Tetra-chlorido[(diphenyl-phosphino)diphenyl-phosphine oxide-κO]zirconium(IV) benzene monosolvate.

In the title centrosymmetric mononuclear Zr(IV) compound, [ZrCl(4){P(O)(C(6)H(5))(2)P(C(6)H(5))(2)}(2)]·C(6)H(6), the central Zr(IV) ion is coordinated by two O atoms from two symmetry-related (diphenyl-phosphino)diphenyl-phosphine ligands and four Cl atoms in a distorted octahedral geometry with the four Cl atoms in the equatorial positions. The mol-ecule lies about a center of inversion and the benzene solvent mol-ecule 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 ).

Related literature

For general background to the structure and coordination mode of (diphenyl­phosphino)diphenyl­phosphine (DPDP), see: Ferguson et al. (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

Crystal data

[ZrCl4(C24H20OP2)2]·C6H6

M = 1083.81

Triclinic,

a = 9.6073 (3) Å

b = 10.1521 (4) Å

c = 14.0204 (10) Å

α = 79.027 (13)°

β = 87.269 (13)°

γ = 73.096 (11)°

V = 1284.42 (11) Å3

Z = 1

Mo Kα radiation

μ = 0.59 mm−1

T = 173 K

0.30 × 0.15 × 0.13 mm

Data collection

Rigaku Mercury diffractometer

Absorption correction: multi-scan (Jacobson, 1998 ▶) T min = 0.900, T max = 0.927

10324 measured reflections

5669 independent reflections

4497 reflections with I > 2σ(I)

R int = 0.031

Refinement

R[F 2 > 2σ(F 2)] = 0.045

wR(F 2) = 0.151

S = 1.02

5669 reflections

296 parameters

H-atom parameters constrained

Δρmax = 1.04 e Å−3

Δρmin = −0.81 e Å−3

Data collection: CrystalClear (Rigaku, 2007 ▶); cell refinement: CrystalClear; 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.

Crystal structure: contains datablocks global, I. DOI: 10.1107/S1600536809031882/ng2624sup1.cif

Structure factors: contains datablocks I. DOI: 10.1107/S1600536809031882/ng2624Isup2.hkl

Additional supplementary materials: crystallographic information; 3D view; checkCIF report

[ZrCl4(C24H20OP2)2]·C6H6	Z = 1
Mr = 1083.81	F(000) = 554.00
Triclinic, P1	Dx = 1.401 Mg m−3
Hall symbol: -P 1	Mo Kα radiation, λ = 0.71070 Å
a = 9.6073 (3) Å	Cell parameters from 3589 reflections
b = 10.1521 (4) Å	θ = 3.2–27.5°
c = 14.0204 (10) Å	µ = 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

Rigaku Mercury diffractometer	4497 reflections with F2 > 2σ(F2)
Detector resolution: 7.31 pixels mm-1	Rint = 0.031
ω scans	θmax = 27.5°
Absorption correction: multi-scan (Jacobson, 1998)	h = −12→12
Tmin = 0.900, Tmax = 0.927	k = −11→13
10324 measured reflections	l = −13→18
5669 independent reflections

Refinement on F2	0 restraints
R[F2 > 2σ(F2)] = 0.045	H-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 reflections	Δρmax = 1.04 e Å−3
296 parameters	Δρmin = −0.81 e Å−3

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).

