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Acta Cryst. (2009). E65, m1129    [ doi:10.1107/S1600536809031882 ]

Tetrachlorido[(diphenylphosphino)diphenylphosphine oxide-[kappa]O]zirconium(IV) benzene monosolvate

T. Ogawa, Y. Kajita and H. Masuda

Abstract top

In the title centrosymmetric mononuclear ZrIV compound, [ZrCl4{P(O)(C6H5)2P(C6H5)2}2]·C6H6, the central ZrIV ion is coordinated by two O atoms from two symmetry-related (diphenylphosphino)diphenylphosphine ligands and four Cl atoms in a distorted octahedral geometry with the four Cl atoms in the equatorial positions. The molecule lies about a center of inversion and the benzene solvent molecule about another center of inversion. The P=O bond [1.528 (2) Å] is slightly longer than a typical P=O double bond (average 1.500 ).

Comment top

The phosphinoyl derivative, (diphenylphosphino)diphenylphosphine (DPDP), has a unique structure and coordination mode (Ferguson 1990 and Muratova et al., 1980). The complex which contains DPDP ligands is very rare and is a novel ZrIV complex with DPDP ligand (Kuramshin & Khramov et al., 1983). The centrosymmetric unit of the title compound, [ZrCl4(C24H20P2O)2] C6H6, contains a neutral ZrIV complex and a solvent benzene molecule (Fig. 1). The compound crystallized in the triclinic space group P1. In the complex, the ZrIV ion is six-coordinated in a slightly distorted octahedral environment by two O atoms of DPDP ligand and four Cl ions. The P atoms do not coordinate to the ZrIV atom. The Zr—Cl(1) [2.4450 (9) Å] and Zr—Cl(2) [2.4627 (9) Å] bond lengths are slightly different each other (Table 1). The P—O bond length [1.5281 (19) Å] is slightly longer compared with a typical double bond (Berners-Price et al., 2009). The P—P bond length [2.2057 (10) Å] is similar to several PIII—PV derivatives.

Related literature top

For general background to the structure and coordination mode of (diphenylphosphino)diphenylphosphine (DPDP), see: Ferguson (1990); Kuramshin & Khramov (1983). For a ZrIV complex with a DPDP ligand, see: Muratova et al. (1980). For comparison P–O bond distances, see: Berners-Price et al. (2009).

Experimental top

The title compound was prepared by the reaction of ZrCl4 (0.03 g, 0.13 mmol) and (diphenylphosphino)diphenylphosphine (0.10 g, 0.26 mmol) in benzene (5 ml). The mixture was filtered and set aside to crystallize at ambient temperature for several days, giving colorless single crystals.

Refinement top

All H atoms were positioned geometrically and refined as riding atoms, with C—H = 0.95 Å and Uiso(H) = 1.2 Ueq(C).

The final difference Fourier map had a peak near the Zr1 atom.

Computing details top

Data collection: CrystalClear (Rigaku, 2007); cell refinement: CrystalClear (Rigaku, 2007); data reduction: CrystalStructure (Rigaku, 2007); program(s) used to solve structure: SIR92 (Altomare et al., 1994); program(s) used to refine structure: SHELXL97 (Sheldrick, 2008); molecular graphics: ORTEP-3 (Farrugia, 1997); software used to prepare material for publication: CrystalStructure (Rigaku, 2007).

