Reduction of bis(naphthalene)vanadium(0) by potassium naphthalene (KNp) in tetrahydrofuran (THF) provides a highly reactive, thermolabile, and so far unisolable brown substance, which affords the first reported derivatives of bis(naphthalene)vanadates. From these solutions, thermally stable (298 K) and structurally characterized compounds have been obtained, including dark-red rods of catena-poly[bis(μ3-η4:η6:η4-naphthalene)tetrakis(tetrahydrofuran)dipotassiumvanadium], [K2V(C4H8O)4(C10H8)2]n or [K(THF)2]2[V(C10H8)2] (3), and red plates of (4,7,13,16,21,24-hexaoxa-1,10-diazabicyclo[8.8.8]hexacosane)potassium [1,2-bis(dimethylphosphanyl)ethane]bis(η4-naphthalene)vanadium tetrahydrofuran monosolvate, [K(C18H36N2O6)][V(C10H8)2(C6H16P2)]·C4H8O or [K([2.2.2]cryptand)][V(C10H8)2(dmpe)]·THF [dmpe is 1,2-bis(dimethylphosphanyl)ethane] (4b). Notably, [V(C10H8)2]2− is the only example of a structurally authenticated homoleptic bis(arene)metallate dianion and was obtained by further reduction of the brown material by KNp in THF, in the presence of trimethylphosphane (PMe3). Addition of anthracene (An) to the brown material in THF afforded deep-violet and paramagnetic crystalline (1,4,7,10,13,16-hexaoxacyclooctadecane)bis(tetrahydrofuran)potassium [(η4-anthracene)(tetrahydrofuran)vanadium]-μ-η4:η2-anthracene-[(1,4,7,10,13,16-hexaoxacyclooctadecane)potassium]-μ-η2:η4-anthracene-[(η4-anthracene)(tetrahydrofuran)vanadium] tetrahydrofuran disolvate, [K(C12H24O6)(C4H8O)2][KV2(C12H24O6)(C4H8O)2(C14H10)4]·2C4H8O or [K(18-crown-6)][K(18-crown-6)(THF)2][V(C14H10)2(THF)]2·2(THF) (5), which readily reacted with PMe3 and dmpe to give new vanadate salts. These were structurally characterized as (1,4,7,10,13,16-hexaoxacyclooctadecane)bis(tetrahydrofuran)potassium bis(η4-anthracene)(trimethylphosphane)vanadium tetrahydrofuran monosolvate, [K(C12H24O6)(C4H8O)2][V(C14H10)2(C3H9P)]·C4H8O or [K(18-crown-6)(THF)2][V(C14H10)2(PMe3)]·THF (6), and tetrakis(1,2-dimethoxyethane)potassium bis(η4-anthracene)[1,2-bis(dimethylphosphanyl)ethane]vanadium, [K(C4H10O2)4][V(C14H10)2(C6H16P2)] or [K(DME)4][V(C14H10)2(dmpe)] (DME is 1,2-dimethoxyethane) (7b). The last three structures contain the first known bis(anthracene)vanadates and are thereby derivatives of the unknown bis(anthracene)vanadium(0). Attempts to obtain the sodium salt analog of 5 in THF resulted instead in the formation of a unique substance, (μ3-η6:η6:η6-anthracene)(μ2-η6:η6-anthracene)tris(tetrahydrofuran)sodiumdivanadium, [NaV2(C14H10)2(C4H8O)3] or [Na(THF)3][V2(C14H10)2] (8), containing the first reported dimetallabis(anthracene) sandwich compound.
Supporting information
CCDC references: 2149661; 2149660; 2149659; 2149658; 2149657; 2149656
For all structures, data collection: SMART (Bruker, 2003); cell refinement: SAINT (Bruker, 2003); data reduction: SAINT (Bruker, 2003). Program(s) used to solve structure: SHELXS97 (Sheldrick, 2008) for (3), (4b), (5), (7b); SIR97 (Altomare et al., 1999) for (6), (8). For all structures, program(s) used to refine structure: SHELXL2018 (Sheldrick, 2015); molecular graphics: SHELXTL (Sheldrick, 2008); software used to prepare material for publication: SHELXTL (Sheldrick, 2008).
catena-Poly[bis(µ-
3η4:
η6:
η4-naphthalene)tetrakis(tetrahydrofuran)dipotassiumvanadium] (3)
top
Crystal data top
[K2V(C4H8O)4(C10H8)2] | F(000) = 1428 |
Mr = 673.88 | Dx = 1.299 Mg m−3 |
Monoclinic, P21/c | Mo Kα radiation, λ = 0.71073 Å |
a = 10.985 (2) Å | Cell parameters from 3155 reflections |
b = 17.243 (4) Å | θ = 2.3–24.9° |
c = 18.532 (4) Å | µ = 0.57 mm−1 |
β = 101.014 (3)° | T = 173 K |
V = 3445.5 (13) Å3 | Rod, red |
Z = 4 | 0.50 × 0.25 × 0.20 mm |
Data collection top
Siemens SMART CCD platform diffractometer | 4007 reflections with I > 2σ(I) |
Radiation source: normal-focus sealed tube | Rint = 0.046 |
ω scans | θmax = 25.1°, θmin = 1.6° |
Absorption correction: multi-scan (SADABS; Sheldrick, 1996) | h = −13→13 |
Tmin = 0.765, Tmax = 0.895 | k = −20→20 |
27058 measured reflections | l = −22→22 |
6104 independent reflections | |
Refinement top
Refinement on F2 | Primary atom site location: structure-invariant direct methods |
Least-squares matrix: full | Secondary atom site location: difference Fourier map |
R[F2 > 2σ(F2)] = 0.047 | Hydrogen site location: mixed |
wR(F2) = 0.120 | H atoms treated by a mixture of independent and constrained refinement |
S = 1.02 | w = 1/[σ2(Fo2) + (0.0525P)2 + 1.6694P] where P = (Fo2 + 2Fc2)/3 |
6104 reflections | (Δ/σ)max = 0.001 |
557 parameters | Δρmax = 0.38 e Å−3 |
381 restraints | Δρmin = −0.24 e Å−3 |
Special details top
Geometry. All esds (except the esd in the dihedral angle between two l.s. planes)
are estimated using the full covariance matrix. The cell esds are taken
into account individually in the estimation of esds in distances, angles
and torsion angles; correlations between esds in cell parameters are only
used when they are defined by crystal symmetry. An approximate (isotropic)
treatment of cell esds is used for estimating esds involving l.s. planes. |
Refinement. The hydrogen atoms on the metal-coordinating carbon atoms were
refined freely to confirm their nature and better describe their
true positions. THF ligand O2/C25-C28 is modeled as disordered over two
positions (0.63 (1):0.37 (1) and THF ligands O3/C29-C32 and
O4/C33-C36 are modeled pairwise as disordered over two
positions (0.605 (5):0.395 (5)). Analogous bond lengths and angles among the disordered THF
ligands were restrained to be similar. Anisotropic displacement
parameters for proximal atoms were restrained to be similar and
restrained toward the expected motion relative to bond direction. |
Fractional atomic coordinates and isotropic or equivalent isotropic displacement parameters (Å2) top | x | y | z | Uiso*/Ueq | Occ. (<1) |
V1 | 0.60377 (5) | 0.46032 (3) | 0.26181 (3) | 0.04505 (16) | |
K1 | 0.89151 (6) | 0.53261 (4) | 0.23117 (4) | 0.0515 (2) | |
K2 | 0.51676 (7) | 0.72934 (4) | 0.34219 (5) | 0.0631 (2) | |
O1 | 1.0749 (2) | 0.47831 (16) | 0.34131 (14) | 0.0802 (8) | |
C1 | 0.5698 (3) | 0.58844 (17) | 0.2404 (2) | 0.0475 (8) | |
H1A | 0.532 (2) | 0.6054 (16) | 0.1984 (15) | 0.036 (8)* | |
C2 | 0.5014 (3) | 0.55658 (18) | 0.2926 (2) | 0.0545 (9) | |
H2A | 0.414 (3) | 0.5553 (15) | 0.2846 (14) | 0.043 (8)* | |
C3 | 0.5707 (4) | 0.5259 (2) | 0.3554 (2) | 0.0622 (10) | |
H3A | 0.538 (3) | 0.5036 (17) | 0.3935 (16) | 0.052 (9)* | |
C4 | 0.7038 (3) | 0.5283 (2) | 0.36138 (19) | 0.0569 (9) | |
H4A | 0.751 (3) | 0.5050 (19) | 0.4024 (17) | 0.062 (10)* | |
C5 | 0.8663 (3) | 0.63372 (19) | 0.36505 (18) | 0.0610 (9) | |
H5A | 0.913066 | 0.615032 | 0.410173 | 0.073* | |
C6 | 0.9119 (3) | 0.6962 (2) | 0.3288 (2) | 0.0639 (9) | |
H6A | 0.990652 | 0.717916 | 0.348691 | 0.077* | |
C7 | 0.8444 (3) | 0.72529 (18) | 0.2662 (2) | 0.0588 (9) | |
H7A | 0.876482 | 0.766749 | 0.241724 | 0.071* | |
C8 | 0.7285 (3) | 0.69490 (16) | 0.23752 (18) | 0.0497 (8) | |
H8A | 0.679141 | 0.718337 | 0.195488 | 0.060* | |
C9 | 0.6831 (3) | 0.63054 (15) | 0.26935 (17) | 0.0438 (7) | |
C10 | 0.7537 (3) | 0.59936 (17) | 0.33517 (17) | 0.0489 (8) | |
C11 | 0.5071 (3) | 0.40996 (18) | 0.15909 (19) | 0.0496 (8) | |
H11A | 0.465 (2) | 0.4385 (16) | 0.1198 (14) | 0.039 (8)* | |
C12 | 0.4510 (3) | 0.38680 (18) | 0.2191 (2) | 0.0544 (9) | |
H12A | 0.362 (3) | 0.4005 (17) | 0.2165 (16) | 0.058 (9)* | |
C13 | 0.5250 (4) | 0.3507 (2) | 0.2808 (2) | 0.0660 (10) | |
H13A | 0.487 (3) | 0.338 (2) | 0.3184 (18) | 0.071 (11)* | |
C14 | 0.6520 (4) | 0.33763 (19) | 0.2823 (2) | 0.0682 (10) | |
H14A | 0.698 (3) | 0.3187 (19) | 0.3267 (18) | 0.067 (11)* | |
C15 | 0.8399 (3) | 0.35185 (19) | 0.2242 (3) | 0.0749 (11) | |
H15A | 0.890613 | 0.328091 | 0.265561 | 0.090* | |
C16 | 0.8943 (3) | 0.3750 (2) | 0.1675 (3) | 0.0767 (12) | |
H16A | 0.979944 | 0.365644 | 0.169020 | 0.092* | |
C17 | 0.8234 (3) | 0.4124 (2) | 0.1076 (2) | 0.0670 (10) | |
H17A | 0.860791 | 0.428960 | 0.068062 | 0.080* | |
C18 | 0.6991 (3) | 0.42570 (19) | 0.10516 (19) | 0.0571 (8) | |
H18A | 0.653396 | 0.453405 | 0.064535 | 0.069* | |
C19 | 0.6367 (3) | 0.39973 (16) | 0.16074 (17) | 0.0462 (7) | |
C20 | 0.7114 (3) | 0.36129 (16) | 0.2248 (2) | 0.0557 (9) | |
C21 | 1.0407 (4) | 0.4390 (3) | 0.4016 (2) | 0.0970 (14) | |
H21A | 0.952829 | 0.422615 | 0.389396 | 0.116* | |
H21B | 1.051782 | 0.473283 | 0.445266 | 0.116* | |
C22 | 1.1208 (6) | 0.3725 (3) | 0.4160 (3) | 0.1160 (18) | |
H22A | 1.086642 | 0.327837 | 0.385033 | 0.139* | |
H22B | 1.133605 | 0.357110 | 0.468384 | 0.139* | |
C23 | 1.2384 (4) | 0.4007 (3) | 0.3962 (3) | 0.1117 (17) | |
H23A | 1.286676 | 0.357349 | 0.380660 | 0.134* | |
H23B | 1.290423 | 0.428246 | 0.437872 | 0.134* | |
C24 | 1.1931 (4) | 0.4546 (3) | 0.3338 (3) | 0.0910 (13) | |
H24A | 1.249070 | 0.499875 | 0.335794 | 0.109* | |
H24B | 1.189698 | 0.427776 | 0.286212 | 0.109* | |
O2 | 1.0782 (10) | 0.5714 (7) | 0.1649 (8) | 0.077 (4) | 0.628 (11) |
C25 | 1.1445 (11) | 0.6423 (6) | 0.1751 (7) | 0.089 (3) | 0.628 (11) |
H25A | 1.196309 | 0.644788 | 0.225009 | 0.107* | 0.628 (11) |
H25B | 1.086505 | 0.686833 | 0.168724 | 0.107* | 0.628 (11) |
C26 | 1.2256 (7) | 0.6442 (4) | 0.1171 (6) | 0.085 (3) | 0.628 (11) |
H26A | 1.181898 | 0.669125 | 0.071303 | 0.102* | 0.628 (11) |
H26B | 1.304246 | 0.672067 | 0.135197 | 0.102* | 0.628 (11) |
C27 | 1.2479 (10) | 0.5612 (6) | 0.1054 (6) | 0.066 (2) | 0.628 (11) |
H27A | 1.323111 | 0.542914 | 0.139373 | 0.079* | 0.628 (11) |
H27B | 1.257945 | 0.551530 | 0.054154 | 0.079* | 0.628 (11) |
C28 | 1.1347 (12) | 0.5218 (6) | 0.1208 (9) | 0.071 (3) | 0.628 (11) |
H28A | 1.076603 | 0.510605 | 0.074238 | 0.085* | 0.628 (11) |
H28B | 1.157562 | 0.472195 | 0.146758 | 0.085* | 0.628 (11) |
O2' | 1.0493 (15) | 0.5847 (11) | 0.1508 (12) | 0.062 (4) | 0.372 (11) |
C25' | 1.1012 (13) | 0.6599 (10) | 0.1630 (13) | 0.084 (4) | 0.372 (11) |
H25C | 1.075843 | 0.684844 | 0.205892 | 0.101* | 0.372 (11) |
H25D | 1.075714 | 0.693231 | 0.119217 | 0.101* | 0.372 (11) |
C26' | 1.2389 (10) | 0.6449 (6) | 0.1772 (10) | 0.073 (4) | 0.372 (11) |
H26C | 1.284395 | 0.689728 | 0.162031 | 0.087* | 0.372 (11) |
H26D | 1.270876 | 0.633921 | 0.229895 | 0.087* | 0.372 (11) |
C27' | 1.2501 (15) | 0.5762 (10) | 0.1314 (12) | 0.073 (4) | 0.372 (11) |
H27C | 1.307517 | 0.537811 | 0.159423 | 0.088* | 0.372 (11) |
H27D | 1.282236 | 0.591282 | 0.087006 | 0.088* | 0.372 (11) |
C28' | 1.1218 (18) | 0.5422 (11) | 0.1101 (14) | 0.068 (5) | 0.372 (11) |
H28C | 1.089952 | 0.548266 | 0.056662 | 0.082* | 0.372 (11) |
H28D | 1.121993 | 0.486447 | 0.122717 | 0.082* | 0.372 (11) |
O3 | 0.3573 (4) | 0.6626 (3) | 0.4086 (3) | 0.0710 (14) | 0.604 (5) |
C29 | 0.2338 (5) | 0.6844 (4) | 0.4020 (3) | 0.075 (2) | 0.604 (5) |
H29A | 0.180861 | 0.653229 | 0.363294 | 0.090* | 0.604 (5) |
H29B | 0.223405 | 0.739839 | 0.388463 | 0.090* | 0.604 (5) |
C30 | 0.1983 (8) | 0.6705 (7) | 0.4739 (5) | 0.092 (4) | 0.604 (5) |
H30A | 0.145922 | 0.623610 | 0.472332 | 0.110* | 0.604 (5) |
H30B | 0.152348 | 0.715465 | 0.488529 | 0.110* | 0.604 (5) |
C31 | 0.3186 (7) | 0.6598 (5) | 0.5258 (4) | 0.084 (2) | 0.604 (5) |
H31A | 0.350566 | 0.709832 | 0.547906 | 0.100* | 0.604 (5) |
H31B | 0.309760 | 0.623139 | 0.565632 | 0.100* | 0.604 (5) |
C32 | 0.4003 (9) | 0.6281 (7) | 0.4791 (7) | 0.082 (3) | 0.604 (5) |
H32A | 0.487790 | 0.642278 | 0.498436 | 0.099* | 0.604 (5) |
H32B | 0.393513 | 0.570884 | 0.476172 | 0.099* | 0.604 (5) |
O3' | 0.3946 (8) | 0.6921 (4) | 0.4571 (6) | 0.095 (3) | 0.396 (5) |
C29' | 0.3557 (13) | 0.6183 (8) | 0.4831 (11) | 0.078 (4) | 0.396 (5) |
H29C | 0.368153 | 0.575811 | 0.449358 | 0.094* | 0.396 (5) |
H29D | 0.403299 | 0.606444 | 0.532818 | 0.094* | 0.396 (5) |
C30' | 0.2248 (13) | 0.6279 (7) | 0.4847 (11) | 0.104 (5) | 0.396 (5) |
H30C | 0.203072 | 0.600588 | 0.527470 | 0.125* | 0.396 (5) |
H30D | 0.172900 | 0.607138 | 0.439201 | 0.125* | 0.396 (5) |
C31' | 0.2058 (13) | 0.7140 (7) | 0.4906 (11) | 0.098 (5) | 0.396 (5) |
H31C | 0.144162 | 0.733235 | 0.448250 | 0.118* | 0.396 (5) |
H31D | 0.176879 | 0.726932 | 0.536562 | 0.118* | 0.396 (5) |
C32' | 0.3261 (13) | 0.7472 (6) | 0.4906 (10) | 0.146 (7) | 0.396 (5) |
H32C | 0.317622 | 0.796429 | 0.462536 | 0.175* | 0.396 (5) |
H32D | 0.369103 | 0.758135 | 0.541548 | 0.175* | 0.396 (5) |
O4 | 0.6532 (10) | 0.7695 (8) | 0.4719 (5) | 0.081 (3) | 0.604 (5) |
C33 | 0.5826 (8) | 0.8098 (4) | 0.5175 (4) | 0.074 (2) | 0.604 (5) |
H33A | 0.573565 | 0.777578 | 0.560354 | 0.089* | 0.604 (5) |
H33B | 0.498894 | 0.822341 | 0.489385 | 0.089* | 0.604 (5) |
C34 | 0.6511 (8) | 0.8813 (4) | 0.5419 (4) | 0.082 (2) | 0.604 (5) |
H34A | 0.645012 | 0.894396 | 0.593078 | 0.098* | 0.604 (5) |
H34B | 0.619777 | 0.925516 | 0.509480 | 0.098* | 0.604 (5) |
C35 | 0.7822 (12) | 0.8614 (8) | 0.5362 (7) | 0.113 (4) | 0.604 (5) |
H35A | 0.830387 | 0.908482 | 0.529361 | 0.135* | 0.604 (5) |
H35B | 0.824942 | 0.833137 | 0.580330 | 0.135* | 0.604 (5) |
C36 | 0.7641 (12) | 0.8116 (8) | 0.4706 (7) | 0.092 (3) | 0.604 (5) |
H36A | 0.755470 | 0.843387 | 0.425357 | 0.110* | 0.604 (5) |
H36B | 0.835180 | 0.775876 | 0.472453 | 0.110* | 0.604 (5) |
O4' | 0.6862 (15) | 0.7764 (13) | 0.4608 (8) | 0.086 (4) | 0.396 (5) |
C33' | 0.6584 (12) | 0.8078 (9) | 0.5278 (8) | 0.096 (4) | 0.396 (5) |
H33C | 0.646994 | 0.764953 | 0.561446 | 0.115* | 0.396 (5) |
H33D | 0.580126 | 0.837739 | 0.516681 | 0.115* | 0.396 (5) |
C34' | 0.7586 (19) | 0.8581 (11) | 0.5633 (8) | 0.095 (5) | 0.396 (5) |
H34C | 0.815621 | 0.830298 | 0.602714 | 0.114* | 0.396 (5) |
H34D | 0.726068 | 0.904743 | 0.584278 | 0.114* | 0.396 (5) |
C35' | 0.8203 (18) | 0.8784 (11) | 0.5026 (8) | 0.148 (6) | 0.396 (5) |
H35C | 0.786849 | 0.927703 | 0.479668 | 0.177* | 0.396 (5) |
H35D | 0.910597 | 0.884500 | 0.520645 | 0.177* | 0.396 (5) |
C36' | 0.796 (2) | 0.8156 (14) | 0.4500 (12) | 0.103 (5) | 0.396 (5) |
H36C | 0.784882 | 0.836368 | 0.399278 | 0.124* | 0.396 (5) |
H36D | 0.867413 | 0.779209 | 0.457402 | 0.124* | 0.396 (5) |
Atomic displacement parameters (Å2) top | U11 | U22 | U33 | U12 | U13 | U23 |
V1 | 0.0455 (3) | 0.0338 (3) | 0.0565 (3) | −0.0086 (2) | 0.0115 (2) | 0.0009 (2) |
K1 | 0.0487 (4) | 0.0441 (4) | 0.0645 (5) | −0.0022 (3) | 0.0179 (3) | −0.0012 (3) |
K2 | 0.0664 (5) | 0.0341 (4) | 0.0940 (6) | −0.0006 (3) | 0.0288 (4) | −0.0033 (4) |
O1 | 0.0587 (16) | 0.100 (2) | 0.0837 (18) | 0.0123 (14) | 0.0191 (13) | 0.0284 (15) |
C1 | 0.0447 (19) | 0.0376 (17) | 0.060 (2) | −0.0010 (14) | 0.0096 (16) | 0.0006 (16) |
C2 | 0.045 (2) | 0.0440 (18) | 0.080 (3) | −0.0138 (15) | 0.0267 (18) | −0.0123 (17) |
C3 | 0.079 (3) | 0.056 (2) | 0.059 (2) | −0.0249 (19) | 0.033 (2) | −0.0061 (18) |
C4 | 0.065 (2) | 0.054 (2) | 0.051 (2) | −0.0161 (17) | 0.0095 (18) | 0.0043 (17) |
C5 | 0.066 (2) | 0.060 (2) | 0.055 (2) | −0.0162 (18) | 0.0061 (17) | −0.0104 (17) |
C6 | 0.059 (2) | 0.056 (2) | 0.077 (3) | −0.0248 (18) | 0.0119 (19) | −0.0100 (19) |
C7 | 0.062 (2) | 0.0403 (18) | 0.079 (2) | −0.0133 (16) | 0.0241 (19) | −0.0014 (17) |
C8 | 0.0483 (19) | 0.0341 (16) | 0.070 (2) | 0.0000 (14) | 0.0195 (16) | 0.0006 (15) |
C9 | 0.0446 (17) | 0.0318 (15) | 0.059 (2) | −0.0048 (13) | 0.0214 (15) | −0.0100 (14) |
C10 | 0.056 (2) | 0.0444 (17) | 0.0495 (18) | −0.0118 (15) | 0.0175 (15) | −0.0103 (15) |
C11 | 0.049 (2) | 0.0357 (17) | 0.062 (2) | 0.0001 (14) | 0.0061 (17) | −0.0047 (16) |
C12 | 0.047 (2) | 0.0384 (17) | 0.080 (3) | −0.0116 (15) | 0.0168 (18) | −0.0129 (17) |
C13 | 0.074 (3) | 0.048 (2) | 0.079 (3) | −0.0250 (19) | 0.023 (2) | 0.0017 (19) |
C14 | 0.069 (3) | 0.0408 (19) | 0.089 (3) | −0.0083 (18) | 0.000 (2) | 0.0233 (19) |
C15 | 0.053 (2) | 0.0324 (18) | 0.132 (4) | 0.0077 (16) | −0.001 (2) | 0.013 (2) |
C16 | 0.051 (2) | 0.0359 (19) | 0.147 (4) | 0.0028 (17) | 0.029 (3) | −0.013 (2) |
C17 | 0.061 (2) | 0.054 (2) | 0.094 (3) | −0.0091 (18) | 0.034 (2) | −0.026 (2) |
C18 | 0.059 (2) | 0.0510 (19) | 0.063 (2) | −0.0050 (16) | 0.0154 (17) | −0.0143 (16) |
C19 | 0.0444 (18) | 0.0276 (15) | 0.067 (2) | −0.0023 (13) | 0.0104 (15) | −0.0113 (14) |
C20 | 0.048 (2) | 0.0264 (15) | 0.088 (3) | −0.0009 (14) | 0.0032 (18) | 0.0067 (16) |
C21 | 0.101 (3) | 0.111 (4) | 0.088 (3) | 0.011 (3) | 0.041 (3) | 0.019 (3) |
C22 | 0.168 (5) | 0.099 (4) | 0.089 (3) | 0.026 (4) | 0.046 (3) | 0.026 (3) |
C23 | 0.075 (3) | 0.099 (4) | 0.148 (5) | 0.029 (3) | −0.011 (3) | 0.006 (3) |
C24 | 0.061 (2) | 0.104 (3) | 0.115 (3) | 0.009 (2) | 0.035 (2) | 0.007 (3) |
O2 | 0.076 (6) | 0.063 (4) | 0.103 (7) | −0.010 (4) | 0.049 (6) | −0.001 (4) |
C25 | 0.072 (8) | 0.064 (5) | 0.136 (7) | −0.002 (5) | 0.033 (6) | −0.025 (5) |
C26 | 0.073 (4) | 0.063 (4) | 0.122 (7) | −0.011 (3) | 0.028 (5) | 0.022 (5) |
C27 | 0.058 (4) | 0.078 (5) | 0.064 (6) | −0.012 (4) | 0.018 (4) | −0.010 (4) |
C28 | 0.074 (5) | 0.046 (5) | 0.103 (7) | 0.003 (4) | 0.041 (5) | 0.012 (4) |
O2' | 0.054 (6) | 0.056 (7) | 0.077 (7) | −0.011 (5) | 0.013 (5) | 0.000 (5) |
C25' | 0.053 (7) | 0.043 (7) | 0.156 (11) | −0.001 (6) | 0.021 (8) | 0.009 (6) |
C26' | 0.054 (6) | 0.044 (5) | 0.118 (9) | −0.003 (5) | 0.012 (7) | 0.002 (6) |
C27' | 0.049 (6) | 0.086 (9) | 0.084 (13) | −0.004 (6) | 0.012 (7) | −0.010 (7) |
C28' | 0.065 (7) | 0.054 (10) | 0.087 (9) | −0.015 (7) | 0.018 (6) | −0.001 (9) |
O3 | 0.069 (3) | 0.072 (3) | 0.077 (3) | 0.014 (2) | 0.028 (2) | 0.016 (3) |
C29 | 0.063 (4) | 0.091 (5) | 0.073 (4) | 0.029 (3) | 0.023 (3) | 0.022 (3) |
C30 | 0.067 (4) | 0.124 (11) | 0.086 (5) | 0.005 (6) | 0.019 (4) | 0.006 (8) |
C31 | 0.095 (5) | 0.088 (5) | 0.068 (4) | −0.005 (4) | 0.016 (3) | 0.008 (4) |
C32 | 0.079 (6) | 0.080 (6) | 0.089 (5) | 0.016 (5) | 0.016 (5) | 0.028 (4) |
O3' | 0.104 (6) | 0.061 (4) | 0.139 (7) | 0.006 (4) | 0.068 (5) | 0.004 (5) |
C29' | 0.097 (8) | 0.052 (5) | 0.085 (8) | 0.018 (6) | 0.017 (7) | −0.003 (5) |
C30' | 0.090 (8) | 0.101 (10) | 0.124 (11) | −0.009 (7) | 0.030 (8) | 0.004 (9) |
C31' | 0.086 (7) | 0.107 (11) | 0.100 (10) | 0.043 (7) | 0.014 (7) | 0.012 (9) |
C32' | 0.168 (11) | 0.058 (6) | 0.253 (18) | 0.026 (7) | 0.145 (13) | 0.025 (8) |
O4 | 0.116 (5) | 0.059 (4) | 0.069 (5) | 0.001 (4) | 0.020 (4) | −0.006 (3) |
C33 | 0.093 (6) | 0.061 (4) | 0.065 (4) | −0.005 (4) | 0.007 (4) | −0.005 (3) |
C34 | 0.119 (6) | 0.058 (4) | 0.065 (4) | −0.016 (4) | 0.010 (4) | 0.002 (3) |
C35 | 0.119 (6) | 0.124 (7) | 0.099 (9) | −0.049 (5) | 0.029 (7) | −0.013 (7) |
C36 | 0.100 (8) | 0.086 (6) | 0.089 (7) | 0.013 (5) | 0.016 (5) | 0.007 (5) |
O4' | 0.126 (10) | 0.066 (7) | 0.067 (6) | −0.002 (6) | 0.022 (7) | −0.004 (5) |
C33' | 0.100 (9) | 0.103 (9) | 0.085 (8) | −0.002 (8) | 0.022 (8) | −0.015 (7) |
C34' | 0.119 (11) | 0.077 (8) | 0.086 (9) | −0.012 (7) | 0.016 (8) | −0.010 (7) |
C35' | 0.199 (13) | 0.152 (11) | 0.096 (11) | −0.092 (10) | 0.039 (9) | −0.020 (8) |
C36' | 0.113 (11) | 0.102 (9) | 0.101 (11) | 0.005 (8) | 0.035 (7) | −0.011 (8) |
Geometric parameters (Å, º) top
V1—C12 | 2.131 (3) | C22—H22B | 0.9900 |
V1—C13 | 2.136 (3) | C23—C24 | 1.493 (6) |
V1—C2 | 2.142 (3) | C23—H23A | 0.9900 |
V1—C3 | 2.159 (3) | C23—H23B | 0.9900 |
V1—C11 | 2.176 (3) | C24—H24A | 0.9900 |
V1—C14 | 2.196 (4) | C24—H24B | 0.9900 |
V1—C19 | 2.234 (3) | O2—C28 | 1.405 (8) |
V1—C20 | 2.257 (3) | O2—C25 | 1.419 (9) |
V1—C1 | 2.263 (3) | C25—C26 | 1.521 (11) |
V1—C4 | 2.283 (3) | C25—H25A | 0.9900 |
V1—K1 | 3.5429 (10) | C25—H25B | 0.9900 |
K1—O2' | 2.648 (11) | C26—C27 | 1.475 (10) |
K1—O2 | 2.669 (7) | C26—H26A | 0.9900 |
K1—O1 | 2.744 (3) | C26—H26B | 0.9900 |
K1—C10 | 2.906 (3) | C27—C28 | 1.492 (10) |
K1—C16 | 2.965 (3) | C27—H27A | 0.9900 |
K1—C9 | 3.035 (3) | C27—H27B | 0.9900 |
K1—C17 | 3.073 (3) | C28—H28A | 0.9900 |
K1—C5 | 3.088 (3) | C28—H28B | 0.9900 |
K1—C15 | 3.166 (3) | O2'—C28' | 1.403 (12) |
K1—C6 | 3.336 (3) | O2'—C25' | 1.417 (12) |
K1—C8 | 3.337 (3) | C25'—C26' | 1.508 (13) |
K1—C18 | 3.381 (3) | C25'—H25C | 0.9900 |
K1—C7 | 3.443 (3) | C25'—H25D | 0.9900 |
K1—C4 | 3.462 (3) | C26'—C27' | 1.477 (13) |
K2—O3 | 2.595 (4) | C26'—H26C | 0.9900 |
K2—O4 | 2.670 (8) | C26'—H26D | 0.9900 |
K2—O4' | 2.718 (12) | C27'—C28' | 1.507 (14) |
K2—O3' | 2.800 (8) | C27'—H27C | 0.9900 |
K2—C12i | 2.990 (3) | C27'—H27D | 0.9900 |
K2—C9 | 3.001 (3) | C28'—H28C | 0.9900 |
K2—C13i | 3.064 (4) | C28'—H28D | 0.9900 |
K2—C2 | 3.112 (3) | O3—C29 | 1.390 (6) |
K2—C11i | 3.125 (3) | O3—C32 | 1.431 (10) |
K2—C1 | 3.197 (3) | C29—C30 | 1.479 (10) |
K2—C14i | 3.257 (4) | C29—H29A | 0.9900 |
K2—C8 | 3.354 (3) | C29—H29B | 0.9900 |
K2—C19i | 3.382 (3) | C30—C31 | 1.490 (11) |
K2—C20i | 3.436 (3) | C30—H30A | 0.9900 |
K2—C10 | 3.456 (3) | C30—H30B | 0.9900 |
O1—C24 | 1.394 (4) | C31—C32 | 1.467 (11) |
O1—C21 | 1.418 (4) | C31—H31A | 0.9900 |
C1—C2 | 1.442 (4) | C31—H31B | 0.9900 |
C1—C9 | 1.453 (4) | C32—H32A | 0.9900 |
C1—H1A | 0.86 (3) | C32—H32B | 0.9900 |
C2—C3 | 1.370 (5) | O3'—C32' | 1.426 (10) |
C2—H2A | 0.95 (3) | O3'—C29' | 1.454 (12) |
C3—C4 | 1.445 (5) | C29'—C30' | 1.453 (13) |
C3—H3A | 0.94 (3) | C29'—H29C | 0.9900 |
C4—C10 | 1.462 (4) | C29'—H29D | 0.9900 |
C4—H4A | 0.93 (3) | C30'—C31' | 1.507 (14) |
C5—C10 | 1.388 (4) | C30'—H30C | 0.9900 |
C5—C6 | 1.410 (5) | C30'—H30D | 0.9900 |
C5—H5A | 0.9500 | C31'—C32' | 1.440 (13) |
C6—C7 | 1.349 (5) | C31'—H31C | 0.9900 |
C6—H6A | 0.9500 | C31'—H31D | 0.9900 |
C7—C8 | 1.386 (4) | C32'—H32C | 0.9900 |
C7—H7A | 0.9500 | C32'—H32D | 0.9900 |
C8—C9 | 1.393 (4) | O4—C36 | 1.423 (9) |
C8—H8A | 0.9500 | O4—C33 | 1.432 (9) |
C9—C10 | 1.420 (4) | C33—C34 | 1.470 (9) |
C11—C12 | 1.427 (5) | C33—H33A | 0.9900 |
C11—C19 | 1.429 (4) | C33—H33B | 0.9900 |
C11—H11A | 0.93 (3) | C34—C35 | 1.504 (14) |
C12—C13 | 1.415 (5) | C34—H34A | 0.9900 |
C12—H12A | 1.00 (3) | C34—H34B | 0.9900 |
C13—C14 | 1.408 (5) | C35—C36 | 1.471 (11) |
C13—H13A | 0.90 (3) | C35—H35A | 0.9900 |
C14—C20 | 1.411 (5) | C35—H35B | 0.9900 |
C14—H14A | 0.94 (3) | C36—H36A | 0.9900 |
C15—C16 | 1.364 (5) | C36—H36B | 0.9900 |
C15—C20 | 1.424 (5) | O4'—C36' | 1.435 (12) |
C15—H15A | 0.9500 | O4'—C33' | 1.440 (12) |
C16—C17 | 1.387 (5) | C33'—C34' | 1.456 (13) |
C16—H16A | 0.9500 | C33'—H33C | 0.9900 |
C17—C18 | 1.377 (5) | C33'—H33D | 0.9900 |
C17—H17A | 0.9500 | C34'—C35' | 1.462 (16) |
C18—C19 | 1.415 (4) | C34'—H34C | 0.9900 |
C18—H18A | 0.9500 | C34'—H34D | 0.9900 |
C19—C20 | 1.466 (4) | C35'—C36' | 1.447 (13) |
C21—C22 | 1.440 (6) | C35'—H35C | 0.9900 |
C21—H21A | 0.9900 | C35'—H35D | 0.9900 |
C21—H21B | 0.9900 | C36'—H36C | 0.9900 |
C22—C23 | 1.490 (7) | C36'—H36D | 0.9900 |
C22—H22A | 0.9900 | | |
| | | |
C12—V1—C13 | 38.74 (13) | C6—C7—H7A | 119.9 |
C12—V1—C2 | 98.27 (13) | C8—C7—H7A | 119.9 |
C13—V1—C2 | 113.07 (15) | K1—C7—H7A | 123.6 |
C12—V1—C3 | 111.62 (13) | C7—C8—C9 | 121.0 (3) |
C13—V1—C3 | 101.24 (15) | C7—C8—K1 | 82.56 (19) |
C2—V1—C3 | 37.13 (13) | C9—C8—K1 | 65.44 (16) |
C12—V1—C11 | 38.69 (12) | C7—C8—K2 | 113.5 (2) |
C13—V1—C11 | 69.26 (14) | C9—C8—K2 | 63.43 (15) |
C2—V1—C11 | 110.44 (14) | K1—C8—K2 | 127.24 (9) |
C3—V1—C11 | 141.56 (14) | C7—C8—H8A | 119.5 |
C12—V1—C14 | 68.76 (14) | C9—C8—H8A | 119.5 |
C13—V1—C14 | 37.89 (14) | K1—C8—H8A | 123.6 |
C2—V1—C14 | 145.26 (14) | K2—C8—H8A | 92.8 |
C3—V1—C14 | 115.95 (16) | C8—C9—C10 | 119.0 (3) |
C11—V1—C14 | 80.08 (14) | C8—C9—C1 | 126.3 (3) |
C12—V1—C19 | 69.66 (12) | C10—C9—C1 | 114.6 (3) |
C13—V1—C19 | 81.95 (14) | C8—C9—K2 | 92.05 (17) |
C2—V1—C19 | 139.74 (13) | C10—C9—K2 | 96.18 (18) |
C3—V1—C19 | 176.25 (13) | C1—C9—K2 | 84.09 (17) |
C11—V1—C19 | 37.79 (11) | C8—C9—K1 | 89.89 (17) |
C14—V1—C19 | 67.78 (14) | C10—C9—K1 | 71.19 (16) |
C12—V1—C20 | 81.83 (12) | C1—C9—K1 | 105.51 (17) |
C13—V1—C20 | 68.45 (14) | K2—C9—K1 | 166.39 (12) |
C2—V1—C20 | 177.63 (14) | C5—C10—C9 | 118.7 (3) |
C3—V1—C20 | 144.95 (15) | C5—C10—C4 | 126.0 (3) |
C11—V1—C20 | 68.19 (12) | C9—C10—C4 | 115.1 (3) |
C14—V1—C20 | 36.92 (13) | C5—C10—K1 | 84.02 (19) |
C19—V1—C20 | 38.11 (11) | C9—C10—K1 | 81.27 (16) |
C12—V1—C1 | 115.07 (13) | C4—C10—K1 | 99.47 (19) |
C13—V1—C1 | 146.56 (14) | C5—C10—K2 | 109.2 (2) |
C2—V1—C1 | 38.09 (11) | C9—C10—K2 | 59.71 (16) |
C3—V1—C1 | 65.31 (14) | C4—C10—K2 | 101.4 (2) |
C11—V1—C1 | 101.52 (13) | K1—C10—K2 | 140.65 (11) |
C14—V1—C1 | 175.55 (13) | C12—C11—C19 | 121.7 (3) |
C19—V1—C1 | 110.94 (12) | C12—C11—V1 | 68.98 (19) |
C20—V1—C1 | 139.81 (12) | C19—C11—V1 | 73.31 (18) |
C12—V1—C4 | 145.98 (13) | C12—C11—K2ii | 71.28 (17) |
C13—V1—C4 | 117.94 (14) | C19—C11—K2ii | 87.64 (17) |
C2—V1—C4 | 65.32 (14) | V1—C11—K2ii | 115.51 (14) |
C3—V1—C4 | 37.84 (13) | C12—C11—H11A | 122.2 (17) |
C11—V1—C4 | 172.43 (13) | C19—C11—H11A | 115.5 (17) |
C14—V1—C4 | 107.01 (15) | V1—C11—H11A | 124.3 (17) |
C19—V1—C4 | 142.01 (12) | K2ii—C11—H11A | 119.6 (17) |
C20—V1—C4 | 115.81 (13) | C13—C12—C11 | 119.1 (3) |
C1—V1—C4 | 71.21 (13) | C13—C12—V1 | 70.82 (19) |
C12—V1—K1 | 144.39 (9) | C11—C12—V1 | 72.32 (18) |
C13—V1—K1 | 137.70 (12) | C13—C12—K2ii | 79.4 (2) |
C2—V1—K1 | 107.44 (9) | C11—C12—K2ii | 81.84 (18) |
C3—V1—K1 | 103.70 (9) | V1—C12—K2ii | 122.62 (14) |
C11—V1—K1 | 107.55 (9) | C13—C12—H12A | 123.3 (17) |
C14—V1—K1 | 100.00 (11) | C11—C12—H12A | 117.5 (17) |
C19—V1—K1 | 74.81 (8) | V1—C12—H12A | 124.9 (17) |
C20—V1—K1 | 71.49 (8) | K2ii—C12—H12A | 112.5 (17) |
C1—V1—K1 | 75.57 (8) | C14—C13—C12 | 120.0 (4) |
C4—V1—K1 | 69.06 (9) | C14—C13—V1 | 73.4 (2) |
O2'—K1—O1 | 93.9 (5) | C12—C13—V1 | 70.45 (19) |
O2—K1—O1 | 84.7 (3) | C14—C13—K2ii | 84.9 (2) |
O2'—K1—C10 | 135.9 (5) | C12—C13—K2ii | 73.6 (2) |
O2—K1—C10 | 138.5 (3) | V1—C13—K2ii | 119.29 (17) |
O1—K1—C10 | 92.48 (9) | C14—C13—H13A | 123 (2) |
O2'—K1—C16 | 91.7 (5) | C12—C13—H13A | 117 (2) |
O2—K1—C16 | 88.8 (3) | V1—C13—H13A | 127 (2) |
O1—K1—C16 | 85.50 (11) | K2ii—C13—H13A | 112 (2) |
C10—K1—C16 | 132.31 (10) | C13—C14—C20 | 122.6 (4) |
O2'—K1—C9 | 123.1 (5) | C13—C14—V1 | 68.8 (2) |
O2—K1—C9 | 130.4 (3) | C20—C14—V1 | 73.87 (19) |
O1—K1—C9 | 119.71 (8) | C13—C14—K2ii | 69.6 (2) |
C10—K1—C9 | 27.55 (8) | C20—C14—K2ii | 85.1 (2) |
C16—K1—C9 | 131.93 (9) | V1—C14—K2ii | 110.14 (15) |
O2'—K1—C17 | 84.4 (5) | C13—C14—H14A | 116 (2) |
O2—K1—C17 | 85.7 (3) | C20—C14—H14A | 121 (2) |
O1—K1—C17 | 111.34 (10) | V1—C14—H14A | 124 (2) |
C10—K1—C17 | 132.66 (9) | K2ii—C14—H14A | 124 (2) |
C16—K1—C17 | 26.49 (10) | C16—C15—C20 | 123.6 (4) |
C9—K1—C17 | 117.50 (9) | C16—C15—K1 | 69.00 (19) |
O2'—K1—C5 | 115.4 (5) | C20—C15—K1 | 93.28 (18) |
O2—K1—C5 | 115.0 (3) | C16—C15—H15A | 118.2 |
O1—K1—C5 | 76.15 (9) | C20—C15—H15A | 118.2 |
C10—K1—C5 | 26.57 (8) | K1—C15—H15A | 108.6 |
C16—K1—C5 | 147.84 (12) | C15—C16—C17 | 119.4 (3) |
C9—K1—C5 | 46.46 (9) | C15—C16—K1 | 85.6 (2) |
C17—K1—C5 | 158.92 (9) | C17—C16—K1 | 81.1 (2) |
O2'—K1—C15 | 116.2 (5) | C15—C16—H16A | 120.3 |
O2—K1—C15 | 112.0 (3) | C17—C16—H16A | 120.3 |
O1—K1—C15 | 78.16 (9) | K1—C16—H16A | 103.3 |
C10—K1—C15 | 107.76 (10) | C18—C17—C16 | 120.4 (4) |
C16—K1—C15 | 25.43 (10) | C18—C17—K1 | 90.6 (2) |
C9—K1—C15 | 114.84 (9) | C16—C17—K1 | 72.4 (2) |
C17—K1—C15 | 44.72 (11) | C18—C17—H17A | 119.8 |
C5—K1—C15 | 123.08 (11) | C16—C17—H17A | 119.8 |
O2'—K1—C6 | 92.0 (5) | K1—C17—H17A | 107.0 |
O2—K1—C6 | 93.5 (3) | C17—C18—C19 | 122.6 (3) |
O1—K1—C6 | 85.48 (9) | C17—C18—K1 | 65.33 (18) |
C10—K1—C6 | 45.15 (8) | C19—C18—K1 | 89.75 (18) |
C16—K1—C6 | 170.46 (12) | C17—C18—H18A | 118.7 |
C9—K1—C6 | 51.57 (8) | C19—C18—H18A | 118.7 |
C17—K1—C6 | 162.96 (11) | K1—C18—H18A | 116.0 |
C5—K1—C6 | 24.98 (8) | C18—C19—C11 | 124.4 (3) |
C15—K1—C6 | 147.94 (11) | C18—C19—C20 | 117.3 (3) |
O2'—K1—C8 | 98.6 (5) | C11—C19—C20 | 118.3 (3) |
O2—K1—C8 | 105.7 (3) | C18—C19—V1 | 129.9 (2) |
O1—K1—C8 | 125.63 (8) | C11—C19—V1 | 68.90 (18) |
C10—K1—C8 | 45.03 (8) | C20—C19—V1 | 71.80 (18) |
C16—K1—C8 | 146.00 (10) | C18—C19—K2ii | 124.93 (19) |
C9—K1—C8 | 24.67 (7) | C11—C19—K2ii | 67.39 (16) |
C17—K1—C8 | 122.40 (10) | C20—C19—K2ii | 79.65 (16) |
