Supporting information
Crystallographic Information File (CIF) https://doi.org/10.1107/S1600536804006877/hb6028sup1.cif | |
Structure factor file (CIF format) https://doi.org/10.1107/S1600536804006877/hb6028Isup2.hkl |
CCDC reference: 238674
Key indicators
- Single-crystal X-ray study
- T = 296 K
- Mean (C-C) = 0.019 Å
- H-atom completeness 87%
- Disorder in solvent or counterion
- R factor = 0.051
- wR factor = 0.135
- Data-to-parameter ratio = 16.9
checkCIF/PLATON results
No syntax errors found
Alert level A PLAT430_ALERT_2_A Short Inter D...A Contact O9 .. O12A .. 2.22 Ang. PLAT430_ALERT_2_A Short Inter D...A Contact O9 .. O12B .. 2.45 Ang. PLAT430_ALERT_2_A Short Inter D...A Contact O10 .. O11A .. 2.32 Ang. PLAT430_ALERT_2_A Short Inter D...A Contact O10 .. O13A .. 2.41 Ang. PLAT430_ALERT_2_A Short Inter D...A Contact O11B .. O13A .. 2.40 Ang.
Alert level B PLAT430_ALERT_2_B Short Inter D...A Contact O3A .. O8A .. 2.75 Ang. PLAT430_ALERT_2_B Short Inter D...A Contact O3A .. O9 .. 2.76 Ang. PLAT430_ALERT_2_B Short Inter D...A Contact O3B .. O8A .. 2.64 Ang. PLAT430_ALERT_2_B Short Inter D...A Contact O5A .. O9 .. 2.65 Ang. PLAT430_ALERT_2_B Short Inter D...A Contact O9 .. O11B .. 2.66 Ang. PLAT432_ALERT_2_B Short Inter X...Y Contact O10 .. N10A .. 2.73 Ang. PLAT432_ALERT_2_B Short Inter X...Y Contact O11A .. C14 .. 2.79 Ang.
Alert level C PLAT041_ALERT_1_C Calc. and Rep. SumFormula Strings Differ .... ? PLAT042_ALERT_1_C Calc. and Rep. MoietyFormula Strings Differ .... ? PLAT045_ALERT_1_C Calculated and Reported Z Differ by ............ 0.25 Ratio PLAT068_ALERT_1_C Reported F000 Differs from Calcd (or Missing)... ? PLAT094_ALERT_2_C Ratio of Maximum / Minimum Residual Density .... 2.78 PLAT241_ALERT_2_C Check High U(eq) as Compared to Neighbors .... N4 PLAT241_ALERT_2_C Check High U(eq) as Compared to Neighbors .... C8 PLAT241_ALERT_2_C Check High U(eq) as Compared to Neighbors .... C17 PLAT302_ALERT_4_C Anion/Solvent Disorder ......................... 50.00 Perc. PLAT313_ALERT_2_C Oxygen with three covalent bonds (rare) ........ O3B PLAT342_ALERT_3_C Low Bond Precision on C-C bonds (x 1000) Ang ... 19 PLAT368_ALERT_2_C Short C(sp2)-C(sp2) Bond C13 - C14 ... 1.22 Ang. PLAT432_ALERT_2_C Short Inter X...Y Contact O5A .. C26 .. 3.01 Ang. PLAT790_ALERT_4_C Centre of Gravity not Within Unit Cell: Resd. # 2 N2 O6 PLAT790_ALERT_4_C Centre of Gravity not Within Unit Cell: Resd. # 3 N2 O6 PLAT790_ALERT_4_C Centre of Gravity not Within Unit Cell: Resd. # 4 N2 O6 PLAT790_ALERT_4_C Centre of Gravity not Within Unit Cell: Resd. # 5 O2 PLAT790_ALERT_4_C Centre of Gravity not Within Unit Cell: Resd. # 6 O2 PLAT790_ALERT_4_C Centre of Gravity not Within Unit Cell: Resd. # 7 O2
Alert level G FORMU01_ALERT_2_G There is a discrepancy between the atom counts in the _chemical_formula_sum and the formula from the _atom_site* data. Atom count from _chemical_formula_sum:C30 H30 N10 O8 Pt2 Atom count from the _atom_site data: C30 H26 N10 O8 Pt2 CELLZ01_ALERT_1_G Difference between formula and atom_site contents detected. CELLZ01_ALERT_1_G WARNING: H atoms missing from atom site list. Is this intentional? From the CIF: _cell_formula_units_Z 4 From the CIF: _chemical_formula_sum C30 H30 N10 O8 Pt2 TEST: Compare cell contents of formula and atom_site data atom Z*formula cif sites diff C 120.00 120.00 0.00 H 120.00 104.00 16.00 N 40.00 40.00 0.00 O 32.00 32.00 0.00 Pt 8.00 8.00 0.00
