In the title compound, (C36H30NP2)[Mg2(C2H3O2)(C5H7O2)4]·H2O, the anion involves two magnesium centres, one bridging acetate, two chelating acetylacetonates and two acetylacetonates each with one bridging and one non-bridging oxygen donor. The water molecule acts as an additional bridge via hydrogen bonds to two acetylacetonate O atoms.
Supporting information
CCDC reference: 209897
Key indicators
- Single-crystal X-ray study
- T = 133 K
- Mean (C-C) = 0.004 Å
- R factor = 0.045
- wR factor = 0.105
- Data-to-parameter ratio = 14.4
checkCIF results
No syntax errors found
ADDSYM reports no extra symmetry
Alert Level B:
PLAT_601 Alert B Structure Contains Solvent Accessible VOIDS of 123.00 A 3
| Author response: There is no evidence that these voids are occupied (see
residual electron density) and I do not believe that they have
a deeper structural significance.
|
0 Alert Level A = Potentially serious problem
1 Alert Level B = Potential problem
0 Alert Level C = Please check
An equimolar mixture of 1,2-diethynylbenzene and (PPN)[Au(acac)2] in acetone was stirred at room temperature for 3.5 h and then filtered to remove traces of gold. The resulting solution was concentrated to dryness under reduced pressure; the residue was washed with diethyl ether (4 × 20 ml), filtered and air dried. Recrystallization from dichloromethane and diethyl ether yielded the expected organometallic gold polymer (24% yield), which was characterized by NMR and IR spectroscopy. However, attempts to grow single crystals of this product from a 1:1 mixture of dichloromethane and acetone (as solvent) and diethyl ether (as precipitant) yielded the crystal of the unexpected title compound (as well as amorphous material). Presumably the magnesium came from solvent drying agents. The acetate could have arisen from acac or acetone.
Water H atoms were refined freely, but with O—H distances restrained to be equal. Methyl H atoms were located in difference syntheses, idealized (C—H = 0.98 Å and H—C—H 109.5°) and refined on the basis of rigid groups allowed to rotate but not tip. Other H atoms were included using a riding model with fixed C—H bond lengths of 0.95 Å; Uiso(H) values were fixed at 1.2Ueq of the parent atom. To improve refinement stability, restraints (DELU and SIMU) were applied to displacement parameters of all non-H atoms.
Data collection: SMART (Bruker, 1998); cell refinement: SAINT (Bruker, 1998); data reduction: SAINT; program(s) used to solve structure: SHELXS97 (Sheldrick, 1990); program(s) used to refine structure: SHELXL97 (Sheldrick, 1997); molecular graphics: XP (Siemens, 1994); software used to prepare material for publication: SHELXL97.
Bis(triphenylphosphine)iminium µ-acetato-di-µ-acetylacetonato-bis[acetylacetonatomagnesate(II)] monohydrate
top
Crystal data top
(C36H30NP2)[Mg2(C2H3O2)(C5H7O2)4]·H2O | F(000) = 2240 |
Mr = 1060.65 | Dx = 1.259 Mg m−3 |
Monoclinic, P21/n | Mo Kα radiation, λ = 0.71073 Å |
a = 19.945 (2) Å | Cell parameters from 7821 reflections |
b = 14.069 (2) Å | θ = 2.5–25° |
c = 20.762 (3) Å | µ = 0.16 mm−1 |
β = 106.209 (6)° | T = 133 K |
V = 5594.6 (13) Å3 | Plate, colourless |
Z = 4 | 0.32 × 0.18 × 0.03 mm |
Data collection top
Bruker SMART 1000 CCD diffractometer | 5934 reflections with I > 2σ(I) |
Radiation source: fine-focus sealed tube | Rint = 0.087 |
Graphite monochromator | θmax = 25.0°, θmin = 1.7° |
Detector resolution: 8.192 pixels mm-1 | h = −23→23 |
ω and ϕ scans | k = −16→16 |
57401 measured reflections | l = −24→24 |
9872 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)] = 0.045 | Hydrogen site location: inferred from neighbouring sites |
wR(F2) = 0.105 | H atoms treated by a mixture of independent and constrained refinement |
S = 0.92 | w = 1/[σ2(Fo2) + (0.05P)2] where P = (Fo2 + 2Fc2)/3 |
9872 reflections | (Δ/σ)max = 0.001 |
684 parameters | Δρmax = 0.47 e Å−3 |
671 restraints | Δρmin = −0.30 e Å−3 |
Crystal data top
(C36H30NP2)[Mg2(C2H3O2)(C5H7O2)4]·H2O | V = 5594.6 (13) Å3 |
Mr = 1060.65 | Z = 4 |
Monoclinic, P21/n | Mo Kα radiation |
a = 19.945 (2) Å | µ = 0.16 mm−1 |
b = 14.069 (2) Å | T = 133 K |
c = 20.762 (3) Å | 0.32 × 0.18 × 0.03 mm |
β = 106.209 (6)° | |
Data collection top
Bruker SMART 1000 CCD diffractometer | 5934 reflections with I > 2σ(I) |
57401 measured reflections | Rint = 0.087 |
9872 independent reflections | |
Refinement top
R[F2 > 2σ(F2)] = 0.045 | 671 restraints |
wR(F2) = 0.105 | H atoms treated by a mixture of independent and constrained refinement |
S = 0.92 | Δρmax = 0.47 e Å−3 |
9872 reflections | Δρmin = −0.30 e Å−3 |
684 parameters | |
Special details top
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. |
Fractional atomic coordinates and isotropic or equivalent isotropic displacement parameters (Å2) top | x | y | z | Uiso*/Ueq | |
P1 | 0.42191 (3) | 0.65911 (5) | 0.14956 (3) | 0.02219 (17) | |