	x	y	z	Uiso*/Ueq
Zr1	1	0	1	0.01849 (13)
Cl1	1.14353 (9)	0.14927 (8)	1.03401 (6)	0.0305 (2)
Cl2	0.79704 (8)	0.12426 (8)	1.09344 (6)	0.02711 (18)
P1	0.79655 (8)	0.24267 (8)	0.80566 (5)	0.01964 (17)
P2	0.87015 (9)	0.33171 (9)	0.66302 (6)	0.0249 (2)
O1	0.9163 (2)	0.1442 (2)	0.87498 (15)	0.0212 (4)
C1	0.6603 (3)	0.1623 (3)	0.7861 (2)	0.0239 (6)
C2	0.6455 (4)	0.1237 (4)	0.6987 (2)	0.0404 (9)
C3	0.5388 (4)	0.0607 (5)	0.6859 (3)	0.0509 (11)
C4	0.4473 (4)	0.0343 (4)	0.7626 (2)	0.0377 (8)
C5	0.4620 (3)	0.0716 (3)	0.8512 (2)	0.0346 (7)
C6	0.5688 (3)	0.1353 (3)	0.8631 (2)	0.0301 (7)
C7	0.7107 (3)	0.3971 (3)	0.8540 (2)	0.0245 (6)
C8	0.5776 (3)	0.4851 (3)	0.8158 (2)	0.0339 (7)
C9	0.5195 (4)	0.6137 (4)	0.8442 (3)	0.0471 (10)
C10	0.5940 (4)	0.6522 (4)	0.9110 (3)	0.0482 (10)
C11	0.7256 (4)	0.5653 (3)	0.9496 (2)	0.0401 (9)
C12	0.7856 (3)	0.4366 (3)	0.9215 (2)	0.0288 (7)
C13	0.9801 (3)	0.4239 (3)	0.7122 (2)	0.0284 (7)
C14	0.9168 (4)	0.5667 (3)	0.7125 (2)	0.0375 (8)
C15	0.9878 (5)	0.6405 (4)	0.7568 (3)	0.0476 (10)
C16	1.1218 (5)	0.5752 (4)	0.7984 (3)	0.0513 (11)
C17	1.1876 (4)	0.4354 (4)	0.7969 (3)	0.0484 (10)
C18	1.1170 (4)	0.3584 (4)	0.7553 (2)	0.0358 (8)
C19	1.0058 (3)	0.1844 (3)	0.6233 (2)	0.0276 (6)
C20	1.0628 (5)	0.2151 (4)	0.5313 (3)	0.0552 (12)
C21	1.1635 (5)	0.1132 (5)	0.4917 (3)	0.0686 (15)
C22	1.2062 (4)	−0.0226 (4)	0.5424 (2)	0.0423 (9)
C23	1.1486 (4)	−0.0549 (4)	0.6320 (2)	0.0410 (9)
C24	1.0484 (4)	0.0476 (3)	0.6725 (2)	0.0358 (8)
C25	0.4088 (12)	0.5582 (15)	0.5682 (6)	0.165 (7)
C26	0.5127 (14)	0.6167 (11)	0.5268 (8)	0.167 (5)
C27	0.6047 (12)	0.5579 (14)	0.4560 (7)	0.171 (6)
H1	0.7090	0.1403	0.6467	0.049*
H2	0.5285	0.0358	0.6252	0.061*
H3	0.3746	−0.0093	0.7543	0.045*
H4	0.3994	0.0537	0.9034	0.041*
H5	0.5794	0.1603	0.9237	0.036*
H6	0.5267	0.4573	0.7704	0.041*
H7	0.4292	0.6746	0.8179	0.056*
H8	0.5540	0.7399	0.9307	0.058*
H9	0.7753	0.5936	0.9954	0.048*
H10	0.8763	0.3765	0.9477	0.035*
H11	0.8247	0.6134	0.6823	0.045*
H12	0.9430	0.7368	0.7582	0.057*
H13	1.1700	0.6262	0.8285	0.061*
H14	1.2819	0.3914	0.8245	0.058*
H15	1.1616	0.2615	0.7562	0.043*
H16	1.0318	0.3079	0.4953	0.066*
H17	1.2033	0.1364	0.4296	0.082*
H18	1.2752	−0.0933	0.5153	0.051*
H19	1.1776	−0.1486	0.6668	0.049*
H20	1.0088	0.0235	0.7345	0.043*
H21	0.3452	0.6006	0.6148	0.199*
H22	0.5231	0.6982	0.5461	0.200*
H23	0.6756	0.6003	0.4258	0.205*

