Tetra­aqua­[2,6-di­acetyl­pyridine bis­(semi­carbazone)]samarium(III) trinitrate

Gioia, M.; Crundwell, G.; Westcott, B.L.

doi:10.1107/S2414314618014542

Tetraaqua[2,6-diacetylpyridine bis(semicarbazone)]samarium(III) trinitrate

M. Gioia, G. Crundwell and B. L. Westcott

The structure of tetraaqua[2,6-diacetylpyridine bis(semicarbazone)]samarium(III) trinitrate, [Sm(C₁₁H₁₅N₇O₂)(H₂O)₄](NO₃)₃, has monoclinic (P2₁/c) symmetry. The 2,6-diacetylpyridine (DAPSC) ligand is pentadentate. The coordination of the DAPSC ligand and four coordinated water molecules around the metal cation is best described as a distorted tricapped trigonal prism. The structure displays intermolecular hydrogen bonding. The structure is isomorphous with many other published lanthanide(III) nitrate salts with the DAPSC ligand, 2,6-diacetylpyridinebis(semicarbazone). One of the three nitrate counter-anions is disordered, which is consistent with the structures of other +3 lanthanide nitrate salts with DAPSC. Refinement of occupancies for the disordered nitrate group gave major and minor occupancies of 54.9 (14) and 45.1 (14)%, respectively.

Keywords: crystal structure; lanthanide(III) salts; DAPSC.

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Supporting information

	Crystallographic Information File (CIF) https://doi.org/10.1107/S2414314618014542/sj4193sup1.cif Contains datablock I
	Structure factor file (CIF format) https://doi.org/10.1107/S2414314618014542/sj4193Isup2.hkl Contains datablock I

CCDC reference: 1873366

checkCIF report

Key indicators

Single-crystal X-ray study
T = 293 K
Mean (C-C) = 0.009 Å
Disorder in solvent or counterion
R factor = 0.049
wR factor = 0.127
Data-to-parameter ratio = 23.9

checkCIF/PLATON results

No syntax errors found



Alert level B
PLAT414_ALERT_2_B Short Intra D-H..H-X       H2       ..H3E              1.89 Ang.
                                                      x,y,z  =      1_555 Check

Author Response: H3E is part of a rotating methyl group and H2 is on a sp2 hybridized nitrogen so its distance is a matter of geometric consequence.

PLAT910_ALERT_3_B Missing # of FCF Reflection(s) Below Theta(Min).         17 Note

Author Response: A handful of reflections were omitted from the refinement.


Alert level C
PLAT242_ALERT_2_C Low    'MainMol' Ueq as Compared to Neighbors of        Sm1 Check
PLAT244_ALERT_4_C Low    'Solvent' Ueq as Compared to Neighbors of         N8 Check
PLAT244_ALERT_4_C Low    'Solvent' Ueq as Compared to Neighbors of         N9 Check
PLAT260_ALERT_2_C Large Average Ueq of Residue Including       O13      0.087 Check
PLAT260_ALERT_2_C Large Average Ueq of Residue Including      O13B      0.113 Check
PLAT342_ALERT_3_C Low Bond Precision on  C-C Bonds ...............     0.0095 Ang.
PLAT414_ALERT_2_C Short Intra D-H..H-X       H6       ..H10A             1.92 Ang.
                                                      x,y,z  =      1_555 Check

Author Response: H3E is part of a rotating methyl group and H2 is on a sp2 hybridized nitrogen so its distance is a matter of geometric consequence.

PLAT480_ALERT_4_C Long H...A H-Bond Reported H5B      ..O8       .       2.66 Ang.
PLAT906_ALERT_3_C Large K Value in the Analysis of Variance ......      5.426 Check
PLAT911_ALERT_3_C Missing FCF Refl Between Thmin & STh/L=    0.600          9 Report
PLAT971_ALERT_2_C Check Calcd Resid. Dens.  1.14A   From Sm1             1.53 eA-3
PLAT972_ALERT_2_C Check Calcd Resid. Dens.  0.73A   From Sm1            -1.51 eA-3
PLAT975_ALERT_2_C Check Calcd Resid. Dens.  0.96A   From O5              0.49 eA-3
PLAT975_ALERT_2_C Check Calcd Resid. Dens.  1.05A   From O2              0.48 eA-3
PLAT976_ALERT_2_C Check Calcd Resid. Dens.  0.92A   From O4             -0.89 eA-3
PLAT976_ALERT_2_C Check Calcd Resid. Dens.  0.43A   From O5             -0.81 eA-3
PLAT976_ALERT_2_C Check Calcd Resid. Dens.  0.52A   From O3             -0.68 eA-3
PLAT976_ALERT_2_C Check Calcd Resid. Dens.  0.93A   From O4             -0.57 eA-3
PLAT976_ALERT_2_C Check Calcd Resid. Dens.  0.82A   From O4             -0.57 eA-3
PLAT976_ALERT_2_C Check Calcd Resid. Dens.  0.61A   From O3             -0.53 eA-3
PLAT976_ALERT_2_C Check Calcd Resid. Dens.  0.61A   From O3             -0.53 eA-3
PLAT976_ALERT_2_C Check Calcd Resid. Dens.  0.57A   From O6             -0.52 eA-3
PLAT977_ALERT_2_C Check Negative Difference Density on H3B              -0.47 eA-3
PLAT978_ALERT_2_C Number C-C Bonds with Positive Residual Density.          0 Info

