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In the crystal structure of the title heterothiol­ate cluster, [MoCu2S4(C19H17P)4]·4H2O, the Mo atom lies on a postion of crystallographic site symmetry \overline{4}, coordinated by four S atoms in a tetra­hedral environment; each pair of S atoms bis-chelates two Cu atoms which are, in addition, coordinated by two phosphine ligands each. The tetra­hedrally coordinated Cu atoms lie on positions of site symmetry 2.

Supporting information

cif

Crystallographic Information File (CIF) https://doi.org/10.1107/S1600536806011111/lh2030sup1.cif
Contains datablocks global, I

hkl

Structure factor file (CIF format) https://doi.org/10.1107/S1600536806011111/lh2030Isup2.hkl
Contains datablock I

CCDC reference: 608441

Key indicators

  • Single-crystal X-ray study
  • T = 291 K
  • Mean [sigma](C-C) = 0.007 Å
  • H-atom completeness 90%
  • Disorder in main residue
  • R factor = 0.046
  • wR factor = 0.148
  • Data-to-parameter ratio = 27.1

checkCIF/PLATON results

No syntax errors found



Alert level A PLAT430_ALERT_2_A Short Inter D...A Contact O1W' .. O1W .. 1.94 Ang.
Author Response: The water molecule is disordered over two positions.

Alert level B PLAT601_ALERT_2_B Structure Contains Solvent Accessible VOIDS of . 156.00 A   3
Alert level C PLAT041_ALERT_1_C Calc. and Rep. SumFormula Strings Differ .... ? PLAT042_ALERT_1_C Calc. and Rep. MoietyFormula Strings Differ .... ? PLAT068_ALERT_1_C Reported F000 Differs from Calcd (or Missing)... ? PLAT094_ALERT_2_C Ratio of Maximum / Minimum Residual Density .... 3.16 PLAT241_ALERT_2_C Check High Ueq as Compared to Neighbors for C13 PLAT241_ALERT_2_C Check High Ueq as Compared to Neighbors for C18 PLAT242_ALERT_2_C Check Low Ueq as Compared to Neighbors for C14 PLAT301_ALERT_3_C Main Residue Disorder ......................... 22.00 Perc. PLAT302_ALERT_4_C Anion/Solvent Disorder ......................... 50.00 Perc. PLAT720_ALERT_4_C Number of Unusual/Non-Standard Label(s) ........ 1 PLAT790_ALERT_4_C Centre of Gravity not Within Unit Cell: Resd. # 2 O PLAT790_ALERT_4_C Centre of Gravity not Within Unit Cell: Resd. # 3 O PLAT850_ALERT_2_C Check Flack Parameter Exact Value 0.00 and su .. 0.02
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:C76 H76 Cu2 Mo1 O4 P4 S4 Atom count from the _atom_site data: C76 H68 Cu2 Mo1 O4 P4 S4 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 2 From the CIF: _chemical_formula_sum C76 H76 Cu2 Mo O4 P4 S4 TEST: Compare cell contents of formula and atom_site data atom Z*formula cif sites diff C 152.00 152.00 0.00 H 152.00 136.00 16.00 Cu 4.00 4.00 0.00 Mo 2.00 2.00 0.00 O 8.00 8.00 0.00 P 8.00 8.00 0.00 S 8.00 8.00 0.00 REFLT03_ALERT_4_G Please check that the estimate of the number of Friedel pairs is correct. If it is not, please give the correct count in the _publ_section_exptl_refinement section of the submitted CIF. From the CIF: _diffrn_reflns_theta_max 27.50 From the CIF: _reflns_number_total 4886 Count of symmetry unique reflns 2576 Completeness (_total/calc) 189.67% TEST3: Check Friedels for noncentro structure Estimate of Friedel pairs measured 2310 Fraction of Friedel pairs measured 0.897 Are heavy atom types Z>Si present yes
1 ALERT level A = In general: serious problem 1 ALERT level B = Potentially serious problem 13 ALERT level C = Check and explain 4 ALERT level G = General alerts; check 5 ALERT type 1 CIF construction/syntax error, inconsistent or missing data 8 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 5 ALERT type 4 Improvement, methodology, query or suggestion

Computing details top

Data collection: SMART (Bruker, 2004); cell refinement: SAINT (Bruker, 2004); data reduction: SAINT; program(s) used to solve structure: SHELXS97 (Sheldrick, 1997); program(s) used to refine structure: SHELXL97 (Sheldrick, 1997); molecular graphics: ORTEPII (Johnson, 1976); software used to prepare material for publication: SHELXL97.