P2 | 0.51267 (3) | 0.79418 (5) | 0.24415 (3) | 0.02287 (17) | |
N | 0.48730 (10) | 0.72242 (15) | 0.18343 (10) | 0.0245 (5) | |
C11 | 0.39393 (12) | 0.68813 (18) | 0.06165 (12) | 0.0240 (6) | |
C12 | 0.44079 (13) | 0.73147 (19) | 0.03258 (13) | 0.0313 (7) | |
H12 | 0.4864 | 0.7469 | 0.0594 | 0.038* | |
C13 | 0.42148 (15) | 0.7521 (2) | −0.03479 (14) | 0.0436 (8) | |
H13 | 0.4539 | 0.7806 | −0.0548 | 0.052* | |
C14 | 0.35455 (15) | 0.7312 (2) | −0.07317 (14) | 0.0425 (8) | |
H14 | 0.3410 | 0.7461 | −0.1197 | 0.051* | |
C15 | 0.30726 (14) | 0.6891 (2) | −0.04482 (13) | 0.0355 (7) | |
H15 | 0.2613 | 0.6753 | −0.0716 | 0.043* | |
C16 | 0.32691 (13) | 0.66679 (19) | 0.02259 (13) | 0.0280 (7) | |
H16 | 0.2947 | 0.6369 | 0.0422 | 0.034* | |
C21 | 0.44520 (12) | 0.53561 (18) | 0.15850 (12) | 0.0230 (6) | |
C22 | 0.39833 (14) | 0.46608 (19) | 0.12550 (13) | 0.0313 (7) | |
H22 | 0.3542 | 0.4841 | 0.0967 | 0.038* | |
C23 | 0.41584 (15) | 0.3711 (2) | 0.13463 (15) | 0.0395 (8) | |
H23 | 0.3839 | 0.3236 | 0.1123 | 0.047* | |
C24 | 0.48076 (16) | 0.3455 (2) | 0.17681 (15) | 0.0414 (8) | |
H24 | 0.4928 | 0.2801 | 0.1833 | 0.050* | |
C25 | 0.52738 (15) | 0.4130 (2) | 0.20888 (14) | 0.0375 (7) | |
H25 | 0.5717 | 0.3944 | 0.2370 | 0.045* | |
C26 | 0.51012 (13) | 0.50835 (19) | 0.20041 (13) | 0.0282 (7) | |
H26 | 0.5424 | 0.5552 | 0.2231 | 0.034* | |
C31 | 0.34850 (12) | 0.67546 (18) | 0.18264 (12) | 0.0217 (6) | |
C32 | 0.30432 (13) | 0.7532 (2) | 0.16235 (13) | 0.0322 (7) | |
H32 | 0.3103 | 0.7940 | 0.1279 | 0.039* | |
C33 | 0.25221 (14) | 0.7707 (2) | 0.19217 (14) | 0.0381 (8) | |
H33 | 0.2222 | 0.8238 | 0.1780 | 0.046* | |
C34 | 0.24276 (14) | 0.7128 (2) | 0.24209 (14) | 0.0354 (7) | |
H34 | 0.2063 | 0.7255 | 0.2622 | 0.042* | |
C35 | 0.28601 (14) | 0.6365 (2) | 0.26281 (14) | 0.0352 (7) | |
H35 | 0.2798 | 0.5964 | 0.2975 | 0.042* | |
C36 | 0.33882 (13) | 0.61787 (19) | 0.23313 (13) | 0.0296 (7) | |
H36 | 0.3687 | 0.5648 | 0.2477 | 0.035* | |
C41 | 0.49764 (12) | 0.74953 (18) | 0.32009 (12) | 0.0233 (6) | |
C42 | 0.44168 (13) | 0.7793 (2) | 0.34263 (13) | 0.0334 (7) | |
H42 | 0.4136 | 0.8309 | 0.3210 | 0.040* | |
C43 | 0.42638 (14) | 0.7346 (2) | 0.39636 (14) | 0.0370 (7) | |
H43 | 0.3883 | 0.7559 | 0.4116 | 0.044* | |
C44 | 0.46649 (14) | 0.6593 (2) | 0.42747 (14) | 0.0346 (7) | |
H44 | 0.4558 | 0.6283 | 0.4641 | 0.042* | |
C45 | 0.52200 (14) | 0.6284 (2) | 0.40585 (14) | 0.0346 (7) | |
H45 | 0.5495 | 0.5763 | 0.4274 | 0.042* | |
C46 | 0.53770 (13) | 0.67349 (19) | 0.35263 (13) | 0.0295 (7) | |
H46 | 0.5763 | 0.6523 | 0.3381 | 0.035* | |
C51 | 0.46989 (13) | 0.90777 (18) | 0.22658 (14) | 0.0274 (6) | |
C52 | 0.43253 (14) | 0.9285 (2) | 0.16098 (15) | 0.0391 (8) | |
H52 | 0.4301 | 0.8830 | 0.1266 | 0.047* | |
C53 | 0.39866 (16) | 1.0154 (2) | 0.14539 (17) | 0.0491 (9) | |
H53 | 0.3732 | 1.0290 | 0.1004 | 0.059* | |
C54 | 0.40182 (16) | 1.0811 (2) | 0.19446 (18) | 0.0502 (9) | |
H54 | 0.3777 | 1.1397 | 0.1836 | 0.060* | |
C55 | 0.43974 (17) | 1.0630 (2) | 0.25938 (18) | 0.0515 (9) | |
H55 | 0.4425 | 1.1095 | 0.2932 | 0.062* | |
C56 | 0.47417 (15) | 0.9766 (2) | 0.27566 (15) | 0.0406 (8) | |
H56 | 0.5007 | 0.9645 | 0.3205 | 0.049* | |
C61 | 0.60425 (12) | 0.81189 (17) | 0.25425 (12) | 0.0211 (6) | |
C62 | 0.64216 (13) | 0.87757 (18) | 0.30002 (13) | 0.0285 (7) | |
H62 | 0.6210 | 0.9096 | 0.3295 | 0.034* | |
C63 | 0.71126 (13) | 0.89618 (19) | 0.30246 (14) | 0.0320 (7) | |
H63 | 0.7371 | 0.9418 | 0.3332 | 0.038* | |
C64 | 0.74240 (14) | 0.8487 (2) | 0.26040 (14) | 0.0321 (7) | |
H64 | 0.7896 | 0.8618 | 0.2622 | 0.038* | |
C65 | 0.70527 (13) | 0.7824 (2) | 0.21583 (13) | 0.0318 (7) | |
H65 | 0.7272 | 0.7488 | 0.1876 | 0.038* | |
C66 | 0.63633 (13) | 0.76471 (19) | 0.21209 (13) | 0.0279 (7) | |
H66 | 0.6106 | 0.7199 | 0.1805 | 0.033* | |
C111 | 0.86813 (14) | 0.32368 (18) | 0.00952 (14) | 0.0342 (7) | |
H11A | 0.9188 | 0.3243 | 0.0300 | 0.041* | |
H11B | 0.8575 | 0.2887 | −0.0330 | 0.041* | |
H11C | 0.8453 | 0.2925 | 0.0400 | 0.041* | |
C112 | 0.84192 (13) | 0.42395 (18) | −0.00338 (14) | 0.0248 (6) | |
C113 | 0.82031 (13) | 0.45767 (18) | −0.06934 (13) | 0.0269 (6) | |
H113 | 0.8244 | 0.4160 | −0.1041 | 0.032* | |
C114 | 0.79327 (13) | 0.54791 (19) | −0.08761 (13) | 0.0247 (6) | |
C115 | 0.77505 (14) | 0.5770 (2) | −0.16052 (13) | 0.0351 (7) | |
H11D | 0.7242 | 0.5800 | −0.1788 | 0.042* | |
H11E | 0.7940 | 0.5302 | −0.1858 | 0.042* | |
H11F | 0.7952 | 0.6396 | −0.1643 | 0.042* | |
C121 | 0.59392 (14) | 0.5250 (2) | 0.05313 (16) | 0.0446 (8) | |
H12A | 0.5845 | 0.4804 | 0.0154 | 0.054* | |
H12B | 0.5523 | 0.5639 | 0.0498 | 0.054* | |
H12C | 0.6057 | 0.4895 | 0.0954 | 0.054* | |
C122 | 0.65436 (14) | 0.5886 (2) | 0.05111 (13) | 0.0293 (7) | |
C123 | 0.64187 (13) | 0.68543 (19) | 0.04048 (13) | 0.0301 (7) | |
H123 | 0.5945 | 0.7054 | 0.0285 | 0.036* | |
C124 | 0.69178 (13) | 0.75524 (19) | 0.04563 (13) | 0.0264 (6) | |
