Synthesis and investigation of the thermal properties of [Co(NH₃)₆][Co(C₂O₄)₃]·3H₂O and [Ir(NH₃)₆][Ir(C₂O₄)₃]

The com­plexes [Co(NH₃)₆][Ir(C₂O₄)₃] and [Ir(NH₃)₆][Co(C₂O₄)₃]·H₂O have previously been synthesized and their thermal properties studied. The [Ir(NH₃)₆][Ir(C₂O₄)₃] and [Co(NH₃)₆][Co(C₂O₄)₃]·3H₂O com­plexes considered here are the end members in a series of possible isostructural solid solutions based on the com­plex salts in the Co–Ir system. Their crystal structures and thermal properties are described in detail, including tem­per­ature-dependent in situ X-ray diffraction. During the thermolysis of these com­pounds, layered metal nanoparticles are formed. Close attention is paid to the details of the [Co(NH₃)₆][Ir(C₂O₄)₃] synthesis. It has been shown that the formation of this com­plex salt is tem­per­ature dependent; upon heating, a new phase of the K₃[Co(NH₃)₆][Ir(C₂O₄)₃]₂·6H₂O salt is formed, which incorporates the initial iridium com­pound into the crystal structure of the double com­plex salt. The target [Co(NH₃)₆][Ir(C₂O₄)₃] product is obtained if the synthesis is carried out at room tem­per­ature.

Computing details

For all structures, data collection: Bruker APEX2; cell refinement: Bruker SAINT; data reduction: Bruker SAINT; program(s) used to solve structure: Bruker SHELXTL; program(s) used to refine structure: Bruker SHELXTL; molecular graphics: Bruker SHELXTL; software used to prepare material for publication: Bruker SHELXTL.

(fil002_CoNH36CoOx33H2O)

Crystal data

[Co(NH3)6]·[Co(C2O4)3]·3(H2O)	Dx = 1.909 Mg m^−3
Mr = 538.17	Mo Kα radiation, λ = 0.71073 Å
Trigonal, P3	Cell parameters from 6138 reflections
a = 12.3686 (2) Å	θ = 2.7–28.3°
c = 21.1962 (4) Å	µ = 1.86 mm^−1
V = 2808.21 (11) Å^3	T = 293 K
Z = 6	Prism, yellow
F(000) = 1656	0.20 × 0.18 × 0.16 mm

Data collection

Bruker–Nonius X8 APEX CCD area-detector diffractometer	4663 independent reflections
Graphite monochromator	3638 reflections with I > 2σ(I)
Detector resolution: 25 pixels mm^-1	Rint = 0.041
φ scans	θmax = 28.3°, θmin = 2.1°
Absorption correction: multi-scan Bruker SADABS	h = −16→16
	k = −16→16
23212 measured reflections	l = −28→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)] = 0.032	Hydrogen site location: mixed
wR(F^2) = 0.084	H atoms treated by a mixture of independent and constrained refinement
S = 1.06	w = 1/[σ^2(Fo^2) + (0.039P)^2 + 0.7848P] where P = (Fo^2 + 2Fc^2)/3
4663 reflections	(Δ/σ)max = 0.001
291 parameters	Δρmax = 0.73 e Å^−3
7 restraints	Δρmin = −0.57 e Å^−3

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
Co1	0.0000	0.0000	0.0000	0.01559 (13)
Co2	0.0000	0.0000	0.5000	0.01885 (14)
Co3	0.3333	0.6667	0.16322 (2)	0.01766 (11)
Co4	0.6667	0.3333	0.30619 (2)	0.02008 (11)
Co5	0.6667	0.3333	0.07108 (2)	0.01625 (10)
Co6	0.0000	0.0000	0.25523 (2)	0.01700 (11)
Co7	0.3333	0.6667	0.39738 (2)	0.02077 (11)
O51	0.56180 (13)	0.19305 (13)	0.01931 (6)	0.0241 (3)
O52	0.52072 (13)	0.28122 (14)	0.12157 (6)	0.0238 (3)
O53	0.36068 (15)	0.05189 (16)	0.00743 (8)	0.0421 (4)
O54	0.31525 (15)	0.15120 (18)	0.11595 (9)	0.0464 (5)
O61	0.07913 (14)	0.14613 (13)	0.20484 (6)	0.0272 (3)
O62	−0.05490 (13)	0.08837 (13)	0.30619 (6)	0.0260 (3)
O63	0.1069 (2)	0.33724 (16)	0.20321 (9)	0.0565 (5)
O64	−0.04094 (17)	0.27410 (16)	0.31225 (8)	0.0432 (4)
O71	0.32486 (14)	0.53567 (14)	0.34811 (7)	0.0296 (3)
O72	0.20664 (14)	0.54019 (14)	0.44719 (7)	0.0281 (3)
O73	0.24387 (18)	0.32935 (15)	0.35340 (8)	0.0456 (5)
O74	0.09892 (17)	0.33326 (15)	0.45471 (8)	0.0425 (4)
N1	0.07181 (16)	0.14927 (16)	0.05477 (8)	0.0244 (4)
H1A	0.1427	0.2087	0.0379	0.037*
H1B	0.0871	0.1295	0.0928	0.037*
H1C	0.0180	0.1768	0.0582	0.037*
N2	−0.09834 (18)	0.04910 (19)	0.44636 (8)	0.0297 (4)
H2A	−0.1251	0.0914	0.4693	0.045*
H2B	−0.1636	−0.0189	0.4306	0.045*
H2C	−0.0508	0.0971	0.4149	0.045*
N31	0.23835 (16)	0.51913 (16)	0.10955 (8)	0.0257 (4)
H31A	0.2184	0.4505	0.1316	0.039*
H31B	0.2846	0.5233	0.0765	0.039*
H31C	0.1690	0.5168	0.0962	0.039*
N32	0.39536 (17)	0.57982 (17)	0.21631 (8)	0.0267 (4)
H32A	0.3601	0.5662	0.2543	0.040*
H32B	0.4779	0.6266	0.2202	0.040*
H32C	0.3763	0.5072	0.1986	0.040*
N41	0.55851 (16)	0.18938 (16)	0.25260 (8)	0.0261 (4)
H41A	0.5428	0.2162	0.2167	0.039*
H41B	0.4871	0.1406	0.2726	0.039*
H41C	0.5967	0.1462	0.2442	0.039*
N42	0.52176 (18)	0.30024 (18)	0.35869 (8)	0.0323 (4)
H42A	0.5345	0.3712	0.3760	0.049*
H42B	0.5118	0.2462	0.3890	0.049*
H42C	0.4535	0.2683	0.3348	0.049*
C51	0.44631 (19)	0.1375 (2)	0.03611 (10)	0.0258 (4)
C52	0.4207 (2)	0.1913 (2)	0.09658 (10)	0.0260 (4)
C61	0.0634 (2)	0.2343 (2)	0.22654 (10)	0.0293 (5)
C62	−0.01663 (19)	0.1998 (2)	0.28676 (10)	0.0253 (4)
C71	0.2541 (2)	0.4267 (2)	0.37254 (10)	0.0280 (5)
C72	0.1795 (2)	0.4297 (2)	0.42989 (10)	0.0271 (5)
O1W	0.4478 (2)	0.4646 (2)	0.10662 (10)	0.0587 (6)
H11W	0.469 (3)	0.409 (2)	0.1287 (11)	0.070*
H12W	0.427 (3)	0.437 (3)	0.0627 (6)	0.070*
O2W	0.36005 (17)	0.30800 (19)	0.23882 (9)	0.0469 (5)
H21W	0.307 (3)	0.239 (2)	0.2134 (14)	0.084 (12)*
H22W	0.305 (2)	0.301 (3)	0.2714 (10)	0.061 (9)*
O3W	0.6144 (2)	0.5063 (2)	0.45118 (9)	0.0561 (6)
H31W	0.586 (3)	0.454 (3)	0.4873 (10)	0.086 (12)*
H32W	0.635 (3)	0.5893 (15)	0.4608 (16)	0.088 (12)*

