Supporting information
Crystallographic Information File (CIF) https://doi.org/10.1107/S0108270113015953/yp3031sup1.cif | |
Structure factor file (CIF format) https://doi.org/10.1107/S0108270113015953/yp3031Isup2.hkl |
CCDC reference: 964737
Data collection: APEX2 (Bruker, 2012); cell refinement: SAINT (Bruker, 2009); data reduction: SAINT (Bruker, 2009); program(s) used to solve structure: SIR97 (Altomare et al., 1999); program(s) used to refine structure: SHELXL2012 (Sheldrick, 2012); molecular graphics: SHELXTL (Sheldrick, 2008); software used to prepare material for publication: SHELXTL (Sheldrick, 2008).
[Rh2(CH3)2(C2H6O3P)2(C15H22BN6)2] | Z = 1 |
Mr = 1048.35 | F(000) = 540 |
Triclinic, P1 | Dx = 1.362 Mg m−3 |
a = 10.1383 (9) Å | Mo Kα radiation, λ = 0.71073 Å |
b = 10.6676 (10) Å | Cell parameters from 4044 reflections |
c = 13.5193 (13) Å | θ = 2.2–29.1° |
α = 71.919 (2)° | µ = 0.76 mm−1 |
β = 88.912 (2)° | T = 100 K |
γ = 67.725 (2)° | Block, yellow |
V = 1278.1 (2) Å3 | 0.22 × 0.20 × 0.12 mm |
Bruker SMART APEX II CCD Platform diffractometer | 7079 reflections with I > 2σ(I) |
Radiation source: fine-focus sealed tube | Rint = 0.075 |
ω scans | θmax = 33.7°, θmin = 2.2° |
Absorption correction: multi-scan SADABS (Sheldrick, 2008) | h = −15→15 |
Tmin = 0.695, Tmax = 0.747 | k = −16→16 |
39087 measured reflections | l = −21→21 |
10151 independent reflections |
Refinement on F2 | Primary atom site location: difference Fourier map |
Least-squares matrix: full | Secondary atom site location: difference Fourier map |
R[F2 > 2σ(F2)] = 0.061 | Hydrogen site location: inferred from neighbouring sites |
wR(F2) = 0.157 | H-atom parameters constrained |
S = 1.02 | w = 1/[σ2(Fo2) + (0.0832P)2]
where P = (Fo2 + 2Fc2)/3 |
10151 reflections | (Δ/σ)max < 0.001 |
280 parameters | Δρmax = 4.57 e Å−3 |
0 restraints | Δρmin = −1.19 e Å−3 |
[Rh2(CH3)2(C2H6O3P)2(C15H22BN6)2] | γ = 67.725 (2)° |
Mr = 1048.35 | V = 1278.1 (2) Å3 |
Triclinic, P1 | Z = 1 |
a = 10.1383 (9) Å | Mo Kα radiation |
b = 10.6676 (10) Å | µ = 0.76 mm−1 |
c = 13.5193 (13) Å | T = 100 K |
α = 71.919 (2)° | 0.22 × 0.20 × 0.12 mm |
β = 88.912 (2)° |
Bruker SMART APEX II CCD Platform diffractometer | 10151 independent reflections |
Absorption correction: multi-scan SADABS (Sheldrick, 2008) | 7079 reflections with I > 2σ(I) |
