Buy article online - an online subscription or single-article purchase is required to access this article.
We report on the synthesis of a new metal–organic framework (MOF) composed of Sn(OCH3)2–tetrakis(pyridin-4-yl)porphyrin linkers, Cu+ connecting nodes and [CuCl2]− counter-ions, namely poly[[bis(methanolato-κO)[μ5-5,10,15,20-tetrakis(pyridin-4-yl)porphyrin-κ81κN5:1′κN10:1′′κN15:1′′′κN20:2κ4N21,N22,N23,N24]copper(I)tin(II)] dichloridocuprate(I)], [CuSn(C40H24N8)(CH3O)2][CuCl2]. Its crystal structure consists of a single-framework coordination polymer of the organic ligand and the CuI ions. The latter are characterized by a tetrahedral coordination geometry [with CN (coordination number) = 4], linking to the pyridyl N-atom sites of four different ligands and imparting to the positively charged polymeric assembly a diamondoid PtS-type topology. Correspondingly, every porphyrin unit is coordinated to four different CuI connectors. The [CuCl2]− anions occupy the intra-lattice voids, along with disordered molecules of the water crystallization solvent. The asymmetric unit of this structure consists of two halves of the porphyrin scaffold, located on centres of crystallographic inversion, and the Cu+ and [CuCl2]− ions. This report provides unique structural evidence for the formation of tetrapyridylporphyrin-based three-dimensional MOFs with a diamondoid architecture that have been observed earlier only on rare occasions.
Supporting information
CCDC reference: 1412136
Data collection: Apex2, Bruker-AXS (Bruker, 2008); cell refinement: Saint, Bruker-AXS (Bruker, 2008); data reduction: Saint, Bruker-AXS (Bruker, 2008); program(s) used to solve structure: SHELXTL2014 (Sheldrick, 2015a); program(s) used to refine structure: SHELXL2014/7 (Sheldrick, 2015b); molecular graphics: Mercury, Crystal Structure Visualization Software (Macrae et al.,
2006); software used to prepare material for publication: SHELXL2014/7 (Sheldrick, 2015b).
Poly[]bis(methanolato-
κO)[µ
5-5,10,15,20-tetrakis(pyridin-4-yl)porphyrin-
κ81
κN5:1'
κN10:1''
κN15:1'''
κN20:2
κ4N21,
N22,
N23,
N24]copper(I)tin(II)]
dichloridocuprate(I)],
top
Crystal data top
[CuSn(C40H24N8)(CH3O)2][CuCl2] | F(000) = 1984 |
Mr = 995.41 | Dx = 1.585 Mg m−3 |
Monoclinic, P21/n | Mo Kα radiation, λ = 0.71073 Å |
a = 10.3340 (2) Å | Cell parameters from 6950 reflections |
b = 15.9714 (4) Å | θ = 2.1–26.4° |
c = 25.3074 (7) Å | µ = 1.78 mm−1 |
β = 93.277 (1)° | T = 110 K |
V = 4170.12 (18) Å3 | Plate, red |
Z = 4 | 0.15 × 0.15 × 0.10 mm |
Data collection top
ApexDuo, Bruker-AXS diffractometer | 8510 independent reflections |
Radiation source: ImuS micro-focus | 6906 reflections with I > 2σ(I) |
Detector resolution: 1.75 pixels mm-1 | Rint = 0.034 |
1 deg. φ and ω scans | θmax = 26.4°, θmin = 2.1° |
Absorption correction: multi-scan Sadabs, Bruker-AXS (Bruker, 2001) | h = −12→12 |
Tmin = 0.776, Tmax = 0.842 | k = −19→19 |
35433 measured reflections | l = −22→31 |
Refinement top
Refinement on F2 | Primary atom site location: structure-invariant direct methods |
Least-squares matrix: full | Secondary atom site location: difference Fourier map |
R[F2 > 2σ(F2)] = 0.050 | Hydrogen site location: inferred from neighbouring sites |
wR(F2) = 0.135 | H-atom parameters constrained |
S = 1.04 | w = 1/[σ2(Fo2) + (0.0567P)2 + 27.5733P] where P = (Fo2 + 2Fc2)/3 |
8510 reflections | (Δ/σ)max = 0.001 |
519 parameters | Δρmax = 3.04 e Å−3 |
0 restraints | Δρmin = −2.05 e Å−3 |
Special details top
Geometry. All e.s.d.'s (except the e.s.d. in the dihedral angle between two l.s. planes)
are estimated using the full covariance matrix. The cell e.s.d.'s are taken
into account individually in the estimation of e.s.d.'s in distances, angles
and torsion angles; correlations between e.s.d.'s in cell parameters are only
used when they are defined by crystal symmetry. An approximate (isotropic)
treatment of cell e.s.d.'s is used for estimating e.s.d.'s involving l.s.
