)
N4—C19—C20—C210.0 (4)C19—C20—C21—C221.6 (4)
C1—N1—C5—C40.0 (3)C19—C20—C21—C24178.3 (2)
C1—C2—C3—C40.5 (5)C20—C21—C22—C231.6 (4)
C1—C2—C3—C6179.9 (3)C21—C22—C23—N40.1 (4)
C2—C3—C4—C51.5 (4)C23—N4—C19—C201.7 (3)
C3—C4—C5—N11.3 (4)C24—C21—C22—C23178.4 (3)
Symmetry codes: (i) x+1, y+1, z+1; (ii) x+1, y, z+3/2.
Hydrogen-bond geometry (Å, º) top
D—H···AD—HH···AD···AD—H···A
C1—H1···O1i0.932.583.075 (3)114
C1—H1···O4i0.932.433.337 (3)165
C5—H5···O10.932.563.082 (3)116
C5—H5···O30.932.383.261 (3)157
C7—H7···S1i0.932.823.576 (2)139
C7—H7···O4i0.932.433.345 (3)170
C11—H11···O10.932.342.942 (2)122
C13—H13···O2ii0.932.453.015 (3)119
C17—H17···O20.932.442.999 (3)119
C19—H19···S10.932.843.593 (2)139
C19—H19···O20.932.472.984 (3)115
C23—H23···O3ii0.932.593.299 (3)134
Symmetry codes: (i) x+1, y+1, z+1; (ii) x+1, y, z+3/2.
Di-µ-sulfato-κ4O:O-bis[tris(4-methylpyridine-κN)copper(II)] (umd1301_a) top
Crystal data top
[Cu2(SO4)2(C6H7N)6]F(000) = 908
Mr = 877.95Dx = 1.546 Mg m3
Monoclinic, P21/cMo Kα radiation, λ = 0.71073 Å
a = 9.1304 (8) ÅCell parameters from 9831 reflections
b = 21.2148 (19) Åθ = 2.9–25.7°
c = 9.9359 (8) ŵ = 1.30 mm1
β = 101.544 (3)°T = 200 K
V = 1885.6 (3) Å3BLOCK, blue
Z = 20.28 × 0.14 × 0.11 mm
Data collection top
Bruker D8 Venture CMOS
diffractometer
3110 reflections with I > 2σ(I)
φ and ω scansRint = 0.053
Absorption correction: multi-scan
(SADABS; Bruker, 2016)
θmax = 25.7°, θmin = 3.4°
Tmin = 0.380, Tmax = 0.429h = 1111
59469 measured reflectionsk = 2525
3580 independent reflectionsl = 1212
Refinement top
Refinement on F2Hydrogen site location: inferred from neighbouring sites
Least-squares matrix: fullH-atom parameters constrained
R[F2 > 2σ(F2)] = 0.027 w = 1/[σ2(Fo2) + (0.0237P)2 + 2.015P]
where P = (Fo2 + 2Fc2)/3
wR(F2) = 0.065(Δ/σ)max = 0.003
S = 1.06Δρmax = 0.27 e Å3
3580 reflectionsΔρmin = 0.31 e Å3
248 parametersExtinction correction: SHELXL2014 (Sheldrick, 2015), Fc*=kFc[1+0.001xFc2λ3/sin(2θ)]-1/4
0 restraintsExtinction coefficient: 0.0044 (5)
Primary atom site location: structure-invariant direct methods
Special details top

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 (Å2) top
xyzUiso*/Ueq
Cu10.34858 (3)0.54221 (2)0.48079 (2)0.01881 (10)
S10.30849 (6)0.42609 (2)0.63867 (5)0.02033 (13)
O10.42042 (15)0.46049 (7)0.56673 (14)0.0193 (3)
O20.2810 (2)0.36429 (8)0.57543 (19)0.0404 (4)
O30.37729 (18)0.42162 (8)0.78368 (15)0.0336 (4)
O40.17490 (17)0.46582 (8)0.61602 (16)0.0309 (4)
N10.41898 (19)0.59060 (8)0.65957 (17)0.0213 (4)
N20.25128 (19)0.62219 (8)0.39875 (17)0.0220 (4)
N30.25106 (19)0.49886 (8)0.30406 (17)0.0199 (4)
C10.5258 (2)0.63458 (10)0.6657 (2)0.0245 (5)
H10.57090.64030.58830.029*
C20.5725 (3)0.67179 (10)0.7800 (2)0.0261 (5)
H20.64780.70270.77950.031*
C30.5105 (3)0.66455 (10)0.8957 (2)0.0268 (5)
C40.4017 (3)0.61830 (11)0.8888 (2)0.0304 (5)
H40.35640.61110.96560.037*
C50.3590 (2)0.58275 (10)0.7717 (2)0.0257 (5)
H50.28430.55140.76990.031*
C60.5586 (3)0.70482 (12)1.0209 (2)0.0409 (6)
H6A0.47060.72441.04600.061*
H6B0.62670.73771.00130.061*
H6C0.60990.67861.09710.061*
C70.3149 (3)0.66404 (11)0.3272 (2)0.0292 (5)
H70.41510.65720.31750.035*
C80.2403 (3)0.71650 (11)0.2672 (2)0.0319 (5)
H80.28930.74500.21720.038*
C90.0942 (3)0.72788 (10)0.2794 (2)0.0276 (5)
C100.0286 (2)0.68434 (11)0.3534 (2)0.0269 (5)
H100.07130.69020.36490.032*
C110.1090 (2)0.63269 (10)0.4097 (2)0.0256 (5)
H110.06180.60300.45870.031*
C120.0077 (3)0.78367 (13)0.2126 (3)0.0501 (7)
H12A0.07710.81490.18840.075*
H12B0.04880.80250.27650.075*
H12C0.06160.77000.12930.075*
C130.1195 (2)0.46930 (10)0.2929 (2)0.0245 (5)
H130.07170.46920.36950.029*
C140.0515 (2)0.43909 (11)0.1740 (2)0.0270 (5)
H140.04260.41920.16940.032*
C150.1192 (2)0.43750 (10)0.0612 (2)0.0236 (5)
C160.2530 (2)0.46990 (10)0.0720 (2)0.0245 (5)
H160.30200.47130.00380.029*
C170.3146 (2)0.50015 (10)0.1932 (2)0.0225 (4)
H170.40540.52280.19840.027*
C180.0528 (3)0.40159 (12)0.0668 (2)0.0364 (6)
H18A0.09200.41840.14450.055*
H18B0.05620.40610.08550.055*
H18C0.07930.35690.05410.055*
Atomic displacement parameters (Å2) top
U11U22U33U12U13U23
Cu10.01960 (14)0.02127 (15)0.01567 (14)0.00091 (10)0.00378 (9)0.00101 (10)
S10.0188 (3)0.0233 (3)0.0215 (3)0.0043 (2)0.0102 (2)0.0006 (2)
O10.0173 (7)0.0230 (7)0.0193 (7)0.0034 (6)0.0077 (6)0.0030 (6)
O20.0462 (10)0.0296 (9)0.0547 (11)0.0177 (8)0.0322 (9)0.0132 (8)
O30.0314 (9)0.0492 (11)0.0219 (8)0.0029 (8)0.0091 (7)0.0118 (7)
O40.0186 (8)0.0425 (10)0.0329 (9)0.0013 (7)0.0086 (7)0.0002 (7)
N10.0229 (9)0.0223 (9)0.0192 (9)0.0017 (7)0.0051 (7)0.0010 (7)
N20.0213 (9)0.0234 (9)0.0210 (9)0.0024 (7)0.0034 (7)0.0016 (7)
