Triaqua­[N-(5-formysalicyl­idene)glycinato(2–)-κ³O,N,O′]zinc(II) monohydrate

The title complex, [Zn(C₁₀H₇NO₄)(H₂O)₃]·H₂O, is a mononuclear complex. The Zn^II atom is coordinated by one N and two O atoms from one Schiff base ligand, and by three O atoms from water mol­ecules. In the crystal structure, the mol­ecules are linked through intra- and inter­molecular O—H...O hydrogen bonds, forming a three-dimensional framework.

Key indicators

• Single-crystal X-ray study
• T = 293 K
• Mean [sigma](C-C) = 0.004 Å
• R factor = 0.037
• wR factor = 0.098
• Data-to-parameter ratio = 13.8

checkCIF/PLATON results

No syntax errors found



Alert level C
PLAT735_ALERT_1_C D-H     Calc     0.85(5), Rep     0.85(2) ......       2.50 su-Ra
              O8   -H8B     1.555   1.555
PLAT736_ALERT_1_C H...A   Calc     1.99(5), Rep     1.99(2) ......       2.50 su-Ra
              H8B  -O7      1.555   1.555

Alert level G
PLAT199_ALERT_1_G Check the Reported _cell_measurement_temperature        293 K
PLAT200_ALERT_1_G Check the Reported _diffrn_ambient_temperature .        293 K

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

   4 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
   0 ALERT type 3 Indicator that the structure quality may be low
   0 ALERT type 4 Improvement, methodology, query or suggestion
   0 ALERT type 5 Informative message, check

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Computing details

Data collection: SMART (Bruker, 1998); cell refinement: SAINT (Bruker, 1998); data reduction: SAINT; 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.

Triaqua[N-(5-formysalicylidene)glycinato(2-)-κ³O,N,O']zinc(II) monohydrate

Crystal data

[Zn(C10H7NO4)(H2O)3]·H2O	F(000) = 1408
Mr = 342.60	Dx = 1.686 Mg m^−3
Orthorhombic, Pbca	Mo Kα radiation, λ = 0.71073 Å
Hall symbol: -P 2ac 2ab	Cell parameters from 987 reflections
a = 11.232 (4) Å	θ = 2.2–26.5°
b = 7.759 (3) Å	µ = 1.86 mm^−1
c = 30.973 (11) Å	T = 293 K
V = 2699.3 (16) Å^3	Block, yellow
Z = 8	0.15 × 0.10 × 0.08 mm

Data collection

Bruker SMART CCD area-detector diffractometer	2947 independent reflections
Radiation source: fine-focus sealed tube	2270 reflections with I > 2σ(I)
Graphite monochromator	Rint = 0.042
φ and ω scans	θmax = 27.0°, θmin = 1.3°
Absorption correction: multi-scan (SADABS; Sheldrick, 1996)	h = −14→11
Tmin = 0.768, Tmax = 0.866	k = −9→9
12398 measured reflections	l = −30→39

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)] = 0.037	Hydrogen site location: inferred from neighbouring sites
wR(F^2) = 0.099	H atoms treated by a mixture of independent and constrained refinement
S = 1.05	w = 1/[σ^2(Fo^2) + (0.0545P)^2 + 0.3452P] where P = (Fo^2 + 2Fc^2)/3
2947 reflections	(Δ/σ)max = 0.001
213 parameters	Δρmax = 0.44 e Å^−3
12 restraints	Δρmin = −0.75 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
Zn1	0.44008 (3)	0.07696 (4)	0.323024 (10)	0.02573 (12)
N1	0.5810 (2)	0.0470 (3)	0.36594 (7)	0.0252 (5)
O1	0.35816 (18)	0.2286 (3)	0.36731 (6)	0.0329 (5)
O2	0.3814 (3)	0.4087 (4)	0.56697 (8)	0.0603 (7)
O3	0.56227 (17)	−0.0721 (3)	0.28558 (7)	0.0323 (5)
O4	0.74188 (18)	−0.1893 (3)	0.28451 (7)	0.0370 (5)
O5	0.3611 (2)	−0.1553 (3)	0.34171 (9)	0.0490 (6)
O6	0.3066 (2)	0.0856 (3)	0.27826 (7)	0.0417 (6)
O7	0.5141 (2)	0.3059 (3)	0.29299 (7)	0.0334 (5)
O8	0.5196 (3)	0.5900 (4)	0.35071 (10)	0.0585 (7)
C1	0.5799 (3)	0.0857 (4)	0.40573 (9)	0.0293 (6)
H1	0.6446	0.0500	0.4222	0.035*
C2	0.4870 (3)	0.1804 (4)	0.42788 (9)	0.0274 (6)
C3	0.5029 (3)	0.2089 (4)	0.47218 (9)	0.0342 (7)
H3	0.5696	0.1619	0.4856	0.041*
C4	0.4240 (3)	0.3038 (4)	0.49683 (10)	0.0367 (7)
C5	0.3262 (3)	0.3777 (4)	0.47639 (10)	0.0397 (8)
H5	0.2734	0.4448	0.4923	0.048*
C6	0.3068 (3)	0.3530 (4)	0.43333 (10)	0.0379 (7)
H6	0.2413	0.4054	0.4205	0.045*
C7	0.3833 (3)	0.2501 (4)	0.40753 (9)	0.0274 (6)
C8	0.4458 (3)	0.3292 (5)	0.54278 (10)	0.0461 (9)
H8	0.5144	0.2807	0.5544	0.055*
C9	0.6830 (3)	−0.0475 (4)	0.34861 (9)	0.0305 (7)
H9A	0.6995	−0.1462	0.3669	0.037*
H9B	0.7526	0.0265	0.3489	0.037*
C10	0.6596 (3)	−0.1085 (3)	0.30279 (9)	0.0261 (6)
H5A	0.398 (3)	−0.253 (3)	0.3421 (15)	0.072 (14)*
H5B	0.2900 (18)	−0.183 (5)	0.3469 (14)	0.072 (14)*
H6A	0.299 (3)	0.161 (3)	0.2594 (9)	0.052 (12)*
H6B	0.284 (4)	−0.009 (3)	0.2690 (12)	0.076 (15)*
H7A	0.485 (2)	0.348 (4)	0.2708 (8)	0.044 (10)*
H7B	0.5883 (15)	0.305 (4)	0.2906 (10)	0.041 (10)*
H8A	0.532 (6)	0.578 (7)	0.3765 (8)	0.14 (3)*
H8B	0.516 (6)	0.509 (6)	0.3323 (15)	0.11 (2)*

