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In the title complex, [Ni(C8H4O4)(C12H30N6)]n, the 14-membered hexa­aza­cyclo­tetra­decane macrocycle ring chelates to the Ni atom through its four secondary N atoms; the Ni atom and the terephthalate anion lie on inversion centers. The terephthalate dianion links adjacent nickel–macrocycle cations through the carboxyl O atoms [Ni—O 2.144 (2) Å] into a linear chain.

Supporting information

cif

Crystallographic Information File (CIF) https://doi.org/10.1107/S160053680400251X/dn6120sup1.cif
Contains datablocks I, global

hkl

Structure factor file (CIF format) https://doi.org/10.1107/S160053680400251X/dn6120Isup2.hkl
Contains datablock I

CCDC reference: 236042

Key indicators

  • Single-crystal X-ray study
  • T = 298 K
  • Mean [sigma](C-C) = 0.003 Å
  • R factor = 0.030
  • wR factor = 0.081
  • Data-to-parameter ratio = 17.5

checkCIF/PLATON results

No syntax errors found



Alert level A PLAT761_ALERT_1_A CIF Contains no X-H Bonds ...................... ? PLAT762_ALERT_1_A CIF Contains no X-Y-H or H-Y-H Angles .......... ?
Alert level C PLAT029_ALERT_3_C _diffrn_measured_fraction_theta_full Low ....... 0.97 PLAT042_ALERT_1_C Calc. and Rep. MoietyFormula Strings Differ .... ? PLAT220_ALERT_2_C Large Non-Solvent C Ueq(max)/Ueq(min) ... 2.82 Ratio PLAT222_ALERT_3_C Large Non-Solvent H Ueq(max)/Ueq(min) ... 3.11 Ratio PLAT420_ALERT_2_C D-H Without Acceptor N1 - H1 ... ?
2 ALERT level A = In general: serious problem 0 ALERT level B = Potentially serious problem 5 ALERT level C = Check and explain 0 ALERT level G = General alerts; check 3 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 2 ALERT type 3 Indicator that the structure quality may be low 0 ALERT type 4 Improvement, methodology, query or suggestion

Computing details top

Data collection: SMART (Bruker, 1999); cell refinement: SAINT (Bruker, 1999); data reduction: SAINT; program(s) used to solve structure: SHELXS97 (Sheldrick, 1997); program(s) used to refine structure: SHELXL97 (Sheldrick, 1997); molecular graphics: ORTEPIII (Burnett & Johnson, 1996) and ORTEP-3 for Windows (Farrugia, 1997); software used to prepare material for publication: SHELXL97.

