Supporting information
Crystallographic Information File (CIF) https://doi.org/10.1107/S1600536806030339/ci2115sup1.cif | |
Structure factor file (CIF format) https://doi.org/10.1107/S1600536806030339/ci2115Isup2.hkl |
CCDC reference: 620740
Data collection: IPDS Software (Stoe & Cie, 1997); cell refinement: IPDS Software; data reduction: X-RED (Stoe & Cie, 1997); program(s) used to solve structure: SHELXS97 (Sheldrick, 1997); program(s) used to refine structure: SHELXL97 (Sheldrick, 1997); molecular graphics: ORTEP-3 for Windows (Farrugia, 1997); software used to prepare material for publication: WinGX (Farrugia, 1999).
[Mg(C7H5S2)2(C4H8O)2] | F(000) = 1000 |
Mr = 474.98 | Dx = 1.306 Mg m−3 |
Monoclinic, P21/n | Mo Kα radiation, λ = 0.71073 Å |
Hall symbol: -P 2yn | Cell parameters from 8000 reflections |
a = 8.3846 (9) Å | θ = 1.5–26° |
b = 14.3899 (9) Å | µ = 0.44 mm−1 |
c = 20.0275 (15) Å | T = 120 K |
β = 90.287 (11)° | Block, red–orange |
V = 2416.4 (4) Å3 | 0.55 × 0.45 × 0.3 mm |
Z = 4 |
Stoe IPDS diffractometer | 2373 reflections with I > 2σ(I) |
φ scans | Rint = 0.039 |
Absorption correction: numerical [X-RED32 (Stoe & Cie, 1997); crystal shape approximated by a polyhedron with 13 faces] | θmax = 25.1°, θmin = 2.5° |
Tmin = 0.781, Tmax = 0.876 | h = −7→9 |
10590 measured reflections | k = −17→17 |
4201 independent reflections | l = −23→23 |
Refinement on F2 | 0 restraints |
Least-squares matrix: full | H-atom parameters constrained |
R[F2 > 2σ(F2)] = 0.040 | w = 1/[σ2(Fo2) + (0.0526P)2] where P = (Fo2 + 2Fc2)/3 |
wR(F2) = 0.097 | (Δ/σ)max < 0.001 |
S = 0.85 | Δρmax = 0.31 e Å−3 |
4201 reflections | Δρmin = −0.19 e Å−3 |
262 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. |
x | y | z | Uiso*/Ueq | ||
C1 | 0.3212 (3) | 0.35213 (19) | 0.06803 (13) | 0.0463 (7) | |
C2 | 0.3600 (4) | 0.27971 (19) | 0.01766 (13) | 0.0476 (7) | |
C3 | 0.3342 (4) | 0.1864 (2) | 0.03151 (16) | 0.0623 (9) | |
H3 | 0.2952 | 0.1691 | 0.0742 | 0.075* | |
C4 | 0.3637 (5) | 0.1189 (2) | −0.01497 (19) | 0.0760 (11) | |
H4 | 0.3425 | 0.0556 | −0.0047 | 0.091* | |
C5 | 0.4237 (5) | 0.1423 (3) | −0.07621 (19) | 0.0791 (11) | |
H5 | 0.4447 | 0.0956 | −0.1085 | 0.095* | |