Atomic displacement parameters (Ų)

	U^11	U^22	U^33	U^12	U^13	U^23
Zn1	0.02540 (19)	0.0320 (2)	0.01975 (19)	0.00256 (14)	−0.00212 (12)	−0.00263 (13)
N1	0.0264 (12)	0.0275 (12)	0.0216 (12)	0.0013 (10)	−0.0015 (9)	−0.0050 (9)
O1	0.0337 (12)	0.0426 (12)	0.0225 (10)	0.0097 (10)	−0.0038 (8)	−0.0059 (9)
O2	0.0651 (18)	0.087 (2)	0.0293 (13)	0.0054 (15)	0.0080 (12)	−0.0185 (13)
O3	0.0296 (11)	0.0442 (12)	0.0231 (10)	0.0066 (10)	−0.0027 (8)	−0.0063 (9)
O4	0.0299 (11)	0.0474 (13)	0.0336 (11)	0.0073 (10)	0.0021 (9)	−0.0152 (10)
O5	0.0313 (13)	0.0378 (14)	0.0779 (19)	−0.0040 (11)	0.0095 (13)	0.0120 (13)
O6	0.0482 (15)	0.0419 (14)	0.0351 (13)	−0.0058 (12)	−0.0191 (11)	0.0059 (12)
O7	0.0306 (12)	0.0426 (13)	0.0271 (12)	−0.0027 (10)	−0.0017 (9)	0.0074 (10)
O8	0.0679 (19)	0.0480 (16)	0.0596 (19)	0.0083 (14)	−0.0101 (15)	−0.0059 (14)
C1	0.0281 (15)	0.0347 (16)	0.0253 (15)	0.0013 (13)	−0.0060 (11)	0.0004 (12)
C2	0.0325 (15)	0.0303 (14)	0.0194 (14)	0.0008 (12)	0.0005 (11)	−0.0028 (12)
C3	0.0405 (18)	0.0403 (17)	0.0218 (15)	0.0039 (15)	−0.0046 (13)	−0.0019 (13)
C4	0.0450 (19)	0.0437 (18)	0.0214 (15)	−0.0024 (15)	0.0033 (13)	−0.0054 (13)
C5	0.0386 (18)	0.0483 (18)	0.0321 (18)	0.0033 (15)	0.0095 (13)	−0.0115 (14)
C6	0.0350 (17)	0.0457 (18)	0.0329 (17)	0.0113 (15)	−0.0017 (14)	−0.0073 (15)
C7	0.0297 (15)	0.0299 (15)	0.0225 (15)	−0.0032 (13)	0.0010 (11)	−0.0009 (12)
C8	0.055 (2)	0.059 (2)	0.0247 (17)	−0.0018 (19)	0.0040 (15)	−0.0089 (16)
C9	0.0272 (15)	0.0355 (16)	0.0287 (16)	0.0042 (13)	−0.0035 (12)	−0.0043 (12)
C10	0.0273 (15)	0.0245 (14)	0.0265 (15)	−0.0030 (12)	0.0020 (12)	−0.0008 (11)

Geometric parameters (Å, º)

