Crystal structure of hexa­sodium tetra­serinolium paratungstate B deca­hydrate, [Na6{(CH2OH)2CHNH3}4][W12O40(OH)2]·10H2O

Sifaki, K.; Gumerova, N.I.; Giester, G.; Rompel, A.

doi:10.1107/S2056989022000457

Crystal structure of hexasodium tetraserinolium paratungstate B decahydrate, [Na₆{(CH₂OH)₂CHNH₃}₄][W₁₂O₄₀(OH)₂]·10H₂O

K. Sifaki, N. I. Gumerova, G. Giester and A. Rompel

The isolation and characterization of an isopolytungstate anion [W₁₂O₄₀(OH)₂]^10– (paradodecatungstate B) with sodium and protonated serinol entities [Na₆((CH₂OH)₂CHNH₃)₄]¹⁰⁺ as counter-cations are reported.

Keywords: crystal structure; metal oxide; polyoxometalate; isopolytungstate; organic–inorganic hybrid; alkoxo ligand.

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Supporting information

	Crystallographic Information File (CIF) https://doi.org/10.1107/S2056989022000457/wm5630sup1.cif Contains datablock I
	Structure factor file (CIF format) https://doi.org/10.1107/S2056989022000457/wm5630Isup2.hkl Contains datablock I

CCDC reference: 2121767

checkCIF report

Key indicators

Single-crystal X-ray study
T = 200 K
Mean (C-C) = 0.008 Å
H-atom completeness 91%
Disorder in main residue
R factor = 0.017
wR factor = 0.043
Data-to-parameter ratio = 11.6

checkCIF/PLATON results

No syntax errors found



Alert level C
PLAT041_ALERT_1_C Calc. and Reported SumFormula    Strings  Differ     Please Check
PLAT043_ALERT_1_C Calculated and Reported Mol. Weight Differ by ..       3.08 Check
PLAT068_ALERT_1_C Reported F000 Differs from Calcd (or Missing)...     Please Check
PLAT220_ALERT_2_C NonSolvent   Resd 1  O   Ueq(max)/Ueq(min) Range        6.0 Ratio
PLAT342_ALERT_3_C Low Bond Precision on  C-C Bonds ...............    0.00825 Ang.
PLAT354_ALERT_3_C Short  O-H (X0.82,N0.98A)  O22      - H22A     .       0.69 Ang.
PLAT354_ALERT_3_C Short  O-H (X0.82,N0.98A)  O24      - H24B     .       0.63 Ang.
PLAT354_ALERT_3_C Short  O-H (X0.82,N0.98A)  O27      - H27      .       0.67 Ang.
PLAT414_ALERT_2_C Short Intra D-H..H-X       H1D      ..H25              1.98 Ang.
                                                      x,y,z  =      1_555 Check
PLAT911_ALERT_3_C Missing FCF Refl Between Thmin & STh/L=    0.600          7 Report
PLAT972_ALERT_2_C Check Calcd Resid. Dens.  0.21A   From W1             -1.63 eA-3
PLAT974_ALERT_2_C Check Calcd Negative Resid. Density on        W5      -1.46 eA-3
PLAT974_ALERT_2_C Check Calcd Negative Resid. Density on        W6      -1.36 eA-3
PLAT974_ALERT_2_C Check Calcd Negative Resid. Density on        W4      -1.36 eA-3
PLAT974_ALERT_2_C Check Calcd Negative Resid. Density on        W3      -1.24 eA-3
PLAT974_ALERT_2_C Check Calcd Negative Resid. Density on        W2      -1.22 eA-3
PLAT975_ALERT_2_C Check Calcd Resid. Dens.  0.91A   From O8              1.04 eA-3
PLAT975_ALERT_2_C Check Calcd Resid. Dens.  0.78A   From O8              0.94 eA-3
PLAT975_ALERT_2_C Check Calcd Resid. Dens.  0.51A   From O8              0.76 eA-3
PLAT976_ALERT_2_C Check Calcd Resid. Dens.  0.98A   From N2             -1.38 eA-3
PLAT976_ALERT_2_C Check Calcd Resid. Dens.  0.99A   From O28            -0.87 eA-3
PLAT977_ALERT_2_C Check Negative Difference Density on H1D       .      -0.32 eA-3
PLAT978_ALERT_2_C Number C-C Bonds with Positive Residual Density.          0 Info

