Supporting information
Crystallographic Information File (CIF) https://doi.org/10.1107/S1600536806056194/bc3026sup1.cif | |
Structure factor file (CIF format) https://doi.org/10.1107/S1600536806056194/bc3026Isup2.hkl |
Data collection: PROCESS-AUTO (Rigaku, 1998); cell refinement: PROCESS-AUTO; data reduction: CrystalStructure (Rigaku, 2005); program(s) used to solve structure: SHELXS97 (Sheldrick, 1997); program(s) used to refine structure: CRYSTALS (Betteridge et al., 2003); molecular graphics: ORTEP-3 for Windows (Farrugia, 1997) and VICS-II (Reference?); software used to prepare material for publication: CrystalStructure.
Cu2[Mo(CN)8]·4H2O | F(000) = 1952.00 |
Mr = 503.23 | Dx = 2.126 Mg m−3 Dm = 2.14 (9) Mg m−3 Dm measured by flotation in toluene and tetrabromoethane |
Orthorhombic, Pbcn | Mo Kα radiation, λ = 0.71075 Å |
Hall symbol: -P 2n 2ab | Cell parameters from 24924 reflections |
a = 11.868 (3) Å | θ = 3.2–27.5° |
b = 14.931 (3) Å | µ = 3.50 mm−1 |
c = 17.741 (4) Å | T = 90 K |
V = 3143.7 (13) Å3 | Cubic, purple |
Z = 8 | 0.10 × 0.10 × 0.10 mm |
Rigaku R-AXIS RAPID diffractometer | 2906 reflections with I > 2σ(I) |
Detector resolution: 10.00 pixels mm-1 | Rint = 0.038 |
ω scans | θmax = 27.5° |
Absorption correction: multi-scan (ABSCOR; Higashi, 1995) | h = −15→15 |
Tmin = 0.559, Tmax = 0.705 | k = −19→18 |
28148 measured reflections | l = −23→21 |
3605 independent reflections |
Refinement on F2 | H-atom parameters not refined |
R[F2 > 2σ(F2)] = 0.037 | w = 1/[0.0008Fo2 + σ(Fo2)]/(4Fo2) |
wR(F2) = 0.099 | (Δ/σ)max < 0.001 |
S = 1.01 | Δρmax = 3.41 e Å−3 |
3605 reflections | Δρmin = −0.73 e Å−3 |
209 parameters |
Refinement. Refinement using all reflections. The weighted R-factor (wR) and goodness of fit (S) are based on F2. R-factor (gt) are based on F. The threshold expression of F2 > 2.0 σ(F2) is used only for calculating R-factor (gt). |
x | y | z | Uiso*/Ueq | ||
Mo | 0.29045 (3) | 0.11916 (2) | 0.63722 (2) | 0.00419 (8) | |
Cu1 | 0.29040 (4) | −0.13933 (3) | 0.43014 (2) | 0.00835 (11) | |
Cu2 | 0.0000 | −0.10334 (4) | 0.7500 | 0.00760 (15) | |
Cu3 | 0.0000 | 0.34278 (4) | 0.7500 | 0.00724 (15) | |
O1 | 0.1220 (2) | −0.1573 (2) | 0.40914 (17) | 0.0235 (8) | |