5 ALERT level A = In general: serious problem 7 ALERT level B = Potentially serious problem 19 ALERT level C = Check and explain 3 ALERT level G = General alerts; check 6 ALERT type 1 CIF construction/syntax error, inconsistent or missing data 20 ALERT type 2 Indicator that the structure model may be wrong or deficient 1 ALERT type 3 Indicator that the structure quality may be low 7 ALERT type 4 Improvement, methodology, query or suggestion
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(C10H8N2)2(C5H5N2)2](NO3)2·4H2O | F(000) = 2000 |
Mr = 1048.82 | Dx = 1.977 Mg m−3 |
Monoclinic, P21/n | Mo Kα radiation, λ = 0.71073 Å |
Hall symbol: -P 2yn | Cell parameters from 5776 reflections |
a = 14.1356 (8) Å | θ = 2.3–20.2° |
b = 16.0180 (9) Å | µ = 7.99 mm−1 |
c = 16.4055 (9) Å | T = 296 K |
β = 108.411 (1)° | Needle, red |
V = 3524.5 (3) Å3 | 0.23 × 0.07 × 0.04 mm |
Z = 4 |
Bruker SMART APEX CCD-detector diffractometer | 7197 independent reflections |
Radiation source: fine-focus sealed tube | 4146 reflections with I > 2σ(I) |
Graphite monochromator | Rint = 0.095 |
Detector resolution: 8.366 pixels mm-1 | θmax = 26.4°, θmin = 2.1° |
ω scans | h = −17→17 |
Absorption correction: gaussian (XPREP in SAINT; Bruker, 2001) | k = −20→20 |
Tmin = 0.298, Tmax = 0.735 | l = −20→20 |
40126 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)] = 0.051 | Hydrogen site location: inferred from neighbouring sites |
wR(F2) = 0.135 | H-atom parameters constrained |
S = 0.90 | w = 1/[σ2(Fo2) + (0.0718P)2] where P = (Fo2 + 2Fc2)/3 |
7197 reflections | (Δ/σ)max = 0.001 |
427 parameters | Δρmax = 2.02 e Å−3 |
28 restraints | Δρmin = −0.73 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) 14.0738 (0.0025) x + 0.7255 (0.0456) y - 3.8878 (0.0434) z = 13.0788 (0.0469) * -0.0197 (0.0081) N1 * -0.0053 (0.0082) N2 * 0.0160 (0.0102) C1 * 0.0097 (0.0117) C2 * 0.0109 (0.0120) C3 * -0.0136 (0.0122) C4 * 0.0046 (0.0101) C5 * -0.0163 (0.0102) C6 * -0.0145 (0.0113) C7 * 0.0060 (0.0119) C8 * 0.0332 (0.0128) C9 * -0.0108 (0.0096) C10 - 3.4871 (0.0098) N5 - 3.4061 (0.0105) N6 - 3.5185 (0.0137) C16 - 3.6638 (0.0147) C17 - 3.8164 (0.0151) C18 - 3.8091 (0.0132) C19 - 3.6357 (0.0100) C20 - 3.6220 (0.0113) C21 - 3.7426 (0.0129) C22 - 3.6904 (0.0152) C23 - 3.4892 (0.0134) C24 - 3.3722 (0.0138) C25 Rms deviation of fitted atoms = 0.0153 13.9748 (0.0052) x + 2.4064 (0.0367) y - 5.2384 (0.0430) z = 11.1204 (0.0338) Angle to previous plane (with approximate e.s.d.) = 7.90 (0.09) * -0.0040 (0.0082) N5 * 0.0129 (0.0081) N6 * -0.0161 (0.0097) C16 * 0.0142 (0.0115) C17 * 0.0155 (0.0113) C18 * -0.0041 (0.0108) C19 * -0.0014 (0.0094) C20 * -0.0222 (0.0101) C21 * -0.0102 (0.0102) C22 * -0.0018 (0.0110) C23 * 0.0147 (0.0102) C24 * 0.0025 (0.0093) C25 3.4415 (0.0107) N1 3.4332 (0.0099) N2 3.4817 (0.0147) C1 3.6277 (0.0150) C2 3.7935 (0.0153) C3 3.7733 (0.0151) C4 3.6286 (0.0112) C5 3.5961 (0.0109) C6 3.7447 (0.0133) C7 3.7314 (0.0152) C8 3.5897 (0.0160) C9 3.4046 (0.0125) C10 Rms deviation of fitted atoms = 0.0120 13.9748 (0.0052) x + 2.4064 (0.0367) y - 5.2384 (0.0430) z = 11.1204 (0.0338) Angle to previous plane (with approximate e.s.d.) = 0.00 (0.10) * -0.0040 (0.0082) N5 * 0.0129 (0.0081) N6 * -0.0161 (0.0097) C16 * 0.0142 (0.0115) C17 * 0.0155 (0.0113) C18 * -0.0041 (0.0108) C19 * -0.0014 (0.0094) C20 * -0.0222 (0.0101) C21 * -0.0102 (0.0102) C22 * -0.0018 (0.0110) C23 * 0.0147 (0.0102) C24 * 0.0025 (0.0093) C25 - 3.4492 (0.0095) N5_$11 - 3.4661 (0.0097) N6_$11 - 3.4371 (0.0123) C16_$11 - 3.4674 (0.0138) C17_$11 - 3.4687 (0.0130) C18_$11 - 3.4491 (0.0123) C19_$11 - 3.4518 (0.0108) C20_$11 - 3.4310 (0.0117) C21_$11 - 3.4429 (0.0118) C22_$11 - 3.4514 (0.0132) C23_$11 - 3.4679 (0.0123) C24_$11 - 3.4557 (0.0117) C25_$11 Rms deviation of fitted atoms = 0.0120 13.9748 (0.0052) x + 2.4064 (0.0367) y - 5.2384 (0.0429) z = 7.6672 (0.0347) Angle to previous plane (with approximate e.s.d.) = 0.00 (0.10) * 0.0040 (0.0082) N5_$11 * -0.0129 (0.0081) N6_$11 * 0.0161 (0.0097) C16_$11 * -0.0142 (0.0115) C17_$11 * -0.0155 (0.0113) C18_$11 * 0.0041 (0.0108) C19_$11 * 0.0014 (0.0094) C20_$11 * 0.0222 (0.0101) C21_$11 * 0.0102 (0.0102) C22_$11 * 0.0018 (0.0110) C23_$11 * -0.0147 (0.0102) C24_$11 * -0.0025 (0.0093) C25_$11 3.4492 (0.0095) N5 3.4661 (0.0098) N6 3.4371 (0.0123) C16 3.4674 (0.0138) C17 3.4687 (0.0130) C18 3.4491 (0.0123) C19 3.4518 (0.0108) C20 3.4310 (0.0117) C21 3.4429 (0.0119) C22 3.4514 (0.0132) C23 3.4679 (0.0124) C24 3.4557 (0.0117) C25 Rms deviation of fitted atoms = 0.0120 14.0738 (0.0025) x + 0.7255 (0.0456) y - 3.8878 (0.0434) z = 13.0788 (0.0469) Angle to previous plane (with approximate e.s.d.) = 7.90 (0.09) * -0.0197 (0.0081) N1 * -0.0053 (0.0082) N2 * 0.0160 (0.0102) C1 * 0.0097 (0.0117) C2 * 0.0109 (0.0120) C3 * -0.0136 (0.0122) C4 * 0.0046 (0.0101) C5 * -0.0163 (0.0102) C6 * -0.0145 (0.0113) C7 * 0.0060 (0.0119) C8 * 0.0332 (0.0128) C9 * -0.0108 (0.0096) C10 3.4608 (0.0096) N1_$12 3.4464 (0.0095) N2_$12 3.4251 (0.0128) C1_$12 3.4314 (0.0139) C2_$12 3.4302 (0.0139) C3_$12 3.4547 (0.0140) C4_$12 3.4364 (0.0117) C5_$12 3.4574 (0.0119) C6_$12 3.4555 (0.0127) C7_$12 3.4351 (0.0135) C8_$12 3.4079 (0.0155) C9_$12 3.4519 (0.0119) C10_$12 Rms deviation of fitted atoms = 0.0153 14.0738 (0.0025) x + 0.7255 (0.0456) y - 3.8878 (0.0433) z = 16.5199 (0.0452) Angle to previous plane (with approximate e.s.d.) = 0.00 (0.06) * 0.0197 (0.0081) N1_$12 * 0.0053 (0.0082) N2_$12 * -0.0160 (0.0102) C1_$12 * -0.0097 (0.0117) C2_$12 * -0.0109 (0.0120) C3_$12 * 0.0136 (0.0122) C4_$12 * -0.0046 (0.0101) C5_$12 * 0.0164 (0.0102) C6_$12 * 0.0145 (0.0113) C7_$12 * -0.0060 (0.0119) C8_$12 * -0.0332 (0.0129) C9_$12 * 0.0108 (0.0096) C10_$12 - 3.4608 (0.0096) N1 - 3.4464 (0.0095) N2 - 3.4251 (0.0127) C1 - 3.4314 (0.0139) C2 - 3.4302 (0.0138) C3 - 3.4547 (0.0140) C4 - 3.4364 (0.0117) C5 - 3.4574 (0.0119) C6 - 3.4555 (0.0127) C7 - 3.4351 (0.0135) C8 - 3.4079 (0.0156) C9 - 3.4519 (0.0119) C10 Rms deviation of fitted atoms = 0.0153 -0.8531 (0.0489) x + 15.9754 (0.0048) y + 0.9496 (0.0628) z = 13.9365 (0.0387) Angle to previous plane (with approximate e.s.d.) = 89.34 (0.26) * -0.0087 (0.0070) N3 * 0.0242 (0.0058) N7 * -0.0081 (0.0076) C11 * 0.0246 (0.0093) C12 * -0.0003 (0.0087) C13 * -0.0170 (0.0080) C14 * -0.0147 (0.0079) C15 Rms deviation of fitted atoms = 0.0162 0.4992 (0.0498) x + 0.4395 (0.0600) y + 15.3672 (0.0197) z = 2.5403 (0.0443) Angle to previous plane (with approximate e.s.d.) = 86.21 (0.32) * 0.0080 (0.0061) N4 * -0.0346 (0.0074) N8 * 