Buy article online - an online subscription or single-article purchase is required to access this article.
Eight new structures of dirhodium complexes, each with four biimidazole (H2bim) ligands, were obtained: [Rh2(H2bim)4(H2O)2](NO3)4·4H2O (I), [Rh2(H2bim)4(H2O)2](ClO4)4·5H2O (II), [Rh2(H2bim)4(MeOH)2](ClO4)4 (III), [Rh2(H2bim)4(DMF)2](BF4)4 (IV), [Rh2(H2bim)4(Mepy)2](SiF6)2·8H2O (V), [{Rh2(H2bim)4(pz)}2(μ-pz)](SiF6)(ClO4)6·12.7H2O (VI), [{Rh2(H2bim)4(pz)}2(μ-pz)](ClO4)8·11.4H2O (VII) and [Rh2(H2bim)4(μ-pz)](SiF6)2·6H2O (VIII). The unbridged Rh—Rh bond distances range between 2.6313 (8) and 2.7052 (5) Å. The dirhodium units adopt a staggered conformation with torsion angles N—Rh—Rh—N of 37.6 (4)–48.98 (8)°. Various assembled structures were constructed by hydrogen bonding between the complexes and the anions: a discrete structure in (IV), one-dimensional structure in (II), two-dimensional structures in (I), (III), (VI), (VII) and (VIII) and a three-dimensional structure in (V).
Supporting information
CCDC references: 1026431; 1026432; 1026433; 1026434; 1026435; 1026436; 1026437; 1026438
Crystal data, data collection and structure refinement details are summarized in Table 1.
S2. Results and discussion
top
For all compounds, data collection: CrystalClear (Molecular Structure Corporation & Rigaku Corporation, 2001); cell refinement: CrystalClear; data reduction: CrystalClear; program(s) used to solve structure: SIR97 (Altomare et al., 1999); program(s) used to refine structure: SHELXL97 (Sheldrick, 2008); molecular graphics: Mercury (Macrae et al., 2008); software used to prepare material for publication: Yadokari-XG 2009 (Wakita, Nemoto et al., 2009).
Crystal data top
C24H28N16O2Rh2·4(NO3)·4(H2O) | Dx = 1.891 Mg m−3 |
Mr = 1098.55 | Mo Kα radiation, λ = 0.71069 Å |
Orthorhombic, Pbcn | Cell parameters from 9401 reflections |
a = 18.843 (3) Å | θ = 3.0–27.5° |
b = 16.642 (3) Å | µ = 0.96 mm−1 |
c = 12.307 (2) Å | T = 123 K |
V = 3859.2 (11) Å3 | Prismatic, green |
Z = 4 | 0.66 × 0.12 × 0.10 mm |
F(000) = 2216 | |
Data collection top
Rigaku/MSC Mercury CCD diffractometer | 4413 independent reflections |
Radiation source: rotating-anode X-ray tube | 4134 reflections with I > 2σ(I) |
Graphite monochromator | Rint = 0.042 |
Detector resolution: 14.62 pixels mm-1 | θmax = 27.5°, θmin = 3.2° |
ω scans | h = −24→17 |
Absorption correction: numerical NUMABS (Higashi, 1999) | k = −21→19 |
Tmin = 0.809, Tmax = 0.956 | l = −15→11 |
29049 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)] = 0.044 | Hydrogen site location: inferred from neighbouring sites |
wR(F2) = 0.080 | H atoms treated by a mixture of independent and constrained refinement |
S = 1.32 | w = 1/[σ2(Fo2) + (0.0208P)2 + 3.7755P] where P = (Fo2 + 2Fc2)/3 |
4416 reflections | (Δ/σ)max = 0.001 |
313 parameters | Δρmax = 0.79 e Å−3 |
0 restraints | Δρmin = −0.57 e Å−3 |
Crystal data top
C24H28N16O2Rh2·4(NO3)·4(H2O) | V = 3859.2 (11) Å3 |
Mr = 1098.55 | Z = 4 |
Orthorhombic, Pbcn | Mo Kα radiation |
a = 18.843 (3) Å | µ = 0.96 mm−1 |
b = 16.642 (3) Å | T = 123 K |
c = 12.307 (2) Å | 0.66 × 0.12 × 0.10 mm |
Data collection top
Rigaku/MSC Mercury CCD diffractometer | 4413 independent reflections |
Absorption correction: numerical NUMABS (Higashi, 1999) | 4134 reflections with I > 2σ(I) |
Tmin = 0.809, Tmax = 0.956 | Rint = 0.042 |
29049 measured reflections | |
Refinement top
R[F2 > 2σ(F2)] = 0.044 | 0 restraints |
wR(F2) = 0.080 | H atoms treated by a mixture of independent and constrained refinement |
S = 1.32 | Δρmax = 0.79 e Å−3 |
4416 reflections | Δρmin = −0.57 e Å−3 |
313 parameters | |
Special details top
Geometry. All e.s.d.'s (except the e.s.d. in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell e.s.d.'s are taken into account individually in the estimation of e.s.d.'s in distances, angles and torsion angles; correlations between e.s.d.'s in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell e.s.d.'s is used for estimating e.s.d.'s involving l.s. planes. |
Refinement. Refinement of F2 against ALL reflections. The weighted R-factor wR and goodness of fit S are based on F2, conventional R-factors R are based on F, with F set to zero for negative F2. The threshold expression of F2 > σ(F2) is used only for calculating R-factors(gt) etc. and is not relevant to the choice of reflections for refinement. R-factors based on F2 are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger. |
Fractional atomic coordinates and isotropic or equivalent isotropic displacement parameters (Å2) top | x | y | z | Uiso*/Ueq | |
Rh1 | 0.496293 (11) | 0.284327 (13) | 0.641384 (16) | 0.01116 (7) | |
N1 | 0.59822 (13) | 0.32611 (15) | 0.62505 (18) | 0.0135 (5) | |
C1 | 0.64592 (15) | 0.26794 (19) | 0.6126 (2) | 0.0150 (6) | |
N2 | 0.71109 (13) | 0.29788 (15) | 0.59918 (19) | 0.0171 (5) | |
H2N | 0.7504 | 0.2701 | 0.5908 | 0.021* | |
C2 | 0.70526 (16) | 0.38076 (19) | 0.6009 (2) | 0.0195 (6) | |
H2 | 0.7426 | 0.4186 | 0.5927 | 0.023* | |
C3 | 0.63508 (16) | 0.39728 (18) | 0.6166 (2) | 0.0161 (6) | |
H3 | 0.6149 | 0.4495 | 0.6211 | 0.019* | |
N3 | 0.55025 (13) | 0.17784 (15) | 0.63014 (18) | 0.0140 (5) | |
C4 | 0.61985 (16) | 0.18639 (19) | 0.6143 (2) | 0.0151 (6) | |
N4 | 0.65146 (14) | 0.11611 (16) | 0.59794 (19) | 0.0189 (6) | |
H4N | 0.6969 | 0.1083 | 0.5852 | 0.023* | |
C5 | 0.60030 (17) | 0.0581 (2) | 0.6046 (2) | 0.0216 (7) | |
H5 | 0.6070 | 0.0018 | 0.5968 | 0.026* | |
C6 | 0.53747 (17) | 0.09677 (19) | 0.6246 (2) | 0.0186 (6) | |
H6 | 0.4926 | 0.0717 | 0.6333 | 0.022* | |
N5 | 0.44123 (13) | 0.39047 (15) | 0.64183 (17) | 0.0134 (5) | |
C7 | 0.37062 (15) | 0.38177 (19) | 0.6380 (2) | 0.0151 (6) | |
N6 | 0.33816 (14) | 0.45272 (16) | 0.63229 (18) | 0.0183 (5) | |
H6N | 0.2921 | 0.4608 | 0.6291 | 0.022* | |
C8 | 0.38953 (17) | 0.5106 (2) | 0.6324 (2) | 0.0197 (6) | |
H8 | 0.3823 | 0.5670 | 0.6294 | 0.024* | |
C9 | 0.45320 (17) | 0.47192 (19) | 0.6375 (2) | 0.0176 (6) | |
H9 | 0.4984 | 0.4971 | 0.6380 | 0.021* | |
N7 | 0.39421 (13) | 0.24234 (15) | 0.64234 (18) | 0.0138 (5) | |
C10 | 0.34518 (16) | 0.30002 (19) | 0.6403 (2) | 0.0156 (6) | |
N8 | 0.27952 (13) | 0.26823 (17) | 0.63876 (19) | 0.0194 (6) | |
H8N | 0.2392 | 0.2950 | 0.6377 | 0.023* | |
C11 | 0.28727 (17) | 0.1858 (2) | 0.6392 (2) | 0.0205 (7) | |
H11 | 0.2501 | 0.1471 | 0.6388 | 0.025* | |
C12 | 0.35840 (16) | 0.17020 (19) | 0.6402 (2) | 0.0170 (6) | |
H12 | 0.3796 | 0.1184 | 0.6394 | 0.020* | |
O1 | 0.49336 (12) | 0.28149 (15) | 0.45463 (17) | 0.0175 (4) | |
H1A | 0.465 (2) | 0.316 (3) | 0.433 (3) | 0.045 (13)* | |
H1B | 0.4778 (19) | 0.241 (2) | 0.436 (3) | 0.020 (10)* | |
N9 | 0.84385 (14) | 0.12376 (17) | 0.61933 (19) | 0.0211 (6) | |
O2 | 0.83313 (13) | 0.19829 (15) | 0.61922 (19) | 0.0303 (6) | |
O3 | 0.79334 (13) | 0.07548 (17) | 0.6175 (2) | 0.0383 (6) | |
O4 | 0.90598 (11) | 0.09783 (14) | 0.62123 (17) | 0.0235 (5) | |
N10 | 0.14816 (15) | 0.44192 (18) | 0.6615 (2) | 0.0246 (6) | |
O5 | 0.19275 (12) | 0.48324 (16) | 0.61076 (19) | 0.0310 (6) | |
O6 | 0.16805 (15) | 0.38192 (16) | 0.7156 (2) | 0.0397 (7) | |
O7 | 0.08408 (13) | 0.46105 (16) | 0.65985 (19) | 0.0312 (6) | |
O8 | 0.12766 (14) | 0.21130 (17) | 0.6437 (2) | 0.0309 (6) | |
H8A | 0.088 (3) | 0.216 (3) | 0.618 (4) | 0.072 (18)* | |
H8B | 0.117 (3) | 0.227 (3) | 0.709 (4) | 0.070 (17)* | |
O9 | 0.45282 (18) | 0.13651 (18) | 0.3771 (2) | 0.0390 (7) | |
H9A | 0.495 (3) | 0.116 (4) | 0.358 (4) | 0.10 (3)* | |
H9B | 0.423 (3) | 0.130 (3) | 0.327 (4) | 0.073 (18)* | |
Atomic displacement parameters (Å2) top | U11 | U22 | U33 | U12 | U13 | U23 |
Rh1 | 0.00905 (12) | 0.01098 (12) | 0.01346 (11) | 0.00023 (8) | −0.00001 (8) | −0.00033 (8) |
N1 | 0.0118 (12) | 0.0141 (13) | 0.0145 (11) | 0.0007 (10) | −0.0005 (9) | −0.0008 (9) |
C1 | 0.0121 (14) | 0.0179 (16) | 0.0149 (13) | 0.0021 (12) | 0.0004 (10) | 0.0017 (11) |
N2 | 0.0122 (13) | 0.0193 (15) | 0.0197 (12) | −0.0003 (11) | 0.0018 (9) | −0.0020 (10) |
C2 | 0.0152 (15) | 0.0201 (17) | 0.0231 (15) | −0.0038 (13) | 0.0015 (12) | 0.0006 (12) |
C3 | 0.0186 (15) | 0.0128 (16) | 0.0167 (14) | −0.0022 (12) | −0.0007 (11) | 0.0016 (11) |
N3 | 0.0129 (12) | 0.0121 (13) | 0.0171 (11) | 0.0009 (10) | −0.0003 (9) | −0.0012 (9) |
C4 | 0.0135 (15) | 0.0170 (16) | 0.0148 (13) | 0.0028 (12) | 0.0008 (11) | −0.0021 (11) |
N4 | 0.0133 (13) | 0.0190 (15) | 0.0245 (13) | 0.0042 (11) | 0.0033 (10) | −0.0016 (10) |
C5 | 0.0226 (17) | 0.0136 (16) | 0.0286 (16) | −0.0007 (13) | 0.0040 (12) | −0.0003 (12) |
C6 | 0.0179 (16) | 0.0150 (16) | 0.0229 (15) | −0.0003 (12) | 0.0019 (12) | 0.0014 (12) |
N5 | 0.0128 (12) | 0.0138 (13) | 0.0136 (11) | 0.0012 (10) | −0.0006 (9) | −0.0006 (9) |
C7 | 0.0124 (14) | 0.0219 (17) | 0.0109 (12) | 0.0012 (12) | −0.0014 (10) | −0.0001 (11) |
N6 | 0.0164 (13) | 0.0192 (14) | 0.0191 (12) | 0.0054 (11) | 0.0005 (10) | 0.0016 (10) |
C8 | 0.0232 (17) | 0.0161 (17) | 0.0198 (14) | 0.0023 (13) | −0.0004 (12) | 0.0006 (12) |
C9 | 0.0199 (16) | 0.0154 (16) | 0.0175 (13) | −0.0016 (12) | −0.0013 (11) | −0.0004 (12) |
N7 | 0.0115 (12) | 0.0147 (13) | 0.0154 (11) | −0.0013 (10) | −0.0010 (9) | −0.0010 (9) |
C10 | 0.0124 (14) | 0.0219 (17) | 0.0124 (13) | 0.0015 (12) | −0.0010 (10) | −0.0004 (11) |
N8 | 0.0106 (12) | 0.0265 (16) | 0.0211 (13) | 0.0000 (11) | −0.0023 (10) | 0.0012 (11) |
C11 | 0.0177 (16) | 0.0230 (18) | 0.0209 (15) | −0.0061 (13) | −0.0037 (12) | 0.0008 (12) |
C12 | 0.0185 (16) | 0.0135 (16) | 0.0189 (14) | −0.0038 (12) | −0.0006 (11) | −0.0009 (12) |
O1 | 0.0188 (12) | 0.0146 (12) | 0.0191 (10) | −0.0006 (11) | −0.0034 (8) | −0.0023 (9) |
N9 | 0.0189 (14) | 0.0251 (16) | 0.0192 (13) | 0.0056 (12) | 0.0019 (10) | 0.0018 (11) |
O2 | 0.0278 (14) | 0.0243 (14) | 0.0387 (14) | 0.0104 (11) | 0.0004 (10) | 0.0032 (10) |
O3 | 0.0166 (13) | 0.0301 (16) | 0.0682 (18) | 0.0006 (11) | 0.0009 (12) | 0.0007 (13) |
O4 | 0.0130 (11) | 0.0236 (13) | 0.0339 (12) | 0.0050 (9) | 0.0020 (9) | 0.0058 (10) |
N10 | 0.0187 (15) | 0.0254 (16) | 0.0297 (14) | 0.0028 (12) | −0.0048 (11) | −0.0067 (12) |
O5 | 0.0195 (13) | 0.0347 (16) | 0.0390 (14) | 0.0026 (11) | −0.0030 (10) | −0.0006 (11) |
O6 | 0.0371 (16) | 0.0309 (16) | 0.0512 (15) | 0.0140 (13) | −0.0038 (12) | 0.0083 (12) |
O7 | 0.0176 (12) | 0.0341 (15) | 0.0419 (14) | 0.0075 (11) | −0.0006 (10) | −0.0036 (11) |
O8 | 0.0206 (14) | 0.0416 (17) | 0.0306 (14) | 0.0014 (12) | −0.0053 (11) | −0.0027 (12) |
O9 | 0.0394 (18) | 0.0331 (17) | 0.0445 (16) | −0.0040 (14) | −0.0044 (14) | −0.0108 (13) |
Geometric parameters (Å, º) top
Rh1—N7 | 2.047 (2) | C7—C10 | 1.443 (4) |
Rh1—N3 | 2.048 (2) | N6—C8 | 1.365 (4) |
Rh1—N5 | 2.049 (2) | N6—H6N | 0.8800 |
Rh1—N1 | 2.053 (2) | C8—C9 | 1.363 (4) |
Rh1—O1 | 2.299 (2) | C8—H8 | 0.9500 |
Rh1—Rh1i | 2.6771 (6) | C9—H9 | 0.9500 |
N1—C1 | 1.330 (4) | N7—C10 | 1.333 (4) |
N1—C3 | 1.377 (4) | N7—C12 | 1.377 (4) |
C1—N2 | 1.336 (4) | C10—N8 | 1.346 (4) |
C1—C4 | 1.443 (4) | N8—C11 | 1.380 (4) |
N2—C2 | 1.384 (4) | N8—H8N | 0.8800 |
N2—H2N | 0.8800 | C11—C12 | 1.365 (4) |
C2—C3 | 1.365 (4) | C11—H11 | 0.9500 |
C2—H2 | 0.9500 | C12—H12 | 0.9500 |
C3—H3 | 0.9500 | O1—H1A | 0.83 (5) |
N3—C4 | 1.333 (4) | O1—H1B | 0.78 (4) |
N3—C6 | 1.372 (4) | N9—O3 | 1.246 (4) |
C4—N4 | 1.328 (4) | N9—O4 | 1.248 (3) |
N4—C5 | 1.367 (4) | N9—O2 | 1.257 (4) |
N4—H4N | 0.8800 | N10—O7 | 1.249 (3) |
C5—C6 | 1.370 (4) | N10—O5 | 1.253 (4) |
C5—H5 | 0.9500 | N10—O6 | 1.257 (4) |
C6—H6 | 0.9500 | O8—H8A | 0.81 (6) |
N5—C7 | 1.339 (4) | O8—H8B | 0.87 (5) |
N5—C9 | 1.375 (4) | O9—H9A | 0.90 (6) |
C7—N6 | 1.332 (4) | O9—H9B | 0.83 (5) |
| | | |
N7—Rh1—N3 | 99.88 (10) | C5—C6—H6 | 125.7 |
N7—Rh1—N5 | 79.53 (10) | N3—C6—H6 | 125.7 |
N3—Rh1—N5 | 176.24 (9) | C7—N5—C9 | 105.6 (3) |
N7—Rh1—N1 | 174.71 (9) | C7—N5—Rh1 | 114.2 (2) |
N3—Rh1—N1 | 79.74 (10) | C9—N5—Rh1 | 140.1 (2) |
N5—Rh1—N1 | 100.49 (10) | N6—C7—N5 | 111.2 (3) |
N7—Rh1—O1 | 88.63 (8) | N6—C7—C10 | 133.2 (3) |
N3—Rh1—O1 | 85.80 (9) | N5—C7—C10 | 115.6 (3) |
N5—Rh1—O1 | 90.47 (9) | C7—N6—C8 | 107.4 (3) |
N1—Rh1—O1 | 86.07 (8) | C7—N6—H6N | 126.3 |
N7—Rh1—Rh1i | 92.48 (6) | C8—N6—H6N | 126.3 |
N3—Rh1—Rh1i | 92.38 (6) | C9—C8—N6 | 107.0 (3) |
N5—Rh1—Rh1i | 91.36 (6) | C9—C8—H8 | 126.5 |
N1—Rh1—Rh1i | 92.81 (6) | N6—C8—H8 | 126.5 |
O1—Rh1—Rh1i | 178.00 (6) | C8—C9—N5 | 108.8 (3) |
C1—N1—C3 | 106.1 (2) | C8—C9—H9 | 125.6 |
C1—N1—Rh1 | 113.4 (2) | N5—C9—H9 | 125.6 |
C3—N1—Rh1 | 140.4 (2) | C10—N7—C12 | 106.7 (2) |
N1—C1—N2 | 111.4 (3) | C10—N7—Rh1 | 113.9 (2) |
N1—C1—C4 | 116.9 (3) | C12—N7—Rh1 | 139.3 (2) |
N2—C1—C4 | 131.7 (3) | N7—C10—N8 | 110.8 (3) |
C1—N2—C2 | 107.3 (3) | N7—C10—C7 | 116.7 (3) |
C1—N2—H2N | 126.4 | N8—C10—C7 | 132.5 (3) |
C2—N2—H2N | 126.4 | C10—N8—C11 | 107.1 (3) |
C3—C2—N2 | 106.2 (3) | C10—N8—H8N | 126.5 |
C3—C2—H2 | 126.9 | C11—N8—H8N | 126.5 |
N2—C2—H2 | 126.9 | C12—C11—N8 | 107.0 (3) |
C2—C3—N1 | 109.0 (3) | C12—C11—H11 | 126.5 |
C2—C3—H3 | 125.5 | N8—C11—H11 | 126.5 |
N1—C3—H3 | 125.5 | C11—C12—N7 | 108.4 (3) |
C4—N3—C6 | 105.7 (3) | C11—C12—H12 | 125.8 |
C4—N3—Rh1 | 113.9 (2) | N7—C12—H12 | 125.8 |
C6—N3—Rh1 | 140.1 (2) | Rh1—O1—H1A | 109 (3) |
N4—C4—N3 | 111.7 (3) | Rh1—O1—H1B | 109 (3) |
N4—C4—C1 | 132.3 (3) | H1A—O1—H1B | 105 (4) |
N3—C4—C1 | 115.9 (3) | O3—N9—O4 | 119.6 (3) |
C4—N4—C5 | 107.3 (3) | O3—N9—O2 | 120.9 (3) |
C4—N4—H4N | 126.4 | O4—N9—O2 | 119.5 (3) |
C5—N4—H4N | 126.4 | O7—N10—O5 | 120.0 (3) |
N4—C5—C6 | 106.8 (3) | O7—N10—O6 | 120.0 (3) |
N4—C5—H5 | 126.6 | O5—N10—O6 | 120.0 (3) |
C6—C5—H5 | 126.6 | H8A—O8—H8B | 97 (4) |
C5—C6—N3 | 108.6 (3) | H9A—O9—H9B | 110 (5) |
| | | |
N1—Rh1—Rh1i—N5i | 39.77 (10) | Rh1—N3—C6—C5 | 172.7 (2) |
N3—Rh1—Rh1i—N7i | 40.03 (10) | N7—Rh1—N5—C7 | −2.58 (18) |
N7—Rh1—N1—C1 | −84.5 (11) | N3—Rh1—N5—C7 | 78.8 (15) |
N3—Rh1—N1—C1 | 1.87 (18) | N1—Rh1—N5—C7 | 172.04 (18) |
N5—Rh1—N1—C1 | −174.31 (18) | O1—Rh1—N5—C7 | 85.94 (19) |
O1—Rh1—N1—C1 | −84.56 (19) | Rh1i—Rh1—N5—C7 | −94.85 (18) |
Rh1i—Rh1—N1—C1 | 93.79 (18) | N7—Rh1—N5—C9 | −176.7 (3) |
N7—Rh1—N1—C3 | 90.7 (11) | N3—Rh1—N5—C9 | −95.3 (15) |
N3—Rh1—N1—C3 | 177.1 (3) | N1—Rh1—N5—C9 | −2.0 (3) |
N5—Rh1—N1—C3 | 0.9 (3) | O1—Rh1—N5—C9 | −88.1 (3) |
O1—Rh1—N1—C3 | 90.7 (3) | Rh1i—Rh1—N5—C9 | 91.1 (3) |
Rh1i—Rh1—N1—C3 | −91.0 (3) | C9—N5—C7—N6 | −0.4 (3) |
C3—N1—C1—N2 | 1.4 (3) | Rh1—N5—C7—N6 | −176.45 (17) |
Rh1—N1—C1—N2 | 178.23 (18) | C9—N5—C7—C10 | 179.3 (2) |
C3—N1—C1—C4 | −177.9 (2) | Rh1—N5—C7—C10 | 3.3 (3) |
Rh1—N1—C1—C4 | −1.1 (3) | N5—C7—N6—C8 | 0.0 (3) |
N1—C1—N2—C2 | −1.3 (3) | C10—C7—N6—C8 | −179.7 (3) |
C4—C1—N2—C2 | 177.9 (3) | C7—N6—C8—C9 | 0.4 (3) |
C1—N2—C2—C3 | 0.6 (3) | N6—C8—C9—N5 | −0.7 (3) |
N2—C2—C3—N1 | 0.3 (3) | C7—N5—C9—C8 | 0.7 (3) |
C1—N1—C3—C2 | −1.0 (3) | Rh1—N5—C9—C8 | 175.0 (2) |
Rh1—N1—C3—C2 | −176.4 (2) | N3—Rh1—N7—C10 | −174.82 (19) |
N7—Rh1—N3—C4 | 172.17 (19) | N5—Rh1—N7—C10 | 1.40 (18) |
N5—Rh1—N3—C4 | 91.4 (15) | N1—Rh1—N7—C10 | −89.4 (11) |
N1—Rh1—N3—C4 | −2.47 (19) | O1—Rh1—N7—C10 | −89.33 (19) |
O1—Rh1—N3—C4 | 84.29 (19) | Rh1i—Rh1—N7—C10 | 92.33 (18) |
Rh1i—Rh1—N3—C4 | −94.90 (19) | N3—Rh1—N7—C12 | 1.8 (3) |
N7—Rh1—N3—C6 | −0.6 (3) | N5—Rh1—N7—C12 | 178.0 (3) |
N5—Rh1—N3—C6 | −81.3 (15) | N1—Rh1—N7—C12 | 87.2 (11) |
N1—Rh1—N3—C6 | −175.2 (3) | O1—Rh1—N7—C12 | 87.3 (3) |
O1—Rh1—N3—C6 | −88.4 (3) | Rh1i—Rh1—N7—C12 | −91.1 (3) |
Rh1i—Rh1—N3—C6 | 92.4 (3) | C12—N7—C10—N8 | 1.0 (3) |
C6—N3—C4—N4 | 0.7 (3) | Rh1—N7—C10—N8 | 178.68 (17) |
Rh1—N3—C4—N4 | −174.43 (18) | C12—N7—C10—C7 | −177.8 (2) |
C6—N3—C4—C1 | 177.8 (2) | Rh1—N7—C10—C7 | −0.1 (3) |
Rh1—N3—C4—C1 | 2.7 (3) | N6—C7—C10—N7 | 177.5 (3) |
N1—C1—C4—N4 | 175.3 (3) | N5—C7—C10—N7 | −2.2 (4) |
N2—C1—C4—N4 | −3.8 (5) | N6—C7—C10—N8 | −0.9 (5) |
N1—C1—C4—N3 | −1.1 (4) | N5—C7—C10—N8 | 179.4 (3) |
N2—C1—C4—N3 | 179.8 (3) | N7—C10—N8—C11 | −0.3 (3) |
N3—C4—N4—C5 | −0.7 (3) | C7—C10—N8—C11 | 178.2 (3) |
C1—C4—N4—C5 | −177.2 (3) | C10—N8—C11—C12 | −0.5 (3) |
C4—N4—C5—C6 | 0.4 (3) | N8—C11—C12—N7 | 1.1 (3) |
N4—C5—C6—N3 | 0.0 (3) | C10—N7—C12—C11 | −1.3 (3) |
C4—N3—C6—C5 | −0.5 (3) | Rh1—N7—C12—C11 | −178.0 (2) |
Symmetry code: (i) −x+1, y, −z+3/2. |
Hydrogen-bond geometry (Å, º) top
D—H···A | D—H | H···A | D···A | D—H···A |
N2—H2N···O2 | 0.88 | 1.99 | 2.845 (3) | 162 |
N4—H4N···O3 | 0.88 | 1.94 | 2.768 (4) | 157 |
N6—H6N···O5 | 0.88 | 1.92 | 2.799 (4) | 175 |
N8—H8N···O6 | 0.88 | 2.19 | 2.981 (4) | 149 |
N8—H8N···O8 | 0.88 | 2.52 | 3.015 (4) | 116 |
O1—H1A···N9ii | 0.83 (5) | 2.57 (5) | 3.354 (4) | 158 (4) |
O1—H1A···O2ii | 0.83 (5) | 2.57 (4) | 3.171 (3) | 130 (4) |
O1—H1A···O4ii | 0.83 (5) | 1.93 (5) | 2.760 (3) | 174 (4) |
O1—H1B···O9 | 0.78 (4) | 1.93 (4) | 2.705 (4) | 171 (4) |
O8—H8A···O1ii | 0.81 (6) | 2.00 (6) | 2.808 (3) | 174 (5) |
O8—H8B···O2i | 0.87 (5) | 2.36 (5) | 3.017 (4) | 133 (4) |
O9—H9A···O7iii | 0.90 (6) | 2.12 (7) | 2.993 (4) | 164 (6) |
O9—H9B···O6iv | 0.83 (5) | 2.21 (6) | 3.038 (4) | 170 (5) |
O9—H9B···O7iv | 0.83 (5) | 2.56 (5) | 3.204 (4) | 135 (5) |
Symmetry codes: (i) −x+1, y, −z+3/2; (ii) x−1/2, −y+1/2, −z+1; (iii) x+1/2, −y+1/2, −z+1; (iv) −x+1/2, −y+1/2, z−1/2. |
Crystal data top
C24H28N16O2Rh2·4(ClO4)·5(H2O) | F(000) = 2544 |
Mr = 1266.32 | Dx = 1.884 Mg m−3 |
Monoclinic, P21/n | Mo Kα radiation, λ = 0.71069 Å |
a = 13.453 (2) Å | Cell parameters from 11005 reflections |
b = 13.334 (2) Å | θ = 3.0–27.5° |
c = 24.906 (4) Å | µ = 1.08 mm−1 |
β = 91.749 (2)° | T = 296 K |
V = 4465.5 (13) Å3 | Prismatic, green |
Z = 4 | 0.41 × 0.35 × 0.34 mm |
Data collection top
Rigaku/MSC Mercury CCD diffractometer | 10190 independent reflections |
Radiation source: rotating-anode X-ray tube | 8188 reflections with I > 2σ(I) |
Graphite monochromator | Rint = 0.034 |
Detector resolution: 14.62 pixels mm-1 | θmax = 27.5°, θmin = 3.0° |
ω scans | h = −17→16 |
Absorption correction: numerical NUMABS (Higashi, 1999) | k = −14→17 |
Tmin = 0.731, Tmax = 0.815 | l = −32→31 |
34616 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)] = 0.058 | Hydrogen site location: inferred from neighbouring sites |
wR(F2) = 0.163 | H atoms treated by a mixture of independent and constrained refinement |
S = 1.08 | w = 1/[σ2(Fo2) + (0.0753P)2 + 6.5586P] where P = (Fo2 + 2Fc2)/3 |
10190 reflections | (Δ/σ)max = 0.001 |
641 parameters | Δρmax = 0.78 e Å−3 |
0 restraints | Δρmin = −0.74 e Å−3 |
Crystal data top
C24H28N16O2Rh2·4(ClO4)·5(H2O) | V = 4465.5 (13) Å3 |
Mr = 1266.32 | Z = 4 |
Monoclinic, P21/n | Mo Kα radiation |
a = 13.453 (2) Å | µ = 1.08 mm−1 |
b = 13.334 (2) Å | T = 296 K |
c = 24.906 (4) Å | 0.41 × 0.35 × 0.34 mm |
β = 91.749 (2)° | |
Data collection top
Rigaku/MSC Mercury CCD diffractometer | 10190 independent reflections |
Absorption correction: numerical NUMABS (Higashi, 1999) | 8188 reflections with I > 2σ(I) |
Tmin = 0.731, Tmax = 0.815 | Rint = 0.034 |
34616 measured reflections | |
Refinement top
R[F2 > 2σ(F2)] = 0.058 | 0 restraints |
wR(F2) = 0.163 | H atoms treated by a mixture of independent and constrained refinement |
S = 1.08 | Δρmax = 0.78 e Å−3 |
10190 reflections | Δρmin = −0.74 e Å−3 |
641 parameters | |
Special details top
Geometry. All e.s.d.'s (except the e.s.d. in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell e.s.d.'s are taken into account individually in the estimation of e.s.d.'s in distances, angles and torsion angles; correlations between e.s.d.'s in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell e.s.d.'s is used for estimating e.s.d.'s involving l.s. planes. |
Refinement. Refinement of F2 against ALL reflections. The weighted R-factor wR and goodness of fit S are based on F2, conventional R-factors R are based on F, with F set to zero for negative F2. The threshold expression of F2 > σ(F2) is used only for calculating R-factors(gt) etc. and is not relevant to the choice of reflections for refinement. R-factors based on F2 are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger. |
Fractional atomic coordinates and isotropic or equivalent isotropic displacement parameters (Å2) top | x | y | z | Uiso*/Ueq | Occ. (<1) |
Rh1 | 0.53955 (2) | 0.26880 (3) | 0.600046 (13) | 0.03340 (11) | |
Rh2 | 0.69975 (2) | 0.26866 (3) | 0.664573 (14) | 0.03684 (12) | |
N1 | 0.4434 (3) | 0.2821 (3) | 0.66190 (15) | 0.0390 (8) | |
C1 | 0.4049 (3) | 0.1948 (4) | 0.6768 (2) | 0.0447 (10) | |
N2 | 0.3366 (3) | 0.2092 (4) | 0.7139 (2) | 0.0639 (13) | |
H2N | 0.3023 | 0.1631 | 0.7287 | 0.077* | |
C2 | 0.3304 (4) | 0.3090 (5) | 0.7241 (3) | 0.0698 (17) | |
H2 | 0.2892 | 0.3401 | 0.7484 | 0.084* | |
C3 | 0.3976 (4) | 0.3550 (4) | 0.6912 (2) | 0.0536 (12) | |
H3 | 0.4097 | 0.4235 | 0.6893 | 0.064* | |
N3 | 0.5097 (3) | 0.1203 (3) | 0.61424 (15) | 0.0396 (8) | |
C4 | 0.4409 (3) | 0.1066 (4) | 0.6505 (2) | 0.0442 (10) | |
N4 | 0.4204 (3) | 0.0088 (3) | 0.65627 (19) | 0.0543 (11) | |
H4N | 0.3783 | −0.0167 | 0.6777 | 0.065* | |
C5 | 0.4781 (4) | −0.0421 (4) | 0.6223 (2) | 0.0582 (13) | |
H5 | 0.4799 | −0.1113 | 0.6178 | 0.070* | |
C6 | 0.5336 (4) | 0.0268 (4) | 0.5956 (2) | 0.0506 (12) | |
H6 | 0.5794 | 0.0128 | 0.5695 | 0.061* | |
N5 | 0.5593 (2) | 0.4171 (3) | 0.58141 (14) | 0.0364 (8) | |
C7 | 0.6056 (3) | 0.4311 (3) | 0.53579 (18) | 0.0385 (9) | |
N6 | 0.6104 (3) | 0.5293 (3) | 0.52416 (16) | 0.0436 (9) | |
H6N | 0.6375 | 0.5556 | 0.4967 | 0.052* | |
C8 | 0.5643 (3) | 0.5798 (4) | 0.5641 (2) | 0.0463 (11) | |
H8 | 0.5557 | 0.6488 | 0.5668 | 0.056* | |
C9 | 0.5337 (3) | 0.5098 (4) | 0.59883 (19) | 0.0428 (10) | |
H9 | 0.5001 | 0.5230 | 0.6301 | 0.051* | |
N7 | 0.6206 (3) | 0.2559 (3) | 0.53224 (15) | 0.0390 (8) | |
C10 | 0.6384 (3) | 0.3432 (4) | 0.50845 (17) | 0.0396 (9) | |
N8 | 0.6826 (3) | 0.3280 (3) | 0.46160 (17) | 0.0536 (10) | |
H8N | 0.7016 | 0.3736 | 0.4398 | 0.064* | |
C11 | 0.6920 (4) | 0.2273 (4) | 0.4549 (2) | 0.0585 (14) | |
H11 | 0.7195 | 0.1953 | 0.4257 | 0.070* | |
C12 | 0.6539 (4) | 0.1817 (4) | 0.4986 (2) | 0.0504 (11) | |
H12 | 0.6509 | 0.1130 | 0.5047 | 0.061* | |
N9 | 0.6384 (3) | 0.3734 (3) | 0.71439 (15) | 0.0423 (8) | |
C13 | 0.5952 (4) | 0.3336 (4) | 0.7567 (2) | 0.0512 (12) | |
N10 | 0.5627 (4) | 0.4057 (4) | 0.78885 (18) | 0.0664 (13) | |
H10N | 0.5319 | 0.3970 | 0.8182 | 0.080* | |
C14 | 0.5871 (5) | 0.4961 (5) | 0.7667 (2) | 0.0676 (16) | |
H14 | 0.5738 | 0.5595 | 0.7804 | 0.081* | |
C15 | 0.6344 (4) | 0.4748 (4) | 0.7210 (2) | 0.0531 (12) | |
H15 | 0.6601 | 0.5220 | 0.6976 | 0.064* | |
N11 | 0.6335 (3) | 0.1765 (3) | 0.71885 (15) | 0.0453 (9) | |
C16 | 0.5913 (4) | 0.2257 (4) | 0.7586 (2) | 0.0502 (12) | |
N12 | 0.5527 (3) | 0.1611 (4) | 0.79328 (18) | 0.0635 (12) | |
H12N | 0.5212 | 0.1765 | 0.8217 | 0.076* | |
C17 | 0.5720 (4) | 0.0677 (5) | 0.7758 (2) | 0.0627 (15) | |
H17 | 0.5539 | 0.0082 | 0.7924 | 0.075* | |
C18 | 0.6224 (4) | 0.0763 (4) | 0.7299 (2) | 0.0520 (12) | |
H18 | 0.6456 | 0.0234 | 0.7093 | 0.062* | |
N13 | 0.7779 (3) | 0.3618 (3) | 0.61590 (15) | 0.0396 (8) | |
C19 | 0.8386 (3) | 0.3131 (4) | 0.58366 (19) | 0.0442 (10) | |
N14 | 0.8953 (3) | 0.3771 (4) | 0.55698 (18) | 0.0559 (11) | |
H14N | 0.9392 | 0.3618 | 0.5340 | 0.067* | |