Tmin = 0.695, Tmax = 0.747 | Rint = 0.075 |
39087 measured reflections |
R[F2 > 2σ(F2)] = 0.061 | 0 restraints |
wR(F2) = 0.157 | H-atom parameters constrained |
S = 1.02 | Δρmax = 4.57 e Å−3 |
10151 reflections | Δρmin = −1.19 e Å−3 |
280 parameters |
Experimental. A crystal was placed on the tip of a 0.1 mm diameter glass capillary tube or fiber and mounted on a Bruker SMART APEXII CCD Platform diffractometer for a data collection at 100.0 (5) K. A preliminary set of cell constants and an orientation matrix were calculated from reflections harvested from three orthogonal wedges of reciprocal space. The full data collection was carried out using Mo Kα radiation (graphite monochromator), with a frame time of 60 s and a detector distance of 4.01 cm. A randomly oriented region of reciprocal space was surveyed; six major sections of frames were collected with 0.50° steps in ω at six different ϕ settings and a detector position of -38° in 2θ. The intensity data were corrected for absorption. Final cell constants were calculated from the xyz centroids of 4044 strong reflections from the actual data collection after integration. The space group P1 was determined based on intensity statistics. A direct methods solution was calculated which provided most non-H atoms from the E map. Full-matrix least-squares/difference Fourier cycles were performed which located the remaining non-H atoms. All non-H atoms were refined with anisotropic displacement parameters. All H atoms were placed in ideal positions and refined as riding atoms with relative isotropic displacement parameters. |
Geometry. All e.s.d.'s (except the e.s.d. in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell e.s.d.'s are taken into account individually in the estimation of e.s.d.'s in distances, angles and torsion angles; correlations between e.s.d.'s in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell e.s.d.'s is used for estimating e.s.d.'s involving l.s. planes. |
