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metal-organic compounds
The title complex, poly[bis(N-methylformamide)tetra-μ-thiocyanatocadmium(II)mercury(II)], [CdHg(NCS)4(C2H5NO)2]n, contains slightly distorted octahedral CdN4O2 and tetrahedral HgS4. The CdII atom is coordinated by the N atoms of four SCN groups and O atoms of two N-methylformamide ligands in a cis orientation. The HgII atom is coordinated by S atoms of one independent and three symmetry-related SCN groups. The two metal atoms, viz. CdII and HgII, are connected by an —S=C=N— bridge, forming an infinite three-dimensional network.
Supporting information
Crystallographic Information File (CIF) https://doi.org/10.1107/S1600536805015394/ci6548sup1.cif | |
Structure factor file (CIF format) https://doi.org/10.1107/S1600536805015394/ci6548Isup2.hkl |
CCDC reference: 274358
Key indicators
- Single-crystal X-ray study
- T = 293 K
- Mean (N-C) = 0.030 Å
- R factor = 0.041
- wR factor = 0.081
- Data-to-parameter ratio = 10.6
checkCIF/PLATON results
No syntax errors found
Alert level C STRVA01_ALERT_4_C Flack test results are ambiguous. From the CIF: _refine_ls_abs_structure_Flack 0.420 From the CIF: _refine_ls_abs_structure_Flack_su 0.020 PLAT033_ALERT_2_C Flack Parameter Value Deviates from Zero ....... 0.42 PLAT220_ALERT_2_C Large Non-Solvent C Ueq(max)/Ueq(min) ... 3.07 Ratio PLAT241_ALERT_2_C Check High Ueq as Compared to Neighbors for S1 PLAT241_ALERT_2_C Check High Ueq as Compared to Neighbors for N1 PLAT241_ALERT_2_C Check High Ueq as Compared to Neighbors for N3 PLAT241_ALERT_2_C Check High Ueq as Compared to Neighbors for N4 PLAT242_ALERT_2_C Check Low Ueq as Compared to Neighbors for Cd1 PLAT242_ALERT_2_C Check Low Ueq as Compared to Neighbors for C1 PLAT242_ALERT_2_C Check Low Ueq as Compared to Neighbors for C3 PLAT242_ALERT_2_C Check Low Ueq as Compared to Neighbors for C4 PLAT731_ALERT_1_C Bond Calc 1.21(2), Rep 1.214(9) ...... 2.22 su-Rat O2 -C7 1.555 1.555 PLAT731_ALERT_1_C Bond Calc 1.46(3), Rep 1.456(10) ...... 3.00 su-Rat N5 -C6 1.555 1.555 PLAT731_ALERT_1_C Bond Calc 1.45(3), Rep 1.455(10) ...... 3.00 su-Rat N6 -C8 1.555 1.555 PLAT764_ALERT_4_C Overcomplete CIF Bond List Detected (Rep/Expd) . 1.12 Ratio
Alert level G REFLT03_ALERT_4_G WARNING: Large fraction of Friedel related reflns may be needed to determine absolute structure From the CIF: _diffrn_reflns_theta_max 26.00 From the CIF: _reflns_number_total 2129 Count of symmetry unique reflns 1978 Completeness (_total/calc) 107.63% TEST3: Check Friedels for noncentro structure Estimate of Friedel pairs measured 151 Fraction of Friedel pairs measured 0.076 Are heavy atom types Z>Si present yes
0 ALERT level A = In general: serious problem 0 ALERT level B = Potentially serious problem 15 ALERT level C = Check and explain 1 ALERT level G = General alerts; check 3 ALERT type 1 CIF construction/syntax error, inconsistent or missing data 10 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 3 ALERT type 4 Improvement, methodology, query or suggestion
Computing details top
Data collection: XSCANS (Bruker,1996); cell refinement: XSCANS; data reduction: SHELXTL (Bruker, 1997); program(s) used to solve structure: SIR97 (Altomare et al., 1999); program(s) used to refine structure: SHELXTL; molecular graphics: SHELXTL; software used to prepare material for publication: SHELXTL.
