Supporting information
Crystallographic Information File (CIF) https://doi.org/10.1107/S0108768111029259/zb5019sup1.cif | |
Structure factor file (CIF format) https://doi.org/10.1107/S0108768111029259/zb5019finalsup2.hkl | |
Structure factor file (CIF format) https://doi.org/10.1107/S0108768111029259/zb5019combinedsup3.hkl | |
Structure factor file (CIF format) https://doi.org/10.1107/S0108768111029259/zb5019xmas1sup4.hkl | |
Structure factor file (CIF format) https://doi.org/10.1107/S0108768111029259/zb501995srv082sup5.hkl |
CCDC references: 849843; 849844; 849845; 849846
Data collection: Siemens XSCANS for final, combined, xmas1; Siemens SMART for 95srv082. Cell refinement: Siemens XSCANS for final, combined, xmas1; Siemens SMART for 95srv082. Data reduction: Siemens XSCANS for final, combined, xmas1; Siemens SAINT for 95srv082. For all compounds, program(s) used to solve structure: SHELXS86 (Sheldrick, 1990); program(s) used to refine structure: SHELXL93 (Sheldrick, 1993); molecular graphics: SHELXTL-Plus; software used to prepare material for publication: SHELXL93.
C23H22F5O2Ta | Z = 2 |
Mr = 606.36 | F(000) = 588 |
Triclinic, P1 | Dx = 1.941 Mg m−3 |
Hall symbol: p 1 | Mo Kα radiation, λ = 0.71073 Å |
a = 9.239 (2) Å | Cell parameters from 50 reflections |
b = 11.647 (2) Å | θ = 4.7–12.3° |
c = 11.803 (2) Å | µ = 5.36 mm−1 |
α = 117.25 (3)° | T = 150 K |
β = 96.37 (3)° | Irregular block, yellow |
γ = 106.63 (3)° | 0.80 × 0.64 × 0.44 mm |
V = 1037.3 (3) Å3 |
Siemens P4 diffractometer | 2985 reflections with I > 2σ(I) |
Radiation source: fine-focus sealed tube | Rint = 0.145 |
Graphite monochromator | θmax = 25.0°, θmin = 2.1° |
ω scans | h = −1→10 |
Absorption correction: empirical (using intensity measurements) ? | k = −11→11 |
Tmin = 0.261, Tmax = 1.000 | l = −14→14 |
3942 measured reflections | 3 standard reflections every 97 reflections |
3310 independent reflections | intensity decay: none |
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)] = 0.073 | Hydrogen site location: inferred from neighbouring sites |
wR(F2) = 0.182 | H atoms treated by a mixture of independent and constrained refinement |
S = 1.02 | Calculated w = 1/[σ2(Fo2) + (0.1572P)2] where P = (Fo2 + 2Fc2)/3 |
3309 reflections | (Δ/σ)max < 0.001 |
221 parameters | Δρmax = 5.30 e Å−3 |
0 restraints | Δρmin = −3.77 e Å−3 |
C23H22F5O2Ta | γ = 106.63 (3)° |
Mr = 606.36 | V = 1037.3 (3) Å3 |
Triclinic, P1 | Z = 2 |
a = 9.239 (2) Å | Mo Kα radiation |
b = 11.647 (2) Å | µ = 5.36 mm−1 |
c = 11.803 (2) Å | T = 150 K |
α = 117.25 (3)° | 0.80 × 0.64 × 0.44 mm |
β = 96.37 (3)° |
Siemens P4 diffractometer | 2985 reflections with I > 2σ(I) |
Absorption correction: empirical (using intensity measurements) ? | Rint = 0.145 |
Tmin = 0.261, Tmax = 1.000 | 3 standard reflections every 97 reflections |
3942 measured reflections | intensity decay: none |
3310 independent reflections |
R[F2 > 2σ(F2)] = 0.073 | 0 restraints |
wR(F2) = 0.182 | H atoms treated by a mixture of independent and constrained refinement |
S = 1.02 | Δρmax = 5.30 e Å−3 |
3309 reflections | Δρmin = −3.77 e Å−3 |
221 parameters |
Experimental. Empirical absorption program: DIFABS. |
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 on F2 for ALL reflections except for 1 with very negative F2 or flagged by the user for potential systematic errors. Weighted R-factors wR and all goodnesses of fit S are based on F2, conventional R-factors R are based on F, with F set to zero for negative F2. The observed criterion of F2 > σ(F2) is used only for calculating _R_factor_obs 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 | ||
Ta | 0.07331 (4) | 0.14666 (4) | 0.02121 (3) | 0.0227 (3) | |
F2 | 0.0398 (9) | 0.3517 (9) | 0.3795 (7) | 0.043 (2) | |
F3 | 0.1504 (11) | 0.4073 (10) | 0.6275 (8) | 0.053 (2) | |
F4 | 0.4415 (11) | 0.4098 (9) | 0.7073 (7) | 0.051 (2) | |
F5 | 0.6121 (9) | 0.3448 (9) | 0.5299 (8) | 0.047 (2) | |
F6 | 0.5032 (8) | 0.2935 (8) | 0.2836 (7) | 0.037 (2) | |
O1 | 0.2143 (10) | 0.2989 (9) | 0.2031 (8) | 0.031 (2) | |
O2 | 0.0221 (9) | 0.0498 (8) | 0.1188 (7) | 0.026 (2) | |
C1 | 0.2678 (15) | 0.3175 (12) | 0.3217 (10) | 0.029 (3) | |
C2 | 0.1807 (15) | 0.3467 (15) | 0.4138 (14) | 0.039 (3) | |
C3 | 0.2366 (17) | 0.3758 (15) | 0.5418 (13) | 0.044 (4) | |
C4 | 0.3809 (18) | 0.3750 (16) | 0.5798 (12) | 0.043 (4) | |
C5 | 0.4719 (16) | 0.3455 (14) | 0.4918 (12) | 0.036 (3) | |
C6 | 0.4124 (14) | 0.3173 (13) | 0.3641 (11) | 0.029 (3) | |
C7 | 0.2984 (14) | 0.1553 (14) | −0.0272 (11) | 0.032 (3) | |
H7A | 0.3681 | 0.2554 | 0.0214 | 0.039* | |
H7B | 0.3445 | 0.1119 | 0.0144 | 0.039* | |
C8 | 0.3170 (14) | 0.0951 (13) | −0.1647 (11) | 0.029 (3) | |
C9 | 0.4144 (15) | 0.1776 (14) | −0.2021 (12) | 0.032 (3) | |
H9A | 0.4747 (15) | 0.2744 (14) | −0.1376 (12) | 0.039* | |
C10 | 0.4270 (16) | 0.1223 (18) | −0.3333 (14) | 0.047 (4) | |
H10A | 0.4942 (16) | 0.1819 (18) | −0.3574 (14) | 0.056* | |
C11 | 0.3455 (16) | −0.0128 (17) | −0.4242 (12) | 0.043 (3) | |
H11A | 0.3518 (16) | −0.0497 (17) | −0.5140 (12) | 0.051* | |
C12 | 0.2506 (15) | −0.0997 (16) | −0.3875 (12) | 0.039 (3) | |
H12A | 0.1947 (15) | −0.1971 (16) | −0.4522 (12) | 0.046* | |
C13 | 0.2365 (14) | −0.0487 (14) | −0.2611 (12) | 0.034 (3) | |
H13A | 0.1720 (14) | −0.1104 (14) | −0.2377 (12) | 0.040* | |
C14 | 0.1002 (15) | 0.3316 (15) | −0.0438 (12) | 0.0361 (9)* | |
C15 | −0.0041 (15) | 0.1989 (15) | −0.1569 (12) | 0.0361 (9)* | |
C16 | −0.1400 (15) | 0.1532 (15) | −0.1155 (12) | 0.0361 (9)* | |
C17 | −0.1136 (15) | 0.2512 (14) | 0.0187 (12) | 0.0361 (9)* | |
C18 | 0.0309 (15) | 0.3613 (15) | 0.0610 (12) | 0.0361 (9)* | |
C14A | 0.2501 (14) | 0.4282 (14) | −0.0396 (12) | 0.0361 (9)* | |
H14A | 0.2266 (14) | 0.4868 (14) | −0.0693 (12) | 0.043* | |
H14B | 0.3182 (14) | 0.4852 (14) | 0.0497 (12) | 0.043* | |
H14C | 0.3015 (14) | 0.3750 (14) | −0.0968 (12) | 0.043* | |
C15A | 0.0125 (15) | 0.1263 (15) | −0.2925 (12) | 0.0361 (9)* | |
H15A | −0.0240 (15) | 0.1627 (15) | −0.3432 (12) | 0.043* | |
H15B | 0.1212 (15) | 0.1407 (15) | −0.2872 (12) | 0.043* | |
H15C | −0.0491 (15) | 0.0281 (15) | −0.3350 (12) | 0.043* | |
C16A | −0.2844 (15) | 0.0233 (15) | −0.2066 (12) | 0.0361 (9)* | |
H16A | −0.3553 (15) | 0.0450 (15) | −0.2521 (12) | 0.043* | |
H16B | −0.2544 (15) | −0.0467 (15) | −0.2704 (12) | 0.043* | |
H16C | −0.3356 (15) | −0.0111 (15) | −0.1557 (12) | 0.043* | |
C17A | −0.2362 (15) | 0.2485 (15) | 0.0926 (12) | 0.0361 (9)* | |
H17A | −0.2988 (15) | 0.2964 (15) | 0.0784 (12) | 0.043* | |
H17B | −0.3029 (15) | 0.1535 (15) | 0.0606 (12) | 0.043* | |
H17C | −0.1852 (15) | 0.2943 (15) | 0.1858 (12) | 0.043* | |
C18A | 0.1005 (15) | 0.4993 (14) | 0.1920 (12) | 0.0361 (9)* | |
H18A | 0.0674 (15) | 0.5666 (14) | 0.1834 (12) | 0.043* | |
H18B | 0.0650 (15) | 0.4869 (14) | 0.2605 (12) | 0.043* | |
H18C | 0.2133 (15) | 0.5318 (14) | 0.2147 (12) | 0.043* |
U11 | U22 | U33 | U12 | U13 | U23 | |
Ta | 0.0252 (3) | 0.0181 (4) | 0.0243 (3) | 0.0069 (2) | 0.0030 (2) | 0.0122 (2) |
F2 | 0.038 (4) | 0.043 (5) | 0.048 (4) | 0.015 (4) | 0.012 (3) | 0.024 (4) |
F3 | 0.066 (5) | 0.055 (6) | 0.042 (4) | 0.026 (4) | 0.029 (4) | 0.022 (4) |
F4 | 0.071 (6) | 0.042 (5) | 0.033 (4) | 0.011 (4) | 0.002 (4) | 0.023 (4) |
F5 | 0.044 (4) | 0.042 (5) | 0.050 (4) | 0.016 (4) | −0.003 (4) | 0.024 (4) |
F6 | 0.036 (4) | 0.033 (4) | 0.034 (4) | 0.011 (3) | 0.008 (3) | 0.015 (3) |
O1 | 0.035 (4) | 0.021 (4) | 0.032 (4) | 0.006 (4) | 0.000 (3) | 0.013 (4) |
O2 | 0.033 (4) | 0.020 (4) | 0.027 (4) | 0.007 (3) | 0.004 (3) | 0.017 (3) |
C1 | 0.048 (7) | 0.009 (6) | 0.025 (5) | 0.003 (5) | 0.002 (5) | 0.009 (5) |
C2 | 0.035 (7) | 0.024 (7) | 0.043 (7) | 0.005 (5) | 0.007 (5) | 0.010 (6) |
C3 | 0.056 (8) | 0.032 (8) | 0.036 (7) | 0.003 (6) | 0.011 (6) | 0.020 (6) |
C4 | 0.059 (9) | 0.035 (8) | 0.026 (6) | 0.003 (7) | −0.001 (6) | 0.020 (6) |
C5 | 0.039 (6) | 0.029 (7) | 0.038 (6) | 0.008 (5) | 0.003 (5) | 0.020 (6) |
C6 | 0.039 (6) | 0.017 (6) | 0.026 (5) | 0.004 (5) | 0.001 (5) | 0.012 (5) |
C7 | 0.033 (6) | 0.034 (7) | 0.030 (6) | 0.010 (5) | 0.004 (4) | 0.020 (5) |
C8 | 0.033 (6) | 0.023 (6) | 0.029 (5) | 0.013 (5) | 0.005 (4) | 0.012 (5) |
C9 | 0.040 (6) | 0.025 (7) | 0.040 (6) | 0.013 (5) | 0.014 (5) | 0.022 (6) |
C10 | 0.038 (7) | 0.069 (11) | 0.051 (8) | 0.022 (7) | 0.016 (6) | 0.043 (8) |
C11 | 0.040 (7) | 0.061 (10) | 0.033 (6) | 0.027 (7) | 0.012 (5) | 0.024 (7) |
C12 | 0.034 (6) | 0.042 (8) | 0.038 (6) | 0.016 (6) | 0.012 (5) | 0.018 (6) |
C13 | 0.033 (6) | 0.036 (8) | 0.038 (6) | 0.015 (6) | 0.009 (5) | 0.022 (6) |
Ta—O2i | 1.950 (8) | C10—H10A | 0.96 |
Ta—O2 | 1.957 (7) | C11—C12 | 1.40 (2) |
Ta—O1 | 2.005 (8) | C11—H11A | 0.96 |
Ta—C7 | 2.204 (12) | C12—C13 | 1.37 (2) |
Ta—C17 | 2.385 (14) | C12—H12A | 0.96 |
