Poly[[diaqua-μ₆-succinato-di-μ₅-succinato-diholmium(III)] monohydrate]

The Ho^III center in the title coordination polymer, {[Ho₂(C₄H₄O₄)₃(H₂O)₂]·H₂O}_n, is nine-coordinated in a tricapped trigonal prism by eight O atoms, derived from six carboxyl­ate groups and a water mol­ecule. One of the independent succinate anions is located about a crystallographic center of inversion and the uncoordinated water mol­ecule lies on a twofold axis. The crystal structure comprises edge-shared HoO₉ polyhedra linked by succinate bridges, forming a three-dimensional network structure.

Key indicators

• Single-crystal X-ray study
• T = 295 K
• Mean [sigma](C-C) = 0.006 Å
• R factor = 0.020
• wR factor = 0.049
• Data-to-parameter ratio = 15.6

checkCIF/PLATON results

No syntax errors found



Alert level C
CELLV02_ALERT_1_C  The supplied cell volume s.u. differs from that
            calculated from the cell parameter s.u.'s by > 2
            Calculated cell volume su =       8.57
            Cell volume su given      =       6.00
PLAT042_ALERT_1_C Calc. and Rep. MoietyFormula Strings Differ ....          ?
PLAT062_ALERT_4_C Rescale T(min) & T(max) by .....................       0.78
PLAT063_ALERT_3_C Crystal Probably too Large for Beam Size .......       0.67 mm
PLAT152_ALERT_1_C Supplied and Calc Volume s.u. Inconsistent .....          ?
PLAT764_ALERT_4_C Overcomplete CIF Bond List Detected (Rep/Expd) .       1.40 Ratio

Alert level G
ABSTM02_ALERT_3_G  When printed, the submitted absorption T values will be
            replaced by the scaled T values. Since the ratio of scaled T's
            is identical to the ratio of reported T values, the scaling
            does not imply a change to the absorption corrections used in
            the study.
            Ratio of Tmax expected/reported      0.778
            Tmax scaled      0.290 Tmin scaled      0.051

   0 ALERT level A = In general: serious problem
   0 ALERT level B = Potentially serious problem
   6 ALERT level C = Check and explain
   1 ALERT level G = General alerts; check

   3 ALERT type 1 CIF construction/syntax error, inconsistent or missing data
   0 ALERT type 2 Indicator that the structure model may be wrong or deficient
   2 ALERT type 3 Indicator that the structure quality may be low
   2 ALERT type 4 Improvement, methodology, query or suggestion

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Computing details

Data collection: RAPID-AUTO (Rigaku ,2004); cell refinement: RAPID-AUTO; data reduction: RAPID-AUTO; program(s) used to solve structure: SHELXS97 (Sheldrick, 1997a); program(s) used to refine structure: SHELXL97 (Sheldrick, 1997a); molecular graphics: SHELXTL (Sheldrick, 1997b); software used to prepare material for publication: SHELXTL.

Poly[[diaqua-µ₆-succinato-di-µ₅-succinato-diholmium(III)] monohydrate]

Crystal data

[Ho2(C4H4O4)3(H2O)2]·H2O	F(000) = 1376
Mr = 732.12	Dx = 2.712 Mg m^−3
Monoclinic, C2/c	Mo Kα radiation, λ = 0.71073 Å
Hall symbol: -C 2yc	Cell parameters from 8491 reflections
a = 19.852 (4) Å	θ = 3.0–27.5°
b = 7.6723 (15) Å	µ = 8.84 mm^−1
c = 13.800 (3) Å	T = 295 K
β = 121.46 (3)°	Prism, yellow
V = 1792.9 (6) Å^3	0.67 × 0.23 × 0.14 mm
Z = 4

Data collection

Rigaku R-AXIS RAPID IP area-detector diffractometer	2058 independent reflections
Radiation source: rotating anode	2011 reflections with I > 2σ(I)
Graphite monochromator	Rint = 0.036
oscillation scans	θmax = 27.5°, θmin = 3.0°
Absorption correction: multi-scan (Jacobson, 1998)	h = −25→25
Tmin = 0.066, Tmax = 0.373	k = −9→9
8553 measured reflections	l = −17→17