Alert level G
PLAT005_ALERT_5_G No Embedded Refinement Details Found  in the CIF     Please Do !
PLAT007_ALERT_5_G Number of Unrefined Donor-H Atoms ..............         14 Report
PLAT128_ALERT_4_G Alternate Setting for Input Space Group  P21/c        P21/n Note
PLAT152_ALERT_1_G The Supplied and Calc. Volume s.u. Differ by ...          2 Units
PLAT199_ALERT_1_G Reported _cell_measurement_temperature ..... (K)        293 Check
PLAT200_ALERT_1_G Reported   _diffrn_ambient_temperature ..... (K)        293 Check
PLAT232_ALERT_2_G Hirshfeld Test Diff (M-X)  Sm1      --O1       .        6.7 s.u.
PLAT232_ALERT_2_G Hirshfeld Test Diff (M-X)  Sm1      --O2       .        6.0 s.u.
PLAT232_ALERT_2_G Hirshfeld Test Diff (M-X)  Sm1      --O3       .        8.2 s.u.
PLAT232_ALERT_2_G Hirshfeld Test Diff (M-X)  Sm1      --O4       .        8.8 s.u.
PLAT232_ALERT_2_G Hirshfeld Test Diff (M-X)  Sm1      --O5       .        5.4 s.u.
PLAT232_ALERT_2_G Hirshfeld Test Diff (M-X)  Sm1      --O6       .        6.3 s.u.
PLAT232_ALERT_2_G Hirshfeld Test Diff (M-X)  Sm1      --N3       .        5.6 s.u.
PLAT232_ALERT_2_G Hirshfeld Test Diff (M-X)  Sm1      --N5       .        7.3 s.u.
PLAT302_ALERT_4_G Anion/Solvent/Minor-Residue Disorder (Resd  4  )       100% Note
PLAT302_ALERT_4_G Anion/Solvent/Minor-Residue Disorder (Resd  5  )       100% Note
PLAT304_ALERT_4_G Non-Integer Number of Atoms in ...... Resd  4          2.20 Check
PLAT304_ALERT_4_G Non-Integer Number of Atoms in ...... Resd  5          1.80 Check
PLAT432_ALERT_2_G Short Inter X...Y Contact  O15      ..C3               2.89 Ang.
                                            1+x,1/2-y,1/2+z  =      4_666 Check
PLAT726_ALERT_2_G H...A   Calc     2.62000, Rep     2.63000 Dev...       0.01 Ang.
              H5B      -N8              1.555   1.656 ........     #   64 Check
PLAT790_ALERT_4_G Centre of Gravity not Within Unit Cell: Resd.  #          2 Note
              N O3
PLAT790_ALERT_4_G Centre of Gravity not Within Unit Cell: Resd.  #          4 Note
              N O3
PLAT790_ALERT_4_G Centre of Gravity not Within Unit Cell: Resd.  #          5 Note
              N O3
PLAT860_ALERT_3_G Number of Least-Squares Restraints .............         12 Note
PLAT912_ALERT_4_G Missing # of FCF Reflections Above STh/L=  0.600       2519 Note
PLAT950_ALERT_5_G Calculated (ThMax) and CIF-Reported Hmax Differ           2 Units
PLAT951_ALERT_5_G Calculated (ThMax) and CIF-Reported Kmax Differ           3 Units
PLAT952_ALERT_5_G Calculated (ThMax) and CIF-Reported Lmax Differ           2 Units
PLAT956_ALERT_1_G Calculated (ThMax) and Actual (FCF) Hmax Differ           2 Units
PLAT957_ALERT_1_G Calculated (ThMax) and Actual (FCF) Kmax Differ           3 Units
PLAT958_ALERT_1_G Calculated (ThMax) and Actual (FCF) Lmax Differ           2 Units

