A centrosymmetric triply alkoxo-bridged titanium-μ2-O-zirconium tetranuclear complex: [TiZr(μ2-O,μ2-O′-methyl­imino­diethano­late)(μ2-O-n-propanolate)2(n-propanolate)2.7(isopropanolate)1.3]2

Gainsford, G.J.; Al-Salim, N.; Kemmitt, T.

doi:10.1107/S1600536802018482

A centrosymmetric triply alkoxo-bridged titanium-μ₂-O-zirconium tetranuclear complex: [TiZr(μ₂-O,μ₂-O′-methyliminodiethanolate)(μ₂-O-n-propanolate)₂(n-propanolate)_2.7(isopropanolate)_1.3]₂

G. J. Gainsford, N. Al-Salim and T. Kemmitt

The centrosymmetric tetranuclear title compound, bis(methyliminodiethanolato)dodecapropanolatodititaniumdizirconium, [Ti₂Zr₂(C₃H₇O)₁₂(C₅H₁₁NO₂)₂], has a zigzag TiZr₂Ti arrangement including novel triple-oxo Ti

Zr bridges. The methyliminodiethanolate ligand is bound to the zirconium in a meridional configuration, with the ethanolate O atoms bridging both the Ti

Zr and Zr

Zr centres. Two n-propanolate O atoms provide the other two Ti

Zr bridges. The remaining propanolate ligands are attached to either Zr or Ti, completing seven- and six-coordination, respectively. The distorted pentagonal bypyramidal [ZrO₅N₂] units edge-share with each other and face-share with the distorted octahedral [TiO₆] units. As well as some conventional conformational disorder involving alternative carbon-chain conformations, there is some iso- and n-propanolate chemical disorder around the Ti atoms.

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Supporting information

	Crystallographic Information File (CIF) https://doi.org/10.1107/S1600536802018482/ww6042sup1.cif Contains datablocks global, I
	Structure factor file (CIF format) https://doi.org/10.1107/S1600536802018482/ww6042Isup2.hkl Contains datablock I

CCDC reference: 200726

checkCIF report

Key indicators

Single-crystal X-ray study
T = 170 K
Mean (C-C) = 0.011 Å
H-atom completeness 61%
R factor = 0.068
wR factor = 0.215
Data-to-parameter ratio = 21.3

checkCIF results

No syntax errors found

ADDSYM reports no extra symmetry

General Notes



FORMU_01  There is a discrepancy between the atom counts in the
          _chemical_formula_sum and the formula from the _atom_site* data.
          Atom count from _chemical_formula_sum:C46 H106 N2 O16 Ti2 Zr2
          Atom count from the _atom_site data:  C46.004 H63.68799 N2 O16 Ti2 Zr

CELLZ_01
         From the CIF: _cell_formula_units_Z    1
         From the CIF: _chemical_formula_sum  C46 H106 N2 O16 Ti2 Zr2
         TEST: Compare cell contents of formula and atom_site data

         atom    Z*formula  cif sites diff
         C         46.00     46.00    0.00
         H        106.00     63.69   42.31
         N          2.00      2.00    0.00
         O         16.00     16.00    0.00
         Ti         2.00      2.00    0.00
         Zr         2.00      2.00    0.00
          Difference between formula and atom_site contents detected.
          WARNING: H atoms missing from atom site list. Is this intentional?

CHEMW_03
         From the CIF: _cell_formula_units_Z                    1
         From the CIF: _chemical_formula_weight          1221.57
         TEST: Calculate formula weight from _atom_site_*
         atom     mass    num     sum
         C        12.01   46.00  552.55
         H         1.01   63.69   64.20
         N        14.01    2.00   28.01
         O        16.00   16.00  255.98
         Ti       47.88    2.00   95.76
         Zr       91.22    2.00  182.45
         Calculated formula weight             1178.96
          The ratio of given/expected molecular weight as calculated
          from the _atom_site* data lies outside
          the range 0.99 <> 1.01

Computing details top

Data collection: SMART (Siemens, 1996); cell refinement: SMART; data reduction: SAINT (Siemens, 1996) and SADABS (Sheldrick, 1996); program(s) used to solve structure: SHELXS97 (Sheldrick, 1997); program(s) used to refine structure: SHELXL97 (Sheldrick, 1997); molecular graphics: ORTEP-3 in WinGX (Farrugia, 1997); software used to prepare material for publication: SHELXL97.

[TiZr(µ₂-O-,µ₂-O'-methyliminodiethanolate)(µ₂-O-n-propanolate)₂ (n-propanolate)_2.7(iso-propanolate)_1.3]₂bis(methyliminodiethanolato)dodecapropanolatodititaniumdizirconium top

Crystal data top

[Ti₂Zr₂(C₃H₇O)₁₂(C₅H₁₁NO₂)₂]	Z = 1
M_r = 1221.57	F(000) = 648
Triclinic, P1	D_x = 1.270 Mg m⁻³
Hall symbol: -P 1	Mo Kα radiation, λ = 0.71073 Å
a = 10.573 (3) Å	Cell parameters from 5923 reflections
b = 11.360 (4) Å	θ = 2.8–25.3°
c = 13.731 (5) Å	µ = 0.61 mm⁻¹
α = 87.593 (5)°	T = 170 K
β = 78.464 (4)°	Rod, colourless
γ = 81.396 (4)°	0.62 × 0.20 × 0.13 mm
V = 1597.7 (9) Å³

Data collection top

Siemens SMART CCD area-detector diffractometer	6398 independent reflections
Radiation source: fine-focus sealed tube	3540 reflections with I > 2σ(I)
Graphite monochromator	R_int = 0.066
Detector resolution: 8.192 pixels mm^-1	θ_max = 26.3°, θ_min = 2.3°
φ and ω scans	h = −6→13
Absorption correction: multi-scan (Blessing, 1995)	k = −14→14
T_min = 0.688, T_max = 0.923	l = −17→17
20444 measured reflections

