Literature DB >> 22904746

catena-Poly[[tetra-aqua-copper(II)]-μ-pyrazine-2-carboxamide-κ(3)N(4):N(1),O-[bis-(sulfato-κO)copper(II)]-μ-pyrazine-2-carboxamide-κ(3)N(1),O:N(4)].

Sadif A Shirvan1, Sara Haydari Dezfuli.   

Abstract

In the crystal of the title polymeric compound, [Cu(2)(SO(4))(2)(C(5)H(5)N(3)O)(2)(H(2)O)(4)](n), two independent n class="Chemical">Cu(II) atoms are located on individual inversion centers. One Cu(II) atom is coordinated by four water mol-ecules and two pyrazine-2-carboxamide ligands in a distorted O(4)N(2) octa-hedral geometry; the other is N,O-chelated by two pyrazine-2-carboxamide ligands and further coordinated by two sulfate anions in a distorted O(4)N(2) octa-hedral geometry. The pyrazine-2-carboxamide ligands bridge the Cu(II) atoms to form a polymeric chain running along [110]. The crystal structure features N-H⋯O, O-H⋯O and weak C-H⋯O hydrogen bonds.

Entities:  

Year:  2012        PMID： 22904746      PMCID： PMC3414139          DOI： 10.1107/S1600536812031844

Source DB:  PubMed          Journal:  Acta Crystallogr Sect E Struct Rep Online        ISSN： 1600-5368


Related literature

For related structures, see: Abu-Youssef et al. (2006 ▶); Azhdari Tehrani et al. (2010 ▶); Goher & Mautner (2000 ▶); Kristiansson (2002 ▶); Mir Mohammad Sadegh et al. (2010 ▶); Munakata et al. (1997 ▶); Pacigova et al. (2008 ▶); Shirvan & Haydari Dezfuli (2012a ▶,b ▶,c ▶).

Experimental

Crystal data

[Cu2(SO4)2(C5H5N3O)2(H2O)4] M = 318.77 Monoclinic, a = 11.2699 (12) Å b = 7.3799 (7) Å c = 11.8669 (15) Å β = 95.267 (9)° V = 982.81 (19) Å3 Z = 4 Mo Kα radiation μ = 2.47 mm−1 T = 298 K 0.25 × 0.20 × 0.04 mm

Data collection

Bruker APEXII CCD area-detector diffractometer Absorption correction: multi-scan (SADABS; Bruker, 2001 ▶) T min = 0.589, T max = 0.926 7420 measured reflections 1928 independent reflections 1544 reflections with I > 2σ(I) R int = 0.090

