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Tp'Rh[P(OMe)3](Me)H, loses methane in pentane solution containing CH2F2 to give the scorpionate complex bis([mu]-dimethyl phosphito)-[kappa]2P:O;[kappa]2O:P-bis{methyl[tris(3,5-dimethyl-1H-pyrazol-1-yl-[kappa]N2)bor­ato]rhodium(III)}, [Rh2(CH3)2(C2H6O3P)2(C15H22BN6)2], in which the phosphine O-Me bond is cleaved. The product is dimeric and resembles the Arbusov-type rearrangement product known to form from trimethyl phosphite.

Supporting information

cif

Crystallographic Information File (CIF) https://doi.org/10.1107/S0108270113015953/yp3031sup1.cif
Contains datablock I

hkl

Structure factor file (CIF format) https://doi.org/10.1107/S0108270113015953/yp3031Isup2.hkl
Contains datablock I

CCDC reference: 964737

Computing details top

Data collection: APEX2 (Bruker, 2012); cell refinement: SAINT (Bruker, 2009); data reduction: SAINT (Bruker, 2009); program(s) used to solve structure: SIR97 (Altomare et al., 1999); program(s) used to refine structure: SHELXL2012 (Sheldrick, 2012); molecular graphics: SHELXTL (Sheldrick, 2008); software used to prepare material for publication: SHELXTL (Sheldrick, 2008).

Bis(µ-dimethyl phosphito)-κ2P:O;κ2O:P-bis{methyl[tris(3,5,-dimethyl-1H-pyrazol-1-yl-κN2)borato]rhodium(III)} top
Crystal data top
[Rh2(CH3)2(C2H6O3P)2(C15H22BN6)2]Z = 1
Mr = 1048.35F(000) = 540
Triclinic, P1Dx = 1.362 Mg m3
a = 10.1383 (9) ÅMo Kα radiation, λ = 0.71073 Å
b = 10.6676 (10) ÅCell parameters from 4044 reflections
c = 13.5193 (13) Åθ = 2.2–29.1°
α = 71.919 (2)°µ = 0.76 mm1
β = 88.912 (2)°T = 100 K
γ = 67.725 (2)°Block, yellow
V = 1278.1 (2) Å30.22 × 0.20 × 0.12 mm
Data collection top
Bruker SMART APEX II CCD Platform
diffractometer
7079 reflections with I > 2σ(I)
Radiation source: fine-focus sealed tubeRint = 0.075
ω scansθmax = 33.7°, θmin = 2.2°
Absorption correction: multi-scan
SADABS (Sheldrick, 2008)
h = 1515
Tmin = 0.695, Tmax = 0.747k = 1616
39087 measured reflectionsl = 2121
10151 independent reflections
Refinement top
Refinement on F2Primary atom site location: difference Fourier map
Least-squares matrix: fullSecondary atom site location: difference Fourier map
R[F2 > 2σ(F2)] = 0.061Hydrogen site location: inferred from neighbouring sites
wR(F2) = 0.157H-atom parameters constrained
S = 1.02 w = 1/[σ2(Fo2) + (0.0832P)2]
where P = (Fo2 + 2Fc2)/3
10151 reflections(Δ/σ)max < 0.001
280 parametersΔρmax = 4.57 e Å3
0 restraintsΔρmin = 1.19 e Å3
Crystal data top
[Rh2(CH3)2(C2H6O3P)2(C15H22BN6)2]γ = 67.725 (2)°
Mr = 1048.35V = 1278.1 (2) Å3
Triclinic, P1Z = 1
a = 10.1383 (9) ÅMo Kα radiation
b = 10.6676 (10) ŵ = 0.76 mm1
c = 13.5193 (13) ÅT = 100 K
α = 71.919 (2)°0.22 × 0.20 × 0.12 mm
β = 88.912 (2)°
Data collection top
Bruker SMART APEX II CCD Platform
diffractometer
10151 independent reflections
Absorption correction: multi-scan
SADABS (Sheldrick, 2008)
7079 reflections with I > 2σ(I)
Tmin = 0.695, Tmax = 0.747Rint = 0.075
39087 measured reflections
Refinement top
R[F2 > 2σ(F2)] = 0.0610 restraints
wR(F2) = 0.157H-atom parameters constrained
S = 1.02Δρmax = 4.57 e Å3
10151 reflectionsΔρmin = 1.19 e Å3
280 parameters
Special details top

