Supporting information
Crystallographic Information File (CIF) https://doi.org/10.1107/S0108270104019705/ob1193sup1.cif | |
Structure factor file (CIF format) https://doi.org/10.1107/S0108270104019705/ob1193Isup2.hkl |
CCDC reference: 254894
All organic solvents and common materials used in the synthesis were of reagent grade and were used without further purification. H3PMo12O40 was prepared according to the literature method (Claude et al., 1983). 1,4-Dimethylpyridinium iodide was prepared according to the method described by Ren et al. (2000). Compound (I) was prepared by mixing a CaCl2/dmf solution (0.01 mol l−1), a DMPI/dmf solution (0.01 mol l−1) and a H3PMo12O40/dmf solution (0.01 mol l−1) in a 1:1:1 molar ratio. After 15 d of slow evaporation of water at room temperature, bright-green crystals of (I) were obtained from the solution; the crystals were transparent without further purification. Analysis calculated: C 12.46, H 2.18, N 4.07%; found: C 12.26, H 2.18, N 3.94%. IR (KBr, cm−1): 1061, 957, 878, 797 (PMo12O403−), 1654 (C=O), 1600, 1497, 1437 (pyridine ring), 1382 (–CH3).
For other DMP salts (Khan et al., 1998; Fun et al., 1996; Houghton & Wallwork, 1999; Mckinney et al., 1997), disordered para-C and para-N atoms could be treated as 50%C + 50%N; however, our attempts to refine the title compound in the same way were unsuccessful. In fact, the DMP cation is rocking, and the populations of the two possible orientations, C1/C7/N1 and C1'/C7'/N1', are 72.5 (10) and 27.5 (10)%, respectively. In the [Ca(dmf)6]2+ cation, the torsional motion of the NMe2 groups of the dmf ligands leads to substantial disorder. Each NMe2 moiety has two possible positions, with site occupancy factors of 72.5 (10) and 27.5 (10)%. These disorders in the cations contribute to the high s.u. values of bond lengths and angles (0.006–0.02 Å and 0.2–1.9°). A number of atoms have apparently high displacement parameters and some of them cannot be treated as anisotropic for the same reasons. All H atoms were positioned geometrically and allowed to ride on their parent atoms, with C—H distances in the range 0.93–0.96 Å, and with Uiso(H) = 1.5Ueq(C) for methyl H atoms and 1.2Ueq(C) for the other H atoms.
Data collection: SMART (Bruker, 2000); cell refinement: SMART; data reduction: SAINT (Bruker, 2000); program(s) used to solve structure: SHELXTL (Bruker, 2000); program(s) used to refine structure: SHELXL97 (Sheldrick, 1997); molecular graphics: SHELXTL; software used to prepare material for publication: SHELXL97.
(C7H10N)[Ca(C3H7NO)6][PMo12O40] | F(000) = 4632.0 |
Mr = 2409.07 | Dx = 2.442 Mg m−3 |
Orthorhombic, Pca21 | Mo Kα radiation, λ = 0.71073 Å |
Hall symbol: P 2c -2ac | Cell parameters from 380 reflections |
a = 38.293 (6) Å | θ = 7.5–27.0° |
b = 13.246 (2) Å | µ = 2.43 mm−1 |
c = 12.888 (2) Å | T = 293 K |
V = 6537.6 (17) Å3 | Block, green |
Z = 4 | 0.49 × 0.11 × 0.08 mm |
Bruker SMART CCD area-detector diffractometer | 14090 independent reflections |
Radiation source: fine-focus sealed tube | 12008 reflections with I > 2σ(I) |
Graphite monochromator | Rint = 0.038 |
ϕ and ω scans | θmax = 27.1°, θmin = 1.6° |
Absorption correction: multi-scan (SADABS; Bruker, 2000) | h = −48→49 |
Tmin = 0.733, Tmax = 0.824 | k = −14→16 |
39117 measured reflections | l = −16→16 |
Refinement on F2 | Secondary atom site location: difference Fourier map |
Least-squares matrix: full | Hydrogen site location: inferred from neighbouring sites |
R[F2 > 2σ(F2)] = 0.060 | H-atom parameters constrained |
wR(F2) = 0.127 | w = 1/[σ2(Fo2) + (0.0518P)2 + 11.3547P] where P = (Fo2 + 2Fc2)/3 |
S = 1.10 | (Δ/σ)max = 0.002 |
14090 reflections | Δρmax = 1.08 e Å−3 |
746 parameters | Δρmin = −0.63 e Å−3 |
377 restraints | Absolute structure: Flack (1983), 6579 Friedel pairs |
Primary atom site location: structure-invariant direct methods | Absolute structure parameter: −0.01 (5) |
(C7H10N)[Ca(C3H7NO)6][PMo12O40] | V = 6537.6 (17) Å3 |
Mr = 2409.07 | Z = 4 |
Orthorhombic, Pca21 | Mo Kα radiation |
a = 38.293 (6) Å | µ = 2.43 mm−1 |
b = 13.246 (2) Å | T = 293 K |
c = 12.888 (2) Å | 0.49 × 0.11 × 0.08 mm |
Bruker SMART CCD area-detector diffractometer | 14090 independent reflections |
Absorption correction: multi-scan (SADABS; Bruker, 2000) | 12008 reflections with I > 2σ(I) |
Tmin = 0.733, Tmax = 0.824 | Rint = 0.038 |
39117 measured reflections |
R[F2 > 2σ(F2)] = 0.060 | H-atom parameters constrained |
wR(F2) = 0.127 | w = 1/[σ2(Fo2) + (0.0518P)2 + 11.3547P] where P = (Fo2 + 2Fc2)/3 |
S = 1.10 | Δρmax = 1.08 e Å−3 |
14090 reflections | Δρmin = −0.63 e Å−3 |
746 parameters | Absolute structure: Flack (1983), 6579 Friedel pairs |
377 restraints | Absolute structure parameter: −0.01 (5) |
Geometry. All e.s.d.'s (except the e.s.d. in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell e.s.d.'s are taken into account individually in the estimation of e.s.d.'s in distances, angles and torsion angles; correlations between e.s.d.'s in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell e.s.d.'s is used for estimating e.s.d.'s involving l.s. planes. |
Refinement. Refinement of F2 against ALL reflections. The weighted R-factor wR and goodness of fit S are based on F2, conventional R-factors R are based on F, with F set to zero for negative F2. The threshold expression of F2 > σ(F2) is used only for calculating R-factors(gt) etc. and is not relevant to the choice of reflections for refinement. R-factors based on F2 are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger. |
x | y | z | Uiso*/Ueq | Occ. (<1) | |
C1 | 0.4538 (4) | 0.1607 (11) | 0.0813 (11) | 0.070 (5) | 0.725 (10) |
H1A | 0.4526 | 0.2223 | 0.0470 | 0.084* | 0.725 (10) |
C2 | 0.4318 (4) | 0.0836 (11) | 0.0546 (12) | 0.073 (5)* | 0.725 (10) |
H2A | 0.4152 | 0.0929 | 0.0027 | 0.088* | 0.725 (10) |
C3 | 0.4342 (3) | −0.0058 (13) | 0.1040 (10) | 0.053 (4)* | 0.725 (10) |
C4 | 0.4578 (3) | −0.0162 (10) | 0.1793 (11) | 0.085 (4)* | 0.725 (10) |
H4A | 0.4589 | −0.0777 | 0.2139 | 0.101* | 0.725 (10) |
C5 | 0.4801 (5) | 0.0578 (9) | 0.2083 (15) | 0.074 (6)* | 0.725 (10) |
H5A | 0.4965 | 0.0478 | 0.2606 | 0.089* | 0.725 (10) |
C6 | 0.4092 (6) | −0.0898 (17) | 0.0766 (17) | 0.124 (8)* | 0.725 (10) |
H6A | 0.4141 | −0.1478 | 0.1190 | 0.185* | 0.725 (10) |
H6B | 0.4120 | −0.1073 | 0.0048 | 0.185* | 0.725 (10) |
H6C | 0.3857 | −0.0679 | 0.0887 | 0.185* | 0.725 (10) |
C7 | 0.5017 (6) | 0.2318 (13) | 0.1863 (17) | 0.101 (7)* | 0.725 (10) |
H7A | 0.4963 | 0.2898 | 0.1445 | 0.151* | 0.725 (10) |
H7B | 0.5254 | 0.2116 | 0.1741 | 0.151* | 0.725 (10) |
H7C | 0.4987 | 0.2485 | 0.2582 | 0.151* | 0.725 (10) |
N1 | 0.4775 (4) | 0.1466 (9) | 0.1581 (11) | 0.069 (4)* | 0.725 (10) |
C1' | 0.4387 (9) | 0.1286 (19) | 0.048 (2) | 0.070 (5) | 0.275 (10) |
H1'A | 0.4306 | 0.1805 | 0.0062 | 0.084* | 0.275 (10) |
C2' | 0.4246 (8) | 0.034 (2) | 0.040 (2) | 0.074 (13)* | 0.275 (10) |
H2'A | 0.4077 | 0.0204 | −0.0094 | 0.089* | 0.275 (10) |
C3' | 0.4354 (7) | −0.0396 (18) | 0.1051 (18) | 0.080 (18)* | 0.275 (10) |
C4' | 0.4578 (3) | −0.0162 (10) | 0.1793 (11) | 0.085 (4)* | 0.275 (10) |
H4'A | 0.4626 | −0.0647 | 0.2295 | 0.101* | 0.275 (10) |
C5' | 0.4742 (11) | 0.0751 (16) | 0.187 (3) | 0.080 (18)* | 0.275 (10) |
H5'A | 0.4911 | 0.0875 | 0.2370 | 0.096* | 0.275 (10) |
C6' | 0.4224 (13) | −0.146 (3) | 0.091 (3) | 0.124 (8)* | 0.275 (10) |
H6'A | 0.4330 | −0.1893 | 0.1420 | 0.185* | 0.275 (10) |
H6'B | 0.4286 | −0.1698 | 0.0227 | 0.185* | 0.275 (10) |
H6'C | 0.3975 | −0.1479 | 0.0986 | 0.185* | 0.275 (10) |
C7' | 0.4795 (12) | 0.2512 (18) | 0.126 (4) | 0.101 (7)* | 0.275 (10) |
H7'A | 0.4979 | 0.2518 | 0.1765 | 0.151* | 0.275 (10) |
H7'B | 0.4615 | 0.2974 | 0.1462 | 0.151* | 0.275 (10) |
H7'C | 0.4888 | 0.2712 | 0.0596 | 0.151* | 0.275 (10) |
N1' | 0.4646 (9) | 0.1463 (13) | 0.118 (2) | 0.057 (10)* | 0.275 (10) |
