The title compound, [MgBr2(C4H8O)4], forms crystals which appear to be monoclinic but are actually twinned triclinic. The current form is a new triclinic polymorph, with Z'= 2, in addition to the already known tetragonal polymorph. Although the geometric parameters of the two polymorphs agree well, their packing patterns are completely different.
Supporting information
CCDC reference: 645523
Data collection: X-AREA (Stoe & Cie, 2001); cell refinement: X-AREA; data reduction: X-AREA; program(s) used to solve structure: SHELXS97 (Sheldrick, 1997); program(s) used to refine structure: SHELXL97 (Sheldrick, 1997); molecular graphics: XP in SHELXTL-Plus (Sheldrick, 1991); software used to prepare material for publication: SHELXL97.
dibromidotetrakis(tetrahydrofuran-
κO)magnesium
top
Crystal data top
[MgBr2(C4H8O)4] | Z = 4 |
Mr = 472.55 | F(000) = 968 |
Triclinic, P1 | Dx = 1.502 Mg m−3 |
Hall symbol: -P 1 | Mo Kα radiation, λ = 0.71073 Å |
a = 8.6620 (9) Å | Cell parameters from 4198 reflections |
b = 15.6820 (12) Å | θ = 4.9–24.6° |
c = 15.6910 (13) Å | µ = 3.93 mm−1 |
α = 80.501 (9)° | T = 173 K |
β = 85.131 (11)° | Block, colourless |
γ = 85.190 (11)° | 0.27 × 0.26 × 0.24 mm |
V = 2089.3 (3) Å3 | |
Data collection top
Stoe IPDSII two-circle diffractometer | 7347 independent reflections |
Radiation source: fine-focus sealed tube | 4969 reflections with I > 2σ(I) |
Graphite monochromator | Rint = 0.080 |
ω scans | θmax = 25.0°, θmin = 2.4° |
Absorption correction: multi-scan (MULABS; Spek, 2003; Blessing, 1995) | h = −10→10 |
Tmin = 0.342, Tmax = 0.420 | k = −18→18 |
22055 measured reflections | l = −18→18 |
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)] = 0.087 | Hydrogen site location: inferred from neighbouring sites |
wR(F2) = 0.232 | H-atom parameters constrained |
S = 1.44 | w = 1/[σ2(Fo2) + (0.091P)2] where P = (Fo2 + 2Fc2)/3 |
7347 reflections | (Δ/σ)max < 0.001 |
416 parameters | Δρmax = 0.97 e Å−3 |
0 restraints | Δρmin = −1.11 e Å−3 |
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 | |
Mg1 | 0.5332 (4) | 0.2517 (2) | 0.2364 (2) | 0.0296 (7) | |
Br1 | 0.6760 (2) | 0.30828 (12) | 0.35037 (11) | 0.0764 (5) | |
Br2 | 0.3991 (2) | 0.18541 (12) | 0.12361 (11) | 0.0814 (5) | |
O11 | 0.6456 (9) | 0.3393 (4) | 0.1393 (4) | 0.0357 (18) | |
C12 | 0.6953 (17) | 0.3213 (9) | 0.0507 (7) | 0.052 (3) | |
H12A | 0.7575 | 0.2651 | 0.0529 | 0.062* | |
H12B | 0.6044 | 0.3202 | 0.0168 | 0.062* | |
C13 | 0.7913 (17) | 0.3950 (9) | 0.0124 (7) | 0.054 (3) | |
H13A | 0.7815 | 0.4096 | −0.0508 | 0.065* | |
H13B | 0.9022 | 0.3798 | 0.0228 | 0.065* | |
C14 | 0.7277 (14) | 0.4717 (7) | 0.0580 (6) | 0.040 (3) | |
H14A | 0.8084 | 0.5128 | 0.0582 | 0.049* | |
H14B | 0.6367 | 0.5030 | 0.0300 | 0.049* | |
C15 | 0.6833 (14) | 0.4284 (7) | 0.1472 (7) | 0.038 (3) | |
H15A | 0.7703 | 0.4261 | 0.1848 | 0.045* | |
H15B | 0.5920 | 0.4603 | 0.1725 | 0.045* | |
O21 | 0.3520 (9) | 0.3500 (5) | 0.2357 (4) | 0.0377 (17) | |
C22 | 0.2829 (15) | 0.3863 (8) | 0.3087 (8) | 0.048 (3) | |
