Supporting information
Crystallographic Information File (CIF) https://doi.org/10.1107/S0108270100019776/oa1112sup1.cif | |
Structure factor file (CIF format) https://doi.org/10.1107/S0108270100019776/oa1112Isup2.hkl |
CCDC reference: 162554
A methanol solution of Rh2(O2CC6H5)4(CH3OH)2 was added to a methanol solution of [K(18-crown-6-ether)(H2O)2][Fe(CN)6]3H2O. The mixture solution was allowed to stand for several days in the dark room until almost all the solvent was evaporated. Small brown block crystals for X-ray data collection were obtained. IR(KBr): ν(C≡N) 2112.77 cm-1
All H atoms except water molecule hydrogen atoms were inserted at calculated positions and treated as riding with isotropic displacement parameters.
Metal cyanide compounds have been used to synthesize coordination polymers (Ward, 1995; Vahrenkamp et al., 1997, and references therein). Hexacyanometallate ions [M(CN)]n- can provide one- (Colacio et al., 2000), two- (Miyasaka et al., 1997) and three-dimensional polymers (Miyasaka et al., 1998a,b; Langenberg et al., 1997) since cyano groups are directed to all three axes. Dirhodium acetate units are connected by Co(CN)63- to form a two-dimensional sheet (Lu et al., 1996). It was the first example for dimetal units to be connected by a metal cyanide. Diruthenium units are also bridged by Co(CN)63- to form a pentanuclear complex (Kim et al., 1998).
Ferric cyanide can also be used as a metal cyanide to connect dimetal units to form one-, two-, or three-dimensional compounds. Only the potassium salt among the ferric cyanides is water-soluble. 18-Crown-6-ether can help increase the solubility of a ferric cyanide (Miyasaka et al., 1998a).
Only trans-cyano groups of the ferric cyanide connect dirhodium units to form an one-dimensional chain compound. The Rh—Rh distance is 2.4109 (4) Å which is a little longer than the typical Rh—Rh distance in tetracarboxylatodirhodium(II,II) complexes. Rh—N(bridging cyano group) distances are 2.208 (3) and 2.200 (3) Å. The chain is not linear with angles of 168.1 (3) and 170.7 (3)° for C5—N1—Rh1 and C10—N6—Rh2ii (ii = x, 3/2 - y, z - 1/2), repectively. The benzoate groups of a dirhodium unit are staggered with those of the next dirhodium unit, and also twisted to the four Fe—CN bonds. The Fe—CN bonds of a ferric cyanide are eclipsed with those bonds of the next ferric cyanide. Actually, the ferric cyanide has the possibility to make three-dimensional network structures since all six cyano groups can connect some complex units. However, a benzoate bridging ligand of a dirhodium complex is too bulky to make a two- or three-dimensional compound. Potassium cations encapsulated by crownether are located between anion chains. Two K atoms K1 and K2 are on general positions whereas K3 and K4 are on inversion centres. The asymmetric unit therefore contains 3 crownether molecules. Each K1 and K2 has a water molecule on the one axial site and the other axial site interact with the phenyl group of the benzoate bridging ligand. K3 and K4 have water molecules on both axial sites since it has an inversion centre on the K atom. There are hydrogen bondings between hydrogen atoms of water molecules bonded to the potassium, K3 and K4, and nitrogen atoms, N2, N3, N4 and N5 of free cyano groups.
For related literature, see: Colacio et al. (2000); Kim et al. (1998); Langenberg et al. (1997); Lu et al. (1996); Miyasaka et al. (1997, 1998a, 1998b); Vahrenkamp et al. (1997); Ward (1995).
Data collection: KappaCCD Server Software (Nonius, 1997); cell refinement: DENZO-SMN (Otwinowski & Minor, 1997); data reduction: DENZO-SMN; program(s) used to solve structure: SHELXTL (Sheldrick, 1998); program(s) used to refine structure: SHELXTL; molecular graphics: SHELXTL; software used to prepare material for publication: SHELXTL.
Fig. 1. ORTEP drawing of compound (I). All H atoms are omitted except the water hydrogen atoms. |
[K(C12H24O6)(H2O)]2[K(C12H24O6)(H2O)2][FeRh2(C7H5O2)4 (CN)6]·8H2O | F(000) = 4220 |
Mr = 2028.66 | Dx = 1.447 Mg m−3 |
Monoclinic, P21/c | Mo Kα radiation, λ = 0.71073 Å |
a = 16.0884 (4) Å | Cell parameters from 75952 reflections |
b = 23.1083 (5) Å | θ = 2.6–27.0° |
c = 25.8233 (6) Å | µ = 0.72 mm−1 |
β = 104.090 (1)° | T = 150 K |
V = 9311.6 (4) Å3 | Block, brown |
Z = 4 | 0.25 × 0.15 × 0.14 mm |
Nonius Kappa-CCD diffractometer | 20305 independent reflections |
Radiation source: fine-focus sealed tube | 13576 reflections with I > 2σ(I) |
Graphite monochromator | Rint = 0.042 |
φ scans and ω scans with κ offsets | θmax = 27.0°, θmin = 2.6° |
Absorption correction: multi-scan (SCALEPACK; Otwinowski & Minor, 1997) | h = −21→20 |
Tmin = 0.840, Tmax = 0.906 | k = −30→29 |
75952 measured reflections | l = −32→31 |
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)] = 0.053 | Hydrogen site location: inferred from neighbouring sites |
wR(F2) = 0.116 | H-atom parameters constrained |
S = 1.02 | w = 1/[σ2(Fo2) + (0.0364P)2 + 9.4629P] where P = (Fo2 + 2Fc2)/3 |
20305 reflections | (Δ/σ)max = 0.003 |
1156 parameters | Δρmax = 1.33 e Å−3 |
64 restraints | Δρmin = −0.69 e Å−3 |
[K(C12H24O6)(H2O)]2[K(C12H24O6)(H2O)2][FeRh2(C7H5O2)4 (CN)6]·8H2O | V = 9311.6 (4) Å3 |
Mr = 2028.66 | Z = 4 |
Monoclinic, P21/c | Mo Kα radiation |
a = 16.0884 (4) Å | µ = 0.72 mm−1 |
b = 23.1083 (5) Å | T = 150 K |
c = 25.8233 (6) Å | 0.25 × 0.15 × 0.14 mm |
β = 104.090 (1)° |
Nonius Kappa-CCD diffractometer | 20305 independent reflections |
Absorption correction: multi-scan (SCALEPACK; Otwinowski & Minor, 1997) | 13576 reflections with I > 2σ(I) |
Tmin = 0.840, Tmax = 0.906 | Rint = 0.042 |
75952 measured reflections |
R[F2 > 2σ(F2)] = 0.053 | 64 restraints |
wR(F2) = 0.116 | H-atom parameters constrained |
S = 1.02 | Δρmax = 1.33 e Å−3 |
20305 reflections | Δρmin = −0.69 e Å−3 |
1156 parameters |
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. |
x | y | z | Uiso*/Ueq | ||
Rh1 | 0.236786 (18) | 0.739165 (11) | 0.705813 (10) | 0.01490 (7) | |
Rh2 | 0.253935 (18) | 0.752744 (11) | 0.800397 (10) | 0.01520 (7) | |
Fe1 | 0.24944 (3) | 0.73350 (2) | 0.503479 (18) | 0.01547 (11) | |
O1 | 0.11733 (16) | 0.77579 (10) | 0.69407 (9) | 0.0201 (6) | |
