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In the crystal structure of the title compound, [Pd(C17H28N4S2)](BF4)2, the PdII atom is coordinated by one N atom from each of the pyrazolyl groups and the two thio­ether S atoms in a slightly distorted square-planar geometry.

Supporting information

cif

Crystallographic Information File (CIF) https://doi.org/10.1107/S1600536804016022/cv6321sup1.cif
Contains datablocks I, global

hkl

Structure factor file (CIF format) https://doi.org/10.1107/S1600536804016022/cv6321Isup2.hkl
Contains datablock I

CCDC reference: 248723

Key indicators

  • Single-crystal X-ray study
  • T = 293 K
  • Mean [sigma](C-C) = 0.008 Å
  • Disorder in solvent or counterion
  • R factor = 0.035
  • wR factor = 0.060
  • Data-to-parameter ratio = 18.2

checkCIF/PLATON results

No syntax errors found



Alert level A PLAT029_ALERT_3_A _diffrn_measured_fraction_theta_full Low ....... 0.91
Author Response: The non-measured intensities are due to the dark zone of MAR345 diffractometer

Alert level B PLAT026_ALERT_3_B Ratio Observed / Unique Reflections too Low .... 37 Perc.
Alert level C REFLT03_ALERT_3_C Reflection count < 95% complete From the CIF: _diffrn_reflns_theta_max 30.00 From the CIF: _diffrn_reflns_theta_full 0.00 From the CIF: _reflns_number_total 6465 TEST2: Reflns within _diffrn_reflns_theta_max Count of symmetry unique reflns 7090 Completeness (_total/calc) 91.18% PLAT042_ALERT_1_C Calc. and Rep. MoietyFormula Strings Differ .... ? PLAT302_ALERT_4_C Anion/Solvent Disorder ......................... 29.00 Perc. PLAT362_ALERT_2_C Short C(sp3)-C(sp2) Bond C11 - C12 ... 1.36 Ang. PLAT432_ALERT_2_C Short Inter X...Y Contact F5' .. C4 .. 2.92 Ang. PLAT779_ALERT_2_C Suspect or Irrelevant (Bond) Angle in CIF ...... 31.10 Deg. F5 -B2 -F5' 1.555 1.555 1.555 PLAT779_ALERT_2_C Suspect or Irrelevant (Bond) Angle in CIF ...... 40.00 Deg. F7 -B2 -F7' 1.555 1.555 1.555 PLAT779_ALERT_2_C Suspect or Irrelevant (Bond) Angle in CIF ...... 42.50 Deg. F6 -B2 -F6' 1.555 1.555 1.555 PLAT779_ALERT_2_C Suspect or Irrelevant (Bond) Angle in CIF ...... 29.50 Deg. F8' -B2 -F8 1.555 1.555 1.555 PLAT790_ALERT_4_C Centre of Gravity not Within Unit Cell: Resd. # 3 B F4
1 ALERT level A = In general: serious problem 1 ALERT level B = Potentially serious problem 10 ALERT level C = Check and explain 0 ALERT level G = General alerts; check 1 ALERT type 1 CIF construction/syntax error, inconsistent or missing data 6 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 2 ALERT type 4 Improvement, methodology, query or suggestion

Computing details top

Data collection: MARXDS (Klein, 2000); cell refinement: MARXDS; data reduction: MARSCALE (Klein, 1998); program(s) used to solve structure: SHELXS97 (Sheldrick, 1998); program(s) used to refine structure: SHELXL97 (Sheldrick, 1998); molecular graphics: ORTEP-3 (Farrugia, (2003); software used to prepare material for publication: CIFTABS (Sheldrick, 1998).

