Supporting information
Crystallographic Information File (CIF) https://doi.org/10.1107/S1600536801002963/ob6029sup1.cif | |
Structure factor file (CIF format) https://doi.org/10.1107/S1600536801002963/ob6029Isup2.hkl |
CCDC reference: 159835
La(NO3)3 (0.5 mmol) in methanol (30 ml) was added dropwise to a solution (methanol–H2O, 1:1, 30 ml) of phen (0.5 mmol) and benzoic acid (1.5 mmol). The mixture was heated and refluxed for 10 h to give a pink solution. The solution was filtered at room temperature and crystals of (I) were obtained after 6 d.
The positions of all H atoms were generated geometrically (C—H distance fixed at 0.96 Å), and allowed to ride on their respective parent C atoms.
Data collection: SMART (Siemens, 1994); cell refinement: SMART; data reduction: SMART; program(s) used to solve structure: SHELXS97 (Sheldrick, 1997); program(s) used to refine structure: SHELXL97 (Sheldrick, 1997); molecular graphics: SHELXL97; software used to prepare material for publication: SHELXL97.
Fig. 1. A view of (I) with the atomic numbering scheme. Displacement ellipsoids are drawn at the 30% probability level. |
[La2(C7H5O2)6(C12H8N2)2] | Z = 1 |
Mr = 1364.92 | F(000) = 679 |
Triclinic, P1 | Dx = 1.585 Mg m−3 |
a = 10.9356 (2) Å | Mo Kα radiation, λ = 0.71073 Å |
b = 11.9818 (2) Å | Cell parameters from 120 reflections |
c = 12.4945 (3) Å | θ = 1.7–25.0° |
α = 104.888 (1)° | µ = 1.54 mm−1 |
β = 93.268 (1)° | T = 293 K |
γ = 113.402 (1)° | Plane, pink |
V = 1428.48 (5) Å3 | 0.31 × 0.21 × 0.20 mm |
Siemens Smart CCD diffractometer | 4901 independent reflections |
Radiation source: fine-focus sealed tube | 4427 reflections with I > 2σ(I) |
Graphite monochromator | Rint = 0.019 |
ω scans | θmax = 25.0°, θmin = 1.7° |
Absorption correction: empirical (using intensity measurements) (SADABS; Sheldrick, 1996) | h = −13→13 |
Tmin = 0.546, Tmax = 0.734 | k = −13→14 |
7321 measured reflections | l = −14→9 |
Refinement on F2 | Secondary atom site location: difference Fourier map |
Least-squares matrix: full | Hydrogen site location: inferred from neighbouring sites |
R[F2 > 2σ(F2)] = 0.024 | H-atom parameters constrained |
wR(F2) = 0.060 | w = 1/[σ2(Fo2) + (0.0302P)2 + 0.0941P] where P = (Fo2 + 2Fc2)/3 |
S = 1.04 | (Δ/σ)max = 0.017 |
4901 reflections | Δρmax = 0.61 e Å−3 |
380 parameters | Δρmin = −0.59 e Å−3 |
0 restraints | Extinction correction: SHELXL97, Fc*=kFc[1+0.001xFc2λ3/sin(2θ)]-1/4 |
Primary atom site location: structure-invariant direct methods | Extinction coefficient: 0.0022 (4) |
[La2(C7H5O2)6(C12H8N2)2] | γ = 113.402 (1)° |