Refinement

R[F 2 > 2σ(F 2)] = 0.035 wR(F 2) = 0.103 S = 1.07 1928 reflections 173 parameters 6 restraints H atoms treated by a mixture of independent and constrained refinement Δρmax = 0.83 e Å−3 Δρmin = −0.69 e Å−3 Data collection: APEX2 (Bruker, 2007 ▶); cell refinement: SAINT (Bruker, 2007 ▶); data reduction: SAINT; program(s) used to solve structure: SHELXS97 (Sheldrick, 2008 ▶); program(s) used to refine structure: SHELXL97 (Sheldrick, 2008 ▶); molecular graphics: SHELXTL (Sheldrick, 2008 ▶); software used to prepare material for publication: SHELXTL. Crystal structure: contains datablock(s) I, global. DOI: 10.1107/S1600536812031844/xu5585sup1.cif Structure factors: contains datablock(s) I. DOI: 10.1107/S1600536812031844/xu5585Isup2.hkl Additional supplementary materials: crystallographic information; 3D view; checkCIF report
[Cu2(SO4)2(C5H5N3O)2(H2O)4]F(000) = 644
Mr = 318.77Dx = 2.154 Mg m−3
Monoclinic, P21/cMo Kα radiation, λ = 0.71073 Å
Hall symbol: -P 2ybcCell parameters from 7420 reflections
a = 11.2699 (12) Åθ = 1.8–26.0°
b = 7.3799 (7) ŵ = 2.47 mm−1
c = 11.8669 (15) ÅT = 298 K
β = 95.267 (9)°Plate, blue
V = 982.81 (19) Å30.25 × 0.20 × 0.04 mm
Z = 4
Bruker APEXII CCD area-detector diffractometer1928 independent reflections
Radiation source: fine-focus sealed tube1544 reflections with I > 2σ(I)
Graphite monochromatorRint = 0.090
ω scansθmax = 26.0°, θmin = 1.8°
Absorption correction: multi-scan (SADABS; Bruker, 2001)h = −13→13
Tmin = 0.589, Tmax = 0.926k = −8→9
7420 measured reflectionsl = −14→14
Refinement on F2Primary atom site location: structure-invariant direct methods
Least-squares matrix: fullSecondary atom site location: difference Fourier map
R[F2 > 2σ(F2)] = 0.035Hydrogen site location: inferred from neighbouring sites
wR(F2) = 0.103H atoms treated by a mixture of independent and constrained refinement
S = 1.07w = 1/[σ2(Fo2) + (0.057P)2] where P = (Fo2 + 2Fc2)/3
1928 reflections(Δ/σ)max = 0.006
173 parametersΔρmax = 0.83 e Å−3
6 restraintsΔρmin = −0.69 e Å−3
Geometry. All e.s.d.'s (except the e.s.d. in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell e.s.d.'s are taken into account individually in the estimation of e.s.d.'s in distances, angles and torsion angles; correlations between e.s.d.'s in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell e.s.d.'s is used for estimating e.s.d.'s involving l.s. planes.
Refinement. Refinement of F2 against ALL reflections. The weighted R-factor wR and goodness of fit S are based on F2, conventional R-factors R are based on F, with F set to zero for negative F2. The threshold expression of F2 > σ(F2) is used only for calculating R-factors(gt) etc. and is not relevant to the choice of reflections for refinement. R-factors based on F2 are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger.