O2 | 0.2912 (3) | 0.6490 (9) | 0.2363 (9) | 0.111 (3) | |
C23 | 0.2794 (4) | 0.5958 (13) | 0.3072 (12) | 0.111 (3) | |
H23A | 0.2786 | 0.5266 | 0.2951 | 0.133* | |
N2 | 0.2684 (3) | 0.6260 (12) | 0.3939 (11) | 0.111 (3) | 0.725 (10) |
C21 | 0.2549 (8) | 0.5650 (19) | 0.475 (2) | 0.151 (10) | 0.725 (10) |
H21A | 0.2493 | 0.4993 | 0.4483 | 0.226* | 0.725 (10) |
H21B | 0.2342 | 0.5957 | 0.5026 | 0.226* | 0.725 (10) |
H21C | 0.2721 | 0.5588 | 0.5288 | 0.226* | 0.725 (10) |
C22 | 0.2672 (8) | 0.7315 (14) | 0.402 (3) | 0.155 (12)* | 0.725 (10) |
H22A | 0.2745 | 0.7613 | 0.3381 | 0.233* | 0.725 (10) |
H22B | 0.2826 | 0.7529 | 0.4569 | 0.233* | 0.725 (10) |
H22C | 0.2438 | 0.7524 | 0.4182 | 0.233* | 0.725 (10) |
N2' | 0.2684 (3) | 0.6260 (12) | 0.3939 (11) | 0.1109 (14) | 0.275 (10) |
C21' | 0.261 (3) | 0.541 (4) | 0.459 (6) | 0.151 (10) | 0.275 (10) |
H21D | 0.2816 | 0.4986 | 0.4624 | 0.226* | 0.275 (10) |
H21E | 0.2422 | 0.5029 | 0.4301 | 0.226* | 0.275 (10) |
H21F | 0.2552 | 0.5636 | 0.5270 | 0.226* | 0.275 (10) |
C22' | 0.285 (2) | 0.710 (4) | 0.441 (6) | 0.155 (12)* | 0.275 (10) |
H22D | 0.2884 | 0.7627 | 0.3910 | 0.233* | 0.275 (10) |
H22E | 0.3077 | 0.6893 | 0.4672 | 0.233* | 0.275 (10) |
H22F | 0.2713 | 0.7345 | 0.4977 | 0.233* | 0.275 (10) |
O3 | 0.3487 (3) | 0.4964 (6) | 0.1815 (7) | 0.086 (2) | |
C33 | 0.3471 (4) | 0.4051 (9) | 0.1787 (11) | 0.086 (2) | |
H33A | 0.3649 | 0.3714 | 0.2136 | 0.103* | |
N3 | 0.3247 (3) | 0.3486 (8) | 0.1350 (9) | 0.086 (2) | 0.725 (10) |
C31 | 0.3233 (7) | 0.2408 (12) | 0.140 (2) | 0.114 (8)* | 0.725 (10) |
H31A | 0.3446 | 0.2158 | 0.1701 | 0.171* | 0.725 (10) |
H31B | 0.3205 | 0.2136 | 0.0719 | 0.171* | 0.725 (10) |
H31C | 0.3040 | 0.2206 | 0.1830 | 0.171* | 0.725 (10) |
C32 | 0.2969 (6) | 0.3955 (18) | 0.077 (2) | 0.127 (9)* | 0.725 (10) |
H32A | 0.3019 | 0.4659 | 0.0680 | 0.191* | 0.725 (10) |
H32B | 0.2753 | 0.3880 | 0.1140 | 0.191* | 0.725 (10) |
H32C | 0.2950 | 0.3637 | 0.0103 | 0.191* | 0.725 (10) |
N3' | 0.3247 (3) | 0.3486 (8) | 0.1350 (9) | 0.0861 (9) | 0.275 (10) |
C31' | 0.3452 (18) | 0.241 (5) | 0.126 (6) | 0.114 (8)* | 0.275 (10) |
H31D | 0.3593 | 0.2311 | 0.1865 | 0.171* | 0.275 (10) |
H31E | 0.3598 | 0.2418 | 0.0653 | 0.171* | 0.275 (10) |
H31F | 0.3285 | 0.1874 | 0.1201 | 0.171* | 0.275 (10) |
C32' | 0.3049 (18) | 0.344 (6) | 0.040 (4) | 0.127 (9)* | 0.275 (10) |
H32D | 0.2932 | 0.4068 | 0.0292 | 0.191* | 0.275 (10) |
H32E | 0.2880 | 0.2904 | 0.0451 | 0.191* | 0.275 (10) |
H32F | 0.3204 | 0.3305 | −0.0167 | 0.191* | 0.275 (10) |
O4 | 0.3250 (3) | 0.6339 (7) | −0.0222 (8) | 0.091 (2) | |
C43 | 0.3357 (4) | 0.6269 (11) | −0.1123 (10) | 0.091 (2) | |
H43A | 0.3418 | 0.5618 | −0.1324 | 0.109* | |
N4 | 0.3397 (3) | 0.6924 (8) | −0.1814 (9) | 0.091 (2) | 0.725 (10) |
C41 | 0.3297 (8) | 0.7943 (15) | −0.158 (2) | 0.157 (11)* | 0.725 (10) |
H41A | 0.3177 | 0.7962 | −0.0930 | 0.236* | 0.725 (10) |
H41B | 0.3146 | 0.8192 | −0.2120 | 0.236* | 0.725 (10) |
H41C | 0.3502 | 0.8359 | −0.1545 | 0.236* | 0.725 (10) |
C42 | 0.3580 (5) | 0.6782 (15) | −0.2779 (13) | 0.080 (5)* | 0.725 (10) |
H42A | 0.3710 | 0.6162 | −0.2753 | 0.119* | 0.725 (10) |
H42B | 0.3738 | 0.7336 | −0.2888 | 0.119* | 0.725 (10) |
H42C | 0.3415 | 0.6755 | −0.3340 | 0.119* | 0.725 (10) |
N4' | 0.3397 (3) | 0.6924 (8) | −0.1814 (9) | 0.0912 (10) | 0.275 (10) |
C41' | 0.354 (2) | 0.787 (3) | −0.146 (4) | 0.157 (11)* | 0.275 (10) |
H41D | 0.3508 | 0.7920 | −0.0721 | 0.236* | 0.275 (10) |
H41E | 0.3415 | 0.8415 | −0.1792 | 0.236* | 0.275 (10) |
H41F | 0.3781 | 0.7904 | −0.1628 | 0.236* | 0.275 (10) |
C42' | 0.3386 (14) | 0.679 (4) | −0.2917 (15) | 0.080 (5)* | 0.275 (10) |
H42D | 0.3343 | 0.6089 | −0.3072 | 0.119* | 0.275 (10) |
H42E | 0.3606 | 0.6985 | −0.3212 | 0.119* | 0.275 (10) |
H42F | 0.3203 | 0.7193 | −0.3206 | 0.119* | 0.275 (10) |
O5 | 0.3969 (2) | 0.6563 (7) | 0.0661 (9) | 0.087 (2) | |
C53 | 0.4200 (3) | 0.5910 (10) | 0.0605 (12) | 0.087 (2) | |
H53A | 0.4180 | 0.5372 | 0.1065 | 0.104* | |
N5 | 0.4459 (3) | 0.5886 (8) | −0.0002 (10) | 0.087 (2) | 0.725 (10) |
C51 | 0.4725 (6) | 0.5125 (15) | −0.007 (2) | 0.103 (7)* | 0.725 (10) |
H51A | 0.4693 | 0.4640 | 0.0470 | 0.154* | 0.725 (10) |
H51B | 0.4951 | 0.5433 | −0.0007 | 0.154* | 0.725 (10) |
H51C | 0.4709 | 0.4793 | −0.0735 | 0.154* | 0.725 (10) |
C52 | 0.4465 (7) | 0.6653 (18) | −0.078 (2) | 0.128 (10)* | 0.725 (10) |
H52A | 0.4266 | 0.6575 | −0.1229 | 0.192* | 0.725 (10) |
H52B | 0.4675 | 0.6592 | −0.1185 | 0.192* | 0.725 (10) |
H52C | 0.4458 | 0.7305 | −0.0460 | 0.192* | 0.725 (10) |
N5' | 0.4459 (3) | 0.5886 (8) | −0.0002 (10) | 0.0866 (10) | 0.275 (10) |
C51' | 0.4650 (17) | 0.501 (4) | 0.037 (6) | 0.103 (7)* | 0.275 (10) |
H51D | 0.4666 | 0.5042 | 0.1116 | 0.154* | 0.275 (10) |
H51E | 0.4881 | 0.5014 | 0.0082 | 0.154* | 0.275 (10) |
H51F | 0.4530 | 0.4409 | 0.0171 | 0.154* | 0.275 (10) |
C52' | 0.463 (2) | 0.650 (5) | −0.075 (5) | 0.128 (10)* | 0.275 (10) |
H52D | 0.4493 | 0.6526 | −0.1374 | 0.192* | 0.275 (10) |
H52E | 0.4856 | 0.6223 | −0.0906 | 0.192* | 0.275 (10) |
H52F | 0.4658 | 0.7173 | −0.0481 | 0.192* | 0.275 (10) |
O6 | 0.3701 (3) | 0.7275 (7) | 0.2864 (7) | 0.096 (2) | |
C63 | 0.3867 (4) | 0.7623 (12) | 0.3582 (11) | 0.096 (2) | |
H63A | 0.3791 | 0.8246 | 0.3826 | 0.116* | |
N6 | 0.4128 (3) | 0.7255 (9) | 0.4044 (9) | 0.096 (2) | 0.725 (10) |
C61 | 0.4252 (7) | 0.6320 (19) | 0.367 (4) | 0.100 (8) | 0.725 (10) |
H61A | 0.4105 | 0.6094 | 0.3111 | 0.151* | 0.725 (10) |
H61B | 0.4248 | 0.5832 | 0.4218 | 0.151* | 0.725 (10) |
H61C | 0.4487 | 0.6400 | 0.3420 | 0.151* | 0.725 (10) |
C62 | 0.4298 (12) | 0.7679 (18) | 0.495 (3) | 0.101 (9) | 0.725 (10) |
H62A | 0.4501 | 0.8051 | 0.4732 | 0.151* | 0.725 (10) |
H62B | 0.4367 | 0.7144 | 0.5405 | 0.151* | 0.725 (10) |
H62C | 0.4139 | 0.8122 | 0.5298 | 0.151* | 0.725 (10) |
N6' | 0.4128 (3) | 0.7255 (9) | 0.4044 (9) | 0.0964 (9) | 0.275 (10) |
C61' | 0.4353 (19) | 0.642 (6) | 0.383 (11) | 0.100 (8) | 0.275 (10) |
H61D | 0.4257 | 0.6023 | 0.3274 | 0.151* | 0.275 (10) |
H61E | 0.4374 | 0.6005 | 0.4439 | 0.151* | 0.275 (10) |
H61F | 0.4580 | 0.6662 | 0.3631 | 0.151* | 0.275 (10) |
C62' | 0.426 (3) | 0.798 (6) | 0.478 (9) | 0.101 (9) | 0.275 (10) |
H62D | 0.4470 | 0.8275 | 0.4518 | 0.151* | 0.275 (10) |
H62E | 0.4307 | 0.7646 | 0.5427 | 0.151* | 0.275 (10) |
H62F | 0.4088 | 0.8498 | 0.4888 | 0.151* | 0.275 (10) |
O7 | 0.3238 (3) | 0.8291 (7) | 0.1205 (10) | 0.103 (3) | |
C73 | 0.3132 (4) | 0.8889 (10) | 0.1840 (14) | 0.103 (3) | |
H73A | 0.3265 | 0.8924 | 0.2443 | 0.124* | |
N7 | 0.2873 (3) | 0.9470 (9) | 0.1826 (13) | 0.103 (3) | 0.725 (10) |
C71 | 0.2764 (8) | 0.999 (2) | 0.2745 (17) | 0.151 (10)* | 0.725 (10) |
H71A | 0.2921 | 0.9833 | 0.3302 | 0.227* | 0.725 (10) |
H71B | 0.2532 | 0.9771 | 0.2929 | 0.227* | 0.725 (10) |
H71C | 0.2764 | 1.0701 | 0.2621 | 0.227* | 0.725 (10) |
C72 | 0.2664 (5) | 0.9541 (18) | 0.0932 (15) | 0.113 (8) | 0.725 (10) |
H72A | 0.2781 | 0.9228 | 0.0359 | 0.170* | 0.725 (10) |
H72B | 0.2621 | 1.0239 | 0.0775 | 0.170* | 0.725 (10) |
H72C | 0.2445 | 0.9206 | 0.1052 | 0.170* | 0.725 (10) |
N7' | 0.2873 (3) | 0.9470 (9) | 0.1826 (13) | 0.1033 (8) | 0.275 (10) |
C71' | 0.2675 (14) | 0.860 (3) | 0.151 (7) | 0.151 (10)* | 0.275 (10) |
H71D | 0.2780 | 0.8005 | 0.1787 | 0.227* | 0.275 (10) |
H71E | 0.2673 | 0.8566 | 0.0763 | 0.227* | 0.275 (10) |
H71F | 0.2440 | 0.8665 | 0.1758 | 0.227* | 0.275 (10) |
C72' | 0.2683 (12) | 1.040 (2) | 0.187 (6) | 0.113 (8) | 0.275 (10) |
H72D | 0.2694 | 1.0734 | 0.1212 | 0.170* | 0.275 (10) |
H72E | 0.2785 | 1.0832 | 0.2393 | 0.170* | 0.275 (10) |
H72F | 0.2444 | 1.0270 | 0.2049 | 0.170* | 0.275 (10) |
Ca1 | 0.34225 (6) | 0.66370 (19) | 0.1451 (2) | 0.0661 (6) | |
O11 | 0.40917 (15) | 0.2816 (4) | 0.6882 (5) | 0.0408 (15) | |
O12 | 0.40646 (16) | 0.1973 (4) | 0.5136 (5) | 0.0407 (14) | |
