metal-organic compounds
The title complex, [Sm2(C6H13NO2)4(H2O)8](ClO4)6, contains dimeric [Sm2(Ile)4(H2O)8]6+cations (Ile is L-isoleucine) and perchlorate anions. The two Sm3+ cations lie on a crystallographic twofold rotation axis. The four isoleucine molecules act as bridging ligands, linking two Sm3+ ions through their carboxyl O atoms. Each Sm3+ ion is also coordinated by four water molecules to complete eightfold coordination in a square antiprismatic fashion. One of the three perchlorate anions in the asymmetric unit is disordered.
Supporting information
Crystallographic Information File (CIF) https://doi.org/10.1107/S1600536803027557/hb6004sup1.cif | |
Structure factor file (CIF format) https://doi.org/10.1107/S1600536803027557/hb6004Isup2.hkl |
CCDC reference: 231809
Key indicators
- Single-crystal X-ray study
- T = 293 K
- Mean (C-C) = 0.024 Å
- H-atom completeness 77%
- Disorder in solvent or counterion
- R factor = 0.052
- wR factor = 0.139
- Data-to-parameter ratio = 10.1
checkCIF/PLATON results
No syntax errors found
Alert level B PLAT220_ALERT_2_B Large Non-Solvent C Ueq(max)/Ueq(min) ... 3.68 Ratio PLAT242_ALERT_2_B Check Low U(eq) as Compared to Neighbors .... C3 PLAT342_ALERT_3_B Low Bond Precision on C-C bonds (x 1000) Ang ... 24 PLAT430_ALERT_2_B Short Inter D...A Contact OW1 .. O9 = 2.84 Ang. PLAT430_ALERT_2_B Short Inter D...A Contact OW2 .. O5 = 2.78 Ang. PLAT430_ALERT_2_B Short Inter D...A Contact OW3 .. O16 = 2.83 Ang. PLAT430_ALERT_2_B Short Inter D...A Contact O13' .. O13' = 2.66 Ang.
Alert level C ABSTM02_ALERT_3_C The ratio of expected to reported Tmax/Tmin(RR) is > 1.10 Tmin and Tmax reported: 0.398 0.473 Tmin and Tmax expected: 0.337 0.473 RR = 1.180 Please check that your absorption correction is appropriate. CHEMW03_ALERT_2_C The ratio of given/expected molecular weight as calculated from the _atom_site* data lies outside the range 0.99 <> 1.01 From the CIF: _cell_formula_units_Z 2 From the CIF: _chemical_formula_weight 1566.22 TEST: Calculate formula weight from _atom_site_* atom mass num sum C 12.01 24.00 288.26 H 1.01 52.00 52.42 N 14.01 4.00 56.03 O 16.00 39.99 639.83 Cl 35.45 6.00 212.65 Sm 150.36 2.00 300.72 Calculated formula weight 1549.91 PLAT041_ALERT_1_C Calc. and Rep. SumFormula Strings Differ .... ? PLAT042_ALERT_1_C Calc. and Rep. MoietyFormula Strings Differ .... ? PLAT043_ALERT_1_C Check Reported Molecular Weight ................ 1566.22 PLAT044_ALERT_1_C Calculated and Reported Dx Differ .............. ? PLAT060_ALERT_3_C Ratio Tmax/Tmin (Exp-to-Rep) (too) Large ....... 1.18 PLAT068_ALERT_1_C Reported F000 Differs from Calcd (or Missing)... ? PLAT202_ALERT_3_C Isotropic non-H Atoms in Anion/Solvent ....... = 5 PLAT221_ALERT_4_C Large Solvent/Anion O Ueq(max)/Ueq(min) ... 3.22 Ratio PLAT222_ALERT_3_C Large Non-Solvent H Ueq(max)/Ueq(min) ... 3.23 Ratio PLAT241_ALERT_2_C Check High U(eq) as Compared to Neighbors .... O1 PLAT242_ALERT_2_C Check Low U(eq) as Compared to Neighbors .... Sm1 PLAT242_ALERT_2_C Check Low U(eq) as Compared to Neighbors .... Sm2 PLAT242_ALERT_2_C Check Low U(eq) as Compared to Neighbors .... C9 PLAT244_ALERT_4_C Low Solvent U(eq) as Compared to Neighbors .... Cl3 PLAT244_ALERT_4_C Low Solvent U(eq) as Compared to Neighbors .... Cl3' PLAT244_ALERT_4_C Low Solvent U(eq) as Compared to Neighbors .... Cl1 PLAT244_ALERT_4_C Low Solvent U(eq) as Compared to Neighbors .... Cl2 PLAT302_ALERT_4_C Anion/Solvent Disorder ......................... 