Supporting information
Crystallographic Information File (CIF) https://doi.org/10.1107/S0108270113016557/wq3037sup1.cif | |
Structure factor file (CIF format) https://doi.org/10.1107/S0108270113016557/wq3037Isup2.hkl |
CCDC reference: 958839
In recent years, growing attention has been paid to the rational design and construction of novel functional metal–organic compounds, owing not only to their intriguing structural diversities and topologies (Ye et al., 2005; Hill et al., 2005; Hong, 2007), but also to their potential applications in many fields, such as ferroelectricity, electrical conductivity, magnetism, molecular adsorption, fluorescence and heterogeneous catalysis (Zhang et al., 2009, 2010; Zhang & Xiong, 2012; Yao et al., 2008; Nouar et al., 2008; Li et al., 2009). Numerous zero-, one-, two- and three-dimensional cadmium complexes, in which the metal centres are connected by small anionic bridging ligands such as Cl- (Willett, 1977; Charles et al., 1984; Puget et al., 1991; Jin & Wu, 2013), have been synthesized and characterized with the aim of designing new materials with interesting physical properties. The diverse structures of these CdII complexes are based on the variable coordination geometry of the metal ion, because of the wide range of different atom contacts. To the best of our knowledge, zero-dimensional [Title compound is linear, i.e. one-dimensional, not zero-dimensional. What is the connection?] cadmium complexes containing five differently coordinated Cd atoms have not been reported so far and thus structural information on such compounds is scarce. We report here the synthesis and structure determination of the title compound, (I), containing a chloride-bridged pentanuclear cluster.
In the crystal structure of (I), the asymmetric unit consists of a [Cd5Cl16(H2O)4]6- anion, two triply protonated tris[(1H-benzimidazol-3-ium-2-yl)methyl]amine cations and one solvent water molecule (Fig. 1). The complex anionic group is a linear [Cd5Cl16(H2O)4]6- pentamer interconnected by bridging (edge-sharing) chloride ligands. Five crystallographically independent CdII cations are present, linked by double chloride anion bridges to form a finite —Cd—Cl2—Cd— ribbon. In this way, the Cd1 and Cd5 centres are five-coordinated by three terminal and two bridging Cl- anions, showing a distorted trigonal–bipyramidal geometry. The Cd2 and Cd3 centres are coordinated by one water and five chloride ligands (four bridging and one terminal), leading to a distorted octahedral coordination environment in which the water ligand occupies an axial position. The Cd2—O4 bond is shorter than Cd3—O3 [2.382 (3) and 2.530 (3) Å, respectively]. The Cd4 cation is surrounded by four chloride ligands and two water molecules, giving rise to a slightly distorted octahedral geometry. The Cl—Cd—Cl angles are in the ranges 84.75 (4)–96.12 (4)° and 174.21 (4)–177.46 (4)°, and the O—Cd—O angle is 171.23 (10)°, deviating slightly from ideal octahedral angle values (90 and 180°). The Cd4—Cl bond lengths are in the range 2.5273 (12)–2.6713 (12) Å, the Cd4—O1 and Cd4—O2 bond lengths are 2.366 (3) and 2.453 (3) Å, respectively, and the Cd3···Cd2 and Cd3···Cd4 distances are 3.736 (1) and 3.719 (1) Å, respectively, both of which are less than the distances to the terminal cadmium ions, viz. Cd1···Cd2 and Cd5···Cd4 of 3.894 (1) and 3.812 (1) Å, respectively. The Cd—Cl bond lengths range from 2.4393 (12) to 2.6927 (12) Å, which appear to be shorter than those observed in the CdCl2 crystal structure (2.74 Å; Pauling & Hoard, 1930). The terminal CdII cations (Cd1 and Cd5) adopt trigonal–bipyrimadal geometries with the chloride ligands; Cl1/Cl2/Cl4 and Cl13/Cl14/Cl16 fill the basal locations for Cd1 and Cd5, respectively, while Cl2/Cl5 and Cl12/Cl15 take up the apical positions. The apical Cd—Cl bonds on the terminal CdII cations have bond lengths in the range 2.6347 (11)–2.6856 (12) Å, while the basal Cd—Cl bond lengths are in the range 2.4393 (12)–2.5843 (11) Å.
There are abundant intra- and intermolecular O—H···O, O—H···Cl, N—H···Cl and N—H···O hydrogen bonds in (I). Intramolecular O—H···Cl hydrogen bonds (O1—H1C···Cl14, O2—H2C···Cl9, O3—H3D···Cl6, O4—H4D···Cl7 and O4—H4D···Cl9; see Table 2) are generated by the water ligands and the Cl- anions in the pentamer. Three hydrogen bonds [O1—H1B···Cl1i, O3—H3C···Cl1i and O4—H4C···Cl14ii; symmetry codes: (i) x + 1, y, z; (ii) x - 1, y, z] extend the anionic groups along the a-axis direction in a zigzag chain. The solvent water molecule forms further hydrogen bonds [O2—H2D···O5ii, O5—H5C···Cl3vii and O5—H5D···Cl6vii; symmetry codes: (ii) x - 1, y, z; (vii) x + 1, y + 1, z] as a bridge to connect two [Cd5Cl16(H2O)4]6- anions oriented parallel and end-to-end to each other. Thus, these zigzag chains are linked together into two-dimensional step-like layers (Fig. 2).
The presence of the organic cations as spacers between the inorganic anions gives rise to distinctive hydrogen-bonding features which influence the structural packing. In (I), the anionic layers are well separated by the triply protonated cations. There is a network of intermolecular hydrogen-bonding interactions between the organic cations and inorganic layers (Table 2). Two kinds of intermolecular N—H···Cl and N—H···O hydrogen bonds contribute to the formation of a three-dimensional supramolecular framework (Fig. 3).
It is notable that the cation has a tweezer-like conformation, which is stabilized not only by the hydrogen bonds (Table 2) between the N atoms on the imidazole rings and the O and Cl atoms of the water molecules and the anionic clusters, respectively, but also by π–π interactions among the organic cations. Such a conformation for free tris[(benzimidazol-2-yl)methyl]amine or its protonated form has been only rarely reported so far, though it is often used as a symmetric tripodal ligand to coordinate to metal ions (Zhou et al., 2000; Miao et al., 1999). The N—H···Cl hydrogen-bond distances are in the range 3.100 (3)–3.432 (3) Å, while the N—H···O distances [N5—H5B···O3iv and N10—H10B···O2vi; symmetry code: (iv) -x + 1, -y, -z + 1; (vi) x + 1, y - 1, z] are 2.942 (4) and 2.815 (4) Å, respectively, both of which are less than the N—H···Cl distances.
The structure of (I) is further stabilised by π–π interactions between the benzene and imidazole rings of the organic cations (Fig. 4). Except for the intramolecular π–π interactions that exist in each cation with a face-to-face (FF) motif, each cation has π–π interactions with three adjacent cations with offset face-to-face (OFF) motifs (Russell et al., 2001). The smallest centroid-to-centroid distance is a Cg2···Cg3 separation of 3.305 (2) Å, while the longest one is a Cg3···Cg5 distance of 3.933 (3) Å [Cg2, Cg3 and Cg5 are the centroids of the N3/C9/C14/N4/C15, N5/C17/C22/N6/C23 and C9–C14 rings, respectively]. The dihedral angle between the N3/C9–C14/N4/C15 and N5/C17–C22/N6/C23 rings is 15.61 (8)°, and that between the N10/C33–C38/N11/C39 and N12/C41–C46/N13/C47 rings is 14.63 (9)°.
Tris[(benzimidazol-2-yl)methyl]amine was prepared by the conventional condensation of 1,2-phenylenediamine with nitrilotriacetic acid (Thompson et al., 1977). Cadmium chloride hydrate (3.0 g, 15 mmol) was dissolved in concentrated hydrochloric acid (10 ml) and tris[(benzimidazol-2-yl)methyl]amine (2.0 g, 5 mmol) was added. After stirring the mixture for several minutes, the liquid was filtered to give a clear solution. Single crystals of (I) suitable for X-ray structure analysis were obtained by slow evaporation of the solution for several days at ambient temperature.
H atoms bonded to C and N atoms were placed in calculated positions, with C—H = 0.97 Å and Uiso(H) = 1.2Ueq(C) for methylene H atoms, C—H = 0.93 Å and Uiso(H) = 1.2Ueq(C) for aromatic H atoms, and N—H = 0.86 Å and Uiso(H) = 1.2Ueq(N). Water H atoms were located in a difference Fourier synthesis and refined with an O—H distance restraint of 0.85 Å and with Uiso(H) = 1.2Ueq(O), except for atom O1, for which O—H = 0.96 Å and Uiso(H) = 1.5Ueq(O).
Data collection: CrystalClear (Rigaku, 2005); cell refinement: CrystalClear (Rigaku, 2005); data reduction: CrystalClear (Rigaku, 2005); program(s) used to solve structure: SHELXS97 (Sheldrick, 2008); program(s) used to refine structure: SHELXL97 (Sheldrick, 2008); molecular graphics: PLATON (Spek, 2009) and DIAMOND (Brandenburg & Putz, 2005); software used to prepare material for publication: SHELXL97 (Sheldrick, 2008).