Atomic displacement parameters (Ų)

	U^11	U^22	U^33	U^12	U^13	U^23
Co1	0.01448 (19)	0.01448 (19)	0.0178 (3)	0.00724 (9)	0.000	0.000
Co2	0.0219 (2)	0.0219 (2)	0.0128 (3)	0.01093 (11)	0.000	0.000
Co3	0.01897 (15)	0.01897 (15)	0.0150 (2)	0.00948 (8)	0.000	0.000
Co4	0.02039 (16)	0.02039 (16)	0.0195 (2)	0.01020 (8)	0.000	0.000
Co5	0.01629 (15)	0.01629 (15)	0.0162 (2)	0.00815 (7)	0.000	0.000
Co6	0.01679 (15)	0.01679 (15)	0.0174 (2)	0.00840 (7)	0.000	0.000
Co7	0.02057 (16)	0.02057 (16)	0.0212 (2)	0.01028 (8)	0.000	0.000
O51	0.0249 (8)	0.0214 (7)	0.0224 (7)	0.0090 (6)	−0.0005 (6)	−0.0029 (6)
O52	0.0220 (7)	0.0296 (8)	0.0206 (7)	0.0136 (7)	0.0025 (6)	0.0003 (6)
O53	0.0285 (9)	0.0405 (10)	0.0475 (10)	0.0099 (8)	−0.0112 (7)	−0.0145 (8)
O54	0.0233 (9)	0.0532 (12)	0.0519 (10)	0.0110 (8)	0.0083 (8)	−0.0055 (9)
O61	0.0279 (8)	0.0233 (8)	0.0271 (7)	0.0104 (7)	0.0076 (6)	0.0062 (6)
O62	0.0277 (8)	0.0264 (8)	0.0276 (7)	0.0163 (7)	0.0088 (6)	0.0015 (6)
O63	0.0793 (15)	0.0257 (9)	0.0582 (12)	0.0214 (10)	0.0122 (11)	0.0165 (8)
O64	0.0491 (11)	0.0418 (10)	0.0547 (11)	0.0347 (9)	−0.0073 (9)	−0.0144 (8)
O71	0.0355 (9)	0.0253 (8)	0.0284 (8)	0.0155 (7)	0.0073 (6)	−0.0007 (6)
O72	0.0260 (8)	0.0252 (8)	0.0298 (7)	0.0102 (7)	0.0074 (6)	−0.0001 (6)
O73	0.0605 (12)	0.0294 (9)	0.0499 (10)	0.0247 (9)	0.0062 (9)	−0.0055 (8)
O74	0.0407 (10)	0.0282 (9)	0.0460 (10)	0.0078 (8)	0.0094 (8)	0.0098 (7)
N1	0.0228 (9)	0.0211 (9)	0.0283 (9)	0.0101 (7)	−0.0029 (7)	−0.0035 (7)
N2	0.0327 (11)	0.0395 (11)	0.0220 (8)	0.0217 (9)	−0.0029 (7)	0.0014 (8)
N31	0.0254 (9)	0.0239 (9)	0.0238 (8)	0.0092 (8)	0.0026 (7)	−0.0032 (7)
N32	0.0311 (10)	0.0296 (10)	0.0228 (8)	0.0177 (8)	0.0030 (7)	0.0053 (7)
N41	0.0244 (9)	0.0243 (9)	0.0269 (9)	0.0102 (8)	−0.0019 (7)	−0.0015 (7)
N42	0.0303 (10)	0.0371 (11)	0.0305 (9)	0.0175 (9)	0.0049 (8)	0.0013 (8)
C51	0.0244 (11)	0.0241 (11)	0.0276 (10)	0.0112 (9)	−0.0048 (8)	−0.0002 (8)
C52	0.0222 (11)	0.0278 (11)	0.0275 (10)	0.0119 (9)	0.0001 (8)	0.0025 (9)
C61	0.0269 (11)	0.0217 (11)	0.0346 (11)	0.0086 (9)	−0.0027 (9)	0.0037 (9)
C62	0.0228 (10)	0.0255 (11)	0.0315 (10)	0.0150 (9)	−0.0060 (8)	−0.0043 (9)
C71	0.0323 (12)	0.0260 (11)	0.0275 (10)	0.0158 (10)	−0.0025 (9)	−0.0019 (9)
C72	0.0266 (11)	0.0244 (11)	0.0291 (10)	0.0119 (9)	−0.0013 (9)	0.0028 (9)
O1W	0.0897 (16)	0.0684 (14)	0.0479 (11)	0.0619 (14)	0.0027 (11)	0.0000 (10)
O2W	0.0277 (10)	0.0476 (12)	0.0556 (12)	0.0115 (9)	0.0020 (9)	0.0004 (9)
O3W	0.0916 (17)	0.0527 (13)	0.0405 (10)	0.0483 (13)	0.0126 (10)	0.0074 (9)

