


Supporting information
![]() | Crystallographic Information File (CIF) https://doi.org/10.1107/S160053680905301X/hy2248sup1.cif |
![]() | Structure factor file (CIF format) https://doi.org/10.1107/S160053680905301X/hy2248Isup2.hkl |
CCDC reference: 766671
Key indicators
- Single-crystal X-ray study
- T = 101 K
- Mean
(C-C) = 0.004 Å
- R factor = 0.022
- wR factor = 0.053
- Data-to-parameter ratio = 21.1
checkCIF/PLATON results
No syntax errors found
Alert level B PLAT919_ALERT_3_B Reflection(s) # Likely Affected by the Beamstop 1
Alert level C PLAT094_ALERT_2_C Ratio of Maximum / Minimum Residual Density .... 2.45 PLAT910_ALERT_3_C Missing # of FCF Reflections Below Th(Min) ..... 1 PLAT911_ALERT_3_C Missing # FCF Refl Between THmin & STh/L= 0.600 2 PLAT912_ALERT_4_C Missing # of FCF Reflections Above STh/L= 0.600 21
Alert level G PLAT960_ALERT_3_G Number of Intensities with I .LT. - 2*sig(I) .. 1 PLAT128_ALERT_4_G Non-standard setting of Space-group P21/c .... P21/n
0 ALERT level A = In general: serious problem 1 ALERT level B = Potentially serious problem 4 ALERT level C = Check and explain 2 ALERT level G = General alerts; check 0 ALERT type 1 CIF construction/syntax error, inconsistent or missing data 1 ALERT type 2 Indicator that the structure model may be wrong or deficient 4 ALERT type 3 Indicator that the structure quality may be low 2 ALERT type 4 Improvement, methodology, query or suggestion 0 ALERT type 5 Informative message, check
Pt(cod)Cl2 (50 mg, 0.13 mmol) (cod = 1,5-cyclooctadiene) was dissolved in dichloromethane (15 ml). Bis(diphenylphosphino)propylamine (57.1 mg, 0.13 mmol) was also dissolved in dichloromethane (10 ml) and was added dropwise to the Pt(cod)Cl2 solution. The solution was stirred for 2 h at room temperature. The reaction mixture was layered with methanol (10 ml). Colourless single crystals suitable for X-ray crystallography was obtained after 1 d (yield 0.066 g, 73.4%).
H atoms were positioned geometrically and refined as riding atoms, with C—H = 0.95 (aromatic), 0.99 (CH2) and 0.98 (CH3) Å and with Uiso(H) = 1.2(1.5 for methyl)Ueq(C). The highest residual electron density was found 0.84Å from Pt and the deepest hole 0.68Å from Pt.
Data collection: APEX2 (Bruker, 2007); cell refinement: SAINT-Plus (Bruker, 2007); data reduction: SAINT-Plus (Bruker, 2007); program(s) used to solve structure: SIR97 (Altomare et al., 1999); program(s) used to refine structure: SHELXL97 (Sheldrick, 2008); molecular graphics: DIAMOND (Brandenburg & Putz, 1999); software used to prepare material for publication: WinGX (Farrugia, 1999).