Ta—C16 | 2.446 (13) | C13—H13A | 0.96 |
Ta—C18 | 2.480 (15) | C14—C18 | 1.40 (2) |
Ta—C15 | 2.528 (13) | C14—C15 | 1.44 (2) |
Ta—C14 | 2.558 (14) | C14—C14A | 1.49 (2) |
Ta—Tai | 3.0644 (13) | C15—C16 | 1.45 (2) |
F2—C2 | 1.35 (2) | C15—C15A | 1.48 (2) |
F3—C3 | 1.34 (2) | C16—C17 | 1.40 (2) |
F4—C4 | 1.367 (14) | C16—C16A | 1.50 (2) |
F5—C5 | 1.33 (2) | C17—C18 | 1.40 (2) |
F6—C6 | 1.324 (15) | C17—C17A | 1.51 (2) |
O1—C1 | 1.326 (13) | C18—C18A | 1.52 (2) |
O2—Tai | 1.950 (8) | C14A—H14A | 0.96 |
C1—C6 | 1.37 (2) | C14A—H14B | 0.96 |
C1—C2 | 1.40 (2) | C14A—H14C | 0.96 |
C2—C3 | 1.39 (2) | C15A—H15A | 0.96 |
C3—C4 | 1.36 (2) | C15A—H15B | 0.96 |
C4—C5 | 1.39 (2) | C15A—H15C | 0.96 |
C5—C6 | 1.39 (2) | C16A—H16A | 0.96 |
C7—C8 | 1.50 (2) | C16A—H16B | 0.96 |
C7—H7A | 0.990 (13) | C16A—H16C | 0.96 |
C7—H7B | 0.990 (13) | C17A—H17A | 0.96 |
C8—C9 | 1.38 (2) | C17A—H17B | 0.96 |
C8—C13 | 1.42 (2) | C17A—H17C | 0.96 |
C9—C10 | 1.41 (2) | C18A—H18A | 0.96 |
C9—H9A | 0.96 | C18A—H18B | 0.96 |
C10—C11 | 1.34 (2) | C18A—H18C | 0.96 |
O2i—Ta—O2 | 76.7 (3) | C8—C9—H9A | 119.4 (7) |
O2i—Ta—O1 | 150.8 (4) | C10—C9—H9A | 119.3 (9) |
O2—Ta—O1 | 80.7 (3) | C11—C10—C9 | 120.2 (13) |
O2i—Ta—C7 | 89.1 (4) | C11—C10—H10A | 119.9 (8) |
O2—Ta—C7 | 113.4 (4) | C9—C10—H10A | 119.9 (9) |
O1—Ta—C7 | 83.2 (4) | C10—C11—C12 | 119.5 (12) |
O2i—Ta—C17 | 108.4 (4) | C10—C11—H11A | 120.2 (8) |
O2—Ta—C17 | 107.7 (4) | C12—C11—H11A | 120.3 (8) |
O1—Ta—C17 | 95.9 (4) | C13—C12—C11 | 121.3 (13) |
C7—Ta—C17 | 138.1 (5) | C13—C12—H12A | 119.3 (8) |
O2i—Ta—C16 | 80.3 (4) | C11—C12—H12A | 119.3 (8) |
O2—Ta—C16 | 119.3 (4) | C12—C13—C8 | 120.1 (12) |
O1—Ta—C16 | 127.5 (4) | C12—C13—H13A | 120.0 (8) |
C7—Ta—C16 | 121.5 (4) | C8—C13—H13A | 119.9 (7) |
C17—Ta—C16 | 33.7 (4) | C18—C14—C15 | 108.3 (11) |
O2i—Ta—C18 | 135.0 (4) | C18—C14—C14A | 124.9 (12) |
O2—Ta—C18 | 126.5 (4) | C15—C14—C14A | 126.6 (11) |
O1—Ta—C18 | 73.8 (4) | C18—C14—Ta | 70.8 (8) |
C7—Ta—C18 | 109.3 (5) | C15—C14—Ta | 72.4 (8) |
C17—Ta—C18 | 33.4 (4) | C14A—C14—Ta | 126.3 (9) |
C16—Ta—C18 | 54.9 (4) | C14—C15—C16 | 105.7 (11) |
O2i—Ta—C15 | 86.3 (4) | C14—C15—C15A | 128.8 (12) |
O2—Ta—C15 | 151.5 (4) | C16—C15—C15A | 125.3 (12) |
O1—Ta—C15 | 121.5 (4) | C14—C15—Ta | 74.7 (7) |
C7—Ta—C15 | 88.7 (4) | C16—C15—Ta | 70.0 (7) |
C17—Ta—C15 | 56.1 (4) | C15A—C15—Ta | 123.8 (10) |
C16—Ta—C15 | 33.7 (4) | C17—C16—C15 | 108.6 (11) |
C18—Ta—C15 | 54.8 (4) | C17—C16—C16A | 127.7 (11) |
O2i—Ta—C14 | 118.5 (4) | C15—C16—C16A | 123.7 (11) |
O2—Ta—C14 | 158.8 (4) | C17—C16—Ta | 70.7 (7) |
O1—Ta—C14 | 88.6 (4) | C15—C16—Ta | 76.2 (8) |
C7—Ta—C14 | 83.2 (5) | C16A—C16—Ta | 120.6 (10) |
C17—Ta—C14 | 54.9 (4) | C18—C17—C16 | 108.2 (11) |
C16—Ta—C14 | 54.7 (4) | C18—C17—C17A | 126.7 (12) |
C18—Ta—C14 | 32.3 (4) | C16—C17—C17A | 124.1 (11) |
C15—Ta—C14 | 32.9 (4) | C18—C17—Ta | 77.0 (8) |
O2i—Ta—Tai | 38.4 (2) | C16—C17—Ta | 75.5 (8) |
O2—Ta—Tai | 38.3 (2) | C17A—C17—Ta | 122.9 (9) |
O1—Ta—Tai | 116.9 (3) | C17—C18—C14 | 109.1 (11) |
C7—Ta—Tai | 104.1 (4) | C17—C18—C18A | 127.8 (11) |
C17—Ta—Tai | 113.3 (3) | C14—C18—C18A | 122.8 (12) |
C16—Ta—Tai | 101.8 (3) | C17—C18—Ta | 69.6 (8) |
C18—Ta—Tai | 146.0 (3) | C14—C18—Ta | 76.9 (9) |
C15—Ta—Tai | 121.3 (3) | C18A—C18—Ta | 124.5 (9) |
C14—Ta—Tai | 154.0 (3) | C14—C14A—H14A | 109.1 (8) |
C1—O1—Ta | 139.8 (8) | C14—C14A—H14B | 109.6 (7) |
Tai—O2—Ta | 103.3 (3) | H14A—C14A—H14B | 109.5 |
O1—C1—C6 | 123.0 (12) | C14—C14A—H14C | 109.7 (8) |
O1—C1—C2 | 120.4 (12) | H14A—C14A—H14C | 109.5 |
C6—C1—C2 | 116.4 (11) | H14B—C14A—H14C | 109.5 |
F2—C2—C3 | 118.3 (13) | C15—C15A—H15A | 109.6 (8) |
F2—C2—C1 | 119.3 (12) | C15—C15A—H15B | 109.5 (7) |
C3—C2—C1 | 122.4 (13) | H15A—C15A—H15B | 109.5 |
F3—C3—C4 | 120.8 (12) | C15—C15A—H15C | 109.4 (8) |
F3—C3—C2 | 119.9 (14) | H15A—C15A—H15C | 109.5 |
C4—C3—C2 | 119.3 (13) | H15B—C15A—H15C | 109.5 |
C3—C4—F4 | 120.2 (14) | C16—C16A—H16A | 109.3 (8) |
C3—C4—C5 | 120.7 (12) | C16—C16A—H16B | 109.5 (7) |
F4—C4—C5 | 118.9 (14) | H16A—C16A—H16B | 109.5 |
F5—C5—C4 | 120.2 (12) | C16—C16A—H16C | 109.6 (7) |
F5—C5—C6 | 121.3 (12) | H16A—C16A—H16C | 109.5 |
C4—C5—C6 | 118.5 (13) | H16B—C16A—H16C | 109.5 |
F6—C6—C1 | 120.0 (10) | C17—C17A—H17A | 109.3 (8) |
F6—C6—C5 | 117.3 (11) | C17—C17A—H17B | 109.7 (8) |
C1—C6—C5 | 122.7 (12) | H17A—C17A—H17B | 109.5 |
C8—C7—Ta | 125.2 (8) | C17—C17A—H17C | 109.4 (7) |
C8—C7—H7A | 106.0 (10) | H17A—C17A—H17C | 109.5 |
Ta—C7—H7A | 106.0 (9) | H17B—C17A—H17C | 109.5 |
C8—C7—H7B | 106.0 (12) | C18—C18A—H18A | 109.4 (7) |
Ta—C7—H7B | 106.0 (8) | C18—C18A—H18B | 109.7 (7) |
H7A—C7—H7B | 106.3 (10) | H18A—C18A—H18B | 109.5 |
C9—C8—C13 | 117.4 (11) | C18—C18A—H18C | 109.3 (7) |
C9—C8—C7 | 121.2 (11) | H18A—C18A—H18C | 109.5 |
C13—C8—C7 | 121.3 (11) | H18B—C18A—H18C | 109.5 |
C8—C9—C10 | 121.3 (12) |
Symmetry code: (i) −x, −y, −z. |
C24H46NTa | F(000) = 1080 |
Mr = 529.57 | Dx = 1.436 Mg m−3 |
Monoclinic, P21/c | Mo Kα radiation, λ = 0.71073 Å |
Hall symbol: -p 2ybc | Cell parameters from 32 reflections |
a = 9.083 (2) Å | θ = 12.4–12.5° |
b = 16.216 (3) Å | µ = 4.50 mm−1 |
c = 16.872 (3) Å | T = 150 K |
β = 99.76 (3)° | Cube, yellow |
V = 2449.1 (8) Å3 | 0.26 × 0.24 × 0.20 mm |
Z = 4 |
Siemens P4 diffractometer | 7822 reflections with I > 2σ(I) |
Radiation source: fine-focus sealed tube | Rint = 0.030 |
Graphite monochromator | θmax = 35.0°, θmin = 2.3° |
2τ/ω scans | h = −1→14 |
Absorption correction: empirical (using intensity measurements) ? | k = −1→26 |
Tmin = 0.267, Tmax = 0.365 | l = −85→27 |
13104 measured reflections | 3 standard reflections every 97 reflections |
10777 independent reflections | intensity decay: none |
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)] = 0.038 | Hydrogen site location: inferred from neighbouring sites |
wR(F2) = 0.064 | H atoms treated by a mixture of independent and constrained refinement |
S = 1.03 | w = 1/[σ2(Fo2) + (0.0192P)2 + 0.0105P] where P = (Fo2 + 2Fc2)/3 |
10777 reflections | (Δ/σ)max = 0.001 |
247 parameters | Δρmax = 1.10 e Å−3 |
0 restraints | Δρmin = −0.79 e Å−3 |
C24H46NTa | V = 2449.1 (8) Å3 |
Mr = 529.57 | Z = 4 |
Monoclinic, P21/c | Mo Kα radiation |
a = 9.083 (2) Å | µ = 4.50 mm−1 |
b = 16.216 (3) Å | T = 150 K |
c = 16.872 (3) Å | 0.26 × 0.24 × 0.20 mm |
β = 99.76 (3)° |
Siemens P4 diffractometer | 7822 reflections with I > 2σ(I) |
Absorption correction: empirical (using intensity measurements) ? | Rint = 0.030 |
Tmin = 0.267, Tmax = 0.365 | 3 standard reflections every 97 reflections |
13104 measured reflections | intensity decay: none |
10777 independent reflections |
R[F2 > 2σ(F2)] = 0.038 | 0 restraints |
wR(F2) = 0.064 | H atoms treated by a mixture of independent and constrained refinement |
S = 1.03 | Δρmax = 1.10 e Å−3 |
10777 reflections | Δρmin = −0.79 e Å−3 |
247 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 on F2 for ALL reflections except for 3 with very negative F2 or flagged by the user for potential systematic errors. Weighted R-factors wR and all goodnesses of fit S are based on F2, conventional R-factors R are based on F, with F set to zero for negative F2. The observed criterion of F2 > σ(F2) is used only for calculating _R_factor_obs 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 | ||
Ta1 | 0.146374 (13) | 0.241189 (6) | 0.429226 (7) | 0.01498 (3) | |
N1 | 0.3194 (2) | 0.24441 (15) | 0.49784 (13) | 0.0180 (4) | |
C11 | 0.1719 (4) | 0.33799 (19) | 0.3413 (2) | 0.0216 (6) | |
H11A | 0.071 (4) | 0.353 (2) | 0.312 (2) | 0.026* | |
H11B | 0.210 (4) | 0.295 (2) | 0.307 (2) | 0.026* | |
C16 | 0.1583 (4) | 0.12800 (19) | 0.3578 (2) | 0.0233 (6) | |
H16A | 0.098 (4) | 0.088 (2) | 0.372 (2) | 0.028* | |
H16B | 0.094 (4) | 0.146 (2) | 0.306 (2) | 0.028* | |
C1 | −0.1038 (4) | 0.17678 (18) | 0.4379 (2) | 0.0214 (6) | |
C2 | −0.1378 (3) | 0.24885 (19) | 0.39201 (17) | 0.0220 (5) | |
C3 | −0.0886 (4) | 0.31756 (18) | 0.4410 (2) | 0.0203 (6) | |
C4 | −0.0203 (4) | 0.28812 (18) | 0.51792 (18) | 0.0189 (6) | |
C5 | −0.0289 (4) | 0.20026 (18) | 0.5159 (2) | 0.0207 (6) | |
C6 | −0.1573 (4) | 0.0910 (2) | 0.4152 (2) | 0.0309 (8) | |
H6A | −0.2576 | 0.0844 | 0.4253 | 0.046* | |
H6B | −0.0932 | 0.0518 | 0.4467 | 0.046* | |
H6C | −0.1554 | 0.0819 | 0.3591 | 0.046* | |
C7 | −0.2176 (4) | 0.2526 (2) | 0.30631 (19) | 0.0324 (7) | |
H7A | −0.3234 | 0.2553 | 0.3055 | 0.049* | |
H7B | −0.1944 | 0.2042 | 0.2781 | 0.049* | |
H7C | −0.1859 | 0.3007 | 0.2807 | 0.049* | |
C8 | −0.1257 (4) | 0.40565 (19) | 0.4198 (2) | 0.0286 (7) | |
H8A | −0.2237 | 0.4181 | 0.4307 | 0.043* | |
H8B | −0.1234 | 0.4143 | 0.3638 | 0.043* | |
H8C | −0.0539 | 0.4410 | 0.4515 | 0.043* | |
C9 | 0.0322 (4) | 0.3397 (2) | 0.5906 (2) | 0.0296 (8) | |
H9A | −0.0506 | 0.3517 | 0.6174 | 0.044* | |
H9B | 0.0733 | 0.3904 | 0.5746 | 0.044* | |
H9C | 0.1074 | 0.3103 | 0.6265 | 0.044* | |