N30.0200 (9)0.0217 (9)0.0178 (8)0.0001 (7)0.0032 (7)0.0005 (7)
C10.0272 (11)0.0261 (11)0.0217 (11)0.0009 (9)0.0089 (9)0.0000 (9)
C20.0285 (12)0.0236 (11)0.0263 (11)0.0032 (9)0.0058 (9)0.0005 (9)
C30.0381 (13)0.0207 (11)0.0206 (11)0.0049 (10)0.0037 (9)0.0013 (9)
C40.0429 (14)0.0293 (12)0.0235 (11)0.0005 (11)0.0175 (10)0.0016 (9)
C50.0280 (12)0.0258 (12)0.0262 (11)0.0026 (9)0.0121 (9)0.0023 (9)
C60.0651 (18)0.0314 (14)0.0252 (12)0.0027 (13)0.0069 (12)0.0064 (11)
C70.0233 (11)0.0326 (13)0.0334 (12)0.0029 (10)0.0096 (10)0.0005 (10)
C80.0328 (13)0.0282 (12)0.0365 (13)0.0069 (10)0.0109 (10)0.0056 (10)
C90.0324 (12)0.0218 (11)0.0282 (12)0.0013 (10)0.0048 (10)0.0036 (9)
C100.0220 (11)0.0298 (12)0.0297 (12)0.0013 (9)0.0071 (9)0.0044 (10)
C110.0263 (11)0.0254 (11)0.0261 (11)0.0053 (9)0.0077 (9)0.0008 (9)
C120.0527 (17)0.0364 (15)0.0621 (19)0.0109 (13)0.0135 (15)0.0147 (14)
C130.0227 (11)0.0292 (12)0.0228 (11)0.0013 (9)0.0069 (9)0.0004 (9)
C140.0218 (11)0.0277 (12)0.0312 (12)0.0065 (9)0.0043 (9)0.0021 (10)
C150.0259 (11)0.0210 (11)0.0217 (11)0.0029 (9)0.0003 (9)0.0012 (9)
C160.0257 (11)0.0308 (12)0.0171 (10)0.0020 (9)0.0049 (9)0.0001 (9)
C170.0209 (10)0.0260 (11)0.0205 (10)0.0009 (9)0.0041 (8)0.0035 (9)
C180.0399 (14)0.0375 (14)0.0287 (13)0.0038 (11)0.0004 (11)0.0097 (11)
Geometric parameters (Å, º) top
Cu1—O11.9853 (14)C6—H6B0.9800
Cu1—O1i2.2525 (14)C6—H6C0.9800
Cu1—N12.0408 (17)C7—H70.9500
Cu1—N22.0106 (18)C7—C81.377 (3)
Cu1—N32.0240 (17)C8—H80.9500
S1—O11.5428 (14)C8—C91.385 (3)
S1—O21.4538 (17)C9—C101.388 (3)
S1—O31.4551 (16)C9—C121.502 (3)
S1—O41.4625 (16)C10—H100.9500
O1—Cu1i2.2525 (14)C10—C111.374 (3)
N1—C11.342 (3)C11—H110.9500
N1—C51.346 (3)C12—H12A0.9800
N2—C71.340 (3)C12—H12B0.9800
N2—C111.344 (3)C12—H12C0.9800
N3—C131.340 (3)C13—H130.9500
N3—C171.344 (3)C13—C141.378 (3)
C1—H10.9500C14—H140.9500
C1—C21.378 (3)C14—C151.385 (3)
C2—H20.9500C15—C161.387 (3)
C2—C31.388 (3)C15—C181.503 (3)
C3—C41.388 (3)C16—H160.9500
C3—C61.500 (3)C16—C171.381 (3)
C4—H40.9500C17—H170.9500
C4—C51.376 (3)C18—H18A0.9800
C5—H50.9500C18—H18B0.9800
C6—H6A0.9800C18—H18C0.9800
O1—Cu1—O1i79.94 (6)H6A—C6—H6B109.5
O1—Cu1—N192.61 (6)H6A—C6—H6C109.5
O1—Cu1—N2172.98 (6)H6B—C6—H6C109.5
O1—Cu1—N391.51 (6)N2—C7—H7118.8
N1—Cu1—O1i92.88 (6)N2—C7—C8122.4 (2)
N2—Cu1—O1i107.02 (6)C8—C7—H7118.8
N2—Cu1—N188.00 (7)C7—C8—H8119.8
N2—Cu1—N387.12 (7)C7—C8—C9120.3 (2)
N3—Cu1—O1i94.26 (6)C9—C8—H8119.8
N3—Cu1—N1172.28 (7)C8—C9—C10117.1 (2)
O2—S1—O1107.41 (9)C8—C9—C12121.9 (2)
O2—S1—O3111.85 (11)C10—C9—C12120.9 (2)
O2—S1—O4112.76 (10)C9—C10—H10120.2
O3—S1—O1107.15 (9)C11—C10—C9119.7 (2)
O3—S1—O4111.80 (10)C11—C10—H10120.2
O4—S1—O1105.39 (9)N2—C11—C10123.0 (2)
Cu1—O1—Cu1i100.06 (5)N2—C11—H11118.5
S1—O1—Cu1114.83 (8)C10—C11—H11118.5
S1—O1—Cu1i145.08 (9)C9—C12—H12A109.5
C1—N1—Cu1119.26 (14)C9—C12—H12B109.5
C1—N1—C5117.40 (18)C9—C12—H12C109.5
C5—N1—Cu1123.27 (15)H12A—C12—H12B109.5
C7—N2—Cu1124.81 (15)H12A—C12—H12C109.5
C7—N2—C11117.51 (19)H12B—C12—H12C109.5
C11—N2—Cu1117.56 (14)N3—C13—H13119.0
C13—N3—Cu1121.04 (14)N3—C13—C14122.1 (2)
C13—N3—C17117.95 (18)C14—C13—H13119.0
C17—N3—Cu1120.98 (14)C13—C14—H14119.8
N1—C1—H1118.7C13—C14—C15120.5 (2)
N1—C1—C2122.6 (2)C15—C14—H14119.8
C2—C1—H1118.7C14—C15—C16117.06 (19)
C1—C2—H2119.7C14—C15—C18121.8 (2)
C1—C2—C3120.6 (2)C16—C15—C18121.1 (2)
C3—C2—H2119.7C15—C16—H16120.1
C2—C3—C4116.4 (2)C17—C16—C15119.7 (2)
C2—C3—C6121.6 (2)C17—C16—H16120.1
C4—C3—C6122.1 (2)N3—C17—C16122.55 (19)
C3—C4—H4119.7N3—C17—H17118.7
C5—C4—C3120.5 (2)C16—C17—H17118.7
C5—C4—H4119.7C15—C18—H18A109.5
N1—C5—C4122.6 (2)C15—C18—H18B109.5
N1—C5—H5118.7C15—C18—H18C109.5
C4—C5—H5118.7H18A—C18—H18B109.5
C3—C6—H6A109.5H18A—C18—H18C109.5
C3—C6—H6B109.5H18B—C18—H18C109.5
C3—C6—H6C109.5
Cu1—N1—C1—C2175.95 (17)C2—C3—C4—C50.6 (3)
Cu1—N1—C5—C4176.14 (17)C3—C4—C5—N10.0 (4)
Cu1—N2—C7—C8176.59 (17)C5—N1—C1—C21.2 (3)
Cu1—N2—C11—C10177.43 (17)C6—C3—C4—C5179.2 (2)
Cu1—N3—C13—C14179.55 (16)C7—N2—C11—C101.1 (3)
Cu1—N3—C17—C16178.49 (16)C7—C8—C9—C100.2 (3)
O2—S1—O1—Cu1i60.22 (17)C7—C8—C9—C12178.5 (2)
O2—S1—O1—Cu1122.28 (11)C8—C9—C10—C110.3 (3)
O3—S1—O1—Cu1117.39 (10)C9—C10—C11—N21.0 (3)
O3—S1—O1—Cu1i60.10 (17)C11—N2—C7—C80.6 (3)
O4—S1—O1—Cu1i179.32 (14)C12—C9—C10—C11178.0 (2)
O4—S1—O1—Cu11.82 (11)C13—N3—C17—C163.1 (3)
N1—C1—C2—C30.6 (3)C13—C14—C15—C163.0 (3)
N2—C7—C8—C90.1 (4)C13—C14—C15—C18176.1 (2)
N3—C13—C14—C151.0 (3)C14—C15—C16—C172.0 (3)
C1—N1—C5—C40.9 (3)C15—C16—C17—N31.1 (3)
C1—C2—C3—C40.3 (3)C17—N3—C13—C142.0 (3)
C1—C2—C3—C6179.5 (2)C18—C15—C16—C17177.2 (2)
Symmetry code: (i) x+1, y+1, z+1.