Refinement. Highly disordered solvent was located in channels parallel to the b axis. Reflection contributions from this solvent were removed using program PLATON, function SQUEEZE (Spek, 2003), which determined there to be 96 electrons in 250 Å3 removed per unit cell. Since the exact identity and amount of solvent could not be determined, no solvent was included in the atom list or molecular formula. (One set of residual peaks did appear to be n-pentane, disordered over an inversion center. However, this did not define the entire solvent area.) Thus all reported items that derive from the molecular formula (e.g., F(000), density, molecular weight, etc.) are known to be incorrect. The large residual peak of 4.57 electrons per Å3, located 0.74 Å from the rhodium atom, may be the result of residual absorption errors. |
x | y | z | Uiso*/Ueq | ||
Rh1 | −0.02530 (3) | 0.08652 (3) | 0.13620 (2) | 0.02025 (8) | |
N1 | 0.1825 (3) | 0.1340 (3) | 0.1157 (2) | 0.0199 (5) | |
N2 | 0.2214 (3) | 0.1671 (3) | 0.1981 (2) | 0.0224 (5) | |
N3 | 0.0743 (3) | −0.0368 (3) | 0.2957 (2) | 0.0226 (5) | |
N4 | 0.1319 (3) | 0.0244 (3) | 0.3475 (2) | 0.0214 (5) | |
N5 | −0.1054 (3) | 0.2678 (3) | 0.1777 (2) | 0.0210 (5) | |
N6 | −0.0217 (3) | 0.2791 (3) | 0.2506 (2) | 0.0201 (5) | |
B1 | 0.1332 (4) | 0.1716 (4) | 0.2910 (3) | 0.0210 (6) | |
H1B | 0.1755 | 0.2024 | 0.3407 | 0.025* | |
C1 | 0.2757 (4) | 0.1502 (4) | 0.0462 (3) | 0.0234 (6) | |
C2 | 0.3735 (4) | 0.1928 (4) | 0.0842 (3) | 0.0270 (7) | |
H2 | 0.4508 | 0.2104 | 0.0504 | 0.032* | |
C3 | 0.3354 (4) | 0.2038 (4) | 0.1802 (3) | 0.0261 (7) | |
C4 | 0.0941 (4) | −0.1671 (4) | 0.3637 (3) | 0.0248 (6) | |
C5 | 0.1614 (4) | −0.1853 (4) | 0.4594 (3) | 0.0306 (7) | |
H5 | 0.1862 | −0.2664 | 0.5210 | 0.037* | |
C6 | 0.1844 (4) | −0.0628 (4) | 0.4467 (3) | 0.0255 (7) | |
C7 | −0.2329 (3) | 0.3788 (4) | 0.1614 (3) | 0.0238 (6) | |
C8 | −0.2314 (4) | 0.4602 (4) | 0.2228 (3) | 0.0262 (7) | |
H8 | −0.3077 | 0.5442 | 0.2262 | 0.031* | |
C9 | −0.0966 (4) | 0.3951 (3) | 0.2784 (3) | 0.0228 (6) | |
C10 | 0.2701 (4) | 0.1286 (4) | −0.0565 (3) | 0.0282 (7) | |
H10A | 0.1859 | 0.1076 | −0.0659 | 0.042* | |
H10B | 0.3572 | 0.0481 | −0.0590 | 0.042* | |
H10C | 0.2633 | 0.2158 | −0.1126 | 0.042* | |
C11 | 0.4018 (4) | 0.2468 (5) | 0.2548 (3) | 0.0413 (10) | |
H11A | 0.4882 | 0.2595 | 0.2287 | 0.062* | |
H11B | 0.4274 | 0.1720 | 0.3236 | 0.062* | |
H11C | 0.3332 | 0.3371 | 0.2612 | 0.062* | |
C12 | 0.0468 (5) | −0.2718 (4) | 0.3396 (3) | 0.0369 (9) | |
H12A | 0.0397 | −0.2533 | 0.2638 | 0.055* | |
H12B | −0.0472 | −0.2614 | 0.3641 | 0.055* | |
H12C | 0.1167 | −0.3694 | 0.3751 | 0.055* | |
