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Calcinaksite, KNa[Ca(H2O)][Si4Ol0], a new natural member of the litidionite group, was found in a calcic xenolith from alkaline basalt of the Bellerberg volcano, Eastern Eifel region, Rhineland–Palatinate, Germany. The crystal structure has been studied based on single-crystal X-ray diffraction data. Triclinic unit-cell parameters are: a = 7.021 (2), b = 8.250 (3), c = 10.145 (2) Å, α = 102.23 (2), β = 100.34 (2), γ = 115.09 (3)°, space group P \bar 1. The structure model was determined by the `charge-flipping' method and refined to R = 0.0527 in anisotropic approximation using 3057 I > 3σ(I). Calcinaksite is a hydrous calcium-dominant litidionite-group mineral. The crystal structure of calcinaksite (like other litidionite-group minerals and related compounds) is based on a heteropoly­hedral framework and is characterized by the presence of several types of channels. Calcium forms distorted CaO5Ø (Ø = H2O) octahedra while Na forms NaO5 square pyramids. Nine-coordinated K atoms are located in a channel extending along [010]. Water molecules occupy a channel running along the [100] direction and are characterized by a rather high equivalent isotropic displacement parameter of 0.053 (2) Å2. In calcinaksite, there are three short distances between the water molecule and oxygen atoms, Ow...O3 [2.844 (5) Å], Ow...O9 [2.736 (4) Å] and Ow...Ow [2.843 (7) Å]. These distances correspond to three hydrogen bonds detected by IR data (the bands at 3340, 3170 and 3540 cm−1).

Supporting information

cif

Crystallographic Information File (CIF) https://doi.org/10.1107/S2052520614012992/bp5069sup1.cif
Contains datablocks global, I

hkl

Structure factor file (CIF format) https://doi.org/10.1107/S2052520614012992/bp5069Isup2.hkl
Contains datablock I

CCDC reference: 1006765

Experimental top

Refinement top

Crystal data, data collection and structure refinement details are summarized in Table 1.

Results and discussion top

Computing details top

Data collection: CrysAlis PRO, Agilent Technologies, Version 1.171.34.49 (release 20-01-2011 CrysAlis171 .NET) (compiled Jan 20 2011,15:58:25); cell refinement: CrysAlis PRO, Agilent Technologies, Version 1.171.34.49 (release 20-01-2011 CrysAlis171 .NET) (compiled Jan 20 2011,15:58:25); data reduction: CrysAlis PRO, Agilent Technologies, Version 1.171.34.49 (release 20-01-2011 CrysAlis171 .NET) (compiled Jan 20 2011,15:58:25).