Figures top
[Figure 1] Fig. 1. The molecular structure of the title molecule, with the atom-numbering scheme. Displacement ellipsoids are drawn at the 50% probability level. Primed atoms are generated by the symmetry operator ((i) -x + 2, -y, -z + 2; (ii) -x + 1, -y + 1, -z + 1).
[Figure 2] Fig. 2. A partial packing diagram of the title compound.
Tetrachlorido[(diphenylphosphino)diphenylphosphine oxide-κO]zirconium(IV) benzene monosolvate top
Crystal data top
[ZrCl4(C24H20OP2)2]·C6H6Z = 1
Mr = 1083.81F(000) = 554.00
Triclinic, P1Dx = 1.401 Mg m−3
Hall symbol: -P 1Mo Kα radiation, λ = 0.71070 Å
a = 9.6073 (3) ÅCell parameters from 3589 reflections
b = 10.1521 (4) Åθ = 3.2–27.5°
c = 14.0204 (10) ŵ = 0.59 mm−1
α = 79.027 (13)°T = 173 K
β = 87.269 (13)°Chip, colorless
γ = 73.096 (11)°0.30 × 0.15 × 0.13 mm
V = 1284.42 (11) Å3
Data collection top
Rigaku Mercury
diffractometer		4497 reflections with F2 > 2σ(F2)
Detector resolution: 7.31 pixels mm-1Rint = 0.031
ω scansθmax = 27.5°
Absorption correction: multi-scan
(Jacobson, 1998)		h = −12→12
Tmin = 0.900, Tmax = 0.927k = −11→13
10324 measured reflectionsl = −13→18
5669 independent reflections
Refinement top
Refinement on F20 restraints
R[F2 > 2σ(F2)] = 0.045H-atom parameters constrained
wR(F2) = 0.151 w = 1/[σ2(Fo2) + (0.1P)2]
where P = (Fo2 + 2Fc2)/3
S = 1.02(Δ/σ)max < 0.001
5669 reflectionsΔρmax = 1.04 e Å−3
296 parametersΔρmin = −0.81 e Å−3
Crystal data top
[ZrCl4(C24H20OP2)2]·C6H6γ = 73.096 (11)°
Mr = 1083.81V = 1284.42 (11) Å3
Triclinic, P1Z = 1
a = 9.6073 (3) ÅMo Kα radiation
b = 10.1521 (4) ŵ = 0.59 mm−1
c = 14.0204 (10) ÅT = 173 K
α = 79.027 (13)°0.30 × 0.15 × 0.13 mm
β = 87.269 (13)°
Data collection top
Rigaku Mercury
diffractometer		5669 independent reflections
Absorption correction: multi-scan
(Jacobson, 1998)		4497 reflections with F2 > 2σ(F2)
Tmin = 0.900, Tmax = 0.927Rint = 0.031
10324 measured reflectionsθmax = 27.5°
Refinement top
R[F2 > 2σ(F2)] = 0.045H-atom parameters constrained
wR(F2) = 0.151Δρmax = 1.04 e Å−3
S = 1.02Δρmin = −0.81 e Å−3
5669 reflectionsAbsolute structure: ?
296 parametersFlack parameter: ?
0 restraintsRogers parameter: ?
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 was performed using all reflections. The weighted R-factor (wR) and goodness of fit (S) are based on F2. R-factor (gt) are based on F. The threshold expression of F2 > 2.0 σ(F2) is used only for calculating R-factor (gt).