C13 | 0.2535 (4) | −0.0249 (4) | 0.5235 (3) | 0.0342 (8) | |
H13A | 0.3344 | −0.0028 | 0.4944 | 0.051* | |
H13B | 0.2880 | −0.1060 | 0.5889 | 0.051* | |
H13C | 0.1832 | 0.0589 | 0.5375 | 0.051* | |
C14 | −0.3559 (4) | 0.4136 (4) | 0.0851 (3) | 0.0307 (7) | |
H14A | −0.3594 | 0.3245 | 0.0815 | 0.046* | |
H14B | −0.3437 | 0.4703 | 0.0157 | 0.046* | |
H14C | −0.4455 | 0.4687 | 0.1077 | 0.046* | |
C15 | −0.0353 (4) | 0.4393 (4) | 0.3549 (3) | 0.0326 (8) | |
H15A | −0.0056 | 0.3618 | 0.4225 | 0.049* | |
H15B | −0.1081 | 0.5258 | 0.3638 | 0.049* | |
H15C | 0.0479 | 0.4591 | 0.3288 | 0.049* | |
C16 | −0.2035 (4) | 0.0506 (4) | 0.1905 (3) | 0.0270 (7) | |
H16A | −0.2371 | 0.0960 | 0.2442 | 0.040* | |
H16B | −0.1785 | −0.0529 | 0.2209 | 0.040* | |
H16C | −0.2797 | 0.0914 | 0.1323 | 0.040* | |
P1 | −0.12505 (9) | 0.18195 (9) | −0.03113 (7) | 0.02162 (16) | |
O1 | −0.0448 (3) | 0.1086 (3) | −0.10500 (17) | 0.0258 (5) | |
O2 | −0.1577 (3) | 0.3492 (3) | −0.0888 (2) | 0.0306 (5) | |
O3 | −0.2858 (3) | 0.1913 (3) | −0.04296 (19) | 0.0283 (5) | |
C17 | −0.3566 (4) | 0.2306 (4) | −0.1463 (3) | 0.0311 (7) | |
H17A | −0.4493 | 0.2216 | −0.1402 | 0.047* | |
H17B | −0.2966 | 0.1670 | −0.1829 | 0.047* | |
H17C | −0.3719 | 0.3300 | −0.1859 | 0.047* | |
C18 | −0.0583 (5) | 0.4104 (4) | −0.0801 (3) | 0.0346 (8) | |
H18A | −0.1084 | 0.5148 | −0.1000 | 0.052* | |
H18B | 0.0157 | 0.3870 | −0.1268 | 0.052* | |
H18C | −0.0134 | 0.3719 | −0.0077 | 0.052* |
U11 | U22 | U33 | U12 | U13 | U23 | |
Rh1 | 0.02014 (12) | 0.02771 (14) | 0.01594 (11) | −0.01066 (10) | 0.00302 (8) | −0.00968 (9) |
N1 | 0.0209 (12) | 0.0235 (13) | 0.0164 (11) | −0.0091 (10) | 0.0019 (9) | −0.0075 (10) |
N2 | 0.0169 (12) | 0.0316 (14) | 0.0205 (12) | −0.0094 (11) | 0.0013 (10) | −0.0110 (11) |
N3 | 0.0267 (14) | 0.0288 (14) | 0.0143 (11) | −0.0133 (12) | 0.0019 (10) | −0.0069 (10) |
N4 | 0.0209 (12) | 0.0232 (13) | 0.0179 (12) | −0.0063 (10) | −0.0007 (10) | −0.0065 (10) |
N5 | 0.0182 (12) | 0.0263 (13) | 0.0199 (12) | −0.0079 (10) | 0.0008 (10) | −0.0103 (11) |
N6 | 0.0196 (12) | 0.0239 (13) | 0.0182 (12) | −0.0094 (10) | 0.0006 (9) | −0.0078 (10) |
B1 | 0.0178 (15) | 0.0287 (18) | 0.0186 (15) | −0.0094 (13) | −0.0004 (12) | −0.0103 (14) |
C1 | 0.0214 (15) | 0.0255 (15) | 0.0239 (15) | −0.0087 (12) | 0.0060 (12) | −0.0099 (13) |
