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The octa­hedral tris­(salicylato)titanate entity in polymeric {[Cu(C3H7NO)2]1/2[Cu(H2O)2]1/2[Ti(C7H4O3)3]}n links adjacent bis­(N,N-dimethyl­formamide)copper and diaqua­copper units through the carboxyl­ate O atoms to form a chain motif. Hydrogen bonds within the chain further consolidate the structure. The two independent Cu atoms lie on different sites of \overline{1} symmetry.

Supporting information

cif

Crystallographic Information File (CIF) https://doi.org/10.1107/S1600536806033447/bt2174sup1.cif
Contains datablocks global, I

hkl

Structure factor file (CIF format) https://doi.org/10.1107/S1600536806033447/bt2174Isup2.hkl
Contains datablock I

CCDC reference: 620702

Key indicators

  • Single-crystal X-ray study
  • T = 295 K
  • Mean [sigma](C-C) = 0.009 Å
  • R factor = 0.089
  • wR factor = 0.191
  • Data-to-parameter ratio = 13.8

checkCIF/PLATON results

No syntax errors found



Alert level C CRYSC01_ALERT_1_C The word below has not been recognised as a standard identifier. Yellowish PLAT042_ALERT_1_C Calc. and Rep. MoietyFormula Strings Differ .... ? PLAT213_ALERT_2_C Atom O3 has ADP max/min Ratio ............. 3.40 prola PLAT220_ALERT_2_C Large Non-Solvent C Ueq(max)/Ueq(min) ... 2.72 Ratio PLAT242_ALERT_2_C Check Low Ueq as Compared to Neighbors for Cu1 PLAT341_ALERT_3_C Low Bond Precision on C-C bonds (x 1000) Ang ... 9 PLAT720_ALERT_4_C Number of Unusual/Non-Standard Label(s) ........ 2 PLAT753_ALERT_4_C Torsion Calc -175.91, Rep -176.1(5) ...... Senseless su C18 -C19 -C20 -C21 1.555 1.555 1.555 1.555
0 ALERT level A = In general: serious problem 0 ALERT level B = Potentially serious problem 8 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 3 ALERT type 2 Indicator that the structure model may be wrong or deficient 1 ALERT type 3 Indicator that the structure quality may be low 2 ALERT type 4 Improvement, methodology, query or suggestion 0 ALERT type 5 Informative message, check

Computing details top

Data collection: SMART (Bruker, 2003); cell refinement: SAINT (Bruker, 2003); data reduction: SAINT; program(s) used to solve structure: SHELXS97 (Sheldrick, 1997); program(s) used to refine structure: SHELXL97 (Sheldrick, 1997); molecular graphics: X-SEED (Barbour, 2001); software used to prepare material for publication: SHELXL97.

