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NaxCuO2 (x ≃ 1.6) has been synthesized for different compositions x, resulting in both commensurate and incommensurate composite crystals. The crystal structures are reported for two incommensurate compounds (x = 1.58 and 1.62) determined by Rietveld refinements against X-ray powder diffraction data. The incommensurate compounds and commensurate Na8Cu5O10 (x = 1.6) are found to possess similar structures, with valence fluctuations of Cu2+/Cu3+ as the origin of the modulations of the CuO2 subsystems; the displacive modulations of Na being defined by the closest Na—O contacts between the subsystems. A comparison of the structure models obtained from single-crystal X-ray diffraction, synchrotron-radiation X-ray powder diffraction and X-ray powder diffraction with Cu Kα1 radiation indicates that single-crystal X-ray diffraction is by far the most accurate method, while powder diffraction with radiation from an X-ray tube provides the least accurate structure model.

Supporting information

cif

Crystallographic Information File (CIF) https://doi.org/10.1107/S0108768106039462/ck5018sup1.cif
Contains datablocks global, I, II, III

rtv

Rietveld powder data file (CIF format) https://doi.org/10.1107/S0108768106039462/ck5018Isup2.rtv
Contains datablock I

hkl

Structure factor file (CIF format) https://doi.org/10.1107/S0108768106039462/ck5018IIsup3.hkl
Contains datablock II

rtv

Rietveld powder data file (CIF format) https://doi.org/10.1107/S0108768106039462/ck5018IIIsup4.rtv
Contains datablock III

Computing details top

Cell refinement: (Jana2000; Petricek and Dusek, 2000) for (I). Program(s) used to solve structure: (Jana2000; Petricek and Dusek, 2000) for (I). For all compounds, program(s) used to refine structure: (Jana2000; Petricek and Dusek, 2000). Molecular graphics: (Diamond 3, Brandenburg, 2004) for (I). For all compounds, software used to prepare material for publication: (Jana2000; Petricek and Dusek, 2000).

Figures top
[Figure 1]
[Figure 2]
[Figure 3]
[Figure 4]
[Figure 5]
[Figure 6]
[Figure 7]
[Figure 8]
[Figure 9]
(I) sodium copper oxide top
Crystal data top
CuNa1.57664O2V = 121.73 (1) Å3
Mr = 661.6Z = 2
Monoclinic, C2/m(0β0)s0†F(000) = 125
q = 0.78832b*‡Dx = 9.023 Mg m3
a = 8.24153 (4) ÅSynchrotron radiation, λ = 0.65046 Å
b = 2.78589 (2) ÅT = 293 K
c = 5.71687 (3) Å?, ? × ? × ? mm
β = 111.9698 (5)°
† Symmetry operations: (1) x1, x2, x3, x4; (2) −x1, x2, −x3, 1/2+x4; (3) −x1, −x2, −x3, −x4; (4) x1, −x2, x3, 1/2−x4; (5) 1/2+x1, 1/2+x2, x3, x4; (6) 1/2−x1, 1/2+x2, −x3, 1/2+x4; (7) 1/2−x1, 1/2−x2, −x3, −x4; (8) 1/2+x1, 1/2−x2, x3, 1/2−x4.

texobject1427800954.png; texobject1427800955.png

Data collection top
Radiation source: NSLS, Brookhaven National Laboratory2θmin = 5°, 2θmax = 43.404°, 2θstep = 0.004°
Refinement top
Rp = 0.07536 parameters
Rwp = 0.1010 restraints
Rexp = 0.050Weighting scheme based on measured s.u.'s
R(F) = 0.048(Δ/σ)max = 0.295
χ2 = NOT FOUNDBackground function: 4 Legendre polynoms
9602 data pointsPreferred orientation correction: none
Profile function: Pseudo-Voigt
Crystal data top
CuNa1.57664O2β = 111.9698 (5)°
Mr = 661.6V = 121.73 (1) Å3
Monoclinic, C2/m(0β0)s0†Z = 2
q = 0.78832b*‡Synchrotron radiation, λ = 0.65046 Å
a = 8.24153 (4) ÅT = 293 K
b = 2.78589 (2) Å?, ? × ? × ? mm
c = 5.71687 (3) Å
† Symmetry operations: (1) x1, x2, x3, x4; (2) −x1, x2, −x3, 1/2+x4; (3) −x1, −x2, −x3, −x4; (4) x1, −x2, x3, 1/2−x4; (5) 1/2+x1, 1/2+x2, x3, x4; (6) 1/2−x1, 1/2+x2, −x3, 1/2+x4; (7) 1/2−x1, 1/2−x2, −x3, −x4; (8) 1/2+x1, 1/2−x2, x3, 1/2−x4.