Experimental. A crystal was placed on the tip of a 0.1 mm diameter glass capillary tube or fiber and mounted on a Bruker SMART APEXII CCD Platform diffractometer for a data collection at 100.0 (5) K. A preliminary set of cell constants and an orientation matrix were calculated from reflections harvested from three orthogonal wedges of reciprocal space. The full data collection was carried out using Mo Kα radiation (graphite monochromator), with a frame time of 60 s and a detector distance of 4.01 cm. A randomly oriented region of reciprocal space was surveyed; six major sections of frames were collected with 0.50° steps in ω at six different ϕ settings and a detector position of -38° in 2θ. The intensity data were corrected for absorption. Final cell constants were calculated from the xyz centroids of 4044 strong reflections from the actual data collection after integration. The space group P1 was determined based on intensity statistics. A direct methods solution was calculated which provided most non-H atoms from the E map. Full-matrix least-squares/difference Fourier cycles were performed which located the remaining non-H atoms. All non-H atoms were refined with anisotropic displacement parameters. All H atoms were placed in ideal positions and refined as riding atoms with relative isotropic displacement parameters.

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. Highly disordered solvent was located in channels parallel to the b axis. Reflection contributions from this solvent were removed using program PLATON, function SQUEEZE (Spek, 2003), which determined there to be 96 electrons in 250 Å3 removed per unit cell. Since the exact identity and amount of solvent could not be determined, no solvent was included in the atom list or molecular formula. (One set of residual peaks did appear to be n-pentane, disordered over an inversion center. However, this did not define the entire solvent area.) Thus all reported items that derive from the molecular formula (e.g., F(000), density, molecular weight, etc.) are known to be incorrect.

The large residual peak of 4.57 electrons per Å3, located 0.74 Å from the rhodium atom, may be the result of residual absorption errors.

