metal-organic compounds
Poly[tetrakis(dimethylformamide)tris(μ4-terephthalato)trimagnesium]
aDepartment of Chemistry, Youngstown State University, One University Plaza, Youngstown, OH 44555, USA
*Correspondence e-mail: srlovelacecameron@ysu.edu
The title framework compound, [Mg3(C8H4O4)3(C3H7NO)4]n or [Mg3(bdc)3(DMF)4]n, was obtained as a side product of the solvothermal reaction of magnesium nitrate, terephthalic acid (bdcH2), and 1,3-bis(4-pyridyl)propane in a 1:2:1 ratio in dimethylformamide (DMF). The consists of three MgII cations, three terephthalate anions, and four coordinating DMF molecules. One of the four DMF molecules was refined as disordered over two mutually exclusive positions, with an occupancy rate for the major moiety of 0.923 (4). The three MgII cations possess distorted octahedral coordination geometries that form linear Mg trimers. Of the three MgII cations, the central MgII is octahedrally coordinated by six different carboxylate O atoms. The terminal MgII cations are bonded to four O atoms of three bdc linkers and to two O atoms of coordinating DMF molecules. The compound has a two-dimensional 36-network structure parallel to (001) that is formed by connection of the Mg trimers as distorted octahedral nodes to the bdc ligands as linkers.
Related literature
For background information on Mg- and Zn-bdc metal-organic frameworks, see: Mallick et al. (2011); Burrows et al. (2005); Edgar et al. (2001); Grzesiak et al. (2006); Rood et al. (2006); Davies et al. (2007); Williams et al. (2005).
Experimental
Crystal data
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Data collection: APEX2 (Bruker, 2011); cell SAINT (Bruker, 2011); data reduction: SAINT; program(s) used to solve structure: SHELXTL (Sheldrick, 2008); program(s) used to refine structure: SHELXLE (Hübschle et al., 2011) and SHELXL97 (Sheldrick, 2008); molecular graphics: DIAMOND (Brandenburg, 2001); software used to prepare material for publication: publCIF (Westrip, 2010).
Supporting information
https://doi.org/10.1107/S1600536812038949/tk5144sup1.cif
contains datablocks I, global. DOI:Structure factors: contains datablock I. DOI: https://doi.org/10.1107/S1600536812038949/tk5144Isup2.hkl
The compound was synthesized under solvothermal conditions. In a typical synthesis, Mg(NO3)2.6H2O (0.129 g, 1.0 mmol) and terepthalic acid (0.169 g, 2.0 mmol) were dissolved in DMF (5.0 ml). Then, 1,3-bis(4-pyridyl)propane (0.101 g, 1.0 mmol) was added to the reaction mixture and stirred for one hour before transferring the mixture into a glass vial. The final mixture was heated to 373 K for 24 h. The vial was then slowly cooled to room temperature yielding colorless plates of the title compound as a minor product along with an unidentified white powder. Crystals are sensitive towards solvent loss and decompose rapidly once taken out of solution.
Reflections 1 1 0, 0 1 1 and 1 0 2 were partially obstructed by the beam stop and were omitted from the refinement.
One of the DMF molecules was refined as disordered over two mutually exclusive positions. The minor moiety was restrained to have a similar geometry as the major moiety, the overlapping O and N atoms were each constrained to have ADPs identical to that in the major moiety, and the ADPs of the C, N and O atoms of the minor moiety were restrained to be similar to each other. The occupancy ratios for the two moieties refined to 0.923 (4) to 0.077 (4).
Carbon-bound hydrogen atoms were placed in calculated positions with C—H bond distances of 0.95 Å (aromatic H and carbonyl H of DMF) and 0.98 Å (methyl H). Methyl group H atoms were allowed to rotate around the C—C bond to best fit the experimental electron density. Uiso(H) values for all H atoms were constrained to a multiple of Ueq of their respective
(1.2 times for aromatic and carbonyl H atoms, and 1.5 times for methyl H atoms).The construction of metal-organic frameworks (MOFs) with light building blocks has been the subject of intense research during the past few years (Mallick et al., 2011). A suitable metal for construction of lightweight frameworks is magnesium. In the present study, the title compound, [Mg3(bdc)3(DMF)4]n, was obtained during part of our investigations into the solvothermal synthesis of lightweight metal organic frameworks. Reaction of magnesium nitrate with terephthalic acid (bdcH2) and 1,3-bis(4-pyridyl)propane (tmdpyr) at 373 K (100 °C) in dimethyl formamide (DMF) yielded the title compound as a minor product along with an unidentified white powder. The crystals of the title compound are sensitive towards solvent loss and decompose rapidly once taken out of solution.
The
of the title framework consists of three magnesium cations, and three anionic bdc units, and four coordinated DMF molecules, respectively (Fig. 1). One of the four DMF molecules was refined as disordered over two mutually exclusive positions with an occupancy ratio of 0.923 (4) to 0.077 (4).The three magnesium cations in the structure form secondary building units (SBUs) that each possesses a chain of three magnesium ions bridged by six bdc linkers and coordinated by four terminal DMF molecules (Fig. 2). There are two types of magnesium coordination environments in the structure. The terminal ions, Mg1 and Mg3, in the SBU exhibit distorted octahedral geometries. Of the six bonds, four are from O atoms of three different bdc linkers (one bdc linker binds with magnesium in a chelating mode) and the other two are from DMF O atoms. The central ion, Mg2, is also distorted octahedrally coordinated, but it binds to six different carboxylate O atoms (four of them are in bidentate mode and two are in
mode). O—Mg—O angles vary between 60.35 (7) and 178.54 (9)°, with the unusually small angle of 60.35 (7)° being associated with the bdc linker in mode. The three distorted octahedral trimeric magnesiums together act as a node that is connected with other nodes through the bdc linkers to give rise to a two-dimensional layered 36-network (Fig. 3). The layers in the structure are stacked atop of one another, with terminal DMF molecules that are projecting into the inter-lamellar space (Fig. 4). The structure is isoreticular to previously reported magnesium and bdc based framework compounds, Mg3(bdc)3(X)4 [X = DMSO, Rood et al., 2006; DMA, Davies et al., 2007] in which the terminal solvent molecules, DMSO and DMA, project in to the inter-lamellar spaces. Similar layered structures have also been reported with zinc-bdc based frameworks (Edgar et al., 2001; Burrows et al., 2005; Williams et al., 2005; Grzesiak et al., 2006).For background information on Mg- and Zn-bdc metal-organic frameworks, see: Mallick et al. (2011); Burrows et al. (2005); Edgar et al. (2001); Grzesiak et al. (2006); Rood et al. (2006); Davies et al. (2007); Williams et al. (2005).