C20 | 0.8703 (4) | 0.4718 (4) | 0.5732 (2) | 0.0602 (14) | |
H20 | 0.8976 | 0.5317 | 0.5614 | 0.072* | |
C21 | 0.7992 (4) | 0.4617 (4) | 0.6093 (2) | 0.0489 (11) | |
H21 | 0.7689 | 0.5143 | 0.6271 | 0.059* | |
N15 | 0.7704 (3) | 0.1651 (3) | 0.61760 (16) | 0.0429 (8) | |
C22 | 0.8347 (3) | 0.2059 (4) | 0.5846 (2) | 0.0448 (10) | |
N16 | 0.8832 (3) | 0.1360 (4) | 0.55801 (19) | 0.0566 (11) | |
H16N | 0.9273 | 0.1460 | 0.5343 | 0.068* | |
C23 | 0.8496 (4) | 0.0443 (4) | 0.5755 (2) | 0.0610 (14) | |
H23 | 0.8704 | −0.0185 | 0.5641 | 0.073* | |
C24 | 0.7804 (4) | 0.0632 (4) | 0.6123 (2) | 0.0519 (12) | |
H24 | 0.7454 | 0.0151 | 0.6311 | 0.062* | |
O1 | 0.3963 (3) | 0.2753 (3) | 0.54537 (15) | 0.0538 (9) | |
O2 | 0.8362 (3) | 0.2659 (4) | 0.72130 (19) | 0.0794 (14) | |
Cl1 | 0.82216 (13) | 0.56104 (17) | 0.41178 (8) | 0.0877 (6) | |
O3 | 0.7225 (3) | 0.5342 (4) | 0.4201 (2) | 0.0953 (16) | |
O4 | 0.8275 (8) | 0.6651 (8) | 0.4169 (5) | 0.251 (6) | |
O5 | 0.8534 (5) | 0.5347 (7) | 0.3606 (3) | 0.147 (3) | |
O6 | 0.8836 (5) | 0.5176 (10) | 0.4482 (3) | 0.226 (6) | |
Cl2 | 0.62259 (12) | 0.29621 (12) | 0.31100 (6) | 0.0670 (4) | |
O7 | 0.6129 (5) | 0.3492 (7) | 0.2641 (3) | 0.176 (4) | |
O8 | 0.7027 (8) | 0.3402 (10) | 0.3378 (3) | 0.247 (7) | |
O9 | 0.5418 (6) | 0.2932 (5) | 0.3436 (4) | 0.160 (3) | |
O10 | 0.6425 (7) | 0.1999 (5) | 0.3012 (5) | 0.220 (5) | |
Cl3 | 0.37165 (15) | 0.4949 (2) | 0.89392 (11) | 0.1040 (7) | |
O11 | 0.4298 (10) | 0.4154 (12) | 0.8840 (6) | 0.288 (7) | |
O12 | 0.2801 (5) | 0.4730 (9) | 0.8978 (6) | 0.280 (8) | |
O13 | 0.3977 (9) | 0.5226 (14) | 0.9437 (4) | 0.312 (9) | |
O14 | 0.4004 (10) | 0.5565 (10) | 0.8582 (5) | 0.260 (6) | |
Cl4A | 0.7636 (3) | 0.2821 (2) | 0.87174 (16) | 0.0626 (10) | 0.649 (8) |
O15A | 0.7851 (6) | 0.3493 (5) | 0.8278 (3) | 0.081 (2) | 0.649 (8) |
Cl4B | 0.7282 (6) | 0.2572 (5) | 0.8980 (4) | 0.081 (2) | 0.351 (8) |
O15B | 0.7235 (13) | 0.1923 (12) | 0.9389 (8) | 0.119 (7) | 0.351 (8) |
O16 | 0.6564 (5) | 0.3039 (5) | 0.8873 (3) | 0.123 (2) | |
O17 | 0.7675 (5) | 0.1868 (4) | 0.8526 (3) | 0.113 (2) | |
O18 | 0.8267 (5) | 0.3083 (5) | 0.9135 (2) | 0.121 (2) | |
O19 | 0.2799 (5) | 0.0158 (4) | 0.7481 (2) | 0.115 (2) | |
O20 | 0.4216 (6) | 0.2069 (7) | 0.8760 (3) | 0.168 (3) | |
O21 | 1.0149 (5) | 0.2533 (5) | 0.4893 (3) | 0.116 (2) | |
O22 | 0.3310 (4) | 0.0906 (4) | 0.5107 (2) | 0.1086 (18) | |
O23 | 1.0140 (5) | 0.2828 (8) | 0.6767 (4) | 0.215 (5) | |
Atomic displacement parameters (Å2) top | U11 | U22 | U33 | U12 | U13 | U23 |
Rh1 | 0.03611 (18) | 0.0295 (2) | 0.03494 (19) | −0.00147 (12) | 0.00621 (13) | 0.00278 (12) |
Rh2 | 0.03811 (19) | 0.0351 (2) | 0.0374 (2) | 0.00114 (13) | 0.00349 (14) | 0.00125 (13) |
N1 | 0.0418 (18) | 0.035 (2) | 0.041 (2) | 0.0015 (15) | 0.0098 (15) | 0.0033 (15) |
C1 | 0.042 (2) | 0.042 (3) | 0.051 (3) | 0.000 (2) | 0.0099 (19) | 0.011 (2) |
N2 | 0.062 (3) | 0.054 (3) | 0.078 (3) | 0.001 (2) | 0.038 (2) | 0.014 (2) |
C2 | 0.076 (4) | 0.056 (4) | 0.080 (4) | 0.016 (3) | 0.045 (3) | 0.010 (3) |
C3 | 0.057 (3) | 0.046 (3) | 0.059 (3) | 0.005 (2) | 0.018 (2) | 0.001 (2) |
N3 | 0.0424 (18) | 0.033 (2) | 0.043 (2) | −0.0018 (15) | 0.0060 (15) | 0.0052 (16) |
C4 | 0.042 (2) | 0.040 (3) | 0.051 (3) | −0.0022 (19) | 0.0051 (19) | 0.009 (2) |
N4 | 0.054 (2) | 0.035 (2) | 0.075 (3) | −0.0118 (18) | 0.014 (2) | 0.009 (2) |
C5 | 0.066 (3) | 0.032 (3) | 0.077 (4) | −0.007 (2) | 0.005 (3) | 0.000 (2) |
C6 | 0.058 (3) | 0.032 (3) | 0.062 (3) | −0.003 (2) | 0.012 (2) | −0.003 (2) |
N5 | 0.0369 (17) | 0.0322 (19) | 0.0400 (19) | −0.0020 (14) | 0.0016 (14) | 0.0025 (15) |
C7 | 0.0349 (19) | 0.040 (2) | 0.041 (2) | −0.0049 (17) | −0.0032 (17) | 0.0070 (19) |
N6 | 0.0450 (19) | 0.037 (2) | 0.049 (2) | −0.0069 (16) | 0.0016 (17) | 0.0136 (17) |
C8 | 0.047 (2) | 0.034 (2) | 0.058 (3) | 0.0000 (19) | −0.005 (2) | 0.001 (2) |
C9 | 0.045 (2) | 0.040 (3) | 0.043 (2) | 0.0000 (18) | 0.0010 (19) | −0.0013 (19) |
N7 | 0.0411 (18) | 0.041 (2) | 0.0354 (19) | −0.0001 (15) | 0.0044 (15) | 0.0010 (15) |
C10 | 0.039 (2) | 0.044 (3) | 0.036 (2) | −0.0044 (18) | 0.0012 (17) | 0.0027 (19) |
N8 | 0.061 (2) | 0.055 (3) | 0.046 (2) | −0.004 (2) | 0.0139 (19) | 0.009 (2) |
C11 | 0.074 (3) | 0.060 (4) | 0.042 (3) | 0.006 (3) | 0.020 (2) | −0.002 (2) |
C12 | 0.059 (3) | 0.045 (3) | 0.048 (3) | 0.004 (2) | 0.010 (2) | −0.005 (2) |
N9 | 0.051 (2) | 0.038 (2) | 0.038 (2) | 0.0023 (16) | 0.0038 (16) | −0.0031 (16) |
C13 | 0.057 (3) | 0.056 (3) | 0.041 (2) | 0.007 (2) | 0.006 (2) | −0.005 (2) |
N10 | 0.082 (3) | 0.074 (4) | 0.044 (2) | 0.013 (3) | 0.013 (2) | −0.010 (2) |
C14 | 0.087 (4) | 0.059 (4) | 0.056 (3) | 0.018 (3) | −0.003 (3) | −0.018 (3) |
C15 | 0.065 (3) | 0.045 (3) | 0.049 (3) | 0.002 (2) | 0.000 (2) | −0.008 (2) |
N11 | 0.047 (2) | 0.047 (2) | 0.042 (2) | 0.0007 (17) | 0.0046 (16) | 0.0056 (18) |
C16 | 0.057 (3) | 0.059 (3) | 0.035 (2) | 0.003 (2) | 0.007 (2) | 0.009 (2) |
N12 | 0.069 (3) | 0.080 (4) | 0.043 (2) | 0.002 (3) | 0.013 (2) | 0.015 (2) |
C17 | 0.069 (3) | 0.061 (4) | 0.058 (3) | −0.005 (3) | 0.001 (3) | 0.017 (3) |
C18 | 0.057 (3) | 0.048 (3) | 0.052 (3) | −0.002 (2) | −0.001 (2) | 0.010 (2) |
N13 | 0.0406 (18) | 0.037 (2) | 0.042 (2) | −0.0040 (15) | 0.0016 (15) | −0.0011 (16) |
C19 | 0.039 (2) | 0.045 (3) | 0.048 (3) | −0.0065 (19) | 0.0028 (19) | 0.003 (2) |
N14 | 0.048 (2) | 0.062 (3) | 0.059 (3) | −0.010 (2) | 0.0158 (19) | 0.007 (2) |
C20 | 0.060 (3) | 0.051 (3) | 0.069 (4) | −0.011 (3) | 0.003 (3) | 0.006 (3) |
C21 | 0.051 (3) | 0.039 (3) | 0.056 (3) | −0.004 (2) | −0.002 (2) | 0.001 (2) |
N15 | 0.0411 (18) | 0.041 (2) | 0.047 (2) | 0.0057 (16) | 0.0054 (16) | 0.0005 (17) |
C22 | 0.039 (2) | 0.049 (3) | 0.046 (3) | 0.002 (2) | 0.0083 (19) | −0.002 (2) |
N16 | 0.050 (2) | 0.056 (3) | 0.064 (3) | 0.008 (2) | 0.016 (2) | −0.008 (2) |
C23 | 0.060 (3) | 0.044 (3) | 0.080 (4) | 0.009 (2) | 0.007 (3) | −0.012 (3) |
C24 | 0.058 (3) | 0.036 (3) | 0.061 (3) | 0.004 (2) | 0.003 (2) | 0.002 (2) |
O1 | 0.0518 (19) | 0.054 (2) | 0.056 (2) | −0.0092 (15) | −0.0046 (16) | 0.0093 (16) |
O2 | 0.056 (2) | 0.114 (4) | 0.068 (3) | 0.008 (2) | −0.013 (2) | 0.010 (2) |
Cl1 | 0.0715 (10) | 0.1087 (15) | 0.0835 (12) | −0.0251 (10) | 0.0136 (9) | 0.0190 (11) |
O3 | 0.067 (3) | 0.102 (4) | 0.119 (4) | −0.012 (3) | 0.028 (3) | 0.024 (3) |
O4 | 0.266 (11) | 0.140 (8) | 0.354 (15) | −0.120 (8) | 0.114 (11) | −0.082 (9) |
O5 | 0.116 (4) | 0.223 (9) | 0.107 (5) | −0.024 (5) | 0.053 (4) | −0.035 (5) |
O6 | 0.088 (4) | 0.432 (17) | 0.159 (7) | 0.027 (7) | −0.001 (5) | 0.138 (9) |
Cl2 | 0.0787 (9) | 0.0601 (9) | 0.0635 (8) | 0.0045 (7) | 0.0220 (7) | 0.0035 (7) |
O7 | 0.161 (6) | 0.205 (8) | 0.158 (6) | −0.067 (6) | −0.058 (5) | 0.124 (6) |
O8 | 0.259 (10) | 0.385 (16) | 0.094 (5) | −0.225 (11) | −0.034 (6) | 0.052 (7) |
O9 | 0.171 (7) | 0.096 (5) | 0.223 (8) | 0.008 (4) | 0.143 (6) | −0.011 (5) |
O10 | 0.278 (11) | 0.071 (4) | 0.324 (12) | 0.035 (5) | 0.228 (10) | 0.013 (6) |
Cl3 | 0.0766 (12) | 0.1158 (18) | 0.1208 (18) | −0.0125 (11) | 0.0247 (11) | 0.0101 (15) |
O11 | 0.252 (12) | 0.311 (18) | 0.310 (16) | 0.114 (12) | 0.134 (11) | −0.009 (13) |
O12 | 0.080 (5) | 0.300 (14) | 0.46 (2) | −0.050 (7) | −0.047 (8) | 0.141 (13) |
O13 | 0.249 (12) | 0.60 (3) | 0.095 (7) | −0.103 (14) | 0.065 (7) | −0.027 (11) |
O14 | 0.350 (16) | 0.210 (12) | 0.222 (11) | −0.090 (11) | 0.054 (11) | 0.091 (9) |
Cl4A | 0.0759 (18) | 0.0410 (15) | 0.0700 (18) | 0.0079 (12) | −0.0118 (14) | −0.0033 (12) |
O15A | 0.123 (6) | 0.049 (4) | 0.070 (4) | 0.000 (4) | −0.011 (4) | 0.010 (3) |
Cl4B | 0.077 (4) | 0.048 (3) | 0.117 (6) | 0.003 (2) | −0.014 (4) | 0.008 (3) |
O15B | 0.126 (13) | 0.058 (9) | 0.172 (18) | 0.012 (9) | 0.000 (12) | 0.032 (11) |
O16 | 0.148 (5) | 0.116 (5) | 0.106 (5) | 0.035 (4) | −0.003 (4) | 0.003 (4) |
O17 | 0.140 (5) | 0.061 (3) | 0.138 (5) | −0.001 (3) | −0.020 (4) | −0.024 (3) |
O18 | 0.160 (5) | 0.110 (5) | 0.091 (4) | −0.040 (4) | −0.013 (4) | −0.015 (4) |
O19 | 0.164 (5) | 0.058 (3) | 0.126 (5) | −0.018 (3) | 0.081 (4) | −0.003 (3) |
O20 | 0.138 (6) | 0.241 (10) | 0.130 (6) | −0.021 (6) | 0.080 (5) | −0.040 (6) |
O21 | 0.122 (5) | 0.123 (5) | 0.107 (5) | −0.020 (4) | 0.059 (4) | −0.017 (4) |
O22 | 0.128 (4) | 0.093 (4) | 0.103 (4) | −0.012 (3) | −0.008 (3) | −0.006 (3) |
O23 | 0.064 (3) | 0.369 (14) | 0.211 (9) | 0.002 (5) | 0.003 (4) | 0.175 (9) |
Geometric parameters (Å, º) top
Rh1—N7 | 2.045 (4) | N10—H10N | 0.8600 |
Rh1—N1 | 2.049 (4) | C14—C15 | 1.352 (8) |
Rh1—N5 | 2.050 (4) | C14—H14 | 0.9300 |
Rh1—N3 | 2.054 (4) | C15—H15 | 0.9300 |
Rh1—O1 | 2.328 (3) | N11—C16 | 1.329 (6) |
Rh1—Rh2 | 2.6488 (6) | N11—C18 | 1.373 (6) |
Rh2—N13 | 2.048 (4) | C16—N12 | 1.336 (7) |
Rh2—N11 | 2.051 (4) | N12—C17 | 1.347 (8) |
Rh2—N9 | 2.057 (4) | N12—H12N | 0.8600 |
Rh2—N15 | 2.061 (4) | C17—C18 | 1.354 (8) |
Rh2—O2 | 2.282 (4) | C17—H17 | 0.9300 |
N1—C1 | 1.331 (6) | C18—H18 | 0.9300 |
N1—C3 | 1.373 (6) | N13—C19 | 1.332 (6) |
C1—N2 | 1.337 (6) | N13—C21 | 1.374 (6) |
C1—C4 | 1.436 (7) | C19—N14 | 1.335 (6) |
N2—C2 | 1.357 (8) | C19—C22 | 1.430 (7) |
N2—H2N | 0.8600 | N14—C20 | 1.372 (7) |
C2—C3 | 1.382 (7) | N14—H14N | 0.8600 |
C2—H2 | 0.9300 | C20—C21 | 1.339 (7) |
C3—H3 | 0.9300 | C20—H20 | 0.9300 |
N3—C4 | 1.325 (6) | C21—H21 | 0.9300 |
N3—C6 | 1.371 (6) | N15—C22 | 1.327 (6) |
C4—N4 | 1.342 (6) | N15—C24 | 1.372 (6) |
N4—C5 | 1.348 (7) | C22—N16 | 1.327 (6) |
N4—H4N | 0.8600 | N16—C23 | 1.379 (7) |
C5—C6 | 1.369 (7) | N16—H16N | 0.8600 |
C5—H5 | 0.9300 | C23—C24 | 1.350 (8) |
C6—H6 | 0.9300 | C23—H23 | 0.9300 |
N5—C7 | 1.325 (6) | C24—H24 | 0.9300 |
N5—C9 | 1.359 (6) | Cl1—O6 | 1.340 (7) |
C7—N6 | 1.343 (6) | Cl1—O4 | 1.395 (9) |
C7—C10 | 1.432 (7) | Cl1—O5 | 1.399 (6) |
N6—C8 | 1.366 (6) | Cl1—O3 | 1.409 (4) |
N6—H6N | 0.8600 | Cl2—O10 | 1.336 (7) |
C8—C9 | 1.345 (7) | Cl2—O7 | 1.368 (6) |
C8—H8 | 0.9300 | Cl2—O9 | 1.376 (6) |
C9—H9 | 0.9300 | Cl2—O8 | 1.381 (7) |
N7—C10 | 1.332 (6) | Cl3—O12 | 1.273 (7) |
N7—C12 | 1.379 (6) | Cl3—O14 | 1.278 (9) |
C10—N8 | 1.341 (6) | Cl3—O13 | 1.330 (11) |
N8—C11 | 1.359 (7) | Cl3—O11 | 1.344 (12) |
N8—H8N | 0.8600 | Cl4A—O17 | 1.360 (6) |
C11—C12 | 1.360 (7) | Cl4A—O18 | 1.367 (6) |
C11—H11 | 0.9300 | Cl4A—O15A | 1.449 (8) |
C12—H12 | 0.9300 | Cl4A—O16 | 1.532 (8) |
N9—C13 | 1.330 (6) | Cl4B—O16 | 1.173 (8) |
N9—C15 | 1.364 (6) | Cl4B—O15B | 1.34 (2) |
C13—N10 | 1.334 (7) | Cl4B—O18 | 1.529 (9) |
C13—C16 | 1.440 (8) | Cl4B—O17 | 1.574 (11) |
N10—C14 | 1.370 (8) | | |
| | | |
O20···O11 | 2.790 (18) | O18···O22ii | 2.770 (8) |
O22···O1 | 2.744 (6) | O23···O7ii | 3.070 (12) |
O23···O2 | 2.678 (8) | O21···O15Biii | 3.193 (18) |
O19···O7i | 2.916 (9) | O22···O12iv | 3.177 (14) |
O19···O8i | 3.146 (11) | O21···O4v | 3.291 (13) |
O19···O5i | 3.018 (9) | O23···O5v | 3.173 (12) |
O20···O21i | 3.100 (10) | O23···O4v | 3.281 (15) |
O20···O8i | 3.131 (12) | | |
| | | |
N7—Rh1—N1 | 173.08 (14) | C15—N9—Rh2 | 139.8 (4) |
N7—Rh1—N5 | 79.53 (15) | N9—C13—N10 | 110.3 (5) |
N1—Rh1—N5 | 100.15 (15) | N9—C13—C16 | 116.2 (4) |
N7—Rh1—N3 | 99.95 (15) | N10—C13—C16 | 133.5 (5) |
N1—Rh1—N3 | 79.78 (15) | C13—N10—C14 | 107.8 (5) |
N5—Rh1—N3 | 175.18 (13) | C13—N10—H10N | 126.1 |
N7—Rh1—O1 | 88.46 (14) | C14—N10—H10N | 126.1 |
N1—Rh1—O1 | 84.62 (14) | C15—C14—N10 | 106.2 (5) |
N5—Rh1—O1 | 86.72 (12) | C15—C14—H14 | 126.9 |
N3—Rh1—O1 | 88.48 (13) | N10—C14—H14 | 126.9 |
N7—Rh1—Rh2 | 93.23 (10) | C14—C15—N9 | 109.3 (5) |
N1—Rh1—Rh2 | 93.69 (10) | C14—C15—H15 | 125.3 |
N5—Rh1—Rh2 | 91.67 (9) | N9—C15—H15 | 125.3 |
N3—Rh1—Rh2 | 93.14 (10) | C16—N11—C18 | 106.3 (4) |
O1—Rh1—Rh2 | 177.42 (10) | C16—N11—Rh2 | 113.5 (3) |
N13—Rh2—N11 | 174.14 (14) | C18—N11—Rh2 | 140.1 (4) |
N13—Rh2—N9 | 99.67 (16) | N11—C16—N12 | 110.3 (5) |
N11—Rh2—N9 | 79.56 (17) | N11—C16—C13 | 116.9 (4) |
N13—Rh2—N15 | 79.41 (16) | N12—C16—C13 | 132.8 (5) |
N11—Rh2—N15 | 100.95 (17) | C16—N12—C17 | 107.7 (5) |
N9—Rh2—N15 | 176.01 (14) | C16—N12—H12N | 126.1 |
N13—Rh2—O2 | 87.62 (16) | C17—N12—H12N | 126.1 |
N11—Rh2—O2 | 86.54 (16) | N12—C17—C18 | 107.6 (5) |
N9—Rh2—O2 | 88.12 (16) | N12—C17—H17 | 126.2 |
N15—Rh2—O2 | 87.96 (16) | C18—C17—H17 | 126.2 |
N13—Rh2—Rh1 | 93.64 (9) | C17—C18—N11 | 108.1 (5) |
N11—Rh2—Rh1 | 92.20 (10) | C17—C18—H18 | 126.0 |
N9—Rh2—Rh1 | 91.82 (10) | N11—C18—H18 | 126.0 |
N15—Rh2—Rh1 | 92.11 (10) | C19—N13—C21 | 105.5 (4) |
O2—Rh2—Rh1 | 178.73 (13) | C19—N13—Rh2 | 113.3 (3) |
C1—N1—C3 | 106.6 (4) | C21—N13—Rh2 | 140.5 (3) |
C1—N1—Rh1 | 113.2 (3) | N13—C19—N14 | 111.0 (5) |
C3—N1—Rh1 | 139.9 (3) | N13—C19—C22 | 117.0 (4) |
N1—C1—N2 | 110.3 (5) | N14—C19—C22 | 132.0 (5) |
N1—C1—C4 | 116.7 (4) | C19—N14—C20 | 107.1 (5) |
N2—C1—C4 | 132.9 (5) | C19—N14—H14N | 126.5 |
C1—N2—C2 | 108.6 (4) | C20—N14—H14N | 126.5 |
C1—N2—H2N | 125.7 | C21—C20—N14 | 106.9 (5) |
C2—N2—H2N | 125.7 | C21—C20—H20 | 126.5 |
N2—C2—C3 | 106.1 (5) | N14—C20—H20 | 126.5 |
N2—C2—H2 | 126.9 | C20—C21—N13 | 109.5 (5) |
C3—C2—H2 | 126.9 | C20—C21—H21 | 125.3 |
N1—C3—C2 | 108.3 (5) | N13—C21—H21 | 125.3 |
N1—C3—H3 | 125.9 | C22—N15—C24 | 106.2 (4) |
C2—C3—H3 | 125.9 | C22—N15—Rh2 | 113.4 (3) |
C4—N3—C6 | 106.4 (4) | C24—N15—Rh2 | 140.0 (4) |
C4—N3—Rh1 | 113.2 (3) | N16—C22—N15 | 111.2 (5) |
C6—N3—Rh1 | 140.2 (3) | N16—C22—C19 | 132.4 (5) |
N3—C4—N4 | 110.9 (4) | N15—C22—C19 | 116.4 (4) |
N3—C4—C1 | 116.8 (4) | C22—N16—C23 | 107.1 (5) |
N4—C4—C1 | 132.3 (5) | C22—N16—H16N | 126.5 |
C4—N4—C5 | 107.3 (4) | C23—N16—H16N | 126.5 |
C4—N4—H4N | 126.3 | C24—C23—N16 | 106.7 (5) |
C5—N4—H4N | 126.3 | C24—C23—H23 | 126.6 |
N4—C5—C6 | 107.4 (5) | N16—C23—H23 | 126.6 |
N4—C5—H5 | 126.3 | C23—C24—N15 | 108.8 (5) |
C6—C5—H5 | 126.3 | C23—C24—H24 | 125.6 |
C5—C6—N3 | 108.0 (5) | N15—C24—H24 | 125.6 |
C5—C6—H6 | 126.0 | O6—Cl1—O4 | 109.8 (8) |
N3—C6—H6 | 126.0 | O6—Cl1—O5 | 108.1 (6) |
C7—N5—C9 | 106.0 (4) | O4—Cl1—O5 | 108.5 (6) |
C7—N5—Rh1 | 113.5 (3) | O6—Cl1—O3 | 111.1 (4) |
C9—N5—Rh1 | 140.3 (3) | O4—Cl1—O3 | 106.6 (5) |
N5—C7—N6 | 110.5 (4) | O5—Cl1—O3 | 112.6 (4) |
N5—C7—C10 | 116.8 (4) | O10—Cl2—O7 | 110.8 (7) |
N6—C7—C10 | 132.7 (4) | O10—Cl2—O9 | 104.2 (4) |
C7—N6—C8 | 107.3 (4) | O7—Cl2—O9 | 117.5 (5) |
C7—N6—H6N | 126.3 | O10—Cl2—O8 | 109.8 (8) |
C8—N6—H6N | 126.3 | O7—Cl2—O8 | 104.3 (5) |
C9—C8—N6 | 106.3 (4) | O9—Cl2—O8 | 110.2 (6) |
C9—C8—H8 | 126.9 | O12—Cl3—O14 | 120.9 (8) |
N6—C8—H8 | 126.9 | O12—Cl3—O13 | 102.8 (9) |
C8—C9—N5 | 110.0 (4) | O14—Cl3—O13 | 113.1 (9) |
C8—C9—H9 | 125.0 | O12—Cl3—O11 | 113.8 (10) |
N5—C9—H9 | 125.0 | O14—Cl3—O11 | 100.8 (9) |
C10—N7—C12 | 106.9 (4) | O13—Cl3—O11 | 104.6 (10) |
C10—N7—Rh1 | 113.7 (3) | O17—Cl4A—O18 | 118.4 (4) |
C12—N7—Rh1 | 138.9 (3) | O17—Cl4A—O15A | 107.6 (5) |
N7—C10—N8 | 110.2 (4) | O18—Cl4A—O15A | 106.4 (5) |
N7—C10—C7 | 116.2 (4) | O17—Cl4A—O16 | 108.2 (5) |
N8—C10—C7 | 133.5 (4) | O18—Cl4A—O16 | 109.1 (4) |
C10—N8—C11 | 107.5 (4) | O15A—Cl4A—O16 | 106.6 (4) |
C10—N8—H8N | 126.2 | O16—Cl4B—O15B | 117.3 (12) |
C11—N8—H8N | 126.2 | O16—Cl4B—O18 | 121.4 (7) |
N8—C11—C12 | 107.8 (5) | O15B—Cl4B—O18 | 99.1 (9) |
N8—C11—H11 | 126.1 | O16—Cl4B—O17 | 116.4 (7) |
C12—C11—H11 | 126.1 | O15B—Cl4B—O17 | 100.8 (9) |
C11—C12—N7 | 107.6 (5) | O18—Cl4B—O17 | 98.0 (6) |
C11—C12—H12 | 126.2 | Cl4B—O16—Cl4A | 35.2 (5) |
N7—C12—H12 | 126.2 | Cl4A—O17—Cl4B | 34.2 (3) |
C13—N9—C15 | 106.3 (4) | Cl4A—O18—Cl4B | 35.1 (3) |
C13—N9—Rh2 | 113.6 (3) | | |
| | | |
N7—Rh1—Rh2—N13 | 42.27 (15) | C12—N7—C10—C7 | 177.6 (4) |
N1—Rh1—Rh2—N13 | −137.62 (15) | Rh1—N7—C10—C7 | 4.7 (5) |
N5—Rh1—Rh2—N13 | −37.33 (15) | N5—C7—C10—N7 | −1.2 (5) |
N3—Rh1—Rh2—N13 | 142.43 (15) | N6—C7—C10—N7 | −179.8 (4) |
O1—Rh1—Rh2—N13 | −89 (2) | N5—C7—C10—N8 | 176.7 (4) |
N7—Rh1—Rh2—N11 | −138.30 (16) | N6—C7—C10—N8 | −2.0 (8) |
N1—Rh1—Rh2—N11 | 41.81 (16) | N7—C10—N8—C11 | 0.9 (5) |
N5—Rh1—Rh2—N11 | 142.10 (16) | C7—C10—N8—C11 | −177.0 (5) |
N3—Rh1—Rh2—N11 | −38.13 (16) | C10—N8—C11—C12 | −0.7 (6) |
O1—Rh1—Rh2—N11 | 91 (2) | N8—C11—C12—N7 | 0.2 (6) |
N7—Rh1—Rh2—N9 | 142.09 (16) | C10—N7—C12—C11 | 0.3 (6) |
N1—Rh1—Rh2—N9 | −37.81 (15) | Rh1—N7—C12—C11 | 170.3 (4) |
N5—Rh1—Rh2—N9 | 62.48 (15) | N13—Rh2—N9—C13 | −169.7 (3) |
N3—Rh1—Rh2—N9 | −117.75 (15) | N11—Rh2—N9—C13 | 4.4 (3) |
O1—Rh1—Rh2—N9 | 11 (2) | N15—Rh2—N9—C13 | −93 (2) |
N7—Rh1—Rh2—N15 | −37.25 (16) | O2—Rh2—N9—C13 | −82.4 (3) |
N1—Rh1—Rh2—N15 | 142.86 (15) | Rh1—Rh2—N9—C13 | 96.3 (3) |
N5—Rh1—Rh2—N15 | −116.85 (15) | N13—Rh2—N9—C15 | 2.8 (5) |
N3—Rh1—Rh2—N15 | 62.91 (15) | N11—Rh2—N9—C15 | 176.9 (5) |
O1—Rh1—Rh2—N15 | −168 (2) | N15—Rh2—N9—C15 | 79 (2) |
N7—Rh1—Rh2—O2 | −131 (6) | O2—Rh2—N9—C15 | 90.1 (5) |
N1—Rh1—Rh2—O2 | 49 (6) | Rh1—Rh2—N9—C15 | −91.2 (5) |
N5—Rh1—Rh2—O2 | 150 (6) | C15—N9—C13—N10 | 1.2 (6) |
N3—Rh1—Rh2—O2 | −31 (6) | Rh2—N9—C13—N10 | 176.1 (3) |
O1—Rh1—Rh2—O2 | 98 (6) | C15—N9—C13—C16 | −179.7 (4) |
N7—Rh1—N1—C1 | 83.3 (13) | Rh2—N9—C13—C16 | −4.7 (5) |
N5—Rh1—N1—C1 | 170.0 (3) | N9—C13—N10—C14 | −0.8 (6) |
N3—Rh1—N1—C1 | −5.1 (3) | C16—C13—N10—C14 | −179.8 (5) |
O1—Rh1—N1—C1 | 84.3 (3) | C13—N10—C14—C15 | 0.1 (6) |
Rh2—Rh1—N1—C1 | −97.6 (3) | N10—C14—C15—N9 | 0.6 (6) |
N7—Rh1—N1—C3 | −89.2 (13) | C13—N9—C15—C14 | −1.1 (6) |
N5—Rh1—N1—C3 | −2.5 (5) | Rh2—N9—C15—C14 | −174.0 (4) |
N3—Rh1—N1—C3 | −177.6 (5) | N13—Rh2—N11—C16 | 79.6 (16) |
O1—Rh1—N1—C3 | −88.2 (5) | N9—Rh2—N11—C16 | −3.4 (3) |
Rh2—Rh1—N1—C3 | 89.9 (5) | N15—Rh2—N11—C16 | 172.5 (3) |
C3—N1—C1—N2 | 0.3 (6) | O2—Rh2—N11—C16 | 85.3 (3) |
Rh1—N1—C1—N2 | −174.6 (3) | Rh1—Rh2—N11—C16 | −94.9 (3) |
C3—N1—C1—C4 | 179.1 (4) | N13—Rh2—N11—C18 | −95.4 (16) |
Rh1—N1—C1—C4 | 4.1 (5) | N9—Rh2—N11—C18 | −178.4 (5) |
N1—C1—N2—C2 | −0.5 (6) | N15—Rh2—N11—C18 | −2.5 (5) |
C4—C1—N2—C2 | −179.0 (5) | O2—Rh2—N11—C18 | −89.7 (5) |
C1—N2—C2—C3 | 0.5 (7) | Rh1—Rh2—N11—C18 | 90.1 (5) |
C1—N1—C3—C2 | 0.0 (6) | C18—N11—C16—N12 | −1.2 (6) |
Rh1—N1—C3—C2 | 172.8 (4) | Rh2—N11—C16—N12 | −177.9 (3) |
N2—C2—C3—N1 | −0.3 (7) | C18—N11—C16—C13 | 178.7 (4) |
N7—Rh1—N3—C4 | −167.6 (3) | Rh2—N11—C16—C13 | 2.0 (5) |
N1—Rh1—N3—C4 | 5.4 (3) | N9—C13—C16—N11 | 1.8 (7) |
N5—Rh1—N3—C4 | −84.2 (18) | N10—C13—C16—N11 | −179.3 (5) |
O1—Rh1—N3—C4 | −79.4 (3) | N9—C13—C16—N12 | −178.3 (5) |
Rh2—Rh1—N3—C4 | 98.6 (3) | N10—C13—C16—N12 | 0.7 (10) |
N7—Rh1—N3—C6 | 6.8 (5) | N11—C16—N12—C17 | 1.0 (6) |
N1—Rh1—N3—C6 | 179.7 (5) | C13—C16—N12—C17 | −178.9 (5) |
N5—Rh1—N3—C6 | 90.1 (18) | C16—N12—C17—C18 | −0.3 (6) |
O1—Rh1—N3—C6 | 94.9 (5) | N12—C17—C18—N11 | −0.4 (6) |
Rh2—Rh1—N3—C6 | −87.1 (5) | C16—N11—C18—C17 | 1.0 (5) |
C6—N3—C4—N4 | 0.6 (5) | Rh2—N11—C18—C17 | 176.2 (4) |
Rh1—N3—C4—N4 | 176.8 (3) | N11—Rh2—N13—C19 | 88.5 (16) |
C6—N3—C4—C1 | 178.9 (4) | N9—Rh2—N13—C19 | 170.5 (3) |
Rh1—N3—C4—C1 | −4.9 (5) | N15—Rh2—N13—C19 | −5.5 (3) |
N1—C1—C4—N3 | 0.5 (6) | O2—Rh2—N13—C19 | 82.8 (3) |
N2—C1—C4—N3 | 178.9 (5) | Rh1—Rh2—N13—C19 | −97.0 (3) |
N1—C1—C4—N4 | 178.4 (5) | N11—Rh2—N13—C21 | −80.3 (17) |
N2—C1—C4—N4 | −3.2 (9) | N9—Rh2—N13—C21 | 1.7 (5) |
N3—C4—N4—C5 | −0.2 (6) | N15—Rh2—N13—C21 | −174.4 (5) |
C1—C4—N4—C5 | −178.1 (5) | O2—Rh2—N13—C21 | −86.0 (5) |
C4—N4—C5—C6 | −0.3 (6) | Rh1—Rh2—N13—C21 | 94.2 (5) |
N4—C5—C6—N3 | 0.6 (6) | C21—N13—C19—N14 | −0.8 (5) |
C4—N3—C6—C5 | −0.7 (5) | Rh2—N13—C19—N14 | −173.4 (3) |
Rh1—N3—C6—C5 | −175.3 (4) | C21—N13—C19—C22 | 177.3 (4) |
N7—Rh1—N5—C7 | 4.2 (3) | Rh2—N13—C19—C22 | 4.7 (5) |
N1—Rh1—N5—C7 | −168.8 (3) | N13—C19—N14—C20 | 0.5 (5) |
N3—Rh1—N5—C7 | −80.1 (18) | C22—C19—N14—C20 | −177.2 (5) |
O1—Rh1—N5—C7 | −84.9 (3) | C19—N14—C20—C21 | 0.0 (6) |
Rh2—Rh1—N5—C7 | 97.1 (3) | N14—C20—C21—N13 | −0.5 (6) |
N7—Rh1—N5—C9 | 177.6 (4) | C19—N13—C21—C20 | 0.8 (5) |
N1—Rh1—N5—C9 | 4.6 (4) | Rh2—N13—C21—C20 | 170.2 (4) |
N3—Rh1—N5—C9 | 93.3 (18) | N13—Rh2—N15—C22 | 5.7 (3) |
O1—Rh1—N5—C9 | 88.5 (4) | N11—Rh2—N15—C22 | −168.4 (3) |
Rh2—Rh1—N5—C9 | −89.5 (4) | N9—Rh2—N15—C22 | −71 (2) |
C9—N5—C7—N6 | 0.3 (4) | O2—Rh2—N15—C22 | −82.3 (3) |
Rh1—N5—C7—N6 | 176.0 (2) | Rh1—Rh2—N15—C22 | 99.0 (3) |
C9—N5—C7—C10 | −178.6 (3) | N13—Rh2—N15—C24 | 177.1 (5) |
Rh1—N5—C7—C10 | −3.0 (4) | N11—Rh2—N15—C24 | 3.1 (5) |
N5—C7—N6—C8 | −0.5 (5) | N9—Rh2—N15—C24 | 100 (2) |
C10—C7—N6—C8 | 178.2 (4) | O2—Rh2—N15—C24 | 89.2 (5) |
C7—N6—C8—C9 | 0.4 (5) | Rh1—Rh2—N15—C24 | −89.6 (5) |
N6—C8—C9—N5 | −0.2 (5) | C24—N15—C22—N16 | 1.4 (5) |
C7—N5—C9—C8 | −0.1 (5) | Rh2—N15—C22—N16 | 175.7 (3) |
Rh1—N5—C9—C8 | −173.8 (3) | C24—N15—C22—C19 | −179.3 (4) |
N1—Rh1—N7—C10 | 83.2 (13) | Rh2—N15—C22—C19 | −5.0 (5) |
N5—Rh1—N7—C10 | −4.8 (3) | N13—C19—C22—N16 | 179.4 (5) |
N3—Rh1—N7—C10 | 170.3 (3) | N14—C19—C22—N16 | −3.0 (9) |
O1—Rh1—N7—C10 | 82.1 (3) | N13—C19—C22—N15 | 0.2 (6) |
Rh2—Rh1—N7—C10 | −95.9 (3) | N14—C19—C22—N15 | 177.8 (5) |
N1—Rh1—N7—C12 | −86.3 (13) | N15—C22—N16—C23 | −1.1 (6) |
N5—Rh1—N7—C12 | −174.3 (5) | C19—C22—N16—C23 | 179.7 (5) |
N3—Rh1—N7—C12 | 0.8 (5) | C22—N16—C23—C24 | 0.4 (6) |
O1—Rh1—N7—C12 | −87.4 (5) | N16—C23—C24—N15 | 0.4 (6) |
Rh2—Rh1—N7—C12 | 94.6 (5) | C22—N15—C24—C23 | −1.1 (6) |
C12—N7—C10—N8 | −0.8 (5) | Rh2—N15—C24—C23 | −172.9 (4) |
Rh1—N7—C10—N8 | −173.6 (3) | | |
Symmetry codes: (i) x−1/2, −y+1/2, z+1/2; (ii) x+1/2, −y+1/2, z+1/2; (iii) x+1/2, −y+1/2, z−1/2; (iv) −x+1/2, y−1/2, −z+3/2; (v) −x+2, −y+1, −z+1. |
Hydrogen-bond geometry (Å, º) top
D—H···A | D—H | H···A | D···A | D—H···A |
N2—H2N···O19 | 0.86 | 2.05 | 2.829 (7) | 151 |
N4—H4N···O19 | 0.86 | 2.27 | 3.013 (7) | 145 |
N4—H4N···O10vi | 0.86 | 2.52 | 3.104 (8) | 126 |
N6—H6N···O3 | 0.86 | 2.27 | 3.038 (7) | 149 |
N6—H6N···O1vii | 0.86 | 2.52 | 3.128 (5) | 128 |
N8—H8N···O3 | 0.86 | 2.22 | 2.991 (7) | 150 |
N8—H8N···O8 | 0.86 | 2.58 | 3.107 (8) | 121 |
N10—H10N···O11 | 0.86 | 2.18 | 3.014 (13) | 163 |
N12—H12N···O20 | 0.86 | 1.97 | 2.819 (8) | 167 |
N14—H14N···O21 | 0.86 | 2.11 | 2.884 (8) | 150 |
N16—H16N···O21 | 0.86 | 2.18 | 2.949 (8) | 148 |
Symmetry codes: (vi) −x+1, −y, −z+1; (vii) −x+1, −y+1, −z+1. |
Crystal data top
C26H32N16O2Rh2·4(ClO4) | Dx = 1.890 Mg m−3 |
Mr = 1204.30 | Mo Kα radiation, λ = 0.71069 Å |
Orthorhombic, Pbcn | Cell parameters from 9792 reflections |
a = 20.119 (5) Å | θ = 3.0–27.5° |
b = 16.115 (4) Å | µ = 1.13 mm−1 |
c = 13.055 (3) Å | T = 296 K |
V = 4232.9 (17) Å3 | Prismatic, green |
Z = 4 | 0.42 × 0.35 × 0.32 mm |
F(000) = 2408 | |
Data collection top
Rigaku/MSC Mercury CCD diffractometer | 4835 independent reflections |
Radiation source: rotating-anode X-ray tube | 4243 reflections with I > 2σ(I) |
Graphite monochromator | Rint = 0.033 |
Detector resolution: 14.62 pixels mm-1 | θmax = 27.5°, θmin = 3.1° |
ω scans | h = −26→25 |
Absorption correction: numerical NUMABS (Higashi, 1999) | k = −20→20 |
Tmin = 0.740, Tmax = 0.803 | l = −14→16 |
30878 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) = 0.126 | H atoms treated by a mixture of independent and constrained refinement |
S = 1.16 | w = 1/[σ2(Fo2) + (0.0552P)2 + 4.7874P] where P = (Fo2 + 2Fc2)/3 |
4838 reflections | (Δ/σ)max = 0.001 |
302 parameters | Δρmax = 1.04 e Å−3 |
1 restraint | Δρmin = −0.61 e Å−3 |
Crystal data top
C26H32N16O2Rh2·4(ClO4) | V = 4232.9 (17) Å3 |
Mr = 1204.30 | Z = 4 |
