Di-μ-chloro-bis­{chloro­[hydro­tris(pyrazol-1-yl)borato)](tetra­hydro­furan)ytterbium(III)} toluene solvate

The mol­ecular structure of the tetra­hydro­furan adduct of the first dimeric mono[tris­(pyrazolyl)borate] (Tp) lanthanide compound of composition [Yb₂(C₉H₁₀BN₆)₂Cl₄(C₄H₈O)₂]·C₇H₈ is reported. The dimeric and centrosymmetric mono-Tp complex features a seven-coordinate Yb atom, bonded to three N atoms of the tridentate ligand, to the O atom of the neutral tetra­hydro­furan ligand, and to one terminal as well as to two bridging Cl atoms. Additionally, a disordered toluene solvent mol­ecule, located on an inversion center, is cocrystallized.

Key indicators

• Single-crystal X-ray study
• T = 100 K
• Mean [sigma](C-C) = 0.008 Å
• H-atom completeness 82%
• Disorder in solvent or counterion
• R factor = 0.041
• wR factor = 0.104
• Data-to-parameter ratio = 16.1

checkCIF/PLATON results

No syntax errors found



Alert level A
PLAT773_ALERT_2_A Suspect C-C Bond in CIF:      C41    -C41     ..       1.75 Ang.

Author Response: part of disorder model for toluene

Alert level C
PLAT041_ALERT_1_C Calc. and Rep. SumFormula Strings    Differ ....          ?
PLAT066_ALERT_1_C Predicted and Reported Transmissions Identical .          ?
PLAT068_ALERT_1_C Reported F000 Differs from Calcd (or Missing)...          ?
PLAT243_ALERT_4_C High  'Solvent' Ueq as Compared to Neighbors for        C42
PLAT244_ALERT_4_C Low   'Solvent' Ueq as Compared to Neighbors for        C41
PLAT302_ALERT_4_C Anion/Solvent Disorder .........................      30.00 Perc.
PLAT720_ALERT_4_C Number of Unusual/Non-Standard Label(s) ........          1
PLAT764_ALERT_4_C Overcomplete CIF Bond List Detected (Rep/Expd) .       1.13 Ratio

Alert level G
FORMU01_ALERT_2_G  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:C33 H44 B2 Cl4 N12 O2 Yb2
            Atom count from the _atom_site data:  C33 H36 B2 Cl4 N12 O2 Yb2
CELLZ01_ALERT_1_G Difference between formula and atom_site contents detected.
CELLZ01_ALERT_1_G WARNING: H atoms missing from atom site list. Is this intentional?
           From the CIF: _cell_formula_units_Z    1
           From the CIF: _chemical_formula_sum  C33 H44 B2 Cl4 N12 O2 Yb2
           TEST: Compare cell contents of formula and atom_site data

           atom    Z*formula  cif sites diff
           C         33.00     33.00    0.00
           H         44.00     36.00    8.00
           B          2.00      2.00    0.00
           Cl         4.00      4.00    0.00
           N         12.00     12.00    0.00
           O          2.00      2.00    0.00
           Yb         2.00      2.00    0.00

   1 ALERT level A = In general: serious problem
   0 ALERT level B = Potentially serious problem
   8 ALERT level C = Check and explain
   3 ALERT level G = General alerts; check

   5 ALERT type 1 CIF construction/syntax error, inconsistent or missing data
   2 ALERT type 2 Indicator that the structure model may be wrong or deficient
   0 ALERT type 3 Indicator that the structure quality may be low
   5 ALERT type 4 Improvement, methodology, query or suggestion
   0 ALERT type 5 Informative message, check

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Computing details

Data collection: SMART (Bruker, 2005); cell refinement: SAINT (Bruker, 2005); data reduction: SAINT; program(s) used to solve structure: SHELXS97 (Sheldrick, 1997); program(s) used to refine structure: SHELXL97 (Sheldrick, 1997); molecular graphics: XP in SHELXTL (Bruker, 2005); software used to prepare material for publication: SHELXTL.