Mr = 1364.92 | V = 1428.48 (5) Å3 |
Triclinic, P1 | Z = 1 |
a = 10.9356 (2) Å | Mo Kα radiation |
b = 11.9818 (2) Å | µ = 1.54 mm−1 |
c = 12.4945 (3) Å | T = 293 K |
α = 104.888 (1)° | 0.31 × 0.21 × 0.20 mm |
β = 93.268 (1)° |
Siemens Smart CCD diffractometer | 4901 independent reflections |
Absorption correction: empirical (using intensity measurements) (SADABS; Sheldrick, 1996) | 4427 reflections with I > 2σ(I) |
Tmin = 0.546, Tmax = 0.734 | Rint = 0.019 |
7321 measured reflections |
R[F2 > 2σ(F2)] = 0.024 | 0 restraints |
wR(F2) = 0.060 | H-atom parameters constrained |
S = 1.04 | Δρmax = 0.61 e Å−3 |
4901 reflections | Δρmin = −0.59 e Å−3 |
380 parameters |
x | y | z | Uiso*/Ueq | ||
La | −0.135359 (14) | −0.064305 (13) | −0.147434 (12) | 0.03130 (7) | |
O1 | −0.1594 (2) | 0.14151 (19) | −0.06398 (19) | 0.0532 (6) | |
O2 | −0.00697 (19) | 0.14069 (18) | 0.05750 (17) | 0.0420 (5) | |
O3 | −0.24532 (19) | −0.13991 (19) | 0.00349 (17) | 0.0444 (5) | |
O4 | −0.09329 (19) | −0.09061 (19) | 0.15456 (17) | 0.0469 (5) | |
O5 | −0.0776 (2) | −0.18940 (18) | −0.32531 (17) | 0.0470 (5) | |
O6 | −0.27652 (19) | −0.28549 (18) | −0.27926 (17) | 0.0465 (5) | |
N1 | −0.1939 (2) | 0.0122 (2) | −0.3216 (2) | 0.0414 (5) | |
N2 | −0.3883 (2) | −0.0725 (2) | −0.1963 (2) | 0.0392 (5) | |
C1 | −0.1033 (3) | 0.0481 (3) | −0.3865 (3) | 0.0499 (7) | |
H1 | −0.0300 | 0.0274 | −0.3826 | 0.060* | |
C2 | −0.1123 (4) | 0.1156 (3) | −0.4605 (3) | 0.0578 (9) | |
H2 | −0.0485 | 0.1361 | −0.5068 | 0.069* | |
C3 | −0.2159 (4) | 0.1506 (3) | −0.4635 (3) | 0.0581 (9) | |
H3 | −0.2212 | 0.1988 | −0.5097 | 0.070* | |
C4 | −0.3144 (3) | 0.1146 (3) | −0.3973 (3) | 0.0485 (7) | |
C5 | −0.4279 (4) | 0.1459 (3) | −0.3971 (3) | 0.0612 (9) | |
H5 | −0.4353 | 0.1964 | −0.4402 | 0.073* | |
C6 | −0.5232 (4) | 0.1043 (3) | −0.3364 (3) | 0.0616 (9) | |
H6 | −0.5959 | 0.1259 | −0.3384 | 0.074* | |
C7 | −0.5155 (3) | 0.0267 (3) | −0.2683 (3) | 0.0468 (7) | |
C8 | −0.6144 (3) | −0.0214 (3) | −0.2047 (3) | 0.0568 (9) | |
H8 | −0.6912 | −0.0059 | −0.2077 | 0.068* | |
C9 | −0.5985 (3) | −0.0902 (3) | −0.1392 (3) | 0.0547 (8) | |
H9 | −0.6631 | −0.1213 | −0.0961 | 0.066* | |
C10 | −0.4830 (3) | −0.1140 (3) | −0.1375 (3) | 0.0481 (7) | |
H10 | −0.4728 | −0.1616 | −0.0923 | 0.058* | |
C11 | −0.4034 (3) | −0.0023 (3) | −0.2620 (2) | 0.0385 (6) | |
C12 | −0.3009 (3) | 0.0423 (3) | −0.3277 (2) | 0.0398 (6) | |
C25 | −0.0702 (3) | 0.1973 (3) | 0.0226 (2) | 0.0367 (6) | |
C26 | −0.0376 (3) | 0.3331 (2) | 0.0848 (2) | 0.0365 (6) | |
C27 | −0.1281 (3) | 0.3832 (3) | 0.0642 (3) | 0.0476 (7) | |
