Supporting information
Crystallographic Information File (CIF) https://doi.org/10.1107/S160053680603491X/wm2032sup1.cif | |
Structure factor file (CIF format) https://doi.org/10.1107/S160053680603491X/wm2032Isup2.hkl |
Key indicators
- Single-crystal X-ray study
- T = 298 K
- Mean (S-O) = 0.001 Å
- R factor = 0.023
- wR factor = 0.076
- Data-to-parameter ratio = 23.8
checkCIF/PLATON results
No syntax errors found
Alert level C PLAT040_ALERT_1_C No H-atoms in this Carbon Containing Compound .. ? PLAT066_ALERT_1_C Predicted and Reported Transmissions Identical . ? PLAT127_ALERT_1_C Implicit Hall Symbol Inconsistent with Explicit -F 2uv 2vw
Alert level G REFLT03_ALERT_1_G ALERT: Expected hkl max differ from CIF values From the CIF: _diffrn_reflns_theta_max 36.59 From the CIF: _reflns_number_total 570 From the CIF: _diffrn_reflns_limit_ max hkl 23. 15. 23. From the CIF: _diffrn_reflns_limit_ min hkl -23. -14. -23. TEST1: Expected hkl limits for theta max Calculated maximum hkl 23. 23. 23. Calculated minimum hkl -23. -23. -23.
0 ALERT level A = In general: serious problem 0 ALERT level B = Potentially serious problem 3 ALERT level C = Check and explain 1 ALERT level G = General alerts; check 4 ALERT type 1 CIF construction/syntax error, inconsistent or missing data 0 ALERT type 2 Indicator that the structure model may be wrong or deficient 0 ALERT type 3 Indicator that the structure quality may be low 0 ALERT type 4 Improvement, methodology, query or suggestion 0 ALERT type 5 Informative message, check
Data collection: SMART (Bruker, 2003); cell refinement: SAINT (Bruker, 2005); data reduction: SAINT; program(s) used to solve structure: SHELXS97 (Sheldrick, 1997); program(s) used to refine structure: SHELXL97 (Sheldrick, 1997); molecular graphics: XtalDraw (Downs & Hall-Wallace, 2003); software used to prepare material for publication: SHELXTL (Bruker, 1997.
Na6Mg2(SO4)(CO3)4 | Dx = 2.583 Mg m−3 |
Mr = 522.66 | Mo Kα radiation, λ = 0.71073 Å |
Cubic, Fd3 | Cell parameters from 3000 reflections |
Hall symbol: -F 2uv 2vw | θ = 2.5–36.6° |
a = 13.9038 (2) Å | µ = 0.63 mm−1 |
V = 2687.82 (7) Å3 | T = 298 K |
Z = 8 | Block, colourless |
F(000) = 2064 | 0.10 × 0.10 × 0.08 mm |
Bruker SMART APEX-II CCD diffractometer | 570 independent reflections |
Radiation source: fine-focus sealed tube | 505 reflections with I > 2σ(I) |
Graphite monochromator | Rint = 0.034 |
φ and ω scans | θmax = 36.6°, θmin = 2.5° |
Absorption correction: multi-scan (SADABS; Sheldrick, 2005) | h = −23→23 |
Tmin = 0.939, Tmax = 0.951 | k = −14→15 |
