The crystal structure of the title compound, [NdZn2(C4H5O2)6(NO3)(C10H8N2)2], is made up of discrete molecules of a trinuclear Zn–Nd–Zn complex, with the central Nd atom linked by three bridging bidentate α-methylacrylate groups to each of the two Zn atoms. The title complex is isostructural with its previously reported La and Pr analogues, and the Nd atom has a distorted square-antiprismatic coordination, formed by six O atoms of the bridging methylacrylate groups and two O atoms of a bidentate chelating nitro group. Both of the Zn atoms have a distorted trigonal-bipyramidal coordination, formed by three O atoms of the bridging methylacrylate groups and two N atoms of the chelating 2,2′-bipyridine ligands.
Supporting information
CCDC reference: 216194
Key indicators
- Single-crystal X-ray study
- T = 293 K
- Mean (C-C) = 0.009 Å
- R factor = 0.039
- wR factor = 0.111
- Data-to-parameter ratio = 13.9
checkCIF/PLATON results
No syntax errors found
Alert level A
PLAT241_ALERT_2_A Check High Ueq as Compared to Neighbors for O2
| Author Response: I know from checking CIF that the U(eq) value of O2 atom is
higher compared
with the average U(eq) for to non-hydrogen atoms bonded to it. I have
confirmed that the atom type is right. Large differences may indicate that
thermal motion of the O2 atom is drastic. This case also appear in the
isostructural complexes of La-Zn and Pr-Zn. It's my pleasure if you let me
know how to solve the problem.
|
Alert level B
PLAT242_ALERT_2_B Check Low Ueq as Compared to Neighbors for Nd
PLAT413_ALERT_2_B Short Inter XH3 .. XHn H31C .. H36B .. 1.97 Ang.
Alert level C
PLAT029_ALERT_3_C _diffrn_measured_fraction_theta_full Low ....... 0.98
PLAT062_ALERT_4_C Rescale T(min) & T(max) by ..................... 0.97
PLAT199_ALERT_1_C Check the Reported _cell_measurement_temperature 293 K
PLAT200_ALERT_1_C Check the Reported _diffrn_ambient_temperature . 293 K
PLAT220_ALERT_2_C Large Non-Solvent C Ueq(max)/Ueq(min) ... 3.04 Ratio
PLAT241_ALERT_2_C Check High Ueq as Compared to Neighbors for O4
| Author Response: I know from checking CIF that the U(eq) value of O2 atom is
higher compared
with the average U(eq) for to non-hydrogen atoms bonded to it. I have
confirmed that the atom type is right. Large differences may indicate that
thermal motion of the O2 atom is drastic. This case also appear in the
isostructural complexes of La-Zn and Pr-Zn. It's my pleasure if you let me
know how to solve the problem.
|
PLAT241_ALERT_2_C Check High Ueq as Compared to Neighbors for O5
| Author Response: I know from checking CIF that the U(eq) value of O2 atom is
higher compared
with the average U(eq) for to non-hydrogen atoms bonded to it. I have
confirmed that the atom type is right. Large differences may indicate that
thermal motion of the O2 atom is drastic. This case also appear in the
isostructural complexes of La-Zn and Pr-Zn. It's my pleasure if you let me
know how to solve the problem.
|
PLAT241_ALERT_2_C Check High Ueq as Compared to Neighbors for O6
| Author Response: I know from checking CIF that the U(eq) value of O2 atom is
higher compared
with the average U(eq) for to non-hydrogen atoms bonded to it. I have
confirmed that the atom type is right. Large differences may indicate that
thermal motion of the O2 atom is drastic. This case also appear in the
isostructural complexes of La-Zn and Pr-Zn. It's my pleasure if you let me
know how to solve the problem.
|
PLAT241_ALERT_2_C Check High Ueq as Compared to Neighbors for O10
| Author Response: I know from checking CIF that the U(eq) value of O2 atom is
higher compared
with the average U(eq) for to non-hydrogen atoms bonded to it. I have
confirmed that the atom type is right. Large differences may indicate that
thermal motion of the O2 atom is drastic. This case also appear in the
isostructural complexes of La-Zn and Pr-Zn. It's my pleasure if you let me
know how to solve the problem.
|
PLAT241_ALERT_2_C Check High Ueq as Compared to Neighbors for O11
| Author Response: I know from checking CIF that the U(eq) value of O2 atom is
higher compared
with the average U(eq) for to non-hydrogen atoms bonded to it. I have
confirmed that the atom type is right. Large differences may indicate that
thermal motion of the O2 atom is drastic. This case also appear in the
isostructural complexes of La-Zn and Pr-Zn. It's my pleasure if you let me
know how to solve the problem.
|
PLAT241_ALERT_2_C Check High Ueq as Compared to Neighbors for O12
| Author Response: I know from checking CIF that the U(eq) value of O2 atom is
higher compared
with the average U(eq) for to non-hydrogen atoms bonded to it. I have
confirmed that the atom type is right. Large differences may indicate that
thermal motion of the O2 atom is drastic. This case also appear in the
isostructural complexes of La-Zn and Pr-Zn. It's my pleasure if you let me
know how to solve the problem.
|
PLAT241_ALERT_2_C Check High Ueq as Compared to Neighbors for O14
| Author Response: I know from checking CIF that the U(eq) value of O2 atom is
higher compared
with the average U(eq) for to non-hydrogen atoms bonded to it. I have
confirmed that the atom type is right. Large differences may indicate that
thermal motion of the O2 atom is drastic. This case also appear in the
isostructural complexes of La-Zn and Pr-Zn. It's my pleasure if you let me
know how to solve the problem.
|
PLAT241_ALERT_2_C Check High Ueq as Compared to Neighbors for O15
| Author Response: I know from checking CIF that the U(eq) value of O2 atom is
higher compared
with the average U(eq) for to non-hydrogen atoms bonded to it. I have
confirmed that the atom type is right. Large differences may indicate that
thermal motion of the O2 atom is drastic. This case also appear in the
isostructural complexes of La-Zn and Pr-Zn. It's my pleasure if you let me
know how to solve the problem.