Hydrogen-bond geometry (Å, º) top
D—H···AD—HH···AD···AD—H···A
C1—H1···O2i0.952.323.247 (3)166
C5—H5···O40.952.453.214 (3)137
C10—H10···O2ii0.952.413.218 (3)143
C11—H11···O4ii0.952.593.299 (3)132
C13—H13···O40.952.443.149 (3)131
C16—H16···O3iii0.952.573.441 (3)152
C17—H17···O1i0.952.573.152 (2)120
C17—H17···O3i0.952.283.235 (3)178
Symmetry codes: (i) x+1, y+1, z+1; (ii) x, y+1, z+1; (iii) x, y, z1.
catena-Poly[[bis(4-methylpyridine-κN)zinc(II)]-sulfato-κ2O:O'] (UMD1448_a) top
Crystal data top
[Zn(SO4)(C6H7N)2]F(000) = 712
Mr = 347.68Dx = 1.635 Mg m3
Monoclinic, P21/cMo Kα radiation, λ = 0.71073 Å
a = 14.9703 (10) ÅCell parameters from 9901 reflections
b = 9.7229 (7) Åθ = 3.0–25.4°
c = 9.8290 (6) ŵ = 1.90 mm1
β = 99.161 (2)°T = 295 K
V = 1412.41 (16) Å3BLOCK, colourless
Z = 40.33 × 0.18 × 0.17 mm
Data collection top
Bruker D8 Venture CMOS
diffractometer
2245 reflections with I > 2σ(I)
φ and ω scansRint = 0.047
Absorption correction: multi-scan
(SADABS; Bruker, 2016)
θmax = 25.4°, θmin = 3.0°
Tmin = 0.368, Tmax = 0.429h = 1818
36405 measured reflectionsk = 1111
2587 independent reflectionsl = 1111
Refinement top
Refinement on F2Hydrogen site location: inferred from neighbouring sites
Least-squares matrix: fullH-atom parameters constrained
R[F2 > 2σ(F2)] = 0.029 w = 1/[σ2(Fo2) + (0.0106P)2 + 2.2444P]
where P = (Fo2 + 2Fc2)/3
wR(F2) = 0.063(Δ/σ)max = 0.001
S = 1.05Δρmax = 0.28 e Å3
2587 reflectionsΔρmin = 0.26 e Å3
184 parametersExtinction correction: SHELXL2014 (Sheldrick, 2015), Fc*=kFc[1+0.001xFc2λ3/sin(2θ)]-1/4
0 restraintsExtinction coefficient: 0.0064 (4)
Primary atom site location: structure-invariant direct methods
Special details top

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 (Å2) top
xyzUiso*/Ueq
Zn10.73426 (2)0.67083 (3)0.34428 (3)0.03279 (12)
S10.77109 (4)0.91047 (7)0.56007 (6)0.03436 (17)
O10.75464 (16)0.8521 (2)0.41889 (19)0.0534 (6)
O20.86570 (14)0.9318 (3)0.6042 (3)0.0683 (7)
O30.71701 (16)1.0322 (2)0.5637 (2)0.0584 (6)
O40.73861 (14)0.8018 (2)0.64984 (18)0.0452 (5)
N10.60062 (15)0.6304 (2)0.3468 (2)0.0400 (5)
N20.81748 (15)0.5253 (2)0.4368 (2)0.0353 (5)
C10.5570 (2)0.6899 (3)0.4395 (3)0.0506 (8)
H1A0.59060.73760.51230.061*
C20.4647 (2)0.6836 (3)0.4320 (3)0.0510 (8)
H2A0.43720.72740.49860.061*
C30.41246 (18)0.6127 (3)0.3264 (3)0.0406 (7)
C40.45827 (19)0.5495 (3)0.2325 (3)0.0490 (8)
H4A0.42620.49950.16010.059*
C50.5506 (2)0.5595 (3)0.2445 (3)0.0466 (7)
H5A0.57960.51570.17960.056*
C60.3116 (2)0.6041 (4)0.3144 (4)0.0618 (9)
H6A0.29090.67110.37410.093*
H6B0.29480.51380.34060.093*
H6C0.28440.62200.22090.093*
C70.8198 (2)0.3996 (3)0.3815 (3)0.0465 (7)
H7A0.78210.38130.29870.056*
C80.8752 (2)0.2967 (3)0.4412 (3)0.0477 (7)
H8A0.87380.21070.39930.057*
C90.93307 (17)0.3198 (3)0.5629 (3)0.0381 (6)
C100.92991 (19)0.4486 (3)0.6201 (3)0.0449 (7)
H10A0.96700.46880.70280.054*
C110.87254 (19)0.5478 (3)0.5561 (3)0.0418 (7)
H11A0.87190.63380.59730.050*
C120.9960 (2)0.2102 (3)0.6282 (4)0.0561 (9)
H12A1.03400.18010.56410.084*
H12B0.96150.13380.65340.084*
H12C1.03290.24650.70910.084*
Atomic displacement parameters (Å2) top
U11U22U33U12U13U23
Zn10.03253 (18)0.03542 (19)0.02896 (17)0.00093 (13)0.00042 (12)0.00190 (13)
S10.0396 (4)0.0349 (4)0.0276 (3)0.0059 (3)0.0023 (3)0.0029 (3)
O10.0915 (17)0.0413 (12)0.0273 (10)0.0098 (11)0.0094 (10)0.0040 (9)
O20.0416 (12)0.0901 (19)0.0710 (16)0.0201 (13)0.0020 (11)0.0040 (14)
O30.0808 (16)0.0455 (13)0.0483 (13)0.0172 (12)0.0084 (11)0.0002 (10)
O40.0614 (13)0.0453 (12)0.0276 (10)0.0145 (10)0.0038 (9)0.0006 (8)
N10.0355 (12)0.0463 (14)0.0371 (13)0.0036 (10)0.0024 (10)0.0001 (11)
N20.0371 (12)0.0349 (12)0.0319 (12)0.0033 (10)0.0008 (9)0.0030 (10)
C10.0433 (16)0.064 (2)0.0440 (17)0.0114 (15)0.0053 (13)0.0160 (15)
C20.0433 (17)0.060 (2)0.0517 (18)0.0053 (15)0.0147 (14)0.0157 (16)
C30.0346 (14)0.0445 (16)0.0415 (16)0.0054 (13)0.0028 (12)0.0045 (13)
C40.0399 (16)0.062 (2)0.0435 (17)0.0141 (15)0.0021 (13)0.0104 (15)
C50.0449 (17)0.0548 (19)0.0411 (16)0.0053 (14)0.0099 (13)0.0113 (14)
C60.0374 (17)0.077 (2)0.071 (2)0.0071 (17)0.0090 (16)0.0064 (19)
C70.0587 (19)0.0421 (17)0.0330 (15)0.0027 (14)0.0102 (13)0.0016 (13)
C80.064 (2)0.0331 (16)0.0420 (17)0.0021 (14)0.0041 (14)0.0022 (13)
C90.0328 (14)0.0377 (15)0.0429 (16)0.0051 (12)0.0031 (11)0.0096 (13)
C100.0447 (16)0.0421 (17)0.0412 (16)0.0048 (13)0.0135 (13)0.0006 (13)
C110.0429 (16)0.0363 (15)0.0426 (16)0.0049 (13)0.0039 (13)0.0015 (13)
C120.0490 (18)0.0463 (19)0.068 (2)0.0035 (15)0.0045 (16)0.0178 (16)
Geometric parameters (Å, º) top
Zn1—O11.915 (2)C4—H4A0.9300
Zn1—O4i1.9410 (18)C4—C51.372 (4)
Zn1—N12.043 (2)C5—H5A0.9300
Zn1—N22.005 (2)C6—H6A0.9600
S1—O11.483 (2)C6—H6B0.9600
S1—O21.429 (2)C6—H6C0.9600
S1—O31.438 (2)C7—H7A0.9300
S1—O41.506 (2)C7—C81.370 (4)
O4—Zn1ii1.9409 (18)C8—H8A0.9300
N1—C11.334 (4)C8—C91.379 (4)
N1—C51.344 (4)C9—C101.377 (4)
N2—C71.341 (4)C9—C121.498 (4)
N2—C111.340 (3)C10—H10A0.9300
C1—H1A0.9300C10—C111.375 (4)
C1—C21.374 (4)C11—H11A0.9300
C2—H2A0.9300C12—H12A0.9600
C2—C31.381 (4)C12—H12B0.9600
C3—C41.379 (4)C12—H12C0.9600
C3—C61.498 (4)