poly[bis(N-methylformamide)tetra-µ-thiocyanato-cadmium(II)mercury(II)] top
Crystal data top
[CdHg(NCS)4(C2H5NO)2] | F(000) = 1232 |
Mr = 663.45 | Dx = 2.282 Mg m−3 |
Orthorhombic, Pna21 | Mo Kα radiation, λ = 0.71069 Å |
Hall symbol: P 2c -2n | Cell parameters from 57 reflections |
a = 16.244 (2) Å | θ = 4.8–12.5° |
b = 7.7670 (8) Å | µ = 9.49 mm−1 |
c = 15.3043 (19) Å | T = 293 K |
V = 1930.9 (4) Å3 | Prism, colourless |
Z = 4 | 0.18 × 0.16 × 0.13 mm |
Data collection top
Bruker P4 diffractometer | 1497 reflections with I > 2σ(I) |
Radiation source: fine-focus sealed tube | Rint = 0.038 |
Graphite monochromator | θmax = 26.0°, θmin = 2.5° |
ω scans | h = −1→20 |
Absorption correction: ψ scan (XSCANS; Bruker, 1996) | k = −9→1 |
Tmin = 0.191, Tmax = 0.290 | l = −18→1 |
2617 measured reflections | 3 standard reflections every 97 reflections |
2129 independent reflections | intensity decay: none |
Refinement top
Refinement on F2 | Hydrogen site location: inferred from neighbouring sites |
Least-squares matrix: full | H-atom parameters constrained |
R[F2 > 2σ(F2)] = 0.041 | w = 1/[σ2(Fo2) + (0.0314P)2] where P = (Fo2 + 2Fc2)/3 |
wR(F2) = 0.081 | (Δ/σ)max = 0.001 |
S = 0.97 | Δρmax = 0.63 e Å−3 |
2129 reflections | Δρmin = −0.88 e Å−3 |
201 parameters | Extinction correction: SHELXTL, Fc*=kFc[1+0.001xFc2λ3/sin(2θ)]-1/4 |
19 restraints | Extinction coefficient: 0.00277 (15) |
Primary atom site location: structure-invariant direct methods | Absolute structure: Flack (1983), 151 Friedel pairs |
Secondary atom site location: difference Fourier map | Absolute structure parameter: 0.42 (2) |
Fractional atomic coordinates and isotropic or equivalent isotropic displacement parameters (Å2) top
x | y | z | Uiso*/Ueq | ||
Hg1 | 0.42893 (4) | 1.04049 (8) | 0.43517 (5) | 0.0566 (2) | |
Cd1 | 0.62078 (7) | 0.50702 (15) | 0.24017 (12) | 0.0483 (3) | |
S1 | 0.4467 (4) | 0.7344 (7) | 0.4881 (4) | 0.0852 (18) | |
O1 | 0.7102 (7) | 0.7384 (12) | 0.2424 (10) | 0.069 (3) | |
O2 | 0.7083 (8) | 0.3781 (16) | 0.1432 (8) | 0.062 (3) | |