(C24H24N7)2[Cd5Cl16(H2O)4]·H2O | Z = 2 |
Mr = 2040.33 | F(000) = 1992 |
Triclinic, P1 | Dx = 1.989 Mg m−3 |
Hall symbol: -P 1 | Mo Kα radiation, λ = 0.71073 Å |
a = 12.879 (3) Å | Cell parameters from 15625 reflections |
b = 13.485 (3) Å | θ = 3.0–27.5° |
c = 21.364 (4) Å | µ = 2.22 mm−1 |
α = 79.74 (3)° | T = 293 K |
β = 86.82 (3)° | Block, colourless |
γ = 68.92 (3)° | 0.24 × 0.22 × 0.20 mm |
V = 3406.6 (15) Å3 |
Rigaku SCXmini diffractometer | 13233 reflections with I > 2σ(I) |
Radiation source: fine-focus sealed tube | Rint = 0.038 |
Graphite monochromator | θmax = 27.5°, θmin = 3.0° |
ω scans | h = −16→16 |
Absorption correction: multi-scan (CrystalClear; Rigaku, 2005) | k = −17→17 |
Tmin = 0.593, Tmax = 0.642 | l = −27→27 |
35082 measured reflections | 3 standard reflections every 180 reflections |
15625 independent reflections | intensity decay: none |
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)] = 0.040 | H-atom parameters constrained |
wR(F2) = 0.076 | w = 1/[σ2(Fo2) + (0.0133P)2 + 3.8476P] where P = (Fo2 + 2Fc2)/3 |
S = 1.07 | (Δ/σ)max = 0.001 |
15625 reflections | Δρmax = 0.62 e Å−3 |
794 parameters | Δρmin = −0.80 e Å−3 |
0 restraints | Extinction correction: SHELXL97 (Sheldrick, 2008), Fc*=kFc[1+0.001xFc2λ3/sin(2θ)]-1/4 |
Primary atom site location: structure-invariant direct methods | Extinction coefficient: 0.00280 (5) |
(C24H24N7)2[Cd5Cl16(H2O)4]·H2O | γ = 68.92 (3)° |
Mr = 2040.33 | V = 3406.6 (15) Å3 |
Triclinic, P1 | Z = 2 |
a = 12.879 (3) Å | Mo Kα radiation |
b = 13.485 (3) Å | µ = 2.22 mm−1 |
c = 21.364 (4) Å | T = 293 K |
α = 79.74 (3)° | 0.24 × 0.22 × 0.20 mm |
β = 86.82 (3)° |
Rigaku SCXmini diffractometer | 13233 reflections with I > 2σ(I) |
Absorption correction: multi-scan (CrystalClear; Rigaku, 2005) | Rint = 0.038 |
Tmin = 0.593, Tmax = 0.642 | 3 standard reflections every 180 reflections |
35082 measured reflections | intensity decay: none |
15625 independent reflections |
R[F2 > 2σ(F2)] = 0.040 | 0 restraints |
wR(F2) = 0.076 | H-atom parameters constrained |
S = 1.07 | Δρmax = 0.62 e Å−3 |
15625 reflections | Δρmin = −0.80 e Å−3 |
794 parameters |
Geometry. All e.s.d.'s (except the e.s.d. in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell e.s.d.'s are taken into account individually in the estimation of e.s.d.'s in distances, angles and torsion angles; correlations between e.s.d.'s in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell e.s.d.'s is used for estimating e.s.d.'s involving l.s. planes. |
Refinement. Refinement of F2 against ALL reflections. The weighted R-factor wR and goodness of fit S are based on F2, conventional R-factors R are based on F, with F set to zero for negative F2. The threshold expression of F2 > σ(F2) is used only for calculating R-factors(gt) etc. and is not relevant to the choice of reflections for refinement. R-factors based on F2 are statistically about twice as large as those based on F, and R-factors based on ALL data will be even larger. |
x | y | z | Uiso*/Ueq | ||
Cd1 | −0.37003 (2) | 0.17841 (2) | 0.313961 (12) | 0.02621 (7) | |
Cd2 | −0.14830 (2) | 0.31472 (2) | 0.277289 (12) | 0.02745 (7) | |
Cd3 | 0.02066 (2) | 0.49276 (2) | 0.251793 (12) | 0.03022 (7) | |
Cd4 | 0.19210 (2) | 0.66662 (2) | 0.218705 (13) | 0.02983 (7) | |
Cd5 | 0.35526 (2) | 0.85597 (2) | 0.180495 (12) | 0.02644 (7) | |
Cl1 | −0.56061 (8) | 0.29319 (8) | 0.27231 (5) | 0.0420 (2) | |
Cl2 | −0.43106 (7) | 0.09588 (7) | 0.42763 (4) | 0.03199 (19) | |
Cl3 | −0.30419 (9) | −0.00264 (7) | 0.28580 (4) | 0.0419 (2) | |
Cl4 | −0.25114 (8) | 0.23990 (7) | 0.37772 (4) | 0.0331 (2) | |
Cl5 | −0.27911 (8) | 0.26390 (9) | 0.21232 (4) | 0.0419 (2) | |
Cl6 | 0.02777 (8) | 0.14529 (7) | 0.28607 (4) | 0.0361 (2) | |
Cl7 | −0.04940 (8) | 0.39343 (7) | 0.35053 (4) | 0.0329 (2) | |
Cl8 | −0.06865 (9) | 0.40761 (8) | 0.18101 (4) | 0.0386 (2) | |
Cl9 | −0.15346 (8) | 0.66576 (7) | 0.24593 (4) | 0.0347 (2) | |
Cl10 | 0.13908 (10) | 0.55746 (9) | 0.31780 (5) | 0.0513 (3) | |
Cl11 | 0.12564 (9) | 0.55784 (8) | 0.15529 (4) | 0.0404 (2) | |
Cl12 | 0.24173 (10) | 0.79124 (10) | 0.27696 (5) | 0.0581 (3) | |
Cl13 | 0.25533 (8) | 0.77274 (7) | 0.11491 (4) | 0.0368 (2) | |
Cl14 | 0.53089 (8) | 0.70960 (8) | 0.22220 (5) | 0.0492 (3) | |
Cl15 | 0.42895 (7) | 0.92269 (7) | 0.06946 (4) | 0.03008 (18) | |
Cl16 | 0.32389 (10) | 1.02939 (8) | 0.21230 (5) | 0.0488 (3) | |
O1 | 0.3799 (3) | 0.5487 (2) | 0.22152 (16) | 0.0635 (9) | |
H1B | 0.3914 | 0.4919 | 0.2576 | 0.095* | |
H1C | 0.4274 | 0.5883 | 0.2253 | 0.095* | |
O2 | 0.0018 (2) | 0.79626 (18) | 0.19833 (11) | 0.0339 (6) | |
H2D | −0.0064 | 0.8457 | 0.2199 | 0.041* | |
H2C | −0.0415 | 0.7636 | 0.2142 | 0.041* | |
O3 | 0.1765 (2) | 0.3107 (2) | 0.26600 (12) | 0.0422 (7) | |
H3C | 0.2329 | 0.3141 | 0.2443 | 0.051* | |
H3D | 0.1553 | 0.2640 | 0.2542 | 0.051* | |
O4 | −0.2878 (2) | 0.4871 (2) | 0.28028 (16) | 0.0610 (9) | |
H4C | −0.3207 | 0.5239 | 0.2458 | 0.073* | |
H4D | −0.2487 | 0.5125 | 0.2988 | 0.073* | |
C1 | 0.4447 (3) | 0.3444 (3) | 0.51401 (17) | 0.0313 (8) | |
C2 | 0.4138 (3) | 0.4037 (3) | 0.45295 (19) | 0.0400 (9) | |
H2A | 0.4304 | 0.3720 | 0.4166 | 0.048* | |
C3 | 0.3569 (3) | 0.5126 (3) | 0.4507 (2) | 0.0496 (11) | |
H3A | 0.3334 | 0.5561 | 0.4114 | 0.060* | |
C4 | 0.3335 (3) | 0.5597 (3) | 0.5049 (2) | 0.0505 (12) | |
H4A | 0.2963 | 0.6338 | 0.5005 | 0.061* | |
C5 | 0.3630 (3) | 0.5013 (3) | 0.5646 (2) | 0.0463 (11) | |
H5A | 0.3456 | 0.5334 | 0.6008 | 0.056* | |
C6 | 0.4203 (3) | 0.3916 (3) | 0.56808 (18) | 0.0346 (8) | |
C7 | 0.5128 (3) | 0.2161 (3) | 0.59702 (17) | 0.0299 (8) | |
C8 | 0.5631 (3) | 0.1091 (3) | 0.63752 (16) | 0.0320 (8) | |
H8A | 0.5945 | 0.1174 | 0.6756 | 0.038* | |
H8B | 0.5058 | 0.0788 | 0.6503 | 0.038* | |
