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An ordered polymorph of CuSm3Se6 crystallizes in the monoclinic space group P21/m. The structure, which contains both monoselenide (Se2-) and diselenide (Se22-) units, comprises a three-dimensional network built from SmSe8 polyhedra and distorted CuSe4 tetrahedra.

Supporting information

cif

Crystallographic Information File (CIF) https://doi.org/10.1107/S1600536804015776/wm6023sup1.cif
Contains datablocks global, I

hkl

Structure factor file (CIF format) https://doi.org/10.1107/S1600536804015776/wm6023Isup2.hkl
Contains datablock I

Key indicators

  • Single-crystal X-ray study
  • T = 153 K
  • Mean [sigma](Se-Se) = 0.002 Å
  • R factor = 0.039
  • wR factor = 0.103
  • Data-to-parameter ratio = 24.8

checkCIF/PLATON results

No syntax errors found



Alert level A PLAT029_ALERT_3_A _diffrn_measured_fraction_theta_full Low ....... 0.93
Alert level B PLAT112_ALERT_2_B ADDSYM Detects Additional (Pseudo) Symm. Elem... c PLAT112_ALERT_2_B ADDSYM Detects Additional (Pseudo) Symm. Elem... b PLAT113_ALERT_2_B ADDSYM Suggests Possible Pseudo/New Spacegroup . Pbcm
Alert level C DIFMX01_ALERT_2_C The maximum difference density is > 0.1*ZMAX*0.75 _refine_diff_density_max given = 5.306 Test value = 4.650 DIFMX02_ALERT_1_C The minimum difference density is > 0.1*ZMAX*0.75 The relevant atom site should be identified. REFLT03_ALERT_3_C Reflection count < 95% complete From the CIF: _diffrn_reflns_theta_max 28.99 From the CIF: _diffrn_reflns_theta_full 0.00 From the CIF: _reflns_number_total 2435 TEST2: Reflns within _diffrn_reflns_theta_max Count of symmetry unique reflns 2628 Completeness (_total/calc) 92.66% PLAT097_ALERT_2_C Maximum (Positive) Residual Density ............ 5.31 e/A   3 PLAT152_ALERT_1_C Supplied and Calc Volume s.u. Inconsistent ..... ?
1 ALERT level A = In general: serious problem 3 ALERT level B = Potentially serious problem 5 ALERT level C = Check and explain 0 ALERT level G = General alerts; check 2 ALERT type 1 CIF construction/syntax error, inconsistent or missing data 5 ALERT type 2 Indicator that the structure model may be wrong or deficient 2 ALERT type 3 Indicator that the structure quality may be low 0 ALERT type 4 Improvement, methodology, query or suggestion

Computing details top

Data collection: SMART (Bruker, 2003); cell refinement: SAINT (Bruker, 2003); data reduction: SAINT; program(s) used to solve structure: SHELXTL (Sheldrick, 2003); program(s) used to refine structure: SHELXTL; molecular graphics: XP in SHELXTL; software used to prepare material for publication: SHELXTL.

