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In the title compound, (C2H8N)2[Ti(C7H4O3)3], the TiIV atom is chelated by three salicylate ligands in a mer-octa­hedral geometry. The cations and complex anions are linked by hydrogen bonds into a layer structure.

Supporting information

cif

Crystallographic Information File (CIF) https://doi.org/10.1107/S160053680502475X/ob6556sup1.cif
Contains datablocks I, global

hkl

Structure factor file (CIF format) https://doi.org/10.1107/S160053680502475X/ob6556Isup2.hkl
Contains datablock I

CCDC reference: 283970

Key indicators

  • Single-crystal X-ray study
  • T = 295 K
  • Mean [sigma](C-C) = 0.004 Å
  • R factor = 0.055
  • wR factor = 0.186
  • Data-to-parameter ratio = 16.9

checkCIF/PLATON results

No syntax errors found



Alert level C ABSTM02_ALERT_3_C The ratio of expected to reported Tmax/Tmin(RR') is < 0.90 Tmin and Tmax reported: 0.784 0.926 Tmin(prime) and Tmax expected: 0.870 0.925 RR(prime) = 0.900 Please check that your absorption correction is appropriate. PLAT029_ALERT_3_C _diffrn_measured_fraction_theta_full Low ....... 0.96 PLAT042_ALERT_1_C Calc. and Rep. MoietyFormula Strings Differ .... ? PLAT061_ALERT_3_C Tmax/Tmin Range Test RR' too Large ............. 0.90 PLAT094_ALERT_2_C Ratio of Maximum / Minimum Residual Density .... 2.41 PLAT244_ALERT_4_C Low 'Solvent' Ueq as Compared to Neighbors for N1 PLAT244_ALERT_4_C Low 'Solvent' Ueq as Compared to Neighbors for N2
0 ALERT level A = In general: serious problem 0 ALERT level B = Potentially serious problem 7 ALERT level C = Check and explain 0 ALERT level G = General alerts; check 1 ALERT type 1 CIF construction/syntax error, inconsistent or missing data 1 ALERT type 2 Indicator that the structure model may be wrong or deficient 3 ALERT type 3 Indicator that the structure quality may be low 2 ALERT type 4 Improvement, methodology, query or suggestion

Computing details top

Data collection: SMART (Bruker, 2002); cell refinement: SAINT (Bruker, 2002); data reduction: SAINT; program(s) used to solve structure: SHELXS97 (Sheldrick, 1997); program(s) used to refine structure: SHELXL97 (Sheldrick, 1997); molecular graphics: ORTEPII (Johnson, 1976); software used to prepare material for publication: SHELXL97.