Orthorhombic, Pbcn | Mo Kα radiation |
a = 20.119 (5) Å | µ = 1.13 mm−1 |
b = 16.115 (4) Å | T = 296 K |
c = 13.055 (3) Å | 0.42 × 0.35 × 0.32 mm |
Data collection top
Rigaku/MSC Mercury CCD diffractometer | 4835 independent reflections |
Absorption correction: numerical NUMABS (Higashi, 1999) | 4243 reflections with I > 2σ(I) |
Tmin = 0.740, Tmax = 0.803 | Rint = 0.033 |
30878 measured reflections | |
Refinement top
R[F2 > 2σ(F2)] = 0.050 | 1 restraint |
wR(F2) = 0.126 | H atoms treated by a mixture of independent and constrained refinement |
S = 1.16 | Δρmax = 1.04 e Å−3 |
4838 reflections | Δρmin = −0.61 e Å−3 |
302 parameters | |
Special details top
Geometry. All e.s.d.'s (except the e.s.d. in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell e.s.d.'s are taken into account individually in the estimation of e.s.d.'s in distances, angles and torsion angles; correlations between e.s.d.'s in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell e.s.d.'s is used for estimating e.s.d.'s involving l.s. planes. |
Refinement. Refinement of F2 against ALL reflections. The weighted R-factor wR and goodness of fit S are based on F2, conventional R-factors R are based on F, with F set to zero for negative F2. The threshold expression of F2 > σ(F2) is used only for calculating R-factors(gt) etc. and is not relevant to the choice of reflections for refinement. R-factors based on F2 are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger. |
Fractional atomic coordinates and isotropic or equivalent isotropic displacement parameters (Å2) top | x | y | z | Uiso*/Ueq | |
Rh1 | 0.497490 (11) | 0.271040 (16) | 0.64762 (2) | 0.03020 (11) | |
N1 | 0.59303 (14) | 0.31328 (19) | 0.6312 (2) | 0.0338 (6) | |
C1 | 0.63709 (18) | 0.2521 (2) | 0.6151 (3) | 0.0380 (8) | |
N2 | 0.69761 (15) | 0.2844 (2) | 0.5973 (3) | 0.0477 (9) | |
H2N | 0.7335 | 0.2569 | 0.5862 | 0.057* | |
C2 | 0.6918 (2) | 0.3688 (3) | 0.6000 (4) | 0.0503 (10) | |
H2 | 0.7256 | 0.4073 | 0.5898 | 0.060* | |
C3 | 0.62670 (19) | 0.3860 (3) | 0.6206 (3) | 0.0417 (9) | |
H3 | 0.6084 | 0.4387 | 0.6263 | 0.050* | |
N3 | 0.54734 (14) | 0.16006 (18) | 0.6369 (2) | 0.0357 (7) | |
C4 | 0.61244 (18) | 0.1688 (2) | 0.6198 (3) | 0.0386 (8) | |
N4 | 0.64145 (16) | 0.0952 (2) | 0.6080 (3) | 0.0475 (8) | |
H4N | 0.6830 | 0.0865 | 0.5969 | 0.057* | |
C5 | 0.5934 (2) | 0.0364 (3) | 0.6169 (4) | 0.0520 (10) | |
H5 | 0.5992 | −0.0207 | 0.6116 | 0.062* | |
C6 | 0.5351 (2) | 0.0768 (2) | 0.6348 (3) | 0.0432 (9) | |
H6 | 0.4938 | 0.0518 | 0.6440 | 0.052* | |
N5 | 0.44682 (15) | 0.38132 (19) | 0.6460 (2) | 0.0353 (7) | |
C7 | 0.38098 (18) | 0.3726 (2) | 0.6400 (3) | 0.0369 (8) | |
N6 | 0.35148 (16) | 0.4461 (2) | 0.6299 (3) | 0.0471 (8) | |
H6N | 0.3094 | 0.4548 | 0.6254 | 0.057* | |
C8 | 0.4001 (2) | 0.5049 (3) | 0.6282 (4) | 0.0504 (10) | |
H8 | 0.3940 | 0.5619 | 0.6216 | 0.061* | |
C9 | 0.4589 (2) | 0.4646 (2) | 0.6377 (3) | 0.0429 (9) | |
H9 | 0.5006 | 0.4894 | 0.6385 | 0.052* | |
N7 | 0.40188 (15) | 0.22891 (19) | 0.6486 (2) | 0.0353 (7) | |
C10 | 0.35631 (18) | 0.2885 (3) | 0.6435 (3) | 0.0388 (8) | |
N8 | 0.29523 (16) | 0.2558 (2) | 0.6397 (3) | 0.0453 (8) | |
H8N | 0.2584 | 0.2829 | 0.6377 | 0.054* | |
C11 | 0.30196 (19) | 0.1716 (3) | 0.6396 (3) | 0.0483 (10) | |
H11 | 0.2678 | 0.1327 | 0.6365 | 0.058* | |
C12 | 0.36819 (19) | 0.1555 (3) | 0.6448 (3) | 0.0432 (9) | |
H12 | 0.3874 | 0.1030 | 0.6457 | 0.052* | |
O1 | 0.49253 (15) | 0.2775 (2) | 0.4713 (3) | 0.0576 (8) | |
H1 | 0.4653 (19) | 0.313 (2) | 0.461 (4) | 0.069* | |
C13 | 0.4931 (5) | 0.2148 (6) | 0.4038 (6) | 0.161 (5) | |
H13 | 0.5125 | 0.1666 | 0.4351 | 0.242* | |
H13A | 0.5189 | 0.2304 | 0.3449 | 0.242* | |
H13B | 0.4484 | 0.2024 | 0.3830 | 0.242* | |
Cl1 | 0.83630 (5) | 0.13164 (7) | 0.64406 (9) | 0.0534 (3) | |
O2 | 0.8199 (3) | 0.1982 (4) | 0.5815 (4) | 0.142 (3) | |
O3 | 0.7906 (2) | 0.0702 (4) | 0.6377 (7) | 0.189 (4) | |
O4 | 0.89949 (15) | 0.1003 (2) | 0.6126 (3) | 0.0670 (9) | |
O5 | 0.8381 (3) | 0.1616 (4) | 0.7444 (3) | 0.128 (2) | |
Cl2 | 0.16651 (6) | 0.41641 (8) | 0.65875 (11) | 0.0644 (4) | |
O6 | 0.2100 (2) | 0.4742 (3) | 0.6073 (5) | 0.133 (2) | |
O7 | 0.17426 (18) | 0.3388 (2) | 0.6079 (3) | 0.0777 (11) | |
O8 | 0.1864 (3) | 0.4092 (5) | 0.7603 (4) | 0.161 (3) | |
O9 | 0.10097 (16) | 0.4456 (2) | 0.6486 (3) | 0.0785 (12) | |
Atomic displacement parameters (Å2) top | U11 | U22 | U33 | U12 | U13 | U23 |
Rh1 | 0.02584 (16) | 0.03121 (17) | 0.03355 (18) | 0.00317 (10) | −0.00061 (10) | −0.00026 (11) |
N1 | 0.0301 (14) | 0.0357 (15) | 0.0355 (17) | −0.0002 (12) | 0.0006 (12) | 0.0013 (13) |
C1 | 0.0297 (17) | 0.044 (2) | 0.040 (2) | 0.0057 (15) | 0.0032 (16) | 0.0006 (17) |
N2 | 0.0302 (16) | 0.058 (2) | 0.055 (2) | 0.0031 (14) | 0.0065 (15) | 0.0012 (17) |
C2 | 0.044 (2) | 0.053 (2) | 0.054 (3) | −0.0092 (19) | 0.0025 (19) | 0.003 (2) |
C3 | 0.0382 (19) | 0.042 (2) | 0.045 (2) | 0.0005 (16) | 0.0004 (17) | 0.0030 (17) |
N3 | 0.0319 (15) | 0.0367 (15) | 0.0386 (18) | 0.0044 (12) | −0.0018 (12) | −0.0008 (13) |
C4 | 0.0352 (18) | 0.042 (2) | 0.039 (2) | 0.0054 (16) | 0.0045 (15) | −0.0017 (16) |
N4 | 0.0411 (17) | 0.0464 (19) | 0.055 (2) | 0.0148 (15) | 0.0071 (16) | −0.0017 (16) |
C5 | 0.056 (2) | 0.040 (2) | 0.060 (3) | 0.0080 (19) | 0.004 (2) | 0.000 (2) |
C6 | 0.045 (2) | 0.0354 (19) | 0.049 (2) | 0.0029 (16) | 0.0010 (17) | 0.0003 (17) |
N5 | 0.0334 (15) | 0.0373 (16) | 0.0352 (17) | 0.0059 (13) | −0.0016 (12) | 0.0008 (13) |
C7 | 0.0355 (18) | 0.0396 (19) | 0.036 (2) | 0.0081 (15) | 0.0000 (15) | −0.0037 (16) |
N6 | 0.0407 (17) | 0.0470 (19) | 0.054 (2) | 0.0168 (15) | −0.0052 (15) | −0.0008 (16) |
C8 | 0.057 (2) | 0.035 (2) | 0.060 (3) | 0.0108 (18) | −0.007 (2) | 0.0002 (19) |
C9 | 0.046 (2) | 0.0375 (19) | 0.046 (2) | 0.0004 (17) | −0.0039 (17) | −0.0014 (17) |
N7 | 0.0295 (15) | 0.0398 (17) | 0.0368 (18) | 0.0027 (12) | −0.0029 (12) | −0.0020 (13) |
C10 | 0.0276 (17) | 0.052 (2) | 0.036 (2) | 0.0052 (16) | −0.0011 (14) | −0.0002 (17) |
N8 | 0.0265 (15) | 0.0531 (19) | 0.056 (2) | 0.0049 (14) | −0.0023 (14) | −0.0023 (16) |
C11 | 0.0346 (19) | 0.052 (2) | 0.059 (3) | −0.0052 (17) | −0.0038 (17) | −0.001 (2) |
C12 | 0.0386 (19) | 0.0384 (19) | 0.053 (3) | −0.0019 (16) | −0.0006 (17) | −0.0070 (17) |
O1 | 0.0607 (19) | 0.069 (2) | 0.0430 (19) | 0.0178 (15) | −0.0112 (15) | 0.0015 (16) |
C13 | 0.244 (13) | 0.168 (9) | 0.071 (5) | 0.132 (8) | −0.051 (6) | −0.050 (5) |
Cl1 | 0.0412 (5) | 0.0613 (6) | 0.0577 (7) | 0.0131 (5) | 0.0093 (5) | 0.0090 (5) |
O2 | 0.142 (4) | 0.179 (5) | 0.105 (4) | 0.120 (4) | 0.052 (3) | 0.074 (4) |
O3 | 0.062 (3) | 0.129 (5) | 0.375 (12) | −0.032 (3) | 0.062 (4) | −0.073 (5) |
O4 | 0.0462 (17) | 0.063 (2) | 0.092 (3) | 0.0149 (15) | 0.0173 (17) | 0.0094 (18) |
O5 | 0.122 (4) | 0.193 (6) | 0.068 (3) | 0.064 (4) | 0.005 (3) | −0.019 (3) |
Cl2 | 0.0445 (6) | 0.0644 (7) | 0.0841 (9) | 0.0197 (5) | −0.0173 (5) | −0.0218 (6) |
O6 | 0.059 (2) | 0.074 (3) | 0.265 (7) | −0.006 (2) | −0.011 (3) | 0.000 (4) |
O7 | 0.070 (2) | 0.066 (2) | 0.097 (3) | 0.0290 (18) | −0.018 (2) | −0.018 (2) |
O8 | 0.166 (5) | 0.220 (7) | 0.096 (4) | 0.102 (5) | −0.070 (4) | −0.064 (4) |
O9 | 0.0445 (17) | 0.078 (2) | 0.114 (3) | 0.0212 (17) | −0.0125 (18) | −0.020 (2) |
Geometric parameters (Å, º) top
Rh1—N7 | 2.040 (3) | N6—C8 | 1.362 (6) |
Rh1—N5 | 2.049 (3) | N6—H6N | 0.8600 |
Rh1—N1 | 2.050 (3) | C8—C9 | 1.357 (6) |
Rh1—N3 | 2.055 (3) | C8—H8 | 0.9300 |
Rh1—O1 | 2.307 (4) | C9—H9 | 0.9300 |
Rh1—Rh1i | 2.6752 (9) | N7—C10 | 1.330 (5) |
N1—C1 | 1.343 (5) | N7—C12 | 1.365 (5) |
N1—C3 | 1.360 (5) | C10—N8 | 1.339 (5) |
C1—N2 | 1.345 (5) | N8—C11 | 1.363 (5) |
C1—C4 | 1.432 (5) | N8—H8N | 0.8600 |
N2—C2 | 1.366 (5) | C11—C12 | 1.359 (5) |
N2—H2N | 0.8600 | C11—H11 | 0.9300 |
C2—C3 | 1.364 (5) | C12—H12 | 0.9300 |
C2—H2 | 0.9300 | O1—C13 | 1.341 (8) |
C3—H3 | 0.9300 | O1—H1 | 0.805 (19) |
N3—C4 | 1.336 (5) | C13—H13 | 0.9600 |
N3—C6 | 1.365 (5) | C13—H13A | 0.9600 |
C4—N4 | 1.331 (5) | C13—H13B | 0.9600 |
N4—C5 | 1.359 (5) | Cl1—O3 | 1.354 (5) |
N4—H4N | 0.8600 | Cl1—O2 | 1.389 (4) |
C5—C6 | 1.362 (6) | Cl1—O5 | 1.396 (5) |
C5—H5 | 0.9300 | Cl1—O4 | 1.428 (3) |
C6—H6 | 0.9300 | Cl2—O8 | 1.389 (5) |
N5—C7 | 1.334 (5) | Cl2—O9 | 1.406 (3) |
N5—C9 | 1.368 (5) | Cl2—O7 | 1.424 (4) |
C7—N6 | 1.330 (5) | Cl2—O6 | 1.443 (5) |
C7—C10 | 1.444 (6) | | |
| | | |
N7—Rh1—N5 | 79.61 (12) | N6—C7—N5 | 110.8 (3) |
N7—Rh1—N1 | 174.38 (12) | N6—C7—C10 | 133.2 (3) |
N5—Rh1—N1 | 100.22 (12) | N5—C7—C10 | 116.0 (3) |
N7—Rh1—N3 | 99.84 (12) | C7—N6—C8 | 107.5 (3) |
N5—Rh1—N3 | 175.47 (12) | C7—N6—H6N | 126.2 |
N1—Rh1—N3 | 79.88 (12) | C8—N6—H6N | 126.2 |
N7—Rh1—O1 | 88.90 (12) | C9—C8—N6 | 106.9 (4) |
N5—Rh1—O1 | 85.94 (11) | C9—C8—H8 | 126.5 |
N1—Rh1—O1 | 85.49 (12) | N6—C8—H8 | 126.5 |
N3—Rh1—O1 | 89.56 (12) | C8—C9—N5 | 108.8 (4) |
N7—Rh1—Rh1i | 91.67 (9) | C8—C9—H9 | 125.6 |
N5—Rh1—Rh1i | 91.66 (8) | N5—C9—H9 | 125.6 |
N1—Rh1—Rh1i | 93.95 (9) | C10—N7—C12 | 106.4 (3) |
N3—Rh1—Rh1i | 92.85 (9) | C10—N7—Rh1 | 114.2 (3) |
O1—Rh1—Rh1i | 177.39 (8) | C12—N7—Rh1 | 139.2 (3) |
C1—N1—C3 | 106.7 (3) | N7—C10—N8 | 110.5 (4) |
C1—N1—Rh1 | 113.0 (2) | N7—C10—C7 | 116.3 (3) |
C3—N1—Rh1 | 139.8 (3) | N8—C10—C7 | 133.2 (4) |
N1—C1—N2 | 109.9 (3) | C10—N8—C11 | 107.6 (3) |
N1—C1—C4 | 116.9 (3) | C10—N8—H8N | 126.2 |
N2—C1—C4 | 133.2 (3) | C11—N8—H8N | 126.2 |
C1—N2—C2 | 107.7 (3) | C12—C11—N8 | 106.7 (4) |
C1—N2—H2N | 126.2 | C12—C11—H11 | 126.6 |
C2—N2—H2N | 126.2 | N8—C11—H11 | 126.6 |
C3—C2—N2 | 106.8 (4) | C11—C12—N7 | 108.8 (4) |
C3—C2—H2 | 126.6 | C11—C12—H12 | 125.6 |
N2—C2—H2 | 126.6 | N7—C12—H12 | 125.6 |
N1—C3—C2 | 108.9 (4) | C13—O1—Rh1 | 128.4 (5) |
N1—C3—H3 | 125.6 | C13—O1—H1 | 116 (4) |
C2—C3—H3 | 125.6 | Rh1—O1—H1 | 103 (4) |
C4—N3—C6 | 106.1 (3) | O1—C13—H13 | 109.5 |
C4—N3—Rh1 | 113.4 (2) | O1—C13—H13A | 109.5 |
C6—N3—Rh1 | 140.2 (3) | H13—C13—H13A | 109.5 |
N4—C4—N3 | 110.8 (3) | O1—C13—H13B | 109.5 |
N4—C4—C1 | 132.7 (3) | H13—C13—H13B | 109.5 |
N3—C4—C1 | 116.5 (3) | H13A—C13—H13B | 109.5 |
C4—N4—C5 | 107.4 (3) | O3—Cl1—O2 | 111.6 (5) |
C4—N4—H4N | 126.3 | O3—Cl1—O5 | 109.1 (4) |
C5—N4—H4N | 126.3 | O2—Cl1—O5 | 106.9 (4) |
N4—C5—C6 | 107.1 (4) | O3—Cl1—O4 | 109.1 (3) |
N4—C5—H5 | 126.4 | O2—Cl1—O4 | 108.4 (2) |
C6—C5—H5 | 126.4 | O5—Cl1—O4 | 111.6 (3) |
C5—C6—N3 | 108.5 (4) | O8—Cl2—O9 | 112.8 (3) |
C5—C6—H6 | 125.7 | O8—Cl2—O7 | 109.9 (3) |
N3—C6—H6 | 125.7 | O9—Cl2—O7 | 110.6 (2) |
C7—N5—C9 | 105.9 (3) | O8—Cl2—O6 | 108.8 (4) |
C7—N5—Rh1 | 113.8 (2) | O9—Cl2—O6 | 108.0 (3) |
C9—N5—Rh1 | 139.7 (3) | O7—Cl2—O6 | 106.5 (3) |
| | | |
N1—Rh1—Rh1i—N5i | 40.76 (12) | N3—Rh1—N5—C7 | |
N3—Rh1—Rh1i—N7i | 41.15 (12) | O1—Rh1—N5—C7 | |
N7—Rh1—N1—C1 | | Rh1—Rh1i—N5—C7 | |
N5—Rh1—N1—C1 | | N7—Rh1—N5—C9 | |
N3—Rh1—N1—C1 | | N1—Rh1—N5—C9 | |
O1—Rh1—N1—C1 | | N3—Rh1—N5—C9 | |
Rh1—Rh1i—N1—C1 | | O1—Rh1—N5—C9 | |
N7—Rh1—N1—C3 | | Rh1—Rh1i—N5—C9 | |
N5—Rh1—N1—C3 | | C9—N5—C7—N6 | |
N3—Rh1—N1—C3 | | Rh1—N5—C7—N6 | |
O1—Rh1—N1—C3 | | C9—N5—C7—C10 | |
Rh1—Rh1i—N1—C3 | | Rh1—N5—C7—C10 | |
C3—N1—C1—N2 | | N5—C7—N6—C8 | |
Rh1—N1—C1—N2 | | C10—C7—N6—C8 | |
C3—N1—C1—C4 | | C7—N6—C8—C9 | |
Rh1—N1—C1—C4 | | N6—C8—C9—N5 | |
N1—C1—N2—C2 | | C7—N5—C9—C8 | |
C4—C1—N2—C2 | | Rh1—N5—C9—C8 | |
C1—N2—C2—C3 | | N5—Rh1—N7—C10 | |
C1—N1—C3—C2 | | N1—Rh1—N7—C10 | |
Rh1—N1—C3—C2 | | N3—Rh1—N7—C10 | |
N2—C2—C3—N1 | | O1—Rh1—N7—C10 | |
N7—Rh1—N3—C4 | | Rh1—Rh1i—N7—C10 | |
N5—Rh1—N3—C4 | | N5—Rh1—N7—C12 | |
N1—Rh1—N3—C4 | | N1—Rh1—N7—C12 | |
O1—Rh1—N3—C4 | | N3—Rh1—N7—C12 | |
Rh1—Rh1i—N3—C4 | | O1—Rh1—N7—C12 | |
N7—Rh1—N3—C6 | | Rh1—Rh1i—N7—C12 | |
N5—Rh1—N3—C6 | | C12—N7—C10—N8 | |
N1—Rh1—N3—C6 | | Rh1—N7—C10—N8 | |
O1—Rh1—N3—C6 | | C12—N7—C10—C7 | |
Rh1—Rh1i—N3—C6 | | Rh1—N7—C10—C7 | |
C6—N3—C4—N4 | | N6—C7—C10—N7 | |
Rh1—N3—C4—N4 | | N5—C7—C10—N7 | |
C6—N3—C4—C1 | | N6—C7—C10—N8 | |
Rh1—N3—C4—C1 | | N5—C7—C10—N8 | |
N1—C1—C4—N4 | | N7—C10—N8—C11 | |
N2—C1—C4—N4 | | C7—C10—N8—C11 | |
N1—C1—C4—N3 | | C10—N8—C11—C12 | |
N2—C1—C4—N3 | | N8—C11—C12—N7 | |
N3—C4—N4—C5 | | C10—N7—C12—C11 | |
C1—C4—N4—C5 | | Rh1—N7—C12—C11 | |
C4—N4—C5—C6 | | N7—Rh1—O1—C13 | |
N4—C5—C6—N3 | | N5—Rh1—O1—C13 | |
C4—N3—C6—C5 | | N1—Rh1—O1—C13 | |
Rh1—N3—C6—C5 | | N3—Rh1—O1—C13 | |
N7—Rh1—N5—C7 | | Rh1—Rh1i—O1—C13 | |
N1—Rh1—N5—C7 | | | |
Symmetry code: (i) −x+1, y, −z+3/2. |
Hydrogen-bond geometry (Å, º) top
D—H···A | D—H | H···A | D···A | D—H···A |
N2—H2N···O2 | 0.86 | 1.98 | 2.833 (5) | 172 |
N4—H4N···O3 | 0.86 | 2.25 | 3.053 (6) | 156 |
N6—H6N···O6 | 0.86 | 2.04 | 2.897 (5) | 177 |
N8—H8N···O7 | 0.86 | 1.96 | 2.808 (5) | 170 |
O1—H1···O4ii | 0.81 (2) | 2.15 (2) | 2.929 (4) | 163 (5) |
Symmetry code: (ii) x−1/2, −y+1/2, −z+1. |
Crystal data top
C30H38N18O2Rh2·4(BF4) | F(000) = 2456 |
Mr = 1235.84 | Dx = 1.754 Mg m−3 |
Monoclinic, C2/c | Mo Kα radiation, λ = 0.71069 Å |
a = 16.073 (10) Å | Cell parameters from 4208 reflections |
b = 19.104 (11) Å | θ = 3.0–27.5° |
c = 16.399 (10) Å | µ = 0.82 mm−1 |
β = 111.673 (6)° | T = 296 K |
V = 4679 (5) Å3 | Prismatic, green |
Z = 4 | 0.47 × 0.38 × 0.23 mm |
Data collection top
Rigaku/MSC Mercury CCD diffractometer | 5356 independent reflections |
Radiation source: rotating-anode X-ray tube | 3475 reflections with I > 2σ(I) |
Graphite monochromator | Rint = 0.056 |
Detector resolution: 14.62 pixels mm-1 | θmax = 27.5°, θmin = 3.0° |
ω scans | h = −20→20 |
Absorption correction: numerical NUMABS (Higashi, 1999) | k = −22→24 |
Tmin = 0.765, Tmax = 0.891 | l = −20→21 |
17721 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)] = 0.066 | Hydrogen site location: inferred from neighbouring sites |
wR(F2) = 0.213 | H-atom parameters constrained |
S = 1.05 | w = 1/[σ2(Fo2) + (0.1143P)2 + 8.0854P] where P = (Fo2 + 2Fc2)/3 |
5356 reflections | (Δ/σ)max < 0.001 |
392 parameters | Δρmax = 2.60 e Å−3 |
474 restraints | Δρmin = −0.94 e Å−3 |
Crystal data top
C30H38N18O2Rh2·4(BF4) | V = 4679 (5) Å3 |
Mr = 1235.84 | Z = 4 |
Monoclinic, C2/c | Mo Kα radiation |
a = 16.073 (10) Å | µ = 0.82 mm−1 |
b = 19.104 (11) Å | T = 296 K |
c = 16.399 (10) Å | 0.47 × 0.38 × 0.23 mm |
β = 111.673 (6)° | |
Data collection top
Rigaku/MSC Mercury CCD diffractometer | 5356 independent reflections |
Absorption correction: numerical NUMABS (Higashi, 1999) | 3475 reflections with I > 2σ(I) |
Tmin = 0.765, Tmax = 0.891 | Rint = 0.056 |
17721 measured reflections | |
Refinement top
R[F2 > 2σ(F2)] = 0.066 | 474 restraints |
wR(F2) = 0.213 | H-atom parameters constrained |
S = 1.05 | Δρmax = 2.60 e Å−3 |
5356 reflections | Δρmin = −0.94 e Å−3 |
392 parameters | |
Special details top
Geometry. All e.s.d.'s (except the e.s.d. in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell e.s.d.'s are taken into account individually in the estimation of e.s.d.'s in distances, angles and torsion angles; correlations between e.s.d.'s in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell e.s.d.'s is used for estimating e.s.d.'s involving l.s. planes. |
Refinement. Refinement of F2 against ALL reflections. The weighted R-factor wR and goodness of fit S are based on F2, conventional R-factors R are based on F, with F set to zero for negative F2. The threshold expression of F2 > σ(F2) is used only for calculating R-factors(gt) etc. and is not relevant to the choice of reflections for refinement. R-factors based on F2 are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger. |
Fractional atomic coordinates and isotropic or equivalent isotropic displacement parameters (Å2) top | x | y | z | Uiso*/Ueq | Occ. (<1) |
Rh1 | 0.41335 (3) | 0.249529 (18) | 0.23305 (3) | 0.03572 (19) | |
N1 | 0.4147 (3) | 0.1473 (2) | 0.2727 (3) | 0.0445 (10) | |
C1 | 0.3907 (4) | 0.1019 (3) | 0.2065 (4) | 0.0484 (13) | |
N2 | 0.3880 (4) | 0.0366 (3) | 0.2348 (4) | 0.0600 (14) | |
H2N | 0.3739 | −0.0006 | 0.2031 | 0.072* | |
C2 | 0.4115 (5) | 0.0404 (3) | 0.3226 (4) | 0.0667 (18) | |
H2 | 0.4163 | 0.0031 | 0.3605 | 0.080* | |
C3 | 0.4269 (4) | 0.1089 (3) | 0.3455 (4) | 0.0547 (15) | |
H3 | 0.4432 | 0.1265 | 0.4022 | 0.066* | |
N3 | 0.3833 (3) | 0.1988 (2) | 0.1155 (3) | 0.0461 (10) | |
C4 | 0.3711 (4) | 0.1304 (3) | 0.1198 (4) | 0.0491 (13) | |
N4 | 0.3405 (3) | 0.1017 (3) | 0.0403 (3) | 0.0596 (13) | |
H4N | 0.3281 | 0.0582 | 0.0281 | 0.071* | |
C5 | 0.3327 (4) | 0.1545 (4) | −0.0182 (4) | 0.0645 (17) | |
H5 | 0.3131 | 0.1502 | −0.0789 | 0.077* | |
C6 | 0.3589 (4) | 0.2139 (3) | 0.0285 (4) | 0.0576 (15) | |
H6 | 0.3601 | 0.2581 | 0.0052 | 0.069* | |
N5 | 0.4278 (3) | 0.2999 (2) | 0.3473 (3) | 0.0448 (10) | |
C7 | 0.4072 (4) | 0.3678 (3) | 0.3355 (4) | 0.0482 (13) | |
N6 | 0.4012 (4) | 0.3952 (3) | 0.4078 (3) | 0.0696 (16) | |
H6N | 0.3886 | 0.4380 | 0.4148 | 0.084* | |
C8 | 0.4183 (5) | 0.3433 (4) | 0.4682 (4) | 0.075 (2) | |
H8 | 0.4197 | 0.3476 | 0.5252 | 0.090* | |
C9 | 0.4330 (4) | 0.2843 (3) | 0.4305 (4) | 0.0551 (14) | |
H9 | 0.4447 | 0.2404 | 0.4566 | 0.066* | |
N7 | 0.4008 (3) | 0.3510 (2) | 0.1913 (3) | 0.0442 (10) | |
C10 | 0.3940 (4) | 0.3959 (3) | 0.2500 (4) | 0.0494 (13) | |
N8 | 0.3768 (5) | 0.4606 (3) | 0.2165 (4) | 0.0656 (15) | |
H8N | 0.3695 | 0.4976 | 0.2431 | 0.079* | |
C11 | 0.3732 (5) | 0.4568 (3) | 0.1329 (4) | 0.0699 (19) | |
H11 | 0.3625 | 0.4938 | 0.0935 | 0.084* | |
C12 | 0.3880 (4) | 0.3886 (3) | 0.1169 (4) | 0.0517 (14) | |
H12 | 0.3892 | 0.3710 | 0.0645 | 0.062* | |
O1 | 0.2648 (3) | 0.2572 (2) | 0.2061 (3) | 0.0508 (11) | |
C13 | 0.2404 (4) | 0.2318 (4) | 0.2615 (5) | 0.0620 (17) | |
H13 | 0.2794 | 0.2013 | 0.3020 | 0.074* | |
N9 | 0.1626 (4) | 0.2445 (3) | 0.2685 (5) | 0.0694 (18) | |
C14 | 0.1026 (7) | 0.2945 (7) | 0.2105 (7) | 0.133 (5) | |
H14 | 0.1353 | 0.3358 | 0.2074 | 0.200* | |
H14A | 0.0567 | 0.3066 | 0.2324 | 0.200* | |
H14B | 0.0756 | 0.2745 | 0.1530 | 0.200* | |
C15 | 0.1370 (6) | 0.2101 (6) | 0.3350 (6) | 0.102 (3) | |
H15 | 0.1793 | 0.1738 | 0.3628 | 0.154* | |
H15A | 0.0784 | 0.1900 | 0.3079 | 0.154* | |
H15B | 0.1363 | 0.2438 | 0.3782 | 0.154* | |
B1 | 0.3728 (6) | 0.5813 (4) | 0.3763 (5) | 0.084 (2) | |
F1 | 0.3661 (4) | 0.6447 (2) | 0.4079 (3) | 0.119 (2) | |
F2A | 0.3234 (11) | 0.5794 (7) | 0.2867 (6) | 0.097 (5) | 0.54 (3) |
F3A | 0.4522 (8) | 0.5549 (8) | 0.3920 (12) | 0.135 (6) | 0.54 (3) |
F4A | 0.3269 (15) | 0.5346 (6) | 0.4113 (12) | 0.135 (6) | 0.54 (3) |
F2B | 0.3065 (11) | 0.5591 (12) | 0.3080 (13) | 0.138 (8) | 0.46 (3) |
F3B | 0.4468 (12) | 0.5868 (13) | 0.3499 (17) | 0.162 (8) | 0.46 (3) |
F4B | 0.399 (3) | 0.5367 (7) | 0.4449 (9) | 0.159 (10) | 0.46 (3) |
B2A | 0.3488 (12) | −0.0920 (9) | 0.0443 (9) | 0.116 (6) | 0.421 (17) |
B2B | 0.3638 (10) | −0.0916 (7) | 0.0493 (8) | 0.118 (5) | 0.579 (17) |
F5 | 0.3608 (7) | −0.0812 (4) | 0.1280 (4) | 0.204 (4) | |
F6A | 0.2633 (11) | −0.1049 (16) | −0.0042 (11) | 0.216 (11) | 0.421 (17) |
F7A | 0.3754 (16) | −0.0348 (8) | 0.0129 (11) | 0.149 (8) | 0.421 (17) |
F8A | 0.3993 (17) | −0.1463 (9) | 0.0386 (12) | 0.149 (9) | 0.421 (17) |
F6B | 0.4504 (8) | −0.0890 (11) | 0.0576 (10) | 0.202 (8) | 0.579 (17) |
F7B | 0.3295 (13) | −0.1534 (6) | 0.0162 (9) | 0.167 (8) | 0.579 (17) |
F8B | 0.3172 (11) | −0.0413 (7) | −0.0046 (9) | 0.176 (7) | 0.579 (17) |
Atomic displacement parameters (Å2) top | U11 | U22 | U33 | U12 | U13 | U23 |
Rh1 | 0.0436 (3) | 0.0330 (3) | 0.0329 (3) | −0.00020 (14) | 0.0169 (2) | 0.00079 (13) |
N1 | 0.059 (3) | 0.031 (2) | 0.045 (2) | −0.0035 (19) | 0.021 (2) | 0.0014 (18) |
C1 | 0.058 (3) | 0.035 (3) | 0.057 (3) | −0.005 (2) | 0.027 (3) | 0.003 (2) |
N2 | 0.087 (4) | 0.031 (3) | 0.067 (3) | −0.008 (2) | 0.034 (3) | −0.002 (2) |
C2 | 0.094 (5) | 0.041 (3) | 0.070 (4) | −0.001 (3) | 0.036 (4) | 0.013 (3) |
C3 | 0.064 (3) | 0.059 (4) | 0.045 (3) | −0.005 (3) | 0.025 (3) | 0.006 (3) |
N3 | 0.053 (2) | 0.043 (3) | 0.042 (2) | 0.0028 (19) | 0.018 (2) | −0.0011 (19) |
C4 | 0.062 (3) | 0.039 (3) | 0.046 (3) | −0.003 (2) | 0.020 (3) | −0.005 (2) |
N4 | 0.077 (3) | 0.046 (3) | 0.049 (3) | −0.007 (2) | 0.016 (2) | −0.010 (2) |
C5 | 0.084 (4) | 0.068 (4) | 0.045 (3) | −0.008 (3) | 0.026 (3) | −0.009 (3) |
C6 | 0.080 (4) | 0.050 (4) | 0.049 (3) | −0.001 (3) | 0.030 (3) | 0.006 (3) |
N5 | 0.055 (2) | 0.041 (2) | 0.041 (2) | 0.0014 (19) | 0.022 (2) | 0.0005 (18) |
C7 | 0.064 (3) | 0.043 (3) | 0.042 (3) | 0.005 (3) | 0.025 (3) | 0.001 (2) |
N6 | 0.115 (5) | 0.052 (3) | 0.057 (3) | 0.008 (3) | 0.049 (3) | −0.006 (2) |
C8 | 0.116 (6) | 0.067 (5) | 0.053 (4) | 0.006 (4) | 0.044 (4) | 0.000 (3) |
C9 | 0.073 (4) | 0.054 (4) | 0.048 (3) | −0.003 (3) | 0.034 (3) | 0.001 (3) |
N7 | 0.055 (2) | 0.039 (2) | 0.038 (2) | −0.0002 (19) | 0.0163 (19) | 0.0001 (18) |
C10 | 0.067 (3) | 0.034 (3) | 0.050 (3) | 0.004 (2) | 0.025 (3) | −0.003 (2) |
N8 | 0.115 (5) | 0.028 (3) | 0.056 (3) | 0.012 (3) | 0.034 (3) | 0.006 (2) |
C11 | 0.112 (6) | 0.043 (4) | 0.057 (4) | 0.010 (3) | 0.032 (4) | 0.010 (3) |
C12 | 0.069 (4) | 0.046 (3) | 0.039 (3) | 0.004 (3) | 0.018 (3) | 0.007 (2) |
O1 | 0.052 (2) | 0.057 (3) | 0.052 (3) | −0.0021 (16) | 0.030 (2) | 0.0060 (17) |
C13 | 0.051 (3) | 0.070 (4) | 0.064 (4) | 0.003 (3) | 0.020 (3) | 0.000 (3) |
N9 | 0.066 (4) | 0.093 (5) | 0.070 (4) | 0.006 (3) | 0.049 (3) | 0.015 (3) |
C14 | 0.096 (6) | 0.196 (13) | 0.131 (9) | 0.061 (8) | 0.069 (7) | 0.075 (9) |
C15 | 0.106 (6) | 0.124 (8) | 0.104 (6) | 0.009 (6) | 0.070 (6) | 0.026 (6) |
B1 | 0.125 (6) | 0.065 (5) | 0.059 (4) | 0.031 (5) | 0.029 (4) | −0.009 (3) |
F1 | 0.190 (5) | 0.070 (3) | 0.084 (3) | 0.045 (3) | 0.033 (3) | −0.010 (2) |
F2A | 0.144 (11) | 0.071 (6) | 0.065 (5) | 0.021 (6) | 0.026 (5) | −0.003 (4) |
F3A | 0.124 (7) | 0.107 (11) | 0.141 (13) | 0.045 (7) | 0.012 (7) | −0.043 (10) |
F4A | 0.207 (15) | 0.101 (7) | 0.114 (11) | 0.026 (8) | 0.077 (11) | 0.021 (7) |
F2B | 0.096 (8) | 0.176 (18) | 0.130 (11) | 0.011 (10) | 0.027 (9) | −0.077 (12) |
F3B | 0.126 (10) | 0.23 (2) | 0.143 (16) | 0.007 (11) | 0.067 (11) | −0.048 (13) |
F4B | 0.31 (3) | 0.066 (7) | 0.087 (8) | 0.068 (12) | 0.062 (12) | 0.000 (6) |
B2A | 0.173 (14) | 0.068 (12) | 0.114 (11) | −0.016 (11) | 0.060 (13) | −0.041 (13) |
B2B | 0.193 (12) | 0.062 (10) | 0.097 (10) | −0.016 (10) | 0.051 (12) | −0.014 (9) |
F5 | 0.363 (11) | 0.135 (6) | 0.136 (5) | −0.021 (6) | 0.118 (6) | −0.060 (4) |
F6A | 0.185 (14) | 0.16 (2) | 0.252 (19) | −0.056 (12) | 0.026 (15) | −0.046 (16) |
F7A | 0.23 (2) | 0.056 (8) | 0.185 (16) | −0.011 (10) | 0.106 (17) | −0.026 (9) |
F8A | 0.27 (2) | 0.073 (10) | 0.141 (15) | 0.035 (14) | 0.119 (16) | 0.009 (10) |
F6B | 0.162 (9) | 0.212 (19) | 0.198 (14) | 0.002 (10) | 0.025 (9) | −0.054 (13) |
F7B | 0.261 (19) | 0.065 (6) | 0.140 (10) | −0.024 (9) | 0.035 (13) | −0.046 (6) |
F8B | 0.218 (15) | 0.074 (8) | 0.171 (9) | 0.021 (9) | −0.002 (11) | −0.013 (7) |
Geometric parameters (Å, º) top
Rh1—N7 | 2.041 (5) | N7—C12 | 1.364 (7) |
Rh1—N5 | 2.042 (4) | C10—N8 | 1.339 (7) |
Rh1—N3 | 2.049 (4) | N8—C11 | 1.353 (9) |
Rh1—N1 | 2.057 (4) | N8—H8N | 0.8600 |
Rh1—O1 | 2.266 (5) | C11—C12 | 1.366 (9) |
Rh1—Rh1i | 2.6313 (18) | C11—H11 | 0.9300 |
N1—C1 | 1.331 (7) | C12—H12 | 0.9300 |
N1—C3 | 1.352 (7) | O1—C13 | 1.216 (9) |