   0 ALERT level A = Most likely a serious problem - resolve or explain
   2 ALERT level B = A potentially serious problem, consider carefully
  24 ALERT level C = Check. Ensure it is not caused by an omission or oversight
  31 ALERT level G = General information/check it is not something unexpected

   6 ALERT type 1 CIF construction/syntax error, inconsistent or missing data
  29 ALERT type 2 Indicator that the structure model may be wrong or deficient
   5 ALERT type 3 Indicator that the structure quality may be low
  12 ALERT type 4 Improvement, methodology, query or suggestion
   5 ALERT type 5 Informative message, check

Computing details top

Data collection: CrysAlis PRO (Rigaku OD, 2018); cell refinement: CrysAlis PRO (Rigaku OD, 2018); data reduction: CrysAlis PRO (Rigaku OD, 2018); program(s) used to solve structure: SHELXS97 (Sheldrick, 2008); program(s) used to refine structure: SHELXL97 (Sheldrick, 2008); molecular graphics: ORTEP-3 for Windows (Farrugia, 2012) and Mercury (Macrae et al., 2008); software used to prepare material for publication: OLEX2 (Dolomanov et al., 2009).

Tetraaqua[2,6-diacetylpyridine bis(semicarbazone)]samarium(III) trinitrate top

Crystal data top

[Sm(C₁₁H₁₅N₇O₂)(H₂O)₄](NO₃)₃	F(000) = 1364
M_r = 685.74	D_x = 1.986 Mg m⁻³
Monoclinic, P2₁/c	Mo Kα radiation, λ = 0.71073 Å
a = 10.0164 (5) Å	Cell parameters from 23000 reflections
b = 22.7494 (3) Å	θ = 4.3–32.9°
c = 15.0848 (8) Å	µ = 2.66 mm⁻¹
β = 138.151 (10)°	T = 293 K
V = 2293.3 (3) Å³	Block, yellow
Z = 4	0.34 × 0.30 × 0.28 mm

Data collection top

Rigaku Oxford Diffraction Xcalibur Sapphire3 diffractometer	9028 independent reflections
Radiation source: fine-focus sealed tube	6975 reflections with I > 2σ(I)
Graphite monochromator	R_int = 0.097
Detector resolution: 16.1790 pixels mm^-1	θ_max = 37.4°, θ_min = 4.1°
ω scans	h = −15→15
Absorption correction: multi-scan (CrysAlis PRO; Rigaku OD, 2018)	k = −35→34
T_min = 0.580, T_max = 1.000	l = −23→23
123615 measured reflections

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)] = 0.049	Hydrogen site location: inferred from neighbouring sites
wR(F²) = 0.127	H-atom parameters constrained
S = 1.03	w = 1/[σ²(F_o²) + (0.0649P)² + 3.2075P] where P = (F_o² + 2F_c²)/3
9028 reflections	(Δ/σ)_max = 0.001
378 parameters	Δρ_max = 1.71 e Å⁻³
12 restraints	Δρ_min = −1.43 e Å⁻³

