Tris(1,2-dimeth-oxy-ethane-κO,O')iodidocalcium iodide.

In the title complex, [CaI(C(4)H(10)O(2))(3)]I, the Ca(II) atom is seven-coordinated by six O atoms from three 1,2-dimeth-oxy-ethane (DME) ligands and one iodide anion in a distorted penta-gonal-bipyramidal geometry. The I atom and one of the O atoms from a DME ligand lie in the axial positions while the other O atoms lie in the basal plane. The other iodide anion is outside the complex cation.

Related literature

For background to polylactide and its copolymers, see: Ha & Gardella (2005 ▶); Simpson et al. (2008 ▶). For ring-opening polymerization of lactides with calcium-based catalysts, see: Chen et al. (2007 ▶); Chisholm et al. (2003 ▶, 2004 ▶); Darensbourg et al. (2002 ▶, 2003a ▶,b ▶); Zhong et al. (2001 ▶).

Experimental

Crystal data

[CaI(C4H10O2)3]I

M = 564.24

Monoclinic,

a = 12.1503 (6) Å

b = 10.7767 (5) Å

c = 16.2295 (8) Å

β = 99.514 (1)°

V = 2095.86 (18) Å3

Z = 4

Mo Kα radiation

μ = 3.26 mm−1

T = 100 K

0.23 × 0.23 × 0.15 mm

Data collection

Bruker APEXII CCD diffractometer

Absorption correction: multi-scan (SADABS; Bruker, 2001 ▶) T min = 0.522, T max = 0.647

14842 measured reflections

4791 independent reflections

4627 reflections with I > 2σ(I)

R int = 0.017

Refinement

R[F 2 > 2σ(F 2)] = 0.016

wR(F 2) = 0.043

S = 1.19

4791 reflections

196 parameters

H-atom parameters constrained

Δρmax = 0.35 e Å−3

Δρmin = −0.91 e Å−3

Data collection: APEX2 (Bruker, 2007 ▶); cell refinement: SAINT (Bruker, 2007 ▶); data reduction: SAINT; program(s) used to solve structure: SHELXTL (Sheldrick, 2008 ▶); program(s) used to refine structure: SHELXTL; molecular graphics: SHELXTL; software used to prepare material for publication: SHELXTL.

Crystal structure: contains datablock(s) global, I. DOI: 10.1107/S160053681200075X/hy2505sup1.cif

Structure factors: contains datablock(s) I. DOI: 10.1107/S160053681200075X/hy2505Isup2.hkl

Additional supplementary materials: crystallographic information; 3D view; checkCIF report

[CaI(C4H10O2)3]I	F(000) = 1104
Mr = 564.24	Dx = 1.788 Mg m−3
Monoclinic, P21/c	Mo Kα radiation, λ = 0.71073 Å
Hall symbol: -P 2ybc	Cell parameters from 9874 reflections
a = 12.1503 (6) Å	θ = 2.0–28.0°
b = 10.7767 (5) Å	µ = 3.26 mm−1
c = 16.2295 (8) Å	T = 100 K
β = 99.514 (1)°	Blocks, colourless
V = 2095.86 (18) Å3	0.23 × 0.23 × 0.15 mm
Z = 4

Bruker APEXII CCD diffractometer	4791 independent reflections
Radiation source: fine-focus sealed tube	4627 reflections with I > 2σ(I)
graphite	Rint = 0.017
φ and ω scans	θmax = 27.5°, θmin = 1.7°
Absorption correction: multi-scan (SADABS; Bruker, 2001)	h = −15→15
Tmin = 0.522, Tmax = 0.647	k = −13→14
14842 measured reflections	l = −21→20

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)] = 0.016	Hydrogen site location: inferred from neighbouring sites
wR(F2) = 0.043	H-atom parameters constrained
S = 1.19	w = 1/[σ2(Fo2) + (0.0191P)2 + 0.9088P] where P = (Fo2 + 2Fc2)/3
4791 reflections	(Δ/σ)max = 0.005
196 parameters	Δρmax = 0.35 e Å−3
0 restraints	Δρmin = −0.91 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.