25.00 Perc. PLAT360_ALERT_2_C Short C(sp3)-C(sp3) Bond C3 - C4 = 1.43 Ang. PLAT430_ALERT_2_C Short Inter D...A Contact OW1 .. O13 = 2.85 Ang. PLAT430_ALERT_2_C Short Inter D...A Contact OW3 .. O10 = 2.85 Ang. PLAT430_ALERT_2_C Short Inter D...A Contact OW4 .. O6 = 2.85 Ang. PLAT432_ALERT_2_C Short Inter X...Y Contact C9 .. O14' = 2.98 Ang. PLAT432_ALERT_2_C Short Inter X...Y Contact C10 .. O13' = 2.98 Ang. PLAT432_ALERT_2_C Short Inter X...Y Contact C10 .. O15' = 2.98 Ang. PLAT432_ALERT_2_C Short Inter X...Y Contact C10 .. Cl3' = 3.23 Ang. PLAT432_ALERT_2_C Short Inter X...Y Contact C12 .. O13' = 3.00 Ang. PLAT432_ALERT_2_C Short Inter X...Y Contact C12 .. O14' = 3.00 Ang. PLAT601_ALERT_2_C Structure Contains Solvent Accessible VOIDS of . 65.00 A 3 PLAT720_ALERT_4_C Number of Unusual/Non-Standard Label(s) ........ 4 PLAT731_ALERT_1_C Bond Calc 1.45(3), Rep 1.443(12) ...... 2.50 su-Rat CL2 -O11 1.555 1.555 PLAT790_ALERT_4_C Centre of Gravity not Within Unit Cell: Resd. # 2 Cl O4 PLAT790_ALERT_4_C Centre of Gravity not Within Unit Cell: Resd. # 3 Cl O4
Alert level G FORMU01_ALERT_2_G There is a discrepancy between the atom counts in the _chemical_formula_sum and the formula from the _atom_site* data. Atom count from _chemical_formula_sum:C24 H68 Cl6 N4 O40 Sm2 Atom count from the _atom_site data: C24 H52 Cl6.002999 N4 O39.99200 CELLZ01_ALERT_1_G Difference between formula and atom_site contents detected. CELLZ01_ALERT_1_G WARNING: H atoms missing from atom site list. Is this intentional? From the CIF: _cell_formula_units_Z 2 From the CIF: _chemical_formula_sum C24 H68 Cl6 N4 O40 Sm2 TEST: Compare cell contents of formula and atom_site data atom Z*formula cif sites diff C 48.00 48.00 0.00 H 136.00 104.00 32.00 Cl 12.00 12.00 0.00 N 8.00 8.00 0.00 O 80.00 79.98 0.02 Sm 4.00 4.00 0.00 REFLT03_ALERT_4_G WARNING: Large fraction of Friedel related reflns may be needed to determine absolute structure From the CIF: _diffrn_reflns_theta_max 26.02 From the CIF: _reflns_number_total 3400 Count of symmetry unique reflns 3084 Completeness (_total/calc) 110.25% TEST3: Check Friedels for noncentro structure Estimate of Friedel pairs measured 316 Fraction of Friedel pairs measured 0.102 Are heavy atom types Z>Si present yes
0 ALERT level A = In general: serious problem 7 ALERT level B = Potentially serious problem 35 ALERT level C = Check and explain 4 ALERT level G = General alerts; check 8 ALERT type 1 CIF construction/syntax error, inconsistent or missing data 23 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 10 ALERT type 4 Improvement, methodology, query or suggestion
Computing details top
Data collection: P4 Software (Siemens, 1995); cell refinement: P4 Software; data reduction: P4 Software; program(s) used to solve structure: SHELXS97 (Sheldrick, 1990); program(s) used to refine structure: SHELXL97 (Sheldrick, 1997); molecular graphics: SHELXTL (Siemens, 1994); software used to prepare material for publication: SHELXL9.