C125 | 0.66871 (13) | 0.85673 (19) | 0.03821 (15) | 0.0374 (8) | |
H12D | 0.6818 | 0.8876 | 0.0823 | 0.045* | |
H12E | 0.6179 | 0.8595 | 0.0192 | 0.045* | |
H12F | 0.6913 | 0.8896 | 0.0083 | 0.045* | |
C131 | 0.89047 (14) | 0.6287 (2) | 0.27173 (13) | 0.0352 (7) | |
H13A | 0.8621 | 0.5744 | 0.2777 | 0.042* | |
H13B | 0.8847 | 0.6809 | 0.3010 | 0.042* | |
H13C | 0.9397 | 0.6099 | 0.2833 | 0.042* | |
C132 | 0.86732 (12) | 0.6610 (2) | 0.19976 (13) | 0.0251 (6) | |
C141 | 1.06767 (13) | 0.8945 (2) | 0.16354 (14) | 0.0363 (7) | |
H14A | 1.0606 | 0.9622 | 0.1528 | 0.044* | |
H14B | 1.1070 | 0.8710 | 0.1485 | 0.044* | |
H14C | 1.0777 | 0.8856 | 0.2121 | 0.044* | |
C142 | 1.00247 (13) | 0.84001 (19) | 0.12838 (13) | 0.0254 (6) | |
C143 | 1.00972 (13) | 0.74988 (19) | 0.10216 (13) | 0.0285 (7) | |
H143 | 1.0560 | 0.7279 | 0.1074 | 0.034* | |
C144 | 0.95620 (13) | 0.68989 (18) | 0.06943 (13) | 0.0265 (6) | |
C145 | 0.97446 (14) | 0.59661 (19) | 0.04343 (15) | 0.0374 (7) | |
H14D | 0.9590 | 0.5444 | 0.0670 | 0.045* | |
H14E | 1.0251 | 0.5928 | 0.0510 | 0.045* | |
H14F | 0.9512 | 0.5918 | −0.0047 | 0.045* | |
C151 | 0.80605 (17) | 1.0370 (2) | −0.05797 (15) | 0.0499 (9) | |
H15A | 0.8474 | 1.0195 | −0.0720 | 0.060* | |
H15B | 0.8038 | 1.1062 | −0.0542 | 0.060* | |
H15C | 0.7640 | 1.0142 | −0.0913 | 0.060* | |
C152 | 0.81044 (13) | 0.9926 (2) | 0.00857 (15) | 0.0328 (7) | |
C153 | 0.79877 (14) | 1.04807 (19) | 0.05984 (15) | 0.0347 (7) | |
H153 | 0.7896 | 1.1137 | 0.0509 | 0.042* | |
C154 | 0.79952 (13) | 1.0149 (2) | 0.12361 (15) | 0.0313 (7) | |
C155 | 0.78221 (16) | 1.0824 (2) | 0.17305 (16) | 0.0475 (9) | |
H15D | 0.7350 | 1.0692 | 0.1762 | 0.057* | |
H15E | 0.7846 | 1.1479 | 0.1579 | 0.057* | |
H15F | 0.8158 | 1.0739 | 0.2172 | 0.057* | |
Mg1 | 0.80572 (4) | 0.60725 (6) | 0.05550 (4) | 0.0243 (2) | |
Mg2 | 0.84854 (4) | 0.82136 (6) | 0.09911 (4) | 0.0241 (2) | |
O1 | 0.84228 (8) | 0.47271 (12) | 0.04795 (9) | 0.0282 (4) | |
O2 | 0.78170 (9) | 0.60996 (12) | −0.04744 (9) | 0.0287 (4) | |
O3 | 0.71300 (9) | 0.54911 (12) | 0.05942 (9) | 0.0316 (5) | |
O4 | 0.75824 (8) | 0.73889 (12) | 0.05953 (8) | 0.0246 (4) | |
O5 | 0.84854 (9) | 0.59797 (12) | 0.15578 (8) | 0.0284 (4) | |
O6 | 0.86739 (8) | 0.74914 (12) | 0.18864 (8) | 0.0271 (4) | |
O7 | 0.94568 (8) | 0.87945 (12) | 0.12574 (9) | 0.0294 (4) | |
O8 | 0.89090 (8) | 0.70740 (12) | 0.05902 (8) | 0.0237 (4) | |
O9 | 0.82423 (8) | 0.90349 (12) | 0.01302 (9) | 0.0296 (4) | |
O10 | 0.81245 (9) | 0.93038 (12) | 0.14365 (9) | 0.0297 (5) | |
O11 | 0.73891 (11) | 0.79538 (16) | −0.09771 (11) | 0.0410 (6) | |
H01 | 0.7489 (15) | 0.7364 (16) | −0.0859 (14) | 0.053 (10)* | |
H02 | 0.7672 (15) | 0.831 (2) | −0.0685 (15) | 0.075 (13)* | |
Atomic displacement parameters (Å2) top | U11 | U22 | U33 | U12 | U13 | U23 |
P1 | 0.0197 (4) | 0.0270 (4) | 0.0190 (4) | 0.0015 (3) | 0.0041 (3) | −0.0017 (3) |
P2 | 0.0212 (4) | 0.0260 (4) | 0.0205 (4) | 0.0024 (3) | 0.0043 (3) | −0.0025 (3) |
N | 0.0212 (11) | 0.0291 (12) | 0.0214 (12) | −0.0002 (10) | 0.0028 (9) | −0.0039 (11) |
C11 | 0.0246 (14) | 0.0276 (15) | 0.0192 (15) | 0.0038 (12) | 0.0050 (11) | 0.0000 (12) |
C12 | 0.0263 (15) | 0.0435 (18) | 0.0237 (16) | −0.0049 (13) | 0.0065 (12) | −0.0004 (14) |
C13 | 0.0417 (18) | 0.062 (2) | 0.0314 (18) | −0.0129 (16) | 0.0170 (15) | 0.0076 (17) |
C14 | 0.0491 (19) | 0.053 (2) | 0.0229 (17) | −0.0023 (16) | 0.0058 (14) | 0.0097 (16) |
C15 | 0.0292 (16) | 0.048 (2) | 0.0254 (17) | 0.0007 (14) | 0.0012 (13) | 0.0024 (15) |
C16 | 0.0251 (14) | 0.0365 (17) | 0.0217 (15) | −0.0003 (13) | 0.0054 (12) | 0.0040 (14) |
C21 | 0.0249 (14) | 0.0270 (15) | 0.0183 (15) | 0.0023 (12) | 0.0079 (12) | −0.0004 (12) |
C22 | 0.0323 (16) | 0.0332 (16) | 0.0261 (16) | 0.0013 (13) | 0.0044 (13) | −0.0007 (14) |
C23 | 0.0494 (19) | 0.0271 (16) | 0.042 (2) | −0.0023 (15) | 0.0121 (16) | −0.0064 (15) |
C24 | 0.059 (2) | 0.0282 (17) | 0.041 (2) | 0.0123 (15) | 0.0204 (17) | 0.0035 (15) |
C25 | 0.0367 (17) | 0.0434 (19) | 0.0334 (18) | 0.0152 (15) | 0.0117 (14) | 0.0075 (16) |
C26 | 0.0252 (15) | 0.0347 (17) | 0.0241 (16) | 0.0036 (13) | 0.0060 (12) | −0.0026 (14) |
C31 | 0.0194 (13) | 0.0271 (15) | 0.0174 (14) | −0.0013 (11) | 0.0032 (11) | −0.0023 (12) |
C32 | 0.0322 (16) | 0.0371 (17) | 0.0302 (17) | 0.0062 (13) | 0.0135 (13) | 0.0060 (14) |
C33 | 0.0325 (16) | 0.0430 (19) | 0.0418 (19) | 0.0157 (14) | 0.0151 (14) | 0.0057 (16) |
C34 | 0.0316 (16) | 0.0421 (18) | 0.0383 (19) | −0.0023 (14) | 0.0191 (14) | −0.0097 (16) |
C35 | 0.0448 (18) | 0.0349 (17) | 0.0313 (18) | −0.0100 (14) | 0.0196 (15) | −0.0027 (14) |
C36 | 0.0306 (15) | 0.0316 (16) | 0.0263 (16) | 0.0011 (13) | 0.0078 (13) | 0.0001 (14) |
C41 | 0.0239 (14) | 0.0264 (15) | 0.0186 (15) | −0.0023 (12) | 0.0041 (11) | −0.0071 (12) |
C42 | 0.0297 (16) | 0.0437 (18) | 0.0261 (17) | 0.0046 (14) | 0.0065 (13) | −0.0012 (15) |