Fractional atomic coordinates and isotropic or equivalent isotropic displacement parameters (Å2) top
xyzUiso*/Ueq
Zr11010.01849 (13)
Cl11.14353 (9)0.14927 (8)1.03401 (6)0.0305 (2)
Cl20.79704 (8)0.12426 (8)1.09344 (6)0.02711 (18)
P10.79655 (8)0.24267 (8)0.80566 (5)0.01964 (17)
P20.87015 (9)0.33171 (9)0.66302 (6)0.0249 (2)
O10.9163 (2)0.1442 (2)0.87498 (15)0.0212 (4)
C10.6603 (3)0.1623 (3)0.7861 (2)0.0239 (6)
C20.6455 (4)0.1237 (4)0.6987 (2)0.0404 (9)
C30.5388 (4)0.0607 (5)0.6859 (3)0.0509 (11)
C40.4473 (4)0.0343 (4)0.7626 (2)0.0377 (8)
C50.4620 (3)0.0716 (3)0.8512 (2)0.0346 (7)
C60.5688 (3)0.1353 (3)0.8631 (2)0.0301 (7)
C70.7107 (3)0.3971 (3)0.8540 (2)0.0245 (6)
C80.5776 (3)0.4851 (3)0.8158 (2)0.0339 (7)
C90.5195 (4)0.6137 (4)0.8442 (3)0.0471 (10)
C100.5940 (4)0.6522 (4)0.9110 (3)0.0482 (10)
C110.7256 (4)0.5653 (3)0.9496 (2)0.0401 (9)
C120.7856 (3)0.4366 (3)0.9215 (2)0.0288 (7)
C130.9801 (3)0.4239 (3)0.7122 (2)0.0284 (7)
C140.9168 (4)0.5667 (3)0.7125 (2)0.0375 (8)
C150.9878 (5)0.6405 (4)0.7568 (3)0.0476 (10)
C161.1218 (5)0.5752 (4)0.7984 (3)0.0513 (11)
C171.1876 (4)0.4354 (4)0.7969 (3)0.0484 (10)
C181.1170 (4)0.3584 (4)0.7553 (2)0.0358 (8)
C191.0058 (3)0.1844 (3)0.6233 (2)0.0276 (6)
C201.0628 (5)0.2151 (4)0.5313 (3)0.0552 (12)
C211.1635 (5)0.1132 (5)0.4917 (3)0.0686 (15)
C221.2062 (4)−0.0226 (4)0.5424 (2)0.0423 (9)
C231.1486 (4)−0.0549 (4)0.6320 (2)0.0410 (9)
C241.0484 (4)0.0476 (3)0.6725 (2)0.0358 (8)
C250.4088 (12)0.5582 (15)0.5682 (6)0.165 (7)
C260.5127 (14)0.6167 (11)0.5268 (8)0.167 (5)
C270.6047 (12)0.5579 (14)0.4560 (7)0.171 (6)
H10.70900.14030.64670.049*
H20.52850.03580.62520.061*
H30.3746−0.00930.75430.045*
H40.39940.05370.90340.041*
H50.57940.16030.92370.036*
H60.52670.45730.77040.041*
H70.42920.67460.81790.056*
H80.55400.73990.93070.058*
H90.77530.59360.99540.048*
H100.87630.37650.94770.035*
H110.82470.61340.68230.045*
H120.94300.73680.75820.057*
H131.17000.62620.82850.061*
H141.28190.39140.82450.058*
H151.16160.26150.75620.043*
H161.03180.30790.49530.066*
H171.20330.13640.42960.082*
H181.2752−0.09330.51530.051*
H191.1776−0.14860.66680.049*
H201.00880.02350.73450.043*
H210.34520.60060.61480.199*
H220.52310.69820.54610.200*
H230.67560.60030.42580.205*
Atomic displacement parameters (Å2) top
U11U22U33U12U13U23
Zr10.0175 (2)0.0156 (2)0.0215 (2)−0.00302 (15)0.00179 (15)−0.00429 (15)
Cl10.0292 (4)0.0249 (3)0.0416 (4)−0.0116 (3)−0.0023 (3)−0.0096 (3)
Cl20.0237 (3)0.0243 (3)0.0309 (4)−0.0023 (3)0.0078 (3)−0.0082 (3)
P10.0202 (3)0.0174 (3)0.0200 (3)−0.0032 (2)0.0018 (2)−0.0041 (2)
P20.0277 (4)0.0234 (4)0.0211 (3)−0.0051 (3)0.0007 (3)−0.0013 (3)
O10.0228 (10)0.0185 (9)0.0204 (10)−0.0038 (8)−0.0003 (8)−0.0020 (8)
C10.0240 (14)0.0194 (14)0.0268 (15)−0.0042 (12)0.0027 (12)−0.0045 (12)
C20.043 (2)0.063 (2)0.0286 (17)−0.032 (2)0.0102 (15)−0.0183 (17)
C30.057 (2)0.075 (3)0.042 (2)−0.042 (2)0.0090 (19)−0.029 (2)
C40.0338 (18)0.044 (2)0.042 (2)−0.0189 (17)−0.0023 (15)−0.0118 (17)
C50.0272 (16)0.0403 (19)0.0376 (19)−0.0138 (15)0.0068 (14)−0.0054 (15)