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)] = 0.068	Hydrogen site location: inferred from neighbouring sites
wR(F²) = 0.215	H-atom parameters constrained
S = 1.02	w = 1/[σ²(F_o²) + (0.1187P)² + 0.4988P] where P = (F_o² + 2F_c²)/3
6398 reflections	(Δ/σ)_max < 0.001
300 parameters	Δρ_max = 0.63 e Å⁻³
7 restraints	Δρ_min = −0.81 e Å⁻³

Special details top

Experimental. Crystal decay was monitored by repeating the initial 10 frames at the end of the data collection and analyzing duplicate reflections. The standard 0.8 mm diameter collimator was used.

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. The meridional (planar) MDEA was modelled with two alternative conformations (a/b) for atoms C1, C72, C81 & C82 with final occupancies 0.731 (7)/0.269 (7) and common U of 0.068 (1) Å². The n-propanolate bound only to Zr (O6) was modelled in two conformations (a/b) to give final occupancis of 0.659 (11)/0.341 (11) and common U of 0.127 (3) Å². The n-propanolate bound to Ti (O1) was modelled in three "interleaving" conformations with a common atom in the three(C12*); the sum total occupancy of all the atoms (C12*, C13A, C13B, C14a)was restrained to a total 2 carbon atoms (SHELXL SUMP)using a fixed U of 0.10 Å². Atom C12* final occupancy was 0.70 (2).

Chemical disorder (iso-/n-propanolate) was modelled for the two other propanolate ligand(s) bound to Ti1. One (O3) was finally modelled by one iso-propanolate (atoms C31, C32a, C33a) and one n-propanolate (C31, C33A, C34B) with full occupancy for C31 and final total occupancies for the remaining atoms of 2 (SHELXL SUMP) function with common U of 0.164 (5) Å². At O2, the final model contained two groups of atoms: the iso-propanolate (C21A, C22A, C23A) and the n-propanolate(C21B, C22B, C23B) with a common U of 0.210 (7) Å² and final occupancies of 0.57 (2)/43 (2) respectively. In addition, the following bond lengths were constrained to be idential (SHELXL SADI option): C61–62 A & C61–62B; C62B—C63B & C62A—C63A; O2–21 A & O2—C21B; C21A—C22A & C21A—C23A; C21B—C22B & C22B—C23B.