planes. |
Fractional atomic coordinates and isotropic or equivalent isotropic displacement parameters (Å2) top | x | y | z | Uiso*/Ueq | |
Sn1 | 0.0000 | 0.0000 | 0.0000 | 0.01109 (11) | |
Sn2 | 1.5000 | 0.5000 | 0.0000 | 0.01409 (12) | |
Cu1 | 0.76038 (5) | 0.21429 (4) | −0.16676 (2) | 0.01493 (14) | |
O1 | −0.0967 (3) | 0.1038 (2) | −0.02501 (15) | 0.0219 (8) | |
C2 | −0.1309 (7) | 0.1677 (4) | 0.0074 (3) | 0.0423 (17) | |
H2A | −0.1933 | 0.1470 | 0.0321 | 0.063* | |
H2B | −0.1703 | 0.2131 | −0.0140 | 0.063* | |
H2C | −0.0535 | 0.1887 | 0.0274 | 0.063* | |
N3 | 0.0688 (4) | −0.0097 (2) | −0.07638 (16) | 0.0140 (8) | |
N4 | 0.1649 (4) | 0.0710 (2) | 0.02472 (16) | 0.0137 (8) | |
C5 | 0.0101 (5) | −0.0534 (3) | −0.11793 (19) | 0.0154 (10) | |
C6 | 0.0895 (5) | −0.0449 (3) | −0.1626 (2) | 0.0224 (11) | |
H6 | 0.0720 | −0.0683 | −0.1968 | 0.027* | |
C7 | 0.1937 (5) | 0.0025 (3) | −0.1472 (2) | 0.0224 (11) | |
H7 | 0.2622 | 0.0183 | −0.1686 | 0.027* | |
C8 | 0.1817 (4) | 0.0248 (3) | −0.09234 (19) | 0.0152 (10) | |
C9 | 0.2706 (4) | 0.0718 (3) | −0.06015 (19) | 0.0138 (9) | |
C10 | 0.2613 (4) | 0.0938 (3) | −0.00687 (19) | 0.0138 (9) | |
C11 | 0.3497 (5) | 0.1477 (3) | 0.0242 (2) | 0.0180 (10) | |
H11 | 0.4263 | 0.1728 | 0.0123 | 0.022* | |
C12 | 0.3042 (5) | 0.1559 (3) | 0.0724 (2) | 0.0174 (10) | |
H12 | 0.3426 | 0.1878 | 0.1009 | 0.021* | |
C13 | 0.1865 (4) | 0.1075 (3) | 0.07346 (19) | 0.0136 (9) | |
C14 | −0.1063 (5) | −0.0990 (3) | −0.11650 (19) | 0.0153 (10) | |
C15 | −0.1458 (4) | −0.1453 (3) | −0.16624 (19) | 0.0144 (9) | |
C16 | −0.2599 (5) | −0.1255 (3) | −0.19579 (19) | 0.0170 (10) | |
H16 | −0.3186 | −0.0854 | −0.1832 | 0.020* | |
C17 | −0.2858 (5) | −0.1654 (3) | −0.2437 (2) | 0.0173 (10) | |
H17 | −0.3623 | −0.1504 | −0.2640 | 0.021* | |
N18 | −0.2089 (4) | −0.2242 (3) | −0.26299 (16) | 0.0172 (9) | |
C19 | −0.1023 (5) | −0.2465 (3) | −0.2324 (2) | 0.0198 (11) | |
H19 | −0.0489 | −0.2901 | −0.2444 | 0.024* | |
C20 | −0.0681 (5) | −0.2087 (3) | −0.1846 (2) | 0.0210 (11) | |
H20 | 0.0077 | −0.2258 | −0.1645 | 0.025* | |
C21 | 0.3874 (4) | 0.1034 (3) | −0.08650 (19) | 0.0133 (9) | |
C22 | 0.5112 (5) | 0.0731 (3) | −0.0732 (2) | 0.0186 (10) | |
H22 | 0.5232 | 0.0299 | −0.0476 | 0.022* | |