C9 | 0.9624 (3) | −0.1278 (3) | 0.51431 (15) | 0.0228 (7) | |
C10 | 1.0445 (3) | −0.2230 (3) | 0.50286 (17) | 0.0309 (8) | |
H10A | 1.0826 | −0.2771 | 0.5357 | 0.037* | |
C11 | 1.0657 (3) | −0.2324 (3) | 0.44001 (18) | 0.0363 (9) | |
H11A | 1.1194 | −0.2952 | 0.4302 | 0.044* | |
C12 | 1.0100 (3) | −0.1514 (3) | 0.39048 (17) | 0.0378 (9) | |
H12A | 1.0278 | −0.1616 | 0.3487 | 0.045* | |
C13 | 0.9292 (3) | −0.0568 (3) | 0.40155 (17) | 0.0361 (9) | |
H13A | 0.8924 | −0.0021 | 0.3686 | 0.043* | |
C14 | 0.9059 (3) | −0.0478 (3) | 0.46493 (16) | 0.0249 (7) | |
C15 | 0.8334 (3) | 0.0024 (3) | 0.55593 (16) | 0.0255 (7) | |
C16 | 0.7535 (3) | 0.0597 (3) | 0.60236 (16) | 0.0291 (8) | |
H16A | 0.7872 | 0.0370 | 0.6445 | 0.035* | |
H16B | 0.7361 | 0.1368 | 0.5905 | 0.035* | |
C17 | 0.7938 (3) | −0.2966 (3) | 0.54095 (15) | 0.0253 (7) | |
C18 | 0.8533 (3) | −0.3994 (3) | 0.52849 (18) | 0.0350 (8) | |
H18A | 0.8857 | −0.4572 | 0.5608 | 0.042* | |
C19 | 0.8613 (3) | −0.4105 (3) | 0.46538 (19) | 0.0396 (9) | |
H19A | 0.8996 | −0.4782 | 0.4548 | 0.048* | |
C20 | 0.8143 (3) | −0.3242 (3) | 0.41698 (18) | 0.0385 (9) | |
H20A | 0.8228 | −0.3358 | 0.3751 | 0.046* | |
C21 | 0.7555 (3) | −0.2220 (3) | 0.42906 (16) | 0.0319 (8) | |
H21A | 0.7245 | −0.1639 | 0.3966 | 0.038* | |
C22 | 0.7453 (3) | −0.2110 (3) | 0.49273 (15) | 0.0243 (7) | |
C23 | 0.7105 (3) | −0.1507 (3) | 0.58409 (15) | 0.0243 (7) | |
C24 | 0.6695 (3) | −0.0771 (3) | 0.63187 (16) | 0.0295 (8) | |
H24A | 0.6006 | −0.0827 | 0.6499 | 0.035* | |
H24B | 0.7238 | −0.0995 | 0.6661 | 0.035* | |
C25 | 0.4528 (3) | 0.3365 (3) | 0.00832 (17) | 0.0303 (8) | |
C26 | 0.4226 (3) | 0.3917 (3) | −0.05355 (19) | 0.0401 (9) | |
H26A | 0.4390 | 0.3572 | −0.0888 | 0.048* | |
C27 | 0.3668 (3) | 0.5011 (4) | −0.0584 (2) | 0.0524 (12) | |
H27A | 0.3446 | 0.5419 | −0.0985 | 0.063* | |
C28 | 0.3424 (3) | 0.5532 (3) | −0.0062 (3) | 0.0519 (12) | |
H28A | 0.3051 | 0.6275 | −0.0126 | 0.062* | |
C29 | 0.3714 (3) | 0.4989 (3) | 0.0546 (2) | 0.0445 (10) | |
H29A | 0.3549 | 0.5339 | 0.0897 | 0.053* | |
C30 | 0.4269 (3) | 0.3885 (3) | 0.06057 (18) | 0.0321 (8) | |
C31 | 0.5175 (3) | 0.2141 (3) | 0.09436 (16) | 0.0280 (7) | |
C32 | 0.5659 (3) | 0.1091 (3) | 0.13786 (16) | 0.0316 (8) | |
H32A | 0.5949 | 0.1206 | 0.1758 | 0.038* | |
H32B | 0.5079 | 0.0797 | 0.1507 | 0.038* | |
C33 | 0.9669 (3) | −0.1367 (3) | 0.01930 (15) | 0.0231 (7) | |
C34 | 1.0464 (3) | −0.2331 (3) | 0.00810 (17) | 0.0308 (8) | |
H34A | 1.0837 | −0.2873 | 0.0411 | 0.037* | |
C35 | 1.0669 (3) | −0.2437 (3) | −0.05451 (19) | 0.0378 (9) | |
H35A | 1.1186 | −0.3077 | −0.0641 | 0.045* | |
C36 | 1.0132 (3) | −0.1622 (3) | −0.10411 (18) | 0.0379 (9) | |
H36A | 1.0309 | −0.1731 | −0.1457 | 0.046* | |
C37 | 0.9351 (3) | −0.0664 (3) | −0.09379 (16) | 0.0327 (8) | |
H37A | 0.8998 | −0.0115 | −0.1270 | 0.039* | |
C38 | 0.9121 (3) | −0.0564 (3) | −0.03030 (16) | 0.0240 (7) | |
C39 | 0.8397 (3) | −0.0048 (3) | 0.06091 (16) | 0.0238 (7) | |
C40 | 0.7595 (3) | 0.0538 (3) | 0.10614 (16) | 0.0283 (7) | |
H40A | 0.7922 | 0.0318 | 0.1485 | 0.034* | |
H40B | 0.7433 | 0.1307 | 0.0938 | 0.034* | |
C41 | 0.7942 (3) | −0.3016 (3) | 0.04773 (15) | 0.0242 (7) | |
C42 | 0.8533 (3) | −0.4046 (3) | 0.03544 (18) | 0.0358 (9) | |
H42A | 0.8857 | −0.4624 | 0.0677 | 0.043* | |
C43 | 0.8607 (3) | −0.4155 (3) | −0.02730 (19) | 0.0395 (9) | |
H43A | 0.8982 | −0.4835 | −0.0377 | 0.047* | |
C44 | 0.8146 (3) | −0.3294 (3) | −0.07612 (18) | 0.0361 (9) | |
H44A | 0.8234 | −0.3413 | −0.1180 | 0.043* | |
C45 | 0.7563 (3) | −0.2270 (3) | −0.06434 (16) | 0.0284 (7) | |
H45A | 0.7254 | −0.1691 | −0.0968 | 0.034* | |
C46 | 0.7467 (3) | −0.2158 (2) | −0.00092 (15) | 0.0218 (7) | |
C47 | 0.7113 (3) | −0.1549 (3) | 0.09066 (15) | 0.0248 (7) | |
C48 | 0.6705 (3) | −0.0794 (3) | 0.13700 (15) | 0.0293 (8) | |
H48A | 0.6001 | −0.0821 | 0.1543 | 0.035* | |
H48B | 0.7234 | −0.1017 | 0.1719 | 0.035* | |
N1 | 0.5026 (2) | 0.2359 (2) | 0.53440 (14) | 0.0304 (7) | |
H1A | 0.5281 | 0.1884 | 0.5100 | 0.036* | |
N2 | 0.4643 (2) | 0.3084 (2) | 0.61898 (14) | 0.0338 (7) | |
H2B | 0.4607 | 0.3155 | 0.6583 | 0.041* | |
N3 | 0.9150 (2) | −0.0916 (2) | 0.56992 (13) | 0.0268 (6) | |
H3B | 0.9359 | −0.1254 | 0.6078 | 0.032* | |
N4 | 0.8273 (2) | 0.0318 (2) | 0.49290 (13) | 0.0267 (6) | |
H4B | 0.7816 | 0.0911 | 0.4727 | 0.032* | |
N5 | 0.7699 (2) | −0.2547 (2) | 0.59717 (13) | 0.0267 (6) | |
H5B | 0.7905 | −0.2908 | 0.6346 | 0.032* | |
N6 | 0.6935 (2) | −0.1217 (2) | 0.52177 (12) | 0.0232 (6) | |
H6A | 0.6563 | −0.0579 | 0.5025 | 0.028* | |
N7 | 0.6504 (2) | 0.0355 (2) | 0.60341 (13) | 0.0248 (6) | |
N8 | 0.5094 (2) | 0.2290 (2) | 0.03123 (13) | 0.0288 (6) | |
H8C | 0.5355 | 0.1792 | 0.0083 | 0.035* | |
N9 | 0.4691 (2) | 0.3092 (2) | 0.11295 (14) | 0.0324 (7) | |
H9A | 0.4648 | 0.3198 | 0.1517 | 0.039* | |
N10 | 0.9204 (2) | −0.1004 (2) | 0.07506 (13) | 0.0245 (6) | |
H10B | 0.9407 | −0.1346 | 0.1129 | 0.029* | |
N11 | 0.8347 (2) | 0.0244 (2) | −0.00246 (13) | 0.0250 (6) | |
H11B | 0.7902 | 0.0843 | −0.0228 | 0.030* | |
N12 | 0.7697 (2) | −0.2593 (2) | 0.10416 (13) | 0.0278 (6) | |
H12B | 0.7894 | −0.2955 | 0.1417 | 0.033* | |
N13 | 0.6955 (2) | −0.1262 (2) | 0.02822 (12) | 0.0235 (6) | |
H13B | 0.6592 | −0.0622 | 0.0088 | 0.028* | |
N14 | 0.6556 (2) | 0.0314 (2) | 0.10697 (12) | 0.0237 (6) | |
O5 | 0.9397 (3) | 0.9824 (2) | 0.23642 (14) | 0.0548 (8) | |
H5C | 0.8751 | 0.9886 | 0.2505 | 0.066* | |
H5D | 0.9608 | 1.0271 | 0.2507 | 0.066* |
U11 | U22 | U33 | U12 | U13 | U23 | |
Cd1 | 0.02552 (13) | 0.02860 (14) | 0.02501 (13) | −0.00950 (10) | −0.00175 (10) | −0.00545 (10) |
Cd2 | 0.02845 (14) | 0.02631 (13) | 0.02904 (14) | −0.01285 (11) | −0.00095 (10) | −0.00138 (10) |
Cd3 | 0.03672 (15) | 0.03111 (14) | 0.02671 (14) | −0.01949 (12) | −0.00244 (11) | 0.00189 (10) |