Geometric parameters (Å, º)

Co1—N1	1.9763 (16)	Co5—O52	1.9119 (14)
Co1—N1^i	1.9763 (16)	Co6—O62	1.8881 (14)
Co1—N1^ii	1.9763 (16)	Co6—O62^v	1.8881 (14)
Co1—N1^iii	1.9763 (16)	Co6—O62^iii	1.8881 (14)
Co1—N1^iv	1.9764 (16)	Co6—O61	1.8964 (14)
Co1—N1^v	1.9764 (16)	Co6—O61^iii	1.8964 (14)
Co2—N2	1.9697 (17)	Co6—O61^v	1.8964 (14)
Co2—N2^vi	1.9697 (17)	Co7—O71^ix	1.8860 (14)
Co2—N2^iii	1.9697 (17)	Co7—O71^x	1.8860 (14)
Co2—N2^vii	1.9697 (17)	Co7—O71	1.8860 (14)
Co2—N2^viii	1.9697 (17)	Co7—O72^ix	1.8883 (14)
Co2—N2^v	1.9697 (17)	Co7—O72	1.8883 (14)
Co3—N32^ix	1.9577 (17)	Co7—O72^x	1.8883 (14)
Co3—N32^x	1.9577 (17)	O51—C51	1.288 (2)
Co3—N32	1.9577 (17)	O52—C52	1.293 (2)
Co3—N31^ix	1.9648 (17)	O53—C51	1.221 (3)
Co3—N31	1.9648 (17)	O54—C52	1.212 (3)
Co3—N31^x	1.9648 (17)	O61—C61	1.285 (3)
Co4—N41^xi	1.9667 (17)	O62—C62	1.281 (2)
Co4—N41	1.9667 (17)	O63—C61	1.213 (3)
Co4—N41^xii	1.9668 (17)	O64—C62	1.226 (2)
Co4—N42^xi	1.9709 (18)	O71—C71	1.292 (3)
Co4—N42^xii	1.9709 (18)	O72—C72	1.287 (3)
Co4—N42	1.9709 (18)	O73—C71	1.216 (3)
Co5—O51	1.9096 (14)	O74—C72	1.227 (3)
Co5—O51^xi	1.9096 (14)	C51—C52	1.548 (3)
Co5—O51^xii	1.9096 (14)	C61—C62	1.539 (3)
Co5—O52^xi	1.9119 (14)	C71—C72	1.537 (3)
Co5—O52^xii	1.9119 (14)
N1—Co1—N1^i	180.0	O51^xii—Co5—O52^xi	174.48 (6)
N1—Co1—N1^ii	91.01 (7)	O51—Co5—O52^xii	174.48 (6)
N1^i—Co1—N1^ii	88.99 (7)	O51^xi—Co5—O52^xii	92.98 (6)
N1—Co1—N1^iii	88.99 (7)	O51^xii—Co5—O52^xii	85.26 (6)
N1^i—Co1—N1^iii	91.01 (7)	O52^xi—Co5—O52^xii	91.73 (6)
N1^ii—Co1—N1^iii	180.00 (11)	O51—Co5—O52	85.27 (6)
N1—Co1—N1^iv	91.01 (7)	O51^xi—Co5—O52	174.48 (6)
N1^i—Co1—N1^iv	88.99 (7)	O51^xii—Co5—O52	92.99 (6)
N1^ii—Co1—N1^iv	88.99 (7)	O52^xi—Co5—O52	91.72 (6)
N1^iii—Co1—N1^iv	91.01 (7)	O52^xii—Co5—O52	91.73 (6)
N1—Co1—N1^v	88.99 (7)	O62—Co6—O62^v	90.52 (6)
N1^i—Co1—N1^v	91.01 (7)	O62—Co6—O62^iii	90.52 (6)
N1^ii—Co1—N1^v	91.01 (7)	O62^v—Co6—O62^iii	90.52 (6)
N1^iii—Co1—N1^v	88.99 (7)	O62—Co6—O61	86.22 (6)
N1^iv—Co1—N1^v	180.00 (11)	O62^v—Co6—O61	92.01 (6)
N2—Co2—N2^vi	89.99 (7)	O62^iii—Co6—O61	175.89 (6)
N2—Co2—N2^iii	90.01 (7)	O62—Co6—O61^iii	92.01 (6)
N2^vi—Co2—N2^iii	180.00 (8)	O62^v—Co6—O61^iii	175.89 (6)
N2—Co2—N2^vii	180.0	O62^iii—Co6—O61^iii	86.22 (6)
N2^vi—Co2—N2^vii	90.01 (7)	O61—Co6—O61^iii	91.39 (6)
N2^iii—Co2—N2^vii	89.99 (7)	O62—Co6—O61^v	175.89 (6)
N2—Co2—N2^viii	89.99 (7)	O62^v—Co6—O61^v	86.22 (6)
N2^vi—Co2—N2^viii	90.01 (7)	O62^iii—Co6—O61^v	92.01 (6)
N2^iii—Co2—N2^viii	89.99 (7)	O61—Co6—O61^v	91.39 (6)
N2^vii—Co2—N2^viii	90.01 (7)	O61^iii—Co6—O61^v	91.39 (6)
N2—Co2—N2^v	90.01 (7)	O71^ix—Co7—O71^x	92.30 (6)
N2^vi—Co2—N2^v	89.99 (7)	O71^ix—Co7—O71	92.30 (6)
N2^iii—Co2—N2^v	90.01 (7)	O71^x—Co7—O71	92.30 (6)
N2^vii—Co2—N2^v	89.99 (7)	O71^ix—Co7—O72^ix	86.05 (6)
N2^viii—Co2—N2^v	180.00 (10)	O71^x—Co7—O72^ix	89.92 (7)
N32^ix—Co3—N32^x	90.26 (7)	O71—Co7—O72^ix	177.29 (6)
N32^ix—Co3—N32	90.25 (7)	O71^ix—Co7—O72	89.92 (7)
N32^x—Co3—N32	90.25 (7)	O71^x—Co7—O72	177.29 (6)
N32^ix—Co3—N31^ix	92.27 (8)	O71—Co7—O72	86.06 (6)
N32^x—Co3—N31^ix	87.73 (7)	O72^ix—Co7—O72	91.79 (6)
N32—Co3—N31^ix	176.78 (7)	O71^ix—Co7—O72^x	177.29 (6)
N32^ix—Co3—N31	87.72 (7)	O71^x—Co7—O72^x	86.05 (6)
N32^x—Co3—N31	176.78 (7)	O71—Co7—O72^x	89.92 (7)
N32—Co3—N31	92.27 (8)	O72^ix—Co7—O72^x	91.79 (6)
N31^ix—Co3—N31	89.84 (7)	O72—Co7—O72^x	91.79 (6)
N32^ix—Co3—N31^x	176.77 (7)	C51—O51—Co5	113.22 (13)
N32^x—Co3—N31^x	92.27 (8)	C52—O52—Co5	113.38 (13)
N32—Co3—N31^x	87.73 (7)	C61—O61—Co6	112.47 (13)
N31^ix—Co3—N31^x	89.84 (7)	C62—O62—Co6	113.12 (13)
N31—Co3—N31^x	89.84 (7)	C71—O71—Co7	113.05 (13)
N41^xi—Co4—N41	89.98 (7)	C72—O72—Co7	112.84 (13)
N41^xi—Co4—N41^xii	89.98 (7)	O53—C51—O51	125.1 (2)
N41—Co4—N41^xii	89.98 (7)	O53—C51—C52	120.64 (19)
N41^xi—Co4—N42^xi	90.10 (8)	O51—C51—C52	114.24 (17)
N41—Co4—N42^xi	88.67 (7)	O54—C52—O52	125.8 (2)
N41^xii—Co4—N42^xi	178.64 (8)	O54—C52—C51	120.96 (19)
N41^xi—Co4—N42^xii	88.67 (7)	O52—C52—C51	113.27 (17)
N41—Co4—N42^xii	178.64 (8)	O63—C61—O61	124.7 (2)
N41^xii—Co4—N42^xii	90.10 (8)	O63—C61—C62	121.0 (2)
N42^xi—Co4—N42^xii	91.25 (8)	O61—C61—C62	114.29 (17)
N41^xi—Co4—N42	178.64 (8)	O64—C62—O62	124.6 (2)
N41—Co4—N42	90.10 (8)	O64—C62—C61	121.5 (2)
N41^xii—Co4—N42	88.67 (7)	O62—C62—C61	113.89 (17)
N42^xi—Co4—N42	91.25 (8)	O73—C71—O71	125.4 (2)
N42^xii—Co4—N42	91.25 (8)	O73—C71—C72	121.4 (2)
O51—Co5—O51^xi	90.27 (6)	O71—C71—C72	113.17 (18)
O51—Co5—O51^xii	90.27 (6)	O74—C72—O72	124.3 (2)
O51^xi—Co5—O51^xii	90.27 (6)	O74—C72—C71	121.4 (2)
O51—Co5—O52^xi	92.98 (6)	O72—C72—C71	114.19 (18)
O51^xi—Co5—O52^xi	85.26 (6)