Fractional atomic coordinates and isotropic or equivalent isotropic displacement parameters (Å2) top
xyzUiso*/Ueq
Rh10.02530 (3)0.08652 (3)0.13620 (2)0.02025 (8)
N10.1825 (3)0.1340 (3)0.1157 (2)0.0199 (5)
N20.2214 (3)0.1671 (3)0.1981 (2)0.0224 (5)
N30.0743 (3)0.0368 (3)0.2957 (2)0.0226 (5)
N40.1319 (3)0.0244 (3)0.3475 (2)0.0214 (5)
N50.1054 (3)0.2678 (3)0.1777 (2)0.0210 (5)
N60.0217 (3)0.2791 (3)0.2506 (2)0.0201 (5)
B10.1332 (4)0.1716 (4)0.2910 (3)0.0210 (6)
H1B0.17550.20240.34070.025*
C10.2757 (4)0.1502 (4)0.0462 (3)0.0234 (6)
C20.3735 (4)0.1928 (4)0.0842 (3)0.0270 (7)
H20.45080.21040.05040.032*
C30.3354 (4)0.2038 (4)0.1802 (3)0.0261 (7)
C40.0941 (4)0.1671 (4)0.3637 (3)0.0248 (6)
C50.1614 (4)0.1853 (4)0.4594 (3)0.0306 (7)
H50.18620.26640.52100.037*
C60.1844 (4)0.0628 (4)0.4467 (3)0.0255 (7)
C70.2329 (3)0.3788 (4)0.1614 (3)0.0238 (6)
C80.2314 (4)0.4602 (4)0.2228 (3)0.0262 (7)
H80.30770.54420.22620.031*
C90.0966 (4)0.3951 (3)0.2784 (3)0.0228 (6)
C100.2701 (4)0.1286 (4)0.0565 (3)0.0282 (7)
H10A0.18590.10760.06590.042*
H10B0.35720.04810.05900.042*
H10C0.26330.21580.11260.042*
C110.4018 (4)0.2468 (5)0.2548 (3)0.0413 (10)
H11A0.48820.25950.22870.062*
H11B0.42740.17200.32360.062*
H11C0.33320.33710.26120.062*
C120.0468 (5)0.2718 (4)0.3396 (3)0.0369 (9)
H12A0.03970.25330.26380.055*
H12B0.04720.26140.36410.055*
H12C0.11670.36940.37510.055*
C130.2535 (4)0.0249 (4)0.5235 (3)0.0342 (8)
H13A0.33440.00280.49440.051*
H13B0.28800.10600.58890.051*
H13C0.18320.05890.53750.051*
C140.3559 (4)0.4136 (4)0.0851 (3)0.0307 (7)
H14A0.35940.32450.08150.046*
H14B0.34370.47030.01570.046*
H14C0.44550.46870.10770.046*
C150.0353 (4)0.4393 (4)0.3549 (3)0.0326 (8)
H15A0.00560.36180.42250.049*
H15B0.10810.52580.36380.049*
H15C0.04790.45910.32880.049*
C160.2035 (4)0.0506 (4)0.1905 (3)0.0270 (7)
H16A0.23710.09600.24420.040*
H16B0.17850.05290.22090.040*
H16C0.27970.09140.13230.040*
P10.12505 (9)0.18195 (9)0.03113 (7)0.02162 (16)
O10.0448 (3)0.1086 (3)0.10500 (17)0.0258 (5)
O20.1577 (3)0.3492 (3)0.0888 (2)0.0306 (5)
O30.2858 (3)0.1913 (3)0.04296 (19)0.0283 (5)
C170.3566 (4)0.2306 (4)0.1463 (3)0.0311 (7)
H17A0.44930.22160.14020.047*
H17B0.29660.16700.18290.047*
H17C0.37190.33000.18590.047*
C180.0583 (5)0.4104 (4)0.0801 (3)0.0346 (8)
H18A0.10840.51480.10000.052*
H18B0.01570.38700.12680.052*
H18C0.01340.37190.00770.052*
Atomic displacement parameters (Å2) top
U11U22U33U12U13U23
Rh10.02014 (12)0.02771 (14)0.01594 (11)0.01066 (10)0.00302 (8)0.00968 (9)
N10.0209 (12)0.0235 (13)0.0164 (11)0.0091 (10)0.0019 (9)0.0075 (10)
N20.0169 (12)0.0316 (14)0.0205 (12)0.0094 (11)0.0013 (10)0.0110 (11)
N30.0267 (14)0.0288 (14)0.0143 (11)0.0133 (12)0.0019 (10)0.0069 (10)
N40.0209 (12)0.0232 (13)0.0179 (12)0.0063 (10)0.0007 (10)0.0065 (10)
N50.0182 (12)0.0263 (13)0.0199 (12)0.0079 (10)0.0008 (10)0.0103 (11)
N60.0196 (12)0.0239 (13)0.0182 (12)0.0094 (10)0.0006 (9)0.0078 (10)
B10.0178 (15)0.0287 (18)0.0186 (15)0.0094 (13)0.0004 (12)0.0103 (14)
C10.0214 (15)0.0255 (15)0.0239 (15)0.0087 (12)0.0060 (12)0.0099 (13)
C20.0185 (14)0.0383 (19)0.0282 (16)0.0139 (14)0.0059 (12)0.0129 (15)