O13 | 0.37516 (15) | 0.1216 (4) | 0.6671 (5) | 0.0377 (13) | |
O14 | 0.35313 (14) | 0.2817 (4) | 0.5886 (5) | 0.0379 (13) | |
O21 | 0.49602 (19) | 0.0362 (6) | 0.4711 (6) | 0.068 (2) | |
O22 | 0.3884 (2) | 0.3864 (7) | 0.9813 (6) | 0.073 (2) | |
O23 | 0.3747 (2) | 0.0473 (6) | 0.2557 (6) | 0.066 (2) | |
O24 | 0.3183 (2) | 0.0770 (6) | 0.9329 (7) | 0.077 (3) | |
O25 | 0.4510 (2) | 0.3937 (6) | 0.3091 (7) | 0.069 (2) | |
O26 | 0.4357 (2) | −0.1064 (6) | 0.7835 (7) | 0.077 (2) | |
O27 | 0.2782 (2) | 0.3976 (7) | 0.7824 (7) | 0.080 (3) | |
O28 | 0.3450 (2) | 0.5554 (6) | 0.4446 (8) | 0.081 (3) | |
O29 | 0.4534 (2) | 0.5600 (6) | 0.6476 (7) | 0.075 (2) | |
O30 | 0.3164 (2) | −0.1115 (6) | 0.5527 (8) | 0.073 (2) | |
O31 | 0.2699 (2) | 0.2061 (6) | 0.4052 (8) | 0.083 (3) | |
O32 | 0.50381 (19) | 0.2066 (6) | 0.8129 (7) | 0.070 (2) | |
O41 | 0.46563 (17) | 0.2200 (5) | 0.4199 (6) | 0.0528 (17) | |
O42 | 0.42893 (17) | 0.0519 (5) | 0.3976 (6) | 0.0519 (17) | |
O43 | 0.47356 (17) | 0.1807 (5) | 0.6216 (5) | 0.0495 (17) | |
O44 | 0.43829 (17) | 0.0145 (5) | 0.6025 (5) | 0.0474 (16) | |
O46 | 0.37223 (19) | 0.2093 (5) | 0.8748 (5) | 0.0504 (17) | |
O47 | 0.43887 (18) | 0.2835 (5) | 0.8713 (5) | 0.0534 (17) | |
O48 | 0.35045 (17) | 0.3770 (5) | 0.7935 (6) | 0.0487 (16) | |
O49 | 0.41431 (19) | 0.4516 (5) | 0.7892 (6) | 0.0555 (18) | |
O51 | 0.34272 (16) | 0.1826 (5) | 0.3896 (5) | 0.0487 (16) | |
O52 | 0.40713 (18) | 0.2232 (5) | 0.3134 (5) | 0.0526 (17) | |
O53 | 0.36629 (16) | 0.0162 (5) | 0.4693 (6) | 0.0472 (16) | |
O56 | 0.32187 (17) | 0.0135 (5) | 0.7286 (6) | 0.0526 (18) | |
O57 | 0.38060 (19) | 0.0154 (5) | 0.8356 (6) | 0.0534 (18) | |
O58 | 0.31478 (17) | 0.2135 (5) | 0.7695 (6) | 0.0534 (18) | |
O61 | 0.38712 (18) | 0.3870 (5) | 0.4160 (6) | 0.0501 (17) | |
O62 | 0.44484 (17) | 0.3888 (5) | 0.5220 (5) | 0.0508 (17) | |
O66 | 0.37799 (17) | −0.0728 (4) | 0.6536 (6) | 0.0479 (16) | |
O67 | 0.44085 (17) | 0.1038 (5) | 0.7793 (5) | 0.0494 (16) | |
O71 | 0.28484 (16) | 0.2848 (5) | 0.5999 (6) | 0.0544 (17) | |
O72 | 0.32122 (17) | 0.4543 (5) | 0.6186 (6) | 0.0509 (17) | |
O76 | 0.39000 (17) | 0.4744 (5) | 0.5950 (6) | 0.0501 (16) | |
O77 | 0.31716 (17) | 0.3633 (5) | 0.4369 (5) | 0.0502 (17) | |
O81 | 0.47096 (18) | 0.3651 (5) | 0.7109 (6) | 0.0567 (18) | |
O86 | 0.31089 (16) | 0.1012 (5) | 0.5452 (6) | 0.0510 (18) | |
P1 | 0.38593 (6) | 0.22059 (17) | 0.61419 (19) | 0.0326 (4) | |
Mo1 | 0.45909 (2) | 0.09734 (7) | 0.50234 (8) | 0.0537 (2) | |
Mo2 | 0.39290 (2) | 0.33640 (7) | 0.86142 (8) | 0.0530 (2) | |
Mo3 | 0.38367 (2) | 0.11011 (7) | 0.36380 (8) | 0.0529 (2) | |
Mo4 | 0.34012 (3) | 0.10554 (7) | 0.82361 (8) | 0.0568 (3) | |
Mo5 | 0.43216 (3) | 0.32239 (7) | 0.39998 (8) | 0.0521 (2) | |
Mo6 | 0.41463 (2) | −0.00554 (7) | 0.73405 (8) | 0.0551 (2) | |
Mo7 | 0.31082 (2) | 0.34814 (8) | 0.71199 (8) | 0.0568 (3) | |
Mo8 | 0.35224 (2) | 0.44311 (7) | 0.49904 (9) | 0.0585 (3) | |
Mo9 | 0.43310 (3) | 0.44847 (7) | 0.65662 (8) | 0.0577 (3) | |
Mo10 | 0.34045 (2) | −0.01011 (6) | 0.58749 (8) | 0.0522 (2) | |
Mo11 | 0.30470 (2) | 0.22709 (7) | 0.47991 (9) | 0.0584 (3) | |
Mo12 | 0.46577 (2) | 0.22994 (7) | 0.75414 (8) | 0.0571 (3) |
U11 | U22 | U33 | U12 | U13 | U23 | |
C1 | 0.084 (14) | 0.076 (12) | 0.051 (12) | 0.021 (10) | −0.004 (10) | 0.026 (9) |
C1' | 0.084 (14) | 0.076 (12) | 0.051 (12) | 0.021 (10) | −0.004 (10) | 0.026 (9) |
O2 | 0.075 (5) | 0.140 (7) | 0.117 (8) | −0.003 (5) | 0.040 (5) | 0.003 (6) |
C23 | 0.075 (5) | 0.140 (7) | 0.117 (8) | −0.003 (5) | 0.040 (5) | 0.003 (6) |
N2 | 0.075 (5) | 0.140 (7) | 0.117 (8) | −0.003 (5) | 0.040 (5) | 0.003 (6) |
C21 | 0.052 (15) | 0.195 (19) | 0.21 (2) | 0.042 (15) | 0.013 (16) | −0.05 (2) |
N2' | 0.0753 (8) | 0.1399 (19) | 0.117 (2) | 0.00 (2) | 0.040 (19) | 0.003 (15) |
C21' | 0.052 (15) | 0.195 (19) | 0.21 (2) | 0.042 (15) | 0.013 (16) | −0.05 (2) |
O3 | 0.130 (6) | 0.066 (4) | 0.062 (4) | −0.002 (4) | 0.008 (4) | −0.001 (4) |
C33 | 0.130 (6) | 0.066 (4) | 0.062 (4) | −0.002 (4) | 0.008 (4) | −0.001 (4) |
N3 | 0.130 (6) | 0.066 (4) | 0.062 (4) | −0.002 (4) | 0.008 (4) | −0.001 (4) |
N3' | 0.1296 (7) | 0.0663 (12) | 0.062 (2) | −0.0018 (18) | 0.0079 (6) | −0.001 (8) |
O4 | 0.119 (6) | 0.069 (4) | 0.086 (6) | −0.022 (4) | 0.011 (5) | −0.008 (4) |
C43 | 0.119 (6) | 0.069 (4) | 0.086 (6) | −0.022 (4) | 0.011 (5) | −0.008 (4) |
N4 | 0.119 (6) | 0.069 (4) | 0.086 (6) | −0.022 (4) | 0.011 (5) | −0.008 (4) |
N4' | 0.1195 (8) | 0.0685 (15) | 0.086 (2) | −0.0222 (15) | 0.0112 (5) | −0.008 (11) |
O5 | 0.065 (4) | 0.077 (5) | 0.117 (6) | −0.010 (3) | 0.015 (4) | −0.021 (4) |
C53 | 0.065 (4) | 0.077 (5) | 0.117 (6) | −0.010 (3) | 0.015 (4) | −0.021 (4) |
N5 | 0.065 (4) | 0.077 (5) | 0.117 (6) | −0.010 (3) | 0.015 (4) | −0.021 (4) |
N5' | 0.0655 (6) | 0.0773 (15) | 0.117 (2) | −0.0104 (18) | 0.0149 (7) | −0.021 (7) |
O6 | 0.127 (7) | 0.095 (5) | 0.068 (5) | −0.019 (5) | −0.014 (4) | −0.009 (4) |
C63 | 0.127 (7) | 0.095 (5) | 0.068 (5) | −0.019 (5) | −0.014 (4) | −0.009 (4) |
N6 | 0.127 (7) | 0.095 (5) | 0.068 (5) | −0.019 (5) | −0.014 (4) | −0.009 (4) |
C61 | 0.103 (17) | 0.054 (9) | 0.144 (19) | −0.021 (12) | 0.050 (18) | −0.022 (10) |
C62 | 0.129 (18) | 0.084 (19) | 0.090 (18) | 0.030 (17) | −0.033 (12) | −0.022 (19) |
N6' | 0.1267 (7) | 0.0948 (19) | 0.068 (4) | −0.019 (19) | −0.014 (9) | −0.009 (17) |
C61' | 0.103 (17) | 0.054 (9) | 0.144 (19) | −0.021 (12) | 0.050 (18) | −0.022 (10) |
C62' | 0.129 (18) | 0.084 (19) | 0.090 (18) | 0.030 (17) | −0.033 (12) | −0.022 (19) |
O7 | 0.093 (5) | 0.077 (5) | 0.140 (8) | 0.016 (4) | 0.013 (5) | −0.017 (5) |
C73 | 0.093 (5) | 0.077 (5) | 0.140 (8) | 0.016 (4) | 0.013 (5) | −0.017 (5) |
N7 | 0.093 (5) | 0.077 (5) | 0.140 (8) | 0.016 (4) | 0.013 (5) | −0.017 (5) |
C72 | 0.101 (16) | 0.110 (18) | 0.13 (2) | 0.003 (13) | 0.027 (16) | 0.024 (15) |
N7' | 0.0930 (8) | 0.077 (2) | 0.1405 (17) | 0.0159 (18) | 0.0134 (5) | −0.017 (10) |
C72' | 0.101 (16) | 0.110 (18) | 0.13 (2) | 0.003 (13) | 0.027 (16) | 0.024 (15) |
Ca1 | 0.0601 (14) | 0.0661 (15) | 0.0721 (17) | −0.0027 (11) | 0.0079 (12) | −0.0057 (13) |
O11 | 0.033 (3) | 0.045 (4) | 0.045 (4) | 0.002 (3) | −0.005 (3) | −0.011 (3) |
O12 | 0.045 (3) | 0.038 (3) | 0.039 (4) | 0.007 (3) | 0.005 (3) | −0.004 (3) |
O13 | 0.035 (3) | 0.037 (3) | 0.041 (4) | 0.004 (2) | −0.001 (3) | −0.010 (3) |
O14 | 0.032 (3) | 0.039 (3) | 0.043 (3) | 0.003 (2) | 0.001 (3) | −0.011 (3) |
O21 | 0.062 (4) | 0.084 (6) | 0.059 (5) | 0.036 (4) | 0.014 (4) | 0.000 (4) |
O22 | 0.091 (6) | 0.082 (6) | 0.046 (5) | −0.020 (4) | 0.011 (4) | −0.029 (4) |
O23 | 0.061 (4) | 0.079 (5) | 0.057 (5) | −0.001 (4) | 0.000 (4) | −0.026 (4) |
O24 | 0.103 (7) | 0.071 (5) | 0.057 (5) | −0.001 (5) | 0.037 (5) | 0.004 (4) |
O25 | 0.082 (6) | 0.062 (5) | 0.064 (5) | 0.000 (4) | 0.028 (4) | 0.003 (4) |
O26 | 0.072 (5) | 0.069 (5) | 0.089 (7) | 0.015 (4) | −0.009 (5) | 0.026 (5) |
O27 | 0.065 (5) | 0.098 (6) | 0.077 (6) | 0.026 (5) | 0.005 (5) | −0.025 (5) |
O28 | 0.085 (6) | 0.059 (5) | 0.100 (7) | 0.014 (4) | 0.004 (5) | 0.023 (5) |
O29 | 0.086 (6) | 0.052 (5) | 0.087 (6) | −0.022 (4) | 0.003 (5) | −0.012 (4) |
O30 | 0.066 (5) | 0.048 (4) | 0.107 (7) | −0.020 (4) | −0.003 (5) | −0.015 (4) |
O31 | 0.057 (5) | 0.077 (5) | 0.113 (8) | 0.013 (4) | −0.030 (5) | −0.026 (5) |
O32 | 0.052 (4) | 0.080 (5) | 0.077 (6) | 0.002 (4) | −0.030 (4) | −0.011 (5) |
O41 | 0.043 (4) | 0.060 (4) | 0.055 (4) | 0.005 (3) | 0.002 (3) | −0.007 (4) |
O42 | 0.048 (4) | 0.060 (4) | 0.048 (4) | 0.016 (3) | 0.003 (3) | −0.004 (3) |
O43 | 0.045 (4) | 0.060 (4) | 0.044 (4) | −0.001 (3) | −0.003 (3) | −0.009 (3) |
O44 | 0.056 (4) | 0.040 (3) | 0.046 (4) | 0.004 (3) | 0.005 (3) | −0.009 (3) |
O46 | 0.070 (4) | 0.042 (4) | 0.040 (4) | 0.001 (3) | 0.003 (3) | −0.005 (3) |
O47 | 0.059 (4) | 0.056 (4) | 0.046 (4) | 0.001 (3) | −0.008 (3) | −0.011 (3) |
