Supporting information
Crystallographic Information File (CIF) https://doi.org/10.1107/S160053680302782X/ob6329sup1.cif | |
Structure factor file (CIF format) https://doi.org/10.1107/S160053680302782X/ob6329Isup2.hkl |
CCDC reference: 231821
Data collection: SMART (Bruker, 2001); cell refinement: SAINT (Bruker, 2001); data reduction: SAINT; program(s) used to solve structure: SHELXS97 (Sheldrick, 1997); program(s) used to refine structure: SHELXL97 (Sheldrick, 1997); molecular graphics: KENX (Sakai, 2002); software used to prepare material for publication: SHELXL97, TEXSAN (Molecular Structure Corporation, 2001), KENX and ORTEPII (Johnson, 1976).
[Pt2(C4H7O2)2(NH3)4]2(ClO4)4 | Z = 2 |
Mr = 1662.82 | F(000) = 1552 |
Triclinic, P1 | Dx = 2.509 Mg m−3 |
Hall symbol: -P 1 | Mo Kα radiation, λ = 0.71073 Å |
a = 10.1557 (6) Å | Cell parameters from 5928 reflections |
b = 14.5963 (8) Å | θ = 2.2–28.3° |
c = 15.5209 (9) Å | µ = 13.00 mm−1 |
α = 74.354 (1)° | T = 296 K |
β = 84.621 (1)° | Prism, yellow |
γ = 85.052 (1)° | 0.31 × 0.14 × 0.05 mm |
V = 2201.3 (2) Å3 |
Bruker SMART APEX CCD-detector diffractometer | 10024 independent reflections |
Radiation source: fine-focus sealed tube | 7784 reflections with I > 2σ(I) |
Graphite monochromator | Rint = 0.058 |
Detector resolution: 8.366 pixels mm-1 | θmax = 27.5°, θmin = 2.2° |
ω scans | h = −13→13 |
Absorption correction: multi-scan (SADABS; Sheldrick, 1996) | k = −18→18 |
Tmin = 0.205, Tmax = 0.536 | l = −20→20 |
21380 measured reflections |
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)] = 0.043 | Hydrogen site location: inferred from neighbouring sites |
wR(F2) = 0.102 | H-atom parameters constrained |
S = 0.96 | w = 1/[σ2(Fo2) + (0.0372P)2] where P = (Fo2 + 2Fc2)/3 |
10024 reflections | (Δ/σ)max < 0.001 |
497 parameters | Δρmax = 2.97 e Å−3 |
49 restraints | Δρmin = −2.16 e Å−3 |
Experimental. The first 50 frames were rescanned at the end of data collection to evaluate any possible decay phenomenon. Since it was judged to be negligible, no decay correction was applied to the data. |
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. Mean-plane data from final SHELXL refinement run:- Least-squares planes (x,y,z in crystal coordinates) and deviations from them (* indicates atom used to define plane) -2.2992 (0.0211) x + 13.8320 (0.0099) y + 2.4412 (0.0317) z = 6.5912 (0.0180) * -0.0026 (0.0028) N1 * 0.0026 (0.0028) N2 * 0.0026 (0.0028) O1 * -0.0026 (0.0028) O3 - 0.0813 (0.0029) Pt1 - 2.9353 (0.0030) Pt2 Rms deviation of fitted atoms = 0.0026 -3.9774 (0.0204) x + 10.7045 (0.0218) y + 10.0759 (0.0257) z = 6.1949 (0.0140) Angle to previous plane (with approximate e.s.d.) = 37.24 (0.18) * 0.0125 (0.0030) N3 * -0.0127 (0.0030) N4 * -0.0124 (0.0030) O2 * 0.0126 (0.0030) O4 0.1024 (0.0030) Pt2 2.9081 (0.0032) Pt1 Rms deviation of fitted atoms = 0.0126 -3.0787 (0.0224) x + 13.1802 (0.0150) y + 6.2784 (0.0322) z = 2.5589 (0.0125) Angle to previous plane (with approximate e.s.d.) = 20.69 (1/4) * -0.0121 (0.0033) N5 * 0.0120 (0.0032) N6 * 0.0119 (0.0032) O5 * -0.0119 (0.0032) O7 - 0.0880 (0.0032) Pt3 - 2.9164 (0.0037) Pt4 Rms deviation of fitted atoms = 0.0120 -2.4050 (0.0237) x + 8.0743 (0.0289) y + 13.6666 (0.0180) z = 0.3493 (0.0126) Angle to previous plane (with approximate e.s.d.) = 40.36 (0.22) * 0.0138 (0.0032) N7 * -0.0139 (0.0033) N8 * -0.0137 (0.0032) O6 * 0.0139 (0.0033) O8 0.0841 (0.0033) Pt4 2.9313 (0.0035) Pt3 Rms deviation of fitted atoms = 0.0138 |