Figures top
[Figure 1]
[Figure 2]
[Figure 3]
[Figure 4]
[Figure 5]
[Figure 6]
[Figure 7]
[Figure 8]
(I) top
Crystal data top
CaKNaO11Si4V = 495.4 (3) Å3
Mr = 392.5Z = 2
Triclinic, P1F(000) = 388
Hall symbol: -P 1Dx = 2.510 Mg m3
a = 7.021 (2) ÅMo Kα radiation, λ = 0.7107 Å
b = 8.250 (3) ÅCell parameters from 1903 reflections
c = 10.145 (2) Åθ = 4.3–57.4°
α = 102.23 (2)°µ = 1.62 mm1
β = 100.34 (2)°T = 293 K
γ = 115.09 (3)°0.25 × 0.18 × 0.13 mm
Data collection top
Xcalibur, Sapphire3
diffractometer
11109 independent reflections
Radiation source: Enhance (Mo) X-ray Source3057 reflections with I > 3σ(I)
Graphite monochromatorRint = 0.073
Detector resolution: 16.0628 pixels mm-1θmax = 57.6°, θmin = 4.3°
ω scansh = 1612
Absorption correction: multi-scan
CrysAlis PRO, Agilent Technologies, Version 1.171.34.49 (release 20-01-2011 CrysAlis171 .NET) (compiled Jan 20 2011,15:58:25) Empirical absorption correction using spherical harmonics, implemented in SCALE3 ABSPACK scaling algorithm.
k = 1619
Tmin = 0.737, Tmax = 1l = 2323
24923 measured reflections
Refinement top
Refinement on F0 constraints
R[F2 > 2σ(F2)] = 0.053Weighting scheme based on measured s.u.'s w = 1/(σ2(F) + 0.0025000002F2)
wR(F2) = 0.075(Δ/σ)max = 0.047
S = 1.06Δρmax = 0.54 e Å3
3057 reflectionsΔρmin = 0.51 e Å3
164 parametersExtinction correction: B-C type 1 Gaussian isotropic (Becker & Coppens, 1974)
0 restraintsExtinction coefficient: 1100 (400)
Crystal data top
CaKNaO11Si4γ = 115.09 (3)°
Mr = 392.5V = 495.4 (3) Å3
Triclinic, P1Z = 2
a = 7.021 (2) ÅMo Kα radiation
b = 8.250 (3) ŵ = 1.62 mm1
c = 10.145 (2) ÅT = 293 K
α = 102.23 (2)°0.25 × 0.18 × 0.13 mm
β = 100.34 (2)°
Data collection top
Xcalibur, Sapphire3
diffractometer
11109 independent reflections
Absorption correction: multi-scan
CrysAlis PRO, Agilent Technologies, Version 1.171.34.49 (release 20-01-2011 CrysAlis171 .NET) (compiled Jan 20 2011,15:58:25) Empirical absorption correction using spherical harmonics, implemented in SCALE3 ABSPACK scaling algorithm.
3057 reflections with I > 3σ(I)
Tmin = 0.737, Tmax = 1Rint = 0.073
24923 measured reflections
Refinement top
R[F2 > 2σ(F2)] = 0.053164 parameters
wR(F2) = 0.0750 restraints
S = 1.06Δρmax = 0.54 e Å3
3057 reflectionsΔρmin = 0.51 e Å3
Fractional atomic coordinates and isotropic or equivalent isotropic displacement parameters (Å2) top
xyzUiso*/Ueq
Ca10.25729 (13)0.73567 (11)0.08326 (7)0.0171 (3)
K0.14714 (16)0.20147 (13)0.49142 (10)0.0263 (3)
Si10.11132 (17)0.39963 (13)0.24679 (10)0.0138 (3)
Na0.7505 (3)0.6953 (3)0.08325 (18)0.0255 (7)
Si20.57768 (17)0.71073 (13)0.36451 (10)0.0144 (3)
Si30.25070 (17)1.10137 (13)0.30732 (10)0.0141 (3)
Si40.33754 (17)0.61793 (14)0.24708 (10)0.0150 (3)
O10.0968 (4)0.3939 (4)0.3013 (3)0.0183 (10)