[PtCl2(C27H27NP2)] | F(000) = 1352 |
Mr = 693.43 | Dx = 1.819 Mg m−3 |
Monoclinic, P21/n | Mo Kα radiation, λ = 0.71073 Å |
Hall symbol: -P 2yn | Cell parameters from 6904 reflections |
a = 10.6301 (4) Å | θ = 2.6–28.2° |
b = 18.8117 (7) Å | µ = 5.90 mm−1 |
c = 12.7653 (5) Å | T = 101 K |
β = 97.326 (1)° | Plate, colourless |
V = 2531.84 (17) Å3 | 0.38 × 0.10 × 0.02 mm |
Z = 4 |
Bruker X8 APEXII Kappa CCD diffractometer | 5347 reflections with I > 2σ(I) |
ω and ϕ scans | Rint = 0.052 |
Absorption correction: multi-scan (SADABS; Bruker, 2001) | θmax = 28.3°, θmin = 2.2° |
Tmin = 0.213, Tmax = 0.891 | h = −14→14 |
50743 measured reflections | k = −25→25 |
6276 independent reflections | l = −17→17 |
Refinement on F2 | 0 restraints |
Least-squares matrix: full | H-atom parameters constrained |
R[F2 > 2σ(F2)] = 0.022 | w = 1/[σ2(Fo2) + (0.0238P)2 + 1.2293P] where P = (Fo2 + 2Fc2)/3 |
wR(F2) = 0.053 | (Δ/σ)max = 0.002 |
S = 1.04 | Δρmax = 1.55 e Å−3 |
6276 reflections | Δρmin = −0.63 e Å−3 |
298 parameters |
[PtCl2(C27H27NP2)] | V = 2531.84 (17) Å3 |
Mr = 693.43 | Z = 4 |
Monoclinic, P21/n | Mo Kα radiation |
a = 10.6301 (4) Å | µ = 5.90 mm−1 |
b = 18.8117 (7) Å | T = 101 K |
c = 12.7653 (5) Å | 0.38 × 0.10 × 0.02 mm |
β = 97.326 (1)° |
Bruker X8 APEXII Kappa CCD diffractometer | 6276 independent reflections |
Absorption correction: multi-scan (SADABS; Bruker, 2001) | 5347 reflections with I > 2σ(I) |
Tmin = 0.213, Tmax = 0.891 | Rint = 0.052 |
50743 measured reflections |
R[F2 > 2σ(F2)] = 0.022 | 0 restraints |
wR(F2) = 0.053 | H-atom parameters constrained |
S = 1.04 | Δρmax = 1.55 e Å−3 |
6276 reflections | Δρmin = −0.63 e Å−3 |
298 parameters |
Experimental. The intensity data was collected on a Bruker X8 Apex II 4 K Kappa CCD diffractometer using an exposure time of 20 s/frame. A total of 1264 frames were collected with a frame width of 0.5° covering up to θ = 28.23° with 99.6% completeness accomplished. |
x | y | z | Uiso*/Ueq | ||
N1 | 0.3830 (2) | 0.20629 (12) | 0.24699 (19) | 0.0122 (5) | |
P1 | 0.27187 (7) | 0.19470 (4) | 0.33006 (6) | 0.01071 (15) | |
P2 | 0.39535 (7) | 0.29612 (4) | 0.24933 (6) | 0.01051 (15) | |
Cl1 | 0.10041 (7) | 0.29205 (4) | 0.47535 (6) | 0.01820 (15) | |
Cl2 | 0.23004 (7) | 0.43335 (4) | 0.36231 (6) | 0.01938 (16) | |
Pt | 0.250086 (9) | 0.308869 (5) | 0.357534 (8) | 0.00997 (4) | |
C1 | 0.4307 (3) | 0.15118 (15) | 0.1788 (2) | 0.0152 (6) | |
H1A | 0.4419 | 0.1731 | 0.11 | 0.018* | |
H1B | 0.3654 | 0.1136 | 0.1651 | 0.018* | |
C2 | 0.5540 (3) | 0.11697 (16) | 0.2238 (2) | 0.0209 (7) | |
