The anionic component of the crystal structure of cubic langbeinite-type diammonium dimanganese(II) trisulfate(IV), (NH4)2Mn2(SO4)3, is a three-dimensional [Mn2(SO4)3]2- network based on SO4 tetrahedra corner-linked to MnIIO6 octahedra. The charge-balancing ammonium cations occupy the cavities in the network. The pairs of independent Mn and N atoms lie on special positions of site symmetry 3.
Supporting information
CCDC reference: 262247
Key indicators
- Single-crystal X-ray study
- T = 295 K
- Mean (S-O) = 0.003 Å
- R factor = 0.030
- wR factor = 0.071
- Data-to-parameter ratio = 11.7
checkCIF/PLATON results
No syntax errors found
Alert level C
ABSTM02_ALERT_3_C The ratio of expected to reported Tmax/Tmin(RR') is < 0.90
Tmin and Tmax reported: 0.584 0.862
Tmin' and Tmax expected: 0.648 0.858
RR' = 0.898
Please check that your absorption correction is appropriate.
PLAT061_ALERT_3_C Tmax/Tmin Range Test RR' too Large ............. 0.89
PLAT480_ALERT_4_C Long H...A H-Bond Reported H11 .. O3 .. 2.62 Ang.
PLAT731_ALERT_1_C Bond Calc 0.85(4), Rep 0.850(10) ...... 4.00 su-Rat
N1 -H11 1.555 1.555
PLAT732_ALERT_1_C Angle Calc 110(3), Rep 109.0(10) ...... 3.00 su-Rat
H11 -N1 -H12 1.555 1.555 1.555
PLAT735_ALERT_1_C D-H Calc 0.85(4), Rep 0.850(10) ...... 4.00 su-Rat
N1 -H11 1.555 1.555
PLAT735_ALERT_1_C D-H Calc 0.85(4), Rep 0.850(10) ...... 4.00 su-Rat
N1 -H11 1.555 1.555
PLAT735_ALERT_1_C D-H Calc 0.85(4), Rep 0.850(10) ...... 4.00 su-Rat
N1 -H11 1.555 1.555
Alert level G
REFLT03_ALERT_4_G Please check that the estimate of the number of Friedel pairs is
correct. If it is not, please give the correct count in the
_publ_section_exptl_refinement section of the submitted CIF.
From the CIF: _diffrn_reflns_theta_max 27.40
From the CIF: _reflns_number_total 818
Count of symmetry unique reflns 477
Completeness (_total/calc) 171.49%
TEST3: Check Friedels for noncentro structure
Estimate of Friedel pairs measured 341
Fraction of Friedel pairs measured 0.715
Are heavy atom types Z>Si present yes
0 ALERT level A = In general: serious problem
0 ALERT level B = Potentially serious problem
8 ALERT level C = Check and explain
1 ALERT level G = General alerts; check
5 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
2 ALERT type 3 Indicator that the structure quality may be low
2 ALERT type 4 Improvement, methodology, query or suggestion
Data collection: SMART (Bruker, 2002); cell refinement: SAINT (Bruker, 2002); data reduction: SAINT; program(s) used to solve structure: SHELXS97 (Sheldrick, 1997); program(s) used to refine structure: SHELXL97 (Sheldrick, 1997); molecular graphics: ORTEPII (Johnson, 1976); software used to prepare material for publication: SHELXL97.
Diammonium dimanganese(II) trissulfate(IV)
top
Crystal data top
(NH4)2Mn2(SO4)3 | Dx = 2.727 Mg m−3 |
Mr = 434.14 | Mo Kα radiation, λ = 0.71073 Å |
Cubic, P213 | Cell parameters from 1534 reflections |