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

(ko123_IrNH36IrOx3)

Crystal data

[Ir(NH3)6][Ir(C2O4)4]	Z = 2
Mr = 750.66	F(000) = 692
Triclinic, P1	Dx = 3.026 Mg m^−3
a = 7.5600 (2) Å	Mo Kα radiation, λ = 0.71073 Å
b = 9.7304 (3) Å	Cell parameters from 4768 reflections
c = 11.9386 (3) Å	θ = 2.2–28.3°
α = 84.368 (1)°	µ = 16.21 mm^−1
β = 87.579 (1)°	T = 293 K
γ = 70.534 (1)°	Plate, yellow
V = 823.99 (4) Å^3	0.10 × 0.07 × 0.04 mm

Data collection

Bruker–Nonius X8 APEX CCD area-detector diffractometer	4063 independent reflections
Graphite monochromator	3532 reflections with I > 2σ(I)
Detector resolution: 25 pixels mm^-1	Rint = 0.034
φ scans	θmax = 28.3°, θmin = 1.7°
Absorption correction: multi-scan Bruker SADABS	h = −10→9
	k = −12→12
7770 measured reflections	l = −15→15

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)] = 0.022	Hydrogen site location: inferred from neighbouring sites
wR(F^2) = 0.056	H-atom parameters constrained
S = 1.01	w = 1/[σ^2(Fo^2)] where P = (Fo^2 + 2Fc^2)/3
4063 reflections	(Δ/σ)max = 0.001
240 parameters	Δρmax = 1.45 e Å^−3
0 restraints	Δρmin = −1.29 e Å^−3