O2 | −0.1556 (3) | −0.0884 (2) | 0.65069 (17) | 0.0292 (9) | |
O3 | 0.1269 (3) | 0.3392 (2) | 0.86412 (18) | 0.0309 (9) | |
O4 | 0.0071 (2) | −0.0876 (2) | 0.53070 (18) | 0.0271 (8) | |
N1 | 0.2588 (2) | −0.01934 (19) | 0.49310 (18) | 0.0108 (8) | |
N2 | 0.0816 (2) | −0.01159 (19) | 0.69120 (18) | 0.0112 (7) | |
N3 | 0.0903 (2) | 0.25040 (19) | 0.70009 (19) | 0.0135 (8) | |
N4 | 0.2240 (2) | 0.2611 (2) | 0.50229 (19) | 0.0128 (8) | |
N5 | 0.4202 (2) | −0.06399 (19) | 0.69443 (18) | 0.0099 (7) | |
N6 | 0.3013 (2) | 0.1102 (2) | 0.82185 (19) | 0.0140 (8) | |
N7 | 0.4196 (2) | 0.3023 (2) | 0.69456 (18) | 0.0126 (8) | |
N8 | 0.5437 (2) | 0.1316 (2) | 0.56187 (18) | 0.0109 (7) | |
C1 | 0.2674 (3) | 0.0310 (2) | 0.5416 (2) | 0.0083 (8) | |
C2 | 0.1510 (3) | 0.0342 (2) | 0.6680 (2) | 0.0089 (8) | |
C3 | 0.1571 (3) | 0.2037 (2) | 0.6762 (2) | 0.0094 (8) | |
C4 | 0.2457 (3) | 0.2090 (2) | 0.5468 (2) | 0.0089 (8) | |
C5 | 0.3766 (3) | −0.0009 (2) | 0.6714 (2) | 0.0093 (8) | |
C6 | 0.3024 (3) | 0.1138 (2) | 0.7581 (2) | 0.0110 (9) | |
C7 | 0.3748 (3) | 0.2392 (2) | 0.6733 (2) | 0.0096 (8) | |
C8 | 0.4539 (3) | 0.1258 (2) | 0.5846 (2) | 0.0093 (9) |
U11 | U22 | U33 | U12 | U13 | U23 | |
Mo | 0.00335 (18) | 0.00464 (17) | 0.00458 (17) | 0.00010 (11) | 0.00070 (11) | −0.00005 (10) |
Cu1 | 0.0063 (2) | 0.0121 (2) | 0.0066 (2) | −0.00105 (17) | 0.00090 (18) | 0.00124 (16) |
Cu2 | 0.0069 (3) | 0.0061 (2) | 0.0098 (3) | 0.0000 | 0.0043 (2) | 0.0000 |
Cu3 | 0.0057 (3) | 0.0049 (2) | 0.0111 (3) | 0.0000 | 0.0042 (2) | 0.0000 |
O1 | 0.0061 (15) | 0.0466 (18) | 0.0178 (15) | −0.0013 (13) | −0.0042 (12) | 0.0031 (13) |
O2 | 0.0234 (19) | 0.0428 (18) | 0.0215 (16) | 0.0063 (16) | −0.0017 (14) | 0.0054 (14) |
O3 | 0.0215 (19) | 0.0464 (19) | 0.0249 (17) | 0.0098 (16) | −0.0023 (14) | 0.0105 (14) |
O4 | 0.0219 (18) | 0.0360 (16) | 0.0235 (17) | −0.0046 (15) | 0.0023 (14) | −0.0060 (14) |
N1 | 0.0084 (17) | 0.0134 (15) | 0.0105 (15) | 0.0024 (12) | −0.0002 (13) | 0.0001 (12) |
N2 | 0.0112 (17) | 0.0077 (13) | 0.0149 (16) | −0.0015 (12) | 0.0022 (14) | −0.0007 (11) |
N3 | 0.0120 (18) | 0.0089 (13) | 0.0195 (17) | 0.0002 (13) | 0.0054 (15) | 0.0013 (12) |
N4 | 0.0117 (19) | 0.0147 (15) | 0.0120 (15) | 0.0043 (12) | 0.0008 (14) | 0.0003 (12) |
