Comprehensive structural study of lanthanide(III) chloride hydrates: [RECl₃·xH₂O (RE = La–Nd, Sm–Lu; x = 6, 7)]

A comprehensive crystallographic study is presented of the complete series of rare-earth(III) chloride hydrates. Early lanthanides form dimeric [(H₂O)₇RE(μ-Cl)₂RE(H₂O)₇]⁴⁺ binuclear complexes in which each RE atom (RE = La³⁺, Ce³⁺) is coordinated by seven H₂O mol­ecules and two bridging inner-sphere chloride ions. Di-μ-chlorido-bis­[hepta­aqua­lanthanide(III)] tetra­chloride, [(H₂O)₇RE(μ-Cl)₂RE(H₂O)₇]Cl₄, crystallizes in the triclinic space group P1. Heavier lanthanides exhibit monomeric [RECl₂(H₂O)₆]⁺ units where each RE atom (RE = Pr³⁺, Nd³⁺, Sm³⁺–Lu³⁺) is coordinated by six H₂O mol­ecules and two inner-sphere chloride ions. Hexa­aqua­dichlorido­lanthanide(III) chlorides, [RECl₂(H₂O)₆]Cl, adopt the monoclinic space group P2/c. In both structures, the cationic inner-sphere complex is counter-charged by the corresponding number of outer-sphere Cl⁻ anions, in which the metal ion and outer-sphere chloride ion lie on crystallographic twofold axes. Crystal structures for all compounds were determined in high quality with refined H-atom positions and were collected at the same temperature (100 K), providing a uniform structural dataset and addressing discrepancies in previous reports. The crystal structure of [HoCl₂(H₂O)₆]Cl is reported for the first time.

1. Chemical context and database survey

The rare-earth trivalent metal chloride hydrates [RECl₃·xH₂O (RE = La–Nd, Sm–Lu; x = 6, 7)] are commonly used as precursors in the synthesis of complex inorganic and organometallic compounds (Boyle & Steele, 2011). Most lanthanides are characterized by the presence of partially filled 4f orbitals, which significantly influence the chemical and physical properties of these elements and their compounds, offering a broad landscape for potential applications. For instance, lanthanide chloride salts possess catalytic (Narasimhulu et al., 2007), luminescent (Hsieh et al., 2013), scintillation (Boatner et al., 2013), and magnetic properties (Layfield & Murugesu, 2015), to name a few. The compositional and structural aspects of the lanthanide (III) chloride hydrate chemistry are well established, with nearly the entire series of RECl₃·xH₂O compositions identified (Boyle et al., 2010; Cotton & Harrowfield, 2011). However, our database survey indicates that while most of the compounds presented in this work are listed in the ICSD database (Release 2024.1; Zagorac et al., 2019), structural data for HoCl₃·6H₂O and TmCl₃·6H₂O are missing from the ICSD, and for HoCl₃·6H₂O, from the CSD (Release 2024.2; Groom et al., 2016) databases (Bakakin et al., 1975; Bel'skii & Struchkov, 1965; Boyle et al., 2010; Habenschuss & Spedding, 1979, 1980a,b,c,d, 1978; Hsieh et al., 2013; Kepert et al., 1983; Knopf et al., 2015; Levason & Webster, 2002; Louer et al., 1989; Marezio et al., 1961; Narasimhulu et al., 2007; Peterson et al., 1979; Reuter et al., 1994; Reuter & Frenzen, 1994; Rheingold & King, 1989; Tambornino et al., 2014; Wegner et al., 2018; Chen et al., 1991).

In addition, most of the reported datasets are of standard quality, lacking refined hydrogen atoms, which complicates the unambiguous inter­pretation of hydrogen bonding and the crystal packing. Another inconsistency involves data collection temperatures, which vary across the series in the previous reports. This study presents a comprehensive crystallographic analysis by providing a uniform structural dataset for the complete series of rare-earth metal(III) chloride hydrates except for radioactive promethium.

2. Structural commentary

The rare-earth metal(III) chloride hydrates [RECl₃·xH₂O (RE = La–Nd, Sm–Lu; x = 6, 7)] adopt two different structure types, with the rare-earth metal being coordinated by seven (for RE = La, Ce) or six (for RE = Pr, Nd, Sm–Lu) water mol­ecules. The degree of hydration is likely influenced by steric effects and aligns well with the decreasing trend of the atomic radii within the lanthanide series (Fig. 5). Metal–ligand bond distances for the La and Ce phases are listed in Tables 1 and 2, respectively, and the metal–ligand distances for the hexa­hydrates are summarized in Table 3. The hydrogen-bond geometrical data for the complete series (La–Lu) are listed in Table 4 to 17.

Table 1
Selected bond lengths (Å) for La

La1—Cl1	2.9187 (5)	La1—O4	2.5873 (13)
La1—O1	2.5443 (13)	La1—O5	2.5233 (14)
La1—O2	2.5504 (13)	La1—O6	2.5413 (15)
La1—O3	2.5315 (13)	La1—O7	2.5643 (13)

Table 2
Selected bond lengths (Å) for Ce

Ce1—Cl1	2.8986 (2)	Ce1—O4	2.5580 (7)
Ce1—O1	2.5276 (7)	Ce1—O5	2.5018 (7)
Ce1—O2	2.5229 (7)	Ce1—O6	2.5214 (7)
Ce1—O3	2.5076 (8)	Ce1—O7	2.5397 (8)

Table 3
Bond distances (Å) for hexa­hydrates

RE	Cl1	O1	O2	O3
Pr	2.8314 (4)	2.4677 (13)	2.4818 (13)	2.4513 (12)
Nd	2.8145 (2)	2.4532 (7)	2.4629 (6)	2.4328 (7)
Sm	2.7906 (3)	2.4269 (8)	2.4349 (8)	2.4057 (8)
Eu	2.7788 (2)	2.4131 (7)	2.4206 (7)	2.3884 (7)
Gd	2.7699 (3)	2.4026 (9)	2.4101 (8)	2.3762 (8)
Tb	2.7617 (3)	2.3870 (9)	2.3940 (9)	2.3646 (9)
Dy	2.7500 (2)	2.3735 (8)	2.3795 (8)	2.3480 (8)
Ho	2.7425 (3)	2.3646 (10)	2.3705 (9)	2.3372 (9)
Er	2.7309 (3)	2.3538 (9)	2.3578 (9)	2.3239 (9)
Tm	2.7246 (2)	2.3414 (7)	2.3446 (8)	2.3142 (7)
Yb	2.7173 (3)	2.3293 (8)	2.3328 (8)	2.3003 (8)
Lu	2.7113 (4)	2.3246 (11)	2.3272 (12)	2.2917 (12)

Table 4
Hydrogen-bond geometry (Å, °) for La

D—H⋯A	D—H	H⋯A	D⋯A	D—H⋯A
O1—H1A⋯Cl3^i	0.75 (3)	2.48 (3)	3.1947 (15)	161 (3)
O1—H1B⋯Cl2	0.79 (3)	2.38 (3)	3.1365 (16)	161 (2)
O2—H2A⋯Cl2^ii	0.80 (3)	2.38 (3)	3.1378 (14)	157 (3)
O2—H2B⋯Cl2^iii	0.79 (3)	2.26 (3)	3.0382 (13)	172 (3)
O3—H3A⋯Cl3	0.82 (3)	2.47 (3)	3.2552 (15)	160 (3)
O3—H3B⋯Cl1^i	0.78 (3)	2.92 (3)	3.2954 (13)	112 (2)
O3—H3B⋯Cl2	0.78 (3)	2.72 (3)	3.4160 (16)	150 (3)
O4—H4A⋯O2^iv	0.78 (3)	2.08 (3)	2.859 (2)	174 (3)
O4—H4B⋯Cl3	0.84 (3)	2.31 (3)	3.1488 (15)	179 (2)
O5—H5A⋯Cl3^v	0.80 (3)	2.34 (3)	3.1308 (14)	167 (3)
O5—H5B⋯Cl2^vi	0.75 (3)	2.44 (3)	3.1690 (15)	163 (3)
O5—H5B⋯O5^vi	0.75 (3)	2.67 (3)	2.986 (3)	108 (2)
O6—H6A⋯Cl3^vii	0.77 (3)	2.57 (3)	3.3288 (16)	168 (3)
O6—H6B⋯Cl1^viii	0.80 (3)	2.93 (3)	3.3705 (14)	117 (2)
O6—H6B⋯O4^ix	0.80 (3)	2.24 (3)	3.038 (2)	169 (3)
Symmetry codes: (i) ; (ii) ; (iii) ; (iv) ; (v) ; (vi) ; (vii) ; (viii) ; (ix) .

Table 5
Hydrogen-bond geometry (Å, °) for Ce

D—H⋯A	D—H	H⋯A	D⋯A	D—H⋯A
O1—H1A⋯Cl3^i	0.762 (19)	2.458 (19)	3.1945 (8)	162.9 (18)
O1—H1B⋯Cl2	0.77 (2)	2.405 (19)	3.1380 (8)	160.6 (17)
O2—H2A⋯Cl2^ii	0.797 (19)	2.251 (19)	3.0368 (8)	168.6 (17)
O2—H2B⋯Cl2^iii	0.783 (19)	2.411 (19)	3.1383 (8)	155.0 (16)
O3—H3A⋯Cl3	0.79 (2)	2.50 (2)	3.2501 (9)	160.9 (18)
O3—H3B⋯Cl1^i	0.80 (2)	2.91 (2)	3.3040 (8)	112.9 (16)
O3—H3B⋯Cl2	0.80 (2)	2.71 (2)	3.4188 (9)	147.3 (18)
O4—H4A⋯O2^iv	0.800 (17)	2.068 (17)	2.8609 (11)	171.2 (16)
O4—H4B⋯Cl3	0.781 (18)	2.369 (18)	3.1466 (8)	173.7 (16)
O5—H5A⋯Cl3^v	0.798 (17)	2.354 (17)	3.1286 (8)	164.0 (16)
O5—H5B⋯Cl2^vi	0.768 (19)	2.446 (19)	3.1699 (8)	157.6 (17)
O5—H5B⋯O5^vi	0.768 (19)	2.601 (17)	2.9858 (15)	112.9 (15)
O6—H6A⋯Cl1^vii	0.82 (2)	2.936 (18)	3.3662 (8)	115.2 (14)
O6—H6A⋯O4^viii	0.82 (2)	2.25 (2)	3.0451 (11)	164.9 (17)
O6—H6B⋯Cl3^ix	0.79 (2)	2.55 (2)	3.3165 (8)	164.4 (18)
Symmetry codes: (i) ; (ii) ; (iii) ; (iv) ; (v) ; (vi) ; (vii) ; (viii) ; (ix) .

Table 6
Hydrogen-bond geometry (Å, °) for Pr

D—H⋯A	D—H	H⋯A	D⋯A	D—H⋯A
O1—H1A⋯Cl1^i	0.75 (3)	2.42 (3)	3.1498 (14)	166 (3)
O1—H1B⋯Cl2^ii	0.78 (3)	2.40 (3)	3.1706 (13)	172 (2)
O2—H2A⋯Cl1^iii	0.76 (3)	2.40 (3)	3.1575 (13)	175 (2)
O2—H2B⋯Cl2^iv	0.77 (2)	2.49 (2)	3.2291 (14)	163 (2)
O3—H3A⋯Cl1^v	0.78 (3)	2.36 (3)	3.1303 (14)	174 (2)
O3—H3B⋯Cl2	0.80 (3)	2.41 (3)	3.1919 (14)	166 (2)
Symmetry codes: (i) ; (ii) ; (iii) ; (iv) ; (v) .

Table 7
Hydrogen-bond geometry (Å, °) for Nd

D—H⋯A	D—H	H⋯A	D⋯A	D—H⋯A
O1—H1A⋯Cl1^i	0.749 (16)	2.418 (16)	3.1491 (7)	165.6 (16)
O1—H1B⋯Cl2^ii	0.722 (17)	2.451 (18)	3.1661 (8)	170.8 (15)
O2—H2A⋯Cl1^iii	0.770 (18)	2.387 (18)	3.1552 (8)	175.3 (17)
O2—H2B⋯Cl2^iv	0.760 (17)	2.490 (17)	3.2267 (8)	164.0 (15)
O3—H3A⋯Cl1^v	0.793 (16)	2.337 (17)	3.1290 (7)	176.1 (15)
O3—H3B⋯Cl2	0.782 (16)	2.413 (16)	3.1894 (7)	172.0 (15)
Symmetry codes: (i) ; (ii) ; (iii) ; (iv) ; (v) .

Table 8
Hydrogen-bond geometry (Å, °) for Sm

D—H⋯A	D—H	H⋯A	D⋯A	D—H⋯A
O1—H1A⋯Cl1^i	0.693 (19)	2.484 (19)	3.1594 (10)	165 (2)
O1—H1B⋯Cl2^ii	0.79 (3)	2.39 (3)	3.1685 (9)	169.2 (19)
O2—H2A⋯Cl1^iii	0.81 (2)	2.35 (2)	3.1586 (9)	175.9 (18)
O2—H2B⋯Cl2^iv	0.78 (2)	2.48 (2)	3.2358 (10)	163.6 (17)
O3—H3A⋯Cl1^v	0.78 (2)	2.36 (2)	3.1367 (10)	176 (2)
O3—H3B⋯Cl2	0.794 (19)	2.41 (2)	3.1908 (9)	167.7 (18)
Symmetry codes: (i) ; (ii) ; (iii) ; (iv) ; (v) .

Table 9
Hydrogen-bond geometry (Å, °) for Eu

D—H⋯A	D—H	H⋯A	D⋯A	D—H⋯A
O1—H1A⋯Cl1^i	0.760 (15)	2.407 (15)	3.1537 (7)	167.5 (16)
O1—H1B⋯Cl2^ii	0.766 (19)	2.407 (19)	3.1649 (8)	170.6 (14)
O2—H2A⋯Cl1^iii	0.784 (16)	2.373 (17)	3.1549 (8)	175.1 (14)
O2—H2B⋯Cl2^iv	0.759 (16)	2.500 (15)	3.2308 (7)	162.1 (14)
O3—H3A⋯Cl1^v	0.783 (16)	2.349 (16)	3.1307 (7)	175.7 (14)
O3—H3B⋯Cl2	0.737 (15)	2.455 (15)	3.1842 (7)	170.3 (15)
Symmetry codes: (i) ; (ii) ; (iii) ; (iv) ; (v) .

Table 10
Hydrogen-bond geometry (Å, °) for Gd

D—H⋯A	D—H	H⋯A	D⋯A	D—H⋯A
O1—H1A⋯Cl1^i	0.79 (2)	2.39 (2)	3.1527 (9)	165 (2)
O1—H1B⋯Cl2^ii	0.75 (2)	2.43 (2)	3.1651 (9)	170.1 (19)
O2—H2A⋯Cl1^iii	0.80 (2)	2.36 (2)	3.1519 (9)	175 (2)
O2—H2B⋯Cl2^iv	0.82 (2)	2.44 (2)	3.2284 (9)	161.7 (18)
O3—H3A⋯Cl1^v	0.83 (2)	2.30 (2)	3.1290 (9)	178 (2)
O3—H3B⋯Cl2	0.79 (2)	2.40 (2)	3.1790 (9)	169.1 (19)
Symmetry codes: (i) ; (ii) ; (iii) ; (iv) ; (v) .

Table 11
Hydrogen-bond geometry (Å, °) for Tb

D—H⋯A	D—H	H⋯A	D⋯A	D—H⋯A
O1—H1A⋯Cl1^i	0.77 (2)	2.41 (2)	3.1527 (9)	164 (2)
O1—H1B⋯Cl2^ii	0.77 (2)	2.40 (2)	3.1661 (10)	172 (2)
O2—H2A⋯Cl1^iii	0.82 (2)	2.33 (2)	3.1524 (10)	175 (2)
O2—H2B⋯Cl2^iv	0.76 (2)	2.51 (2)	3.2283 (10)	158.8 (19)
O3—H3A⋯Cl1^v	0.81 (2)	2.33 (2)	3.1297 (10)	173.2 (19)
O3—H3B⋯Cl2	0.77 (2)	2.43 (2)	3.1798 (9)	166 (2)
Symmetry codes: (i) ; (ii) ; (iii) ; (iv) ; (v) .

Table 12
Hydrogen-bond geometry (Å, °) for Dy

D—H⋯A	D—H	H⋯A	D⋯A	D—H⋯A
O1—H1A⋯Cl1^i	0.755 (19)	2.413 (19)	3.1545 (9)	167.6 (19)
O1—H1B⋯Cl2^ii	0.78 (2)	2.39 (2)	3.1655 (8)	172.6 (16)
O2—H2A⋯Cl1^iii	0.79 (2)	2.37 (2)	3.1511 (9)	175.7 (19)
O2—H2B⋯Cl2^iv	0.712 (19)	2.544 (19)	3.2303 (8)	162.7 (19)
O3—H3A⋯Cl1^v	0.787 (19)	2.342 (19)	3.1276 (8)	176.2 (18)
O3—H3B⋯Cl2	0.75 (2)	2.44 (2)	3.1766 (8)	167.1 (19)
Symmetry codes: (i) ; (ii) ; (iii) ; (iv) ; (v) .

Table 13
Hydrogen-bond geometry (Å, °) for Ho

D—H⋯A	D—H	H⋯A	D⋯A	D—H⋯A
O1—H1A⋯Cl1^i	0.78 (2)	2.40 (2)	3.1589 (11)	166 (2)
O1—H1B⋯Cl2^ii	0.76 (2)	2.41 (2)	3.1678 (10)	170 (2)
O2—H2A⋯Cl1^iii	0.79 (2)	2.37 (2)	3.1546 (10)	172 (2)
O2—H2B⋯Cl2^iv	0.79 (2)	2.48 (2)	3.2320 (10)	161.6 (19)
O3—H3A⋯Cl1^v	0.79 (2)	2.35 (2)	3.1309 (10)	172 (2)
O3—H3B⋯Cl2	0.82 (2)	2.36 (2)	3.1765 (10)	168.9 (19)
Symmetry codes: (i) ; (ii) ; (iii) ; (iv) ; (v) .

Table 14
Hydrogen-bond geometry (Å, °) for Er

D—H⋯A	D—H	H⋯A	D⋯A	D—H⋯A
O1—H1A⋯Cl1^i	0.78 (2)	2.39 (2)	3.1557 (10)	166 (2)
O1—H1B⋯Cl2^ii	0.76 (3)	2.41 (3)	3.1632 (10)	170 (2)
O2—H2A⋯Cl1^iii	0.76 (2)	2.39 (2)	3.1502 (10)	176 (2)
O2—H2B⋯Cl2^iv	0.79 (2)	2.47 (2)	3.2287 (10)	161 (2)
O3—H3A⋯Cl1^v	0.77 (2)	2.36 (2)	3.1286 (10)	172 (2)
O3—H3B⋯Cl2	0.78 (2)	2.41 (2)	3.1689 (9)	167 (2)
Symmetry codes: (i) ; (ii) ; (iii) ; (iv) ; (v) .