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	Occ. (<1)
Ir1	0.09273 (2)	0.77320 (2)	0.26275 (2)	0.01794 (5)
Ir2	0.53618 (2)	0.24648 (2)	0.23156 (2)	0.02161 (6)
O11	0.2861 (5)	0.3030 (4)	0.1528 (3)	0.0311 (8)
O12	0.6343 (5)	0.1664 (4)	0.0801 (3)	0.0283 (8)
O13	0.1646 (5)	0.2229 (5)	0.0159 (3)	0.0395 (10)
O14	0.5240 (5)	0.1352 (5)	−0.0800 (3)	0.0395 (10)
O21	0.4276 (5)	0.3222 (4)	0.3817 (3)	0.0277 (8)
O22	0.4705 (5)	0.0665 (4)	0.2969 (3)	0.0286 (8)
O23	0.2916 (5)	0.2561 (4)	0.5359 (3)	0.0338 (9)
O24	0.3180 (5)	−0.0023 (4)	0.4421 (3)	0.0324 (8)
O31	0.5988 (5)	0.4303 (4)	0.1756 (3)	0.0294 (8)
O32	0.7924 (5)	0.1922 (4)	0.3072 (3)	0.0280 (8)
O33	0.8078 (6)	0.5377 (5)	0.2054 (4)	0.0539 (12)
O34	0.9707 (6)	0.3096 (5)	0.3658 (4)	0.0565 (13)
N1	0.0973 (7)	0.9646 (5)	0.1678 (4)	0.0476 (14)
H1A	−0.0054	1.0007	0.1259	0.071*
H1B	0.1984	0.9443	0.1232	0.071*
H1C	0.1009	1.0303	0.2138	0.071*
N2	0.0129 (6)	0.8884 (5)	0.4022 (3)	0.0271 (9)
H2A	0.1144	0.8848	0.4391	0.041*	0.5
H2B	−0.0525	0.9812	0.3808	0.041*	0.5
H2C	−0.0580	0.8492	0.4471	0.041*	0.5
H2D	−0.1118	0.9253	0.4056	0.041*	0.5
H2E	0.0551	0.8289	0.4639	0.041*	0.5
H2F	0.0606	0.9610	0.3976	0.041*	0.5
N3	0.0806 (6)	0.5871 (5)	0.3600 (4)	0.0310 (10)
H3A	0.0180	0.6129	0.4236	0.047*
H3B	0.1964	0.5279	0.3760	0.047*
H3C	0.0221	0.5410	0.3220	0.047*
N4	0.1711 (6)	0.6527 (5)	0.1226 (3)	0.0325 (10)
H4A	0.1468	0.5691	0.1360	0.049*
H4B	0.2933	0.6334	0.1091	0.049*
H4C	0.1067	0.7043	0.0630	0.049*
N5	0.3761 (6)	0.7266 (6)	0.3012 (4)	0.0360 (11)
H5A	0.4440	0.7169	0.2380	0.054*
H5B	0.4155	0.6437	0.3459	0.054*
H5C	0.3889	0.7993	0.3362	0.054*
N6	−0.1858 (5)	0.8258 (5)	0.2256 (3)	0.0267 (9)
H6A	−0.2523	0.9045	0.2597	0.040*
H6B	−0.2248	0.7511	0.2495	0.040*
H6C	−0.2010	0.8446	0.1515	0.040*
C11	0.2980 (7)	0.2357 (6)	0.0635 (4)	0.0255 (10)
C12	0.5002 (7)	0.1724 (6)	0.0155 (4)	0.0258 (10)
C21	0.3637 (6)	0.2307 (5)	0.4442 (4)	0.0233 (10)
C22	0.3825 (6)	0.0862 (6)	0.3927 (4)	0.0234 (10)
C31	0.7473 (8)	0.4361 (6)	0.2231 (4)	0.0306 (11)
C32	0.8479 (7)	0.3037 (6)	0.3063 (5)	0.0291 (11)

Atomic displacement parameters (Ų)

	U^11	U^22	U^33	U^12	U^13	U^23
Ir1	0.01602 (9)	0.01434 (10)	0.02228 (9)	−0.00286 (7)	0.00066 (7)	−0.00411 (7)
Ir2	0.02165 (11)	0.01802 (10)	0.02402 (10)	−0.00442 (8)	−0.00113 (7)	−0.00381 (7)
O11	0.0183 (17)	0.040 (2)	0.0305 (18)	−0.0016 (16)	−0.0021 (14)	−0.0085 (16)
O12	0.0232 (18)	0.033 (2)	0.0300 (17)	−0.0108 (16)	0.0040 (14)	−0.0079 (16)
O13	0.030 (2)	0.056 (3)	0.0348 (19)	−0.015 (2)	−0.0058 (16)	−0.0056 (18)
O14	0.039 (2)	0.056 (3)	0.0228 (18)	−0.013 (2)	0.0051 (16)	−0.0101 (17)
O21	0.033 (2)	0.0224 (19)	0.0272 (17)	−0.0075 (16)	0.0037 (15)	−0.0062 (14)
O22	0.035 (2)	0.0224 (19)	0.0320 (18)	−0.0129 (16)	0.0044 (15)	−0.0077 (15)
O23	0.031 (2)	0.043 (3)	0.0271 (18)	−0.0100 (19)	0.0071 (16)	−0.0120 (17)
O24	0.0270 (19)	0.033 (2)	0.042 (2)	−0.0175 (17)	0.0004 (15)	0.0014 (17)
O31	0.033 (2)	0.022 (2)	0.0351 (19)	−0.0124 (16)	−0.0056 (15)	0.0042 (15)
O32	0.0221 (18)	0.0198 (19)	0.0395 (19)	−0.0040 (15)	−0.0088 (15)	0.0024 (15)
O33	0.061 (3)	0.028 (2)	0.079 (3)	−0.025 (2)	−0.021 (2)	0.008 (2)
O34	0.054 (3)	0.048 (3)	0.075 (3)	−0.029 (2)	−0.038 (2)	0.018 (2)
N1	0.049 (3)	0.030 (3)	0.055 (3)	−0.006 (2)	0.024 (3)	0.008 (2)
N2	0.026 (2)	0.029 (2)	0.031 (2)	−0.0144 (19)	0.0040 (17)	−0.0132 (18)
N3	0.029 (2)	0.022 (2)	0.042 (2)	−0.0096 (19)	−0.0007 (19)	0.0002 (19)
N4	0.027 (2)	0.033 (3)	0.033 (2)	0.000 (2)	−0.0006 (18)	−0.0146 (19)
N5	0.017 (2)	0.046 (3)	0.049 (3)	−0.013 (2)	0.0023 (19)	−0.017 (2)
N6	0.019 (2)	0.029 (2)	0.029 (2)	−0.0018 (18)	−0.0040 (16)	−0.0077 (18)
C11	0.023 (2)	0.028 (3)	0.021 (2)	−0.005 (2)	0.0009 (18)	0.003 (2)
C12	0.028 (3)	0.026 (3)	0.023 (2)	−0.010 (2)	0.0024 (19)	0.002 (2)
C21	0.017 (2)	0.025 (3)	0.024 (2)	0.001 (2)	−0.0036 (18)	−0.0078 (19)
C22	0.017 (2)	0.024 (3)	0.028 (2)	−0.004 (2)	−0.0039 (18)	−0.005 (2)
C31	0.035 (3)	0.021 (3)	0.035 (3)	−0.010 (2)	−0.003 (2)	0.001 (2)
C32	0.019 (2)	0.021 (3)	0.045 (3)	−0.004 (2)	−0.005 (2)	0.000 (2)