|
PLAT242_ALERT_2_C Check Low Ueq as Compared to Neighbors for C21
PLAT242_ALERT_2_C Check Low Ueq as Compared to Neighbors for C22
PLAT242_ALERT_2_C Check Low Ueq as Compared to Neighbors for C26
PLAT242_ALERT_2_C Check Low Ueq as Compared to Neighbors for C30
PLAT242_ALERT_2_C Check Low Ueq as Compared to Neighbors for C34
PLAT242_ALERT_2_C Check Low Ueq as Compared to Neighbors for C38
PLAT242_ALERT_2_C Check Low Ueq as Compared to Neighbors for C42
PLAT342_ALERT_3_C Low Bond Precision on C-C bonds (x 1000) Ang ... 9
PLAT380_ALERT_4_C Check Incorrectly? Oriented X(sp2)-Methyl Moiety C23
PLAT380_ALERT_4_C Check Incorrectly? Oriented X(sp2)-Methyl Moiety C31
PLAT380_ALERT_4_C Check Incorrectly? Oriented X(sp2)-Methyl Moiety C44
1 ALERT level A = In general: serious problem
2 ALERT level B = Potentially serious problem
24 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
19 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
4 ALERT type 4 Improvement, methodology, query or suggestion
Data collection: PROCESS-AUTO (Rigaku, 1998); cell refinement: PROCESS-AUTO; data reduction: CrystalStructure (Rigaku/MSC, 2002); program(s) used to solve structure: SIR92 (Altomare et al., 1993); program(s) used to refine structure: SHELXL97 (Sheldrick, 1997); molecular graphics: ORTEP-3 for Windows (Farrugia, 1997); software used to prepare material for publication: WinGX (Farrugia, 1999).
Bis(2,2'-bipyridine)-1k
2N:
N';3k
2N:
N'-hexakis(µ-
α-methylacrylato)-
1:2k
6O:
O';2:3k
6O:
O'-nitrato-2k
2O:
O'-dizinc(II)neodymium(III)
top
Crystal data top
[NdZn2(C4H5O2)6(NO3)(C10H8N2)2] | Z = 2 |
Mr = 1159.84 | F(000) = 1170 |
Triclinic, P1 | Dx = 1.605 Mg m−3 |
Hall symbol: -P 1 | Mo Kα radiation, λ = 0.71069 Å |
a = 11.3751 (9) Å | Cell parameters from 8348 reflections |
b = 13.7258 (8) Å | θ = 2.5–27.5° |
c = 16.4798 (11) Å | µ = 2.13 mm−1 |
α = 103.903 (4)° | T = 293 K |
β = 99.490 (4)° | Chunk, pink |
γ = 100.168 (5)° | 0.30 × 0.30 × 0.20 mm |
V = 2399.9 (3) Å3 | |
Data collection top
Rigaku R-AXIS RAPID diffractometer | 8421 independent reflections |
Radiation source: fine-focus sealed tube | 7077 reflections with I > 2σ(I) |
Graphite monochromator | Rint = 0.031 |
Detector resolution: 10.00 pixels mm-1 | θmax = 25.1°, θmin = 1.3° |
ω scans | h = −13→13 |
Absorption correction: multi-scan (ABSCOR; Higashi, 1995) | k = −16→16 |
Tmin = 0.568, Tmax = 0.675 | l = −19→19 |
18091 measured reflections | |
Refinement top
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)] = 0.039 | H-atom parameters constrained |
wR(F2) = 0.111 | w = 1/[σ2(Fo2) + (0.0658P)2 + 3.3948P] where P = (Fo2 + 2Fc2)/3 |
S = 1.01 | (Δ/σ)max = 0.002 |
8421 reflections | Δρmax = 0.67 e Å−3 |
605 parameters | Δρmin = −0.77 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: 0.0053 (4) |
Special details top
Experimental. The elemental analyses on C, H and N were performed using a Carlo-Erba 1110
Elemental Analyzer; Nd and Zn were determined by titration with edta. Calcd.
for C44H46O15N5NdZn2, %: C 45.56; H 3.97; N 6.04; Nd 12.44; Zn 11.28. Found,
%: C 45.55; H 4.01; N 6.14; Nd 12.26; Zn 11.35. Infrared spectra were recorded
with a Nicolet 560 spectrophotometer (4000?400 cm?1) using a powdered sample
spread on a KBr plate. IR spectra: ?as (COO) 1574, ?s (COO) 1408, ? (C=C)