C2 | 0.0185 (14) | 0.0383 (19) | 0.0282 (16) | −0.0139 (14) | 0.0059 (12) | −0.0129 (15) |
C3 | 0.0188 (14) | 0.0352 (18) | 0.0265 (16) | −0.0113 (13) | 0.0022 (12) | −0.0122 (14) |
C4 | 0.0301 (17) | 0.0224 (15) | 0.0201 (15) | −0.0098 (13) | 0.0052 (12) | −0.0055 (12) |
C5 | 0.0334 (19) | 0.0297 (18) | 0.0209 (16) | −0.0088 (15) | 0.0021 (14) | −0.0024 (13) |
C6 | 0.0227 (15) | 0.0334 (18) | 0.0172 (14) | −0.0070 (13) | 0.0009 (11) | −0.0089 (13) |
C7 | 0.0171 (14) | 0.0268 (16) | 0.0247 (15) | −0.0062 (12) | 0.0036 (12) | −0.0080 (13) |
C8 | 0.0250 (16) | 0.0202 (15) | 0.0294 (17) | −0.0049 (13) | 0.0039 (13) | −0.0080 (13) |
C9 | 0.0261 (16) | 0.0218 (15) | 0.0204 (14) | −0.0099 (13) | 0.0044 (12) | −0.0060 (12) |
C10 | 0.0329 (18) | 0.0386 (19) | 0.0238 (16) | −0.0215 (16) | 0.0111 (13) | −0.0156 (14) |
C11 | 0.032 (2) | 0.076 (3) | 0.034 (2) | −0.034 (2) | 0.0079 (16) | −0.026 (2) |
C12 | 0.052 (2) | 0.033 (2) | 0.0282 (18) | −0.0228 (19) | 0.0018 (17) | −0.0047 (15) |
C13 | 0.036 (2) | 0.041 (2) | 0.0183 (15) | −0.0085 (17) | −0.0076 (14) | −0.0083 (15) |
C14 | 0.0206 (16) | 0.0353 (19) | 0.0328 (19) | −0.0049 (14) | −0.0019 (13) | −0.0136 (16) |
C15 | 0.0340 (19) | 0.0323 (19) | 0.038 (2) | −0.0136 (16) | 0.0066 (15) | −0.0193 (16) |
C16 | 0.0266 (16) | 0.0392 (19) | 0.0239 (16) | −0.0180 (15) | 0.0069 (13) | −0.0160 (14) |
P1 | 0.0219 (4) | 0.0243 (4) | 0.0194 (4) | −0.0089 (3) | 0.0009 (3) | −0.0082 (3) |
O1 | 0.0318 (13) | 0.0317 (13) | 0.0153 (10) | −0.0151 (11) | −0.0014 (9) | −0.0062 (9) |
O2 | 0.0353 (14) | 0.0246 (12) | 0.0279 (13) | −0.0089 (11) | −0.0030 (11) | −0.0066 (10) |
O3 | 0.0250 (12) | 0.0383 (14) | 0.0220 (11) | −0.0114 (11) | −0.0002 (9) | −0.0116 (10) |
C17 | 0.0239 (16) | 0.039 (2) | 0.0271 (17) | −0.0066 (15) | −0.0035 (13) | −0.0125 (15) |
C18 | 0.040 (2) | 0.0305 (19) | 0.0320 (19) | −0.0190 (17) | −0.0010 (16) | −0.0011 (15) |
Rh1—N5 | 2.044 (3) | C10—H10A | 0.9800 |
Rh1—C16 | 2.062 (3) | C10—H10B | 0.9800 |
Rh1—O1i | 2.104 (2) | C10—H10C | 0.9800 |
Rh1—N3 | 2.172 (3) | C11—H11A | 0.9800 |
Rh1—P1 | 2.2480 (9) | C11—H11B | 0.9800 |
Rh1—N1 | 2.339 (3) | C11—H11C | 0.9800 |
N1—C1 | 1.339 (4) | C12—H12A | 0.9800 |
N1—N2 | 1.375 (4) | C12—H12B | 0.9800 |
N2—C3 | 1.349 (4) | C12—H12C | 0.9800 |
N2—B1 | 1.529 (4) | C13—H13A | 0.9800 |