xyzUiso*/Ueq
C10.2270 (3)0.3902 (5)0.4101 (3)0.0263 (7)
H10.21890.48790.36050.032*
C20.3319 (3)0.2877 (5)0.4182 (3)0.0272 (8)
H20.39360.32090.37560.033*
C30.2541 (3)0.1005 (5)0.5473 (3)0.0262 (8)
H30.26090.00010.59480.031*
C40.1517 (3)0.2024 (5)0.5411 (3)0.0230 (7)
C50.0473 (3)0.1773 (5)0.6079 (3)0.0261 (7)
N10.1397 (2)0.3496 (4)0.4721 (2)0.0230 (6)
N20.3451 (2)0.1431 (4)0.4860 (2)0.0229 (6)
N30.0314 (3)0.0226 (4)0.6589 (3)0.0333 (8)
H3C−0.02960.00770.69650.040*
H3B0.0820−0.06390.65470.040*
O1−0.0233 (2)0.3090 (4)0.6107 (2)0.0281 (6)
O20.5178 (3)0.0396 (4)0.3047 (2)0.0364 (7)
H2B0.465 (3)0.007 (6)0.255 (3)0.040 (13)*
H2C0.562 (3)0.107 (5)0.272 (3)0.045 (14)*
O30.5887 (2)0.2275 (4)0.5292 (2)0.0280 (6)
H3D0.627 (4)0.248 (7)0.5901 (17)0.069 (18)*
H3E0.620 (3)0.286 (5)0.481 (2)0.033 (12)*
O40.3372 (2)0.5564 (4)0.6316 (2)0.0313 (6)
O50.2000 (3)0.4720 (4)0.7649 (2)0.0364 (7)
O60.1397 (2)0.6869 (4)0.6196 (2)0.0330 (6)
O70.2862 (2)0.7724 (4)0.7689 (2)0.0340 (6)
Cu10.00000.50000.50000.0258 (2)
Cu20.50000.00000.50000.02044 (18)
S10.23960 (7)0.61972 (11)0.69724 (6)0.0199 (2)
U11U22U33U12U13U23
C10.0328 (19)0.0213 (18)0.0248 (16)−0.0008 (15)0.0027 (14)0.0046 (14)
C20.0224 (17)0.028 (2)0.0322 (18)0.0006 (15)0.0065 (14)0.0026 (15)
C30.0231 (17)0.026 (2)0.0297 (16)0.0046 (15)0.0026 (13)0.0052 (15)
C40.0208 (17)0.0205 (18)0.0272 (16)0.0014 (13)−0.0011 (13)−0.0019 (14)
C50.0228 (17)0.0268 (19)0.0282 (16)0.0018 (14)0.0000 (14)−0.0001 (15)
N10.0220 (14)0.0189 (15)0.0275 (14)0.0025 (11)−0.0019 (12)0.0008 (11)
N20.0162 (13)0.0230 (16)0.0294 (14)0.0010 (11)0.0021 (11)0.0023 (12)
N30.0307 (17)0.0274 (18)0.0445 (18)0.0118 (13)0.0175 (15)0.0125 (15)
O10.0254 (12)0.0270 (14)0.0325 (12)0.0096 (10)0.0050 (10)0.0026 (11)
O20.0283 (14)0.0500 (19)0.0305 (13)−0.0121 (13)0.0003 (12)0.0030 (13)
O30.0292 (14)0.0275 (15)0.0263 (12)−0.0081 (11)−0.0023 (11)0.0035 (11)
O40.0297 (13)0.0359 (15)0.0290 (12)0.0042 (11)0.0068 (11)0.0007 (11)
O50.0350 (15)0.0319 (16)0.0429 (15)0.0014 (12)0.0080 (12)0.0126 (12)
O60.0321 (14)0.0281 (15)0.0358 (13)0.0082 (11)−0.0135 (11)−0.0032 (11)
O70.0360 (14)0.0310 (16)0.0336 (13)−0.0032 (12)−0.0044 (11)−0.0098 (12)
Cu10.0225 (3)0.0205 (4)0.0344 (3)0.0111 (2)0.0028 (2)0.0033 (2)
Cu20.0126 (3)0.0198 (3)0.0290 (3)0.0020 (2)0.0018 (2)0.0008 (2)
S10.0176 (4)0.0204 (4)0.0212 (4)0.0009 (3)−0.0011 (3)0.0001 (3)
Cu1—O11.961 (3)O2—H2B0.83 (3)
Cu1—O62.447 (3)O2—H2C0.83 (4)
Cu1—N11.979 (3)O3—H3D0.82 (3)
Cu1—O1i1.961 (3)O3—H3E0.82 (3)