O2 | 0.13363 (16) | 0.78642 (10) | 0.78280 (9) | 0.0216 (6) | |
O3 | 0.18367 (16) | 0.66008 (10) | 0.71555 (9) | 0.0197 (6) | |
O4 | 0.19748 (16) | 0.67472 (10) | 0.80386 (9) | 0.0212 (6) | |
O5 | 0.35729 (16) | 0.70515 (10) | 0.72340 (9) | 0.0206 (6) | |
O6 | 0.37202 (16) | 0.71459 (10) | 0.81248 (9) | 0.0188 (6) | |
O7 | 0.29242 (16) | 0.81762 (10) | 0.70228 (9) | 0.0205 (6) | |
O8 | 0.31019 (16) | 0.83076 (10) | 0.79098 (9) | 0.0190 (6) | |
N1 | 0.22889 (19) | 0.72957 (12) | 0.61971 (11) | 0.0178 (7) | |
N2 | 0.0523 (2) | 0.73853 (13) | 0.45991 (12) | 0.0281 (8) | |
N3 | 0.2475 (2) | 0.59918 (14) | 0.50097 (12) | 0.0252 (7) | |
N4 | 0.4473 (2) | 0.73304 (13) | 0.54512 (12) | 0.0260 (7) | |
N5 | 0.2524 (2) | 0.86766 (14) | 0.50746 (13) | 0.0331 (8) | |
N6 | 0.2647 (2) | 0.73666 (12) | 0.38643 (11) | 0.0192 (7) | |
C1 | 0.0902 (2) | 0.78816 (15) | 0.73472 (14) | 0.0204 (8) | |
C2 | 0.1752 (2) | 0.64517 (15) | 0.76112 (14) | 0.0193 (8) | |
C3 | 0.3993 (2) | 0.70123 (14) | 0.77173 (14) | 0.0182 (8) | |
C4 | 0.3194 (2) | 0.84587 (15) | 0.74553 (13) | 0.0184 (8) | |
C5 | 0.2366 (2) | 0.73104 (14) | 0.57660 (13) | 0.0172 (8) | |
C6 | 0.1254 (3) | 0.73576 (15) | 0.47697 (13) | 0.0199 (8) | |
C7 | 0.2483 (2) | 0.64940 (16) | 0.50164 (13) | 0.0175 (7) | |
C8 | 0.3736 (3) | 0.73266 (15) | 0.52894 (13) | 0.0201 (8) | |
C9 | 0.2512 (2) | 0.81767 (16) | 0.50631 (14) | 0.0217 (8) | |
C10 | 0.2597 (2) | 0.73493 (14) | 0.43002 (14) | 0.0188 (8) | |
C11 | −0.0028 (3) | 0.80440 (15) | 0.72577 (14) | 0.0228 (9) | |
C12 | −0.0453 (3) | 0.79096 (18) | 0.76569 (16) | 0.0340 (10) | |
H12A | −0.0146 | 0.7748 | 0.7986 | 0.041* | |
C13 | −0.1328 (3) | 0.8014 (2) | 0.75665 (17) | 0.0429 (12) | |
H13A | −0.1623 | 0.7916 | 0.7831 | 0.051* | |
C14 | −0.1768 (3) | 0.82610 (19) | 0.70915 (17) | 0.0404 (12) | |
H14A | −0.2365 | 0.8333 | 0.7030 | 0.049* | |
C15 | −0.1338 (3) | 0.84038 (17) | 0.67046 (16) | 0.0330 (10) | |
H15A | −0.1642 | 0.8581 | 0.6382 | 0.040* | |
C16 | −0.0473 (3) | 0.82901 (16) | 0.67838 (15) | 0.0258 (9) | |
H16A | −0.0185 | 0.8381 | 0.6513 | 0.031* | |
C21 | 0.1352 (2) | 0.58737 (14) | 0.76547 (14) | 0.0181 (8) | |
C22 | 0.1354 (3) | 0.56430 (16) | 0.81529 (15) | 0.0270 (9) | |
H22A | 0.1593 | 0.5859 | 0.8467 | 0.032* | |
C23 | 0.1010 (3) | 0.51023 (17) | 0.81937 (17) | 0.0369 (11) | |
H23A | 0.1015 | 0.4948 | 0.8535 | 0.044* | |
C24 | 0.0659 (3) | 0.47844 (17) | 0.77387 (17) | 0.0350 (11) | |
H24A | 0.0426 | 0.4411 | 0.7767 | 0.042* | |
C25 | 0.0651 (3) | 0.50150 (16) | 0.72409 (16) | 0.0323 (10) | |
H25 | 0.0407 | 0.4799 | 0.6927 | 0.039* | |
C26 | 0.0995 (2) | 0.55584 (15) | 0.71984 (15) | 0.0234 (9) | |
H26 | 0.0986 | 0.5714 | 0.6857 | 0.028* | |
C31 | 0.4898 (3) | 0.68055 (15) | 0.78177 (14) | 0.0221 (9) | |
C32 | 0.5308 (3) | 0.65630 (16) | 0.83040 (15) | 0.0293 (10) | |
H32A | 0.5002 | 0.6503 | 0.8571 | 0.035* | |
C33 | 0.6158 (3) | 0.64095 (18) | 0.83988 (17) | 0.0378 (11) | |
H33A | 0.6432 | 0.6237 | 0.8731 | 0.045* | |
C36 | 0.5361 (3) | 0.68937 (17) | 0.74319 (15) | 0.0291 (9) | |
H36A | 0.5086 | 0.7056 | 0.7096 | 0.035* | |
C34 | 0.6619 (3) | 0.65004 (18) | 0.80225 (18) | 0.0406 (12) | |
H34A | 0.7207 | 0.6396 | 0.8095 | 0.049* | |
C35 | 0.6217 (3) | 0.67460 (19) | 0.75374 (17) | 0.0380 (11) | |
H35A | 0.6532 | 0.6813 | 0.7276 | 0.046* | |
C41 | 0.3649 (2) | 0.90148 (15) | 0.74198 (14) | 0.0192 (8) | |
C42 | 0.3929 (3) | 0.93573 (15) | 0.78731 (14) | 0.0259 (9) | |
H42 | 0.3855 | 0.9229 | 0.8209 | 0.031* | |
C43 | 0.4314 (3) | 0.98871 (16) | 0.78325 (16) | 0.0306 (10) | |
H43 | 0.4493 | 1.0123 | 0.8141 | 0.037* | |
C44 | 0.4442 (3) | 1.00758 (17) | 0.73499 (16) | 0.0327 (10) | |
H44A | 0.4709 | 1.0438 | 0.7326 | 0.039* | |
C45 | 0.4176 (3) | 0.97282 (17) | 0.68994 (16) | 0.0327 (10) | |
H45A | 0.4265 | 0.9854 | 0.6567 | 0.039* | |
C46 | 0.3785 (3) | 0.92021 (16) | 0.69323 (15) | 0.0271 (9) | |
H46A | 0.3607 | 0.8967 | 0.6623 | 0.032* | |
K1 | 0.58215 (6) | 0.95905 (4) | 0.88792 (3) | 0.0299 (2) | |
O11 | 0.62998 (18) | 0.86742 (12) | 0.82540 (11) | 0.0352 (7) | |
O12 | 0.53774 (18) | 0.84207 (11) | 0.90339 (10) | 0.0303 (7) | |
O13 | 0.43597 (18) | 0.93303 (11) | 0.92327 (10) | 0.0292 (7) | |
O14 | 0.47653 (18) | 1.04801 (11) | 0.91375 (10) | 0.0282 (6) | |
O15 | 0.59106 (18) | 1.07197 (11) | 0.85216 (10) | 0.0299 (7) | |
O16 | 0.69074 (19) | 0.98241 (12) | 0.82399 (11) | 0.0358 (7) | |
O17 | 0.6850 (2) | 0.89236 (13) | 0.97107 (13) | 0.0525 (9) | |
H1W | 0.7282 (11) | 0.8807 (12) | 0.9604 (7) | 0.063* | |
H2W | 0.6553 (8) | 0.8631 (8) | 0.9758 (10) | 0.063* | |
C101 | 0.7011 (3) | 0.9395 (2) | 0.78678 (18) | 0.0490 (13) | |
H10A | 0.7530 | 0.9477 | 0.7739 | 0.059* | |
H10B | 0.6510 | 0.9397 | 0.7557 | 0.059* | |
C102 | 0.7091 (3) | 0.8818 (2) | 0.81317 (19) | 0.0461 (13) | |
H10C | 0.7237 | 0.8522 | 0.7891 | 0.055* | |
H10D | 0.7555 | 0.8827 | 0.8463 | 0.055* | |
C103 | 0.6342 (3) | 0.81239 (18) | 0.85130 (19) | 0.0417 (12) | |
H10E | 0.6812 | 0.8124 | 0.8842 | 0.050* | |
H10F | 0.6461 | 0.7817 | 0.8274 | 0.050* | |
C104 | 0.5506 (3) | 0.80076 (18) | 0.86494 (18) | 0.0409 (12) | |
H10G | 0.5033 | 0.8034 | 0.8323 | 0.049* | |
H10H | 0.5508 | 0.7612 | 0.8796 | 0.049* | |
C105 | 0.4581 (3) | 0.83225 (16) | 0.91679 (16) | 0.0316 (10) | |
H10I | 0.4597 | 0.7946 | 0.9354 | 0.038* | |
H10J | 0.4112 | 0.8309 | 0.8839 | 0.038* | |
C106 | 0.4421 (3) | 0.87977 (17) | 0.95208 (16) | 0.0353 (11) | |
H10K | 0.3882 | 0.8724 | 0.9630 | 0.042* | |
H10L | 0.4897 | 0.8818 | 0.9846 | 0.042* | |
C107 | 0.3965 (3) | 0.97713 (17) | 0.94772 (16) | 0.0345 (10) | |
H10M | 0.4304 | 0.9840 | 0.9847 | 0.041* | |
H10N | 0.3381 | 0.9650 | 0.9491 | 0.041* | |
C108 | 0.3922 (3) | 1.03115 (17) | 0.91548 (17) | 0.0350 (11) | |
H10O | 0.3572 | 1.0243 | 0.8788 | 0.042* | |
H10P | 0.3649 | 1.0624 | 0.9317 | 0.042* | |
C109 | 0.4792 (3) | 1.10354 (16) | 0.88979 (16) | 0.0326 (10) | |
H10Q | 0.4605 | 1.1338 | 0.9117 | 0.039* | |
H10R | 0.4400 | 1.1042 | 0.8537 | 0.039* | |
C110 | 0.5679 (3) | 1.11517 (16) | 0.88608 (16) | 0.0336 (11) | |
H11A | 0.5717 | 1.1542 | 0.8710 | 0.040* | |
H11B | 0.6075 | 1.1136 | 0.9220 | 0.040* | |
C111 | 0.6745 (3) | 1.08168 (18) | 0.84384 (17) | 0.0374 (11) | |
H11C | 0.7186 | 1.0758 | 0.8776 | 0.045* | |
