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The dications and tetraanion in the title compound, (C
6H
16N
2)
2[Mo
5O
15(HPO
4)
2]·2H
2O, occupy special positions in the crystal structure. One of the independent cations lies on a site of
symmetry and the other lies on a site of 2 symmetry. The tetraanion, which has 2 site symmetry, consists of a five-unit ring of vertex/edge-sharing MoO
6 octahedra; the ring is capped by two P(OH) units on opposite sides. The anions are linked
via hydrogen bonds involving the H atom of the hydrogenphosphate group into a zigzag chain running along the
c axis. The chains are incorporated into the network structure through hydrogen bonds involving the cations and lattice water molecules.
Supporting information
CCDC reference: 234798
Key indicators
- Single-crystal X-ray study
- T = 298 K
- R factor = 0.034
- wR factor = 0.095
- Data-to-parameter ratio = 15.5
checkCIF/PLATON results
No syntax errors found
Alert level A
PLAT391_ALERT_3_A Deviating Methyl C3 H-C-H Bond Angle ...... 125.10 Deg.
| Author Response: The cation on the two-fold axis is disordered. The treatment of
the
disorder is described. The angle is an artifact of the disorder.
|
PLAT391_ALERT_3_A Deviating Methyl C3 H-C-H Bond Angle ...... 88.24 Deg.
| Author Response: The cation on the two-fold axis is disordered. The treatment of
the
disorder is described. The angle is an artifact of the disorder.
|
Alert level B
PLAT420_ALERT_2_B D-H Without Acceptor O1W - H1W2 ... ?
Alert level C
ABSTM02_ALERT_3_C The ratio of expected to reported Tmax/Tmin(RR') is < 0.90
Tmin and Tmax reported: 0.438 0.662
Tmin' and Tmax expected: 0.509 0.662
RR' = 0.862
Please check that your absorption correction is appropriate.
PLAT042_ALERT_1_C Calc. and Rep. MoietyFormula Strings Differ .... ?
PLAT061_ALERT_3_C Tmax/Tmin Range Test RR' too Large ............. 0.84
PLAT302_ALERT_4_C Anion/Solvent Disorder ......................... 26.00 Perc.
PLAT432_ALERT_2_C Short Inter X...Y Contact O6 .. C1' = 2.99 Ang.
PLAT720_ALERT_4_C Number of Unusual/Non-Standard Label(s) ........ 10
PLAT790_ALERT_4_C Centre of Gravity not Within Unit Cell: Resd. # 4
H2 O
2 ALERT level A = In general: serious problem
1 ALERT level B = Potentially serious problem
7 ALERT level C = Check and explain
0 ALERT level G = General alerts; check
1 ALERT type 1 CIF construction/syntax error, inconsistent or missing data
2 ALERT type 2 Indicator that the structure model may be wrong or deficient
4 ALERT type 3 Indicator that the structure quality may be low
3 ALERT type 4 Improvement, methodology, query or suggestion
Data collection: SMART (Bruker, 2001); cell refinement: SMART; data reduction: SAINT (Bruker, 2001); program(s) used to solve structure: SHELXS97 (Sheldrick, 1997); program(s) used to refine structure: SHELXL97 (Sheldrick, 1997); molecular graphics: ORTEPII (Johnson, 1976); software used to prepare material for publication: SHELXL97.