Table 15
Hydrogen-bond geometry (Å, °) for Tm

D—H⋯A	D—H	H⋯A	D⋯A	D—H⋯A
O1—H1A⋯Cl1^i	0.73 (2)	2.44 (2)	3.1573 (8)	165 (2)
O1—H1B⋯Cl2^ii	0.81 (2)	2.36 (2)	3.1602 (8)	169.7 (16)
O2—H2A⋯Cl1^iii	0.78 (2)	2.38 (2)	3.1485 (8)	173.4 (19)
O2—H2B⋯Cl2^iv	0.737 (18)	2.528 (18)	3.2301 (8)	159.7 (18)
O3—H3A⋯Cl1^v	0.789 (19)	2.343 (19)	3.1280 (8)	173.4 (18)
O3—H3B⋯Cl2	0.75 (2)	2.43 (2)	3.1714 (8)	169.4 (17)
Symmetry codes: (i) ; (ii) ; (iii) ; (iv) ; (v) .

Table 16
Hydrogen-bond geometry (Å, °) for Yb

D—H⋯A	D—H	H⋯A	D⋯A	D—H⋯A
O1—H1A⋯Cl1^i	0.74 (2)	2.43 (2)	3.1570 (9)	168 (2)
O1—H1B⋯Cl2^ii	0.74 (2)	2.44 (2)	3.1623 (9)	167 (2)
O2—H2A⋯Cl1^iii	0.72 (2)	2.44 (2)	3.1486 (9)	175 (2)
O2—H2B⋯Cl2^iv	0.795 (19)	2.472 (19)	3.2287 (9)	159.5 (16)
O3—H3A⋯Cl1^v	0.720 (19)	2.409 (19)	3.1273 (9)	175.4 (19)
O3—H3B⋯Cl2	0.84 (2)	2.33 (2)	3.1643 (8)	168.8 (17)
Symmetry codes: (i) ; (ii) ; (iii) ; (iv) ; (v) .

Table 17
Hydrogen-bond geometry (Å, °) for Lu

D—H⋯A	D—H	H⋯A	D⋯A	D—H⋯A
O1—H1A⋯Cl1^i	0.77 (3)	2.42 (3)	3.1591 (13)	163 (3)
O1—H1B⋯Cl2^ii	0.76 (3)	2.40 (3)	3.1625 (12)	171 (2)
O2—H2A⋯Cl1^iii	0.73 (3)	2.42 (3)	3.1517 (13)	175 (3)
O2—H2B⋯Cl2^iv	0.82 (3)	2.45 (3)	3.2327 (13)	160 (3)
O3—H3A⋯Cl1^v	0.79 (3)	2.34 (3)	3.1290 (13)	174 (3)
O3—H3B⋯Cl2	0.77 (3)	2.41 (3)	3.1653 (12)	167 (3)
Symmetry codes: (i) ; (ii) ; (iii) ; (iv) ; (v) .

The early rare-earth metal (RE = La–Pr) chloride hydrates adopt the [LaCl₃(H₂O)₇] structure type and crystallize in the triclinic space group P, although there are a few reports on RECl₃(H₂O)₃ trihydrates (RE = La, Ce) crystallizing in the hexa­gonal space group P2m or the ortho­rhom­bic space group Pnma (Reuter et al., 1994; Reuter & Frenzen, 1994). This structure type is characterized by the Wyckoff sequence i¹¹ (excluding H atoms) and the Pearson Symbol aP50, with 11 atomic sites occupying general positions. The crystal structure of [RECl₃(H₂O)₇] (RE = La, Ce, Pr) is better described as a dimeric [(H₂O)₇RE(μ-Cl)₂RE(H₂O)₇]Cl₄ mol­ecule in which each RE atom is coordinated by seven water mol­ecules and the two lanthanide ions are linked by the two inner-sphere bridging chloride (μ-Cl) anions (Fig. 1). This complex [(H₂O)₇RE(μ-Cl)₂RE(H₂O)₇]⁴⁺ inner-sphere cation is charge-balanced by four Cl⁻ anions located in the outer-sphere. While we identified the La- and Ce-bearing analogs, we did not find a Pr-containing compound within this structure type.

Figure 1 Mol­ecular structure of the dimeric [(H2O)7RE(μ-Cl)2RE(H2O)7]Cl4 compound (RE = La, Ce) with displacement ellipsoids drawn at 50% probability. Hydrogen bonds are shown as bold dashed lines. RE, Cl, O, and H atoms are represented in blue, green, red, and black, respectively. Symmetry code: (i) −x, −y, 1 − z.

Each unit cell consists of a single [(H₂O)₇RE(μ-Cl)₂RE(H₂O)₇]Cl₄ (RE = La, Ce) formula unit with [(H₂O)₇RE(μ-Cl)₂RE(H₂O)₇]⁴⁺ binuclear cations linked via O—H⋯Cl hydrogen bonds ranging in H⋯Cl length from ca. 2.25 Å to 2.51 Å. Two outer-sphere Cl atoms link neighboring cations via these hydrogen bonds (Fig. 2).

Figure 2 Schematic view of the packing diagram for the dimeric [(H2O)7RE(μ-Cl)2RE(H2O)7]Cl4 compound (RE = La, Ce). Hydrogen bonds are shown as bold dashed lines, and the unit cell is outlined. RE, Cl, O, and H atoms are represented in blue, green, red, and black, respectively.

The heavier lanthanides (RE = Pr, Nd, Sm–Lu) crystallize in the monoclinic crystal system with the space group P2/c (note that most of the datasets were previously reported in the unconventional space group P2/n). They adopt the GdCl₃·6H₂O structure type, characterized by the Wyckoff sequence g⁴fe (excluding H atoms) and Pearson Symbol mP44. Each RECl₃·6H₂O formula unit consists of an [RECl₂(H₂O)₆]⁺ inner-sphere monomeric cation charge-balanced by a Cl⁻ anion located in the outer-sphere (Fig. 3). The RE³⁺ cation is coordinated by six water mol­ecules and two chloride anions in distorted square anti­prism fashion and is positioned on a crystallographic twofold axis.

Figure 3 Mol­ecular structure of the RECl2(H2O)6Cl compound (RE = Pr, Nd, Sm–Lu) with displacement ellipsoids drawn at 50% probability. Hydrogen bonds are shown as bold dashed lines. RE, Cl, O, and H atoms are represented in blue, green, red, and black, respectively. Symmetry code: (i) 1 − x, y, 1/2 - z.

Each unit cell of the RECl₂(H₂O)₆Cl (RE = Pr, Nd, Sm–Lu) structure type contains two formula units, with [RECl₂(H₂O)₆]⁺ cations linked via O—H⋯Cl and O—H⋯O hydrogen bonds (Fig. 4). Each outer-sphere chloride ion accepts six O—H⋯Cl contacts (ca. 2.36–2.48 Å for the Ho-bearing structure), thus linking six neighboring cations. The inner sphere Cl atom forms three hydrogen O—H⋯Cl bonds (ca. 2.35–2.40 Å for the Ho-bearing structure), thus linking four [RECl₂(H₂O)₆]⁺ cations.

Figure 4 Schematic view of the packing diagram for the RECl2(H2O)6Cl compound (RE = Pr, Nd, Sm–Lu). Hydrogen bonds are shown as bold dashed lines, and the unit cell is outlined. RE, Cl, O, and H atoms are represented in blue, green, red, and black, respectively.

An analysis of unit-cell volumes across the La–Lu series indicates a gradual decrease (Fig. 5), which is expected due to the decreasing trend for atomic radii of the lanthanides. This reduction in atomic size for heavier RE leads to smaller unit cell volumes in their crystal structures. The notably larger unit-cell volumes of the La- and Ce-bearing compounds are explained by the higher number of coordinated water mol­ecules and different structural arrangements. The variations of other parameters are shown in Fig. 6.

Figure 5 Variation of unit-cell volumes for RECl3·xH2O (RE = La–Nd, Sm–Lu; x = 6, 7) as determined from single-crystal X-ray diffraction experiments.

Figure 6 Variation of unit-cell parameters for RECl3·6H2O as determined from single-crystal X-ray diffraction experiments.

3. Synthesis and crystallization

Single-crystal X-ray diffraction (SCXRD) data collections were performed using commercially available chemicals supplied by Edgetech Industries LLC without further purification. However, large single crystals suitable for property measurements can also be obtained by recrystallization, as reported elsewhere (Chen et al., 1991, Peterson et al., 1979).

4. Refinement and Methodology

Crystal data are summarized in Table 18. SCXRD data were collected under a constant stream of cold nitro­gen gas to protect the crystals from air and moisture and to control the measurement temperature. After the structures were solved, the STRUCTURE TIDY (Gelato & Parthé, 1987) program was used to standardize the atomic coordinates, and the unit cell was transformed to the conventional monoclinic space group P2/c for the RECl₂(H₂O)₆Cl series.

Table 18
Experimental details

For all structures: Z = 2. Experiments were carried out at 100 K with Ag Kα radiation, λ = 0.56086 Å using a Bruker D8 Venture Duo. Absorption was corrected for by multi-scan methods (SADABS; Krause et al., 2016). All H-atom parameters were refined.

	[LaCl(H2O)7]Cl2	[CeCl(H2O)7]Cl2	[PrCl2(H2O)6]Cl
Crystal data
Mr	371.37	372.58	355.36
Crystal system, space group	Triclinic, P	Triclinic, P	Monoclinic, P2/c
a, b, c (Å)	7.9432 (5), 8.2316 (4), 9.2203 (5)	7.8995 (3), 8.2129 (3), 9.1961 (3)	7.9997 (3), 6.5647 (2), 12.1734 (4)
α, β, γ (°)	70.507 (2), 73.098 (2), 81.522 (2)	70.451 (1), 73.172 (1), 81.658 (1)	90, 127.388 (1), 90
V (Å^3)	542.92 (5)	537.39 (3)	507.95 (3)
μ (mm^−1)	2.42	2.60	2.90
Crystal size (mm)	0.28 × 0.12 × 0.06	0.26 × 0.22 × 0.17	0.06 × 0.06 × 0.05
Data collection
Tmin, Tmax	0.044, 0.064	0.214, 0.257	0.218, 0.257
No. of measured, independent and observed [I > 2σ(I)] reflections	43724, 3350, 3078	28063, 3304, 3239	15235, 1567, 1486
Rint	0.069	0.031	0.058
(sin θ/λ)max (Å^−1)	0.717	0.718	0.716
Refinement
R[F^2 > 2σ(F^2)], wR(F^2), S	0.016, 0.032, 1.01	0.009, 0.019, 1.17	0.014, 0.027, 1.05
No. of reflections	3350	3304	1567
No. of parameters	157	157	71
Δρmax, Δρmin (e Å^−3)	0.40, −0.44	0.32, −0.30	0.38, −0.39

	[NdCl2(H2O)6]Cl	[SmCl2(H2O)6]Cl	[EuCl2(H2O)6]Cl
Crystal data
Mr	358.69	364.80	366.41
Crystal system, space group	Monoclinic, P2/c	Monoclinic, P2/c	Monoclinic, P2/c
a, b, c (Å)	7.9710 (3), 6.5460 (2), 12.1246 (5)	7.9375 (8), 6.5351 (7), 12.0713 (11)	7.9062 (2), 6.5092 (2), 12.0410 (4)
α, β, γ (°)	90, 127.324 (1), 90	90, 127.217 (2), 90	90, 127.231 (1), 90
V (Å^3)	503.09 (3)	498.65 (9)	493.38 (3)
μ (mm^−1)	3.11	3.51	3.75
Crystal size (mm)	0.16 × 0.12 × 0.11	0.25 × 0.21 × 0.18	0.13 × 0.13 × 0.11
Data collection
Tmin, Tmax	0.201, 0.257	0.204, 0.257	0.218, 0.257
No. of measured, independent and observed [I > 2σ(I)] reflections	23233, 1559, 1536	27415, 1553, 1533	21905, 1529, 1504
Rint	0.036	0.046	0.038
(sin θ/λ)max (Å^−1)	0.716	0.717	0.716
Refinement
R[F^2 > 2σ(F^2)], wR(F^2), S	0.007, 0.017, 1.11	0.010, 0.023, 1.19	0.007, 0.016, 1.13
No. of reflections	1559	1553	1529
No. of parameters	72	72	72
Δρmax, Δρmin (e Å^−3)	0.25, −0.30	0.48, −0.85	0.29, −0.32

	[GdCl2(H2O)6]Cl	[TbCl2(H2O)6]Cl	[DyCl2(H2O)6]Cl
Crystal data
Mr	371.70	373.37	376.95
Crystal system, space group	Monoclinic, P2/c	Monoclinic, P2/c	Monoclinic, P2/c
a, b, c (Å)	7.8835 (3), 6.4964 (3), 12.0176 (4)	7.8646 (3), 6.4903 (3), 11.9871 (5)	7.8439 (3), 6.4693 (3), 11.9660 (5)
α, β, γ (°)	90, 127.186 (1), 90	90, 127.134 (1), 90	90, 127.143 (1), 90
V (Å^3)	490.33 (3)	487.79 (4)	484.02 (4)
μ (mm^−1)	3.99	4.24	4.51
Crystal size (mm)	0.33 × 0.25 × 0.20	0.3 × 0.16 × 0.12	0.23 × 0.19 × 0.14
Data collection
Tmin, Tmax	0.172, 0.257	0.223, 0.257	0.184, 0.257
No. of measured, independent and observed [I > 2σ(I)] reflections	26021, 1532, 1520	11117, 1503, 1481	21844, 1501, 1485
Rint	0.037	0.024	0.037
(sin θ/λ)max (Å^−1)	0.718	0.716	0.718
Refinement
R[F^2 > 2σ(F^2)], wR(F^2), S	0.009, 0.021, 1.23	0.009, 0.020, 1.10	0.008, 0.018, 1.19
No. of reflections	1532	1503	1501
No. of parameters	72	72	72
Δρmax, Δρmin (e Å^−3)	0.44, −0.38	0.36, −0.37	0.42, −0.48

	[HoCl2(H2O)6]Cl	[ErCl2(H2O)6]Cl	[TmCl2(H2O)6]Cl
Crystal data
Mr	379.38	381.71	383.38
Crystal system, space group	Monoclinic, P2/c	Monoclinic, P2/c	Monoclinic, P2/c
a, b, c (Å)	7.8303 (3), 6.4651 (2), 11.9509 (4)	7.8035 (2), 6.4488 (2), 11.9182 (4)	7.7889 (4), 6.4490 (3), 11.8760 (6)
α, β, γ (°)	90, 127.086 (1), 90	90, 127.044 (1), 90	90, 126.961 (1), 90
V (Å^3)	482.63 (3)	478.71 (3)	476.66 (4)
μ (mm^−1)	4.77	5.07	5.37
Crystal size (mm)	0.14 × 0.10 × 0.07	0.23 × 0.22 × 0.17	0.17 × 0.11 × 0.10
Data collection
Tmin, Tmax	0.222, 0.257	0.175, 0.257	0.207, 0.257
No. of measured, independent and observed [I > 2σ(I)] reflections	10309, 1480, 1454	24599, 1481, 1479	16364, 1481, 1464
Rint	0.026	0.034	0.033
(sin θ/λ)max (Å^−1)	0.715	0.717	0.717
Refinement
R[F^2 > 2σ(F^2)], wR(F^2), S	0.009, 0.020, 1.07	0.009, 0.020, 1.30	0.007, 0.016, 1.15
No. of reflections	1480	1481	1481
No. of parameters	72	72	72
Δρmax, Δρmin (e Å^−3)	0.31, −0.36	0.47, −0.88	0.39, −0.48

	[YbCl2(H2O)6]Cl	[LuCl2(H2O)6]Cl
Crystal data
Mr	387.49	389.42
Crystal system, space group	Monoclinic, P2/c	Monoclinic, P2/c
a, b, c (Å)	7.7666 (2), 6.4305 (2), 11.8745 (3)	7.7621 (3), 6.4241 (3), 11.8671 (5)
α, β, γ (°)	90, 126.991 (1), 90	90, 127.008 (1), 90
V (Å^3)	473.69 (2)	472.54 (4)
μ (mm^−1)	5.69	6.00
Crystal size (mm)	0.30 × 0.23 × 0.20	0.17 × 0.14 × 0.14
Data collection
Tmin, Tmax	0.168, 0.257	0.201, 0.257
No. of measured, independent and observed [I > 2σ(I)] reflections	19224, 1464, 1439	23799, 1464, 1436
Rint	0.035	0.041
(sin θ/λ)max (Å^−1)	0.717	0.718
Refinement
R[F^2 > 2σ(F^2)], wR(F^2), S	0.008, 0.017, 1.19	0.009, 0.020, 1.28
No. of reflections	1464	1464
No. of parameters	72	72
Δρmax, Δρmin (e Å^−3)	0.62, −0.74	0.78, −0.82
Computer programs: SAINT (Bruker, 2016), SHELXT2018/2 (Sheldrick, 2015a), SHELXL2018/1 (Sheldrick, 2015b), CrystalMaker (Palmer, 2014) and publCIF (Westrip, 2010).

Supporting information

Computing details

Di-µ-chlorido-bis[heptaaqualanthanum(III)] tetrachloride (La)

Crystal data

[LaCl(H2O)7]Cl2	Z = 2
Mr = 371.37	F(000) = 356
Triclinic, P1	Dx = 2.272 Mg m^−3
a = 7.9432 (5) Å	Ag Kα radiation, λ = 0.56086 Å
b = 8.2316 (4) Å	Cell parameters from 9869 reflections
c = 9.2203 (5) Å	θ = 2.4–23.7°
α = 70.507 (2)°	µ = 2.42 mm^−1
β = 73.098 (2)°	T = 100 K
γ = 81.522 (2)°	Plate, colorless
V = 542.92 (5) Å^3	0.28 × 0.12 × 0.06 mm

Data collection

Bruker D8 Venture Duo diffractometer	3078 reflections with I > 2σ(I)
ω scans	Rint = 0.069
Absorption correction: multi-scan SADABS-2016/2 (Bruker, 2016)	θmax = 23.7°, θmin = 2.1°
Tmin = 0.044, Tmax = 0.064	h = −11→11
43724 measured reflections	k = −11→11
3350 independent reflections	l = −13→13

Refinement

Refinement on F^2	Hydrogen site location: difference Fourier map
Least-squares matrix: full	All H-atom parameters refined
R[F^2 > 2σ(F^2)] = 0.016	w = 1/[σ^2(Fo^2) + (0.0128P)^2] where P = (Fo^2 + 2Fc^2)/3
wR(F^2) = 0.032	(Δ/σ)max = 0.001
S = 1.01	Δρmax = 0.40 e Å^−3
3350 reflections	Δρmin = −0.44 e Å^−3
157 parameters	Extinction correction: SHELXL-2018/1 (Sheldrick 2015b), Fc^*=kFc[1+0.001xFc^2λ^3/sin(2θ)]^-1/4
0 restraints	Extinction coefficient: 0.0070 (6)
Primary atom site location: dual

Special details

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.

