Bis(1,10-phenanthroline-κ²N,N′)(sulfato-κ²O,O′)cadmium(II) 1,2-ethanediol solvate

In the structure of the title compound, [Cd(SO₄)(C₁₂H₈N₂)₂]·C₂H₆O₂, the [Cd(SO₄)(C₁₂H₈N₂)₂] and C₂H₆O₂ entities are connected by hydrogen bonding. The formula unit lies on a special position of site symmetry 2. The Cd^II centre is coordinated by four N atoms from two chelating 1,10-phenanthroline ligands and two O atoms from the bidentate sulfate ligand in a distorted octa­hedral geometry. The two chelating NCCN groups subtend a dihedral angle of 74.50 (9)°.

Key indicators

• Single-crystal X-ray study
• T = 293 K
• Mean [sigma](C-C) = 0.005 Å
• R factor = 0.031
• wR factor = 0.077
• Data-to-parameter ratio = 17.9

checkCIF/PLATON results

No syntax errors found



Alert level B
PLAT232_ALERT_2_B Hirshfeld Test Diff (M-X)  Cd1    -   O1      ..      16.50 su

Alert level C
PLAT125_ALERT_4_C No _symmetry_space_group_name_Hall Given .......          ?
PLAT199_ALERT_1_C Check the Reported _cell_measurement_temperature        293 K
PLAT200_ALERT_1_C Check the Reported _diffrn_ambient_temperature .        293 K
PLAT241_ALERT_2_C Check High      Ueq as Compared to Neighbors for         O1
PLAT242_ALERT_2_C Check Low       Ueq as Compared to Neighbors for         S1

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

   2 ALERT type 1 CIF construction/syntax error, inconsistent or missing data
   3 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
   1 ALERT type 4 Improvement, methodology, query or suggestion

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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, 1997); program(s) used to refine structure: SHELXL97 (Sheldrick, 1997); molecular graphics: SHELXTL (Bruker, 1998); software used to prepare material for publication: SHELXTL.

Bis(1,10-phenanthroline-κ²N,N')(sulfato- κ²O,O')cadmium(II) 1,2-ethanediol solvate

Crystal data

[Cd(SO4)(C12H8N2)2]·C2H6O2	F(000) = 1272
Mr = 630.94	Dx = 1.682 Mg m^−3
Monoclinic, C2/c	Mo Kα radiation, λ = 0.71073 Å
a = 18.022 (2) Å	Cell parameters from 3452 reflections
b = 12.1978 (14) Å	θ = 3.2–27.5°
c = 13.2366 (15) Å	µ = 1.01 mm^−1
β = 121.115 (2)°	T = 293 K
V = 2491.2 (5) Å^3	Block, pale-yellow
Z = 4	0.35 × 0.29 × 0.20 mm