1659, ? (C?H) 2970 cm?1. |
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 | x | y | z | Uiso*/Ueq | |
Nd | 0.64580 (2) | 0.76273 (2) | 0.257174 (16) | 0.03877 (11) | |
Zn1 | 0.71145 (5) | 0.90467 (4) | 0.08070 (3) | 0.04022 (15) | |
Zn2 | 0.71461 (5) | 0.57395 (5) | 0.40035 (4) | 0.04550 (16) | |
O1 | 0.7974 (3) | 0.7877 (3) | 0.0361 (3) | 0.0577 (9) | |
O2 | 0.7851 (4) | 0.7598 (5) | 0.1594 (3) | 0.0965 (17) | |
O3 | 0.5418 (3) | 0.8247 (3) | 0.0198 (2) | 0.0497 (8) | |
O4 | 0.5253 (3) | 0.7415 (3) | 0.1180 (2) | 0.0635 (11) | |
O5 | 0.6568 (3) | 1.0052 (3) | 0.1702 (3) | 0.0634 (10) | |
O6 | 0.7194 (4) | 0.9423 (3) | 0.2780 (3) | 0.0749 (12) | |
O7 | 0.4688 (4) | 0.8529 (3) | 0.2777 (3) | 0.0667 (11) | |
O8 | 0.4227 (3) | 0.6895 (3) | 0.2615 (3) | 0.0641 (11) | |
O9 | 0.2826 (4) | 0.7771 (5) | 0.2732 (4) | 0.105 (2) | |
O10 | 0.6367 (4) | 0.7876 (4) | 0.4046 (2) | 0.0691 (11) | |
O11 | 0.6194 (4) | 0.6611 (3) | 0.4671 (3) | 0.0632 (10) | |
O12 | 0.8449 (3) | 0.7616 (4) | 0.3335 (3) | 0.0696 (11) | |
O13 | 0.8640 (3) | 0.6927 (3) | 0.4423 (3) | 0.0605 (10) | |
O14 | 0.6278 (4) | 0.5829 (3) | 0.2393 (3) | 0.0709 (12) | |
O15 | 0.5678 (4) | 0.4760 (3) | 0.3120 (3) | 0.0651 (10) | |
N1 | 0.7336 (4) | 0.9912 (3) | −0.0069 (3) | 0.0435 (9) | |
N2 | 0.8953 (3) | 1.0039 (3) | 0.1327 (3) | 0.0450 (9) | |
N3 | 0.8368 (4) | 0.4789 (3) | 0.3547 (3) | 0.0512 (10) | |
N4 | 0.7356 (4) | 0.4870 (3) | 0.4888 (3) | 0.0468 (10) | |
N5 | 0.3888 (4) | 0.7736 (5) | 0.2708 (3) | 0.0674 (14) | |
C1 | 0.6460 (5) | 0.9830 (4) | −0.0752 (3) | 0.0512 (12) | |
H1 | 0.5707 | 0.9379 | −0.0839 | 0.061* | |
C2 | 0.6643 (6) | 1.0393 (5) | −0.1326 (4) | 0.0627 (15) | |
H2 | 0.6018 | 1.0335 | −0.1789 | 0.075* | |
C3 | 0.7758 (6) | 1.1037 (5) | −0.1205 (4) | 0.0625 (15) | |
H3 | 0.7905 | 1.1417 | −0.1590 | 0.075* | |
C4 | 0.8663 (5) | 1.1120 (4) | −0.0508 (4) | 0.0545 (13) | |
H4 | 0.9430 | 1.1548 | −0.0423 | 0.065* | |
C5 | 0.8422 (4) | 1.0561 (3) | 0.0062 (3) | 0.0418 (11) | |
C6 | 0.9325 (4) | 1.0643 (4) | 0.0854 (3) | 0.0411 (10) | |
C7 | 1.0478 (5) | 1.1297 (4) | 0.1101 (4) | 0.0529 (13) | |
H7 | 1.0735 | 1.1704 | 0.0758 | 0.064* | |
C8 | 1.1230 (5) | 1.1339 (5) | 0.1847 (4) | 0.0627 (15) | |
H8 | 1.2004 | 1.1777 | 0.2017 | 0.075* | |
C9 | 1.0850 (5) | 1.0737 (5) | 0.2346 (4) | 0.0618 (15) | |
H9 | 1.1349 | 1.0765 | 0.2862 | 0.074* | |
C10 | 0.9701 (5) | 1.0084 (5) | 0.2062 (4) | 0.0567 (14) | |
H10 | 0.9438 | 0.9662 | 0.2392 | 0.068* | |
C11 | 0.8848 (6) | 0.4781 (5) | 0.2861 (4) | 0.0681 (16) | |
H11 | 0.8575 | 0.5157 | 0.2498 | 0.082* | |
C12 | 0.9722 (7) | 0.4248 (6) | 0.2660 (5) | 0.086 (2) | |
H12 | 1.0025 | 0.4253 | 0.2169 | 0.103* | |
C13 | 1.0134 (6) | 0.3711 (6) | 0.3204 (5) | 0.085 (2) | |
H13 | 1.0734 | 0.3349 | 0.3092 | 0.102* | |
C14 | 0.9660 (6) | 0.3711 (5) | 0.3915 (4) | 0.0672 (16) | |
H14 | 0.9938 | 0.3352 | 0.4292 | 0.081* | |
C15 | 0.8765 (5) | 0.4248 (4) | 0.4067 (4) | 0.0512 (12) | |
C16 | 0.8155 (4) | 0.4264 (4) | 0.4801 (3) | 0.0484 (12) | |
C17 | 0.8363 (6) | 0.3680 (5) | 0.5366 (4) | 0.0687 (17) | |
H17 | 0.8933 | 0.3271 | 0.5313 | 0.082* | |
C18 | 0.7721 (7) | 0.3708 (6) | 0.6007 (5) | 0.080 (2) | |
H18 | 0.7854 | 0.3320 | 0.6391 | 0.096* | |
C19 | 0.6889 (6) | 0.4309 (5) | 0.6073 (4) | 0.0703 (17) | |