catena-Poly{hemi[diaquacopper(II)]hemi[bis(N,N-dimethylformide-κO)copper(II)][tris(salicylato-κ2O,O')titanate(IV)]} top
Crystal data top
[Cu(C3H7NO)2]1/2[Cu(H2O)2]1/2[Ti(C7H4O3)3]Z = 2
Mr = 610.86F(000) = 622
Triclinic, P1Dx = 1.651 Mg m3
Hall symbol: -P 1Mo Kα radiation, λ = 0.71073 Å
a = 9.629 (1) ÅCell parameters from 1021 reflections
b = 9.915 (1) Åθ = 2.5–20.2°
c = 14.558 (2) ŵ = 1.25 mm1
α = 70.783 (2)°T = 295 K
β = 85.346 (2)°Block, yellow–green
γ = 69.579 (2)°0.16 × 0.08 × 0.07 mm
V = 1229.1 (2) Å3
Data collection top
Bruker APEX area-detector
diffractometer
4291 independent reflections
Radiation source: fine-focus sealed tube2943 reflections with I > 2σ(I)
Graphite monochromatorRint = 0.056
φ and ω scansθmax = 25.0°, θmin = 1.5°
Absorption correction: multi-scan
(SADABS; Sheldrick, 1996)
h = 1111
Tmin = 0.825, Tmax = 0.917k = 1111
8739 measured reflectionsl = 1717
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)] = 0.089Hydrogen site location: inferred from neighbouring sites
wR(F2) = 0.191H-atom parameters constrained
S = 1.13 w = 1/[σ2(Fo2) + (0.0665P)2 + 1.6052P]
where P = (Fo2 + 2Fc2)/3
4291 reflections(Δ/σ)max = 0.001
310 parametersΔρmax = 0.52 e Å3
0 restraintsΔρmin = 0.40 e Å3
Fractional atomic coordinates and isotropic or equivalent isotropic displacement parameters (Å2) top
xyzUiso*/Ueq
Ti10.2933 (1)0.6136 (2)0.7580 (1)0.0309 (4)
Cu10.50001.00000.50000.0381 (4)
Cu20.50000.50000.50000.0409 (4)
O10.4655 (5)0.5191 (6)0.8374 (3)0.039 (1)
O20.4069 (5)0.7520 (6)0.6785 (3)0.040 (1)
O30.5811 (6)0.8543 (6)0.6250 (3)0.044 (2)
O40.2255 (5)0.4530 (6)0.8172 (3)0.034 (1)
O50.3778 (5)0.5023 (6)0.6593 (3)0.035 (1)
O60.4854 (6)0.3149 (6)0.6026 (4)0.044 (1)
O70.1887 (5)0.7453 (5)0.8254 (3)0.036 (1)
O80.1373 (5)0.7407 (6)0.6535 (3)0.036 (1)
O90.0759 (6)0.8863 (7)0.5786 (4)0.057 (2)
O100.6861 (6)0.4745 (7)0.5588 (4)0.048 (2)
O1w0.3261 (6)0.9473 (7)0.5067 (4)0.077 (2)
N10.9322 (7)0.3793 (8)0.5947 (5)0.043 (2)
C10.5863 (4)0.5507 (5)0.8473 (3)0.027 (2)
C20.6763 (5)0.4623 (5)0.9306 (3)0.041 (2)
C30.8042 (5)0.4892 (6)0.9445 (3)0.051 (2)
C40.8420 (5)0.6045 (6)0.8750 (3)0.049 (2)
C50.7519 (5)0.6929 (5)0.7917 (3)0.034 (2)