H2A | 0.5478 | 0.0999 | 0.2963 | 0.025* | |
H2B | 0.6232 | 0.1525 | 0.2276 | 0.025* | |
C3 | 0.5846 (3) | 0.05447 (15) | 0.1546 (2) | 0.0205 (7) | |
H3A | 0.6649 | 0.0327 | 0.1847 | 0.031* | |
H3B | 0.5918 | 0.0715 | 0.0831 | 0.031* | |
H3C | 0.5165 | 0.0191 | 0.1518 | 0.031* | |
C11 | 0.1349 (3) | 0.15250 (15) | 0.2579 (2) | 0.0129 (6) | |
C12 | 0.1292 (3) | 0.07992 (16) | 0.2354 (2) | 0.0178 (6) | |
H12 | 0.1963 | 0.0495 | 0.2638 | 0.021* | |
C13 | 0.0254 (3) | 0.05216 (17) | 0.1714 (2) | 0.0208 (7) | |
H13 | 0.0215 | 0.0026 | 0.1569 | 0.025* | |
C14 | −0.0725 (3) | 0.09605 (17) | 0.1286 (2) | 0.0210 (7) | |
H14 | −0.1427 | 0.0767 | 0.0842 | 0.025* | |
C15 | −0.0678 (3) | 0.16837 (18) | 0.1507 (2) | 0.0204 (7) | |
H15 | −0.1352 | 0.1985 | 0.1219 | 0.025* | |
C16 | 0.0354 (3) | 0.19657 (16) | 0.2150 (2) | 0.0174 (6) | |
H16 | 0.0385 | 0.2461 | 0.2299 | 0.021* | |
C21 | 0.3394 (3) | 0.13850 (15) | 0.4372 (2) | 0.0123 (6) | |
C22 | 0.4622 (3) | 0.15416 (16) | 0.4831 (2) | 0.0189 (6) | |
H22 | 0.5072 | 0.1921 | 0.4557 | 0.023* | |
C23 | 0.5195 (3) | 0.11521 (16) | 0.5679 (2) | 0.0192 (7) | |
H23 | 0.6035 | 0.1264 | 0.5981 | 0.023* | |
C24 | 0.4550 (3) | 0.06004 (16) | 0.6087 (2) | 0.0189 (6) | |
H24 | 0.4945 | 0.033 | 0.6667 | 0.023* | |
C25 | 0.3330 (3) | 0.04456 (17) | 0.5647 (3) | 0.0255 (7) | |
H25 | 0.2885 | 0.0066 | 0.5925 | 0.031* | |
C26 | 0.2738 (3) | 0.08392 (16) | 0.4798 (2) | 0.0206 (7) | |
H26 | 0.1889 | 0.0735 | 0.4511 | 0.025* | |
C31 | 0.5551 (3) | 0.32517 (15) | 0.2956 (2) | 0.0134 (6) | |
C32 | 0.6533 (3) | 0.31537 (15) | 0.2338 (2) | 0.0174 (6) | |
H32 | 0.6376 | 0.2925 | 0.1671 | 0.021* | |
C33 | 0.7734 (3) | 0.33934 (17) | 0.2709 (3) | 0.0226 (7) | |
H33 | 0.8413 | 0.3316 | 0.2305 | 0.027* | |
C34 | 0.7957 (3) | 0.37464 (17) | 0.3668 (3) | 0.0250 (8) | |
H34 | 0.8786 | 0.3912 | 0.3914 | 0.03* | |
C35 | 0.6988 (3) | 0.38594 (16) | 0.4269 (3) | 0.0205 (7) | |
H35 | 0.7146 | 0.4109 | 0.4919 | 0.025* | |
C36 | 0.5776 (3) | 0.36064 (15) | 0.3920 (2) | 0.0157 (6) | |
H36 | 0.5107 | 0.3675 | 0.4337 | 0.019* | |
C41 | 0.3704 (3) | 0.32672 (15) | 0.1144 (2) | 0.0124 (6) | |
C42 | 0.2932 (3) | 0.28739 (15) | 0.0390 (2) | 0.0152 (6) | |
H42 | 0.253 | 0.2453 | 0.0593 | 0.018* | |
C43 | 0.2749 (3) | 0.30953 (15) | −0.0655 (2) | 0.0158 (6) | |
H43 | 0.2215 | 0.283 | −0.1167 | 0.019* | |
C44 | 0.3346 (3) | 0.37023 (16) | −0.0948 (2) | 0.0169 (6) | |
H44 | 0.3245 | 0.3846 | −0.1667 | 0.02* | |
C45 | 0.4088 (3) | 0.41015 (16) | −0.0201 (2) | 0.0182 (6) | |