Bis(3,5-dimethylpiperazinium)
di-µ
5-hydrogenphosphato-penta-µ
2-oxo-pentakis[dioxomolybdenum(III)]
dihydrate
top
Crystal data top
(C6H16N2)2[Mo5O15(HPO4)2]·2H2O | F(000) = 2312 |
Mr = 1180.10 | Dx = 2.395 Mg m−3 |
Monoclinic, C2/c | Mo Kα radiation, λ = 0.71073 Å |
Hall symbol: -C 2yc | Cell parameters from 6915 reflections |
a = 10.8677 (5) Å | θ = 2.4–27.0° |
b = 21.960 (1) Å | µ = 2.06 mm−1 |
c = 13.7160 (6) Å | T = 298 K |
β = 90.715 (1)° | Prism, colorless |
V = 3273.1 (3) Å3 | 0.32 × 0.26 × 0.20 mm |
Z = 4 | |
Data collection top
Bruker APEX area-detector diffractometer | 3538 independent reflections |
Radiation source: fine-focus sealed tube | 3017 reflections with I > 2σ(I)' |
Graphite monochromator | Rint = 0.049 |
φ and ω scans | θmax = 27.0°, θmin = 1.9° |
Absorption correction: multi-scan (SADABS; Sheldrick, 1996) | h = −10→13 |
Tmin = 0.438, Tmax = 0.662 | k = −25→27 |
9212 measured reflections | l = −17→16 |
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: inferred from neighbouring sites |
wR(F2) = 0.095 | H-atom parameters constrained |
S = 1.04 | w = 1/[σ2(Fo2) + (0.0473P)2] where P = (Fo2 + 2Fc2)/3 |
3538 reflections | (Δ/σ)max = 0.001 |
228 parameters | Δρmax = 0.88 e Å−3 |
13 restraints | Δρmin = −1.01 e Å−3 |
Fractional atomic coordinates and isotropic or equivalent isotropic displacement parameters (Å2) top | x | y | z | Uiso*/Ueq | Occ. (<1) |
Mo1 | 0.0000 | 0.69434 (2) | 0.2500 | 0.0209 (2) | |
Mo2 | 0.25271 (4) | 0.60436 (2) | 0.28370 (3) | 0.0220 (1) | |
Mo3 | 0.16853 (4) | 0.45807 (2) | 0.25107 (3) | 0.0181 (1) | |
P1 | 0.0189 (1) | 0.56061 (5) | 0.11368 (8) | 0.0168 (2) | |
O1 | −0.0185 (3) | 0.5845 (1) | 0.0104 (2) | 0.026 (1) | |
O2 | 0.0969 (3) | 0.5035 (1) | 0.1077 (2) | 0.019 (1) | |
O3 | 0.0887 (3) | 0.6129 (1) | 0.1621 (2) | 0.020 (1) | |
O4 | −0.0638 (4) | 0.7418 (2) | 0.3313 (3) | 0.039 (1) | |
O5 | 0.1435 (3) | 0.6676 (1) | 0.3201 (2) | 0.024 (1) | |
O6 | 0.3464 (3) | 0.6420 (2) | 0.2053 (3) | 0.038 (1) | |