C60.6241 (4)0.6660 (5)0.7778 (3)0.025 (2)
C70.5324 (8)0.7641 (8)0.6891 (5)0.027 (2)
C80.2935 (6)0.3042 (5)0.8291 (4)0.039 (2)
C90.2691 (6)0.2010 (6)0.9144 (3)0.048 (2)
C100.3357 (7)0.0458 (6)0.9307 (3)0.060 (3)
C110.4269 (7)0.0062 (5)0.8615 (4)0.066 (3)
C120.4514 (6)0.0971 (6)0.7761 (4)0.050 (2)
C130.3847 (6)0.2523 (6)0.7599 (3)0.036 (2)
C140.4175 (8)0.3636 (10)0.6687 (5)0.036 (2)
C150.0683 (4)0.8727 (5)0.8046 (3)0.035 (2)
C160.0354 (6)0.9513 (6)0.8715 (3)0.051 (2)
C170.0904 (6)1.0805 (6)0.8566 (3)0.057 (3)
C180.1832 (5)1.1311 (5)0.7749 (4)0.058 (3)
C190.1502 (4)1.0525 (5)0.7080 (3)0.046 (2)
C200.0245 (4)0.9233 (4)0.7229 (2)0.032 (2)
C210.0119 (6)0.8493 (6)0.6467 (3)0.032 (2)
C220.8148 (9)0.389 (1)0.5512 (5)0.044 (2)
C230.921 (1)0.469 (1)0.6588 (7)0.067 (3)
C241.077 (1)0.266 (1)0.5928 (7)0.062 (3)
H1w10.25181.02740.48350.115*
H1w20.31190.90320.56570.115*
H20.65100.38520.97710.049*
H30.86450.43001.00020.061*
H40.92760.62240.88420.059*
H50.77720.77000.74520.041*
H90.20810.23570.96070.057*
H100.31940.02330.98780.072*
H110.47150.11000.87240.079*
H120.51240.06230.72990.060*
H160.09750.91740.92610.061*
H170.11241.13310.90130.069*
H180.26731.21760.76500.070*
H190.21231.08640.65340.055*
H220.82690.32830.51200.053*
H23a0.82990.55390.64380.101*
H23b1.00320.50500.64940.101*
H23c0.92250.40660.72530.101*
H24a1.07210.21500.54810.092*
H24b1.10440.19360.65680.092*
H24c1.14920.31550.57230.092*
Atomic displacement parameters (Å2) top
U11U22U33U12U13U23
Ti10.0251 (7)0.0351 (8)0.0270 (7)0.0118 (6)0.0053 (6)0.0002 (6)
Cu10.0260 (7)0.0436 (9)0.0287 (7)0.0129 (6)0.0085 (6)0.0119 (6)
Cu20.0339 (8)0.059 (1)0.0259 (7)0.0143 (7)0.0014 (6)0.0099 (7)
O10.033 (3)0.043 (3)0.033 (3)0.017 (3)0.011 (2)0.005 (2)
O20.034 (3)0.040 (3)0.030 (3)0.022 (3)0.012 (2)0.021 (2)
O30.042 (3)0.048 (3)0.028 (3)0.029 (3)0.012 (2)0.024 (2)
O40.028 (3)0.039 (3)0.035 (3)0.016 (2)0.007 (2)0.007 (2)
O50.035 (3)0.034 (3)0.031 (3)0.009 (3)0.004 (2)0.007 (2)
O60.045 (3)0.047 (4)0.036 (3)0.013 (3)0.005 (3)0.013 (3)
O70.041 (3)0.033 (3)0.026 (3)0.009 (3)0.013 (2)0.001 (2)
O80.026 (3)0.043 (3)0.028 (3)0.003 (2)0.012 (2)0.004 (2)
O90.041 (4)0.078 (5)0.045 (4)0.002 (3)0.021 (3)0.024 (3)