[1,9-Bis(3,5-dimethylpyrazol-1-yl-κN2)-3,7-dithianonane- κ2S,S']palladate(II) bis(tetrafluoroborate) top
Crystal data top
[Pd(C17H28N4S2)](BF4)2F(000) = 1272
Mr = 632.57Dx = 1.731 Mg m3
Monoclinic, P21/cMo Kα radiation, λ = 0.71069 Å
Hall symbol: -P 2ybcCell parameters from 8324 reflections
a = 11.759 (1) Åθ = 2.9–30.0°
b = 18.650 (1) ŵ = 1.01 mm1
c = 11.880 (1) ÅT = 293 K
β = 111.29 (2)°Prism, yellow
V = 2427.5 (5) Å30.20 × 0.07 × 0.07 mm
Z = 4
Data collection top
MAR345 with image-plate detector
diffractometer
2400 reflections with I > 2σ(I)
Radiation source: fine-focus sealed tubeRint = 0.093
Graphite monochromatorθmax = 30.0°, θmin = 2.9°
φ scansh = 1515
9639 measured reflectionsk = 026
6465 independent reflectionsl = 015
Refinement top
Refinement on F2Primary atom site location: structure-invariant direct methods
Least-squares matrix: fullSecondary atom site location: difference Fourier map
R[F2 > 2σ(F2)] = 0.035Hydrogen site location: inferred from neighbouring sites
wR(F2) = 0.060H atoms treated by a mixture of independent and constrained refinement
S = 1.15 w = 1/[σ2(Fo2) + (0.0062P)2]
where P = (Fo2 + 2Fc2)/3
5502 reflections(Δ/σ)max < 0.001
303 parametersΔρmax = 0.59 e Å3
259 restraintsΔρmin = 0.71 e Å3
Fractional atomic coordinates and isotropic or equivalent isotropic displacement parameters (Å2) top
xyzUiso*/UeqOcc. (<1)
Pd0.26189 (4)0.02442 (2)0.72402 (4)0.06044 (13)
S10.31289 (13)0.03276 (10)0.90495 (12)0.0784 (4)
S20.11754 (13)0.05896 (9)0.62420 (13)0.0743 (4)
N10.2134 (3)0.0473 (2)0.4601 (4)0.0486 (11)
N20.2105 (3)0.0788 (2)0.5661 (3)0.0545 (10)
N30.3936 (4)0.0981 (2)0.8150 (3)0.0516 (11)
N40.3882 (5)0.1318 (3)0.9097 (4)0.0616 (16)
C10.1776 (4)0.0796 (3)0.8950 (4)0.0641 (15)
H10.18180.09110.97610.077*
H1A0.10820.04800.85920.077*
C20.1559 (4)0.1476 (3)0.8224 (5)0.0663 (15)
H20.21170.18380.87070.080*
H2A0.07370.16400.80920.080*
C30.1701 (4)0.1440 (3)0.7027 (4)0.0691 (15)
H30.12440.18290.65230.083*
H3A0.25550.15060.71440.083*
C40.1460 (5)0.0739 (4)0.4824 (5)0.063 (2)
H40.16840.12380.48020.077*
H4A0.06980.06630.41510.077*
C50.2448 (4)0.0271 (3)0.4619 (4)0.0655 (14)
H50.32290.03570.52600.079*
H5A0.25230.04000.38580.079*
C60.1830 (4)0.0945 (3)0.3731 (4)0.0517 (12)
