Tris(ethyl­enediamine-κ²N,N′)cadmium(II) dinitrate

The title compound, [Cd(C₂H₈N₂)₃](NO₃)₂, crystallizes with distorted Cd(en)₃²⁺ octa­hedra. Extensive hydrogen bonding is present between the ethyl­enediamine and nitrate groups.

Key indicators

• Single-crystal synchrotron study
• T = 150 K
• Mean [sigma](C-C) = 0.005 Å
• Disorder in main residue
• R factor = 0.049
• wR factor = 0.118
• Data-to-parameter ratio = 24.2

checkCIF/PLATON results

No syntax errors found



Alert level B
ABSTM02_ALERT_3_B  The ratio of expected to reported Tmax/Tmin(RR') is < 0.75
            Tmin and Tmax reported:      0.647     1.000
            Tmin(prime) and Tmax expected:      0.979     0.989
            RR(prime) =      0.654
            Please check that your absorption correction is appropriate.

Alert level C
PLAT041_ALERT_1_C Calc. and Rep. SumFormula Strings    Differ ....          ?
PLAT042_ALERT_1_C Calc. and Rep. MoietyFormula Strings Differ ....          ?
PLAT128_ALERT_4_C Non-standard setting of Space group C2/c    ....    I2/a
PLAT301_ALERT_3_C Main Residue  Disorder .........................      14.00 Perc.

Alert level G
  ABSMU_01  Radiation type not identified. Calculation of
            _exptl_absorpt_correction_mu not performed.
CELLZ01_ALERT_1_G Difference between formula and atom_site contents detected.
CELLZ01_ALERT_1_G ALERT: check formula stoichiometry or atom site occupancies.
           From the CIF: _cell_formula_units_Z    8
           From the CIF: _chemical_formula_sum  C6 H24 Cd N8 O6
           TEST: Compare cell contents of formula and atom_site data

           atom    Z*formula  cif sites diff
           C         48.00     48.00    0.00
           H        192.00    192.00    0.00
           Cd         8.00      8.00    0.00
           N         64.00     64.02   -0.02
           O         48.00     48.07   -0.07

   0 ALERT level A = In general: serious problem
   1 ALERT level B = Potentially serious problem
   4 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
   2 ALERT type 3 Indicator that the structure quality may be low
   1 ALERT type 4 Improvement, methodology, query or suggestion


checkCIF publication errors

Alert level A
PUBL022_ALERT_1_A There is a mismatched ~ on line 128
              The title compound, [Cd(C~2~H~8~N~2)~3~](NO~3~)~2~, crystallises with distorted
              If you require a ~ then it should be escaped
              with a \, i.e. \~
              Otherwise there must be a matching closing ~, e.g. C~2~H~4~

   1 ALERT level A = Data missing that is essential or data in wrong format
   0 ALERT level G = General alerts. Data that may be required is missing

---

Computing details

Data collection: APEXII (Bruker, 2004); cell refinement: APEXII; data reduction: APEXII; program(s) used to solve structure: SHELXS97 (Sheldrick, 1997); program(s) used to refine structure: SHELXL97 (Sheldrick, 1997); molecular graphics: WinGX (Version 1.64; Farrugia, 1999); software used to prepare material for publication: SHELXL97.

Tris(ethylenediamine-κ²N,N')cadmium(II) dinitrate

Crystal data

[Cd(C2H8N2)3](NO3)2	F(000) = 1696
Mr = 416.73	Dx = 1.715 Mg m^−3
Monoclinic, I2/a	Synchrotron radiation, λ = 0.67110 Å
Hall symbol: -I 2ya	Cell parameters from 2733 reflections
a = 15.2574 (12) Å	θ = 2.9–23.0°
b = 11.0441 (8) Å	µ = 1.39 mm^−1
c = 19.155 (2) Å	T = 150 K
β = 90.246 (1)°	Block, colourless
V = 3227.6 (5) Å^3	0.02 × 0.01 × 0.01 mm
Z = 8

Data collection

Bruker D8 diffractometer	5813 independent reflections
Radiation source: Daresbury SRS, Station 9.8	4525 reflections with I > 2σ(I)
Silicon 111 monochromator	Rint = 0.076
ω rotation with narrow frame scans	θmax = 31.1°, θmin = 2.0°
Absorption correction: multi-scan (SADABS; Bruker, 2004)	h = −22→23
Tmin = 0.647, Tmax = 1.00	k = −16→16
20814 measured reflections	l = −29→28