O20.1242 (5)0.8828 (4)0.2283 (3)0.0205 (10)
O30.3028 (5)0.4210 (4)0.3485 (3)0.0224 (11)
O40.1143 (5)1.2081 (4)0.2586 (3)0.0239 (11)
O50.2893 (5)1.1384 (4)0.4772 (3)0.0215 (10)
O60.5844 (5)0.8104 (4)0.2484 (3)0.0224 (11)
O70.3270 (5)0.5800 (4)0.3673 (3)0.0217 (10)
O80.4969 (5)1.2081 (4)0.2892 (3)0.0207 (10)
O90.4137 (5)0.6427 (4)0.0846 (3)0.0207 (11)
O100.0952 (5)0.4206 (4)0.0948 (3)0.0192 (10)
O_wat0.2839 (8)0.9805 (5)0.0292 (4)0.0529 (19)
Atomic displacement parameters (Å2) top
U11U22U33U12U13U23
Ca10.0181 (3)0.0208 (3)0.0150 (3)0.0113 (3)0.0056 (2)0.0058 (2)
K0.0280 (5)0.0229 (4)0.0297 (4)0.0111 (3)0.0089 (4)0.0145 (3)
Si10.0139 (4)0.0146 (4)0.0164 (4)0.0075 (3)0.0066 (3)0.0081 (3)
Na0.0205 (8)0.0322 (9)0.0243 (8)0.0133 (7)0.0074 (7)0.0080 (7)
Si20.0148 (4)0.0142 (4)0.0143 (4)0.0066 (3)0.0049 (3)0.0054 (3)
Si30.0149 (4)0.0133 (4)0.0150 (4)0.0065 (3)0.0055 (3)0.0061 (3)
Si40.0140 (4)0.0163 (4)0.0167 (4)0.0073 (3)0.0063 (3)0.0075 (3)
O10.0135 (11)0.0249 (12)0.0204 (11)0.0100 (10)0.0072 (9)0.0115 (10)
O20.0221 (13)0.0148 (10)0.0228 (12)0.0072 (10)0.0090 (10)0.0047 (9)
O30.0207 (14)0.0201 (12)0.0267 (13)0.0119 (11)0.0059 (11)0.0045 (10)
O40.0227 (14)0.0213 (12)0.0318 (15)0.0128 (11)0.0077 (12)0.0124 (11)
O50.0269 (14)0.0191 (11)0.0148 (11)0.0072 (11)0.0068 (10)0.0064 (9)
O60.0227 (13)0.0266 (13)0.0202 (12)0.0109 (11)0.0085 (10)0.0123 (10)
O70.0161 (12)0.0247 (12)0.0210 (12)0.0071 (10)0.0062 (10)0.0066 (10)
O80.0169 (12)0.0193 (11)0.0265 (13)0.0064 (10)0.0097 (10)0.0113 (10)
O90.0217 (13)0.0253 (13)0.0195 (12)0.0125 (11)0.0079 (10)0.0116 (10)
O100.0214 (13)0.0199 (11)0.0185 (11)0.0089 (10)0.0082 (10)0.0106 (9)
O_wat0.068 (3)0.0262 (17)0.0371 (19)0.0049 (18)0.0008 (19)0.0117 (15)
Geometric parameters (Å, º) top
Ca1—Ca1i3.760 (5)K—O3ix2.821 (4)
Ca1—Kii4.481 (2)K—O5ii2.661 (4)
Ca1—Naiii3.430 (3)K—O7ii2.896 (4)
Ca1—Na3.617 (3)Si1—O11.639 (4)
Ca1—Naiv3.571 (4)Si1—O4x1.618 (4)
Ca1—O22.283 (4)Si1—O71.630 (3)
Ca1—O62.333 (4)Si1—O101.577 (3)
Ca1—O92.351 (4)Na—Naiv3.400 (5)
Ca1—O102.394 (4)Na—O2xi2.377 (4)
Ca1—O10i2.398 (4)Si2—O3iv1.631 (4)
K—Kv4.714 (4)Si2—O5xii1.621 (3)
K—Kvi4.614 (3)Si2—O61.569 (4)
K—Kii4.409 (5)Si2—O71.638 (4)
K—Si13.598 (2)Si3—O21.567 (3)
K—Si1ii3.647 (3)Si3—O41.633 (4)
K—Navii4.384 (3)Si3—O51.636 (3)
K—Si2viii3.471 (4)Si3—O81.640 (4)
K—Si2vii3.694 (3)Si4—O1i1.635 (3)
K—Si3ii3.478 (2)Si4—O31.620 (4)
K—Si4ix3.661 (4)Si4—O8xiii1.618 (4)
K—Si4i3.495 (2)Si4—O91.579 (3)
K—O12.726 (4)
Ca1i—Ca1—Kii92.34 (4)Si2viii—K—Si2vii99.88 (6)
Ca1i—Ca1—Naiii59.35 (5)Si2viii—K—Si3ii53.34 (4)
Ca1i—Ca1—Na111.96 (6)Si2viii—K—Si4ix144.34 (6)
Ca1i—Ca1—Naiv55.72 (5)Si2viii—K—Si4i110.36 (5)
Ca1i—Ca1—O297.99 (8)Si2viii—K—O1118.59 (7)
Ca1i—Ca1—O6128.08 (9)Si2viii—K—O3ix123.75 (10)
Ca1i—Ca1—O989.49 (7)Si2viii—K—O5ii26.72 (7)