N5 | 0.0082 (16) | 0.0110 (14) | 0.0106 (15) | −0.0003 (12) | 0.0007 (13) | 0.0004 (11) |
N6 | 0.0147 (19) | 0.0186 (16) | 0.0086 (17) | 0.0006 (13) | −0.0026 (14) | −0.0007 (12) |
N7 | 0.0127 (18) | 0.0130 (15) | 0.0120 (15) | −0.0006 (13) | −0.0033 (14) | −0.0007 (12) |
N8 | 0.0077 (17) | 0.0125 (14) | 0.0126 (15) | −0.0001 (12) | 0.0015 (13) | 0.0001 (12) |
C1 | 0.0073 (18) | 0.0101 (16) | 0.0076 (17) | 0.0008 (13) | −0.0003 (14) | 0.0012 (13) |
C2 | 0.010 (2) | 0.0074 (15) | 0.0095 (17) | 0.0049 (14) | −0.0016 (15) | −0.0015 (13) |
C3 | 0.010 (2) | 0.0063 (15) | 0.0120 (17) | −0.0014 (14) | 0.0021 (15) | 0.0010 (13) |
C4 | 0.0056 (18) | 0.0121 (16) | 0.0090 (17) | 0.0000 (14) | −0.0003 (14) | −0.0021 (14) |
C5 | 0.0072 (18) | 0.0122 (16) | 0.0084 (16) | −0.0029 (14) | 0.0016 (15) | −0.0014 (13) |
C6 | 0.0073 (19) | 0.0130 (17) | 0.013 (2) | −0.0001 (13) | −0.0010 (15) | −0.0006 (13) |
C7 | 0.0070 (18) | 0.0123 (16) | 0.0097 (17) | 0.0049 (14) | 0.0023 (15) | 0.0009 (13) |
C8 | 0.012 (2) | 0.0091 (16) | 0.0073 (16) | 0.0001 (14) | 0.0005 (15) | 0.0023 (13) |
Mo—C1 | 2.165 (3) | Cu2—N7i | 1.966 (3) |
Mo—C2 | 2.155 (3) | Cu2—N7v | 1.966 (3) |
Mo—C3 | 2.139 (3) | Cu3—N3 | 1.958 (3) |
Mo—C4 | 2.158 (3) | Cu3—N3iv | 1.958 (3) |
Mo—C5 | 2.151 (3) | Cu3—N5vi | 1.951 (3) |
Mo—C6 | 2.152 (4) | Cu3—N5vii | 1.951 (3) |
Mo—C7 | 2.150 (3) | N1—C1 | 1.147 (4) |
Mo—C8 | 2.155 (4) | N2—C2 | 1.147 (4) |
Cu1—O1 | 2.051 (3) | N3—C3 | 1.138 (4) |
Cu1—N1 | 2.144 (2) | N4—C4 | 1.137 (4) |
Cu1—N4i | 1.970 (3) | N5—C5 | 1.150 (4) |
Cu1—N6ii | 1.974 (3) | N6—C6 | 1.131 (5) |
Cu1—N8iii | 1.977 (3) | N7—C7 | 1.146 (4) |
Cu2—N2 | 1.976 (3) | N8—C8 | 1.143 (5) |
Cu2—N2iv | 1.976 (3) | ||
Cu2···O2 | 2.562 (3) | O1···N3viii | 3.469 (4) |
Cu2···O2iv | 2.562 (3) | N1···O2viii | 3.255 (4) |
Cu3···O3 | 2.524 (3) | N1···O4 | 3.225 (4) |
Cu3···O3iv | 2.524 (3) | N1···O4viii | 3.562 (4) |
O2···Cu2 | 2.562 (3) | N2···O2 | 3.124 (4) |
O2···O4 | 2.875 (4) | N2···O2iv | 3.155 (4) |
O2···O3v | 2.810 (5) | N2···O4 | 3.190 (4) |
O2···N1viii | 3.255 (4) | N3···O3 | 3.227 (4) |
O2···N2 | 3.124 (4) | N3···O3iv | 3.114 (4) |
O2···N2iv | 3.155 (4) | N3···O1viii | 3.469 (4) |
O2···N6iv | 3.466 (4) | N4···O3xii | 3.374 (4) |