Data collection: APEX2 (Bruker, 2011); cell
SAINT (Bruker, 2011); data reduction: SAINT (Bruker, 2011); program(s) used to solve structure: SHELXTL (Sheldrick, 2008); program(s) used to refine structure: SHELXLE (Hübschle et al., 2011) and SHELXL97 (Sheldrick, 2008); molecular graphics: DIAMOND (Brandenburg, 2001); software used to prepare material for publication: publCIF (Westrip, 2010).[Mg3(C8H4O4)3(C3H7NO)4] | F(000) = 1792 |
Mr = 857.65 | Dx = 1.396 Mg m−3 |
Monoclinic, P21/c | Mo Kα radiation, λ = 0.71073 Å |
Hall symbol: -P 2ybc | Cell parameters from 4706 reflections |
a = 18.158 (2) Å | θ = 2.3–30.2° |
b = 9.5046 (13) Å | µ = 0.15 mm−1 |
c = 24.066 (3) Å | T = 100 K |
β = 100.825 (2)° | Plate, colourless |
V = 4079.6 (10) Å3 | 0.34 × 0.20 × 0.05 mm |
Z = 4 |
Bruker SMART APEX CCD diffractometer | 10014 independent reflections |
Radiation source: fine-focus sealed tube | 7598 reflections with I > 2σ(I) |
Graphite monochromator | Rint = 0.039 |
ω scans | θmax = 28.3°, θmin = 1.1° |
Absorption correction: multi-scan (SADABS; Bruker, 2011) | h = −16→24 |
Tmin = 0.619, Tmax = 0.746 | k = −12→12 |
21816 measured reflections | l = −32→27 |
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)] = 0.066 | Hydrogen site location: inferred from neighbouring sites |
wR(F2) = 0.149 | H-atom parameters constrained |
S = 1.12 | w = 1/[σ2(Fo2) + (0.045P)2 + 5.8483P] where P = (Fo2 + 2Fc2)/3 |
10014 reflections | (Δ/σ)max < 0.001 |
574 parameters | Δρmax = 0.46 e Å−3 |
33 restraints | Δρmin = −0.35 e Å−3 |
[Mg3(C8H4O4)3(C3H7NO)4] | V = 4079.6 (10) Å3 |
Mr = 857.65 | Z = 4 |
Monoclinic, P21/c | Mo Kα radiation |
a = 18.158 (2) Å | µ = 0.15 mm−1 |
b = 9.5046 (13) Å | T = 100 K |
c = 24.066 (3) Å | 0.34 × 0.20 × 0.05 mm |
β = 100.825 (2)° |
Bruker SMART APEX CCD diffractometer | 10014 independent reflections |
Absorption correction: multi-scan (SADABS; Bruker, 2011) | 7598 reflections with I > 2σ(I) |
Tmin = 0.619, Tmax = 0.746 | Rint = 0.039 |
21816 measured reflections |
R[F2 > 2σ(F2)] = 0.066 | 33 restraints |
wR(F2) = 0.149 | H-atom parameters constrained |
S = 1.12 | Δρmax = 0.46 e Å−3 |
10014 reflections | Δρmin = −0.35 e Å−3 |
574 parameters |
Geometry. All e.s.d.'s (except the e.s.d. in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell e.s.d.'s are taken into account individually in the estimation of e.s.d.'s in distances, angles and torsion angles; correlations between e.s.d.'s in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell e.s.d.'s is used for estimating e.s.d.'s involving l.s. planes. |
Refinement. Refinement 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) | |
Mg1 | 0.20949 (5) | 0.47092 (9) | 0.09756 (4) | 0.00978 (18) | |
Mg2 | 0.25057 (4) | 0.41016 (9) | 0.24603 (4) | 0.00810 (17) | |
Mg3 | 0.28787 (5) | 0.33064 (9) | 0.39299 (4) | 0.00983 (18) | |
O1 | 0.30953 (10) | 0.3705 (2) | 0.11070 (8) | 0.0152 (4) | |
O2 | 0.33782 (10) | 0.3615 (2) | 0.20560 (8) | 0.0146 (4) | |
O3 | 0.67833 (10) | 0.0492 (2) | 0.20601 (8) | 0.0138 (4) | |
O4 | 0.64810 (10) | 0.0028 (2) | 0.11299 (8) | 0.0147 (4) | |
O5 | 0.14333 (10) | 0.3020 (2) | 0.10680 (8) | 0.0138 (4) | |
O6 | 0.17971 (10) | 0.2685 (2) | 0.20005 (8) | 0.0132 (4) | |
O7 | −0.16247 (10) | −0.0372 (2) | 0.21503 (8) | 0.0135 (4) | |
O8 | −0.18736 (9) | −0.0683 (2) | 0.12085 (8) | 0.0134 (4) | |
O9 | 0.26181 (10) | 0.6786 (2) | 0.12084 (8) | 0.0140 (4) | |
O10 | 0.21240 (9) | 0.55376 (19) | 0.18163 (7) | 0.0104 (4) | |
O11 | 0.23514 (10) | 1.1286 (2) | 0.36602 (8) | 0.0135 (4) | |
O12 | 0.28604 (9) | 1.25894 (19) | 0.30769 (7) | 0.0106 (4) | |
O13 | 0.21208 (10) | 0.4826 (2) | 0.01346 (8) | 0.0175 (4) | |
O14 | 0.10924 (10) | 0.5856 (2) | 0.07525 (8) | 0.0169 (4) | |
O16 | 0.28667 (10) | 0.3291 (2) | 0.47647 (8) | 0.0160 (4) | |
N1 | 0.26651 (13) | 0.6147 (3) | −0.04601 (10) | 0.0189 (5) | |
N2 | −0.01117 (12) | 0.6279 (3) | 0.08363 (11) | 0.0204 (5) | |
N4 | 0.24305 (14) | 0.4812 (3) | 0.53454 (11) | 0.0203 (5) | |
C1 | 0.35166 (14) | 0.3411 (3) | 0.15737 (12) | 0.0128 (5) | |
C2 | 0.42644 (14) | 0.2735 (3) | 0.15462 (12) | 0.0143 (5) | |
C3 | 0.44180 (14) | 0.2137 (3) | 0.10546 (12) | 0.0158 (5) | |
H3 | 0.4056 | 0.2187 | 0.0714 | 0.019* | |
C4 | 0.51035 (14) | 0.1461 (3) | 0.10581 (11) | 0.0152 (5) | |
H4 | 0.5203 | 0.1042 | 0.0722 | 0.018* | |
C5 | 0.56423 (14) | 0.1400 (3) | 0.15565 (11) | 0.0135 (5) | |
C6 | 0.54986 (16) | 0.2045 (4) | 0.20400 (13) | 0.0272 (7) | |
H6 | 0.5870 | 0.2041 | 0.2376 | 0.033* | |
C7 | 0.48118 (16) | 0.2702 (4) | 0.20368 (13) | 0.0280 (8) | |
H7 | 0.4716 | 0.3132 | 0.2372 | 0.034* | |
C8 | 0.63647 (13) | 0.0582 (3) | 0.15837 (11) | 0.0116 (5) | |
C9 | 0.13477 (13) | 0.2544 (3) | 0.15446 (11) | 0.0112 (5) | |
C10 | 0.06273 (13) | 0.1758 (3) | 0.15667 (11) | 0.0115 (5) | |
C11 | 0.01302 (14) | 0.1379 (3) | 0.10717 (11) | 0.0141 (5) | |
H11 | 0.0251 | 0.1584 | 0.0713 | 0.017* | |
C12 | −0.05394 (14) | 0.0702 (3) | 0.11033 (11) | 0.0148 (5) | |
H12 | −0.0869 | 0.0430 | 0.0766 | 0.018* | |
C13 | −0.07311 (13) | 0.0421 (3) | 0.16273 (11) | 0.0119 (5) | |
C14 | −0.02315 (15) | 0.0784 (3) | 0.21175 (12) | 0.0196 (6) | |
H14 | −0.0352 | 0.0579 | 0.2476 | 0.024* | |
C15 | 0.04437 (15) | 0.1445 (3) | 0.20874 (11) | 0.0183 (6) | |
H15 | 0.0781 | 0.1684 | 0.2426 | 0.022* | |
C16 | −0.14698 (13) | −0.0274 (3) | 0.16669 (11) | 0.0110 (5) | |
C17 | 0.24114 (13) | 0.6691 (3) | 0.16770 (11) | 0.0108 (5) | |