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 > 2σ(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	U_iso*/U_eq	Occ. (<1)
Zr1	0.46367 (5)	0.03509 (5)	0.63346 (5)	0.0495 (2)
Ti1	0.27192 (10)	0.23902 (10)	0.75993 (9)	0.0550 (3)
O1	0.1240 (5)	0.1931 (5)	0.8395 (4)	0.0911 (17)
O2	0.3241 (5)	0.3241 (5)	0.8519 (4)	0.0906 (17)
O3	0.1993 (5)	0.3640 (4)	0.6901 (4)	0.0866 (16)
O4	0.4638 (4)	0.2212 (4)	0.6644 (3)	0.0575 (11)
O5	0.2696 (4)	0.1212 (4)	0.6397 (3)	0.0572 (11)
O6	0.6312 (4)	−0.0241 (4)	0.6679 (3)	0.0648 (12)
O7	0.3805 (4)	0.0720 (4)	0.7912 (3)	0.0637 (12)
O8	0.4689 (4)	−0.0979 (3)	0.5199 (3)	0.0564 (11)
N1	0.3742 (5)	−0.1363 (5)	0.7136 (4)	0.0629 (14)
C31	0.1853 (14)	0.4899 (11)	0.6779 (14)	0.164 (6)
C32A	0.227 (2)	0.5144 (18)	0.5710 (15)	0.164 (5)*	0.732 (16)
H32A	0.2254	0.6004	0.5599	0.197*	0.732 (16)
H32B	0.1683	0.4853	0.5340	0.197*	0.732 (16)
H32C	0.3163	0.4738	0.5481	0.197*	0.732 (16)
C33A	0.0382 (17)	0.5483 (16)	0.7072 (15)	0.164 (5)*	0.90 (2)
C41	0.5700 (7)	0.2641 (6)	0.6937 (6)	0.0683 (19)
H41A	0.6530	0.2218	0.6562	0.082*
H41B	0.5671	0.2465	0.7653	0.082*
C42	0.5666 (8)	0.3979 (7)	0.6753 (7)	0.086 (2)
H42A	0.4841	0.4404	0.7133	0.103*
H42B	0.5691	0.4158	0.6038	0.103*
C43	0.6829 (9)	0.4428 (8)	0.7068 (9)	0.118 (4)
H43A	0.6778	0.5288	0.6946	0.142*
H43B	0.7647	0.4021	0.6682	0.142*
H43C	0.6800	0.4259	0.7778	0.142*
C51	0.1961 (6)	0.1466 (6)	0.5630 (5)	0.0612 (17)
H51A	0.2265	0.0858	0.5107	0.073*
H51B	0.2111	0.2251	0.5325	0.073*
C52	0.0508 (6)	0.1479 (8)	0.6032 (6)	0.078 (2)
H52A	0.0363	0.0692	0.6335	0.093*
H52B	0.0211	0.2081	0.6560	0.093*
C53	−0.0296 (7)	0.1754 (9)	0.5242 (7)	0.099 (3)
H53A	−0.1220	0.1761	0.5539	0.118*
H53B	−0.0028	0.1144	0.4727	0.118*
H53C	−0.0163	0.2536	0.4943	0.118*
C61	0.7322 (9)	−0.0376 (10)	0.7224 (9)	0.116 (4)
C71	0.3365 (8)	−0.0151 (7)	0.8603 (6)	0.083 (2)
H71A	0.2399	−0.0046	0.8744	0.100*
H71B	0.3657	−0.0059	0.9234	0.100*
C1A	0.2359 (9)	−0.1338 (9)	0.7075 (10)	0.083 (4)	0.731 (7)
H1A1	0.2052	−0.2065	0.7380	0.099*	0.731 (7)
H1A2	0.2273	−0.1289	0.6377	0.099*	0.731 (7)
H1A3	0.1835	−0.0642	0.7429	0.099*	0.731 (7)
C11A	0.026 (2)	0.270 (2)	0.915 (2)	0.100*	0.45 (2)
C12*	−0.0679 (14)	0.1974 (13)	0.9577 (11)	0.100*	0.698 (16)
C13A	−0.164 (2)	0.2358 (19)	0.8983 (15)	0.100*	0.479 (15)
C14A	−0.1032 (19)	0.1356 (19)	0.8949 (15)	0.100*	0.489 (16)