H45 | 0.4477 | 0.4525 | −0.0406 | 0.022* | |
C46 | 0.4272 (3) | 0.38889 (15) | 0.0847 (2) | 0.0169 (6) | |
H46 | 0.4782 | 0.4166 | 0.136 | 0.02* |
U11 | U22 | U33 | U12 | U13 | U23 | |
N1 | 0.0146 (12) | 0.0097 (12) | 0.0134 (12) | 0.0010 (9) | 0.0058 (10) | 0.0007 (9) |
P1 | 0.0109 (3) | 0.0113 (4) | 0.0104 (3) | 0.0002 (3) | 0.0030 (3) | 0.0000 (3) |
P2 | 0.0100 (3) | 0.0112 (4) | 0.0104 (4) | 0.0005 (3) | 0.0014 (3) | 0.0010 (3) |
Cl1 | 0.0176 (4) | 0.0213 (4) | 0.0176 (4) | 0.0008 (3) | 0.0093 (3) | −0.0008 (3) |
Cl2 | 0.0240 (4) | 0.0116 (3) | 0.0225 (4) | 0.0025 (3) | 0.0025 (3) | 0.0003 (3) |
Pt | 0.01023 (6) | 0.01022 (6) | 0.00961 (6) | 0.00052 (4) | 0.00187 (4) | −0.00044 (4) |
C1 | 0.0176 (15) | 0.0141 (15) | 0.0151 (15) | −0.0014 (12) | 0.0065 (12) | −0.0006 (11) |
C2 | 0.0232 (17) | 0.0208 (17) | 0.0182 (16) | 0.0031 (13) | 0.0009 (13) | 0.0009 (13) |
C3 | 0.0251 (17) | 0.0124 (15) | 0.0257 (17) | 0.0050 (13) | 0.0099 (14) | 0.0021 (13) |
C11 | 0.0131 (14) | 0.0176 (15) | 0.0084 (14) | −0.0023 (11) | 0.0034 (11) | 0.0003 (11) |
C12 | 0.0166 (15) | 0.0183 (16) | 0.0192 (16) | 0.0002 (12) | 0.0044 (12) | −0.0024 (12) |
C13 | 0.0231 (16) | 0.0186 (16) | 0.0215 (17) | −0.0059 (13) | 0.0056 (13) | −0.0064 (13) |
C14 | 0.0156 (15) | 0.0328 (19) | 0.0146 (16) | −0.0079 (13) | 0.0022 (12) | −0.0028 (13) |
C15 | 0.0168 (15) | 0.0304 (18) | 0.0140 (15) | −0.0009 (13) | 0.0014 (12) | 0.0030 (13) |
C16 | 0.0158 (15) | 0.0174 (16) | 0.0191 (16) | −0.0006 (12) | 0.0022 (12) | −0.0012 (12) |
C21 | 0.0148 (14) | 0.0111 (14) | 0.0117 (14) | 0.0015 (11) | 0.0039 (11) | −0.0004 (11) |
C22 | 0.0185 (16) | 0.0192 (16) | 0.0189 (16) | −0.0045 (13) | 0.0023 (13) | 0.0066 (13) |
C23 | 0.0131 (15) | 0.0239 (17) | 0.0201 (16) | −0.0035 (12) | −0.0002 (12) | 0.0047 (13) |
C24 | 0.0231 (16) | 0.0166 (16) | 0.0169 (16) | 0.0041 (13) | 0.0020 (13) | 0.0056 (12) |
C25 | 0.0296 (18) | 0.0218 (17) | 0.0246 (18) | −0.0095 (14) | 0.0019 (14) | 0.0101 (14) |
C26 | 0.0158 (15) | 0.0250 (17) | 0.0203 (16) | −0.0040 (13) | −0.0004 (12) | 0.0032 (13) |
C31 | 0.0120 (14) | 0.0131 (14) | 0.0149 (15) | −0.0023 (11) | 0.0006 (11) | 0.0045 (11) |
C32 | 0.0177 (15) | 0.0172 (16) | 0.0175 (16) | 0.0015 (12) | 0.0026 (12) | 0.0065 (12) |
C33 | 0.0148 (15) | 0.0212 (17) | 0.0321 (19) | 0.0021 (13) | 0.0043 (14) | 0.0129 (14) |
C34 | 0.0143 (15) | 0.0197 (17) | 0.038 (2) | −0.0043 (13) | −0.0084 (14) | 0.0147 (14) |
C35 | 0.0249 (17) | 0.0144 (15) | 0.0191 (16) | −0.0019 (13) | −0.0096 (13) | 0.0035 (12) |