0.0109 (0.0078) C26 * 0.0223 (0.0092) C27 * -0.0258 (0.0086) C28 * 0.0038 (0.0084) C29 * 0.0155 (0.0089) C30 Rms deviation of fitted atoms = 0.0200 13.8619 (0.0092) x - 0.7758 (0.0524) y - 2.1273 (0.0554) z = 11.4958 (0.0508) Angle to previous plane (with approximate e.s.d.) = 77.12 (0.29) * 0.0119 (0.0049) N1 * -0.0122 (0.0051) N2 * -0.0109 (0.0045) N3 * 0.0112 (0.0047) N4 0.0014 (0.0048) Pt1 - 2.8093 (0.0056) Pt2 Rms deviation of fitted atoms = 0.0116 13.7351 (0.0108) x + 3.5629 (0.0525) y - 6.2784 (0.0509) z = 12.0386 (0.0422) Angle to previous plane (with approximate e.s.d.) = 22.04 (0.15) * 0.0063 (0.0047) N5 * -0.0062 (0.0047) N6 * -0.0059 (0.0044) N7 * 0.0058 (0.0044) N8 2.8071 (0.0052) Pt1 - 0.0125 (0.0045) Pt2 Rms deviation of fitted atoms = 0.0061 |
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 | 0.89884 (3) | 0.91251 (3) | 0.11964 (3) | 0.06841 (17) | |
Pt2 | 0.69224 (3) | 0.88877 (2) | 0.10329 (3) | 0.06378 (16) | |
O3A | 0.707 (2) | 1.295 (2) | −0.116 (2) | 0.248 (6)* | 0.50 |
O3B | 0.708 (3) | 1.331 (2) | −0.1574 (18) | 0.248 (6)* | 0.50 |
O4A | 0.631 (3) | 1.4054 (16) | −0.104 (2) | 0.248 (6)* | 0.50 |
O4B | 0.5744 (19) | 1.335 (2) | −0.124 (3) | 0.248 (6)* | 0.50 |
O5A | 0.552 (2) | 1.293 (2) | −0.138 (3) | 0.248 (6)* | 0.50 |
O5B | 0.714 (2) | 1.361 (2) | −0.0307 (16) | 0.248 (6)* | 0.50 |
O8A | 0.8875 (19) | 1.2732 (16) | −0.1439 (16) | 0.154 (8)* | 0.50 |
O8B | 0.9337 (14) | 1.3199 (12) | −0.1002 (12) | 0.109 (6)* | 0.50 |
O9 | 0.604 (2) | 1.168 (2) | −0.221 (2) | 0.217 (12)* | 0.50 |
O10 | 0.340 (2) | 1.037 (2) | −0.506 (2) | 0.235 (13)* | 0.50 |
O11A | 0.3295 (17) | 1.093 (2) | −0.379 (2) | 0.257 (6)* | 0.50 |
O11B | 0.6152 (16) | 1.131 (2) | −0.376 (2) | 0.257 (6)* | 0.50 |
O12A | 0.450 (2) | 1.117 (2) | −0.2692 (16) | 0.257 (6)* | 0.50 |
O12B | 0.743 (2) | 1.173 (2) | −0.2802 (16) | 0.257 (6)* | 0.50 |
O13A | 0.472 (2) | 1.053 (2) | −0.372 (2) | 0.257 (6)* | 0.50 |
O13B | 0.751 (2) | 1.138 (2) | −0.4004 (18) | 0.257 (6)* | 0.50 |
N1 | 0.9057 (6) | 1.0387 (5) | 0.1136 (6) | 0.067 (2) | |
N2 | 0.8793 (6) | 0.9269 (6) | −0.0068 (6) | 0.072 (2) | |
N3 | 0.9173 (8) | 0.9061 (5) | 0.2481 (6) | 0.073 (3) | |
N4 | 0.8918 (8) | 0.7878 (5) | 0.1143 (6) | 0.092 (3) | |
H4 | 0.9434 | 0.7634 | 0.1084 | 0.110* | |
N5 | 0.6514 (6) | 1.0093 (5) | 0.0795 (6) | 0.072 (2) | |
N6 | 0.6344 (6) | 0.8852 (5) | −0.0263 (5) | 0.063 (2) | |
N7 | 0.7477 (8) | 0.9001 (5) | 0.2300 (6) | 0.076 (3) | |
H7 | 0.7038 | 0.9064 | 0.2558 | 0.091* | |
N8 | 0.7316 (7) | 0.7671 (5) | 0.1174 (5) | 0.070 (2) | |
N9A | 0.6292 (18) | 1.3310 (17) | −0.1194 (13) | 0.248 (6)* | 0.50 |
N9B | 0.6646 (18) | 1.3421 (12) | −0.1040 (17) | 0.248 (6)* | 0.50 |
N10A | 0.4166 (17) | 1.0880 (10) | −0.3390 (15) | 0.257 (6)* | 0.50 |
N10B | 0.7031 (16) | 1.1473 (11) | −0.3520 (14) | 0.257 (6)* | 0.50 |
C1 | 0.9229 (9) | 1.0929 (7) | 0.1765 (8) | 0.084 (4) | |
H1 | 0.9416 | 1.0719 | 0.2322 | 0.101* | |
C2 | 0.9156 (10) | 1.1758 (8) | 0.1674 (9) | 0.100 (4) | |
H2 | 0.9266 | 1.2105 | 0.2150 | 0.120* | |
C3 | 0.8919 (11) | 1.2079 (8) | 0.0872 (10) | 0.108 (4) | |
H3 | 0.8878 | 1.2653 | 0.0786 | 0.129* | |
C4 | 0.8740 (11) | 1.1545 (8) | 0.0189 (9) | 0.104 (4) | |
H4A | 0.8555 | 1.1753 | −0.0368 | 0.125* | |
C5 | 0.8837 (8) | 1.0698 (7) | 0.0334 (8) | 0.071 (3) | |