O1—Zn1—O4i102.86 (8)C5—C4—H4A119.6
O1—Zn1—N1105.61 (10)N1—C5—C4122.3 (3)
O1—Zn1—N2115.24 (9)N1—C5—H5A118.8
O4i—Zn1—N1102.98 (9)C4—C5—H5A118.8
O4i—Zn1—N2115.32 (9)C3—C6—H6A109.5
N2—Zn1—N1113.43 (9)C3—C6—H6B109.5
O1—S1—O4105.01 (11)C3—C6—H6C109.5
O2—S1—O1110.40 (15)H6A—C6—H6B109.5
O2—S1—O3114.06 (16)H6A—C6—H6C109.5
O2—S1—O4108.72 (14)H6B—C6—H6C109.5
O3—S1—O1109.13 (13)N2—C7—H7A118.5
O3—S1—O4109.11 (13)N2—C7—C8123.0 (3)
S1—O1—Zn1134.66 (13)C8—C7—H7A118.5
S1—O4—Zn1ii123.04 (12)C7—C8—H8A119.8
C1—N1—Zn1120.74 (19)C7—C8—C9120.4 (3)
C1—N1—C5117.3 (2)C9—C8—H8A119.8
C5—N1—Zn1121.3 (2)C8—C9—C12121.4 (3)
C7—N2—Zn1120.91 (18)C10—C9—C8116.4 (3)
C11—N2—Zn1122.21 (19)C10—C9—C12122.2 (3)
C11—N2—C7116.9 (2)C9—C10—H10A119.6
N1—C1—H1A118.6C11—C10—C9120.7 (3)
N1—C1—C2122.8 (3)C11—C10—H10A119.6
C2—C1—H1A118.6N2—C11—C10122.5 (3)
C1—C2—H2A119.8N2—C11—H11A118.7
C1—C2—C3120.5 (3)C10—C11—H11A118.7
C3—C2—H2A119.8C9—C12—H12A109.5
C2—C3—C6122.0 (3)C9—C12—H12B109.5
C4—C3—C2116.3 (3)C9—C12—H12C109.5
C4—C3—C6121.7 (3)H12A—C12—H12B109.5
C3—C4—H4A119.6H12A—C12—H12C109.5
C5—C4—C3120.8 (3)H12B—C12—H12C109.5
Zn1—N1—C1—C2169.3 (3)C1—C2—C3—C40.6 (5)
Zn1—N1—C5—C4169.5 (2)C1—C2—C3—C6179.7 (3)
Zn1—N2—C7—C8179.7 (2)C2—C3—C4—C50.8 (5)
Zn1—N2—C11—C10179.9 (2)C3—C4—C5—N10.1 (5)
O1—S1—O4—Zn1ii174.58 (14)C5—N1—C1—C21.5 (5)
O2—S1—O1—Zn198.2 (2)C6—C3—C4—C5179.4 (3)
O2—S1—O4—Zn1ii67.26 (19)C7—N2—C11—C100.6 (4)
O3—S1—O1—Zn1135.7 (2)C7—C8—C9—C101.4 (5)
O3—S1—O4—Zn1ii57.70 (18)C7—C8—C9—C12178.4 (3)
O4—S1—O1—Zn118.8 (2)C8—C9—C10—C111.0 (4)
N1—C1—C2—C30.6 (5)C9—C10—C11—N20.0 (5)
N2—C7—C8—C90.9 (5)C11—N2—C7—C80.1 (4)
C1—N1—C5—C41.2 (5)C12—C9—C10—C11178.8 (3)
Symmetry codes: (i) x, y+3/2, z1/2; (ii) x, y+3/2, z+1/2.
Hydrogen-bond geometry (Å, º) top
D—H···AD—HH···AD···AD—H···A
C1—H1A···O40.932.483.325 (3)150
C5—H5A···O3i0.932.553.401 (4)153
C7—H7A···O3i0.932.513.321 (4)147
Symmetry code: (i) x, y+3/2, z1/2.
catena-Poly[[tris(4-methylpyridine-κN)zinc(II)]-sulfato-κ2O:O'] (umd1540c_a) top
Crystal data top
[Zn(SO4)(C6H7N)2]Dx = 1.499 Mg m3
Mr = 440.81Mo Kα radiation, λ = 0.71073 Å
Orthorhombic, P212121Cell parameters from 8899 reflections
a = 9.4926 (5) Åθ = 2.9–25.2°
b = 11.4128 (7) ŵ = 1.39 mm1
c = 18.0235 (11) ÅT = 296 K
V = 1952.6 (2) Å3ROD, colourless
Z = 40.2 × 0.03 × 0.03 mm
F(000) = 912
Data collection top
Bruker D8 Venture CMOS
diffractometer
3118 reflections with I > 2σ(I)
φ and ω scansRint = 0.060
Absorption correction: multi-scan
(SADABS; Bruker, 2016)
θmax = 25.4°, θmin = 2.9°
Tmin = 0.450, Tmax = 0.490h = 118
24507 measured reflectionsk = 1313
3561 independent reflectionsl = 2121
Refinement top
Refinement on F2H-atom parameters constrained
Least-squares matrix: full w = 1/[σ2(Fo2) + (0.0216P)2 + 0.4739P]
where P = (Fo2 + 2Fc2)/3
R[F2 > 2σ(F2)] = 0.027(Δ/σ)max = 0.001
wR(F2) = 0.056Δρmax = 0.21 e Å3
S = 1.03Δρmin = 0.33 e Å3
3561 reflectionsExtinction correction: SHELXL2014 (Sheldrick, 2015), Fc*=kFc[1+0.001xFc2λ3/sin(2θ)]-1/4
248 parametersExtinction coefficient: 0.0025 (6)
0 restraintsAbsolute structure: Flack x determined using 1244 quotients [(I+)-(I-)]/[(I+)+(I-)] (Parsons et al., 2013)
Primary atom site location: structure-invariant direct methodsAbsolute structure parameter: 0.002 (7)
Hydrogen site location: inferred from neighbouring sites
Special details top

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 (Å2) top
xyzUiso*/Ueq
Zn10.63333 (4)0.71323 (4)0.53749 (2)0.02618 (13)
S10.32426 (9)0.70122 (9)0.59603 (5)0.0257 (2)
O10.4259 (2)0.7098 (3)0.53201 (14)0.0312 (6)
O20.3635 (3)0.7833 (3)0.65349 (13)0.0458 (7)
O30.3196 (3)0.5814 (3)0.62307 (16)0.0414 (7)
O40.1848 (3)0.7333 (2)0.56397 (13)0.0297 (6)
N10.7391 (3)0.6428 (3)0.62840 (18)0.0294 (8)
N20.6501 (3)0.8884 (3)0.58363 (17)0.0299 (7)
N30.6465 (4)0.5285 (3)0.49194 (17)0.0378 (8)
C10.8793 (4)0.6460 (3)0.6338 (2)0.0358 (9)
H10.92900.69290.60070.043*
C20.9538 (4)0.5834 (4)0.6859 (2)0.0390 (11)
H21.05160.58860.68750.047*
C30.8829 (4)0.5126 (3)0.7359 (2)0.0300 (9)
C40.7381 (4)0.5124 (4)0.7321 (2)0.0326 (10)
H40.68590.46920.76610.039*
C50.6702 (4)0.5761 (3)0.6778 (2)0.0325 (10)
H50.57250.57270.67540.039*
C60.9593 (5)0.4383 (4)0.7926 (3)0.0505 (13)
H6A1.02350.48650.82010.076*
H6B1.01080.37750.76760.076*
H6C0.89220.40380.82580.076*
C70.6571 (4)0.9810 (3)0.5392 (2)0.0391 (10)
H70.65660.96900.48820.047*
C80.6649 (6)1.0932 (4)0.5655 (3)0.0560 (15)
H80.67001.15530.53220.067*
C90.6653 (5)1.1157 (4)0.6403 (3)0.0495 (13)
C100.6562 (5)1.0207 (4)0.6866 (2)0.0420 (11)
H100.65551.03110.73780.050*
C110.6481 (5)0.9097 (4)0.6566 (2)0.0381 (10)
H110.64090.84630.68880.046*
C120.6763 (9)1.2407 (5)0.6692 (3)0.102 (3)
H12A0.73701.24240.71180.153*
H12B0.58441.26830.68290.153*
H12C0.71451.29030.63110.153*
C130.7642 (5)0.4938 (4)0.4579 (3)0.0504 (12)
H130.84260.54250.46020.061*
C140.7758 (6)0.3903 (4)0.4196 (3)0.0558 (14)
H140.86030.37060.39660.067*
C150.6629 (6)0.3163 (4)0.4152 (3)0.0531 (13)
C160.5436 (6)0.3499 (4)0.4520 (3)0.0592 (14)
H160.46520.30100.45200.071*
C170.5381 (5)0.4556 (4)0.4891 (3)0.0467 (12)
H170.45500.47640.51300.056*