C1—N2 | 1.337 (7) | C13—N9 | 1.319 (9) |
C1—C4 | 1.444 (8) | C13—H13 | 0.9300 |
N2—C2 | 1.350 (8) | N9—C14 | 1.439 (11) |
N2—H2N | 0.8600 | N9—C15 | 1.458 (10) |
C2—C3 | 1.358 (9) | C14—H14 | 0.9600 |
C2—H2 | 0.9300 | C14—H14A | 0.9600 |
C3—H3 | 0.9300 | C14—H14B | 0.9600 |
N3—C4 | 1.328 (7) | C15—H15 | 0.9600 |
N3—C6 | 1.363 (7) | C15—H15A | 0.9600 |
C4—N4 | 1.331 (7) | C15—H15B | 0.9600 |
N4—C5 | 1.365 (8) | B1—F2B | 1.300 (11) |
N4—H4N | 0.8600 | B1—F3A | 1.306 (10) |
C5—C6 | 1.348 (9) | B1—F1 | 1.338 (8) |
C5—H5 | 0.9300 | B1—F4B | 1.349 (10) |
C6—H6 | 0.9300 | B1—F2A | 1.389 (10) |
N5—C7 | 1.336 (7) | B1—F4A | 1.408 (11) |
N5—C9 | 1.368 (7) | B1—F3B | 1.412 (12) |
C7—N6 | 1.332 (7) | B2A—F5 | 1.330 (13) |
C7—C10 | 1.442 (8) | B2A—F6A | 1.333 (14) |
N6—C8 | 1.357 (8) | B2A—F8A | 1.341 (14) |
N6—H6N | 0.8600 | B2A—F7A | 1.344 (14) |
C8—C9 | 1.348 (9) | B2B—F5 | 1.324 (13) |
C8—H8 | 0.9300 | B2B—F7B | 1.331 (13) |
C9—H9 | 0.9300 | B2B—F8B | 1.333 (13) |
N7—C10 | 1.324 (7) | B2B—F6B | 1.350 (13) |
| | | |
N7—Rh1—N5 | 79.88 (18) | N5—C9—H9 | 125.7 |
N7—Rh1—N3 | 99.97 (18) | C10—N7—C12 | 106.4 (5) |
N5—Rh1—N3 | 173.40 (17) | C10—N7—Rh1 | 113.3 (4) |
N7—Rh1—N1 | 175.25 (17) | C12—N7—Rh1 | 139.9 (4) |
N5—Rh1—N1 | 99.96 (18) | N7—C10—N8 | 111.1 (5) |
N3—Rh1—N1 | 79.63 (18) | N7—C10—C7 | 116.3 (5) |
N7—Rh1—O1 | 84.66 (16) | N8—C10—C7 | 132.5 (6) |
N5—Rh1—O1 | 84.44 (17) | C10—N8—C11 | 106.9 (5) |
N3—Rh1—O1 | 88.97 (17) | C10—N8—H8N | 126.6 |
N1—Rh1—O1 | 90.60 (16) | C11—N8—H8N | 126.6 |
N7—Rh1—Rh1i | 92.08 (13) | N8—C11—C12 | 107.5 (5) |
N5—Rh1—Rh1i | 93.04 (13) | N8—C11—H11 | 126.3 |
N3—Rh1—Rh1i | 93.55 (13) | C12—C11—H11 | 126.3 |
N1—Rh1—Rh1i | 92.67 (13) | N7—C12—C11 | 108.1 (5) |
O1—Rh1—Rh1i | 176.18 (10) | N7—C12—H12 | 125.9 |
C1—N1—C3 | 105.8 (5) | C11—C12—H12 | 125.9 |
C1—N1—Rh1 | 113.2 (4) | C13—O1—Rh1 | 115.8 (4) |
C3—N1—Rh1 | 140.8 (4) | O1—C13—N9 | 124.7 (7) |
N1—C1—N2 | 111.1 (5) | O1—C13—H13 | 117.7 |
N1—C1—C4 | 116.7 (5) | N9—C13—H13 | 117.7 |
N2—C1—C4 | 132.1 (6) | C13—N9—C14 | 119.4 (7) |
C1—N2—C2 | 106.7 (5) | C13—N9—C15 | 121.4 (7) |
C1—N2—H2N | 126.6 | C14—N9—C15 | 119.2 (7) |
C2—N2—H2N | 126.6 | N9—C14—H14 | 109.5 |
N2—C2—C3 | 107.3 (5) | N9—C14—H14A | 109.5 |
N2—C2—H2 | 126.3 | H14—C14—H14A | 109.5 |
C3—C2—H2 | 126.3 | N9—C14—H14B | 109.5 |
N1—C3—C2 | 109.0 (5) | H14—C14—H14B | 109.5 |
N1—C3—H3 | 125.5 | H14A—C14—H14B | 109.5 |
C2—C3—H3 | 125.5 | N9—C15—H15 | 109.5 |
C4—N3—C6 | 105.8 (5) | N9—C15—H15A | 109.5 |
C4—N3—Rh1 | 113.7 (4) | H15—C15—H15A | 109.5 |
C6—N3—Rh1 | 139.6 (4) | N9—C15—H15B | 109.5 |
N3—C4—N4 | 111.2 (5) | H15—C15—H15B | 109.5 |
N3—C4—C1 | 116.2 (5) | H15A—C15—H15B | 109.5 |
N4—C4—C1 | 132.6 (6) | F2B—B1—F1 | 118.2 (10) |
C4—N4—C5 | 106.8 (5) | F3A—B1—F1 | 119.1 (9) |
C4—N4—H4N | 126.6 | F2B—B1—F4B | 114.8 (11) |
C5—N4—H4N | 126.6 | F1—B1—F4B | 107.1 (7) |
C6—C5—N4 | 107.1 (5) | F3A—B1—F2A | 109.5 (9) |
C6—C5—H5 | 126.5 | F1—B1—F2A | 109.7 (7) |
N4—C5—H5 | 126.5 | F3A—B1—F4A | 107.2 (8) |
C5—C6—N3 | 109.0 (6) | F1—B1—F4A | 106.6 (8) |
C5—C6—H6 | 125.5 | F2A—B1—F4A | 103.5 (9) |
N3—C6—H6 | 125.5 | F2B—B1—F3B | 106.0 (10) |
C7—N5—C9 | 106.1 (5) | F1—B1—F3B | 104.4 (9) |
C7—N5—Rh1 | 112.7 (3) | F4B—B1—F3B | 105.0 (9) |
C9—N5—Rh1 | 139.2 (4) | F5—B2A—F6A | 111.6 (13) |
N6—C7—N5 | 110.4 (5) | F5—B2A—F8A | 109.3 (12) |
N6—C7—C10 | 133.3 (6) | F6A—B2A—F8A | 109.5 (13) |
N5—C7—C10 | 116.3 (5) | F5—B2A—F7A | 108.9 (12) |
C7—N6—C8 | 107.5 (5) | F6A—B2A—F7A | 109.0 (13) |
C7—N6—H6N | 126.2 | F8A—B2A—F7A | 108.4 (12) |
C8—N6—H6N | 126.2 | F5—B2B—F7B | 111.9 (12) |
C9—C8—N6 | 107.4 (6) | F5—B2B—F8B | 108.9 (12) |
C9—C8—H8 | 126.3 | F7B—B2B—F8B | 108.8 (12) |
N6—C8—H8 | 126.3 | F5—B2B—F6B | 107.7 (11) |
C8—C9—N5 | 108.6 (6) | F7B—B2B—F6B | 109.3 (12) |
C8—C9—H9 | 125.7 | F8B—B2B—F6B | 110.2 (12) |
| | | |
N1—Rh1—Rh1i—N3i | −43.72 (18) | O1—Rh1—N5—C7 | −74.8 (4) |
N5—Rh1—Rh1i—N7i | −43.72 (17) | Rh1i—Rh1—N5—C7 | 102.3 (4) |
N7—Rh1—N1—C1 | 81 (2) | N7—Rh1—N5—C9 | 171.5 (6) |
N5—Rh1—N1—C1 | 169.0 (4) | N3—Rh1—N5—C9 | 82.2 (16) |
N3—Rh1—N1—C1 | −4.3 (4) | N1—Rh1—N5—C9 | −3.7 (6) |
O1—Rh1—N1—C1 | 84.5 (4) | O1—Rh1—N5—C9 | 85.9 (6) |
Rh1i—Rh1—N1—C1 | −97.4 (4) | Rh1i—Rh1—N5—C9 | −97.0 (6) |
N7—Rh1—N1—C3 | −93 (2) | C9—N5—C7—N6 | 1.2 (7) |
N5—Rh1—N1—C3 | −5.4 (7) | Rh1—N5—C7—N6 | 168.2 (4) |
N3—Rh1—N1—C3 | −178.7 (7) | C9—N5—C7—C10 | −177.3 (5) |
O1—Rh1—N1—C3 | −89.8 (6) | Rh1—N5—C7—C10 | −10.3 (7) |
Rh1i—Rh1—N1—C3 | 88.2 (6) | N5—C7—N6—C8 | 0.0 (8) |
C3—N1—C1—N2 | −0.4 (7) | C10—C7—N6—C8 | 178.1 (7) |
Rh1—N1—C1—N2 | −176.7 (4) | C7—N6—C8—C9 | −1.2 (9) |
C3—N1—C1—C4 | 178.4 (5) | N6—C8—C9—N5 | 1.9 (8) |
Rh1—N1—C1—C4 | 2.1 (7) | C7—N5—C9—C8 | −1.9 (7) |
N1—C1—N2—C2 | −0.3 (8) | Rh1—N5—C9—C8 | −163.4 (5) |
C4—C1—N2—C2 | −178.8 (7) | N5—Rh1—N7—C10 | −9.7 (4) |
C1—N2—C2—C3 | 0.9 (8) | N3—Rh1—N7—C10 | 163.6 (4) |
C1—N1—C3—C2 | 1.0 (7) | N1—Rh1—N7—C10 | 79 (2) |
Rh1—N1—C3—C2 | 175.6 (5) | O1—Rh1—N7—C10 | 75.6 (4) |
N2—C2—C3—N1 | −1.2 (8) | Rh1i—Rh1—N7—C10 | −102.4 (4) |
N7—Rh1—N3—C4 | −169.1 (4) | N5—Rh1—N7—C12 | 179.1 (6) |
N5—Rh1—N3—C4 | −81.0 (15) | N3—Rh1—N7—C12 | −7.5 (6) |
N1—Rh1—N3—C4 | 6.1 (4) | N1—Rh1—N7—C12 | −92 (2) |
O1—Rh1—N3—C4 | −84.7 (4) | O1—Rh1—N7—C12 | −95.6 (6) |
Rh1i—Rh1—N3—C4 | 98.2 (4) | Rh1i—Rh1—N7—C12 | 86.4 (6) |
N7—Rh1—N3—C6 | −1.4 (7) | C12—N7—C10—N8 | 0.4 (7) |
N5—Rh1—N3—C6 | 86.7 (16) | Rh1—N7—C10—N8 | −173.7 (4) |
N1—Rh1—N3—C6 | 173.8 (7) | C12—N7—C10—C7 | −178.7 (5) |
O1—Rh1—N3—C6 | 83.0 (6) | Rh1—N7—C10—C7 | 7.2 (7) |
Rh1i—Rh1—N3—C6 | −94.2 (6) | N6—C7—C10—N7 | −175.9 (7) |
C6—N3—C4—N4 | 0.2 (7) | N5—C7—C10—N7 | 2.1 (8) |
Rh1—N3—C4—N4 | 171.9 (4) | N6—C7—C10—N8 | 5.1 (13) |
C6—N3—C4—C1 | −178.6 (5) | N5—C7—C10—N8 | −176.8 (7) |
Rh1—N3—C4—C1 | −6.9 (7) | N7—C10—N8—C11 | −0.5 (8) |
N1—C1—C4—N3 | 3.2 (8) | C7—C10—N8—C11 | 178.5 (7) |
N2—C1—C4—N3 | −178.3 (6) | C10—N8—C11—C12 | 0.3 (9) |
N1—C1—C4—N4 | −175.2 (6) | C10—N7—C12—C11 | −0.2 (7) |
N2—C1—C4—N4 | 3.3 (12) | Rh1—N7—C12—C11 | 171.3 (5) |
N3—C4—N4—C5 | 0.0 (7) | N8—C11—C12—N7 | −0.1 (8) |
C1—C4—N4—C5 | 178.5 (7) | N7—Rh1—O1—C13 | −136.6 (5) |
C4—N4—C5—C6 | −0.2 (7) | N5—Rh1—O1—C13 | −56.3 (5) |
N4—C5—C6—N3 | 0.3 (8) | N3—Rh1—O1—C13 | 123.3 (5) |
C4—N3—C6—C5 | −0.3 (7) | N1—Rh1—O1—C13 | 43.7 (5) |
Rh1—N3—C6—C5 | −168.5 (5) | Rh1i—Rh1—O1—C13 | −105.3 (17) |
N7—Rh1—N5—C7 | 10.7 (4) | Rh1—O1—C13—N9 | 163.8 (6) |
N3—Rh1—N5—C7 | −78.6 (15) | O1—C13—N9—C14 | −3.6 (13) |
N1—Rh1—N5—C7 | −164.4 (4) | O1—C13—N9—C15 | 177.8 (8) |
Symmetry code: (i) −x+1, y, −z+1/2. |
Hydrogen-bond geometry (Å, º) top
D—H···A | D—H | H···A | D···A | D—H···A |
N2—H2N···F5 | 0.86 | 1.93 | 2.786 (8) | 170 |
N4—H4N···F8B | 0.86 | 1.97 | 2.818 (15) | 171 |
N4—H4N···F7A | 0.86 | 1.98 | 2.738 (17) | 146 |
N6—H6N···F4B | 0.86 | 1.94 | 2.773 (13) | 163 |
N6—H6N···F4A | 0.86 | 2.09 | 2.927 (16) | 166 |
N6—H6N···F3A | 0.86 | 2.54 | 3.19 (2) | 134 |
N8—H8N···F2A | 0.86 | 1.97 | 2.817 (15) | 167 |
N8—H8N···F2B | 0.86 | 2.08 | 2.884 (19) | 155 |
N8—H8N···F3B | 0.86 | 2.43 | 3.169 (19) | 144 |
N8—H8N···F3A | 0.86 | 2.56 | 3.227 (15) | 136 |
Crystal data top
C36H38N18Rh2·2(SiF6)·8(H2O) | Dx = 1.726 Mg m−3 |
Mr = 1356.97 | Mo Kα radiation, λ = 0.71069 Å |
Tetragonal, I4122 | Cell parameters from 14243 reflections |
a = 17.6300 (5) Å | θ = 3.0–27.5° |
c = 16.8037 (6) Å | µ = 0.79 mm−1 |
V = 5222.9 (3) Å3 | T = 296 K |
Z = 4 | Prismatic, red |
F(000) = 2744 | 0.41 × 0.40 × 0.40 mm |
Data collection top
Rigaku/MSC Mercury CCD diffractometer | 3004 independent reflections |
Radiation source: rotating-anode X-ray tube | 2952 reflections with I > 2σ(I) |
Graphite monochromator | Rint = 0.024 |
Detector resolution: 14.62 pixels mm-1 | θmax = 27.5°, θmin = 3.3° |
ω scans | h = −22→21 |
Absorption correction: numerical NUMABS (Higashi, 1999) | k = −22→22 |
Tmin = 0.727, Tmax = 0.814 | l = −14→21 |
20508 measured reflections | |
Refinement top
Refinement on F2 | Secondary atom site location: difference Fourier map |
Least-squares matrix: full | Hydrogen site location: inferred from neighbouring sites |
R[F2 > 2σ(F2)] = 0.027 | H atoms treated by a mixture of independent and constrained refinement |
wR(F2) = 0.073 | w = 1/[σ2(Fo2) + (0.0493P)2 + 1.975P] where P = (Fo2 + 2Fc2)/3 |
S = 1.12 | (Δ/σ)max = 0.001 |
3004 reflections | Δρmax = 0.80 e Å−3 |
220 parameters | Δρmin = −0.36 e Å−3 |
15 restraints | Absolute structure: Flack H D (1983), Acta Cryst. A39, 876-881 |
Primary atom site location: structure-invariant direct methods | Absolute structure parameter: −0.02 (3) |
Crystal data top
C36H38N18Rh2·2(SiF6)·8(H2O) | Z = 4 |
Mr = 1356.97 | Mo Kα radiation |
Tetragonal, I4122 | µ = 0.79 mm−1 |
a = 17.6300 (5) Å | T = 296 K |
c = 16.8037 (6) Å | 0.41 × 0.40 × 0.40 mm |
V = 5222.9 (3) Å3 | |
Data collection top
Rigaku/MSC Mercury CCD diffractometer | 3004 independent reflections |
Absorption correction: numerical NUMABS (Higashi, 1999) | 2952 reflections with I > 2σ(I) |
Tmin = 0.727, Tmax = 0.814 | Rint = 0.024 |
20508 measured reflections | |
Refinement top
R[F2 > 2σ(F2)] = 0.027 | H atoms treated by a mixture of independent and constrained refinement |
wR(F2) = 0.073 | Δρmax = 0.80 e Å−3 |
S = 1.12 | Δρmin = −0.36 e Å−3 |
3004 reflections | Absolute structure: Flack H D (1983), Acta Cryst. A39, 876-881 |
220 parameters | Absolute structure parameter: −0.02 (3) |
15 restraints | |
Special details top
Geometry. All e.s.d.'s (except the e.s.d. in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell e.s.d.'s are taken into account individually in the estimation of e.s.d.'s in distances, angles and torsion angles; correlations between e.s.d.'s in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell e.s.d.'s is used for estimating e.s.d.'s involving l.s. planes. |
Refinement. Refinement of F2 against ALL reflections. The weighted R-factor wR and goodness of fit S are based on F2, conventional R-factors R are based on F, with F set to zero for negative F2. The threshold expression of F2 > σ(F2) is used only for calculating R-factors(gt) etc. and is not relevant to the choice of reflections for refinement. R-factors based on F2 are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger. |
Fractional atomic coordinates and isotropic or equivalent isotropic displacement parameters (Å2) top | x | y | z | Uiso*/Ueq | Occ. (<1) |
Rh1 | 0.445750 (10) | 0.445750 (10) | 0.0000 | 0.02735 (9) | |
N1 | 0.36851 (12) | 0.51661 (12) | 0.05284 (12) | 0.0312 (4) | |
C1 | 0.36143 (16) | 0.50496 (15) | 0.13091 (16) | 0.0367 (5) | |
N2 | 0.30158 (14) | 0.54327 (15) | 0.15982 (15) | 0.0441 (5) | |
H2N | 0.2866 | 0.5440 | 0.2085 | 0.053* | |
C2 | 0.26894 (16) | 0.58083 (16) | 0.09758 (19) | 0.0423 (6) | |
H2 | 0.2263 | 0.6118 | 0.0999 | 0.051* | |
C3 | 0.31059 (14) | 0.56455 (15) | 0.03147 (18) | 0.0365 (5) | |
H3 | 0.3014 | 0.5828 | −0.0195 | 0.044* | |
N3 | 0.46441 (13) | 0.42079 (13) | 0.11796 (13) | 0.0353 (4) | |
C4 | 0.41519 (17) | 0.45467 (15) | 0.16714 (15) | 0.0387 (5) | |
N4 | 0.42891 (19) | 0.43573 (15) | 0.24257 (14) | 0.0550 (6) | |
H4N | 0.4047 | 0.4516 | 0.2838 | 0.066* | |
C5 | 0.4885 (2) | 0.3865 (2) | 0.2420 (2) | 0.0606 (9) | |
H5 | 0.5104 | 0.3636 | 0.2863 | 0.073* | |
C6 | 0.5098 (2) | 0.37689 (17) | 0.16603 (18) | 0.0465 (6) | |
H6 | 0.5490 | 0.3456 | 0.1487 | 0.056* | |
N5 | 0.35452 (13) | 0.35452 (13) | 0.0000 | 0.0423 (6) | |
C7 | 0.3687 (2) | 0.2847 (3) | 0.0156 (5) | 0.124 (3) | |
H7 | 0.4187 | 0.2714 | 0.0266 | 0.148* | |
C8 | 0.3152 (3) | 0.2287 (3) | 0.0172 (6) | 0.157 (4) | |
H8 | 0.3298 | 0.1796 | 0.0307 | 0.189* | |
C9 | 0.2425 (2) | 0.2425 (2) | 0.0000 | 0.0865 (19) | |
C10 | 0.1817 (3) | 0.1817 (3) | 0.0000 | 0.163 (6) | |
H10A | 0.1340 | 0.2038 | −0.0150 | 0.245* | 0.50 |
H10B | 0.1776 | 0.1602 | 0.0523 | 0.245* | 0.50 |
H10C | 0.1951 | 0.1427 | −0.0373 | 0.245* | 0.50 |
Si1 | 0.22790 (15) | 0.54844 (14) | 0.3697 (2) | 0.0739 (10) | 0.50 |
F1 | 0.1635 (7) | 0.4809 (4) | 0.3825 (6) | 0.146 (4) | 0.50 |
F2 | 0.2708 (7) | 0.5186 (7) | 0.4520 (4) | 0.128 (4) | 0.50 |
F3 | 0.2914 (7) | 0.6168 (6) | 0.3578 (7) | 0.149 (4) | 0.50 |
F4 | 0.2837 (6) | 0.4894 (4) | 0.3167 (4) | 0.096 (2) | 0.50 |
F5 | 0.1905 (6) | 0.5772 (7) | 0.2878 (4) | 0.131 (3) | 0.50 |
F6 | 0.1762 (6) | 0.6065 (5) | 0.4258 (5) | 0.114 (3) | 0.50 |
O1 | 0.34398 (18) | 0.7500 | 0.1250 | 0.0542 (7) | |
O2 | 0.23366 (16) | 0.73366 (16) | 0.2500 | 0.0739 (10) | |
O4 | 0.4094 (13) | 0.4941 (15) | 0.5655 (11) | 0.270 (11) | 0.50 |
O3 | 0.4212 (10) | 0.4807 (14) | 0.3987 (10) | 0.242 (10) | 0.50 |
Atomic displacement parameters (Å2) top | U11 | U22 | U33 | U12 | U13 | U23 |
Rh1 | 0.03114 (10) | 0.03114 (10) | 0.01978 (12) | 0.00846 (8) | 0.00059 (6) | −0.00059 (6) |
N1 | 0.0344 (10) | 0.0350 (10) | 0.0241 (9) | 0.0057 (8) | 0.0019 (8) | −0.0024 (7) |
C1 | 0.0447 (13) | 0.0372 (12) | 0.0282 (12) | 0.0073 (11) | 0.0093 (10) | −0.0024 (10) |
N2 | 0.0462 (12) | 0.0473 (13) | 0.0388 (13) | 0.0053 (10) | 0.0173 (10) | −0.0091 (10) |
C2 | 0.0355 (12) | 0.0398 (13) | 0.0517 (17) | 0.0075 (10) | 0.0066 (12) | −0.0097 (12) |
C3 | 0.0339 (11) | 0.0322 (12) | 0.0434 (13) | 0.0047 (9) | −0.0044 (10) | −0.0007 (10) |
N3 | 0.0436 (11) | 0.0369 (10) | 0.0255 (10) | 0.0085 (9) | 0.0007 (8) | 0.0007 (8) |
C4 | 0.0529 (14) | 0.0397 (13) | 0.0234 (11) | 0.0061 (11) | 0.0068 (10) | 0.0002 (10) |
N4 | 0.0895 (19) | 0.0537 (14) | 0.0219 (10) | 0.0183 (11) | 0.0079 (12) | 0.0059 (10) |
C5 | 0.091 (2) | 0.0585 (17) | 0.0322 (16) | 0.0159 (17) | −0.0100 (17) | 0.0105 (15) |
C6 | 0.0608 (18) | 0.0420 (15) | 0.0368 (14) | 0.0142 (12) | −0.0055 (13) | 0.0068 (12) |
N5 | 0.0424 (9) | 0.0424 (9) | 0.0421 (16) | 0.0122 (12) | 0.0013 (11) | −0.0013 (11) |
C7 | 0.0434 (18) | 0.068 (3) | 0.260 (9) | 0.0111 (17) | 0.022 (3) | 0.080 (4) |
C8 | 0.063 (2) | 0.063 (2) | 0.347 (13) | 0.0024 (19) | 0.011 (5) | 0.086 (5) |
C9 | 0.0553 (16) | 0.0553 (16) | 0.149 (6) | −0.006 (2) | 0.008 (3) | −0.008 (3) |
C10 | 0.087 (4) | 0.087 (4) | 0.316 (17) | −0.044 (4) | 0.042 (8) | −0.042 (8) |
Si1 | 0.115 (3) | 0.0649 (11) | 0.0414 (12) | −0.0008 (13) | 0.028 (2) | 0.0082 (11) |
F1 | 0.207 (11) | 0.115 (6) | 0.116 (6) | −0.060 (7) | 0.097 (8) | −0.005 (5) |
F2 | 0.167 (10) | 0.170 (10) | 0.047 (4) | 0.078 (8) | 0.031 (5) | −0.001 (5) |
F3 | 0.178 (10) | 0.093 (5) | 0.175 (12) | −0.025 (6) | 0.051 (8) | 0.005 (7) |
F4 | 0.146 (7) | 0.088 (4) | 0.053 (4) | 0.004 (5) | 0.043 (4) | −0.001 (3) |
F5 | 0.158 (8) | 0.171 (8) | 0.064 (4) | 0.007 (6) | 0.019 (4) | 0.034 (5) |
F6 | 0.158 (9) | 0.103 (5) | 0.079 (5) | 0.051 (6) | 0.021 (5) | −0.008 (4) |
O1 | 0.0447 (16) | 0.0604 (18) | 0.0574 (18) | 0.000 | 0.000 | −0.0204 (14) |
O2 | 0.0829 (16) | 0.0829 (16) | 0.0561 (19) | −0.0102 (19) | 0.0072 (16) | −0.0072 (16) |
O4 | 0.28 (2) | 0.39 (3) | 0.144 (14) | 0.09 (2) | −0.007 (15) | −0.026 (18) |
O3 | 0.173 (13) | 0.39 (3) | 0.158 (13) | 0.105 (17) | 0.023 (10) | −0.118 (15) |
Geometric parameters (Å, º) top
Rh1—N1i | 2.0502 (19) | C5—C6 | 1.342 (5) |
Rh1—N1 | 2.0502 (18) | C5—H5 | 0.9300 |
Rh1—N3i | 2.057 (2) | C6—H6 | 0.9300 |
Rh1—N3 | 2.057 (2) | N5—C7i | 1.283 (4) |
Rh1—N5 | 2.275 (3) | N5—C7 | 1.283 (4) |
Rh1—Rh1ii | 2.7052 (5) | C7—C8 | 1.367 (7) |
N1—C1 | 1.334 (3) | C7—H7 | 0.9300 |
N1—C3 | 1.373 (3) | C8—C9 | 1.337 (6) |
C1—N2 | 1.344 (3) | C8—H8 | 0.9300 |
C1—C4 | 1.434 (4) | C9—C8i | 1.337 (6) |
N2—C2 | 1.365 (4) | C9—C10 | 1.514 (8) |
N2—H2N | 0.8600 | C10—H10A | 0.9600 |
C2—C3 | 1.362 (4) | C10—H10B | 0.9600 |
C2—H2 | 0.9300 | C10—H10C | 0.9600 |
C3—H3 | 0.9300 | Si1—F5 | 1.607 (8) |
N3—C4 | 1.339 (3) | Si1—F3 | 1.658 (10) |
N3—C6 | 1.376 (3) | Si1—F1 | 1.659 (8) |
C4—N4 | 1.333 (3) | Si1—F2 | 1.662 (8) |
N4—C5 | 1.363 (5) | Si1—F6 | 1.664 (7) |
N4—H4N | 0.8600 | Si1—F4 | 1.687 (7) |
| | | |
N1i—Rh1—N1 | 175.55 (12) | C6—C5—N4 | 107.6 (3) |
N1i—Rh1—N3i | 79.59 (8) | C6—C5—H5 | 126.2 |
N1—Rh1—N3i | 100.24 (8) | N4—C5—H5 | 126.2 |
N1i—Rh1—N3 | 100.24 (8) | C5—C6—N3 | 108.9 (3) |
N1—Rh1—N3 | 79.59 (8) | C5—C6—H6 | 125.5 |
N3i—Rh1—N3 | 175.62 (13) | N3—C6—H6 | 125.5 |
N1i—Rh1—N5 | 87.78 (6) | C7i—N5—C7 | 114.6 (5) |
N1—Rh1—N5 | 87.78 (6) | C7i—N5—Rh1 | 122.7 (2) |
N3i—Rh1—N5 | 87.81 (7) | C7—N5—Rh1 | 122.7 (2) |
N3—Rh1—N5 | 87.81 (7) | N5—C7—C8 | 124.2 (4) |
N1i—Rh1—Rh1ii | 92.22 (6) | N5—C7—H7 | 117.9 |
N1—Rh1—Rh1ii | 92.23 (6) | C8—C7—H7 | 117.9 |
N3i—Rh1—Rh1ii | 92.19 (7) | C9—C8—C7 | 121.8 (4) |
N3—Rh1—Rh1ii | 92.19 (7) | C9—C8—H8 | 119.1 |
N5—Rh1—Rh1ii | 180.0 | C7—C8—H8 | 119.1 |
C1—N1—C3 | 106.4 (2) | C8—C9—C8i | 113.3 (5) |
C1—N1—Rh1 | 113.22 (16) | C8—C9—C10 | 123.3 (3) |
C3—N1—Rh1 | 139.08 (18) | C8i—C9—C10 | 123.3 (3) |
N1—C1—N2 | 110.6 (3) | C9—C10—H10A | 109.5 |
N1—C1—C4 | 116.8 (2) | C9—C10—H10B | 109.5 |
N2—C1—C4 | 132.6 (3) | H10A—C10—H10B | 109.5 |
C1—N2—C2 | 107.3 (2) | C9—C10—H10C | 109.5 |
C1—N2—H2N | 126.3 | H10A—C10—H10C | 109.5 |
C2—N2—H2N | 126.3 | H10B—C10—H10C | 109.5 |
C3—C2—N2 | 107.2 (2) | F5—Si1—F3 | 86.8 (6) |
C3—C2—H2 | 126.4 | F5—Si1—F1 | 93.3 (6) |
N2—C2—H2 | 126.4 | F3—Si1—F1 | 179.1 (6) |
C2—C3—N1 | 108.5 (2) | F5—Si1—F2 | 177.1 (5) |
C2—C3—H3 | 125.8 | F3—Si1—F2 | 91.3 (8) |
N1—C3—H3 | 125.8 | F1—Si1—F2 | 88.6 (7) |
C4—N3—C6 | 105.4 (2) | F5—Si1—F6 | 93.8 (5) |
C4—N3—Rh1 | 113.30 (17) | F3—Si1—F6 | 89.5 (6) |
C6—N3—Rh1 | 141.2 (2) | F1—Si1—F6 | 89.6 (5) |
N4—C4—N3 | 111.0 (3) | F2—Si1—F6 | 88.4 (4) |
N4—C4—C1 | 132.7 (3) | F5—Si1—F4 | 89.0 (5) |
N3—C4—C1 | 116.3 (2) | F3—Si1—F4 | 89.5 (5) |
C4—N4—C5 | 107.0 (3) | F1—Si1—F4 | 91.4 (4) |
C4—N4—H4N | 126.5 | F2—Si1—F4 | 88.8 (4) |
C5—N4—H4N | 126.5 | F6—Si1—F4 | 177.0 (6) |
| | | |
N1—Rh1ii—Rh1ii—N3 | | Rh1ii—Rh1—N3—C6 | −86.0 (3) |
N1i—Rh1—N1—C1 | 79.98 (19) | C6—N3—C4—N4 | 1.6 (3) |
N3i—Rh1—N1—C1 | 167.35 (19) | Rh1—N3—C4—N4 | 179.0 (2) |
N3—Rh1—N1—C1 | −8.20 (19) | C6—N3—C4—C1 | 179.3 (3) |
N5—Rh1—N1—C1 | 79.98 (19) | Rh1—N3—C4—C1 | −3.3 (3) |
Rh1ii—Rh1—N1—C1 | −100.02 (19) | N1—C1—C4—N4 | 173.2 (3) |
N1i—Rh1—N1—C3 | −84.6 (3) | N2—C1—C4—N4 | −8.7 (6) |
N3i—Rh1—N1—C3 | 2.7 (3) | N1—C1—C4—N3 | −3.9 (4) |
N3—Rh1—N1—C3 | −172.8 (3) | N2—C1—C4—N3 | 174.2 (3) |
N5—Rh1—N1—C3 | −84.6 (3) | N3—C4—N4—C5 | −1.2 (4) |
Rh1ii—Rh1—N1—C3 | 95.4 (3) | C1—C4—N4—C5 | −178.4 (3) |
C3—N1—C1—N2 | 0.1 (3) | C4—N4—C5—C6 | 0.3 (4) |
Rh1—N1—C1—N2 | −169.46 (19) | N4—C5—C6—N3 | 0.7 (4) |
C3—N1—C1—C4 | 178.6 (2) | C4—N3—C6—C5 | −1.4 (4) |
Rh1—N1—C1—C4 | 9.0 (3) | Rh1—N3—C6—C5 | −177.6 (3) |
N1—C1—N2—C2 | 0.1 (3) | N1i—Rh1—N5—C7i | −140.2 (5) |
C4—C1—N2—C2 | −178.0 (3) | N1—Rh1—N5—C7i | 39.8 (5) |
C1—N2—C2—C3 | −0.3 (3) | N3i—Rh1—N5—C7i | −60.6 (5) |
N2—C2—C3—N1 | 0.4 (3) | N3—Rh1—N5—C7i | 119.4 (5) |
C1—N1—C3—C2 | −0.3 (3) | Rh1ii—Rh1—N5—C7i | −165.9 (5) |
Rh1—N1—C3—C2 | 165.0 (2) | N1i—Rh1—N5—C7 | 39.8 (5) |
N1i—Rh1—N3—C4 | −169.34 (19) | N1—Rh1—N5—C7 | −140.2 (5) |
N1—Rh1—N3—C4 | 6.14 (19) | N3i—Rh1—N5—C7 | 119.4 (5) |
N3i—Rh1—N3—C4 | −82.00 (19) | N3—Rh1—N5—C7 | −60.6 (5) |
N5—Rh1—N3—C4 | −82.00 (19) | Rh1ii—Rh1—N5—C7 | 14.1 (5) |
Rh1ii—Rh1—N3—C4 | 98.00 (19) | C7i—N5—C7—C8 | −0.9 (7) |
N1i—Rh1—N3—C6 | 6.6 (4) | Rh1—N5—C7—C8 | 179.1 (7) |
N1—Rh1—N3—C6 | −177.9 (4) | N5—C7—C8—C9 | 2.0 (14) |
N3i—Rh1—N3—C6 | 94.0 (3) | C7—C8—C9—C8i | −0.9 (6) |
N5—Rh1—N3—C6 | 94.0 (3) | C7—C8—C9—C10 | 179.1 (6) |
Symmetry codes: (i) y, x, −z; (ii) −x+1, −y+1, z. |
Hydrogen-bond geometry (Å, º) top
D—H···A | D—H | H···A | D···A | D—H···A |
N2—H2N···F2iii | 0.86 | 1.87 | 2.684 (7) | 158 |
N2—H2N···F4 | 0.86 | 2.06 | 2.819 (8) | 147 |
N2—H2N···F5 | 0.86 | 2.23 | 2.970 (10) | 144 |
N2—H2N···F6iii | 0.86 | 2.33 | 3.004 (9) | 136 |
N4—H4N···F1iii | 0.86 | 1.92 | 2.774 (7) | 171 |
N4—H4N···F4 | 0.86 | 2.30 | 2.999 (9) | 138 |
N4—H4N···O3 | 0.86 | 2.02 | 2.744 (14) | 141 |
Symmetry code: (iii) −x+1/2, y, −z+3/4. |
Crystal data top
C60H60N38Rh4·SiF6·6(ClO4)·12.7(H2O) | Dx = 1.777 Mg m−3 |
Mr = 2692.69 | Mo Kα radiation, λ = 0.71069 Å |
Orthorhombic, Pbca | Cell parameters from 25234 reflections |
a = 20.170 (2) Å | θ = 3.3–27.5° |
b = 21.875 (3) Å | µ = 0.94 mm−1 |
c = 22.541 (3) Å | T = 296 K |
V = 9946 (2) Å3 | Prismatic, red |
Z = 4 | 0.50 × 0.42 × 0.31 mm |
F(000) = 5420 | |
Data collection top
Rigaku/MSC Mercury CCD diffractometer | 11352 independent reflections |
Radiation source: rotating-anode X-ray tube | 10339 reflections with I > 2σ(I) |
Graphite monochromator | Rint = 0.035 |
Detector resolution: 14.62 pixels mm-1 | θmax = 27.5°, θmin = 3.3° |
ω scans | h = −26→24 |
Absorption correction: numerical NUMABS (Higashi, 1999) | k = −28→27 |
Tmin = 0.832, Tmax = 0.894 | l = −22→29 |
71587 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)] = 0.059 | Hydrogen site location: inferred from neighbouring sites |
wR(F2) = 0.180 | H atoms treated by a mixture of independent and constrained refinement |
S = 1.17 | w = 1/[σ2(Fo2) + (0.0782P)2 + 29.1806P] where P = (Fo2 + 2Fc2)/3 |
11379 reflections | (Δ/σ)max = 0.002 |
712 parameters | Δρmax = 1.65 e Å−3 |
12 restraints | Δρmin = −1.44 e Å−3 |
Crystal data top
C60H60N38Rh4·SiF6·6(ClO4)·12.7(H2O) | V = 9946 (2) Å3 |
Mr = 2692.69 | Z = 4 |
Orthorhombic, Pbca | Mo Kα radiation |
a = 20.170 (2) Å | µ = 0.94 mm−1 |
b = 21.875 (3) Å | T = 296 K |
c = 22.541 (3) Å | 0.50 × 0.42 × 0.31 mm |
Data collection top
Rigaku/MSC Mercury CCD diffractometer | 11352 independent reflections |
Absorption correction: numerical NUMABS (Higashi, 1999) | 10339 reflections with I > 2σ(I) |
Tmin = 0.832, Tmax = 0.894 | Rint = 0.035 |
71587 measured reflections | |
Refinement top
R[F2 > 2σ(F2)] = 0.059 | 12 restraints |
wR(F2) = 0.180 | H atoms treated by a mixture of independent and constrained refinement |
S = 1.17 | w = 1/[σ2(Fo2) + (0.0782P)2 + 29.1806P] where P = (Fo2 + 2Fc2)/3 |
11379 reflections | Δρmax = 1.65 e Å−3 |
712 parameters | Δρmin = −1.44 e Å−3 |
Special details top
Geometry. All e.s.d.'s (except the e.s.d. in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell e.s.d.'s are taken into account individually in the estimation of e.s.d.'s in distances, angles and torsion angles; correlations between e.s.d.'s in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell e.s.d.'s is used for estimating e.s.d.'s involving l.s. planes. |
Refinement. Refinement of F2 against ALL reflections. The weighted R-factor wR and goodness of fit S are based on F2, conventional R-factors R are based on F, with F set to zero for negative F2. The threshold expression of F2 > σ(F2) is used only for calculating R-factors(gt) etc. and is not relevant to the choice of reflections for refinement. R-factors based on F2 are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger. |
Fractional atomic coordinates and isotropic or equivalent isotropic displacement parameters (Å2) top | x | y | z | Uiso*/Ueq | Occ. (<1) |
Rh1 | 0.285008 (17) | 0.702100 (16) | 0.559554 (17) | 0.03460 (12) | |
Rh2 | 0.376560 (16) | 0.616341 (15) | 0.534188 (16) | 0.03148 (11) | |
N1 | 0.3360 (2) | 0.76822 (18) | 0.5135 (2) | 0.0413 (9) | |
C1 | 0.3731 (3) | 0.8043 (2) | 0.5486 (3) | 0.0506 (14) | |
N2 | 0.3990 (3) | 0.8501 (2) | 0.5177 (3) | 0.0626 (14) | |
