A triclinic polymorph of catena-poly[[diaqua­cobalt(II)]-μ-{μ-mellitato-κ²O¹:O⁴-bis­[penta­aqua­cobalt(II)]}-κ⁴O²,O³:O⁵,O⁶] hexa­hydrate]

A second, triclinic, polymorph of the title compound, {[Co₃(C₁₂O₁₂)(H₂O)₁₂]·6H₂O}_n, is reported. This polymorph forms a three-dimensional framework through O—H...O hydrogen-bond inter­actions between the one-dimensional [Co₃{C₆(COO)₆}₃(H₂O)₁₂]_n chains and the solvent water mol­ecules. The mellitate ligand lies on an inversion center.

Key indicators

• Single-crystal X-ray study
• T = 291 K
• Mean [sigma](C-C) = 0.003 Å
• R factor = 0.027
• wR factor = 0.080
• Data-to-parameter ratio = 16.7

checkCIF/PLATON results

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Computing details

Data collection: SMART (Bruker, 1998); cell refinement: SMART; data reduction: SAINT (Bruker, 1998); program(s) used to solve structure: SHELXS97 (Sheldrick, 1997); program(s) used to refine structure: SHELXL97 (Sheldrick, 1997); molecular graphics: SHELXTL (Bruker, 1998); software used to prepare material for publication: SHELXTL.

catena-poly[[diaquacobalt(II)]-µ- {µ-mellitato-κ²O¹:O⁴-bis[pentaaquacobalt(II)]}- κ⁴O²,O³:O⁵,O⁶] hexahydrate]

Crystal data

[Co3(C12O12)(H2O)12]·6H2O	Z = 1
Mr = 837.20	F(000) = 429
Triclinic, P1	Dx = 1.840 Mg m^−3
Hall symbol: -P 1	Mo Kα radiation, λ = 0.71073 Å
a = 8.4910 (17) Å	Cell parameters from 989 reflections
b = 9.6550 (19) Å	θ = 3.3–26.7°
c = 10.812 (2) Å	µ = 1.74 mm^−1
α = 70.66 (3)°	T = 291 K
β = 67.36 (3)°	Needle, red
γ = 72.18 (3)°	0.2 × 0.2 × 0.18 mm
V = 755.5 (3) Å^3

Data collection

Bruker SMART CCD area-detector diffractometer	3435 independent reflections
Radiation source: fine-focus sealed tube	3034 reflections with I > 2σ(I)
Graphite monochromator	Rint = 0.017
φ and ω scans	θmax = 27.5°, θmin = 2.1°
Absorption correction: multi-scan (SADABS; Sheldrick, 1996)	h = −10→1
Tmin = 0.698, Tmax = 0.723	k = −12→11
4119 measured reflections	l = −14→13

Refinement

Refinement on F^2	Secondary atom site location: difference Fourier map
Least-squares matrix: full	Hydrogen site location: inferred from neighbouring sites
R[F^2 > 2σ(F^2)] = 0.027	H-atom parameters constrained
wR(F^2) = 0.080	w = 1/[σ^2(Fo^2) + (0.049P)^2 + 0.4002P] where P = (Fo^2 + 2Fc^2)/3
S = 0.98	(Δ/σ)max = 0.002
3435 reflections	Δρmax = 0.43 e Å^−3
206 parameters	Δρmin = −0.41 e Å^−3
0 restraints	Extinction correction: SHELXL97, Fc^*=kFc[1+0.001xFc^2λ^3/sin(2θ)]^-1/4
Primary atom site location: structure-invariant direct methods	Extinction coefficient: 0.0067 (16)

Special details

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.

Fractional atomic coordinates and isotropic or equivalent isotropic displacement parameters (Ų)