C6 | 0.4533 (6) | 0.2339 (3) | −0.09049 (17) | 0.0861 (12) | |
H6 | 0.4968 | 0.2501 | −0.1326 | 0.103* | |
C7 | 0.4207 (5) | 0.3032 (2) | −0.04436 (15) | 0.0690 (10) | |
H7 | 0.4399 | 0.3665 | −0.0552 | 0.083* | |
C8 | 0.4361 (4) | 0.54025 (19) | 0.27621 (13) | 0.0513 (8) | |
C9 | 0.5488 (4) | 0.5613 (2) | 0.33166 (14) | 0.0535 (8) | |
C10 | 0.4968 (5) | 0.5623 (3) | 0.39717 (16) | 0.0743 (10) | |
H10 | 0.3905 | 0.5445 | 0.4073 | 0.089* | |
C11 | 0.6002 (6) | 0.5892 (3) | 0.44820 (17) | 0.0899 (13) | |
H11 | 0.5627 | 0.5908 | 0.4929 | 0.108* | |
C12 | 0.7543 (6) | 0.6134 (3) | 0.4353 (2) | 0.0827 (11) | |
H12 | 0.8222 | 0.6343 | 0.4703 | 0.099* | |
C13 | 0.8100 (5) | 0.6072 (3) | 0.3717 (2) | 0.0852 (11) | |
H13 | 0.9186 | 0.6208 | 0.3627 | 0.102* | |
C14 | 0.7088 (5) | 0.5812 (2) | 0.32028 (17) | 0.0730 (10) | |
H14 | 0.7494 | 0.5768 | 0.2762 | 0.088* | |
C15 | −0.1283 (5) | 0.4530 (3) | 0.11636 (17) | 0.0815 (11) | |
H15A | −0.0726 | 0.4591 | 0.0731 | 0.098* | |
H15B | −0.1958 | 0.5086 | 0.1231 | 0.098* | |
C16 | −0.2249 (6) | 0.3690 (3) | 0.1173 (2) | 0.1140 (17) | |
H16A | −0.1761 | 0.3193 | 0.09 | 0.137* | |
H16B | −0.3342 | 0.3813 | 0.1007 | 0.137* | |
C17 | −0.2257 (6) | 0.3432 (3) | 0.1905 (2) | 0.1066 (15) | |
H17A | −0.3115 | 0.3766 | 0.2144 | 0.128* | |
H17B | −0.2417 | 0.2755 | 0.1962 | 0.128* | |
C18 | −0.0682 (5) | 0.3715 (3) | 0.21545 (19) | 0.0930 (13) | |
H18A | −0.076 | 0.3957 | 0.2616 | 0.112* | |
H18B | 0.0065 | 0.3182 | 0.2152 | 0.112* | |
C19 | 0.0721 (7) | 0.6857 (3) | 0.19979 (19) | 0.1181 (19) | |
H19A | 0.0003 | 0.653 | 0.2311 | 0.142* | |
H19B | 0.1668 | 0.7072 | 0.2251 | 0.142* | |
C20 | −0.0076 (7) | 0.7623 (3) | 0.1711 (2) | 0.1102 (16) | |
H20A | 0.0187 | 0.8202 | 0.1956 | 0.132* | |
H20B | −0.1245 | 0.753 | 0.1722 | 0.132* | |
C21 | 0.0488 (7) | 0.7673 (3) | 0.1026 (2) | 0.1101 (17) | |
H21A | 0.138 | 0.812 | 0.099 | 0.132* | |
H21B | −0.0383 | 0.7873 | 0.0723 | 0.132* | |
C22 | 0.1031 (6) | 0.6718 (3) | 0.08529 (16) | 0.0914 (14) | |
H22A | 0.0235 | 0.6403 | 0.0564 | 0.11* | |
H22B | 0.2062 | 0.674 | 0.0614 | 0.11* | |
S1 | 0.27312 (11) | 0.46031 (5) | 0.04190 (3) | 0.0543 (2) | |
S2 | 0.32480 (12) | 0.32459 (6) | 0.14979 (4) | 0.0616 (2) | |