C23 | 0.6168 (5) | 0.1058 (3) | −0.0974 (2) | 0.0190 (10) | |
H23 | 0.7005 | 0.0842 | −0.0877 | 0.023* | |
N24 | 0.6058 (4) | 0.1672 (2) | −0.13399 (15) | 0.0140 (8) | |
C25 | 0.4862 (5) | 0.1953 (3) | −0.1468 (2) | 0.0181 (10) | |
H25 | 0.4764 | 0.2381 | −0.1728 | 0.022* | |
C26 | 0.3765 (4) | 0.1660 (3) | −0.12460 (19) | 0.0169 (10) | |
H26 | 0.2940 | 0.1885 | −0.1352 | 0.020* | |
N27 | 0.8937 (4) | 0.2770 (2) | −0.12257 (17) | 0.0166 (8) | |
C28 | 0.9949 (5) | 0.2358 (3) | −0.1009 (2) | 0.0181 (10) | |
H28 | 0.9969 | 0.1766 | −0.1043 | 0.022* | |
C29 | 1.0978 (5) | 0.2753 (3) | −0.0737 (2) | 0.0203 (11) | |
H29 | 1.1677 | 0.2432 | −0.0584 | 0.024* | |
C30 | 1.0984 (5) | 0.3614 (3) | −0.06900 (19) | 0.0164 (10) | |
C31 | 0.9911 (6) | 0.4046 (3) | −0.0898 (3) | 0.0317 (14) | |
H31 | 0.9862 | 0.4638 | −0.0864 | 0.038* | |
C32 | 0.8908 (5) | 0.3603 (3) | −0.1155 (3) | 0.0298 (14) | |
H32 | 0.8165 | 0.3903 | −0.1288 | 0.036* | |
C33 | 1.2164 (5) | 0.4058 (3) | −0.0462 (2) | 0.0180 (10) | |
C34 | 1.2377 (5) | 0.4066 (3) | 0.0086 (2) | 0.0170 (10) | |
C35 | 1.1560 (5) | 0.3705 (3) | 0.0466 (2) | 0.0209 (11) | |
H35 | 1.0752 | 0.3435 | 0.0389 | 0.025* | |
C36 | 1.2148 (5) | 0.3820 (3) | 0.0956 (2) | 0.0200 (11) | |
H36 | 1.1833 | 0.3635 | 0.1282 | 0.024* | |
C37 | 1.3338 (5) | 0.4273 (3) | 0.0891 (2) | 0.0166 (10) | |
C38 | 1.4244 (5) | 0.4532 (3) | 0.1294 (2) | 0.0193 (10) | |
C39 | 1.5413 (5) | 0.4973 (3) | 0.1226 (2) | 0.0203 (11) | |
C40 | 1.6274 (6) | 0.5300 (4) | 0.1640 (2) | 0.0302 (13) | |
H40 | 1.6167 | 0.5254 | 0.2009 | 0.036* | |
C41 | 1.7260 (6) | 0.5683 (4) | 0.1412 (2) | 0.0311 (13) | |
H41 | 1.7977 | 0.5952 | 0.1592 | 0.037* | |
C42 | 1.2961 (5) | 0.4386 (3) | −0.0851 (2) | 0.0190 (10) | |
C43 | 1.4001 (5) | 0.4286 (3) | 0.18511 (19) | 0.0174 (10) | |
C44 | 1.2894 (5) | 0.4536 (3) | 0.2097 (2) | 0.0218 (11) | |
H44 | 1.2267 | 0.4882 | 0.1915 | 0.026* | |
C45 | 1.2721 (5) | 0.4276 (3) | 0.2608 (2) | 0.0207 (11) | |
H45 | 1.1967 | 0.4462 | 0.2771 | 0.025* | |
N46 | 1.3541 (4) | 0.3781 (3) | 0.28868 (17) | 0.0190 (9) | |
C47 | 1.4625 (5) | 0.3557 (3) | 0.2655 (2) | 0.0224 (11) | |
H47 | 1.5246 | 0.3223 | 0.2850 | 0.027* | |
C48 | 1.4877 (5) | 0.3794 (3) | 0.2142 (2) | 0.0211 (11) | |
H48 | 1.5653 | 0.3617 | 0.1992 | 0.025* | |
