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The Ru atoms of the title compound, [Ru2Br2(C4H4N2)(C5H5N)8](PF6)2.2C3H7NO, are coordinated by the four N atoms of the pyridine (py) ligands and a bromide. Two such units are bridged by a pyrazine (pz) unit, which is disposed about a centre of inversion, so as to form a trans pseudo-octahedral geometry about Ru. The py units are in an eclipsed conformation when viewed down the internuclear axis. The Ru—N(pz) distance is 2.079 (3) Å, while the Ru—Br distance is 2.5524 (4) Å.

Supporting information

cif

Crystallographic Information File (CIF) https://doi.org/10.1107/S1600536803016398/tk6120sup1.cif
Contains datablocks global, I

hkl

Structure factor file (CIF format) https://doi.org/10.1107/S1600536803016398/tk6120Isup2.hkl
Contains datablock I

CCDC reference: 221660

Key indicators

  • Single-crystal X-ray study
  • T = 293 K
  • Mean [sigma](C-C) = 0.006 Å
  • Some non-H atoms missing
  • Disorder in solvent or counterion
  • R factor = 0.042
  • wR factor = 0.115
  • Data-to-parameter ratio = 19.8

checkCIF results

No syntax errors found

ADDSYM reports no extra symmetry


Red Alert Alert Level A:
PLAT_601 Alert A Structure Contains Solvent Accessible VOIDS of . 252.00 A   3
Author response: During the structure refinement, the atoms of the DMF solvent molecule were observed but could not be modelled satisfactorily. The SQUEEZE routine in PLATON was used to modify the HKL file and the solvent equated to one molecule of DMF, per molecule of complex.

Yellow Alert Alert Level C:
PLAT_302 Alert C Anion/Solvent Disorder ......................... 36.00 Perc. General Notes
FORMU_01 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:C50 H58 Br2 F12 N12 O2 P2 Ru2 Atom count from the _atom_site data: C44 H44 Br2 F12 N10 P2 Ru2 CELLZ_01 From the CIF: _cell_formula_units_Z 4 From the CIF: _chemical_formula_sum C50 H58 Br2 F12 N12 O2 P2 Ru2 TEST: Compare cell contents of formula and atom_site data atom Z*formula cif sites diff C 200.00 176.00 24.00 H 232.00 176.00 56.00 Br 8.00 8.00 0.00 F 48.00 48.00 0.00 N 48.00 40.00 8.00 O 8.00 0.00 8.00 P 8.00 8.00 0.00 Ru 8.00 8.00 0.00 Difference between formula and atom_site contents detected. ALERT: Large difference may be due to a symmetry error - see SYMMG tests CHEMW_03 From the CIF: _cell_formula_units_Z 4 From the CIF: _chemical_formula_weight 1510.98 TEST: Calculate formula weight from _atom_site_* atom mass num sum C 12.01 44.00 528.48 H 1.01 44.00 44.35 N 14.01 10.00 140.07 O 16.00 0.00 0.00 F 19.00 12.00 227.98 P 30.97 2.00 61.95 Br 79.90 2.00 159.81 Ru 101.07 2.00 202.14 Calculated formula weight 1364.78 ALERT: The ratio of given/expected molecular weight as calculated from the _atom_site* data lies outside the range 0.90 <> 1.10
1 Alert Level A = Potentially serious problem
0 Alert Level B = Potential problem
1 Alert Level C = Please check

Computing details top

Data collection: COLLECT (Nonius, 1997-2001); cell refinement: DENZO-SMN (Otwinowski & Minor, 1997); data reduction: DENZO-SMN; program(s) used to solve structure: SHELXS97 (Sheldrick, 1990); program(s) used to refine structure: SHELXL97 (Sheldrick, 1997); molecular graphics: SHELXTL (Sheldrick 1999); software used to prepare material for publication: SHELXTL.

