Supporting information
Crystallographic Information File (CIF) https://doi.org/10.1107/S0108270100002250/qa0209sup1.cif | |
Structure factor file (CIF format) https://doi.org/10.1107/S0108270100002250/qa0209Isup2.hkl |
CCDC reference: 143319
C2Me4(C5H4)2ZrCl2 (1.1 g, 2.9 mmol) and lithium tetrahydroborate (0.25 g, 11.5 mmol) were stirred in tetrahydrofuran at room temperature for 12 h (James et al., 1967). The solvent was removed and the residue extracted three times with 70 ml toluene. The yellow solution was concentrated until precipitation started. After warming and addition of 20 ml pentane, the solution was cooled to 193 K. Filtration and washing with pentane yielded 570 mg of a colourless powder (59% yield). NMR (250 MHz, C6D6): 6.18 (t, 4H), 5.59 (t, 4H), 0.76 (s, 12H), 1.0 [bq, J(BH) = 60 Hz, 8H]. Elemental analysis: calculated C 57.7, H 8.7%; found C 57.4, H 8.3% All operations were carried out under exclusion of air and moisture. Solvents were dried by standard techniques.
Data collection: MolEN; cell refinement: MolEN; data reduction: MolEN; program(s) used to solve structure: SHELXS86 (Sheldrick, 1985); program(s) used to refine structure: SHELXL97 (Sheldrick, 1997).
[Zr(BH4)2(C16H20)] | Z = 2 |
Mr = 333.22 | F(000) = 348 |
Triclinic, P1 | Dx = 1.315 Mg m−3 |
a = 7.699 (2) Å | Mo Kα radiation, λ = 0.71073 Å |
b = 9.341 (2) Å | Cell parameters from 25 reflections |
c = 12.934 (3) Å | θ = 14.0–15.9° |
α = 77.77 (3)° | µ = 0.64 mm−1 |
β = 78.52 (3)° | T = 153 K |
γ = 69.09 (3)° | Block cut from a needle, colourless |
V = 841.4 (3) Å3 | 0.4 × 0.4 × 0.4 mm |
Enraf-Nonius CAD-4 diffractometer | 3360 reflections with I > 2σ(I) |
Radiation source: fine-focus sealed tube | Rint = 0.014 |
Graphite monochromator | θmax = 26.9°, θmin = 2.4° |
ω/2θ scans | h = 0→9 |
Absorption correction: ψ scan (MolEN; Enraf-Nonius, 1990) | k = −11→11 |
Tmin = 0.696, Tmax = 0.775 | l = −16→16 |
5012 measured reflections | 3 standard reflections every 60 min |
3653 independent reflections | intensity decay: 1.0% |
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)] = 0.023 | Hydrogen site location: difference Fourier map |
wR(F2) = 0.058 | All H-atom parameters refined |
S = 1.04 | w = 1/[σ2(Fo2) + (0.0351P)2 + 0.3682P] where P = (Fo2 + 2Fc2)/3 |
3653 reflections | (Δ/σ)max < 0.001 |
284 parameters | Δρmax = 0.81 e Å−3 |
0 restraints | Δρmin = −0.69 e Å−3 |
