Bis(μ-N-acetyl-N-phenyl­glycinato-κ2O:O′)­bis­[tri­aqua(1,10-phenanthroline-κ2N,N′)­lanthanum(III)] bis(N-acetyl-N-phenyl­glycinate) dinitrate dihydrate

Fu, A.-Y.; Wang, D.-Q.; Shen, Q.-J.; Zhang, C.-L.

doi:10.1107/S1600536804021002

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Bis(μ-N-acetyl-N-phenylglycinato-κ²O:O′)bis[triaqua(1,10-phenanthroline-κ²N,N′)lanthanum(III)] bis(N-acetyl-N-phenylglycinate) dinitrate dihydrate

A.-Y. Fu, D.-Q. Wang, Q.-J. Shen and C.-L. Zhang

In the title complex, [La₂(C₁₀H₁₀NO₃)₂(C₁₂H₈N₂)₄(H₂O)₆](C₁₀H₁₀NO₃)₂(NO₃)₂·2H₂O, each La^III ion is nine-coordinated by four N atoms from two bidentate 1,10-phenanthroline ligands and by five O atoms (two from N-acetyl-N-phenylglycinate ligands and three from water molecules). The La^III cations, which exhibit distorted tricapped trigonal prismatic coordination, are bridged by two N-acetyl-N-phenylglycinate ligands into a dimeric structure, generated by inversion symmetry. The crystal structure is stabilized by a three-dimensional hydrogen-bond network.

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Supporting information

	Crystallographic Information File (CIF) https://doi.org/10.1107/S1600536804021002/hb6082sup1.cif Contains datablocks global, I
	Structure factor file (CIF format) https://doi.org/10.1107/S1600536804021002/hb6082Isup2.hkl Contains datablock I

CCDC reference: 251622

checkCIF report

Key indicators

Single-crystal X-ray study
T = 298 K
Mean (C-C) = 0.007 Å
R factor = 0.032
wR factor = 0.083
Data-to-parameter ratio = 12.7

checkCIF/PLATON results

No syntax errors found



Alert level C
PLAT042_ALERT_1_C Calc. and Rep. MoietyFormula Strings Differ ....          ?
PLAT220_ALERT_2_C Large Non-Solvent    C     Ueq(max)/Ueq(min) ...       3.46 Ratio
PLAT222_ALERT_3_C Large Non-Solvent    H     Ueq(max)/Ueq(min) ...       3.07 Ratio
PLAT241_ALERT_2_C Check High   U(eq) as Compared to Neighbors  for         C9
PLAT242_ALERT_2_C Check Low    U(eq) as Compared to Neighbors  for         C5
PLAT244_ALERT_4_C Low  Solvent U(eq) as Compared to Neighbors  for         N7
PLAT331_ALERT_2_C Small Average Phenyl C-C Dist.   C5     -C10           1.37 Ang.
PLAT380_ALERT_4_C Incorrectly Oriented X(sp2)-Methyl Moiety ......         C4
PLAT731_ALERT_1_C Bond    Calc     0.89(3), Rep   0.893(10) ......       3.00 su-Rat
              O4   -H1      1.555   1.555
PLAT731_ALERT_1_C Bond    Calc     0.90(3), Rep   0.898(10) ......       3.00 su-Rat
              O4   -H2      1.555   1.555
PLAT731_ALERT_1_C Bond    Calc     0.90(3), Rep   0.896(10) ......       3.00 su-Rat
              O5   -H4      1.555   1.555
PLAT731_ALERT_1_C Bond    Calc     0.90(4), Rep   0.897(10) ......       4.00 su-Rat
              O6   -H5      1.555   1.555
PLAT731_ALERT_1_C Bond    Calc     0.90(3), Rep   0.902(10) ......       3.00 su-Rat
              O13  -H15     1.555   1.555
PLAT731_ALERT_1_C Bond    Calc     0.91(4), Rep   0.901(10) ......       4.00 su-Rat
              O13  -H16     1.555   1.555
PLAT735_ALERT_1_C D-H     Calc     0.89(3), Rep   0.893(10) ......       3.00 su-Rat
              O4   -H1      1.555   1.555
PLAT735_ALERT_1_C D-H     Calc     0.90(3), Rep   0.898(10) ......       3.00 su-Rat
              O4   -H2      1.555   1.555
PLAT735_ALERT_1_C D-H     Calc     0.90(3), Rep   0.896(10) ......       3.00 su-Rat
              O5   -H4      1.555   1.555
PLAT735_ALERT_1_C D-H     Calc     0.90(4), Rep   0.897(10) ......       4.00 su-Rat
              O6   -H5      1.555   1.555
PLAT735_ALERT_1_C D-H     Calc     0.90(3), Rep   0.902(10) ......       3.00 su-Rat
              O13  -H15     1.555   1.555
PLAT735_ALERT_1_C D-H     Calc     0.91(4), Rep   0.901(10) ......       4.00 su-Rat
              O13  -H16     1.555   1.555
PLAT736_ALERT_1_C H...A   Calc     1.72(3), Rep   1.720(11) ......       2.73 su-Rat
              H2   -O7      1.555   1.555
PLAT736_ALERT_1_C H...A   Calc     1.88(4), Rep   1.879(17) ......       2.35 su-Rat
              H5   -O11     1.555   2.666
PLAT736_ALERT_1_C H...A   Calc     2.01(3), Rep   2.015(12) ......       2.50 su-Rat
              H15  -O12     1.555   2.666

