Bis[hexa­amminecobalt(III)] penta­chloride nitrate

Wu, Q.; Du, C.; Lv, Y.; Chen, G.; Pan, Q.

doi:10.1107/S1600536812021332

inorganic compounds

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ISSN: 2056-9890

Volume 68| Part 6| June 2012| Pages i45-i46

doi:10.1107/S1600536812021332

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Bis[hexaamminecobalt(III)] pentachloride nitrate

Qihui Wu,^a Chunyu Du,^a Yang Lv,^a Guoliang Chen ^a and Qinhe Pan ^a ^*

^aDepartment of Materials and Chemical Engineering, Ministry of Education Key Laboratory of Advanced Materials of Tropical Island Resources, Hainan University, Haikou 570228, People's Republic of China
^*Correspondence e-mail: panqinhe@163.com

(Received 26 April 2012; accepted 10 May 2012; online 16 May 2012)

The title compound, [Co(NH₃)₆]₂Cl₅(NO₃), was obtained under hydrothermal conditions. The asymmetric unit contains three Co³⁺ ions, one lying on an inversion center and the other two located at 2/m positions. All Co³⁺ ions are six-coordinated by NH₃ molecules, forming [Co(NH₃)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. (2003a ,b ); 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. (2010a ,b , 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

[Co(NH₃)₆]₂Cl₅(NO₃)
M_r = 561.53
Monoclinic, C 2/m
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[F² > 2σ(F²)] = 0.050
wR(F²) = 0.140
S = 1.02
2813 reflections
119 parameters
H-atom parameters constrained
Δρ_max = 0.65 e Å⁻³
Δρ_min = −0.71 e Å⁻³

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⋯O2^iv	0.89	2.53	3.155 (6)	128
N4—H4A⋯Cl3^v	0.89	2.79	3.287 (4)	117
N4—H4B⋯Cl4	0.89	2.62	3.448 (5)	155
N4—H4C⋯Cl2^v	0.89	2.73	3.321 (4)	125
N5—H5A⋯Cl1^vi	0.89	2.77	3.375 (4)	127
N5—H5A⋯Cl4^vii	0.89	2.91	3.456 (4)	122
N5—H5B⋯O2^vii	0.89	2.17	3.048 (5)	168
N5—H5C⋯Cl3^vi	0.89	2.56	3.337 (4)	146
N6—H6A⋯Cl4^vii	0.89	2.76	3.339 (4)	124
N6—H6C⋯Cl3^viii	0.89	2.93	3.445 (4)	118
N7—H7A⋯Cl4^iv	0.89	2.78	3.368 (4)	125
N7—H7B⋯Cl3^viii	0.89	2.87	3.394 (4)	119
Symmetry codes: (i) x, -y+1, z; (ii) -x, -y+1, -z+1; (iii) -x, -y+1, -z; (iv) -x+1, -y+1, -z+1; (v) $[x+{\script{1\over 2}}, y+{\script{1\over 2}}, z]$ ; (vi) $[-x+{\script{1\over 2}}, -y+{\script{1\over 2}}, -z+1]$ ; (vii) $[x-{\script{1\over 2}}, y-{\script{1\over 2}}, z]$ ; (viii) x, y, z+1.

Data collection: 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.

Supporting information

Crystal structure: contains datablocks I, global. DOI: 10.1107/S1600536812021332/yk2056sup1.cif

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

checkCIF report

Comment top

Rencently, more attention has been paid to transition metal complexes, because they can to be employed as templates in the synthesis of various open-framework materials, including metal phosphates (Wang et al., 2003a,b) and germanates (Pan et al., 2005,2008). Our continued interest has been focused on the synthesis of microporous open-framework metal-organic hybride materials by introducing transition metal complexes as templates (Pan et al., 2010a,b, 2011; Tong & Pan, 2011; Liang et al., 2011). Unexpectedly, the title compound, [Co(NH₃)₆]₂(NO₃)Cl₅, was obtained.

