Literature DB >> 21579654

catena-Poly[diquinolinium [[diaqua-cobaltate(II)]-μ-cyclo-tetra-phosphato] hexa-hydrate].

Hanène Hemissi, Mohammed Rzaigui, Zeid Abdullah Al Othman.

Abstract

The cyclo-tetra-phosphate anion, [P(4)O(12)](4-), forms the title complex with cobalt(II) and quinolinium, {(C(9)H(8)N)(2)[Co(P(4)O(12))(H(2)O)(2)]·6H(2)O}(n). In the complex anion, the Co(II) ion, lying on an inversion center, is surrounded by four phosphate O atoms and two water mol-ecules in a slightly distorted octa-hedral geometry. The crystal structure consists of anionic ribbons of formula {[Co(P(4)O(12))(H(2)O)(2)](2-)}(n) extending along [100]. A network of O-H⋯O, N-H⋯O and C-H⋯O hydrogen bonds consolidates the crystal packing.

Entities: CellLine Chemical Disease Gene Species

Year: 2010 PMID： 21579654 PMCID： PMC2979730 DOI： 10.1107/S1600536810002096

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

Related literature

For the crystal chemistry of condensed phosphates, see: Durif (1995 ▶). For general background to transition metal–organic derivatives of polyoxoanions, see: Feher & Budzichowski (1995 ▶); Guerrero et al. (1999 ▶); Ikotun et al. (2008 ▶); Lugmair & Tilley (1998 ▶). For general background to hydrogen bonds, see: Blessing (1986 ▶); Brown (1976 ▶); Steiner & Saenger (1993 ▶). For the synthesis, see: Ondik (1964 ▶).

Experimental

Crystal data

(C9H8N)2[Co(P4O12)(H2O)2]·6H2O M = 779.27 Triclinic, a = 7.443 (3) Å b = 10.037 (4) Å c = 10.682 (7) Å α = 83.74 (4)° β = 70.98 (4)° γ = 85.71 (3)° V = 749.4 (6) Å3 Z = 1 Ag Kα radiation λ = 0.56083 Å μ = 0.46 mm−1 T = 293 K 0.20 × 0.18 × 0.16 mm

Data collection

Enraf–Nonius TurboCAD-4 diffractometer 12878 measured reflections 7242 independent reflections 4531 reflections with I > 2σ(I) R int = 0.039 2 standard reflections every 120 min intensity decay: 2%

Refinement

R[F 2 > 2σ(F 2)] = 0.057 wR(F 2) = 0.164 S = 0.98 7242 reflections 237 parameters 13 restraints H atoms treated by a mixture of independent and constrained refinement Δρmax = 1.11 e Å−3 Δρmin = −1.46 e Å−3 Data collection: CAD-4 EXPRESS (Enraf–Nonius, 1989 ▶); cell refinement: CAD-4 EXPRESS; data reduction: XCAD4 (Harms & Wocadlo, 1995 ▶); program(s) used to solve structure: SHELXS97 (Sheldrick, 2008 ▶); program(s) used to refine structure: SHELXL97 (Sheldrick, 2008 ▶); molecular graphics: ORTEP-3 (Farrugia, 1997 ▶); software used to prepare material for publication: WinGX (Farrugia, 1999 ▶). Crystal structure: contains datablocks I, global. DOI: 10.1107/S1600536810002096/hy2272sup1.cif Structure factors: contains datablocks I. DOI: 10.1107/S1600536810002096/hy2272Isup2.hkl Additional supplementary materials: crystallographic information; 3D view; checkCIF report

(C₉H₈N)₂[Co(P₄O₁₂)(H₂O)₂]·6H₂O	Z = 1
M_r = 779.27	F(000) = 401
Triclinic, P1	D_x = 1.727 Mg m⁻³
Hall symbol: -P 1	Ag Kα radiation, λ = 0.56083 Å
a = 7.443 (3) Å	Cell parameters from 25 reflections
b = 10.037 (4) Å	θ = 9.0–11.0°
c = 10.682 (7) Å	µ = 0.46 mm⁻¹
α = 83.74 (4)°	T = 293 K
β = 70.98 (4)°	Prism, pink
γ = 85.71 (3)°	0.20 × 0.18 × 0.16 mm
V = 749.4 (6) Å³