(I) top
Crystal data top
[Ru2Br2(C4H4N2)(C5H5N)8](PF6)2·2C3H7NOF(000) = 3016
Mr = 1510.98Dx = 1.695 Mg m3
Monoclinic, C2/cMo Kα radiation, λ = 0.71073 Å
Hall symbol: -C 2ycCell parameters from 42564 reflections
a = 19.0401 (4) Åθ = 2.6–27.5°
b = 14.6334 (4) ŵ = 2.00 mm1
c = 21.2490 (5) ÅT = 293 K
β = 90.5609 (12)°Prism, dark red
V = 5920.1 (2) Å30.18 × 0.10 × 0.02 mm
Z = 4
Data collection top
Nonius KappaCCD
diffractometer
6741 independent reflections
Radiation source: fine-focus sealed tube5561 reflections with I > 2σ(I)
Graphite monochromatorRint = 0.046
φ scans, and ω scans with κ offsetsθmax = 27.5°, θmin = 2.9°
Absorption correction: multi-scan
(DENZO-SMN; Otwinowski & Minor, 1997)
h = 2424
Tmin = 0.715, Tmax = 0.961k = 1818
21516 measured reflectionsl = 2727
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)] = 0.042Hydrogen site location: inferred from neighbouring sites
wR(F2) = 0.115H-atom parameters constrained
S = 1.07 w = 1/[σ2(Fo2) + (0.0569P)2 + 4.3116P]
where P = (Fo2 + 2Fc2)/3
6741 reflections(Δ/σ)max = 0.001
341 parametersΔρmax = 0.48 e Å3
4 restraintsΔρmin = 0.90 e Å3
Special details top

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. Some highly disordered solvent peaks of DMF molecule were observed but could not be modelled satisfactorily. The SQUEEZE routine in PLATON was used to modify the HKL file and the solvent equated to one molecule of dimethylformamide, per molecule of complex.