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	Uiso*/Ueq
Ca1	0.74096 (2)	0.25280 (3)	0.987454 (18)	0.01103 (6)
I1	0.589004 (9)	0.206685 (9)	1.116467 (6)	0.01643 (4)
I2	0.169983 (9)	0.297669 (9)	0.264013 (7)	0.01675 (4)
O1	0.91500 (9)	0.19272 (10)	1.07103 (7)	0.0141 (2)
O2	0.89431 (10)	0.28746 (10)	0.91541 (7)	0.0165 (2)
O3	0.80225 (9)	0.44050 (10)	1.07187 (7)	0.0152 (2)
O4	0.66028 (9)	0.44389 (10)	0.92287 (7)	0.0163 (2)
O5	0.60542 (9)	0.17389 (11)	0.87284 (7)	0.0164 (2)
O6	0.77110 (9)	0.02920 (10)	0.95308 (7)	0.0155 (2)
C1	0.92225 (14)	0.09314 (15)	1.13105 (10)	0.0178 (3)
H1A	0.8532	0.0897	1.1548	0.027*
H1B	0.9857	0.1078	1.1758	0.027*
H1C	0.9328	0.0143	1.1033	0.027*
C2	1.01205 (14)	0.19625 (14)	1.03155 (10)	0.0166 (3)
H2A	1.0198	0.1169	1.0024	0.020*
H2B	1.0797	0.2086	1.0740	0.020*
C3	0.99948 (14)	0.30183 (15)	0.96992 (11)	0.0185 (3)
H3A	1.0016	0.3821	0.9998	0.022*
H3B	1.0613	0.3005	0.9371	0.022*
C4	0.88796 (16)	0.3613 (2)	0.84086 (12)	0.0305 (4)
H4A	0.8171	0.3450	0.8040	0.046*
H4B	0.9500	0.3397	0.8119	0.046*
H4C	0.8925	0.4494	0.8559	0.046*
C5	0.84956 (14)	0.42976 (16)	1.15957 (10)	0.0193 (3)
H5A	0.9184	0.3808	1.1655	0.029*
H5B	0.7960	0.3885	1.1894	0.029*
H5C	0.8663	0.5127	1.1831	0.029*
C6	0.71418 (14)	0.53093 (15)	1.05910 (10)	0.0187 (3)
H6A	0.7380	0.6076	1.0907	0.022*
H6B	0.6471	0.4981	1.0790	0.022*
C7	0.68799 (15)	0.55864 (15)	0.96726 (11)	0.0200 (3)
H7A	0.6244	0.6170	0.9559	0.024*
H7B	0.7534	0.5975	0.9484	0.024*
C8	0.61548 (15)	0.46988 (16)	0.83621 (10)	0.0213 (3)
H8A	0.6066	0.3920	0.8046	0.032*
H8B	0.6668	0.5246	0.8127	0.032*
H8C	0.5427	0.5106	0.8327	0.032*
C9	0.48713 (14)	0.20029 (17)	0.85691 (12)	0.0231 (4)
H9A	0.4718	0.2731	0.8893	0.035*
H9B	0.4460	0.1287	0.8733	0.035*
H9C	0.4635	0.2169	0.7972	0.035*
C10	0.63075 (14)	0.06361 (15)	0.82961 (10)	0.0178 (3)
H10A	0.6216	0.0796	0.7688	0.021*
H10B	0.5797	−0.0045	0.8393	0.021*
C11	0.74998 (14)	0.02824 (15)	0.86297 (10)	0.0179 (3)
H11A	0.7652	−0.0557	0.8427	0.021*
H11B	0.8010	0.0873	0.8417	0.021*
C12	0.71396 (15)	−0.07020 (15)	0.98863 (11)	0.0201 (3)
H12A	0.7403	−0.0744	1.0490	0.030*
H12B	0.7294	−0.1491	0.9628	0.030*
H12C	0.6334	−0.0544	0.9782	0.030*