C10 | 0.0123 (4) | 0.1426 (2) | 0.5862 (2) | 0.0284 (7) | |
H10A | −0.0726 | 0.1346 | 0.6123 | 0.043* | |
H10B | 0.0928 | 0.1660 | 0.6237 | 0.043* | |
H10C | 0.0431 | 0.0905 | 0.5675 | 0.043* | |
C12 | 0.2765 (4) | 0.41433 (19) | 0.3516 (2) | 0.0220 (6) | |
C13 | 0.4401 (4) | 0.3875 (2) | 0.3630 (2) | 0.0289 (7) | |
H13A | 0.5032 | 0.4353 | 0.3693 | 0.043* | |
H13B | 0.4572 | 0.3567 | 0.3168 | 0.043* | |
H13C | 0.4625 | 0.3535 | 0.4101 | 0.043* | |
C14 | 0.2440 (5) | 0.4678 (2) | 0.2756 (2) | 0.0351 (9) | |
H14A | 0.3085 | 0.5151 | 0.2817 | 0.053* | |
H14B | 0.1418 | 0.4856 | 0.2674 | 0.053* | |
H14C | 0.2615 | 0.4361 | 0.2300 | 0.053* | |
C15 | 0.2503 (4) | 0.4662 (2) | 0.4235 (2) | 0.0307 (7) | |
H15A | 0.3159 | 0.5130 | 0.4289 | 0.046* | |
H15B | 0.2701 | 0.4334 | 0.4715 | 0.046* | |
H15C | 0.1485 | 0.4847 | 0.4153 | 0.046* | |
C17 | 0.3004 (4) | 0.08473 (18) | 0.3418 (2) | 0.0210 (6) | |
C18 | 0.3708 (5) | 0.0383 (2) | 0.4175 (2) | 0.0331 (8) | |
H18A | 0.3968 | 0.0767 | 0.4609 | 0.050* | |
H18B | 0.4591 | 0.0103 | 0.4077 | 0.050* | |
H18C | 0.3008 | −0.0013 | 0.4314 | 0.050* | |
C19 | 0.2602 (5) | 0.0218 (2) | 0.2731 (2) | 0.0329 (8) | |
H19A | 0.3493 | −0.0052 | 0.2633 | 0.049* | |
H19B | 0.2138 | 0.0499 | 0.2252 | 0.049* | |
H19C | 0.1923 | −0.0184 | 0.2881 | 0.049* | |
C20 | 0.4124 (4) | 0.1464 (2) | 0.3179 (2) | 0.0311 (7) | |
H20A | 0.4386 | 0.1860 | 0.3602 | 0.047* | |
H20B | 0.3684 | 0.1743 | 0.2694 | 0.047* | |
H20C | 0.5005 | 0.1176 | 0.3090 | 0.047* | |
C21 | 0.4452 (3) | 0.2476 (2) | 0.56384 (16) | 0.0228 (6) | |
C22 | 0.5898 (4) | 0.2210 (2) | 0.5342 (2) | 0.0321 (8) | |
H22A | 0.6089 | 0.2577 | 0.4925 | 0.048* | |
H22B | 0.5784 | 0.1658 | 0.5135 | 0.048* | |
H22D | 0.6720 | 0.2229 | 0.5782 | 0.048* | |
C23 | 0.4173 (4) | 0.1880 (2) | 0.6303 (2) | 0.0302 (7) | |
H23A | 0.3276 | 0.2036 | 0.6494 | 0.045* | |
H23D | 0.5002 | 0.1900 | 0.6739 | 0.045* | |
H23B | 0.4068 | 0.1329 | 0.6092 | 0.045* | |
C24 | 0.4657 (4) | 0.3353 (2) | 0.5971 (2) | 0.0316 (7) | |
H24D | 0.3764 | 0.3525 | 0.6157 | 0.047* | |
H24A | 0.4855 | 0.3719 | 0.5555 | 0.047* | |
H24B | 0.5481 | 0.3365 | 0.6410 | 0.047* |
U11 | U22 | U33 | U12 | U13 | U23 | |
Ta1 | 0.01440 (4) | 0.01465 (4) | 0.01567 (4) | 0.00049 (5) | 0.00195 (3) | −0.00093 (5) |
N1 | 0.0168 (9) | 0.0187 (11) | 0.0187 (10) | 0.0002 (9) | 0.0036 (8) | 0.0004 (9) |
C11 | 0.0217 (15) | 0.0211 (13) | 0.0217 (15) | −0.0010 (11) | 0.0028 (12) | −0.0004 (11) |
C16 | 0.0198 (15) | 0.0210 (14) | 0.0287 (17) | 0.0013 (12) | 0.0029 (13) | −0.0055 (12) |
C1 | 0.0183 (15) | 0.0195 (13) | 0.0270 (17) | −0.0012 (11) | 0.0052 (13) | −0.0040 (11) |
C2 | 0.0133 (10) | 0.0275 (15) | 0.0241 (12) | 0.0004 (12) | 0.0006 (9) | −0.0012 (12) |
C3 | 0.0141 (14) | 0.0198 (13) | 0.0275 (17) | 0.0042 (10) | 0.0049 (12) | 0.0004 (11) |
C4 | 0.0170 (14) | 0.0198 (12) | 0.0200 (14) | 0.0026 (10) | 0.0032 (12) | −0.0012 (10) |
C5 | 0.0190 (15) | 0.0185 (13) | 0.0253 (16) | 0.0005 (11) | 0.0057 (13) | 0.0037 (11) |
C6 | 0.0269 (18) | 0.0226 (15) | 0.044 (2) | −0.0059 (13) | 0.0093 (16) | −0.0097 (14) |
C7 | 0.0228 (14) | 0.048 (2) | 0.0244 (13) | −0.0024 (17) | −0.0025 (11) | 0.0005 (16) |
C8 | 0.0250 (18) | 0.0227 (15) | 0.038 (2) | 0.0058 (13) | 0.0061 (15) | 0.0035 (13) |
C9 | 0.0306 (19) | 0.0294 (17) | 0.0294 (19) | 0.0046 (14) | 0.0068 (15) | −0.0090 (13) |
C10 | 0.0270 (18) | 0.0296 (16) | 0.0288 (18) | −0.0011 (13) | 0.0053 (15) | 0.0105 (13) |
C12 | 0.0223 (16) | 0.0224 (14) | 0.0220 (15) | −0.0009 (11) | 0.0059 (13) | 0.0031 (11) |
C13 | 0.0238 (16) | 0.0319 (17) | 0.0315 (18) | −0.0019 (13) | 0.0059 (14) | 0.0021 (14) |
C14 | 0.039 (2) | 0.0292 (17) | 0.038 (2) | −0.0023 (15) | 0.0080 (19) | 0.0114 (15) |
C15 | 0.0328 (19) | 0.0270 (16) | 0.0335 (19) | −0.0060 (14) | 0.0092 (16) | −0.0043 (13) |
C17 | 0.0243 (16) | 0.0187 (13) | 0.0205 (15) | 0.0030 (11) | 0.0054 (13) | −0.0007 (10) |
C18 | 0.041 (2) | 0.0264 (16) | 0.0306 (18) | 0.0079 (15) | 0.0021 (16) | 0.0043 (13) |
C19 | 0.040 (2) | 0.0284 (17) | 0.030 (2) | 0.0045 (15) | 0.0049 (17) | −0.0098 (14) |
C20 | 0.0330 (19) | 0.0306 (17) | 0.0326 (19) | 0.0000 (15) | 0.0136 (16) | −0.0022 (14) |
C21 | 0.0195 (12) | 0.0315 (16) | 0.0170 (11) | −0.0033 (13) | 0.0016 (9) | −0.0002 (12) |
C22 | 0.0194 (14) | 0.046 (2) | 0.0295 (16) | 0.0045 (14) | 0.0002 (13) | 0.0028 (15) |
C23 | 0.0282 (17) | 0.0379 (18) | 0.0227 (15) | −0.0009 (15) | −0.0010 (14) | 0.0053 (13) |
C24 | 0.0289 (18) | 0.0355 (18) | 0.0278 (17) | −0.0079 (15) | −0.0025 (15) | −0.0038 (14) |
Ta1—N1 | 1.788 (2) | C10—H10A | 0.9600 |
Ta1—C11 | 2.199 (3) | C10—H10B | 0.9600 |
Ta1—C16 | 2.208 (3) | C10—H10C | 0.9600 |
Ta1—H11B | 2.40 (3) | C12—C13 | 1.529 (5) |
Ta1—C4 | 2.425 (3) | C12—C15 | 1.527 (5) |
Ta1—C5 | 2.429 (3) | C12—C14 | 1.534 (5) |
Ta1—C3 | 2.504 (3) | C13—H13A | 0.9600 |
Ta1—C1 | 2.527 (3) | C13—H13B | 0.9600 |
Ta1—C2 | 2.554 (3) | C13—H13C | 0.9600 |
Ta1—H16B | 2.57 (4) | C14—H14A | 0.9600 |
N1—C21 | 1.455 (3) | C14—H14B | 0.9600 |
C11—C12 | 1.552 (4) | C14—H14C | 0.9600 |
C11—H11A | 0.99 (4) | C15—H15A | 0.9600 |
C11—H11B | 1.01 (4) | C15—H15B | 0.9600 |
C16—C17 | 1.533 (5) | C15—H15C | 0.9600 |
C16—H16A | 0.91 (4) | C17—C18 | 1.526 (5) |
C16—H16B | 1.01 (4) | C17—C20 | 1.529 (5) |
C1—C2 | 1.407 (4) | C17—C19 | 1.541 (5) |
C1—C5 | 1.427 (5) | C18—H18A | 0.9600 |
C1—C6 | 1.502 (4) | C18—H18B | 0.9600 |
C2—C3 | 1.414 (4) | C18—H18C | 0.9600 |
C2—C7 | 1.505 (4) | C19—H19A | 0.9600 |
C3—C4 | 1.422 (4) | C19—H19B | 0.9600 |
C3—C8 | 1.497 (4) | C19—H19C | 0.9600 |
C4—C5 | 1.427 (4) | C20—H20A | 0.9600 |
C4—C9 | 1.495 (4) | C20—H20B | 0.9600 |
C5—C10 | 1.508 (4) | C20—H20C | 0.9600 |
C6—H6A | 0.9600 | C21—C24 | 1.528 (4) |
C6—H6B | 0.9600 | C21—C23 | 1.534 (4) |
C6—H6C | 0.9600 | C21—C22 | 1.544 (4) |
C7—H7A | 0.9600 | C22—H22A | 0.9600 |
C7—H7B | 0.9600 | C22—H22B | 0.9600 |
C7—H7C | 0.9600 | C22—H22D | 0.9600 |
C8—H8A | 0.9600 | C23—H23A | 0.9600 |
C8—H8B | 0.9600 | C23—H23D | 0.9600 |
C8—H8C | 0.9600 | C23—H23B | 0.9600 |
C9—H9A | 0.9600 | C24—H24D | 0.9600 |
C9—H9B | 0.9600 | C24—H24A | 0.9600 |
C9—H9C | 0.9600 | C24—H24B | 0.9600 |
N1—Ta1—C11 | 103.55 (12) | C2—C7—H7B | 109.5 |
N1—Ta1—C16 | 104.98 (12) | H7A—C7—H7B | 109.5 |
C11—Ta1—C16 | 101.82 (13) | C2—C7—H7C | 109.5 |
N1—Ta1—H11B | 103.4 (9) | H7A—C7—H7C | 109.5 |
C11—Ta1—H11B | 24.7 (9) | H7B—C7—H7C | 109.5 |
C16—Ta1—H11B | 78.0 (9) | C3—C8—H8A | 109.5 |
N1—Ta1—C4 | 99.41 (10) | C3—C8—H8B | 109.5 |
C11—Ta1—C4 | 109.91 (11) | H8A—C8—H8B | 109.5 |
C16—Ta1—C4 | 133.72 (12) | C3—C8—H8C | 109.5 |
H11B—Ta1—C4 | 133.1 (9) | H8A—C8—H8C | 109.5 |
N1—Ta1—C5 | 102.24 (11) | H8B—C8—H8C | 109.5 |
C11—Ta1—C5 | 139.10 (12) | C4—C9—H9A | 109.5 |
C16—Ta1—C5 | 101.48 (12) | C4—C9—H9B | 109.5 |
H11B—Ta1—C5 | 153.5 (9) | H9A—C9—H9B | 109.5 |
C4—Ta1—C5 | 34.20 (9) | C4—C9—H9C | 109.5 |
N1—Ta1—C3 | 126.98 (11) | H9A—C9—H9C | 109.5 |
C11—Ta1—C3 | 83.64 (12) | H9B—C9—H9C | 109.5 |
C16—Ta1—C3 | 125.15 (12) | C5—C10—H10A | 109.5 |
H11B—Ta1—C3 | 102.8 (9) | C5—C10—H10B | 109.5 |
C4—Ta1—C3 | 33.49 (10) | H10A—C10—H10B | 109.5 |
C5—Ta1—C3 | 55.47 (10) | C5—C10—H10C | 109.5 |
N1—Ta1—C1 | 132.46 (11) | H10A—C10—H10C | 109.5 |
C11—Ta1—C1 | 122.18 (12) | H10B—C10—H10C | 109.5 |
C16—Ta1—C1 | 79.38 (11) | C13—C12—C15 | 109.6 (3) |
H11B—Ta1—C1 | 123.4 (9) | C13—C12—C14 | 108.1 (3) |
C4—Ta1—C1 | 55.43 (10) | C15—C12—C14 | 108.6 (3) |
C5—Ta1—C1 | 33.40 (11) | C13—C12—C11 | 110.5 (3) |
C3—Ta1—C1 | 54.07 (10) | C15—C12—C11 | 110.7 (3) |
N1—Ta1—C2 | 153.98 (9) | C14—C12—C11 | 109.3 (3) |
C11—Ta1—C2 | 90.99 (11) | C12—C13—H13A | 109.5 |
C16—Ta1—C2 | 92.72 (11) | C12—C13—H13B | 109.5 |
H11B—Ta1—C2 | 98.7 (9) | H13A—C13—H13B | 109.5 |
C4—Ta1—C2 | 54.95 (10) | C12—C13—H13C | 109.5 |
C5—Ta1—C2 | 54.77 (10) | H13A—C13—H13C | 109.5 |
C3—Ta1—C2 | 32.45 (10) | H13B—C13—H13C | 109.5 |
C1—Ta1—C2 | 32.13 (10) | C12—C14—H14A | 109.5 |
N1—Ta1—H16B | 124.2 (9) | C12—C14—H14B | 109.5 |
C11—Ta1—H16B | 84.7 (8) | H14A—C14—H14B | 109.5 |
C16—Ta1—H16B | 22.8 (9) | C12—C14—H14C | 109.5 |
H11B—Ta1—H16B | 63.9 (12) | H14A—C14—H14C | 109.5 |
C4—Ta1—H16B | 129.8 (9) | H14B—C14—H14C | 109.5 |
C5—Ta1—H16B | 105.9 (9) | C12—C15—H15A | 109.5 |
C3—Ta1—H16B | 108.6 (9) | C12—C15—H15B | 109.5 |
C1—Ta1—H16B | 75.8 (9) | H15A—C15—H15B | 109.5 |
C2—Ta1—H16B | 77.9 (9) | C12—C15—H15C | 109.5 |
C21—N1—Ta1 | 170.68 (19) | H15A—C15—H15C | 109.5 |
C12—C11—Ta1 | 128.8 (2) | H15B—C15—H15C | 109.5 |
C12—C11—H11A | 111 (2) | C18—C17—C20 | 109.9 (3) |
Ta1—C11—H11A | 108 (2) | C18—C17—C16 | 108.9 (3) |
C12—C11—H11B | 110 (2) | C20—C17—C16 | 111.4 (3) |
Ta1—C11—H11B | 89 (2) | C18—C17—C19 | 108.4 (3) |
H11A—C11—H11B | 105 (3) | C20—C17—C19 | 108.6 (3) |
C17—C16—Ta1 | 126.7 (2) | C16—C17—C19 | 109.7 (3) |
C17—C16—H16A | 107 (2) | C17—C18—H18A | 109.5 |