Cd4 | 0.03477 (15) | 0.02896 (14) | 0.03084 (14) | −0.01747 (11) | 0.00041 (11) | −0.00492 (10) |
Cd5 | 0.02703 (14) | 0.02876 (14) | 0.02387 (13) | −0.01015 (11) | −0.00147 (10) | −0.00439 (10) |
Cl1 | 0.0282 (5) | 0.0428 (5) | 0.0455 (6) | −0.0046 (4) | −0.0033 (4) | 0.0005 (4) |
Cl2 | 0.0336 (5) | 0.0395 (5) | 0.0203 (4) | −0.0114 (4) | 0.0032 (3) | −0.0030 (3) |
Cl3 | 0.0657 (7) | 0.0297 (5) | 0.0275 (5) | −0.0121 (4) | −0.0023 (4) | −0.0076 (4) |
Cl4 | 0.0442 (5) | 0.0358 (5) | 0.0265 (5) | −0.0238 (4) | −0.0033 (4) | −0.0023 (4) |
Cl5 | 0.0476 (6) | 0.0633 (7) | 0.0270 (5) | −0.0363 (5) | −0.0015 (4) | −0.0025 (4) |
Cl6 | 0.0391 (5) | 0.0332 (5) | 0.0286 (5) | −0.0030 (4) | −0.0050 (4) | −0.0060 (4) |
Cl7 | 0.0466 (5) | 0.0372 (5) | 0.0214 (4) | −0.0242 (4) | −0.0005 (4) | −0.0018 (3) |
Cl8 | 0.0595 (6) | 0.0452 (5) | 0.0220 (4) | −0.0334 (5) | −0.0012 (4) | −0.0012 (4) |
Cl9 | 0.0398 (5) | 0.0355 (5) | 0.0253 (4) | −0.0102 (4) | −0.0015 (4) | −0.0025 (4) |
Cl10 | 0.0732 (8) | 0.0736 (7) | 0.0257 (5) | −0.0538 (6) | −0.0112 (5) | 0.0066 (5) |
Cl11 | 0.0654 (7) | 0.0435 (5) | 0.0288 (5) | −0.0369 (5) | 0.0140 (4) | −0.0149 (4) |
Cl12 | 0.0739 (8) | 0.0869 (9) | 0.0505 (7) | −0.0621 (7) | 0.0334 (6) | −0.0442 (6) |
Cl13 | 0.0539 (6) | 0.0363 (5) | 0.0282 (5) | −0.0276 (4) | −0.0094 (4) | 0.0022 (4) |
Cl14 | 0.0374 (6) | 0.0495 (6) | 0.0425 (6) | 0.0045 (5) | −0.0084 (4) | −0.0012 (5) |
Cl15 | 0.0345 (5) | 0.0354 (5) | 0.0183 (4) | −0.0114 (4) | 0.0023 (3) | −0.0023 (3) |
Cl16 | 0.0832 (8) | 0.0350 (5) | 0.0277 (5) | −0.0192 (5) | 0.0031 (5) | −0.0085 (4) |
O1 | 0.0503 (19) | 0.0406 (17) | 0.091 (3) | −0.0129 (15) | −0.0065 (18) | 0.0071 (16) |
O2 | 0.0404 (15) | 0.0302 (13) | 0.0348 (15) | −0.0165 (11) | 0.0005 (12) | −0.0065 (11) |
O3 | 0.0393 (16) | 0.0452 (16) | 0.0411 (16) | −0.0175 (13) | 0.0005 (13) | 0.0003 (12) |
O4 | 0.0441 (18) | 0.0439 (18) | 0.076 (2) | −0.0014 (14) | −0.0028 (16) | 0.0093 (16) |
C1 | 0.0268 (19) | 0.0311 (19) | 0.034 (2) | −0.0078 (15) | −0.0020 (15) | −0.0043 (15) |
C2 | 0.032 (2) | 0.045 (2) | 0.040 (2) | −0.0124 (18) | −0.0022 (17) | −0.0030 (18) |
C3 | 0.034 (2) | 0.044 (3) | 0.063 (3) | −0.0121 (19) | −0.011 (2) | 0.011 (2) |
C4 | 0.038 (2) | 0.031 (2) | 0.078 (4) | −0.0073 (18) | −0.007 (2) | −0.003 (2) |
C5 | 0.038 (2) | 0.033 (2) | 0.066 (3) | −0.0054 (18) | 0.001 (2) | −0.021 (2) |
C6 | 0.0281 (19) | 0.030 (2) | 0.042 (2) | −0.0055 (16) | −0.0032 (17) | −0.0072 (16) |
C7 | 0.0243 (18) | 0.0308 (19) | 0.030 (2) | −0.0027 (15) | −0.0007 (15) | −0.0096 (15) |
C8 | 0.0298 (19) | 0.035 (2) | 0.0238 (18) | −0.0007 (15) | 0.0024 (15) | −0.0088 (15) |
C9 | 0.0188 (16) | 0.0301 (18) | 0.0201 (17) | −0.0106 (14) | −0.0003 (13) | −0.0015 (13) |
C10 | 0.0243 (18) | 0.0323 (19) | 0.0290 (19) | −0.0037 (15) | −0.0023 (15) | −0.0001 (15) |
C11 | 0.031 (2) | 0.038 (2) | 0.035 (2) | −0.0060 (17) | 0.0047 (16) | −0.0119 (17) |
C12 | 0.040 (2) | 0.051 (2) | 0.0202 (19) | −0.0130 (19) | 0.0024 (16) | −0.0066 (16) |
C13 | 0.036 (2) | 0.045 (2) | 0.0218 (19) | −0.0118 (18) | −0.0031 (16) | 0.0027 (16) |
C14 | 0.0259 (17) | 0.0284 (18) | 0.0215 (17) | −0.0118 (14) | −0.0006 (14) | −0.0023 (13) |
C15 | 0.0232 (17) | 0.0305 (18) | 0.0265 (18) | −0.0135 (14) | −0.0031 (14) | −0.0046 (14) |
C16 | 0.0295 (19) | 0.0318 (19) | 0.0281 (19) | −0.0110 (15) | −0.0017 (15) | −0.0097 (14) |
C17 | 0.0298 (18) | 0.0277 (18) | 0.0212 (17) | −0.0129 (15) | 0.0014 (14) | −0.0059 (13) |
C18 | 0.037 (2) | 0.0291 (19) | 0.037 (2) | −0.0095 (16) | −0.0007 (17) | −0.0042 (16) |
C19 | 0.041 (2) | 0.038 (2) | 0.041 (2) | −0.0103 (18) | 0.0088 (18) | −0.0209 (18) |
C20 | 0.046 (2) | 0.052 (2) | 0.023 (2) | −0.020 (2) | 0.0073 (17) | −0.0163 (17) |
C21 | 0.037 (2) | 0.039 (2) | 0.0213 (18) | −0.0168 (17) | −0.0004 (15) | −0.0037 (15) |
C22 | 0.0275 (18) | 0.0275 (17) | 0.0212 (17) | −0.0139 (14) | 0.0005 (14) | −0.0045 (13) |
C23 | 0.0224 (17) | 0.0298 (18) | 0.0230 (17) | −0.0114 (14) | 0.0014 (13) | −0.0064 (13) |
C24 | 0.038 (2) | 0.0304 (19) | 0.0222 (18) | −0.0133 (16) | 0.0030 (15) | −0.0080 (14) |
C25 | 0.0246 (18) | 0.0323 (19) | 0.036 (2) | −0.0113 (15) | 0.0016 (15) | −0.0084 (15) |
C26 | 0.039 (2) | 0.042 (2) | 0.036 (2) | −0.0135 (18) | −0.0066 (18) | 0.0005 (17) |
C27 | 0.036 (2) | 0.048 (3) | 0.063 (3) | −0.014 (2) | −0.009 (2) | 0.016 (2) |
C28 | 0.032 (2) | 0.032 (2) | 0.085 (4) | −0.0063 (18) | 0.002 (2) | −0.006 (2) |
C29 | 0.030 (2) | 0.033 (2) | 0.070 (3) | −0.0068 (17) | 0.007 (2) | −0.018 (2) |
C30 | 0.0247 (18) | 0.033 (2) | 0.039 (2) | −0.0094 (15) | 0.0028 (16) | −0.0097 (16) |
C31 | 0.0213 (17) | 0.0345 (19) | 0.0286 (19) | −0.0078 (15) | 0.0014 (14) | −0.0118 (15) |
C32 | 0.0260 (18) | 0.036 (2) | 0.0247 (19) | −0.0014 (15) | 0.0032 (15) | −0.0067 (15) |
C33 | 0.0206 (16) | 0.0252 (17) | 0.0247 (18) | −0.0101 (13) | 0.0006 (13) | −0.0030 (13) |
C34 | 0.0261 (18) | 0.0267 (18) | 0.035 (2) | −0.0039 (15) | −0.0075 (15) | −0.0040 (15) |
C35 | 0.035 (2) | 0.034 (2) | 0.043 (2) | −0.0055 (17) | 0.0030 (18) | −0.0175 (17) |
C36 | 0.040 (2) | 0.046 (2) | 0.028 (2) | −0.0127 (18) | 0.0030 (17) | −0.0124 (17) |
C37 | 0.034 (2) | 0.042 (2) | 0.0207 (18) | −0.0135 (17) | 0.0017 (15) | −0.0034 (15) |
C38 | 0.0214 (16) | 0.0259 (17) | 0.0251 (18) | −0.0097 (14) | −0.0004 (13) | −0.0029 (13) |
C39 | 0.0217 (17) | 0.0282 (18) | 0.0249 (18) | −0.0123 (14) | 0.0012 (13) | −0.0057 (13) |
C40 | 0.0289 (19) | 0.0310 (19) | 0.0273 (19) | −0.0109 (15) | −0.0003 (15) | −0.0100 (14) |
C41 | 0.0302 (18) | 0.0246 (17) | 0.0205 (17) | −0.0129 (14) | −0.0012 (14) | −0.0034 (13) |
C42 | 0.045 (2) | 0.0231 (18) | 0.034 (2) | −0.0073 (16) | −0.0046 (17) | −0.0013 (15) |
C43 | 0.044 (2) | 0.029 (2) | 0.044 (2) | −0.0070 (17) | 0.0003 (19) | −0.0144 (17) |