Enraf–Nonius TurboCAD-4 diffractometer	R_int = 0.039
Radiation source: fine-focus sealed tube	θ_max = 28.0°, θ_min = 2.2°
graphite	h = −12→12
non–profiled ω/2θ scans	k = −16→16
12878 measured reflections	l = −17→10
7242 independent reflections	2 standard reflections every 120 min
4531 reflections with I > 2σ(I)	intensity decay: 2%

Refinement on F²	Primary atom site location: structure-invariant direct methods
Least-squares matrix: full	Secondary atom site location: difference Fourier map
R[F² > 2σ(F²)] = 0.057	Hydrogen site location: inferred from neighbouring sites
wR(F²) = 0.164	H atoms treated by a mixture of independent and constrained refinement
S = 0.98	w = 1/[σ²(F_o²) + (0.097P)²] where P = (F_o² + 2F_c²)/3
7242 reflections	(Δ/σ)_max = 0.022
237 parameters	Δρ_max = 1.11 e Å⁻³
13 restraints	Δρ_min = −1.46 e Å⁻³

	x	y	z	U_iso*/U_eq
Co1	0.5000	0.5000	0.5000	0.02117 (10)
P2	0.84035 (7)	0.67186 (5)	0.52866 (5)	0.02037 (11)
P1	0.94639 (7)	0.49127 (5)	0.31420 (5)	0.02082 (11)
O5	0.7442 (2)	0.47075 (18)	0.33361 (17)	0.0290 (3)
O9	0.8351 (3)	0.81917 (16)	0.5033 (2)	0.0353 (4)
O8	0.9759 (3)	0.63833 (17)	0.6180 (2)	0.0329 (4)
O7	0.9688 (2)	0.61035 (16)	0.39418 (17)	0.0284 (3)
O1	0.4503 (3)	0.68127 (18)	0.39353 (19)	0.0348 (4)
O6	1.0732 (3)	0.5182 (2)	0.17668 (18)	0.0410 (4)
C1	1.2832 (4)	0.9562 (2)	−0.0159 (3)	0.0314 (4)
N1	1.3663 (3)	0.8353 (2)	−0.0577 (2)	0.0350 (4)
H1	1.3836	0.7736	0.0002	0.042*
C2	1.2288 (5)	0.9765 (3)	0.1194 (3)	0.0432 (6)
H2	1.2488	0.9092	0.1811	0.052*
C6	1.2539 (4)	1.0555 (3)	−0.1110 (3)	0.0370 (5)
C7	1.3093 (5)	1.0269 (3)	−0.2441 (3)	0.0447 (6)
H7	1.2879	1.0908	−0.3082	0.054*
C3	1.1460 (6)	1.0973 (4)	0.1583 (4)	0.0549 (8)
H3	1.1094	1.1128	0.2476	0.066*
C8	1.3942 (5)	0.9057 (4)	−0.2799 (3)	0.0495 (7)
H8	1.4340	0.8876	−0.3686	0.059*
C9	1.4211 (4)	0.8100 (3)	−0.1843 (3)	0.0437 (6)
H9	1.4780	0.7269	−0.2086	0.052*
C5	1.1660 (5)	1.1797 (3)	−0.0655 (4)	0.0512 (8)
H5	1.1433	1.2478	−0.1255	0.061*
C4	1.1153 (6)	1.1986 (3)	0.0652 (4)	0.0607 (10)
H4	1.0590	1.2805	0.0940	0.073*
O10	0.6636 (2)	0.59823 (17)	0.58700 (16)	0.0282 (3)
O2	1.3962 (3)	0.65569 (19)	0.14615 (19)	0.0358 (4)
O3	1.3081 (3)	0.5195 (2)	−0.0816 (2)	0.0412 (4)
O4	0.2153 (3)	0.9054 (2)	0.4559 (3)	0.0549 (6)
H11	0.369 (4)	0.735 (3)	0.436 (3)	0.044 (10)*
H21	0.436 (5)	0.674 (4)	0.320 (2)	0.052 (11)*
H12	1.496 (3)	0.610 (3)	0.118 (4)	0.052 (11)*
H22	1.299 (3)	0.613 (3)	0.163 (4)	0.046 (10)*
H13	1.208 (4)	0.513 (4)	−0.013 (2)	0.052 (11)*
H23	1.264 (5)	0.505 (4)	−0.145 (2)	0.056 (11)*
H14	0.231 (5)	0.990 (2)	0.451 (4)	0.056 (11)*
H24	0.098 (3)	0.897 (3)	0.465 (4)	0.056 (11)*