C5—K1—C8 | 50.73 (9) | V1—C19—K2ii | 105.06 (11) |
C15—K1—C8 | 137.22 (9) | C14—C20—C15 | 125.1 (3) |
C6—K1—C8 | 41.63 (9) | C14—C20—C19 | 118.3 (3) |
O2'—K1—C18 | 100.7 (5) | C15—C20—C19 | 116.6 (3) |
O2—K1—C18 | 104.6 (3) | C14—C20—V1 | 69.2 (2) |
O1—K1—C18 | 126.94 (9) | C15—C20—V1 | 131.8 (2) |
C10—K1—C18 | 109.74 (8) | C19—C20—V1 | 70.09 (16) |
C16—K1—C18 | 43.79 (10) | C14—C20—K2ii | 70.8 (2) |
C9—K1—C18 | 93.70 (8) | C15—C20—K2ii | 125.3 (2) |
C17—K1—C18 | 24.02 (8) | C19—C20—K2ii | 75.54 (16) |
C5—K1—C18 | 136.27 (9) | V1—C20—K2ii | 102.87 (11) |
C15—K1—C18 | 49.59 (10) | O1—C21—C22 | 106.4 (4) |
C6—K1—C18 | 143.52 (9) | O1—C21—H21A | 110.4 |
C8—K1—C18 | 102.28 (8) | C22—C21—H21A | 110.4 |
O2'—K1—C7 | 85.2 (5) | O1—C21—H21B | 110.4 |
O2—K1—C7 | 90.1 (3) | C22—C21—H21B | 110.4 |
O1—K1—C7 | 107.71 (9) | H21A—C21—H21B | 108.6 |
C10—K1—C7 | 51.44 (8) | C21—C22—C23 | 102.8 (4) |
C16—K1—C7 | 166.59 (12) | C21—C22—H22A | 111.2 |
C9—K1—C7 | 43.28 (7) | C23—C22—H22A | 111.2 |
C17—K1—C7 | 140.11 (10) | C21—C22—H22B | 111.2 |
C5—K1—C7 | 42.59 (9) | C23—C22—H22B | 111.2 |
C15—K1—C7 | 157.73 (10) | H22A—C22—H22B | 109.1 |
C6—K1—C7 | 22.88 (8) | C22—C23—C24 | 102.6 (4) |
C8—K1—C7 | 23.53 (7) | C22—C23—H23A | 111.3 |
C18—K1—C7 | 124.04 (9) | C24—C23—H23A | 111.3 |
O2'—K1—C4 | 160.1 (5) | C22—C23—H23B | 111.3 |
O2—K1—C4 | 159.8 (3) | C24—C23—H23B | 111.3 |
O1—K1—C4 | 85.68 (9) | H23A—C23—H23B | 109.2 |
C10—K1—C4 | 24.62 (8) | O1—C24—C23 | 106.5 (4) |
C16—K1—C4 | 108.10 (10) | O1—C24—H24A | 110.4 |
C9—K1—C4 | 43.36 (8) | C23—C24—H24A | 110.4 |
C17—K1—C4 | 114.35 (9) | O1—C24—H24B | 110.4 |
C5—K1—C4 | 45.18 (8) | C23—C24—H24B | 110.4 |
C15—K1—C4 | 83.21 (10) | H24A—C24—H24B | 108.6 |
C6—K1—C4 | 68.09 (8) | C28—O2—C25 | 109.2 (6) |
C8—K1—C4 | 66.29 (8) | C28—O2—K1 | 125.4 (8) |
C18—K1—C4 | 95.32 (8) | C25—O2—K1 | 125.1 (7) |
C7—K1—C4 | 75.99 (8) | O2—C25—C26 | 106.2 (7) |
O2'—K1—V1 | 155.4 (5) | O2—C25—H25A | 110.5 |
O2—K1—V1 | 161.7 (3) | C26—C25—H25A | 110.5 |
O1—K1—V1 | 108.14 (6) | O2—C25—H25B | 110.5 |
C10—K1—V1 | 55.90 (6) | C26—C25—H25B | 110.5 |
C16—K1—V1 | 79.55 (8) | H25A—C25—H25B | 108.7 |
C9—K1—V1 | 54.74 (5) | C27—C26—C25 | 102.7 (6) |
C17—K1—V1 | 77.55 (7) | C27—C26—H26A | 111.2 |
C5—K1—V1 | 81.39 (6) | C25—C26—H26A | 111.2 |
C15—K1—V1 | 60.13 (7) | C27—C26—H26B | 111.2 |
C6—K1—V1 | 100.37 (6) | C25—C26—H26B | 111.2 |
C8—K1—V1 | 77.76 (5) | H26A—C26—H26B | 109.1 |
C18—K1—V1 | 57.30 (6) | C26—C27—C28 | 104.1 (7) |
C7—K1—V1 | 97.96 (6) | C26—C27—H27A | 110.9 |
C4—K1—V1 | 38.03 (6) | C28—C27—H27A | 110.9 |
O3—K2—O4 | 90.1 (3) | C26—C27—H27B | 110.9 |
O4'—K2—O3' | 78.9 (4) | C28—C27—H27B | 110.9 |
O3—K2—C12i | 136.27 (12) | H27A—C27—H27B | 108.9 |
O4—K2—C12i | 91.1 (3) | O2—C28—C27 | 108.2 (7) |
O3—K2—C9 | 119.09 (13) | O2—C28—H28A | 110.1 |
O4—K2—C9 | 105.5 (3) | C27—C28—H28A | 110.1 |
O4'—K2—C9 | 98.7 (4) | O2—C28—H28B | 110.1 |
O3'—K2—C9 | 129.31 (17) | C27—C28—H28B | 110.1 |
C12i—K2—C9 | 102.60 (9) | H28A—C28—H28B | 108.4 |
O3—K2—C13i | 129.59 (12) | C28'—O2'—C25' | 108.1 (11) |
O4—K2—C13i | 118.1 (3) | C28'—O2'—K1 | 128.7 (13) |
C12i—K2—C13i | 27.01 (9) | C25'—O2'—K1 | 120.5 (13) |
C9—K2—C13i | 94.04 (10) | O2'—C25'—C26' | 103.3 (11) |
O3—K2—C2 | 73.28 (13) | O2'—C25'—H25C | 111.1 |
O4—K2—C2 | 120.2 (3) | C26'—C25'—H25C | 111.1 |
O4'—K2—C2 | 121.0 (5) | O2'—C25'—H25D | 111.1 |
O3'—K2—C2 | 89.90 (18) | C26'—C25'—H25D | 111.1 |
C12i—K2—C2 | 139.52 (10) | H25C—C25'—H25D | 109.1 |
C9—K2—C2 | 47.72 (8) | C27'—C26'—C25' | 103.1 (10) |
C13i—K2—C2 | 116.23 (11) | C27'—C26'—H26C | 111.1 |
O3—K2—C11i | 112.47 (13) | C25'—C26'—H26C | 111.1 |
O4—K2—C11i | 77.3 (3) | C27'—C26'—H26D | 111.1 |
C12i—K2—C11i | 26.88 (9) | C25'—C26'—H26D | 111.1 |
C9—K2—C11i | 128.29 (9) | H26C—C26'—H26D | 109.1 |
C13i—K2—C11i | 46.64 (10) | C26'—C27'—C28' | 106.6 (10) |
C2—K2—C11i | 162.15 (10) | C26'—C27'—H27C | 110.4 |
O3—K2—C1 | 99.13 (14) | C28'—C27'—H27C | 110.4 |
O4—K2—C1 | 126.5 (3) | C26'—C27'—H27D | 110.4 |
O4'—K2—C1 | 122.0 (4) | C28'—C27'—H27D | 110.4 |
O3'—K2—C1 | 116.25 (18) | H27C—C27'—H27D | 108.6 |
C12i—K2—C1 | 114.70 (10) | O2'—C28'—C27' | 104.7 (11) |
C9—K2—C1 | 26.87 (8) | O2'—C28'—H28C | 110.8 |
C13i—K2—C1 | 95.63 (10) | C27'—C28'—H28C | 110.8 |
C2—K2—C1 | 26.38 (8) | O2'—C28'—H28D | 110.8 |
C11i—K2—C1 | 141.02 (9) | C27'—C28'—H28D | 110.8 |
O3—K2—C14i | 104.23 (12) | H28C—C28'—H28D | 108.9 |
O4—K2—C14i | 129.4 (3) | C29—O3—C32 | 109.9 (5) |
C12i—K2—C14i | 45.82 (10) | C29—O3—K2 | 125.0 (3) |
C9—K2—C14i | 108.66 (10) | C32—O3—K2 | 118.8 (5) |
C13i—K2—C14i | 25.50 (10) | O3—C29—C30 | 107.3 (5) |
C2—K2—C14i | 110.39 (10) | O3—C29—H29A | 110.3 |
C11i—K2—C14i | 52.24 (9) | C30—C29—H29A | 110.3 |
C1—K2—C14i | 99.27 (10) | O3—C29—H29B | 110.3 |
O3—K2—C8 | 143.28 (13) | C30—C29—H29B | 110.3 |
O4—K2—C8 | 103.6 (2) | H29A—C29—H29B | 108.5 |
O4'—K2—C8 | 94.4 (3) | C29—C30—C31 | 104.4 (6) |
O3'—K2—C8 | 152.30 (18) | C29—C30—H30A | 110.9 |
C12i—K2—C8 | 78.20 (8) | C31—C30—H30A | 110.9 |
C9—K2—C8 | 24.52 (7) | C29—C30—H30B | 110.9 |
C13i—K2—C8 | 73.28 (9) | C31—C30—H30B | 110.9 |
C2—K2—C8 | 70.38 (8) | H30A—C30—H30B | 108.9 |
C11i—K2—C8 | 103.80 (8) | C32—C31—C30 | 103.4 (7) |
C1—K2—C8 | 45.53 (7) | C32—C31—H31A | 111.1 |
C14i—K2—C8 | 93.19 (9) | C30—C31—H31A | 111.1 |
O3—K2—C19i | 90.76 (11) | C32—C31—H31B | 111.1 |
O4—K2—C19i | 88.9 (3) | C30—C31—H31B | 111.1 |
C12i—K2—C19i | 45.57 (8) | H31A—C31—H31B | 109.0 |
C9—K2—C19i | 146.12 (8) | O3—C32—C31 | 104.5 (6) |
C13i—K2—C19i | 52.52 (9) | O3—C32—H32A | 110.8 |
C2—K2—C19i | 145.89 (9) | C31—C32—H32A | 110.8 |
C11i—K2—C19i | 24.97 (7) | O3—C32—H32B | 110.8 |
C1—K2—C19i | 142.85 (9) | C31—C32—H32B | 110.8 |
C14i—K2—C19i | 43.63 (8) | H32A—C32—H32B | 108.9 |
C8—K2—C19i | 122.89 (7) | C32'—O3'—C29' | 103.1 (8) |
O3—K2—C20i | 87.32 (11) | C32'—O3'—K2 | 123.2 (7) |
O4—K2—C20i | 113.5 (3) | C29'—O3'—K2 | 131.8 (8) |
O4'—K2—C20i | 115.7 (5) | C30'—C29'—O3' | 105.2 (9) |
O3'—K2—C20i | 90.2 (2) | C30'—C29'—H29C | 110.7 |
C12i—K2—C20i | 52.60 (8) | O3'—C29'—H29C | 110.7 |
C9—K2—C20i | 132.69 (9) | C30'—C29'—H29D | 110.7 |
C13i—K2—C20i | 44.26 (10) | O3'—C29'—H29D | 110.7 |
C2—K2—C20i | 122.18 (9) | H29C—C29'—H29D | 108.8 |
C11i—K2—C20i | 44.20 (8) | C29'—C30'—C31' | 105.4 (10) |
C1—K2—C20i | 119.51 (9) | C29'—C30'—H30C | 110.7 |
C14i—K2—C20i | 24.15 (9) | C31'—C30'—H30C | 110.7 |
C8—K2—C20i | 116.53 (9) | C29'—C30'—H30D | 110.7 |
C19i—K2—C20i | 24.81 (7) | C31'—C30'—H30D | 110.7 |
O3—K2—C10 | 108.17 (11) | H30C—C30'—H30D | 108.8 |
O4—K2—C10 | 84.5 (3) | C32'—C31'—C30' | 104.6 (9) |
O4'—K2—C10 | 79.6 (4) | C32'—C31'—H31C | 110.8 |
O3'—K2—C10 | 110.73 (18) | C30'—C31'—H31C | 110.8 |
C12i—K2—C10 | 115.46 (8) | C32'—C31'—H31D | 110.8 |
C9—K2—C10 | 24.11 (7) | C30'—C31'—H31D | 110.8 |
C13i—K2—C10 | 114.94 (9) | H31C—C31'—H31D | 108.9 |
C2—K2—C10 | 50.71 (8) | O3'—C32'—C31' | 107.2 (10) |
C11i—K2—C10 | 135.13 (8) | O3'—C32'—H32C | 110.3 |
C1—K2—C10 | 42.39 (8) | C31'—C32'—H32C | 110.3 |
C14i—K2—C10 | 132.53 (9) | O3'—C32'—H32D | 110.3 |
C8—K2—C10 | 41.67 (7) | C31'—C32'—H32D | 110.3 |
C19i—K2—C10 | 159.93 (7) | H32C—C32'—H32D | 108.5 |
C20i—K2—C10 | 156.67 (8) | C36—O4—C33 | 109.0 (7) |
C24—O1—C21 | 109.3 (3) | C36—O4—K2 | 116.9 (8) |
C24—O1—K1 | 126.2 (2) | C33—O4—K2 | 112.5 (7) |
C21—O1—K1 | 118.8 (2) | O4—C33—C34 | 106.6 (7) |
C2—C1—C9 | 117.5 (3) | O4—C33—H33A | 110.4 |
C2—C1—V1 | 66.43 (18) | C34—C33—H33A | 110.4 |
C9—C1—V1 | 108.8 (2) | O4—C33—H33B | 110.4 |
C2—C1—K2 | 73.54 (17) | C34—C33—H33B | 110.4 |
C9—C1—K2 | 69.04 (16) | H33A—C33—H33B | 108.6 |
V1—C1—K2 | 132.93 (14) | C33—C34—C35 | 103.2 (7) |
C2—C1—H1A | 121.0 (19) | C33—C34—H34A | 111.1 |
C9—C1—H1A | 113.2 (19) | C35—C34—H34A | 111.1 |
V1—C1—H1A | 121.6 (19) | C33—C34—H34B | 111.1 |
K2—C1—H1A | 99.6 (18) | C35—C34—H34B | 111.1 |
C3—C2—C1 | 116.2 (3) | H34A—C34—H34B | 109.1 |
C3—C2—V1 | 72.1 (2) | C36—C35—C34 | 102.2 (9) |
C1—C2—V1 | 75.48 (18) | C36—C35—H35A | 111.3 |
C3—C2—K2 | 97.4 (2) | C34—C35—H35A | 111.3 |
C1—C2—K2 | 80.08 (17) | C36—C35—H35B | 111.3 |
V1—C2—K2 | 144.95 (14) | C34—C35—H35B | 111.3 |
C3—C2—H2A | 120.5 (17) | H35A—C35—H35B | 109.2 |
C1—C2—H2A | 123.2 (17) | O4—C36—C35 | 105.3 (8) |
V1—C2—H2A | 120.7 (17) | O4—C36—H36A | 110.7 |
K2—C2—H2A | 93.7 (17) | C35—C36—H36A | 110.7 |
C2—C3—C4 | 116.3 (3) | O4—C36—H36B | 110.7 |
C2—C3—V1 | 70.8 (2) | C35—C36—H36B | 110.7 |
C4—C3—V1 | 75.7 (2) | H36A—C36—H36B | 108.8 |
C2—C3—H3A | 124.5 (18) | C36'—O4'—C33' | 105.5 (10) |
C4—C3—H3A | 119.2 (18) | C36'—O4'—K2 | 119.6 (12) |
V1—C3—H3A | 122.7 (18) | C33'—O4'—K2 | 125.8 (11) |
C3—C4—C10 | 115.9 (3) | O4'—C33'—C34' | 110.3 (10) |
C3—C4—V1 | 66.42 (19) | O4'—C33'—H33C | 109.6 |
C10—C4—V1 | 108.3 (2) | C34'—C33'—H33C | 109.6 |
C3—C4—K1 | 132.5 (2) | O4'—C33'—H33D | 109.6 |
C10—C4—K1 | 55.91 (16) | C34'—C33'—H33D | 109.6 |
V1—C4—K1 | 72.92 (9) | H33C—C33'—H33D | 108.1 |
C3—C4—H4A | 117 (2) | C33'—C34'—C35' | 102.5 (11) |
C10—C4—H4A | 117 (2) | C33'—C34'—H34C | 111.3 |
V1—C4—H4A | 123 (2) | C35'—C34'—H34C | 111.3 |
K1—C4—H4A | 105.4 (19) | C33'—C34'—H34D | 111.3 |
C10—C5—C6 | 120.4 (3) | C35'—C34'—H34D | 111.3 |
C10—C5—K1 | 69.41 (17) | H34C—C34'—H34D | 109.2 |
C6—C5—K1 | 87.4 (2) | C36'—C35'—C34' | 106.8 (11) |
C10—C5—H5A | 119.8 | C36'—C35'—H35C | 110.4 |
C6—C5—H5A | 119.8 | C34'—C35'—H35C | 110.4 |
K1—C5—H5A | 113.6 | C36'—C35'—H35D | 110.4 |
C7—C6—C5 | 120.5 (3) | C34'—C35'—H35D | 110.4 |
C7—C6—K1 | 83.0 (2) | H35C—C35'—H35D | 108.6 |
C5—C6—K1 | 67.62 (18) | O4'—C36'—C35' | 107.9 (11) |
C7—C6—H6A | 119.8 | O4'—C36'—H36C | 110.1 |
C5—C6—H6A | 119.8 | C35'—C36'—H36C | 110.1 |
K1—C6—H6A | 120.4 | O4'—C36'—H36D | 110.1 |
C6—C7—C8 | 120.2 (3) | C35'—C36'—H36D | 110.1 |
C6—C7—K1 | 74.1 (2) | H36C—C36'—H36D | 108.4 |
C8—C7—K1 | 73.92 (17) | | |
| | | |
C9—C1—C2—C3 | −38.5 (4) | C15—C16—C17—C18 | −0.3 (5) |
V1—C1—C2—C3 | 61.2 (3) | K1—C16—C17—C18 | −80.1 (3) |
K2—C1—C2—C3 | −93.4 (3) | C15—C16—C17—K1 | 79.8 (3) |
C9—C1—C2—V1 | −99.7 (3) | C16—C17—C18—C19 | −2.7 (5) |
K2—C1—C2—V1 | −154.66 (13) | K1—C17—C18—C19 | −72.6 (3) |
C9—C1—C2—K2 | 54.9 (2) | C16—C17—C18—K1 | 69.9 (3) |
V1—C1—C2—K2 | 154.66 (13) | C17—C18—C19—C11 | −177.8 (3) |
C1—C2—C3—C4 | −0.7 (4) | K1—C18—C19—C11 | 122.1 (3) |
V1—C2—C3—C4 | 62.4 (3) | C17—C18—C19—C20 | 3.6 (4) |
K2—C2—C3—C4 | −83.2 (3) | K1—C18—C19—C20 | −56.5 (2) |
C1—C2—C3—V1 | −63.1 (2) | C17—C18—C19—V1 | 92.1 (4) |
K2—C2—C3—V1 | −145.64 (12) | K1—C18—C19—V1 | 31.9 (3) |
C2—C3—C4—C10 | 40.1 (4) | C17—C18—C19—K2ii | −93.0 (3) |
V1—C3—C4—C10 | 99.8 (3) | K1—C18—C19—K2ii | −153.07 (16) |
C2—C3—C4—V1 | −59.7 (3) | C12—C11—C19—C18 | −175.9 (3) |
C2—C3—C4—K1 | −26.4 (5) | V1—C11—C19—C18 | −124.6 (3) |
V1—C3—C4—K1 | 33.3 (3) | K2ii—C11—C19—C18 | 117.8 (3) |
C10—C5—C6—C7 | 2.6 (5) | C12—C11—C19—C20 | 2.7 (4) |
K1—C5—C6—C7 | 66.8 (3) | V1—C11—C19—C20 | 54.0 (2) |
C10—C5—C6—K1 | −64.2 (3) | K2ii—C11—C19—C20 | −63.6 (2) |
C5—C6—C7—C8 | 1.1 (5) | C12—C11—C19—V1 | −51.3 (3) |
K1—C6—C7—C8 | 60.0 (3) | K2ii—C11—C19—V1 | −117.54 (11) |
C5—C6—C7—K1 | −58.9 (3) | C12—C11—C19—K2ii | 66.2 (3) |
C6—C7—C8—C9 | −4.7 (5) | V1—C11—C19—K2ii | 117.54 (11) |
K1—C7—C8—C9 | 55.4 (2) | C13—C14—C20—C15 | 178.0 (3) |
C6—C7—C8—K1 | −60.1 (3) | V1—C14—C20—C15 | 127.2 (3) |
C6—C7—C8—K2 | 67.4 (4) | K2ii—C14—C20—C15 | −120.2 (3) |
K1—C7—C8—K2 | 127.50 (15) | C13—C14—C20—C19 | −1.1 (5) |
C7—C8—C9—C10 | 4.5 (4) | V1—C14—C20—C19 | −51.8 (3) |
K1—C8—C9—C10 | 68.3 (2) | K2ii—C14—C20—C19 | 60.8 (3) |
K2—C8—C9—C10 | −98.2 (3) | C13—C14—C20—V1 | 50.7 (3) |
C7—C8—C9—C1 | −173.1 (3) | K2ii—C14—C20—V1 | 112.63 (11) |
K1—C8—C9—C1 | −109.3 (3) | C13—C14—C20—K2ii | −61.9 (3) |
K2—C8—C9—C1 | 84.2 (3) | V1—C14—C20—K2ii | −112.63 (11) |
C7—C8—C9—K2 | 102.7 (3) | C16—C15—C20—C14 | 179.6 (3) |
K1—C8—C9—K2 | 166.53 (12) | K1—C15—C20—C14 | −113.5 (3) |
C7—C8—C9—K1 | −63.8 (3) | C16—C15—C20—C19 | −1.3 (5) |
K2—C8—C9—K1 | −166.53 (12) | K1—C15—C20—C19 | 65.5 (3) |
C2—C1—C9—C8 | −145.4 (3) | C16—C15—C20—V1 | −87.7 (5) |
V1—C1—C9—C8 | 142.0 (2) | K1—C15—C20—V1 | −20.8 (4) |
K2—C1—C9—C8 | −88.2 (3) | C16—C15—C20—K2ii | 89.4 (4) |
C2—C1—C9—C10 | 36.9 (4) | K1—C15—C20—K2ii | 156.24 (17) |
V1—C1—C9—C10 | −35.7 (3) | C18—C19—C20—C14 | 177.5 (3) |
K2—C1—C9—C10 | 94.1 (2) | C11—C19—C20—C14 | −1.2 (4) |
C2—C1—C9—K2 | −57.2 (3) | V1—C19—C20—C14 | 51.4 (3) |
V1—C1—C9—K2 | −129.80 (15) | K2ii—C19—C20—C14 | −58.3 (3) |
C2—C1—C9—K1 | 113.0 (3) | C18—C19—C20—C15 | −1.6 (4) |
V1—C1—C9—K1 | 40.4 (2) | C11—C19—C20—C15 | 179.7 (3) |
K2—C1—C9—K1 | 170.17 (14) | V1—C19—C20—C15 | −127.7 (3) |
C6—C5—C10—C9 | −2.7 (5) | K2ii—C19—C20—C15 | 122.5 (3) |
K1—C5—C10—C9 | −76.6 (2) | C18—C19—C20—V1 | 126.1 (3) |
C6—C5—C10—C4 | 171.3 (3) | C11—C19—C20—V1 | −52.6 (2) |
K1—C5—C10—C4 | 97.4 (3) | K2ii—C19—C20—V1 | −109.76 (8) |
C6—C5—C10—K1 | 73.9 (3) | C18—C19—C20—K2ii | −124.1 (2) |
C6—C5—C10—K2 | −68.0 (3) | C11—C19—C20—K2ii | 57.2 (2) |
K1—C5—C10—K2 | −141.89 (15) | V1—C19—C20—K2ii | 109.76 (8) |
C8—C9—C10—C5 | −0.8 (4) | C24—O1—C21—C22 | −18.8 (5) |
C1—C9—C10—C5 | 177.1 (3) | K1—O1—C21—C22 | 136.5 (4) |
K2—C9—C10—C5 | −96.6 (3) | O1—C21—C22—C23 | 32.9 (6) |
K1—C9—C10—C5 | 78.2 (3) | C21—C22—C23—C24 | −33.9 (5) |
C8—C9—C10—C4 | −175.4 (3) | C21—O1—C24—C23 | −3.5 (5) |
C1—C9—C10—C4 | 2.5 (4) | K1—O1—C24—C23 | −156.5 (3) |
K2—C9—C10—C4 | 88.8 (3) | C22—C23—C24—O1 | 23.4 (5) |
K1—C9—C10—C4 | −96.4 (3) | C28—O2—C25—C26 | 15.8 (15) |
C8—C9—C10—K1 | −79.0 (2) | K1—O2—C25—C26 | −170.5 (9) |
C1—C9—C10—K1 | 98.9 (2) | O2—C25—C26—C27 | −28.6 (12) |
K2—C9—C10—K1 | −174.79 (9) | C25—C26—C27—C28 | 29.7 (11) |
C8—C9—C10—K2 | 95.8 (3) | C25—O2—C28—C27 | 3.4 (17) |
C1—C9—C10—K2 | −86.3 (2) | K1—O2—C28—C27 | −170.3 (10) |
K1—C9—C10—K2 | 174.79 (9) | C26—C27—C28—O2 | −21.6 (14) |
C3—C4—C10—C5 | 145.2 (3) | C28'—O2'—C25'—C26' | −39 (3) |
V1—C4—C10—C5 | −142.7 (3) | K1—O2'—C25'—C26' | 124.0 (15) |
K1—C4—C10—C5 | −89.5 (3) | O2'—C25'—C26'—C27' | 32 (2) |
C3—C4—C10—C9 | −40.6 (4) | C25'—C26'—C27'—C28' | −15 (2) |
V1—C4—C10—C9 | 31.5 (3) | C25'—O2'—C28'—C27' | 29 (3) |
K1—C4—C10—C9 | 84.7 (2) | K1—O2'—C28'—C27' | −132.0 (17) |
C3—C4—C10—K1 | −125.4 (3) | C26'—C27'—C28'—O2' | −7 (2) |
V1—C4—C10—K1 | −53.3 (2) | C32—O3—C29—C30 | 5.8 (11) |
C3—C4—C10—K2 | 21.1 (3) | K2—O3—C29—C30 | −145.9 (6) |
V1—C4—C10—K2 | 93.20 (17) | O3—C29—C30—C31 | 14.6 (10) |
K1—C4—C10—K2 | 146.45 (16) | C29—C30—C31—C32 | −28.7 (10) |
C19—C11—C12—C13 | −1.9 (4) | C29—O3—C32—C31 | −24.2 (11) |
V1—C11—C12—C13 | −55.1 (3) | K2—O3—C32—C31 | 129.4 (6) |
K2ii—C11—C12—C13 | 73.0 (3) | C30—C31—C32—O3 | 32.2 (11) |
C19—C11—C12—V1 | 53.2 (3) | C32'—O3'—C29'—C30' | 37.1 (19) |
K2ii—C11—C12—V1 | 128.12 (11) | K2—O3'—C29'—C30' | −127.2 (13) |
C19—C11—C12—K2ii | −74.9 (3) | O3'—C29'—C30'—C31' | −23 (2) |
V1—C11—C12—K2ii | −128.12 (11) | C29'—C30'—C31'—C32' | 1 (2) |
C11—C12—C13—C14 | −0.4 (5) | C29'—O3'—C32'—C31' | −37.1 (18) |
V1—C12—C13—C14 | −56.3 (3) | K2—O3'—C32'—C31' | 128.9 (11) |
K2ii—C12—C13—C14 | 74.0 (3) | C30'—C31'—C32'—O3' | 22 (2) |
C11—C12—C13—V1 | 55.9 (3) | C36—O4—C33—C34 | 2.7 (13) |
K2ii—C12—C13—V1 | 130.23 (12) | K2—O4—C33—C34 | −128.5 (6) |
C11—C12—C13—K2ii | −74.4 (3) | O4—C33—C34—C35 | −24.1 (10) |
V1—C12—C13—K2ii | −130.23 (12) | C33—C34—C35—C36 | 35.8 (12) |
C12—C13—C14—C20 | 1.9 (5) | C33—O4—C36—C35 | 20.5 (15) |
V1—C13—C14—C20 | −52.9 (3) | K2—O4—C36—C35 | 149.4 (10) |
K2ii—C13—C14—C20 | 69.7 (3) | C34—C35—C36—O4 | −34.7 (15) |
C12—C13—C14—V1 | 54.9 (3) | C36'—O4'—C33'—C34' | −8 (2) |
K2ii—C13—C14—V1 | 122.62 (13) | K2—O4'—C33'—C34' | −153.7 (14) |
C12—C13—C14—K2ii | −67.8 (3) | O4'—C33'—C34'—C35' | 21 (2) |
V1—C13—C14—K2ii | −122.62 (13) | C33'—C34'—C35'—C36' | −27 (3) |
C20—C15—C16—C17 | 2.3 (5) | C33'—O4'—C36'—C35' | −10 (3) |
K1—C15—C16—C17 | −77.2 (3) | K2—O4'—C36'—C35' | 139.0 (17) |
C20—C15—C16—K1 | 79.5 (3) | C34'—C35'—C36'—O4' | 23 (3) |
Symmetry codes: (i) −x+1, y+1/2, −z+1/2; (ii) −x+1, y−1/2, −z+1/2. |
(4,7,13,16,21,24-Hexaoxa-1,10-diazabicyclo[8.8.8]hexacosane)potassium
[1,2-bis(dimethylphosphanyl)ethane]bis(naphthalene)vanadium tetrahydrofuran (4b)
top
Crystal data top
[K(C18H36N2O6)][V(C10H8)2(C6H16P2)]·C4H8O | F(000) = 506 |
Mr = 945.08 | Dx = 1.278 Mg m−3 |
Monoclinic, P2 | Mo Kα radiation, λ = 0.71073 Å |
a = 10.3028 (11) Å | Cell parameters from 2618 reflections |
b = 8.6409 (9) Å | θ = 2.4–23.6° |
c = 14.5778 (15) Å | µ = 0.40 mm−1 |
β = 108.835 (2)° | T = 173 K |
V = 1228.3 (2) Å3 | Plate, red |
Z = 1 | 0.25 × 0.15 × 0.03 mm |
Data collection top
Siemens SMART CCD platform diffractometer | 3491 reflections with I > 2σ(I) |
Radiation source: normal-focus sealed tube | Rint = 0.048 |
ω scans | θmax = 25.1°, θmin = 1.5° |
Absorption correction: multi-scan (SADABS; Sheldrick, 1996) | h = −12→12 |
Tmin = 0.906, Tmax = 0.988 | k = −10→10 |
10165 measured reflections | l = −17→17 |
4352 independent reflections | |
Refinement top
Refinement on F2 | Secondary atom site location: difference Fourier map |
Least-squares matrix: full | Hydrogen site location: mixed |
R[F2 > 2σ(F2)] = 0.040 | H atoms treated by a mixture of independent and constrained refinement |
wR(F2) = 0.089 | w = 1/[σ2(Fo2) + (0.0359P)2 + 0.0452P] where P = (Fo2 + 2Fc2)/3 |
S = 1.04 | (Δ/σ)max < 0.001 |
4352 reflections | Δρmax = 0.34 e Å−3 |
295 parameters | Δρmin = −0.28 e Å−3 |
1 restraint | Absolute structure: Flack x determined using 1372 quotients [(I+)-(I-)]/[(I+)+(I-)]
(Parsons et al., 2013) |
Primary atom site location: structure-invariant direct methods | Absolute structure parameter: 0.05 (2) |
Special details top
Geometry. All esds (except the esd in the dihedral angle between two l.s. planes)
are estimated using the full covariance matrix. The cell esds are taken
into account individually in the estimation of esds in distances, angles
and torsion angles; correlations between esds in cell parameters are only
used when they are defined by crystal symmetry. An approximate (isotropic)
treatment of cell esds is used for estimating esds involving l.s. planes. |
Refinement. The hydrogen atoms on the metal-coordinating carbon atoms were
refined freely to confirm their nature and better describe their
true positions. |
Fractional atomic coordinates and isotropic or equivalent isotropic displacement parameters (Å2) top | x | y | z | Uiso*/Ueq | |
V1 | 0.500000 | 0.96419 (11) | 0.500000 | 0.0178 (3) | |
K1 | 1.000000 | 0.56885 (18) | 1.000000 | 0.0283 (4) | |
P1 | 0.37156 (13) | 0.75182 (14) | 0.53759 (9) | 0.0241 (3) | |
O1 | 1.0616 (4) | 0.8533 (5) | 0.9270 (3) | 0.0487 (10) | |
O2 | 0.8276 (4) | 0.4414 (5) | 0.8252 (2) | 0.0435 (10) | |
O3 | 0.7597 (3) | 0.4034 (5) | 0.9947 (2) | 0.0453 (11) | |
O4 | 0.000000 | 0.3999 (7) | 0.500000 | 0.070 (2) | |
N1 | 1.0928 (4) | 0.5669 (6) | 0.8261 (3) | 0.0382 (11) | |
C1 | 0.4668 (5) | 1.1215 (5) | 0.6203 (3) | 0.0227 (11) | |
H1 | 0.393 (4) | 1.197 (5) | 0.607 (3) | 0.015 (11)* | |
C2 | 0.5834 (5) | 1.1596 (6) | 0.5923 (3) | 0.0243 (11) | |
H2 | 0.595 (4) | 1.258 (6) | 0.570 (3) | 0.021 (12)* | |
C3 | 0.6851 (5) | 1.0471 (6) | 0.6072 (3) | 0.0249 (11) | |
H3 | 0.765 (4) | 1.063 (5) | 0.596 (3) | 0.014 (11)* | |
C4 | 0.6583 (5) | 0.9095 (6) | 0.6533 (3) | 0.0249 (11) | |
H4 | 0.718 (4) | 0.828 (5) | 0.661 (3) | 0.010 (11)* | |
C5 | 0.6383 (5) | 0.8515 (6) | 0.8195 (3) | 0.0303 (12) | |
H5 | 0.713578 | 0.781749 | 0.834836 | 0.036* | |
C6 | 0.5666 (6) | 0.8743 (7) | 0.8849 (3) | 0.0367 (13) | |
H6 | 0.592547 | 0.818106 | 0.944115 | 0.044* | |
C7 | 0.4596 (5) | 0.9764 (7) | 0.8650 (3) | 0.0368 (13) | |
H7 | 0.410300 | 0.989677 | 0.909429 | 0.044* | |
C8 | 0.4237 (5) | 1.0611 (6) | 0.7787 (3) | 0.0315 (12) | |
H8 | 0.350993 | 1.134168 | 0.765401 | 0.038* | |
C9 | 0.4924 (5) | 1.0400 (6) | 0.7124 (3) | 0.0244 (11) | |
C10 | 0.5995 (5) | 0.9307 (5) | 0.7320 (3) | 0.0228 (11) | |
C11 | 0.1832 (5) | 0.7433 (7) | 0.4893 (4) | 0.0347 (12) | |
H11A | 0.153444 | 0.634942 | 0.482504 | 0.052* | |
H11B | 0.151363 | 0.793915 | 0.425726 | 0.052* | |
H11C | 0.144318 | 0.796465 | 0.533786 | 0.052* | |
C12 | 0.3877 (6) | 0.6753 (6) | 0.6583 (4) | 0.0364 (14) | |
H12A | 0.327048 | 0.585791 | 0.651803 | 0.055* | |
H12B | 0.361953 | 0.755744 | 0.696618 | 0.055* | |
H12C | 0.482842 | 0.643698 | 0.691009 | 0.055* | |
C13 | 0.4222 (5) | 0.5742 (6) | 0.4885 (4) | 0.0321 (12) | |
H13A | 0.393811 | 0.482347 | 0.517844 | 0.039* | |
H13B | 0.376532 | 0.569827 | 0.417467 | 0.039* | |
C14 | 0.9994 (7) | 0.9838 (8) | 0.9504 (4) | 0.0615 (18) | |
H14A | 0.903322 | 0.989324 | 0.906807 | 0.074* | |
H14B | 1.047626 | 1.077370 | 0.939003 | 0.074* | |
C15 | 1.0702 (7) | 0.8538 (8) | 0.8334 (5) | 0.0620 (19) | |
H15A | 1.115669 | 0.950379 | 0.823547 | 0.074* | |
H15B | 0.976443 | 0.852846 | 0.785968 | 0.074* | |
C16 | 1.1469 (8) | 0.7205 (9) | 0.8150 (5) | 0.069 (2) | |
H16A | 1.150334 | 0.729183 | 0.748107 | 0.083* | |
H16B | 1.242324 | 0.727211 | 0.859588 | 0.083* | |
C17 | 0.9761 (6) | 0.5311 (8) | 0.7408 (4) | 0.0565 (19) | |
H17A | 1.011472 | 0.501107 | 0.687697 | 0.068* | |
H17B | 0.921511 | 0.626686 | 0.720217 | 0.068* | |
C18 | 0.8833 (6) | 0.4073 (7) | 0.7521 (4) | 0.0494 (17) | |
H18A | 0.808066 | 0.393309 | 0.690096 | 0.059* | |
H18B | 0.934761 | 0.308707 | 0.767639 | 0.059* | |
C19 | 0.7279 (6) | 0.3348 (8) | 0.8314 (4) | 0.0532 (18) | |
H19A | 0.771179 | 0.232021 | 0.848988 | 0.064* | |
H19B | 0.656620 | 0.325427 | 0.767057 | 0.064* | |
C20 | 0.6641 (6) | 0.3793 (9) | 0.9015 (4) | 0.063 (2) | |
H20A | 0.611306 | 0.475703 | 0.879642 | 0.075* | |
H20B | 0.598794 | 0.297535 | 0.905440 | 0.075* | |
C21 | 0.6992 (6) | 0.4365 (9) | 1.0649 (4) | 0.0561 (19) | |
H21A | 0.633461 | 0.353248 | 1.065485 | 0.067* | |
H21B | 0.647196 | 0.534507 | 1.047958 | 0.067* | |
C22 | 0.8015 (6) | 0.4508 (9) | 1.1629 (4) | 0.0589 (18) | |
H22A | 0.752165 | 0.474711 | 1.209304 | 0.071* | |
H22B | 0.846683 | 0.349160 | 1.181420 | 0.071* | |
C23 | 0.1144 (6) | 0.3055 (7) | 0.5429 (5) | 0.0598 (19) | |
H23A | 0.164708 | 0.342480 | 0.609088 | 0.072* | |
H23B | 0.177470 | 0.307670 | 0.504036 | 0.072* | |
C24 | 0.0626 (6) | 0.1451 (7) | 0.5465 (4) | 0.0555 (17) | |
H24A | 0.035608 | 0.128176 | 0.605008 | 0.067* | |
H24B | 0.130978 | 0.066211 | 0.543807 | 0.067* | |
Atomic displacement parameters (Å2) top | U11 | U22 | U33 | U12 | U13 | U23 |
V1 | 0.0211 (6) | 0.0172 (6) | 0.0136 (6) | 0.000 | 0.0038 (5) | 0.000 |
K1 | 0.0239 (8) | 0.0346 (9) | 0.0240 (8) | 0.000 | 0.0043 (7) | 0.000 |
P1 | 0.0295 (7) | 0.0217 (7) | 0.0230 (7) | −0.0057 (6) | 0.0111 (6) | −0.0041 (6) |
O1 | 0.053 (2) | 0.040 (2) | 0.050 (2) | 0.001 (2) | 0.013 (2) | 0.010 (2) |
O2 | 0.042 (2) | 0.058 (3) | 0.0311 (19) | −0.021 (2) | 0.0129 (17) | −0.0161 (19) |
O3 | 0.033 (2) | 0.072 (3) | 0.030 (2) | −0.0185 (19) | 0.0072 (17) | −0.0089 (18) |
O4 | 0.047 (4) | 0.036 (4) | 0.120 (6) | 0.000 | 0.019 (4) | 0.000 |
N1 | 0.027 (2) | 0.058 (3) | 0.030 (2) | 0.004 (2) | 0.0104 (19) | 0.008 (2) |
C1 | 0.029 (3) | 0.017 (3) | 0.021 (2) | 0.003 (2) | 0.006 (2) | −0.004 (2) |
C2 | 0.035 (3) | 0.020 (3) | 0.015 (2) | −0.007 (2) | 0.004 (2) | −0.002 (2) |
C3 | 0.023 (3) | 0.034 (3) | 0.017 (2) | −0.004 (2) | 0.005 (2) | 0.000 (2) |
C4 | 0.023 (3) | 0.027 (3) | 0.021 (3) | 0.003 (2) | 0.002 (2) | 0.003 (2) |
C5 | 0.031 (3) | 0.035 (3) | 0.020 (3) | 0.001 (3) | 0.001 (2) | 0.006 (2) |
C6 | 0.050 (3) | 0.045 (3) | 0.012 (2) | −0.011 (3) | 0.007 (2) | 0.003 (2) |
C7 | 0.046 (3) | 0.047 (3) | 0.021 (2) | −0.012 (3) | 0.016 (2) | −0.003 (3) |
C8 | 0.038 (3) | 0.034 (3) | 0.025 (3) | −0.004 (3) | 0.013 (2) | −0.008 (2) |
C9 | 0.027 (3) | 0.029 (3) | 0.014 (2) | −0.010 (2) | 0.003 (2) | −0.003 (2) |
C10 | 0.026 (3) | 0.023 (3) | 0.017 (2) | −0.006 (2) | 0.003 (2) | 0.000 (2) |
C11 | 0.032 (3) | 0.035 (3) | 0.040 (3) | −0.011 (3) | 0.015 (2) | −0.007 (3) |
C12 | 0.054 (4) | 0.030 (3) | 0.033 (3) | −0.021 (3) | 0.024 (3) | −0.002 (2) |
C13 | 0.046 (3) | 0.020 (3) | 0.035 (3) | −0.007 (3) | 0.020 (3) | −0.004 (2) |
C14 | 0.063 (4) | 0.040 (4) | 0.073 (4) | 0.000 (4) | 0.011 (4) | 0.006 (3) |
C15 | 0.064 (4) | 0.056 (4) | 0.069 (5) | −0.012 (4) | 0.027 (4) | 0.021 (4) |
C16 | 0.072 (5) | 0.085 (6) | 0.063 (5) | −0.011 (4) | 0.038 (4) | 0.020 (4) |
C17 | 0.051 (4) | 0.089 (5) | 0.025 (3) | −0.004 (4) | 0.007 (3) | 0.001 (3) |
C18 | 0.045 (3) | 0.069 (5) | 0.029 (3) | −0.004 (3) | 0.005 (3) | −0.010 (3) |
C19 | 0.053 (4) | 0.063 (4) | 0.037 (4) | −0.023 (4) | 0.005 (3) | −0.012 (3) |
C20 | 0.046 (4) | 0.096 (5) | 0.042 (4) | −0.035 (4) | 0.008 (3) | −0.015 (4) |
C21 | 0.039 (3) | 0.091 (6) | 0.040 (3) | −0.025 (4) | 0.015 (3) | −0.007 (3) |
C22 | 0.046 (3) | 0.096 (5) | 0.036 (3) | −0.029 (4) | 0.016 (3) | −0.003 (4) |
C23 | 0.047 (4) | 0.048 (4) | 0.078 (5) | 0.009 (3) | 0.012 (4) | −0.013 (3) |
C24 | 0.055 (4) | 0.050 (4) | 0.068 (4) | 0.011 (3) | 0.029 (3) | 0.014 (3) |
Geometric parameters (Å, º) top
V1—C2i | 2.157 (5) | C6—H6 | 0.9500 |
V1—C2 | 2.157 (5) | C7—C8 | 1.399 (7) |
V1—C3 | 2.161 (5) | C7—H7 | 0.9500 |
V1—C3i | 2.161 (5) | C8—C9 | 1.382 (6) |
V1—C1 | 2.329 (5) | C8—H8 | 0.9500 |
V1—C1i | 2.329 (5) | C9—C10 | 1.410 (6) |
V1—C4 | 2.350 (5) | C11—H11A | 0.9800 |
V1—C4i | 2.350 (5) | C11—H11B | 0.9800 |
V1—P1 | 2.4263 (14) | C11—H11C | 0.9800 |
V1—P1i | 2.4263 (14) | C12—H12A | 0.9800 |
K1—O2 | 2.818 (3) | C12—H12B | 0.9800 |
K1—O2ii | 2.818 (3) | C12—H12C | 0.9800 |
K1—O1 | 2.830 (4) | C13—C13i | 1.528 (9) |
K1—O1ii | 2.830 (4) | C13—H13A | 0.9900 |
K1—O3ii | 2.838 (3) | C13—H13B | 0.9900 |
K1—O3 | 2.838 (4) | C14—C14ii | 1.444 (12) |
K1—N1ii | 2.984 (4) | C14—H14A | 0.9900 |
K1—N1 | 2.984 (4) | C14—H14B | 0.9900 |
P1—C12 | 1.837 (5) | C15—C16 | 1.470 (10) |
P1—C13 | 1.839 (5) | C15—H15A | 0.9900 |
P1—C11 | 1.840 (5) | C15—H15B | 0.9900 |
O1—C14 | 1.393 (7) | C16—H16A | 0.9900 |
O1—C15 | 1.396 (7) | C16—H16B | 0.9900 |
O2—C18 | 1.395 (6) | C17—C18 | 1.480 (8) |
O2—C19 | 1.404 (7) | C17—H17A | 0.9900 |
O3—C21 | 1.389 (6) | C17—H17B | 0.9900 |
O3—C20 | 1.412 (6) | C18—H18A | 0.9900 |
O4—C23iii | 1.404 (6) | C18—H18B | 0.9900 |
O4—C23 | 1.404 (6) | C19—C20 | 1.435 (8) |
N1—C22ii | 1.451 (7) | C19—H19A | 0.9900 |
N1—C17 | 1.457 (7) | C19—H19B | 0.9900 |
N1—C16 | 1.468 (8) | C20—H20A | 0.9900 |
C1—C2 | 1.426 (7) | C20—H20B | 0.9900 |
C1—C9 | 1.463 (6) | C21—C22 | 1.482 (7) |
C1—H1 | 0.97 (4) | C21—H21A | 0.9900 |
C2—C3 | 1.395 (7) | C21—H21B | 0.9900 |
C2—H2 | 0.93 (5) | C22—H22A | 0.9900 |
C3—C4 | 1.436 (7) | C22—H22B | 0.9900 |
C3—H3 | 0.90 (4) | C23—C24 | 1.492 (9) |
C4—C10 | 1.472 (6) | C23—H23A | 0.9900 |
C4—H4 | 0.92 (4) | C23—H23B | 0.9900 |
C5—C10 | 1.387 (6) | C24—C24iii | 1.539 (12) |
C5—C6 | 1.396 (7) | C24—H24A | 0.9900 |
C5—H5 | 0.9500 | C24—H24B | 0.9900 |
C6—C7 | 1.368 (7) | | |
| | | |
C2i—V1—C2 | 77.0 (3) | C4—C3—H3 | 123 (3) |
C2i—V1—C3 | 105.8 (2) | V1—C3—H3 | 125 (3) |
C2—V1—C3 | 37.69 (18) | C3—C4—C10 | 116.9 (4) |
C2i—V1—C3i | 37.69 (18) | C3—C4—V1 | 64.4 (3) |
C2—V1—C3i | 105.8 (2) | C10—C4—V1 | 112.5 (3) |
C3—V1—C3i | 141.3 (3) | C3—C4—H4 | 118 (3) |
C2i—V1—C1 | 83.51 (17) | C10—C4—H4 | 115 (3) |
C2—V1—C1 | 36.80 (17) | V1—C4—H4 | 120 (2) |
C3—V1—C1 | 64.66 (18) | C10—C5—C6 | 120.0 (5) |
C3i—V1—C1 | 92.35 (17) | C10—C5—H5 | 120.0 |
C2i—V1—C1i | 36.81 (17) | C6—C5—H5 | 120.0 |
C2—V1—C1i | 83.51 (18) | C7—C6—C5 | 120.9 (5) |
C3—V1—C1i | 92.35 (18) | C7—C6—H6 | 119.5 |
C3i—V1—C1i | 64.66 (18) | C5—C6—H6 | 119.5 |
C1—V1—C1i | 108.6 (2) | C6—C7—C8 | 119.3 (5) |
C2i—V1—C4 | 139.89 (18) | C6—C7—H7 | 120.3 |
C2—V1—C4 | 63.27 (18) | C8—C7—H7 | 120.3 |
C3—V1—C4 | 36.83 (17) | C9—C8—C7 | 120.9 (5) |
C3i—V1—C4 | 159.04 (18) | C9—C8—H8 | 119.6 |
C1—V1—C4 | 68.11 (17) | C7—C8—H8 | 119.6 |
C1i—V1—C4 | 127.42 (17) | C8—C9—C10 | 119.4 (4) |
C2i—V1—C4i | 63.27 (18) | C8—C9—C1 | 126.7 (5) |
C2—V1—C4i | 139.89 (18) | C10—C9—C1 | 113.9 (4) |
C3—V1—C4i | 159.04 (18) | C5—C10—C9 | 119.4 (4) |
C3i—V1—C4i | 36.83 (17) | C5—C10—C4 | 125.9 (4) |