C30.0188 (14)0.0352 (18)0.0265 (16)0.0113 (13)0.0022 (12)0.0122 (14)
C40.0301 (17)0.0224 (15)0.0201 (15)0.0098 (13)0.0052 (12)0.0055 (12)
C50.0334 (19)0.0297 (18)0.0209 (16)0.0088 (15)0.0021 (14)0.0024 (13)
C60.0227 (15)0.0334 (18)0.0172 (14)0.0070 (13)0.0009 (11)0.0089 (13)
C70.0171 (14)0.0268 (16)0.0247 (15)0.0062 (12)0.0036 (12)0.0080 (13)
C80.0250 (16)0.0202 (15)0.0294 (17)0.0049 (13)0.0039 (13)0.0080 (13)
C90.0261 (16)0.0218 (15)0.0204 (14)0.0099 (13)0.0044 (12)0.0060 (12)
C100.0329 (18)0.0386 (19)0.0238 (16)0.0215 (16)0.0111 (13)0.0156 (14)
C110.032 (2)0.076 (3)0.034 (2)0.034 (2)0.0079 (16)0.026 (2)
C120.052 (2)0.033 (2)0.0282 (18)0.0228 (19)0.0018 (17)0.0047 (15)
C130.036 (2)0.041 (2)0.0183 (15)0.0085 (17)0.0076 (14)0.0083 (15)
C140.0206 (16)0.0353 (19)0.0328 (19)0.0049 (14)0.0019 (13)0.0136 (16)
C150.0340 (19)0.0323 (19)0.038 (2)0.0136 (16)0.0066 (15)0.0193 (16)
C160.0266 (16)0.0392 (19)0.0239 (16)0.0180 (15)0.0069 (13)0.0160 (14)
P10.0219 (4)0.0243 (4)0.0194 (4)0.0089 (3)0.0009 (3)0.0082 (3)
O10.0318 (13)0.0317 (13)0.0153 (10)0.0151 (11)0.0014 (9)0.0062 (9)
O20.0353 (14)0.0246 (12)0.0279 (13)0.0089 (11)0.0030 (11)0.0066 (10)
O30.0250 (12)0.0383 (14)0.0220 (11)0.0114 (11)0.0002 (9)0.0116 (10)
C170.0239 (16)0.039 (2)0.0271 (17)0.0066 (15)0.0035 (13)0.0125 (15)
C180.040 (2)0.0305 (19)0.0320 (19)0.0190 (17)0.0010 (16)0.0011 (15)
Geometric parameters (Å, º) top
Rh1—N52.044 (3)C10—H10A0.9800
Rh1—C162.062 (3)C10—H10B0.9800
Rh1—O1i2.104 (2)C10—H10C0.9800
Rh1—N32.172 (3)C11—H11A0.9800
Rh1—P12.2480 (9)C11—H11B0.9800
Rh1—N12.339 (3)C11—H11C0.9800
N1—C11.339 (4)C12—H12A0.9800
N1—N21.375 (4)C12—H12B0.9800
N2—C31.349 (4)C12—H12C0.9800
N2—B11.529 (4)C13—H13A0.9800
N3—C41.349 (4)C13—H13B0.9800
N3—N41.358 (4)C13—H13C0.9800
N4—C61.351 (4)C14—H14A0.9800
N4—B11.523 (5)C14—H14B0.9800
N5—C71.346 (4)C14—H14C0.9800
N5—N61.375 (4)C15—H15A0.9800
N6—C91.347 (4)C15—H15B0.9800
N6—B11.536 (4)C15—H15C0.9800
B1—H1B1.0000C16—H16A0.9800
C1—C21.400 (5)C16—H16B0.9800
C1—C101.482 (5)C16—H16C0.9800
C2—C31.375 (5)P1—O11.498 (3)
C2—H20.9500P1—O31.602 (3)
C3—C111.492 (5)P1—O21.612 (3)
C4—C51.398 (5)O1—Rh1i2.104 (2)
C4—C121.490 (5)O2—C181.417 (5)
C5—C61.371 (5)O3—C171.446 (4)
C5—H50.9500C17—H17A0.9800
C6—C131.495 (5)C17—H17B0.9800
C7—C81.378 (5)C17—H17C0.9800
C7—C141.489 (5)C18—H18A0.9800
C8—C91.383 (5)C18—H18B0.9800
C8—H80.9500C18—H18C0.9800
C9—C151.492 (5)
N5—Rh1—C1686.29 (12)C8—C9—C15129.2 (3)
N5—Rh1—O1i174.10 (10)C1—C10—H10A109.5
C16—Rh1—O1i88.32 (12)C1—C10—H10B109.5
N5—Rh1—N389.56 (11)H10A—C10—H10B109.5
C16—Rh1—N384.87 (13)C1—C10—H10C109.5
O1i—Rh1—N387.56 (10)H10A—C10—H10C109.5
N5—Rh1—P198.63 (8)H10B—C10—H10C109.5
C16—Rh1—P192.59 (10)C3—C11—H11A109.5
O1i—Rh1—P184.00 (7)C3—C11—H11B109.5
N3—Rh1—P1171.26 (8)H11A—C11—H11B109.5
N5—Rh1—N184.59 (10)C3—C11—H11C109.5
C16—Rh1—N1165.55 (11)H11A—C11—H11C109.5
O1i—Rh1—N1100.22 (9)H11B—C11—H11C109.5
N3—Rh1—N183.89 (10)C4—C12—H12A109.5
P1—Rh1—N199.82 (7)C4—C12—H12B109.5
C1—N1—N2105.5 (3)H12A—C12—H12B109.5
C1—N1—Rh1141.5 (2)C4—C12—H12C109.5
N2—N1—Rh1112.80 (18)H12A—C12—H12C109.5