Tetra-µ-alpha-isoleucine-bis[tetraaquasamarium(III)] hexaperchlorate top
Crystal data top
[Sm2(C6H13NO2)4(H2O)8](ClO4)6 | F(000) = 1572 |
Mr = 1566.22 | Dx = 1.759 Mg m−3 |
Monoclinic, C2 | Mo Kα radiation, λ = 0.71073 Å |
Hall symbol: C2y | Cell parameters from 26 reflections |
a = 21.682 (3) Å | θ = 5.2–13.8° |
b = 10.3815 (19) Å | µ = 2.34 mm−1 |
c = 15.177 (4) Å | T = 293 K |
β = 120.03 (3)° | Prismatic, colorless |
V = 2957.7 (14) Å3 | 0.52 × 0.40 × 0.32 mm |
Z = 2 |
Data collection top
Siemens P4 diffractometer | 3009 reflections with I > 2σ(I) |
Radiation source: fine-focus sealed tube | Rint = 0.037 |
Graphite monochromator | θmax = 26.0°, θmin = 1.9° |
ω scans | h = −25→26 |
Absorption correction: ψ scan (Sheldrick, 1983) | k = −1→12 |
Tmin = 0.398, Tmax = 0.473 | l = −18→18 |
6875 measured reflections | 3 standard reflections every 97 reflections |
3400 independent reflections | intensity decay: none |
Refinement top
Refinement on F2 | Secondary atom site location: difference Fourier map |
Least-squares matrix: full | Hydrogen site location: inferred from neighbouring sites |
R[F2 > 2σ(F2)] = 0.052 | H-atom parameters constrained |
wR(F2) = 0.139 | w = 1/[σ2(Fo2) + (0.1P)2] where P = (Fo2 + 2Fc2)/3 |
S = 1.03 | (Δ/σ)max = 0.050 |
3400 reflections | Δρmax = 1.17 e Å−3 |
338 parameters | Δρmin = −1.03 e Å−3 |
49 restraints | Absolute structure: Flack (1983), XXXX Friedel pairs |
Primary atom site location: structure-invariant direct methods | Absolute structure parameter: −0.00 (3) |
Fractional atomic coordinates and isotropic or equivalent isotropic displacement parameters (Å2) top
x | y | z | Uiso*/Ueq | Occ. (<1) | |
Sm1 | 0.5000 | 0.83519 (6) | 0.5000 | 0.0408 (2) | |
Sm2 | 0.5000 | 0.40682 (6) | 0.5000 | 0.0474 (3) | |
OW1 | 0.5542 (6) | 0.9625 (15) | 0.6591 (9) | 0.080 (4) | |
OW2 | 0.4108 (6) | 0.9822 (14) | 0.4967 (9) | 0.068 (3) | |
OW3 | 0.5533 (6) | 0.2737 (16) | 0.6536 (10) | 0.081 (4) | |
OW4 | 0.4064 (7) | 0.2632 (16) | 0.4978 (11) | 0.083 (4) | |
O1 | 0.6138 (6) | 0.7406 (15) | 0.6167 (9) | 0.067 (3) | |
O2 | 0.5993 (6) | 0.5239 (14) | 0.6034 (9) | 0.064 (3) | |
O3 | 0.4692 (5) | 0.7039 (10) | 0.5949 (8) | 0.060 (3) | |
O4 | 0.4664 (5) | 0.4947 (11) | 0.6171 (8) | 0.061 (3) | |
N1 | 0.7524 (6) | 0.7205 (18) | 0.6996 (11) | 0.092 (5) | |