O7 | 0.3357 (4) | 0.5994 (2) | 0.3895 (3) | 0.039 (1) | |
O8 | 0.2839 (3) | 0.5228 (1) | 0.2328 (3) | 0.025 (1) | |
O9 | 0.0988 (3) | 0.5447 (1) | 0.3311 (2) | 0.019 (1) | |
O10 | 0.0000 | 0.4329 (2) | 0.2500 | 0.020 (1) | |
O11 | 0.2317 (3) | 0.4072 (2) | 0.1714 (3) | 0.029 (1) | |
O12 | 0.2089 (3) | 0.4293 (2) | 0.3617 (3) | 0.030 (1) | |
O1W | −0.1881 (5) | 0.6924 (2) | 0.5060 (4) | 0.070 (2) | |
N1 | 0.0531 (8) | 0.6931 (4) | 0.8374 (6) | 0.038 (2) | 0.50 |
N1' | −0.0540 (8) | 0.7419 (4) | 0.6659 (6) | 0.038 (2) | 0.50 |
N2 | 0.3973 (4) | 0.5228 (2) | 0.5527 (3) | 0.037 (1) | |
C1 | 0.1339 (8) | 0.7127 (9) | 0.7549 (7) | 0.039 (3) | 0.50 |
C1' | −0.1309 (8) | 0.725 (1) | 0.7494 (7) | 0.039 (3) | 0.50 |
C2 | 0.0645 (8) | 0.7073 (5) | 0.6601 (6) | 0.040 (3) | 0.50 |
C2' | −0.0577 (9) | 0.7339 (5) | 0.8411 (6) | 0.040 (3) | 0.50 |
C3 | 0.1332 (7) | 0.7236 (3) | 0.5676 (5) | 0.053 (2) | |
C4 | 0.4025 (5) | 0.4577 (2) | 0.5229 (4) | 0.032 (1) | |
C5 | 0.4785 (5) | 0.4501 (2) | 0.4285 (4) | 0.030 (1) | |
C6 | 0.4890 (6) | 0.3839 (3) | 0.4037 (6) | 0.057 (2) | |
H1 | −0.0323 | 0.5556 | −0.0259 | 0.038* | |
H1w1 | −0.1543 | 0.7060 | 0.4536 | 0.084* | |
H1w2 | −0.2408 | 0.6656 | 0.4865 | 0.084* | |
H1n1 | 0.0291 | 0.6543 | 0.8284 | 0.046* | 0.50 |
H1n2 | 0.0953 | 0.6954 | 0.8941 | 0.046* | 0.50 |
H1n3 | −0.0368 | 0.7819 | 0.6694 | 0.046* | 0.50 |
H1n4 | −0.0976 | 0.7356 | 0.6106 | 0.046* | 0.50 |
H1a | 0.1599 | 0.7545 | 0.7647 | 0.047* | 0.50 |
H1b | 0.2068 | 0.6872 | 0.7534 | 0.047* | 0.50 |
H1'1 | −0.1569 | 0.6832 | 0.7436 | 0.047* | 0.50 |
H1'2 | −0.2037 | 0.7508 | 0.7505 | 0.047* | 0.50 |
H2 | 0.0418 | 0.6643 | 0.6537 | 0.048* | 0.50 |
H2' | −0.0284 | 0.7761 | 0.8423 | 0.048* | 0.50 |
H2n1 | 0.3523 | 0.5259 | 0.6071 | 0.044* | |
H2n2 | 0.3590 | 0.5442 | 0.5054 | 0.044* | |
H3a | 0.2084 | 0.7008 | 0.5651 | 0.079* | |
H3b | 0.1516 | 0.7663 | 0.5676 | 0.079* | |
H3c | 0.0829 | 0.7139 | 0.5117 | 0.079* | |
H4a | 0.3197 | 0.4425 | 0.5117 | 0.038* | |
