Literature DB >> 25249873

Poly[[hexa-aqua-sesqui(μ-benzene-1,2,4,5-tetra-carboxyl-ato)dicopper(II)disodium] monohydrate].

Magatte Camara1, Mohamed Fadel Keita1, Cherif Cheikh Samsidine Cisse1, Carole Daiguebonne2, Olivier Guillou2.   

Abstract

In the title compound, {[Cu2Na2(C10H2O8)1.5(H2O)6]·H2O} n , the Cu(2+) ion is hexa-coordinated by five O atoms from benzene-1,2,4,5-tetra-carboxyl-ate (btec(4-)) ligands and one water mol-ecule. The Na(+) ion is also hexa-coordinated, by four O atoms from btec(4-) ligands and two water mol-ecules. One of the two btec(4-) mol-ecules sits on a crystallographic inversion centre. CuO6 and NaO6 octa-hedra are connected, forming bi-dimensional layers. These layers, which extend parallel to the ac plane, are further inter-connected by μ10- or μ11-bridging btec(4-) ligands and by O-H⋯O hydrogen bonds, involving both btec(4-) ligands and water mol-ecules, forming a three-dimensional network.

Entities:  

Keywords:  crystal structure

Year:  2014        PMID： 25249873      PMCID： PMC4158492          DOI： 10.1107/S1600536814014755

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


Related literature

For related structures, see: Camara et al. (2013 ▶); Luo et al. (2013 ▶); Gong & Zhang (2011 ▶); Liu et al. (2010 ▶); Zhang et al. (2007 ▶). For related crystal-growth methods in gels, see: Henisch (1988 ▶); Henisch & Roy (1970 ▶); Daiguebonne et al. (2003 ▶).

Experimental

Crystal data

[Cu2Na2(C10H2O8)1.5(H2O)6]·H2O M = 674.34 Monoclinic, a = 8.0844 (1) Å b = 16.9103 (3) Å c = 15.6815 (3) Å β = 98.055 (1)° V = 2122.66 (6) Å3 Z = 4 Mo Kα radiation μ = 2.15 mm−1 T = 293 K 0.11 × 0.08 × 0.07 mm

Data collection

Bruker APEXII diffractometer Absorption correction: multi-scan (SADABS; Bruker, 2007 ▶) T min = 0.701, T max = 0.848 34613 measured reflections 8438 independent reflections 4356 reflections with I > 2σ(I) R int = 0.058