C43 | 0.0304 (16) | 0.054 (2) | 0.0291 (18) | 0.0002 (15) | 0.0126 (14) | −0.0035 (16) |
C44 | 0.0398 (17) | 0.0413 (18) | 0.0234 (16) | −0.0109 (15) | 0.0097 (14) | −0.0023 (14) |
C45 | 0.0366 (17) | 0.0323 (17) | 0.0330 (18) | −0.0023 (14) | 0.0067 (14) | 0.0023 (14) |
C46 | 0.0295 (15) | 0.0320 (16) | 0.0279 (17) | 0.0016 (13) | 0.0097 (13) | −0.0044 (14) |
C51 | 0.0248 (15) | 0.0263 (15) | 0.0322 (17) | 0.0031 (12) | 0.0096 (13) | 0.0010 (14) |
C52 | 0.0412 (18) | 0.0356 (17) | 0.0363 (19) | 0.0073 (14) | 0.0042 (15) | −0.0005 (15) |
C53 | 0.0454 (19) | 0.046 (2) | 0.050 (2) | 0.0150 (16) | 0.0046 (17) | 0.0147 (18) |
C54 | 0.048 (2) | 0.0364 (19) | 0.069 (3) | 0.0222 (16) | 0.0198 (18) | 0.0118 (19) |
C55 | 0.062 (2) | 0.0365 (19) | 0.059 (2) | 0.0160 (17) | 0.0228 (19) | −0.0058 (18) |
C56 | 0.0444 (18) | 0.0394 (18) | 0.0364 (19) | 0.0092 (15) | 0.0088 (15) | −0.0051 (16) |
C61 | 0.0222 (13) | 0.0219 (14) | 0.0183 (15) | 0.0001 (11) | 0.0039 (11) | 0.0024 (12) |
C62 | 0.0311 (15) | 0.0305 (16) | 0.0237 (16) | 0.0032 (13) | 0.0073 (13) | −0.0024 (13) |
C63 | 0.0292 (16) | 0.0296 (16) | 0.0321 (17) | −0.0062 (13) | 0.0001 (13) | 0.0004 (14) |
C64 | 0.0247 (15) | 0.0408 (18) | 0.0299 (17) | −0.0013 (13) | 0.0063 (13) | 0.0095 (15) |
C65 | 0.0289 (15) | 0.0452 (18) | 0.0235 (16) | 0.0022 (14) | 0.0108 (13) | 0.0022 (14) |
C66 | 0.0283 (15) | 0.0331 (16) | 0.0212 (16) | −0.0002 (13) | 0.0054 (12) | −0.0045 (13) |
C111 | 0.0373 (17) | 0.0293 (16) | 0.0372 (18) | 0.0003 (13) | 0.0124 (14) | −0.0017 (14) |
C112 | 0.0215 (14) | 0.0226 (14) | 0.0319 (17) | −0.0033 (12) | 0.0102 (12) | −0.0022 (14) |
C113 | 0.0303 (15) | 0.0247 (15) | 0.0279 (16) | −0.0032 (12) | 0.0120 (13) | −0.0054 (13) |
C114 | 0.0216 (14) | 0.0287 (16) | 0.0250 (16) | −0.0086 (12) | 0.0083 (12) | −0.0037 (13) |
C115 | 0.0402 (17) | 0.0349 (17) | 0.0299 (17) | −0.0032 (14) | 0.0095 (14) | −0.0012 (14) |
C121 | 0.0358 (17) | 0.0419 (18) | 0.061 (2) | −0.0105 (15) | 0.0212 (16) | −0.0105 (17) |
C122 | 0.0271 (15) | 0.0388 (17) | 0.0233 (16) | −0.0079 (13) | 0.0093 (13) | −0.0110 (14) |
C123 | 0.0187 (14) | 0.0377 (17) | 0.0330 (17) | −0.0015 (13) | 0.0058 (12) | −0.0067 (14) |
C124 | 0.0236 (14) | 0.0346 (16) | 0.0203 (15) | 0.0037 (12) | 0.0050 (12) | −0.0003 (13) |
C125 | 0.0262 (15) | 0.0364 (17) | 0.049 (2) | 0.0076 (13) | 0.0098 (14) | 0.0075 (16) |
C131 | 0.0422 (17) | 0.0348 (17) | 0.0288 (17) | −0.0026 (14) | 0.0104 (14) | −0.0041 (14) |
C132 | 0.0202 (14) | 0.0308 (17) | 0.0247 (16) | 0.0005 (12) | 0.0069 (12) | −0.0015 (14) |
C141 | 0.0273 (15) | 0.0364 (17) | 0.046 (2) | −0.0032 (13) | 0.0110 (14) | −0.0032 (15) |
C142 | 0.0248 (14) | 0.0283 (15) | 0.0250 (16) | −0.0035 (12) | 0.0101 (12) | 0.0031 (13) |
C143 | 0.0211 (14) | 0.0317 (16) | 0.0346 (17) | 0.0015 (12) | 0.0111 (13) | 0.0001 (14) |
C144 | 0.0286 (15) | 0.0266 (15) | 0.0268 (16) | 0.0024 (12) | 0.0119 (13) | 0.0044 (13) |
C145 | 0.0301 (16) | 0.0339 (17) | 0.052 (2) | 0.0028 (13) | 0.0172 (14) | −0.0071 (16) |
C151 | 0.061 (2) | 0.0390 (19) | 0.050 (2) | 0.0051 (16) | 0.0171 (17) | 0.0181 (17) |
C152 | 0.0273 (16) | 0.0295 (17) | 0.0404 (19) | −0.0022 (13) | 0.0074 (14) | 0.0062 (15) |
C153 | 0.0359 (17) | 0.0214 (15) | 0.0464 (19) | 0.0029 (13) | 0.0106 (15) | 0.0061 (15) |
C154 | 0.0230 (15) | 0.0251 (16) | 0.0453 (19) | −0.0003 (12) | 0.0088 (14) | −0.0021 (15) |
C155 | 0.053 (2) | 0.0309 (18) | 0.063 (2) | 0.0038 (15) | 0.0246 (17) | −0.0097 (17) |
Mg1 | 0.0248 (5) | 0.0237 (5) | 0.0244 (5) | 0.0000 (4) | 0.0069 (4) | −0.0011 (4) |
Mg2 | 0.0234 (5) | 0.0212 (5) | 0.0281 (5) | 0.0014 (4) | 0.0079 (4) | −0.0007 (4) |
O1 | 0.0322 (11) | 0.0264 (10) | 0.0264 (11) | 0.0012 (8) | 0.0087 (9) | −0.0018 (9) |
O2 | 0.0327 (10) | 0.0258 (10) | 0.0261 (11) | 0.0011 (9) | 0.0060 (8) | −0.0015 (9) |
O3 | 0.0260 (10) | 0.0295 (11) | 0.0392 (12) | −0.0031 (8) | 0.0091 (9) | −0.0010 (9) |
O4 | 0.0196 (9) | 0.0272 (10) | 0.0263 (10) | 0.0007 (8) | 0.0056 (8) | −0.0001 (8) |
O5 | 0.0343 (11) | 0.0260 (10) | 0.0227 (11) | −0.0029 (9) | 0.0045 (8) | 0.0004 (9) |
O6 | 0.0294 (10) | 0.0243 (10) | 0.0279 (11) | −0.0005 (8) | 0.0087 (8) | −0.0018 (9) |
O7 | 0.0228 (10) | 0.0269 (10) | 0.0395 (12) | −0.0006 (8) | 0.0103 (9) | −0.0018 (9) |
O8 | 0.0219 (9) | 0.0245 (10) | 0.0260 (10) | 0.0016 (8) | 0.0090 (8) | −0.0002 (8) |
O9 | 0.0309 (10) | 0.0259 (11) | 0.0321 (11) | 0.0024 (9) | 0.0091 (9) | 0.0031 (9) |
O10 | 0.0320 (11) | 0.0231 (10) | 0.0367 (12) | 0.0038 (8) | 0.0138 (9) | 0.0002 (9) |
O11 | 0.0537 (14) | 0.0352 (14) | 0.0302 (13) | 0.0055 (12) | 0.0053 (11) | 0.0035 (12) |
Geometric parameters (Å, º) top
P1—N | 1.574 (2) | C111—C112 | 1.502 (3) |
P1—C21 | 1.795 (3) | C111—H11A | 0.9800 |
P1—C31 | 1.797 (2) | C111—H11B | 0.9800 |
P1—C11 | 1.800 (3) | C111—H11C | 0.9800 |
P2—N | 1.584 (2) | C112—O1 | 1.266 (3) |