C36 | 0.0176 (15) | 0.0145 (15) | 0.0140 (15) | 0.0002 (12) | −0.0016 (12) | 0.0043 (11) |
C41 | 0.0129 (14) | 0.0129 (14) | 0.0114 (14) | 0.0033 (11) | 0.0020 (11) | 0.0011 (11) |
C42 | 0.0176 (15) | 0.0114 (14) | 0.0160 (15) | 0.0007 (11) | 0.0003 (12) | −0.0003 (11) |
C43 | 0.0207 (16) | 0.0157 (15) | 0.0106 (14) | 0.0026 (12) | 0.0001 (12) | −0.0038 (11) |
C44 | 0.0183 (15) | 0.0221 (16) | 0.0099 (14) | 0.0077 (12) | 0.0002 (12) | 0.0024 (12) |
C45 | 0.0177 (15) | 0.0178 (16) | 0.0189 (16) | −0.0050 (12) | 0.0015 (12) | 0.0069 (12) |
C46 | 0.0159 (15) | 0.0153 (15) | 0.0179 (16) | −0.0017 (12) | −0.0039 (12) | 0.0011 (12) |
N1—C1 | 1.484 (3) | C21—C22 | 1.393 (4) |
N1—P2 | 1.695 (2) | C22—C23 | 1.383 (4) |
N1—P1 | 1.699 (2) | C22—H22 | 0.95 |
P1—C21 | 1.804 (3) | C23—C24 | 1.383 (4) |
P1—C11 | 1.804 (3) | C23—H23 | 0.95 |
Pt—P1 | 2.1932 (7) | C24—C25 | 1.378 (4) |
P1—P2 | 2.6019 (10) | C24—H24 | 0.95 |
P2—C41 | 1.804 (3) | C25—C26 | 1.394 (4) |
P2—C31 | 1.810 (3) | C25—H25 | 0.95 |
Pt—P2 | 2.2121 (7) | C26—H26 | 0.95 |
Pt—Cl1 | 2.3461 (7) | C31—C36 | 1.394 (4) |
Pt—Cl2 | 2.3528 (7) | C31—C32 | 1.399 (4) |
C1—C2 | 1.507 (4) | C32—C33 | 1.379 (4) |
C1—H1A | 0.99 | C32—H32 | 0.95 |
C1—H1B | 0.99 | C33—C34 | 1.387 (5) |
C2—C3 | 1.530 (4) | C33—H33 | 0.95 |
C2—H2A | 0.99 | C34—C35 | 1.377 (5) |
C2—H2B | 0.99 | C34—H34 | 0.95 |
C3—H3A | 0.98 | C35—C36 | 1.392 (4) |
C3—H3B | 0.98 | C35—H35 | 0.95 |
C3—H3C | 0.98 | C36—H36 | 0.95 |
C11—C12 | 1.395 (4) | C41—C46 | 1.391 (4) |
C11—C16 | 1.400 (4) | C41—C42 | 1.394 (4) |
C12—C13 | 1.388 (4) | C42—C43 | 1.388 (4) |
C12—H12 | 0.95 | C42—H42 | 0.95 |
C13—C14 | 1.385 (4) | C43—C44 | 1.381 (4) |
C13—H13 | 0.95 | C43—H43 | 0.95 |
C14—C15 | 1.389 (4) | C44—C45 | 1.380 (4) |
C14—H14 | 0.95 | C44—H44 | 0.95 |
C15—C16 | 1.389 (4) | C45—C46 | 1.386 (4) |
C15—H15 | 0.95 | C45—H45 | 0.95 |
C16—H16 | 0.95 | C46—H46 | 0.95 |
C21—C26 | 1.390 (4) | ||
C1—N1—P2 | 132.48 (19) | C14—C15—H15 | 120 |
C1—N1—P1 | 126.38 (19) | C15—C16—C11 | 120.4 (3) |
P2—N1—P1 | 100.11 (12) | C15—C16—H16 | 119.8 |
N1—P1—C21 | 107.92 (12) | C11—C16—H16 | 119.8 |
N1—P1—C11 | 108.52 (12) | C26—C21—C22 | 118.8 (3) |
C21—P1—C11 | 110.26 (14) | C26—C21—P1 | 124.0 (2) |
N1—P1—Pt | 94.02 (8) | C22—C21—P1 | 117.1 (2) |
C21—P1—Pt | 119.51 (10) | C23—C22—C21 | 120.9 (3) |
C11—P1—Pt | 114.70 (10) | C23—C22—H22 | 119.6 |
C21—P1—P2 | 123.93 (10) | C21—C22—H22 | 119.6 |
C11—P1—P2 | 122.36 (10) | C22—C23—C24 | 120.2 (3) |
Pt—P1—P2 | 54.13 (2) | C22—C23—H23 | 119.9 |
N1—P2—C41 | 107.43 (13) | C24—C23—H23 | 119.9 |
