Supporting information
Crystallographic Information File (CIF) https://doi.org/10.1107/S1600536804023104/lh6276sup1.cif | |
Structure factor file (CIF format) https://doi.org/10.1107/S1600536804023104/lh6276Isup2.hkl |
CCDC reference: 252955
Key indicators
- Single-crystal X-ray study
- T = 293 K
- Mean (C-C) = 0.013 Å
- R factor = 0.053
- wR factor = 0.152
- Data-to-parameter ratio = 20.6
checkCIF/PLATON results
No syntax errors found
Alert level A REFI017_ALERT_1_A _refine_diff_density_max is missing Maximum value of final difference map (e A-3). The following tests will not be performed DIFMN_01,DIFMX_01,DIFMX_02 REFI018_ALERT_1_A _refine_diff_density_min is missing Minimum value of final difference map (e A-3). The following tests will not be performed DIFMN_01,DIFMN_02,DIFMN_03 PLAT027_ALERT_3_A _diffrn_reflns_theta_full (too) Low ............ 0.00 Deg. PLAT029_ALERT_3_A _diffrn_measured_fraction_theta_full Low ....... 0.00 PLAT037_ALERT_1_A _diffrn_reflns_theta_full .......... Not Given . ? PLAT038_ALERT_1_A _diffrn_measured_fraction_theta_max Not Given . ? PLAT039_ALERT_1_A _diffrn_measured_fraction_theta_full Not Given . ? PLAT095_ALERT_1_A No Residual Density Maximum Given .............. ? PLAT096_ALERT_1_A No Residual Density Minimum Given .............. ?
Alert level C PLAT042_ALERT_1_C Calc. and Rep. MoietyFormula Strings Differ .... ? PLAT241_ALERT_2_C Check High U(eq) as Compared to Neighbors for C11 PLAT241_ALERT_2_C Check High U(eq) as Compared to Neighbors for Se1 PLAT242_ALERT_2_C Check Low U(eq) as Compared to Neighbors for Pd PLAT342_ALERT_3_C Low Bond Precision on C-C bonds (x 1000) Ang ... 13
Alert level G REFLT03_ALERT_1_G ALERT: Expected hkl max differ from CIF values From the CIF: _diffrn_reflns_theta_max 27.50 From the CIF: _reflns_number_total 5698 From the CIF: _diffrn_reflns_limit_ max hkl 1. 14. 16. From the CIF: _diffrn_reflns_limit_ min hkl -12. -14. -16. TEST1: Expected hkl limits for theta max Calculated maximum hkl 12. 16. 16. Calculated minimum hkl -12. -16. -16.
9 ALERT level A = In general: serious problem 0 ALERT level B = Potentially serious problem 5 ALERT level C = Check and explain 1 ALERT level G = General alerts; check 9 ALERT type 1 CIF construction/syntax error, inconsistent or missing data 3 ALERT type 2 Indicator that the structure model may be wrong or deficient 3 ALERT type 3 Indicator that the structure quality may be low 0 ALERT type 4 Improvement, methodology, query or suggestion
Data collection: XSCANS (Siemens, 1991-1996); cell refinement: XSCANS; data reduction: SHELXTL (Bruker, 2000); program(s) used to solve structure: SHELXTL; program(s) used to refine structure: SHELXTL; molecular graphics: SHELXTL; software used to prepare material for publication: SHELXTL.
