Bis[hexa-amminecobalt(III)] penta-chloride nitrate.

The title compound, [Co(NH(3))(6)](2)Cl(5)(NO(3)), was obtained under hydro-thermal conditions. The asymmetric unit contains three Co(3+) ions, one lying on an inversion center and the other two located at 2/m positions. All Co(3+) ions are six-coordinated by NH(3) mol-ecules, forming [Co(NH(3))(6)](3+) octahedra, with Co-N distances in the range 1.945 (4)-1.967 (3) Å. The nitrate N atom and one of the O atoms lie at a mirror plane. Among the Cl(-) anions, one lies in a general position, one on a twofold axis and two on a mirror plane. N-H⋯O and N-H⋯Cl hydrogen bonds link the cations and anions into a three-dimensional network.

Related literature

For metal phosphates and germanates prepared using metal complexes as templates, see: Wang et al. (2003 ▶); Pan et al. (2005 ▶, 2008 ▶). For our continued research inter­est focused on the synthesis of microporous open-framework metal-organic hybride materials by introducing transition metal complexes as templates, see: Pan et al. (2010 ▶, 2011 ▶); Tong & Pan (2011 ▶); Liang et al. (2011 ▶). For a structure containing a [Co(NH3)6]3+ cation, see: Han et al. (2012 ▶).

Experimental

Crystal data

pan class="Chemical">[Co(NH3)6]2Cl5(pan class="Gene">NO3)

M = 561.53

Monoclinic,

a = 21.118 (4) Å

b = 14.985 (3) Å

c = 6.8491 (11) Å

β = 92.147 (3)°

V = 2165.8 (6) Å3

Z = 4

Mo Kα radiation

μ = 2.18 mm−1

T = 296 K

0.20 × 0.12 × 0.10 mm

Data collection

Bruker APEXII CCD area-detector diffractometer

Absorption correction: multi-scan (SADABS; Bruker, 2005 ▶) T min = 0.738, T max = 0.770

7927 measured reflections

2813 independent reflections

1870 reflections with I > 2σ(I)

R int = 0.046

Refinement

R[F 2 > 2σ(F 2)] = 0.050

wR(F 2) = 0.140

S = 1.02

2813 reflections

119 parameters

H-atom parameters constrained

Δρmax = 0.65 e Å−3

Δρmin = −0.71 e Å−3

Data collection: pan class="Gene">APEX2 (Bruker, 2005 ▶); cell refinement: SAINT (Bruker, 2005 ▶); data reduction: SAINT; program(s) used to solve structure: SHELXS97 (Sheldrick, 2008 ▶); program(s) used to refine structure: SHELXL97 (Sheldrick, 2008 ▶); molecular graphics: SHELXTL (Sheldrick, 2008 ▶); software used to prepare material for publication: SHELXTL.

Crystal structure: contains datablock(s) I, global. DOI: 10.1107/S1600536812021332/yk2056sup1.cif

Structure factors: contains datablock(s) I. DOI: 10.1107/S1600536812021332/yk2056Isup2.hkl

Additional supplementary materials: crystallographic information; 3D view; checkCIF report

[Co(NH3)6]2Cl5(NO3)	F(000) = 1160
Mr = 561.53	Dx = 1.722 Mg m−3
Monoclinic, C2/m	Mo Kα radiation, λ = 0.71073 Å
Hall symbol: -C 2y	Cell parameters from 7927 reflections
a = 21.118 (4) Å	θ = 1.7–28.4°
b = 14.985 (3) Å	µ = 2.18 mm−1
c = 6.8491 (11) Å	T = 296 K
β = 92.147 (3)°	Rod, yellow
V = 2165.8 (6) Å3	0.2 × 0.12 × 0.10 mm
Z = 4

Bruker APEXII CCD area-detector diffractometer	2813 independent reflections
Radiation source: fine-focus sealed tube	1870 reflections with I > 2σ(I)
Graphite monochromator	Rint = 0.046
Detector resolution: 83.66 pixels mm-1	θmax = 28.4°, θmin = 1.7°
φ and ω scans	h = −27→28
Absorption correction: multi-scan (SADABS; Bruker, 2005)	k = −19→20
Tmin = 0.738, Tmax = 0.770	l = −6→9
7927 measured reflections