Alert level G
FORMU01_ALERT_1_G  There is a discrepancy between the atom counts in the
            _chemical_formula_sum and _chemical_formula_moiety. This is
            usually due to the moiety formula being in the wrong format.
            Atom count from _chemical_formula_sum:   C12 H62 N4 Na6 O60 W12
            Atom count from _chemical_formula_moiety:C12 H56 N4 Na6 O60 W12
FORMU01_ALERT_2_G  There is a discrepancy between the atom counts in the
            _chemical_formula_sum and the formula from the _atom_site* data.
            Atom count from _chemical_formula_sum:C12 H62 N4 Na6 O60 W12
            Atom count from the _atom_site data:  C12 H56 N4 Na6 O60 W12
CELLZ01_ALERT_1_G Difference between formula and atom_site contents detected.
CELLZ01_ALERT_1_G WARNING: H atoms missing from atom site list. Is this intentional?
           From the CIF: _cell_formula_units_Z    1
           From the CIF: _chemical_formula_sum  C12 H62 N4 Na6 O60 W12
           TEST: Compare cell contents of formula and atom_site data

           atom    Z*formula  cif sites diff
           C         12.00     12.00    0.00
           H         62.00     56.00    6.00
           N          4.00      4.00    0.00
           Na         6.00      6.00    0.00
           O         60.00     60.00    0.00
           W         12.00     12.00    0.00
PLAT003_ALERT_2_G Number of Uiso or Uij Restrained non-H Atoms ...          2 Report
PLAT004_ALERT_5_G Polymeric Structure Found with Maximum Dimension          3 Info
PLAT007_ALERT_5_G Number of Unrefined Donor-H Atoms ..............          6 Report
PLAT042_ALERT_1_G Calc. and Reported Moiety Formula Strings Differ     Please Check
PLAT045_ALERT_1_G Calculated and Reported Z Differ by a Factor ...       2.00 Check
PLAT083_ALERT_2_G SHELXL Second Parameter in WGHT  Unusually Large       5.20 Why ?
PLAT154_ALERT_1_G The s.u.'s on the Cell Angles are Equal ..(Note)      0.002 Degree
PLAT178_ALERT_4_G The CIF-Embedded .res File Contains SIMU Records          1 Report
PLAT301_ALERT_3_G Main Residue  Disorder ..............(Resd  1  )         1% Note
PLAT302_ALERT_4_G Anion/Solvent/Minor-Residue Disorder (Resd  2  )       100% Note
PLAT311_ALERT_2_G Isolated Disordered Oxygen Atom (No H's ?) .....       O30B Check
PLAT780_ALERT_1_G Coordinates do not Form a Properly Connected Set     Please Do !
PLAT793_ALERT_4_G Model has Chirality at C2          (Centro SPGR)          R Verify
PLAT793_ALERT_4_G Model has Chirality at C5          (Centro SPGR)          R Verify
PLAT794_ALERT_5_G Tentative Bond Valency for W1        (VI)      .       6.00 Info
PLAT794_ALERT_5_G Tentative Bond Valency for W2        (VI)      .       6.03 Info
PLAT794_ALERT_5_G Tentative Bond Valency for W3        (VI)      .       6.09 Info
PLAT794_ALERT_5_G Tentative Bond Valency for W4        (VI)      .       6.12 Info
PLAT794_ALERT_5_G Tentative Bond Valency for W5        (VI)      .       6.16 Info
PLAT794_ALERT_5_G Tentative Bond Valency for W6        (VI)      .       6.10 Info
PLAT860_ALERT_3_G Number of Least-Squares Restraints .............          6 Note
PLAT898_ALERT_4_G Second Reported H-M Symbol in CIF Ignored ......          ! Check
PLAT910_ALERT_3_G Missing # of FCF Reflection(s) Below Theta(Min).          3 Note
PLAT933_ALERT_2_G Number of HKL-OMIT Records in Embedded .res File         12 Note

   0 ALERT level A = Most likely a serious problem - resolve or explain
   0 ALERT level B = A potentially serious problem, consider carefully
  23 ALERT level C = Check. Ensure it is not caused by an omission or oversight
  28 ALERT level G = General information/check it is not something unexpected

  10 ALERT type 1 CIF construction/syntax error, inconsistent or missing data
  20 ALERT type 2 Indicator that the structure model may be wrong or deficient
   8 ALERT type 3 Indicator that the structure quality may be low
   5 ALERT type 4 Improvement, methodology, query or suggestion
   8 ALERT type 5 Informative message, check

Computing details top

Data collection: APEX3 (Bruker, 2016); cell refinement: SAINT (Bruker, 2016); data reduction: SAINT (Bruker, 2016); program(s) used to solve structure: olex2.solve (Bourhis et al., 2015); program(s) used to refine structure: SHELXL (Sheldrick, 2015); molecular graphics: OLEX2 (Dolomanov et al., 2009); software used to prepare material for publication: OLEX2 (Dolomanov et al., 2009).