C180.6692 (8)0.2030 (5)0.3704 (3)0.092 (2)
H18A0.74710.15640.38710.138*
H18B0.68120.22130.31880.138*
H18C0.58320.16010.37710.138*
Atomic displacement parameters (Å2) top
U11U22U33U12U13U23
Zn10.0254 (2)0.0290 (2)0.0242 (2)0.0005 (2)0.00078 (19)0.0021 (2)
S10.0231 (5)0.0323 (5)0.0216 (4)0.0001 (4)0.0011 (3)0.0004 (4)
O10.0250 (12)0.0431 (15)0.0254 (13)0.0037 (12)0.0028 (10)0.0028 (16)
O20.0448 (16)0.0613 (18)0.0312 (14)0.0061 (19)0.0037 (13)0.0188 (15)
O30.0409 (18)0.0413 (18)0.0421 (18)0.0013 (13)0.0021 (14)0.0162 (14)
O40.0230 (13)0.0404 (17)0.0257 (13)0.0063 (12)0.0027 (10)0.0015 (12)
N10.0284 (19)0.0284 (19)0.0315 (19)0.0021 (14)0.0045 (14)0.0022 (16)
N20.0310 (19)0.0318 (17)0.0269 (17)0.0018 (15)0.0010 (15)0.0010 (14)
N30.046 (2)0.0337 (18)0.0343 (19)0.0044 (18)0.0013 (18)0.0034 (15)
C10.032 (2)0.040 (2)0.035 (2)0.004 (2)0.004 (2)0.0093 (19)
C20.026 (2)0.052 (3)0.038 (3)0.003 (2)0.0035 (19)0.009 (2)
C30.033 (2)0.032 (2)0.024 (2)0.0062 (19)0.0027 (18)0.0011 (16)
C40.037 (2)0.030 (2)0.030 (2)0.0056 (18)0.0040 (19)0.0067 (19)
C50.027 (2)0.037 (2)0.034 (2)0.0069 (18)0.0008 (18)0.0049 (19)
C60.051 (3)0.060 (3)0.041 (3)0.016 (2)0.005 (2)0.012 (2)
C70.057 (3)0.032 (2)0.028 (2)0.0040 (19)0.008 (2)0.003 (2)
C80.093 (4)0.036 (3)0.039 (3)0.001 (3)0.014 (3)0.000 (2)
C90.068 (4)0.034 (2)0.047 (3)0.003 (2)0.010 (2)0.015 (2)
C100.047 (3)0.048 (3)0.031 (2)0.004 (2)0.001 (2)0.014 (2)
C110.040 (3)0.045 (2)0.029 (2)0.002 (2)0.003 (2)0.0006 (19)
C120.192 (8)0.046 (4)0.069 (4)0.009 (4)0.022 (5)0.029 (3)
C130.048 (3)0.043 (3)0.060 (3)0.009 (2)0.007 (3)0.001 (3)
C140.068 (4)0.047 (3)0.052 (3)0.023 (3)0.011 (3)0.006 (3)
C150.084 (4)0.037 (3)0.038 (3)0.018 (3)0.010 (3)0.004 (2)
C160.066 (3)0.039 (3)0.072 (4)0.008 (2)0.015 (3)0.007 (3)
C170.048 (3)0.036 (3)0.055 (3)0.002 (2)0.000 (2)0.003 (2)
C180.157 (7)0.048 (3)0.072 (4)0.018 (5)0.020 (4)0.029 (3)
Geometric parameters (Å, º) top
Zn1—O11.972 (2)C6—H6B0.9600
Zn1—O4i1.989 (2)C6—H6C0.9600
Zn1—N12.083 (3)C7—H70.9300
Zn1—N22.172 (3)C7—C81.368 (6)
Zn1—N32.265 (3)C8—H80.9300
S1—O11.507 (2)C8—C91.372 (6)
S1—O21.445 (3)C9—C101.371 (6)
S1—O31.452 (3)C9—C121.523 (6)
S1—O41.490 (3)C10—H100.9300
O4—Zn1ii1.989 (2)C10—C111.380 (5)
N1—C11.334 (5)C11—H110.9300
N1—C51.342 (5)C12—H12A0.9600
N2—C71.327 (5)C12—H12B0.9600
N2—C111.338 (5)C12—H12C0.9600
N3—C131.335 (5)C13—H130.9300
N3—C171.325 (6)C13—C141.373 (7)
C1—H10.9300C14—H140.9300
C1—C21.376 (6)C14—C151.367 (7)
C2—H20.9300C15—C161.368 (7)
C2—C31.386 (6)C15—C181.525 (6)
C3—C41.376 (6)C16—H160.9300
C3—C61.512 (5)C16—C171.380 (7)
C4—H40.9300C17—H170.9300
C4—C51.378 (6)C18—H18A0.9600
C5—H50.9300C18—H18B0.9600
C6—H6A0.9600C18—H18C0.9600
O1—Zn1—O4i101.86 (10)H6A—C6—H6B109.5
O1—Zn1—N1120.88 (12)H6A—C6—H6C109.5
O1—Zn1—N296.34 (12)H6B—C6—H6C109.5
O1—Zn1—N391.06 (13)N2—C7—H7118.7
O4i—Zn1—N1136.31 (12)N2—C7—C8122.6 (4)
O4i—Zn1—N292.97 (11)C8—C7—H7118.7
O4i—Zn1—N386.48 (11)C7—C8—H8119.5
N1—Zn1—N291.08 (12)C7—C8—C9121.0 (4)
N1—Zn1—N384.23 (13)C9—C8—H8119.5
N2—Zn1—N3172.53 (14)C8—C9—C12120.7 (5)
O2—S1—O1109.97 (16)C10—C9—C8116.8 (4)
O2—S1—O3112.19 (18)C10—C9—C12122.5 (4)
O2—S1—O4110.32 (17)C9—C10—H10120.3
O3—S1—O1109.74 (17)C9—C10—C11119.4 (4)
O3—S1—O4109.55 (16)C11—C10—H10120.3
O4—S1—O1104.81 (14)N2—C11—C10123.4 (4)
S1—O1—Zn1127.02 (15)N2—C11—H11118.3
S1—O4—Zn1ii130.57 (15)C10—C11—H11118.3
C1—N1—Zn1121.8 (3)C9—C12—H12A109.5
C1—N1—C5117.0 (4)C9—C12—H12B109.5
C5—N1—Zn1120.4 (3)C9—C12—H12C109.5
C7—N2—Zn1120.4 (3)H12A—C12—H12B109.5
C7—N2—C11116.7 (3)H12A—C12—H12C109.5
C11—N2—Zn1122.8 (3)H12B—C12—H12C109.5
C13—N3—Zn1119.3 (3)N3—C13—H13118.2
C17—N3—Zn1123.8 (3)N3—C13—C14123.6 (5)
C17—N3—C13116.4 (4)C14—C13—H13118.2
N1—C1—H1118.4C13—C14—H14120.1
N1—C1—C2123.2 (4)C15—C14—C13119.8 (5)
C2—C1—H1118.4C15—C14—H14120.1
C1—C2—H2120.1C14—C15—C16116.7 (4)
C1—C2—C3119.8 (4)C14—C15—C18121.6 (5)
C3—C2—H2120.1C16—C15—C18121.8 (5)
C2—C3—C6122.2 (4)C15—C16—H16119.6
C4—C3—C2117.0 (4)C15—C16—C17120.7 (5)
C4—C3—C6120.8 (4)C17—C16—H16119.6
C3—C4—H4119.9N3—C17—C16122.6 (5)
C3—C4—C5120.1 (4)N3—C17—H17118.7
C5—C4—H4119.9C16—C17—H17118.7
N1—C5—C4122.8 (4)C15—C18—H18A109.5
N1—C5—H5118.6C15—C18—H18B109.5
C4—C5—H5118.6C15—C18—H18C109.5
C3—C6—H6A109.5H18A—C18—H18B109.5
C3—C6—H6B109.5H18A—C18—H18C109.5
C3—C6—H6C109.5H18B—C18—H18C109.5
Zn1—N1—C1—C2168.4 (3)C2—C3—C4—C53.2 (6)
Zn1—N1—C5—C4169.5 (3)C3—C4—C5—N12.0 (7)
Zn1—N2—C7—C8178.7 (4)C5—N1—C1—C21.2 (6)
Zn1—N2—C11—C10178.8 (3)C6—C3—C4—C5176.8 (4)
Zn1—N3—C13—C14170.6 (4)C7—N2—C11—C101.6 (6)
Zn1—N3—C17—C16170.8 (4)C7—C8—C9—C100.6 (8)
O1—S1—O4—Zn1ii3.6 (3)C7—C8—C9—C12179.1 (5)
O2—S1—O1—Zn147.0 (3)C8—C9—C10—C110.4 (7)
O2—S1—O4—Zn1ii114.7 (2)C9—C10—C11—N20.7 (7)
O3—S1—O1—Zn176.8 (2)C11—N2—C7—C81.3 (6)
O3—S1—O4—Zn1ii121.3 (2)C12—C9—C10—C11179.3 (5)
O4—S1—O1—Zn1165.61 (19)C13—N3—C17—C161.2 (7)
N1—C1—C2—C30.1 (7)C13—C14—C15—C161.7 (8)
N2—C7—C8—C90.2 (8)C13—C14—C15—C18177.2 (5)
N3—C13—C14—C150.3 (8)C14—C15—C16—C172.2 (8)
C1—N1—C5—C40.3 (6)C15—C16—C17—N30.8 (8)
C1—C2—C3—C42.3 (6)C17—N3—C13—C141.7 (7)
C1—C2—C3—C6177.7 (4)C18—C15—C16—C17176.7 (5)
Symmetry codes: (i) x+1/2, y+3/2, z+1; (ii) x1/2, y+3/2, z+1.