Bis(dimethylammonium) mer-tris(salicylato-κ2O,O')titanate(IV) top
Crystal data top
(C2H8N)2[Ti(C7H4O3)3]F(000) = 1144
Mr = 548.39Dx = 1.426 Mg m3
Monoclinic, P21/nMo Kα radiation, λ = 0.71073 Å
Hall symbol: -P 2ynCell parameters from 3721 reflections
a = 11.589 (1) Åθ = 2.2–25.2°
b = 14.270 (1) ŵ = 0.39 mm1
c = 15.463 (1) ÅT = 295 K
β = 92.259 (1)°Block, red
V = 2555.1 (3) Å30.35 × 0.22 × 0.20 mm
Z = 4
Data collection top
Bruker APEX area-detector
diffractometer
5654 independent reflections
Radiation source: fine-focus sealed tube4430 reflections with I > 2σ(I)
Graphite monochromatorRint = 0.029
φ and ω scansθmax = 27.5°, θmin = 1.9°
Absorption correction: multi-scan
SADABS (Sheldrick, 1996)
h = 1315
Tmin = 0.784, Tmax = 0.926k = 1813
14492 measured reflectionsl = 1920
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)] = 0.055Hydrogen site location: inferred from neighbouring sites
wR(F2) = 0.186H-atom parameters constrained
S = 1.07 w = 1/[σ2(Fo2) + (0.1131P)2 + 0.5921P]
where P = (Fo2 + 2Fc2)/3
5654 reflections(Δ/σ)max = 0.001
334 parametersΔρmax = 0.65 e Å3
0 restraintsΔρmin = 0.27 e Å3
Fractional atomic coordinates and isotropic or equivalent isotropic displacement parameters (Å2) top
xyzUiso*/Ueq
Ti10.60858 (4)0.25981 (3)0.62969 (3)0.0346 (2)
O10.7426 (2)0.1916 (1)0.6588 (1)0.0422 (5)
O20.7127 (2)0.3599 (1)0.5919 (1)0.0417 (5)
O30.8649 (2)0.4493 (2)0.5843 (2)0.0655 (7)
O40.5971 (2)0.3123 (1)0.7423 (1)0.0434 (5)
O50.4688 (2)0.3451 (1)0.6003 (1)0.0395 (4)
O60.3017 (2)0.4143 (1)0.6145 (1)0.0456 (5)
O70.5880 (2)0.2168 (1)0.5145 (1)0.0415 (5)
O80.4988 (2)0.1623 (1)0.6607 (1)0.0418 (5)
O90.3362 (2)0.0828 (2)0.6519 (1)0.0575 (6)
N10.6948 (2)0.5871 (2)0.5648 (2)0.0460 (6)
N20.1845 (2)0.5769 (2)0.6740 (2)0.0507 (6)
C10.8541 (2)0.2040 (2)0.6468 (2)0.034 (1)
C20.9310 (2)0.1294 (2)0.6612 (2)0.042 (1)
C31.0469 (3)0.1398 (2)0.6503 (2)0.050 (1)
C41.0908 (3)0.2247 (3)0.6248 (2)0.056 (1)
C51.0170 (2)0.2985 (2)0.6088 (2)0.050 (1)
C60.8988 (2)0.2900 (2)0.6185 (2)0.035 (1)
C70.8226 (2)0.3716 (2)0.5976 (2)0.036 (1)
C80.5074 (2)0.3420 (2)0.7847 (2)0.037 (1)
C90.5179 (3)0.3494 (2)0.8751 (2)0.048 (1)
C100.4245 (3)0.3727 (2)0.9226 (2)0.055 (1)
C110.3170 (3)0.3900 (2)0.8824 (2)0.051 (1)