Geometric parameters (Å, º)

Ir1—N6	2.051 (4)	O13—C11	1.226 (6)
Ir1—N2	2.056 (4)	O14—C12	1.217 (6)
Ir1—N3	2.079 (4)	O21—C21	1.308 (6)
Ir1—N4	2.089 (4)	O22—C22	1.296 (6)
Ir1—N1	2.093 (4)	O23—C21	1.212 (5)
Ir1—N5	2.098 (4)	O24—C22	1.218 (6)
Ir2—O11	2.029 (3)	O31—C31	1.298 (6)
Ir2—O21	2.041 (3)	O32—C32	1.287 (6)
Ir2—O31	2.043 (3)	O33—C31	1.219 (6)
Ir2—O22	2.050 (3)	O34—C32	1.211 (6)
Ir2—O12	2.051 (3)	C11—C12	1.553 (7)
Ir2—O32	2.053 (3)	C21—C22	1.550 (7)
O11—C11	1.289 (6)	C31—C32	1.545 (7)
O12—C12	1.283 (6)
N6—Ir1—N2	88.43 (16)	O31—Ir2—O32	81.82 (14)
N6—Ir1—N3	89.42 (17)	O22—Ir2—O32	97.18 (14)
N2—Ir1—N3	88.87 (17)	O12—Ir2—O32	96.99 (14)
N6—Ir1—N4	91.04 (17)	C11—O11—Ir2	112.1 (3)
N2—Ir1—N4	178.71 (16)	C12—O12—Ir2	111.8 (3)
N3—Ir1—N4	89.95 (18)	C21—O21—Ir2	112.9 (3)
N6—Ir1—N1	89.42 (19)	C22—O22—Ir2	112.5 (3)
N2—Ir1—N1	89.62 (19)	C31—O31—Ir2	112.3 (3)
N3—Ir1—N1	178.13 (18)	C32—O32—Ir2	111.5 (3)
N4—Ir1—N1	91.55 (19)	O13—C11—O11	125.0 (5)
N6—Ir1—N5	178.15 (18)	O13—C11—C12	120.5 (5)
N2—Ir1—N5	90.40 (17)	O11—C11—C12	114.5 (4)
N3—Ir1—N5	91.98 (18)	O14—C12—O12	123.7 (5)
N4—Ir1—N5	90.16 (18)	O14—C12—C11	119.9 (5)
N1—Ir1—N5	89.1 (2)	O12—C12—C11	116.4 (4)
O11—Ir2—O21	95.91 (14)	O23—C21—O21	123.0 (5)
O11—Ir2—O31	96.78 (14)	O23—C21—C22	121.3 (4)
O21—Ir2—O31	94.33 (14)	O21—C21—C22	115.7 (4)
O11—Ir2—O22	84.27 (15)	O24—C22—O22	123.4 (5)
O21—Ir2—O22	82.35 (14)	O24—C22—C21	120.3 (4)
O31—Ir2—O22	176.61 (13)	O22—C22—C21	116.3 (4)
O11—Ir2—O12	81.90 (14)	O33—C31—O31	123.9 (5)
O21—Ir2—O12	177.12 (13)	O33—C31—C32	120.1 (5)
O31—Ir2—O12	87.81 (14)	O31—C31—C32	115.9 (4)
O22—Ir2—O12	95.54 (14)	O34—C32—O32	124.2 (5)
O11—Ir2—O32	178.26 (13)	O34—C32—C31	119.9 (5)
O21—Ir2—O32	85.24 (14)	O32—C32—C31	115.9 (4)

(lav147_K3CoNH36IrOx32)

Crystal data

K3[Co(NH3)6][Ir(C2O4)3]2·6H2O	Dx = 2.442 Mg m^−3
Mr = 1299.05	Mo Kα radiation, λ = 0.71073 Å
Trigonal, R3:H	Cell parameters from 3992 reflections
a = 10.2003 (8) Å	θ = 2.4–26.3°
c = 29.408 (4) Å	µ = 8.45 mm^−1
V = 2649.8 (5) Å^3	T = 150 K
Z = 3	Plate, yellow
F(000) = 1866	0.12 × 0.08 × 0.04 mm

Data collection

Bruker–Nonius X8 APEX CCD area-detector diffractometer	1200 independent reflections
Graphite monochromator	1135 reflections with I > 2σ(I)
Detector resolution: 25 pixels mm^-1	Rint = 0.042
φ scans	θmax = 26.4°, θmin = 2.7°
Absorption correction: multi-scan Bruker SADABS	h = −12→12
	k = −12→12
7274 measured reflections	l = −36→36

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)] = 0.018	Hydrogen site location: inferred from neighbouring sites
wR(F^2) = 0.042	H-atom parameters constrained
S = 1.11	w = 1/[σ^2(Fo^2) + (0.0141P)^2 + 7.2472P] where P = (Fo^2 + 2Fc^2)/3
1200 reflections	(Δ/σ)max = 0.001
93 parameters	Δρmax = 0.91 e Å^−3
12 restraints	Δρmin = −0.56 e Å^−3

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	Occ. (<1)
Ir1	0.6667	0.3333	0.08004 (2)	0.01547 (8)
Co1	0.0000	0.0000	0.0000	0.0172 (2)
K1	0.3333	0.6667	0.03822 (4)	0.0217 (3)
K2	0.3333	0.6667	0.1667	0.0283 (4)
O1	0.5179 (3)	0.3765 (3)	0.11451 (8)	0.0234 (5)
O2	0.6966 (2)	0.5142 (2)	0.04310 (8)	0.0208 (5)
O3	0.4024 (3)	0.5104 (3)	0.10575 (9)	0.0377 (6)
O4	0.5980 (3)	0.6627 (3)	0.03424 (9)	0.0304 (6)
N1	0.1590 (3)	0.1575 (3)	0.03811 (11)	0.0283 (7)
H1A	0.2479	0.2028	0.0225	0.042*
H1B	0.1700	0.1148	0.0639	0.042*
H1C	0.1326	0.2279	0.0455	0.042*
C1	0.4974 (4)	0.4780 (4)	0.09466 (11)	0.0217 (7)
C2	0.6043 (4)	0.5605 (3)	0.05389 (11)	0.0193 (7)
O1W	0.2420 (9)	0.0704 (9)	0.1268 (2)	0.068 (2)	0.5
O2W	0.1778 (12)	−0.0544 (12)	0.1227 (3)	0.104 (3)	0.5