Di-µ-chloro-bis{chloro[hydrotris(pyrazol-1- yl)borato)](tetrahydrofuran)ytterbium(III)] toluene solvate

Crystal data

[Yb2(C9H10BN6)2Cl4(C4H8O)2]·C7H8	Z = 1
Mr = 1150.30	F(000) = 560
Triclinic, P1	Dx = 1.825 Mg m^−3
Hall symbol: -P 1	Mo Kα radiation, λ = 0.71073 Å
a = 9.209 (3) Å	Cell parameters from 5645 reflections
b = 10.919 (3) Å	θ = 2.2–28.2°
c = 11.881 (3) Å	µ = 4.74 mm^−1
α = 105.733 (4)°	T = 100 K
β = 105.648 (4)°	Blade, colourless
γ = 103.250 (4)°	0.30 × 0.10 × 0.05 mm
V = 1046.7 (5) Å^3

Data collection

Bruker SMART APEX CCD diffractometer	4221 independent reflections
Radiation source: fine-focus sealed tube	4053 reflections with I > 2σ(I)
Graphite monochromator	Rint = 0.024
φ and ω scans	θmax = 28.2°, θmin = 2.1°
Absorption correction: multi-scan (SADABS; Sheldrick, 1996)	h = −11→11
Tmin = 0.574, Tmax = 0.789	k = −13→14
6253 measured reflections	l = −14→12

Refinement

Refinement on F^2	Primary atom site location: structure-invariant direct methods
Least-squares matrix: full	Secondary atom site location: difference Fourier map
R[F^2 > 2σ(F^2)] = 0.041	Hydrogen site location: inferred from neighbouring sites
wR(F^2) = 0.104	H-atom parameters constrained
S = 1.06	w = 1/[σ^2(Fo^2) + (0.08P)^2 + 0.69P] where P = (Fo^2 + 2Fc^2)/3
4221 reflections	(Δ/σ)max = 0.013
262 parameters	Δρmax = 2.99 e Å^−3
0 restraints	Δρmin = −2.80 e Å^−3

Special details

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. Toluene disorder on inversion center. Fully modeled. H atoms neglected in final model but included in all intensive calculations. 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 > σ(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 (Ų)

	x	y	z	Uiso*/Ueq	Occ. (<1)
Yb1	0.352000 (18)	0.432548 (15)	0.303116 (15)	0.01902 (10)
Cl1	0.35125 (13)	0.42505 (11)	0.52895 (10)	0.0254 (2)
Cl2	0.30855 (16)	0.65200 (13)	0.29849 (14)	0.0348 (3)
O1	0.0858 (4)	0.3452 (3)	0.2884 (3)	0.0245 (7)
N1	0.1777 (4)	0.3181 (4)	0.0876 (4)	0.0235 (8)
N2	0.2036 (5)	0.2223 (4)	0.0025 (4)	0.0231 (8)
N3	0.5186 (4)	0.4346 (4)	0.1779 (4)	0.0230 (8)
N4	0.4979 (5)	0.3258 (4)	0.0778 (4)	0.0227 (8)
N5	0.3854 (5)	0.2163 (4)	0.2630 (4)	0.0234 (8)
N6	0.3793 (5)	0.1415 (4)	0.1480 (4)	0.0236 (8)
C1	0.0350 (5)	0.3282 (5)	0.0266 (5)	0.0282 (10)
H1A	−0.0146	0.3874	0.0630	0.034*
C2	−0.0275 (6)	0.2392 (5)	−0.0969 (5)	0.0300 (11)
H2A	−0.1249	0.2262	−0.1595	0.036*
C3	0.0821 (7)	0.1740 (5)	−0.1085 (5)	0.0313 (12)
H3A	0.0737	0.1064	−0.1822	0.038*
C4	0.6361 (5)	0.5352 (5)	0.1815 (5)	0.0262 (10)
H4A	0.6746	0.6240	0.2412	0.031*
C5	0.6946 (6)	0.4935 (5)	0.0874 (5)	0.0282 (10)
H5A	0.7792	0.5452	0.0711	0.034*
C6	0.6030 (6)	0.3602 (5)	0.0224 (5)	0.0270 (10)
H6A	0.6122	0.3023	−0.0493	0.032*
C7	0.4114 (6)	0.1450 (5)	0.3369 (5)	0.0274 (10)
H7A	0.4222	0.1739	0.4226	0.033*
C8	0.4207 (6)	0.0219 (5)	0.2707 (5)	0.0312 (11)
H8A	0.4373	−0.0479	0.3007	0.037*
C9	0.4002 (6)	0.0243 (5)	0.1521 (5)	0.0279 (10)
H9A	0.4007	−0.0455	0.0841	0.034*
C10	−0.0080 (6)	0.4216 (5)	0.3385 (5)	0.0291 (10)
H10A	−0.0439	0.4729	0.2858	0.035*
H10B	0.0555	0.4852	0.4248	0.035*
C11	−0.1500 (6)	0.3166 (6)	0.3369 (6)	0.0374 (12)
H11A	−0.1297	0.3050	0.4189	0.045*
H11B	−0.2477	0.3420	0.3157	0.045*
C12	−0.1650 (6)	0.1896 (5)	0.2362 (5)	0.0349 (12)
H12A	−0.2207	0.1080	0.2485	0.042*
H12B	−0.2227	0.1873	0.1518	0.042*
C13	0.0067 (6)	0.2018 (5)	0.2548 (5)	0.0274 (10)
H13A	0.0523	0.1701	0.3225	0.033*
H13B	0.0170	0.1489	0.1769	0.033*
C40	0.9745 (18)	0.1517 (12)	0.5721 (11)	0.046 (3)	0.50
C41	0.9213 (14)	0.0283 (11)	0.5096 (9)	0.033 (2)	0.50
C42	0.8019 (11)	0.0678 (9)	0.5189 (8)	0.060 (2)
C43	1.0911 (8)	0.1120 (6)	0.5620 (5)	0.0449 (15)
C44	0.7890 (15)	−0.0736 (13)	0.4458 (13)	0.043 (3)	0.50
B1	0.3613 (7)	0.1931 (5)	0.0376 (5)	0.0252 (11)
H1B1	0.3648	0.1244	−0.0361	0.030*