C3—N2—N1111.1 (3)H12B—C12—H12C109.5
C3—N2—B1127.3 (3)C6—C13—H13A109.5
N1—N2—B1121.4 (2)C6—C13—H13B109.5
C4—N3—N4106.1 (3)H13A—C13—H13B109.5
C4—N3—Rh1135.8 (2)C6—C13—H13C109.5
N4—N3—Rh1118.1 (2)H13A—C13—H13C109.5
C6—N4—N3111.0 (3)H13B—C13—H13C109.5
C6—N4—B1129.2 (3)C7—C14—H14A109.5
N3—N4—B1119.7 (3)C7—C14—H14B109.5
C7—N5—N6106.4 (3)H14A—C14—H14B109.5
C7—N5—Rh1135.7 (2)C7—C14—H14C109.5
N6—N5—Rh1117.3 (2)H14A—C14—H14C109.5
C9—N6—N5109.7 (3)H14B—C14—H14C109.5
C9—N6—B1127.6 (3)C9—C15—H15A109.5
N5—N6—B1122.7 (2)C9—C15—H15B109.5
N4—B1—N2110.5 (3)H15A—C15—H15B109.5
N4—B1—N6108.8 (3)C9—C15—H15C109.5
N2—B1—N6109.1 (3)H15A—C15—H15C109.5
N4—B1—H1B109.5H15B—C15—H15C109.5
N2—B1—H1B109.5Rh1—C16—H16A109.5
N6—B1—H1B109.5Rh1—C16—H16B109.5
N1—C1—C2110.2 (3)H16A—C16—H16B109.5
N1—C1—C10123.4 (3)Rh1—C16—H16C109.5
C2—C1—C10126.4 (3)H16A—C16—H16C109.5
C3—C2—C1106.2 (3)H16B—C16—H16C109.5
C3—C2—H2126.9O1—P1—O3106.79 (13)
C1—C2—H2126.9O1—P1—O2104.61 (14)
N2—C3—C2107.0 (3)O3—P1—O298.02 (14)
N2—C3—C11123.8 (3)O1—P1—Rh1115.92 (10)
C2—C3—C11129.2 (3)O3—P1—Rh1112.81 (10)
N3—C4—C5109.3 (3)O2—P1—Rh1116.77 (10)
N3—C4—C12124.5 (3)P1—O1—Rh1i142.60 (15)
C5—C4—C12126.2 (3)C18—O2—P1122.7 (2)
C6—C5—C4106.5 (3)C17—O3—P1119.2 (2)
C6—C5—H5126.8O3—C17—H17A109.5
C4—C5—H5126.8O3—C17—H17B109.5
N4—C6—C5107.0 (3)H17A—C17—H17B109.5
N4—C6—C13123.7 (3)O3—C17—H17C109.5
C5—C6—C13129.3 (3)H17A—C17—H17C109.5
N5—C7—C8109.9 (3)H17B—C17—H17C109.5
N5—C7—C14125.5 (3)O2—C18—H18A109.5
C8—C7—C14124.6 (3)O2—C18—H18B109.5
C7—C8—C9106.3 (3)H18A—C18—H18B109.5
C7—C8—H8126.9O2—C18—H18C109.5
C9—C8—H8126.9H18A—C18—H18C109.5
N6—C9—C8107.7 (3)H18B—C18—H18C109.5
N6—C9—C15123.1 (3)
C1—N1—N2—C30.4 (4)C1—C2—C3—C11179.3 (4)
Rh1—N1—N2—C3175.6 (2)N4—N3—C4—C51.5 (4)
C1—N1—N2—B1175.6 (3)Rh1—N3—C4—C5177.0 (2)
Rh1—N1—N2—B10.3 (4)N4—N3—C4—C12179.8 (3)
C4—N3—N4—C61.3 (4)Rh1—N3—C4—C121.3 (6)
Rh1—N3—N4—C6177.5 (2)N3—C4—C5—C61.2 (4)
C4—N3—N4—B1177.4 (3)C12—C4—C5—C6179.5 (4)
Rh1—N3—N4—B13.8 (4)N3—N4—C6—C50.6 (4)
C7—N5—N6—C90.1 (3)B1—N4—C6—C5177.9 (3)
Rh1—N5—N6—C9172.5 (2)N3—N4—C6—C13179.5 (3)
C7—N5—N6—B1179.9 (3)B1—N4—C6—C131.9 (5)
Rh1—N5—N6—B17.4 (4)C4—C5—C6—N40.4 (4)
C6—N4—B1—N2116.9 (3)C4—C5—C6—C13179.5 (3)
N3—N4—B1—N261.6 (4)N6—N5—C7—C80.0 (4)
C6—N4—B1—N6123.4 (3)Rh1—N5—C7—C8170.4 (2)
N3—N4—B1—N658.2 (4)N6—N5—C7—C14177.4 (3)
C3—N2—B1—N4123.3 (4)Rh1—N5—C7—C1412.2 (5)
N1—N2—B1—N462.3 (4)N5—C7—C8—C90.1 (4)
C3—N2—B1—N6117.1 (3)C14—C7—C8—C9177.3 (3)
N1—N2—B1—N657.3 (4)N5—N6—C9—C80.2 (4)
C9—N6—B1—N4116.9 (3)B1—N6—C9—C8179.8 (3)
N5—N6—B1—N463.0 (4)N5—N6—C9—C15178.8 (3)
C9—N6—B1—N2122.5 (3)B1—N6—C9—C151.2 (5)
N5—N6—B1—N257.6 (4)C7—C8—C9—N60.2 (4)
N2—N1—C1—C20.2 (4)C7—C8—C9—C15178.8 (3)
Rh1—N1—C1—C2174.2 (3)O3—P1—O1—Rh1i63.0 (3)
N2—N1—C1—C10178.4 (3)O2—P1—O1—Rh1i166.3 (2)
Rh1—N1—C1—C104.4 (6)Rh1—P1—O1—Rh1i63.6 (3)
N1—C1—C2—C30.7 (4)O1—P1—O2—C1885.5 (3)
C10—C1—C2—C3177.9 (3)O3—P1—O2—C18164.7 (3)
N1—N2—C3—C20.8 (4)Rh1—P1—O2—C1844.1 (3)
B1—N2—C3—C2175.7 (3)O1—P1—O3—C1742.6 (3)
N1—N2—C3—C11179.4 (4)O2—P1—O3—C1765.4 (3)
B1—N2—C3—C114.5 (6)Rh1—P1—O3—C17171.1 (2)
C1—C2—C3—N20.9 (4)
Symmetry code: (i) x, y, z.