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)] = 0.050	Hydrogen site location: inferred from neighbouring sites
wR(F^2) = 0.118	H atoms treated by a mixture of independent and constrained refinement
S = 1.07	w = 1/[σ^2(Fo^2) + (0.0288P)^2 + 0.6151P] where P = (Fo^2 + 2Fc^2)/3
5813 reflections	(Δ/σ)max = 0.001
240 parameters	Δρmax = 1.03 e Å^−3
27 restraints	Δρmin = −0.69 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	Occ. (<1)
Cd1	0.442462 (15)	0.23521 (2)	0.129797 (11)	0.02619 (8)
N1	0.5590 (2)	0.3111 (3)	0.06172 (18)	0.0370 (7)
N2	0.5730 (2)	0.1975 (3)	0.19676 (17)	0.0349 (6)
N3	0.3995 (2)	0.4060 (3)	0.19550 (14)	0.0304 (6)
N4	0.33449 (18)	0.3296 (2)	0.06123 (14)	0.0267 (5)
N5	0.3585 (2)	0.1068 (3)	0.20132 (15)	0.0311 (6)
N6	0.4291 (2)	0.0502 (3)	0.06669 (15)	0.0337 (6)
C2	0.6452 (3)	0.2678 (3)	0.1657 (2)	0.0437 (10)
H2A	0.7009	0.2366	0.1825	0.052*
H2B	0.6406	0.3518	0.1800	0.052*
C1	0.6422 (3)	0.2600 (3)	0.0876 (2)	0.0420 (9)
H1A	0.6910	0.3045	0.0680	0.050*
H1B	0.6471	0.1761	0.0732	0.050*
C3	0.3177 (2)	0.4542 (3)	0.16578 (17)	0.0342 (7)
H3A	0.3087	0.5363	0.1823	0.041*
H3B	0.2687	0.4053	0.1813	0.041*
C4	0.3208 (2)	0.4540 (3)	0.08681 (17)	0.0317 (7)
H4A	0.2662	0.4857	0.0682	0.038*
H4B	0.3682	0.5056	0.0710	0.038*
C5	0.3646 (2)	−0.0180 (3)	0.17641 (19)	0.0384 (8)
H5A	0.3175	−0.0656	0.1963	0.046*
H5B	0.4198	−0.0529	0.1915	0.046*
C6	0.3586 (2)	−0.0220 (3)	0.09748 (19)	0.0384 (8)
H6A	0.3631	−0.1052	0.0816	0.046*
H6B	0.3023	0.0095	0.0824	0.046*
N20	0.0311 (5)	0.3791 (7)	0.1174 (3)	0.0309 (9)*	0.477 (8)
O20	−0.0252 (4)	0.2931 (6)	0.1166 (5)	0.0418 (7)*	0.477 (8)
O21	0.0435 (5)	0.4291 (8)	0.1724 (4)	0.0418 (7)*	0.477 (8)
O22	0.0550 (5)	0.4171 (8)	0.0609 (4)	0.0418 (7)*	0.477 (8)
N20B	0.0159 (5)	0.3553 (6)	0.1143 (3)	0.0309 (9)*	0.331 (6)
O20B	−0.0219 (6)	0.2656 (7)	0.0867 (6)	0.0418 (7)*	0.331 (6)
O21B	0.0136 (6)	0.3783 (9)	0.1762 (4)	0.0418 (7)*	0.331 (6)
O22B	0.0724 (6)	0.4106 (10)	0.0732 (5)	0.0418 (7)*	0.331 (6)
N20C	0.0159 (5)	0.3553 (6)	0.1143 (3)	0.0309 (9)*	0.195 (7)
O20C	−0.0367 (10)	0.3012 (14)	0.1498 (10)	0.0418 (7)*	0.195 (7)
O21C	0.0640 (11)	0.4458 (16)	0.1619 (9)	0.0418 (7)*	0.195 (7)
O22C	0.0388 (11)	0.3729 (16)	0.0589 (8)	0.0418 (7)*	0.195 (7)
O10	0.17031 (18)	0.1547 (2)	0.05793 (12)	0.0404 (6)
O11	0.17461 (16)	0.1930 (2)	0.16849 (12)	0.0330 (5)
O12	0.09792 (18)	0.0432 (2)	0.12984 (14)	0.0456 (7)
N10	0.14703 (17)	0.1306 (2)	0.11827 (13)	0.0247 (5)
H2C	0.564 (3)	0.218 (4)	0.2379 (12)	0.042 (12)*
H1D	0.557 (2)	0.3877 (17)	0.0653 (18)	0.026 (9)*
H4D	0.2885 (17)	0.286 (3)	0.062 (2)	0.028 (10)*
H5C	0.3063 (14)	0.130 (3)	0.200 (2)	0.040 (11)*
H4C	0.353 (2)	0.329 (3)	0.0198 (11)	0.031 (10)*
H2D	0.584 (2)	0.1221 (18)	0.1935 (19)	0.037 (11)*
H1C	0.548 (3)	0.291 (4)	0.0189 (12)	0.054 (14)*
H6D	0.420 (3)	0.067 (4)	0.0234 (11)	0.048 (12)*
H6C	0.4763 (17)	0.011 (3)	0.0670 (19)	0.039 (11)*
H5D	0.382 (3)	0.116 (4)	0.2401 (13)	0.044 (12)*
H3C	0.4376 (18)	0.462 (2)	0.1950 (18)	0.027 (9)*
H3D	0.398 (3)	0.395 (4)	0.2386 (10)	0.055 (13)*