[Zr(BH4)2(C16H20)] | γ = 69.09 (3)° |
Mr = 333.22 | V = 841.4 (3) Å3 |
Triclinic, P1 | Z = 2 |
a = 7.699 (2) Å | Mo Kα radiation |
b = 9.341 (2) Å | µ = 0.64 mm−1 |
c = 12.934 (3) Å | T = 153 K |
α = 77.77 (3)° | 0.4 × 0.4 × 0.4 mm |
β = 78.52 (3)° |
Enraf-Nonius CAD-4 diffractometer | 3360 reflections with I > 2σ(I) |
Absorption correction: ψ scan (MolEN; Enraf-Nonius, 1990) | Rint = 0.014 |
Tmin = 0.696, Tmax = 0.775 | 3 standard reflections every 60 min |
5012 measured reflections | intensity decay: 1.0% |
3653 independent reflections |
R[F2 > 2σ(F2)] = 0.023 | 0 restraints |
wR(F2) = 0.058 | All H-atom parameters refined |
S = 1.04 | Δρmax = 0.81 e Å−3 |
3653 reflections | Δρmin = −0.69 e Å−3 |
284 parameters |
Geometry. All e.s.d.'s (except the e.s.d. in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell e.s.d.'s are taken into account individually in the estimation of e.s.d.'s in distances, angles and torsion angles; correlations between e.s.d.'s in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell e.s.d.'s is used for estimating e.s.d.'s involving l.s. planes. |
Refinement. Refinement of F2 against ALL reflections. The weighted R-factor wR and goodness of fit S are based on F2, conventional R-factors R are based on F, with F set to zero for negative F2. The threshold expression of F2 > σ(F2) is used only for calculating R-factors(gt) etc. and is not relevant to the choice of reflections for refinement. R-factors based on F2 are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger. |
x | y | z | Uiso*/Ueq | ||
Zr1 | −0.25624 (2) | −0.04144 (2) | 0.25148 (1) | 0.01553 (6) | |
B1 | −0.3376 (3) | 0.1093 (3) | 0.41112 (17) | 0.0287 (4) | |
B2 | −0.1841 (4) | 0.1515 (3) | 0.08607 (18) | 0.0336 (5) | |
C1 | −0.4236 (2) | −0.20897 (18) | 0.21681 (13) | 0.0178 (3) | |
C2 | −0.5218 (2) | −0.14160 (19) | 0.30943 (14) | 0.0194 (3) | |
C3 | −0.6051 (2) | 0.0197 (2) | 0.27883 (16) | 0.0252 (4) | |
C4 | −0.5545 (3) | 0.0551 (2) | 0.16936 (16) | 0.0275 (4) | |
C5 | −0.4410 (3) | −0.0854 (2) | 0.13072 (15) | 0.0225 (3) | |
C6 | −0.0768 (2) | −0.32500 (19) | 0.28687 (14) | 0.0213 (3) | |
C7 | −0.0728 (3) | −0.2598 (2) | 0.37514 (15) | 0.0260 (4) | |
C8 | 0.0340 (3) | −0.1581 (2) | 0.34076 (17) | 0.0310 (4) | |
C9 | 0.0927 (3) | −0.1568 (2) | 0.23129 (17) | 0.0299 (4) | |
C10 | 0.0223 (2) | −0.2569 (2) | 0.19692 (15) | 0.0241 (4) | |
