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The crystal structures of C4Br4S and C4Br4Se have been determined from X-ray powder diffraction data, using direct-space search techniques. In the case of C4Br4S two crystalline phases occur, a stable orthorhombic and a metastable monoclinic phase. For the orthorhombic phase two different structural models were found that fit the experimental data equally well. The diversity in crystal structure models and packings of C4Br4S is explained.

Supporting information

cif

Crystallographic Information File (CIF) https://doi.org/10.1107/S010876810703652X/av5088sup1.cif
Contains datablocks C4Br4Sa_publ, C4Br4Sab_publ, C4Br4Sb_publ, C4Br4S2G_publ, C4Br4S2S_publ, C4Br4Se_publ, C4Br4S2G_phase_1, C4Br4S2G_phase_2, C4Br4S2S_phase_1, C4Br4S2S_phase_2, C4Br4S2G_p_01, C4Br4S2S_p_01, C4Br4S2G_overall, C4Br4S2S_overall

rtv

Rietveld powder data file (CIF format) https://doi.org/10.1107/S010876810703652X/av5088sup2.rtv
Contains datablock C4Br4Sb_publ

rtv

Rietveld powder data file (CIF format) https://doi.org/10.1107/S010876810703652X/av5088sup3.rtv
Contains datablock C4Br4Sab_publ

rtv

Rietveld powder data file (CIF format) https://doi.org/10.1107/S010876810703652X/av5088sup4.rtv
Contains datablocks C4Br4S2G_publ, C4Br4S2G_overall, C4Br4S2G_phase_1, C4Br4S2G_phase_2, C4Br4S2G_p_01

rtv

Rietveld powder data file (CIF format) https://doi.org/10.1107/S010876810703652X/av5088sup5.rtv
Contains datablocks C4Br4S2S_publ, C4Br4S2S_overall, C4Br4S2S_phase_1, C4Br4S2S_phase_2, C4Br4S2S_p_01

rtv

Rietveld powder data file (CIF format) https://doi.org/10.1107/S010876810703652X/av5088sup6.rtv
Contains datablock C4Br4Se_publ