	x	y	z	Uiso*/Ueq
Co1	0.5000	0.0000	1.0000	0.01794 (11)
Co2	0.34720 (3)	0.24878 (3)	0.42170 (2)	0.01937 (10)
O1	0.28345 (17)	0.04854 (17)	1.16329 (14)	0.0250 (3)
O2	0.0187 (2)	0.1831 (2)	1.23759 (18)	0.0393 (4)
O3	0.38586 (17)	0.17210 (16)	0.86311 (15)	0.0262 (3)
O4	0.16647 (18)	0.33925 (15)	0.80109 (14)	0.0244 (3)
O5	0.25542 (16)	0.11501 (15)	0.63073 (12)	0.0201 (3)
O6	−0.0281 (2)	0.1780 (2)	0.65570 (16)	0.0432 (5)
C1	0.1262 (2)	0.0976 (2)	1.16628 (17)	0.0180 (3)
C2	0.0635 (2)	0.04587 (18)	1.07862 (16)	0.0140 (3)
C3	0.1144 (2)	0.09931 (18)	0.93500 (16)	0.0147 (3)
C4	0.0508 (2)	0.05364 (19)	0.85640 (16)	0.0149 (3)
C5	0.2310 (2)	0.21247 (19)	0.86072 (17)	0.0167 (3)
C6	0.0959 (2)	0.1200 (2)	0.70176 (17)	0.0179 (3)
O7	0.41451 (19)	−0.17185 (17)	0.97466 (15)	0.0298 (3)
O8	0.4220 (2)	0.05917 (17)	0.34532 (15)	0.0297 (3)
O9	0.60327 (19)	0.20535 (18)	0.42938 (16)	0.0317 (3)
O10	0.10663 (19)	0.30449 (18)	0.39011 (14)	0.0289 (3)
O11	0.2893 (3)	0.42570 (17)	0.50883 (16)	0.0395 (4)
O12	0.44107 (19)	0.37460 (17)	0.21820 (15)	0.0308 (3)
O13	0.2298 (2)	0.57568 (18)	−0.14138 (18)	0.0378 (4)
O14	−0.2133 (2)	0.39773 (19)	−0.11067 (17)	0.0373 (4)
O15	0.6435 (2)	0.29519 (18)	−0.36427 (16)	0.0336 (3)
H7A	0.4932	−0.2170	0.9156	0.050*
H7B	0.3435	−0.2272	1.0317	0.050*
H8A	0.3782	0.0538	0.2888	0.050*
H8B	0.5275	0.0122	0.3300	0.050*
H9B	0.6127	0.2309	0.4937	0.050*
H10A	0.0423	0.2678	0.4700	0.050*
H10B	0.0800	0.2705	0.3392	0.050*
H11A	0.2392	0.4191	0.5947	0.050*
H11B	0.3255	0.5066	0.4633	0.050*
H12A	0.5353	0.3991	0.2050	0.050*
H12B	0.3651	0.4459	0.1902	0.050*
H13A	0.1612	0.6448	−0.1796	0.050*
H13B	0.2190	0.5006	−0.1597	0.050*
H14A	−0.1063	0.3914	−0.1587	0.050*
H14B	−0.2092	0.4046	−0.0356	0.050*
H15A	0.5649	0.2689	−0.2887	0.050*
H15B	0.7330	0.2401	−0.3426	0.050*
H9A	0.6569	0.1155	0.4518	0.050*

Atomic displacement parameters (Ų)