C11 | −0.3233 (2) | −0.38148 (19) | 0.21138 (14) | 0.0208 (3) | |
C12 | −0.1650 (2) | −0.44810 (19) | 0.28787 (15) | 0.0238 (4) | |
C13 | −0.2445 (3) | −0.4029 (2) | 0.09454 (16) | 0.0290 (4) | |
C14 | −0.4730 (3) | −0.4629 (2) | 0.24496 (18) | 0.0297 (4) | |
C15 | −0.2425 (3) | −0.5001 (2) | 0.40367 (17) | 0.0331 (4) | |
C16 | −0.0067 (3) | −0.5913 (2) | 0.2514 (2) | 0.0377 (5) | |
H2 | −0.536 (3) | −0.192 (3) | 0.3778 (19) | 0.027 (5)* | |
H5 | −0.383 (3) | −0.093 (2) | 0.0589 (18) | 0.023 (5)* | |
H1A | −0.361 (3) | −0.009 (3) | 0.4068 (19) | 0.034 (6)* | |
H15C | −0.342 (3) | −0.423 (3) | 0.4339 (19) | 0.034 (6)* | |
H2B | −0.154 (3) | 0.016 (3) | 0.0976 (19) | 0.036 (6)* | |
H10 | 0.045 (3) | −0.277 (2) | 0.1262 (19) | 0.027 (5)* | |
H3 | −0.673 (3) | 0.090 (3) | 0.324 (2) | 0.035 (6)* | |
H13C | −0.349 (4) | −0.352 (3) | 0.048 (2) | 0.038 (6)* | |
H7 | −0.129 (3) | −0.277 (3) | 0.442 (2) | 0.032 (6)* | |
H13B | −0.150 (3) | −0.356 (3) | 0.0637 (19) | 0.035 (6)* | |
H14C | −0.546 (3) | −0.443 (3) | 0.315 (2) | 0.032 (6)* | |
H4 | −0.586 (3) | 0.155 (3) | 0.1277 (19) | 0.032 (6)* | |
H15B | −0.141 (4) | −0.533 (3) | 0.446 (2) | 0.040 (6)* | |
H13A | −0.192 (3) | −0.512 (3) | 0.0913 (19) | 0.031 (6)* | |
H14B | −0.416 (3) | −0.564 (3) | 0.250 (2) | 0.041 (7)* | |
H8 | 0.054 (3) | −0.103 (3) | 0.384 (2) | 0.038 (6)* | |
H1C | −0.472 (4) | 0.202 (3) | 0.418 (2) | 0.047 (7)* | |
H2D | −0.053 (4) | 0.173 (3) | 0.079 (2) | 0.043 (7)* | |
H16C | 0.063 (3) | −0.567 (3) | 0.185 (2) | 0.032 (6)* | |
H2A | −0.278 (4) | 0.184 (3) | 0.165 (2) | 0.045 (7)* | |
H15A | −0.280 (3) | −0.592 (3) | 0.409 (2) | 0.040 (7)* | |
H14A | −0.561 (4) | −0.424 (3) | 0.194 (2) | 0.040 (6)* | |
H16B | 0.076 (3) | −0.629 (3) | 0.304 (2) | 0.034 (6)* | |
H2C | −0.267 (4) | 0.212 (3) | 0.022 (2) | 0.045 (7)* | |
H9 | 0.159 (4) | −0.099 (3) | 0.187 (2) | 0.044 (7)* | |
H1B | −0.247 (3) | 0.135 (3) | 0.330 (2) | 0.042 (7)* | |
H1D | −0.248 (4) | 0.086 (3) | 0.473 (2) | 0.046 (7)* | |
H16A | −0.051 (4) | −0.669 (4) | 0.247 (2) | 0.060 (9)* |
U11 | U22 | U33 | U12 | U13 | U23 | |
Zr1 | 0.01831 (9) | 0.01429 (8) | 0.01530 (9) | −0.00710 (6) | −0.00153 (5) | −0.00270 (5) |
B1 | 0.0420 (12) | 0.0304 (11) | 0.0211 (10) | −0.0204 (10) | 0.0018 (9) | −0.0104 (8) |
B2 | 0.0502 (14) | 0.0258 (10) | 0.0233 (11) | −0.0178 (10) | 0.0056 (10) | −0.0011 (8) |
C1 | 0.0166 (7) | 0.0159 (7) | 0.0230 (8) | −0.0049 (6) | −0.0065 (6) | −0.0042 (6) |