	U11	U22	U33	U12	U13	U23
Zr1	0.0175 (2)	0.0156 (2)	0.0215 (2)	−0.00302 (15)	0.00179 (15)	−0.00429 (15)
Cl1	0.0292 (4)	0.0249 (3)	0.0416 (4)	−0.0116 (3)	−0.0023 (3)	−0.0096 (3)
Cl2	0.0237 (3)	0.0243 (3)	0.0309 (4)	−0.0023 (3)	0.0078 (3)	−0.0082 (3)
P1	0.0202 (3)	0.0174 (3)	0.0200 (3)	−0.0032 (2)	0.0018 (2)	−0.0041 (2)
P2	0.0277 (4)	0.0234 (4)	0.0211 (3)	−0.0051 (3)	0.0007 (3)	−0.0013 (3)
O1	0.0228 (10)	0.0185 (9)	0.0204 (10)	−0.0038 (8)	−0.0003 (8)	−0.0020 (8)
C1	0.0240 (14)	0.0194 (14)	0.0268 (15)	−0.0042 (12)	0.0027 (12)	−0.0045 (12)
C2	0.043 (2)	0.063 (2)	0.0286 (17)	−0.032 (2)	0.0102 (15)	−0.0183 (17)
C3	0.057 (2)	0.075 (3)	0.042 (2)	−0.042 (2)	0.0090 (19)	−0.029 (2)
C4	0.0338 (18)	0.044 (2)	0.042 (2)	−0.0189 (17)	−0.0023 (15)	−0.0118 (17)
C5	0.0272 (16)	0.0403 (19)	0.0376 (19)	−0.0138 (15)	0.0068 (14)	−0.0054 (15)
C6	0.0313 (17)	0.0321 (17)	0.0274 (16)	−0.0106 (14)	0.0035 (13)	−0.0057 (13)
C7	0.0252 (15)	0.0184 (14)	0.0291 (15)	−0.0046 (12)	0.0053 (12)	−0.0064 (12)
C8	0.0274 (16)	0.0271 (16)	0.045 (2)	−0.0015 (14)	−0.0034 (15)	−0.0106 (15)
C9	0.036 (2)	0.033 (2)	0.063 (2)	0.0057 (16)	0.0071 (19)	−0.0124 (19)
C10	0.060 (2)	0.0254 (18)	0.055 (2)	−0.0007 (18)	0.014 (2)	−0.0178 (17)
C11	0.063 (2)	0.0270 (17)	0.0353 (19)	−0.0181 (18)	0.0053 (17)	−0.0107 (15)
C12	0.0389 (18)	0.0210 (15)	0.0262 (15)	−0.0097 (14)	0.0031 (13)	−0.0026 (12)
C13	0.0317 (16)	0.0284 (16)	0.0237 (15)	−0.0091 (14)	0.0075 (13)	−0.0025 (12)
C14	0.049 (2)	0.0249 (17)	0.0371 (19)	−0.0130 (16)	0.0107 (16)	0.0007 (14)
C15	0.072 (3)	0.0304 (19)	0.047 (2)	−0.026 (2)	0.019 (2)	−0.0107 (17)
C16	0.070 (3)	0.053 (2)	0.049 (2)	−0.041 (2)	0.012 (2)	−0.019 (2)
C17	0.046 (2)	0.060 (2)	0.049 (2)	−0.028 (2)	−0.0003 (19)	−0.015 (2)
C18	0.0355 (18)	0.0371 (19)	0.0354 (18)	−0.0113 (16)	0.0031 (15)	−0.0074 (15)
C19	0.0296 (16)	0.0298 (16)	0.0247 (15)	−0.0089 (13)	0.0026 (12)	−0.0080 (13)
C20	0.077 (3)	0.036 (2)	0.045 (2)	−0.008 (2)	0.030 (2)	−0.0062 (18)
C21	0.085 (3)	0.056 (2)	0.046 (2)	0.003 (2)	0.039 (2)	−0.009 (2)
C22	0.050 (2)	0.041 (2)	0.0311 (18)	−0.0035 (18)	0.0114 (16)	−0.0136 (16)
C23	0.051 (2)	0.0328 (18)	0.0328 (18)	−0.0020 (17)	0.0065 (17)	−0.0076 (15)
C24	0.047 (2)	0.0298 (17)	0.0247 (16)	−0.0032 (15)	0.0104 (15)	−0.0053 (13)
C25	0.142 (9)	0.180 (11)	0.057 (4)	0.105 (9)	0.007 (4)	0.026 (6)
C26	0.168 (10)	0.152 (9)	0.091 (6)	0.074 (8)	−0.027 (6)	0.014 (6)
C27	0.146 (8)	0.169 (10)	0.084 (6)	0.082 (8)	0.016 (5)	0.048 (6)