Fractional atomic coordinates and isotropic or equivalent isotropic displacement parameters (Å2) top
xyzUiso*/UeqOcc. (<1)
Br10.323952 (19)0.36001 (3)0.266899 (16)0.03966 (11)
Ru10.294415 (12)0.314466 (18)0.153748 (12)0.02643 (9)
P10.00851 (5)0.28739 (7)0.05085 (5)0.0403 (2)
F1A0.01396 (18)0.2068 (2)0.0051 (2)0.0811 (11)0.91
F2A0.04451 (16)0.2475 (3)0.10225 (18)0.0836 (12)0.91
F3A0.03014 (19)0.3654 (2)0.09742 (18)0.0781 (10)0.91
F4A0.06082 (16)0.3261 (3)0.00082 (18)0.0843 (12)0.91
F1B0.0229 (19)0.255 (3)0.0198 (7)0.069 (8)*0.09
F2B0.0471 (10)0.2075 (13)0.0574 (14)0.042 (5)*0.09
F3B0.0214 (19)0.321 (3)0.1174 (9)0.070 (9)*0.09
F4B0.0550 (13)0.3781 (13)0.0442 (16)0.056 (7)*0.09
F50.05360 (12)0.34935 (17)0.02347 (12)0.0518 (6)
F60.06946 (13)0.2253 (2)0.07838 (15)0.0644 (7)
N10.20645 (14)0.2482 (2)0.19077 (13)0.0324 (6)
N20.35535 (14)0.19496 (19)0.16546 (14)0.0320 (6)
N30.38489 (14)0.3855 (2)0.12560 (13)0.0307 (6)
N40.23714 (14)0.43628 (19)0.14201 (13)0.0307 (6)
N50.26864 (13)0.27619 (18)0.06217 (12)0.0269 (5)
C10.16471 (18)0.2920 (3)0.23229 (17)0.0384 (8)
H10.17290.35500.24020.046*
C20.1102 (2)0.2485 (4)0.2643 (2)0.0524 (11)
H20.08190.28130.29310.063*
C30.0983 (2)0.1575 (4)0.2534 (2)0.0574 (13)
H30.06260.12580.27540.069*
C40.1388 (2)0.1127 (3)0.2099 (2)0.0515 (11)
H40.13030.05010.20080.062*
C50.19202 (19)0.1592 (3)0.17967 (19)0.0394 (8)
H50.21940.12720.14980.047*
C60.35035 (19)0.1445 (3)0.21843 (19)0.0392 (8)
H60.31940.16420.25050.047*
C70.3889 (2)0.0650 (3)0.2278 (2)0.0506 (10)
H70.38400.03110.26560.061*
C80.4340 (3)0.0360 (3)0.1823 (2)0.0590 (12)
H80.46020.01880.18760.071*
C90.4405 (2)0.0874 (3)0.1286 (2)0.0551 (11)
H90.47190.06940.09640.066*
C100.4009 (2)0.1660 (3)0.12217 (19)0.0426 (9)
H100.40620.20130.08500.051*
C110.44568 (17)0.3750 (3)0.15845 (17)0.0372 (8)
H110.44820.32900.18990.045*
C120.50432 (18)0.4289 (3)0.1481 (2)0.0448 (9)
H120.54600.41960.17210.054*
C130.50156 (19)0.4958 (3)0.10305 (19)0.0442 (9)
H130.54060.53480.09620.053*
C140.44085 (19)0.5053 (3)0.06793 (18)0.0399 (8)
H140.43830.54990.03550.048*
C150.38409 (17)0.4498 (2)0.07970 (15)0.0324 (7)
H150.34280.45720.05480.039*
C160.26637 (18)0.5171 (2)0.15867 (16)0.0345 (7)
H160.30960.51650.18140.041*
C170.2364 (2)0.6003 (3)0.1442 (2)0.0458 (9)
H170.25880.65550.15670.055*
C180.1732 (2)0.6028 (3)0.1110 (2)0.0536 (10)
H180.15220.65930.09940.064*
C190.1419 (2)0.5212 (3)0.0958 (2)0.0469 (9)
H190.09780.52050.07430.056*
C200.17450 (18)0.4406 (3)0.11142 (17)0.0357 (7)
H200.15200.38490.10020.043*