Zn1—O1	2.028 (2)	O8—H8A	0.85 (2)
Zn1—O6	2.043 (2)	O8—H8B	0.85 (5)
Zn1—N1	2.080 (2)	C1—C2	1.450 (4)
Zn1—O5	2.090 (2)	C1—H1	0.9300
Zn1—O3	2.137 (2)	C2—C3	1.401 (4)
Zn1—O7	2.171 (2)	C2—C7	1.430 (4)
N1—C1	1.269 (4)	C3—C4	1.382 (4)
N1—C9	1.461 (4)	C3—H3	0.9300
O1—C7	1.288 (3)	C4—C5	1.391 (5)
O2—C8	1.210 (4)	C4—C8	1.457 (4)
O3—C10	1.248 (3)	C5—C6	1.365 (4)
O4—C10	1.252 (3)	C5—H5	0.9300
O5—H5A	0.865 (18)	C6—C7	1.420 (4)
O5—H5B	0.843 (18)	C6—H6	0.9300
O6—H6A	0.830 (17)	C8—H8	0.9300
O6—H6B	0.830 (18)	C9—C10	1.519 (4)
O7—H7A	0.827 (17)	C9—H9A	0.9700
O7—H7B	0.837 (17)	C9—H9B	0.9700
O1—Zn1—O6	96.14 (10)	C2—C1—H1	117.0
O1—Zn1—N1	88.74 (8)	C3—C2—C7	118.4 (3)
O6—Zn1—N1	174.70 (10)	C3—C2—C1	116.8 (3)
O1—Zn1—O5	96.92 (10)	C7—C2—C1	124.7 (2)
O6—Zn1—O5	84.55 (11)	C4—C3—C2	122.9 (3)
N1—Zn1—O5	92.84 (10)	C4—C3—H3	118.6
O1—Zn1—O3	166.54 (8)	C2—C3—H3	118.6
O6—Zn1—O3	96.94 (9)	C3—C4—C5	118.3 (3)
N1—Zn1—O3	78.31 (9)	C3—C4—C8	120.3 (3)
O5—Zn1—O3	87.48 (10)	C5—C4—C8	121.4 (3)
O1—Zn1—O7	89.35 (9)	C6—C5—C4	120.9 (3)
O6—Zn1—O7	87.89 (9)	C6—C5—H5	119.6
N1—Zn1—O7	94.24 (9)	C4—C5—H5	119.6
O5—Zn1—O7	170.64 (10)	C5—C6—C7	122.1 (3)
O3—Zn1—O7	87.97 (8)	C5—C6—H6	118.9
C1—N1—C9	118.9 (2)	C7—C6—H6	118.9
C1—N1—Zn1	125.9 (2)	O1—C7—C6	119.0 (3)
C9—N1—Zn1	114.70 (17)	O1—C7—C2	123.8 (3)
C7—O1—Zn1	129.03 (18)	C6—C7—C2	117.2 (3)
C10—O3—Zn1	116.93 (18)	O2—C8—C4	125.0 (4)
Zn1—O5—H5A	124 (3)	O2—C8—H8	117.5
Zn1—O5—H5B	132 (3)	C4—C8—H8	117.5
H5A—O5—H5B	103 (2)	N1—C9—C10	111.3 (2)
Zn1—O6—H6A	125 (2)	N1—C9—H9A	109.4
Zn1—O6—H6B	116 (3)	C10—C9—H9A	109.4
H6A—O6—H6B	110 (3)	N1—C9—H9B	109.4
Zn1—O7—H7A	122 (2)	C10—C9—H9B	109.4
Zn1—O7—H7B	114 (2)	H9A—C9—H9B	108.0
H7A—O7—H7B	109 (2)	O3—C10—O4	124.5 (3)
H8A—O8—H8B	126 (5)	O3—C10—C9	118.7 (2)
N1—C1—C2	125.9 (3)	O4—C10—C9	116.8 (2)
N1—C1—H1	117.0

Hydrogen-bond geometry (Å, º)

D—H···A	D—H	H···A	D···A	D—H···A
O8—H8B···O7	0.85 (2)	1.99 (2)	2.838 (4)	175 (6)
O7—H7B···O4^i	0.84 (2)	1.92 (2)	2.754 (3)	178 (3)
O5—H5A···O8^ii	0.87 (2)	1.85 (2)	2.675 (4)	159 (4)
O5—H5B···O1^iii	0.84 (2)	1.91 (2)	2.740 (3)	169 (4)
O6—H6A···O4^iv	0.83 (2)	1.85 (2)	2.669 (3)	170 (3)
O6—H6B···O4^v	0.83 (2)	2.22 (3)	2.977 (3)	152 (3)
O7—H7A···O3^iv	0.83 (2)	1.93 (2)	2.748 (3)	171 (3)

Symmetry codes: (i) −x+3/2, y+1/2, z; (ii) x, y−1, z; (iii) −x+1/2, y−1/2, z; (iv) −x+1, y+1/2, −z+1/2; (v) x−1/2, y, −z+1/2.