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. |
x | y | z | Uiso*/Ueq | Occ. (<1) | |
Pt1 | 0.03826 (3) | 0.38756 (2) | 0.50681 (2) | 0.03241 (9) | |
Pt2 | 0.16675 (3) | 0.20936 (2) | 0.46839 (2) | 0.02939 (9) | |
Pt3 | 0.34062 (3) | 0.17275 (2) | 0.19793 (2) | 0.03620 (9) | |
Pt4 | 0.46568 (3) | 0.03829 (2) | 0.09104 (2) | 0.03489 (9) | |
Cl1 | 0.8086 (2) | 0.12558 (16) | 0.29275 (16) | 0.0472 (5) | |
Cl2 | 0.3480 (2) | −0.09795 (15) | 0.44009 (16) | 0.0439 (5) | |
Cl3 | 0.4254 (2) | 0.30054 (16) | 0.71422 (19) | 0.0571 (6) | |
Cl4 | −0.0307 (2) | 0.13471 (18) | 0.76021 (16) | 0.0509 (6) | |
O1 | −0.0156 (6) | 0.4071 (4) | 0.3798 (4) | 0.0413 (14) | |
O2 | 0.0737 (6) | 0.2711 (4) | 0.3547 (4) | 0.0430 (15) | |
O3 | 0.2212 (5) | 0.4328 (4) | 0.4552 (4) | 0.0407 (14) | |
O4 | 0.3154 (5) | 0.2981 (4) | 0.4239 (4) | 0.0390 (14) | |
O5 | 0.2335 (6) | 0.2077 (4) | 0.0879 (4) | 0.0521 (17) | |
O6 | 0.2998 (6) | 0.0918 (4) | 0.0231 (4) | 0.0469 (15) | |
O7 | 0.4934 (6) | 0.2474 (4) | 0.1282 (4) | 0.0513 (17) | |
O8 | 0.5598 (6) | 0.1591 (4) | 0.0311 (4) | 0.0443 (15) | |
O9 | 0.8830 (10) | 0.1513 (7) | 0.2094 (6) | 0.112 (3) | |
O10 | 0.8979 (7) | 0.0747 (6) | 0.3568 (5) | 0.077 (2) | |
O11 | 0.7075 (7) | 0.0637 (6) | 0.2909 (7) | 0.086 (3) | |
O12 | 0.7473 (8) | 0.2079 (5) | 0.3149 (6) | 0.091 (3) | |
O13 | 0.2622 (7) | −0.0176 (4) | 0.4497 (5) | 0.068 (2) | |
O14 | 0.2707 (7) | −0.1785 (5) | 0.4596 (6) | 0.076 (2) | |
O15 | 0.4471 (7) | −0.1144 (6) | 0.5015 (6) | 0.079 (2) | |
O16 | 0.4078 (8) | −0.0772 (5) | 0.3508 (5) | 0.076 (2) | |
O17A | 0.5632 (9) | 0.3129 (12) | 0.6867 (10) | 0.0924 (19)* | 0.50 |
O17B | 0.5628 (9) | 0.3072 (14) | 0.7117 (11) | 0.0924 (19)* | 0.50 |
O18A | 0.3704 (14) | 0.2595 (10) | 0.6529 (9) | 0.0924 (19)* | 0.50 |
O18B | 0.3866 (15) | 0.3167 (12) | 0.6238 (7) | 0.0924 (19)* | 0.50 |
O19A | 0.4141 (14) | 0.2374 (9) | 0.8016 (7) | 0.0924 (19)* | 0.50 |
O19B | 0.3904 (15) | 0.2071 (8) | 0.7615 (10) | 0.0924 (19)* | 0.50 |
O20A | 0.3591 (16) | 0.3897 (7) | 0.7125 (10) | 0.0924 (19)* | 0.50 |
O20B | 0.3573 (18) | 0.3747 (11) | 0.7474 (13) | 0.0924 (19)* | 0.50 |
O21A | −0.0929 (16) | 0.2304 (7) | 0.7569 (10) | 0.105 (2)* | 0.50 |
O21B | −0.079 (2) | 0.2141 (11) | 0.7944 (14) | 0.105 (2)* | 0.50 |
O22A | −0.0620 (15) | 0.0738 (9) | 0.8456 (7) | 0.105 (2)* | 0.50 |
O22B | −0.0962 (18) | 0.0528 (10) | 0.8099 (12) | 0.105 (2)* | 0.50 |
O23A | 0.1062 (9) | 0.1439 (11) | 0.7393 (11) | 0.105 (2)* | 0.50 |
O23B | 0.1056 (10) | 0.1094 (14) | 0.7748 (15) | 0.105 (2)* | 0.50 |
O24A | −0.0881 (15) | 0.1021 (11) | 0.6930 (9) | 0.105 (2)* | 0.50 |
O24B | −0.063 (2) | 0.1497 (14) | 0.6697 (8) | 0.105 (2)* | 0.50 |
N1 | −0.1493 (7) | 0.3533 (5) | 0.5563 (6) | 0.049 (2) | |