Atomic displacement parameters (Ų)

	U^11	U^22	U^33	U^12	U^13	U^23
Cd1	0.02701 (13)	0.03150 (13)	0.02006 (12)	0.00162 (8)	0.00162 (9)	0.00239 (7)
N1	0.0351 (16)	0.0348 (16)	0.0413 (18)	0.0020 (13)	0.0124 (14)	0.0086 (14)
N2	0.0404 (17)	0.0319 (15)	0.0323 (16)	0.0044 (13)	−0.0076 (13)	−0.0013 (12)
N3	0.0405 (16)	0.0345 (15)	0.0162 (12)	−0.0058 (12)	0.0033 (11)	−0.0048 (10)
N4	0.0278 (13)	0.0306 (14)	0.0217 (12)	0.0023 (11)	−0.0022 (10)	−0.0015 (10)
N5	0.0295 (15)	0.0383 (15)	0.0254 (14)	−0.0033 (12)	0.0017 (12)	0.0039 (11)
N6	0.0396 (17)	0.0371 (15)	0.0244 (14)	0.0153 (13)	−0.0035 (12)	−0.0055 (11)
C2	0.0306 (19)	0.040 (2)	0.061 (3)	0.0014 (15)	−0.0097 (18)	−0.0065 (17)
C1	0.0331 (19)	0.0345 (19)	0.058 (3)	−0.0006 (14)	0.0100 (18)	−0.0022 (16)
C3	0.0379 (18)	0.0331 (17)	0.0318 (17)	0.0048 (14)	0.0050 (14)	−0.0084 (13)
C4	0.0351 (17)	0.0306 (16)	0.0293 (16)	0.0048 (13)	−0.0035 (13)	−0.0012 (12)
C5	0.041 (2)	0.0319 (17)	0.042 (2)	−0.0007 (15)	−0.0039 (16)	0.0075 (15)
C6	0.044 (2)	0.0280 (16)	0.043 (2)	0.0029 (14)	−0.0110 (16)	−0.0068 (14)
O10	0.0489 (16)	0.0518 (16)	0.0205 (11)	−0.0044 (12)	0.0014 (10)	0.0049 (10)
O11	0.0342 (13)	0.0391 (13)	0.0256 (11)	−0.0047 (10)	−0.0014 (9)	−0.0069 (10)
O12	0.0501 (16)	0.0372 (14)	0.0495 (16)	−0.0209 (12)	−0.0042 (13)	0.0067 (12)
N10	0.0266 (13)	0.0250 (12)	0.0224 (12)	−0.0002 (10)	−0.0020 (10)	0.0034 (9)

Geometric parameters (Å, º)