Refinement on F2	Primary atom site location: structure-invariant direct methods
Least-squares matrix: full	Secondary atom site location: difference Fourier map
R[F2 > 2σ(F2)] = 0.050	Hydrogen site location: inferred from neighbouring sites
wR(F2) = 0.140	H-atom parameters constrained
S = 1.02	w = 1/[σ2(Fo2) + (0.0641P)2 + 4.8344P] where P = (Fo2 + 2Fc2)/3
2813 reflections	(Δ/σ)max < 0.001
119 parameters	Δρmax = 0.65 e Å−3
0 restraints	Δρmin = −0.71 e Å−3

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

	x	y	z	Uiso*/Ueq
Co1	0.2500	0.2500	0.5000	0.0193 (2)
N7	0.25395 (17)	0.3197 (3)	0.7422 (5)	0.0329 (9)
H7A	0.2923	0.3440	0.7585	0.040*
H7B	0.2465	0.2842	0.8429	0.040*
H7C	0.2249	0.3627	0.7353	0.040*
N6	0.16170 (16)	0.2158 (3)	0.5415 (5)	0.0342 (9)
H6A	0.1477	0.1812	0.4434	0.041*
H6B	0.1378	0.2646	0.5463	0.041*
H6C	0.1596	0.1861	0.6535	0.041*
N5	0.27844 (19)	0.1439 (3)	0.6414 (6)	0.0401 (10)
H5A	0.2811	0.0984	0.5585	0.048*
H5B	0.2509	0.1306	0.7323	0.048*
H5C	0.3164	0.1541	0.6982	0.048*
Co2	0.5000	0.5000	0.0000	0.0212 (3)
Cl4	0.66930 (8)	0.5000	0.4229 (2)	0.0350 (4)
N4	0.55640 (18)	0.5926 (3)	0.1076 (6)	0.0411 (10)
H4A	0.5852	0.6062	0.0208	0.049*
H4B	0.5758	0.5727	0.2168	0.049*
H4C	0.5339	0.6410	0.1341	0.049*
N3	0.4522 (2)	0.5000	0.2394 (7)	0.0329 (12)
H3A	0.4278	0.4517	0.2435	0.040*
H3B	0.4787	0.5000	0.3435	0.040*
Co3	0.0000	0.5000	0.0000	0.0208 (3)
N2	−0.0927 (2)	0.5000	−0.0085 (7)	0.0289 (11)
H2A	−0.1072	0.4517	−0.0712	0.035*
H2B	−0.1075	0.5000	0.1114	0.035*
N1	0.00050 (17)	0.5934 (3)	0.2019 (5)	0.0330 (9)
H1A	0.0403	0.6075	0.2360	0.040*
H1B	−0.0191	0.5734	0.3061	0.040*
H1C	−0.0195	0.6415	0.1551	0.040*
Cl3	0.12244 (5)	0.28432 (8)	0.00154 (16)	0.0351 (3)
Cl2	0.0000	0.19040 (14)	0.5000	0.0485 (5)
Cl1	0.11173 (8)	0.5000	0.5167 (2)	0.0459 (5)
O2	0.68054 (15)	0.5722 (2)	0.9173 (5)	0.0392 (8)
N8	0.7099 (2)	0.5000	0.9396 (7)	0.0291 (11)
O1	0.7671 (2)	0.5000	0.9832 (8)	0.0507 (14)

	U11	U22	U33	U12	U13	U23
Co1	0.0190 (4)	0.0185 (4)	0.0206 (4)	0.0001 (3)	0.0021 (3)	0.0002 (3)
N7	0.032 (2)	0.039 (2)	0.028 (2)	−0.0044 (17)	0.0031 (15)	−0.0072 (15)
N6	0.0265 (19)	0.036 (2)	0.041 (2)	−0.0052 (17)	0.0084 (16)	−0.0079 (18)
N5	0.046 (2)	0.032 (2)	0.042 (2)	0.0034 (19)	−0.0037 (18)	0.0093 (17)
Co2	0.0179 (5)	0.0211 (6)	0.0247 (6)	0.000	0.0025 (4)	0.000
Cl4	0.0419 (9)	0.0284 (8)	0.0347 (9)	0.000	−0.0006 (7)	0.000
N4	0.033 (2)	0.044 (3)	0.047 (2)	−0.0102 (19)	0.0093 (18)	−0.0124 (19)
N3	0.027 (3)	0.043 (3)	0.028 (3)	0.000	0.005 (2)	0.000
Co3	0.0165 (5)	0.0220 (6)	0.0239 (6)	0.000	0.0019 (4)	0.000
N2	0.017 (2)	0.029 (3)	0.040 (3)	0.000	−0.001 (2)	0.000
N1	0.030 (2)	0.035 (2)	0.034 (2)	0.0027 (17)	−0.0011 (16)	−0.0044 (16)
Cl3	0.0334 (6)	0.0315 (6)	0.0405 (7)	0.0048 (5)	0.0037 (5)	0.0012 (5)
Cl2	0.0462 (10)	0.0521 (12)	0.0478 (11)	0.000	0.0079 (8)	0.000
Cl1	0.0361 (9)	0.0683 (13)	0.0337 (9)	0.000	0.0056 (7)	0.000
O2	0.0395 (19)	0.036 (2)	0.043 (2)	0.0092 (15)	0.0046 (15)	−0.0019 (14)
N8	0.024 (3)	0.037 (3)	0.027 (3)	0.000	0.004 (2)	0.000
O1	0.022 (2)	0.053 (4)	0.077 (4)	0.000	−0.005 (2)	0.000