H22A | 0.3423 | 0.4343 | 0.3195 | 0.058* | |
H22B | 0.2793 | 0.3418 | 0.3613 | 0.058* | |
C23 | 0.1132 (16) | 0.4209 (11) | 0.2837 (11) | 0.070 (4) | |
H23A | 0.0340 | 0.3845 | 0.3173 | 0.084* | |
H23B | 0.0898 | 0.4818 | 0.2928 | 0.084* | |
C24 | 0.1223 (15) | 0.4132 (10) | 0.1885 (10) | 0.066 (4) | |
H24A | 0.0634 | 0.3642 | 0.1798 | 0.079* | |
H24B | 0.0767 | 0.4670 | 0.1549 | 0.079* | |
C25 | 0.2757 (17) | 0.3993 (9) | 0.1611 (8) | 0.056 (4) | |
H25A | 0.3231 | 0.4552 | 0.1417 | 0.067* | |
H25B | 0.2858 | 0.3661 | 0.1122 | 0.067* | |
O31 | 0.4001 (9) | 0.1769 (5) | 0.3345 (5) | 0.044 (2) | |
C32 | 0.2360 (15) | 0.1651 (9) | 0.3349 (8) | 0.054 (3) | |
H32A | 0.2006 | 0.1781 | 0.2755 | 0.065* | |
H32B | 0.1736 | 0.2029 | 0.3716 | 0.065* | |
C33 | 0.2233 (16) | 0.0732 (10) | 0.3712 (10) | 0.071 (5) | |
H33A | 0.2431 | 0.0366 | 0.3252 | 0.085* | |
H33B | 0.1185 | 0.0637 | 0.3999 | 0.085* | |
C34 | 0.3472 (15) | 0.0520 (9) | 0.4371 (7) | 0.049 (3) | |
H34A | 0.4048 | −0.0044 | 0.4317 | 0.059* | |
H34B | 0.2994 | 0.0495 | 0.4970 | 0.059* | |
C35 | 0.4570 (16) | 0.1277 (8) | 0.4140 (7) | 0.048 (3) | |
H35A | 0.4496 | 0.1637 | 0.4605 | 0.058* | |
H35B | 0.5663 | 0.1052 | 0.4045 | 0.058* | |
O41 | 0.7155 (9) | 0.1549 (5) | 0.2299 (6) | 0.045 (2) | |
C42 | 0.7011 (19) | 0.0643 (9) | 0.2230 (15) | 0.086 (6) | |
H42A | 0.6659 | 0.0324 | 0.2802 | 0.103* | |
H42B | 0.6226 | 0.0606 | 0.1817 | 0.103* | |
C43 | 0.8473 (17) | 0.0257 (11) | 0.1938 (12) | 0.073 (4) | |
H43A | 0.8398 | 0.0043 | 0.1385 | 0.088* | |
H43B | 0.8841 | −0.0231 | 0.2375 | 0.088* | |
C44 | 0.9561 (17) | 0.0995 (10) | 0.1817 (10) | 0.065 (4) | |
H44A | 1.0562 | 0.0782 | 0.2065 | 0.078* | |
H44B | 0.9771 | 0.1211 | 0.1192 | 0.078* | |
C45 | 0.8842 (14) | 0.1679 (10) | 0.2244 (11) | 0.062 (4) | |
H45A | 0.9062 | 0.2252 | 0.1905 | 0.074* | |
H45B | 0.9217 | 0.1639 | 0.2829 | 0.074* | |
Mg2 | 0.5228 (4) | 0.2559 (2) | 0.7201 (2) | 0.0301 (7) | |
Br3 | 0.6589 (2) | 0.36779 (12) | 0.78819 (11) | 0.0789 (5) | |
Br4 | 0.3830 (2) | 0.14575 (11) | 0.65671 (10) | 0.0769 (5) | |
O51 | 0.7160 (9) | 0.2453 (5) | 0.6326 (5) | 0.0393 (17) | |
C52 | 0.8120 (18) | 0.3176 (9) | 0.5852 (9) | 0.066 (4) | |
H52A | 0.7535 | 0.3548 | 0.5397 | 0.080* | |
H52B | 0.8434 | 0.3540 | 0.6258 | 0.080* | |
C53 | 0.9457 (16) | 0.2716 (11) | 0.5475 (9) | 0.064 (4) | |
H53A | 0.9604 | 0.2944 | 0.4849 | 0.077* | |
H53B | 1.0398 | 0.2815 | 0.5752 | 0.077* | |
C54 | 0.926 (2) | 0.1817 (12) | 0.5590 (14) | 0.093 (6) | |
H54A | 0.9982 | 0.1500 | 0.6011 | 0.112* | |
H54B | 0.9496 | 0.1599 | 0.5032 | 0.112* | |
C55 | 0.7649 (16) | 0.1683 (9) | 0.5912 (11) | 0.062 (4) | |
H55A | 0.7583 | 0.1143 | 0.6337 | 0.075* | |
H55B | 0.6998 | 0.1652 | 0.5430 | 0.075* | |
O61 | 0.4165 (9) | 0.3611 (4) | 0.6352 (4) | 0.0327 (16) | |
C62 | 0.3537 (14) | 0.4428 (7) | 0.6605 (7) | 0.041 (3) | |
H62A | 0.4336 | 0.4856 | 0.6512 | 0.049* | |
H62B | 0.3147 | 0.4345 | 0.7223 | 0.049* | |
C63 | 0.2198 (14) | 0.4728 (7) | 0.6014 (7) | 0.036 (2) | |