C2 | 0.0160 (7) | 0.0205 (8) | 0.0241 (9) | −0.0082 (6) | −0.0026 (6) | −0.0049 (7) |
C3 | 0.0170 (8) | 0.0215 (8) | 0.0375 (10) | −0.0021 (7) | −0.0064 (7) | −0.0107 (8) |
C4 | 0.0285 (9) | 0.0171 (8) | 0.0365 (10) | −0.0016 (7) | −0.0171 (8) | −0.0020 (7) |
C5 | 0.0271 (9) | 0.0199 (8) | 0.0226 (9) | −0.0069 (7) | −0.0109 (7) | −0.0019 (7) |
C6 | 0.0167 (7) | 0.0185 (8) | 0.0261 (9) | −0.0010 (6) | −0.0079 (6) | −0.0016 (6) |
C7 | 0.0243 (9) | 0.0274 (9) | 0.0247 (9) | −0.0050 (7) | −0.0105 (7) | −0.0001 (7) |
C8 | 0.0242 (9) | 0.0364 (10) | 0.0380 (11) | −0.0092 (8) | −0.0148 (8) | −0.0090 (9) |
C9 | 0.0172 (8) | 0.0338 (10) | 0.0404 (11) | −0.0102 (7) | −0.0030 (7) | −0.0070 (8) |
C10 | 0.0158 (8) | 0.0260 (9) | 0.0292 (10) | −0.0042 (7) | −0.0011 (7) | −0.0078 (7) |
C11 | 0.0229 (8) | 0.0146 (7) | 0.0259 (9) | −0.0049 (6) | −0.0061 (7) | −0.0047 (6) |
C12 | 0.0242 (8) | 0.0147 (7) | 0.0308 (9) | −0.0032 (7) | −0.0090 (7) | −0.0005 (7) |
C13 | 0.0336 (10) | 0.0239 (9) | 0.0301 (10) | −0.0066 (8) | −0.0041 (8) | −0.0108 (7) |
C14 | 0.0299 (10) | 0.0193 (9) | 0.0438 (12) | −0.0117 (8) | −0.0072 (9) | −0.0050 (8) |
C15 | 0.0399 (11) | 0.0260 (10) | 0.0316 (11) | −0.0117 (9) | −0.0121 (9) | 0.0074 (8) |
C16 | 0.0322 (11) | 0.0193 (9) | 0.0571 (15) | 0.0021 (8) | −0.0134 (11) | −0.0080 (9) |
Zr1—C10 | 2.463 (2) | C4—C5 | 1.422 (3) |
Zr1—C2 | 2.4647 (18) | C4—H4 | 0.95 (2) |
Zr1—C7 | 2.485 (2) | C5—H5 | 0.95 (2) |
Zr1—C5 | 2.4911 (18) | C6—C7 | 1.413 (3) |
Zr1—C9 | 2.494 (2) | C6—C10 | 1.421 (3) |
Zr1—C6 | 2.5020 (19) | C6—C12 | 1.527 (2) |
Zr1—C8 | 2.504 (2) | C7—C8 | 1.417 (3) |
Zr1—C1 | 2.5051 (17) | C7—H7 | 0.90 (2) |
Zr1—C3 | 2.5057 (19) | C8—C9 | 1.397 (3) |
Zr1—C4 | 2.510 (2) | C8—H8 | 0.90 (3) |
Zr1—B1 | 2.594 (2) | C9—C10 | 1.414 (3) |
Zr1—B2 | 2.597 (2) | C9—H9 | 0.91 (3) |
Zr1—H1A | 2.05 (2) | C10—H10 | 0.94 (2) |
Zr1—H2B | 2.02 (2) | C11—C13 | 1.539 (3) |
Zr1—H2A | 2.13 (3) | C11—C14 | 1.543 (3) |
Zr1—H1B | 2.15 (3) | C11—C12 | 1.590 (2) |
B1—H1A | 1.19 (2) | C12—C16 | 1.540 (3) |
B1—H1C | 1.09 (3) | C12—C15 | 1.542 (3) |
B1—H1B | 1.17 (3) | C13—H13C | 1.02 (3) |
B1—H1D | 1.10 (3) | C13—H13B | 0.96 (2) |
B2—H2B | 1.18 (2) | C13—H13A | 0.96 (2) |
B2—H2D | 1.08 (3) | C14—H14C | 0.98 (2) |
B2—H2A | 1.15 (3) | C14—H14B | 0.89 (3) |
B2—H2C | 1.08 (3) | C14—H14A | 0.97 (3) |
C1—C5 | 1.412 (2) | C15—H15C | 0.93 (2) |
