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Mixed-valence copper(I/II) atoms have been introduced successfully into a Pb/I skeleton to obtain two heterometallic iodo­plumbates, namely poly[bis(tetra-n-butyl­ammonium) [bis­(μ3-di­methyl­dithio­carbamato)dodeca-μ3-iodido-hexa-μ2-iodido-tetra­copper(I)copper(II)hexa­lead(II)]], {(C16H36N)2[Cu4ICuIIPb6(C3H6NS2)2I18]}n, (I), and poly[[μ3-iodido-tri-μ2-iodido-iodido­[bis­(1,10-phenanthro­line)copper(I)]copper(I)copper(II)lead(II)] hemiiodine], {[CuICuIIPbI5(C12H8N2)2]·0.5I2}n, (II), under solution and solvothermal conditions, respectively. Compound (I) contains two-dimensional anionic layers, which are built upon the linkages of CuII(S2CNMe2)2 units and one-dimensional anionic Pb/I/CuI chains. Tetra-n-butyl­ammonium cations are located between the anionic layers and connected to them via C—H...I hydrogen-bonding inter­actions. Com­pound (II) exhibits a one-dimensional neutral structure, which is composed of [PbI5] square pyramids, [CuII4] tetra­hedra and [CuIIN4I] trigonal bipyramids. Face-to-face aromatic π–π stacking inter­actions between adjacent 1,10-phen­anthroline ligands stabilize the structure and assemble compound (II) into a three-dimensional supra­molecular structure. I2 mol­ecules lie in the voids of the structure.

Supporting information

cif

Crystallographic Information File (CIF) https://doi.org/10.1107/S2053229617015807/ov3096sup1.cif
Contains datablocks global, I, II

hkl

Structure factor file (CIF format) https://doi.org/10.1107/S2053229617015807/ov3096Isup2.hkl
Contains datablock I

hkl

Structure factor file (CIF format) https://doi.org/10.1107/S2053229617015807/ov3096IIsup3.hkl
Contains datablock II

CCDC references: 1582962; 1582961

Computing details top

For both structures, data collection: CrystalClear (Rigaku, 2007); cell refinement: CrystalClear (Rigaku, 2007); data reduction: CrystalClear (Rigaku, 2007); program(s) used to solve structure: SHELXT (Sheldrick, 2015a); program(s) used to refine structure: SHELXL2014 (Sheldrick, 2015b); molecular graphics: XP (Sheldrick, 1998); software used to prepare material for publication: SHELXL97 (Sheldrick, 2008).

Poly[tetra-n-butylammonium [bis(µ2-dimethyldithiocarbamato)dodeca-µ3-iodido-hexa-µ2-iodido-tetracopper(I)copper(II)hexalead(II)]] (I) top
Crystal data top
(C16H36N)2[Cu5Pb6(C3H6NS2)2I18]Z = 1
Mr = 4570.37F(000) = 1995
Triclinic, P1Dx = 3.215 Mg m3
a = 13.5451 (18) ÅMo Kα radiation, λ = 0.71073 Å
b = 13.8890 (19) ÅCell parameters from 4164 reflections
c = 14.4514 (12) Åθ = 3.0–27.5°
α = 94.449 (3)°µ = 17.75 mm1
β = 92.316 (3)°T = 293 K
γ = 119.009 (4)°Prism, gray
V = 2361.0 (5) Å30.2 × 0.18 × 0.06 mm
Data collection top
Rigaku Mercury
diffractometer
8225 independent reflections
Radiation source: fine-focus sealed tube5419 reflections with I > 2σ(I)
Graphite monochromatorRint = 0.042
ω scansθmax = 25.0°, θmin = 3.0°
Absorption correction: multi-scan
(CrystalClear; Rigaku, 2007)
h = 1616
Tmin = 0.292, Tmax = 1.000k = 1615
15026 measured reflectionsl = 1715
Refinement top
Refinement on F2Primary atom site location: structure-invariant direct methods
Least-squares matrix: fullSecondary atom site location: difference Fourier map
R[F2 > 2σ(F2)] = 0.054Hydrogen site location: inferred from neighbouring sites
wR(F2) = 0.128H-atom parameters constrained
S = 1.07 w = 1/[σ2(Fo2) + (0.0454P)2 + 0.023P]
where P = (Fo2 + 2Fc2)/3
8225 reflections(Δ/σ)max < 0.001
340 parametersΔρmax = 2.25 e Å3
1 restraintΔρmin = 2.97 e Å3
Special details top

Geometry. All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes.

Refinement. Refinement of F2 against ALL reflections. The weighted R-factor wR and goodness of fit S are based on F2, conventional R-factors R are based on F, with F set to zero for negative F2. The threshold expression of F2 > 2sigma(F2) is used only for calculating R-factors(gt) etc. and is not relevant to the choice of reflections for refinement. R-factors based on F2 are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger.