Hall symbol: P 2ac 2ab 3 | θ = 3.5–21.5° |
a = 10.188 (2) Å | µ = 3.05 mm−1 |
V = 1057.5 (4) Å3 | T = 295 K |
Z = 4 | Block, pale yellow |
F(000) = 864 | 0.14 × 0.08 × 0.05 mm |
Data collection top
Bruker APEX area-detector diffractometer | 818 independent reflections |
Radiation source: fine-focus sealed tube | 765 reflections with I > 2σ(I) |
Graphite monochromator | Rint = 0.069 |
φ and ω scan | θmax = 27.4°, θmin = 2.8° |
Absorption correction: multi-scan (SADABS; Bruker, 2002) | h = −13→13 |
Tmin = 0.584, Tmax = 0.862 | k = −12→13 |
7327 measured reflections | l = −12→8 |
Refinement top
Refinement on F2 | Secondary atom site location: difference Fourier map |
Least-squares matrix: full | Hydrogen site location: difference Fourier map |
R[F2 > 2σ(F2)] = 0.030 | Only H-atom coordinates refined |
wR(F2) = 0.071 | w = 1/[σ2(Fo2) + (0.043P)2] where P = (Fo2 + 2Fc2)/3 |
S = 1.05 | (Δ/σ)max = 0.001 |
818 reflections | Δρmax = 0.36 e Å−3 |
70 parameters | Δρmin = −0.35 e Å−3 |
8 restraints | Absolute structure: Flack (1983), 342 Friedel pairs |
Primary atom site location: structure-invariant direct methods | Absolute structure parameter: 0.01 (4) |
Special details top
Refinement. A dimensionless value (µ*2r, r = equivalent radius of the crystal) of 0.30 was
used in the absorption correction step. |
Fractional atomic coordinates and isotropic or equivalent isotropic displacement parameters (Å2) top | x | y | z | Uiso*/Ueq | |
Mn1 | 0.84380 (5) | 0.84380 (5) | 0.84380 (5) | 0.0127 (2) | |
Mn2 | 0.91670 (5) | 0.41670 (5) | 1.08330 (5) | 0.0119 (2) | |
S | 0.87483 (8) | 0.53107 (9) | 0.76320 (9) | 0.0107 (2) | |
O1 | 0.9191 (3) | 0.6682 (3) | 0.7510 (3) | 0.0201 (6) | |
O2 | 0.8463 (3) | 0.4993 (3) | 0.9015 (3) | 0.0237 (7) | |
O3 | 0.9770 (3) | 0.4445 (3) | 0.7117 (3) | 0.0227 (6) | |
O4 | 0.7545 (3) | 0.5095 (3) | 0.6872 (3) | 0.0250 (7) | |
N1 | 1.2010 (3) | 0.7010 (3) | 0.7990 (3) | 0.021 (1) | |
N2 | 0.5665 (3) | 0.4335 (3) | 0.9335 (3) | 0.019 (1) | |
H11 | 1.211 (7) | 0.775 (3) | 0.835 (4) | 0.08 (2)* | |
H12 | 1.1528 (6) | 0.6528 (6) | 0.8472 (6) | 0.10 (5)* | |
H21 | 0.6415 (19) | 0.469 (3) | 0.925 (4) | 0.03 (2)* | |
H22 | 0.5182 (6) | 0.4818 (6) | 0.9818 (6) | 0.03 (2)* | |
Atomic displacement parameters (Å2) top | U11 | U22 | U33 | U12 | U13 | U23 |
Mn1 | 0.0127 (2) | 0.0127 (2) | 0.0127 (2) | −0.0007 (2) | −0.0007 (2) | −0.0007 (2) |
Mn2 | 0.0119 (2) | 0.0119 (2) | 0.0119 (2) | −0.0002 (2) | 0.0002 (2) | 0.0002 (2) |
S | 0.0102 (4) | 0.0111 (5) | 0.0107 (4) | 0.0016 (3) | −0.0001 (3) | 0.0007 (3) |
O1 | 0.024 (1) | 0.012 (1) | 0.024 (2) | −0.004 (1) | 0.006 (1) | −0.001 (1) |
O2 | 0.028 (2) | 0.030 (2) | 0.013 (1) | 0.004 (1) | 0.003 (1) | 0.008 (1) |
O3 | 0.019 (2) | 0.022 (2) | 0.027 (2) | 0.010 (1) | 0.005 (1) | −0.002 (1) |
O4 | 0.018 (1) | 0.029 (2) | 0.027 (2) | 0.002 (1) | −0.012 (1) | −0.003 (1) |
N1 | 0.021 (1) | 0.021 (1) | 0.021 (1) | −0.004 (2) | 0.004 (2) | 0.004 (2) |