C1—C2 | 1.422 (2) | C15—H15B | 0.97 (3) |
C1—C11 | 1.528 (2) | C15—H15A | 0.99 (3) |
C2—C3 | 1.413 (2) | C16—H16C | 0.94 (3) |
C2—H2 | 0.91 (2) | C16—H16B | 0.94 (2) |
C3—C4 | 1.393 (3) | C16—H16A | 0.92 (3) |
C3—H3 | 0.92 (3) | ||
C10—Zr1—C2 | 107.74 (6) | H2B—Zr1—H1B | 104.1 (10) |
C10—Zr1—C7 | 54.69 (7) | H2A—Zr1—H1B | 60.0 (10) |
C2—Zr1—C7 | 88.55 (7) | Zr1—B1—H1A | 50.5 (11) |
C10—Zr1—C5 | 91.44 (7) | Zr1—B1—H1C | 117.6 (14) |
C2—Zr1—C5 | 54.51 (6) | H1A—B1—H1C | 110.3 (18) |
C7—Zr1—C5 | 121.11 (6) | Zr1—B1—H1B | 54.8 (12) |
C10—Zr1—C9 | 33.14 (6) | H1A—B1—H1B | 104.7 (17) |
C2—Zr1—C9 | 135.75 (6) | H1C—B1—H1B | 110.3 (18) |
C7—Zr1—C9 | 54.42 (7) | Zr1—B1—H1D | 125.1 (13) |
C5—Zr1—C9 | 121.00 (7) | H1A—B1—H1D | 108.0 (18) |
C10—Zr1—C6 | 33.25 (6) | H1C—B1—H1D | 117.2 (19) |
C2—Zr1—C6 | 80.89 (6) | H1B—B1—H1D | 105.6 (18) |
C7—Zr1—C6 | 32.92 (6) | Zr1—B2—H2B | 48.8 (12) |
C5—Zr1—C6 | 91.60 (6) | Zr1—B2—H2D | 116.1 (13) |
C9—Zr1—C6 | 54.87 (7) | H2B—B2—H2D | 109.0 (18) |
C10—Zr1—C8 | 54.50 (7) | Zr1—B2—H2A | 53.7 (13) |
C2—Zr1—C8 | 120.93 (7) | H2B—B2—H2A | 101.9 (17) |
C7—Zr1—C8 | 33.00 (7) | H2D—B2—H2A | 111.0 (18) |
C5—Zr1—C8 | 144.38 (6) | Zr1—B2—H2C | 128.3 (14) |
C9—Zr1—C8 | 32.45 (7) | H2B—B2—H2C | 111.3 (18) |
C6—Zr1—C8 | 54.70 (7) | H2D—B2—H2C | 115.6 (19) |
C10—Zr1—C1 | 82.12 (6) | H2A—B2—H2C | 107.2 (18) |
C2—Zr1—C1 | 33.24 (6) | C5—C1—C2 | 106.41 (15) |
C7—Zr1—C1 | 90.64 (6) | C5—C1—C11 | 126.92 (16) |
C5—Zr1—C1 | 32.84 (6) | C2—C1—C11 | 126.65 (15) |
C9—Zr1—C1 | 115.06 (6) | C5—C1—Zr1 | 73.03 (10) |
C6—Zr1—C1 | 66.84 (6) | C2—C1—Zr1 | 71.82 (9) |
C8—Zr1—C1 | 120.80 (6) | C11—C1—Zr1 | 121.39 (11) |
C10—Zr1—C3 | 136.82 (6) | C3—C2—C1 | 108.71 (16) |
C2—Zr1—C3 | 33.01 (6) | C3—C2—Zr1 | 75.09 (10) |
C7—Zr1—C3 | 117.40 (7) | C1—C2—Zr1 | 74.94 (10) |
C5—Zr1—C3 | 54.17 (7) | C3—C2—H2 | 123.8 (14) |
C9—Zr1—C3 | 168.63 (6) | C1—C2—H2 | 127.4 (14) |
C6—Zr1—C3 | 113.81 (6) | Zr1—C2—H2 | 118.8 (14) |
C8—Zr1—C3 | 144.66 (7) | C4—C3—C2 | 108.17 (16) |
C1—Zr1—C3 | 54.74 (6) | C4—C3—Zr1 | 74.07 (11) |
C10—Zr1—C4 | 124.07 (7) | C2—C3—Zr1 | 71.90 (10) |
C2—Zr1—C4 | 54.34 (6) | C4—C3—H3 | 125.9 (15) |
C7—Zr1—C4 | 142.09 (7) | C2—C3—H3 | 125.7 (15) |
C5—Zr1—C4 | 33.03 (6) | Zr1—C3—H3 | 116.1 (15) |
C9—Zr1—C4 | 149.10 (7) | C3—C4—C5 | 107.87 (16) |
C6—Zr1—C4 | 121.17 (6) | C3—C4—Zr1 | 73.69 (11) |
C8—Zr1—C4 | 175.08 (6) | C5—C4—Zr1 | 72.74 (10) |