H1A | −0.2033 | 0.4058 | 0.5456 | 0.073* | |
H1B | −0.1500 | 0.3271 | 0.6152 | 0.073* | |
H1C | −0.1764 | 0.3121 | 0.5297 | 0.073* | |
N2 | 0.0911 (7) | 0.3805 (5) | 0.6310 (5) | 0.0404 (17) | |
H2A | 0.1791 | 0.3773 | 0.6306 | 0.061* | |
H2B | 0.0599 | 0.3288 | 0.6698 | 0.061* | |
H2C | 0.0576 | 0.4322 | 0.6472 | 0.061* | |
N3 | 0.0287 (7) | 0.1122 (5) | 0.5082 (5) | 0.0449 (18) | |
H3A | −0.0227 | 0.1170 | 0.4636 | 0.067* | |
H3B | −0.0206 | 0.1229 | 0.5554 | 0.067* | |
H3C | 0.0685 | 0.0540 | 0.5231 | 0.067* | |
N4 | 0.2709 (7) | 0.1395 (5) | 0.5723 (5) | 0.0445 (18) | |
H4A | 0.3441 | 0.1694 | 0.5712 | 0.067* | |
H4B | 0.2929 | 0.0803 | 0.5686 | 0.067* | |
H4C | 0.2221 | 0.1378 | 0.6233 | 0.067* | |
N5 | 0.1818 (7) | 0.1079 (5) | 0.2683 (5) | 0.0488 (19) | |
H5A | 0.1085 | 0.1447 | 0.2531 | 0.073* | |
H5B | 0.1901 | 0.0982 | 0.3267 | 0.073* | |
H5C | 0.1765 | 0.0522 | 0.2561 | 0.073* | |
N6 | 0.4369 (7) | 0.1494 (5) | 0.3100 (5) | 0.0424 (17) | |
H6A | 0.5185 | 0.1693 | 0.2957 | 0.064* | |
H6B | 0.4413 | 0.0874 | 0.3374 | 0.064* | |
H6C | 0.3936 | 0.1813 | 0.3466 | 0.064* | |
N7 | 0.3775 (7) | −0.0855 (5) | 0.1435 (5) | 0.0485 (19) | |
H7A | 0.4181 | −0.1304 | 0.1197 | 0.073* | |
H7B | 0.2927 | −0.0775 | 0.1313 | 0.073* | |
H7C | 0.3827 | −0.1031 | 0.2027 | 0.073* | |
N8 | 0.6372 (7) | −0.0185 (5) | 0.1476 (6) | 0.051 (2) | |
H8A | 0.6216 | −0.0721 | 0.1898 | 0.077* | |
H8B | 0.6686 | 0.0230 | 0.1720 | 0.077* | |
H8C | 0.6964 | −0.0311 | 0.1056 | 0.077* | |
C1 | 0.0139 (8) | 0.3505 (6) | 0.3309 (6) | 0.0383 (19) | |
C2 | −0.0205 (10) | 0.3828 (7) | 0.2338 (7) | 0.051 (2) | |
H2 | −0.0395 | 0.3259 | 0.2162 | 0.061* | |
C3 | −0.1389 (12) | 0.4510 (9) | 0.2177 (8) | 0.083 (4) | |
H3D | −0.1191 | 0.5107 | 0.2266 | 0.124* | |
H3E | −0.2116 | 0.4256 | 0.2589 | 0.124* | |
H3F | −0.1624 | 0.4606 | 0.1573 | 0.124* | |
C4 | 0.0993 (12) | 0.4233 (10) | 0.1768 (8) | 0.093 (4) | |
H4D | 0.1294 | 0.4726 | 0.1991 | 0.139* | |
H4E | 0.0767 | 0.4495 | 0.1160 | 0.139* | |
H4F | 0.1685 | 0.3737 | 0.1790 | 0.139* | |
C5 | 0.3154 (8) | 0.3832 (6) | 0.4236 (6) | 0.0380 (19) | |
C6 | 0.4371 (8) | 0.4357 (6) | 0.3796 (6) | 0.042 (2) | |
H6 | 0.4208 | 0.5023 | 0.3817 | 0.050* | |
C7 | 0.5544 (10) | 0.3950 (8) | 0.4313 (8) | 0.074 (3) | |
H7D | 0.5792 | 0.3323 | 0.4242 | 0.110* | |
H7E | 0.5327 | 0.3912 | 0.4936 | 0.110* | |
H7F | 0.6270 | 0.4351 | 0.4093 | 0.110* | |
C8 | 0.4589 (12) | 0.4350 (10) | 0.2848 (8) | 0.093 (5) | |
H8D | 0.5379 | 0.4666 | 0.2589 | 0.140* | |
H8E | 0.3845 | 0.4676 | 0.2530 | 0.140* | |
H8F | 0.4684 | 0.3703 | 0.2806 | 0.140* | |
C9 | 0.2261 (9) | 0.1618 (6) | 0.0313 (6) | 0.043 (2) | |
C10 | 0.1209 (9) | 0.1938 (7) | −0.0352 (7) | 0.050 (2) | |
C11A | 0.119 (3) | 0.303 (2) | −0.082 (2) | 0.094 (6)* | 0.50 |
H11A | 0.0689 | 0.3166 | −0.1339 | 0.141* | 0.50 |
H11B | 0.2084 | 0.3207 | −0.1001 | 0.141* | 0.50 |
H11C | 0.0794 | 0.3376 | −0.0411 | 0.141* | 0.50 |
C11B | 0.073 (3) | 0.298 (2) | −0.041 (2) | 0.094 (6)* | 0.50 |
H11D | 0.0211 | 0.3224 | −0.0916 | 0.141* | 0.50 |
H11E | 0.1486 | 0.3354 | −0.0476 | 0.141* | 0.50 |
H11F | 0.0204 | 0.3011 | 0.0130 | 0.141* | 0.50 |