O48 | 0.045 (4) | 0.052 (4) | 0.049 (4) | 0.001 (3) | 0.006 (3) | −0.012 (3) |
O49 | 0.064 (4) | 0.038 (4) | 0.065 (5) | −0.006 (3) | −0.003 (4) | −0.011 (3) |
O51 | 0.041 (3) | 0.053 (4) | 0.052 (4) | 0.008 (3) | 0.001 (3) | −0.010 (3) |
O52 | 0.058 (4) | 0.057 (4) | 0.043 (4) | 0.009 (3) | 0.000 (3) | −0.003 (3) |
O53 | 0.045 (3) | 0.040 (3) | 0.056 (4) | 0.002 (3) | 0.002 (3) | −0.019 (3) |
O56 | 0.046 (4) | 0.044 (4) | 0.068 (5) | −0.010 (3) | 0.012 (4) | −0.005 (3) |
O57 | 0.060 (4) | 0.054 (4) | 0.046 (4) | −0.001 (3) | 0.000 (3) | 0.006 (3) |
O58 | 0.043 (4) | 0.055 (4) | 0.062 (5) | −0.004 (3) | 0.014 (3) | −0.014 (4) |
O61 | 0.058 (4) | 0.044 (4) | 0.048 (4) | 0.009 (3) | −0.005 (3) | 0.005 (3) |
O62 | 0.053 (4) | 0.050 (4) | 0.050 (4) | −0.006 (3) | 0.001 (3) | −0.005 (3) |
O66 | 0.056 (4) | 0.037 (3) | 0.052 (4) | −0.002 (3) | 0.004 (3) | −0.013 (3) |
O67 | 0.052 (4) | 0.055 (4) | 0.042 (4) | 0.003 (3) | −0.001 (3) | −0.012 (3) |
O71 | 0.040 (3) | 0.061 (4) | 0.062 (5) | 0.005 (3) | 0.001 (3) | −0.017 (4) |
O72 | 0.048 (4) | 0.046 (4) | 0.058 (5) | 0.011 (3) | 0.009 (3) | −0.009 (3) |
O76 | 0.055 (4) | 0.037 (3) | 0.057 (4) | 0.002 (3) | 0.001 (3) | −0.004 (3) |
O77 | 0.046 (4) | 0.059 (4) | 0.046 (4) | 0.014 (3) | 0.001 (3) | −0.004 (3) |
O81 | 0.053 (4) | 0.056 (4) | 0.062 (5) | −0.015 (3) | −0.006 (4) | −0.004 (4) |
O86 | 0.036 (3) | 0.052 (4) | 0.066 (5) | −0.006 (3) | 0.003 (3) | −0.011 (3) |
P1 | 0.0310 (10) | 0.0315 (10) | 0.0351 (11) | 0.0019 (8) | 0.0027 (8) | −0.0062 (9) |
Mo1 | 0.0477 (5) | 0.0669 (6) | 0.0465 (5) | 0.0236 (4) | 0.0063 (4) | −0.0017 (5) |
Mo2 | 0.0562 (5) | 0.0593 (6) | 0.0435 (5) | −0.0078 (4) | 0.0025 (4) | −0.0203 (4) |
Mo3 | 0.0525 (5) | 0.0628 (6) | 0.0434 (5) | −0.0007 (4) | 0.0036 (4) | −0.0211 (4) |
Mo4 | 0.0704 (6) | 0.0470 (5) | 0.0529 (6) | −0.0075 (4) | 0.0228 (5) | −0.0055 (4) |
Mo5 | 0.0598 (5) | 0.0493 (5) | 0.0472 (5) | −0.0006 (4) | 0.0153 (4) | 0.0003 (4) |
Mo6 | 0.0530 (5) | 0.0458 (5) | 0.0665 (7) | 0.0051 (4) | −0.0007 (5) | 0.0107 (4) |
Mo7 | 0.0475 (5) | 0.0682 (6) | 0.0546 (6) | 0.0190 (4) | 0.0084 (4) | −0.0118 (5) |
Mo8 | 0.0529 (5) | 0.0461 (5) | 0.0765 (7) | 0.0123 (4) | 0.0028 (5) | 0.0092 (5) |
Mo9 | 0.0681 (6) | 0.0447 (5) | 0.0604 (6) | −0.0197 (4) | −0.0015 (5) | −0.0075 (4) |
Mo10 | 0.0550 (5) | 0.0412 (5) | 0.0604 (6) | −0.0138 (4) | −0.0013 (5) | −0.0105 (4) |
Mo11 | 0.0459 (5) | 0.0578 (6) | 0.0716 (7) | 0.0133 (4) | −0.0185 (5) | −0.0237 (5) |
Mo12 | 0.0428 (5) | 0.0623 (6) | 0.0662 (6) | 0.0047 (4) | −0.0152 (5) | −0.0185 (5) |
C1—N1 | 1.355 (8) | N6—C61 | 1.411 (13) |
C1—C2 | 1.369 (12) | N6—C62 | 1.445 (13) |
C1—H1A | 0.9300 | C61—H61A | 0.9600 |
C2—C3 | 1.347 (12) | C61—H61B | 0.9600 |
C2—H2A | 0.9300 | C61—H61C | 0.9600 |
C3—C4 | 1.333 (11) | C62—H62A | 0.9600 |
C3—C6 | 1.51 (2) | C62—H62B | 0.9600 |
C4—C5 | 1.353 (11) | C62—H62C | 0.9600 |
C4—H4A | 0.9300 | C61'—H61D | 0.9600 |
C5—N1 | 1.346 (8) | C61'—H61E | 0.9600 |
C5—H5A | 0.9300 | C61'—H61F | 0.9600 |
C6—H6A | 0.9600 | C62'—H62D | 0.9600 |
C6—H6B | 0.9600 | C62'—H62E | 0.9600 |
C6—H6C | 0.9600 | C62'—H62F | 0.9600 |
C7—N1 | 1.50 (2) | O7—C73 | 1.209 (13) |
C7—H7A | 0.9600 | O7—Ca1 | 2.324 (10) |
C7—H7B | 0.9600 | C73—N7 | 1.255 (12) |
C7—H7C | 0.9600 | C73—H73A | 0.9300 |
C1'—N1' | 1.354 (8) | N7—C72 | 1.408 (13) |
C1'—C2' | 1.370 (13) | N7—C71 | 1.431 (14) |
C1'—H1'A | 0.9300 | C71—H71A | 0.9600 |
C2'—C3' | 1.346 (13) | C71—H71B | 0.9600 |
C2'—H2'A | 0.9300 | C71—H71C | 0.9600 |
C3'—C6' | 1.51 (2) | C72—H72A | 0.9600 |
C5'—N1' | 1.349 (8) | C72—H72B | 0.9600 |
C5'—H5'A | 0.9300 | C72—H72C | 0.9600 |
C6'—H6'A | 0.9600 | C71'—H71D | 0.9600 |
C6'—H6'B | 0.9600 | C71'—H71E | 0.9600 |
C6'—H6'C | 0.9600 | C71'—H71F | 0.9600 |
C7'—N1' | 1.51 (2) | C72'—H72D | 0.9600 |
C7'—H7'A | 0.9600 | C72'—H72E | 0.9600 |
C7'—H7'B | 0.9600 | C72'—H72F | 0.9600 |
C7'—H7'C | 0.9600 | O11—P1 | 1.535 (6) |
O2—C23 | 1.239 (13) | O11—Mo12 | 2.426 (6) |
O2—Ca1 | 2.289 (10) | O11—Mo9 | 2.427 (6) |
C23—N2 | 1.259 (13) | O11—Mo2 | 2.429 (6) |
C23—H23A | 0.9300 | O12—P1 | 1.547 (7) |
N2—C22 | 1.403 (14) | O12—Mo3 | 2.413 (6) |
N2—C21 | 1.417 (14) | O12—Mo1 | 2.416 (6) |
C21—H21A | 0.9600 | O12—Mo5 | 2.420 (6) |
C21—H21B | 0.9600 | O13—P1 | 1.534 (6) |
C21—H21C | 0.9600 | O13—Mo6 | 2.422 (6) |
C22—H22A | 0.9600 | O13—Mo10 | 2.422 (6) |
C22—H22B | 0.9600 | O13—Mo4 | 2.432 (6) |
C22—H22C | 0.9600 | O14—P1 | 1.530 (6) |
C21'—H21D | 0.9600 | O14—Mo8 | 2.430 (6) |
C21'—H21E | 0.9600 | O14—Mo11 | 2.434 (6) |
C21'—H21F | 0.9600 | O14—Mo7 | 2.435 (6) |
C22'—H22D | 0.9600 | O21—Mo1 | 1.678 (6) |
C22'—H22E | 0.9600 | O22—Mo2 | 1.690 (7) |
C22'—H22F | 0.9600 | O23—Mo3 | 1.659 (7) |
O3—C33 | 1.212 (11) | O24—Mo4 | 1.681 (8) |
O3—Ca1 | 2.278 (9) | O25—Mo5 | 1.669 (8) |
C33—N3 | 1.271 (12) | O26—Mo6 | 1.686 (8) |
C33—H33A | 0.9300 | O27—Mo7 | 1.677 (8) |
N3—C31 | 1.430 (13) | O28—Mo8 | 1.668 (8) |
N3—C32 | 1.441 (14) | O29—Mo9 | 1.674 (7) |
C31—H31A | 0.9600 | O30—Mo10 | 1.689 (7) |
C31—H31B | 0.9600 | O31—Mo11 | 1.668 (8) |
C31—H31C | 0.9600 | O32—Mo12 | 1.671 (7) |
C32—H32A | 0.9600 | O41—Mo5 | 1.884 (7) |
C32—H32B | 0.9600 | O41—Mo1 | 1.958 (7) |
C32—H32C | 0.9600 | O42—Mo1 | 1.876 (7) |
C31'—H31D | 0.9600 | O42—Mo3 | 1.946 (6) |
C31'—H31E | 0.9600 | O43—Mo12 | 1.853 (7) |
C31'—H31F | 0.9600 | O43—Mo1 | 1.972 (7) |
C32'—H32D | 0.9600 | O44—Mo1 | 1.872 (7) |
C32'—H32E | 0.9600 | O44—Mo6 | 1.941 (7) |
C32'—H32F | 0.9600 | O46—Mo2 | 1.869 (7) |
O4—C43 | 1.235 (12) | O46—Mo4 | 1.959 (7) |
O4—Ca1 | 2.289 (11) | O47—Mo2 | 1.899 (7) |
C43—N4 | 1.253 (12) | O47—Mo12 | 1.960 (7) |
C43—H43A | 0.9300 | O48—Mo7 | 1.884 (7) |
N4—C41 | 1.434 (14) | O48—Mo2 | 1.923 (7) |
N4—C42 | 1.441 (13) | O49—Mo9 | 1.855 (8) |
C41—H41A | 0.9600 | O49—Mo2 | 1.966 (7) |
C41—H41B | 0.9600 | O51—Mo3 | 1.869 (6) |
C41—H41C | 0.9600 | O51—Mo11 | 1.955 (6) |
C42—H42A | 0.9600 | O52—Mo3 | 1.864 (7) |
C42—H42B | 0.9600 | O52—Mo5 | 1.972 (7) |
C42—H42C | 0.9600 | O53—Mo10 | 1.850 (7) |
C41'—H41D | 0.9600 | O53—Mo3 | 1.959 (7) |
C41'—H41E | 0.9600 | O56—Mo4 | 1.864 (7) |
C41'—H41F | 0.9600 | O56—Mo10 | 1.978 (8) |
C42'—H42D | 0.9600 | O57—Mo6 | 1.868 (7) |
C42'—H42E | 0.9600 | O57—Mo4 | 1.963 (7) |
C42'—H42F | 0.9600 | O58—Mo4 | 1.864 (7) |
O5—C53 | 1.238 (12) | O58—Mo7 | 1.937 (7) |
O5—Ca1 | 2.329 (9) | O61—Mo8 | 1.866 (7) |
C53—N5 | 1.266 (12) | O61—Mo5 | 1.936 (7) |
C53—H53A | 0.9300 | O62—Mo5 | 1.866 (7) |
N5—C52 | 1.430 (14) | O62—Mo9 | 1.959 (7) |
N5—C51 | 1.435 (13) | O66—Mo10 | 1.866 (7) |
C51—H51A | 0.9600 | O66—Mo6 | 1.959 (7) |
C51—H51B | 0.9600 | O67—Mo6 | 1.857 (7) |
C51—H51C | 0.9600 | O67—Mo12 | 1.951 (7) |
C52—H52A | 0.9600 | O71—Mo11 | 1.885 (7) |
C52—H52B | 0.9600 | O71—Mo7 | 1.945 (7) |
C52—H52C | 0.9600 | O72—Mo7 | 1.894 (7) |
C51'—H51D | 0.9600 | O72—Mo8 | 1.951 (7) |
C51'—H51E | 0.9600 | O76—Mo9 | 1.863 (7) |
C51'—H51F | 0.9600 | O76—Mo8 | 1.948 (7) |
C52'—H52D | 0.9600 | O77—Mo8 | 1.888 (7) |
C52'—H52E | 0.9600 | O77—Mo11 | 1.947 (7) |
C52'—H52F | 0.9600 | O81—Mo12 | 1.885 (7) |
O6—C63 | 1.212 (12) | O81—Mo9 | 1.952 (7) |
O6—Ca1 | 2.275 (10) | O86—Mo11 | 1.883 (7) |
C63—N6 | 1.262 (13) | O86—Mo10 | 1.937 (7) |
C63—H63A | 0.9300 | ||
N1—C1—C2 | 119.6 (14) | Mo3—O12—Mo1 | 89.5 (2) |
N1—C1—H1A | 120.2 | P1—O12—Mo5 | 125.3 (3) |
C2—C1—H1A | 120.2 | Mo3—O12—Mo5 | 89.5 (2) |
C3—C2—C1 | 119.6 (16) | Mo1—O12—Mo5 | 90.0 (2) |
C3—C2—H2A | 120.2 | P1—O13—Mo6 | 125.8 (3) |
C1—C2—H2A | 120.2 | P1—O13—Mo10 | 125.1 (4) |
C4—C3—C2 | 118.8 (15) | Mo6—O13—Mo10 | 89.55 (18) |
C4—C3—C6 | 121.5 (11) | P1—O13—Mo4 | 126.3 (3) |
C2—C3—C6 | 119.6 (10) | Mo6—O13—Mo4 | 89.3 (2) |
C3—C4—C5 | 123.6 (15) | Mo10—O13—Mo4 | 89.2 (2) |
C3—C4—H4A | 118.2 | P1—O14—Mo8 | 125.4 (3) |
C5—C4—H4A | 118.2 | P1—O14—Mo11 | 126.3 (3) |
N1—C5—C4 | 117.0 (15) | Mo8—O14—Mo11 | 88.7 (2) |
N1—C5—H5A | 121.5 | P1—O14—Mo7 | 126.6 (4) |
C4—C5—H5A | 121.5 | Mo8—O14—Mo7 | 89.02 (19) |
