Poly­[[hexaacetatodiethano­ltrimagnesium(II)] diethanol solvate], a polymeric acetate-bridged magnesium chain structure

The title compound, [Mg₃(C₂H₃O₂)₆(C₂H₆O)₂]·2C₂H₆O, contains infinite chains of magnesium ions bridged by acetate ligands in three different coordination modes. There are two independent Mg^II ions in the asymmetric unit, and one lies on a twofold axis. The coordination geometry around each Mg ion is distorted octahedral.

Key indicators

• Single-crystal X-ray study
• T = 150 K
• Mean [sigma](C-C) = 0.005 Å
Some non-H atoms missing
• R factor = 0.036
• wR factor = 0.092
• Data-to-parameter ratio = 12.0

checkCIF results

No syntax errors found

ADDSYM reports no extra symmetry


 Alert Level A:



ABSMU_01  Alert A The ratio of given/expected absorption coefficient lies
          outside the range 0.90 <> 1.10
          Calculated value of mu =     0.132
          Value of mu given      =     0.165

CHEMW_01  Alert A The ratio of given/expected molecular weight as calculated
          from the _chemical_formula_sum lies outside
          the range 0.90 <> 1.10
          Calculated formula weight =   483.4620
          Formula weight given      =   611.4700


 Alert Level C:



CHEMW_01  Alert C The difference between the given and expected weight for
          compound is greater 1 mass unit. Check that all hydrogen
          atoms have been taken into account.

STRVAL_01
         From the CIF: _refine_ls_abs_structure_Flack   -0.600
         From the CIF: _refine_ls_abs_structure_Flack_su    0.300
           Alert C Flack parameter is too small

General Notes



FORMU_01  There is a discrepancy between the atom counts in the
          _chemical_formula_sum and _chemical_formula_moiety. This is
          usually due to the moiety formula being in the wrong format.
          Atom count from _chemical_formula_sum:   C20 H42 Mg3 O8
          Atom count from _chemical_formula_moiety:C20 H42 Mg3 O16

FORMU_01  There is a discrepancy between the atom counts in the
          _chemical_formula_sum and the formula from the _atom_site* data.
          Atom count from _chemical_formula_sum:C20 H42 Mg3 O8
          Atom count from the _atom_site data:  C20 H42 Mg3 O16

CELLZ_01
         From the CIF: _cell_formula_units_Z    2
         From the CIF: _chemical_formula_sum  C20 H42 Mg3 O8
         TEST: Compare cell contents of formula and atom_site data

         atom    Z*formula  cif sites diff
         C         40.00     40.00    0.00
         H         84.00     84.00    0.00
         Mg         6.00      6.00    0.00
         O         16.00     32.00  -16.00
          Difference between formula and atom_site contents detected.
          ALERT: Large difference may be due to a
          symmetry error - see SYMMG tests

REFLT_03
         From the CIF: _diffrn_reflns_theta_max           27.46
         From the CIF: _reflns_number_total               2628
         Count of symmetry unique reflns         1829
         Completeness (_total/calc)            143.69%
         TEST3: Check Friedels for noncentro structure
         Estimate of Friedel pairs measured       799
         Fraction of Friedel pairs measured     0.437
         Are heavy atom types Z>Si present           no
          ALERT: MoKa measured Friedel data cannot be used to
                 determine absolute structure in a light-atom
                 study EXCEPT under VERY special conditions.
                 It is preferred that Friedel data is merged in such cases.


 2 Alert Level A = Potentially serious problem

 0 Alert Level B = Potential problem

 2 Alert Level C = Please check

---

Computing details

Data collection: DENZO (Otwinoski & Minor, 1997) and COLLECT (Hooft, 1998); cell refinement: DENZO and COLLECT; data reduction: DENZO, COLLECT and maXus (Mackay et al., 1998); program(s) used to solve structure: SHELXS97 (Sheldrick, 1997); program(s) used to refine structure: SHELXL97 (Sheldrick, 1997); molecular graphics: CAMERON (Watkin et al., 1993) and ATOMS (Dowty, 1999); software used to prepare material for publication: WinGX (Farrugia et al., 1998).