Tetrakis(benzyldiphenylphosphine-κP)tetra-µ2-sulfido- dicopper(I)molybdenum(VI) tetrahydrate top
Crystal data top
[MoCu2S4(C19H17P)4]·4H2ODx = 1.163 Mg m3
Mr = 1528.51Mo Kα radiation, λ = 0.71073 Å
Tetragonal, I4Cell parameters from 3407 reflections
Hall symbol: I -4θ = 2.7–25.7°
a = 13.777 (1) ŵ = 0.83 mm1
c = 22.995 (2) ÅT = 291 K
V = 4364.3 (4) Å3Plate, red
Z = 20.39 × 0.28 × 0.06 mm
F(000) = 1576
Data collection top
Bruker APEX-II area-detector
diffractometer
4886 independent reflections
Radiation source: fine-focus sealed tube3959 reflections with I > 2σ(I)
Graphite monochromatorRint = 0.017
φ and ω scansθmax = 27.5°, θmin = 2.7°
Absorption correction: multi-scan
(SADABS; Sheldrick, 1996)
h = 1715
Tmin = 0.831, Tmax = 0.952k = 177
9215 measured reflectionsl = 2529
Refinement top
Refinement on F2Secondary atom site location: difference Fourier map
Least-squares matrix: fullHydrogen site location: inferred from neighbouring sites
R[F2 > 2σ(F2)] = 0.046H-atom parameters constrained
wR(F2) = 0.148 w = 1/[σ2(Fo2) + (0.0923P)2]
where P = (Fo2 + 2Fc2)/3
S = 1.11(Δ/σ)max = 0.001
4886 reflectionsΔρmax = 0.79 e Å3
180 parametersΔρmin = 0.25 e Å3
49 restraintsAbsolute structure: Flack (1983), 2328 Friedel pairs
Primary atom site location: structure-invariant direct methodsAbsolute structure parameter: 0.00 (2)
Fractional atomic coordinates and isotropic or equivalent isotropic displacement parameters (Å2) top
xyzUiso*/UeqOcc. (<1)
Mo11.00000.50000.25000.0440 (2)
Cu11.00000.50000.12961 (2)0.0482 (2)
S11.0529 (1)0.3822 (1)0.19337 (5)0.0592 (3)
P10.8803 (1)0.4323 (1)0.07304 (5)0.0556 (3)
O1w1.161 (1)0.111 (1)0.2339 (6)0.177 (4)0.50
O1w'1.068 (1)0.215 (1)0.2229 (6)0.177 (4)0.50
C10.938 (1)0.3502 (7)0.0211 (3)0.063 (2)0.50
C20.947 (1)0.3740 (6)0.0374 (3)0.085 (3)0.50
C30.993 (1)0.3103 (7)0.0754 (3)0.092 (3)0.50
C41.029 (1)0.2228 (7)0.0550 (4)0.100 (4)0.50
C51.021 (1)0.1990 (6)0.0035 (4)0.096 (3)0.50
C60.975 (1)0.2627 (7)0.0416 (3)0.089 (3)0.50
C1'0.928 (1)0.3281 (7)0.0300 (3)0.063 (2)0.50
C2'0.942 (1)0.3371 (6)0.0296 (3)0.085 (3)0.50
C3'0.994 (1)0.2666 (7)0.0596 (3)0.092 (3)0.50
C4'1.031 (1)0.1871 (7)0.0300 (4)0.100 (4)0.50
C5'1.017 (1)0.1781 (7)0.0296 (4)0.096 (3)0.50
C6'0.965 (1)0.2486 (7)0.0596 (3)0.089 (3)0.50