C18 | 0.24572 (14) | 0.7919 (3) | 0.20711 (11) | 0.0122 (5) | |
C19 | 0.29401 (14) | 0.9041 (3) | 0.20265 (12) | 0.0144 (5) | |
H19 | 0.3251 | 0.9017 | 0.1750 | 0.017* | |
C20 | 0.29669 (14) | 1.0191 (3) | 0.23864 (12) | 0.0140 (5) | |
H20 | 0.3299 | 1.0949 | 0.2359 | 0.017* | |
C21 | 0.25055 (14) | 1.0230 (3) | 0.27868 (11) | 0.0119 (5) | |
C22 | 0.20191 (14) | 0.9115 (3) | 0.28294 (11) | 0.0143 (5) | |
H22 | 0.1704 | 0.9144 | 0.3103 | 0.017* | |
C23 | 0.19968 (15) | 0.7962 (3) | 0.24713 (12) | 0.0146 (5) | |
H23 | 0.1666 | 0.7202 | 0.2500 | 0.018* | |
C24 | 0.25574 (13) | 1.1429 (3) | 0.31948 (11) | 0.0112 (5) | |
C25 | 0.26467 (15) | 0.5073 (3) | −0.01164 (11) | 0.0149 (5) | |
H25 | 0.3062 | 0.4447 | −0.0056 | 0.018* | |
C26 | 0.20341 (19) | 0.7121 (4) | −0.05927 (15) | 0.0313 (8) | |
H26A | 0.2223 | 0.8077 | −0.0625 | 0.047* | |
H26B | 0.1740 | 0.7090 | −0.0291 | 0.047* | |
H26C | 0.1716 | 0.6848 | −0.0952 | 0.047* | |
C27 | 0.32811 (18) | 0.6340 (4) | −0.07655 (13) | 0.0258 (7) | |
H27A | 0.3083 | 0.6350 | −0.1173 | 0.039* | |
H27B | 0.3639 | 0.5565 | −0.0675 | 0.039* | |
H27C | 0.3534 | 0.7234 | −0.0653 | 0.039* | |
C28 | 0.05722 (14) | 0.5785 (3) | 0.10208 (12) | 0.0173 (6) | |
H28 | 0.0672 | 0.5349 | 0.1382 | 0.021* | |
C29 | −0.03021 (19) | 0.6938 (5) | 0.02858 (15) | 0.0386 (9) | |
H29A | −0.0737 | 0.6460 | 0.0061 | 0.058* | |
H29B | 0.0125 | 0.6868 | 0.0092 | 0.058* | |
H29C | −0.0423 | 0.7931 | 0.0332 | 0.058* | |
C30 | −0.07011 (17) | 0.6193 (4) | 0.11684 (15) | 0.0325 (8) | |
H30A | −0.1142 | 0.5730 | 0.0945 | 0.049* | |
H30B | −0.0837 | 0.7143 | 0.1271 | 0.049* | |
H30C | −0.0522 | 0.5648 | 0.1513 | 0.049* | |
O15 | 0.39003 (12) | 0.2178 (3) | 0.41379 (13) | 0.0163 (6) | 0.923 (4) |
C31 | 0.43687 (16) | 0.2254 (4) | 0.38262 (14) | 0.0205 (7) | 0.923 (4) |
H31 | 0.4223 | 0.2736 | 0.3477 | 0.025* | 0.923 (4) |
N3 | 0.50494 (17) | 0.1726 (3) | 0.39358 (14) | 0.0223 (7) | 0.923 (4) |
C32 | 0.55482 (19) | 0.1786 (4) | 0.35236 (17) | 0.0331 (9) | 0.923 (4) |
H32A | 0.6058 | 0.2014 | 0.3718 | 0.050* | 0.923 (4) |
H32B | 0.5371 | 0.2512 | 0.3241 | 0.050* | 0.923 (4) |
H32C | 0.5549 | 0.0871 | 0.3336 | 0.050* | 0.923 (4) |
C33 | 0.5317 (2) | 0.0975 (6) | 0.44580 (19) | 0.0518 (14) | 0.923 (4) |
H33A | 0.5822 | 0.1304 | 0.4624 | 0.078* | 0.923 (4) |
H33B | 0.5332 | −0.0035 | 0.4380 | 0.078* | 0.923 (4) |
H33C | 0.4978 | 0.1149 | 0.4723 | 0.078* | 0.923 (4) |
O15B | 0.3792 (13) | 0.193 (4) | 0.423 (2) | 0.0163 (6) | 0.077 (4) |
C31B | 0.4482 (14) | 0.211 (4) | 0.4268 (15) | 0.021 (4) | 0.077 (4) |
H31B | 0.4709 | 0.2819 | 0.4521 | 0.026* | 0.077 (4) |
N3B | 0.4921 (15) | 0.140 (4) | 0.3991 (18) | 0.0223 (7) | 0.077 (4) |
C32B | 0.461 (2) | 0.052 (5) | 0.3498 (16) | 0.034 (8) | 0.077 (4) |
H32D | 0.4994 | 0.0368 | 0.3268 | 0.051* | 0.077 (4) |
H32E | 0.4178 | 0.1004 | 0.3270 | 0.051* | 0.077 (4) |
H32F | 0.4448 | −0.0384 | 0.3627 | 0.051* | 0.077 (4) |
C33B | 0.5715 (15) | 0.168 (5) | 0.405 (2) | 0.041 (9) | 0.077 (4) |
H33D | 0.5894 | 0.1304 | 0.3717 | 0.061* | 0.077 (4) |
H33E | 0.5988 | 0.1230 | 0.4391 | 0.061* | 0.077 (4) |
H33F | 0.5801 | 0.2698 | 0.4070 | 0.061* | 0.077 (4) |
C34 | 0.23760 (16) | 0.3682 (3) | 0.50274 (12) | 0.0186 (6) | |
H34 | 0.1934 | 0.3128 | 0.4996 | 0.022* | |
C35 | 0.31082 (17) | 0.5676 (4) | 0.54180 (15) | 0.0290 (7) | |
H35A | 0.2977 | 0.6662 | 0.5469 | 0.044* | |
H35B | 0.3338 | 0.5591 | 0.5082 | 0.044* | |
H35C | 0.3464 | 0.5355 | 0.5752 | 0.044* | |
C36 | 0.18345 (18) | 0.5209 (4) | 0.56510 (14) | 0.0275 (7) | |
H36A | 0.1673 | 0.6176 | 0.5551 | 0.041* | |
H36B | 0.2025 | 0.5149 | 0.6059 | 0.041* | |
H36C | 0.1408 | 0.4569 | 0.5547 | 0.041* |
U11 | U22 | U33 | U12 | U13 | U23 | |
Mg1 | 0.0078 (4) | 0.0106 (4) | 0.0116 (4) | 0.0001 (3) | 0.0037 (3) | −0.0002 (3) |
Mg2 | 0.0061 (4) | 0.0082 (4) | 0.0103 (4) | 0.0000 (3) | 0.0024 (3) | −0.0007 (3) |
Mg3 | 0.0090 (4) | 0.0092 (4) | 0.0117 (4) | −0.0002 (3) | 0.0030 (3) | −0.0006 (3) |
O1 | 0.0104 (9) | 0.0187 (10) | 0.0168 (10) | 0.0035 (7) | 0.0032 (7) | −0.0010 (8) |
O2 | 0.0094 (8) | 0.0197 (10) | 0.0163 (10) | 0.0038 (7) | 0.0068 (7) | 0.0006 (8) |
O3 | 0.0107 (8) | 0.0142 (10) | 0.0159 (9) | 0.0041 (7) | 0.0007 (7) | 0.0016 (8) |
O4 | 0.0125 (9) | 0.0167 (10) | 0.0159 (10) | 0.0066 (7) | 0.0056 (7) | 0.0014 (8) |
O5 | 0.0131 (9) | 0.0147 (9) | 0.0142 (9) | −0.0053 (7) | 0.0045 (7) | 0.0003 (8) |
O6 | 0.0109 (8) | 0.0132 (9) | 0.0146 (9) | −0.0035 (7) | −0.0002 (7) | −0.0018 (8) |
O7 | 0.0110 (8) | 0.0176 (10) | 0.0135 (9) | −0.0025 (7) | 0.0067 (7) | 0.0001 (8) |
O8 | 0.0097 (8) | 0.0166 (10) | 0.0140 (9) | −0.0026 (7) | 0.0028 (7) | 0.0007 (8) |
O9 | 0.0168 (9) | 0.0127 (9) | 0.0142 (9) | −0.0011 (7) | 0.0070 (7) | 0.0001 (8) |
O10 | 0.0111 (8) | 0.0078 (8) | 0.0122 (9) | 0.0000 (6) | 0.0017 (7) | 0.0009 (7) |
O11 | 0.0159 (9) | 0.0117 (9) | 0.0147 (9) | −0.0014 (7) | 0.0075 (7) | −0.0018 (7) |
O12 | 0.0101 (8) | 0.0101 (9) | 0.0119 (9) | −0.0008 (6) | 0.0030 (7) | −0.0002 (7) |
O13 | 0.0159 (9) | 0.0250 (11) | 0.0124 (9) | −0.0017 (8) | 0.0049 (7) | −0.0014 (8) |
O14 | 0.0121 (9) | 0.0226 (11) | 0.0166 (10) | 0.0060 (8) | 0.0046 (7) | 0.0033 (8) |
O16 | 0.0190 (9) | 0.0188 (10) | 0.0109 (9) | 0.0029 (8) | 0.0050 (7) | 0.0003 (8) |
N1 | 0.0228 (12) | 0.0161 (12) | 0.0194 (12) | −0.0002 (9) | 0.0078 (10) | 0.0002 (10) |
N2 | 0.0111 (11) | 0.0288 (14) | 0.0217 (13) | 0.0066 (10) | 0.0042 (9) | 0.0019 (11) |
