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The title compound, [Mg(C7H5S2)2(C4H8O)2], was obtained by the reaction of PhMgBr with an excess of CS2. The magnesium(II) cation is six-coordinated by two dithio­benzoate ligands coordinating through their S atoms in a bidentate chelating fashion and two O atoms from two tetra­hydro­furan ligands, in a distorted octa­hedral geometry.

Supporting information

cif

Crystallographic Information File (CIF) https://doi.org/10.1107/S1600536806030339/ci2115sup1.cif
Contains datablocks global, I

hkl

Structure factor file (CIF format) https://doi.org/10.1107/S1600536806030339/ci2115Isup2.hkl
Contains datablock I

CCDC reference: 620740

Key indicators

  • Single-crystal X-ray study
  • T = 120 K
  • Mean [sigma](C-C) = 0.005 Å
  • R factor = 0.040
  • wR factor = 0.097
  • Data-to-parameter ratio = 16.0

checkCIF/PLATON results

No syntax errors found



Alert level B PLAT241_ALERT_2_B Check High Ueq as Compared to Neighbors for C19
Alert level C PLAT220_ALERT_2_C Large Non-Solvent C Ueq(max)/Ueq(min) ... 2.55 Ratio PLAT241_ALERT_2_C Check High Ueq as Compared to Neighbors for C16 PLAT242_ALERT_2_C Check Low Ueq as Compared to Neighbors for O2 PLAT340_ALERT_3_C Low Bond Precision on C-C bonds (x 1000) Ang ... 5 PLAT360_ALERT_2_C Short C(sp3)-C(sp3) Bond C19 - C20 ... 1.41 Ang.
0 ALERT level A = In general: serious problem 1 ALERT level B = Potentially serious problem 5 ALERT level C = Check and explain 0 ALERT level G = General alerts; check 0 ALERT type 1 CIF construction/syntax error, inconsistent or missing data 5 ALERT type 2 Indicator that the structure model may be wrong or deficient 1 ALERT type 3 Indicator that the structure quality may be low 0 ALERT type 4 Improvement, methodology, query or suggestion 0 ALERT type 5 Informative message, check

Computing details top

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).

Bis(dithiobenzoato-κ2S,S')bis(tetrahydrofuran-κO)magnesium(II) top
Crystal data top
[Mg(C7H5S2)2(C4H8O)2]F(000) = 1000
Mr = 474.98Dx = 1.306 Mg m3
Monoclinic, P21/nMo Kα radiation, λ = 0.71073 Å
Hall symbol: -P 2ynCell parameters from 8000 reflections
a = 8.3846 (9) Åθ = 1.5–26°
b = 14.3899 (9) ŵ = 0.44 mm1
c = 20.0275 (15) ÅT = 120 K
β = 90.287 (11)°Block, red–orange
V = 2416.4 (4) Å30.55 × 0.45 × 0.3 mm
Z = 4
Data collection top
Stoe IPDS
diffractometer
2373 reflections with I > 2σ(I)
φ scansRint = 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 = 0.876h = 79
10590 measured reflectionsk = 1717
4201 independent reflectionsl = 2323
Refinement top
Refinement on F20 restraints
Least-squares matrix: fullH-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 = 0.85Δρmax = 0.31 e Å3
4201 reflectionsΔρmin = 0.19 e Å3
262 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.