O100.039 (4)0.061 (4)0.038 (3)0.016 (3)0.008 (3)0.009 (3)
O1w0.040 (4)0.092 (5)0.062 (4)0.040 (4)0.024 (3)0.048 (4)
N10.041 (4)0.049 (4)0.038 (4)0.013 (3)0.006 (3)0.015 (3)
C10.022 (4)0.039 (4)0.018 (3)0.009 (3)0.004 (3)0.008 (3)
C20.041 (5)0.056 (6)0.016 (4)0.020 (4)0.006 (3)0.005 (4)
C30.052 (6)0.069 (6)0.021 (4)0.018 (5)0.017 (4)0.000 (4)
C40.039 (5)0.073 (6)0.034 (5)0.028 (5)0.016 (4)0.004 (4)
C50.044 (5)0.034 (5)0.024 (4)0.021 (4)0.012 (3)0.003 (3)
C60.028 (4)0.016 (4)0.026 (4)0.001 (3)0.003 (3)0.005 (3)
C70.030 (4)0.026 (4)0.020 (4)0.009 (3)0.003 (3)0.002 (3)
C80.039 (5)0.048 (6)0.038 (5)0.023 (4)0.002 (4)0.013 (4)
C90.056 (6)0.058 (6)0.034 (5)0.029 (5)0.017 (4)0.013 (4)
C100.081 (7)0.044 (6)0.048 (6)0.028 (5)0.005 (5)0.000 (5)
C110.084 (8)0.050 (6)0.062 (7)0.027 (6)0.007 (6)0.011 (5)
C120.052 (6)0.061 (6)0.048 (5)0.025 (5)0.016 (4)0.029 (5)
C130.032 (4)0.042 (5)0.033 (4)0.011 (4)0.007 (4)0.011 (4)
C140.024 (4)0.052 (6)0.029 (4)0.008 (4)0.008 (3)0.015 (4)
C150.047 (5)0.033 (5)0.024 (4)0.017 (4)0.002 (4)0.006 (3)
C160.071 (6)0.039 (5)0.033 (5)0.012 (5)0.009 (4)0.003 (4)
C170.069 (7)0.057 (6)0.044 (6)0.019 (5)0.013 (5)0.019 (5)
C180.051 (6)0.051 (6)0.063 (6)0.006 (5)0.000 (5)0.019 (5)
C190.038 (5)0.040 (5)0.056 (6)0.011 (4)0.002 (4)0.014 (4)
C200.032 (4)0.032 (4)0.032 (4)0.016 (4)0.003 (3)0.003 (3)
C210.029 (4)0.033 (5)0.031 (4)0.013 (4)0.010 (3)0.000 (3)
C220.042 (5)0.062 (6)0.028 (4)0.026 (5)0.004 (4)0.007 (4)
C230.058 (6)0.091 (8)0.066 (7)0.021 (6)0.011 (5)0.043 (6)
C240.047 (6)0.070 (7)0.075 (7)0.022 (5)0.008 (5)0.033 (6)
Geometric parameters (Å, º) top
Ti1—O11.865 (5)C8—C131.3900
Ti1—O22.054 (5)C9—C101.3900
Ti1—O41.853 (5)C10—C111.3900
Ti1—O52.043 (5)C12—C131.3900
Ti1—O71.857 (5)C11—C121.3900
Ti1—O81.986 (5)C13—C141.513 (9)
Cu1—O31.929 (4)C15—C161.3900
Cu1—O3i1.929 (4)C15—C201.3900
Cu1—O1w1.907 (5)C16—C171.3900
Cu1—O1wi1.907 (5)C17—C181.3900
Cu2—O61.990 (5)C18—C191.3900
Cu2—O6ii1.990 (5)C19—C201.3900
Cu2—O101.949 (5)C20—C211.4783
Cu2—O10ii1.949 (5)O1w—H1w10.85
O1—C11.335 (5)O1w—H1w20.85
O2—C71.282 (8)C2—H20.93
O3—C71.250 (8)C3—H30.93
O4—C81.346 (6)C4—H40.93
O5—C141.254 (9)C5—H50.93
O6—C141.253 (9)C9—H90.93
O7—C151.347 (6)C10—H100.93
O8—C211.292 (7)C11—H110.93