texobject1427800956.png; texobject1427800957.png

Data collection top
2θmin = 5°, 2θmax = 43.404°, 2θstep = 0.004°
Refinement top
Rp = 0.0759602 data points
Rwp = 0.10136 parameters
Rexp = 0.0500 restraints
R(F) = 0.048(Δ/σ)max = 0.295
χ2 = NOT FOUND
Fractional atomic coordinates and isotropic or equivalent isotropic displacement parameters (Å2) top
xyzUiso*/Ueq
Cu100.500.0038 (2)*
O10.0493 (3)00.2416 (3)0.0091 (7)*
Na10.1512 (3)0.250.3832 (4)0.0141 (6)*
Bond lengths (Å) top
AverageMinimumMaximum
Cu1—Cu1i2.790 (2)2.763 (4)2.816 (4)
Cu1—Cu1ii2.790 (2)2.764 (4)2.816 (4)
Cu1—Cu1iii4.3546 (15)4.217 (2)4.494 (2)
Cu1—Cu1iv4.3543 (15)4.217 (2)4.494 (2)
Cu1—Cu1v4.3551 (15)4.217 (2)4.494 (2)
Cu1—Cu1vi4.3554 (15)4.217 (2)4.494 (2)
Cu1—O1i4.376 (8)4.314 (6)4.490 (11)
Cu1—O1vii4.714 (9)4.599 (10)4.791 (5)
Cu1—O11.899 (8)1.841 (7)1.961 (8)
Cu1—O1viii4.715 (9)4.599 (9)4.791 (5)
Cu1—O1ii1.898 (8)1.841 (7)1.962 (8)
Cu1—O1ix4.376 (8)4.314 (6)4.490 (11)
Cu1—O1x4.532 (6)4.271 (12)4.878 (12)
Cu1—O1iv4.427 (9)4.392 (18)4.476 (18)
Cu1—O1v5.050 (8)4.908 (7)5.260 (7)
Cu1—O1vi4.214 (8)3.989 (16)4.391 (15)
Cu1—O1xi5.051 (8)4.908 (7)5.260 (7)
Cu1—O1xii4.376 (8)4.314 (6)4.490 (11)
Cu1—O1xiii1.899 (8)1.841 (7)1.961 (8)
Cu1—O1xiv4.715 (9)4.599 (10)4.791 (5)
Cu1—O1xv1.898 (8)1.841 (7)1.962 (8)
Cu1—O1xvi4.714 (9)4.599 (9)4.791 (5)
Cu1—O1xvii4.377 (8)4.314 (6)4.490 (11)
Cu1—O1xviii5.049 (8)4.908 (7)5.260 (7)
Cu1—O1xix4.213 (8)3.989 (16)4.391 (15)
Cu1—O1xx5.049 (8)4.908 (7)5.260 (7)
Cu1—O1xxi4.427 (9)4.392 (18)4.476 (18)
Cu1—O1xxii4.534 (6)4.271 (12)4.878 (12)
Cu1—Na1vii816.4 (11)3.084 (4)5.162 (6)
Cu1—Na1viii734.9 (11)3.075 (3)4.248 (8)
Cu1—Na1xxiii1159.5 (10)4.232 (5)6.972 (6)
Cu1—Na1i1317.8 (11)4.952 (7)8.515 (5)
Cu1—Na1755.7 (13)2.902 (5)4.952 (7)
Cu1—Na1ii670.3 (14)2.899 (5)4.058 (5)
Cu1—Na1ix1120.9 (11)4.058 (5)6.861 (6)
Cu1—Na1vi770.7 (10)3.127 (4)5.181 (5)
Cu1—Na1xi648.8 (10)2.641 (9)4.233 (5)
Cu1—Na1xxiv1146.2 (9)4.233 (5)7.515 (6)
Cu1—Na1xiii1011.4 (11)3.834 (5)6.324 (5)
Cu1—Na1xv630.0 (13)2.899 (5)3.834 (5)
Cu1—Na1xvii863.0 (13)3.201 (10)5.922 (5)
Cu1—Na1xiv1055.5 (10)4.172 (5)6.565 (5)
Cu1—Na1xvi697.5 (11)3.075 (3)4.172 (5)
Cu1—Na1xxv919.1 (11)3.738 (8)6.149 (5)
Cu1—Na1xix995.9 (9)3.365 (4)6.564 (5)
Cu1—Na1xx632.8 (10)2.641 (9)3.374 (6)
Cu1—Na1xxvi854.5 (10)3.183 (9)5.329 (5)
O1—O1i2.789 (11)2.668 (14)3.008 (15)
O1—O1ii2.789 (11)2.668 (14)3.008 (15)
O1—O1iii4.355 (13)4.267 (11)4.484 (16)
O1—O1iv4.354 (13)4.267 (11)4.484 (16)
O1—O1v4.355 (13)4.267 (11)4.484 (16)
O1—O1vi4.355 (13)4.267 (11)4.484 (16)
O1—O1xii3.795 (11)3.729 (13)3.862 (12)
O1—O1xxvii4.354 (13)4.116 (11)4.474 (15)
O1—O1xiii2.575 (11)2.50 (2)2.654 (14)
O1—O1xiv3.346 (13)3.301 (17)3.39 (2)
O1—O1xv3.795 (11)3.729 (13)3.862 (12)
O1—O1xvi4.353 (13)4.116 (11)4.474 (15)
O1—O1xviii4.871 (11)4.633 (13)5.051 (13)
O1—O1xix4.871 (11)4.633 (13)5.051 (13)
O1—O1xxviii3.783 (10)3.640 (8)4.067 (12)
O1—O1xxii3.784 (10)3.640 (8)4.067 (12)
O1—Na1vii952.7 (19)4.578 (14)5.444 (11)
O1—Na1viii1076 (2)4.578 (14)6.169 (9)
O1—Na1i998 (2)3.507 (11)6.988 (7)
O1—Na1495 (2)2.230 (11)3.507 (11)
O1—Na1ii695 (2)2.257 (12)4.620 (8)
O1—Na1ix1300.7 (18)4.620 (8)7.808 (8)
O1—Na1v1003.5 (19)3.709 (9)6.400 (7)
O1—Na1vi542 (2)2.189 (7)3.709 (9)
O1—Na1xi706.7 (19)2.189 (7)4.981 (8)
O1—Na1xxiv1344.1 (18)4.981 (8)8.486 (8)
O1—Na1xiii980 (2)4.193 (12)5.889 (10)
O1—Na1xv841 (2)3.93 (2)4.693 (14)
O1—Na1xvii1208 (2)4.693 (14)7.635 (9)
O1—Na1xxvii1293.3 (17)4.749 (8)7.933 (8)
O1—Na1xiv680.0 (19)2.250 (10)4.749 (8)
O1—Na1xvi481.1 (19)2.220 (9)3.246 (9)
O1—Na1xxv989.6 (18)3.246 (9)6.769 (7)
O1—Na1xix941.6 (17)3.799 (7)5.978 (8)
O1—Na1xx826.8 (17)3.756 (15)4.811 (7)
O1—Na1xxvi1184.5 (18)4.781 (10)7.023 (8)
O1—Na1xxix1062 (2)4.480 (8)6.457 (10)
O1—Na1xxx960 (2)4.480 (8)5.339 (14)
O1—Na1xxii1091 (2)4.625 (10)6.823 (9)
O1—Na1xxxi962.3 (19)4.446 (6)5.236 (11)
Na1—Na1i3.553 (7)3.059 (10)4.233 (10)
Na1—Na1ii3.549 (7)3.059 (10)4.233 (10)
Na1—Na1iii5.444 (9)4.811 (11)5.758 (7)
Na1—Na1iv4.163 (9)3.639 (18)4.617 (17)
Na1—Na1xxxii5.444 (9)4.811 (11)5.758 (7)
Na1—Na1v5.444 (9)4.811 (11)5.758 (7)
Na1—Na1vi4.161 (9)3.639 (18)4.617 (17)
Na1—Na1xi5.440 (9)4.811 (11)5.758 (7)
Na1—Na1xiv2.982 (8)2.550 (6)3.197 (9)
Na1—Na1xvi2.980 (8)2.550 (6)3.197 (9)
Na1—Na1xix4.453 (8)4.347 (9)4.534 (7)
Na1—Na1xxix3.064 (10)3.029 (9)3.088 (9)
Na1—Na1xx4.453 (8)4.347 (9)4.534 (7)
Na1—Na1xxx3.064 (10)3.029 (9)3.088 (9)
Symmetry codes: (i) x1, x21, x3, x4; (ii) x1, x2+1, x3, x4; (iii) x11/2, x21/2, x3, x4; (iv) x11/2, x2+1/2, x3, x4; (v) x1+1/2, x21/2, x3, x4; (vi) x1+1/2, x2+1/2, x3, x4; (vii) x1, x2, x31, x4; (viii) x1, x2+1, x31, x4; (ix) x1, x2+2, x3, x4; (x) x11/2, x2+1/2, x31, x4; (xi) x1+1/2, x2+3/2, x3, x4; (xii) x1, x21, x3, x4; (xiii) x1, x2, x3, x4; (xiv) x1, x2, x3+1, x4; (xv) x1, x2+1, x3, x4; (xvi) x1, x2+1, x3+1, x4; (xvii) x1, x2+2, x3, x4; (xviii) x11/2, x21/2, x3, x4; (xix) x11/2, x2+1/2, x3, x4; (xx) x11/2, x2+3/2, x3, x4; (xxi) x1+1/2, x2+1/2, x3, x4; (xxii) x1+1/2, x2+1/2, x3+1, x4; (xxiii) x1, x2+2, x31, x4; (xxiv) x1+1/2, x2+5/2, x3, x4; (xxv) x1, x2+2, x3+1, x4; (xxvi) x11/2, x2+5/2, x3, x4; (xxvii) x1, x21, x3+1, x4; (xxviii) x1+1/2, x21/2, x3+1, x4; (xxix) x11/2, x2+1/2, x3+1, x4; (xxx) x11/2, x2+3/2, x3+1, x4; (xxxi) x1+1/2, x2+3/2, x3+1, x4; (xxxii) x11/2, x2+3/2, x3, x4.
(II) top
Crystal data top
Cu5Na8O10V = 121.73 Å3
Mr = 661.6Z = 1
Monoclinic, C2/m(0β0)s0†F(000) = 125
q = 0.80000b*‡Dx = 9.023 Mg m3
a = 8.2417 ÅX-ray radiation, λ = 0.70926 Å
b = 2.7859 ŵ = 22.32 mm1
c = 5.7167 ÅT = 293 K
β = 111.9709° × × mm
† Symmetry operations: (1) x1, x2, x3, x4; (2) −x1, x2, −x3, 1/2+x4; (3) −x1, −x2, −x3, −x4; (4) x1, −x2, x3, 1/2−x4; (5) 1/2+x1, 1/2+x2, x3, x4; (6) 1/2−x1, 1/2+x2, −x3, 1/2+x4; (7) 1/2−x1, 1/2−x2, −x3, −x4; (8) 1/2+x1, 1/2−x2, x3, 1/2−x4.

