Crystal structure of silver [(propane-1,3-diyl­dinitrilo-κ²N,N′)­tetra­acetato-κ⁴O,O′,O′′,O′′′]chromate(III) from synchrotron X-ray data

In the title complex, the Cr³⁺ ion is coordinated by the four O and two N atoms of the 1,3-pdta ligand, displaying a distorted octa­hedral geometry. The Ag⁺ cation is surrounded by six O atoms from neighboring 1,3-pdta groups and water mol­ecules.

Key indicators

• Single-crystal synchrotron study
• T = 260 K
• Mean [sigma](C-C) = 0.003 Å
• R factor = 0.020
• wR factor = 0.051
• Data-to-parameter ratio = 19.0

checkCIF/PLATON results

No syntax errors found



Alert level C
PLAT314_ALERT_2_C Small Angle for H2O: Metal-O9       -H1O1      .      92.89 Degree
PLAT911_ALERT_3_C Missing FCF Refl Between Thmin & STh/L=    0.600         56 Report
PLAT913_ALERT_3_C Missing # of Very Strong Reflections in FCF ....         23 Note

Alert level G
ABSMU01_ALERT_1_G  Calculation of _exptl_absorpt_correction_mu
                not performed for this radiation type.
PLAT002_ALERT_2_G Number of Distance or Angle Restraints on AtSite          9 Note
PLAT004_ALERT_5_G Polymeric Structure Found with Maximum Dimension          3 Info
PLAT019_ALERT_1_G _diffrn_measured_fraction_theta_full/*_max < 1.0      0.987 Report
PLAT042_ALERT_1_G Calc. and Reported MoietyFormula Strings  Differ     Please Check
PLAT172_ALERT_4_G The CIF-Embedded .res File Contains DFIX Records          3 Report
PLAT173_ALERT_4_G The CIF-Embedded .res File Contains DANG Records          3 Report
PLAT232_ALERT_2_G Hirshfeld Test Diff (M-X) Ag1      --O6        .        6.8 s.u.
PLAT232_ALERT_2_G Hirshfeld Test Diff (M-X) Ag1      --O9        .       14.9 s.u.
PLAT232_ALERT_2_G Hirshfeld Test Diff (M-X) Ag1      --O11       .       11.6 s.u.
PLAT232_ALERT_2_G Hirshfeld Test Diff (M-X) Ag1      --O4_b      .        7.0 s.u.
PLAT232_ALERT_2_G Hirshfeld Test Diff (M-X) Ag1      --O2_d      .        6.2 s.u.
PLAT720_ALERT_4_G Number of Unusual/Non-Standard Labels ..........          6 Note
PLAT791_ALERT_4_G Model has Chirality at N2          (Chiral SPGR)          S Verify
PLAT860_ALERT_3_G Number of Least-Squares Restraints .............          9 Note
PLAT910_ALERT_3_G Missing # of FCF Reflection(s) Below Theta(Min).          1 Note
PLAT933_ALERT_2_G Number of OMIT Records in Embedded .res File ...          4 Note
PLAT978_ALERT_2_G Number C-C Bonds with Positive Residual Density.          6 Info

   0 ALERT level A = Most likely a serious problem - resolve or explain
   0 ALERT level B = A potentially serious problem, consider carefully
   3 ALERT level C = Check. Ensure it is not caused by an omission or oversight
  18 ALERT level G = General information/check it is not something unexpected

   3 ALERT type 1 CIF construction/syntax error, inconsistent or missing data
   9 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
   4 ALERT type 4 Improvement, methodology, query or suggestion
   1 ALERT type 5 Informative message, check

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Computing details

Data collection: PAL BL2D-SMDC (Shin et al., 2016); cell refinement: HKL3000sm (Otwinowski & Minor, 1997); data reduction: HKL3000sm (Otwinowski & Minor, 1997); program(s) used to solve structure: SHELXT2014 (Sheldrick, 2015a); program(s) used to refine structure: SHELXL2016 (Sheldrick, 2015b); molecular graphics: DIAMOND (Putz & Brandenburg, 2014); software used to prepare material for publication: publCIF (Westrip, 2010).