H63A | 0.1985 | 0.5365 | 0.5937 | 0.044* | |
H63B | 0.1235 | 0.4446 | 0.6246 | 0.044* | |
C64 | 0.2855 (15) | 0.4425 (8) | 0.5159 (7) | 0.045 (3) | |
H64A | 0.2005 | 0.4330 | 0.4808 | 0.054* | |
H64B | 0.3524 | 0.4856 | 0.4813 | 0.054* | |
C65 | 0.3784 (14) | 0.3587 (7) | 0.5445 (6) | 0.036 (2) | |
H65A | 0.3170 | 0.3086 | 0.5427 | 0.043* | |
H65B | 0.4747 | 0.3537 | 0.5063 | 0.043* | |
O71 | 0.3342 (9) | 0.2648 (5) | 0.8119 (4) | 0.0338 (16) | |
C72 | 0.1750 (13) | 0.2644 (8) | 0.7925 (7) | 0.040 (3) | |
H72A | 0.1438 | 0.2043 | 0.7979 | 0.049* | |
H72B | 0.1592 | 0.2946 | 0.7329 | 0.049* | |
C73 | 0.0807 (16) | 0.3131 (11) | 0.8604 (9) | 0.064 (4) | |
H73A | −0.0284 | 0.2972 | 0.8698 | 0.077* | |
H73B | 0.0830 | 0.3768 | 0.8443 | 0.077* | |
C74 | 0.1756 (16) | 0.2773 (10) | 0.9409 (8) | 0.056 (4) | |
H74A | 0.1581 | 0.3156 | 0.9856 | 0.067* | |
H74B | 0.1484 | 0.2181 | 0.9670 | 0.067* | |
C75 | 0.3388 (14) | 0.2772 (10) | 0.9025 (7) | 0.049 (3) | |
H75A | 0.3828 | 0.3328 | 0.9053 | 0.059* | |
H75B | 0.4039 | 0.2296 | 0.9344 | 0.059* | |
O81 | 0.6313 (9) | 0.1544 (5) | 0.8070 (5) | 0.0426 (19) | |
C82 | 0.7997 (16) | 0.1451 (9) | 0.8194 (8) | 0.057 (3) | |
H82A | 0.8458 | 0.2019 | 0.8079 | 0.068* | |
H82B | 0.8562 | 0.1059 | 0.7820 | 0.068* | |
C83 | 0.7995 (19) | 0.1045 (12) | 0.9175 (10) | 0.072 (4) | |
H83A | 0.8939 | 0.0654 | 0.9286 | 0.087* | |
H83B | 0.7955 | 0.1504 | 0.9542 | 0.087* | |
C84 | 0.6566 (17) | 0.0549 (9) | 0.9359 (8) | 0.058 (4) | |
H84A | 0.5915 | 0.0738 | 0.9852 | 0.069* | |
H84B | 0.6853 | −0.0079 | 0.9505 | 0.069* | |
C85 | 0.5681 (15) | 0.0737 (8) | 0.8536 (8) | 0.045 (3) | |
H85A | 0.5885 | 0.0260 | 0.8190 | 0.054* | |
H85B | 0.4549 | 0.0822 | 0.8677 | 0.054* | |
Atomic displacement parameters (Å2) top | U11 | U22 | U33 | U12 | U13 | U23 |
Mg1 | 0.0284 (18) | 0.0293 (15) | 0.0315 (16) | −0.0046 (14) | −0.0093 (14) | −0.0008 (13) |
Br1 | 0.0900 (13) | 0.0755 (10) | 0.0665 (9) | −0.0170 (10) | −0.0161 (9) | −0.0089 (8) |
Br2 | 0.0984 (14) | 0.0770 (11) | 0.0730 (10) | −0.0118 (10) | −0.0194 (10) | −0.0150 (9) |
O11 | 0.056 (5) | 0.029 (4) | 0.025 (3) | −0.014 (3) | 0.007 (3) | −0.013 (3) |
C12 | 0.071 (9) | 0.056 (7) | 0.033 (6) | −0.010 (7) | 0.008 (6) | −0.023 (5) |
C13 | 0.063 (9) | 0.065 (8) | 0.030 (5) | −0.010 (7) | 0.022 (6) | −0.002 (5) |
C14 | 0.044 (7) | 0.046 (6) | 0.031 (5) | −0.017 (5) | −0.003 (5) | 0.003 (5) |
C15 | 0.044 (7) | 0.042 (6) | 0.031 (5) | −0.006 (5) | 0.000 (5) | −0.013 (4) |
O21 | 0.045 (5) | 0.044 (4) | 0.023 (3) | 0.006 (4) | −0.013 (3) | −0.001 (3) |
C22 | 0.042 (7) | 0.056 (7) | 0.049 (7) | −0.003 (6) | 0.007 (6) | −0.020 (6) |
C23 | 0.028 (7) | 0.085 (11) | 0.090 (11) | −0.009 (7) | 0.016 (7) | −0.003 (8) |
C24 | 0.029 (8) | 0.078 (10) | 0.087 (10) | −0.003 (7) | −0.027 (7) | 0.011 (8) |
C25 | 0.067 (10) | 0.051 (7) | 0.048 (7) | 0.021 (7) | −0.031 (7) | −0.005 (6) |
O31 | 0.038 (5) | 0.048 (4) | 0.045 (4) | −0.015 (4) | −0.028 (4) | 0.015 (3) |
