Download citation
Download citation
link to html
Detailed neutron powder diffraction measurements have been carried out on two polymorphs of anhydrous magnesium sulfate, α-MgSO4 and β-MgSO4. α-MgSO4 is orthorhombic, space group Cmcm (Z = 4); at 4.2 K the unit-cell dimensions are a = 5.16863 (3), b = 7.86781 (5), c = 6.46674 (5) Å, V = 262.975 (2) Å3calc = 3040.16 (2) kg m−3], and at 300 K, a = 5.17471 (3), b = 7.87563 (5), c = 6.49517 (5) Å, V = 264.705 (2) Å3calc = 3020.29 (2) kg m−3]. The axial and volumetric thermal expansion coefficients are positive at all temperatures and exhibit no unusual behaviour. Structures were refined at 4.2 and 300 K to RP < 3%; less precise structural parameters were determined during warming from 4.2 to 300 K. β-MgSO4 has a more complex structure, crystallizing in space group Pbnm (Z = 4); the unit-cell dimensions at 4.2 K are a = 4.73431 (8), b = 8.58170 (12), c = 6.67266 (11) Å, V = 271.100 (5) Å3calc = 2949.04 (5) kg m−3], and at 300 K, a = 4.74598 (7), b = 8.58310 (10), c = 6.70933 (10) Å, V = 273.306 (4) Å3calc = 2925.42 (4) kg m−3]. The thermal expansivities of the a and c axes, and the volumetric thermal expansion coefficient, are positive at all temperatures and normally behaved. However, the thermal expansion of the b axis is both very small and negative below ∼125 K. Structural and thermal motion parameters for β-MgSO4 as a function of temperature are also reported.

Supporting information

cif

Crystallographic Information File (CIF) https://doi.org/10.1107/S0021889807029937/db5013sup1.cif
Contains datablocks global, ALPHAMGSO4_300KNEW_publ, ALPHAMGSO4_300KNEW_overall, ALPHAMGSO4_300KNEW_phase_1, ALPHAMGSO4_300KNEW_p_01, ALPHAMGSO4_300KNEW_p_02, ALPHAMGSO4BEST4KFIT_publ, ALPHAMGSO4BEST4KFIT_overall, ALPHAMGSO4BEST4KFIT_phase_1, ALPHAMGSO4BEST4KFIT_p_01, ALPHAMGSO4BEST4KFIT_p_02, BETAMGSO4_300KPROFIL_publ, BETAMGSO4_300KPROFIL_overall, BETAMGSO4_300KPROFIL_phase_1, BETAMGSO4_300KPROFIL_p_01, BETAMGSO4_300KPROFIL_p_02, BETAMGSO4_4KPROFILE_publ, BETAMGSO4_4KPROFILE_overall, BETAMGSO4_4KPROFILE_phase_1, BETAMGSO4_4KPROFILE_p_01, BETAMGSO4_4KPROFILE_p_02

zip

Zip compressed file https://doi.org/10.1107/S0021889807029937/db5013sup2.zip
DAT files and GSAS refinement files for α-MgSO<inf>4</inf>

zip

Zip compressed file https://doi.org/10.1107/S0021889807029937/db5013sup3.zip
DAT files and GSAS refinement files for β-MgSO<inf>4</inf>