C60.0313 (17)0.0321 (17)0.0274 (16)−0.0106 (14)0.0035 (13)−0.0057 (13)
C70.0252 (15)0.0184 (14)0.0291 (15)−0.0046 (12)0.0053 (12)−0.0064 (12)
C80.0274 (16)0.0271 (16)0.045 (2)−0.0015 (14)−0.0034 (15)−0.0106 (15)
C90.036 (2)0.033 (2)0.063 (2)0.0057 (16)0.0071 (19)−0.0124 (19)
C100.060 (2)0.0254 (18)0.055 (2)−0.0007 (18)0.014 (2)−0.0178 (17)
C110.063 (2)0.0270 (17)0.0353 (19)−0.0181 (18)0.0053 (17)−0.0107 (15)
C120.0389 (18)0.0210 (15)0.0262 (15)−0.0097 (14)0.0031 (13)−0.0026 (12)
C130.0317 (16)0.0284 (16)0.0237 (15)−0.0091 (14)0.0075 (13)−0.0025 (12)
C140.049 (2)0.0249 (17)0.0371 (19)−0.0130 (16)0.0107 (16)0.0007 (14)
C150.072 (3)0.0304 (19)0.047 (2)−0.026 (2)0.019 (2)−0.0107 (17)
C160.070 (3)0.053 (2)0.049 (2)−0.041 (2)0.012 (2)−0.019 (2)
C170.046 (2)0.060 (2)0.049 (2)−0.028 (2)−0.0003 (19)−0.015 (2)
C180.0355 (18)0.0371 (19)0.0354 (18)−0.0113 (16)0.0031 (15)−0.0074 (15)
C190.0296 (16)0.0298 (16)0.0247 (15)−0.0089 (13)0.0026 (12)−0.0080 (13)
C200.077 (3)0.036 (2)0.045 (2)−0.008 (2)0.030 (2)−0.0062 (18)
C210.085 (3)0.056 (2)0.046 (2)0.003 (2)0.039 (2)−0.009 (2)
C220.050 (2)0.041 (2)0.0311 (18)−0.0035 (18)0.0114 (16)−0.0136 (16)
C230.051 (2)0.0328 (18)0.0328 (18)−0.0020 (17)0.0065 (17)−0.0076 (15)
C240.047 (2)0.0298 (17)0.0247 (16)−0.0032 (15)0.0104 (15)−0.0053 (13)
C250.142 (9)0.180 (11)0.057 (4)0.105 (9)0.007 (4)0.026 (6)
C260.168 (10)0.152 (9)0.091 (6)0.074 (8)−0.027 (6)0.014 (6)
C270.146 (8)0.169 (10)0.084 (6)0.082 (8)0.016 (5)0.048 (6)
Geometric parameters (Å, º) top
Zr1—Cl12.4450 (9)C19—C241.380 (4)
Zr1—Cl1i2.4450 (9)C20—C211.379 (6)
Zr1—Cl22.4627 (7)C21—C221.377 (5)
Zr1—Cl2i2.4627 (7)C22—C231.369 (5)
Zr1—O12.0820 (18)C23—C241.386 (5)
Zr1—O1i2.0820 (18)C25—C261.358 (19)
P1—P22.2057 (10)C25—C27ii1.33 (2)
P1—O11.5281 (19)C26—C271.399 (16)
P1—C11.787 (3)C2—H10.950
P1—C7)1.788 (3)C3—H20.950
P2—C131.833 (4)C4—H30.950
P2—C191.833 (3)C5—H40.950
C1—C21.382 (5)C6—H50.950
C1—C61.397 (4)C8—H60.950
C2—C31.391 (7)C9—H70.950
C3—C41.392 (6)C10—H80.950
C4—C51.390 (6)C11—H90.950
C5—C61.394 (6)C12—H100.950
C7—C81.393 (4)C14—H110.950
C7—C121.397 (5)C15—H120.950
C8—C91.387 (5)C16—H130.950
C9—C101.382 (7)C17—H140.950
C10—C111.379 (5)C18—H150.950
C11—C121.389 (5)C20—H160.950
C13—C141.400 (4)C21—H170.950
C13—C181.397 (4)C22—H180.950
C14—C151.388 (7)C23—H190.950
C15—C161.366 (6)C24—H200.950
C16—C171.379 (6)C25—H210.950
C17—C181.390 (7)C26—H220.950
C19—C201.392 (5)C27—H230.950
Cl(1)···C(11)iii3.525 (4)H(7)···H(3)xi3.057
Cl(2)···C(4)iv3.562 (4)H(7)···H(13)ix2.668
Cl(2)···C(5)iv3.585 (4)H(7)···H(14)ix3.540
C(4)···Cl(2)iv3.562 (4)H(7)···H(19)xiii3.174
C(5)···Cl(2)iv3.585 (4)H(7)···H(21)3.273
C(11)···Cl(1)iii3.525 (4)H(8)···Cl(1)iii3.494
Cl(1)···H(4)v3.032H(8)···Cl(2)vi3.258
Cl(1)···H(8)iii3.494H(8)···C(4)xi3.362
Cl(1)···H(9)iii2.887H(8)···C(5)xi3.208
Cl(1)···H(12)iii3.318H(8)···C(6)vi3.398
Cl(2)···H(3)iv2.911H(8)···H(3)xi3.321
Cl(2)···H(4)iv2.961H(8)···H(4)xi3.055
Cl(2)···H(7)vi2.927H(8)···H(4)vi3.535
Cl(2)···H(8)vi3.258H(8)···H(5)vi2.572
Cl(2)···H(13)iii3.045H(9)···Cl(1)iii2.887