H4b | 0.4399 | 0.4338 | 0.5749 | 0.038* | |
H5 | 0.4377 | 0.4718 | 0.3747 | 0.036* | |
H6a | 0.5366 | 0.3793 | 0.3457 | 0.085* | |
H6b | 0.4083 | 0.3672 | 0.3930 | 0.085* | |
H6c | 0.5288 | 0.3627 | 0.4566 | 0.085* | |
Atomic displacement parameters (Å2) top | U11 | U22 | U33 | U12 | U13 | U23 |
Mo1 | 0.0237 (3) | 0.0152 (3) | 0.0238 (3) | 0.000 | −0.0039 (2) | 0.000 |
Mo2 | 0.0182 (2) | 0.0176 (2) | 0.0299 (3) | −0.0024 (2) | −0.0041 (2) | −0.0011 (2) |
Mo3 | 0.0158 (2) | 0.0161 (2) | 0.0225 (2) | 0.0014 (2) | −0.0011 (2) | 0.0009 (2) |
P1 | 0.0220 (6) | 0.0159 (6) | 0.0125 (6) | −0.0011 (5) | −0.0013 (4) | −0.0004 (4) |
O1 | 0.041 (2) | 0.018 (2) | 0.018 (2) | −0.001 (2) | −0.006 (2) | −0.001 (1) |
O2 | 0.024 (2) | 0.019 (2) | 0.014 (2) | 0.002 (1) | 0.000 (1) | −0.001 (1) |
O3 | 0.024 (2) | 0.018 (2) | 0.020 (2) | −0.004 (1) | 0.000 (1) | 0.000 (1) |
O4 | 0.038 (2) | 0.027 (2) | 0.051 (3) | 0.007 (2) | 0.001 (2) | −0.011 (2) |
O5 | 0.025 (2) | 0.019 (2) | 0.027 (2) | −0.001 (1) | −0.008 (1) | −0.008 (1) |
O6 | 0.032 (2) | 0.027 (2) | 0.055 (3) | −0.008 (2) | 0.011 (2) | 0.004 (2) |
O7 | 0.036 (2) | 0.036 (2) | 0.044 (2) | 0.003 (2) | −0.020 (2) | −0.007 (2) |
O8 | 0.013 (2) | 0.021 (2) | 0.040 (2) | 0.000 (1) | −0.001 (1) | −0.00192) |
O9 | 0.021 (2) | 0.018 (2) | 0.018 (2) | 0.001 (1) | 0.000 (1) | 0.000 (1) |
O10 | 0.016 (2) | 0.016 (2) | 0.029 (3) | 0.000 | 0.000 (2) | 0.000 |
O11 | 0.026 (2) | 0.023 (2) | 0.039 (2) | 0.005 (2) | 0.007 (2) | −0.003 (2) |
O12 | 0.031 (2) | 0.032 (2) | 0.028 (2) | 0.002 (2) | −0.009 (2) | 0.009 (2) |
O1w | 0.069 (3) | 0.090 (4) | 0.049 (3) | 0.001 (3) | 0.013 (3) | −0.021 (3) |
N1 | 0.051 (4) | 0.022 (3) | 0.043 (4) | 0.002 (3) | 0.004 (3) | 0.001 (3) |
N1' | 0.051 (4) | 0.022 (3) | 0.043 (4) | 0.002 (3) | 0.004 (3) | 0.001 (3) |
N2 | 0.018 (2) | 0.056 (3) | 0.036 (3) | 0.003 (2) | 0.003 (2) | −0.015 (2) |
C1 | 0.039 (4) | 0.046 (8) | 0.033 (4) | −0.004 (6) | 0.010 (3) | −0.006 (6) |
C1' | 0.039 (4) | 0.046 (8) | 0.033 (4) | −0.004 (6) | 0.010 (3) | −0.006 (6) |