N4 | 0.0222 (12) | 0.0177 (13) | 0.0227 (13) | −0.0023 (9) | 0.0082 (10) | −0.0024 (10) |
C1 | 0.0094 (11) | 0.0113 (12) | 0.0185 (13) | −0.0007 (9) | 0.0046 (10) | −0.0002 (10) |
C2 | 0.0113 (12) | 0.0156 (13) | 0.0170 (13) | 0.0032 (10) | 0.0047 (10) | −0.0005 (11) |
C3 | 0.0119 (12) | 0.0212 (14) | 0.0140 (13) | 0.0043 (10) | 0.0013 (10) | −0.0003 (11) |
C4 | 0.0130 (12) | 0.0201 (14) | 0.0126 (13) | 0.0070 (10) | 0.0030 (10) | −0.0021 (11) |
C5 | 0.0093 (11) | 0.0155 (13) | 0.0168 (13) | 0.0025 (9) | 0.0053 (10) | 0.0010 (11) |
C6 | 0.0144 (14) | 0.048 (2) | 0.0176 (15) | 0.0133 (13) | −0.0013 (11) | −0.0077 (14) |
C7 | 0.0175 (14) | 0.051 (2) | 0.0165 (14) | 0.0158 (14) | 0.0042 (11) | −0.0103 (14) |
C8 | 0.0089 (11) | 0.0093 (12) | 0.0176 (13) | 0.0001 (9) | 0.0051 (9) | 0.0026 (10) |
C9 | 0.0080 (11) | 0.0121 (12) | 0.0142 (12) | −0.0002 (9) | 0.0041 (9) | −0.0006 (10) |
C10 | 0.0077 (11) | 0.0134 (13) | 0.0139 (13) | −0.0015 (9) | 0.0033 (9) | 0.0016 (10) |
C11 | 0.0111 (12) | 0.0203 (14) | 0.0120 (12) | −0.0021 (10) | 0.0051 (9) | 0.0023 (11) |
C12 | 0.0111 (12) | 0.0194 (14) | 0.0135 (13) | −0.0034 (10) | 0.0013 (9) | 0.0004 (11) |
C13 | 0.0087 (11) | 0.0157 (13) | 0.0126 (12) | −0.0026 (9) | 0.0054 (9) | 0.0009 (10) |
C14 | 0.0155 (13) | 0.0323 (17) | 0.0123 (13) | −0.0078 (12) | 0.0055 (10) | 0.0005 (12) |
C15 | 0.0150 (13) | 0.0284 (16) | 0.0111 (13) | −0.0089 (11) | 0.0014 (10) | −0.0006 (12) |
C16 | 0.0095 (11) | 0.0084 (12) | 0.0159 (13) | 0.0002 (9) | 0.0048 (9) | 0.0018 (10) |
C17 | 0.0093 (11) | 0.0093 (12) | 0.0136 (12) | 0.0022 (9) | 0.0015 (9) | −0.0005 (10) |
C18 | 0.0133 (12) | 0.0084 (12) | 0.0140 (13) | 0.0005 (9) | 0.0005 (10) | 0.0008 (10) |
C19 | 0.0144 (12) | 0.0128 (13) | 0.0177 (13) | −0.0016 (10) | 0.0072 (10) | −0.0023 (11) |
C20 | 0.0163 (12) | 0.0079 (12) | 0.0187 (13) | −0.0018 (9) | 0.0055 (10) | 0.0013 (10) |
C21 | 0.0113 (11) | 0.0096 (12) | 0.0147 (13) | 0.0022 (9) | 0.0020 (9) | −0.0011 (10) |
C22 | 0.0169 (12) | 0.0110 (12) | 0.0162 (13) | −0.0004 (10) | 0.0067 (10) | −0.0005 (10) |
C23 | 0.0164 (13) | 0.0101 (12) | 0.0186 (14) | −0.0026 (10) | 0.0064 (10) | −0.0010 (10) |
C24 | 0.0106 (11) | 0.0100 (12) | 0.0130 (12) | 0.0007 (9) | 0.0022 (9) | −0.0003 (10) |
C25 | 0.0154 (12) | 0.0154 (13) | 0.0139 (13) | 0.0003 (10) | 0.0031 (10) | −0.0018 (10) |
C26 | 0.0373 (19) | 0.0222 (17) | 0.0322 (18) | 0.0086 (14) | 0.0009 (14) | 0.0043 (14) |
C27 | 0.0329 (17) | 0.0253 (17) | 0.0223 (16) | −0.0101 (13) | 0.0130 (13) | 0.0015 (13) |
C28 | 0.0141 (12) | 0.0189 (14) | 0.0190 (14) | 0.0029 (10) | 0.0032 (10) | 0.0011 (11) |
C29 | 0.0261 (17) | 0.059 (3) | 0.0301 (19) | 0.0200 (17) | 0.0031 (14) | 0.0126 (18) |
C30 | 0.0196 (15) | 0.045 (2) | 0.038 (2) | 0.0080 (14) | 0.0167 (14) | 0.0013 (17) |
O15 | 0.0123 (11) | 0.0183 (14) | 0.0193 (15) | 0.0039 (9) | 0.0054 (9) | 0.0026 (9) |
C31 | 0.0144 (14) | 0.0218 (17) | 0.0253 (17) | 0.0065 (12) | 0.0036 (12) | 0.0014 (14) |
N3 | 0.0122 (13) | 0.0260 (18) | 0.0293 (16) | 0.0041 (11) | 0.0056 (11) | 0.0071 (14) |
C32 | 0.0197 (17) | 0.039 (2) | 0.043 (2) | 0.0097 (15) | 0.0128 (16) | 0.0039 (18) |
C33 | 0.030 (2) | 0.079 (4) | 0.046 (3) | 0.025 (2) | 0.0068 (18) | 0.030 (3) |
O15B | 0.0123 (11) | 0.0183 (14) | 0.0193 (15) | 0.0039 (9) | 0.0054 (9) | 0.0026 (9) |
C31B | 0.015 (7) | 0.024 (7) | 0.026 (7) | 0.007 (7) | 0.005 (7) | 0.006 (7) |
N3B | 0.0122 (13) | 0.0260 (18) | 0.0293 (16) | 0.0041 (11) | 0.0056 (11) | 0.0071 (14) |
C32B | 0.021 (14) | 0.037 (16) | 0.049 (16) | −0.008 (13) | 0.019 (13) | 0.006 (15) |
C33B | 0.015 (14) | 0.052 (17) | 0.057 (17) | 0.004 (14) | 0.011 (14) | −0.013 (16) |
C34 | 0.0201 (14) | 0.0173 (14) | 0.0188 (14) | −0.0015 (11) | 0.0045 (11) | 0.0010 (12) |
C35 | 0.0259 (16) | 0.0258 (17) | 0.0372 (19) | −0.0053 (13) | 0.0105 (14) | −0.0102 (15) |
C36 | 0.0290 (17) | 0.0271 (17) | 0.0295 (17) | −0.0036 (13) | 0.0138 (13) | −0.0079 (14) |
Mg1—O1 | 2.024 (2) | C10—C15 | 1.388 (4) |
Mg1—O13 | 2.036 (2) | C10—C11 | 1.400 (4) |
Mg1—O5 | 2.042 (2) | C11—C12 | 1.390 (4) |
Mg1—O14 | 2.103 (2) | C11—H11 | 0.9500 |
Mg1—O10 | 2.162 (2) | C12—C13 | 1.396 (4) |
Mg1—O9 | 2.217 (2) | C12—H12 | 0.9500 |
Mg1—C17 | 2.522 (3) | C13—C14 | 1.390 (4) |
Mg1—Mg2 | 3.5575 (13) | C13—C16 | 1.514 (3) |
Mg2—O6 | 2.0393 (19) | C14—C15 | 1.392 (4) |
Mg2—O3i | 2.046 (2) | C14—H14 | 0.9500 |
Mg2—O2 | 2.0614 (19) | C15—H15 | 0.9500 |
Mg2—O7ii | 2.0619 (19) | C17—C18 | 1.497 (4) |
Mg2—O12iii | 2.079 (2) | C18—C23 | 1.390 (4) |
Mg2—O10 | 2.0837 (19) | C18—C19 | 1.397 (4) |
Mg2—Mg3 | 3.5550 (13) | C19—C20 | 1.390 (4) |
Mg3—O16 | 2.013 (2) | C19—H19 | 0.9500 |
Mg3—O4i | 2.028 (2) | C20—C21 | 1.391 (4) |
Mg3—O8ii | 2.0338 (19) | C20—H20 | 0.9500 |
Mg3—O15 | 2.120 (2) | C21—C22 | 1.396 (4) |
Mg3—O15B | 2.127 (18) | C21—C24 | 1.496 (4) |
Mg3—O12iii | 2.157 (2) | C22—C23 | 1.390 (4) |
Mg3—O11iii | 2.189 (2) | C22—H22 | 0.9500 |
Mg3—C24iii | 2.503 (3) | C23—H23 | 0.9500 |
O1—C1 | 1.266 (3) | C24—Mg3vi | 2.503 (3) |
O2—C1 | 1.248 (3) | C25—H25 | 0.9500 |
O3—C8 | 1.254 (3) | C26—H26A | 0.9800 |
O3—Mg2iv | 2.0456 (19) | C26—H26B | 0.9800 |
O4—C8 | 1.265 (3) | C26—H26C | 0.9800 |
O4—Mg3iv | 2.028 (2) | C27—H27A | 0.9800 |
O5—C9 | 1.270 (3) | C27—H27B | 0.9800 |
O6—C9 | 1.246 (3) | C27—H27C | 0.9800 |
O7—C16 | 1.251 (3) | C28—H28 | 0.9500 |
O7—Mg2v | 2.0618 (19) | C29—H29A | 0.9800 |