N1—P2—C31 | 111.98 (13) | C25—C24—C23 | 119.4 (3) |
C41—P2—C31 | 103.49 (13) | C25—C24—H24 | 120.3 |
N1—P2—Pt | 93.46 (8) | C23—C24—H24 | 120.3 |
C41—P2—Pt | 122.17 (9) | C24—C25—C26 | 120.9 (3) |
C31—P2—Pt | 117.65 (10) | C24—C25—H25 | 119.6 |
C41—P2—P1 | 126.30 (10) | C26—C25—H25 | 119.6 |
C31—P2—P1 | 126.28 (10) | C21—C26—C25 | 119.8 (3) |
Pt—P2—P1 | 53.46 (2) | C21—C26—H26 | 120.1 |
P1—Pt—P2 | 72.40 (3) | C25—C26—H26 | 120.1 |
P1—Pt—Cl1 | 93.70 (3) | C36—C31—C32 | 120.3 (3) |
P2—Pt—Cl1 | 165.96 (3) | C36—C31—P2 | 118.8 (2) |
P1—Pt—Cl2 | 172.11 (3) | C32—C31—P2 | 120.9 (2) |
P2—Pt—Cl2 | 101.35 (3) | C33—C32—C31 | 119.2 (3) |
Cl1—Pt—Cl2 | 92.67 (3) | C33—C32—H32 | 120.4 |
N1—C1—C2 | 114.9 (2) | C31—C32—H32 | 120.4 |
N1—C1—H1A | 108.6 | C32—C33—C34 | 120.4 (3) |
C2—C1—H1A | 108.6 | C32—C33—H33 | 119.8 |
N1—C1—H1B | 108.6 | C34—C33—H33 | 119.8 |
C2—C1—H1B | 108.6 | C35—C34—C33 | 120.7 (3) |
H1A—C1—H1B | 107.5 | C35—C34—H34 | 119.7 |
C1—C2—C3 | 110.3 (3) | C33—C34—H34 | 119.7 |
C1—C2—H2A | 109.6 | C34—C35—C36 | 119.8 (3) |
C3—C2—H2A | 109.6 | C34—C35—H35 | 120.1 |
C1—C2—H2B | 109.6 | C36—C35—H35 | 120.1 |
C3—C2—H2B | 109.6 | C35—C36—C31 | 119.6 (3) |
H2A—C2—H2B | 108.1 | C35—C36—H36 | 120.2 |
C2—C3—H3A | 109.5 | C31—C36—H36 | 120.2 |
C2—C3—H3B | 109.5 | C46—C41—C42 | 119.8 (3) |
H3A—C3—H3B | 109.5 | C46—C41—P2 | 120.8 (2) |
C2—C3—H3C | 109.5 | C42—C41—P2 | 119.4 (2) |
H3A—C3—H3C | 109.5 | C43—C42—C41 | 120.1 (3) |
H3B—C3—H3C | 109.5 | C43—C42—H42 | 119.9 |
C12—C11—C16 | 119.2 (3) | C41—C42—H42 | 119.9 |
C12—C11—P1 | 123.2 (2) | C44—C43—C42 | 119.7 (3) |
C16—C11—P1 | 117.4 (2) | C44—C43—H43 | 120.1 |
C13—C12—C11 | 120.0 (3) | C42—C43—H43 | 120.1 |
C13—C12—H12 | 120 | C45—C44—C43 | 120.3 (3) |
C11—C12—H12 | 120 | C45—C44—H44 | 119.8 |
C14—C13—C12 | 120.6 (3) | C43—C44—H44 | 119.8 |
C14—C13—H13 | 119.7 | C44—C45—C46 | 120.5 (3) |
C12—C13—H13 | 119.7 | C44—C45—H45 | 119.7 |
C13—C14—C15 | 119.8 (3) | C46—C45—H45 | 119.7 |
C13—C14—H14 | 120.1 | C45—C46—C41 | 119.5 (3) |
C15—C14—H14 | 120.1 | C45—C46—H46 | 120.2 |
C16—C15—C14 | 120.0 (3) | C41—C46—H46 | 120.2 |
C16—C15—H15 | 120 | ||
C1—N1—P1—C21 | 68.6 (3) | C16—C11—C12—C13 | −0.3 (4) |
P2—N1—P1—C21 | −121.87 (13) | P1—C11—C12—C13 | −174.2 (2) |
C1—N1—P1—C11 | −50.9 (3) | C11—C12—C13—C14 | 0.7 (4) |
P2—N1—P1—C11 | 118.66 (14) | C12—C13—C14—C15 | −0.8 (5) |
C1—N1—P1—Pt | −168.6 (2) | C13—C14—C15—C16 | 0.5 (4) |
P2—N1—P1—Pt | 0.93 (11) | C14—C15—C16—C11 | −0.1 (4) |
C1—N1—P1—P2 | −169.5 (3) | C12—C11—C16—C15 | 0.0 (4) |
C1—N1—P2—C41 | 42.3 (3) | P1—C11—C16—C15 | 174.3 (2) |