CCDC references: 665697; 665698; 665699; 665700; 665701; 665702; 665703; 665704

Computing details top

(C4Br4S2G_phase_1) top
Crystal data top
C4Br4Sc = 8.824 (4) Å
Mr = 399.72β = 109.181 (3)°
Monoclinic, PnV = 418.1 (5) Å3
a = 12.419 (5) ÅZ = 2
b = 4.0397 (17) Å
Refinement top
Preferred orientation correction: Spherical Harmonic ODF PHASE 4 spherical harmonic order= 4 The sample symmetry is: cylindrical (fiber texture) Index = 2 0 -2 Coeff= -0.2896 Index = 2 0 0 Coeff= 0.6004 Index = 2 0 2 Coeff= 0.1875 Index = 4 0 -4 Coeff= 0.0771 Index = 4 0 -2 Coeff= 0.1331 Index = 4 0 0 Coeff= 0.3744 Index = 4 0 2 Coeff= 0.2432 Index = 4 0 4 Coeff= 0.1470
Fractional atomic coordinates and isotropic or equivalent isotropic displacement parameters (Å2) top
xyzUiso*/Ueq
S110.5249 (6)0.086 (5)0.7188 (8)0.01226*
C110.3956 (12)0.125 (9)0.7364 (12)0.01226*
C120.3146 (10)0.235 (7)0.5964 (11)0.01226*
C130.3581 (9)0.223 (7)0.4673 (10)0.01226*
C140.4725 (12)0.135 (10)0.5204 (14)0.01226*
Br110.3733 (8)0.122 (3)0.9395 (8)0.01226*
Br120.1862 (6)0.484 (3)0.5967 (12)0.01226*
Br130.2969 (8)0.476 (3)0.2774 (9)0.01226*
Br140.5668 (6)0.096 (4)0.3896 (9)0.01226*
Geometric parameters (Å, º) top
S11—C111.670 (9)C14—S111.667 (9)
S11—C122.549 (9)C14—C131.387 (8)
S11—C132.550 (8)C14—Br132.860 (10)
S11—C141.667 (9)C14—Br141.902 (7)
S11—Br113.125 (9)Br11—S113.125 (9)
S11—Br143.116 (9)Br11—C111.901 (8)
C11—S111.670 (9)Br11—C122.908 (8)
C11—C121.386 (8)Br11—Br123.474 (11)
C11—Br111.901 (8)Br12—C112.877 (10)
C11—Br122.877 (10)Br12—C121.885 (9)
C12—S112.549 (9)Br12—Br113.474 (11)
C12—C111.386 (8)Br12—Br133.518 (13)
C12—C131.413 (7)Br13—C122.918 (9)
C12—Br112.908 (8)Br13—C131.896 (9)
C12—Br121.885 (9)Br13—C142.860 (10)
C12—Br132.918 (9)Br13—Br123.518 (13)
C13—S112.550 (8)Br13—Br143.520 (12)
C13—C121.413 (7)Br14—S113.116 (9)
C13—C141.387 (8)Br14—C141.902 (7)
C13—Br131.896 (9)Br14—Br133.520 (12)
C11—S11—C1491.8 (4)C12—C13—C14110.9 (6)
S11—C11—C12112.7 (6)C12—C13—Br13123.0 (8)
S11—C11—Br11122.0 (8)C14—C13—Br13120.3 (10)
C12—C11—Br11123.7 (6)S11—C14—C13112.8 (5)
C11—C12—C13110.5 (5)S11—C14—Br14121.5 (6)
C11—C12—Br12122.4 (9)C13—C14—Br14125.6 (6)
C13—C12—Br12124.6 (7)
(C4Br4S2G_phase_2) top
Crystal data top
C4Br4Sb = 4.034 (3) Å
Mr = 399.72c = 16.350 (12) Å
Orthorhombic, Pca21V = 833.8 (19) Å3
a = 12.643 (10) ÅZ = 4
Refinement top
Preferred orientation correction: Spherical Harmonic ODF PHASE 4 spherical harmonic order= 4 The sample symmetry is: cylindrical (fiber texture) Index = 2 0 0 Coeff= 0.1174 Index = 2 0 2 Coeff= 0.3335 Index = 4 0 0 Coeff= 0.0494 Index = 4 0 2 Coeff= 0.0110 Index = 4 0 4 Coeff= -0.1731
Fractional atomic coordinates and isotropic or equivalent isotropic displacement parameters (Å2) top
xyzUiso*/Ueq
S210.4287 (11)0.891 (7)0.2800 (8)0.01529*
C210.340 (2)0.814 (15)0.3525 (6)0.01529*
C220.241 (2)0.687 (14)0.3213 (5)0.01529*
C230.246 (2)0.658 (14)0.2361 (4)0.01529*
C240.345 (2)0.797 (16)0.2065 (5)0.01529*
Br210.3691 (16)0.960 (6)0.4641 (7)0.01529*
Br220.1230 (17)0.493 (6)0.3868 (11)0.01529*
Br230.1240 (12)0.505 (4)0.1695 (11)0.01529*
Br240.3812 (14)0.906 (6)0.0949 (7)0.01529*
Geometric parameters (Å, º) top
S21—C211.660 (9)C23—Br231.985 (8)
S21—C241.648 (9)C24—S211.648 (9)
S21—Br213.116 (9)C24—C231.453 (8)
S21—Br243.086 (9)C24—Br241.933 (9)
C21—S211.660 (9)Br21—S213.116 (9)
C21—C221.451 (8)Br21—C211.951 (9)
C21—Br211.951 (9)Br22—C221.993 (9)
C22—C211.451 (8)Br22—Br233.553 (13)
C22—C231.400 (9)Br23—C231.985 (8)
C22—Br221.993 (9)Br23—Br223.553 (13)
C23—C221.400 (9)Br24—S213.086 (9)
C23—C241.453 (8)Br24—C241.933 (9)
C21—S21—C2492.5 (5)C22—C23—C24109.8 (7)
S21—C21—C22113.5 (5)C22—C23—Br23122.4 (8)
S21—C21—Br21119.1 (7)C24—C23—Br23127.2 (6)
C22—C21—Br21126.7 (10)S21—C24—C23113.6 (5)
C21—C22—C23109.8 (6)S21—C24—Br24118.9 (7)