O8—C16 | 1.266 (3) | C29—H29B | 0.9800 |
O8—Mg3v | 2.0338 (19) | C29—H29C | 0.9800 |
O9—C17 | 1.257 (3) | C30—H30A | 0.9800 |
O10—C17 | 1.285 (3) | C30—H30B | 0.9800 |
O11—C24 | 1.253 (3) | C30—H30C | 0.9800 |
O11—Mg3vi | 2.189 (2) | O15—C31 | 1.237 (4) |
O12—C24 | 1.288 (3) | C31—N3 | 1.314 (4) |
O12—Mg2vi | 2.079 (2) | C31—H31 | 0.9500 |
O12—Mg3vi | 2.157 (2) | N3—C33 | 1.448 (5) |
O13—C25 | 1.244 (3) | N3—C32 | 1.465 (4) |
O14—C28 | 1.242 (3) | C32—H32A | 0.9800 |
O16—C34 | 1.242 (3) | C32—H32B | 0.9800 |
N1—C25 | 1.318 (4) | C32—H32C | 0.9800 |
N1—C26 | 1.461 (4) | C33—H33A | 0.9800 |
N1—C27 | 1.461 (4) | C33—H33B | 0.9800 |
N2—C28 | 1.324 (3) | C33—H33C | 0.9800 |
N2—C29 | 1.447 (4) | O15B—C31B | 1.250 (19) |
N2—C30 | 1.453 (4) | C31B—N3B | 1.318 (18) |
N4—C34 | 1.312 (4) | C31B—H31B | 0.9500 |
N4—C35 | 1.463 (4) | N3B—C33B | 1.448 (18) |
N4—C36 | 1.468 (4) | N3B—C32B | 1.473 (19) |
C1—C2 | 1.515 (3) | C32B—H32D | 0.9800 |
C2—C3 | 1.388 (4) | C32B—H32E | 0.9800 |
C2—C7 | 1.394 (4) | C32B—H32F | 0.9800 |
C3—C4 | 1.399 (4) | C33B—H33D | 0.9800 |
C3—H3 | 0.9500 | C33B—H33E | 0.9800 |
C4—C5 | 1.399 (4) | C33B—H33F | 0.9800 |
C4—H4 | 0.9500 | C34—H34 | 0.9500 |
C5—C6 | 1.383 (4) | C35—H35A | 0.9800 |
C5—C8 | 1.516 (3) | C35—H35B | 0.9800 |
C6—C7 | 1.393 (4) | C35—H35C | 0.9800 |
C6—H6 | 0.9500 | C36—H36A | 0.9800 |
C7—H7 | 0.9500 | C36—H36B | 0.9800 |
C9—C10 | 1.516 (3) | C36—H36C | 0.9800 |
O1—Mg1—O13 | 89.62 (8) | C5—C6—C7 | 120.3 (3) |
O1—Mg1—O5 | 98.14 (9) | C5—C6—H6 | 119.9 |
O13—Mg1—O5 | 105.97 (9) | C7—C6—H6 | 119.9 |
O1—Mg1—O14 | 173.16 (9) | C6—C7—C2 | 120.7 (3) |
O13—Mg1—O14 | 84.17 (8) | C6—C7—H7 | 119.7 |
O5—Mg1—O14 | 86.35 (8) | C2—C7—H7 | 119.7 |
O1—Mg1—O10 | 99.32 (8) | O3—C8—O4 | 126.1 (2) |
O13—Mg1—O10 | 155.37 (9) | O3—C8—C5 | 116.5 (2) |
O5—Mg1—O10 | 95.50 (8) | O4—C8—C5 | 117.4 (2) |
O14—Mg1—O10 | 85.30 (8) | O6—C9—O5 | 125.9 (2) |
O1—Mg1—O9 | 92.91 (8) | O6—C9—C10 | 116.7 (2) |
O13—Mg1—O9 | 96.53 (8) | O5—C9—C10 | 117.4 (2) |
O5—Mg1—O9 | 154.90 (8) | C15—C10—C11 | 119.2 (2) |
O14—Mg1—O9 | 84.98 (8) | C15—C10—C9 | 119.5 (2) |
O10—Mg1—O9 | 60.35 (7) | C11—C10—C9 | 121.3 (2) |
O1—Mg1—C17 | 99.35 (8) | C12—C11—C10 | 120.2 (2) |
O13—Mg1—C17 | 125.41 (9) | C12—C11—H11 | 119.9 |
O5—Mg1—C17 | 125.37 (9) | C10—C11—H11 | 119.9 |
O14—Mg1—C17 | 82.04 (8) | C11—C12—C13 | 120.5 (2) |
O10—Mg1—C17 | 30.63 (7) | C11—C12—H12 | 119.8 |
O9—Mg1—C17 | 29.88 (8) | C13—C12—H12 | 119.8 |
O1—Mg1—Mg2 | 75.75 (6) | C14—C13—C12 | 119.0 (2) |
O13—Mg1—Mg2 | 165.35 (7) | C14—C13—C16 | 120.0 (2) |
O5—Mg1—Mg2 | 77.27 (6) | C12—C13—C16 | 121.0 (2) |
O14—Mg1—Mg2 | 110.41 (6) | C13—C14—C15 | 120.6 (3) |
O10—Mg1—Mg2 | 32.40 (5) | C13—C14—H14 | 119.7 |
O9—Mg1—Mg2 | 83.78 (6) | C15—C14—H14 | 119.7 |
C17—Mg1—Mg2 | 58.04 (6) | C10—C15—C14 | 120.5 (2) |
O6—Mg2—O3i | 178.51 (9) | C10—C15—H15 | 119.8 |
O6—Mg2—O2 | 93.34 (8) | C14—C15—H15 | 119.8 |
O3i—Mg2—O2 | 87.23 (8) | O7—C16—O8 | 126.4 (2) |
O6—Mg2—O7ii | 86.70 (8) | O7—C16—C13 | 116.6 (2) |
O3i—Mg2—O7ii | 92.76 (8) | O8—C16—C13 | 117.0 (2) |
O2—Mg2—O7ii | 178.54 (9) | O9—C17—O10 | 120.0 (2) |
O6—Mg2—O12iii | 90.58 (8) | O9—C17—C18 | 121.5 (2) |
O3i—Mg2—O12iii | 88.04 (8) | O10—C17—C18 | 118.5 (2) |
O2—Mg2—O12iii | 91.11 (8) | O9—C17—Mg1 | 61.46 (14) |
O7ii—Mg2—O12iii | 90.35 (8) | O10—C17—Mg1 | 59.02 (13) |
O6—Mg2—O10 | 86.62 (8) | C18—C17—Mg1 | 170.10 (17) |
O3i—Mg2—O10 | 94.77 (8) | C23—C18—C19 | 119.9 (2) |
O2—Mg2—O10 | 88.49 (8) | C23—C18—C17 | 119.5 (2) |
O7ii—Mg2—O10 | 90.06 (8) | C19—C18—C17 | 120.5 (2) |
O12iii—Mg2—O10 | 177.14 (8) | C20—C19—C18 | 120.1 (2) |
O6—Mg2—Mg3 | 112.48 (6) | C20—C19—H19 | 120.0 |
O3i—Mg2—Mg3 | 66.04 (6) | C18—C19—H19 | 120.0 |
O2—Mg2—Mg3 | 113.72 (6) | C19—C20—C21 | 119.8 (2) |
O7ii—Mg2—Mg3 | 67.58 (6) | C19—C20—H20 | 120.1 |
O12iii—Mg2—Mg3 | 33.64 (5) | C21—C20—H20 | 120.1 |
O10—Mg2—Mg3 | 148.63 (6) | C20—C21—C22 | 120.2 (2) |
O6—Mg2—Mg1 | 64.55 (6) | C20—C21—C24 | 120.2 (2) |
O3i—Mg2—Mg1 | 116.93 (6) | C22—C21—C24 | 119.5 (2) |
O2—Mg2—Mg1 | 66.24 (6) | C23—C22—C21 | 119.9 (2) |
O7ii—Mg2—Mg1 | 112.51 (6) | C23—C22—H22 | 120.1 |
O12iii—Mg2—Mg1 | 143.84 (6) | C21—C22—H22 | 120.1 |
O10—Mg2—Mg1 | 33.79 (5) | C18—C23—C22 | 120.1 (2) |
Mg3—Mg2—Mg1 | 176.90 (3) | C18—C23—H23 | 120.0 |
O16—Mg3—O4i | 100.97 (9) | C22—C23—H23 | 120.0 |
O16—Mg3—O8ii | 89.38 (8) | O11—C24—O12 | 120.1 (2) |
O4i—Mg3—O8ii | 96.67 (9) | O11—C24—C21 | 120.8 (2) |
O16—Mg3—O15 | 86.20 (10) | O12—C24—C21 | 119.0 (2) |
O4i—Mg3—O15 | 86.40 (10) | O11—C24—Mg3vi | 60.98 (14) |
O8ii—Mg3—O15 | 175.03 (10) | O12—C24—Mg3vi | 59.53 (13) |
O16—Mg3—O15B | 79.4 (12) | C21—C24—Mg3vi | 169.95 (18) |
O4i—Mg3—O15B | 95.7 (10) | O13—C25—N1 | 124.3 (3) |
O8ii—Mg3—O15B | 164.7 (9) | O13—C25—H25 | 117.9 |
O15—Mg3—O15B | 10.6 (9) | N1—C25—H25 | 117.9 |
O16—Mg3—O12iii | 161.12 (9) | N1—C26—H26A | 109.5 |
O4i—Mg3—O12iii | 95.39 (8) | N1—C26—H26B | 109.5 |
O8ii—Mg3—O12iii | 98.07 (8) | H26A—C26—H26B | 109.5 |
O15—Mg3—O12iii | 85.49 (11) | N1—C26—H26C | 109.5 |
O15B—Mg3—O12iii | 89.8 (13) | H26A—C26—H26C | 109.5 |
O16—Mg3—O11iii | 101.73 (8) | H26B—C26—H26C | 109.5 |
O4i—Mg3—O11iii | 155.71 (9) | N1—C27—H27A | 109.5 |
O8ii—Mg3—O11iii | 92.10 (8) | N1—C27—H27B | 109.5 |
O15—Mg3—O11iii | 86.60 (10) | H27A—C27—H27B | 109.5 |
O15B—Mg3—O11iii | 80.2 (12) | N1—C27—H27C | 109.5 |
O12iii—Mg3—O11iii | 60.87 (7) | H27A—C27—H27C | 109.5 |
O16—Mg3—C24iii | 130.95 (9) | H27B—C27—H27C | 109.5 |