C32 | 0.045 (8) | 0.062 (8) | 0.052 (7) | −0.007 (6) | −0.015 (6) | 0.011 (6) |
C33 | 0.039 (8) | 0.085 (10) | 0.084 (10) | −0.036 (7) | −0.027 (7) | 0.027 (8) |
C34 | 0.049 (7) | 0.059 (7) | 0.035 (6) | −0.008 (6) | −0.006 (5) | 0.014 (5) |
C35 | 0.059 (8) | 0.050 (7) | 0.032 (5) | −0.018 (6) | −0.022 (6) | 0.021 (5) |
O41 | 0.032 (4) | 0.029 (4) | 0.078 (6) | −0.010 (3) | −0.013 (4) | −0.011 (4) |
C42 | 0.057 (10) | 0.030 (7) | 0.174 (18) | −0.012 (7) | −0.024 (11) | −0.015 (9) |
C43 | 0.048 (9) | 0.066 (9) | 0.112 (13) | 0.000 (7) | 0.004 (9) | −0.039 (9) |
C44 | 0.048 (8) | 0.079 (10) | 0.078 (9) | −0.010 (7) | −0.008 (7) | −0.035 (8) |
C45 | 0.023 (7) | 0.062 (9) | 0.104 (11) | −0.005 (6) | −0.011 (7) | −0.019 (8) |
Mg2 | 0.0278 (18) | 0.0307 (16) | 0.0346 (17) | −0.0082 (14) | −0.0073 (15) | −0.0076 (14) |
Br3 | 0.0824 (13) | 0.0756 (11) | 0.0841 (11) | −0.0163 (9) | −0.0171 (10) | −0.0177 (8) |
Br4 | 0.0883 (13) | 0.0726 (10) | 0.0722 (10) | −0.0186 (9) | −0.0028 (9) | −0.0139 (8) |
O51 | 0.039 (5) | 0.033 (4) | 0.048 (4) | −0.013 (3) | 0.004 (4) | −0.008 (3) |
C52 | 0.071 (10) | 0.061 (8) | 0.065 (8) | −0.040 (8) | 0.009 (8) | 0.009 (7) |
C53 | 0.041 (8) | 0.089 (11) | 0.059 (8) | −0.025 (7) | 0.020 (6) | −0.007 (7) |
C54 | 0.071 (12) | 0.086 (12) | 0.124 (15) | −0.015 (10) | 0.048 (11) | −0.041 (11) |
C55 | 0.041 (8) | 0.051 (8) | 0.096 (11) | −0.014 (6) | 0.019 (7) | −0.020 (7) |
O61 | 0.041 (4) | 0.032 (4) | 0.028 (3) | 0.001 (3) | −0.007 (3) | −0.012 (3) |
C62 | 0.049 (7) | 0.036 (6) | 0.040 (6) | −0.005 (5) | 0.001 (5) | −0.012 (5) |
C63 | 0.040 (6) | 0.031 (5) | 0.040 (6) | 0.003 (5) | −0.001 (5) | −0.015 (4) |
C64 | 0.056 (8) | 0.049 (7) | 0.029 (5) | 0.005 (6) | −0.001 (5) | −0.005 (5) |
C65 | 0.047 (7) | 0.040 (6) | 0.023 (5) | −0.001 (5) | −0.018 (5) | −0.008 (4) |
O71 | 0.032 (4) | 0.050 (4) | 0.020 (3) | 0.000 (3) | −0.009 (3) | −0.007 (3) |
C72 | 0.037 (7) | 0.059 (7) | 0.033 (5) | −0.013 (5) | −0.006 (5) | −0.025 (5) |
C73 | 0.034 (7) | 0.101 (11) | 0.070 (8) | −0.013 (7) | −0.013 (7) | −0.037 (8) |
C74 | 0.058 (9) | 0.078 (9) | 0.038 (6) | −0.014 (7) | 0.006 (6) | −0.027 (6) |
C75 | 0.028 (6) | 0.087 (9) | 0.036 (6) | −0.002 (6) | −0.006 (5) | −0.015 (6) |
O81 | 0.033 (4) | 0.042 (4) | 0.054 (4) | −0.020 (4) | −0.016 (4) | 0.007 (4) |
C82 | 0.046 (8) | 0.066 (8) | 0.054 (7) | −0.008 (6) | −0.007 (6) | 0.009 (6) |
C83 | 0.058 (10) | 0.099 (12) | 0.071 (9) | 0.001 (9) | −0.012 (8) | −0.045 (9) |
C84 | 0.061 (9) | 0.061 (8) | 0.044 (7) | −0.009 (7) | 0.001 (6) | 0.013 (6) |
C85 | 0.047 (8) | 0.043 (6) | 0.048 (6) | −0.023 (6) | −0.006 (6) | −0.003 (5) |
Geometric parameters (Å, º) top
Mg1—O31 | 2.099 (8) | Mg2—O51 | 2.087 (9) |
Mg1—O41 | 2.105 (9) | Mg2—O71 | 2.096 (8) |
Mg1—O21 | 2.105 (8) | Mg2—O81 | 2.128 (8) |
Mg1—O11 | 2.106 (8) | Mg2—O61 | 2.138 (8) |
Mg1—Br1 | 2.569 (3) | Mg2—Br4 | 2.562 (4) |
Mg1—Br2 | 2.592 (3) | Mg2—Br3 | 2.605 (4) |
O11—C15 | 1.488 (13) | O51—C52 | 1.518 (14) |
O11—C12 | 1.485 (12) | O51—C55 | 1.479 (15) |