N49 | 1.4106 (4) | 0.4815 (3) | −0.07523 (16) | 0.0169 (9) | |
N50 | 1.3443 (4) | 0.4413 (3) | 0.03592 (16) | 0.0174 (9) | |
O51 | 1.5961 (4) | 0.3889 (2) | −0.00144 (15) | 0.0263 (8) | |
C52 | 1.5754 (8) | 0.3290 (4) | −0.0402 (3) | 0.053 (2) | |
H52A | 1.4828 | 0.3155 | −0.0440 | 0.080* | |
H52B | 1.6247 | 0.2784 | −0.0304 | 0.080* | |
H52C | 1.6040 | 0.3506 | −0.0739 | 0.080* | |
Cu2 | 1.85333 (7) | 0.62527 (6) | 0.26033 (3) | 0.0407 (2) | |
Cl1 | 1.74574 (15) | 0.73684 (12) | 0.25157 (8) | 0.0466 (4) | |
Cl2 | 1.95335 (15) | 0.51048 (11) | 0.26176 (8) | 0.0450 (4) | |
Atomic displacement parameters (Å2) top | U11 | U22 | U33 | U12 | U13 | U23 |
Sn1 | 0.0098 (2) | 0.0161 (2) | 0.0077 (2) | −0.00263 (16) | 0.00339 (16) | −0.00134 (17) |
Sn2 | 0.0147 (2) | 0.0169 (2) | 0.0103 (2) | −0.00555 (17) | −0.00201 (17) | −0.00054 (18) |
Cu1 | 0.0118 (3) | 0.0231 (3) | 0.0099 (3) | −0.0063 (2) | 0.0011 (2) | 0.0018 (2) |
O1 | 0.0223 (18) | 0.0211 (18) | 0.022 (2) | 0.0007 (14) | −0.0008 (16) | 0.0048 (15) |
C2 | 0.057 (4) | 0.037 (3) | 0.034 (4) | 0.024 (3) | 0.014 (3) | 0.007 (3) |
N3 | 0.0134 (18) | 0.020 (2) | 0.009 (2) | −0.0050 (15) | 0.0052 (15) | −0.0032 (16) |
N4 | 0.0131 (18) | 0.019 (2) | 0.009 (2) | −0.0039 (15) | 0.0041 (15) | −0.0034 (16) |
C5 | 0.017 (2) | 0.023 (2) | 0.006 (2) | −0.0013 (19) | 0.0036 (19) | −0.0049 (19) |
C6 | 0.026 (3) | 0.034 (3) | 0.008 (2) | −0.009 (2) | 0.008 (2) | −0.005 (2) |
C7 | 0.021 (2) | 0.034 (3) | 0.013 (3) | −0.006 (2) | 0.008 (2) | −0.004 (2) |
C8 | 0.014 (2) | 0.020 (2) | 0.012 (2) | −0.0005 (18) | 0.0054 (19) | 0.0002 (19) |
C9 | 0.012 (2) | 0.017 (2) | 0.012 (2) | −0.0014 (17) | 0.0051 (18) | 0.0003 (19) |
C10 | 0.014 (2) | 0.016 (2) | 0.011 (2) | −0.0020 (17) | 0.0024 (19) | 0.0014 (18) |
C11 | 0.016 (2) | 0.021 (2) | 0.017 (3) | −0.0042 (19) | 0.002 (2) | −0.001 (2) |
C12 | 0.015 (2) | 0.025 (2) | 0.013 (2) | −0.0057 (19) | 0.0032 (19) | −0.004 (2) |
C13 | 0.011 (2) | 0.017 (2) | 0.012 (2) | −0.0025 (17) | 0.0003 (18) | −0.0039 (19) |
C14 | 0.019 (2) | 0.021 (2) | 0.007 (2) | −0.0030 (19) | 0.0007 (19) | −0.0008 (19) |
C15 | 0.016 (2) | 0.018 (2) | 0.010 (2) | −0.0030 (18) | 0.0052 (19) | 0.0001 (19) |
C16 | 0.019 (2) | 0.019 (2) | 0.013 (2) | 0.0018 (19) | 0.004 (2) | 0.000 (2) |