Fractional atomic coordinates and isotropic or equivalent isotropic displacement parameters (Å2) top
xyzUiso*/Ueq
Pb10.78395 (4)0.54800 (5)0.14198 (4)0.04921 (17)
Pb20.44999 (4)0.55866 (5)0.13182 (4)0.04591 (16)
Pb30.10823 (4)0.54407 (5)0.14509 (4)0.05083 (17)
I10.87323 (8)0.75541 (9)0.28315 (7)0.0701 (3)
I20.88582 (9)0.41767 (11)0.24340 (8)0.0737 (4)
I31.00233 (7)0.66921 (8)0.03035 (6)0.0508 (2)
I40.66799 (7)0.33047 (8)0.02209 (7)0.0533 (3)
I50.66716 (7)0.66489 (8)0.01621 (6)0.0484 (2)
I60.56146 (7)0.45017 (7)0.25881 (6)0.0448 (2)
I70.55174 (8)0.75647 (8)0.29859 (7)0.0548 (3)
I80.22709 (7)0.41926 (7)0.23799 (6)0.0438 (2)
I90.22479 (10)0.71448 (9)0.31892 (8)0.0738 (3)
Cu10.50000.50000.50000.0432 (6)
Cu20.67072 (14)0.66172 (16)0.34186 (13)0.0599 (5)
Cu30.34868 (15)0.61775 (16)0.34117 (13)0.0598 (5)
S10.6747 (3)0.6552 (3)0.5045 (2)0.0477 (8)
S20.6244 (3)0.4301 (3)0.5121 (2)0.0476 (8)
N10.2781 (12)0.0559 (11)0.2225 (11)0.080 (4)
N20.8389 (9)0.6019 (11)0.5184 (7)0.058 (3)
C10.7289 (10)0.5653 (12)0.5128 (9)0.048 (3)
C20.9218 (11)0.7195 (14)0.5339 (12)0.088 (6)
H2A0.88340.76220.53390.132*
H2B0.97200.73860.48520.132*
H2C0.96480.73520.59300.132*
C30.8793 (13)0.5204 (15)0.5157 (12)0.087 (6)
H3A0.81560.44680.50540.131*
H3B0.92120.52930.57390.131*
H3C0.92750.53200.46600.131*
C40.4025 (16)0.1434 (13)0.2611 (14)0.095 (6)
H4A0.44190.18490.21090.115*
H4B0.39990.19520.30870.115*
C50.4693 (16)0.094 (2)0.302 (2)0.145 (10)
H5A0.42750.04940.34990.174*
H5B0.47340.04380.25340.174*
C60.582 (2)0.170 (2)0.342 (2)0.168 (11)
H6A0.62550.20840.29160.201*
H6B0.57830.22440.38480.201*
C70.646 (2)0.129 (3)0.389 (2)0.222 (16)
H7A0.71820.19050.41380.333*
H7B0.65770.08000.34650.333*
H7C0.60560.09050.43920.333*
C80.2199 (13)0.0153 (13)0.2973 (12)0.078 (5)
H8A0.26090.05350.31350.093*
H8B0.14460.07120.27140.093*
C90.2082 (17)0.0426 (16)0.3871 (15)0.103 (7)
H9A0.28100.10540.41040.124*
H9B0.15520.06930.37510.124*
C100.1657 (17)0.0396 (17)0.4582 (14)0.103 (6)
H10A0.09360.10260.43350.124*
H10B0.21890.06640.46880.124*
C110.1509 (16)0.0091 (17)0.5492 (14)0.113 (7)
H11A0.12510.04580.59210.170*
H11B0.09610.03320.53960.170*
H11C0.22210.07120.57420.170*
C120.2168 (18)0.1191 (17)0.1949 (15)0.105 (7)
H12A0.21400.16190.25000.126*
H12B0.26020.17070.15160.126*
C130.096 (2)0.044 (2)0.1499 (18)0.145 (10)
H13A0.09990.01240.08880.174*
H13B0.05750.01680.18730.174*
C140.033 (3)0.095 (2)0.141 (3)0.29 (3)
H14A0.08510.17350.15760.352*
H14B0.01160.08650.07440.352*
C150.059 (3)0.073 (4)0.183 (3)0.30 (3)
H15A0.09240.11400.15920.457*
H15B0.03920.09290.24840.457*
H15C0.11170.00510.17060.457*
C160.2782 (13)0.0207 (12)0.1408 (11)0.069 (4)
H16A0.20030.07570.12040.083*
H16B0.31640.05950.16250.083*
C170.3364 (16)0.0386 (14)0.0553 (13)0.089 (6)
H17A0.30360.08300.03560.107*
H17B0.41670.08740.07220.107*
C180.3194 (16)0.0474 (16)0.0229 (14)0.098 (6)
H18A0.23910.09870.03690.118*
H18B0.35590.08890.00400.118*
C190.3686 (19)0.007 (2)0.1086 (16)0.151 (10)
H19A0.35700.04910.15800.227*
H19B0.44830.05670.09500.227*
H19C0.33180.04710.12760.227*
Atomic displacement parameters (Å2) top
U11U22U33U12U13U23