C12—C13 | 1.495 (18) | C52—C53 | 1.45 (2) |
C12—H12A | 0.9900 | C52—H52A | 0.9900 |
C12—H12B | 0.9900 | C52—H52B | 0.9900 |
C13—C14 | 1.539 (17) | C53—C54 | 1.41 (2) |
C13—H13A | 0.9900 | C53—H53A | 0.9900 |
C13—H13B | 0.9900 | C53—H53B | 0.9900 |
C14—C15 | 1.485 (15) | C54—C55 | 1.47 (2) |
C14—H14A | 0.9900 | C54—H54A | 0.9900 |
C14—H14B | 0.9900 | C54—H54B | 0.9900 |
C15—H15A | 0.9900 | C55—H55A | 0.9900 |
C15—H15B | 0.9900 | C55—H55B | 0.9900 |
O21—C22 | 1.427 (14) | O61—C62 | 1.452 (13) |
O21—C25 | 1.467 (13) | O61—C65 | 1.495 (11) |
C22—C23 | 1.58 (2) | C62—C63 | 1.541 (16) |
C22—H22A | 0.9900 | C62—H62A | 0.9900 |
C22—H22B | 0.9900 | C62—H62B | 0.9900 |
C23—C24 | 1.51 (2) | C63—C64 | 1.545 (15) |
C23—H23A | 0.9900 | C63—H63A | 0.9900 |
C23—H23B | 0.9900 | C63—H63B | 0.9900 |
C24—C25 | 1.37 (2) | C64—C65 | 1.505 (16) |
C24—H24A | 0.9900 | C64—H64A | 0.9900 |
C24—H24B | 0.9900 | C64—H64B | 0.9900 |
C25—H25A | 0.9900 | C65—H65A | 0.9900 |
C25—H25B | 0.9900 | C65—H65B | 0.9900 |
O31—C32 | 1.448 (15) | O71—C72 | 1.438 (13) |
O31—C35 | 1.455 (12) | O71—C75 | 1.471 (12) |
C32—C33 | 1.468 (19) | C72—C73 | 1.551 (17) |
C32—H32A | 0.9900 | C72—H72A | 0.9900 |
C32—H32B | 0.9900 | C72—H72B | 0.9900 |
C33—C34 | 1.532 (17) | C73—C74 | 1.57 (2) |
C33—H33A | 0.9900 | C73—H73A | 0.9900 |
C33—H33B | 0.9900 | C73—H73B | 0.9900 |
C34—C35 | 1.561 (17) | C74—C75 | 1.488 (18) |
C34—H34A | 0.9900 | C74—H74A | 0.9900 |
C34—H34B | 0.9900 | C74—H74B | 0.9900 |
C35—H35A | 0.9900 | C75—H75A | 0.9900 |
C35—H35B | 0.9900 | C75—H75B | 0.9900 |
O41—C42 | 1.458 (15) | O81—C85 | 1.476 (13) |
O41—C45 | 1.486 (14) | O81—C82 | 1.480 (15) |
C42—C43 | 1.43 (2) | C82—C83 | 1.57 (2) |
C42—H42A | 0.9900 | C82—H82A | 0.9900 |
C42—H42B | 0.9900 | C82—H82B | 0.9900 |
C43—C44 | 1.53 (2) | C83—C84 | 1.50 (2) |
C43—H43A | 0.9900 | C83—H83A | 0.9900 |
C43—H43B | 0.9900 | C83—H83B | 0.9900 |
C44—C45 | 1.43 (2) | C84—C85 | 1.532 (17) |
C44—H44A | 0.9900 | C84—H84A | 0.9900 |
C44—H44B | 0.9900 | C84—H84B | 0.9900 |
C45—H45A | 0.9900 | C85—H85A | 0.9900 |
C45—H45B | 0.9900 | C85—H85B | 0.9900 |
| | | |
O31—Mg1—O41 | 94.6 (3) | O51—Mg2—O71 | 177.8 (3) |
O31—Mg1—O21 | 87.7 (3) | O51—Mg2—O81 | 88.2 (3) |
O41—Mg1—O21 | 177.0 (4) | O71—Mg2—O81 | 89.8 (3) |
O31—Mg1—O11 | 172.9 (4) | O51—Mg2—O61 | 92.1 (3) |
O41—Mg1—O11 | 92.5 (3) | O71—Mg2—O61 | 89.9 (3) |
O21—Mg1—O11 | 85.3 (3) | O81—Mg2—O61 | 178.0 (3) |
O31—Mg1—Br1 | 90.6 (2) | O51—Mg2—Br4 | 91.9 (2) |
O41—Mg1—Br1 | 88.4 (2) | O71—Mg2—Br4 | 89.1 (2) |
O21—Mg1—Br1 | 93.5 (2) | O81—Mg2—Br4 | 90.7 (2) |
O11—Mg1—Br1 | 89.1 (2) | O61—Mg2—Br4 | 91.3 (2) |
O31—Mg1—Br2 | 88.4 (2) | O51—Mg2—Br3 | 89.7 (2) |
O41—Mg1—Br2 | 88.3 (2) | O71—Mg2—Br3 | 89.3 (2) |
O21—Mg1—Br2 | 89.8 (2) | O81—Mg2—Br3 | 89.1 (2) |
O11—Mg1—Br2 | 92.3 (2) | O61—Mg2—Br3 | 89.0 (2) |
Br1—Mg1—Br2 | 176.43 (16) | Br4—Mg2—Br3 | 178.38 (17) |
C15—O11—C12 | 109.7 (8) | C52—O51—C55 | 106.2 (9) |
C15—O11—Mg1 | 126.1 (6) | C52—O51—Mg2 | 127.6 (8) |
C12—O11—Mg1 | 124.2 (6) | C55—O51—Mg2 | 125.2 (7) |