C44 | 0.042 (2) | 0.041 (2) | 0.027 (2) | −0.0142 (18) | 0.0042 (17) | −0.0140 (16) |
C45 | 0.035 (2) | 0.0310 (19) | 0.0204 (17) | −0.0126 (15) | −0.0031 (14) | −0.0033 (14) |
C46 | 0.0237 (17) | 0.0226 (16) | 0.0209 (17) | −0.0112 (13) | −0.0018 (13) | −0.0012 (12) |
C47 | 0.0264 (17) | 0.0285 (18) | 0.0238 (17) | −0.0144 (14) | −0.0017 (14) | −0.0049 (13) |
C48 | 0.037 (2) | 0.0330 (19) | 0.0192 (17) | −0.0135 (16) | 0.0024 (15) | −0.0058 (14) |
N1 | 0.0308 (16) | 0.0283 (16) | 0.0281 (16) | −0.0031 (13) | 0.0002 (13) | −0.0104 (12) |
N2 | 0.0345 (17) | 0.0334 (17) | 0.0300 (17) | −0.0041 (14) | 0.0003 (13) | −0.0139 (13) |
N3 | 0.0250 (15) | 0.0333 (16) | 0.0202 (15) | −0.0088 (12) | −0.0034 (12) | −0.0018 (12) |
N4 | 0.0262 (15) | 0.0253 (15) | 0.0252 (15) | −0.0073 (12) | −0.0020 (12) | 0.0008 (11) |
N5 | 0.0339 (16) | 0.0268 (15) | 0.0176 (14) | −0.0093 (13) | −0.0023 (12) | −0.0012 (11) |
N6 | 0.0248 (14) | 0.0215 (14) | 0.0221 (14) | −0.0078 (11) | −0.0031 (11) | −0.0011 (11) |
N7 | 0.0227 (14) | 0.0255 (15) | 0.0255 (15) | −0.0058 (12) | 0.0008 (12) | −0.0087 (11) |
N8 | 0.0310 (16) | 0.0286 (16) | 0.0256 (16) | −0.0065 (13) | 0.0008 (12) | −0.0100 (12) |
N9 | 0.0319 (17) | 0.0352 (17) | 0.0289 (17) | −0.0066 (13) | 0.0031 (13) | −0.0145 (13) |
N10 | 0.0253 (15) | 0.0285 (15) | 0.0201 (14) | −0.0105 (12) | −0.0018 (11) | −0.0027 (11) |
N11 | 0.0245 (15) | 0.0245 (14) | 0.0220 (15) | −0.0054 (12) | −0.0002 (11) | −0.0010 (11) |
N12 | 0.0389 (17) | 0.0271 (15) | 0.0177 (14) | −0.0135 (13) | −0.0054 (12) | 0.0010 (11) |
N13 | 0.0268 (15) | 0.0206 (14) | 0.0229 (15) | −0.0085 (11) | −0.0024 (12) | −0.0020 (11) |
N14 | 0.0225 (14) | 0.0279 (15) | 0.0206 (14) | −0.0083 (12) | 0.0018 (11) | −0.0062 (11) |
O5 | 0.069 (2) | 0.0440 (17) | 0.0528 (19) | −0.0148 (15) | −0.0005 (16) | −0.0217 (14) |
Cd1—Cl3 | 2.4533 (12) | C20—C21 | 1.376 (5) |
Cd1—Cl1 | 2.4962 (14) | C20—H20A | 0.9300 |
Cd1—Cl4 | 2.5368 (11) | C21—C22 | 1.389 (4) |
Cd1—Cl2 | 2.6847 (11) | C21—H21A | 0.9300 |
Cd1—Cl5 | 2.6856 (12) | C22—N6 | 1.386 (4) |
Cd2—O4 | 2.382 (3) | C23—N5 | 1.319 (4) |
Cd2—Cl6 | 2.5622 (14) | C23—N6 | 1.326 (4) |
Cd2—Cl8 | 2.5738 (12) | C23—C24 | 1.493 (4) |
Cd2—Cl5 | 2.5814 (11) | C24—N7 | 1.469 (4) |
Cd2—Cl7 | 2.6424 (11) | C24—H24A | 0.9700 |
Cd2—Cl4 | 2.6927 (12) | C24—H24B | 0.9700 |
Cd3—O3 | 2.530 (3) | C25—N8 | 1.378 (4) |
Cd3—Cl9 | 2.5789 (14) | C25—C30 | 1.386 (5) |
Cd3—Cl8 | 2.5863 (11) | C25—C26 | 1.397 (5) |
Cd3—Cl7 | 2.5902 (12) | C26—C27 | 1.377 (6) |
Cd3—Cl10 | 2.5904 (12) | C26—H26A | 0.9300 |
Cd3—Cl11 | 2.5978 (12) | C27—C28 | 1.383 (6) |
Cd4—O1 | 2.366 (3) | C27—H27A | 0.9300 |
Cd4—O2 | 2.453 (3) | C28—C29 | 1.373 (6) |
Cd4—Cl12 | 2.5273 (12) | C28—H28A | 0.9300 |
Cd4—Cl11 | 2.5417 (11) | C29—C30 | 1.385 (5) |
Cd4—Cl10 | 2.5628 (13) | C29—H29A | 0.9300 |
Cd4—Cl13 | 2.6713 (12) | C30—N9 | 1.384 (5) |
Cd5—Cl16 | 2.4393 (12) | C31—N8 | 1.332 (4) |
Cd5—Cl14 | 2.4883 (15) | C31—N9 | 1.330 (4) |
Cd5—Cl13 | 2.5843 (11) | C31—C32 | 1.489 (5) |
Cd5—Cl15 | 2.6347 (11) | C32—N14 | 1.469 (4) |
Cd5—Cl12 | 2.6628 (13) | C32—H32A | 0.9700 |
O1—H1B | 0.9601 | C32—H32B | 0.9700 |
O1—H1C | 0.9599 | C33—C34 | 1.386 (5) |
O2—H2D | 0.8501 | C33—C38 | 1.385 (4) |
O2—H2C | 0.8499 | C33—N10 | 1.391 (4) |
O3—H3C | 0.8500 | C34—C35 | 1.372 (5) |
O3—H3D | 0.8500 | C34—H34A | 0.9300 |
O4—H4C | 0.8500 | C35—C36 | 1.389 (5) |
O4—H4D | 0.8498 | C35—H35A | 0.9300 |
C1—N1 | 1.383 (4) | C36—C37 | 1.368 (5) |
C1—C6 | 1.384 (5) | C36—H36A | 0.9300 |
C1—C2 | 1.398 (5) | C37—C38 | 1.392 (5) |
C2—C3 | 1.379 (6) | C37—H37A | 0.9300 |
C2—H2A | 0.9300 | C38—N11 | 1.385 (4) |
C3—C4 | 1.385 (6) | C39—N10 | 1.328 (4) |
C3—H3A | 0.9300 | C39—N11 | 1.339 (4) |
C4—C5 | 1.370 (6) | C39—C40 | 1.483 (4) |
C4—H4A | 0.9300 | C40—N14 | 1.473 (4) |
C5—C6 | 1.386 (5) | C40—H40A | 0.9700 |
C5—H5A | 0.9300 | C40—H40B | 0.9700 |
C6—N2 | 1.392 (5) | C41—C42 | 1.387 (5) |
C7—N1 | 1.321 (4) | C41—C46 | 1.388 (4) |
C7—N2 | 1.333 (4) | C41—N12 | 1.397 (4) |
C7—C8 | 1.481 (5) | C42—C43 | 1.369 (5) |
C8—N7 | 1.464 (4) | C42—H42A | 0.9300 |
C8—H8A | 0.9700 | C43—C44 | 1.390 (5) |
C8—H8B | 0.9700 | C43—H43A | 0.9300 |
C9—C14 | 1.386 (4) | C44—C45 | 1.375 (5) |
C9—C10 | 1.390 (5) | C44—H44A | 0.9300 |
C9—N3 | 1.391 (4) | C45—C46 | 1.383 (4) |
C10—C11 | 1.374 (5) | C45—H45A | 0.9300 |
C10—H10A | 0.9300 | C46—N13 | 1.390 (4) |
C11—C12 | 1.391 (5) | C47—N12 | 1.322 (4) |
C11—H11A | 0.9300 | C47—N13 | 1.327 (4) |
C12—C13 | 1.376 (5) | C47—C48 | 1.487 (4) |
C12—H12A | 0.9300 | C48—N14 | 1.465 (4) |
C13—C14 | 1.387 (5) | C48—H48A | 0.9700 |
C13—H13A | 0.9300 | C48—H48B | 0.9700 |
C14—N4 | 1.384 (4) | N1—H1A | 0.8600 |
C15—N3 | 1.320 (4) | N2—H2B | 0.8600 |
C15—N4 | 1.332 (4) | N3—H3B | 0.8600 |
C15—C16 | 1.493 (5) | N4—H4B | 0.8600 |
C16—N7 | 1.475 (4) | N5—H5B | 0.8600 |
C16—H16A | 0.9700 | N6—H6A | 0.8600 |
C16—H16B | 0.9700 | N8—H8C | 0.8600 |
C17—C22 | 1.383 (5) | N9—H9A | 0.8600 |
C17—C18 | 1.387 (5) | N10—H10B | 0.8600 |
C17—N5 | 1.390 (4) | N11—H11B | 0.8600 |
C18—C19 | 1.377 (5) | N12—H12B | 0.8600 |
C18—H18A | 0.9300 | N13—H13B | 0.8600 |
C19—C20 | 1.387 (5) | O5—H5C | 0.8501 |
C19—H19A | 0.9300 | O5—H5D | 0.8500 |
Cl3—Cd1—Cl1 | 113.44 (4) | C18—C19—C20 | 122.3 (3) |
Cl3—Cd1—Cl4 | 122.08 (4) | C18—C19—H19A | 118.8 |
Cl1—Cd1—Cl4 | 124.47 (4) | C20—C19—H19A | 118.8 |
Cl3—Cd1—Cl2 | 88.75 (4) | C21—C20—C19 | 122.0 (3) |
Cl1—Cd1—Cl2 | 97.33 (4) | C21—C20—H20A | 119.0 |
Cl4—Cd1—Cl2 | 85.20 (3) | C19—C20—H20A | 119.0 |
Cl3—Cd1—Cl5 | 94.46 (4) | C20—C21—C22 | 115.8 (3) |
Cl1—Cd1—Cl5 | 90.57 (4) | C20—C21—H21A | 122.1 |
Cl4—Cd1—Cl5 | 84.63 (3) | C22—C21—H21A | 122.1 |
Cl2—Cd1—Cl5 | 169.50 (3) | C17—C22—N6 | 106.5 (3) |
O4—Cd2—Cl6 | 167.60 (9) | C17—C22—C21 | 122.2 (3) |
O4—Cd2—Cl8 | 86.65 (8) | N6—C22—C21 | 131.3 (3) |