Fractional atomic coordinates and isotropic or equivalent isotropic displacement parameters (Ų)

	x	y	z	Uiso*/Ueq
La1	0.21799 (2)	0.18615 (2)	0.32361 (2)	0.00928 (4)
Cl1	−0.14698 (6)	0.17974 (5)	0.51434 (5)	0.01189 (8)
Cl2	0.21093 (6)	0.77753 (5)	0.03491 (5)	0.01465 (8)
Cl3	0.34270 (6)	0.38778 (5)	0.71161 (5)	0.01506 (9)
O1	0.0304 (2)	0.42402 (17)	0.17472 (17)	0.0149 (3)
O2	0.07092 (19)	0.08113 (17)	0.16194 (16)	0.0148 (3)
O3	0.2234 (2)	0.46276 (18)	0.38494 (18)	0.0188 (3)
O4	0.2311 (2)	0.09299 (18)	0.61748 (16)	0.0153 (3)
O5	0.3868 (2)	0.35162 (17)	0.04773 (16)	0.0145 (3)
O6	0.5212 (2)	0.2280 (2)	0.34138 (17)	0.0173 (3)
O7	0.4532 (2)	−0.01065 (18)	0.19716 (17)	0.0164 (3)
H1A	−0.060 (4)	0.447 (3)	0.219 (3)	0.030 (7)*
H1B	0.077 (4)	0.509 (3)	0.119 (3)	0.028 (7)*
H2A	0.015 (4)	0.143 (3)	0.103 (3)	0.033 (7)*
H2B	0.116 (4)	0.003 (4)	0.131 (3)	0.035 (7)*
H3A	0.259 (4)	0.470 (4)	0.458 (3)	0.042 (8)*
H3B	0.199 (4)	0.553 (4)	0.330 (4)	0.051 (9)*
H4A	0.144 (4)	0.052 (3)	0.677 (3)	0.027 (7)*
H4B	0.261 (4)	0.171 (3)	0.644 (3)	0.030 (7)*
H5A	0.360 (4)	0.367 (4)	−0.033 (3)	0.038 (8)*
H5B	0.485 (4)	0.339 (4)	0.031 (4)	0.046 (9)*
H6A	0.549 (5)	0.312 (4)	0.344 (4)	0.059 (11)*
H6B	0.596 (4)	0.151 (4)	0.352 (3)	0.048 (9)*
H7A	0.535 (4)	0.031 (4)	0.131 (3)	0.036 (8)*
H7B	0.464 (5)	−0.115 (4)	0.228 (4)	0.057 (10)*

Atomic displacement parameters (Ų)

	U^11	U^22	U^33	U^12	U^13	U^23
La1	0.00924 (5)	0.00899 (5)	0.00984 (5)	−0.00066 (3)	−0.00284 (3)	−0.00281 (3)
Cl1	0.0113 (2)	0.01008 (16)	0.01293 (17)	−0.00054 (14)	−0.00208 (15)	−0.00269 (14)
Cl2	0.0132 (2)	0.01316 (18)	0.01800 (19)	−0.00013 (15)	−0.00398 (16)	−0.00561 (15)
Cl3	0.0163 (2)	0.01438 (18)	0.01599 (19)	0.00004 (16)	−0.00586 (17)	−0.00548 (15)
O1	0.0113 (7)	0.0128 (6)	0.0165 (6)	−0.0003 (5)	−0.0020 (5)	−0.0007 (5)
O2	0.0168 (7)	0.0134 (6)	0.0173 (6)	0.0035 (5)	−0.0082 (6)	−0.0072 (5)
O3	0.0242 (8)	0.0134 (6)	0.0228 (7)	0.0012 (6)	−0.0101 (6)	−0.0083 (6)
O4	0.0155 (7)	0.0178 (6)	0.0135 (6)	−0.0060 (5)	−0.0035 (6)	−0.0041 (5)
O5	0.0128 (7)	0.0175 (6)	0.0122 (6)	−0.0009 (5)	−0.0036 (5)	−0.0028 (5)
O6	0.0130 (7)	0.0187 (7)	0.0231 (7)	−0.0009 (6)	−0.0062 (6)	−0.0086 (6)
O7	0.0157 (8)	0.0126 (6)	0.0187 (7)	−0.0007 (5)	−0.0016 (6)	−0.0044 (5)

Geometric parameters (Å, º)

La1—Cl1^i	2.9376 (4)	O2—H2B	0.79 (3)
La1—Cl1	2.9187 (5)	O3—H3A	0.82 (3)
La1—O1	2.5443 (13)	O3—H3B	0.78 (3)
La1—O2	2.5504 (13)	O4—H4A	0.78 (3)
La1—O3	2.5315 (13)	O4—H4B	0.84 (3)
La1—O4	2.5873 (13)	O5—H5A	0.80 (3)
La1—O5	2.5233 (14)	O5—H5B	0.75 (3)
La1—O6	2.5413 (15)	O6—H6A	0.77 (3)
La1—O7	2.5643 (13)	O6—H6B	0.80 (3)
O1—H1A	0.75 (3)	O7—H7A	0.78 (3)
O1—H1B	0.79 (3)	O7—H7B	0.81 (3)
O2—H2A	0.80 (3)
Cl1—La1—Cl1^i	73.941 (12)	O6—La1—O1	123.86 (5)
O1—La1—Cl1^i	128.72 (4)	O6—La1—O2	141.04 (4)
O1—La1—Cl1	69.96 (4)	O6—La1—O4	69.20 (5)
O1—La1—O2	67.52 (4)	O6—La1—O7	69.14 (5)
O1—La1—O4	130.45 (4)	O7—La1—Cl1^i	68.54 (4)
O1—La1—O7	124.76 (4)	O7—La1—Cl1	139.55 (4)
O2—La1—Cl1	79.41 (3)	O7—La1—O4	104.74 (4)
O2—La1—Cl1^i	71.07 (3)	La1—Cl1—La1^i	106.059 (12)
O2—La1—O4	135.97 (5)	La1—O1—H1A	119 (2)
O2—La1—O7	74.71 (4)	La1—O1—H1B	117 (2)
O3—La1—Cl1^i	140.68 (4)	H1A—O1—H1B	109 (3)
O3—La1—Cl1	84.97 (4)	La1—O2—H2A	124.0 (19)
O3—La1—O1	70.08 (5)	La1—O2—H2B	119 (2)
O3—La1—O2	137.58 (4)	H2A—O2—H2B	110 (2)
O3—La1—O4	74.18 (5)	La1—O3—H3A	125.3 (19)
O3—La1—O6	68.30 (5)	La1—O3—H3B	123 (2)
O3—La1—O7	134.49 (5)	H3A—O3—H3B	112 (3)
O4—La1—Cl1^i	68.28 (3)	La1—O4—H4A	112.1 (19)
O4—La1—Cl1	73.83 (4)	La1—O4—H4B	114.3 (17)
O5—La1—Cl1	136.61 (3)	H4A—O4—H4B	112 (2)
O5—La1—Cl1^i	133.83 (3)	La1—O5—H5A	126 (2)
O5—La1—O1	66.80 (5)	La1—O5—H5B	116 (2)
O5—La1—O2	81.23 (5)	H5A—O5—H5B	108 (3)
O5—La1—O3	83.78 (5)	La1—O6—H6A	124 (3)
O5—La1—O4	140.90 (5)	La1—O6—H6B	123 (2)
O5—La1—O6	72.77 (5)	H6A—O6—H6B	112 (3)
O5—La1—O7	68.91 (5)	La1—O7—H7A	119 (2)
O6—La1—Cl1	138.86 (3)	La1—O7—H7B	128 (2)
O6—La1—Cl1^i	107.32 (4)	H7A—O7—H7B	113 (3)

Symmetry code: (i) −x, −y, −z+1.

Hydrogen-bond geometry (Å, º)

D—H···A	D—H	H···A	D···A	D—H···A
O1—H1A···Cl3^ii	0.75 (3)	2.48 (3)	3.1947 (15)	161 (3)
O1—H1B···Cl2	0.79 (3)	2.38 (3)	3.1365 (16)	161 (2)
O2—H2A···Cl2^iii	0.80 (3)	2.38 (3)	3.1378 (14)	157 (3)
O2—H2B···Cl2^iv	0.79 (3)	2.26 (3)	3.0382 (13)	172 (3)
O3—H3A···Cl3	0.82 (3)	2.47 (3)	3.2552 (15)	160 (3)
O3—H3B···Cl1^ii	0.78 (3)	2.92 (3)	3.2954 (13)	112 (2)
O3—H3B···Cl2	0.78 (3)	2.72 (3)	3.4160 (16)	150 (3)
O4—H4A···O2^i	0.78 (3)	2.08 (3)	2.859 (2)	174 (3)
O4—H4B···Cl3	0.84 (3)	2.31 (3)	3.1488 (15)	179 (2)
O5—H5A···Cl3^v	0.80 (3)	2.34 (3)	3.1308 (14)	167 (3)
O5—H5B···Cl2^vi	0.75 (3)	2.44 (3)	3.1690 (15)	163 (3)
O5—H5B···O5^vi	0.75 (3)	2.67 (3)	2.986 (3)	108 (2)
O6—H6A···Cl3^vii	0.77 (3)	2.57 (3)	3.3288 (16)	168 (3)
O6—H6B···Cl1^viii	0.80 (3)	2.93 (3)	3.3705 (14)	117 (2)
O6—H6B···O4^ix	0.80 (3)	2.24 (3)	3.038 (2)	169 (3)

Symmetry codes: (i) −x, −y, −z+1; (ii) −x, −y+1, −z+1; (iii) −x, −y+1, −z; (iv) x, y−1, z; (v) x, y, z−1; (vi) −x+1, −y+1, −z; (vii) −x+1, −y+1, −z+1; (viii) x+1, y, z; (ix) −x+1, −y, −z+1.

Di-µ-chlorido-bis[heptaaquacerium(III)] tetrachloride, (Ce)

Crystal data

[CeCl(H2O)7]Cl2	Z = 2
Mr = 372.58	F(000) = 358
Triclinic, P1	Dx = 2.303 Mg m^−3
a = 7.8995 (3) Å	Ag Kα radiation, λ = 0.56086 Å
b = 8.2129 (3) Å	Cell parameters from 9812 reflections
c = 9.1961 (3) Å	θ = 2.5–23.7°
α = 70.451 (1)°	µ = 2.60 mm^−1
β = 73.172 (1)°	T = 100 K
γ = 81.658 (1)°	Plate, colorless
V = 537.39 (3) Å^3	0.26 × 0.22 × 0.17 mm

Data collection

Bruker D8 Venture Duo diffractometer	3239 reflections with I > 2σ(I)
ω scans	Rint = 0.031
Absorption correction: multi-scan SADABS-2016/2 (Bruker, 2016)	θmax = 23.7°, θmin = 1.9°
Tmin = 0.214, Tmax = 0.257	h = −11→11
28063 measured reflections	k = −11→11
3304 independent reflections	l = −13→13

Refinement

Refinement on F^2	Hydrogen site location: difference Fourier map
Least-squares matrix: full	All H-atom parameters refined
R[F^2 > 2σ(F^2)] = 0.009	w = 1/[σ^2(Fo^2) + (0.0036P)^2 + 0.0733P] where P = (Fo^2 + 2Fc^2)/3
wR(F^2) = 0.019	(Δ/σ)max = 0.001
S = 1.17	Δρmax = 0.32 e Å^−3
3304 reflections	Δρmin = −0.29 e Å^−3
157 parameters	Extinction correction: SHELXL-2018/1 (Sheldrick 2015b), Fc^*=kFc[1+0.001xFc^2λ^3/sin(2θ)]^-1/4
0 restraints	Extinction coefficient: 0.0349 (8)
Primary atom site location: dual

Special details

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.

Fractional atomic coordinates and isotropic or equivalent isotropic displacement parameters (Ų)

	x	y	z	Uiso*/Ueq
Ce1	0.21779 (2)	0.18632 (2)	0.32382 (2)	0.00590 (2)
Cl1	−0.14612 (3)	0.17948 (3)	0.51435 (3)	0.00867 (4)
Cl2	0.21050 (3)	0.77796 (3)	0.03514 (3)	0.01125 (4)
Cl3	0.34287 (3)	0.38691 (3)	0.71200 (3)	0.01174 (4)
O1	0.03034 (11)	0.42224 (10)	0.17488 (9)	0.01184 (13)
O2	0.07253 (10)	0.08169 (10)	0.16291 (9)	0.01131 (13)
O3	0.22060 (11)	0.46047 (10)	0.38631 (10)	0.01504 (14)
O4	0.23110 (10)	0.09321 (10)	0.61518 (9)	0.01193 (13)
O5	0.38549 (10)	0.35125 (10)	0.04929 (8)	0.01117 (13)
O6	0.52006 (10)	0.22922 (11)	0.34141 (9)	0.01312 (14)
O7	0.45125 (10)	−0.00898 (10)	0.19850 (9)	0.01262 (14)
H1A	−0.062 (3)	0.449 (2)	0.218 (2)	0.034 (5)*
H1B	0.074 (2)	0.507 (2)	0.120 (2)	0.034 (5)*
H2A	0.122 (2)	0.003 (2)	0.132 (2)	0.034 (5)*
H2B	0.020 (2)	0.144 (2)	0.103 (2)	0.033 (4)*
H3A	0.251 (3)	0.468 (2)	0.458 (2)	0.042 (5)*
H3B	0.191 (3)	0.554 (3)	0.333 (2)	0.050 (6)*
H4A	0.142 (2)	0.055 (2)	0.6783 (19)	0.023 (4)*
H4B	0.255 (2)	0.162 (2)	0.6465 (19)	0.028 (4)*
H5A	0.353 (2)	0.362 (2)	−0.028 (2)	0.026 (4)*
H5B	0.487 (3)	0.348 (2)	0.027 (2)	0.034 (5)*
H6A	0.602 (3)	0.156 (2)	0.343 (2)	0.035 (5)*
H6B	0.553 (3)	0.312 (3)	0.347 (2)	0.044 (5)*
H7A	0.535 (2)	0.030 (2)	0.134 (2)	0.028 (4)*
H7B	0.472 (2)	−0.108 (3)	0.232 (2)	0.039 (5)*

Atomic displacement parameters (Ų)

	U^11	U^22	U^33	U^12	U^13	U^23
Ce1	0.00610 (3)	0.00554 (3)	0.00634 (3)	−0.00042 (2)	−0.00203 (2)	−0.00178 (2)
Cl1	0.00832 (9)	0.00669 (9)	0.00983 (9)	−0.00012 (7)	−0.00148 (7)	−0.00192 (7)
Cl2	0.01010 (10)	0.00970 (10)	0.01461 (10)	0.00029 (8)	−0.00330 (8)	−0.00484 (8)
Cl3	0.01327 (10)	0.01078 (10)	0.01287 (10)	0.00063 (8)	−0.00533 (8)	−0.00471 (8)
O1	0.0101 (3)	0.0093 (3)	0.0125 (3)	0.0001 (3)	−0.0021 (3)	0.0003 (3)
O2	0.0137 (3)	0.0101 (3)	0.0124 (3)	0.0033 (3)	−0.0068 (3)	−0.0051 (3)
O3	0.0198 (4)	0.0105 (3)	0.0190 (4)	0.0010 (3)	−0.0093 (3)	−0.0070 (3)
O4	0.0126 (3)	0.0141 (3)	0.0105 (3)	−0.0051 (3)	−0.0029 (3)	−0.0040 (3)
O5	0.0093 (3)	0.0133 (3)	0.0096 (3)	−0.0008 (3)	−0.0022 (3)	−0.0019 (3)
O6	0.0090 (3)	0.0151 (3)	0.0178 (3)	−0.0006 (3)	−0.0049 (3)	−0.0071 (3)
O7	0.0103 (3)	0.0086 (3)	0.0157 (3)	0.0003 (3)	0.0003 (3)	−0.0031 (3)

Geometric parameters (Å, º)

Ce1—Cl1^i	2.9282 (2)	O2—H2B	0.783 (19)
Ce1—Cl1	2.8986 (2)	O3—H3A	0.79 (2)
Ce1—O1	2.5276 (7)	O3—H3B	0.80 (2)
Ce1—O2	2.5229 (7)	O4—H4A	0.800 (17)
Ce1—O3	2.5076 (8)	O4—H4B	0.781 (18)
Ce1—O4	2.5580 (7)	O5—H5A	0.798 (17)
Ce1—O5	2.5018 (7)	O5—H5B	0.768 (19)
Ce1—O6	2.5214 (7)	O6—H6A	0.82 (2)
Ce1—O7	2.5397 (8)	O6—H6B	0.79 (2)
O1—H1A	0.762 (19)	O7—H7A	0.775 (18)
O1—H1B	0.77 (2)	O7—H7B	0.78 (2)
O2—H2A	0.797 (19)
Cl1—Ce1—Cl1^i	73.953 (7)	O6—Ce1—O1	123.87 (3)
O1—Ce1—Cl1^i	128.491 (19)	O6—Ce1—O2	140.89 (3)
O1—Ce1—Cl1	70.026 (19)	O6—Ce1—O4	69.23 (2)
O1—Ce1—O4	130.70 (2)	O6—Ce1—O7	69.36 (3)
O1—Ce1—O7	124.61 (3)	O7—Ce1—Cl1^i	68.459 (19)
O2—Ce1—Cl1	79.796 (18)	O7—Ce1—Cl1	139.540 (18)
O2—Ce1—Cl1^i	70.981 (18)	O7—Ce1—O4	104.66 (3)
O2—Ce1—O1	67.44 (2)	Ce1—Cl1—Ce1^i	106.047 (7)
O2—Ce1—O4	135.98 (2)	Ce1—O1—H1A	120.9 (13)
O2—Ce1—O7	74.40 (3)	Ce1—O1—H1B	117.9 (13)
O3—Ce1—Cl1^i	140.40 (2)	H1A—O1—H1B	105.8 (18)
O3—Ce1—Cl1	84.317 (19)	Ce1—O2—H2A	117.0 (13)
O3—Ce1—O1	70.16 (3)	Ce1—O2—H2B	123.0 (12)
O3—Ce1—O2	137.56 (3)	H2A—O2—H2B	111.1 (17)
O3—Ce1—O4	74.09 (3)	Ce1—O3—H3A	125.9 (14)
O3—Ce1—O6	68.59 (3)	Ce1—O3—H3B	122.9 (14)
O3—Ce1—O7	135.12 (3)	H3A—O3—H3B	111.1 (19)
O4—Ce1—Cl1^i	68.263 (18)	Ce1—O4—H4A	114.1 (11)
O4—Ce1—Cl1	73.723 (18)	Ce1—O4—H4B	117.9 (12)
O5—Ce1—Cl1	136.599 (19)	H4A—O4—H4B	104.8 (15)
O5—Ce1—Cl1^i	133.776 (18)	Ce1—O5—H5A	122.1 (12)
O5—Ce1—O1	66.70 (3)	Ce1—O5—H5B	120.1 (13)
O5—Ce1—O2	81.00 (2)	H5A—O5—H5B	108.9 (17)
O5—Ce1—O3	84.25 (3)	Ce1—O6—H6A	124.5 (12)
O5—Ce1—O4	141.04 (3)	Ce1—O6—H6B	127.8 (15)
O5—Ce1—O6	72.84 (2)	H6A—O6—H6B	107.7 (18)
O5—Ce1—O7	69.00 (3)	Ce1—O7—H7A	119.7 (12)
O6—Ce1—Cl1	138.654 (18)	Ce1—O7—H7B	129.6 (14)
O6—Ce1—Cl1^i	107.53 (2)	H7A—O7—H7B	107.2 (18)

Symmetry code: (i) −x, −y, −z+1.