Computing details top

Figures top
[Figure 1]
[Figure 2]
[Figure 3]
[Figure 4]
[Figure 5]
[Figure 6]
[Figure 7]
[Figure 8]
[Figure 9]
[Figure 10]
(ALPHAMGSO4_300KNEW_phase_1) alpha-magnesium sulfate top
Crystal data top
SO42·MgO62+V = 264.71 (1) Å3
Mr = 120.37Z = 4
Orthorhombic, CmcmMelting point: 1200 K
a = 5.17471 (3) Å? radiation, λ = ? Å
b = 7.87563 (5) ÅT = 300 K
c = 6.49517 (5) Å?; ?, ?; ? × ?; ? mm
Data collection top
HRPD, ISIS Facility
diffractometer
Radiation source: Pulsed neutron spallation
Refinement top
Least-squares matrix: full4404 data points
Rp = 0.027Profile function: TOF Profile function number 3 with 21 terms Profile coefficients for exponential pseudovoigt convolution Von Dreele, 1990 (unpublished) #1 (alp ) = 0.3423 #2 (bet-0) = 0.026201 #3 (bet-1) = 0.009785 #4 (sig-0) = 0.0 #5 (sig-1) = 955.3 #6 (sig-2) = 0.0 #7 (gam-0) = 0.00 #8 (gam-1) = 34.24 #9 (gam-2) = 0.00 #10(gsf ) = 0.00 #11(g1ec ) = 0.00 #12(g2ec ) = 0.00 #13(rstr ) = 0.000 #14(rsta ) = 0.000 #15(rsca ) = 0.000 #16(L11) = 0.473 #17(L22) = 0.365 #18(L33) = 1.445 #19(L12) = 0.108 #20(L13) = -0.168 #21(L23) = -0.280 Peak tails are ignored where the intensity is below 0.0010 times the peak Aniso. broadening axis 0.0 0.0 1.0
Rwp = 0.03250 parameters
Rexp = 0.0270 restraints
R(F2) = 0.09217(Δ/σ)max = 0.04
χ2 = 3.133Background function: GSAS Background function number 1 with 5 terms. Shifted Chebyshev function of 1st kind 1: 1.42228 2: 0.520597 3: -1.141080E-02 4: -2.737090E-02 5: -1.666800E-02
Crystal data top
SO42·MgO62+V = 264.71 (1) Å3
Mr = 120.37Z = 4
Orthorhombic, Cmcm? radiation, λ = ? Å
a = 5.17471 (3) ÅT = 300 K
b = 7.87563 (5) Å?; ?, ?; ? × ?; ? mm
c = 6.49517 (5) Å
Data collection top
HRPD, ISIS Facility
diffractometer
Refinement top
Rp = 0.027χ2 = 3.133
Rwp = 0.0324404 data points
Rexp = 0.02750 parameters
R(F2) = 0.092170 restraints
Fractional atomic coordinates and isotropic or equivalent isotropic displacement parameters (Å2) top
xyzUiso*/Ueq
Mg10.00.00.00.01254
S0.00.3508 (2)0.250.0105 (4)*
O10.00.24939 (8)0.06357 (8)0.01275
O20.23321 (13)0.46184 (7)0.250.01188
Atomic displacement parameters (Å2) top
U11U22U33U12U13U23
Mg10.0144 (6)0.0135 (7)0.0097 (7)0.00.00.0002 (4)
O10.0125 (4)0.0129 (4)0.01288 (330.00.00.00367 (29
O20.0093 (4)0.0148 (4)0.0116 (4)0.00340 (310.00.0
Geometric parameters (Å, º) top
Mg1—Mg1i3.2476 (1)S—Mg1ii3.2045 (14)
Mg1—Mg1ii3.2476 (1)S—O11.4505 (10)
Mg1—S3.2045 (14)S—O1viii1.4505 (10)
Mg1—Si3.2045 (14)S—O21.4904 (10)
Mg1—O12.0071 (6)S—O2ix1.4904 (10)
Mg1—O1iii2.0071 (6)O1—Mg12.0071 (6)
Mg1—O2iv2.1524 (4)O1—S1.4505 (10)
Mg1—O2v2.1524 (4)O2—Mg1x2.1524 (4)
Mg1—O2vi2.1524 (4)O2—Mg1xi2.1524 (4)
Mg1—O2vii2.1524 (4)O2—S1.4904 (10)
S—Mg13.2045 (14)
O1—Mg1—O1iii179.972O2v—Mg1—O2vii100.21 (3)
O1—Mg1—O2iv88.936 (19)O2vi—Mg1—O2vii79.79 (3)
O1—Mg1—O2v88.936 (19)O1—S—O1xii113.20 (12)