N1 | 0.5378 (9) | 0.623 (2) | 0.3449 (12) | 0.074 (5) | |
N2 | 0.7044 (8) | 0.3802 (19) | 0.3457 (12) | 0.062 (4) | |
N3 | 0.5469 (10) | 0.652 (2) | 0.1335 (12) | 0.077 (5) | |
N4 | 0.5462 (9) | 0.258 (2) | 0.2328 (12) | 0.073 (5) | |
N5 | 0.7479 (10) | 1.016 (2) | 0.2332 (16) | 0.097 (7) | |
H5N | 0.7325 | 1.1173 | 0.2169 | 0.116* | |
N6 | 0.8193 (9) | 0.383 (2) | 0.0536 (10) | 0.080 (5) | |
H6N | 0.8598 | 0.4444 | 0.0348 | 0.096* | |
C1 | 0.5021 (11) | 0.670 (2) | 0.4042 (13) | 0.061 (6) | |
C2 | 0.7448 (9) | 0.351 (2) | 0.4047 (12) | 0.054 (5) | |
C3 | 0.5069 (9) | 0.701 (2) | 0.0785 (12) | 0.044 (4) | |
C4 | 0.4970 (10) | 0.1554 (19) | 0.2469 (12) | 0.049 (4) | |
C5 | 0.6911 (10) | 0.8875 (16) | 0.2323 (17) | 0.072 (6) | |
H5 | 0.6360 | 0.9150 | 0.2237 | 0.086* | |
C6 | 0.8331 (11) | 0.993 (3) | 0.260 (2) | 0.133 (10) | |
H6A | 0.8618 | 1.1007 | 0.2557 | 0.199* | |
H6B | 0.8591 | 0.9094 | 0.2232 | 0.199* | |
H6C | 0.8346 | 0.9537 | 0.3197 | 0.199* | |
C7 | 0.7699 (9) | 0.449 (2) | 0.1164 (12) | 0.061 (6) | |
H7 | 0.7841 | 0.5546 | 0.1406 | 0.074* | |
C8 | 0.8063 (13) | 0.213 (3) | 0.0165 (17) | 0.126 (10) | |
H8A | 0.8484 | 0.1892 | −0.0258 | 0.188* | |
H8B | 0.7534 | 0.2090 | −0.0114 | 0.188* | |
H8C | 0.8084 | 0.1284 | 0.0622 | 0.188* | |
S3 | 0.4535 (3) | 0.7702 (7) | −0.0056 (4) | 0.0620 (13) | |
S4 | 0.4260 (3) | 0.0136 (6) | 0.2704 (3) | 0.0718 (15) | |
S2 | 0.8042 (3) | 0.2952 (7) | 0.4873 (4) | 0.0742 (16) |
Atomic displacement parameters (Å2) top
U11 | U22 | U33 | U12 | U13 | U23 | |
Hg1 | 0.0579 (4) | 0.0615 (4) | 0.0504 (3) | 0.0109 (3) | 0.0010 (5) | −0.0087 (6) |
Cd1 | 0.0499 (6) | 0.0474 (6) | 0.0477 (6) | 0.0014 (6) | 0.0035 (7) | −0.0017 (7) |
S1 | 0.128 (5) | 0.062 (3) | 0.065 (3) | 0.023 (3) | 0.039 (4) | 0.015 (3) |
O1 | 0.065 (7) | 0.049 (7) | 0.094 (10) | −0.004 (6) | 0.018 (9) | −0.007 (9) |
O2 | 0.059 (7) | 0.063 (8) | 0.065 (9) | −0.026 (7) | 0.012 (7) | −0.017 (7) |
N1 | 0.068 (10) | 0.092 (12) | 0.061 (10) | 0.038 (9) | −0.001 (9) | −0.024 (11) |
N2 | 0.057 (9) | 0.066 (9) | 0.064 (10) | 0.009 (8) | −0.012 (10) | −0.005 (10) |