Poly[hexakis-acetato bis-ethanol trismagnesium(II)] ethanol solvate

Crystal data

[Mg3(C2H3O2)6(C2H6O)2]·2C2H6O	Dx = 1.322 Mg m^−3
Mr = 611.47	Melting point: not measured K
Monoclinic, C2	Mo Kα radiation, λ = 0.71073 Å
a = 13.3931 (8) Å	Cell parameters from 4981 reflections
b = 16.2214 (12) Å	θ = 3.2–27.5°
c = 8.3414 (6) Å	µ = 0.17 mm^−1
β = 122.013 (3)°	T = 150 K
V = 1536.62 (18) Å^3	Block, colourless
Z = 2	0.2 × 0.1 × 0.1 mm
F(000) = 652

Data collection

Nonius KappaCCD area-detector diffractometer	2628 independent reflections
Radiation source: Nonius FR591 rotating anode	2434 reflections with I > 2σ(I)
Graphite monochromator	Rint = 0.026
Detector resolution: 9.091 pixels per mm pixels mm^-1	θmax = 27.5°, θmin = 3.2°
Φ and ω scans to fill Ewald sphere	h = −17→17
Absorption correction: multi-scan (SORTAV; Blessing, 1995)	k = −20→16
Tmin = 0.941, Tmax = 0.962	l = −10→10
4981 measured reflections

Refinement

Refinement on F^2	H atoms treated by a mixture of independent and constrained refinement
Least-squares matrix: full	w = 1/[σ^2(Fo^2) + (0.034P)^2 + 1.1389P] where P = (Fo^2 + 2Fc^2)/3
R[F^2 > 2σ(F^2)] = 0.036	(Δ/σ)max < 0.001
wR(F^2) = 0.092	Δρmax = 0.53 e Å^−3
S = 1.08	Δρmin = −0.25 e Å^−3
2628 reflections	Absolute structure: Flack (1983), 799 Friedel pairs
219 parameters	Absolute structure parameter: −0.6 (3)
1 restraint

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	Occ. (<1)
Mg1	1	0.58208 (7)	0.5	0.0180 (3)
Mg2	0.90869 (6)	0.68968 (6)	0.77402 (10)	0.01791 (19)
O1	0.94170 (13)	0.69743 (12)	0.5542 (2)	0.0186 (4)
O2	0.84674 (15)	0.57378 (12)	0.6900 (2)	0.0234 (4)
O3	0.89785 (16)	0.49772 (12)	0.5234 (3)	0.0246 (4)
O4	0.87380 (15)	0.58825 (12)	0.2172 (2)	0.0226 (4)
O5	0.91139 (14)	0.66336 (11)	0.0303 (2)	0.0189 (4)
O6	0.94158 (15)	0.81119 (12)	0.8425 (2)	0.0233 (4)
O7	0.73631 (16)	0.72984 (14)	0.6007 (3)	0.0258 (5)
O8	0.6514 (2)	0.85627 (17)	0.6878 (4)	0.0494 (7)
C1	1	0.7375 (2)	0.5	0.0188 (7)
C2	1	0.8279 (3)	0.5	0.0450 (12)
C3	0.8375 (2)	0.51123 (18)	0.5965 (3)	0.0222 (6)
C4	0.7477 (3)	0.4467 (2)	0.5649 (5)	0.0389 (8)
C5	0.8417 (2)	0.62350 (17)	0.0642 (3)	0.0197 (5)
C6	0.7141 (2)	0.6176 (3)	−0.0888 (4)	0.0302 (7)
C7	1	0.8471 (2)	1	0.0238 (8)
C8	1	0.9404 (3)	1	0.0427 (12)
C9	0.6315 (2)	0.6919 (3)	0.4485 (4)	0.0344 (7)
C10	0.6399 (2)	0.6809 (3)	0.2781 (4)	0.0410 (8)
C11	0.6931 (3)	0.8752 (2)	0.8793 (5)	0.0467 (9)
C12	0.5979 (4)	0.8737 (3)	0.9161 (5)	0.0666 (12)
H2A	1.0312	0.8481	0.6288	0.067*	0.5
H2B	0.9193	0.8481	0.4169	0.067*	0.5
H2C	1.0495	0.8481	0.4542	0.067*	0.5
H4A	0.706 (4)	0.461 (3)	0.625 (6)	0.077 (14)*
H4B	0.791 (4)	0.391 (3)	0.630 (6)	0.068 (13)*
H4C	0.699 (3)	0.428 (3)	0.428 (6)	0.059 (11)*
H6A	0.677 (3)	0.595 (2)	−0.034 (5)	0.039 (9)*
H6B	0.697 (5)	0.668 (5)	−0.125 (8)	0.12 (2)*
H6C	0.710 (3)	0.584 (2)	−0.188 (5)	0.043 (9)*
H7O	0.722 (3)	0.766 (3)	0.640 (5)	0.045 (12)*
H8A	1.0326	0.9605	0.9262	0.064*	0.5
H8B	0.9191	0.9605	0.9435	0.064*	0.5
H8C	1.0483	0.9605	1.1302	0.064*	0.5
H8O	0.633 (3)	0.896 (3)	0.614 (5)	0.051 (11)*
H9A	0.615 (3)	0.631 (3)	0.493 (5)	0.053 (11)*
H9B	0.560 (3)	0.732 (2)	0.420 (4)	0.044 (9)*
H10A	0.5678	0.6547	0.177	0.061*
H10B	0.7078	0.6459	0.3105	0.061*
H10C	0.6496	0.7348	0.2351	0.061*
H11A	0.7298	0.9306	0.9096	0.056*
H11B	0.7543	0.8348	0.9624	0.056*
H12A	0.6295	0.8869	1.0492	0.1*
H12B	0.5623	0.8186	0.8881	0.1*
H12C	0.538	0.9144	0.8356	0.1*