catena-Poly[[tetrakis(4-methylpyridine-κN)cadmium(II)]-sulfato-κ2O:O'] (umd1375_a) top
Crystal data top
[Cd(SO4)(C6H7N)4]F(000) = 2368
Mr = 580.96Dx = 1.487 Mg m3
Monoclinic, C2/cMo Kα radiation, λ = 0.71073 Å
a = 11.4545 (12) ÅCell parameters from 9677 reflections
b = 18.657 (2) Åθ = 3.0–25.7°
c = 24.714 (3) ŵ = 0.96 mm1
β = 100.691 (3)°T = 297 K
V = 5190.0 (10) Å3BLOCK, colourless
Z = 80.34 × 0.2 × 0.18 mm
Data collection top
Bruker D8 Venture CMOS
diffractometer
4336 reflections with I > 2σ(I)
φ and ω scansRint = 0.038
Absorption correction: multi-scan
(SADABS; Bruker, 2016)
θmax = 25.8°, θmin = 3.0°
Tmin = 0.224, Tmax = 0.259h = 1313
89835 measured reflectionsk = 2222
4957 independent reflectionsl = 3030
Refinement top
Refinement on F2Hydrogen site location: inferred from neighbouring sites
Least-squares matrix: fullH-atom parameters constrained
R[F2 > 2σ(F2)] = 0.026 w = 1/[σ2(Fo2) + (0.0313P)2 + 8.6618P]
where P = (Fo2 + 2Fc2)/3
wR(F2) = 0.071(Δ/σ)max = 0.001
S = 1.09Δρmax = 0.74 e Å3
4957 reflectionsΔρmin = 0.34 e Å3
314 parametersExtinction correction: SHELXL2014 (Sheldrick, 2015), Fc*=kFc[1+0.001xFc2λ3/sin(2θ)]-1/4
18 restraintsExtinction coefficient: 0.00105 (7)
Primary atom site location: structure-invariant direct methods
Special details top

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 (Å2) top
xyzUiso*/Ueq
Cd10.50000.50000.50000.03761 (9)
Cd20.50000.47768 (2)0.25000.03604 (9)
S10.67059 (5)0.47963 (4)0.39044 (2)0.03846 (15)
O10.57078 (17)0.48567 (12)0.42023 (8)0.0565 (5)
O20.6224 (2)0.47972 (15)0.33195 (8)0.0767 (7)
O30.7461 (3)0.54068 (17)0.40324 (14)0.1038 (10)
O40.7339 (2)0.41422 (16)0.40457 (10)0.0870 (8)
N10.69302 (19)0.49835 (12)0.55385 (9)0.0416 (5)
N20.48552 (19)0.37501 (13)0.50421 (9)0.0475 (5)
N30.62050 (18)0.56493 (12)0.21844 (8)0.0411 (5)
N40.37958 (19)0.38282 (12)0.27345 (9)0.0447 (5)
C10.7931 (2)0.47415 (17)0.53984 (11)0.0522 (7)
H10.78890.45360.50530.063*
C20.9015 (3)0.47826 (19)0.57395 (12)0.0606 (8)
H20.96860.46060.56230.073*
C30.9119 (2)0.50853 (17)0.62568 (12)0.0508 (7)
C40.8090 (2)0.53346 (17)0.63967 (11)0.0521 (7)
H40.81090.55490.67380.062*
C50.7035 (2)0.52700 (16)0.60374 (11)0.0477 (7)
H50.63510.54360.61480.057*
C61.0286 (3)0.5145 (3)0.66412 (16)0.0960 (15)
H6A1.09130.51690.64330.144*
H6B1.04010.47330.68780.144*
H6C1.02930.55710.68600.144*
C70.5607 (3)0.33064 (17)0.48611 (13)0.0577 (8)
H70.61820.34980.46830.069*
C80.5566 (4)0.25743 (19)0.49280 (15)0.0755 (10)
H80.61150.22840.48000.091*
C90.4720 (4)0.22718 (19)0.51828 (16)0.0754 (10)
C100.3928 (3)0.27309 (18)0.53557 (14)0.0640 (8)
H100.33230.25500.55200.077*
C110.4028 (3)0.34583 (16)0.52866 (12)0.0524 (7)
H110.34940.37590.54160.063*
C120.4641 (6)0.1468 (2)0.5266 (3)0.132 (2)
H12A0.41930.13740.55500.198*
H12B0.54270.12740.53720.198*
H12C0.42550.12480.49290.198*
C130.5875 (3)0.59980 (15)0.17102 (11)0.0484 (6)
H130.51200.59140.15070.058*
C140.6599 (3)0.64749 (17)0.15084 (13)0.0608 (8)
H140.63270.67080.11760.073*
C150.7720 (3)0.66099 (18)0.17936 (15)0.0626 (8)
C160.8052 (3)0.6257 (2)0.22835 (16)0.0692 (9)
H160.88030.63350.24940.083*
C170.7286 (2)0.57882 (18)0.24682 (13)0.0563 (7)
H170.75330.55600.28040.068*
C180.8554 (4)0.7123 (2)0.1581 (2)0.1022 (15)
H18A0.81010.74620.13360.153*
H18B0.90680.68590.13880.153*
H18C0.90240.73730.18850.153*
C190.4080 (3)0.34684 (16)0.32063 (12)0.0514 (7)
H190.47930.35750.34390.062*
C200.3363 (3)0.29446 (17)0.33643 (14)0.0597 (8)
H200.35980.27070.36970.072*
C210.2299 (3)0.27737 (17)0.30290 (14)0.0609 (8)
C220.2021 (3)0.31364 (19)0.25367 (14)0.0638 (8)
H220.13190.30340.22940.077*
C230.2781 (3)0.36497 (17)0.24042 (12)0.0542 (7)
H230.25780.38840.20680.065*
C240.1456 (4)0.2226 (2)0.31918 (17)0.0899 (13)
H24A0.18990.18770.34320.135*
H24B0.10340.19920.28680.135*
H24C0.09010.24620.33790.135*
Atomic displacement parameters (Å2) top
U11U22U33U12U13U23
Cd10.03155 (14)0.04792 (17)0.03387 (14)0.00385 (10)0.00739 (10)0.00098 (10)
Cd20.03247 (14)0.04608 (17)0.03132 (14)0.0000.01050 (10)0.000
S10.0296 (3)0.0605 (4)0.0262 (3)0.0049 (3)0.0075 (2)0.0016 (2)
O10.0434 (11)0.0866 (15)0.0451 (11)0.0059 (10)0.0227 (9)0.0010 (10)
O20.0671 (14)0.130 (2)0.0306 (10)0.0288 (13)0.0030 (10)0.0046 (11)
O30.0834 (18)0.113 (2)0.131 (2)0.0468 (17)0.0617 (18)0.0550 (19)
O40.0931 (18)0.104 (2)0.0715 (15)0.0555 (16)0.0351 (13)0.0270 (14)
N10.0368 (11)0.0494 (13)0.0384 (12)0.0039 (9)0.0062 (9)0.0011 (9)
N20.0480 (13)0.0514 (14)0.0446 (13)0.0025 (10)0.0122 (10)0.0014 (10)
N30.0355 (11)0.0474 (13)0.0411 (12)0.0035 (9)0.0092 (9)0.0011 (9)