Special details top

Geometry. All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds 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 > 2sigma(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	Occ. (<1)
Sm1	0.43786 (2)	0.39014 (2)	0.21680 (2)	0.02632 (6)
O1	0.1686 (4)	0.33450 (12)	0.1319 (3)	0.0427 (6)
O2	0.2300 (4)	0.47121 (12)	0.0923 (3)	0.0427 (6)
O3	0.2453 (5)	0.37078 (16)	−0.0110 (3)	0.0520 (7)
H3A	0.1393	0.3921	−0.0633	0.078*
H3B	0.2007	0.3354	−0.0319	0.078*
O4	0.7198 (5)	0.43890 (15)	0.4159 (3)	0.0520 (7)
H4A	0.7277	0.4753	0.4004	0.078*
H4B	0.8312	0.4230	0.4514	0.078*
O5	0.5973 (5)	0.33437 (13)	0.4133 (3)	0.0497 (7)
H5A	0.5071	0.3152	0.4018	0.074*
H5B	0.6561	0.3581	0.4821	0.074*
O6	0.3400 (5)	0.43687 (15)	0.3072 (3)	0.0531 (8)
H6A	0.3160	0.4773	0.2902	0.080*
H6B	0.4425	0.4369	0.3999	0.080*
N1	0.0147 (6)	0.24779 (17)	0.0794 (5)	0.0550 (10)
H1A	−0.0845	0.2645	0.0564	0.066*
H1B	0.0166	0.2102	0.0742	0.066*
N2	0.3166 (5)	0.25034 (14)	0.1562 (4)	0.0428 (7)
H2	0.3179	0.2126	0.1530	0.051*
N3	0.4651 (5)	0.28430 (14)	0.1948 (3)	0.0381 (6)
N4	0.7029 (5)	0.36044 (15)	0.2395 (3)	0.0388 (6)
N5	0.5609 (5)	0.46636 (15)	0.1683 (4)	0.0411 (7)
N6	0.4595 (5)	0.51843 (15)	0.1209 (4)	0.0452 (8)
H6	0.5039	0.5498	0.1178	0.054*
N7	0.1732 (6)	0.56525 (16)	0.0225 (4)	0.0510 (9)
H7A	0.0595	0.5665	−0.0071	0.061*
H7B	0.2161	0.5956	0.0155	0.061*
C1	0.1656 (6)	0.28011 (16)	0.1229 (4)	0.0380 (7)
C2	0.6125 (7)	0.26076 (18)	0.2265 (4)	0.0421 (8)
C3	0.6383 (10)	0.1961 (2)	0.2250 (7)	0.0695 (16)
H3C	0.7503	0.1823	0.3144	0.104*
H3D	0.6616	0.1886	0.1747	0.104*
H3E	0.5194	0.1759	0.1848	0.104*
C4	0.7537 (6)	0.30343 (19)	0.2572 (4)	0.0408 (8)
C5	0.9236 (7)	0.2862 (2)	0.2931 (5)	0.0538 (11)
H5	0.9588	0.2467	0.3063	0.065*
C6	1.0377 (8)	0.3290 (3)	0.3083 (6)	0.0609 (13)
H6C	1.1538	0.3186	0.3355	0.073*
C7	0.9796 (8)	0.3867 (2)	0.2833 (6)	0.0542 (12)
H7	1.0520	0.4156	0.2895	0.065*
C8	0.8098 (6)	0.4013 (2)	0.2484 (4)	0.0413 (8)
C9	0.7288 (6)	0.46160 (19)	0.2099 (4)	0.0411 (8)
C10	0.8339 (8)	0.5109 (2)	0.2159 (6)	0.0581 (12)
H10A	0.7642	0.5470	0.1925	0.087*
H10B	0.8367	0.5034	0.1547	0.087*
H10C	0.9684	0.5139	0.3043	0.087*
C11	0.2812 (6)	0.51712 (17)	0.0783 (4)	0.0395 (8)
O7	−0.1567 (6)	0.37785 (16)	−0.3329 (4)	0.0583 (9)
O8	−0.3794 (8)	0.4429 (3)	−0.4153 (4)	0.1019 (19)
O9	−0.1190 (6)	0.43889 (19)	−0.2064 (4)	0.0661 (10)
N8	−0.2184 (6)	0.41941 (17)	−0.3193 (4)	0.0478 (8)
O10	0.3359 (7)	0.6816 (2)	0.0444 (5)	0.0779 (12)
O11	0.5420 (7)	0.63334 (18)	0.0667 (5)	0.0734 (11)
O12	0.5472 (8)	0.72787 (19)	0.0658 (5)	0.0800 (13)
N9	0.4759 (6)	0.68165 (16)	0.0580 (4)	0.0472 (8)
N10	1.1785 (13)	0.4007 (4)	0.5921 (13)	0.057 (3)	0.549 (14)
O13	1.0404 (14)	0.3721 (4)	0.5584 (10)	0.081 (3)	0.549 (14)
O14	1.140 (2)	0.4516 (4)	0.5481 (15)	0.088 (5)	0.549 (14)
O15	1.3432 (14)	0.3775 (4)	0.6638 (14)	0.124 (6)	0.549 (14)
N10B	1.218 (2)	0.4132 (7)	0.583 (2)	0.079 (5)	0.451 (14)
O13B	1.172 (3)	0.3651 (5)	0.5935 (18)	0.118 (6)	0.451 (14)
O14B	1.385 (2)	0.4221 (7)	0.633 (2)	0.140 (8)	0.451 (14)
O15B	1.102 (3)	0.4556 (8)	0.532 (3)	0.118 (9)	0.451 (14)