S3 | 0.49202 (11) | 0.56067 (6) | 0.19715 (4) | 0.0640 (3) | |
S4 | 0.25183 (11) | 0.49763 (7) | 0.29300 (4) | 0.0648 (3) | |
O1 | −0.0142 (3) | 0.44346 (15) | 0.17040 (10) | 0.0663 (6) | |
O2 | 0.1202 (3) | 0.62366 (14) | 0.14753 (9) | 0.0603 (6) | |
Mg1 | 0.21656 (13) | 0.49314 (7) | 0.16523 (4) | 0.0519 (3) |
U11 | U22 | U33 | U12 | U13 | U23 | |
C1 | 0.0427 (19) | 0.0525 (17) | 0.0435 (15) | −0.0059 (14) | −0.0033 (13) | 0.0046 (13) |
C2 | 0.0439 (19) | 0.0510 (17) | 0.0479 (16) | −0.0007 (14) | −0.0068 (13) | 0.0013 (14) |
C3 | 0.062 (2) | 0.057 (2) | 0.068 (2) | −0.0053 (17) | 0.0003 (17) | 0.0010 (17) |
C4 | 0.081 (3) | 0.056 (2) | 0.091 (3) | −0.0060 (19) | −0.001 (2) | −0.011 (2) |
C5 | 0.092 (3) | 0.069 (3) | 0.076 (2) | 0.009 (2) | −0.005 (2) | −0.021 (2) |
C6 | 0.121 (4) | 0.082 (3) | 0.056 (2) | 0.006 (2) | 0.015 (2) | −0.0072 (19) |
C7 | 0.102 (3) | 0.056 (2) | 0.0493 (18) | 0.0002 (19) | 0.0099 (18) | −0.0006 (15) |
C8 | 0.059 (2) | 0.0499 (17) | 0.0452 (16) | 0.0007 (15) | 0.0017 (14) | 0.0006 (13) |
C9 | 0.059 (2) | 0.0547 (18) | 0.0466 (17) | 0.0080 (16) | −0.0072 (15) | −0.0038 (14) |
C10 | 0.064 (3) | 0.105 (3) | 0.0536 (19) | 0.016 (2) | −0.0033 (17) | −0.0166 (19) |
C11 | 0.092 (4) | 0.125 (3) | 0.052 (2) | 0.016 (3) | −0.012 (2) | −0.025 (2) |
C12 | 0.080 (3) | 0.086 (3) | 0.081 (3) | 0.000 (2) | −0.032 (2) | −0.006 (2) |
C13 | 0.077 (3) | 0.097 (3) | 0.081 (3) | −0.018 (2) | −0.018 (2) | 0.010 (2) |
C14 | 0.070 (3) | 0.086 (3) | 0.063 (2) | −0.014 (2) | −0.0059 (19) | −0.0004 (18) |
C15 | 0.062 (3) | 0.116 (3) | 0.066 (2) | −0.011 (2) | −0.0071 (18) | 0.018 (2) |
C16 | 0.122 (4) | 0.136 (4) | 0.084 (3) | −0.065 (3) | −0.017 (3) | 0.007 (3) |
C17 | 0.097 (4) | 0.114 (3) | 0.109 (3) | −0.044 (3) | −0.006 (3) | 0.024 (3) |
C18 | 0.083 (3) | 0.109 (3) | 0.087 (3) | −0.022 (3) | 0.003 (2) | 0.045 (2) |
C19 | 0.206 (6) | 0.085 (3) | 0.063 (2) | 0.050 (3) | 0.030 (3) | −0.008 (2) |
C20 | 0.151 (5) | 0.097 (3) | 0.082 (3) | 0.042 (3) | 0.012 (3) | −0.007 (2) |
C21 | 0.163 (5) | 0.080 (3) | 0.087 (3) | 0.033 (3) | 0.016 (3) | 0.016 (2) |
C22 | 0.143 (4) | 0.078 (3) | 0.054 (2) | 0.019 (3) | 0.002 (2) | 0.0079 (19) |