Data collection

Bruker SMART CCD 1K area-detector diffractometer	3101 independent reflections
Radiation source: fine-focus sealed tube	2710 reflections with I > 2σ(I)
Graphite monochromator	Rint = 0.031
φ and ω scans	θmax = 28.3°, θmin = 2.1°
Absorption correction: multi-scan (SADABS; Sheldrick, 1996)	h = −24→12
Tmin = 0.719, Tmax = 0.823	k = −16→16
8598 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)] = 0.031	Hydrogen site location: inferred from neighbouring sites
wR(F^2) = 0.077	H-atom parameters constrained
S = 1.09	w = 1/[σ^2(Fo^2) + (0.0348P)^2 + 1.3354P] where P = (Fo^2 + 2Fc^2)/3
3101 reflections	(Δ/σ)max = 0.001
173 parameters	Δρmax = 0.49 e Å^−3
12 restraints	Δρmin = −0.35 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
Cd1	0.5000	0.68715 (2)	0.2500	0.03350 (10)
S1	0.5000	0.44572 (6)	0.2500	0.02955 (17)
N2	0.60679 (14)	0.80245 (15)	0.39265 (19)	0.0347 (5)
O2	0.57667 (12)	0.37764 (16)	0.29145 (18)	0.0476 (5)
O1	0.48849 (13)	0.51948 (16)	0.15375 (16)	0.0482 (5)
C4	0.72996 (17)	0.82525 (19)	0.2418 (2)	0.0359 (5)
C11	0.66922 (16)	0.83380 (18)	0.3707 (2)	0.0305 (5)
N1	0.59864 (14)	0.72769 (17)	0.19176 (19)	0.0356 (4)
C1	0.59493 (19)	0.6901 (2)	0.0950 (3)	0.0433 (6)
H1A	0.5496	0.6437	0.0455	0.052*
C12	0.66481 (16)	0.79502 (18)	0.2644 (2)	0.0313 (5)
C7	0.73898 (17)	0.90134 (19)	0.4483 (2)	0.0360 (5)
C6	0.80368 (18)	0.9301 (2)	0.4218 (2)	0.0431 (6)
H6A	0.8495	0.9748	0.4736	0.052*
C10	0.6118 (2)	0.8378 (2)	0.4911 (2)	0.0430 (6)
H10A	0.5688	0.8170	0.5062	0.052*
C3	0.7235 (2)	0.7837 (2)	0.1379 (3)	0.0451 (6)
H3A	0.7653	0.8017	0.1195	0.054*
C5	0.79974 (18)	0.8935 (2)	0.3228 (2)	0.0445 (6)
H5A	0.8428	0.9131	0.3074	0.053*
C8	0.7417 (2)	0.9363 (2)	0.5518 (2)	0.0449 (6)
H8A	0.7866	0.9810	0.6057	0.054*
C2	0.6561 (2)	0.7172 (2)	0.0646 (3)	0.0489 (7)
H2B	0.6509	0.6904	−0.0045	0.059*
C9	0.6788 (2)	0.9048 (2)	0.5726 (2)	0.0483 (7)
H9A	0.6803	0.9276	0.6407	0.058*
O3	0.5490 (2)	0.1707 (2)	0.1850 (3)	0.0854 (9)
H3	0.5469	0.2299	0.2128	0.128*
C13	0.5394 (4)	0.0875 (3)	0.2471 (5)	0.0972 (14)
H13A	0.5887	0.0894	0.3272	0.117*
H13B	0.5419	0.0185	0.2125	0.117*

Atomic displacement parameters (Ų)

	U^11	U^22	U^33	U^12	U^13	U^23
Cd1	0.03050 (15)	0.03271 (14)	0.04268 (16)	0.000	0.02275 (12)	0.000
S1	0.0248 (4)	0.0307 (4)	0.0319 (4)	0.000	0.0138 (3)	0.000
N2	0.0369 (12)	0.0342 (11)	0.0384 (11)	−0.0013 (9)	0.0233 (10)	−0.0006 (8)
O2	0.0368 (11)	0.0480 (11)	0.0610 (12)	0.0110 (8)	0.0274 (10)	0.0081 (9)
O1	0.0569 (13)	0.0443 (10)	0.0405 (10)	−0.0012 (9)	0.0231 (10)	0.0085 (8)
C4	0.0335 (13)	0.0369 (13)	0.0416 (13)	0.0025 (10)	0.0225 (11)	0.0090 (10)
C11	0.0316 (12)	0.0272 (11)	0.0336 (11)	0.0030 (9)	0.0176 (10)	0.0049 (9)
N1	0.0338 (11)	0.0382 (11)	0.0403 (11)	−0.0037 (9)	0.0231 (10)	−0.0045 (9)
C1	0.0431 (16)	0.0474 (15)	0.0453 (15)	−0.0064 (12)	0.0270 (13)	−0.0110 (12)
C12	0.0302 (12)	0.0306 (11)	0.0348 (12)	0.0014 (9)	0.0181 (11)	0.0031 (9)
C7	0.0360 (14)	0.0313 (11)	0.0345 (12)	0.0013 (10)	0.0137 (11)	0.0039 (10)
C6	0.0327 (14)	0.0400 (14)	0.0445 (14)	−0.0081 (11)	0.0114 (12)	0.0044 (11)
C10	0.0513 (17)	0.0429 (14)	0.0449 (15)	−0.0010 (12)	0.0319 (14)	−0.0011 (11)
C3	0.0474 (17)	0.0511 (15)	0.0517 (16)	−0.0027 (13)	0.0361 (15)	0.0015 (13)
C5	0.0326 (14)	0.0510 (15)	0.0508 (16)	−0.0035 (12)	0.0223 (13)	0.0093 (13)
C8	0.0470 (16)	0.0408 (14)	0.0354 (13)	−0.0034 (12)	0.0131 (13)	−0.0028 (11)
C2	0.0608 (19)	0.0523 (16)	0.0478 (16)	−0.0026 (14)	0.0380 (16)	−0.0056 (13)
C9	0.0615 (19)	0.0492 (16)	0.0361 (13)	−0.0003 (14)	0.0266 (14)	−0.0064 (12)
O3	0.119 (2)	0.0703 (16)	0.1022 (19)	0.0018 (15)	0.0820 (19)	−0.0129 (14)
C13	0.117 (3)	0.065 (2)	0.114 (3)	0.022 (2)	0.064 (3)	0.003 (2)

