The title compound, [Cu(NCS)2(C12H9N2)]n, is a one-dimensional coordination polymer containing tetrahedrally coordinated CuI atoms bound to one N atom from a protonated 4,7-phenanthroline ligand, and one N and two S atoms from three distinct thiocyanate anions. In the crystal structure, chain motifs align parallel to the a axis, formed from the linkage of neighboring CuI atoms through bridging thiocyanate ligands.
Supporting information
CCDC reference: 273353
Key indicators
- Single-crystal X-ray study
- T = 94 K
- Mean (C-C) = 0.004 Å
- R factor = 0.033
- wR factor = 0.064
- Data-to-parameter ratio = 17.3
checkCIF/PLATON results
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Alert level G
REFLT03_ALERT_4_G Please check that the estimate of the number of Friedel pairs is
correct. If it is not, please give the correct count in the
_publ_section_exptl_refinement section of the submitted CIF.
From the CIF: _diffrn_reflns_theta_max 28.27
From the CIF: _reflns_number_total 3348
Count of symmetry unique reflns 2043
Completeness (_total/calc) 163.88%
TEST3: Check Friedels for noncentro structure
Estimate of Friedel pairs measured 1305
Fraction of Friedel pairs measured 0.639
Are heavy atom types Z>Si present yes
0 ALERT level A = In general: serious problem
0 ALERT level B = Potentially serious problem
0 ALERT level C = Check and explain
1 ALERT level G = General alerts; check
0 ALERT type 1 CIF construction/syntax error, inconsistent or missing data
0 ALERT type 2 Indicator that the structure model may be wrong or deficient
0 ALERT type 3 Indicator that the structure quality may be low
1 ALERT type 4 Improvement, methodology, query or suggestion
0 ALERT type 5 Informative message, check
Data collection: SMART (Bruker, 2001); cell refinement: SAINT-Plus (Bruker, 2003); data reduction: SAINT-Plus; program(s) used to solve structure: SHELXS97 (Sheldrick, 1997); program(s) used to refine structure: SHELXL97 (Sheldrick, 1997); molecular graphics: Crystal Maker (Crystal Maker, 2005); software used to prepare material for publication: SHELXS97.
catena[[(4,7-phenanthrolin-4-ium-
κN7)(thiocyanato-
κS)copper(I)]- µ-thiocyanato-
κ2N:
S]
top
Crystal data top
[Cu(NCS)2(C12H9N2)] | F(000) = 728 |
Mr = 360.91 | Dx = 1.711 Mg m−3 |
Orthorhombic, P212121 | Mo Kα radiation, λ = 0.71073 Å |
Hall symbol: P 2ac 2ab | Cell parameters from 9353 reflections |
a = 5.6662 (3) Å | θ = 1.7–28.3° |
b = 10.1801 (6) Å | µ = 1.85 mm−1 |
c = 24.2927 (15) Å | T = 94 K |
V = 1401.26 (14) Å3 | Block, red |
Z = 4 | 0.50 × 0.40 × 0.30 mm |
Data collection top
Bruker P4 diffractometer | 3348 independent reflections |
Radiation source: fine-focus sealed tube, Bruker | 2979 reflections with I > 2σ(I) |