H19 | 0.6431 | 0.4327 | 0.6493 | 0.084* | |
C20 | 0.6741 (5) | 0.4885 (5) | 0.5511 (4) | 0.0611 (15) | |
H20 | 0.6187 | 0.5307 | 0.5565 | 0.073* | |
C21 | 0.8199 (4) | 0.7417 (4) | 0.0910 (3) | 0.0499 (12) | |
C22 | 0.8990 (5) | 0.6648 (5) | 0.0743 (4) | 0.0631 (15) | |
C23 | 0.9061 (7) | 0.6213 (5) | −0.0122 (5) | 0.0782 (19) | |
H23A | 0.8504 | 0.6442 | −0.0500 | 0.117* | |
H23B | 0.8846 | 0.5475 | −0.0257 | 0.117* | |
H23C | 0.9879 | 0.6431 | −0.0190 | 0.117* | |
C24 | 0.9670 (9) | 0.6462 (8) | 0.1437 (7) | 0.125 (4) | |
H24A | 1.0213 | 0.6033 | 0.1357 | 0.150* | |
H24B | 0.9587 | 0.6767 | 0.1987 | 0.150* | |
C25 | 0.4835 (4) | 0.7611 (4) | 0.0509 (3) | 0.0424 (11) | |
C26 | 0.3560 (5) | 0.7078 (4) | 0.0030 (4) | 0.0524 (13) | |
C27 | 0.3112 (6) | 0.7308 (6) | −0.0768 (4) | 0.0766 (19) | |
H27A | 0.3745 | 0.7788 | −0.0881 | 0.115* | |
H27B | 0.2413 | 0.7603 | −0.0721 | 0.115* | |
H27C | 0.2883 | 0.6684 | −0.1229 | 0.115* | |
C28 | 0.2882 (6) | 0.6421 (6) | 0.0356 (5) | 0.088 (2) | |
H28A | 0.2084 | 0.6088 | 0.0068 | 0.106* | |
H28B | 0.3212 | 0.6302 | 0.0868 | 0.106* | |
C29 | 0.6821 (4) | 1.0102 (4) | 0.2487 (4) | 0.0521 (13) | |
C30 | 0.6698 (5) | 1.1059 (4) | 0.3091 (4) | 0.0541 (13) | |
C31 | 0.6561 (7) | 1.1942 (5) | 0.2746 (5) | 0.083 (2) | |
H31A | 0.6588 | 1.1764 | 0.2151 | 0.125* | |
H31B | 0.7214 | 1.2526 | 0.3055 | 0.125* | |
H31C | 0.5791 | 1.2111 | 0.2810 | 0.125* | |
C32 | 0.6696 (6) | 1.1093 (7) | 0.3907 (4) | 0.085 (2) | |
H32A | 0.6605 | 1.1687 | 0.4282 | 0.102* | |
H32B | 0.6785 | 1.0522 | 0.4102 | 0.102* | |
C33 | 0.6232 (4) | 0.7524 (5) | 0.4668 (3) | 0.0496 (12) | |
C34 | 0.6119 (5) | 0.8255 (5) | 0.5471 (4) | 0.0576 (14) | |
C35 | 0.6077 (8) | 0.9233 (6) | 0.5502 (6) | 0.104 (3) | |
H35A | 0.6008 | 0.9679 | 0.6006 | 0.125* | |
H35B | 0.6118 | 0.9465 | 0.5019 | 0.125* | |
C36 | 0.6059 (7) | 0.7831 (7) | 0.6208 (4) | 0.092 (2) | |
H36A | 0.6111 | 0.7123 | 0.6050 | 0.137* | |
H36B | 0.5299 | 0.7878 | 0.6379 | 0.137* | |
H36C | 0.6727 | 0.8217 | 0.6676 | 0.137* | |
C37 | 0.8960 (4) | 0.7606 (4) | 0.4064 (3) | 0.0480 (12) | |
C38 | 1.0030 (5) | 0.8466 (4) | 0.4537 (4) | 0.0572 (14) | |
C39 | 1.0829 (7) | 0.8906 (6) | 0.4036 (6) | 0.094 (2) | |
H39A | 1.0542 | 0.8539 | 0.3440 | 0.140* | |
H39B | 1.1651 | 0.8847 | 0.4227 | 0.140* | |
H39C | 1.0814 | 0.9619 | 0.4113 | 0.140* | |
C40 | 1.0197 (7) | 0.8806 (5) | 0.5397 (5) | 0.084 (2) | |
H40A | 0.9652 | 0.8505 | 0.5677 | 0.100* | |
H40B | 1.0858 | 0.9342 | 0.5709 | 0.100* | |
C41 | 0.5595 (5) | 0.5031 (4) | 0.2445 (4) | 0.0511 (12) | |
C42 | 0.4676 (5) | 0.4342 (4) | 0.1674 (3) | 0.0510 (12) | |
C43 | 0.4632 (7) | 0.4547 (5) | 0.0923 (4) | 0.0756 (18) | |
H43A | 0.4084 | 0.4105 | 0.0438 | 0.091* | |
H43B | 0.5148 | 0.5131 | 0.0883 | 0.091* | |
C44 | 0.3894 (7) | 0.3440 (6) | 0.1789 (5) | 0.090 (2) | |
H44A | 0.4074 | 0.3443 | 0.2380 | 0.135* | |
H44B | 0.4045 | 0.2825 | 0.1441 | 0.135* | |
H44C | 0.3051 | 0.3459 | 0.1621 | 0.135* | |
Atomic displacement parameters (Å2) top | U11 | U22 | U33 | U12 | U13 | U23 |
Nd | 0.04006 (15) | 0.04404 (17) | 0.03887 (16) | 0.01091 (11) | 0.00957 (10) | 0.02226 (11) |
Zn1 | 0.0384 (3) | 0.0422 (3) | 0.0419 (3) | 0.0051 (2) | 0.0090 (2) | 0.0180 (2) |
Zn2 | 0.0459 (3) | 0.0501 (3) | 0.0435 (3) | 0.0123 (3) | 0.0036 (2) | 0.0216 (3) |