Refinement

R[F 2 > 2σ(F 2)] = 0.049 wR(F 2) = 0.144 S = 0.94 8438 reflections 373 parameters 15 restraints H atoms treated by a mixture of independent and constrained refinement Δρmax = 1.49 e Å−3 Δρmin = −1.02 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: SHELXL2014 (Sheldrick, 2008 ▶); molecular graphics: DIAMOND (Brandenburg, 1999 ▶); software used to prepare material for publication: publCIF (Westrip, 2010 ▶). Crystal structure: contains datablock(s) I. DOI: 10.1107/S1600536814014755/pk2525sup1.cif Structure factors: contains datablock(s) I. DOI: 10.1107/S1600536814014755/pk2525Isup2.hkl CCDC reference: 1009732 Additional supporting information: crystallographic information; 3D view; checkCIF report
[Cu2Na2(C10H2O8)1.5(H2O)6]·H2OF(000) = 1356
Mr = 674.34Dx = 2.110 Mg m−3
Monoclinic, P21/cMo Kα radiation, λ = 0.71073 Å
a = 8.0844 (1) ÅCell parameters from 31092 reflections
b = 16.9103 (3) Åθ = 2.9–32.0°
c = 15.6815 (3) ŵ = 2.15 mm−1
β = 98.055 (1)°T = 293 K
V = 2122.66 (6) Å3Cobblestone, blue
Z = 40.11 × 0.08 × 0.07 mm
Bruker APEXII diffractometer8438 independent reflections
Radiation source: Fine-focus sealed tube4356 reflections with I > 2σ(I)
Graphite monochromatorRint = 0.058
CCD rotation images, thin slices scansθmax = 34.8°, θmin = 3.5°
Absorption correction: multi-scan (SADABS; Bruker, 2007)h = −11→12
Tmin = 0.701, Tmax = 0.848k = −26→21
34613 measured reflectionsl = −20→24
Refinement on F215 restraints
Least-squares matrix: fullHydrogen site location: inferred from neighbouring sites
R[F2 > 2σ(F2)] = 0.049H atoms treated by a mixture of independent and constrained refinement
wR(F2) = 0.144w = 1/[σ2(Fo2) + (0.0813P)2] where P = (Fo2 + 2Fc2)/3
S = 0.94(Δ/σ)max = 0.010
8438 reflectionsΔρmax = 1.49 e Å−3
373 parametersΔρmin = −1.02 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.
xyzUiso*/Ueq
Cu10.15805 (4)0.25569 (2)0.80720 (2)0.01609 (10)
Cu2−0.45959 (4)0.26469 (2)0.54858 (2)0.01697 (10)
Na1−0.17322 (14)0.13536 (7)0.78727 (8)0.0284 (3)
Na2−0.13005 (15)0.15430 (8)0.56592 (9)0.0329 (3)
O1120.2924 (2)0.17014 (11)0.76659 (13)0.0195 (4)
O211−0.5911 (2)0.17609 (11)0.58371 (13)0.0215 (4)
O10.1863 (2)0.31650 (12)0.69877 (13)0.0224 (4)
O4−0.4112 (3)0.11473 (14)0.85120 (16)0.0316 (5)
O511−0.2307 (2)0.27440 (11)0.78365 (14)0.0256 (5)
O811−0.3190 (2)0.35241 (11)0.52142 (13)0.0204 (4)
O812−0.0757 (2)0.29573 (12)0.57293 (14)0.0271 (5)
O1110.0408 (2)0.13710 (12)0.70094 (13)0.0230 (4)
O212−0.3474 (2)0.13420 (12)0.65142 (14)0.0260 (5)
O2−0.4857 (2)0.31465 (12)0.66155 (14)0.0228 (4)
O412−0.3727 (2)0.19907 (11)0.46253 (13)0.0215 (4)
O7110.3056 (2)0.15899 (12)0.98797 (15)0.0308 (5)
O5120.0052 (2)0.33892 (11)0.83143 (13)0.0214 (4)
O4110.3855 (2)0.31657 (12)0.87600 (15)0.0317 (5)
C8−0.0749 (3)0.42790 (15)0.51646 (17)0.0166 (5)
O7120.0771 (2)0.18442 (11)0.89280 (13)0.0222 (4)