   0 ALERT level A = In general: serious problem
   0 ALERT level B = Potentially serious problem
  23 ALERT level C = Check and explain
   0 ALERT level G = General alerts; check

  16 ALERT type 1 CIF construction/syntax error, inconsistent or missing data
   4 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

Computing details top

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

Bis(µ-N-acetyl-N-phenylglycinato-κ²O:O')bis[triaqua(1,10-phenanthroline- κ²N,N')lanthanum(III)] bis(µ-N-acetyl-N-phenylglycinate) dinitrate dihydrate top

Crystal data top

[La₂(C₁₀H₁₀NO₃)₂(C₁₂H₈N₂)₄(H₂O)₆](C₁₀H₁₀NO₃)₂(NO₃)₂·2H₂O	Z = 1
M_r = 2035.54	F(000) = 1036
Triclinic, P1	D_x = 1.524 Mg m⁻³
Hall symbol: -P 1	Mo Kα radiation, λ = 0.71073 Å
a = 11.4722 (19) Å	Cell parameters from 6354 reflections
b = 14.271 (2) Å	θ = 2.4–27.8°
c = 14.986 (2) Å	µ = 1.04 mm⁻¹
α = 66.966 (2)°	T = 298 K
β = 86.448 (2)°	Block, yellow
γ = 79.303 (2)°	0.45 × 0.37 × 0.19 mm
V = 2218.6 (6) Å³

Data collection top

Bruker SMART CCD area-detector diffractometer	7742 independent reflections
Radiation source: fine-focus sealed tube	6642 reflections with I > 2σ(I)
Graphite monochromator	R_int = 0.017
φ and ω scans	θ_max = 25.0°, θ_min = 1.7°
Absorption correction: multi-scan (SADABS; Siemens, 1996)	h = −13→13
T_min = 0.653, T_max = 0.828	k = −16→16
11765 measured reflections	l = −14→17

Refinement top

Refinement on F²	Primary atom site location: structure-invariant direct methods
Least-squares matrix: full	Secondary atom site location: difference Fourier map
R[F² > 2σ(F²)] = 0.032	Hydrogen site location: difmap and geom
wR(F²) = 0.083	H atoms treated by a mixture of independent and constrained refinement
S = 1.01	w = 1/[σ²(F_o²) + (0.0434P)² + 1.4707P] where P = (F_o² + 2F_c²)/3
7742 reflections	(Δ/σ)_max = 0.001
610 parameters	Δρ_max = 0.82 e Å⁻³
12 restraints	Δρ_min = −0.45 e Å⁻³