C6 | 0.8670 (8) | 1.0084 (8) | −0.0333 (7) | 0.078 (3) | |
C7 | 0.8422 (9) | 1.0240 (9) | −0.1206 (8) | 0.099 (4) | |
H7A | 0.8328 | 1.0785 | −0.1411 | 0.118* | |
C8 | 0.8313 (11) | 0.9573 (13) | −0.1778 (10) | 0.125 (6) | |
H8 | 0.8141 | 0.9682 | −0.2364 | 0.149* | |
C9 | 0.8447 (12) | 0.8794 (10) | −0.1507 (10) | 0.106 (5) | |
H9 | 0.8398 | 0.8354 | −0.1887 | 0.127* | |
C10 | 0.8661 (9) | 0.8660 (8) | −0.0645 (9) | 0.089 (4) | |
H10 | 0.8717 | 0.8112 | −0.0450 | 0.107* | |
C11 | 1.0101 (11) | 0.9078 (7) | 0.3029 (10) | 0.100 (4) | |
H11 | 1.0626 | 0.9105 | 0.2803 | 0.120* | |
C12 | 1.0329 (12) | 0.9058 (8) | 0.3919 (9) | 0.101 (5) | |
H12 | 1.0978 | 0.9093 | 0.4291 | 0.121* | |
C13 | 0.9516 (13) | 0.8982 (7) | 0.4199 (9) | 0.095 (4) | |
H13 | 0.9628 | 0.8950 | 0.4788 | 0.115* | |
C14 | 0.8652 (9) | 0.8954 (6) | 0.3725 (7) | 0.071 (3) | |
H14 | 0.8141 | 0.8903 | 0.3966 | 0.085* | |
C15 | 0.8405 (10) | 0.8996 (5) | 0.2808 (7) | 0.067 (3) | |
C16 | 0.6628 (9) | 1.0700 (7) | 0.1400 (8) | 0.085 (3) | |
H16 | 0.6849 | 1.0562 | 0.1980 | 0.102* | |
C17 | 0.6413 (10) | 1.1532 (8) | 0.1150 (12) | 0.111 (5) | |
H17 | 0.6511 | 1.1947 | 0.1565 | 0.133* | |
C18 | 0.6058 (10) | 1.1740 (9) | 0.0295 (11) | 0.104 (4) | |
H18 | 0.5907 | 1.2289 | 0.0118 | 0.124* | |
C19 | 0.5939 (9) | 1.1119 (8) | −0.0269 (9) | 0.088 (4) | |
H19 | 0.5687 | 1.1245 | −0.0852 | 0.106* | |
C20 | 0.6169 (7) | 1.0306 (6) | −0.0035 (7) | 0.063 (3) | |
C21 | 0.6047 (8) | 0.9607 (7) | −0.0640 (7) | 0.069 (3) | |
C22 | 0.5721 (9) | 0.9690 (9) | −0.1494 (8) | 0.089 (4) | |
H22 | 0.5543 | 1.0215 | −0.1736 | 0.106* | |
C23 | 0.5646 (10) | 0.8994 (9) | −0.2031 (8) | 0.097 (4) | |
H23 | 0.5410 | 0.9049 | −0.2626 | 0.116* | |
C24 | 0.5935 (9) | 0.8219 (8) | −0.1649 (8) | 0.088 (4) | |
H24 | 0.5906 | 0.7743 | −0.1980 | 0.106* | |
C25 | 0.6264 (9) | 0.8181 (7) | −0.0764 (8) | 0.081 (3) | |
H25 | 0.6439 | 0.7664 | −0.0503 | 0.097* | |
C26 | 0.6556 (9) | 0.7124 (8) | 0.1243 (7) | 0.084 (3) | |
H26 | 0.5962 | 0.7354 | 0.1271 | 0.100* | |
C27 | 0.6654 (10) | 0.6285 (7) | 0.1272 (8) | 0.089 (4) | |
H27 | 0.6147 | 0.5940 | 0.1323 | 0.107* | |
C28 | 0.7563 (11) | 0.5953 (7) | 0.1220 (8) | 0.094 (4) | |
H28 | 0.7645 | 0.5378 | 0.1201 | 0.113* | |
C29 | 0.8330 (9) | 0.6487 (7) | 0.1199 (7) | 0.082 (3) | |
H29 | 0.8938 | 0.6268 | 0.1194 | 0.098* | |
C30 | 0.8187 (8) | 0.7368 (7) | 0.1187 (6) | 0.067 (3) |
U11 | U22 | U33 | U12 | U13 | U23 | |
Pt1 | 0.0759 (3) | 0.0569 (3) | 0.0670 (3) | −0.0075 (2) | 0.0148 (2) | −0.00046 (19) |
Pt2 | 0.0749 (3) | 0.0538 (3) | 0.0572 (3) | −0.00105 (19) | 0.0132 (2) | −0.00249 (18) |
N1 | 0.074 (6) | 0.050 (5) | 0.075 (6) | −0.013 (4) | 0.019 (5) | 0.001 (5) |
N2 | 0.074 (6) | 0.072 (6) | 0.071 (6) | −0.009 (5) | 0.024 (5) | −0.014 (5) |
N3 | 0.082 (7) | 0.055 (5) | 0.066 (6) | −0.007 (5) | −0.002 (5) | 0.007 (4) |
N4 | 0.115 (8) | 0.050 (5) | 0.105 (8) | −0.005 (5) | 0.027 (7) | −0.002 (5) |
N5 | 0.066 (5) | 0.065 (6) | 0.079 (6) | 0.009 (4) | 0.015 (5) | −0.014 (5) |
N6 | 0.067 (5) | 0.056 (5) | 0.058 (5) | −0.002 (4) | 0.010 (4) | −0.003 (4) |
N7 | 0.085 (7) | 0.084 (7) | 0.058 (6) | −0.001 (5) | 0.022 (5) | −0.008 (4) |
N8 | 0.088 (7) | 0.050 (5) | 0.062 (5) | 0.008 (5) | 0.010 (5) | 0.004 (4) |
C1 | 0.104 (10) | 0.064 (8) | 0.081 (9) | −0.020 (7) | 0.025 (7) | −0.004 (6) |