C120.3075 (3)0.3893 (2)0.7942 (2)0.043 (1)
C130.4010 (2)0.3668 (2)0.7436 (2)0.034 (1)
C140.3890 (2)0.3752 (2)0.6478 (2)0.033 (1)
C150.5051 (2)0.1654 (2)0.4749 (2)0.035 (1)
C160.5050 (3)0.1574 (2)0.3843 (2)0.047 (1)
C170.4226 (3)0.1032 (3)0.3412 (2)0.058 (1)
C180.3372 (3)0.0591 (3)0.3858 (2)0.067 (1)
C190.3358 (3)0.0673 (2)0.4740 (2)0.058 (1)
C200.4200 (2)0.1197 (2)0.5204 (2)0.039 (1)
C210.4164 (2)0.1212 (2)0.6164 (2)0.039 (1)
C220.7549 (3)0.6720 (3)0.5974 (3)0.073 (1)
C230.5802 (3)0.5721 (3)0.5997 (2)0.071 (1)
C240.2662 (3)0.6466 (3)0.6468 (2)0.070 (1)
C250.0679 (3)0.5863 (3)0.6350 (3)0.076 (1)
H1a0.73920.53690.57780.055*
H1b0.68710.59080.50680.055*
H2a0.21180.51980.66090.061*
H2b0.18020.57990.73190.061*
H20.90280.07160.67840.050*
H31.09630.08930.66020.061*
H41.16980.23190.61840.067*
H51.04690.35550.59110.060*
H90.58900.33850.90320.058*
H100.43320.37680.98250.066*
H110.25300.40190.91510.061*
H120.23690.40410.76700.051*
H160.56050.18870.35340.056*
H170.42450.09640.28140.070*
H180.28090.02390.35610.080*
H190.27800.03750.50380.070*
H22a0.82890.67660.57190.109*
H22b0.76540.66820.65920.109*
H22c0.70960.72630.58230.109*
H23a0.54700.51580.57560.106*
H23b0.53120.62440.58480.106*
H23c0.58750.56640.66160.106*
H24a0.34010.63510.67490.105*
H24b0.23950.70790.66220.105*
H24c0.27300.64320.58520.105*
H25a0.01960.53750.65630.114*
H25b0.07090.58140.57320.114*
H25c0.03670.64620.64990.114*
Atomic displacement parameters (Å2) top
U11U22U33U12U13U23
Ti10.0286 (3)0.0393 (3)0.0362 (3)0.0001 (2)0.0036 (2)0.0000 (2)
O10.034 (1)0.043 (1)0.050 (1)0.004 (1)0.009 (1)0.008 (1)
O20.031 (1)0.039 (1)0.055 (1)0.001 (1)0.003 (1)0.007 (1)
O30.043 (1)0.038 (1)0.115 (2)0.006 (1)0.003 (1)0.005 (1)
O40.036 (1)0.057 (1)0.036 (1)0.006 (1)0.003 (1)0.007 (1)
O50.037 (1)0.050 (1)0.032 (1)0.004 (1)0.003 (1)0.002 (1)
O60.041 (1)0.057 (1)0.039 (1)0.014 (1)0.002 (1)0.003 (1)
O70.037 (1)0.051 (1)0.038 (1)0.009 (1)0.011 (1)0.006 (1)
O80.041 (1)0.046 (1)0.039 (1)0.007 (1)0.003 (1)0.004 (1)
O90.048 (1)0.076 (2)0.049 (1)0.021 (1)0.012 (1)0.009 (1)
N10.057 (2)0.040 (1)0.040 (1)0.010 (1)0.007 (1)0.001 (1)
N20.056 (2)0.050 (2)0.046 (1)0.005 (1)0.003 (1)0.007 (1)
C10.032 (1)0.041 (1)0.030 (1)0.004 (1)0.002 (1)0.004 (1)