Cu1—O6i2.447 (3)N1—C11.316 (4)
Cu1—N1i1.979 (3)N1—C41.360 (5)
Cu2—O22.363 (2)N2—C21.337 (5)
Cu2—O31.968 (3)N2—C31.348 (4)
Cu2—N22.034 (2)N3—C51.312 (5)
Cu2—O2ii2.363 (2)N3—H3C0.8600
Cu2—O3ii1.968 (3)N3—H3B0.8600
Cu2—N2ii2.034 (2)C1—C21.399 (5)
S1—O41.481 (2)C3—C41.374 (5)
S1—O51.449 (3)C4—C51.489 (5)
S1—O61.474 (3)C1—H10.9300
S1—O71.479 (3)C2—H20.9300
O1—C51.258 (4)C3—H30.9300
S1···C43.683 (4)O7···H2Cvi2.03 (3)
S1···O2iii3.479 (3)O7···H3Dvii1.87 (3)
S1···H3Biv2.9500O7···H1x2.2400
S1···H3Cv2.9000O7···H2Biii2.90 (4)
S1···H3iv3.0800N1···S13.439 (3)
S1···H2Cvi3.01 (4)N1···O12.593 (3)
S1···H3Evi2.84 (3)N1···O43.177 (4)
S1···H3Dvii2.97 (3)N1···O63.043 (4)
S1···H2Biii2.74 (4)N1···N22.764 (4)
O1···O53.207 (4)N1···C52.368 (4)
O1···N12.593 (3)N1···O1i2.966 (4)
O1···C42.343 (4)N1···O6i3.247 (3)
O1···N3v3.165 (4)N2···O23.126 (4)
O1···C1i3.187 (4)N2···O32.816 (3)
O1···O6i2.921 (3)N2···N12.764 (4)
O1···N1i2.966 (4)N2···O2ii3.110 (4)
O2···O4viii2.845 (4)N2···O3ii2.845 (4)
O2···N2ii3.110 (4)N2···O5viii3.081 (4)
O2···O33.044 (4)N3···O6xi2.820 (4)
O2···N23.126 (4)N3···C4xii3.428 (5)
O2···C23.174 (5)N3···O1xiii3.165 (4)
O2···S1viii3.479 (3)N3···O5xiii2.862 (5)
O2···O3ii3.106 (4)N3···H32.7700
O2···O7vi2.815 (4)C1···O43.059 (4)
O2···C3ii3.152 (5)C1···O5viii3.180 (5)
O3···N2ii2.845 (4)C1···O7xiv3.108 (5)
O3···O7ix2.687 (3)C2···O43.213 (4)
O3···C23.100 (4)C2···O5viii2.949 (5)
O3···O4vi2.679 (4)C3···O5viii3.393 (4)
O3···O23.044 (4)C4···O53.323 (4)
O3···N22.816 (3)C4···S13.683 (4)
O3···O2ii3.106 (4)C4···N3xii3.428 (5)
O3···C3ii3.181 (4)C5···O53.252 (5)
O4···N13.177 (4)C3···H3B2.7000
O4···C23.213 (4)H1···O1i2.7100
O4···O2iii2.845 (4)H1···O7xiv2.2400
O4···O3vi2.679 (4)H2···O22.6800
O4···C13.059 (4)H2···O32.8100
O5···C2iii2.949 (5)H2B···S1viii2.74 (4)
O5···C1iii3.180 (5)H2B···O4viii2.01 (4)
O5···C53.252 (5)H2B···O7viii2.90 (4)
O5···N2iii3.081 (4)H2C···S1vi3.01 (4)
O5···C43.323 (4)H2C···O7vi2.03 (3)
O5···O13.207 (4)H2C···H3ii2.5500
O5···C3iii3.393 (4)H2C···H3Dviii2.58 (5)
O5···N3v2.862 (5)H3···S1xi3.0800
O6···N1i3.247 (3)H3···O6xi2.7100
O6···N3iv2.820 (4)H3···O7xi2.6600
O6···N13.043 (4)H3···N32.7700
O6···O1i2.921 (3)H3···H3B2.2500
O6···C5i3.419 (4)H3···O2ii2.6800
O7···O3vii2.687 (3)H3···O3ii2.8800
O7···C1x3.108 (5)H3···H2Cii2.5500
O7···O2vi2.815 (4)H3B···S1xi2.9500
O1···H3Cv2.7400H3B···O6xi2.0100
O1···H1i2.7100H3B···O7xi2.8300
O2···H3ii2.6800H3B···C32.7000
O2···H22.6800H3B···H32.2500
O3···H22.8100H3C···S1xiii2.9000
O3···H3ii2.8800H3C···O1xiii2.7400
O4···H2Biii2.01 (4)H3C···O5xiii2.0300
O4···H3Evi1.87 (3)H3D···S1ix2.97 (3)
O5···H3Cv2.0300H3D···O7ix1.87 (3)
O6···H3Biv2.0100H3D···H2Ciii2.58 (5)
O6···H3iv2.7100H3E···S1vi2.84 (3)