C21A	0.341 (4)	0.364 (3)	0.950 (2)	0.210 (7)*	0.57 (2)
C22A	0.435 (4)	0.278 (3)	0.985 (3)	0.210 (7)*	0.57 (2)
C23A	0.251 (4)	0.464 (4)	0.987 (3)	0.210 (7)*	0.57 (2)
C62A	0.7809 (17)	−0.1565 (15)	0.7414 (13)	0.127 (4)*	0.659 (11)
H62A	0.8186	−0.1968	0.6774	0.153*	0.659 (11)
H62B	0.7081	−0.1977	0.7757	0.153*	0.659 (11)
C63A	0.8902 (17)	−0.1673 (18)	0.8082 (14)	0.127 (4)*	0.659 (11)
H63A	0.9517	−0.1114	0.7833	0.153*	0.659 (11)
H63B	0.9371	−0.2487	0.8050	0.153*	0.659 (11)
H63C	0.8486	−0.1484	0.8773	0.153*	0.659 (11)
C72A	0.3901 (10)	−0.1390 (9)	0.8192 (7)	0.0680 (14)*	0.731 (7)
H72A	0.4834	−0.1593	0.8230	0.082*	0.731 (7)
H72B	0.3414	−0.1992	0.8577	0.082*	0.731 (7)
C81A	0.4598 (11)	−0.2247 (9)	0.5479 (8)	0.0680 (14)*	0.731 (7)
C82A	0.4578 (10)	−0.2410 (9)	0.6569 (8)	0.0680 (14)*	0.731 (7)
H82A	0.5478	−0.2480	0.6692	0.082*	0.731 (7)
H82B	0.4225	−0.3153	0.6807	0.082*	0.731 (7)
C1B	0.478 (3)	−0.238 (2)	0.724 (2)	0.0680 (14)*	0.269 (7)
H1B1	0.5260	−0.2191	0.7745	0.082*	0.269 (7)
H1B2	0.5390	−0.2519	0.6603	0.082*	0.269 (7)
H1B3	0.4385	−0.3099	0.7448	0.082*	0.269 (7)
C11B	−0.0051 (19)	0.2454 (17)	0.8671 (17)	0.100*	0.55 (2)
C13B	−0.005 (3)	0.199 (3)	1.023 (2)	0.100*	0.334 (14)
C21B	0.345 (5)	0.281 (4)	0.956 (3)	0.210 (7)*	0.43 (2)
C22B	0.379 (5)	0.379 (4)	1.023 (4)	0.210 (7)*	0.43 (2)
C23B	0.341 (5)	0.498 (4)	0.961 (4)	0.210 (7)*	0.43 (2)
C34B	0.024 (4)	0.512 (3)	0.632 (3)	0.164 (5)*	0.370 (19)
H34A	0.1033	0.5170	0.5814	0.197*	0.370 (19)
H34B	−0.0503	0.5607	0.6108	0.197*	0.370 (19)
H34C	0.0089	0.4294	0.6410	0.197*	0.370 (19)
C62B	0.722 (3)	−0.024 (3)	0.821 (2)	0.127 (4)*	0.341 (11)
H62C	0.6537	−0.0682	0.8595	0.153*	0.341 (11)
H62D	0.7014	0.0606	0.8393	0.153*	0.341 (11)
C63B	0.870 (3)	−0.083 (3)	0.839 (3)	0.127 (4)*	0.341 (11)
H63D	0.8617	−0.1473	0.8886	0.153*	0.341 (11)
H63E	0.9111	−0.0211	0.8629	0.153*	0.341 (11)
H63F	0.9230	−0.1145	0.7763	0.153*	0.341 (11)
C72B	0.280 (3)	−0.096 (2)	0.808 (2)	0.0680 (14)*	0.269 (7)
H72C	0.1971	−0.0560	0.7914	0.082*	0.269 (7)
H72D	0.2611	−0.1665	0.8505	0.082*	0.269 (7)
C81B	0.389 (3)	−0.197 (2)	0.537 (2)	0.0680 (14)*	0.269 (7)
H81C	0.3364	−0.1962	0.4854	0.082*	0.269 (7)
H81D	0.4472	−0.2746	0.5348	0.082*	0.269 (7)
C82B	0.303 (3)	−0.182 (3)	0.636 (2)	0.0680 (14)*	0.269 (7)
H82C	0.2745	−0.2588	0.6595	0.082*	0.269 (7)
H82D	0.2251	−0.1241	0.6306	0.082*	0.269 (7)