O2···N7i | 3.334 (4) | N4···N8xiii | 2.905 (4) |
O2···N7v | 3.317 (4) | N8···N4xiv | 2.905 (4) |
O4···O2 | 2.875 (4) | N8···N6xv | 2.783 (4) |
O4···O4viii | 2.839 (4) | N6···O2iv | 3.466 (4) |
O4···O1 | 2.755 (4) | N6···N8xv | 2.783 (4) |
O4···N1 | 3.225 (4) | N6···C8xv | 3.354 (5) |
O4···N1viii | 3.562 (4) | N5···O3i | 3.386 (4) |
O4···N2 | 3.190 (4) | N5···O3xvi | 3.030 (4) |
O4···N7i | 3.451 (4) | N5···N5xv | 2.734 (4) |
O4···C2 | 3.486 (4) | N5···C5xv | 3.517 (4) |
O4···C1 | 3.565 (5) | N7···O2vi | 3.334 (4) |
O3···Cu3 | 2.524 (3) | N7···O2ix | 3.317 (4) |
O3···O2ix | 2.810 (5) | N7···O4vi | 3.451 (4) |
O3···O1x | 2.832 (4) | N7···N7xv | 2.740 (4) |
O3···N3 | 3.227 (4) | N7···C7xv | 3.513 (5) |
O3···N3iv | 3.114 (4) | C2···O4 | 3.486 (4) |
O3···N4xi | 3.374 (4) | C5···N5xv | 3.517 (4) |
O3···N5vi | 3.386 (4) | C8···N6xv | 3.354 (5) |
O3···N5vii | 3.030 (4) | C7···N7xv | 3.513 (5) |
O1···O4 | 2.755 (4) | C1···O4 | 3.565 (5) |
O1···O3ii | 2.832 (4) | ||
C2—Mo—C5 | 78.65 (14) | N7i—Cu2—N7v | 88.38 (13) |
C2—Mo—C8 | 145.86 (12) | N3—Cu3—N3iv | 90.43 (13) |
C2—Mo—C4 | 111.41 (14) | N3—Cu3—N5vi | 90.50 (12) |
C2—Mo—C7 | 140.62 (13) | N3—Cu3—N5vii | 175.30 (14) |
C2—Mo—C3 | 72.42 (13) | N3iv—Cu3—N5vi | 175.30 (14) |
C2—Mo—C6 | 77.08 (13) | N3iv—Cu3—N5vii | 90.50 (13) |
C2—Mo—C1 | 75.11 (13) | N5vi—Cu3—N5vii | 88.95 (13) |
C5—Mo—C8 | 74.46 (13) | O1—Cu1—N1 | 91.91 (12) |
C5—Mo—C4 | 147.64 (13) | O1—Cu1—N4i | 86.28 (13) |
C5—Mo—C7 | 112.91 (14) | O1—Cu1—N8iii | 172.36 (12) |
C5—Mo—C3 | 138.81 (13) | O1—Cu1—N6ii | 85.16 (13) |
C5—Mo—C6 | 69.91 (13) | N1—Cu1—N4i | 106.09 (12) |
C5—Mo—C1 | 76.95 (13) | N1—Cu1—N8iii | 95.04 (12) |
C8—Mo—C4 | 82.60 (14) | N1—Cu1—N6ii | 109.53 (12) |
C8—Mo—C7 | 70.82 (13) | N4i—Cu1—N8iii | 94.80 (13) |
C8—Mo—C3 | 141.15 (12) | N4i—Cu1—N6ii | 143.56 (13) |
C8—Mo—C6 | 111.98 (14) | N8iii—Cu1—N6ii | 89.53 (13) |
C8—Mo—C1 | 78.60 (14) | Cu1—N1—C1 | 157.3 (3) |
C4—Mo—C7 | 79.49 (13) | Cu2—N2—C2 | 162.8 (3) |
C4—Mo—C3 | 72.02 (14) | Cu3—N3—C3 | 168.9 (3) |
C4—Mo—C6 | 141.34 (13) | Cu1vi—N4—C4 | 170.6 (3) |
C4—Mo—C1 | 76.37 (13) | Cu1iii—N8—C8 | 155.2 (3) |
C7—Mo—C3 | 75.90 (14) | Cu1x—N6—C6 | 164.3 (3) |
C7—Mo—C6 | 72.78 (13) | Cu3i—N5—C5 | 169.3 (3) |