S1 | 0.0742 (6) | 0.0519 (4) | 0.0367 (4) | 0.0020 (4) | 0.0005 (3) | 0.0057 (3) |
S2 | 0.0801 (7) | 0.0623 (5) | 0.0425 (4) | 0.0022 (5) | −0.0044 (4) | 0.0120 (4) |
S3 | 0.0650 (6) | 0.0822 (6) | 0.0447 (4) | −0.0126 (5) | 0.0046 (4) | 0.0011 (4) |
S4 | 0.0618 (6) | 0.0942 (6) | 0.0385 (4) | −0.0116 (5) | 0.0002 (4) | 0.0050 (4) |
O1 | 0.0643 (16) | 0.0811 (15) | 0.0533 (12) | −0.0173 (12) | −0.0073 (11) | 0.0222 (11) |
O2 | 0.0812 (17) | 0.0600 (13) | 0.0397 (10) | 0.0057 (11) | 0.0022 (10) | −0.0015 (9) |
Mg1 | 0.0603 (7) | 0.0599 (6) | 0.0355 (5) | −0.0036 (5) | −0.0008 (4) | 0.0034 (4) |
C1—C2 | 1.487 (4) | C15—H15A | 0.99 |
C1—S2 | 1.685 (3) | C15—H15B | 0.99 |
C1—S1 | 1.690 (3) | C16—C17 | 1.512 (5) |
C2—C7 | 1.387 (4) | C16—H16A | 0.99 |
C2—C3 | 1.388 (4) | C16—H16B | 0.99 |
C3—C4 | 1.370 (4) | C17—C18 | 1.468 (6) |
C3—H3 | 0.95 | C17—H17A | 0.99 |
C4—C5 | 1.370 (5) | C17—H17B | 0.99 |
C4—H4 | 0.95 | C18—O1 | 1.448 (4) |
C5—C6 | 1.371 (5) | C18—H18A | 0.99 |
C5—H5 | 0.95 | C18—H18B | 0.99 |
C6—C7 | 1.388 (4) | C19—C20 | 1.410 (5) |
C6—H6 | 0.95 | C19—O2 | 1.435 (4) |
C7—H7 | 0.95 | C19—H19A | 0.99 |
C8—C9 | 1.486 (4) | C19—H19B | 0.99 |
C8—S3 | 1.679 (3) | C20—C21 | 1.455 (5) |
C8—S4 | 1.698 (3) | C20—H20A | 0.99 |
C9—C10 | 1.385 (4) | C20—H20B | 0.99 |
C9—C14 | 1.391 (5) | C21—C22 | 1.490 (5) |
C10—C11 | 1.392 (5) | C21—H21A | 0.99 |
C10—H10 | 0.95 | C21—H21B | 0.99 |
C11—C12 | 1.364 (5) | C22—O2 | 1.432 (4) |
C11—H11 | 0.95 | C22—H22A | 0.99 |
C12—C13 | 1.361 (5) | C22—H22B | 0.99 |
C12—H12 | 0.95 | S1—Mg1 | 2.5614 (11) |
C13—C14 | 1.383 (5) | S2—Mg1 | 2.6086 (13) |
C13—H13 | 0.95 | S3—Mg1 | 2.5831 (14) |
C14—H14 | 0.95 | S4—Mg1 | 2.5753 (11) |
C15—O1 | 1.447 (4) | O1—Mg1 | 2.065 (2) |
C15—C16 | 1.455 (5) | O2—Mg1 | 2.074 (2) |
C2—C1—S2 | 119.4 (2) | C16—C17—H17B | 110.8 |
C2—C1—S1 | 119.20 (19) | H17A—C17—H17B | 108.9 |
S2—C1—S1 | 121.37 (16) | O1—C18—C17 | 105.7 (3) |
C7—C2—C3 | 118.2 (3) | O1—C18—H18A | 110.6 |
C7—C2—C1 | 121.3 (3) | C17—C18—H18A | 110.6 |
C3—C2—C1 | 120.5 (2) | O1—C18—H18B | 110.6 |
C4—C3—C2 | 121.5 (3) | C17—C18—H18B | 110.6 |
C4—C3—H3 | 119.3 | H18A—C18—H18B | 108.7 |
C2—C3—H3 | 119.3 | C20—C19—O2 | 108.9 (3) |
C3—C4—C5 | 120.1 (3) | C20—C19—H19A | 109.9 |