C70.7842 (2)0.3672 (2)0.11048 (13)0.057 (1)
C80.7335 (3)0.2914 (3)0.08459 (14)0.076 (2)
C90.6601 (3)0.2444 (2)0.11500 (19)0.090 (2)
C100.6373 (3)0.2732 (3)0.17131 (18)0.094 (2)
C110.6880 (3)0.3489 (3)0.19720 (13)0.089 (2)
C120.7614 (2)0.3960 (2)0.16679 (13)0.069 (1)
C130.8094 (4)0.5088 (5)0.0231 (2)0.080 (2)
C140.7433 (2)0.5778 (3)0.0544 (2)0.070 (1)
C150.6457 (2)0.5549 (3)0.0615 (2)0.084 (2)
C160.5850 (2)0.6177 (3)0.0918 (2)0.093 (2)
C170.6219 (3)0.7032 (3)0.1151 (2)0.104 (2)
C180.7195 (4)0.7260 (3)0.1080 (2)0.118 (3)
C190.7802 (2)0.6633 (3)0.0777 (2)0.099 (2)
H20.92210.43250.05110.102*0.50
H30.99840.32620.11460.111*0.50
H41.06000.18020.08040.120*0.50
H51.04530.14050.01720.115*0.50
H60.96900.24680.08070.106*0.50
H2'0.91650.39030.04940.102*0.50
H3'1.00320.27260.09950.111*0.50
H4'1.06620.13990.05010.120*0.50
H5'1.04250.12490.04930.115*0.50
H6'0.95570.24250.09950.106*0.50
H80.74880.27210.04690.091*
H90.62620.19370.09770.107*
H100.58820.24170.19170.112*
H110.67280.36820.23490.107*
H120.79530.44670.18410.082*
H13a0.85360.54560.00120.096*
H13b0.77090.46750.00210.096*
H150.62110.49770.04600.100*
H160.51980.60240.09660.112*
H170.58130.74520.13530.124*
H180.74420.78330.12350.141*
H190.84550.67860.07290.118*
Atomic displacement parameters (Å2) top
U11U22U33U12U13U23
Mo10.0484 (2)0.0484 (2)0.0353 (3)0.0000.0000.000
Cu10.0513 (5)0.0535 (5)0.0400 (4)0.0006 (4)0.0000.000
S10.0778 (7)0.0526 (5)0.0472 (5)0.0123 (5)0.0001 (6)0.0008 (5)
P10.0490 (6)0.0742 (8)0.0436 (6)0.0004 (6)0.0038 (5)0.0082 (5)
O1w0.211 (8)0.204 (8)0.117 (6)0.042 (6)0.041 (6)0.007 (6)
O1w'0.211 (8)0.204 (8)0.117 (6)0.042 (6)0.041 (6)0.007 (6)
C10.042 (4)0.087 (5)0.060 (3)0.017 (4)0.008 (3)0.024 (3)
C20.081 (4)0.105 (8)0.069 (4)0.021 (6)0.016 (3)0.021 (5)
C30.096 (5)0.112 (8)0.067 (5)0.001 (6)0.023 (5)0.012 (5)
C40.099 (5)0.118 (8)0.083 (7)0.002 (5)0.017 (6)0.040 (6)
C50.084 (4)0.097 (5)0.105 (8)0.003 (4)0.015 (6)0.039 (6)
C60.076 (5)0.108 (5)0.082 (6)0.013 (4)0.008 (5)0.037 (5)
C1'0.042 (4)0.087 (5)0.060 (3)0.017 (4)0.008 (3)0.024 (3)
C2'0.081 (4)0.105 (8)0.069 (4)0.021 (6)0.016 (3)0.021 (5)
C3'0.096 (5)0.112 (8)0.067 (5)0.001 (6)0.023 (5)0.012 (5)
C4'0.099 (5)0.118 (8)0.083 (7)0.002 (5)0.017 (6)0.040 (6)
C5'0.084 (4)0.097 (5)0.105 (8)0.003 (4)0.015 (6)0.039 (6)