O9—C211.229 (7)C12—H120.93
O10—C221.255 (9)C16—H160.93
N1—C221.300 (9)C17—H170.93
N1—C241.46 (1)C18—H180.93
N1—C231.46 (1)C19—H190.93
C1—C21.3900C22—H220.93
C1—C61.3900C23—H23a0.96
C2—C31.3900C23—H23b0.96
C3—C41.3900C23—H23c0.96
C4—C51.3900C24—H24a0.96
C5—C61.3900C24—H24b0.96
C6—C71.467 (7)C24—H24c0.96
C8—C91.3900
O1—Ti1—O283.2 (2)O6—C14—O5120.4 (7)
O1—Ti1—O492.0 (2)O6—C14—C13118.9 (7)
O1—Ti1—O594.2 (2)O5—C14—C13120.8 (7)
O1—Ti1—O797.4 (2)O7—C15—C16116.8 (3)
O1—Ti1—O8166.8 (2)O7—C15—C20123.1 (3)
O2—Ti1—O4165.4 (2)C16—C15—C20120.0
O2—Ti1—O582.1 (2)C17—C16—C15120.0
O2—Ti1—O794.5 (2)C16—C17—C18120.0
O2—Ti1—O883.7 (2)C19—C18—C17120.0
O4—Ti1—O584.5 (2)C20—C19—C18120.0
O4—Ti1—O799.7 (2)C19—C20—C15120.0
O4—Ti1—O8100.3 (2)C19—C20—C21118.2
O5—Ti1—O7167.5 (2)C15—C20—C21121.7
O5—Ti1—O882.3 (2)O9—C21—O8119.6 (4)
O7—Ti1—O885.4 (2)O9—C21—C20121.5 (4)
O3—Cu1—O3i180O8—C21—C20118.9 (3)
O3—Cu1—O1w94.3 (2)O10—C22—N1124.1 (8)
O3—Cu1—O1wi85.7 (2)Cu1—O1w—H1w1109.5
O1w—Cu1—O1wi180Cu1—O1w—H1w2109.5
O6—Cu2—O6ii180H1w1—O1w—H1w2109.5
O6—Cu2—O1091.2 (2)C3—C2—H2120.0
O6—Cu2—O10ii88.8 (2)C1—C2—H2120.0
O10—Cu2—O10ii180C2—C3—H3120.0
C1—O1—Ti1136.5 (4)C4—C3—H3120.0
C7—O2—Ti1134.8 (4)C5—C4—H4120.0
C7—O3—Cu1132.5 (5)C3—C4—H4120.0
C8—O4—Ti1129.0 (4)C6—C5—H5120.0
C14—O5—Ti1130.3 (5)C4—C5—H5120.0
C14—O6—Cu2104.0 (5)C8—C9—H9120.0
C15—O7—Ti1134.7 (4)C10—C9—H9120.0
C21—O8—Ti1134.8 (4)C11—C10—H10120.0
C22—O10—Cu2129.0 (6)C9—C10—H10120.0
C22—N1—C24122.3 (7)C10—C11—H11120.0
C22—N1—C23120.9 (7)C12—C11—H11120.0
C24—N1—C23116.4 (7)C13—C12—H12120.0
O1—C1—C2117.5 (3)C11—C12—H12120.0
O1—C1—C6122.5 (3)C17—C16—H16120.0
C2—C1—C6120.0C15—C16—H16120.0
C3—C2—C1120.0C16—C17—H17120.0
C2—C3—C4120.0C18—C17—H17120.0
C5—C4—C3120.0C19—C18—H18120.0
C6—C5—C4120.0C17—C18—H18120.0
C5—C6—C1120.0C20—C19—H19120.0
C5—C6—C7117.6 (4)C18—C19—H19120.0
C1—C6—C7122.4 (4)O10—C22—H22118.0
O3—C7—O2122.0 (6)N1—C22—H22118.0
O3—C7—C6118.8 (6)N1—C23—H23a109.5
O2—C7—C6119.2 (5)N1—C23—H23b109.5
O4—C8—C9117.3 (4)H23a—C23—H23b109.5
O4—C8—C13122.7 (4)N1—C23—H23c109.5
C9—C8—C13120.0H23a—C23—H23c109.5
C8—C9—C10120.0H23b—C23—H23c109.5
C11—C10—C9120.0N1—C24—H24a109.5
C10—C11—C12120.0N1—C24—H24b109.5