H11D | 0.6792 | 1.1218 | 0.8315 | 0.045* | |
C112 | 0.6868 (3) | 1.0398 (2) | 0.80284 (18) | 0.0436 (12) | |
H11D' | 0.6387 | 1.0428 | 0.7707 | 0.052* | |
H11E | 0.7406 | 1.0488 | 0.7923 | 0.052* | |
K2 | −0.08470 (6) | 0.53804 (3) | 0.61407 (3) | 0.0281 (2) | |
O21 | −0.05323 (19) | 0.65457 (11) | 0.59088 (11) | 0.0328 (7) | |
O22 | 0.06294 (18) | 0.56599 (11) | 0.58148 (10) | 0.0294 (7) | |
O23 | 0.01956 (18) | 0.44957 (11) | 0.58681 (10) | 0.0303 (7) | |
O24 | −0.08988 (19) | 0.42395 (11) | 0.65138 (11) | 0.0354 (7) | |
O25 | −0.1796 (2) | 0.51358 (13) | 0.68865 (12) | 0.0457 (8) | |
O26 | −0.1323 (2) | 0.62670 (12) | 0.67511 (12) | 0.0427 (8) | |
O27 | −0.2086 (2) | 0.51995 (12) | 0.52878 (12) | 0.0396 (8) | |
H3W | −0.2270 (15) | 0.4866 (3) | 0.5169 (10) | 0.047* | |
H4W | −0.2442 (15) | 0.5455 (4) | 0.5131 (10) | 0.047* | |
C201 | −0.1507 (4) | 0.6779 (2) | 0.6442 (2) | 0.0630 (17) | |
H20A | −0.1676 | 0.7090 | 0.6660 | 0.076* | |
H20B | −0.1992 | 0.6708 | 0.6130 | 0.076* | |
C202 | −0.0762 (4) | 0.69632 (19) | 0.6260 (2) | 0.0531 (14) | |
H20C | −0.0887 | 0.7338 | 0.6071 | 0.064* | |
H20D | −0.0273 | 0.7021 | 0.6572 | 0.064* | |
C203 | 0.0312 (3) | 0.66586 (17) | 0.58450 (17) | 0.0333 (10) | |
H20E | 0.0721 | 0.6679 | 0.6199 | 0.040* | |
H20F | 0.0321 | 0.7035 | 0.5663 | 0.040* | |
C204 | 0.0568 (3) | 0.61907 (17) | 0.55250 (17) | 0.0360 (11) | |
H20G | 0.0138 | 0.6153 | 0.5180 | 0.043* | |
H20H | 0.1128 | 0.6284 | 0.5450 | 0.043* | |
C205 | 0.1015 (3) | 0.52209 (17) | 0.55647 (15) | 0.0314 (10) | |
H20I | 0.1603 | 0.5339 | 0.5557 | 0.038* | |
H20J | 0.0679 | 0.5166 | 0.5192 | 0.038* | |
C206 | 0.1045 (3) | 0.46691 (17) | 0.58654 (16) | 0.0344 (10) | |
H20K | 0.1322 | 0.4365 | 0.5696 | 0.041* | |
H20L | 0.1387 | 0.4723 | 0.6237 | 0.041* | |
C207 | 0.0166 (3) | 0.39343 (16) | 0.60943 (16) | 0.0341 (11) | |
H20M | 0.0573 | 0.3914 | 0.6449 | 0.041* | |
H20N | 0.0332 | 0.3637 | 0.5862 | 0.041* | |
C208 | −0.0722 (3) | 0.38219 (17) | 0.61470 (16) | 0.0382 (12) | |
H20O | −0.1137 | 0.3861 | 0.5796 | 0.046* | |
H20P | −0.0767 | 0.3425 | 0.6283 | 0.046* | |
C209 | −0.1716 (3) | 0.41590 (19) | 0.6623 (2) | 0.0468 (13) | |
H20Q | −0.1787 | 0.3752 | 0.6724 | 0.056* | |
H20R | −0.2177 | 0.4254 | 0.6305 | 0.056* | |
C210 | −0.1752 (3) | 0.4552 (2) | 0.7072 (2) | 0.0501 (14) | |
H21A | −0.2263 | 0.4462 | 0.7207 | 0.060* | |
H21B | −0.1236 | 0.4499 | 0.7368 | 0.060* | |
C211 | −0.1765 (4) | 0.5557 (2) | 0.7291 (2) | 0.0560 (14) | |
H21C | −0.1191 | 0.5556 | 0.7542 | 0.067* | |
H21D | −0.2196 | 0.5465 | 0.7495 | 0.067* | |
C212 | −0.1945 (4) | 0.6135 (2) | 0.7037 (2) | 0.0632 (16) | |
H21E | −0.2522 | 0.6135 | 0.6790 | 0.076* | |
H21F | −0.1934 | 0.6432 | 0.7314 | 0.076* | |
K3 | 0.0000 | 1.0000 | 0.5000 | 0.0314 (3) | |
O31 | −0.1395 (2) | 1.04363 (13) | 0.42965 (12) | 0.0462 (8) | |
O32 | −0.1418 (2) | 0.92572 (14) | 0.46211 (14) | 0.0533 (9) | |
O33 | −0.0085 (2) | 0.88973 (13) | 0.55412 (12) | 0.0439 (8) | |
O34 | −0.0924 (2) | 1.07034 (13) | 0.55466 (12) | 0.0489 (9) | |
H5W | −0.0609 (7) | 1.0978 (8) | 0.5697 (11) | 0.059* | |
H6W | −0.1366 (11) | 1.0832 (11) | 0.5328 (5) | 0.059* | |
C301 | −0.2047 (4) | 1.0041 (2) | 0.4061 (2) | 0.0729 (19) | |
H30A | −0.1883 | 0.9831 | 0.3766 | 0.087* | |
H30B | −0.2587 | 1.0253 | 0.3910 | 0.087* | |
C302 | −0.2177 (3) | 0.9614 (2) | 0.4482 (2) | 0.0668 (17) | |
H30C | −0.2260 | 0.9823 | 0.4800 | 0.080* | |
H30D | −0.2690 | 0.9373 | 0.4338 | 0.080* | |
C303 | −0.1519 (4) | 0.8831 (2) | 0.5007 (2) | 0.0649 (16) | |
H30E | −0.1977 | 0.8554 | 0.4843 | 0.078* | |
H30F | −0.1679 | 0.9021 | 0.5312 | 0.078* | |
C304 | −0.0678 (3) | 0.8519 (2) | 0.5193 (2) | 0.0539 (14) | |
H30G | −0.0760 | 0.8162 | 0.5386 | 0.065* | |
H30H | −0.0452 | 0.8410 | 0.4883 | 0.065* | |
C305 | 0.0734 (3) | 0.86427 (19) | 0.56982 (18) | 0.0446 (13) | |
H30I | 0.0941 | 0.8538 | 0.5379 | 0.054* | |
H30J | 0.0708 | 0.8286 | 0.5907 | 0.054* | |
C306 | 0.1329 (3) | 0.9070 (2) | 0.60315 (18) | 0.0495 (13) | |
H30K | 0.1106 | 0.9191 | 0.6340 | 0.059* | |
H30L | 0.1901 | 0.8893 | 0.6169 | 0.059* | |
K4 | 0.5000 | 1.0000 | 0.5000 | 0.0354 (3) | |
O41 | 0.6303 (2) | 0.98949 (12) | 0.59337 (11) | 0.0397 (8) | |
O42 | 0.54822 (19) | 1.09840 (11) | 0.56555 (11) | 0.0344 (7) | |
O43 | 0.44526 (19) | 1.11088 (12) | 0.45939 (11) | 0.0382 (7) | |
O44 | 0.3935 (2) | 0.94414 (13) | 0.55597 (12) | 0.0489 (9) | |
H7W | 0.3471 (9) | 0.9345 (13) | 0.5339 (5) | 0.059* | |
H8W | 0.4189 (9) | 0.9137 (9) | 0.5706 (12) | 0.059* | |
C401 | 0.6344 (3) | 1.03636 (18) | 0.63010 (16) | 0.0406 (11) | |
H40A | 0.6877 | 1.0338 | 0.6588 | 0.049* | |
H40B | 0.5849 | 1.0346 | 0.6466 | 0.049* | |
C402 | 0.6326 (3) | 1.09211 (18) | 0.59992 (17) | 0.0398 (11) | |
H40C | 0.6457 | 1.1251 | 0.6251 | 0.048* | |
H40D | 0.6760 | 1.0912 | 0.5785 | 0.048* | |
C403 | 0.5393 (3) | 1.15149 (17) | 0.53662 (17) | 0.0380 (11) | |
H40E | 0.5829 | 1.1538 | 0.5155 | 0.046* | |
H40F | 0.5479 | 1.1846 | 0.5617 | 0.046* | |
C404 | 0.4517 (3) | 1.15404 (18) | 0.50043 (17) | 0.0393 (11) | |
H40G | 0.4082 | 1.1467 | 0.5210 | 0.047* | |
H40H | 0.4412 | 1.1929 | 0.4841 | 0.047* | |
C405 | 0.3643 (3) | 1.1117 (2) | 0.42157 (19) | 0.0495 (13) | |
H40I | 0.3545 | 1.1500 | 0.4040 | 0.059* | |
H40J | 0.3178 | 1.1044 | 0.4398 | 0.059* | |
C406 | 0.3640 (3) | 1.06560 (19) | 0.38076 (18) | 0.0459 (12) | |
H40K | 0.3107 | 1.0679 | 0.3520 | 0.055* | |
H40L | 0.4133 | 1.0710 | 0.3646 | 0.055* | |
O1W | 0.0634 (2) | 0.82464 (13) | 0.37229 (12) | 0.0445 (8) | |
H9W | 0.069 (3) | 0.7999 (13) | 0.3973 (11) | 0.053* | |
H10W | 0.098 (2) | 0.8163 (16) | 0.3532 (14) | 0.053* | |
O2W | −0.1266 (2) | 0.74026 (15) | 0.41203 (16) | 0.0589 (10) | |
H11W | −0.0722 (4) | 0.7388 (19) | 0.4218 (19) | 0.071* | |
H12W | −0.142 (2) | 0.7702 (13) | 0.3929 (17) | 0.071* | |
O3W | 0.4301 (2) | 0.79917 (19) | 0.64301 (15) | 0.0707 (12) | |
H13W | 0.3824 (16) | 0.795 (2) | 0.6510 (18) | 0.085* | |
H14W | 0.429 (3) | 0.782 (2) | 0.6137 (11) | 0.085* | |
O4W | −0.1165 (2) | 0.85601 (17) | 0.36766 (17) | 0.0683 (11) | |
H15W | −0.0687 (16) | 0.850 (2) | 0.360 (2) | 0.082* | |
H16W | −0.113 (3) | 0.8860 (14) | 0.3874 (18) | 0.082* | |
O5W | 0.5858 (3) | 0.83273 (17) | 0.70291 (17) | 0.0731 (12) | |