C1—V1—C4i | 127.42 (17) | C9—C10—C4 | 114.7 (4) |
C1i—V1—C4i | 68.11 (17) | P1—C11—H11A | 109.5 |
C4—V1—C4i | 156.8 (2) | P1—C11—H11B | 109.5 |
C2i—V1—P1 | 126.62 (14) | H11A—C11—H11B | 109.5 |
C2—V1—P1 | 125.99 (13) | P1—C11—H11C | 109.5 |
C3—V1—P1 | 120.41 (14) | H11A—C11—H11C | 109.5 |
C3i—V1—P1 | 89.74 (14) | H11B—C11—H11C | 109.5 |
C1—V1—P1 | 92.76 (12) | P1—C12—H12A | 109.5 |
C1i—V1—P1 | 146.57 (12) | P1—C12—H12B | 109.5 |
C4—V1—P1 | 83.96 (12) | H12A—C12—H12B | 109.5 |
C4i—V1—P1 | 78.51 (13) | P1—C12—H12C | 109.5 |
C2i—V1—P1i | 125.99 (13) | H12A—C12—H12C | 109.5 |
C2—V1—P1i | 126.62 (14) | H12B—C12—H12C | 109.5 |
C3—V1—P1i | 89.74 (14) | C13i—C13—P1 | 108.9 (2) |
C3i—V1—P1i | 120.41 (13) | C13i—C13—H13A | 109.9 |
C1—V1—P1i | 146.57 (12) | P1—C13—H13A | 109.9 |
C1i—V1—P1i | 92.76 (12) | C13i—C13—H13B | 109.9 |
C4—V1—P1i | 78.51 (13) | P1—C13—H13B | 109.9 |
C4i—V1—P1i | 83.96 (12) | H13A—C13—H13B | 108.3 |
P1—V1—P1i | 81.72 (7) | O1—C14—C14ii | 112.9 (4) |
O2—K1—O2ii | 133.98 (18) | O1—C14—H14A | 109.0 |
O2—K1—O1 | 98.73 (12) | C14ii—C14—H14A | 109.0 |
O2ii—K1—O1 | 121.80 (12) | O1—C14—H14B | 109.0 |
O2—K1—O1ii | 121.80 (11) | C14ii—C14—H14B | 109.0 |
O2ii—K1—O1ii | 98.73 (12) | H14A—C14—H14B | 107.8 |
O1—K1—O1ii | 59.48 (18) | O1—C15—C16 | 112.6 (5) |
O2—K1—O3ii | 96.74 (11) | O1—C15—H15A | 109.1 |
O2ii—K1—O3ii | 59.25 (10) | C16—C15—H15A | 109.1 |
O1—K1—O3ii | 98.52 (11) | O1—C15—H15B | 109.1 |
O1ii—K1—O3ii | 136.61 (12) | C16—C15—H15B | 109.1 |
O2—K1—O3 | 59.25 (10) | H15A—C15—H15B | 107.8 |
O2ii—K1—O3 | 96.74 (11) | N1—C16—C15 | 116.3 (5) |
O1—K1—O3 | 136.61 (12) | N1—C16—H16A | 108.2 |
O1ii—K1—O3 | 98.52 (11) | C15—C16—H16A | 108.2 |
O3ii—K1—O3 | 119.50 (17) | N1—C16—H16B | 108.2 |
O2—K1—N1ii | 118.99 (11) | C15—C16—H16B | 108.2 |
O2ii—K1—N1ii | 60.72 (11) | H16A—C16—H16B | 107.4 |
O1—K1—N1ii | 119.77 (14) | N1—C17—C18 | 116.3 (5) |
O1ii—K1—N1ii | 60.87 (13) | N1—C17—H17A | 108.2 |
O3ii—K1—N1ii | 119.33 (11) | C18—C17—H17A | 108.2 |
O3—K1—N1ii | 60.29 (11) | N1—C17—H17B | 108.2 |
O2—K1—N1 | 60.72 (11) | C18—C17—H17B | 108.2 |
O2ii—K1—N1 | 118.99 (11) | H17A—C17—H17B | 107.4 |
O1—K1—N1 | 60.88 (13) | O2—C18—C17 | 111.9 (5) |
O1ii—K1—N1 | 119.77 (14) | O2—C18—H18A | 109.2 |
O3ii—K1—N1 | 60.29 (11) | C17—C18—H18A | 109.2 |
O3—K1—N1 | 119.33 (11) | O2—C18—H18B | 109.2 |
N1ii—K1—N1 | 179.4 (2) | C17—C18—H18B | 109.2 |
C12—P1—C13 | 97.1 (2) | H18A—C18—H18B | 107.9 |
C12—P1—C11 | 96.4 (2) | O2—C19—C20 | 112.5 (5) |
C13—P1—C11 | 102.4 (2) | O2—C19—H19A | 109.1 |
C12—P1—V1 | 126.95 (18) | C20—C19—H19A | 109.1 |
C13—P1—V1 | 107.41 (16) | O2—C19—H19B | 109.1 |
C11—P1—V1 | 121.91 (19) | C20—C19—H19B | 109.1 |
C14—O1—C15 | 114.6 (5) | H19A—C19—H19B | 107.8 |
C14—O1—K1 | 115.8 (3) | O3—C20—C19 | 112.8 (5) |
C15—O1—K1 | 117.6 (4) | O3—C20—H20A | 109.0 |
C18—O2—C19 | 113.6 (4) | C19—C20—H20A | 109.0 |
C18—O2—K1 | 118.6 (3) | O3—C20—H20B | 109.0 |
C19—O2—K1 | 117.3 (3) | C19—C20—H20B | 109.0 |
C21—O3—C20 | 113.5 (4) | H20A—C20—H20B | 107.8 |
C21—O3—K1 | 118.1 (3) | O3—C21—C22 | 112.3 (5) |
C20—O3—K1 | 115.6 (3) | O3—C21—H21A | 109.2 |
C23iii—O4—C23 | 108.9 (6) | C22—C21—H21A | 109.2 |
C22ii—N1—C17 | 109.3 (5) | O3—C21—H21B | 109.2 |
C22ii—N1—C16 | 109.8 (5) | C22—C21—H21B | 109.2 |
C17—N1—C16 | 109.6 (5) | H21A—C21—H21B | 107.9 |
C22ii—N1—K1 | 110.2 (3) | N1ii—C22—C21 | 116.0 (5) |
C17—N1—K1 | 108.9 (3) | N1ii—C22—H22A | 108.3 |
C16—N1—K1 | 109.0 (4) | C21—C22—H22A | 108.3 |
C2—C1—C9 | 117.1 (4) | N1ii—C22—H22B | 108.3 |
C2—C1—V1 | 65.0 (3) | C21—C22—H22B | 108.3 |
C9—C1—V1 | 112.6 (3) | H22A—C22—H22B | 107.4 |
C2—C1—H1 | 118 (2) | O4—C23—C24 | 107.3 (5) |
C9—C1—H1 | 114 (2) | O4—C23—H23A | 110.3 |
V1—C1—H1 | 122 (2) | C24—C23—H23A | 110.3 |
C3—C2—C1 | 117.1 (4) | O4—C23—H23B | 110.3 |
C3—C2—V1 | 71.3 (3) | C24—C23—H23B | 110.3 |
C1—C2—V1 | 78.2 (3) | H23A—C23—H23B | 108.5 |
C3—C2—H2 | 121 (3) | C23—C24—C24iii | 100.2 (4) |
C1—C2—H2 | 122 (3) | C23—C24—H24A | 111.7 |
V1—C2—H2 | 124 (3) | C24iii—C24—H24A | 111.7 |
C2—C3—C4 | 113.7 (4) | C23—C24—H24B | 111.7 |
C2—C3—V1 | 71.0 (3) | C24iii—C24—H24B | 111.7 |
C4—C3—V1 | 78.8 (3) | H24A—C24—H24B | 109.5 |
C2—C3—H3 | 123 (3) | | |
| | | |
C9—C1—C2—C3 | 42.0 (6) | C12—P1—C13—C13i | −89.1 (4) |
V1—C1—C2—C3 | −61.7 (4) | C11—P1—C13—C13i | 172.8 (4) |
C9—C1—C2—V1 | 103.7 (4) | V1—P1—C13—C13i | 43.3 (4) |
C1—C2—C3—C4 | −2.5 (6) | C15—O1—C14—C14ii | −176.1 (6) |
V1—C2—C3—C4 | −68.0 (4) | K1—O1—C14—C14ii | 42.0 (8) |
C1—C2—C3—V1 | 65.4 (4) | C14—O1—C15—C16 | 175.1 (5) |
C2—C3—C4—C10 | −40.1 (6) | K1—O1—C15—C16 | −43.8 (6) |
V1—C3—C4—C10 | −103.4 (4) | C22ii—N1—C16—C15 | −161.6 (6) |
C2—C3—C4—V1 | 63.3 (3) | C17—N1—C16—C15 | 78.4 (7) |
C10—C5—C6—C7 | −1.3 (8) | K1—N1—C16—C15 | −40.8 (7) |
C5—C6—C7—C8 | −1.3 (8) | O1—C15—C16—N1 | 59.0 (8) |
C6—C7—C8—C9 | 1.7 (8) | C22ii—N1—C17—C18 | 78.5 (6) |
C7—C8—C9—C10 | 0.5 (7) | C16—N1—C17—C18 | −161.1 (5) |
C7—C8—C9—C1 | −179.2 (5) | K1—N1—C17—C18 | −42.0 (6) |
C2—C1—C9—C8 | 142.5 (5) | C19—O2—C18—C17 | 173.6 (5) |
V1—C1—C9—C8 | −145.0 (4) | K1—O2—C18—C17 | −42.4 (6) |
C2—C1—C9—C10 | −37.2 (6) | N1—C17—C18—O2 | 58.7 (7) |
V1—C1—C9—C10 | 35.3 (5) | C18—O2—C19—C20 | −175.2 (5) |
C6—C5—C10—C9 | 3.4 (7) | K1—O2—C19—C20 | 40.4 (6) |
C6—C5—C10—C4 | −175.0 (4) | C21—O3—C20—C19 | −176.0 (6) |
C8—C9—C10—C5 | −3.0 (7) | K1—O3—C20—C19 | 42.9 (7) |
C1—C9—C10—C5 | 176.7 (4) | O2—C19—C20—O3 | −55.6 (8) |
C8—C9—C10—C4 | 175.6 (4) | C20—O3—C21—C22 | 176.2 (6) |
C1—C9—C10—C4 | −4.7 (6) | K1—O3—C21—C22 | −43.8 (7) |
C3—C4—C10—C5 | −137.4 (5) | O3—C21—C22—N1ii | 57.9 (8) |
V1—C4—C10—C5 | 151.0 (4) | C23iii—O4—C23—C24 | −13.3 (3) |
C3—C4—C10—C9 | 44.1 (6) | O4—C23—C24—C24iii | 33.0 (7) |
V1—C4—C10—C9 | −27.5 (5) | | |
Symmetry codes: (i) −x+1, y, −z+1; (ii) −x+2, y, −z+2; (iii) −x, y, −z+1. |
(1,4,7,10,13,16-Hexaoxacyclooctadecane)bis(tetrahydrofuran)potassium
[(
η4-anthracene)(tetrahydrofuran)vanadium]-µ-
η4:
η2-anthracene-[(1,4,7,10,13,16-Hexaoxacyclooctadecane)potassium]-µ-
η2:
η4-anthracene-[(
η4-anthracene)(tetrahydrofuran)vanadium] tetrahydrofuran disolvate (5)
top
Crystal data top
[K(C12H24O6)(C4H8O)2][KV2(C12H24O6)(C4H8O)2(C14H10)4]·2C4H8O | Z = 1 |
Mr = 1854.20 | F(000) = 988 |
Triclinic, P1 | Dx = 1.293 Mg m−3 |
a = 9.1729 (16) Å | Mo Kα radiation, λ = 0.71073 Å |
b = 9.3501 (16) Å | Cell parameters from 2579 reflections |
c = 27.928 (5) Å | θ = 1.5–25.1° |
α = 89.695 (3)° | µ = 0.35 mm−1 |
β = 88.670 (3)° | T = 173 K |
γ = 83.918 (4)° | Plate, brown |
V = 2381.2 (7) Å3 | 0.30 × 0.10 × 0.05 mm |
Data collection top
Siemens SMART CCD platform diffractometer | 4713 reflections with I > 2σ(I) |
Radiation source: normal-focus sealed tube | Rint = 0.065 |
ω scans | θmax = 25.1°, θmin = 1.5° |
Absorption correction: multi-scan (SADABS; Sheldrick, 1996) | h = −10→10 |
Tmin = 0.902, Tmax = 0.983 | k = −11→11 |
21602 measured reflections | l = −33→33 |
8389 independent reflections | |
Refinement top
Refinement on F2 | Primary atom site location: structure-invariant direct methods |
Least-squares matrix: full | Secondary atom site location: difference Fourier map |
R[F2 > 2σ(F2)] = 0.053 | Hydrogen site location: mixed |
wR(F2) = 0.122 | H atoms treated by a mixture of independent and constrained refinement |
S = 1.04 | w = 1/[σ2(Fo2) + (0.0338P)2 + 1.6334P] where P = (Fo2 + 2Fc2)/3 |
8389 reflections | (Δ/σ)max = 0.001 |
647 parameters | Δρmax = 0.43 e Å−3 |
124 restraints | Δρmin = −0.36 e Å−3 |
Special details top
Geometry. All esds (except the esd in the dihedral angle between two l.s. planes)
are estimated using the full covariance matrix. The cell esds are taken
into account individually in the estimation of esds in distances, angles
and torsion angles; correlations between esds in cell parameters are only
used when they are defined by crystal symmetry. An approximate (isotropic)
treatment of cell esds is used for estimating esds involving l.s. planes. |
Refinement. THF ligand O8/C45-C48 is modeled as disordered over two
positions (0.58 (1):0.42 (1)). Analogous bond lengths and
angles were restrained to be similar. Anisotropic displacement
parameters for proximal atoms were restrained to be similar
and restrained toward the expected motion relative to bond
direction. |
Fractional atomic coordinates and isotropic or equivalent isotropic displacement parameters (Å2) top | x | y | z | Uiso*/Ueq | Occ. (<1) |
V1 | 0.61559 (7) | 0.68854 (7) | 0.22063 (2) | 0.03069 (18) | |
K1 | 1.000000 | 0.000000 | 0.000000 | 0.0397 (3) | |
O1 | 0.4874 (3) | 0.5133 (3) | 0.21158 (8) | 0.0335 (6) | |
O2 | 1.1953 (3) | 0.1333 (3) | 0.05585 (10) | 0.0483 (8) | |
O3 | 1.1105 (3) | −0.1326 (3) | 0.08378 (10) | 0.0496 (8) | |
O4 | 0.9680 (3) | −0.2902 (3) | 0.01570 (10) | 0.0471 (7) | |
O5 | 0.2992 (3) | 0.7921 (3) | 0.49853 (8) | 0.0336 (6) | |
O6 | 0.4001 (3) | 0.9214 (3) | 0.41287 (8) | 0.0332 (6) | |
O7 | 0.5460 (3) | 1.1676 (3) | 0.41741 (8) | 0.0348 (6) | |
C1 | 0.4097 (4) | 0.8286 (4) | 0.24723 (14) | 0.0346 (10) | |
H1 | 0.338 (4) | 0.876 (4) | 0.2245 (12) | 0.042* | |
C2 | 0.5414 (5) | 0.8914 (5) | 0.25687 (16) | 0.0415 (11) | |
H2 | 0.560 (4) | 0.973 (4) | 0.2418 (14) | 0.050* | |
C3 | 0.6426 (5) | 0.8161 (5) | 0.28532 (15) | 0.0394 (11) | |
H3 | 0.732 (4) | 0.846 (4) | 0.2928 (13) | 0.047* | |
C4 | 0.6111 (4) | 0.6813 (5) | 0.30323 (14) | 0.0376 (11) | |
H4 | 0.681 (4) | 0.624 (4) | 0.3194 (13) | 0.045* | |
C5 | 0.2218 (5) | 0.4175 (4) | 0.38004 (14) | 0.0410 (10) | |
H5 | 0.290580 | 0.368303 | 0.400933 | 0.049* | |
C6 | 0.0771 (5) | 0.3876 (4) | 0.38201 (15) | 0.0466 (12) | |
H6 | 0.046816 | 0.319470 | 0.404494 | 0.056* | |
C7 | −0.0239 (5) | 0.4575 (5) | 0.35104 (16) | 0.0455 (11) | |
H7 | −0.122496 | 0.434920 | 0.351967 | 0.055* | |
C8 | 0.0174 (4) | 0.5582 (4) | 0.31927 (14) | 0.0394 (10) | |
H8 | −0.053122 | 0.605014 | 0.298461 | 0.047* | |
C9 | 0.2097 (4) | 0.7005 (4) | 0.28560 (13) | 0.0318 (9) | |
H9 | 0.138953 | 0.753303 | 0.266231 | 0.038* | |
C10 | 0.4157 (4) | 0.5524 (4) | 0.34380 (13) | 0.0338 (9) | |
H10 | 0.486226 | 0.503866 | 0.364225 | 0.041* | |
C11 | 0.3529 (4) | 0.7311 (4) | 0.28201 (12) | 0.0277 (9) | |
C12 | 0.4602 (4) | 0.6517 (4) | 0.31178 (12) | 0.0298 (9) | |
C13 | 0.2684 (4) | 0.5195 (4) | 0.34759 (13) | 0.0320 (9) | |
C14 | 0.1629 (4) | 0.5939 (4) | 0.31687 (13) | 0.0295 (9) | |
C15 | 0.6353 (4) | 0.7286 (4) | 0.13986 (14) | 0.0359 (10) | |
H15 | 0.561 (4) | 0.789 (4) | 0.1214 (13) | 0.043* | |
C16 | 0.7422 (5) | 0.7957 (5) | 0.16582 (15) | 0.0425 (11) | |
H16 | 0.735 (4) | 0.894 (4) | 0.1659 (14) | 0.051* | |
C17 | 0.8398 (5) | 0.7093 (5) | 0.19297 (15) | 0.0429 (11) | |
H17 | 0.906 (4) | 0.748 (4) | 0.2127 (14) | 0.051* | |
C18 | 0.8289 (4) | 0.5595 (5) | 0.19324 (14) | 0.0392 (11) | |
H18 | 0.885 (4) | 0.498 (4) | 0.2136 (13) | 0.047* | |
C19 | 0.7584 (5) | 0.1364 (5) | 0.09092 (17) | 0.0505 (12) | |
H19 | 0.823 (5) | 0.075 (5) | 0.1083 (15) | 0.061* | |
C20 | 0.6838 (6) | 0.0774 (6) | 0.0550 (2) | 0.0596 (14) | |
H20 | 0.712 (5) | −0.024 (5) | 0.0484 (15) | 0.072* | |
C21 | 0.5852 (6) | 0.1638 (6) | 0.02846 (18) | 0.0611 (14) | |
H21 | 0.534694 | 0.122988 | 0.003484 | 0.073* | |
C22 | 0.5587 (5) | 0.3091 (5) | 0.03767 (14) | 0.0499 (12) | |
H22 | 0.490715 | 0.367337 | 0.018845 | 0.060* | |
C23 | 0.6036 (4) | 0.5202 (4) | 0.08601 (12) | 0.0337 (9) | |
H23 | 0.536824 | 0.579411 | 0.067034 | 0.040* | |
C24 | 0.8062 (4) | 0.3496 (4) | 0.13952 (13) | 0.0378 (10) | |
H24 | 0.878349 | 0.292579 | 0.157145 | 0.045* | |
C25 | 0.6702 (4) | 0.5817 (4) | 0.12369 (12) | 0.0307 (9) | |
C26 | 0.7738 (4) | 0.4926 (4) | 0.15130 (13) | 0.0320 (9) | |
C27 | 0.7348 (4) | 0.2844 (4) | 0.10164 (13) | 0.0369 (10) | |
C28 | 0.6317 (4) | 0.3720 (4) | 0.07482 (13) | 0.0338 (9) | |
C29 | 0.3529 (4) | 0.5242 (4) | 0.18441 (13) | 0.0375 (10) | |
H29A | 0.375004 | 0.529100 | 0.149609 | 0.045* | |
H29B | 0.287385 | 0.610966 | 0.193859 | 0.045* | |
C30 | 0.2833 (5) | 0.3905 (5) | 0.19658 (19) | 0.0670 (15) | |
H30A | 0.213404 | 0.407386 | 0.224034 | 0.080* | |
H30B | 0.230294 | 0.357865 | 0.168864 | 0.080* | |
C31 | 0.4053 (6) | 0.2846 (6) | 0.2089 (2) | 0.0879 (19) | |
H31A | 0.445826 | 0.232370 | 0.179981 | 0.105* | |
H31B | 0.373157 | 0.214096 | 0.232385 | 0.105* | |
C32 | 0.5178 (5) | 0.3699 (4) | 0.23011 (14) | 0.0424 (11) | |
H32A | 0.509185 | 0.369782 | 0.265508 | 0.051* | |
H32B | 0.618084 | 0.328817 | 0.220506 | 0.051* | |
C33 | 1.1696 (5) | 0.2837 (5) | 0.05542 (16) | 0.0584 (13) | |
H33A | 1.250326 | 0.325378 | 0.071513 | 0.070* | |
H33B | 1.076857 | 0.314745 | 0.073018 | 0.070* | |
C34 | 1.2226 (5) | 0.0760 (6) | 0.10221 (16) | 0.0657 (15) | |
H34A | 1.139170 | 0.107652 | 0.124148 | 0.079* | |
H34B | 1.312007 | 0.111491 | 0.114869 | 0.079* | |
C35 | 1.2424 (5) | −0.0846 (6) | 0.09950 (16) | 0.0629 (14) | |
H35A | 1.323814 | −0.116374 | 0.076834 | 0.075* | |
H35B | 1.266677 | −0.125894 | 0.131411 | 0.075* | |
C36 | 1.1160 (5) | −0.2857 (5) | 0.08353 (16) | 0.0589 (13) | |
H36A | 1.130117 | −0.323672 | 0.116451 | 0.071* | |
H36B | 1.199468 | −0.327037 | 0.063128 | 0.071* | |
C37 | 0.9766 (5) | −0.3271 (5) | 0.06470 (16) | 0.0547 (13) | |
H37A | 0.972737 | −0.431919 | 0.068720 | 0.066* | |
H37B | 0.892417 | −0.276411 | 0.082694 | 0.066* | |
C38 | 0.8396 (5) | −0.3356 (5) | −0.00504 (16) | 0.0530 (13) | |
H38A | 0.751355 | −0.295916 | 0.013493 | 0.064* | |
H38B | 0.844407 | −0.441822 | −0.004223 | 0.064* | |
K2 | 0.500000 | 1.000000 | 0.500000 | 0.0328 (3) | |
C39 | 0.3167 (5) | 0.6885 (4) | 0.53558 (14) | 0.0434 (11) | |
H39A | 0.407940 | 0.623802 | 0.529791 | 0.052* | |
H39B | 0.233135 | 0.629623 | 0.536114 | 0.052* | |
C40 | 0.2961 (4) | 0.7294 (4) | 0.45206 (13) | 0.0375 (10) | |
H40A | 0.215754 | 0.666741 | 0.450940 | 0.045* | |
H40B | 0.389837 | 0.669636 | 0.445180 | 0.045* | |
C41 | 0.2730 (4) | 0.8453 (4) | 0.41557 (13) | 0.0361 (10) | |
H41A | 0.256139 | 0.803108 | 0.383994 | 0.043* | |
H41B | 0.185777 | 0.912067 | 0.424545 | 0.043* | |
C42 | 0.3904 (4) | 1.0254 (4) | 0.37573 (13) | 0.0374 (10) | |
H42A | 0.306428 | 1.098767 | 0.382241 | 0.045* | |
H42B | 0.374573 | 0.978782 | 0.344817 | 0.045* | |
C43 | 0.5296 (4) | 1.0953 (4) | 0.37304 (13) | 0.0398 (10) | |
H43A | 0.613988 | 1.021760 | 0.367330 | 0.048* | |
H43B | 0.526260 | 1.165139 | 0.346219 | 0.048* | |
C44 | 0.6762 (4) | 1.2374 (4) | 0.41767 (13) | 0.0411 (10) | |
H44A | 0.675653 | 1.308257 | 0.391180 | 0.049* | |
H44B | 0.763055 | 1.165964 | 0.413154 | 0.049* | |
O8 | 0.6704 (6) | 0.7450 (7) | 0.4742 (2) | 0.044 (2) | 0.582 (11) |
C45 | 0.7922 (10) | 0.7415 (15) | 0.5047 (4) | 0.052 (3) | 0.582 (11) |
H45A | 0.833063 | 0.641126 | 0.511179 | 0.062* | 0.582 (11) |
H45B | 0.763610 | 0.789371 | 0.535568 | 0.062* | 0.582 (11) |
C46 | 0.8998 (18) | 0.820 (2) | 0.4782 (6) | 0.093 (5) | 0.582 (11) |
H46A | 1.000896 | 0.787380 | 0.488093 | 0.112* | 0.582 (11) |
H46B | 0.880055 | 0.924682 | 0.483497 | 0.112* | 0.582 (11) |
C47 | 0.878 (2) | 0.782 (3) | 0.4257 (6) | 0.056 (4) | 0.582 (11) |
H47A | 0.878604 | 0.868755 | 0.405060 | 0.067* | 0.582 (11) |
H47B | 0.956232 | 0.708331 | 0.414213 | 0.067* | 0.582 (11) |
C48 | 0.7312 (17) | 0.7261 (17) | 0.4265 (4) | 0.038 (3) | 0.582 (11) |
H48A | 0.666102 | 0.779641 | 0.403251 | 0.045* | 0.582 (11) |
H48B | 0.741736 | 0.623016 | 0.417776 | 0.045* | 0.582 (11) |
O8' | 0.7675 (10) | 0.8254 (10) | 0.5026 (3) | 0.052 (3) | 0.418 (11) |
C45' | 0.885 (2) | 0.8626 (18) | 0.4715 (7) | 0.042 (3) | 0.418 (11) |
H45C | 0.981176 | 0.819005 | 0.483194 | 0.051* | 0.418 (11) |
H45D | 0.886734 | 0.968305 | 0.469872 | 0.051* | 0.418 (11) |
C46' | 0.856 (3) | 0.804 (3) | 0.4238 (7) | 0.047 (5) | 0.418 (11) |
H46C | 0.947876 | 0.762332 | 0.407887 | 0.056* | 0.418 (11) |
H46D | 0.808112 | 0.880759 | 0.403052 | 0.056* | 0.418 (11) |
C47' | 0.752 (3) | 0.687 (2) | 0.4343 (6) | 0.048 (5) | 0.418 (11) |
H47C | 0.656911 | 0.709671 | 0.418359 | 0.058* | 0.418 (11) |
H47D | 0.796775 | 0.591257 | 0.423345 | 0.058* | 0.418 (11) |
C48' | 0.731 (2) | 0.6893 (14) | 0.4875 (5) | 0.047 (3) | 0.418 (11) |
H48C | 0.628538 | 0.676739 | 0.496637 | 0.056* | 0.418 (11) |
H48D | 0.796568 | 0.611158 | 0.502416 | 0.056* | 0.418 (11) |
O9 | −0.1375 (4) | 0.0950 (4) | 0.31276 (15) | 0.0904 (12) | |
C49 | −0.1379 (6) | 0.1502 (7) | 0.2653 (2) | 0.094 (2) | |
H49A | −0.164189 | 0.255662 | 0.265583 | 0.113* | |
H49B | −0.210531 | 0.105947 | 0.246074 | 0.113* | |
C50 | 0.0130 (6) | 0.1147 (6) | 0.24421 (18) | 0.0719 (15) | |
H50A | 0.039998 | 0.191474 | 0.222199 | 0.086* | |
H50B | 0.021534 | 0.022146 | 0.226801 | 0.086* | |
C51 | 0.1059 (4) | 0.1052 (5) | 0.28796 (14) | 0.0472 (11) | |
H51A | 0.196146 | 0.038466 | 0.282909 | 0.057* | |
H51B | 0.133164 | 0.200823 | 0.297100 | 0.057* | |
C52 | 0.0057 (5) | 0.0481 (5) | 0.32491 (16) | 0.0545 (12) | |
H52A | 0.020373 | −0.058302 | 0.325535 | 0.065* | |
H52B | 0.026564 | 0.084091 | 0.357044 | 0.065* | |
Atomic displacement parameters (Å2) top | U11 | U22 | U33 | U12 | U13 | U23 |
V1 | 0.0293 (4) | 0.0358 (4) | 0.0277 (4) | −0.0075 (3) | 0.0025 (3) | −0.0055 (3) |
K1 | 0.0465 (8) | 0.0397 (8) | 0.0353 (7) | −0.0142 (6) | −0.0074 (6) | 0.0030 (6) |
O1 | 0.0331 (15) | 0.0355 (16) | 0.0326 (15) | −0.0064 (12) | −0.0037 (12) | 0.0005 (12) |
O2 | 0.0490 (19) | 0.053 (2) | 0.0447 (19) | −0.0133 (15) | 0.0004 (14) | −0.0171 (16) |
O3 | 0.051 (2) | 0.053 (2) | 0.0438 (18) | 0.0020 (16) | −0.0050 (15) | 0.0040 (15) |
O4 | 0.0533 (19) | 0.0436 (18) | 0.0448 (18) | −0.0109 (15) | 0.0158 (15) | −0.0023 (14) |
O5 | 0.0396 (16) | 0.0319 (15) | 0.0306 (15) | −0.0099 (12) | −0.0018 (12) | −0.0018 (13) |
O6 | 0.0317 (15) | 0.0392 (16) | 0.0302 (15) | −0.0088 (12) | −0.0077 (12) | 0.0004 (13) |
O7 | 0.0351 (16) | 0.0416 (16) | 0.0297 (15) | −0.0139 (13) | −0.0002 (12) | −0.0029 (13) |
C1 | 0.032 (2) | 0.038 (2) | 0.033 (2) | −0.0006 (19) | 0.0017 (18) | −0.001 (2) |
C2 | 0.044 (3) | 0.036 (3) | 0.045 (3) | −0.009 (2) | 0.014 (2) | −0.009 (2) |
C3 | 0.033 (2) | 0.053 (3) | 0.035 (2) | −0.015 (2) | 0.007 (2) | −0.017 (2) |
C4 | 0.027 (2) | 0.057 (3) | 0.028 (2) | −0.003 (2) | −0.0008 (18) | −0.007 (2) |
C5 | 0.050 (3) | 0.030 (2) | 0.042 (3) | −0.002 (2) | 0.008 (2) | −0.013 (2) |
C6 | 0.056 (3) | 0.037 (3) | 0.048 (3) | −0.015 (2) | 0.021 (2) | −0.006 (2) |
C7 | 0.033 (3) | 0.046 (3) | 0.059 (3) | −0.012 (2) | 0.014 (2) | −0.013 (2) |
C8 | 0.032 (2) | 0.041 (3) | 0.046 (3) | −0.006 (2) | 0.0054 (19) | −0.010 (2) |
C9 | 0.024 (2) | 0.035 (2) | 0.035 (2) | 0.0034 (17) | −0.0006 (17) | −0.0043 (19) |
C10 | 0.030 (2) | 0.042 (2) | 0.028 (2) | 0.0017 (19) | 0.0023 (17) | −0.0077 (19) |
C11 | 0.027 (2) | 0.030 (2) | 0.025 (2) | 0.0009 (17) | 0.0024 (17) | −0.0107 (17) |
C12 | 0.028 (2) | 0.038 (2) | 0.023 (2) | −0.0013 (18) | 0.0014 (17) | −0.0117 (18) |
C13 | 0.036 (2) | 0.031 (2) | 0.028 (2) | −0.0030 (18) | 0.0096 (18) | −0.0100 (18) |
C14 | 0.029 (2) | 0.033 (2) | 0.027 (2) | −0.0059 (18) | 0.0062 (17) | −0.0111 (18) |
C15 | 0.038 (2) | 0.038 (3) | 0.032 (2) | −0.005 (2) | 0.0009 (19) | 0.0012 (19) |
C16 | 0.048 (3) | 0.041 (3) | 0.041 (3) | −0.019 (2) | 0.014 (2) | −0.007 (2) |
C17 | 0.037 (3) | 0.061 (3) | 0.033 (3) | −0.017 (2) | 0.008 (2) | −0.012 (2) |
C18 | 0.031 (2) | 0.055 (3) | 0.029 (2) | 0.005 (2) | −0.0023 (18) | −0.005 (2) |
C19 | 0.056 (3) | 0.042 (3) | 0.053 (3) | −0.004 (2) | 0.016 (2) | 0.000 (2) |
C20 | 0.067 (4) | 0.041 (3) | 0.072 (4) | −0.017 (3) | 0.024 (3) | −0.017 (3) |
C21 | 0.063 (4) | 0.063 (4) | 0.062 (3) | −0.031 (3) | 0.015 (3) | −0.024 (3) |
C22 | 0.052 (3) | 0.066 (3) | 0.036 (3) | −0.027 (2) | 0.006 (2) | −0.009 (2) |
C23 | 0.037 (2) | 0.042 (3) | 0.022 (2) | −0.0040 (19) | −0.0003 (17) | 0.0047 (19) |
C24 | 0.039 (2) | 0.045 (3) | 0.028 (2) | 0.004 (2) | 0.0040 (19) | 0.001 (2) |
C25 | 0.032 (2) | 0.038 (2) | 0.022 (2) | −0.0082 (18) | 0.0043 (17) | 0.0012 (18) |
C26 | 0.027 (2) | 0.045 (3) | 0.024 (2) | −0.0034 (19) | 0.0029 (17) | −0.0023 (19) |
C27 | 0.044 (3) | 0.036 (3) | 0.030 (2) | −0.007 (2) | 0.0108 (19) | −0.004 (2) |
C28 | 0.035 (2) | 0.046 (3) | 0.022 (2) | −0.014 (2) | 0.0078 (18) | −0.0038 (19) |
C29 | 0.032 (2) | 0.050 (3) | 0.032 (2) | −0.010 (2) | −0.0037 (18) | −0.002 (2) |
C30 | 0.055 (3) | 0.058 (3) | 0.092 (4) | −0.026 (3) | −0.009 (3) | −0.013 (3) |
C31 | 0.076 (4) | 0.053 (3) | 0.140 (6) | −0.030 (3) | −0.020 (4) | 0.011 (4) |
C32 | 0.053 (3) | 0.033 (2) | 0.040 (2) | −0.001 (2) | 0.005 (2) | 0.004 (2) |
C33 | 0.058 (3) | 0.062 (3) | 0.060 (3) | −0.026 (3) | 0.014 (2) | −0.021 (3) |
C34 | 0.064 (3) | 0.094 (4) | 0.041 (3) | −0.016 (3) | −0.015 (3) | −0.015 (3) |
C35 | 0.066 (4) | 0.081 (4) | 0.040 (3) | 0.003 (3) | −0.011 (2) | −0.003 (3) |
C36 | 0.071 (4) | 0.049 (3) | 0.051 (3) | 0.020 (3) | 0.003 (3) | 0.009 (2) |
C37 | 0.066 (3) | 0.043 (3) | 0.054 (3) | −0.001 (2) | 0.019 (3) | 0.007 (2) |
C38 | 0.054 (3) | 0.040 (3) | 0.067 (3) | −0.021 (2) | 0.020 (3) | −0.015 (2) |
K2 | 0.0336 (7) | 0.0359 (7) | 0.0297 (7) | −0.0080 (6) | 0.0011 (5) | −0.0015 (6) |
C39 | 0.048 (3) | 0.038 (3) | 0.048 (3) | −0.018 (2) | −0.004 (2) | 0.005 (2) |
C40 | 0.037 (2) | 0.037 (2) | 0.040 (2) | −0.0079 (19) | −0.0045 (19) | −0.011 (2) |
C41 | 0.033 (2) | 0.042 (3) | 0.034 (2) | −0.0061 (19) | −0.0041 (18) | −0.011 (2) |
C42 | 0.044 (3) | 0.040 (2) | 0.030 (2) | −0.006 (2) | −0.0063 (19) | −0.004 (2) |
C43 | 0.045 (3) | 0.050 (3) | 0.025 (2) | −0.008 (2) | 0.0001 (19) | −0.003 (2) |
C44 | 0.041 (3) | 0.051 (3) | 0.034 (2) | −0.018 (2) | −0.0033 (19) | 0.009 (2) |
O8 | 0.032 (4) | 0.066 (5) | 0.033 (3) | −0.002 (3) | 0.000 (2) | −0.002 (3) |
C45 | 0.050 (5) | 0.066 (7) | 0.038 (4) | −0.001 (6) | −0.008 (4) | −0.004 (6) |
C46 | 0.060 (7) | 0.162 (14) | 0.064 (7) | −0.042 (9) | −0.001 (6) | −0.014 (8) |
C47 | 0.044 (6) | 0.066 (10) | 0.057 (6) | −0.009 (6) | 0.013 (5) | −0.009 (7) |
C48 | 0.041 (5) | 0.042 (8) | 0.028 (4) | 0.004 (5) | −0.004 (4) | 0.000 (4) |
O8' | 0.060 (6) | 0.047 (6) | 0.053 (5) | −0.023 (5) | 0.016 (4) | −0.010 (5) |
C45' | 0.043 (7) | 0.027 (6) | 0.057 (8) | −0.006 (5) | 0.008 (6) | −0.007 (6) |
C46' | 0.056 (11) | 0.046 (9) | 0.038 (6) | −0.004 (8) | 0.010 (6) | 0.015 (6) |
C47' | 0.055 (10) | 0.050 (11) | 0.041 (7) | −0.013 (8) | 0.005 (7) | −0.008 (7) |
C48' | 0.049 (9) | 0.052 (7) | 0.041 (7) | −0.019 (6) | 0.009 (6) | −0.010 (6) |
O9 | 0.051 (2) | 0.114 (3) | 0.109 (3) | −0.023 (2) | 0.006 (2) | 0.012 (3) |
C49 | 0.060 (4) | 0.095 (5) | 0.132 (6) | −0.025 (3) | −0.053 (4) | 0.040 (4) |
C50 | 0.068 (4) | 0.084 (4) | 0.066 (4) | −0.013 (3) | −0.018 (3) | 0.020 (3) |
C51 | 0.041 (3) | 0.059 (3) | 0.041 (3) | −0.002 (2) | 0.000 (2) | −0.001 (2) |
C52 | 0.063 (3) | 0.049 (3) | 0.050 (3) | −0.003 (2) | 0.008 (3) | −0.003 (2) |
Geometric parameters (Å, º) top
V1—O1 | 2.135 (2) | C25—C26 | 1.433 (5) |
V1—C2 | 2.191 (4) | C27—C28 | 1.410 (5) |
V1—C16 | 2.200 (4) | C29—C30 | 1.497 (5) |
V1—C3 | 2.203 (4) | C29—H29A | 0.9900 |
V1—C17 | 2.208 (4) | C29—H29B | 0.9900 |
V1—C15 | 2.291 (4) | C30—C31 | 1.460 (6) |
V1—C1 | 2.293 (4) | C30—H30A | 0.9900 |
V1—C18 | 2.304 (4) | C30—H30B | 0.9900 |
V1—C4 | 2.307 (4) | C31—C32 | 1.503 (6) |
K1—O4i | 2.791 (3) | C31—H31A | 0.9900 |
K1—O4 | 2.791 (3) | C31—H31B | 0.9900 |
K1—O2 | 2.796 (3) | C32—H32A | 0.9900 |
K1—O2i | 2.796 (3) | C32—H32B | 0.9900 |
K1—O3 | 2.802 (3) | C33—C38i | 1.487 (6) |
K1—O3i | 2.802 (3) | C33—H33A | 0.9900 |
K1—C20i | 3.263 (5) | C33—H33B | 0.9900 |
K1—C20 | 3.264 (5) | C34—C35 | 1.496 (6) |
K1—C19 | 3.487 (4) | C34—H34A | 0.9900 |
K1—C19i | 3.487 (4) | C34—H34B | 0.9900 |
K1—H20 | 2.97 (4) | C35—H35A | 0.9900 |
O1—C32 | 1.437 (4) | C35—H35B | 0.9900 |
O1—C29 | 1.458 (4) | C36—C37 | 1.483 (6) |
O2—C33 | 1.401 (5) | C36—H36A | 0.9900 |
O2—C34 | 1.416 (5) | C36—H36B | 0.9900 |
O3—C35 | 1.414 (5) | C37—H37A | 0.9900 |
O3—C36 | 1.428 (5) | C37—H37B | 0.9900 |
O4—C37 | 1.411 (5) | C38—H38A | 0.9900 |
O4—C38 | 1.429 (5) | C38—H38B | 0.9900 |
O5—C39 | 1.413 (4) | K2—O8ii | 2.797 (6) |
O5—C40 | 1.429 (4) | K2—O8 | 2.797 (6) |
O5—K2 | 2.817 (2) | K2—O8' | 2.801 (10) |
O6—C42 | 1.416 (4) | K2—O8'ii | 2.801 (10) |
O6—C41 | 1.429 (4) | C39—C44ii | 1.487 (5) |
O6—K2 | 2.751 (2) | C39—H39A | 0.9900 |
O7—C44 | 1.421 (4) | C39—H39B | 0.9900 |
O7—C43 | 1.433 (4) | C40—C41 | 1.485 (5) |
O7—K2 | 2.830 (2) | C40—H40A | 0.9900 |
C1—C2 | 1.430 (5) | C40—H40B | 0.9900 |
C1—C11 | 1.454 (5) | C41—H41A | 0.9900 |
C1—H1 | 0.99 (3) | C41—H41B | 0.9900 |
C2—C3 | 1.371 (6) | C42—C43 | 1.494 (5) |
C2—H2 | 0.90 (4) | C42—H42A | 0.9900 |
C3—C4 | 1.409 (6) | C42—H42B | 0.9900 |
C3—H3 | 0.92 (4) | C43—H43A | 0.9900 |
C4—C12 | 1.454 (5) | C43—H43B | 0.9900 |
C4—H4 | 0.91 (4) | C44—H44A | 0.9900 |
C5—C6 | 1.385 (5) | C44—H44B | 0.9900 |
C5—C13 | 1.404 (5) | O8—C45 | 1.419 (9) |
C5—H5 | 0.9500 | O8—C48 | 1.437 (12) |
C6—C7 | 1.391 (6) | C45—C46 | 1.474 (14) |
C6—H6 | 0.9500 | C45—H45A | 0.9900 |
C7—C8 | 1.367 (5) | C45—H45B | 0.9900 |
C7—H7 | 0.9500 | C46—C47 | 1.529 (18) |
C8—C14 | 1.409 (5) | C46—H46A | 0.9900 |
C8—H8 | 0.9500 | C46—H46B | 0.9900 |
C9—C11 | 1.375 (5) | C47—C48 | 1.500 (17) |
C9—C14 | 1.416 (5) | C47—H47A | 0.9900 |
C9—H9 | 0.9500 | C47—H47B | 0.9900 |
C10—C12 | 1.372 (5) | C48—H48A | 0.9900 |
C10—C13 | 1.418 (5) | C48—H48B | 0.9900 |
C10—H10 | 0.9500 | O8'—C48' | 1.417 (12) |
C11—C12 | 1.445 (5) | O8'—C45' | 1.442 (14) |
C13—C14 | 1.431 (5) | C45'—C46' | 1.48 (2) |
C15—C16 | 1.431 (5) | C45'—H45C | 0.9900 |
C15—C25 | 1.449 (5) | C45'—H45D | 0.9900 |
C15—H15 | 0.99 (4) | C46'—C47' | 1.55 (2) |
C16—C17 | 1.379 (6) | C46'—H46C | 0.9900 |
C16—H16 | 0.92 (4) | C46'—H46D | 0.9900 |
C17—C18 | 1.415 (6) | C47'—C48' | 1.492 (16) |
C17—H17 | 0.93 (4) | C47'—H47C | 0.9900 |
C18—C26 | 1.456 (5) | C47'—H47D | 0.9900 |
C18—H18 | 0.93 (4) | C48'—H48C | 0.9900 |
C19—C20 | 1.378 (6) | C48'—H48D | 0.9900 |
C19—C27 | 1.411 (6) | O9—C52 | 1.389 (5) |
C19—H19 | 0.92 (4) | O9—C49 | 1.420 (6) |
C20—C21 | 1.375 (7) | C49—C50 | 1.496 (7) |
C20—H20 | 0.97 (4) | C49—H49A | 0.9900 |
C21—C22 | 1.378 (6) | C49—H49B | 0.9900 |
C21—H21 | 0.9500 | C50—C51 | 1.503 (6) |
C22—C28 | 1.412 (5) | C50—H50A | 0.9900 |
C22—H22 | 0.9500 | C50—H50B | 0.9900 |
C23—C25 | 1.386 (5) | C51—C52 | 1.500 (5) |
C23—C28 | 1.418 (5) | C51—H51A | 0.9900 |
C23—H23 | 0.9500 | C51—H51B | 0.9900 |
C24—C26 | 1.378 (5) | C52—H52A | 0.9900 |
C24—C27 | 1.429 (5) | C52—H52B | 0.9900 |
C24—H24 | 0.9500 | | |
| | | |
O1—V1—C2 | 125.52 (13) | C28—C27—C19 | 118.5 (4) |
O1—V1—C16 | 128.10 (13) | C28—C27—C24 | 118.1 (4) |
C2—V1—C16 | 92.81 (16) | C19—C27—C24 | 123.4 (4) |
O1—V1—C3 | 129.04 (13) | C27—C28—C22 | 118.9 (4) |
C2—V1—C3 | 36.36 (15) | C27—C28—C23 | 119.2 (3) |
C16—V1—C3 | 102.74 (16) | C22—C28—C23 | 121.9 (4) |
O1—V1—C17 | 128.08 (13) | O1—C29—C30 | 105.0 (3) |
C2—V1—C17 | 106.33 (16) | O1—C29—H29A | 110.7 |
C16—V1—C17 | 36.45 (15) | C30—C29—H29A | 110.7 |
C3—V1—C17 | 93.65 (15) | O1—C29—H29B | 110.7 |
O1—V1—C15 | 92.98 (12) | C30—C29—H29B | 110.7 |
C2—V1—C15 | 109.40 (16) | H29A—C29—H29B | 108.8 |
C16—V1—C15 | 37.09 (14) | C31—C30—C29 | 104.8 (4) |
C3—V1—C15 | 134.97 (16) | C31—C30—H30A | 110.8 |
C17—V1—C15 | 64.74 (16) | C29—C30—H30A | 110.8 |
O1—V1—C1 | 89.61 (12) | C31—C30—H30B | 110.8 |
C2—V1—C1 | 37.10 (14) | C29—C30—H30B | 110.8 |
C16—V1—C1 | 113.07 (16) | H30A—C30—H30B | 108.9 |
C3—V1—C1 | 64.51 (15) | C30—C31—C32 | 105.3 (4) |
C17—V1—C1 | 140.27 (16) | C30—C31—H31A | 110.7 |
C15—V1—C1 | 106.47 (15) | C32—C31—H31A | 110.7 |
O1—V1—C18 | 93.51 (13) | C30—C31—H31B | 110.7 |
C2—V1—C18 | 140.06 (16) | C32—C31—H31B | 110.7 |
C16—V1—C18 | 64.18 (17) | H31A—C31—H31B | 108.8 |
C3—V1—C18 | 113.93 (15) | O1—C32—C31 | 105.7 (3) |
C17—V1—C18 | 36.48 (15) | O1—C32—H32A | 110.6 |
C15—V1—C18 | 72.47 (15) | C31—C32—H32A | 110.6 |
C1—V1—C18 | 176.75 (16) | O1—C32—H32B | 110.6 |
O1—V1—C4 | 95.73 (13) | C31—C32—H32B | 110.6 |
C2—V1—C4 | 63.99 (17) | H32A—C32—H32B | 108.7 |