Atomic displacement parameters (Å²) top

	U¹¹	U²²	U³³	U¹²	U¹³	U²³
Zr1	0.0394 (3)	0.0442 (4)	0.0635 (4)	−0.0038 (2)	−0.0074 (3)	−0.0038 (3)
Ti1	0.0430 (6)	0.0533 (7)	0.0659 (8)	−0.0001 (5)	−0.0065 (5)	−0.0150 (6)
O1	0.054 (3)	0.101 (4)	0.104 (4)	0.004 (3)	0.009 (3)	−0.014 (3)
O2	0.079 (4)	0.096 (4)	0.094 (4)	−0.001 (3)	−0.012 (3)	−0.039 (3)
O3	0.080 (4)	0.060 (3)	0.114 (4)	0.008 (3)	−0.014 (3)	−0.009 (3)
O4	0.048 (2)	0.053 (2)	0.074 (3)	−0.0115 (19)	−0.011 (2)	−0.015 (2)
O5	0.042 (2)	0.058 (3)	0.072 (3)	−0.0067 (19)	−0.010 (2)	−0.005 (2)
O6	0.049 (2)	0.069 (3)	0.076 (3)	−0.001 (2)	−0.016 (2)	0.000 (2)
O7	0.053 (3)	0.066 (3)	0.068 (3)	0.000 (2)	−0.007 (2)	−0.003 (2)
O8	0.059 (3)	0.040 (2)	0.070 (3)	−0.0153 (19)	−0.007 (2)	0.000 (2)
N1	0.057 (3)	0.050 (3)	0.078 (4)	−0.007 (3)	−0.007 (3)	0.003 (3)
C31	0.144 (12)	0.096 (9)	0.245 (18)	−0.007 (8)	−0.027 (11)	−0.004 (10)
C41	0.059 (4)	0.066 (4)	0.084 (5)	−0.016 (3)	−0.015 (4)	−0.016 (4)
C42	0.073 (5)	0.069 (5)	0.121 (7)	−0.019 (4)	−0.018 (5)	−0.025 (5)
C43	0.083 (6)	0.094 (7)	0.189 (11)	−0.035 (5)	−0.031 (7)	−0.043 (7)
C51	0.048 (4)	0.060 (4)	0.077 (5)	−0.002 (3)	−0.019 (3)	−0.003 (3)
C52	0.048 (4)	0.096 (6)	0.086 (6)	−0.004 (4)	−0.012 (4)	−0.004 (4)
C53	0.051 (4)	0.125 (8)	0.119 (7)	0.003 (5)	−0.027 (5)	−0.005 (6)
C61	0.085 (6)	0.145 (9)	0.136 (9)	−0.035 (6)	−0.059 (6)	0.047 (7)
C71	0.089 (6)	0.089 (6)	0.064 (5)	−0.008 (5)	−0.003 (4)	0.008 (4)
C1A	0.061 (6)	0.063 (6)	0.124 (10)	−0.025 (5)	−0.011 (6)	0.023 (6)

Geometric parameters (Å, º) top

Zr1—O6	1.940 (4)	C52—H52B	0.9900
Zr1—O5	2.124 (4)	C53—H53A	0.9800
Zr1—O4	2.174 (4)	C53—H53B	0.9800
Zr1—O7	2.201 (5)	C53—H53C	0.9800
Zr1—O8	2.203 (4)	C61—C62B	1.35 (2)
Zr1—O8ⁱ	2.209 (4)	C61—C62A	1.404 (16)
Zr1—N1	2.418 (5)	C71—C72B	1.46 (3)
Ti1—O2	1.837 (5)	C71—C72A	1.524 (12)
Ti1—O3	1.839 (5)	C71—H71A	0.9900
Ti1—O1	1.851 (5)	C71—H71B	0.9900
Ti1—O7	2.140 (4)	C1A—H1A1	0.9800
Ti1—O4	2.171 (4)	C1A—H1A2	0.9800
Ti1—O5	2.174 (4)	C1A—H1A3	0.9800
O1—C11B	1.388 (19)	C11A—C12*	1.40 (3)
O1—C11A	1.52 (2)	C12*—C14A	1.28 (2)
O2—C21A	1.50 (3)	C12*—C13A	1.44 (2)
O2—C21B	1.54 (3)	C13A—C14A	1.22 (2)
O3—C31	1.422 (13)	C21A—C23A	1.40 (3)
O4—C41	1.422 (7)	C21A—C22A	1.42 (3)
O5—C51	1.425 (7)	C62A—C63A	1.602 (19)
O6—C61	1.409 (9)	C62A—H62A	0.9900
O7—C71	1.407 (9)	C62A—H62B	0.9900
O8—C81A	1.488 (11)	C63A—H63A	0.9800
O8—C81B	1.49 (3)	C63A—H63B	0.9800
O8—Zr1ⁱ	2.209 (4)	C63A—H63C	0.9800
N1—C1A	1.477 (10)	C72A—H72A	0.9900
N1—C72A	1.492 (11)	C72A—H72B	0.9900
N1—C1B	1.50 (3)	C81A—C82A	1.497 (14)
N1—C72B	1.50 (3)	C82A—H82A	0.9900
N1—C82A	1.513 (11)	C82A—H82B	0.9900
N1—C82B	1.56 (3)	C1B—H1B1	0.9800
C31—C32A	1.47 (2)	C1B—H1B2	0.9800
C31—C33A	1.58 (2)	C1B—H1B3	0.9800
C32A—H32A	0.9800	C21B—C22B	1.60 (5)
C32A—H32B	0.9800	C22B—C23B	1.61 (5)
C32A—H32C	0.9800	C34B—H34A	0.9800
C33A—C34B	1.17 (4)	C34B—H34B	0.9800
C41—C42	1.527 (10)	C34B—H34C	0.9800
C41—H41A	0.9900	C62B—C63B	1.67 (3)
C41—H41B	0.9900	C62B—H62C	0.9900
C42—C43	1.542 (10)	C62B—H62D	0.9900
C42—H42A	0.9900	C63B—H63D	0.9800
C42—H42B	0.9900	C63B—H63E	0.9800
C43—H43A	0.9800	C63B—H63F	0.9800
C43—H43B	0.9800	C72B—H72C	0.9900
C43—H43C	0.9800	C72B—H72D	0.9900
C51—C52	1.524 (9)	C81B—C82B	1.47 (4)
C51—H51A	0.9900	C81B—H81C	0.9900
C51—H51B	0.9900	C81B—H81D	0.9900
C52—C53	1.503 (10)	C82B—H82C	0.9900
C52—H52A	0.9900	C82B—H82D	0.9900