The title compound is composed of [Co(NH₃)₆]³⁺ cations and the counterions Cl^- and NO₃^-, as shown in Fig. 1. The asymmetric part of this crystal structure contains three Co³⁺ ions; one is located on an inversion center, and the other two are positioned on the twofold rotation axis with center of symmetry (2/m). All Co(III) ions are six coordinated by NH₃ molecules to form [Co(NH₃)₆]³⁺ cations, having a slightly distorted octahedral geometry, as in the structure of [Co(NH₃)₆]₃[Zn₈(HPO₄)₈(PO₄)₂](PO₄) (Han et al., 2012). The Co—N bond distances are in the range from 1.945 (4) to 1.967 (3) Å. For the counterions, the N8 atom of NO₃^- anion is located on mirror plane and displays a trigonal geometry by bonded to three O atoms with the N—O distances of 1.234 (6)–1.253 (4) Å. The Cl^- anions are located in different positions: inversion center for Cl2, mirror plane for Cl1 and Cl4, and general position for Cl3. The [Co(NH₃)₆]³⁺ cations interact with the counterions Cl^- and NO₃^- via hydrogen bonds; the distances of N—H···O hydrogen bonds are in the range 3.048 (5)–3.155 (6) Å, and the distances of N—H···Cl hydrogen bonds lie in the range from 3.287 (4) to 3.484 (4) Å (Table 1), to form an extensive three-dimensional hydrogen-bonding network.

Related literature top

metal-organic hybride materials by introducing transition metal complexes as

templates, see: Pan et al. (2010a,b, 2011); Tong & Pan (2011); Liang et al. (2011). For a structure containing a [Co(NH₃)₆]³⁺ cation, see: Han et al. (2012).

Experimental top

In a typical synthesis, a mixture of Cd(NO₃)₂.4H₂O (0.231 g), pyromellitic acid (0.0254 g), [Co(NH₃)₆]Cl₃ (0.03 g), NaOH (0.016 g) and H₂O (10 ml) were added in a 20 ml Teflon-lined reactor under autogenous pressure at 100°C for 3 days. Yellow rod-like crystals were obtained.

Computing details top

Data collection: APEX2 (Bruker, 2005); cell refinement: SAINT (Bruker, 2005); data reduction: SAINT (Bruker, 2005); 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 (Sheldrick, 2008).

Figures top

Fig. 1. A view of the asymmetric unit of title compound showing the atom labelling scheme. Ellipsoids are drawn at the 30% probability level. [Symmetry codes: (i) -x, 1 - y, -z; (ii) -x, y, -z; (iii) x, 1 - y, z; (iv) 1 - x, 1 - y, -z; (v) 1 - x, y, -z; (vi) 1/2 - x, 1/2 - y, 1 - z]. (iv) x, -y + 1, z; (v) -x, -y + 1, -z; (vi) -x, y, -z.

Bis[hexaamminecobalt(III)] pentachloride nitrate top

Crystal data top

[Co(NH₃)₆]₂Cl₅(NO₃)	F(000) = 1160
M_r = 561.53	D_x = 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

Data collection top

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

Refinement top

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(F_o²) + (0.0641P)² + 4.8344P] where P = (F_o² + 2F_c²)/3
2813 reflections	(Δ/σ)_max < 0.001
119 parameters	Δρ_max = 0.65 e Å⁻³
0 restraints	Δρ_min = −0.71 e Å⁻³

Crystal data top

[Co(NH₃)₆]₂Cl₅(NO₃)	V = 2165.8 (6) Å³
M_r = 561.53	Z = 4
Monoclinic, C2/m	Mo Kα radiation
a = 21.118 (4) Å	µ = 2.18 mm⁻¹
b = 14.985 (3) Å	T = 296 K
c = 6.8491 (11) Å	0.2 × 0.12 × 0.10 mm
β = 92.147 (3)°

Data collection top

Bruker APEXII CCD area-detector diffractometer	2813 independent reflections
Absorption correction: multi-scan (SADABS; Bruker, 2005)	1870 reflections with I > 2σ(I)
T_min = 0.738, T_max = 0.770	R_int = 0.046
7927 measured reflections

Refinement top

R[F² > 2σ(F²)] = 0.050	0 restraints
wR(F²) = 0.140	H-atom parameters constrained
S = 1.02	Δρ_max = 0.65 e Å⁻³
2813 reflections	Δρ_min = −0.71 e Å⁻³
119 parameters

Special details top

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.