C16—V1—C4 | 134.89 (15) | O2—C33—C38i | 109.4 (4) |
C3—V1—C4 | 36.32 (14) | O2—C33—H33A | 109.8 |
C17—V1—C4 | 110.48 (15) | C38i—C33—H33A | 109.8 |
C15—V1—C4 | 171.15 (15) | O2—C33—H33B | 109.8 |
C1—V1—C4 | 72.11 (15) | C38i—C33—H33B | 109.8 |
C18—V1—C4 | 108.44 (15) | H33A—C33—H33B | 108.2 |
O4i—K1—O4 | 180.0 | O2—C34—C35 | 109.2 (4) |
O4i—K1—O2 | 60.96 (9) | O2—C34—H34A | 109.8 |
O4—K1—O2 | 119.04 (9) | C35—C34—H34A | 109.8 |
O4i—K1—O2i | 119.04 (9) | O2—C34—H34B | 109.8 |
O4—K1—O2i | 60.96 (9) | C35—C34—H34B | 109.8 |
O2—K1—O2i | 180.0 | H34A—C34—H34B | 108.3 |
O4i—K1—O3 | 119.05 (8) | O3—C35—C34 | 108.6 (4) |
O4—K1—O3 | 60.95 (8) | O3—C35—H35A | 110.0 |
O2—K1—O3 | 59.65 (9) | C34—C35—H35A | 110.0 |
O2i—K1—O3 | 120.35 (9) | O3—C35—H35B | 110.0 |
O4i—K1—O3i | 60.96 (8) | C34—C35—H35B | 110.0 |
O4—K1—O3i | 119.05 (8) | H35A—C35—H35B | 108.3 |
O2—K1—O3i | 120.35 (9) | O3—C36—C37 | 109.0 (4) |
O2i—K1—O3i | 59.65 (9) | O3—C36—H36A | 109.9 |
O3—K1—O3i | 180.0 | C37—C36—H36A | 109.9 |
O4i—K1—C20i | 88.03 (11) | O3—C36—H36B | 109.9 |
O4—K1—C20i | 91.97 (11) | C37—C36—H36B | 109.9 |
O2—K1—C20i | 76.24 (11) | H36A—C36—H36B | 108.3 |
O2i—K1—C20i | 103.76 (11) | O4—C37—C36 | 109.1 (4) |
O3—K1—C20i | 90.58 (12) | O4—C37—H37A | 109.9 |
O3i—K1—C20i | 89.42 (12) | C36—C37—H37A | 109.9 |
O4i—K1—C20 | 91.97 (11) | O4—C37—H37B | 109.9 |
O4—K1—C20 | 88.03 (11) | C36—C37—H37B | 109.9 |
O2—K1—C20 | 103.76 (11) | H37A—C37—H37B | 108.3 |
O2i—K1—C20 | 76.24 (11) | O4—C38—C33i | 109.1 (3) |
O3—K1—C20 | 89.42 (12) | O4—C38—H38A | 109.9 |
O3i—K1—C20 | 90.58 (12) | C33i—C38—H38A | 109.9 |
C20i—K1—C20 | 180.0 | O4—C38—H38B | 109.9 |
O4i—K1—C19 | 83.09 (9) | C33i—C38—H38B | 109.9 |
O4—K1—C19 | 96.91 (9) | H38A—C38—H38B | 108.3 |
O2—K1—C19 | 80.66 (10) | O6—K2—O6ii | 180.00 (4) |
O2i—K1—C19 | 99.34 (10) | O6—K2—O8ii | 106.19 (13) |
O3—K1—C19 | 75.28 (10) | O6ii—K2—O8ii | 73.82 (13) |
O3i—K1—C19 | 104.72 (10) | O6—K2—O8 | 73.81 (13) |
C20i—K1—C19 | 156.74 (11) | O6ii—K2—O8 | 106.19 (13) |
C20—K1—C19 | 23.26 (11) | O8ii—K2—O8 | 180.0 (2) |
O4i—K1—C19i | 96.91 (9) | O6—K2—O8' | 100.28 (19) |
O4—K1—C19i | 83.09 (9) | O6ii—K2—O8' | 79.72 (19) |
O2—K1—C19i | 99.34 (10) | O6—K2—O8'ii | 79.72 (19) |
O2i—K1—C19i | 80.66 (10) | O6ii—K2—O8'ii | 100.28 (19) |
O3—K1—C19i | 104.72 (10) | O8ii—K2—O8'ii | 30.5 (2) |
O3i—K1—C19i | 75.28 (10) | O8—K2—O8'ii | 149.5 (2) |
C20i—K1—C19i | 23.26 (11) | O8'—K2—O8'ii | 180.0 |
C20—K1—C19i | 156.74 (11) | O6—K2—O5ii | 118.35 (7) |
C19—K1—C19i | 180.0 | O6ii—K2—O5ii | 61.65 (7) |
O4i—K1—H20 | 109.0 (9) | O8ii—K2—O5ii | 75.54 (13) |
O4—K1—H20 | 71.0 (9) | O8—K2—O5ii | 104.46 (13) |
O2—K1—H20 | 113.7 (8) | O6—K2—O5 | 61.65 (7) |
O2i—K1—H20 | 66.3 (8) | O6ii—K2—O5 | 118.35 (7) |
O3—K1—H20 | 83.4 (8) | O8ii—K2—O5 | 104.46 (13) |
O3i—K1—H20 | 96.6 (8) | O8—K2—O5 | 75.54 (13) |
C20i—K1—H20 | 162.8 (8) | O8'—K2—O5 | 101.26 (18) |
C20—K1—H20 | 17.2 (8) | O8'ii—K2—O5 | 78.74 (18) |
C19—K1—H20 | 35.1 (8) | O5ii—K2—O5 | 180.0 |
C19i—K1—H20 | 144.9 (8) | O6—K2—O7 | 59.91 (7) |
C32—O1—C29 | 109.8 (3) | O6ii—K2—O7 | 120.09 (7) |
C32—O1—V1 | 126.8 (2) | O8ii—K2—O7 | 80.33 (14) |
C29—O1—V1 | 123.4 (2) | O8—K2—O7 | 99.67 (14) |
C33—O2—C34 | 112.9 (3) | O8'—K2—O7 | 100.6 (2) |
C33—O2—K1 | 113.3 (2) | O8'ii—K2—O7 | 79.4 (2) |
C34—O2—K1 | 117.0 (3) | O5ii—K2—O7 | 59.90 (7) |
C35—O3—C36 | 112.4 (3) | O5—K2—O7 | 120.10 (7) |
C35—O3—K1 | 114.9 (3) | O6—K2—O7ii | 120.09 (7) |
C36—O3—K1 | 114.1 (2) | O6ii—K2—O7ii | 59.91 (7) |
C37—O4—C38 | 111.5 (3) | O8ii—K2—O7ii | 99.67 (14) |
C37—O4—K1 | 112.0 (2) | O8—K2—O7ii | 80.33 (14) |
C38—O4—K1 | 113.6 (2) | O5ii—K2—O7ii | 120.10 (7) |
C39—O5—C40 | 113.0 (3) | O5—K2—O7ii | 59.90 (7) |
C39—O5—K2 | 114.4 (2) | O7—K2—O7ii | 180.0 |
C40—O5—K2 | 110.9 (2) | O5—C39—C44ii | 109.4 (3) |
C42—O6—C41 | 111.7 (3) | O5—C39—H39A | 109.8 |
C42—O6—K2 | 117.9 (2) | C44ii—C39—H39A | 109.8 |
C41—O6—K2 | 114.7 (2) | O5—C39—H39B | 109.8 |
C44—O7—C43 | 112.0 (3) | C44ii—C39—H39B | 109.8 |
C44—O7—K2 | 114.5 (2) | H39A—C39—H39B | 108.2 |
C43—O7—K2 | 114.4 (2) | O5—C40—C41 | 109.4 (3) |
C2—C1—C11 | 119.6 (4) | O5—C40—H40A | 109.8 |
C2—C1—V1 | 67.6 (2) | C41—C40—H40A | 109.8 |
C11—C1—V1 | 99.9 (2) | O5—C40—H40B | 109.8 |
C2—C1—H1 | 120 (2) | C41—C40—H40B | 109.8 |
C11—C1—H1 | 116 (2) | H40A—C40—H40B | 108.2 |
V1—C1—H1 | 121 (2) | O6—C41—C40 | 108.9 (3) |
C3—C2—C1 | 118.0 (4) | O6—C41—H41A | 109.9 |
C3—C2—V1 | 72.3 (2) | C40—C41—H41A | 109.9 |
C1—C2—V1 | 75.3 (2) | O6—C41—H41B | 109.9 |
C3—C2—H2 | 122 (3) | C40—C41—H41B | 109.9 |
C1—C2—H2 | 120 (3) | H41A—C41—H41B | 108.3 |
V1—C2—H2 | 117 (2) | O6—C42—C43 | 109.1 (3) |
C2—C3—C4 | 118.2 (4) | O6—C42—H42A | 109.9 |
C2—C3—V1 | 71.3 (2) | C43—C42—H42A | 109.9 |
C4—C3—V1 | 75.8 (2) | O6—C42—H42B | 109.9 |
C2—C3—H3 | 125 (2) | C43—C42—H42B | 109.9 |
C4—C3—H3 | 117 (2) | H42A—C42—H42B | 108.3 |
V1—C3—H3 | 122 (2) | O7—C43—C42 | 108.6 (3) |
C3—C4—C12 | 120.6 (4) | O7—C43—H43A | 110.0 |
C3—C4—V1 | 67.8 (2) | C42—C43—H43A | 110.0 |
C12—C4—V1 | 99.6 (2) | O7—C43—H43B | 110.0 |
C3—C4—H4 | 120 (2) | C42—C43—H43B | 110.0 |
C12—C4—H4 | 116 (2) | H43A—C43—H43B | 108.4 |
V1—C4—H4 | 121 (2) | O7—C44—C39ii | 108.5 (3) |
C6—C5—C13 | 120.9 (4) | O7—C44—H44A | 110.0 |
C6—C5—H5 | 119.5 | C39ii—C44—H44A | 110.0 |
C13—C5—H5 | 119.5 | O7—C44—H44B | 110.0 |
C5—C6—C7 | 119.9 (4) | C39ii—C44—H44B | 110.0 |
C5—C6—H6 | 120.0 | H44A—C44—H44B | 108.4 |
C7—C6—H6 | 120.0 | C45—O8—C48 | 105.7 (8) |
C8—C7—C6 | 120.6 (4) | C45—O8—K2 | 103.5 (7) |
C8—C7—H7 | 119.7 | C48—O8—K2 | 120.6 (7) |
C6—C7—H7 | 119.7 | O8—C45—C46 | 104.8 (10) |
C7—C8—C14 | 121.1 (4) | O8—C45—H45A | 110.8 |
C7—C8—H8 | 119.4 | C46—C45—H45A | 110.8 |
C14—C8—H8 | 119.4 | O8—C45—H45B | 110.8 |
C11—C9—C14 | 122.9 (4) | C46—C45—H45B | 110.8 |
C11—C9—H9 | 118.5 | H45A—C45—H45B | 108.9 |
C14—C9—H9 | 118.5 | C45—C46—C47 | 104.2 (10) |
C12—C10—C13 | 122.6 (4) | C45—C46—H46A | 110.9 |
C12—C10—H10 | 118.7 | C47—C46—H46A | 110.9 |
C13—C10—H10 | 118.7 | C45—C46—H46B | 110.9 |
C9—C11—C12 | 118.5 (3) | C47—C46—H46B | 110.9 |
C9—C11—C1 | 125.2 (4) | H46A—C46—H46B | 108.9 |
C12—C11—C1 | 116.0 (3) | C48—C47—C46 | 103.3 (9) |
C10—C12—C11 | 119.3 (3) | C48—C47—H47A | 111.1 |
C10—C12—C4 | 125.2 (4) | C46—C47—H47A | 111.1 |
C11—C12—C4 | 115.4 (3) | C48—C47—H47B | 111.1 |
C5—C13—C10 | 123.0 (4) | C46—C47—H47B | 111.1 |
C5—C13—C14 | 118.7 (4) | H47A—C47—H47B | 109.1 |
C10—C13—C14 | 118.3 (3) | O8—C48—C47 | 107.5 (9) |
C8—C14—C9 | 123.1 (4) | O8—C48—H48A | 110.2 |
C8—C14—C13 | 118.6 (4) | C47—C48—H48A | 110.2 |
C9—C14—C13 | 118.3 (3) | O8—C48—H48B | 110.2 |
C16—C15—C25 | 119.1 (4) | C47—C48—H48B | 110.2 |
C16—C15—V1 | 68.0 (2) | H48A—C48—H48B | 108.5 |
C25—C15—V1 | 99.5 (3) | C48'—O8'—C45' | 106.9 (10) |
C16—C15—H15 | 119 (2) | C48'—O8'—K2 | 103.7 (10) |
C25—C15—H15 | 117 (2) | C45'—O8'—K2 | 117.9 (10) |
V1—C15—H15 | 124 (2) | O8'—C45'—C46' | 105.5 (12) |
C17—C16—C15 | 118.1 (4) | O8'—C45'—H45C | 110.6 |
C17—C16—V1 | 72.1 (2) | C46'—C45'—H45C | 110.6 |
C15—C16—V1 | 74.9 (2) | O8'—C45'—H45D | 110.6 |
C17—C16—H16 | 124 (3) | C46'—C45'—H45D | 110.6 |
C15—C16—H16 | 118 (3) | H45C—C45'—H45D | 108.8 |
V1—C16—H16 | 118 (2) | C45'—C46'—C47' | 104.8 (10) |
C16—C17—C18 | 118.0 (4) | C45'—C46'—H46C | 110.8 |
C16—C17—V1 | 71.5 (2) | C47'—C46'—H46C | 110.8 |
C18—C17—V1 | 75.5 (2) | C45'—C46'—H46D | 110.8 |
C16—C17—H17 | 122 (2) | C47'—C46'—H46D | 110.8 |
C18—C17—H17 | 120 (2) | H46C—C46'—H46D | 108.9 |
V1—C17—H17 | 119 (2) | C48'—C47'—C46' | 104.1 (11) |
C17—C18—C26 | 119.4 (4) | C48'—C47'—H47C | 110.9 |
C17—C18—V1 | 68.0 (2) | C46'—C47'—H47C | 110.9 |
C26—C18—V1 | 99.7 (2) | C48'—C47'—H47D | 110.9 |
C17—C18—H18 | 121 (2) | C46'—C47'—H47D | 110.9 |
C26—C18—H18 | 116 (2) | H47C—C47'—H47D | 109.0 |
V1—C18—H18 | 121 (2) | O8'—C48'—C47' | 106.1 (11) |
C20—C19—C27 | 121.4 (5) | O8'—C48'—H48C | 110.5 |
C20—C19—K1 | 69.2 (3) | C47'—C48'—H48C | 110.5 |
C27—C19—K1 | 122.5 (3) | O8'—C48'—H48D | 110.5 |
C20—C19—H19 | 118 (3) | C47'—C48'—H48D | 110.5 |
C27—C19—H19 | 121 (3) | H48C—C48'—H48D | 108.7 |
K1—C19—H19 | 79 (3) | C52—O9—C49 | 109.1 (4) |
C21—C20—C19 | 119.8 (5) | O9—C49—C50 | 107.5 (4) |
C21—C20—K1 | 113.3 (3) | O9—C49—H49A | 110.2 |
C19—C20—K1 | 87.5 (3) | C50—C49—H49A | 110.2 |
C21—C20—H20 | 124 (3) | O9—C49—H49B | 110.2 |
C19—C20—H20 | 116 (3) | C50—C49—H49B | 110.2 |
K1—C20—H20 | 64 (3) | H49A—C49—H49B | 108.5 |
C20—C21—C22 | 120.8 (5) | C49—C50—C51 | 102.1 (4) |
C20—C21—H21 | 119.6 | C49—C50—H50A | 111.3 |
C22—C21—H21 | 119.6 | C51—C50—H50A | 111.3 |
C21—C22—C28 | 120.6 (5) | C49—C50—H50B | 111.3 |
C21—C22—H22 | 119.7 | C51—C50—H50B | 111.3 |
C28—C22—H22 | 119.7 | H50A—C50—H50B | 109.2 |
C25—C23—C28 | 122.3 (4) | C52—C51—C50 | 102.2 (4) |
C25—C23—H23 | 118.9 | C52—C51—H51A | 111.3 |
C28—C23—H23 | 118.9 | C50—C51—H51A | 111.3 |
C26—C24—C27 | 122.2 (4) | C52—C51—H51B | 111.3 |
C26—C24—H24 | 118.9 | C50—C51—H51B | 111.3 |
C27—C24—H24 | 118.9 | H51A—C51—H51B | 109.2 |
C23—C25—C26 | 118.5 (3) | O9—C52—C51 | 107.7 (4) |
C23—C25—C15 | 124.8 (4) | O9—C52—H52A | 110.2 |
C26—C25—C15 | 116.5 (3) | C51—C52—H52A | 110.2 |
C24—C26—C25 | 119.6 (3) | O9—C52—H52B | 110.2 |
C24—C26—C18 | 124.2 (4) | C51—C52—H52B | 110.2 |
C25—C26—C18 | 115.9 (3) | H52A—C52—H52B | 108.5 |
| | | |
C11—C1—C2—C3 | 28.5 (5) | V1—C18—C26—C25 | 40.0 (4) |
V1—C1—C2—C3 | −60.3 (3) | C20—C19—C27—C28 | 0.4 (6) |
C11—C1—C2—V1 | 88.8 (3) | K1—C19—C27—C28 | 84.4 (4) |
C1—C2—C3—C4 | 0.2 (6) | C20—C19—C27—C24 | 178.0 (4) |
V1—C2—C3—C4 | −61.7 (3) | K1—C19—C27—C24 | −97.9 (4) |
C1—C2—C3—V1 | 61.9 (3) | C26—C24—C27—C28 | 2.1 (5) |
C2—C3—C4—C12 | −28.8 (5) | C26—C24—C27—C19 | −175.5 (4) |
V1—C3—C4—C12 | −88.2 (3) | C19—C27—C28—C22 | −1.4 (5) |
C2—C3—C4—V1 | 59.4 (3) | C24—C27—C28—C22 | −179.2 (3) |
C13—C5—C6—C7 | 1.0 (6) | C19—C27—C28—C23 | 178.2 (3) |
C5—C6—C7—C8 | −1.5 (6) | C24—C27—C28—C23 | 0.5 (5) |
C6—C7—C8—C14 | 0.2 (6) | C21—C22—C28—C27 | 1.5 (6) |
C14—C9—C11—C12 | −0.5 (5) | C21—C22—C28—C23 | −178.2 (4) |
C14—C9—C11—C1 | 173.4 (3) | C25—C23—C28—C27 | −2.4 (5) |
C2—C1—C11—C9 | 157.7 (4) | C25—C23—C28—C22 | 177.3 (3) |
V1—C1—C11—C9 | −132.6 (3) | C32—O1—C29—C30 | 12.8 (4) |
C2—C1—C11—C12 | −28.2 (5) | V1—O1—C29—C30 | −167.6 (3) |
V1—C1—C11—C12 | 41.5 (3) | O1—C29—C30—C31 | −27.2 (5) |
C13—C10—C12—C11 | 2.8 (5) | C29—C30—C31—C32 | 31.0 (6) |
C13—C10—C12—C4 | −174.4 (3) | C29—O1—C32—C31 | 6.2 (4) |
C9—C11—C12—C10 | −2.3 (5) | V1—O1—C32—C31 | −173.4 (3) |
C1—C11—C12—C10 | −176.8 (3) | C30—C31—C32—O1 | −23.3 (5) |
C9—C11—C12—C4 | 175.1 (3) | C34—O2—C33—C38i | 173.1 (4) |
C1—C11—C12—C4 | 0.6 (4) | K1—O2—C33—C38i | −50.8 (4) |
C3—C4—C12—C10 | −154.9 (4) | C33—O2—C34—C35 | 177.6 (4) |
V1—C4—C12—C10 | 135.2 (3) | K1—O2—C34—C35 | 43.3 (5) |
C3—C4—C12—C11 | 27.8 (5) | C36—O3—C35—C34 | −175.7 (4) |
V1—C4—C12—C11 | −42.1 (3) | K1—O3—C35—C34 | 51.7 (4) |
C6—C5—C13—C10 | −179.2 (3) | O2—C34—C35—O3 | −62.6 (5) |
C6—C5—C13—C14 | 0.8 (5) | C35—O3—C36—C37 | −177.6 (4) |
C12—C10—C13—C5 | 179.6 (3) | K1—O3—C36—C37 | −44.5 (4) |
C12—C10—C13—C14 | −0.4 (5) | C38—O4—C37—C36 | 176.5 (3) |
C7—C8—C14—C9 | −178.0 (3) | K1—O4—C37—C36 | −55.0 (4) |
C7—C8—C14—C13 | 1.7 (5) | O3—C36—C37—O4 | 67.7 (4) |
C11—C9—C14—C8 | −177.4 (3) | C37—O4—C38—C33i | 175.5 (3) |
C11—C9—C14—C13 | 2.9 (5) | K1—O4—C38—C33i | 47.9 (4) |
C5—C13—C14—C8 | −2.1 (5) | C40—O5—C39—C44ii | 178.1 (3) |
C10—C13—C14—C8 | 177.9 (3) | K2—O5—C39—C44ii | 50.0 (4) |
C5—C13—C14—C9 | 177.6 (3) | C39—O5—C40—C41 | 178.3 (3) |
C10—C13—C14—C9 | −2.4 (5) | K2—O5—C40—C41 | −51.7 (3) |
C25—C15—C16—C17 | −29.1 (5) | C42—O6—C41—C40 | 174.9 (3) |
V1—C15—C16—C17 | 59.6 (3) | K2—O6—C41—C40 | −47.7 (3) |
C25—C15—C16—V1 | −88.8 (3) | O5—C40—C41—O6 | 67.8 (4) |
C15—C16—C17—C18 | 0.4 (6) | C41—O6—C42—C43 | −176.9 (3) |
V1—C16—C17—C18 | 61.5 (3) | K2—O6—C42—C43 | 47.2 (4) |
C15—C16—C17—V1 | −61.1 (3) | C44—O7—C43—C42 | −179.9 (3) |
C16—C17—C18—C26 | 29.5 (5) | K2—O7—C43—C42 | 47.8 (3) |
V1—C17—C18—C26 | 88.9 (3) | O6—C42—C43—O7 | −62.3 (4) |
C16—C17—C18—V1 | −59.4 (3) | C43—O7—C44—C39ii | 179.0 (3) |
C27—C19—C20—C21 | 0.7 (7) | K2—O7—C44—C39ii | −48.6 (4) |
K1—C19—C20—C21 | −115.6 (5) | C48—O8—C45—C46 | 38.8 (13) |
C27—C19—C20—K1 | 116.2 (4) | K2—O8—C45—C46 | −88.8 (10) |
C19—C20—C21—C22 | −0.6 (7) | O8—C45—C46—C47 | −34.6 (17) |
K1—C20—C21—C22 | −101.7 (4) | C45—C46—C47—C48 | 17 (2) |
C20—C21—C22—C28 | −0.5 (7) | C45—O8—C48—C47 | −27.5 (15) |
C28—C23—C25—C26 | 1.7 (5) | K2—O8—C48—C47 | 89.2 (14) |
C28—C23—C25—C15 | −173.5 (3) | C46—C47—C48—O8 | 5 (2) |
C16—C15—C25—C23 | −157.2 (4) | C48'—O8'—C45'—C46' | 35 (2) |
V1—C15—C25—C23 | 132.8 (3) | K2—O8'—C45'—C46' | −81.0 (18) |
C16—C15—C25—C26 | 27.5 (5) | O8'—C45'—C46'—C47' | −21 (3) |
V1—C15—C25—C26 | −42.6 (3) | C45'—C46'—C47'—C48' | 0 (3) |
C27—C24—C26—C25 | −2.8 (5) | C45'—O8'—C48'—C47' | −35.1 (19) |
C27—C24—C26—C18 | 171.7 (4) | K2—O8'—C48'—C47' | 90.1 (14) |
C23—C25—C26—C24 | 0.9 (5) | C46'—C47'—C48'—O8' | 21 (2) |
C15—C25—C26—C24 | 176.5 (3) | C52—O9—C49—C50 | 8.9 (6) |
C23—C25—C26—C18 | −174.0 (3) | O9—C49—C50—C51 | −26.6 (6) |
C15—C25—C26—C18 | 1.6 (5) | C49—C50—C51—C52 | 32.8 (5) |
C17—C18—C26—C24 | 155.2 (4) | C49—O9—C52—C51 | 13.0 (5) |
V1—C18—C26—C24 | −134.6 (3) | C50—C51—C52—O9 | −29.2 (5) |
C17—C18—C26—C25 | −30.1 (5) | | |
Symmetry codes: (i) −x+2, −y, −z; (ii) −x+1, −y+2, −z+1. |
(1,4,7,10,13,16-Hexaoxacyclooctadecane)bis(tetrahydrofuran)potassium bis(
η4-anthracene)(trimethylphosphane)vanadium
tetrahydrofuran monosolvate (6)
top
Crystal data top
[K(C20H40O8)][V(C14H10)2(C3H9P)]·C4H8O | Z = 2 |
Mr = 1003.17 | F(000) = 1072 |
Triclinic, P1 | Dx = 1.249 Mg m−3 |
a = 9.6431 (12) Å | Mo Kα radiation, λ = 0.71073 Å |
b = 14.4883 (18) Å | Cell parameters from 2957 reflections |
c = 20.804 (3) Å | θ = 2.3–25.0° |
α = 74.992 (2)° | µ = 0.35 mm−1 |
β = 84.667 (2)° | T = 173 K |
γ = 71.815 (2)° | Block, green |
V = 2667.0 (6) Å3 | 0.40 × 0.20 × 0.20 mm |
Data collection top
Siemens SMART CCD platform diffractometer | 6704 reflections with I > 2σ(I) |
Radiation source: normal-focus sealed tube | Rint = 0.039 |
ω scans | θmax = 25.1°, θmin = 1.5° |
Absorption correction: multi-scan (SADABS; Sheldrick, 1996) | h = −11→11 |
Tmin = 0.874, Tmax = 0.934 | k = −17→17 |
23058 measured reflections | l = −24→24 |
9330 independent reflections | |
Refinement top
Refinement on F2 | Primary atom site location: structure-invariant direct methods |
Least-squares matrix: full | Secondary atom site location: difference Fourier map |
R[F2 > 2σ(F2)] = 0.054 | Hydrogen site location: mixed |
wR(F2) = 0.118 | H atoms treated by a mixture of independent and constrained refinement |
S = 1.07 | w = 1/[σ2(Fo2) + (0.0392P)2 + 2.0007P] where P = (Fo2 + 2Fc2)/3 |
9330 reflections | (Δ/σ)max = 0.001 |
773 parameters | Δρmax = 0.31 e Å−3 |
409 restraints | Δρmin = −0.42 e Å−3 |
Special details top
Geometry. All esds (except the esd in the dihedral angle between two l.s. planes)
are estimated using the full covariance matrix. The cell esds are taken
into account individually in the estimation of esds in distances, angles
and torsion angles; correlations between esds in cell parameters are only
used when they are defined by crystal symmetry. An approximate (isotropic)
treatment of cell esds is used for estimating esds involving l.s. planes. |
Refinement. The positional parameters of the hydrogen atoms on the
metal-coordinating carbon atoms were refined to best describe
their true positions. THF ligand O4/C38-C41 is modeled as disordered over two positions
(0.815 (7):0.185 (7)) and THF ligand O8/C48-C51 is modeled as
disordered over three positions (0.45 (1):0.39 (1):0.16 (1)). Analogous bond lengths and angles among the disordered THF
ligands were restrained to be similar. Anisotropic displacement
parameters for proximal atoms were restrained to be similar and
restrained toward the expected motion relative to bond direction. |
Fractional atomic coordinates and isotropic or equivalent isotropic displacement parameters (Å2) top | x | y | z | Uiso*/Ueq | Occ. (<1) |
V1 | 0.14191 (5) | 0.67738 (4) | 0.82810 (2) | 0.02842 (14) | |
P1 | −0.12299 (8) | 0.72274 (6) | 0.80245 (4) | 0.0333 (2) | |
C1 | 0.2684 (3) | 0.5893 (2) | 0.92309 (15) | 0.0301 (7) | |
H1 | 0.291 (3) | 0.620 (2) | 0.9525 (15) | 0.036* | |
C2 | 0.1276 (3) | 0.5751 (2) | 0.92835 (15) | 0.0322 (7) | |
H2 | 0.059 (3) | 0.597 (2) | 0.9608 (15) | 0.039* | |
C3 | 0.0926 (3) | 0.5349 (2) | 0.88069 (15) | 0.0316 (7) | |
H3 | 0.001 (3) | 0.523 (2) | 0.8818 (14) | 0.038* | |
C4 | 0.1979 (3) | 0.5096 (2) | 0.83079 (16) | 0.0320 (7) | |
H4 | 0.172 (3) | 0.487 (2) | 0.7972 (15) | 0.038* | |
C5 | 0.7249 (3) | 0.3443 (2) | 0.79159 (15) | 0.0386 (8) | |
H5 | 0.701343 | 0.317400 | 0.758433 | 0.046* | |
C6 | 0.8693 (4) | 0.3223 (2) | 0.80726 (17) | 0.0440 (9) | |
H6 | 0.943795 | 0.280351 | 0.785381 | 0.053* | |
C7 | 0.9056 (3) | 0.3622 (2) | 0.85545 (16) | 0.0399 (8) | |
H7 | 1.005075 | 0.347975 | 0.865994 | 0.048* | |
C8 | 0.7976 (3) | 0.4218 (2) | 0.88759 (15) | 0.0332 (7) | |
H8 | 0.824055 | 0.447642 | 0.920614 | 0.040* | |
C9 | 0.5344 (3) | 0.50584 (19) | 0.90630 (14) | 0.0264 (6) | |
H9 | 0.558681 | 0.534034 | 0.938537 | 0.032* | |
C10 | 0.4616 (3) | 0.4255 (2) | 0.81069 (14) | 0.0312 (7) | |
H10 | 0.436003 | 0.398307 | 0.778228 | 0.037* | |
C11 | 0.3896 (3) | 0.52456 (19) | 0.89342 (13) | 0.0243 (6) | |
C12 | 0.3518 (3) | 0.4829 (2) | 0.84349 (13) | 0.0262 (6) | |
C13 | 0.6114 (3) | 0.4053 (2) | 0.82333 (14) | 0.0298 (7) | |
C14 | 0.6494 (3) | 0.4457 (2) | 0.87310 (14) | 0.0278 (6) | |
C15 | 0.2101 (3) | 0.7463 (2) | 0.72187 (16) | 0.0324 (7) | |
H15 | 0.227 (3) | 0.713 (2) | 0.6895 (15) | 0.039* | |
C16 | 0.3252 (3) | 0.7173 (2) | 0.76805 (16) | 0.0338 (7) | |
H16 | 0.412 (3) | 0.664 (2) | 0.7650 (14) | 0.041* | |
C17 | 0.2998 (3) | 0.7635 (2) | 0.82006 (16) | 0.0347 (7) | |
H17 | 0.370 (3) | 0.744 (2) | 0.8539 (15) | 0.042* | |
C18 | 0.1610 (3) | 0.8361 (2) | 0.82346 (16) | 0.0358 (7) | |
H18 | 0.141 (3) | 0.866 (2) | 0.8596 (15) | 0.043* | |
C19 | −0.1767 (4) | 1.1440 (2) | 0.6823 (2) | 0.0589 (11) | |
H19 | −0.197484 | 1.175784 | 0.718212 | 0.071* | |
C20 | −0.2464 (5) | 1.1928 (3) | 0.6228 (3) | 0.0731 (13) | |
H20 | −0.315036 | 1.257459 | 0.617978 | 0.088* | |
C21 | −0.2167 (4) | 1.1479 (3) | 0.5697 (2) | 0.0686 (12) | |
H21 | −0.264274 | 1.182354 | 0.528497 | 0.082* | |
C22 | −0.1190 (4) | 1.0538 (3) | 0.57614 (19) | 0.0519 (9) | |
H22 | −0.100366 | 1.023883 | 0.539402 | 0.062* | |
C23 | 0.0540 (3) | 0.9031 (2) | 0.64598 (15) | 0.0351 (7) | |
H23 | 0.077318 | 0.873080 | 0.609248 | 0.042* | |
C24 | −0.0015 (3) | 0.9946 (2) | 0.75195 (17) | 0.0405 (8) | |
H24 | −0.016703 | 1.026881 | 0.787472 | 0.049* | |
C25 | 0.1181 (3) | 0.8500 (2) | 0.70642 (15) | 0.0315 (7) | |
C26 | 0.0907 (3) | 0.8983 (2) | 0.76123 (15) | 0.0329 (7) | |
C27 | −0.0745 (3) | 1.0472 (2) | 0.69116 (18) | 0.0426 (8) | |
C28 | −0.0459 (3) | 1.0010 (2) | 0.63674 (17) | 0.0396 (8) | |
C29 | −0.1635 (4) | 0.6493 (3) | 0.75131 (17) | 0.0484 (9) | |
H29A | −0.269525 | 0.666094 | 0.747409 | 0.073* | |
H29B | −0.123124 | 0.577818 | 0.772163 | 0.073* | |
H29C | −0.119720 | 0.664738 | 0.706932 | 0.073* | |
C30 | −0.2472 (3) | 0.7031 (2) | 0.87313 (16) | 0.0424 (8) | |
H30A | −0.341494 | 0.706816 | 0.856930 | 0.064* | |
H30B | −0.261139 | 0.754908 | 0.897492 | 0.064* | |
H30C | −0.205433 | 0.636958 | 0.902827 | 0.064* | |
C31 | −0.2266 (4) | 0.8493 (2) | 0.75948 (19) | 0.0534 (10) | |
H31A | −0.327749 | 0.851702 | 0.754329 | 0.080* | |
H31B | −0.182614 | 0.867750 | 0.715499 | 0.080* | |
H31C | −0.225084 | 0.896477 | 0.785540 | 0.080* | |
K1 | 0.500000 | 0.000000 | 1.000000 | 0.0319 (2) | |
O1 | 0.4224 (2) | −0.17579 (14) | 1.04205 (10) | 0.0369 (5) | |
O2 | 0.7082 (2) | −0.17985 (14) | 0.99839 (10) | 0.0363 (5) | |
O3 | 0.8013 (2) | −0.00662 (15) | 0.98100 (10) | 0.0365 (5) | |
C32 | 0.2744 (3) | −0.1698 (2) | 1.03501 (16) | 0.0389 (8) | |
H32A | 0.255595 | −0.232793 | 1.060398 | 0.047* | |
H32B | 0.253243 | −0.159594 | 0.987579 | 0.047* | |
C33 | 0.5225 (3) | −0.2592 (2) | 1.02242 (16) | 0.0393 (8) | |
H33A | 0.515182 | −0.251092 | 0.974004 | 0.047* | |
H33B | 0.499415 | −0.321395 | 1.046152 | 0.047* | |
C34 | 0.6737 (4) | −0.2660 (2) | 1.03873 (16) | 0.0416 (8) | |
H34A | 0.679136 | −0.268272 | 1.086423 | 0.050* | |
H34B | 0.744067 | −0.327675 | 1.029669 | 0.050* | |
C35 | 0.8558 (3) | −0.1830 (2) | 1.00367 (18) | 0.0434 (8) | |
H35A | 0.922606 | −0.244036 | 0.992115 | 0.052* | |
H35B | 0.875611 | −0.184825 | 1.049906 | 0.052* | |
C36 | 0.8806 (3) | −0.0922 (2) | 0.95727 (17) | 0.0422 (8) | |
H36A | 0.985990 | −0.098319 | 0.954586 | 0.051* | |
H36B | 0.847428 | −0.085275 | 0.912151 | 0.051* | |
C37 | 0.8201 (3) | 0.0840 (2) | 0.93909 (16) | 0.0399 (8) | |
H37A | 0.792780 | 0.091390 | 0.892907 | 0.048* | |
H37B | 0.923578 | 0.082283 | 0.938860 | 0.048* | |
O4 | 0.5010 (5) | 0.0235 (3) | 0.86625 (17) | 0.0623 (12) | 0.815 (7) |
C38 | 0.3935 (7) | −0.0098 (4) | 0.8448 (3) | 0.0645 (17) | 0.815 (7) |
H38A | 0.341475 | −0.041157 | 0.883393 | 0.077* | 0.815 (7) |
H38B | 0.438233 | −0.058855 | 0.817769 | 0.077* | 0.815 (7) |
C39 | 0.2904 (7) | 0.0845 (5) | 0.8035 (4) | 0.091 (2) | 0.815 (7) |
H39A | 0.249748 | 0.069793 | 0.766644 | 0.109* | 0.815 (7) |
H39B | 0.208955 | 0.115367 | 0.831239 | 0.109* | 0.815 (7) |
C40 | 0.3829 (8) | 0.1516 (5) | 0.7773 (4) | 0.094 (2) | 0.815 (7) |
H40A | 0.336120 | 0.218530 | 0.786073 | 0.113* | 0.815 (7) |
H40B | 0.399387 | 0.159499 | 0.728776 | 0.113* | 0.815 (7) |
C41 | 0.5243 (8) | 0.1010 (6) | 0.8138 (3) | 0.060 (2) | 0.815 (7) |
H41A | 0.602689 | 0.073354 | 0.783609 | 0.072* | 0.815 (7) |
H41B | 0.553454 | 0.149308 | 0.831537 | 0.072* | 0.815 (7) |
O4' | 0.419 (3) | 0.0681 (17) | 0.8714 (7) | 0.081 (5) | 0.185 (7) |
C38' | 0.320 (3) | 0.029 (2) | 0.8481 (11) | 0.068 (5) | 0.185 (7) |
H38C | 0.217997 | 0.069745 | 0.853210 | 0.081* | 0.185 (7) |
H38D | 0.332120 | −0.040978 | 0.872847 | 0.081* | 0.185 (7) |
C39' | 0.360 (3) | 0.035 (2) | 0.7758 (10) | 0.076 (6) | 0.185 (7) |
H39C | 0.413305 | −0.032185 | 0.769307 | 0.091* | 0.185 (7) |
H39D | 0.270813 | 0.062433 | 0.748612 | 0.091* | 0.185 (7) |
C40' | 0.453 (3) | 0.101 (2) | 0.7558 (9) | 0.071 (6) | 0.185 (7) |
H40C | 0.400592 | 0.164636 | 0.724489 | 0.086* | 0.185 (7) |
H40D | 0.543554 | 0.068485 | 0.733961 | 0.086* | 0.185 (7) |
C41' | 0.486 (5) | 0.122 (3) | 0.8186 (11) | 0.067 (7) | 0.185 (7) |
H41C | 0.593297 | 0.099480 | 0.825153 | 0.080* | 0.185 (7) |
H41D | 0.448869 | 0.194248 | 0.816440 | 0.080* | 0.185 (7) |
K2 | 1.000000 | 0.500000 | 0.500000 | 0.0440 (3) | |
O5 | 1.0375 (3) | 0.29683 (15) | 0.52926 (11) | 0.0474 (6) | |
O6 | 1.1351 (3) | 0.37377 (16) | 0.62033 (11) | 0.0507 (6) | |
O7 | 1.0386 (3) | 0.58458 (17) | 0.60017 (11) | 0.0521 (6) | |
C42 | 1.1244 (4) | 0.2336 (2) | 0.58431 (17) | 0.0512 (9) | |
H42A | 1.229190 | 0.220053 | 0.571868 | 0.061* | |
H42B | 1.102219 | 0.168983 | 0.598290 | 0.061* | |
C43 | 1.0914 (4) | 0.2850 (2) | 0.63992 (17) | 0.0517 (9) | |
H43A | 0.985545 | 0.302301 | 0.650431 | 0.062* | |
H43B | 1.144691 | 0.240072 | 0.680241 | 0.062* | |
C44 | 1.1191 (5) | 0.4230 (3) | 0.67292 (17) | 0.0579 (10) | |
H44A | 1.187876 | 0.380888 | 0.709073 | 0.069* | |
H44B | 1.018492 | 0.434864 | 0.691426 | 0.069* | |
C45 | 1.1508 (5) | 0.5209 (3) | 0.64501 (18) | 0.0604 (11) | |
H45A | 1.154767 | 0.552331 | 0.681471 | 0.072* | |
H45B | 1.246431 | 0.509555 | 0.621471 | 0.072* | |
C46 | 1.0527 (5) | 0.6825 (3) | 0.57669 (19) | 0.0628 (11) | |
H46A | 1.150069 | 0.678723 | 0.555688 | 0.075* | |
H46B | 1.043599 | 0.713886 | 0.614481 | 0.075* | |
C47 | 0.9369 (5) | 0.7444 (3) | 0.52727 (17) | 0.0545 (10) | |
H47A | 0.839521 | 0.743939 | 0.546900 | 0.065* | |
H47B | 0.939821 | 0.814515 | 0.514155 | 0.065* | |
O8 | 0.7227 (13) | 0.5501 (14) | 0.5475 (7) | 0.087 (5) | 0.388 (12) |
C48 | 0.603 (2) | 0.6311 (15) | 0.5218 (8) | 0.069 (5) | 0.388 (12) |
H48A | 0.588376 | 0.635151 | 0.474603 | 0.082* | 0.388 (12) |
H48B | 0.616589 | 0.694728 | 0.525140 | 0.082* | 0.388 (12) |
C49 | 0.4768 (13) | 0.6110 (14) | 0.5638 (7) | 0.075 (4) | 0.388 (12) |
H49A | 0.416759 | 0.586829 | 0.539691 | 0.090* | 0.388 (12) |
H49B | 0.414507 | 0.672237 | 0.576615 | 0.090* | 0.388 (12) |
C50 | 0.5442 (14) | 0.5320 (17) | 0.6237 (8) | 0.098 (5) | 0.388 (12) |
H50A | 0.506200 | 0.554090 | 0.664794 | 0.117* | 0.388 (12) |
H50B | 0.521703 | 0.469120 | 0.625574 | 0.117* | 0.388 (12) |
C51 | 0.7048 (15) | 0.5160 (17) | 0.6169 (8) | 0.079 (5) | 0.388 (12) |
H51A | 0.736122 | 0.555798 | 0.641602 | 0.095* | 0.388 (12) |
H51B | 0.760026 | 0.444369 | 0.632816 | 0.095* | 0.388 (12) |
O8' | 0.7529 (17) | 0.508 (2) | 0.5754 (12) | 0.084 (5) | 0.162 (9) |
C48' | 0.657 (3) | 0.532 (4) | 0.5240 (16) | 0.072 (6) | 0.162 (9) |
H48C | 0.650532 | 0.470302 | 0.513818 | 0.087* | 0.162 (9) |
H48D | 0.690381 | 0.573053 | 0.483444 | 0.087* | 0.162 (9) |
C49' | 0.513 (3) | 0.589 (4) | 0.547 (2) | 0.088 (6) | 0.162 (9) |
H49C | 0.439017 | 0.554568 | 0.547843 | 0.105* | 0.162 (9) |
H49D | 0.479134 | 0.657241 | 0.517755 | 0.105* | 0.162 (9) |
C50' | 0.535 (3) | 0.595 (4) | 0.616 (2) | 0.097 (7) | 0.162 (9) |
H50C | 0.497015 | 0.665265 | 0.620630 | 0.116* | 0.162 (9) |
H50D | 0.484791 | 0.553628 | 0.649672 | 0.116* | 0.162 (9) |
C51' | 0.695 (3) | 0.556 (3) | 0.6254 (16) | 0.082 (7) | 0.162 (9) |
H51C | 0.736056 | 0.612197 | 0.622283 | 0.099* | 0.162 (9) |
H51D | 0.718822 | 0.509293 | 0.669622 | 0.099* | 0.162 (9) |
O8" | 0.7093 (12) | 0.5178 (12) | 0.5375 (7) | 0.093 (5) | 0.451 (11) |
C48" | 0.596 (2) | 0.6049 (14) | 0.5134 (7) | 0.083 (5) | 0.451 (11) |
H48E | 0.521069 | 0.588976 | 0.492075 | 0.099* | 0.451 (11) |
H48F | 0.633410 | 0.653867 | 0.479930 | 0.099* | 0.451 (11) |
C49" | 0.5305 (18) | 0.6469 (9) | 0.5712 (7) | 0.099 (4) | 0.451 (11) |
H49E | 0.550308 | 0.711187 | 0.567382 | 0.118* | 0.451 (11) |
H49F | 0.423476 | 0.659146 | 0.572870 | 0.118* | 0.451 (11) |
C50" | 0.597 (2) | 0.5734 (11) | 0.6315 (6) | 0.095 (4) | 0.451 (11) |
H50E | 0.522847 | 0.561523 | 0.666105 | 0.114* | 0.451 (11) |
H50F | 0.669752 | 0.594899 | 0.650040 | 0.114* | 0.451 (11) |
C51" | 0.6703 (18) | 0.4810 (9) | 0.6049 (7) | 0.093 (5) | 0.451 (11) |
H51E | 0.758117 | 0.438046 | 0.630952 | 0.111* | 0.451 (11) |
H51F | 0.602095 | 0.441338 | 0.607251 | 0.111* | 0.451 (11) |
O9 | 0.5561 (5) | 0.8637 (3) | 0.5708 (2) | 0.1391 (17) | |
C52 | 0.6254 (6) | 0.9318 (4) | 0.5800 (3) | 0.0980 (17) | |
H52A | 0.660297 | 0.965313 | 0.536688 | 0.118* | |
H52B | 0.710308 | 0.895984 | 0.609485 | 0.118* | |
C53 | 0.5171 (5) | 1.0069 (4) | 0.6105 (3) | 0.1009 (17) | |
H53A | 0.474171 | 1.069270 | 0.576463 | 0.121* | |
H53B | 0.562821 | 1.023080 | 0.645154 | 0.121* | |
C54 | 0.4016 (6) | 0.9565 (5) | 0.6409 (3) | 0.1106 (19) | |
H54A | 0.413951 | 0.929899 | 0.689577 | 0.133* | |
H54B | 0.302122 | 1.003604 | 0.631886 | 0.133* | |
C55 | 0.4285 (7) | 0.8763 (6) | 0.6076 (4) | 0.147 (3) | |
H55A | 0.432875 | 0.813131 | 0.641219 | 0.177* | |
H55B | 0.345940 | 0.890959 | 0.577801 | 0.177* | |
Atomic displacement parameters (Å2) top | U11 | U22 | U33 | U12 | U13 | U23 |
V1 | 0.0248 (3) | 0.0293 (3) | 0.0317 (3) | −0.0105 (2) | 0.0007 (2) | −0.0057 (2) |
P1 | 0.0265 (4) | 0.0348 (4) | 0.0378 (5) | −0.0104 (3) | −0.0002 (3) | −0.0064 (4) |
C1 | 0.0340 (17) | 0.0301 (16) | 0.0291 (17) | −0.0110 (13) | −0.0009 (13) | −0.0104 (13) |
C2 | 0.0302 (17) | 0.0317 (16) | 0.0309 (17) | −0.0092 (13) | 0.0038 (14) | −0.0030 (14) |
C3 | 0.0255 (16) | 0.0309 (16) | 0.0364 (18) | −0.0115 (13) | −0.0037 (14) | 0.0005 (14) |
C4 | 0.0314 (17) | 0.0330 (16) | 0.0337 (18) | −0.0105 (13) | −0.0058 (14) | −0.0088 (14) |
C5 | 0.043 (2) | 0.0354 (17) | 0.0341 (18) | −0.0083 (15) | 0.0053 (15) | −0.0081 (14) |
C6 | 0.039 (2) | 0.0375 (18) | 0.044 (2) | −0.0047 (15) | 0.0150 (16) | −0.0047 (16) |