Ca1i—Ca1—O1038.36 (8)Si2viii—K—O7ii122.97 (7)
Ca1i—Ca1—O10i38.29 (9)Si2vii—K—Si3ii81.44 (5)
Kii—Ca1—Naiii65.75 (4)Si2vii—K—Si4ix49.21 (4)
Kii—Ca1—Na112.11 (4)Si2vii—K—Si4i128.04 (5)
Kii—Ca1—Naiv115.95 (5)Si2vii—K—O1101.23 (7)
Kii—Ca1—O238.88 (9)Si2vii—K—O3ix24.64 (8)
Kii—Ca1—O672.31 (9)Si2vii—K—O5ii87.92 (9)
Kii—Ca1—O9151.85 (10)Si2vii—K—O7ii122.79 (7)
Kii—Ca1—O1075.45 (8)Si3ii—K—Si4ix98.86 (5)
Kii—Ca1—O10i108.36 (9)Si3ii—K—Si4i150.31 (5)
Naiii—Ca1—Na170.17 (6)Si3ii—K—O1171.93 (6)
Naiii—Ca1—Naiv115.07 (6)Si3ii—K—O3ix92.75 (9)
Naiii—Ca1—O243.67 (8)Si3ii—K—O5ii26.94 (7)
Naiii—Ca1—O6137.87 (10)Si3ii—K—O7ii94.63 (8)
Naiii—Ca1—O9136.63 (8)Si4ix—K—Si4i103.98 (5)
Naiii—Ca1—O1083.60 (11)Si4ix—K—O188.53 (6)
Naiii—Ca1—O10i46.54 (10)Si4ix—K—O3ix24.88 (8)
Na—Ca1—Naiv56.45 (6)Si4ix—K—O5ii121.30 (8)
Na—Ca1—O2140.45 (8)Si4ix—K—O7ii75.76 (7)
Na—Ca1—O642.27 (10)Si4i—K—O127.03 (7)
Na—Ca1—O942.41 (9)Si4i—K—O3ix115.77 (9)
Na—Ca1—O1086.58 (11)Si4i—K—O5ii134.62 (7)
Na—Ca1—O10i130.22 (10)Si4i—K—O7ii73.25 (8)
Naiv—Ca1—O2147.26 (9)O1—K—O3ix92.64 (9)
Naiv—Ca1—O686.39 (10)O1—K—O5ii145.05 (9)
Naiv—Ca1—O944.96 (9)O1—K—O7ii90.31 (11)
Naiv—Ca1—O1044.07 (10)O3ix—K—O5ii107.36 (12)
Naiv—Ca1—O10i80.46 (10)O3ix—K—O7ii100.27 (10)
O2—Ca1—O698.85 (12)O5ii—K—O7ii113.06 (11)
O2—Ca1—O9167.10 (13)K—Si1—Kii74.96 (5)
O2—Ca1—O10103.36 (13)K—Si1—O145.95 (13)
O2—Ca1—O10i89.27 (12)K—Si1—O4x64.10 (13)
O6—Ca1—O984.53 (12)K—Si1—O795.75 (13)
O6—Ca1—O1089.90 (12)K—Si1—O10150.25 (12)
O6—Ca1—O10i165.64 (13)Kii—Si1—O156.46 (10)
O9—Ca1—O1089.03 (12)Kii—Si1—O4x131.97 (12)
O9—Ca1—O10i90.17 (12)Kii—Si1—O750.43 (15)
O10—Ca1—O10i76.65 (12)Kii—Si1—O10113.72 (14)
Ca1ii—K—Kv62.54 (4)O1—Si1—O4x104.25 (19)
Ca1ii—K—Kvi97.43 (3)O1—Si1—O7104.00 (17)
Ca1ii—K—Kii99.41 (4)O1—Si1—O10113.23 (19)
Ca1ii—K—Si1151.00 (4)O4x—Si1—O7108.51 (18)
Ca1ii—K—Si1ii48.31 (3)O4x—Si1—O10114.30 (18)
Ca1ii—K—Navii45.52 (4)O7—Si1—O10111.78 (16)
Ca1ii—K—Si2viii97.03 (4)Ca1—Na—Ca1xi170.17 (8)
Ca1ii—K—Si2vii92.66 (4)Ca1—Na—Ca1iv123.55 (6)
Ca1ii—K—Si3ii48.51 (3)Ca1—Na—Kvii112.72 (6)
Ca1ii—K—Si4ix71.24 (4)Ca1—Na—Naiv61.10 (7)
Ca1ii—K—Si4i122.90 (4)Ca1—Na—O2xi132.96 (13)
Ca1ii—K—O1138.23 (8)Ca1xi—Na—Ca1iv64.93 (6)
Ca1ii—K—O3ix83.88 (8)Ca1xi—Na—Kvii68.73 (5)
Ca1ii—K—O5ii73.75 (8)Ca1xi—Na—Naiv127.09 (9)
Ca1ii—K—O7ii50.02 (7)Ca1xi—Na—O2xi41.54 (10)
Kv—K—Kvi97.64 (5)Ca1iv—Na—Kvii96.64 (7)
Kv—K—Kii129.75 (5)Ca1iv—Na—Naiv62.45 (7)
Kv—K—Si1139.72 (4)Ca1iv—Na—O2xi101.32 (13)
Kv—K—Si1ii91.17 (5)Kvii—Na—Naiv122.17 (8)
Kv—K—Navii99.49 (5)Kvii—Na—O2xi41.93 (9)
Kv—K—Si2viii53.48 (4)Naiv—Na—O2xi158.61 (15)
Kv—K—Si2vii136.50 (5)Kxiv—Si2—Kvii80.12 (5)
Kv—K—Si3ii55.19 (4)Kxiv—Si2—O3iv124.92 (10)
Kv—K—Si4ix133.19 (5)Kxiv—Si2—O5xii47.55 (13)
Kv—K—Si4i95.15 (4)Kxiv—Si2—O664.65 (10)
Kv—K—O1121.29 (7)Kxiv—Si2—O7123.75 (14)