H27 | −0.2096 | 0.3313 | 0.0145 | 0.057* | |
C28 | −0.0972 (4) | 0.5099 (3) | 0.1173 (3) | 0.0587 (9) | |
H28 | −0.1587 | 0.5429 | 0.1048 | 0.070* | |
C29 | 0.0246 (4) | 0.5869 (3) | 0.1887 (3) | 0.0632 (10) | |
H29 | 0.0458 | 0.6725 | 0.2235 | 0.076* | |
C30 | 0.1146 (4) | 0.5389 (3) | 0.2091 (3) | 0.0605 (9) | |
H30 | 0.1969 | 0.5920 | 0.2574 | 0.073* | |
C31 | 0.0839 (3) | 0.4112 (3) | 0.1578 (3) | 0.0471 (7) | |
H31 | 0.1449 | 0.3783 | 0.1725 | 0.057* | |
C32 | −0.2088 (3) | −0.1552 (2) | 0.0936 (2) | 0.0370 (6) | |
C33 | −0.3104 (3) | −0.2564 (2) | 0.1341 (2) | 0.0377 (6) | |
C34 | −0.4448 (3) | −0.3183 (3) | 0.0809 (3) | 0.0550 (8) | |
H34 | −0.4724 | −0.2972 | 0.0202 | 0.066* | |
C35 | −0.5378 (4) | −0.4113 (4) | 0.1178 (3) | 0.0698 (11) | |
H35 | −0.6279 | −0.4518 | 0.0819 | 0.084* | |
C36 | −0.4993 (4) | −0.4443 (3) | 0.2060 (3) | 0.0671 (10) | |
H36 | −0.5623 | −0.5083 | 0.2293 | 0.081* | |
C37 | −0.3676 (4) | −0.3829 (3) | 0.2601 (3) | 0.0650 (10) | |
H37 | −0.3412 | −0.4049 | 0.3207 | 0.078* | |
C38 | −0.2730 (3) | −0.2881 (3) | 0.2254 (3) | 0.0500 (8) | |
H38 | −0.1839 | −0.2458 | 0.2638 | 0.060* | |
C39 | −0.1889 (3) | −0.2858 (3) | −0.3417 (2) | 0.0376 (6) | |
C40 | −0.2195 (3) | −0.4036 (3) | −0.4372 (2) | 0.0392 (6) | |
C41 | −0.1209 (4) | −0.4147 (3) | −0.4977 (3) | 0.0545 (8) | |
H41 | −0.0335 | −0.3495 | −0.4777 | 0.065* | |
C42 | −0.1520 (5) | −0.5227 (4) | −0.5882 (3) | 0.0714 (11) | |
H42 | −0.0853 | −0.5303 | −0.6284 | 0.086* | |
C43 | −0.2805 (5) | −0.6179 (4) | −0.6181 (3) | 0.0759 (12) | |
H43 | −0.3011 | −0.6897 | −0.6794 | 0.091* | |
C44 | −0.3795 (4) | −0.6087 (3) | −0.5587 (3) | 0.0670 (10) | |
H44 | −0.4671 | −0.6735 | −0.5800 | 0.080* | |
C45 | −0.3483 (3) | −0.5025 (3) | −0.4670 (3) | 0.0495 (7) | |
H45 | −0.4145 | −0.4974 | −0.4250 | 0.059* |
U11 | U22 | U33 | U12 | U13 | U23 | |
La | 0.03122 (10) | 0.02742 (10) | 0.03333 (10) | 0.01076 (7) | 0.00642 (6) | 0.00887 (6) |
O1 | 0.0514 (12) | 0.0375 (11) | 0.0609 (14) | 0.0211 (10) | −0.0101 (11) | 0.0000 (10) |
O2 | 0.0470 (11) | 0.0388 (10) | 0.0498 (12) | 0.0256 (9) | 0.0116 (9) | 0.0169 (9) |
O3 | 0.0410 (11) | 0.0505 (12) | 0.0467 (12) | 0.0173 (9) | 0.0155 (9) | 0.0252 (10) |
O4 | 0.0388 (11) | 0.0417 (11) | 0.0498 (12) | 0.0056 (9) | 0.0094 (9) | 0.0154 (10) |
O5 | 0.0474 (12) | 0.0368 (11) | 0.0471 (12) | 0.0112 (9) | 0.0145 (10) | 0.0070 (9) |
O6 | 0.0421 (11) | 0.0410 (11) | 0.0468 (12) | 0.0127 (9) | 0.0131 (10) | 0.0048 (9) |
N1 | 0.0445 (13) | 0.0411 (13) | 0.0405 (13) | 0.0191 (11) | 0.0098 (11) | 0.0138 (11) |