C20.046 (2)0.042 (2)0.037 (1)0.007 (1)0.006 (1)0.001 (1)
C30.041 (2)0.057 (2)0.053 (2)0.016 (1)0.009 (1)0.003 (1)
C40.029 (2)0.069 (2)0.070 (2)0.006 (1)0.001 (1)0.004 (2)
C50.035 (2)0.052 (2)0.062 (2)0.004 (1)0.002 (1)0.002 (2)
C60.031 (1)0.041 (1)0.033 (1)0.001 (1)0.003 (1)0.005 (1)
C70.035 (1)0.038 (1)0.036 (1)0.001 (1)0.003 (1)0.004 (1)
C80.044 (2)0.030 (1)0.037 (1)0.000 (1)0.003 (1)0.001 (1)
C90.058 (2)0.048 (2)0.038 (2)0.007 (1)0.008 (1)0.001 (1)
C100.083 (2)0.047 (2)0.035 (2)0.006 (2)0.002 (2)0.002 (1)
C110.062 (2)0.045 (2)0.046 (2)0.005 (1)0.022 (1)0.001 (1)
C120.046 (2)0.037 (1)0.045 (2)0.005 (1)0.006 (1)0.003 (1)
C130.040 (1)0.027 (1)0.033 (1)0.001 (1)0.002 (1)0.001 (1)
C140.034 (1)0.031 (1)0.033 (1)0.003 (1)0.003 (1)0.001 (1)
C150.035 (1)0.032 (1)0.039 (1)0.004 (1)0.004 (1)0.001 (1)
C160.050 (2)0.054 (2)0.037 (1)0.000 (1)0.012 (1)0.001 (1)
C170.068 (2)0.069 (2)0.038 (2)0.007 (2)0.005 (2)0.006 (2)
C180.075 (2)0.075 (2)0.049 (2)0.027 (2)0.011 (2)0.000 (2)
C190.056 (2)0.063 (2)0.055 (2)0.024 (2)0.004 (2)0.014 (2)
C200.039 (2)0.037 (1)0.039 (1)0.001 (1)0.003 (1)0.006 (1)
C210.038 (2)0.036 (1)0.042 (2)0.002 (1)0.005 (1)0.005 (1)
C220.063 (2)0.057 (2)0.097 (3)0.002 (2)0.014 (2)0.015 (2)
C230.078 (3)0.068 (2)0.066 (2)0.009 (2)0.008 (2)0.0029 (2)
C240.071 (3)0.064 (2)0.073 (2)0.016 (2)0.001 (2)0.0024 (2)
C250.052 (2)0.096 (3)0.079 (3)0.001 (2)0.012 (2)0.024 (2)
Geometric parameters (Å, º) top
Ti1—O11.872 (2)C15—C161.406 (4)
Ti1—O21.973 (2)C16—C171.380 (4)
Ti1—O52.063 (2)C17—C181.380 (5)
Ti1—O41.906 (2)C18—C191.370 (5)
Ti1—O71.891 (2)C19—C201.404 (4)
Ti1—O81.958 (2)C20—C211.486 (4)
O1—C11.324 (3)N1—H1b0.90
O2—C71.284 (3)N1—H1a0.90
O3—C71.233 (3)N2—H2b0.90
O4—C81.319 (3)N2—H2a0.90
O5—C141.278 (3)C2—H20.93
O6—C141.248 (3)C3—H30.93
O7—C151.337 (3)C4—H40.93
O8—C211.293 (3)C5—H50.93
O9—C211.228 (3)C9—H90.93
N1—C231.469 (4)C10—H100.93
N1—C221.475 (4)C11—H110.93
N2—C241.447 (4)C12—H120.93
N2—C251.464 (4)C16—H160.93
C1—C21.401 (4)C17—H170.93
C1—C61.409 (4)C18—H180.93
C2—C31.368 (4)C19—H190.93
C3—C41.377 (5)C22—H22a0.96
C4—C51.373 (4)C22—H22b0.96
C5—C61.390 (4)C22—H22c0.96
C6—C71.489 (4)C23—H23a0.96
C8—C91.403 (4)C23—H23b0.96
C8—C131.410 (4)C23—H23c0.96