C2 | 0.132 (11) | 0.074 (9) | 0.094 (10) | −0.020 (8) | 0.035 (9) | 0.000 (7) |
C3 | 0.147 (13) | 0.059 (8) | 0.122 (12) | −0.015 (8) | 0.048 (11) | 0.008 (8) |
C4 | 0.143 (13) | 0.078 (9) | 0.091 (10) | −0.017 (9) | 0.038 (9) | 0.015 (8) |
C5 | 0.065 (7) | 0.070 (8) | 0.077 (8) | −0.013 (6) | 0.021 (6) | 0.005 (6) |
C6 | 0.076 (7) | 0.087 (9) | 0.075 (8) | −0.020 (6) | 0.031 (6) | 0.011 (7) |
C7 | 0.119 (10) | 0.108 (10) | 0.072 (9) | −0.038 (9) | 0.035 (8) | −0.001 (8) |
C8 | 0.108 (11) | 0.196 (19) | 0.082 (10) | −0.045 (13) | 0.046 (9) | −0.018 (12) |
C9 | 0.134 (13) | 0.110 (12) | 0.083 (11) | −0.034 (10) | 0.045 (9) | −0.017 (9) |
C10 | 0.081 (8) | 0.093 (9) | 0.099 (11) | −0.016 (7) | 0.036 (8) | −0.015 (8) |
C11 | 0.094 (10) | 0.062 (8) | 0.132 (13) | 0.001 (7) | 0.019 (10) | 0.022 (7) |
C12 | 0.106 (11) | 0.096 (10) | 0.066 (9) | −0.007 (8) | −0.022 (8) | 0.017 (7) |
C13 | 0.134 (14) | 0.069 (8) | 0.074 (9) | 0.000 (8) | 0.019 (10) | 0.012 (6) |
C14 | 0.079 (8) | 0.065 (7) | 0.055 (7) | 0.001 (6) | 0.001 (6) | 0.012 (5) |
C15 | 0.094 (9) | 0.039 (6) | 0.070 (8) | −0.006 (5) | 0.029 (7) | 0.005 (5) |
C16 | 0.098 (9) | 0.083 (9) | 0.069 (8) | −0.002 (7) | 0.020 (7) | −0.017 (6) |
C17 | 0.104 (10) | 0.050 (8) | 0.179 (17) | −0.001 (7) | 0.045 (11) | −0.047 (9) |
C18 | 0.091 (10) | 0.087 (10) | 0.118 (12) | 0.017 (8) | 0.012 (9) | 0.009 (9) |
C19 | 0.079 (8) | 0.075 (8) | 0.091 (9) | 0.010 (6) | 0.000 (7) | 0.001 (7) |
C20 | 0.059 (6) | 0.059 (6) | 0.065 (7) | 0.010 (5) | 0.009 (5) | −0.003 (5) |
C21 | 0.069 (7) | 0.067 (7) | 0.062 (7) | −0.001 (5) | 0.008 (6) | 0.001 (5) |
C22 | 0.084 (8) | 0.102 (10) | 0.073 (8) | 0.001 (7) | 0.017 (7) | 0.007 (7) |
C23 | 0.096 (10) | 0.119 (12) | 0.062 (8) | −0.020 (8) | 0.005 (7) | −0.008 (8) |
C24 | 0.085 (8) | 0.094 (10) | 0.081 (9) | 0.001 (7) | 0.019 (7) | −0.017 (7) |
C25 | 0.096 (9) | 0.070 (8) | 0.071 (8) | −0.004 (6) | 0.018 (7) | −0.018 (6) |
C26 | 0.092 (8) | 0.075 (8) | 0.083 (8) | −0.011 (7) | 0.025 (7) | 0.009 (6) |
C27 | 0.096 (10) | 0.064 (8) | 0.089 (9) | −0.015 (7) | 0.002 (7) | 0.026 (6) |
C28 | 0.120 (11) | 0.056 (7) | 0.081 (9) | −0.004 (8) | −0.005 (8) | 0.016 (6) |
C29 | 0.094 (8) | 0.056 (7) | 0.080 (8) | −0.004 (6) | 0.003 (6) | 0.008 (6) |
C30 | 0.068 (7) | 0.057 (7) | 0.062 (7) | −0.001 (6) | 0.000 (6) | 0.004 (5) |
Pt1—N1 | 2.028 (8) | C9—C10 | 1.367 (18) |
Pt1—N2 | 2.017 (9) | C11—C12 | 1.391 (19) |
Pt1—N3 | 2.043 (9) | C12—C13 | 1.372 (19) |
Pt1—N4 | 2.001 (9) | C13—C14 | 1.224 (16) |
Pt2—N5 | 2.017 (8) | C14—C15 | 1.434 (15) |
Pt2—N6 | 2.024 (8) | C16—C17 | 1.399 (17) |
Pt2—N7 | 1.985 (9) | C17—C18 | 1.373 (19) |
Pt2—N8 | 2.020 (8) | C18—C19 | 1.333 (16) |
Pt1—Pt2 | 2.8724 (6) | C19—C20 | 1.369 (14) |
O3A—N9A | 1.227 (10) | C20—C21 | 1.470 (13) |
O4A—N9A | 1.215 (10) | C21—C22 | 1.336 (14) |
O5A—N9A | 1.205 (10) | C22—C23 | 1.405 (17) |
O3B—N9B | 1.228 (10) | C23—C24 | 1.391 (16) |
O4B—N9B | 1.217 (10) | C24—C25 | 1.379 (15) |
O5B—N9B | 1.222 (10) | C26—C27 | 1.350 (15) |
O11A—N10A | 1.200 (10) | C27—C28 | 1.417 (18) |
O12A—N10A | 1.186 (10) | C28—C29 | 1.390 (17) |
O13A—N10A | 1.216 (10) | C29—C30 | 1.426 (14) |
O11B—N10B | 1.208 (10) | N4—H4 | 0.8600 |
O12B—N10B | 1.205 (10) | N7—H7 | 0.8600 |
O13B—N10B | 1.202 (10) | C1—H1 | 0.9300 |
N1—C1 | 1.311 (13) | C2—H2 | 0.9300 |