C210.20344 (16)0.2471 (2)0.04590 (15)0.0287 (6)
H210.16850.24440.07740.034*
C220.18596 (16)0.2217 (2)0.01457 (16)0.0298 (6)
H220.13940.20140.02290.036*
Atomic displacement parameters (Å2) top
U11U22U33U12U13U23
Br10.0421 (2)0.0472 (2)0.02950 (19)0.00843 (15)0.00730 (15)0.00066 (15)
Ru10.02395 (14)0.02955 (15)0.02571 (15)0.00255 (9)0.00417 (10)0.00040 (10)
P10.0318 (4)0.0449 (6)0.0442 (5)0.0007 (4)0.0019 (4)0.0018 (4)
F1A0.069 (2)0.063 (2)0.112 (3)0.0135 (17)0.042 (2)0.032 (2)
F2A0.0494 (16)0.123 (3)0.079 (2)0.0046 (19)0.0102 (16)0.044 (2)
F3A0.084 (2)0.066 (2)0.085 (2)0.0133 (17)0.034 (2)0.0324 (18)
F4A0.0462 (16)0.132 (3)0.075 (2)0.0038 (19)0.0168 (16)0.038 (2)
F50.0422 (12)0.0551 (15)0.0582 (15)0.0093 (11)0.0046 (11)0.0005 (12)
F60.0452 (13)0.0613 (16)0.087 (2)0.0041 (12)0.0202 (13)0.0031 (15)
N10.0287 (13)0.0381 (16)0.0303 (14)0.0024 (12)0.0044 (11)0.0027 (12)
N20.0292 (13)0.0336 (15)0.0331 (15)0.0002 (11)0.0048 (12)0.0031 (12)
N30.0267 (12)0.0355 (15)0.0299 (14)0.0022 (11)0.0043 (11)0.0001 (12)
N40.0296 (13)0.0319 (15)0.0305 (14)0.0020 (11)0.0034 (11)0.0033 (11)
N50.0253 (12)0.0268 (13)0.0285 (13)0.0022 (10)0.0014 (10)0.0011 (11)
C10.0326 (16)0.051 (2)0.0313 (17)0.0002 (15)0.0014 (14)0.0029 (15)
C20.0323 (18)0.083 (3)0.043 (2)0.002 (2)0.0041 (16)0.016 (2)
C30.0309 (19)0.076 (3)0.065 (3)0.013 (2)0.0075 (19)0.034 (3)
C40.041 (2)0.049 (2)0.064 (3)0.0176 (18)0.023 (2)0.021 (2)
C50.0360 (18)0.0370 (19)0.045 (2)0.0071 (15)0.0128 (16)0.0106 (16)
C60.0371 (18)0.041 (2)0.040 (2)0.0030 (15)0.0034 (15)0.0060 (16)
C70.057 (2)0.047 (2)0.048 (2)0.0108 (19)0.0066 (19)0.0144 (19)
C80.064 (3)0.051 (3)0.062 (3)0.024 (2)0.006 (2)0.008 (2)
C90.051 (2)0.061 (3)0.053 (3)0.023 (2)0.003 (2)0.000 (2)
C100.0383 (19)0.047 (2)0.042 (2)0.0066 (16)0.0030 (16)0.0036 (17)
C110.0294 (16)0.046 (2)0.0360 (18)0.0071 (14)0.0069 (14)0.0035 (16)
C120.0286 (16)0.058 (2)0.048 (2)0.0094 (16)0.0098 (16)0.0005 (19)
C130.0329 (17)0.053 (2)0.047 (2)0.0130 (17)0.0008 (16)0.0040 (18)
C140.0393 (18)0.044 (2)0.0365 (18)0.0083 (16)0.0002 (15)0.0037 (16)
C150.0312 (15)0.0376 (18)0.0285 (16)0.0045 (14)0.0030 (13)0.0010 (14)
C160.0374 (17)0.0328 (18)0.0332 (17)0.0035 (14)0.0006 (14)0.0044 (14)
C170.053 (2)0.035 (2)0.049 (2)0.0008 (17)0.0005 (18)0.0007 (17)
C180.058 (2)0.042 (2)0.061 (3)0.0122 (19)0.007 (2)0.005 (2)
C190.046 (2)0.049 (2)0.046 (2)0.0112 (18)0.0099 (18)0.0061 (18)
C200.0345 (16)0.0360 (18)0.0364 (18)0.0024 (14)0.0081 (14)0.0048 (15)
C210.0253 (14)0.0303 (17)0.0304 (16)0.0018 (12)0.0010 (12)0.0024 (13)