(I) top
Crystal data top
CuSm3Se6F(000) = 1676
Mr = 988.35Dx = 6.860 Mg m3
Monoclinic, P21/mMo Kα radiation, λ = 0.71073 Å
Hall symbol: -P 2ybCell parameters from 4189 reflections
a = 7.1357 (10) Åθ = 2.6–29.0°
b = 16.986 (3) ŵ = 43.07 mm1
c = 7.8957 (12) ÅT = 153 K
β = 90.585 (2)°Needle, red
V = 957.0 (2) Å30.24 × 0.05 × 0.04 mm
Z = 4
Data collection top
Bruker 1000 CCD
diffractometer
2435 independent reflections
Radiation source: fine-focus sealed tube1976 reflections with I > 2σ(I)
Graphite monochromatorRint = 0.048
ω scansθmax = 29.0°, θmin = 2.6°
Absorption correction: numerical
face indexed (SHELXTL)
h = 99
Tmin = 0.029, Tmax = 0.210k = 2223
11410 measured reflectionsl = 1010
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)] = 0.039 w = 1/[σ2(Fo2) + (0.04P)2 + 34P]
where P = (Fo2 + 2Fc2)/3
wR(F2) = 0.103(Δ/σ)max = 0.002
S = 1.05Δρmax = 5.31 e Å3
2435 reflectionsΔρmin = 3.74 e Å3
98 parametersExtinction correction: SHELXTL, Fc*=kFc[1+0.001xFc2λ3/sin(2θ)]-1/4
0 restraintsExtinction coefficient: 0.00117 (8)
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. Refinement of F2 against ALL reflections. The weighted R-factor wR and goodness of fit S are based on F2, conventional R-factors R are based on F, with F set to zero for negative F2. The threshold expression of F2 > σ(F2) is used only for calculating R-factors(gt) etc. and is not relevant to the choice of reflections for refinement. R-factors based on F2 are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger.