N2 | 0.0354 (12) | 0.0356 (12) | 0.0413 (13) | 0.0123 (10) | 0.0056 (10) | 0.0082 (10) |
C1 | 0.0551 (18) | 0.0504 (18) | 0.0489 (18) | 0.0235 (15) | 0.0165 (15) | 0.0194 (15) |
C2 | 0.073 (2) | 0.0526 (19) | 0.0503 (19) | 0.0245 (18) | 0.0204 (17) | 0.0221 (16) |
C3 | 0.078 (2) | 0.0501 (19) | 0.0495 (19) | 0.0255 (18) | 0.0083 (17) | 0.0245 (16) |
C4 | 0.0556 (18) | 0.0397 (16) | 0.0453 (17) | 0.0193 (14) | −0.0024 (14) | 0.0093 (14) |
C5 | 0.074 (2) | 0.059 (2) | 0.060 (2) | 0.0384 (19) | −0.0013 (19) | 0.0198 (18) |
C6 | 0.062 (2) | 0.056 (2) | 0.071 (2) | 0.0390 (18) | −0.0004 (19) | 0.0062 (18) |
C7 | 0.0469 (17) | 0.0409 (16) | 0.0472 (17) | 0.0227 (14) | 0.0018 (14) | −0.0003 (13) |
C8 | 0.0467 (18) | 0.0541 (19) | 0.064 (2) | 0.0283 (16) | 0.0054 (16) | −0.0013 (17) |
C9 | 0.0417 (16) | 0.0553 (19) | 0.056 (2) | 0.0181 (15) | 0.0131 (15) | 0.0027 (16) |
C10 | 0.0431 (16) | 0.0448 (17) | 0.0496 (18) | 0.0136 (13) | 0.0102 (14) | 0.0114 (14) |
C11 | 0.0384 (15) | 0.0311 (14) | 0.0358 (15) | 0.0127 (12) | −0.0031 (12) | −0.0008 (12) |
C12 | 0.0446 (16) | 0.0347 (14) | 0.0361 (15) | 0.0172 (13) | 0.0011 (12) | 0.0052 (12) |
C25 | 0.0342 (14) | 0.0330 (14) | 0.0453 (16) | 0.0158 (12) | 0.0123 (13) | 0.0122 (12) |
C26 | 0.0423 (15) | 0.0316 (14) | 0.0386 (15) | 0.0164 (12) | 0.0115 (12) | 0.0135 (12) |
C27 | 0.0500 (17) | 0.0427 (16) | 0.0526 (18) | 0.0246 (14) | 0.0092 (14) | 0.0106 (14) |
C28 | 0.079 (2) | 0.0486 (18) | 0.062 (2) | 0.0418 (18) | 0.0163 (19) | 0.0147 (17) |
C29 | 0.096 (3) | 0.0342 (16) | 0.055 (2) | 0.0294 (18) | 0.009 (2) | 0.0045 (15) |
C30 | 0.069 (2) | 0.0392 (17) | 0.055 (2) | 0.0125 (16) | −0.0056 (17) | 0.0052 (15) |
C31 | 0.0499 (17) | 0.0406 (16) | 0.0471 (17) | 0.0162 (14) | 0.0016 (14) | 0.0139 (14) |
C32 | 0.0379 (15) | 0.0320 (14) | 0.0421 (16) | 0.0140 (12) | 0.0165 (13) | 0.0126 (12) |
C33 | 0.0400 (15) | 0.0294 (13) | 0.0440 (16) | 0.0137 (12) | 0.0164 (12) | 0.0116 (12) |
C34 | 0.0477 (18) | 0.0550 (19) | 0.0517 (19) | 0.0067 (15) | 0.0088 (15) | 0.0238 (16) |
C35 | 0.050 (2) | 0.063 (2) | 0.070 (2) | −0.0059 (17) | 0.0113 (18) | 0.0255 (19) |
C36 | 0.067 (2) | 0.050 (2) | 0.081 (3) | 0.0103 (18) | 0.032 (2) | 0.0337 (19) |
C37 | 0.075 (2) | 0.063 (2) | 0.078 (3) | 0.032 (2) | 0.028 (2) | 0.048 (2) |
C38 | 0.0489 (17) | 0.0478 (17) | 0.065 (2) | 0.0228 (15) | 0.0172 (16) | 0.0313 (16) |
C39 | 0.0419 (15) | 0.0328 (14) | 0.0357 (15) | 0.0141 (13) | 0.0027 (12) | 0.0105 (12) |
C40 | 0.0545 (17) | 0.0350 (14) | 0.0311 (14) | 0.0217 (13) | 0.0043 (12) | 0.0119 (12) |