C13—C12—O11 | 103.9 (9) | C53—C52—O51 | 103.3 (11) |
C13—C12—H12A | 111.0 | C53—C52—H52A | 111.1 |
O11—C12—H12A | 111.0 | O51—C52—H52A | 111.1 |
C13—C12—H12B | 111.0 | C53—C52—H52B | 111.1 |
O11—C12—H12B | 111.0 | O51—C52—H52B | 111.1 |
H12A—C12—H12B | 109.0 | H52A—C52—H52B | 109.1 |
C12—C13—C14 | 105.8 (9) | C54—C53—C52 | 111.0 (12) |
C12—C13—H13A | 110.6 | C54—C53—H53A | 109.4 |
C14—C13—H13A | 110.6 | C52—C53—H53A | 109.4 |
C12—C13—H13B | 110.6 | C54—C53—H53B | 109.4 |
C14—C13—H13B | 110.6 | C52—C53—H53B | 109.4 |
H13A—C13—H13B | 108.7 | H53A—C53—H53B | 108.0 |
C15—C14—C13 | 102.6 (9) | C53—C54—C55 | 107.9 (14) |
C15—C14—H14A | 111.3 | C53—C54—H54A | 110.1 |
C13—C14—H14A | 111.3 | C55—C54—H54A | 110.1 |
C15—C14—H14B | 111.3 | C53—C54—H54B | 110.1 |
C13—C14—H14B | 111.3 | C55—C54—H54B | 110.1 |
H14A—C14—H14B | 109.2 | H54A—C54—H54B | 108.4 |
O11—C15—C14 | 106.3 (8) | C54—C55—O51 | 103.7 (11) |
O11—C15—H15A | 110.5 | C54—C55—H55A | 111.0 |
C14—C15—H15A | 110.5 | O51—C55—H55A | 111.0 |
O11—C15—H15B | 110.5 | C54—C55—H55B | 111.0 |
C14—C15—H15B | 110.5 | O51—C55—H55B | 111.0 |
H15A—C15—H15B | 108.7 | H55A—C55—H55B | 109.0 |
C22—O21—C25 | 105.1 (9) | C62—O61—C65 | 109.3 (7) |
C22—O21—Mg1 | 126.6 (7) | C62—O61—Mg2 | 124.7 (6) |
C25—O21—Mg1 | 128.2 (7) | C65—O61—Mg2 | 125.6 (6) |
O21—C22—C23 | 105.0 (10) | O61—C62—C63 | 104.4 (8) |
O21—C22—H22A | 110.7 | O61—C62—H62A | 110.9 |
C23—C22—H22A | 110.7 | C63—C62—H62A | 110.9 |
O21—C22—H22B | 110.7 | O61—C62—H62B | 110.9 |
C23—C22—H22B | 110.7 | C63—C62—H62B | 110.9 |
H22A—C22—H22B | 108.8 | H62A—C62—H62B | 108.9 |
C24—C23—C22 | 101.6 (11) | C62—C63—C64 | 101.8 (9) |
C24—C23—H23A | 111.5 | C62—C63—H63A | 111.4 |
C22—C23—H23A | 111.5 | C64—C63—H63A | 111.4 |
C24—C23—H23B | 111.5 | C62—C63—H63B | 111.4 |
C22—C23—H23B | 111.5 | C64—C63—H63B | 111.4 |
H23A—C23—H23B | 109.3 | H63A—C63—H63B | 109.3 |
C25—C24—C23 | 108.2 (11) | C65—C64—C63 | 104.2 (8) |
C25—C24—H24A | 110.1 | C65—C64—H64A | 110.9 |
C23—C24—H24A | 110.1 | C63—C64—H64A | 110.9 |
C25—C24—H24B | 110.1 | C65—C64—H64B | 110.9 |
C23—C24—H24B | 110.1 | C63—C64—H64B | 110.9 |
H24A—C24—H24B | 108.4 | H64A—C64—H64B | 108.9 |
C24—C25—O21 | 106.3 (12) | O61—C65—C64 | 106.1 (8) |
C24—C25—H25A | 110.5 | O61—C65—H65A | 110.5 |
O21—C25—H25A | 110.5 | C64—C65—H65A | 110.5 |
C24—C25—H25B | 110.5 | O61—C65—H65B | 110.5 |
O21—C25—H25B | 110.5 | C64—C65—H65B | 110.5 |
H25A—C25—H25B | 108.7 | H65A—C65—H65B | 108.7 |
C32—O31—C35 | 108.1 (8) | C72—O71—C75 | 109.1 (8) |
C32—O31—Mg1 | 126.1 (6) | C72—O71—Mg2 | 123.5 (5) |
C35—O31—Mg1 | 125.8 (7) | C75—O71—Mg2 | 127.4 (6) |
O31—C32—C33 | 103.9 (10) | O71—C72—C73 | 104.7 (8) |
O31—C32—H32A | 111.0 | O71—C72—H72A | 110.8 |
C33—C32—H32A | 111.0 | C73—C72—H72A | 110.8 |
O31—C32—H32B | 111.0 | O71—C72—H72B | 110.8 |
C33—C32—H32B | 111.0 | C73—C72—H72B | 110.8 |
H32A—C32—H32B | 109.0 | H72A—C72—H72B | 108.9 |
C32—C33—C34 | 105.2 (10) | C72—C73—C74 | 99.1 (11) |
C32—C33—H33A | 110.7 | C72—C73—H73A | 112.0 |