C7 | 0.0276 (17) | 0.0375 (18) | 0.047 (2) | −0.0104 (14) | 0.0024 (15) | 0.0025 (16) |
C8 | 0.0300 (17) | 0.0322 (16) | 0.0372 (18) | −0.0166 (13) | −0.0009 (14) | 0.0011 (14) |
C9 | 0.0310 (16) | 0.0250 (14) | 0.0256 (15) | −0.0126 (12) | −0.0009 (12) | −0.0048 (12) |
C10 | 0.0387 (18) | 0.0314 (16) | 0.0265 (16) | −0.0118 (14) | −0.0036 (13) | −0.0095 (13) |
C11 | 0.0274 (16) | 0.0232 (14) | 0.0216 (15) | −0.0102 (12) | −0.0011 (12) | −0.0007 (12) |
C12 | 0.0308 (16) | 0.0249 (14) | 0.0230 (15) | −0.0117 (12) | −0.0020 (12) | −0.0012 (12) |
C13 | 0.0324 (17) | 0.0265 (15) | 0.0263 (16) | −0.0090 (13) | 0.0015 (13) | 0.0001 (13) |
C14 | 0.0299 (16) | 0.0236 (14) | 0.0277 (16) | −0.0122 (12) | 0.0001 (13) | 0.0027 (12) |
C15 | 0.0371 (18) | 0.0292 (16) | 0.0332 (18) | −0.0120 (14) | 0.0052 (14) | −0.0109 (14) |
C16 | 0.0259 (17) | 0.0312 (16) | 0.0408 (19) | −0.0089 (13) | 0.0060 (14) | −0.0043 (14) |
C17 | 0.0326 (18) | 0.0373 (17) | 0.0379 (19) | −0.0201 (14) | −0.0024 (14) | −0.0028 (15) |
C18 | 0.0388 (19) | 0.0388 (18) | 0.0371 (19) | −0.0185 (15) | 0.0047 (15) | −0.0154 (15) |
C19 | 0.053 (2) | 0.0305 (19) | 0.089 (3) | −0.0120 (17) | 0.009 (2) | −0.011 (2) |
C20 | 0.059 (3) | 0.032 (2) | 0.107 (4) | −0.0040 (19) | 0.000 (3) | 0.005 (2) |
C21 | 0.060 (3) | 0.046 (2) | 0.083 (3) | −0.016 (2) | −0.014 (2) | 0.019 (2) |
C22 | 0.049 (2) | 0.042 (2) | 0.056 (2) | −0.0154 (17) | −0.0044 (18) | 0.0077 (17) |
C23 | 0.0397 (18) | 0.0308 (16) | 0.0358 (18) | −0.0138 (14) | 0.0032 (14) | −0.0071 (14) |
C24 | 0.0418 (19) | 0.0335 (17) | 0.052 (2) | −0.0161 (15) | 0.0094 (16) | −0.0189 (16) |
C25 | 0.0271 (16) | 0.0320 (16) | 0.0379 (18) | −0.0144 (13) | 0.0060 (13) | −0.0086 (14) |
C26 | 0.0322 (17) | 0.0310 (16) | 0.0414 (19) | −0.0179 (14) | 0.0082 (14) | −0.0114 (14) |
C27 | 0.0363 (18) | 0.0285 (16) | 0.063 (2) | −0.0146 (14) | 0.0059 (17) | −0.0069 (16) |
C28 | 0.0361 (18) | 0.0310 (17) | 0.049 (2) | −0.0149 (14) | 0.0018 (15) | 0.0004 (15) |
C29 | 0.043 (2) | 0.060 (2) | 0.046 (2) | −0.0158 (17) | −0.0051 (16) | −0.0193 (18) |
C30 | 0.0313 (18) | 0.050 (2) | 0.048 (2) | −0.0134 (15) | 0.0051 (15) | −0.0160 (16) |
C31 | 0.0331 (19) | 0.047 (2) | 0.071 (3) | −0.0115 (16) | −0.0080 (18) | 0.0027 (18) |
K1 | 0.0286 (5) | 0.0259 (5) | 0.0395 (6) | −0.0099 (4) | 0.0013 (4) | −0.0033 (4) |
O1 | 0.0376 (12) | 0.0308 (11) | 0.0460 (13) | −0.0168 (9) | 0.0000 (10) | −0.0077 (10) |
O2 | 0.0310 (12) | 0.0277 (11) | 0.0453 (13) | −0.0062 (9) | −0.0045 (10) | −0.0019 (9) |
O3 | 0.0314 (12) | 0.0376 (12) | 0.0415 (13) | −0.0131 (9) | 0.0061 (10) | −0.0102 (10) |
C32 | 0.0411 (19) | 0.0377 (18) | 0.044 (2) | −0.0243 (15) | −0.0002 (15) | −0.0047 (15) |
C33 | 0.052 (2) | 0.0261 (16) | 0.0405 (19) | −0.0169 (15) | 0.0063 (16) | −0.0054 (14) |
C34 | 0.048 (2) | 0.0261 (16) | 0.042 (2) | −0.0054 (14) | −0.0009 (16) | −0.0015 (14) |
C35 | 0.0326 (18) | 0.0376 (18) | 0.057 (2) | −0.0006 (14) | −0.0075 (16) | −0.0166 (17) |
C36 | 0.0270 (17) | 0.051 (2) | 0.053 (2) | −0.0114 (15) | 0.0053 (15) | −0.0230 (17) |
C37 | 0.0359 (18) | 0.0461 (19) | 0.0423 (19) | −0.0251 (15) | 0.0045 (15) | −0.0044 (16) |
O4 | 0.079 (3) | 0.065 (3) | 0.045 (2) | −0.035 (2) | −0.0175 (19) | 0.0052 (17) |
C38 | 0.081 (4) | 0.071 (4) | 0.054 (3) | −0.044 (3) | 0.002 (3) | −0.014 (3) |
C39 | 0.070 (4) | 0.098 (5) | 0.114 (6) | −0.026 (3) | −0.023 (4) | −0.034 (4) |
C40 | 0.106 (5) | 0.073 (4) | 0.102 (5) | −0.034 (4) | −0.055 (4) | 0.009 (4) |
C41 | 0.062 (4) | 0.068 (4) | 0.051 (3) | −0.027 (4) | −0.004 (3) | −0.005 (3) |
O4' | 0.116 (13) | 0.091 (13) | 0.061 (8) | −0.069 (10) | −0.013 (9) | −0.009 (8) |
C38' | 0.079 (12) | 0.063 (12) | 0.078 (10) | −0.037 (9) | −0.006 (9) | −0.024 (9) |
C39' | 0.073 (13) | 0.088 (13) | 0.083 (10) | −0.035 (10) | −0.011 (9) | −0.034 (10) |
C40' | 0.085 (14) | 0.072 (13) | 0.060 (9) | −0.034 (11) | −0.024 (9) | 0.000 (9) |
C41' | 0.082 (16) | 0.071 (14) | 0.062 (11) | −0.042 (13) | −0.004 (10) | −0.016 (9) |
K2 | 0.0662 (7) | 0.0347 (5) | 0.0331 (6) | −0.0180 (5) | −0.0005 (5) | −0.0083 (4) |
O5 | 0.0704 (16) | 0.0351 (12) | 0.0366 (13) | −0.0167 (12) | −0.0055 (12) | −0.0058 (10) |
O6 | 0.0794 (18) | 0.0453 (14) | 0.0343 (13) | −0.0316 (13) | −0.0021 (12) | −0.0050 (11) |
O7 | 0.0862 (19) | 0.0438 (13) | 0.0366 (13) | −0.0357 (13) | −0.0073 (13) | −0.0055 (11) |
C42 | 0.062 (2) | 0.0361 (19) | 0.053 (2) | −0.0148 (17) | −0.0097 (19) | −0.0028 (17) |
C43 | 0.071 (3) | 0.0384 (19) | 0.043 (2) | −0.0214 (18) | −0.0118 (18) | 0.0050 (16) |
C44 | 0.093 (3) | 0.054 (2) | 0.033 (2) | −0.032 (2) | −0.0108 (19) | −0.0042 (17) |
C45 | 0.099 (3) | 0.055 (2) | 0.037 (2) | −0.036 (2) | −0.012 (2) | −0.0070 (18) |
C46 | 0.107 (3) | 0.051 (2) | 0.047 (2) | −0.047 (2) | −0.009 (2) | −0.0090 (19) |
C47 | 0.086 (3) | 0.041 (2) | 0.046 (2) | −0.030 (2) | 0.006 (2) | −0.0151 (17) |
O8 | 0.069 (6) | 0.099 (10) | 0.053 (6) | 0.009 (5) | 0.025 (5) | −0.002 (6) |
C48 | 0.066 (7) | 0.063 (9) | 0.069 (8) | −0.020 (6) | 0.011 (6) | −0.006 (6) |
C49 | 0.055 (6) | 0.070 (9) | 0.089 (9) | −0.012 (6) | 0.019 (5) | −0.015 (6) |
C50 | 0.065 (7) | 0.134 (12) | 0.070 (8) | −0.031 (8) | 0.015 (6) | 0.012 (8) |
C51 | 0.068 (6) | 0.110 (11) | 0.054 (6) | −0.027 (7) | 0.004 (5) | −0.012 (7) |
O8' | 0.075 (8) | 0.098 (10) | 0.071 (9) | −0.006 (8) | −0.009 (7) | −0.027 (8) |
C48' | 0.068 (10) | 0.078 (12) | 0.068 (9) | −0.012 (9) | −0.011 (7) | −0.020 (9) |
C49' | 0.071 (9) | 0.088 (12) | 0.089 (10) | −0.008 (9) | −0.002 (8) | −0.012 (10) |
C50' | 0.072 (10) | 0.119 (13) | 0.079 (10) | −0.012 (11) | 0.015 (9) | −0.016 (10) |
C51' | 0.076 (11) | 0.117 (14) | 0.067 (10) | −0.038 (12) | 0.005 (9) | −0.038 (10) |
O8" | 0.089 (7) | 0.086 (8) | 0.072 (6) | 0.019 (6) | 0.006 (5) | −0.023 (5) |
C48" | 0.076 (7) | 0.080 (10) | 0.078 (6) | −0.014 (7) | −0.002 (6) | −0.005 (6) |
C49" | 0.086 (8) | 0.075 (7) | 0.114 (8) | −0.008 (6) | 0.021 (7) | −0.014 (6) |
C50" | 0.086 (9) | 0.135 (9) | 0.070 (6) | −0.033 (8) | −0.003 (6) | −0.033 (6) |
C51" | 0.072 (8) | 0.089 (8) | 0.093 (8) | −0.014 (6) | 0.006 (7) | 0.004 (6) |
O9 | 0.111 (3) | 0.139 (4) | 0.200 (5) | −0.078 (3) | 0.062 (3) | −0.069 (3) |
C52 | 0.083 (4) | 0.108 (4) | 0.108 (4) | −0.047 (3) | −0.003 (3) | −0.011 (3) |
C53 | 0.068 (3) | 0.089 (4) | 0.131 (5) | −0.020 (3) | 0.008 (3) | −0.009 (3) |
C54 | 0.090 (4) | 0.108 (4) | 0.144 (5) | −0.050 (4) | 0.011 (4) | −0.027 (4) |
C55 | 0.135 (6) | 0.168 (7) | 0.174 (7) | −0.100 (5) | 0.091 (5) | −0.066 (6) |
Geometric parameters (Å, º) top
V1—C16 | 2.208 (3) | C38—H38B | 0.9900 |
V1—C17 | 2.222 (3) | C39—C40 | 1.488 (8) |
V1—C3 | 2.243 (3) | C39—H39A | 0.9900 |
V1—C2 | 2.245 (3) | C39—H39B | 0.9900 |
V1—C1 | 2.279 (3) | C40—C41 | 1.501 (8) |
V1—C15 | 2.304 (3) | C40—H40A | 0.9900 |
V1—C4 | 2.307 (3) | C40—H40B | 0.9900 |
V1—C18 | 2.340 (3) | C41—H41A | 0.9900 |
V1—P1 | 2.5031 (10) | C41—H41B | 0.9900 |
P1—C31 | 1.826 (3) | O4'—C41' | 1.406 (15) |
P1—C29 | 1.827 (3) | O4'—C38' | 1.419 (15) |
P1—C30 | 1.829 (3) | C38'—C39' | 1.504 (16) |
C1—C2 | 1.427 (4) | C38'—H38C | 0.9900 |
C1—C11 | 1.451 (4) | C38'—H38D | 0.9900 |
C1—H1 | 0.92 (3) | C39'—C40' | 1.466 (17) |
C2—C3 | 1.386 (4) | C39'—H39C | 0.9900 |
C2—H2 | 0.95 (3) | C39'—H39D | 0.9900 |
C3—C4 | 1.418 (4) | C40'—C41' | 1.495 (16) |
C3—H3 | 0.95 (3) | C40'—H40C | 0.9900 |
C4—C12 | 1.444 (4) | C40'—H40D | 0.9900 |
C4—H4 | 0.93 (3) | C41'—H41C | 0.9900 |
C5—C6 | 1.379 (5) | C41'—H41D | 0.9900 |
C5—C13 | 1.407 (4) | K2—O8ii | 2.706 (9) |
C5—H5 | 0.9500 | K2—O8 | 2.706 (9) |
C6—C7 | 1.397 (5) | K2—O8'ii | 2.716 (15) |
C6—H6 | 0.9500 | K2—O8' | 2.716 (15) |
C7—C8 | 1.374 (4) | K2—O5ii | 2.759 (2) |
C7—H7 | 0.9500 | K2—O5 | 2.759 (2) |
C8—C14 | 1.404 (4) | K2—O7 | 2.781 (2) |
C8—H8 | 0.9500 | K2—O7ii | 2.781 (2) |
C9—C11 | 1.375 (4) | K2—O8" | 2.789 (11) |
C9—C14 | 1.425 (4) | K2—O8"ii | 2.789 (11) |
C9—H9 | 0.9500 | K2—O6 | 2.839 (2) |
C10—C12 | 1.374 (4) | K2—O6ii | 2.839 (2) |
C10—C13 | 1.417 (4) | K2—H48Dii | 2.86 (3) |
C10—H10 | 0.9500 | O5—C42 | 1.417 (4) |
C11—C12 | 1.452 (4) | O5—C47ii | 1.421 (4) |
C13—C14 | 1.438 (4) | O6—C43 | 1.425 (4) |
C15—C16 | 1.425 (4) | O6—C44 | 1.426 (4) |
C15—C25 | 1.455 (4) | O7—C45 | 1.418 (4) |
C15—H15 | 0.91 (3) | O7—C46 | 1.421 (4) |
C16—C17 | 1.379 (4) | C42—C43 | 1.491 (5) |
C16—H16 | 0.96 (3) | C42—H42A | 0.9900 |
C17—C18 | 1.430 (4) | C42—H42B | 0.9900 |
C17—H17 | 0.95 (3) | C43—H43A | 0.9900 |
C18—C26 | 1.458 (4) | C43—H43B | 0.9900 |
C18—H18 | 0.93 (3) | C44—C45 | 1.501 (5) |
C19—C20 | 1.375 (6) | C44—H44A | 0.9900 |
C19—C27 | 1.417 (4) | C44—H44B | 0.9900 |
C19—H19 | 0.9500 | C45—H45A | 0.9900 |
C20—C21 | 1.387 (6) | C45—H45B | 0.9900 |
C20—H20 | 0.9500 | C46—C47 | 1.489 (5) |
C21—C22 | 1.374 (5) | C46—H46A | 0.9900 |
C21—H21 | 0.9500 | C46—H46B | 0.9900 |
C22—C28 | 1.415 (5) | C47—H47A | 0.9900 |
C22—H22 | 0.9500 | C47—H47B | 0.9900 |
C23—C25 | 1.379 (4) | O8—C48 | 1.393 (12) |
C23—C28 | 1.420 (4) | O8—C51 | 1.412 (12) |
C23—H23 | 0.9500 | C48—C49 | 1.490 (15) |
C24—C26 | 1.376 (4) | C48—H48A | 0.9900 |
C24—C27 | 1.417 (5) | C48—H48B | 0.9900 |
C24—H24 | 0.9500 | C49—C50 | 1.494 (13) |
C25—C26 | 1.450 (4) | C49—H49A | 0.9900 |
C27—C28 | 1.423 (5) | C49—H49B | 0.9900 |
C29—H29A | 0.9800 | C50—C51 | 1.491 (13) |
C29—H29B | 0.9800 | C50—H50A | 0.9900 |
C29—H29C | 0.9800 | C50—H50B | 0.9900 |
C30—H30A | 0.9800 | C51—H51A | 0.9900 |
C30—H30B | 0.9800 | C51—H51B | 0.9900 |
C30—H30C | 0.9800 | O8'—C48' | 1.379 (15) |
C31—H31A | 0.9800 | O8'—C51' | 1.385 (15) |
C31—H31B | 0.9800 | C48'—C49' | 1.493 (17) |
C31—H31C | 0.9800 | C48'—H48C | 0.9900 |
K1—O4' | 2.699 (13) | C48'—H48D | 0.9900 |
K1—O4'i | 2.699 (13) | C49'—C50' | 1.496 (18) |
K1—O4i | 2.714 (4) | C49'—H49C | 0.9900 |
K1—O4 | 2.714 (4) | C49'—H49D | 0.9900 |
K1—O2i | 2.7549 (19) | C50'—C51' | 1.482 (17) |
K1—O2 | 2.7549 (19) | C50'—H50C | 0.9900 |
K1—O1 | 2.7793 (19) | C50'—H50D | 0.9900 |
K1—O1i | 2.7793 (19) | C51'—H51C | 0.9900 |
K1—O3i | 2.870 (2) | C51'—H51D | 0.9900 |
K1—O3 | 2.870 (2) | O8"—C48" | 1.399 (12) |
O1—C33 | 1.419 (3) | O8"—C51" | 1.425 (11) |
O1—C32 | 1.422 (4) | C48"—C49" | 1.488 (14) |
O2—C35 | 1.423 (4) | C48"—H48E | 0.9900 |
O2—C34 | 1.427 (3) | C48"—H48F | 0.9900 |
O3—C36 | 1.422 (3) | C49"—C50" | 1.468 (14) |
O3—C37 | 1.429 (3) | C49"—H49E | 0.9900 |
C32—C37i | 1.489 (4) | C49"—H49F | 0.9900 |
C32—H32A | 0.9900 | C50"—C51" | 1.523 (13) |
C32—H32B | 0.9900 | C50"—H50E | 0.9900 |
C33—C34 | 1.495 (4) | C50"—H50F | 0.9900 |
C33—H33A | 0.9900 | C51"—H51E | 0.9900 |
C33—H33B | 0.9900 | C51"—H51F | 0.9900 |
C34—H34A | 0.9900 | O9—C55 | 1.375 (6) |
C34—H34B | 0.9900 | O9—C52 | 1.410 (6) |
C35—C36 | 1.488 (4) | C52—C53 | 1.484 (7) |
C35—H35A | 0.9900 | C52—H52A | 0.9900 |
C35—H35B | 0.9900 | C52—H52B | 0.9900 |
C36—H36A | 0.9900 | C53—C54 | 1.519 (7) |
C36—H36B | 0.9900 | C53—H53A | 0.9900 |
C37—H37A | 0.9900 | C53—H53B | 0.9900 |
C37—H37B | 0.9900 | C54—C55 | 1.446 (8) |
O4—C41 | 1.406 (6) | C54—H54A | 0.9900 |
O4—C38 | 1.419 (6) | C54—H54B | 0.9900 |
C38—C39 | 1.516 (7) | C55—H55A | 0.9900 |
C38—H38A | 0.9900 | C55—H55B | 0.9900 |
| | | |
C16—V1—C17 | 36.29 (11) | C40—C39—C38 | 104.3 (5) |
C16—V1—C3 | 135.95 (11) | C40—C39—H39A | 110.9 |
C17—V1—C3 | 144.25 (12) | C38—C39—H39A | 110.9 |
C16—V1—C2 | 133.31 (11) | C40—C39—H39B | 110.9 |
C17—V1—C2 | 115.31 (12) | C38—C39—H39B | 110.9 |
C3—V1—C2 | 35.96 (11) | H39A—C39—H39B | 108.9 |
C16—V1—C1 | 97.33 (11) | C39—C40—C41 | 105.3 (5) |
C17—V1—C1 | 81.39 (11) | C39—C40—H40A | 110.7 |
C3—V1—C1 | 64.02 (11) | C41—C40—H40A | 110.7 |
C2—V1—C1 | 36.76 (10) | C39—C40—H40B | 110.7 |
C16—V1—C15 | 36.75 (11) | C41—C40—H40B | 110.7 |
C17—V1—C15 | 63.72 (12) | H40A—C40—H40B | 108.8 |
C3—V1—C15 | 136.26 (11) | O4—C41—C40 | 106.9 (5) |
C2—V1—C15 | 164.48 (11) | O4—C41—H41A | 110.3 |
C1—V1—C15 | 133.43 (11) | C40—C41—H41A | 110.3 |
C16—V1—C4 | 101.61 (11) | O4—C41—H41B | 110.3 |
C17—V1—C4 | 126.44 (11) | C40—C41—H41B | 110.3 |
C3—V1—C4 | 36.28 (10) | H41A—C41—H41B | 108.6 |
C2—V1—C4 | 64.00 (11) | C41'—O4'—C38' | 111.7 (14) |
C1—V1—C4 | 72.57 (11) | C41'—O4'—K1 | 127.3 (15) |
C15—V1—C4 | 103.37 (11) | C38'—O4'—K1 | 119.2 (13) |
C16—V1—C18 | 63.78 (11) | O4'—C38'—C39' | 104.8 (13) |
C17—V1—C18 | 36.42 (11) | O4'—C38'—H38C | 110.8 |
C3—V1—C18 | 152.93 (12) | C39'—C38'—H38C | 110.8 |
C2—V1—C18 | 118.46 (12) | O4'—C38'—H38D | 110.8 |
C1—V1—C18 | 99.36 (11) | C39'—C38'—H38D | 110.8 |
C15—V1—C18 | 70.78 (11) | H38C—C38'—H38D | 108.9 |
C4—V1—C18 | 162.86 (11) | C40'—C39'—C38' | 107.7 (12) |
C16—V1—P1 | 131.35 (9) | C40'—C39'—H39C | 110.2 |
C17—V1—P1 | 134.53 (9) | C38'—C39'—H39C | 110.2 |
C3—V1—P1 | 79.15 (8) | C40'—C39'—H39D | 110.2 |
C2—V1—P1 | 95.19 (8) | C38'—C39'—H39D | 110.2 |
C1—V1—P1 | 131.23 (8) | H39C—C39'—H39D | 108.5 |
C15—V1—P1 | 95.24 (8) | C39'—C40'—C41' | 105.8 (12) |
C4—V1—P1 | 96.49 (8) | C39'—C40'—H40C | 110.6 |
C18—V1—P1 | 100.06 (8) | C41'—C40'—H40C | 110.6 |
C31—P1—C29 | 100.86 (17) | C39'—C40'—H40D | 110.6 |
C31—P1—C30 | 98.78 (16) | C41'—C40'—H40D | 110.6 |
C29—P1—C30 | 100.73 (16) | H40C—C40'—H40D | 108.7 |
C31—P1—V1 | 122.03 (11) | O4'—C41'—C40' | 107.5 (14) |
C29—P1—V1 | 114.17 (11) | O4'—C41'—H41C | 110.2 |
C30—P1—V1 | 116.86 (11) | C40'—C41'—H41C | 110.2 |
C2—C1—C11 | 120.2 (3) | O4'—C41'—H41D | 110.2 |
C2—C1—V1 | 70.33 (17) | C40'—C41'—H41D | 110.2 |
C11—C1—V1 | 97.80 (18) | H41C—C41'—H41D | 108.5 |
C2—C1—H1 | 117.8 (19) | O8ii—K2—O8 | 180.0 |
C11—C1—H1 | 117.3 (19) | O8ii—K2—O8'ii | 15.5 (6) |
V1—C1—H1 | 122.5 (18) | O8—K2—O8'ii | 164.5 (6) |
C3—C2—C1 | 116.9 (3) | O8'ii—K2—O8' | 180.0 |
C3—C2—V1 | 71.96 (17) | O8ii—K2—O5ii | 95.5 (4) |
C1—C2—V1 | 72.92 (17) | O8—K2—O5ii | 84.5 (4) |
C3—C2—H2 | 121.9 (19) | O8ii—K2—O5 | 84.5 (4) |
C1—C2—H2 | 121.0 (19) | O8—K2—O5 | 95.5 (4) |
V1—C2—H2 | 120.8 (18) | O8'ii—K2—O5 | 95.4 (6) |
C2—C3—C4 | 118.7 (3) | O8'—K2—O5 | 84.6 (6) |
C2—C3—V1 | 72.08 (17) | O5ii—K2—O5 | 180.00 (10) |
C4—C3—V1 | 74.30 (17) | O8ii—K2—O7 | 99.5 (4) |
C2—C3—H3 | 120.8 (18) | O8—K2—O7 | 80.5 (4) |
C4—C3—H3 | 120.4 (18) | O8'ii—K2—O7 | 103.6 (6) |
V1—C3—H3 | 125.7 (18) | O8'—K2—O7 | 76.4 (6) |
C3—C4—C12 | 120.6 (3) | O5ii—K2—O7 | 61.08 (6) |
C3—C4—V1 | 69.42 (17) | O5—K2—O7 | 118.92 (6) |
C12—C4—V1 | 97.10 (18) | O8ii—K2—O7ii | 80.5 (4) |
C3—C4—H4 | 118.5 (19) | O8—K2—O7ii | 99.5 (4) |
C12—C4—H4 | 116.9 (19) | O5ii—K2—O7ii | 118.92 (6) |
V1—C4—H4 | 122.8 (18) | O5—K2—O7ii | 61.08 (6) |
C6—C5—C13 | 121.9 (3) | O7—K2—O7ii | 180.0 |
C6—C5—H5 | 119.1 | O5ii—K2—O8" | 94.6 (3) |
C13—C5—H5 | 119.1 | O5—K2—O8" | 85.4 (3) |
C5—C6—C7 | 119.7 (3) | O7—K2—O8" | 92.0 (3) |
C5—C6—H6 | 120.2 | O7ii—K2—O8" | 88.0 (3) |
C7—C6—H6 | 120.2 | O8ii—K2—O8"ii | 12.6 (6) |
C8—C7—C6 | 120.0 (3) | O8—K2—O8"ii | 167.4 (6) |
C8—C7—H7 | 120.0 | O8'ii—K2—O8"ii | 18.5 (6) |
C6—C7—H7 | 120.0 | O8'—K2—O8"ii | 161.5 (6) |
C7—C8—C14 | 122.0 (3) | O5ii—K2—O8"ii | 85.4 (3) |
C7—C8—H8 | 119.0 | O5—K2—O8"ii | 94.6 (3) |
C14—C8—H8 | 119.0 | O7—K2—O8"ii | 88.0 (3) |
C11—C9—C14 | 122.5 (3) | O7ii—K2—O8"ii | 92.0 (3) |
C11—C9—H9 | 118.8 | O8"—K2—O8"ii | 180.0 |
C14—C9—H9 | 118.8 | O8ii—K2—O6 | 82.4 (3) |
C12—C10—C13 | 122.7 (3) | O8—K2—O6 | 97.6 (3) |
C12—C10—H10 | 118.7 | O8'ii—K2—O6 | 97.4 (5) |
C13—C10—H10 | 118.7 | O8'—K2—O6 | 82.6 (5) |
C9—C11—C1 | 124.8 (3) | O5ii—K2—O6 | 120.17 (6) |
C9—C11—C12 | 119.0 (2) | O5—K2—O6 | 59.83 (6) |
C1—C11—C12 | 116.1 (2) | O7—K2—O6 | 60.45 (7) |
C10—C12—C4 | 125.2 (3) | O7ii—K2—O6 | 119.55 (7) |
C10—C12—C11 | 119.2 (3) | O8"—K2—O6 | 98.9 (3) |
C4—C12—C11 | 115.6 (2) | O8"ii—K2—O6 | 81.1 (3) |
C5—C13—C10 | 123.3 (3) | O8ii—K2—O6ii | 97.6 (3) |
C5—C13—C14 | 118.2 (3) | O8—K2—O6ii | 82.4 (3) |
C10—C13—C14 | 118.4 (3) | O5ii—K2—O6ii | 59.83 (6) |
C8—C14—C9 | 123.5 (3) | O5—K2—O6ii | 120.17 (6) |
C8—C14—C13 | 118.2 (3) | O7—K2—O6ii | 119.55 (7) |
C9—C14—C13 | 118.3 (3) | O7ii—K2—O6ii | 60.45 (7) |
C16—C15—C25 | 118.5 (3) | O6—K2—O6ii | 180.0 |
C16—C15—V1 | 67.93 (17) | O8ii—K2—H48Dii | 27.5 (7) |
C25—C15—V1 | 105.21 (19) | O8—K2—H48Dii | 152.5 (7) |
C16—C15—H15 | 115.7 (19) | O5ii—K2—H48Dii | 99.4 (12) |
C25—C15—H15 | 118.1 (19) | O5—K2—H48Dii | 80.6 (12) |
V1—C15—H15 | 121.4 (19) | O7—K2—H48Dii | 77.8 (6) |
C17—C16—C15 | 116.9 (3) | O7ii—K2—H48Dii | 102.2 (6) |
C17—C16—V1 | 72.41 (17) | O6—K2—H48Dii | 56.8 (9) |
C15—C16—V1 | 75.32 (17) | O6ii—K2—H48Dii | 123.2 (9) |
C17—C16—H16 | 122.0 (18) | C42—O5—C47ii | 112.9 (3) |
C15—C16—H16 | 120.9 (18) | C42—O5—K2 | 118.92 (18) |
V1—C16—H16 | 117.3 (18) | C47ii—O5—K2 | 114.31 (18) |
C16—C17—C18 | 117.8 (3) | C43—O6—C44 | 112.4 (2) |
C16—C17—V1 | 71.30 (17) | C43—O6—K2 | 111.23 (19) |
C18—C17—V1 | 76.30 (18) | C44—O6—K2 | 114.09 (19) |
C16—C17—H17 | 120.6 (19) | C45—O7—C46 | 112.1 (3) |
C18—C17—H17 | 121.5 (18) | C45—O7—K2 | 113.33 (19) |
V1—C17—H17 | 119.2 (19) | C46—O7—K2 | 114.01 (19) |
C17—C18—C26 | 118.2 (3) | O5—C42—C43 | 108.3 (3) |
C17—C18—V1 | 67.27 (17) | O5—C42—H42A | 110.0 |
C26—C18—V1 | 104.1 (2) | C43—C42—H42A | 110.0 |
C17—C18—H18 | 118 (2) | O5—C42—H42B | 110.0 |
C26—C18—H18 | 115.9 (19) | C43—C42—H42B | 110.0 |
V1—C18—H18 | 123.8 (19) | H42A—C42—H42B | 108.4 |
C20—C19—C27 | 121.3 (4) | O6—C43—C42 | 108.8 (3) |
C20—C19—H19 | 119.4 | O6—C43—H43A | 109.9 |
C27—C19—H19 | 119.4 | C42—C43—H43A | 109.9 |
C19—C20—C21 | 120.2 (4) | O6—C43—H43B | 109.9 |
C19—C20—H20 | 119.9 | C42—C43—H43B | 109.9 |
C21—C20—H20 | 119.9 | H43A—C43—H43B | 108.3 |
C22—C21—C20 | 120.6 (4) | O6—C44—C45 | 108.0 (3) |
C22—C21—H21 | 119.7 | O6—C44—H44A | 110.1 |
C20—C21—H21 | 119.7 | C45—C44—H44A | 110.1 |
C21—C22—C28 | 120.9 (4) | O6—C44—H44B | 110.1 |
C21—C22—H22 | 119.5 | C45—C44—H44B | 110.1 |
C28—C22—H22 | 119.5 | H44A—C44—H44B | 108.4 |
C25—C23—C28 | 122.3 (3) | O7—C45—C44 | 108.6 (3) |
C25—C23—H23 | 118.9 | O7—C45—H45A | 110.0 |
C28—C23—H23 | 118.9 | C44—C45—H45A | 110.0 |
C26—C24—C27 | 122.2 (3) | O7—C45—H45B | 110.0 |
C26—C24—H24 | 118.9 | C44—C45—H45B | 110.0 |
C27—C24—H24 | 118.9 | H45A—C45—H45B | 108.3 |
C23—C25—C26 | 118.9 (3) | O7—C46—C47 | 109.7 (3) |
C23—C25—C15 | 125.8 (3) | O7—C46—H46A | 109.7 |
C26—C25—C15 | 115.3 (3) | C47—C46—H46A | 109.7 |
C24—C26—C25 | 119.1 (3) | O7—C46—H46B | 109.7 |
C24—C26—C18 | 125.7 (3) | C47—C46—H46B | 109.7 |
C25—C26—C18 | 115.1 (3) | H46A—C46—H46B | 108.2 |
C24—C27—C19 | 122.7 (3) | O5ii—C47—C46 | 108.2 (3) |
C24—C27—C28 | 119.0 (3) | O5ii—C47—H47A | 110.1 |
C19—C27—C28 | 118.3 (3) | C46—C47—H47A | 110.1 |
C22—C28—C23 | 122.8 (3) | O5ii—C47—H47B | 110.1 |
C22—C28—C27 | 118.8 (3) | C46—C47—H47B | 110.1 |
C23—C28—C27 | 118.4 (3) | H47A—C47—H47B | 108.4 |
P1—C29—H29A | 109.5 | C48—O8—C51 | 110.1 (10) |
P1—C29—H29B | 109.5 | C48—O8—K2 | 129.4 (10) |
H29A—C29—H29B | 109.5 | C51—O8—K2 | 116.0 (9) |
P1—C29—H29C | 109.5 | O8—C48—C49 | 104.7 (10) |
H29A—C29—H29C | 109.5 | O8—C48—H48A | 110.8 |
H29B—C29—H29C | 109.5 | C49—C48—H48A | 110.8 |
P1—C30—H30A | 109.5 | O8—C48—H48B | 110.8 |
P1—C30—H30B | 109.5 | C49—C48—H48B | 110.8 |
H30A—C30—H30B | 109.5 | H48A—C48—H48B | 108.9 |
P1—C30—H30C | 109.5 | C48—C49—C50 | 104.7 (9) |
H30A—C30—H30C | 109.5 | C48—C49—H49A | 110.8 |
H30B—C30—H30C | 109.5 | C50—C49—H49A | 110.8 |
P1—C31—H31A | 109.5 | C48—C49—H49B | 110.8 |
P1—C31—H31B | 109.5 | C50—C49—H49B | 110.8 |
H31A—C31—H31B | 109.5 | H49A—C49—H49B | 108.9 |
P1—C31—H31C | 109.5 | C51—C50—C49 | 106.5 (9) |
H31A—C31—H31C | 109.5 | C51—C50—H50A | 110.4 |
H31B—C31—H31C | 109.5 | C49—C50—H50A | 110.4 |
O4i—K1—O4 | 180.0 | C51—C50—H50B | 110.4 |
O4i—K1—O2i | 83.97 (11) | C49—C50—H50B | 110.4 |
O4—K1—O2i | 96.03 (11) | H50A—C50—H50B | 108.6 |
O4'—K1—O2 | 101.7 (6) | O8—C51—C50 | 102.1 (10) |
O4'i—K1—O2 | 78.3 (6) | O8—C51—H51A | 111.3 |
O4i—K1—O2 | 96.03 (11) | C50—C51—H51A | 111.3 |
O4—K1—O2 | 83.97 (11) | O8—C51—H51B | 111.3 |
O2i—K1—O2 | 180.00 (6) | C50—C51—H51B | 111.3 |
O4'—K1—O1 | 103.6 (4) | H51A—C51—H51B | 109.2 |
O4'i—K1—O1 | 76.4 (4) | C48'—O8'—C51' | 113.1 (18) |
O4i—K1—O1 | 80.16 (10) | C48'—O8'—K2 | 97.4 (18) |
O4—K1—O1 | 99.84 (10) | C51'—O8'—K2 | 132 (2) |
O2i—K1—O1 | 119.02 (6) | O8'—C48'—C49' | 106.2 (14) |
O2—K1—O1 | 60.98 (6) | O8'—C48'—H48C | 110.5 |
O4i—K1—O1i | 99.85 (10) | C49'—C48'—H48C | 110.5 |
O4—K1—O1i | 80.16 (10) | O8'—C48'—H48D | 110.5 |
O2i—K1—O1i | 60.98 (6) | C49'—C48'—H48D | 110.5 |
O2—K1—O1i | 119.02 (6) | H48C—C48'—H48D | 108.7 |
O1—K1—O1i | 180.00 (7) | C48'—C49'—C50' | 106.5 (13) |
O4i—K1—O3i | 84.95 (10) | C48'—C49'—H49C | 110.4 |
O4—K1—O3i | 95.05 (10) | C50'—C49'—H49C | 110.4 |
O2i—K1—O3i | 60.79 (6) | C48'—C49'—H49D | 110.4 |
O2—K1—O3i | 119.21 (6) | C50'—C49'—H49D | 110.4 |
O1—K1—O3i | 59.42 (6) | H49C—C49'—H49D | 108.6 |
O1i—K1—O3i | 120.58 (6) | C51'—C50'—C49' | 104.6 (13) |
O4'—K1—O3 | 98.4 (5) | C51'—C50'—H50C | 110.8 |
O4'i—K1—O3 | 81.6 (5) | C49'—C50'—H50C | 110.8 |
O4i—K1—O3 | 95.05 (10) | C51'—C50'—H50D | 110.8 |
O4—K1—O3 | 84.95 (10) | C49'—C50'—H50D | 110.8 |
O2i—K1—O3 | 119.21 (6) | H50C—C50'—H50D | 108.9 |
O2—K1—O3 | 60.79 (6) | O8'—C51'—C50' | 107.0 (15) |
O1—K1—O3 | 120.58 (6) | O8'—C51'—H51C | 110.3 |
O1i—K1—O3 | 59.42 (6) | C50'—C51'—H51C | 110.3 |
O3i—K1—O3 | 180.0 | O8'—C51'—H51D | 110.3 |
C33—O1—C32 | 112.7 (2) | C50'—C51'—H51D | 110.3 |
C33—O1—K1 | 114.19 (16) | H51C—C51'—H51D | 108.6 |
C32—O1—K1 | 117.82 (16) | C48"—O8"—C51" | 105.3 (10) |
C35—O2—C34 | 113.6 (2) | C48"—O8"—K2 | 122.4 (12) |
C35—O2—K1 | 116.18 (16) | C51"—O8"—K2 | 120.9 (10) |
C34—O2—K1 | 114.74 (17) | O8"—C48"—C49" | 107.3 (11) |
C36—O3—C37 | 112.4 (2) | O8"—C48"—H48E | 110.3 |
C36—O3—K1 | 109.56 (16) | C49"—C48"—H48E | 110.3 |
C37—O3—K1 | 112.59 (16) | O8"—C48"—H48F | 110.3 |
O1—C32—C37i | 108.1 (2) | C49"—C48"—H48F | 110.3 |
O1—C32—H32A | 110.1 | H48E—C48"—H48F | 108.5 |
C37i—C32—H32A | 110.1 | C50"—C49"—C48" | 107.4 (9) |
O1—C32—H32B | 110.1 | C50"—C49"—H49E | 110.2 |
C37i—C32—H32B | 110.1 | C48"—C49"—H49E | 110.2 |
H32A—C32—H32B | 108.4 | C50"—C49"—H49F | 110.2 |
O1—C33—C34 | 108.9 (2) | C48"—C49"—H49F | 110.2 |
O1—C33—H33A | 109.9 | H49E—C49"—H49F | 108.5 |
C34—C33—H33A | 109.9 | C49"—C50"—C51" | 101.5 (9) |
O1—C33—H33B | 109.9 | C49"—C50"—H50E | 111.5 |
C34—C33—H33B | 109.9 | C51"—C50"—H50E | 111.5 |
H33A—C33—H33B | 108.3 | C49"—C50"—H50F | 111.5 |
O2—C34—C33 | 108.1 (2) | C51"—C50"—H50F | 111.5 |
O2—C34—H34A | 110.1 | H50E—C50"—H50F | 109.3 |
C33—C34—H34A | 110.1 | O8"—C51"—C50" | 105.7 (10) |
O2—C34—H34B | 110.1 | O8"—C51"—H51E | 110.6 |
C33—C34—H34B | 110.1 | C50"—C51"—H51E | 110.6 |
H34A—C34—H34B | 108.4 | O8"—C51"—H51F | 110.6 |
O2—C35—C36 | 108.7 (3) | C50"—C51"—H51F | 110.6 |
O2—C35—H35A | 110.0 | H51E—C51"—H51F | 108.7 |
C36—C35—H35A | 110.0 | C55—O9—C52 | 108.2 (5) |
O2—C35—H35B | 110.0 | O9—C52—C53 | 107.8 (4) |
C36—C35—H35B | 110.0 | O9—C52—H52A | 110.1 |
H35A—C35—H35B | 108.3 | C53—C52—H52A | 110.1 |
O3—C36—C35 | 109.0 (3) | O9—C52—H52B | 110.1 |
O3—C36—H36A | 109.9 | C53—C52—H52B | 110.1 |
C35—C36—H36A | 109.9 | H52A—C52—H52B | 108.5 |
O3—C36—H36B | 109.9 | C52—C53—C54 | 104.4 (5) |
C35—C36—H36B | 109.9 | C52—C53—H53A | 110.9 |
H36A—C36—H36B | 108.3 | C54—C53—H53A | 110.9 |
O3—C37—C32i | 108.6 (2) | C52—C53—H53B | 110.9 |
O3—C37—H37A | 110.0 | C54—C53—H53B | 110.9 |
C32i—C37—H37A | 110.0 | H53A—C53—H53B | 108.9 |
O3—C37—H37B | 110.0 | C55—C54—C53 | 103.0 (5) |
C32i—C37—H37B | 110.0 | C55—C54—H54A | 111.2 |
H37A—C37—H37B | 108.3 | C53—C54—H54A | 111.2 |
C41—O4—C38 | 107.0 (4) | C55—C54—H54B | 111.2 |
C41—O4—K1 | 130.6 (4) | C53—C54—H54B | 111.2 |
C38—O4—K1 | 113.4 (3) | H54A—C54—H54B | 109.1 |
O4—C38—C39 | 104.4 (4) | O9—C55—C54 | 112.7 (5) |
O4—C38—H38A | 110.9 | O9—C55—H55A | 109.1 |
C39—C38—H38A | 110.9 | C54—C55—H55A | 109.1 |
O4—C38—H38B | 110.9 | O9—C55—H55B | 109.1 |
C39—C38—H38B | 110.9 | C54—C55—H55B | 109.1 |
H38A—C38—H38B | 108.9 | H55A—C55—H55B | 107.8 |
| | | |
C11—C1—C2—C3 | −28.9 (4) | C25—C23—C28—C22 | −176.1 (3) |
V1—C1—C2—C3 | 58.7 (2) | C25—C23—C28—C27 | 3.1 (4) |
C11—C1—C2—V1 | −87.6 (3) | C24—C27—C28—C22 | 180.0 (3) |
C1—C2—C3—C4 | 0.7 (4) | C19—C27—C28—C22 | 0.7 (4) |
V1—C2—C3—C4 | 59.9 (2) | C24—C27—C28—C23 | 0.7 (4) |
C1—C2—C3—V1 | −59.2 (2) | C19—C27—C28—C23 | −178.5 (3) |
C2—C3—C4—C12 | 27.3 (4) | C33—O1—C32—C37i | 176.5 (2) |
V1—C3—C4—C12 | 86.1 (3) | K1—O1—C32—C37i | −47.2 (3) |
C2—C3—C4—V1 | −58.8 (2) | C32—O1—C33—C34 | −173.6 (2) |
C13—C5—C6—C7 | −0.6 (5) | K1—O1—C33—C34 | 48.4 (3) |
C5—C6—C7—C8 | 0.8 (4) | C35—O2—C34—C33 | −173.2 (2) |
C6—C7—C8—C14 | −0.8 (4) | K1—O2—C34—C33 | 49.9 (3) |
C14—C9—C11—C1 | −176.6 (2) | O1—C33—C34—O2 | −65.5 (3) |
C14—C9—C11—C12 | −0.9 (4) | C34—O2—C35—C36 | 177.3 (3) |
C2—C1—C11—C9 | −155.3 (3) | K1—O2—C35—C36 | −46.4 (3) |
V1—C1—C11—C9 | 133.0 (2) | C37—O3—C36—C35 | 179.7 (3) |
C2—C1—C11—C12 | 28.9 (4) | K1—O3—C36—C35 | −54.3 (3) |
V1—C1—C11—C12 | −42.8 (2) | O2—C35—C36—O3 | 68.9 (3) |
C13—C10—C12—C4 | 177.2 (3) | C36—O3—C37—C32i | 176.1 (3) |
C13—C10—C12—C11 | −0.3 (4) | K1—O3—C37—C32i | 51.8 (3) |
C3—C4—C12—C10 | 156.1 (3) | C41—O4—C38—C39 | −36.0 (7) |
V1—C4—C12—C10 | −133.7 (3) | K1—O4—C38—C39 | 114.9 (5) |
C3—C4—C12—C11 | −26.3 (4) | O4—C38—C39—C40 | 27.4 (8) |
V1—C4—C12—C11 | 44.0 (2) | C38—C39—C40—C41 | −9.6 (8) |
C9—C11—C12—C10 | 0.4 (4) | C38—O4—C41—C40 | 30.1 (8) |
C1—C11—C12—C10 | 176.4 (2) | K1—O4—C41—C40 | −113.8 (7) |
C9—C11—C12—C4 | −177.4 (2) | C39—C40—C41—O4 | −11.7 (9) |
C1—C11—C12—C4 | −1.3 (3) | C41'—O4'—C38'—C39' | 16 (4) |
C6—C5—C13—C10 | −177.0 (3) | K1—O4'—C38'—C39' | −150 (2) |
C6—C5—C13—C14 | 0.4 (4) | O4'—C38'—C39'—C40' | −15 (4) |
C12—C10—C13—C5 | 178.1 (3) | C38'—C39'—C40'—C41' | 9 (4) |
C12—C10—C13—C14 | 0.7 (4) | C38'—O4'—C41'—C40' | −11 (5) |
C7—C8—C14—C9 | 178.8 (3) | K1—O4'—C41'—C40' | 154 (3) |
C7—C8—C14—C13 | 0.5 (4) | C39'—C40'—C41'—O4' | 1 (4) |
C11—C9—C14—C8 | −177.0 (3) | C47ii—O5—C42—C43 | 178.7 (3) |
C11—C9—C14—C13 | 1.4 (4) | K2—O5—C42—C43 | 40.6 (3) |
C5—C13—C14—C8 | −0.3 (4) | C44—O6—C43—C42 | −174.9 (3) |
C10—C13—C14—C8 | 177.2 (2) | K2—O6—C43—C42 | 55.8 (3) |
C5—C13—C14—C9 | −178.7 (2) | O5—C42—C43—O6 | −64.2 (4) |
C10—C13—C14—C9 | −1.2 (4) | C43—O6—C44—C45 | −173.4 (3) |
C25—C15—C16—C17 | 34.7 (4) | K2—O6—C44—C45 | −45.6 (4) |
V1—C15—C16—C17 | −61.1 (2) | C46—O7—C45—C44 | 174.0 (3) |
C25—C15—C16—V1 | 95.8 (3) | K2—O7—C45—C44 | −55.2 (3) |
C15—C16—C17—C18 | 0.1 (4) | O6—C44—C45—O7 | 67.8 (4) |
V1—C16—C17—C18 | −62.6 (2) | C45—O7—C46—C47 | 177.1 (3) |
C15—C16—C17—V1 | 62.7 (2) | K2—O7—C46—C47 | 46.7 (4) |
C16—C17—C18—C26 | −34.3 (4) | O7—C46—C47—O5ii | −65.4 (4) |
V1—C17—C18—C26 | −94.3 (3) | C51—O8—C48—C49 | −33 (2) |
C16—C17—C18—V1 | 59.9 (2) | K2—O8—C48—C49 | 172.1 (16) |
C27—C19—C20—C21 | −0.4 (6) | O8—C48—C49—C50 | 16 (2) |
C19—C20—C21—C22 | 0.8 (6) | C48—C49—C50—C51 | 5 (2) |
C20—C21—C22—C28 | −0.4 (6) | C48—O8—C51—C50 | 35 (2) |
C28—C23—C25—C26 | −4.3 (4) | K2—O8—C51—C50 | −166.0 (18) |
C28—C23—C25—C15 | 173.7 (3) | C49—C50—C51—O8 | −23 (2) |
C16—C15—C25—C23 | 147.3 (3) | C51'—O8'—C48'—C49' | −10 (6) |
V1—C15—C25—C23 | −139.9 (3) | K2—O8'—C48'—C49' | −152 (4) |
C16—C15—C25—C26 | −34.6 (4) | O8'—C48'—C49'—C50' | 0 (6) |
V1—C15—C25—C26 | 38.2 (3) | C48'—C49'—C50'—C51' | 9 (6) |
C27—C24—C26—C25 | 2.1 (4) | C48'—O8'—C51'—C50' | 16 (5) |
C27—C24—C26—C18 | −174.9 (3) | K2—O8'—C51'—C50' | 141 (3) |
C23—C25—C26—C24 | 1.7 (4) | C49'—C50'—C51'—O8' | −15 (5) |
C15—C25—C26—C24 | −176.5 (3) | C51"—O8"—C48"—C49" | 28 (2) |
C23—C25—C26—C18 | 179.0 (3) | K2—O8"—C48"—C49" | −115.8 (17) |
C15—C25—C26—C18 | 0.8 (4) | O8"—C48"—C49"—C50" | −8 (2) |
C17—C18—C26—C24 | −149.8 (3) | C48"—C49"—C50"—C51" | −14 (2) |
V1—C18—C26—C24 | 138.7 (3) | C48"—O8"—C51"—C50" | −37 (2) |
C17—C18—C26—C25 | 33.0 (4) | K2—O8"—C51"—C50" | 107.3 (15) |
V1—C18—C26—C25 | −38.4 (3) | C49"—C50"—C51"—O8" | 30.8 (19) |
C26—C24—C27—C19 | 175.9 (3) | C55—O9—C52—C53 | −14.6 (7) |
C26—C24—C27—C28 | −3.3 (5) | O9—C52—C53—C54 | 20.1 (6) |
C20—C19—C27—C24 | −179.6 (3) | C52—C53—C54—C55 | −17.6 (7) |