C2 | 0.042 (4) | 0.025 (8) | 0.053 (5) | 0.004 (3) | 0.018 (4) | −0.003 (3) |
C2' | 0.042 (4) | 0.025 (8) | 0.053 (5) | 0.004 (3) | 0.018 (4) | −0.003 (3) |
C3 | 0.061 (4) | 0.048 (4) | 0.049 (4) | −0.004 (3) | 0.027 (3) | 0.004 (3) |
C4 | 0.022 (3) | 0.036 (3) | 0.038 (3) | −0.005 (2) | 0.000 (2) | 0.004 (2) |
C5 | 0.021 (3) | 0.041 (3) | 0.029 (3) | 0.001 (2) | −0.003 (2) | −0.008 (2) |
C6 | 0.038 (4) | 0.053 (4) | 0.079 (5) | 0.004 (3) | −0.009 (3) | −0.033 (4) |
Geometric parameters (Å, º) top
Mo1—O3 | 2.369 (3) | N2—C4 | 1.488 (7) |
Mo1—O3i | 2.369 (3) | N2—C5iii | 1.495 (6) |
Mo1—O4 | 1.683 (4) | C4—C5 | 1.553 (7) |
Mo1—O4i | 1.683 (4) | C5—N2iii | 1.495 (6) |
Mo1—O5 | 1.914 (3) | C5—C6 | 1.500 (8) |
Mo1—O5i | 1.914 (3) | O1—H1 | 0.82 |
Mo2—O3 | 2.433 (3) | O1w—H1w1 | 0.86 |
Mo2—O5 | 1.897 (3) | O1w—H1w2 | 0.86 |
Mo2—O6 | 1.704 (4) | N1—H1n1 | 0.90 |
Mo2—O7 | 1.703 (4) | N1—H1n2 | 0.90 |
Mo2—O8 | 1.953 (3) | N1'—H1n3 | 0.90 |
Mo2—O9 | 2.228 (3) | N1'—H1n4 | 0.90 |
Mo3—O2 | 2.331 (3) | C1—H1a | 0.97 |
Mo3—O8 | 1.914 (3) | C1—H1b | 0.97 |
Mo3—O9 | 2.328 (3) | C1'—H1'1 | 0.97 |
Mo3—O10 | 1.913 (1) | C1'—H1'2 | 0.97 |
Mo3—O11 | 1.713 (3) | C2—H2 | 0.98 |
Mo3—O12 | 1.697 (3) | C2'—H2' | 0.98 |
P1—O2 | 1.516 (3) | N2—H2n1 | 0.90 |
P1—O3 | 1.524 (3) | N2—H2n2 | 0.90 |
P1—O9i | 1.534 (3) | C3—H3a | 0.96 |
P1—O1 | 1.560 (3) | C3—H3b | 0.96 |
N1—C1 | 1.503 (9) | C3—H3c | 0.96 |
N1—C2' | 1.501 (8) | C4—H4a | 0.97 |
N1'—C1' | 1.471 (9) | C4—H4b | 0.97 |
N1'—C2 | 1.499 (8) | C5—H5 | 0.98 |
C1—C2 | 1.500 (9) | C6—H6a | 0.96 |
C1'—C2' | 1.491 (9) | C6—H6b | 0.96 |
C2—C3 | 1.523 (7) | C6—H6c | 0.96 |
C2'—C3ii | 1.52 (1) | | |
| | | |
O3—Mo1—O3i | 81.9 (2) | N1'—C2—C1 | 109.7 (7) |
O3—Mo1—O4 | 168.2 (2) | N1'—C2—C3 | 110.8 (7) |
O3—Mo1—O4i | 87.5 (2) | C1—C2—C3 | 117.3 (8) |
O3—Mo1—O5 | 71.9 (1) | C1'—C2'—N1 | 108.4 (7) |
O3—Mo1—O5i | 81.2 (1) | C1'—C2'—C3ii | 112.8 (8) |
O3i—Mo1—O4 | 87.5 (2) | N1—C2'—C3ii | 112.3 (7) |