C13—C12—C11120.0H24a—C24—H24b109.5
C12—C13—C8120.0N1—C24—H24c109.5
C12—C13—C14119.5 (5)H24a—C24—H24c109.5
C8—C13—C14120.4 (5)H24b—C24—H24c109.5
O4—Ti1—O1—C1179.3 (6)O1—C1—C6—C71.4 (6)
O7—Ti1—O1—C180.7 (6)C2—C1—C6—C7179.2 (5)
O8—Ti1—O1—C120.6 (14)Cu1—O3—C7—O22 (1)
O5—Ti1—O1—C194.6 (6)Cu1—O3—C7—C6179.8 (4)
O2—Ti1—O1—C113.1 (6)Ti1—O2—C7—O3175.2 (5)
O4—Ti1—O2—C776 (1)Ti1—O2—C7—C63 (1)
O7—Ti1—O2—C792.7 (7)C5—C6—C7—O38.5 (8)
O1—Ti1—O2—C74.2 (7)C1—C6—C7—O3172.3 (5)
O8—Ti1—O2—C7177.5 (7)C5—C6—C7—O2173.5 (5)
O5—Ti1—O2—C799.4 (7)C1—C6—C7—O25.8 (8)
O1w—Cu1—O3—C73.4 (8)Ti1—O4—C8—C9144.6 (4)
O1wi—Cu1—O3—C7176.6 (8)Ti1—O4—C8—C1335.7 (7)
O7—Ti1—O4—C8152.5 (5)O4—C8—C9—C10179.7 (5)
O1—Ti1—O4—C854.7 (5)C11—C12—C13—C14177.4 (5)
O8—Ti1—O4—C8120.5 (5)O4—C8—C13—C12179.7 (5)
O5—Ti1—O4—C839.3 (5)O4—C8—C13—C143.0 (6)
O2—Ti1—O4—C816 (1)C9—C8—C13—C14177.3 (5)
O4—Ti1—O5—C1426.9 (6)Cu2—O6—C14—O50.6 (8)
O7—Ti1—O5—C14138 (1)Cu2—O6—C14—C13179.5 (5)
O1—Ti1—O5—C1464.8 (6)Ti1—O5—C14—O6170.3 (5)
O8—Ti1—O5—C14128.0 (6)Ti1—O5—C14—C139.5 (9)
O2—Ti1—O5—C14147.3 (6)C12—C13—C14—O610.9 (8)
O10ii—Cu2—O6—C1491.3 (5)C8—C13—C14—O6171.7 (5)
O10—Cu2—O6—C1488.7 (5)C12—C13—C14—O5168.9 (5)
O4—Ti1—O7—C15103.6 (6)C8—C13—C14—O58.5 (8)
O1—Ti1—O7—C15163.1 (5)Ti1—O7—C15—C16171.5 (4)
O8—Ti1—O7—C153.9 (5)Ti1—O7—C15—C2011.1 (8)
O5—Ti1—O7—C155.6 (14)O7—C15—C16—C17177.6 (5)
O2—Ti1—O7—C1579.4 (6)C18—C19—C20—C21176.1 (5)
O4—Ti1—O8—C2190.2 (6)O7—C15—C20—C19177.4 (5)
O7—Ti1—O8—C218.9 (6)O7—C15—C20—C216.8 (5)
O1—Ti1—O8—C21112 (1)C16—C15—C20—C21175.8
O5—Ti1—O8—C21173.2 (6)Ti1—O8—C21—O9165.2 (5)
O2—Ti1—O8—C21103.9 (6)Ti1—O8—C21—C2013.1 (7)
O6—Cu2—O10—C2281.1 (7)C19—C20—C21—O910.1 (6)
O6ii—Cu2—O10—C2298.9 (7)C15—C20—C21—O9174.0 (6)
Ti1—O1—C1—C2166.6 (4)C19—C20—C21—O8171.7 (5)
Ti1—O1—C1—C614.0 (8)C15—C20—C21—O84.2 (5)
O1—C1—C2—C3179.4 (5)Cu2—O10—C22—N1179.3 (5)
C4—C5—C6—C7179.2 (5)C24—N1—C22—O10172.8 (8)
O1—C1—C6—C5179.4 (5)C23—N1—C22—O101.2 (13)
Symmetry codes: (i) x+1, y+2, z+1; (ii) x+1, y+1, z+1.
Hydrogen-bond geometry (Å, º) top
D—H···AD—HH···AD···AD—H···A
O1w—H1w1···O9iii0.851.772.536 (7)148
O1w—H1w2···O20.851.862.586 (7)143
Symmetry code: (iii) x, y+2, z+1.
 

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