C41 | 0.070 (2) | 0.0488 (18) | 0.0497 (19) | 0.0295 (16) | 0.0184 (16) | 0.0156 (15) |
C42 | 0.112 (3) | 0.075 (3) | 0.050 (2) | 0.062 (3) | 0.027 (2) | 0.0160 (19) |
C43 | 0.126 (4) | 0.055 (2) | 0.046 (2) | 0.051 (3) | −0.007 (2) | −0.0020 (17) |
C44 | 0.082 (3) | 0.0412 (18) | 0.057 (2) | 0.0186 (18) | −0.017 (2) | 0.0014 (16) |
C45 | 0.0537 (18) | 0.0404 (16) | 0.0464 (18) | 0.0157 (14) | −0.0025 (14) | 0.0098 (14) |
La—O2i | 2.4460 (19) | C6—C7 | 1.433 (5) |
La—O3 | 2.4685 (19) | C7—C11 | 1.404 (4) |
La—O4i | 2.4756 (18) | C7—C8 | 1.404 (5) |
La—O6 | 2.5173 (19) | C8—C9 | 1.351 (5) |
La—O1 | 2.542 (2) | C9—C10 | 1.402 (5) |
La—O5 | 2.6048 (19) | C11—C12 | 1.438 (4) |
La—N1 | 2.704 (2) | C25—C26 | 1.495 (4) |
La—N2 | 2.756 (2) | C26—C31 | 1.382 (4) |
La—O2 | 2.860 (2) | C26—C27 | 1.388 (4) |
O1—C25 | 1.249 (3) | C27—C28 | 1.382 (4) |
O2—C25 | 1.272 (3) | C28—C29 | 1.373 (5) |
O2—Lai | 2.4460 (19) | C29—C30 | 1.364 (5) |
O3—C32 | 1.255 (4) | C30—C31 | 1.389 (4) |
O4—C32 | 1.259 (3) | C32—C33 | 1.506 (4) |
O4—Lai | 2.4756 (18) | C33—C38 | 1.382 (4) |
O5—C39 | 1.262 (3) | C33—C34 | 1.386 (4) |
O6—C39 | 1.270 (3) | C34—C35 | 1.379 (4) |
N1—C1 | 1.325 (4) | C35—C36 | 1.361 (6) |
N1—C12 | 1.358 (4) | C36—C37 | 1.365 (5) |
N2—C10 | 1.314 (4) | C37—C38 | 1.385 (4) |
N2—C11 | 1.363 (4) | C39—C40 | 1.498 (4) |
C1—C2 | 1.399 (5) | C40—C41 | 1.380 (4) |
C2—C3 | 1.357 (5) | C40—C45 | 1.383 (4) |
C3—C4 | 1.395 (5) | C41—C42 | 1.388 (5) |
C4—C12 | 1.416 (4) | C42—C43 | 1.364 (6) |
C4—C5 | 1.432 (5) | C43—C44 | 1.371 (6) |
C5—C6 | 1.334 (5) | C44—C45 | 1.382 (4) |
O2i—La—O3 | 72.52 (7) | C2—C3—C4 | 120.2 (3) |
O2i—La—O4i | 79.10 (7) | C3—C4—C12 | 117.6 (3) |
O3—La—O4i | 134.26 (7) | C3—C4—C5 | 123.5 (3) |
O2i—La—O6 | 91.19 (7) | C12—C4—C5 | 118.8 (3) |
O3—La—O6 | 87.38 (7) | C6—C5—C4 | 121.5 (3) |
O4i—La—O6 | 128.87 (6) | C5—C6—C7 | 121.2 (3) |
O2i—La—O1 | 126.03 (7) | C11—C7—C8 | 117.1 (3) |
O3—La—O1 | 87.45 (7) | C11—C7—C6 | 119.5 (3) |
O4i—La—O1 | 81.04 (7) | C8—C7—C6 | 123.3 (3) |
O6—La—O1 | 138.47 (7) | C9—C8—C7 | 120.3 (3) |
O2i—La—O5 | 80.24 (7) | C8—C9—C10 | 118.8 (3) |
O3—La—O5 | 129.53 (7) | N2—C10—C9 | 123.4 (3) |
O4i—La—O5 | 77.79 (6) | N2—C11—C7 | 122.4 (3) |
O6—La—O5 | 51.07 (6) | N2—C11—C12 | 118.4 (3) |
O1—La—O5 | 141.97 (7) | C7—C11—C12 | 119.3 (3) |
O2i—La—N1 | 148.16 (7) | N1—C12—C4 | 121.8 (3) |
O3—La—N1 | 138.33 (7) | N1—C12—C11 | 118.5 (3) |
O4i—La—N1 | 79.48 (7) | C4—C12—C11 | 119.6 (3) |
O6—La—N1 | 84.22 (7) | O1—C25—O2 | 121.0 (2) |
O1—La—N1 | 72.91 (7) | O1—C25—C26 | 118.8 (3) |
O5—La—N1 | 72.40 (7) | O2—C25—C26 | 120.2 (3) |