Cl6—Cd2—Cl8 | 90.97 (5) | N5—C23—N6 | 109.3 (3) |
O4—Cd2—Cl5 | 90.67 (9) | N5—C23—C24 | 125.4 (3) |
Cl6—Cd2—Cl5 | 101.68 (4) | N6—C23—C24 | 125.3 (3) |
Cl8—Cd2—Cl5 | 95.95 (4) | N7—C24—C23 | 111.8 (3) |
O4—Cd2—Cl7 | 79.30 (9) | N7—C24—H24A | 109.3 |
Cl6—Cd2—Cl7 | 88.44 (4) | C23—C24—H24A | 109.3 |
Cl8—Cd2—Cl7 | 87.58 (3) | N7—C24—H24B | 109.3 |
Cl5—Cd2—Cl7 | 169.19 (3) | C23—C24—H24B | 109.3 |
O4—Cd2—Cl4 | 86.66 (8) | H24A—C24—H24B | 107.9 |
Cl6—Cd2—Cl4 | 95.66 (4) | N8—C25—C30 | 106.7 (3) |
Cl8—Cd2—Cl4 | 173.30 (3) | N8—C25—C26 | 131.3 (3) |
Cl5—Cd2—Cl4 | 83.63 (3) | C30—C25—C26 | 122.1 (3) |
Cl7—Cd2—Cl4 | 91.67 (3) | C27—C26—C25 | 114.9 (4) |
O3—Cd3—Cl9 | 172.63 (6) | C27—C26—H26A | 122.6 |
O3—Cd3—Cl8 | 84.31 (7) | C25—C26—H26A | 122.6 |
Cl9—Cd3—Cl8 | 93.06 (4) | C26—C27—C28 | 123.0 (4) |
O3—Cd3—Cl7 | 79.70 (7) | C26—C27—H27A | 118.5 |
Cl9—Cd3—Cl7 | 93.37 (4) | C28—C27—H27A | 118.5 |
Cl8—Cd3—Cl7 | 88.43 (3) | C29—C28—C27 | 122.2 (4) |
O3—Cd3—Cl10 | 87.86 (7) | C29—C28—H28A | 118.9 |
Cl9—Cd3—Cl10 | 95.19 (4) | C27—C28—H28A | 118.9 |
Cl8—Cd3—Cl10 | 171.18 (4) | C28—C29—C30 | 115.8 (4) |
Cl7—Cd3—Cl10 | 94.18 (4) | C28—C29—H29A | 122.1 |
O3—Cd3—Cl11 | 88.99 (7) | C30—C29—H29A | 122.1 |
Cl9—Cd3—Cl11 | 97.97 (5) | C29—C30—C25 | 122.1 (4) |
Cl8—Cd3—Cl11 | 91.39 (3) | C29—C30—N9 | 132.1 (4) |
Cl7—Cd3—Cl11 | 168.65 (3) | C25—C30—N9 | 105.8 (3) |
Cl10—Cd3—Cl11 | 84.39 (4) | N8—C31—N9 | 108.3 (3) |
O1—Cd4—O2 | 171.23 (10) | N8—C31—C32 | 126.6 (3) |
O1—Cd4—Cl12 | 91.16 (9) | N9—C31—C32 | 125.0 (3) |
O2—Cd4—Cl12 | 91.64 (7) | N14—C32—C31 | 111.3 (3) |
O1—Cd4—Cl11 | 94.02 (9) | N14—C32—H32A | 109.4 |
O2—Cd4—Cl11 | 82.87 (7) | C31—C32—H32A | 109.4 |
Cl12—Cd4—Cl11 | 174.21 (4) | N14—C32—H32B | 109.4 |
O1—Cd4—Cl10 | 93.85 (9) | C31—C32—H32B | 109.4 |
O2—Cd4—Cl10 | 94.12 (7) | H32A—C32—H32B | 108.0 |
Cl12—Cd4—Cl10 | 96.12 (4) | C34—C33—C38 | 121.4 (3) |
Cl11—Cd4—Cl10 | 86.11 (4) | C34—C33—N10 | 132.2 (3) |
O1—Cd4—Cl13 | 83.75 (9) | C38—C33—N10 | 106.3 (3) |
O2—Cd4—Cl13 | 88.23 (7) | C35—C34—C33 | 116.1 (3) |
Cl12—Cd4—Cl13 | 84.75 (4) | C35—C34—H34A | 121.9 |
Cl11—Cd4—Cl13 | 93.24 (3) | C33—C34—H34A | 121.9 |
Cl10—Cd4—Cl13 | 177.46 (4) | C34—C35—C36 | 122.3 (3) |
Cl16—Cd5—Cl14 | 114.71 (5) | C34—C35—H35A | 118.8 |
Cl16—Cd5—Cl13 | 138.39 (4) | C36—C35—H35A | 118.8 |
Cl14—Cd5—Cl13 | 106.89 (4) | C37—C36—C35 | 122.2 (4) |
Cl16—Cd5—Cl15 | 90.12 (4) | C37—C36—H36A | 118.9 |
Cl14—Cd5—Cl15 | 98.41 (5) | C35—C36—H36A | 118.9 |
Cl13—Cd5—Cl15 | 84.62 (3) | C36—C37—C38 | 115.6 (3) |
Cl16—Cd5—Cl12 | 94.43 (4) | C36—C37—H37A | 122.2 |
Cl14—Cd5—Cl12 | 90.84 (5) | C38—C37—H37A | 122.2 |
Cl13—Cd5—Cl12 | 83.83 (4) | C33—C38—N11 | 106.1 (3) |
Cl15—Cd5—Cl12 | 166.90 (3) | C33—C38—C37 | 122.3 (3) |
Cd1—Cl4—Cd2 | 96.20 (3) | N11—C38—C37 | 131.5 (3) |
Cd2—Cl5—Cd1 | 95.32 (4) | N10—C39—N11 | 108.2 (3) |
Cd3—Cl7—Cd2 | 91.11 (3) | N10—C39—C40 | 126.3 (3) |
Cd2—Cl8—Cd3 | 92.77 (3) | N11—C39—C40 | 125.1 (3) |
Cd4—Cl10—Cd3 | 92.39 (4) | N14—C40—C39 | 110.6 (3) |
Cd4—Cl11—Cd3 | 92.71 (4) | N14—C40—H40A | 109.5 |
Cd4—Cl12—Cd5 | 94.47 (4) | C39—C40—H40A | 109.5 |
Cd5—Cl13—Cd4 | 92.96 (3) | N14—C40—H40B | 109.5 |
Cd4—O1—H1B | 109.2 | C39—C40—H40B | 109.5 |
Cd4—O1—H1C | 109.2 | H40A—C40—H40B | 108.1 |
H1B—O1—H1C | 109.5 | C42—C41—C46 | 121.6 (3) |
Cd4—O2—H2D | 106.8 | C42—C41—N12 | 132.3 (3) |
Cd4—O2—H2C | 106.6 | C46—C41—N12 | 106.1 (3) |
H2D—O2—H2C | 106.6 | C43—C42—C41 | 115.7 (3) |
Cd3—O3—H3C | 110.8 | C43—C42—H42A | 122.2 |
Cd3—O3—H3D | 110.4 | C41—C42—H42A | 122.2 |
H3C—O3—H3D | 108.8 | C42—C43—C44 | 122.8 (3) |
Cd2—O4—H4C | 118.4 | C42—C43—H43A | 118.6 |
Cd2—O4—H4D | 97.0 | C44—C43—H43A | 118.6 |
H4C—O4—H4D | 118.0 | C45—C44—C43 | 121.9 (3) |
N1—C1—C6 | 106.3 (3) | C45—C44—H44A | 119.0 |
N1—C1—C2 | 131.1 (3) | C43—C44—H44A | 119.0 |
C6—C1—C2 | 122.5 (3) | C44—C45—C46 | 115.6 (3) |
C3—C2—C1 | 114.9 (4) | C44—C45—H45A | 122.2 |
C3—C2—H2A | 122.5 | C46—C45—H45A | 122.2 |
C1—C2—H2A | 122.5 | C45—C46—N13 | 131.4 (3) |
C2—C3—C4 | 122.4 (4) | C45—C46—C41 | 122.5 (3) |
C2—C3—H3A | 118.8 | N13—C46—C41 | 106.1 (3) |
C4—C3—H3A | 118.8 | N12—C47—N13 | 109.3 (3) |
C5—C4—C3 | 122.5 (4) | N12—C47—C48 | 126.4 (3) |
C5—C4—H4A | 118.7 | N13—C47—C48 | 124.3 (3) |
C3—C4—H4A | 118.7 | N14—C48—C47 | 111.3 (3) |
C4—C5—C6 | 116.1 (4) | N14—C48—H48A | 109.4 |
C4—C5—H5A | 121.9 | C47—C48—H48A | 109.4 |
C6—C5—H5A | 121.9 | N14—C48—H48B | 109.4 |
C1—C6—C5 | 121.5 (4) | C47—C48—H48B | 109.4 |
C1—C6—N2 | 106.0 (3) | H48A—C48—H48B | 108.0 |
C5—C6—N2 | 132.5 (4) | C7—N1—C1 | 109.9 (3) |
N1—C7—N2 | 108.6 (3) | C7—N1—H1A | 125.1 |
N1—C7—C8 | 126.6 (3) | C1—N1—H1A | 125.1 |
N2—C7—C8 | 124.6 (3) | C7—N2—C6 | 109.2 (3) |
N7—C8—C7 | 111.0 (3) | C7—N2—H2B | 125.4 |
N7—C8—H8A | 109.4 | C6—N2—H2B | 125.4 |
C7—C8—H8A | 109.4 | C15—N3—C9 | 109.9 (3) |
N7—C8—H8B | 109.4 | C15—N3—H3B | 125.0 |
C7—C8—H8B | 109.4 | C9—N3—H3B | 125.0 |
H8A—C8—H8B | 108.0 | C15—N4—C14 | 109.5 (3) |
C14—C9—C10 | 121.5 (3) | C15—N4—H4B | 125.2 |
C14—C9—N3 | 105.8 (3) | C14—N4—H4B | 125.2 |
C10—C9—N3 | 132.7 (3) | C23—N5—C17 | 109.3 (3) |
C11—C10—C9 | 116.0 (3) | C23—N5—H5B | 125.3 |
C11—C10—H10A | 122.0 | C17—N5—H5B | 125.3 |
C9—C10—H10A | 122.0 | C23—N6—C22 | 109.0 (3) |
C10—C11—C12 | 122.5 (3) | C23—N6—H6A | 125.5 |
C10—C11—H11A | 118.8 | C22—N6—H6A | 125.5 |
C12—C11—H11A | 118.8 | C8—N7—C24 | 110.6 (3) |
C13—C12—C11 | 121.8 (3) | C8—N7—C16 | 110.3 (3) |
C13—C12—H12A | 119.1 | C24—N7—C16 | 111.4 (3) |
C11—C12—H12A | 119.1 | C31—N8—C25 | 109.5 (3) |
C12—C13—C14 | 115.9 (3) | C31—N8—H8C | 125.2 |
C12—C13—H13A | 122.0 | C25—N8—H8C | 125.2 |
C14—C13—H13A | 122.0 | C31—N9—C30 | 109.8 (3) |
N4—C14—C13 | 131.4 (3) | C31—N9—H9A | 125.1 |
N4—C14—C9 | 106.3 (3) | C30—N9—H9A | 125.1 |
C13—C14—C9 | 122.3 (3) | C39—N10—C33 | 109.6 (3) |