Atomic displacement parameters (Å²) top

	U¹¹	U²²	U³³	U¹²	U¹³	U²³
Sm1	0.02879 (9)	0.02325 (9)	0.03029 (9)	0.00034 (5)	0.02301 (8)	0.00002 (5)
O1	0.0467 (15)	0.0318 (13)	0.0576 (17)	−0.0029 (11)	0.0412 (14)	−0.0039 (11)
O2	0.0433 (14)	0.0350 (13)	0.0496 (16)	0.0043 (11)	0.0346 (14)	0.0061 (11)
O3	0.0559 (18)	0.0561 (18)	0.0452 (16)	0.0046 (15)	0.0380 (16)	0.0020 (14)
O4	0.0573 (18)	0.0544 (18)	0.0499 (17)	−0.0153 (14)	0.0417 (16)	−0.0069 (14)
O5	0.068 (2)	0.0384 (15)	0.0420 (15)	−0.0060 (13)	0.0408 (16)	−0.0023 (12)
O6	0.064 (2)	0.0532 (18)	0.0533 (17)	0.0096 (15)	0.0470 (17)	0.0002 (14)
N1	0.052 (2)	0.0370 (18)	0.079 (3)	−0.0106 (15)	0.050 (2)	−0.0113 (17)
N2	0.0464 (18)	0.0312 (15)	0.0522 (19)	−0.0010 (13)	0.0371 (17)	−0.0042 (13)
N3	0.0413 (16)	0.0341 (15)	0.0409 (16)	0.0036 (12)	0.0312 (15)	0.0001 (12)
N4	0.0414 (16)	0.0418 (17)	0.0428 (16)	0.0025 (13)	0.0343 (15)	−0.0002 (13)
N5	0.0413 (16)	0.0389 (16)	0.0457 (17)	0.0035 (13)	0.0332 (15)	0.0058 (13)
N6	0.0455 (18)	0.0329 (16)	0.060 (2)	0.0027 (13)	0.0403 (18)	0.0087 (14)
N7	0.059 (2)	0.0358 (17)	0.068 (2)	0.0100 (15)	0.050 (2)	0.0116 (16)
C1	0.0399 (18)	0.0333 (17)	0.0417 (18)	−0.0013 (14)	0.0307 (17)	−0.0017 (14)
C2	0.050 (2)	0.0363 (18)	0.046 (2)	0.0067 (16)	0.0371 (19)	0.0014 (15)
C3	0.089 (4)	0.034 (2)	0.113 (5)	0.011 (2)	0.083 (4)	0.003 (3)
C4	0.0411 (19)	0.045 (2)	0.0402 (19)	0.0071 (15)	0.0313 (17)	0.0031 (15)
C5	0.049 (2)	0.057 (3)	0.062 (3)	0.012 (2)	0.043 (2)	0.003 (2)
C6	0.049 (2)	0.070 (3)	0.076 (3)	0.007 (2)	0.050 (3)	0.002 (3)
C7	0.042 (2)	0.068 (3)	0.061 (3)	0.0018 (19)	0.041 (2)	0.003 (2)
C8	0.0386 (19)	0.050 (2)	0.0419 (19)	0.0009 (16)	0.0320 (18)	0.0024 (16)
C9	0.0390 (19)	0.047 (2)	0.0412 (19)	−0.0019 (15)	0.0312 (17)	0.0029 (15)
C10	0.057 (3)	0.058 (3)	0.077 (3)	−0.005 (2)	0.055 (3)	0.004 (2)
C11	0.0425 (19)	0.0373 (18)	0.0403 (18)	0.0044 (15)	0.0313 (17)	0.0054 (14)
O7	0.070 (2)	0.0537 (18)	0.060 (2)	0.0003 (17)	0.051 (2)	−0.0055 (16)
O8	0.098 (3)	0.119 (4)	0.050 (2)	0.053 (3)	0.043 (2)	0.016 (2)
O9	0.065 (2)	0.089 (3)	0.0483 (18)	−0.0188 (19)	0.0434 (18)	−0.0213 (18)
N8	0.055 (2)	0.047 (2)	0.0429 (18)	−0.0066 (16)	0.0369 (18)	−0.0027 (15)
O10	0.078 (3)	0.075 (3)	0.108 (4)	0.015 (2)	0.077 (3)	0.013 (2)
O11	0.114 (3)	0.050 (2)	0.102 (3)	0.015 (2)	0.094 (3)	0.009 (2)
O12	0.106 (3)	0.059 (2)	0.096 (3)	−0.015 (2)	0.081 (3)	−0.005 (2)
N9	0.056 (2)	0.0414 (18)	0.0499 (19)	0.0048 (15)	0.0409 (18)	0.0029 (14)
N10	0.054 (5)	0.038 (6)	0.046 (4)	0.018 (4)	0.027 (4)	0.000 (4)
O13	0.060 (5)	0.047 (4)	0.100 (7)	0.000 (4)	0.049 (5)	0.017 (4)
O14	0.072 (6)	0.019 (4)	0.090 (7)	−0.004 (3)	0.036 (5)	0.003 (4)
O15	0.057 (6)	0.062 (6)	0.185 (13)	0.017 (4)	0.070 (7)	0.018 (6)
N10B	0.098 (12)	0.056 (9)	0.096 (11)	0.009 (9)	0.076 (10)	−0.003 (8)
O13B	0.121 (15)	0.040 (6)	0.181 (16)	0.022 (7)	0.109 (13)	0.031 (7)
O14B	0.095 (9)	0.117 (14)	0.206 (19)	−0.033 (9)	0.111 (12)	−0.052 (12)
O15B	0.132 (15)	0.092 (12)	0.19 (2)	0.034 (10)	0.140 (17)	0.042 (12)