	U¹¹	U²²	U³³	U¹²	U¹³	U²³
Co1	0.01923 (17)	0.02359 (18)	0.02047 (18)	0.00158 (13)	−0.00587 (13)	−0.00424 (13)
P2	0.0235 (2)	0.0164 (2)	0.0224 (2)	0.00486 (16)	−0.00927 (18)	−0.00462 (16)
P1	0.0217 (2)	0.0241 (2)	0.0155 (2)	0.00357 (17)	−0.00460 (16)	−0.00431 (17)
O5	0.0228 (7)	0.0389 (9)	0.0272 (8)	0.0059 (6)	−0.0095 (6)	−0.0111 (6)
O9	0.0451 (10)	0.0176 (7)	0.0457 (11)	0.0086 (6)	−0.0190 (8)	−0.0054 (7)
O8	0.0385 (9)	0.0262 (7)	0.0439 (10)	0.0039 (6)	−0.0270 (8)	−0.0061 (7)
O7	0.0277 (7)	0.0257 (7)	0.0277 (8)	−0.0016 (6)	−0.0009 (6)	−0.0091 (6)
O1	0.0473 (10)	0.0289 (8)	0.0294 (9)	0.0092 (7)	−0.0153 (8)	−0.0057 (7)
O6	0.0442 (10)	0.0516 (11)	0.0189 (7)	−0.0067 (9)	0.0032 (7)	−0.0060 (7)
C1	0.0319 (10)	0.0283 (10)	0.0328 (12)	0.0007 (8)	−0.0094 (9)	−0.0019 (8)
N1	0.0377 (11)	0.0283 (9)	0.0329 (11)	0.0020 (8)	−0.0050 (8)	0.0013 (8)
C2	0.0487 (15)	0.0478 (15)	0.0337 (13)	0.0005 (12)	−0.0135 (11)	−0.0072 (11)
C6	0.0421 (13)	0.0286 (11)	0.0394 (13)	−0.0012 (9)	−0.0137 (11)	0.0025 (9)
C7	0.0512 (16)	0.0462 (15)	0.0356 (14)	−0.0076 (12)	−0.0154 (12)	0.0092 (12)
C3	0.064 (2)	0.0542 (19)	0.0495 (18)	−0.0019 (16)	−0.0158 (16)	−0.0233 (15)
C8	0.0562 (18)	0.0559 (18)	0.0300 (13)	−0.0067 (14)	−0.0044 (12)	−0.0033 (12)
C9	0.0460 (15)	0.0368 (13)	0.0383 (14)	0.0024 (11)	0.0004 (11)	−0.0071 (11)
C5	0.0574 (19)	0.0280 (12)	0.069 (2)	0.0018 (12)	−0.0237 (16)	−0.0006 (13)
C4	0.062 (2)	0.0364 (15)	0.082 (3)	0.0054 (14)	−0.0164 (19)	−0.0267 (17)
O10	0.0251 (7)	0.0347 (8)	0.0249 (7)	−0.0022 (6)	−0.0056 (6)	−0.0095 (6)
O2	0.0398 (10)	0.0339 (9)	0.0312 (9)	0.0008 (7)	−0.0094 (8)	0.0001 (7)
O3	0.0451 (11)	0.0543 (12)	0.0253 (9)	0.0030 (9)	−0.0129 (8)	−0.0072 (8)
O4	0.0449 (12)	0.0263 (9)	0.091 (2)	0.0085 (8)	−0.0178 (12)	−0.0164 (11)