O4i—Mg3—C24iii | 125.85 (9) | O14—C28—N2 | 124.3 (3) |
O8ii—Mg3—C24iii | 97.93 (8) | O14—C28—H28 | 117.8 |
O15—Mg3—C24iii | 83.32 (11) | N2—C28—H28 | 117.8 |
O15B—Mg3—C24iii | 82.0 (14) | N2—C29—H29A | 109.5 |
O12iii—Mg3—C24iii | 30.96 (8) | N2—C29—H29B | 109.5 |
O11iii—Mg3—C24iii | 30.04 (8) | H29A—C29—H29B | 109.5 |
O16—Mg3—Mg2 | 163.43 (7) | N2—C29—H29C | 109.5 |
O4i—Mg3—Mg2 | 76.26 (6) | H29A—C29—H29C | 109.5 |
O8ii—Mg3—Mg2 | 74.89 (6) | H29B—C29—H29C | 109.5 |
O15—Mg3—Mg2 | 109.72 (9) | N2—C30—H30A | 109.5 |
O15B—Mg3—Mg2 | 117.1 (12) | N2—C30—H30B | 109.5 |
O12iii—Mg3—Mg2 | 32.27 (5) | H30A—C30—H30B | 109.5 |
O11iii—Mg3—Mg2 | 84.30 (6) | N2—C30—H30C | 109.5 |
C24iii—Mg3—Mg2 | 58.19 (6) | H30A—C30—H30C | 109.5 |
C1—O1—Mg1 | 128.18 (18) | H30B—C30—H30C | 109.5 |
C1—O2—Mg2 | 141.34 (17) | C31—O15—Mg3 | 119.9 (2) |
C8—O3—Mg2iv | 140.36 (18) | O15—C31—N3 | 125.7 (3) |
C8—O4—Mg3iv | 126.01 (17) | O15—C31—H31 | 117.1 |
C9—O5—Mg1 | 123.60 (17) | N3—C31—H31 | 117.1 |
C9—O6—Mg2 | 142.32 (18) | C31—N3—C33 | 120.8 (3) |
C16—O7—Mg2v | 140.37 (17) | C31—N3—C32 | 121.8 (3) |
C16—O8—Mg3v | 130.02 (17) | C33—N3—C32 | 117.2 (3) |
C17—O9—Mg1 | 88.66 (15) | C31B—O15B—Mg3 | 130 (3) |
C17—O10—Mg2 | 131.15 (16) | O15B—C31B—N3B | 126 (3) |
C17—O10—Mg1 | 90.35 (15) | O15B—C31B—H31B | 117.2 |
Mg2—O10—Mg1 | 113.81 (9) | N3B—C31B—H31B | 117.2 |
C24—O11—Mg3vi | 88.98 (15) | C31B—N3B—C33B | 123 (2) |
C24—O12—Mg2vi | 131.40 (16) | C31B—N3B—C32B | 121 (2) |
C24—O12—Mg3vi | 89.52 (15) | C33B—N3B—C32B | 114 (2) |
Mg2vi—O12—Mg3vi | 114.08 (9) | N3B—C32B—H32D | 109.5 |
C25—O13—Mg1 | 130.98 (18) | N3B—C32B—H32E | 109.5 |
C28—O14—Mg1 | 123.08 (18) | H32D—C32B—H32E | 109.5 |
C34—O16—Mg3 | 130.47 (19) | N3B—C32B—H32F | 109.5 |
C25—N1—C26 | 121.1 (3) | H32D—C32B—H32F | 109.5 |
C25—N1—C27 | 121.7 (3) | H32E—C32B—H32F | 109.5 |
C26—N1—C27 | 117.0 (3) | N3B—C33B—H33D | 109.5 |
C28—N2—C29 | 120.5 (3) | N3B—C33B—H33E | 109.5 |
C28—N2—C30 | 122.5 (3) | H33D—C33B—H33E | 109.5 |
C29—N2—C30 | 117.0 (2) | N3B—C33B—H33F | 109.5 |
C34—N4—C35 | 120.0 (3) | H33D—C33B—H33F | 109.5 |
C34—N4—C36 | 121.4 (3) | H33E—C33B—H33F | 109.5 |
C35—N4—C36 | 118.6 (3) | O16—C34—N4 | 124.0 (3) |
O2—C1—O1 | 126.7 (2) | O16—C34—H34 | 118.0 |
O2—C1—C2 | 116.5 (2) | N4—C34—H34 | 118.0 |
O1—C1—C2 | 116.9 (2) | N4—C35—H35A | 109.5 |
C3—C2—C7 | 119.2 (2) | N4—C35—H35B | 109.5 |
C3—C2—C1 | 122.4 (2) | H35A—C35—H35B | 109.5 |
C7—C2—C1 | 118.4 (2) | N4—C35—H35C | 109.5 |
C2—C3—C4 | 120.3 (2) | H35A—C35—H35C | 109.5 |
C2—C3—H3 | 119.9 | H35B—C35—H35C | 109.5 |
C4—C3—H3 | 119.9 | N4—C36—H36A | 109.5 |
C5—C4—C3 | 120.1 (2) | N4—C36—H36B | 109.5 |
C5—C4—H4 | 119.9 | H36A—C36—H36B | 109.5 |
C3—C4—H4 | 119.9 | N4—C36—H36C | 109.5 |
C6—C5—C4 | 119.4 (2) | H36A—C36—H36C | 109.5 |
C6—C5—C8 | 119.3 (2) | H36B—C36—H36C | 109.5 |
C4—C5—C8 | 121.2 (2) | ||
O1—Mg1—Mg2—O6 | −98.15 (9) | O9—Mg1—O13—C25 | 53.0 (3) |
O13—Mg1—Mg2—O6 | −100.7 (3) | C17—Mg1—O13—C25 | 61.3 (3) |
O5—Mg1—Mg2—O6 | 3.81 (8) | Mg2—Mg1—O13—C25 | −37.4 (5) |
O14—Mg1—Mg2—O6 | 84.97 (9) | O13—Mg1—O14—C28 | 152.1 (2) |
O10—Mg1—Mg2—O6 | 126.44 (11) | O5—Mg1—O14—C28 | 45.6 (2) |
O9—Mg1—Mg2—O6 | 167.24 (8) | O10—Mg1—O14—C28 | −50.2 (2) |
C17—Mg1—Mg2—O6 | 150.99 (9) | O9—Mg1—O14—C28 | −110.8 (2) |
O1—Mg1—Mg2—O3i | 81.68 (9) | C17—Mg1—O14—C28 | −80.8 (2) |
O13—Mg1—Mg2—O3i | 79.1 (3) | Mg2—Mg1—O14—C28 | −29.3 (2) |
O5—Mg1—Mg2—O3i | −176.36 (9) | O4i—Mg3—O16—C34 | 101.4 (3) |
O14—Mg1—Mg2—O3i | −95.20 (9) | O8ii—Mg3—O16—C34 | 4.7 (3) |
O10—Mg1—Mg2—O3i | −53.73 (11) | O15—Mg3—O16—C34 | −173.0 (3) |
O9—Mg1—Mg2—O3i | −12.93 (9) | O15B—Mg3—O16—C34 | −164.8 (11) |
C17—Mg1—Mg2—O3i | −29.18 (9) | O12iii—Mg3—O16—C34 | −109.0 (3) |
O1—Mg1—Mg2—O2 | 8.12 (9) | O11iii—Mg3—O16—C34 | −87.3 (3) |
O13—Mg1—Mg2—O2 | 5.5 (3) | C24iii—Mg3—O16—C34 | −95.3 (3) |
O5—Mg1—Mg2—O2 | 110.07 (9) | Mg2—Mg3—O16—C34 | 22.7 (4) |
O14—Mg1—Mg2—O2 | −168.77 (9) | Mg2—O2—C1—O1 | 13.8 (5) |
O10—Mg1—Mg2—O2 | −127.30 (11) | Mg2—O2—C1—C2 | −165.9 (2) |
O9—Mg1—Mg2—O2 | −86.50 (8) | Mg1—O1—C1—O2 | 4.3 (4) |
C17—Mg1—Mg2—O2 | −102.74 (9) | Mg1—O1—C1—C2 | −175.96 (17) |
O1—Mg1—Mg2—O7ii | −172.71 (9) | O2—C1—C2—C3 | 163.9 (3) |
O13—Mg1—Mg2—O7ii | −175.3 (3) | O1—C1—C2—C3 | −15.9 (4) |
O5—Mg1—Mg2—O7ii | −70.76 (9) | O2—C1—C2—C7 | −15.3 (4) |
O14—Mg1—Mg2—O7ii | 10.41 (10) | O1—C1—C2—C7 | 164.9 (3) |
O10—Mg1—Mg2—O7ii | 51.87 (11) | C7—C2—C3—C4 | 2.5 (4) |
O9—Mg1—Mg2—O7ii | 92.68 (8) | C1—C2—C3—C4 | −176.7 (3) |
C17—Mg1—Mg2—O7ii | 76.43 (9) | C2—C3—C4—C5 | −0.8 (4) |
O1—Mg1—Mg2—O12iii | −47.37 (12) | C3—C4—C5—C6 | −1.7 (4) |
O13—Mg1—Mg2—O12iii | −50.0 (3) | C3—C4—C5—C8 | 175.4 (3) |
O5—Mg1—Mg2—O12iii | 54.58 (11) | C4—C5—C6—C7 | 2.5 (5) |
O14—Mg1—Mg2—O12iii | 135.75 (11) | C8—C5—C6—C7 | −174.6 (3) |
O10—Mg1—Mg2—O12iii | 177.21 (14) | C5—C6—C7—C2 | −0.8 (6) |
O9—Mg1—Mg2—O12iii | −141.99 (11) | C3—C2—C7—C6 | −1.7 (5) |
C17—Mg1—Mg2—O12iii | −158.23 (12) | C1—C2—C7—C6 | 177.5 (3) |
O1—Mg1—Mg2—O10 | 135.42 (11) | Mg2iv—O3—C8—O4 | −34.2 (4) |
O13—Mg1—Mg2—O10 | 132.8 (3) | Mg2iv—O3—C8—C5 | 144.0 (2) |
O5—Mg1—Mg2—O10 | −122.63 (11) | Mg3iv—O4—C8—O3 | 24.5 (4) |
O14—Mg1—Mg2—O10 | −41.47 (11) | Mg3iv—O4—C8—C5 | −153.63 (18) |
O9—Mg1—Mg2—O10 | 40.80 (10) | C6—C5—C8—O3 | 2.9 (4) |
C17—Mg1—Mg2—O10 | 24.56 (11) | C4—C5—C8—O3 | −174.2 (3) |
O6—Mg2—Mg3—O16 | −100.1 (2) | C6—C5—C8—O4 | −178.8 (3) |
O3i—Mg2—Mg3—O16 | 80.0 (2) | C4—C5—C8—O4 | 4.1 (4) |