H1A | 0.7417 | 0.7229 | 0.6349 | 0.110* | |
H1B | 0.7991 | 0.7096 | 0.7395 | 0.110* | |
H1C | 0.7394 | 0.7943 | 0.7155 | 0.110* | |
N2 | 0.4127 (8) | 0.5139 (14) | 0.7390 (11) | 0.082 (4) | |
H2A | 0.3970 | 0.4529 | 0.6915 | 0.098* | |
H2B | 0.3809 | 0.5264 | 0.7589 | 0.098* | |
H2C | 0.4539 | 0.4894 | 0.7921 | 0.098* | |
C1 | 0.6360 (5) | 0.618 (2) | 0.6380 (7) | 0.051 (2) | |
C2 | 0.7145 (6) | 0.613 (3) | 0.7144 (9) | 0.063 (3) | |
H2 | 0.7335 | 0.5333 | 0.7032 | 0.075* | |
C3 | 0.7267 (6) | 0.609 (2) | 0.8240 (9) | 0.068 (4) | |
H3 | 0.7046 | 0.6873 | 0.8325 | 0.081* | |
C4 | 0.6931 (10) | 0.502 (2) | 0.8424 (17) | 0.106 (7) | |
H4A | 0.7186 | 0.4246 | 0.8466 | 0.127* | |
H4B | 0.6448 | 0.4948 | 0.7877 | 0.127* | |
H4C | 0.6934 | 0.5150 | 0.9053 | 0.127* | |
C5 | 0.8078 (8) | 0.616 (5) | 0.9061 (12) | 0.132 (11) | |
H5A | 0.8309 | 0.6805 | 0.8862 | 0.159* | |
H5B | 0.8299 | 0.5336 | 0.9098 | 0.159* | |
C6 | 0.8181 (12) | 0.649 (5) | 1.0082 (14) | 0.186 (14) | |
H6A | 0.7795 | 0.6149 | 1.0147 | 0.223* | |
H6B | 0.8193 | 0.7414 | 1.0156 | 0.223* | |
H6C | 0.8623 | 0.6136 | 1.0602 | 0.223* | |
C7 | 0.4561 (5) | 0.609 (2) | 0.6316 (8) | 0.050 (3) | |
C8 | 0.4229 (6) | 0.634 (2) | 0.6973 (9) | 0.058 (3) | |
H8 | 0.3758 | 0.6723 | 0.6538 | 0.070* | |
C9 | 0.4691 (7) | 0.7350 (14) | 0.7825 (10) | 0.058 (3) | |
H9 | 0.4739 | 0.8133 | 0.7503 | 0.069* | |
C10 | 0.4309 (10) | 0.770 (2) | 0.8454 (13) | 0.095 (6) | |
H10A | 0.3820 | 0.7915 | 0.7993 | 0.114* | |
H10B | 0.4544 | 0.8426 | 0.8887 | 0.114* | |
H10C | 0.4332 | 0.6977 | 0.8862 | 0.114* | |
C11 | 0.5429 (9) | 0.682 (2) | 0.8543 (14) | 0.109 (7) | |
H11A | 0.5395 | 0.6157 | 0.8969 | 0.131* | |
H11B | 0.5618 | 0.6420 | 0.8149 | 0.131* | |
C12 | 0.5930 (12) | 0.786 (3) | 0.9206 (15) | 0.186 (14) | |
H12A | 0.5777 | 0.8676 | 0.8863 | 0.223* | |
H12B | 0.6403 | 0.7678 | 0.9340 | 0.223* | |
H12C | 0.5928 | 0.7899 | 0.9837 | 0.223* | |
Cl1 | 0.75194 (18) | 1.4054 (4) | 0.5258 (3) | 0.0687 (9) | |
O5 | 0.8066 (7) | 1.3472 (18) | 0.5142 (13) | 0.131 (6) | |
O6 | 0.6846 (7) | 1.361 (3) | 0.4326 (10) | 0.181 (13) | |
O7 | 0.7483 (7) | 1.3457 (15) | 0.6075 (8) | 0.103 (4) | |
O8 | 0.7497 (14) | 1.5386 (11) | 0.5271 (19) | 0.196 (12) | |
Cl2 | 0.7407 (2) | 1.0627 (5) | 0.7789 (4) | 0.0823 (11) | |