Ta1—C16—H16A | 111 (2) | C17—C18—H18B | 109.5 |
C17—C16—H16B | 111 (2) | H18A—C18—H18B | 109.5 |
Ta1—C16—H16B | 99 (2) | C17—C18—H18C | 109.5 |
H16A—C16—H16B | 99 (3) | H18A—C18—H18C | 109.5 |
C2—C1—C5 | 108.1 (3) | H18B—C18—H18C | 109.5 |
C2—C1—C6 | 126.8 (3) | C17—C19—H19A | 109.5 |
C5—C1—C6 | 124.4 (3) | C17—C19—H19B | 109.5 |
C2—C1—Ta1 | 74.98 (17) | H19A—C19—H19B | 109.5 |
C5—C1—Ta1 | 69.50 (18) | C17—C19—H19C | 109.5 |
C6—C1—Ta1 | 128.6 (2) | H19A—C19—H19C | 109.5 |
C1—C2—C3 | 108.4 (2) | H19B—C19—H19C | 109.5 |
C1—C2—C7 | 126.0 (3) | C17—C20—H20A | 109.5 |
C3—C2—C7 | 125.7 (3) | C17—C20—H20B | 109.5 |
C1—C2—Ta1 | 72.89 (18) | H20A—C20—H20B | 109.5 |
C3—C2—Ta1 | 71.83 (17) | C17—C20—H20C | 109.5 |
C7—C2—Ta1 | 122.70 (19) | H20A—C20—H20C | 109.5 |
C2—C3—C4 | 108.3 (3) | H20B—C20—H20C | 109.5 |
C2—C3—C8 | 125.2 (3) | N1—C21—C24 | 110.2 (3) |
C4—C3—C8 | 125.7 (3) | N1—C21—C23 | 109.3 (2) |
C2—C3—Ta1 | 75.72 (16) | C24—C21—C23 | 110.1 (3) |
C4—C3—Ta1 | 70.19 (17) | N1—C21—C22 | 110.1 (2) |
C8—C3—Ta1 | 127.9 (2) | C24—C21—C22 | 108.8 (3) |
C3—C4—C5 | 107.4 (3) | C23—C21—C22 | 108.4 (3) |
C3—C4—C9 | 126.2 (3) | C21—C22—H22A | 109.5 |
C5—C4—C9 | 126.0 (3) | C21—C22—H22B | 109.5 |
C3—C4—Ta1 | 76.32 (18) | H22A—C22—H22B | 109.5 |
C5—C4—Ta1 | 73.06 (19) | C21—C22—H22D | 109.5 |
C9—C4—Ta1 | 122.5 (2) | H22A—C22—H22D | 109.5 |
C1—C5—C4 | 107.7 (3) | H22B—C22—H22D | 109.5 |
C1—C5—C10 | 125.2 (3) | C21—C23—H23A | 109.5 |
C4—C5—C10 | 126.5 (3) | C21—C23—H23D | 109.5 |
C1—C5—Ta1 | 77.10 (19) | H23A—C23—H23D | 109.5 |
C4—C5—Ta1 | 72.7 (2) | C21—C23—H23B | 109.5 |
C10—C5—Ta1 | 122.9 (2) | H23A—C23—H23B | 109.5 |
C1—C6—H6A | 109.5 | H23D—C23—H23B | 109.5 |
C1—C6—H6B | 109.5 | C21—C24—H24D | 109.5 |
H6A—C6—H6B | 109.5 | C21—C24—H24A | 109.5 |
C1—C6—H6C | 109.5 | H24D—C24—H24A | 109.5 |
H6A—C6—H6C | 109.5 | C21—C24—H24B | 109.5 |
H6B—C6—H6C | 109.5 | H24D—C24—H24B | 109.5 |
C2—C7—H7A | 109.5 | H24A—C24—H24B | 109.5 |
C34H15F20O4Ta | F(000) = 2016 |
Mr = 1048.41 | Dx = 2.089 Mg m−3 |
Orthorhombic, Pbcm | Mo Kα radiation, λ = 0.71073 Å |
Hall symbol: -P2c2b | Cell parameters from 57 reflections |
a = 8.341 (2) Å | θ = 5.3–12.1° |
b = 26.389 (5) Å | µ = 3.45 mm−1 |
c = 15.145 (3) Å | T = 150 K |
V = 3333.6 (12) Å3 | Needle, yellow |
Z = 4 | 0.46 × 0.12 × 0.08 mm |
Siemens P4 diffractometer | 2150 reflections with I > 2σ(I) |
Radiation source: fine-focus sealed tube | Rint = 0.054 |
Graphite monochromator | θmax = 25.0°, θmin = 2.1° |
ω scans | h = −1→9 |
Absorption correction: empirical (using intensity measurements) ? | k = −31→1 |
Tmin = 0.674, Tmax = 0.770 | l = −1→18 |
3749 measured reflections | 3 standard reflections every 97 reflections |
3043 independent reflections | intensity decay: none |
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)] = 0.045 | Hydrogen site location: inferred from neighbouring sites |
wR(F2) = 0.101 | Riding |
S = 1.01 | w = 1/[σ2(Fo2) + (0.0378P)2] where P = (Fo2 + 2Fc2)/3 |
3043 reflections | (Δ/σ)max < 0.001 |
283 parameters | Δρmax = 0.85 e Å−3 |
0 restraints | Δρmin = −1.09 e Å−3 |
C34H15F20O4Ta | V = 3333.6 (12) Å3 |
Mr = 1048.41 | Z = 4 |
Orthorhombic, Pbcm | Mo Kα radiation |
a = 8.341 (2) Å | µ = 3.45 mm−1 |
b = 26.389 (5) Å | T = 150 K |
c = 15.145 (3) Å | 0.46 × 0.12 × 0.08 mm |
Siemens P4 diffractometer | 2150 reflections with I > 2σ(I) |
Absorption correction: empirical (using intensity measurements) ? | Rint = 0.054 |
Tmin = 0.674, Tmax = 0.770 | 3 standard reflections every 97 reflections |
3749 measured reflections | intensity decay: none |
3043 independent reflections |
R[F2 > 2σ(F2)] = 0.045 | 0 restraints |
wR(F2) = 0.101 | Riding |
S = 1.01 | Δρmax = 0.85 e Å−3 |
3043 reflections | Δρmin = −1.09 e Å−3 |
283 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 on F2 for ALL reflections except for 1 with very negative F2 or flagged by the user for potential systematic errors. Weighted R-factors wR and all goodnesses of fit S are based on F2, conventional R-factors R are based on F, with F set to zero for negative F2. The observed criterion of F2 > σ(F2) is used only for calculating _R_factor_obs 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 | Occ. (<1) | |
Ta1 | 0.18380 (5) | 0.133175 (19) | 0.2500 | 0.01544 (14) | |
C1 | −0.1055 (13) | 0.1426 (4) | 0.2500 | 0.023 (3) | |
C2 | −0.0501 (9) | 0.1690 (3) | 0.1742 (5) | 0.0214 (17) | |
C3 | 0.0490 (9) | 0.2096 (3) | 0.2029 (5) | 0.0173 (16) | |
C4 | −0.2235 (12) | 0.1004 (5) | 0.2500 | 0.028 (3) | |
H4A | −0.3303 | 0.1140 | 0.2500 | 0.042* | |
H4B | −0.2082 | 0.0800 | 0.3018 | 0.042* | 0.50 |
H4BA | −0.2082 | 0.0800 | 0.1982 | 0.042* | 0.50 |
C5 | −0.0922 (10) | 0.1553 (4) | 0.0805 (5) | 0.033 (2) | |
H5A | −0.1871 | 0.1733 | 0.0631 | 0.049* | |
H5B | −0.1111 | 0.1195 | 0.0766 | 0.049* | |
H5C | −0.0051 | 0.1644 | 0.0422 | 0.049* | |
C6 | 0.1279 (10) | 0.2474 (3) | 0.1439 (6) | 0.031 (2) | |
H6A | 0.0555 | 0.2750 | 0.1328 | 0.047* | |
H6B | 0.1561 | 0.2315 | 0.0891 | 0.047* | |
H6C | 0.2230 | 0.2601 | 0.1720 | 0.047* | |
O1 | 0.2321 (6) | 0.1232 (2) | 0.1229 (3) | 0.0285 (14) | |
C7 | 0.3464 (9) | 0.1091 (3) | 0.0680 (5) | 0.0203 (18) | |
C8 | 0.3589 (9) | 0.1303 (3) | −0.0164 (5) | 0.0231 (17) | |
F8 | 0.2576 (6) | 0.16855 (19) | −0.0373 (3) | 0.0353 (12) | |
C9 | 0.4754 (11) | 0.1159 (3) | −0.0750 (5) | 0.030 (2) | |
F9 | 0.4794 (6) | 0.1386 (2) | −0.1551 (3) | 0.0476 (14) | |
C10 | 0.5845 (11) | 0.0787 (4) | −0.0527 (6) | 0.037 (2) | |
F10 | 0.6961 (7) | 0.0656 (3) | −0.1124 (4) | 0.0598 (17) | |
C11 | 0.5746 (10) | 0.0569 (3) | 0.0282 (6) | 0.028 (2) | |
F11 | 0.6825 (7) | 0.0210 (2) | 0.0511 (4) | 0.0507 (14) | |
C12 | 0.4577 (11) | 0.0716 (3) | 0.0860 (5) | 0.0268 (19) | |
F12 | 0.4528 (6) | 0.04799 (19) | 0.1659 (3) | 0.0376 (12) | |
O2 | 0.3890 (9) | 0.1690 (3) | 0.2500 | 0.0298 (19) | |
C13 | 0.4961 (13) | 0.2073 (4) | 0.2500 | 0.024 (3) | |
C14 | 0.5538 (10) | 0.2275 (3) | 0.1719 (5) | 0.0232 (18) | |
F14 | 0.5028 (6) | 0.20997 (18) | 0.0941 (3) | 0.0376 (13) | |
C15 | 0.6670 (10) | 0.2657 (3) | 0.1724 (5) | 0.0289 (19) | |
F15 | 0.7199 (6) | 0.2849 (2) | 0.0943 (3) | 0.0438 (15) | |
C16 | 0.7245 (13) | 0.2856 (4) | 0.2500 | 0.025 (3) | |
F16 | 0.8301 (9) | 0.3232 (3) | 0.2500 | 0.0420 (18) | |
O3 | 0.1266 (9) | 0.0632 (3) | 0.2500 | 0.0270 (19) | |
C17 | 0.0591 (13) | 0.0175 (4) | 0.2500 | 0.021 (2) | |
C18 | 0.0239 (10) | −0.0070 (3) | 0.3271 (6) | 0.029 (2) | |
F18 | 0.0550 (7) | 0.0159 (2) | 0.4042 (3) | 0.0450 (14) | |
C19 | −0.0439 (10) | −0.0544 (3) | 0.3290 (7) | 0.041 (3) | |
F19 | −0.0749 (8) | −0.0777 (2) | 0.4059 (4) | 0.069 (2) | |
C20 | −0.0771 (15) | −0.0792 (4) | 0.2500 | 0.043 (4) | |
F20 | −0.1422 (10) | −0.1249 (3) | 0.2500 | 0.082 (4) |
U11 | U22 | U33 | U12 | U13 | U23 | |
Ta1 | 0.0128 (2) | 0.0158 (2) | 0.0177 (2) | 0.0006 (3) | 0.000 | 0.000 |
C1 | 0.005 (5) | 0.017 (7) | 0.047 (7) | 0.002 (5) | 0.000 | 0.000 |
C2 | 0.009 (4) | 0.027 (4) | 0.028 (4) | 0.000 (3) | −0.004 (4) | 0.003 (3) |
C3 | 0.011 (4) | 0.018 (4) | 0.022 (4) | 0.006 (3) | 0.002 (4) | 0.006 (3) |
C4 | 0.009 (6) | 0.023 (6) | 0.051 (8) | 0.000 (5) | 0.000 | 0.000 |
C5 | 0.024 (5) | 0.054 (6) | 0.021 (4) | 0.007 (4) | −0.011 (4) | −0.004 (4) |
C6 | 0.026 (4) | 0.031 (5) | 0.037 (5) | 0.005 (4) | 0.003 (4) | 0.017 (4) |
O1 | 0.027 (3) | 0.039 (4) | 0.020 (3) | 0.011 (3) | 0.005 (2) | −0.003 (3) |
C7 | 0.019 (5) | 0.029 (4) | 0.013 (3) | 0.000 (4) | 0.003 (3) | −0.001 (3) |
C8 | 0.024 (4) | 0.020 (4) | 0.025 (4) | −0.004 (4) | −0.008 (3) | 0.007 (4) |
F8 | 0.038 (3) | 0.039 (3) | 0.029 (3) | 0.001 (2) | −0.003 (2) | 0.005 (2) |
C9 | 0.037 (6) | 0.037 (5) | 0.015 (4) | −0.017 (4) | 0.014 (4) | −0.003 (4) |
F9 | 0.046 (3) | 0.077 (4) | 0.019 (2) | −0.017 (3) | 0.007 (2) | 0.007 (3) |
C10 | 0.031 (5) | 0.047 (6) | 0.033 (5) | −0.002 (5) | 0.008 (5) | −0.016 (5) |
F10 | 0.040 (3) | 0.091 (5) | 0.049 (3) | 0.010 (4) | 0.023 (3) | −0.021 (3) |
C11 | 0.014 (4) | 0.026 (5) | 0.045 (5) | 0.006 (4) | 0.004 (4) | −0.007 (4) |
F11 | 0.033 (3) | 0.058 (4) | 0.061 (3) | 0.013 (3) | 0.004 (3) | −0.012 (3) |
C12 | 0.029 (5) | 0.025 (4) | 0.027 (5) | 0.005 (4) | −0.006 (4) | −0.003 (4) |
F12 | 0.030 (3) | 0.050 (3) | 0.033 (3) | 0.007 (3) | 0.003 (3) | 0.015 (2) |
O2 | 0.013 (4) | 0.030 (5) | 0.046 (5) | −0.003 (4) | 0.000 | 0.000 |
C13 | 0.015 (6) | 0.017 (6) | 0.041 (7) | 0.010 (5) | 0.000 | 0.000 |
C14 | 0.015 (4) | 0.024 (4) | 0.031 (4) | 0.001 (4) | −0.003 (4) | −0.007 (4) |
F14 | 0.036 (3) | 0.043 (3) | 0.034 (3) | −0.011 (3) | 0.003 (2) | −0.010 (2) |
C15 | 0.024 (5) | 0.025 (4) | 0.037 (5) | −0.003 (4) | 0.017 (4) | 0.006 (4) |
F15 | 0.043 (4) | 0.053 (3) | 0.035 (3) | −0.015 (3) | 0.012 (3) | 0.002 (3) |
C16 | 0.013 (7) | 0.032 (7) | 0.029 (6) | 0.000 (5) | 0.000 | 0.000 |
F16 | 0.034 (4) | 0.037 (4) | 0.055 (4) | −0.018 (4) | 0.000 | 0.000 |