Fractional atomic coordinates and isotropic or equivalent isotropic displacement parameters (Å²) top

	x	y	z	U_iso*/U_eq
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)

Atomic displacement parameters (Å²) top

	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

Geometric parameters (Å, º) top

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—N2^v	1.956 (5)
N7—H7C	0.8900	Co3—N1	1.967 (3)
N6—H6A	0.8900	Co3—N1^vi	1.967 (3)
N6—H6B	0.8900	Co3—N1^v	1.967 (3)
N6—H6C	0.8900	Co3—N1^iv	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—N4^iv	1.955 (4)	N8—O1	1.234 (6)
Co2—N3	1.958 (5)	N8—O2^iv	1.253 (4)

N5ⁱ—Co1—N5	180.000 (1)	N4^iv—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)	N4^iv—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—N2^v	180.0
Co1—N7—H7B	109.5	N2—Co3—N1	90.00 (15)
H7A—N7—H7B	109.5	N2^v—Co3—N1	90.00 (15)
Co1—N7—H7C	109.5	N2—Co3—N1^vi	90.00 (15)
H7A—N7—H7C	109.5	N2^v—Co3—N1^vi	90.00 (15)
H7B—N7—H7C	109.5	N1—Co3—N1^vi	89.3 (2)
Co1—N6—H6A	109.5	N2—Co3—N1^v	90.00 (15)
Co1—N6—H6B	109.5	N2^v—Co3—N1^v	90.00 (15)
H6A—N6—H6B	109.5	N1—Co3—N1^v	180.0 (2)
Co1—N6—H6C	109.5	N1^vi—Co3—N1^v	90.7 (2)
H6A—N6—H6C	109.5	N2—Co3—N1^iv	90.00 (15)
H6B—N6—H6C	109.5	N2^v—Co3—N1^iv	90.00 (15)
Co1—N5—H5A	109.5	N1—Co3—N1^iv	90.7 (2)
Co1—N5—H5B	109.5	N1^vi—Co3—N1^iv	180.00 (16)
H5A—N5—H5B	109.5	N1^v—Co3—N1^iv	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—N4^iv	90.4 (3)	Co3—N1—H1C	109.5
N4ⁱⁱ—Co2—N4^iv	89.6 (3)	H1A—N1—H1C	109.5
N4ⁱⁱⁱ—Co2—N4^iv	180.00 (17)	H1B—N1—H1C	109.5
N4—Co2—N3	90.59 (16)	O1—N8—O2^iv	120.3 (3)
N4ⁱⁱ—Co2—N3	89.41 (16)	O1—N8—O2	120.3 (3)
N4ⁱⁱⁱ—Co2—N3	89.41 (16)	O2^iv—N8—O2	119.4 (5)

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

Hydrogen-bond geometry (Å, º) top

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···Cl3^iv	0.89	2.90	3.484 (4)	125
N1—H1B···Cl1^vii	0.89	2.59	3.410 (4)	154
N1—H1C···Cl3^v	0.89	2.63	3.431 (4)	150
N3—H3A···O2^viii	0.89	2.53	3.155 (6)	128
N4—H4A···Cl3^ix	0.89	2.79	3.287 (4)	117
N4—H4B···Cl4	0.89	2.62	3.448 (5)	155
N4—H4C···Cl2^ix	0.89	2.73	3.321 (4)	125
N5—H5A···Cl1ⁱ	0.89	2.77	3.375 (4)	127
N5—H5A···Cl4^x	0.89	2.91	3.456 (4)	122
N5—H5B···O2^x	0.89	2.17	3.048 (5)	168
N5—H5C···Cl3ⁱ	0.89	2.56	3.337 (4)	146
N6—H6A···Cl4^x	0.89	2.76	3.339 (4)	124
N6—H6C···Cl3^xi	0.89	2.93	3.445 (4)	118
N7—H7A···Cl4^viii	0.89	2.78	3.368 (4)	125
N7—H7B···Cl3^xi	0.89	2.87	3.394 (4)	119