N3—C15—N4 | 108.4 (3) | C39—N10—H10B | 125.2 |
N3—C15—C16 | 125.6 (3) | C33—N10—H10B | 125.2 |
N4—C15—C16 | 125.7 (3) | C39—N11—C38 | 109.7 (3) |
N7—C16—C15 | 110.2 (3) | C39—N11—H11B | 125.1 |
N7—C16—H16A | 109.6 | C38—N11—H11B | 125.1 |
C15—C16—H16A | 109.6 | C47—N12—C41 | 109.1 (3) |
N7—C16—H16B | 109.6 | C47—N12—H12B | 125.4 |
C15—C16—H16B | 109.6 | C41—N12—H12B | 125.4 |
H16A—C16—H16B | 108.1 | C47—N13—C46 | 109.3 (3) |
C22—C17—C18 | 121.8 (3) | C47—N13—H13B | 125.3 |
C22—C17—N5 | 105.9 (3) | C46—N13—H13B | 125.3 |
C18—C17—N5 | 132.3 (3) | C48—N14—C32 | 110.7 (3) |
C19—C18—C17 | 115.9 (3) | C48—N14—C40 | 112.3 (3) |
C19—C18—H18A | 122.1 | C32—N14—C40 | 111.2 (3) |
C17—C18—H18A | 122.1 | H5C—O5—H5D | 108.5 |
Cl3—Cd1—Cl4—Cd2 | 88.41 (5) | C18—C17—C22—N6 | −179.9 (3) |
Cl1—Cd1—Cl4—Cd2 | −90.49 (5) | N5—C17—C22—N6 | −0.6 (4) |
Cl2—Cd1—Cl4—Cd2 | 173.91 (3) | C18—C17—C22—C21 | −1.6 (5) |
Cl5—Cd1—Cl4—Cd2 | −3.49 (3) | N5—C17—C22—C21 | 177.7 (3) |
O4—Cd2—Cl4—Cd1 | 94.70 (9) | C20—C21—C22—C17 | 1.7 (5) |
Cl6—Cd2—Cl4—Cd1 | −97.53 (4) | C20—C21—C22—N6 | 179.6 (3) |
Cl8—Cd2—Cl4—Cd1 | 90.4 (2) | N5—C23—C24—N7 | 155.2 (3) |
Cl5—Cd2—Cl4—Cd1 | 3.64 (3) | N6—C23—C24—N7 | −24.3 (5) |
Cl7—Cd2—Cl4—Cd1 | 173.88 (3) | N8—C25—C26—C27 | −179.2 (4) |
O4—Cd2—Cl5—Cd1 | −90.00 (9) | C30—C25—C26—C27 | 0.7 (5) |
Cl6—Cd2—Cl5—Cd1 | 91.06 (5) | C25—C26—C27—C28 | 0.2 (6) |
Cl8—Cd2—Cl5—Cd1 | −176.70 (3) | C26—C27—C28—C29 | −0.6 (7) |
Cl7—Cd2—Cl5—Cd1 | −68.07 (16) | C27—C28—C29—C30 | 0.1 (6) |
Cl4—Cd2—Cl5—Cd1 | −3.43 (3) | C28—C29—C30—C25 | 0.8 (6) |
Cl3—Cd1—Cl5—Cd2 | −118.22 (5) | C28—C29—C30—N9 | 179.4 (4) |
Cl1—Cd1—Cl5—Cd2 | 128.22 (4) | N8—C25—C30—C29 | 178.6 (3) |
Cl4—Cd1—Cl5—Cd2 | 3.64 (3) | C26—C25—C30—C29 | −1.3 (6) |
Cl2—Cd1—Cl5—Cd2 | −10.72 (19) | N8—C25—C30—N9 | −0.3 (4) |
O3—Cd3—Cl7—Cd2 | −87.04 (7) | C26—C25—C30—N9 | 179.8 (3) |
Cl9—Cd3—Cl7—Cd2 | 90.44 (4) | N8—C31—C32—N14 | 31.1 (5) |
Cl8—Cd3—Cl7—Cd2 | −2.54 (3) | N9—C31—C32—N14 | −152.8 (3) |
Cl10—Cd3—Cl7—Cd2 | −174.10 (3) | C38—C33—C34—C35 | −0.1 (5) |
Cl11—Cd3—Cl7—Cd2 | −91.80 (15) | N10—C33—C34—C35 | 175.6 (3) |
O4—Cd2—Cl7—Cd3 | −84.50 (8) | C33—C34—C35—C36 | 1.3 (6) |
Cl6—Cd2—Cl7—Cd3 | 93.59 (5) | C34—C35—C36—C37 | −0.9 (6) |
Cl8—Cd2—Cl7—Cd3 | 2.55 (3) | C35—C36—C37—C38 | −0.7 (6) |
Cl5—Cd2—Cl7—Cd3 | −106.83 (15) | C34—C33—C38—N11 | 176.4 (3) |
Cl4—Cd2—Cl7—Cd3 | −170.78 (3) | N10—C33—C38—N11 | −0.3 (3) |
O4—Cd2—Cl8—Cd3 | 76.86 (9) | C34—C33—C38—C37 | −1.5 (5) |
Cl6—Cd2—Cl8—Cd3 | −90.95 (4) | N10—C33—C38—C37 | −178.2 (3) |
Cl5—Cd2—Cl8—Cd3 | 167.19 (3) | C36—C37—C38—C33 | 1.9 (5) |
Cl7—Cd2—Cl8—Cd3 | −2.56 (3) | C36—C37—C38—N11 | −175.4 (3) |
Cl4—Cd2—Cl8—Cd3 | 81.1 (2) | N10—C39—C40—N14 | −94.7 (4) |
O3—Cd3—Cl8—Cd2 | 82.41 (7) | N11—C39—C40—N14 | 77.2 (4) |
Cl9—Cd3—Cl8—Cd2 | −90.68 (5) | C46—C41—C42—C43 | −0.3 (5) |
Cl7—Cd3—Cl8—Cd2 | 2.61 (3) | N12—C41—C42—C43 | −179.6 (4) |
Cl10—Cd3—Cl8—Cd2 | 109.99 (19) | C41—C42—C43—C44 | 1.3 (6) |
Cl11—Cd3—Cl8—Cd2 | 171.26 (3) | C42—C43—C44—C45 | −1.2 (6) |
O1—Cd4—Cl10—Cd3 | −109.70 (9) | C43—C44—C45—C46 | −0.1 (5) |
O2—Cd4—Cl10—Cd3 | 66.62 (7) | C44—C45—C46—N13 | 179.5 (3) |
Cl12—Cd4—Cl10—Cd3 | 158.71 (4) | C44—C45—C46—C41 | 1.1 (5) |
Cl11—Cd4—Cl10—Cd3 | −15.93 (4) | C42—C41—C46—C45 | −0.9 (5) |
Cl13—Cd4—Cl10—Cd3 | −91.1 (7) | N12—C41—C46—C45 | 178.5 (3) |
O3—Cd3—Cl10—Cd4 | 104.81 (7) | C42—C41—C46—N13 | −179.6 (3) |
Cl9—Cd3—Cl10—Cd4 | −81.92 (5) | N12—C41—C46—N13 | −0.2 (3) |
Cl8—Cd3—Cl10—Cd4 | 77.3 (2) | N12—C47—C48—N14 | 154.0 (3) |
Cl7—Cd3—Cl10—Cd4 | −175.69 (3) | N13—C47—C48—N14 | −24.9 (5) |
Cl11—Cd3—Cl10—Cd4 | 15.61 (4) | N2—C7—N1—C1 | −0.5 (4) |
O1—Cd4—Cl11—Cd3 | 109.47 (9) | C8—C7—N1—C1 | 175.9 (3) |
O2—Cd4—Cl11—Cd3 | −78.77 (7) | C6—C1—N1—C7 | 0.6 (4) |
Cl12—Cd4—Cl11—Cd3 | −97.0 (3) | C2—C1—N1—C7 | 179.7 (4) |
Cl10—Cd4—Cl11—Cd3 | 15.88 (4) | N1—C7—N2—C6 | 0.2 (4) |
Cl13—Cd4—Cl11—Cd3 | −166.57 (3) | C8—C7—N2—C6 | −176.3 (3) |
O3—Cd3—Cl11—Cd4 | −103.70 (7) | C1—C6—N2—C7 | 0.1 (4) |
Cl9—Cd3—Cl11—Cd4 | 78.73 (4) | C5—C6—N2—C7 | −179.7 (4) |
Cl8—Cd3—Cl11—Cd4 | 172.02 (3) | N4—C15—N3—C9 | −2.2 (4) |
Cl7—Cd3—Cl11—Cd4 | −99.02 (14) | C16—C15—N3—C9 | 171.6 (3) |
Cl10—Cd3—Cl11—Cd4 | −15.75 (4) | C14—C9—N3—C15 | 1.6 (4) |
O1—Cd4—Cl12—Cd5 | 68.72 (9) | C10—C9—N3—C15 | −175.3 (4) |
O2—Cd4—Cl12—Cd5 | −102.96 (7) | N3—C15—N4—C14 | 1.9 (4) |
Cl11—Cd4—Cl12—Cd5 | −84.8 (3) | C16—C15—N4—C14 | −171.9 (3) |
Cl10—Cd4—Cl12—Cd5 | 162.72 (4) | C13—C14—N4—C15 | 177.2 (4) |
Cl13—Cd4—Cl12—Cd5 | −14.89 (4) | C9—C14—N4—C15 | −0.9 (4) |
Cl16—Cd5—Cl12—Cd4 | 153.66 (5) | N6—C23—N5—C17 | 0.2 (4) |
Cl14—Cd5—Cl12—Cd4 | −91.47 (5) | C24—C23—N5—C17 | −179.3 (3) |
Cl13—Cd5—Cl12—Cd4 | 15.43 (4) | C22—C17—N5—C23 | 0.2 (4) |
Cl15—Cd5—Cl12—Cd4 | 43.63 (17) | C18—C17—N5—C23 | 179.5 (4) |
Cl16—Cd5—Cl13—Cd4 | −104.28 (6) | N5—C23—N6—C22 | −0.6 (4) |
Cl14—Cd5—Cl13—Cd4 | 74.45 (5) | C24—C23—N6—C22 | 179.0 (3) |
Cl15—Cd5—Cl13—Cd4 | 171.62 (3) | C17—C22—N6—C23 | 0.7 (4) |
Cl12—Cd5—Cl13—Cd4 | −14.55 (4) | C21—C22—N6—C23 | −177.3 (4) |
O1—Cd4—Cl13—Cd5 | −76.42 (9) | C7—C8—N7—C24 | −158.2 (3) |
O2—Cd4—Cl13—Cd5 | 107.13 (7) | C7—C8—N7—C16 | 78.1 (4) |
Cl12—Cd4—Cl13—Cd5 | 15.33 (4) | C23—C24—N7—C8 | 151.6 (3) |
Cl11—Cd4—Cl13—Cd5 | −170.12 (3) | C23—C24—N7—C16 | −85.3 (3) |
Cl10—Cd4—Cl13—Cd5 | −95.1 (7) | C15—C16—N7—C8 | −167.4 (3) |
N1—C1—C2—C3 | −179.2 (4) | C15—C16—N7—C24 | 69.3 (3) |
C6—C1—C2—C3 | −0.2 (5) | N9—C31—N8—C25 | −0.9 (4) |
C1—C2—C3—C4 | 0.7 (6) | C32—C31—N8—C25 | 175.7 (3) |
C2—C3—C4—C5 | −1.4 (7) | C30—C25—N8—C31 | 0.7 (4) |
C3—C4—C5—C6 | 1.3 (6) | C26—C25—N8—C31 | −179.4 (4) |
N1—C1—C6—C5 | 179.4 (3) | N8—C31—N9—C30 | 0.8 (4) |
C2—C1—C6—C5 | 0.2 (6) | C32—C31—N9—C30 | −175.9 (3) |
N1—C1—C6—N2 | −0.4 (4) | C29—C30—N9—C31 | −179.0 (4) |
C2—C1—C6—N2 | −179.6 (3) | C25—C30—N9—C31 | −0.3 (4) |