C3—C6—H6A | 109.5 | Mo11—O14—Mo7 | 88.64 (18) |
C3—C6—H6B | 109.5 | Mo5—O41—Mo1 | 125.8 (4) |
H6A—C6—H6B | 109.5 | Mo1—O42—Mo3 | 125.6 (4) |
C3—C6—H6C | 109.5 | Mo12—O43—Mo1 | 150.5 (4) |
H6A—C6—H6C | 109.5 | Mo1—O44—Mo6 | 151.8 (4) |
H6B—C6—H6C | 109.5 | Mo2—O46—Mo4 | 150.1 (4) |
N1—C7—H7A | 109.5 | Mo2—O47—Mo12 | 124.7 (4) |
N1—C7—H7B | 109.5 | Mo7—O48—Mo2 | 151.3 (4) |
H7A—C7—H7B | 109.5 | Mo9—O49—Mo2 | 125.5 (3) |
N1—C7—H7C | 109.5 | Mo3—O51—Mo11 | 152.4 (4) |
H7A—C7—H7C | 109.5 | Mo3—O52—Mo5 | 124.9 (4) |
H7B—C7—H7C | 109.5 | Mo10—O53—Mo3 | 150.8 (3) |
C5—N1—C1 | 121.4 (13) | Mo4—O56—Mo10 | 124.9 (3) |
C5—N1—C7 | 119.6 (9) | Mo6—O57—Mo4 | 125.9 (4) |
C1—N1—C7 | 119.0 (8) | Mo4—O58—Mo7 | 152.9 (4) |
N1'—C1'—C2' | 119.7 (16) | Mo8—O61—Mo5 | 151.0 (4) |
N1'—C1'—H1'A | 120.1 | Mo5—O62—Mo9 | 151.3 (4) |
C2'—C1'—H1'A | 120.1 | Mo10—O66—Mo6 | 126.2 (3) |
C3'—C2'—C1' | 119.7 (17) | Mo6—O67—Mo12 | 151.7 (4) |
C3'—C2'—H2'A | 120.1 | Mo11—O71—Mo7 | 125.3 (3) |
C1'—C2'—H2'A | 120.1 | Mo7—O72—Mo8 | 125.0 (3) |
C2'—C3'—C6' | 120.2 (10) | Mo9—O76—Mo8 | 152.7 (4) |
N1'—C5'—H5'A | 121.7 | Mo8—O77—Mo11 | 124.9 (4) |
C3'—C6'—H6'A | 109.5 | Mo12—O81—Mo9 | 124.4 (3) |
C3'—C6'—H6'B | 109.5 | Mo11—O86—Mo10 | 150.9 (4) |
H6'A—C6'—H6'B | 109.5 | O14—P1—O13 | 109.1 (3) |
C3'—C6'—H6'C | 109.5 | O14—P1—O11 | 109.4 (3) |
H6'A—C6'—H6'C | 109.5 | O13—P1—O11 | 109.2 (4) |
H6'B—C6'—H6'C | 109.5 | O14—P1—O12 | 110.0 (4) |
N1'—C7'—H7'A | 109.5 | O13—P1—O12 | 109.8 (3) |
N1'—C7'—H7'B | 109.5 | O11—P1—O12 | 109.3 (3) |
H7'A—C7'—H7'B | 109.5 | O21—Mo1—O44 | 103.9 (3) |
N1'—C7'—H7'C | 109.5 | O21—Mo1—O42 | 101.0 (4) |
H7'A—C7'—H7'C | 109.5 | O44—Mo1—O42 | 92.6 (3) |
H7'B—C7'—H7'C | 109.5 | O21—Mo1—O41 | 99.3 (3) |
C5'—N1'—C1' | 120.9 (14) | O44—Mo1—O41 | 156.3 (3) |
C5'—N1'—C7' | 119.7 (10) | O42—Mo1—O41 | 87.4 (3) |
C1'—N1'—C7' | 118.9 (9) | O21—Mo1—O43 | 102.7 (4) |
C23—O2—Ca1 | 137.7 (11) | O44—Mo1—O43 | 84.9 (3) |
O2—C23—N2 | 126.6 (18) | O42—Mo1—O43 | 156.0 (3) |
O2—C23—H23A | 116.7 | O41—Mo1—O43 | 85.6 (3) |
N2—C23—H23A | 116.7 | O21—Mo1—O12 | 169.0 (3) |
C23—N2—C22 | 113.3 (19) | O44—Mo1—O12 | 85.7 (2) |
C23—N2—C21 | 126.5 (19) | O42—Mo1—O12 | 72.9 (2) |
C22—N2—C21 | 119.9 (15) | O41—Mo1—O12 | 71.6 (2) |
N2—C21—H21A | 109.5 | O43—Mo1—O12 | 83.1 (2) |
N2—C21—H21B | 109.5 | O22—Mo2—O46 | 103.0 (4) |
H21A—C21—H21B | 109.5 | O22—Mo2—O47 | 100.3 (4) |
N2—C21—H21C | 109.5 | O46—Mo2—O47 | 93.1 (3) |
H21A—C21—H21C | 109.5 | O22—Mo2—O48 | 102.7 (4) |
H21B—C21—H21C | 109.5 | O46—Mo2—O48 | 86.3 (3) |
N2—C22—H22A | 109.5 | O47—Mo2—O48 | 156.5 (3) |
N2—C22—H22B | 109.5 | O22—Mo2—O49 | 99.9 (4) |
H22A—C22—H22B | 109.5 | O46—Mo2—O49 | 156.9 (3) |
N2—C22—H22C | 109.5 | O47—Mo2—O49 | 86.1 (3) |
H22A—C22—H22C | 109.5 | O48—Mo2—O49 | 85.4 (3) |
H22B—C22—H22C | 109.5 | O22—Mo2—O11 | 169.7 (3) |
H21D—C21'—H21E | 109.5 | O46—Mo2—O11 | 85.7 (2) |
H21D—C21'—H21F | 109.5 | O47—Mo2—O11 | 73.3 (2) |
H21E—C21'—H21F | 109.5 | O48—Mo2—O11 | 83.2 (2) |
H22D—C22'—H22E | 109.5 | O49—Mo2—O11 | 71.9 (3) |
H22D—C22'—H22F | 109.5 | O23—Mo3—O52 | 102.1 (4) |
H22E—C22'—H22F | 109.5 | O23—Mo3—O51 | 103.5 (3) |
C33—O3—Ca1 | 163.6 (11) | O52—Mo3—O51 | 93.1 (3) |
O3—C33—N3 | 129.5 (15) | O23—Mo3—O42 | 100.0 (3) |
O3—C33—H33A | 115.2 | O52—Mo3—O42 | 88.1 (3) |
N3—C33—H33A | 115.2 | O51—Mo3—O42 | 155.7 (3) |
C33—N3—C31 | 126.2 (15) | O23—Mo3—O53 | 101.2 (4) |
C33—N3—C32 | 118.3 (15) | O52—Mo3—O53 | 156.3 (3) |
C31—N3—C32 | 115.4 (13) | O51—Mo3—O53 | 85.3 (3) |
N3—C31—H31A | 109.5 | O42—Mo3—O53 | 84.0 (3) |
N3—C31—H31B | 109.5 | O23—Mo3—O12 | 170.7 (3) |
H31A—C31—H31B | 109.5 | O52—Mo3—O12 | 73.7 (3) |
N3—C31—H31C | 109.5 | O51—Mo3—O12 | 85.1 (2) |
H31A—C31—H31C | 109.5 | O42—Mo3—O12 | 71.9 (2) |
H31B—C31—H31C | 109.5 | O53—Mo3—O12 | 82.6 (2) |
N3—C32—H32A | 109.5 | O24—Mo4—O58 | 103.1 (4) |
N3—C32—H32B | 109.5 | O24—Mo4—O56 | 102.5 (4) |
H32A—C32—H32B | 109.5 | O58—Mo4—O56 | 93.5 (3) |
N3—C32—H32C | 109.5 | O24—Mo4—O46 | 100.8 (4) |
H32A—C32—H32C | 109.5 | O58—Mo4—O46 | 85.1 (3) |
H32B—C32—H32C | 109.5 | O56—Mo4—O46 | 156.3 (3) |
H31D—C31'—H31E | 109.5 | O24—Mo4—O57 | 101.0 (4) |
H31D—C31'—H31F | 109.5 | O58—Mo4—O57 | 155.1 (3) |
H31E—C31'—H31F | 109.5 | O56—Mo4—O57 | 87.1 (3) |
H32D—C32'—H32E | 109.5 | O46—Mo4—O57 | 84.5 (3) |
H32D—C32'—H32F | 109.5 | O24—Mo4—O13 | 171.5 (3) |
H32E—C32'—H32F | 109.5 | O58—Mo4—O13 | 84.8 (3) |
C43—O4—Ca1 | 143.5 (11) | O56—Mo4—O13 | 73.7 (3) |
O4—C43—N4 | 131.0 (15) | O46—Mo4—O13 | 82.6 (2) |
O4—C43—H43A | 114.5 | O57—Mo4—O13 | 71.5 (3) |
N4—C43—H43A | 114.5 | O25—Mo5—O62 | 102.3 (4) |
C43—N4—C41 | 118.2 (16) | O25—Mo5—O41 | 102.0 (4) |
C43—N4—C42 | 125.6 (14) | O62—Mo5—O41 | 92.8 (3) |
C41—N4—C42 | 115.5 (13) | O25—Mo5—O61 | 102.1 (4) |
N4—C41—H41A | 109.5 | O62—Mo5—O61 | 86.2 (3) |
N4—C41—H41B | 109.5 | O41—Mo5—O61 | 155.5 (3) |
H41A—C41—H41B | 109.5 | O25—Mo5—O52 | 100.9 (4) |
N4—C41—H41C | 109.5 | O62—Mo5—O52 | 156.5 (3) |
H41A—C41—H41C | 109.5 | O41—Mo5—O52 | 85.9 (3) |
H41B—C41—H41C | 109.5 | O61—Mo5—O52 | 85.5 (3) |
N4—C42—H42A | 109.5 | O25—Mo5—O12 | 171.1 (3) |
N4—C42—H42B | 109.5 | O62—Mo5—O12 | 85.4 (3) |
H42A—C42—H42B | 109.5 | O41—Mo5—O12 | 72.6 (3) |
N4—C42—H42C | 109.5 | O61—Mo5—O12 | 82.9 (2) |
H42A—C42—H42C | 109.5 | O52—Mo5—O12 | 71.9 (3) |
H42B—C42—H42C | 109.5 | O26—Mo6—O67 | 103.9 (4) |
H41D—C41'—H41E | 109.5 | O26—Mo6—O57 | 100.8 (4) |
H41D—C41'—H41F | 109.5 | O67—Mo6—O57 | 92.4 (3) |
H41E—C41'—H41F | 109.5 | O26—Mo6—O44 | 102.4 (4) |
H42D—C42'—H42E | 109.5 | O67—Mo6—O44 | 85.1 (3) |
H42D—C42'—H42F | 109.5 | O57—Mo6—O44 | 156.6 (3) |
H42E—C42'—H42F | 109.5 | O26—Mo6—O66 | 100.5 (4) |
C53—O5—Ca1 | 134.1 (9) | O67—Mo6—O66 | 155.3 (3) |
O5—C53—N5 | 127.9 (14) | O57—Mo6—O66 | 86.5 (3) |
O5—C53—H53A | 116.1 | O44—Mo6—O66 | 86.2 (3) |
N5—C53—H53A | 116.1 | O26—Mo6—O13 | 169.9 (3) |
C53—N5—C52 | 115.5 (15) | O67—Mo6—O13 | 84.6 (3) |
C53—N5—C51 | 127.9 (15) | O57—Mo6—O13 | 73.2 (3) |
C52—N5—C51 | 116.2 (13) | O44—Mo6—O13 | 83.4 (2) |
N5—C51—H51A | 109.5 | O66—Mo6—O13 | 71.4 (2) |
N5—C51—H51B | 109.5 | O27—Mo7—O48 | 102.7 (4) |
H51A—C51—H51B | 109.5 | O27—Mo7—O72 | 102.1 (4) |
N5—C51—H51C | 109.5 | O48—Mo7—O72 | 91.9 (3) |
H51A—C51—H51C | 109.5 | O27—Mo7—O58 | 102.2 (4) |
H51B—C51—H51C | 109.5 | O48—Mo7—O58 | 84.9 (3) |
N5—C52—H52A | 109.5 | O72—Mo7—O58 | 155.6 (3) |
N5—C52—H52B | 109.5 | O27—Mo7—O71 | 100.9 (4) |
H52A—C52—H52B | 109.5 | O48—Mo7—O71 | 156.0 (3) |
N5—C52—H52C | 109.5 | O72—Mo7—O71 | 87.5 (3) |
H52A—C52—H52C | 109.5 | O58—Mo7—O71 | 85.8 (3) |
H52B—C52—H52C | 109.5 | O27—Mo7—O14 | 171.9 (4) |
H51D—C51'—H51E | 109.5 | O48—Mo7—O14 | 84.3 (2) |
H51D—C51'—H51F | 109.5 | O72—Mo7—O14 | 73.3 (2) |
H51E—C51'—H51F | 109.5 | O58—Mo7—O14 | 82.2 (2) |
H52D—C52'—H52E | 109.5 | O71—Mo7—O14 | 72.5 (2) |
H52D—C52'—H52F | 109.5 | O28—Mo8—O61 | 103.5 (4) |
H52E—C52'—H52F | 109.5 | O28—Mo8—O77 | 101.6 (4) |
C63—O6—Ca1 | 176.2 (12) | O61—Mo8—O77 | 92.4 (3) |
O6—C63—N6 | 128.9 (16) | O28—Mo8—O76 | 101.6 (4) |
O6—C63—H63A | 115.6 | O61—Mo8—O76 | 85.3 (3) |
N6—C63—H63A | 115.6 | O77—Mo8—O76 | 156.5 (3) |
C63—N6—C61 | 116.3 (17) | O28—Mo8—O72 | 99.4 (4) |
C63—N6—C62 | 125.9 (15) | O61—Mo8—O72 | 156.8 (3) |
C61—N6—C62 | 117.7 (14) | O77—Mo8—O72 | 86.8 (3) |
N6—C61—H61A | 109.5 | O76—Mo8—O72 | 86.2 (3) |
N6—C61—H61B | 109.5 | O28—Mo8—O14 | 170.7 (3) |
H61A—C61—H61B | 109.5 | O61—Mo8—O14 | 84.9 (2) |
N6—C61—H61C | 109.5 | O77—Mo8—O14 | 73.7 (3) |
H61A—C61—H61C | 109.5 | O76—Mo8—O14 | 82.8 (2) |
H61B—C61—H61C | 109.5 | O72—Mo8—O14 | 72.6 (2) |
N6—C62—H62A | 109.5 | O29—Mo9—O49 | 103.0 (4) |
N6—C62—H62B | 109.5 | O29—Mo9—O76 | 102.7 (4) |
H62A—C62—H62B | 109.5 | O49—Mo9—O76 | 92.6 (3) |
N6—C62—H62C | 109.5 | O29—Mo9—O81 | 100.3 (4) |
H62A—C62—H62C | 109.5 | O49—Mo9—O81 | 88.3 (3) |
H62B—C62—H62C | 109.5 | O76—Mo9—O81 | 156.2 (3) |
H61D—C61'—H61E | 109.5 | O29—Mo9—O62 | 100.8 (4) |
