Literature DB >> 22969440

Pb(6)Co(9)(TeO(6))(5).

Abstract

Pb(6)Co(9)(TeO(6))(5), hexa-lead(II) nona-cobalt(II) penta-tellur-ate(VI), is isotypic with its nickel(II) analogue. The asymmetric unit contains two Pb atoms (site symmetries .2., ..2), four Co atoms (..2, ..2, 3.., 3.2) two Te atoms (..2, 3..) and six O atoms (all in general positions), with the Te and Co sites in octa-hedral coordination environments. The crystal structure can be subdivided into two types of layers parallel to (001). The first layer at z ≃ 0.25 is made up of edge-sharing [CoO(6)] and [TeO(6)] octa-hedra, with 1/6 of the octa-hedral holes not occupied. The second layer, situated at z ≃ 0, consist of an alternating arrangement of Pb(II) atoms and of double octa-hedra that are made up from face-sharing [CoO(6)] and [TeO(6)] octa-hedra. The two types of layers are linked together through corner-sharing of [CoO(6)] and [TeO(6)] octa-hedra. The Pb(II) atoms are situated in the cavities of the framework and are stereochemically active with one-sided [4]- and [6]-coordinations, respectively.

Entities: Chemical Disease Gene

Year: 2012 PMID： 22969440 PMCID： PMC3435567 DOI： 10.1107/S1600536812037038

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

Related literature

For the isotypic nickel analogue, see: Wedel et al. (1998 ▶). Reviews on the crystal chemistry of oxotellurates(VI) and of the geometry of [CoIIO6] polyhedra are given by Levason (1997 ▶) and Wildner (1992 ▶), respectively. For Pb5TeO8, see: Artner & Weil (2012 ▶). For the bond-valence method, see: Brown (2002 ▶).

Experimental

Crystal data

Pb6Co9(TeO6)5 M = 2891.51 Hexagonal, a = 10.3915 (1) Å c = 13.6273 (2) Å V = 1274.37 (3) Å3 Z = 2 Mo Kα radiation μ = 50.89 mm−1 T = 293 K 0.07 × 0.06 × 0.05 mm

Data collection

Bruker APEXII CCD diffractometer Absorption correction: numerical (HABITUS; Herrendorf, 1997 ▶) T min = 0.123, T max = 0.200 45686 measured reflections 2262 independent reflections 1908 reflections with I > 2σ(I) R int = 0.068

Refinement

R[F 2 > 2σ(F 2)] = 0.025 wR(F 2) = 0.056 S = 1.09 2262 reflections 81 parameters Δρmax = 2.96 e Å−3 Δρmin = −2.59 e Å−3 Absolute structure: Flack (1983 ▶), 882 Friedel pairs Flack parameter: 0.134 (10) Data collection: APEX2 (Bruker, 2004 ▶); cell refinement: SAINT (Bruker, 2004 ▶); data reduction: SAINT; program(s) used to solve structure: SHELXS97 (Sheldrick, 2008 ▶); program(s) used to refine structure: SHELXL97 (Sheldrick, 2008 ▶); molecular graphics: ATOMS for Windows (Dowty, 2006 ▶); software used to prepare material for publication: publCIF (Westrip, 2010 ▶). Crystal structure: contains datablock(s) I, global. DOI: 10.1107/S1600536812037038/br2208sup1.cif Structure factors: contains datablock(s) I. DOI: 10.1107/S1600536812037038/br2208Isup2.hkl Additional supplementary materials: crystallographic information; 3D view; checkCIF report

Pb₆Co₉(TeO₆)₅	D_x = 7.535 Mg m⁻³
M_r = 2891.51	Mo Kα radiation, λ = 0.71073 Å
Hexagonal, P6₃22	Cell parameters from 6739 reflections
Hall symbol: P 6c 2c	θ = 2.8–36.8°
a = 10.3915 (1) Å	µ = 50.89 mm⁻¹
c = 13.6273 (2) Å	T = 293 K
V = 1274.37 (3) Å³	Parallelepiped, dark red
Z = 2	0.07 × 0.06 × 0.05 mm
F(000) = 2470