Hexasodium tetraserinolium di-µ₃-hydroxido-tetra-µ₃-oxido-octadeca-µ-oxido-octadecaoxidododecatungstate decahydrate top

Crystal data top

[Na₆(C₃H₁₀NO₂)₄][W₁₂O₄₀(OH)₂]·10H₂O	Z = 1
M_r = 3566.79	F(000) = 1596
Triclinic, P1	D_x = 3.943 Mg m⁻³
a = 12.0541 (8) Å	Mo Kα radiation, λ = 0.71073 Å
b = 12.0821 (8) Å	Cell parameters from 9742 reflections
c = 12.7050 (8) Å	θ = 2.2–33.1°
α = 73.180 (2)°	µ = 23.04 mm⁻¹
β = 65.308 (2)°	T = 200 K
γ = 64.345 (2)°	Block, clear colourless
V = 1502.07 (17) Å³	0.05 × 0.05 × 0.05 mm

Data collection top

Bruker APEXII CCD diffractometer	5404 reflections with I > 2σ(I)
Radiation source: sealed x-ray tube	R_int = 0.038
φ and ω scans	θ_max = 25.4°, θ_min = 2.2°
Absorption correction: multi-scan (SADABS; Krause et al., 2015)	h = −14→14
T_min = 0.245, T_max = 0.747	k = −14→14
39702 measured reflections	l = −15→15
5490 independent reflections

Refinement top

Refinement on F²	Primary atom site location: iterative
Least-squares matrix: full	Hydrogen site location: mixed
R[F² > 2σ(F²)] = 0.017	H atoms treated by a mixture of independent and constrained refinement
wR(F²) = 0.043	w = 1/[σ²(F_o²) + (0.0095P)² + 5.2022P] where P = (F_o² + 2F_c²)/3
S = 1.25	(Δ/σ)_max = 0.002
5490 reflections	Δρ_max = 0.99 e Å⁻³
472 parameters	Δρ_min = −1.61 e Å⁻³
6 restraints

Special details top

Geometry. All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes.

Refinement. olex2_refinement_description 1. Fixed Uiso At 1.2 times of: All C(H) groups, All C(H,H) groups, All O(H) groups At 1.5 times of: All N(H,H,H) groups, All O(H,H) groups 2. Uiso/Uaniso restraints and constraints O30A ~ O30B: within 2A with sigma of 0.04 and sigma for terminal atoms of 0.08 within 2A 3. Others Sof(O30A)=1-FVAR(1) Sof(O30B)=FVAR(1) 4.a Ternary CH refined with riding coordinates: C2(H2), C5(H5) 4.b Secondary CH2 refined with riding coordinates: C1(H1D,H1E), C3(H3A,H3B), C4(H4A,H4B), C6(H6A,H6B) 4.c Idealised Me refined as rotating group: N1(H1A,H1B,H1C), N2(H2A,H2B,H2C)

Fractional atomic coordinates and isotropic or equivalent isotropic displacement parameters (Å²) top