O3i—Mo1—O4i | 168.2 (2) | C4—N2—C5iii | 113.1 (4) |
O3i—Mo1—O5 | 81.2 (1) | N2—C4—C5 | 110.7 (4) |
O3i—Mo1—O5i | 71.9 (1) | N2iii—C5—C6 | 110.8 (4) |
O4—Mo1—O4i | 103.4 (3) | N2iii—C5—C4 | 107.6 (4) |
O4—Mo1—O5 | 101.4 (2) | C6—C5—C4 | 109.6 (5) |
O4—Mo1—O5i | 100.6 (2) | P1—O1—H1 | 109.5 |
O4i—Mo1—O5 | 100.6 (2) | H1w1—O1w—H1w2 | 105.4 |
O4i—Mo1—O5i | 101.4 (2) | C2'—N1—H1n1 | 109.8 |
O5—Mo1—O5i | 144.2 (2) | C1—N1—H1n1 | 109.8 |
O3—Mo2—O8 | 87.4 (1) | C2'—N1—H1n2 | 109.8 |
O3—Mo2—O9 | 72.5 (1) | C1—N1—H1n2 | 109.8 |
O3—Mo2—O5 | 70.7 (1) | H1n1—N1—H1n2 | 108.2 |
O3—Mo2—O6 | 88.2 (2) | C1'—N1'—H1n3 | 108.7 |
O3—Mo2—O7 | 164.8 (2) | C2—N1'—H1n3 | 108.7 |
O5—Mo2—O6 | 101.1 (2) | C1'—N1'—H1n4 | 108.7 |
O5—Mo2—O7 | 98.6 (2) | C2—N1'—H1n4 | 108.7 |
O5—Mo2—O8 | 151.3 (1) | H1n3—N1'—H1n4 | 107.6 |
O5—Mo2—O9 | 83.1 (1) | C2—C1—H1a | 109.7 |
O6—Mo2—O7 | 104.7 (2) | N1—C1—H1a | 109.7 |
O6—Mo2—O8 | 96.4 (2) | C2—C1—H1b | 109.7 |
O6—Mo2—O9 | 157.9 (2) | N1—C1—H1b | 109.7 |
O7—Mo2—O8 | 98.8 (2) | H1a—C1—H1b | 108.2 |
O7—Mo2—O9 | 96.0 (2) | N1'—C1'—H1'1 | 109.9 |
O8—Mo2—O9 | 72.5 (1) | C2'—C1'—H1'1 | 109.9 |
O2—Mo3—O8 | 77.5 (1) | N1'—C1'—H1'2 | 109.9 |
O2—Mo3—O9 | 86.6 (1) | C2'—C1'—H1'2 | 109.9 |
O2—Mo3—O10 | 78.9 (1) | H1'1—C1'—H1'2 | 108.3 |
O2—Mo3—O11 | 82.7 (1) | N1'—C2—H2 | 106.1 |
O2—Mo3—O12 | 173.8 (2) | C1—C2—H2 | 106.1 |
O8—Mo3—O9 | 70.9 (1) | C3—C2—H2 | 106.1 |
O8—Mo3—O10 | 147.4 (2) | C1'—C2'—H2' | 107.7 |
O8—Mo3—O11 | 97.6 (2) | N1—C2'—H2' | 107.7 |
O8—Mo3—O12 | 103.4 (2) | C3ii—C2'—H2' | 107.7 |
O9—Mo3—O10 | 85.6 (1) | C4—N2—H2n1 | 109.0 |
O9—Mo3—O11 | 165.8 (1) | C5iii—N2—H2n1 | 109.0 |
O9—Mo3—O12 | 87.9 (1) | C4—N2—H2n2 | 109.0 |
O10—Mo3—O11 | 101.4 (2) | C5iii—N2—H2n2 | 109.0 |
O10—Mo3—O12 | 97.8 (1) | H2n1—N2—H2n2 | 107.8 |
O11—Mo3—O12 | 103.1 (2) | C2—C3—H3a | 109.5 |
O2—P1—O3 | 111.7 (2) | C2—C3—H3b | 109.5 |
O2—P1—O9i | 108.0 (2) | H3a—C3—H3b | 109.5 |
O3—P1—O9i | 111.7 (2) | C2—C3—H3c | 109.5 |
O2—P1—O1 | 111.6 (2) | H3a—C3—H3c | 109.5 |
O3—P1—O1 | 105.4 (2) | H3b—C3—H3c | 109.5 |