P1—N1—P2—C41 | −126.24 (13) | N1—P1—C21—C26 | −138.4 (3) |
C1—N1—P2—C31 | −70.6 (3) | C11—P1—C21—C26 | −20.0 (3) |
P1—N1—P2—C31 | 120.79 (14) | Pt—P1—C21—C26 | 116.1 (2) |
C1—N1—P2—Pt | 167.6 (2) | P2—P1—C21—C26 | −179.4 (2) |
P1—N1—P2—Pt | −0.92 (11) | N1—P1—C21—C22 | 45.4 (3) |
C1—N1—P2—P1 | 168.6 (3) | C11—P1—C21—C22 | 163.8 (2) |
C21—P1—P2—N1 | 76.89 (17) | Pt—P1—C21—C22 | −60.1 (2) |
C11—P1—P2—N1 | −80.10 (17) | P2—P1—C21—C22 | 4.4 (3) |
Pt—P1—P2—N1 | −178.85 (13) | C26—C21—C22—C23 | 1.5 (5) |
N1—P1—P2—C41 | 72.71 (17) | P1—C21—C22—C23 | 177.9 (2) |
C21—P1—P2—C41 | 149.61 (16) | C21—C22—C23—C24 | −0.3 (5) |
C11—P1—P2—C41 | −7.38 (17) | C22—C23—C24—C25 | −0.4 (5) |
Pt—P1—P2—C41 | −106.14 (12) | C23—C24—C25—C26 | −0.2 (5) |
N1—P1—P2—C31 | −81.22 (18) | C22—C21—C26—C25 | −2.1 (5) |
C21—P1—P2—C31 | −4.33 (17) | P1—C21—C26—C25 | −178.2 (2) |
C11—P1—P2—C31 | −161.32 (16) | C24—C25—C26—C21 | 1.5 (5) |
Pt—P1—P2—C31 | 99.93 (12) | N1—P2—C31—C36 | −113.0 (2) |
N1—P1—P2—Pt | 178.85 (13) | C41—P2—C31—C36 | 131.6 (2) |
C21—P1—P2—Pt | −104.26 (11) | Pt—P2—C31—C36 | −6.4 (3) |
C11—P1—P2—Pt | 98.75 (11) | P1—P2—C31—C36 | −69.7 (3) |
N1—P1—Pt—P2 | −0.74 (9) | N1—P2—C31—C32 | 70.1 (3) |
C21—P1—Pt—P2 | 112.48 (11) | C41—P2—C31—C32 | −45.3 (3) |
C11—P1—Pt—P2 | −113.24 (10) | Pt—P2—C31—C32 | 176.61 (19) |
N1—P1—Pt—Cl1 | −178.70 (9) | P1—P2—C31—C32 | 113.3 (2) |
C21—P1—Pt—Cl1 | −65.49 (11) | C36—C31—C32—C33 | 1.9 (4) |
C11—P1—Pt—Cl1 | 68.80 (10) | P2—C31—C32—C33 | 178.9 (2) |
P2—P1—Pt—Cl1 | −177.96 (3) | C31—C32—C33—C34 | −1.9 (4) |
N1—P2—Pt—P1 | 0.74 (9) | C32—C33—C34—C35 | 0.4 (5) |
C41—P2—Pt—P1 | 113.85 (12) | C33—C34—C35—C36 | 1.1 (4) |
C31—P2—Pt—P1 | −116.32 (11) | C34—C35—C36—C31 | −1.1 (4) |
N1—P2—Pt—Cl1 | 9.15 (15) | C32—C31—C36—C35 | −0.4 (4) |
C41—P2—Pt—Cl1 | 122.27 (15) | P2—C31—C36—C35 | −177.4 (2) |
C31—P2—Pt—Cl1 | −107.90 (14) | N1—P2—C41—C46 | −150.9 (2) |
P1—P2—Pt—Cl1 | 8.41 (11) | C31—P2—C41—C46 | −32.3 (3) |
N1—P2—Pt—Cl2 | −174.28 (9) | Pt—P2—C41—C46 | 103.3 (2) |
C41—P2—Pt—Cl2 | −61.16 (12) | P1—P2—C41—C46 | 169.10 (19) |
C31—P2—Pt—Cl2 | 68.67 (11) | N1—P2—C41—C42 | 29.1 (3) |
P1—P2—Pt—Cl2 | −175.02 (3) | C31—P2—C41—C42 | 147.7 (2) |
P2—N1—C1—C2 | 96.3 (3) | Pt—P2—C41—C42 | −76.7 (2) |
P1—N1—C1—C2 | −97.7 (3) | P1—P2—C41—C42 | −10.9 (3) |
N1—C1—C2—C3 | 172.2 (2) | C46—C41—C42—C43 | 1.1 (4) |
N1—P1—C11—C12 | 78.3 (3) | P2—C41—C42—C43 | −178.8 (2) |
C21—P1—C11—C12 | −39.7 (3) | C41—C42—C43—C44 | 0.7 (4) |
Pt—P1—C11—C12 | −178.1 (2) | C42—C43—C44—C45 | −2.1 (4) |