C(2)···H(17)vii3.413H(9)···C(16)iii3.110
C(2)···H(18)vii3.110H(9)···C(17)iii2.899
C(3)···H(17)vii3.277H(9)···H(10)iii3.588
C(3)···H(18)vii3.282H(9)···H(13)iii2.949
C(3)···H(23)ii3.560H(9)···H(14)iii2.582
C(4)···H(8)viii3.362H(10)···H(9)iii3.588
C(4)···H(15)ix3.020H(10)···H(13)iii3.143
C(5)···H(8)viii3.208H(11)···C(20)x3.460
C(5)···H(14)ix3.164H(11)···C(21)x3.354
C(5)···H(15)ix3.157H(11)···H(16)x2.879
C(6)···H(4)iv3.442H(11)···H(17)x2.667
C(6)···H(8)vi3.398H(11)···H(22)3.352
C(6)···H(14)ix3.176H(12)···Cl(1)iii3.318
C(8)···H(14)ix3.237H(12)···C(23)xi3.490
C(8)···H(21)3.481H(12)···C(24)xi3.568
C(9)···H(13)ix3.339H(12)···H(17)x2.930
C(10)···H(5)vi3.352H(12)···H(19)xi2.960
C(11)···H(13)iii3.366H(12)···H(20)xi3.109
C(11)···H(14)iii3.275H(13)···Cl(2)iii3.045
C(12)···H(13)iii3.465H(13)···C(9)v3.339
C(13)···H(16)x3.566H(13)···C(11)iii3.366
C(14)···H(16)x3.027H(13)···C(12)iii3.465
C(14)···H(17)x3.209H(13)···H(6)v3.492
C(15)···H(16)x3.479H(13)···H(7)v2.668
C(15)···H(17)x3.335H(13)···H(9)iii2.949
C(15)···H(19)xi3.244H(13)···H(10)iii3.143
C(16)···H(7)v3.426H(13)···H(19)xi2.912
C(16)···H(9)iii3.110H(13)···H(21)v3.382
C(16)···H(19)xi3.220H(14)···C(5)v3.164
C(16)···H(21)v3.293H(14)···C(6)v3.176
C(17)···H(6)v3.327H(14)···C(8)v3.237
C(17)···H(9)iii2.899H(14)···C(11)iii3.275
C(17)···H(21)v3.332H(14)···H(4)v3.268
C(17)···H(23)x3.371H(14)···H(5)v3.293
C(18)···H(23)x3.192H(14)···H(6)v2.665
C(20)···H(11)x3.460H(14)···H(7)v3.540
C(21)···H(1)vii3.425H(14)···H(9)iii2.582
C(21)···H(2)vii3.408H(14)···H(21)v3.424
C(21)···H(11)x3.354H(14)···H(23)x3.500
C(22)···H(1)vii3.091H(15)···C(4)v3.020
C(22)···H(2)v3.600H(15)···C(5)v3.157
C(22)···H(2)vii3.375H(15)···H(3)v2.914
C(22)···H(3)v3.494H(15)···H(4)v3.149
C(22)···H(22)xii3.500H(15)···H(23)x3.233
C(23)···H(3)v3.020H(16)···C(13)x3.566
C(23)···H(12)viii3.490H(16)···C(14)x3.027
C(23)···H(21)xii3.506H(16)···C(15)x3.479
C(24)···H(3)v3.242H(16)···H(11)x2.879
C(24)···H(12)viii3.568H(16)···H(23)x3.494
C(25)···H(6)2.983H(17)···C(2)vii3.413
C(25)···H(18)xiii3.342H(17)···C(3)vii3.277
C(26)···H(1)ii3.419H(17)···C(14)x3.209
C(26)···H(6)3.481H(17)···C(15)x3.335
C(26)···H(18)xiii3.138H(17)···H(1)vii3.071
C(27)···H(6)ii3.518H(17)···H(2)vii2.827
H(1)···C(21)vii3.425H(17)···H(11)x2.667
H(1)···C(22)vii3.091H(17)···H(12)x2.930
H(1)···C(26)ii3.419H(17)···H(22)x3.566
H(1)···H(17)vii3.071H(18)···C(2)vii3.110
H(1)···H(18)vii2.397H(18)···C(3)vii3.282
H(1)···H(22)ii3.424H(18)···C(25)xii3.342
H(2)···C(21)vii3.408H(18)···C(26)xii3.138
H(2)···C(22)ix3.600H(18)···H(1)vii2.397
H(2)···C(22)vii3.375H(18)···H(2)vii2.762
H(2)···H(17)vii2.827H(18)···H(21)xii3.046
H(2)···H(18)vii2.762H(18)···H(22)xii2.675
H(2)···H(22)ii3.190H(19)···C(15)viii3.244
H(2)···H(23)ii3.595H(19)···C(16)viii3.220
H(3)···Cl(2)iv2.911H(19)···H(3)v3.088
H(3)···C(22)ix3.494H(19)···H(7)xii3.174
H(3)···C(23)ix3.020H(19)···H(12)viii2.960
H(3)···C(24)ix3.242H(19)···H(13)viii2.912
H(3)···H(7)viii3.057H(19)···H(21)xii2.796
H(3)···H(8)viii3.321H(20)···H(3)v3.452
H(3)···H(15)ix2.914H(20)···H(12)viii3.109
H(3)···H(19)ix3.088H(21)···C(8)3.481
