(2,2'-Bipyridine-5,5'-dicarboxylic acid)tetra­chloro­platinum(IV) monohydrate

In the mononuclear title compound, [PtCl₄(C₁₂H₈N₂O₄)]·H₂O, the Pt^IV atom is six-coordinated in octa­hedral configuration by two N atoms from the 2,2'-bipyridine-5,5'-dicarboxylic acid ligand and four terminal Cl atoms. In the crystal structure, the mol­ecules are linked together through extensive inter­molecular hydrogen bonding, forming a three-dimensional structure.

Key indicators

• Single-crystal X-ray study
• T = 298 K
• Mean [sigma](C-C) = 0.006 Å
• R factor = 0.028
• wR factor = 0.070
• Data-to-parameter ratio = 15.2

checkCIF/PLATON results

No syntax errors found



Alert level B
PLAT029_ALERT_3_B _diffrn_measured_fraction_theta_full Low .......       0.95

Alert level C
ABSTM02_ALERT_3_C  The ratio of expected to reported Tmax/Tmin(RR) is > 1.10
            Tmin and Tmax reported:      0.231     0.656
            Tmin and Tmax expected:      0.153     0.631
            RR =      1.459
            Please check that your absorption correction is appropriate.
PLAT060_ALERT_3_C Ratio Tmax/Tmin (Exp-to-Rep) (too) Large .......       1.46
PLAT062_ALERT_4_C Rescale T(min) & T(max) by .....................       0.96
PLAT152_ALERT_1_C Supplied and Calc Volume s.u. Inconsistent .....          ?
PLAT164_ALERT_4_C Nr. of Refined C-H H-Atoms in Heavy-At Struct...          6
PLAT222_ALERT_3_C Large Non-Solvent    H     Ueq(max)/Ueq(min) ...       3.68 Ratio
PLAT242_ALERT_2_C Check Low       Ueq as Compared to Neighbors for         C6

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

   1 ALERT type 1 CIF construction/syntax error, inconsistent or missing data
   1 ALERT type 2 Indicator that the structure model may be wrong or deficient
   4 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: SMART (Bruker, 1998); cell refinement: SMART; data reduction: SAINT (Bruker, 2001); program(s) used to solve structure: SHELXTL (Bruker, 2000); program(s) used to refine structure: SHELXL97 (Sheldrick, 1997); molecular graphics: SHELXTL; software used to prepare material for publication: SHELXL97.

(2,2'-Bipyridine-5,5'-dicarboxylic acid)tetrachloroplatinum(IV) monohydrate

Crystal data

[PtCl4(C12H8N2O4)]·H2O	F(000) = 1128
Mr = 599.11	Dx = 2.417 Mg m^−3
Monoclinic, P21/c	Mo Kα radiation, λ = 0.71073 Å
Hall symbol: -P 2ybc	Cell parameters from 5858 reflections
a = 15.905 (3) Å	θ = 2.7–28.3°
b = 8.9969 (18) Å	µ = 9.20 mm^−1
c = 12.512 (3) Å	T = 298 K
β = 113.12 (3)°	Cube, yellow
V = 1646.6 (6) Å^3	0.22 × 0.22 × 0.05 mm
Z = 4

Data collection

Siemens SMART CCD diffractometer	3903 independent reflections
Radiation source: fine-focus sealed tube	3318 reflections with I > 2σ(I)
Graphite monochromator	Rint = 0.049
ω scans	θmax = 28.3°, θmin = 2.7°
Absorption correction: multi-scan (SADABS; Sheldrick, 1997)	h = −20→20
Tmin = 0.231, Tmax = 0.656	k = −12→7
10397 measured reflections	l = −16→15