N3—C4 | 1.349 (4) | C13—H13B | 0.9800 |
N3—N4 | 1.358 (4) | C13—H13C | 0.9800 |
N4—C6 | 1.351 (4) | C14—H14A | 0.9800 |
N4—B1 | 1.523 (5) | C14—H14B | 0.9800 |
N5—C7 | 1.346 (4) | C14—H14C | 0.9800 |
N5—N6 | 1.375 (4) | C15—H15A | 0.9800 |
N6—C9 | 1.347 (4) | C15—H15B | 0.9800 |
N6—B1 | 1.536 (4) | C15—H15C | 0.9800 |
B1—H1B | 1.0000 | C16—H16A | 0.9800 |
C1—C2 | 1.400 (5) | C16—H16B | 0.9800 |
C1—C10 | 1.482 (5) | C16—H16C | 0.9800 |
C2—C3 | 1.375 (5) | P1—O1 | 1.498 (3) |
C2—H2 | 0.9500 | P1—O3 | 1.602 (3) |
C3—C11 | 1.492 (5) | P1—O2 | 1.612 (3) |
C4—C5 | 1.398 (5) | O1—Rh1i | 2.104 (2) |
C4—C12 | 1.490 (5) | O2—C18 | 1.417 (5) |
C5—C6 | 1.371 (5) | O3—C17 | 1.446 (4) |
C5—H5 | 0.9500 | C17—H17A | 0.9800 |
C6—C13 | 1.495 (5) | C17—H17B | 0.9800 |
C7—C8 | 1.378 (5) | C17—H17C | 0.9800 |
C7—C14 | 1.489 (5) | C18—H18A | 0.9800 |
C8—C9 | 1.383 (5) | C18—H18B | 0.9800 |
C8—H8 | 0.9500 | C18—H18C | 0.9800 |
C9—C15 | 1.492 (5) | ||
N5—Rh1—C16 | 86.29 (12) | C8—C9—C15 | 129.2 (3) |
N5—Rh1—O1i | 174.10 (10) | C1—C10—H10A | 109.5 |
C16—Rh1—O1i | 88.32 (12) | C1—C10—H10B | 109.5 |
N5—Rh1—N3 | 89.56 (11) | H10A—C10—H10B | 109.5 |
C16—Rh1—N3 | 84.87 (13) | C1—C10—H10C | 109.5 |
O1i—Rh1—N3 | 87.56 (10) | H10A—C10—H10C | 109.5 |
N5—Rh1—P1 | 98.63 (8) | H10B—C10—H10C | 109.5 |
C16—Rh1—P1 | 92.59 (10) | C3—C11—H11A | 109.5 |
O1i—Rh1—P1 | 84.00 (7) | C3—C11—H11B | 109.5 |
N3—Rh1—P1 | 171.26 (8) | H11A—C11—H11B | 109.5 |
N5—Rh1—N1 | 84.59 (10) | C3—C11—H11C | 109.5 |
C16—Rh1—N1 | 165.55 (11) | H11A—C11—H11C | 109.5 |
O1i—Rh1—N1 | 100.22 (9) | H11B—C11—H11C | 109.5 |
N3—Rh1—N1 | 83.89 (10) | C4—C12—H12A | 109.5 |
P1—Rh1—N1 | 99.82 (7) | C4—C12—H12B | 109.5 |
C1—N1—N2 | 105.5 (3) | H12A—C12—H12B | 109.5 |
C1—N1—Rh1 | 141.5 (2) | C4—C12—H12C | 109.5 |
N2—N1—Rh1 | 112.80 (18) | H12A—C12—H12C | 109.5 |
C3—N2—N1 | 111.1 (3) | H12B—C12—H12C | 109.5 |
C3—N2—B1 | 127.3 (3) | C6—C13—H13A | 109.5 |
N1—N2—B1 | 121.4 (2) | C6—C13—H13B | 109.5 |
C4—N3—N4 | 106.1 (3) | H13A—C13—H13B | 109.5 |
C4—N3—Rh1 | 135.8 (2) | C6—C13—H13C | 109.5 |
N4—N3—Rh1 | 118.1 (2) | H13A—C13—H13C | 109.5 |
C6—N4—N3 | 111.0 (3) | H13B—C13—H13C | 109.5 |
C6—N4—B1 | 129.2 (3) | C7—C14—H14A | 109.5 |
N3—N4—B1 | 119.7 (3) | C7—C14—H14B | 109.5 |
C7—N5—N6 | 106.4 (3) | H14A—C14—H14B | 109.5 |
C7—N5—Rh1 | 135.7 (2) | C7—C14—H14C | 109.5 |