H(3)···H(20)ix3.452H(21)···C(16)ix3.293
H(4)···Cl(1)ix3.032H(21)···C(17)ix3.332
H(4)···Cl(2)iv2.961H(21)···C(23)xiii3.506
H(4)···C(6)iv3.442H(21)···H(6)2.756
H(4)···H(4)iv3.226H(21)···H(7)3.273
H(4)···H(5)iv2.901H(21)···H(13)ix3.382
H(4)···H(8)viii3.055H(21)···H(14)ix3.424
H(4)···H(8)vi3.535H(21)···H(18)xiii3.046
H(4)···H(14)ix3.268H(21)···H(19)xiii2.796
H(4)···H(15)ix3.149H(22)···C(22)xiii3.500
H(5)···C(10)vi3.352H(22)···H(1)ii3.424
H(5)···H(4)iv2.901H(22)···H(2)ii3.190
H(5)···H(8)vi2.572H(22)···H(6)3.593
H(5)···H(14)ix3.293H(22)···H(11)3.352
H(6)···C(17)ix3.327H(22)···H(17)x3.566
H(6)···C(25)2.983H(22)···H(18)xiii2.675
H(6)···C(26)3.481H(23)···C(3)ii3.560
H(6)···C(27)ii3.518H(23)···C(17)x3.371
H(6)···H(13)ix3.492H(23)···C(18)x3.192
H(6)···H(14)ix2.665H(23)···H(2)ii3.595
H(6)···H(21)2.756H(23)···H(14)x3.500
H(6)···H(22)3.593H(23)···H(15)x3.233
H(7)···Cl(2)vi2.927H(23)···H(16)x3.494
H(7)···C(16)ix3.426
Cl(1)—Zr(1)—Cl(1)i180C(20)—C(21)—C(22)119.9 (4)
Cl(1)—Zr(1)—Cl(2)89.73 (2)C(21)—C(22)—C(23)119.6 (3)
Cl(1)—Zr(1)—Cl(2)i90.27 (2)C(22)—C(23)—C(24)120.7 (3)
Cl(1)—Zr(1)—O(1)90.01 (7)C(19)—C(24)—C(23)120.5 (3)
Cl(1)—Zr(1)—O(1)i89.99 (7)C(26)—C(25)—C(27)ii120.6 (10)
Cl(1)i—Zr(1)—Cl(2)90.27 (2)C(25)—C(26)—C(27)120.5 (13)
Cl(1)i—Zr(1)—Cl(2)i89.73 (2)C(25)ii—C(27)—C(26)118.9 (12)
Cl(1)i—Zr(1)—O(1)89.99 (7)C(1)—C(2)—H(1)119.6
Cl(1)i—Zr(1)—O(1)i90.01 (7)C(3)—C(2)—H(1)119.6
Cl(2)—Zr(1)—Cl(2)i180C(2)—C(3)—H(2)120.2
Cl(2)—Zr(1)—O(1)89.43 (5)C(4)—C(3)—H(2)120.2
Cl(2)—Zr(1)—O(1)i90.57 (5)C(3)—C(4)—H(3)119.9
Cl(2)i—Zr(1)—O(1)90.57 (5)C(5)—C(4)—H(3)119.9
Cl(2)i—Zr(1)—O(1)i89.43 (5)C(4)—C(5)—H(4)120.1
O(1)—Zr(1)—O(1)i180C(6)—C(5)—H(4)120.1
P(2)—P(1)—O(1)115.79 (9)C(1)—C(6)—H(5)120.0
P(2)—P(1)—C(1)108.46 (10)C(5)—C(6)—H(5)120.0
P(2)—P(1)—C(7)101.63 (10)C(7)—C(8)—H(6)120.1
O(1)—P(1)—C(1)111.99 (13)C(9)—C(8)—H(6)120.1
O(1)—P(1)—C(7)109.97 (14)C(8)—C(9)—H(7)120.3
C(1)—P(1)—C(7)108.32 (15)C(10)—C(9)—H(7)120.3
P(1)—P(2)—C(13)95.26 (11)C(9)—C(10)—H(8)119.4
P(1)—P(2)—C(19)105.04 (10)C(11)—C(10)—H(8)119.5
C(13)—P(2)—C(19)103.65 (16)C(10)—C(11)—H(9)119.9
Zr(1)—O(1)—P(1)155.63 (13)C(12)—C(11)—H(9)119.9
P(1)—C(1)—C(2)122.1 (2)C(7)—C(12)—H(10)120.5
P(1)—C(1)—C(6)118.3 (2)C(11)—C(12)—H(10)120.5
C(2)—C(1)—C(6)119.6 (3)C(13)—C(14)—H(11)119.8
C(1)—C(2)—C(3)120.7 (3)C(15)—C(14)—H(11)119.8
C(2)—C(3)—C(4)119.7 (4)C(14)—C(15)—H(12)119.9
C(3)—C(4)—C(5)120.1 (4)C(16)—C(15)—H(12)119.9
C(4)—C(5)—C(6)119.8 (3)C(15)—C(16)—H(13)119.8
C(1)—C(6)—C(5)120.1 (3)C(17)—C(16)—H(13)119.8
P(1)—C(7)—C(8)119.6 (2)C(16)—C(17)—H(14)119.8
P(1)—C(7)—C(12)119.5 (2)C(18)—C(17)—H(14)119.8
C(8)—C(7)—C(12)120.4 (3)C(13)—C(18)—H(15)120.1
C(7)—C(8)—C(9)119.8 (3)C(17)—C(18)—H(15)120.1
C(8)—C(9)—C(10)119.4 (3)C(19)—C(20)—H(16)119.4
C(9)—C(10)—C(11)121.1 (3)C(21)—C(20)—H(16)119.4
C(10)—C(11)—C(12)120.2 (4)C(20)—C(21)—H(17)120.1
C(7)—C(12)—C(11)119.0 (3)C(22)—C(21)—H(17)120.1
P(2)—C(13)—C(14)117.1 (2)C(21)—C(22)—H(18)120.2
P(2)—C(13)—C(18)124.0 (2)C(23)—C(22)—H(18)120.2
C(14)—C(13)—C(18)118.8 (3)C(22)—C(23)—H(19)119.6