Atomic displacement parameters (Ų)

	U^11	U^22	U^33	U^12	U^13	U^23
Yb1	0.01447 (14)	0.01624 (14)	0.01964 (14)	0.00165 (9)	0.00112 (10)	0.00395 (9)
Cl1	0.0172 (5)	0.0281 (5)	0.0207 (5)	−0.0013 (4)	0.0011 (4)	0.0059 (4)
Cl2	0.0312 (6)	0.0229 (6)	0.0432 (7)	0.0086 (5)	0.0023 (6)	0.0120 (5)
O1	0.0166 (15)	0.0224 (16)	0.0260 (16)	0.0033 (12)	0.0037 (13)	0.0023 (13)
N1	0.0161 (18)	0.0255 (19)	0.0228 (19)	0.0020 (15)	0.0019 (16)	0.0082 (16)
N2	0.0201 (19)	0.0169 (17)	0.0205 (18)	−0.0016 (15)	−0.0005 (16)	0.0030 (14)
N3	0.0177 (18)	0.0203 (18)	0.0217 (18)	0.0014 (15)	0.0008 (16)	0.0037 (15)
N4	0.0223 (19)	0.0187 (18)	0.0234 (18)	0.0050 (15)	0.0061 (16)	0.0052 (15)
N5	0.0192 (19)	0.0220 (19)	0.0243 (19)	0.0034 (15)	0.0048 (17)	0.0066 (16)
N6	0.0196 (18)	0.0167 (17)	0.0273 (19)	0.0031 (14)	0.0044 (16)	0.0029 (15)
C1	0.018 (2)	0.035 (3)	0.030 (2)	0.009 (2)	0.002 (2)	0.014 (2)
C2	0.015 (2)	0.031 (3)	0.029 (2)	−0.0049 (18)	−0.005 (2)	0.011 (2)
C3	0.030 (3)	0.020 (2)	0.025 (2)	−0.004 (2)	−0.005 (2)	0.0039 (19)
C4	0.019 (2)	0.024 (2)	0.025 (2)	−0.0030 (17)	0.0002 (19)	0.0087 (17)
C5	0.019 (2)	0.031 (3)	0.032 (2)	0.0039 (19)	0.006 (2)	0.014 (2)
C6	0.024 (2)	0.030 (2)	0.029 (2)	0.0108 (19)	0.009 (2)	0.013 (2)
C7	0.024 (2)	0.025 (2)	0.031 (2)	0.0055 (19)	0.005 (2)	0.013 (2)
C8	0.028 (2)	0.021 (2)	0.038 (3)	0.0063 (19)	0.006 (2)	0.009 (2)
C9	0.025 (2)	0.018 (2)	0.035 (3)	0.0062 (18)	0.007 (2)	0.0062 (19)
C10	0.022 (2)	0.025 (2)	0.035 (3)	0.0071 (19)	0.010 (2)	0.003 (2)
C11	0.024 (3)	0.037 (3)	0.042 (3)	0.002 (2)	0.014 (2)	0.004 (2)
C12	0.018 (2)	0.032 (3)	0.035 (3)	−0.006 (2)	0.004 (2)	0.001 (2)
C13	0.024 (2)	0.020 (2)	0.030 (2)	0.0020 (18)	0.006 (2)	0.0032 (18)
C40	0.065 (9)	0.028 (6)	0.034 (6)	0.015 (6)	0.007 (6)	0.006 (5)
C41	0.039 (6)	0.033 (5)	0.022 (4)	0.005 (5)	0.008 (5)	0.010 (4)
C42	0.063 (5)	0.061 (5)	0.047 (4)	0.010 (4)	0.010 (4)	0.022 (4)
C43	0.051 (4)	0.029 (3)	0.031 (3)	−0.006 (3)	−0.001 (3)	0.006 (2)
C44	0.037 (6)	0.044 (7)	0.047 (7)	0.006 (5)	0.012 (6)	0.021 (6)
B1	0.027 (3)	0.020 (2)	0.022 (2)	0.003 (2)	0.007 (2)	0.0037 (19)