C70.1712 (5)0.0756 (3)0.2477 (4)0.0703 (17)
H70.18890.02560.24400.085*
H7A0.22760.10360.22460.085*
H7B0.08950.08530.19350.085*
C80.1671 (5)0.1592 (3)0.4166 (4)0.0685 (15)
H80.14970.20240.37480.082*
C90.1823 (4)0.1473 (3)0.5393 (4)0.0638 (12)
C100.1750 (6)0.2004 (3)0.6356 (5)0.100 (2)
H100.19050.17550.71040.120*
H10A0.09510.22150.60930.120*
H10B0.23500.23750.64720.120*
C110.4958 (7)0.1212 (4)0.7859 (6)0.083 (3)
C120.5194 (7)0.0910 (3)0.6925 (6)0.106 (3)
H120.44990.06370.64340.120*
H12A0.58900.06000.72370.120*
H12B0.53610.12800.64450.120*
C130.5462 (3)0.1728 (2)0.8783 (3)0.0674 (9)
H130.61680.19890.88880.080*
C140.4772 (5)0.1798 (3)0.9517 (4)0.0677 (13)
C150.5044 (5)0.2287 (3)1.0492 (4)0.0792 (18)
H150.44500.22391.08680.095*
H15A0.50250.27681.01970.095*
H15B0.58420.21861.10740.095*
C160.3028 (8)0.1125 (5)0.9642 (7)0.082 (3)
H160.22080.11840.90540.101*
H16A0.31210.14481.03090.101*
C170.3182 (5)0.0352 (4)1.0111 (5)0.094 (2)
H170.25470.02551.04310.112*
H17A0.39590.03171.07780.112*
B10.5016 (7)0.1252 (5)0.6662 (7)0.105 (3)
F10.4004 (3)0.1633 (2)0.5977 (3)0.1020 (12)
F20.4738 (3)0.0860 (2)0.7485 (3)0.1038 (12)
F30.5362 (3)0.0815 (2)0.5920 (3)0.1045 (11)
F40.5930 (3)0.1724 (2)0.7255 (3)0.1044 (12)
B20.9512 (6)0.1359 (4)0.8436 (7)0.105 (3)
F51.0261 (7)0.0812 (4)0.8412 (8)0.110 (3)*0.50
F60.9904 (6)0.1706 (4)0.9493 (6)0.103 (2)*0.50
F70.9384 (7)0.1835 (4)0.7536 (7)0.108 (3)*0.50
F80.8390 (6)0.1024 (5)0.8256 (7)0.098 (3)*0.50
F5'0.9865 (8)0.0859 (4)0.7779 (7)0.108 (3)*0.50
F7'0.9973 (7)0.2005 (4)0.8249 (8)0.115 (3)*0.50
F8'0.8292 (6)0.1387 (5)0.8095 (7)0.112 (3)*0.50
F6'1.0071 (6)0.1190 (5)0.9645 (6)0.109 (3)*0.50
Atomic displacement parameters (Å2) top
U11U22U33U12U13U23
Pd0.06212 (19)0.0546 (3)0.0548 (2)0.0005 (3)0.00957 (14)0.0001 (3)
S10.0832 (9)0.0729 (12)0.0659 (8)0.0065 (9)0.0114 (7)0.0063 (9)
S20.0729 (9)0.0599 (11)0.0727 (9)0.0038 (7)0.0057 (7)0.0040 (8)
N10.045 (2)0.039 (3)0.061 (3)0.0105 (17)0.0195 (18)0.0076 (19)
N20.060 (2)0.051 (3)0.056 (2)0.005 (2)0.0242 (18)0.003 (2)
N30.078 (3)0.053 (3)0.0495 (17)0.020 (2)0.022 (2)0.0145 (18)
N40.071 (4)0.061 (5)0.047 (2)0.009 (4)0.019 (2)0.011 (2)
C10.069 (3)0.082 (5)0.045 (3)0.009 (3)0.027 (2)0.023 (3)
C20.054 (3)0.074 (4)0.085 (4)0.010 (3)0.042 (3)0.004 (3)