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)] = 0.028	Hydrogen site location: inferred from neighbouring sites
wR(F^2) = 0.070	All H-atom parameters refined
S = 1.03	w = 1/[σ^2(Fo^2) + (0.0282P)^2] where P = (Fo^2 + 2Fc^2)/3
3903 reflections	(Δ/σ)max = 0.002
257 parameters	Δρmax = 1.53 e Å^−3
0 restraints	Δρmin = −1.44 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
Pt1	0.228299 (11)	1.130034 (16)	0.114022 (12)	0.02309 (7)
Cl1	0.35974 (9)	1.15458 (13)	0.07720 (11)	0.0383 (3)
Cl2	0.28462 (9)	1.28363 (12)	0.27300 (9)	0.0382 (3)
Cl3	0.09638 (9)	1.09048 (14)	0.14705 (12)	0.0411 (3)
Cl4	0.16589 (9)	1.33482 (12)	0.00032 (10)	0.0367 (3)
C1	0.3341 (3)	0.9314 (5)	0.3188 (4)	0.0261 (9)
C2	0.3686 (3)	0.7975 (5)	0.3716 (3)	0.0270 (9)
C3	0.3487 (3)	0.6677 (5)	0.3052 (4)	0.0315 (10)
C4	0.2944 (3)	0.6775 (5)	0.1875 (4)	0.0314 (10)
C5	0.2624 (3)	0.8140 (5)	0.1384 (3)	0.0237 (9)
C6	0.4238 (3)	0.7931 (5)	0.5004 (4)	0.0328 (10)
C7	0.2063 (3)	0.8358 (5)	0.0146 (3)	0.0223 (8)
C8	0.1804 (3)	0.7229 (5)	−0.0663 (4)	0.0276 (9)
C9	0.1306 (3)	0.7566 (5)	−0.1830 (4)	0.0273 (9)
C10	0.1081 (3)	0.9025 (5)	−0.2153 (3)	0.0253 (9)
C11	0.1331 (3)	1.0142 (5)	−0.1315 (4)	0.0280 (10)
C12	0.0585 (3)	0.9454 (5)	−0.3396 (3)	0.0274 (9)
N1	0.2827 (2)	0.9386 (4)	0.2050 (3)	0.0241 (7)
N2	0.1819 (2)	0.9802 (4)	−0.0194 (3)	0.0240 (7)
O1	0.4350 (3)	0.8990 (4)	0.5604 (3)	0.0628 (13)
O2	0.4552 (4)	0.6614 (4)	0.5340 (3)	0.0615 (13)
O3	0.0162 (2)	1.0667 (3)	−0.3635 (2)	0.0340 (7)
O4	0.0627 (3)	0.8526 (4)	−0.4139 (3)	0.0405 (9)
O5W	0.5151 (3)	0.6034 (6)	0.7510 (3)	0.0546 (12)
H1	0.340 (3)	1.024 (5)	0.362 (3)	0.019 (10)*
H2	0.372 (3)	0.584 (5)	0.342 (4)	0.028 (12)*
H3	0.278 (3)	0.597 (5)	0.145 (4)	0.028 (13)*
H4	0.464 (5)	0.644 (7)	0.601 (6)	0.07 (2)*
H5	0.193 (3)	0.630 (4)	−0.035 (4)	0.027 (13)*
H6	0.112 (4)	0.673 (6)	−0.238 (4)	0.042 (14)*
H7	0.119 (3)	1.113 (4)	−0.149 (4)	0.021 (11)*
H8	0.037 (4)	0.863 (6)	−0.478 (6)	0.05 (2)*
H9	0.511 (5)	0.537 (8)	0.784 (6)	0.08 (3)*
H10	0.556 (5)	0.669 (7)	0.788 (6)	0.08 (2)*

Atomic displacement parameters (Ų)