Fractional atomic coordinates and isotropic or equivalent isotropic displacement parameters (Å2) top
xyzUiso*/Ueq
C10.3212 (3)0.35213 (19)0.06803 (13)0.0463 (7)
C20.3600 (4)0.27971 (19)0.01766 (13)0.0476 (7)
C30.3342 (4)0.1864 (2)0.03151 (16)0.0623 (9)
H30.29520.16910.07420.075*
C40.3637 (5)0.1189 (2)0.01497 (19)0.0760 (11)
H40.34250.05560.00470.091*
C50.4237 (5)0.1423 (3)0.07621 (19)0.0791 (11)
H50.44470.09560.10850.095*
C60.4533 (6)0.2339 (3)0.09049 (17)0.0861 (12)
H60.49680.25010.13260.103*
C70.4207 (5)0.3032 (2)0.04436 (15)0.0690 (10)
H70.43990.36650.05520.083*
C80.4361 (4)0.54025 (19)0.27621 (13)0.0513 (8)
C90.5488 (4)0.5613 (2)0.33166 (14)0.0535 (8)
C100.4968 (5)0.5623 (3)0.39717 (16)0.0743 (10)
H100.39050.54450.40730.089*
C110.6002 (6)0.5892 (3)0.44820 (17)0.0899 (13)
H110.56270.59080.49290.108*
C120.7543 (6)0.6134 (3)0.4353 (2)0.0827 (11)
H120.82220.63430.47030.099*
C130.8100 (5)0.6072 (3)0.3717 (2)0.0852 (11)
H130.91860.62080.36270.102*
C140.7088 (5)0.5812 (2)0.32028 (17)0.0730 (10)
H140.74940.57680.27620.088*
C150.1283 (5)0.4530 (3)0.11636 (17)0.0815 (11)
H15A0.07260.45910.07310.098*
H15B0.19580.50860.12310.098*
C160.2249 (6)0.3690 (3)0.1173 (2)0.1140 (17)
H16A0.17610.31930.090.137*
H16B0.33420.38130.10070.137*
C170.2257 (6)0.3432 (3)0.1905 (2)0.1066 (15)
H17A0.31150.37660.21440.128*
H17B0.24170.27550.19620.128*
C180.0682 (5)0.3715 (3)0.21545 (19)0.0930 (13)
H18A0.0760.39570.26160.112*
H18B0.00650.31820.21520.112*
C190.0721 (7)0.6857 (3)0.19979 (19)0.1181 (19)
H19A0.00030.6530.23110.142*
H19B0.16680.70720.22510.142*
C200.0076 (7)0.7623 (3)0.1711 (2)0.1102 (16)
H20A0.01870.82020.19560.132*
H20B0.12450.7530.17220.132*
C210.0488 (7)0.7673 (3)0.1026 (2)0.1101 (17)
H21A0.1380.8120.0990.132*
H21B0.03830.78730.07230.132*
C220.1031 (6)0.6718 (3)0.08529 (16)0.0914 (14)
H22A0.02350.64030.05640.11*
H22B0.20620.6740.06140.11*
S10.27312 (11)0.46031 (5)0.04190 (3)0.0543 (2)
S20.32480 (12)0.32459 (6)0.14979 (4)0.0616 (2)
S30.49202 (11)0.56067 (6)0.19715 (4)0.0640 (3)
S40.25183 (11)0.49763 (7)0.29300 (4)0.0648 (3)
O10.0142 (3)0.44346 (15)0.17040 (10)0.0663 (6)
O20.1202 (3)0.62366 (14)0.14753 (9)0.0603 (6)
Mg10.21656 (13)0.49314 (7)0.16523 (4)0.0519 (3)
Atomic displacement parameters (Å2) top
U11U22U33U12U13U23
C10.0427 (19)0.0525 (17)0.0435 (15)0.0059 (14)0.0033 (13)0.0046 (13)