Geometric parameters (Å, º) top

Sm1—O1	2.317 (3)	N7—C11	1.312 (5)
Sm1—O2	2.332 (3)	N7—H7A	0.8600
Sm1—O4	2.364 (3)	N7—H7B	0.8600
Sm1—O3	2.418 (3)	C2—C4	1.476 (6)
Sm1—O5	2.427 (3)	C2—C3	1.497 (6)
Sm1—O6	2.438 (3)	C3—H3C	0.9600
Sm1—N3	2.473 (3)	C3—H3D	0.9600
Sm1—N4	2.504 (3)	C3—H3E	0.9600
Sm1—N5	2.530 (3)	C4—C5	1.404 (6)
O1—C1	1.243 (4)	C5—C6	1.385 (8)
O2—C11	1.249 (5)	C5—H5	0.9300
O3—H3A	0.8584	C6—C7	1.371 (7)
O3—H3B	0.8585	C6—H6C	0.9300
O4—H4A	0.8808	C7—C8	1.395 (6)
O4—H4B	0.8797	C7—H7	0.9300
O5—H5A	0.8970	C8—C9	1.476 (6)
O5—H5B	0.8972	C9—C10	1.494 (6)
O6—H6A	0.9362	C10—H10A	0.9600
O6—H6B	0.9325	C10—H10B	0.9600
N1—C1	1.333 (5)	C10—H10C	0.9600
N1—H1A	0.8600	O7—N8	1.228 (5)
N1—H1B	0.8600	O8—N8	1.227 (6)
N2—N3	1.363 (5)	O9—N8	1.250 (5)
N2—C1	1.367 (5)	O10—N9	1.257 (6)
N2—H2	0.8600	O11—N9	1.238 (5)
N3—C2	1.282 (5)	O12—N9	1.226 (6)
N4—C4	1.345 (5)	N10—O15	1.229 (8)
N4—C8	1.347 (5)	N10—O13	1.243 (9)
N5—C9	1.290 (5)	N10—O14	1.247 (9)
N5—N6	1.365 (5)	N10B—O14B	1.234 (10)
N6—C11	1.376 (5)	N10B—O13B	1.242 (10)
N6—H6	0.8600	N10B—O15B	1.243 (10)