	U^11	U^22	U^33	U^12	U^13	U^23
Pt1	0.02827 (11)	0.01843 (10)	0.02014 (10)	0.00023 (6)	0.00689 (7)	−0.00080 (5)
Cl1	0.0363 (7)	0.0421 (6)	0.0388 (6)	−0.0034 (5)	0.0172 (5)	−0.0010 (5)
Cl2	0.0536 (7)	0.0288 (5)	0.0284 (5)	−0.0046 (5)	0.0120 (5)	−0.0092 (4)
Cl3	0.0400 (7)	0.0347 (6)	0.0547 (7)	0.0023 (6)	0.0252 (6)	0.0052 (5)
Cl4	0.0479 (7)	0.0216 (5)	0.0350 (6)	0.0058 (5)	0.0103 (5)	0.0051 (4)
C1	0.027 (2)	0.025 (2)	0.022 (2)	0.0022 (18)	0.0057 (17)	−0.0005 (17)
C2	0.028 (2)	0.031 (2)	0.020 (2)	0.0024 (19)	0.0073 (17)	0.0023 (17)
C3	0.040 (3)	0.023 (2)	0.028 (2)	0.001 (2)	0.009 (2)	0.0020 (18)
C4	0.040 (3)	0.018 (2)	0.031 (2)	0.003 (2)	0.008 (2)	−0.0003 (18)
C5	0.031 (2)	0.021 (2)	0.0191 (19)	−0.0010 (18)	0.0090 (17)	0.0007 (15)
C6	0.037 (3)	0.037 (3)	0.020 (2)	0.000 (2)	0.0061 (19)	0.0040 (18)
C7	0.025 (2)	0.0232 (19)	0.0175 (19)	−0.0022 (17)	0.0071 (17)	−0.0017 (15)
C8	0.036 (3)	0.022 (2)	0.022 (2)	−0.0023 (19)	0.0086 (18)	−0.0011 (16)
C9	0.031 (2)	0.030 (2)	0.022 (2)	−0.0021 (19)	0.0105 (18)	−0.0040 (17)
C10	0.028 (2)	0.027 (2)	0.019 (2)	−0.0030 (19)	0.0076 (17)	−0.0040 (16)
C11	0.030 (2)	0.024 (2)	0.024 (2)	0.0009 (19)	0.0046 (18)	0.0034 (16)
C12	0.024 (2)	0.030 (2)	0.024 (2)	−0.0027 (19)	0.0053 (18)	−0.0027 (17)
N1	0.0316 (19)	0.0173 (16)	0.0213 (17)	0.0031 (15)	0.0079 (15)	0.0011 (13)
N2	0.0304 (19)	0.0215 (17)	0.0163 (16)	0.0008 (15)	0.0050 (14)	−0.0037 (13)
O1	0.095 (4)	0.047 (2)	0.0274 (19)	0.014 (2)	0.004 (2)	−0.0051 (16)
O2	0.093 (4)	0.041 (2)	0.025 (2)	0.013 (2)	−0.003 (2)	0.0066 (16)
O3	0.0381 (19)	0.0345 (17)	0.0259 (15)	0.0096 (15)	0.0087 (14)	0.0024 (13)
O4	0.044 (2)	0.050 (2)	0.0185 (17)	0.0133 (16)	0.0026 (16)	−0.0058 (14)
O5W	0.059 (3)	0.060 (3)	0.030 (2)	−0.020 (2)	0.002 (2)	0.0074 (19)

Geometric parameters (Å, º)