Co1—O10ⁱ	2.1064 (16)	N1—H1	0.8600
Co1—O10	2.1064 (16)	C2—C3	1.361 (5)
Co1—O1ⁱ	2.1127 (18)	C2—H2	0.9300
Co1—O1	2.1127 (18)	C6—C7	1.402 (4)
Co1—O5ⁱ	2.1159 (16)	C6—C5	1.421 (4)
Co1—O5	2.1159 (16)	C7—C8	1.362 (5)
P2—O9	1.4737 (17)	C7—H7	0.9300
P2—O10	1.4748 (17)	C3—C4	1.403 (6)
P2—O8	1.5963 (17)	C3—H3	0.9300
P2—O7	1.6029 (16)	C8—C9	1.377 (5)
P1—O6	1.4730 (18)	C8—H8	0.9300
P1—O5	1.4779 (17)	C9—H9	0.9300
P1—O8ⁱⁱ	1.5833 (18)	C5—C4	1.354 (6)
P1—O7	1.5913 (17)	C5—H5	0.9300
O8—P1ⁱⁱ	1.5833 (18)	C4—H4	0.9300
O1—H11	0.830 (17)	O2—H12	0.827 (17)
O1—H21	0.831 (17)	O2—H22	0.825 (17)
C1—N1	1.372 (3)	O3—H13	0.863 (17)
C1—C6	1.401 (4)	O3—H23	0.875 (17)
C1—C2	1.402 (4)	O4—H14	0.855 (18)
N1—C9	1.326 (4)	O4—H24	0.855 (17)

O10ⁱ—Co1—O10	180.00 (8)	N1—C1—C2	119.6 (2)
O10ⁱ—Co1—O1ⁱ	90.99 (7)	C6—C1—C2	122.1 (3)
O10—Co1—O1ⁱ	89.01 (7)	C9—N1—C1	122.4 (2)
O10ⁱ—Co1—O1	89.01 (7)	C9—N1—H1	118.8
O10—Co1—O1	90.99 (7)	C1—N1—H1	118.8
O1ⁱ—Co1—O1	180.0	C3—C2—C1	118.3 (3)
O10ⁱ—Co1—O5ⁱ	89.95 (6)	C3—C2—H2	120.8
O10—Co1—O5ⁱ	90.05 (6)	C1—C2—H2	120.8
O1ⁱ—Co1—O5ⁱ	86.22 (7)	C1—C6—C7	118.8 (3)
O1—Co1—O5ⁱ	93.78 (7)	C1—C6—C5	117.5 (3)
O10ⁱ—Co1—O5	90.05 (6)	C7—C6—C5	123.7 (3)
O10—Co1—O5	89.95 (6)	C8—C7—C6	120.1 (3)
O1ⁱ—Co1—O5	93.78 (7)	C8—C7—H7	119.9
O1—Co1—O5	86.22 (7)	C6—C7—H7	119.9
O5ⁱ—Co1—O5	180.0	C2—C3—C4	120.8 (3)
O9—P2—O10	121.11 (11)	C2—C3—H3	119.6
O9—P2—O8	105.29 (10)	C4—C3—H3	119.6
O10—P2—O8	110.13 (10)	C7—C8—C9	119.8 (3)
O9—P2—O7	108.09 (10)	C7—C8—H8	120.1
O10—P2—O7	109.91 (9)	C9—C8—H8	120.1
O8—P2—O7	100.23 (10)	N1—C9—C8	120.5 (3)
O6—P1—O5	117.41 (11)	N1—C9—H9	119.7
O6—P1—O8ⁱⁱ	109.43 (12)	C8—C9—H9	119.7
O5—P1—O8ⁱⁱ	106.81 (10)	C4—C5—C6	119.9 (3)
O6—P1—O7	106.60 (11)	C4—C5—H5	120.0
O5—P1—O7	111.38 (9)	C6—C5—H5	120.0
O8ⁱⁱ—P1—O7	104.47 (10)	C5—C4—C3	121.3 (3)
P1—O5—Co1	130.02 (10)	C5—C4—H4	119.3
P1ⁱⁱ—O8—P2	137.26 (12)	C3—C4—H4	119.3
P1—O7—P2	134.40 (11)	P2—O10—Co1	131.90 (10)
Co1—O1—H11	117 (2)	H12—O2—H22	113 (3)
Co1—O1—H21	116 (3)	H13—O3—H23	102 (2)
H11—O1—H21	110 (2)	H14—O4—H24	107 (3)
N1—C1—C6	118.3 (2)