O3 | 0.018 (4) | 0.020 (4) | 0.043 (5) | −0.011 (3) | 0.000 | 0.000 |
C17 | 0.005 (5) | 0.023 (6) | 0.034 (6) | −0.001 (5) | 0.000 | 0.000 |
C18 | 0.022 (4) | 0.025 (4) | 0.039 (5) | 0.005 (4) | 0.010 (4) | −0.005 (4) |
F18 | 0.054 (4) | 0.049 (3) | 0.031 (3) | 0.000 (3) | 0.010 (3) | 0.009 (3) |
C19 | 0.019 (4) | 0.029 (5) | 0.074 (7) | 0.000 (4) | 0.006 (5) | 0.026 (5) |
F19 | 0.061 (4) | 0.058 (4) | 0.086 (5) | −0.002 (3) | 0.020 (4) | 0.044 (4) |
C20 | 0.021 (7) | 0.011 (6) | 0.098 (12) | −0.001 (6) | 0.000 | 0.000 |
F20 | 0.041 (5) | 0.021 (5) | 0.185 (11) | −0.020 (4) | 0.000 | 0.000 |
Ta1—O3 | 1.907 (7) | C8—F8 | 1.355 (9) |
Ta1—O2 | 1.955 (8) | C8—C9 | 1.370 (11) |
Ta1—O1i | 1.985 (5) | C9—F9 | 1.354 (9) |
Ta1—O1 | 1.985 (5) | C9—C10 | 1.380 (13) |
Ta1—C3i | 2.417 (7) | C10—F10 | 1.343 (10) |
Ta1—C3 | 2.417 (7) | C10—C11 | 1.355 (12) |
Ta1—C1 | 2.426 (11) | C11—F11 | 1.351 (10) |
Ta1—C2i | 2.453 (7) | C11—C12 | 1.367 (11) |
Ta1—C2 | 2.453 (7) | C12—F12 | 1.361 (9) |
C1—C2i | 1.420 (10) | O2—C13 | 1.349 (13) |
C1—C2 | 1.420 (10) | C13—C14i | 1.383 (10) |
C1—C4 | 1.487 (15) | C13—C14 | 1.383 (10) |
C2—C3 | 1.423 (10) | C14—F14 | 1.335 (9) |
C2—C5 | 1.504 (10) | C14—C15 | 1.383 (11) |
C3—C3i | 1.426 (14) | C15—F15 | 1.360 (9) |
C3—C6 | 1.492 (10) | C15—C16 | 1.373 (10) |
C4—H4A | 0.9600 | C16—F16 | 1.328 (13) |
C4—H4B | 0.9600 | C16—C15i | 1.373 (10) |
C4—H4BA | 0.9600 | O3—C17 | 1.330 (13) |
C5—H5A | 0.9600 | C17—C18 | 1.368 (10) |
C5—H5B | 0.9600 | C17—C18i | 1.368 (10) |
C5—H5C | 0.9600 | C18—F18 | 1.341 (9) |
C6—H6A | 0.9600 | C18—C19 | 1.373 (12) |
C6—H6B | 0.9600 | C19—F19 | 1.343 (10) |
C6—H6C | 0.9600 | C19—C20 | 1.391 (12) |
O1—C7 | 1.318 (9) | C20—F20 | 1.322 (14) |
C7—C12 | 1.384 (11) | C20—C19i | 1.391 (12) |
C7—C8 | 1.398 (10) | ||
O3—Ta1—O2 | 133.4 (3) | H4B—C4—H4BA | 109.5 |
O3—Ta1—O1i | 85.57 (17) | C2—C5—H5A | 109.5 |
O2—Ta1—O1i | 83.46 (17) | C2—C5—H5B | 109.5 |
O3—Ta1—O1 | 85.57 (17) | H5A—C5—H5B | 109.5 |
O2—Ta1—O1 | 83.46 (17) | C2—C5—H5C | 109.5 |
O1i—Ta1—O1 | 151.9 (3) | H5A—C5—H5C | 109.5 |
O3—Ta1—C3i | 133.8 (3) | H5B—C5—H5C | 109.5 |
O2—Ta1—C3i | 90.2 (3) | C3—C6—H6A | 109.5 |
O1i—Ta1—C3i | 85.3 (2) | C3—C6—H6B | 109.5 |
O1—Ta1—C3i | 119.4 (2) | H6A—C6—H6B | 109.5 |
O3—Ta1—C3 | 133.8 (3) | C3—C6—H6C | 109.5 |
O2—Ta1—C3 | 90.2 (3) | H6A—C6—H6C | 109.5 |
O1i—Ta1—C3 | 119.4 (2) | H6B—C6—H6C | 109.5 |
O1—Ta1—C3 | 85.3 (2) | C7—O1—Ta1 | 142.8 (5) |
C3i—Ta1—C3 | 34.3 (3) | O1—C7—C12 | 124.2 (7) |
O3—Ta1—C1 | 81.4 (3) | O1—C7—C8 | 121.2 (7) |
O2—Ta1—C1 | 145.2 (4) | C12—C7—C8 | 114.6 (7) |
O1i—Ta1—C1 | 102.45 (16) | F8—C8—C9 | 119.8 (7) |
O1—Ta1—C1 | 102.45 (16) | F8—C8—C7 | 117.7 (7) |
C3i—Ta1—C1 | 56.7 (3) | C9—C8—C7 | 122.3 (8) |
C3—Ta1—C1 | 56.7 (3) | F9—C9—C8 | 118.4 (8) |
O3—Ta1—C2i | 100.0 (3) | F9—C9—C10 | 121.3 (8) |
O2—Ta1—C2i | 120.7 (3) | C8—C9—C10 | 120.3 (7) |
O1i—Ta1—C2i | 76.0 (2) | F10—C10—C11 | 122.8 (9) |
O1—Ta1—C2i | 131.8 (2) | F10—C10—C9 | 118.3 (8) |
C3i—Ta1—C2i | 34.0 (2) | C11—C10—C9 | 118.9 (8) |
C3—Ta1—C2i | 56.4 (2) | F11—C11—C10 | 119.3 (8) |
C1—Ta1—C2i | 33.8 (2) | F11—C11—C12 | 120.7 (8) |
O3—Ta1—C2 | 100.0 (3) | C10—C11—C12 | 120.1 (8) |
O2—Ta1—C2 | 120.7 (3) | F12—C12—C11 | 117.4 (7) |
O1i—Ta1—C2 | 131.8 (2) | F12—C12—C7 | 118.9 (7) |
O1—Ta1—C2 | 76.0 (2) | C11—C12—C7 | 123.7 (8) |
C3i—Ta1—C2 | 56.4 (2) | C13—O2—Ta1 | 160.3 (7) |
C3—Ta1—C2 | 34.0 (2) | O2—C13—C14i | 121.2 (5) |
C1—Ta1—C2 | 33.8 (2) | O2—C13—C14 | 121.2 (5) |
C2i—Ta1—C2 | 55.8 (4) | C14i—C13—C14 | 117.5 (10) |
C2i—C1—C2 | 108.0 (9) | F14—C14—C15 | 118.4 (7) |
C2i—C1—C4 | 125.6 (5) | F14—C14—C13 | 120.7 (7) |
C2—C1—C4 | 125.6 (5) | C15—C14—C13 | 120.9 (8) |
C2i—C1—Ta1 | 74.1 (5) | F15—C15—C16 | 119.3 (7) |
C2—C1—Ta1 | 74.1 (5) | F15—C15—C14 | 119.2 (8) |
C4—C1—Ta1 | 125.5 (8) | C16—C15—C14 | 121.5 (8) |
C1—C2—C3 | 108.1 (7) | F16—C16—C15 | 121.2 (5) |
C1—C2—C5 | 124.7 (7) | F16—C16—C15i | 121.2 (5) |
C3—C2—C5 | 127.2 (7) | C15—C16—C15i | 117.7 (10) |
C1—C2—Ta1 | 72.0 (5) | C17—O3—Ta1 | 169.5 (7) |
C3—C2—Ta1 | 71.6 (4) | O3—C17—C18 | 121.4 (5) |
C5—C2—Ta1 | 122.3 (5) | O3—C17—C18i | 121.4 (5) |
C2—C3—C3i | 107.8 (4) | C18—C17—C18i | 117.2 (10) |
C2—C3—C6 | 125.3 (7) | F18—C18—C19 | 118.3 (8) |
C3i—C3—C6 | 126.8 (5) | F18—C18—C17 | 119.2 (7) |
C2—C3—Ta1 | 74.4 (4) | C19—C18—C17 | 122.6 (9) |
C3i—C3—Ta1 | 72.84 (17) | F19—C19—C18 | 120.9 (9) |
C6—C3—Ta1 | 122.0 (5) | F19—C19—C20 | 119.5 (8) |
C1—C4—H4A | 109.5 | C18—C19—C20 | 119.5 (9) |
C1—C4—H4B | 109.5 | F20—C20—C19 | 120.7 (6) |
H4A—C4—H4B | 109.5 | F20—C20—C19i | 120.7 (6) |
C1—C4—H4BA | 109.5 | C19—C20—C19i | 118.6 (11) |
H4A—C4—H4BA | 109.5 |
Symmetry code: (i) x, y, −z+1/2. |
C44H30F20O6Ta2.C7H8 | F(000) = 2872 |
Mr = 1488.71 | Dx = 2.004 Mg m−3 |
Monoclinic, P21/n | Mo Kα radiation, λ = 0.71073 Å |
Hall symbol: -P2yn | Cell parameters from 429 reflections |
a = 12.793 (2) Å | θ = 3.6–19.2° |
b = 15.242 (2) Å | µ = 4.56 mm−1 |
c = 25.708 (3) Å | T = 150 K |
β = 100.178 (5)° | Irregular shape, yellow |
V = 4933.9 (12) Å3 | 0.8 × 0.45 × 0.3 mm |
Z = 4 |
Siemens SMART CCD diffractometer | 6926 independent reflections |
Radiation source: fine-focus sealed tube | 6101 reflections with I > 2σ(I) |
Graphite monochromator | Rint = 0.053 |
ω scans | θmax = 23.3°, θmin = 1.6° |
Absorption correction: empirical (using intensity measurements) ? | h = −14→10 |
Tmin = 0.343, Tmax = 0.447 | k = −16→16 |
17825 measured reflections | l = −18→28 |
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)] = 0.063 | Hydrogen site location: inferred from neighbouring sites |
wR(F2) = 0.094 | Riding |
S = 2.26 | w = 1/[σ2(Fo2) + (0.010P)2] where P = (Fo2 + 2Fc2)/3 |
6922 reflections | (Δ/σ)max < 0.001 |
619 parameters | Δρmax = 1.32 e Å−3 |
0 restraints | Δρmin = −0.96 e Å−3 |
C44H30F20O6Ta2.C7H8 | V = 4933.9 (12) Å3 |
Mr = 1488.71 | Z = 4 |
Monoclinic, P21/n | Mo Kα radiation |
a = 12.793 (2) Å | µ = 4.56 mm−1 |
b = 15.242 (2) Å | T = 150 K |
c = 25.708 (3) Å | 0.8 × 0.45 × 0.3 mm |
β = 100.178 (5)° |
Siemens SMART CCD diffractometer | 6926 independent reflections |
Absorption correction: empirical (using intensity measurements) ? | 6101 reflections with I > 2σ(I) |
Tmin = 0.343, Tmax = 0.447 | Rint = 0.053 |
17825 measured reflections | θmax = 23.3° |
R[F2 > 2σ(F2)] = 0.063 | 0 restraints |
wR(F2) = 0.094 | Riding |
S = 2.26 | Δρmax = 1.32 e Å−3 |
6922 reflections | Δρmin = −0.96 e Å−3 |
619 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 on F2 for ALL reflections except for 3 with very negative F2 or flagged by the user for potential systematic errors. Weighted R-factors wR and all goodnesses of fit S are based on F2, conventional R-factors R are based on F, with F set to zero for negative F2. The observed criterion of F2 > σ(F2) is used only for calculating _R_factor_obs 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 | Occ. (<1) | |
Ta1 | 0.27368 (3) | 0.20981 (3) | 0.083963 (16) | 0.02718 (13) | |
Ta2 | 0.19551 (3) | 0.12229 (3) | 0.176869 (16) | 0.02686 (12) | |
O10 | 0.3210 (5) | 0.1322 (4) | 0.1449 (2) | 0.0277 (15) | |
O11 | 0.1480 (5) | 0.1951 (4) | 0.1143 (2) | 0.0292 (15) | |
C1 | 0.3251 (8) | 0.0881 (6) | 0.0313 (3) | 0.029 (2) | |
C1A | 0.3956 (8) | 0.0134 (6) | 0.0543 (4) | 0.043 (3) | |
H1AA | 0.4055 | −0.0263 | 0.0266 | 0.065* | |
H1AB | 0.3631 | −0.0171 | 0.0799 | 0.065* | |
H1AC | 0.4632 | 0.0361 | 0.0710 | 0.065* | |
C2 | 0.3552 (8) | 0.1645 (7) | 0.0075 (4) | 0.033 (2) | |
C2A | 0.4653 (7) | 0.1919 (7) | 0.0016 (4) | 0.042 (3) | |
H2AA | 0.4818 | 0.1677 | −0.0305 | 0.062* | |
H2AB | 0.5154 | 0.1707 | 0.0312 | 0.062* | |
H2AC | 0.4689 | 0.2547 | 0.0003 | 0.062* | |
C3 | 0.2600 (8) | 0.2123 (6) | −0.0128 (4) | 0.034 (2) | |
C3A | 0.2566 (9) | 0.2945 (7) | −0.0439 (4) | 0.053 (3) | |
H3AA | 0.2515 | 0.2805 | −0.0807 | 0.079* | |
H3AB | 0.3203 | 0.3276 | −0.0322 | 0.079* | |
H3AC | 0.1960 | 0.3286 | −0.0390 | 0.079* | |
C4 | 0.1716 (8) | 0.1646 (6) | −0.0003 (4) | 0.033 (2) | |
C4A | 0.0567 (8) | 0.1904 (7) | −0.0155 (5) | 0.053 (3) | |
H4AA | 0.0286 | 0.1672 | −0.0499 | 0.080* | |
H4AB | 0.0510 | 0.2532 | −0.0163 | 0.080* | |
H4AC | 0.0173 | 0.1672 | 0.0099 | 0.080* | |
C5 | 0.2112 (7) | 0.0876 (6) | 0.0268 (4) | 0.029 (2) | |
C5A | 0.1476 (7) | 0.0133 (6) | 0.0427 (4) | 0.035 (3) | |
H5AA | 0.1313 | −0.0273 | 0.0139 | 0.053* | |
H5AB | 0.0828 | 0.0355 | 0.0516 | 0.053* | |
H5AC | 0.1878 | −0.0160 | 0.0728 | 0.053* | |
O1 | 0.4151 (5) | 0.2633 (4) | 0.1058 (3) | 0.0372 (17) | |
C6 | 0.5039 (7) | 0.2647 (6) | 0.1429 (4) | 0.029 (2) | |
C7 | 0.5345 (8) | 0.3402 (6) | 0.1706 (4) | 0.036 (3) | |
F7 | 0.4697 (4) | 0.4120 (3) | 0.1633 (2) | 0.0431 (15) | |
C8 | 0.6257 (8) | 0.3450 (6) | 0.2089 (4) | 0.032 (2) | |
F8 | 0.6509 (4) | 0.4215 (4) | 0.2351 (2) | 0.0477 (16) | |