Pb10.0415 (3)0.0600 (4)0.0470 (3)0.0260 (3)0.0008 (2)0.0051 (3)
Pb20.0434 (3)0.0564 (4)0.0420 (3)0.0271 (3)0.0016 (2)0.0103 (3)
Pb30.0490 (3)0.0646 (4)0.0473 (3)0.0346 (3)0.0018 (2)0.0089 (3)
I10.0468 (6)0.0669 (7)0.0644 (7)0.0049 (5)0.0069 (5)0.0087 (6)
I20.0636 (7)0.1042 (10)0.0692 (7)0.0485 (7)0.0139 (6)0.0400 (7)
I30.0459 (5)0.0560 (6)0.0539 (6)0.0260 (5)0.0059 (4)0.0161 (5)
I40.0528 (6)0.0503 (6)0.0596 (6)0.0271 (5)0.0032 (5)0.0133 (5)
I50.0483 (5)0.0506 (6)0.0467 (5)0.0231 (5)0.0084 (4)0.0138 (5)
I60.0442 (5)0.0412 (5)0.0461 (5)0.0180 (4)0.0017 (4)0.0124 (4)
I70.0581 (6)0.0429 (6)0.0611 (6)0.0227 (5)0.0056 (5)0.0124 (5)
I80.0460 (5)0.0461 (5)0.0415 (5)0.0239 (4)0.0036 (4)0.0087 (4)
I90.0989 (8)0.0700 (8)0.0753 (7)0.0636 (7)0.0233 (6)0.0081 (6)
Cu10.0392 (12)0.0437 (14)0.0476 (14)0.0208 (11)0.0049 (10)0.0106 (11)
Cu20.0575 (11)0.0651 (13)0.0581 (12)0.0297 (10)0.0008 (9)0.0168 (10)
Cu30.0672 (12)0.0601 (12)0.0585 (12)0.0353 (11)0.0022 (9)0.0167 (10)
S10.047 (2)0.045 (2)0.047 (2)0.0194 (18)0.0015 (16)0.0104 (17)
S20.050 (2)0.052 (2)0.047 (2)0.0304 (19)0.0065 (16)0.0095 (17)
N10.099 (11)0.047 (8)0.106 (12)0.041 (9)0.029 (9)0.029 (8)
N20.054 (8)0.103 (11)0.032 (6)0.048 (8)0.007 (5)0.028 (7)
C10.035 (7)0.066 (10)0.043 (8)0.025 (7)0.005 (6)0.014 (7)
C20.027 (8)0.104 (15)0.094 (13)0.002 (9)0.003 (8)0.036 (12)
C30.085 (12)0.129 (17)0.091 (14)0.083 (13)0.016 (10)0.029 (12)
C40.101 (15)0.036 (10)0.112 (16)0.007 (11)0.024 (13)0.017 (10)
C50.053 (13)0.12 (2)0.23 (3)0.021 (14)0.020 (15)0.01 (2)
C60.17 (3)0.09 (2)0.22 (3)0.06 (2)0.04 (2)0.02 (2)
C70.23 (4)0.20 (4)0.21 (3)0.09 (3)0.12 (3)0.00 (3)
C80.073 (11)0.054 (11)0.102 (14)0.023 (9)0.011 (10)0.036 (11)
C90.126 (17)0.075 (14)0.123 (18)0.054 (13)0.043 (14)0.042 (14)
C100.119 (17)0.096 (16)0.097 (16)0.055 (14)0.003 (13)0.003 (13)
C110.104 (16)0.099 (17)0.109 (17)0.030 (14)0.028 (13)0.007 (13)
C120.144 (19)0.085 (15)0.121 (18)0.075 (15)0.051 (15)0.051 (14)
C130.15 (2)0.17 (3)0.17 (3)0.11 (2)0.02 (2)0.06 (2)
C140.20 (4)0.10 (2)0.63 (9)0.09 (3)0.11 (5)0.09 (4)
C150.29 (5)0.46 (7)0.39 (6)0.32 (5)0.21 (4)0.27 (5)
C160.068 (11)0.036 (9)0.091 (13)0.014 (8)0.006 (9)0.012 (9)
C170.117 (15)0.063 (12)0.100 (15)0.049 (12)0.034 (12)0.033 (11)
C180.102 (15)0.082 (15)0.121 (18)0.054 (13)0.004 (13)0.012 (14)
C190.15 (2)0.19 (3)0.106 (19)0.08 (2)0.038 (17)0.03 (2)
Geometric parameters (Å, º) top
Pb1—I13.0714 (12)C3—H3B0.9600
Pb1—I23.1622 (11)C3—H3C0.9600
Pb1—I33.1880 (10)C4—C51.51 (3)
Pb1—I63.2518 (10)C4—H4A0.9700
Pb1—I53.3404 (10)C4—H4B0.9700
Pb1—I43.3469 (12)C5—C61.43 (3)
Pb2—I4i3.1623 (10)C5—H5A0.9700
Pb2—I53.1924 (10)C5—H5B0.9700
Pb2—I73.2075 (12)C6—C71.42 (3)
Pb2—I63.2141 (9)C6—H6A0.9700
Pb2—I83.2224 (10)C6—H6B0.9700
Pb2—I5i3.2636 (12)C7—H7A0.9600
Pb3—I93.0883 (13)C7—H7B0.9600
Pb3—I2ii3.1272 (11)C7—H7C0.9600
Pb3—I83.2082 (10)C8—C91.53 (2)
Pb3—I3ii3.2405 (10)C8—H8A0.9700
Pb3—I4i3.3431 (11)C8—H8B0.9700
Pb3—I3i3.4163 (12)C9—C101.51 (2)
I1—Cu22.6144 (19)C9—H9A0.9700
I2—Pb3iii3.1272 (11)C9—H9B0.9700
I3—Pb3iii3.2405 (10)C10—C111.50 (2)
I3—Pb3i3.4163 (12)C10—H10A0.9700
I4—Pb2i3.1623 (10)C10—H10B0.9700