C34—C33—H33A | 110.7 | C74—C73—H73A | 112.0 |
C32—C33—H33B | 110.7 | C72—C73—H73B | 112.0 |
C34—C33—H33B | 110.7 | C74—C73—H73B | 112.0 |
H33A—C33—H33B | 108.8 | H73A—C73—H73B | 109.6 |
C33—C34—C35 | 104.6 (9) | C75—C74—C73 | 102.4 (10) |
C33—C34—H34A | 110.8 | C75—C74—H74A | 111.3 |
C35—C34—H34A | 110.8 | C73—C74—H74A | 111.3 |
C33—C34—H34B | 110.8 | C75—C74—H74B | 111.3 |
C35—C34—H34B | 110.8 | C73—C74—H74B | 111.3 |
H34A—C34—H34B | 108.9 | H74A—C74—H74B | 109.2 |
O31—C35—C34 | 103.7 (8) | O71—C75—C74 | 106.7 (9) |
O31—C35—H35A | 111.0 | O71—C75—H75A | 110.4 |
C34—C35—H35A | 111.0 | C74—C75—H75A | 110.4 |
O31—C35—H35B | 111.0 | O71—C75—H75B | 110.4 |
C34—C35—H35B | 111.0 | C74—C75—H75B | 110.4 |
H35A—C35—H35B | 109.0 | H75A—C75—H75B | 108.6 |
C42—O41—C45 | 107.0 (10) | C85—O81—C82 | 105.8 (9) |
C42—O41—Mg1 | 126.7 (8) | C85—O81—Mg2 | 129.3 (7) |
C45—O41—Mg1 | 126.1 (7) | C82—O81—Mg2 | 124.1 (7) |
C43—C42—O41 | 110.1 (12) | O81—C82—C83 | 101.1 (10) |
C43—C42—H42A | 109.6 | O81—C82—H82A | 111.5 |
O41—C42—H42A | 109.6 | C83—C82—H82A | 111.5 |
C43—C42—H42B | 109.6 | O81—C82—H82B | 111.5 |
O41—C42—H42B | 109.6 | C83—C82—H82B | 111.5 |
H42A—C42—H42B | 108.1 | H82A—C82—H82B | 109.4 |
C42—C43—C44 | 104.0 (12) | C84—C83—C82 | 105.3 (11) |
C42—C43—H43A | 111.0 | C84—C83—H83A | 110.7 |
C44—C43—H43A | 111.0 | C82—C83—H83A | 110.7 |
C42—C43—H43B | 111.0 | C84—C83—H83B | 110.7 |
C44—C43—H43B | 111.0 | C82—C83—H83B | 110.7 |
H43A—C43—H43B | 109.0 | H83A—C83—H83B | 108.8 |
C45—C44—C43 | 108.9 (12) | C83—C84—C85 | 106.8 (11) |
C45—C44—H44A | 109.9 | C83—C84—H84A | 110.4 |
C43—C44—H44A | 109.9 | C85—C84—H84A | 110.4 |
C45—C44—H44B | 109.9 | C83—C84—H84B | 110.4 |
C43—C44—H44B | 109.9 | C85—C84—H84B | 110.4 |
H44A—C44—H44B | 108.3 | H84A—C84—H84B | 108.6 |
C44—C45—O41 | 104.6 (10) | O81—C85—C84 | 103.1 (9) |
C44—C45—H45A | 110.8 | O81—C85—H85A | 111.1 |
O41—C45—H45A | 110.8 | C84—C85—H85A | 111.1 |
C44—C45—H45B | 110.8 | O81—C85—H85B | 111.1 |
O41—C45—H45B | 110.8 | C84—C85—H85B | 111.1 |
H45A—C45—H45B | 108.9 | H85A—C85—H85B | 109.1 |
| | | |
O41—Mg1—O11—C15 | −124.6 (8) | O81—Mg2—O51—C52 | −129.7 (9) |
O21—Mg1—O11—C15 | 57.4 (8) | O61—Mg2—O51—C52 | 48.4 (10) |
Br1—Mg1—O11—C15 | −36.2 (8) | Br4—Mg2—O51—C52 | 139.7 (9) |
Br2—Mg1—O11—C15 | 147.1 (8) | Br3—Mg2—O51—C52 | −40.6 (9) |
O41—Mg1—O11—C12 | 57.3 (9) | O81—Mg2—O51—C55 | 64.1 (10) |
O21—Mg1—O11—C12 | −120.7 (9) | O61—Mg2—O51—C55 | −117.9 (10) |
Br1—Mg1—O11—C12 | 145.6 (8) | Br4—Mg2—O51—C55 | −26.5 (10) |
Br2—Mg1—O11—C12 | −31.1 (9) | Br3—Mg2—O51—C55 | 153.2 (10) |
C15—O11—C12—C13 | 10.9 (13) | C55—O51—C52—C53 | −22.4 (14) |
Mg1—O11—C12—C13 | −170.7 (8) | Mg2—O51—C52—C53 | 169.3 (8) |
O11—C12—C13—C14 | −28.1 (13) | O51—C52—C53—C54 | 7.6 (19) |
C12—C13—C14—C15 | 34.9 (13) | C52—C53—C54—C55 | 10 (2) |
C12—O11—C15—C14 | 11.1 (12) | C53—C54—C55—O51 | −24 (2) |
Mg1—O11—C15—C14 | −167.3 (7) | C52—O51—C55—C54 | 28.4 (16) |
C13—C14—C15—O11 | −27.6 (12) | Mg2—O51—C55—C54 | −162.9 (12) |
O31—Mg1—O21—C22 | 52.9 (9) | O51—Mg2—O61—C62 | −130.1 (8) |