P2—C61 | 1.797 (2) | C112—C113 | 1.399 (4) |
P2—C41 | 1.798 (3) | C113—C114 | 1.390 (4) |
P2—C51 | 1.800 (3) | C113—H113 | 0.9500 |
C11—C12 | 1.387 (3) | C114—O2 | 1.272 (3) |
C11—C16 | 1.389 (3) | C114—C115 | 1.511 (4) |
C12—C13 | 1.374 (3) | C115—H11D | 0.9800 |
C12—H12 | 0.9500 | C115—H11E | 0.9800 |
C13—C14 | 1.382 (4) | C115—H11F | 0.9800 |
C13—H13 | 0.9500 | C121—C122 | 1.511 (4) |
C14—C15 | 1.378 (4) | C121—H12A | 0.9800 |
C14—H14 | 0.9500 | C121—H12B | 0.9800 |
C15—C16 | 1.380 (3) | C121—H12C | 0.9800 |
C15—H15 | 0.9500 | C122—O3 | 1.262 (3) |
C16—H16 | 0.9500 | C122—C123 | 1.392 (4) |
C21—C22 | 1.394 (3) | C123—C124 | 1.381 (3) |
C21—C26 | 1.397 (3) | C123—H123 | 0.9500 |
C22—C23 | 1.381 (4) | C124—O4 | 1.296 (3) |
C22—H22 | 0.9500 | C124—C125 | 1.495 (4) |
C23—C24 | 1.393 (4) | C125—H12D | 0.9800 |
C23—H23 | 0.9500 | C125—H12E | 0.9800 |
C24—C25 | 1.365 (4) | C125—H12F | 0.9800 |
C24—H24 | 0.9500 | C131—C132 | 1.506 (4) |
C25—C26 | 1.384 (4) | C131—H13A | 0.9800 |
C25—H25 | 0.9500 | C131—H13B | 0.9800 |
C26—H26 | 0.9500 | C131—H13C | 0.9800 |
C31—C36 | 1.380 (3) | C132—O5 | 1.253 (3) |
C31—C32 | 1.394 (3) | C132—O6 | 1.261 (3) |
C32—C33 | 1.373 (3) | C141—C142 | 1.511 (3) |
C32—H32 | 0.9500 | C141—H14A | 0.9800 |
C33—C34 | 1.373 (4) | C141—H14B | 0.9800 |
C33—H33 | 0.9500 | C141—H14C | 0.9800 |
C34—C35 | 1.368 (4) | C142—O7 | 1.249 (3) |
C34—H34 | 0.9500 | C142—C143 | 1.403 (3) |
C35—C36 | 1.386 (3) | C143—C144 | 1.382 (3) |
C35—H35 | 0.9500 | C143—H143 | 0.9500 |
C36—H36 | 0.9500 | C144—O8 | 1.283 (3) |
C41—C42 | 1.390 (3) | C144—C145 | 1.502 (3) |
C41—C46 | 1.392 (3) | C145—H14D | 0.9800 |
C42—C43 | 1.387 (4) | C145—H14E | 0.9800 |
C42—H42 | 0.9500 | C145—H14F | 0.9800 |
C43—C44 | 1.376 (4) | C151—C152 | 1.496 (4) |
C43—H43 | 0.9500 | C151—H15A | 0.9800 |
C44—C45 | 1.376 (4) | C151—H15B | 0.9800 |
C44—H44 | 0.9500 | C151—H15C | 0.9800 |
C45—C46 | 1.383 (4) | C152—O9 | 1.281 (3) |
C45—H45 | 0.9500 | C152—C153 | 1.391 (4) |
C46—H46 | 0.9500 | C153—C154 | 1.400 (4) |
C51—C52 | 1.389 (4) | C153—H153 | 0.9500 |
C51—C56 | 1.391 (4) | C154—O10 | 1.262 (3) |
C52—C53 | 1.391 (4) | C154—C155 | 1.508 (4) |
C52—H52 | 0.9500 | C155—H15D | 0.9800 |
C53—C54 | 1.364 (4) | C155—H15E | 0.9800 |
C53—H53 | 0.9500 | C155—H15F | 0.9800 |
C54—C55 | 1.373 (4) | Mg1—O5 | 2.0220 (19) |
C54—H54 | 0.9500 | Mg1—O3 | 2.0445 (19) |
C55—C56 | 1.391 (4) | Mg1—O1 | 2.0501 (19) |
C55—H55 | 0.9500 | Mg1—O2 | 2.0560 (19) |
C56—H56 | 0.9500 | Mg1—O4 | 2.0926 (18) |
C61—C62 | 1.388 (3) | Mg1—O8 | 2.1926 (18) |
C61—C66 | 1.389 (3) | Mg1—Mg2 | 3.1925 (12) |
C62—C63 | 1.390 (3) | Mg2—O10 | 2.0243 (19) |
C62—H62 | 0.9500 | Mg2—O7 | 2.0320 (18) |
C63—C64 | 1.377 (4) | Mg2—O6 | 2.0588 (19) |
C63—H63 | 0.9500 | Mg2—O9 | 2.0692 (19) |
C64—C65 | 1.376 (4) | Mg2—O8 | 2.0904 (18) |
C64—H64 | 0.9500 | Mg2—O4 | 2.1069 (18) |
C65—C66 | 1.378 (3) | O11—H01 | 0.87 (2) |
C65—H65 | 0.9500 | O11—H02 | 0.87 (2) |
C66—H66 | 0.9500 | | |
| | | |
N—P1—C21 | 110.09 (11) | C114—C113—C112 | 124.5 (3) |
N—P1—C31 | 114.76 (11) | C114—C113—H113 | 117.7 |
C21—P1—C31 | 107.42 (12) | C112—C113—H113 | 117.7 |
N—P1—C11 | 107.96 (12) | O2—C114—C113 | 125.1 (2) |
C21—P1—C11 | 108.81 (12) | O2—C114—C115 | 115.7 (2) |
C31—P1—C11 | 107.66 (11) | C113—C114—C115 | 119.1 (2) |
N—P2—C61 | 105.65 (11) | C114—C115—H11D | 109.5 |
N—P2—C41 | 112.38 (12) | C114—C115—H11E | 109.5 |
C61—P2—C41 | 111.03 (11) | H11D—C115—H11E | 109.5 |
N—P2—C51 | 112.12 (12) | C114—C115—H11F | 109.5 |
C61—P2—C51 | 108.02 (11) | H11D—C115—H11F | 109.5 |
C41—P2—C51 | 107.59 (12) | H11E—C115—H11F | 109.5 |
P1—N—P2 | 139.22 (14) | C122—C121—H12A | 109.5 |
C12—C11—C16 | 119.8 (2) | C122—C121—H12B | 109.5 |
C12—C11—P1 | 119.00 (19) | H12A—C121—H12B | 109.5 |
C16—C11—P1 | 121.2 (2) | C122—C121—H12C | 109.5 |
C13—C12—C11 | 120.3 (2) | H12A—C121—H12C | 109.5 |
C13—C12—H12 | 119.9 | H12B—C121—H12C | 109.5 |
C11—C12—H12 | 119.9 | O3—C122—C123 | 124.8 (2) |
C12—C13—C14 | 119.5 (3) | O3—C122—C121 | 116.9 (3) |
C12—C13—H13 | 120.2 | C123—C122—C121 | 118.4 (2) |
C14—C13—H13 | 120.2 | C124—C123—C122 | 126.2 (2) |
C15—C14—C13 | 120.8 (3) | C124—C123—H123 | 116.9 |
C15—C14—H14 | 119.6 | C122—C123—H123 | 116.9 |
C13—C14—H14 | 119.6 | O4—C124—C123 | 124.1 (2) |
C14—C15—C16 | 119.8 (3) | O4—C124—C125 | 117.3 (2) |
C14—C15—H15 | 120.1 | C123—C124—C125 | 118.5 (2) |
C16—C15—H15 | 120.1 | C124—C125—H12D | 109.5 |
C15—C16—C11 | 119.8 (2) | C124—C125—H12E | 109.5 |
C15—C16—H16 | 120.1 | H12D—C125—H12E | 109.5 |
C11—C16—H16 | 120.1 | C124—C125—H12F | 109.5 |
C22—C21—C26 | 119.4 (2) | H12D—C125—H12F | 109.5 |
C22—C21—P1 | 120.66 (19) | H12E—C125—H12F | 109.5 |
C26—C21—P1 | 119.9 (2) | C132—C131—H13A | 109.5 |
C23—C22—C21 | 120.2 (3) | C132—C131—H13B | 109.5 |
C23—C22—H22 | 119.9 | H13A—C131—H13B | 109.5 |
C21—C22—H22 | 119.9 | C132—C131—H13C | 109.5 |
C22—C23—C24 | 119.5 (3) | H13A—C131—H13C | 109.5 |