Graphite monochromator | Rint = 0.043 |
ω scans | θmax = 28.3°, θmin = 1.7° |
Absorption correction: multi-scan (SADABS; Sheldrick, 1996) | h = −7→7 |
Tmin = 0.450, Tmax = 0.574 | k = −13→12 |
9353 measured reflections | l = −26→32 |
Refinement top
Refinement on F2 | Secondary atom site location: difference Fourier map |
Least-squares matrix: full | Hydrogen site location: inferred from neighbouring sites |
R[F2 > 2σ(F2)] = 0.033 | H atoms treated by a mixture of independent and constrained refinement |
wR(F2) = 0.064 | w = 1/[σ2(Fo2) + (0.0236P)2 + 0.6847P] where P = (Fo2 + 2Fc2)/3 |
S = 1.06 | (Δ/σ)max = 0.001 |
3348 reflections | Δρmax = 0.52 e Å−3 |
193 parameters | Δρmin = −0.42 e Å−3 |
1 restraint | Absolute structure: Flack (1983), 1346 Friedel pairs |
Primary atom site location: structure-invariant direct methods | Absolute structure parameter: 0.031 (13) |
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. |
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. |
Fractional atomic coordinates and isotropic or equivalent isotropic displacement parameters (Å2) top | x | y | z | Uiso*/Ueq | |
Cu1 | 0.39478 (6) | 0.51765 (3) | 0.089768 (14) | 0.01316 (9) | |
S1 | 0.23929 (13) | 0.53924 (8) | 0.17876 (3) | 0.01771 (17) | |
S2 | 0.16398 (13) | 0.63461 (7) | 0.02734 (3) | 0.01529 (16) | |
N1 | 0.9852 (4) | −0.0154 (3) | 0.18942 (9) | 0.0145 (5) | |
H1A | 1.101 (4) | 0.019 (3) | 0.2088 (11) | 0.017* | |
N2 | 0.3566 (4) | 0.3104 (2) | 0.08004 (10) | 0.0131 (5) | |
N3 | 0.6329 (5) | 0.5527 (3) | 0.24980 (11) | 0.0256 (6) | |
N4 | 0.7198 (4) | 0.5617 (2) | 0.07025 (10) | 0.0146 (5) | |
C1 | 0.9770 (6) | −0.1462 (3) | 0.18806 (12) | 0.0172 (7) | |
H1 | 1.0885 | −0.1949 | 0.2073 | 0.021* | |
C2 | 0.8038 (6) | −0.2097 (3) | 0.15816 (13) | 0.0175 (7) | |
H2 | 0.7978 | −0.3010 | 0.1575 | 0.021* | |
C3 | 0.6387 (6) | −0.1364 (3) | 0.12916 (12) | 0.0164 (6) | |
H3 | 0.5228 | −0.1785 | 0.1086 | 0.020* | |
C4 | 0.6467 (5) | 0.0023 (3) | 0.13094 (11) | 0.0130 (6) | |
C5 | 0.8261 (5) | 0.0619 (3) | 0.16231 (11) | 0.0130 (6) | |
C6 | 0.8493 (5) | 0.2013 (3) | 0.16641 (12) | 0.0143 (6) | |
H6 | 0.9694 | 0.2383 | 0.1874 | 0.017* | |
C7 | 0.5052 (5) | 0.2244 (3) | 0.10681 (12) | 0.0134 (6) | |
C8 | 0.4792 (5) | 0.0866 (3) | 0.10222 (12) | 0.0121 (6) | |
C9 | 0.6932 (5) | 0.2789 (3) | 0.13918 (12) | 0.0134 (6) | |
H9 | 0.7085 | 0.3696 | 0.1416 | 0.016* | |
C10 | 0.2937 (5) | 0.0372 (3) | 0.06969 (11) | 0.0144 (6) | |
H10 | 0.2720 | −0.0529 | 0.0658 | 0.017* | |
C11 | 0.1457 (5) | 0.1239 (3) | 0.04383 (12) | 0.0148 (6) | |
H11 | 0.0210 | 0.0933 | 0.0225 | 0.018* | |
C12 | 0.1841 (5) | 0.2590 (3) | 0.04991 (12) | 0.0139 (6) | |
H12 | 0.0827 | 0.3163 | 0.0317 | 0.017* | |
C13 | 0.9030 (5) | 0.5913 (3) | 0.05257 (11) | 0.0124 (6) | |