Bruker APEXII CCD diffractometer	2262 independent reflections
Radiation source: fine-focus sealed tube	1908 reflections with I > 2σ(I)
Graphite monochromator	R_int = 0.068
ω and φ scans	θ_max = 37.6°, θ_min = 2.3°
Absorption correction: numerical (HABITUS; Herrendorf, 1997)	h = −16→17
T_min = 0.123, T_max = 0.200	k = −17→17
45686 measured reflections	l = −22→23

Refinement on F²	Secondary atom site location: difference Fourier map
Least-squares matrix: full	w = 1/[σ²(F_o²) + (0.0244P)²] where P = (F_o² + 2F_c²)/3
R[F² > 2σ(F²)] = 0.025	(Δ/σ)_max < 0.001
wR(F²) = 0.056	Δρ_max = 2.96 e Å⁻³
S = 1.09	Δρ_min = −2.59 e Å⁻³
2262 reflections	Extinction correction: SHELXL97 (Sheldrick, 2008), Fc^*=kFc[1+0.001xFc²λ³/sin(2θ)]^-1/4
81 parameters	Extinction coefficient: 0.00019 (3)
0 restraints	Absolute structure: Flack (1983), 882 Friedel pairs
Primary atom site location: structure-invariant direct methods	Flack parameter: 0.134 (10)

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.

	x	y	z	U_iso*/U_eq
Pb1	0.26736 (3)	0.26736 (3)	0.0000	0.01216 (6)
Pb2	0.38848 (3)	1.0000	0.0000	0.01881 (8)
Te1	0.3333	0.6667	−0.09611 (4)	0.00407 (10)
Te2	0.16730 (4)	0.33460 (9)	0.2500	0.00433 (8)
Co1	0.3333	0.6667	0.11832 (9)	0.0066 (2)
Co2	0.16885 (10)	0.3377 (2)	−0.2500	0.00664 (18)
Co3	0.0000	0.0000	0.2500	0.0087 (3)
Co4	0.00992 (19)	0.50496 (10)	−0.2500	0.00566 (18)
O1	0.3366 (5)	0.3241 (5)	−0.1717 (3)	0.0077 (8)
O2	0.1726 (7)	0.5050 (6)	−0.1628 (3)	0.0083 (10)
O3	0.1702 (7)	0.1801 (6)	0.3277 (3)	0.0105 (9)
O5	0.3239 (8)	0.4818 (6)	0.3295 (3)	0.0076 (10)
O6	0.3481 (4)	0.5265 (4)	−0.0034 (4)	0.0069 (6)

	U¹¹	U²²	U³³	U¹²	U¹³	U²³
Pb1	0.01117 (9)	0.01117 (9)	0.01243 (12)	0.00429 (9)	0.00014 (9)	−0.00014 (9)
Pb2	0.01104 (9)	0.01201 (13)	0.03372 (18)	0.00601 (7)	−0.00268 (13)	−0.0054 (3)
Te1	0.00414 (14)	0.00414 (14)	0.0039 (2)	0.00207 (7)	0.000	0.000
Te2	0.00362 (13)	0.00380 (19)	0.00564 (18)	0.00190 (10)	0.0002 (4)	0.000
Co1	0.0066 (3)	0.0066 (3)	0.0066 (5)	0.00332 (16)	0.000	0.000
Co2	0.0057 (3)	0.0069 (5)	0.0077 (4)	0.0035 (2)	0.0006 (10)	0.000
Co3	0.0061 (4)	0.0061 (4)	0.0140 (7)	0.00305 (19)	0.000	0.000
Co4	0.0031 (5)	0.0045 (3)	0.0089 (4)	0.0015 (2)	0.000	−0.0002 (3)
O1	0.011 (2)	0.008 (2)	0.0048 (15)	0.0055 (14)	0.0003 (13)	−0.0022 (13)
O2	0.007 (2)	0.006 (2)	0.012 (2)	0.0022 (17)	−0.0001 (16)	−0.0034 (15)
O3	0.011 (2)	0.012 (2)	0.0077 (16)	0.0059 (15)	0.0000 (15)	0.0011 (15)
O5	0.004 (2)	0.006 (2)	0.0072 (18)	−0.0011 (18)	−0.0005 (18)	0.0009 (15)
O6	0.0058 (14)	0.0070 (14)	0.0075 (15)	0.0029 (11)	−0.001 (2)	0.002 (2)