N3 | 0.077 (12) | 0.083 (12) | 0.069 (12) | −0.011 (10) | −0.010 (11) | 0.006 (11) |
N4 | 0.082 (11) | 0.071 (10) | 0.065 (11) | −0.028 (9) | −0.005 (10) | −0.010 (11) |
N5 | 0.109 (14) | 0.039 (8) | 0.142 (18) | 0.014 (11) | −0.046 (16) | −0.005 (14) |
N6 | 0.073 (11) | 0.112 (14) | 0.054 (10) | −0.032 (10) | 0.017 (10) | −0.016 (11) |
C1 | 0.068 (12) | 0.039 (9) | 0.078 (18) | 0.011 (9) | −0.001 (11) | −0.006 (10) |
C2 | 0.040 (8) | 0.055 (10) | 0.066 (15) | −0.011 (8) | −0.001 (9) | 0.008 (10) |
C3 | 0.033 (9) | 0.049 (10) | 0.048 (11) | −0.014 (8) | 0.014 (8) | −0.006 (10) |
C4 | 0.073 (12) | 0.037 (8) | 0.037 (9) | −0.003 (8) | −0.004 (10) | 0.003 (10) |
C5 | 0.053 (11) | 0.045 (10) | 0.116 (19) | 0.015 (9) | −0.004 (14) | 0.001 (15) |
C6 | 0.132 (16) | 0.105 (14) | 0.16 (2) | −0.028 (14) | −0.024 (16) | −0.004 (15) |
C7 | 0.049 (10) | 0.064 (15) | 0.072 (14) | 0.010 (11) | 0.003 (11) | −0.014 (13) |
C8 | 0.114 (15) | 0.123 (16) | 0.140 (18) | −0.032 (13) | 0.033 (14) | −0.056 (14) |
S3 | 0.052 (3) | 0.075 (3) | 0.059 (3) | −0.002 (2) | −0.006 (3) | 0.005 (3) |
S4 | 0.092 (4) | 0.079 (3) | 0.044 (3) | −0.029 (3) | −0.007 (3) | −0.006 (3) |
S2 | 0.051 (3) | 0.103 (4) | 0.069 (3) | −0.026 (3) | −0.010 (3) | 0.032 (3) |
Geometric parameters (Å, º) top
Hg1—S2i | 2.524 (4) | N5—H5N | 0.86 |
Hg1—S1 | 2.528 (5) | N6—C7 | 1.352 (10) |
Hg1—S4ii | 2.531 (5) | N6—C8 | 1.455 (10) |
Hg1—S3iii | 2.576 (5) | N6—H6N | 0.86 |
Cd1—N1 | 2.281 (16) | C2—S2 | 1.649 (17) |
Cd1—O2 | 2.286 (12) | C3—S3 | 1.643 (19) |
Cd1—N4 | 2.286 (15) | C4—S4 | 1.635 (17) |
Cd1—O1 | 2.311 (10) | C5—H5 | 0.93 |
Cd1—N3 | 2.316 (18) | C6—H6A | 0.96 |
Cd1—N2 | 2.328 (16) | C6—H6B | 0.96 |
S1—C1 | 1.646 (19) | C6—H6C | 0.96 |
O1—C5 | 1.208 (9) | C7—H7 | 0.93 |
O2—C7 | 1.214 (9) | C8—H8A | 0.96 |
N1—C1 | 1.14 (2) | C8—H8B | 0.96 |
N2—C2 | 1.14 (2) | C8—H8C | 0.96 |
N3—C3 | 1.13 (2) | S3—Hg1iv | 2.576 (5) |
N4—C4 | 1.149 (18) | S4—Hg1v | 2.531 (5) |
N5—C5 | 1.360 (10) | S2—Hg1vi | 2.524 (4) |
N5—C6 | 1.456 (10) | ||
S2i—Hg1—S1 | 117.8 (2) | C6—N5—H5N | 118.1 |