texobject1427800958.png; texobject1427800959.png

Data collection top
5656 independent reflectionsk = ??
4523 reflections with I > 3σ(I)l = ??
h = ??
Refinement top
Refinement on F5656 reflections
R[F2 > 2σ(F2)] = 0.035107 parameters
wR(F2) = 0.033Weighting scheme based on measured s.u.'s w = 1/σ2(F)
S = 2.95(Δ/σ)max = 0.002
Crystal data top
Cu5Na8O10β = 111.9709°
Mr = 661.6V = 121.73 Å3
Monoclinic, C2/m(0β0)s0†Z = 1
q = 0.80000b*‡X-ray radiation, λ = 0.70926 Å
a = 8.2417 ŵ = 22.32 mm1
b = 2.7859 ÅT = 293 K
c = 5.7167 Å × × mm
† Symmetry operations: (1) x1, x2, x3, x4; (2) −x1, x2, −x3, 1/2+x4; (3) −x1, −x2, −x3, −x4; (4) x1, −x2, x3, 1/2−x4; (5) 1/2+x1, 1/2+x2, x3, x4; (6) 1/2−x1, 1/2+x2, −x3, 1/2+x4; (7) 1/2−x1, 1/2−x2, −x3, −x4; (8) 1/2+x1, 1/2−x2, x3, 1/2−x4.