O2—Mg2—Mg3—O16 | 155.4 (2) | Mg2—O6—C9—O5 | 39.7 (5) |
O7ii—Mg2—Mg3—O16 | −23.9 (2) | Mg2—O6—C9—C10 | −138.9 (2) |
O12iii—Mg2—Mg3—O16 | −153.1 (3) | Mg1—O5—C9—O6 | −24.4 (4) |
O10—Mg2—Mg3—O16 | 23.7 (3) | Mg1—O5—C9—C10 | 154.17 (18) |
O6—Mg2—Mg3—O4i | 177.61 (9) | O6—C9—C10—C15 | 10.5 (4) |
O3i—Mg2—Mg3—O4i | −2.25 (8) | O5—C9—C10—C15 | −168.1 (3) |
O2—Mg2—Mg3—O4i | 73.09 (9) | O6—C9—C10—C11 | −171.5 (2) |
O7ii—Mg2—Mg3—O4i | −106.16 (9) | O5—C9—C10—C11 | 9.8 (4) |
O12iii—Mg2—Mg3—O4i | 124.63 (11) | C15—C10—C11—C12 | 0.2 (4) |
O10—Mg2—Mg3—O4i | −58.60 (13) | C9—C10—C11—C12 | −177.7 (3) |
O6—Mg2—Mg3—O8ii | −81.45 (9) | C10—C11—C12—C13 | 1.4 (4) |
O3i—Mg2—Mg3—O8ii | 98.69 (9) | C11—C12—C13—C14 | −2.1 (4) |
O2—Mg2—Mg3—O8ii | 174.04 (9) | C11—C12—C13—C16 | 178.1 (3) |
O7ii—Mg2—Mg3—O8ii | −5.22 (8) | C12—C13—C14—C15 | 1.3 (5) |
O12iii—Mg2—Mg3—O8ii | −134.43 (11) | C16—C13—C14—C15 | −178.9 (3) |
O10—Mg2—Mg3—O8ii | 42.34 (13) | C11—C10—C15—C14 | −1.0 (4) |
O6—Mg2—Mg3—O15 | 96.60 (11) | C9—C10—C15—C14 | 177.0 (3) |
O3i—Mg2—Mg3—O15 | −83.26 (11) | C13—C14—C15—C10 | 0.3 (5) |
O2—Mg2—Mg3—O15 | −7.92 (12) | Mg2v—O7—C16—O8 | −9.1 (5) |
O7ii—Mg2—Mg3—O15 | 172.82 (11) | Mg2v—O7—C16—C13 | 170.08 (19) |
O12iii—Mg2—Mg3—O15 | 43.62 (12) | Mg3v—O8—C16—O7 | −2.5 (4) |
O10—Mg2—Mg3—O15 | −139.61 (14) | Mg3v—O8—C16—C13 | 178.32 (17) |
O6—Mg2—Mg3—O15B | 88.2 (12) | C14—C13—C16—O7 | 6.4 (4) |
O3i—Mg2—Mg3—O15B | −91.7 (12) | C12—C13—C16—O7 | −173.8 (2) |
O2—Mg2—Mg3—O15B | −16.3 (12) | C14—C13—C16—O8 | −174.4 (3) |
O7ii—Mg2—Mg3—O15B | 164.4 (12) | C12—C13—C16—O8 | 5.4 (4) |
O12iii—Mg2—Mg3—O15B | 35.2 (12) | Mg1—O9—C17—O10 | 7.9 (2) |
O10—Mg2—Mg3—O15B | −148.0 (12) | Mg1—O9—C17—C18 | −169.1 (2) |
O6—Mg2—Mg3—O12iii | 52.98 (11) | Mg2—O10—C17—O9 | 114.6 (2) |
O3i—Mg2—Mg3—O12iii | −126.88 (11) | Mg1—O10—C17—O9 | −8.1 (2) |
O2—Mg2—Mg3—O12iii | −51.54 (11) | Mg2—O10—C17—C18 | −68.3 (3) |
O7ii—Mg2—Mg3—O12iii | 129.21 (11) | Mg1—O10—C17—C18 | 168.96 (19) |
O10—Mg2—Mg3—O12iii | 176.77 (15) | Mg2—O10—C17—Mg1 | 122.78 (19) |
O6—Mg2—Mg3—O11iii | 12.28 (8) | O1—Mg1—C17—O9 | 79.45 (15) |
O3i—Mg2—Mg3—O11iii | −167.58 (8) | O13—Mg1—C17—O9 | −16.80 (18) |
O2—Mg2—Mg3—O11iii | −92.23 (9) | O5—Mg1—C17—O9 | −173.53 (14) |
O7ii—Mg2—Mg3—O11iii | 88.51 (8) | O14—Mg1—C17—O9 | −93.78 (15) |
O12iii—Mg2—Mg3—O11iii | −40.70 (10) | O10—Mg1—C17—O9 | 172.0 (2) |
O10—Mg2—Mg3—O11iii | 136.07 (12) | Mg2—Mg1—C17—O9 | 146.06 (16) |
O6—Mg2—Mg3—C24iii | 28.17 (9) | O1—Mg1—C17—O10 | −92.53 (14) |
O3i—Mg2—Mg3—C24iii | −151.69 (9) | O13—Mg1—C17—O10 | 171.22 (13) |
O2—Mg2—Mg3—C24iii | −76.35 (10) | O5—Mg1—C17—O10 | 14.49 (17) |
O7ii—Mg2—Mg3—C24iii | 104.40 (9) | O14—Mg1—C17—O10 | 94.24 (14) |
O12iii—Mg2—Mg3—C24iii | −24.81 (11) | O9—Mg1—C17—O10 | −172.0 (2) |
O10—Mg2—Mg3—C24iii | 151.96 (13) | Mg2—Mg1—C17—O10 | −25.92 (11) |
O13—Mg1—O1—C1 | 170.4 (2) | O9—C17—C18—C23 | 156.9 (2) |
O5—Mg1—O1—C1 | −83.5 (2) | O10—C17—C18—C23 | −20.2 (3) |
O10—Mg1—O1—C1 | 13.5 (2) | O9—C17—C18—C19 | −21.0 (4) |
O9—Mg1—O1—C1 | 73.9 (2) | O10—C17—C18—C19 | 162.0 (2) |
C17—Mg1—O1—C1 | 44.5 (2) | C23—C18—C19—C20 | 0.8 (4) |
Mg2—Mg1—O1—C1 | −8.9 (2) | C17—C18—C19—C20 | 178.6 (2) |
O6—Mg2—O2—C1 | 45.6 (3) | C18—C19—C20—C21 | −0.7 (4) |
O3i—Mg2—O2—C1 | −135.8 (3) | C19—C20—C21—C22 | 0.3 (4) |
O12iii—Mg2—O2—C1 | 136.3 (3) | C19—C20—C21—C24 | 177.0 (2) |
O10—Mg2—O2—C1 | −40.9 (3) | C20—C21—C22—C23 | 0.1 (4) |
Mg1—Mg2—O2—C1 | −14.6 (3) | C24—C21—C22—C23 | −176.6 (2) |
O1—Mg1—O5—C9 | 81.0 (2) | C19—C18—C23—C22 | −0.4 (4) |
O13—Mg1—O5—C9 | 172.94 (19) | C17—C18—C23—C22 | −178.2 (2) |
O14—Mg1—O5—C9 | −104.2 (2) | C21—C22—C23—C18 | −0.1 (4) |
O10—Mg1—O5—C9 | −19.3 (2) | Mg3vi—O11—C24—O12 | −7.1 (2) |
O9—Mg1—O5—C9 | −34.2 (3) | Mg3vi—O11—C24—C21 | 168.6 (2) |
C17—Mg1—O5—C9 | −26.6 (2) | Mg2vi—O12—C24—O11 | −115.2 (2) |
Mg2—Mg1—O5—C9 | 7.69 (18) | Mg3vi—O12—C24—O11 | 7.2 (2) |
O2—Mg2—O6—C9 | −85.1 (3) | Mg2vi—O12—C24—C21 | 69.0 (3) |
O7ii—Mg2—O6—C9 | 93.4 (3) | Mg3vi—O12—C24—C21 | −168.5 (2) |
O12iii—Mg2—O6—C9 | −176.3 (3) | Mg2vi—O12—C24—Mg3vi | −122.45 (19) |
O10—Mg2—O6—C9 | 3.1 (3) | C20—C21—C24—O11 | −156.0 (2) |
Mg3—Mg2—O6—C9 | 157.5 (3) | C22—C21—C24—O11 | 20.7 (4) |
Mg1—Mg2—O6—C9 | −23.5 (3) | C20—C21—C24—O12 | 19.7 (4) |
O1—Mg1—O9—C17 | −103.77 (15) | C22—C21—C24—O12 | −163.6 (2) |
O13—Mg1—O9—C17 | 166.29 (15) | C20—C21—C24—Mg3vi | −59.0 (12) |
O5—Mg1—O9—C17 | 12.5 (3) | C22—C21—C24—Mg3vi | 117.7 (10) |
O14—Mg1—O9—C17 | 82.75 (15) | Mg1—O13—C25—N1 | −119.3 (3) |
O10—Mg1—O9—C17 | −4.69 (13) | C26—N1—C25—O13 | −2.7 (4) |
Mg2—Mg1—O9—C17 | −28.45 (13) | C27—N1—C25—O13 | −176.8 (3) |
O6—Mg2—O10—C17 | −159.9 (2) | Mg1—O14—C28—N2 | −166.9 (2) |
O3i—Mg2—O10—C17 | 20.6 (2) | C29—N2—C28—O14 | 0.9 (5) |
O2—Mg2—O10—C17 | −66.5 (2) | C30—N2—C28—O14 | −179.0 (3) |
O7ii—Mg2—O10—C17 | 113.4 (2) | O16—Mg3—O15—C31 | −153.7 (3) |
Mg3—Mg2—O10—C17 | 70.4 (3) | O4i—Mg3—O15—C31 | −52.5 (3) |
Mg1—Mg2—O10—C17 | −113.2 (2) | O15B—Mg3—O15—C31 | 157 (8) |
O6—Mg2—O10—Mg1 | −46.69 (9) | O12iii—Mg3—O15—C31 | 43.2 (3) |
O3i—Mg2—O10—Mg1 | 133.84 (9) | O11iii—Mg3—O15—C31 | 104.3 (3) |
O2—Mg2—O10—Mg1 | 46.74 (10) | C24iii—Mg3—O15—C31 | 74.3 (3) |
O7ii—Mg2—O10—Mg1 | −133.39 (9) | Mg2—Mg3—O15—C31 | 21.6 (3) |
Mg3—Mg2—O10—Mg1 | −176.40 (6) | Mg3—O15—C31—N3 | 172.7 (3) |
O1—Mg1—O10—C17 | 92.63 (14) | O15—C31—N3—C33 | 0.0 (6) |
O13—Mg1—O10—C17 | −17.4 (3) | O15—C31—N3—C32 | 175.8 (4) |
O5—Mg1—O10—C17 | −168.17 (14) | O16—Mg3—O15B—C31B | −109 (4) |