Hydrogen-bond geometry (Å, º)

D—H···A	D—H	H···A	D···A	D—H···A
O1—H1A···Cl3^ii	0.762 (19)	2.458 (19)	3.1945 (8)	162.9 (18)
O1—H1B···Cl2	0.77 (2)	2.405 (19)	3.1380 (8)	160.6 (17)
O2—H2A···Cl2^iii	0.797 (19)	2.251 (19)	3.0368 (8)	168.6 (17)
O2—H2B···Cl2^iv	0.783 (19)	2.411 (19)	3.1383 (8)	155.0 (16)
O3—H3A···Cl3	0.79 (2)	2.50 (2)	3.2501 (9)	160.9 (18)
O3—H3B···Cl1^ii	0.80 (2)	2.91 (2)	3.3040 (8)	112.9 (16)
O3—H3B···Cl2	0.80 (2)	2.71 (2)	3.4188 (9)	147.3 (18)
O4—H4A···O2^i	0.800 (17)	2.068 (17)	2.8609 (11)	171.2 (16)
O4—H4B···Cl3	0.781 (18)	2.369 (18)	3.1466 (8)	173.7 (16)
O5—H5A···Cl3^v	0.798 (17)	2.354 (17)	3.1286 (8)	164.0 (16)
O5—H5B···Cl2^vi	0.768 (19)	2.446 (19)	3.1699 (8)	157.6 (17)
O5—H5B···O5^vi	0.768 (19)	2.601 (17)	2.9858 (15)	112.9 (15)
O6—H6A···Cl1^vii	0.82 (2)	2.936 (18)	3.3662 (8)	115.2 (14)
O6—H6A···O4^viii	0.82 (2)	2.25 (2)	3.0451 (11)	164.9 (17)
O6—H6B···Cl3^ix	0.79 (2)	2.55 (2)	3.3165 (8)	164.4 (18)

Symmetry codes: (i) −x, −y, −z+1; (ii) −x, −y+1, −z+1; (iii) x, y−1, z; (iv) −x, −y+1, −z; (v) x, y, z−1; (vi) −x+1, −y+1, −z; (vii) x+1, y, z; (viii) −x+1, −y, −z+1; (ix) −x+1, −y+1, −z+1.

Hexaaquadichloridoprotactinium(III) chloride (Pr)

Crystal data

[PrCl2(H2O)6]Cl	F(000) = 340
Mr = 355.36	Dx = 2.323 Mg m^−3
Monoclinic, P2/c	Ag Kα radiation, λ = 0.56086 Å
a = 7.9997 (3) Å	Cell parameters from 6065 reflections
b = 6.5647 (2) Å	θ = 2.5–23.7°
c = 12.1734 (4) Å	µ = 2.90 mm^−1
β = 127.388 (1)°	T = 100 K
V = 507.95 (3) Å^3	Plate, green
Z = 2	0.06 × 0.06 × 0.05 mm

Data collection

Bruker D8 Venture Duo diffractometer	1486 reflections with I > 2σ(I)
ω scans	Rint = 0.058
Absorption correction: multi-scan SADABS-2016/2 (Bruker, 2016)	θmax = 23.7°, θmin = 2.5°
Tmin = 0.218, Tmax = 0.257	h = −11→11
15235 measured reflections	k = −9→9
1567 independent reflections	l = −17→17

Refinement

Refinement on F^2	Primary atom site location: dual
Least-squares matrix: full	Hydrogen site location: difference Fourier map
R[F^2 > 2σ(F^2)] = 0.014	All H-atom parameters refined
wR(F^2) = 0.027	w = 1/[σ^2(Fo^2) + (0.0063P)^2] where P = (Fo^2 + 2Fc^2)/3
S = 1.05	(Δ/σ)max < 0.001
1567 reflections	Δρmax = 0.38 e Å^−3
71 parameters	Δρmin = −0.39 e Å^−3
0 restraints

Special details

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.

Fractional atomic coordinates and isotropic or equivalent isotropic displacement parameters (Ų)

	x	y	z	Uiso*/Ueq
Pr1	0.500000	0.14679 (2)	0.250000	0.00584 (3)
Cl1	0.29528 (6)	−0.17308 (5)	0.05469 (4)	0.01042 (7)
Cl2	0.000000	0.62270 (8)	0.250000	0.01100 (10)
O1	0.1632 (2)	0.29975 (19)	0.05765 (13)	0.0114 (2)
O2	0.2337 (2)	0.0446 (2)	0.28224 (14)	0.0120 (2)
O3	0.4395 (2)	0.42625 (18)	0.35562 (13)	0.0116 (2)
H1A	0.063 (4)	0.265 (4)	0.044 (3)	0.030 (7)*
H1B	0.132 (4)	0.327 (3)	−0.015 (3)	0.027 (7)*
H2A	0.251 (4)	0.083 (4)	0.348 (3)	0.032 (7)*
H2B	0.192 (4)	−0.065 (4)	0.268 (2)	0.025 (6)*
H3A	0.508 (4)	0.524 (4)	0.384 (2)	0.030 (7)*
H3B	0.323 (4)	0.454 (4)	0.328 (3)	0.027 (7)*

Atomic displacement parameters (Ų)

	U^11	U^22	U^33	U^12	U^13	U^23
Pr1	0.00553 (6)	0.00602 (5)	0.00598 (6)	0.000	0.00349 (5)	0.000
Cl1	0.00986 (19)	0.00979 (16)	0.01028 (17)	−0.00112 (13)	0.00542 (15)	−0.00229 (13)
Cl2	0.0102 (3)	0.0119 (2)	0.0114 (2)	0.000	0.0068 (2)	0.000
O1	0.0075 (6)	0.0150 (6)	0.0101 (6)	0.0006 (5)	0.0046 (5)	0.0029 (4)
O2	0.0139 (7)	0.0124 (6)	0.0140 (6)	−0.0029 (5)	0.0107 (6)	−0.0020 (5)
O3	0.0089 (6)	0.0101 (5)	0.0159 (6)	−0.0013 (5)	0.0076 (5)	−0.0040 (5)

Geometric parameters (Å, º)

Pr1—Cl1^i	2.8312 (4)	Pr1—O3^i	2.4513 (12)
Pr1—Cl1	2.8312 (4)	O1—H1A	0.75 (3)
Pr1—O1^i	2.4677 (13)	O1—H1B	0.78 (3)
Pr1—O1	2.4677 (13)	O2—H2A	0.76 (3)
Pr1—O2	2.4818 (13)	O2—H2B	0.77 (2)
Pr1—O2^i	2.4817 (13)	O3—H3A	0.78 (3)
Pr1—O3	2.4513 (12)	O3—H3B	0.80 (3)
Cl1—Pr1—Cl1^i	84.250 (16)	O3^i—Pr1—O1	69.35 (5)
O1—Pr1—Cl1^i	147.16 (3)	O3—Pr1—O1	75.14 (4)
O1^i—Pr1—Cl1	147.16 (3)	O3^i—Pr1—O1^i	75.14 (4)
O1^i—Pr1—Cl1^i	76.31 (3)	O3—Pr1—O1^i	69.35 (5)
O1—Pr1—Cl1	76.31 (3)	O3—Pr1—O2^i	138.35 (4)
O1^i—Pr1—O1	131.98 (6)	O3^i—Pr1—O2	138.35 (4)
O1—Pr1—O2^i	120.50 (4)	O3^i—Pr1—O2^i	69.97 (4)
O1—Pr1—O2	73.29 (4)	O3—Pr1—O2	69.97 (4)
O1^i—Pr1—O2^i	73.29 (4)	O3^i—Pr1—O3	83.09 (6)
O1^i—Pr1—O2	120.50 (4)	Pr1—O1—H1A	119 (2)
O2^i—Pr1—Cl1	77.35 (3)	Pr1—O1—H1B	125.5 (19)
O2—Pr1—Cl1^i	77.35 (3)	H1A—O1—H1B	105 (3)
O2^i—Pr1—Cl1^i	79.51 (3)	Pr1—O2—H2A	117 (2)
O2—Pr1—Cl1	79.51 (3)	Pr1—O2—H2B	121.3 (18)
O2^i—Pr1—O2	148.63 (6)	H2A—O2—H2B	108 (2)
O3—Pr1—Cl1	142.92 (3)	Pr1—O3—H3A	122.8 (18)
O3—Pr1—Cl1^i	108.20 (3)	Pr1—O3—H3B	120.2 (17)
O3^i—Pr1—Cl1	108.20 (3)	H3A—O3—H3B	109 (2)
O3^i—Pr1—Cl1^i	142.92 (3)

Symmetry code: (i) −x+1, y, −z+1/2.

Hydrogen-bond geometry (Å, º)

D—H···A	D—H	H···A	D···A	D—H···A
O1—H1A···Cl1^ii	0.75 (3)	2.42 (3)	3.1498 (14)	166 (3)
O1—H1B···Cl2^iii	0.78 (3)	2.40 (3)	3.1706 (13)	172 (2)
O2—H2A···Cl1^iv	0.76 (3)	2.40 (3)	3.1575 (13)	175 (2)
O2—H2B···Cl2^v	0.77 (2)	2.49 (2)	3.2291 (14)	163 (2)
O3—H3A···Cl1^vi	0.78 (3)	2.36 (3)	3.1303 (14)	174 (2)
O3—H3B···Cl2	0.80 (3)	2.41 (3)	3.1919 (14)	166 (2)

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

Hexaaquadichloridoneodymium(III) chloride (Nd)

Crystal data

[NdCl2(H2O)6]Cl	F(000) = 342
Mr = 358.69	Dx = 2.368 Mg m^−3
Monoclinic, P2/c	Ag Kα radiation, λ = 0.56086 Å
a = 7.9710 (3) Å	Cell parameters from 9892 reflections
b = 6.5460 (2) Å	θ = 2.5–23.7°
c = 12.1246 (5) Å	µ = 3.11 mm^−1
β = 127.324 (1)°	T = 100 K
V = 503.09 (3) Å^3	Plate, purple
Z = 2	0.16 × 0.12 × 0.11 mm

Data collection

Bruker D8 Venture Duo diffractometer	1536 reflections with I > 2σ(I)
ω scans	Rint = 0.036
Absorption correction: multi-scan SADABS-2016/2 (Bruker, 2016)	θmax = 23.7°, θmin = 2.5°
Tmin = 0.201, Tmax = 0.257	h = −11→11
23233 measured reflections	k = −9→9
1559 independent reflections	l = −17→17

Refinement

Refinement on F^2	Hydrogen site location: difference Fourier map
Least-squares matrix: full	All H-atom parameters refined
R[F^2 > 2σ(F^2)] = 0.007	w = 1/[σ^2(Fo^2) + (0.0058P)^2 + 0.0784P] where P = (Fo^2 + 2Fc^2)/3
wR(F^2) = 0.017	(Δ/σ)max = 0.001
S = 1.11	Δρmax = 0.25 e Å^−3
1559 reflections	Δρmin = −0.30 e Å^−3
72 parameters	Extinction correction: SHELXL-2018/1 (Sheldrick 2015b), Fc^*=kFc[1+0.001xFc^2λ^3/sin(2θ)]^-1/4
0 restraints	Extinction coefficient: 0.0145 (7)
Primary atom site location: dual

Special details

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.

Fractional atomic coordinates and isotropic or equivalent isotropic displacement parameters (Ų)

	x	y	z	Uiso*/Ueq
Nd1	0.500000	0.14781 (2)	0.250000	0.00585 (3)
Cl1	0.29595 (3)	−0.17132 (3)	0.05545 (2)	0.01031 (4)
Cl2	0.000000	0.62320 (5)	0.250000	0.01090 (5)
O1	0.16396 (10)	0.30014 (11)	0.05851 (7)	0.01173 (12)
O2	0.23447 (10)	0.04554 (11)	0.28178 (8)	0.01176 (12)
O3	0.44019 (11)	0.42581 (11)	0.35561 (7)	0.01172 (12)
H1A	0.063 (2)	0.268 (3)	0.0458 (17)	0.031 (4)*
H1B	0.137 (2)	0.327 (2)	−0.0083 (18)	0.024 (4)*
H2A	0.246 (3)	0.083 (3)	0.3463 (18)	0.034 (4)*
H2B	0.187 (2)	−0.061 (3)	0.2652 (16)	0.028 (4)*
H3A	0.511 (2)	0.526 (3)	0.3820 (16)	0.029 (4)*
H3B	0.327 (3)	0.463 (2)	0.3272 (16)	0.028 (4)*

Atomic displacement parameters (Ų)

	U^11	U^22	U^33	U^12	U^13	U^23
Nd1	0.00556 (3)	0.00614 (4)	0.00597 (4)	0.000	0.00356 (3)	0.000
Cl1	0.01013 (8)	0.00972 (9)	0.00982 (9)	−0.00096 (6)	0.00539 (7)	−0.00215 (7)
Cl2	0.01039 (12)	0.01175 (13)	0.01133 (13)	0.000	0.00699 (10)	0.000
O1	0.0084 (3)	0.0150 (3)	0.0102 (3)	0.0005 (2)	0.0048 (2)	0.0031 (2)
O2	0.0136 (3)	0.0115 (3)	0.0142 (3)	−0.0033 (2)	0.0105 (3)	−0.0026 (3)
O3	0.0102 (3)	0.0104 (3)	0.0154 (3)	−0.0013 (2)	0.0081 (2)	−0.0037 (2)

Geometric parameters (Å, º)

Nd1—Cl1	2.8145 (2)	Nd1—O3^i	2.4328 (7)
Nd1—Cl1^i	2.8145 (2)	O1—H1A	0.749 (16)
Nd1—O1^i	2.4532 (7)	O1—H1B	0.722 (17)
Nd1—O1	2.4532 (7)	O2—H2A	0.770 (18)
Nd1—O2^i	2.4629 (6)	O2—H2B	0.760 (17)
Nd1—O2	2.4629 (6)	O3—H3A	0.793 (16)
Nd1—O3	2.4328 (7)	O3—H3B	0.782 (16)
Cl1^i—Nd1—Cl1	84.154 (9)	O3^i—Nd1—O1	69.38 (2)
O1—Nd1—Cl1	76.348 (18)	O3—Nd1—O1	75.17 (2)
O1^i—Nd1—Cl1^i	76.348 (18)	O3^i—Nd1—O1^i	75.17 (2)
O1^i—Nd1—Cl1	147.078 (18)	O3—Nd1—O1^i	69.38 (2)
O1—Nd1—Cl1^i	147.077 (18)	O3—Nd1—O2	70.11 (2)
O1^i—Nd1—O1	132.04 (3)	O3^i—Nd1—O2^i	70.11 (2)
O1—Nd1—O2	73.13 (2)	O3^i—Nd1—O2	138.33 (2)
O1—Nd1—O2^i	120.74 (2)	O3—Nd1—O2^i	138.33 (2)
O1^i—Nd1—O2	120.74 (2)	O3^i—Nd1—O3	83.16 (3)
O1^i—Nd1—O2^i	73.13 (2)	Nd1—O1—H1A	119.8 (13)
O2—Nd1—Cl1^i	77.397 (17)	Nd1—O1—H1B	125.2 (12)
O2^i—Nd1—Cl1	77.398 (17)	H1A—O1—H1B	106.3 (16)
O2—Nd1—Cl1	79.318 (18)	Nd1—O2—H2A	119.3 (12)
O2^i—Nd1—Cl1^i	79.318 (18)	Nd1—O2—H2B	123.0 (12)
O2—Nd1—O2^i	148.45 (3)	H2A—O2—H2B	107.0 (16)
O3—Nd1—Cl1^i	108.189 (17)	Nd1—O3—H3A	120.5 (11)
O3—Nd1—Cl1	142.963 (17)	Nd1—O3—H3B	122.7 (11)
O3^i—Nd1—Cl1^i	142.964 (17)	H3A—O3—H3B	105.9 (15)
O3^i—Nd1—Cl1	108.190 (17)

Symmetry code: (i) −x+1, y, −z+1/2.