P2—P1—C11—C12 | 120.1 (2) | C43—C44—C45—C46 | 1.7 (5) |
N1—P1—C11—C16 | −95.8 (2) | C44—C45—C46—C41 | 0.2 (5) |
C21—P1—C11—C16 | 146.2 (2) | C42—C41—C46—C45 | −1.6 (4) |
Pt—P1—C11—C16 | 7.9 (3) | P2—C41—C46—C45 | 178.4 (2) |
P2—P1—C11—C16 | −54.0 (3) |
D—H···A | D—H | H···A | D···A | D—H···A |
C1—H1A···Cl1i | 0.99 | 2.64 | 3.512 (3) | 147 |
Symmetry code: (i) x+1/2, −y+1/2, z−1/2. |
Experimental details
Crystal data | |
Chemical formula | [PtCl2(C27H27NP2)] |
Mr | 693.43 |
Crystal system, space group | Monoclinic, P21/n |
Temperature (K) | 101 |
a, b, c (Å) | 10.6301 (4), 18.8117 (7), 12.7653 (5) |
β (°) | 97.326 (1) |
V (Å3) | 2531.84 (17) |
Z | 4 |
Radiation type | Mo Kα |
µ (mm−1) | 5.90 |
Crystal size (mm) | 0.38 × 0.10 × 0.02 |
Data collection | |
Diffractometer | Bruker X8 APEXII Kappa CCD diffractometer |
Absorption correction | Multi-scan (SADABS; Bruker, 2001) |
Tmin, Tmax | 0.213, 0.891 |
No. of measured, independent and observed [I > 2σ(I)] reflections | 50743, 6276, 5347 |
Rint | 0.052 |
(sin θ/λ)max (Å−1) | 0.667 |
Refinement | |
R[F2 > 2σ(F2)], wR(F2), S | 0.022, 0.053, 1.04 |
No. of reflections | 6276 |
No. of parameters | 298 |
H-atom treatment | H-atom parameters constrained |
Δρmax, Δρmin (e Å−3) | 1.55, −0.63 |
Computer programs: APEX2 (Bruker, 2007), SAINT-Plus (Bruker, 2007), SIR97 (Altomare et al., 1999), SHELXL97 (Sheldrick, 2008), DIAMOND (Brandenburg & Putz, 1999), WinGX (Farrugia, 1999).
D—H···A | D—H | H···A | D···A | D—H···A |
C1—H1A···Cl1i | 0.99 | 2.64 | 3.512 (3) | 147.1 |
Symmetry code: (i) x+1/2, −y+1/2, z−1/2. |
In the title compound (Fig. 1 and Table 1), all bond distances and angles are considered to be normal and fall within range reported for similar complexes (Browning et al., 1992; Fei et al., 2006; Calabrò et al., 2004). The square-planar geometry of the complex is highly distorted with a P1—Pt—P2 bite angle of 72.40 (3)° and a Cl1—Pt—Cl2 angle of 92.7 (1). The reported P1—Pt—P2 small bite angle forces the P1—N1—P2 angle to 100.1 (1)° which illustrates the distorted geometry from the ideal tetrahedral geometry of the N atom. The distance between the N1 atom and the plane created by C1, P1 and P2 is 0.093 (2) Å. The P atoms are also severely distorted from the expected tetrahedral configuration with Pt—P1—N1 and Pt—P2—N1 angles being 94.0 (1) and 93.5 (1)°, respectively. The molecules of the title compound pack horizontal rows in the unit cell across the bc plane (Fig. 2). Intermolecular hydrogen bond exists between C1—H1A and Cl1(1/2+x, 1/2-y, -1/2+z) (Table 2).