O1—Mg1—O2vi91.064 (19)O1—S—O2108.849 (16)
O1—Mg1—O2vii91.064 (19)O1—S—O2ix108.849 (16)
O1iii—Mg1—O2iv91.064 (19)O1xii—S—O2108.849 (16)
O1iii—Mg1—O2v91.064 (19)O1xii—S—O2ix108.849 (16)
O1iii—Mg1—O2vi88.936 (19)O2—S—O2ix108.13 (12)
O1iii—Mg1—O2vii88.936 (19)Mg1—O1—S135.27 (6)
O2iv—Mg1—O2v79.79 (3)Mg1x—O2—Mg1xi97.95 (3)
O2iv—Mg1—O2vi100.21 (3)Mg1x—O2—S126.96 (2)
O2iv—Mg1—O2vii179.9657Mg1xi—O2—S126.96 (2)
O2v—Mg1—O2vi179.972
Symmetry codes: (i) x, y, z1/2; (ii) x, y, z+1/2; (iii) x, y, z; (iv) x1/2, y1/2, z; (v) x+1/2, y1/2, z; (vi) x1/2, y+1/2, z1/2; (vii) x+1/2, y+1/2, z1/2; (viii) x, y, z+1/2; (ix) x, y, z; (x) x+1/2, y+1/2, z; (xi) x+1/2, y+1/2, z+1/2; (xii) x1, y1, z+3/2.
(ALPHAMGSO4BEST4KFIT_phase_1) alpha-magnesium sulfate top
Crystal data top
SO42·MgO62+V = 262.98 (1) Å3
Mr = 120.37Z = 4
Orthorhombic, CmcmMelting point: 1200 K
a = 5.16863 (3) Å? radiation, λ = ? Å
b = 7.86781 (5) ÅT = 4 K
c = 6.46674 (5) Å?; ?, ?; ? × ?; ? mm
Data collection top
HRPD, ISIS Facility
diffractometer
Specimen mounting: slab can
Radiation source: Pulsed neutron spallation
Refinement top
Least-squares matrix: full4404 data points
Rp = 0.029Profile function: TOF Profile function number 3 with 21 terms Profile coefficients for exponential pseudovoigt convolution Von Dreele, 1990 (unpublished) #1 (alp ) = 0.3423 #2 (bet-0) = 0.026201 #3 (bet-1) = 0.009785 #4 (sig-0) = 0.0 #5 (sig-1) = 1212.2 #6 (sig-2) = 0.0 #7 (gam-0) = 0.00 #8 (gam-1) = 35.70 #9 (gam-2) = 0.00 #10(gsf ) = 0.00 #11(g1ec ) = 0.00 #12(g2ec ) = 0.00 #13(rstr ) = 0.000 #14(rsta ) = 0.000 #15(rsca ) = 0.000 #16(L11) = 0.509 #17(L22) = 0.543 #18(L33) = 1.926 #19(L12) = 0.163 #20(L13) = -0.337 #21(L23) = -0.386 Peak tails are ignored where the intensity is below 0.0010 times the peak Aniso. broadening axis 0.0 0.0 1.0
Rwp = 0.03641 parameters
Rexp = 0.0270 restraints
R(F2) = 0.08920(Δ/σ)max = 0.17
χ2 = 3.881Background function: GSAS Background function number 1 with 5 terms. Shifted Chebyshev function of 1st kind 1: 1.24219 2: 0.442743 3: -4.282540E-02 4: -1.056000E-02 5: -1.243180E-02
Crystal data top
SO42·MgO62+V = 262.98 (1) Å3
Mr = 120.37Z = 4
Orthorhombic, Cmcm? radiation, λ = ? Å
a = 5.16863 (3) ÅT = 4 K
b = 7.86781 (5) Å?; ?, ?; ? × ?; ? mm
c = 6.46674 (5) Å
Data collection top
HRPD, ISIS Facility
diffractometer
Specimen mounting: slab can
Refinement top
Rp = 0.0294404 data points
Rwp = 0.03641 parameters
Rexp = 0.0270 restraints
R(F2) = 0.08920(Δ/σ)max = 0.17
χ2 = 3.881
Fractional atomic coordinates and isotropic or equivalent isotropic displacement parameters (Å2) top
xyzUiso*/Ueq
Mg10.00.00.00.0084 (3)*
S0.00.3510 (2)0.250.0079 (4)*
O10.00.24966 (8)0.06264 (9)0.00822 (18)*
O20.23393 (14)0.46246 (7)0.250.00833 (19)*
Geometric parameters (Å, º) top
Mg1—Mg1i3.2334 (1)S—Mg1ii3.2003 (14)