C220.0245 (14)0.0319 (16)0.0328 (16)0.0025 (12)0.0027 (12)0.0001 (14)
Geometric parameters (Å, º) top
Ru1—Br12.5524 (4)C4—H40.9499
Ru1—N12.095 (3)C5—H50.9500
Ru1—N22.112 (3)C6—C71.389 (5)
Ru1—N32.103 (3)C6—H60.9501
Ru1—N42.103 (3)C7—C81.367 (7)
Ru1—N52.079 (3)C7—H70.9499
P1—F1A1.591 (3)C8—C91.373 (7)
P1—F2A1.591 (3)C8—H80.9500
P1—F3A1.569 (3)C9—C101.381 (6)
P1—F4A1.580 (3)C9—H90.9500
P1—F1B1.595 (10)C10—H100.9500
P1—F2B1.582 (10)C11—C121.386 (5)
P1—F3B1.597 (10)C11—H110.9500
P1—F4B1.601 (10)C12—C131.370 (6)
P1—F51.604 (2)C12—H120.9501
P1—F61.590 (3)C13—C141.377 (5)
N1—C51.351 (5)C13—H130.9502
N1—C11.354 (5)C14—C151.376 (5)
N2—C101.339 (5)C14—H140.9499
N2—C61.350 (5)C15—H150.9500
N3—C111.354 (4)C16—C171.379 (5)
N3—C151.356 (4)C16—H160.9500
N4—C161.353 (4)C17—C181.389 (6)
N4—C201.354 (4)C17—H170.9500
N5—C22i1.337 (4)C18—C191.372 (6)
N5—C211.354 (4)C18—H180.9499
C1—C21.400 (5)C19—C201.374 (5)
C1—H10.9500C19—H190.9500
C2—C31.370 (7)C20—H200.9499
C2—H20.9499C21—C221.375 (5)
C3—C41.376 (7)C21—H210.9500
C3—H30.9501C22—N5i1.337 (4)
C4—C51.384 (5)C22—H220.9499
N1—Ru1—N290.73 (11)C3—C2—H2120.5
N1—Ru1—N3174.38 (11)C1—C2—H2120.7
N1—Ru1—N491.22 (11)C2—C3—C4118.9 (4)
N1—Ru1—N592.55 (10)C2—C3—H3120.6
N2—Ru1—N389.54 (11)C4—C3—H3120.5
N2—Ru1—N4177.91 (10)C3—C4—C5119.7 (4)
N2—Ru1—N590.66 (11)C3—C4—H4120.0
N3—Ru1—N488.44 (11)C5—C4—H4120.3
N3—Ru1—N593.06 (10)N1—C5—C4122.8 (4)
N4—Ru1—N590.00 (10)N1—C5—H5118.7
N1—Ru1—Br186.38 (8)C4—C5—H5118.5
N2—Ru1—Br189.40 (8)N2—C6—C7122.4 (4)
N3—Ru1—Br188.02 (8)N2—C6—H6118.8
N4—Ru1—Br189.98 (8)C7—C6—H6118.8
N5—Ru1—Br1178.92 (7)C8—C7—C6119.6 (4)
F3A—P1—F4A90.6 (2)C8—C7—H7120.3
F3A—P1—F689.27 (16)C6—C7—H7120.1
F4A—P1—F690.18 (17)C7—C8—C9118.6 (4)
F2B—P1—F692.0 (9)C7—C8—H8120.7
F3A—P1—F1A178.6 (3)C9—C8—H8120.7
F4A—P1—F1A90.7 (2)C8—C9—C10119.1 (4)
F6—P1—F1A90.15 (16)C8—C9—H9120.5
F3A—P1—F2A90.1 (2)C10—C9—H9120.5
F4A—P1—F2A179.3 (3)N2—C10—C9123.5 (4)
F6—P1—F2A89.91 (17)N2—C10—H10118.3
F1A—P1—F2A88.6 (3)C9—C10—H10118.2
F2B—P1—F1B88.4 (18)N3—C11—C12122.7 (3)
F6—P1—F1B93.3 (12)N3—C11—H11118.6
F2B—P1—F3B85.2 (18)C12—C11—H11118.7
F6—P1—F3B96.0 (13)C13—C12—C11119.4 (3)
F1B—P1—F3B168.9 (19)C13—C12—H12120.3
F2B—P1—F4B171.5 (14)C11—C12—H12120.3
F6—P1—F4B95.9 (10)C12—C13—C14118.5 (3)
F1B—P1—F4B94.2 (19)C12—C13—H13120.8
F3B—P1—F4B90.9 (19)C14—C13—H13120.7
F3A—P1—F590.93 (16)C13—C14—C15119.9 (4)
F4A—P1—F590.43 (16)C13—C14—H14120.0
F2B—P1—F587.4 (9)C15—C14—H14120.1
F6—P1—F5179.36 (17)N3—C15—C14122.5 (3)
F1A—P1—F589.64 (15)N3—C15—H15118.9
F2A—P1—F589.48 (16)C14—C15—H15118.7