C(13)—C(14)—C(15)120.4 (3)C(24)—C(23)—H(19)119.6
C(14)—C(15)—C(16)120.2 (3)C(19)—C(24)—H(20)119.8
C(15)—C(16)—C(17)120.3 (5)C(23)—C(24)—H(20)119.8
C(16)—C(17)—C(18)120.5 (4)C(26)—C(25)—H(21)119.7
C(13)—C(18)—C(17)119.8 (3)C(27)ii—C(25)—H(21)119.7
P(2)—C(19)—C(20)115.2 (2)C(25)—C(26)—H(22)119.7
P(2)—C(19)—C(24)126.5 (2)C(27)—C(26)—H(22)119.8
C(20)—C(19)—C(24)118.2 (3)C(25)ii—C(27)—H(23)120.6
C(19)—C(20)—C(21)121.1 (3)C(26)—C(27)—H(23)120.6
Cl(1)—Zr(1)—O(1)—P(1)−126.6 (3)C(19)—P(2)—C(13)—C(18)−30.0 (3)
Cl(1)—Zr(1)—O(1)i—P(1)i−53.4 (3)P(1)—C(1)—C(2)—C(3)179.7 (2)
Cl(1)i—Zr(1)—O(1)—P(1)53.4 (3)P(1)—C(1)—C(6)—C(5)−179.4 (2)
Cl(1)i—Zr(1)—O(1)i—P(1)i126.6 (3)C(2)—C(1)—C(6)—C(5)−1.0 (4)
Cl(2)—Zr(1)—O(1)—P(1)−36.8 (3)C(6)—C(1)—C(2)—C(3)1.3 (5)
Cl(2)—Zr(1)—O(1)i—P(1)i−143.2 (3)C(1)—C(2)—C(3)—C(4)−1.0 (5)
Cl(2)i—Zr(1)—O(1)—P(1)143.2 (3)C(2)—C(3)—C(4)—C(5)0.4 (5)
Cl(2)i—Zr(1)—O(1)i—P(1)i36.8 (3)C(3)—C(4)—C(5)—C(6)−0.1 (4)
P(2)—P(1)—O(1)—Zr(1)−171.5 (3)C(4)—C(5)—C(6)—C(1)0.4 (4)
O(1)—P(1)—P(2)—C(13)−61.58 (14)P(1)—C(7)—C(8)—C(9)−171.8 (3)
O(1)—P(1)—P(2)—C(19)44.08 (17)P(1)—C(7)—C(12)—C(11)172.2 (2)
P(2)—P(1)—C(1)—C(2)19.8 (2)C(8)—C(7)—C(12)—C(11)−0.2 (5)
P(2)—P(1)—C(1)—C(6)−161.7 (2)C(12)—C(7)—C(8)—C(9)0.6 (5)
C(1)—P(1)—P(2)—C(13)171.56 (13)C(7)—C(8)—C(9)—C(10)−0.7 (6)
C(1)—P(1)—P(2)—C(19)−82.77 (16)C(8)—C(9)—C(10)—C(11)0.4 (6)
P(2)—P(1)—C(7)—C(8)72.2 (2)C(9)—C(10)—C(11)—C(12)0.0 (6)
P(2)—P(1)—C(7)—C(12)−100.3 (2)C(10)—C(11)—C(12)—C(7)−0.1 (4)
C(7)—P(1)—P(2)—C(13)57.55 (15)P(2)—C(13)—C(14)—C(15)173.9 (3)
C(7)—P(1)—P(2)—C(19)163.22 (17)P(2)—C(13)—C(18)—C(17)−175.3 (2)
O(1)—P(1)—C(1)—C(2)−109.2 (2)C(14)—C(13)—C(18)—C(17)−0.4 (5)
O(1)—P(1)—C(1)—C(6)69.2 (2)C(18)—C(13)—C(14)—C(15)−1.4 (5)
C(1)—P(1)—O(1)—Zr(1)−46.5 (4)C(13)—C(14)—C(15)—C(16)1.6 (6)
O(1)—P(1)—C(7)—C(8)−164.6 (2)C(14)—C(15)—C(16)—C(17)−0.1 (5)
O(1)—P(1)—C(7)—C(12)22.9 (3)C(15)—C(16)—C(17)—C(18)−1.6 (6)
C(7)—P(1)—O(1)—Zr(1)74.0 (3)C(16)—C(17)—C(18)—C(13)1.9 (6)
C(1)—P(1)—C(7)—C(8)−41.9 (3)P(2)—C(19)—C(20)—C(21)−178.6 (4)
C(1)—P(1)—C(7)—C(12)145.6 (2)P(2)—C(19)—C(24)—C(23)177.4 (3)
C(7)—P(1)—C(1)—C(2)129.4 (2)C(20)—C(19)—C(24)—C(23)1.9 (6)
C(7)—P(1)—C(1)—C(6)−52.2 (2)C(24)—C(19)—C(20)—C(21)−2.5 (7)
P(1)—P(2)—C(13)—C(14)−98.1 (2)C(19)—C(20)—C(21)—C(22)1.8 (8)
P(1)—P(2)—C(13)—C(18)76.9 (2)C(20)—C(21)—C(22)—C(23)−0.3 (7)
P(1)—P(2)—C(19)—C(20)177.0 (3)C(21)—C(22)—C(23)—C(24)−0.4 (7)
P(1)—P(2)—C(19)—C(24)1.3 (3)C(22)—C(23)—C(24)—C(19)−0.5 (6)
C(13)—P(2)—C(19)—C(20)−83.7 (3)C(26)—C(25)—C(27)ii—C(26)ii−1.8 (15)
C(13)—P(2)—C(19)—C(24)100.6 (3)C(27)ii—C(25)—C(26)—C(27)1.8 (16)
C(19)—P(2)—C(13)—C(14)155.0 (2)C(25)—C(26)—C(27)—C(25)ii−1.8 (15)
Symmetry codes: (i) −x+2, −y, −z+2; (ii) −x+1, −y+1, −z+1; (iii) −x+2, −y+1, −z+2; (iv) −x+1, −y, −z+2; (v) x+1, y, z; (vi) −x+1, −y+1, −z+2; (vii) −x+2, −y, −z+1; (viii) x, y−1, z; (ix) x−1, y, z; (x) −x+2, −y+1, −z+1; (xi) x, y+1, z; (xii) x+1, y−1, z; (xiii) x−1, y+1, z.
Selected bond lengths (Å) top
Zr1—Cl12.4450 (9)Zr1—O12.0820 (18)
Zr1—Cl22.4627 (7)
Acknowledgements top