Mg1—Mg1ii3.2334 (1)S—Mg1x3.2659 (6)
Mg1—S3.2003 (14)S—Mg1xi3.2659 (6)
Mg1—Si3.2003 (14)S—Mg1xii3.2659 (6)
Mg1—Siii3.2659 (6)S—Mg1xiii3.2659 (6)
Mg1—Siv3.2659 (6)S—O11.4506 (10)
Mg1—Sv3.2659 (6)S—O1xiv1.4506 (10)
Mg1—Svi3.2659 (6)S—O21.4935 (11)
Mg1—O12.0056 (6)S—O2xv1.4935 (11)
Mg1—O1vii2.0056 (6)O1—Mg12.0056 (6)
Mg1—O2iii2.1429 (4)O1—S1.4506 (10)
Mg1—O2viii2.1429 (4)O2—Mg1xi2.1429 (4)
Mg1—O2v2.1429 (4)O2—Mg1xiii2.1429 (4)
Mg1—O2ix2.1429 (4)O2—S1.4935 (11)
S—Mg13.2003 (14)
O1—Mg1—O1vii180.0O2viii—Mg1—O2ix100.16 (3)
O1—Mg1—O2iii89.005 (19)O2v—Mg1—O2ix79.84 (3)
O1—Mg1—O2viii89.005 (19)O1—S—O1xvi113.28 (11)
O1—Mg1—O2v90.995 (19)O1—S—O2108.830 (16)
O1—Mg1—O2ix90.995 (19)O1—S—O2xv108.830 (16)
O1vii—Mg1—O2iii90.995 (19)O1xvi—S—O2108.830 (16)
O1vii—Mg1—O2viii90.995 (19)O1xvi—S—O2xv108.830 (16)
O1vii—Mg1—O2v89.005 (19)O2—S—O2xv108.12 (12)
O1vii—Mg1—O2ix89.005 (19)Mg1—O1—S135.01 (6)
O2iii—Mg1—O2viii79.84 (3)Mg1xi—O2—Mg1xiii97.95 (3)
O2iii—Mg1—O2v100.16 (3)Mg1xi—O2—S126.90 (2)
O2iii—Mg1—O2ix180.0Mg1xiii—O2—S126.90 (2)
O2viii—Mg1—O2v180.0
Symmetry codes: (i) x, y, z1/2; (ii) x, y, z+1/2; (iii) x1/2, y1/2, z; (iv) x+1/2, y1/2, z; (v) x1/2, y+1/2, z1/2; (vi) x+1/2, y+1/2, z1/2; (vii) x, y, z; (viii) x+1/2, y1/2, z; (ix) x+1/2, y+1/2, z1/2; (x) x1/2, y+1/2, z; (xi) x+1/2, y+1/2, z; (xii) x1/2, y+1/2, z+1/2; (xiii) x+1/2, y+1/2, z+1/2; (xiv) x, y, z+1/2; (xv) x, y, z; (xvi) x1, y1, z+3/2.
(BETAMGSO4_300KPROFIL_phase_1) alpha-magnesium sulfate top
Crystal data top
SO42·MgO62+V = 273.31 (1) Å3
Mr = 120.37Z = 4
Orthorhombic, PbnmMelting point: 1200 K
a = 4.74599 (7) Å? radiation, λ = ? Å
b = 8.5831 (1) ÅT = 300 K
c = 6.70934 (10) Å?; ?, ?; ? × ?; ? mm
Data collection top
HRPD, ISIS Facility
diffractometer
Radiation source: Pulsed neutron spallation
Refinement top
Least-squares matrix: full4404 data points
Rp = 0.038Profile function: TOF Profile function number 3 with 21 terms Profile coefficients for exponential pseudovoigt convolution Von Dreele, 1990 (unpublished) #1 (alp ) = 0.3423 #2 (bet-0) = 0.026201 #3 (bet-1) = 0.009785 #4 (sig-0) = 0.0 #5 (sig-1) = 1213.0 #6 (sig-2) = 823.6 #7 (gam-0) = 0.00 #8 (gam-1) = 54.16 #9 (gam-2) = 0.00 #10(gsf ) = 0.00 #11(g1ec ) = 0.00 #12(g2ec ) = 0.00 #13(rstr ) = 0.000 #14(rsta ) = 0.000 #15(rsca ) = 0.000 #16(L11) = 1.294 #17(L22) = 0.264 #18(L33) = 1.480 #19(L12) = 0.242 #20(L13) = 0.499 #21(L23) = 0.340 Peak tails are ignored where the intensity is below 0.0010 times the peak Aniso. broadening axis 0.0 1.0 0.0
Rwp = 0.04561 parameters
Rexp = 0.0333 restraints
R(F2) = 0.07342(Δ/σ)max = 0.27
χ2 = 4.410Background function: GSAS Background function number 1 with 5 terms. Shifted Chebyshev function of 1st kind 1: 1.19515 2: 0.318323 3: 3.560090E-02 4: -1.899200E-02 5: -2.705870E-03
Crystal data top
SO42·MgO62+V = 273.31 (1) Å3
Mr = 120.37Z = 4
Orthorhombic, Pbnm? radiation, λ = ? Å