C21—C22—Br22126.7 (9)C23—C24—Br24127.4 (8)
C23—C22—Br22122.4 (8)
(C4Br4S2S_phase_1) top
Crystal data top
C4Br4Sb = 3.9973 (4) Å
Mr = 399.72c = 16.3267 (15) Å
Orthorhombic, Pca21V = 819.7 (2) Å3
a = 12.5599 (12) ÅZ = 4
Refinement top
Preferred orientation correction: Spherical Harmonic ODF PHASE 4 spherical harmonic order= 4 The sample symmetry is: cylindrical (fiber texture) Index = 2 0 0 Coeff= 0.5624 Index = 2 0 2 Coeff= 0.2451 Index = 4 0 0 Coeff= 0.5976 Index = 4 0 2 Coeff= 0.0529 Index = 4 0 4 Coeff= -0.0365
Fractional atomic coordinates and isotropic or equivalent isotropic displacement parameters (Å2) top
xyzUiso*/Ueq
S110.4235 (9)0.950 (4)0.2790 (6)0.025*
C110.337 (3)0.851 (17)0.3548 (6)0.025*
C120.238 (3)0.718 (18)0.3223 (7)0.025*
C130.235 (3)0.713 (18)0.2364 (8)0.025*
C140.3300 (19)0.888 (12)0.2060 (6)0.025*
Br110.3760 (15)0.955 (2)0.4641 (4)0.00786*
Br120.1244 (17)0.491 (3)0.3847 (6)0.00786*
Br130.1257 (15)0.489 (3)0.1679 (6)0.00786*
Br140.3800 (11)0.887 (2)0.0965 (4)0.00786*
Geometric parameters (Å, º) top
S11—C111.695 (11)C13—Br131.986 (11)
S11—C141.691 (12)C14—S111.691 (12)
S11—Br113.080 (9)C14—C131.468 (12)
S11—Br143.039 (10)C14—Br141.895 (12)
C11—S111.695 (11)Br11—S113.080 (9)
C11—C121.448 (11)Br11—C111.898 (11)
C11—Br111.898 (11)Br12—C121.974 (12)
C12—C111.448 (11)Br12—Br133.540 (5)
C12—C131.404 (11)Br13—C131.986 (11)
C12—Br121.974 (12)Br13—Br123.540 (5)
C13—C121.404 (11)Br14—S113.039 (10)
C13—C141.468 (12)Br14—C141.895 (12)
C11—S11—C1492.0 (8)C12—C13—C14108.0 (12)
S11—C11—C12111.6 (9)C12—C13—Br13126.0 (12)
S11—C11—Br11117.9 (8)C14—C13—Br13125.9 (12)
C12—C11—Br11130.3 (11)S11—C14—C13113.3 (14)
C11—C12—C13113.2 (13)S11—C14—Br14115.8 (10)
C11—C12—Br12126.8 (15)C13—C14—Br14125.9 (15)
C13—C12—Br12119.3 (11)
(C4Br4S2S_phase_2) top
Crystal data top
C4Br4Sc = 8.816 (7) Å
Mr = 399.72β = 109.452 (3)°
Monoclinic, PnV = 411.9 (9) Å3
a = 12.376 (10) ÅZ = 2
b = 4.004 (3) Å
Refinement top
Preferred orientation correction: Spherical Harmonic ODF PHASE 4 spherical harmonic order= 4 The sample symmetry is: cylindrical (fiber texture) Index = 2 0 -2 Coeff= -0.0704 Index = 2 0 0 Coeff= -0.2127 Index = 2 0 2 Coeff= 0.1838 Index = 4 0 -4 Coeff= -0.0304 Index = 4 0 -2 Coeff= 0.0261 Index = 4 0 0 Coeff= 0.1302 Index = 4 0 2 Coeff= 0.0435 Index = 4 0 4 Coeff= 0.0993
Fractional atomic coordinates and isotropic or equivalent isotropic displacement parameters (Å2) top
xyzUiso*/Ueq
S210.5267 (14)0.060 (11)0.7208 (15)0.025*
C210.399 (3)0.17 (2)0.741 (3)0.025*
C220.326 (3)0.331 (17)0.606 (2)0.025*
C230.364 (3)0.285 (18)0.474 (2)0.025*
C240.474 (3)0.16 (2)0.523 (3)0.025*
Br210.3705 (14)0.113 (6)0.9377 (15)0.00786*
Br220.1761 (10)0.481 (6)0.5920 (19)0.00786*
Br230.2911 (13)0.466 (6)0.2628 (12)0.00786*
Br240.5615 (12)0.078 (7)0.3852 (14)0.00786*
Geometric parameters (Å, º) top
S21—C211.698 (11)C24—S211.692 (10)
S21—C232.587 (10)C24—C231.391 (10)
S21—C241.692 (10)C24—Br232.909 (11)
S21—Br213.146 (11)C24—Br241.900 (9)
S21—Br243.129 (11)Br21—S213.146 (11)
C21—S211.698 (11)Br21—C211.899 (9)
C21—C221.394 (11)Br21—Br223.517 (19)
C21—Br211.899 (9)Br22—C212.918 (11)
C21—Br222.918 (11)Br22—C221.910 (11)
C22—C211.394 (11)Br22—Br213.517 (19)
C22—C231.405 (11)Br23—C231.920 (11)
C22—Br221.910 (11)Br23—C242.909 (11)
C23—S212.587 (10)Br23—Br243.52 (2)
C23—C221.405 (11)Br24—S213.129 (11)
C23—C241.391 (10)Br24—C241.900 (9)
C23—Br231.920 (11)Br24—Br233.52 (2)
C21—S21—C2489.9 (6)C22—C23—C24110.9 (9)
S21—C21—C22113.4 (9)C22—C23—Br23125.4 (11)
S21—C21—Br21121.9 (7)C24—C23—Br23122.1 (10)
C22—C21—Br21124.3 (8)S21—C24—C23113.8 (6)
C21—C22—C23109.9 (11)S21—C24—Br24121.1 (7)
C21—C22—Br22123.3 (10)C23—C24—Br24125.1 (9)
C23—C22—Br22124.7 (11)
 

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