O9 | 0.7031 (7) | 0.9637 (14) | 0.7979 (12) | 0.116 (5) | |
O10 | 0.6914 (9) | 1.1669 (16) | 0.725 (2) | 0.244 (17) | |
O11 | 0.7652 (12) | 1.012 (2) | 0.7131 (17) | 0.207 (11) | |
O12 | 0.8003 (8) | 1.102 (3) | 0.8715 (11) | 0.195 (11) | |
Cl3 | 0.4628 (3) | 1.1715 (6) | 0.7883 (5) | 0.0844 (17)* | 0.804 (11) |
O13 | 0.4645 (12) | 1.079 (2) | 0.7237 (16) | 0.168 (11)* | 0.804 (11) |
O14 | 0.3946 (9) | 1.221 (3) | 0.7585 (19) | 0.190 (12)* | 0.804 (11) |
O15 | 0.4927 (11) | 1.117 (3) | 0.8919 (12) | 0.165 (8)* | 0.804 (11) |
O16 | 0.5115 (9) | 1.2791 (16) | 0.8028 (14) | 0.115 (6)* | 0.804 (11) |
Cl3' | 0.4814 (9) | 1.0524 (14) | 0.8173 (12) | 0.049 (5)* | 0.195 (11) |
O13' | 0.5103 (17) | 1.017 (3) | 0.9207 (17) | 0.37 (8)* | 0.195 (11) |
O14' | 0.519 (2) | 0.999 (2) | 0.771 (3) | 0.37 (8)* | 0.195 (11) |
O15' | 0.4063 (13) | 1.034 (4) | 0.757 (3) | 0.37 (8)* | 0.195 (11) |
O16' | 0.493 (3) | 1.1952 (18) | 0.818 (4) | 0.37 (8)* | 0.195 (11) |
Atomic displacement parameters (Å2) top
U11 | U22 | U33 | U12 | U13 | U23 | |
Sm1 | 0.0373 (4) | 0.0430 (5) | 0.0549 (4) | 0.000 | 0.0327 (3) | 0.000 |
Sm2 | 0.0472 (5) | 0.0399 (5) | 0.0751 (6) | 0.000 | 0.0456 (5) | 0.000 |
OW1 | 0.082 (8) | 0.081 (10) | 0.093 (7) | −0.003 (8) | 0.057 (6) | −0.019 (8) |
OW2 | 0.078 (7) | 0.056 (7) | 0.096 (7) | 0.015 (7) | 0.063 (6) | 0.011 (7) |
OW3 | 0.076 (7) | 0.076 (9) | 0.113 (9) | 0.023 (7) | 0.064 (7) | 0.046 (8) |
OW4 | 0.072 (7) | 0.067 (8) | 0.144 (11) | −0.006 (8) | 0.080 (8) | 0.006 (10) |
O1 | 0.043 (5) | 0.073 (8) | 0.086 (7) | 0.005 (5) | 0.033 (5) | −0.003 (7) |
O2 | 0.059 (6) | 0.071 (7) | 0.073 (6) | −0.011 (6) | 0.042 (5) | −0.012 (6) |
O3 | 0.063 (5) | 0.058 (7) | 0.076 (6) | −0.004 (5) | 0.049 (5) | 0.001 (5) |
O4 | 0.073 (6) | 0.050 (6) | 0.086 (6) | 0.001 (5) | 0.060 (5) | −0.002 (5) |
N1 | 0.044 (5) | 0.126 (13) | 0.113 (10) | −0.009 (7) | 0.045 (6) | 0.032 (10) |
N2 | 0.121 (11) | 0.076 (8) | 0.103 (9) | −0.013 (9) | 0.097 (10) | 0.007 (8) |
C1 | 0.046 (5) | 0.064 (7) | 0.052 (5) | 0.012 (11) | 0.032 (4) | −0.005 (11) |
C2 | 0.042 (5) | 0.071 (9) | 0.083 (7) | 0.004 (10) | 0.037 (5) | 0.008 (12) |
C3 | 0.058 (6) | 0.069 (11) | 0.081 (7) | 0.029 (9) | 0.039 (6) | 0.035 (10) |
C4 | 0.082 (11) | 0.121 (18) | 0.133 (15) | 0.019 (12) | 0.069 (11) | 0.040 (15) |