texobject1427800960.png; texobject1427800961.png

Data collection top
5656 independent reflections4523 reflections with I > 3σ(I)
Refinement top
R[F2 > 2σ(F2)] = 0.0355656 reflections
wR(F2) = 0.033107 parameters
S = 2.95
Fractional atomic coordinates and isotropic or equivalent isotropic displacement parameters (Å2) top
xyzUiso*/Ueq
Cu100.500.0107
O10.0520400.2422770.0161
Na10.1541820.250.3778550.0268
Atomic displacement parameters (Å2) top
U11U22U33U12U13U23
Cu10.0126590.0109290.00816500.0033390
O10.0230030.0148620.00942900.0049930
Na10.0216590.0428640.01600400.0072360
Bond lengths (Å) top
AverageMinimumMaximum
Cu1—Cu1i2.78952.75772.8181
Cu1—Cu1ii2.78952.75772.8181
Cu1—O11.89911.85791.9298
Cu1—O1ii1.89911.85791.9298
Cu1—Na1iii17.57453.05994.1968
Cu1—Na120.36213.21155.1372
Cu1—Na1ii15.73152.89613.776
Cu1—Na1iv20.53053.25285.1985
Cu1—Na1v15.63252.7383.3056
Cu1—O111.90041.83321.9504
Cu1—O11ii1.90041.83321.9504
Cu1—Na11ii16.25162.89583.8568
Cu1—Na11vi19.31483.07494.7487
Cu1—Na11vii18.00093.10544.1987
Cu1—Na11viii15.61022.80673.4583
Cu1—Na11ix19.44053.26275.1377
O1—O1i2.78862.7092.8845
O1—O1ii2.78862.7092.8845
O1—Na113.40192.29483.6968
O1—Na1ii15.50592.32424.3988
O1—Na1iv14.36952.29623.7564
O1—Na1v15.81042.29623.8109
O1—O112.57762.51762.654
O1—O11x3.36533.34823.3886
O1—Na11x18.68812.35514.8118
O1—Na11vii11.61552.29792.3551
O1—Na11xi21.73723.00065.4042
Na1—Na1i3.49323.07933.9071
Na1—Na1ii3.49323.07933.9071
Na1—O11x9.38422.27722.4236
Na1—O11vii10.72872.33013.6216
Na1—Na11x2.99942.79453.1618
Na1—Na11vii2.99942.79453.1618
Na1—Na11xii3.05052.99113.1095
Na1—Na11xiii3.05052.99113.1095
O11—O11i2.7922.69483
O11—O11ii2.7922.69483
O11—Na1119.0252.56644.7373
O11—Na11ii11.90682.31152.5664
O11—Na11vi22.01613.17555.5575
O11—Na11xiv19.48682.77145.1699
O11—Na11viii12.05322.28312.7714
Na11—Na11i3.49613.07333.8669
Na11—Na11ii3.49613.07333.8669
Symmetry codes: (i) x1, x21, x3, x4; (ii) x1, x2+1, x3, x4; (iii) x1, x2+1, x31, x4; (iv) x1+1/2, x2+1/2, x3, x4; (v) x1+1/2, x2+3/2, x3, x4; (vi) x1, x2+2, x3, x4; (vii) x1, x2+1, x3+1, x4; (viii) x11/2, x2+3/2, x3, x4; (ix) x11/2, x2+5/2, x3, x4; (x) x1, x2, x3+1, x4; (xi) x1, x2+2, x3+1, x4; (xii) x11/2, x2+1/2, x3+1, x4; (xiii) x11/2, x2+3/2, x3+1, x4; (xiv) x11/2, x2+1/2, x3, x4.
(III) top
Crystal data top
CuNa1.61689O2V = 122.11 (1) Å3
Mr = 661.6Z = 2
Monoclinic, C2/m(0β0)s0†F(000) = 126
q = 0.80844(3)b*‡Dx = 8.994 Mg m3
a = 8.23682 (15) ÅX-ray radiation, λ = 1.54059 Å
b = 2.79269 (4) ÅT = 293 K
c = 5.71224 (10) Å?, ? × ? × ? mm
β = 111.6696 (9)°
† Symmetry operations: (1) x1, x2, x3, x4; (2) −x1, x2, −x3, 1/2+x4; (3) −x1, −x2, −x3, −x4; (4) x1, −x2, x3, 1/2−x4; (5) 1/2+x1, 1/2+x2, x3, x4; (6) 1/2−x1, 1/2+x2, −x3, 1/2+x4; (7) 1/2−x1, 1/2−x2, −x3, −x4; (8) 1/2+x1, 1/2−x2, x3, 1/2−x4.