C4—C5—C6—C1 | −0.8 (6) | N11—C39—N10—C33 | −2.2 (4) |
C4—C5—C6—N2 | 179.1 (4) | C40—C39—N10—C33 | 170.8 (3) |
N1—C7—C8—N7 | 30.2 (5) | C34—C33—N10—C39 | −174.6 (4) |
N2—C7—C8—N7 | −153.9 (3) | C38—C33—N10—C39 | 1.6 (3) |
C14—C9—C10—C11 | 0.1 (5) | N10—C39—N11—C38 | 2.1 (4) |
N3—C9—C10—C11 | 176.6 (3) | C40—C39—N11—C38 | −171.1 (3) |
C9—C10—C11—C12 | 0.7 (6) | C33—C38—N11—C39 | −1.1 (4) |
C10—C11—C12—C13 | −0.4 (6) | C37—C38—N11—C39 | 176.6 (3) |
C11—C12—C13—C14 | −0.8 (6) | N13—C47—N12—C41 | 0.4 (4) |
C12—C13—C14—N4 | −176.1 (4) | C48—C47—N12—C41 | −178.6 (3) |
C12—C13—C14—C9 | 1.7 (5) | C42—C41—N12—C47 | 179.2 (4) |
C10—C9—C14—N4 | 176.9 (3) | C46—C41—N12—C47 | −0.1 (4) |
N3—C9—C14—N4 | −0.4 (3) | N12—C47—N13—C46 | −0.5 (4) |
C10—C9—C14—C13 | −1.4 (5) | C48—C47—N13—C46 | 178.5 (3) |
N3—C9—C14—C13 | −178.7 (3) | C45—C46—N13—C47 | −178.1 (3) |
N3—C15—C16—N7 | −95.7 (4) | C41—C46—N13—C47 | 0.5 (4) |
N4—C15—C16—N7 | 77.0 (4) | C47—C48—N14—C32 | 149.9 (3) |
C22—C17—C18—C19 | 0.3 (5) | C47—C48—N14—C40 | −85.2 (3) |
N5—C17—C18—C19 | −178.9 (4) | C31—C32—N14—C48 | −156.3 (3) |
C17—C18—C19—C20 | 0.9 (6) | C31—C32—N14—C40 | 78.2 (3) |
C18—C19—C20—C21 | −0.7 (6) | C39—C40—N14—C48 | 70.3 (3) |
C19—C20—C21—C22 | −0.6 (6) | C39—C40—N14—C32 | −165.1 (3) |
D—H···A | D—H | H···A | D···A | D—H···A |
O1—H1B···Cl1i | 0.96 | 2.49 | 3.240 (3) | 135 |
O1—H1C···Cl14 | 0.96 | 2.44 | 3.397 (3) | 171 |
O2—H2D···O5ii | 0.85 | 1.81 | 2.610 (4) | 156 |
O2—H2C···Cl9 | 0.85 | 2.29 | 3.130 (3) | 173 |
O3—H3C···Cl1i | 0.85 | 2.66 | 3.317 (3) | 135 |
O3—H3D···Cl6 | 0.85 | 2.67 | 3.387 (3) | 144 |
O4—H4C···Cl14ii | 0.85 | 2.53 | 3.154 (3) | 131 |
O4—H4D···Cl7 | 0.85 | 2.67 | 3.212 (3) | 123 |
O4—H4D···Cl9 | 0.85 | 2.81 | 3.400 (3) | 128 |
N1—H1A···Cl2i | 0.86 | 2.27 | 3.108 (3) | 166 |
N2—H2B···Cl14iii | 0.86 | 2.52 | 3.361 (3) | 167 |
N3—H3B···Cl6iv | 0.86 | 2.29 | 3.100 (3) | 157 |
N4—H4B···Cl4i | 0.86 | 2.52 | 3.275 (3) | 147 |
N4—H4B···Cl2i | 0.86 | 2.93 | 3.432 (3) | 119 |
N5—H5B···O3iv | 0.86 | 2.14 | 2.942 (4) | 155 |
N6—H6A···Cl2i | 0.86 | 2.34 | 3.178 (3) | 166 |
N8—H8C···Cl15v | 0.86 | 2.27 | 3.107 (3) | 166 |
N9—H9A···Cl1i | 0.86 | 2.56 | 3.382 (3) | 161 |
N10—H10B···O2vi | 0.86 | 1.96 | 2.815 (4) | 173 |
N11—H11B···Cl13v | 0.86 | 2.43 | 3.207 (3) | 151 |
N12—H12B···Cl9vi | 0.86 | 2.29 | 3.114 (3) | 159 |
N13—H13B···Cl15v | 0.86 | 2.28 | 3.102 (3) | 161 |
O5—H5C···Cl3vii | 0.85 | 2.36 | 3.205 (4) | 176 |
O5—H5D···Cl6vii | 0.85 | 2.31 | 3.161 (3) | 177 |
Symmetry codes: (i) x+1, y, z; (ii) x−1, y, z; (iii) −x+1, −y+1, −z+1; (iv) −x+1, −y, −z+1; (v) −x+1, −y+1, −z; (vi) x+1, y−1, z; (vii) x+1, y+1, z. |
Experimental details
Crystal data | |
Chemical formula | (C24H24N7)2[Cd5Cl16(H2O)4]·H2O |
Mr | 2040.33 |
Crystal system, space group | Triclinic, P1 |
Temperature (K) | 293 |
a, b, c (Å) | 12.879 (3), 13.485 (3), 21.364 (4) |
α, β, γ (°) | 79.74 (3), 86.82 (3), 68.92 (3) |
V (Å3) | 3406.6 (15) |
Z | 2 |
Radiation type | Mo Kα |
µ (mm−1) | 2.22 |
Crystal size (mm) | 0.24 × 0.22 × 0.20 |
Data collection | |
Diffractometer | Rigaku SCXmini diffractometer |
Absorption correction | Multi-scan (CrystalClear; Rigaku, 2005) |
Tmin, Tmax | 0.593, 0.642 |
No. of measured, independent and observed [I > 2σ(I)] reflections | 35082, 15625, 13233 |
Rint | 0.038 |
(sin θ/λ)max (Å−1) | 0.649 |
Refinement | |
R[F2 > 2σ(F2)], wR(F2), S | 0.040, 0.076, 1.07 |
No. of reflections | 15625 |
No. of parameters | 794 |
H-atom treatment | H-atom parameters constrained |
Δρmax, Δρmin (e Å−3) | 0.62, −0.80 |
Computer programs: CrystalClear (Rigaku, 2005), SHELXS97 (Sheldrick, 2008), SHELXL97 (Sheldrick, 2008), PLATON (Spek, 2009) and DIAMOND (Brandenburg & Putz, 2005).
Cd1—Cl3 | 2.4533 (12) | Cd3—Cl7 | 2.5902 (12) |
Cd1—Cl1 | 2.4962 (14) | Cd3—Cl10 | 2.5904 (12) |
Cd1—Cl4 | 2.5368 (11) | Cd3—Cl11 | 2.5978 (12) |
Cd1—Cl2 | 2.6847 (11) | Cd4—O1 | 2.366 (3) |
Cd1—Cl5 | 2.6856 (12) | Cd4—O2 | 2.453 (3) |
Cd2—O4 | 2.382 (3) | Cd4—Cl12 | 2.5273 (12) |
Cd2—Cl6 | 2.5622 (14) | Cd4—Cl11 | 2.5417 (11) |
Cd2—Cl8 | 2.5738 (12) | Cd4—Cl10 | 2.5628 (13) |
Cd2—Cl5 | 2.5814 (11) | Cd4—Cl13 | 2.6713 (12) |
Cd2—Cl7 | 2.6424 (11) | Cd5—Cl16 | 2.4393 (12) |
Cd2—Cl4 | 2.6927 (12) | Cd5—Cl14 | 2.4883 (15) |
Cd3—O3 | 2.530 (3) | Cd5—Cl13 | 2.5843 (11) |
Cd3—Cl9 | 2.5789 (14) | Cd5—Cl15 | 2.6347 (11) |
Cd3—Cl8 | 2.5863 (11) | Cd5—Cl12 | 2.6628 (13) |
D—H···A | D—H | H···A | D···A | D—H···A |
O1—H1B···Cl1i | 0.96 | 2.49 | 3.240 (3) | 135.0 |
O1—H1C···Cl14 | 0.96 | 2.44 | 3.397 (3) | 171.4 |
O2—H2D···O5ii | 0.85 | 1.81 | 2.610 (4) | 155.5 |
O2—H2C···Cl9 | 0.85 | 2.29 | 3.130 (3) | 172.8 |
O3—H3C···Cl1i | 0.85 | 2.66 | 3.317 (3) | 134.8 |
O3—H3D···Cl6 | 0.85 | 2.67 | 3.387 (3) | 143.6 |
O4—H4C···Cl14ii | 0.85 | 2.53 | 3.154 (3) | 131.2 |
O4—H4D···Cl7 | 0.85 | 2.67 | 3.212 (3) | 123.4 |
O4—H4D···Cl9 | 0.85 | 2.81 | 3.400 (3) | 128.2 |
N1—H1A···Cl2i | 0.86 | 2.27 | 3.108 (3) | 166.0 |
N2—H2B···Cl14iii | 0.86 | 2.52 | 3.361 (3) | 167.0 |
N3—H3B···Cl6iv | 0.86 | 2.29 | 3.100 (3) | 157.0 |
N4—H4B···Cl4i | 0.86 | 2.52 | 3.275 (3) | 146.9 |
N4—H4B···Cl2i | 0.86 | 2.93 | 3.432 (3) | 119.3 |
N5—H5B···O3iv | 0.86 | 2.14 | 2.942 (4) | 155.2 |
N6—H6A···Cl2i | 0.86 | 2.34 | 3.178 (3) | 165.8 |
N8—H8C···Cl15v | 0.86 | 2.27 | 3.107 (3) | 165.7 |
N9—H9A···Cl1i | 0.86 | 2.56 | 3.382 (3) | 161.1 |
N10—H10B···O2vi | 0.86 | 1.96 | 2.815 (4) | 172.5 |
N11—H11B···Cl13v | 0.86 | 2.43 | 3.207 (3) | 150.9 |
N12—H12B···Cl9vi | 0.86 | 2.29 | 3.114 (3) | 159.4 |
N13—H13B···Cl15v | 0.86 | 2.28 | 3.102 (3) | 161.2 |
O5—H5C···Cl3vii | 0.85 | 2.36 | 3.205 (4) | 176.3 |
O5—H5D···Cl6vii | 0.85 | 2.31 | 3.161 (3) | 176.6 |
Symmetry codes: (i) x+1, y, z; (ii) x−1, y, z; (iii) −x+1, −y+1, −z+1; (iv) −x+1, −y, −z+1; (v) −x+1, −y+1, −z; (vi) x+1, y−1, z; (vii) x+1, y+1, z. |