C5 | 0.065 (8) | 0.25 (3) | 0.081 (9) | 0.01 (2) | 0.031 (7) | −0.05 (2) |
C6 | 0.102 (10) | 0.35 (4) | 0.073 (7) | −0.06 (2) | 0.023 (7) | −0.027 (17) |
C7 | 0.049 (5) | 0.056 (10) | 0.061 (5) | 0.004 (7) | 0.040 (4) | 0.015 (8) |
C8 | 0.052 (5) | 0.061 (9) | 0.074 (6) | −0.006 (9) | 0.041 (5) | −0.010 (10) |
C9 | 0.063 (7) | 0.056 (7) | 0.060 (6) | −0.013 (6) | 0.035 (6) | −0.013 (6) |
C10 | 0.093 (11) | 0.117 (15) | 0.085 (10) | −0.027 (12) | 0.053 (9) | −0.026 (11) |
C11 | 0.085 (11) | 0.122 (17) | 0.082 (10) | 0.015 (12) | 0.013 (9) | −0.020 (11) |
C12 | 0.102 (10) | 0.35 (4) | 0.073 (7) | −0.06 (2) | 0.023 (7) | −0.027 (17) |
Cl1 | 0.0571 (17) | 0.085 (2) | 0.084 (2) | 0.0053 (18) | 0.0500 (17) | 0.0065 (19) |
O5 | 0.097 (10) | 0.143 (15) | 0.196 (16) | 0.019 (11) | 0.105 (11) | 0.041 (16) |
O6 | 0.097 (10) | 0.33 (4) | 0.124 (11) | 0.024 (19) | 0.059 (9) | 0.04 (2) |
O7 | 0.118 (9) | 0.132 (12) | 0.092 (7) | 0.010 (10) | 0.077 (7) | 0.025 (9) |
O8 | 0.32 (4) | 0.106 (13) | 0.27 (3) | −0.05 (2) | 0.23 (3) | −0.037 (18) |
Cl2 | 0.0573 (19) | 0.098 (3) | 0.095 (3) | −0.0102 (19) | 0.0408 (19) | −0.015 (2) |
O9 | 0.106 (10) | 0.101 (11) | 0.159 (13) | −0.026 (9) | 0.080 (10) | −0.013 (11) |
O10 | 0.154 (17) | 0.118 (18) | 0.54 (5) | 0.031 (15) | 0.23 (3) | 0.06 (3) |
O11 | 0.26 (2) | 0.21 (2) | 0.31 (3) | −0.01 (2) | 0.25 (2) | −0.04 (3) |
O12 | 0.138 (13) | 0.20 (2) | 0.134 (12) | −0.084 (19) | −0.015 (10) | −0.004 (19) |
Geometric parameters (Å, º) top
Sm1—O3i | 2.310 (10) | C5—C6 | 1.49 (3) |
Sm1—O3 | 2.310 (10) | C5—H5A | 0.9700 |
Sm1—OW2i | 2.445 (12) | C5—H5B | 0.9700 |
Sm1—OW2 | 2.445 (12) | C6—H6A | 0.9600 |
Sm1—O1i | 2.411 (12) | C6—H6B | 0.9600 |
Sm1—O1 | 2.411 (12) | C6—H6C | 0.9600 |
Sm1—OW1 | 2.474 (13) | C7—C8 | 1.518 (15) |
Sm1—OW1i | 2.474 (13) | C8—C9 | 1.57 (2) |
Sm2—O2 | 2.279 (13) | C8—H8 | 0.9800 |
Sm2—O2i | 2.279 (13) | C9—C10 | 1.59 (2) |
Sm2—O4i | 2.412 (9) | C9—C11 | 1.52 (2) |
Sm2—O4 | 2.412 (9) | C9—H9 | 0.9800 |
Sm2—OW3i | 2.446 (12) | C10—H10A | 0.9600 |
Sm2—OW3 | 2.446 (12) | C10—H10B | 0.9600 |
Sm2—OW4 | 2.505 (13) | C10—H10C | 0.9600 |
Sm2—OW4i | 2.505 (13) | C11—C12 | 1.51 (3) |
O1—C1 | 1.34 (3) | C11—H11A | 0.9700 |
O2—C1 | 1.20 (2) | C11—H11B | 0.9700 |
O3—C7 | 1.23 (2) | C12—H12A | 0.9600 |
O4—C7 | 1.25 (3) | C12—H12B | 0.9600 |