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

	x	y	z	U_iso*/U_eq
La1	0.879649 (16)	0.170938 (14)	0.150180 (13)	0.02839 (7)
N1	1.0577 (2)	−0.2468 (2)	0.16427 (19)	0.0352 (6)
N2	0.9673 (3)	0.0224 (2)	0.3227 (2)	0.0380 (7)
N3	1.1205 (2)	0.1005 (2)	0.17514 (19)	0.0340 (6)
N4	0.7033 (3)	0.2232 (2)	0.0147 (2)	0.0423 (7)
N5	0.7743 (3)	0.3805 (2)	0.0481 (2)	0.0441 (7)
N6	0.3312 (2)	0.2135 (2)	0.40713 (19)	0.0326 (6)
N7	0.2182 (3)	0.5549 (2)	0.6955 (2)	0.0416 (7)
O1	0.9291 (2)	0.02147 (17)	0.10807 (17)	0.0406 (6)
O2	0.8432 (2)	−0.1170 (2)	0.1682 (2)	0.0564 (7)
O3	1.0306 (2)	−0.23997 (18)	0.01428 (16)	0.0374 (5)
O4	0.7284 (2)	0.05162 (19)	0.21712 (19)	0.0435 (6)
O5	0.7396 (2)	0.2262 (2)	0.2606 (2)	0.0496 (7)
O6	0.9854 (2)	0.2713 (2)	0.2185 (2)	0.0459 (6)
O7	0.5632 (2)	0.03808 (19)	0.34780 (19)	0.0509 (7)
O8	0.5170 (2)	0.2097 (2)	0.2835 (2)	0.0510 (7)
O9	0.2104 (2)	0.2224 (2)	0.29035 (19)	0.0504 (7)
O10	0.2875 (3)	0.6159 (3)	0.6730 (3)	0.0955 (12)
O11	0.1137 (3)	0.5849 (3)	0.7068 (3)	0.0861 (11)
O12	0.2540 (4)	0.4658 (3)	0.7045 (3)	0.0894 (11)
O13	0.7605 (3)	0.7268 (3)	0.1313 (2)	0.0764 (10)
C1	0.9296 (3)	−0.0742 (3)	0.1367 (2)	0.0357 (8)
C2	1.0506 (3)	−0.1351 (2)	0.1284 (3)	0.0372 (8)
H2A	1.0732	−0.1103	0.0608	0.045*
H2B	1.1081	−0.1205	0.1638	0.045*
C3	1.0436 (3)	−0.2918 (2)	0.1030 (2)	0.0332 (7)
C4	1.0443 (4)	−0.4055 (3)	0.1437 (3)	0.0469 (9)
H4A	1.0551	−0.4325	0.2128	0.070*
H4B	1.1080	−0.4386	0.1158	0.070*
H4C	0.9702	−0.4184	0.1286	0.070*
C5	1.0857 (3)	−0.3050 (3)	0.2657 (2)	0.0407 (8)
C6	1.2011 (4)	−0.3463 (4)	0.2932 (4)	0.0710 (13)
H6	1.2603	−0.3373	0.2468	0.085*
C7	1.2296 (6)	−0.4017 (5)	0.3902 (5)	0.100 (2)
H7	1.3082	−0.4306	0.4088	0.120*
C8	1.1444 (8)	−0.4142 (5)	0.4581 (4)	0.105 (2)
H8	1.1640	−0.4512	0.5233	0.126*
C9	1.0316 (8)	−0.3727 (5)	0.4306 (4)	0.115 (3)
H9	0.9734	−0.3809	0.4777	0.138*
C10	0.9986 (5)	−0.3176 (4)	0.3335 (3)	0.0796 (16)
H10	0.9195	−0.2902	0.3154	0.096*
C11	1.1968 (3)	0.1391 (3)	0.1066 (3)	0.0464 (9)
H11	1.1671	0.1926	0.0493	0.056*
C12	1.3191 (3)	0.1044 (4)	0.1152 (3)	0.0567 (11)
H12	1.3691	0.1353	0.0653	0.068*
C13	1.3639 (3)	0.0249 (4)	0.1976 (3)	0.0562 (11)
H13	1.4452	0.0006	0.2048	0.067*
C14	1.2872 (3)	−0.0203 (3)	0.2717 (3)	0.0428 (9)
C15	1.1650 (3)	0.0207 (2)	0.2584 (2)	0.0340 (8)
C16	1.0849 (3)	−0.0208 (3)	0.3349 (2)	0.0356 (8)
C17	1.1290 (4)	−0.1043 (3)	0.4210 (3)	0.0472 (9)
C18	1.0479 (4)	−0.1411 (3)	0.4948 (3)	0.0617 (12)