Refinement

Refinement on F^2	Primary atom site location: structure-invariant direct methods
Least-squares matrix: full	Secondary atom site location: difference Fourier map
R[F^2 > 2σ(F^2)] = 0.020	Hydrogen site location: inferred from neighbouring sites
wR(F^2) = 0.049	H-atom parameters constrained
S = 1.05	w = 1/[σ^2(Fo^2) + (0.0139P)^2 + 15.8528P] where P = (Fo^2 + 2Fc^2)/3
2058 reflections	(Δ/σ)max = 0.001
132 parameters	Δρmax = 0.92 e Å^−3
0 restraints	Δρmin = −1.59 e Å^−3

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
Ho1	0.268916 (8)	0.217620 (18)	0.230019 (11)	0.00885 (7)
O1W	0.33298 (16)	0.3880 (3)	0.1523 (2)	0.0192 (5)
H1A	0.3233	0.4962	0.1396	0.023*
H1B	0.3293	0.3492	0.0920	0.023*
O1	0.17158 (17)	0.7362 (3)	0.5283 (2)	0.0182 (5)
O2	0.18728 (14)	0.5174 (3)	0.6376 (2)	0.0163 (5)
O3	0.17989 (16)	0.5268 (3)	0.3411 (2)	0.0201 (5)
O4	0.19710 (19)	0.2451 (4)	0.3246 (3)	0.0232 (6)
O5	0.32311 (13)	0.4827 (3)	0.3393 (2)	0.0146 (5)
O6	0.40612 (16)	0.2702 (3)	0.3790 (2)	0.0203 (6)
C1	0.15305 (18)	0.5847 (5)	0.5384 (3)	0.0115 (6)
C2	0.0906 (2)	0.4836 (5)	0.4377 (3)	0.0153 (7)
H2A	0.0651	0.5606	0.3724	0.018*
H2B	0.0509	0.4449	0.4536	0.018*
C3	0.1230 (2)	0.3249 (5)	0.4077 (3)	0.0169 (7)
H3A	0.1564	0.2587	0.4764	0.020*
H3B	0.0791	0.2507	0.3562	0.020*
C4	0.17016 (19)	0.3706 (4)	0.3529 (3)	0.0122 (6)
C5	0.39427 (19)	0.4243 (5)	0.3927 (3)	0.0128 (6)
C6	0.4601 (2)	0.5446 (5)	0.4695 (3)	0.0237 (8)
H6A	0.4496	0.5925	0.5254	0.028*
H6B	0.4617	0.6407	0.4251	0.028*
O2W	0.5000	0.4745 (15)	0.2500	0.114 (3)
H2C	0.4608	0.4201	0.2445	0.136*

Atomic displacement parameters (Ų)

	U^11	U^22	U^33	U^12	U^13	U^23
Ho1	0.01035 (9)	0.00585 (11)	0.01101 (9)	−0.00045 (5)	0.00604 (7)	−0.00017 (5)
O1W	0.0298 (14)	0.0121 (13)	0.0242 (13)	−0.0027 (11)	0.0200 (11)	−0.0026 (10)
O1	0.0275 (14)	0.0093 (12)	0.0148 (12)	0.0002 (11)	0.0090 (11)	0.0005 (9)
O2	0.0168 (11)	0.0175 (13)	0.0109 (10)	−0.0023 (10)	0.0047 (9)	0.0028 (9)
O3	0.0305 (14)	0.0100 (12)	0.0323 (14)	−0.0021 (11)	0.0251 (12)	−0.0009 (10)
O4	0.0356 (16)	0.0113 (12)	0.0382 (17)	0.0001 (12)	0.0300 (15)	−0.0016 (12)
O5	0.0094 (10)	0.0162 (13)	0.0150 (11)	−0.0003 (10)	0.0041 (9)	−0.0043 (9)
O6	0.0137 (12)	0.0115 (13)	0.0263 (14)	−0.0005 (10)	0.0038 (11)	−0.0007 (10)
C1	0.0107 (14)	0.0129 (16)	0.0117 (14)	0.0045 (13)	0.0065 (12)	−0.0001 (12)
C2	0.0142 (15)	0.0186 (18)	0.0132 (15)	0.0001 (14)	0.0073 (13)	−0.0024 (13)
C3	0.0225 (17)	0.0147 (17)	0.0198 (16)	−0.0046 (15)	0.0155 (14)	−0.0041 (14)
C4	0.0149 (15)	0.0077 (15)	0.0151 (14)	−0.0021 (12)	0.0086 (12)	−0.0015 (12)
C5	0.0114 (15)	0.0129 (16)	0.0129 (14)	−0.0006 (13)	0.0054 (12)	0.0016 (12)
C6	0.0110 (17)	0.0168 (19)	0.031 (2)	−0.0015 (15)	0.0024 (15)	−0.0070 (16)
O2W	0.075 (5)	0.130 (9)	0.130 (8)	0.000	0.050 (6)	0.000