Hydrogen-bond geometry (Å, º)

D—H···A	D—H	H···A	D···A	D—H···A
O1—H1A···Cl1^ii	0.749 (16)	2.418 (16)	3.1491 (7)	165.6 (16)
O1—H1B···Cl2^iii	0.722 (17)	2.451 (18)	3.1661 (8)	170.8 (15)
O2—H2A···Cl1^iv	0.770 (18)	2.387 (18)	3.1552 (8)	175.3 (17)
O2—H2B···Cl2^v	0.760 (17)	2.490 (17)	3.2267 (8)	164.0 (15)
O3—H3A···Cl1^vi	0.793 (16)	2.337 (17)	3.1290 (7)	176.1 (15)
O3—H3B···Cl2	0.782 (16)	2.413 (16)	3.1894 (7)	172.0 (15)

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

Hexaaquadichloridosamarium(III) chloride (Sm)

Crystal data

[SmCl2(H2O)6]Cl	F(000) = 346
Mr = 364.80	Dx = 2.430 Mg m^−3
Monoclinic, P2/c	Ag Kα radiation, λ = 0.56086 Å
a = 7.9375 (8) Å	Cell parameters from 9537 reflections
b = 6.5351 (7) Å	θ = 3.0–23.7°
c = 12.0713 (11) Å	µ = 3.51 mm^−1
β = 127.217 (2)°	T = 100 K
V = 498.65 (9) Å^3	Plate, yellow
Z = 2	0.25 × 0.21 × 0.18 mm

Data collection

Bruker D8 Venture Duo diffractometer	1533 reflections with I > 2σ(I)
ω scans	Rint = 0.046
Absorption correction: multi-scan SADABS-2016/2 (Bruker, 2016)	θmax = 23.7°, θmin = 2.5°
Tmin = 0.204, Tmax = 0.257	h = −11→11
27415 measured reflections	k = −9→9
1553 independent reflections	l = −17→16

Refinement

Refinement on F^2	Hydrogen site location: difference Fourier map
Least-squares matrix: full	All H-atom parameters refined
R[F^2 > 2σ(F^2)] = 0.010	w = 1/[σ^2(Fo^2) + (0.0104P)^2] where P = (Fo^2 + 2Fc^2)/3
wR(F^2) = 0.023	(Δ/σ)max = 0.001
S = 1.19	Δρmax = 0.48 e Å^−3
1553 reflections	Δρmin = −0.85 e Å^−3
72 parameters	Extinction correction: SHELXL-2018/1 (Sheldrick 2015b), Fc^*=kFc[1+0.001xFc^2λ^3/sin(2θ)]^-1/4
0 restraints	Extinction coefficient: 0.0299 (11)
Primary atom site location: dual

Special details

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.

Fractional atomic coordinates and isotropic or equivalent isotropic displacement parameters (Ų)

	x	y	z	Uiso*/Ueq
Sm1	0.500000	0.14983 (2)	0.250000	0.00823 (4)
Cl1	0.29725 (4)	−0.16793 (4)	0.05721 (3)	0.01414 (5)
Cl2	0.000000	0.62416 (6)	0.250000	0.01522 (7)
O1	0.16623 (14)	0.30030 (14)	0.06034 (9)	0.01545 (15)
O2	0.23649 (13)	0.04788 (14)	0.28158 (9)	0.01546 (15)
O3	0.44104 (14)	0.42539 (13)	0.35504 (9)	0.01546 (15)
H1A	0.072 (3)	0.272 (3)	0.048 (2)	0.030 (5)*
H1B	0.135 (4)	0.333 (3)	−0.013 (3)	0.039 (6)*
H2A	0.250 (3)	0.085 (3)	0.351 (2)	0.028 (4)*
H2B	0.187 (3)	−0.062 (3)	0.2644 (18)	0.024 (4)*
H3A	0.510 (3)	0.525 (3)	0.381 (2)	0.041 (5)*
H3B	0.324 (3)	0.457 (3)	0.3251 (18)	0.029 (4)*

Atomic displacement parameters (Ų)

	U^11	U^22	U^33	U^12	U^13	U^23
Sm1	0.00783 (5)	0.00820 (5)	0.00880 (4)	0.000	0.00510 (3)	0.000
Cl1	0.01386 (12)	0.01289 (12)	0.01390 (11)	−0.00140 (8)	0.00746 (10)	−0.00317 (8)
Cl2	0.01447 (16)	0.01628 (16)	0.01618 (16)	0.000	0.00993 (14)	0.000
O1	0.0105 (4)	0.0191 (4)	0.0140 (4)	0.0011 (3)	0.0059 (3)	0.0040 (3)
O2	0.0174 (4)	0.0152 (4)	0.0192 (4)	−0.0043 (3)	0.0139 (3)	−0.0029 (3)
O3	0.0141 (4)	0.0131 (4)	0.0204 (4)	−0.0018 (3)	0.0111 (3)	−0.0052 (3)

Geometric parameters (Å, º)

Sm1—Cl1	2.7906 (3)	Sm1—O3	2.4057 (8)
Sm1—Cl1^i	2.7906 (3)	O1—H1A	0.693 (19)
Sm1—O1^i	2.4269 (8)	O1—H1B	0.79 (3)
Sm1—O1	2.4269 (8)	O2—H2A	0.81 (2)
Sm1—O2	2.4349 (8)	O2—H2B	0.78 (2)
Sm1—O2^i	2.4349 (8)	O3—H3A	0.78 (2)
Sm1—O3^i	2.4057 (8)	O3—H3B	0.794 (19)
Cl1^i—Sm1—Cl1	83.829 (14)	O3—Sm1—O1	75.20 (3)
O1—Sm1—Cl1	76.40 (2)	O3^i—Sm1—O1	69.44 (3)
O1^i—Sm1—Cl1^i	76.40 (2)	O3—Sm1—O1^i	69.44 (3)
O1^i—Sm1—Cl1	146.94 (2)	O3^i—Sm1—O1^i	75.20 (3)
O1—Sm1—Cl1^i	146.94 (2)	O3^i—Sm1—O2^i	70.30 (3)
O1^i—Sm1—O1	132.20 (4)	O3—Sm1—O2	70.30 (3)
O1—Sm1—O2^i	120.94 (3)	O3—Sm1—O2^i	138.31 (3)
O1—Sm1—O2	73.00 (3)	O3^i—Sm1—O2	138.31 (3)
O1^i—Sm1—O2^i	73.00 (3)	O3—Sm1—O3^i	83.07 (4)
O1^i—Sm1—O2	120.94 (3)	Sm1—O1—H1A	120.8 (17)
O2^i—Sm1—Cl1^i	79.06 (2)	Sm1—O1—H1B	126.5 (17)
O2—Sm1—Cl1	79.06 (2)	H1A—O1—H1B	105 (2)
O2^i—Sm1—Cl1	77.44 (2)	Sm1—O2—H2A	119.3 (13)
O2—Sm1—Cl1^i	77.44 (2)	Sm1—O2—H2B	123.1 (13)
O2^i—Sm1—O2	148.24 (4)	H2A—O2—H2B	106.3 (18)
O3^i—Sm1—Cl1^i	143.00 (2)	Sm1—O3—H3A	121.5 (16)
O3^i—Sm1—Cl1	108.38 (2)	Sm1—O3—H3B	120.0 (13)
O3—Sm1—Cl1^i	108.38 (2)	H3A—O3—H3B	108 (2)
O3—Sm1—Cl1	143.00 (2)

Symmetry code: (i) −x+1, y, −z+1/2.

Hydrogen-bond geometry (Å, º)

D—H···A	D—H	H···A	D···A	D—H···A
O1—H1A···Cl1^ii	0.693 (19)	2.484 (19)	3.1594 (10)	165 (2)
O1—H1B···Cl2^iii	0.79 (3)	2.39 (3)	3.1685 (9)	169.2 (19)
O2—H2A···Cl1^iv	0.81 (2)	2.35 (2)	3.1586 (9)	175.9 (18)
O2—H2B···Cl2^v	0.78 (2)	2.48 (2)	3.2358 (10)	163.6 (17)
O3—H3A···Cl1^vi	0.78 (2)	2.36 (2)	3.1367 (10)	176 (2)
O3—H3B···Cl2	0.794 (19)	2.41 (2)	3.1908 (9)	167.7 (18)

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

Hexaaquadichloridoeuropium(III) chloride (Eu)

Crystal data

[EuCl2(H2O)6]Cl	F(000) = 348
Mr = 366.41	Dx = 2.466 Mg m^−3
Monoclinic, P2/c	Ag Kα radiation, λ = 0.56086 Å
a = 7.9062 (2) Å	Cell parameters from 9987 reflections
b = 6.5092 (2) Å	θ = 2.5–23.7°
c = 12.0410 (4) Å	µ = 3.75 mm^−1
β = 127.231 (1)°	T = 100 K
V = 493.38 (3) Å^3	Plate, colorless
Z = 2	0.13 × 0.13 × 0.11 mm

Data collection

Bruker D8 Venture Duo diffractometer	1504 reflections with I > 2σ(I)
ω scans	Rint = 0.038
Absorption correction: multi-scan SADABS-2016/2 (Bruker, 2016)	θmax = 23.7°, θmin = 2.5°
Tmin = 0.218, Tmax = 0.257	h = −11→11
21905 measured reflections	k = −9→9
1529 independent reflections	l = −17→17

Refinement

Refinement on F^2	Hydrogen site location: difference Fourier map
Least-squares matrix: full	All H-atom parameters refined
R[F^2 > 2σ(F^2)] = 0.007	w = 1/[σ^2(Fo^2) + (0.0058P)^2] where P = (Fo^2 + 2Fc^2)/3
wR(F^2) = 0.016	(Δ/σ)max = 0.001
S = 1.13	Δρmax = 0.29 e Å^−3
1529 reflections	Δρmin = −0.32 e Å^−3
72 parameters	Extinction correction: SHELXL-2018/1 (Sheldrick 2015b), Fc^*=kFc[1+0.001xFc^2λ^3/sin(2θ)]^-1/4
0 restraints	Extinction coefficient: 0.0155 (6)
Primary atom site location: dual

Special details

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.

Fractional atomic coordinates and isotropic or equivalent isotropic displacement parameters (Ų)

	x	y	z	Uiso*/Ueq
Eu1	0.500000	0.15065 (2)	0.250000	0.00549 (3)
Cl1	0.29777 (3)	−0.16684 (3)	0.05730 (2)	0.00967 (4)
Cl2	0.000000	0.62348 (4)	0.250000	0.01034 (6)
O1	0.16667 (11)	0.30060 (11)	0.06078 (8)	0.01088 (13)
O2	0.23665 (11)	0.04821 (11)	0.28100 (8)	0.01108 (13)
O3	0.44219 (11)	0.42430 (10)	0.35568 (8)	0.01082 (13)
H1A	0.062 (2)	0.268 (2)	0.0449 (17)	0.029 (4)*
H1B	0.134 (3)	0.332 (2)	−0.011 (2)	0.028 (4)*
H2A	0.250 (2)	0.085 (2)	0.3479 (17)	0.024 (4)*
H2B	0.193 (2)	−0.060 (2)	0.2653 (16)	0.026 (4)*
H3A	0.513 (2)	0.523 (2)	0.3791 (16)	0.030 (4)*
H3B	0.334 (2)	0.458 (2)	0.3268 (16)	0.025 (4)*

Atomic displacement parameters (Ų)

	U^11	U^22	U^33	U^12	U^13	U^23
Eu1	0.00511 (3)	0.00572 (3)	0.00569 (4)	0.000	0.00329 (3)	0.000
Cl1	0.00927 (9)	0.00919 (9)	0.00941 (10)	−0.00089 (7)	0.00505 (8)	−0.00199 (7)
Cl2	0.00946 (13)	0.01139 (13)	0.01076 (14)	0.000	0.00643 (12)	0.000
O1	0.0075 (3)	0.0138 (3)	0.0098 (3)	0.0005 (2)	0.0044 (3)	0.0026 (3)
O2	0.0130 (3)	0.0106 (3)	0.0135 (3)	−0.0026 (2)	0.0101 (3)	−0.0020 (3)
O3	0.0083 (3)	0.0095 (3)	0.0147 (4)	−0.0013 (2)	0.0071 (3)	−0.0039 (3)

Geometric parameters (Å, º)

Eu1—Cl1	2.7788 (2)	Eu1—O3	2.3884 (7)
Eu1—Cl1^i	2.7788 (2)	O1—H1A	0.760 (15)
Eu1—O1^i	2.4131 (7)	O1—H1B	0.766 (19)
Eu1—O1	2.4131 (7)	O2—H2A	0.784 (16)
Eu1—O2	2.4206 (7)	O2—H2B	0.759 (16)
Eu1—O2^i	2.4206 (7)	O3—H3A	0.783 (16)
Eu1—O3^i	2.3884 (7)	O3—H3B	0.737 (15)
Cl1^i—Eu1—Cl1	83.904 (10)	O3—Eu1—O1	75.50 (3)
O1—Eu1—Cl1	76.376 (18)	O3^i—Eu1—O1	69.33 (2)
O1^i—Eu1—Cl1^i	76.376 (18)	O3—Eu1—O1^i	69.33 (2)
O1^i—Eu1—Cl1	146.839 (18)	O3^i—Eu1—O1^i	75.50 (3)
O1—Eu1—Cl1^i	146.840 (18)	O3^i—Eu1—O2^i	70.34 (2)
O1^i—Eu1—O1	132.29 (3)	O3—Eu1—O2	70.34 (2)
O1—Eu1—O2^i	121.05 (3)	O3—Eu1—O2^i	138.36 (2)
O1—Eu1—O2	72.97 (3)	O3^i—Eu1—O2	138.36 (2)
O1^i—Eu1—O2^i	72.97 (3)	O3—Eu1—O3^i	83.55 (3)
O1^i—Eu1—O2	121.05 (3)	Eu1—O1—H1A	121.7 (12)
O2^i—Eu1—Cl1^i	79.036 (19)	Eu1—O1—H1B	127.1 (12)
O2—Eu1—Cl1	79.037 (19)	H1A—O1—H1B	102.6 (16)
O2^i—Eu1—Cl1	77.317 (17)	Eu1—O2—H2A	118.7 (11)
O2—Eu1—Cl1^i	77.317 (17)	Eu1—O2—H2B	121.7 (11)
O2^i—Eu1—O2	148.02 (3)	H2A—O2—H2B	107.3 (15)
O3^i—Eu1—Cl1^i	143.185 (18)	Eu1—O3—H3A	118.5 (11)
O3^i—Eu1—Cl1	107.979 (18)	Eu1—O3—H3B	120.7 (12)
O3—Eu1—Cl1^i	107.980 (18)	H3A—O3—H3B	107.7 (15)
O3—Eu1—Cl1	143.185 (18)

Symmetry code: (i) −x+1, y, −z+1/2.

Hydrogen-bond geometry (Å, º)

D—H···A	D—H	H···A	D···A	D—H···A
O1—H1A···Cl1^ii	0.760 (15)	2.407 (15)	3.1537 (7)	167.5 (16)
O1—H1B···Cl2^iii	0.766 (19)	2.407 (19)	3.1649 (8)	170.6 (14)
O2—H2A···Cl1^iv	0.784 (16)	2.373 (17)	3.1549 (8)	175.1 (14)
O2—H2B···Cl2^v	0.759 (16)	2.500 (15)	3.2308 (7)	162.1 (14)
O3—H3A···Cl1^vi	0.783 (16)	2.349 (16)	3.1307 (7)	175.7 (14)
O3—H3B···Cl2	0.737 (15)	2.455 (15)	3.1842 (7)	170.3 (15)

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

Hexaaquadichloridogadolinium(III) chloride (Gd)

Crystal data

[GdCl2(H2O)6]Cl	F(000) = 350
Mr = 371.70	Dx = 2.518 Mg m^−3
Monoclinic, P2/c	Ag Kα radiation, λ = 0.56086 Å
a = 7.8835 (3) Å	Cell parameters from 9213 reflections
b = 6.4964 (3) Å	θ = 2.5–23.8°
c = 12.0176 (4) Å	µ = 3.99 mm^−1
β = 127.186 (1)°	T = 100 K
V = 490.33 (3) Å^3	Plate, colorless
Z = 2	0.33 × 0.25 × 0.20 mm

Data collection

Bruker D8 Venture Duo diffractometer	1520 reflections with I > 2σ(I)
ω scans	Rint = 0.037
Absorption correction: multi-scan SADABS-2016/2 (Bruker, 2016)	θmax = 23.8°, θmin = 2.5°
Tmin = 0.172, Tmax = 0.257	h = −11→11
26021 measured reflections	k = −9→9
1532 independent reflections	l = −17→17

Refinement

Refinement on F^2	Hydrogen site location: difference Fourier map
Least-squares matrix: full	All H-atom parameters refined
R[F^2 > 2σ(F^2)] = 0.009	w = 1/[σ^2(Fo^2) + (0.0082P)^2 + 0.0734P] where P = (Fo^2 + 2Fc^2)/3
wR(F^2) = 0.021	(Δ/σ)max = 0.001
S = 1.23	Δρmax = 0.44 e Å^−3
1532 reflections	Δρmin = −0.38 e Å^−3
72 parameters	Extinction correction: SHELXL-2018/1 (Sheldrick 2015b), Fc^*=kFc[1+0.001xFc^2λ^3/sin(2θ)]^-1/4
0 restraints	Extinction coefficient: 0.0279 (9)
Primary atom site location: dual

Special details

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.