C20.0439 (19)0.0510 (17)0.0479 (16)0.0007 (14)0.0068 (13)0.0013 (14)
C30.062 (2)0.057 (2)0.068 (2)0.0053 (17)0.0003 (17)0.0010 (17)
C40.081 (3)0.056 (2)0.091 (3)0.0060 (19)0.001 (2)0.011 (2)
C50.092 (3)0.069 (3)0.076 (2)0.009 (2)0.005 (2)0.021 (2)
C60.121 (4)0.082 (3)0.056 (2)0.006 (2)0.015 (2)0.0072 (19)
C70.102 (3)0.056 (2)0.0493 (18)0.0002 (19)0.0099 (18)0.0006 (15)
C80.059 (2)0.0499 (17)0.0452 (16)0.0007 (15)0.0017 (14)0.0006 (13)
C90.059 (2)0.0547 (18)0.0466 (17)0.0080 (16)0.0072 (15)0.0038 (14)
C100.064 (3)0.105 (3)0.0536 (19)0.016 (2)0.0033 (17)0.0166 (19)
C110.092 (4)0.125 (3)0.052 (2)0.016 (3)0.012 (2)0.025 (2)
C120.080 (3)0.086 (3)0.081 (3)0.000 (2)0.032 (2)0.006 (2)
C130.077 (3)0.097 (3)0.081 (3)0.018 (2)0.018 (2)0.010 (2)
C140.070 (3)0.086 (3)0.063 (2)0.014 (2)0.0059 (19)0.0004 (18)
C150.062 (3)0.116 (3)0.066 (2)0.011 (2)0.0071 (18)0.018 (2)
C160.122 (4)0.136 (4)0.084 (3)0.065 (3)0.017 (3)0.007 (3)
C170.097 (4)0.114 (3)0.109 (3)0.044 (3)0.006 (3)0.024 (3)
C180.083 (3)0.109 (3)0.087 (3)0.022 (3)0.003 (2)0.045 (2)
C190.206 (6)0.085 (3)0.063 (2)0.050 (3)0.030 (3)0.008 (2)
C200.151 (5)0.097 (3)0.082 (3)0.042 (3)0.012 (3)0.007 (2)
C210.163 (5)0.080 (3)0.087 (3)0.033 (3)0.016 (3)0.016 (2)
C220.143 (4)0.078 (3)0.054 (2)0.019 (3)0.002 (2)0.0079 (19)
S10.0742 (6)0.0519 (4)0.0367 (4)0.0020 (4)0.0005 (3)0.0057 (3)
S20.0801 (7)0.0623 (5)0.0425 (4)0.0022 (5)0.0044 (4)0.0120 (4)
S30.0650 (6)0.0822 (6)0.0447 (4)0.0126 (5)0.0046 (4)0.0011 (4)
S40.0618 (6)0.0942 (6)0.0385 (4)0.0116 (5)0.0002 (4)0.0050 (4)
O10.0643 (16)0.0811 (15)0.0533 (12)0.0173 (12)0.0073 (11)0.0222 (11)
O20.0812 (17)0.0600 (13)0.0397 (10)0.0057 (11)0.0022 (10)0.0015 (9)
Mg10.0603 (7)0.0599 (6)0.0355 (5)0.0036 (5)0.0008 (4)0.0034 (4)
Geometric parameters (Å, º) top
C1—C21.487 (4)C15—H15A0.99
C1—S21.685 (3)C15—H15B0.99
C1—S11.690 (3)C16—C171.512 (5)
C2—C71.387 (4)C16—H16A0.99
C2—C31.388 (4)C16—H16B0.99
C3—C41.370 (4)C17—C181.468 (6)
C3—H30.95C17—H17A0.99
C4—C51.370 (5)C17—H17B0.99
C4—H40.95C18—O11.448 (4)
C5—C61.371 (5)C18—H18A0.99
C5—H50.95C18—H18B0.99
C6—C71.388 (4)C19—C201.410 (5)
C6—H60.95C19—O21.435 (4)
C7—H70.95C19—H19A0.99
C8—C91.486 (4)C19—H19B0.99
C8—S31.679 (3)C20—C211.455 (5)
C8—S41.698 (3)C20—H20A0.99
C9—C101.385 (4)C20—H20B0.99
C9—C141.391 (5)C21—C221.490 (5)
C10—C111.392 (5)C21—H21A0.99
C10—H100.95C21—H21B0.99
C11—C121.364 (5)C22—O21.432 (4)