C12 | −0.0007 (13) | 0.1478 (11) | 0.0083 (10) | 0.107 (5) | |
H12A | 0.0149 | 0.0798 | 0.0211 | 0.160* | |
H12B | −0.0711 | 0.1681 | −0.0311 | 0.160* | |
H12C | −0.0250 | 0.1655 | 0.0631 | 0.160* | |
C13 | 0.5579 (9) | 0.2330 (7) | 0.0590 (6) | 0.047 (2) | |
C14 | 0.6404 (13) | 0.3114 (8) | 0.0047 (8) | 0.076 (4) | |
C15 | 0.7024 (16) | 0.3597 (10) | 0.0598 (10) | 0.122 (6) | |
H15A | 0.7600 | 0.4055 | 0.0221 | 0.183* | |
H15B | 0.7530 | 0.3138 | 0.1027 | 0.183* | |
H15C | 0.6351 | 0.3918 | 0.0907 | 0.183* | |
C16A | 0.661 (3) | 0.325 (2) | −0.070 (2) | 0.114 (8)* | 0.50 |
H16A | 0.5852 | 0.3586 | −0.0993 | 0.171* | 0.50 |
H16B | 0.6780 | 0.2649 | −0.0848 | 0.171* | 0.50 |
H16C | 0.7367 | 0.3620 | −0.0891 | 0.171* | 0.50 |
C16B | 0.540 (3) | 0.380 (2) | −0.057 (2) | 0.114 (8)* | 0.50 |
H16D | 0.5857 | 0.4108 | −0.1131 | 0.171* | 0.50 |
H16E | 0.5010 | 0.4272 | −0.0281 | 0.171* | 0.50 |
H16F | 0.4716 | 0.3439 | −0.0682 | 0.171* | 0.50 |
U11 | U22 | U33 | U12 | U13 | U23 | |
Pt1 | 0.03024 (17) | 0.02851 (16) | 0.0422 (2) | 0.00238 (12) | −0.00290 (13) | −0.01698 (14) |
Pt2 | 0.03077 (16) | 0.02392 (15) | 0.03383 (19) | −0.00107 (11) | 0.00238 (12) | −0.01001 (13) |
Pt3 | 0.03871 (19) | 0.03870 (19) | 0.03267 (19) | 0.00409 (13) | 0.00091 (13) | −0.01516 (15) |
Pt4 | 0.03641 (18) | 0.03552 (18) | 0.03400 (19) | 0.00310 (13) | −0.00032 (13) | −0.01376 (15) |
Cl1 | 0.0459 (13) | 0.0500 (13) | 0.0450 (14) | −0.0006 (10) | −0.0003 (10) | −0.0131 (11) |
Cl2 | 0.0381 (12) | 0.0408 (12) | 0.0532 (14) | 0.0000 (9) | −0.0028 (10) | −0.0138 (11) |
Cl3 | 0.0593 (15) | 0.0369 (12) | 0.0756 (19) | −0.0015 (10) | −0.0199 (13) | −0.0112 (12) |
Cl4 | 0.0455 (13) | 0.0652 (15) | 0.0456 (14) | −0.0080 (11) | 0.0014 (10) | −0.0210 (12) |
O1 | 0.051 (4) | 0.031 (3) | 0.043 (4) | 0.006 (3) | −0.011 (3) | −0.013 (3) |
O2 | 0.067 (4) | 0.024 (3) | 0.038 (4) | 0.004 (3) | −0.004 (3) | −0.010 (3) |
O3 | 0.030 (3) | 0.028 (3) | 0.064 (4) | −0.001 (2) | 0.003 (3) | −0.013 (3) |
O4 | 0.034 (3) | 0.032 (3) | 0.051 (4) | −0.004 (2) | 0.010 (3) | −0.014 (3) |
O5 | 0.062 (4) | 0.059 (4) | 0.035 (4) | 0.022 (3) | −0.011 (3) | −0.018 (3) |
O6 | 0.048 (4) | 0.053 (4) | 0.043 (4) | 0.009 (3) | −0.012 (3) | −0.019 (3) |
O7 | 0.064 (4) | 0.049 (4) | 0.044 (4) | −0.020 (3) | 0.012 (3) | −0.019 (3) |
O8 | 0.053 (4) | 0.039 (3) | 0.040 (4) | −0.004 (3) | 0.007 (3) | −0.013 (3) |
O9 | 0.119 (8) | 0.136 (8) | 0.053 (6) | 0.032 (6) | 0.030 (5) | −0.004 (6) |
O10 | 0.059 (5) | 0.097 (6) | 0.071 (6) | −0.013 (4) | −0.026 (4) | −0.003 (5) |
O11 | 0.050 (5) | 0.089 (6) | 0.142 (9) | −0.001 (4) | −0.028 (5) | −0.064 (6) |
O12 | 0.085 (6) | 0.055 (5) | 0.131 (9) | −0.003 (4) | 0.029 (6) | −0.036 (5) |
O13 | 0.073 (5) | 0.043 (4) | 0.083 (6) | 0.009 (3) | 0.013 (4) | −0.017 (4) |
O14 | 0.069 (5) | 0.051 (4) | 0.116 (7) | −0.014 (4) | −0.012 (5) | −0.031 (5) |
O15 | 0.045 (4) | 0.116 (7) | 0.076 (6) | −0.014 (4) | −0.016 (4) | −0.016 (5) |
O16 | 0.089 (6) | 0.080 (5) | 0.054 (5) | 0.003 (4) | 0.018 (4) | −0.019 (4) |
N1 | 0.035 (4) | 0.037 (4) | 0.080 (6) | −0.004 (3) | −0.002 (4) | −0.024 (4) |