N40.0413 (12)0.0460 (13)0.0501 (13)0.0009 (10)0.0171 (10)0.0014 (10)
C10.0470 (16)0.074 (2)0.0370 (14)0.0145 (14)0.0102 (12)0.0046 (13)
C20.0435 (16)0.096 (2)0.0444 (16)0.0218 (15)0.0140 (13)0.0004 (15)
C30.0346 (14)0.076 (2)0.0414 (15)0.0014 (13)0.0056 (11)0.0057 (13)
C40.0451 (15)0.072 (2)0.0393 (14)0.0031 (14)0.0083 (12)0.0132 (13)
C50.0340 (13)0.0639 (18)0.0467 (15)0.0031 (12)0.0113 (11)0.0137 (13)
C60.0418 (19)0.183 (5)0.059 (2)0.005 (2)0.0025 (16)0.007 (2)
C70.0604 (18)0.0611 (19)0.0569 (18)0.0072 (15)0.0251 (15)0.0006 (14)
C80.099 (3)0.055 (2)0.081 (2)0.0172 (19)0.040 (2)0.0067 (17)
C90.105 (3)0.0510 (19)0.076 (2)0.0013 (19)0.033 (2)0.0039 (17)
C100.075 (2)0.058 (2)0.064 (2)0.0127 (16)0.0251 (17)0.0039 (15)
C110.0526 (17)0.0557 (18)0.0509 (17)0.0011 (13)0.0153 (13)0.0062 (13)
C120.190 (6)0.053 (2)0.175 (5)0.005 (3)0.091 (5)0.005 (3)
C130.0498 (15)0.0516 (16)0.0426 (15)0.0060 (12)0.0053 (12)0.0001 (12)
C140.077 (2)0.0550 (18)0.0525 (18)0.0102 (16)0.0177 (16)0.0036 (14)
C150.0604 (19)0.0580 (19)0.077 (2)0.0128 (15)0.0322 (17)0.0038 (16)
C160.0366 (16)0.081 (2)0.088 (3)0.0143 (15)0.0079 (15)0.001 (2)
C170.0380 (15)0.070 (2)0.0585 (18)0.0054 (13)0.0019 (13)0.0089 (15)
C180.101 (3)0.089 (3)0.132 (4)0.036 (3)0.062 (3)0.000 (3)
C190.0501 (16)0.0513 (17)0.0556 (17)0.0051 (13)0.0173 (13)0.0028 (13)
C200.071 (2)0.0539 (18)0.0591 (18)0.0036 (15)0.0254 (16)0.0075 (14)
C210.072 (2)0.0558 (18)0.0632 (19)0.0140 (15)0.0328 (17)0.0090 (15)
C220.0589 (19)0.074 (2)0.061 (2)0.0203 (16)0.0163 (15)0.0097 (16)
C230.0531 (17)0.0617 (19)0.0496 (16)0.0073 (14)0.0142 (13)0.0017 (14)
C240.106 (3)0.085 (3)0.089 (3)0.037 (2)0.044 (2)0.005 (2)
Geometric parameters (Å, º) top
Cd1—O1i2.2822 (19)C7—H70.9300
Cd1—O12.2822 (19)C7—C81.378 (5)
Cd1—N1i2.360 (2)C8—H80.9300
Cd1—N12.360 (2)C8—C91.371 (5)
Cd1—N22.342 (2)C9—C101.372 (5)
Cd1—N2i2.342 (2)C9—C121.518 (6)
Cd2—O2ii2.240 (2)C10—H100.9300
Cd2—O22.240 (2)C10—C111.375 (4)
Cd2—N3ii2.358 (2)C11—H110.9300
Cd2—N32.358 (2)C12—H12A0.9600
Cd2—N42.381 (2)C12—H12B0.9600
Cd2—N4ii2.381 (2)C12—H12C0.9600
S1—O11.4745 (19)C13—H130.9300
S1—O21.448 (2)C13—C141.372 (4)
S1—O31.430 (3)C14—H140.9300
S1—O41.429 (2)C14—C151.368 (5)
N1—C11.336 (3)C15—C161.369 (5)
N1—C51.329 (3)C15—C181.514 (4)
N2—C71.330 (4)C16—H160.9300
N2—C111.332 (4)C16—C171.375 (4)
N3—C131.332 (3)C17—H170.9300
N3—C171.330 (3)C18—H18A0.9600
N4—C191.332 (4)C18—H18B0.9600
N4—C231.332 (4)C18—H18C0.9600
C1—H10.9300C19—H190.9300
C1—C21.367 (4)C19—C201.378 (4)
C2—H20.9300C20—H200.9300
C2—C31.382 (4)C20—C211.378 (5)
C3—C41.370 (4)C21—C221.377 (5)
C3—C61.493 (4)C21—C241.510 (4)
C4—H40.9300C22—H220.9300
C4—C51.365 (4)C22—C231.374 (4)
C5—H50.9300C23—H230.9300
C6—H6A0.9600C24—H24A0.9600
C6—H6B0.9600C24—H24B0.9600
C6—H6C0.9600C24—H24C0.9600
O1i—Cd1—O1180.0C3—C6—H6C109.5
O1—Cd1—N192.28 (7)H6A—C6—H6B109.5
O1i—Cd1—N187.72 (7)H6A—C6—H6C109.5
O1—Cd1—N1i87.72 (7)H6B—C6—H6C109.5
O1i—Cd1—N1i92.28 (7)N2—C7—H7118.7
O1i—Cd1—N292.23 (8)N2—C7—C8122.6 (3)
O1i—Cd1—N2i87.77 (8)C8—C7—H7118.7
O1—Cd1—N287.77 (8)C7—C8—H8119.8
O1—Cd1—N2i92.23 (8)C9—C8—C7120.4 (3)
N1—Cd1—N1i180.0C9—C8—H8119.8
N2—Cd1—N1i88.36 (8)C8—C9—C10116.8 (3)
N2i—Cd1—N1i91.64 (8)C8—C9—C12122.2 (4)
N2—Cd1—N191.64 (8)C10—C9—C12121.0 (4)
N2i—Cd1—N188.36 (8)C9—C10—H10119.9
N2—Cd1—N2i180.0C9—C10—C11120.2 (3)
O2ii—Cd2—O2178.05 (15)C11—C10—H10119.9
O2ii—Cd2—N3ii88.89 (9)N2—C11—C10122.8 (3)
O2ii—Cd2—N389.77 (8)N2—C11—H11118.6
O2—Cd2—N3ii89.77 (8)C10—C11—H11118.6
O2—Cd2—N388.89 (9)C9—C12—H12A109.5
O2—Cd2—N494.95 (9)C9—C12—H12B109.5
O2—Cd2—N4ii86.50 (8)C9—C12—H12C109.5
O2ii—Cd2—N4ii94.95 (9)H12A—C12—H12B109.5
O2ii—Cd2—N486.50 (8)H12A—C12—H12C109.5
N3ii—Cd2—N392.71 (10)H12B—C12—H12C109.5
N3ii—Cd2—N491.81 (7)N3—C13—H13118.5
N3ii—Cd2—N4ii174.08 (7)N3—C13—C14123.0 (3)
N3—Cd2—N4ii91.81 (7)C14—C13—H13118.5
N3—Cd2—N4174.08 (7)C13—C14—H14119.8
N4—Cd2—N4ii83.95 (10)C15—C14—C13120.3 (3)
O2—S1—O1108.14 (13)C15—C14—H14119.8
O3—S1—O1108.78 (14)C14—C15—C16116.6 (3)
O3—S1—O2108.82 (19)C14—C15—C18122.0 (4)
O4—S1—O1110.40 (14)C16—C15—C18121.4 (3)
O4—S1—O2109.08 (15)C15—C16—H16119.7
O4—S1—O3111.6 (2)C15—C16—C17120.7 (3)
S1—O1—Cd1150.80 (13)C17—C16—H16119.7
S1—O2—Cd2163.96 (16)N3—C17—C16122.5 (3)
C1—N1—Cd1128.14 (18)N3—C17—H17118.7
C5—N1—Cd1115.61 (17)C16—C17—H17118.7
C5—N1—C1116.2 (2)C15—C18—H18A109.5
C7—N2—Cd1123.3 (2)C15—C18—H18B109.5
C7—N2—C11117.2 (3)C15—C18—H18C109.5
C11—N2—Cd1119.31 (18)H18A—C18—H18B109.5
C13—N3—Cd2122.70 (17)H18A—C18—H18C109.5
C17—N3—Cd2120.31 (18)H18B—C18—H18C109.5
C17—N3—C13116.9 (2)N4—C19—H19118.5
C19—N4—Cd2121.96 (19)N4—C19—C20122.9 (3)