N6—N5—Rh1 | 117.3 (2) | H14A—C14—H14C | 109.5 |
C9—N6—N5 | 109.7 (3) | H14B—C14—H14C | 109.5 |
C9—N6—B1 | 127.6 (3) | C9—C15—H15A | 109.5 |
N5—N6—B1 | 122.7 (2) | C9—C15—H15B | 109.5 |
N4—B1—N2 | 110.5 (3) | H15A—C15—H15B | 109.5 |
N4—B1—N6 | 108.8 (3) | C9—C15—H15C | 109.5 |
N2—B1—N6 | 109.1 (3) | H15A—C15—H15C | 109.5 |
N4—B1—H1B | 109.5 | H15B—C15—H15C | 109.5 |
N2—B1—H1B | 109.5 | Rh1—C16—H16A | 109.5 |
N6—B1—H1B | 109.5 | Rh1—C16—H16B | 109.5 |
N1—C1—C2 | 110.2 (3) | H16A—C16—H16B | 109.5 |
N1—C1—C10 | 123.4 (3) | Rh1—C16—H16C | 109.5 |
C2—C1—C10 | 126.4 (3) | H16A—C16—H16C | 109.5 |
C3—C2—C1 | 106.2 (3) | H16B—C16—H16C | 109.5 |
C3—C2—H2 | 126.9 | O1—P1—O3 | 106.79 (13) |
C1—C2—H2 | 126.9 | O1—P1—O2 | 104.61 (14) |
N2—C3—C2 | 107.0 (3) | O3—P1—O2 | 98.02 (14) |
N2—C3—C11 | 123.8 (3) | O1—P1—Rh1 | 115.92 (10) |
C2—C3—C11 | 129.2 (3) | O3—P1—Rh1 | 112.81 (10) |
N3—C4—C5 | 109.3 (3) | O2—P1—Rh1 | 116.77 (10) |
N3—C4—C12 | 124.5 (3) | P1—O1—Rh1i | 142.60 (15) |
C5—C4—C12 | 126.2 (3) | C18—O2—P1 | 122.7 (2) |
C6—C5—C4 | 106.5 (3) | C17—O3—P1 | 119.2 (2) |
C6—C5—H5 | 126.8 | O3—C17—H17A | 109.5 |
C4—C5—H5 | 126.8 | O3—C17—H17B | 109.5 |
N4—C6—C5 | 107.0 (3) | H17A—C17—H17B | 109.5 |
N4—C6—C13 | 123.7 (3) | O3—C17—H17C | 109.5 |
C5—C6—C13 | 129.3 (3) | H17A—C17—H17C | 109.5 |
N5—C7—C8 | 109.9 (3) | H17B—C17—H17C | 109.5 |
N5—C7—C14 | 125.5 (3) | O2—C18—H18A | 109.5 |
C8—C7—C14 | 124.6 (3) | O2—C18—H18B | 109.5 |
C7—C8—C9 | 106.3 (3) | H18A—C18—H18B | 109.5 |
C7—C8—H8 | 126.9 | O2—C18—H18C | 109.5 |
C9—C8—H8 | 126.9 | H18A—C18—H18C | 109.5 |
N6—C9—C8 | 107.7 (3) | H18B—C18—H18C | 109.5 |
N6—C9—C15 | 123.1 (3) | ||
C1—N1—N2—C3 | 0.4 (4) | C1—C2—C3—C11 | −179.3 (4) |
Rh1—N1—N2—C3 | −175.6 (2) | N4—N3—C4—C5 | 1.5 (4) |
C1—N1—N2—B1 | 175.6 (3) | Rh1—N3—C4—C5 | −177.0 (2) |
Rh1—N1—N2—B1 | −0.3 (4) | N4—N3—C4—C12 | 179.8 (3) |
C4—N3—N4—C6 | −1.3 (4) | Rh1—N3—C4—C12 | 1.3 (6) |
Rh1—N3—N4—C6 | 177.5 (2) | N3—C4—C5—C6 | −1.2 (4) |
C4—N3—N4—B1 | 177.4 (3) | C12—C4—C5—C6 | −179.5 (4) |
Rh1—N3—N4—B1 | −3.8 (4) | N3—N4—C6—C5 | 0.6 (4) |
C7—N5—N6—C9 | −0.1 (3) | B1—N4—C6—C5 | −177.9 (3) |
Rh1—N5—N6—C9 | −172.5 (2) | N3—N4—C6—C13 | −179.5 (3) |
C7—N5—N6—B1 | 179.9 (3) | B1—N4—C6—C13 | 1.9 (5) |
Rh1—N5—N6—B1 | 7.4 (4) | C4—C5—C6—N4 | 0.4 (4) |
C6—N4—B1—N2 | 116.9 (3) | C4—C5—C6—C13 | −179.5 (3) |
