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In the title complex, [Ti(C36H40BN6)Cl3]·2CH2Cl2, the Ti atom is coordinated by three N atoms that are constrained to a facial arrangement by the TpMs ligand [TpMs = HB(3-mesityl-pyrazol­yl)3] and three chloride ligands in a distorted octa­hedral geometry. The complex mol­ecules are located on crystallographic mirror planes.

Supporting information

cif

Crystallographic Information File (CIF) https://doi.org/10.1107/S1600536806032788/ac2031sup1.cif
Contains datablocks I, global

hkl

Structure factor file (CIF format) https://doi.org/10.1107/S1600536806032788/ac2031Isup2.hkl
Contains datablock I

CCDC reference: 620499

Key indicators

  • Single-crystal X-ray study
  • T = 130 K
  • Mean [sigma](C-C) = 0.005 Å
  • R factor = 0.045
  • wR factor = 0.120
  • Data-to-parameter ratio = 14.8

checkCIF/PLATON results

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Alert level A PLAT073_ALERT_1_A H-atoms ref, but _hydrogen_treatment reported as constr
Alert level C PLAT042_ALERT_1_C Calc. and Rep. MoietyFormula Strings Differ .... ?
1 ALERT level A = In general: serious problem 0 ALERT level B = Potentially serious problem 1 ALERT level C = Check and explain 0 ALERT level G = General alerts; check 2 ALERT type 1 CIF construction/syntax error, inconsistent or missing data 0 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 0 ALERT type 4 Improvement, methodology, query or suggestion 0 ALERT type 5 Informative message, check

Computing details top

Data collection: SMART (Bruker, 2002); cell refinement: SAINT-Plus (Bruker, 2002); data reduction: SADABS (Bruker, 2002); program(s) used to solve structure: SHELXTL (Bruker, 2002); program(s) used to refine structure: SHELXTL; molecular graphics: SHELXTL; software used to prepare material for publication: SHELXTL.