(C24H20P)2[PdMo2Se8] | Z = 1 |
Mr = 1608.70 | F(000) = 760 |
Triclinic, P1 | Dx = 2.064 Mg m−3 |
Hall symbol: -P 1 | Mo Kα radiation, λ = 0.71073 Å |
a = 9.4976 (9) Å | Cell parameters from 26 reflections |
b = 12.5798 (16) Å | θ = 6.5–40.9° |
c = 12.622 (3) Å | µ = 6.54 mm−1 |
α = 66.096 (13)° | T = 293 K |
β = 84.511 (13)° | Flake/arrowhead, black |
γ = 70.047 (9)° | 0.48 × 0.42 × 0.36 mm |
V = 1294.3 (4) Å3 |
Siemens P4 diffractometer | 3974 reflections with I > 2σ(I) |
Radiation source: fine-focus sealed tube | Rint = 0.030 |
Graphite monochromator | θmax = 27.5°, θmin = 1.8° |
2θ/ω scans | h = −12→1 |
Absorption correction: ψ scan (SHELXTL; Bruker, 2000) | k = −14→14 |
Tmin = 0.058, Tmax = 0.095 | l = −16→16 |
6737 measured reflections | 3 standard reflections every 50 reflections |
5698 independent reflections | intensity decay: none |
Refinement on F2 | 0 restraints |
Least-squares matrix: full | Primary atom site location: structure-invariant direct methods |
R[F2 > 2σ(F2)] = 0.053 | Secondary atom site location: difference Fourier map |
wR(F2) = 0.152 | Hydrogen site location: inferred from neighbouring sites |
S = 1.02 | H-atom parameters not refined |
5698 reflections | w = 1/[σ2(Fo2) + (0.0733P)2 + 3.8281P] where P = (Fo2 + 2Fc2)/3 |
277 parameters | (Δ/σ)max < 0.001 |
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. |
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 | ||
Pd | 0.5000 | 1.0000 | 0.5000 | 0.04141 (19) | |
Mo | 0.59122 (8) | 0.73359 (6) | 0.63255 (6) | 0.04971 (19) | |
Se1 | 0.75179 (9) | 0.85259 (8) | 0.57127 (9) | 0.0674 (3) | |
Se2 | 0.34324 (9) | 0.87305 (7) | 0.59939 (7) | 0.0544 (2) | |
Se3 | 0.62285 (11) | 0.61955 (8) | 0.52642 (8) | 0.0625 (2) | |
Se4 | 0.63823 (15) | 0.60700 (10) | 0.82382 (8) | 0.0866 (4) | |
P | 0.9099 (2) | 0.75393 (16) | 0.16666 (15) | 0.0390 (4) | |
C1 | 0.8624 (8) | 0.6184 (6) | 0.2538 (6) | 0.0428 (15) | |
C2 | 0.7294 (8) | 0.6092 (7) | 0.2236 (7) | 0.0516 (17) | |
H2A | 0.6659 | 0.6737 | 0.1624 | 0.062* | |
C3 | 0.6946 (10) | 0.5043 (8) | 0.2852 (7) | 0.059 (2) | |
H3A | 0.6079 | 0.4971 | 0.2646 | 0.071* | |
C4 | 0.7844 (11) | 0.4112 (8) | 0.3757 (7) | 0.061 (2) | |
H4A | 0.7579 | 0.3412 | 0.4173 | 0.073* | |
C5 | 0.9157 (11) | 0.4185 (7) | 0.4075 (7) | 0.062 (2) | |
H5A | 0.9777 | 0.3531 | 0.4690 | 0.074* | |
C6 | 0.9541 (8) | 0.5245 (7) | 0.3466 (6) | 0.0502 (17) | |
H6A | 1.0403 | 0.5315 | 0.3683 | 0.060* | |
C7 | 0.9875 (8) | 0.7419 (6) | 0.0350 (6) | 0.0439 (15) | |
C8 | 1.0918 (10) | 0.7974 (8) | −0.0191 (7) | 0.060 (2) | |
H8A | 1.1244 | 0.8397 | 0.0137 | 0.072* | |
C9 | 1.1483 (11) | 0.7906 (9) | −0.1219 (8) | 0.072 (3) | |