H18	1.0735	−0.1970	0.5519	0.074*
C19	0.9325 (4)	−0.0955 (3)	0.4829 (3)	0.0592 (11)
H19	0.8787	−0.1181	0.5324	0.071*
C20	0.8953 (4)	−0.0143 (3)	0.3957 (3)	0.0488 (10)
H20	0.8155	0.0158	0.3882	0.059*
C21	1.3284 (4)	−0.1045 (3)	0.3600 (3)	0.0588 (11)
H21	1.4090	−0.1317	0.3685	0.071*
C22	1.2532 (4)	−0.1449 (3)	0.4308 (3)	0.0634 (12)
H22	1.2823	−0.2003	0.4872	0.076*
C23	0.6688 (4)	0.1486 (4)	−0.0029 (3)	0.0532 (10)
H23	0.7061	0.0808	0.0311	0.064*
C24	0.5796 (4)	0.1658 (5)	−0.0697 (3)	0.0707 (14)
H24	0.5578	0.1107	−0.0792	0.085*
C25	0.5254 (4)	0.2638 (5)	−0.1201 (4)	0.0754 (15)
H25	0.4655	0.2767	−0.1646	0.091*
C26	0.5592 (3)	0.3458 (4)	−0.1055 (3)	0.0605 (12)
C27	0.6500 (3)	0.3224 (3)	−0.0361 (3)	0.0437 (9)
C28	0.6877 (3)	0.4044 (3)	−0.0196 (3)	0.0448 (9)
C29	0.6364 (4)	0.5080 (3)	−0.0762 (3)	0.0594 (12)
C30	0.6769 (5)	0.5862 (4)	−0.0602 (4)	0.0777 (16)
H30	0.6452	0.6550	−0.0960	0.093*
C31	0.7621 (5)	0.5624 (3)	0.0072 (4)	0.0780 (15)
H31	0.7897	0.6142	0.0183	0.094*
C32	0.8081 (5)	0.4576 (3)	0.0603 (3)	0.0634 (12)
H32	0.8661	0.4420	0.1071	0.076*
C33	0.5090 (4)	0.4518 (5)	−0.1596 (4)	0.0828 (17)
H33	0.4499	0.4675	−0.2056	0.099*
C34	0.5453 (4)	0.5279 (4)	−0.1454 (3)	0.0784 (17)
H34	0.5106	0.5960	−0.1814	0.094*
C35	0.5015 (3)	0.1220 (3)	0.3410 (2)	0.0365 (8)
C36	0.3972 (3)	0.1140 (3)	0.4110 (2)	0.0356 (8)
H36A	0.3431	0.0769	0.3967	0.043*
H36B	0.4272	0.0736	0.4766	0.043*
C37	0.2425 (3)	0.2629 (3)	0.3418 (2)	0.0359 (8)
C38	0.1817 (4)	0.3676 (3)	0.3354 (3)	0.0587 (11)
H38A	0.1208	0.3945	0.2862	0.088*
H38B	0.2384	0.4133	0.3192	0.088*
H38C	0.1467	0.3622	0.3968	0.088*
C39	0.3702 (3)	0.2579 (3)	0.4690 (3)	0.0360 (8)
C40	0.4537 (3)	0.3206 (3)	0.4380 (3)	0.0451 (9)
H40	0.4869	0.3341	0.3770	0.054*
C41	0.4890 (4)	0.3641 (3)	0.4980 (3)	0.0554 (11)
H41	0.5451	0.4074	0.4771	0.066*
C42	0.4401 (4)	0.3426 (4)	0.5887 (4)	0.0672 (13)
H42	0.4633	0.3718	0.6289	0.081*
C43	0.3585 (4)	0.2792 (4)	0.6198 (3)	0.0708 (14)
H43	0.3258	0.2658	0.6810	0.085*
C44	0.3234 (4)	0.2342 (3)	0.5609 (3)	0.0546 (10)
H44	0.2695	0.1890	0.5831	0.065*
H1	0.751 (3)	−0.0094 (16)	0.212 (3)	0.065*
H2	0.670 (3)	0.045 (3)	0.261 (2)	0.065*
H3	0.6620 (13)	0.222 (3)	0.261 (3)	0.065*
H4	0.746 (3)	0.276 (2)	0.282 (3)	0.065*
H5	0.946 (3)	0.307 (3)	0.252 (3)	0.065*
H14	1.0631 (10)	0.261 (3)	0.231 (3)	0.065*
H15	0.759 (4)	0.6698 (19)	0.1859 (18)	0.065*
H16	0.800 (3)	0.769 (2)	0.145 (3)	0.065*