C9 | 0.6919 (8) | 0.2726 (7) | 0.2178 (4) | 0.045 (3) | |
F9 | 0.7831 (5) | 0.2786 (4) | 0.2527 (3) | 0.0593 (18) | |
C10 | 0.6655 (8) | 0.1970 (7) | 0.1896 (4) | 0.040 (3) | |
F10 | 0.7296 (5) | 0.1287 (4) | 0.1980 (3) | 0.0590 (18) | |
C11 | 0.5714 (8) | 0.1935 (6) | 0.1531 (4) | 0.033 (2) | |
F11 | 0.5498 (4) | 0.1179 (3) | 0.1265 (2) | 0.0416 (14) | |
O2 | 0.0696 (5) | 0.0516 (4) | 0.1551 (3) | 0.0350 (17) | |
C12 | −0.0293 (8) | 0.0268 (6) | 0.1394 (4) | 0.032 (2) | |
C13 | −0.0675 (7) | −0.0534 (7) | 0.1533 (4) | 0.034 (2) | |
F13 | 0.0010 (4) | −0.1057 (3) | 0.1863 (3) | 0.0502 (17) | |
C14 | −0.1700 (9) | −0.0814 (7) | 0.1385 (5) | 0.045 (3) | |
F14 | −0.1999 (5) | −0.1605 (4) | 0.1536 (3) | 0.0570 (18) | |
C15 | −0.2437 (8) | −0.0298 (8) | 0.1054 (4) | 0.041 (3) | |
F15 | −0.3441 (4) | −0.0559 (4) | 0.0901 (2) | 0.0568 (18) | |
C16 | −0.2105 (9) | 0.0485 (8) | 0.0904 (4) | 0.047 (3) | |
F16 | −0.2784 (5) | 0.1022 (5) | 0.0596 (3) | 0.0637 (19) | |
C17 | −0.1054 (8) | 0.0777 (7) | 0.1065 (4) | 0.039 (3) | |
F17 | −0.0779 (5) | 0.1562 (4) | 0.0897 (3) | 0.0574 (18) | |
O3 | 0.2644 (5) | 0.0088 (4) | 0.2046 (3) | 0.0353 (17) | |
C18 | 0.3346 (8) | −0.0448 (6) | 0.1891 (4) | 0.030 (2) | |
C19 | 0.4449 (8) | −0.0278 (6) | 0.2012 (3) | 0.030 (2) | |
F19 | 0.4797 (4) | 0.0449 (4) | 0.2282 (2) | 0.0419 (14) | |
C20 | 0.5194 (8) | −0.0843 (7) | 0.1865 (4) | 0.037 (3) | |
F20 | 0.6222 (4) | −0.0632 (4) | 0.1984 (2) | 0.0503 (17) | |
C21 | 0.4867 (8) | −0.1606 (7) | 0.1601 (4) | 0.034 (3) | |
F21 | 0.5580 (5) | −0.2162 (4) | 0.1458 (2) | 0.0512 (16) | |
C22 | 0.3789 (9) | −0.1795 (6) | 0.1483 (4) | 0.036 (3) | |
F22 | 0.3483 (5) | −0.2545 (4) | 0.1233 (2) | 0.0543 (17) | |
C23 | 0.3063 (8) | −0.1228 (6) | 0.1627 (4) | 0.035 (2) | |
F23 | 0.2024 (4) | −0.1429 (3) | 0.1501 (2) | 0.0473 (16) | |
O4 | 0.2274 (5) | 0.3301 (4) | 0.0675 (3) | 0.047 (2) | |
C24 | 0.2154 (8) | 0.4150 (7) | 0.0610 (4) | 0.036 (3) | |
C25 | 0.1166 (8) | 0.4557 (7) | 0.0618 (4) | 0.038 (3) | |
F25 | 0.0341 (5) | 0.4065 (4) | 0.0692 (3) | 0.0537 (17) | |
C26 | 0.1009 (9) | 0.5450 (7) | 0.0546 (4) | 0.046 (3) | |
F26 | 0.0069 (5) | 0.5807 (4) | 0.0562 (3) | 0.067 (2) | |
C27 | 0.1837 (9) | 0.5971 (6) | 0.0454 (4) | 0.040 (3) | |
F27 | 0.1699 (5) | 0.6845 (3) | 0.0393 (3) | 0.067 (2) | |
C28 | 0.2805 (8) | 0.5601 (6) | 0.0455 (4) | 0.036 (3) | |
F28 | 0.3644 (5) | 0.6108 (4) | 0.0383 (3) | 0.0630 (19) | |
C29 | 0.2959 (9) | 0.4704 (6) | 0.0522 (4) | 0.041 (3) | |
F29 | 0.3905 (5) | 0.4358 (4) | 0.0479 (3) | 0.0531 (17) | |
C30 | 0.2738 (9) | 0.1960 (7) | 0.2583 (5) | 0.050 (3)* | |
C30A | 0.3974 (18) | 0.2201 (15) | 0.2649 (9) | 0.016 (5)* | 0.37 |
H30A | 0.4228 | 0.2748 | 0.2810 | 0.023* | 0.37 |
H30B | 0.3289 | 0.2287 | 0.2434 | 0.023* | 0.37 |
H30C | 0.4462 | 0.1991 | 0.2434 | 0.023* | 0.37 |
C30B | 0.3928 (18) | 0.1848 (15) | 0.2876 (10) | 0.088 (8)* | 0.63 |
H30D | 0.4031 | 0.2135 | 0.3213 | 0.132* | 0.63 |
H30E | 0.4461 | 0.1404 | 0.2878 | 0.132* | 0.63 |
H30F | 0.3237 | 0.1582 | 0.2808 | 0.132* | 0.63 |
C31 | 0.2053 (9) | 0.1373 (7) | 0.2734 (5) | 0.051 (3)* | |
C31A | 0.2790 (18) | 0.0688 (15) | 0.3125 (9) | 0.019 (6)* | 0.37 |
H31A | 0.3122 | 0.0885 | 0.3470 | 0.028* | 0.37 |
H31B | 0.2829 | 0.1144 | 0.2872 | 0.028* | 0.37 |
H31C | 0.3149 | 0.0175 | 0.3031 | 0.028* | 0.37 |
C31B | 0.2149 (16) | 0.0567 (14) | 0.3128 (9) | 0.076 (7)* | 0.63 |
H31D | 0.1972 | 0.0737 | 0.3462 | 0.114* | 0.63 |
H31E | 0.2040 | −0.0052 | 0.3078 | 0.114* | 0.63 |
H31F | 0.1705 | 0.0879 | 0.2848 | 0.114* | 0.63 |
C32 | 0.1047 (9) | 0.1605 (7) | 0.2507 (5) | 0.051 (3)* | |
C32A | −0.028 (3) | 0.144 (2) | 0.2486 (14) | 0.065 (10)* | 0.37 |
H32A | −0.0595 | 0.1759 | 0.2741 | 0.098* | 0.37 |
H32B | −0.0832 | 0.1206 | 0.2220 | 0.098* | 0.37 |
H32C | 0.0160 | 0.1826 | 0.2324 | 0.098* | 0.37 |
C32B | 0.0119 (13) | 0.0992 (11) | 0.2649 (7) | 0.042 (5)* | 0.63 |
H32D | 0.0081 | 0.0993 | 0.3019 | 0.063* | 0.63 |
H32E | 0.0844 | 0.1067 | 0.2606 | 0.063* | 0.63 |
H32F | −0.0146 | 0.0444 | 0.2496 | 0.063* | 0.63 |
C33 | 0.1077 (9) | 0.2352 (7) | 0.2209 (5) | 0.050 (3)* | |
C33A | 0.052 (2) | 0.3169 (18) | 0.1856 (11) | 0.041 (8)* | 0.37 |
H33A | 0.0398 | 0.3692 | 0.2044 | 0.062* | 0.37 |
H33B | 0.0479 | 0.3304 | 0.1488 | 0.062* | 0.37 |
H33C | 0.1217 | 0.2945 | 0.1995 | 0.062* | 0.37 |
C33B | −0.0031 (14) | 0.2712 (12) | 0.1898 (8) | 0.055 (5)* | 0.63 |
H33D | −0.0505 | 0.2945 | 0.2115 | 0.083* | 0.63 |
H33E | 0.0313 | 0.2198 | 0.2063 | 0.083* | 0.63 |
H33F | −0.0427 | 0.2560 | 0.1557 | 0.083* | 0.63 |
C34 | 0.2158 (9) | 0.2568 (7) | 0.2247 (4) | 0.047 (3)* | |
C34A | 0.2942 (18) | 0.3315 (15) | 0.2135 (9) | 0.024 (6)* | 0.37 |
H34A | 0.3107 | 0.3740 | 0.2412 | 0.036* | 0.37 |
H34B | 0.3469 | 0.3339 | 0.1911 | 0.036* | 0.37 |
H34C | 0.2936 | 0.2739 | 0.2286 | 0.036* | 0.37 |
C34B | 0.2346 (6) | 0.3424 (5) | 0.1956 (3) | 0.067 (6)* | 0.63 |
H34D | 0.2061 | 0.3942 | 0.2092 | 0.100* | 0.63 |
H34E | 0.1878 | 0.2938 | 0.1977 | 0.100* | 0.63 |
H34F | 0.2413 | 0.3519 | 0.1594 | 0.100* | 0.63 |
C35 | 0.7545 (6) | 0.4299 (5) | 0.1099 (3) | 0.086* | |
C36 | 0.6550 (6) | 0.4680 (5) | 0.0949 (3) | 0.086* | |
H36A | 0.6035 | 0.4399 | 0.0705 | 0.103* | |
C37 | 0.6326 (6) | 0.5480 (5) | 0.1164 (3) | 0.086* | |
H37A | 0.5658 | 0.5728 | 0.1061 | 0.103* | |
C38 | 0.7081 | 0.5919 | 0.1532 | 0.086* | |
H38A | 0.6921 | 0.6454 | 0.1674 | 0.103* | |
C39 | 0.8076 | 0.5538 | 0.1682 | 0.086* | |
H39A | 0.8591 | 0.5819 | 0.1926 | 0.103* | |
C40 | 0.8301 | 0.4738 | 0.1467 | 0.086* | |
H40A | 0.8969 | 0.4490 | 0.1570 | 0.103* | |
C41 | 0.7659 | 0.3476 | 0.0862 | 0.086* | |
H41A | 0.7014 | 0.3332 | 0.0625 | 0.129* | |
H41B | 0.7804 | 0.3034 | 0.1131 | 0.129* | |
H41C | 0.8235 | 0.3501 | 0.0669 | 0.129* |
U11 | U22 | U33 | U12 | U13 | U23 | |
Ta1 | 0.0319 (2) | 0.0235 (2) | 0.0268 (2) | 0.00272 (19) | 0.00705 (18) | 0.00278 (19) |
Ta2 | 0.0304 (2) | 0.0232 (2) | 0.0282 (2) | 0.00268 (19) | 0.00850 (18) | 0.00188 (19) |
O10 | 0.032 (4) | 0.028 (4) | 0.025 (4) | 0.009 (3) | 0.011 (3) | 0.008 (3) |
O11 | 0.034 (4) | 0.024 (4) | 0.031 (4) | 0.003 (3) | 0.009 (3) | 0.004 (3) |
C1 | 0.054 (7) | 0.017 (5) | 0.012 (5) | 0.013 (5) | 0.000 (5) | −0.004 (4) |
C1A | 0.052 (7) | 0.046 (7) | 0.030 (6) | 0.008 (6) | 0.000 (5) | −0.006 (5) |
C2 | 0.040 (6) | 0.044 (6) | 0.020 (6) | −0.004 (5) | 0.020 (5) | −0.011 (5) |
C2A | 0.038 (6) | 0.055 (7) | 0.034 (7) | −0.002 (5) | 0.010 (5) | 0.005 (6) |
C3 | 0.060 (7) | 0.031 (6) | 0.011 (5) | 0.004 (5) | 0.005 (5) | 0.001 (5) |
C3A | 0.077 (9) | 0.050 (7) | 0.034 (7) | 0.009 (7) | 0.017 (6) | 0.015 (6) |
C4 | 0.033 (6) | 0.038 (6) | 0.027 (6) | 0.000 (5) | 0.000 (5) | 0.005 (5) |
C4A | 0.035 (7) | 0.062 (8) | 0.059 (8) | 0.007 (6) | −0.003 (6) | 0.009 (6) |
C5 | 0.022 (5) | 0.038 (6) | 0.028 (6) | −0.004 (5) | 0.002 (4) | 0.001 (5) |
C5A | 0.033 (6) | 0.038 (6) | 0.034 (6) | 0.006 (5) | 0.005 (5) | −0.006 (5) |
O1 | 0.038 (4) | 0.035 (4) | 0.037 (4) | −0.012 (3) | 0.001 (3) | 0.005 (3) |
C6 | 0.025 (6) | 0.035 (6) | 0.028 (6) | −0.010 (5) | 0.008 (5) | 0.004 (5) |
C7 | 0.042 (7) | 0.027 (6) | 0.042 (7) | −0.007 (5) | 0.019 (6) | −0.008 (5) |
F7 | 0.046 (4) | 0.039 (3) | 0.047 (4) | −0.001 (3) | 0.013 (3) | 0.000 (3) |
C8 | 0.047 (7) | 0.033 (6) | 0.021 (6) | −0.010 (5) | 0.017 (5) | −0.005 (5) |
F8 | 0.056 (4) | 0.041 (4) | 0.044 (4) | −0.014 (3) | 0.002 (3) | −0.017 (3) |
C9 | 0.036 (7) | 0.055 (8) | 0.042 (7) | 0.001 (6) | 0.002 (5) | −0.020 (6) |
F9 | 0.045 (4) | 0.069 (5) | 0.059 (5) | −0.003 (4) | −0.004 (3) | −0.024 (4) |
C10 | 0.030 (6) | 0.050 (7) | 0.040 (7) | −0.005 (6) | 0.003 (5) | −0.015 (6) |
F10 | 0.047 (4) | 0.063 (4) | 0.061 (5) | 0.016 (4) | −0.006 (3) | −0.022 (4) |
C11 | 0.030 (6) | 0.033 (6) | 0.038 (6) | −0.011 (5) | 0.016 (5) | −0.017 (5) |
F11 | 0.052 (4) | 0.034 (3) | 0.039 (4) | 0.001 (3) | 0.007 (3) | −0.011 (3) |
O2 | 0.023 (4) | 0.036 (4) | 0.045 (5) | −0.005 (3) | 0.004 (3) | −0.002 (3) |
C12 | 0.039 (7) | 0.027 (6) | 0.032 (6) | −0.005 (5) | 0.016 (5) | 0.002 (5) |
C13 | 0.024 (6) | 0.039 (6) | 0.040 (7) | 0.006 (5) | 0.006 (5) | 0.005 (5) |
F13 | 0.045 (4) | 0.037 (4) | 0.070 (5) | −0.002 (3) | 0.014 (3) | 0.010 (3) |
C14 | 0.046 (7) | 0.041 (7) | 0.050 (8) | −0.012 (6) | 0.016 (6) | −0.017 (6) |
F14 | 0.048 (4) | 0.046 (4) | 0.081 (5) | −0.019 (3) | 0.020 (4) | −0.007 (4) |
C15 | 0.036 (7) | 0.053 (8) | 0.036 (7) | −0.015 (6) | 0.011 (5) | −0.024 (6) |
F15 | 0.032 (4) | 0.091 (5) | 0.047 (4) | −0.015 (4) | 0.004 (3) | −0.024 (4) |
C16 | 0.044 (7) | 0.066 (8) | 0.028 (7) | 0.019 (7) | 0.002 (6) | −0.002 (6) |
F16 | 0.044 (4) | 0.097 (5) | 0.046 (4) | 0.011 (4) | −0.001 (3) | 0.019 (4) |
C17 | 0.047 (7) | 0.034 (6) | 0.041 (7) | 0.003 (6) | 0.020 (6) | 0.006 (5) |
F17 | 0.049 (4) | 0.052 (4) | 0.071 (5) | 0.011 (3) | 0.012 (4) | 0.022 (4) |