C22—C23—H23 | 120.3 | H13B—C131—H13C | 109.5 |
C24—C23—H23 | 120.3 | O5—C132—O6 | 125.3 (2) |
C25—C24—C23 | 120.9 (3) | O5—C132—C131 | 117.1 (2) |
C25—C24—H24 | 119.5 | O6—C132—C131 | 117.6 (2) |
C23—C24—H24 | 119.5 | C142—C141—H14A | 109.5 |
C24—C25—C26 | 120.1 (3) | C142—C141—H14B | 109.5 |
C24—C25—H25 | 120.0 | H14A—C141—H14B | 109.5 |
C26—C25—H25 | 120.0 | C142—C141—H14C | 109.5 |
C25—C26—C21 | 120.0 (3) | H14A—C141—H14C | 109.5 |
C25—C26—H26 | 120.0 | H14B—C141—H14C | 109.5 |
C21—C26—H26 | 120.0 | O7—C142—C143 | 125.1 (2) |
C36—C31—C32 | 118.6 (2) | O7—C142—C141 | 116.3 (2) |
C36—C31—P1 | 121.10 (19) | C143—C142—C141 | 118.6 (2) |
C32—C31—P1 | 119.9 (2) | C144—C143—C142 | 126.4 (2) |
C33—C32—C31 | 120.0 (3) | C144—C143—H143 | 116.8 |
C33—C32—H32 | 120.0 | C142—C143—H143 | 116.8 |
C31—C32—H32 | 120.0 | O8—C144—C143 | 125.0 (2) |
C32—C33—C34 | 121.0 (3) | O8—C144—C145 | 116.3 (2) |
C32—C33—H33 | 119.5 | C143—C144—C145 | 118.6 (2) |
C34—C33—H33 | 119.5 | C144—C145—H14D | 109.5 |
C35—C34—C33 | 119.7 (3) | C144—C145—H14E | 109.5 |
C35—C34—H34 | 120.1 | H14D—C145—H14E | 109.5 |
C33—C34—H34 | 120.1 | C144—C145—H14F | 109.5 |
C34—C35—C36 | 120.0 (3) | H14D—C145—H14F | 109.5 |
C34—C35—H35 | 120.0 | H14E—C145—H14F | 109.5 |
C36—C35—H35 | 120.0 | C152—C151—H15A | 109.5 |
C31—C36—C35 | 120.7 (3) | C152—C151—H15B | 109.5 |
C31—C36—H36 | 119.6 | H15A—C151—H15B | 109.5 |
C35—C36—H36 | 119.6 | C152—C151—H15C | 109.5 |
C42—C41—C46 | 118.3 (2) | H15A—C151—H15C | 109.5 |
C42—C41—P2 | 122.4 (2) | H15B—C151—H15C | 109.5 |
C46—C41—P2 | 118.7 (2) | O9—C152—C153 | 124.9 (3) |
C43—C42—C41 | 120.8 (3) | O9—C152—C151 | 115.5 (3) |
C43—C42—H42 | 119.6 | C153—C152—C151 | 119.5 (3) |
C41—C42—H42 | 119.6 | C152—C153—C154 | 125.2 (3) |
C44—C43—C42 | 119.8 (3) | C152—C153—H153 | 117.4 |
C44—C43—H43 | 120.1 | C154—C153—H153 | 117.4 |
C42—C43—H43 | 120.1 | O10—C154—C153 | 125.0 (3) |
C43—C44—C45 | 120.3 (3) | O10—C154—C155 | 115.7 (3) |
C43—C44—H44 | 119.8 | C153—C154—C155 | 119.3 (3) |
C45—C44—H44 | 119.8 | C154—C155—H15D | 109.5 |
C44—C45—C46 | 119.9 (3) | C154—C155—H15E | 109.5 |
C44—C45—H45 | 120.0 | H15D—C155—H15E | 109.5 |
C46—C45—H45 | 120.0 | C154—C155—H15F | 109.5 |
C45—C46—C41 | 120.8 (3) | H15D—C155—H15F | 109.5 |
C45—C46—H46 | 119.6 | H15E—C155—H15F | 109.5 |
C41—C46—H46 | 119.6 | O5—Mg1—O3 | 93.44 (8) |
C52—C51—C56 | 118.6 (3) | O5—Mg1—O1 | 87.83 (8) |
C52—C51—P2 | 118.6 (2) | O3—Mg1—O1 | 88.78 (8) |
C56—C51—P2 | 122.7 (2) | O5—Mg1—O2 | 168.66 (8) |
C51—C52—C53 | 120.4 (3) | O3—Mg1—O2 | 95.62 (8) |
C51—C52—H52 | 119.8 | O1—Mg1—O2 | 85.55 (8) |
C53—C52—H52 | 119.8 | O5—Mg1—O4 | 94.69 (7) |
C54—C53—C52 | 120.3 (3) | O3—Mg1—O4 | 85.87 (7) |
C54—C53—H53 | 119.9 | O1—Mg1—O4 | 174.21 (8) |
C52—C53—H53 | 119.9 | O2—Mg1—O4 | 92.77 (7) |
C53—C54—C55 | 120.4 (3) | O5—Mg1—O8 | 84.64 (7) |
C53—C54—H54 | 119.8 | O3—Mg1—O8 | 163.10 (8) |
C55—C54—H54 | 119.8 | O1—Mg1—O8 | 107.88 (7) |
C54—C55—C56 | 120.0 (3) | O2—Mg1—O8 | 88.64 (7) |
C54—C55—H55 | 120.0 | O4—Mg1—O8 | 77.58 (7) |
C56—C55—H55 | 120.0 | O10—Mg2—O7 | 90.26 (8) |
C51—C56—C55 | 120.4 (3) | O10—Mg2—O6 | 87.71 (8) |
C51—C56—H56 | 119.8 | O7—Mg2—O6 | 91.88 (7) |
C55—C56—H56 | 119.8 | O10—Mg2—O9 | 86.79 (8) |
C62—C61—C66 | 119.4 (2) | O7—Mg2—O9 | 89.21 (7) |
C62—C61—P2 | 120.92 (19) | O6—Mg2—O9 | 174.40 (8) |
C66—C61—P2 | 119.49 (19) | O10—Mg2—O8 | 176.24 (8) |
C61—C62—C63 | 119.7 (2) | O7—Mg2—O8 | 87.49 (7) |
C61—C62—H62 | 120.2 | O6—Mg2—O8 | 89.35 (7) |
C63—C62—H62 | 120.2 | O9—Mg2—O8 | 96.18 (8) |
C64—C63—C62 | 120.2 (3) | O10—Mg2—O4 | 102.78 (7) |
C64—C63—H63 | 119.9 | O7—Mg2—O4 | 166.88 (8) |
C62—C63—H63 | 119.9 | O6—Mg2—O4 | 90.07 (7) |
C65—C64—C63 | 120.1 (3) | O9—Mg2—O4 | 90.11 (7) |
C65—C64—H64 | 119.9 | O8—Mg2—O4 | 79.56 (7) |
C63—C64—H64 | 119.9 | C112—O1—Mg1 | 130.25 (17) |
C64—C65—C66 | 120.1 (3) | C114—O2—Mg1 | 129.52 (17) |
C64—C65—H65 | 119.9 | C122—O3—Mg1 | 129.24 (17) |
C66—C65—H65 | 119.9 | C124—O4—Mg1 | 126.47 (16) |
C65—C66—C61 | 120.4 (2) | C124—O4—Mg2 | 134.34 (16) |
C65—C66—H66 | 119.8 | Mg1—O4—Mg2 | 98.97 (7) |
C61—C66—H66 | 119.8 | C132—O5—Mg1 | 131.24 (17) |
C112—C111—H11A | 109.5 | C132—O6—Mg2 | 129.89 (17) |
C112—C111—H11B | 109.5 | C142—O7—Mg2 | 128.14 (17) |
H11A—C111—H11B | 109.5 | C144—O8—Mg2 | 125.75 (16) |
C112—C111—H11C | 109.5 | C144—O8—Mg1 | 128.52 (16) |
H11A—C111—H11C | 109.5 | Mg2—O8—Mg1 | 96.35 (7) |
H11B—C111—H11C | 109.5 | C152—O9—Mg2 | 127.05 (18) |
O1—C112—C113 | 124.6 (2) | C154—O10—Mg2 | 128.98 (18) |
O1—C112—C111 | 116.0 (2) | H01—O11—H02 | 108 (3) |
C113—C112—C111 | 119.3 (2) | | |
| | | |
C21—P1—N—P2 | −115.0 (2) | C142—C143—C144—C145 | 178.6 (3) |
C31—P1—N—P2 | 6.4 (3) | O9—C152—C153—C154 | −0.8 (4) |
C11—P1—N—P2 | 126.4 (2) | C151—C152—C153—C154 | 178.3 (3) |
C61—P2—N—P1 | 167.9 (2) | C152—C153—C154—O10 | 1.7 (4) |
C41—P2—N—P1 | 46.7 (2) | C152—C153—C154—C155 | −176.8 (3) |
