Supporting information
Crystallographic Information File (CIF) https://doi.org/10.1107/S1600536804018513/wm6026sup1.cif | |
Structure factor file (CIF format) https://doi.org/10.1107/S1600536804018513/wm6026Isup2.hkl |
Key indicators
- Single-crystal X-ray study
- T = 153 K
- Mean (S-P) = 0.002 Å
- R factor = 0.020
- wR factor = 0.049
- Data-to-parameter ratio = 27.8
checkCIF/PLATON results
No syntax errors found
Alert level B PLAT029_ALERT_3_B _diffrn_measured_fraction_theta_full Low ....... 0.96
Alert level C STRVA01_ALERT_4_C Flack test results are ambiguous. From the CIF: _refine_ls_abs_structure_Flack 0.550 From the CIF: _refine_ls_abs_structure_Flack_su 0.007 PLAT033_ALERT_2_C Flack Parameter Value Deviates from Zero ....... 0.55 PLAT042_ALERT_1_C Calc. and Rep. MoietyFormula Strings Differ .... ?
Alert level G ABSTM02_ALERT_3_G The ratio of expected to reported Tmax/Tmin(RR) is > 2.00 Tmin and Tmax reported: 0.047 0.603 Tmin and Tmax expected: 0.010 0.613 RR = 4.708 Please check that your absorption correction is appropriate. 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 28.82 From the CIF: _reflns_number_total 1807 Count of symmetry unique reflns 1153 Completeness (_total/calc) 156.72% TEST3: Check Friedels for noncentro structure Estimate of Friedel pairs measured 654 Fraction of Friedel pairs measured 0.567 Are heavy atom types Z>Si present yes
0 ALERT level A = In general: serious problem 1 ALERT level B = Potentially serious problem 3 ALERT level C = Check and explain 2 ALERT level G = General alerts; check 1 ALERT type 1 CIF construction/syntax error, inconsistent or missing data 1 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, 2003); cell refinement: SAINT-Plus (Bruker, 2003); data reduction: SAINT-Plus; 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.
RbPbPS4 | F(000) = 792 |
Mr = 451.87 | Dx = 4.053 Mg m−3 |
Orthorhombic, P212121 | Mo Kα radiation, λ = 0.71073 Å |
Hall symbol: P 2ac 2ab | Cell parameters from 7200 reflections |
a = 6.3987 (7) Å | θ = 2.4–28.8° |
b = 6.6899 (7) Å | µ = 30.54 mm−1 |
c = 17.2975 (19) Å | T = 153 K |
V = 740.45 (14) Å3 | Plate, yellow |
Z = 4 | 0.18 × 0.16 × 0.02 mm |
Bruker SMART 1000 CCD diffractometer | 1807 independent reflections |
Radiation source: fine-focus sealed tube | 1759 reflections with I > 2σ(I) |
Graphite monochromator | Rint = 0.032 |
ω scans | θmax = 28.8°, θmin = 2.4° |
Absorption correction: numerical face indexed (SHELXTL; Sheldrick, 2003) | h = −8→8 |
Tmin = 0.047, Tmax = 0.603 | k = −9→9 |
8784 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)] = 0.020 | w = 1/[σ2(Fo2) + (0.02P)2] where P = (Fo2 + 2Fc2)/3 |