Atomic displacement parameters (Ų)

	U^11	U^22	U^33	U^12	U^13	U^23
Mg1	0.0221 (6)	0.0189 (6)	0.0170 (6)	0	0.0131 (5)	0
Mg2	0.0191 (4)	0.0227 (4)	0.0141 (4)	0.0000 (4)	0.0103 (3)	0.0000 (3)
O1	0.0220 (8)	0.0224 (9)	0.0162 (7)	0.0009 (8)	0.0135 (6)	0.0010 (7)
O2	0.0259 (9)	0.0237 (10)	0.0226 (9)	−0.0029 (8)	0.0143 (8)	−0.0024 (8)
O3	0.0353 (10)	0.0225 (10)	0.0239 (9)	−0.0085 (8)	0.0209 (8)	−0.0053 (8)
O4	0.0263 (9)	0.0254 (10)	0.0163 (8)	−0.0047 (8)	0.0114 (7)	0.0013 (8)
O5	0.0198 (8)	0.0232 (10)	0.0172 (7)	−0.0023 (7)	0.0122 (6)	0.0000 (7)
O6	0.0281 (9)	0.0236 (10)	0.0203 (9)	−0.0007 (8)	0.0142 (7)	0.0005 (8)
O7	0.0222 (9)	0.0318 (12)	0.0221 (10)	0.0038 (9)	0.0109 (8)	0.0006 (9)
O8	0.0775 (17)	0.0389 (14)	0.0519 (15)	0.0271 (13)	0.0480 (14)	0.0218 (12)
C1	0.0200 (16)	0.026 (2)	0.0122 (16)	0	0.0098 (14)	0
C2	0.069 (3)	0.030 (3)	0.070 (3)	0	0.059 (3)	0
C3	0.0240 (12)	0.0251 (15)	0.0153 (11)	−0.0022 (12)	0.0089 (10)	0.0025 (11)
C4	0.0456 (19)	0.043 (2)	0.0415 (19)	−0.0164 (17)	0.0321 (17)	−0.0110 (16)
C5	0.0232 (12)	0.0221 (14)	0.0179 (12)	−0.0014 (11)	0.0137 (10)	−0.0014 (10)
C6	0.0227 (13)	0.050 (2)	0.0194 (13)	−0.0072 (14)	0.0119 (11)	0.0022 (14)
C7	0.0251 (18)	0.023 (2)	0.0256 (19)	0	0.0153 (16)	0
C8	0.055 (3)	0.028 (2)	0.036 (2)	0	0.018 (2)	0
C9	0.0224 (12)	0.056 (2)	0.0213 (13)	0.0010 (16)	0.0089 (10)	0.0012 (15)
C10	0.0293 (14)	0.066 (2)	0.0233 (13)	0.0029 (16)	0.0111 (11)	−0.0016 (16)
C11	0.050 (2)	0.040 (2)	0.052 (2)	0.0048 (17)	0.0277 (17)	0.0036 (17)
C12	0.068 (2)	0.092 (4)	0.046 (2)	0.011 (2)	0.0352 (19)	0.015 (2)

Geometric parameters (Å, º)