texobject1427800962.png; texobject1427800963.png

Data collection top
2θmin = 9.987°, 2θmax = 79.977°, 2θstep = 0.01°
Refinement top
Rp = 0.094Profile function: Pseudo-Voigt
Rwp = 0.12237 parameters
Rexp = 0.063Weighting scheme based on measured s.u.'s
R(F) = 0.056(Δ/σ)max = 0.049
χ2 = NOT FOUNDBackground function: 5 Legendre polynoms
7000 data pointsPreferred orientation correction: none
Crystal data top
CuNa1.61689O2β = 111.6696 (9)°
Mr = 661.6V = 122.11 (1) Å3
Monoclinic, C2/m(0β0)s0†Z = 2
q = 0.80844(3)b*‡X-ray radiation, λ = 1.54059 Å
a = 8.23682 (15) ÅT = 293 K
b = 2.79269 (4) Å?, ? × ? × ? mm
c = 5.71224 (10) Å
† Symmetry operations: (1) x1, x2, x3, x4; (2) −x1, x2, −x3, 1/2+x4; (3) −x1, −x2, −x3, −x4; (4) x1, −x2, x3, 1/2−x4; (5) 1/2+x1, 1/2+x2, x3, x4; (6) 1/2−x1, 1/2+x2, −x3, 1/2+x4; (7) 1/2−x1, 1/2−x2, −x3, −x4; (8) 1/2+x1, 1/2−x2, x3, 1/2−x4.

texobject1427800964.png; texobject1427800965.png

Data collection top
2θmin = 9.987°, 2θmax = 79.977°, 2θstep = 0.01°
Refinement top
Rp = 0.094χ2 = NOT FOUND
Rwp = 0.1227000 data points
Rexp = 0.06337 parameters
R(F) = 0.056
Fractional atomic coordinates and isotropic or equivalent isotropic displacement parameters (Å2) top
xyzUiso*/Ueq
Cu100.500.0024 (4)*
O10.0526 (3)00.2465 (5)0.0208 (10)*
Na10.1566 (4)0.250.3717 (5)0.0183 (9)*
Bond lengths (Å) top
AverageMinimumMaximum
Cu1—Cu1i2.797 (3)2.781 (4)2.812 (4)
Cu1—Cu1ii2.796 (3)2.781 (4)2.812 (4)
Cu1—O11.919 (10)1.857 (12)1.982 (10)
Cu1—O1ii1.918 (10)1.857 (12)1.982 (10)
Cu1—O1iii1.919 (10)1.857 (12)1.982 (10)
Cu1—O1iv1.918 (10)1.857 (12)1.982 (10)
Cu1—Na1376.3 (8)2.876 (8)4.854 (7)
Cu1—Na1ii331.7 (8)2.876 (8)4.020 (9)
Cu1—Na1v318.7 (6)2.548 (10)3.927 (6)
Cu1—Na1iv312.9 (8)2.876 (8)3.805 (7)
Cu1—Na1vi313.0 (6)2.548 (10)3.366 (6)
O1—O1i2.795 (13)2.733 (16)2.915 (16)
O1—O1ii2.794 (13)2.733 (16)2.915 (16)
O1—O1iii2.625 (14)2.54 (3)2.711 (18)
O1—Na1248.1 (14)2.175 (13)3.384 (12)
O1—Na1ii345.2 (13)2.214 (14)4.592 (10)
O1—Na1vii266.2 (12)2.147 (9)3.710 (11)
O1—Na1v346.0 (12)2.147 (9)4.741 (9)
O1—Na1viii339.6 (12)2.231 (13)4.689 (9)
O1—Na1ix243.6 (12)2.210 (12)3.264 (11)
Na1—Na1viii3.038 (9)2.656 (7)3.228 (10)
Na1—Na1ix3.036 (9)2.656 (7)3.228 (10)
Symmetry codes: (i) x1, x21, x3, x4; (ii) x1, x2+1, x3, x4; (iii) x1, x2, x3, x4; (iv) x1, x2+1, x3, x4; (v) x1+1/2, x2+3/2, x3, x4; (vi) x11/2, x2+3/2, x3, x4; (vii) x1+1/2, x2+1/2, x3, x4; (viii) x1, x2, x3+1, x4; (ix) x1, x2+1, x3+1, x4.

Experimental details

(I)(II)(III)
Crystal data
Chemical formulaCuNa1.57664O2Cu5Na8O10CuNa1.61689O2
Mr661.6661.6661.6
Crystal system, space groupMonoclinic, C2/m(0β0)s0†Monoclinic, C2/m(0β0)s0‡Monoclinic, C2/m(0β0)s
Temperature (K)293293293
Wave vectorsq = 0.78832b*††q = 0.80000b*‡‡q = 0.80844(3)b*§§
a, b, c (Å)8.24153 (4), 2.78589 (2), 5.71687 (3)8.2417, 2.7859, 5.71678.23682 (15), 2.79269 (4), 5.71224 (10)
β (°) 111.9698 (5) 111.9709 111.6696 (9)
V3)121.73 (1)121.73122.11 (1)
Z212
Radiation typeSynchrotron, λ = 0.65046 ÅX-ray, λ = 0.70926 ÅX-ray, λ = 1.54059 Å
µ (mm1)22.32
Specimen shape, size (mm)?, ? × ? × ? × × ?, ? × ? × ?
Data collection
Diffractometer???
Specimen mounting??
Data collection mode??
Data collection method???
Absorption correction
No. of measured, independent and
observed reflections
?, 5656, 4523
Rint?
θ values (°)2θmin = 5 2θmax = 43.404 2θstep = 0.004θmax = ?2θmin = 9.987 2θmax = 79.977 2θstep = 0.01
Refinement
R factors and goodness of fitRp = 0.075, Rwp = 0.101, Rexp = 0.050, R(F) = 0.048, χ2 = NOT FOUNDR[F2 > 2σ(F2)] = 0.035, wR(F2) = 0.033, S = 2.95Rp = 0.094, Rwp = 0.122, Rexp = 0.063, R(F) = 0.056, χ2 = NOT FOUND
No. of reflections/data points960256567000
No. of parameters3610737
No. of restraints0??
(Δ/σ)max0.2950.0020.049
Δρmax, Δρmin (e Å3)?, ?