Symmetry codes: (i) −x+1/2, −y+1/2, −z+1; (iv) x, −y+1, z; (v) −x, −y+1, −z; (vii) −x, −y+1, −z+1; (viii) −x+1, −y+1, −z+1; (ix) x+1/2, y+1/2, z; (x) x−1/2, y−1/2, z; (xi) x, y, z+1.

Experimental details

Crystal data
Chemical formula	[Co(NH₃)₆]₂Cl₅(NO₃)
M_r	561.53
Crystal system, space group	Monoclinic, C2/m
Temperature (K)	296
a, b, c (Å)	21.118 (4), 14.985 (3), 6.8491 (11)
β (°)	92.147 (3)
V (Å³)	2165.8 (6)
Z	4
Radiation type	Mo Kα
µ (mm⁻¹)	2.18
Crystal size (mm)	0.2 × 0.12 × 0.10

Data collection
Diffractometer	Bruker APEXII CCD area-detector diffractometer
Absorption correction	Multi-scan (SADABS; Bruker, 2005)
T_min, T_max	0.738, 0.770
No. of measured, independent and observed [I > 2σ(I)] reflections	7927, 2813, 1870
R_int	0.046
(sin θ/λ)_max (Å⁻¹)	0.669

Refinement
R[F² > 2σ(F²)], wR(F²), S	0.050, 0.140, 1.02
No. of reflections	2813
No. of parameters	119
H-atom treatment	H-atom parameters constrained
Δρ_max, Δρ_min (e Å⁻³)	0.65, −0.71

Computer programs: APEX2 (Bruker, 2005), SAINT (Bruker, 2005), SHELXS97 (Sheldrick, 2008), SHELXL97 (Sheldrick, 2008), SHELXTL (Sheldrick, 2008).

Hydrogen-bond geometry (Å, º) top

D—H···A	D—H	H···A	D···A	D—H···A
N1—H1A···Cl1	0.89	2.89	3.427 (4)	120.4
N1—H1A···Cl3ⁱ	0.89	2.90	3.484 (4)	124.5
N1—H1B···Cl1ⁱⁱ	0.89	2.59	3.410 (4)	154.4
N1—H1C···Cl3ⁱⁱⁱ	0.89	2.63	3.431 (4)	149.6
N3—H3A···O2^iv	0.89	2.53	3.155 (6)	128.2
N4—H4A···Cl3^v	0.89	2.79	3.287 (4)	116.9
N4—H4B···Cl4	0.89	2.62	3.448 (5)	154.8
N4—H4C···Cl2^v	0.89	2.73	3.321 (4)	124.6
N5—H5A···Cl1^vi	0.89	2.77	3.375 (4)	126.7
N5—H5A···Cl4^vii	0.89	2.91	3.456 (4)	121.6
N5—H5B···O2^vii	0.89	2.17	3.048 (5)	167.6
N5—H5C···Cl3^vi	0.89	2.56	3.337 (4)	146.2
N6—H6A···Cl4^vii	0.89	2.76	3.339 (4)	124.1
N6—H6C···Cl3^viii	0.89	2.93	3.445 (4)	118.2
N7—H7A···Cl4^iv	0.89	2.78	3.368 (4)	124.5
N7—H7B···Cl3^viii	0.89	2.87	3.394 (4)	118.8

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

Acknowledgements

This work was supported by the Program for New Century Excellent Talents in Universities (NCET-11–0929), the National Natural Science Foundation of China (No. 21101047), the Natural Science Foundation of Hainan Province (No. 211010) and the Priming Scientific Research Foundation of Hainan University (No. kyqd1051).

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