C23—N4—Cd2121.02 (19)C20—C19—H19118.5
C23—N4—C19117.0 (2)C19—C20—H20120.0
N1—C1—H1118.5C21—C20—C19120.0 (3)
N1—C1—C2123.1 (3)C21—C20—H20120.0
C2—C1—H1118.5C20—C21—C24122.3 (3)
C1—C2—H2119.8C22—C21—C20116.8 (3)
C1—C2—C3120.4 (3)C22—C21—C24120.9 (3)
C3—C2—H2119.8C21—C22—H22120.0
C2—C3—C6122.1 (3)C23—C22—C21120.0 (3)
C4—C3—C2116.2 (3)C23—C22—H22120.0
C4—C3—C6121.7 (3)N4—C23—C22123.2 (3)
C3—C4—H4119.8N4—C23—H23118.4
C5—C4—C3120.3 (3)C22—C23—H23118.4
C5—C4—H4119.8C21—C24—H24A109.5
N1—C5—C4123.8 (2)C21—C24—H24B109.5
N1—C5—H5118.1C21—C24—H24C109.5
C4—C5—H5118.1H24A—C24—H24B109.5
C3—C6—H6A109.5H24A—C24—H24C109.5
C3—C6—H6B109.5H24B—C24—H24C109.5
Cd1—N1—C1—C2177.6 (2)C5—N1—C1—C20.3 (5)
Cd1—N1—C5—C4177.2 (2)C6—C3—C4—C5179.7 (3)
Cd1—N2—C7—C8174.8 (3)C7—N2—C11—C100.0 (4)
Cd1—N2—C11—C10176.2 (2)C7—C8—C9—C100.8 (6)
Cd2—N3—C13—C14176.0 (2)C7—C8—C9—C12180.0 (4)
Cd2—N3—C17—C16175.6 (3)C8—C9—C10—C112.1 (6)
Cd2—N4—C19—C20176.3 (2)C9—C10—C11—N21.7 (5)
Cd2—N4—C23—C22175.9 (2)C11—N2—C7—C81.2 (5)
O1—S1—O2—Cd28.4 (7)C12—C9—C10—C11178.7 (4)
O2—S1—O1—Cd1172.5 (3)C13—N3—C17—C161.3 (5)
O3—S1—O1—Cd154.5 (3)C13—C14—C15—C161.1 (5)
O3—S1—O2—Cd2126.4 (7)C13—C14—C15—C18179.0 (3)
O4—S1—O1—Cd168.2 (3)C14—C15—C16—C170.6 (5)
O4—S1—O2—Cd2111.7 (7)C15—C16—C17—N30.6 (5)
N1—C1—C2—C30.1 (5)C17—N3—C13—C140.8 (4)
N2—C7—C8—C90.9 (6)C18—C15—C16—C17179.5 (4)
N3—C13—C14—C150.4 (5)C19—N4—C23—C221.9 (4)
N4—C19—C20—C210.1 (5)C19—C20—C21—C221.4 (5)
C1—N1—C5—C41.0 (4)C19—C20—C21—C24177.4 (3)
C1—C2—C3—C40.2 (5)C20—C21—C22—C231.1 (5)
C1—C2—C3—C6179.6 (4)C21—C22—C23—N40.6 (5)
C2—C3—C4—C50.8 (5)C23—N4—C19—C201.6 (4)
C3—C4—C5—N11.3 (5)C24—C21—C22—C23177.8 (3)
Symmetry codes: (i) x+1, y+1, z+1; (ii) x+1, y, z+1/2.
Hydrogen-bond geometry (Å, º) top
D—H···AD—HH···AD···AD—H···A
C1—H1···O40.932.563.471 (4)167
C5—H5···O1i0.932.423.097 (3)130
C7—H7···O40.932.543.452 (4)167
C11—H11···O3i0.932.453.360 (4)164
C17—H17···O20.932.573.205 (4)126
C23—H23···O2ii0.932.493.136 (4)127
Symmetry codes: (i) x+1, y+1, z+1; (ii) x+1, y, z+1/2.
Synthetic conditions for the isolation of crystals of compounds (1)–(7) top
CompoundSaltmg of SaltH2O (ml)4-Picoline (ml)T (°C)
(1)Fe(SO4)·7H2O8.80.02.090
(2)Co(SO4)·7H2O4.80.22.085
(3)Ni(SO4)·6H2O3.70.22.090
(4)Cu(SO4) anhydrous11.60.23.090
(5)Zn(SO4)·7H2O9.80.12.050
(6)Zn(SO4)·7H2O23.00.02.060
(7)Cd(SO4)·8/3H2O9.80.01.580
Geometric parameters (Å, °) for the reported complexes top
M = Fe, (1)M = Co, (2)M = Ni, (3)M = Cd, (7)
M—OFe1—O12.056 (1)Co1—O12.090 (1)Ni1—O12.098 (1)Cd1—O12.282 (2)
Fe2—O22.025 (1)Co2—O22.053 (1)Ni2—O22.058 (1)Cd2—O22.240 (2)
M—NFe1—N12.229 (2)Co1—N12.174 (2)Ni1—N12.119 (2)Cd1—N12.360 (2)
Fe1—N22.240 (2)Co1—N22.187 (2)Ni1—N22.132 (2)Cd1—N22.343 (2)
Fe2—N32.242 (2)Co2—N32.187 (2)Ni2—N32.154 (2)Cd2—N32.358 (2)
Fe2—N42.257 (2)Co2—N42.208 (2)Ni2—N42.131 (2)Cd2—N42.381 (2)
O—M—OO1—Fe1—O1i180.0O1—Co1—O1i180.0O1—Ni1—O1i180.0O1—Cd1—O1i180.0
O2—Fe2—O2ii178.03 (9)O2—Co2—O2iii177.5 (1)O2—Ni2—O2ii180.0O2—Cd2—O2iii178.1 (2)
N—M—NN1—Fe1—N292.13 (6)N1—Co1—N292.27 (7)N1—Ni1—N291.99 (7)N1—Cd1—N291.64 (8)
N1—Fe1—N2i87.87 (6)N1—Co1—N2i87.73 (7)N1—Ni1—N2i88.01 (7)N1—Cd1—N2i88.36 (8)
N1—Fe1—N1i180.0N1—Co1—N1i180.0N1—Ni1—N1i180.00 (9)N1—Cd1—N1i180.0
N2—Fe1—N2i180.0N2—Co1—N2i180.0N2—Ni1—N2i180.0N2—Cd1—N2i180.0
N3—Fe2—N3ii92.81 (5)N3—Co2—N3iii90.57 (9)N3—Ni2—N3ii85.30 (9)N3—Cd2—N3iii92.7 (1)
N3—Fe2—N4ii90.47 (8)N3—Co2—N4iii92.58 (6)N3—Ni2—N4ii92.02 (6)N3—Cd2—N4iii91.81 (7)
N4—Fe2—N4ii84.16 (8)N4—Co2—N4iii84.47 (9)N4—Ni2—N4ii90.81 (9)N4—Cd2—N4iii84.0 (1)
N3—Fe2—N4175.09 (5)N3—Co2—N4175.43 (6)N3—Ni2—N4175.91 (6)N3—Cd2—N4174.08 (7)
M = Cu, (4)M = Zn, (5)M = Zn, (6)
M—OCu1—O11.985 (1)Zn1—O11.915 (2)Zn1—O11.972 (2)
Cu1—O1i2.253 (1)Zn1—O4iv1.941 (2)Zn1—O4v1.989 (2)
M—NCu1—N12.041 (2)Zn1—N12.043 (2)Zn1—N12.083 (3)
Cu1—N22.011 (2)Zn1—N22.005 (2)Zn1—N22.172 (3)
Cu1—N32.024 (2)Zn1—N32.265 (3)
O—M—OO1—Cu1—O1i79.94 (6)O1—Zn1—O4iv102.86 (8)O1—Zn1—O4v101.9 (1)
N—M—NN1—Cu1—N288.00 (7)N1—Zn1—N2113.43 (9)N1—Zn1—N291.1 (1)
N1—Cu1—N3172.28 (7)N1—Zn1—N384.2 (1)
N2—Cu1—N387.12 (7)N2—Zn1—N3172.5 (1)
Symmetry codes: (i) -x+1, -y+1, -z+1; (ii) -x+1, y, -z+3/2; (iii) -x+1, y, -z+1/2; (iv) x, -y+3/2, z-1/2; (v) x+1/2, -y+3/2, -z+1.
Crystal field stabilization energy [units are Dq (Oh)] top
Observed geometries are highlighted in bold.
TetrahedralTrigonal bipyramidalSquare pyramidalOctahedral
Iron (d6)2.672.734.574
Cobalt (d7)5.345.459.148
Nickel (d8)3.566.271012
Copper (d9)1.787.099.146
Zinc (d10)0000
Cadmium (d10)0000
 

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