We gratefully acknowledge the support of this work by a Grant-in-Aid for Scientific Research from the Ministry of Education, Science, Sports and Culture.

references
References top

Altomare, A., Cascarano, G., Giacovazzo, C., Guagliardi, A., Burla, M., Polidori, G. & Camalli, M. (1994). J. Appl. Cryst. 27, 435.

Berners-Price, S. J., Navarro, M. & Skelton, B. W. (2009). Acta Cryst. E65, o542.

Farrugia, L. J. (1997). J. Appl. Cryst. 30, 565.

Ferguson, G., Myers, M. & Spalding, T. R. (1990). Acta Cryst. C46, 122–124.

Jacobson, R. (1998). Private communication to the Rigaku Corporation, Tokyo, Japan.

Kuramshin, I. Ya. & Khramov, A. S. (1983). Deposited Doc. (VINITI 2649-83), 26. [Please provide more information; it is not clear what this reference refers to.]

Muratova, A. A., Sobanova, O. B., Yarkova, E. G., Khramov, A. S. & Pudovik, A. N. (1980). Zh. Obshch. Khim. 50, 275–280.

Rigaku (2007). CrystalClear and CrystalStructure. Rigaku Corporation, Tokyo, Japan.

Sheldrick, G. M. (2008). Acta Cryst. A64, 112–122.