O14—Mg1—O10—C17 | −82.30 (14) | O4i—Mg3—O15B—C31B | −9 (4) |
O9—Mg1—O10—C17 | 4.59 (13) | O8ii—Mg3—O15B—C31B | −152 (3) |
Mg2—Mg1—O10—C17 | 136.21 (17) | O15—Mg3—O15B—C31B | 21 (5) |
O1—Mg1—O10—Mg2 | −43.59 (10) | O12iii—Mg3—O15B—C31B | 87 (4) |
O13—Mg1—O10—Mg2 | −153.57 (16) | O11iii—Mg3—O15B—C31B | 147 (5) |
O5—Mg1—O10—Mg2 | 55.62 (10) | C24iii—Mg3—O15B—C31B | 117 (4) |
O14—Mg1—O10—Mg2 | 141.49 (10) | Mg2—Mg3—O15B—C31B | 69 (5) |
O9—Mg1—O10—Mg2 | −131.63 (11) | Mg3—O15B—C31B—N3B | −117 (5) |
C17—Mg1—O10—Mg2 | −136.21 (17) | O15B—C31B—N3B—C33B | 178 (5) |
O1—Mg1—O13—C25 | −39.9 (3) | O15B—C31B—N3B—C32B | 15 (7) |
O5—Mg1—O13—C25 | −138.3 (2) | Mg3—O16—C34—N4 | −108.5 (3) |
O14—Mg1—O13—C25 | 137.2 (3) | C35—N4—C34—O16 | −1.6 (5) |
O10—Mg1—O13—C25 | 72.1 (3) | C36—N4—C34—O16 | −179.3 (3) |
Symmetry codes: (i) −x+1, y+1/2, −z+1/2; (ii) −x, y+1/2, −z+1/2; (iii) x, y−1, z; (iv) −x+1, y−1/2, −z+1/2; (v) −x, y−1/2, −z+1/2; (vi) x, y+1, z. |
Experimental details
Crystal data | |
Chemical formula | [Mg3(C8H4O4)3(C3H7NO)4] |
Mr | 857.65 |
Crystal system, space group | Monoclinic, P21/c |
Temperature (K) | 100 |
a, b, c (Å) | 18.158 (2), 9.5046 (13), 24.066 (3) |
β (°) | 100.825 (2) |
V (Å3) | 4079.6 (10) |
Z | 4 |
Radiation type | Mo Kα |
µ (mm−1) | 0.15 |
Crystal size (mm) | 0.34 × 0.20 × 0.05 |
Data collection | |
Diffractometer | Bruker SMART APEX CCD |
Absorption correction | Multi-scan (SADABS; Bruker, 2011) |
Tmin, Tmax | 0.619, 0.746 |
No. of measured, independent and observed [I > 2σ(I)] reflections | 21816, 10014, 7598 |
Rint | 0.039 |
(sin θ/λ)max (Å−1) | 0.667 |
Refinement | |
R[F2 > 2σ(F2)], wR(F2), S | 0.066, 0.149, 1.12 |
No. of reflections | 10014 |
No. of parameters | 574 |
No. of restraints | 33 |
H-atom treatment | H-atom parameters constrained |
Δρmax, Δρmin (e Å−3) | 0.46, −0.35 |
Computer programs: APEX2 (Bruker, 2011), SAINT (Bruker, 2011), SHELXTL (Sheldrick, 2008), SHELXLE (Hübschle et al., 2011) and SHELXL97 (Sheldrick, 2008), DIAMOND (Brandenburg, 2001), publCIF (Westrip, 2010).
Acknowledgements
We thank the Department of Energy (DOE), USA, for financial support (grant CDP-3.10). The X-ray diffractometer was funded by the National Science Foundation (grant 0087210), Ohio Board of Regents (grant CAP-491), and by Youngstown State University.
References
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This is an open-access article distributed under the terms of the Creative Commons Attribution (CC-BY) Licence, which permits unrestricted use, distribution, and reproduction in any medium, provided the original authors and source are cited.
The construction of metal-organic frameworks (MOFs) with light building blocks has been the subject of intense research during the past few years (Mallick et al., 2011). A suitable metal for construction of lightweight frameworks is magnesium. In the present study, the title compound, [Mg3(bdc)3(DMF)4]n, was obtained during part of our investigations into the solvothermal synthesis of lightweight metal organic frameworks. Reaction of magnesium nitrate with terephthalic acid (bdcH2) and 1,3-bis(4-pyridyl)propane (tmdpyr) at 373 K (100 °C) in dimethyl formamide (DMF) yielded the title compound as a minor product along with an unidentified white powder. The crystals of the title compound are sensitive towards solvent loss and decompose rapidly once taken out of solution.
The asymmetric unit of the title framework consists of three magnesium cations, and three anionic bdc units, and four coordinated DMF molecules, respectively (Fig. 1). One of the four DMF molecules was refined as disordered over two mutually exclusive positions with an occupancy ratio of 0.923 (4) to 0.077 (4).
The three magnesium cations in the structure form secondary building units (SBUs) that each possesses a chain of three magnesium ions bridged by six bdc linkers and coordinated by four terminal DMF molecules (Fig. 2). There are two types of magnesium coordination environments in the structure. The terminal ions, Mg1 and Mg3, in the SBU exhibit distorted octahedral geometries. Of the six bonds, four are from O atoms of three different bdc linkers (one bdc linker binds with magnesium in a chelating mode) and the other two are from DMF O atoms. The central ion, Mg2, is also distorted octahedrally coordinated, but it binds to six different carboxylate O atoms (four of them are in bidentate mode and two are in chelation mode). O—Mg—O angles vary between 60.35 (7) and 178.54 (9)°, with the unusually small angle of 60.35 (7)° being associated with the bdc linker in chelation mode. The three distorted octahedral trimeric magnesiums together act as a node that is connected with other nodes through the bdc linkers to give rise to a two-dimensional layered 36-network (Fig. 3). The layers in the structure are stacked atop of one another, with terminal DMF molecules that are projecting into the inter-lamellar space (Fig. 4). The structure is isoreticular to previously reported magnesium and bdc based framework compounds, Mg3(bdc)3(X)4 [X = DMSO, Rood et al., 2006; DMA, Davies et al., 2007] in which the terminal solvent molecules, DMSO and DMA, project in to the inter-lamellar spaces. Similar layered structures have also been reported with zinc-bdc based frameworks (Edgar et al., 2001; Burrows et al., 2005; Williams et al., 2005; Grzesiak et al., 2006).