O2i—La—N2 | 148.23 (7) | C31—C26—C27 | 119.5 (3) |
O3—La—N2 | 78.28 (7) | C31—C26—C25 | 121.1 (3) |
O4i—La—N2 | 131.77 (7) | C27—C26—C25 | 119.3 (3) |
O6—La—N2 | 75.01 (7) | C28—C27—C26 | 120.1 (3) |
O1—La—N2 | 63.59 (7) | C29—C28—C27 | 119.8 (3) |
O5—La—N2 | 110.24 (7) | C30—C29—C28 | 120.6 (3) |
N1—La—N2 | 60.11 (7) | C29—C30—C31 | 120.2 (3) |
O2i—La—O2 | 78.60 (6) | C26—C31—C30 | 119.7 (3) |
O3—La—O2 | 73.34 (6) | O3—C32—O4 | 124.9 (2) |
O4i—La—O2 | 66.31 (6) | O3—C32—C33 | 118.2 (2) |
O6—La—O2 | 160.12 (7) | O4—C32—C33 | 116.9 (3) |
O1—La—O2 | 47.49 (6) | C38—C33—C34 | 118.5 (3) |
O5—La—O2 | 141.02 (6) | C38—C33—C32 | 121.2 (3) |
N1—La—O2 | 113.37 (6) | C34—C33—C32 | 120.3 (3) |
N2—La—O2 | 104.95 (6) | C35—C34—C33 | 120.3 (3) |
C25—O1—La | 103.24 (17) | C36—C35—C34 | 120.8 (3) |
C25—O2—Lai | 170.92 (18) | C35—C36—C37 | 119.6 (3) |
C25—O2—La | 87.49 (16) | C36—C37—C38 | 120.6 (3) |
Lai—O2—La | 101.40 (6) | C33—C38—C37 | 120.2 (3) |
C32—O3—La | 136.59 (17) | O5—C39—O6 | 121.6 (2) |
C32—O4—Lai | 139.76 (18) | O5—C39—C40 | 119.5 (3) |
C39—O5—La | 91.70 (16) | O6—C39—C40 | 118.9 (2) |
C39—O6—La | 95.59 (16) | C41—C40—C45 | 119.1 (3) |
C1—N1—C12 | 118.2 (3) | C41—C40—C39 | 120.8 (3) |
C1—N1—La | 120.1 (2) | C45—C40—C39 | 120.1 (3) |
C12—N1—La | 119.95 (18) | C40—C41—C42 | 120.1 (3) |
C10—N2—C11 | 118.1 (3) | C43—C42—C41 | 120.0 (4) |
C10—N2—La | 121.6 (2) | C42—C43—C44 | 120.6 (3) |
C11—N2—La | 118.13 (17) | C43—C44—C45 | 119.6 (4) |
N1—C1—C2 | 123.3 (3) | C44—C45—C40 | 120.6 (3) |
C3—C2—C1 | 118.8 (3) |
Symmetry code: (i) −x, −y, −z. |
Experimental details
Crystal data | |
Chemical formula | [La2(C7H5O2)6(C12H8N2)2] |
Mr | 1364.92 |
Crystal system, space group | Triclinic, P1 |
Temperature (K) | 293 |
a, b, c (Å) | 10.9356 (2), 11.9818 (2), 12.4945 (3) |
α, β, γ (°) | 104.888 (1), 93.268 (1), 113.402 (1) |
V (Å3) | 1428.48 (5) |
Z | 1 |
Radiation type | Mo Kα |
µ (mm−1) | 1.54 |
Crystal size (mm) | 0.31 × 0.21 × 0.20 |
Data collection | |
Diffractometer | Siemens Smart CCD diffractometer |
Absorption correction | Empirical (using intensity measurements) (SADABS; Sheldrick, 1996) |
Tmin, Tmax | 0.546, 0.734 |
No. of measured, independent and observed [I > 2σ(I)] reflections | 7321, 4901, 4427 |
Rint | 0.019 |
(sin θ/λ)max (Å−1) | 0.596 |
Refinement | |
R[F2 > 2σ(F2)], wR(F2), S | 0.024, 0.060, 1.04 |
No. of reflections | 4901 |
No. of parameters | 380 |
H-atom treatment | H-atom parameters constrained |
Δρmax, Δρmin (e Å−3) | 0.61, −0.59 |
Computer programs: SMART (Siemens, 1994), SMART, SHELXS97 (Sheldrick, 1997), SHELXL97 (Sheldrick, 1997), SHELXL97.