C20—C19—C27—C28 | −0.3 (5) | C52—O9—C55—C54 | 2.7 (9) |
C21—C22—C28—C23 | 178.9 (3) | C53—C54—C55—O9 | 9.8 (8) |
C21—C22—C28—C27 | −0.3 (5) | | |
Symmetry codes: (i) −x+1, −y, −z+2; (ii) −x+2, −y+1, −z+1. |
Tetrakis(1,2-dimethoxyethane)potassium
bis(
η4-anthracene)[1,2-bis(dimethylphosphanyl)ethane]vanadium (7b)
top
Crystal data top
[K(C4H10O2)4][V(C14H10)2(C6H16P2)] | Z = 2 |
Mr = 957.08 | F(000) = 1024 |
Triclinic, P1 | Dx = 1.241 Mg m−3 |
a = 12.4421 (7) Å | Mo Kα radiation, λ = 0.71073 Å |
b = 13.9771 (8) Å | Cell parameters from 3223 reflections |
c = 15.1934 (9) Å | θ = 2.6–26.3° |
α = 97.350 (1)° | µ = 0.39 mm−1 |
β = 93.436 (1)° | T = 173 K |
γ = 101.178 (1)° | Plate, green |
V = 2561.0 (3) Å3 | 0.50 × 0.30 × 0.10 mm |
Data collection top
Siemens SMART CCD platform diffractometer | 8129 reflections with I > 2σ(I) |
Radiation source: normal-focus sealed tube | Rint = 0.029 |
ω scans | θmax = 26.4°, θmin = 1.7° |
Absorption correction: multi-scan (SADABS; Sheldrick, 1996) | h = −15→15 |
Tmin = 0.830, Tmax = 0.962 | k = −17→17 |
28378 measured reflections | l = −18→18 |
10457 independent reflections | |
Refinement top
Refinement on F2 | Primary atom site location: structure-invariant direct methods |
Least-squares matrix: full | Secondary atom site location: difference Fourier map |
R[F2 > 2σ(F2)] = 0.034 | Hydrogen site location: mixed |
wR(F2) = 0.093 | H atoms treated by a mixture of independent and constrained refinement |
S = 1.02 | w = 1/[σ2(Fo2) + (0.0417P)2 + 0.8265P] where P = (Fo2 + 2Fc2)/3 |
10457 reflections | (Δ/σ)max = 0.001 |
821 parameters | Δρmax = 0.36 e Å−3 |
644 restraints | Δρmin = −0.26 e Å−3 |
Special details top
Geometry. All esds (except the esd in the dihedral angle between two l.s. planes)
are estimated using the full covariance matrix. The cell esds are taken
into account individually in the estimation of esds in distances, angles
and torsion angles; correlations between esds in cell parameters are only
used when they are defined by crystal symmetry. An approximate (isotropic)
treatment of cell esds is used for estimating esds involving l.s. planes. |
Refinement. The positional parameters of the hydrogen atoms on the
metal-coordinating carbon atoms were refined to best describe
their true positions. Pairs of DME ligands on the cation were modeled as disordered
over two positions: C35-O1-C36-C37-O2-C38 and
C43-O5-C44-C45-O6-C46, 0.744 (5):0.256 (5), C39-O3-C40-C41-O4-C42
and C47-O7-C48-C49-O8-C50, 0.635 (3):0.365 (3). Analogous bond lengths and angles among the disordered DME
ligands were restrained to be similar. Anisotropic displacement
parameters for proximal atoms were restrained to be similar and
restrained toward the expected motion relative to bond direction. |
Fractional atomic coordinates and isotropic or equivalent isotropic displacement parameters (Å2) top | x | y | z | Uiso*/Ueq | Occ. (<1) |
V1 | 0.06146 (2) | 0.21760 (2) | 0.23164 (2) | 0.02722 (8) | |
K1 | 0.46861 (3) | 0.79672 (3) | 0.20340 (3) | 0.03572 (10) | |
P1 | −0.02590 (4) | 0.15573 (4) | 0.35565 (3) | 0.03570 (12) | |
P2 | 0.12894 (4) | 0.35153 (3) | 0.35090 (3) | 0.03387 (11) | |
C1 | 0.00094 (15) | 0.33835 (13) | 0.16375 (11) | 0.0326 (4) | |
H1 | 0.0255 (15) | 0.4042 (15) | 0.1868 (13) | 0.039* | |
C2 | −0.08314 (15) | 0.28078 (13) | 0.20589 (12) | 0.0339 (4) | |
H2 | −0.1204 (16) | 0.3105 (14) | 0.2528 (13) | 0.041* | |
C3 | −0.11181 (15) | 0.18010 (14) | 0.17233 (12) | 0.0344 (4) | |
H3 | −0.1656 (16) | 0.1378 (14) | 0.1959 (13) | 0.041* | |
C4 | −0.05677 (15) | 0.14718 (13) | 0.09964 (11) | 0.0327 (4) | |
H4 | −0.0656 (15) | 0.0786 (15) | 0.0826 (12) | 0.039* | |
C5 | 0.04827 (16) | 0.21634 (17) | −0.20169 (12) | 0.0446 (5) | |
H5 | 0.033119 | 0.148006 | −0.224015 | 0.054* | |
C6 | 0.08338 (17) | 0.28371 (19) | −0.25811 (14) | 0.0531 (6) | |
H6 | 0.091370 | 0.261729 | −0.318715 | 0.064* | |
C7 | 0.10704 (17) | 0.38396 (19) | −0.22592 (14) | 0.0525 (6) | |
H7 | 0.130943 | 0.430296 | −0.264862 | 0.063* | |
C8 | 0.09615 (15) | 0.41647 (16) | −0.13844 (14) | 0.0440 (5) | |
H8 | 0.113379 | 0.485135 | −0.117451 | 0.053* | |
C9 | 0.04696 (14) | 0.38030 (13) | 0.01208 (12) | 0.0336 (4) | |
H9 | 0.064382 | 0.448667 | 0.034329 | 0.040* | |
C10 | −0.00513 (14) | 0.17942 (13) | −0.05244 (11) | 0.0342 (4) | |
H10 | −0.022541 | 0.110859 | −0.073866 | 0.041* | |
C11 | 0.01029 (13) | 0.31435 (12) | 0.06883 (11) | 0.0299 (4) | |
C12 | −0.01882 (13) | 0.21086 (12) | 0.03491 (11) | 0.0297 (4) | |
C13 | 0.03435 (14) | 0.24661 (14) | −0.11165 (11) | 0.0347 (4) | |
C14 | 0.05966 (14) | 0.34938 (14) | −0.07895 (12) | 0.0347 (4) | |
C15 | 0.19018 (14) | 0.14433 (13) | 0.29735 (12) | 0.0316 (4) | |
H15 | 0.1786 (15) | 0.1142 (14) | 0.3478 (13) | 0.038* | |
C16 | 0.13836 (15) | 0.09077 (13) | 0.21315 (12) | 0.0328 (4) | |
H16 | 0.0990 (16) | 0.0256 (15) | 0.2073 (13) | 0.039* | |
C17 | 0.15892 (15) | 0.14169 (13) | 0.14043 (12) | 0.0337 (4) | |
H17 | 0.1310 (16) | 0.1146 (14) | 0.0809 (14) | 0.040* | |
C18 | 0.22395 (15) | 0.23891 (13) | 0.15800 (11) | 0.0326 (4) | |
H18 | 0.2270 (15) | 0.2763 (14) | 0.1104 (13) | 0.039* | |
C19 | 0.61191 (15) | 0.38668 (13) | 0.28334 (13) | 0.0401 (4) | |
H19 | 0.626944 | 0.418608 | 0.232556 | 0.048* | |
C20 | 0.69306 (16) | 0.39876 (14) | 0.35145 (14) | 0.0440 (5) | |
H20 | 0.762971 | 0.439078 | 0.347525 | 0.053* | |
C21 | 0.67329 (16) | 0.35205 (15) | 0.42648 (13) | 0.0440 (5) | |
H21 | 0.729301 | 0.361144 | 0.473874 | 0.053* | |
C22 | 0.57294 (16) | 0.29312 (15) | 0.43151 (13) | 0.0418 (4) | |
H22 | 0.560411 | 0.261085 | 0.482548 | 0.050* | |
C23 | 0.38342 (14) | 0.21556 (13) | 0.36483 (11) | 0.0343 (4) | |
H23 | 0.371007 | 0.180314 | 0.413972 | 0.041* | |
C24 | 0.41975 (15) | 0.31444 (12) | 0.21805 (12) | 0.0334 (4) | |
H24 | 0.432148 | 0.346682 | 0.167111 | 0.040* | |
C25 | 0.30069 (14) | 0.20396 (12) | 0.29843 (11) | 0.0297 (4) | |
C26 | 0.31890 (14) | 0.25626 (12) | 0.22332 (11) | 0.0298 (4) | |
C27 | 0.50657 (14) | 0.32796 (12) | 0.28680 (12) | 0.0329 (4) | |
C28 | 0.48755 (15) | 0.27878 (13) | 0.36263 (11) | 0.0335 (4) | |
C29 | −0.16977 (18) | 0.16037 (18) | 0.37401 (15) | 0.0558 (6) | |
H29A | −0.185252 | 0.143403 | 0.433226 | 0.084* | |
H29B | −0.218808 | 0.113209 | 0.328573 | 0.084* | |
H29C | −0.181882 | 0.226957 | 0.370006 | 0.084* | |
C30 | −0.03589 (17) | 0.02695 (15) | 0.37493 (14) | 0.0461 (5) | |
H30A | −0.063794 | 0.018859 | 0.433060 | 0.069* | |
H30B | 0.037040 | 0.010305 | 0.373932 | 0.069* | |
H30C | −0.086239 | −0.016821 | 0.328052 | 0.069* | |
C31 | 0.0406 (2) | 0.22322 (17) | 0.46620 (13) | 0.0592 (6) | |
H31A | −0.013854 | 0.254400 | 0.497905 | 0.071* | |
H31B | 0.062948 | 0.175356 | 0.502631 | 0.071* | |
C32 | 0.14081 (18) | 0.30210 (15) | 0.45722 (12) | 0.0455 (5) | |
H32A | 0.207628 | 0.273645 | 0.460465 | 0.055* | |
H32B | 0.148611 | 0.356404 | 0.507339 | 0.055* | |
C33 | 0.03947 (17) | 0.43937 (14) | 0.38107 (13) | 0.0434 (5) | |
H33A | 0.074267 | 0.486276 | 0.433194 | 0.065* | |
H33B | −0.031712 | 0.403364 | 0.395105 | 0.065* | |
H33C | 0.028338 | 0.475119 | 0.330951 | 0.065* | |
C34 | 0.26084 (17) | 0.43904 (14) | 0.35982 (14) | 0.0476 (5) | |
H34A | 0.268505 | 0.484713 | 0.415476 | 0.071* | |
H34B | 0.263513 | 0.476171 | 0.309201 | 0.071* | |
H34C | 0.321026 | 0.403006 | 0.359542 | 0.071* | |
C35 | 0.5179 (5) | 0.5464 (3) | 0.1194 (3) | 0.0858 (15) | 0.744 (5) |
H35A | 0.440814 | 0.530642 | 0.132616 | 0.129* | 0.744 (5) |
H35B | 0.565685 | 0.543059 | 0.172108 | 0.129* | 0.744 (5) |
H35C | 0.530351 | 0.498967 | 0.069712 | 0.129* | 0.744 (5) |
O1 | 0.5420 (5) | 0.6425 (3) | 0.0961 (5) | 0.0513 (14) | 0.744 (5) |
C36 | 0.6532 (4) | 0.6687 (3) | 0.0768 (4) | 0.0616 (13) | 0.744 (5) |
H36A | 0.665093 | 0.626134 | 0.022423 | 0.074* | 0.744 (5) |
H36B | 0.702050 | 0.657493 | 0.126613 | 0.074* | 0.744 (5) |
C37 | 0.6817 (3) | 0.7737 (3) | 0.0629 (2) | 0.0506 (9) | 0.744 (5) |
H37A | 0.757389 | 0.788990 | 0.044396 | 0.061* | 0.744 (5) |
H37B | 0.630567 | 0.786312 | 0.015326 | 0.061* | 0.744 (5) |
O2 | 0.67425 (19) | 0.83395 (17) | 0.14318 (16) | 0.0438 (6) | 0.744 (5) |
C38 | 0.7198 (7) | 0.9339 (6) | 0.1419 (8) | 0.070 (3) | 0.744 (5) |
H38A | 0.711179 | 0.972251 | 0.198758 | 0.105* | 0.744 (5) |
H38B | 0.681953 | 0.957618 | 0.093252 | 0.105* | 0.744 (5) |
H38C | 0.798191 | 0.941468 | 0.132822 | 0.105* | 0.744 (5) |
C35' | 0.5931 (11) | 0.5694 (8) | 0.1349 (7) | 0.061 (3) | 0.256 (5) |
H35D | 0.532961 | 0.539892 | 0.167914 | 0.092* | 0.256 (5) |
H35E | 0.661539 | 0.587164 | 0.174052 | 0.092* | 0.256 (5) |
H35F | 0.601701 | 0.521977 | 0.083762 | 0.092* | 0.256 (5) |
O1' | 0.5686 (13) | 0.6553 (9) | 0.1043 (11) | 0.041 (3) | 0.256 (5) |
C36' | 0.6513 (14) | 0.6970 (10) | 0.0532 (12) | 0.066 (4) | 0.256 (5) |
H36C | 0.652016 | 0.651393 | −0.002197 | 0.079* | 0.256 (5) |
H36D | 0.723995 | 0.707557 | 0.087190 | 0.079* | 0.256 (5) |
C37' | 0.6311 (12) | 0.7911 (7) | 0.0308 (7) | 0.064 (3) | 0.256 (5) |
H37C | 0.685703 | 0.816676 | −0.009677 | 0.076* | 0.256 (5) |
H37D | 0.557089 | 0.780331 | −0.001219 | 0.076* | 0.256 (5) |
O2' | 0.6375 (6) | 0.8614 (5) | 0.1063 (6) | 0.051 (2) | 0.256 (5) |
C38' | 0.7407 (16) | 0.9245 (17) | 0.130 (2) | 0.058 (6) | 0.256 (5) |
H38D | 0.738115 | 0.967934 | 0.185026 | 0.088* | 0.256 (5) |
H38E | 0.759102 | 0.964293 | 0.081868 | 0.088* | 0.256 (5) |
H38F | 0.796729 | 0.885156 | 0.137891 | 0.088* | 0.256 (5) |
C39 | 0.5834 (5) | 0.6439 (3) | 0.3592 (4) | 0.0760 (14) | 0.635 (3) |
H39A | 0.513094 | 0.597412 | 0.343065 | 0.114* | 0.635 (3) |
H39B | 0.612193 | 0.637230 | 0.419028 | 0.114* | 0.635 (3) |
H39C | 0.635962 | 0.629815 | 0.316279 | 0.114* | 0.635 (3) |
O3 | 0.5673 (3) | 0.7410 (2) | 0.3579 (2) | 0.0519 (8) | 0.635 (3) |
C40 | 0.6655 (3) | 0.8127 (4) | 0.3804 (3) | 0.0488 (10) | 0.635 (3) |
H40A | 0.708445 | 0.817517 | 0.327762 | 0.059* | 0.635 (3) |
H40B | 0.710869 | 0.793402 | 0.428245 | 0.059* | 0.635 (3) |
C41 | 0.6373 (5) | 0.9093 (5) | 0.4110 (4) | 0.0489 (11) | 0.635 (3) |
H41A | 0.585717 | 0.901870 | 0.457933 | 0.059* | 0.635 (3) |
H41B | 0.704749 | 0.957077 | 0.436784 | 0.059* | 0.635 (3) |
O4 | 0.5888 (2) | 0.94514 (18) | 0.33961 (15) | 0.0429 (6) | 0.635 (3) |
C42 | 0.5415 (3) | 1.0266 (3) | 0.3689 (3) | 0.0592 (10) | 0.635 (3) |
H42A | 0.510483 | 1.050640 | 0.317173 | 0.089* | 0.635 (3) |
H42B | 0.598230 | 1.079313 | 0.402502 | 0.089* | 0.635 (3) |
H42C | 0.483145 | 1.006300 | 0.407187 | 0.089* | 0.635 (3) |
C39' | 0.5007 (6) | 0.6010 (4) | 0.3541 (5) | 0.0530 (16) | 0.365 (3) |
H39D | 0.433589 | 0.571367 | 0.315415 | 0.080* | 0.365 (3) |
H39E | 0.482308 | 0.613288 | 0.415830 | 0.080* | 0.365 (3) |
H39F | 0.552176 | 0.555987 | 0.350197 | 0.080* | 0.365 (3) |
O3' | 0.5504 (4) | 0.6917 (4) | 0.3265 (4) | 0.0479 (13) | 0.365 (3) |
C40' | 0.6482 (6) | 0.7347 (6) | 0.3785 (4) | 0.0554 (16) | 0.365 (3) |
H40C | 0.698474 | 0.687713 | 0.376752 | 0.066* | 0.365 (3) |
H40D | 0.632730 | 0.751407 | 0.441166 | 0.066* | 0.365 (3) |
C41' | 0.6999 (6) | 0.8241 (6) | 0.3440 (5) | 0.0566 (19) | 0.365 (3) |
H41C | 0.767603 | 0.855412 | 0.382850 | 0.068* | 0.365 (3) |
H41D | 0.722186 | 0.804901 | 0.283893 | 0.068* | 0.365 (3) |
O4' | 0.6315 (4) | 0.8964 (4) | 0.3383 (3) | 0.0546 (12) | 0.365 (3) |
C42' | 0.6055 (13) | 0.9356 (11) | 0.4216 (8) | 0.087 (4) | 0.365 (3) |
H42D | 0.572351 | 0.992832 | 0.415616 | 0.130* | 0.365 (3) |
H42E | 0.672667 | 0.956002 | 0.462238 | 0.130* | 0.365 (3) |
H42F | 0.553372 | 0.885564 | 0.445574 | 0.130* | 0.365 (3) |
C43 | 0.2278 (4) | 0.5968 (4) | 0.1347 (3) | 0.0958 (16) | 0.744 (5) |
H43A | 0.281466 | 0.588615 | 0.091139 | 0.144* | 0.744 (5) |
H43B | 0.169741 | 0.625714 | 0.108714 | 0.144* | 0.744 (5) |
H43C | 0.195308 | 0.532420 | 0.150836 | 0.144* | 0.744 (5) |
O5 | 0.2812 (3) | 0.6601 (3) | 0.2122 (2) | 0.0570 (9) | 0.744 (5) |
C44 | 0.2040 (3) | 0.6826 (4) | 0.2720 (4) | 0.0602 (13) | 0.744 (5) |
H44A | 0.162277 | 0.621370 | 0.289856 | 0.072* | 0.744 (5) |
H44B | 0.151325 | 0.716288 | 0.243198 | 0.072* | 0.744 (5) |
C45 | 0.2657 (4) | 0.7483 (3) | 0.3517 (3) | 0.0632 (11) | 0.744 (5) |
H45A | 0.214003 | 0.758190 | 0.397495 | 0.076* | 0.744 (5) |
H45B | 0.321548 | 0.715313 | 0.377109 | 0.076* | 0.744 (5) |
O6 | 0.3187 (2) | 0.8412 (2) | 0.3321 (2) | 0.0553 (7) | 0.744 (5) |
C46 | 0.2475 (6) | 0.9092 (5) | 0.3308 (5) | 0.0766 (18) | 0.744 (5) |
H46A | 0.288819 | 0.972565 | 0.318419 | 0.115* | 0.744 (5) |
H46B | 0.217517 | 0.918386 | 0.388710 | 0.115* | 0.744 (5) |
H46C | 0.187156 | 0.883664 | 0.284164 | 0.115* | 0.744 (5) |
C43' | 0.2845 (11) | 0.5417 (10) | 0.1312 (9) | 0.089 (4) | 0.256 (5) |
H43D | 0.355499 | 0.527687 | 0.114882 | 0.133* | 0.256 (5) |
H43E | 0.244429 | 0.556997 | 0.079005 | 0.133* | 0.256 (5) |
H43F | 0.241353 | 0.483989 | 0.152234 | 0.133* | 0.256 (5) |
O5' | 0.3027 (8) | 0.6251 (7) | 0.2012 (8) | 0.062 (3) | 0.256 (5) |
C44' | 0.1994 (10) | 0.6433 (10) | 0.2266 (9) | 0.062 (3) | 0.256 (5) |
H44C | 0.151738 | 0.581621 | 0.238337 | 0.075* | 0.256 (5) |
H44D | 0.161633 | 0.669430 | 0.178619 | 0.075* | 0.256 (5) |
C45' | 0.2231 (13) | 0.7193 (9) | 0.3116 (9) | 0.068 (4) | 0.256 (5) |
H45C | 0.153940 | 0.725323 | 0.338802 | 0.082* | 0.256 (5) |
H45D | 0.273021 | 0.699030 | 0.355650 | 0.082* | 0.256 (5) |
O6' | 0.2733 (7) | 0.8103 (6) | 0.2857 (6) | 0.060 (2) | 0.256 (5) |
C46' | 0.277 (2) | 0.8925 (14) | 0.3508 (13) | 0.091 (6) | 0.256 (5) |
H46D | 0.315855 | 0.952040 | 0.329668 | 0.136* | 0.256 (5) |
H46E | 0.315671 | 0.883171 | 0.406112 | 0.136* | 0.256 (5) |
H46F | 0.201843 | 0.899464 | 0.361790 | 0.136* | 0.256 (5) |
C47 | 0.3673 (5) | 0.7200 (4) | −0.0484 (3) | 0.0735 (14) | 0.635 (3) |
H47A | 0.411532 | 0.670629 | −0.039393 | 0.110* | 0.635 (3) |
H47B | 0.396683 | 0.758009 | −0.094625 | 0.110* | 0.635 (3) |
H47C | 0.290928 | 0.687007 | −0.066884 | 0.110* | 0.635 (3) |
O7 | 0.3713 (6) | 0.7833 (4) | 0.0311 (3) | 0.0771 (16) | 0.635 (3) |
C48 | 0.3132 (5) | 0.8600 (5) | 0.0201 (4) | 0.0769 (16) | 0.635 (3) |
H48A | 0.353875 | 0.905719 | −0.016847 | 0.092* | 0.635 (3) |
H48B | 0.239909 | 0.831188 | −0.011517 | 0.092* | 0.635 (3) |
C49 | 0.3001 (4) | 0.9131 (5) | 0.1032 (4) | 0.0761 (16) | 0.635 (3) |
H49A | 0.257712 | 0.867218 | 0.139062 | 0.091* | 0.635 (3) |
H49B | 0.256427 | 0.963409 | 0.092649 | 0.091* | 0.635 (3) |
O8 | 0.4013 (4) | 0.9609 (3) | 0.1531 (3) | 0.0752 (11) | 0.635 (3) |
C50 | 0.4433 (6) | 1.0533 (4) | 0.1293 (4) | 0.101 (2) | 0.635 (3) |
H50A | 0.513109 | 1.082284 | 0.164810 | 0.152* | 0.635 (3) |
H50B | 0.390715 | 1.096347 | 0.140523 | 0.152* | 0.635 (3) |
H50C | 0.455686 | 1.045923 | 0.065926 | 0.152* | 0.635 (3) |
C47' | 0.3098 (12) | 0.7430 (7) | −0.0198 (9) | 0.123 (5) | 0.365 (3) |
H47D | 0.341560 | 0.684670 | −0.015811 | 0.184* | 0.365 (3) |
H47E | 0.311911 | 0.759301 | −0.080586 | 0.184* | 0.365 (3) |
H47F | 0.233335 | 0.729466 | −0.004648 | 0.184* | 0.365 (3) |
O7' | 0.3701 (11) | 0.8220 (7) | 0.0394 (7) | 0.081 (3) | 0.365 (3) |
C48' | 0.3130 (8) | 0.8994 (7) | 0.0576 (6) | 0.058 (2) | 0.365 (3) |
H48C | 0.256132 | 0.880522 | 0.098506 | 0.070* | 0.365 (3) |
H48D | 0.275534 | 0.910183 | 0.001453 | 0.070* | 0.365 (3) |
C49' | 0.3862 (6) | 0.9894 (6) | 0.0971 (5) | 0.0588 (17) | 0.365 (3) |
H49C | 0.434076 | 1.013468 | 0.051514 | 0.071* | 0.365 (3) |
H49D | 0.341474 | 1.039346 | 0.113350 | 0.071* | 0.365 (3) |
O8' | 0.4537 (5) | 0.9837 (4) | 0.1731 (5) | 0.0576 (16) | 0.365 (3) |
C50' | 0.5278 (6) | 1.0682 (5) | 0.2094 (6) | 0.075 (2) | 0.365 (3) |
H50D | 0.568345 | 1.055740 | 0.262626 | 0.112* | 0.365 (3) |
H50E | 0.488251 | 1.121128 | 0.225666 | 0.112* | 0.365 (3) |
H50F | 0.579497 | 1.087693 | 0.165594 | 0.112* | 0.365 (3) |
Atomic displacement parameters (Å2) top | U11 | U22 | U33 | U12 | U13 | U23 |
V1 | 0.03367 (16) | 0.02644 (15) | 0.02166 (14) | 0.00820 (12) | −0.00060 (11) | 0.00209 (11) |
K1 | 0.0330 (2) | 0.0395 (2) | 0.0360 (2) | 0.00905 (17) | 0.00047 (16) | 0.00930 (17) |
P1 | 0.0442 (3) | 0.0393 (3) | 0.0252 (2) | 0.0117 (2) | 0.00355 (19) | 0.00551 (19) |
P2 | 0.0402 (3) | 0.0327 (2) | 0.0278 (2) | 0.0117 (2) | −0.00283 (19) | −0.00288 (18) |
C1 | 0.0413 (10) | 0.0253 (9) | 0.0302 (9) | 0.0097 (7) | −0.0057 (7) | 0.0002 (7) |
C2 | 0.0365 (10) | 0.0386 (10) | 0.0278 (9) | 0.0129 (8) | −0.0012 (7) | 0.0029 (7) |
C3 | 0.0329 (9) | 0.0408 (10) | 0.0287 (9) | 0.0042 (8) | −0.0006 (7) | 0.0080 (8) |
C4 | 0.0384 (10) | 0.0271 (9) | 0.0289 (9) | 0.0012 (7) | −0.0046 (7) | 0.0018 (7) |
C5 | 0.0424 (11) | 0.0607 (13) | 0.0317 (10) | 0.0143 (9) | −0.0007 (8) | 0.0056 (9) |
C6 | 0.0464 (12) | 0.0877 (18) | 0.0322 (11) | 0.0227 (12) | 0.0063 (9) | 0.0194 (11) |
C7 | 0.0402 (11) | 0.0793 (17) | 0.0483 (13) | 0.0180 (11) | 0.0087 (9) | 0.0369 (12) |
C8 | 0.0350 (10) | 0.0534 (12) | 0.0492 (12) | 0.0126 (9) | 0.0021 (9) | 0.0235 (10) |
C9 | 0.0335 (9) | 0.0303 (9) | 0.0373 (10) | 0.0079 (7) | −0.0043 (7) | 0.0076 (7) |
C10 | 0.0351 (9) | 0.0344 (9) | 0.0307 (9) | 0.0058 (7) | −0.0040 (7) | 0.0007 (7) |
C11 | 0.0285 (9) | 0.0308 (9) | 0.0304 (9) | 0.0077 (7) | −0.0048 (7) | 0.0052 (7) |
C12 | 0.0292 (9) | 0.0313 (9) | 0.0267 (9) | 0.0046 (7) | −0.0047 (7) | 0.0028 (7) |
C13 | 0.0297 (9) | 0.0470 (11) | 0.0287 (9) | 0.0106 (8) | −0.0021 (7) | 0.0078 (8) |
C14 | 0.0259 (9) | 0.0444 (10) | 0.0369 (10) | 0.0097 (7) | −0.0015 (7) | 0.0151 (8) |
C15 | 0.0369 (9) | 0.0323 (9) | 0.0280 (9) | 0.0090 (7) | 0.0033 (7) | 0.0094 (7) |
C16 | 0.0380 (10) | 0.0269 (9) | 0.0331 (9) | 0.0079 (7) | 0.0008 (7) | 0.0018 (7) |
C17 | 0.0402 (10) | 0.0362 (10) | 0.0259 (9) | 0.0149 (8) | 0.0007 (7) | −0.0015 (7) |
C18 | 0.0416 (10) | 0.0358 (10) | 0.0233 (8) | 0.0126 (8) | 0.0032 (7) | 0.0080 (7) |
C19 | 0.0403 (10) | 0.0352 (10) | 0.0482 (11) | 0.0115 (8) | 0.0087 (9) | 0.0106 (8) |
C20 | 0.0345 (10) | 0.0396 (11) | 0.0578 (13) | 0.0086 (8) | 0.0040 (9) | 0.0043 (9) |
C21 | 0.0392 (11) | 0.0477 (12) | 0.0433 (11) | 0.0120 (9) | −0.0047 (9) | −0.0013 (9) |
C22 | 0.0430 (11) | 0.0486 (11) | 0.0340 (10) | 0.0106 (9) | 0.0007 (8) | 0.0057 (8) |
C23 | 0.0378 (10) | 0.0396 (10) | 0.0277 (9) | 0.0101 (8) | 0.0024 (7) | 0.0098 (7) |
C24 | 0.0410 (10) | 0.0318 (9) | 0.0304 (9) | 0.0117 (8) | 0.0065 (8) | 0.0082 (7) |
C25 | 0.0368 (9) | 0.0286 (9) | 0.0261 (8) | 0.0115 (7) | 0.0042 (7) | 0.0045 (7) |
C26 | 0.0398 (10) | 0.0270 (8) | 0.0253 (8) | 0.0128 (7) | 0.0046 (7) | 0.0040 (7) |
C27 | 0.0377 (10) | 0.0280 (9) | 0.0351 (9) | 0.0124 (7) | 0.0063 (8) | 0.0019 (7) |
C28 | 0.0382 (10) | 0.0342 (9) | 0.0297 (9) | 0.0122 (8) | 0.0029 (7) | 0.0027 (7) |
C29 | 0.0583 (14) | 0.0766 (16) | 0.0444 (12) | 0.0291 (12) | 0.0219 (10) | 0.0211 (11) |
C30 | 0.0508 (12) | 0.0457 (11) | 0.0451 (12) | 0.0097 (9) | 0.0109 (9) | 0.0161 (9) |
C31 | 0.0881 (18) | 0.0603 (14) | 0.0238 (10) | 0.0047 (13) | 0.0028 (10) | 0.0031 (9) |
C32 | 0.0613 (13) | 0.0485 (12) | 0.0262 (9) | 0.0187 (10) | −0.0065 (9) | −0.0029 (8) |
C33 | 0.0503 (12) | 0.0421 (11) | 0.0381 (11) | 0.0183 (9) | 0.0011 (9) | −0.0056 (8) |
C34 | 0.0477 (12) | 0.0381 (11) | 0.0512 (12) | 0.0086 (9) | −0.0035 (9) | −0.0119 (9) |
C35 | 0.132 (4) | 0.038 (2) | 0.085 (3) | 0.014 (2) | −0.011 (3) | 0.0131 (19) |
O1 | 0.050 (3) | 0.0348 (15) | 0.069 (2) | 0.0101 (16) | −0.0064 (18) | 0.0109 (14) |
C36 | 0.054 (2) | 0.061 (3) | 0.069 (3) | 0.025 (2) | −0.009 (2) | −0.012 (2) |
C37 | 0.0392 (18) | 0.068 (2) | 0.0419 (18) | 0.0078 (16) | 0.0054 (14) | 0.0001 (16) |
O2 | 0.0423 (12) | 0.0425 (12) | 0.0447 (13) | 0.0021 (9) | 0.0080 (10) | 0.0067 (9) |
C38 | 0.075 (5) | 0.055 (3) | 0.075 (3) | −0.009 (3) | 0.020 (3) | 0.017 (2) |
C35' | 0.080 (8) | 0.053 (6) | 0.053 (6) | 0.022 (6) | −0.001 (6) | 0.012 (5) |
O1' | 0.035 (6) | 0.043 (5) | 0.047 (5) | 0.005 (4) | 0.007 (5) | 0.016 (4) |
C36' | 0.068 (7) | 0.060 (7) | 0.079 (8) | 0.014 (5) | 0.051 (6) | 0.021 (5) |
C37' | 0.081 (8) | 0.051 (5) | 0.060 (6) | 0.008 (5) | 0.039 (6) | 0.011 (4) |
O2' | 0.043 (4) | 0.042 (4) | 0.063 (5) | −0.007 (3) | 0.023 (3) | 0.003 (3) |
C38' | 0.035 (6) | 0.049 (7) | 0.093 (16) | 0.005 (5) | −0.006 (8) | 0.027 (8) |
C39 | 0.097 (4) | 0.043 (2) | 0.087 (3) | 0.022 (3) | −0.011 (3) | 0.004 (2) |
O3 | 0.0567 (19) | 0.0468 (18) | 0.0559 (19) | 0.0165 (15) | −0.0028 (14) | 0.0152 (14) |
C40 | 0.049 (2) | 0.065 (3) | 0.037 (2) | 0.020 (2) | −0.0033 (17) | 0.016 (2) |
C41 | 0.052 (3) | 0.062 (3) | 0.030 (3) | 0.005 (2) | −0.0006 (19) | 0.009 (2) |
O4 | 0.0536 (14) | 0.0436 (14) | 0.0352 (13) | 0.0195 (11) | 0.0046 (10) | 0.0049 (10) |
C42 | 0.057 (2) | 0.049 (2) | 0.070 (2) | 0.0179 (17) | 0.0084 (18) | −0.0076 (17) |
C39' | 0.069 (4) | 0.035 (3) | 0.058 (4) | 0.015 (3) | 0.013 (3) | 0.008 (3) |
O3' | 0.046 (2) | 0.045 (3) | 0.052 (3) | 0.006 (2) | −0.009 (2) | 0.016 (2) |
C40' | 0.049 (4) | 0.069 (4) | 0.050 (4) | 0.013 (3) | −0.003 (3) | 0.015 (3) |
C41' | 0.044 (4) | 0.070 (4) | 0.049 (5) | −0.004 (3) | −0.007 (3) | 0.008 (4) |
O4' | 0.070 (3) | 0.049 (3) | 0.037 (3) | −0.006 (2) | 0.000 (2) | 0.005 (2) |
C42' | 0.112 (11) | 0.080 (9) | 0.058 (6) | −0.003 (6) | 0.022 (6) | −0.001 (5) |
C43 | 0.069 (3) | 0.102 (4) | 0.091 (3) | −0.022 (3) | −0.020 (2) | −0.012 (3) |
O5 | 0.0303 (16) | 0.068 (2) | 0.0641 (17) | −0.0041 (14) | 0.0052 (12) | −0.0032 (15) |
C44 | 0.039 (2) | 0.064 (3) | 0.082 (4) | 0.008 (2) | 0.014 (3) | 0.028 (2) |
C45 | 0.073 (3) | 0.076 (3) | 0.052 (2) | 0.028 (2) | 0.019 (2) | 0.0232 (19) |
O6 | 0.0515 (15) | 0.0548 (15) | 0.0625 (18) | 0.0188 (12) | 0.0056 (13) | 0.0072 (13) |
C46 | 0.073 (3) | 0.074 (3) | 0.091 (4) | 0.040 (2) | 0.000 (2) | 0.005 (3) |
C43' | 0.067 (8) | 0.084 (8) | 0.097 (8) | −0.001 (6) | −0.007 (6) | −0.026 (6) |
O5' | 0.039 (4) | 0.068 (6) | 0.079 (5) | 0.014 (4) | 0.013 (4) | −0.001 (4) |
C44' | 0.046 (5) | 0.064 (6) | 0.080 (8) | 0.016 (5) | 0.005 (5) | 0.015 (5) |
C45' | 0.056 (8) | 0.096 (7) | 0.048 (8) | −0.003 (6) | 0.019 (6) | 0.015 (6) |
O6' | 0.054 (4) | 0.066 (4) | 0.063 (5) | 0.020 (3) | 0.012 (4) | 0.008 (4) |
C46' | 0.100 (16) | 0.098 (10) | 0.072 (11) | 0.021 (10) | 0.029 (10) | −0.013 (9) |
C47 | 0.088 (4) | 0.091 (4) | 0.040 (2) | 0.027 (3) | −0.010 (2) | −0.002 (2) |
O7 | 0.076 (3) | 0.122 (5) | 0.044 (2) | 0.059 (3) | −0.0115 (18) | −0.001 (3) |
C48 | 0.067 (3) | 0.117 (5) | 0.060 (4) | 0.048 (3) | 0.005 (3) | 0.017 (3) |
C49 | 0.066 (3) | 0.106 (4) | 0.074 (4) | 0.051 (3) | 0.007 (3) | 0.027 (3) |
O8 | 0.088 (3) | 0.052 (2) | 0.098 (3) | 0.029 (2) | 0.018 (2) | 0.026 (2) |
C50 | 0.171 (6) | 0.069 (3) | 0.093 (4) | 0.061 (4) | 0.064 (4) | 0.036 (3) |
C47' | 0.154 (11) | 0.085 (6) | 0.122 (10) | 0.046 (7) | −0.081 (9) | −0.005 (6) |
O7' | 0.100 (5) | 0.090 (5) | 0.059 (4) | 0.056 (4) | −0.037 (4) | −0.003 (3) |
C48' | 0.066 (5) | 0.075 (5) | 0.039 (6) | 0.029 (4) | −0.001 (5) | 0.008 (4) |
C49' | 0.060 (4) | 0.058 (4) | 0.072 (5) | 0.029 (3) | 0.011 (3) | 0.033 (4) |
O8' | 0.051 (3) | 0.041 (3) | 0.078 (4) | 0.012 (2) | −0.009 (3) | 0.002 (2) |
C50' | 0.065 (4) | 0.042 (4) | 0.111 (7) | 0.015 (3) | 0.005 (4) | −0.016 (4) |
Geometric parameters (Å, º) top
V1—C16 | 2.1677 (18) | C37—H37B | 0.9900 |
V1—C2 | 2.1886 (18) | O2—C38 | 1.405 (8) |
V1—C17 | 2.2002 (17) | C38—H38A | 0.9800 |
V1—C3 | 2.2232 (18) | C38—H38B | 0.9800 |
V1—C15 | 2.3056 (17) | C38—H38C | 0.9800 |
V1—C1 | 2.3076 (17) | C35'—O1' | 1.420 (12) |
V1—C18 | 2.3561 (18) | C35'—H35D | 0.9800 |
V1—C4 | 2.3948 (17) | C35'—H35E | 0.9800 |
V1—P1 | 2.4036 (5) | C35'—H35F | 0.9800 |
V1—P2 | 2.4151 (5) | O1'—C36' | 1.408 (12) |
K1—O2' | 2.718 (5) | C36'—C37' | 1.463 (13) |
K1—O5 | 2.734 (3) | C36'—H36C | 0.9900 |
K1—O2 | 2.746 (2) | C36'—H36D | 0.9900 |
K1—O8' | 2.750 (6) | C37'—O2' | 1.400 (10) |
K1—O8 | 2.770 (4) | C37'—H37C | 0.9900 |
K1—O3' | 2.782 (5) | C37'—H37D | 0.9900 |
K1—O7 | 2.786 (5) | O2'—C38' | 1.405 (14) |
K1—O7' | 2.804 (9) | C38'—H38D | 0.9800 |
K1—O4' | 2.815 (4) | C38'—H38E | 0.9800 |
K1—O6' | 2.827 (6) | C38'—H38F | 0.9800 |
K1—O5' | 2.841 (10) | C39—O3 | 1.411 (5) |
K1—O3 | 2.850 (3) | C39—H39A | 0.9800 |
K1—O1' | 2.852 (11) | C39—H39B | 0.9800 |
K1—O4 | 2.855 (2) | C39—H39C | 0.9800 |
K1—O1 | 2.861 (5) | O3—C40 | 1.415 (5) |
K1—O6 | 2.875 (3) | C40—C41 | 1.486 (7) |
P1—C29 | 1.840 (2) | C40—H40A | 0.9900 |
P1—C30 | 1.842 (2) | C40—H40B | 0.9900 |
P1—C31 | 1.876 (2) | C41—O4 | 1.402 (6) |
P2—C34 | 1.833 (2) | C41—H41A | 0.9900 |
P2—C33 | 1.8448 (18) | C41—H41B | 0.9900 |
P2—C32 | 1.8453 (19) | O4—C42 | 1.415 (4) |
C1—C2 | 1.427 (3) | C42—H42A | 0.9800 |
C1—C11 | 1.455 (2) | C42—H42B | 0.9800 |
C1—H1 | 0.927 (19) | C42—H42C | 0.9800 |
C2—C3 | 1.403 (3) | C39'—O3' | 1.425 (7) |
C2—H2 | 0.97 (2) | C39'—H39D | 0.9800 |
C3—C4 | 1.408 (3) | C39'—H39E | 0.9800 |
C3—H3 | 0.92 (2) | C39'—H39F | 0.9800 |
C4—C12 | 1.449 (2) | O3'—C40' | 1.395 (7) |
C4—H4 | 0.944 (19) | C40'—C41' | 1.465 (9) |
C5—C6 | 1.380 (3) | C40'—H40C | 0.9900 |
C5—C13 | 1.410 (3) | C40'—H40D | 0.9900 |
C5—H5 | 0.9500 | C41'—O4' | 1.450 (9) |
C6—C7 | 1.392 (3) | C41'—H41C | 0.9900 |
C6—H6 | 0.9500 | C41'—H41D | 0.9900 |
C7—C8 | 1.372 (3) | O4'—C42' | 1.396 (10) |
C7—H7 | 0.9500 | C42'—H42D | 0.9800 |
C8—C14 | 1.415 (3) | C42'—H42E | 0.9800 |
C8—H8 | 0.9500 | C42'—H42F | 0.9800 |
C9—C11 | 1.374 (2) | C43—O5 | 1.422 (5) |
C9—C14 | 1.423 (3) | C43—H43A | 0.9800 |
C9—H9 | 0.9500 | C43—H43B | 0.9800 |
C10—C12 | 1.375 (2) | C43—H43C | 0.9800 |
C10—C13 | 1.422 (3) | O5—C44 | 1.413 (5) |
C10—H10 | 0.9500 | C44—C45 | 1.494 (6) |
C11—C12 | 1.440 (2) | C44—H44A | 0.9900 |
C13—C14 | 1.426 (3) | C44—H44B | 0.9900 |
C15—C16 | 1.443 (2) | C45—O6 | 1.415 (4) |
C15—C25 | 1.461 (2) | C45—H45A | 0.9900 |
C15—H15 | 0.93 (2) | C45—H45B | 0.9900 |
C16—C17 | 1.399 (3) | O6—C46 | 1.421 (5) |
C16—H16 | 0.938 (19) | C46—H46A | 0.9800 |
C17—C18 | 1.424 (3) | C46—H46B | 0.9800 |
C17—H17 | 0.95 (2) | C46—H46C | 0.9800 |
C18—C26 | 1.458 (2) | C43'—O5' | 1.446 (11) |
C18—H18 | 0.94 (2) | C43'—H43D | 0.9800 |
C19—C20 | 1.372 (3) | C43'—H43E | 0.9800 |
C19—C27 | 1.413 (3) | C43'—H43F | 0.9800 |
C19—H19 | 0.9500 | O5'—C44' | 1.424 (11) |
C20—C21 | 1.396 (3) | C44'—C45' | 1.538 (13) |
C20—H20 | 0.9500 | C44'—H44C | 0.9900 |
C21—C22 | 1.368 (3) | C44'—H44D | 0.9900 |
C21—H21 | 0.9500 | C45'—O6' | 1.419 (12) |
C22—C28 | 1.412 (3) | C45'—H45C | 0.9900 |
C22—H22 | 0.9500 | C45'—H45D | 0.9900 |
C23—C25 | 1.368 (2) | O6'—C46' | 1.408 (13) |
C23—C28 | 1.425 (2) | C46'—H46D | 0.9800 |
C23—H23 | 0.9500 | C46'—H46E | 0.9800 |
C24—C26 | 1.369 (2) | C46'—H46F | 0.9800 |
C24—C27 | 1.424 (2) | C47—O7 | 1.394 (6) |
C24—H24 | 0.9500 | C47—H47A | 0.9800 |
C25—C26 | 1.438 (2) | C47—H47B | 0.9800 |
C27—C28 | 1.424 (2) | C47—H47C | 0.9800 |
C29—H29A | 0.9800 | O7—C48 | 1.426 (6) |
C29—H29B | 0.9800 | C48—C49 | 1.414 (7) |
C29—H29C | 0.9800 | C48—H48A | 0.9900 |
C30—H30A | 0.9800 | C48—H48B | 0.9900 |
C30—H30B | 0.9800 | C49—O8 | 1.428 (7) |
C30—H30C | 0.9800 | C49—H49A | 0.9900 |
C31—C32 | 1.522 (3) | C49—H49B | 0.9900 |
C31—H31A | 0.9900 | O8—C50 | 1.396 (6) |
C31—H31B | 0.9900 | C50—H50A | 0.9800 |
C32—H32A | 0.9900 | C50—H50B | 0.9800 |
C32—H32B | 0.9900 | C50—H50C | 0.9800 |
C33—H33A | 0.9800 | C47'—O7' | 1.391 (11) |
C33—H33B | 0.9800 | C47'—H47D | 0.9800 |
C33—H33C | 0.9800 | C47'—H47E | 0.9800 |
C34—H34A | 0.9800 | C47'—H47F | 0.9800 |
C34—H34B | 0.9800 | O7'—C48' | 1.411 (10) |
C34—H34C | 0.9800 | C48'—C49' | 1.439 (11) |
C35—O1 | 1.413 (5) | C48'—H48C | 0.9900 |
C35—H35A | 0.9800 | C48'—H48D | 0.9900 |
C35—H35B | 0.9800 | C49'—O8' | 1.406 (9) |
C35—H35C | 0.9800 | C49'—H49C | 0.9900 |
O1—C36 | 1.419 (6) | C49'—H49D | 0.9900 |
C36—C37 | 1.488 (5) | O8'—C50' | 1.378 (8) |
C36—H36A | 0.9900 | C50'—H50D | 0.9800 |
C36—H36B | 0.9900 | C50'—H50E | 0.9800 |
C37—O2 | 1.409 (4) | C50'—H50F | 0.9800 |
C37—H37A | 0.9900 | | |
| | | |
C16—V1—C2 | 148.01 (7) | H34A—C34—H34C | 109.5 |
C16—V1—C17 | 37.36 (7) | H34B—C34—H34C | 109.5 |
C2—V1—C17 | 131.19 (7) | O1—C35—H35A | 109.5 |