Trichloro[tris(3-mesitylpyrazol-1-yl)borohydrido]titanium dichloromethane disolvate top
Crystal data top
[Ti(C36H40BN6)Cl3]·2CH2Cl2F(000) = 920
Mr = 891.65Dx = 1.377 Mg m3
Monoclinic, P21/mMo Kα radiation, λ = 0.71073 Å
Hall symbol: -P 2ybCell parameters from 1024 reflections
a = 7.964 (3) Åθ = 2.5–25.0°
b = 22.940 (7) ŵ = 0.67 mm1
c = 11.844 (4) ÅT = 130 K
β = 96.484 (5)°Rod, red
V = 2149.9 (12) Å30.45 × 0.15 × 0.15 mm
Z = 2
Data collection top
Bruker SMART APEX CCD
diffractometer
3894 independent reflections
Radiation source: fine-focus sealed tube3026 reflections with I > 2σ(I)
Graphite monochromatorRint = 0.047
Detector resolution: 8.33 pixels mm-1θmax = 25.0°, θmin = 2.5°
ω scansh = 99
Absorption correction: multi-scan
(SADABS; Bruker, 2002)
k = 2725
Tmin = 0.670, Tmax = 0.90l = 1414
16493 measured reflections
Refinement top
Refinement on F2Primary atom site location: structure-invariant direct methods
Least-squares matrix: fullSecondary atom site location: difference Fourier map
R[F2 > 2σ(F2)] = 0.045Hydrogen site location: inferred from neighbouring sites
wR(F2) = 0.120H-atom parameters constrained
S = 1.05 w = 1/[σ2(Fo2) + (0.0635P)2 + 0.8057P]
where P = (Fo2 + 2Fc2)/3
3894 reflections(Δ/σ)max = 0.002
264 parametersΔρmax = 0.92 e Å3
0 restraintsΔρmin = 0.64 e Å3
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 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 (Å2) top
xyzUiso*/UeqOcc. (<1)
H220.639 (5)0.75000.650 (3)0.028 (9)*
B10.4971 (5)0.75000.6513 (4)0.0233 (10)
C10.4819 (5)0.75000.4314 (4)0.0367 (11)
H10.59990.75000.42580.044*
C20.3559 (6)0.75000.3407 (4)0.0447 (13)
H20.37010.75000.26220.054*
C30.2029 (5)0.75000.3890 (3)0.0284 (10)
C40.0332 (5)0.75000.3203 (3)0.0262 (10)
C50.0404 (4)0.69637 (14)0.2806 (2)0.0285 (7)
C60.1875 (4)0.69778 (15)0.2040 (3)0.0329 (7)
H60.23920.66200.17930.040*
C70.2611 (5)0.75000.1624 (4)0.0339 (11)
C80.0429 (4)0.63853 (15)0.3128 (3)0.0404 (8)
H8A0.04150.60730.30220.061*
H8B0.09150.63970.39260.061*
H8C0.13270.63110.26450.061*
C90.4118 (6)0.75000.0706 (4)0.0538 (15)
H9A0.37670.76520.00040.081*0.50
H9B0.50160.77470.09480.081*0.50
H9C0.45400.71010.05850.081*0.50
C100.5326 (4)0.65091 (14)0.7567 (3)0.0319 (7)
H100.65180.64750.75890.038*
C110.4259 (4)0.61060 (15)0.7996 (3)0.0364 (8)
H110.45760.57470.83580.044*
C120.2624 (3)0.63349 (13)0.7788 (2)0.0257 (7)
C130.1100 (3)0.60693 (13)0.8215 (2)0.0253 (7)
C140.0755 (4)0.62181 (14)0.9326 (2)0.0282 (7)
C150.0548 (4)0.59238 (14)0.9795 (3)0.0302 (7)
H150.07950.60281.05340.036*
C160.1489 (3)0.54844 (13)0.9215 (3)0.0279 (7)
C170.1124 (4)0.53415 (13)0.8118 (3)0.0287 (7)
H170.17710.50480.77050.034*
C180.0178 (3)0.56223 (13)0.7612 (2)0.0268 (7)