O1 | 0.062 (2) | 0.050 (2) | 0.065 (2) | 0.0165 (18) | 0.0152 (19) | 0.0196 (19) |
O2 | 0.061 (3) | 0.171 (5) | 0.057 (3) | 0.027 (3) | 0.028 (2) | 0.020 (3) |
O3 | 0.0448 (18) | 0.055 (2) | 0.047 (2) | 0.0014 (16) | 0.0054 (15) | 0.0212 (17) |
O4 | 0.058 (2) | 0.084 (3) | 0.047 (2) | 0.001 (2) | 0.0019 (17) | 0.031 (2) |
O5 | 0.054 (2) | 0.074 (3) | 0.055 (3) | 0.0147 (19) | 0.0124 (18) | 0.004 (2) |
O6 | 0.062 (2) | 0.054 (2) | 0.117 (4) | 0.012 (2) | 0.024 (2) | 0.037 (3) |
O7 | 0.065 (2) | 0.076 (3) | 0.082 (3) | 0.030 (2) | 0.026 (2) | 0.047 (2) |
O8 | 0.054 (2) | 0.078 (3) | 0.079 (3) | 0.018 (2) | 0.023 (2) | 0.049 (2) |
O9 | 0.060 (3) | 0.178 (6) | 0.138 (5) | 0.060 (3) | 0.053 (3) | 0.114 (5) |
O10 | 0.081 (3) | 0.099 (3) | 0.050 (2) | 0.045 (2) | 0.025 (2) | 0.038 (2) |
O11 | 0.070 (2) | 0.060 (2) | 0.070 (3) | 0.022 (2) | 0.028 (2) | 0.022 (2) |
O12 | 0.050 (2) | 0.104 (3) | 0.058 (3) | 0.022 (2) | 0.0047 (18) | 0.030 (2) |
O13 | 0.051 (2) | 0.052 (2) | 0.079 (3) | 0.0107 (17) | −0.0007 (19) | 0.029 (2) |
O14 | 0.058 (2) | 0.042 (2) | 0.107 (4) | 0.0097 (18) | 0.015 (2) | 0.014 (2) |
O15 | 0.065 (2) | 0.070 (3) | 0.052 (2) | 0.015 (2) | −0.0086 (18) | 0.015 (2) |
N1 | 0.043 (2) | 0.044 (2) | 0.049 (2) | 0.0123 (18) | 0.0113 (18) | 0.0195 (19) |
N2 | 0.038 (2) | 0.049 (2) | 0.047 (2) | 0.0036 (18) | 0.0094 (18) | 0.0168 (19) |
N3 | 0.048 (2) | 0.054 (3) | 0.050 (3) | 0.011 (2) | 0.0064 (19) | 0.014 (2) |
N4 | 0.046 (2) | 0.050 (2) | 0.046 (2) | 0.0081 (19) | 0.0046 (18) | 0.022 (2) |
N5 | 0.053 (3) | 0.109 (4) | 0.073 (3) | 0.035 (3) | 0.029 (2) | 0.064 (3) |
C1 | 0.047 (3) | 0.056 (3) | 0.055 (3) | 0.014 (2) | 0.008 (2) | 0.025 (3) |
C2 | 0.065 (3) | 0.073 (4) | 0.066 (4) | 0.028 (3) | 0.012 (3) | 0.040 (3) |
C3 | 0.079 (4) | 0.064 (4) | 0.063 (4) | 0.024 (3) | 0.024 (3) | 0.040 (3) |
C4 | 0.062 (3) | 0.050 (3) | 0.060 (3) | 0.012 (3) | 0.023 (3) | 0.024 (3) |
C5 | 0.044 (2) | 0.035 (2) | 0.050 (3) | 0.009 (2) | 0.015 (2) | 0.015 (2) |
C6 | 0.042 (2) | 0.038 (2) | 0.044 (3) | 0.007 (2) | 0.014 (2) | 0.011 (2) |
C7 | 0.048 (3) | 0.047 (3) | 0.064 (3) | 0.003 (2) | 0.017 (3) | 0.018 (3) |
C8 | 0.048 (3) | 0.062 (4) | 0.065 (4) | −0.007 (3) | 0.009 (3) | 0.011 (3) |
C9 | 0.047 (3) | 0.071 (4) | 0.055 (3) | 0.000 (3) | 0.001 (2) | 0.011 (3) |
C10 | 0.046 (3) | 0.072 (4) | 0.052 (3) | 0.003 (3) | 0.008 (2) | 0.026 (3) |
C11 | 0.069 (4) | 0.086 (5) | 0.057 (4) | 0.026 (3) | 0.020 (3) | 0.024 (3) |
C12 | 0.086 (5) | 0.105 (6) | 0.062 (4) | 0.024 (4) | 0.028 (4) | 0.004 (4) |
C13 | 0.070 (4) | 0.083 (5) | 0.092 (6) | 0.032 (4) | 0.012 (4) | −0.001 (4) |
C14 | 0.065 (4) | 0.062 (4) | 0.074 (4) | 0.026 (3) | 0.007 (3) | 0.013 (3) |
C15 | 0.047 (3) | 0.041 (3) | 0.058 (3) | 0.007 (2) | −0.002 (2) | 0.012 (2) |
C16 | 0.045 (3) | 0.040 (3) | 0.056 (3) | 0.005 (2) | −0.002 (2) | 0.019 (2) |
C17 | 0.073 (4) | 0.054 (3) | 0.083 (5) | 0.019 (3) | 0.000 (3) | 0.034 (3) |
C18 | 0.091 (5) | 0.081 (5) | 0.080 (5) | 0.008 (4) | 0.009 (4) | 0.055 (4) |
C19 | 0.070 (4) | 0.085 (5) | 0.066 (4) | 0.009 (3) | 0.020 (3) | 0.044 (4) |
C20 | 0.053 (3) | 0.071 (4) | 0.065 (4) | 0.009 (3) | 0.011 (3) | 0.035 (3) |
C21 | 0.039 (2) | 0.057 (3) | 0.050 (3) | 0.005 (2) | 0.013 (2) | 0.011 (3) |