Kv—K—O3ix143.66 (8)Kvii—Si2—O3iv46.15 (9)
Kv—K—O5ii52.32 (9)Kvii—Si2—O5xii64.73 (15)
Kv—K—O7ii69.51 (7)Kvii—Si2—O6105.89 (14)
Kvi—K—Kii132.20 (4)Kvii—Si2—O7140.03 (15)
Kvi—K—Si196.70 (4)O3iv—Si2—O5xii104.11 (18)
Kvi—K—Si1ii134.19 (4)O3iv—Si2—O6112.9 (2)
Kvi—K—Navii66.17 (5)O3iv—Si2—O7107.94 (18)
Kvi—K—Si2viii52.06 (4)O5xii—Si2—O6112.16 (16)
Kvi—K—Si2vii47.82 (4)O5xii—Si2—O7105.79 (17)
Kvi—K—Si3ii55.37 (4)O6—Si2—O7113.24 (18)
Kvi—K—Si4ix95.06 (5)Kii—Si3—O261.58 (13)
Kvi—K—Si4i139.02 (4)Kii—Si3—O4129.50 (13)
Kvi—K—O1121.05 (8)Kii—Si3—O547.47 (12)
Kvi—K—O3ix71.96 (9)Kii—Si3—O8120.16 (15)
Kvi—K—O5ii45.50 (9)O2—Si3—O4112.94 (17)
Kvi—K—O7ii147.44 (8)O2—Si3—O5108.82 (17)
Kii—K—Si153.03 (4)O2—Si3—O8113.5 (2)
Kii—K—Si1ii52.01 (4)O4—Si3—O5107.17 (19)
Kii—K—Navii96.19 (5)O4—Si3—O8108.03 (19)
Kii—K—Si2viii161.90 (4)O5—Si3—O8106.01 (16)
Kii—K—Si2vii86.91 (5)Kxv—Si4—Ki76.02 (5)
Kii—K—Si3ii144.74 (4)Kxv—Si4—O1i56.00 (11)
Kii—K—Si4ix50.29 (4)Kxv—Si4—O347.12 (13)
Kii—K—Si4i53.69 (4)Kxv—Si4—O8xiii122.71 (11)
Kii—K—O143.33 (6)Kxv—Si4—O9124.15 (11)
Kii—K—O3ix65.87 (9)Ki—Si4—O1i49.27 (12)
Kii—K—O5ii171.22 (7)Ki—Si4—O3102.18 (13)
Kii—K—O7ii64.36 (7)Ki—Si4—O8xiii57.64 (13)
Si1—K—Si1ii105.04 (5)Ki—Si4—O9144.59 (15)
Si1—K—Navii120.73 (5)O1i—Si4—O3102.75 (16)
Si1—K—Si2viii111.61 (5)O1i—Si4—O8xiii104.22 (19)
Si1—K—Si2vii78.44 (4)O1i—Si4—O9114.03 (19)
Si1—K—Si3ii152.07 (5)O3—Si4—O8xiii109.27 (18)
Si1—K—Si4ix82.39 (5)O3—Si4—O9112.7 (2)
Si1—K—Si4i51.69 (4)O8xiii—Si4—O9113.08 (14)
Si1—K—O125.60 (8)K—O1—Si1108.45 (18)
Si1—K—O3ix76.63 (8)K—O1—Si4i103.71 (14)
Si1—K—O5ii132.51 (9)Si1—O1—Si4i141.8 (2)
Si1—K—O7ii112.52 (8)Ca1—O2—Naiii94.79 (11)
Si1ii—K—Navii68.05 (5)Ca1—O2—Si3122.60 (19)
Si1ii—K—Si2viii141.79 (5)Naiii—O2—Si3127.6 (2)
Si1ii—K—Si2vii97.61 (5)Kxv—O3—Si2iv109.21 (12)
Si1ii—K—Si3ii96.63 (5)Kxv—O3—Si4108.00 (19)
Si1ii—K—Si4ix50.08 (4)Si2iv—O3—Si4140.87 (19)
Si1ii—K—Si4i84.01 (5)Si1xvi—O4—Si3149.87 (18)
Si1ii—K—O190.59 (8)Kii—O5—Si2xii105.73 (17)
Si1ii—K—O3ix74.58 (9)Kii—O5—Si3105.59 (14)
Si1ii—K—O5ii121.88 (9)Si2xii—O5—Si3146.5 (2)
Si1ii—K—O7ii25.71 (6)Ca1—O6—Si2120.13 (16)
Navii—K—Si2viii100.73 (6)Kii—O7—Si1103.86 (18)
Navii—K—Si2vii47.18 (4)Kii—O7—Si2113.12 (15)
Navii—K—Si3ii52.27 (5)Si1—O7—Si2131.9 (2)
Navii—K—Si4ix46.82 (4)Si3—O8—Si4xiii145.0 (3)
Navii—K—Si4i148.52 (5)Ca1—O9—Si4124.8 (2)
Navii—K—O1134.67 (6)Ca1—O10—Ca1i103.35 (15)
Navii—K—O3ix44.23 (8)Ca1—O10—Si1116.90 (14)
Navii—K—O5ii75.11 (8)Ca1i—O10—Si1119.90 (17)
Navii—K—O7ii86.00 (8)
Symmetry codes: (i) x, y+1, z; (ii) x, y+1, z+1; (iii) x1, y, z; (iv) x+1, y+1, z; (v) x1, y, z+1; (vi) x, y, z+1; (vii) x+1, y+1, z+1; (viii) x1, y1, z; (ix) x, y, z+1; (x) x, y1, z; (xi) x+1, y, z; (xii) x+1, y+2, z+1; (xiii) x+1, y+2, z; (xiv) x+1, y+1, z; (xv) x, y, z1; (xvi) x, y+1, z.