	U^11	U^22	U^33	U^12	U^13	U^23
Co1	0.01520 (17)	0.02189 (18)	0.01802 (17)	−0.00539 (13)	−0.00535 (12)	−0.00487 (12)
Co2	0.02092 (14)	0.02111 (15)	0.01632 (14)	−0.00561 (10)	−0.00624 (10)	−0.00323 (9)
O1	0.0165 (6)	0.0417 (8)	0.0231 (6)	−0.0069 (6)	−0.0062 (5)	−0.0151 (6)
O2	0.0321 (8)	0.0530 (10)	0.0477 (9)	0.0096 (7)	−0.0220 (7)	−0.0365 (8)
O3	0.0188 (6)	0.0296 (7)	0.0292 (7)	−0.0119 (5)	−0.0097 (5)	0.0032 (5)
O4	0.0271 (7)	0.0192 (6)	0.0265 (7)	−0.0080 (5)	−0.0099 (5)	−0.0003 (5)
O5	0.0166 (6)	0.0264 (6)	0.0141 (6)	−0.0054 (5)	−0.0030 (4)	−0.0020 (5)
O6	0.0202 (7)	0.0772 (13)	0.0215 (7)	−0.0129 (8)	−0.0098 (6)	0.0078 (7)
C1	0.0195 (8)	0.0229 (8)	0.0149 (7)	−0.0075 (7)	−0.0066 (6)	−0.0044 (6)
C2	0.0118 (7)	0.0176 (7)	0.0139 (7)	−0.0029 (6)	−0.0049 (6)	−0.0045 (6)
C3	0.0118 (7)	0.0175 (7)	0.0143 (7)	−0.0044 (6)	−0.0039 (6)	−0.0020 (6)
C4	0.0130 (7)	0.0184 (8)	0.0124 (7)	−0.0035 (6)	−0.0038 (6)	−0.0026 (6)
C5	0.0185 (8)	0.0194 (8)	0.0141 (7)	−0.0079 (6)	−0.0049 (6)	−0.0033 (6)
C6	0.0183 (8)	0.0220 (8)	0.0145 (7)	−0.0069 (6)	−0.0059 (6)	−0.0023 (6)
O7	0.0259 (7)	0.0329 (8)	0.0333 (8)	−0.0131 (6)	−0.0008 (6)	−0.0151 (6)
O8	0.0356 (8)	0.0285 (7)	0.0318 (7)	0.0022 (6)	−0.0187 (6)	−0.0143 (6)
O9	0.0271 (7)	0.0356 (8)	0.0325 (8)	−0.0064 (6)	−0.0128 (6)	−0.0043 (6)
O10	0.0269 (7)	0.0405 (8)	0.0226 (7)	−0.0092 (6)	−0.0098 (5)	−0.0074 (6)
O11	0.0670 (12)	0.0259 (7)	0.0235 (7)	−0.0187 (8)	−0.0045 (7)	−0.0063 (6)
O12	0.0282 (7)	0.0319 (8)	0.0265 (7)	−0.0084 (6)	−0.0088 (6)	0.0022 (6)
O13	0.0400 (9)	0.0300 (8)	0.0499 (10)	−0.0105 (7)	−0.0211 (8)	−0.0065 (7)
O14	0.0274 (8)	0.0396 (9)	0.0364 (8)	−0.0042 (7)	−0.0071 (6)	−0.0049 (7)
O15	0.0268 (7)	0.0353 (8)	0.0338 (8)	−0.0127 (6)	−0.0108 (6)	0.0050 (6)

Geometric parameters (Å, º)