S2i—Hg1—S4ii | 110.0 (2) | C7—N6—C8 | 122.2 (17) |
S1—Hg1—S4ii | 104.11 (19) | C7—N6—H6N | 118.9 |
S2i—Hg1—S3iii | 101.26 (16) | C8—N6—H6N | 118.9 |
S1—Hg1—S3iii | 109.8 (2) | N1—C1—S1 | 177.5 (18) |
S4ii—Hg1—S3iii | 114.33 (17) | N2—C2—S2 | 176.1 (18) |
N1—Cd1—O2 | 175.7 (6) | N3—C3—S3 | 176.5 (16) |
N1—Cd1—N4 | 93.3 (6) | N4—C4—S4 | 177.7 (18) |
O2—Cd1—N4 | 85.8 (5) | O1—C5—N5 | 122.0 (15) |
N1—Cd1—O1 | 93.0 (5) | O1—C5—H5 | 119.0 |
O2—Cd1—O1 | 87.7 (4) | N5—C5—H5 | 119.0 |
N4—Cd1—O1 | 172.9 (5) | N5—C6—H6A | 109.5 |
N1—Cd1—N3 | 89.8 (5) | N5—C6—H6B | 109.5 |
O2—Cd1—N3 | 94.4 (6) | H6A—C6—H6B | 109.5 |
N4—Cd1—N3 | 95.8 (6) | N5—C6—H6C | 109.5 |
O1—Cd1—N3 | 87.6 (5) | H6A—C6—H6C | 109.5 |
N1—Cd1—N2 | 91.4 (6) | H6B—C6—H6C | 109.5 |
O2—Cd1—N2 | 84.4 (4) | O2—C7—N6 | 124.0 (17) |
N4—Cd1—N2 | 89.1 (6) | O2—C7—H7 | 118.0 |
O1—Cd1—N2 | 87.3 (5) | N6—C7—H7 | 118.0 |
N3—Cd1—N2 | 174.8 (6) | N6—C8—H8A | 109.5 |
C1—S1—Hg1 | 95.6 (7) | N6—C8—H8B | 109.5 |
C5—O1—Cd1 | 125.6 (11) | H8A—C8—H8B | 109.5 |
C7—O2—Cd1 | 122.3 (11) | N6—C8—H8C | 109.5 |
C1—N1—Cd1 | 171.5 (16) | H8A—C8—H8C | 109.5 |
C2—N2—Cd1 | 165.9 (15) | H8B—C8—H8C | 109.5 |
C3—N3—Cd1 | 170.6 (17) | C3—S3—Hg1iv | 94.1 (5) |
C4—N4—Cd1 | 161.2 (16) | C4—S4—Hg1v | 98.7 (6) |
C5—N5—C6 | 123.8 (16) | C2—S2—Hg1vi | 95.4 (6) |
C5—N5—H5N | 118.1 | ||
S2i—Hg1—S1—C1 | 154.3 (6) | O2—Cd1—N2—C2 | 133 (6) |
S4ii—Hg1—S1—C1 | 32.3 (7) | N4—Cd1—N2—C2 | −141 (6) |
S3iii—Hg1—S1—C1 | −90.6 (7) | O1—Cd1—N2—C2 | 45 (6) |
N1—Cd1—O1—C5 | −54 (2) | N1—Cd1—N4—C4 | −2 (5) |
O2—Cd1—O1—C5 | 130 (2) | O2—Cd1—N4—C4 | 174 (5) |
N3—Cd1—O1—C5 | 35 (2) | N3—Cd1—N4—C4 | −92 (5) |
N2—Cd1—O1—C5 | −146 (2) | N2—Cd1—N4—C4 | 89 (5) |
O1—Cd1—O2—C7 | −2.3 (16) | Cd1—O1—C5—N5 | −178.9 (19) |
N3—Cd1—O2—C7 | 85.1 (16) | C6—N5—C5—O1 | −11 (5) |
N2—Cd1—O2—C7 | −89.8 (16) | Cd1—O2—C7—N6 | −174.0 (15) |
N1—Cd1—N2—C2 | −48 (6) | C8—N6—C7—O2 | −5 (3) |
Symmetry codes: (i) x−1/2, −y+3/2, z; (ii) x, y+1, z; (iii) −x+1, −y+2, z+1/2; (iv) −x+1, −y+2, z−1/2; (v) x, y−1, z; (vi) x+1/2, −y+3/2, z. |
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