I4—Pb3i3.3431 (11)C11—H11A0.9600
I5—Pb2i3.2636 (12)C11—H11B0.9600
I6—Cu22.712 (2)C11—H11C0.9600
I7—Cu22.6121 (19)C12—C131.53 (3)
I7—Cu32.615 (2)C12—H12A0.9700
I8—Cu32.701 (2)C12—H12B0.9700
I9—Cu32.6333 (19)C13—C141.36 (3)
Cu1—S1iv2.295 (3)C13—H13A0.9700
Cu1—S12.295 (3)C13—H13B0.9700
Cu1—S2iv2.324 (3)C14—C151.317 (18)
Cu1—S22.324 (3)C14—H14A0.9700
Cu2—S12.359 (4)C14—H14B0.9700
Cu3—S2iv2.337 (4)C15—H15A0.9600
S1—C11.736 (13)C15—H15B0.9600
S2—C11.717 (14)C15—H15C0.9600
S2—Cu3iv2.337 (4)C16—C171.56 (2)
N1—C81.500 (17)C16—H16A0.9700
N1—C161.527 (19)C16—H16B0.9700
N1—C121.53 (2)C17—C181.50 (3)
N1—C41.57 (2)C17—H17A0.9700
N2—C11.316 (14)C17—H17B0.9700
N2—C21.457 (19)C18—C191.51 (2)
N2—C31.477 (17)C18—H18A0.9700
C2—H2A0.9600C18—H18B0.9700
C2—H2B0.9600C19—H19A0.9600
C2—H2C0.9600C19—H19B0.9600
C3—H3A0.9600C19—H19C0.9600
I1—Pb1—I299.77 (4)N2—C2—H2C109.5
I1—Pb1—I390.32 (3)H2A—C2—H2C109.5
I2—Pb1—I392.07 (3)H2B—C2—H2C109.5
I1—Pb1—I684.85 (3)N2—C3—H3A109.5
I2—Pb1—I692.70 (3)N2—C3—H3B109.5
I3—Pb1—I6173.72 (3)H3A—C3—H3B109.5
I1—Pb1—I586.19 (3)N2—C3—H3C109.5
I2—Pb1—I5174.01 (4)H3A—C3—H3C109.5
I3—Pb1—I587.29 (3)H3B—C3—H3C109.5
I6—Pb1—I588.39 (2)C5—C4—N1114.0 (15)
I1—Pb1—I4173.87 (3)C5—C4—H4A108.8
I2—Pb1—I486.18 (3)N1—C4—H4A108.8
I3—Pb1—I490.96 (3)C5—C4—H4B108.8
I6—Pb1—I493.43 (3)N1—C4—H4B108.8
I5—Pb1—I487.88 (3)H4A—C4—H4B107.7
I4i—Pb2—I592.11 (3)C6—C5—C4117 (2)
I4i—Pb2—I792.26 (3)C6—C5—H5A108.1
I5—Pb2—I795.25 (3)C4—C5—H5A108.1
I4i—Pb2—I6175.18 (3)C6—C5—H5B108.1
I5—Pb2—I691.68 (3)C4—C5—H5B108.1
I7—Pb2—I684.43 (3)H5A—C5—H5B107.3
I4i—Pb2—I891.98 (3)C7—C6—C5120 (3)
I5—Pb2—I8172.19 (3)C7—C6—H6A107.4
I7—Pb2—I891.23 (3)C5—C6—H6A107.4
I6—Pb2—I884.62 (2)C7—C6—H6B107.4
I4i—Pb2—I5i92.45 (3)C5—C6—H6B107.4
I5—Pb2—I5i90.66 (3)H6A—C6—H6B106.9
I7—Pb2—I5i172.30 (3)C6—C7—H7A109.5
I6—Pb2—I5i90.49 (3)C6—C7—H7B109.5
I8—Pb2—I5i82.52 (3)H7A—C7—H7B109.5
I9—Pb3—I2ii91.45 (4)C6—C7—H7C109.5
I9—Pb3—I883.43 (3)H7A—C7—H7C109.5
I2ii—Pb3—I893.52 (3)H7B—C7—H7C109.5
I9—Pb3—I3ii100.27 (3)N1—C8—C9117.1 (14)
I2ii—Pb3—I3ii91.72 (3)N1—C8—H8A108.0
I8—Pb3—I3ii173.51 (3)C9—C8—H8A108.0
I9—Pb3—I4i93.20 (3)N1—C8—H8B108.0
I2ii—Pb3—I4i174.95 (3)C9—C8—H8B108.0
I8—Pb3—I4i88.98 (2)H8A—C8—H8B107.3
I3ii—Pb3—I4i85.50 (3)C10—C9—C8108.5 (15)
I9—Pb3—I3i170.34 (3)C10—C9—H9A110.0
I2ii—Pb3—I3i88.57 (3)C8—C9—H9A110.0
I8—Pb3—I3i86.92 (3)C10—C9—H9B110.0
I3ii—Pb3—I3i89.39 (3)C8—C9—H9B110.0
I4i—Pb3—I3i87.18 (3)H9A—C9—H9B108.4
Cu2—I1—Pb186.15 (5)C11—C10—C9112.7 (18)
Pb3iii—I2—Pb189.24 (3)C11—C10—H10A109.0
Pb1—I3—Pb3iii86.81 (3)C9—C10—H10A109.0
Pb1—I3—Pb3i91.64 (3)C11—C10—H10B109.0
Pb3iii—I3—Pb3i90.61 (3)C9—C10—H10B109.0
Pb2i—I4—Pb3i88.64 (3)H10A—C10—H10B107.8
Pb2i—I4—Pb190.58 (3)C10—C11—H11A109.5
Pb3i—I4—Pb190.20 (3)C10—C11—H11B109.5
Pb2—I5—Pb2i89.34 (3)H11A—C11—H11B109.5
Pb2—I5—Pb189.34 (3)C10—C11—H11C109.5
Pb2i—I5—Pb188.96 (3)H11A—C11—H11C109.5
Cu2—I6—Pb279.95 (4)H11B—C11—H11C109.5
Cu2—I6—Pb181.07 (4)C13—C12—N1113.6 (17)
Pb2—I6—Pb190.55 (2)C13—C12—H12A108.8
Cu2—I7—Cu3103.34 (6)N1—C12—H12A108.8
Cu2—I7—Pb281.53 (5)C13—C12—H12B108.8
Cu3—I7—Pb274.89 (5)N1—C12—H12B108.8
Cu3—I8—Pb382.27 (4)H12A—C12—H12B107.7