N1—C5 | 1.349 (13) | C3—H3 | 0.9300 |
N2—C10 | 1.331 (14) | C4—H4A | 0.9300 |
N2—C6 | 1.368 (13) | C7—H7A | 0.9300 |
N3—C11 | 1.336 (15) | C8—H8 | 0.9300 |
N3—C15 | 1.358 (14) | C9—H9 | 0.9300 |
N4—C30 | 1.336 (13) | C10—H10 | 0.9300 |
N5—C20 | 1.336 (12) | C11—H11 | 0.9300 |
N5—C16 | 1.363 (13) | C12—H12 | 0.9300 |
N6—C25 | 1.335 (12) | C13—H13 | 0.9300 |
N6—C21 | 1.362 (12) | C14—H14 | 0.9300 |
N7—C15 | 1.314 (14) | C16—H16 | 0.9300 |
N8—C30 | 1.317 (13) | C17—H17 | 0.9300 |
N8—C26 | 1.418 (14) | C18—H18 | 0.9300 |
N9A—N9B | 0.52 (4) | C19—H19 | 0.9300 |
C1—C2 | 1.337 (15) | C22—H22 | 0.9300 |
C2—C3 | 1.353 (17) | C23—H23 | 0.9300 |
C3—C4 | 1.368 (17) | C24—H24 | 0.9300 |
C4—C5 | 1.378 (16) | C25—H25 | 0.9300 |
C5—C6 | 1.433 (15) | C26—H26 | 0.9300 |
C6—C7 | 1.387 (15) | C27—H27 | 0.9300 |
C7—C8 | 1.397 (19) | C28—H28 | 0.9300 |
C8—C9 | 1.32 (2) | C29—H29 | 0.9300 |
Pt1···Pt1i | 6.2077 (9) | C8···C1i | 3.56 (2) |
Pt2···Pt2ii | 6.4875 (9) | C6···C6i | 3.58 (2) |
N1···N5 | 3.491 (12) | C9···C1i | 3.471 (19) |
N2···N6 | 3.440 (12) | N2···C5i | 3.513 (14) |
C1···C16 | 3.552 (17) | N2···C6i | 3.590 (13) |
C9···C24 | 3.605 (19) | N5···C21ii | 3.582 (13) |
C10···C25 | 3.418 (16) | N6···C18ii | 3.509 (16) |
C9···N1i | 3.630 (17) | C16···C22ii | 3.431 (17) |
C10···C4i | 3.525 (19) | C18···C25ii | 3.602 (18) |
C10···C5i | 3.562 (15) | C20···C20ii | 3.48 (2) |
C8···N1i | 3.530 (17) | ||
N4—Pt1—N2 | 94.6 (4) | N5—C16—C17 | 120.1 (12) |
N4—Pt1—N1 | 174.8 (4) | C18—C17—C16 | 120.4 (12) |
N2—Pt1—N1 | 80.2 (4) | C19—C18—C17 | 117.0 (13) |
N4—Pt1—N3 | 89.0 (3) | C18—C19—C20 | 123.2 (13) |
N2—Pt1—N3 | 176.3 (3) | N5—C20—C19 | 120.5 (10) |
N1—Pt1—N3 | 96.2 (3) | N5—C20—C21 | 114.9 (9) |
N7—Pt2—N5 | 96.3 (4) | C19—C20—C21 | 124.6 (10) |
N7—Pt2—N8 | 88.0 (3) | C22—C21—N6 | 121.3 (10) |
N5—Pt2—N8 | 175.6 (3) | C22—C21—C20 | 124.1 (11) |
N7—Pt2—N6 | 176.3 (3) | N6—C21—C20 | 114.6 (9) |
N5—Pt2—N6 | 80.1 (3) | C21—C22—C23 | 120.7 (12) |
N8—Pt2—N6 | 95.6 (3) | C24—C23—C22 | 118.2 (12) |
N4—Pt1—Pt2 | 80.1 (3) | C25—C24—C23 | 117.8 (12) |
N2—Pt1—Pt2 | 96.5 (2) | N6—C25—C24 | 123.2 (11) |
N1—Pt1—Pt2 | 101.0 (2) | C27—C26—N8 | 123.0 (12) |
N3—Pt1—Pt2 | 83.4 (3) | C26—C27—C28 | 117.2 (12) |
N7—Pt2—Pt1 | 80.6 (3) | C29—C28—C27 | 120.0 (11) |
N5—Pt2—Pt1 | 96.4 (2) | C28—C29—C30 | 120.0 (13) |
N8—Pt2—Pt1 | 83.2 (3) | N8—C30—N4 | 120.6 (10) |
N6—Pt2—Pt1 | 99.4 (2) | N8—C30—C29 | 119.5 (11) |
C1—N1—C5 | 116.9 (10) | N4—C30—C29 | 119.8 (11) |
C1—N1—Pt1 | 128.4 (8) | C30—N4—H4 | 115.2 |
C5—N1—Pt1 | 114.5 (7) | Pt1—N4—H4 | 115.2 |
C10—N2—C6 | 119.8 (11) | C15—N7—H7 | 114.8 |
C10—N2—Pt1 | 126.2 (9) | Pt2—N7—H7 | 114.8 |
C6—N2—Pt1 | 113.5 (7) | N1—C1—H1 | 117.2 |
C11—N3—C15 | 118.2 (11) | C2—C1—H1 | 117.2 |
C11—N3—Pt1 | 118.2 (10) | C1—C2—H2 | 120.9 |
C15—N3—Pt1 | 123.6 (8) | C3—C2—H2 | 120.9 |
C30—N4—Pt1 | 129.6 (8) | C2—C3—H3 | 120.5 |
C20—N5—C16 | 118.7 (9) | C4—C3—H3 | 120.5 |
C20—N5—Pt2 | 115.6 (7) | C3—C4—H4A | 120.2 |
C16—N5—Pt2 | 125.5 (8) | C5—C4—H4A | 120.2 |
C25—N6—C21 | 118.7 (9) | C6—C7—H7A | 120.2 |
C25—N6—Pt2 | 126.7 (7) | C8—C7—H7A | 120.2 |
C21—N6—Pt2 | 114.6 (7) | C9—C8—H8 | 119.2 |
C15—N7—Pt2 | 130.5 (8) | C7—C8—H8 | 119.2 |
C30—N8—C26 | 120.0 (9) | C8—C9—H9 | 121.3 |
C30—N8—Pt2 | 125.4 (7) | C10—C9—H9 | 121.3 |
C26—N8—Pt2 | 114.6 (8) | N2—C10—H10 | 118.1 |