Silver [(propane-1,3-diyldinitrilo-κ²N,N')tetraacetato-κ⁴O,O',O'',O''']chromate(III)

Crystal data

Ag[Cr(C11H14N2O8)]·3H2O	Dx = 2.059 Mg m^−3
Mr = 516.16	Synchrotron radiation, λ = 0.610 Å
Orthorhombic, P212121	Cell parameters from 33074 reflections
a = 8.7800 (18) Å	θ = 0.4–33.7°
b = 11.443 (2) Å	µ = 1.25 mm^−1
c = 16.573 (3) Å	T = 260 K
V = 1665.1 (6) Å^3	Block, purple
Z = 4	0.17 × 0.13 × 0.07 mm
F(000) = 1036

Data collection

ADSC Q210 CCD area detector diffractometer	4738 reflections with I > 2σ(I)
Radiation source: PLSII 2D bending magnet	Rint = 0.041
ω scan	θmax = 25.5°, θmin = 2.1°
Absorption correction: empirical (using intensity measurements) (HKL3000sm Scalepack; Otwinowski & Minor, 1997)	h = −12→12
Tmin = 0.843, Tmax = 1.000	k = −16→16
14937 measured reflections	l = −23→23
4807 independent reflections

Refinement

Refinement on F^2	Hydrogen site location: mixed
Least-squares matrix: full	H atoms treated by a mixture of independent and constrained refinement
R[F^2 > 2σ(F^2)] = 0.020	w = 1/[σ^2(Fo^2) + (0.0272P)^2 + 0.5713P] where P = (Fo^2 + 2Fc^2)/3
wR(F^2) = 0.051	(Δ/σ)max = 0.002
S = 1.07	Δρmax = 0.41 e Å^−3
4807 reflections	Δρmin = −0.65 e Å^−3
253 parameters	Absolute structure: Flack x determined using 2027 quotients [(I^+)-(I^-)]/[(I^+)+(I^-)] (Parsons et al., 2013)
9 restraints	Absolute structure parameter: −0.008 (6)

Special details

Geometry. All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes.

Fractional atomic coordinates and isotropic or equivalent isotropic displacement parameters (Ų)

	x	y	z	Uiso*/Ueq
Cr1	0.24189 (3)	0.37102 (2)	0.24502 (2)	0.00967 (6)
O1	0.12226 (18)	0.25175 (12)	0.30121 (9)	0.0175 (3)
O2	−0.0055 (2)	0.21547 (15)	0.41423 (11)	0.0251 (3)
O3	0.08051 (18)	0.39909 (14)	0.16628 (9)	0.0186 (3)
O4	−0.16003 (19)	0.45764 (18)	0.15293 (11)	0.0282 (4)
O5	0.40372 (17)	0.35453 (13)	0.32531 (9)	0.0177 (3)
O6	0.63816 (19)	0.40881 (18)	0.35973 (11)	0.0286 (4)
O7	0.35275 (18)	0.27005 (12)	0.16811 (9)	0.0184 (3)
O8	0.5114 (3)	0.27410 (18)	0.06396 (14)	0.0398 (5)
N1	0.11336 (19)	0.48076 (14)	0.31737 (10)	0.0116 (3)
N2	0.38257 (19)	0.50019 (14)	0.19855 (11)	0.0132 (3)
C1	0.0637 (2)	0.28284 (17)	0.36905 (12)	0.0150 (3)
C2	0.0876 (2)	0.41046 (17)	0.39202 (12)	0.0165 (3)
H21	−0.001299	0.439533	0.420408	0.020*
H22	0.174899	0.417403	0.427556	0.020*
C3	−0.0428 (2)	0.45009 (19)	0.19226 (12)	0.0163 (3)
C4	−0.0348 (2)	0.50289 (17)	0.27589 (13)	0.0155 (3)
H41	−0.050662	0.586572	0.271860	0.019*
H42	−0.116537	0.470866	0.308456	0.019*
C5	0.5249 (2)	0.41833 (17)	0.31713 (12)	0.0159 (3)
C6	0.5206 (2)	0.50999 (17)	0.25100 (15)	0.0177 (3)
H61	0.522708	0.587001	0.275442	0.021*
H62	0.611006	0.502164	0.217770	0.021*
C7	0.4341 (3)	0.32390 (19)	0.11558 (13)	0.0192 (4)
C8	0.4251 (3)	0.45637 (18)	0.11673 (13)	0.0204 (4)
H81	0.522910	0.488802	0.101292	0.024*
H82	0.349954	0.482279	0.077731	0.024*
C9	0.1955 (2)	0.59037 (17)	0.33877 (13)	0.0183 (4)
H91	0.286801	0.569504	0.368393	0.022*
H92	0.131325	0.635424	0.374865	0.022*
C10	0.2416 (3)	0.66904 (17)	0.26797 (15)	0.0214 (4)
H10	0.153858	0.716501	0.254216	0.026*
H10B	0.319794	0.721905	0.287443	0.026*
C11	0.3006 (2)	0.61414 (17)	0.18957 (14)	0.0189 (4)
H11	0.214770	0.602452	0.153619	0.023*
H11B	0.368853	0.669379	0.163804	0.023*
Ag1	0.66176 (2)	0.43997 (2)	0.51158 (2)	0.02983 (6)
O9	0.4276 (2)	0.55599 (18)	0.50044 (10)	0.0323 (4)
H1O1	0.426 (5)	0.571 (3)	0.5503 (8)	0.039*
H2O1	0.455 (4)	0.6206 (19)	0.4800 (19)	0.039*
O10	0.8668 (3)	0.31407 (19)	0.54800 (12)	0.0345 (4)
H1O2	0.869 (5)	0.264 (3)	0.5862 (15)	0.041*
H2O2	0.899 (4)	0.276 (3)	0.5075 (14)	0.041*
O11	0.8203 (3)	0.60117 (17)	0.44997 (13)	0.0333 (4)
H1O3	0.758 (4)	0.637 (3)	0.421 (2)	0.040*
H2O3	0.853 (4)	0.649 (3)	0.4838 (18)	0.040*