H2N | 0.4239 | 0.8787 | 0.5315 | 0.075* | |
C2 | 0.3789 (3) | 0.8436 (3) | 0.4604 (4) | 0.0656 (18) | |
H2 | 0.3902 | 0.8688 | 0.4287 | 0.079* | |
C3 | 0.3394 (3) | 0.7937 (3) | 0.4580 (3) | 0.0545 (14) | |
H3 | 0.3180 | 0.7790 | 0.4243 | 0.065* | |
N3 | 0.3427 (2) | 0.7378 (2) | 0.6263 (2) | 0.0458 (10) | |
C4 | 0.3773 (3) | 0.7869 (3) | 0.6097 (3) | 0.0501 (13) | |
N4 | 0.4128 (3) | 0.8083 (3) | 0.6558 (3) | 0.0730 (17) | |
H4N | 0.4392 | 0.8392 | 0.6555 | 0.088* | |
C5 | 0.3990 (4) | 0.7722 (4) | 0.7025 (4) | 0.079 (2) | |
H5 | 0.4164 | 0.7765 | 0.7405 | 0.095* | |
C6 | 0.3562 (4) | 0.7291 (3) | 0.6854 (3) | 0.0631 (17) | |
H6 | 0.3387 | 0.6985 | 0.7093 | 0.076* | |
N5 | 0.2228 (2) | 0.66996 (19) | 0.4944 (2) | 0.0429 (9) | |
C7 | 0.1756 (3) | 0.6327 (2) | 0.5148 (3) | 0.0510 (14) | |
N6 | 0.1355 (3) | 0.6166 (2) | 0.4703 (3) | 0.0705 (18) | |
H6N | 0.1017 | 0.5927 | 0.4729 | 0.085* | |
C8 | 0.1569 (4) | 0.6441 (3) | 0.4209 (4) | 0.0706 (19) | |
H8 | 0.1377 | 0.6409 | 0.3835 | 0.085* | |
C9 | 0.2110 (3) | 0.6775 (3) | 0.4346 (3) | 0.0528 (14) | |
H9 | 0.2358 | 0.7012 | 0.4086 | 0.063* | |
N7 | 0.2288 (2) | 0.6413 (2) | 0.6074 (2) | 0.0501 (11) | |
C10 | 0.1784 (3) | 0.6188 (3) | 0.5767 (4) | 0.0589 (16) | |
N8 | 0.1395 (3) | 0.5844 (3) | 0.6119 (4) | 0.080 (2) | |
H8N | 0.1047 | 0.5645 | 0.6013 | 0.095* | |
C11 | 0.1657 (4) | 0.5870 (4) | 0.6673 (4) | 0.085 (3) | |
H11 | 0.1486 | 0.5681 | 0.7009 | 0.102* | |
C12 | 0.2208 (4) | 0.6218 (3) | 0.6650 (3) | 0.0684 (19) | |
H12 | 0.2485 | 0.6310 | 0.6967 | 0.082* | |
N9 | 0.4529 (2) | 0.67712 (17) | 0.5442 (2) | 0.0386 (9) | |
C13 | 0.4819 (3) | 0.6748 (2) | 0.5972 (3) | 0.0441 (11) | |
N10 | 0.5328 (2) | 0.7140 (2) | 0.5997 (3) | 0.0558 (12) | |
H10N | 0.5582 | 0.7205 | 0.6297 | 0.067* | |
C14 | 0.5368 (3) | 0.7418 (3) | 0.5457 (3) | 0.0593 (15) | |
H14 | 0.5677 | 0.7712 | 0.5346 | 0.071* | |
C15 | 0.4883 (3) | 0.7190 (2) | 0.5112 (3) | 0.0483 (12) | |
H15 | 0.4800 | 0.7296 | 0.4720 | 0.058* | |
N11 | 0.3992 (2) | 0.60354 (19) | 0.6218 (2) | 0.0406 (9) | |
C16 | 0.4538 (3) | 0.6336 (2) | 0.6395 (2) | 0.0442 (11) | |
N12 | 0.4687 (3) | 0.6182 (2) | 0.6952 (2) | 0.0594 (13) | |
H12N | 0.5012 | 0.6325 | 0.7156 | 0.071* | |
C17 | 0.4242 (4) | 0.5764 (3) | 0.7142 (3) | 0.0635 (16) | |
H17 | 0.4233 | 0.5576 | 0.7512 | 0.076* | |
C18 | 0.3805 (3) | 0.5670 (3) | 0.6687 (3) | 0.0530 (13) | |
H18 | 0.3445 | 0.5405 | 0.6693 | 0.064* | |
N13 | 0.3605 (2) | 0.62420 (18) | 0.44503 (19) | 0.0384 (9) | |
C19 | 0.3217 (3) | 0.5808 (2) | 0.4229 (2) | 0.0438 (11) | |
N14 | 0.3198 (3) | 0.5833 (3) | 0.3638 (2) | 0.0680 (15) | |
H14N | 0.2975 | 0.5598 | 0.3406 | 0.082* | |
C20 | 0.3604 (4) | 0.6306 (3) | 0.3470 (3) | 0.0718 (19) | |
H20 | 0.3694 | 0.6429 | 0.3083 | 0.086* | |
C21 | 0.3847 (3) | 0.6560 (3) | 0.3971 (3) | 0.0540 (13) | |
H21 | 0.4131 | 0.6894 | 0.3989 | 0.065* | |
N15 | 0.30583 (19) | 0.54976 (18) | 0.52193 (19) | 0.0380 (8) | |
C22 | 0.2900 (3) | 0.5411 (2) | 0.4654 (2) | 0.0432 (11) | |
N16 | 0.2459 (3) | 0.4958 (2) | 0.4603 (3) | 0.0556 (12) | |
H16N | 0.2284 | 0.4827 | 0.4280 | 0.067* | |
C23 | 0.2340 (3) | 0.4744 (3) | 0.5157 (3) | 0.0571 (15) | |
H23 | 0.2058 | 0.4423 | 0.5255 | 0.069* | |
C24 | 0.2701 (3) | 0.5075 (2) | 0.5537 (3) | 0.0481 (12) | |
H24 | 0.2709 | 0.5027 | 0.5947 | 0.058* | |
N17 | 0.2080 (2) | 0.77348 (19) | 0.5770 (2) | 0.0437 (10) | |
C25 | 0.1788 (4) | 0.7800 (3) | 0.6296 (3) | 0.0644 (17) | |
H25 | 0.1909 | 0.7545 | 0.6608 | 0.077* | |
C26 | 0.1309 (4) | 0.8240 (4) | 0.6385 (4) | 0.085 (3) | |
H26 | 0.1119 | 0.8275 | 0.6759 | 0.102* | |
N18 | 0.1107 (3) | 0.8616 (3) | 0.5956 (3) | 0.0786 (18) | |
C27 | 0.1400 (4) | 0.8545 (3) | 0.5440 (3) | 0.0680 (18) | |
H27 | 0.1277 | 0.8799 | 0.5129 | 0.082* | |
C28 | 0.1882 (3) | 0.8112 (3) | 0.5342 (3) | 0.0530 (13) | |
H28 | 0.2074 | 0.8082 | 0.4968 | 0.064* | |
N19 | 0.45273 (18) | 0.54441 (17) | 0.51296 (19) | 0.0361 (8) | |
C29 | 0.4560 (3) | 0.4916 (2) | 0.5429 (2) | 0.0421 (11) | |
H29 | 0.4258 | 0.4842 | 0.5732 | 0.051* | |
C30 | 0.4973 (2) | 0.5519 (2) | 0.4700 (2) | 0.0406 (11) | |
H30 | 0.4968 | 0.5879 | 0.4480 | 0.049* | |
Cl1 | 0.2778 (2) | 0.58238 (11) | 0.19874 (16) | 0.1522 (17) | |
O1 | 0.2233 (6) | 0.5459 (5) | 0.1986 (7) | 0.218 (6) | |
O2 | 0.3269 (9) | 0.5550 (5) | 0.2311 (6) | 0.286 (10) | |
O3 | 0.2965 (8) | 0.5927 (6) | 0.1370 (5) | 0.235 (7) | |
O4 | 0.2651 (5) | 0.6388 (4) | 0.2261 (5) | 0.164 (4) | |
Cl2 | 0.50273 (10) | 0.69105 (11) | 0.83968 (9) | 0.0785 (5) | |
O5 | 0.4665 (8) | 0.6378 (7) | 0.8369 (5) | 0.256 (9) | |
O6 | 0.5326 (4) | 0.6946 (4) | 0.8946 (3) | 0.122 (3) | |
O7 | 0.4637 (8) | 0.7368 (7) | 0.8328 (5) | 0.267 (9) | |
O8 | 0.5462 (3) | 0.6853 (4) | 0.7924 (3) | 0.113 (2) | |
Cl3 | 0.64557 (13) | 0.59097 (13) | 0.63762 (11) | 0.0989 (8) | |
O9 | 0.6837 (6) | 0.6371 (5) | 0.6036 (5) | 0.188 (5) | |
O10 | 0.6148 (3) | 0.6242 (4) | 0.6822 (3) | 0.117 (3) | |
O11 | 0.6952 (4) | 0.5514 (3) | 0.6597 (4) | 0.124 (3) | |
O12 | 0.6029 (4) | 0.5617 (5) | 0.6002 (5) | 0.161 (4) | |
Si1 | 0.0000 | 0.5000 | 0.5000 | 0.0809 (10) | |
F1 | 0.0061 (3) | 0.5712 (3) | 0.4753 (6) | 0.196 (5) | |
F2 | 0.0731 (3) | 0.4893 (3) | 0.4715 (5) | 0.172 (4) | |
F3 | 0.0333 (6) | 0.5196 (6) | 0.5631 (5) | 0.243 (6) | |
O1W | 0.3069 (5) | 0.8489 (5) | 0.3071 (4) | 0.149 (3) | |
O2W | 0.2339 (5) | 0.7416 (4) | 0.3008 (4) | 0.145 (3) | |
O3W | 0.5974 (4) | 0.7635 (3) | 0.7008 (3) | 0.103 (2) | |
O4W | 0.1611 (6) | 0.4761 (5) | 0.3607 (5) | 0.191 (5) | |
O5W | 0.5199 (19) | 0.8690 (15) | 0.701 (2) | 0.15 (2) | 0.26 (3) |
O6W | 0.6244 (17) | 0.9272 (13) | 0.7204 (11) | 0.233 (12) | 0.50 |
O7W | 0.4936 (11) | 0.9107 (10) | 0.6510 (13) | 0.303 (17) | 0.74 (3) |
O8W | 0.4435 (18) | 0.5109 (17) | 0.2650 (18) | 0.29 (3) | 0.50 (4) |
O9W | 0.5150 (19) | 0.5739 (16) | 0.2977 (16) | 0.20 (2) | 0.35 (3) |
Atomic displacement parameters (Å2) top | U11 | U22 | U33 | U12 | U13 | U23 |
Rh1 | 0.0332 (2) | 0.03079 (19) | 0.0399 (2) | 0.00056 (13) | 0.00202 (14) | −0.00012 (13) |
Rh2 | 0.03014 (19) | 0.02803 (18) | 0.0363 (2) | −0.00111 (12) | 0.00235 (13) | −0.00109 (13) |
N1 | 0.038 (2) | 0.034 (2) | 0.052 (3) | −0.0003 (16) | 0.0027 (18) | 0.0032 (17) |
C1 | 0.038 (3) | 0.036 (3) | 0.078 (4) | 0.001 (2) | 0.001 (3) | −0.007 (3) |
N2 | 0.050 (3) | 0.039 (2) | 0.099 (5) | −0.008 (2) | 0.010 (3) | −0.004 (3) |
C2 | 0.069 (4) | 0.045 (3) | 0.083 (5) | 0.002 (3) | 0.018 (4) | 0.015 (3) |
C3 | 0.062 (4) | 0.045 (3) | 0.056 (3) | 0.003 (3) | 0.012 (3) | 0.005 (2) |
N3 | 0.047 (2) | 0.042 (2) | 0.049 (3) | 0.0094 (18) | −0.0012 (19) | −0.0065 (19) |
C4 | 0.045 (3) | 0.042 (3) | 0.063 (4) | 0.003 (2) | −0.010 (2) | −0.013 (2) |
N4 | 0.067 (4) | 0.060 (3) | 0.092 (5) | 0.004 (3) | −0.023 (3) | −0.030 (3) |
C5 | 0.092 (5) | 0.084 (5) | 0.061 (4) | 0.023 (4) | −0.024 (4) | −0.024 (4) |
C6 | 0.081 (4) | 0.065 (4) | 0.043 (3) | 0.026 (3) | −0.004 (3) | −0.011 (3) |
N5 | 0.036 (2) | 0.038 (2) | 0.055 (3) | 0.0017 (16) | −0.0005 (18) | −0.0040 (18) |
C7 | 0.032 (2) | 0.040 (3) | 0.081 (4) | −0.006 (2) | 0.004 (3) | −0.009 (3) |
N6 | 0.041 (3) | 0.054 (3) | 0.116 (6) | −0.010 (2) | −0.019 (3) | −0.010 (3) |
C8 | 0.063 (4) | 0.071 (4) | 0.078 (5) | 0.006 (3) | −0.025 (4) | −0.020 (4) |
C9 | 0.050 (3) | 0.054 (3) | 0.054 (3) | 0.004 (2) | −0.011 (2) | −0.007 (3) |
N7 | 0.048 (2) | 0.039 (2) | 0.063 (3) | 0.0046 (19) | 0.019 (2) | 0.007 (2) |
C10 | 0.040 (3) | 0.042 (3) | 0.094 (5) | 0.003 (2) | 0.021 (3) | 0.006 (3) |
N8 | 0.061 (3) | 0.056 (3) | 0.122 (6) | −0.010 (3) | 0.038 (4) | 0.015 (4) |
C11 | 0.086 (5) | 0.067 (4) | 0.104 (7) | 0.008 (4) | 0.049 (5) | 0.031 (4) |
C12 | 0.079 (5) | 0.057 (4) | 0.069 (4) | 0.015 (3) | 0.030 (4) | 0.017 (3) |
N9 | 0.037 (2) | 0.0292 (18) | 0.050 (2) | −0.0010 (15) | 0.0033 (17) | −0.0020 (16) |
C13 | 0.039 (2) | 0.041 (3) | 0.052 (3) | −0.001 (2) | −0.003 (2) | −0.005 (2) |
N10 | 0.039 (2) | 0.060 (3) | 0.069 (3) | −0.012 (2) | −0.005 (2) | −0.013 (2) |
C14 | 0.048 (3) | 0.049 (3) | 0.082 (4) | −0.013 (3) | 0.007 (3) | −0.003 (3) |
C15 | 0.039 (3) | 0.042 (3) | 0.063 (4) | −0.006 (2) | 0.008 (2) | 0.001 (2) |
N11 | 0.040 (2) | 0.037 (2) | 0.045 (2) | 0.0022 (16) | 0.0006 (18) | −0.0015 (17) |
C16 | 0.047 (3) | 0.043 (3) | 0.043 (3) | 0.004 (2) | −0.004 (2) | −0.003 (2) |
N12 | 0.063 (3) | 0.066 (3) | 0.049 (3) | 0.002 (2) | −0.015 (2) | −0.002 (2) |
C17 | 0.075 (4) | 0.067 (4) | 0.048 (3) | 0.003 (3) | 0.003 (3) | 0.009 (3) |
C18 | 0.063 (4) | 0.053 (3) | 0.044 (3) | 0.004 (3) | 0.002 (2) | 0.003 (2) |
N13 | 0.040 (2) | 0.036 (2) | 0.039 (2) | 0.0014 (16) | 0.0022 (17) | −0.0014 (16) |
C19 | 0.049 (3) | 0.041 (3) | 0.042 (3) | 0.002 (2) | 0.000 (2) | −0.004 (2) |
N14 | 0.090 (4) | 0.069 (3) | 0.044 (3) | −0.016 (3) | −0.004 (3) | −0.005 (2) |
C20 | 0.101 (6) | 0.073 (4) | 0.042 (3) | −0.016 (4) | 0.003 (3) | 0.008 (3) |
C21 | 0.060 (3) | 0.053 (3) | 0.049 (3) | −0.005 (3) | 0.003 (3) | 0.008 (3) |
N15 | 0.0339 (19) | 0.0321 (19) | 0.048 (2) | −0.0005 (15) | 0.0031 (17) | −0.0007 (16) |
C22 | 0.042 (3) | 0.039 (3) | 0.049 (3) | −0.001 (2) | 0.000 (2) | −0.009 (2) |
N16 | 0.051 (3) | 0.047 (3) | 0.069 (3) | −0.014 (2) | −0.006 (2) | −0.011 (2) |
C23 | 0.045 (3) | 0.048 (3) | 0.078 (4) | −0.012 (2) | 0.006 (3) | −0.005 (3) |
C24 | 0.046 (3) | 0.038 (3) | 0.060 (3) | −0.008 (2) | 0.008 (2) | 0.001 (2) |
N17 | 0.042 (2) | 0.037 (2) | 0.052 (3) | 0.0079 (17) | −0.0004 (19) | −0.0009 (19) |
C25 | 0.075 (4) | 0.058 (3) | 0.060 (4) | 0.026 (3) | 0.009 (3) | 0.005 (3) |
C26 | 0.094 (6) | 0.078 (5) | 0.083 (6) | 0.035 (4) | 0.032 (4) | 0.001 (4) |
N18 | 0.080 (4) | 0.069 (4) | 0.087 (5) | 0.032 (3) | 0.010 (4) | 0.001 (3) |
C27 | 0.072 (4) | 0.060 (4) | 0.072 (5) | 0.031 (3) | −0.007 (3) | 0.007 (3) |
C28 | 0.052 (3) | 0.051 (3) | 0.056 (3) | 0.010 (3) | 0.003 (3) | 0.004 (3) |
N19 | 0.0327 (19) | 0.0295 (18) | 0.046 (2) | 0.0030 (14) | 0.0027 (16) | −0.0020 (16) |
C29 | 0.040 (2) | 0.035 (2) | 0.051 (3) | 0.0040 (19) | 0.013 (2) | 0.006 (2) |
C30 | 0.039 (2) | 0.034 (2) | 0.048 (3) | 0.0020 (19) | 0.011 (2) | 0.005 (2) |
Cl1 | 0.255 (4) | 0.0656 (13) | 0.136 (3) | −0.0206 (19) | −0.112 (3) | −0.0087 (14) |
O1 | 0.217 (11) | 0.174 (10) | 0.265 (15) | −0.123 (9) | 0.011 (10) | −0.057 (10) |
O2 | 0.51 (3) | 0.163 (10) | 0.187 (12) | 0.131 (13) | −0.222 (15) | −0.074 (8) |
O3 | 0.354 (19) | 0.247 (14) | 0.103 (7) | −0.143 (14) | −0.059 (9) | −0.002 (8) |
O4 | 0.209 (10) | 0.094 (5) | 0.189 (10) | 0.003 (6) | −0.085 (8) | −0.050 (6) |
Cl2 | 0.0714 (11) | 0.1059 (15) | 0.0583 (10) | 0.0127 (10) | 0.0067 (8) | −0.0187 (10) |
O5 | 0.318 (16) | 0.307 (16) | 0.142 (9) | −0.220 (15) | 0.070 (10) | −0.096 (10) |
O6 | 0.122 (6) | 0.182 (8) | 0.063 (4) | 0.004 (5) | −0.009 (4) | −0.032 (4) |
O7 | 0.333 (17) | 0.351 (18) | 0.116 (8) | 0.277 (16) | −0.003 (9) | −0.013 (9) |
O8 | 0.102 (5) | 0.170 (7) | 0.066 (4) | 0.001 (5) | 0.024 (3) | −0.022 (4) |
Cl3 | 0.0959 (15) | 0.1162 (18) | 0.0847 (15) | 0.0401 (14) | −0.0151 (12) | −0.0281 (13) |
O9 | 0.217 (11) | 0.194 (10) | 0.153 (9) | −0.046 (9) | 0.044 (8) | 0.065 (8) |
O10 | 0.094 (5) | 0.153 (7) | 0.102 (5) | 0.034 (4) | 0.004 (4) | −0.049 (5) |
O11 | 0.127 (6) | 0.112 (5) | 0.133 (6) | 0.050 (5) | −0.030 (5) | −0.015 (5) |
O12 | 0.122 (6) | 0.186 (9) | 0.175 (9) | 0.015 (6) | −0.052 (6) | −0.092 (7) |
Si1 | 0.0410 (12) | 0.0498 (14) | 0.152 (3) | −0.0023 (10) | 0.0031 (16) | −0.0129 (17) |
F1 | 0.077 (4) | 0.065 (3) | 0.447 (16) | 0.011 (3) | 0.063 (6) | 0.026 (6) |
F2 | 0.076 (4) | 0.098 (4) | 0.340 (12) | 0.009 (3) | 0.064 (5) | −0.018 (6) |
F3 | 0.224 (11) | 0.302 (15) | 0.203 (10) | −0.066 (10) | −0.083 (9) | −0.075 (10) |
O1W | 0.178 (8) | 0.165 (8) | 0.104 (6) | −0.023 (7) | 0.020 (6) | −0.039 (6) |
O2W | 0.134 (7) | 0.139 (7) | 0.163 (8) | 0.026 (5) | 0.050 (6) | 0.014 (6) |
O3W | 0.120 (5) | 0.104 (5) | 0.086 (4) | −0.020 (4) | −0.016 (4) | −0.010 (4) |
O4W | 0.243 (12) | 0.155 (8) | 0.174 (9) | 0.030 (8) | −0.116 (9) | −0.062 (7) |
O5W | 0.16 (3) | 0.09 (2) | 0.20 (4) | −0.02 (2) | −0.06 (3) | 0.02 (2) |
O6W | 0.35 (3) | 0.23 (2) | 0.125 (15) | 0.082 (19) | −0.004 (16) | −0.036 (15) |
O7W | 0.27 (2) | 0.22 (2) | 0.42 (4) | −0.156 (19) | −0.13 (2) | 0.08 (2) |
O8W | 0.27 (3) | 0.28 (3) | 0.33 (4) | 0.08 (2) | 0.01 (2) | −0.01 (2) |
O9W | 0.22 (4) | 0.18 (3) | 0.19 (4) | −0.01 (3) | 0.05 (3) | −0.03 (2) |
Geometric parameters (Å, º) top
Rh1—N7 | 2.053 (4) | N12—C17 | 1.354 (9) |
Rh1—N1 | 2.056 (4) | N12—H12N | 0.8600 |
Rh1—N3 | 2.056 (5) | C17—C18 | 1.367 (9) |
Rh1—N5 | 2.056 (4) | C17—H17 | 0.9300 |
Rh1—N17 | 2.238 (4) | C18—H18 | 0.9300 |
Rh1—Rh2 | 2.6943 (5) | N13—C19 | 1.327 (7) |
Rh2—N13 | 2.044 (4) | N13—C21 | 1.375 (7) |
Rh2—N11 | 2.047 (4) | C19—N14 | 1.335 (7) |
Rh2—N9 | 2.048 (4) | C19—C22 | 1.442 (8) |
Rh2—N15 | 2.058 (4) | N14—C20 | 1.373 (9) |
Rh2—N19 | 2.251 (4) | N14—H14N | 0.8600 |
N1—C1 | 1.345 (7) | C20—C21 | 1.352 (9) |
N1—C3 | 1.372 (7) | C20—H20 | 0.9300 |
C1—N2 | 1.327 (8) | C21—H21 | 0.9300 |
C1—C4 | 1.433 (9) | N15—C22 | 1.329 (7) |
N2—C2 | 1.363 (10) | N15—C24 | 1.375 (7) |
N2—H2N | 0.8600 | C22—N16 | 1.336 (7) |
C2—C3 | 1.354 (9) | N16—C23 | 1.356 (9) |
C2—H2 | 0.9300 | N16—H16N | 0.8600 |
C3—H3 | 0.9300 | C23—C24 | 1.338 (8) |
N3—C4 | 1.334 (7) | C23—H23 | 0.9300 |
N3—C6 | 1.375 (8) | C24—H24 | 0.9300 |
C4—N4 | 1.347 (8) | N17—C25 | 1.331 (8) |
N4—C5 | 1.346 (11) | N17—C28 | 1.332 (7) |
N4—H4N | 0.8600 | C25—C26 | 1.379 (9) |
C5—C6 | 1.336 (11) | C25—H25 | 0.9300 |
C5—H5 | 0.9300 | C26—N18 | 1.334 (10) |
C6—H6 | 0.9300 | C26—H26 | 0.9300 |
N5—C7 | 1.335 (7) | N18—C27 | 1.314 (10) |
N5—C9 | 1.378 (8) | C27—C28 | 1.376 (8) |
C7—N6 | 1.338 (8) | C27—H27 | 0.9300 |
C7—C10 | 1.429 (10) | C28—H28 | 0.9300 |
N6—C8 | 1.337 (10) | N19—C30 | 1.332 (6) |
N6—H6N | 0.8600 | N19—C29 | 1.340 (6) |
C8—C9 | 1.349 (9) | C29—C30i | 1.370 (7) |
C8—H8 | 0.9300 | C29—H29 | 0.9300 |
C9—H9 | 0.9300 | C30—C29i | 1.370 (7) |
N7—C10 | 1.325 (9) | C30—H30 | 0.9300 |
N7—C12 | 1.376 (8) | Cl1—O1 | 1.358 (9) |
C10—N8 | 1.347 (8) | Cl1—O2 | 1.369 (11) |
N8—C11 | 1.356 (12) | Cl1—O4 | 1.403 (8) |
N8—H8N | 0.8600 | Cl1—O3 | 1.460 (12) |
C11—C12 | 1.350 (11) | Cl2—O7 | 1.284 (9) |
C11—H11 | 0.9300 | Cl2—O5 | 1.376 (11) |
C12—H12 | 0.9300 | Cl2—O6 | 1.379 (7) |
N9—C13 | 1.330 (7) | Cl2—O8 | 1.386 (6) |
N9—C15 | 1.379 (7) | Cl3—O12 | 1.365 (8) |
C13—N10 | 1.340 (7) | Cl3—O10 | 1.388 (6) |
C13—C16 | 1.430 (8) | Cl3—O11 | 1.413 (7) |
N10—C14 | 1.362 (9) | Cl3—O9 | 1.483 (9) |
N10—H10N | 0.8600 | Si1—F2ii | 1.625 (6) |
C14—C15 | 1.346 (9) | Si1—F2 | 1.625 (6) |
C14—H14 | 0.9300 | Si1—F3 | 1.631 (9) |
C15—H15 | 0.9300 | Si1—F3ii | 1.631 (9) |
N11—C16 | 1.344 (7) | Si1—F1 | 1.660 (6) |
N11—C18 | 1.379 (7) | Si1—F1ii | 1.660 (6) |
C16—N12 | 1.334 (7) | | |
| | | |
N7—Rh1—N1 | 175.44 (17) | N9—C15—H15 | 125.9 |
N7—Rh1—N3 | 100.0 (2) | C16—N11—C18 | 106.2 (5) |
N1—Rh1—N3 | 79.56 (18) | C16—N11—Rh2 | 113.8 (4) |
N7—Rh1—N5 | 79.5 (2) | C18—N11—Rh2 | 139.4 (4) |
N1—Rh1—N5 | 100.68 (18) | N12—C16—N11 | 110.0 (5) |
N3—Rh1—N5 | 176.52 (16) | N12—C16—C13 | 134.3 (5) |
N7—Rh1—N17 | 88.62 (17) | N11—C16—C13 | 115.7 (5) |
N1—Rh1—N17 | 86.84 (16) | C16—N12—C17 | 108.6 (5) |
N3—Rh1—N17 | 89.94 (17) | C16—N12—H12N | 125.7 |
N5—Rh1—N17 | 86.61 (17) | C17—N12—H12N | 125.7 |
N7—Rh1—Rh2 | 92.24 (12) | N12—C17—C18 | 106.9 (6) |
N1—Rh1—Rh2 | 92.31 (11) | N12—C17—H17 | 126.5 |
N3—Rh1—Rh2 | 91.83 (12) | C18—C17—H17 | 126.5 |
N5—Rh1—Rh2 | 91.63 (12) | C17—C18—N11 | 108.2 (6) |
N17—Rh1—Rh2 | 177.87 (13) | C17—C18—H18 | 125.9 |
N13—Rh2—N11 | 175.11 (16) | N11—C18—H18 | 125.9 |
N13—Rh2—N9 | 99.99 (17) | C19—N13—C21 | 106.0 (5) |
N11—Rh2—N9 | 79.30 (17) | C19—N13—Rh2 | 113.8 (3) |
N13—Rh2—N15 | 79.47 (17) | C21—N13—Rh2 | 139.4 (4) |
N11—Rh2—N15 | 100.81 (17) | N13—C19—N14 | 111.3 (5) |
N9—Rh2—N15 | 175.04 (16) | N13—C19—C22 | 116.3 (5) |
N13—Rh2—N19 | 87.60 (16) | N14—C19—C22 | 132.4 (5) |
N11—Rh2—N19 | 87.54 (16) | C19—N14—C20 | 106.8 (5) |
N9—Rh2—N19 | 87.93 (15) | C19—N14—H14N | 126.6 |
N15—Rh2—N19 | 87.12 (15) | C20—N14—H14N | 126.6 |
N13—Rh2—Rh1 | 92.36 (11) | C21—C20—N14 | 107.2 (6) |
N11—Rh2—Rh1 | 92.50 (12) | C21—C20—H20 | 126.4 |
N9—Rh2—Rh1 | 92.30 (11) | N14—C20—H20 | 126.4 |
N15—Rh2—Rh1 | 92.65 (11) | C20—C21—N13 | 108.7 (5) |
N19—Rh2—Rh1 | 179.77 (10) | C20—C21—H21 | 125.7 |
C1—N1—C3 | 105.6 (5) | N13—C21—H21 | 125.7 |
C1—N1—Rh1 | 113.3 (4) | C22—N15—C24 | 106.2 (4) |
C3—N1—Rh1 | 140.5 (4) | C22—N15—Rh2 | 113.4 (3) |
N2—C1—N1 | 110.8 (6) | C24—N15—Rh2 | 140.4 (4) |
N2—C1—C4 | 133.0 (6) | N15—C22—N16 | 110.3 (5) |
N1—C1—C4 | 116.2 (5) | N15—C22—C19 | 116.4 (4) |
C1—N2—C2 | 107.5 (5) | N16—C22—C19 | 133.3 (5) |
C1—N2—H2N | 126.2 | C22—N16—C23 | 107.2 (5) |
C2—N2—H2N | 126.2 | C22—N16—H16N | 126.4 |
C3—C2—N2 | 107.2 (6) | C23—N16—H16N | 126.4 |
C3—C2—H2 | 126.4 | C24—C23—N16 | 107.9 (5) |
N2—C2—H2 | 126.4 | C24—C23—H23 | 126.1 |
C2—C3—N1 | 108.8 (6) | N16—C23—H23 | 126.1 |
C2—C3—H3 | 125.6 | C23—C24—N15 | 108.4 (6) |
N1—C3—H3 | 125.6 | C23—C24—H24 | 125.8 |
C4—N3—C6 | 106.2 (5) | N15—C24—H24 | 125.8 |
C4—N3—Rh1 | 113.4 (4) | C25—N17—C28 | 116.6 (5) |
C6—N3—Rh1 | 140.3 (5) | C25—N17—Rh1 | 122.6 (4) |
N3—C4—N4 | 110.1 (6) | C28—N17—Rh1 | 120.8 (4) |
N3—C4—C1 | 116.9 (5) | N17—C25—C26 | 120.9 (6) |
N4—C4—C1 | 132.9 (6) | N17—C25—H25 | 119.5 |
C5—N4—C4 | 106.8 (6) | C26—C25—H25 | 119.5 |
C5—N4—H4N | 126.6 | N18—C26—C25 | 122.7 (7) |
C4—N4—H4N | 126.6 | N18—C26—H26 | 118.7 |
C6—C5—N4 | 108.8 (6) | C25—C26—H26 | 118.7 |
C6—C5—H5 | 125.6 | C27—N18—C26 | 115.5 (6) |
N4—C5—H5 | 125.6 | N18—C27—C28 | 122.9 (6) |
C5—C6—N3 | 108.1 (7) | N18—C27—H27 | 118.6 |
C5—C6—H6 | 126.0 | C28—C27—H27 | 118.6 |
N3—C6—H6 | 126.0 | N17—C28—C27 | 121.4 (6) |
C7—N5—C9 | 106.7 (5) | N17—C28—H28 | 119.3 |
C7—N5—Rh1 | 113.4 (4) | C27—C28—H28 | 119.3 |
C9—N5—Rh1 | 139.8 (4) | C30—N19—C29 | 116.0 (4) |
N5—C7—N6 | 109.5 (6) | C30—N19—Rh2 | 122.0 (3) |
N5—C7—C10 | 116.0 (5) | C29—N19—Rh2 | 122.0 (3) |
N6—C7—C10 | 134.5 (6) | N19—C29—C30i | 121.8 (5) |
C8—N6—C7 | 108.1 (5) | N19—C29—H29 | 119.1 |
C8—N6—H6N | 126.0 | C30i—C29—H29 | 119.1 |
C7—N6—H6N | 126.0 | N19—C30—C29i | 122.2 (5) |
N6—C8—C9 | 108.3 (6) | N19—C30—H30 | 118.9 |
N6—C8—H8 | 125.9 | C29i—C30—H30 | 118.9 |
C9—C8—H8 | 125.9 | O1—Cl1—O2 | 109.3 (10) |
C8—C9—N5 | 107.5 (6) | O1—Cl1—O4 | 111.7 (8) |
C8—C9—H9 | 126.3 | O2—Cl1—O4 | 106.4 (6) |
N5—C9—H9 | 126.3 | O1—Cl1—O3 | 107.3 (8) |
C10—N7—C12 | 106.7 (6) | O2—Cl1—O3 | 112.9 (11) |
C10—N7—Rh1 | 113.0 (4) | O4—Cl1—O3 | 109.3 (8) |
C12—N7—Rh1 | 139.6 (5) | O7—Cl2—O5 | 109.2 (12) |
N7—C10—N8 | 110.4 (7) | O7—Cl2—O6 | 109.5 (7) |
N7—C10—C7 | 117.4 (5) | O5—Cl2—O6 | 108.6 (8) |
N8—C10—C7 | 132.2 (7) | O7—Cl2—O8 | 111.5 (7) |
C10—N8—C11 | 107.0 (7) | O5—Cl2—O8 | 103.0 (6) |
C10—N8—H8N | 126.5 | O6—Cl2—O8 | 114.7 (5) |
C11—N8—H8N | 126.5 | O12—Cl3—O10 | 114.3 (5) |
C12—C11—N8 | 108.0 (7) | O12—Cl3—O11 | 112.2 (6) |
C12—C11—H11 | 126.0 | O10—Cl3—O11 | 112.4 (5) |
N8—C11—H11 | 126.0 | O12—Cl3—O9 | 109.0 (8) |
C11—C12—N7 | 107.9 (8) | O10—Cl3—O9 | 104.5 (7) |
C11—C12—H12 | 126.0 | O11—Cl3—O9 | 103.4 (7) |
N7—C12—H12 | 126.0 | F2ii—Si1—F2 | 179.998 (2) |
C13—N9—C15 | 106.4 (4) | F2ii—Si1—F3 | 89.5 (6) |
C13—N9—Rh2 | 113.9 (3) | F2—Si1—F3 | 90.5 (6) |
C15—N9—Rh2 | 139.6 (4) | F2ii—Si1—F3ii | 90.5 (6) |
N9—C13—N10 | 110.5 (5) | F2—Si1—F3ii | 89.5 (6) |
N9—C13—C16 | 116.7 (5) | F3—Si1—F3ii | 180.0 (7) |
N10—C13—C16 | 132.8 (5) | F2ii—Si1—F1 | 93.7 (3) |
C13—N10—C14 | 107.1 (5) | F2—Si1—F1 | 86.3 (3) |
C13—N10—H10N | 126.5 | F3—Si1—F1 | 90.9 (6) |
C14—N10—H10N | 126.5 | F3ii—Si1—F1 | 89.1 (6) |
C15—C14—N10 | 107.9 (5) | F2ii—Si1—F1ii | 86.3 (3) |
C15—C14—H14 | 126.1 | F2—Si1—F1ii | 93.7 (3) |
N10—C14—H14 | 126.1 | F3—Si1—F1ii | 89.1 (6) |
C14—C15—N9 | 108.1 (6) | F3ii—Si1—F1ii | 90.9 (6) |
C14—C15—H15 | 125.9 | F1—Si1—F1ii | 179.998 (1) |
| | | |
N7—Rh1—Rh2—N13 | 118.86 (19) | Rh1—Rh2—N9—C13 | 97.6 (3) |
N1—Rh1—Rh2—N13 | −61.41 (17) | N13—Rh2—N9—C15 | 4.9 (5) |
N3—Rh1—Rh2—N13 | −141.03 (18) | N11—Rh2—N9—C15 | 180.0 (6) |
N5—Rh1—Rh2—N13 | 39.35 (17) | N15—Rh2—N9—C15 | 88 (2) |
N17—Rh1—Rh2—N13 | 5 (3) | N19—Rh2—N9—C15 | 92.1 (5) |
N7—Rh1—Rh2—N11 | −61.7 (2) | Rh1—Rh2—N9—C15 | −87.9 (5) |
N1—Rh1—Rh2—N11 | 118.08 (17) | C15—N9—C13—N10 | 1.3 (6) |
N3—Rh1—Rh2—N11 | 38.46 (18) | Rh2—N9—C13—N10 | 177.6 (3) |
N5—Rh1—Rh2—N11 | −141.16 (17) | C15—N9—C13—C16 | −179.5 (5) |
N17—Rh1—Rh2—N11 | −175 (23) | Rh2—N9—C13—C16 | −3.2 (6) |
N7—Rh1—Rh2—N9 | −141.0 (2) | N9—C13—N10—C14 | −0.8 (6) |
N1—Rh1—Rh2—N9 | 38.70 (18) | C16—C13—N10—C14 | −179.8 (6) |
N3—Rh1—Rh2—N9 | −40.92 (18) | C13—N10—C14—C15 | 0.0 (7) |
N5—Rh1—Rh2—N9 | 139.46 (18) | N10—C14—C15—N9 | 0.8 (7) |
N17—Rh1—Rh2—N9 | 105 (3) | C13—N9—C15—C14 | −1.3 (6) |
N7—Rh1—Rh2—N15 | 39.3 (2) | Rh2—N9—C15—C14 | −176.1 (4) |
N1—Rh1—Rh2—N15 | −140.97 (18) | N13—Rh2—N11—C16 | 75 (2) |
N3—Rh1—Rh2—N15 | 139.41 (18) | N9—Rh2—N11—C16 | −7.0 (3) |
N5—Rh1—Rh2—N15 | −40.21 (18) | N15—Rh2—N11—C16 | 168.0 (3) |
N17—Rh1—Rh2—N15 | −74 (3) | N19—Rh2—N11—C16 | 81.4 (4) |
N7—Rh1—Rh2—N19 | 37 (27) | Rh1—Rh2—N11—C16 | −98.9 (3) |
N1—Rh1—Rh2—N19 | −144 (34) | N13—Rh2—N11—C18 | −94 (2) |
N3—Rh1—Rh2—N19 | 137 (34) | N9—Rh2—N11—C18 | −176.3 (6) |
N5—Rh1—Rh2—N19 | −43 (27) | N15—Rh2—N11—C18 | −1.3 (6) |
N17—Rh1—Rh2—N19 | −77 (27) | N19—Rh2—N11—C18 | −87.9 (6) |
N7—Rh1—N1—C1 | 78 (3) | Rh1—Rh2—N11—C18 | 91.8 (5) |
N3—Rh1—N1—C1 | −7.0 (3) | C18—N11—C16—N12 | −1.2 (6) |
N5—Rh1—N1—C1 | 169.4 (3) | Rh2—N11—C16—N12 | −174.0 (4) |
N17—Rh1—N1—C1 | 83.5 (4) | C18—N11—C16—C13 | −179.8 (5) |
Rh2—Rh1—N1—C1 | −98.5 (3) | Rh2—N11—C16—C13 | 7.4 (6) |
N7—Rh1—N1—C3 | −91 (3) | N9—C13—C16—N12 | 179.1 (6) |
N3—Rh1—N1—C3 | −176.4 (6) | N10—C13—C16—N12 | −2.0 (11) |
N5—Rh1—N1—C3 | 0.0 (6) | N9—C13—C16—N11 | −2.8 (7) |
N17—Rh1—N1—C3 | −85.9 (6) | N10—C13—C16—N11 | 176.1 (5) |
Rh2—Rh1—N1—C3 | 92.1 (6) | N11—C16—N12—C17 | 1.3 (7) |
C3—N1—C1—N2 | −0.1 (6) | C13—C16—N12—C17 | 179.5 (6) |
Rh1—N1—C1—N2 | −173.1 (4) | C16—N12—C17—C18 | −0.9 (7) |
C3—N1—C1—C4 | 179.9 (5) | N12—C17—C18—N11 | 0.1 (7) |
Rh1—N1—C1—C4 | 6.9 (6) | C16—N11—C18—C17 | 0.7 (6) |
N1—C1—N2—C2 | −0.8 (7) | Rh2—N11—C18—C17 | 170.5 (5) |
C4—C1—N2—C2 | 179.2 (6) | N11—Rh2—N13—C19 | 86 (2) |
C1—N2—C2—C3 | 1.3 (7) | N9—Rh2—N13—C19 | 167.3 (4) |
N2—C2—C3—N1 | −1.3 (7) | N15—Rh2—N13—C19 | −7.7 (4) |
C1—N1—C3—C2 | 0.9 (6) | N19—Rh2—N13—C19 | 79.9 (4) |
Rh1—N1—C3—C2 | 170.7 (5) | Rh1—Rh2—N13—C19 | −99.9 (3) |
N7—Rh1—N3—C4 | −169.3 (4) | N11—Rh2—N13—C21 | −82 (2) |
N1—Rh1—N3—C4 | 6.1 (4) | N9—Rh2—N13—C21 | −0.4 (6) |
N5—Rh1—N3—C4 | −88 (3) | N15—Rh2—N13—C21 | −175.4 (6) |
N17—Rh1—N3—C4 | −80.7 (4) | N19—Rh2—N13—C21 | −87.8 (6) |
Rh2—Rh1—N3—C4 | 98.1 (4) | Rh1—Rh2—N13—C21 | 92.4 (6) |
N7—Rh1—N3—C6 | 7.3 (6) | C21—N13—C19—N14 | −0.2 (6) |
N1—Rh1—N3—C6 | −177.3 (6) | Rh2—N13—C19—N14 | −171.9 (4) |
N5—Rh1—N3—C6 | 88 (3) | C21—N13—C19—C22 | −179.8 (5) |
N17—Rh1—N3—C6 | 95.9 (6) | Rh2—N13—C19—C22 | 8.5 (6) |
Rh2—Rh1—N3—C6 | −85.3 (6) | N13—C19—N14—C20 | 0.8 (8) |
C6—N3—C4—N4 | 1.2 (6) | C22—C19—N14—C20 | −179.7 (6) |