O1—Sm1—O2	90.78 (10)	C8—N4—Sm1	120.7 (3)
O1—Sm1—O4	139.06 (11)	C9—N5—N6	121.3 (4)
O2—Sm1—O4	99.03 (12)	C9—N5—Sm1	122.8 (3)
O1—Sm1—O3	75.33 (12)	N6—N5—Sm1	114.5 (3)
O2—Sm1—O3	73.21 (12)	N5—N6—C11	115.2 (3)
O4—Sm1—O3	145.52 (12)	N5—N6—H6	122.4
O1—Sm1—O5	79.97 (11)	C11—N6—H6	122.4
O2—Sm1—O5	141.02 (11)	C11—N7—H7A	120.0
O4—Sm1—O5	67.49 (11)	C11—N7—H7B	120.0
O3—Sm1—O5	137.95 (11)	H7A—N7—H7B	120.0
O1—Sm1—O6	76.13 (11)	O1—C1—N1	122.0 (4)
O2—Sm1—O6	67.41 (12)	O1—C1—N2	121.5 (4)
O4—Sm1—O6	71.45 (12)	N1—C1—N2	116.5 (3)
O3—Sm1—O6	130.31 (12)	N3—C2—C4	114.2 (4)
O5—Sm1—O6	73.61 (12)	N3—C2—C3	124.6 (4)
O1—Sm1—N3	66.00 (11)	C4—C2—C3	121.0 (4)
O2—Sm1—N3	141.57 (11)	C2—C3—H3C	109.5
O4—Sm1—N3	118.73 (12)	C2—C3—H3D	109.5
O3—Sm1—N3	71.51 (12)	H3C—C3—H3D	109.5
O5—Sm1—N3	67.49 (11)	C2—C3—H3E	109.5
O6—Sm1—N3	129.07 (12)	H3C—C3—H3E	109.5
O1—Sm1—N4	127.38 (10)	H3D—C3—H3E	109.5
O2—Sm1—N4	122.90 (11)	N4—C4—C5	121.1 (4)
O4—Sm1—N4	79.15 (12)	N4—C4—C2	116.1 (3)
O3—Sm1—N4	77.72 (12)	C5—C4—C2	122.6 (4)
O5—Sm1—N4	91.48 (12)	C6—C5—C4	118.8 (4)
O6—Sm1—N4	150.29 (12)	C6—C5—H5	120.6
N3—Sm1—N4	62.86 (11)	C4—C5—H5	120.6
O1—Sm1—N5	146.23 (11)	C7—C6—C5	120.0 (5)
O2—Sm1—N5	63.90 (11)	C7—C6—H6C	120.0
O4—Sm1—N5	70.59 (12)	C5—C6—H6C	120.0
O3—Sm1—N5	76.05 (12)	C6—C7—C8	118.6 (5)
O5—Sm1—N5	133.78 (11)	C6—C7—H7	120.7
O6—Sm1—N5	110.36 (12)	C8—C7—H7	120.7
N3—Sm1—N5	120.15 (12)	N4—C8—C7	122.0 (4)
N4—Sm1—N5	61.93 (11)	N4—C8—C9	116.0 (4)
C1—O1—Sm1	121.9 (3)	C7—C8—C9	121.9 (4)
C11—O2—Sm1	124.4 (3)	N5—C9—C8	113.9 (4)
Sm1—O3—H3A	109.6	N5—C9—C10	124.9 (4)
Sm1—O3—H3B	109.8	C8—C9—C10	121.2 (4)
H3A—O3—H3B	104.1	C9—C10—H10A	109.5
Sm1—O4—H4A	111.3	C9—C10—H10B	109.5
Sm1—O4—H4B	110.7	H10A—C10—H10B	109.5
H4A—O4—H4B	103.0	C9—C10—H10C	109.5
Sm1—O5—H5A	111.6	H10A—C10—H10C	109.5
Sm1—O5—H5B	111.5	H10B—C10—H10C	109.5
H5A—O5—H5B	102.4	O2—C11—N7	124.0 (4)
Sm1—O6—H6A	113.8	O2—C11—N6	119.5 (4)
Sm1—O6—H6B	112.7	N7—C11—N6	116.4 (4)
H6A—O6—H6B	100.4	O8—N8—O7	121.4 (4)
C1—N1—H1A	120.0	O8—N8—O9	117.8 (5)
C1—N1—H1B	120.0	O7—N8—O9	120.8 (4)
H1A—N1—H1B	120.0	O12—N9—O11	121.7 (5)
N3—N2—C1	115.7 (3)	O12—N9—O10	121.0 (4)
N3—N2—H2	122.2	O11—N9—O10	117.3 (4)
C1—N2—H2	122.2	O15—N10—O13	119.4 (10)
C2—N3—N2	120.6 (3)	O15—N10—O14	123.1 (11)
C2—N3—Sm1	124.6 (3)	O13—N10—O14	117.5 (9)
N2—N3—Sm1	114.5 (2)	O14B—N10B—O13B	122.0 (13)
C4—N4—C8	119.4 (4)	O14B—N10B—O15B	117.9 (13)
C4—N4—Sm1	119.5 (3)	O13B—N10B—O15B	119.7 (13)