C190.1846 (4)0.66517 (15)1.0057 (3)0.0364 (8)
H19A0.11410.68671.05410.055*
H19B0.23680.69260.95660.055*
H19C0.27310.64411.05350.055*
C200.2821 (4)0.51609 (15)0.9790 (3)0.0363 (8)
H20A0.22740.49381.04350.054*
H20B0.34390.48940.92450.054*
H20C0.36120.54421.00620.054*
C210.0609 (4)0.54097 (15)0.6464 (3)0.0385 (8)
H21A0.08790.57440.60030.058*
H21B0.03610.52000.60750.058*
H21C0.15860.51480.65750.058*
C220.4094 (5)0.4100 (3)0.5924 (4)0.0907 (18)
H22A0.37660.36840.59380.109*
H22B0.30880.43230.56010.109*
Cl10.08270 (8)0.67738 (3)0.56819 (6)0.02569 (19)
Cl20.04479 (11)0.75000.81292 (8)0.0247 (2)
Cl30.5645 (2)0.41766 (7)0.50458 (11)0.0986 (5)
Cl40.46653 (14)0.43332 (5)0.73188 (9)0.0697 (3)
N10.2351 (4)0.75000.5048 (3)0.0222 (7)
N20.4099 (4)0.75000.5285 (3)0.0236 (8)
N30.2685 (3)0.68602 (10)0.72349 (19)0.0214 (5)
N40.4384 (3)0.69543 (10)0.71174 (19)0.0241 (5)
Ti10.07869 (8)0.75000.65196 (6)0.01901 (19)
Atomic displacement parameters (Å2) top
U11U22U33U12U13U23
B10.012 (2)0.030 (3)0.028 (2)0.0000.0032 (18)0.000
C10.017 (2)0.063 (3)0.032 (2)0.0000.0131 (18)0.000
C20.028 (3)0.083 (4)0.025 (2)0.0000.0102 (19)0.000
C30.023 (2)0.038 (3)0.024 (2)0.0000.0052 (17)0.000
C40.022 (2)0.038 (3)0.020 (2)0.0000.0084 (17)0.000
C50.0243 (16)0.0371 (19)0.0255 (16)0.0026 (13)0.0094 (12)0.0023 (13)
C60.0274 (17)0.042 (2)0.0301 (17)0.0073 (14)0.0068 (13)0.0076 (15)
C70.021 (2)0.057 (3)0.024 (2)0.0000.0043 (18)0.000
C80.046 (2)0.038 (2)0.0376 (19)0.0090 (16)0.0083 (16)0.0027 (15)
C90.024 (3)0.097 (5)0.039 (3)0.0000.005 (2)0.000
C100.0146 (14)0.041 (2)0.0401 (18)0.0080 (13)0.0009 (13)0.0046 (15)
C110.0216 (16)0.040 (2)0.048 (2)0.0078 (14)0.0034 (14)0.0141 (16)
C120.0202 (15)0.0304 (17)0.0262 (15)0.0017 (13)0.0019 (12)0.0032 (13)
C130.0172 (14)0.0271 (17)0.0314 (16)0.0040 (12)0.0020 (12)0.0072 (13)
C140.0239 (15)0.0319 (17)0.0275 (16)0.0006 (13)0.0023 (12)0.0058 (13)
C150.0280 (16)0.0358 (19)0.0274 (16)0.0029 (14)0.0054 (13)0.0049 (14)
C160.0180 (15)0.0313 (18)0.0344 (17)0.0056 (13)0.0037 (12)0.0090 (14)
C170.0225 (15)0.0266 (17)0.0361 (17)0.0007 (13)0.0010 (13)0.0015 (14)
C180.0216 (15)0.0277 (17)0.0311 (16)0.0028 (13)0.0023 (12)0.0019 (13)
C190.0357 (18)0.042 (2)0.0303 (17)0.0093 (15)0.0007 (14)0.0038 (15)
C200.0228 (16)0.041 (2)0.046 (2)0.0028 (14)0.0048 (14)0.0117 (16)
C210.0394 (19)0.037 (2)0.0407 (19)0.0007 (16)0.0102 (15)0.0034 (16)
C220.047 (3)0.125 (5)0.098 (4)0.003 (3)0.001 (2)0.068 (3)
Cl10.0169 (3)0.0315 (4)0.0286 (4)0.0026 (3)0.0025 (3)0.0034 (3)
Cl20.0145 (5)0.0377 (6)0.0223 (5)0.0000.0043 (4)0.000
Cl30.1340 (13)0.1005 (11)0.0655 (8)0.0310 (9)0.0306 (8)0.0035 (7)
Cl40.0732 (8)0.0805 (8)0.0561 (6)0.0222 (6)0.0095 (5)0.0159 (6)