Pb1—O6ⁱ	2.387 (4)	Te2—O3ⁱⁱⁱ	1.937 (7)
Pb1—O6	2.387 (4)	Te2—O3	1.937 (7)
Pb1—O1ⁱ	2.432 (4)	Te2—O1^xii	1.939 (5)
Pb1—O1	2.432 (4)	Te2—O1ⁱ	1.939 (5)
Pb1—O3ⁱⁱ	3.327 (7)	Co1—O5^x	2.004 (6)
Pb1—O3ⁱⁱⁱ	3.327 (7)	Co1—O5ⁱⁱⁱ	2.004 (6)
Pb1—O3^iv	3.453 (7)	Co1—O5^xiii	2.004 (6)
Pb1—O3^v	3.453 (7)	Co1—O6^vi	2.262 (5)
Pb1—Pb2^vi	3.5764 (4)	Co1—O6^vii	2.262 (5)
Pb1—Pb2^vii	3.5777 (2)	Co1—O6	2.262 (5)
Pb2—O6^viii	2.420 (3)	Co2—O2^xiv	2.090 (6)
Pb2—O6^vii	2.420 (3)	Co2—O2	2.090 (6)
Pb2—O2^ix	2.726 (5)	Co2—O3ⁱ	2.090 (8)
Pb2—O2^vi	2.726 (5)	Co2—O3^iv	2.090 (8)
Pb2—O5^x	2.727 (5)	Co2—O1	2.108 (6)
Pb2—O5^xi	2.727 (5)	Co2—O1^xiv	2.108 (6)
Pb2—O6^vi	3.155 (3)	Co3—O3^xv	2.107 (4)
Pb2—O6^ix	3.155 (3)	Co3—O3	2.107 (4)
Pb2—O3^xi	3.230 (4)	Co3—O3^xvi	2.107 (4)
Pb2—O3^x	3.230 (4)	Co3—O3^xvii	2.107 (4)
Te1—O2^vi	1.906 (5)	Co3—O3ⁱⁱⁱ	2.107 (4)
Te1—O2	1.906 (5)	Co3—O3^v	2.107 (4)
Te1—O2^vii	1.906 (5)	Co4—O2	2.067 (7)
Te1—O6^vi	1.991 (4)	Co4—O2^xviii	2.067 (7)
Te1—O6^vii	1.991 (4)	Co4—O1^vi	2.071 (4)
Te1—O6	1.991 (4)	Co4—O1^xiv	2.071 (4)
Te2—O5	1.917 (6)	Co4—O5^xix	2.116 (7)
Te2—O5ⁱⁱⁱ	1.917 (6)	Co4—O5^iv	2.116 (7)