Atomic displacement parameters (Å²) top

	U¹¹	U²²	U³³	U¹²	U¹³	U²³
La1	0.02920 (11)	0.02427 (11)	0.02977 (11)	−0.00269 (7)	−0.00187 (7)	−0.00899 (8)
N1	0.0427 (17)	0.0271 (15)	0.0305 (15)	−0.0004 (12)	0.0015 (12)	−0.0083 (12)
N2	0.0383 (16)	0.0380 (17)	0.0313 (16)	−0.0072 (13)	−0.0011 (13)	−0.0062 (13)
N3	0.0333 (15)	0.0346 (16)	0.0308 (15)	−0.0042 (12)	0.0008 (12)	−0.0101 (13)
N4	0.0360 (16)	0.0491 (19)	0.0423 (18)	−0.0065 (14)	−0.0055 (13)	−0.0176 (15)
N5	0.057 (2)	0.0328 (16)	0.0383 (17)	0.0028 (14)	−0.0074 (15)	−0.0131 (14)
N6	0.0285 (14)	0.0318 (15)	0.0370 (16)	−0.0002 (12)	−0.0029 (12)	−0.0147 (13)
N7	0.0463 (19)	0.0423 (19)	0.0415 (18)	−0.0048 (15)	−0.0011 (14)	−0.0231 (15)
O1	0.0532 (15)	0.0238 (12)	0.0443 (14)	−0.0066 (11)	0.0082 (11)	−0.0138 (11)
O2	0.0444 (16)	0.0345 (14)	0.090 (2)	−0.0119 (12)	0.0150 (14)	−0.0232 (14)
O3	0.0424 (14)	0.0340 (13)	0.0286 (13)	−0.0044 (10)	−0.0009 (10)	−0.0054 (10)
O4	0.0432 (15)	0.0385 (14)	0.0546 (17)	−0.0132 (12)	0.0149 (12)	−0.0235 (13)
O5	0.0428 (15)	0.0471 (16)	0.0686 (19)	−0.0128 (13)	0.0161 (13)	−0.0330 (14)
O6	0.0351 (14)	0.0517 (16)	0.0611 (17)	−0.0026 (12)	−0.0093 (12)	−0.0335 (14)
O7	0.0471 (15)	0.0399 (15)	0.0559 (17)	0.0029 (12)	0.0140 (12)	−0.0148 (13)
O8	0.0431 (15)	0.0371 (15)	0.0614 (18)	−0.0052 (12)	0.0154 (13)	−0.0099 (13)
O9	0.0430 (15)	0.0604 (17)	0.0529 (17)	−0.0057 (13)	−0.0111 (12)	−0.0273 (14)
O10	0.087 (3)	0.095 (3)	0.134 (4)	−0.050 (2)	0.033 (2)	−0.065 (3)
O11	0.052 (2)	0.114 (3)	0.120 (3)	−0.0082 (19)	0.0111 (19)	−0.080 (3)
O12	0.119 (3)	0.048 (2)	0.103 (3)	0.004 (2)	−0.013 (2)	−0.0367 (19)
O13	0.083 (2)	0.083 (3)	0.071 (2)	−0.039 (2)	0.0004 (19)	−0.0278 (19)
C1	0.044 (2)	0.0305 (19)	0.0320 (19)	−0.0033 (16)	0.0029 (15)	−0.0131 (15)
C2	0.044 (2)	0.0288 (18)	0.037 (2)	−0.0071 (15)	0.0073 (15)	−0.0112 (15)
C3	0.0329 (18)	0.0280 (17)	0.0315 (19)	−0.0006 (14)	0.0023 (14)	−0.0063 (15)
C4	0.064 (3)	0.0290 (19)	0.043 (2)	−0.0081 (17)	−0.0013 (18)	−0.0082 (16)
C5	0.055 (2)	0.0328 (19)	0.0330 (19)	−0.0067 (17)	−0.0024 (17)	−0.0120 (16)
C6	0.058 (3)	0.081 (3)	0.063 (3)	−0.012 (3)	−0.015 (2)	−0.014 (3)
C7	0.113 (5)	0.094 (5)	0.084 (4)	−0.020 (4)	−0.058 (4)	−0.013 (4)
C8	0.196 (8)	0.072 (4)	0.042 (3)	−0.018 (5)	−0.042 (4)	−0.012 (3)
C9	0.180 (7)	0.096 (5)	0.037 (3)	0.005 (5)	0.023 (4)	−0.007 (3)
C10	0.084 (4)	0.085 (4)	0.040 (3)	0.011 (3)	0.015 (2)	−0.005 (2)
C11	0.042 (2)	0.052 (2)	0.038 (2)	−0.0059 (18)	0.0009 (17)	−0.0112 (18)
C12	0.040 (2)	0.078 (3)	0.054 (3)	−0.016 (2)	0.0110 (19)	−0.026 (2)
C13	0.033 (2)	0.074 (3)	0.067 (3)	0.003 (2)	−0.005 (2)	−0.038 (3)
C14	0.038 (2)	0.039 (2)	0.051 (2)	0.0039 (16)	−0.0086 (17)	−0.0211 (18)
C15	0.0350 (18)	0.0283 (17)	0.039 (2)	−0.0001 (14)	−0.0072 (15)	−0.0147 (15)
C16	0.0395 (19)	0.0285 (17)	0.0354 (19)	−0.0033 (15)	−0.0068 (15)	−0.0089 (15)
C17	0.055 (2)	0.034 (2)	0.044 (2)	−0.0044 (18)	−0.0121 (18)	−0.0052 (17)
C18	0.081 (3)	0.047 (2)	0.042 (2)	−0.020 (2)	−0.013 (2)	0.0054 (19)
C19	0.069 (3)	0.061 (3)	0.039 (2)	−0.029 (2)	0.003 (2)	−0.004 (2)
C20	0.047 (2)	0.054 (2)	0.038 (2)	−0.0140 (19)	0.0038 (17)	−0.0080 (18)
C21	0.044 (2)	0.055 (3)	0.069 (3)	0.012 (2)	−0.018 (2)	−0.021 (2)
C22	0.065 (3)	0.045 (2)	0.060 (3)	0.006 (2)	−0.025 (2)	−0.001 (2)
C23	0.047 (2)	0.065 (3)	0.055 (3)	−0.014 (2)	−0.0007 (19)	−0.029 (2)
C24	0.058 (3)	0.107 (4)	0.063 (3)	−0.035 (3)	−0.001 (2)	−0.042 (3)
C25	0.046 (3)	0.125 (5)	0.057 (3)	−0.017 (3)	−0.014 (2)	−0.035 (3)
C26	0.034 (2)	0.092 (4)	0.043 (2)	0.003 (2)	−0.0053 (18)	−0.019 (2)
C27	0.0278 (18)	0.060 (3)	0.0324 (19)	0.0044 (17)	−0.0001 (15)	−0.0123 (18)
C28	0.041 (2)	0.047 (2)	0.033 (2)	0.0101 (17)	0.0019 (16)	−0.0085 (17)
C29	0.063 (3)	0.051 (3)	0.040 (2)	0.020 (2)	0.004 (2)	−0.006 (2)
C30	0.111 (4)	0.039 (3)	0.056 (3)	0.020 (3)	0.002 (3)	−0.004 (2)
C31	0.127 (5)	0.036 (2)	0.066 (3)	−0.006 (3)	−0.003 (3)	−0.018 (2)
C32	0.098 (4)	0.036 (2)	0.051 (3)	−0.003 (2)	−0.012 (2)	−0.013 (2)
C33	0.048 (3)	0.115 (5)	0.055 (3)	0.020 (3)	−0.020 (2)	−0.013 (3)
C34	0.066 (3)	0.078 (4)	0.050 (3)	0.033 (3)	−0.009 (2)	−0.001 (3)
C35	0.0288 (17)	0.041 (2)	0.038 (2)	−0.0035 (15)	−0.0004 (14)	−0.0139 (17)
C36	0.0340 (18)	0.0334 (18)	0.0369 (19)	−0.0019 (15)	0.0004 (15)	−0.0127 (15)
C37	0.0308 (18)	0.0358 (19)	0.0375 (19)	−0.0066 (15)	0.0012 (15)	−0.0103 (16)
C38	0.054 (3)	0.042 (2)	0.071 (3)	0.0104 (19)	−0.022 (2)	−0.017 (2)
C39	0.0307 (18)	0.0369 (19)	0.042 (2)	0.0033 (15)	−0.0046 (15)	−0.0199 (16)
C40	0.044 (2)	0.046 (2)	0.048 (2)	−0.0096 (17)	−0.0045 (17)	−0.0188 (18)
C41	0.050 (2)	0.048 (2)	0.075 (3)	−0.0070 (19)	−0.012 (2)	−0.030 (2)
C42	0.064 (3)	0.082 (3)	0.073 (3)	0.001 (3)	−0.017 (2)	−0.053 (3)
C43	0.068 (3)	0.106 (4)	0.059 (3)	−0.016 (3)	0.009 (2)	−0.055 (3)
C44	0.052 (2)	0.070 (3)	0.050 (2)	−0.015 (2)	0.0090 (19)	−0.033 (2)