a = 4.74599 (7) ÅT = 300 K
b = 8.5831 (1) Å?; ?, ?; ? × ?; ? mm
c = 6.70934 (10) Å
Data collection top
HRPD, ISIS Facility
diffractometer
Refinement top
Rp = 0.0384404 data points
Rwp = 0.04561 parameters
Rexp = 0.0333 restraints
R(F2) = 0.07342(Δ/σ)max = 0.27
χ2 = 4.410
Fractional atomic coordinates and isotropic or equivalent isotropic displacement parameters (Å2) top
xyzUiso*/Ueq
O30.3375 (2)0.12661 (15)0.06959 (15)0.01483
O20.4641 (4)0.35188 (15)0.250.01412
O10.7709 (3)0.1265 (3)0.250.01333
S0.4780 (5)0.1812 (2)0.250.0129 (7)*
Mg0.00.00.00.01312
Atomic displacement parameters (Å2) top
U11U22U33U12U13U23
O30.0143 (7)0.0268 (7)0.0034 (5)0.0027 (7)0.0022 (5)0.0007 (8)
O20.0300 (14)0.0034 (5)0.0089 (10)0.0055 (10)0.00.0
O10.0034 (5)0.0073 (10)0.0292 (10)0.0029 (8)0.00.0
Mg0.0186 (13)0.0110 (8)0.0098 (11)0.0035 (10)0.0028 (8)0.0073 (11)
Geometric parameters (Å, º) top
O3—S1.4592 (12)S—Mgii3.2113 (14)
O3—Mg1.9910 (11)S—Mgvi3.2214 (18)
O2—S1.4666 (16)Mg—O31.9910 (11)
O2—Mgi2.1116 (8)Mg—O3vii1.9910 (11)
O2—Mgii2.1116 (8)Mg—O2viii2.1116 (8)
O1—S1.4673 (18)Mg—O2ix2.1116 (8)
O1—Mgiii2.2749 (13)Mg—O1x2.2749 (13)
O1—Mgiv2.2749 (13)Mg—O1xi2.2749 (13)
S—O31.4592 (12)Mg—S3.2214 (18)
S—O3v1.4592 (12)Mg—Sviii3.2113 (14)
S—O21.4666 (16)Mg—Six3.2113 (14)
S—O11.4673 (18)Mg—Sxii3.2214 (18)
S—Mg3.2214 (18)Mg—Mgxii3.3547 (1)
S—Mgi3.2113 (14)Mg—Mgvi3.3547 (1)
S—O3—Mg137.50 (11)O3—Mg—O2viii94.44 (6)
S—O2—Mgi126.72 (3)O3—Mg—O2ix85.56 (6)
S—O2—Mgii126.72 (3)O3—Mg—O1x87.19 (6)
Mgi—O2—Mgii105.19 (6)O3—Mg—O1xi92.81 (6)
S—O1—Mgiii127.27 (5)O3vii—Mg—O2viii85.56 (6)
S—O1—Mgiv127.27 (5)O3vii—Mg—O2ix94.44 (6)
Mgiii—O1—Mgiv95.01 (7)O3vii—Mg—O1x92.81 (6)
O3—S—O3xiii112.11 (18)O3vii—Mg—O1xi87.19 (6)
O3—S—O2107.47 (10)O2viii—Mg—O2ix179.9802
O3—S—O1109.29 (10)O2viii—Mg—O1x74.95 (5)
O3xiv—S—O2107.47 (10)O2viii—Mg—O1xi105.05 (5)
O3v—S—O1109.29 (10)O2ix—Mg—O1x105.05 (5)
O2—S—O1111.2 (2)O2ix—Mg—O1xi74.95 (5)
O3—Mg—O3vii180.0O1x—Mg—O1xi180.0
Symmetry codes: (i) x+1/2, y+1/2, z; (ii) x+1/2, y+1/2, z+1/2; (iii) x+1, y, z; (iv) x+1, y, z+1/2; (v) x, y, z+1/2; (vi) x, y, z+1/2; (vii) x, y, z; (viii) x+1/2, y1/2, z; (ix) x1/2, y+1/2, z1/2; (x) x1, y, z; (xi) x+1, y, z1/2; (xii) x, y, z1/2; (xiii) x1, y1, z+3/2; (xiv) x1, y1, z+1/2.
(BETAMGSO4_4KPROFILE_phase_1) alpha-magnesium sulfate top
Crystal data top
SO42·MgO62+V = 271.10 (1) Å3
Mr = 120.37Z = 4
Orthorhombic, PbnmMelting point: 1200 K
a = 4.73431 (8) Å? radiation, λ = ? Å
b = 8.58171 (12) ÅT = 4 K
c = 6.67266 (11) Å?; ?, ?; ? × ?; ? mm
Data collection top
HRPD, ISIS Facility
diffractometer
Radiation source: Pulsed neutron spallation
Refinement top
Least-squares matrix: full4404 data points