C11—H110.95C22—H22A0.99
C12—C131.361 (5)C22—H22B0.99
C12—H120.95S1—Mg12.5614 (11)
C13—C141.383 (5)S2—Mg12.6086 (13)
C13—H130.95S3—Mg12.5831 (14)
C14—H140.95S4—Mg12.5753 (11)
C15—O11.447 (4)O1—Mg12.065 (2)
C15—C161.455 (5)O2—Mg12.074 (2)
C2—C1—S2119.4 (2)C16—C17—H17B110.8
C2—C1—S1119.20 (19)H17A—C17—H17B108.9
S2—C1—S1121.37 (16)O1—C18—C17105.7 (3)
C7—C2—C3118.2 (3)O1—C18—H18A110.6
C7—C2—C1121.3 (3)C17—C18—H18A110.6
C3—C2—C1120.5 (2)O1—C18—H18B110.6
C4—C3—C2121.5 (3)C17—C18—H18B110.6
C4—C3—H3119.3H18A—C18—H18B108.7
C2—C3—H3119.3C20—C19—O2108.9 (3)
C3—C4—C5120.1 (3)C20—C19—H19A109.9
C3—C4—H4119.9O2—C19—H19A109.9
C5—C4—H4119.9C20—C19—H19B109.9
C4—C5—C6119.4 (3)O2—C19—H19B109.9
C4—C5—H5120.3H19A—C19—H19B108.3
C6—C5—H5120.3C19—C20—C21105.5 (4)
C5—C6—C7121.0 (3)C19—C20—H20A110.7
C5—C6—H6119.5C21—C20—H20A110.7
C7—C6—H6119.5C19—C20—H20B110.7
C2—C7—C6119.7 (3)C21—C20—H20B110.7
C2—C7—H7120.2H20A—C20—H20B108.8
C6—C7—H7120.2C20—C21—C22106.0 (3)
C9—C8—S3119.3 (2)C20—C21—H21A110.5
C9—C8—S4120.1 (2)C22—C21—H21A110.5
S3—C8—S4120.57 (19)C20—C21—H21B110.5
C10—C9—C14117.5 (3)C22—C21—H21B110.5
C10—C9—C8120.5 (3)H21A—C21—H21B108.7
C14—C9—C8122.0 (3)O2—C22—C21105.8 (3)
C9—C10—C11120.0 (4)O2—C22—H22A110.6
C9—C10—H10120C21—C22—H22A110.6
C11—C10—H10120O2—C22—H22B110.6
C12—C11—C10121.3 (4)C21—C22—H22B110.6
C12—C11—H11119.4H22A—C22—H22B108.7
C10—C11—H11119.4C1—S1—Mg185.20 (9)
C11—C12—C13119.3 (4)C1—S2—Mg183.80 (10)
C11—C12—H12120.3C8—S3—Mg185.07 (12)
C13—C12—H12120.3C8—S4—Mg184.97 (10)
C12—C13—C14120.2 (4)C15—O1—C18109.0 (3)
C12—C13—H13119.9C15—O1—Mg1123.07 (18)
C14—C13—H13119.9C18—O1—Mg1125.1 (2)
C13—C14—C9121.5 (3)C22—O2—C19107.9 (3)
C13—C14—H14119.3C22—O2—Mg1128.57 (18)
C9—C14—H14119.3C19—O2—Mg1123.3 (2)
O1—C15—C16106.1 (3)O1—Mg1—O287.59 (10)
O1—C15—H15A110.5O1—Mg1—S199.35 (7)
C16—C15—H15A110.5O2—Mg1—S194.35 (6)
O1—C15—H15B110.5O1—Mg1—S493.55 (7)
C16—C15—H15B110.5O2—Mg1—S4100.94 (6)
H15A—C15—H15B108.7S1—Mg1—S4160.38 (5)
C15—C16—C17102.8 (3)O1—Mg1—S3162.61 (7)
C15—C16—H16A111.2O2—Mg1—S392.78 (8)
C17—C16—H16A111.2S1—Mg1—S397.95 (4)
C15—C16—H16B111.2S4—Mg1—S369.30 (4)
C17—C16—H16B111.2O1—Mg1—S290.61 (8)
H16A—C16—H16B109.1O2—Mg1—S2163.13 (7)
C18—C17—C16104.7 (3)S1—Mg1—S269.39 (3)
C18—C17—H17A110.8S4—Mg1—S295.91 (4)
C16—C17—H17A110.8S3—Mg1—S293.90 (5)
C18—C17—H17B110.8
 

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