Atomic displacement parameters (Ų)

	U^11	U^22	U^33	U^12	U^13	U^23
Cr1	0.00884 (12)	0.01014 (11)	0.01002 (11)	−0.00089 (9)	0.00008 (9)	0.00054 (9)
O1	0.0211 (7)	0.0136 (6)	0.0177 (6)	−0.0061 (5)	0.0050 (5)	−0.0013 (5)
O2	0.0265 (8)	0.0234 (7)	0.0253 (8)	−0.0017 (6)	0.0088 (7)	0.0093 (6)
O3	0.0137 (6)	0.0295 (7)	0.0127 (6)	0.0031 (5)	−0.0030 (5)	−0.0026 (5)
O4	0.0137 (6)	0.0496 (10)	0.0212 (7)	0.0015 (7)	−0.0065 (6)	0.0017 (7)
O5	0.0133 (6)	0.0219 (7)	0.0180 (6)	−0.0021 (5)	−0.0042 (5)	0.0052 (5)
O6	0.0154 (7)	0.0474 (10)	0.0230 (8)	−0.0030 (6)	−0.0080 (6)	0.0007 (7)
O7	0.0211 (7)	0.0143 (6)	0.0199 (7)	0.0007 (5)	0.0072 (6)	−0.0012 (5)
O8	0.0520 (13)	0.0286 (9)	0.0388 (11)	−0.0050 (9)	0.0299 (10)	−0.0106 (8)
N1	0.0116 (6)	0.0113 (6)	0.0119 (6)	−0.0005 (5)	−0.0009 (5)	−0.0003 (5)
N2	0.0117 (7)	0.0118 (7)	0.0160 (7)	−0.0009 (5)	0.0001 (5)	0.0022 (5)
C1	0.0140 (8)	0.0163 (8)	0.0147 (8)	−0.0005 (6)	0.0008 (6)	0.0039 (6)
C2	0.0206 (9)	0.0182 (8)	0.0108 (7)	0.0008 (7)	0.0019 (7)	0.0011 (6)
C3	0.0114 (8)	0.0233 (8)	0.0144 (8)	−0.0021 (7)	−0.0017 (6)	0.0044 (7)
C4	0.0110 (7)	0.0192 (9)	0.0163 (8)	0.0017 (6)	−0.0018 (6)	0.0003 (6)
C5	0.0110 (7)	0.0210 (8)	0.0157 (8)	−0.0002 (6)	−0.0018 (6)	−0.0034 (7)
C6	0.0108 (7)	0.0167 (7)	0.0258 (9)	−0.0031 (6)	−0.0016 (7)	0.0007 (7)
C7	0.0201 (9)	0.0205 (8)	0.0169 (9)	−0.0021 (7)	0.0049 (7)	−0.0025 (7)
C8	0.0253 (10)	0.0191 (9)	0.0167 (8)	−0.0036 (7)	0.0074 (8)	0.0019 (7)
C9	0.0203 (9)	0.0147 (7)	0.0200 (9)	−0.0028 (6)	−0.0008 (7)	−0.0056 (6)
C10	0.0201 (9)	0.0121 (7)	0.0319 (10)	−0.0014 (7)	0.0024 (8)	0.0002 (7)
C11	0.0215 (9)	0.0121 (8)	0.0230 (9)	0.0017 (6)	0.0009 (7)	0.0052 (7)
Ag1	0.03046 (10)	0.03290 (9)	0.02614 (9)	0.00309 (7)	0.00069 (7)	0.00446 (7)
O9	0.0440 (10)	0.0339 (8)	0.0191 (8)	−0.0016 (8)	−0.0045 (7)	0.0039 (7)
O10	0.0401 (11)	0.0378 (10)	0.0257 (9)	0.0108 (8)	0.0103 (8)	0.0094 (7)
O11	0.0376 (10)	0.0302 (8)	0.0320 (9)	0.0014 (8)	−0.0099 (8)	−0.0045 (7)