N1—C2 | 1.46 (3) | C12—H12C | 0.9600 |
N1—H1A | 0.8900 | Cl1—O8 | 1.385 (12) |
N1—H1B | 0.8900 | Cl1—O7 | 1.424 (9) |
N1—H1C | 0.8900 | Cl1—O5 | 1.417 (11) |
N2—C8 | 1.47 (3) | Cl1—O6 | 1.509 (13) |
N2—H2A | 0.8900 | Cl2—O12 | 1.413 (11) |
N2—H2B | 0.8900 | Cl2—O10 | 1.450 (13) |
N2—H2C | 0.8900 | Cl2—O9 | 1.428 (11) |
C1—C2 | 1.507 (14) | Cl2—O11 | 1.443 (12) |
C2—C3 | 1.550 (14) | Cl3—O14 | 1.408 (14) |
C2—H2 | 0.9800 | Cl3—O13 | 1.388 (14) |
C3—C4 | 1.43 (3) | Cl3—O15 | 1.481 (13) |
C3—C5 | 1.568 (19) | Cl3—O16 | 1.476 (14) |
C3—H3 | 0.9800 | Cl3'—O13' | 1.418 (18) |
C4—H4A | 0.9600 | Cl3'—O16' | 1.503 (17) |
C4—H4B | 0.9600 | Cl3'—O15' | 1.425 (18) |
C4—H4C | 0.9600 | Cl3'—O14' | 1.426 (19) |
O3i—Sm1—O3 | 107.7 (5) | C4—C3—C5 | 111 (2) |
O3i—Sm1—OW2i | 84.8 (4) | C4—C3—C2 | 113.6 (19) |
O3—Sm1—OW2i | 145.9 (4) | C5—C3—C2 | 111.8 (11) |
O3i—Sm1—OW2 | 145.9 (4) | C4—C3—H3 | 106.7 |
O3—Sm1—OW2 | 84.8 (4) | C5—C3—H3 | 106.6 |
OW2i—Sm1—OW2 | 102.7 (6) | C2—C3—H3 | 106.7 |
O3i—Sm1—O1i | 79.1 (4) | C3—C4—H4A | 109.5 |
O3—Sm1—O1i | 73.1 (4) | C3—C4—H4B | 109.5 |
OW2i—Sm1—O1i | 141.0 (4) | H4A—C4—H4B | 109.5 |
OW2—Sm1—O1i | 74.4 (5) | C3—C4—H4C | 109.5 |
O3i—Sm1—O1 | 73.1 (4) | H4A—C4—H4C | 109.5 |
O3—Sm1—O1 | 79.1 (4) | H4B—C4—H4C | 109.5 |
OW2i—Sm1—O1 | 74.4 (5) | C3—C5—C6 | 111.2 (14) |
OW2—Sm1—O1 | 141.0 (4) | C3—C5—H5A | 109.4 |
O1i—Sm1—O1 | 131.9 (7) | C6—C5—H5A | 109.4 |
O3i—Sm1—OW1 | 141.2 (4) | C3—C5—H5B | 109.4 |
O3—Sm1—OW1 | 81.4 (4) | C6—C5—H5B | 109.4 |
OW2i—Sm1—OW1 | 70.2 (4) | H5A—C5—H5B | 108.0 |
OW2—Sm1—OW1 | 70.8 (4) | C5—C6—H6A | 109.5 |
O1i—Sm1—OW1 | 138.3 (4) | C5—C6—H6B | 109.5 |
O1—Sm1—OW1 | 71.8 (5) | H6A—C6—H6B | 109.5 |
O3i—Sm1—OW1i | 81.4 (4) | C5—C6—H6C | 109.5 |
O3—Sm1—OW1i | 141.2 (4) | H6A—C6—H6C | 109.5 |
OW2i—Sm1—OW1i | 70.8 (4) | H6B—C6—H6C | 109.5 |
OW2—Sm1—OW1i | 70.2 (4) | O4—C7—O3 | 125.4 (11) |
O1i—Sm1—OW1i | 71.8 (5) | O4—C7—C8 | 117.7 (16) |
O1—Sm1—OW1i | 138.3 (4) | O3—C7—C8 | 116.8 (17) |
OW1—Sm1—OW1i | 115.4 (7) | N2—C8—C7 | 111.2 (17) |
O2—Sm2—O2i | 115.5 (7) | N2—C8—C9 | 112.5 (11) |
O2—Sm2—O4i | 77.0 (4) | C7—C8—C9 | 109.8 (11) |
O2i—Sm2—O4i | 79.7 (4) | N2—C8—H8 | 107.7 |
O2—Sm2—O4 | 79.7 (4) | C7—C8—H8 | 107.7 |
O2i—Sm2—O4 | 77.0 (4) | C9—C8—H8 | 107.7 |
O4i—Sm2—O4 | 135.5 (5) | C8—C9—C10 | 109.7 (11) |