H17W | 0.5334 (8) | 0.825 (2) | 0.689 (2) | 0.088* | |
H18W | 0.617 (2) | 0.8062 (17) | 0.695 (2) | 0.088* | |
O6W | −0.1807 (2) | 0.68322 (19) | 0.49241 (18) | 0.0776 (12) | |
H19W | −0.1326 (15) | 0.674 (2) | 0.5127 (18) | 0.093* | |
H20W | −0.174 (3) | 0.7097 (19) | 0.4709 (17) | 0.093* | |
O7W | 0.6227 (3) | 0.7408 (2) | 0.6205 (3) | 0.1100 (17) | |
H21W | 0.621 (4) | 0.770 (2) | 0.641 (2) | 0.132* | |
H22W | 0.5727 (19) | 0.736 (3) | 0.600 (2) | 0.132* | |
O8W | 0.2612 (8) | 1.2259 (3) | 0.4509 (4) | 0.223 (4) | |
H23W | 0.249 (9) | 1.225 (5) | 0.481 (3) | 0.267* | |
H24W | 0.270 (9) | 1.2609 (18) | 0.443 (5) | 0.267* |
U11 | U22 | U33 | U12 | U13 | U23 | |
Rh1 | 0.01781 (17) | 0.01860 (14) | 0.00902 (13) | −0.00044 (12) | 0.00465 (11) | −0.00224 (11) |
Rh2 | 0.01895 (16) | 0.01851 (14) | 0.00912 (13) | −0.00088 (12) | 0.00529 (11) | −0.00235 (11) |
Fe1 | 0.0201 (3) | 0.0181 (3) | 0.0094 (2) | 0.0004 (2) | 0.0060 (2) | 0.0003 (2) |
O1 | 0.0194 (15) | 0.0273 (14) | 0.0144 (12) | 0.0049 (11) | 0.0054 (11) | −0.0013 (11) |
O2 | 0.0173 (15) | 0.0313 (15) | 0.0164 (13) | 0.0039 (11) | 0.0047 (11) | −0.0056 (11) |
O3 | 0.0283 (16) | 0.0193 (13) | 0.0125 (12) | −0.0019 (11) | 0.0067 (11) | −0.0021 (10) |
O4 | 0.0277 (17) | 0.0243 (14) | 0.0127 (12) | −0.0049 (11) | 0.0073 (11) | −0.0023 (10) |
O5 | 0.0208 (15) | 0.0274 (14) | 0.0139 (13) | 0.0030 (11) | 0.0049 (11) | −0.0040 (11) |
O6 | 0.0208 (15) | 0.0237 (13) | 0.0123 (12) | 0.0016 (11) | 0.0046 (11) | −0.0018 (10) |
O7 | 0.0260 (16) | 0.0215 (13) | 0.0148 (13) | −0.0054 (11) | 0.0065 (11) | −0.0027 (10) |
O8 | 0.0261 (16) | 0.0194 (13) | 0.0125 (12) | −0.0029 (11) | 0.0065 (11) | −0.0029 (10) |
N1 | 0.0231 (18) | 0.0208 (16) | 0.0107 (14) | −0.0032 (13) | 0.0062 (13) | −0.0027 (12) |
N2 | 0.024 (2) | 0.0308 (19) | 0.0285 (18) | 0.0009 (16) | 0.0049 (16) | −0.0025 (15) |
N3 | 0.027 (2) | 0.0256 (18) | 0.0247 (17) | −0.0026 (15) | 0.0101 (14) | −0.0012 (15) |
N4 | 0.027 (2) | 0.0258 (18) | 0.0251 (17) | 0.0013 (15) | 0.0068 (16) | 0.0013 (14) |
N5 | 0.029 (2) | 0.026 (2) | 0.046 (2) | −0.0003 (16) | 0.0126 (18) | −0.0008 (16) |
N6 | 0.0242 (19) | 0.0227 (16) | 0.0119 (14) | 0.0048 (13) | 0.0068 (13) | 0.0049 (13) |
C1 | 0.025 (2) | 0.0164 (18) | 0.0193 (19) | −0.0005 (16) | 0.0048 (17) | −0.0029 (15) |
C2 | 0.019 (2) | 0.0223 (19) | 0.0169 (18) | 0.0033 (16) | 0.0054 (16) | −0.0009 (15) |
C3 | 0.023 (2) | 0.0142 (18) | 0.0186 (19) | −0.0023 (15) | 0.0067 (17) | −0.0025 (15) |
C4 | 0.017 (2) | 0.0202 (19) | 0.0175 (19) | 0.0031 (15) | 0.0041 (16) | −0.0020 (15) |
C5 | 0.020 (2) | 0.0154 (18) | 0.0167 (18) | −0.0015 (15) | 0.0056 (16) | 0.0005 (14) |
C6 | 0.025 (2) | 0.0217 (19) | 0.0140 (17) | −0.0002 (17) | 0.0072 (17) | 0.0016 (15) |
C7 | 0.016 (2) | 0.026 (2) | 0.0118 (16) | −0.0008 (16) | 0.0063 (14) | 0.0010 (16) |
C8 | 0.030 (2) | 0.0188 (19) | 0.0154 (17) | 0.0020 (17) | 0.0124 (17) | 0.0022 (15) |
C9 | 0.017 (2) | 0.027 (2) | 0.023 (2) | 0.0008 (17) | 0.0082 (17) | 0.0027 (17) |
C10 | 0.019 (2) | 0.0172 (18) | 0.0203 (19) | 0.0044 (15) | 0.0052 (16) | 0.0035 (15) |
C11 | 0.024 (2) | 0.024 (2) | 0.0203 (19) | 0.0038 (17) | 0.0043 (17) | −0.0050 (16) |
C12 | 0.025 (3) | 0.052 (3) | 0.025 (2) | 0.010 (2) | 0.0080 (19) | −0.0004 (19) |
C13 | 0.036 (3) | 0.061 (3) | 0.034 (3) | 0.010 (2) | 0.014 (2) | −0.002 (2) |
C14 | 0.027 (3) | 0.053 (3) | 0.040 (3) | 0.012 (2) | 0.006 (2) | −0.015 (2) |
C15 | 0.034 (3) | 0.030 (2) | 0.033 (2) | 0.0106 (19) | 0.003 (2) | −0.0004 (18) |
C16 | 0.026 (2) | 0.026 (2) | 0.025 (2) | 0.0045 (17) | 0.0071 (18) | −0.0051 (17) |
C21 | 0.017 (2) | 0.0171 (18) | 0.0216 (19) | 0.0012 (15) | 0.0064 (16) | −0.0009 (15) |
C22 | 0.032 (3) | 0.026 (2) | 0.024 (2) | −0.0007 (18) | 0.0108 (19) | −0.0002 (17) |
C23 | 0.050 (3) | 0.028 (2) | 0.035 (2) | −0.001 (2) | 0.016 (2) | 0.0100 (19) |
C24 | 0.037 (3) | 0.020 (2) | 0.047 (3) | −0.0034 (19) | 0.009 (2) | 0.005 (2) |
C25 | 0.038 (3) | 0.022 (2) | 0.033 (2) | −0.0014 (19) | 0.001 (2) | −0.0055 (18) |
C26 | 0.025 (2) | 0.021 (2) | 0.023 (2) | −0.0004 (17) | 0.0050 (17) | −0.0005 (16) |
C31 | 0.026 (2) | 0.0209 (19) | 0.0186 (19) | 0.0018 (16) | 0.0045 (17) | −0.0077 (15) |
C32 | 0.037 (3) | 0.026 (2) | 0.025 (2) | 0.0080 (19) | 0.007 (2) | −0.0036 (17) |
C33 | 0.038 (3) | 0.040 (3) | 0.029 (2) | 0.015 (2) | −0.004 (2) | −0.003 (2) |
C36 | 0.026 (3) | 0.039 (2) | 0.023 (2) | 0.0019 (19) | 0.0069 (19) | −0.0045 (18) |
C34 | 0.025 (3) | 0.045 (3) | 0.048 (3) | 0.016 (2) | 0.000 (2) | −0.012 (2) |
C35 | 0.030 (3) | 0.049 (3) | 0.038 (3) | 0.006 (2) | 0.014 (2) | −0.008 (2) |
C41 | 0.018 (2) | 0.0209 (19) | 0.0186 (18) | 0.0027 (15) | 0.0034 (16) | 0.0025 (15) |
C42 | 0.034 (3) | 0.025 (2) | 0.0185 (19) | −0.0037 (18) | 0.0060 (18) | −0.0001 (16) |
C43 | 0.034 (3) | 0.027 (2) | 0.028 (2) | −0.0066 (19) | 0.002 (2) | −0.0017 (18) |
C44 | 0.035 (3) | 0.026 (2) | 0.034 (2) | −0.0082 (19) | 0.004 (2) | 0.0047 (19) |
C45 | 0.037 (3) | 0.036 (2) | 0.025 (2) | −0.005 (2) | 0.008 (2) | 0.0103 (19) |
C46 | 0.031 (3) | 0.030 (2) | 0.020 (2) | −0.0035 (18) | 0.0061 (18) | 0.0016 (17) |
K1 | 0.0332 (6) | 0.0269 (5) | 0.0341 (5) | −0.0003 (4) | 0.0169 (4) | 0.0039 (4) |
O11 | 0.0283 (18) | 0.0378 (17) | 0.0431 (18) | −0.0030 (13) | 0.0157 (15) | −0.0086 (14) |
O12 | 0.0320 (18) | 0.0297 (15) | 0.0318 (15) | −0.0061 (13) | 0.0125 (13) | −0.0034 (12) |
O13 | 0.0325 (18) | 0.0319 (15) | 0.0274 (15) | 0.0016 (13) | 0.0154 (13) | 0.0042 (12) |
O14 | 0.0325 (18) | 0.0247 (14) | 0.0274 (15) | 0.0005 (12) | 0.0077 (13) | 0.0018 (12) |
O15 | 0.0314 (18) | 0.0273 (15) | 0.0304 (15) | −0.0092 (13) | 0.0062 (13) | −0.0004 (12) |
O16 | 0.0368 (19) | 0.0408 (17) | 0.0342 (16) | −0.0065 (14) | 0.0175 (14) | 0.0000 (14) |
O17 | 0.044 (2) | 0.0415 (19) | 0.067 (2) | −0.0037 (16) | 0.0028 (18) | −0.0074 (17) |
C101 | 0.049 (3) | 0.064 (3) | 0.044 (3) | −0.010 (3) | 0.030 (3) | −0.010 (2) |
C102 | 0.034 (3) | 0.054 (3) | 0.057 (3) | −0.008 (2) | 0.024 (3) | −0.024 (2) |
C103 | 0.039 (3) | 0.032 (2) | 0.054 (3) | 0.006 (2) | 0.012 (2) | −0.016 (2) |
C104 | 0.049 (3) | 0.031 (2) | 0.047 (3) | −0.009 (2) | 0.017 (2) | −0.011 (2) |