O7···H3iv2.6600H3E···O4vi1.87 (3)
O7···H3Biv2.8300
O1—Cu1—O697.77 (10)O5—S1—O7111.47 (15)
O1—Cu1—N182.32 (10)O6—S1—O7108.29 (16)
O1—Cu1—O1i180.00Cu1—O1—C5114.4 (2)
O1—Cu1—O6i82.23 (10)Cu1—O6—S1125.95 (17)
O1—Cu1—N1i97.68 (10)Cu2—O2—H2B123 (3)
O6—Cu1—N186.20 (10)Cu2—O2—H2C130 (3)
O1i—Cu1—O682.23 (10)H2B—O2—H2C105 (4)
O6—Cu1—O6i180.00Cu2—O3—H3D122 (3)
O6—Cu1—N1i93.80 (10)Cu2—O3—H3E125 (2)
O1i—Cu1—N197.68 (10)H3D—O3—H3E107 (4)
O6i—Cu1—N193.80 (10)Cu1—N1—C4112.6 (2)
N1—Cu1—N1i180.00C1—N1—C4118.7 (3)
O1i—Cu1—O6i97.77 (10)Cu1—N1—C1127.8 (2)
O1i—Cu1—N1i82.32 (10)C2—N2—C3117.6 (3)
O6i—Cu1—N1i86.20 (10)Cu2—N2—C2120.7 (2)
O2—Cu2—O388.84 (10)Cu2—N2—C3121.7 (2)
O2—Cu2—N290.30 (10)C5—N3—H3C120.00
O2—Cu2—O2ii180.00C5—N3—H3B120.00
O2—Cu2—O3ii91.16 (10)H3B—N3—H3C120.00
O2—Cu2—N2ii89.70 (10)N1—C1—C2120.6 (3)
O3—Cu2—N289.41 (11)N2—C2—C1121.3 (3)
O2ii—Cu2—O391.16 (10)N2—C3—C4121.4 (3)
O3—Cu2—O3ii180.00N1—C4—C5112.3 (3)
O3—Cu2—N2ii90.59 (11)C3—C4—C5127.2 (3)
O2ii—Cu2—N289.70 (10)N1—C4—C3120.4 (3)
O3ii—Cu2—N290.59 (11)N3—C5—C4120.1 (3)
N2—Cu2—N2ii180.00O1—C5—N3123.1 (3)
O2ii—Cu2—O3ii88.84 (10)O1—C5—C4116.8 (3)
O2ii—Cu2—N2ii90.30 (10)N1—C1—H1120.00
O3ii—Cu2—N2ii89.41 (11)C2—C1—H1120.00
O4—S1—O5109.61 (17)N2—C2—H2119.00
O4—S1—O6109.82 (14)C1—C2—H2119.00
O4—S1—O7107.53 (14)N2—C3—H3119.00
O5—S1—O6110.07 (17)C4—C3—H3119.00
O6—Cu1—O1—C5−91.3 (2)O3ii—Cu2—N2—C353.3 (3)
N1—Cu1—O1—C5−6.2 (2)O5—S1—O6—Cu1−47.0 (2)
O6i—Cu1—O1—C588.7 (2)O7—S1—O6—Cu1−169.06 (14)
N1i—Cu1—O1—C5173.8 (2)O4—S1—O6—Cu173.8 (2)
O1—Cu1—O6—S141.74 (18)Cu1—O1—C5—C412.7 (4)
N1—Cu1—O6—S1−39.97 (17)Cu1—O1—C5—N3−166.3 (3)
O1i—Cu1—O6—S1−138.26 (18)C4—N1—C1—C2−2.3 (5)
N1i—Cu1—O6—S1140.03 (17)Cu1—N1—C1—C2166.0 (3)
O1—Cu1—N1—C4−1.9 (2)Cu1—N1—C4—C58.4 (4)
O6—Cu1—N1—C496.4 (2)C1—N1—C4—C5178.4 (3)
O1i—Cu1—N1—C4178.1 (2)Cu1—N1—C4—C3−168.8 (3)
O1—Cu1—N1—C1−170.8 (3)C1—N1—C4—C31.2 (5)
O6—Cu1—N1—C1−72.5 (3)C3—N2—C2—C1−0.7 (5)
O1i—Cu1—N1—C19.2 (3)C2—N2—C3—C4−0.4 (5)
O6i—Cu1—N1—C1107.6 (3)Cu2—N2—C3—C4177.2 (3)
O6i—Cu1—N1—C4−83.6 (2)Cu2—N2—C2—C1−178.3 (3)
O3—Cu2—N2—C3−126.7 (3)N1—C1—C2—N22.1 (5)
O2ii—Cu2—N2—C3−35.5 (3)N2—C3—C4—N10.2 (5)
O2—Cu2—N2—C3144.5 (3)N2—C3—C4—C5−176.6 (3)
O2—Cu2—N2—C2−38.0 (3)N1—C4—C5—O1−14.2 (5)
O3—Cu2—N2—C250.8 (3)C3—C4—C5—N3−18.3 (6)
O2ii—Cu2—N2—C2142.0 (3)N1—C4—C5—N3164.8 (3)
O3ii—Cu2—N2—C2−129.2 (3)C3—C4—C5—O1162.7 (4)
D—H···AD—HH···AD···AD—H···A
O2—H2B···O4viii0.83 (3)2.01 (4)2.845 (4)177 (5)
O2—H2C···O7vi0.83 (4)2.03 (3)2.815 (4)159 (3)
O3—H3D···O7ix0.82 (3)1.87 (3)2.687 (3)175 (5)
O3—H3E···O4vi0.82 (3)1.87 (3)2.679 (4)169 (3)
N3—H3B···O6xi0.862.012.820 (4)157
N3—H3C···O5xiii0.862.032.862 (5)162
C1—H1···O7xiv0.932.243.108 (5)154
Table 1