O6—Zr1—O5	162.60 (18)	O5—C51—H51A	109.3
O6—Zr1—O4	96.50 (18)	C52—C51—H51A	109.3
O5—Zr1—O4	73.58 (15)	O5—C51—H51B	109.3
O6—Zr1—O7	89.80 (18)	C52—C51—H51B	109.3
O5—Zr1—O7	73.46 (16)	H51A—C51—H51B	108.0
O4—Zr1—O7	69.80 (17)	C53—C52—C51	112.7 (7)
O6—Zr1—O8	97.57 (18)	C53—C52—H52A	109.0
O5—Zr1—O8	98.39 (16)	C51—C52—H52A	109.0
O4—Zr1—O8	146.61 (17)	C53—C52—H52B	109.0
O7—Zr1—O8	140.14 (16)	C51—C52—H52B	109.0
O6—Zr1—O8ⁱ	99.39 (18)	H52A—C52—H52B	107.8
O5—Zr1—O8ⁱ	93.29 (16)	C52—C53—H53A	109.5
O4—Zr1—O8ⁱ	81.30 (16)	C52—C53—H53B	109.5
O7—Zr1—O8ⁱ	150.52 (17)	H53A—C53—H53B	109.5
O8—Zr1—O8ⁱ	66.62 (17)	C52—C53—H53C	109.5
O6—Zr1—N1	90.47 (19)	H53A—C53—H53C	109.5
O5—Zr1—N1	88.20 (18)	H53B—C53—H53C	109.5
O4—Zr1—N1	138.97 (18)	C62B—C61—C62A	84.4 (17)
O7—Zr1—N1	69.84 (19)	C62B—C61—O6	127.9 (16)
O8—Zr1—N1	70.98 (18)	C62A—C61—O6	114.3 (11)
O8ⁱ—Zr1—N1	137.33 (17)	O7—C71—C72B	107.2 (12)
O2—Ti1—O3	98.9 (3)	O7—C71—C72A	110.0 (7)
O2—Ti1—O1	98.7 (3)	O7—C71—H71A	109.7
O3—Ti1—O1	100.9 (3)	O7—C71—H71B	109.7
O2—Ti1—O7	95.8 (2)	C72A—C71—H71B	109.7
O3—Ti1—O7	160.6 (2)	H71A—C71—H71B	108.2
O1—Ti1—O7	89.5 (2)	N1—C1A—H1A1	109.5
O2—Ti1—O4	92.2 (2)	N1—C1A—H1A2	109.5
O3—Ti1—O4	95.6 (2)	N1—C1A—H1A3	109.5
O1—Ti1—O4	158.5 (2)	C12*—C11A—O1	105.6 (17)
O7—Ti1—O4	71.01 (17)	C14A—C12*—C11A	114.3 (19)
O2—Ti1—O5	163.6 (2)	C11A—C12*—C13A	99.1 (16)
O3—Ti1—O5	89.1 (2)	C23A—C21A—C22A	138 (3)
O1—Ti1—O5	93.8 (2)	C23A—C21A—O2	113 (3)
O7—Ti1—O5	73.69 (17)	C22A—C21A—O2	108 (3)
O4—Ti1—O5	72.66 (15)	C61—C62A—C63A	112.4 (13)
C11B—O1—Ti1	134.7 (9)	C61—C62A—H62A	109.1
C11A—O1—Ti1	126.0 (10)	C63A—C62A—H62A	109.1
C21A—O2—Ti1	160.1 (16)	C61—C62A—H62B	109.1
C21B—O2—Ti1	126.8 (18)	C63A—C62A—H62B	109.1
C31—O3—Ti1	143.3 (8)	H62A—C62A—H62B	107.8
C41—O4—Ti1	121.3 (4)	N1—C72A—C71	106.8 (7)
C41—O4—Zr1	123.3 (4)	N1—C72A—H72A	110.4
Ti1—O4—Zr1	93.51 (16)	C71—C72A—H72A	110.4
C51—O5—Zr1	130.4 (4)	N1—C72A—H72B	110.4
C51—O5—Ti1	126.1 (4)	C71—C72A—H72B	110.4
Zr1—O5—Ti1	94.85 (16)	H72A—C72A—H72B	108.6
C61—O6—Zr1	158.4 (6)	O8—C81A—C82A	109.1 (8)
C71—O7—Ti1	126.7 (4)	C81A—C82A—N1	110.3 (8)
C71—O7—Zr1	123.5 (4)	C81A—C82A—H82A	109.6
Ti1—O7—Zr1	93.61 (18)	N1—C82A—H82A	109.6
C81A—O8—Zr1	121.0 (5)	C81A—C82A—H82B	109.6
C81B—O8—Zr1	123.1 (11)	N1—C82A—H82B	109.6
C81A—O8—Zr1ⁱ	124.0 (5)	H82A—C82A—H82B	108.1
C81B—O8—Zr1ⁱ	119.6 (11)	N1—C1B—H1B1	109.5
Zr1—O8—Zr1ⁱ	113.38 (17)	N1—C1B—H1B2	109.5
C1A—N1—C72A	110.9 (7)	H1B1—C1B—H1B2	109.5
C1B—N1—C72B	116.0 (16)	N1—C1B—H1B3	109.5
C1A—N1—C82A	110.5 (7)	H1B1—C1B—H1B3	109.5
C72A—N1—C82A	111.2 (6)	H1B2—C1B—H1B3	109.5
C72B—N1—C82A	145.7 (12)	C22B—C21B—O2	116 (3)
C72A—N1—C82B	146.6 (12)	C21B—C22B—C23B	100 (4)
C1B—N1—C82B	103.5 (16)	C33A—C34B—H34A	109.5
C72B—N1—C82B	111.7 (15)	C33A—C34B—H34B	109.5
C1A—N1—Zr1	112.4 (5)	H34A—C34B—H34B	109.5
C72A—N1—Zr1	107.6 (5)	C33A—C34B—H34C	109.5
C1B—N1—Zr1	112.1 (11)	H34A—C34B—H34C	109.5
C72B—N1—Zr1	108.6 (11)	H34B—C34B—H34C	109.5
C82A—N1—Zr1	104.0 (5)	C61—C62B—C63B	103 (2)
C82B—N1—Zr1	104.3 (11)	C61—C62B—H62C	111.2
O3—C31—C32A	106.8 (14)	C63B—C62B—H62C	111.2
O3—C31—C33A	111.5 (12)	C61—C62B—H62D	111.2
C32A—C31—C33A	106.6 (15)	C63B—C62B—H62D	111.2
C31—C32A—H32A	109.5	H62C—C62B—H62D	109.1
C31—C32A—H32B	109.5	C62B—C63B—H63D	109.5
H32A—C32A—H32B	109.5	C62B—C63B—H63E	109.5
C31—C32A—H32C	109.5	H63D—C63B—H63E	109.5
H32A—C32A—H32C	109.5	C62B—C63B—H63F	109.5
H32B—C32A—H32C	109.5	H63D—C63B—H63F	109.5
C34B—C33A—C31	87 (3)	H63E—C63B—H63F	109.5
O4—C41—C42	112.0 (6)	C71—C72B—N1	109.6 (17)
O4—C41—H41A	109.2	C71—C72B—H72C	109.8
C42—C41—H41A	109.2	N1—C72B—H72C	109.8
O4—C41—H41B	109.2	C71—C72B—H72D	109.8
C42—C41—H41B	109.2	N1—C72B—H72D	109.8
H41A—C41—H41B	107.9	H72C—C72B—H72D	108.2
C41—C42—C43	111.3 (7)	C82B—C81B—O8	108 (2)
C41—C42—H42A	109.4	C82B—C81B—H81C	110.1
C43—C42—H42A	109.4	O8—C81B—H81C	110.1
C41—C42—H42B	109.4	C82B—C81B—H81D	110.1
C43—C42—H42B	109.4	O8—C81B—H81D	110.1
H42A—C42—H42B	108.0	H81C—C81B—H81D	108.4
C42—C43—H43A	109.5	C81B—C82B—N1	112 (2)
C42—C43—H43B	109.5	C81B—C82B—H82C	109.3
H43A—C43—H43B	109.5	N1—C82B—H82C	109.3
C42—C43—H43C	109.5	C81B—C82B—H82D	109.3
H43A—C43—H43C	109.5	N1—C82B—H82D	109.3
H43B—C43—H43C	109.5	H82C—C82B—H82D	107.9
O5—C51—C52	111.4 (6)