Fractional atomic coordinates and isotropic or equivalent isotropic displacement parameters (Å2) top
xyzUiso*/Ueq
Sm10.25766 (7)0.08696 (3)0.44000 (6)0.00550 (16)
Sm20.27305 (7)0.58962 (3)0.05685 (7)0.00589 (16)
Sm30.23408 (10)0.25000.05439 (9)0.00612 (18)
Sm40.76271 (10)0.25000.55643 (9)0.00541 (18)
Cu0.1045 (2)0.02915 (11)0.7935 (2)0.0256 (4)
Se10.11069 (14)0.08227 (5)0.09093 (13)0.0059 (2)
Se20.11745 (14)0.58195 (5)0.40358 (13)0.0053 (2)
Se30.41961 (13)0.17705 (6)0.74452 (12)0.0059 (2)
Se40.57020 (13)0.00053 (5)0.25244 (12)0.0054 (2)
Se50.57110 (13)0.17658 (6)0.24961 (12)0.0058 (2)
Se60.11781 (19)0.25000.39813 (18)0.0062 (3)
Se70.87119 (19)0.25000.90384 (18)0.0058 (3)
Atomic displacement parameters (Å2) top
U11U22U33U12U13U23
Sm10.0061 (3)0.0036 (3)0.0068 (3)0.00058 (17)0.0013 (2)0.00016 (17)
Sm20.0063 (3)0.0041 (3)0.0072 (3)0.00098 (17)0.00172 (19)0.00024 (17)
Sm30.0069 (4)0.0039 (3)0.0076 (4)0.0000.0012 (3)0.000
Sm40.0058 (3)0.0034 (3)0.0069 (4)0.0000.0019 (3)0.000
Cu0.0152 (8)0.0418 (10)0.0198 (8)0.0095 (7)0.0011 (6)0.0081 (7)
Se10.0056 (5)0.0036 (4)0.0083 (5)0.0015 (3)0.0028 (4)0.0006 (3)
Se20.0047 (5)0.0034 (5)0.0079 (5)0.0003 (3)0.0015 (4)0.0003 (3)
Se30.0048 (4)0.0051 (5)0.0075 (5)0.0004 (3)0.0021 (3)0.0000 (3)
Se40.0032 (4)0.0046 (5)0.0083 (5)0.0002 (3)0.0021 (3)0.0001 (4)
Se50.0043 (4)0.0055 (5)0.0076 (5)0.0001 (3)0.0016 (3)0.0001 (3)
Se60.0062 (6)0.0031 (6)0.0093 (7)0.0000.0004 (5)0.000
Se70.0058 (6)0.0030 (6)0.0086 (7)0.0000.0026 (5)0.000
Geometric parameters (Å, º) top
Sm1—Se12.9400 (12)Sm4—Se5ii3.0374 (12)
Sm1—Se2i2.9606 (12)Sm4—Se33.1320 (12)
Sm1—Se62.9611 (8)Sm4—Se3ii3.1320 (12)
Sm1—Se2ii3.0512 (11)Cu—Se2i2.3840 (18)
Sm1—Se43.0643 (11)Cu—Se4iii2.4063 (18)
Sm1—Se33.0662 (11)Cu—Se1xiv2.516 (2)
Sm1—Se4iii3.0909 (11)Cu—Se1xv2.608 (2)
Sm1—Se53.1062 (11)Cu—Sm2i3.1266 (16)
Sm1—Cu3.1639 (17)Cu—Sm2xvi3.1288 (17)
Sm2—Se7iv2.9300 (8)Se1—Cuxi2.516 (2)
Sm2—Se22.9676 (12)Se1—Cuxv2.608 (2)
Sm2—Se1v2.9682 (12)Se1—Sm2xvii2.9682 (12)
Sm2—Se4ii3.0263 (11)Se1—Sm2ii3.1536 (11)
Sm2—Se5vi3.0544 (11)Se2—Cuviii2.3840 (18)
Sm2—Se3vii3.0667 (11)Se2—Sm1viii2.9605 (12)
Sm2—Se4vi3.0920 (11)Se2—Sm4iv2.9957 (10)