Geometric parameters (Å, º)

Cr1—O3	1.9530 (15)	C4—H41	0.9700
Cr1—O5	1.9558 (15)	C4—H42	0.9700
Cr1—O1	1.9578 (14)	C5—C6	1.517 (3)
Cr1—O7	1.9766 (15)	C6—H61	0.9700
Cr1—N1	2.0708 (17)	C6—H62	0.9700
Cr1—N2	2.0745 (16)	C7—C8	1.518 (3)
O1—C1	1.287 (2)	C8—H81	0.9700
O2—C1	1.234 (2)	C8—H82	0.9700
O3—C3	1.303 (2)	C9—C10	1.533 (3)
O4—C3	1.222 (2)	C9—H91	0.9700
O5—C5	1.298 (2)	C9—H92	0.9700
O6—C5	1.224 (3)	C10—C11	1.533 (3)
O6—Ag1	2.5501 (19)	C10—H10	0.9700
O7—C7	1.284 (3)	C10—H10B	0.9700
O8—C7	1.232 (3)	C11—H11	0.9700
N1—C9	1.490 (2)	C11—H11B	0.9700
N1—C4	1.493 (2)	Ag1—O10	2.383 (2)
N1—C2	1.493 (2)	Ag1—O9	2.455 (2)
N2—C8	1.493 (3)	Ag1—O11	2.526 (2)
N2—C6	1.496 (3)	O9—H1O1	0.844 (13)
N2—C11	1.497 (3)	O9—H2O1	0.848 (13)
C1—C2	1.524 (3)	O10—H1O2	0.854 (13)
C2—H21	0.9700	O10—H2O2	0.847 (13)
C2—H22	0.9700	O11—H1O3	0.839 (13)
C3—C4	1.514 (3)	O11—H2O3	0.834 (13)
O3—Cr1—O5	176.04 (7)	O6—C5—C6	119.87 (19)
O3—Cr1—O1	92.48 (7)	O5—C5—C6	116.36 (17)
O5—Cr1—O1	89.94 (7)	N2—C6—C5	112.83 (16)
O3—Cr1—O7	91.29 (7)	N2—C6—H61	109.0
O5—Cr1—O7	91.41 (7)	C5—C6—H61	109.0
O1—Cr1—O7	99.41 (6)	N2—C6—H62	109.0
O3—Cr1—N1	83.79 (7)	C5—C6—H62	109.0
O5—Cr1—N1	93.47 (7)	H61—C6—H62	107.8
O1—Cr1—N1	81.66 (6)	O8—C7—O7	123.7 (2)
O7—Cr1—N1	175.01 (7)	O8—C7—C8	120.0 (2)
O3—Cr1—N2	93.82 (7)	O7—C7—C8	116.21 (18)
O5—Cr1—N2	83.61 (7)	N2—C8—C7	111.09 (16)
O1—Cr1—N2	173.07 (7)	N2—C8—H81	109.4
O7—Cr1—N2	83.33 (7)	C7—C8—H81	109.4
N1—Cr1—N2	96.16 (7)	N2—C8—H82	109.4
C1—O1—Cr1	115.94 (12)	C7—C8—H82	109.4
C3—O3—Cr1	117.10 (13)	H81—C8—H82	108.0
C5—O5—Cr1	118.06 (13)	N1—C9—C10	116.11 (17)
C5—O6—Ag1	128.51 (15)	N1—C9—H91	108.3
C7—O7—Cr1	115.52 (13)	C10—C9—H91	108.3
C9—N1—C4	112.86 (15)	N1—C9—H92	108.3
C9—N1—C2	109.26 (16)	C10—C9—H92	108.3
C4—N1—C2	109.93 (16)	H91—C9—H92	107.4
C9—N1—Cr1	112.63 (12)	C11—C10—C9	119.81 (16)
C4—N1—Cr1	108.12 (12)	C11—C10—H10	107.4
C2—N1—Cr1	103.64 (11)	C9—C10—H10	107.4
C8—N2—C6	110.51 (16)	C11—C10—H10B	107.4
C8—N2—C11	108.81 (16)	C9—C10—H10B	107.4
C6—N2—C11	112.46 (16)	H10—C10—H10B	106.9
C8—N2—Cr1	104.29 (12)	N2—C11—C10	115.79 (17)
C6—N2—Cr1	108.67 (12)	N2—C11—H11	108.3