C1—Zr1—C4 | 54.69 (6) | C3—C4—H4 | 126.7 (14) |
C3—Zr1—C4 | 32.24 (7) | C5—C4—H4 | 125.4 (14) |
C10—Zr1—B1 | 131.45 (8) | Zr1—C4—H4 | 117.9 (14) |
C2—Zr1—B1 | 93.83 (7) | C1—C5—C4 | 108.76 (16) |
C7—Zr1—B1 | 83.97 (8) | C1—C5—Zr1 | 74.13 (10) |
C5—Zr1—B1 | 135.03 (7) | C4—C5—Zr1 | 74.23 (10) |
C9—Zr1—B1 | 103.96 (8) | C1—C5—H5 | 126.4 (12) |
C6—Zr1—B1 | 116.30 (7) | C4—C5—H5 | 124.8 (13) |
C8—Zr1—B1 | 77.02 (8) | Zr1—C5—H5 | 116.1 (13) |
C1—Zr1—B1 | 127.03 (7) | C7—C6—C10 | 106.62 (16) |
C3—Zr1—B1 | 81.63 (8) | C7—C6—C12 | 126.97 (17) |
C4—Zr1—B1 | 103.99 (8) | C10—C6—C12 | 126.39 (16) |
C10—Zr1—B2 | 92.64 (8) | C7—C6—Zr1 | 72.87 (10) |
C2—Zr1—B2 | 131.76 (8) | C10—C6—Zr1 | 71.87 (10) |
C7—Zr1—B2 | 136.74 (8) | C12—C6—Zr1 | 121.76 (11) |
C5—Zr1—B2 | 82.56 (8) | C6—C7—C8 | 108.69 (17) |
C9—Zr1—B2 | 82.55 (9) | C6—C7—Zr1 | 74.21 (10) |
C6—Zr1—B2 | 125.63 (7) | C8—C7—Zr1 | 74.25 (11) |
C8—Zr1—B2 | 106.63 (9) | C6—C7—H7 | 127.1 (15) |
C1—Zr1—B2 | 114.32 (7) | C8—C7—H7 | 124.2 (15) |
C3—Zr1—B2 | 105.84 (8) | Zr1—C7—H7 | 116.8 (15) |
C4—Zr1—B2 | 77.87 (8) | C9—C8—C7 | 108.01 (18) |
B1—Zr1—B2 | 104.67 (7) | C9—C8—Zr1 | 73.38 (11) |
C10—Zr1—H1A | 124.6 (6) | C7—C8—Zr1 | 72.75 (10) |
C2—Zr1—H1A | 71.3 (7) | C9—C8—H8 | 128.0 (16) |
C7—Zr1—H1A | 70.1 (6) | C7—C8—H8 | 124.0 (16) |
C5—Zr1—H1A | 122.5 (7) | Zr1—C8—H8 | 117.8 (16) |
C9—Zr1—H1A | 110.2 (6) | C8—C9—C10 | 108.04 (18) |
C6—Zr1—H1A | 97.9 (6) | C8—C9—Zr1 | 74.17 (11) |
C8—Zr1—H1A | 78.0 (6) | C10—C9—Zr1 | 72.22 (10) |
C1—Zr1—H1A | 103.1 (7) | C8—C9—H9 | 128.1 (17) |
C3—Zr1—H1A | 70.4 (6) | C10—C9—H9 | 123.8 (17) |
C4—Zr1—H1A | 100.7 (6) | Zr1—C9—H9 | 117.0 (16) |
B1—Zr1—H1A | 26.7 (7) | C9—C10—C6 | 108.57 (17) |
B2—Zr1—H1A | 130.5 (7) | C9—C10—Zr1 | 74.64 (11) |
C10—Zr1—H2B | 70.5 (7) | C6—C10—Zr1 | 74.88 (10) |
C2—Zr1—H2B | 124.9 (7) | C9—C10—H10 | 124.3 (13) |
C7—Zr1—H2B | 123.0 (7) | C6—C10—H10 | 127.1 (13) |
C5—Zr1—H2B | 70.3 (7) | Zr1—C10—H10 | 119.3 (13) |
C9—Zr1—H2B | 71.7 (7) | C1—C11—C13 | 109.14 (15) |
C6—Zr1—H2B | 101.8 (7) | C1—C11—C14 | 107.37 (14) |
C8—Zr1—H2B | 102.8 (7) | C13—C11—C14 | 106.19 (15) |
C1—Zr1—H2B | 96.8 (7) | C1—C11—C12 | 109.42 (13) |
C3—Zr1—H2B | 112.5 (7) | C13—C11—C12 | 112.65 (15) |
C4—Zr1—H2B | 80.4 (7) | C14—C11—C12 | 111.89 (15) |
B1—Zr1—H2B | 129.7 (7) | C6—C12—C16 | 107.46 (16) |
B2—Zr1—H2B | 26.1 (7) | C6—C12—C15 | 109.23 (16) |