C17 | 0.016 (2) | 0.018 (2) | 0.018 (3) | 0.0028 (18) | −0.003 (2) | 0.000 (2) |
N18 | 0.0168 (19) | 0.024 (2) | 0.011 (2) | 0.0029 (17) | −0.0010 (16) | −0.0056 (17) |
C19 | 0.013 (2) | 0.028 (3) | 0.018 (3) | 0.0042 (19) | 0.001 (2) | −0.008 (2) |
C20 | 0.018 (2) | 0.032 (3) | 0.013 (3) | 0.000 (2) | −0.001 (2) | −0.003 (2) |
C21 | 0.014 (2) | 0.017 (2) | 0.010 (2) | −0.0039 (17) | 0.0036 (18) | −0.0032 (18) |
C22 | 0.018 (2) | 0.022 (2) | 0.016 (3) | 0.0002 (19) | 0.005 (2) | 0.011 (2) |
C23 | 0.011 (2) | 0.025 (3) | 0.021 (3) | 0.0029 (19) | 0.002 (2) | 0.004 (2) |
N24 | 0.0150 (19) | 0.019 (2) | 0.009 (2) | −0.0030 (15) | 0.0036 (16) | −0.0015 (16) |
C25 | 0.021 (2) | 0.020 (2) | 0.013 (2) | −0.0007 (19) | 0.005 (2) | 0.006 (2) |
C26 | 0.013 (2) | 0.024 (2) | 0.015 (3) | 0.0037 (18) | 0.0042 (19) | 0.007 (2) |
N27 | 0.0142 (19) | 0.018 (2) | 0.017 (2) | −0.0045 (16) | −0.0008 (16) | 0.0022 (17) |
C28 | 0.022 (2) | 0.013 (2) | 0.018 (3) | −0.0047 (18) | −0.003 (2) | 0.0022 (19) |
C29 | 0.016 (2) | 0.025 (3) | 0.019 (3) | −0.001 (2) | −0.007 (2) | 0.001 (2) |
C30 | 0.020 (2) | 0.019 (2) | 0.010 (2) | −0.0040 (19) | −0.0015 (19) | 0.0057 (19) |
C31 | 0.030 (3) | 0.018 (3) | 0.046 (4) | −0.004 (2) | −0.011 (3) | 0.000 (3) |
C32 | 0.023 (3) | 0.018 (3) | 0.046 (4) | 0.003 (2) | −0.016 (3) | −0.004 (2) |
C33 | 0.018 (2) | 0.019 (2) | 0.017 (3) | −0.0051 (19) | −0.001 (2) | 0.001 (2) |
C34 | 0.016 (2) | 0.021 (2) | 0.014 (3) | −0.0036 (18) | −0.003 (2) | 0.000 (2) |
C35 | 0.017 (2) | 0.022 (2) | 0.024 (3) | −0.0037 (19) | 0.000 (2) | 0.000 (2) |
C36 | 0.022 (2) | 0.023 (2) | 0.015 (3) | −0.004 (2) | −0.001 (2) | 0.005 (2) |
C37 | 0.016 (2) | 0.020 (2) | 0.013 (2) | −0.0024 (19) | −0.0012 (19) | −0.0011 (19) |
C38 | 0.023 (2) | 0.023 (3) | 0.012 (3) | −0.005 (2) | 0.000 (2) | 0.000 (2) |
C39 | 0.023 (3) | 0.023 (2) | 0.014 (3) | −0.007 (2) | −0.003 (2) | 0.000 (2) |
C40 | 0.033 (3) | 0.044 (3) | 0.014 (3) | −0.017 (3) | −0.002 (2) | −0.001 (2) |
C41 | 0.033 (3) | 0.040 (3) | 0.019 (3) | −0.019 (3) | −0.008 (2) | −0.002 (3) |
C42 | 0.022 (2) | 0.020 (2) | 0.014 (3) | −0.010 (2) | −0.005 (2) | 0.000 (2) |
C43 | 0.022 (2) | 0.019 (2) | 0.011 (2) | −0.0071 (19) | 0.003 (2) | −0.0018 (19) |