Co1—N5i	1.945 (4)	Co2—N3ii	1.958 (5)
Co1—N5	1.945 (4)	N4—H4A	0.8900
Co1—N7	1.960 (3)	N4—H4B	0.8900
Co1—N7i	1.960 (3)	N4—H4C	0.8900
Co1—N6	1.965 (3)	N3—H3A	0.8900
Co1—N6i	1.965 (3)	N3—H3B	0.8900
N7—H7A	0.8900	Co3—N2	1.956 (5)
N7—H7B	0.8900	Co3—N2v	1.956 (5)
N7—H7C	0.8900	Co3—N1	1.967 (3)
N6—H6A	0.8900	Co3—N1vi	1.967 (3)
N6—H6B	0.8900	Co3—N1v	1.967 (3)
N6—H6C	0.8900	Co3—N1iv	1.967 (3)
N5—H5A	0.8900	N2—H2A	0.8900
N5—H5B	0.8900	N2—H2B	0.8900
N5—H5C	0.8900	N1—H1A	0.8900
Co2—N4	1.955 (4)	N1—H1B	0.8900
Co2—N4ii	1.955 (4)	N1—H1C	0.8900
Co2—N4iii	1.955 (4)	O2—N8	1.253 (4)
Co2—N4iv	1.955 (4)	N8—O1	1.234 (6)
Co2—N3	1.958 (5)	N8—O2iv	1.253 (4)
N5i—Co1—N5	180.000 (1)	N4iv—Co2—N3	90.59 (16)
N5i—Co1—N7	89.33 (16)	N4—Co2—N3ii	89.41 (16)
N5—Co1—N7	90.67 (16)	N4ii—Co2—N3ii	90.59 (16)
N5i—Co1—N7i	90.67 (16)	N4iii—Co2—N3ii	90.59 (16)
N5—Co1—N7i	89.33 (16)	N4iv—Co2—N3ii	89.41 (16)
N7—Co1—N7i	180.0	N3—Co2—N3ii	180.000 (1)
N5i—Co1—N6	90.47 (17)	Co2—N4—H4A	109.5
N5—Co1—N6	89.53 (17)	Co2—N4—H4B	109.5
N7—Co1—N6	91.56 (15)	H4A—N4—H4B	109.5
N7i—Co1—N6	88.44 (15)	Co2—N4—H4C	109.5
N5i—Co1—N6i	89.53 (17)	H4A—N4—H4C	109.5
N5—Co1—N6i	90.47 (17)	H4B—N4—H4C	109.5
N7—Co1—N6i	88.44 (15)	Co2—N3—H3A	110.1
N7i—Co1—N6i	91.56 (15)	Co2—N3—H3B	110.0
N6—Co1—N6i	180.00 (6)	H3A—N3—H3B	108.9
Co1—N7—H7A	109.5	N2—Co3—N2v	180.0
Co1—N7—H7B	109.5	N2—Co3—N1	90.00 (15)
H7A—N7—H7B	109.5	N2v—Co3—N1	90.00 (15)
Co1—N7—H7C	109.5	N2—Co3—N1vi	90.00 (15)
H7A—N7—H7C	109.5	N2v—Co3—N1vi	90.00 (15)
H7B—N7—H7C	109.5	N1—Co3—N1vi	89.3 (2)
Co1—N6—H6A	109.5	N2—Co3—N1v	90.00 (15)
Co1—N6—H6B	109.5	N2v—Co3—N1v	90.00 (15)
H6A—N6—H6B	109.5	N1—Co3—N1v	180.0 (2)
Co1—N6—H6C	109.5	N1vi—Co3—N1v	90.7 (2)
H6A—N6—H6C	109.5	N2—Co3—N1iv	90.00 (15)
H6B—N6—H6C	109.5	N2v—Co3—N1iv	90.00 (15)
Co1—N5—H5A	109.5	N1—Co3—N1iv	90.7 (2)
Co1—N5—H5B	109.5	N1vi—Co3—N1iv	180.00 (16)
H5A—N5—H5B	109.5	N1v—Co3—N1iv	89.3 (2)
Co1—N5—H5C	109.5	Co3—N2—H2A	109.9
H5A—N5—H5C	109.5	Co3—N2—H2B	111.0
H5B—N5—H5C	109.5	H2A—N2—H2B	108.6
N4—Co2—N4ii	180.0	Co3—N1—H1A	109.5
N4—Co2—N4iii	89.6 (3)	Co3—N1—H1B	109.5
N4ii—Co2—N4iii	90.4 (3)	H1A—N1—H1B	109.5
N4—Co2—N4iv	90.4 (3)	Co3—N1—H1C	109.5
N4ii—Co2—N4iv	89.6 (3)	H1A—N1—H1C	109.5
N4iii—Co2—N4iv	180.00 (17)	H1B—N1—H1C	109.5
N4—Co2—N3	90.59 (16)	O1—N8—O2iv	120.3 (3)
N4ii—Co2—N3	89.41 (16)	O1—N8—O2	120.3 (3)
N4iii—Co2—N3	89.41 (16)	O2iv—N8—O2	119.4 (5)