Sm2—Cuviii3.1266 (16)Se2—Sm1ii3.0513 (11)
Sm2—Cuix3.1288 (17)Se3—Se3ii2.479 (2)
Sm2—Se1ii3.1536 (11)Se3—Sm3xiv3.0563 (12)
Sm3—Se7x2.8381 (16)Se3—Sm2xiii3.0667 (11)
Sm3—Se62.8461 (16)Se4—Cuiii2.4063 (18)
Sm3—Se12.9968 (10)Se4—Sm2ii3.0263 (11)
Sm3—Se1ii2.9969 (10)Se4—Sm1iii3.0909 (11)
Sm3—Se3xi3.0563 (12)Se4—Sm2xviii3.0919 (11)
Sm3—Se3ix3.0563 (12)Se5—Se5ii2.494 (2)
Sm3—Se53.1047 (12)Se5—Sm2xviii3.0543 (11)
Sm3—Se5ii3.1047 (12)Se6—Sm4xix2.8368 (16)
Sm4—Se6xii2.8368 (16)Se6—Sm1ii2.9611 (8)
Sm4—Se72.8426 (16)Se7—Sm3xx2.8382 (16)
Sm4—Se2xiii2.9956 (10)Se7—Sm2xiii2.9299 (8)
Sm4—Se2iv2.9957 (10)Se7—Sm2iv2.9300 (8)
Sm4—Se53.0374 (12)
Se1—Sm1—Se2i94.30 (3)Se7—Sm4—Se2iv79.84 (3)
Se1—Sm1—Se678.70 (3)Se2xiii—Sm4—Se2iv144.69 (5)
Se2i—Sm1—Se676.60 (3)Se6xii—Sm4—Se592.60 (4)
Se1—Sm1—Se2ii76.86 (3)Se7—Sm4—Se5152.32 (3)
Se2i—Sm1—Se2ii73.46 (3)Se2xiii—Sm4—Se579.54 (3)
Se6—Sm1—Se2ii139.39 (4)Se2iv—Sm4—Se5126.94 (3)
Se1—Sm1—Se477.78 (3)Se6xii—Sm4—Se5ii92.60 (4)
Se2i—Sm1—Se4148.59 (3)Se7—Sm4—Se5ii152.32 (3)
Se6—Sm1—Se4129.81 (4)Se2xiii—Sm4—Se5ii126.94 (3)
Se2ii—Sm1—Se475.14 (3)Se2iv—Sm4—Se5ii79.54 (3)
Se1—Sm1—Se3151.24 (3)Se5—Sm4—Se5ii48.48 (4)
Se2i—Sm1—Se391.28 (3)Se6xii—Sm4—Se3156.20 (2)
Se6—Sm1—Se375.21 (3)Se7—Sm4—Se375.46 (4)
Se2ii—Sm1—Se3131.59 (3)Se2xiii—Sm4—Se378.27 (3)
Se4—Sm1—Se3110.35 (3)Se2iv—Sm4—Se3123.42 (3)
Se1—Sm1—Se4iii149.16 (3)Se5—Sm4—Se382.42 (3)
Se2i—Sm1—Se4iii90.70 (3)Se5ii—Sm4—Se3101.13 (3)
Se6—Sm1—Se4iii131.92 (4)Se6xii—Sm4—Se3ii156.20 (2)
Se2ii—Sm1—Se4iii75.48 (3)Se7—Sm4—Se3ii75.46 (4)
Se4—Sm1—Se4iii82.18 (3)Se2xiii—Sm4—Se3ii123.42 (3)
Se3—Sm1—Se4iii58.69 (3)Se2iv—Sm4—Se3ii78.27 (3)
Se1—Sm1—Se579.12 (3)Se5—Sm4—Se3ii101.13 (3)
Se2i—Sm1—Se5150.99 (3)Se5ii—Sm4—Se3ii82.42 (3)
Se6—Sm1—Se574.40 (3)Se3—Sm4—Se3ii46.62 (4)
Se2ii—Sm1—Se5130.71 (3)Se2i—Cu—Se4iii128.02 (7)
Se4—Sm1—Se557.98 (3)Se2i—Cu—Se1xiv118.65 (7)
Se3—Sm1—Se582.38 (3)Se4iii—Cu—Se1xiv102.01 (7)
Se4iii—Sm1—Se5109.48 (3)Se2i—Cu—Se1xv96.41 (6)
Se1—Sm1—Cu134.06 (4)Se4iii—Cu—Se1xv118.23 (7)
Se2i—Sm1—Cu45.67 (3)Se1xiv—Cu—Se1xv86.47 (6)
Se6—Sm1—Cu105.65 (4)Se2i—Cu—Sm2i63.50 (4)
Se2ii—Sm1—Cu71.06 (4)Se4iii—Cu—Sm2i164.16 (8)
Se4—Sm1—Cu122.50 (4)Se1xiv—Cu—Sm2i62.37 (4)