C5−0.2469 (3)0.40780 (15)0.82911 (17)0.0172 (5)
C81−0.1595 (3)0.35232 (15)0.53885 (18)0.0177 (5)
C51−0.1527 (3)0.33362 (15)0.81388 (18)0.0165 (5)
C70.0755 (3)0.07233 (15)0.98119 (17)0.0167 (5)
C6−0.1850 (3)0.47968 (15)0.80321 (19)0.0191 (6)
H6−0.08660.48000.77880.023*
O50.1040 (3)0.13627 (18)0.50399 (18)0.0505 (7)
C4−0.3963 (3)0.09269 (15)0.36547 (17)0.0159 (5)
O3−0.1803 (4)−0.00918 (16)0.7752 (2)0.0556 (8)
OW1−0.4788 (3)−0.03675 (15)0.88423 (19)0.0526 (7)
C2−0.5855 (3)0.05086 (15)0.64934 (18)0.0161 (5)
C21−0.4989 (3)0.12554 (15)0.62866 (17)0.0160 (5)
C10.2666 (3)0.05056 (15)0.68709 (18)0.0169 (5)
C90.1473 (3)−0.00066 (16)0.96511 (18)0.0185 (5)
H90.2465−0.00130.94140.022*
C110.1920 (3)0.12402 (15)0.71862 (17)0.0166 (5)
C3−0.4787 (3)0.02144 (16)0.37516 (18)0.0194 (6)
H3−0.57850.02190.39840.023*
C41−0.4697 (3)0.16482 (15)0.40121 (17)0.0159 (5)
O6−0.1540 (4)0.0144 (2)0.5561 (3)0.0822 (11)
C710.1614 (3)0.14565 (15)0.95356 (18)0.0179 (6)
H42−0.494 (3)0.133 (2)0.824 (2)0.050*
H22−0.425 (4)0.300 (2)0.7052 (17)0.050*
H110.122 (3)0.300 (2)0.6598 (18)0.050*
H21−0.481 (4)0.3594 (12)0.650 (2)0.050*
H510.088 (5)0.153 (2)0.4512 (14)0.050*
H41−0.396 (4)0.136 (2)0.8981 (15)0.050*
H520.104 (5)0.0878 (10)0.499 (2)0.050*
H31−0.176 (5)−0.039 (2)0.7328 (16)0.050*
H120.282 (2)0.318 (2)0.690 (2)0.050*
H32−0.166 (5)−0.0448 (19)0.8137 (18)0.050*
U11U22U33U12U13U23
Cu10.01508 (17)0.01221 (17)0.0216 (2)0.00191 (11)0.00483 (13)−0.00013 (12)
Cu20.01881 (18)0.01265 (17)0.0207 (2)−0.00348 (11)0.00713 (13)−0.00177 (13)
Na10.0240 (6)0.0267 (7)0.0351 (7)−0.0005 (5)0.0067 (5)0.0006 (5)
Na20.0270 (6)0.0356 (7)0.0363 (8)0.0007 (5)0.0054 (5)0.0006 (6)
O1120.0192 (9)0.0127 (9)0.0264 (11)0.0019 (7)0.0021 (8)−0.0046 (8)
O2110.0209 (10)0.0132 (9)0.0307 (12)−0.0032 (7)0.0047 (8)0.0029 (8)
O10.0197 (10)0.0255 (11)0.0226 (11)0.0017 (8)0.0057 (8)0.0037 (9)
O40.0267 (12)0.0390 (14)0.0286 (13)0.0027 (9)0.0022 (9)−0.0038 (10)
O5110.0274 (11)0.0149 (10)0.0328 (13)0.0023 (8)−0.0015 (9)−0.0042 (8)
O8110.0189 (10)0.0136 (9)0.0297 (12)−0.0050 (7)0.0063 (8)0.0008 (8)
O8120.0270 (11)0.0190 (11)0.0338 (13)−0.0015 (8)−0.0015 (9)0.0063 (9)
O1110.0161 (10)0.0230 (11)0.0296 (12)0.0032 (7)0.0020 (8)−0.0030 (8)
O2120.0175 (10)0.0261 (11)0.0338 (13)−0.0070 (8)0.0015 (8)0.0023 (9)
O20.0277 (11)0.0203 (10)0.0203 (12)−0.0015 (8)0.0034 (8)−0.0017 (9)
O4120.0198 (9)0.0197 (10)0.0255 (11)−0.0020 (7)0.0050 (8)−0.0092 (8)
O7110.0218 (11)0.0276 (12)0.0405 (14)−0.0103 (8)−0.0042 (9)0.0035 (10)
O5120.0171 (10)0.0147 (10)0.0330 (12)0.0031 (7)0.0058 (8)−0.0023 (8)
O4110.0262 (11)0.0282 (12)0.0390 (14)−0.0121 (9)−0.0016 (9)0.0025 (10)
C80.0179 (13)0.0145 (13)0.0174 (14)−0.0042 (9)0.0030 (10)−0.0013 (10)
O7120.0223 (10)0.0199 (10)0.0246 (11)−0.0003 (8)0.0041 (8)0.0056 (8)
C50.0199 (13)0.0132 (13)0.0193 (14)0.0023 (9)0.0054 (10)−0.0002 (10)
C810.0181 (13)0.0167 (13)0.0194 (14)−0.0027 (10)0.0064 (10)−0.0046 (10)