Cu3—I8—Pb273.56 (4)C14—C13—C12115 (3)
Pb3—I8—Pb290.00 (3)C14—C13—H13A108.6
Cu3—I9—Pb385.71 (5)C12—C13—H13A108.6
S1iv—Cu1—S1180.0 (2)C14—C13—H13B108.6
S1iv—Cu1—S2iv76.84 (12)C12—C13—H13B108.6
S1—Cu1—S2iv103.16 (12)H13A—C13—H13B107.6
S1iv—Cu1—S2103.16 (12)C15—C14—C13125 (3)
S1—Cu1—S276.84 (12)C15—C14—H14A106.0
S2iv—Cu1—S2180.000 (1)C13—C14—H14A106.0
S1—Cu2—I7107.69 (11)C15—C14—H14B106.0
S1—Cu2—I1112.69 (11)C13—C14—H14B106.0
I7—Cu2—I1113.72 (7)H14A—C14—H14B106.3
S1—Cu2—I6107.76 (11)C14—C15—H15A109.5
I7—Cu2—I6108.25 (7)C14—C15—H15B109.5
I1—Cu2—I6106.49 (7)H15A—C15—H15B109.5
S2iv—Cu3—I7105.29 (11)C14—C15—H15C109.5
S2iv—Cu3—I9119.76 (11)H15A—C15—H15C109.5
I7—Cu3—I9106.42 (7)H15B—C15—H15C109.5
S2iv—Cu3—I8103.13 (11)N1—C16—C17114.8 (12)
I7—Cu3—I8119.63 (7)N1—C16—H16A108.6
I9—Cu3—I8103.55 (7)C17—C16—H16A108.6
C1—S1—Cu185.6 (4)N1—C16—H16B108.6
C1—S1—Cu299.2 (4)C17—C16—H16B108.6
Cu1—S1—Cu295.14 (14)H16A—C16—H16B107.5
C1—S2—Cu185.1 (4)C18—C17—C16108.9 (14)
C1—S2—Cu3iv104.7 (4)C18—C17—H17A109.9
Cu1—S2—Cu3iv115.84 (15)C16—C17—H17A109.9
C8—N1—C16107.0 (12)C18—C17—H17B109.9
C8—N1—C12110.0 (12)C16—C17—H17B109.9
C16—N1—C12112.2 (15)H17A—C17—H17B108.3
C8—N1—C4109.1 (14)C17—C18—C19110.4 (17)
C16—N1—C4110.6 (12)C17—C18—H18A109.6
C12—N1—C4107.9 (14)C19—C18—H18A109.6
C1—N2—C2122.5 (13)C17—C18—H18B109.6
C1—N2—C3118.5 (13)C19—C18—H18B109.6
C2—N2—C3118.8 (12)H18A—C18—H18B108.1
N2—C1—S2126.4 (11)C18—C19—H19A109.5
N2—C1—S1121.1 (11)C18—C19—H19B109.5
S2—C1—S1112.4 (6)H19A—C19—H19B109.5
N2—C2—H2A109.5C18—C19—H19C109.5
N2—C2—H2B109.5H19A—C19—H19C109.5
H2A—C2—H2B109.5H19B—C19—H19C109.5
Symmetry codes: (i) x+1, y+1, z; (ii) x1, y, z; (iii) x+1, y, z; (iv) x+1, y+1, z+1.
Hydrogen-bond geometry (Å, º) top
D—H···AD—HH···AD···AD—H···A
C8—H8A···I9v0.973.023.82 (2)140
Symmetry code: (v) x, y1, z.
Poly[[µ3-iodido-tri-µ2-iodido-iodido[bis(1,10-phenanthroline)copper(I)]copper(I)copper(II)lead(II)] hemiiodine] (II) top
Crystal data top
[Cu2PbI5(C12H8N2)2]·0.5I2F(000) = 2584
Mr = 1456.08Dx = 2.982 Mg m3
Monoclinic, C2/mMo Kα radiation, λ = 0.71073 Å
a = 17.5853 (9) ÅCell parameters from 3122 reflections
b = 18.1041 (8) Åθ = 3.3–28.2°
c = 13.0705 (6) ŵ = 12.21 mm1
β = 128.789 (5)°T = 293 K
V = 3243.5 (3) Å3Prism, gray
Z = 40.3 × 0.1 × 0.1 mm
Data collection top
Rigaku Mercury
diffractometer
3837 independent reflections
Radiation source: fine-focus sealed tube2846 reflections with I > 2σ(I)
Graphite monochromatorRint = 0.026
ω scansθmax = 29.3°, θmin = 3.0°
Absorption correction: multi-scan
(CrystalClear; Rigaku, 2007)
h = 2319
Tmin = 0.403, Tmax = 1.000k = 2422
7250 measured reflectionsl = 1516
Refinement top
Refinement on F2Primary atom site location: structure-invariant direct methods
Least-squares matrix: fullSecondary atom site location: difference Fourier map
R[F2 > 2σ(F2)] = 0.039Hydrogen site location: inferred from neighbouring sites
wR(F2) = 0.086H-atom parameters constrained
S = 1.01 w = 1/[σ2(Fo2) + (0.0331P)2 + 0.5P]
where P = (Fo2 + 2Fc2)/3
3837 reflections(Δ/σ)max = 0.001
187 parametersΔρmax = 1.77 e Å3
1 restraintΔρmin = 1.80 e Å3
Special details top