O6ⁱ—Pb1—O6	84.58 (16)	O5ⁱⁱⁱ—Te2—O1^xii	85.9 (2)
O6ⁱ—Pb1—O1ⁱ	79.26 (18)	O3ⁱⁱⁱ—Te2—O1^xii	87.0 (2)
O6—Pb1—O1ⁱ	77.79 (18)	O3—Te2—O1^xii	93.7 (2)
O6ⁱ—Pb1—O1	77.79 (18)	O5—Te2—O1ⁱ	85.9 (2)
O6—Pb1—O1	79.26 (18)	O5ⁱⁱⁱ—Te2—O1ⁱ	93.3 (2)
O1ⁱ—Pb1—O1	148.79 (19)	O3ⁱⁱⁱ—Te2—O1ⁱ	93.7 (2)
O6ⁱ—Pb1—O3ⁱⁱ	95.87 (13)	O3—Te2—O1ⁱ	87.0 (2)
O6—Pb1—O3ⁱⁱ	133.98 (17)	O1^xii—Te2—O1ⁱ	179.0 (3)
O1ⁱ—Pb1—O3ⁱⁱ	147.68 (15)	O5^x—Co1—O5ⁱⁱⁱ	108.14 (14)
O1—Pb1—O3ⁱⁱ	56.26 (15)	O5^x—Co1—O5^xiii	108.14 (14)
O6ⁱ—Pb1—O3ⁱⁱⁱ	133.98 (17)	O5ⁱⁱⁱ—Co1—O5^xiii	108.14 (14)
O6—Pb1—O3ⁱⁱⁱ	95.87 (13)	O5^x—Co1—O6^vi	87.99 (18)
O1ⁱ—Pb1—O3ⁱⁱⁱ	56.26 (15)	O5ⁱⁱⁱ—Co1—O6^vi	85.39 (19)
O1—Pb1—O3ⁱⁱⁱ	147.68 (15)	O5^xiii—Co1—O6^vi	153.55 (18)
O3ⁱⁱ—Pb1—O3ⁱⁱⁱ	114.8 (2)	O5^x—Co1—O6^vii	85.39 (19)
O6ⁱ—Pb1—O3^iv	138.20 (17)	O5ⁱⁱⁱ—Co1—O6^vii	153.55 (18)
O6—Pb1—O3^iv	95.05 (13)	O5^xiii—Co1—O6^vii	87.99 (18)
O1ⁱ—Pb1—O3^iv	141.63 (15)	O6^vi—Co1—O6^vii	72.17 (17)
O1—Pb1—O3^iv	61.26 (14)	O5^x—Co1—O6	153.55 (18)
O3ⁱⁱ—Pb1—O3^iv	55.44 (13)	O5ⁱⁱⁱ—Co1—O6	87.99 (18)
O3ⁱⁱⁱ—Pb1—O3^iv	87.73 (10)	O5^xiii—Co1—O6	85.39 (18)
O6ⁱ—Pb1—O3^v	95.05 (13)	O6^vi—Co1—O6	72.17 (17)
O6—Pb1—O3^v	138.20 (17)	O6^vii—Co1—O6	72.17 (17)
O1ⁱ—Pb1—O3^v	61.26 (14)	O2^xiv—Co2—O2	87.8 (3)
O1—Pb1—O3^v	141.63 (15)	O2^xiv—Co2—O3ⁱ	92.52 (17)
O3ⁱⁱ—Pb1—O3^v	87.73 (10)	O2—Co2—O3ⁱ	174.4 (3)
O3ⁱⁱⁱ—Pb1—O3^v	55.44 (13)	O2^xiv—Co2—O3^iv	174.4 (3)
O3^iv—Pb1—O3^v	111.4 (2)	O2—Co2—O3^iv	92.52 (17)
O6^viii—Pb2—O6^vii	83.17 (17)	O3ⁱ—Co2—O3^iv	87.7 (2)
O6^viii—Pb2—O2^ix	61.34 (16)	O2^xiv—Co2—O1	89.3 (2)
O6^vii—Pb2—O2^ix	107.91 (19)	O2—Co2—O1	95.5 (2)
O6^viii—Pb2—O2^vi	107.91 (19)	O3ⁱ—Co2—O1	78.9 (2)
O6^vii—Pb2—O2^vi	61.34 (16)	O3^iv—Co2—O1	96.2 (2)
O2^ix—Pb2—O2^vi	166.8 (3)	O2^xiv—Co2—O1^xiv	95.5 (2)
O6^viii—Pb2—O5^x	106.77 (19)	O2—Co2—O1^xiv	89.3 (2)
O6^vii—Pb2—O5^x	68.25 (16)	O3ⁱ—Co2—O1^xiv	96.2 (2)
O2^ix—Pb2—O5^x	66.27 (12)	O3^iv—Co2—O1^xiv	78.9 (2)
O2^vi—Pb2—O5^x	112.94 (13)	O1—Co2—O1^xiv	173.3 (3)
O6^viii—Pb2—O5^xi	68.25 (16)	O3^xv—Co3—O3	175.2 (5)
O6^vii—Pb2—O5^xi	106.77 (19)	O3^xv—Co3—O3^xvi	79.5 (4)
O2^ix—Pb2—O5^xi	112.94 (13)	O3—Co3—O3^xvi	96.96 (14)
O2^vi—Pb2—O5^xi	66.27 (12)	O3^xv—Co3—O3^xvii	86.8 (4)
O5^x—Pb2—O5^xi	173.7 (3)	O3—Co3—O3^xvii	96.96 (14)
O6^viii—Pb2—O6^vi	138.39 (2)	O3^xvi—Co3—O3^xvii	96.96 (14)
O6^vii—Pb2—O6^vi	55.23 (15)	O3^xv—Co3—O3ⁱⁱⁱ	96.96 (14)
O2^ix—Pb2—O6^vi	126.25 (15)	O3—Co3—O3ⁱⁱⁱ	79.5 (4)
O2^vi—Pb2—O6^vi	55.67 (17)	O3^xvi—Co3—O3ⁱⁱⁱ	86.8 (4)