N2 | 0.019 (1) | 0.019 (1) | 0.019 (1) | 0.002 (2) | 0.002 (2) | −0.002 (2) |
Geometric parameters (Å, º) top
Mn1—O1 | 2.164 (3) | Mn2—O4viii | 2.175 (3) |
Mn1—O1i | 2.164 (3) | Mn2—O4ix | 2.175 (3) |
Mn1—O1ii | 2.164 (3) | S—O1 | 1.473 (3) |
Mn1—O3iii | 2.169 (3) | S—O2 | 1.475 (3) |
Mn1—O3iv | 2.169 (3) | S—O3 | 1.462 (3) |
Mn1—O3v | 2.169 (3) | S—O4 | 1.467 (3) |
Mn2—O2 | 2.157 (3) | N1—H11 | 0.85 (1) |
Mn2—O2vi | 2.157 (3) | N1—H12 | 0.85 (1) |
Mn2—O2v | 2.157 (3) | N2—H21 | 0.85 (1) |
Mn2—O4vii | 2.175 (3) | N2—H22 | 0.85 (1) |
| | | |
O1—Mn1—O1i | 95.0 (1) | O2vi—Mn2—O4vii | 173.6 (1) |
O1—Mn1—O3iii | 88.8 (1) | O2vi—Mn2—O4viii | 90.9 (1) |
O1—Mn1—O3iv | 174.2 (1) | O2vi—Mn2—O4ix | 81.6 (1) |
O1—Mn1—O1ii | 95.0 (1) | O2v—Mn2—O4vii | 81.6 (1) |
O1—Mn1—O3v | 89.1 (1) | O2v—Mn2—O4viii | 173.6 (1) |
O1i—Mn1—O3iii | 89.1 (1) | O2v—Mn2—O4ix | 90.9 (1) |
O1i—Mn1—O1ii | 95.0 (1) | O4vii—Mn2—O4viii | 93.2 (1) |
O1i—Mn1—O3iv | 88.8 (1) | O4vii—Mn2—O4ix | 93.2 (1) |
O1i—Mn1—O3v | 174.2 (1) | O4viii—Mn2—O4ix | 93.2 (1) |
O1ii—Mn1—O3iii | 174.2 (1) | O1—S—O2 | 110.4 (2) |
O1ii—Mn1—O3iv | 89.1 (1) | O1—S—O3 | 108.9 (2) |
O1ii—Mn1—O3v | 88.8 (1) | O1—S—O4 | 110.7 (2) |
O3iii—Mn1—O3iv | 86.8 (1) | O2—S—O3 | 110.6 (2) |
O3iii—Mn1—O3v | 86.8 (1) | O2—S—O4 | 107.9 (2) |
O3v—Mn1—O3iv | 86.8 (1) | O3—S—O4 | 108.4 (2) |
O2—Mn2—O2vi | 94.6 (1) | S—O1—Mn1 | 129.7 (2) |
O2—Mn2—O2v | 94.6 (1) | S—O2—Mn2 | 147.2 (2) |
O2—Mn2—O4vii | 90.9 (1) | S—O3—Mn1x | 168.0 (2) |
O2—Mn2—O4viii | 81.6 (1) | S—O4—Mn2xi | 151.1 (2) |
O2—Mn2—O4ix | 173.6 (1) | H11—N1—H12 | 109 (1) |
O2vi—Mn2—O2v | 94.6 (1) | H21—N2—H22 | 109 (1) |
| | | |
O3—S—O1—Mn1 | −164.4 (2) | O1—S—O2—Mn2 | −95.4 (4) |
O4—S—O1—Mn1 | 76.6 (2) | O2v—Mn2—O2—S | 88.4 (3) |
O2—S—O1—Mn1 | −42.8 (3) | O2vi—Mn2—O2—S | −6.6 (4) |
O1ii—Mn1—O1—S | −11.0 (2) | O4vii—Mn2—O2—S | 170.1 (4) |
O1i—Mn1—O1—S | −106.4 (1) | O4viii—Mn2—O2—S | −96.8 (4) |
O3v—Mn1—O1—S | 77.7 (2) | O3—S—O4—Mn2xi | −135.9 (4) |
O3iii—Mn1—O1—S | 164.6 (2) | O1—S—O4—Mn2xi | −16.5 (5) |
O3—S—O2—Mn2 | 25.2 (4) | O2—S—O4—Mn2xi | 104.4 (4) |
O4—S—O2—Mn2 | 143.5 (3) | | |
Symmetry codes: (i) z, x, y; (ii) y, z, x; (iii) −x+2, y+1/2, −z+3/2; (iv) −z+3/2, −x+2, y+1/2; (v) y+1/2, −z+3/2, −x+2; (vi) −z+2, x−1/2, −y+3/2; (vii) −x+3/2, −y+1, z+1/2; (viii) −z+3/2, −x+1, y+1/2; (ix) −y+3/2, −z+1, x+1/2; (x) −x+2, y−1/2, −z+3/2; (xi) −x+3/2, −y+1, z−1/2. |
Hydrogen-bond geometry (Å, º) top
D—H···A | D—H | H···A | D···A | D—H···A |
N1—H11···O1v | 0.85 (1) | 2.55 (3) | 2.933 (4) | 108 (3) |
N1—H11···O3iii | 0.85 (1) | 2.62 (8) | 3.075 (3) | 115 (6) |
N1—H11···O4iii | 0.85 (1) | 2.42 (2) | 3.178 (5) | 149 (4) |
N1—H12···O1 | 0.85 (1) | 2.58 (1) | 2.933 (4) | 106 (1) |
N2—H21···O2 | 0.85 (1) | 2.12 (1) | 2.946 (4) | 163 (3) |
N2—H22···O3ii | 0.85 (1) | 2.46 (1) | 3.127 (6) | 136 (2) |
Symmetry codes: (ii) y, z, x; (iii) −x+2, y+1/2, −z+3/2; (v) y+1/2, −z+3/2, −x+2. |