C510.0186 (13)0.0138 (13)0.0179 (14)0.0020 (9)0.0054 (10)0.0009 (10)
C70.0145 (12)0.0146 (13)0.0213 (15)0.0004 (9)0.0039 (10)0.0033 (10)
C60.0184 (13)0.0157 (13)0.0251 (16)0.0001 (10)0.0096 (11)0.0026 (11)
O50.0407 (15)0.075 (2)0.0365 (16)−0.0024 (15)0.0076 (12)0.0115 (15)
C40.0162 (12)0.0153 (13)0.0167 (14)−0.0008 (9)0.0038 (10)−0.0028 (10)
O30.0532 (16)0.0305 (15)0.087 (2)0.0089 (12)0.0230 (17)0.0051 (15)
OW10.0622 (17)0.0350 (15)0.0592 (19)−0.0121 (12)0.0036 (14)−0.0014 (13)
C20.0168 (12)0.0116 (12)0.0203 (14)−0.0009 (9)0.0045 (10)0.0001 (10)
C210.0177 (13)0.0132 (12)0.0188 (14)−0.0041 (9)0.0082 (10)−0.0055 (10)
C10.0184 (13)0.0131 (12)0.0200 (14)−0.0001 (9)0.0049 (10)−0.0026 (10)
C90.0160 (13)0.0173 (13)0.0227 (15)0.0010 (10)0.0050 (10)0.0021 (11)
C110.0217 (14)0.0110 (12)0.0185 (14)0.0004 (10)0.0076 (10)−0.0002 (10)
C30.0172 (13)0.0194 (14)0.0228 (15)−0.0013 (10)0.0074 (11)−0.0037 (11)
C410.0181 (13)0.0113 (12)0.0186 (14)−0.0013 (9)0.0036 (10)0.0006 (10)
O60.068 (2)0.073 (2)0.106 (3)−0.0037 (17)0.015 (2)−0.015 (2)
C710.0219 (14)0.0115 (12)0.0217 (15)0.0003 (10)0.0077 (11)0.0000 (10)
Cu1—O5121.9450 (17)O111—C111.235 (3)
Cu1—O1121.9676 (17)O212—C211.235 (3)
Cu1—O7121.9821 (19)O412—C411.290 (3)
Cu1—O12.027 (2)O711—C711.235 (3)
Cu1—O4112.247 (2)O711—Cu2ii2.380 (2)
Cu1—Na13.3431 (12)O512—C511.271 (3)
Cu2—O4121.9523 (18)O411—C41ii1.223 (3)
Cu2—O8111.9519 (17)C8—C9iii1.390 (4)
Cu2—O2111.9603 (18)C8—C7iv1.404 (3)
Cu2—O22.000 (2)C8—C811.514 (3)
Cu2—O711i2.380 (2)O712—C711.273 (3)
Cu2—Na23.2331 (13)C5—C61.396 (4)
Na1—O42.317 (2)C5—C4v1.406 (3)
Na1—O1112.342 (2)C5—C511.504 (3)
Na1—O2122.384 (2)C7—C8v1.404 (3)
Na1—O5112.396 (2)C7—C91.402 (4)
Na1—O32.452 (3)C7—C711.514 (3)
Na1—O7122.566 (2)C6—C1iii1.387 (4)
Na1—Na23.5514 (19)C4—C31.396 (4)
Na2—O52.266 (3)C4—C5iv1.406 (3)
Na2—O62.377 (4)C4—C411.499 (3)
Na2—O2122.379 (2)C2—C3vi1.403 (3)
Na2—O1112.378 (2)C2—C1vii1.407 (4)
Na2—O8122.431 (2)C2—C211.501 (3)
Na2—O4122.482 (2)C1—C6viii1.387 (4)
O112—C111.289 (3)C1—C2ix1.407 (4)
O211—C211.279 (3)C1—C111.495 (3)
O511—C511.241 (3)C9—C8viii1.390 (4)
O811—C811.280 (3)C3—C2vi1.403 (3)
O812—C811.248 (3)C41—O411i1.223 (3)
O512—Cu1—O112171.78 (8)O5—Na2—Cu2140.32 (9)
O512—Cu1—O71291.64 (8)O6—Na2—Cu2120.71 (9)
O112—Cu1—O71291.24 (8)O212—Na2—Cu257.65 (5)
O512—Cu1—O186.91 (8)O111—Na2—Cu2120.96 (6)
O112—Cu1—O188.24 (8)O812—Na2—Cu265.00 (5)
O712—Cu1—O1164.40 (8)O412—Na2—Cu237.09 (4)
O512—Cu1—O41194.25 (8)O5—Na2—Na1127.53 (9)
O112—Cu1—O41192.33 (8)O6—Na2—Na187.46 (10)
O712—Cu1—O411106.20 (8)O212—Na2—Na141.83 (6)
O1—Cu1—O41189.40 (8)O111—Na2—Na140.82 (5)
O512—Cu1—Na186.34 (6)O812—Na2—Na194.95 (6)
O112—Cu1—Na189.62 (6)O412—Na2—Na1119.28 (6)
O712—Cu1—Na149.99 (6)Cu2—Na2—Na186.65 (3)
O1—Cu1—Na1114.41 (6)C11—O112—Cu1107.64 (15)
O411—Cu1—Na1156.16 (6)C21—O211—Cu2111.63 (16)