O2—Sm2—OW3i | 142.2 (4) | C8—C9—C11 | 110.8 (14) |
O2i—Sm2—OW3i | 79.2 (5) | C10—C9—C11 | 109.4 (13) |
O4i—Sm2—OW3i | 71.6 (4) | C8—C9—H9 | 109.0 |
O4—Sm2—OW3i | 138.0 (4) | C10—C9—H9 | 109.0 |
O2—Sm2—OW3 | 79.2 (5) | C11—C9—H9 | 109.0 |
O2i—Sm2—OW3 | 142.2 (4) | C9—C10—H10A | 109.5 |
O4i—Sm2—OW3 | 138.0 (3) | C9—C10—H10B | 109.5 |
O4—Sm2—OW3 | 71.6 (4) | H10A—C10—H10B | 109.5 |
OW3i—Sm2—OW3 | 111.2 (8) | C9—C10—H10C | 109.5 |
O2—Sm2—OW4 | 143.8 (4) | H10A—C10—H10C | 109.5 |
O2i—Sm2—OW4 | 80.1 (5) | H10B—C10—H10C | 109.5 |
O4i—Sm2—OW4 | 139.2 (4) | C12—C11—C9 | 111.3 (18) |
O4—Sm2—OW4 | 72.2 (4) | C12—C11—H11A | 109.4 |
OW3i—Sm2—OW4 | 70.0 (4) | C9—C11—H11A | 109.4 |
OW3—Sm2—OW4 | 70.7 (5) | C12—C11—H11B | 109.4 |
O2—Sm2—OW4i | 80.1 (5) | C9—C11—H11B | 109.4 |
O2i—Sm2—OW4i | 143.8 (4) | H11A—C11—H11B | 108.0 |
O4i—Sm2—OW4i | 72.2 (4) | C11—C12—H12A | 109.5 |
O4—Sm2—OW4i | 139.2 (4) | C11—C12—H12B | 109.5 |
OW3i—Sm2—OW4i | 70.7 (5) | H12A—C12—H12B | 109.5 |
OW3—Sm2—OW4i | 70.0 (4) | C11—C12—H12C | 109.5 |
OW4—Sm2—OW4i | 106.9 (7) | H12A—C12—H12C | 109.5 |
C1—O1—Sm1 | 132.4 (10) | H12B—C12—H12C | 109.5 |
C1—O2—Sm2 | 157.7 (12) | O8—Cl1—O7 | 113.9 (10) |
C7—O3—Sm1 | 163.0 (10) | O8—Cl1—O5 | 117.7 (10) |
C7—O4—Sm2 | 129.5 (9) | O7—Cl1—O5 | 109.7 (8) |
C2—N1—H1A | 109.5 | O8—Cl1—O6 | 107.1 (11) |
C2—N1—H1B | 109.5 | O7—Cl1—O6 | 103.6 (9) |
H1A—N1—H1B | 109.5 | O5—Cl1—O6 | 103.3 (9) |
C2—N1—H1C | 109.5 | O12—Cl2—O10 | 112.9 (12) |
H1A—N1—H1C | 109.5 | O12—Cl2—O9 | 109.8 (10) |
H1B—N1—H1C | 109.5 | O10—Cl2—O9 | 108.3 (8) |
C8—N2—H2A | 109.5 | O12—Cl2—O11 | 109.0 (11) |
C8—N2—H2B | 109.5 | O10—Cl2—O11 | 107.9 (12) |
H2A—N2—H2B | 109.5 | O9—Cl2—O11 | 108.9 (10) |
C8—N2—H2C | 109.5 | O14—Cl3—O13 | 114.8 (13) |
H2A—N2—H2C | 109.5 | O14—Cl3—O15 | 108.0 (12) |
H2B—N2—H2C | 109.5 | O13—Cl3—O15 | 109.5 (13) |
O2—C1—O1 | 125.9 (11) | O14—Cl3—O16 | 109.4 (12) |
O2—C1—C2 | 124 (2) | O13—Cl3—O16 | 111.1 (11) |
O1—C1—C2 | 110.1 (19) | O15—Cl3—O16 | 103.3 (10) |
N1—C2—C1 | 111.4 (17) | O13'—Cl3'—O16' | 105.5 (16) |
N1—C2—C3 | 112.2 (17) | O13'—Cl3'—O15' | 114.0 (17) |
C1—C2—C3 | 110.2 (9) | O16'—Cl3'—O15' | 105.6 (16) |
N1—C2—H2 | 107.6 | O13'—Cl3'—O14' | 113.3 (17) |
C1—C2—H2 | 107.6 | O16'—Cl3'—O14' | 105.0 (16) |
C3—C2—H2 | 107.6 | O15'—Cl3'—O14' | 112.3 (17) |
Symmetry code: (i) −x+1, y, −z+1. |