Se3—Sm1—Cu66.04 (4)Se1xv—Cu—Sm2i66.01 (4)
Se4iii—Sm1—Cu45.23 (3)Se2i—Cu—Sm2xvi157.61 (8)
Se5—Sm1—Cu146.71 (4)Se4iii—Cu—Sm2xvi66.44 (4)
Se7iv—Sm2—Se278.93 (3)Se1xiv—Cu—Sm2xvi66.91 (4)
Se7iv—Sm2—Se1v75.94 (3)Se1xv—Cu—Sm2xvi61.52 (4)
Se2—Sm2—Se1v90.48 (3)Sm2i—Cu—Sm2xvi106.70 (5)
Se7iv—Sm2—Se4ii131.41 (4)Se2i—Cu—Sm162.66 (4)
Se2—Sm2—Se4ii76.93 (3)Se4iii—Cu—Sm165.78 (4)
Se1v—Sm2—Se4ii144.90 (3)Se1xiv—Cu—Sm1135.17 (7)
Se7iv—Sm2—Se5vi76.43 (3)Se1xv—Cu—Sm1138.06 (7)
Se2—Sm2—Se5vi153.48 (3)Sm2i—Cu—Sm1122.56 (5)
Se1v—Sm2—Se5vi92.91 (3)Sm2xvi—Cu—Sm1130.73 (5)
Se4ii—Sm2—Se5vi112.96 (3)Cuxi—Se1—Cuxv93.54 (6)
Se7iv—Sm2—Se3vii75.27 (3)Cuxi—Se1—Sm1152.56 (5)
Se2—Sm2—Se3vii79.74 (3)Cuxv—Se1—Sm184.10 (5)
Se1v—Sm2—Se3vii150.86 (3)Cuxi—Se1—Sm2xvii68.95 (4)
Se4ii—Sm2—Se3vii59.36 (3)Cuxv—Se1—Sm2xvii67.91 (4)
Se5vi—Sm2—Se3vii84.65 (3)Sm1—Se1—Sm2xvii133.33 (4)
Se7iv—Sm2—Se4vi131.99 (4)Cuxi—Se1—Sm3104.68 (5)
Se2—Sm2—Se4vi148.09 (3)Cuxv—Se1—Sm3153.92 (6)
Se1v—Sm2—Se4vi90.50 (3)Sm1—Se1—Sm387.83 (3)
Se4ii—Sm2—Se4vi84.16 (3)Sm2xvii—Se1—Sm3101.12 (3)
Se5vi—Sm2—Se4vi58.23 (3)Cuxi—Se1—Sm2ii65.88 (4)
Se3vii—Sm2—Se4vi112.23 (3)Cuxv—Se1—Sm2ii64.92 (4)
Se7iv—Sm2—Cuviii87.73 (4)Sm1—Se1—Sm2ii88.70 (3)
Se2—Sm2—Cuviii45.97 (4)Sm2xvii—Se1—Sm2ii110.10 (3)
Se1v—Sm2—Cuviii48.68 (4)Sm3—Se1—Sm2ii139.77 (4)
Se4ii—Sm2—Cuviii104.06 (4)Cuviii—Se2—Sm1viii71.67 (5)
Se5vi—Sm2—Cuviii141.30 (4)Cuviii—Se2—Sm270.54 (5)
Se3vii—Sm2—Cuviii125.47 (4)Sm1viii—Se2—Sm2137.05 (4)
Se4vi—Sm2—Cuviii117.25 (4)Cuviii—Se2—Sm4iv127.90 (6)
Se7iv—Sm2—Cuix122.47 (5)Sm1viii—Se2—Sm4iv100.77 (3)
Se2—Sm2—Cuix116.10 (4)Sm2—Se2—Sm4iv86.92 (3)
Se1v—Sm2—Cuix50.57 (4)Cuviii—Se2—Sm1ii85.57 (5)
Se4ii—Sm2—Cuix105.99 (4)Sm1viii—Se2—Sm1ii106.54 (3)
Se5vi—Sm2—Cuix85.75 (4)Sm2—Se2—Sm1ii90.16 (3)
Se3vii—Sm2—Cuix156.95 (4)Sm4iv—Se2—Sm1ii142.48 (4)
Se4vi—Sm2—Cuix45.51 (3)Se3ii—Se3—Sm3xiv66.078 (19)
Cuviii—Sm2—Cuix73.30 (5)Se3ii—Se3—Sm1119.94 (2)
Se7iv—Sm2—Se1ii136.22 (4)Sm3xiv—Se3—Sm1131.86 (4)
Se2—Sm2—Se1ii74.90 (3)Se3ii—Se3—Sm2xiii118.96 (2)
Se1v—Sm2—Se1ii69.90 (3)Sm3xiv—Se3—Sm2xiii95.76 (3)
Se4ii—Sm2—Se1ii75.17 (3)Sm1—Se3—Sm2xiii114.91 (3)
Se5vi—Sm2—Se1ii130.72 (3)Se3ii—Se3—Sm466.692 (19)