C1—N2—N3—C2	−179.1 (4)	C2—C4—C5—C6	174.1 (5)
C1—N2—N3—Sm1	6.2 (4)	C4—C5—C6—C7	−2.6 (8)
C9—N5—N6—C11	179.2 (4)	C5—C6—C7—C8	2.8 (9)
Sm1—N5—N6—C11	−14.3 (5)	C4—N4—C8—C7	−3.9 (6)
Sm1—O1—C1—N1	177.1 (3)	Sm1—N4—C8—C7	169.0 (4)
Sm1—O1—C1—N2	−3.5 (5)	C4—N4—C8—C9	172.0 (4)
N3—N2—C1—O1	−2.2 (6)	Sm1—N4—C8—C9	−15.2 (5)
N3—N2—C1—N1	177.1 (4)	C6—C7—C8—N4	0.4 (8)
N2—N3—C2—C4	176.1 (4)	C6—C7—C8—C9	−175.2 (5)
Sm1—N3—C2—C4	−9.9 (5)	N6—N5—C9—C8	−175.8 (4)
N2—N3—C2—C3	0.1 (7)	Sm1—N5—C9—C8	18.9 (5)
Sm1—N3—C2—C3	174.1 (4)	N6—N5—C9—C10	2.2 (7)
C8—N4—C4—C5	4.0 (6)	Sm1—N5—C9—C10	−163.2 (4)
Sm1—N4—C4—C5	−168.9 (3)	N4—C8—C9—N5	−2.2 (6)
C8—N4—C4—C2	−171.2 (4)	C7—C8—C9—N5	173.7 (4)
Sm1—N4—C4—C2	15.8 (5)	N4—C8—C9—C10	179.8 (4)
N3—C2—C4—N4	−4.3 (5)	C7—C8—C9—C10	−4.4 (7)
C3—C2—C4—N4	171.9 (4)	Sm1—O2—C11—N7	−171.0 (3)
N3—C2—C4—C5	−179.5 (4)	Sm1—O2—C11—N6	10.1 (6)
C3—C2—C4—C5	−3.3 (7)	N5—N6—C11—O2	4.2 (6)
N4—C4—C5—C6	−0.8 (7)	N5—N6—C11—N7	−174.8 (4)

Hydrogen-bond geometry (Å, º) top

D—H···A	D—H	H···A	D···A	D—H···A
O3—H3A···O9	0.86	2.04	2.895 (6)	173
O4—H4B···O14	0.88	2.33	3.050 (15)	139
O4—H4B···O13	0.88	1.82	2.638 (11)	155
O4—H4B···O15B	0.88	2.11	2.805 (19)	135
O4—H4B···N10	0.88	2.42	3.278 (9)	164
O4—H4A···O14ⁱ	0.88	1.89	2.706 (9)	153
O4—H4A···O15Bⁱ	0.88	1.96	2.735 (19)	147
O4—H4A···O14Bⁱ	0.88	2.47	3.239 (17)	146
O4—H4A···N10Bⁱ	0.88	2.57	3.420 (15)	164
O5—H5A···O12ⁱⁱ	0.90	2.21	2.957 (6)	141
O5—H5B···O7ⁱⁱⁱ	0.90	1.93	2.767 (5)	155
O5—H5B···N8ⁱⁱⁱ	0.90	2.63	3.511 (5)	170
O5—H5B···O8ⁱⁱⁱ	0.90	2.66	3.455 (6)	149
O6—H6A···O8^iv	0.94	2.34	3.055 (6)	133
O6—H6A···O9^iv	0.94	2.33	3.192 (6)	154
O6—H6B···O8ⁱⁱⁱ	0.93	1.89	2.812 (6)	171
N1—H1A···O10^iv	0.86	2.11	2.938 (6)	162
N1—H1B···O13^v	0.86	1.93	2.780 (8)	173
N1—H1B···O13B^v	0.86	2.18	2.936 (13)	146
N2—H2···O15^v	0.86	2.06	2.914 (11)	175
N2—H2···O13B^v	0.86	2.03	2.801 (13)	149
O3—H3A···O2	0.86	2.53	2.833 (5)	102
O3—H3B···N3	0.86	2.56	2.858 (5)	101
O4—H4A···N5	0.88	2.52	2.831 (5)	101
N6—H6···O11	0.86	2.19	3.031 (5)	166
N7—H7A···O2^iv	0.86	2.29	3.095 (5)	156
N7—H7B···O10	0.86	2.16	2.995 (6)	163

Symmetry codes: (i) −x+2, −y+1, −z+1; (ii) −x+1, y−1/2, −z+1/2; (iii) x+1, y, z+1; (iv) −x, −y+1, −z; (v) x−1, −y+1/2, z−1/2.

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Tetra­aqua­[2,6-di­acetyl­pyridine bis­(semi­carbazone)]samarium(III) trinitrate

Supporting information

Key indicators

checkCIF/PLATON results

Tetraaqua[2,6-diacetylpyridine bis(semicarbazone)]samarium(III) trinitrate