Rh1—N3—C4—N4 | 178.9 (4) | C19—N14—C20—C21 | −1.1 (9) |
C6—N3—C4—C1 | 177.9 (5) | N14—C20—C21—N13 | 1.0 (9) |
Rh1—N3—C4—C1 | −4.4 (6) | C19—N13—C21—C20 | −0.5 (7) |
N2—C1—C4—N3 | 178.2 (6) | Rh2—N13—C21—C20 | 167.8 (5) |
N1—C1—C4—N3 | −1.8 (7) | N13—Rh2—N15—C22 | 5.6 (3) |
N2—C1—C4—N4 | −5.9 (11) | N11—Rh2—N15—C22 | −169.5 (3) |
N1—C1—C4—N4 | 174.1 (6) | N9—Rh2—N15—C22 | −79 (2) |
N3—C4—N4—C5 | −1.0 (7) | N19—Rh2—N15—C22 | −82.5 (4) |
C1—C4—N4—C5 | −177.1 (6) | Rh1—Rh2—N15—C22 | 97.5 (3) |
C4—N4—C5—C6 | 0.4 (8) | N13—Rh2—N15—C24 | −178.6 (6) |
N4—C5—C6—N3 | 0.3 (8) | N11—Rh2—N15—C24 | 6.4 (6) |
C4—N3—C6—C5 | −0.9 (7) | N9—Rh2—N15—C24 | 97 (2) |
Rh1—N3—C6—C5 | −177.6 (5) | N19—Rh2—N15—C24 | 93.3 (5) |
N7—Rh1—N5—C7 | 5.9 (4) | Rh1—Rh2—N15—C24 | −86.7 (5) |
N1—Rh1—N5—C7 | −169.5 (4) | C24—N15—C22—N16 | 0.4 (6) |
N3—Rh1—N5—C7 | −76 (3) | Rh2—N15—C22—N16 | 177.6 (4) |
N17—Rh1—N5—C7 | −83.3 (4) | C24—N15—C22—C19 | 179.9 (5) |
Rh2—Rh1—N5—C7 | 97.9 (4) | Rh2—N15—C22—C19 | −2.8 (6) |
N7—Rh1—N5—C9 | −179.5 (6) | N13—C19—C22—N15 | −3.8 (7) |
N1—Rh1—N5—C9 | 5.1 (6) | N14—C19—C22—N15 | 176.7 (6) |
N3—Rh1—N5—C9 | 99 (3) | N13—C19—C22—N16 | 175.6 (6) |
N17—Rh1—N5—C9 | 91.2 (6) | N14—C19—C22—N16 | −3.9 (11) |
Rh2—Rh1—N5—C9 | −87.6 (6) | N15—C22—N16—C23 | −0.9 (7) |
C9—N5—C7—N6 | 0.4 (6) | C19—C22—N16—C23 | 179.7 (6) |
Rh1—N5—C7—N6 | 176.7 (4) | C22—N16—C23—C24 | 1.0 (7) |
C9—N5—C7—C10 | −179.8 (5) | N16—C23—C24—N15 | −0.8 (7) |
Rh1—N5—C7—C10 | −3.4 (6) | C22—N15—C24—C23 | 0.3 (6) |
N5—C7—N6—C8 | −0.4 (7) | Rh2—N15—C24—C23 | −175.7 (4) |
C10—C7—N6—C8 | 179.7 (6) | N7—Rh1—N17—C25 | 41.6 (5) |
C7—N6—C8—C9 | 0.3 (8) | N1—Rh1—N17—C25 | −138.0 (5) |
N6—C8—C9—N5 | −0.1 (7) | N3—Rh1—N17—C25 | −58.4 (5) |
C7—N5—C9—C8 | −0.2 (6) | N5—Rh1—N17—C25 | 121.1 (5) |
Rh1—N5—C9—C8 | −175.0 (5) | Rh2—Rh1—N17—C25 | 155 (3) |
N1—Rh1—N7—C10 | 85 (3) | N7—Rh1—N17—C28 | −137.2 (5) |
N3—Rh1—N7—C10 | 168.9 (4) | N1—Rh1—N17—C28 | 43.3 (5) |
N5—Rh1—N7—C10 | −7.6 (4) | N3—Rh1—N17—C28 | 122.8 (5) |
N17—Rh1—N7—C10 | 79.2 (4) | N5—Rh1—N17—C28 | −57.6 (5) |
Rh2—Rh1—N7—C10 | −98.8 (4) | Rh2—Rh1—N17—C28 | −23 (3) |
N1—Rh1—N7—C12 | −84 (3) | C28—N17—C25—C26 | −0.3 (11) |
N3—Rh1—N7—C12 | 0.8 (6) | Rh1—N17—C25—C26 | −179.1 (6) |
N5—Rh1—N7—C12 | −175.7 (6) | N17—C25—C26—N18 | 0.7 (14) |
N17—Rh1—N7—C12 | −88.9 (6) | C25—C26—N18—C27 | −0.7 (14) |
Rh2—Rh1—N7—C12 | 93.1 (6) | C26—N18—C27—C28 | 0.3 (13) |
C12—N7—C10—N8 | −1.6 (7) | C25—N17—C28—C27 | 0.0 (10) |
Rh1—N7—C10—N8 | −173.6 (4) | Rh1—N17—C28—C27 | 178.8 (5) |
C12—N7—C10—C7 | −179.8 (5) | N18—C27—C28—N17 | 0.0 (12) |
Rh1—N7—C10—C7 | 8.2 (6) | N13—Rh2—N19—C30 | 45.3 (4) |
N5—C7—C10—N7 | −3.3 (8) | N11—Rh2—N19—C30 | −134.2 (4) |
N6—C7—C10—N7 | 176.6 (6) | N9—Rh2—N19—C30 | −54.8 (4) |
N5—C7—C10—N8 | 179.1 (6) | N15—Rh2—N19—C30 | 124.9 (4) |
N6—C7—C10—N8 | −1.1 (12) | Rh1—Rh2—N19—C30 | 128 (26) |
N7—C10—N8—C11 | 1.8 (7) | N13—Rh2—N19—C29 | −134.8 (4) |
C7—C10—N8—C11 | 179.6 (6) | N11—Rh2—N19—C29 | 45.7 (4) |
C10—N8—C11—C12 | −1.2 (8) | N9—Rh2—N19—C29 | 125.1 (4) |
N8—C11—C12—N7 | 0.3 (8) | N15—Rh2—N19—C29 | −55.3 (4) |
C10—N7—C12—C11 | 0.8 (7) | Rh1—Rh2—N19—C29 | −53 (27) |
Rh1—N7—C12—C11 | 169.4 (5) | C30—N19—C29—C30i | 0.2 (9) |
N13—Rh2—N9—C13 | −169.6 (3) | Rh2—N19—C29—C30i | −179.6 (4) |
N11—Rh2—N9—C13 | 5.5 (3) | C29—N19—C30—C29i | −0.2 (9) |
N15—Rh2—N9—C13 | −86 (2) | Rh2—N19—C30—C29i | 179.6 (4) |
N19—Rh2—N9—C13 | −82.4 (4) | | |
Symmetry codes: (i) −x+1, −y+1, −z+1; (ii) −x, −y+1, −z+1. |
Hydrogen-bond geometry (Å, º) top
D—H···A | D—H | H···A | D···A | D—H···A |
N2—H2N···F1iii | 0.86 | 1.99 | 2.767 (7) | 149 |
N4—H4N···O7W | 0.86 | 1.91 | 2.773 (17) | 176 |
N4—H4N···O5W | 0.86 | 2.03 | 2.73 (3) | 138 |
N6—H6N···F1 | 0.86 | 1.99 | 2.794 (8) | 156 |
N6—H6N···F2 | 0.86 | 2.34 | 3.056 (9) | 142 |
N8—H8N···F3 | 0.86 | 1.94 | 2.794 (11) | 170 |
N10—H10N···O3W | 0.86 | 2.02 | 2.841 (8) | 159 |
N12—H12N···O8 | 0.86 | 2.27 | 3.067 (9) | 154 |
N12—H12N···O10 | 0.86 | 2.42 | 2.965 (9) | 122 |
N14—H14N···O11i | 0.86 | 2.44 | 3.011 (10) | 125 |
N14—H14N···O2 | 0.86 | 2.54 | 3.058 (13) | 119 |
N16—H16N···O4W | 0.86 | 2.04 | 2.856 (10) | 158 |
N16—H16N···O11i | 0.86 | 2.62 | 3.131 (10) | 120 |
Symmetry codes: (i) −x+1, −y+1, −z+1; (iii) x+1/2, −y+3/2, −z+1. |
Crystal data top
C60H60N38Rh4·8(ClO4)·11.41(H2O) | Dx = 1.847 Mg m−3 |
Mr = 2726.26 | Mo Kα radiation, λ = 0.71069 Å |
Orthorhombic, Pbca | Cell parameters from 19919 reflections |
a = 20.289 (4) Å | θ = 3.1–27.5° |
b = 21.524 (5) Å | µ = 0.99 mm−1 |
c = 22.450 (5) Å | T = 296 K |
V = 9804 (4) Å3 | Prismatic, red |
Z = 4 | 0.42 × 0.35 × 0.25 mm |
F(000) = 5488 | |
Data collection top
Rigaku/MSC Mercury CCD diffractometer | 11220 independent reflections |
Radiation source: rotating-anode X-ray tube | 8509 reflections with I > 2σ(I) |
Graphite monochromator | Rint = 0.104 |
Detector resolution: 14.6306 pixels mm-1 | θmax = 27.5°, θmin = 3.1° |
ω scans | h = −25→26 |
Absorption correction: numerical NUMABS (Higashi, 1999) | k = −17→27 |
Tmin = 0.807, Tmax = 0.884 | l = −29→29 |
72426 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)] = 0.092 | Hydrogen site location: inferred from neighbouring sites |
wR(F2) = 0.231 | H atoms treated by a mixture of independent and constrained refinement |
S = 1.15 | w = 1/[σ2(Fo2) + (0.0905P)2 + 33.6829P] where P = (Fo2 + 2Fc2)/3 |
11220 reflections | (Δ/σ)max = 0.001 |
706 parameters | Δρmax = 1.49 e Å−3 |
19 restraints | Δρmin = −1.06 e Å−3 |
Crystal data top
C60H60N38Rh4·8(ClO4)·11.41(H2O) | V = 9804 (4) Å3 |
Mr = 2726.26 | Z = 4 |
Orthorhombic, Pbca | Mo Kα radiation |
a = 20.289 (4) Å | µ = 0.99 mm−1 |
b = 21.524 (5) Å | T = 296 K |
c = 22.450 (5) Å | 0.42 × 0.35 × 0.25 mm |
Data collection top
Rigaku/MSC Mercury CCD diffractometer | 11220 independent reflections |
Absorption correction: numerical NUMABS (Higashi, 1999) | 8509 reflections with I > 2σ(I) |
Tmin = 0.807, Tmax = 0.884 | Rint = 0.104 |
72426 measured reflections | |
Refinement top
R[F2 > 2σ(F2)] = 0.092 | 19 restraints |
wR(F2) = 0.231 | H atoms treated by a mixture of independent and constrained refinement |
S = 1.15 | w = 1/[σ2(Fo2) + (0.0905P)2 + 33.6829P] where P = (Fo2 + 2Fc2)/3 |
11220 reflections | Δρmax = 1.49 e Å−3 |
706 parameters | Δρmin = −1.06 e Å−3 |
Special details top
Experimental. ???? |
Geometry. All e.s.d.'s (except the e.s.d. in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell e.s.d.'s are taken into account individually in the estimation of e.s.d.'s in distances, angles and torsion angles; correlations between e.s.d.'s in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell e.s.d.'s is used for estimating e.s.d.'s involving l.s. planes. |
Refinement. Refinement of F2 against ALL reflections. The weighted R-factor wR and goodness of fit S are based on F2, conventional R-factors R are based on F, with F set to zero for negative F2. The threshold expression of F2 > σ(F2) is used only for calculating R-factors(gt) etc. and is not relevant to the choice of reflections for refinement. R-factors based on F2 are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger. |
Fractional atomic coordinates and isotropic or equivalent isotropic displacement parameters (Å2) top | x | y | z | Uiso*/Ueq | Occ. (<1) |
Rh1 | 0.28661 (3) | 0.70345 (3) | 0.56605 (2) | 0.03821 (17) | |
Rh2 | 0.37753 (3) | 0.61688 (2) | 0.53858 (2) | 0.03527 (16) | |
N1 | 0.3341 (3) | 0.7707 (3) | 0.5160 (3) | 0.0470 (15) | |
C1 | 0.3720 (4) | 0.8078 (4) | 0.5485 (4) | 0.056 (2) | |
N2 | 0.3962 (4) | 0.8542 (3) | 0.5151 (4) | 0.069 (2) | |
H2N | 0.4211 | 0.8839 | 0.5272 | 0.083* | |
C2 | 0.3738 (5) | 0.8453 (4) | 0.4581 (5) | 0.070 (3) | |
H2 | 0.3832 | 0.8698 | 0.4250 | 0.085* | |
C3 | 0.3359 (4) | 0.7950 (4) | 0.4595 (4) | 0.056 (2) | |
H3 | 0.3137 | 0.7786 | 0.4269 | 0.067* | |
N3 | 0.3474 (3) | 0.7431 (3) | 0.6295 (3) | 0.0490 (15) | |
C4 | 0.3805 (4) | 0.7923 (4) | 0.6101 (4) | 0.058 (2) | |
N4 | 0.4179 (4) | 0.8155 (4) | 0.6541 (4) | 0.075 (2) | |
H4N | 0.4441 | 0.8469 | 0.6518 | 0.090* | |
C5 | 0.4067 (6) | 0.7801 (6) | 0.7024 (5) | 0.084 (3) | |
H5 | 0.4259 | 0.7856 | 0.7397 | 0.101* | |
C6 | 0.3633 (5) | 0.7357 (5) | 0.6880 (4) | 0.067 (3) | |
H6 | 0.3469 | 0.7052 | 0.7134 | 0.081* | |
N5 | 0.2218 (3) | 0.6667 (3) | 0.5047 (3) | 0.0408 (13) | |
C7 | 0.1783 (4) | 0.6287 (4) | 0.5302 (4) | 0.0507 (19) | |
N6 | 0.1350 (4) | 0.6086 (4) | 0.4889 (4) | 0.063 (2) | |
H6N | 0.1020 | 0.5843 | 0.4950 | 0.076* | |
C8 | 0.1532 (5) | 0.6340 (5) | 0.4357 (5) | 0.066 (3) | |
H8 | 0.1327 | 0.6271 | 0.3993 | 0.080* | |
C9 | 0.2064 (4) | 0.6710 (4) | 0.4450 (4) | 0.055 (2) | |
H9 | 0.2282 | 0.6947 | 0.4166 | 0.065* | |
N7 | 0.2356 (3) | 0.6428 (3) | 0.6188 (3) | 0.0467 (15) | |
C10 | 0.1848 (4) | 0.6171 (3) | 0.5927 (4) | 0.0485 (18) | |
N8 | 0.1505 (4) | 0.5832 (4) | 0.6319 (4) | 0.065 (2) | |
H8N | 0.1164 | 0.5609 | 0.6240 | 0.078* | |
C11 | 0.1791 (5) | 0.5902 (5) | 0.6865 (4) | 0.068 (3) | |
H11 | 0.1648 | 0.5736 | 0.7224 | 0.082* | |
C12 | 0.2316 (5) | 0.6258 (4) | 0.6776 (4) | 0.063 (2) | |
H12 | 0.2615 | 0.6375 | 0.7069 | 0.075* | |
N9 | 0.4530 (3) | 0.6796 (3) | 0.5470 (3) | 0.0398 (13) | |
C13 | 0.4828 (4) | 0.6769 (4) | 0.5995 (4) | 0.0489 (18) | |
N10 | 0.5329 (3) | 0.7177 (3) | 0.6013 (3) | 0.0581 (18) | |
H10N | 0.5583 | 0.7251 | 0.6311 | 0.070* | |
C14 | 0.5356 (4) | 0.7451 (4) | 0.5460 (4) | 0.063 (2) | |
H14 | 0.5656 | 0.7752 | 0.5340 | 0.076* | |
C15 | 0.4881 (4) | 0.7213 (3) | 0.5132 (4) | 0.0519 (19) | |
H15 | 0.4797 | 0.7312 | 0.4736 | 0.062* | |
N11 | 0.4022 (3) | 0.6039 (3) | 0.6265 (3) | 0.0423 (14) | |
C16 | 0.4560 (4) | 0.6349 (3) | 0.6425 (3) | 0.0439 (17) | |
N12 | 0.4732 (4) | 0.6189 (4) | 0.6979 (3) | 0.064 (2) | |
H12N | 0.5058 | 0.6336 | 0.7179 | 0.077* | |
C17 | 0.4302 (5) | 0.5754 (4) | 0.7169 (4) | 0.064 (2) | |
H17 | 0.4309 | 0.5554 | 0.7536 | 0.076* | |
C18 | 0.3861 (4) | 0.5661 (4) | 0.6727 (3) | 0.0526 (19) | |
H18 | 0.3508 | 0.5385 | 0.6737 | 0.063* | |
N13 | 0.3591 (3) | 0.6256 (3) | 0.4492 (3) | 0.0412 (13) | |
C19 | 0.3220 (4) | 0.5800 (4) | 0.4277 (3) | 0.0471 (17) | |
N14 | 0.3204 (4) | 0.5829 (4) | 0.3681 (3) | 0.065 (2) | |
H14N | 0.2993 | 0.5582 | 0.3448 | 0.078* | |
C20 | 0.3580 (6) | 0.6318 (5) | 0.3510 (4) | 0.073 (3) | |
H20 | 0.3657 | 0.6451 | 0.3122 | 0.088* | |
C21 | 0.3821 (4) | 0.6571 (4) | 0.4014 (4) | 0.055 (2) | |
H21 | 0.4104 | 0.6911 | 0.4031 | 0.066* | |
N15 | 0.3074 (3) | 0.5487 (3) | 0.5275 (3) | 0.0393 (13) | |
C22 | 0.2913 (4) | 0.5394 (3) | 0.4711 (4) | 0.0447 (17) | |
N16 | 0.2485 (4) | 0.4928 (3) | 0.4661 (3) | 0.0596 (18) | |
H16N | 0.2311 | 0.4796 | 0.4335 | 0.072* | |
C23 | 0.2372 (5) | 0.4700 (4) | 0.5209 (4) | 0.062 (2) | |
H23 | 0.2102 | 0.4366 | 0.5306 | 0.074* | |
C24 | 0.2732 (4) | 0.5052 (4) | 0.5594 (4) | 0.0519 (19) | |
H24 | 0.2744 | 0.5005 | 0.6006 | 0.062* | |
N17 | 0.2086 (3) | 0.7745 (3) | 0.5835 (3) | 0.0459 (14) | |
C25 | 0.1804 (5) | 0.7835 (4) | 0.6359 (4) | 0.060 (2) | |
H25 | 0.1938 | 0.7600 | 0.6684 | 0.072* | |
C26 | 0.1315 (6) | 0.8271 (5) | 0.6430 (5) | 0.081 (3) | |
H26 | 0.1135 | 0.8323 | 0.6807 | 0.097* | |
N18 | 0.1088 (4) | 0.8620 (4) | 0.5992 (4) | 0.075 (2) | |
C27 | 0.1375 (5) | 0.8526 (4) | 0.5473 (4) | 0.063 (2) | |
H27 | 0.1239 | 0.8759 | 0.5147 | 0.076* | |
C28 | 0.1870 (4) | 0.8094 (4) | 0.5397 (4) | 0.057 (2) | |
H28 | 0.2057 | 0.8049 | 0.5021 | 0.068* | |
N19 | 0.4529 (3) | 0.5445 (3) | 0.5144 (3) | 0.0393 (13) | |
C29 | 0.4577 (4) | 0.4910 (3) | 0.5438 (3) | 0.0413 (16) | |
H29 | 0.4287 | 0.4832 | 0.5750 | 0.050* | |
C30 | 0.4959 (4) | 0.5532 (3) | 0.4705 (3) | 0.0445 (17) | |
H30 | 0.4946 | 0.5901 | 0.4489 | 0.053* | |
Cl1 | 0.2784 (2) | 0.58212 (17) | 0.20406 (19) | 0.1286 (15) | |
O1 | 0.2231 (7) | 0.5460 (6) | 0.2042 (7) | 0.187 (6) | |
O2 | 0.3295 (8) | 0.5535 (5) | 0.2354 (6) | 0.193 (7) | |
O3 | 0.2972 (8) | 0.5916 (7) | 0.1422 (5) | 0.198 (7) | |
O4 | 0.2645 (7) | 0.6403 (4) | 0.2322 (5) | 0.165 (5) | |
Cl2 | 0.50756 (14) | 0.69240 (14) | 0.84318 (12) | 0.0789 (7) | |
O5 | 0.4635 (8) | 0.6450 (8) | 0.8381 (6) | 0.220 (8) | |
O6 | 0.5378 (5) | 0.6906 (6) | 0.8985 (4) | 0.137 (4) | |
O7 | 0.4742 (8) | 0.7450 (7) | 0.8379 (5) | 0.217 (8) | |
O8 | 0.5518 (4) | 0.6851 (5) | 0.7955 (4) | 0.111 (3) | |
Cl3 | 0.64676 (16) | 0.59659 (16) | 0.63272 (13) | 0.0886 (9) | |
O9 | 0.6855 (6) | 0.6403 (6) | 0.5983 (5) | 0.158 (5) | |
O10 | 0.6163 (4) | 0.6302 (4) | 0.6793 (4) | 0.104 (3) | |
O11 | 0.6923 (5) | 0.5536 (4) | 0.6566 (4) | 0.125 (3) | |
O12 | 0.6007 (5) | 0.5672 (5) | 0.5943 (5) | 0.140 (4) | |
Cl4 | 0.00139 (18) | 0.48605 (18) | 0.59243 (19) | 0.1097 (11) | |
O13 | −0.0592 (5) | 0.5080 (6) | 0.5705 (7) | 0.178 (6) | |
O14 | 0.0024 (5) | 0.4208 (4) | 0.5774 (6) | 0.152 (5) | |
O15 | 0.0519 (6) | 0.5168 (7) | 0.5621 (6) | 0.191 (6) | |
O16 | 0.0074 (9) | 0.4967 (7) | 0.6545 (6) | 0.214 (7) | |
O1W | 0.3173 (6) | 0.8456 (6) | 0.3115 (4) | 0.142 (4) | |
O2W | 0.2372 (6) | 0.7423 (6) | 0.3120 (5) | 0.156 (4) | |
O3W | 0.5991 (5) | 0.7671 (4) | 0.7013 (4) | 0.119 (3) | |
O4W | 0.1792 (6) | 0.4799 (7) | 0.3533 (6) | 0.190 (6) | |
O5W | 0.523 (2) | 0.8785 (19) | 0.702 (3) | 0.18 (2) | 0.30 (3) |
O6W | 0.6142 (17) | 0.9137 (13) | 0.7117 (11) | 0.277 (18) | 0.70 (3) |
O7W | 0.4892 (16) | 0.9167 (16) | 0.770 (2) | 0.34 (2) | 0.70 (3) |
Atomic displacement parameters (Å2) top | U11 | U22 | U33 | U12 | U13 | U23 |
Rh1 | 0.0368 (3) | 0.0390 (3) | 0.0388 (3) | 0.0020 (2) | −0.0010 (2) | −0.0019 (2) |
Rh2 | 0.0337 (3) | 0.0343 (3) | 0.0378 (3) | −0.0003 (2) | 0.0013 (2) | −0.0016 (2) |
N1 | 0.045 (4) | 0.041 (3) | 0.055 (4) | 0.000 (3) | 0.005 (3) | −0.002 (3) |
C1 | 0.045 (4) | 0.046 (4) | 0.076 (6) | 0.010 (4) | 0.005 (4) | −0.003 (4) |
N2 | 0.061 (5) | 0.041 (4) | 0.105 (7) | −0.007 (3) | 0.017 (5) | −0.005 (4) |
C2 | 0.067 (6) | 0.053 (5) | 0.091 (8) | 0.006 (4) | 0.022 (6) | 0.002 (5) |
C3 | 0.057 (5) | 0.052 (5) | 0.060 (5) | −0.001 (4) | 0.008 (4) | 0.005 (4) |
N3 | 0.044 (3) | 0.053 (4) | 0.050 (4) | 0.004 (3) | −0.005 (3) | −0.015 (3) |
C4 | 0.047 (5) | 0.051 (5) | 0.076 (6) | 0.006 (4) | −0.011 (4) | −0.020 (4) |
N4 | 0.069 (5) | 0.071 (5) | 0.084 (6) | −0.001 (4) | −0.018 (5) | −0.030 (5) |
C5 | 0.079 (7) | 0.101 (8) | 0.072 (7) | 0.016 (6) | −0.019 (6) | −0.042 (7) |
C6 | 0.063 (6) | 0.085 (7) | 0.053 (5) | 0.019 (5) | −0.007 (4) | −0.018 (5) |
N5 | 0.042 (3) | 0.039 (3) | 0.042 (3) | 0.002 (3) | 0.001 (3) | −0.002 (3) |
C7 | 0.037 (4) | 0.047 (4) | 0.068 (5) | −0.003 (3) | −0.002 (4) | −0.018 (4) |
N6 | 0.051 (4) | 0.063 (5) | 0.076 (5) | −0.007 (3) | −0.009 (4) | −0.012 (4) |
C8 | 0.053 (5) | 0.075 (6) | 0.072 (6) | 0.018 (5) | −0.023 (5) | −0.024 (5) |
C9 | 0.058 (5) | 0.051 (5) | 0.054 (5) | 0.015 (4) | −0.009 (4) | −0.003 (4) |
N7 | 0.052 (4) | 0.047 (4) | 0.041 (3) | 0.010 (3) | 0.008 (3) | 0.002 (3) |
C10 | 0.045 (4) | 0.040 (4) | 0.061 (5) | 0.008 (3) | 0.009 (4) | −0.004 (4) |
N8 | 0.049 (4) | 0.063 (5) | 0.082 (6) | −0.003 (3) | 0.023 (4) | 0.006 (4) |
C11 | 0.078 (7) | 0.081 (7) | 0.046 (5) | 0.016 (5) | 0.021 (5) | 0.016 (5) |
C12 | 0.078 (6) | 0.058 (5) | 0.052 (5) | 0.013 (5) | 0.013 (5) | 0.009 (4) |
N9 | 0.039 (3) | 0.031 (3) | 0.049 (3) | 0.005 (2) | 0.000 (3) | −0.002 (2) |
C13 | 0.047 (4) | 0.049 (4) | 0.050 (4) | −0.003 (3) | −0.005 (4) | −0.009 (4) |
N10 | 0.046 (4) | 0.064 (4) | 0.064 (5) | −0.002 (3) | −0.012 (3) | −0.016 (4) |
C14 | 0.051 (5) | 0.052 (5) | 0.086 (7) | −0.010 (4) | 0.010 (5) | −0.005 (5) |
C15 | 0.046 (4) | 0.039 (4) | 0.070 (5) | −0.004 (3) | 0.009 (4) | 0.000 (4) |
N11 | 0.046 (3) | 0.041 (3) | 0.040 (3) | 0.000 (3) | 0.002 (3) | −0.005 (3) |
C16 | 0.035 (4) | 0.048 (4) | 0.048 (4) | 0.009 (3) | −0.004 (3) | −0.011 (3) |
N12 | 0.056 (4) | 0.077 (5) | 0.060 (4) | 0.005 (4) | −0.018 (4) | −0.008 (4) |
C17 | 0.080 (6) | 0.062 (5) | 0.049 (5) | −0.002 (5) | −0.004 (5) | 0.001 (4) |
C18 | 0.055 (5) | 0.058 (5) | 0.045 (4) | 0.001 (4) | 0.004 (4) | 0.001 (4) |
N13 | 0.039 (3) | 0.043 (3) | 0.041 (3) | 0.002 (3) | 0.004 (3) | −0.003 (3) |
C19 | 0.047 (4) | 0.052 (4) | 0.043 (4) | −0.008 (3) | −0.003 (3) | −0.004 (3) |
N14 | 0.079 (5) | 0.071 (5) | 0.045 (4) | −0.018 (4) | −0.005 (4) | −0.007 (4) |
C20 | 0.096 (8) | 0.072 (6) | 0.052 (5) | −0.020 (6) | −0.001 (5) | 0.014 (5) |
C21 | 0.058 (5) | 0.060 (5) | 0.048 (4) | −0.003 (4) | 0.002 (4) | 0.009 (4) |
N15 | 0.035 (3) | 0.041 (3) | 0.041 (3) | −0.002 (2) | 0.005 (2) | 0.001 (3) |
C22 | 0.041 (4) | 0.035 (4) | 0.058 (5) | −0.001 (3) | −0.004 (3) | −0.012 (3) |
N16 | 0.055 (4) | 0.056 (4) | 0.068 (5) | −0.017 (3) | −0.007 (4) | −0.018 (4) |
C23 | 0.060 (5) | 0.053 (5) | 0.072 (6) | −0.021 (4) | 0.012 (5) | −0.005 (4) |
C24 | 0.042 (4) | 0.053 (5) | 0.060 (5) | 0.004 (3) | 0.013 (4) | 0.004 (4) |
N17 | 0.039 (3) | 0.042 (3) | 0.056 (4) | 0.007 (3) | −0.004 (3) | 0.000 (3) |
C25 | 0.063 (5) | 0.058 (5) | 0.060 (5) | 0.024 (4) | 0.005 (4) | 0.003 (4) |
C26 | 0.097 (8) | 0.083 (7) | 0.064 (6) | 0.024 (6) | 0.027 (6) | −0.003 (5) |
N18 | 0.083 (6) | 0.071 (5) | 0.071 (5) | 0.035 (4) | 0.010 (4) | 0.006 (4) |
C27 | 0.073 (6) | 0.058 (5) | 0.059 (5) | 0.026 (5) | 0.008 (5) | 0.011 (4) |
C28 | 0.052 (5) | 0.065 (5) | 0.053 (5) | 0.014 (4) | 0.002 (4) | 0.003 (4) |
N19 | 0.040 (3) | 0.033 (3) | 0.044 (3) | −0.001 (2) | 0.005 (3) | −0.001 (2) |
C29 | 0.043 (4) | 0.041 (4) | 0.040 (4) | 0.007 (3) | 0.008 (3) | 0.006 (3) |
C30 | 0.042 (4) | 0.036 (4) | 0.055 (4) | 0.007 (3) | 0.003 (3) | 0.008 (3) |
Cl1 | 0.189 (4) | 0.079 (2) | 0.118 (3) | −0.028 (2) | −0.069 (3) | −0.004 (2) |
O1 | 0.190 (12) | 0.153 (11) | 0.219 (14) | −0.105 (10) | 0.013 (10) | −0.046 (10) |
O2 | 0.303 (18) | 0.129 (9) | 0.147 (10) | 0.042 (11) | −0.126 (12) | −0.020 (8) |
O3 | 0.308 (18) | 0.201 (13) | 0.085 (7) | −0.123 (13) | −0.023 (9) | −0.010 (8) |
O4 | 0.251 (13) | 0.068 (5) | 0.177 (11) | −0.004 (7) | −0.120 (10) | −0.037 (6) |
Cl2 | 0.0708 (16) | 0.099 (2) | 0.0673 (15) | 0.0153 (14) | 0.0043 (12) | −0.0202 (14) |
O5 | 0.260 (17) | 0.245 (16) | 0.154 (11) | −0.161 (15) | 0.061 (11) | −0.075 (11) |
O6 | 0.131 (8) | 0.215 (12) | 0.065 (5) | 0.030 (8) | −0.015 (5) | −0.040 (6) |
O7 | 0.299 (18) | 0.232 (15) | 0.120 (9) | 0.196 (15) | 0.014 (10) | 0.000 (9) |
O8 | 0.091 (6) | 0.167 (9) | 0.075 (5) | 0.020 (6) | 0.024 (5) | −0.016 (5) |
Cl3 | 0.090 (2) | 0.103 (2) | 0.0733 (17) | 0.0298 (17) | −0.0069 (15) | −0.0128 (16) |
O9 | 0.157 (10) | 0.180 (11) | 0.136 (9) | −0.052 (9) | 0.016 (8) | 0.050 (9) |
O10 | 0.084 (5) | 0.152 (8) | 0.076 (5) | 0.048 (5) | 0.000 (4) | −0.032 (5) |
O11 | 0.155 (9) | 0.103 (7) | 0.117 (7) | 0.061 (6) | −0.032 (6) | −0.019 (6) |
O12 | 0.122 (8) | 0.179 (11) | 0.119 (8) | −0.001 (7) | −0.045 (6) | −0.061 (8) |
Cl4 | 0.093 (2) | 0.109 (3) | 0.128 (3) | −0.013 (2) | 0.006 (2) | −0.034 (2) |
O13 | 0.091 (8) | 0.150 (10) | 0.293 (17) | 0.043 (7) | −0.045 (9) | −0.057 (11) |
O14 | 0.101 (7) | 0.078 (6) | 0.277 (15) | −0.003 (5) | 0.031 (8) | −0.048 (8) |
O15 | 0.149 (11) | 0.220 (14) | 0.202 (13) | −0.125 (10) | 0.049 (9) | −0.019 (10) |
O16 | 0.32 (2) | 0.222 (15) | 0.097 (8) | 0.027 (15) | −0.015 (11) | −0.050 (9) |
O1W | 0.162 (10) | 0.171 (10) | 0.094 (7) | 0.000 (8) | −0.006 (7) | −0.023 (7) |
O2W | 0.133 (10) | 0.170 (11) | 0.165 (11) | 0.029 (8) | 0.026 (8) | 0.018 (9) |
O3W | 0.135 (8) | 0.115 (7) | 0.108 (7) | −0.020 (6) | −0.019 (6) | −0.038 (6) |
O4W | 0.152 (11) | 0.260 (15) | 0.159 (11) | 0.061 (11) | −0.066 (9) | −0.104 (11) |
O5W | 0.18 (4) | 0.14 (3) | 0.23 (4) | −0.11 (3) | −0.06 (3) | 0.02 (3) |
O6W | 0.42 (4) | 0.26 (3) | 0.150 (19) | 0.14 (3) | −0.02 (2) | −0.012 (18) |
O7W | 0.29 (3) | 0.28 (3) | 0.44 (4) | −0.10 (2) | 0.08 (3) | 0.13 (3) |
Geometric parameters (Å, º) top
Rh1—N7 | 2.043 (6) | C16—N12 | 1.337 (10) |
Rh1—N5 | 2.062 (6) | N12—C17 | 1.348 (11) |
Rh1—N3 | 2.069 (6) | N12—H12N | 0.8600 |
Rh1—N1 | 2.071 (6) | C17—C18 | 1.352 (12) |
Rh1—N17 | 2.235 (6) | C17—H17 | 0.9300 |
Rh1—Rh2 | 2.6935 (8) | C18—H18 | 0.9300 |
Rh2—N13 | 2.049 (6) | N13—C19 | 1.327 (9) |
Rh2—N9 | 2.050 (6) | N13—C21 | 1.354 (10) |
Rh2—N11 | 2.056 (6) | C19—N14 | 1.341 (10) |
Rh2—N15 | 2.059 (6) | C19—C22 | 1.449 (11) |
Rh2—N19 | 2.248 (6) | N14—C20 | 1.354 (12) |
N1—C1 | 1.327 (11) | N14—H14N | 0.8600 |
N1—C3 | 1.372 (10) | C20—C21 | 1.348 (13) |
C1—N2 | 1.341 (11) | C20—H20 | 0.9300 |
C1—C4 | 1.434 (13) | C21—H21 | 0.9300 |
N2—C2 | 1.371 (13) | N15—C22 | 1.323 (9) |
N2—H2N | 0.8600 | N15—C24 | 1.367 (10) |
C2—C3 | 1.329 (13) | C22—N16 | 1.332 (9) |
C2—H2 | 0.9300 | N16—C23 | 1.343 (11) |
C3—H3 | 0.9300 | N16—H16N | 0.8600 |
N3—C4 | 1.328 (11) | C23—C24 | 1.364 (12) |
N3—C6 | 1.361 (11) | C23—H23 | 0.9300 |
C4—N4 | 1.341 (11) | C24—H24 | 0.9300 |
N4—C5 | 1.345 (14) | N17—C28 | 1.314 (10) |
N4—H4N | 0.8600 | N17—C25 | 1.323 (10) |
C5—C6 | 1.341 (15) | C25—C26 | 1.374 (13) |
C5—H5 | 0.9300 | C25—H25 | 0.9300 |
C6—H6 | 0.9300 | C26—N18 | 1.320 (13) |
N5—C7 | 1.334 (10) | C26—H26 | 0.9300 |
N5—C9 | 1.379 (10) | N18—C27 | 1.319 (11) |
C7—N6 | 1.347 (10) | C27—C28 | 1.379 (12) |
C7—C10 | 1.432 (12) | C27—H27 | 0.9300 |
N6—C8 | 1.364 (13) | C28—H28 | 0.9300 |
N6—H6N | 0.8600 | N19—C30 | 1.331 (9) |
C8—C9 | 1.356 (13) | N19—C29 | 1.331 (9) |
C8—H8 | 0.9300 | C29—C30i | 1.378 (10) |
C9—H9 | 0.9300 | C29—H29 | 0.9300 |
N7—C10 | 1.308 (10) | C30—C29i | 1.378 (10) |
N7—C12 | 1.372 (10) | C30—H30 | 0.9300 |
C10—N8 | 1.339 (10) | Cl1—O1 | 1.365 (11) |
N8—C11 | 1.365 (12) | Cl1—O2 | 1.396 (12) |
N8—H8N | 0.8600 | Cl1—O4 | 1.431 (10) |
C11—C12 | 1.327 (13) | Cl1—O3 | 1.454 (12) |
C11—H11 | 0.9300 | Cl2—O7 | 1.324 (11) |
C12—H12 | 0.9300 | Cl2—O5 | 1.361 (12) |
N9—C13 | 1.325 (10) | Cl2—O6 | 1.385 (9) |
N9—C15 | 1.375 (10) | Cl2—O8 | 1.406 (8) |
C13—N10 | 1.344 (10) | Cl3—O10 | 1.413 (8) |
C13—C16 | 1.430 (11) | Cl3—O11 | 1.413 (9) |
N10—C14 | 1.374 (12) | Cl3—O12 | 1.421 (9) |
N10—H10N | 0.8600 | Cl3—O9 | 1.449 (10) |
C14—C15 | 1.316 (12) | Cl4—O15 | 1.396 (10) |
C14—H14 | 0.9300 | Cl4—O13 | 1.406 (11) |
C15—H15 | 0.9300 | Cl4—O16 | 1.418 (12) |
N11—C16 | 1.329 (9) | Cl4—O14 | 1.444 (9) |
N11—C18 | 1.357 (10) | | |
| | | |
N7—Rh1—N5 | 79.6 (3) | C15—C14—H14 | 126.0 |
N7—Rh1—N3 | 99.6 (3) | N10—C14—H14 | 126.0 |
N5—Rh1—N3 | 176.9 (2) | C14—C15—N9 | 108.9 (8) |
N7—Rh1—N1 | 175.3 (2) | C14—C15—H15 | 125.5 |
N5—Rh1—N1 | 101.7 (3) | N9—C15—H15 | 125.5 |
N3—Rh1—N1 | 78.9 (3) | C16—N11—C18 | 107.0 (7) |
N7—Rh1—N17 | 88.7 (2) | C16—N11—Rh2 | 113.0 (5) |
N5—Rh1—N17 | 85.9 (2) | C18—N11—Rh2 | 139.1 (5) |
N3—Rh1—N17 | 91.1 (2) | N11—C16—N12 | 109.6 (7) |
N1—Rh1—N17 | 86.9 (2) | N11—C16—C13 | 116.6 (7) |
N7—Rh1—Rh2 | 92.15 (17) | N12—C16—C13 | 133.8 (7) |
N5—Rh1—Rh2 | 91.04 (16) | C16—N12—C17 | 107.8 (7) |
N3—Rh1—Rh2 | 91.96 (18) | C16—N12—H12N | 126.1 |
N1—Rh1—Rh2 | 92.34 (17) | C17—N12—H12N | 126.1 |
N17—Rh1—Rh2 | 176.61 (17) | N12—C17—C18 | 107.4 (8) |
N13—Rh2—N9 | 99.6 (2) | N12—C17—H17 | 126.3 |
N13—Rh2—N11 | 175.6 (2) | C18—C17—H17 | 126.3 |
N9—Rh2—N11 | 79.6 (2) | C17—C18—N11 | 108.2 (8) |
N13—Rh2—N15 | 79.7 (2) | C17—C18—H18 | 125.9 |