O412—Cu2—O81190.24 (8)C51—O511—Na1134.11 (18)
O412—Cu2—O21191.24 (8)C81—O811—Cu2123.53 (17)
O811—Cu2—O211176.00 (8)C81—O812—Na2130.61 (18)
O412—Cu2—O2160.91 (9)C11—O111—Na1131.02 (19)
O811—Cu2—O290.52 (8)C11—O111—Na2130.92 (18)
O211—Cu2—O286.87 (8)Na1—O111—Na297.59 (8)
O412—Cu2—O711i112.09 (8)C21—O212—Na2129.39 (19)
O811—Cu2—O711i87.53 (8)C21—O212—Na1134.18 (18)
O211—Cu2—O711i95.34 (8)Na2—O212—Na196.43 (8)
O2—Cu2—O711i86.99 (8)C41—O412—Cu2122.04 (16)
O412—Cu2—Na250.05 (6)C41—O412—Na2133.81 (17)
O811—Cu2—Na287.65 (6)Cu2—O412—Na292.86 (8)
O211—Cu2—Na290.46 (6)C71—O711—Cu2ii157.62 (19)
O2—Cu2—Na2110.93 (6)C51—O512—Cu1123.57 (17)
O711i—Cu2—Na2161.47 (6)C41ii—O411—Cu1162.7 (2)
O4—Na1—O111167.85 (10)C9iii—C8—C7iv119.8 (2)
O4—Na1—O21287.88 (9)C9iii—C8—C81117.9 (2)
O111—Na1—O21282.84 (8)C7iv—C8—C81122.2 (2)
O4—Na1—O51189.31 (9)C71—O712—Cu1128.85 (17)
O111—Na1—O51197.50 (8)C71—O712—Na1127.40 (17)
O212—Na1—O51184.18 (8)Cu1—O712—Na193.74 (8)
O4—Na1—O382.61 (10)C6—C5—C4v119.1 (2)
O111—Na1—O388.80 (9)C6—C5—C51118.0 (2)
O212—Na1—O385.32 (11)C4v—C5—C51122.8 (2)
O511—Na1—O3166.98 (10)O812—C81—O811124.2 (2)
O4—Na1—O712113.41 (9)O812—C81—C8120.7 (2)
O111—Na1—O71277.81 (7)O811—C81—C8115.1 (2)
O212—Na1—O712153.24 (8)O511—C51—O512125.5 (2)
O511—Na1—O71280.26 (7)O511—C51—C5119.5 (2)
O3—Na1—O712112.32 (10)O512—C51—C5115.0 (2)
O4—Na1—Cu1138.94 (8)C8v—C7—C9118.1 (2)
O111—Na1—Cu153.08 (5)C8v—C7—C71124.9 (2)
O212—Na1—Cu1116.99 (6)C9—C7—C71116.8 (2)
O511—Na1—Cu163.58 (5)C1iii—C6—C5121.7 (2)
O3—Na1—Cu1128.59 (8)C3—C4—C5iv119.3 (2)
O712—Na1—Cu136.27 (4)C3—C4—C41116.2 (2)
O4—Na1—Na2129.62 (8)C5iv—C4—C41124.3 (2)
O111—Na1—Na241.59 (6)C3vi—C2—C1vii118.8 (2)
O212—Na1—Na241.74 (5)C3vi—C2—C21118.2 (2)
O511—Na1—Na286.20 (7)C1vii—C2—C21122.9 (2)
O3—Na1—Na291.09 (9)O212—C21—O211123.9 (2)
O712—Na1—Na2115.12 (6)O212—C21—C2120.7 (2)
Cu1—Na1—Na281.34 (3)O211—C21—C2115.3 (2)
O5—Na2—O684.46 (12)C6viii—C1—C2ix119.6 (2)
O5—Na2—O212161.73 (11)C6viii—C1—C11117.5 (2)
O6—Na2—O21280.49 (11)C2ix—C1—C11122.8 (2)
O5—Na2—O11187.09 (9)C8viii—C9—C7122.0 (2)
O6—Na2—O11188.17 (12)O111—C11—O112123.0 (2)
O212—Na2—O11182.16 (8)O111—C11—C1120.5 (2)
O5—Na2—O81289.73 (10)O112—C11—C1116.5 (2)
O6—Na2—O812174.00 (11)C2vi—C3—C4121.5 (2)
O212—Na2—O812104.95 (8)O411i—C41—O412125.4 (2)
O111—Na2—O81290.07 (8)O411i—C41—C4120.0 (2)
O5—Na2—O412113.10 (10)O412—C41—C4114.4 (2)
O6—Na2—O412102.21 (11)O711—C71—O712127.3 (2)
O212—Na2—O41280.39 (7)O711—C71—C7117.9 (2)
O111—Na2—O412157.86 (8)O712—C71—C7114.7 (2)
O812—Na2—O41281.41 (7)
D—H···AD—HH···AD···AD—H···A
O4—H42···O112vii0.81 (2)1.93 (2)2.737 (3)174 (4)
O2—H22···O5110.82 (2)1.91 (2)2.697 (3)162 (4)
O1—H11···O8120.80 (2)1.95 (2)2.708 (3)159 (4)
O2—H21···OW1x0.78 (2)1.85 (2)2.618 (3)167 (4)
O5—H51···O512iv0.87 (2)1.91 (2)2.744 (3)161 (4)
O1—H12···O2ix0.81 (2)1.99 (2)2.794 (3)176 (4)
O3—H32···O1viii0.85 (2)2.36 (3)2.977 (3)130 (3)
Table 1