12979 measured reflections | l = −23→23 |
Refinement on F2 | Primary atom site location: structure-invariant direct methods |
Least-squares matrix: full | Secondary atom site location: difference Fourier map |
R[F2 > 2σ(F2)] = 0.023 | w = 1/[σ2(Fo2) + (0.0575P)2] where P = (Fo2 + 2Fc2)/3 |
wR(F2) = 0.076 | (Δ/σ)max < 0.001 |
S = 1.01 | Δρmax = 0.41 e Å−3 |
570 reflections | Δρmin = −0.39 e Å−3 |
24 parameters | Extinction correction: SHELXL97, Fc*=kFc[1+0.001xFc2λ3/sin(2θ)]-1/4 |
0 restraints | Extinction coefficient: none |
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. |
x | y | z | Uiso*/Ueq | ||
S | 0.1250 | 0.1250 | 0.1250 | 0.01191 (15) | |
Mg | 1.0000 | 0.5000 | 0.0000 | 0.00903 (15) | |
C | 1.03207 (5) | 0.71793 (5) | 0.03207 (5) | 0.0087 (2) | |
Na | 0.34379 (4) | 0.1250 | 0.1250 | 0.01915 (16) | |
O1 | 0.26626 (4) | 0.22529 (4) | 0.35333 (4) | 0.01226 (14) | |
O2 | 0.06362 (4) | 0.06362 (4) | 0.06362 (4) | 0.0195 (2) |
U11 | U22 | U33 | U12 | U13 | U23 | |
S | 0.01191 (15) | 0.01191 (15) | 0.01191 (15) | 0.000 | 0.000 | 0.000 |
Mg | 0.00903 (15) | 0.00903 (15) | 0.00903 (15) | −0.00030 (11) | −0.00030 (11) | −0.00030 (11) |
C | 0.0087 (2) | 0.0087 (2) | 0.0087 (2) | −0.00005 (19) | 0.00005 (19) | −0.00005 (19) |
Na | 0.0139 (2) | 0.0229 (3) | 0.0206 (3) | 0.000 | 0.000 | −0.00774 (17) |
O1 | 0.0149 (2) | 0.0117 (2) | 0.0102 (2) | −0.00012 (16) | 0.00191 (16) | 0.00302 (16) |
O2 | 0.0195 (2) | 0.0195 (2) | 0.0195 (2) | −0.00351 (18) | −0.00351 (18) | −0.00351 (18) |
S—O2i | 1.4782 (10) | Mg—Naxvi | 3.2799 (3) |
S—O2 | 1.4782 (10) | Mg—Naxvii | 3.2799 (3) |
S—O2ii | 1.4782 (10) | Mg—Naxviii | 3.2799 (3) |
S—O2iii | 1.4782 (10) | Mg—Naxix | 3.2799 (3) |
S—Naiv | 3.0421 (5) | C—O1xx | 1.2857 (5) |
S—Na | 3.0421 (5) | C—O1xxi | 1.2857 (5) |
S—Nav | 3.0421 (5) | C—O1ix | 1.2857 (5) |
S—Navi | 3.0421 (5) | Na—O1xxii | 2.3915 (7) |
S—Nai | 3.0421 (5) | Na—O1xxiii | 2.3915 (7) |
S—Navii | 3.0421 (5) | Na—O1iv | 2.4124 (5) |
Mg—O1viii | 2.0804 (5) | Na—O1vii | 2.4124 (5) |
Mg—O1ix | 2.0804 (5) | Na—O2i | 2.4994 (5) |
Mg—O1x | 2.0804 (5) | Na—O2ii | 2.4994 (5) |
Mg—O1xi | 2.0804 (5) | Na—Mgxxiv | 3.2799 (3) |
Mg—O1xii | 2.0804 (5) | Na—Mgxxv | 3.2799 (3) |
Mg—O1xiii | 2.0804 (5) | Na—Naxxiii | 3.5297 (1) |
Mg—Naxiv | 3.2799 (3) | Na—Naxxvi | 3.5297 (1) |
Mg—Naxv | 3.2799 (3) | Na—Naxxvii | 3.5297 (1) |
O2i—S—O2 | 109.5 | O1xxiii—Na—O1iv | 102.758 (16) |
O2i—S—O2ii | 109.5 | O1xxii—Na—O1vii | 102.757 (16) |
O2—S—O2ii | 109.5 | O1xxiii—Na—O1vii | 72.25 (2) |
O2i—S—O2iii | 109.5 | O1iv—Na—O1vii | 173.70 (3) |