O5^x—Pb2—O6^vi	60.10 (16)	O3^xvii—Co3—O3ⁱⁱⁱ	175.2 (5)
O5^xi—Pb2—O6^vi	120.76 (15)	O3^xv—Co3—O3^v	96.96 (14)
O6^viii—Pb2—O6^ix	55.23 (15)	O3—Co3—O3^v	86.8 (4)
O6^vii—Pb2—O6^ix	138.39 (2)	O3^xvi—Co3—O3^v	175.2 (5)
O2^ix—Pb2—O6^ix	55.67 (17)	O3^xvii—Co3—O3^v	79.5 (4)
O2^vi—Pb2—O6^ix	126.25 (15)	O3ⁱⁱⁱ—Co3—O3^v	96.96 (14)
O5^x—Pb2—O6^ix	120.76 (15)	O2—Co4—O2^xviii	89.8 (3)
O5^xi—Pb2—O6^ix	60.10 (16)	O2—Co4—O1^vi	96.9 (2)
O6^vi—Pb2—O6^ix	166.38 (13)	O2^xviii—Co4—O1^vi	91.0 (2)
O6^viii—Pb2—O3^xi	120.59 (18)	O2—Co4—O1^xiv	91.0 (2)
O6^vii—Pb2—O3^xi	121.18 (18)	O2^xviii—Co4—O1^xiv	96.9 (2)
O2^ix—Pb2—O3^xi	130.9 (2)	O1^vi—Co4—O1^xiv	168.8 (4)
O2^vi—Pb2—O3^xi	60.21 (13)	O2—Co4—O5^xix	174.7 (3)
O5^x—Pb2—O3^xi	132.1 (2)	O2^xviii—Co4—O5^xix	90.92 (16)
O5^xi—Pb2—O3^xi	53.44 (14)	O1^vi—Co4—O5^xix	77.8 (2)
O6^vi—Pb2—O3^xi	86.29 (19)	O1^xiv—Co4—O5^xix	94.2 (2)
O6^ix—Pb2—O3^xi	84.37 (18)	O2—Co4—O5^iv	90.92 (16)
O6^viii—Pb2—O3^x	121.18 (18)	O2^xviii—Co4—O5^iv	174.7 (3)
O6^vii—Pb2—O3^x	120.59 (18)	O1^vi—Co4—O5^iv	94.2 (2)
O2^ix—Pb2—O3^x	60.21 (13)	O1^xiv—Co4—O5^iv	77.8 (2)
O2^vi—Pb2—O3^x	130.9 (2)	O5^xix—Co4—O5^iv	88.9 (3)
O5^x—Pb2—O3^x	53.44 (14)	Te2ⁱⁱ—O1—Co4^vii	98.54 (19)
O5^xi—Pb2—O3^x	132.1 (2)	Te2ⁱⁱ—O1—Co2	96.67 (17)
O6^vi—Pb2—O3^x	84.37 (18)	Co4^vii—O1—Co2	89.3 (2)
O6^ix—Pb2—O3^x	86.29 (19)	Te2ⁱⁱ—O1—Pb1	116.6 (2)
O3^xi—Pb2—O3^x	93.32 (14)	Co4^vii—O1—Pb1	136.07 (18)
O2^vi—Te1—O2	99.15 (18)	Co2—O1—Pb1	110.4 (2)
O2^vi—Te1—O2^vii	99.15 (18)	Te1—O2—Co4	129.1 (3)
O2—Te1—O2^vii	99.15 (18)	Te1—O2—Co2	130.4 (4)
O2^vi—Te1—O6^vi	90.7 (2)	Co4—O2—Co2	89.87 (19)
O2—Te1—O6^vi	85.2 (2)	Te1—O2—Pb2^vii	95.48 (17)
O2^vii—Te1—O6^vi	168.4 (2)	Co4—O2—Pb2^vii	96.4 (2)
O2^vi—Te1—O6^vii	85.2 (2)	Co2—O2—Pb2^vii	111.0 (2)
O2—Te1—O6^vii	168.4 (2)	Te2—O3—Co2^xx	97.34 (17)
O2^vii—Te1—O6^vii	90.7 (2)	Te2—O3—Co3	96.2 (2)
O6^vi—Te1—O6^vii	84.0 (2)	Co2^xx—O3—Co3	92.8 (3)
O2^vi—Te1—O6	168.4 (2)	Te2—O5—Co1^xiii	125.5 (4)
O2—Te1—O6	90.7 (2)	Te2—O5—Co4^xx	97.7 (2)
O2^vii—Te1—O6	85.2 (2)	Co1^xiii—O5—Co4^xx	120.3 (3)
O6^vi—Te1—O6	84.0 (2)	Te2—O5—Pb2^xxi	117.3 (2)
O6^vii—Te1—O6	84.0 (2)	Co1^xiii—O5—Pb2^xxi	97.82 (18)
O5—Te2—O5ⁱⁱⁱ	92.5 (3)	Co4^xx—O5—Pb2^xxi	95.2 (2)
O5—Te2—O3ⁱⁱⁱ	177.8 (2)	Te1—O6—Co1	86.54 (14)
O5ⁱⁱⁱ—Te2—O3ⁱⁱⁱ	89.6 (2)	Te1—O6—Pb1	136.5 (2)
O5—Te2—O3	89.6 (2)	Co1—O6—Pb1	127.8 (2)
O5ⁱⁱⁱ—Te2—O3	177.8 (2)	Te1—O6—Pb2^vi	103.41 (16)
O3ⁱⁱⁱ—Te2—O3	88.2 (2)	Co1—O6—Pb2^vi	100.34 (16)
O5—Te2—O1^xii	93.3 (2)	Pb1—O6—Pb2^vi	96.12 (13)