C14 | 0.4718 (5) | 0.5465 (3) | 0.22029 (12) | 0.0155 (6) | |
Atomic displacement parameters (Å2) top | U11 | U22 | U33 | U12 | U13 | U23 |
Cu1 | 0.00972 (15) | 0.01546 (16) | 0.01432 (17) | 0.00013 (14) | −0.00014 (14) | 0.00009 (15) |
S1 | 0.0131 (3) | 0.0266 (4) | 0.0134 (4) | 0.0037 (3) | 0.0002 (3) | −0.0007 (3) |
S2 | 0.0097 (4) | 0.0211 (4) | 0.0151 (4) | −0.0013 (3) | 0.0002 (3) | 0.0047 (3) |
N1 | 0.0143 (11) | 0.0172 (13) | 0.0118 (12) | −0.0012 (11) | −0.0014 (9) | −0.0015 (11) |
N2 | 0.0125 (12) | 0.0158 (11) | 0.0109 (12) | 0.0014 (9) | 0.0014 (10) | −0.0011 (9) |
N3 | 0.0206 (14) | 0.0379 (16) | 0.0181 (13) | 0.0025 (13) | −0.0009 (12) | 0.0058 (12) |
N4 | 0.0121 (13) | 0.0154 (12) | 0.0162 (13) | 0.0013 (10) | −0.0030 (10) | 0.0002 (10) |
C1 | 0.0229 (17) | 0.0167 (15) | 0.0121 (16) | 0.0057 (13) | 0.0003 (12) | 0.0015 (13) |
C2 | 0.0248 (18) | 0.0122 (14) | 0.0154 (16) | 0.0020 (12) | −0.0030 (13) | 0.0019 (12) |
C3 | 0.0195 (16) | 0.0147 (13) | 0.0149 (15) | −0.0015 (13) | −0.0008 (13) | −0.0019 (12) |
C4 | 0.0132 (13) | 0.0166 (14) | 0.0093 (12) | −0.0008 (12) | 0.0004 (10) | −0.0003 (12) |
C5 | 0.0144 (14) | 0.0175 (14) | 0.0072 (14) | 0.0059 (11) | 0.0028 (11) | 0.0034 (11) |
C6 | 0.0118 (16) | 0.0170 (14) | 0.0142 (15) | −0.0010 (11) | −0.0026 (12) | −0.0036 (12) |
C7 | 0.0138 (14) | 0.0144 (14) | 0.0121 (15) | 0.0012 (11) | 0.0034 (12) | 0.0000 (12) |
C8 | 0.0128 (14) | 0.0134 (13) | 0.0102 (15) | 0.0006 (10) | 0.0004 (11) | 0.0017 (11) |
C9 | 0.0149 (15) | 0.0145 (14) | 0.0107 (14) | −0.0019 (11) | 0.0003 (12) | −0.0026 (12) |
C10 | 0.0161 (14) | 0.0160 (14) | 0.0112 (14) | −0.0026 (12) | 0.0021 (11) | −0.0015 (12) |
C11 | 0.0136 (16) | 0.0184 (14) | 0.0123 (14) | −0.0041 (12) | −0.0009 (12) | −0.0028 (12) |
C12 | 0.0123 (14) | 0.0194 (15) | 0.0099 (14) | 0.0031 (11) | 0.0009 (12) | 0.0013 (12) |
C13 | 0.0136 (15) | 0.0123 (13) | 0.0113 (14) | 0.0029 (12) | −0.0038 (12) | 0.0005 (11) |
C14 | 0.0153 (14) | 0.0194 (16) | 0.0118 (15) | 0.0048 (11) | 0.0040 (12) | 0.0036 (12) |
Geometric parameters (Å, º) top
Cu1—N4 | 1.954 (2) | C3—C4 | 1.413 (4) |
Cu1—N2 | 2.134 (2) | C3—H3 | 0.9300 |
Cu1—S2 | 2.3298 (8) | C4—C5 | 1.408 (4) |
Cu1—S1 | 2.3449 (9) | C4—C8 | 1.458 (4) |
S1—C14 | 1.661 (3) | C5—C6 | 1.428 (4) |
S2—C13i | 1.661 (3) | C6—C9 | 1.358 (4) |
N1—C1 | 1.332 (4) | C6—H6 | 0.9300 |
N1—C5 | 1.366 (4) | C7—C8 | 1.415 (4) |
N1—H1A | 0.882 (18) | C7—C9 | 1.436 (4) |
N2—C12 | 1.328 (4) | C8—C10 | 1.408 (4) |
N2—C7 | 1.378 (4) | C9—H9 | 0.9300 |
N3—C14 | 1.162 (4) | C10—C11 | 1.370 (4) |
N4—C13 | 1.163 (4) | C10—H10 | 0.9300 |
C1—C2 | 1.382 (4) | C11—H11 | 0.9300 |
C1—H1 | 0.9300 | C12—C11 | 1.401 (4) |
C2—C3 | 1.389 (4) | C12—H12 | 0.9300 |