N10.0109 (16)0.030 (2)0.0267 (18)0.0000.0042 (13)0.000
N20.0102 (16)0.035 (2)0.0256 (18)0.0000.0043 (13)0.000
N30.0114 (11)0.0289 (14)0.0241 (12)0.0026 (10)0.0030 (9)0.0005 (10)
N40.0112 (11)0.0311 (14)0.0298 (13)0.0023 (10)0.0021 (10)0.0004 (11)
Ti10.0099 (3)0.0266 (4)0.0207 (4)0.0000.0030 (3)0.000
Geometric parameters (Å, º) top
B1—N4i1.541 (4)C14—C151.404 (4)
B1—H221.13 (4)C14—C191.525 (4)
C1—N21.341 (5)C15—C161.391 (4)
C1—C21.385 (6)C15—H150.9500
C1—H10.9500C16—C171.401 (4)
C2—C31.403 (6)C16—C201.518 (4)
C2—H20.9500C17—C181.411 (4)
C3—N11.367 (5)C17—H170.9500
C3—C41.497 (6)C18—C211.519 (4)
C4—C51.420 (4)C19—H19A0.9800
C4—C5i1.420 (4)C19—H19B0.9800
C5—C61.399 (4)C19—H19C0.9800
C5—C81.513 (4)C20—H20A0.9800
C6—C71.399 (4)C20—H20B0.9800
C6—H60.9500C20—H20C0.9800
C7—C6i1.399 (4)C21—H21A0.9800
C7—C91.525 (6)C21—H21B0.9800
C8—H8A0.9800C21—H21C0.9800
C8—H8B0.9800C22—Cl31.711 (5)
C8—H8C0.9800C22—Cl41.748 (5)
C9—H9A0.9800C22—H22A0.9900
C9—H9B0.9800C22—H22B0.9900
C9—H9C0.9800Ti1—N12.253 (3)
C10—N41.341 (4)Ti1—N32.206 (2)
C10—C111.390 (4)B1—N21.539 (6)
C10—H100.9500Ti1—Cl12.2635 (9)
C11—C121.399 (4)Ti1—Cl22.2417 (12)
C11—H110.9500B1—N41.541 (4)
C12—N31.375 (4)N1—N21.389 (4)
C12—C131.497 (4)N3—N41.393 (3)
C13—C181.408 (4)Ti1—N3i2.206 (2)
C13—C141.416 (4)Ti1—Cl1i2.2635 (9)
N2—B1—N4i108.1 (2)C16—C17—H17119.1
N2—B1—H22109.2 (18)C18—C17—H17119.1
N4i—B1—H22111.3 (9)C13—C18—C17118.9 (3)
N4—B1—H22111.3 (9)C13—C18—C21122.0 (3)
N2—C1—C2108.8 (4)C17—C18—C21119.0 (3)
N2—C1—H1125.6C14—C19—H19A109.5
C2—C1—H1125.6C14—C19—H19B109.5
C1—C2—C3105.7 (4)H19A—C19—H19B109.5
C1—C2—H2127.2C14—C19—H19C109.5
C3—C2—H2127.2H19A—C19—H19C109.5
N1—C3—C2109.7 (4)H19B—C19—H19C109.5
N1—C3—C4126.9 (3)C16—C20—H20A109.5
C2—C3—C4123.4 (4)C16—C20—H20B109.5
C5—C4—C5i120.1 (4)H20A—C20—H20B109.5
C5—C4—C3119.58 (19)C16—C20—H20C109.5
C5i—C4—C3119.58 (19)H20A—C20—H20C109.5
C6—C5—C4118.6 (3)H20B—C20—H20C109.5
C6—C5—C8119.7 (3)C18—C21—H21A109.5
C4—C5—C8121.6 (3)C18—C21—H21B109.5
C7—C6—C5122.4 (3)H21A—C21—H21B109.5
C7—C6—H6118.8C18—C21—H21C109.5
C5—C6—H6118.8H21A—C21—H21C109.5
C6i—C7—C6117.8 (4)H21B—C21—H21C109.5
C6i—C7—C9121.1 (2)Cl3—C22—Cl4114.5 (3)
C6—C7—C9121.1 (2)Cl3—C22—H22A108.6
C5—C8—H8A109.5Cl4—C22—H22A108.6
C5—C8—H8B109.5Cl3—C22—H22B108.6
H8A—C8—H8B109.5Cl4—C22—H22B108.6
C5—C8—H8C109.5H22A—C22—H22B107.6
H8A—C8—H8C109.5C3—N1—N2105.8 (3)
H8B—C8—H8C109.5C3—N1—Ti1136.0 (3)
C7—C9—H9A109.5N2—N1—Ti1118.3 (2)
C7—C9—H9B109.5N4—N3—Ti1119.33 (17)
H9A—C9—H9B109.5N3—Ti1—N183.25 (8)
C7—C9—H9C109.5N3i—Ti1—N383.40 (12)
H9A—C9—H9C109.5N3—Ti1—Cl190.53 (6)
H9B—C9—H9C109.5N1—Ti1—Cl189.83 (6)
N4—C10—C11108.3 (2)N3—Ti1—Cl291.19 (6)
N4—C10—H10125.9Cl2—Ti1—N1172.53 (9)