O9i—P1—O1 | 108.4 (2) | N2—C4—H4a | 109.5 |
P1—O2—Mo3 | 119.3 (2) | C5—C4—H4a | 109.5 |
P1—O3—Mo1 | 125.9 (2) | N2—C4—H4b | 109.5 |
P1—O3—Mo2 | 126.7 (2) | C5—C4—H4b | 109.5 |
Mo1—O3—Mo2 | 90.5 (1) | H4a—C4—H4b | 108.1 |
Mo2—O5—Mo1 | 127.0 (2) | N2iii—C5—H5 | 109.6 |
Mo3—O8—Mo2 | 121.2 (2) | C6—C5—H5 | 109.6 |
P1i—O9—Mo2 | 130.0 (2) | C4—C5—H5 | 109.6 |
P1i—O9—Mo3 | 134.2 (2) | C5—C6—H6a | 109.5 |
Mo2—O9—Mo3 | 95.3 (1) | C5—C6—H6b | 109.5 |
Mo3i—O10—Mo3 | 146.3 (2) | H6a—C6—H6b | 109.5 |
C2'—N1—C1 | 109.4 (7) | C5—C6—H6c | 109.5 |
C1'—N1'—C2 | 114.3 (7) | H6a—C6—H6c | 109.5 |
C2—C1—N1 | 109.8 (7) | H6b—C6—H6c | 109.5 |
N1'—C1'—C2' | 108.9 (7) | | |
| | | |
O3—P1—O2—Mo3 | 61.5 (2) | O9—Mo3—O8—Mo2 | −3.3 (2) |
O9i—P1—O2—Mo3 | −61.7 (2) | O2—Mo3—O8—Mo2 | 87.5 (2) |
O1—P1—O2—Mo3 | 179.3 (2) | O7—Mo2—O8—Mo3 | 96.9 (2) |
O11—Mo3—O2—P1 | 179.5 (2) | O6—Mo2—O8—Mo3 | −157.0 (2) |
O10—Mo3—O2—P1 | 76.3 (2) | O5—Mo2—O8—Mo3 | −29.7 (4) |
O8—Mo3—O2—P1 | −81.0 (2) | O9—Mo2—O8—Mo3 | 3.37 (17) |
O9—Mo3—O2—P1 | −9.8 (2) | O3—Mo2—O8—Mo3 | −69.1 (2) |
O2—P1—O3—Mo1 | −152.3 (2) | O7—Mo2—O9—P1i | 87.2 (3) |
O9i—P1—O3—Mo1 | −31.2 (3) | O6—Mo2—O9—P1i | −113.1 (4) |
O1—P1—O3—Mo1 | 86.3 (2) | O5—Mo2—O9—P1i | −10.8 (2) |
O2—P1—O3—Mo2 | −28.7 (3) | O8—Mo2—O9—P1i | −175.4 (3) |
O9i—P1—O3—Mo2 | 92.4 (2) | O3—Mo2—O9—P1i | −82.6 (2) |
O1—P1—O3—Mo2 | −150.1 (2) | O7—Mo2—O9—Mo3 | −99.8 (2) |
O4i—Mo1—O3—P1 | −120.5 (2) | O6—Mo2—O9—Mo3 | 60.0 (4) |
O4—Mo1—O3—P1 | 80.9 (8) | O5—Mo2—O9—Mo3 | 162.3 (1) |
O5i—Mo1—O3—P1 | −18.5 (2) | O8—Mo2—O9—Mo3 | −2.4 (1) |
O5—Mo1—O3—P1 | 137.6 (2) | O3—Mo2—O9—Mo3 | 90.4 (1) |
O3i—Mo1—O3—P1 | 54.3 (2) | O12—Mo3—O9—P1i | −80.1 (3) |
O4i—Mo1—O3—Mo2 | 101.4 (2) | O11—Mo3—O9—P1i | 138.2 (5) |
O4—Mo1—O3—Mo2 | −57.2 (8) | O10—Mo3—O9—P1i | 17.9 (2) |
O5i—Mo1—O3—Mo2 | −156.7 (1) | O8—Mo3—O9—P1i | 175.0 (3) |
O5—Mo1—O3—Mo2 | −0.5 (1) | O2—Mo3—O9—P1i | 97.1 (2) |
O3i—Mo1—O3—Mo2 | −83.8 (1) | O12—Mo3—O9—Mo2 | 107.4 (2) |
O7—Mo2—O3—P1 | −90.6 (6) | O11—Mo3—O9—Mo2 | −34.4 (6) |