Geometry. All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes.

Refinement. Refinement of F2 against ALL reflections. The weighted R-factor wR and goodness of fit S are based on F2, conventional R-factors R are based on F, with F set to zero for negative F2. The threshold expression of F2 > 2sigma(F2) is used only for calculating R-factors(gt) etc. and is not relevant to the choice of reflections for refinement. R-factors based on F2 are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger.

Fractional atomic coordinates and isotropic or equivalent isotropic displacement parameters (Å2) top
xyzUiso*/UeqOcc. (<1)
Pb10.33381 (3)1.00000.24178 (4)0.04529 (14)
I10.50000.88817 (3)0.50000.03561 (17)
I20.44875 (5)1.00000.14749 (8)0.0531 (2)
I30.19990 (4)1.12533 (3)0.05619 (6)0.05326 (17)
I40.08048 (6)1.00000.20893 (8)0.0513 (2)
I50.01894 (7)1.00000.41125 (11)0.0718 (3)
Cu10.50000.73835 (6)0.50000.0327 (3)
Cu20.0946 (5)1.00000.0131 (6)0.0640 (14)0.572 (4)
Cu2'0.0734 (8)1.0360 (5)0.0133 (9)0.075 (2)0.2141 (19)
N10.6309 (4)0.6825 (3)0.6218 (6)0.0343 (14)
N20.5332 (4)0.7359 (3)0.3799 (6)0.0296 (13)
C10.6774 (6)0.6545 (4)0.7410 (8)0.047 (2)
H1A0.65150.66260.78400.056*
C20.7613 (6)0.6145 (5)0.8040 (10)0.062 (3)
H2A0.78990.59490.88660.074*
C30.8035 (6)0.6031 (4)0.7460 (9)0.053 (2)
H3A0.86220.57760.78990.063*
C40.7564 (5)0.6305 (4)0.6189 (9)0.0430 (19)
C50.6692 (5)0.6706 (3)0.5606 (7)0.0329 (16)
C60.7914 (6)0.6217 (4)0.5450 (10)0.052 (2)
H6A0.84900.59580.58230.063*
C70.7432 (6)0.6500 (4)0.4241 (9)0.047 (2)
H7A0.76890.64440.38030.056*
C80.6524 (6)0.6889 (4)0.3608 (8)0.0412 (18)
C90.6181 (5)0.6990 (3)0.4320 (7)0.0318 (16)
C100.5990 (6)0.7187 (4)0.2374 (9)0.052 (2)
H10A0.62000.71280.18780.062*
C110.5156 (6)0.7569 (4)0.1869 (8)0.0460 (19)
H11A0.47950.77720.10320.055*
C120.4849 (5)0.7651 (4)0.2619 (8)0.0390 (17)
H12A0.42860.79210.22780.047*
Atomic displacement parameters (Å2) top
U11U22U33U12U13U23
Pb10.0464 (3)0.0454 (3)0.0369 (3)0.0000.0225 (2)0.000
I10.0414 (4)0.0288 (3)0.0372 (4)0.0000.0249 (3)0.000
I20.0334 (4)0.0648 (5)0.0521 (5)0.0000.0225 (4)0.000
I30.0560 (3)0.0607 (4)0.0533 (4)0.0196 (3)0.0392 (3)0.0185 (3)
I40.0552 (5)0.0543 (5)0.0414 (5)0.0000.0288 (4)0.000
I50.0629 (6)0.0390 (4)0.0936 (8)0.0000.0394 (6)0.000
Cu10.0307 (6)0.0391 (7)0.0363 (7)0.0000.0249 (6)0.000
Cu20.061 (3)0.056 (4)0.056 (2)0.0000.027 (2)0.000
Cu2'0.075 (6)0.086 (8)0.055 (4)0.025 (5)0.037 (4)0.008 (5)
N10.032 (3)0.040 (3)0.037 (4)0.005 (3)0.025 (3)0.005 (3)
N20.031 (3)0.032 (3)0.034 (3)0.002 (3)0.024 (3)0.003 (3)