Rp = 0.042Profile function: TOF Profile function number 3 with 21 terms Profile coefficients for exponential pseudovoigt convolution Von Dreele, 1990 (unpublished) #1 (alp ) = 0.3423 #2 (bet-0) = 0.026201 #3 (bet-1) = 0.009785 #4 (sig-0) = 0.0 #5 (sig-1) = 3231.3 #6 (sig-2) = 974.1 #7 (gam-0) = 0.00 #8 (gam-1) = 52.99 #9 (gam-2) = 0.00 #10(gsf ) = 0.00 #11(g1ec ) = 0.00 #12(g2ec ) = 0.00 #13(rstr ) = 0.000 #14(rsta ) = 0.000 #15(rsca ) = 0.000 #16(L11) = 2.214 #17(L22) = 0.514 #18(L33) = 2.557 #19(L12) = 0.555 #20(L13) = -0.218 #21(L23) = -0.087 Peak tails are ignored where the intensity is below 0.0010 times the peak Aniso. broadening axis 0.0 1.0 0.0
Rwp = 0.05048 parameters
Rexp = 0.0300 restraints
R(F2) = 0.08309(Δ/σ)max = 0.25
χ2 = 6.200Background function: GSAS Background function number 1 with 5 terms. Shifted Chebyshev function of 1st kind 1: 1.14930 2: 0.339049 3: -7.066090E-03 4: -1.534120E-02 5: -8.436520E-04
Crystal data top
SO42·MgO62+V = 271.10 (1) Å3
Mr = 120.37Z = 4
Orthorhombic, Pbnm? radiation, λ = ? Å
a = 4.73431 (8) ÅT = 4 K
b = 8.58171 (12) Å?; ?, ?; ? × ?; ? mm
c = 6.67266 (11) Å
Data collection top
HRPD, ISIS Facility
diffractometer
Refinement top
Rp = 0.0424404 data points
Rwp = 0.05048 parameters
Rexp = 0.0300 restraints
R(F2) = 0.08309(Δ/σ)max = 0.25
χ2 = 6.200
Fractional atomic coordinates and isotropic or equivalent isotropic displacement parameters (Å2) top
xyzUiso*/Ueq
O30.3385 (2)0.12604 (12)0.06902 (13)0.0082 (3)*
O20.4628 (3)0.35178 (14)0.250.0068 (4)*
O10.7759 (3)0.1266 (3)0.250.0079 (4)*
S0.4817 (7)0.1804 (3)0.250.0089 (7)*
Mg0.00.00.00.0059 (4)*
Geometric parameters (Å, º) top
O3—S1.4612 (18)S—Mgii3.2115 (19)
O3—Mg1.9875 (10)S—Mgvi3.222 (3)
O2—S1.474 (3)Mg—O31.9875 (10)
O2—Mgi2.1051 (8)Mg—O3vii1.9875 (10)
O2—Mgii2.1051 (8)Mg—O2viii2.1051 (8)
O1—S1.468 (4)Mg—O2ix2.1051 (8)
O1—Mgiii2.2557 (12)Mg—O1x2.2557 (12)
O1—Mgiv2.2557 (12)Mg—O1xi2.2557 (12)
S—O31.4612 (18)Mg—S3.222 (3)
S—O3v1.4612 (18)Mg—Sviii3.2115 (19)
S—O21.474 (3)Mg—Six3.2115 (19)
S—O11.468 (4)Mg—Sxii3.222 (3)
S—Mg3.222 (3)Mg—Mgxii3.3363 (1)
S—Mgi3.2115 (19)Mg—Mgvi3.3363 (1)
S—O3—Mg137.66 (12)O3—Mg—O2viii94.46 (5)
S—O2—Mgi126.73 (4)O3—Mg—O2ix85.54 (5)
S—O2—Mgii126.73 (4)O3—Mg—O1x86.89 (5)
Mgi—O2—Mgii104.82 (5)O3—Mg—O1xi93.11 (5)
S—O1—Mgiii126.72 (6)O3vii—Mg—O2viii85.54 (5)
S—O1—Mgiv126.72 (6)O3vii—Mg—O2ix94.46 (5)
Mgiii—O1—Mgiv95.38 (7)O3vii—Mg—O1x93.11 (5)
O3—S—O3xiii111.5 (2)O3vii—Mg—O1xi86.89 (5)
O3—S—O2106.88 (13)O2viii—Mg—O2ix179.9802
O3—S—O1109.87 (13)O2viii—Mg—O1x75.18 (5)
O3xiv—S—O2106.88 (13)O2viii—Mg—O1xi104.82 (5)
O3v—S—O1109.87 (13)O2ix—Mg—O1x104.82 (5)
O2—S—O1111.8 (2)O2ix—Mg—O1xi75.18 (5)
O3—Mg—O3vii180.0O1x—Mg—O1xi180.0
Symmetry codes: (i) x+1/2, y+1/2, z; (ii) x+1/2, y+1/2, z+1/2; (iii) x+1, y, z; (iv) x+1, y, z+1/2; (v) x, y, z+1/2; (vi) x, y, z+1/2; (vii) x, y, z; (viii) x+1/2, y1/2, z; (ix) x1/2, y+1/2, z1/2; (x) x1, y, z; (xi) x+1, y, z1/2; (xii) x, y, z1/2; (xiii) x1, y1, z+3/2; (xiv) x1, y1, z+1/2.