	U11	U22	U33	U12	U13	U23
Ca1	0.01102 (14)	0.01151 (14)	0.01052 (13)	−0.00026 (10)	0.00169 (10)	−0.00006 (10)
I1	0.01616 (6)	0.01888 (6)	0.01554 (6)	−0.00274 (3)	0.00641 (4)	0.00003 (3)
I2	0.01794 (6)	0.01398 (6)	0.01738 (6)	−0.00181 (3)	0.00008 (4)	0.00072 (3)
O1	0.0140 (5)	0.0152 (5)	0.0132 (5)	0.0014 (4)	0.0025 (4)	0.0007 (4)
O2	0.0161 (6)	0.0204 (6)	0.0132 (5)	−0.0004 (4)	0.0032 (4)	0.0048 (4)
O3	0.0160 (5)	0.0152 (5)	0.0132 (5)	0.0025 (4)	−0.0010 (4)	−0.0025 (4)
O4	0.0204 (6)	0.0127 (5)	0.0144 (5)	0.0004 (4)	−0.0013 (4)	0.0010 (4)
O5	0.0132 (5)	0.0182 (5)	0.0167 (5)	−0.0002 (4)	−0.0009 (4)	−0.0025 (4)
O6	0.0169 (5)	0.0137 (5)	0.0148 (5)	−0.0023 (4)	−0.0003 (4)	−0.0011 (4)
C1	0.0223 (8)	0.0171 (7)	0.0135 (7)	0.0011 (6)	0.0011 (6)	0.0029 (6)
C2	0.0134 (7)	0.0203 (8)	0.0165 (8)	0.0019 (6)	0.0034 (6)	−0.0010 (6)
C3	0.0142 (8)	0.0198 (8)	0.0216 (8)	−0.0027 (6)	0.0032 (6)	0.0001 (6)
C4	0.0237 (9)	0.0439 (12)	0.0260 (9)	0.0068 (8)	0.0102 (7)	0.0214 (8)
C5	0.0234 (8)	0.0192 (8)	0.0135 (7)	0.0005 (6)	−0.0021 (6)	−0.0037 (6)
C6	0.0186 (8)	0.0149 (7)	0.0216 (8)	0.0035 (6)	0.0007 (6)	−0.0043 (6)
C7	0.0227 (8)	0.0120 (7)	0.0233 (8)	0.0009 (6)	−0.0018 (7)	−0.0007 (6)
C8	0.0242 (9)	0.0237 (8)	0.0147 (8)	0.0015 (7)	−0.0005 (6)	0.0045 (6)
C9	0.0121 (8)	0.0301 (10)	0.0256 (9)	0.0001 (6)	−0.0009 (7)	0.0016 (7)
C10	0.0205 (8)	0.0180 (7)	0.0141 (7)	−0.0037 (6)	−0.0001 (6)	−0.0028 (6)
C11	0.0211 (8)	0.0176 (7)	0.0150 (7)	−0.0011 (6)	0.0032 (6)	−0.0043 (6)
C12	0.0225 (8)	0.0152 (7)	0.0219 (8)	−0.0039 (6)	0.0014 (7)	0.0021 (6)