N9—Rh2—N15 | 175.2 (2) | N11—C18—H18 | 125.9 |
N11—Rh2—N15 | 100.8 (2) | C19—N13—C21 | 106.2 (7) |
N13—Rh2—N19 | 87.2 (2) | C19—N13—Rh2 | 113.1 (5) |
N9—Rh2—N19 | 88.3 (2) | C21—N13—Rh2 | 139.3 (6) |
N11—Rh2—N19 | 88.4 (2) | N13—C19—N14 | 110.0 (7) |
N15—Rh2—N19 | 87.0 (2) | N13—C19—C22 | 116.3 (6) |
N13—Rh2—Rh1 | 92.05 (17) | N14—C19—C22 | 133.7 (7) |
N9—Rh2—Rh1 | 92.01 (16) | C19—N14—C20 | 107.8 (7) |
N11—Rh2—Rh1 | 92.33 (17) | C19—N14—H14N | 126.1 |
N15—Rh2—Rh1 | 92.72 (16) | C20—N14—H14N | 126.1 |
N19—Rh2—Rh1 | 179.23 (16) | C21—C20—N14 | 106.3 (8) |
C1—N1—C3 | 105.3 (7) | C21—C20—H20 | 126.9 |
C1—N1—Rh1 | 113.1 (6) | N14—C20—H20 | 126.9 |
C3—N1—Rh1 | 141.2 (6) | C20—C21—N13 | 109.7 (8) |
N1—C1—N2 | 110.6 (9) | C20—C21—H21 | 125.1 |
N1—C1—C4 | 117.4 (8) | N13—C21—H21 | 125.1 |
N2—C1—C4 | 132.0 (9) | C22—N15—C24 | 105.9 (6) |
C1—N2—C2 | 107.3 (8) | C22—N15—Rh2 | 113.1 (5) |
C1—N2—H2N | 126.3 | C24—N15—Rh2 | 140.8 (6) |
C2—N2—H2N | 126.3 | N15—C22—N16 | 110.8 (7) |
C3—C2—N2 | 106.4 (9) | N15—C22—C19 | 116.6 (6) |
C3—C2—H2 | 126.8 | N16—C22—C19 | 132.6 (7) |
N2—C2—H2 | 126.8 | C22—N16—C23 | 108.0 (7) |
C2—C3—N1 | 110.3 (9) | C22—N16—H16N | 126.0 |
C2—C3—H3 | 124.8 | C23—N16—H16N | 126.0 |
N1—C3—H3 | 124.8 | N16—C23—C24 | 106.6 (7) |
C4—N3—C6 | 106.9 (8) | N16—C23—H23 | 126.7 |
C4—N3—Rh1 | 113.9 (6) | C24—C23—H23 | 126.7 |
C6—N3—Rh1 | 139.2 (7) | C23—C24—N15 | 108.7 (8) |
N3—C4—N4 | 110.0 (9) | C23—C24—H24 | 125.7 |
N3—C4—C1 | 116.2 (7) | N15—C24—H24 | 125.7 |
N4—C4—C1 | 133.7 (10) | C28—N17—C25 | 115.9 (7) |
C4—N4—C5 | 106.7 (9) | C28—N17—Rh1 | 119.8 (6) |
C4—N4—H4N | 126.6 | C25—N17—Rh1 | 124.3 (5) |
C5—N4—H4N | 126.6 | N17—C25—C26 | 121.1 (8) |
C6—C5—N4 | 108.7 (9) | N17—C25—H25 | 119.5 |
C6—C5—H5 | 125.7 | C26—C25—H25 | 119.5 |
N4—C5—H5 | 125.7 | N18—C26—C25 | 123.7 (9) |
C5—C6—N3 | 107.8 (10) | N18—C26—H26 | 118.2 |
C5—C6—H6 | 126.1 | C25—C26—H26 | 118.2 |
N3—C6—H6 | 126.1 | C27—N18—C26 | 114.6 (8) |
C7—N5—C9 | 107.9 (7) | N18—C27—C28 | 122.4 (9) |
C7—N5—Rh1 | 111.8 (5) | N18—C27—H27 | 118.8 |
C9—N5—Rh1 | 140.3 (6) | C28—C27—H27 | 118.8 |
N5—C7—N6 | 109.5 (8) | N17—C28—C27 | 122.4 (8) |
N5—C7—C10 | 117.8 (7) | N17—C28—H28 | 118.8 |
N6—C7—C10 | 132.8 (8) | C27—C28—H28 | 118.8 |
C7—N6—C8 | 107.3 (8) | C30—N19—C29 | 116.2 (6) |
C7—N6—H6N | 126.3 | C30—N19—Rh2 | 121.8 (5) |
C8—N6—H6N | 126.3 | C29—N19—Rh2 | 122.0 (5) |
C9—C8—N6 | 108.4 (8) | N19—C29—C30i | 122.2 (7) |
C9—C8—H8 | 125.8 | N19—C29—H29 | 118.9 |
N6—C8—H8 | 125.8 | C30i—C29—H29 | 118.9 |
C8—C9—N5 | 107.0 (8) | N19—C30—C29i | 121.6 (7) |
C8—C9—H9 | 126.5 | N19—C30—H30 | 119.2 |
N5—C9—H9 | 126.5 | C29i—C30—H30 | 119.2 |
C10—N7—C12 | 105.7 (7) | O1—Cl1—O2 | 111.0 (10) |
C10—N7—Rh1 | 114.2 (5) | O1—Cl1—O4 | 109.6 (9) |
C12—N7—Rh1 | 139.3 (6) | O2—Cl1—O4 | 108.0 (7) |
N7—C10—N8 | 110.3 (8) | O1—Cl1—O3 | 107.3 (8) |
N7—C10—C7 | 116.0 (7) | O2—Cl1—O3 | 110.4 (10) |
N8—C10—C7 | 133.7 (8) | O4—Cl1—O3 | 110.5 (8) |
C10—N8—C11 | 107.9 (8) | O7—Cl2—O5 | 107.2 (12) |
C10—N8—H8N | 126.1 | O7—Cl2—O6 | 109.3 (8) |
C11—N8—H8N | 126.1 | O5—Cl2—O6 | 110.2 (9) |
C12—C11—N8 | 105.7 (8) | O7—Cl2—O8 | 110.8 (8) |
C12—C11—H11 | 127.1 | O5—Cl2—O8 | 105.7 (7) |
N8—C11—H11 | 127.1 | O6—Cl2—O8 | 113.4 (6) |
C11—C12—N7 | 110.3 (9) | O10—Cl3—O11 | 109.9 (6) |
C11—C12—H12 | 124.9 | O10—Cl3—O12 | 113.0 (6) |
N7—C12—H12 | 124.9 | O11—Cl3—O12 | 111.6 (7) |
C13—N9—C15 | 106.4 (7) | O10—Cl3—O9 | 107.3 (7) |
C13—N9—Rh2 | 113.2 (5) | O11—Cl3—O9 | 105.9 (8) |
C15—N9—Rh2 | 140.0 (6) | O12—Cl3—O9 | 108.8 (7) |
N9—C13—N10 | 110.1 (7) | O15—Cl4—O13 | 108.2 (10) |
N9—C13—C16 | 117.0 (7) | O15—Cl4—O16 | 109.8 (10) |
N10—C13—C16 | 132.9 (8) | O13—Cl4—O16 | 111.4 (10) |
C13—N10—C14 | 106.5 (7) | O15—Cl4—O14 | 109.6 (8) |
C13—N10—H10N | 126.8 | O13—Cl4—O14 | 105.0 (7) |
C14—N10—H10N | 126.8 | O16—Cl4—O14 | 112.6 (10) |
C15—C14—N10 | 108.0 (8) | | |
| | | |
N7—Rh1—Rh2—N13 | 122.2 (3) | Rh1—Rh2—N9—C13 | 97.9 (5) |
N5—Rh1—Rh2—N13 | 42.5 (2) | N13—Rh2—N9—C15 | 2.3 (8) |
N3—Rh1—Rh2—N13 | −138.2 (3) | N11—Rh2—N9—C15 | 177.8 (8) |
N1—Rh1—Rh2—N13 | −59.2 (3) | N15—Rh2—N9—C15 | 83 (3) |
N17—Rh1—Rh2—N13 | 18 (3) | N19—Rh2—N9—C15 | 89.1 (8) |
N7—Rh1—Rh2—N9 | −138.1 (3) | Rh1—Rh2—N9—C15 | −90.2 (8) |
N5—Rh1—Rh2—N9 | 142.2 (2) | C15—N9—C13—N10 | 3.4 (9) |
N3—Rh1—Rh2—N9 | −38.5 (3) | Rh2—N9—C13—N10 | 178.0 (5) |
N1—Rh1—Rh2—N9 | 40.5 (2) | C15—N9—C13—C16 | −178.6 (7) |
N17—Rh1—Rh2—N9 | 118 (3) | Rh2—N9—C13—C16 | −4.0 (9) |
N7—Rh1—Rh2—N11 | −58.5 (3) | N9—C13—N10—C14 | −2.4 (9) |
N5—Rh1—Rh2—N11 | −138.1 (2) | C16—C13—N10—C14 | −180.0 (9) |
N3—Rh1—Rh2—N11 | 41.2 (3) | C13—N10—C14—C15 | 0.4 (10) |
N1—Rh1—Rh2—N11 | 120.1 (3) | N10—C14—C15—N9 | 1.6 (10) |
N17—Rh1—Rh2—N11 | −163 (3) | C13—N9—C15—C14 | −3.1 (9) |
N7—Rh1—Rh2—N15 | 42.4 (2) | Rh2—N9—C15—C14 | −175.4 (6) |
N5—Rh1—Rh2—N15 | −37.2 (2) | N13—Rh2—N11—C16 | 73 (3) |
N3—Rh1—Rh2—N15 | 142.1 (3) | N9—Rh2—N11—C16 | −6.9 (5) |
N1—Rh1—Rh2—N15 | −139.0 (2) | N15—Rh2—N11—C16 | 168.2 (5) |
N17—Rh1—Rh2—N15 | −62 (3) | N19—Rh2—N11—C16 | 81.6 (5) |
N7—Rh1—Rh2—N19 | 107 (11) | Rh1—Rh2—N11—C16 | −98.6 (5) |
N5—Rh1—Rh2—N19 | 27 (11) | N13—Rh2—N11—C18 | −94 (3) |
N3—Rh1—Rh2—N19 | −153 (11) | N9—Rh2—N11—C18 | −174.5 (8) |
N1—Rh1—Rh2—N19 | −74 (11) | N15—Rh2—N11—C18 | 0.7 (8) |
N17—Rh1—Rh2—N19 | 3 (12) | N19—Rh2—N11—C18 | −85.9 (8) |
N7—Rh1—N1—C1 | 65 (3) | Rh1—Rh2—N11—C18 | 93.9 (8) |
N5—Rh1—N1—C1 | 170.4 (5) | C18—N11—C16—N12 | −1.5 (8) |
N3—Rh1—N1—C1 | −6.5 (5) | Rh2—N11—C16—N12 | −173.0 (5) |
N17—Rh1—N1—C1 | 85.3 (6) | C18—N11—C16—C13 | 178.5 (7) |
Rh2—Rh1—N1—C1 | −98.0 (5) | Rh2—N11—C16—C13 | 7.0 (8) |
N7—Rh1—N1—C3 | −107 (3) | N9—C13—C16—N11 | −2.1 (10) |
N5—Rh1—N1—C3 | −1.3 (9) | N10—C13—C16—N11 | 175.3 (8) |
N3—Rh1—N1—C3 | −178.2 (9) | N9—C13—C16—N12 | 178.0 (8) |
N17—Rh1—N1—C3 | −86.5 (9) | N10—C13—C16—N12 | −4.6 (16) |
Rh2—Rh1—N1—C3 | 90.2 (9) | N11—C16—N12—C17 | 1.6 (9) |
C3—N1—C1—N2 | 1.0 (9) | C13—C16—N12—C17 | −178.4 (8) |
Rh1—N1—C1—N2 | −173.7 (5) | C16—N12—C17—C18 | −1.1 (10) |
C3—N1—C1—C4 | −178.6 (7) | N12—C17—C18—N11 | 0.1 (10) |
Rh1—N1—C1—C4 | 6.8 (9) | C16—N11—C18—C17 | 0.9 (9) |
N1—C1—N2—C2 | −1.5 (10) | Rh2—N11—C18—C17 | 168.8 (6) |
C4—C1—N2—C2 | 177.9 (9) | N9—Rh2—N13—C19 | 165.5 (5) |
C1—N2—C2—C3 | 1.4 (10) | N11—Rh2—N13—C19 | 86 (3) |
N2—C2—C3—N1 | −0.9 (10) | N15—Rh2—N13—C19 | −9.7 (5) |
C1—N1—C3—C2 | 0.0 (10) | N19—Rh2—N13—C19 | 77.7 (5) |
Rh1—N1—C3—C2 | 172.1 (7) | Rh1—Rh2—N13—C19 | −102.1 (5) |
N7—Rh1—N3—C4 | −170.1 (6) | N9—Rh2—N13—C21 | 1.5 (9) |
N5—Rh1—N3—C4 | −96 (5) | N11—Rh2—N13—C21 | −78 (3) |
N1—Rh1—N3—C4 | 5.4 (6) | N15—Rh2—N13—C21 | −173.7 (9) |
N17—Rh1—N3—C4 | −81.3 (6) | N19—Rh2—N13—C21 | −86.3 (8) |
Rh2—Rh1—N3—C4 | 97.4 (5) | Rh1—Rh2—N13—C21 | 93.9 (8) |
N7—Rh1—N3—C6 | 6.7 (9) | C21—N13—C19—N14 | −1.1 (9) |
N5—Rh1—N3—C6 | 81 (5) | Rh2—N13—C19—N14 | −170.3 (6) |
N1—Rh1—N3—C6 | −177.8 (9) | C21—N13—C19—C22 | −179.8 (7) |
N17—Rh1—N3—C6 | 95.6 (9) | Rh2—N13—C19—C22 | 11.0 (9) |
Rh2—Rh1—N3—C6 | −85.8 (8) | N13—C19—N14—C20 | 0.4 (11) |
C6—N3—C4—N4 | 1.4 (10) | C22—C19—N14—C20 | 178.7 (9) |
Rh1—N3—C4—N4 | 179.2 (5) | C19—N14—C20—C21 | 0.5 (12) |
C6—N3—C4—C1 | 178.7 (7) | N14—C20—C21—N13 | −1.2 (12) |
Rh1—N3—C4—C1 | −3.5 (9) | C19—N13—C21—C20 | 1.4 (10) |
N1—C1—C4—N3 | −2.3 (11) | Rh2—N13—C21—C20 | 166.1 (7) |
N2—C1—C4—N3 | 178.3 (8) | N13—Rh2—N15—C22 | 6.9 (5) |
N1—C1—C4—N4 | 174.2 (9) | N9—Rh2—N15—C22 | −75 (3) |
N2—C1—C4—N4 | −5.3 (17) | N11—Rh2—N15—C22 | −168.6 (5) |
N3—C4—N4—C5 | −1.1 (11) | N19—Rh2—N15—C22 | −80.8 (5) |
C1—C4—N4—C5 | −177.7 (9) | Rh1—Rh2—N15—C22 | 98.5 (5) |
C4—N4—C5—C6 | 0.4 (12) | N13—Rh2—N15—C24 | −178.8 (8) |
N4—C5—C6—N3 | 0.4 (11) | N9—Rh2—N15—C24 | 99 (3) |
C4—N3—C6—C5 | −1.1 (10) | N11—Rh2—N15—C24 | 5.7 (8) |
Rh1—N3—C6—C5 | −178.1 (7) | N19—Rh2—N15—C24 | 93.5 (8) |
N7—Rh1—N5—C7 | 5.5 (5) | Rh1—Rh2—N15—C24 | −87.2 (8) |
N3—Rh1—N5—C7 | −69 (5) | C24—N15—C22—N16 | 0.5 (9) |
N1—Rh1—N5—C7 | −169.9 (5) | Rh2—N15—C22—N16 | 176.7 (5) |
N17—Rh1—N5—C7 | −83.9 (5) | C24—N15—C22—C19 | −179.5 (7) |
Rh2—Rh1—N5—C7 | 97.5 (5) | Rh2—N15—C22—C19 | −3.2 (8) |
N7—Rh1—N5—C9 | −178.9 (8) | N13—C19—C22—N15 | −5.3 (11) |
N3—Rh1—N5—C9 | 106 (5) | N14—C19—C22—N15 | 176.5 (9) |
N1—Rh1—N5—C9 | 5.7 (8) | N13—C19—C22—N16 | 174.8 (8) |
N17—Rh1—N5—C9 | 91.7 (8) | N14—C19—C22—N16 | −3.5 (16) |
Rh2—Rh1—N5—C9 | −86.9 (8) | N15—C22—N16—C23 | −1.3 (10) |
C9—N5—C7—N6 | −0.4 (9) | C19—C22—N16—C23 | 178.7 (9) |
Rh1—N5—C7—N6 | 176.7 (5) | C22—N16—C23—C24 | 1.5 (10) |
C9—N5—C7—C10 | 179.9 (7) | N16—C23—C24—N15 | −1.3 (10) |
Rh1—N5—C7—C10 | −3.1 (8) | C22—N15—C24—C23 | 0.5 (9) |
N5—C7—N6—C8 | 1.4 (9) | Rh2—N15—C24—C23 | −174.1 (6) |
C10—C7—N6—C8 | −179.0 (8) | N7—Rh1—N17—C28 | −137.8 (7) |
C7—N6—C8—C9 | −1.8 (10) | N5—Rh1—N17—C28 | −58.1 (7) |
N6—C8—C9—N5 | 1.6 (10) | N3—Rh1—N17—C28 | 122.7 (7) |
C7—N5—C9—C8 | −0.8 (9) | N1—Rh1—N17—C28 | 43.9 (7) |
Rh1—N5—C9—C8 | −176.5 (6) | Rh2—Rh1—N17—C28 | −34 (3) |
N5—Rh1—N7—C10 | −7.5 (5) | N7—Rh1—N17—C25 | 40.6 (7) |
N3—Rh1—N7—C10 | 169.5 (5) | N5—Rh1—N17—C25 | 120.3 (7) |
N1—Rh1—N7—C10 | 99 (3) | N3—Rh1—N17—C25 | −58.9 (7) |
N17—Rh1—N7—C10 | 78.6 (5) | N1—Rh1—N17—C25 | −137.8 (7) |
Rh2—Rh1—N7—C10 | −98.1 (5) | Rh2—Rh1—N17—C25 | 145 (3) |
N5—Rh1—N7—C12 | −175.2 (9) | C28—N17—C25—C26 | 0.0 (14) |
N3—Rh1—N7—C12 | 1.8 (9) | Rh1—N17—C25—C26 | −178.4 (8) |
N1—Rh1—N7—C12 | −69 (4) | N17—C25—C26—N18 | 0.8 (18) |
N17—Rh1—N7—C12 | −89.1 (8) | C25—C26—N18—C27 | −1.0 (18) |
Rh2—Rh1—N7—C12 | 94.2 (8) | C26—N18—C27—C28 | 0.4 (16) |
C12—N7—C10—N8 | −2.0 (9) | C25—N17—C28—C27 | −0.6 (14) |
Rh1—N7—C10—N8 | −173.7 (5) | Rh1—N17—C28—C27 | 177.9 (7) |
C12—N7—C10—C7 | 179.8 (7) | N18—C27—C28—N17 | 0.4 (16) |
Rh1—N7—C10—C7 | 8.1 (8) | N13—Rh2—N19—C30 | 45.7 (6) |
N5—C7—C10—N7 | −3.3 (10) | N9—Rh2—N19—C30 | −54.0 (6) |
N6—C7—C10—N7 | 177.0 (8) | N11—Rh2—N19—C30 | −133.6 (6) |
N5—C7—C10—N8 | 178.9 (8) | N15—Rh2—N19—C30 | 125.5 (6) |
N6—C7—C10—N8 | −0.7 (16) | Rh1—Rh2—N19—C30 | 61 (11) |
N7—C10—N8—C11 | 3.1 (10) | N13—Rh2—N19—C29 | −135.4 (6) |
C7—C10—N8—C11 | −179.1 (8) | N9—Rh2—N19—C29 | 124.9 (6) |
C10—N8—C11—C12 | −2.9 (10) | N11—Rh2—N19—C29 | 45.3 (6) |
N8—C11—C12—N7 | 1.7 (10) | N15—Rh2—N19—C29 | −55.6 (6) |
C10—N7—C12—C11 | 0.1 (10) | Rh1—Rh2—N19—C29 | −120 (11) |
Rh1—N7—C12—C11 | 168.4 (7) | C30—N19—C29—C30i | −0.4 (12) |
N13—Rh2—N9—C13 | −169.7 (5) | Rh2—N19—C29—C30i | −179.4 (6) |
N11—Rh2—N9—C13 | 5.9 (5) | C29—N19—C30—C29i | 0.4 (12) |
N15—Rh2—N9—C13 | −89 (3) | Rh2—N19—C30—C29i | 179.4 (6) |
N19—Rh2—N9—C13 | −82.8 (5) | | |
Symmetry code: (i) −x+1, −y+1, −z+1. |
Hydrogen-bond geometry (Å, º) top
D—H···A | D—H | H···A | D···A | D—H···A |
N2—H2N···O14ii | 0.86 | 2.08 | 2.872 (13) | 154 |
N4—H4N···O5W | 0.86 | 2.08 | 2.75 (4) | 135 |
N4—H4N···O14ii | 0.86 | 2.55 | 3.273 (16) | 142 |
N6—H6N···O15 | 0.86 | 2.33 | 3.075 (14) | 145 |
N6—H6N···O13iii | 0.86 | 2.62 | 3.233 (14) | 129 |
N8—H8N···O15 | 0.86 | 2.13 | 2.915 (15) | 151 |
N8—H8N···Cl4 | 0.86 | 2.92 | 3.782 (9) | 178 |
N10—H10N···O3W | 0.86 | 2.00 | 2.824 (11) | 161 |
N10—H10N···O10 | 0.86 | 2.59 | 3.077 (11) | 117 |
N12—H12N···O8 | 0.86 | 2.27 | 3.062 (12) | 154 |
N12—H12N···O10 | 0.86 | 2.41 | 2.945 (11) | 121 |
N14—H14N···O11i | 0.86 | 2.41 | 3.001 (12) | 126 |
N14—H14N···O2 | 0.86 | 2.53 | 3.049 (14) | 120 |
N16—H16N···O4W | 0.86 | 2.09 | 2.910 (13) | 160 |
N16—H16N···O11i | 0.86 | 2.65 | 3.167 (12) | 120 |
Symmetry codes: (i) −x+1, −y+1, −z+1; (ii) −x+1/2, y+1/2, z; (iii) −x, −y+1, −z+1. |
Crystal data top
C28H28F12N18Rh2·2(SiF6)·6(H2O) | F(000) = 2432 |
Mr = 1214.78 | Dx = 1.887 Mg m−3 |
Monoclinic, C2/c | Mo Kα radiation, λ = 0.71069 Å |
a = 27.057 (5) Å | Cell parameters from 6156 reflections |
b = 9.9832 (15) Å | θ = 3.0–27.5° |
c = 18.718 (3) Å | µ = 0.95 mm−1 |
β = 122.2560 (19)° | T = 296 K |
V = 4275.6 (13) Å3 | Prismatic, red |
Z = 4 | 0.59 × 0.39 × 0.21 mm |
Data collection top
Rigaku/MSC Mercury CCD diffractometer | 4873 independent reflections |
Radiation source: rotating-anode X-ray tube | 4409 reflections with I > 2σ(I) |
Graphite monochromator | Rint = 0.025 |
Detector resolution: 14.62 pixels mm-1 | θmax = 27.5°, θmin = 3.8° |
ω scans | h = −34→21 |
Absorption correction: numerical NUMABS (Higashi, 1999) | k = −12→10 |
Tmin = 0.747, Tmax = 0.867 | l = −20→24 |
16660 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)] = 0.048 | Hydrogen site location: inferred from neighbouring sites |
wR(F2) = 0.136 | H atoms treated by a mixture of independent and constrained refinement |
S = 1.09 | w = 1/[σ2(Fo2) + (0.0767P)2 + 22.3201P] where P = (Fo2 + 2Fc2)/3 |
4873 reflections | (Δ/σ)max < 0.001 |
309 parameters | Δρmax = 1.37 e Å−3 |
0 restraints | Δρmin = −1.21 e Å−3 |
Crystal data top
C28H28F12N18Rh2·2(SiF6)·6(H2O) | V = 4275.6 (13) Å3 |
Mr = 1214.78 | Z = 4 |
Monoclinic, C2/c | Mo Kα radiation |
a = 27.057 (5) Å | µ = 0.95 mm−1 |
b = 9.9832 (15) Å | T = 296 K |
c = 18.718 (3) Å | 0.59 × 0.39 × 0.21 mm |
β = 122.2560 (19)° | |
Data collection top
Rigaku/MSC Mercury CCD diffractometer | 4873 independent reflections |
Absorption correction: numerical NUMABS (Higashi, 1999) | 4409 reflections with I > 2σ(I) |
Tmin = 0.747, Tmax = 0.867 | Rint = 0.025 |
16660 measured reflections | |
Refinement top
R[F2 > 2σ(F2)] = 0.048 | 0 restraints |
wR(F2) = 0.136 | H atoms treated by a mixture of independent and constrained refinement |
S = 1.09 | w = 1/[σ2(Fo2) + (0.0767P)2 + 22.3201P] where P = (Fo2 + 2Fc2)/3 |
4873 reflections | Δρmax = 1.37 e Å−3 |
309 parameters | Δρmin = −1.21 e Å−3 |
Special details top
Geometry. All e.s.d.'s (except the e.s.d. in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell e.s.d.'s are taken into account individually in the estimation of e.s.d.'s in distances, angles and torsion angles; correlations between e.s.d.'s in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell e.s.d.'s is used for estimating e.s.d.'s involving l.s. planes. |
Refinement. Refinement of F2 against ALL reflections. The weighted R-factor wR and goodness of fit S are based on F2, conventional R-factors R are based on F, with F set to zero for negative F2. The threshold expression of F2 > σ(F2) is used only for calculating R-factors(gt) etc. and is not relevant to the choice of reflections for refinement. R-factors based on F2 are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger. |
Fractional atomic coordinates and isotropic or equivalent isotropic displacement parameters (Å2) top | x | y | z | Uiso*/Ueq | |
Rh1 | 0.5000 | 0.48681 (4) | 0.2500 | 0.02135 (13) | |
Rh2 | 0.5000 | 0.21732 (4) | 0.2500 | 0.02278 (13) | |
N1 | 0.55449 (15) | 0.4974 (3) | 0.2053 (2) | 0.0289 (7) | |
C1 | 0.61052 (18) | 0.5151 (4) | 0.2656 (3) | 0.0316 (8) | |
N2 | 0.64316 (19) | 0.5329 (5) | 0.2329 (3) | 0.0517 (11) | |
H2N | 0.6803 | 0.5453 | 0.2606 | 0.062* | |
C2 | 0.6067 (3) | 0.5277 (8) | 0.1471 (4) | 0.0673 (18) | |
H2 | 0.6173 | 0.5369 | 0.1076 | 0.081* | |
C3 | 0.5518 (2) | 0.5066 (5) | 0.1305 (3) | 0.0464 (12) | |
H3 | 0.5181 | 0.4995 | 0.0770 | 0.056* | |
N3 | 0.58000 (14) | 0.4915 (3) | 0.3611 (2) | 0.0264 (6) | |
C4 | 0.62451 (18) | 0.5126 (4) | 0.3513 (3) | 0.0299 (8) | |
N4 | 0.67424 (16) | 0.5295 (4) | 0.4261 (2) | 0.0421 (9) | |
H4N | 0.7081 | 0.5452 | 0.4342 | 0.051* | |
C5 | 0.6616 (2) | 0.5175 (5) | 0.4866 (3) | 0.0484 (12) | |
H5 | 0.6879 | 0.5234 | 0.5447 | 0.058* | |
C6 | 0.6035 (2) | 0.4951 (4) | 0.4465 (3) | 0.0365 (9) | |
H6 | 0.5827 | 0.4839 | 0.4727 | 0.044* | |
N5 | 0.49934 (15) | 0.2108 (3) | 0.1393 (2) | 0.0292 (7) | |
C7 | 0.55188 (19) | 0.1931 (4) | 0.1512 (3) | 0.0344 (9) | |
N6 | 0.54808 (19) | 0.1764 (5) | 0.0777 (3) | 0.0460 (9) | |
H6N | 0.5769 | 0.1639 | 0.0712 | 0.055* | |
C8 | 0.4904 (2) | 0.1825 (6) | 0.0147 (3) | 0.0472 (11) | |
H8 | 0.4747 | 0.1743 | −0.0430 | 0.057* | |
C9 | 0.4605 (2) | 0.2030 (4) | 0.0536 (3) | 0.0369 (9) | |
H9 | 0.4201 | 0.2106 | 0.0263 | 0.044* | |
N7 | 0.58799 (14) | 0.2093 (3) | 0.2966 (2) | 0.0289 (7) | |
C10 | 0.60043 (18) | 0.1946 (4) | 0.2374 (3) | 0.0345 (9) | |
N8 | 0.65797 (17) | 0.1829 (5) | 0.2720 (3) | 0.0481 (10) | |
H8N | 0.6756 | 0.1733 | 0.2453 | 0.058* | |
C11 | 0.6838 (2) | 0.1889 (6) | 0.3576 (4) | 0.0525 (13) | |
H11 | 0.7236 | 0.1836 | 0.3980 | 0.063* | |
C12 | 0.64002 (19) | 0.2042 (4) | 0.3727 (3) | 0.0383 (9) | |
H12 | 0.6447 | 0.2102 | 0.4256 | 0.046* | |
N9 | 0.5000 | 0.7202 (4) | 0.2500 | 0.0237 (9) | |
C13 | 0.53399 (19) | 0.7867 (4) | 0.3200 (3) | 0.0326 (9) | |
H13 | 0.5580 | 0.7402 | 0.3700 | 0.039* | |
C14 | 0.53457 (19) | 0.9261 (4) | 0.3204 (3) | 0.0349 (9) | |
H14 | 0.5594 | 0.9718 | 0.3704 | 0.042* | |
N10 | 0.5000 | 0.9941 (4) | 0.2500 | 0.0277 (9) | |
Si1 | 0.81273 (6) | 0.5852 (2) | 0.41399 (10) | 0.0581 (4) | |
F1 | 0.8146 (7) | 0.7193 (11) | 0.3712 (7) | 0.279 (7) | |
F2 | 0.8735 (4) | 0.6493 (11) | 0.4859 (6) | 0.210 (5) | |
F3 | 0.8438 (4) | 0.5230 (10) | 0.3688 (7) | 0.214 (5) | |
F4 | 0.7547 (3) | 0.5092 (10) | 0.3475 (7) | 0.226 (6) | |
F5 | 0.7766 (5) | 0.6599 (9) | 0.4453 (10) | 0.253 (7) | |
F6 | 0.8270 (8) | 0.4585 (14) | 0.4673 (8) | 0.313 (8) | |
O1 | 0.5947 (3) | 0.8697 (6) | 0.1915 (4) | 0.0985 (18) | |
O2 | 0.6770 (4) | 0.8445 (8) | 0.3646 (5) | 0.138 (3) | |
O3 | 0.7085 (5) | 0.7199 (9) | 0.1683 (10) | 0.198 (5) | |
Atomic displacement parameters (Å2) top | U11 | U22 | U33 | U12 | U13 | U23 |
Rh1 | 0.0230 (2) | 0.01753 (19) | 0.0232 (2) | 0.000 | 0.01210 (17) | 0.000 |
Rh2 | 0.0231 (2) | 0.0165 (2) | 0.0283 (2) | 0.000 | 0.01339 (17) | 0.000 |
N1 | 0.0305 (17) | 0.0294 (16) | 0.0290 (17) | −0.0016 (12) | 0.0174 (15) | −0.0001 (12) |
C1 | 0.0285 (19) | 0.032 (2) | 0.038 (2) | −0.0027 (15) | 0.0203 (18) | 0.0011 (16) |
N2 | 0.038 (2) | 0.081 (3) | 0.046 (2) | −0.013 (2) | 0.029 (2) | −0.006 (2) |
C2 | 0.059 (3) | 0.114 (5) | 0.045 (3) | −0.023 (3) | 0.039 (3) | −0.008 (3) |
C3 | 0.047 (3) | 0.066 (3) | 0.031 (2) | −0.011 (2) | 0.024 (2) | −0.005 (2) |
N3 | 0.0275 (16) | 0.0229 (15) | 0.0263 (16) | −0.0010 (11) | 0.0127 (13) | 0.0002 (11) |
C4 | 0.0264 (18) | 0.0290 (19) | 0.031 (2) | −0.0034 (14) | 0.0132 (16) | −0.0007 (14) |
N4 | 0.0259 (17) | 0.055 (2) | 0.036 (2) | −0.0086 (16) | 0.0103 (16) | −0.0017 (17) |
C5 | 0.042 (3) | 0.058 (3) | 0.031 (2) | −0.009 (2) | 0.010 (2) | −0.001 (2) |
C6 | 0.038 (2) | 0.042 (2) | 0.028 (2) | −0.0036 (17) | 0.0166 (18) | 0.0011 (16) |
N5 | 0.0313 (17) | 0.0236 (15) | 0.0330 (17) | 0.0009 (12) | 0.0174 (15) | −0.0016 (12) |
C7 | 0.036 (2) | 0.032 (2) | 0.040 (2) | 0.0041 (17) | 0.0234 (19) | −0.0026 (17) |
N6 | 0.046 (2) | 0.058 (2) | 0.044 (2) | 0.0068 (19) | 0.031 (2) | −0.0056 (19) |
C8 | 0.051 (3) | 0.057 (3) | 0.035 (2) | 0.005 (2) | 0.024 (2) | −0.004 (2) |
C9 | 0.038 (2) | 0.036 (2) | 0.034 (2) | 0.0031 (17) | 0.0169 (19) | −0.0016 (16) |
N7 | 0.0267 (16) | 0.0215 (15) | 0.0377 (18) | 0.0013 (11) | 0.0166 (15) | −0.0002 (12) |
C10 | 0.0277 (19) | 0.032 (2) | 0.045 (2) | 0.0039 (16) | 0.0201 (18) | −0.0016 (17) |
N8 | 0.0290 (19) | 0.060 (2) | 0.057 (3) | 0.0052 (18) | 0.0243 (19) | −0.006 (2) |
C11 | 0.027 (2) | 0.060 (3) | 0.056 (3) | 0.009 (2) | 0.013 (2) | −0.002 (3) |
C12 | 0.030 (2) | 0.037 (2) | 0.039 (2) | 0.0032 (16) | 0.0119 (18) | 0.0007 (17) |
N9 | 0.026 (2) | 0.022 (2) | 0.023 (2) | 0.000 | 0.0129 (18) | 0.000 |
C13 | 0.040 (2) | 0.0222 (19) | 0.0237 (19) | 0.0040 (15) | 0.0086 (17) | 0.0028 (13) |
C14 | 0.038 (2) | 0.0219 (19) | 0.031 (2) | 0.0025 (15) | 0.0092 (17) | −0.0006 (15) |
N10 | 0.025 (2) | 0.027 (2) | 0.028 (2) | 0.000 | 0.0115 (19) | 0.000 |
Si1 | 0.0305 (7) | 0.0998 (14) | 0.0438 (8) | −0.0039 (7) | 0.0197 (6) | 0.0054 (8) |
F1 | 0.49 (2) | 0.151 (9) | 0.217 (12) | −0.006 (11) | 0.207 (14) | 0.057 (8) |
F2 | 0.115 (6) | 0.308 (14) | 0.129 (6) | −0.012 (6) | 0.012 (5) | −0.095 (7) |
F3 | 0.197 (8) | 0.295 (11) | 0.265 (10) | −0.140 (8) | 0.201 (8) | −0.178 (9) |
F4 | 0.063 (4) | 0.219 (9) | 0.288 (12) | −0.032 (4) | 0.021 (5) | −0.121 (8) |
F5 | 0.226 (10) | 0.194 (9) | 0.50 (2) | −0.052 (7) | 0.306 (13) | −0.127 (10) |
F6 | 0.46 (2) | 0.270 (14) | 0.240 (13) | 0.083 (14) | 0.208 (15) | 0.175 (11) |
O1 | 0.092 (4) | 0.099 (4) | 0.100 (5) | −0.008 (3) | 0.048 (4) | −0.008 (3) |
O2 | 0.170 (8) | 0.126 (7) | 0.115 (6) | 0.047 (5) | 0.075 (6) | 0.036 (4) |
O3 | 0.203 (10) | 0.126 (7) | 0.370 (17) | −0.035 (7) | 0.222 (12) | −0.012 (9) |
Geometric parameters (Å, º) top
Rh1—N1 | 2.049 (3) | C7—N6 | 1.334 (6) |
Rh1—N1i | 2.049 (3) | C7—C10 | 1.437 (6) |
Rh1—N3 | 2.051 (3) | N6—C8 | 1.366 (7) |
Rh1—N3i | 2.051 (3) | N6—H6N | 0.8600 |
Rh1—N9 | 2.330 (4) | C8—C9 | 1.362 (7) |
Rh1—Rh2 | 2.6904 (7) | C8—H8 | 0.9300 |
Rh2—N7i | 2.054 (3) | C9—H9 | 0.9300 |
Rh2—N7 | 2.054 (3) | N7—C10 | 1.328 (6) |
Rh2—N5i | 2.063 (3) | N7—C12 | 1.368 (6) |
Rh2—N5 | 2.063 (3) | C10—N8 | 1.334 (6) |
Rh2—N10ii | 2.228 (5) | N8—C11 | 1.365 (7) |
N1—C1 | 1.333 (6) | N8—H8N | 0.8600 |
N1—C3 | 1.367 (6) | C11—C12 | 1.364 (7) |
C1—N2 | 1.329 (6) | C11—H11 | 0.9300 |
C1—C4 | 1.438 (6) | C12—H12 | 0.9300 |
N2—C2 | 1.365 (7) | N9—C13i | 1.310 (4) |
N2—H2N | 0.8600 | N9—C13 | 1.310 (4) |
C2—C3 | 1.361 (8) | C13—C14 | 1.391 (6) |
C2—H2 | 0.9300 | C13—H13 | 0.9300 |
C3—H3 | 0.9300 | C14—N10 | 1.325 (5) |
N3—C4 | 1.328 (5) | C14—H14 | 0.9300 |
N3—C6 | 1.369 (5) | N10—C14i | 1.325 (5) |
C4—N4 | 1.337 (6) | N10—Rh2iii | 2.228 (4) |
N4—C5 | 1.352 (7) | Si1—F6 | 1.528 (9) |
N4—H4N | 0.8600 | Si1—F5 | 1.570 (6) |
C5—C6 | 1.352 (7) | Si1—F1 | 1.575 (9) |
C5—H5 | 0.9300 | Si1—F4 | 1.582 (6) |
C6—H6 | 0.9300 | Si1—F2 | 1.601 (8) |
N5—C7 | 1.328 (5) | Si1—F3 | 1.602 (6) |
N5—C9 | 1.374 (6) | | |
| | | |
O1···O2 | 2.797 (10) | O3···F4iv | 3.120 (14) |
O1···F3iv | 2.895 (15) | O3···F6iv | 3.23 (1) |
O2···F5 | 2.931 (13) | O3···F3iv | 3.254 (14) |
O2···F5v | 3.08 (1) | | |
| | | |
N1—Rh1—N1i | 174.10 (18) | N3—C6—H6 | 125.3 |
N1—Rh1—N3 | 79.22 (14) | C7—N5—C9 | 105.8 (4) |
N1i—Rh1—N3 | 100.64 (14) | C7—N5—Rh2 | 113.7 (3) |
N1—Rh1—N3i | 100.64 (14) | C9—N5—Rh2 | 140.0 (3) |
N1i—Rh1—N3i | 79.22 (14) | N5—C7—N6 | 111.0 (4) |
N3—Rh1—N3i | 177.39 (17) | N5—C7—C10 | 116.2 (4) |
N1—Rh1—N9 | 87.05 (9) | N6—C7—C10 | 132.8 (4) |
N1i—Rh1—N9 | 87.05 (9) | C7—N6—C8 | 108.0 (4) |
N3—Rh1—N9 | 88.70 (8) | C7—N6—H6N | 126.0 |
N3i—Rh1—N9 | 88.70 (8) | C8—N6—H6N | 126.0 |
N1—Rh1—Rh2 | 92.95 (9) | C9—C8—N6 | 106.1 (4) |
N1i—Rh1—Rh2 | 92.95 (9) | C9—C8—H8 | 127.0 |
N3—Rh1—Rh2 | 91.30 (8) | N6—C8—H8 | 127.0 |
N3i—Rh1—Rh2 | 91.30 (8) | C8—C9—N5 | 109.3 (4) |
N9—Rh1—Rh2 | 180.000 (1) | C8—C9—H9 | 125.4 |
N7i—Rh2—N7 | 175.53 (17) | N5—C9—H9 | 125.4 |
N7i—Rh2—N5i | 79.18 (14) | C10—N7—C12 | 106.6 (4) |
N7—Rh2—N5i | 100.67 (14) | C10—N7—Rh2 | 113.7 (3) |
N7i—Rh2—N5 | 100.67 (14) | C12—N7—Rh2 | 139.4 (3) |
N7—Rh2—N5 | 79.18 (14) | N7—C10—N8 | 110.7 (4) |
N5i—Rh2—N5 | 176.37 (17) | N7—C10—C7 | 116.8 (4) |
N7i—Rh2—N10ii | 87.77 (8) | N8—C10—C7 | 132.5 (4) |
N7—Rh2—N10ii | 87.77 (8) | C10—N8—C11 | 107.5 (4) |
N5i—Rh2—N10ii | 88.18 (9) | C10—N8—H8N | 126.3 |
N5—Rh2—N10ii | 88.19 (9) | C11—N8—H8N | 126.3 |
N7i—Rh2—Rh1 | 92.23 (8) | C12—C11—N8 | 106.9 (4) |
N7—Rh2—Rh1 | 92.23 (8) | C12—C11—H11 | 126.6 |
N5i—Rh2—Rh1 | 91.81 (9) | N8—C11—H11 | 126.6 |