wR(F2) = 0.049 | (Δ/σ)max = 0.001 |
S = 1.39 | Δρmax = 2.11 e Å−3 |
1807 reflections | Δρmin = −1.57 e Å−3 |
65 parameters | Absolute structure: Flack (1983): 704 Friedel pairs |
0 restraints | Absolute structure parameter: 0.550 (7) |
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. The structure was refined as an enantiomeric twin, the final twin ratio being 0.55:0.45. |
x | y | z | Uiso*/Ueq | ||
Rb | 0.02119 (9) | 0.00342 (8) | 0.04319 (3) | 0.02110 (13) | |
Pb | 0.28891 (3) | 0.47494 (3) | 0.230842 (12) | 0.01418 (7) | |
P | 0.2189 (2) | 0.01031 (19) | 0.34791 (8) | 0.0100 (3) | |
S1 | 0.1533 (2) | 0.0316 (2) | 0.23134 (8) | 0.0131 (3) | |
S2 | 0.3990 (2) | 0.25142 (19) | 0.37520 (10) | 0.0142 (3) | |
S3 | 0.6101 (3) | 0.25876 (19) | 0.13163 (10) | 0.0134 (3) | |
S4 | 0.0472 (2) | 0.5039 (2) | 0.08806 (8) | 0.0135 (3) |
U11 | U22 | U33 | U12 | U13 | U23 | |
Rb | 0.0374 (3) | 0.0118 (3) | 0.0142 (3) | −0.0009 (2) | 0.0062 (2) | −0.0007 (2) |
Pb | 0.01344 (10) | 0.01498 (11) | 0.01413 (11) | 0.00007 (8) | −0.00011 (8) | 0.00066 (9) |
P | 0.0121 (6) | 0.0077 (6) | 0.0103 (6) | −0.0002 (6) | 0.0001 (5) | 0.0003 (5) |
S1 | 0.0152 (6) | 0.0152 (6) | 0.0089 (6) | −0.0015 (5) | 0.0010 (5) | 0.0003 (7) |
S2 | 0.0181 (8) | 0.0069 (6) | 0.0178 (8) | −0.0015 (5) | −0.0035 (7) | 0.0000 (5) |
S3 | 0.0176 (7) | 0.0070 (6) | 0.0155 (8) | −0.0013 (5) | 0.0000 (6) | 0.0004 (5) |
S4 | 0.0158 (6) | 0.0130 (7) | 0.0116 (6) | 0.0004 (6) | 0.0045 (5) | 0.0004 (6) |
Rb—S1 | 3.3680 (15) | Pb—Pbviii | 4.3504 (4) |
Rb—S2i | 3.4075 (17) | Pb—Pbix | 4.3504 (4) |
Rb—S4ii | 3.4345 (16) | Pb—Rbvii | 4.3877 (7) |
Rb—S4 | 3.4412 (16) | P—S4iv | 2.0320 (18) |
Rb—S3iii | 3.4639 (17) | P—S2 | 2.038 (2) |
Rb—S2iv | 3.4734 (17) | P—S3ix | 2.0381 (19) |
Rb—S3v | 3.4898 (17) | P—S1 | 2.0644 (19) |
Rb—Pi | 3.7660 (15) | P—Pbix | 3.4392 (14) |
Rb—S4iii | 3.7887 (14) | P—Pbiv | 3.5315 (14) |
Rb—Pbiv | 4.3877 (7) | P—Rbx | 3.7660 (15) |
Rb—Rbvi | 4.8324 (9) | S1—Pbiv | 2.9290 (13) |
Rb—Rbiii | 4.8324 (9) | S2—Pbix | 3.2823 (16) |
Pb—S4 | 2.9204 (14) | S2—Rbx | 3.4075 (17) |
Pb—S1vii | 2.9290 (14) | S2—Rbvii | 3.4733 (17) |
Pb—S2 | 2.9945 (16) | S3—Pviii | 2.0381 (19) |
Pb—S3 | 3.0430 (16) | S3—Pbix | 3.1116 (16) |
Pb—S1 | 3.0900 (14) | S3—Rbvi | 3.4640 (17) |
Pb—S3viii | 3.1116 (16) | S3—Rbxi | 3.4898 (17) |
Pb—S2viii | 3.2823 (16) | S4—Pvii | 2.0320 (18) |
Pb—Pviii | 3.4392 (14) | S4—Rbxii | 3.4345 (16) |
Pb—Pvii | 3.5315 (14) | S4—Rbvi | 3.7888 (14) |
S1—Rb—S2i | 144.54 (4) | S1vii—Pb—Pvii | 35.75 (4) |
S1—Rb—S4ii | 79.86 (4) | S2—Pb—Pvii | 124.86 (4) |
S2i—Rb—S4ii | 72.46 (3) | S3—Pb—Pvii | 115.83 (4) |