Ca1—O1	2.4046 (12)	C3—H3B	0.9900
Ca1—O2	2.3872 (12)	C4—H4A	0.9800
Ca1—O3	2.4871 (11)	C4—H4B	0.9800
Ca1—O4	2.4415 (11)	C4—H4C	0.9800
Ca1—O5	2.4254 (12)	C5—H5A	0.9800
Ca1—O6	2.5138 (11)	C5—H5B	0.9800
Ca1—I1	3.0525 (3)	C5—H5C	0.9800
O1—C2	1.4325 (19)	C6—C7	1.502 (2)
O1—C1	1.4421 (18)	C6—H6A	0.9900
O2—C3	1.437 (2)	C6—H6B	0.9900
O2—C4	1.439 (2)	C7—H7A	0.9900
O3—C6	1.4369 (19)	C7—H7B	0.9900
O3—C5	1.4489 (18)	C8—H8A	0.9800
O4—C7	1.4427 (19)	C8—H8B	0.9800
O4—C8	1.4490 (19)	C8—H8C	0.9800
O5—C10	1.4390 (19)	C9—H9A	0.9800
O5—C9	1.446 (2)	C9—H9B	0.9800
O6—C11	1.4425 (19)	C9—H9C	0.9800
O6—C12	1.4473 (19)	C10—C11	1.509 (2)
C1—H1A	0.9800	C10—H10A	0.9900
C1—H1B	0.9800	C10—H10B	0.9900
C1—H1C	0.9800	C11—H11A	0.9900
C2—C3	1.506 (2)	C11—H11B	0.9900
C2—H2A	0.9900	C12—H12A	0.9800
C2—H2B	0.9900	C12—H12B	0.9800
C3—H3A	0.9900	C12—H12C	0.9800
O2—Ca1—O1	68.51 (4)	O2—C4—H4B	109.5
O2—Ca1—O5	99.51 (4)	H4A—C4—H4B	109.5
O1—Ca1—O5	139.51 (4)	O2—C4—H4C	109.5
O2—Ca1—O4	87.03 (4)	H4A—C4—H4C	109.5
O1—Ca1—O4	136.26 (4)	H4B—C4—H4C	109.5
O5—Ca1—O4	78.05 (4)	O3—C5—H5A	109.5
O2—Ca1—O3	87.46 (4)	O3—C5—H5B	109.5
O1—Ca1—O3	75.70 (4)	H5A—C5—H5B	109.5
O5—Ca1—O3	144.21 (4)	O3—C5—H5C	109.5
O4—Ca1—O3	67.23 (4)	H5A—C5—H5C	109.5
O2—Ca1—O6	83.52 (4)	H5B—C5—H5C	109.5
O1—Ca1—O6	73.76 (4)	O3—C6—C7	107.98 (13)
O5—Ca1—O6	66.36 (4)	O3—C6—H6A	110.1
O4—Ca1—O6	140.91 (4)	C7—C6—H6A	110.1
O3—Ca1—O6	149.37 (4)	O3—C6—H6B	110.1
O2—Ca1—I1	166.17 (3)	C7—C6—H6B	110.1
O1—Ca1—I1	98.31 (3)	H6A—C6—H6B	108.4
O5—Ca1—I1	93.32 (3)	O4—C7—C6	108.59 (13)
O4—Ca1—I1	100.74 (3)	O4—C7—H7A	110.0
O3—Ca1—I1	85.10 (3)	C6—C7—H7A	110.0
O6—Ca1—I1	97.06 (3)	O4—C7—H7B	110.0
C2—O1—C1	111.03 (12)	C6—C7—H7B	110.0
C2—O1—Ca1	116.92 (9)	H7A—C7—H7B	108.4
C1—O1—Ca1	122.09 (9)	O4—C8—H8A	109.5
C3—O2—C4	112.11 (13)	O4—C8—H8B	109.5
C3—O2—Ca1	113.70 (9)	H8A—C8—H8B	109.5
C4—O2—Ca1	124.09 (10)	O4—C8—H8C	109.5
C6—O3—C5	111.16 (12)	H8A—C8—H8C	109.5
C6—O3—Ca1	108.91 (9)	H8B—C8—H8C	109.5
C5—O3—Ca1	120.68 (9)	O5—C9—H9A	109.5
C7—O4—C8	109.77 (12)	O5—C9—H9B	109.5
C7—O4—Ca1	117.68 (9)	H9A—C9—H9B	109.5
C8—O4—Ca1	129.75 (9)	O5—C9—H9C	109.5
C10—O5—C9	111.20 (12)	H9A—C9—H9C	109.5
C10—O5—Ca1	119.39 (9)	H9B—C9—H9C	109.5
C9—O5—Ca1	126.65 (10)	O5—C10—C11	107.67 (12)
C11—O6—C12	112.47 (12)	O5—C10—H10A	110.2
C11—O6—Ca1	102.93 (8)	C11—C10—H10A	110.2
C12—O6—Ca1	121.60 (9)	O5—C10—H10B	110.2
O1—C1—H1A	109.5	C11—C10—H10B	110.2
O1—C1—H1B	109.5	H10A—C10—H10B	108.5
H1A—C1—H1B	109.5	O6—C11—C10	111.17 (13)
O1—C1—H1C	109.5	O6—C11—Ca1	50.70 (7)
H1A—C1—H1C	109.5	C10—C11—Ca1	84.46 (9)
H1B—C1—H1C	109.5	O6—C11—H11A	109.4
O1—C2—C3	108.45 (13)	C10—C11—H11A	109.4
O1—C2—H2A	110.0	Ca1—C11—H11A	159.8
C3—C2—H2A	110.0	O6—C11—H11B	109.4
O1—C2—H2B	110.0	C10—C11—H11B	109.4
C3—C2—H2B	110.0	Ca1—C11—H11B	79.7
H2A—C2—H2B	108.4	H11A—C11—H11B	108.0
O2—C3—C2	108.03 (13)	O6—C12—H12A	109.5
O2—C3—H3A	110.1	O6—C12—H12B	109.5
C2—C3—H3A	110.1	H12A—C12—H12B	109.5
O2—C3—H3B	110.1	O6—C12—H12C	109.5
C2—C3—H3B	110.1	H12A—C12—H12C	109.5
H3A—C3—H3B	108.4	H12B—C12—H12C	109.5
O2—C4—H4A	109.5

Table 1

Selected bond lengths (Å)

Ca1—O1	2.4046 (12)
Ca1—O2	2.3872 (12)
Ca1—O3	2.4871 (11)
Ca1—O4	2.4415 (11)
Ca1—O5	2.4254 (12)
Ca1—O6	2.5138 (11)
Ca1—I1	3.0525 (3)