Hydrogen-bond geometry (Å, °)

D—H⋯A D—HH⋯A D⋯A D—H⋯A
O4—H42⋯O112i 0.81 (2)1.93 (2)2.737 (3)174 (4)
O2—H22⋯O5110.82 (2)1.91 (2)2.697 (3)162 (4)
O1—H11⋯O8120.80 (2)1.95 (2)2.708 (3)159 (4)
O2—H21⋯OW1ii 0.78 (2)1.85 (2)2.618 (3)167 (4)
O5—H51⋯O512iii 0.87 (2)1.91 (2)2.744 (3)161 (4)
O1—H12⋯O2iv 0.81 (2)1.99 (2)2.794 (3)176 (4)
O3—H32⋯O1v 0.85 (2)2.36 (3)2.977 (3)130 (3)

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

  3 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.  Poly[μ-aqua-aqua-(μ-benzene-1,2,4,5-tetra-carboxyl-ato)gadolinate(III)potassium(I)].

Authors:  Xue Yun Gong; Lei Zhang
Journal:  Acta Crystallogr Sect E Struct Rep Online       Date:  2011-05-11

3.  Poly[[octaaqua-μ4-(benzene-1,2,4,5-tetra-carboxyl-ato)-dicobalt(II)] octa-hydrate].

Authors:  Magatte Camara; Modou Tine; Carole Daiguebonne; Olivier Guillou; Thierry Roisnel
Journal:  Acta Crystallogr Sect E Struct Rep Online       Date:  2013-11-23
  3 in total

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