C105 | 0.033 (3) | 0.028 (2) | 0.034 (2) | −0.0071 (19) | 0.008 (2) | 0.0075 (18) |
C106 | 0.033 (3) | 0.040 (3) | 0.038 (3) | 0.000 (2) | 0.017 (2) | 0.012 (2) |
C107 | 0.033 (3) | 0.043 (3) | 0.032 (2) | 0.002 (2) | 0.018 (2) | 0.000 (2) |
C108 | 0.034 (3) | 0.034 (2) | 0.040 (3) | 0.005 (2) | 0.015 (2) | −0.004 (2) |
C109 | 0.045 (3) | 0.020 (2) | 0.030 (2) | 0.0049 (19) | 0.004 (2) | −0.0004 (17) |
C110 | 0.048 (3) | 0.020 (2) | 0.028 (2) | −0.0033 (19) | 0.000 (2) | −0.0028 (17) |
C111 | 0.031 (3) | 0.034 (2) | 0.045 (3) | −0.010 (2) | 0.004 (2) | 0.016 (2) |
C112 | 0.028 (3) | 0.063 (3) | 0.045 (3) | −0.003 (2) | 0.019 (2) | 0.021 (2) |
K2 | 0.0305 (6) | 0.0244 (5) | 0.0319 (5) | −0.0027 (4) | 0.0123 (4) | 0.0009 (4) |
O21 | 0.0381 (19) | 0.0235 (15) | 0.0412 (17) | −0.0034 (13) | 0.0180 (15) | −0.0055 (12) |
O22 | 0.0330 (18) | 0.0296 (15) | 0.0282 (15) | −0.0021 (13) | 0.0127 (13) | 0.0010 (12) |
O23 | 0.0326 (18) | 0.0290 (15) | 0.0280 (15) | −0.0012 (13) | 0.0049 (13) | 0.0006 (12) |
O24 | 0.0313 (19) | 0.0290 (16) | 0.0450 (18) | −0.0098 (13) | 0.0077 (15) | −0.0006 (13) |
O25 | 0.053 (2) | 0.0419 (19) | 0.050 (2) | −0.0049 (16) | 0.0288 (17) | 0.0077 (16) |
O26 | 0.048 (2) | 0.0375 (18) | 0.052 (2) | 0.0026 (15) | 0.0305 (17) | −0.0051 (15) |
O27 | 0.041 (2) | 0.0293 (16) | 0.0479 (19) | −0.0010 (14) | 0.0102 (16) | −0.0048 (14) |
C201 | 0.084 (5) | 0.035 (3) | 0.090 (4) | 0.009 (3) | 0.058 (4) | −0.005 (3) |
C202 | 0.083 (4) | 0.029 (2) | 0.061 (3) | −0.003 (3) | 0.043 (3) | −0.012 (2) |
C203 | 0.035 (3) | 0.028 (2) | 0.037 (2) | −0.0095 (19) | 0.009 (2) | 0.0060 (19) |
C204 | 0.035 (3) | 0.037 (2) | 0.040 (3) | 0.000 (2) | 0.018 (2) | 0.011 (2) |
C205 | 0.030 (3) | 0.040 (2) | 0.027 (2) | −0.003 (2) | 0.011 (2) | −0.0056 (19) |
C206 | 0.036 (3) | 0.036 (2) | 0.030 (2) | 0.005 (2) | 0.007 (2) | −0.0080 (19) |
C207 | 0.047 (3) | 0.021 (2) | 0.030 (2) | 0.003 (2) | 0.002 (2) | −0.0026 (18) |
C208 | 0.050 (3) | 0.022 (2) | 0.033 (2) | −0.008 (2) | −0.008 (2) | 0.0037 (18) |
C209 | 0.032 (3) | 0.036 (3) | 0.071 (4) | −0.007 (2) | 0.009 (3) | 0.018 (2) |
C210 | 0.033 (3) | 0.056 (3) | 0.066 (3) | −0.002 (2) | 0.022 (3) | 0.033 (3) |
C211 | 0.061 (4) | 0.067 (4) | 0.054 (3) | 0.001 (3) | 0.040 (3) | −0.001 (3) |
C212 | 0.075 (4) | 0.062 (4) | 0.070 (4) | −0.005 (3) | 0.051 (3) | −0.010 (3) |
K3 | 0.0287 (8) | 0.0310 (7) | 0.0322 (7) | 0.0012 (6) | 0.0028 (6) | −0.0017 (5) |
O31 | 0.041 (2) | 0.0426 (19) | 0.0468 (19) | 0.0065 (16) | −0.0051 (16) | 0.0020 (15) |
O32 | 0.042 (2) | 0.044 (2) | 0.070 (2) | −0.0007 (16) | 0.0058 (19) | −0.0012 (17) |
O33 | 0.047 (2) | 0.0389 (18) | 0.050 (2) | 0.0076 (16) | 0.0196 (17) | 0.0035 (15) |
O34 | 0.051 (2) | 0.057 (2) | 0.0350 (18) | 0.0165 (17) | 0.0047 (16) | 0.0000 (15) |
C301 | 0.064 (4) | 0.061 (4) | 0.069 (4) | 0.002 (3) | −0.031 (3) | 0.001 (3) |
C302 | 0.033 (3) | 0.056 (3) | 0.100 (5) | −0.003 (3) | −0.008 (3) | 0.003 (3) |
C303 | 0.054 (4) | 0.051 (3) | 0.087 (4) | −0.019 (3) | 0.012 (3) | 0.008 (3) |
C304 | 0.058 (4) | 0.036 (3) | 0.064 (3) | −0.008 (3) | 0.009 (3) | 0.003 (2) |
C305 | 0.054 (3) | 0.041 (3) | 0.048 (3) | 0.018 (2) | 0.028 (3) | 0.018 (2) |
C306 | 0.049 (4) | 0.059 (3) | 0.038 (3) | 0.014 (3) | 0.004 (3) | 0.013 (2) |
K4 | 0.0361 (9) | 0.0343 (7) | 0.0330 (7) | −0.0018 (6) | 0.0027 (6) | −0.0062 (6) |
O41 | 0.047 (2) | 0.0379 (17) | 0.0318 (16) | −0.0065 (15) | 0.0050 (15) | −0.0020 (14) |
O42 | 0.038 (2) | 0.0343 (16) | 0.0313 (16) | −0.0111 (14) | 0.0093 (14) | −0.0026 (13) |
O43 | 0.037 (2) | 0.0360 (17) | 0.0396 (17) | −0.0002 (14) | 0.0055 (15) | −0.0016 (14) |
O44 | 0.048 (2) | 0.055 (2) | 0.044 (2) | −0.0078 (17) | 0.0098 (17) | −0.0093 (16) |
C401 | 0.040 (3) | 0.050 (3) | 0.031 (2) | −0.007 (2) | 0.006 (2) | −0.008 (2) |
C402 | 0.040 (3) | 0.043 (3) | 0.038 (3) | −0.011 (2) | 0.013 (2) | −0.010 (2) |
C403 | 0.054 (3) | 0.029 (2) | 0.038 (2) | −0.008 (2) | 0.024 (2) | −0.007 (2) |
C404 | 0.046 (3) | 0.029 (2) | 0.046 (3) | 0.001 (2) | 0.017 (2) | 0.003 (2) |
C405 | 0.042 (3) | 0.047 (3) | 0.055 (3) | 0.005 (2) | 0.001 (3) | 0.007 (2) |
C406 | 0.046 (3) | 0.046 (3) | 0.039 (3) | −0.004 (2) | −0.003 (2) | 0.005 (2) |
O1W | 0.053 (2) | 0.046 (2) | 0.0377 (19) | 0.0091 (16) | 0.0172 (17) | 0.0127 (15) |
O2W | 0.032 (2) | 0.052 (2) | 0.086 (3) | 0.0006 (17) | 0.001 (2) | 0.0068 (19) |
O3W | 0.051 (3) | 0.111 (3) | 0.056 (2) | −0.027 (2) | 0.025 (2) | −0.051 (2) |
O4W | 0.056 (3) | 0.062 (3) | 0.076 (3) | 0.004 (2) | −0.005 (2) | −0.006 (2) |
O5W | 0.055 (3) | 0.081 (3) | 0.079 (3) | −0.015 (2) | 0.008 (3) | 0.013 (2) |
O6W | 0.042 (3) | 0.084 (3) | 0.096 (3) | −0.013 (2) | −0.005 (2) | 0.030 (2) |
O7W | 0.084 (4) | 0.084 (4) | 0.146 (5) | −0.004 (3) | −0.003 (3) | 0.009 (3) |
O8W | 0.240 (10) | 0.154 (7) | 0.295 (12) | 0.019 (7) | 0.104 (10) | 0.040 (7) |
Rh1—O7 | 2.034 (2) | O14—C108 | 1.422 (5) |
Rh1—O5 | 2.038 (2) | O14—C109 | 1.430 (4) |
Rh1—O1 | 2.054 (2) | O15—C111 | 1.427 (5) |
Rh1—O3 | 2.059 (2) | O15—C110 | 1.435 (4) |
Rh1—N1 | 2.207 (3) | O16—C101 | 1.419 (5) |
Rh1—Rh2 | 2.4109 (4) | O16—C112 | 1.430 (5) |
Rh2—O4 | 2.031 (2) | C101—C102 | 1.489 (6) |
Rh2—O2 | 2.032 (2) | C103—C104 | 1.495 (6) |
Rh2—O6 | 2.048 (2) | C105—C106 | 1.489 (5) |
Rh2—O8 | 2.058 (2) | C107—C108 | 1.493 (5) |
Rh2—N6i | 2.200 (3) | C109—C110 | 1.479 (6) |
Fe1—C7 | 1.944 (4) | C111—C112 | 1.483 (6) |
Fe1—C10 | 1.944 (3) | K2—O27 | 2.620 (3) |
Fe1—C8 | 1.944 (4) | K2—O22 | 2.782 (3) |
Fe1—C9 | 1.946 (4) | K2—O25 | 2.791 (3) |
Fe1—C6 | 1.947 (4) | K2—O26 | 2.803 (3) |
Fe1—C5 | 1.950 (3) | K2—O24 | 2.815 (3) |
O1—C1 | 1.264 (4) | K2—O21 | 2.831 (3) |
O2—C1 | 1.268 (4) | K2—O23 | 2.840 (3) |
O3—C2 | 1.265 (4) | O21—C203 | 1.431 (5) |
O4—C2 | 1.273 (4) | O21—C202 | 1.432 (5) |
O5—C3 | 1.270 (4) | O22—C205 | 1.424 (4) |
O6—C3 | 1.273 (4) | O22—C204 | 1.428 (4) |
O7—C4 | 1.275 (4) | O23—C206 | 1.425 (5) |
O8—C4 | 1.267 (4) | O23—C207 | 1.428 (4) |
N1—C5 | 1.150 (4) | O24—C209 | 1.423 (5) |
N2—C6 | 1.152 (5) | O24—C208 | 1.428 (5) |
N3—C7 | 1.161 (4) | O25—C211 | 1.420 (5) |
N4—C8 | 1.158 (5) | O25—C210 | 1.427 (5) |
N5—C9 | 1.156 (5) | O26—C212 | 1.413 (5) |
N6—C10 | 1.148 (4) | O26—C201 | 1.417 (5) |
N6—Rh2ii | 2.200 (3) | C201—C202 | 1.454 (6) |