C10.041 (5)0.050 (5)0.052 (6)0.016 (4)0.030 (4)0.017 (4)
C20.053 (5)0.070 (6)0.063 (7)0.023 (5)0.036 (5)0.028 (5)
C30.036 (4)0.047 (5)0.063 (6)0.012 (4)0.025 (5)0.013 (4)
C40.034 (4)0.035 (4)0.067 (6)0.002 (3)0.035 (4)0.003 (4)
C50.025 (4)0.029 (3)0.046 (5)0.006 (3)0.023 (4)0.003 (3)
C60.040 (5)0.045 (5)0.075 (7)0.005 (4)0.038 (5)0.015 (5)
C70.043 (5)0.048 (5)0.067 (6)0.007 (4)0.042 (5)0.017 (4)
C80.045 (5)0.043 (4)0.048 (5)0.005 (4)0.035 (4)0.012 (4)
C90.037 (4)0.025 (3)0.041 (4)0.006 (3)0.029 (4)0.008 (3)
C100.061 (6)0.055 (5)0.061 (6)0.014 (5)0.049 (5)0.018 (4)
C110.055 (5)0.048 (5)0.038 (5)0.013 (4)0.030 (4)0.006 (4)
C120.040 (4)0.039 (4)0.044 (5)0.002 (3)0.029 (4)0.000 (4)
Geometric parameters (Å, º) top
Pb1—I22.9538 (9)Cu2'—Cu2'iii2.38 (2)
Pb1—I3i3.0693 (6)Cu2'—I4iv2.565 (10)
Pb1—I33.0693 (6)Cu2'—Cu2'iv2.71 (2)
Pb1—Cu23.298 (7)Cu2'—Cu2iv2.827 (8)
Pb1—I1ii3.4165 (5)N1—C11.325 (9)
Pb1—I13.4165 (5)N1—C51.350 (8)
I1—Cu12.7124 (13)N2—C121.319 (9)
I1—Pb1ii3.4165 (5)N2—C91.366 (8)
I3—Cu2'2.513 (12)C1—C21.362 (10)
I3—Cu22.755 (4)C1—H1A0.9300
I4—Cu2'2.517 (10)C2—C31.368 (11)
I4—Cu2'i2.517 (10)C2—H2A0.9300
I4—Cu2'iii2.565 (10)C3—C41.403 (11)
I4—Cu2'iv2.565 (10)C3—H3A0.9300
I4—Cu22.590 (6)C4—C51.412 (9)
I4—Cu2iv2.722 (7)C4—C61.442 (11)
I5—I5v2.786 (2)C5—C91.415 (10)
Cu1—N21.988 (5)C6—C71.342 (11)
Cu1—N2vi1.988 (5)C6—H6A0.9300
Cu1—N1vi2.064 (6)C7—C81.441 (10)
Cu1—N12.064 (6)C7—H7A0.9300
Cu2—Cu2'0.752 (9)C8—C101.370 (11)
Cu2—Cu2'i0.752 (9)C8—C91.402 (9)
Cu2—I4iv2.722 (7)C10—C111.361 (11)
Cu2—Cu2'iii2.827 (8)C10—H10A0.9300
Cu2—Cu2'iv2.827 (8)C11—C121.393 (10)
Cu2—I3i2.755 (4)C11—H11A0.9300
Cu2'—Cu2'i1.305 (18)C12—H12A0.9300
I2—Pb1—I3i93.270 (18)I4—Cu2—Pb1164.1 (3)
I2—Pb1—I393.270 (18)I4iv—Cu2—Pb187.93 (17)
I3i—Pb1—I395.33 (3)Cu2'iii—Cu2—Pb1138.83 (16)
I2—Pb1—Cu2116.08 (13)Cu2'iv—Cu2—Pb1138.83 (16)
I3i—Pb1—Cu251.11 (4)I3—Cu2—Pb160.15 (12)
I3—Pb1—Cu251.11 (4)I3i—Cu2—Pb160.15 (12)
I2—Pb1—I1ii91.531 (17)Cu2—Cu2'—Cu2'i29.9 (13)
I3i—Pb1—I1ii167.623 (18)Cu2—Cu2'—Cu2'iii119.6 (13)
I3—Pb1—I1ii95.777 (16)Cu2'i—Cu2'—Cu2'iii90.000 (5)
Cu2—Pb1—I1ii135.34 (7)Cu2—Cu2'—I487.0 (11)
I2—Pb1—I191.531 (17)Cu2'i—Cu2'—I475.0 (2)
I3i—Pb1—I195.777 (16)Cu2'iii—Cu2'—I463.1 (4)
I3—Pb1—I1167.623 (18)Cu2—Cu2'—I3100.8 (14)
Cu2—Pb1—I1135.34 (7)Cu2'i—Cu2'—I3130.0 (2)
I1ii—Pb1—I172.680 (19)Cu2'iii—Cu2'—I3139.5 (2)
Cu1—I1—Pb1ii126.340 (10)I4—Cu2'—I3125.8 (4)
Cu1—I1—Pb1126.340 (10)Cu2—Cu2'—I4iv93.9 (12)
Pb1ii—I1—Pb1107.320 (19)Cu2'i—Cu2'—I4iv75.27 (19)
Cu2'—I3—Cu215.6 (3)Cu2'iii—Cu2'—I4iv61.1 (4)