H61D—C61'—H61F | 109.5 | O49—Mo9—O62 | 156.1 (3) |
H61E—C61'—H61F | 109.5 | O76—Mo9—O62 | 84.3 (3) |
H62D—C62'—H62E | 109.5 | O81—Mo9—O62 | 85.4 (3) |
H62D—C62'—H62F | 109.5 | O29—Mo9—O11 | 172.3 (4) |
H62E—C62'—H62F | 109.5 | O49—Mo9—O11 | 73.7 (3) |
C73—O7—Ca1 | 128.8 (11) | O76—Mo9—O11 | 84.5 (2) |
O7—C73—N7 | 131.1 (18) | O81—Mo9—O11 | 72.8 (2) |
O7—C73—H73A | 114.5 | O62—Mo9—O11 | 82.4 (2) |
N7—C73—H73A | 114.5 | O30—Mo10—O53 | 102.9 (4) |
C73—N7—C72 | 120.2 (17) | O30—Mo10—O66 | 100.8 (4) |
C73—N7—C71 | 120.8 (19) | O53—Mo10—O66 | 92.8 (3) |
C72—N7—C71 | 118.6 (13) | O30—Mo10—O86 | 102.3 (4) |
N7—C71—H71A | 109.5 | O53—Mo10—O86 | 86.4 (3) |
N7—C71—H71B | 109.5 | O66—Mo10—O86 | 156.5 (3) |
H71A—C71—H71B | 109.5 | O30—Mo10—O56 | 100.0 (4) |
N7—C71—H71C | 109.5 | O53—Mo10—O56 | 156.9 (3) |
H71A—C71—H71C | 109.5 | O66—Mo10—O56 | 85.8 (3) |
H71B—C71—H71C | 109.5 | O86—Mo10—O56 | 85.9 (3) |
N7—C72—H72A | 109.5 | O30—Mo10—O13 | 170.0 (4) |
N7—C72—H72B | 109.5 | O53—Mo10—O13 | 85.4 (2) |
H72A—C72—H72B | 109.5 | O66—Mo10—O13 | 72.8 (2) |
N7—C72—H72C | 109.5 | O86—Mo10—O13 | 83.8 (2) |
H72A—C72—H72C | 109.5 | O56—Mo10—O13 | 72.2 (2) |
H72B—C72—H72C | 109.5 | O31—Mo11—O86 | 102.2 (4) |
H71D—C71'—H71E | 109.5 | O31—Mo11—O71 | 102.6 (4) |
H71D—C71'—H71F | 109.5 | O86—Mo11—O71 | 92.5 (3) |
H71E—C71'—H71F | 109.5 | O31—Mo11—O77 | 100.7 (4) |
H72D—C72'—H72E | 109.5 | O86—Mo11—O77 | 156.5 (3) |
H72D—C72'—H72F | 109.5 | O71—Mo11—O77 | 87.5 (3) |
H72E—C72'—H72F | 109.5 | O31—Mo11—O51 | 101.6 (4) |
O6—Ca1—O3 | 98.4 (4) | O86—Mo11—O51 | 84.6 (3) |
O6—Ca1—O2 | 91.2 (4) | O71—Mo11—O51 | 155.7 (3) |
O3—Ca1—O2 | 84.5 (4) | O77—Mo11—O51 | 85.8 (3) |
O6—Ca1—O4 | 162.5 (4) | O31—Mo11—O14 | 172.2 (3) |
O3—Ca1—O4 | 93.3 (3) | O86—Mo11—O14 | 84.8 (2) |
O2—Ca1—O4 | 102.9 (4) | O71—Mo11—O14 | 73.4 (2) |
O6—Ca1—O7 | 84.4 (4) | O77—Mo11—O14 | 72.7 (2) |
O3—Ca1—O7 | 168.0 (4) | O51—Mo11—O14 | 82.2 (2) |
O2—Ca1—O7 | 83.7 (4) | O32—Mo12—O43 | 102.3 (4) |
O4—Ca1—O7 | 86.9 (4) | O32—Mo12—O81 | 102.6 (4) |
O6—Ca1—O5 | 86.8 (4) | O43—Mo12—O81 | 92.5 (3) |
O3—Ca1—O5 | 87.2 (4) | O32—Mo12—O67 | 101.1 (4) |
O2—Ca1—O5 | 171.1 (4) | O43—Mo12—O67 | 86.0 (3) |
O4—Ca1—O5 | 80.8 (4) | O81—Mo12—O67 | 156.0 (3) |
O7—Ca1—O5 | 104.7 (4) | O32—Mo12—O47 | 100.1 (4) |
P1—O11—Mo12 | 126.0 (3) | O43—Mo12—O47 | 157.2 (3) |
P1—O11—Mo9 | 126.5 (4) | O81—Mo12—O47 | 86.5 (3) |
Mo12—O11—Mo9 | 88.76 (19) | O67—Mo12—O47 | 85.7 (3) |
P1—O11—Mo2 | 125.4 (3) | O32—Mo12—O11 | 171.8 (3) |
Mo12—O11—Mo2 | 89.5 (2) | O43—Mo12—O11 | 85.4 (3) |
Mo9—O11—Mo2 | 88.79 (19) | O81—Mo12—O11 | 73.9 (3) |
P1—O12—Mo3 | 125.6 (3) | O67—Mo12—O11 | 82.1 (2) |
P1—O12—Mo1 | 125.7 (4) | O47—Mo12—O11 | 72.5 (2) |
N1—C1—C2—C3 | −0.9 (13) | Mo3—O52—Mo5—O12 | −1.4 (3) |
C1—C2—C3—C4 | 1.1 (15) | P1—O12—Mo5—O62 | 40.3 (4) |
C1—C2—C3—C6 | 178.4 (14) | Mo3—O12—Mo5—O62 | 175.2 (3) |
C2—C3—C4—C5 | −1 (2) | Mo1—O12—Mo5—O62 | −95.3 (3) |
C6—C3—C4—C5 | −178.3 (18) | P1—O12—Mo5—O41 | 134.6 (5) |
C3—C4—C5—N1 | 1 (3) | Mo3—O12—Mo5—O41 | −90.4 (3) |
C4—C5—N1—C1 | −1 (3) | Mo1—O12—Mo5—O41 | −0.9 (3) |
C4—C5—N1—C7 | −179.7 (17) | P1—O12—Mo5—O61 | −46.5 (4) |
C2—C1—N1—C5 | 1 (2) | Mo3—O12—Mo5—O61 | 88.5 (3) |
C2—C1—N1—C7 | 179.7 (13) | Mo1—O12—Mo5—O61 | 178.0 (3) |
N1'—C1'—C2'—C3' | 3 (2) | P1—O12—Mo5—O52 | −134.1 (5) |
C1'—C2'—C3'—C6' | −174 (2) | Mo3—O12—Mo5—O52 | 0.9 (2) |
C2'—C1'—N1'—C5' | −7 (5) | Mo1—O12—Mo5—O52 | 90.4 (3) |
C2'—C1'—N1'—C7' | −179 (2) | Mo12—O67—Mo6—O26 | 129.9 (8) |
Ca1—O2—C23—N2 | 120.4 (18) | Mo12—O67—Mo6—O57 | −128.3 (8) |
O2—C23—N2—C22 | 6 (3) | Mo12—O67—Mo6—O44 | 28.3 (8) |
O2—C23—N2—C21 | −180 (2) | Mo12—O67—Mo6—O66 | −41.6 (13) |
Ca1—O3—C33—N3 | −23 (5) | Mo12—O67—Mo6—O13 | −55.5 (8) |
O3—C33—N3—C31 | −176 (2) | Mo4—O57—Mo6—O26 | −168.7 (5) |
O3—C33—N3—C32 | 2 (3) | Mo4—O57—Mo6—O67 | 86.7 (5) |
Ca1—O4—C43—N4 | −88 (3) | Mo4—O57—Mo6—O44 | 3.4 (11) |
O4—C43—N4—C41 | −2 (3) | Mo4—O57—Mo6—O66 | −68.6 (5) |
O4—C43—N4—C42 | 168.4 (18) | Mo4—O57—Mo6—O13 | 3.0 (4) |
Ca1—O5—C53—N5 | 165.9 (11) | Mo1—O44—Mo6—O26 | −135.9 (9) |
O5—C53—N5—C52 | −7 (3) | Mo1—O44—Mo6—O67 | −32.7 (8) |
O5—C53—N5—C51 | −179.3 (19) | Mo1—O44—Mo6—O57 | 52.0 (13) |
O6—C63—N6—C61 | 1 (3) | Mo1—O44—Mo6—O66 | 124.1 (8) |
O6—C63—N6—C62 | −175 (3) | Mo1—O44—Mo6—O13 | 52.4 (8) |
Ca1—O7—C73—N7 | −134.1 (17) | Mo10—O66—Mo6—O26 | 172.4 (5) |
O7—C73—N7—C72 | −4 (3) | Mo10—O66—Mo6—O67 | −15.9 (10) |
O7—C73—N7—C71 | 169 (2) | Mo10—O66—Mo6—O57 | 72.1 (5) |
C33—O3—Ca1—O6 | 176 (4) | Mo10—O66—Mo6—O44 | −85.6 (5) |
C33—O3—Ca1—O2 | 85 (4) | Mo10—O66—Mo6—O13 | −1.3 (4) |
C33—O3—Ca1—O4 | −17 (4) | P1—O13—Mo6—O26 | −172 (2) |
C33—O3—Ca1—O7 | 74 (4) | Mo10—O13—Mo6—O26 | −37 (2) |
C33—O3—Ca1—O5 | −98 (4) | Mo4—O13—Mo6—O26 | 52 (2) |
C23—O2—Ca1—O6 | −70.6 (18) | P1—O13—Mo6—O67 | 40.1 (4) |
C23—O2—Ca1—O3 | 27.7 (17) | Mo10—O13—Mo6—O67 | 174.8 (3) |
C23—O2—Ca1—O4 | 119.8 (17) | Mo4—O13—Mo6—O67 | −96.1 (3) |
C23—O2—Ca1—O7 | −154.8 (18) | P1—O13—Mo6—O57 | 134.2 (5) |
C43—O4—Ca1—O6 | 38 (2) | Mo10—O13—Mo6—O57 | −91.1 (3) |
C43—O4—Ca1—O3 | −93.7 (17) | Mo4—O13—Mo6—O57 | −2.0 (3) |
C43—O4—Ca1—O2 | −178.8 (16) | P1—O13—Mo6—O44 | −45.6 (4) |
C43—O4—Ca1—O7 | 98.3 (17) | Mo10—O13—Mo6—O44 | 89.0 (2) |
C43—O4—Ca1—O5 | −7.1 (16) | Mo4—O13—Mo6—O44 | 178.2 (2) |
C73—O7—Ca1—O6 | −43.0 (14) | P1—O13—Mo6—O66 | −133.8 (5) |
C73—O7—Ca1—O3 | 61 (3) | Mo10—O13—Mo6—O66 | 0.8 (2) |
C73—O7—Ca1—O2 | 48.8 (14) | Mo4—O13—Mo6—O66 | 90.0 (3) |
C73—O7—Ca1—O4 | 152.1 (14) | Mo2—O48—Mo7—O27 | 129.9 (9) |
C73—O7—Ca1—O5 | −128.2 (13) | Mo2—O48—Mo7—O72 | −127.2 (8) |
C53—O5—Ca1—O6 | 90.9 (14) | Mo2—O48—Mo7—O58 | 28.5 (8) |
C53—O5—Ca1—O3 | −7.7 (14) | Mo2—O48—Mo7—O71 | −39.0 (14) |
C53—O5—Ca1—O4 | −101.5 (14) | Mo2—O48—Mo7—O14 | −54.1 (8) |
C53—O5—Ca1—O7 | 174.2 (13) | Mo8—O72—Mo7—O27 | −170.4 (5) |
Mo8—O14—P1—O13 | −177.8 (4) | Mo8—O72—Mo7—O48 | 86.2 (5) |
Mo11—O14—P1—O13 | −58.6 (5) | Mo8—O72—Mo7—O58 | 4.3 (10) |
Mo7—O14—P1—O13 | 62.0 (5) | Mo8—O72—Mo7—O71 | −69.8 (4) |
Mo8—O14—P1—O11 | 62.7 (5) | Mo8—O72—Mo7—O14 | 2.7 (4) |
Mo11—O14—P1—O11 | −178.0 (4) | Mo4—O58—Mo7—O27 | −131.9 (9) |
Mo7—O14—P1—O11 | −57.4 (5) | Mo4—O58—Mo7—O48 | −30.1 (9) |
Mo8—O14—P1—O12 | −57.3 (5) | Mo4—O58—Mo7—O72 | 53.4 (14) |
Mo11—O14—P1—O12 | 61.9 (5) | Mo4—O58—Mo7—O71 | 127.8 (9) |
Mo7—O14—P1—O12 | −177.5 (3) | Mo4—O58—Mo7—O14 | 54.9 (9) |
Mo6—O13—P1—O14 | −177.2 (4) | Mo11—O71—Mo7—O27 | 171.8 (5) |
Mo10—O13—P1—O14 | 63.2 (5) | Mo11—O71—Mo7—O48 | −19.2 (11) |
Mo4—O13—P1—O14 | −56.4 (5) | Mo11—O71—Mo7—O72 | 69.9 (5) |
Mo6—O13—P1—O11 | −57.7 (5) | Mo11—O71—Mo7—O58 | −86.6 (5) |
Mo10—O13—P1—O11 | −177.3 (3) | Mo11—O71—Mo7—O14 | −3.4 (4) |
Mo4—O13—P1—O11 | 63.1 (5) | P1—O14—Mo7—O48 | 39.7 (4) |
Mo6—O13—P1—O12 | 62.2 (5) | Mo8—O14—Mo7—O48 | −95.5 (3) |
Mo10—O13—P1—O12 | −57.4 (5) | Mo11—O14—Mo7—O48 | 175.8 (3) |
Mo4—O13—P1—O12 | −177.0 (4) | P1—O14—Mo7—O72 | 133.4 (5) |
Mo12—O11—P1—O14 | −177.9 (4) | Mo8—O14—Mo7—O72 | −1.8 (2) |
Mo9—O11—P1—O14 | −57.7 (5) | Mo11—O14—Mo7—O72 | −90.5 (3) |
Mo2—O11—P1—O14 | 61.9 (5) | P1—O14—Mo7—O58 | −45.9 (4) |
Mo12—O11—P1—O13 | 62.7 (5) | Mo8—O14—Mo7—O58 | 178.9 (3) |
Mo9—O11—P1—O13 | −177.1 (3) | Mo11—O14—Mo7—O58 | 90.2 (3) |
Mo2—O11—P1—O13 | −57.5 (5) | P1—O14—Mo7—O71 | −133.9 (5) |
Mo12—O11—P1—O12 | −57.5 (5) | Mo8—O14—Mo7—O71 | 90.9 (3) |
Mo9—O11—P1—O12 | 62.7 (5) | Mo11—O14—Mo7—O71 | 2.1 (3) |
Mo2—O11—P1—O12 | −177.7 (3) | Mo5—O61—Mo8—O28 | 128.6 (8) |
Mo3—O12—P1—O14 | −57.1 (5) | Mo5—O61—Mo8—O77 | −128.8 (8) |
Mo1—O12—P1—O14 | −177.2 (3) | Mo5—O61—Mo8—O76 | 27.7 (8) |
Mo5—O12—P1—O14 | 62.4 (5) | Mo5—O61—Mo8—O72 | −41.2 (13) |
Mo3—O12—P1—O13 | 62.9 (5) | Mo5—O61—Mo8—O14 | −55.5 (8) |
Mo1—O12—P1—O13 | −57.1 (5) | Mo11—O77—Mo8—O28 | −169.5 (5) |
Mo5—O12—P1—O13 | −177.6 (4) | Mo11—O77—Mo8—O61 | 86.2 (4) |
Mo3—O12—P1—O11 | −177.2 (3) | Mo11—O77—Mo8—O76 | 2.4 (10) |
Mo1—O12—P1—O11 | 62.8 (5) | Mo11—O77—Mo8—O72 | −70.6 (4) |