C7—Mo—C1 | 143.02 (14) | Cu2vi—N7—C7 | 168.4 (3) |
C3—Mo—C6 | 75.44 (14) | Mo—C1—N1 | 176.0 (3) |
C3—Mo—C1 | 121.25 (14) | Mo—C2—N2 | 173.2 (3) |
C6—Mo—C1 | 140.08 (12) | Mo—C3—N3 | 176.1 (3) |
N2—Cu2—N2iv | 92.21 (12) | Mo—C4—N4 | 175.3 (3) |
N2—Cu2—N7i | 89.72 (12) | Mo—C5—N5 | 175.4 (3) |
N2—Cu2—N7v | 177.89 (12) | Mo—C6—N6 | 175.5 (3) |
N2iv—Cu2—N7i | 177.89 (12) | Mo—C7—N7 | 178.0 (3) |
N2iv—Cu2—N7v | 89.72 (12) | Mo—C8—N8 | 174.8 (3) |
N2—Cu2—N2iv—C2iv | 108.1 (9) | N5vii—Cu3—N5vi—C5vi | 24.9 (17) |
N2iv—Cu2—N2—C2 | 108.1 (9) | O1—Cu1—N1—C1 | 136.1 (7) |
N2—Cu2—N7i—C7i | 149.8 (16) | O1—Cu1—N4i—C4i | −42.4 (19) |
N7i—Cu2—N2—C2 | −71.0 (9) | O1—Cu1—N8iii—C8iii | 36.3 (13) |
N2—Cu2—N7v—C7v | −6 (4) | O1—Cu1—N6ii—C6ii | −69.5 (12) |
N7v—Cu2—N2—C2 | −96 (3) | N1—Cu1—N4i—C4i | 48.5 (19) |
N2iv—Cu2—N7i—C7i | −6 (4) | N4i—Cu1—N1—C1 | 49.4 (8) |
N7i—Cu2—N2iv—C2iv | −96 (3) | N1—Cu1—N8iii—C8iii | −119.2 (6) |
N2iv—Cu2—N7v—C7v | 149.8 (16) | N8iii—Cu1—N1—C1 | −47.1 (7) |
N7v—Cu2—N2iv—C2iv | −71.0 (9) | N1—Cu1—N6ii—C6ii | −159.8 (12) |
N7i—Cu2—N7v—C7v | −31.1 (16) | N6ii—Cu1—N1—C1 | −138.4 (7) |
N7v—Cu2—N7i—C7i | −31.1 (16) | N4i—Cu1—N8iii—C8iii | 134.2 (6) |
N3—Cu3—N3iv—C3iv | −125.3 (16) | N8iii—Cu1—N4i—C4i | 145.2 (19) |
N3iv—Cu3—N3—C3 | −125.3 (16) | N4i—Cu1—N6ii—C6ii | 7.6 (13) |
N3—Cu3—N5vi—C5vi | −150.5 (17) | N6ii—Cu1—N4i—C4i | −119.1 (19) |
N5vi—Cu3—N3—C3 | 59.3 (16) | N8iii—Cu1—N6ii—C6ii | 105.0 (12) |
N3—Cu3—N5vii—C5vii | 108 (2) | N6ii—Cu1—N8iii—C8iii | −9.6 (6) |
N5vii—Cu3—N3—C3 | −24 (2) | Cu1vi—N4—C4—Mo | 45 (5) |
N3iv—Cu3—N5vi—C5vi | 108 (2) | Cu1iii—N8—C8—Mo | 20 (3) |
N5vi—Cu3—N3iv—C3iv | −24 (2) | Cu1x—N6—C6—Mo | −85 (4) |
N3iv—Cu3—N5vii—C5vii | −150.5 (17) | Cu3i—N5—C5—Mo | −38 (5) |
N5vii—Cu3—N3iv—C3iv | 59.3 (16) | Cu2vi—N7—C7—Mo | 14 (11) |
N5vi—Cu3—N5vii—C5vii | 24.9 (17) |
Symmetry codes: (i) −x+1/2, y−1/2, z; (ii) x, −y, z−1/2; (iii) −x+1, −y, −z+1; (iv) −x, y, −z+3/2; (v) x−1/2, y−1/2, −z+3/2; (vi) −x+1/2, y+1/2, z; (vii) x−1/2, y+1/2, −z+3/2; (viii) −x, −y, −z+1; (ix) x+1/2, y+1/2, −z+3/2; (x) x, −y, z+1/2; (xi) −x+1/2, −y+1/2, z+1/2; (xii) −x+1/2, −y+1/2, z−1/2; (xiii) x−1/2, −y+1/2, −z+1; (xiv) x+1/2, −y+1/2, −z+1; (xv) −x+1, y, −z+3/2; (xvi) x+1/2, y−1/2, −z+3/2. |