C44 | 0.026 (3) | 0.018 (2) | 0.022 (3) | 0.004 (2) | 0.001 (2) | 0.003 (2) |
C45 | 0.022 (2) | 0.019 (2) | 0.021 (3) | 0.003 (2) | 0.005 (2) | −0.002 (2) |
N46 | 0.019 (2) | 0.023 (2) | 0.016 (2) | 0.0020 (17) | 0.0039 (17) | 0.0005 (17) |
C47 | 0.021 (2) | 0.028 (3) | 0.018 (3) | −0.001 (2) | 0.003 (2) | 0.003 (2) |
C48 | 0.017 (2) | 0.033 (3) | 0.014 (3) | −0.003 (2) | 0.007 (2) | −0.001 (2) |
N49 | 0.019 (2) | 0.020 (2) | 0.011 (2) | −0.0075 (16) | −0.0023 (17) | 0.0014 (16) |
N50 | 0.0169 (19) | 0.022 (2) | 0.012 (2) | −0.0063 (16) | −0.0024 (17) | −0.0001 (17) |
O51 | 0.029 (2) | 0.0251 (19) | 0.023 (2) | 0.0025 (16) | −0.0081 (17) | −0.0041 (16) |
C52 | 0.067 (5) | 0.037 (4) | 0.055 (5) | 0.018 (3) | −0.007 (4) | −0.014 (3) |
Cu2 | 0.0279 (4) | 0.0577 (5) | 0.0364 (5) | −0.0080 (4) | −0.0005 (3) | 0.0040 (4) |
Cl1 | 0.0303 (8) | 0.0598 (11) | 0.0488 (10) | −0.0091 (7) | −0.0062 (7) | 0.0070 (8) |
Cl2 | 0.0239 (7) | 0.0563 (10) | 0.0549 (11) | −0.0021 (7) | 0.0040 (7) | 0.0077 (8) |
Geometric parameters (Å, º) top
Sn1—O1 | 2.019 (3) | C21—C26 | 1.390 (7) |
Sn1—O1i | 2.019 (3) | C21—C22 | 1.390 (7) |
Sn1—N3 | 2.103 (4) | C22—C23 | 1.383 (7) |
Sn1—N3i | 2.103 (4) | C23—N24 | 1.350 (6) |
Sn1—N4 | 2.112 (4) | N24—C25 | 1.337 (6) |
Sn1—N4i | 2.112 (4) | C25—C26 | 1.375 (7) |
Sn2—O51 | 2.035 (4) | N27—C28 | 1.327 (6) |
Sn2—O51ii | 2.035 (4) | N27—C32 | 1.342 (7) |
Sn2—N49 | 2.089 (4) | C28—C29 | 1.385 (7) |
Sn2—N49ii | 2.089 (4) | C29—C30 | 1.379 (7) |
Sn2—N50 | 2.112 (4) | C30—C31 | 1.384 (7) |
Sn2—N50ii | 2.112 (4) | C30—C33 | 1.498 (6) |
Cu1—N24 | 1.989 (4) | C31—C32 | 1.387 (7) |
Cu1—N27 | 1.994 (4) | C33—C34 | 1.392 (7) |
Cu1—N18iii | 2.074 (4) | C33—C42 | 1.420 (7) |
Cu1—N46iv | 2.124 (4) | C34—N50 | 1.383 (6) |
O1—C2 | 1.368 (7) | C34—C35 | 1.436 (7) |
N3—C8 | 1.372 (6) | C35—C36 | 1.363 (7) |
N3—C5 | 1.374 (6) | C36—C37 | 1.445 (7) |
N4—C10 | 1.363 (6) | C37—N50 | 1.374 (6) |
N4—C13 | 1.371 (6) | C37—C38 | 1.407 (7) |
C5—C14 | 1.409 (7) | C38—C39 | 1.417 (7) |
C5—C6 | 1.441 (7) | C38—C43 | 1.498 (7) |
C6—C7 | 1.355 (7) | C39—N49ii | 1.366 (7) |
C7—C8 | 1.445 (7) | C39—C40 | 1.434 (7) |
C8—C9 | 1.409 (7) | C40—C41 | 1.347 (8) |
C9—C10 | 1.402 (7) | C41—C42ii | 1.429 (7) |
C9—C21 | 1.500 (6) | C42—N49 | 1.377 (6) |
C10—C11 | 1.453 (6) | C42—C41ii | 1.429 (7) |