Geometric parameters (Å, º) top

La1—O1	2.415 (2)	C11—C12	1.395 (5)
La1—O5	2.483 (2)	C11—H11	0.9300
La1—O3ⁱ	2.503 (2)	C12—C13	1.358 (6)
La1—O4	2.542 (2)	C12—H12	0.9300
La1—O6	2.553 (2)	C13—C14	1.397 (6)
La1—N2	2.726 (3)	C13—H13	0.9300
La1—N4	2.745 (3)	C14—C15	1.409 (5)
La1—N3	2.755 (3)	C14—C21	1.428 (6)
La1—N5	2.838 (3)	C15—C16	1.432 (5)
N1—C3	1.341 (4)	C16—C17	1.413 (5)
N1—C5	1.442 (4)	C17—C18	1.401 (6)
N1—C2	1.458 (4)	C17—C22	1.428 (6)
N2—C20	1.324 (5)	C18—C19	1.352 (6)
N2—C16	1.366 (4)	C18—H18	0.9300
N3—C11	1.322 (4)	C19—C20	1.390 (5)
N3—C15	1.365 (4)	C19—H19	0.9300
N4—C23	1.322 (5)	C20—H20	0.9300
N4—C27	1.361 (5)	C21—C22	1.340 (6)
N5—C32	1.311 (5)	C21—H21	0.9300
N5—C28	1.365 (5)	C22—H22	0.9300
N6—C37	1.344 (4)	C23—C24	1.397 (6)
N6—C39	1.441 (4)	C23—H23	0.9300
N6—C36	1.461 (4)	C24—C25	1.350 (7)
N7—O12	1.218 (4)	C24—H24	0.9300
N7—O11	1.221 (4)	C25—C26	1.396 (7)
N7—O10	1.223 (4)	C25—H25	0.9300
O1—C1	1.260 (4)	C26—C27	1.419 (5)
O2—C1	1.233 (4)	C26—C33	1.432 (7)
O3—C3	1.245 (4)	C27—C28	1.429 (6)
O3—La1ⁱ	2.503 (2)	C28—C29	1.417 (5)
O4—H1	0.893 (10)	C29—C30	1.391 (7)
O4—H2	0.898 (10)	C29—C34	1.429 (7)
O5—H3	0.903 (10)	C30—C31	1.350 (7)
O5—H4	0.896 (10)	C30—H30	0.9300
O6—H5	0.897 (10)	C31—C32	1.405 (6)
O6—H14	0.896 (10)	C31—H31	0.9300
O7—C35	1.243 (4)	C32—H32	0.9300
O8—C35	1.248 (4)	C33—C34	1.326 (8)
O9—C37	1.237 (4)	C33—H33	0.9300
O13—H15	0.902 (10)	C34—H34	0.9300
O13—H16	0.901 (10)	C35—C36	1.533 (5)
C1—C2	1.520 (5)	C36—H36A	0.9700
C2—H2A	0.9700	C36—H36B	0.9700
C2—H2B	0.9700	C37—C38	1.497 (5)
C3—C4	1.492 (5)	C38—H38A	0.9600
C4—H4A	0.9600	C38—H38B	0.9600
C4—H4B	0.9600	C38—H38C	0.9600
C4—H4C	0.9600	C39—C40	1.369 (5)
C5—C6	1.363 (6)	C39—C44	1.383 (5)
C5—C10	1.364 (6)	C40—C41	1.390 (5)
C6—C7	1.382 (7)	C40—H40	0.9300
C6—H6	0.9300	C41—C42	1.378 (6)
C7—C8	1.350 (9)	C41—H41	0.9300
C7—H7	0.9300	C42—C43	1.357 (7)
C8—C9	1.335 (9)	C42—H42	0.9300
C8—H8	0.9300	C43—C44	1.391 (6)
C9—C10	1.394 (7)	C43—H43	0.9300
C9—H9	0.9300	C44—H44	0.9300
C10—H10	0.9300