O11—Mg1—O21—C22 | −126.4 (9) | O71—Mg2—O61—C62 | 48.8 (8) |
Br1—Mg1—O21—C22 | −37.5 (9) | Br4—Mg2—O61—C62 | 138.0 (8) |
Br2—Mg1—O21—C22 | 141.3 (9) | Br3—Mg2—O61—C62 | −40.4 (8) |
O31—Mg1—O21—C25 | −130.9 (10) | O51—Mg2—O61—C65 | 57.6 (8) |
O11—Mg1—O21—C25 | 49.8 (10) | O71—Mg2—O61—C65 | −123.5 (8) |
Br1—Mg1—O21—C25 | 138.6 (9) | Br4—Mg2—O61—C65 | −34.4 (8) |
Br2—Mg1—O21—C25 | −42.5 (10) | Br3—Mg2—O61—C65 | 147.2 (8) |
C25—O21—C22—C23 | 28.9 (13) | C65—O61—C62—C63 | 23.8 (11) |
Mg1—O21—C22—C23 | −154.2 (8) | Mg2—O61—C62—C63 | −149.6 (7) |
O21—C22—C23—C24 | −10.5 (14) | O61—C62—C63—C64 | −36.1 (11) |
C22—C23—C24—C25 | −13.2 (16) | C62—C63—C64—C65 | 35.2 (11) |
C23—C24—C25—O21 | 31.9 (16) | C62—O61—C65—C64 | −1.2 (12) |
C22—O21—C25—C24 | −39.0 (14) | Mg2—O61—C65—C64 | 172.1 (7) |
Mg1—O21—C25—C24 | 144.2 (10) | C63—C64—C65—O61 | −21.7 (12) |
O41—Mg1—O31—C32 | −132.2 (10) | O81—Mg2—O71—C72 | −129.7 (8) |
O21—Mg1—O31—C32 | 45.9 (10) | O61—Mg2—O71—C72 | 52.3 (8) |
Br1—Mg1—O31—C32 | 139.4 (10) | Br4—Mg2—O71—C72 | −39.0 (8) |
Br2—Mg1—O31—C32 | −44.0 (10) | Br3—Mg2—O71—C72 | 141.3 (8) |
O41—Mg1—O31—C35 | 47.7 (9) | O81—Mg2—O71—C75 | 54.1 (9) |
O21—Mg1—O31—C35 | −134.3 (9) | O61—Mg2—O71—C75 | −124.0 (9) |
Br1—Mg1—O31—C35 | −40.8 (9) | Br4—Mg2—O71—C75 | 144.7 (9) |
Br2—Mg1—O31—C35 | 135.8 (9) | Br3—Mg2—O71—C75 | −35.0 (9) |
C35—O31—C32—C33 | −39.6 (14) | C75—O71—C72—C73 | 22.4 (13) |
Mg1—O31—C32—C33 | 140.2 (10) | Mg2—O71—C72—C73 | −154.5 (9) |
O31—C32—C33—C34 | 33.6 (15) | O71—C72—C73—C74 | −38.5 (13) |
C32—C33—C34—C35 | −16.5 (16) | C72—C73—C74—C75 | 40.5 (13) |
C32—O31—C35—C34 | 28.2 (13) | C72—O71—C75—C74 | 4.5 (14) |
Mg1—O31—C35—C34 | −151.7 (8) | Mg2—O71—C75—C74 | −178.8 (8) |
C33—C34—C35—O31 | −6.5 (15) | C73—C74—C75—O71 | −28.9 (14) |
O31—Mg1—O41—C42 | 49.4 (13) | O51—Mg2—O81—C85 | −129.2 (10) |
O11—Mg1—O41—C42 | −131.2 (13) | O71—Mg2—O81—C85 | 51.8 (10) |
Br1—Mg1—O41—C42 | 139.8 (13) | Br4—Mg2—O81—C85 | −37.3 (10) |
Br2—Mg1—O41—C42 | −38.9 (13) | Br3—Mg2—O81—C85 | 141.1 (9) |
O31—Mg1—O41—C45 | −136.0 (10) | O51—Mg2—O81—C82 | 38.9 (9) |
O11—Mg1—O41—C45 | 43.5 (10) | O71—Mg2—O81—C82 | −140.0 (9) |
Br1—Mg1—O41—C45 | −45.5 (10) | Br4—Mg2—O81—C82 | 130.8 (9) |
Br2—Mg1—O41—C45 | 135.7 (10) | Br3—Mg2—O81—C82 | −50.8 (9) |
C45—O41—C42—C43 | −13 (2) | C85—O81—C82—C83 | −42.3 (13) |
Mg1—O41—C42—C43 | 162.2 (11) | Mg2—O81—C82—C83 | 147.2 (9) |
O41—C42—C43—C44 | −1 (2) | O81—C82—C83—C84 | 28.6 (15) |
C42—C43—C44—C45 | 15 (2) | C82—C83—C84—C85 | −5.4 (16) |
C43—C44—C45—O41 | −22.8 (17) | C82—O81—C85—C84 | 39.5 (13) |
C42—O41—C45—C44 | 22.1 (17) | Mg2—O81—C85—C84 | −150.7 (8) |
Mg1—O41—C45—C44 | −153.4 (10) | C83—C84—C85—O81 | −19.9 (15) |
Coordinates of the Mg atoms in the unit cell of (I). topAtom | x | y | z |
Mg1 | 0.5332 (4) | 0.2517 (2) | 0.2364 (2) |
Mg2 | 0.5228 (4) | 0.2559 (2) | 0.7201 (2) |
Mg1i | 0.4668 (4) | 0.7483 (2) | 0.7636 (2) |
Mg2i | 0.4772 (4) | 0.7441 (2) | 0.2799 (2) |
Symmetry operator (i) 1-x, 1-y, 1-z. |