C22 | 0.064 (3) | 0.056 (3) | 0.088 (5) | 0.019 (3) | 0.031 (3) | 0.040 (3) |
C23 | 0.088 (5) | 0.058 (4) | 0.099 (5) | 0.025 (3) | 0.042 (4) | 0.022 (4) |
C24 | 0.154 (9) | 0.151 (9) | 0.116 (8) | 0.093 (8) | 0.035 (7) | 0.078 (7) |
C25 | 0.039 (2) | 0.049 (3) | 0.039 (3) | 0.009 (2) | 0.007 (2) | 0.015 (2) |
C26 | 0.044 (3) | 0.051 (3) | 0.055 (3) | 0.004 (2) | 0.005 (2) | 0.009 (2) |
C27 | 0.053 (3) | 0.101 (5) | 0.062 (4) | 0.007 (3) | −0.013 (3) | 0.023 (4) |
C28 | 0.054 (4) | 0.086 (5) | 0.120 (6) | −0.012 (3) | 0.006 (4) | 0.048 (5) |
C29 | 0.036 (2) | 0.054 (3) | 0.064 (4) | 0.001 (2) | 0.016 (2) | 0.016 (3) |
C30 | 0.048 (3) | 0.055 (3) | 0.054 (3) | 0.007 (2) | 0.004 (2) | 0.014 (3) |
C31 | 0.095 (5) | 0.056 (4) | 0.088 (5) | 0.011 (4) | 0.010 (4) | 0.012 (4) |
C32 | 0.085 (5) | 0.110 (6) | 0.061 (4) | 0.032 (4) | 0.015 (4) | 0.019 (4) |
C33 | 0.043 (3) | 0.071 (4) | 0.040 (3) | 0.020 (2) | 0.010 (2) | 0.020 (3) |
C34 | 0.056 (3) | 0.070 (4) | 0.050 (3) | 0.016 (3) | 0.016 (2) | 0.019 (3) |
C35 | 0.129 (7) | 0.076 (5) | 0.120 (7) | 0.031 (5) | 0.069 (6) | 0.020 (5) |
C36 | 0.105 (6) | 0.127 (7) | 0.046 (4) | 0.030 (5) | 0.023 (4) | 0.023 (4) |
C37 | 0.038 (2) | 0.053 (3) | 0.055 (3) | 0.019 (2) | 0.006 (2) | 0.016 (3) |
C38 | 0.049 (3) | 0.047 (3) | 0.075 (4) | 0.013 (2) | 0.004 (3) | 0.020 (3) |
C39 | 0.078 (5) | 0.084 (5) | 0.122 (7) | 0.008 (4) | 0.019 (4) | 0.044 (5) |
C40 | 0.086 (5) | 0.058 (4) | 0.084 (5) | 0.009 (3) | −0.018 (4) | 0.007 (3) |
C41 | 0.047 (3) | 0.045 (3) | 0.060 (3) | 0.017 (2) | 0.005 (2) | 0.014 (3) |
C42 | 0.054 (3) | 0.050 (3) | 0.047 (3) | 0.013 (2) | 0.003 (2) | 0.014 (2) |
C43 | 0.095 (5) | 0.076 (4) | 0.057 (4) | 0.020 (4) | 0.010 (3) | 0.023 (3) |
C44 | 0.094 (5) | 0.081 (5) | 0.073 (5) | −0.023 (4) | −0.003 (4) | 0.023 (4) |
Geometric parameters (Å, º) top
Nd—O2 | 2.438 (4) | C13—C14 | 1.369 (10) |
Nd—O4 | 2.393 (4) | C13—H13 | 0.9300 |
Nd—O6 | 2.380 (4) | C14—C15 | 1.379 (8) |
Nd—O7 | 2.570 (4) | C14—H14 | 0.9300 |
Nd—O8 | 2.579 (4) | C15—C16 | 1.488 (8) |
Nd—O10 | 2.393 (4) | C16—C17 | 1.385 (7) |
Nd—O12 | 2.407 (4) | C17—C18 | 1.377 (10) |
Nd—O14 | 2.382 (4) | C17—H17 | 0.9300 |
Zn1—O1 | 2.073 (4) | C18—C19 | 1.363 (10) |
Zn1—O3 | 2.005 (3) | C18—H18 | 0.9300 |
Zn1—O5 | 2.024 (4) | C19—C20 | 1.363 (8) |
Zn1—N1 | 2.097 (4) | C19—H19 | 0.9300 |
Zn1—N2 | 2.192 (4) | C20—H20 | 0.9300 |
Zn2—O11 | 2.008 (4) | C21—C22 | 1.509 (8) |
Zn2—O13 | 2.029 (4) | C22—C24 | 1.375 (10) |
Zn2—O15 | 2.045 (4) | C22—C23 | 1.428 (9) |
Zn2—N3 | 2.171 (5) | C23—H23A | 0.9600 |
Zn2—N4 | 2.104 (4) | C23—H23B | 0.9600 |
O1—C21 | 1.241 (6) | C23—H23C | 0.9600 |
O2—C21 | 1.238 (7) | C24—H24A | 0.9300 |
O3—C25 | 1.259 (5) | C24—H24B | 0.9300 |
O4—C25 | 1.240 (6) | C25—C26 | 1.494 (7) |
O5—C29 | 1.260 (7) | C26—C28 | 1.349 (8) |
O6—C29 | 1.254 (7) | C26—C27 | 1.458 (8) |
O7—N5 | 1.258 (6) | C27—H27A | 0.9600 |
O8—N5 | 1.263 (7) | C27—H27B | 0.9600 |
O9—N5 | 1.225 (6) | C27—H27C | 0.9600 |
O10—C33 | 1.254 (6) | C28—H28A | 0.9300 |
O11—C33 | 1.249 (7) | C28—H28B | 0.9300 |
O12—C37 | 1.250 (6) | C29—C30 | 1.490 (8) |
O13—C37 | 1.251 (6) | C30—C32 | 1.336 (9) |
O14—C41 | 1.256 (6) | C30—C31 | 1.478 (9) |
O15—C41 | 1.249 (7) | C31—H31A | 0.9600 |
N1—C5 | 1.341 (6) | C31—H31B | 0.9600 |
N1—C1 | 1.342 (6) | C31—H31C | 0.9600 |