Experimental details

(ALPHAMGSO4_300KNEW_phase_1)(ALPHAMGSO4BEST4KFIT_phase_1)(BETAMGSO4_300KPROFIL_phase_1)(BETAMGSO4_4KPROFILE_phase_1)
Crystal data
Chemical formulaSO42·MgO62+SO42·MgO62+SO42·MgO62+SO42·MgO62+
Mr120.37120.37120.37120.37
Crystal system, space groupOrthorhombic, CmcmOrthorhombic, CmcmOrthorhombic, PbnmOrthorhombic, Pbnm
Temperature (K)30043004
a, b, c (Å)5.17471 (3), 7.87563 (5), 6.49517 (5)5.16863 (3), 7.86781 (5), 6.46674 (5)4.74599 (7), 8.5831 (1), 6.70934 (10)4.73431 (8), 8.58171 (12), 6.67266 (11)
V3)264.71 (1)262.98 (1)273.31 (1)271.10 (1)
Z4444
Radiation type?, λ = ? Å?, λ = ? Å?, λ = ? Å?, λ = ? Å
Specimen shape, size (mm)?; ?, ?; ? × ?; ??; ?, ?; ? × ?; ??; ?, ?; ? × ?; ??; ?, ?; ? × ?; ?
Data collection
Data collection methodHRPD, ISIS FacilityHRPD, ISIS FacilityHRPD, ISIS FacilityHRPD, ISIS Facility
Specimen mounting?; ?Slab can?; ??; ?
Data collection mode?; ??; ??; ??; ?
Scan method?; ??; ??; ??; ?
2θ values (°)2θmin = ? 2θmax = ? 2θstep = ?2θmin = ? 2θmax = ? 2θstep = ?2θmin = ? 2θmax = ? 2θstep = ?2θmin = ? 2θmax = ? 2θstep = ?
Refinement
R factors and goodness of fitRp = 0.027, Rwp = 0.032, Rexp = 0.027, R(F2) = 0.09217, χ2 = 3.133Rp = 0.029, Rwp = 0.036, Rexp = 0.027, R(F2) = 0.08920, χ2 = 3.881Rp = 0.038, Rwp = 0.045, Rexp = 0.033, R(F2) = 0.07342, χ2 = 4.410Rp = 0.042, Rwp = 0.050, Rexp = 0.030, R(F2) = 0.08309, χ2 = 6.200
No. of data points4404440444044404
No. of parameters50416148
No. of restraints0030
(Δ/σ)max0.040.170.270.25

Computer programs: GSAS.

 

Follow J. Appl. Cryst.
Sign up for e-alerts
Follow J. Appl. Cryst. on Twitter
Follow us on facebook
Sign up for RSS feeds