H9A | 1.2206 | 0.8267 | −0.1568 | 0.086* | |
C10 | 1.1001 (12) | 0.7327 (10) | −0.1718 (8) | 0.078 (3) | |
H10A | 1.1397 | 0.7283 | −0.2408 | 0.094* | |
C11 | 0.9929 (14) | 0.6800 (11) | −0.1218 (9) | 0.088 (3) | |
H11A | 0.9558 | 0.6441 | −0.1594 | 0.106* | |
C12 | 0.9400 (10) | 0.6796 (8) | −0.0170 (7) | 0.062 (2) | |
H12A | 0.8728 | 0.6383 | 0.0195 | 0.075* | |
C13 | 1.0461 (8) | 0.7751 (6) | 0.2409 (6) | 0.0424 (15) | |
C14 | 1.1928 (9) | 0.6983 (7) | 0.2564 (7) | 0.0520 (17) | |
H14A | 1.2211 | 0.6338 | 0.2319 | 0.062* | |
C15 | 1.2984 (9) | 0.7179 (9) | 0.3089 (7) | 0.061 (2) | |
H15A | 1.3973 | 0.6653 | 0.3215 | 0.073* | |
C16 | 1.2558 (10) | 0.8150 (9) | 0.3419 (7) | 0.062 (2) | |
H16A | 1.3271 | 0.8299 | 0.3745 | 0.075* | |
C17 | 1.1097 (11) | 0.8905 (9) | 0.3274 (8) | 0.069 (2) | |
H17A | 1.0817 | 0.9555 | 0.3512 | 0.083* | |
C18 | 1.0026 (10) | 0.8698 (8) | 0.2770 (7) | 0.059 (2) | |
H18A | 0.9028 | 0.9200 | 0.2680 | 0.071* | |
C19 | 0.7445 (7) | 0.8866 (6) | 0.1334 (6) | 0.0413 (15) | |
C20 | 0.7230 (8) | 0.9846 (7) | 0.0241 (6) | 0.0467 (16) | |
H20A | 0.7874 | 0.9773 | −0.0347 | 0.056* | |
C21 | 0.6041 (10) | 1.0924 (7) | 0.0053 (8) | 0.061 (2) | |
H21A | 0.5888 | 1.1585 | −0.0664 | 0.073* | |
C22 | 0.5080 (9) | 1.1020 (8) | 0.0931 (8) | 0.062 (2) | |
H22A | 0.4289 | 1.1749 | 0.0800 | 0.074* | |
C23 | 0.5280 (9) | 1.0060 (8) | 0.1981 (7) | 0.057 (2) | |
H23A | 0.4611 | 1.0135 | 0.2556 | 0.068* | |
C24 | 0.6451 (9) | 0.8985 (7) | 0.2204 (6) | 0.0514 (17) | |
H24A | 0.6587 | 0.8338 | 0.2929 | 0.062* |
U11 | U22 | U33 | U12 | U13 | U23 | |
Pd | 0.0402 (4) | 0.0422 (4) | 0.0451 (4) | −0.0175 (3) | 0.0070 (3) | −0.0184 (3) |
Mo | 0.0529 (4) | 0.0469 (4) | 0.0510 (4) | −0.0189 (3) | 0.0027 (3) | −0.0193 (3) |
Se1 | 0.0429 (5) | 0.0543 (5) | 0.0966 (7) | −0.0168 (4) | −0.0012 (4) | −0.0205 (5) |
Se2 | 0.0482 (4) | 0.0545 (5) | 0.0656 (5) | −0.0258 (4) | 0.0158 (4) | −0.0245 (4) |
Se3 | 0.0689 (6) | 0.0581 (5) | 0.0620 (5) | −0.0152 (4) | 0.0019 (4) | −0.0300 (4) |
Se4 | 0.1292 (10) | 0.0720 (6) | 0.0548 (5) | −0.0350 (6) | −0.0064 (6) | −0.0180 (5) |
P | 0.0392 (9) | 0.0408 (9) | 0.0395 (9) | −0.0177 (7) | 0.0039 (7) | −0.0154 (7) |
C1 | 0.042 (4) | 0.037 (3) | 0.051 (4) | −0.016 (3) | 0.012 (3) | −0.019 (3) |
C2 | 0.045 (4) | 0.054 (4) | 0.058 (4) | −0.023 (3) | 0.008 (3) | −0.020 (4) |
C3 | 0.058 (5) | 0.065 (5) | 0.068 (5) | −0.036 (4) | 0.018 (4) | −0.030 (4) |
C4 | 0.079 (6) | 0.054 (5) | 0.061 (5) | −0.034 (5) | 0.027 (4) | −0.028 (4) |
C5 | 0.078 (6) | 0.040 (4) | 0.052 (4) | −0.010 (4) | 0.010 (4) | −0.012 (3) |
C6 | 0.046 (4) | 0.052 (4) | 0.050 (4) | −0.015 (3) | 0.006 (3) | −0.019 (3) |