O1—La1—O5	136.86 (9)	C12—C11—H11	118.0
O1—La1—O3ⁱ	76.41 (8)	C13—C12—C11	118.8 (4)
O5—La1—O3ⁱ	141.59 (8)	C13—C12—H12	120.6
O1—La1—O4	68.90 (8)	C11—C12—H12	120.6
O5—La1—O4	68.75 (8)	C12—C13—C14	119.7 (4)
O3ⁱ—La1—O4	131.56 (8)	C12—C13—H13	120.2
O1—La1—O6	137.74 (8)	C14—C13—H13	120.2
O5—La1—O6	72.64 (9)	C13—C14—C15	118.0 (3)
O3ⁱ—La1—O6	94.25 (8)	C13—C14—C21	122.5 (4)
O4—La1—O6	134.11 (9)	C15—C14—C21	119.5 (4)
O1—La1—N2	79.01 (8)	N3—C15—C14	122.0 (3)
O5—La1—N2	81.15 (9)	N3—C15—C16	118.7 (3)
O3ⁱ—La1—N2	132.32 (8)	C14—C15—C16	119.3 (3)
O4—La1—N2	72.77 (9)	N2—C16—C17	121.7 (3)
O6—La1—N2	77.72 (9)	N2—C16—C15	118.8 (3)
O1—La1—N4	81.82 (9)	C17—C16—C15	119.5 (3)
O5—La1—N4	91.60 (9)	C18—C17—C16	117.6 (4)
O3ⁱ—La1—N4	72.15 (8)	C18—C17—C22	123.0 (4)
O4—La1—N4	70.39 (9)	C16—C17—C22	119.4 (4)
O6—La1—N4	135.01 (9)	C19—C18—C17	120.0 (4)
N2—La1—N4	142.56 (9)	C19—C18—H18	120.0
O1—La1—N3	71.44 (8)	C17—C18—H18	120.0
O5—La1—N3	127.88 (9)	C18—C19—C20	119.1 (4)
O3ⁱ—La1—N3	73.48 (8)	C18—C19—H19	120.5
O4—La1—N3	122.56 (8)	C20—C19—H19	120.5
O6—La1—N3	66.42 (8)	N2—C20—C19	123.6 (4)
N2—La1—N3	60.12 (8)	N2—C20—H20	118.2
N4—La1—N3	140.38 (8)	C19—C20—H20	118.2
O1—La1—N5	134.17 (8)	C22—C21—C14	121.3 (4)
O5—La1—N5	71.85 (9)	C22—C21—H21	119.4
O3ⁱ—La1—N5	69.94 (8)	C14—C21—H21	119.4
O4—La1—N5	113.09 (9)	C21—C22—C17	121.0 (4)
O6—La1—N5	76.00 (9)	C21—C22—H22	119.5
N2—La1—N5	146.76 (8)	C17—C22—H22	119.5
N4—La1—N5	59.01 (9)	N4—C23—C24	123.7 (4)
N3—La1—N5	124.35 (9)	N4—C23—H23	118.1
C3—N1—C5	122.8 (3)	C24—C23—H23	118.1
C3—N1—C2	120.2 (3)	C25—C24—C23	118.8 (5)
C5—N1—C2	117.0 (3)	C25—C24—H24	120.6
C20—N2—C16	117.9 (3)	C23—C24—H24	120.6
C20—N2—La1	120.5 (2)	C24—C25—C26	120.1 (4)
C16—N2—La1	121.4 (2)	C24—C25—H25	120.0
C11—N3—C15	117.5 (3)	C26—C25—H25	120.0
C11—N3—La1	122.0 (2)	C25—C26—C27	118.0 (4)
C15—N3—La1	120.5 (2)	C25—C26—C33	122.8 (4)
C23—N4—C27	118.2 (3)	C27—C26—C33	119.1 (5)
C23—N4—La1	118.6 (3)	N4—C27—C26	121.3 (4)
C27—N4—La1	123.2 (2)	N4—C27—C28	119.1 (3)
C32—N5—C28	117.4 (3)	C26—C27—C28	119.6 (4)
C32—N5—La1	122.8 (3)	N5—C28—C29	122.1 (4)
C28—N5—La1	119.8 (2)	N5—C28—C27	118.9 (3)
C37—N6—C39	122.8 (3)	C29—C28—C27	118.9 (4)
C37—N6—C36	119.0 (3)	C30—C29—C28	117.6 (4)
C39—N6—C36	118.1 (3)	C30—C29—C34	122.9 (4)
O12—N7—O11	121.0 (4)	C28—C29—C34	119.5 (5)
O12—N7—O10	119.5 (4)	C31—C30—C29	120.2 (4)
O11—N7—O10	119.4 (4)	C31—C30—H30	119.9
C1—O1—La1	145.1 (2)	C29—C30—H30	119.9
C3—O3—La1ⁱ	149.2 (2)	C30—C31—C32	118.6 (5)