Geometric parameters (Å, º)

Cd1—N1^i	2.327 (2)	C1—C2	1.395 (4)
Cd1—N1	2.327 (2)	C1—H1A	0.9300
Cd1—N2	2.343 (2)	C7—C8	1.412 (4)
Cd1—N2^i	2.343 (2)	C7—C6	1.424 (4)
Cd1—O1	2.361 (2)	C6—C5	1.351 (4)
Cd1—O1^i	2.361 (2)	C6—H6A	0.9300
Cd1—S1	2.9449 (9)	C10—C9	1.394 (4)
S1—O2^i	1.4548 (19)	C10—H10A	0.9300
S1—O2	1.4548 (19)	C3—C2	1.363 (4)
S1—O1^i	1.4841 (18)	C3—H3A	0.9300
S1—O1	1.4841 (18)	C5—H5A	0.9300
N2—C10	1.331 (3)	C8—C9	1.352 (4)
N2—C11	1.354 (3)	C8—H8A	0.9300
C4—C12	1.403 (3)	C2—H2B	0.9300
C4—C3	1.413 (4)	C9—H9A	0.9300
C4—C5	1.425 (4)	O3—C13	1.372 (5)
C11—C7	1.407 (3)	O3—H3	0.8200
C11—C12	1.447 (3)	C13—C13^i	1.460 (10)
N1—C1	1.329 (3)	C13—H13A	0.9700
N1—C12	1.355 (3)	C13—H13B	0.9700
N1^i—Cd1—N1	155.47 (10)	C1—N1—C12	118.7 (2)
N1^i—Cd1—N2	93.18 (7)	C1—N1—Cd1	125.40 (18)
N1—Cd1—N2	71.91 (7)	C12—N1—Cd1	115.86 (15)
N1^i—Cd1—N2^i	71.91 (7)	N1—C1—C2	122.9 (3)
N1—Cd1—N2^i	93.18 (7)	N1—C1—H1A	118.6
N2—Cd1—N2^i	106.24 (10)	C2—C1—H1A	118.6
N1^i—Cd1—O1	119.58 (7)	N1—C12—C4	122.3 (2)
N1—Cd1—O1	82.79 (7)	N1—C12—C11	118.3 (2)
N2—Cd1—O1	139.56 (7)	C4—C12—C11	119.4 (2)
N2^i—Cd1—O1	106.17 (7)	C11—C7—C8	117.1 (2)
N1^i—Cd1—O1^i	82.79 (7)	C11—C7—C6	120.1 (2)
N1—Cd1—O1^i	119.58 (7)	C8—C7—C6	122.9 (2)
N2—Cd1—O1^i	106.17 (7)	C5—C6—C7	121.2 (2)
N2^i—Cd1—O1^i	139.56 (7)	C5—C6—H6A	119.4
O1—Cd1—O1^i	59.98 (9)	C7—C6—H6A	119.4
N1^i—Cd1—S1	102.27 (5)	N2—C10—C9	122.7 (3)
N1—Cd1—S1	102.27 (5)	N2—C10—H10A	118.6
N2—Cd1—S1	126.88 (5)	C9—C10—H10A	118.6
N2^i—Cd1—S1	126.88 (5)	C2—C3—C4	120.1 (2)
O1—Cd1—S1	29.99 (4)	C2—C3—H3A	120.0
O1^i—Cd1—S1	29.99 (4)	C4—C3—H3A	120.0