† Symmetry operations: (1) x1, x2, x3, x4; (2) −x1, x2, −x3, 1/2+x4; (3) −x1, −x2, −x3, −x4; (4) x1, −x2, x3, 1/2−x4; (5) 1/2+x1, 1/2+x2, x3, x4; (6) 1/2−x1, 1/2+x2, −x3, 1/2+x4; (7) 1/2−x1, 1/2−x2, −x3, −x4; (8) 1/2+x1, 1/2−x2, x3, 1/2−x4.

‡ Symmetry operations: (1) x1, x2, x3, x4; (2) −x1, x2, −x3, 1/2+x4; (3) −x1, −x2, −x3, −x4; (4) x1, −x2, x3, 1/2−x4; (5) 1/2+x1, 1/2+x2, x3, x4; (6) 1/2−x1, 1/2+x2, −x3, 1/2+x4; (7) 1/2−x1, 1/2−x2, −x3, −x4; (8) 1/2+x1, 1/2−x2, x3, 1/2−x4.

§ Symmetry operations: (1) x1, x2, x3, x4; (2) −x1, x2, −x3, 1/2+x4; (3) −x1, −x2, −x3, −x4; (4) x1, −x2, x3, 1/2−x4; (5) 1/2+x1, 1/2+x2, x3, x4; (6) 1/2−x1, 1/2+x2, −x3, 1/2+x4; (7) 1/2−x1, 1/2−x2, −x3, −x4; (8) 1/2+x1, 1/2−x2, x3, 1/2−x4.

†† texobject1427800966.png; texobject1427800967.png

‡‡ texobject1427800968.png; texobject1427800969.png

§§ texobject1427800970.png; texobject1427800971.png

Computer programs: (Jana2000; Petricek and Dusek, 2000), (Diamond 3, Brandenburg, 2004).