O2—S—O2iii | 109.5 | O1xxii—Na—O2i | 158.180 (15) |
O2ii—S—O2iii | 109.5 | O1xxiii—Na—O2i | 114.24 (3) |
O1viii—Mg—O1ix | 94.20 (2) | O1iv—Na—O2i | 88.136 (16) |
O1viii—Mg—O1x | 94.20 (2) | O1vii—Na—O2i | 97.396 (17) |
O1ix—Mg—O1x | 94.20 (2) | O1xxii—Na—O2ii | 114.24 (3) |
O1viii—Mg—O1xi | 85.80 (2) | O1xxiii—Na—O2ii | 158.180 (15) |
O1ix—Mg—O1xi | 85.80 (2) | O1iv—Na—O2ii | 97.396 (17) |
O1x—Mg—O1xi | 180.00 (3) | O1vii—Na—O2ii | 88.136 (16) |
O1viii—Mg—O1xii | 85.80 (2) | O2i—Na—O2ii | 57.75 (5) |
O1ix—Mg—O1xii | 180.00 (3) | Cxxviii—O1—Mgxxix | 132.27 (5) |
O1x—Mg—O1xii | 85.80 (2) | Cxxviii—O1—Naxxvi | 117.29 (3) |
O1xi—Mg—O1xii | 94.20 (2) | Mgxxix—O1—Naxxvi | 94.096 (19) |
O1viii—Mg—O1xiii | 180.0 | Cxxviii—O1—Nav | 116.85 (6) |
O1ix—Mg—O1xiii | 85.80 (2) | Mgxxix—O1—Nav | 93.49 (2) |
O1x—Mg—O1xiii | 85.80 (2) | Naxxvi—O1—Nav | 94.57 (2) |
O1xi—Mg—O1xiii | 94.20 (2) | S—O2—Navi | 96.39 (2) |
O1xii—Mg—O1xiii | 94.20 (2) | S—O2—Nai | 96.39 (2) |
O1xx—C—O1xxi | 119.993 (2) | Navi—O2—Nai | 118.778 (9) |
O1xx—C—O1ix | 119.993 (2) | S—O2—Navii | 96.39 (2) |
O1xxi—C—O1ix | 119.993 (2) | Navi—O2—Navii | 118.778 (9) |
O1xxii—Na—O1xxiii | 80.27 (3) | Nai—O2—Navii | 118.778 (9) |
O1xxii—Na—O1iv | 72.25 (2) |
Symmetry codes: (i) −x+1/4, −y+1/4, z; (ii) −x+1/4, y, −z+1/4; (iii) x, −y+1/4, −z+1/4; (iv) z, x, y; (v) y, z, x; (vi) −y+1/4, z, −x+1/4; (vii) z, −x+1/4, −y+1/4; (viii) −z+3/2, x+1/4, y−1/4; (ix) y+3/4, −z+1, x−1/4; (x) x+3/4, y+1/4, −z+1/2; (xi) −x+5/4, −y+3/4, z−1/2; (xii) −y+5/4, z, −x+1/4; (xiii) z+1/2, −x+3/4, −y+1/4; (xiv) y+1, z+1/2, x−1/2; (xv) −z+1, −x+1, −y; (xvi) z+1, x, y; (xvii) −x+3/2, −y+1/2, −z; (xviii) x+1/2, y+1/2, z; (xix) −y+1, −z+1/2, −x+1/2; (xx) z+3/4, −x+1, y−1/4; (xxi) x+3/4, −y+1, z−1/4; (xxii) y+1/4, z−1/4, −x+1/2; (xxiii) y+1/4, −z+1/2, x−1/4; (xxiv) x−1/2, −y+3/4, −z+1/4; (xxv) x−1/2, y−1/2, z; (xxvi) −z+1/2, x−1/4, y+1/4; (xxvii) −z+1/2, −x+1/2, −y; (xxviii) x−3/4, −y+1, z+1/4; (xxix) −x+5/4, −y+3/4, z+1/2. |
Bonds | Tychite | Ferrotychite |
S-O (x4) | 1.4782 (10) | 1.483 (1) |
C-O (x3) | 1.2857 (5) | 1.287 (1) |
Na-O1 (x2) | 2.4994 (5) | 2.485 (1) |
Na-O2 (x2) | 2.3915 (7) | 2.388 (1) |
Na-O2 (x2) | 2.4124 (5) | 2.409 (1) |
M-O (x6) | 2.0804 (5) | 2.132 (1) |
Peak Positions (cm-1) | Mode Assignments |
144, 360 | Lattice Vibrations |
493.8 | ν2 SO4 symmetric bend |
629.7 | ν4 SO4 antisymmetric bending |
708.7 | ν4 CO3 in-plane bending |
859.2 | ν2 CO3 out-of-plane bending |
967.1 | ν1 SO4 primary internal stretching mode |
1108.1 | ν1 CO3 primary internal stretching mode |
1136.6 | ν3 SO4 antisymmetric stretching |