Table 1

Selected bond lengths (Å)

Te1—O2	1.906 (5)
Te1—O6	1.991 (4)
Te2—O5	1.917 (6)
Te2—O3	1.937 (7)
Te2—O1ⁱ	1.939 (5)
Co1—O5ⁱⁱ	2.004 (6)
Co1—O6	2.262 (5)
Co2—O2	2.090 (6)
Co2—O3ⁱⁱⁱ	2.090 (8)
Co2—O1	2.108 (6)
Co3—O3	2.107 (4)
Co4—O2	2.067 (7)
Co4—O1^iv	2.071 (4)
Co4—O5^v	2.116 (7)

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

1 in total

1. A short history of SHELX.

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

1 in total

1. Large spontaneous exchange bias in a weak ferromagnet Pb₆Ni₉(TeO₆)₅.

Authors: B Koteswararao; Tanmoy Chakrabarty; Tathamay Basu; Binoy Krishna Hazra; P V Srinivasarao; P L Paulose; S Srinath
Journal: Sci Rep Date: 2017-08-15 Impact factor: 4.379

1 in total

Pb(6)Co(9)(TeO(6))(5).

Related literature

Experimental

Crystal data

Data collection

Refinement

1. A short history of SHELX.

1. Large spontaneous exchange bias in a weak ferromagnet Pb6Ni9(TeO6)5.

1. Large spontaneous exchange bias in a weak ferromagnet Pb₆Ni₉(TeO₆)₅.