O6—Mo2—O3—P1 | 120.6 (3) | O10—Mo3—O9—Mo2 | −154.7 (1) |
O5—Mo2—O3—P1 | −137.1 (3) | O8—Mo3—O9—Mo2 | 2.5 (1) |
O8—Mo2—O3—P1 | 24.1 (2) | O2—Mo3—O9—Mo2 | −75.5 (1) |
O9—Mo2—O3—P1 | −48.4 (2) | O12—Mo3—O10—Mo3i | 115.7 (1) |
O7—Mo2—O3—Mo1 | 47.0 (6) | O11—Mo3—O10—Mo3i | −139.1 (1) |
O6—Mo2—O3—Mo1 | −101.8 (1) | O8—Mo3—O10—Mo3i | −14.6 (2) |
O5—Mo2—O3—Mo1 | 0.5 (1) | O9—Mo3—O10—Mo3i | 28.41 (8) |
O8—Mo2—O3—Mo1 | 161.7 (1) | O2—Mo3—O10—Mo3i | −58.99 (8) |
O9—Mo2—O3—Mo1 | 89.2 (1) | C2'—N1—C1—C2 | −61 (1) |
O7—Mo2—O5—Mo1 | −169.7 (2) | C2—N1'—C1'—C2' | 57 (2) |
O6—Mo2—O5—Mo1 | 83.3 (2) | C1'—N1'—C2—C1 | −54 (2) |
O8—Mo2—O5—Mo1 | −43.0 (4) | C1'—N1'—C2—C3 | 175 (1) |
O9—Mo2—O5—Mo1 | −74.6 (2) | N1—C1—C2—N1' | 54 (1) |
O3—Mo2—O5—Mo1 | −0.8 (2) | N1—C1—C2—C3 | −178 (1) |
O4i—Mo1—O5—Mo2 | −83.0 (2) | N1'—C1'—C2'—N1 | −60 (1) |
O4—Mo1—O5—Mo2 | 170.8 (2) | N1'—C1'—C2'—C3ii | 175 (1) |
O5i—Mo1—O5—Mo2 | 44.0 (2) | C1—N1—C2'—C1' | 64 (1) |
O3i—Mo1—O5—Mo2 | 85.1 (2) | C1—N1—C2'—C3ii | −170.7 (9) |
O3—Mo1—O5—Mo2 | 0.8 (2) | C5iii—N2—C4—C5 | −59.2 (6) |
O12—Mo3—O8—Mo2 | −86.3 (2) | N2—C4—C5—N2iii | 56.0 (6) |
O11—Mo3—O8—Mo2 | 168.2 (2) | N2—C4—C5—C6 | 176.5 (4) |
O10—Mo3—O8—Mo2 | 42.8 (3) | | |
Symmetry codes: (i) −x, y, −z+1/2; (ii) −x, y, −z+3/2; (iii) −x+1, −y+1, −z+1. |
Hydrogen-bond geometry (Å, º) top
D—H···A | D—H | H···A | D···A | D—H···A |
O1—H1···O2iv | 0.82 | 1.85 | 2.656 (4) | 168 |
O1w—H1w1···O4 | 0.86 | 2.11 | 2.970 (7) | 177 |
N1—H1n1···O10v | 0.90 | 2.22 | 3.067 (9) | 158 |
N1—H1n2···O1wii | 0.90 | 1.69 | 2.59 (1) | 172 |
N1′—H1n3···O6vi | 0.90 | 2.16 | 2.825 (9) | 130 |
N1′—H1n4···O1w | 0.90 | 1.97 | 2.84 (1) | 160 |
N2—H2n1···O8vii | 0.90 | 2.17 | 2.950 (6) | 145 |
N2—H2n1···O11vii | 0.90 | 2.16 | 2.886 (6) | 137 |
N2—H2n2···O7 | 0.90 | 2.01 | 2.872 (6) | 160 |
Symmetry codes: (ii) −x, y, −z+3/2; (iv) −x, −y+1, −z; (v) −x, −y+1, −z+1; (vi) x−1/2, −y+3/2, z+1/2; (vii) x, −y+1, z+1/2. |
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