Selected bond lengths (Å) for (I) top
AverageMinimumMaximum
Cu1—Cu1i2.790 (2)2.763 (4)2.816 (4)
Cu1—Cu1ii2.790 (2)2.764 (4)2.816 (4)
Cu1—Cu1iii4.3546 (15)4.217 (2)4.494 (2)
Cu1—Cu1iv4.3543 (15)4.217 (2)4.494 (2)
Cu1—Cu1v4.3551 (15)4.217 (2)4.494 (2)
Cu1—Cu1vi4.3554 (15)4.217 (2)4.494 (2)
Cu1—O1i4.376 (8)4.314 (6)4.490 (11)
Cu1—O1vii4.714 (9)4.599 (10)4.791 (5)
Cu1—O11.899 (8)1.841 (7)1.961 (8)
Cu1—O1viii4.715 (9)4.599 (9)4.791 (5)
Cu1—O1ii1.898 (8)1.841 (7)1.962 (8)
Cu1—O1ix4.376 (8)4.314 (6)4.490 (11)
Cu1—O1x4.532 (6)4.271 (12)4.878 (12)
Cu1—O1iv4.427 (9)4.392 (18)4.476 (18)
Cu1—O1v5.050 (8)4.908 (7)5.260 (7)
Cu1—O1vi4.214 (8)3.989 (16)4.391 (15)
Cu1—O1xi5.051 (8)4.908 (7)5.260 (7)
Cu1—O1xii4.376 (8)4.314 (6)4.490 (11)
Cu1—O1xiii1.899 (8)1.841 (7)1.961 (8)
Cu1—O1xiv4.715 (9)4.599 (10)4.791 (5)
Cu1—O1xv1.898 (8)1.841 (7)1.962 (8)
Cu1—O1xvi4.714 (9)4.599 (9)4.791 (5)
Cu1—O1xvii4.377 (8)4.314 (6)4.490 (11)
Cu1—O1xviii5.049 (8)4.908 (7)5.260 (7)
Cu1—O1xix4.213 (8)3.989 (16)4.391 (15)
Cu1—O1xx5.049 (8)4.908 (7)5.260 (7)
Cu1—O1xxi4.427 (9)4.392 (18)4.476 (18)
Cu1—O1xxii4.534 (6)4.271 (12)4.878 (12)
Cu1—Na1vii816.4 (11)3.084 (4)5.162 (6)
Cu1—Na1viii734.9 (11)3.075 (3)4.248 (8)
Cu1—Na1xxiii1159.5 (10)4.232 (5)6.972 (6)
Cu1—Na1i1317.8 (11)4.952 (7)8.515 (5)
Cu1—Na1755.7 (13)2.902 (5)4.952 (7)
Cu1—Na1ii670.3 (14)2.899 (5)4.058 (5)
Cu1—Na1ix1120.9 (11)4.058 (5)6.861 (6)
Cu1—Na1vi770.7 (10)3.127 (4)5.181 (5)
Cu1—Na1xi648.8 (10)2.641 (9)4.233 (5)
Cu1—Na1xxiv1146.2 (9)4.233 (5)7.515 (6)
Cu1—Na1xiii1011.4 (11)3.834 (5)6.324 (5)
Cu1—Na1xv630.0 (13)2.899 (5)3.834 (5)
Cu1—Na1xvii863.0 (13)3.201 (10)5.922 (5)
Cu1—Na1xiv1055.5 (10)4.172 (5)6.565 (5)
Cu1—Na1xvi697.5 (11)3.075 (3)4.172 (5)
Cu1—Na1xxv919.1 (11)3.738 (8)6.149 (5)
Cu1—Na1xix995.9 (9)3.365 (4)6.564 (5)
Cu1—Na1xx632.8 (10)2.641 (9)3.374 (6)
Cu1—Na1xxvi854.5 (10)3.183 (9)5.329 (5)
O1—O1i2.789 (11)2.668 (14)3.008 (15)
O1—O1ii2.789 (11)2.668 (14)3.008 (15)
O1—O1iii4.355 (13)4.267 (11)4.484 (16)
O1—O1iv4.354 (13)4.267 (11)4.484 (16)
O1—O1v4.355 (13)4.267 (11)4.484 (16)
O1—O1vi4.355 (13)4.267 (11)4.484 (16)
O1—O1xii3.795 (11)3.729 (13)3.862 (12)
O1—O1xxvii4.354 (13)4.116 (11)4.474 (15)
O1—O1xiii2.575 (11)2.50 (2)2.654 (14)
O1—O1xiv3.346 (13)3.301 (17)3.39 (2)
O1—O1xv3.795 (11)3.729 (13)3.862 (12)
O1—O1xvi4.353 (13)4.116 (11)4.474 (15)
O1—O1xviii4.871 (11)4.633 (13)5.051 (13)
O1—O1xix4.871 (11)4.633 (13)5.051 (13)
O1—O1xxviii3.783 (10)3.640 (8)4.067 (12)
O1—O1xxii3.784 (10)3.640 (8)4.067 (12)
O1—Na1vii952.7 (19)4.578 (14)5.444 (11)
O1—Na1viii1076 (2)4.578 (14)6.169 (9)
O1—Na1i998 (2)3.507 (11)6.988 (7)
O1—Na1495 (2)2.230 (11)3.507 (11)
O1—Na1ii695 (2)2.257 (12)4.620 (8)
O1—Na1ix1300.7 (18)4.620 (8)7.808 (8)
O1—Na1v1003.5 (19)3.709 (9)6.400 (7)
O1—Na1vi542 (2)2.189 (7)3.709 (9)
O1—Na1xi706.7 (19)2.189 (7)4.981 (8)
O1—Na1xxiv1344.1 (18)4.981 (8)8.486 (8)
O1—Na1xiii980 (2)4.193 (12)5.889 (10)
O1—Na1xv841 (2)3.93 (2)4.693 (14)
O1—Na1xvii1208 (2)4.693 (14)7.635 (9)
O1—Na1xxvii1293.3 (17)4.749 (8)7.933 (8)
O1—Na1xiv680.0 (19)2.250 (10)4.749 (8)
O1—Na1xvi481.1 (19)2.220 (9)3.246 (9)
O1—Na1xxv989.6 (18)3.246 (9)6.769 (7)
O1—Na1xix941.6 (17)3.799 (7)5.978 (8)
O1—Na1xx826.8 (17)3.756 (15)4.811 (7)
O1—Na1xxvi1184.5 (18)4.781 (10)7.023 (8)
O1—Na1xxix1062 (2)4.480 (8)6.457 (10)
O1—Na1xxx960 (2)4.480 (8)5.339 (14)
O1—Na1xxii1091 (2)4.625 (10)6.823 (9)
O1—Na1xxxi962.3 (19)4.446 (6)5.236 (11)
Na1—Na1i3.553 (7)3.059 (10)4.233 (10)
Na1—Na1ii3.549 (7)3.059 (10)4.233 (10)
Na1—Na1iii5.444 (9)4.811 (11)5.758 (7)
Na1—Na1iv4.163 (9)3.639 (18)4.617 (17)
Na1—Na1xxxii5.444 (9)4.811 (11)5.758 (7)
Na1—Na1v5.444 (9)4.811 (11)5.758 (7)
Na1—Na1vi4.161 (9)3.639 (18)4.617 (17)
Na1—Na1xi5.440 (9)4.811 (11)5.758 (7)
Na1—Na1xiv2.982 (8)2.550 (6)3.197 (9)
Na1—Na1xvi2.980 (8)2.550 (6)3.197 (9)
Na1—Na1xix4.453 (8)4.347 (9)4.534 (7)
Na1—Na1xxix3.064 (10)3.029 (9)3.088 (9)