C51—P2—N—P1 | −74.7 (2) | C113—C112—O1—Mg1 | 6.1 (4) |
N—P1—C11—C12 | 20.6 (2) | C111—C112—O1—Mg1 | −175.11 (16) |
C21—P1—C11—C12 | −98.9 (2) | O5—Mg1—O1—C112 | −173.7 (2) |
C31—P1—C11—C12 | 145.0 (2) | O3—Mg1—O1—C112 | 92.8 (2) |
N—P1—C11—C16 | −160.3 (2) | O2—Mg1—O1—C112 | −2.9 (2) |
C21—P1—C11—C16 | 80.3 (2) | O8—Mg1—O1—C112 | −90.0 (2) |
C31—P1—C11—C16 | −35.9 (2) | C113—C114—O2—Mg1 | 6.4 (4) |
C16—C11—C12—C13 | −0.9 (4) | C115—C114—O2—Mg1 | −174.07 (16) |
P1—C11—C12—C13 | 178.3 (2) | O5—Mg1—O2—C114 | 51.2 (5) |
C11—C12—C13—C14 | 1.3 (4) | O3—Mg1—O2—C114 | −91.6 (2) |
C12—C13—C14—C15 | −0.7 (5) | O1—Mg1—O2—C114 | −3.2 (2) |
C13—C14—C15—C16 | −0.4 (5) | O4—Mg1—O2—C114 | −177.7 (2) |
C14—C15—C16—C11 | 0.8 (4) | O8—Mg1—O2—C114 | 104.8 (2) |
C12—C11—C16—C15 | −0.2 (4) | C123—C122—O3—Mg1 | −3.6 (4) |
P1—C11—C16—C15 | −179.3 (2) | C121—C122—O3—Mg1 | 176.49 (18) |
N—P1—C21—C22 | −172.1 (2) | O5—Mg1—O3—C122 | 108.1 (2) |
C31—P1—C21—C22 | 62.3 (2) | O1—Mg1—O3—C122 | −164.2 (2) |
C11—P1—C21—C22 | −54.0 (2) | O2—Mg1—O3—C122 | −78.7 (2) |
N—P1—C21—C26 | 9.8 (2) | O4—Mg1—O3—C122 | 13.6 (2) |
C31—P1—C21—C26 | −115.8 (2) | O8—Mg1—O3—C122 | 25.2 (4) |
C11—P1—C21—C26 | 127.9 (2) | C123—C124—O4—Mg1 | 15.4 (4) |
C26—C21—C22—C23 | 0.5 (4) | C125—C124—O4—Mg1 | −167.78 (18) |
P1—C21—C22—C23 | −177.7 (2) | C123—C124—O4—Mg2 | −158.0 (2) |
C21—C22—C23—C24 | −0.3 (4) | C125—C124—O4—Mg2 | 18.8 (4) |
C22—C23—C24—C25 | −0.4 (5) | O5—Mg1—O4—C124 | −112.3 (2) |
C23—C24—C25—C26 | 0.8 (5) | O3—Mg1—O4—C124 | −19.2 (2) |
C24—C25—C26—C21 | −0.6 (4) | O2—Mg1—O4—C124 | 76.3 (2) |
C22—C21—C26—C25 | 0.0 (4) | O8—Mg1—O4—C124 | 164.3 (2) |
P1—C21—C26—C25 | 178.1 (2) | O5—Mg1—O4—Mg2 | 62.92 (8) |
N—P1—C31—C36 | −93.7 (2) | O3—Mg1—O4—Mg2 | 156.04 (8) |
C21—P1—C31—C36 | 29.0 (2) | O2—Mg1—O4—Mg2 | −108.53 (8) |
C11—P1—C31—C36 | 146.1 (2) | O8—Mg1—O4—Mg2 | −20.53 (7) |
N—P1—C31—C32 | 79.6 (2) | O10—Mg2—O4—C124 | 19.0 (2) |
C21—P1—C31—C32 | −157.7 (2) | O7—Mg2—O4—C124 | −154.7 (3) |
C11—P1—C31—C32 | −40.7 (2) | O6—Mg2—O4—C124 | 106.7 (2) |
C36—C31—C32—C33 | −0.4 (4) | O9—Mg2—O4—C124 | −67.7 (2) |
P1—C31—C32—C33 | −173.9 (2) | O8—Mg2—O4—C124 | −164.0 (2) |
C31—C32—C33—C34 | 0.1 (4) | O10—Mg2—O4—Mg1 | −155.57 (8) |
C32—C33—C34—C35 | 0.3 (4) | O7—Mg2—O4—Mg1 | 30.7 (4) |
C33—C34—C35—C36 | −0.4 (4) | O6—Mg2—O4—Mg1 | −67.90 (8) |
C32—C31—C36—C35 | 0.4 (4) | O9—Mg2—O4—Mg1 | 117.69 (8) |
P1—C31—C36—C35 | 173.8 (2) | O8—Mg2—O4—Mg1 | 21.42 (7) |
C34—C35—C36—C31 | 0.0 (4) | O6—C132—O5—Mg1 | −5.3 (4) |
N—P2—C41—C42 | −100.9 (2) | C131—C132—O5—Mg1 | 173.58 (16) |
C61—P2—C41—C42 | 141.0 (2) | O3—Mg1—O5—C132 | −113.9 (2) |
C51—P2—C41—C42 | 23.0 (2) | O1—Mg1—O5—C132 | 157.4 (2) |
N—P2—C41—C46 | 70.3 (2) | O2—Mg1—O5—C132 | 103.2 (5) |
C61—P2—C41—C46 | −47.8 (2) | O4—Mg1—O5—C132 | −27.8 (2) |
C51—P2—C41—C46 | −165.84 (19) | O8—Mg1—O5—C132 | 49.2 (2) |
C46—C41—C42—C43 | 0.3 (4) | O5—C132—O6—Mg2 | −7.3 (4) |
P2—C41—C42—C43 | 171.5 (2) | C131—C132—O6—Mg2 | 173.83 (16) |
C41—C42—C43—C44 | −0.7 (4) | O10—Mg2—O6—C132 | 150.6 (2) |
C42—C43—C44—C45 | 0.4 (4) | O7—Mg2—O6—C132 | −119.2 (2) |
C43—C44—C45—C46 | 0.1 (4) | O8—Mg2—O6—C132 | −31.7 (2) |
C44—C45—C46—C41 | −0.5 (4) | O4—Mg2—O6—C132 | 47.8 (2) |
C42—C41—C46—C45 | 0.3 (4) | C143—C142—O7—Mg2 | 11.6 (4) |
P2—C41—C46—C45 | −171.2 (2) | C141—C142—O7—Mg2 | −167.59 (18) |
N—P2—C51—C52 | −13.1 (3) | O10—Mg2—O7—C142 | 161.9 (2) |
C61—P2—C51—C52 | 102.9 (2) | O6—Mg2—O7—C142 | 74.2 (2) |
C41—P2—C51—C52 | −137.1 (2) | O9—Mg2—O7—C142 | −111.3 (2) |
N—P2—C51—C56 | 168.6 (2) | O8—Mg2—O7—C142 | −15.1 (2) |
C61—P2—C51—C56 | −75.4 (3) | O4—Mg2—O7—C142 | −24.2 (5) |
C41—P2—C51—C56 | 44.5 (3) | C143—C144—O8—Mg2 | −8.5 (4) |
C56—C51—C52—C53 | −1.7 (4) | C145—C144—O8—Mg2 | 171.59 (17) |
P2—C51—C52—C53 | 179.9 (2) | C143—C144—O8—Mg1 | −146.9 (2) |
C51—C52—C53—C54 | 0.0 (5) | C145—C144—O8—Mg1 | 33.2 (3) |
C52—C53—C54—C55 | 1.5 (5) | O7—Mg2—O8—C144 | 13.4 (2) |
C53—C54—C55—C56 | −1.2 (5) | O6—Mg2—O8—C144 | −78.5 (2) |
C52—C51—C56—C55 | 2.0 (4) | O9—Mg2—O8—C144 | 102.3 (2) |
P2—C51—C56—C55 | −179.7 (2) | O4—Mg2—O8—C144 | −168.7 (2) |
C54—C55—C56—C51 | −0.6 (5) | O7—Mg2—O8—Mg1 | 161.83 (7) |
N—P2—C61—C62 | 174.6 (2) | O6—Mg2—O8—Mg1 | 69.92 (7) |
C41—P2—C61—C62 | −63.3 (2) | O9—Mg2—O8—Mg1 | −109.24 (7) |
C51—P2—C61—C62 | 54.4 (2) | O4—Mg2—O8—Mg1 | −20.27 (7) |
N—P2—C61—C66 | −0.3 (2) | O5—Mg1—O8—C144 | 71.7 (2) |
C41—P2—C61—C66 | 121.8 (2) | O3—Mg1—O8—C144 | 155.8 (3) |
C51—P2—C61—C66 | −120.5 (2) | O1—Mg1—O8—C144 | −14.3 (2) |
C66—C61—C62—C63 | 0.9 (4) | O2—Mg1—O8—C144 | −99.2 (2) |
P2—C61—C62—C63 | −174.08 (19) | O4—Mg1—O8—C144 | 167.7 (2) |
C61—C62—C63—C64 | −1.0 (4) | O5—Mg1—O8—Mg2 | −75.45 (8) |
C62—C63—C64—C65 | −0.1 (4) | O3—Mg1—O8—Mg2 | 8.7 (3) |
C63—C64—C65—C66 | 1.4 (4) | O1—Mg1—O8—Mg2 | −161.42 (7) |
C64—C65—C66—C61 | −1.5 (4) | O2—Mg1—O8—Mg2 | 113.70 (8) |
C62—C61—C66—C65 | 0.4 (4) | O4—Mg1—O8—Mg2 | 20.56 (7) |