catena-Poly[[(3,10-diethyl-1,3,5,8,10,12-hexaazacyclotetradecane)nickel(II)]- µ-terephthalato] top
Crystal data top
[Ni(C8H4O4)·(C12H30N6)]Z = 1
Mr = 481.24F(000) = 256
Triclinic, P1Dx = 1.421 Mg m3
Hall symbol: -P 1Mo Kα radiation, λ = 0.71073 Å
a = 7.5818 (5) ÅCell parameters from 2995 reflections
b = 8.3976 (5) Åθ = 4.0–30.0°
c = 9.7596 (6) ŵ = 0.90 mm1
α = 105.506 (1)°T = 298 K
β = 97.283 (1)°Plate, yellow
γ = 105.853 (1)°0.27 × 0.23 × 0.08 mm
V = 562.45 (6) Å3
Data collection top
Bruker SMART 1K area-detector
diffractometer
2500 independent reflections
Radiation source: medium-focus sealed tube2397 reflections with I > 2σ(I)
Graphite monochromatorRint = 0.010
Detector resolution: 8.33 pixels mm-1θmax = 27.5°, θmin = 4.3°
φ and ω scansh = 99
Absorption correction: multi-scan
(SADABS; Sheldrick, 1996)
k = 710
Tmin = 0.792, Tmax = 0.931l = 1212
3389 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)] = 0.030Hydrogen site location: inferred from neighbouring sites
wR(F2) = 0.081H-atom parameters constrained
S = 1.05 w = 1/[σ2(Fo2) + (0.0496P)2 + 0.1456P]
where P = (Fo2 + 2Fc2)/3
2500 reflections(Δ/σ)max = 0.001
143 parametersΔρmax = 0.42 e Å3
0 restraintsΔρmin = 0.25 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*/Ueq
Ni10.50000.50000.50000.02670 (10)
O10.70930 (17)0.50960 (15)0.67450 (13)0.0394 (3)
O20.7174 (3)0.23744 (19)0.63580 (16)0.0692 (5)
N10.7031 (2)0.53250 (19)0.37877 (16)0.0368 (3)
H10.80430.51370.42420.044*
N20.5859 (2)0.2276 (2)0.22423 (17)0.0437 (4)
N30.41514 (19)0.23181 (17)0.42201 (14)0.0322 (3)
H30.49800.19680.47300.039*
C10.6401 (3)0.4055 (3)0.2276 (2)0.0444 (4)
H1A0.53470.42610.17630.053*
H1B0.74140.42630.17640.053*
C20.4131 (3)0.1583 (2)0.26518 (18)0.0398 (4)
H2A0.38390.03280.24090.048*
H2B0.31340.18020.20800.048*
C30.2329 (3)0.1704 (2)0.4606 (2)0.0434 (4)
H3A0.20520.04910.45630.052*
H3B0.13420.17900.39200.052*
C40.7592 (3)0.7181 (3)0.3862 (2)0.0477 (4)
H4A0.66920.73560.31660.057*
H4B0.88140.75170.36220.057*
C50.7394 (3)0.1609 (3)0.2609 (2)0.0546 (5)
H5A0.73250.13480.35140.066*
H5B0.85840.25090.27600.066*
C60.7338 (5)0.0014 (4)0.1460 (3)0.0787 (8)
H6A0.61940.09030.13440.118*
H6B0.83920.03430.17380.118*
H6C0.73910.02590.05580.118*
C70.7602 (2)0.3927 (2)0.71099 (17)0.0337 (3)
C80.8831 (2)0.4493 (2)0.86186 (16)0.0278 (3)
C90.9303 (2)0.6184 (2)0.95599 (17)0.0321 (3)
H90.88330.69850.92720.038*
C100.9536 (2)0.3308 (2)0.90788 (17)0.0317 (3)
H100.92230.21680.84660.038*
Atomic displacement parameters (Å2) top
U11U22U33U12U13U23
Ni10.03022 (16)0.02514 (15)0.02236 (15)0.00937 (10)0.00228 (10)0.00683 (10)
O10.0460 (7)0.0347 (6)0.0326 (6)0.0147 (5)0.0122 (5)0.0105 (5)
O20.1018 (13)0.0464 (8)0.0435 (8)0.0420 (8)0.0340 (8)0.0070 (6)
N10.0371 (7)0.0376 (7)0.0348 (7)0.0131 (6)0.0043 (6)0.0104 (6)
N20.0488 (8)0.0448 (8)0.0353 (8)0.0237 (7)0.0035 (6)0.0027 (6)
N30.0342 (7)0.0286 (6)0.0300 (7)0.0111 (5)0.0048 (5)0.0078 (5)
C10.0509 (10)0.0505 (10)0.0320 (9)0.0186 (8)0.0106 (7)0.0101 (7)
C20.0456 (9)0.0322 (8)0.0318 (8)0.0144 (7)0.0080 (7)0.0000 (6)
C30.0396 (9)0.0313 (8)0.0522 (11)0.0053 (7)0.0023 (8)0.0114 (7)
C40.0507 (10)0.0425 (10)0.0507 (11)0.0095 (8)0.0168 (9)0.0190 (8)
C50.0567 (12)0.0688 (14)0.0412 (10)0.0368 (11)0.0046 (9)0.0078 (9)
C60.100 (2)0.0658 (15)0.0746 (17)0.0551 (15)0.0066 (15)0.0064 (13)
C70.0378 (8)0.0374 (8)0.0254 (7)0.0178 (7)0.0040 (6)0.0080 (6)
C80.0277 (7)0.0326 (7)0.0233 (7)0.0119 (6)0.0012 (5)0.0100 (6)
C90.0363 (8)0.0319 (7)0.0295 (7)0.0160 (6)0.0027 (6)0.0113 (6)
C100.0371 (8)0.0282 (7)0.0271 (7)0.0131 (6)0.0036 (6)0.0063 (6)
Geometric parameters (Å, º) top
Ni1—N32.0574 (13)N2—C51.468 (2)
Ni1—N12.0617 (14)N3—C31.471 (2)
Ni1—O12.1440 (11)N3—C21.486 (2)
O1—C71.2644 (19)C3—C4i1.521 (3)
O2—C71.241 (2)C5—C61.485 (3)
N1—C41.478 (2)C7—C81.516 (2)
N1—C11.498 (2)C8—C91.389 (2)
N2—C11.426 (3)C8—C101.395 (2)
N2—C21.434 (3)C9—C10ii1.385 (2)
N3—Ni1—N194.25 (6)C2—N3—Ni1114.62 (10)
N3i—Ni1—N185.75 (6)N2—C1—N1113.35 (15)
N3—Ni1—O192.27 (5)N2—C2—N3114.44 (13)
N3i—Ni1—O187.73 (5)N3—C3—C4i109.04 (14)
N1—Ni1—O188.64 (6)N1—C4—C3i109.17 (15)
N1i—Ni1—O191.36 (6)N2—C5—C6112.85 (18)
C7—O1—Ni1132.79 (11)O2—C7—O1126.14 (14)
C4—N1—C1114.75 (15)O2—C7—C8117.72 (14)
C4—N1—Ni1106.09 (11)O1—C7—C8116.14 (14)
C1—N1—Ni1112.67 (11)C9—C8—C10118.61 (13)
C1—N2—C2118.14 (14)C9—C8—C7121.55 (13)
C1—N2—C5116.07 (17)C10—C8—C7119.83 (14)
C2—N2—C5116.98 (17)C10ii—C9—C8120.82 (14)
C3—N3—C2113.98 (13)C9ii—C10—C8120.57 (14)
C3—N3—Ni1106.17 (10)
Symmetry codes: (i) x+1, y+1, z+1; (ii) x+2, y+1, z+2.
Hydrogen-bond geometry (Å, º) top
D—H···AD—HH···AD···AD—H···A
N3—H3···O20.912.032.878 (2)154
 

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