N2—C6 | 1.330 (6) | C32—H32A | 0.9300 |
N2—C10 | 1.342 (7) | C32—H32B | 0.9300 |
N3—C15 | 1.337 (7) | C33—C34 | 1.497 (8) |
N3—C11 | 1.333 (7) | C34—C35 | 1.340 (10) |
N4—C16 | 1.339 (7) | C34—C36 | 1.473 (8) |
N4—C20 | 1.332 (7) | C35—H35A | 0.9300 |
C1—C2 | 1.377 (7) | C35—H35B | 0.9300 |
C1—H1 | 0.9300 | C36—H36A | 0.9600 |
C2—C3 | 1.366 (8) | C36—H36B | 0.9600 |
C2—H2 | 0.9300 | C36—H36C | 0.9600 |
C3—C4 | 1.378 (8) | C37—C38 | 1.491 (7) |
C3—H3 | 0.9300 | C38—C40 | 1.350 (9) |
C4—C5 | 1.379 (7) | C38—C39 | 1.472 (9) |
C4—H4 | 0.9300 | C39—H39A | 0.9600 |
C5—C6 | 1.489 (7) | C39—H39B | 0.9600 |
C6—C7 | 1.387 (7) | C39—H39C | 0.9600 |
C7—C8 | 1.359 (8) | C40—H40A | 0.9300 |
C7—H7 | 0.9300 | C40—H40B | 0.9300 |
C8—C9 | 1.366 (8) | C41—C42 | 1.495 (7) |
C8—H8 | 0.9300 | C42—C43 | 1.328 (8) |
C9—C10 | 1.383 (7) | C42—C44 | 1.463 (8) |
C9—H9 | 0.9300 | C43—H43A | 0.9300 |
C10—H10 | 0.9300 | C43—H43B | 0.9300 |
C11—C12 | 1.372 (10) | C44—H44A | 0.9600 |
C11—H11 | 0.9300 | C44—H44B | 0.9600 |
C12—C13 | 1.367 (11) | C44—H44C | 0.9600 |
C12—H12 | 0.9300 | | |
| | | |
O2—Nd—O4 | 72.96 (15) | C14—C13—H13 | 120.2 |
O2—Nd—O6 | 79.27 (19) | C12—C13—H13 | 120.2 |
O2—Nd—O7 | 133.17 (17) | C13—C14—C15 | 119.3 (6) |
O2—Nd—O8 | 141.40 (16) | C13—C14—H14 | 120.3 |
O2—Nd—O10 | 143.61 (15) | C15—C14—H14 | 120.3 |
O2—Nd—O12 | 71.50 (16) | N3—C15—C14 | 121.6 (6) |
O2—Nd—O14 | 89.97 (19) | N3—C15—C16 | 114.8 (5) |
O4—Nd—O6 | 92.39 (15) | C14—C15—C16 | 123.6 (5) |
O4—Nd—O7 | 72.58 (15) | N4—C16—C17 | 120.4 (5) |
O4—Nd—O8 | 73.61 (13) | N4—C16—C15 | 116.3 (4) |
O4—Nd—O10 | 143.20 (14) | C17—C16—C15 | 123.3 (5) |
O4—Nd—O12 | 143.86 (14) | C16—C17—C18 | 119.5 (6) |
O4—Nd—O14 | 94.60 (15) | C16—C17—H17 | 120.2 |
O6—Nd—O7 | 71.52 (14) | C18—C17—H17 | 120.2 |
O6—Nd—O8 | 120.90 (14) | C19—C18—C17 | 119.3 (6) |
O6—Nd—O10 | 92.15 (17) | C19—C18—H18 | 120.3 |
O6—Nd—O12 | 87.37 (16) | C17—C18—H18 | 120.3 |
O6—Nd—O14 | 164.87 (14) | C18—C19—C20 | 118.5 (6) |
O7—Nd—O8 | 49.40 (14) | C18—C19—H19 | 120.7 |
O7—Nd—O10 | 74.37 (13) | C20—C19—H19 | 120.7 |
O7—Nd—O12 | 139.97 (15) | N4—C20—C19 | 123.0 (6) |
O7—Nd—O14 | 123.43 (14) | N4—C20—H20 | 118.5 |
O8—Nd—O10 | 72.79 (14) | C19—C20—H20 | 118.5 |
O8—Nd—O12 | 135.72 (13) | O1—C21—O2 | 122.9 (6) |
O8—Nd—O14 | 74.04 (14) | O1—C21—C22 | 117.3 (5) |
O10—Nd—O12 | 72.84 (14) | O2—C21—C22 | 119.7 (6) |
O10—Nd—O14 | 90.28 (16) | C24—C22—C23 | 123.7 (7) |
O12—Nd—O14 | 79.08 (15) | C24—C22—C21 | 117.9 (7) |
O1—Zn1—O3 | 95.52 (15) | C23—C22—C21 | 118.2 (6) |
O1—Zn1—O5 | 155.69 (17) | C22—C23—H23A | 109.5 |
O1—Zn1—N1 | 100.83 (15) | C22—C23—H23B | 109.5 |
O1—Zn1—N2 | 86.54 (16) | H23A—C23—H23B | 109.5 |
O3—Zn1—O5 | 95.04 (15) | C22—C23—H23C | 109.5 |
O3—Zn1—N1 | 95.45 (14) | H23A—C23—H23C | 109.5 |
O3—Zn1—N2 | 171.61 (14) | H23B—C23—H23C | 109.5 |
O5—Zn1—N1 | 99.89 (17) | C22—C24—H24A | 120.0 |
O5—Zn1—N2 | 86.19 (16) | C22—C24—H24B | 120.0 |
N1—Zn1—N2 | 76.16 (15) | H24A—C24—H24B | 120.0 |
O11—Zn2—O13 | 89.89 (17) | O4—C25—O3 | 124.0 (4) |
O11—Zn2—O15 | 96.83 (18) | O4—C25—C26 | 119.1 (4) |
O11—Zn2—N3 | 167.84 (17) | O3—C25—C26 | 116.8 (4) |
O11—Zn2—N4 | 93.33 (17) | C28—C26—C27 | 123.4 (5) |
O13—Zn2—O15 | 155.01 (17) | C28—C26—C25 | 119.0 (5) |
O13—Zn2—N3 | 86.48 (16) | C27—C26—C25 | 117.6 (5) |