C11—C12 | 1.340 (7) | C43—C48 | 1.380 (7) |
C12—C13 | 1.442 (6) | C43—C44 | 1.391 (7) |
C13—C14i | 1.413 (7) | C44—C45 | 1.380 (7) |
C14—C13i | 1.413 (7) | C45—N46 | 1.332 (6) |
C14—C15 | 1.496 (6) | N46—C47 | 1.342 (7) |
C15—C20 | 1.389 (7) | N46—Cu1vi | 2.124 (4) |
C15—C16 | 1.396 (7) | C47—C48 | 1.391 (7) |
C16—C17 | 1.382 (7) | N49—C39ii | 1.366 (7) |
C17—N18 | 1.340 (6) | O51—C52 | 1.379 (8) |
N18—C19 | 1.357 (6) | Cu2—Cl2 | 2.104 (2) |
N18—Cu1v | 2.074 (4) | Cu2—Cl1 | 2.105 (2) |
C19—C20 | 1.379 (7) | | |
| | | |
O1—Sn1—O1i | 180.0 | C17—C16—C15 | 118.7 (4) |
O1—Sn1—N3 | 87.70 (15) | N18—C17—C16 | 123.7 (4) |
O1i—Sn1—N3 | 92.30 (15) | C17—N18—C19 | 117.0 (4) |
O1—Sn1—N3i | 92.30 (15) | C17—N18—Cu1v | 121.1 (3) |
O1i—Sn1—N3i | 87.70 (15) | C19—N18—Cu1v | 121.6 (3) |
N3—Sn1—N3i | 180.0 | N18—C19—C20 | 123.0 (5) |
O1—Sn1—N4 | 91.60 (15) | C19—C20—C15 | 119.3 (5) |
O1i—Sn1—N4 | 88.40 (15) | C26—C21—C22 | 117.0 (4) |
N3—Sn1—N4 | 90.15 (15) | C26—C21—C9 | 121.0 (4) |
N3i—Sn1—N4 | 89.85 (15) | C22—C21—C9 | 121.9 (4) |
O1—Sn1—N4i | 88.40 (15) | C23—C22—C21 | 120.0 (4) |
O1i—Sn1—N4i | 91.59 (15) | N24—C23—C22 | 122.7 (4) |
N3—Sn1—N4i | 89.85 (15) | C25—N24—C23 | 116.8 (4) |
N3i—Sn1—N4i | 90.15 (15) | C25—N24—Cu1 | 121.6 (3) |
N4—Sn1—N4i | 180.0 | C23—N24—Cu1 | 121.5 (3) |
O51—Sn2—O51ii | 180.0 | N24—C25—C26 | 123.9 (4) |
O51—Sn2—N49 | 92.94 (16) | C25—C26—C21 | 119.5 (4) |
O51ii—Sn2—N49 | 87.06 (16) | C28—N27—C32 | 117.4 (4) |
O51—Sn2—N49ii | 87.06 (16) | C28—N27—Cu1 | 119.0 (3) |
O51ii—Sn2—N49ii | 92.95 (16) | C32—N27—Cu1 | 123.5 (3) |
N49—Sn2—N49ii | 180.0 | N27—C28—C29 | 122.9 (4) |
O51—Sn2—N50 | 90.30 (16) | C30—C29—C28 | 119.7 (5) |
O51ii—Sn2—N50 | 89.71 (16) | C29—C30—C31 | 117.7 (5) |
N49—Sn2—N50 | 91.22 (15) | C29—C30—C33 | 120.4 (4) |
N49ii—Sn2—N50 | 88.78 (15) | C31—C30—C33 | 121.8 (4) |
O51—Sn2—N50ii | 89.70 (16) | C30—C31—C32 | 119.0 (5) |
O51ii—Sn2—N50ii | 90.30 (16) | N27—C32—C31 | 123.1 (5) |
N49—Sn2—N50ii | 88.78 (15) | C34—C33—C42 | 128.5 (4) |
N49ii—Sn2—N50ii | 91.22 (15) | C34—C33—C30 | 117.8 (4) |
N50—Sn2—N50ii | 180.0 | C42—C33—C30 | 113.6 (4) |
N24—Cu1—N27 | 120.13 (17) | N50—C34—C33 | 125.4 (4) |
N24—Cu1—N18iii | 111.32 (16) | N50—C34—C35 | 107.9 (4) |
N27—Cu1—N18iii | 112.20 (16) | C33—C34—C35 | 126.7 (4) |