Co1—O1^i	2.0588 (15)	C3—C5	1.513 (2)
Co1—O1	2.0588 (16)	C4—C2^ii	1.399 (2)
Co1—O3	2.0930 (16)	C4—C6	1.517 (2)
Co1—O3^i	2.0931 (16)	O7—H7A	0.8499
Co1—O7^i	2.1322 (15)	O7—H7B	0.8494
Co1—O7	2.1322 (15)	O8—H8A	0.8495
Co2—O11	2.0596 (16)	O8—H8B	0.8497
Co2—O10	2.0788 (15)	O9—H9B	0.8489
Co2—O8	2.0790 (15)	O9—H9A	0.8496
Co2—O12	2.1034 (17)	O10—H10A	0.8499
Co2—O9	2.1138 (16)	O10—H10B	0.8495
Co2—O5	2.1702 (15)	O11—H11A	0.8491
O1—C1	1.264 (2)	O11—H11B	0.8499
O2—C1	1.236 (2)	O12—H12A	0.8495
O3—C5	1.260 (2)	O12—H12B	0.8497
O4—C5	1.246 (2)	O13—H13A	0.8492
O5—C6	1.269 (2)	O13—H13B	0.8499
O6—C6	1.237 (2)	O14—H14A	0.8501
C1—C2	1.515 (2)	O14—H14B	0.8500
C2—C3	1.398 (2)	O15—H15A	0.8509
C2—C4^ii	1.399 (2)	O15—H15B	0.8502
C3—C4	1.398 (2)
O1^i—Co1—O1	180.0	C3—C2—C4^ii	119.91 (15)
O1^i—Co1—O3	90.06 (6)	C3—C2—C1	120.95 (15)
O1—Co1—O3	89.94 (6)	C4^ii—C2—C1	119.12 (14)
O1^i—Co1—O3^i	89.94 (6)	C2—C3—C4	120.04 (15)
O1—Co1—O3^i	90.06 (6)	C2—C3—C5	121.83 (15)
O3—Co1—O3^i	180.0	C4—C3—C5	118.07 (14)
O1^i—Co1—O7^i	95.35 (6)	C3—C4—C2^ii	120.05 (15)
O1—Co1—O7^i	84.65 (6)	C3—C4—C6	120.00 (15)
O3—Co1—O7^i	85.54 (6)	C2^ii—C4—C6	119.82 (15)
O3^i—Co1—O7^i	94.46 (6)	O4—C5—O3	124.74 (17)
O1^i—Co1—O7	84.65 (6)	O4—C5—C3	117.30 (15)
O1—Co1—O7	95.35 (6)	O3—C5—C3	117.96 (15)
O3—Co1—O7	94.46 (6)	O6—C6—O5	125.27 (16)
O3^i—Co1—O7	85.54 (6)	O6—C6—C4	116.47 (16)
O7^i—Co1—O7	180.0	O5—C6—C4	118.24 (15)
O11—Co2—O10	93.33 (8)	Co1—O7—H7A	111.7
O11—Co2—O8	174.37 (7)	Co1—O7—H7B	130.7
O10—Co2—O8	91.67 (7)	H7A—O7—H7B	111.2
O11—Co2—O12	94.18 (7)	Co2—O8—H8A	121.2
O10—Co2—O12	86.79 (7)	Co2—O8—H8B	118.6
O8—Co2—O12	88.70 (7)	H8A—O8—H8B	111.4
O11—Co2—O9	87.61 (8)	Co2—O9—H9B	115.7
O10—Co2—O9	173.30 (6)	Co2—O9—H9A	120.0
O8—Co2—O9	87.73 (7)	H9B—O9—H9A	93.7
O12—Co2—O9	86.52 (7)	Co2—O10—H10A	101.4
O11—Co2—O5	86.69 (6)	Co2—O10—H10B	126.2
O10—Co2—O5	94.09 (6)	H10A—O10—H10B	101.6
O8—Co2—O5	90.36 (6)	Co2—O11—H11A	122.5
O12—Co2—O5	178.73 (5)	Co2—O11—H11B	122.1
O9—Co2—O5	92.59 (6)	H11A—O11—H11B	114.9
C1—O1—Co1	128.71 (12)	Co2—O12—H12A	111.1
C5—O3—Co1	130.99 (12)	Co2—O12—H12B	114.7
C6—O5—Co2	124.30 (12)	H12A—O12—H12B	114.8
O2—C1—O1	124.62 (17)	H13A—O13—H13B	99.8
O2—C1—C2	117.44 (16)	H14A—O14—H14B	100.1
O1—C1—C2	117.92 (15)	H15A—O15—H15B	99.2

Symmetry codes: (i) −x+1, −y, −z+2; (ii) −x, −y, −z+2.

Hydrogen-bond geometry (Å, º)

D—H···A	D—H	H···A	D···A	D—H···A
O7—H7A···O12^iii	0.85	2.24	2.992 (2)	147
O7—H7B···O14^iv	0.85	2.03	2.839 (2)	159
O8—H8A···O1^v	0.85	1.85	2.694 (2)	178
O8—H8B···O5^iii	0.85	1.99	2.799 (2)	159
O9—H9A···O5^iii	0.85	2.47	3.144 (2)	137
O9—H9B···O15^vi	0.85	1.96	2.810 (2)	177
O10—H10A···O6	0.85	1.84	2.655 (2)	160
O10—H10B···O2^v	0.85	1.88	2.723 (2)	176
O11—H11A···O4	0.85	2.01	2.832 (2)	162
O11—H11B···O15^vii	0.85	1.90	2.738 (2)	168
O12—H12A···O13^vii	0.85	1.91	2.738 (2)	165
O12—H12B···O14^viii	0.85	1.87	2.713 (2)	174
O13—H13A···O2^ix	0.85	2.00	2.835 (2)	170
O13—H13B···O4^v	0.85	1.95	2.799 (2)	174
O14—H14A···O4^v	0.85	2.11	2.916 (2)	157
O14—H14B···O13^viii	0.85	1.92	2.768 (2)	173
O15—H15A···O3^v	0.85	1.95	2.785 (2)	166
O15—H15B···O6^x	0.85	1.93	2.734 (2)	158

Symmetry codes: (iii) −x+1, −y, −z+1; (iv) −x, −y, −z+1; (v) x, y, z−1; (vi) x, y, z+1; (vii) −x+1, −y+1, −z; (viii) −x, −y+1, −z; (ix) −x, −y+1, −z+1; (x) x+1, y, z−1.