Mo5—O12—P1—O11 | −57.7 (5) | Mo11—O77—Mo8—O14 | 2.2 (3) |
Mo6—O44—Mo1—O21 | 135.0 (8) | Mo9—O76—Mo8—O28 | −134.2 (9) |
Mo6—O44—Mo1—O42 | −123.0 (8) | Mo9—O76—Mo8—O61 | −31.3 (9) |
Mo6—O44—Mo1—O41 | −33.5 (14) | Mo9—O76—Mo8—O77 | 53.9 (14) |
Mo6—O44—Mo1—O43 | 33.1 (8) | Mo9—O76—Mo8—O72 | 127.0 (9) |
Mo6—O44—Mo1—O12 | −50.4 (8) | Mo9—O76—Mo8—O14 | 54.1 (9) |
Mo3—O42—Mo1—O21 | −166.6 (5) | Mo7—O72—Mo8—O28 | 172.4 (5) |
Mo3—O42—Mo1—O44 | 88.6 (5) | Mo7—O72—Mo8—O61 | −17.7 (11) |
Mo3—O42—Mo1—O41 | −67.6 (5) | Mo7—O72—Mo8—O77 | 71.2 (5) |
Mo3—O42—Mo1—O43 | 5.3 (11) | Mo7—O72—Mo8—O76 | −86.4 (5) |
Mo3—O42—Mo1—O12 | 3.9 (4) | Mo7—O72—Mo8—O14 | −2.7 (4) |
Mo5—O41—Mo1—O21 | 172.1 (5) | P1—O14—Mo8—O61 | 39.8 (5) |
Mo5—O41—Mo1—O44 | −19.2 (10) | Mo11—O14—Mo8—O61 | −95.5 (3) |
Mo5—O41—Mo1—O42 | 71.4 (5) | Mo7—O14—Mo8—O61 | 175.9 (3) |
Mo5—O41—Mo1—O43 | −85.7 (5) | P1—O14—Mo8—O77 | 133.9 (5) |
Mo5—O41—Mo1—O12 | −1.4 (4) | Mo11—O14—Mo8—O77 | −1.4 (2) |
Mo12—O43—Mo1—O21 | −134.2 (8) | Mo7—O14—Mo8—O77 | −90.1 (2) |
Mo12—O43—Mo1—O44 | −31.0 (8) | P1—O14—Mo8—O76 | −46.0 (4) |
Mo12—O43—Mo1—O42 | 53.9 (13) | Mo11—O14—Mo8—O76 | 178.7 (3) |
Mo12—O43—Mo1—O41 | 127.2 (8) | Mo7—O14—Mo8—O76 | 90.0 (3) |
Mo12—O43—Mo1—O12 | 55.2 (8) | P1—O14—Mo8—O72 | −134.3 (5) |
P1—O12—Mo1—O21 | −169.7 (17) | Mo11—O14—Mo8—O72 | 90.4 (3) |
Mo3—O12—Mo1—O21 | 55.0 (18) | Mo7—O14—Mo8—O72 | 1.7 (2) |
Mo5—O12—Mo1—O21 | −34.4 (18) | Mo2—O49—Mo9—O29 | −169.9 (5) |
P1—O12—Mo1—O44 | 38.6 (4) | Mo2—O49—Mo9—O76 | 86.4 (5) |
Mo3—O12—Mo1—O44 | −96.7 (3) | Mo2—O49—Mo9—O81 | −69.8 (5) |
Mo5—O12—Mo1—O44 | 173.8 (3) | Mo2—O49—Mo9—O62 | 4.8 (11) |
P1—O12—Mo1—O42 | 132.7 (5) | Mo2—O49—Mo9—O11 | 2.9 (4) |
Mo3—O12—Mo1—O42 | −2.6 (3) | Mo8—O76—Mo9—O29 | 131.1 (9) |
Mo5—O12—Mo1—O42 | −92.1 (3) | Mo8—O76—Mo9—O49 | −124.9 (9) |
P1—O12—Mo1—O41 | −134.4 (5) | Mo8—O76—Mo9—O81 | −33.3 (15) |
Mo3—O12—Mo1—O41 | 90.4 (3) | Mo8—O76—Mo9—O62 | 31.3 (9) |
Mo5—O12—Mo1—O41 | 0.9 (2) | Mo8—O76—Mo9—O11 | −51.6 (9) |
P1—O12—Mo1—O43 | −46.8 (4) | Mo12—O81—Mo9—O29 | 173.4 (5) |
Mo3—O12—Mo1—O43 | 178.0 (3) | Mo12—O81—Mo9—O49 | 70.5 (5) |
Mo5—O12—Mo1—O43 | 88.5 (3) | Mo12—O81—Mo9—O76 | −22.1 (11) |
Mo4—O46—Mo2—O22 | 131.8 (8) | Mo12—O81—Mo9—O62 | −86.5 (5) |
Mo4—O46—Mo2—O47 | −126.9 (8) | Mo12—O81—Mo9—O11 | −3.0 (4) |
Mo4—O46—Mo2—O48 | 29.5 (8) | Mo5—O62—Mo9—O29 | −131.7 (8) |
Mo4—O46—Mo2—O49 | −39.8 (13) | Mo5—O62—Mo9—O49 | 53.5 (13) |
Mo4—O46—Mo2—O11 | −53.9 (8) | Mo5—O62—Mo9—O76 | −29.9 (8) |
Mo12—O47—Mo2—O22 | −170.6 (5) | Mo5—O62—Mo9—O81 | 128.6 (9) |
Mo12—O47—Mo2—O46 | 85.6 (4) | Mo5—O62—Mo9—O11 | 55.4 (8) |
Mo12—O47—Mo2—O48 | −2.3 (10) | P1—O11—Mo9—O49 | 133.0 (5) |
Mo12—O47—Mo2—O49 | −71.2 (4) | Mo12—O11—Mo9—O49 | −91.4 (3) |
Mo12—O47—Mo2—O11 | 1.1 (4) | Mo2—O11—Mo9—O49 | −1.9 (3) |
Mo7—O48—Mo2—O22 | −132.0 (9) | P1—O11—Mo9—O76 | 38.7 (4) |
Mo7—O48—Mo2—O46 | −29.5 (8) | Mo12—O11—Mo9—O76 | 174.3 (3) |
Mo7—O48—Mo2—O47 | 59.8 (13) | Mo2—O11—Mo9—O76 | −96.2 (3) |
Mo7—O48—Mo2—O49 | 128.9 (9) | P1—O11—Mo9—O81 | −133.7 (5) |
Mo7—O48—Mo2—O11 | 56.6 (8) | Mo12—O11—Mo9—O81 | 1.9 (3) |
Mo9—O49—Mo2—O22 | 170.6 (5) | Mo2—O11—Mo9—O81 | 91.4 (3) |
Mo9—O49—Mo2—O46 | −17.8 (11) | P1—O11—Mo9—O62 | −46.2 (4) |
Mo9—O49—Mo2—O47 | 70.9 (5) | Mo12—O11—Mo9—O62 | 89.4 (2) |
Mo9—O49—Mo2—O48 | −87.2 (5) | Mo2—O11—Mo9—O62 | 178.9 (3) |
Mo9—O49—Mo2—O11 | −2.9 (4) | Mo3—O53—Mo10—O30 | 130.9 (8) |
P1—O11—Mo2—O22 | −172.2 (19) | Mo3—O53—Mo10—O66 | −127.4 (8) |
Mo12—O11—Mo2—O22 | 52 (2) | Mo3—O53—Mo10—O86 | 29.1 (8) |
Mo9—O11—Mo2—O22 | −37 (2) | Mo3—O53—Mo10—O56 | −41.6 (13) |
P1—O11—Mo2—O46 | 40.4 (4) | Mo3—O53—Mo10—O13 | −54.9 (8) |
Mo12—O11—Mo2—O46 | −95.2 (3) | Mo6—O66—Mo10—O30 | −170.7 (5) |
Mo9—O11—Mo2—O46 | 176.0 (3) | Mo6—O66—Mo10—O53 | 85.6 (5) |
P1—O11—Mo2—O47 | 134.9 (5) | Mo6—O66—Mo10—O86 | −1.7 (10) |
Mo12—O11—Mo2—O47 | −0.7 (2) | Mo6—O66—Mo10—O56 | −71.3 (4) |
Mo9—O11—Mo2—O47 | −89.5 (3) | Mo6—O66—Mo10—O13 | 1.3 (4) |
P1—O11—Mo2—O48 | −46.5 (4) | Mo11—O86—Mo10—O30 | −134.1 (9) |
Mo12—O11—Mo2—O48 | 177.9 (3) | Mo11—O86—Mo10—O53 | −31.8 (9) |
Mo9—O11—Mo2—O48 | 89.2 (2) | Mo11—O86—Mo10—O66 | 56.9 (13) |
P1—O11—Mo2—O49 | −133.8 (5) | Mo11—O86—Mo10—O56 | 126.5 (9) |
Mo12—O11—Mo2—O49 | 90.6 (3) | Mo11—O86—Mo10—O13 | 54.0 (8) |
Mo9—O11—Mo2—O49 | 1.8 (2) | Mo4—O56—Mo10—O30 | 172.0 (5) |
Mo5—O52—Mo3—O23 | −170.0 (4) | Mo4—O56—Mo10—O53 | −15.5 (10) |
Mo5—O52—Mo3—O51 | 85.4 (4) | Mo4—O56—Mo10—O66 | 71.8 (4) |
Mo5—O52—Mo3—O42 | −70.3 (4) | Mo4—O56—Mo10—O86 | −86.3 (4) |
Mo5—O52—Mo3—O53 | 0.2 (10) | Mo4—O56—Mo10—O13 | −1.5 (4) |
Mo5—O52—Mo3—O12 | 1.4 (3) | P1—O13—Mo10—O30 | −174.4 (17) |
Mo11—O51—Mo3—O23 | 130.1 (8) | Mo6—O13—Mo10—O30 | 50.5 (19) |
Mo11—O51—Mo3—O52 | −126.6 (8) | Mo4—O13—Mo10—O30 | −38.9 (19) |
Mo11—O51—Mo3—O42 | −34.4 (13) | P1—O13—Mo10—O53 | 40.0 (4) |
Mo11—O51—Mo3—O53 | 29.7 (8) | Mo6—O13—Mo10—O53 | −95.2 (2) |
Mo11—O51—Mo3—O12 | −53.3 (8) | Mo4—O13—Mo10—O53 | 175.5 (2) |
Mo1—O42—Mo3—O23 | 171.5 (5) | P1—O13—Mo10—O66 | 134.3 (4) |
Mo1—O42—Mo3—O52 | 69.5 (5) | Mo6—O13—Mo10—O66 | −0.9 (2) |
Mo1—O42—Mo3—O51 | −23.8 (10) | Mo4—O13—Mo10—O66 | −90.2 (3) |
Mo1—O42—Mo3—O53 | −88.2 (5) | P1—O13—Mo10—O86 | −46.9 (4) |
Mo1—O42—Mo3—O12 | −4.0 (4) | Mo6—O13—Mo10—O86 | 177.9 (3) |
Mo10—O53—Mo3—O23 | −131.5 (8) | Mo4—O13—Mo10—O86 | 88.6 (3) |
Mo10—O53—Mo3—O52 | 58.2 (12) | P1—O13—Mo10—O56 | −134.6 (4) |
Mo10—O53—Mo3—O51 | −28.6 (8) | Mo6—O13—Mo10—O56 | 90.3 (3) |
Mo10—O53—Mo3—O42 | 129.5 (8) | Mo4—O13—Mo10—O56 | 1.0 (2) |
Mo10—O53—Mo3—O12 | 57.1 (8) | Mo10—O86—Mo11—O31 | 132.0 (9) |
P1—O12—Mo3—O52 | 133.8 (5) | Mo10—O86—Mo11—O71 | −124.6 (9) |
Mo1—O12—Mo3—O52 | −90.9 (3) | Mo10—O86—Mo11—O77 | −35.1 (14) |
Mo5—O12—Mo3—O52 | −0.9 (2) | Mo10—O86—Mo11—O51 | 31.2 (8) |
P1—O12—Mo3—O51 | 39.1 (4) | Mo10—O86—Mo11—O14 | −51.5 (8) |
Mo1—O12—Mo3—O51 | 174.4 (3) | Mo7—O71—Mo11—O31 | −169.7 (5) |
Mo5—O12—Mo3—O51 | −95.6 (3) | Mo7—O71—Mo11—O86 | 87.2 (5) |
P1—O12—Mo3—O42 | −132.8 (5) | Mo7—O71—Mo11—O77 | −69.3 (5) |
Mo1—O12—Mo3—O42 | 2.5 (2) | Mo7—O71—Mo11—O51 | 5.0 (11) |
Mo5—O12—Mo3—O42 | 92.5 (3) | Mo7—O71—Mo11—O14 | 3.4 (4) |
P1—O12—Mo3—O53 | −46.7 (4) | Mo8—O77—Mo11—O31 | 173.6 (5) |
Mo1—O12—Mo3—O53 | 88.6 (2) | Mo8—O77—Mo11—O86 | −19.3 (10) |
Mo5—O12—Mo3—O53 | 178.6 (2) | Mo8—O77—Mo11—O71 | 71.2 (4) |
Mo7—O58—Mo4—O24 | 130.2 (9) | Mo8—O77—Mo11—O51 | −85.3 (4) |
Mo7—O58—Mo4—O56 | −126.0 (9) | Mo8—O77—Mo11—O14 | −2.2 (3) |
Mo7—O58—Mo4—O46 | 30.3 (9) | Mo3—O51—Mo11—O31 | −132.0 (8) |
Mo7—O58—Mo4—O57 | −35.3 (14) | Mo3—O51—Mo11—O86 | −30.7 (8) |
Mo7—O58—Mo4—O13 | −52.8 (9) | Mo3—O51—Mo11—O71 | 53.2 (13) |
Mo10—O56—Mo4—O24 | −170.7 (5) | Mo3—O51—Mo11—O77 | 127.9 (8) |
Mo10—O56—Mo4—O58 | 85.0 (5) | Mo3—O51—Mo11—O14 | 54.8 (8) |
Mo10—O56—Mo4—O46 | −0.7 (10) | P1—O14—Mo11—O86 | 40.0 (5) |
Mo10—O56—Mo4—O57 | −70.1 (4) | Mo8—O14—Mo11—O86 | 174.6 (3) |
Mo10—O56—Mo4—O13 | 1.5 (4) | Mo7—O14—Mo11—O86 | −96.3 (3) |
Mo2—O46—Mo4—O24 | −132.1 (8) | P1—O14—Mo11—O71 | 134.1 (5) |
Mo2—O46—Mo4—O58 | −29.6 (8) | Mo8—O14—Mo11—O71 | −91.2 (3) |
Mo2—O46—Mo4—O56 | 57.9 (12) | Mo7—O14—Mo11—O71 | −2.2 (3) |
Mo2—O46—Mo4—O57 | 127.8 (8) | P1—O14—Mo11—O77 | −133.3 (5) |
Mo2—O46—Mo4—O13 | 55.8 (8) | Mo8—O14—Mo11—O77 | 1.4 (2) |
Mo6—O57—Mo4—O24 | 173.0 (5) | Mo7—O14—Mo11—O77 | 90.4 (2) |
Mo6—O57—Mo4—O58 | −21.4 (10) | P1—O14—Mo11—O51 | −45.2 (5) |
Mo6—O57—Mo4—O56 | 70.8 (5) | Mo8—O14—Mo11—O51 | 89.4 (2) |
Mo6—O57—Mo4—O46 | −87.0 (5) | Mo7—O14—Mo11—O51 | 178.5 (3) |
Mo6—O57—Mo4—O13 | −3.0 (4) | Mo1—O43—Mo12—O32 | 130.1 (8) |
P1—O13—Mo4—O58 | 38.4 (4) | Mo1—O43—Mo12—O81 | −126.5 (8) |
Mo6—O13—Mo4—O58 | 174.2 (3) | Mo1—O43—Mo12—O67 | 29.6 (8) |
Mo10—O13—Mo4—O58 | −96.2 (3) | Mo1—O43—Mo12—O47 | −39.3 (14) |
P1—O13—Mo4—O56 | 133.6 (5) | Mo1—O43—Mo12—O11 | −52.8 (8) |
Mo6—O13—Mo4—O56 | −90.6 (3) | Mo9—O81—Mo12—O32 | −169.4 (5) |
Mo10—O13—Mo4—O56 | −1.0 (2) | Mo9—O81—Mo12—O43 | 87.4 (5) |
P1—O13—Mo4—O46 | −47.3 (4) | Mo9—O81—Mo12—O67 | 1.5 (11) |