C16—V1—C3 | 111.06 (7) | O1—C35—H35B | 109.5 |
C2—V1—C3 | 37.07 (7) | H35A—C35—H35B | 109.5 |
C17—V1—C3 | 107.34 (7) | O1—C35—H35C | 109.5 |
C16—V1—C15 | 37.47 (6) | H35A—C35—H35C | 109.5 |
C2—V1—C15 | 163.04 (7) | H35B—C35—H35C | 109.5 |
C17—V1—C15 | 63.93 (6) | C35—O1—C36 | 111.4 (4) |
C3—V1—C15 | 139.82 (7) | C35—O1—K1 | 118.4 (4) |
C16—V1—C1 | 145.47 (7) | C36—O1—K1 | 113.4 (3) |
C2—V1—C1 | 36.90 (7) | O1—C36—C37 | 111.1 (4) |
C17—V1—C1 | 109.01 (7) | O1—C36—H36A | 109.4 |
C3—V1—C1 | 64.00 (7) | C37—C36—H36A | 109.4 |
C15—V1—C1 | 155.58 (7) | O1—C36—H36B | 109.4 |
C16—V1—C18 | 64.29 (7) | C37—C36—H36B | 109.4 |
C2—V1—C18 | 127.10 (7) | H36A—C36—H36B | 108.0 |
C17—V1—C18 | 36.21 (6) | O2—C37—C36 | 109.0 (3) |
C3—V1—C18 | 128.38 (6) | O2—C37—K1 | 45.68 (13) |
C15—V1—C18 | 69.23 (6) | C36—C37—K1 | 82.8 (3) |
C1—V1—C18 | 91.35 (6) | O2—C37—H37A | 109.9 |
C16—V1—C4 | 88.04 (7) | C36—C37—H37A | 109.9 |
C2—V1—C4 | 62.78 (6) | K1—C37—H37A | 155.6 |
C17—V1—C4 | 72.94 (7) | O2—C37—H37B | 109.9 |
C3—V1—C4 | 35.26 (6) | C36—C37—H37B | 109.9 |
C15—V1—C4 | 125.33 (6) | K1—C37—H37B | 85.4 |
C1—V1—C4 | 69.06 (6) | H37A—C37—H37B | 108.3 |
C18—V1—C4 | 94.80 (6) | C38—O2—C37 | 113.0 (5) |
C16—V1—P1 | 89.78 (5) | C38—O2—K1 | 115.2 (4) |
C2—V1—P1 | 87.16 (5) | C37—O2—K1 | 112.79 (17) |
C17—V1—P1 | 126.66 (5) | O2—C38—H38A | 109.5 |
C3—V1—P1 | 80.97 (5) | O2—C38—H38B | 109.5 |
C15—V1—P1 | 76.23 (5) | H38A—C38—H38B | 109.5 |
C1—V1—P1 | 121.02 (5) | O2—C38—H38C | 109.5 |
C18—V1—P1 | 145.35 (5) | H38A—C38—H38C | 109.5 |
C4—V1—P1 | 107.51 (5) | H38B—C38—H38C | 109.5 |
C16—V1—P2 | 120.98 (5) | O1'—C35'—H35D | 109.5 |
C2—V1—P2 | 89.49 (5) | O1'—C35'—H35E | 109.5 |
C17—V1—P2 | 127.44 (5) | H35D—C35'—H35E | 109.5 |
C3—V1—P2 | 123.19 (5) | O1'—C35'—H35F | 109.5 |
C15—V1—P2 | 83.86 (5) | H35D—C35'—H35F | 109.5 |
C1—V1—P2 | 83.34 (5) | H35E—C35'—H35F | 109.5 |
C18—V1—P2 | 95.23 (5) | C36'—O1'—C35' | 110.8 (11) |
C4—V1—P2 | 150.79 (5) | C36'—O1'—K1 | 113.8 (8) |
P1—V1—P2 | 78.169 (19) | C35'—O1'—K1 | 125.3 (9) |
O5—K1—O2 | 146.76 (8) | O1'—C36'—C37' | 109.9 (11) |
O2'—K1—O8' | 72.8 (2) | O1'—C36'—H36C | 109.7 |
O5—K1—O8 | 106.33 (13) | C37'—C36'—H36C | 109.7 |
O2—K1—O8 | 96.89 (11) | O1'—C36'—H36D | 109.7 |
O2'—K1—O3' | 106.7 (2) | C37'—C36'—H36D | 109.7 |
O8'—K1—O3' | 143.08 (18) | H36C—C36'—H36D | 108.2 |
O5—K1—O7 | 80.12 (18) | O2'—C37'—C36' | 112.3 (11) |
O2—K1—O7 | 90.71 (16) | O2'—C37'—H37C | 109.1 |
O8—K1—O7 | 61.73 (15) | C36'—C37'—H37C | 109.1 |
O2'—K1—O7' | 74.4 (4) | O2'—C37'—H37D | 109.1 |
O8'—K1—O7' | 61.1 (2) | C36'—C37'—H37D | 109.1 |
O3'—K1—O7' | 155.7 (2) | H37C—C37'—H37D | 107.9 |
O2'—K1—O4' | 78.5 (2) | C37'—O2'—C38' | 115.7 (13) |
O8'—K1—O4' | 83.91 (15) | C37'—O2'—K1 | 107.3 (5) |
O3'—K1—O4' | 60.55 (15) | C38'—O2'—K1 | 132.6 (14) |
O7'—K1—O4' | 140.6 (3) | O2'—C38'—H38D | 109.5 |
O2'—K1—O6' | 154.1 (2) | O2'—C38'—H38E | 109.5 |
O8'—K1—O6' | 81.5 (2) | H38D—C38'—H38E | 109.5 |
O3'—K1—O6' | 95.5 (2) | O2'—C38'—H38F | 109.5 |
O7'—K1—O6' | 90.9 (3) | H38D—C38'—H38F | 109.5 |
O4'—K1—O6' | 101.9 (2) | H38E—C38'—H38F | 109.5 |
O2'—K1—O5' | 138.1 (2) | O3—C39—H39A | 109.5 |
O8'—K1—O5' | 130.8 (2) | O3—C39—H39B | 109.5 |
O3'—K1—O5' | 75.0 (3) | H39A—C39—H39B | 109.5 |
O7'—K1—O5' | 88.1 (4) | O3—C39—H39C | 109.5 |
O4'—K1—O5' | 130.6 (3) | H39A—C39—H39C | 109.5 |
O6'—K1—O5' | 60.1 (2) | H39B—C39—H39C | 109.5 |
O5—K1—O3 | 90.41 (11) | C39—O3—C40 | 112.8 (4) |
O2—K1—O3 | 87.74 (9) | C39—O3—K1 | 121.1 (3) |
O8—K1—O3 | 138.11 (12) | C40—O3—K1 | 104.4 (2) |
O7—K1—O3 | 160.14 (13) | O3—C40—C41 | 109.1 (4) |
O2'—K1—O1' | 61.2 (3) | O3—C40—H40A | 109.9 |
O8'—K1—O1' | 129.6 (3) | C41—C40—H40A | 109.9 |
O3'—K1—O1' | 73.6 (4) | O3—C40—H40B | 109.9 |
O7'—K1—O1' | 86.5 (4) | C41—C40—H40B | 109.9 |
O4'—K1—O1' | 104.9 (4) | H40A—C40—H40B | 108.3 |
O6'—K1—O1' | 140.5 (3) | O4—C41—C40 | 110.4 (4) |
O5'—K1—O1' | 80.4 (3) | O4—C41—H41A | 109.6 |
O5—K1—O4 | 129.21 (9) | C40—C41—H41A | 109.6 |
O2—K1—O4 | 77.46 (7) | O4—C41—H41B | 109.6 |
O8—K1—O4 | 80.05 (11) | C40—C41—H41B | 109.6 |
O7—K1—O4 | 138.40 (14) | H41A—C41—H41B | 108.1 |
O3—K1—O4 | 60.30 (8) | C41—O4—C42 | 111.9 (3) |
O5—K1—O1 | 86.07 (12) | C41—O4—K1 | 114.8 (3) |
O2—K1—O1 | 60.74 (11) | C42—O4—K1 | 118.4 (2) |
O8—K1—O1 | 129.10 (16) | O4—C42—H42A | 109.5 |
O7—K1—O1 | 72.78 (17) | O4—C42—H42B | 109.5 |
O3—K1—O1 | 89.29 (15) | H42A—C42—H42B | 109.5 |
O4—K1—O1 | 129.42 (14) | O4—C42—H42C | 109.5 |
O5—K1—O6 | 61.36 (9) | H42A—C42—H42C | 109.5 |
O2—K1—O6 | 149.72 (8) | H42B—C42—H42C | 109.5 |
O8—K1—O6 | 76.01 (11) | O3'—C39'—H39D | 109.5 |
O7—K1—O6 | 110.45 (14) | O3'—C39'—H39E | 109.5 |
O3—K1—O6 | 79.34 (9) | H39D—C39'—H39E | 109.5 |
O4—K1—O6 | 72.34 (8) | O3'—C39'—H39F | 109.5 |
O1—K1—O6 | 145.06 (11) | H39D—C39'—H39F | 109.5 |
C29—P1—C30 | 95.76 (10) | H39E—C39'—H39F | 109.5 |
C29—P1—C31 | 98.58 (11) | C40'—O3'—C39' | 111.1 (5) |
C30—P1—C31 | 100.81 (10) | C40'—O3'—K1 | 119.0 (4) |
C29—P1—V1 | 122.31 (7) | C39'—O3'—K1 | 129.5 (4) |
C30—P1—V1 | 121.94 (7) | O3'—C40'—C41' | 109.2 (6) |
C31—P1—V1 | 113.00 (7) | O3'—C40'—H40C | 109.8 |
C34—P2—C33 | 98.83 (9) | C41'—C40'—H40C | 109.8 |
C34—P2—C32 | 100.21 (10) | O3'—C40'—H40D | 109.8 |
C33—P2—C32 | 99.57 (9) | C41'—C40'—H40D | 109.8 |
C34—P2—V1 | 126.24 (7) | H40C—C40'—H40D | 108.3 |
C33—P2—V1 | 118.15 (7) | O4'—C41'—C40' | 115.0 (6) |
C32—P2—V1 | 109.56 (7) | O4'—C41'—K1 | 54.1 (3) |
C2—C1—C11 | 120.08 (16) | C40'—C41'—K1 | 88.2 (4) |
C2—C1—V1 | 67.02 (10) | O4'—C41'—H41C | 108.5 |
C11—C1—V1 | 106.54 (11) | C40'—C41'—H41C | 108.5 |
C2—C1—H1 | 118.5 (12) | K1—C41'—H41C | 160.8 |
C11—C1—H1 | 115.0 (12) | O4'—C41'—H41D | 108.5 |
V1—C1—H1 | 120.2 (12) | C40'—C41'—H41D | 108.5 |
C3—C2—C1 | 116.15 (17) | K1—C41'—H41D | 74.7 |
C3—C2—V1 | 72.81 (10) | H41C—C41'—H41D | 107.5 |
C1—C2—V1 | 76.08 (10) | C42'—O4'—C41' | 112.6 (8) |
C3—C2—H2 | 122.3 (11) | C42'—O4'—K1 | 122.2 (7) |
C1—C2—H2 | 121.5 (11) | C41'—O4'—K1 | 101.3 (4) |
V1—C2—H2 | 123.0 (11) | O4'—C42'—H42D | 109.5 |
C2—C3—C4 | 116.77 (17) | O4'—C42'—H42E | 109.5 |
C2—C3—V1 | 70.13 (10) | H42D—C42'—H42E | 109.5 |
C4—C3—V1 | 79.04 (11) | O4'—C42'—H42F | 109.5 |
C2—C3—H3 | 121.5 (12) | H42D—C42'—H42F | 109.5 |
C4—C3—H3 | 121.7 (12) | H42E—C42'—H42F | 109.5 |
V1—C3—H3 | 121.7 (12) | O5—C43—H43A | 109.5 |
C3—C4—C12 | 121.42 (16) | O5—C43—H43B | 109.5 |
C3—C4—V1 | 65.70 (10) | H43A—C43—H43B | 109.5 |
C12—C4—V1 | 103.68 (11) | O5—C43—H43C | 109.5 |
C3—C4—H4 | 117.9 (12) | H43A—C43—H43C | 109.5 |
C12—C4—H4 | 117.6 (12) | H43B—C43—H43C | 109.5 |
V1—C4—H4 | 116.7 (12) | C44—O5—C43 | 110.8 (3) |
C6—C5—C13 | 121.5 (2) | C44—O5—K1 | 119.4 (2) |
C6—C5—H5 | 119.2 | C43—O5—K1 | 121.1 (3) |
C13—C5—H5 | 119.2 | O5—C44—C45 | 107.9 (3) |
C5—C6—C7 | 119.8 (2) | O5—C44—H44A | 110.1 |
C5—C6—H6 | 120.1 | C45—C44—H44A | 110.1 |
C7—C6—H6 | 120.1 | O5—C44—H44B | 110.1 |
C8—C7—C6 | 120.59 (19) | C45—C44—H44B | 110.1 |
C8—C7—H7 | 119.7 | H44A—C44—H44B | 108.4 |
C6—C7—H7 | 119.7 | O6—C45—C44 | 113.0 (3) |
C7—C8—C14 | 121.1 (2) | O6—C45—H45A | 109.0 |
C7—C8—H8 | 119.5 | C44—C45—H45A | 109.0 |
C14—C8—H8 | 119.5 | O6—C45—H45B | 109.0 |
C11—C9—C14 | 122.04 (16) | C44—C45—H45B | 109.0 |
C11—C9—H9 | 119.0 | H45A—C45—H45B | 107.8 |
C14—C9—H9 | 119.0 | C45—O6—C46 | 113.0 (4) |
C12—C10—C13 | 121.88 (17) | C45—O6—K1 | 104.6 (2) |
C12—C10—H10 | 119.1 | C46—O6—K1 | 128.0 (4) |
C13—C10—H10 | 119.1 | O6—C46—H46A | 109.5 |
C9—C11—C12 | 119.19 (16) | O6—C46—H46B | 109.5 |
C9—C11—C1 | 125.97 (16) | H46A—C46—H46B | 109.5 |
C12—C11—C1 | 114.80 (15) | O6—C46—H46C | 109.5 |
C10—C12—C11 | 119.57 (16) | H46A—C46—H46C | 109.5 |
C10—C12—C4 | 125.22 (16) | H46B—C46—H46C | 109.5 |
C11—C12—C4 | 115.15 (15) | O5'—C43'—H43D | 109.5 |
C5—C13—C10 | 123.00 (18) | O5'—C43'—H43E | 109.5 |
C5—C13—C14 | 118.40 (17) | H43D—C43'—H43E | 109.5 |
C10—C13—C14 | 118.60 (16) | O5'—C43'—H43F | 109.5 |
C8—C14—C9 | 122.70 (18) | H43D—C43'—H43F | 109.5 |
C8—C14—C13 | 118.64 (18) | H43E—C43'—H43F | 109.5 |
C9—C14—C13 | 118.66 (16) | C44'—O5'—C43' | 109.3 (9) |
C16—C15—C25 | 117.82 (15) | C44'—O5'—K1 | 114.8 (7) |
C16—C15—V1 | 66.07 (10) | C43'—O5'—K1 | 123.4 (8) |
C25—C15—V1 | 110.71 (11) | O5'—C44'—C45' | 107.0 (11) |
C16—C15—H15 | 117.8 (12) | O5'—C44'—H44C | 110.3 |
C25—C15—H15 | 113.8 (12) | C45'—C44'—H44C | 110.3 |
V1—C15—H15 | 122.8 (12) | O5'—C44'—H44D | 110.3 |
C17—C16—C15 | 114.26 (16) | C45'—C44'—H44D | 110.3 |
C17—C16—V1 | 72.58 (10) | H44C—C44'—H44D | 108.6 |
C15—C16—V1 | 76.46 (10) | O6'—C45'—C44' | 106.7 (11) |
C17—C16—H16 | 123.0 (12) | O6'—C45'—H45C | 110.4 |
C15—C16—H16 | 122.5 (12) | C44'—C45'—H45C | 110.4 |
V1—C16—H16 | 123.3 (12) | O6'—C45'—H45D | 110.4 |
C16—C17—C18 | 117.42 (16) | C44'—C45'—H45D | 110.4 |
C16—C17—V1 | 70.06 (10) | H45C—C45'—H45D | 108.6 |
C18—C17—V1 | 77.87 (10) | C46'—O6'—C45' | 113.9 (12) |
C16—C17—H17 | 123.1 (12) | C46'—O6'—K1 | 117.1 (11) |
C18—C17—H17 | 119.5 (11) | C45'—O6'—K1 | 111.8 (7) |
V1—C17—H17 | 121.7 (12) | O6'—C46'—H46D | 109.5 |
C17—C18—C26 | 117.33 (15) | O6'—C46'—H46E | 109.5 |
C17—C18—V1 | 65.92 (10) | H46D—C46'—H46E | 109.5 |
C26—C18—V1 | 109.43 (11) | O6'—C46'—H46F | 109.5 |
C17—C18—H18 | 116.4 (11) | H46D—C46'—H46F | 109.5 |
C26—C18—H18 | 118.8 (12) | H46E—C46'—H46F | 109.5 |
V1—C18—H18 | 117.5 (11) | O7—C47—H47A | 109.5 |
C20—C19—C27 | 121.69 (18) | O7—C47—H47B | 109.5 |
C20—C19—H19 | 119.2 | H47A—C47—H47B | 109.5 |
C27—C19—H19 | 119.2 | O7—C47—H47C | 109.5 |
C19—C20—C21 | 120.26 (18) | H47A—C47—H47C | 109.5 |
C19—C20—H20 | 119.9 | H47B—C47—H47C | 109.5 |
C21—C20—H20 | 119.9 | C47—O7—C48 | 111.6 (5) |
C22—C21—C20 | 119.75 (18) | C47—O7—K1 | 135.2 (4) |
C22—C21—H21 | 120.1 | C48—O7—K1 | 113.2 (3) |
C20—C21—H21 | 120.1 | C49—C48—O7 | 111.5 (5) |
C21—C22—C28 | 121.57 (18) | C49—C48—H48A | 109.3 |
C21—C22—H22 | 119.2 | O7—C48—H48A | 109.3 |
C28—C22—H22 | 119.2 | C49—C48—H48B | 109.3 |
C25—C23—C28 | 122.12 (16) | O7—C48—H48B | 109.3 |
C25—C23—H23 | 118.9 | H48A—C48—H48B | 108.0 |
C28—C23—H23 | 118.9 | C48—C49—O8 | 114.0 (5) |
C26—C24—C27 | 121.85 (16) | C48—C49—H49A | 108.8 |
C26—C24—H24 | 119.1 | O8—C49—H49A | 108.8 |
C27—C24—H24 | 119.1 | C48—C49—H49B | 108.8 |
C23—C25—C26 | 119.42 (16) | O8—C49—H49B | 108.8 |
C23—C25—C15 | 125.65 (15) | H49A—C49—H49B | 107.7 |
C26—C25—C15 | 114.89 (15) | C50—O8—C49 | 112.8 (5) |
C24—C26—C25 | 119.49 (16) | C50—O8—K1 | 141.2 (4) |
C24—C26—C18 | 126.41 (15) | C49—O8—K1 | 99.0 (3) |
C25—C26—C18 | 114.09 (15) | O8—C50—H50A | 109.5 |
C19—C27—C28 | 117.83 (16) | O8—C50—H50B | 109.5 |
C19—C27—C24 | 123.45 (16) | H50A—C50—H50B | 109.5 |
C28—C27—C24 | 118.72 (16) | O8—C50—H50C | 109.5 |
C22—C28—C27 | 118.87 (17) | H50A—C50—H50C | 109.5 |
C22—C28—C23 | 122.80 (16) | H50B—C50—H50C | 109.5 |
C27—C28—C23 | 118.32 (16) | O7'—C47'—H47D | 109.5 |
P1—C29—H29A | 109.5 | O7'—C47'—H47E | 109.5 |
P1—C29—H29B | 109.5 | H47D—C47'—H47E | 109.5 |
H29A—C29—H29B | 109.5 | O7'—C47'—H47F | 109.5 |
P1—C29—H29C | 109.5 | H47D—C47'—H47F | 109.5 |
H29A—C29—H29C | 109.5 | H47E—C47'—H47F | 109.5 |
H29B—C29—H29C | 109.5 | C47'—O7'—C48' | 113.0 (9) |
P1—C30—H30A | 109.5 | C47'—O7'—K1 | 122.1 (8) |
P1—C30—H30B | 109.5 | C48'—O7'—K1 | 106.4 (6) |
H30A—C30—H30B | 109.5 | O7'—C48'—C49' | 111.5 (8) |
P1—C30—H30C | 109.5 | O7'—C48'—K1 | 50.7 (5) |
H30A—C30—H30C | 109.5 | C49'—C48'—K1 | 82.7 (5) |
H30B—C30—H30C | 109.5 | O7'—C48'—H48C | 109.3 |
C32—C31—P1 | 112.62 (14) | C49'—C48'—H48C | 109.3 |
C32—C31—H31A | 109.1 | K1—C48'—H48C | 81.7 |
P1—C31—H31A | 109.1 | O7'—C48'—H48D | 109.3 |
C32—C31—H31B | 109.1 | C49'—C48'—H48D | 109.3 |
P1—C31—H31B | 109.1 | K1—C48'—H48D | 160.0 |
H31A—C31—H31B | 107.8 | H48C—C48'—H48D | 108.0 |
C31—C32—P2 | 111.34 (14) | O8'—C49'—C48' | 116.2 (7) |
C31—C32—H32A | 109.4 | O8'—C49'—H49C | 108.2 |
P2—C32—H32A | 109.4 | C48'—C49'—H49C | 108.2 |
C31—C32—H32B | 109.4 | O8'—C49'—H49D | 108.2 |
P2—C32—H32B | 109.4 | C48'—C49'—H49D | 108.2 |
H32A—C32—H32B | 108.0 | H49C—C49'—H49D | 107.4 |
P2—C33—H33A | 109.5 | C50'—O8'—C49' | 116.9 (7) |
P2—C33—H33B | 109.5 | C50'—O8'—K1 | 124.6 (5) |
H33A—C33—H33B | 109.5 | C49'—O8'—K1 | 115.7 (5) |
P2—C33—H33C | 109.5 | O8'—C50'—H50D | 109.5 |
H33A—C33—H33C | 109.5 | O8'—C50'—H50E | 109.5 |
H33B—C33—H33C | 109.5 | H50D—C50'—H50E | 109.5 |
P2—C34—H34A | 109.5 | O8'—C50'—H50F | 109.5 |
P2—C34—H34B | 109.5 | H50D—C50'—H50F | 109.5 |
H34A—C34—H34B | 109.5 | H50E—C50'—H50F | 109.5 |
P2—C34—H34C | 109.5 | | |
| | | |
C11—C1—C2—C3 | 33.9 (2) | V1—C18—C26—C25 | 34.13 (17) |
V1—C1—C2—C3 | −62.55 (14) | C20—C19—C27—C28 | −1.8 (3) |
C11—C1—C2—V1 | 96.42 (15) | C20—C19—C27—C24 | 179.25 (17) |
C1—C2—C3—C4 | −1.5 (2) | C26—C24—C27—C19 | 179.43 (16) |
V1—C2—C3—C4 | −65.87 (14) | C26—C24—C27—C28 | 0.5 (2) |
C1—C2—C3—V1 | 64.38 (14) | C21—C22—C28—C27 | −0.7 (3) |
C2—C3—C4—C12 | −30.7 (2) | C21—C22—C28—C23 | 178.06 (18) |
V1—C3—C4—C12 | −91.62 (15) | C19—C27—C28—C22 | 1.9 (2) |
C2—C3—C4—V1 | 60.95 (14) | C24—C27—C28—C22 | −179.12 (16) |
C13—C5—C6—C7 | 0.7 (3) | C19—C27—C28—C23 | −176.97 (16) |
C5—C6—C7—C8 | 0.2 (3) | C24—C27—C28—C23 | 2.1 (2) |
C6—C7—C8—C14 | −0.6 (3) | C25—C23—C28—C22 | 178.64 (17) |
C14—C9—C11—C12 | −1.5 (2) | C25—C23—C28—C27 | −2.6 (3) |
C14—C9—C11—C1 | 176.11 (16) | C29—P1—C31—C32 | −133.07 (18) |
C2—C1—C11—C9 | 148.50 (18) | C30—P1—C31—C32 | 129.34 (17) |
V1—C1—C11—C9 | −138.88 (15) | V1—P1—C31—C32 | −2.4 (2) |
C2—C1—C11—C12 | −33.8 (2) | P1—C31—C32—P2 | 28.7 (2) |
V1—C1—C11—C12 | 38.84 (17) | C34—P2—C32—C31 | −178.35 (15) |
C13—C10—C12—C11 | −1.8 (3) | C33—P2—C32—C31 | 80.79 (16) |
C13—C10—C12—C4 | −178.92 (16) | V1—P2—C32—C31 | −43.80 (16) |
C9—C11—C12—C10 | 2.7 (2) | C35—O1—C36—C37 | −173.2 (4) |
C1—C11—C12—C10 | −175.18 (15) | K1—O1—C36—C37 | −36.6 (5) |
C9—C11—C12—C4 | −179.87 (15) | O1—C36—C37—O2 | 64.4 (5) |
C1—C11—C12—C4 | 2.2 (2) | O1—C36—C37—K1 | 26.4 (4) |
C3—C4—C12—C10 | −152.89 (18) | C36—C37—O2—C38 | 168.5 (6) |
V1—C4—C12—C10 | 137.45 (15) | K1—C37—O2—C38 | −132.9 (6) |
C3—C4—C12—C11 | 29.9 (2) | C36—C37—O2—K1 | −58.6 (3) |
V1—C4—C12—C11 | −39.80 (16) | C35'—O1'—C36'—C37' | −173.7 (13) |
C6—C5—C13—C10 | 177.86 (18) | K1—O1'—C36'—C37' | −26.3 (18) |
C6—C5—C13—C14 | −1.3 (3) | O1'—C36'—C37'—O2' | 64.0 (18) |
C12—C10—C13—C5 | −179.47 (17) | C36'—C37'—O2'—C38' | 93.5 (18) |
C12—C10—C13—C14 | −0.3 (3) | C36'—C37'—O2'—K1 | −66.0 (11) |
C7—C8—C14—C9 | −179.76 (17) | C39—O3—C40—C41 | −158.6 (4) |
C7—C8—C14—C13 | 0.1 (3) | K1—O3—C40—C41 | 68.0 (4) |
C11—C9—C14—C8 | 179.27 (16) | O3—C40—C41—O4 | −69.2 (5) |
C11—C9—C14—C13 | −0.6 (2) | C40—C41—O4—C42 | 168.4 (4) |
C5—C13—C14—C8 | 0.8 (2) | C40—C41—O4—K1 | 29.7 (6) |
C10—C13—C14—C8 | −178.33 (16) | C39'—O3'—C40'—C41' | 176.3 (6) |
C5—C13—C14—C9 | −179.31 (16) | K1—O3'—C40'—C41' | −10.5 (8) |
C10—C13—C14—C9 | 1.5 (2) | O3'—C40'—C41'—O4' | 56.0 (8) |
C25—C15—C16—C17 | −38.2 (2) | O3'—C40'—C41'—K1 | 7.5 (6) |
V1—C15—C16—C17 | 63.50 (13) | C40'—C41'—O4'—C42' | 64.6 (10) |
C25—C15—C16—V1 | −101.73 (14) | K1—C41'—O4'—C42' | 132.2 (8) |
C15—C16—C17—C18 | −1.9 (2) | C40'—C41'—O4'—K1 | −67.6 (6) |
V1—C16—C17—C18 | 63.89 (15) | C43—O5—C44—C45 | 179.5 (4) |
C15—C16—C17—V1 | −65.76 (14) | K1—O5—C44—C45 | −32.5 (4) |
C16—C17—C18—C26 | 40.6 (2) | O5—C44—C45—O6 | 65.5 (4) |
V1—C17—C18—C26 | 100.32 (14) | C44—C45—O6—C46 | 83.0 (5) |
C16—C17—C18—V1 | −59.71 (14) | C44—C45—O6—K1 | −60.4 (3) |
C27—C19—C20—C21 | 0.5 (3) | C43'—O5'—C44'—C45' | 169.9 (12) |
C19—C20—C21—C22 | 0.8 (3) | K1—O5'—C44'—C45' | −46.5 (14) |
C20—C21—C22—C28 | −0.6 (3) | O5'—C44'—C45'—O6' | 70.8 (15) |
C28—C23—C25—C26 | 0.6 (3) | C44'—C45'—O6'—C46' | 165.8 (15) |
C28—C23—C25—C15 | −177.06 (16) | C44'—C45'—O6'—K1 | −58.5 (13) |
C16—C15—C25—C23 | −142.65 (18) | C47—O7—C48—C49 | 169.3 (6) |
V1—C15—C25—C23 | 144.26 (15) | K1—O7—C48—C49 | −11.8 (7) |
C16—C15—C25—C26 | 39.6 (2) | O7—C48—C49—O8 | 61.1 (8) |
V1—C15—C25—C26 | −33.46 (17) | C48—C49—O8—C50 | 85.0 (6) |
C27—C24—C26—C25 | −2.5 (2) | C48—C49—O8—K1 | −72.3 (6) |
C27—C24—C26—C18 | 178.68 (16) | C47'—O7'—C48'—C49' | −163.4 (11) |
C23—C25—C26—C24 | 2.0 (2) | K1—O7'—C48'—C49' | 60.1 (10) |
C15—C25—C26—C24 | 179.87 (15) | C47'—O7'—C48'—K1 | 136.5 (15) |
C23—C25—C26—C18 | −179.05 (15) | O7'—C48'—C49'—O8' | −53.1 (11) |
C15—C25—C26—C18 | −1.2 (2) | K1—C48'—C49'—O8' | −10.6 (6) |
C17—C18—C26—C24 | 140.74 (18) | C48'—C49'—O8'—C50' | 177.1 (8) |
V1—C18—C26—C24 | −147.00 (15) | C48'—C49'—O8'—K1 | 14.8 (9) |
C17—C18—C26—C25 | −38.1 (2) | | |
(µ
3-
η6:
η6:
η6-Anthracene)(µ
2-
η6:
η6-anthracene)tris(tetrahydrofuran)sodiumdivanadium (8)
top
Crystal data top
[NaV2(C14H10)2(C4H8O)3] | Z = 2 |
Mr = 697.62 | F(000) = 730 |
Triclinic, P1 | Dx = 1.430 Mg m−3 |
a = 10.9951 (16) Å | Mo Kα radiation, λ = 0.71073 Å |
b = 12.0777 (18) Å | Cell parameters from 2463 reflections |
c = 13.502 (2) Å | θ = 1.6–27.5° |
α = 78.594 (3)° | µ = 0.63 mm−1 |
β = 68.517 (3)° | T = 173 K |
γ = 78.738 (3)° | Block, red-brown |
V = 1620.6 (4) Å3 | 0.30 × 0.30 × 0.20 mm |
Data collection top
Siemens SMART CCD platform diffractometer | 4598 reflections with I > 2σ(I) |
Radiation source: normal-focus sealed tube | Rint = 0.054 |
ω scans | θmax = 27.5°, θmin = 1.6° |
Absorption correction: multi-scan (SADABS; Sheldrick, 1996) | h = −14→14 |
Tmin = 0.834, Tmax = 0.884 | k = −15→15 |
19641 measured reflections | l = −17→17 |
7405 independent reflections | |
Refinement top
Refinement on F2 | Primary atom site location: structure-invariant direct methods |
Least-squares matrix: full | Secondary atom site location: difference Fourier map |
R[F2 > 2σ(F2)] = 0.044 | Hydrogen site location: mixed |
wR(F2) = 0.119 | H atoms treated by a mixture of independent and constrained refinement |
S = 1.02 | w = 1/[σ2(Fo2) + (0.0492P)2 + 0.2398P] where P = (Fo2 + 2Fc2)/3 |
7405 reflections | (Δ/σ)max = 0.001 |
631 parameters | Δρmax = 0.42 e Å−3 |
381 restraints | Δρmin = −0.29 e Å−3 |
Special details top
Geometry. All esds (except the esd in the dihedral angle between two l.s. planes)
are estimated using the full covariance matrix. The cell esds are taken
into account individually in the estimation of esds in distances, angles
and torsion angles; correlations between esds in cell parameters are only
used when they are defined by crystal symmetry. An approximate (isotropic)
treatment of cell esds is used for estimating esds involving l.s. planes. |
Refinement. The three THF ligands are modeled as disordered over two
positions (0.58 (1):0.42 (1)). Analogous bond lengths and
angles were restrained to be similar. Anisotropic displacement
parameters for proximal atoms were restrained to be similar
and restrained toward the expected motion relative to bond
direction. |
Fractional atomic coordinates and isotropic or equivalent isotropic displacement parameters (Å2) top | x | y | z | Uiso*/Ueq | Occ. (<1) |
V1 | 0.08628 (4) | 0.56776 (4) | 0.72351 (3) | 0.02182 (13) | |
V2 | 0.53909 (4) | 0.49681 (4) | 0.75667 (3) | 0.02019 (12) | |
C1 | 0.0427 (3) | 0.4023 (2) | 0.8257 (2) | 0.0292 (6) | |
H1 | 0.007 (2) | 0.389 (2) | 0.897 (2) | 0.017 (7)* | |
C2 | −0.0390 (3) | 0.4324 (3) | 0.7611 (2) | 0.0317 (7) | |
H2 | −0.126 (3) | 0.446 (2) | 0.796 (2) | 0.039 (9)* | |
C3 | 0.0187 (3) | 0.4572 (2) | 0.6492 (2) | 0.0296 (6) | |
H3 | −0.037 (3) | 0.483 (2) | 0.606 (2) | 0.027 (7)* | |
C4 | 0.1567 (3) | 0.4504 (2) | 0.6011 (2) | 0.0260 (6) | |
H4 | 0.194 (3) | 0.473 (2) | 0.527 (2) | 0.030 (8)* | |
C5 | 0.6035 (3) | 0.3786 (2) | 0.6336 (2) | 0.0246 (6) | |
H5 | 0.644 (3) | 0.395 (2) | 0.562 (2) | 0.027 (7)* | |
C6 | 0.6852 (3) | 0.3502 (2) | 0.6978 (2) | 0.0286 (6) | |
H6 | 0.775 (3) | 0.358 (2) | 0.662 (2) | 0.031 (8)* | |
C7 | 0.6283 (3) | 0.3272 (2) | 0.8101 (2) | 0.0300 (7) | |
H7 | 0.682 (3) | 0.314 (2) | 0.850 (2) | 0.032 (8)* | |
C8 | 0.4899 (3) | 0.3326 (2) | 0.8588 (2) | 0.0263 (6) | |
H8 | 0.449 (2) | 0.320 (2) | 0.934 (2) | 0.021 (7)* | |
C9 | 0.2670 (3) | 0.3595 (2) | 0.8409 (2) | 0.0249 (6) | |
H9 | 0.233 (3) | 0.341 (2) | 0.917 (2) | 0.034 (8)* | |
C10 | 0.3810 (3) | 0.4047 (2) | 0.6176 (2) | 0.0221 (6) | |
H10 | 0.421 (3) | 0.422 (2) | 0.543 (2) | 0.034 (8)* | |
C11 | 0.1840 (3) | 0.3876 (2) | 0.7794 (2) | 0.0236 (6) | |
C12 | 0.2438 (2) | 0.4121 (2) | 0.6623 (2) | 0.0216 (5) | |
C13 | 0.4640 (2) | 0.3772 (2) | 0.6794 (2) | 0.0205 (5) | |
C14 | 0.4046 (2) | 0.3528 (2) | 0.7959 (2) | 0.0222 (6) | |
C15 | 0.0197 (3) | 0.6861 (2) | 0.8464 (2) | 0.0277 (6) | |
H15 | −0.023 (3) | 0.667 (2) | 0.921 (2) | 0.034 (8)* | |
C16 | −0.0615 (3) | 0.7129 (2) | 0.7815 (2) | 0.0303 (6) | |
H16 | −0.151 (3) | 0.711 (2) | 0.814 (2) | 0.027 (7)* | |
C17 | −0.0029 (3) | 0.7356 (2) | 0.6691 (2) | 0.0298 (6) | |
H17 | −0.057 (2) | 0.748 (2) | 0.626 (2) | 0.023 (7)* | |
C18 | 0.1352 (3) | 0.7317 (2) | 0.6217 (2) | 0.0276 (6) | |
H18 | 0.169 (3) | 0.742 (2) | 0.549 (2) | 0.037 (9)* | |
C19 | 0.5821 (2) | 0.6649 (2) | 0.6570 (2) | 0.0230 (6) | |
H19 | 0.626 (2) | 0.680 (2) | 0.578 (2) | 0.020 (7)* | |
C20 | 0.6628 (3) | 0.6321 (2) | 0.7222 (2) | 0.0265 (6) | |
H20 | 0.749 (3) | 0.627 (2) | 0.690 (2) | 0.023 (7)* | |
C21 | 0.6050 (3) | 0.6063 (2) | 0.8343 (2) | 0.0258 (6) | |
H21 | 0.659 (3) | 0.576 (2) | 0.881 (2) | 0.032 (8)* | |
C22 | 0.4656 (3) | 0.6127 (2) | 0.8820 (2) | 0.0237 (6) | |
H22 | 0.429 (2) | 0.592 (2) | 0.957 (2) | 0.024 (7)* | |
C23 | 0.2426 (2) | 0.6624 (2) | 0.8641 (2) | 0.0222 (6) | |
H23 | 0.202 (3) | 0.643 (2) | 0.936 (2) | 0.041 (9)* | |
C24 | 0.3565 (2) | 0.7135 (2) | 0.6414 (2) | 0.0212 (5) | |
H24 | 0.399 (2) | 0.7279 (19) | 0.5685 (19) | 0.013 (6)* | |
C25 | 0.1589 (2) | 0.6879 (2) | 0.8023 (2) | 0.0223 (6) | |
C26 | 0.2197 (2) | 0.7136 (2) | 0.6848 (2) | 0.0208 (5) | |
C27 | 0.4412 (2) | 0.6795 (2) | 0.70301 (19) | 0.0198 (5) | |
C28 | 0.3802 (2) | 0.6525 (2) | 0.8198 (2) | 0.0209 (5) | |
Na1 | 0.27079 (12) | 0.89469 (9) | 0.76847 (10) | 0.0401 (3) | |
O1 | 0.1991 (18) | 0.9538 (11) | 0.9328 (8) | 0.060 (3) | 0.580 (10) |
C29 | 0.169 (2) | 1.0690 (11) | 0.9583 (15) | 0.057 (3) | 0.580 (10) |
H29A | 0.078566 | 1.082458 | 1.010707 | 0.068* | 0.580 (10) |
H29B | 0.176740 | 1.125297 | 0.892846 | 0.068* | 0.580 (10) |
C30 | 0.272 (2) | 1.0759 (14) | 1.0064 (19) | 0.056 (4) | 0.580 (10) |
H30A | 0.234756 | 1.125798 | 1.063446 | 0.067* | 0.580 (10) |
H30B | 0.349521 | 1.106656 | 0.950440 | 0.067* | 0.580 (10) |
C31 | 0.3102 (16) | 0.9545 (14) | 1.0530 (14) | 0.049 (3) | 0.580 (10) |
H31A | 0.406906 | 0.932391 | 1.024654 | 0.059* | 0.580 (10) |
H31B | 0.280768 | 0.946222 | 1.132416 | 0.059* | 0.580 (10) |
C32 | 0.2399 (10) | 0.8828 (8) | 1.0171 (9) | 0.047 (2) | 0.580 (10) |
H32A | 0.299878 | 0.814436 | 0.990053 | 0.056* | 0.580 (10) |
H32B | 0.162303 | 0.857756 | 1.077676 | 0.056* | 0.580 (10) |
O2 | 0.1282 (9) | 1.0339 (8) | 0.7084 (9) | 0.054 (3) | 0.580 (10) |
C33 | 0.0264 (12) | 1.0140 (9) | 0.6742 (9) | 0.066 (3) | 0.580 (10) |
H33A | 0.048004 | 0.937479 | 0.651140 | 0.079* | 0.580 (10) |
H33B | −0.058417 | 1.016244 | 0.734780 | 0.079* | 0.580 (10) |
C34 | 0.0143 (10) | 1.0980 (7) | 0.5879 (7) | 0.067 (3) | 0.580 (10) |
H34A | −0.079125 | 1.130466 | 0.600454 | 0.080* | 0.580 (10) |
H34B | 0.049925 | 1.065439 | 0.519444 | 0.080* | 0.580 (10) |
C35 | 0.0939 (15) | 1.1874 (11) | 0.5852 (11) | 0.070 (3) | 0.580 (10) |
H35A | 0.170068 | 1.192476 | 0.517405 | 0.084* | 0.580 (10) |
H35B | 0.038842 | 1.262827 | 0.590339 | 0.084* | 0.580 (10) |
C36 | 0.1386 (9) | 1.1535 (6) | 0.6757 (7) | 0.048 (2) | 0.580 (10) |
H36A | 0.083063 | 1.197446 | 0.735028 | 0.058* | 0.580 (10) |
H36B | 0.231147 | 1.167099 | 0.655113 | 0.058* | 0.580 (10) |
O3 | 0.4576 (9) | 0.9738 (10) | 0.7301 (11) | 0.064 (3) | 0.580 (10) |
C37 | 0.5584 (9) | 0.9235 (8) | 0.7750 (10) | 0.052 (2) | 0.580 (10) |
H37A | 0.554821 | 0.840762 | 0.798306 | 0.062* | 0.580 (10) |
H37B | 0.548632 | 0.959973 | 0.837519 | 0.062* | 0.580 (10) |
C38 | 0.6847 (10) | 0.9443 (13) | 0.6858 (15) | 0.054 (3) | 0.580 (10) |
H38A | 0.709339 | 0.890827 | 0.632564 | 0.064* | 0.580 (10) |
H38B | 0.758065 | 0.939665 | 0.712981 | 0.064* | 0.580 (10) |
C39 | 0.6450 (12) | 1.0641 (13) | 0.6404 (14) | 0.083 (4) | 0.580 (10) |
H39A | 0.665851 | 1.119781 | 0.674646 | 0.099* | 0.580 (10) |
H39B | 0.692158 | 1.077560 | 0.561881 | 0.099* | 0.580 (10) |
C40 | 0.5005 (10) | 1.0753 (9) | 0.6639 (11) | 0.085 (4) | 0.580 (10) |
H40A | 0.455061 | 1.142220 | 0.701515 | 0.102* | 0.580 (10) |
H40B | 0.481100 | 1.085039 | 0.596423 | 0.102* | 0.580 (10) |
O1' | 0.175 (3) | 0.9621 (17) | 0.9309 (11) | 0.070 (5) | 0.420 (10) |
C29' | 0.189 (3) | 1.0776 (16) | 0.935 (2) | 0.069 (5) | 0.420 (10) |
H29C | 0.102784 | 1.126495 | 0.950671 | 0.082* | 0.420 (10) |
H29D | 0.250127 | 1.110110 | 0.865464 | 0.082* | 0.420 (10) |
C30' | 0.244 (3) | 1.0705 (17) | 1.024 (2) | 0.052 (5) | 0.420 (10) |
H30C | 0.179348 | 1.108779 | 1.083790 | 0.063* | 0.420 (10) |
H30D | 0.325933 | 1.106869 | 0.996552 | 0.063* | 0.420 (10) |
C31' | 0.274 (2) | 0.9433 (18) | 1.060 (2) | 0.057 (4) | 0.420 (10) |
H31C | 0.365653 | 0.912585 | 1.020016 | 0.068* | 0.420 (10) |
H31D | 0.259401 | 0.927654 | 1.138054 | 0.068* | 0.420 (10) |
C32' | 0.1756 (15) | 0.8944 (14) | 1.0333 (14) | 0.062 (4) | 0.420 (10) |
H32C | 0.204088 | 0.812590 | 1.025608 | 0.074* | 0.420 (10) |
H32D | 0.087257 | 0.903202 | 1.089242 | 0.074* | 0.420 (10) |
O2' | 0.1671 (12) | 1.0333 (12) | 0.6809 (13) | 0.048 (3) | 0.420 (10) |
C33' | 0.0325 (14) | 1.0216 (12) | 0.7146 (14) | 0.076 (5) | 0.420 (10) |
H33C | −0.008186 | 1.020425 | 0.793360 | 0.091* | 0.420 (10) |
H33D | 0.021911 | 0.949456 | 0.696160 | 0.091* | 0.420 (10) |
C34' | −0.0306 (11) | 1.1190 (12) | 0.6592 (15) | 0.105 (5) | 0.420 (10) |
H34C | −0.085142 | 1.173757 | 0.709262 | 0.126* | 0.420 (10) |
H34D | −0.087266 | 1.093717 | 0.627793 | 0.126* | 0.420 (10) |
C35' | 0.0807 (15) | 1.1718 (15) | 0.5731 (12) | 0.056 (4) | 0.420 (10) |
H35C | 0.103591 | 1.141360 | 0.504630 | 0.067* | 0.420 (10) |
H35D | 0.059470 | 1.255785 | 0.560872 | 0.067* | 0.420 (10) |
C36' | 0.1880 (12) | 1.1376 (10) | 0.6180 (11) | 0.059 (3) | 0.420 (10) |
H36C | 0.274542 | 1.131223 | 0.559597 | 0.071* | 0.420 (10) |
H36D | 0.186672 | 1.194719 | 0.662003 | 0.071* | 0.420 (10) |
O3' | 0.4465 (14) | 0.9929 (17) | 0.7010 (14) | 0.066 (3) | 0.420 (10) |
C37' | 0.5310 (18) | 0.9564 (17) | 0.7613 (14) | 0.075 (4) | 0.420 (10) |
H37C | 0.524437 | 0.875642 | 0.793156 | 0.090* | 0.420 (10) |
H37D | 0.505095 | 1.002678 | 0.820509 | 0.090* | 0.420 (10) |
C38' | 0.6698 (17) | 0.969 (2) | 0.689 (2) | 0.079 (6) | 0.420 (10) |
H38C | 0.719402 | 0.994028 | 0.727286 | 0.095* | 0.420 (10) |
H38D | 0.716865 | 0.896676 | 0.661893 | 0.095* | 0.420 (10) |
C39' | 0.6506 (19) | 1.058 (2) | 0.602 (2) | 0.110 (8) | 0.420 (10) |
H39C | 0.662653 | 1.133010 | 0.612767 | 0.132* | 0.420 (10) |
H39D | 0.714592 | 1.039358 | 0.531503 | 0.132* | 0.420 (10) |
C40' | 0.5145 (18) | 1.0586 (18) | 0.6062 (13) | 0.113 (7) | 0.420 (10) |
H40C | 0.469037 | 1.137818 | 0.603765 | 0.136* | 0.420 (10) |
H40D | 0.515939 | 1.027109 | 0.543352 | 0.136* | 0.420 (10) |
Atomic displacement parameters (Å2) top | U11 | U22 | U33 | U12 | U13 | U23 |
V1 | 0.0161 (2) | 0.0284 (3) | 0.0216 (2) | −0.00287 (19) | −0.00717 (19) | −0.00361 (19) |
V2 | 0.0172 (2) | 0.0220 (2) | 0.0229 (2) | −0.00241 (18) | −0.00867 (19) | −0.00321 (18) |
C1 | 0.0229 (15) | 0.0382 (17) | 0.0243 (15) | −0.0119 (12) | −0.0047 (12) | 0.0023 (13) |
C2 | 0.0202 (15) | 0.0396 (18) | 0.0358 (17) | −0.0089 (13) | −0.0080 (13) | −0.0046 (14) |
C3 | 0.0246 (15) | 0.0386 (17) | 0.0328 (16) | −0.0070 (13) | −0.0166 (13) | −0.0058 (13) |
C4 | 0.0242 (14) | 0.0341 (16) | 0.0220 (14) | −0.0067 (12) | −0.0084 (12) | −0.0051 (12) |
C5 | 0.0200 (14) | 0.0278 (15) | 0.0260 (15) | −0.0013 (11) | −0.0068 (12) | −0.0073 (12) |
C6 | 0.0189 (14) | 0.0264 (15) | 0.0400 (17) | 0.0000 (11) | −0.0093 (13) | −0.0081 (13) |
C7 | 0.0284 (16) | 0.0263 (15) | 0.0404 (18) | 0.0003 (12) | −0.0216 (14) | −0.0006 (13) |