C6'0.076 (5)0.108 (5)0.082 (6)0.013 (4)0.008 (5)0.037 (5)
C70.049 (2)0.063 (3)0.060 (3)0.001 (2)0.012 (2)0.002 (2)
C80.066 (3)0.077 (3)0.085 (4)0.008 (2)0.009 (3)0.021 (3)
C90.076 (4)0.090 (4)0.102 (5)0.027 (3)0.006 (4)0.015 (4)
C100.061 (3)0.100 (4)0.120 (6)0.022 (3)0.002 (3)0.027 (4)
C110.080 (3)0.127 (5)0.060 (3)0.023 (3)0.009 (3)0.004 (3)
C120.061 (3)0.082 (3)0.063 (3)0.012 (2)0.001 (2)0.009 (2)
C130.075 (3)0.116 (4)0.048 (3)0.001 (3)0.009 (2)0.018 (3)
C140.056 (3)0.089 (4)0.066 (3)0.003 (3)0.012 (2)0.031 (3)
C150.060 (3)0.093 (4)0.098 (4)0.003 (3)0.015 (3)0.019 (3)
C160.063 (3)0.096 (5)0.121 (5)0.006 (3)0.006 (3)0.022 (4)
C170.090 (5)0.096 (5)0.125 (6)0.036 (4)0.020 (4)0.009 (4)
C180.121 (6)0.080 (4)0.152 (8)0.004 (4)0.050 (6)0.016 (5)
C190.073 (4)0.087 (4)0.136 (6)0.000 (3)0.034 (4)0.037 (4)
Geometric parameters (Å, º) top
Mo1—S12.205 (1)C13—C141.501 (7)
Mo1—S1i2.205 (1)C14—C151.39
Mo1—S1ii2.205 (1)C14—C191.39
Mo1—S1iii2.205 (1)C15—C161.39
Cu1—P12.298 (1)C16—C171.39
Cu1—P1i2.298 (1)C17—C181.39
Cu1—S12.306 (1)C18—C191.39
Cu1—S1i2.306 (1)C2—H20.93
P1—C71.817 (3)C3—H30.93
P1—C11.826 (5)C4—H40.93
P1—C131.840 (5)C5—H50.93
P1—C1'1.861 (5)C6—H60.93
C1—C21.39C2'—H2'0.93
C1—C61.39C3'—H3'0.93
C2—C31.39C4'—H4'0.93
C3—C41.39C5'—H5'0.93
C4—C51.39C6'—H6'0.93
C5—C61.39C8—H80.93
C1'—C2'1.39C9—H90.93
C1'—C6'1.39C10—H100.93
C2'—C3'1.39C11—H110.93
C3'—C4'1.39C12—H120.93
C4'—C5'1.39C13—H13a0.97
C5'—C6'1.39C13—H13b0.97
C7—C81.39C15—H150.93
C7—C121.39C16—H160.93
C8—C91.39C17—H170.93
C9—C101.39C18—H180.93
C10—C111.39C19—H190.93
C11—C121.39
S1—Mo1—S1i107.62 (6)C19—C18—C17120.0
S1—Mo1—S1ii110.40 (3)C18—C19—C14120.0
S1—Mo1—S1iii110.40 (3)C1—C2—H2120.0
P1—Cu1—P1i111.05 (6)C3—C2—H2120.0
P1—Cu1—S1107.51 (5)C4—C3—H3120.0
P1—Cu1—S1i114.77 (4)C2—C3—H3120.0
S1—Cu1—S1i101.04 (6)C3—C4—H4120.0
Mo1—S1—Cu175.67 (3)C5—C4—H4120.0
C7—P1—C1108.7 (5)C4—C5—H5120.0
C7—P1—C13101.0 (2)C6—C5—H5120.0
C1—P1—C13100.2 (3)C5—C6—H6120.0
C7—P1—C1'97.2 (5)C1—C6—H6120.0
C13—P1—C1'107.2 (4)C1'—C2'—H2'120.0
C7—P1—Cu1117.1 (1)C3'—C2'—H2'120.0
C1—P1—Cu1108.0 (6)C4'—C3'—H3'120.0
C13—P1—Cu1120.1 (2)C2'—C3'—H3'120.0
C1'—P1—Cu1111.3 (5)C3'—C4'—H4'120.0
C2—C1—C6120.0C5'—C4'—H4'120.0
C2—C1—P1121.6 (3)C4'—C5'—H5'120.0
C6—C1—P1118.3 (3)C6'—C5'—H5'120.0