Selected bond lengths (Å)

Cu1—O11.961 (3)
Cu1—O62.447 (3)
Cu1—N11.979 (3)
Cu2—O22.363 (2)
Cu2—O31.968 (3)
Cu2—N22.034 (2)
Table 2

Hydrogen-bond geometry (Å, °)

D—H⋯A D—HH⋯A D⋯A D—H⋯A
O2—H2B⋯O4i 0.83 (3)2.01 (4)2.845 (4)177 (5)
O2—H2C⋯O7ii 0.83 (4)2.03 (3)2.815 (4)159 (3)
O3—H3D⋯O7iii 0.82 (3)1.87 (3)2.687 (3)175 (5)
O3—H3E⋯O4ii 0.82 (3)1.87 (3)2.679 (4)169 (3)
N3—H3B⋯O6iv 0.862.012.820 (4)157
N3—H3C⋯O5v 0.862.032.862 (5)162
C1—H1⋯O7vi 0.932.243.108 (5)154

Symmetry codes: (i) ; (ii) ; (iii) ; (iv) ; (v) ; (vi) .

  7 in total

1.  A short history of SHELX.

Authors:  George M Sheldrick
Journal:  Acta Crystallogr A       Date:  2007-12-21       Impact factor: 2.290

2.  Interpretation of the multiple vanadium-oxygen bonds in the central VO(eta2-O2)+ group. Synthesis, structure, supramolecular interactions and DFT studies for complexes with 2,2'-bipyridine, 1,10-phenanthroline, pyrazinato(1-) and pyrazinamide ligands.

Authors:  Silvia Pacigová; Róbert Gyepes; Jozef Tatiersky; Michal Sivák
Journal:  Dalton Trans       Date:  2008-01-07       Impact factor: 4.390

3.  Dichloridobis(pyrazine-2-carboxamide-κN(4))zinc(II).

Authors:  Sadif A Shirvan; Sara Haydari Dezfuli
Journal:  Acta Crystallogr Sect E Struct Rep Online       Date:  2012-04-04

4.  catena-Poly[[bis-(pyrazine-2-carbox-amide)mercury(II)]-di-μ-chlorido].

Authors:  Alireza Azhdari Tehrani; Bahareh Mir Mohammad Sadegh; Hamid Reza Khavasi
Journal:  Acta Crystallogr Sect E Struct Rep Online       Date:  2010-02-06

5.  catena-Poly[[bis-(pyrazine-2-carbox-amide-κN)mercury(II)]-di-μ-bromido].

Authors:  Bahareh Mir Mohammad Sadegh; Alireza Azhdari Tehrani; Hamid Reza Khavasi
Journal:  Acta Crystallogr Sect E Struct Rep Online       Date:  2010-01-16

6.  catena-Poly[[[aqua-(pyrazine-2-carboxamide-κ(2)N(1),O)zinc]-μ-pyrazine-2-carboxamide-κ(3)N(1),O:N(4)] dinitrate].

Authors:  Sadif A Shirvan; Sara Haydari Dezfuli
Journal:  Acta Crystallogr Sect E Struct Rep Online       Date:  2012-04-18

7.  Dibromidobis(pyrazine-2-carboxamide-κN(4))zinc.

Authors:  Sadif A Shirvan; Sara Haydari Dezfuli
Journal:  Acta Crystallogr Sect E Struct Rep Online       Date:  2012-03-31
  7 in total

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