C11—N2—Cr1	111.80 (12)	C10—C11—H11	108.3
O2—C1—O1	123.65 (19)	N2—C11—H11B	108.3
O2—C1—C2	120.98 (19)	C10—C11—H11B	108.3
O1—C1—C2	115.36 (16)	H11—C11—H11B	107.4
N1—C2—C1	109.28 (15)	O10—Ag1—O9	168.15 (6)
N1—C2—H21	109.8	O10—Ag1—O11	97.34 (7)
C1—C2—H21	109.8	O9—Ag1—O11	92.08 (7)
N1—C2—H22	109.8	O10—Ag1—O6	103.11 (7)
C1—C2—H22	109.8	O9—Ag1—O6	86.18 (6)
H21—C2—H22	108.3	O11—Ag1—O6	75.40 (6)
O4—C3—O3	123.7 (2)	Ag1—O9—H1O1	93 (3)
O4—C3—C4	119.96 (19)	Ag1—O9—H2O1	105 (3)
O3—C3—C4	116.29 (16)	H1O1—O9—H2O1	103 (3)
N1—C4—C3	113.23 (15)	Ag1—O10—H1O2	128 (3)
N1—C4—H41	108.9	Ag1—O10—H2O2	111 (3)
C3—C4—H41	108.9	H1O2—O10—H2O2	104 (3)
N1—C4—H42	108.9	Ag1—O11—H1O3	103 (3)
C3—C4—H42	108.9	Ag1—O11—H2O3	113 (3)
H41—C4—H42	107.7	H1O3—O11—H2O3	107 (3)
O6—C5—O5	123.8 (2)
Cr1—O1—C1—O2	−174.74 (17)	C11—N2—C6—C5	129.15 (18)
Cr1—O1—C1—C2	4.1 (2)	Cr1—N2—C6—C5	4.8 (2)
C9—N1—C2—C1	−157.68 (16)	O6—C5—C6—N2	173.04 (19)
C4—N1—C2—C1	77.96 (19)	O5—C5—C6—N2	−7.8 (3)
Cr1—N1—C2—C1	−37.41 (17)	Cr1—O7—C7—O8	179.2 (2)
O2—C1—C2—N1	−156.79 (19)	Cr1—O7—C7—C8	−3.9 (3)
O1—C1—C2—N1	24.3 (2)	C6—N2—C8—C7	84.3 (2)
Cr1—O3—C3—O4	−168.99 (18)	C11—N2—C8—C7	−151.72 (18)
Cr1—O3—C3—C4	11.7 (2)	Cr1—N2—C8—C7	−32.3 (2)
C9—N1—C4—C3	120.00 (18)	O8—C7—C8—N2	−157.0 (2)
C2—N1—C4—C3	−117.75 (18)	O7—C7—C8—N2	25.9 (3)
Cr1—N1—C4—C3	−5.26 (18)	C4—N1—C9—C10	−61.7 (2)
O4—C3—C4—N1	177.0 (2)	C2—N1—C9—C10	175.70 (17)
O3—C3—C4—N1	−3.6 (2)	Cr1—N1—C9—C10	61.1 (2)
Ag1—O6—C5—O5	−62.2 (3)	N1—C9—C10—C11	−39.4 (3)
Ag1—O6—C5—C6	117.0 (2)	C8—N2—C11—C10	177.20 (17)
Cr1—O5—C5—O6	−173.92 (17)	C6—N2—C11—C10	−60.0 (2)
Cr1—O5—C5—C6	6.9 (2)	Cr1—N2—C11—C10	62.6 (2)
C8—N2—C6—C5	−109.04 (19)	C9—C10—C11—N2	−30.0 (3)

Hydrogen-bond geometry (Å, º)

D—H···A	D—H	H···A	D···A	D—H···A
O9—H1O1···O3^i	0.84 (1)	1.95 (1)	2.797 (2)	178 (3)
O9—H2O1···O8^ii	0.85 (1)	1.93 (1)	2.767 (3)	172 (4)
O10—H1O2···O5^iii	0.85 (1)	2.02 (1)	2.870 (2)	173 (4)
O10—H2O2···O2^iv	0.85 (1)	1.89 (1)	2.729 (3)	170 (4)
O11—H1O3···O7^ii	0.84 (1)	2.33 (2)	3.142 (3)	163 (4)
O11—H2O3···O8^v	0.83 (1)	1.99 (2)	2.791 (3)	161 (3)

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