N2 | 0.042 (4) | 0.034 (4) | 0.049 (5) | 0.004 (3) | −0.008 (3) | −0.017 (3) |
N3 | 0.047 (4) | 0.042 (4) | 0.045 (5) | −0.013 (3) | 0.007 (3) | −0.012 (4) |
N4 | 0.048 (4) | 0.036 (4) | 0.044 (5) | 0.003 (3) | −0.002 (3) | −0.004 (3) |
N5 | 0.037 (4) | 0.064 (5) | 0.043 (5) | −0.002 (4) | 0.011 (3) | −0.016 (4) |
N6 | 0.046 (4) | 0.050 (4) | 0.029 (4) | 0.001 (3) | 0.001 (3) | −0.009 (3) |
N7 | 0.051 (5) | 0.046 (4) | 0.045 (5) | 0.005 (3) | −0.005 (4) | −0.008 (4) |
N8 | 0.047 (5) | 0.048 (5) | 0.062 (6) | 0.015 (3) | −0.021 (4) | −0.020 (4) |
C1 | 0.043 (5) | 0.035 (5) | 0.040 (5) | −0.012 (4) | −0.003 (4) | −0.010 (4) |
C2 | 0.062 (6) | 0.054 (6) | 0.043 (6) | −0.005 (5) | −0.011 (5) | −0.021 (5) |
C3 | 0.083 (9) | 0.100 (9) | 0.056 (8) | 0.036 (7) | −0.025 (6) | −0.013 (7) |
C4 | 0.090 (10) | 0.127 (11) | 0.038 (7) | 0.001 (8) | 0.000 (6) | 0.014 (7) |
C5 | 0.033 (5) | 0.039 (5) | 0.042 (5) | −0.001 (3) | −0.002 (4) | −0.011 (4) |
C6 | 0.032 (5) | 0.033 (4) | 0.058 (6) | −0.006 (3) | 0.002 (4) | −0.006 (4) |
C7 | 0.047 (6) | 0.080 (8) | 0.079 (9) | −0.019 (5) | −0.015 (6) | 0.013 (7) |
C8 | 0.083 (9) | 0.143 (12) | 0.057 (8) | −0.069 (9) | 0.016 (7) | −0.021 (8) |
C9 | 0.053 (6) | 0.043 (5) | 0.030 (5) | 0.005 (4) | 0.001 (4) | −0.006 (4) |
C10 | 0.042 (5) | 0.060 (6) | 0.045 (6) | 0.014 (4) | −0.010 (4) | −0.010 (5) |
C12 | 0.087 (10) | 0.155 (14) | 0.080 (11) | −0.012 (10) | −0.041 (8) | −0.022 (10) |
C13 | 0.050 (6) | 0.049 (6) | 0.037 (5) | −0.012 (4) | 0.005 (4) | −0.004 (4) |
C14 | 0.111 (10) | 0.064 (7) | 0.056 (8) | −0.038 (7) | 0.024 (7) | −0.019 (6) |
C15 | 0.173 (16) | 0.112 (12) | 0.095 (12) | −0.079 (12) | −0.008 (11) | −0.027 (10) |
Pt1—Pt2 | 2.9881 (4) | N4—H4A | 0.8900 |
Pt1—Pt1i | 3.2619 (6) | N4—H4B | 0.8900 |
Pt3—Pt4 | 3.0246 (4) | N4—H4C | 0.8900 |
Pt4—Pt4ii | 3.3049 (6) | N5—H5A | 0.8900 |
Pt2—Pt3 | 4.5478 (5) | N5—H5B | 0.8900 |
Pt1—N1 | 2.037 (7) | N5—H5C | 0.8900 |
Pt1—N2 | 2.023 (7) | N6—H6A | 0.8900 |
Pt1—O1 | 2.034 (6) | N6—H6B | 0.8900 |
Pt1—O3 | 2.044 (5) | N6—H6C | 0.8900 |
Pt2—N3 | 2.016 (6) | N7—H7A | 0.8900 |
Pt2—N4 | 2.002 (7) | N7—H7B | 0.8900 |
Pt2—O2 | 2.031 (6) | N7—H7C | 0.8900 |
Pt2—O4 | 2.023 (5) | N8—H8A | 0.8900 |
Pt3—N5 | 2.017 (7) | N8—H8B | 0.8900 |
Pt3—N6 | 2.011 (7) | N8—H8C | 0.8900 |
Pt3—O5 | 2.035 (6) | C1—C2 | 1.517 (12) |
Pt3—O7 | 2.027 (6) | C2—C3 | 1.488 (13) |
Pt4—N7 | 2.020 (7) | C2—C4 | 1.502 (14) |
Pt4—N8 | 2.033 (7) | C2—H2 | 0.9800 |
Pt4—O6 | 2.055 (6) | C3—H3D | 0.9600 |
Pt4—O8 | 2.032 (6) | C3—H3E | 0.9600 |
Cl1—O9 | 1.410 (8) | C3—H3F | 0.9600 |
Cl1—O12 | 1.416 (7) | C4—H4D | 0.9600 |
Cl1—O10 | 1.421 (7) | C4—H4E | 0.9600 |
Cl1—O11 | 1.432 (7) | C4—H4F | 0.9600 |
Cl2—O15 | 1.411 (7) | C5—C6 | 1.518 (11) |
Cl2—O14 | 1.420 (7) | C6—C8 | 1.470 (14) |
Cl2—O16 | 1.424 (7) | C6—C7 | 1.489 (13) |
Cl2—O13 | 1.432 (6) | C6—H6 | 0.9800 |
Cl3—O17B | 1.404 (9) | C7—H7D | 0.9600 |
Cl3—O20A | 1.408 (8) | C7—H7E | 0.9600 |
Cl3—O19A | 1.421 (8) | C7—H7F | 0.9600 |
Cl3—O19B | 1.421 (9) | C8—H8D | 0.9600 |
Cl3—O20B | 1.422 (9) | C8—H8E | 0.9600 |
Cl3—O18A | 1.428 (8) | C8—H8F | 0.9600 |