Se3vii—Sm2—Se1ii131.77 (3)Sm3xiv—Se3—Sm4124.49 (3)
Se4vi—Sm2—Se1ii75.55 (3)Sm1—Se3—Sm496.65 (3)
Cuviii—Sm2—Se1ii49.07 (4)Sm2xiii—Se3—Sm482.86 (3)
Cuix—Sm2—Se1ii47.21 (4)Cuiii—Se4—Sm2ii119.28 (6)
Se7x—Sm3—Se697.23 (5)Cuiii—Se4—Sm1151.77 (6)
Se7x—Sm3—Se176.86 (2)Sm2ii—Se4—Sm188.82 (3)
Se6—Sm3—Se179.60 (3)Cuiii—Se4—Sm1iii68.99 (4)
Se7x—Sm3—Se1ii76.86 (2)Sm2ii—Se4—Sm1iii115.37 (3)
Se6—Sm3—Se1ii79.60 (3)Sm1—Se4—Sm1iii97.82 (3)
Se1—Sm3—Se1ii143.87 (5)Cuiii—Se4—Sm2xviii68.06 (5)
Se7x—Sm3—Se3xi93.76 (4)Sm2ii—Se4—Sm2xviii95.84 (3)
Se6—Sm3—Se3xi153.67 (2)Sm1—Se4—Sm2xviii114.72 (3)
Se1—Sm3—Se3xi79.73 (3)Sm1iii—Se4—Sm2xviii135.38 (4)
Se1ii—Sm3—Se3xi126.34 (3)Se5ii—Se5—Sm465.76 (2)
Se7x—Sm3—Se3ix93.76 (4)Se5ii—Se5—Sm2xviii118.93 (2)
Se6—Sm3—Se3ix153.67 (2)Sm4—Se5—Sm2xviii131.75 (4)
Se1—Sm3—Se3ix126.35 (3)Se5ii—Se5—Sm366.318 (19)
Se1ii—Sm3—Se3ix79.73 (3)Sm4—Se5—Sm3124.83 (4)
Se3xi—Sm3—Se3ix47.84 (4)Sm2xviii—Se5—Sm395.01 (3)
Se7x—Sm3—Se5155.06 (2)Se5ii—Se5—Sm1119.35 (2)
Se6—Sm3—Se576.02 (4)Sm4—Se5—Sm197.80 (3)
Se1—Sm3—Se578.30 (3)Sm2xviii—Se5—Sm1114.59 (3)
Se1ii—Sm3—Se5124.12 (3)Sm3—Se5—Sm183.06 (3)
Se3xi—Sm3—Se583.97 (3)Sm4xix—Se6—Sm3133.67 (6)
Se3ix—Sm3—Se5102.75 (3)Sm4xix—Se6—Sm1104.62 (3)
Se7x—Sm3—Se5ii155.05 (2)Sm3—Se6—Sm190.30 (3)
Se6—Sm3—Se5ii76.02 (4)Sm4xix—Se6—Sm1ii104.61 (3)
Se1—Sm3—Se5ii124.12 (3)Sm3—Se6—Sm1ii90.30 (3)
Se1ii—Sm3—Se5ii78.29 (3)Sm1—Se6—Sm1ii138.54 (5)
Se3xi—Sm3—Se5ii102.75 (3)Sm3xx—Se7—Sm4129.98 (6)
Se3ix—Sm3—Se5ii83.97 (3)Sm3xx—Se7—Sm2xiii106.00 (3)
Se5—Sm3—Se5ii47.37 (4)Sm4—Se7—Sm2xiii90.56 (3)
Se6xii—Sm4—Se7100.92 (5)Sm3xx—Se7—Sm2iv106.00 (3)
Se6xii—Sm4—Se2xiii77.95 (2)Sm4—Se7—Sm2iv90.56 (3)
Se7—Sm4—Se2xiii79.84 (2)Sm2xiii—Se7—Sm2iv136.82 (5)
Se6xii—Sm4—Se2iv77.94 (2)
Symmetry codes: (i) x, y1/2, z+1; (ii) x, y+1/2, z; (iii) x+1, y, z+1; (iv) x+1, y+1, z+1; (v) x, y+1/2, z; (vi) x+1, y+1/2, z; (vii) x+1, y+1/2, z+1; (viii) x, y+1/2, z+1; (ix) x, y+1/2, z1; (x) x1, y, z1; (xi) x, y, z1; (xii) x+1, y, z; (xiii) x+1, y1/2, z+1; (xiv) x, y, z+1; (xv) x, y, z+1; (xvi) x, y+1/2, z+1; (xvii) x, y1/2, z; (xviii) x+1, y1/2, z; (xix) x1, y, z; (xx) x+1, y, z+1.
 

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