O2—Ti1—O1—C11B	84.7 (16)	O5—Zr1—O8—Zr1ⁱ	90.0 (2)
O3—Ti1—O1—C11B	−16.1 (16)	O4—Zr1—O8—Zr1ⁱ	17.2 (4)
O7—Ti1—O1—C11B	−179.5 (15)	O7—Zr1—O8—Zr1ⁱ	164.16 (18)
O4—Ti1—O1—C11B	−155.6 (15)	N1—Zr1—O8—Zr1ⁱ	175.1 (2)
O5—Ti1—O1—C11B	−105.9 (15)	O6—Zr1—N1—C1A	−179.9 (7)
O2—Ti1—O1—C11A	40.4 (14)	O5—Zr1—N1—C1A	17.4 (6)
O3—Ti1—O1—C11A	−60.5 (14)	O4—Zr1—N1—C1A	79.6 (7)
O7—Ti1—O1—C11A	136.1 (14)	O7—Zr1—N1—C1A	90.4 (6)
O4—Ti1—O1—C11A	160.1 (14)	O8—Zr1—N1—C1A	−82.1 (6)
O5—Ti1—O1—C11A	−150.2 (14)	O8ⁱ—Zr1—N1—C1A	−75.5 (7)
O3—Ti1—O2—C21A	129 (4)	O6—Zr1—N1—C72A	57.7 (5)
O1—Ti1—O2—C21A	26 (4)	O5—Zr1—N1—C72A	−105.0 (5)
O7—Ti1—O2—C21A	−64 (4)	O4—Zr1—N1—C72A	−42.8 (6)
O4—Ti1—O2—C21A	−135 (4)	O7—Zr1—N1—C72A	−32.0 (5)
O5—Ti1—O2—C21A	−113 (4)	O8—Zr1—N1—C72A	155.5 (5)
O3—Ti1—O2—C21B	155 (3)	O8ⁱ—Zr1—N1—C72A	162.1 (5)
O1—Ti1—O2—C21B	53 (3)	O6—Zr1—N1—C1B	−20.7 (13)
O7—Ti1—O2—C21B	−38 (3)	O5—Zr1—N1—C1B	176.7 (13)
O4—Ti1—O2—C21B	−109 (3)	O4—Zr1—N1—C1B	−121.2 (13)
O5—Ti1—O2—C21B	−87 (3)	O7—Zr1—N1—C1B	−110.3 (13)
O2—Ti1—O3—C31	9.5 (13)	O8—Zr1—N1—C1B	77.2 (13)
O1—Ti1—O3—C31	110.2 (13)	O8ⁱ—Zr1—N1—C1B	83.8 (13)
O7—Ti1—O3—C31	−128.8 (13)	O6—Zr1—N1—C72B	108.8 (12)
O4—Ti1—O3—C31	−83.6 (13)	O5—Zr1—N1—C72B	−53.8 (12)
O5—Ti1—O3—C31	−156.1 (13)	O4—Zr1—N1—C72B	8.3 (12)
O2—Ti1—O4—C41	4.3 (5)	O7—Zr1—N1—C72B	19.2 (12)
O3—Ti1—O4—C41	103.4 (5)	O8—Zr1—N1—C72B	−153.3 (12)
O1—Ti1—O4—C41	−116.5 (7)	O8ⁱ—Zr1—N1—C72B	−146.7 (11)
O7—Ti1—O4—C41	−91.1 (5)	O6—Zr1—N1—C82A	−60.4 (5)
O5—Ti1—O4—C41	−169.3 (5)	O5—Zr1—N1—C82A	136.9 (5)
O2—Ti1—O4—Zr1	137.2 (2)	O4—Zr1—N1—C82A	−160.9 (5)
O3—Ti1—O4—Zr1	−123.7 (2)	O7—Zr1—N1—C82A	−150.0 (5)
O1—Ti1—O4—Zr1	16.4 (7)	O8—Zr1—N1—C82A	37.4 (5)
O7—Ti1—O4—Zr1	41.84 (16)	O8ⁱ—Zr1—N1—C82A	44.0 (6)
O5—Ti1—O4—Zr1	−36.41 (16)	O6—Zr1—N1—C82B	−132.0 (12)
O6—Zr1—O4—C41	3.3 (5)	O5—Zr1—N1—C82B	65.4 (12)
O5—Zr1—O4—C41	168.7 (5)	O4—Zr1—N1—C82B	127.6 (12)
O7—Zr1—O4—C41	90.7 (5)	O7—Zr1—N1—C82B	138.4 (12)
O8—Zr1—O4—C41	−111.1 (5)	O8—Zr1—N1—C82B	−34.1 (12)
O8ⁱ—Zr1—O4—C41	−95.2 (5)	O8ⁱ—Zr1—N1—C82B	−27.5 (12)
N1—Zr1—O4—C41	101.6 (5)	Ti1—O3—C31—C32A	127.2 (14)
O6—Zr1—O4—Ti1	−128.18 (18)	Ti1—O3—C31—C33A	−116.7 (13)
O5—Zr1—O4—Ti1	37.21 (17)	O3—C31—C33A—C34B	−75 (3)
O7—Zr1—O4—Ti1	−40.80 (15)	C32A—C31—C33A—C34B	41 (3)
O8—Zr1—O4—Ti1	117.4 (3)	Ti1—O4—C41—C42	−81.1 (7)
O8ⁱ—Zr1—O4—Ti1	133.27 (17)	Zr1—O4—C41—C42	159.9 (5)
N1—Zr1—O4—Ti1	−29.9 (3)	O4—C41—C42—C43	−179.6 (7)
O6—Zr1—O5—C51	167.7 (6)	Zr1—O5—C51—C52	150.1 (5)
O4—Zr1—O5—C51	110.8 (5)	Ti1—O5—C51—C52	−70.7 (7)
O7—Zr1—O5—C51	−175.9 (5)	O5—C51—C52—C53	179.6 (6)
O8—Zr1—O5—C51	−36.0 (5)	Zr1—O6—C61—C62B	28 (3)
O8ⁱ—Zr1—O5—C51	30.9 (5)	Zr1—O6—C61—C62A	130.9 (15)
N1—Zr1—O5—C51	−106.4 (5)	Ti1—O7—C71—C72B	91.0 (13)
O6—Zr1—O5—Ti1	19.7 (7)	Zr1—O7—C71—C72B	−34.9 (13)
O4—Zr1—O5—Ti1	−37.21 (17)	Ti1—O7—C71—C72A	142.5 (6)
O7—Zr1—O5—Ti1	36.05 (17)	Zr1—O7—C71—C72A	16.5 (9)
O8—Zr1—O5—Ti1	176.02 (15)	C11B—O1—C11A—C12*	62 (2)
O8ⁱ—Zr1—O5—Ti1	−117.15 (16)	Ti1—O1—C11A—C12*	−179.4 (10)
N1—Zr1—O5—Ti1	105.54 (19)	O1—C11A—C12*—C14A	−43 (2)
O2—Ti1—O5—C51	−135.9 (9)	O1—C11A—C12*—C13A	−96.7 (18)
O3—Ti1—O5—C51	−16.4 (5)	C11A—C12*—C13A—C14A	113.6 (19)