O3 | 0.037 (4) | 0.032 (4) | 0.041 (4) | 0.004 (3) | 0.018 (4) | 0.003 (3) |
C18 | 0.034 (6) | 0.031 (6) | 0.025 (6) | 0.010 (5) | 0.005 (5) | 0.017 (5) |
C19 | 0.052 (7) | 0.022 (5) | 0.014 (5) | 0.002 (5) | 0.003 (5) | 0.008 (4) |
F19 | 0.044 (4) | 0.038 (3) | 0.039 (4) | 0.002 (3) | −0.005 (3) | −0.010 (3) |
C20 | 0.037 (7) | 0.044 (7) | 0.031 (6) | 0.014 (5) | 0.007 (5) | 0.002 (5) |
F20 | 0.033 (4) | 0.062 (4) | 0.054 (4) | 0.012 (3) | 0.000 (3) | 0.003 (3) |
C21 | 0.035 (6) | 0.048 (7) | 0.020 (6) | 0.019 (6) | 0.004 (5) | −0.001 (5) |
F21 | 0.056 (4) | 0.046 (4) | 0.053 (4) | 0.023 (3) | 0.014 (3) | −0.005 (3) |
C22 | 0.056 (8) | 0.021 (6) | 0.030 (6) | 0.011 (5) | 0.008 (5) | 0.003 (5) |
F22 | 0.070 (5) | 0.035 (4) | 0.056 (4) | −0.001 (3) | 0.005 (3) | −0.012 (3) |
C23 | 0.040 (7) | 0.028 (6) | 0.039 (7) | −0.004 (5) | 0.011 (5) | 0.006 (5) |
F23 | 0.037 (4) | 0.040 (4) | 0.065 (4) | −0.007 (3) | 0.012 (3) | 0.007 (3) |
O4 | 0.051 (5) | 0.023 (4) | 0.068 (6) | 0.004 (3) | 0.015 (4) | 0.016 (4) |
C24 | 0.047 (7) | 0.030 (6) | 0.030 (6) | −0.001 (5) | 0.002 (5) | 0.001 (5) |
C25 | 0.036 (6) | 0.053 (7) | 0.025 (6) | −0.007 (6) | 0.006 (5) | 0.002 (5) |
F25 | 0.047 (4) | 0.050 (4) | 0.066 (5) | 0.003 (3) | 0.015 (3) | 0.011 (3) |
C26 | 0.051 (8) | 0.044 (7) | 0.039 (7) | 0.024 (6) | 0.001 (6) | −0.001 (6) |
F26 | 0.066 (5) | 0.055 (4) | 0.077 (5) | 0.027 (4) | 0.005 (4) | −0.004 (4) |
C27 | 0.059 (8) | 0.026 (6) | 0.028 (6) | 0.004 (6) | −0.009 (6) | −0.001 (5) |
F27 | 0.093 (5) | 0.018 (3) | 0.083 (5) | 0.010 (3) | −0.001 (4) | 0.002 (3) |
C28 | 0.043 (7) | 0.025 (6) | 0.033 (6) | −0.006 (5) | −0.010 (5) | 0.009 (5) |
F28 | 0.077 (5) | 0.041 (4) | 0.068 (5) | −0.020 (4) | 0.004 (4) | 0.017 (3) |
C29 | 0.062 (8) | 0.023 (6) | 0.038 (7) | 0.010 (6) | 0.007 (6) | 0.006 (5) |
F29 | 0.045 (4) | 0.049 (4) | 0.068 (5) | 0.004 (3) | 0.018 (3) | 0.011 (3) |
Ta1—O11 | 1.921 (6) | C23—F23 | 1.346 (10) |
Ta1—O4 | 1.949 (6) | O4—C24 | 1.311 (11) |
Ta1—O10 | 1.972 (6) | C24—C29 | 1.381 (13) |
Ta1—O1 | 1.973 (6) | C24—C25 | 1.412 (13) |
Ta1—C5 | 2.420 (9) | C25—F25 | 1.335 (10) |
Ta1—C4 | 2.424 (10) | C25—C26 | 1.384 (14) |
Ta1—C1 | 2.455 (8) | C26—F26 | 1.327 (11) |
Ta1—C3 | 2.463 (9) | C26—C27 | 1.377 (14) |
Ta1—C2 | 2.480 (8) | C27—F27 | 1.350 (11) |
Ta1—Ta2 | 3.0542 (6) | C27—C28 | 1.360 (13) |
Ta2—O10 | 1.934 (6) | C28—F28 | 1.362 (10) |
Ta2—O2 | 1.937 (6) | C28—C29 | 1.387 (13) |
Ta2—O11 | 1.960 (6) | C29—F29 | 1.343 (11) |
Ta2—O3 | 2.014 (6) | C30—C31 | 1.356 (14) |
Ta2—C34 | 2.381 (11) | C30—C34 | 1.389 (14) |
Ta2—C30 | 2.431 (11) | C30—C30B | 1.58 (2) |
Ta2—C33 | 2.441 (11) | C30—C30A | 1.60 (2) |
Ta2—C32 | 2.463 (11) | C30A—C30B | 0.80 (3) |
Ta2—C31 | 2.473 (11) | C30A—H30A | 0.9600 |
C1—C2 | 1.400 (12) | C30A—H30B | 0.9600 |
C1—C5 | 1.442 (12) | C30A—H30C | 0.9600 |
C1—C1A | 1.507 (12) | C30B—H30D | 0.9600 |
C1A—H1AA | 0.9600 | C30B—H30E | 0.9600 |
C1A—H1AB | 0.9600 | C30B—H30F | 0.9600 |
C1A—H1AC | 0.9600 | C31—C32 | 1.362 (14) |
C2—C3 | 1.437 (13) | C31—C31B | 1.58 (2) |
C2—C2A | 1.501 (12) | C31—C31A | 1.63 (2) |
C2A—H2AA | 0.9600 | C31A—C31B | 0.84 (2) |
C2A—H2AB | 0.9600 | C31A—H31A | 0.9600 |
C2A—H2AC | 0.9600 | C31A—H31B | 0.9600 |
C3—C4 | 1.428 (13) | C31A—H31C | 0.9600 |
C3—C3A | 1.483 (13) | C31B—H31D | 0.9600 |
C3A—H3AA | 0.9600 | C31B—H31E | 0.9600 |
C3A—H3AB | 0.9600 | C31B—H31F | 0.9600 |
C3A—H3AC | 0.9600 | C32—C33 | 1.376 (14) |
C4—C5 | 1.413 (12) | C32—C32B | 1.603 (19) |
C4—C4A | 1.504 (12) | C32—C32A | 1.71 (3) |
C4A—H4AA | 0.9600 | C32A—C32B | 0.91 (3) |
C4A—H4AB | 0.9600 | C32A—H32A | 0.9600 |
C4A—H4AC | 0.9600 | C32A—H32B | 0.9600 |
C5—C5A | 1.492 (12) | C32A—H32C | 0.9600 |
C5A—H5AA | 0.9600 | C32B—H32D | 0.9600 |
C5A—H5AB | 0.9600 | C32B—H32E | 0.9600 |
C5A—H5AC | 0.9600 | C32B—H32F | 0.9600 |
O1—C6 | 1.349 (10) | C33—C34 | 1.409 (14) |
C6—C7 | 1.373 (12) | C33—C33B | 1.60 (2) |
C6—C11 | 1.382 (12) | C33—C33A | 1.63 (3) |
C7—F7 | 1.366 (11) | C33A—C33B | 1.01 (3) |
C7—C8 | 1.389 (14) | C33A—H33A | 0.9600 |
C8—F8 | 1.356 (10) | C33A—H33B | 0.9600 |
C8—C9 | 1.386 (13) | C33A—H33C | 0.9600 |
C9—F9 | 1.343 (11) | C33B—H33D | 0.9600 |
C9—C10 | 1.370 (13) | C33B—H33E | 0.9600 |
C10—F10 | 1.319 (11) | C33B—H33F | 0.9600 |
C10—C11 | 1.391 (13) | C34—C34B | 1.544 (13) |
C11—F11 | 1.345 (10) | C34—C34A | 1.58 (2) |
O2—C12 | 1.313 (10) | C34A—C34B | 0.83 (2) |
C12—C13 | 1.387 (12) | C34A—H34A | 0.9600 |
C12—C17 | 1.405 (13) | C34A—H34B | 0.9600 |
C13—F13 | 1.364 (10) | C34A—H34C | 0.9600 |
C13—C14 | 1.367 (13) | C34B—H34D | 0.9600 |
C14—F14 | 1.345 (12) | C34B—H34E | 0.9600 |
C14—C15 | 1.395 (15) | C34B—H34F | 0.9600 |
C15—F15 | 1.336 (11) | C35—C36 | 1.3900 |
C15—C16 | 1.345 (15) | C35—C40 | 1.398 (8) |
C16—F16 | 1.345 (11) | C35—C41 | 1.413 (8) |
C16—C17 | 1.407 (14) | C36—C37 | 1.3901 |
C17—F17 | 1.339 (10) | C36—H36A | 0.9300 |
O3—C18 | 1.326 (10) | C37—C38 | 1.398 (8) |
C18—C23 | 1.385 (13) | C37—H37A | 0.9299 |
C18—C19 | 1.414 (13) | C38—C39 | 1.3900 |
C19—F19 | 1.340 (10) | C38—H38A | 0.9300 |
C19—C20 | 1.386 (13) | C39—C40 | 1.3900 |
C20—F20 | 1.335 (11) | C39—H39A | 0.9300 |
C20—C21 | 1.375 (13) | C40—H40A | 0.9300 |
C21—F21 | 1.342 (10) | C41—H41A | 0.9600 |
C21—C22 | 1.388 (13) | C41—H41B | 0.9600 |
C22—F22 | 1.336 (10) | C41—H41C | 0.9600 |
C22—C23 | 1.367 (13) | ||
O11—Ta1—O4 | 87.3 (3) | F21—C21—C22 | 120.4 (9) |
O11—Ta1—O10 | 76.6 (2) | C20—C21—C22 | 119.1 (9) |
O4—Ta1—O10 | 140.8 (3) | F22—C22—C23 | 121.0 (10) |
O11—Ta1—O1 | 136.3 (3) | F22—C22—C21 | 118.6 (9) |
O4—Ta1—O1 | 84.3 (3) | C23—C22—C21 | 120.4 (9) |
O10—Ta1—O1 | 83.3 (3) | F23—C23—C22 | 118.7 (9) |
O11—Ta1—C5 | 87.0 (3) | F23—C23—C18 | 118.4 (9) |
O4—Ta1—C5 | 122.5 (3) | C22—C23—C18 | 122.9 (10) |
O10—Ta1—C5 | 92.5 (3) | C24—O4—Ta1 | 168.6 (7) |
O1—Ta1—C5 | 132.8 (3) | O4—C24—C29 | 123.4 (10) |
O11—Ta1—C4 | 88.4 (3) | O4—C24—C25 | 121.1 (10) |
O4—Ta1—C4 | 88.8 (3) | C29—C24—C25 | 115.4 (10) |
O10—Ta1—C4 | 125.6 (3) | F25—C25—C26 | 118.2 (10) |
O1—Ta1—C4 | 134.0 (3) | F25—C25—C24 | 119.2 (10) |
C5—Ta1—C4 | 33.9 (3) | C26—C25—C24 | 122.6 (10) |
O11—Ta1—C1 | 117.5 (3) | F26—C26—C27 | 119.8 (10) |
O4—Ta1—C1 | 133.8 (3) | F26—C26—C25 | 120.7 (11) |
O10—Ta1—C1 | 84.9 (3) | C27—C26—C25 | 119.5 (10) |
O1—Ta1—C1 | 98.5 (3) | F27—C27—C28 | 120.7 (10) |
C5—Ta1—C1 | 34.4 (3) | F27—C27—C26 | 120.0 (10) |
C4—Ta1—C1 | 56.4 (3) | C28—C27—C26 | 119.2 (10) |
O11—Ta1—C3 | 119.8 (3) | C27—C28—F28 | 120.3 (9) |
O4—Ta1—C3 | 78.6 (3) | C27—C28—C29 | 121.2 (10) |
O10—Ta1—C3 | 140.3 (3) | F28—C28—C29 | 118.5 (10) |
O1—Ta1—C3 | 100.3 (3) | F29—C29—C24 | 118.8 (9) |
C5—Ta1—C3 | 56.0 (3) | F29—C29—C28 | 119.2 (10) |
C4—Ta1—C3 | 34.0 (3) | C24—C29—C28 | 121.9 (10) |
C1—Ta1—C3 | 55.4 (3) | C31—C30—C34 | 108.5 (10) |
O11—Ta1—C2 | 142.1 (3) | C31—C30—C30B | 114.0 (13) |
O4—Ta1—C2 | 104.1 (3) | C34—C30—C30B | 137.0 (13) |
O10—Ta1—C2 | 110.5 (3) | C31—C30—C30A | 142.7 (13) |
O1—Ta1—C2 | 81.2 (3) | C34—C30—C30A | 108.8 (12) |
C5—Ta1—C2 | 56.3 (3) | C30B—C30—C30A | 29.2 (10) |
C4—Ta1—C2 | 56.5 (3) | C31—C30—Ta2 | 75.7 (7) |
C1—Ta1—C2 | 33.0 (3) | C34—C30—Ta2 | 71.3 (7) |
C3—Ta1—C2 | 33.8 (3) | C30B—C30—Ta2 | 125.1 (11) |
O11—Ta1—Ta2 | 38.55 (18) | C30A—C30—Ta2 | 116.5 (10) |
O4—Ta1—Ta2 | 116.8 (2) | C30B—C30A—C30 | 74 (3) |
O10—Ta1—Ta2 | 38.12 (16) | C30B—C30A—H30A | 109.5 |
O1—Ta1—Ta2 | 111.59 (19) | C30—C30A—H30A | 119.7 |
C5—Ta1—Ta2 | 91.2 (2) | C30B—C30A—H30B | 109.5 |
C4—Ta1—Ta2 | 112.1 (2) | C30—C30A—H30B | 35.5 |
C1—Ta1—Ta2 | 105.0 (2) | H30A—C30A—H30B | 109.5 |
C3—Ta1—Ta2 | 145.3 (2) | C30B—C30A—H30C | 109.5 |
C2—Ta1—Ta2 | 137.7 (2) | C30—C30A—H30C | 126.3 |
O10—Ta2—O2 | 129.1 (3) | H30A—C30A—H30C | 109.5 |
O10—Ta2—O11 | 76.6 (2) | H30B—C30A—H30C | 109.5 |
O2—Ta2—O11 | 87.5 (3) | C30A—C30B—C30 | 77 (3) |
O10—Ta2—O3 | 82.7 (2) | C30A—C30B—H30D | 109.5 |
O2—Ta2—O3 | 85.1 (3) | C30—C30B—H30D | 110.3 |
O11—Ta2—O3 | 146.1 (2) | C30A—C30B—H30E | 109.5 |
O10—Ta2—C34 | 97.4 (3) | C30—C30B—H30E | 134.5 |
O2—Ta2—C34 | 129.6 (3) | H30D—C30B—H30E | 109.5 |
O11—Ta2—C34 | 85.7 (3) | C30A—C30B—H30F | 109.5 |
O3—Ta2—C34 | 123.8 (3) | C30—C30B—H30F | 35.1 |
O10—Ta2—C30 | 94.7 (3) | H30D—C30B—H30F | 109.5 |
O2—Ta2—C30 | 134.5 (3) | H30E—C30B—H30F | 109.5 |
O11—Ta2—C30 | 117.7 (3) | C30—C31—C32 | 108.4 (11) |
O3—Ta2—C30 | 90.3 (3) | C30—C31—C31B | 135.6 (13) |
C34—Ta2—C30 | 33.5 (3) | C32—C31—C31B | 115.8 (12) |
O10—Ta2—C33 | 128.8 (3) | C30—C31—C31A | 105.5 (12) |
O2—Ta2—C33 | 95.7 (3) | C32—C31—C31A | 146.1 (13) |
O11—Ta2—C33 | 83.1 (3) | C31B—C31—C31A | 30.3 (9) |
O3—Ta2—C33 | 130.5 (3) | C30—C31—Ta2 | 72.2 (7) |
C34—Ta2—C33 | 33.9 (3) | C32—C31—Ta2 | 73.6 (7) |
C30—Ta2—C33 | 55.1 (4) | C31B—C31—Ta2 | 123.7 (10) |
O10—Ta2—C32 | 148.0 (3) | C31A—C31—Ta2 | 118.8 (10) |
O2—Ta2—C32 | 82.7 (3) | C31B—C31A—C31 | 72 (2) |