Geometric parameters (Å, º)

Ho1—O1W	2.429 (3)	O3—Ho1^v	2.276 (2)
Ho1—O1^i	2.448 (3)	O4—C4	1.259 (4)
Ho1—O2^i	2.496 (3)	O5—C5	1.286 (4)
Ho1—O2^ii	2.385 (3)	O5—Ho1^v	2.383 (3)
Ho1—O3^iii	2.276 (2)	O6—C5	1.239 (4)
Ho1—O4	2.392 (3)	C1—C2	1.507 (5)
Ho1—O5	2.423 (2)	C1—Ho1^iv	2.869 (3)
Ho1—O5^iii	2.383 (3)	C2—C3	1.531 (5)
Ho1—O6	2.442 (3)	C2—H2A	0.9700
Ho1—C5	2.813 (3)	C2—H2B	0.9700
Ho1—C1^i	2.869 (3)	C3—C4	1.520 (5)
O1W—H1A	0.8500	C3—H3A	0.9700
O1W—H1B	0.8501	C3—H3B	0.9700
O1—C1	1.249 (4)	C5—C6	1.496 (5)
O1—Ho1^iv	2.448 (3)	C6—C6^vi	1.514 (7)
O2—C1	1.277 (4)	C6—H6A	0.9700
O2—Ho1^ii	2.385 (3)	C6—H6B	0.9700
O2—Ho1^iv	2.496 (3)	O2W—H2C	0.8509
O3—C4	1.238 (4)
O3^iii—Ho1—O5^iii	76.21 (9)	O6—Ho1—C1^i	133.94 (9)
O3^iii—Ho1—O2^ii	77.16 (9)	O1^i—Ho1—C1^i	25.63 (9)
O5^iii—Ho1—O2^ii	68.42 (9)	O2^i—Ho1—C1^i	26.38 (9)
O3^iii—Ho1—O4	145.01 (10)	C5—Ho1—C1^i	112.78 (10)
O5^iii—Ho1—O4	74.64 (9)	Ho1—O1W—H1A	120.2
O2^ii—Ho1—O4	74.41 (10)	Ho1—O1W—H1B	116.5
O3^iii—Ho1—O5	130.91 (9)	H1A—O1W—H1B	104.2
O5^iii—Ho1—O5	152.00 (3)	C1—O1—Ho1^iv	96.4 (2)
O2^ii—Ho1—O5	106.96 (9)	C1—O2—Ho1^ii	154.7 (2)
O4—Ho1—O5	77.53 (9)	C1—O2—Ho1^iv	93.3 (2)
O3^iii—Ho1—O1W	72.61 (9)	Ho1^ii—O2—Ho1^iv	110.14 (9)
O5^iii—Ho1—O1W	134.29 (8)	C4—O3—Ho1^v	144.6 (2)
O2^ii—Ho1—O1W	132.81 (9)	C4—O4—Ho1	135.0 (2)
O4—Ho1—O1W	142.38 (9)	C5—O5—Ho1^v	151.2 (2)
O5—Ho1—O1W	70.04 (8)	C5—O5—Ho1	93.6 (2)
O3^iii—Ho1—O6	85.21 (10)	Ho1^v—O5—Ho1	112.75 (9)
O5^iii—Ho1—O6	138.38 (8)	C5—O6—Ho1	93.9 (2)
O2^ii—Ho1—O6	71.30 (9)	O1—C1—O2	118.3 (3)
O4—Ho1—O6	104.28 (11)	O1—C1—C2	121.6 (3)
O5—Ho1—O6	53.10 (8)	O2—C1—C2	120.1 (3)