Fractional atomic coordinates and isotropic or equivalent isotropic displacement parameters (Ų)

	x	y	z	Uiso*/Ueq
Gd1	0.500000	0.15160 (2)	0.250000	0.00581 (3)
Cl1	0.29831 (4)	−0.16561 (4)	0.05775 (3)	0.01005 (5)
Cl2	0.000000	0.62367 (6)	0.250000	0.01075 (7)
O1	0.16722 (14)	0.30084 (14)	0.06138 (9)	0.01150 (15)
O2	0.23723 (13)	0.04881 (14)	0.28098 (9)	0.01135 (15)
O3	0.44242 (14)	0.42417 (13)	0.35554 (9)	0.01117 (15)
H1A	0.060 (3)	0.266 (3)	0.047 (2)	0.028 (5)*
H1B	0.139 (3)	0.329 (3)	−0.008 (2)	0.023 (5)*
H2A	0.254 (3)	0.086 (3)	0.350 (2)	0.029 (5)*
H2B	0.189 (3)	−0.068 (3)	0.264 (2)	0.030 (5)*
H3A	0.513 (4)	0.532 (3)	0.381 (2)	0.037 (5)*
H3B	0.325 (3)	0.458 (3)	0.326 (2)	0.027 (5)*

Atomic displacement parameters (Ų)

	U^11	U^22	U^33	U^12	U^13	U^23
Gd1	0.00572 (4)	0.00572 (4)	0.00615 (4)	0.000	0.00367 (3)	0.000
Cl1	0.00989 (11)	0.00916 (11)	0.00986 (11)	−0.00088 (8)	0.00532 (10)	−0.00202 (8)
Cl2	0.01014 (16)	0.01129 (16)	0.01144 (16)	0.000	0.00685 (14)	0.000
O1	0.0083 (4)	0.0145 (4)	0.0100 (4)	0.0004 (3)	0.0046 (3)	0.0025 (3)
O2	0.0127 (4)	0.0110 (4)	0.0138 (4)	−0.0024 (3)	0.0098 (3)	−0.0017 (3)
O3	0.0100 (4)	0.0088 (4)	0.0151 (4)	−0.0010 (3)	0.0078 (3)	−0.0032 (3)

Geometric parameters (Å, º)

Gd1—Cl1^i	2.7699 (3)	Gd1—O3^i	2.3762 (8)
Gd1—Cl1	2.7699 (3)	O1—H1A	0.79 (2)
Gd1—O1	2.4026 (9)	O1—H1B	0.75 (2)
Gd1—O1^i	2.4026 (9)	O2—H2A	0.80 (2)
Gd1—O2^i	2.4101 (8)	O2—H2B	0.82 (2)
Gd1—O2	2.4101 (8)	O3—H3A	0.83 (2)
Gd1—O3	2.3762 (8)	O3—H3B	0.79 (2)
Cl1—Gd1—Cl1^i	83.855 (12)	O3^i—Gd1—O1^i	75.58 (3)
O1^i—Gd1—Cl1^i	76.37 (2)	O3—Gd1—O1^i	69.37 (3)
O1—Gd1—Cl1	76.37 (2)	O3^i—Gd1—O1	69.37 (3)
O1—Gd1—Cl1^i	146.74 (2)	O3—Gd1—O1	75.58 (3)
O1^i—Gd1—Cl1	146.74 (2)	O3—Gd1—O2	70.41 (3)
O1—Gd1—O1^i	132.40 (4)	O3^i—Gd1—O2^i	70.41 (3)
O1^i—Gd1—O2	121.09 (3)	O3^i—Gd1—O2	138.44 (3)
O1^i—Gd1—O2^i	72.98 (3)	O3—Gd1—O2^i	138.44 (3)
O1—Gd1—O2	72.97 (3)	O3^i—Gd1—O3	83.65 (4)
O1—Gd1—O2^i	121.09 (3)	Gd1—O1—H1A	120.3 (15)
O2—Gd1—Cl1	78.99 (2)	Gd1—O1—H1B	125.0 (15)
O2^i—Gd1—Cl1^i	78.99 (2)	H1A—O1—H1B	106 (2)
O2—Gd1—Cl1^i	77.21 (2)	Gd1—O2—H2A	117.6 (15)
O2^i—Gd1—Cl1	77.21 (2)	Gd1—O2—H2B	121.9 (14)
O2—Gd1—O2^i	147.83 (4)	H2A—O2—H2B	108 (2)
O3—Gd1—Cl1	143.24 (2)	Gd1—O3—H3A	121.6 (14)
O3—Gd1—Cl1^i	107.92 (2)	Gd1—O3—H3B	121.0 (14)
O3^i—Gd1—Cl1	107.92 (2)	H3A—O3—H3B	106 (2)
O3^i—Gd1—Cl1^i	143.24 (2)

Symmetry code: (i) −x+1, y, −z+1/2.

Hydrogen-bond geometry (Å, º)

D—H···A	D—H	H···A	D···A	D—H···A
O1—H1A···Cl1^ii	0.79 (2)	2.39 (2)	3.1527 (9)	165 (2)
O1—H1B···Cl2^iii	0.75 (2)	2.43 (2)	3.1651 (9)	170.1 (19)
O2—H2A···Cl1^iv	0.80 (2)	2.36 (2)	3.1519 (9)	175 (2)
O2—H2B···Cl2^v	0.82 (2)	2.44 (2)	3.2284 (9)	161.7 (18)
O3—H3A···Cl1^vi	0.83 (2)	2.30 (2)	3.1290 (9)	178 (2)
O3—H3B···Cl2	0.79 (2)	2.40 (2)	3.1790 (9)	169.1 (19)

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

Hexaaquadichloridoterbium(III) chloride (Tb)

Crystal data

[TbCl2(H2O)6]Cl	F(000) = 352
Mr = 373.37	Dx = 2.542 Mg m^−3
Monoclinic, P2/c	Ag Kα radiation, λ = 0.56086 Å
a = 7.8646 (3) Å	Cell parameters from 9445 reflections
b = 6.4903 (3) Å	θ = 2.5–23.7°
c = 11.9871 (5) Å	µ = 4.24 mm^−1
β = 127.134 (1)°	T = 100 K
V = 487.79 (4) Å^3	Plate, colorless
Z = 2	0.3 × 0.16 × 0.12 mm

Data collection

Bruker D8 Venture Duo diffractometer	1481 reflections with I > 2σ(I)
ω scans	Rint = 0.024
Absorption correction: multi-scan SADABS-2016/2 (Bruker, 2016)	θmax = 23.7°, θmin = 2.5°
Tmin = 0.223, Tmax = 0.257	h = −10→11
11117 measured reflections	k = −9→9
1503 independent reflections	l = −17→17

Refinement

Refinement on F^2	Hydrogen site location: difference Fourier map
Least-squares matrix: full	All H-atom parameters refined
R[F^2 > 2σ(F^2)] = 0.009	w = 1/[σ^2(Fo^2) + (0.008P)^2 + 0.0701P] where P = (Fo^2 + 2Fc^2)/3
wR(F^2) = 0.020	(Δ/σ)max < 0.001
S = 1.10	Δρmax = 0.36 e Å^−3
1503 reflections	Δρmin = −0.37 e Å^−3
72 parameters	Extinction correction: SHELXL-2018/1 (Sheldrick 2015b), Fc^*=kFc[1+0.001xFc^2λ^3/sin(2θ)]^-1/4
0 restraints	Extinction coefficient: 0.0117 (6)
Primary atom site location: dual

Special details

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.

Fractional atomic coordinates and isotropic or equivalent isotropic displacement parameters (Ų)

	x	y	z	Uiso*/Ueq
Tb1	0.500000	0.15305 (2)	0.250000	0.00536 (3)
Cl1	0.29840 (4)	−0.16404 (4)	0.05842 (3)	0.00937 (5)
Cl2	0.000000	0.62554 (6)	0.250000	0.01012 (7)
O1	0.16832 (14)	0.30085 (14)	0.06248 (10)	0.01064 (16)
O2	0.23848 (14)	0.05048 (15)	0.28092 (10)	0.01085 (16)
O3	0.44279 (14)	0.42471 (14)	0.35533 (9)	0.01056 (16)
H1A	0.065 (3)	0.265 (3)	0.049 (2)	0.026 (5)*
H1B	0.139 (3)	0.325 (3)	−0.011 (2)	0.028 (5)*
H2A	0.257 (3)	0.088 (3)	0.353 (2)	0.030 (5)*
H2B	0.194 (3)	−0.058 (3)	0.262 (2)	0.026 (5)*
H3A	0.519 (3)	0.525 (3)	0.383 (2)	0.028 (5)*
H3B	0.327 (3)	0.453 (3)	0.326 (2)	0.033 (5)*

Atomic displacement parameters (Ų)

	U^11	U^22	U^33	U^12	U^13	U^23
Tb1	0.00486 (4)	0.00550 (4)	0.00570 (4)	0.000	0.00318 (3)	0.000
Cl1	0.00902 (11)	0.00878 (12)	0.00908 (11)	−0.00078 (8)	0.00481 (10)	−0.00186 (9)
Cl2	0.00953 (16)	0.01080 (17)	0.01046 (17)	0.000	0.00626 (14)	0.000
O1	0.0076 (4)	0.0132 (4)	0.0094 (4)	0.0004 (3)	0.0043 (3)	0.0024 (3)
O2	0.0123 (4)	0.0102 (4)	0.0132 (4)	−0.0030 (3)	0.0094 (3)	−0.0027 (3)
O3	0.0089 (4)	0.0088 (4)	0.0145 (4)	−0.0011 (3)	0.0073 (3)	−0.0035 (3)

Geometric parameters (Å, º)

Tb1—Cl1^i	2.7617 (3)	Tb1—O3	2.3646 (9)
Tb1—Cl1	2.7617 (3)	O1—H1A	0.77 (2)
Tb1—O1	2.3870 (9)	O1—H1B	0.77 (2)
Tb1—O1^i	2.3870 (9)	O2—H2A	0.82 (2)
Tb1—O2^i	2.3940 (9)	O2—H2B	0.76 (2)
Tb1—O2	2.3940 (9)	O3—H3A	0.81 (2)
Tb1—O3^i	2.3646 (9)	O3—H3B	0.77 (2)
Cl1—Tb1—Cl1^i	83.649 (12)	O3—Tb1—O1^i	69.48 (3)
O1^i—Tb1—Cl1^i	76.35 (2)	O3^i—Tb1—O1^i	75.59 (3)
O1—Tb1—Cl1	76.35 (2)	O3—Tb1—O1	75.59 (3)
O1—Tb1—Cl1^i	146.61 (2)	O3^i—Tb1—O1	69.49 (3)
O1^i—Tb1—Cl1	146.61 (2)	O3^i—Tb1—O2	138.44 (3)
O1—Tb1—O1^i	132.61 (4)	O3—Tb1—O2^i	138.44 (3)
O1^i—Tb1—O2	121.23 (3)	O3—Tb1—O2	70.52 (3)
O1^i—Tb1—O2^i	72.84 (3)	O3^i—Tb1—O2^i	70.52 (3)
O1—Tb1—O2	72.84 (3)	O3—Tb1—O3^i	83.57 (5)
O1—Tb1—O2^i	121.24 (3)	Tb1—O1—H1A	119.7 (16)
O2—Tb1—Cl1	78.81 (2)	Tb1—O1—H1B	124.1 (16)
O2^i—Tb1—Cl1^i	78.81 (2)	H1A—O1—H1B	106 (2)
O2—Tb1—Cl1^i	77.27 (2)	Tb1—O2—H2A	117.3 (14)
O2^i—Tb1—Cl1	77.27 (2)	Tb1—O2—H2B	119.8 (15)
O2—Tb1—O2^i	147.71 (5)	H2A—O2—H2B	110 (2)
O3^i—Tb1—Cl1	108.08 (2)	Tb1—O3—H3A	119.5 (14)
O3^i—Tb1—Cl1^i	143.22 (2)	Tb1—O3—H3B	118.8 (16)
O3—Tb1—Cl1	143.22 (2)	H3A—O3—H3B	112 (2)
O3—Tb1—Cl1^i	108.08 (2)

Symmetry code: (i) −x+1, y, −z+1/2.

Hydrogen-bond geometry (Å, º)

D—H···A	D—H	H···A	D···A	D—H···A
O1—H1A···Cl1^ii	0.77 (2)	2.41 (2)	3.1527 (9)	164 (2)
O1—H1B···Cl2^iii	0.77 (2)	2.40 (2)	3.1661 (10)	172 (2)
O2—H2A···Cl1^iv	0.82 (2)	2.33 (2)	3.1524 (10)	175 (2)
O2—H2B···Cl2^v	0.76 (2)	2.51 (2)	3.2283 (10)	158.8 (19)
O3—H3A···Cl1^vi	0.81 (2)	2.33 (2)	3.1297 (10)	173.2 (19)
O3—H3B···Cl2	0.77 (2)	2.43 (2)	3.1798 (9)	166 (2)

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

Hexaaquadichloridodysprosium(III) chloride (Dy)

Crystal data

[DyCl2(H2O)6]Cl	F(000) = 354
Mr = 376.95	Dx = 2.586 Mg m^−3
Monoclinic, P2/c	Ag Kα radiation, λ = 0.56086 Å
a = 7.8439 (3) Å	Cell parameters from 9894 reflections
b = 6.4693 (3) Å	θ = 2.7–23.7°
c = 11.9660 (5) Å	µ = 4.51 mm^−1
β = 127.143 (1)°	T = 100 K
V = 484.02 (4) Å^3	Plate, yellow
Z = 2	0.23 × 0.19 × 0.14 mm

Data collection

Bruker D8 Venture Duo diffractometer	1485 reflections with I > 2σ(I)
ω scans	Rint = 0.037
Absorption correction: multi-scan SADABS-2016/2 (Bruker, 2016)	θmax = 23.8°, θmin = 2.5°
Tmin = 0.184, Tmax = 0.257	h = −11→11
21844 measured reflections	k = −9→9
1501 independent reflections	l = −17→17

Refinement

Refinement on F^2	Hydrogen site location: difference Fourier map
Least-squares matrix: full	All H-atom parameters refined
R[F^2 > 2σ(F^2)] = 0.008	w = 1/[σ^2(Fo^2) + (0.006P)^2 + 0.0553P] where P = (Fo^2 + 2Fc^2)/3
wR(F^2) = 0.018	(Δ/σ)max < 0.001
S = 1.19	Δρmax = 0.42 e Å^−3
1501 reflections	Δρmin = −0.48 e Å^−3
72 parameters	Extinction correction: SHELXL-2018/1 (Sheldrick 2015b), Fc^*=kFc[1+0.001xFc^2λ^3/sin(2θ)]^-1/4
0 restraints	Extinction coefficient: 0.0098 (6)
Primary atom site location: dual

Special details

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.

Fractional atomic coordinates and isotropic or equivalent isotropic displacement parameters (Ų)

	x	y	z	Uiso*/Ueq
Dy1	0.500000	0.15396 (2)	0.250000	0.00517 (3)
Cl1	0.29906 (4)	−0.16263 (3)	0.05869 (3)	0.00928 (5)
Cl2	0.000000	0.62489 (5)	0.250000	0.00990 (6)
O1	0.16915 (13)	0.30103 (12)	0.06305 (8)	0.01025 (14)
O2	0.23924 (13)	0.05125 (12)	0.28056 (9)	0.01049 (14)
O3	0.44370 (14)	0.42381 (12)	0.35560 (8)	0.01037 (14)
H1A	0.065 (3)	0.264 (3)	0.046 (2)	0.027 (4)*
H1B	0.133 (3)	0.330 (2)	−0.011 (2)	0.030 (5)*
H2A	0.253 (3)	0.086 (3)	0.349 (2)	0.034 (5)*
H2B	0.195 (3)	−0.050 (3)	0.2644 (19)	0.026 (5)*
H3A	0.513 (3)	0.525 (3)	0.3771 (18)	0.028 (4)*
H3B	0.332 (3)	0.453 (3)	0.326 (2)	0.033 (5)*

Atomic displacement parameters (Ų)

	U^11	U^22	U^33	U^12	U^13	U^23
Dy1	0.00492 (4)	0.00544 (4)	0.00538 (4)	0.000	0.00322 (3)	0.000
Cl1	0.00897 (11)	0.00907 (10)	0.00889 (10)	−0.00078 (7)	0.00491 (9)	−0.00194 (7)
Cl2	0.00935 (15)	0.01086 (13)	0.01022 (15)	0.000	0.00630 (13)	0.000
O1	0.0068 (3)	0.0132 (3)	0.0090 (3)	0.0003 (3)	0.0038 (3)	0.0022 (3)
O2	0.0121 (4)	0.0100 (3)	0.0127 (4)	−0.0028 (3)	0.0093 (3)	−0.0018 (3)
O3	0.0084 (4)	0.0097 (3)	0.0137 (3)	−0.0014 (3)	0.0070 (3)	−0.0033 (3)

Geometric parameters (Å, º)

Dy1—Cl1^i	2.7500 (2)	Dy1—O3^i	2.3480 (8)
Dy1—Cl1	2.7500 (2)	O1—H1A	0.755 (19)
Dy1—O1	2.3735 (8)	O1—H1B	0.78 (2)
Dy1—O1^i	2.3735 (8)	O2—H2A	0.79 (2)
Dy1—O2^i	2.3796 (8)	O2—H2B	0.712 (19)
Dy1—O2	2.3795 (8)	O3—H3A	0.787 (19)
Dy1—O3	2.3480 (8)	O3—H3B	0.75 (2)
Cl1—Dy1—Cl1^i	83.719 (11)	O3^i—Dy1—O1^i	75.83 (3)
O1^i—Dy1—Cl1^i	76.29 (2)	O3—Dy1—O1^i	69.43 (3)
O1—Dy1—Cl1	76.29 (2)	O3^i—Dy1—O1	69.43 (3)
O1—Dy1—Cl1^i	146.52 (2)	O3—Dy1—O1	75.83 (3)
O1^i—Dy1—Cl1	146.52 (2)	O3—Dy1—O2	70.52 (3)
O1—Dy1—O1^i	132.73 (4)	O3^i—Dy1—O2^i	70.52 (3)
O1^i—Dy1—O2	121.28 (3)	O3^i—Dy1—O2	138.48 (3)
O1^i—Dy1—O2^i	72.82 (3)	O3—Dy1—O2^i	138.48 (3)
O1—Dy1—O2	72.82 (3)	O3^i—Dy1—O3	83.94 (4)
O1—Dy1—O2^i	121.28 (3)	Dy1—O1—H1A	121.1 (14)
O2—Dy1—Cl1	78.83 (2)	Dy1—O1—H1B	127.6 (15)
O2^i—Dy1—Cl1^i	78.82 (2)	H1A—O1—H1B	101 (2)
O2—Dy1—Cl1^i	77.17 (2)	Dy1—O2—H2A	119.3 (15)
O2^i—Dy1—Cl1	77.17 (2)	Dy1—O2—H2B	122.6 (15)
O2—Dy1—O2^i	147.57 (4)	H2A—O2—H2B	106 (2)
O3—Dy1—Cl1	143.34 (2)	Dy1—O3—H3A	118.6 (13)
O3—Dy1—Cl1^i	107.77 (2)	Dy1—O3—H3B	118.8 (15)
O3^i—Dy1—Cl1	107.77 (2)	H3A—O3—H3B	109.0 (19)
O3^i—Dy1—Cl1^i	143.34 (2)

Symmetry code: (i) −x+1, y, −z+1/2.