H1A—Zr1—H2B | 156.2 (10) | C16—C12—C15 | 106.33 (17) |
C10—Zr1—H2A | 116.7 (7) | C6—C12—C11 | 109.79 (13) |
C2—Zr1—H2A | 124.4 (7) | C16—C12—C11 | 111.71 (16) |
C7—Zr1—H2A | 144.5 (7) | C15—C12—C11 | 112.15 (16) |
C5—Zr1—H2A | 91.6 (7) | C11—C13—H13C | 109.7 (14) |
C9—Zr1—H2A | 98.5 (7) | C11—C13—H13B | 114.4 (14) |
C6—Zr1—H2A | 149.9 (7) | H13B—C13—H13C | 105.3 (19) |
C8—Zr1—H2A | 111.8 (7) | C11—C13—H13A | 108.3 (14) |
C1—Zr1—H2A | 123.9 (7) | H13C—C13—H13A | 110.4 (19) |
C3—Zr1—H2A | 92.1 (7) | H13B—C13—H13A | 108.7 (19) |
C4—Zr1—H2A | 73.1 (7) | C11—C14—H14C | 113.0 (14) |
B1—Zr1—H2A | 81.1 (7) | C11—C14—H14B | 108.9 (16) |
B2—Zr1—H2A | 25.9 (7) | H14C—C14—H14B | 107 (2) |
H1A—Zr1—H2A | 105.5 (10) | C11—C14—H14A | 109.2 (15) |
H2B—Zr1—H2A | 51.7 (10) | H14C—C14—H14A | 107 (2) |
C10—Zr1—H1B | 123.7 (6) | H14B—C14—H14A | 112 (2) |
C2—Zr1—H1B | 118.3 (7) | C12—C15—H15C | 114.1 (15) |
C7—Zr1—H1B | 94.5 (7) | C12—C15—H15B | 107.8 (15) |
C5—Zr1—H1B | 141.4 (6) | H15B—C15—H15C | 108 (2) |
C9—Zr1—H1B | 90.8 (6) | C12—C15—H15A | 111.0 (15) |
C6—Zr1—H1B | 126.3 (7) | H15C—C15—H15A | 109 (2) |
C8—Zr1—H1B | 74.1 (6) | H15B—C15—H15A | 106 (2) |
C1—Zr1—H1B | 151.0 (7) | C12—C16—H16C | 112.5 (14) |
C3—Zr1—H1B | 98.1 (7) | C12—C16—H16B | 106.5 (14) |
C4—Zr1—H1B | 109.0 (6) | H16C—C16—H16B | 108 (2) |
B1—Zr1—H1B | 26.4 (7) | C12—C16—H16A | 112.2 (19) |
B2—Zr1—H1B | 80.4 (7) | H16C—C16—H16A | 109 (2) |
H1A—Zr1—H1B | 52.8 (9) | H16B—C16—H16A | 108 (2) |
Experimental details
Crystal data | |
Chemical formula | [Zr(BH4)2(C16H20)] |
Mr | 333.22 |
Crystal system, space group | Triclinic, P1 |
Temperature (K) | 153 |
a, b, c (Å) | 7.699 (2), 9.341 (2), 12.934 (3) |
α, β, γ (°) | 77.77 (3), 78.52 (3), 69.09 (3) |
V (Å3) | 841.4 (3) |
Z | 2 |
Radiation type | Mo Kα |
µ (mm−1) | 0.64 |
Crystal size (mm) | 0.4 × 0.4 × 0.4 |
Data collection | |
Diffractometer | Enraf-Nonius CAD-4 diffractometer |
Absorption correction | ψ scan (MolEN; Enraf-Nonius, 1990) |
Tmin, Tmax | 0.696, 0.775 |
No. of measured, independent and observed [I > 2σ(I)] reflections | 5012, 3653, 3360 |
Rint | 0.014 |
(sin θ/λ)max (Å−1) | 0.637 |
Refinement | |
R[F2 > 2σ(F2)], wR(F2), S | 0.023, 0.058, 1.04 |
No. of reflections | 3653 |
No. of parameters | 284 |
H-atom treatment | All H-atom parameters refined |
Δρmax, Δρmin (e Å−3) | 0.81, −0.69 |
Computer programs: MolEN, SHELXS86 (Sheldrick, 1985), SHELXL97 (Sheldrick, 1997).