N3—N4—B1—N2 | −61.6 (4) | N6—N5—C7—C8 | 0.0 (4) |
C6—N4—B1—N6 | −123.4 (3) | Rh1—N5—C7—C8 | 170.4 (2) |
N3—N4—B1—N6 | 58.2 (4) | N6—N5—C7—C14 | 177.4 (3) |
C3—N2—B1—N4 | −123.3 (4) | Rh1—N5—C7—C14 | −12.2 (5) |
N1—N2—B1—N4 | 62.3 (4) | N5—C7—C8—C9 | 0.1 (4) |
C3—N2—B1—N6 | 117.1 (3) | C14—C7—C8—C9 | −177.3 (3) |
N1—N2—B1—N6 | −57.3 (4) | N5—N6—C9—C8 | 0.2 (4) |
C9—N6—B1—N4 | 116.9 (3) | B1—N6—C9—C8 | −179.8 (3) |
N5—N6—B1—N4 | −63.0 (4) | N5—N6—C9—C15 | −178.8 (3) |
C9—N6—B1—N2 | −122.5 (3) | B1—N6—C9—C15 | 1.2 (5) |
N5—N6—B1—N2 | 57.6 (4) | C7—C8—C9—N6 | −0.2 (4) |
N2—N1—C1—C2 | 0.2 (4) | C7—C8—C9—C15 | 178.8 (3) |
Rh1—N1—C1—C2 | 174.2 (3) | O3—P1—O1—Rh1i | −63.0 (3) |
N2—N1—C1—C10 | −178.4 (3) | O2—P1—O1—Rh1i | −166.3 (2) |
Rh1—N1—C1—C10 | −4.4 (6) | Rh1—P1—O1—Rh1i | 63.6 (3) |
N1—C1—C2—C3 | −0.7 (4) | O1—P1—O2—C18 | −85.5 (3) |
C10—C1—C2—C3 | 177.9 (3) | O3—P1—O2—C18 | 164.7 (3) |
N1—N2—C3—C2 | −0.8 (4) | Rh1—P1—O2—C18 | 44.1 (3) |
B1—N2—C3—C2 | −175.7 (3) | O1—P1—O3—C17 | −42.6 (3) |
N1—N2—C3—C11 | 179.4 (4) | O2—P1—O3—C17 | 65.4 (3) |
B1—N2—C3—C11 | 4.5 (6) | Rh1—P1—O3—C17 | −171.1 (2) |
C1—C2—C3—N2 | 0.9 (4) |
Symmetry code: (i) −x, −y, −z. |
Experimental details
Crystal data | |
Chemical formula | [Rh2(CH3)2(C2H6O3P)2(C15H22BN6)2] |
Mr | 1048.35 |
Crystal system, space group | Triclinic, P1 |
Temperature (K) | 100 |
a, b, c (Å) | 10.1383 (9), 10.6676 (10), 13.5193 (13) |
α, β, γ (°) | 71.919 (2), 88.912 (2), 67.725 (2) |
V (Å3) | 1278.1 (2) |
Z | 1 |
Radiation type | Mo Kα |
µ (mm−1) | 0.76 |
Crystal size (mm) | 0.22 × 0.20 × 0.12 |
Data collection | |
Diffractometer | Bruker SMART APEX II CCD Platform diffractometer |
Absorption correction | Multi-scan SADABS (Sheldrick, 2008) |
Tmin, Tmax | 0.695, 0.747 |
No. of measured, independent and observed [I > 2σ(I)] reflections | 39087, 10151, 7079 |
Rint | 0.075 |
(sin θ/λ)max (Å−1) | 0.781 |
Refinement | |
R[F2 > 2σ(F2)], wR(F2), S | 0.061, 0.157, 1.02 |
No. of reflections | 10151 |
No. of parameters | 280 |
H-atom treatment | H-atom parameters constrained |
Δρmax, Δρmin (e Å−3) | 4.57, −1.19 |
Computer programs: APEX2 (Bruker, 2012), SAINT (Bruker, 2009), SIR97 (Altomare et al., 1999), SHELXL2012 (Sheldrick, 2012), SHELXTL (Sheldrick, 2008).
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