N24—Cu1—N46iv | 111.10 (16) | C36—C35—C34 | 107.9 (4) |
N27—Cu1—N46iv | 108.98 (16) | C35—C36—C37 | 107.5 (5) |
N18iii—Cu1—N46iv | 88.65 (17) | N50—C37—C38 | 125.2 (4) |
C2—O1—Sn1 | 124.4 (4) | N50—C37—C36 | 108.0 (4) |
C8—N3—C5 | 108.9 (4) | C38—C37—C36 | 126.8 (5) |
C8—N3—Sn1 | 125.4 (3) | C37—C38—C39 | 126.4 (5) |
C5—N3—Sn1 | 125.7 (3) | C37—C38—C43 | 117.7 (4) |
C10—N4—C13 | 109.1 (4) | C39—C38—C43 | 115.8 (4) |
C10—N4—Sn1 | 125.1 (3) | N49ii—C39—C38 | 125.9 (4) |
C13—N4—Sn1 | 125.6 (3) | N49ii—C39—C40 | 108.0 (4) |
N3—C5—C14 | 125.7 (4) | C38—C39—C40 | 126.1 (5) |
N3—C5—C6 | 107.9 (4) | C41—C40—C39 | 107.8 (5) |
C14—C5—C6 | 126.5 (4) | C40—C41—C42ii | 107.9 (5) |
C7—C6—C5 | 107.7 (4) | N49—C42—C33 | 125.7 (4) |
C6—C7—C8 | 107.8 (4) | N49—C42—C41ii | 107.8 (4) |
N3—C8—C9 | 125.5 (4) | C33—C42—C41ii | 126.4 (4) |
N3—C8—C7 | 107.7 (4) | C48—C43—C44 | 117.1 (5) |
C9—C8—C7 | 126.7 (4) | C48—C43—C38 | 120.8 (5) |
C10—C9—C8 | 127.7 (4) | C44—C43—C38 | 122.1 (5) |
C10—C9—C21 | 116.4 (4) | C45—C44—C43 | 119.1 (5) |
C8—C9—C21 | 115.9 (4) | N46—C45—C44 | 124.2 (5) |
N4—C10—C9 | 126.2 (4) | C45—N46—C47 | 116.6 (4) |
N4—C10—C11 | 107.4 (4) | C45—N46—Cu1vi | 113.4 (3) |
C9—C10—C11 | 126.4 (4) | C47—N46—Cu1vi | 117.7 (3) |
C12—C11—C10 | 107.9 (4) | N46—C47—C48 | 122.7 (5) |
C11—C12—C13 | 107.7 (4) | C43—C48—C47 | 120.1 (5) |
N4—C13—C14i | 125.4 (4) | C39ii—N49—C42 | 108.4 (4) |
N4—C13—C12 | 107.8 (4) | C39ii—N49—Sn2 | 126.9 (3) |
C14i—C13—C12 | 126.7 (4) | C42—N49—Sn2 | 124.5 (3) |
C5—C14—C13i | 127.5 (4) | C37—N50—C34 | 108.7 (4) |
C5—C14—C15 | 115.2 (4) | C37—N50—Sn2 | 126.7 (3) |
C13i—C14—C15 | 117.2 (4) | C34—N50—Sn2 | 124.5 (3) |
C20—C15—C16 | 118.2 (4) | C52—O51—Sn2 | 124.2 (4) |
C20—C15—C14 | 120.5 (4) | Cl2—Cu2—Cl1 | 174.45 (8) |
C16—C15—C14 | 121.3 (4) | | |
Symmetry codes: (i) −x, −y, −z; (ii) −x+3, −y+1, −z; (iii) −x+1/2, y+1/2, −z−1/2; (iv) x−1/2, −y+1/2, z−1/2; (v) −x+1/2, y−1/2, −z−1/2; (vi) x+1/2, −y+1/2, z+1/2. |
Subscribe to Acta Crystallographica Section C: Structural Chemistry
The full text of this article is available to subscribers to the journal.
If you have already registered and are using a computer listed in your registration details, please email
support@iucr.org for assistance.