D—H···A	D—H	H···A	D···A	D—H···A
N1—H1···O2	0.86	1.88	2.728 (3)	171
O1—H11···O4	0.83 (3)	1.98 (3)	2.747 (3)	154 (3)
O1—H21···O2ⁱⁱⁱ	0.84 (3)	2.00 (3)	2.841 (3)	179 (4)
O2—H12···O3^iv	0.83 (3)	1.85 (3)	2.666 (3)	168 (3)
O2—H22···O6	0.83 (3)	1.95 (3)	2.771 (3)	172 (4)
O3—H13···O6	0.86 (2)	1.95 (2)	2.743 (3)	152 (3)
O3—H23···O5^v	0.87 (3)	2.02 (2)	2.833 (3)	154 (3)
O4—H14···O9^vi	0.86 (2)	2.01 (2)	2.824 (3)	157 (4)
O4—H24···O9ⁱⁱⁱ	0.86 (3)	2.06 (3)	2.890 (3)	163 (3)
C7—H7···O9^vii	0.93	2.59	3.459 (4)	156
C9—H9···O3	0.93	2.54	3.080 (4)	118
C9—H9···O10^viii	0.93	2.59	3.381 (3)	143

Table 1

Hydrogen-bond geometry (Å, °)

D—H⋯A	D—H	H⋯A	D⋯A	D—H⋯A
N1—H1⋯O2	0.86	1.88	2.728 (3)	171
O1—H11⋯O4	0.83 (3)	1.98 (3)	2.747 (3)	154 (3)
O1—H21⋯O2ⁱ	0.84 (3)	2.00 (3)	2.841 (3)	179 (4)
O2—H12⋯O3ⁱⁱ	0.83 (3)	1.85 (3)	2.666 (3)	168 (3)
O2—H22⋯O6	0.83 (3)	1.95 (3)	2.771 (3)	172 (4)
O3—H13⋯O6	0.86 (2)	1.95 (2)	2.743 (3)	152 (3)
O3—H23⋯O5ⁱⁱⁱ	0.87 (3)	2.02 (2)	2.833 (3)	154 (3)
O4—H14⋯O9^iv	0.86 (2)	2.01 (2)	2.824 (3)	157 (4)
O4—H24⋯O9ⁱ	0.86 (3)	2.06 (3)	2.890 (3)	163 (3)
C7—H7⋯O9^v	0.93	2.59	3.459 (4)	156
C9—H9⋯O3	0.93	2.54	3.080 (4)	118
C9—H9⋯O10^vi	0.93	2.59	3.381 (3)	143

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

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

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Authors: Sirine Toumi; Samah Akriche Toumi; Mohamed Rzaigui
Journal: Acta Crystallogr Sect E Struct Rep Online Date: 2013-10-12

1 in total