O2^i—S1—O2	110.38 (17)	C6—C5—C4	120.4 (2)
O2^i—S1—O1^i	110.73 (11)	C6—C5—H5A	119.8
O2—S1—O1^i	109.76 (11)	C4—C5—H5A	119.8
O2^i—S1—O1	109.76 (11)	C9—C8—C7	120.0 (3)
O2—S1—O1	110.73 (11)	C9—C8—H8A	120.0
O1^i—S1—O1	105.37 (16)	C7—C8—H8A	120.0
O2^i—S1—Cd1	124.81 (8)	C3—C2—C1	118.8 (3)
O2—S1—Cd1	124.81 (8)	C3—C2—H2B	120.6
O1^i—S1—Cd1	52.68 (8)	C1—C2—H2B	120.6
O1—S1—Cd1	52.68 (8)	C8—C9—C10	119.4 (3)
C10—N2—C11	118.4 (2)	C8—C9—H9A	120.3
C10—N2—Cd1	126.54 (18)	C10—C9—H9A	120.3
C11—N2—Cd1	115.10 (15)	C13—O3—H3	109.5
S1—O1—Cd1	97.33 (10)	O3—C13—C13^i	117.3 (4)
C12—C4—C3	117.2 (2)	O3—C13—H13A	108.0
C12—C4—C5	120.2 (2)	C13^i—C13—H13A	108.0
C3—C4—C5	122.6 (2)	O3—C13—H13B	108.0
N2—C11—C7	122.5 (2)	C13^i—C13—H13B	108.0
N2—C11—C12	118.8 (2)	H13A—C13—H13B	107.2
C7—C11—C12	118.7 (2)
N1^i—Cd1—S1—O2^i	40.03 (11)	N1^i—Cd1—N1—C1	−126.0 (2)
N1—Cd1—S1—O2^i	−139.97 (11)	N2—Cd1—N1—C1	179.1 (2)
N2—Cd1—S1—O2^i	143.57 (11)	N2^i—Cd1—N1—C1	−74.8 (2)
N2^i—Cd1—S1—O2^i	−36.43 (11)	O1—Cd1—N1—C1	31.1 (2)
O1—Cd1—S1—O2^i	−89.30 (14)	O1^i—Cd1—N1—C1	80.4 (2)
O1^i—Cd1—S1—O2^i	90.70 (14)	S1—Cd1—N1—C1	54.0 (2)
N1^i—Cd1—S1—O2	−139.97 (11)	N1^i—Cd1—N1—C12	54.28 (16)
N1—Cd1—S1—O2	40.03 (11)	N2—Cd1—N1—C12	−0.62 (16)
N2—Cd1—S1—O2	−36.43 (11)	N2^i—Cd1—N1—C12	105.43 (17)
N2^i—Cd1—S1—O2	143.57 (11)	O1—Cd1—N1—C12	−148.66 (18)
O1—Cd1—S1—O2	90.70 (14)	O1^i—Cd1—N1—C12	−99.33 (17)
O1^i—Cd1—S1—O2	−89.30 (14)	S1—Cd1—N1—C12	−125.72 (16)
N1^i—Cd1—S1—O1^i	−50.67 (12)	C12—N1—C1—C2	−0.2 (4)
N1—Cd1—S1—O1^i	129.33 (12)	Cd1—N1—C1—C2	−180.0 (2)
N2—Cd1—S1—O1^i	52.87 (12)	C1—N1—C12—C4	−0.8 (4)
N2^i—Cd1—S1—O1^i	−127.13 (12)	Cd1—N1—C12—C4	178.95 (17)