P2—C61—C66—C65 | 175.4 (2) | C153—C152—O9—Mg2 | −10.5 (4) |
O1—C112—C113—C114 | −3.1 (4) | C151—C152—O9—Mg2 | 170.46 (17) |
C111—C112—C113—C114 | 178.1 (2) | O10—Mg2—O9—C152 | 14.6 (2) |
C112—C113—C114—O2 | −3.3 (4) | O7—Mg2—O9—C152 | −75.8 (2) |
C112—C113—C114—C115 | 177.1 (2) | O8—Mg2—O9—C152 | −163.1 (2) |
O3—C122—C123—C124 | −8.8 (5) | O4—Mg2—O9—C152 | 117.3 (2) |
C121—C122—C123—C124 | 171.1 (3) | C153—C154—O10—Mg2 | 9.3 (4) |
C122—C123—C124—O4 | 2.1 (4) | C155—C154—O10—Mg2 | −172.16 (18) |
C122—C123—C124—C125 | −174.7 (3) | O7—Mg2—O10—C154 | 75.1 (2) |
O7—C142—C143—C144 | −0.1 (4) | O6—Mg2—O10—C154 | 166.9 (2) |
C141—C142—C143—C144 | 179.1 (3) | O9—Mg2—O10—C154 | −14.1 (2) |
C142—C143—C144—O8 | −1.3 (4) | O4—Mg2—O10—C154 | −103.5 (2) |
Hydrogen-bond geometry (Å, º) top
D—H···A | D—H | H···A | D···A | D—H···A |
O11—H01···O2 | 0.87 (2) | 1.98 (2) | 2.851 (3) | 172 (3) |
O11—H02···O9 | 0.87 (2) | 2.03 (2) | 2.883 (3) | 169 (3) |
C62—H62···O1i | 0.95 | 2.60 | 3.362 (3) | 138 |
C63—H63···O3i | 0.95 | 2.65 | 3.566 (3) | 163 |
C25—H25···O6ii | 0.95 | 2.64 | 3.428 (3) | 140 |
C54—H54···O11iii | 0.95 | 2.67 | 3.433 (4) | 138 |
Symmetry codes: (i) −x+3/2, y+1/2, −z+1/2; (ii) −x+3/2, y−1/2, −z+1/2; (iii) −x+1, −y+2, −z. |
Experimental details
Crystal data |
Chemical formula | (C36H30NP2)[Mg2(C2H3O2)(C5H7O2)4]·H2O |
Mr | 1060.65 |
Crystal system, space group | Monoclinic, P21/n |
Temperature (K) | 133 |
a, b, c (Å) | 19.945 (2), 14.069 (2), 20.762 (3) |
β (°) | 106.209 (6) |
V (Å3) | 5594.6 (13) |
Z | 4 |
Radiation type | Mo Kα |
µ (mm−1) | 0.16 |
Crystal size (mm) | 0.32 × 0.18 × 0.03 |
|
Data collection |
Diffractometer | Bruker SMART 1000 CCD diffractometer |
Absorption correction | – |
No. of measured, independent and observed [I > 2σ(I)] reflections | 57401, 9872, 5934 |
Rint | 0.087 |
(sin θ/λ)max (Å−1) | 0.595 |
|
Refinement |
R[F2 > 2σ(F2)], wR(F2), S | 0.045, 0.105, 0.92 |
No. of reflections | 9872 |
No. of parameters | 684 |
No. of restraints | 671 |
H-atom treatment | H atoms treated by a mixture of independent and constrained refinement |
Δρmax, Δρmin (e Å−3) | 0.47, −0.30 |
Selected geometric parameters (Å, º) topMg1—O5 | 2.0220 (19) | Mg2—O10 | 2.0243 (19) |
Mg1—O3 | 2.0445 (19) | Mg2—O7 | 2.0320 (18) |
Mg1—O1 | 2.0501 (19) | Mg2—O6 | 2.0588 (19) |
Mg1—O2 | 2.0560 (19) | Mg2—O9 | 2.0692 (19) |
Mg1—O4 | 2.0926 (18) | Mg2—O8 | 2.0904 (18) |
Mg1—O8 | 2.1926 (18) | Mg2—O4 | 2.1069 (18) |
| | | |
O5—Mg1—O3 | 93.44 (8) | O7—Mg2—O8 | 87.49 (7) |
O5—Mg1—O1 | 87.83 (8) | O6—Mg2—O8 | 89.35 (7) |
O3—Mg1—O1 | 88.78 (8) | O9—Mg2—O8 | 96.18 (8) |
O5—Mg1—O2 | 168.66 (8) | O10—Mg2—O4 | 102.78 (7) |
O3—Mg1—O2 | 95.62 (8) | O7—Mg2—O4 | 166.88 (8) |
O1—Mg1—O2 | 85.55 (8) | O6—Mg2—O4 | 90.07 (7) |
O5—Mg1—O4 | 94.69 (7) | O9—Mg2—O4 | 90.11 (7) |
O3—Mg1—O4 | 85.87 (7) | O8—Mg2—O4 | 79.56 (7) |
O1—Mg1—O4 | 174.21 (8) | C112—O1—Mg1 | 130.25 (17) |
O2—Mg1—O4 | 92.77 (7) | C114—O2—Mg1 | 129.52 (17) |
O5—Mg1—O8 | 84.64 (7) | C122—O3—Mg1 | 129.24 (17) |
O3—Mg1—O8 | 163.10 (8) | C124—O4—Mg1 | 126.47 (16) |
O1—Mg1—O8 | 107.88 (7) | C124—O4—Mg2 | 134.34 (16) |
O2—Mg1—O8 | 88.64 (7) | Mg1—O4—Mg2 | 98.97 (7) |
O4—Mg1—O8 | 77.58 (7) | C132—O5—Mg1 | 131.24 (17) |
O10—Mg2—O7 | 90.26 (8) | C132—O6—Mg2 | 129.89 (17) |
O10—Mg2—O6 | 87.71 (8) | C142—O7—Mg2 | 128.14 (17) |
O7—Mg2—O6 | 91.88 (7) | C144—O8—Mg2 | 125.75 (16) |
O10—Mg2—O9 | 86.79 (8) | C144—O8—Mg1 | 128.52 (16) |
O7—Mg2—O9 | 89.21 (7) | Mg2—O8—Mg1 | 96.35 (7) |
O6—Mg2—O9 | 174.40 (8) | C152—O9—Mg2 | 127.05 (18) |
O10—Mg2—O8 | 176.24 (8) | C154—O10—Mg2 | 128.98 (18) |
Hydrogen-bond geometry (Å, º) top
D—H···A | D—H | H···A | D···A | D—H···A |
O11—H01···O2 | 0.87 (2) | 1.98 (2) | 2.851 (3) | 172 (3) |
O11—H02···O9 | 0.87 (2) | 2.03 (2) | 2.883 (3) | 169 (3) |
C62—H62···O1i | 0.95 | 2.60 | 3.362 (3) | 138 |
C63—H63···O3i | 0.95 | 2.65 | 3.566 (3) | 163 |
C25—H25···O6ii | 0.95 | 2.64 | 3.428 (3) | 140 |
C54—H54···O11iii | 0.95 | 2.67 | 3.433 (4) | 138 |
Symmetry codes: (i) −x+3/2, y+1/2, −z+1/2; (ii) −x+3/2, y−1/2, −z+1/2; (iii) −x+1, −y+2, −z. |
The title compound, (I), arose in small quantities as an unexpected crystalline product during the study of gold–acetylide complexes (see Experimental).
The anion (Fig. 1) involves two magnesium centres with distorted octahedral coordination. The acetate ligand bridges the metal centres. Of the four acetylacetonate ligands, two are chelating (one at each Mg); the other two each have one oxygen (O4 and O8) that bridges both Mg centres and one (O2 and O7) that coordinates to only one Mg. The water molecule bridges the acetylacetonate atoms O2 and O9 by hydrogen bonding. The Mg···Mg distance is 3.1925 (12) Å.
The related structures of hexakis(acetylacetonato)trimagnesium(II) and hexakis(ethylacetoacetato)trimagnesium(II) have been described by Weiß et al. (1985) and Petrov et al. (1992).