N5—Rh2—Rh1 | 91.81 (9) | C11—C12—N7 | 108.3 (4) |
N10ii—Rh2—Rh1 | 180.0 | C11—C12—H12 | 125.9 |
C1—N1—C3 | 105.8 (4) | N7—C12—H12 | 125.9 |
C1—N1—Rh1 | 113.7 (3) | C13i—N9—C13 | 119.1 (4) |
C3—N1—Rh1 | 140.0 (3) | C13i—N9—Rh1 | 120.5 (2) |
N2—C1—N1 | 111.3 (4) | C13—N9—Rh1 | 120.5 (2) |
N2—C1—C4 | 132.3 (4) | N9—C13—C14 | 120.8 (4) |
N1—C1—C4 | 116.5 (4) | N9—C13—H13 | 119.6 |
C1—N2—C2 | 107.3 (4) | C14—C13—H13 | 119.6 |
C1—N2—H2N | 126.4 | N10—C14—C13 | 120.5 (4) |
C2—N2—H2N | 126.4 | N10—C14—H14 | 119.8 |
C3—C2—N2 | 106.9 (4) | C13—C14—H14 | 119.8 |
C3—C2—H2 | 126.6 | C14i—N10—C14 | 118.3 (5) |
N2—C2—H2 | 126.6 | C14i—N10—Rh2iii | 120.8 (2) |
C2—C3—N1 | 108.8 (5) | C14—N10—Rh2iii | 120.8 (2) |
C2—C3—H3 | 125.6 | F6—Si1—F5 | 98.0 (7) |
N1—C3—H3 | 125.6 | F6—Si1—F1 | 166.1 (9) |
C4—N3—C6 | 105.5 (3) | F5—Si1—F1 | 89.0 (7) |
C4—N3—Rh1 | 114.0 (3) | F6—Si1—F4 | 85.2 (8) |
C6—N3—Rh1 | 140.0 (3) | F5—Si1—F4 | 88.1 (5) |
N3—C4—N4 | 110.8 (4) | F1—Si1—F4 | 107.2 (7) |
N3—C4—C1 | 116.0 (4) | F6—Si1—F2 | 89.6 (8) |
N4—C4—C1 | 133.2 (4) | F5—Si1—F2 | 93.5 (5) |
C4—N4—C5 | 107.6 (4) | F1—Si1—F2 | 77.9 (7) |
C4—N4—H4N | 126.2 | F4—Si1—F2 | 174.7 (6) |
C5—N4—H4N | 126.2 | F6—Si1—F3 | 90.2 (7) |
C6—C5—N4 | 106.8 (4) | F5—Si1—F3 | 170.9 (7) |
C6—C5—H5 | 126.6 | F1—Si1—F3 | 83.8 (6) |
N4—C5—H5 | 126.6 | F4—Si1—F3 | 88.8 (5) |
C5—C6—N3 | 109.3 (4) | F2—Si1—F3 | 90.3 (5) |
C5—C6—H6 | 125.3 | | |
| | | |
N1—Rh1—Rh2—N7i | −138.71 (14) | C1—C4—N4—C5 | 179.5 (5) |
N1i—Rh1—Rh2—N7i | 41.29 (14) | C4—N4—C5—C6 | −0.9 (6) |
N3—Rh1—Rh2—N7i | 142.02 (14) | N4—C5—C6—N3 | 0.8 (6) |
N3i—Rh1—Rh2—N7i | −37.98 (14) | C4—N3—C6—C5 | −0.4 (5) |
N9—Rh1—Rh2—N7i | −159 (100) | Rh1—N3—C6—C5 | −170.7 (3) |
N1—Rh1—Rh2—N7 | 41.29 (14) | N7i—Rh2—N5—C7 | −169.9 (3) |
N1i—Rh1—Rh2—N7 | −138.71 (14) | N7—Rh2—N5—C7 | 5.6 (3) |
N3—Rh1—Rh2—N7 | −37.98 (14) | N5i—Rh2—N5—C7 | −82.5 (3) |
N3i—Rh1—Rh2—N7 | 142.02 (14) | N10ii—Rh2—N5—C7 | −82.5 (3) |
N9—Rh1—Rh2—N7 | 21 (100) | Rh1—Rh2—N5—C7 | 97.5 (3) |
N1—Rh1—Rh2—N5i | 142.05 (14) | N7i—Rh2—N5—C9 | −0.2 (4) |
N1i—Rh1—Rh2—N5i | −37.95 (14) | N7—Rh2—N5—C9 | 175.2 (4) |
N3—Rh1—Rh2—N5i | 62.78 (13) | N5i—Rh2—N5—C9 | 87.1 (4) |
N3i—Rh1—Rh2—N5i | −117.22 (13) | N10ii—Rh2—N5—C9 | 87.1 (4) |
N9—Rh1—Rh2—N5i | 122 (100) | Rh1—Rh2—N5—C9 | −92.9 (4) |
N1—Rh1—Rh2—N5 | −37.95 (14) | C9—N5—C7—N6 | 0.7 (5) |
N1i—Rh1—Rh2—N5 | 142.05 (14) | Rh2—N5—C7—N6 | 173.8 (3) |
N3—Rh1—Rh2—N5 | −117.22 (13) | C9—N5—C7—C10 | −178.9 (4) |
N3i—Rh1—Rh2—N5 | 62.78 (13) | Rh2—N5—C7—C10 | −5.8 (5) |
N9—Rh1—Rh2—N5 | −58 (100) | N5—C7—N6—C8 | −0.4 (6) |
N1—Rh1—Rh2—N10ii | 153 (16) | C10—C7—N6—C8 | 179.1 (5) |
N1i—Rh1—Rh2—N10ii | −27 (16) | C7—N6—C8—C9 | −0.1 (6) |
N3—Rh1—Rh2—N10ii | 74 (16) | N6—C8—C9—N5 | 0.6 (6) |
N3i—Rh1—Rh2—N10ii | −106 (16) | C7—N5—C9—C8 | −0.8 (5) |
N9—Rh1—Rh2—N10ii | 133 (100) | Rh2—N5—C9—C8 | −170.9 (4) |
N1i—Rh1—N1—C1 | 83.0 (3) | N7i—Rh2—N7—C10 | 84.1 (3) |
N3—Rh1—N1—C1 | −6.3 (3) | N5i—Rh2—N7—C10 | 171.8 (3) |
N3i—Rh1—N1—C1 | 171.1 (3) | N5—Rh2—N7—C10 | −4.5 (3) |
N9—Rh1—N1—C1 | 83.0 (3) | N10ii—Rh2—N7—C10 | 84.1 (3) |
Rh2—Rh1—N1—C1 | −97.0 (3) | Rh1—Rh2—N7—C10 | −95.9 (3) |
N1i—Rh1—N1—C3 | −87.5 (5) | N7i—Rh2—N7—C12 | −89.4 (4) |
N3—Rh1—N1—C3 | −176.8 (5) | N5i—Rh2—N7—C12 | −1.6 (4) |
N3i—Rh1—N1—C3 | 0.6 (5) | N5—Rh2—N7—C12 | −177.9 (4) |
N9—Rh1—N1—C3 | −87.5 (5) | N10ii—Rh2—N7—C12 | −89.3 (4) |
Rh2—Rh1—N1—C3 | 92.5 (5) | Rh1—Rh2—N7—C12 | 90.6 (4) |
C3—N1—C1—N2 | −0.9 (5) | C12—N7—C10—N8 | −1.1 (5) |
Rh1—N1—C1—N2 | −174.6 (3) | Rh2—N7—C10—N8 | −176.7 (3) |
C3—N1—C1—C4 | 178.7 (4) | C12—N7—C10—C7 | 178.4 (4) |
Rh1—N1—C1—C4 | 5.0 (4) | Rh2—N7—C10—C7 | 2.9 (5) |
N1—C1—N2—C2 | 0.6 (6) | N5—C7—C10—N7 | 2.0 (6) |
C4—C1—N2—C2 | −179.0 (5) | N6—C7—C10—N7 | −177.5 (5) |
C1—N2—C2—C3 | 0.0 (7) | N5—C7—C10—N8 | −178.6 (5) |
N2—C2—C3—N1 | −0.6 (7) | N6—C7—C10—N8 | 1.9 (9) |
C1—N1—C3—C2 | 0.9 (6) | N7—C10—N8—C11 | 0.6 (6) |
Rh1—N1—C3—C2 | 171.9 (4) | C7—C10—N8—C11 | −178.8 (5) |
N1—Rh1—N3—C4 | 6.7 (3) | C10—N8—C11—C12 | 0.1 (6) |
N1i—Rh1—N3—C4 | −167.3 (3) | N8—C11—C12—N7 | −0.8 (6) |
N3i—Rh1—N3—C4 | −80.6 (3) | C10—N7—C12—C11 | 1.2 (5) |
N9—Rh1—N3—C4 | −80.6 (3) | Rh2—N7—C12—C11 | 174.9 (4) |
Rh2—Rh1—N3—C4 | 99.4 (3) | N1—Rh1—N9—C13i | 81.1 (3) |
N1—Rh1—N3—C6 | 176.5 (4) | N1i—Rh1—N9—C13i | −98.9 (3) |
N1i—Rh1—N3—C6 | 2.5 (4) | N3—Rh1—N9—C13i | 160.3 (3) |
N3i—Rh1—N3—C6 | 89.2 (4) | N3i—Rh1—N9—C13i | −19.7 (3) |
N9—Rh1—N3—C6 | 89.2 (4) | Rh2—Rh1—N9—C13i | 101 (100) |
Rh2—Rh1—N3—C6 | −90.8 (4) | N1—Rh1—N9—C13 | −98.9 (3) |
C6—N3—C4—N4 | −0.2 (5) | N1i—Rh1—N9—C13 | 81.1 (3) |
Rh1—N3—C4—N4 | 173.0 (3) | N3—Rh1—N9—C13 | −19.7 (3) |
C6—N3—C4—C1 | −179.3 (3) | N3i—Rh1—N9—C13 | 160.3 (3) |
Rh1—N3—C4—C1 | −6.1 (4) | Rh2—Rh1—N9—C13 | −79 (100) |
N2—C1—C4—N3 | −179.8 (5) | C13i—N9—C13—C14 | −0.5 (3) |
N1—C1—C4—N3 | 0.7 (5) | Rh1—N9—C13—C14 | 179.5 (3) |
N2—C1—C4—N4 | 1.4 (9) | N9—C13—C14—N10 | 1.0 (6) |
N1—C1—C4—N4 | −178.1 (4) | C13—C14—N10—C14i | −0.5 (3) |
N3—C4—N4—C5 | 0.7 (5) | C13—C14—N10—Rh2iii | 179.5 (3) |
Symmetry codes: (i) −x+1, y, −z+1/2; (ii) x, y−1, z; (iii) x, y+1, z; (iv) −x+3/2, y+1/2, −z+1/2; (v) −x+3/2, −y+3/2, −z+1. |
Hydrogen-bond geometry (Å, º) top
D—H···A | D—H | H···A | D···A | D—H···A |
N2—H2N···F4 | 0.86 | 1.83 | 2.619 (9) | 153 |
N4—H4N···F5 | 0.86 | 2.09 | 2.903 (8) | 157 |
N4—H4N···F4 | 0.86 | 2.56 | 3.219 (12) | 135 |
N6—H6N···F2vi | 0.86 | 2.12 | 2.948 (12) | 161 |
N6—H6N···F3vi | 0.86 | 2.30 | 2.963 (8) | 134 |
N6—H6N···F1vi | 0.86 | 2.59 | 3.332 (17) | 145 |
N8—H8N···F1vi | 0.86 | 2.38 | 3.161 (13) | 152 |
N8—H8N···F3vi | 0.86 | 2.43 | 3.060 (12) | 131 |
Symmetry code: (vi) −x+3/2, y−1/2, −z+1/2. |
Experimental details
| (I) | (II) | (III) | (IV) |
Crystal data |
Chemical formula | C24H28N16O2Rh2·4(NO3)·4(H2O) | C24H28N16O2Rh2·4(ClO4)·5(H2O) | C26H32N16O2Rh2·4(ClO4) | C30H38N18O2Rh2·4(BF4) |
Mr | 1098.55 | 1266.32 | 1204.30 | 1235.84 |
Crystal system, space group | Orthorhombic, Pbcn | Monoclinic, P21/n | Orthorhombic, Pbcn | Monoclinic, C2/c |
Temperature (K) | 123 | 296 | 296 | 296 |
a, b, c (Å) | 18.843 (3), 16.642 (3), 12.307 (2) | 13.453 (2), 13.334 (2), 24.906 (4) | 20.119 (5), 16.115 (4), 13.055 (3) | 16.073 (10), 19.104 (11), 16.399 (10) |
α, β, γ (°) | 90, 90, 90 | 90, 91.749 (2), 90 | 90, 90, 90 | 90, 111.673 (6), 90 |
V (Å3) | 3859.2 (11) | 4465.5 (13) | 4232.9 (17) | 4679 (5) |
Z | 4 | 4 | 4 | 4 |
Radiation type | Mo Kα | Mo Kα | Mo Kα | Mo Kα |
µ (mm−1) | 0.96 | 1.08 | 1.13 | 0.82 |
Crystal size (mm) | 0.66 × 0.12 × 0.10 | 0.41 × 0.35 × 0.34 | 0.42 × 0.35 × 0.32 | 0.47 × 0.38 × 0.23 |
|
Data collection |
Diffractometer | Rigaku/MSC Mercury CCD diffractometer | Rigaku/MSC Mercury CCD diffractometer | Rigaku/MSC Mercury CCD diffractometer | Rigaku/MSC Mercury CCD diffractometer |
Absorption correction | Numerical NUMABS (Higashi, 1999) | Numerical NUMABS (Higashi, 1999) | Numerical NUMABS (Higashi, 1999) | Numerical NUMABS (Higashi, 1999) |
Tmin, Tmax | 0.809, 0.956 | 0.731, 0.815 | 0.740, 0.803 | 0.765, 0.891 |
No. of measured, independent and observed [I > 2σ(I)] reflections | 29049, 4413, 4134 | 34616, 10190, 8188 | 30878, 4835, 4243 | 17721, 5356, 3475 |
Rint | 0.042 | 0.034 | 0.033 | 0.056 |
(sin θ/λ)max (Å−1) | 0.649 | 0.649 | 0.649 | 0.650 |
|
Refinement |
R[F2 > 2σ(F2)], wR(F2), S | 0.044, 0.080, 1.32 | 0.058, 0.163, 1.08 | 0.050, 0.126, 1.16 | 0.066, 0.213, 1.05 |
No. of reflections | 4416 | 10190 | 4838 | 5356 |
No. of parameters | 313 | 641 | 302 | 392 |
No. of restraints | 0 | 0 | 1 | 474 |
H-atom treatment | H atoms treated by a mixture of independent and constrained refinement | H atoms treated by a mixture of independent and constrained refinement | H atoms treated by a mixture of independent and constrained refinement | H-atom parameters constrained |
| w = 1/[σ2(Fo2) + (0.0208P)2 + 3.7755P] where P = (Fo2 + 2Fc2)/3 | w = 1/[σ2(Fo2) + (0.0753P)2 + 6.5586P] where P = (Fo2 + 2Fc2)/3 | w = 1/[σ2(Fo2) + (0.0552P)2 + 4.7874P] where P = (Fo2 + 2Fc2)/3 | w = 1/[σ2(Fo2) + (0.1143P)2 + 8.0854P] where P = (Fo2 + 2Fc2)/3 |
Δρmax, Δρmin (e Å−3) | 0.79, −0.57 | 0.78, −0.74 | 1.04, −0.61 | 2.60, −0.94 |
Absolute structure | ? | ? | ? | ? |
Absolute structure parameter | ? | ? | ? | ? |
| (V) | (VI) | (VII) | (VIII) |
Crystal data |
Chemical formula | C36H38N18Rh2·2(SiF6)·8(H2O) | C60H60N38Rh4·SiF6·6(ClO4)·12.7(H2O) | C60H60N38Rh4·8(ClO4)·11.41(H2O) | C28H28F12N18Rh2·2(SiF6)·6(H2O) |
Mr | 1356.97 | 2692.69 | 2726.26 | 1214.78 |
Crystal system, space group | Tetragonal, I4122 | Orthorhombic, Pbca | Orthorhombic, Pbca | Monoclinic, C2/c |
Temperature (K) | 296 | 296 | 296 | 296 |
a, b, c (Å) | 17.6300 (5), 17.6300 (5), 16.8037 (6) | 20.170 (2), 21.875 (3), 22.541 (3) | 20.289 (4), 21.524 (5), 22.450 (5) | 27.057 (5), 9.9832 (15), 18.718 (3) |
α, β, γ (°) | 90, 90, 90 | 90, 90, 90 | 90, 90, 90 | 90, 122.2560 (19), 90 |
V (Å3) | 5222.9 (3) | 9946 (2) | 9804 (4) | 4275.6 (13) |
Z | 4 | 4 | 4 | 4 |
Radiation type | Mo Kα | Mo Kα | Mo Kα | Mo Kα |
µ (mm−1) | 0.79 | 0.94 | 0.99 | 0.95 |
Crystal size (mm) | 0.41 × 0.40 × 0.40 | 0.50 × 0.42 × 0.31 | 0.42 × 0.35 × 0.25 | 0.59 × 0.39 × 0.21 |
|
Data collection |
Diffractometer | Rigaku/MSC Mercury CCD diffractometer | Rigaku/MSC Mercury CCD diffractometer | Rigaku/MSC Mercury CCD diffractometer | Rigaku/MSC Mercury CCD diffractometer |
Absorption correction | Numerical NUMABS (Higashi, 1999) | Numerical NUMABS (Higashi, 1999) | Numerical NUMABS (Higashi, 1999) | Numerical NUMABS (Higashi, 1999) |
Tmin, Tmax | 0.727, 0.814 | 0.832, 0.894 | 0.807, 0.884 | 0.747, 0.867 |
No. of measured, independent and observed [I > 2σ(I)] reflections | 20508, 3004, 2952 | 71587, 11352, 10339 | 72426, 11220, 8509 | 16660, 4873, 4409 |
Rint | 0.024 | 0.035 | 0.104 | 0.025 |
(sin θ/λ)max (Å−1) | 0.649 | 0.649 | 0.649 | 0.649 |
|
Refinement |
R[F2 > 2σ(F2)], wR(F2), S | 0.027, 0.073, 1.12 | 0.059, 0.180, 1.17 | 0.092, 0.231, 1.15 | 0.048, 0.136, 1.09 |
No. of reflections | 3004 | 11379 | 11220 | 4873 |
No. of parameters | 220 | 712 | 706 | 309 |
No. of restraints | 15 | 12 | 19 | 0 |
H-atom treatment | H atoms treated by a mixture of independent and constrained refinement | H atoms treated by a mixture of independent and constrained refinement | H atoms treated by a mixture of independent and constrained refinement | H atoms treated by a mixture of independent and constrained refinement |
| w = 1/[σ2(Fo2) + (0.0493P)2 + 1.975P] where P = (Fo2 + 2Fc2)/3 | w = 1/[σ2(Fo2) + (0.0782P)2 + 29.1806P] where P = (Fo2 + 2Fc2)/3 | w = 1/[σ2(Fo2) + (0.0905P)2 + 33.6829P] where P = (Fo2 + 2Fc2)/3 | w = 1/[σ2(Fo2) + (0.0767P)2 + 22.3201P] where P = (Fo2 + 2Fc2)/3 |
Δρmax, Δρmin (e Å−3) | 0.80, −0.36 | 1.65, −1.44 | 1.49, −1.06 | 1.37, −1.21 |
Absolute structure | Flack H D (1983), Acta Cryst. A39, 876-881 | ? | ? | ? |
Absolute structure parameter | −0.02 (3) | ? | ? | ? |
Selected geometric parameters (Å, º) for (I) topRh1—N7 | 2.047 (2) | Rh1—N1 | 2.053 (2) |
Rh1—N3 | 2.048 (2) | Rh1—O1 | 2.299 (2) |
Rh1—N5 | 2.049 (2) | Rh1—Rh1i | 2.6771 (6) |
| | | |
N7—Rh1—N3 | 99.88 (10) | N5—Rh1—O1 | 90.47 (9) |
N7—Rh1—N5 | 79.53 (10) | N1—Rh1—O1 | 86.07 (8) |
N3—Rh1—N5 | 176.24 (9) | N7—Rh1—Rh1i | 92.48 (6) |
N7—Rh1—N1 | 174.71 (9) | N3—Rh1—Rh1i | 92.38 (6) |
N3—Rh1—N1 | 79.74 (10) | N5—Rh1—Rh1i | 91.36 (6) |
N5—Rh1—N1 | 100.49 (10) | N1—Rh1—Rh1i | 92.81 (6) |
N7—Rh1—O1 | 88.63 (8) | O1—Rh1—Rh1i | 178.00 (6) |
N3—Rh1—O1 | 85.80 (9) | | |
| | | |
N1—Rh1—Rh1i—N5i | 39.77 (10) | N3—Rh1—Rh1i—N7i | 40.03 (10) |
Symmetry code: (i) −x+1, y, −z+3/2. |
Hydrogen-bond geometry (Å, º) for (I) top
D—H···A | D—H | H···A | D···A | D—H···A |
N2—H2N···O2 | 0.88 | 1.99 | 2.845 (3) | 162.3 |
N4—H4N···O3 | 0.88 | 1.94 | 2.768 (4) | 156.5 |
N6—H6N···O5 | 0.88 | 1.92 | 2.799 (4) | 175.2 |
N8—H8N···O6 | 0.88 | 2.19 | 2.981 (4) | 148.7 |
N8—H8N···O8 | 0.88 | 2.52 | 3.015 (4) | 116.0 |
O1—H1A···N9ii | 0.83 (5) | 2.57 (5) | 3.354 (4) | 158 (4) |
O1—H1A···O2ii | 0.83 (5) | 2.57 (4) | 3.171 (3) | 130 (4) |
O1—H1A···O4ii | 0.83 (5) | 1.93 (5) | 2.760 (3) | 174 (4) |
O1—H1B···O9 | 0.78 (4) | 1.93 (4) | 2.705 (4) | 171 (4) |
O8—H8A···O1ii | 0.81 (6) | 2.00 (6) | 2.808 (3) | 174 (5) |
O8—H8B···O2i | 0.87 (5) | 2.36 (5) | 3.017 (4) | 133 (4) |
O9—H9A···O7iii | 0.90 (6) | 2.12 (7) | 2.993 (4) | 164 (6) |
O9—H9B···O6iv | 0.83 (5) | 2.21 (6) | 3.038 (4) | 170 (5) |
O9—H9B···O7iv | 0.83 (5) | 2.56 (5) | 3.204 (4) | 135 (5) |
Symmetry codes: (i) −x+1, y, −z+3/2; (ii) x−1/2, −y+1/2, −z+1; (iii) x+1/2, −y+1/2, −z+1; (iv) −x+1/2, −y+1/2, z−1/2. |
Selected geometric parameters (Å, º) for (II) topRh1—N7 | 2.045 (4) | Rh2—N13 | 2.048 (4) |
Rh1—N1 | 2.049 (4) | Rh2—N11 | 2.051 (4) |
Rh1—N5 | 2.050 (4) | Rh2—N9 | 2.057 (4) |
Rh1—N3 | 2.054 (4) | Rh2—N15 | 2.061 (4) |
Rh1—O1 | 2.328 (3) | Rh2—O2 | 2.282 (4) |
Rh1—Rh2 | 2.6488 (6) | | |
| | | |
O20···O11 | 2.790 (18) | O18···O22ii | 2.770 (8) |
O22···O1 | 2.744 (6) | O23···O7ii | 3.070 (12) |
O23···O2 | 2.678 (8) | O21···O15Biii | 3.193 (18) |
O19···O7i | 2.916 (9) | O22···O12iv | 3.177 (14) |
O19···O8i | 3.146 (11) | O21···O4v | 3.291 (13) |
O19···O5i | 3.018 (9) | O23···O5v | 3.173 (12) |
O20···O21i | 3.100 (10) | O23···O4v | 3.281 (15) |
O20···O8i | 3.131 (12) | | |
| | | |
N7—Rh1—N1 | 173.08 (14) | N13—Rh2—N11 | 174.14 (14) |
N7—Rh1—N5 | 79.53 (15) | N13—Rh2—N9 | 99.67 (16) |
N1—Rh1—N5 | 100.15 (15) | N11—Rh2—N9 | 79.56 (17) |
N7—Rh1—N3 | 99.95 (15) | N13—Rh2—N15 | 79.41 (16) |
N1—Rh1—N3 | 79.78 (15) | N11—Rh2—N15 | 100.95 (17) |
N5—Rh1—N3 | 175.18 (13) | N9—Rh2—N15 | 176.01 (14) |
N7—Rh1—O1 | 88.46 (14) | N13—Rh2—O2 | 87.62 (16) |
N1—Rh1—O1 | 84.62 (14) | N11—Rh2—O2 | 86.54 (16) |
N5—Rh1—O1 | 86.72 (12) | N9—Rh2—O2 | 88.12 (16) |
N3—Rh1—O1 | 88.48 (13) | N15—Rh2—O2 | 87.96 (16) |
N7—Rh1—Rh2 | 93.23 (10) | N13—Rh2—Rh1 | 93.64 (9) |
N1—Rh1—Rh2 | 93.69 (10) | N11—Rh2—Rh1 | 92.20 (10) |
N5—Rh1—Rh2 | 91.67 (9) | N9—Rh2—Rh1 | 91.82 (10) |
N3—Rh1—Rh2 | 93.14 (10) | N15—Rh2—Rh1 | 92.11 (10) |
O1—Rh1—Rh2 | 177.42 (10) | O2—Rh2—Rh1 | 178.73 (13) |
| | | |
N5—Rh1—Rh2—N13 | −37.33 (15) | N1—Rh1—Rh2—N9 | −37.81 (15) |
N3—Rh1—Rh2—N11 | −38.13 (16) | N7—Rh1—Rh2—N15 | −37.25 (16) |
Symmetry codes: (i) x−1/2, −y+1/2, z+1/2; (ii) x+1/2, −y+1/2, z+1/2; (iii) x+1/2, −y+1/2, z−1/2; (iv) −x+1/2, y−1/2, −z+3/2; (v) −x+2, −y+1, −z+1. |
Hydrogen-bond geometry (Å, º) for (II) top
D—H···A | D—H | H···A | D···A | D—H···A |
N2—H2N···O19 | 0.86 | 2.05 | 2.829 (7) | 150.9 |
N4—H4N···O19 | 0.86 | 2.27 | 3.013 (7) | 144.5 |
N4—H4N···O10vi | 0.86 | 2.52 | 3.104 (8) | 126.4 |
N6—H6N···O3 | 0.86 | 2.27 | 3.038 (7) | 148.7 |
N6—H6N···O1vii | 0.86 | 2.52 | 3.128 (5) | 128.2 |
N8—H8N···O3 | 0.86 | 2.22 | 2.991 (7) | 149.9 |
N8—H8N···O8 | 0.86 | 2.58 | 3.107 (8) | 120.7 |
N10—H10N···O11 | 0.86 | 2.18 | 3.014 (13) | 162.5 |
N12—H12N···O20 | 0.86 | 1.97 | 2.819 (8) | 166.8 |
N14—H14N···O21 | 0.86 | 2.11 | 2.884 (8) | 150.2 |
N16—H16N···O21 | 0.86 | 2.18 | 2.949 (8) | 148.0 |
Symmetry codes: (vi) −x+1, −y, −z+1; (vii) −x+1, −y+1, −z+1. |
Selected geometric parameters (Å, º) for (III) topRh1—N7 | 2.040 (3) | Rh1—N3 | 2.055 (3) |
Rh1—N5 | 2.049 (3) | Rh1—O1 | 2.307 (4) |
Rh1—N1 | 2.050 (3) | Rh1—Rh1i | 2.6752 (9) |
| | | |
N7—Rh1—N5 | 79.61 (12) | N1—Rh1—O1 | 85.49 (12) |
N7—Rh1—N1 | 174.38 (12) | N3—Rh1—O1 | 89.56 (12) |
N5—Rh1—N1 | 100.22 (12) | N7—Rh1—Rh1i | 91.67 (9) |
N7—Rh1—N3 | 99.84 (12) | N5—Rh1—Rh1i | 91.66 (8) |
N5—Rh1—N3 | 175.47 (12) | N1—Rh1—Rh1i | 93.95 (9) |
N1—Rh1—N3 | 79.88 (12) | N3—Rh1—Rh1i | 92.85 (9) |
N7—Rh1—O1 | 88.90 (12) | O1—Rh1—Rh1i | 177.39 (8) |
N5—Rh1—O1 | 85.94 (11) | | |
| | | |
N1—Rh1—Rh1i—N5i | 40.76 (12) | N3—Rh1—Rh1i—N7i | 41.15 (12) |
Symmetry code: (i) −x+1, y, −z+3/2. |
Hydrogen-bond geometry (Å, º) for (III) top
D—H···A | D—H | H···A | D···A | D—H···A |
N2—H2N···O2 | 0.86 | 1.98 | 2.833 (5) | 171.6 |
N4—H4N···O3 | 0.86 | 2.25 | 3.053 (6) | 156.4 |
N6—H6N···O6 | 0.86 | 2.04 | 2.897 (5) | 177.3 |
N8—H8N···O7 | 0.86 | 1.96 | 2.808 (5) | 170.0 |
O1—H1···O4ii | 0.805 (19) | 2.15 (2) | 2.929 (4) | 163 (5) |
Symmetry code: (ii) x−1/2, −y+1/2, −z+1. |
Selected geometric parameters (Å, º) for (IV) topRh1—N7 | 2.041 (5) | Rh1—N1 | 2.057 (4) |
Rh1—N5 | 2.042 (4) | Rh1—O1 | 2.266 (5) |
Rh1—N3 | 2.049 (4) | Rh1—Rh1i | 2.6313 (18) |
| | | |
N7—Rh1—N5 | 79.88 (18) | N3—Rh1—O1 | 88.97 (17) |
N7—Rh1—N3 | 99.97 (18) | N1—Rh1—O1 | 90.60 (16) |
N5—Rh1—N3 | 173.40 (17) | N7—Rh1—Rh1i | 92.08 (13) |
N7—Rh1—N1 | 175.25 (17) | N5—Rh1—Rh1i | 93.04 (13) |
N5—Rh1—N1 | 99.96 (18) | N3—Rh1—Rh1i | 93.55 (13) |
N3—Rh1—N1 | 79.63 (18) | N1—Rh1—Rh1i | 92.67 (13) |
N7—Rh1—O1 | 84.66 (16) | O1—Rh1—Rh1i | 176.18 (10) |
N5—Rh1—O1 | 84.44 (17) | | |
| | | |
N1—Rh1—Rh1i—N3i | −43.72 (18) | N5—Rh1—Rh1i—N7i | −43.72 (17) |
Symmetry code: (i) −x+1, y, −z+1/2. |
Hydrogen-bond geometry (Å, º) for (IV) top
D—H···A | D—H | H···A | D···A | D—H···A |
N2—H2N···F5 | 0.86 | 1.93 | 2.786 (8) | 170.1 |
N4—H4N···F8B | 0.86 | 1.97 | 2.818 (15) | 170.7 |
N4—H4N···F7A | 0.86 | 1.98 | 2.738 (17) | 145.8 |
N6—H6N···F4B | 0.86 | 1.94 | 2.773 (13) | 162.7 |
N6—H6N···F4A | 0.86 | 2.09 | 2.927 (16) | 165.9 |
N6—H6N···F3A | 0.86 | 2.54 | 3.19 (2) | 133.6 |
N8—H8N···F2A | 0.86 | 1.97 | 2.817 (15) | 166.8 |
N8—H8N···F2B | 0.86 | 2.08 | 2.884 (19) | 154.9 |
N8—H8N···F3B | 0.86 | 2.43 | 3.169 (19) | 144.2 |
N8—H8N···F3A | 0.86 | 2.56 | 3.227 (15) | 135.7 |
Selected geometric parameters (Å, º) for (V) topRh1—N1i | 2.0502 (19) | Rh1—N5 | 2.275 (3) |
Rh1—N3 | 2.057 (2) | Rh1—Rh1ii | 2.7052 (5) |
| | | |
N5—Rh1—Rh1ii | 180.0 | | |
| | | |
N1—Rh1ii—Rh1ii—N3 | | | |
Symmetry codes: (i) y, x, −z; (ii) −x+1, −y+1, z. |
Hydrogen-bond geometry (Å, º) for (V) top
D—H···A | D—H | H···A | D···A | D—H···A |
N2—H2N···F2iii | 0.86 | 1.87 | 2.684 (7) | 158.3 |
N2—H2N···F4 | 0.86 | 2.06 | 2.819 (8) | 147.3 |
N2—H2N···F5 | 0.86 | 2.23 | 2.970 (10) | 143.6 |
N2—H2N···F6iii | 0.86 | 2.33 | 3.004 (9) | 135.6 |
N4—H4N···F1iii | 0.86 | 1.92 | 2.774 (7) | 170.8 |
N4—H4N···F4 | 0.86 | 2.30 | 2.999 (9) | 138.3 |
N4—H4N···O3 | 0.86 | 2.02 | 2.744 (14) | 141.4 |
Symmetry code: (iii) −x+1/2, y, −z+3/4. |
Selected geometric parameters (Å, º) for (VI) topRh1—N7 | 2.053 (4) | Rh2—N13 | 2.044 (4) |
Rh1—N1 | 2.056 (4) | Rh2—N11 | 2.047 (4) |
Rh1—N3 | 2.056 (5) | Rh2—N9 | 2.048 (4) |
Rh1—N5 | 2.056 (4) | Rh2—N15 | 2.058 (4) |
Rh1—N17 | 2.238 (4) | Rh2—N19 | 2.251 (4) |
Rh1—Rh2 | 2.6943 (5) | | |
| | | |
N17—Rh1—Rh2 | 177.87 (13) | N19—Rh2—Rh1 | 179.77 (10) |
| | | |
N5—Rh1—Rh2—N13 | 39.35 (17) | N1—Rh1—Rh2—N9 | 38.70 (18) |
N3—Rh1—Rh2—N11 | 38.46 (18) | N7—Rh1—Rh2—N15 | 39.3 (2) |
Hydrogen-bond geometry (Å, º) for (VI) top
D—H···A | D—H | H···A | D···A | D—H···A |
N2—H2N···F1i | 0.86 | 1.99 | 2.767 (7) | 149.1 |
N4—H4N···O7W | 0.86 | 1.91 | 2.773 (17) | 176.0 |
N4—H4N···O5W | 0.86 | 2.03 | 2.73 (3) | 138.1 |
N6—H6N···F1 | 0.86 | 1.99 | 2.794 (8) | 156.1 |
N6—H6N···F2 | 0.86 | 2.34 | 3.056 (9) | 141.6 |
N8—H8N···F3 | 0.86 | 1.94 | 2.794 (11) | 169.6 |
N10—H10N···O3W | 0.86 | 2.02 | 2.841 (8) | 159.1 |
N12—H12N···O8 | 0.86 | 2.27 | 3.067 (9) | 153.9 |
N12—H12N···O10 | 0.86 | 2.42 | 2.965 (9) | 121.9 |
N14—H14N···O11ii | 0.86 | 2.44 | 3.011 (10) | 124.5 |
N14—H14N···O2 | 0.86 | 2.54 | 3.058 (13) | 119.4 |
N16—H16N···O4W | 0.86 | 2.04 | 2.856 (10) | 158.1 |
N16—H16N···O11ii | 0.86 | 2.62 | 3.131 (10) | 119.6 |
Symmetry codes: (i) x+1/2, −y+3/2, −z+1; (ii) −x+1, −y+1, −z+1. |
Selected geometric parameters (Å, º) for (VII) topRh1—N7 | 2.043 (6) | Rh2—N13 | 2.049 (6) |
Rh1—N5 | 2.062 (6) | Rh2—N9 | 2.050 (6) |
Rh1—N3 | 2.069 (6) | Rh2—N11 | 2.056 (6) |
Rh1—N1 | 2.071 (6) | Rh2—N15 | 2.059 (6) |
Rh1—N17 | 2.235 (6) | Rh2—N19 | 2.248 (6) |
Rh1—Rh2 | 2.6935 (8) | | |
| | | |
N17—Rh1—Rh2 | 176.61 (17) | N19—Rh2—Rh1 | 179.23 (16) |
| | | |
N5—Rh1—Rh2—N13 | 42.5 (2) | N3—Rh1—Rh2—N11 | 41.2 (3) |
N1—Rh1—Rh2—N9 | 40.5 (2) | N7—Rh1—Rh2—N15 | 42.4 (2) |
Hydrogen-bond geometry (Å, º) for (VII) top
D—H···A | D—H | H···A | D···A | D—H···A |
N2—H2N···O14i | 0.86 | 2.08 | 2.872 (13) | 153.6 |
N4—H4N···O5W | 0.86 | 2.08 | 2.75 (4) | 134.5 |
N4—H4N···O14i | 0.86 | 2.55 | 3.273 (16) | 142.4 |
N6—H6N···O15 | 0.86 | 2.33 | 3.075 (14) | 145.3 |
N6—H6N···O13ii | 0.86 | 2.62 | 3.233 (14) | 129.1 |
N8—H8N···O15 | 0.86 | 2.13 | 2.915 (15) | 151.1 |
N8—H8N···Cl4 | 0.86 | 2.92 | 3.782 (9) | 177.8 |
N10—H10N···O3W | 0.86 | 2.00 | 2.824 (11) | 161.3 |
N10—H10N···O10 | 0.86 | 2.59 | 3.077 (11) | 116.7 |
N12—H12N···O8 | 0.86 | 2.27 | 3.062 (12) | 153.9 |
N12—H12N···O10 | 0.86 | 2.41 | 2.945 (11) | 121.3 |
N14—H14N···O11iii | 0.86 | 2.41 | 3.001 (12) | 126.1 |
N14—H14N···O2 | 0.86 | 2.53 | 3.049 (14) | 119.5 |
N16—H16N···O4W | 0.86 | 2.09 | 2.910 (13) | 160.0 |
N16—H16N···O11iii | 0.86 | 2.65 | 3.167 (12) | 119.9 |
Symmetry codes: (i) −x+1/2, y+1/2, z; (ii) −x, −y+1, −z+1; (iii) −x+1, −y+1, −z+1. |
Selected geometric parameters (Å, º) for (VIII) topRh1—N1 | 2.049 (3) | Rh2—N7 | 2.054 (3) |
Rh1—N3 | 2.051 (3) | Rh2—N5 | 2.063 (3) |
Rh1—N9 | 2.330 (4) | Rh2—N10i | 2.228 (5) |
Rh1—Rh2 | 2.6904 (7) | | |
| | | |
O1···O2 | 2.797 (10) | O3···F4ii | 3.120 (14) |
O1···F3ii | 2.895 (15) | O3···F6ii | 3.23 (1) |
O2···F5 | 2.931 (13) | O3···F3ii | 3.254 (14) |
O2···F5iii | 3.08 (1) | | |
| | | |
N1—Rh1—N1iv | 174.10 (18) | N7iv—Rh2—N7 | 175.53 (17) |
N1—Rh1—N3 | 79.22 (14) | N7iv—Rh2—N5iv | 79.18 (14) |
N1iv—Rh1—N3 | 100.64 (14) | N7—Rh2—N5iv | 100.67 (14) |
N1—Rh1—N3iv | 100.64 (14) | N7iv—Rh2—N5 | 100.67 (14) |
N1iv—Rh1—N3iv | 79.22 (14) | N7—Rh2—N5 | 79.18 (14) |
N3—Rh1—N3iv | 177.39 (17) | N5iv—Rh2—N5 | 176.37 (17) |
N1—Rh1—N9 | 87.05 (9) | N7iv—Rh2—N10i | 87.77 (8) |
N1iv—Rh1—N9 | 87.05 (9) | N7—Rh2—N10i | 87.77 (8) |
N3—Rh1—N9 | 88.70 (8) | N5iv—Rh2—N10i | 88.18 (9) |
N3iv—Rh1—N9 | 88.70 (8) | N5—Rh2—N10i | 88.19 (9) |
N1—Rh1—Rh2 | 92.95 (9) | N7iv—Rh2—Rh1 | 92.23 (8) |
N1iv—Rh1—Rh2 | 92.95 (9) | N7—Rh2—Rh1 | 92.23 (8) |
N3—Rh1—Rh2 | 91.30 (8) | N5iv—Rh2—Rh1 | 91.81 (9) |
N3iv—Rh1—Rh2 | 91.30 (8) | N5—Rh2—Rh1 | 91.81 (9) |
N9—Rh1—Rh2 | 180.000 (1) | N10i—Rh2—Rh1 | 180.0 |
| | | |
N3—Rh1—Rh2—N7 | −37.98 (14) | N1—Rh1—Rh2—N5 | −37.95 (14) |
Symmetry codes: (i) x, y−1, z; (ii) −x+3/2, y+1/2, −z+1/2; (iii) −x+3/2, −y+3/2, −z+1; (iv) −x+1, y, −z+1/2. |
Hydrogen-bond geometry (Å, º) for (VIII) top
D—H···A | D—H | H···A | D···A | D—H···A |
N2—H2N···F4 | 0.86 | 1.83 | 2.619 (9) | 152.6 |
N4—H4N···F5 | 0.86 | 2.09 | 2.903 (8) | 157.2 |
N4—H4N···F4 | 0.86 | 2.56 | 3.219 (12) | 134.7 |
N6—H6N···F2v | 0.86 | 2.12 | 2.948 (12) | 161.3 |
N6—H6N···F3v | 0.86 | 2.30 | 2.963 (8) | 134.4 |
N6—H6N···F1v | 0.86 | 2.59 | 3.332 (17) | 145.2 |
N8—H8N···F1v | 0.86 | 2.38 | 3.161 (13) | 151.5 |
N8—H8N···F3v | 0.86 | 2.43 | 3.060 (12) | 130.8 |
Symmetry code: (v) −x+3/2, y−1/2, −z+1/2. |
Subscribe to Acta Crystallographica Section B: Structural Science, Crystal Engineering and Materials
The full text of this article is available to subscribers to the journal.
If you have already registered and are using a computer listed in your registration details, please email
support@iucr.org for assistance.