F1B—P1—F587.0 (12)N4—C16—C17123.1 (3)
F3B—P1—F583.7 (13)N4—C16—H16118.4
F4B—P1—F584.7 (10)C17—C16—H16118.5
C5—N1—C1116.7 (3)C16—C17—C18119.3 (4)
C5—N1—Ru1122.8 (2)C16—C17—H17120.4
C1—N1—Ru1120.1 (2)C18—C17—H17120.3
C10—N2—C6116.8 (3)C19—C18—C17118.1 (4)
C10—N2—Ru1122.7 (2)C19—C18—H18121.0
C6—N2—Ru1120.5 (2)C17—C18—H18120.9
C11—N3—C15116.9 (3)C20—C19—C18119.7 (4)
C11—N3—Ru1119.7 (2)C20—C19—H19120.1
C15—N3—Ru1123.0 (2)C18—C19—H19120.2
C16—N4—C20116.3 (3)N4—C20—C19123.4 (3)
C16—N4—Ru1119.9 (2)N4—C20—H20118.3
C20—N4—Ru1123.3 (2)C19—C20—H20118.3
C22i—N5—C21114.3 (3)N5—C21—C22122.5 (3)
C22i—N5—Ru1123.6 (2)N5—C21—H21118.7
C21—N5—Ru1122.1 (2)C22—C21—H21118.8
N1—C1—C2123.0 (4)N5i—C22—C21123.2 (3)
N1—C1—H1118.6N5i—C22—H22118.3
C2—C1—H1118.5C21—C22—H22118.4
C3—C2—C1118.8 (4)
N5—Ru1—N1—C554.0 (3)N3—Ru1—N5—C21162.2 (3)
N4—Ru1—N1—C5144.1 (3)N2—Ru1—N5—C21108.2 (3)
N2—Ru1—N1—C536.7 (3)C5—N1—C1—C21.8 (5)
Br1—Ru1—N1—C5126.0 (3)Ru1—N1—C1—C2172.3 (3)
N5—Ru1—N1—C1132.2 (3)N1—C1—C2—C30.1 (6)
N4—Ru1—N1—C142.1 (3)C1—C2—C3—C42.0 (6)
N2—Ru1—N1—C1137.1 (3)C2—C3—C4—C52.0 (6)
Br1—Ru1—N1—C147.8 (2)C1—N1—C5—C41.8 (5)
N5—Ru1—N2—C1045.9 (3)Ru1—N1—C5—C4172.1 (3)
N1—Ru1—N2—C10138.5 (3)C3—C4—C5—N10.0 (6)
N3—Ru1—N2—C1047.2 (3)C10—N2—C6—C71.6 (5)
Br1—Ru1—N2—C10135.2 (3)Ru1—N2—C6—C7179.3 (3)
N5—Ru1—N2—C6135.0 (3)N2—C6—C7—C80.4 (6)
N1—Ru1—N2—C642.4 (3)C6—C7—C8—C90.6 (7)
N3—Ru1—N2—C6131.9 (3)C7—C8—C9—C100.4 (7)
Br1—Ru1—N2—C643.9 (3)C6—N2—C10—C91.8 (6)
N5—Ru1—N3—C11135.5 (3)Ru1—N2—C10—C9179.1 (3)
N4—Ru1—N3—C11134.6 (3)C8—C9—C10—N20.9 (7)
N2—Ru1—N3—C1144.8 (3)C15—N3—C11—C122.3 (5)
Br1—Ru1—N3—C1144.6 (3)Ru1—N3—C11—C12170.7 (3)
N5—Ru1—N3—C1552.0 (3)N3—C11—C12—C130.0 (6)
N4—Ru1—N3—C1537.9 (3)C11—C12—C13—C142.0 (6)
N2—Ru1—N3—C15142.6 (3)C12—C13—C14—C151.7 (6)
Br1—Ru1—N3—C15128.0 (3)C11—N3—C15—C142.6 (5)
N5—Ru1—N4—C16131.4 (3)Ru1—N3—C15—C14170.2 (3)
N1—Ru1—N4—C16136.1 (3)C13—C14—C15—N30.6 (6)
N3—Ru1—N4—C1638.3 (3)C20—N4—C16—C172.0 (5)
Br1—Ru1—N4—C1649.7 (2)Ru1—N4—C16—C17170.4 (3)
N5—Ru1—N4—C2040.5 (3)N4—C16—C17—C180.0 (6)
N1—Ru1—N4—C2052.1 (3)C16—C17—C18—C192.2 (7)
N3—Ru1—N4—C20133.5 (3)C17—C18—C19—C202.3 (7)
Br1—Ru1—N4—C20138.4 (3)C16—N4—C20—C191.9 (5)
N1—Ru1—N5—C22i162.8 (3)Ru1—N4—C20—C19170.3 (3)
N4—Ru1—N5—C22i105.9 (3)C18—C19—C20—N40.3 (6)
N3—Ru1—N5—C22i17.5 (3)C22i—N5—C21—C220.3 (5)
N2—Ru1—N5—C22i72.1 (3)Ru1—N5—C21—C22180.0 (2)
N1—Ru1—N5—C2117.5 (3)N5—C21—C22—N5i0.3 (6)
N4—Ru1—N5—C2173.8 (3)
Symmetry code: (i) x+1/2, y+1/2, z.
 

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