C9—C101.372 (4)C24—H24a0.96
C10—C111.392 (5)C24—H24b0.96
C11—C121.364 (4)C24—H24c0.96
C12—C131.399 (4)C25—H25a0.96
C13—C141.487 (3)C25—H25b0.96
C15—C201.395 (4)C25—H25c0.96
O1—Ti1—O286.35 (8)O9—C21—C20119.5 (2)
O1—Ti1—O494.11 (8)O8—C21—C20119.1 (2)
O1—Ti1—O5175.11 (8)C23—N1—H1b108.6
O1—Ti1—O896.46 (8)C22—N1—H1b108.6
O1—Ti1—O797.50 (9)C23—N1—H1a108.6
O2—Ti1—O492.97 (9)C22—N1—H1a108.6
O2—Ti1—O589.51 (8)H1b—N1—H1a107.6
O2—Ti1—O790.66 (8)C24—N2—H2b108.5
O2—Ti1—O8176.31 (8)C25—N2—H2b108.5
O4—Ti1—O583.49 (8)C24—N2—H2a108.5
O4—Ti1—O7168.03 (8)C25—N2—H2a108.5
O4—Ti1—O889.23 (9)H2b—N2—H2a107.5
O5—Ti1—O785.14 (8)C3—C2—H2119.3
O5—Ti1—O887.79 (8)C1—C2—H2119.3
O7—Ti1—O886.60 (8)C2—C3—H3119.8
C1—O1—Ti1134.6 (2)C4—C3—H3119.8
C7—O2—Ti1133.7 (2)C5—C4—H4120.3
C8—O4—Ti1131.6 (2)C3—C4—H4120.3
C14—O5—Ti1130.6 (2)C4—C5—H5119.2
C15—O7—Ti1132.1 (2)C6—C5—H5119.2
C21—O8—Ti1131.7 (2)C10—C9—H9119.6
C23—N1—C22114.6 (3)C8—C9—H9119.6
C24—N2—C25114.9 (3)C9—C10—H10119.5
O1—C1—C2119.7 (3)C11—C10—H10119.5
O1—C1—C6122.2 (2)C12—C11—H11120.7
C2—C1—C6118.1 (2)C10—C11—H11120.7
C3—C2—C1121.3 (3)C11—C12—H12119.1
C2—C3—C4120.4 (3)C13—C12—H12119.1
C5—C4—C3119.4 (3)C17—C16—H16120.0
C4—C5—C6121.6 (3)C15—C16—H16120.0
C5—C6—C1119.0 (3)C16—C17—H17119.6
C5—C6—C7119.2 (3)C18—C17—H17119.6
C1—C6—C7121.8 (2)C19—C18—H18120.2
O3—C7—O2120.4 (2)C17—C18—H18120.2
O3—C7—C6120.2 (2)C18—C19—H19119.4
O2—C7—C6119.5 (2)C20—C19—H19119.4
O4—C8—C9118.7 (2)N1—C22—H22a109.5
O4—C8—C13123.3 (2)N1—C22—H22b109.5
C9—C8—C13118.0 (3)H22a—C22—H22b109.5
C10—C9—C8120.8 (3)N1—C22—H22c109.5
C9—C10—C11121.0 (3)H22a—C22—H22c109.5
C12—C11—C10118.7 (3)H22b—C22—H22c109.5
C11—C12—C13121.8 (3)N1—C23—H23a109.5
C12—C13—C8119.3 (2)N1—C23—H23b109.5
C12—C13—C14119.6 (2)H23a—C23—H23b109.5
C8—C13—C14121.0 (2)N1—C23—H23c109.5
O6—C14—O5120.3 (2)H23a—C23—H23c109.5
O6—C14—C13119.4 (2)H23b—C23—H23c109.5
O5—C14—C13120.3 (2)N2—C24—H24a109.5
O7—C15—C20122.4 (2)N2—C24—H24b109.5
O7—C15—C16118.2 (2)H24a—C24—H24b109.5
C20—C15—C16119.4 (2)N2—C24—H24c109.5
C17—C16—C15120.0 (3)H24a—C24—H24c109.5
C16—C17—C18120.7 (3)H24b—C24—H24c109.5
C19—C18—C17119.7 (3)N2—C25—H25a109.5
C18—C19—C20121.2 (3)N2—C25—H25b109.5
C15—C20—C19118.9 (3)H25a—C25—H25b109.5