La1—O4—H1	113 (2)	C30—C31—H31	120.7
La1—O4—H2	136 (2)	C32—C31—H31	120.7
H1—O4—H2	108 (2)	N5—C32—C31	124.1 (4)
La1—O5—H3	121 (2)	N5—C32—H32	117.9
La1—O5—H4	126 (2)	C31—C32—H32	117.9
H3—O5—H4	108 (2)	C34—C33—C26	121.2 (5)
La1—O6—H5	121 (2)	C34—C33—H33	119.4
La1—O6—H14	127 (2)	C26—C33—H33	119.4
H5—O6—H14	108 (2)	C33—C34—C29	121.6 (5)
H15—O13—H16	108 (2)	C33—C34—H34	119.2
O2—C1—O1	125.4 (3)	C29—C34—H34	119.2
O2—C1—C2	121.7 (3)	O7—C35—O8	126.4 (3)
O1—C1—C2	112.9 (3)	O7—C35—C36	115.1 (3)
N1—C2—C1	115.3 (3)	O8—C35—C36	118.5 (3)
N1—C2—H2A	108.4	N6—C36—C35	114.4 (3)
C1—C2—H2A	108.4	N6—C36—H36A	108.7
N1—C2—H2B	108.4	C35—C36—H36A	108.7
C1—C2—H2B	108.4	N6—C36—H36B	108.7
H2A—C2—H2B	107.5	C35—C36—H36B	108.7
O3—C3—N1	120.8 (3)	H36A—C36—H36B	107.6
O3—C3—C4	120.8 (3)	O9—C37—N6	121.3 (3)
N1—C3—C4	118.3 (3)	O9—C37—C38	121.0 (3)
C3—C4—H4A	109.5	N6—C37—C38	117.6 (3)
C3—C4—H4B	109.5	C37—C38—H38A	109.5
H4A—C4—H4B	109.5	C37—C38—H38B	109.5
C3—C4—H4C	109.5	H38A—C38—H38B	109.5
H4A—C4—H4C	109.5	C37—C38—H38C	109.5
H4B—C4—H4C	109.5	H38A—C38—H38C	109.5
C6—C5—C10	120.4 (4)	H38B—C38—H38C	109.5
C6—C5—N1	118.9 (4)	C40—C39—C44	120.6 (3)
C10—C5—N1	120.7 (4)	C40—C39—N6	120.6 (3)
C5—C6—C7	119.6 (5)	C44—C39—N6	118.8 (3)
C5—C6—H6	120.2	C39—C40—C41	119.9 (4)
C7—C6—H6	120.2	C39—C40—H40	120.1
C8—C7—C6	120.6 (6)	C41—C40—H40	120.1
C8—C7—H7	119.7	C42—C41—C40	119.4 (4)
C6—C7—H7	119.7	C42—C41—H41	120.3
C9—C8—C7	119.3 (5)	C40—C41—H41	120.3
C9—C8—H8	120.4	C43—C42—C41	120.6 (4)
C7—C8—H8	120.4	C43—C42—H42	119.7
C8—C9—C10	122.1 (6)	C41—C42—H42	119.7
C8—C9—H9	119.0	C42—C43—C44	120.6 (4)
C10—C9—H9	119.0	C42—C43—H43	119.7
C5—C10—C9	118.0 (5)	C44—C43—H43	119.7
C5—C10—H10	121.0	C39—C44—C43	118.9 (4)
C9—C10—H10	121.0	C39—C44—H44	120.6
N3—C11—C12	124.0 (4)	C43—C44—H44	120.6
N3—C11—H11	118.0

O1—C1—C2—N1	177.6 (3)

Symmetry code: (i) −x+2, −y, −z.

Hydrogen-bond geometry (Å, º) top

D—H···A	D—H	H···A	D···A	D—H···A
O4—H1···O2	0.89 (1)	2.00 (2)	2.855 (3)	159 (3)
O4—H2···O7	0.90 (1)	1.72 (1)	2.616 (3)	175 (4)
O5—H3···O8	0.90 (1)	1.71 (1)	2.598 (4)	169 (4)
O5—H4···O10ⁱⁱ	0.90 (1)	1.89 (2)	2.760 (4)	164 (3)
O6—H5···O11ⁱⁱ	0.90 (1)	1.88 (2)	2.744 (4)	161 (4)
O6—H14···O9ⁱⁱⁱ	0.90 (1)	1.84 (2)	2.719 (3)	165 (4)
O13—H15···O12ⁱⁱ	0.90 (1)	2.02 (1)	2.910 (5)	172 (3)
O13—H16···O2^iv	0.90 (1)	1.95 (2)	2.825 (4)	164 (4)

Symmetry codes: (ii) −x+1, −y+1, −z+1; (iii) x+1, y, z; (iv) x, y+1, z.

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