Geometric parameters (Å, º)

Yb1—O1	2.358 (3)	C5—H5A	0.9500
Yb1—N5	2.387 (4)	C6—H6A	0.9500
Yb1—N3	2.409 (4)	C7—C8	1.395 (7)
Yb1—N1	2.413 (4)	C7—H7A	0.9500
Yb1—Cl2	2.5307 (14)	C8—C9	1.379 (8)
Yb1—Cl1^i	2.7010 (12)	C8—H8A	0.9500
Yb1—Cl1	2.7082 (13)	C9—H9A	0.9500
Yb1—Yb1^i	4.3622 (12)	C10—C11	1.520 (7)
Cl1—Yb1^i	2.7010 (12)	C10—H10A	0.9900
O1—C13	1.457 (5)	C10—H10B	0.9900
O1—C10	1.461 (6)	C11—C12	1.516 (8)
N1—N2	1.358 (6)	C11—H11A	0.9900
N1—C1	1.365 (6)	C11—H11B	0.9900
N2—C3	1.351 (7)	C12—C13	1.505 (7)
N2—B1	1.531 (7)	C12—H12A	0.9900
N3—C4	1.336 (6)	C12—H12B	0.9900
N3—N4	1.367 (5)	C13—H13A	0.9900
N4—C6	1.349 (6)	C13—H13B	0.9900
N4—B1	1.541 (6)	C40—C41	1.251 (16)
N5—C7	1.333 (6)	C40—C43	1.269 (16)
N5—N6	1.367 (6)	C40—C42	1.497 (16)
N6—C9	1.349 (6)	C41—C42	1.290 (15)
N6—B1	1.547 (7)	C41—C44	1.311 (17)
C1—C2	1.394 (7)	C41—C43	1.476 (12)
C1—H1A	0.9500	C41—C43^ii	1.498 (13)
C2—C3	1.377 (8)	C41—C41^ii	1.75 (2)
C2—H2A	0.9500	C42—C44	1.512 (16)
C3—H3A	0.9500	C43—C44^ii	1.285 (15)
C4—C5	1.382 (7)	C43—C41^ii	1.498 (13)
C4—H4A	0.9500	C44—C43^ii	1.285 (15)
C5—C6	1.380 (7)	B1—H1B1	1.0000
O1—Yb1—N5	92.19 (13)	N5—C7—H7A	124.8
O1—Yb1—N3	141.94 (12)	C8—C7—H7A	124.8
N5—Yb1—N3	76.65 (13)	C9—C8—C7	104.5 (4)
O1—Yb1—N1	69.09 (12)	C9—C8—H8A	127.7
N5—Yb1—N1	78.96 (14)	C7—C8—H8A	127.7
N3—Yb1—N1	73.06 (13)	N6—C9—C8	109.1 (4)
O1—Yb1—Cl2	89.91 (9)	N6—C9—H9A	125.5
N5—Yb1—Cl2	168.16 (11)	C8—C9—H9A	125.5
N3—Yb1—Cl2	94.61 (10)	O1—C10—C11	105.2 (4)
N1—Yb1—Cl2	90.94 (10)	O1—C10—H10A	110.7
O1—Yb1—Cl1^i	142.07 (8)	C11—C10—H10A	110.7
N5—Yb1—Cl1^i	96.67 (10)	O1—C10—H10B	110.7
N3—Yb1—Cl1^i	75.89 (9)	C11—C10—H10B	110.7
N1—Yb1—Cl1^i	148.82 (9)	H10A—C10—H10B	108.8
Cl2—Yb1—Cl1^i	88.77 (4)	C12—C11—C10	103.6 (4)
O1—Yb1—Cl1	71.34 (8)	C12—C11—H11A	111.1
N5—Yb1—Cl1	86.47 (10)	C10—C11—H11A	111.1
N3—Yb1—Cl1	141.95 (9)	C12—C11—H11B	111.0
N1—Yb1—Cl1	137.01 (9)	C10—C11—H11B	111.0
Cl2—Yb1—Cl1	105.23 (4)	H11A—C11—H11B	109.0
Cl1^i—Yb1—Cl1	72.50 (4)	C13—C12—C11	102.2 (4)
O1—Yb1—Yb1^i	106.85 (8)	C13—C12—H12A	111.3