O1—Ti1—O5—C51	84.5 (5)	C11A—C12*—C14A—C13A	−82.9 (19)
O7—Ti1—O5—C51	172.8 (5)	C21B—O2—C21A—C23A	−134 (7)
O4—Ti1—O5—C51	−112.5 (5)	Ti1—O2—C21A—C23A	−98 (5)
O2—Ti1—O5—Zr1	14.2 (9)	C21B—O2—C21A—C22A	38 (4)
O3—Ti1—O5—Zr1	133.7 (2)	Ti1—O2—C21A—C22A	75 (5)
O1—Ti1—O5—Zr1	−125.5 (2)	C62B—C61—C62A—C63A	−47.7 (19)
O7—Ti1—O5—Zr1	−37.20 (17)	O6—C61—C62A—C63A	−177.0 (12)
O4—Ti1—O5—Zr1	37.50 (17)	C1A—N1—C72A—C71	−73.1 (9)
O5—Zr1—O6—C61	−10.2 (17)	C1B—N1—C72A—C71	158.6 (13)
O4—Zr1—O6—C61	43.8 (14)	C72B—N1—C72A—C71	−49.3 (14)
O7—Zr1—O6—C61	−25.9 (14)	C82A—N1—C72A—C71	163.5 (7)
O8—Zr1—O6—C61	−166.6 (14)	C82B—N1—C72A—C71	−113 (2)
O8ⁱ—Zr1—O6—C61	126.0 (14)	Zr1—N1—C72A—C71	50.2 (8)
N1—Zr1—O6—C61	−95.7 (14)	O7—C71—C72A—N1	−44.4 (9)
O2—Ti1—O7—C71	90.9 (6)	C72B—C71—C72A—N1	51.3 (15)
O3—Ti1—O7—C71	−130.3 (8)	C81B—O8—C81A—C82A	−108 (3)
O1—Ti1—O7—C71	−7.7 (6)	Zr1—O8—C81A—C82A	−4.1 (10)
O4—Ti1—O7—C71	−178.7 (6)	Zr1ⁱ—O8—C81A—C82A	160.0 (6)
O5—Ti1—O7—C71	−101.8 (6)	O8—C81A—C82A—N1	40.3 (10)
O2—Ti1—O7—Zr1	−131.6 (2)	C1A—N1—C82A—C81A	67.0 (10)
O3—Ti1—O7—Zr1	7.1 (7)	C72A—N1—C82A—C81A	−169.4 (8)
O1—Ti1—O7—Zr1	129.8 (2)	C1B—N1—C82A—C81A	−162 (2)
O4—Ti1—O7—Zr1	−41.22 (15)	C72B—N1—C82A—C81A	144 (2)
O5—Ti1—O7—Zr1	35.62 (16)	C82B—N1—C82A—C81A	46.4 (13)
O6—Zr1—O7—C71	−82.1 (5)	Zr1—N1—C82A—C81A	−53.9 (8)
O5—Zr1—O7—C71	102.8 (5)	C21A—O2—C21B—C22B	−10 (3)
O4—Zr1—O7—C71	−179.1 (5)	Ti1—O2—C21B—C22B	−175 (3)
O8—Zr1—O7—C71	19.6 (6)	O2—C21B—C22B—C23B	13 (5)
O8ⁱ—Zr1—O7—C71	169.0 (5)	C62A—C61—C62B—C63B	51 (2)
N1—Zr1—O7—C71	8.5 (5)	O6—C61—C62B—C63B	167.4 (16)
O6—Zr1—O7—Ti1	138.52 (19)	O7—C71—C72B—N1	50.1 (19)
O5—Zr1—O7—Ti1	−36.65 (16)	C72A—C71—C72B—N1	−51.8 (13)
O4—Zr1—O7—Ti1	41.52 (16)	C1A—N1—C72B—C71	−151 (2)
O8—Zr1—O7—Ti1	−119.9 (2)	C72A—N1—C72B—C71	53.6 (14)
O8ⁱ—Zr1—O7—Ti1	29.5 (4)	C1B—N1—C72B—C71	83 (2)
N1—Zr1—O7—Ti1	−130.9 (2)	C82A—N1—C72B—C71	117.4 (19)
O6—Zr1—O8—C81A	68.7 (6)	C82B—N1—C72B—C71	−158.3 (17)
O5—Zr1—O8—C81A	−104.4 (6)	Zr1—N1—C72B—C71	−43.8 (19)
O4—Zr1—O8—C81A	−177.2 (5)	C81A—O8—C81B—C82B	101 (3)
O7—Zr1—O8—C81A	−30.2 (6)	Zr1—O8—C81B—C82B	5 (3)
O8ⁱ—Zr1—O8—C81A	165.7 (6)	Zr1ⁱ—O8—C81B—C82B	−151.0 (16)
N1—Zr1—O8—C81A	−19.2 (6)	O8—C81B—C82B—N1	−39 (3)
O6—Zr1—O8—C81B	105.7 (14)	C1A—N1—C82B—C81B	159 (3)
O5—Zr1—O8—C81B	−67.4 (14)	C72A—N1—C82B—C81B	−145.7 (18)
O4—Zr1—O8—C81B	−140.2 (14)	C1B—N1—C82B—C81B	−66 (2)
O7—Zr1—O8—C81B	6.8 (14)	C72B—N1—C82B—C81B	168 (2)
O8ⁱ—Zr1—O8—C81B	−157.3 (14)	C82A—N1—C82B—C81B	−48.6 (19)
N1—Zr1—O8—C81B	17.8 (14)	Zr1—N1—C82B—C81B	51 (2)
O6—Zr1—O8—Zr1ⁱ	−97.0 (2)

Symmetry code: (i) −x+1, −y, −z+1.

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A centrosymmetric triply alkoxo-bridged titanium-μ2-O-zirconium tetranuclear complex: [TiZr(μ2-O,μ2-O′-methyl­imino­diethano­late)(μ2-O-n-propanolate)2(n-propanolate)2.7(isopropanolate)1.3]2

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A centrosymmetric triply alkoxo-bridged titanium-μ₂-O-zirconium tetranuclear complex: [TiZr(μ₂-O,μ₂-O′-methyliminodiethanolate)(μ₂-O-n-propanolate)₂(n-propanolate)_2.7(isopropanolate)_1.3]₂