O4—C5	1.249 (3)	C2—H2C	0.9800
O4—Mg1	2.0503 (16)	C2—H2A	0.9800
O5—C5	1.284 (3)	C2—H2B	0.9800
O5—Mg2^i	2.1173 (17)	O8—C11	1.418 (4)
O5—Mg2^ii	2.1614 (18)	O8—H8O	0.83 (4)
O6—C7	1.260 (3)	C3—O2	1.245 (3)
O6—Mg2	2.034 (2)	C3—C4	1.508 (4)
O3—C3	1.264 (3)	C4—H4C	1.01 (4)
O3—Mg1	2.016 (2)	C4—H4A	0.95 (5)
C1—O1	1.269 (3)	C4—H4B	1.05 (5)
C1—O1^i	1.269 (3)	C11—C12	1.462 (5)
C1—C2	1.467 (6)	C11—H11A	0.9900
C1—Mg1	2.521 (4)	C11—H11B	0.9900
C7—O6^iii	1.260 (3)	C12—H12A	0.9800
C7—C8	1.513 (6)	C12—H12B	0.9800
C5—C6	1.499 (4)	C12—H12C	0.9800
C9—O7	1.439 (3)	Mg1—O3^i	2.016 (2)
C9—C10	1.495 (4)	Mg1—O4^i	2.0503 (16)
C9—H9B	1.08 (4)	Mg1—O1^i	2.165 (2)
C9—H9A	1.11 (4)	Mg1—O1	2.165 (2)
C10—H10A	0.9800	Mg1—Mg2^i	3.5679 (10)
C10—H10B	0.9800	Mg1—Mg2	3.5679 (10)
C10—H10C	0.9800	Mg2—O2	2.024 (2)
C6—H6C	0.97 (4)	Mg2—O7	2.075 (2)
C6—H6A	0.90 (3)	Mg2—O1	2.1056 (17)
C6—H6B	0.86 (7)	Mg2—O5^i	2.1173 (17)
C8—H8C	0.9800	Mg2—O5^iv	2.1614 (18)
C8—H8B	0.9800	Mg2—Mg2^iii	3.2278 (15)
C8—H8A	0.9800	O7—H7O	0.75 (4)
C5—O4—Mg1	145.63 (17)	O3—Mg1—O4^i	96.30 (8)
C5—O5—Mg2^i	126.50 (15)	O3^i—Mg1—O4^i	87.51 (7)
C5—O5—Mg2^ii	133.18 (15)	O3—Mg1—O4	87.51 (7)
Mg2^i—O5—Mg2^ii	97.94 (7)	O3^i—Mg1—O4	96.30 (8)
C7—O6—Mg2	131.5 (2)	O4^i—Mg1—O4	174.41 (13)
C3—O3—Mg1	124.72 (18)	O3—Mg1—O1^i	160.89 (8)
O1—C1—O1^i	118.4 (3)	O3^i—Mg1—O1^i	103.18 (7)
O1—C1—C2	120.82 (17)	O4^i—Mg1—O1^i	91.68 (7)
O1^i—C1—C2	120.82 (17)	O4—Mg1—O1^i	83.47 (7)
O1—C1—Mg1	59.18 (17)	O3—Mg1—O1	103.18 (7)
O1^i—C1—Mg1	59.18 (17)	O3^i—Mg1—O1	160.89 (8)
C2—C1—Mg1	180.000 (1)	O4^i—Mg1—O1	83.47 (7)
O6—C7—O6^iii	124.9 (4)	O4—Mg1—O1	91.68 (7)
O6—C7—C8	117.54 (18)	O1^i—Mg1—O1	60.45 (9)
O6^iii—C7—C8	117.54 (18)	O3—Mg1—C1	132.75 (6)
O4—C5—O5	124.0 (2)	O3^i—Mg1—C1	132.75 (6)
O4—C5—C6	117.4 (2)	O4^i—Mg1—C1	87.20 (6)
O5—C5—C6	118.6 (2)	O4—Mg1—C1	87.20 (6)
O7—C9—C10	111.1 (2)	O1^i—Mg1—C1	30.22 (5)
O7—C9—H9B	105.8 (18)	O1—Mg1—C1	30.22 (5)
C10—C9—H9B	111.6 (17)	O3—Mg1—Mg2^i	150.99 (5)
O7—C9—H9A	110.9 (19)	O3^i—Mg1—Mg2^i	77.85 (5)
C10—C9—H9A	110 (2)	O4^i—Mg1—Mg2^i	111.08 (6)
H9B—C9—H9A	108 (3)	O4—Mg1—Mg2^i	65.96 (5)
C9—C10—H10A	109.5	O1^i—Mg1—Mg2^i	32.82 (4)