S1—Rb—S4 | 73.46 (3) | S1—Pb—Pvii | 78.87 (3) |
S2i—Rb—S4 | 132.22 (4) | S3viii—Pb—Pvii | 116.43 (4) |
S4ii—Rb—S4 | 153.30 (5) | S2viii—Pb—Pvii | 107.85 (4) |
S1—Rb—S3iii | 140.96 (4) | Pviii—Pb—Pvii | 133.25 (4) |
S2i—Rb—S3iii | 57.37 (3) | S4—Pb—Pbviii | 113.99 (3) |
S4ii—Rb—S3iii | 129.51 (4) | S1vii—Pb—Pbviii | 117.80 (3) |
S4—Rb—S3iii | 75.05 (3) | S2—Pb—Pbviii | 96.36 (3) |
S1—Rb—S2iv | 80.14 (4) | S3—Pb—Pbviii | 91.83 (3) |
S2i—Rb—S2iv | 102.70 (4) | S1—Pb—Pbviii | 155.77 (3) |
S4ii—Rb—S2iv | 58.23 (3) | S3viii—Pb—Pbviii | 44.38 (3) |
S4—Rb—S2iv | 114.71 (3) | S2viii—Pb—Pbviii | 43.45 (3) |
S3iii—Rb—S2iv | 134.82 (4) | Pviii—Pb—Pbviii | 55.87 (2) |
S1—Rb—S3v | 74.82 (4) | Pvii—Pb—Pbviii | 125.36 (2) |
S2i—Rb—S3v | 137.03 (4) | S4—Pb—Pbix | 120.58 (3) |
S4ii—Rb—S3v | 114.44 (3) | S1vii—Pb—Pbix | 131.72 (3) |
S4—Rb—S3v | 57.41 (3) | S2—Pb—Pbix | 48.92 (3) |
S3iii—Rb—S3v | 106.36 (4) | S3—Pb—Pbix | 45.66 (3) |
S2iv—Rb—S3v | 58.39 (3) | S1—Pb—Pbix | 55.66 (3) |
S1—Rb—Pi | 139.22 (4) | S3viii—Pb—Pbix | 102.93 (3) |
S2i—Rb—Pi | 32.52 (3) | S2viii—Pb—Pbix | 98.08 (3) |
S4ii—Rb—Pi | 99.07 (3) | Pviii—Pb—Pbix | 62.91 (2) |
S4—Rb—Pi | 101.81 (3) | Pvii—Pb—Pbix | 132.98 (2) |
S3iii—Rb—Pi | 32.40 (3) | Pbviii—Pb—Pbix | 100.508 (12) |
S2iv—Rb—Pi | 133.99 (4) | S4—Pb—Rbvii | 120.73 (3) |
S3v—Rb—Pi | 137.56 (4) | S1vii—Pb—Rbvii | 50.10 (3) |
S1—Rb—S4iii | 141.33 (3) | S2—Pb—Rbvii | 52.07 (3) |
S2i—Rb—S4iii | 66.58 (4) | S3—Pb—Rbvii | 145.94 (3) |
S4ii—Rb—S4iii | 99.30 (3) | S1—Pb—Rbvii | 84.96 (3) |
S4—Rb—S4iii | 100.75 (3) | S3viii—Pb—Rbvii | 52.15 (3) |
S3iii—Rb—S4iii | 67.31 (4) | S2viii—Pb—Rbvii | 138.46 (3) |
S2iv—Rb—S4iii | 67.52 (4) | Pviii—Pb—Rbvii | 139.81 (2) |
S3v—Rb—S4iii | 70.47 (4) | Pvii—Pb—Rbvii | 85.67 (2) |
Pi—Rb—S4iii | 79.38 (3) | Pbviii—Pb—Rbvii | 96.413 (11) |
S1—Rb—Pbiv | 41.85 (2) | Pbix—Pb—Rbvii | 100.282 (11) |
S2i—Rb—Pbiv | 143.68 (3) | S4iv—P—S2 | 111.36 (9) |
S4ii—Rb—Pbiv | 77.19 (2) | S4iv—P—S3ix | 109.75 (8) |
S4—Rb—Pbiv | 82.14 (2) | S2—P—S3ix | 108.05 (8) |
S3iii—Rb—Pbiv | 150.68 (3) | S4iv—P—S1 | 111.30 (8) |
S2iv—Rb—Pbiv | 42.84 (3) | S2—P—S1 | 106.65 (8) |
S3v—Rb—Pbiv | 44.75 (3) | S3ix—P—S1 | 109.62 (8) |
Pi—Rb—Pbiv | 176.05 (3) | S4iv—P—Pbix | 169.07 (7) |
S4iii—Rb—Pbiv | 99.86 (3) | S2—P—Pbix | 68.19 (6) |
S1—Rb—Rbvi | 95.41 (3) | S3ix—P—Pbix | 61.34 (6) |
S2i—Rb—Rbvi | 88.78 (3) | S1—P—Pbix | 78.71 (5) |
S4ii—Rb—Rbvi | 134.59 (3) | S4iv—P—Pbiv | 55.78 (5) |
S4—Rb—Rbvi | 51.20 (3) | S2—P—Pbiv | 131.50 (7) |
S3iii—Rb—Rbvi | 46.20 (3) | S3ix—P—Pbiv | 120.37 (7) |
S2iv—Rb—Rbvi | 165.82 (3) | S1—P—Pbiv | 56.00 (5) |