O1W—Ho1—O6	70.84 (10)	O1—C1—Ho1^iv	57.98 (18)
O3^iii—Ho1—O1^i	82.40 (10)	O2—C1—Ho1^iv	60.27 (18)
O5^iii—Ho1—O1^i	70.63 (9)	C2—C1—Ho1^iv	178.6 (2)
O2^ii—Ho1—O1^i	137.42 (9)	C1—C2—C3	113.6 (3)
O4—Ho1—O1^i	105.44 (11)	C1—C2—H2A	108.9
O5—Ho1—O1^i	114.63 (9)	C3—C2—H2A	108.9
O1W—Ho1—O1^i	72.81 (9)	C1—C2—H2B	108.9
O6—Ho1—O1^i	143.61 (10)	C3—C2—H2B	108.9
O3^iii—Ho1—O2^i	128.35 (9)	H2A—C2—H2B	107.7
O5^iii—Ho1—O2^i	104.71 (9)	C4—C3—C2	113.9 (3)
O2^ii—Ho1—O2^i	152.54 (2)	C4—C3—H3A	108.8
O4—Ho1—O2^i	78.13 (9)	C2—C3—H3A	108.8
O5—Ho1—O2^i	66.01 (9)	C4—C3—H3B	108.8
O1W—Ho1—O2^i	71.69 (9)	C2—C3—H3B	108.8
O6—Ho1—O2^i	115.92 (9)	H3A—C3—H3B	107.7
O1^i—Ho1—O2^i	52.01 (8)	O3—C4—O4	125.4 (3)
O3^iii—Ho1—C5	107.36 (10)	O3—C4—C3	117.9 (3)
O5^iii—Ho1—C5	156.96 (9)	O4—C4—C3	116.7 (3)
O2^ii—Ho1—C5	89.87 (9)	O6—C5—O5	119.0 (3)
O4—Ho1—C5	92.64 (10)	O6—C5—C6	122.1 (3)
O5—Ho1—C5	27.14 (9)	O5—C5—C6	118.9 (3)
O1W—Ho1—C5	66.43 (9)	O6—C5—Ho1	60.00 (18)
O6—Ho1—C5	26.05 (9)	O5—C5—Ho1	59.28 (17)
O1^i—Ho1—C5	132.09 (9)	C6—C5—Ho1	174.3 (3)
O2^i—Ho1—C5	90.96 (9)	C5—C6—C6^vi	112.9 (4)
O3^iii—Ho1—C1^i	105.43 (10)	C5—C6—H6A	109.0
O5^iii—Ho1—C1^i	87.25 (9)	C6^vi—C6—H6A	109.0
O2^ii—Ho1—C1^i	154.42 (9)	C5—C6—H6B	109.0
O4—Ho1—C1^i	92.12 (10)	C6^vi—C6—H6B	109.0
O5—Ho1—C1^i	90.68 (9)	H6A—C6—H6B	107.8
O1W—Ho1—C1^i	70.20 (9)

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

Hydrogen-bond geometry (Å, º)

D—H···A	D—H	H···A	D···A	D—H···A
O1W—H1A···O4^v	0.85	2.06	2.857 (4)	155
O1W—H1B···O1^iii	0.85	1.86	2.709 (4)	172
O2W—H2C···O1W	0.85	2.18	2.930 (4)	147

Symmetry codes: (iii) −x+1/2, y−1/2, −z+1/2; (v) −x+1/2, y+1/2, −z+1/2.