La—O2i | 2.4460 (19) | La—O5 | 2.6048 (19) |
La—O3 | 2.4685 (19) | La—N1 | 2.704 (2) |
La—O4i | 2.4756 (18) | La—N2 | 2.756 (2) |
La—O6 | 2.5173 (19) | La—O2 | 2.860 (2) |
La—O1 | 2.542 (2) | ||
O2i—La—O3 | 72.52 (7) | O1—La—N1 | 72.91 (7) |
O2i—La—O4i | 79.10 (7) | O5—La—N1 | 72.40 (7) |
O3—La—O4i | 134.26 (7) | O2i—La—N2 | 148.23 (7) |
O2i—La—O6 | 91.19 (7) | O3—La—N2 | 78.28 (7) |
O3—La—O6 | 87.38 (7) | O4i—La—N2 | 131.77 (7) |
O4i—La—O6 | 128.87 (6) | O6—La—N2 | 75.01 (7) |
O2i—La—O1 | 126.03 (7) | O1—La—N2 | 63.59 (7) |
O3—La—O1 | 87.45 (7) | O5—La—N2 | 110.24 (7) |
O4i—La—O1 | 81.04 (7) | N1—La—N2 | 60.11 (7) |
O6—La—O1 | 138.47 (7) | O2i—La—O2 | 78.60 (6) |
O2i—La—O5 | 80.24 (7) | O3—La—O2 | 73.34 (6) |
O3—La—O5 | 129.53 (7) | O4i—La—O2 | 66.31 (6) |
O4i—La—O5 | 77.79 (6) | O6—La—O2 | 160.12 (7) |
O6—La—O5 | 51.07 (6) | O1—La—O2 | 47.49 (6) |
O1—La—O5 | 141.97 (7) | O5—La—O2 | 141.02 (6) |
O2i—La—N1 | 148.16 (7) | N1—La—O2 | 113.37 (6) |
O3—La—N1 | 138.33 (7) | N2—La—O2 | 104.95 (6) |
O4i—La—N1 | 79.48 (7) | Lai—O2—La | 101.40 (6) |
O6—La—N1 | 84.22 (7) |
Symmetry code: (i) −x, −y, −z. |
Lanthanide complexes play an important role in special materials having optical, electronic, magnetic and biological importance (Deborah et al., 2000; Farrugia et al., 2000). The varied coordination modes of lanthanide elements and carboxylate groups also stimulated our interest in this work.
In the title compound, (I), two La atoms are bridged by four benzoate groups, forming a binuclear cage structure with Ci symmetry. Among them, two benzoate groups also behave as chelating ligands to the La atoms. Another benzoate ion and a 1,10-phenanthroline (phen) molecule chelate with each La atom in the terminal position of the cage. The irregular nine-coordinate environment of the La atom is completed by six O and two N atoms. The La—O bond lengths are in the range of 2.4460 (19) to 2.860 (2) Å (Table 1). The La—N1 and La—N2 bond lengths are 2.704 (2) and 2.756 (2) Å, respectively. The distance between the two La atoms is 4.1143 (3) Å. These values are slightly longer than in the SmIII–benzoate complex Sm2(C12H8N2)2(C6H5CO2)6 (Niu et al., 1999) due to the effect of the Lanthanide contraction.