Experimental details

Crystal data
Chemical formulaCaKNaO11Si4
Mr392.5
Crystal system, space groupTriclinic, P1
Temperature (K)293
a, b, c (Å)7.021 (2), 8.250 (3), 10.145 (2)
α, β, γ (°)102.23 (2), 100.34 (2), 115.09 (3)
V3)495.4 (3)
Z2
Radiation typeMo Kα
µ (mm1)1.62
Crystal size (mm)0.25 × 0.18 × 0.13
Data collection
DiffractometerXcalibur, Sapphire3
diffractometer
Absorption correctionMulti-scan
CrysAlis PRO, Agilent Technologies, Version 1.171.34.49 (release 20-01-2011 CrysAlis171 .NET) (compiled Jan 20 2011,15:58:25) Empirical absorption correction using spherical harmonics, implemented in SCALE3 ABSPACK scaling algorithm.
Tmin, Tmax0.737, 1
No. of measured, independent and
observed [I > 3σ(I)] reflections
24923, 11109, 3057
Rint0.073
(sin θ/λ)max1)1.187
Refinement
R[F2 > 2σ(F2)], wR(F2), S 0.053, 0.075, 1.06
No. of reflections3057
No. of parameters164
Δρmax, Δρmin (e Å3)0.54, 0.51

Computer programs: CrysAlis PRO, Agilent Technologies, Version 1.171.34.49 (release 20-01-2011 CrysAlis171 .NET) (compiled Jan 20 2011,15:58:25).

 

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