Zr1—Cl1	2.4450 (9)	C19—C24	1.380 (4)
Zr1—Cl1i	2.4450 (9)	C20—C21	1.379 (6)
Zr1—Cl2	2.4627 (7)	C21—C22	1.377 (5)
Zr1—Cl2i	2.4627 (7)	C22—C23	1.369 (5)
Zr1—O1	2.0820 (18)	C23—C24	1.386 (5)
Zr1—O1i	2.0820 (18)	C25—C26	1.358 (19)
P1—P2	2.2057 (10)	C25—C27ii	1.33 (2)
P1—O1	1.5281 (19)	C26—C27	1.399 (16)
P1—C1	1.787 (3)	C2—H1	0.950
P1—C7)	1.788 (3)	C3—H2	0.950
P2—C13	1.833 (4)	C4—H3	0.950
P2—C19	1.833 (3)	C5—H4	0.950
C1—C2	1.382 (5)	C6—H5	0.950
C1—C6	1.397 (4)	C8—H6	0.950
C2—C3	1.391 (7)	C9—H7	0.950
C3—C4	1.392 (6)	C10—H8	0.950
C4—C5	1.390 (6)	C11—H9	0.950
C5—C6	1.394 (6)	C12—H10	0.950
C7—C8	1.393 (4)	C14—H11	0.950
C7—C12	1.397 (5)	C15—H12	0.950
C8—C9	1.387 (5)	C16—H13	0.950
C9—C10	1.382 (7)	C17—H14	0.950
C10—C11	1.379 (5)	C18—H15	0.950
C11—C12	1.389 (5)	C20—H16	0.950
C13—C14	1.400 (4)	C21—H17	0.950
C13—C18	1.397 (4)	C22—H18	0.950
C14—C15	1.388 (7)	C23—H19	0.950
C15—C16	1.366 (6)	C24—H20	0.950
C16—C17	1.379 (6)	C25—H21	0.950
C17—C18	1.390 (7)	C26—H22	0.950
C19—C20	1.392 (5)	C27—H23	0.950
Cl(1)···C(11)iii	3.525 (4)	H(7)···H(3)xi	3.057
Cl(2)···C(4)iv	3.562 (4)	H(7)···H(13)ix	2.668
Cl(2)···C(5)iv	3.585 (4)	H(7)···H(14)ix	3.540
C(4)···Cl(2)iv	3.562 (4)	H(7)···H(19)xiii	3.174
C(5)···Cl(2)iv	3.585 (4)	H(7)···H(21)	3.273
C(11)···Cl(1)iii	3.525 (4)	H(8)···Cl(1)iii	3.494
Cl(1)···H(4)v	3.032	H(8)···Cl(2)vi	3.258
Cl(1)···H(8)iii	3.494	H(8)···C(4)xi	3.362
Cl(1)···H(9)iii	2.887	H(8)···C(5)xi	3.208
Cl(1)···H(12)iii	3.318	H(8)···C(6)vi	3.398
Cl(2)···H(3)iv	2.911	H(8)···H(3)xi	3.321
Cl(2)···H(4)iv	2.961	H(8)···H(4)xi	3.055
Cl(2)···H(7)vi	2.927	H(8)···H(4)vi	3.535
Cl(2)···H(8)vi	3.258	H(8)···H(5)vi	2.572
Cl(2)···H(13)iii	3.045	H(9)···Cl(1)iii	2.887
C(2)···H(17)vii	3.413	H(9)···C(16)iii	3.110
C(2)···H(18)vii	3.110	H(9)···C(17)iii	2.899
C(3)···H(17)vii	3.277	H(9)···H(10)iii	3.588
C(3)···H(18)vii	3.282	H(9)···H(13)iii	2.949
C(3)···H(23)ii	3.560	H(9)···H(14)iii	2.582
C(4)···H(8)viii	3.362	H(10)···H(9)iii	3.588
C(4)···H(15)ix	3.020	H(10)···H(13)iii	3.143
C(5)···H(8)viii	3.208	H(11)···C(20)x	3.460
C(5)···H(14)ix	3.164	H(11)···C(21)x	3.354
C(5)···H(15)ix	3.157	H(11)···H(16)x	2.879
C(6)···H(4)iv	3.442	H(11)···H(17)x	2.667
C(6)···H(8)vi	3.398	H(11)···H(22)	3.352
C(6)···H(14)ix	3.176	H(12)···Cl(1)iii	3.318
C(8)···H(14)ix	3.237	H(12)···C(23)xi	3.490