Cl3—O17A | 1.437 (8) | C9—C10 | 1.513 (12) |
Cl3—O18B | 1.446 (9) | C10—C12 | 1.474 (16) |
Cl4—O23A | 1.408 (8) | C10—C11A | 1.56 (3) |
Cl4—O22A | 1.408 (8) | C10—C11B | 1.54 (3) |
Cl4—O22B | 1.418 (9) | C11A—H11A | 0.9600 |
Cl4—O23B | 1.424 (9) | C11A—H11B | 0.9600 |
Cl4—O24B | 1.427 (9) | C11A—H11C | 0.9600 |
Cl4—O21B | 1.432 (9) | C11B—H11D | 0.9600 |
Cl4—O24A | 1.444 (8) | C11B—H11E | 0.9600 |
Cl4—O21A | 1.472 (8) | C11B—H11F | 0.9600 |
O1—C1 | 1.265 (9) | C12—H12A | 0.9600 |
O2—C1 | 1.241 (10) | C12—H12B | 0.9600 |
O3—C5 | 1.290 (9) | C12—H12C | 0.9600 |
O4—C5 | 1.241 (9) | C13—C14 | 1.494 (13) |
O5—C9 | 1.251 (10) | C14—C15 | 1.459 (16) |
O6—C9 | 1.242 (10) | C14—C16A | 1.12 (3) |
O7—C13 | 1.263 (10) | C14—C16B | 1.57 (3) |
O8—C13 | 1.265 (10) | C15—H15A | 0.9600 |
N1—H1A | 0.8900 | C15—H15B | 0.9600 |
N1—H1B | 0.8900 | C15—H15C | 0.9600 |
N1—H1C | 0.8900 | C16A—H16A | 0.9600 |
N2—H2A | 0.8900 | C16A—H16B | 0.9600 |
N2—H2B | 0.8900 | C16A—H16C | 0.9600 |
N2—H2C | 0.8900 | C16B—H16D | 0.9600 |
N3—H3A | 0.8900 | C16B—H16E | 0.9600 |
N3—H3B | 0.8900 | C16B—H16F | 0.9600 |
N3—H3C | 0.8900 | ||
Pt2—Pt1—Pt1i | 161.515 (18) | H3A—N3—H3C | 109.5 |
Pt3—Pt4—Pt4ii | 155.255 (19) | H3B—N3—H3C | 109.5 |
N2—Pt1—O1 | 175.1 (2) | Pt2—N4—H4A | 109.5 |
N2—Pt1—N1 | 91.1 (3) | Pt2—N4—H4B | 109.5 |
O1—Pt1—N1 | 90.0 (3) | H4A—N4—H4B | 109.5 |
N2—Pt1—O3 | 89.2 (3) | Pt2—N4—H4C | 109.5 |
O1—Pt1—O3 | 89.3 (2) | H4A—N4—H4C | 109.5 |
N1—Pt1—O3 | 175.6 (2) | H4B—N4—H4C | 109.5 |
N2—Pt1—Pt2 | 103.81 (18) | Pt3—N5—H5A | 109.5 |
O1—Pt1—Pt2 | 80.52 (15) | Pt3—N5—H5B | 109.5 |
N1—Pt1—Pt2 | 104.57 (19) | H5A—N5—H5B | 109.5 |
O3—Pt1—Pt2 | 79.64 (14) | Pt3—N5—H5C | 109.5 |
N2—Pt1—Pt1i | 85.16 (18) | H5A—N5—H5C | 109.5 |
O1—Pt1—Pt1i | 90.03 (15) | H5B—N5—H5C | 109.5 |
N1—Pt1—Pt1i | 91.18 (19) | Pt3—N6—H6A | 109.5 |
O3—Pt1—Pt1i | 84.42 (14) | Pt3—N6—H6B | 109.5 |
N4—Pt2—N3 | 89.8 (3) | H6A—N6—H6B | 109.5 |
N4—Pt2—O4 | 89.1 (3) | Pt3—N6—H6C | 109.5 |
N3—Pt2—O4 | 174.8 (2) | H6A—N6—H6C | 109.5 |
N4—Pt2—O2 | 173.4 (2) | H6B—N6—H6C | 109.5 |
N3—Pt2—O2 | 90.5 (3) | Pt4—N7—H7A | 109.5 |
O4—Pt2—O2 | 90.0 (2) | Pt4—N7—H7B | 109.5 |
N4—Pt2—Pt1 | 108.4 (2) | H7A—N7—H7B | 109.5 |
N3—Pt2—Pt1 | 105.3 (2) | Pt4—N7—H7C | 109.5 |
O4—Pt2—Pt1 | 79.79 (14) | H7A—N7—H7C | 109.5 |
O2—Pt2—Pt1 | 77.82 (14) | H7B—N7—H7C | 109.5 |
N4—Pt2—Pt3 | 114.6 (2) | Pt4—N8—H8A | 109.5 |
N3—Pt2—Pt3 | 104.5 (2) | Pt4—N8—H8B | 109.5 |
O4—Pt2—Pt3 | 71.47 (16) | H8A—N8—H8B | 109.5 |
O2—Pt2—Pt3 | 59.04 (16) | Pt4—N8—H8C | 109.5 |
Pt1—Pt2—Pt3 | 126.901 (12) | H8A—N8—H8C | 109.5 |
N6—Pt3—N5 | 91.4 (3) | H8B—N8—H8C | 109.5 |
N6—Pt3—O7 | 88.9 (3) | O2—C1—O1 | 125.3 (8) |
N5—Pt3—O7 | 175.7 (3) | O2—C1—C2 | 116.3 (8) |
N6—Pt3—O5 | 174.3 (3) | O1—C1—C2 | 118.3 (8) |
N5—Pt3—O5 | 87.8 (3) | C3—C2—C4 | 111.4 (10) |
O7—Pt3—O5 | 91.5 (3) | C3—C2—C1 | 114.3 (9) |
N6—Pt3—Pt4 | 108.14 (19) | C4—C2—C1 | 108.5 (8) |
N5—Pt3—Pt4 | 105.3 (2) | C3—C2—H2 | 107.5 |
O7—Pt3—Pt4 | 78.73 (16) | C4—C2—H2 | 107.5 |
O5—Pt3—Pt4 | 77.52 (16) | C1—C2—H2 | 107.5 |
N6—Pt3—Pt2 | 53.38 (19) | C2—C3—H3D | 109.5 |
N5—Pt3—Pt2 | 55.0 (2) | C2—C3—H3E | 109.5 |