C1—C11 | 1.504 (5) | C203—C204 | 1.479 (5) |
C2—C21 | 1.499 (5) | C205—C206 | 1.488 (5) |
C3—C31 | 1.494 (5) | C207—C208 | 1.490 (6) |
C4—C41 | 1.493 (5) | C209—C210 | 1.485 (6) |
C11—C16 | 1.381 (5) | C211—C212 | 1.486 (7) |
C11—C12 | 1.404 (5) | K3—O31 | 2.715 (3) |
C12—C13 | 1.390 (6) | K3—O31iii | 2.715 (3) |
C13—C14 | 1.382 (6) | K3—O34iii | 2.804 (3) |
C14—C15 | 1.385 (6) | K3—O34 | 2.804 (3) |
C15—C16 | 1.383 (5) | K3—O32 | 2.832 (3) |
C21—C26 | 1.385 (5) | K3—O32iii | 2.832 (3) |
C21—C22 | 1.392 (5) | K3—O33 | 2.925 (3) |
C22—C23 | 1.381 (5) | K3—O33iii | 2.925 (3) |
C23—C24 | 1.384 (6) | O31—C301 | 1.412 (6) |
C24—C25 | 1.388 (5) | O31—C306iii | 1.440 (5) |
C25—C26 | 1.388 (5) | O32—C303 | 1.437 (6) |
C31—C32 | 1.386 (5) | O32—C302 | 1.445 (6) |
C31—C36 | 1.396 (5) | O33—C305 | 1.410 (5) |
C32—C33 | 1.377 (6) | O33—C304 | 1.436 (5) |
C33—C34 | 1.374 (6) | C301—C302 | 1.520 (7) |
C36—C35 | 1.380 (6) | C303—C304 | 1.505 (7) |
C34—C35 | 1.384 (6) | C305—C306 | 1.494 (6) |
C41—C42 | 1.394 (5) | C306—O31iii | 1.440 (5) |
C41—C46 | 1.397 (5) | K4—O41iv | 2.794 (3) |
C42—C43 | 1.388 (5) | K4—O41 | 2.794 (3) |
C43—C44 | 1.382 (5) | K4—O44iv | 2.810 (3) |
C44—C45 | 1.393 (5) | K4—O44 | 2.810 (3) |
C45—C46 | 1.381 (5) | K4—O43 | 2.827 (3) |
K1—O16 | 2.734 (3) | K4—O43iv | 2.827 (3) |
K1—O15 | 2.783 (3) | K4—O42iv | 2.828 (3) |
K1—O13 | 2.788 (3) | K4—O42 | 2.828 (3) |
K1—O17 | 2.827 (3) | O41—C406iv | 1.430 (5) |
K1—O14 | 2.848 (3) | O41—C401 | 1.431 (5) |
K1—O12 | 2.849 (3) | O42—C403 | 1.425 (5) |
K1—O11 | 2.879 (3) | O42—C402 | 1.438 (5) |
O11—C102 | 1.424 (5) | O43—C405 | 1.425 (5) |
O11—C103 | 1.431 (5) | O43—C404 | 1.441 (5) |
O12—C105 | 1.424 (5) | C401—C402 | 1.502 (6) |
O12—C104 | 1.428 (5) | C403—C404 | 1.490 (6) |
O13—C107 | 1.426 (4) | C405—C406 | 1.497 (6) |
O13—C106 | 1.429 (4) | C406—O41iv | 1.430 (5) |
O7—Rh1—O5 | 87.05 (10) | O12—C104—C103 | 109.5 (3) |
O7—Rh1—O1 | 91.85 (10) | O12—C105—C106 | 109.3 (3) |
O5—Rh1—O1 | 175.56 (9) | O13—C106—C105 | 108.5 (3) |
O7—Rh1—O3 | 175.69 (9) | O13—C107—C108 | 108.4 (3) |
O5—Rh1—O3 | 91.78 (10) | O14—C108—C107 | 109.4 (3) |
O1—Rh1—O3 | 89.00 (10) | O14—C109—C110 | 108.8 (3) |
O7—Rh1—N1 | 87.84 (10) | O15—C110—C109 | 108.1 (3) |
O5—Rh1—N1 | 90.23 (10) | O15—C111—C112 | 107.4 (3) |
O1—Rh1—N1 | 94.03 (10) | O16—C112—C111 | 109.5 (3) |
O3—Rh1—N1 | 96.32 (9) | O27—K2—O22 | 108.29 (9) |
O7—Rh1—Rh2 | 89.22 (6) | O27—K2—O25 | 96.65 (10) |
O5—Rh1—Rh2 | 87.50 (6) | O22—K2—O25 | 155.00 (9) |
O1—Rh1—Rh2 | 88.18 (6) | O27—K2—O26 | 109.46 (10) |
O3—Rh1—Rh2 | 86.58 (6) | O22—K2—O26 | 111.75 (9) |
N1—Rh1—Rh2 | 176.38 (8) | O25—K2—O26 | 59.32 (9) |
O4—Rh2—O2 | 86.45 (10) | O27—K2—O24 | 93.35 (9) |
O4—Rh2—O6 | 91.10 (10) | O22—K2—O24 | 114.80 (9) |
O2—Rh2—O6 | 175.17 (9) | O25—K2—O24 | 60.50 (9) |
O4—Rh2—O8 | 175.77 (9) | O26—K2—O24 | 117.21 (9) |
O2—Rh2—O8 | 93.46 (10) | O27—K2—O21 | 96.47 (9) |
O6—Rh2—O8 | 88.67 (10) | O22—K2—O21 | 60.35 (8) |
O4—Rh2—N6i | 88.88 (10) | O25—K2—O21 | 119.64 (9) |
O2—Rh2—N6i | 91.12 (10) | O26—K2—O21 | 60.73 (8) |
O6—Rh2—N6i | 92.99 (10) | O24—K2—O21 | 170.05 (9) |
O8—Rh2—N6i | 95.35 (10) | O27—K2—O23 | 92.95 (9) |
O4—Rh2—Rh1 | 89.25 (6) | O22—K2—O23 | 59.52 (8) |
O2—Rh2—Rh1 | 87.44 (6) | O25—K2—O23 | 118.73 (9) |
O6—Rh2—Rh1 | 88.37 (6) | O26—K2—O23 | 157.58 (9) |
O8—Rh2—Rh1 | 86.53 (6) | O24—K2—O23 | 58.61 (8) |
N6i—Rh2—Rh1 | 177.71 (8) | O21—K2—O23 | 119.04 (8) |
C7—Fe1—C10 | 89.76 (14) | C203—O21—C202 | 110.4 (3) |
C7—Fe1—C8 | 90.06 (15) | C203—O21—K2 | 114.9 (2) |
C10—Fe1—C8 | 90.34 (14) | C202—O21—K2 | 114.8 (2) |
C7—Fe1—C9 | 179.26 (15) | C205—O22—C204 | 110.9 (3) |
C10—Fe1—C9 | 90.90 (14) | C205—O22—K2 | 118.0 (2) |
C8—Fe1—C9 | 89.61 (15) | C204—O22—K2 | 113.7 (2) |
C7—Fe1—C6 | 90.89 (15) | C206—O23—C207 | 112.6 (3) |
C10—Fe1—C6 | 88.85 (14) | C206—O23—K2 | 115.1 (2) |
C8—Fe1—C6 | 178.74 (15) | C207—O23—K2 | 118.2 (2) |
C9—Fe1—C6 | 89.44 (15) | C209—O24—C208 | 112.7 (3) |
C7—Fe1—C5 | 89.54 (13) | C209—O24—K2 | 107.2 (2) |
C10—Fe1—C5 | 178.66 (15) | C208—O24—K2 | 112.2 (2) |
C8—Fe1—C5 | 90.81 (14) | C211—O25—C210 | 114.2 (4) |
C9—Fe1—C5 | 89.81 (14) | C211—O25—K2 | 116.3 (3) |
C6—Fe1—C5 | 90.02 (14) | C210—O25—K2 | 115.6 (3) |
C1—O1—Rh1 | 118.1 (2) | C212—O26—C201 | 113.4 (4) |
C1—O2—Rh2 | 119.9 (2) | C212—O26—K2 | 117.4 (3) |
C2—O3—Rh1 | 119.8 (2) | C201—O26—K2 | 110.0 (2) |
C2—O4—Rh2 | 118.2 (2) | O26—C201—C202 | 110.6 (4) |
C3—O5—Rh1 | 119.8 (2) | O21—C202—C201 | 111.6 (4) |
C3—O6—Rh2 | 118.2 (2) | O21—C203—C204 | 109.4 (3) |
C4—O7—Rh1 | 118.5 (2) | O22—C204—C203 | 109.2 (3) |
C4—O8—Rh2 | 120.3 (2) | O22—C205—C206 | 109.7 (3) |
C5—N1—Rh1 | 168.1 (3) | O23—C206—C205 | 109.5 (3) |
C10—N6—Rh2ii | 170.7 (3) | O23—C207—C208 | 108.9 (3) |
O1—C1—O2 | 125.9 (3) | O24—C208—C207 | 107.0 (3) |
O1—C1—C11 | 117.4 (3) | O24—C209—C210 | 106.8 (4) |
O2—C1—C11 | 116.7 (3) | O25—C210—C209 | 109.0 (4) |
O3—C2—O4 | 126.1 (3) | O25—C211—C212 | 108.7 (4) |
O3—C2—C21 | 117.3 (3) | O26—C212—C211 | 109.8 (4) |
O4—C2—C21 | 116.6 (3) | O31—K3—O31iii | 180.000 (1) |
O5—C3—O6 | 125.9 (3) | O31—K3—O34iii | 109.37 (9) |
O5—C3—C31 | 117.2 (3) | O31iii—K3—O34iii | 70.63 (9) |
O6—C3—C31 | 116.9 (3) | O31—K3—O34 | 70.63 (9) |
O8—C4—O7 | 125.4 (3) | O31iii—K3—O34 | 109.37 (9) |
O8—C4—C41 | 117.6 (3) | O34iii—K3—O34 | 180.000 (1) |
O7—C4—C41 | 117.0 (3) | O31—K3—O32 | 61.88 (9) |
N1—C5—Fe1 | 179.8 (4) | O31iii—K3—O32 | 118.12 (9) |
N2—C6—Fe1 | 177.5 (3) | O34iii—K3—O32 | 87.48 (10) |
N3—C7—Fe1 | 179.4 (3) | O34—K3—O32 | 92.52 (10) |
N4—C8—Fe1 | 178.3 (3) | O31—K3—O32iii | 118.12 (9) |
N5—C9—Fe1 | 179.3 (3) | O31iii—K3—O32iii | 61.88 (9) |
N6—C10—Fe1 | 178.7 (3) | O34iii—K3—O32iii | 92.52 (10) |
C16—C11—C12 | 120.1 (4) | O34—K3—O32iii | 87.48 (10) |
C16—C11—C1 | 121.4 (3) | O32—K3—O32iii | 180.00 (10) |
C12—C11—C1 | 118.4 (3) | O31—K3—O33 | 121.07 (10) |
C13—C12—C11 | 119.5 (4) | O31iii—K3—O33 | 58.93 (10) |
C14—C13—C12 | 120.0 (4) | O34iii—K3—O33 | 80.08 (9) |
C13—C14—C15 | 120.1 (4) | O34—K3—O33 | 99.92 (9) |
C16—C15—C14 | 120.6 (4) | O32—K3—O33 | 60.64 (9) |
C11—C16—C15 | 119.7 (4) | O32iii—K3—O33 | 119.36 (9) |
C26—C21—C22 | 119.5 (3) | O31—K3—O33iii | 58.93 (10) |
C26—C21—C2 | 120.1 (3) | O31iii—K3—O33iii | 121.07 (10) |