Cd1—N1	2.364 (3)	C2—C1	1.499 (6)
Cd1—N2	2.400 (3)	C2—H2A	0.9700
Cd1—N3	2.362 (3)	C2—H2B	0.9700
Cd1—N4	2.347 (3)	C1—H1A	0.9700
Cd1—N5	2.355 (3)	C1—H1B	0.9700
Cd1—N6	2.382 (3)	C3—C4	1.514 (5)
N1—C1	1.473 (5)	C3—H3A	0.9700
N1—H1D	0.849 (18)	C3—H3B	0.9700
N1—H1C	0.863 (19)	C4—H4A	0.9700
N2—C2	1.476 (5)	C4—H4B	0.9700
N2—H2C	0.832 (19)	C5—C6	1.515 (5)
N2—H2D	0.851 (18)	C5—H5A	0.9700
N3—C3	1.469 (5)	C5—H5B	0.9700
N3—H3C	0.849 (18)	C6—H6A	0.9700
N3—H3D	0.835 (19)	C6—H6B	0.9700
N4—C4	1.474 (4)	N20—O21	1.205 (8)
N4—H4D	0.851 (18)	N20—O22	1.217 (8)
N4—H4C	0.842 (18)	N20—O20	1.280 (8)
N5—C5	1.461 (5)	N20B—O21B	1.213 (8)
N5—H5C	0.836 (18)	N20B—O20B	1.261 (9)
N5—H5D	0.831 (18)	N20B—O22B	1.319 (10)
N6—C6	1.466 (5)	O10—N10	1.240 (3)
N6—H6D	0.861 (18)	O11—N10	1.255 (3)
N6—H6C	0.839 (18)	O12—N10	1.243 (3)
N4—Cd1—N5	102.16 (10)	C6—N6—H6C	110 (3)
N1—Cd1—N2	74.45 (12)	Cd1—N6—H6C	112 (3)
N3—Cd1—N4	75.38 (10)	H6D—N6—H6C	105 (3)
N5—Cd1—N6	74.52 (11)	N2—C2—C1	110.6 (3)
N5—Cd1—N3	91.03 (10)	N2—C2—H2A	109.5
N4—Cd1—N1	93.54 (11)	C1—C2—H2A	109.5
N5—Cd1—N1	161.31 (11)	N2—C2—H2B	109.5
N3—Cd1—N1	102.82 (11)	C1—C2—H2B	109.5
N4—Cd1—N6	92.23 (10)	H2A—C2—H2B	108.1
N3—Cd1—N6	158.76 (11)	N1—C1—C2	109.7 (3)
N1—Cd1—N6	94.99 (12)	N1—C1—H1A	109.7
N4—Cd1—N2	162.73 (11)	C2—C1—H1A	109.7
N5—Cd1—N2	92.11 (11)	N1—C1—H1B	109.7
N3—Cd1—N2	94.91 (11)	C2—C1—H1B	109.7
N6—Cd1—N2	101.01 (10)	H1A—C1—H1B	108.2
C1—N1—Cd1	109.1 (2)	N3—C3—C4	110.9 (3)
C1—N1—H1D	113 (2)	N3—C3—H3A	109.5
Cd1—N1—H1D	107 (2)	C4—C3—H3A	109.5
C1—N1—H1C	112 (3)	N3—C3—H3B	109.5
Cd1—N1—H1C	107 (3)	C4—C3—H3B	109.5
H1D—N1—H1C	109 (4)	H3A—C3—H3B	108.0
C2—N2—Cd1	108.2 (2)	N4—C4—C3	109.8 (3)
C2—N2—H2C	111 (3)	N4—C4—H4A	109.7
Cd1—N2—H2C	109 (3)	C3—C4—H4A	109.7
C2—N2—H2D	110 (3)	N4—C4—H4B	109.7
Cd1—N2—H2D	107 (3)	C3—C4—H4B	109.7
H2C—N2—H2D	112 (4)	H4A—C4—H4B	108.2
C3—N3—Cd1	108.67 (19)	N5—C5—C6	110.5 (3)
C3—N3—H3C	108 (2)	N5—C5—H5A	109.6
Cd1—N3—H3C	113 (2)	C6—C5—H5A	109.6
C3—N3—H3D	114 (3)	N5—C5—H5B	109.6
Cd1—N3—H3D	115 (3)	C6—C5—H5B	109.6
H3C—N3—H3D	98 (4)	H5A—C5—H5B	108.1
C4—N4—Cd1	109.17 (19)	N6—C6—C5	110.1 (3)
C4—N4—H4D	114 (2)	N6—C6—H6A	109.6
Cd1—N4—H4D	109 (2)	C5—C6—H6A	109.6
C4—N4—H4C	112 (3)	N6—C6—H6B	109.6
Cd1—N4—H4C	107 (2)	C5—C6—H6B	109.6
H4D—N4—H4C	107 (3)	H6A—C6—H6B	108.1
C5—N5—Cd1	110.0 (2)	O21—N20—O22	125.0 (7)
C5—N5—H5C	110 (3)	O21—N20—O20	116.9 (7)
Cd1—N5—H5C	109 (3)	O22—N20—O20	116.6 (7)
C5—N5—H5D	112 (3)	O21B—N20B—O20B	124.0 (8)
Cd1—N5—H5D	102 (3)	O21B—N20B—O22B	120.5 (8)
H5C—N5—H5D	114 (4)	O20B—N20B—O22B	114.4 (8)
C6—N6—Cd1	108.9 (2)	O10—N10—O12	120.6 (3)
C6—N6—H6D	113 (3)	O10—N10—O11	120.0 (3)
Cd1—N6—H6D	109 (3)	O12—N10—O11	119.4 (3)

Hydrogen-bond geometry (Å, º)

D—H···A	D—H	H···A	D···A	D—H···A
N4—H4D···O10	0.85 (2)	2.31 (2)	3.163 (4)	175 (3)
N5—H5C···O11	0.84 (2)	2.21 (2)	3.026 (4)	166 (4)
N4—H4C···O10^i	0.84 (2)	2.46 (3)	2.991 (3)	122 (3)
N6—H6D···O10^i	0.86 (2)	2.29 (3)	3.050 (4)	148 (4)
N2—H2D···O12^ii	0.85 (2)	2.21 (2)	2.976 (4)	150 (3)
N6—H6C···O12^ii	0.84 (2)	2.29 (3)	3.022 (4)	146 (4)
N3—H3D···O11^iii	0.84 (2)	2.31 (3)	3.047 (4)	147 (4)

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