C15—C20—C21123.0 (2)N2—C25—H25c109.5
C19—C20—C21118.1 (3)H25a—C25—H25c109.5
O9—C21—O8121.4 (2)H25b—C25—H25c109.5
O7—Ti1—O1—C182.4 (2)C1—C6—C7—O3170.2 (3)
O4—Ti1—O1—C1100.5 (2)C5—C6—C7—O2168.1 (2)
O8—Ti1—O1—C1169.8 (2)C1—C6—C7—O211.0 (4)
O2—Ti1—O1—C17.8 (2)Ti1—O4—C8—C9159.9 (2)
O1—Ti1—O2—C77.4 (2)Ti1—O4—C8—C1320.2 (4)
O7—Ti1—O2—C7104.9 (2)O4—C8—C9—C10174.7 (3)
O4—Ti1—O2—C786.5 (2)C13—C8—C9—C105.3 (4)
O5—Ti1—O2—C7170.0 (2)C8—C9—C10—C110.4 (5)
O1—Ti1—O4—C8152.6 (2)C9—C10—C11—C124.0 (5)
O7—Ti1—O4—C813.4 (6)C10—C11—C12—C133.4 (5)
O8—Ti1—O4—C856.2 (2)C11—C12—C13—C81.6 (4)
O2—Ti1—O4—C8120.9 (2)C11—C12—C13—C14174.6 (3)
O5—Ti1—O4—C831.7 (2)O4—C8—C13—C12174.2 (2)
O7—Ti1—O5—C14147.7 (2)C9—C8—C13—C125.8 (4)
O4—Ti1—O5—C1428.6 (2)O4—C8—C13—C149.7 (4)
O8—Ti1—O5—C1460.9 (2)C9—C8—C13—C14170.2 (2)
O2—Ti1—O5—C14121.6 (2)Ti1—O5—C14—O6168.6 (2)
O1—Ti1—O7—C15115.1 (2)Ti1—O5—C14—C1313.4 (4)
O4—Ti1—O7—C1550.8 (6)C12—C13—C14—O69.8 (4)
O8—Ti1—O7—C1519.0 (2)C8—C13—C14—O6166.3 (2)
O2—Ti1—O7—C15158.5 (2)C12—C13—C14—O5172.2 (2)
O5—Ti1—O7—C1569.1 (2)C8—C13—C14—O511.7 (4)
O1—Ti1—O8—C21123.1 (2)Ti1—O7—C15—C2010.3 (4)
O7—Ti1—O8—C2125.9 (2)Ti1—O7—C15—C16170.0 (2)
O4—Ti1—O8—C21142.8 (2)O7—C15—C16—C17178.4 (3)
O5—Ti1—O8—C2159.3 (2)C20—C15—C16—C171.2 (4)
Ti1—O1—C1—C2166.7 (2)C15—C16—C17—C182.2 (5)
Ti1—O1—C1—C612.4 (4)C16—C17—C18—C191.5 (6)
O1—C1—C2—C3179.3 (2)C17—C18—C19—C200.2 (6)
C6—C1—C2—C31.6 (4)O7—C15—C20—C19179.9 (3)
C1—C2—C3—C40.0 (4)C16—C15—C20—C190.5 (4)
C2—C3—C4—C51.1 (5)O7—C15—C20—C212.2 (4)
C3—C4—C5—C60.6 (5)C16—C15—C20—C21177.4 (2)
C4—C5—C6—C11.1 (4)C18—C19—C20—C151.2 (5)
C4—C5—C6—C7178.0 (3)C18—C19—C20—C21176.8 (3)
O1—C1—C6—C5178.8 (2)Ti1—O8—C21—O9158.0 (2)
C2—C1—C6—C52.1 (4)Ti1—O8—C21—C2022.6 (4)
O1—C1—C6—C72.1 (4)C15—C20—C21—O9176.8 (3)
C2—C1—C6—C7176.9 (2)C19—C20—C21—O95.3 (4)
Ti1—O2—C7—O3165.1 (2)C15—C20—C21—O83.8 (4)
Ti1—O2—C7—C616.1 (4)C19—C20—C21—O8174.1 (3)
C5—C6—C7—O310.7 (4)
Hydrogen-bond geometry (Å, º) top
D—H···AD—HH···AD···AD—H···A
N1—H1a···O30.901.922.793 (3)163
N1—H1b···O6i0.901.892.775 (3)169
N2—H2a···O60.901.982.859 (3)165
N2—H2b···O9ii0.901.812.714 (3)177
Symmetry codes: (i) x+1, y+1, z+1; (ii) x+1/2, y+1/2, z+3/2.
 

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