C22—C21—C2 | 120.4 (3) | O34iii—K3—O33iii | 99.92 (9) |
C23—C22—C21 | 120.4 (4) | O34—K3—O33iii | 80.08 (9) |
C22—C23—C24 | 120.2 (4) | O32—K3—O33iii | 119.36 (9) |
C23—C24—C25 | 119.5 (4) | O32iii—K3—O33iii | 60.64 (9) |
C26—C25—C24 | 120.4 (4) | O33—K3—O33iii | 180.000 (1) |
C21—C26—C25 | 120.0 (3) | C301—O31—C306iii | 114.3 (4) |
C32—C31—C36 | 119.2 (4) | C301—O31—K3 | 117.1 (3) |
C32—C31—C3 | 120.9 (3) | C306iii—O31—K3 | 121.4 (3) |
C36—C31—C3 | 119.7 (3) | C303—O32—C302 | 109.4 (4) |
C33—C32—C31 | 119.8 (4) | C303—O32—K3 | 113.1 (3) |
C34—C33—C32 | 121.2 (4) | C302—O32—K3 | 107.5 (3) |
C35—C36—C31 | 120.2 (4) | C305—O33—C304 | 111.0 (4) |
C33—C34—C35 | 119.3 (4) | C305—O33—K3 | 110.6 (2) |
C36—C35—C34 | 120.3 (4) | C304—O33—K3 | 109.4 (3) |
C42—C41—C46 | 119.5 (3) | O31—C301—C302 | 109.2 (4) |
C42—C41—C4 | 120.0 (3) | O32—C302—C301 | 107.1 (5) |
C46—C41—C4 | 120.6 (3) | O32—C303—C304 | 107.8 (4) |
C43—C42—C41 | 119.7 (3) | O33—C304—C303 | 108.5 (4) |
C44—C43—C42 | 120.9 (4) | O33—C305—C306 | 108.2 (4) |
C43—C44—C45 | 119.2 (4) | O31iii—C306—C305 | 108.3 (4) |
C46—C45—C44 | 120.6 (4) | O41iv—K4—O41 | 180.000 (1) |
C45—C46—C41 | 120.1 (4) | O41iv—K4—O44iv | 86.54 (9) |
O16—K1—O15 | 61.47 (8) | O41—K4—O44iv | 93.46 (9) |
O16—K1—O13 | 162.65 (9) | O41iv—K4—O44 | 93.46 (9) |
O15—K1—O13 | 115.25 (8) | O41—K4—O44 | 86.54 (9) |
O16—K1—O17 | 102.96 (10) | O44iv—K4—O44 | 180.00 (11) |
O15—K1—O17 | 134.03 (9) | O41iv—K4—O43 | 60.04 (8) |
O13—K1—O17 | 91.05 (9) | O41—K4—O43 | 119.96 (8) |
O16—K1—O14 | 120.28 (8) | O44iv—K4—O43 | 64.32 (9) |
O15—K1—O14 | 58.85 (8) | O44—K4—O43 | 115.68 (9) |
O13—K1—O14 | 58.66 (8) | O41iv—K4—O43iv | 119.96 (8) |
O17—K1—O14 | 119.21 (9) | O41—K4—O43iv | 60.04 (8) |
O16—K1—O12 | 119.41 (8) | O44iv—K4—O43iv | 115.68 (9) |
O15—K1—O12 | 166.18 (9) | O44—K4—O43iv | 64.32 (9) |
O13—K1—O12 | 59.27 (8) | O43—K4—O43iv | 180.00 (11) |
O17—K1—O12 | 59.79 (9) | O41iv—K4—O42iv | 60.95 (8) |
O14—K1—O12 | 117.89 (8) | O41—K4—O42iv | 119.05 (8) |
O16—K1—O11 | 60.61 (8) | O44iv—K4—O42iv | 100.04 (8) |
O15—K1—O11 | 117.46 (8) | O44—K4—O42iv | 79.96 (8) |
O13—K1—O11 | 112.77 (8) | O43—K4—O42iv | 119.43 (8) |
O17—K1—O11 | 80.68 (9) | O43iv—K4—O42iv | 60.57 (8) |
O14—K1—O11 | 156.71 (9) | O41iv—K4—O42 | 119.05 (8) |
O12—K1—O11 | 59.41 (8) | O41—K4—O42 | 60.95 (8) |
C102—O11—C103 | 111.5 (3) | O44iv—K4—O42 | 79.96 (8) |
C102—O11—K1 | 109.2 (2) | O44—K4—O42 | 100.04 (8) |
C103—O11—K1 | 112.4 (2) | O43—K4—O42 | 60.57 (8) |
C105—O12—C104 | 110.7 (3) | O43iv—K4—O42 | 119.43 (8) |
C105—O12—K1 | 117.2 (2) | O42iv—K4—O42 | 180.00 (6) |
C104—O12—K1 | 116.9 (2) | C406iv—O41—C401 | 112.1 (3) |
C107—O13—C106 | 111.5 (3) | C406iv—O41—K4 | 115.4 (2) |
C107—O13—K1 | 119.5 (2) | C401—O41—K4 | 114.2 (2) |
C106—O13—K1 | 113.5 (2) | C403—O42—C402 | 111.7 (3) |
C108—O14—C109 | 112.9 (3) | C403—O42—K4 | 113.6 (2) |
C108—O14—K1 | 115.9 (2) | C402—O42—K4 | 111.6 (2) |
C109—O14—K1 | 117.6 (2) | C405—O43—C404 | 112.7 (3) |
C111—O15—C110 | 112.0 (3) | C405—O43—K4 | 114.6 (2) |
C111—O15—K1 | 108.9 (2) | C404—O43—K4 | 113.2 (2) |
C110—O15—K1 | 114.1 (2) | O41—C401—C402 | 108.2 (3) |
C101—O16—C112 | 113.1 (3) | O42—C402—C401 | 107.6 (4) |
C101—O16—K1 | 117.9 (2) | O42—C403—C404 | 108.8 (3) |
C112—O16—K1 | 116.0 (2) | O43—C404—C403 | 108.8 (4) |
O16—C101—C102 | 109.2 (4) | O43—C405—C406 | 108.6 (4) |
O11—C102—C101 | 109.1 (4) | O41iv—C406—C405 | 108.4 (4) |
O11—C103—C104 | 109.1 (4) |
Symmetry codes: (i) x, −y+3/2, z+1/2; (ii) x, −y+3/2, z−1/2; (iii) −x, −y+2, −z+1; (iv) −x+1, −y+2, −z+1. |
D—H···A | D—H | H···A | D···A | D—H···A |
O17—H1W···O6Wv | 0.85 (1) | 2.10 (1) | 2.728 (5) | 130 (1) |
O17—H2W···O12 | 0.86 (1) | 2.36 (2) | 2.829 (4) | 115 (1) |
O27—H3W···N3vi | 0.86 (1) | 2.04 (1) | 2.885 (4) | 168 (1) |
O27—H4W···O17vii | 0.85 (1) | 1.98 (1) | 2.831 (4) | 172 (4) |
O34—H5W···O1Wiii | 0.84 (1) | 2.34 (1) | 3.039 (4) | 140 (1) |
O34—H6W···N5iii | 0.85 (1) | 2.21 (1) | 3.040 (5) | 166 (1) |
O44—H7W···N5 | 0.85 (1) | 2.16 (2) | 2.909 (5) | 147 (2) |
O44—H8W···O43iv | 0.85 (1) | 2.55 (1) | 3.000 (5) | 114 (1) |
O1W—H9W···N2 | 0.85 (1) | 2.21 (1) | 3.051 (4) | 167 (4) |
O1W—H10W···O4ii | 0.85 (1) | 2.28 (1) | 3.104 (4) | 162 (4) |
O2W—H11W···N2 | 0.85 (1) | 2.01 (1) | 2.842 (5) | 168 (5) |
O2W—H12W···O4W | 0.85 (1) | 2.16 (2) | 2.930 (5) | 151 (4) |
O3W—H13W···O7 | 0.85 (1) | 2.25 (2) | 3.014 (4) | 150 (4) |
O3W—H14W···N4 | 0.85 (1) | 2.18 (1) | 3.023 (4) | 171 (5) |
O4W—H15W···O1W | 0.85 (1) | 2.15 (2) | 2.957 (5) | 158 (6) |
O4W—H16W···O32 | 0.85 (1) | 2.29 (3) | 3.032 (5) | 146 (5) |
O5W—H17W···O3W | 0.85 (1) | 1.89 (2) | 2.717 (5) | 164 (5) |
O5W—H18W···O7W | 0.85 (1) | 2.46 (3) | 3.164 (7) | 140 (4) |
O6W—H19W···O21 | 0.85 (1) | 2.16 (3) | 2.928 (5) | 151 (5) |
O6W—H20W···O2W | 0.85 (1) | 1.99 (3) | 2.772 (5) | 153 (6) |
O7W—H21W···O5W | 0.85 (1) | 2.34 (2) | 3.164 (7) | 163 (7) |
O7W—H22W···N4 | 0.86 (1) | 2.17 (1) | 3.019 (6) | 173 (7) |
O8W—H23W···O6Wiii | 0.85 (1) | 2.55 (12) | 3.025 (10) | 116 (10) |
Symmetry codes: (ii) x, −y+3/2, z−1/2; (iii) −x, −y+2, −z+1; (iv) −x+1, −y+2, −z+1; (v) x+1, −y+3/2, z+1/2; (vi) −x, −y+1, −z+1; (vii) x−1, −y+3/2, z−1/2. |
Experimental details
Crystal data | |
Chemical formula | [K(C12H24O6)(H2O)]2[K(C12H24O6)(H2O)2][FeRh2(C7H5O2)4 (CN)6]·8H2O |
Mr | 2028.66 |
Crystal system, space group | Monoclinic, P21/c |
Temperature (K) | 150 |
a, b, c (Å) | 16.0884 (4), 23.1083 (5), 25.8233 (6) |
β (°) | 104.090 (1) |
V (Å3) | 9311.6 (4) |
Z | 4 |
Radiation type | Mo Kα |
µ (mm−1) | 0.72 |
Crystal size (mm) | 0.25 × 0.15 × 0.14 |
Data collection | |
Diffractometer | Nonius Kappa-CCD |
Absorption correction | Multi-scan (SCALEPACK; Otwinowski & Minor, 1997) |
Tmin, Tmax | 0.840, 0.906 |
No. of measured, independent and observed [I > 2σ(I)] reflections | 75952, 20305, 13576 |
Rint | 0.042 |
(sin θ/λ)max (Å−1) | 0.639 |
Refinement | |
R[F2 > 2σ(F2)], wR(F2), S | 0.053, 0.116, 1.02 |
No. of reflections | 20305 |
No. of parameters | 1156 |
No. of restraints | 64 |
H-atom treatment | H-atom parameters constrained |
Δρmax, Δρmin (e Å−3) | 1.33, −0.69 |
Computer programs: KappaCCD Server Software (Nonius, 1997), DENZO-SMN (Otwinowski & Minor, 1997), DENZO-SMN, SHELXTL (Sheldrick, 1998), SHELXTL.