C30.065 (3)0.063 (4)0.070 (3)0.010 (3)0.014 (2)0.000 (3)
C40.051 (5)0.056 (5)0.054 (4)0.008 (4)0.003 (3)0.016 (4)
C50.058 (3)0.081 (4)0.048 (3)0.002 (4)0.0084 (19)0.000 (4)
C60.068 (3)0.058 (4)0.034 (2)0.001 (3)0.025 (2)0.003 (2)
C70.072 (4)0.063 (4)0.061 (3)0.017 (3)0.011 (3)0.005 (3)
C80.068 (3)0.071 (4)0.066 (3)0.004 (3)0.024 (3)0.000 (3)
C90.067 (3)0.072 (3)0.075 (2)0.014 (2)0.044 (2)0.000 (2)
C100.099 (5)0.071 (5)0.084 (4)0.011 (4)0.020 (3)0.009 (4)
C110.083 (6)0.044 (5)0.076 (5)0.008 (4)0.014 (5)0.013 (4)
C120.095 (6)0.054 (4)0.090 (6)0.017 (4)0.026 (5)0.007 (4)
C130.0758 (15)0.069 (3)0.072 (2)0.0171 (16)0.0301 (15)0.003 (2)
C140.079 (3)0.075 (4)0.076 (2)0.015 (3)0.023 (2)0.008 (2)
C150.107 (5)0.059 (4)0.060 (3)0.004 (4)0.017 (3)0.005 (3)
C160.072 (8)0.078 (7)0.060 (5)0.033 (6)0.012 (5)0.024 (5)
C170.092 (4)0.112 (6)0.073 (4)0.013 (5)0.026 (3)0.002 (4)
B10.116 (7)0.108 (9)0.089 (6)0.002 (6)0.034 (5)0.009 (6)
F10.104 (3)0.095 (3)0.099 (3)0.003 (2)0.028 (2)0.001 (2)
F20.110 (3)0.101 (3)0.097 (3)0.006 (2)0.034 (2)0.000 (2)
F30.100 (3)0.106 (3)0.104 (3)0.006 (2)0.034 (2)0.003 (3)
F40.100 (3)0.099 (3)0.109 (3)0.005 (2)0.031 (2)0.003 (2)
B20.085 (6)0.141 (10)0.088 (6)0.012 (6)0.029 (5)0.011 (7)
Geometric parameters (Å, º) top
Pd—N22.022 (4)C8—C91.420 (6)
Pd—N32.059 (4)C8—H80.9300
Pd—S12.2761 (15)C9—C101.539 (7)
Pd—S22.2900 (16)C10—H100.9600
S1—C171.773 (6)C10—H10A0.9600
S1—C11.781 (5)C10—H10B0.9600
S2—C31.829 (5)C11—C121.360 (10)
S2—C41.854 (6)C11—C131.419 (8)
N1—C61.304 (5)C12—H120.9600
N1—N21.401 (5)C12—H12A0.9600
N1—C51.435 (6)C12—H12B0.9600
N2—C91.330 (6)C13—C141.397 (5)
N3—N41.310 (5)C13—H130.9300
N3—C111.432 (9)C14—C151.417 (6)
N4—C141.330 (7)C15—H150.9600
N4—C161.425 (10)C15—H15A0.9600
C1—C21.503 (7)C15—H15B0.9600
C1—H10.9700C16—C171.532 (9)
C1—H1A0.9700C16—H160.9700
C2—C31.493 (7)C16—H16A0.9700
C2—H20.9700C17—H170.9700
C2—H2A0.9700C17—H17A0.9700
C3—H30.9700B1—F31.366 (8)
C3—H3A0.9700B1—F21.352 (8)
C4—C51.542 (8)B1—F41.370 (8)
C4—H40.9700B1—F11.372 (7)
C4—H4A0.9700B2—F61.337 (8)
C5—H50.9700B2—F51.354 (9)
C5—H5A0.9700B2—F71.356 (8)
C6—C81.351 (6)B2—F81.404 (8)
C6—C71.488 (6)B2—F8'1.343 (8)
C7—H70.9600B2—F5'1.373 (9)
C7—H7A0.9600B2—F7'1.372 (9)