C8 | 0.0265 (15) | 0.0263 (15) | 0.0246 (15) | −0.0029 (11) | −0.0101 (12) | 0.0024 (12) |
C9 | 0.0257 (14) | 0.0239 (14) | 0.0247 (15) | −0.0053 (11) | −0.0104 (12) | 0.0029 (11) |
C10 | 0.0241 (14) | 0.0222 (14) | 0.0220 (14) | −0.0038 (11) | −0.0081 (12) | −0.0062 (11) |
C11 | 0.0244 (14) | 0.0214 (13) | 0.0257 (14) | −0.0071 (11) | −0.0081 (11) | −0.0018 (11) |
C12 | 0.0219 (13) | 0.0207 (13) | 0.0249 (14) | −0.0047 (11) | −0.0095 (11) | −0.0047 (11) |
C13 | 0.0187 (13) | 0.0171 (13) | 0.0254 (14) | −0.0019 (10) | −0.0061 (11) | −0.0056 (10) |
C14 | 0.0239 (14) | 0.0164 (13) | 0.0278 (14) | −0.0047 (10) | −0.0120 (12) | 0.0020 (11) |
C15 | 0.0186 (14) | 0.0374 (17) | 0.0255 (15) | −0.0022 (12) | −0.0034 (12) | −0.0102 (13) |
C16 | 0.0156 (14) | 0.0367 (17) | 0.0372 (17) | 0.0010 (12) | −0.0076 (13) | −0.0093 (13) |
C17 | 0.0246 (15) | 0.0328 (16) | 0.0361 (17) | 0.0010 (12) | −0.0184 (14) | −0.0031 (13) |
C18 | 0.0242 (15) | 0.0321 (16) | 0.0276 (16) | −0.0010 (12) | −0.0131 (13) | −0.0008 (13) |
C19 | 0.0196 (13) | 0.0245 (14) | 0.0240 (14) | −0.0062 (11) | −0.0057 (12) | −0.0015 (11) |
C20 | 0.0163 (14) | 0.0301 (15) | 0.0331 (16) | −0.0070 (12) | −0.0063 (12) | −0.0047 (12) |
C21 | 0.0250 (14) | 0.0318 (15) | 0.0268 (15) | −0.0049 (12) | −0.0149 (12) | −0.0051 (12) |
C22 | 0.0248 (14) | 0.0287 (15) | 0.0207 (14) | −0.0051 (11) | −0.0096 (12) | −0.0053 (11) |
C23 | 0.0208 (14) | 0.0286 (15) | 0.0163 (13) | −0.0054 (11) | −0.0028 (11) | −0.0056 (11) |
C24 | 0.0214 (13) | 0.0232 (14) | 0.0190 (14) | −0.0035 (11) | −0.0069 (11) | −0.0021 (11) |
C25 | 0.0210 (13) | 0.0224 (14) | 0.0245 (14) | −0.0015 (11) | −0.0075 (11) | −0.0073 (11) |
C26 | 0.0194 (13) | 0.0186 (13) | 0.0236 (13) | 0.0001 (10) | −0.0075 (11) | −0.0031 (11) |
C27 | 0.0193 (13) | 0.0178 (13) | 0.0229 (13) | −0.0048 (10) | −0.0068 (11) | −0.0029 (10) |
C28 | 0.0235 (13) | 0.0206 (13) | 0.0228 (13) | −0.0044 (10) | −0.0105 (11) | −0.0060 (11) |
Na1 | 0.0517 (8) | 0.0255 (6) | 0.0508 (8) | −0.0077 (5) | −0.0257 (6) | −0.0042 (5) |
O1 | 0.122 (7) | 0.026 (3) | 0.053 (4) | 0.000 (3) | −0.060 (4) | −0.004 (3) |
C29 | 0.086 (6) | 0.029 (4) | 0.060 (7) | 0.002 (4) | −0.036 (6) | −0.005 (4) |
C30 | 0.055 (7) | 0.041 (5) | 0.072 (9) | −0.003 (4) | −0.020 (6) | −0.016 (5) |
C31 | 0.055 (7) | 0.049 (5) | 0.050 (5) | −0.010 (4) | −0.020 (5) | −0.015 (4) |
C32 | 0.079 (7) | 0.032 (3) | 0.041 (4) | −0.008 (4) | −0.037 (5) | 0.002 (3) |
O2 | 0.075 (6) | 0.031 (3) | 0.075 (7) | −0.020 (4) | −0.055 (6) | 0.017 (4) |
C33 | 0.077 (5) | 0.056 (5) | 0.090 (7) | −0.035 (4) | −0.054 (5) | 0.009 (4) |
C34 | 0.083 (6) | 0.074 (5) | 0.068 (5) | −0.041 (5) | −0.054 (5) | 0.017 (4) |
C35 | 0.123 (8) | 0.044 (4) | 0.072 (7) | −0.034 (5) | −0.064 (5) | 0.011 (4) |
C36 | 0.073 (6) | 0.031 (3) | 0.058 (5) | −0.014 (3) | −0.040 (4) | 0.001 (4) |
O3 | 0.037 (3) | 0.033 (4) | 0.125 (8) | −0.010 (3) | −0.040 (4) | 0.012 (4) |
C37 | 0.041 (4) | 0.032 (4) | 0.082 (6) | −0.003 (3) | −0.021 (3) | −0.009 (4) |
C38 | 0.034 (4) | 0.036 (4) | 0.081 (6) | 0.005 (3) | −0.008 (4) | −0.018 (4) |
C39 | 0.055 (5) | 0.045 (5) | 0.144 (13) | −0.027 (4) | −0.033 (7) | 0.015 (6) |
C40 | 0.052 (4) | 0.049 (4) | 0.147 (10) | −0.018 (4) | −0.041 (6) | 0.027 (6) |
O1' | 0.133 (11) | 0.040 (7) | 0.050 (6) | −0.019 (6) | −0.046 (6) | 0.003 (5) |
C29' | 0.123 (13) | 0.033 (6) | 0.064 (9) | −0.004 (7) | −0.051 (9) | −0.009 (6) |
C30' | 0.075 (13) | 0.028 (5) | 0.056 (8) | −0.011 (6) | −0.024 (9) | −0.005 (5) |
C31' | 0.078 (13) | 0.038 (6) | 0.064 (7) | −0.010 (7) | −0.038 (9) | 0.001 (5) |
C32' | 0.090 (10) | 0.050 (7) | 0.060 (7) | −0.019 (8) | −0.045 (8) | 0.008 (5) |
O2' | 0.052 (5) | 0.037 (4) | 0.055 (6) | −0.010 (4) | −0.023 (5) | 0.007 (3) |
C33' | 0.056 (6) | 0.045 (6) | 0.097 (10) | −0.002 (5) | −0.006 (7) | 0.016 (6) |
C34' | 0.056 (6) | 0.096 (9) | 0.137 (12) | −0.004 (6) | −0.037 (8) | 0.043 (9) |
C35' | 0.077 (7) | 0.066 (9) | 0.034 (5) | 0.007 (6) | −0.037 (5) | −0.013 (5) |
C36' | 0.071 (7) | 0.052 (6) | 0.068 (8) | −0.031 (6) | −0.044 (6) | 0.024 (6) |
O3' | 0.065 (6) | 0.047 (7) | 0.086 (7) | −0.013 (5) | −0.034 (4) | 0.014 (5) |
C37' | 0.078 (8) | 0.082 (11) | 0.062 (6) | −0.007 (8) | −0.028 (6) | −0.002 (7) |
C38' | 0.063 (7) | 0.087 (15) | 0.089 (9) | −0.011 (8) | −0.020 (7) | −0.028 (9) |
C39' | 0.065 (7) | 0.074 (10) | 0.131 (14) | −0.002 (7) | 0.009 (8) | 0.032 (10) |
C40' | 0.093 (8) | 0.112 (12) | 0.099 (11) | −0.024 (8) | −0.020 (9) | 0.052 (10) |
Geometric parameters (Å, º) top
V1—C17 | 2.184 (3) | Na1—O3' | 2.269 (10) |
V1—C3 | 2.192 (3) | Na1—O1 | 2.276 (8) |
V1—C16 | 2.196 (3) | Na1—O3 | 2.279 (7) |
V1—C2 | 2.206 (3) | Na1—O1' | 2.294 (12) |
V1—C18 | 2.213 (3) | Na1—O2 | 2.304 (7) |
V1—C4 | 2.214 (3) | O1—C32 | 1.437 (9) |
V1—C1 | 2.219 (3) | O1—C29 | 1.446 (10) |
V1—C15 | 2.230 (3) | C29—C30 | 1.519 (11) |
V1—C11 | 2.343 (3) | C29—H29A | 0.9900 |
V1—C12 | 2.347 (3) | C29—H29B | 0.9900 |
V1—C25 | 2.358 (2) | C30—C31 | 1.520 (10) |
V1—C26 | 2.369 (2) | C30—H30A | 0.9900 |
V2—C7 | 2.198 (3) | C30—H30B | 0.9900 |
V2—C20 | 2.200 (3) | C31—C32 | 1.512 (9) |
V2—C21 | 2.202 (3) | C31—H31A | 0.9900 |
V2—C6 | 2.204 (3) | C31—H31B | 0.9900 |
V2—C8 | 2.218 (3) | C32—H32A | 0.9900 |
V2—C22 | 2.229 (3) | C32—H32B | 0.9900 |
V2—C5 | 2.232 (3) | O2—C33 | 1.432 (10) |
V2—C19 | 2.233 (3) | O2—C36 | 1.439 (9) |
V2—C13 | 2.356 (2) | C33—C34 | 1.413 (9) |
V2—C14 | 2.357 (2) | C33—H33A | 0.9900 |
V2—C27 | 2.358 (2) | C33—H33B | 0.9900 |
V2—C28 | 2.361 (2) | C34—C35 | 1.505 (10) |
C1—C2 | 1.421 (4) | C34—H34A | 0.9900 |
C1—C11 | 1.436 (4) | C34—H34B | 0.9900 |
C1—H1 | 0.90 (2) | C35—C36 | 1.436 (10) |
C2—C3 | 1.402 (4) | C35—H35A | 0.9900 |
C2—H2 | 0.89 (3) | C35—H35B | 0.9900 |
C3—C4 | 1.407 (4) | C36—H36A | 0.9900 |
C3—H3 | 0.96 (3) | C36—H36B | 0.9900 |
C4—C12 | 1.439 (3) | O3—C40 | 1.417 (9) |
C4—H4 | 0.94 (3) | O3—C37 | 1.431 (8) |
C5—C6 | 1.417 (4) | C37—C38 | 1.495 (10) |
C5—C13 | 1.431 (3) | C37—H37A | 0.9900 |
C5—H5 | 0.91 (3) | C37—H37B | 0.9900 |
C6—C7 | 1.405 (4) | C38—C39 | 1.502 (12) |
C6—H6 | 0.94 (3) | C38—H38A | 0.9900 |
C7—C8 | 1.413 (4) | C38—H38B | 0.9900 |
C7—H7 | 0.90 (3) | C39—C40 | 1.486 (9) |
C8—C14 | 1.439 (4) | C39—H39A | 0.9900 |
C8—H8 | 0.94 (2) | C39—H39B | 0.9900 |
C9—C11 | 1.400 (3) | C40—H40A | 0.9900 |
C9—C14 | 1.402 (4) | C40—H40B | 0.9900 |
C9—H9 | 0.96 (3) | O1'—C29' | 1.448 (12) |
C10—C12 | 1.396 (3) | O1'—C32' | 1.462 (12) |
C10—C13 | 1.404 (3) | C29'—C30' | 1.509 (13) |
C10—H10 | 0.94 (3) | C29'—H29C | 0.9900 |
C11—C12 | 1.465 (3) | C29'—H29D | 0.9900 |
C13—C14 | 1.458 (3) | C30'—C31' | 1.526 (12) |
C15—C16 | 1.420 (4) | C30'—H30C | 0.9900 |
C15—C25 | 1.428 (3) | C30'—H30D | 0.9900 |
C15—H15 | 0.95 (3) | C31'—C32' | 1.507 (12) |
C16—C17 | 1.408 (4) | C31'—H31C | 0.9900 |
C16—H16 | 0.93 (3) | C31'—H31D | 0.9900 |
C17—C18 | 1.410 (4) | C32'—H32C | 0.9900 |
C17—H17 | 0.95 (3) | C32'—H32D | 0.9900 |
C18—C26 | 1.437 (4) | O2'—C36' | 1.381 (10) |
C18—H18 | 0.90 (3) | O2'—C33' | 1.408 (12) |
C19—C20 | 1.420 (4) | C33'—C34' | 1.462 (12) |
C19—C27 | 1.432 (3) | C33'—H33C | 0.9900 |
C19—H19 | 0.99 (2) | C33'—H33D | 0.9900 |
C20—C21 | 1.407 (4) | C34'—C35' | 1.492 (14) |
C20—H20 | 0.89 (3) | C34'—H34C | 0.9900 |
C21—C22 | 1.421 (4) | C34'—H34D | 0.9900 |
C21—H21 | 0.99 (3) | C35'—C36' | 1.471 (12) |
C22—C28 | 1.436 (3) | C35'—H35C | 0.9900 |
C22—H22 | 0.94 (2) | C35'—H35D | 0.9900 |
C23—C28 | 1.398 (3) | C36'—H36C | 0.9900 |
C23—C25 | 1.410 (3) | C36'—H36D | 0.9900 |
C23—Na1 | 2.872 (3) | O3'—C40' | 1.398 (11) |
C23—H23 | 0.91 (3) | O3'—C37' | 1.405 (11) |
C24—C26 | 1.400 (3) | C37'—C38' | 1.496 (13) |
C24—C27 | 1.417 (3) | C37'—H37C | 0.9900 |
C24—Na1 | 2.848 (3) | C37'—H37D | 0.9900 |
C24—H24 | 0.92 (2) | C38'—C39' | 1.477 (15) |
C25—C26 | 1.473 (3) | C38'—H38C | 0.9900 |
C25—Na1 | 2.880 (3) | C38'—H38D | 0.9900 |
C26—Na1 | 2.880 (3) | C39'—C40' | 1.475 (13) |
C27—C28 | 1.466 (3) | C39'—H39C | 0.9900 |
C27—Na1 | 2.974 (3) | C39'—H39D | 0.9900 |
C28—Na1 | 2.986 (3) | C40'—H40C | 0.9900 |
Na1—O2' | 2.227 (9) | C40'—H40D | 0.9900 |
| | | |
C17—V1—C3 | 101.19 (11) | C26—C24—H24 | 121.1 (15) |
C17—V1—C16 | 37.48 (10) | C27—C24—H24 | 114.9 (15) |
C3—V1—C16 | 113.51 (11) | Na1—C24—H24 | 120.2 (15) |
C17—V1—C2 | 113.74 (11) | C23—C25—C15 | 123.9 (2) |
C3—V1—C2 | 37.19 (10) | C23—C25—C26 | 117.9 (2) |
C16—V1—C2 | 101.40 (11) | C15—C25—C26 | 118.2 (2) |
C17—V1—C18 | 37.40 (10) | C23—C25—V1 | 130.64 (18) |
C3—V1—C18 | 113.62 (11) | C15—C25—V1 | 67.03 (14) |
C16—V1—C18 | 67.27 (11) | C26—C25—V1 | 72.26 (14) |
C2—V1—C18 | 143.85 (11) | C23—C25—Na1 | 75.48 (15) |
C17—V1—C4 | 113.30 (11) | C15—C25—Na1 | 121.37 (18) |
C3—V1—C4 | 37.25 (10) | C26—C25—Na1 | 75.19 (14) |
C16—V1—C4 | 143.51 (10) | V1—C25—Na1 | 145.53 (11) |
C2—V1—C4 | 66.89 (11) | C24—C26—C18 | 124.2 (2) |
C18—V1—C4 | 101.11 (11) | C24—C26—C25 | 118.1 (2) |
C17—V1—C1 | 144.04 (11) | C18—C26—C25 | 117.6 (2) |
C3—V1—C1 | 67.16 (11) | C24—C26—V1 | 132.04 (18) |
C16—V1—C1 | 113.74 (11) | C18—C26—V1 | 65.89 (15) |
C2—V1—C1 | 37.47 (10) | C25—C26—V1 | 71.44 (14) |
C18—V1—C1 | 178.49 (10) | C24—C26—Na1 | 74.60 (14) |
C4—V1—C1 | 78.74 (11) | C18—C26—Na1 | 123.10 (17) |
C17—V1—C15 | 67.13 (11) | C25—C26—Na1 | 75.18 (14) |
C3—V1—C15 | 143.93 (10) | V1—C26—Na1 | 144.75 (11) |
C16—V1—C15 | 37.42 (10) | C24—C27—C19 | 123.6 (2) |
C2—V1—C15 | 114.05 (11) | C24—C27—C28 | 117.7 (2) |
C18—V1—C15 | 78.56 (11) | C19—C27—C28 | 118.6 (2) |
C4—V1—C15 | 178.81 (10) | C24—C27—V2 | 130.64 (17) |
C1—V1—C15 | 101.56 (11) | C19—C27—V2 | 67.11 (14) |
C17—V1—C11 | 179.20 (10) | C28—C27—V2 | 72.01 (14) |
C3—V1—C11 | 78.54 (10) | C24—C27—Na1 | 71.05 (14) |
C16—V1—C11 | 143.32 (10) | C19—C27—Na1 | 125.63 (16) |
C2—V1—C11 | 66.50 (10) | C28—C27—Na1 | 76.24 (14) |
C18—V1—C11 | 142.02 (10) | V2—C27—Na1 | 147.57 (10) |
C4—V1—C11 | 66.04 (10) | C23—C28—C22 | 123.5 (2) |
C1—V1—C11 | 36.55 (9) | C23—C28—C27 | 118.5 (2) |
C15—V1—C11 | 113.53 (10) | C22—C28—C27 | 117.9 (2) |
C17—V1—C12 | 142.79 (10) | C23—C28—V2 | 131.10 (18) |
C3—V1—C12 | 66.48 (9) | C22—C28—V2 | 66.82 (14) |
C16—V1—C12 | 179.71 (11) | C27—C28—V2 | 71.80 (14) |
C2—V1—C12 | 78.42 (10) | C23—C28—Na1 | 71.68 (15) |
C18—V1—C12 | 113.01 (10) | C22—C28—Na1 | 126.07 (17) |
C4—V1—C12 | 36.63 (9) | C27—C28—Na1 | 75.29 (14) |
C1—V1—C12 | 65.98 (10) | V2—C28—Na1 | 146.44 (11) |
C15—V1—C12 | 142.45 (9) | O2'—Na1—O3' | 87.8 (5) |
C11—V1—C12 | 36.40 (9) | O1—Na1—O3 | 87.6 (6) |
C17—V1—C25 | 78.40 (10) | O2'—Na1—O1' | 95.3 (7) |
C3—V1—C25 | 179.52 (10) | O3'—Na1—O1' | 98.1 (9) |
C16—V1—C25 | 66.30 (9) | O1—Na1—O2 | 92.8 (5) |
C2—V1—C25 | 143.20 (10) | O3—Na1—O2 | 106.1 (4) |
C18—V1—C25 | 65.90 (10) | O2'—Na1—C24 | 105.2 (5) |
C4—V1—C25 | 142.70 (9) | O3'—Na1—C24 | 102.1 (6) |
C1—V1—C25 | 113.31 (10) | O1—Na1—C24 | 149.4 (4) |
C15—V1—C25 | 36.13 (9) | O3—Na1—C24 | 103.7 (4) |
C11—V1—C25 | 101.87 (9) | O1'—Na1—C24 | 151.5 (5) |
C12—V1—C25 | 113.71 (9) | O2—Na1—C24 | 110.5 (3) |
C17—V1—C26 | 66.21 (9) | O2'—Na1—C23 | 136.9 (4) |
C3—V1—C26 | 143.31 (10) | O3'—Na1—C23 | 132.6 (5) |
C16—V1—C26 | 78.23 (10) | O1—Na1—C23 | 91.5 (4) |
C2—V1—C26 | 179.47 (10) | O3—Na1—C23 | 123.4 (3) |
C18—V1—C26 | 36.36 (9) | O1'—Na1—C23 | 93.1 (5) |
C4—V1—C26 | 113.63 (9) | O2—Na1—C23 | 130.4 (2) |
C1—V1—C26 | 142.33 (10) | C24—Na1—C23 | 58.45 (8) |
C15—V1—C26 | 65.43 (9) | O2'—Na1—C25 | 109.0 (4) |
C11—V1—C26 | 113.56 (9) | O3'—Na1—C25 | 150.6 (6) |
C12—V1—C26 | 101.94 (8) | O1—Na1—C25 | 105.5 (4) |
C25—V1—C26 | 36.30 (8) | O3—Na1—C25 | 146.3 (3) |
C7—V2—C20 | 113.99 (10) | O1'—Na1—C25 | 103.9 (6) |
C7—V2—C21 | 101.29 (11) | O2—Na1—C25 | 104.2 (3) |
C20—V2—C21 | 37.26 (10) | C24—Na1—C25 | 50.95 (7) |
C7—V2—C6 | 37.21 (10) | C23—Na1—C25 | 28.39 (7) |
C20—V2—C6 | 102.62 (11) | O2'—Na1—C26 | 94.7 (5) |
C21—V2—C6 | 114.53 (10) | O3'—Na1—C26 | 128.7 (6) |
C7—V2—C8 | 37.33 (10) | O1—Na1—C26 | 134.8 (5) |
C20—V2—C8 | 143.26 (10) | O3—Na1—C26 | 131.8 (4) |
C21—V2—C8 | 112.67 (10) | O1'—Na1—C26 | 132.3 (6) |
C6—V2—C8 | 66.99 (10) | O2—Na1—C26 | 95.2 (3) |
C7—V2—C22 | 113.33 (11) | C24—Na1—C26 | 28.28 (7) |
C20—V2—C22 | 67.03 (10) | C23—Na1—C26 | 50.87 (7) |
C21—V2—C22 | 37.39 (9) | C25—Na1—C26 | 29.62 (7) |
C6—V2—C22 | 144.19 (10) | O2'—Na1—C27 | 131.4 (5) |
C8—V2—C22 | 100.11 (10) | O3'—Na1—C27 | 91.7 (6) |
C7—V2—C5 | 66.90 (10) | O1—Na1—C27 | 127.5 (3) |
C20—V2—C5 | 115.35 (10) | O3—Na1—C27 | 88.2 (4) |
C21—V2—C5 | 145.16 (10) | O1'—Na1—C27 | 132.7 (5) |
C6—V2—C5 | 37.25 (10) | O2—Na1—C27 | 138.2 (3) |
C8—V2—C5 | 78.54 (11) | C24—Na1—C27 | 28.07 (7) |
C22—V2—C5 | 177.43 (10) | C23—Na1—C27 | 49.79 (7) |
C7—V2—C19 | 144.41 (10) | C25—Na1—C27 | 59.02 (7) |
C20—V2—C19 | 37.35 (9) | C26—Na1—C27 | 50.17 (7) |
C21—V2—C19 | 67.01 (10) | O2'—Na1—C28 | 153.3 (5) |
C6—V2—C19 | 114.87 (10) | O3'—Na1—C28 | 105.6 (5) |
C8—V2—C19 | 178.12 (10) | O1—Na1—C28 | 100.9 (3) |
C22—V2—C19 | 78.52 (10) | O3—Na1—C28 | 97.7 (3) |
C5—V2—C19 | 102.78 (10) | O1'—Na1—C28 | 105.2 (5) |
C7—V2—C13 | 78.01 (10) | O2—Na1—C28 | 153.0 (3) |
C20—V2—C13 | 144.68 (10) | C24—Na1—C28 | 49.97 (7) |
C21—V2—C13 | 178.05 (9) | C23—Na1—C28 | 27.53 (7) |
C6—V2—C13 | 66.00 (9) | C25—Na1—C28 | 49.89 (7) |
C8—V2—C13 | 65.67 (9) | C26—Na1—C28 | 58.76 (7) |
C22—V2—C13 | 141.22 (9) | C27—Na1—C28 | 28.48 (7) |
C5—V2—C13 | 36.22 (9) | C32—O1—C29 | 106.8 (7) |
C19—V2—C13 | 114.61 (9) | C32—O1—Na1 | 118.8 (8) |
C7—V2—C14 | 66.20 (9) | C29—O1—Na1 | 128.5 (10) |
C20—V2—C14 | 179.19 (10) | O1—C29—C30 | 103.5 (10) |
C21—V2—C14 | 142.01 (10) | O1—C29—H29A | 111.1 |
C6—V2—C14 | 78.01 (10) | C30—C29—H29A | 111.1 |
C8—V2—C14 | 36.50 (9) | O1—C29—H29B | 111.1 |
C22—V2—C14 | 112.16 (9) | C30—C29—H29B | 111.1 |
C5—V2—C14 | 65.46 (9) | H29A—C29—H29B | 109.0 |
C19—V2—C14 | 142.84 (9) | C29—C30—C31 | 105.9 (8) |
C13—V2—C14 | 36.04 (8) | C29—C30—H30A | 110.6 |
C7—V2—C27 | 178.84 (10) | C31—C30—H30A | 110.6 |
C20—V2—C27 | 66.07 (9) | C29—C30—H30B | 110.6 |
C21—V2—C27 | 78.06 (9) | C31—C30—H30B | 110.6 |
C6—V2—C27 | 143.93 (10) | H30A—C30—H30B | 108.7 |
C8—V2—C27 | 142.02 (9) | C32—C31—C30 | 104.3 (7) |
C22—V2—C27 | 65.57 (9) | C32—C31—H31A | 110.9 |
C5—V2—C27 | 114.18 (9) | C30—C31—H31A | 110.9 |
C19—V2—C27 | 36.21 (8) | C32—C31—H31B | 110.9 |
C13—V2—C27 | 102.61 (9) | C30—C31—H31B | 110.9 |
C14—V2—C27 | 113.72 (9) | H31A—C31—H31B | 108.9 |
C7—V2—C28 | 142.67 (10) | O1—C32—C31 | 106.5 (8) |
C20—V2—C28 | 78.17 (9) | O1—C32—H32A | 110.4 |
C21—V2—C28 | 66.23 (9) | C31—C32—H32A | 110.4 |
C6—V2—C28 | 179.18 (9) | O1—C32—H32B | 110.4 |
C8—V2—C28 | 112.52 (10) | C31—C32—H32B | 110.4 |
C22—V2—C28 | 36.32 (9) | H32A—C32—H32B | 108.6 |
C5—V2—C28 | 142.21 (9) | C33—O2—C36 | 105.3 (6) |
C19—V2—C28 | 65.62 (9) | C33—O2—Na1 | 125.4 (7) |
C13—V2—C28 | 113.23 (8) | C36—O2—Na1 | 128.1 (6) |
C14—V2—C28 | 101.20 (9) | C34—C33—O2 | 109.9 (7) |
C27—V2—C28 | 36.19 (8) | C34—C33—H33A | 109.7 |
C2—C1—C11 | 121.9 (3) | O2—C33—H33A | 109.7 |
C2—C1—V1 | 70.77 (16) | C34—C33—H33B | 109.7 |
C11—C1—V1 | 76.42 (15) | O2—C33—H33B | 109.7 |
C2—C1—H1 | 120.6 (16) | H33A—C33—H33B | 108.2 |
C11—C1—H1 | 117.5 (16) | C33—C34—C35 | 104.7 (6) |
V1—C1—H1 | 127.5 (16) | C33—C34—H34A | 110.8 |
C3—C2—C1 | 119.6 (3) | C35—C34—H34A | 110.8 |
C3—C2—V1 | 70.85 (16) | C33—C34—H34B | 110.8 |
C1—C2—V1 | 71.77 (16) | C35—C34—H34B | 110.8 |
C3—C2—H2 | 123.5 (19) | H34A—C34—H34B | 108.9 |
C1—C2—H2 | 116.2 (19) | C36—C35—C34 | 106.8 (7) |
V1—C2—H2 | 120.6 (19) | C36—C35—H35A | 110.4 |
C2—C3—C4 | 120.2 (3) | C34—C35—H35A | 110.4 |
C2—C3—V1 | 71.96 (16) | C36—C35—H35B | 110.4 |
C4—C3—V1 | 72.24 (15) | C34—C35—H35B | 110.4 |
C2—C3—H3 | 119.1 (16) | H35A—C35—H35B | 108.6 |
C4—C3—H3 | 120.6 (16) | C35—C36—O2 | 106.6 (7) |
V1—C3—H3 | 125.4 (15) | C35—C36—H36A | 110.4 |
C3—C4—C12 | 122.2 (2) | O2—C36—H36A | 110.4 |
C3—C4—V1 | 70.51 (16) | C35—C36—H36B | 110.4 |
C12—C4—V1 | 76.73 (15) | O2—C36—H36B | 110.4 |
C3—C4—H4 | 119.7 (16) | H36A—C36—H36B | 108.6 |
C12—C4—H4 | 118.2 (16) | C40—O3—C37 | 106.0 (6) |
V1—C4—H4 | 124.3 (16) | C40—O3—Na1 | 131.2 (6) |
C6—C5—C13 | 121.7 (3) | C37—O3—Na1 | 122.8 (6) |
C6—C5—V2 | 70.32 (15) | O3—C37—C38 | 104.6 (8) |
C13—C5—V2 | 76.61 (15) | O3—C37—H37A | 110.8 |
C6—C5—H5 | 117.0 (17) | C38—C37—H37A | 110.8 |
C13—C5—H5 | 121.3 (17) | O3—C37—H37B | 110.8 |
V2—C5—H5 | 127.7 (17) | C38—C37—H37B | 110.8 |
C7—C6—C5 | 119.9 (3) | H37A—C37—H37B | 108.9 |
C7—C6—V2 | 71.15 (16) | C37—C38—C39 | 99.6 (8) |
C5—C6—V2 | 72.44 (15) | C37—C38—H38A | 111.9 |
C7—C6—H6 | 123.0 (17) | C39—C38—H38A | 111.9 |
C5—C6—H6 | 116.6 (17) | C37—C38—H38B | 111.9 |
V2—C6—H6 | 121.2 (16) | C39—C38—H38B | 111.9 |
C6—C7—C8 | 120.0 (3) | H38A—C38—H38B | 109.6 |
C6—C7—V2 | 71.64 (16) | C40—C39—C38 | 105.9 (7) |
C8—C7—V2 | 72.10 (15) | C40—C39—H39A | 110.5 |
C6—C7—H7 | 118.5 (17) | C38—C39—H39A | 110.5 |
C8—C7—H7 | 121.4 (17) | C40—C39—H39B | 110.5 |
V2—C7—H7 | 124.4 (17) | C38—C39—H39B | 110.5 |
C7—C8—C14 | 121.7 (3) | H39A—C39—H39B | 108.7 |
C7—C8—V2 | 70.57 (16) | O3—C40—C39 | 106.8 (7) |
C14—C8—V2 | 77.04 (15) | O3—C40—H40A | 110.4 |
C7—C8—H8 | 121.7 (15) | C39—C40—H40A | 110.4 |
C14—C8—H8 | 116.5 (15) | O3—C40—H40B | 110.4 |
V2—C8—H8 | 127.5 (15) | C39—C40—H40B | 110.4 |
C11—C9—C14 | 123.2 (2) | H40A—C40—H40B | 108.6 |
C11—C9—H9 | 121.7 (17) | C29'—O1'—C32' | 107.4 (11) |
C14—C9—H9 | 115.1 (16) | C29'—O1'—Na1 | 117.7 (17) |
C12—C10—C13 | 123.1 (2) | C32'—O1'—Na1 | 123.8 (13) |
C12—C10—H10 | 119.5 (17) | O1'—C29'—C30' | 106.4 (11) |
C13—C10—H10 | 117.3 (17) | O1'—C29'—H29C | 110.5 |
C9—C11—C1 | 123.2 (2) | C30'—C29'—H29C | 110.5 |
C9—C11—C12 | 118.5 (2) | O1'—C29'—H29D | 110.5 |
C1—C11—C12 | 118.2 (2) | C30'—C29'—H29D | 110.5 |
C9—C11—V1 | 128.81 (18) | H29C—C29'—H29D | 108.6 |
C1—C11—V1 | 67.02 (15) | C29'—C30'—C31' | 105.4 (11) |
C12—C11—V1 | 71.95 (14) | C29'—C30'—H30C | 110.7 |
C10—C12—C4 | 123.8 (2) | C31'—C30'—H30C | 110.7 |
C10—C12—C11 | 118.3 (2) | C29'—C30'—H30D | 110.7 |
C4—C12—C11 | 117.7 (2) | C31'—C30'—H30D | 110.7 |
C10—C12—V1 | 129.74 (18) | H30C—C30'—H30D | 108.8 |
C4—C12—V1 | 66.64 (14) | C32'—C31'—C30' | 102.0 (10) |
C11—C12—V1 | 71.64 (14) | C32'—C31'—H31C | 111.4 |
C10—C13—C5 | 122.8 (2) | C30'—C31'—H31C | 111.4 |
C10—C13—C14 | 118.6 (2) | C32'—C31'—H31D | 111.4 |
C5—C13—C14 | 118.5 (2) | C30'—C31'—H31D | 111.4 |
C10—C13—V2 | 129.85 (17) | H31C—C31'—H31D | 109.2 |
C5—C13—V2 | 67.16 (14) | O1'—C32'—C31' | 103.3 (12) |
C14—C13—V2 | 72.04 (14) | O1'—C32'—H32C | 111.1 |
C9—C14—C8 | 123.5 (2) | C31'—C32'—H32C | 111.1 |
C9—C14—C13 | 118.3 (2) | O1'—C32'—H32D | 111.1 |
C8—C14—C13 | 117.9 (2) | C31'—C32'—H32D | 111.1 |
C9—C14—V2 | 129.16 (18) | H32C—C32'—H32D | 109.1 |
C8—C14—V2 | 66.46 (14) | C36'—O2'—C33' | 109.2 (9) |
C13—C14—V2 | 71.91 (13) | C36'—O2'—Na1 | 139.1 (9) |
C16—C15—C25 | 122.3 (3) | C33'—O2'—Na1 | 110.4 (8) |
C16—C15—V1 | 70.01 (16) | O2'—C33'—C34' | 107.4 (9) |
C25—C15—V1 | 76.84 (15) | O2'—C33'—H33C | 110.2 |
C16—C15—H15 | 116.7 (17) | C34'—C33'—H33C | 110.2 |
C25—C15—H15 | 121.0 (17) | O2'—C33'—H33D | 110.2 |
V1—C15—H15 | 126.2 (17) | C34'—C33'—H33D | 110.2 |
C17—C16—C15 | 119.4 (2) | H33C—C33'—H33D | 108.5 |
C17—C16—V1 | 70.80 (16) | C33'—C34'—C35' | 104.9 (9) |
C15—C16—V1 | 72.57 (16) | C33'—C34'—H34C | 110.8 |
C17—C16—H16 | 121.3 (16) | C35'—C34'—H34C | 110.8 |
C15—C16—H16 | 119.2 (16) | C33'—C34'—H34D | 110.8 |
V1—C16—H16 | 125.4 (16) | C35'—C34'—H34D | 110.8 |
C16—C17—C18 | 120.2 (3) | H34C—C34'—H34D | 108.8 |
C16—C17—V1 | 71.72 (16) | C36'—C35'—C34' | 102.2 (9) |
C18—C17—V1 | 72.40 (16) | C36'—C35'—H35C | 111.3 |
C16—C17—H17 | 118.7 (15) | C34'—C35'—H35C | 111.3 |
C18—C17—H17 | 120.9 (15) | C36'—C35'—H35D | 111.3 |
V1—C17—H17 | 124.1 (15) | C34'—C35'—H35D | 111.3 |
C17—C18—C26 | 122.1 (3) | H35C—C35'—H35D | 109.2 |
C17—C18—V1 | 70.20 (16) | O2'—C36'—C35' | 106.8 (9) |
C26—C18—V1 | 77.75 (15) | O2'—C36'—H36C | 110.4 |
C17—C18—H18 | 117.2 (18) | C35'—C36'—H36C | 110.4 |
C26—C18—H18 | 120.7 (19) | O2'—C36'—H36D | 110.4 |
V1—C18—H18 | 125.0 (18) | C35'—C36'—H36D | 110.4 |
C20—C19—C27 | 121.5 (2) | H36C—C36'—H36D | 108.6 |
C20—C19—V2 | 70.09 (15) | C40'—O3'—C37' | 107.5 (10) |
C27—C19—V2 | 76.67 (14) | C40'—O3'—Na1 | 139.8 (12) |
C20—C19—H19 | 118.2 (14) | C37'—O3'—Na1 | 110.5 (10) |
C27—C19—H19 | 120.2 (14) | O3'—C37'—C38' | 109.2 (11) |
V2—C19—H19 | 127.2 (14) | O3'—C37'—Na1 | 44.0 (7) |
C21—C20—C19 | 120.1 (2) | C38'—C37'—Na1 | 143.1 (15) |
C21—C20—V2 | 71.44 (15) | O3'—C37'—H37C | 109.8 |
C19—C20—V2 | 72.56 (15) | C38'—C37'—H37C | 109.8 |
C21—C20—H20 | 122.1 (17) | Na1—C37'—H37C | 70.8 |
C19—C20—H20 | 117.9 (17) | O3'—C37'—H37D | 109.8 |
V2—C20—H20 | 127.0 (17) | C38'—C37'—H37D | 109.8 |
C20—C21—C22 | 119.8 (2) | Na1—C37'—H37D | 104.3 |
C20—C21—V2 | 71.30 (15) | H37C—C37'—H37D | 108.3 |
C22—C21—V2 | 72.32 (15) | C39'—C38'—C37' | 102.4 (10) |
C20—C21—H21 | 122.0 (16) | C39'—C38'—H38C | 111.3 |
C22—C21—H21 | 118.0 (16) | C37'—C38'—H38C | 111.3 |
V2—C21—H21 | 123.5 (16) | C39'—C38'—H38D | 111.3 |
C21—C22—C28 | 121.8 (2) | C37'—C38'—H38D | 111.3 |
C21—C22—V2 | 70.29 (15) | H38C—C38'—H38D | 109.2 |
C28—C22—V2 | 76.86 (14) | C40'—C39'—C38' | 105.9 (11) |
C21—C22—H22 | 118.5 (16) | C40'—C39'—H39C | 110.6 |
C28—C22—H22 | 119.6 (16) | C38'—C39'—H39C | 110.6 |
V2—C22—H22 | 126.7 (16) | C40'—C39'—H39D | 110.6 |
C28—C23—C25 | 123.6 (2) | C38'—C39'—H39D | 110.6 |
C28—C23—Na1 | 80.78 (15) | H39C—C39'—H39D | 108.7 |
C25—C23—Na1 | 76.13 (15) | O3'—C40'—C39' | 109.6 (11) |
C28—C23—H23 | 120.1 (18) | O3'—C40'—H40C | 109.8 |
C25—C23—H23 | 115.8 (18) | C39'—C40'—H40C | 109.8 |
Na1—C23—H23 | 122.0 (18) | O3'—C40'—H40D | 109.8 |
C26—C24—C27 | 123.6 (2) | C39'—C40'—H40D | 109.8 |
C26—C24—Na1 | 77.11 (15) | H40C—C40'—H40D | 108.2 |
C27—C24—Na1 | 80.88 (15) | | |
| | | |
C11—C1—C2—C3 | −5.1 (4) | V1—C18—C26—C24 | 125.7 (2) |
V1—C1—C2—C3 | 54.3 (3) | C17—C18—C26—C25 | 5.8 (4) |
C11—C1—C2—V1 | −59.4 (2) | V1—C18—C26—C25 | −51.1 (2) |
C1—C2—C3—C4 | 1.2 (4) | C17—C18—C26—V1 | 56.9 (2) |
V1—C2—C3—C4 | 55.9 (2) | C17—C18—C26—Na1 | −84.0 (3) |
C1—C2—C3—V1 | −54.7 (3) | V1—C18—C26—Na1 | −140.92 (15) |
C2—C3—C4—C12 | 3.6 (4) | C23—C25—C26—C24 | −1.2 (3) |
V1—C3—C4—C12 | 59.3 (2) | C15—C25—C26—C24 | −178.9 (2) |
C2—C3—C4—V1 | −55.7 (2) | V1—C25—C26—C24 | −128.4 (2) |
C13—C5—C6—C7 | −4.3 (4) | Na1—C25—C26—C24 | 63.1 (2) |
V2—C5—C6—C7 | 55.1 (2) | C23—C25—C26—C18 | 175.7 (2) |
C13—C5—C6—V2 | −59.4 (2) | C15—C25—C26—C18 | −2.0 (4) |
C5—C6—C7—C8 | −0.1 (4) | V1—C25—C26—C18 | 48.6 (2) |
V2—C6—C7—C8 | 55.6 (2) | Na1—C25—C26—C18 | −119.9 (2) |
C5—C6—C7—V2 | −55.7 (2) | C23—C25—C26—V1 | 127.2 (2) |
C6—C7—C8—C14 | 4.8 (4) | C15—C25—C26—V1 | −50.5 (2) |
V2—C7—C8—C14 | 60.2 (2) | Na1—C25—C26—V1 | −168.50 (8) |
C6—C7—C8—V2 | −55.4 (2) | C23—C25—C26—Na1 | −64.3 (2) |
C14—C9—C11—C1 | −175.4 (2) | C15—C25—C26—Na1 | 118.0 (2) |
C14—C9—C11—C12 | −0.5 (4) | V1—C25—C26—Na1 | 168.50 (8) |
C14—C9—C11—V1 | −89.6 (3) | C26—C24—C27—C19 | 171.5 (2) |
C2—C1—C11—C9 | 179.1 (3) | Na1—C24—C27—C19 | −120.8 (2) |
V1—C1—C11—C9 | 122.4 (2) | C26—C24—C27—C28 | −5.5 (4) |
C2—C1—C11—C12 | 4.2 (4) | Na1—C24—C27—C28 | 62.3 (2) |
V1—C1—C11—C12 | −52.5 (2) | C26—C24—C27—V2 | 84.0 (3) |
C2—C1—C11—V1 | 56.7 (2) | Na1—C24—C27—V2 | 151.81 (19) |
C13—C10—C12—C4 | 174.0 (2) | C26—C24—C27—Na1 | −67.8 (2) |
C13—C10—C12—C11 | −1.4 (4) | C20—C19—C27—C24 | 179.1 (2) |
C13—C10—C12—V1 | 87.7 (3) | V2—C19—C27—C24 | −124.6 (2) |
C3—C4—C12—C10 | −179.7 (2) | C20—C19—C27—C28 | −4.0 (4) |
V1—C4—C12—C10 | −123.3 (2) | V2—C19—C27—C28 | 52.3 (2) |
C3—C4—C12—C11 | −4.3 (4) | C20—C19—C27—V2 | −56.2 (2) |
V1—C4—C12—C11 | 52.1 (2) | C20—C19—C27—Na1 | 89.3 (3) |
C3—C4—C12—V1 | −56.4 (2) | V2—C19—C27—Na1 | 145.55 (16) |
C9—C11—C12—C10 | 0.9 (4) | C25—C23—C28—C22 | −171.9 (2) |
C1—C11—C12—C10 | 176.1 (2) | Na1—C23—C28—C22 | 121.6 (2) |
V1—C11—C12—C10 | 125.9 (2) | C25—C23—C28—C27 | 5.4 (4) |
C9—C11—C12—C4 | −174.7 (2) | Na1—C23—C28—C27 | −61.0 (2) |
C1—C11—C12—C4 | 0.4 (4) | C25—C23—C28—V2 | −84.7 (3) |
V1—C11—C12—C4 | −49.7 (2) | Na1—C23—C28—V2 | −151.17 (19) |
C9—C11—C12—V1 | −125.0 (2) | C25—C23—C28—Na1 | 66.4 (2) |
C1—C11—C12—V1 | 50.2 (2) | C21—C22—C28—C23 | −178.5 (2) |
C12—C10—C13—C5 | −174.9 (2) | V2—C22—C28—C23 | 125.0 (2) |
C12—C10—C13—C14 | 1.3 (4) | C21—C22—C28—C27 | 4.1 (4) |
C12—C10—C13—V2 | −88.5 (3) | V2—C22—C28—C27 | −52.3 (2) |
C6—C5—C13—C10 | −179.8 (2) | C21—C22—C28—V2 | 56.4 (2) |
V2—C5—C13—C10 | 123.8 (2) | C21—C22—C28—Na1 | −87.6 (3) |
C6—C5—C13—C14 | 4.0 (4) | V2—C22—C28—Na1 | −144.06 (16) |
V2—C5—C13—C14 | −52.4 (2) | C24—C27—C28—C23 | −0.4 (3) |
C6—C5—C13—V2 | 56.4 (2) | C19—C27—C28—C23 | −177.5 (2) |
C11—C9—C14—C8 | 175.1 (2) | V2—C27—C28—C23 | −127.5 (2) |
C11—C9—C14—C13 | 0.5 (4) | Na1—C27—C28—C23 | 59.2 (2) |
C11—C9—C14—V2 | 89.6 (3) | C24—C27—C28—C22 | 177.1 (2) |
C7—C8—C14—C9 | −179.6 (2) | C19—C27—C28—C22 | 0.0 (3) |
V2—C8—C14—C9 | −122.5 (2) | V2—C27—C28—C22 | 50.0 (2) |
C7—C8—C14—C13 | −5.0 (4) | Na1—C27—C28—C22 | −123.4 (2) |
V2—C8—C14—C13 | 52.1 (2) | C24—C27—C28—V2 | 127.1 (2) |
C7—C8—C14—V2 | −57.1 (2) | C19—C27—C28—V2 | −50.0 (2) |
C10—C13—C14—C9 | −0.8 (3) | Na1—C27—C28—V2 | −173.33 (8) |
C5—C13—C14—C9 | 175.5 (2) | C24—C27—C28—Na1 | −59.6 (2) |
V2—C13—C14—C9 | 125.4 (2) | C19—C27—C28—Na1 | 123.3 (2) |
C10—C13—C14—C8 | −175.7 (2) | V2—C27—C28—Na1 | 173.33 (8) |
C5—C13—C14—C8 | 0.6 (3) | C32—O1—C29—C30 | 36.9 (17) |
V2—C13—C14—C8 | −49.5 (2) | Na1—O1—C29—C30 | −115.0 (15) |
C10—C13—C14—V2 | −126.2 (2) | O1—C29—C30—C31 | −26 (2) |
C5—C13—C14—V2 | 50.2 (2) | C29—C30—C31—C32 | 7 (2) |
C25—C15—C16—C17 | 3.8 (4) | C29—O1—C32—C31 | −33.2 (15) |
V1—C15—C16—C17 | −55.1 (2) | Na1—O1—C32—C31 | 121.9 (12) |
C25—C15—C16—V1 | 58.9 (2) | C30—C31—C32—O1 | 15.4 (17) |
C15—C16—C17—C18 | 0.0 (4) | C36—O2—C33—C34 | 24.1 (13) |
V1—C16—C17—C18 | −55.9 (2) | Na1—O2—C33—C34 | −144.1 (9) |
C15—C16—C17—V1 | 56.0 (2) | O2—C33—C34—C35 | −12.1 (14) |
C16—C17—C18—C26 | −4.9 (4) | C33—C34—C35—C36 | −4.4 (15) |
V1—C17—C18—C26 | −60.5 (2) | C34—C35—C36—O2 | 19.0 (14) |
C16—C17—C18—V1 | 55.6 (2) | C33—O2—C36—C35 | −26.2 (13) |
C27—C19—C20—C21 | 3.9 (4) | Na1—O2—C36—C35 | 141.6 (11) |
V2—C19—C20—C21 | −55.4 (2) | C40—O3—C37—C38 | −38.4 (14) |
C27—C19—C20—V2 | 59.3 (2) | Na1—O3—C37—C38 | 142.2 (12) |
C19—C20—C21—C22 | 0.3 (4) | O3—C37—C38—C39 | 40.6 (15) |
V2—C20—C21—C22 | −55.7 (2) | C37—C38—C39—C40 | −28.4 (17) |
C19—C20—C21—V2 | 56.0 (2) | C37—O3—C40—C39 | 19.3 (16) |
C20—C21—C22—C28 | −4.3 (4) | Na1—O3—C40—C39 | −161.4 (12) |
V2—C21—C22—C28 | −59.5 (2) | C38—C39—C40—O3 | 6.8 (18) |
C20—C21—C22—V2 | 55.2 (2) | C32'—O1'—C29'—C30' | 19 (3) |
C28—C23—C25—C15 | 173.0 (2) | Na1—O1'—C29'—C30' | −127 (2) |
Na1—C23—C25—C15 | −118.3 (3) | O1'—C29'—C30'—C31' | 6 (3) |
C28—C23—C25—C26 | −4.6 (4) | C29'—C30'—C31'—C32' | −27 (3) |
Na1—C23—C25—C26 | 64.2 (2) | C29'—O1'—C32'—C31' | −37 (2) |
C28—C23—C25—V1 | 85.4 (3) | Na1—O1'—C32'—C31' | 106.3 (19) |
Na1—C23—C25—V1 | 154.2 (2) | C30'—C31'—C32'—O1' | 39 (2) |
C28—C23—C25—Na1 | −68.7 (2) | C36'—O2'—C33'—C34' | 7 (2) |
C16—C15—C25—C23 | 179.7 (3) | Na1—O2'—C33'—C34' | 176.4 (12) |
V1—C15—C25—C23 | −124.6 (2) | O2'—C33'—C34'—C35' | 13 (2) |
C16—C15—C25—C26 | −2.8 (4) | C33'—C34'—C35'—C36' | −26.2 (18) |
V1—C15—C25—C26 | 53.0 (2) | C33'—O2'—C36'—C35' | −24.2 (19) |
C16—C15—C25—V1 | −55.7 (2) | Na1—O2'—C36'—C35' | 170.6 (17) |
C16—C15—C25—Na1 | 86.5 (3) | C34'—C35'—C36'—O2' | 31.0 (17) |
V1—C15—C25—Na1 | 142.22 (15) | C40'—O3'—C37'—C38' | −18 (3) |
C27—C24—C26—C18 | −170.5 (2) | Na1—O3'—C37'—C38' | 149.2 (16) |
Na1—C24—C26—C18 | 119.8 (2) | C40'—O3'—C37'—Na1 | −167 (3) |
C27—C24—C26—C25 | 6.3 (4) | O3'—C37'—C38'—C39' | 24 (3) |
Na1—C24—C26—C25 | −63.4 (2) | Na1—C37'—C38'—C39' | 60 (3) |
C27—C24—C26—V1 | −83.5 (3) | C37'—C38'—C39'—C40' | −20 (3) |
Na1—C24—C26—V1 | −153.2 (2) | C37'—O3'—C40'—C39' | 4 (3) |
C27—C24—C26—Na1 | 69.7 (2) | Na1—O3'—C40'—C39' | −157 (2) |
C17—C18—C26—C24 | −177.4 (3) | C38'—C39'—C40'—O3' | 11 (3) |