C7 | 0.046 (4) | 0.043 (4) | 0.047 (4) | −0.018 (3) | 0.008 (3) | −0.021 (3) |
C8 | 0.075 (6) | 0.074 (5) | 0.057 (4) | −0.052 (5) | 0.024 (4) | −0.034 (4) |
C9 | 0.081 (6) | 0.091 (7) | 0.064 (5) | −0.046 (6) | 0.033 (5) | −0.043 (5) |
C10 | 0.104 (8) | 0.089 (7) | 0.069 (6) | −0.052 (6) | 0.040 (6) | −0.049 (5) |
C11 | 0.128 (10) | 0.106 (8) | 0.075 (6) | −0.074 (8) | 0.026 (6) | −0.056 (6) |
C12 | 0.069 (6) | 0.079 (6) | 0.064 (5) | −0.045 (5) | 0.016 (4) | −0.039 (5) |
C13 | 0.046 (4) | 0.046 (4) | 0.039 (3) | −0.023 (3) | 0.005 (3) | −0.014 (3) |
C14 | 0.049 (4) | 0.052 (4) | 0.058 (4) | −0.021 (4) | 0.002 (3) | −0.020 (4) |
C15 | 0.048 (5) | 0.073 (6) | 0.060 (5) | −0.026 (4) | −0.006 (4) | −0.018 (4) |
C16 | 0.063 (5) | 0.076 (6) | 0.055 (5) | −0.037 (5) | −0.004 (4) | −0.019 (4) |
C17 | 0.077 (6) | 0.067 (6) | 0.080 (6) | −0.021 (5) | −0.015 (5) | −0.043 (5) |
C18 | 0.057 (5) | 0.065 (5) | 0.069 (5) | −0.020 (4) | −0.006 (4) | −0.038 (4) |
C19 | 0.038 (4) | 0.045 (4) | 0.049 (4) | −0.018 (3) | 0.002 (3) | −0.023 (3) |
C20 | 0.046 (4) | 0.050 (4) | 0.045 (4) | −0.024 (3) | 0.003 (3) | −0.014 (3) |
C21 | 0.062 (5) | 0.037 (4) | 0.075 (5) | −0.016 (4) | −0.022 (4) | −0.008 (4) |
C22 | 0.050 (5) | 0.054 (5) | 0.091 (6) | −0.008 (4) | −0.008 (4) | −0.041 (5) |
C23 | 0.045 (4) | 0.070 (5) | 0.065 (5) | −0.011 (4) | 0.001 (4) | −0.042 (4) |
C24 | 0.055 (5) | 0.054 (4) | 0.048 (4) | −0.021 (4) | 0.010 (3) | −0.022 (3) |
Pd—Se2 | 2.4459 (8) | C9—C10 | 1.338 (13) |
Pd—Se2i | 2.4459 (8) | C9—H9A | 0.9300 |
Pd—Se1 | 2.4495 (9) | C10—C11 | 1.369 (14) |
Pd—Se1i | 2.4495 (9) | C10—H10A | 0.9300 |
Pd—Mo | 2.9212 (9) | C11—C12 | 1.368 (12) |
Pd—Moi | 2.9212 (9) | C11—H11A | 0.9300 |
Mo—Se3 | 2.2647 (11) | C12—H12A | 0.9300 |
Mo—Se4 | 2.2735 (13) | C13—C18 | 1.366 (10) |
Mo—Se1 | 2.3578 (11) | C13—C14 | 1.376 (11) |
Mo—Se2 | 2.3608 (11) | C14—C15 | 1.391 (11) |
P—C19 | 1.789 (7) | C14—H14A | 0.9300 |
P—C7 | 1.795 (7) | C15—C16 | 1.368 (13) |
P—C1 | 1.797 (7) | C15—H15A | 0.9300 |
P—C13 | 1.814 (7) | C16—C17 | 1.368 (13) |
C1—C6 | 1.378 (10) | C16—H16A | 0.9300 |
C1—C2 | 1.408 (10) | C17—C18 | 1.394 (11) |
C2—C3 | 1.368 (11) | C17—H17A | 0.9300 |
C2—H2A | 0.9300 | C18—H18A | 0.9300 |
C3—C4 | 1.351 (12) | C19—C24 | 1.398 (10) |
C3—H3A | 0.9300 | C19—C20 | 1.404 (10) |
C4—C5 | 1.389 (13) | C20—C21 | 1.383 (11) |
C4—H4A | 0.9300 | C20—H20A | 0.9300 |
C5—C6 | 1.397 (11) | C21—C22 | 1.384 (13) |
C5—H5A | 0.9300 | C21—H21A | 0.9300 |
C6—H6A | 0.9300 | C22—C23 | 1.358 (12) |
C7—C8 | 1.375 (10) | C22—H22A | 0.9300 |
C7—C12 | 1.401 (10) | C23—C24 | 1.368 (11) |
C8—C9 | 1.380 (11) | C23—H23A | 0.9300 |