Pt1—N2	2.044 (3)	C6—O2	1.290 (6)
Pt1—N1	2.058 (3)	C7—N2	1.374 (5)
Pt1—Cl2	2.2955 (11)	C7—C8	1.378 (6)
Pt1—Cl4	2.3010 (12)	C8—C9	1.394 (6)
Pt1—Cl3	2.3196 (13)	C8—H5	0.91 (4)
Pt1—Cl1	2.3212 (14)	C9—C10	1.379 (6)
C1—N1	1.337 (5)	C9—H6	0.98 (5)
C1—C2	1.380 (6)	C10—C11	1.393 (6)
C1—H1	0.98 (4)	C10—C12	1.492 (6)
C2—C3	1.396 (6)	C11—N2	1.345 (5)
C2—C6	1.503 (5)	C11—H7	0.92 (4)
C3—C4	1.387 (6)	C12—O3	1.255 (5)
C3—H2	0.88 (5)	C12—O4	1.271 (5)
C4—C5	1.378 (6)	O2—H4	0.81 (7)
C4—H3	0.87 (5)	O4—H8	0.75 (6)
C5—N1	1.357 (5)	O5W—H9	0.75 (7)
C5—C7	1.467 (5)	O5W—H10	0.87 (7)
C6—O1	1.183 (6)
N2—Pt1—N1	80.69 (13)	O1—C6—O2	126.2 (5)
N2—Pt1—Cl2	175.75 (10)	O1—C6—C2	122.6 (5)
N1—Pt1—Cl2	95.07 (10)	O2—C6—C2	111.2 (4)
N2—Pt1—Cl4	95.36 (10)	N2—C7—C8	120.2 (4)
N1—Pt1—Cl4	175.89 (9)	N2—C7—C5	115.7 (4)
Cl2—Pt1—Cl4	88.89 (5)	C8—C7—C5	124.1 (4)
N2—Pt1—Cl3	89.00 (11)	C7—C8—C9	119.5 (4)
N1—Pt1—Cl3	89.21 (11)	C7—C8—H5	114 (3)
Cl2—Pt1—Cl3	90.60 (5)	C9—C8—H5	126 (3)
Cl4—Pt1—Cl3	91.84 (5)	C10—C9—C8	119.3 (4)
N2—Pt1—Cl1	88.01 (11)	C10—C9—H6	123 (3)
N1—Pt1—Cl1	88.50 (11)	C8—C9—H6	117 (3)
Cl2—Pt1—Cl1	92.25 (5)	C9—C10—C11	120.2 (4)
Cl4—Pt1—Cl1	90.26 (5)	C9—C10—C12	121.4 (4)
Cl3—Pt1—Cl1	176.48 (4)	C11—C10—C12	118.4 (4)
N1—C1—C2	120.9 (4)	N2—C11—C10	119.9 (4)
N1—C1—H1	116 (2)	N2—C11—H7	117 (3)
C2—C1—H1	123 (2)	C10—C11—H7	123 (3)
C1—C2—C3	119.4 (4)	O3—C12—O4	125.0 (4)
C1—C2—C6	119.4 (4)	O3—C12—C10	119.2 (4)
C3—C2—C6	121.1 (4)	O4—C12—C10	115.8 (4)
C4—C3—C2	118.7 (4)	C1—N1—C5	120.8 (4)
C4—C3—H2	125 (3)	C1—N1—Pt1	125.3 (3)
C2—C3—H2	117 (3)	C5—N1—Pt1	113.9 (3)
C5—C4—C3	119.8 (4)	C11—N2—C7	121.0 (3)
C5—C4—H3	120 (3)	C11—N2—Pt1	125.2 (3)
C3—C4—H3	121 (3)	C7—N2—Pt1	113.8 (3)
N1—C5—C4	120.4 (4)	C6—O2—H4	114 (5)
N1—C5—C7	115.9 (4)	C12—O4—H8	122 (4)
C4—C5—C7	123.7 (4)	H9—O5W—H10	117 (7)
N1—C1—C2—C3	−0.7 (7)	C2—C1—N1—Pt1	−178.9 (3)
N1—C1—C2—C6	−178.2 (4)	C4—C5—N1—C1	0.3 (7)
C1—C2—C3—C4	−0.1 (7)	C7—C5—N1—C1	−179.4 (4)
C6—C2—C3—C4	177.4 (4)	C4—C5—N1—Pt1	179.9 (4)
C2—C3—C4—C5	0.9 (8)	C7—C5—N1—Pt1	0.2 (5)
C3—C4—C5—N1	−1.0 (7)	N2—Pt1—N1—C1	178.9 (4)
C3—C4—C5—C7	178.6 (4)	Cl2—Pt1—N1—C1	−1.5 (4)
C1—C2—C6—O1	4.3 (8)	Cl3—Pt1—N1—C1	−92.0 (4)
C3—C2—C6—O1	−173.2 (5)	Cl1—Pt1—N1—C1	90.7 (4)
C1—C2—C6—O2	−176.2 (5)	N2—Pt1—N1—C5	−0.7 (3)
C3—C2—C6—O2	6.4 (7)	Cl3—Pt1—N1—C5	88.4 (3)
N1—C5—C7—N2	0.7 (6)	Cl1—Pt1—N1—C5	−88.9 (3)
C4—C5—C7—N2	−178.9 (4)	C10—C11—N2—C7	−1.1 (7)
N1—C5—C7—C8	178.8 (4)	C10—C11—N2—Pt1	177.8 (3)
C4—C5—C7—C8	−0.8 (7)	C8—C7—N2—C11	−0.5 (7)
N2—C7—C8—C9	1.1 (7)	C5—C7—N2—C11	177.7 (4)
C5—C7—C8—C9	−177.0 (4)	C8—C7—N2—Pt1	−179.5 (3)
C7—C8—C9—C10	−0.1 (7)	C5—C7—N2—Pt1	−1.3 (5)
C8—C9—C10—C11	−1.5 (7)	N1—Pt1—N2—C11	−177.9 (4)
C8—C9—C10—C12	177.2 (4)	Cl4—Pt1—N2—C11	1.0 (4)
C9—C10—C11—N2	2.1 (7)	Cl3—Pt1—N2—C11	92.8 (4)
C12—C10—C11—N2	−176.7 (4)	Cl1—Pt1—N2—C11	−89.1 (4)
C9—C10—C12—O3	159.3 (4)	N1—Pt1—N2—C7	1.1 (3)
C11—C10—C12—O3	−21.9 (6)	Cl4—Pt1—N2—C7	179.9 (3)
C9—C10—C12—O4	−20.4 (6)	Cl3—Pt1—N2—C7	−88.3 (3)
C11—C10—C12—O4	158.3 (4)	Cl1—Pt1—N2—C7	89.9 (3)
C2—C1—N1—C5	0.6 (7)

Hydrogen-bond geometry (Å, º)

D—H···A	D—H	H···A	D···A	D—H···A
O2—H4···O5W	0.81 (7)	1.76 (7)	2.553 (5)	164 (8)
O5W—H10···Cl1^i	0.87 (7)	2.32 (7)	3.157 (5)	163 (6)
O4—H8···O3^ii	0.75 (6)	1.93 (6)	2.667 (5)	167 (6)
O5W—H9···O1^iii	0.75 (7)	2.18 (7)	2.848 (6)	150 (7)

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