Atomic displacement parameters (Ų)

	U^11	U^22	U^33	U^12	U^13	U^23
Ir1	0.01488 (9)	0.01488 (9)	0.01664 (12)	0.00744 (5)	0.000	0.000
Co1	0.0151 (3)	0.0151 (3)	0.0215 (5)	0.00756 (16)	0.000	0.000
K1	0.0205 (4)	0.0205 (4)	0.0240 (6)	0.0103 (2)	0.000	0.000
K2	0.0323 (6)	0.0323 (6)	0.0202 (9)	0.0162 (3)	0.000	0.000
O1	0.0266 (13)	0.0262 (12)	0.0206 (12)	0.0156 (11)	0.0087 (9)	0.0061 (9)
O2	0.0207 (12)	0.0197 (11)	0.0226 (12)	0.0106 (10)	0.0059 (9)	0.0044 (9)
O3	0.0416 (16)	0.0465 (17)	0.0411 (16)	0.0342 (14)	0.0160 (12)	0.0088 (13)
O4	0.0295 (14)	0.0243 (13)	0.0425 (16)	0.0173 (11)	0.0065 (11)	0.0128 (11)
N1	0.0251 (16)	0.0253 (16)	0.0320 (17)	0.0108 (13)	−0.0059 (12)	−0.0061 (12)
C1	0.0244 (17)	0.0222 (17)	0.0207 (16)	0.0132 (15)	0.0036 (13)	−0.0003 (13)
C2	0.0170 (16)	0.0168 (16)	0.0215 (17)	0.0065 (13)	0.0010 (12)	−0.0009 (12)
O1W	0.073 (4)	0.070 (4)	0.047 (3)	0.024 (3)	0.001 (3)	0.012 (3)
O2W	0.112 (5)	0.116 (5)	0.080 (5)	0.052 (4)	−0.006 (4)	−0.003 (4)

Geometric parameters (Å, º)