Experimental details

Crystal data
Chemical formula[Rh2(CH3)2(C2H6O3P)2(C15H22BN6)2]
Mr1048.35
Crystal system, space groupTriclinic, P1
Temperature (K)100
a, b, c (Å)10.1383 (9), 10.6676 (10), 13.5193 (13)
α, β, γ (°)71.919 (2), 88.912 (2), 67.725 (2)
V3)1278.1 (2)
Z1
Radiation typeMo Kα
µ (mm1)0.76
Crystal size (mm)0.22 × 0.20 × 0.12
Data collection
DiffractometerBruker SMART APEX II CCD Platform
diffractometer
Absorption correctionMulti-scan
SADABS (Sheldrick, 2008)
Tmin, Tmax0.695, 0.747
No. of measured, independent and
observed [I > 2σ(I)] reflections
39087, 10151, 7079
Rint0.075
(sin θ/λ)max1)0.781
Refinement
R[F2 > 2σ(F2)], wR(F2), S 0.061, 0.157, 1.02
No. of reflections10151
No. of parameters280
H-atom treatmentH-atom parameters constrained
Δρmax, Δρmin (e Å3)4.57, 1.19

Computer programs: APEX2 (Bruker, 2012), SAINT (Bruker, 2009), SIR97 (Altomare et al., 1999), SHELXL2012 (Sheldrick, 2012), SHELXTL (Sheldrick, 2008).

 

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