C8—H8A | 0.9300 | C24—H24A | 0.9300 |
Se2—Pd—Se2i | 180.000 (1) | C12—C7—P | 121.0 (6) |
Se2—Pd—Se1 | 101.53 (3) | C7—C8—C9 | 120.2 (8) |
Se2i—Pd—Se1 | 78.47 (3) | C7—C8—H8A | 119.9 |
Se2—Pd—Se1i | 78.47 (3) | C9—C8—H8A | 119.9 |
Se2i—Pd—Se1i | 101.53 (3) | C10—C9—C8 | 120.7 (8) |
Se1—Pd—Se1i | 180.000 (1) | C10—C9—H9A | 119.6 |
Se2—Pd—Mo | 51.26 (3) | C8—C9—H9A | 119.6 |
Se2i—Pd—Mo | 128.74 (3) | C9—C10—C11 | 120.4 (8) |
Se1—Pd—Mo | 51.17 (3) | C9—C10—H10A | 119.8 |
Se1i—Pd—Mo | 128.83 (3) | C11—C10—H10A | 119.8 |
Se2—Pd—Moi | 128.74 (3) | C12—C11—C10 | 120.4 (9) |
Se2i—Pd—Moi | 51.26 (3) | C12—C11—H11A | 119.8 |
Se1—Pd—Moi | 128.83 (3) | C10—C11—H11A | 119.8 |
Se1i—Pd—Moi | 51.17 (3) | C11—C12—C7 | 119.6 (8) |
Mo—Pd—Moi | 180.00 (3) | C11—C12—H12A | 120.2 |
Se3—Mo—Se4 | 109.56 (5) | C7—C12—H12A | 120.2 |
Se3—Mo—Se1 | 110.01 (5) | C18—C13—C14 | 120.9 (7) |
Se4—Mo—Se1 | 110.63 (5) | C18—C13—P | 119.5 (6) |
Se3—Mo—Se2 | 109.11 (4) | C14—C13—P | 119.6 (6) |
Se4—Mo—Se2 | 110.55 (5) | C13—C14—C15 | 119.5 (8) |
Se1—Mo—Se2 | 106.95 (4) | C13—C14—H14A | 120.2 |
Se3—Mo—Pd | 115.45 (4) | C15—C14—H14A | 120.2 |
Se4—Mo—Pd | 134.98 (4) | C16—C15—C14 | 119.6 (8) |
Se1—Mo—Pd | 54.02 (3) | C16—C15—H15A | 120.2 |
Se2—Mo—Pd | 53.91 (3) | C14—C15—H15A | 120.2 |
Mo—Se1—Pd | 74.81 (3) | C17—C16—C15 | 120.8 (8) |
Mo—Se2—Pd | 74.83 (3) | C17—C16—H16A | 119.6 |
C19—P—C7 | 109.9 (3) | C15—C16—H16A | 119.6 |
C19—P—C1 | 109.1 (3) | C16—C17—C18 | 119.9 (8) |
C7—P—C1 | 109.5 (3) | C16—C17—H17A | 120.1 |
C19—P—C13 | 107.8 (3) | C18—C17—H17A | 120.1 |
C7—P—C13 | 108.3 (3) | C13—C18—C17 | 119.3 (8) |
C1—P—C13 | 112.2 (3) | C13—C18—H18A | 120.3 |
C6—C1—C2 | 120.4 (7) | C17—C18—H18A | 120.3 |
C6—C1—P | 121.4 (6) | C24—C19—C20 | 119.8 (7) |
C2—C1—P | 118.2 (6) | C24—C19—P | 119.8 (6) |
C3—C2—C1 | 119.2 (8) | C20—C19—P | 119.9 (5) |
C3—C2—H2A | 120.4 | C21—C20—C19 | 118.8 (7) |
C1—C2—H2A | 120.4 | C21—C20—H20A | 120.6 |
C4—C3—C2 | 120.9 (8) | C19—C20—H20A | 120.6 |
C4—C3—H3A | 119.6 | C20—C21—C22 | 120.1 (8) |
C2—C3—H3A | 119.6 | C20—C21—H21A | 119.9 |
C3—C4—C5 | 120.9 (8) | C22—C21—H21A | 119.9 |
C3—C4—H4A | 119.6 | C23—C22—C21 | 120.7 (8) |
C5—C4—H4A | 119.6 | C23—C22—H22A | 119.6 |
C4—C5—C6 | 119.6 (8) | C21—C22—H22A | 119.6 |
C4—C5—H5A | 120.2 | C22—C23—C24 | 120.8 (8) |
C6—C5—H5A | 120.2 | C22—C23—H23A | 119.6 |
C1—C6—C5 | 118.9 (8) | C24—C23—H23A | 119.6 |
C1—C6—H6A | 120.5 | C23—C24—C19 | 119.6 (7) |
C5—C6—H6A | 120.5 | C23—C24—H24A | 120.2 |
C8—C7—C12 | 118.5 (7) | C19—C24—H24A | 120.2 |
C8—C7—P | 120.4 (6) |
Symmetry code: (i) −x+1, −y+2, −z+1. |
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