C2—H2 | 0.9300 | C13—S2ii | 1.661 (3) |
| | | |
N4—Cu1—N2 | 107.20 (9) | N1—C5—C4 | 119.2 (3) |
N4—Cu1—S2 | 104.70 (7) | N1—C5—C6 | 118.6 (3) |
N2—Cu1—S2 | 112.11 (7) | C4—C5—C6 | 122.2 (3) |
N4—Cu1—S1 | 123.80 (8) | C9—C6—C5 | 118.9 (3) |
N2—Cu1—S1 | 99.01 (7) | C9—C6—H6 | 120.5 |
S2—Cu1—S1 | 109.96 (3) | C5—C6—H6 | 120.5 |
C14—S1—Cu1 | 105.43 (10) | N2—C7—C8 | 122.0 (3) |
C13i—S2—Cu1 | 97.12 (10) | N2—C7—C9 | 117.8 (3) |
C1—N1—C5 | 122.7 (3) | C8—C7—C9 | 120.2 (3) |
C1—N1—H1A | 116 (2) | C10—C8—C7 | 118.4 (3) |
C5—N1—H1A | 121 (2) | C10—C8—C4 | 123.0 (3) |
C12—N2—C7 | 117.3 (2) | C7—C8—C4 | 118.6 (3) |
C12—N2—Cu1 | 121.67 (19) | C11—C10—C8 | 118.9 (3) |
C7—N2—Cu1 | 120.94 (19) | C11—C10—H10 | 120.5 |
C13—N4—Cu1 | 172.0 (2) | C8—C10—H10 | 120.5 |
N1—C1—C2 | 120.4 (3) | C6—C9—C7 | 121.7 (3) |
N1—C1—H1 | 119.8 | C6—C9—H9 | 119.1 |
C2—C1—H1 | 119.8 | C7—C9—H9 | 119.1 |
C1—C2—C3 | 119.6 (3) | N3—C14—S1 | 179.1 (3) |
C1—C2—H2 | 120.2 | N2—C12—C11 | 124.0 (3) |
C3—C2—H2 | 120.2 | N2—C12—H12 | 118.0 |
C2—C3—C4 | 120.0 (3) | C11—C12—H12 | 118.0 |
C2—C3—H3 | 120.0 | N4—C13—S2ii | 179.6 (3) |
C4—C3—H3 | 120.0 | C10—C11—C12 | 119.3 (3) |
C5—C4—C3 | 118.1 (3) | C10—C11—H11 | 120.4 |
C5—C4—C8 | 118.3 (2) | C12—C11—H11 | 120.4 |
C3—C4—C8 | 123.5 (3) | | |
| | | |
N4—Cu1—S1—C14 | −18.74 (14) | N1—C5—C6—C9 | 179.4 (3) |
N2—Cu1—S1—C14 | 99.07 (13) | C4—C5—C6—C9 | 0.0 (4) |
S2—Cu1—S1—C14 | −143.35 (11) | C12—N2—C7—C8 | 0.8 (4) |
N4—Cu1—S2—C13i | −177.08 (12) | Cu1—N2—C7—C8 | 178.2 (2) |
N2—Cu1—S2—C13i | 67.04 (12) | C12—N2—C7—C9 | 179.6 (3) |
S1—Cu1—S2—C13i | −42.07 (10) | Cu1—N2—C7—C9 | −3.0 (4) |
N4—Cu1—N2—C12 | −127.5 (2) | N2—C7—C8—C10 | −0.7 (4) |
S2—Cu1—N2—C12 | −13.1 (2) | C9—C7—C8—C10 | −179.5 (3) |
S1—Cu1—N2—C12 | 102.8 (2) | N2—C7—C8—C4 | 178.8 (2) |
N4—Cu1—N2—C7 | 55.2 (2) | C9—C7—C8—C4 | 0.0 (4) |
S2—Cu1—N2—C7 | 169.57 (19) | C5—C4—C8—C10 | 179.9 (3) |
S1—Cu1—N2—C7 | −74.5 (2) | C3—C4—C8—C10 | −0.3 (4) |
C5—N1—C1—C2 | 0.4 (4) | C5—C4—C8—C7 | 0.4 (4) |
N1—C1—C2—C3 | 0.4 (5) | C3—C4—C8—C7 | −179.7 (3) |
C1—C2—C3—C4 | −0.8 (5) | C7—C8—C10—C11 | 0.0 (4) |
C2—C3—C4—C5 | 0.5 (4) | C4—C8—C10—C11 | −179.5 (3) |
C2—C3—C4—C8 | −179.4 (3) | C5—C6—C9—C7 | 0.4 (4) |
C1—N1—C5—C4 | −0.8 (4) | N2—C7—C9—C6 | −179.3 (3) |
C1—N1—C5—C6 | 179.8 (3) | C8—C7—C9—C6 | −0.5 (5) |
C3—C4—C5—N1 | 0.3 (4) | C7—N2—C12—C11 | −0.1 (4) |
C8—C4—C5—N1 | −179.8 (2) | Cu1—N2—C12—C11 | −177.5 (2) |
C3—C4—C5—C6 | 179.7 (3) | C8—C10—C11—C12 | 0.7 (4) |
C8—C4—C5—C6 | −0.4 (4) | N2—C12—C11—C10 | −0.6 (5) |
Symmetry codes: (i) x−1, y, z; (ii) x+1, y, z. |
Hydrogen-bond geometry (Å, º) top
D—H···A | D—H | H···A | D···A | D—H···A |
N1—H1A···N3iii | 0.88 (2) | 1.84 (2) | 2.710 (2) | 167 (1) |
Symmetry code: (iii) −x+2, y−1/2, −z+1/2. |