Na1—Na1xx4.453 (8)4.347 (9)4.534 (7)
Na1—Na1xxx3.064 (10)3.029 (9)3.088 (9)
Symmetry codes: (i) x1, x21, x3, x4; (ii) x1, x2+1, x3, x4; (iii) x11/2, x21/2, x3, x4; (iv) x11/2, x2+1/2, x3, x4; (v) x1+1/2, x21/2, x3, x4; (vi) x1+1/2, x2+1/2, x3, x4; (vii) x1, x2, x31, x4; (viii) x1, x2+1, x31, x4; (ix) x1, x2+2, x3, x4; (x) x11/2, x2+1/2, x31, x4; (xi) x1+1/2, x2+3/2, x3, x4; (xii) x1, x21, x3, x4; (xiii) x1, x2, x3, x4; (xiv) x1, x2, x3+1, x4; (xv) x1, x2+1, x3, x4; (xvi) x1, x2+1, x3+1, x4; (xvii) x1, x2+2, x3, x4; (xviii) x11/2, x21/2, x3, x4; (xix) x11/2, x2+1/2, x3, x4; (xx) x11/2, x2+3/2, x3, x4; (xxi) x1+1/2, x2+1/2, x3, x4; (xxii) x1+1/2, x2+1/2, x3+1, x4; (xxiii) x1, x2+2, x31, x4; (xxiv) x1+1/2, x2+5/2, x3, x4; (xxv) x1, x2+2, x3+1, x4; (xxvi) x11/2, x2+5/2, x3, x4; (xxvii) x1, x21, x3+1, x4; (xxviii) x1+1/2, x21/2, x3+1, x4; (xxix) x11/2, x2+1/2, x3+1, x4; (xxx) x11/2, x2+3/2, x3+1, x4; (xxxi) x1+1/2, x2+3/2, x3+1, x4; (xxxii) x11/2, x2+3/2, x3, x4.
Selected bond lengths (Å) for (II) top
AverageMinimumMaximum
Cu1—Cu1i2.78952.75772.8181
Cu1—Cu1ii2.78952.75772.8181
Cu1—O11.89911.85791.9298
Cu1—O1ii1.89911.85791.9298
Cu1—Na1iii17.57453.05994.1968
Cu1—Na120.36213.21155.1372
Cu1—Na1ii15.73152.89613.776
Cu1—Na1iv20.53053.25285.1985
Cu1—Na1v15.63252.7383.3056
Cu1—O111.90041.83321.9504
Cu1—O11ii1.90041.83321.9504
Cu1—Na11ii16.25162.89583.8568
Cu1—Na11vi19.31483.07494.7487
Cu1—Na11vii18.00093.10544.1987
Cu1—Na11viii15.61022.80673.4583
Cu1—Na11ix19.44053.26275.1377
O1—O1i2.78862.7092.8845
O1—O1ii2.78862.7092.8845
O1—Na113.40192.29483.6968
O1—Na1ii15.50592.32424.3988
O1—Na1iv14.36952.29623.7564
O1—Na1v15.81042.29623.8109
O1—O112.57762.51762.654
O1—O11x3.36533.34823.3886
O1—Na11x18.68812.35514.8118
O1—Na11vii11.61552.29792.3551
O1—Na11xi21.73723.00065.4042
Na1—Na1i3.49323.07933.9071
Na1—Na1ii3.49323.07933.9071
Na1—O11x9.38422.27722.4236
Na1—O11vii10.72872.33013.6216
Na1—Na11x2.99942.79453.1618
Na1—Na11vii2.99942.79453.1618
Na1—Na11xii3.05052.99113.1095
Na1—Na11xiii3.05052.99113.1095
O11—O11i2.7922.69483
O11—O11ii2.7922.69483
O11—Na1119.0252.56644.7373
O11—Na11ii11.90682.31152.5664
O11—Na11vi22.01613.17555.5575
O11—Na11xiv19.48682.77145.1699
O11—Na11viii12.05322.28312.7714
Na11—Na11i3.49613.07333.8669
Na11—Na11ii3.49613.07333.8669
Symmetry codes: (i) x1, x21, x3, x4; (ii) x1, x2+1, x3, x4; (iii) x1, x2+1, x31, x4; (iv) x1+1/2, x2+1/2, x3, x4; (v) x1+1/2, x2+3/2, x3, x4; (vi) x1, x2+2, x3, x4; (vii) x1, x2+1, x3+1, x4; (viii) x11/2, x2+3/2, x3, x4; (ix) x11/2, x2+5/2, x3, x4; (x) x1, x2, x3+1, x4; (xi) x1, x2+2, x3+1, x4; (xii) x11/2, x2+1/2, x3+1, x4; (xiii) x11/2, x2+3/2, x3+1, x4; (xiv) x11/2, x2+1/2, x3, x4.
Selected bond lengths (Å) for (III) top
AverageMinimumMaximum
Cu1—Cu1i2.797 (3)2.781 (4)2.812 (4)
Cu1—Cu1ii2.796 (3)2.781 (4)2.812 (4)
Cu1—O11.919 (10)1.857 (12)1.982 (10)
Cu1—O1ii1.918 (10)1.857 (12)1.982 (10)
Cu1—O1iii1.919 (10)1.857 (12)1.982 (10)
Cu1—O1iv1.918 (10)1.857 (12)1.982 (10)
Cu1—Na1376.3 (8)2.876 (8)4.854 (7)
Cu1—Na1ii331.7 (8)2.876 (8)4.020 (9)
Cu1—Na1v318.7 (6)2.548 (10)3.927 (6)
Cu1—Na1iv312.9 (8)2.876 (8)3.805 (7)
Cu1—Na1vi313.0 (6)2.548 (10)3.366 (6)
O1—O1i2.795 (13)2.733 (16)2.915 (16)
O1—O1ii2.794 (13)2.733 (16)2.915 (16)
O1—O1iii2.625 (14)2.54 (3)2.711 (18)
O1—Na1248.1 (14)2.175 (13)3.384 (12)
O1—Na1ii345.2 (13)2.214 (14)4.592 (10)
O1—Na1vii266.2 (12)2.147 (9)3.710 (11)
O1—Na1v346.0 (12)2.147 (9)4.741 (9)
O1—Na1viii339.6 (12)2.231 (13)4.689 (9)
O1—Na1ix243.6 (12)2.210 (12)3.264 (11)
Na1—Na1viii3.038 (9)2.656 (7)3.228 (10)
Na1—Na1ix3.036 (9)2.656 (7)3.228 (10)
Symmetry codes: (i) x1, x21, x3, x4; (ii) x1, x2+1, x3, x4; (iii) x1, x2, x3, x4; (iv) x1, x2+1, x3, x4; (v) x1+1/2, x2+3/2, x3, x4; (vi) x11/2, x2+3/2, x3, x4; (vii) x1+1/2, x2+1/2, x3, x4; (viii) x1, x2, x3+1, x4; (ix) x1, x2+1, x3+1, x4.
 

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