C3—C4—H4 | 119.9 | O2—C19—H19A | 109.9 |
C5—C4—H4 | 119.9 | C20—C19—H19B | 109.9 |
C4—C5—C6 | 119.4 (3) | O2—C19—H19B | 109.9 |
C4—C5—H5 | 120.3 | H19A—C19—H19B | 108.3 |
C6—C5—H5 | 120.3 | C19—C20—C21 | 105.5 (4) |
C5—C6—C7 | 121.0 (3) | C19—C20—H20A | 110.7 |
C5—C6—H6 | 119.5 | C21—C20—H20A | 110.7 |
C7—C6—H6 | 119.5 | C19—C20—H20B | 110.7 |
C2—C7—C6 | 119.7 (3) | C21—C20—H20B | 110.7 |
C2—C7—H7 | 120.2 | H20A—C20—H20B | 108.8 |
C6—C7—H7 | 120.2 | C20—C21—C22 | 106.0 (3) |
C9—C8—S3 | 119.3 (2) | C20—C21—H21A | 110.5 |
C9—C8—S4 | 120.1 (2) | C22—C21—H21A | 110.5 |
S3—C8—S4 | 120.57 (19) | C20—C21—H21B | 110.5 |
C10—C9—C14 | 117.5 (3) | C22—C21—H21B | 110.5 |
C10—C9—C8 | 120.5 (3) | H21A—C21—H21B | 108.7 |
C14—C9—C8 | 122.0 (3) | O2—C22—C21 | 105.8 (3) |
C9—C10—C11 | 120.0 (4) | O2—C22—H22A | 110.6 |
C9—C10—H10 | 120 | C21—C22—H22A | 110.6 |
C11—C10—H10 | 120 | O2—C22—H22B | 110.6 |
C12—C11—C10 | 121.3 (4) | C21—C22—H22B | 110.6 |
C12—C11—H11 | 119.4 | H22A—C22—H22B | 108.7 |
C10—C11—H11 | 119.4 | C1—S1—Mg1 | 85.20 (9) |
C11—C12—C13 | 119.3 (4) | C1—S2—Mg1 | 83.80 (10) |
C11—C12—H12 | 120.3 | C8—S3—Mg1 | 85.07 (12) |
C13—C12—H12 | 120.3 | C8—S4—Mg1 | 84.97 (10) |
C12—C13—C14 | 120.2 (4) | C15—O1—C18 | 109.0 (3) |
C12—C13—H13 | 119.9 | C15—O1—Mg1 | 123.07 (18) |
C14—C13—H13 | 119.9 | C18—O1—Mg1 | 125.1 (2) |
C13—C14—C9 | 121.5 (3) | C22—O2—C19 | 107.9 (3) |
C13—C14—H14 | 119.3 | C22—O2—Mg1 | 128.57 (18) |
C9—C14—H14 | 119.3 | C19—O2—Mg1 | 123.3 (2) |
O1—C15—C16 | 106.1 (3) | O1—Mg1—O2 | 87.59 (10) |
O1—C15—H15A | 110.5 | O1—Mg1—S1 | 99.35 (7) |
C16—C15—H15A | 110.5 | O2—Mg1—S1 | 94.35 (6) |
O1—C15—H15B | 110.5 | O1—Mg1—S4 | 93.55 (7) |
C16—C15—H15B | 110.5 | O2—Mg1—S4 | 100.94 (6) |
H15A—C15—H15B | 108.7 | S1—Mg1—S4 | 160.38 (5) |
C15—C16—C17 | 102.8 (3) | O1—Mg1—S3 | 162.61 (7) |
C15—C16—H16A | 111.2 | O2—Mg1—S3 | 92.78 (8) |
C17—C16—H16A | 111.2 | S1—Mg1—S3 | 97.95 (4) |
C15—C16—H16B | 111.2 | S4—Mg1—S3 | 69.30 (4) |
C17—C16—H16B | 111.2 | O1—Mg1—S2 | 90.61 (8) |
H16A—C16—H16B | 109.1 | O2—Mg1—S2 | 163.13 (7) |
C18—C17—C16 | 104.7 (3) | S1—Mg1—S2 | 69.39 (3) |
C18—C17—H17A | 110.8 | S4—Mg1—S2 | 95.91 (4) |
C16—C17—H17A | 110.8 | S3—Mg1—S2 | 93.90 (5) |
C18—C17—H17B | 110.8 |