C1—C2—C3120.0C5'—C6'—H6'120.0
C4—C3—C2120.0C1'—C6'—H6'120.0
C3—C4—C5120.0C7—C8—H8120.0
C4—C5—C6120.0C9—C8—H8120.0
C5—C6—C1120.0C8—C9—H9120.0
C2'—C1'—C6'120.0C10—C9—H9120.0
C2'—C1'—P1120.3 (3)C11—C10—H10120.0
C6'—C1'—P1118.6 (3)C9—C10—H10120.0
C1'—C2'—C3'120.0C12—C11—H11120.0
C4'—C3'—C2'120.0C10—C11—H11120.0
C3'—C4'—C5'120.0C11—C12—H12120.0
C4'—C5'—C6'120.0C7—C12—H12120.0
C5'—C6'—C1'120.0C14—C13—H13a109.1
C8—C7—C12120.0P1—C13—H13a109.1
C8—C7—P1122.3 (2)C14—C13—H13b109.1
C12—C7—P1117.7 (2)P1—C13—H13b109.1
C7—C8—C9120.0H13a—C13—H13b107.8
C8—C9—C10120.0C16—C15—H15120.0
C11—C10—C9120.0C14—C15—H15120.0
C12—C11—C10120.0C15—C16—H16120.0
C11—C12—C7120.0C17—C16—H16120.0
C14—C13—P1112.6 (3)C18—C17—H17120.0
C15—C14—C19120.0C16—C17—H17120.0
C15—C14—C13120.0 (4)C19—C18—H18120.0
C19—C14—C13120.0 (4)C17—C18—H18120.0
C16—C15—C14120.0C18—C19—H19120.0
C15—C16—C17120.0C14—C19—H19120.0
C18—C17—C16120.0
S1iii—Mo1—S1—Cu1120.56 (2)C1—P1—C1'—C2'31 (4)
S1ii—Mo1—S1—Cu1120.56 (2)C13—P1—C1'—C2'26 (1)
Cu1ii—Mo1—S1—Cu1180Cu1—P1—C1'—C2'107.2 (8)
P1—Cu1—S1—Mo1120.61 (4)C7—P1—C1'—C6'62.0 (8)
P1i—Cu1—S1—Mo1115.32 (5)C1—P1—C1'—C6'137 (5)
P1i—Cu1—P1—C7175.5 (2)C13—P1—C1'—C6'166.0 (7)
S1i—Cu1—P1—C762.4 (2)Cu1—P1—C1'—C6'60.8 (8)
S1—Cu1—P1—C749.2 (2)P1—C1'—C2'—C3'168 (1)
P1i—Cu1—P1—C152.4 (3)P1—C1'—C6'—C5'168 (1)
S1i—Cu1—P1—C1174.6 (3)C1—P1—C7—C829.3 (5)
S1—Cu1—P1—C173.9 (3)C13—P1—C7—C875.6 (3)
P1i—Cu1—P1—C1361.5 (2)C1'—P1—C7—C833.5 (4)
S1i—Cu1—P1—C1360.7 (2)Cu1—P1—C7—C8152.0 (2)
S1—Cu1—P1—C13172.2 (2)C1—P1—C7—C12151.2 (5)
P1i—Cu1—P1—C1'64.9 (3)C13—P1—C7—C12103.9 (3)
S1i—Cu1—P1—C1'172.9 (3)C1'—P1—C7—C12146.9 (4)
S1—Cu1—P1—C1'61.4 (3)Cu1—P1—C7—C1228.4 (3)
C7—P1—C1—C2125.7 (8)P1—C7—C8—C9179.5 (3)
C13—P1—C1—C220 (1)P1—C7—C12—C11179.6 (3)
C1'—P1—C1—C2146 (5)C7—P1—C13—C1461.6 (4)
Cu1—P1—C1—C2106.3 (9)C1—P1—C13—C14173.1 (7)
C7—P1—C1—C655.3 (8)C1'—P1—C13—C14162.8 (6)
C13—P1—C1—C6160.8 (7)Cu1—P1—C13—C1469.0 (4)
C1'—P1—C1—C635 (4)P1—C13—C14—C1598.5 (4)
Cu1—P1—C1—C672.7 (8)P1—C13—C14—C1979.9 (4)
P1—C1—C2—C3179 (1)C13—C14—C15—C16178.4 (4)
P1—C1—C6—C5179 (1)C13—C14—C19—C18178.4 (4)
C7—P1—C1'—C2'130.0 (9)
Symmetry codes: (i) x+2, y+1, z; (ii) y+1/2, x+3/2, z+1/2; (iii) y+3/2, x1/2, z+1/2.
 

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