S3v—Rb—Rbvi | 107.48 (3) | Pbix—P—Pbiv | 133.25 (4) |
Pi—Rb—Rbvi | 56.43 (2) | S4iv—P—Rbx | 83.15 (6) |
S4iii—Rb—Rbvi | 110.71 (3) | S2—P—Rbx | 64.02 (6) |
Pbiv—Rb—Rbvi | 127.191 (19) | S3ix—P—Rbx | 65.62 (6) |
S1—Rb—Rbiii | 115.26 (3) | S1—P—Rbx | 165.34 (7) |
S2i—Rb—Rbiii | 100.20 (3) | Pbix—P—Rbx | 87.09 (3) |
S4ii—Rb—Rbiii | 140.01 (3) | Pbiv—P—Rbx | 138.64 (4) |
S4—Rb—Rbiii | 55.77 (3) | P—S1—Pbiv | 88.25 (6) |
S3iii—Rb—Rbiii | 61.66 (3) | P—S1—Pb | 90.69 (6) |
S2iv—Rb—Rbiii | 86.82 (3) | Pbiv—S1—Pb | 113.34 (4) |
S3v—Rb—Rbiii | 45.76 (3) | P—S1—Rb | 172.30 (7) |
Pi—Rb—Rbiii | 91.82 (3) | Pbiv—S1—Rb | 88.05 (4) |
S4iii—Rb—Rbiii | 45.06 (2) | Pb—S1—Rb | 96.98 (4) |
Pbiv—Rb—Rbiii | 90.325 (13) | P—S2—Pb | 93.96 (7) |
Rbvi—Rb—Rbiii | 82.914 (19) | P—S2—Pbix | 76.61 (6) |
S4—Pb—S1vii | 70.65 (4) | Pb—S2—Pbix | 87.63 (4) |
S4—Pb—S2 | 149.64 (4) | P—S2—Rbx | 83.47 (6) |
S1vii—Pb—S2 | 96.07 (4) | Pb—S2—Rbx | 174.99 (6) |
S4—Pb—S3 | 84.97 (4) | Pbix—S2—Rbx | 95.93 (4) |
S1vii—Pb—S3 | 147.13 (4) | P—S2—Rbvii | 92.33 (7) |
S2—Pb—S3 | 94.25 (4) | Pb—S2—Rbvii | 85.09 (4) |
S4—Pb—S1 | 85.27 (4) | Pbix—S2—Rbvii | 166.32 (5) |
S1vii—Pb—S1 | 81.51 (3) | Rbx—S2—Rbvii | 90.70 (4) |
S2—Pb—S1 | 65.45 (4) | Pviii—S3—Pb | 82.66 (6) |
S3—Pb—S1 | 74.64 (4) | Pviii—S3—Pbix | 105.04 (7) |
S4—Pb—S3viii | 135.72 (4) | Pb—S3—Pbix | 89.95 (4) |
S1vii—Pb—S3viii | 87.19 (4) | Pviii—S3—Rbvi | 81.98 (6) |
S2—Pb—S3viii | 67.56 (4) | Pb—S3—Rbvi | 99.39 (4) |
S3—Pb—S3viii | 125.51 (2) | Pbix—S3—Rbvi | 169.05 (5) |
S1—Pb—S3viii | 129.93 (4) | Pviii—S3—Rbxi | 94.34 (7) |
S4—Pb—S2viii | 79.17 (4) | Pb—S3—Rbxi | 171.47 (6) |
S1vii—Pb—S2viii | 129.76 (4) | Pbix—S3—Rbxi | 83.10 (4) |
S2—Pb—S2viii | 127.17 (2) | Rbvi—S3—Rbxi | 88.04 (4) |
S3—Pb—S2viii | 62.73 (3) | Pvii—S4—Pb | 89.10 (6) |
S1—Pb—S2viii | 135.50 (4) | Pvii—S4—Rbxii | 93.56 (6) |
S3viii—Pb—S2viii | 87.53 (4) | Pb—S4—Rbxii | 106.35 (4) |
S4—Pb—Pviii | 98.36 (3) | Pvii—S4—Rb | 95.90 (6) |
S1vii—Pb—Pviii | 164.61 (4) | Pb—S4—Rb | 98.73 (4) |
S2—Pb—Pviii | 98.58 (4) | Rbxii—S4—Rb | 153.29 (5) |
S3—Pb—Pviii | 36.00 (4) | Pvii—S4—Rbvi | 176.19 (7) |
S1—Pb—Pviii | 108.92 (3) | Pb—S4—Rbvi | 94.70 (4) |
S3viii—Pb—Pviii | 94.05 (4) | Rbxii—S4—Rbvi | 85.18 (3) |
S2viii—Pb—Pviii | 35.20 (3) | Rb—S4—Rbvi | 83.74 (3) |
S4—Pb—Pvii | 35.12 (3) |
Symmetry codes: (i) −x+1/2, −y, z−1/2; (ii) x, y−1, z; (iii) x−1/2, −y+1/2, −z; (iv) −x, y−1/2, −z+1/2; (v) x−1, y, z; (vi) x+1/2, −y+1/2, −z; (vii) −x, y+1/2, −z+1/2; (viii) −x+1, y+1/2, −z+1/2; (ix) −x+1, y−1/2, −z+1/2; (x) −x+1/2, −y, z+1/2; (xi) x+1, y, z; (xii) x, y+1, z. |
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