C(8)···H(21)	3.481	H(12)···C(24)xi	3.568
C(9)···H(13)ix	3.339	H(12)···H(17)x	2.930
C(10)···H(5)vi	3.352	H(12)···H(19)xi	2.960
C(11)···H(13)iii	3.366	H(12)···H(20)xi	3.109
C(11)···H(14)iii	3.275	H(13)···Cl(2)iii	3.045
C(12)···H(13)iii	3.465	H(13)···C(9)v	3.339
C(13)···H(16)x	3.566	H(13)···C(11)iii	3.366
C(14)···H(16)x	3.027	H(13)···C(12)iii	3.465
C(14)···H(17)x	3.209	H(13)···H(6)v	3.492
C(15)···H(16)x	3.479	H(13)···H(7)v	2.668
C(15)···H(17)x	3.335	H(13)···H(9)iii	2.949
C(15)···H(19)xi	3.244	H(13)···H(10)iii	3.143
C(16)···H(7)v	3.426	H(13)···H(19)xi	2.912
C(16)···H(9)iii	3.110	H(13)···H(21)v	3.382
C(16)···H(19)xi	3.220	H(14)···C(5)v	3.164
C(16)···H(21)v	3.293	H(14)···C(6)v	3.176
C(17)···H(6)v	3.327	H(14)···C(8)v	3.237
C(17)···H(9)iii	2.899	H(14)···C(11)iii	3.275
C(17)···H(21)v	3.332	H(14)···H(4)v	3.268
C(17)···H(23)x	3.371	H(14)···H(5)v	3.293
C(18)···H(23)x	3.192	H(14)···H(6)v	2.665
C(20)···H(11)x	3.460	H(14)···H(7)v	3.540
C(21)···H(1)vii	3.425	H(14)···H(9)iii	2.582
C(21)···H(2)vii	3.408	H(14)···H(21)v	3.424
C(21)···H(11)x	3.354	H(14)···H(23)x	3.500
C(22)···H(1)vii	3.091	H(15)···C(4)v	3.020
C(22)···H(2)v	3.600	H(15)···C(5)v	3.157
C(22)···H(2)vii	3.375	H(15)···H(3)v	2.914
C(22)···H(3)v	3.494	H(15)···H(4)v	3.149
C(22)···H(22)xii	3.500	H(15)···H(23)x	3.233
C(23)···H(3)v	3.020	H(16)···C(13)x	3.566
C(23)···H(12)viii	3.490	H(16)···C(14)x	3.027
C(23)···H(21)xii	3.506	H(16)···C(15)x	3.479
C(24)···H(3)v	3.242	H(16)···H(11)x	2.879
C(24)···H(12)viii	3.568	H(16)···H(23)x	3.494
C(25)···H(6)	2.983	H(17)···C(2)vii	3.413
C(25)···H(18)xiii	3.342	H(17)···C(3)vii	3.277
C(26)···H(1)ii	3.419	H(17)···C(14)x	3.209
C(26)···H(6)	3.481	H(17)···C(15)x	3.335
C(26)···H(18)xiii	3.138	H(17)···H(1)vii	3.071
C(27)···H(6)ii	3.518	H(17)···H(2)vii	2.827
H(1)···C(21)vii	3.425	H(17)···H(11)x	2.667
H(1)···C(22)vii	3.091	H(17)···H(12)x	2.930
H(1)···C(26)ii	3.419	H(17)···H(22)x	3.566
H(1)···H(17)vii	3.071	H(18)···C(2)vii	3.110
H(1)···H(18)vii	2.397	H(18)···C(3)vii	3.282
H(1)···H(22)ii	3.424	H(18)···C(25)xii	3.342
H(2)···C(21)vii	3.408	H(18)···C(26)xii	3.138
H(2)···C(22)ix	3.600	H(18)···H(1)vii	2.397
H(2)···C(22)vii	3.375	H(18)···H(2)vii	2.762
H(2)···H(17)vii	2.827	H(18)···H(21)xii	3.046
H(2)···H(18)vii	2.762	H(18)···H(22)xii	2.675