C7—H7B0.9600B2—F6'1.381 (8)
N2—Pd—N393.84 (15)C6—C8—C9105.7 (5)
N2—Pd—S1176.85 (12)C6—C8—H8127.2
N3—Pd—S185.81 (11)C9—C8—H8127.1
N2—Pd—S286.81 (12)N2—C9—C8108.8 (4)
N3—Pd—S2179.10 (12)N2—C9—C10121.1 (4)
S1—Pd—S293.58 (6)C8—C9—C10130.0 (5)
C17—S1—C1101.4 (3)C9—C10—H10109.6
C17—S1—Pd105.4 (2)C9—C10—H10A109.9
C1—S1—Pd104.16 (16)H10—C10—H10A109.5
C3—S2—C4101.2 (3)C9—C10—H10B108.9
C3—S2—Pd105.95 (17)H10—C10—H10B109.5
C4—S2—Pd103.2 (2)H10A—C10—H10B109.5
C6—N1—N2109.9 (4)C12—C11—C13139.5 (8)
C6—N1—C5131.3 (4)C12—C11—N3120.7 (6)
N2—N1—C5118.8 (4)C13—C11—N399.7 (6)
C9—N2—N1105.8 (3)C11—C12—H12110.2
C9—N2—Pd132.0 (3)C11—C12—H12A108.9
N1—N2—Pd121.8 (3)H12—C12—H12A109.5
N4—N3—C11111.7 (5)C11—C12—H12B109.3
N4—N3—Pd120.6 (4)H12—C12—H12B109.5
C11—N3—Pd127.6 (4)H12A—C12—H12B109.5
N3—N4—C14111.6 (5)C14—C13—C11111.9 (5)
N3—N4—C16122.1 (6)C14—C13—H13124.7
C14—N4—C16126.1 (5)C11—C13—H13123.5
C2—C1—S1114.4 (4)N4—C14—C13105.1 (4)
C2—C1—H1108.9N4—C14—C15130.8 (4)
S1—C1—H1108.8C13—C14—C15124.1 (5)
C2—C1—H1A108.3C14—C15—H15109.7
S1—C1—H1A108.6C14—C15—H15A109.5
H1—C1—H1A107.6H15—C15—H15A109.5
C3—C2—C1117.0 (5)C14—C15—H15B109.3
C3—C2—H2107.8H15—C15—H15B109.5
C1—C2—H2107.7H15A—C15—H15B109.5
C3—C2—H2A108.3N4—C16—C17113.2 (6)
C1—C2—H2A108.4N4—C16—H16109.2
H2—C2—H2A107.3C17—C16—H16109.1
C2—C3—S2113.0 (4)N4—C16—H16A108.8
C2—C3—H3108.9C17—C16—H16A108.7
S2—C3—H3109.0H16—C16—H16A107.7
C2—C3—H3A109.1C16—C17—S1116.4 (5)
S2—C3—H3A108.9C16—C17—H17108.2
H3—C3—H3A107.7S1—C17—H17108.0
C5—C4—S2117.0 (4)C16—C17—H17A108.4
C5—C4—H4107.7S1—C17—H17A108.2
S2—C4—H4108.2H17—C17—H17A107.3
C5—C4—H4A108.2F3—B1—F2110.6 (7)
S2—C4—H4A108.2F3—B1—F4110.7 (6)
H4—C4—H4A107.3F2—B1—F4109.1 (6)
N1—C5—C4110.2 (4)F3—B1—F1108.9 (6)
N1—C5—H5109.8F2—B1—F1108.9 (6)
C4—C5—H5109.7F4—B1—F1108.7 (6)
N1—C5—H5A109.2F6—B2—F5112.3 (7)
C4—C5—H5A109.9F6—B2—F7109.0 (7)
H5—C5—H5A108.1F5—B2—F7111.3 (7)
N1—C6—C8109.6 (4)F6—B2—F8110.0 (7)
N1—C6—C7122.2 (5)F5—B2—F8104.2 (7)
C8—C6—C7128.2 (5)F7—B2—F8110.0 (7)
C6—C7—H7109.5F8'—B2—F5'111.4 (7)
C6—C7—H7A109.8F8'—B2—F7'111.0 (8)
H7—C7—H7A109.5F5'—B2—F7'106.6 (7)
C6—C7—H7B109.2F8'—B2—F6'112.1 (7)
H7—C7—H7B109.5F5'—B2—F6'108.0 (7)
H7A—C7—H7B109.5F7'—B2—F6'107.6 (7)
 

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