O7—Pt3—Pt2 | 122.30 (17) | H3D—C3—H3E | 109.5 |
O5—Pt3—Pt2 | 122.07 (17) | C2—C3—H3F | 109.5 |
Pt4—Pt3—Pt2 | 147.371 (13) | H3D—C3—H3F | 109.5 |
N7—Pt4—O8 | 176.0 (3) | H3E—C3—H3F | 109.5 |
N7—Pt4—N8 | 91.5 (3) | C2—C4—H4D | 109.5 |
O8—Pt4—N8 | 88.1 (3) | C2—C4—H4E | 109.5 |
N7—Pt4—O6 | 88.8 (3) | H4D—C4—H4E | 109.5 |
O8—Pt4—O6 | 91.2 (3) | C2—C4—H4F | 109.5 |
N8—Pt4—O6 | 174.5 (3) | H4D—C4—H4F | 109.5 |
N7—Pt4—Pt3 | 105.4 (2) | H4E—C4—H4F | 109.5 |
O8—Pt4—Pt3 | 78.47 (15) | O4—C5—O3 | 126.8 (7) |
N8—Pt4—Pt3 | 106.4 (2) | O4—C5—C6 | 117.1 (7) |
O6—Pt4—Pt3 | 78.81 (16) | O3—C5—C6 | 116.1 (7) |
N7—Pt4—Pt4ii | 85.8 (2) | C8—C6—C7 | 112.5 (9) |
O8—Pt4—Pt4ii | 90.33 (16) | C8—C6—C5 | 111.0 (8) |
N8—Pt4—Pt4ii | 95.1 (2) | C7—C6—C5 | 110.0 (8) |
O6—Pt4—Pt4ii | 79.45 (16) | C8—C6—H6 | 107.7 |
O9—Cl1—O12 | 110.2 (5) | C7—C6—H6 | 107.7 |
O9—Cl1—O10 | 106.8 (5) | C5—C6—H6 | 107.7 |
O12—Cl1—O10 | 112.2 (5) | C6—C7—H7D | 109.5 |
O9—Cl1—O11 | 111.3 (6) | C6—C7—H7E | 109.5 |
O12—Cl1—O11 | 108.4 (5) | H7D—C7—H7E | 109.5 |
O10—Cl1—O11 | 108.0 (5) | C6—C7—H7F | 109.5 |
O15—Cl2—O14 | 109.5 (5) | H7D—C7—H7F | 109.5 |
O15—Cl2—O16 | 109.7 (5) | H7E—C7—H7F | 109.5 |
O14—Cl2—O16 | 111.8 (5) | C6—C8—H8D | 109.5 |
O15—Cl2—O13 | 109.3 (5) | C6—C8—H8E | 109.5 |
O14—Cl2—O13 | 108.0 (4) | H8D—C8—H8E | 109.5 |
O16—Cl2—O13 | 108.5 (5) | C6—C8—H8F | 109.5 |
O20A—Cl3—O19A | 111.2 (6) | H8D—C8—H8F | 109.5 |
O17B—Cl3—O19B | 110.3 (7) | H8E—C8—H8F | 109.5 |
O17B—Cl3—O20B | 110.0 (11) | O6—C9—O5 | 125.8 (9) |
O19B—Cl3—O20B | 114.7 (11) | O6—C9—C10 | 115.6 (8) |
O20A—Cl3—O18A | 109.6 (6) | O5—C9—C10 | 118.6 (8) |
O19A—Cl3—O18A | 109.3 (6) | C12—C10—C9 | 106.8 (9) |
O20A—Cl3—O17A | 109.5 (6) | C12—C10—C11B | 98.7 (14) |
O19A—Cl3—O17A | 109.0 (6) | C9—C10—C11B | 109.5 (14) |
O18A—Cl3—O17A | 108.3 (6) | C12—C10—C11A | 121.5 (14) |
O17B—Cl3—O18B | 109.2 (7) | C9—C10—C11A | 112.5 (14) |
O19B—Cl3—O18B | 106.7 (7) | C10—C11A—H11A | 109.5 |
O20B—Cl3—O18B | 105.6 (11) | C10—C11A—H11B | 109.5 |
O23A—Cl4—O22A | 113.6 (6) | C10—C11A—H11C | 109.5 |
O22B—Cl4—O23B | 104.0 (12) | C10—C11B—H11D | 109.5 |
O22B—Cl4—O24B | 105.6 (11) | C10—C11B—H11E | 109.5 |
O23B—Cl4—O24B | 114.8 (12) | H11D—C11B—H11E | 109.5 |
O22B—Cl4—O21B | 109.1 (12) | C10—C11B—H11F | 109.5 |
O23B—Cl4—O21B | 111.8 (12) | H11D—C11B—H11F | 109.5 |
O24B—Cl4—O21B | 111.0 (12) | H11E—C11B—H11F | 109.5 |
O23A—Cl4—O24A | 110.6 (6) | C10—C12—H12A | 109.5 |
O22A—Cl4—O24A | 109.4 (6) | C10—C12—H12B | 109.5 |
O23A—Cl4—O21A | 107.6 (6) | H12A—C12—H12B | 109.5 |
O22A—Cl4—O21A | 108.7 (6) | C10—C12—H12C | 109.5 |
O24A—Cl4—O21A | 106.6 (6) | H12A—C12—H12C | 109.5 |
C1—O1—Pt1 | 125.9 (6) | H12B—C12—H12C | 109.5 |
C1—O2—Pt2 | 130.0 (5) | O7—C13—O8 | 126.6 (8) |
C5—O3—Pt1 | 125.8 (5) | O7—C13—C14 | 116.6 (9) |
C5—O4—Pt2 | 127.8 (5) | O8—C13—C14 | 116.8 (8) |
C9—O5—Pt3 | 128.6 (6) | C16A—C14—C15 | 124 (2) |
C9—O6—Pt4 | 126.4 (6) | C16A—C14—C13 | 122 (2) |
C13—O7—Pt3 | 126.0 (6) | C15—C14—C13 | 112.9 (11) |
C13—O8—Pt4 | 126.9 (5) | C15—C14—C16B | 112.0 (15) |
Pt1—N1—H1A | 109.5 | C13—C14—C16B | 103.6 (15) |
Pt1—N1—H1B | 109.5 | C14—C15—H15A | 109.5 |