O11—Ta2—C32 | 112.2 (3) | C31B—C31A—H31A | 109.5 |
O3—Ta2—C32 | 99.6 (3) | C31—C31A—H31A | 118.9 |
C34—Ta2—C32 | 54.7 (4) | C31B—C31A—H31B | 109.5 |
C30—Ta2—C32 | 53.5 (4) | C31—C31A—H31B | 37.9 |
C33—Ta2—C32 | 32.6 (3) | H31A—C31A—H31B | 109.5 |
O10—Ta2—C31 | 121.3 (3) | C31B—C31A—H31C | 109.5 |
O2—Ta2—C31 | 103.5 (3) | C31—C31A—H31C | 128.1 |
O11—Ta2—C31 | 136.4 (3) | H31A—C31A—H31C | 109.5 |
O3—Ta2—C31 | 77.5 (3) | H31B—C31A—H31C | 109.5 |
C34—Ta2—C31 | 54.6 (4) | C31A—C31B—C31 | 78 (2) |
C30—Ta2—C31 | 32.1 (3) | C31A—C31B—H31D | 109.5 |
C33—Ta2—C31 | 54.2 (4) | C31—C31B—H31D | 111.0 |
C32—Ta2—C31 | 32.0 (3) | C31A—C31B—H31E | 109.5 |
O10—Ta2—Ta1 | 39.00 (17) | C31—C31B—H31E | 133.2 |
O2—Ta2—Ta1 | 112.80 (19) | H31D—C31B—H31E | 109.5 |
O11—Ta2—Ta1 | 37.63 (17) | C31A—C31B—H31F | 109.5 |
O3—Ta2—Ta1 | 117.94 (17) | C31—C31B—H31F | 33.7 |
C34—Ta2—Ta1 | 90.4 (3) | H31D—C31B—H31F | 109.5 |
C30—Ta2—Ta1 | 109.2 (3) | H31E—C31B—H31F | 109.5 |
C33—Ta2—Ta1 | 107.2 (3) | C31—C32—C33 | 109.6 (11) |
C32—Ta2—Ta1 | 139.8 (3) | C31—C32—C32B | 115.7 (11) |
C31—Ta2—Ta1 | 141.1 (3) | C33—C32—C32B | 134.7 (12) |
Ta2—O10—Ta1 | 102.9 (3) | C31—C32—C32A | 146.5 (15) |
Ta1—O11—Ta2 | 103.8 (3) | C33—C32—C32A | 103.2 (14) |
C2—C1—C5 | 108.8 (8) | C32B—C32—C32A | 31.7 (11) |
C2—C1—C1A | 127.4 (9) | C31—C32—Ta2 | 74.4 (7) |
C5—C1—C1A | 123.6 (9) | C33—C32—Ta2 | 72.8 (7) |
C2—C1—Ta1 | 74.5 (5) | C32B—C32—Ta2 | 120.5 (9) |
C5—C1—Ta1 | 71.5 (5) | C32A—C32—Ta2 | 122.8 (13) |
C1A—C1—Ta1 | 123.7 (6) | C32B—C32A—C32 | 68 (2) |
C1—C1A—H1AA | 109.5 | C32B—C32A—H32A | 109.5 |
C1—C1A—H1AB | 109.5 | C32—C32A—H32A | 115.9 |
H1AA—C1A—H1AB | 109.5 | C32B—C32A—H32B | 109.5 |
C1—C1A—H1AC | 109.5 | C32—C32A—H32B | 132.7 |
H1AA—C1A—H1AC | 109.5 | H32A—C32A—H32B | 109.5 |
H1AB—C1A—H1AC | 109.5 | C32B—C32A—H32C | 109.5 |
C1—C2—C3 | 107.4 (8) | C32—C32A—H32C | 42.7 |
C1—C2—C2A | 127.7 (9) | H32A—C32A—H32C | 109.5 |
C3—C2—C2A | 124.9 (9) | H32B—C32A—H32C | 109.5 |
C1—C2—Ta1 | 72.5 (5) | C32A—C32B—C32 | 81 (3) |
C3—C2—Ta1 | 72.5 (5) | C32A—C32B—H32D | 109.5 |
C2A—C2—Ta1 | 122.4 (6) | C32—C32B—H32D | 113.2 |
C2—C2A—H2AA | 109.5 | C32A—C32B—H32E | 109.5 |
C2—C2A—H2AB | 109.5 | C32—C32B—H32E | 30.0 |
H2AA—C2A—H2AB | 109.5 | H32D—C32B—H32E | 109.5 |
C2—C2A—H2AC | 109.5 | C32A—C32B—H32F | 109.5 |
H2AA—C2A—H2AC | 109.5 | C32—C32B—H32F | 129.4 |
H2AB—C2A—H2AC | 109.5 | H32D—C32B—H32F | 109.5 |
C4—C3—C2 | 108.3 (8) | H32E—C32B—H32F | 109.5 |
C4—C3—C3A | 127.1 (9) | C32—C33—C34 | 106.2 (10) |
C2—C3—C3A | 124.5 (9) | C32—C33—C33B | 117.0 (11) |
C4—C3—Ta1 | 71.5 (5) | C34—C33—C33B | 136.7 (11) |
C2—C3—Ta1 | 73.7 (5) | C32—C33—C33A | 153.1 (14) |
C3A—C3—Ta1 | 123.2 (7) | C34—C33—C33A | 100.6 (12) |
C3—C3A—H3AA | 109.5 | C33B—C33—C33A | 36.6 (10) |
C3—C3A—H3AB | 109.5 | C32—C33—Ta2 | 74.6 (7) |
H3AA—C3A—H3AB | 109.5 | C34—C33—Ta2 | 70.7 (6) |
C3—C3A—H3AC | 109.5 | C33B—C33—Ta2 | 116.8 (9) |
H3AA—C3A—H3AC | 109.5 | C33A—C33—Ta2 | 118.1 (11) |
H3AB—C3A—H3AC | 109.5 | C33B—C33A—C33 | 69.9 (19) |
C5—C4—C3 | 107.7 (8) | C33B—C33A—H33A | 109.5 |
C5—C4—C4A | 126.4 (9) | C33—C33A—H33A | 116.6 |
C3—C4—C4A | 125.8 (9) | C33B—C33A—H33B | 109.5 |
C5—C4—Ta1 | 72.9 (5) | C33—C33A—H33B | 131.2 |
C3—C4—Ta1 | 74.5 (5) | H33A—C33A—H33B | 109.5 |
C4A—C4—Ta1 | 120.4 (7) | C33B—C33A—H33C | 109.5 |
C4—C4A—H4AA | 109.5 | C33—C33A—H33C | 40.3 |
C4—C4A—H4AB | 109.5 | H33A—C33A—H33C | 109.5 |
H4AA—C4A—H4AB | 109.5 | H33B—C33A—H33C | 109.5 |
C4—C4A—H4AC | 109.5 | C33A—C33B—C33 | 73 (2) |
H4AA—C4A—H4AC | 109.5 | C33A—C33B—H33D | 109.5 |
H4AB—C4A—H4AC | 109.5 | C33—C33B—H33D | 115.6 |
C4—C5—C1 | 107.7 (8) | C33A—C33B—H33E | 109.5 |
C4—C5—C5A | 126.9 (8) | C33—C33B—H33E | 36.9 |
C1—C5—C5A | 125.0 (8) | H33D—C33B—H33E | 109.5 |
C4—C5—Ta1 | 73.2 (5) | C33A—C33B—H33F | 109.5 |
C1—C5—Ta1 | 74.1 (5) | C33—C33B—H33F | 130.7 |
C5A—C5—Ta1 | 123.7 (6) | H33D—C33B—H33F | 109.5 |
C5—C5A—H5AA | 109.5 | H33E—C33B—H33F | 109.5 |
C5—C5A—H5AB | 109.5 | C30—C34—C33 | 107.3 (10) |
H5AA—C5A—H5AB | 109.5 | C30—C34—C34B | 138.9 (10) |
C5—C5A—H5AC | 109.5 | C33—C34—C34B | 113.6 (9) |
H5AA—C5A—H5AC | 109.5 | C30—C34—C34A | 107.9 (12) |
H5AB—C5A—H5AC | 109.5 | C33—C34—C34A | 143.6 (13) |
C6—O1—Ta1 | 145.4 (6) | C34B—C34—C34A | 31.0 (9) |
O1—C6—C7 | 120.5 (9) | C30—C34—Ta2 | 75.2 (7) |
O1—C6—C11 | 122.8 (9) | C33—C34—Ta2 | 75.3 (6) |
C7—C6—C11 | 116.6 (9) | C34B—C34—Ta2 | 119.3 (7) |
F7—C7—C6 | 119.3 (9) | C34A—C34—Ta2 | 122.8 (11) |
F7—C7—C8 | 117.9 (9) | C34B—C34A—C34 | 72.3 (17) |
C6—C7—C8 | 122.6 (10) | C34B—C34A—H34A | 109.5 |
F8—C8—C9 | 121.2 (9) | C34—C34A—H34A | 114.5 |
F8—C8—C7 | 119.6 (9) | C34B—C34A—H34B | 109.5 |
C9—C8—C7 | 119.1 (9) | C34—C34A—H34B | 132.3 |
F9—C9—C10 | 121.0 (10) | H34A—C34A—H34B | 109.5 |
F9—C9—C8 | 119.3 (9) | C34B—C34A—H34C | 109.5 |
C10—C9—C8 | 119.7 (10) | C34—C34A—H34C | 38.3 |
F10—C10—C9 | 119.3 (9) | H34A—C34A—H34C | 109.5 |
F10—C10—C11 | 121.2 (9) | H34B—C34A—H34C | 109.5 |
C9—C10—C11 | 119.5 (10) | C34A—C34B—C34 | 76.7 (18) |
F11—C11—C6 | 120.7 (9) | C34A—C34B—H34D | 109.5 |
F11—C11—C10 | 116.9 (9) | C34—C34B—H34D | 114.6 |
C6—C11—C10 | 122.4 (9) | C34A—C34B—H34E | 109.5 |
C12—O2—Ta2 | 162.8 (6) | C34—C34B—H34E | 33.8 |
O2—C12—C13 | 122.6 (9) | H34D—C34B—H34E | 109.5 |
O2—C12—C17 | 123.6 (9) | C34A—C34B—H34F | 109.5 |
C13—C12—C17 | 113.8 (9) | C34—C34B—H34F | 130.1 |
F13—C13—C14 | 118.1 (9) | H34D—C34B—H34F | 109.5 |
F13—C13—C12 | 117.3 (9) | H34E—C34B—H34F | 109.5 |
C14—C13—C12 | 124.6 (10) | C36—C35—C40 | 118.5 (4) |
F14—C14—C13 | 120.5 (11) | C36—C35—C41 | 114.2 (3) |
F14—C14—C15 | 119.1 (10) | C40—C35—C41 | 127.3 (6) |
C13—C14—C15 | 120.4 (10) | C35—C36—C37 | 120.0 |
F15—C15—C16 | 121.0 (11) | C35—C36—H36A | 120.0 |
F15—C15—C14 | 121.5 (10) | C37—C36—H36A | 120.0 |
C16—C15—C14 | 117.5 (10) | C36—C37—C38 | 121.5 (4) |
F16—C16—C15 | 120.3 (11) | C36—C37—H37A | 119.2 |
F16—C16—C17 | 117.7 (11) | C38—C37—H37A | 119.2 |
C15—C16—C17 | 122.0 (11) | C39—C38—C37 | 118.5 (4) |
F17—C17—C12 | 119.5 (9) | C39—C38—H38A | 120.8 |
F17—C17—C16 | 118.7 (10) | C37—C38—H38A | 120.8 |
C12—C17—C16 | 121.8 (10) | C38—C39—C40 | 120.0 |
C18—O3—Ta2 | 134.5 (6) | C38—C39—H39A | 120.0 |
O3—C18—C23 | 122.9 (9) | C40—C39—H39A | 120.0 |
O3—C18—C19 | 121.5 (9) | C39—C40—C35 | 121.5 (4) |
C23—C18—C19 | 115.5 (9) | C39—C40—H40A | 119.2 |
F19—C19—C20 | 118.3 (9) | C35—C40—H40A | 119.2 |
F19—C19—C18 | 119.5 (8) | C35—C41—H41A | 109.5 |
C20—C19—C18 | 122.2 (9) | C35—C41—H41B | 109.5 |
F20—C20—C21 | 121.2 (9) | H41A—C41—H41B | 109.5 |
F20—C20—C19 | 119.0 (9) | C35—C41—H41C | 109.5 |
C21—C20—C19 | 119.8 (10) | H41A—C41—H41C | 109.5 |
F21—C21—C20 | 120.5 (9) | H41B—C41—H41C | 109.5 |
Experimental details
(final) | (combined) | (xmas1) | (95srv082) | |
Crystal data | ||||
Chemical formula | C23H22F5O2Ta | C24H46NTa | C34H15F20O4Ta | C44H30F20O6Ta2.C7H8 |
Mr | 606.36 | 529.57 | 1048.41 | 1488.71 |
Crystal system, space group | Triclinic, P1 | Monoclinic, P21/c | Orthorhombic, Pbcm | Monoclinic, P21/n |
Temperature (K) | 150 | 150 | 150 | 150 |
a, b, c (Å) | 9.239 (2), 11.647 (2), 11.803 (2) | 9.083 (2), 16.216 (3), 16.872 (3) | 8.341 (2), 26.389 (5), 15.145 (3) | 12.793 (2), 15.242 (2), 25.708 (3) |
α, β, γ (°) | 117.25 (3), 96.37 (3), 106.63 (3) | 90, 99.76 (3), 90 | 90, 90, 90 | 90, 100.178 (5), 90 |
V (Å3) | 1037.3 (3) | 2449.1 (8) | 3333.6 (12) | 4933.9 (12) |
Z | 2 | 4 | 4 | 4 |
Radiation type | Mo Kα | Mo Kα | Mo Kα | Mo Kα |
µ (mm−1) | 5.36 | 4.50 | 3.45 | 4.56 |
Crystal size (mm) | 0.80 × 0.64 × 0.44 | 0.26 × 0.24 × 0.20 | 0.46 × 0.12 × 0.08 | 0.8 × 0.45 × 0.3 |
Data collection | ||||
Diffractometer | Siemens P4 diffractometer | Siemens P4 diffractometer | Siemens P4 diffractometer | Siemens SMART CCD diffractometer |
Absorption correction | Empirical (using intensity measurements) | Empirical (using intensity measurements) | Empirical (using intensity measurements) | Empirical (using intensity measurements) |
Tmin, Tmax | 0.261, 1.000 | 0.267, 0.365 | 0.674, 0.770 | 0.343, 0.447 |
No. of measured, independent and observed [I > 2σ(I)] reflections | 3942, 3310, 2985 | 13104, 10777, 7822 | 3749, 3043, 2150 | 17825, 6926, 6101 |
Rint | 0.145 | 0.030 | 0.054 | 0.053 |
θmax (°) | 25.0 | 35.0 | 25.0 | 23.3 |
(sin θ/λ)max (Å−1) | 0.595 | 0.807 | 0.595 | 0.556 |
Refinement | ||||
R[F2 > 2σ(F2)], wR(F2), S | 0.073, 0.182, 1.02 | 0.038, 0.064, 1.03 | 0.045, 0.101, 1.01 | 0.063, 0.094, 2.26 |
No. of reflections | 3309 | 10777 | 3043 | 6922 |
No. of parameters | 221 | 247 | 283 | 619 |
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 | Riding | Riding |
Δρmax, Δρmin (e Å−3) | 5.30, −3.77 | 1.10, −0.79 | 0.85, −1.09 | 1.32, −0.96 |
Computer programs: Siemens XSCANS, Siemens SMART, Siemens SAINT, SHELXS86 (Sheldrick, 1990), SHELXL93 (Sheldrick, 1993), SHELXTL-Plus, SHELXL93.
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