Ir1—O2^i	2.028 (2)	K1—O2^iii	2.942 (2)
Ir1—O2	2.028 (2)	K1—C2^ix	3.467 (3)
Ir1—O2^ii	2.028 (2)	K1—C2^x	3.467 (3)
Ir1—O1^ii	2.048 (2)	K1—C2	3.466 (3)
Ir1—O1^i	2.048 (2)	K2—O3^xii	2.715 (2)
Ir1—O1	2.048 (2)	K2—O3^xiii	2.715 (3)
Ir1—K1^iii	3.4778 (13)	K2—O3^xiv	2.715 (2)
Co1—N1	1.965 (3)	K2—O3^x	2.714 (2)
Co1—N1^iv	1.965 (3)	K2—O3^ix	2.714 (3)
Co1—N1^v	1.965 (3)	K2—O3	2.715 (2)
Co1—N1^vi	1.965 (3)	K2—K1^xii	3.7773 (13)
Co1—N1^vii	1.965 (3)	O1—C1	1.294 (4)
Co1—N1^viii	1.965 (3)	O2—C2	1.286 (4)
K1—O4^ix	2.722 (2)	O2—K1^iii	2.942 (2)
K1—O4^x	2.722 (2)	O3—C1	1.214 (4)
K1—O4	2.722 (2)	O4—C2	1.221 (4)
K1—O3^x	2.847 (3)	N1—H1A	0.9100
K1—O3^ix	2.847 (3)	N1—H1B	0.9100
K1—O3	2.847 (3)	N1—H1C	0.9100
K1—O2^v	2.942 (2)	C1—C2	1.555 (4)
K1—O2^xi	2.942 (2)	O1W—O2W	1.109 (11)
O2^i—Ir1—O2	94.01 (9)	O2^v—K1—C2^ix	83.23 (7)
O2^i—Ir1—O2^ii	94.00 (9)	O2^xi—K1—C2^ix	76.18 (7)
O2—Ir1—O2^ii	94.01 (9)	O2^iii—K1—C2^ix	132.92 (7)
O2^i—Ir1—O1^ii	86.43 (9)	O4^ix—K1—C2^x	105.09 (7)
O2—Ir1—O1^ii	175.97 (8)	O4^x—K1—C2^x	18.14 (7)
O2^ii—Ir1—O1^ii	81.97 (8)	O4—K1—C2^x	135.00 (7)
O2^i—Ir1—O1^i	81.97 (8)	O3^x—K1—C2^x	43.38 (7)
O2—Ir1—O1^i	86.43 (9)	O3^ix—K1—C2^x	120.08 (8)
O2^ii—Ir1—O1^i	175.97 (8)	O3—K1—C2^x	86.98 (8)
O1^ii—Ir1—O1^i	97.60 (8)	O2^v—K1—C2^x	76.18 (7)
O2^i—Ir1—O1	175.97 (8)	O2^xi—K1—C2^x	132.92 (7)
O2—Ir1—O1	81.97 (8)	O2^iii—K1—C2^x	83.23 (7)
O2^ii—Ir1—O1	86.43 (9)	C2^ix—K1—C2^x	118.26 (2)
O1^ii—Ir1—O1	97.60 (8)	O4^ix—K1—C2	135.00 (7)
O1^i—Ir1—O1	97.60 (8)	O4^x—K1—C2	105.09 (7)
O2^i—Ir1—K1^iii	57.62 (6)	O4—K1—C2	18.14 (7)
O2—Ir1—K1^iii	57.62 (6)	O3^x—K1—C2	120.08 (8)
O2^ii—Ir1—K1^iii	57.62 (6)	O3^ix—K1—C2	86.98 (8)
O1^ii—Ir1—K1^iii	119.68 (6)	O3—K1—C2	43.38 (7)
O1^i—Ir1—K1^iii	119.68 (6)	O2^v—K1—C2	132.92 (7)
O1—Ir1—K1^iii	119.68 (6)	O2^xi—K1—C2	83.23 (7)
N1—Co1—N1^iv	180.0	O2^iii—K1—C2	76.18 (7)
N1—Co1—N1^v	89.31 (13)	C2^ix—K1—C2	118.26 (2)
N1^iv—Co1—N1^v	90.69 (13)	C2^x—K1—C2	118.26 (2)
N1—Co1—N1^vi	90.69 (13)	O3^xii—K2—O3^xiii	81.18 (8)
N1^iv—Co1—N1^vi	89.31 (13)	O3^xii—K2—O3^xiv	81.18 (8)
N1^v—Co1—N1^vi	89.31 (13)	O3^xiii—K2—O3^xiv	81.18 (8)
N1—Co1—N1^vii	89.31 (13)	O3^xii—K2—O3^x	98.81 (8)
N1^iv—Co1—N1^vii	90.69 (13)	O3^xiii—K2—O3^x	98.81 (8)
N1^v—Co1—N1^vii	90.69 (13)	O3^xiv—K2—O3^x	180.0
N1^vi—Co1—N1^vii	180.00 (18)	O3^xii—K2—O3^ix	98.82 (8)
N1—Co1—N1^viii	90.69 (13)	O3^xiii—K2—O3^ix	180.0
N1^iv—Co1—N1^viii	89.31 (13)	O3^xiv—K2—O3^ix	98.82 (8)
N1^v—Co1—N1^viii	180.0 (2)	O3^x—K2—O3^ix	81.19 (8)
N1^vi—Co1—N1^viii	90.69 (13)	O3^xii—K2—O3	180.00 (9)
N1^vii—Co1—N1^viii	89.31 (13)	O3^xiii—K2—O3	98.82 (8)
O4^ix—K1—O4^x	119.817 (9)	O3^xiv—K2—O3	98.82 (8)
O4^ix—K1—O4	119.816 (9)	O3^x—K2—O3	81.19 (8)
O4^x—K1—O4	119.817 (9)	O3^ix—K2—O3	81.19 (8)
O4^ix—K1—O3^x	83.27 (8)	O3^xii—K2—K1^xii	48.71 (6)
O4^x—K1—O3^x	59.80 (7)	O3^xiii—K2—K1^xii	48.71 (6)
O4—K1—O3^x	135.26 (8)	O3^xiv—K2—K1^xii	48.70 (6)
O4^ix—K1—O3^ix	59.80 (7)	O3^x—K2—K1^xii	131.29 (6)
O4^x—K1—O3^ix	135.25 (8)	O3^ix—K2—K1^xii	131.29 (6)
O4—K1—O3^ix	83.28 (8)	O3—K2—K1^xii	131.29 (6)
O3^x—K1—O3^ix	76.70 (8)	O3^xii—K2—K1	131.29 (6)
O4^ix—K1—O3	135.25 (8)	O3^xiii—K2—K1	131.29 (6)
O4^x—K1—O3	83.27 (8)	O3^xiv—K2—K1	131.30 (6)
O4—K1—O3	59.80 (7)	O3^x—K2—K1	48.71 (6)
O3^x—K1—O3	76.70 (8)	O3^ix—K2—K1	48.71 (6)
O3^ix—K1—O3	76.70 (8)	O3—K2—K1	48.71 (6)
O4^ix—K1—O2^v	66.78 (7)	K1^xii—K2—K1	180.0
O4^x—K1—O2^v	75.43 (7)	C1—O1—Ir1	112.50 (19)
O4—K1—O2^v	122.74 (8)	C2—O2—Ir1	113.40 (19)
O3^x—K1—O2^v	101.13 (7)	C2—O2—K1^iii	124.42 (19)
O3^ix—K1—O2^v	126.46 (6)	Ir1—O2—K1^iii	86.77 (7)
O3—K1—O2^v	156.09 (7)	C1—O3—K2	144.4 (2)
O4^ix—K1—O2^xi	75.43 (7)	C1—O3—K1	114.8 (2)
O4^x—K1—O2^xi	122.75 (8)	K2—O3—K1	85.53 (7)
O4—K1—O2^xi	66.78 (7)	C2—O4—K1	117.9 (2)
O3^x—K1—O2^xi	156.09 (7)	Co1—N1—H1A	109.5
O3^ix—K1—O2^xi	101.13 (7)	Co1—N1—H1B	109.5
O3—K1—O2^xi	126.46 (7)	H1A—N1—H1B	109.5
O2^v—K1—O2^xi	60.57 (7)	Co1—N1—H1C	109.5
O4^ix—K1—O2^iii	122.75 (8)	H1A—N1—H1C	109.5
O4^x—K1—O2^iii	66.78 (7)	H1B—N1—H1C	109.5
O4—K1—O2^iii	75.43 (7)	O3—C1—O1	124.6 (3)
O3^x—K1—O2^iii	126.46 (7)	O3—C1—C2	119.9 (3)
O3^ix—K1—O2^iii	156.09 (7)	O1—C1—C2	115.5 (3)
O3—K1—O2^iii	101.13 (7)	O3—C1—K1	47.02 (18)
O2^v—K1—O2^iii	60.57 (7)	O1—C1—K1	163.4 (2)
O2^xi—K1—O2^iii	60.57 (7)	C2—C1—K1	74.81 (17)
O4^ix—K1—C2^ix	18.14 (7)	O4—C2—O2	123.9 (3)
O4^x—K1—C2^ix	135.00 (7)	O4—C2—C1	120.3 (3)
O4—K1—C2^ix	105.09 (7)	O2—C2—C1	115.8 (3)
O3^x—K1—C2^ix	86.98 (8)	O4—C2—K1	43.94 (16)
O3^ix—K1—C2^ix	43.38 (7)	O2—C2—K1	157.8 (2)
O3—K1—C2^ix	120.08 (8)	C1—C2—K1	79.54 (17)

Symmetry codes: (i) −x+y+1, −x+1, z; (ii) −y+1, x−y, z; (iii) −x+1, −y+1, −z; (iv) −x, −y, −z; (v) x−y, x, −z; (vi) −y, x−y, z; (vii) y, −x+y, −z; (viii) −x+y, −x, z; (ix) −y+1, x−y+1, z; (x) −x+y, −x+1, z; (xi) y, −x+y+1, −z; (xii) −x+2/3, −y+4/3, −z+1/3; (xiii) y−1/3, −x+y+1/3, −z+1/3; (xiv) x−y+2/3, x+1/3, −z+1/3.