C9—C10—H10B	109.5	O1—Mg1—Mg2^i	89.71 (5)
H10A—C10—H10B	109.5	C1—Mg1—Mg2^i	60.71 (2)
C9—C10—H10C	109.5	O3—Mg1—Mg2	77.85 (5)
H10A—C10—H10C	109.5	O3^i—Mg1—Mg2	150.99 (5)
H10B—C10—H10C	109.5	O4^i—Mg1—Mg2	65.96 (5)
C5—C6—H6C	106 (2)	O4—Mg1—Mg2	111.08 (6)
C5—C6—H6A	106 (2)	O1^i—Mg1—Mg2	89.71 (5)
H6C—C6—H6A	114 (3)	O1—Mg1—Mg2	32.82 (4)
C5—C6—H6B	102 (4)	C1—Mg1—Mg2	60.71 (2)
H6C—C6—H6B	110 (4)	Mg2^i—Mg1—Mg2	121.43 (4)
H6A—C6—H6B	116 (5)	O2—Mg2—O6	170.09 (8)
C7—C8—H8C	109.5	O2—Mg2—O7	87.13 (8)
C7—C8—H8B	109.5	O6—Mg2—O7	83.50 (8)
H8C—C8—H8B	109.5	O2—Mg2—O1	89.47 (8)
C7—C8—H8A	109.5	O6—Mg2—O1	94.16 (8)
H8C—C8—H8A	109.5	O7—Mg2—O1	92.52 (7)
H8B—C8—H8A	109.5	O2—Mg2—O5^i	99.77 (8)
C1—C2—H2C	109.5	O6—Mg2—O5^i	89.45 (8)
C1—C2—H2A	109.5	O7—Mg2—O5^i	172.58 (9)
H2C—C2—H2A	109.5	O1—Mg2—O5^i	90.28 (7)
C1—C2—H2B	109.5	O2—Mg2—O5^iv	87.00 (8)
H2C—C2—H2B	109.5	O6—Mg2—O5^iv	91.50 (8)
H2A—C2—H2B	109.5	O7—Mg2—O5^iv	100.39 (7)
C11—O8—H8O	117 (3)	O1—Mg2—O5^iv	166.41 (7)
O2—C3—O3	124.5 (2)	O5^i—Mg2—O5^iv	77.42 (7)
O2—C3—C4	118.7 (2)	O2—Mg2—Mg2^iii	108.79 (5)
O3—C3—C4	116.8 (3)	O6—Mg2—Mg2^iii	75.81 (5)
C3—C4—H4C	113 (2)	O7—Mg2—Mg2^iii	133.49 (7)
C3—C4—H4A	112 (3)	O1—Mg2—Mg2^iii	129.66 (6)
H4C—C4—H4A	117 (3)	O5^i—Mg2—Mg2^iii	41.54 (5)
C3—C4—H4B	109 (2)	O5^iv—Mg2—Mg2^iii	40.52 (5)
H4C—C4—H4B	100 (3)	O2—Mg2—Mg1	62.66 (5)
H4A—C4—H4B	104 (3)	O6—Mg2—Mg1	123.86 (6)
O8—C11—C12	111.4 (3)	O7—Mg2—Mg1	109.86 (6)
O8—C11—H11A	109.3	O1—Mg2—Mg1	33.88 (5)
C12—C11—H11A	109.3	O5^i—Mg2—Mg1	76.04 (5)
O8—C11—H11B	109.3	O5^iv—Mg2—Mg1	134.85 (6)
C12—C11—H11B	109.3	Mg2^iii—Mg2—Mg1	116.32 (3)
H11A—C11—H11B	108.0	C1—O1—Mg2	142.51 (16)
C11—C12—H12A	109.5	C1—O1—Mg1	90.60 (18)
C11—C12—H12B	109.5	Mg2—O1—Mg1	113.31 (8)
H12A—C12—H12B	109.5	C3—O2—Mg2	149.32 (17)
C11—C12—H12C	109.5	C9—O7—Mg2	133.2 (2)
H12A—C12—H12C	109.5	C9—O7—H7O	111 (3)
H12B—C12—H12C	109.5	Mg2—O7—H7O	113 (3)
O3—Mg1—O3^i	94.51 (12)

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

Hydrogen-bond geometry (Å, º)

D—H···A	D—H	H···A	D···A	D—H···A
O8—H8O···O3^v	0.83 (4)	1.92 (4)	2.751 (3)	172 (4)
O7—H7O···O8	0.75 (4)	1.89 (4)	2.628 (3)	167 (4)

Symmetry code: (v) −x+3/2, y+1/2, −z+1.