Hydrogen-bond geometry (Å, º)

D—H···A	D—H	H···A	D···A	D—H···A
O1—H1A···Cl1^ii	0.755 (19)	2.413 (19)	3.1545 (9)	167.6 (19)
O1—H1B···Cl2^iii	0.78 (2)	2.39 (2)	3.1655 (8)	172.6 (16)
O2—H2A···Cl1^iv	0.79 (2)	2.37 (2)	3.1511 (9)	175.7 (19)
O2—H2B···Cl2^v	0.712 (19)	2.544 (19)	3.2303 (8)	162.7 (19)
O3—H3A···Cl1^vi	0.787 (19)	2.342 (19)	3.1276 (8)	176.2 (18)
O3—H3B···Cl2	0.75 (2)	2.44 (2)	3.1766 (8)	167.1 (19)

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

Hexaaquadichloridoholmium(III) chloride (Ho)

Crystal data

[HoCl2(H2O)6]Cl	F(000) = 356
Mr = 379.38	Dx = 2.611 Mg m^−3
Monoclinic, P2/c	Ag Kα radiation, λ = 0.56086 Å
a = 7.8303 (3) Å	Cell parameters from 7807 reflections
b = 6.4651 (2) Å	θ = 2.5–23.7°
c = 11.9509 (4) Å	µ = 4.77 mm^−1
β = 127.086 (1)°	T = 100 K
V = 482.63 (3) Å^3	Plate, yellow
Z = 2	0.14 × 0.10 × 0.07 mm

Data collection

Bruker D8 Venture Duo diffractometer	1454 reflections with I > 2σ(I)
ω scans	Rint = 0.026
Absorption correction: multi-scan SADABS-2016/2 (Bruker, 2016)	θmax = 23.7°, θmin = 2.5°
Tmin = 0.222, Tmax = 0.257	h = −11→11
10309 measured reflections	k = −9→9
1480 independent reflections	l = −17→17

Refinement

Refinement on F^2	Hydrogen site location: difference Fourier map
Least-squares matrix: full	All H-atom parameters refined
R[F^2 > 2σ(F^2)] = 0.009	w = 1/[σ^2(Fo^2) + (0.0056P)^2 + 0.0614P] where P = (Fo^2 + 2Fc^2)/3
wR(F^2) = 0.020	(Δ/σ)max = 0.001
S = 1.07	Δρmax = 0.31 e Å^−3
1480 reflections	Δρmin = −0.36 e Å^−3
72 parameters	Extinction correction: SHELXL-2018/1 (Sheldrick 2015b), Fc^*=kFc[1+0.001xFc^2λ^3/sin(2θ)]^-1/4
0 restraints	Extinction coefficient: 0.0063 (5)
Primary atom site location: dual

Special details

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.

Fractional atomic coordinates and isotropic or equivalent isotropic displacement parameters (Ų)

	x	y	z	Uiso*/Ueq
Ho1	0.500000	0.15471 (2)	0.250000	0.00548 (3)
Cl1	0.29952 (5)	−0.16158 (4)	0.05941 (3)	0.00938 (5)
Cl2	0.000000	0.62505 (6)	0.250000	0.01026 (8)
O1	0.17011 (16)	0.30132 (14)	0.06373 (10)	0.01068 (17)
O2	0.24000 (16)	0.05173 (14)	0.28059 (10)	0.01065 (17)
O3	0.44395 (16)	0.42345 (14)	0.35534 (10)	0.01033 (17)
H1A	0.063 (3)	0.262 (3)	0.047 (2)	0.027 (5)*
H1B	0.140 (4)	0.330 (3)	−0.008 (3)	0.030 (6)*
H2A	0.253 (4)	0.091 (3)	0.348 (2)	0.029 (6)*
H2B	0.188 (3)	−0.059 (3)	0.260 (2)	0.026 (5)*
H3A	0.518 (4)	0.522 (3)	0.384 (2)	0.035 (6)*
H3B	0.322 (4)	0.459 (3)	0.325 (2)	0.029 (5)*

Atomic displacement parameters (Ų)

	U^11	U^22	U^33	U^12	U^13	U^23
Ho1	0.00520 (4)	0.00572 (4)	0.00561 (4)	0.000	0.00329 (3)	0.000
Cl1	0.00892 (13)	0.00922 (11)	0.00888 (12)	−0.00084 (9)	0.00478 (11)	−0.00183 (9)
Cl2	0.00948 (18)	0.01124 (17)	0.01035 (18)	0.000	0.00613 (16)	0.000
O1	0.0081 (4)	0.0135 (4)	0.0091 (4)	0.0002 (3)	0.0045 (4)	0.0023 (3)
O2	0.0122 (4)	0.0098 (4)	0.0130 (4)	−0.0027 (3)	0.0092 (4)	−0.0023 (3)
O3	0.0085 (4)	0.0092 (4)	0.0135 (4)	−0.0011 (3)	0.0067 (4)	−0.0027 (3)

Geometric parameters (Å, º)

Ho1—Cl1^i	2.7425 (3)	Ho1—O3^i	2.3372 (9)
Ho1—Cl1	2.7425 (3)	O1—H1A	0.78 (2)
Ho1—O1	2.3646 (10)	O1—H1B	0.76 (2)
Ho1—O1^i	2.3646 (10)	O2—H2A	0.79 (2)
Ho1—O2^i	2.3706 (9)	O2—H2B	0.79 (2)
Ho1—O2	2.3705 (9)	O3—H3A	0.79 (2)
Ho1—O3	2.3372 (9)	O3—H3B	0.82 (2)
Cl1—Ho1—Cl1^i	83.578 (12)	O3^i—Ho1—O1^i	75.86 (3)
O1^i—Ho1—Cl1^i	76.33 (2)	O3—Ho1—O1^i	69.40 (3)
O1—Ho1—Cl1	76.33 (2)	O3^i—Ho1—O1	69.41 (3)
O1—Ho1—Cl1^i	146.51 (3)	O3—Ho1—O1	75.86 (3)
O1^i—Ho1—Cl1	146.51 (3)	O3—Ho1—O2	70.61 (3)
O1—Ho1—O1^i	132.74 (5)	O3^i—Ho1—O2^i	70.61 (3)
O1^i—Ho1—O2	121.30 (3)	O3^i—Ho1—O2	138.55 (3)
O1^i—Ho1—O2^i	72.88 (3)	O3—Ho1—O2^i	138.55 (3)
O1—Ho1—O2	72.88 (3)	O3^i—Ho1—O3	83.96 (5)
O1—Ho1—O2^i	121.31 (3)	Ho1—O1—H1A	120.3 (16)
O2—Ho1—Cl1	78.70 (2)	Ho1—O1—H1B	125.2 (17)
O2^i—Ho1—Cl1^i	78.70 (2)	H1A—O1—H1B	104 (2)
O2—Ho1—Cl1^i	77.13 (2)	Ho1—O2—H2A	118.2 (16)
O2^i—Ho1—Cl1	77.13 (2)	Ho1—O2—H2B	122.9 (15)
O2—Ho1—O2^i	147.38 (5)	H2A—O2—H2B	109 (2)
O3—Ho1—Cl1	143.35 (3)	Ho1—O3—H3A	120.6 (16)
O3—Ho1—Cl1^i	107.83 (2)	Ho1—O3—H3B	121.1 (14)
O3^i—Ho1—Cl1	107.83 (2)	H3A—O3—H3B	109 (2)
O3^i—Ho1—Cl1^i	143.35 (3)

Symmetry code: (i) −x+1, y, −z+1/2.

Hydrogen-bond geometry (Å, º)

D—H···A	D—H	H···A	D···A	D—H···A
O1—H1A···Cl1^ii	0.78 (2)	2.40 (2)	3.1589 (11)	166 (2)
O1—H1B···Cl2^iii	0.76 (2)	2.41 (2)	3.1678 (10)	170 (2)
O2—H2A···Cl1^iv	0.79 (2)	2.37 (2)	3.1546 (10)	172 (2)
O2—H2B···Cl2^v	0.79 (2)	2.48 (2)	3.2320 (10)	161.6 (19)
O3—H3A···Cl1^vi	0.79 (2)	2.35 (2)	3.1309 (10)	172 (2)
O3—H3B···Cl2	0.82 (2)	2.36 (2)	3.1765 (10)	168.9 (19)

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

Hexaaquadichloridoerbium(III) chloride (Er)

Crystal data

[ErCl2(H2O)6]Cl	F(000) = 358
Mr = 381.71	Dx = 2.648 Mg m^−3
Monoclinic, P2/c	Ag Kα radiation, λ = 0.56086 Å
a = 7.8035 (2) Å	Cell parameters from 9658 reflections
b = 6.4488 (2) Å	θ = 2.5–23.7°
c = 11.9182 (4) Å	µ = 5.07 mm^−1
β = 127.044 (1)°	T = 100 K
V = 478.71 (3) Å^3	Plate, pink
Z = 2	0.23 × 0.22 × 0.17 mm

Data collection

Bruker D8 Venture Duo diffractometer	1479 reflections with I > 2σ(I)
ω scans	Rint = 0.034
Absorption correction: multi-scan SADABS-2016/2 (Bruker, 2016)	θmax = 23.7°, θmin = 2.5°
Tmin = 0.175, Tmax = 0.257	h = −11→10
24599 measured reflections	k = −9→9
1481 independent reflections	l = −17→17

Refinement

Refinement on F^2	Hydrogen site location: difference Fourier map
Least-squares matrix: full	All H-atom parameters refined
R[F^2 > 2σ(F^2)] = 0.009	w = 1/[σ^2(Fo^2) + (0.0069P)^2 + 0.1191P] where P = (Fo^2 + 2Fc^2)/3
wR(F^2) = 0.020	(Δ/σ)max = 0.001
S = 1.30	Δρmax = 0.47 e Å^−3
1481 reflections	Δρmin = −0.88 e Å^−3
72 parameters	Extinction correction: SHELXL-2018/1 (Sheldrick 2015b), Fc^*=kFc[1+0.001xFc^2λ^3/sin(2θ)]^-1/4
0 restraints	Extinction coefficient: 0.0321 (9)
Primary atom site location: structure-invariant direct methods

Special details

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.

Fractional atomic coordinates and isotropic or equivalent isotropic displacement parameters (Ų)

	x	y	z	Uiso*/Ueq
Er1	0.500000	0.15555 (2)	0.250000	0.00519 (3)
Cl1	0.29999 (4)	−0.16033 (4)	0.05990 (3)	0.00919 (5)
Cl2	0.000000	0.62527 (6)	0.250000	0.00995 (7)
O1	0.17058 (14)	0.30150 (14)	0.06411 (10)	0.01031 (15)
O2	0.24065 (14)	0.05247 (15)	0.28058 (10)	0.01036 (15)
O3	0.44402 (15)	0.42330 (14)	0.35511 (10)	0.01044 (15)
H1A	0.062 (4)	0.263 (4)	0.048 (2)	0.029 (5)*
H1B	0.141 (4)	0.332 (3)	−0.007 (3)	0.029 (6)*
H2A	0.259 (4)	0.083 (4)	0.348 (2)	0.027 (5)*
H2B	0.193 (3)	−0.061 (4)	0.263 (2)	0.024 (5)*
H3A	0.518 (4)	0.519 (4)	0.380 (2)	0.029 (5)*
H3B	0.327 (4)	0.455 (4)	0.323 (2)	0.030 (5)*

Atomic displacement parameters (Ų)

	U^11	U^22	U^33	U^12	U^13	U^23
Er1	0.00491 (4)	0.00568 (4)	0.00476 (4)	0.000	0.00279 (3)	0.000
Cl1	0.00883 (11)	0.00906 (12)	0.00820 (12)	−0.00080 (8)	0.00435 (10)	−0.00190 (8)
Cl2	0.00931 (15)	0.01105 (16)	0.00951 (16)	0.000	0.00568 (14)	0.000
O1	0.0075 (4)	0.0128 (4)	0.0083 (4)	0.0003 (3)	0.0036 (3)	0.0022 (3)
O2	0.0119 (4)	0.0105 (4)	0.0110 (4)	−0.0024 (3)	0.0081 (3)	−0.0017 (3)
O3	0.0087 (4)	0.0091 (4)	0.0130 (4)	−0.0011 (3)	0.0063 (3)	−0.0033 (3)

Geometric parameters (Å, º)

Er1—Cl1	2.7309 (3)	Er1—O3^i	2.3239 (9)
Er1—Cl1^i	2.7309 (3)	O1—H1A	0.78 (2)
Er1—O1	2.3538 (9)	O1—H1B	0.76 (3)
Er1—O1^i	2.3538 (9)	O2—H2A	0.76 (2)
Er1—O2^i	2.3579 (9)	O2—H2B	0.79 (2)
Er1—O2	2.3578 (9)	O3—H3A	0.77 (2)
Er1—O3	2.3239 (9)	O3—H3B	0.78 (2)
Cl1^i—Er1—Cl1	83.525 (12)	O3^i—Er1—O1^i	75.93 (3)
O1^i—Er1—Cl1	146.45 (2)	O3—Er1—O1^i	69.45 (3)
O1—Er1—Cl1^i	146.45 (2)	O3^i—Er1—O1	69.45 (3)
O1—Er1—Cl1	76.30 (2)	O3—Er1—O1	75.93 (3)
O1^i—Er1—Cl1^i	76.30 (2)	O3—Er1—O2	70.65 (3)
O1—Er1—O1^i	132.86 (5)	O3^i—Er1—O2^i	70.65 (3)
O1^i—Er1—O2	121.31 (3)	O3^i—Er1—O2	138.62 (3)
O1^i—Er1—O2^i	72.89 (3)	O3—Er1—O2^i	138.62 (3)
O1—Er1—O2	72.89 (3)	O3^i—Er1—O3	84.03 (5)
O1—Er1—O2^i	121.31 (3)	Er1—O1—H1A	120.7 (17)
O2—Er1—Cl1^i	77.07 (2)	Er1—O1—H1B	125.5 (19)
O2^i—Er1—Cl1	77.07 (2)	H1A—O1—H1B	104 (2)
O2—Er1—Cl1	78.64 (2)	Er1—O2—H2A	117.7 (17)
O2^i—Er1—Cl1^i	78.64 (2)	Er1—O2—H2B	122.2 (15)
O2—Er1—O2^i	147.25 (5)	H2A—O2—H2B	106 (2)
O3—Er1—Cl1^i	107.82 (2)	Er1—O3—H3A	117.0 (17)
O3—Er1—Cl1	143.35 (2)	Er1—O3—H3B	118.2 (17)
O3^i—Er1—Cl1^i	143.35 (2)	H3A—O3—H3B	112 (2)
O3^i—Er1—Cl1	107.82 (2)

Symmetry code: (i) −x+1, y, −z+1/2.

Hydrogen-bond geometry (Å, º)

D—H···A	D—H	H···A	D···A	D—H···A
O1—H1A···Cl1^ii	0.78 (2)	2.39 (2)	3.1557 (10)	166 (2)
O1—H1B···Cl2^iii	0.76 (3)	2.41 (3)	3.1632 (10)	170 (2)
O2—H2A···Cl1^iv	0.76 (2)	2.39 (2)	3.1502 (10)	176 (2)
O2—H2B···Cl2^v	0.79 (2)	2.47 (2)	3.2287 (10)	161 (2)
O3—H3A···Cl1^vi	0.77 (2)	2.36 (2)	3.1286 (10)	172 (2)
O3—H3B···Cl2	0.78 (2)	2.41 (2)	3.1689 (9)	167 (2)

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

Hexaaquadichloridotantalum(III) chloride (Tm)

Crystal data

[TmCl2(H2O)6]Cl	F(000) = 360
Mr = 383.38	Dx = 2.671 Mg m^−3
Monoclinic, P2/c	Ag Kα radiation, λ = 0.56086 Å
a = 7.7889 (4) Å	Cell parameters from 9923 reflections
b = 6.4490 (3) Å	θ = 2.6–23.7°
c = 11.8760 (6) Å	µ = 5.37 mm^−1
β = 126.961 (1)°	T = 100 K
V = 476.66 (4) Å^3	Plate, colorless
Z = 2	0.17 × 0.11 × 0.10 mm

Data collection

Bruker D8 Venture Duo diffractometer	1464 reflections with I > 2σ(I)
ω scans	Rint = 0.033
Absorption correction: multi-scan SADABS-2016/2 (Bruker, 2016)	θmax = 23.7°, θmin = 2.5°
Tmin = 0.207, Tmax = 0.257	h = −11→11
16364 measured reflections	k = −9→9
1481 independent reflections	l = −17→16

Refinement

Refinement on F^2	Hydrogen site location: difference Fourier map
Least-squares matrix: full	All H-atom parameters refined
R[F^2 > 2σ(F^2)] = 0.007	w = 1/[σ^2(Fo^2) + 0.0685P] where P = (Fo^2 + 2Fc^2)/3
wR(F^2) = 0.016	(Δ/σ)max = 0.001
S = 1.15	Δρmax = 0.39 e Å^−3
1481 reflections	Δρmin = −0.48 e Å^−3
72 parameters	Extinction correction: SHELXL-2018/1 (Sheldrick 2015b), Fc^*=kFc[1+0.001xFc^2λ^3/sin(2θ)]^-1/4
0 restraints	Extinction coefficient: 0.0056 (5)
Primary atom site location: dual

Special details

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.

Fractional atomic coordinates and isotropic or equivalent isotropic displacement parameters (Ų)

	x	y	z	Uiso*/Ueq
Tm1	0.500000	0.15657 (2)	0.250000	0.00505 (3)
Cl1	0.30008 (4)	−0.15947 (3)	0.06069 (2)	0.00896 (4)
Cl2	0.000000	0.62678 (5)	0.250000	0.00941 (6)
O1	0.17163 (12)	0.30137 (11)	0.06506 (8)	0.00987 (13)
O2	0.24195 (12)	0.05360 (12)	0.28076 (8)	0.00989 (13)
O3	0.44427 (13)	0.42399 (11)	0.35464 (8)	0.01000 (13)
H1A	0.072 (3)	0.261 (3)	0.050 (2)	0.032 (5)*
H1B	0.140 (3)	0.331 (2)	−0.012 (2)	0.020 (4)*
H2A	0.252 (3)	0.089 (3)	0.347 (2)	0.033 (5)*
H2B	0.197 (3)	−0.052 (3)	0.2624 (18)	0.019 (4)*
H3A	0.518 (3)	0.523 (3)	0.3800 (19)	0.028 (4)*
H3B	0.332 (3)	0.458 (3)	0.3247 (19)	0.023 (4)*

Atomic displacement parameters (Ų)

	U^11	U^22	U^33	U^12	U^13	U^23
Tm1	0.00468 (3)	0.00528 (3)	0.00526 (3)	0.000	0.00302 (2)	0.000
Cl1	0.00875 (9)	0.00886 (9)	0.00844 (9)	−0.00085 (7)	0.00472 (8)	−0.00185 (7)
Cl2	0.00877 (13)	0.01055 (13)	0.00955 (13)	0.000	0.00584 (12)	0.000
O1	0.0068 (3)	0.0126 (3)	0.0084 (3)	0.0002 (2)	0.0037 (3)	0.0021 (2)
O2	0.0117 (3)	0.0094 (3)	0.0117 (3)	−0.0028 (3)	0.0087 (3)	−0.0021 (3)
O3	0.0085 (3)	0.0087 (3)	0.0134 (3)	−0.0013 (3)	0.0069 (3)	−0.0033 (2)

Geometric parameters (Å, º)

Tm1—Cl1	2.7246 (2)	Tm1—O3^i	2.3142 (7)
Tm1—Cl1^i	2.7246 (2)	O1—H1A	0.73 (2)
Tm1—O1^i	2.3414 (7)	O1—H1B	0.81 (2)
Tm1—O1	2.3414 (7)	O2—H2A	0.78 (2)
Tm1—O2^i	2.3446 (8)	O2—H2B	0.737 (18)
Tm1—O2	2.3446 (8)	O3—H3A	0.789 (19)
Tm1—O3	2.3142 (7)	O3—H3B	0.75 (2)
Cl1^i—Tm1—Cl1	83.158 (10)	O3^i—Tm1—O1	69.57 (3)
O1—Tm1—Cl1	76.368 (19)	O3—Tm1—O1	75.80 (3)
O1^i—Tm1—Cl1^i	76.368 (19)	O3^i—Tm1—O1^i	75.80 (3)
O1^i—Tm1—Cl1	146.34 (2)	O3—Tm1—O1^i	69.57 (3)
O1—Tm1—Cl1^i	146.34 (2)	O3—Tm1—O2	70.87 (3)
O1^i—Tm1—O1	132.99 (4)	O3^i—Tm1—O2^i	70.87 (3)
O1—Tm1—O2	72.77 (3)	O3^i—Tm1—O2	138.58 (3)
O1—Tm1—O2^i	121.47 (3)	O3—Tm1—O2^i	138.58 (3)
O1^i—Tm1—O2	121.47 (3)	O3^i—Tm1—O3	83.65 (4)
O1^i—Tm1—O2^i	72.77 (3)	Tm1—O1—H1A	118.9 (16)
O2—Tm1—Cl1^i	77.157 (19)	Tm1—O1—H1B	124.8 (13)
O2^i—Tm1—Cl1	77.156 (19)	H1A—O1—H1B	105 (2)
O2—Tm1—Cl1	78.38 (2)	Tm1—O2—H2A	120.0 (15)
O2^i—Tm1—Cl1^i	78.38 (2)	Tm1—O2—H2B	120.9 (14)
O2—Tm1—O2^i	147.09 (4)	H2A—O2—H2B	108 (2)
O3—Tm1—Cl1^i	108.24 (2)	Tm1—O3—H3A	118.8 (14)
O3—Tm1—Cl1	143.31 (2)	Tm1—O3—H3B	120.2 (13)
O3^i—Tm1—Cl1^i	143.31 (2)	H3A—O3—H3B	108.5 (19)
O3^i—Tm1—Cl1	108.24 (2)

Symmetry code: (i) −x+1, y, −z+1/2.