O13—Zn2—N4 | 104.27 (15) | C26—C27—H27A | 109.5 |
O15—Zn2—N3 | 91.29 (17) | C26—C27—H27B | 109.5 |
O15—Zn2—N4 | 99.36 (16) | H27A—C27—H27B | 109.5 |
N3—Zn2—N4 | 76.38 (17) | C26—C27—H27C | 109.5 |
C21—O1—Zn1 | 110.6 (3) | H27A—C27—H27C | 109.5 |
C21—O2—Nd | 158.9 (4) | H27B—C27—H27C | 109.5 |
C25—O3—Zn1 | 120.3 (3) | C26—C28—H28A | 120.0 |
C25—O4—Nd | 160.3 (4) | C26—C28—H28B | 120.0 |
C29—O5—Zn1 | 122.5 (4) | H28A—C28—H28B | 120.0 |
C29—O6—Nd | 135.4 (4) | O6—C29—O5 | 124.5 (6) |
N5—O7—Nd | 97.0 (3) | O6—C29—C30 | 119.2 (5) |
N5—O8—Nd | 96.4 (3) | O5—C29—C30 | 116.3 (5) |
C33—O10—Nd | 150.8 (4) | C32—C30—C31 | 122.4 (6) |
C33—O11—Zn2 | 122.3 (3) | C32—C30—C29 | 120.1 (6) |
C37—O12—Nd | 139.1 (3) | C31—C30—C29 | 117.5 (5) |
C37—O13—Zn2 | 127.5 (3) | C30—C31—H31A | 109.5 |
C41—O14—Nd | 143.3 (4) | C30—C31—H31B | 109.5 |
C41—O15—Zn2 | 108.4 (4) | H31A—C31—H31B | 109.5 |
C5—N1—C1 | 119.4 (4) | C30—C31—H31C | 109.5 |
C5—N1—Zn1 | 117.3 (3) | H31A—C31—H31C | 109.5 |
C1—N1—Zn1 | 123.3 (3) | H31B—C31—H31C | 109.5 |
C6—N2—C10 | 119.1 (4) | C30—C32—H32A | 120.0 |
C6—N2—Zn1 | 115.0 (3) | C30—C32—H32B | 120.0 |
C10—N2—Zn1 | 125.9 (3) | H32A—C32—H32B | 120.0 |
C15—N3—C11 | 118.0 (5) | O11—C33—O10 | 125.0 (5) |
C15—N3—Zn2 | 115.1 (4) | O11—C33—C34 | 117.4 (5) |
C11—N3—Zn2 | 126.5 (4) | O10—C33—C34 | 117.7 (5) |
C16—N4—C20 | 119.1 (5) | C35—C34—C36 | 123.2 (7) |
C16—N4—Zn2 | 116.7 (3) | C35—C34—C33 | 120.9 (6) |
C20—N4—Zn2 | 124.1 (4) | C36—C34—C33 | 115.9 (6) |
O9—N5—O7 | 121.8 (6) | C34—C35—H35A | 120.0 |
O9—N5—O8 | 121.0 (6) | C34—C35—H35B | 120.0 |
O7—N5—O8 | 117.2 (4) | H35A—C35—H35B | 120.0 |
N1—C1—C2 | 121.9 (5) | C34—C36—H36A | 109.5 |
N1—C1—H1 | 119.0 | C34—C36—H36B | 109.5 |
C2—C1—H1 | 119.0 | H36A—C36—H36B | 109.5 |
C1—C2—C3 | 118.9 (5) | C34—C36—H36C | 109.5 |
C1—C2—H2 | 120.6 | H36A—C36—H36C | 109.5 |
C3—C2—H2 | 120.6 | H36B—C36—H36C | 109.5 |
C4—C3—C2 | 119.4 (5) | O13—C37—O12 | 124.9 (5) |
C4—C3—H3 | 120.3 | O13—C37—C38 | 117.8 (5) |
C2—C3—H3 | 120.3 | O12—C37—C38 | 117.3 (5) |
C5—C4—C3 | 119.4 (5) | C40—C38—C37 | 118.2 (6) |
C5—C4—H4 | 120.3 | C40—C38—C39 | 124.0 (6) |
C3—C4—H4 | 120.3 | C37—C38—C39 | 117.9 (6) |
N1—C5—C4 | 120.9 (5) | C38—C39—H39A | 109.5 |
N1—C5—C6 | 116.1 (4) | C38—C39—H39B | 109.5 |
C4—C5—C6 | 123.0 (4) | H39A—C39—H39B | 109.5 |
N2—C6—C7 | 121.0 (5) | C38—C39—H39C | 109.5 |
N2—C6—C5 | 115.3 (4) | H39A—C39—H39C | 109.5 |
C7—C6—C5 | 123.8 (4) | H39B—C39—H39C | 109.5 |
C8—C7—C6 | 119.6 (5) | C38—C40—H40A | 120.0 |
C8—C7—H7 | 120.2 | C38—C40—H40B | 120.0 |
C6—C7—H7 | 120.2 | H40A—C40—H40B | 120.0 |
C7—C8—C9 | 119.9 (5) | O14—C41—O15 | 122.3 (5) |
C7—C8—H8 | 120.0 | O14—C41—C42 | 120.2 (5) |
C9—C8—H8 | 120.0 | O15—C41—C42 | 117.5 (5) |
C8—C9—C10 | 118.1 (5) | C43—C42—C44 | 123.2 (6) |
C8—C9—H9 | 120.9 | C43—C42—C41 | 119.7 (5) |
C10—C9—H9 | 120.9 | C44—C42—C41 | 117.0 (5) |
N2—C10—C9 | 122.3 (5) | C42—C43—H43A | 120.0 |
N2—C10—H10 | 118.9 | C42—C43—H43B | 120.0 |
C9—C10—H10 | 118.9 | H43A—C43—H43B | 120.0 |
N3—C11—C12 | 123.7 (6) | C42—C44—H44A | 109.5 |
N3—C11—H11 | 118.2 | C42—C44—H44B | 109.5 |
C12—C11—H11 | 118.2 | H44A—C44—H44B | 109.5 |
C11—C12—C13 | 117.8 (7) | C42—C44—H44C | 109.5 |
C11—C12—H12 | 121.1 | H44A—C44—H44C | 109.5 |
C13—C12—H12 | 121.1 | H44B—C44—H44C | 109.5 |
C14—C13—C12 | 119.6 (7) | | |