Mo6—O13—Mo4—O46 | 88.5 (2) | Mo9—O81—Mo12—O47 | −69.8 (5) |
Mo10—O13—Mo4—O46 | 178.1 (2) | Mo9—O81—Mo12—O11 | 3.0 (4) |
P1—O13—Mo4—O57 | −133.9 (5) | Mo6—O67—Mo12—O32 | −130.2 (8) |
Mo6—O13—Mo4—O57 | 1.9 (2) | Mo6—O67—Mo12—O43 | −28.4 (8) |
Mo10—O13—Mo4—O57 | 91.4 (3) | Mo6—O67—Mo12—O81 | 58.9 (12) |
Mo9—O62—Mo5—O25 | 130.8 (9) | Mo6—O67—Mo12—O47 | 130.3 (8) |
Mo9—O62—Mo5—O41 | −126.2 (8) | Mo6—O67—Mo12—O11 | 57.5 (8) |
Mo9—O62—Mo5—O61 | 29.2 (8) | Mo2—O47—Mo12—O32 | 175.3 (5) |
Mo9—O62—Mo5—O52 | −40.2 (13) | Mo2—O47—Mo12—O43 | −15.2 (10) |
Mo9—O62—Mo5—O12 | −53.9 (8) | Mo2—O47—Mo12—O81 | 73.1 (5) |
Mo1—O41—Mo5—O25 | −171.2 (5) | Mo2—O47—Mo12—O67 | −84.2 (4) |
Mo1—O41—Mo5—O62 | 85.7 (5) | Mo2—O47—Mo12—O11 | −1.1 (4) |
Mo1—O41—Mo5—O61 | −1.1 (10) | P1—O11—Mo12—O43 | 40.0 (5) |
Mo1—O41—Mo5—O52 | −70.8 (5) | Mo9—O11—Mo12—O43 | −96.0 (3) |
Mo1—O41—Mo5—O12 | 1.4 (4) | Mo2—O11—Mo12—O43 | 175.3 (3) |
Mo8—O61—Mo5—O25 | −129.8 (8) | P1—O11—Mo12—O81 | 134.0 (5) |
Mo8—O61—Mo5—O62 | −28.1 (8) | Mo9—O11—Mo12—O81 | −2.0 (3) |
Mo8—O61—Mo5—O41 | 60.2 (12) | Mo2—O11—Mo12—O81 | −90.8 (3) |
Mo8—O61—Mo5—O52 | 130.0 (8) | P1—O11—Mo12—O67 | −46.6 (5) |
Mo8—O61—Mo5—O12 | 57.7 (8) | Mo9—O11—Mo12—O67 | 177.4 (3) |
Mo3—O52—Mo5—O25 | 173.2 (4) | Mo2—O11—Mo12—O67 | 88.6 (3) |
Mo3—O52—Mo5—O62 | −15.8 (10) | P1—O11—Mo12—O47 | −134.6 (5) |
Mo3—O52—Mo5—O41 | 71.7 (4) | Mo9—O11—Mo12—O47 | 89.5 (3) |
Mo3—O52—Mo5—O61 | −85.3 (4) | Mo2—O11—Mo12—O47 | 0.7 (2) |
D—H···A | D—H | H···A | D···A | D—H···A |
C4—H4A···O32i | 0.93 | 2.57 | 3.390 (3) | 148 |
C4—H4′A···O32i | 0.93 | 2.52 | 3.390 (3) | 156 |
C7—H7B···O26i | 0.96 | 2.48 | 3.176 (8) | 129 |
C51—H51B···O62ii | 0.96 | 2.49 | 3.446 (6) | 176 |
C53—O5···C6′iii | 1.24 (1) | 2.81 (1) | 3.501 (7) | 114 (1) |
Symmetry codes: (i) −x+1, −y, z−1/2; (ii) −x+1, −y+1, z−1/2; (iii) x, y+1, z. |
Experimental details
Crystal data | |
Chemical formula | (C7H10N)[Ca(C3H7NO)6][PMo12O40] |
Mr | 2409.07 |
Crystal system, space group | Orthorhombic, Pca21 |
Temperature (K) | 293 |
a, b, c (Å) | 38.293 (6), 13.246 (2), 12.888 (2) |
V (Å3) | 6537.6 (17) |
Z | 4 |
Radiation type | Mo Kα |
µ (mm−1) | 2.43 |
Crystal size (mm) | 0.49 × 0.11 × 0.08 |
Data collection | |
Diffractometer | Bruker SMART CCD area-detector diffractometer |
Absorption correction | Multi-scan (SADABS; Bruker, 2000) |
Tmin, Tmax | 0.733, 0.824 |
No. of measured, independent and observed [I > 2σ(I)] reflections | 39117, 14090, 12008 |
Rint | 0.038 |
(sin θ/λ)max (Å−1) | 0.640 |
Refinement | |
R[F2 > 2σ(F2)], wR(F2), S | 0.060, 0.127, 1.10 |
No. of reflections | 14090 |
No. of parameters | 746 |
No. of restraints | 377 |
H-atom treatment | H-atom parameters constrained |
w = 1/[σ2(Fo2) + (0.0518P)2 + 11.3547P] where P = (Fo2 + 2Fc2)/3 | |
Δρmax, Δρmin (e Å−3) | 1.08, −0.63 |
Absolute structure | Flack (1983), 6579 Friedel pairs |
Absolute structure parameter | −0.01 (5) |
Computer programs: SMART (Bruker, 2000), SMART, SAINT (Bruker, 2000), SHELXTL (Bruker, 2000), SHELXL97 (Sheldrick, 1997), SHELXTL, SHELXL97.
O2—Ca1 | 2.289 (10) | O22—Mo2 | 1.690 (7) |
O3—Ca1 | 2.278 (9) | O23—Mo3 | 1.659 (7) |
O4—Ca1 | 2.289 (11) | O24—Mo4 | 1.681 (8) |
O5—Ca1 | 2.329 (9) | O25—Mo5 | 1.669 (8) |
O6—Ca1 | 2.275 (10) | O26—Mo6 | 1.686 (8) |
O7—Ca1 | 2.324 (10) | O27—Mo7 | 1.677 (8) |
O11—P1 | 1.535 (6) | O28—Mo8 | 1.668 (8) |
O12—P1 | 1.547 (7) | O29—Mo9 | 1.674 (7) |
O13—P1 | 1.534 (6) | O30—Mo10 | 1.689 (7) |
O14—P1 | 1.530 (6) | O31—Mo11 | 1.668 (8) |
O21—Mo1 | 1.678 (6) | O32—Mo12 | 1.671 (7) |
D—H···A | D—H | H···A | D···A | D—H···A |
C4—H4A···O32i | 0.93 | 2.57 | 3.390 (3) | 148 |
C4—H4'A···O32i | 0.93 | 2.52 | 3.390 (3) | 156 |
C7—H7B···O26i | 0.96 | 2.48 | 3.176 (8) | 129 |
C51—H51B···O62ii | 0.96 | 2.49 | 3.446 (6) | 176 |
C53—O5···C6'iii | 1.238 (12) | 2.808 (8) | 3.501 (7) | 114.11 (6) |
Symmetry codes: (i) −x+1, −y, z−1/2; (ii) −x+1, −y+1, z−1/2; (iii) x, y+1, z. |
In crystal engineering and polyoxometalate (POM) chemistry, one of the major challenges is to establish reliable connections between new molecular and supramolecular structures on the basis of intermolecular interactions (Desiraju, 1995; Niu et al., 2003). Ideally, we would like to identify substructural units in a target supermolecule that can be assembled from logically chosen precursor molecules. We attempt here to use a simple method to realise such molecular assemblies. This paper deals with the preparation and crystal structure of a new supramolecular compound obtained from the reaction of 1,4-dimethylpyridinium iodide (DMPI), CaCl2 and Keggin-type H3PMo12O40. The synthesis and structure of the title compound, (I), in which infinite stacking assemblies are achieved, may serve as useful models for the design of functional molecular assemblies.
The title compound is built from three subunits, viz. two cations {1,4-dimethylpyridine (DMP) and a [Ca(dmf)6]2+ complex cation (dmf is dimethylformamide} and dodecamolybdophosphate anions ([PMo12O40]3−; denoted POM). In the [Ca(dmf)6]2+ complex cation, the Ca atom is coordinated in a distorted octahedral fashion by six O atoms of dmf ligands. The Ca—O bond lengths range from 2.275 (10) to 2.329 (9) Å (Table 1), with para-O—Ca—para-O angles from 162.5 (4) to 171.1 (4)° and ortho-O—Ca—ortho-O angles from 80.8 (4) to 104.7 (4)°. Because all dmf ligands are the same, the difference in bond lengths and angles (which causes a distorted octahedron) must be the result of internal pressure, induced by the crystal packing and intermolecular interactions. The Keggin structure [PMo12O40]3− consists of one PO4 tetrahedron (atom Oa) surrounded by four corner-sharing Mo3O13 sets formed by three edge-sharing MoO6 octahedra (corner-sharing O atoms between Mo3O13 are denoted Ob, edge-sharing O atoms inside Mo3O13 are denoted Oc and unshared terminal O atoms are denoted Ot). The P—Oa bond distances are 1.530 (6)—1.547 (7) Å, with angles of 109.1 (3)–110.0 (4)°, showing that the PO4 tetrahedron is distorted to small entent. In the MoO6 octahedra, the Mo—Ot, Mo—Oa and Mo—Ob,c bond distances fall in the ranges 1.659 (7)–1.690 (7), 2.413 (6)–2.435 (6) and 1.850 (7)–1.978 (8) Å, and the mean values are 1.676, 2.426 and 1.912 Å, respectively. These results show that the MoO6 octahedra of the polyanions in (I) are severely distorted because of the influence of the outer cations (Pope, 1983; Niu et al., 2002, 2003; Wang et al., 2002). The three subunits of (I) form an infinite three-dimensional assembly via electrostatic forces. Weak C—H···O, C—H···Mo and C=O···C interactions help to link the cations and anions together (Fig. 1 and Table 2). DMP cations and POM anions, as well as [Ca(dmf)6]2+ cations and POM anions, participate in weak interactions, and DMP cations and Ca(dmf)62+ cations are also linked via carbonyl O and methyl C atoms [O5···C6' = 2.808 (8) Å]. This type of interaction is similar to a carbonyl–carbonyl interaction (Allen et al., 1998). On the other hand, the O5···C6 distance [3.399 (9) Å] is longer than the sum of van der Waals radii for C and O atoms (3.22 Å).
The packing structure is a multilayered system, in which different types of layers can be found in point of different subunits. For example, three types of layers can be found along [100] (a axis) for every two of the subunits (Figs. 2 and 3). The POM and DMP ions constitute graphite-like layers; two types of weak interactions (O···H and Mo···H) occur inside the layers, but no such interactions are present between layers. The POM ion forms zigzag ribbons through this kind of interactions. In the same way, the POM and [Ca(dmf)6]2+ ions constitute interlaced layers; each POM ion forms weak interactions (O···H and Mo···H) with every [Ca(dmf)6]2+ cation around it, and vice versa, thus building the framework of the crystal.
Table 2. C—H···O and C=O···C interaction geometry (Å, °)