H(2)···H(22)ii	3.190	H(19)···C(15)viii	3.244
H(2)···H(23)ii	3.595	H(19)···C(16)viii	3.220
H(3)···Cl(2)iv	2.911	H(19)···H(3)v	3.088
H(3)···C(22)ix	3.494	H(19)···H(7)xii	3.174
H(3)···C(23)ix	3.020	H(19)···H(12)viii	2.960
H(3)···C(24)ix	3.242	H(19)···H(13)viii	2.912
H(3)···H(7)viii	3.057	H(19)···H(21)xii	2.796
H(3)···H(8)viii	3.321	H(20)···H(3)v	3.452
H(3)···H(15)ix	2.914	H(20)···H(12)viii	3.109
H(3)···H(19)ix	3.088	H(21)···C(8)	3.481
H(3)···H(20)ix	3.452	H(21)···C(16)ix	3.293
H(4)···Cl(1)ix	3.032	H(21)···C(17)ix	3.332
H(4)···Cl(2)iv	2.961	H(21)···C(23)xiii	3.506
H(4)···C(6)iv	3.442	H(21)···H(6)	2.756
H(4)···H(4)iv	3.226	H(21)···H(7)	3.273
H(4)···H(5)iv	2.901	H(21)···H(13)ix	3.382
H(4)···H(8)viii	3.055	H(21)···H(14)ix	3.424
H(4)···H(8)vi	3.535	H(21)···H(18)xiii	3.046
H(4)···H(14)ix	3.268	H(21)···H(19)xiii	2.796
H(4)···H(15)ix	3.149	H(22)···C(22)xiii	3.500
H(5)···C(10)vi	3.352	H(22)···H(1)ii	3.424
H(5)···H(4)iv	2.901	H(22)···H(2)ii	3.190
H(5)···H(8)vi	2.572	H(22)···H(6)	3.593
H(5)···H(14)ix	3.293	H(22)···H(11)	3.352
H(6)···C(17)ix	3.327	H(22)···H(17)x	3.566
H(6)···C(25)	2.983	H(22)···H(18)xiii	2.675
H(6)···C(26)	3.481	H(23)···C(3)ii	3.560
H(6)···C(27)ii	3.518	H(23)···C(17)x	3.371
H(6)···H(13)ix	3.492	H(23)···C(18)x	3.192
H(6)···H(14)ix	2.665	H(23)···H(2)ii	3.595
H(6)···H(21)	2.756	H(23)···H(14)x	3.500
H(6)···H(22)	3.593	H(23)···H(15)x	3.233
H(7)···Cl(2)vi	2.927	H(23)···H(16)x	3.494
H(7)···C(16)ix	3.426
Cl(1)—Zr(1)—Cl(1)i	180	C(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)i	90.27 (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)i	89.99 (7)	C(26)—C(25)—C(27)ii	120.6 (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)i	89.73 (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)i	90.01 (7)	C(3)—C(2)—H(1)	119.6
Cl(2)—Zr(1)—Cl(2)i	180	C(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)i	90.57 (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)i	89.43 (5)	C(4)—C(5)—H(4)	120.1
O(1)—Zr(1)—O(1)i	180	C(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)i	126.6 (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)i	36.8 (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)

Table 1

Selected bond lengths (Å)

Zr1—Cl1	2.4450 (9)
Zr1—Cl2	2.4627 (7)
Zr1—O1	2.0820 (18)