O1—Cd1—S1—O1^i	180.0	C1—N1—C12—C11	−178.8 (2)
N1^i—Cd1—S1—O1	129.33 (12)	Cd1—N1—C12—C11	0.9 (3)
N1—Cd1—S1—O1	−50.67 (12)	C3—C4—C12—N1	0.9 (4)
N2—Cd1—S1—O1	−127.13 (12)	C5—C4—C12—N1	−178.0 (2)
N2^i—Cd1—S1—O1	52.87 (12)	C3—C4—C12—C11	178.9 (2)
O1^i—Cd1—S1—O1	180.0	C5—C4—C12—C11	0.0 (3)
N1^i—Cd1—N2—C10	20.9 (2)	N2—C11—C12—N1	−0.7 (3)
N1—Cd1—N2—C10	−179.0 (2)	C7—C11—C12—N1	178.3 (2)
N2^i—Cd1—N2—C10	93.0 (2)	N2—C11—C12—C4	−178.8 (2)
O1—Cd1—N2—C10	−125.0 (2)	C7—C11—C12—C4	0.2 (3)
O1^i—Cd1—N2—C10	−62.5 (2)	N2—C11—C7—C8	−0.2 (3)
S1—Cd1—N2—C10	−87.0 (2)	C12—C11—C7—C8	−179.2 (2)
N1^i—Cd1—N2—C11	−159.88 (16)	N2—C11—C7—C6	178.8 (2)
N1—Cd1—N2—C11	0.23 (15)	C12—C11—C7—C6	−0.2 (3)
N2^i—Cd1—N2—C11	−87.80 (16)	C11—C7—C6—C5	−0.1 (4)
O1—Cd1—N2—C11	54.3 (2)	C8—C7—C6—C5	178.9 (3)
O1^i—Cd1—N2—C11	116.71 (16)	C11—N2—C10—C9	−0.6 (4)
S1—Cd1—N2—C11	92.20 (16)	Cd1—N2—C10—C9	178.7 (2)
O2^i—S1—O1—Cd1	119.26 (10)	C12—C4—C3—C2	0.0 (4)
O2—S1—O1—Cd1	−118.62 (11)	C5—C4—C3—C2	178.9 (3)
O1^i—S1—O1—Cd1	0.0	C7—C6—C5—C4	0.3 (4)
N1^i—Cd1—O1—S1	−60.35 (12)	C12—C4—C5—C6	−0.2 (4)
N1—Cd1—O1—S1	130.37 (11)	C3—C4—C5—C6	−179.1 (3)
N2—Cd1—O1—S1	79.50 (14)	C11—C7—C8—C9	−0.1 (4)
N2^i—Cd1—O1—S1	−138.39 (9)	C6—C7—C8—C9	−179.0 (3)
O1^i—Cd1—O1—S1	0.0	C4—C3—C2—C1	−0.9 (4)
C10—N2—C11—C7	0.5 (3)	N1—C1—C2—C3	1.1 (5)
Cd1—N2—C11—C7	−178.85 (17)	C7—C8—C9—C10	0.0 (4)
C10—N2—C11—C12	179.5 (2)	N2—C10—C9—C8	0.3 (4)
Cd1—N2—C11—C12	0.2 (3)	O3—C13—C13^i—O3^i	−67.3 (9)

Symmetry code: (i) −x+1, y, −z+1/2.

Hydrogen-bond geometry (Å, º)

D—H···A	D—H	H···A	D···A	D—H···A
O3—H3···O2	0.82	2.01	2.807 (3)	164