D—H···A	D—H	H···A	D···A	D—H···A
N1—H1A···Cl1	0.89	2.89	3.427 (4)	120
N1—H1A···Cl3iv	0.89	2.90	3.484 (4)	125
N1—H1B···Cl1vii	0.89	2.59	3.410 (4)	154
N1—H1C···Cl3v	0.89	2.63	3.431 (4)	150
N3—H3A···O2viii	0.89	2.53	3.155 (6)	128
N4—H4A···Cl3ix	0.89	2.79	3.287 (4)	117
N4—H4B···Cl4	0.89	2.62	3.448 (5)	155
N4—H4C···Cl2ix	0.89	2.73	3.321 (4)	125
N5—H5A···Cl1i	0.89	2.77	3.375 (4)	127
N5—H5A···Cl4x	0.89	2.91	3.456 (4)	122
N5—H5B···O2x	0.89	2.17	3.048 (5)	168
N5—H5C···Cl3i	0.89	2.56	3.337 (4)	146
N6—H6A···Cl4x	0.89	2.76	3.339 (4)	124
N6—H6C···Cl3xi	0.89	2.93	3.445 (4)	118
N7—H7A···Cl4viii	0.89	2.78	3.368 (4)	125
N7—H7B···Cl3xi	0.89	2.87	3.394 (4)	119

Table 1

Hydrogen-bond geometry (Å, °)

D—H⋯A	D—H	H⋯A	D⋯A	D—H⋯A
N1—H1A⋯Cl1	0.89	2.89	3.427 (4)	120
N1—H1A⋯Cl3i	0.89	2.90	3.484 (4)	125
N1—H1B⋯Cl1ii	0.89	2.59	3.410 (4)	154
N1—H1C⋯Cl3iii	0.89	2.63	3.431 (4)	150
N3—H3A⋯O2iv	0.89	2.53	3.155 (6)	128
N4—H4A⋯Cl3v	0.89	2.79	3.287 (4)	117
N4—H4B⋯Cl4	0.89	2.62	3.448 (5)	155
N4—H4C⋯Cl2v	0.89	2.73	3.321 (4)	125
N5—H5A⋯Cl1vi	0.89	2.77	3.375 (4)	127
N5—H5A⋯Cl4vii	0.89	2.91	3.456 (4)	122
N5—H5B⋯O2vii	0.89	2.17	3.048 (5)	168
N5—H5C⋯Cl3vi	0.89	2.56	3.337 (4)	146
N6—H6A⋯Cl4vii	0.89	2.76	3.339 (4)	124
N6—H6C⋯Cl3viii	0.89	2.93	3.445 (4)	118
N7—H7A⋯Cl4iv	0.89	2.78	3.368 (4)	125
N7—H7B⋯Cl3viii	0.89	2.87	3.394 (4)	119

Symmetry codes: (i) ; (ii) ; (iii) ; (iv) ; (v) ; (vi) ; (vii) ; (viii) .