N5—Yb1—Yb1^i	91.93 (10)	C11—C12—H12A	111.3
N3—Yb1—Yb1^i	109.75 (9)	C13—C12—H12B	111.3
N1—Yb1—Yb1^i	169.70 (9)	C11—C12—H12B	111.3
Cl2—Yb1—Yb1^i	98.61 (3)	H12A—C12—H12B	109.2
Cl1^i—Yb1—Yb1^i	36.31 (2)	O1—C13—C12	104.1 (4)
Cl1—Yb1—Yb1^i	36.19 (3)	O1—C13—H13A	110.9
Yb1^i—Cl1—Yb1	107.50 (4)	C12—C13—H13A	110.9
C13—O1—C10	109.7 (3)	O1—C13—H13B	110.9
C13—O1—Yb1	122.2 (3)	C12—C13—H13B	110.9
C10—O1—Yb1	126.4 (3)	H13A—C13—H13B	108.9
N2—N1—C1	105.8 (4)	C41—C40—C43	71.7 (9)
N2—N1—Yb1	124.5 (3)	C41—C40—C42	55.1 (8)
C1—N1—Yb1	129.6 (3)	C43—C40—C42	126.9 (10)
C3—N2—N1	110.4 (4)	C40—C41—C42	72.2 (10)
C3—N2—B1	129.8 (4)	C40—C41—C44	143.1 (14)
N1—N2—B1	119.5 (4)	C42—C41—C44	71.0 (9)
C4—N3—N4	106.0 (4)	C40—C41—C43	54.7 (8)
C4—N3—Yb1	130.5 (3)	C42—C41—C43	126.9 (9)
N4—N3—Yb1	123.4 (3)	C44—C41—C43	161.9 (12)
C6—N4—N3	109.6 (4)	C40—C41—C43^ii	162.7 (13)
C6—N4—B1	129.6 (4)	C42—C41—C43^ii	125.0 (9)
N3—N4—B1	120.7 (4)	C44—C41—C43^ii	53.9 (8)
C7—N5—N6	107.0 (4)	C43—C41—C43^ii	108.1 (8)
C7—N5—Yb1	131.2 (3)	C40—C41—C41^ii	109.3 (12)
N6—N5—Yb1	121.7 (3)	C42—C41—C41^ii	177.6 (12)
C9—N6—N5	108.9 (4)	C44—C41—C41^ii	107.4 (12)
C9—N6—B1	127.9 (4)	C43—C41—C41^ii	54.6 (6)
N5—N6—B1	123.1 (4)	C43^ii—C41—C41^ii	53.5 (6)
N1—C1—C2	110.1 (5)	C41—C42—C40	52.7 (8)
N1—C1—H1A	124.9	C41—C42—C44	55.1 (8)
C2—C1—H1A	124.9	C40—C42—C44	107.8 (9)
C3—C2—C1	105.2 (4)	C40—C43—C44^ii	178.8 (10)
C3—C2—H2A	127.4	C40—C43—C41	53.6 (8)
C1—C2—H2A	127.4	C44^ii—C43—C41	127.4 (9)
N2—C3—C2	108.4 (5)	C40—C43—C41^ii	125.4 (9)
N2—C3—H3A	125.8	C44^ii—C43—C41^ii	55.6 (8)
C2—C3—H3A	125.8	C41—C43—C41^ii	71.9 (8)
N3—C4—C5	111.3 (5)	C43^ii—C44—C41	70.5 (9)
N3—C4—H4A	124.3	C43^ii—C44—C42	124.3 (10)
C5—C4—H4A	124.3	C41—C44—C42	53.8 (8)
C6—C5—C4	104.7 (4)	N2—B1—N4	107.8 (4)
C6—C5—H5A	127.6	N2—B1—N6	110.0 (4)
C4—C5—H5A	127.6	N4—B1—N6	109.2 (4)
N4—C6—C5	108.4 (4)	N2—B1—H1B1	109.9
N4—C6—H6A	125.8	N4—B1—H1B1	109.9
C5—C6—H6A	125.8	N6—B1—H1B1	109.9
N5—C7—C8	110.5 (5)

Symmetry codes: (i) −x+1, −y+1, −z+1; (ii) −x+2, −y, −z+1.