Hydrogen-bond geometry (Å, º)

D—H···A	D—H	H···A	D···A	D—H···A
O1—H1A···Cl1^ii	0.73 (2)	2.44 (2)	3.1573 (8)	165 (2)
O1—H1B···Cl2^iii	0.81 (2)	2.36 (2)	3.1602 (8)	169.7 (16)
O2—H2A···Cl1^iv	0.78 (2)	2.38 (2)	3.1485 (8)	173.4 (19)
O2—H2B···Cl2^v	0.737 (18)	2.528 (18)	3.2301 (8)	159.7 (18)
O3—H3A···Cl1^vi	0.789 (19)	2.343 (19)	3.1280 (8)	173.4 (18)
O3—H3B···Cl2	0.75 (2)	2.43 (2)	3.1714 (8)	169.4 (17)

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

Hexaaquadichloridoytterbium(III) chloride (Yb)

Crystal data

[YbCl2(H2O)6]Cl	F(000) = 362
Mr = 387.49	Dx = 2.717 Mg m^−3
Monoclinic, P2/c	Ag Kα radiation, λ = 0.56086 Å
a = 7.7666 (2) Å	Cell parameters from 9892 reflections
b = 6.4305 (2) Å	θ = 3.0–23.7°
c = 11.8745 (3) Å	µ = 5.69 mm^−1
β = 126.991 (1)°	T = 100 K
V = 473.69 (2) Å^3	Plate, colorless
Z = 2	0.30 × 0.23 × 0.20 mm

Data collection

Bruker D8 Venture Duo diffractometer	1439 reflections with I > 2σ(I)
ω scans	Rint = 0.035
Absorption correction: multi-scan SADABS-2016/2 (Bruker, 2016)	θmax = 23.7°, θmin = 2.5°
Tmin = 0.168, Tmax = 0.257	h = −11→11
19224 measured reflections	k = −9→9
1464 independent reflections	l = −16→16

Refinement

Refinement on F^2	Hydrogen site location: difference Fourier map
Least-squares matrix: full	All H-atom parameters refined
R[F^2 > 2σ(F^2)] = 0.008	w = 1/[σ^2(Fo^2) + (0.0064P)^2] where P = (Fo^2 + 2Fc^2)/3
wR(F^2) = 0.017	(Δ/σ)max = 0.001
S = 1.19	Δρmax = 0.62 e Å^−3
1464 reflections	Δρmin = −0.74 e Å^−3
72 parameters	Extinction correction: SHELXL-2018/1 (Sheldrick 2015b), Fc^*=kFc[1+0.001xFc^2λ^3/sin(2θ)]^-1/4
0 restraints	Extinction coefficient: 0.0290 (7)
Primary atom site location: dual

Special details

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.

Fractional atomic coordinates and isotropic or equivalent isotropic displacement parameters (Ų)

	x	y	z	Uiso*/Ueq
Yb1	0.500000	0.15772 (2)	0.250000	0.00506 (3)
Cl1	0.30072 (4)	−0.15810 (3)	0.06078 (3)	0.00886 (5)
Cl2	0.000000	0.62670 (5)	0.250000	0.00966 (7)
O1	0.17225 (14)	0.30159 (13)	0.06541 (9)	0.01013 (15)
O2	0.24258 (13)	0.05444 (13)	0.28053 (9)	0.00973 (15)
O3	0.44456 (14)	0.42323 (12)	0.35473 (9)	0.01004 (15)
H1A	0.069 (3)	0.261 (3)	0.047 (2)	0.030 (5)*
H1B	0.148 (3)	0.330 (3)	−0.003 (2)	0.025 (5)*
H2A	0.257 (3)	0.085 (3)	0.344 (2)	0.028 (5)*
H2B	0.193 (3)	−0.059 (3)	0.2600 (19)	0.022 (4)*
H3A	0.509 (3)	0.516 (3)	0.3768 (19)	0.025 (5)*
H3B	0.318 (3)	0.461 (3)	0.321 (2)	0.026 (4)*

Atomic displacement parameters (Ų)

	U^11	U^22	U^33	U^12	U^13	U^23
Yb1	0.00471 (4)	0.00511 (4)	0.00532 (4)	0.000	0.00301 (3)	0.000
Cl1	0.00835 (11)	0.00860 (10)	0.00832 (12)	−0.00077 (8)	0.00433 (10)	−0.00180 (8)
Cl2	0.00878 (15)	0.01064 (14)	0.00987 (17)	0.000	0.00577 (14)	0.000
O1	0.0073 (4)	0.0127 (3)	0.0087 (4)	0.0002 (3)	0.0040 (3)	0.0025 (3)
O2	0.0110 (4)	0.0096 (3)	0.0111 (4)	−0.0024 (3)	0.0079 (3)	−0.0020 (3)
O3	0.0084 (3)	0.0081 (3)	0.0137 (4)	−0.0015 (3)	0.0066 (3)	−0.0030 (3)

Geometric parameters (Å, º)

Yb1—Cl1	2.7173 (3)	Yb1—H2A	2.74 (2)
Yb1—Cl1^i	2.7173 (3)	Yb1—H3A	2.729 (18)
Yb1—O1	2.3293 (8)	O1—H1A	0.74 (2)
Yb1—O1^i	2.3293 (8)	O1—H1B	0.74 (2)
Yb1—O2^i	2.3329 (8)	O2—H2A	0.72 (2)
Yb1—O2	2.3328 (8)	O2—H2B	0.795 (19)
Yb1—O3^i	2.3003 (8)	O3—H3A	0.720 (19)
Yb1—O3	2.3003 (8)	O3—H3B	0.84 (2)
Cl1^i—Yb1—Cl1	83.270 (11)	O3^i—Yb1—Cl1	107.85 (2)
Cl1^i—Yb1—H2A	74.1 (4)	O3^i—Yb1—Cl1^i	143.42 (2)
Cl1—Yb1—H2A	91.1 (4)	O3—Yb1—Cl1^i	107.85 (2)
Cl1—Yb1—H3A	154.1 (4)	O3—Yb1—Cl1	143.42 (2)
Cl1^i—Yb1—H3A	111.2 (4)	O3^i—Yb1—O1^i	76.11 (3)
O1^i—Yb1—Cl1^i	76.26 (2)	O3—Yb1—O1^i	69.54 (3)
O1—Yb1—Cl1^i	146.22 (2)	O3^i—Yb1—O1	69.55 (3)
O1^i—Yb1—Cl1	146.22 (2)	O3—Yb1—O1	76.11 (3)
O1—Yb1—Cl1	76.26 (2)	O3—Yb1—O2^i	138.77 (3)
O1—Yb1—O1^i	133.20 (4)	O3—Yb1—O2	70.77 (3)
O1—Yb1—O2^i	121.35 (3)	O3^i—Yb1—O2^i	70.77 (3)
O1—Yb1—O2	72.89 (3)	O3^i—Yb1—O2	138.77 (3)
O1^i—Yb1—O2	121.35 (3)	O3—Yb1—O3^i	84.16 (4)
O1^i—Yb1—O2^i	72.89 (3)	O3—Yb1—H2A	60.6 (4)
O1^i—Yb1—H2A	108.3 (4)	O3^i—Yb1—H2A	138.0 (4)
O1—Yb1—H2A	79.7 (4)	O3—Yb1—H3A	13.3 (4)
O1—Yb1—H3A	80.5 (4)	O3^i—Yb1—H3A	73.8 (4)
O1^i—Yb1—H3A	59.6 (4)	H2A—Yb1—H3A	73.5 (6)
O2^i—Yb1—Cl1^i	78.50 (2)	Yb1—O1—H1A	120.9 (16)
O2—Yb1—Cl1	78.50 (2)	Yb1—O1—H1B	122.8 (16)
O2—Yb1—Cl1^i	76.92 (2)	H1A—O1—H1B	105 (2)
O2^i—Yb1—Cl1	76.92 (2)	Yb1—O2—H2A	118.2 (16)
O2—Yb1—O2^i	146.92 (4)	Yb1—O2—H2B	121.4 (12)
O2^i—Yb1—H2A	151.2 (4)	H2A—O2—H2B	108 (2)
O2—Yb1—H2A	13.3 (4)	Yb1—O3—H3A	119.6 (14)
O2—Yb1—H3A	84.0 (4)	Yb1—O3—H3B	120.0 (13)
O2^i—Yb1—H3A	125.8 (4)	H3A—O3—H3B	107.0 (18)

Symmetry code: (i) −x+1, y, −z+1/2.

Hydrogen-bond geometry (Å, º)

D—H···A	D—H	H···A	D···A	D—H···A
O1—H1A···Cl1^ii	0.74 (2)	2.43 (2)	3.1570 (9)	168 (2)
O1—H1B···Cl2^iii	0.74 (2)	2.44 (2)	3.1623 (9)	167 (2)
O2—H2A···Cl1^iv	0.72 (2)	2.44 (2)	3.1486 (9)	175 (2)
O2—H2B···Cl2^v	0.795 (19)	2.472 (19)	3.2287 (9)	159.5 (16)
O3—H3A···Cl1^vi	0.720 (19)	2.409 (19)	3.1273 (9)	175.4 (19)
O3—H3B···Cl2	0.84 (2)	2.33 (2)	3.1643 (8)	168.8 (17)

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

Hexaaquadichloridolutetium(III) chloride (Lu)

Crystal data

[LuCl2(H2O)6]Cl	F(000) = 364
Mr = 389.42	Dx = 2.737 Mg m^−3
Monoclinic, P2/c	Ag Kα radiation, λ = 0.56086 Å
a = 7.7621 (3) Å	Cell parameters from 9948 reflections
b = 6.4241 (3) Å	θ = 2.5–23.7°
c = 11.8671 (5) Å	µ = 6.00 mm^−1
β = 127.008 (1)°	T = 100 K
V = 472.54 (4) Å^3	Plate, colorless
Z = 2	0.17 × 0.14 × 0.14 mm

Data collection

Bruker D8 Venture Duo diffractometer	1436 reflections with I > 2σ(I)
ω scans	Rint = 0.041
Absorption correction: multi-scan SADABS-2016/2 (Bruker, 2016)	θmax = 23.7°, θmin = 2.5°
Tmin = 0.201, Tmax = 0.257	h = −11→11
23799 measured reflections	k = −9→9
1464 independent reflections	l = −16→17

Refinement

Refinement on F^2	Hydrogen site location: difference Fourier map
Least-squares matrix: full	All H-atom parameters refined
R[F^2 > 2σ(F^2)] = 0.009	w = 1/[σ^2(Fo^2) + 0.3367P] where P = (Fo^2 + 2Fc^2)/3
wR(F^2) = 0.020	(Δ/σ)max < 0.001
S = 1.28	Δρmax = 0.78 e Å^−3
1464 reflections	Δρmin = −0.82 e Å^−3
72 parameters	Extinction correction: SHELXL-2018/1 (Sheldrick 2015b), Fc^*=kFc[1+0.001xFc^2λ^3/sin(2θ)]^-1/4
0 restraints	Extinction coefficient: 0.0094 (5)
Primary atom site location: dual

Special details

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.

Fractional atomic coordinates and isotropic or equivalent isotropic displacement parameters (Ų)

	x	y	z	Uiso*/Ueq
Lu1	0.500000	0.15824 (2)	0.250000	0.00529 (4)
Cl1	0.30110 (5)	−0.15719 (6)	0.06103 (4)	0.00912 (6)
Cl2	0.000000	0.62590 (8)	0.250000	0.00994 (9)
O1	0.17244 (18)	0.30166 (18)	0.06562 (12)	0.0104 (2)
O2	0.24293 (19)	0.05447 (19)	0.28021 (12)	0.0101 (2)
O3	0.4452 (2)	0.42271 (19)	0.35486 (12)	0.0102 (2)
H1A	0.070 (4)	0.258 (4)	0.052 (3)	0.027 (7)*
H1B	0.142 (4)	0.328 (4)	−0.007 (3)	0.022 (6)*
H2A	0.255 (4)	0.086 (4)	0.344 (3)	0.028 (7)*
H2B	0.193 (4)	−0.064 (5)	0.261 (3)	0.033 (7)*
H3A	0.517 (5)	0.523 (5)	0.378 (3)	0.037 (8)*
H3B	0.328 (4)	0.454 (4)	0.322 (3)	0.026 (7)*

Atomic displacement parameters (Ų)

	U^11	U^22	U^33	U^12	U^13	U^23
Lu1	0.00480 (5)	0.00564 (5)	0.00535 (4)	0.000	0.00301 (3)	0.000
Cl1	0.00841 (14)	0.00916 (14)	0.00864 (14)	−0.00059 (12)	0.00451 (12)	−0.00171 (12)
Cl2	0.0089 (2)	0.0111 (2)	0.0103 (2)	0.000	0.00602 (18)	0.000
O1	0.0070 (5)	0.0131 (5)	0.0093 (5)	−0.0002 (4)	0.0039 (4)	0.0021 (4)
O2	0.0110 (5)	0.0107 (5)	0.0115 (5)	−0.0028 (4)	0.0083 (4)	−0.0020 (4)
O3	0.0076 (5)	0.0097 (5)	0.0130 (5)	−0.0010 (4)	0.0061 (4)	−0.0028 (4)

Geometric parameters (Å, º)

Lu1—Cl1^i	2.7113 (4)	Lu1—O3^i	2.2917 (12)
Lu1—Cl1	2.7113 (4)	O1—H1A	0.77 (3)
Lu1—O1^i	2.3246 (11)	O1—H1B	0.76 (3)
Lu1—O1	2.3246 (11)	O2—H2A	0.73 (3)
Lu1—O2^i	2.3272 (12)	O2—H2B	0.82 (3)
Lu1—O2	2.3272 (12)	O3—H3A	0.79 (3)
Lu1—O3	2.2917 (12)	O3—H3B	0.77 (3)
Cl1—Lu1—Cl1^i	83.270 (15)	O3^i—Lu1—O1	69.54 (4)
O1—Lu1—Cl1^i	146.14 (3)	O3—Lu1—O1	76.23 (4)
O1^i—Lu1—Cl1	146.14 (3)	O3^i—Lu1—O1^i	76.23 (4)
O1^i—Lu1—Cl1^i	76.23 (3)	O3—Lu1—O1^i	69.53 (4)
O1—Lu1—Cl1	76.23 (3)	O3—Lu1—O2	70.87 (4)
O1^i—Lu1—O1	133.30 (6)	O3^i—Lu1—O2^i	70.87 (4)
O1—Lu1—O2	72.85 (4)	O3^i—Lu1—O2	138.80 (4)
O1—Lu1—O2^i	121.47 (4)	O3—Lu1—O2^i	138.80 (4)
O1^i—Lu1—O2	121.47 (4)	O3^i—Lu1—O3	84.31 (6)
O1^i—Lu1—O2^i	72.85 (4)	Lu1—O1—H1A	118 (2)
O2—Lu1—Cl1	78.41 (3)	Lu1—O1—H1B	125.0 (19)
O2^i—Lu1—Cl1^i	78.41 (3)	H1A—O1—H1B	106 (3)
O2—Lu1—Cl1^i	76.86 (3)	Lu1—O2—H2A	119 (2)
O2^i—Lu1—Cl1	76.86 (3)	Lu1—O2—H2B	121.7 (19)
O2—Lu1—O2^i	146.71 (6)	H2A—O2—H2B	107 (3)
O3—Lu1—Cl1	143.49 (3)	Lu1—O3—H3A	118 (2)
O3—Lu1—Cl1^i	107.72 (3)	Lu1—O3—H3B	117.7 (19)
O3^i—Lu1—Cl1	107.72 (3)	H3A—O3—H3B	109 (3)
O3^i—Lu1—Cl1^i	143.49 (3)

Symmetry code: (i) −x+1, y, −z+1/2.

Hydrogen-bond geometry (Å, º)

D—H···A	D—H	H···A	D···A	D—H···A
O1—H1A···Cl1^ii	0.77 (3)	2.42 (3)	3.1591 (13)	163 (3)
O1—H1B···Cl2^iii	0.76 (3)	2.40 (3)	3.1625 (12)	171 (2)
O2—H2A···Cl1^iv	0.73 (3)	2.42 (3)	3.1517 (13)	175 (3)
O2—H2B···Cl2^v	0.82 (3)	2.45 (3)	3.2327 (13)	160 (3)
O3—H3A···Cl1^vi	0.79 (3)	2.34 (3)	3.1290 (13)	174 (3)
O3—H3B···Cl2	0.77 (3)	2.41 (3)	3.1653 (12)	167 (3)

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