O5A—N9A—O4A | 120.9 (9) | C9—C10—H10 | 118.1 |
O5A—N9A—O3A | 119.9 (9) | N3—C11—H11 | 118.0 |
O4A—N9A—O3A | 119.3 (9) | C12—C11—H11 | 118.0 |
O4B—N9B—O5B | 120.5 (9) | C13—C12—H12 | 122.8 |
O4B—N9B—O3B | 120.4 (9) | C11—C12—H12 | 122.8 |
O5B—N9B—O3B | 119.1 (9) | C14—C13—H13 | 117.9 |
O12A—N10A—O11A | 121.6 (9) | C12—C13—H13 | 117.9 |
O12A—N10A—O13A | 119.8 (9) | C13—C14—H14 | 119.1 |
O11A—N10A—O13A | 118.7 (9) | C15—C14—H14 | 119.1 |
O13B—N10B—O12B | 120.3 (9) | N5—C16—H16 | 119.9 |
O13B—N10B—O11B | 119.3 (9) | C17—C16—H16 | 119.9 |
O12B—N10B—O11B | 120.3 (9) | C18—C17—H17 | 119.8 |
N1—C1—C2 | 125.6 (12) | C16—C17—H17 | 119.8 |
C1—C2—C3 | 118.2 (13) | C19—C18—H18 | 121.5 |
C2—C3—C4 | 119.0 (13) | C17—C18—H18 | 121.5 |
C3—C4—C5 | 119.5 (12) | C18—C19—H19 | 118.4 |
N1—C5—C4 | 120.7 (11) | C20—C19—H19 | 118.4 |
N1—C5—C6 | 115.0 (10) | C21—C22—H22 | 119.6 |
C4—C5—C6 | 124.2 (11) | C23—C22—H22 | 119.6 |
N2—C6—C7 | 117.7 (12) | C24—C23—H23 | 120.9 |
N2—C6—C5 | 116.0 (10) | C22—C23—H23 | 120.9 |
C7—C6—C5 | 126.2 (12) | C25—C24—H24 | 121.1 |
C6—C7—C8 | 119.6 (14) | C23—C24—H24 | 121.1 |
C9—C8—C7 | 121.6 (15) | N6—C25—H25 | 118.4 |
C8—C9—C10 | 117.3 (15) | C24—C25—H25 | 118.4 |
N2—C10—C9 | 123.8 (13) | C27—C26—H26 | 118.5 |
N3—C11—C12 | 123.9 (14) | N8—C26—H26 | 118.5 |
C13—C12—C11 | 114.4 (13) | C26—C27—H27 | 121.4 |
C14—C13—C12 | 124.3 (14) | C28—C27—H27 | 121.4 |
C13—C14—C15 | 121.9 (14) | C29—C28—H28 | 120.0 |
N7—C15—N3 | 120.7 (10) | C27—C28—H28 | 120.0 |
N7—C15—C14 | 122.0 (11) | C28—C29—H29 | 120.0 |
N3—C15—C14 | 117.3 (11) | C30—C29—H29 | 120.0 |
N3—Pt1—Pt2—N7 | 6.2 (3) | C13—C14—C15—N7 | −177.1 (11) |
N1—Pt1—Pt2—N5 | 6.4 (4) | C13—C14—C15—N3 | 0.7 (15) |
N4—Pt1—Pt2—N8 | 7.2 (4) | C20—N5—C16—C17 | −1.9 (17) |
N2—Pt1—Pt2—N6 | 6.2 (3) | N5—C16—C17—C18 | 2 (2) |
C5—N1—C1—C2 | 3.4 (19) | C16—C17—C18—C19 | 0 (2) |
N1—C1—C2—C3 | −2 (2) | C17—C18—C19—C20 | −1 (2) |
C1—C2—C3—C4 | 2 (2) | C16—N5—C20—C19 | 0.3 (16) |
C2—C3—C4—C5 | −2 (2) | C16—N5—C20—C21 | −178.5 (9) |
C1—N1—C5—C4 | −3.8 (16) | C18—C19—C20—N5 | 1.3 (19) |
C1—N1—C5—C6 | 179.1 (10) | C18—C19—C20—C21 | −180.0 (12) |
C3—C4—C5—N1 | 3.3 (19) | C25—N6—C21—C22 | −2.8 (16) |
C3—C4—C5—C6 | −179.9 (12) | C25—N6—C21—C20 | −179.8 (9) |
C10—N2—C6—C7 | −0.9 (16) | N5—C20—C21—C22 | −179.3 (11) |
C10—N2—C6—C5 | −179.4 (9) | C19—C20—C21—C22 | 1.9 (18) |
N1—C5—C6—N2 | −2.5 (15) | N5—C20—C21—N6 | −2.5 (13) |
C4—C5—C6—N2 | −179.4 (10) | C19—C20—C21—N6 | 178.7 (10) |
N1—C5—C6—C7 | 179.2 (11) | N6—C21—C22—C23 | 1.9 (18) |
C4—C5—C6—C7 | 2 (2) | C20—C21—C22—C23 | 178.6 (11) |
N2—C6—C7—C8 | −0.4 (18) | C21—C22—C23—C24 | −1 (2) |
C5—C6—C7—C8 | 178.0 (12) | C22—C23—C24—C25 | 0.9 (19) |
C6—C7—C8—C9 | 0 (2) | C21—N6—C25—C24 | 2.8 (17) |
C7—C8—C9—C10 | 2 (2) | C23—C24—C25—N6 | −1.9 (19) |
C6—N2—C10—C9 | 3.1 (18) | C30—N8—C26—C27 | −4.2 (17) |
C8—C9—C10—N2 | −4 (2) | N8—C26—C27—C28 | −0.6 (18) |
C15—N3—C11—C12 | −1.9 (16) | C26—C27—C28—C29 | 4.1 (18) |
N3—C11—C12—C13 | 2.6 (18) | C27—C28—C29—C30 | −3.1 (18) |
C11—C12—C13—C14 | −2 (2) | C26—N8—C30—N4 | −178.3 (9) |
C12—C13—C14—C15 | 0 (2) | C26—N8—C30—C29 | 5.2 (15) |
C11—N3—C15—N7 | 178.0 (9) | C28—C29—C30—N8 | −1.6 (16) |
C11—N3—C15—C14 | 0.1 (13) | C28—C29—C30—N4 | −178.2 (10) |
Symmetry codes: (i) −x+2, −y+2, −z; (ii) −x+1, −y+2, −z. |
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