Cu2'—I3—Pb180.5 (2)I4—Cu2'—I4iv115.5 (5)
Cu2—I3—Pb168.74 (12)I3—Cu2'—I4iv117.3 (3)
Cu2'—I4—Cu2'i30.0 (4)Cu2—Cu2'—Cu2'iv91.0 (14)
Cu2'—I4—Cu2'iii55.8 (5)Cu2'i—Cu2'—Cu2'iv61.3 (4)
Cu2'i—I4—Cu2'iii64.5 (5)Cu2'iii—Cu2'—Cu2'iv28.7 (4)
Cu2'—I4—Cu2'iv64.5 (5)I4—Cu2'—Cu2'iv58.6 (3)
Cu2'i—I4—Cu2'iv55.8 (5)I3—Cu2'—Cu2'iv167.5 (6)
Cu2'iii—I4—Cu2'iv29.5 (4)I4iv—Cu2'—Cu2'iv56.9 (4)
Cu2'—I4—Cu216.9 (2)Cu2—Cu2'—Cu2iv106.4 (14)
Cu2'i—I4—Cu216.9 (2)Cu2'i—Cu2'—Cu2iv76.66 (19)
Cu2'iii—I4—Cu266.5 (2)Cu2'iii—Cu2'—Cu2iv13.37 (18)
Cu2'iv—I4—Cu266.5 (2)I4—Cu2'—Cu2iv60.9 (3)
Cu2'—I4—Cu2iv65.2 (2)I3—Cu2'—Cu2iv152.5 (4)
Cu2'i—I4—Cu2iv65.2 (2)I4iv—Cu2'—Cu2iv57.2 (2)
Cu2'iii—I4—Cu2iv16.0 (2)Cu2'iv—Cu2'—Cu2iv15.4 (2)
Cu2'iv—I4—Cu2iv16.0 (2)C1—N1—C5117.7 (6)
Cu2—I4—Cu2iv72.0 (3)C1—N1—Cu1131.6 (5)
N2—Cu1—N2vi177.4 (3)C5—N1—Cu1110.6 (5)
N2—Cu1—N1vi96.7 (2)C12—N2—C9118.8 (6)
N2vi—Cu1—N1vi82.0 (2)C12—N2—Cu1128.4 (5)
N2—Cu1—N182.0 (2)C9—N2—Cu1112.8 (5)
N2vi—Cu1—N196.7 (2)N1—C1—C2123.5 (8)
N1vi—Cu1—N1121.4 (3)N1—C1—H1A118.2
N2—Cu1—I191.28 (15)C2—C1—H1A118.2
N2vi—Cu1—I191.28 (15)C1—C2—C3120.2 (9)
N1vi—Cu1—I1119.31 (15)C1—C2—H2A119.9
N1—Cu1—I1119.31 (16)C3—C2—H2A119.9
Cu2'—Cu2—Cu2'i120 (3)C2—C3—C4118.7 (7)
Cu2'—Cu2—I476.1 (11)C2—C3—H3A120.6
Cu2'i—Cu2—I476.1 (11)C4—C3—H3A120.6
Cu2'—Cu2—I4iv70.1 (12)C3—C4—C5117.2 (7)
Cu2'i—Cu2—I4iv70.1 (12)C3—C4—C6124.8 (7)
I4—Cu2—I4iv108.0 (3)C5—C4—C6118.0 (8)
Cu2'—Cu2—Cu2'iii47.0 (13)N1—C5—C4122.7 (7)
Cu2'i—Cu2—Cu2'iii73.6 (14)N1—C5—C9117.7 (6)
I4—Cu2—Cu2'iii56.3 (2)C4—C5—C9119.7 (7)
I4iv—Cu2—Cu2'iii53.9 (2)C7—C6—C4121.8 (7)
Cu2'—Cu2—Cu2'iv73.6 (14)C7—C6—H6A119.1
Cu2'i—Cu2—Cu2'iv47.0 (13)C4—C6—H6A119.1
I4—Cu2—Cu2'iv56.3 (2)C6—C7—C8121.2 (7)
I4iv—Cu2—Cu2'iv53.9 (2)C6—C7—H7A119.4
Cu2'iii—Cu2—Cu2'iv26.7 (4)C8—C7—H7A119.4
Cu2'—Cu2—I363.7 (12)C10—C8—C9117.9 (7)
Cu2'i—Cu2—I3170.0 (12)C10—C8—C7124.3 (7)
I4—Cu2—I3113.83 (15)C9—C8—C7117.8 (8)
I4iv—Cu2—I3104.68 (16)N2—C9—C8121.5 (7)
Cu2'iii—Cu2—I3110.62 (16)N2—C9—C5116.9 (6)
Cu2'iv—Cu2—I3137.1 (3)C8—C9—C5121.5 (6)
Cu2'—Cu2—I3i170.0 (12)C11—C10—C8120.4 (7)
Cu2'i—Cu2—I3i63.7 (12)C11—C10—H10A119.8
I4—Cu2—I3i113.83 (15)C8—C10—H10A119.8
I4iv—Cu2—I3i104.68 (16)C10—C11—C12119.3 (8)
Cu2'iii—Cu2—I3i137.1 (3)C10—C11—H11A120.4
Cu2'iv—Cu2—I3i110.62 (16)C12—C11—H11A120.4
I3—Cu2—I3i110.9 (3)N2—C12—C11122.0 (7)
Cu2'—Cu2—Pb1110.5 (12)N2—C12—H12A119.0
Cu2'i—Cu2—Pb1110.5 (12)C11—C12—H12A119.0
Symmetry codes: (i) x, y+2, z; (ii) x+1, y+2, z+1; (iii) x, y, z; (iv) x, y+2, z; (v) x, y+2, z+1; (vi) x+1, y, z+1.
 

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