H1A—N1—H1B | 109.5 | C14—C15—H15B | 109.5 |
Pt1—N1—H1C | 109.5 | H15A—C15—H15B | 109.5 |
H1A—N1—H1C | 109.5 | C14—C15—H15C | 109.5 |
H1B—N1—H1C | 109.5 | H15A—C15—H15C | 109.5 |
Pt1—N2—H2A | 109.5 | H15B—C15—H15C | 109.5 |
Pt1—N2—H2B | 109.5 | C14—C16A—H16A | 109.5 |
H2A—N2—H2B | 109.5 | C14—C16A—H16B | 109.5 |
Pt1—N2—H2C | 109.5 | C14—C16A—H16C | 109.5 |
H2A—N2—H2C | 109.5 | C14—C16B—H16D | 109.5 |
H2B—N2—H2C | 109.5 | C14—C16B—H16E | 109.5 |
Pt2—N3—H3A | 109.5 | H16D—C16B—H16E | 109.5 |
Pt2—N3—H3B | 109.5 | C14—C16B—H16F | 109.5 |
H3A—N3—H3B | 109.5 | H16D—C16B—H16F | 109.5 |
Pt2—N3—H3C | 109.5 | H16E—C16B—H16F | 109.5 |
N2—Pt1—Pt2—N4 | −2.2 (3) | O1—C1—C2—C4 | 95.7 (10) |
N1—Pt1—Pt2—N3 | −2.1 (3) | O4—C5—C6—C8 | 59.4 (12) |
O3—Pt1—Pt2—O4 | −1.2 (3) | O3—C5—C6—C8 | −119.1 (10) |
O1—Pt1—Pt2—O2 | −2.5 (2) | O4—C5—C6—C7 | −65.8 (11) |
N5—Pt3—Pt4—N7 | −12.4 (3) | O3—C5—C6—C7 | 115.8 (9) |
O7—Pt3—Pt4—O8 | −11.4 (3) | O6—C9—C10—C12 | 94.8 (11) |
N6—Pt3—Pt4—N8 | −12.0 (3) | O5—C9—C10—C12 | −86.4 (12) |
O5—Pt3—Pt4—O6 | −10.9 (3) | O6—C9—C10—C11B | −159.2 (14) |
O2—C1—C2—C3 | 153.2 (9) | O5—C9—C10—C11B | 19.6 (17) |
O1—C1—C2—C3 | −29.3 (12) | O6—C9—C10—C11A | −129.5 (14) |
O2—C1—C2—C4 | −81.8 (11) | O5—C9—C10—C11A | 49.4 (16) |
Symmetry codes: (i) −x, −y+1, −z+1; (ii) −x+1, −y, −z. |
D—H···A | D—H | H···A | D···A | D—H···A |
N1—H1B···O21A | 0.89 | 2.36 | 3.222 (17) | 162 |
N1—H1B···O24B | 0.89 | 2.60 | 3.117 (19) | 118 |
N2—H2A···O18B | 0.89 | 2.22 | 3.065 (17) | 159 |
N2—H2A···O20A | 0.89 | 2.37 | 3.135 (18) | 144 |
N2—H2B···O21A | 0.89 | 2.29 | 3.135 (18) | 158 |
N3—H3C···O13 | 0.89 | 2.47 | 3.128 (9) | 131 |
N3—H3B···O24A | 0.89 | 2.13 | 2.970 (16) | 157 |
N3—H3B···O24B | 0.89 | 1.92 | 2.768 (16) | 159 |
N4—H4A···O18A | 0.89 | 2.11 | 2.716 (11) | 125 |
N4—H4C···O23A | 0.89 | 2.07 | 2.963 (16) | 176 |
N5—H5A···O2 | 0.89 | 2.71 | 3.110 (8) | 108 |
N5—H5B···O13 | 0.89 | 2.31 | 3.057 (11) | 141 |
N6—H6C···O4 | 0.89 | 2.38 | 3.248 (8) | 165 |
N6—H6A···O11 | 0.89 | 2.36 | 2.943 (10) | 123 |
N6—H6A···O12 | 0.89 | 2.50 | 3.348 (11) | 160 |
N6—H6B···O16 | 0.89 | 2.41 | 3.231 (10) | 154 |
N8—H8B···O11 | 0.89 | 2.16 | 2.963 (11) | 149 |
N1—H1C···O14iii | 0.89 | 2.21 | 3.005 (9) | 149 |
N1—H1A···O3i | 0.89 | 2.34 | 3.105 (8) | 144 |
N2—H2C···O1i | 0.89 | 2.28 | 3.093 (8) | 152 |
N3—H3C···O10iv | 0.89 | 2.29 | 3.041 (11) | 142 |
N3—H3A···O10v | 0.89 | 2.16 | 2.998 (11) | 157 |
N4—H4B···O11iv | 0.89 | 2.59 | 3.151 (11) | 122 |
N4—H4A···O15iv | 0.89 | 2.48 | 3.013 (10) | 119 |
N5—H5C···O22Biii | 0.89 | 2.30 | 3.133 (19) | 156 |
N5—H5C···O24Aiii | 0.89 | 2.40 | 3.172 (16) | 145 |
N5—H5A···O9v | 0.89 | 2.44 | 3.213 (13) | 146 |
N7—H7B···O22Aiii | 0.89 | 2.34 | 3.185 (17) | 160 |
N7—H7B···O22Biii | 0.89 | 2.16 | 2.91 (2) | 142 |
N7—H7A···O8ii | 0.89 | 2.47 | 3.167 (9) | 135 |
N7—H7A···O19Aiv | 0.89 | 2.39 | 2.938 (15) | 120 |
N8—H8C···O6ii | 0.89 | 2.39 | 3.109 (9) | 138 |
N8—H8A···O19Aiv | 0.89 | 2.44 | 3.155 (14) | 138 |
N8—H8A···O19Biv | 0.89 | 1.92 | 2.759 (12) | 156 |
Symmetry codes: (i) −x, −y+1, −z+1; (ii) −x+1, −y, −z; (iii) −x, −y, −z+1; (iv) −x+1, −y, −z+1; (v) x−1, y, z. |