Rh1—O7 | 2.034 (2) | Fe1—C5 | 1.950 (3) |
Rh1—O5 | 2.038 (2) | O1—C1 | 1.264 (4) |
Rh1—O1 | 2.054 (2) | O2—C1 | 1.268 (4) |
Rh1—O3 | 2.059 (2) | O3—C2 | 1.265 (4) |
Rh1—N1 | 2.207 (3) | O4—C2 | 1.273 (4) |
Rh1—Rh2 | 2.4109 (4) | O5—C3 | 1.270 (4) |
Rh2—O4 | 2.031 (2) | O6—C3 | 1.273 (4) |
Rh2—O2 | 2.032 (2) | O7—C4 | 1.275 (4) |
Rh2—O6 | 2.048 (2) | O8—C4 | 1.267 (4) |
Rh2—O8 | 2.058 (2) | N1—C5 | 1.150 (4) |
Rh2—N6i | 2.200 (3) | N2—C6 | 1.152 (5) |
Fe1—C7 | 1.944 (4) | N3—C7 | 1.161 (4) |
Fe1—C10 | 1.944 (3) | N4—C8 | 1.158 (5) |
Fe1—C8 | 1.944 (4) | N5—C9 | 1.156 (5) |
Fe1—C9 | 1.946 (4) | N6—C10 | 1.148 (4) |
Fe1—C6 | 1.947 (4) | N6—Rh2ii | 2.200 (3) |
O7—Rh1—O5 | 87.05 (10) | C7—Fe1—C10 | 89.76 (14) |
O7—Rh1—O1 | 91.85 (10) | C7—Fe1—C8 | 90.06 (15) |
O5—Rh1—O1 | 175.56 (9) | C10—Fe1—C8 | 90.34 (14) |
O7—Rh1—O3 | 175.69 (9) | C7—Fe1—C9 | 179.26 (15) |
O5—Rh1—O3 | 91.78 (10) | C10—Fe1—C9 | 90.90 (14) |
O1—Rh1—O3 | 89.00 (10) | C8—Fe1—C9 | 89.61 (15) |
O7—Rh1—N1 | 87.84 (10) | C7—Fe1—C6 | 90.89 (15) |
O5—Rh1—N1 | 90.23 (10) | C10—Fe1—C6 | 88.85 (14) |
O1—Rh1—N1 | 94.03 (10) | C8—Fe1—C6 | 178.74 (15) |
O3—Rh1—N1 | 96.32 (9) | C9—Fe1—C6 | 89.44 (15) |
N1—Rh1—Rh2 | 176.38 (8) | C7—Fe1—C5 | 89.54 (13) |
O4—Rh2—O2 | 86.45 (10) | C10—Fe1—C5 | 178.66 (15) |
O4—Rh2—O6 | 91.10 (10) | C8—Fe1—C5 | 90.81 (14) |
O2—Rh2—O6 | 175.17 (9) | C9—Fe1—C5 | 89.81 (14) |
O4—Rh2—O8 | 175.77 (9) | C6—Fe1—C5 | 90.02 (14) |
O2—Rh2—O8 | 93.46 (10) | C10—N6—Rh2ii | 170.7 (3) |
O6—Rh2—O8 | 88.67 (10) | N1—C5—Fe1 | 179.8 (4) |
O4—Rh2—N6i | 88.88 (10) | N2—C6—Fe1 | 177.5 (3) |
O2—Rh2—N6i | 91.12 (10) | N3—C7—Fe1 | 179.4 (3) |
O6—Rh2—N6i | 92.99 (10) | N4—C8—Fe1 | 178.3 (3) |
O8—Rh2—N6i | 95.35 (10) | N5—C9—Fe1 | 179.3 (3) |
N6i—Rh2—Rh1 | 177.71 (8) | N6—C10—Fe1 | 178.7 (3) |
Symmetry codes: (i) x, −y+3/2, z+1/2; (ii) x, −y+3/2, z−1/2. |
D—H···A | D—H | H···A | D···A | D—H···A |
O17—H1W···O6Wiii | 0.851 (5) | 2.104 (10) | 2.728 (5) | 129.8 (10) |
O17—H2W···O12 | 0.855 (5) | 2.364 (16) | 2.829 (4) | 114.6 (12) |
O27—H3W···N3iv | 0.855 (5) | 2.043 (7) | 2.885 (4) | 167.9 (10) |
O27—H4W···O17v | 0.853 (5) | 1.983 (8) | 2.831 (4) | 172 (4) |
O34—H5W···O1Wvi | 0.844 (5) | 2.344 (7) | 3.039 (4) | 140.0 (10) |
O34—H6W···N5vi | 0.847 (5) | 2.213 (7) | 3.040 (5) | 165.5 (11) |
O44—H7W···N5 | 0.851 (5) | 2.160 (15) | 2.909 (5) | 147 (2) |
O44—H8W···O43vii | 0.853 (5) | 2.554 (13) | 3.000 (5) | 113.7 (9) |
O1W—H9W···N2 | 0.852 (5) | 2.214 (10) | 3.051 (4) | 167 (4) |
O1W—H10W···O4ii | 0.852 (5) | 2.284 (13) | 3.104 (4) | 162 (4) |
O2W—H11W···N2 | 0.850 (5) | 2.005 (12) | 2.842 (5) | 168 (5) |
O2W—H12W···O4W | 0.851 (5) | 2.16 (2) | 2.930 (5) | 151 (4) |
O3W—H13W···O7 | 0.848 (5) | 2.25 (2) | 3.014 (4) | 150 (4) |
O3W—H14W···N4 | 0.849 (5) | 2.183 (10) | 3.023 (4) | 171 (5) |
O4W—H15W···O1W | 0.851 (5) | 2.15 (2) | 2.957 (5) | 158 (6) |
O4W—H16W···O32 | 0.852 (5) | 2.29 (3) | 3.032 (5) | 146 (5) |
O5W—H17W···O3W | 0.853 (5) | 1.886 (17) | 2.717 (5) | 164 (5) |
O5W—H18W···O7W | 0.853 (5) | 2.46 (3) | 3.164 (7) | 140 (4) |
O6W—H19W···O21 | 0.849 (5) | 2.16 (3) | 2.928 (5) | 151 (5) |
O6W—H20W···O2W | 0.851 (5) | 1.99 (3) | 2.772 (5) | 153 (6) |
O7W—H21W···O5W | 0.854 (5) | 2.34 (2) | 3.164 (7) | 163 (7) |
O7W—H22W···N4 | 0.855 (5) | 2.170 (13) | 3.019 (6) | 173 (7) |
O8W—H23W···O6Wvi | 0.854 (5) | 2.55 (12) | 3.025 (10) | 116 (10) |
Symmetry codes: (ii) x, −y+3/2, z−1/2; (iii) x+1, −y+3/2, z+1/2; (iv) −x, −y+1, −z+1; (v) x−1, −y+3/2, z−1/2; (vi) −x, −y+2, −z+1; (vii) −x+1, −y+2, −z+1. |
Metal cyanide compounds have been used to synthesize coordination polymers (Ward, 1995; Vahrenkamp et al., 1997, and references therein). Hexacyanometallate ions [M(CN)]n- can provide one- (Colacio et al., 2000), two- (Miyasaka et al., 1997) and three-dimensional polymers (Miyasaka et al., 1998a,b; Langenberg et al., 1997) since cyano groups are directed to all three axes. Dirhodium acetate units are connected by Co(CN)63- to form a two-dimensional sheet (Lu et al., 1996). It was the first example for dimetal units to be connected by a metal cyanide. Diruthenium units are also bridged by Co(CN)63- to form a pentanuclear complex (Kim et al., 1998).
Ferric cyanide can also be used as a metal cyanide to connect dimetal units to form one-, two-, or three-dimensional compounds. Only the potassium salt among the ferric cyanides is water-soluble. 18-Crown-6-ether can help increase the solubility of a ferric cyanide (Miyasaka et al., 1998a).
Only trans-cyano groups of the ferric cyanide connect dirhodium units to form an one-dimensional chain compound. The Rh—Rh distance is 2.4109 (4) Å which is a little longer than the typical Rh—Rh distance in tetracarboxylatodirhodium(II,II) complexes. Rh—N(bridging cyano group) distances are 2.208 (3) and 2.200 (3) Å. The chain is not linear with angles of 168.1 (3) and 170.7 (3)° for C5—N1—Rh1 and C10—N6—Rh2ii (ii = x, 3/2 - y, z - 1/2), repectively. The benzoate groups of a dirhodium unit are staggered with those of the next dirhodium unit, and also twisted to the four Fe—CN bonds. The Fe—CN bonds of a ferric cyanide are eclipsed with those bonds of the next ferric cyanide. Actually, the ferric cyanide has the possibility to make three-dimensional network structures since all six cyano groups can connect some complex units. However, a benzoate bridging ligand of a dirhodium complex is too bulky to make a two- or three-dimensional compound. Potassium cations encapsulated by crownether are located between anion chains. Two K atoms K1 and K2 are on general positions whereas K3 and K4 are on inversion centres. The asymmetric unit therefore contains 3 crownether molecules. Each K1 and K2 has a water molecule on the one axial site and the other axial site interact with the phenyl group of the benzoate bridging ligand. K3 and K4 have water molecules on both axial sites since it has an inversion centre on the K atom. There are hydrogen bondings between hydrogen atoms of water molecules bonded to the potassium, K3 and K4, and nitrogen atoms, N2, N3, N4 and N5 of free cyano groups.