C11—C10—H10125.9N3i—Ti1—Cl1171.27 (6)
C10—C11—C12106.3 (3)N3i—Ti1—Cl291.19 (6)
C10—C11—H11126.8Cl1—Ti1—Cl1i94.78 (5)
C12—C11—H11126.8Cl2—Ti1—Cl195.22 (3)
N3—C12—C11109.3 (3)N2—B1—N4108.1 (2)
N3—C12—C13126.2 (2)N4i—B1—N4108.7 (3)
C11—C12—C13124.2 (3)C1—N2—N1110.1 (3)
C18—C13—C14120.1 (3)C1—N2—B1128.3 (3)
C18—C13—C12121.4 (3)N1—N2—B1121.7 (3)
C14—C13—C12117.8 (3)C12—N3—N4105.7 (2)
C15—C14—C13118.8 (3)C12—N3—Ti1134.96 (18)
C15—C14—C19119.2 (3)C10—N4—N3110.4 (2)
C13—C14—C19121.8 (3)C10—N4—B1128.2 (3)
C16—C15—C14122.3 (3)N3—N4—B1121.4 (2)
C16—C15—H15118.9N3i—Ti1—N183.25 (8)
C14—C15—H15118.9N3i—Ti1—Cl1i90.53 (6)
C15—C16—C17118.1 (3)N3—Ti1—Cl1i171.27 (6)
C15—C16—C20119.8 (3)Cl2—Ti1—Cl1i95.22 (3)
C17—C16—C20122.0 (3)N1—Ti1—Cl1i89.83 (6)
C16—C17—C18121.8 (3)
N2—C1—C2—C30.000 (2)C4—C3—N1—Ti10.000 (1)
C1—C2—C3—N10.000 (2)C2—C1—N2—N10.000 (2)
C1—C2—C3—C4180.000 (1)C2—C1—N2—B1180.000 (3)
N1—C3—C4—C594.9 (3)C3—N1—N2—C10.0
C2—C3—C4—C585.1 (3)Ti1—N1—N2—C1180.000 (1)
N1—C3—C4—C5i94.9 (3)C3—N1—N2—B1180.000 (2)
C2—C3—C4—C5i85.1 (3)Ti1—N1—N2—B10.000 (1)
C5i—C4—C5—C61.2 (5)N4i—B1—N2—C1121.2 (2)
C3—C4—C5—C6171.4 (3)N4—B1—N2—C1121.2 (2)
C5i—C4—C5—C8174.5 (2)N4i—B1—N2—N158.8 (2)
C3—C4—C5—C84.3 (5)N4—B1—N2—N158.8 (2)
C4—C5—C6—C72.1 (5)C11—C12—N3—N40.7 (3)
C8—C5—C6—C7173.6 (3)C13—C12—N3—N4173.6 (3)
C5—C6—C7—C6i3.0 (6)C11—C12—N3—Ti1176.9 (2)
C5—C6—C7—C9174.3 (3)C13—C12—N3—Ti18.8 (4)
N4—C10—C11—C120.5 (4)C11—C10—N4—N30.1 (3)
C10—C11—C12—N30.7 (4)C11—C10—N4—B1178.3 (3)
C10—C11—C12—C13173.7 (3)C12—N3—N4—C100.4 (3)
N3—C12—C13—C18101.1 (4)Ti1—N3—N4—C10177.68 (19)
C11—C12—C13—C1885.5 (4)C12—N3—N4—B1178.9 (3)
N3—C12—C13—C1488.2 (4)Ti1—N3—N4—B10.8 (3)
C11—C12—C13—C1485.3 (4)N2—B1—N4—C10118.4 (3)
C18—C13—C14—C151.8 (4)N4i—B1—N4—C10124.4 (3)
C12—C13—C14—C15172.6 (3)N2—B1—N4—N359.9 (3)
C18—C13—C14—C19173.2 (3)N4i—B1—N4—N357.3 (4)
C12—C13—C14—C192.3 (4)C12—N3—Ti1—N3i140.3 (2)
C13—C14—C15—C161.2 (4)N4—N3—Ti1—N3i42.4 (2)
C19—C14—C15—C16173.9 (3)C12—N3—Ti1—Cl249.2 (3)
C14—C15—C16—C170.9 (4)N4—N3—Ti1—Cl2133.44 (18)
C14—C15—C16—C20176.9 (3)C12—N3—Ti1—N1135.8 (3)
C15—C16—C17—C181.2 (4)N4—N3—Ti1—N141.57 (18)
C20—C16—C17—C18176.5 (3)C12—N3—Ti1—Cl146.0 (3)
C14—C13—C18—C172.1 (4)N4—N3—Ti1—Cl1131.33 (18)
C12—C13—C18—C17172.6 (3)C3—N1—Ti1—N3i137.94 (6)
C14—C13—C18—C21174.3 (3)N2—N1—Ti1—N3i42.06 (6)
C12—C13—C18—C213.8 (4)C3—N1—Ti1—N3137.94 (6)
C16—C17—C18—C131.8 (4)N2—N1—Ti1—N342.06 (6)
C16—C17—C18—C21174.7 (3)C3—N1—Ti1—Cl147.39 (2)
C2—C3—N1—N20.000 (1)N2—N1—Ti1—Cl1132.61 (2)
C4—C3—N1—N2180.000 (2)C3—N1—Ti1—Cl1i47.39 (2)
C2—C3—N1—Ti1180.000 (2)N2—N1—Ti1—Cl1i132.61 (2)
Symmetry code: (i) x, y+3/2, z.
 

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