	x	y	z	U_iso*/U_eq	Occ. (<1)
W1	0.42560 (2)	0.74680 (2)	0.16437 (2)	0.00609 (5)
W2	0.38107 (2)	0.76530 (2)	0.46722 (2)	0.00492 (5)
W3	0.43557 (2)	0.58129 (2)	0.71174 (2)	0.00468 (5)
W4	0.70356 (2)	0.65943 (2)	0.21152 (2)	0.00538 (5)
W5	0.66091 (2)	0.68816 (2)	0.50890 (2)	0.00550 (5)
W6	0.79490 (2)	0.36191 (2)	0.62441 (2)	0.00589 (5)
Na1	0.2506 (2)	0.6297 (2)	0.05508 (18)	0.0188 (4)
Na2	0.2644 (2)	0.32264 (19)	0.11025 (19)	0.0195 (5)
Na3	−0.1267 (2)	−0.09506 (18)	0.40382 (18)	0.0166 (4)
O1	0.3975 (3)	0.7093 (3)	0.0574 (3)	0.0103 (7)
O2	0.2557 (3)	0.7800 (3)	0.2802 (3)	0.0091 (7)
O3	0.4137 (3)	0.9003 (3)	0.1124 (3)	0.0119 (7)
O4	0.6114 (3)	0.6631 (3)	0.1144 (3)	0.0077 (7)
O5	0.4911 (3)	0.7439 (3)	0.3094 (3)	0.0068 (6)
O6	0.2927 (3)	0.6703 (3)	0.4788 (3)	0.0098 (7)
O7	0.2695 (3)	0.9141 (3)	0.4594 (3)	0.0114 (7)
O8	0.5351 (3)	0.5906 (3)	0.5163 (3)	0.0061 (6)
O9	0.5209 (3)	0.8146 (3)	0.4727 (3)	0.0070 (6)
O10	0.3393 (3)	0.7379 (3)	0.6367 (3)	0.0058 (6)
O11	0.3480 (3)	0.5000 (3)	0.6978 (3)	0.0096 (7)
O12	0.3556 (3)	0.6163 (3)	0.8530 (3)	0.0108 (7)
O13	0.5815 (3)	0.4361 (3)	0.7240 (3)	0.0077 (7)
O14	0.5651 (3)	0.6687 (3)	0.6669 (3)	0.0081 (7)
O15	0.7266 (3)	0.7992 (3)	0.1354 (3)	0.0116 (7)
O16	0.8550 (3)	0.5513 (3)	0.1411 (3)	0.0092 (7)
O17	0.7336 (3)	0.6599 (3)	0.3434 (3)	0.0088 (7)
O18	0.7542 (3)	0.7663 (3)	0.5051 (3)	0.0113 (7)
O19	0.7760 (3)	0.5146 (3)	0.5302 (3)	0.0090 (7)
O20	0.9485 (3)	0.2716 (3)	0.5427 (3)	0.0104 (7)
O21	0.8303 (3)	0.3935 (3)	0.7318 (3)	0.0113 (7)
O22	0.3854 (4)	0.4292 (4)	0.1050 (4)	0.0193 (9)
H22A	0.447 (7)	0.401 (7)	0.068 (6)	0.029*
H22B	0.397 (7)	0.418 (6)	0.174 (6)	0.029*
O23	0.1180 (4)	0.5313 (4)	0.0558 (3)	0.0156 (8)
H23A	0.138 (7)	0.511 (6)	−0.005 (6)	0.023*
H23B	0.032 (7)	0.540 (6)	0.087 (6)	0.023*
O24	0.1349 (4)	0.3728 (4)	0.3060 (4)	0.0203 (9)
H24A	0.155 (7)	0.334 (6)	0.368 (6)	0.030*
H24B	0.143 (8)	0.423 (7)	0.300 (7)	0.030*
O25	0.3957 (4)	0.1204 (3)	0.1540 (4)	0.0187 (8)
H25	0.390 (7)	0.070 (6)	0.137 (6)	0.022*
O26	0.1374 (4)	0.2320 (4)	0.0943 (4)	0.0260 (9)
H26	0.161 (7)	0.230 (6)	0.018 (6)	0.031*
O27	0.0421 (4)	−0.0116 (4)	0.3221 (4)	0.0269 (10)
H27	0.101 (7)	−0.057 (7)	0.313 (7)	0.032*
O28	−0.0593 (4)	−0.2184 (4)	0.2434 (4)	0.0249 (9)
H28A	−0.002 (8)	−0.277 (7)	0.247 (7)	0.037*
H28B	−0.118 (8)	−0.237 (7)	0.254 (7)	0.037*
O29	0.7568 (4)	0.0498 (4)	0.2733 (4)	0.0182 (8)
H29	0.735 (6)	0.119 (6)	0.287 (6)	0.022*
N1	0.6651 (4)	0.0491 (4)	0.0932 (4)	0.0135 (9)
H1A	0.620503	0.082305	0.041998	0.020*
H1B	0.694572	−0.035013	0.100535	0.020*
H1C	0.734329	0.074419	0.066187	0.020*
N2	−0.0763 (4)	0.3259 (4)	0.3009 (4)	0.0123 (9)
H2A	−0.109556	0.387738	0.249053	0.018*
H2B	−0.004148	0.332753	0.301037	0.018*
H2C	−0.137617	0.331930	0.373678	0.018*
C1	0.4520 (5)	0.0653 (5)	0.2438 (5)	0.0165 (11)
H1D	0.472355	−0.025201	0.257484	0.020*
H1E	0.388654	0.099437	0.317357	0.020*
C2	0.5768 (5)	0.0910 (4)	0.2092 (4)	0.0107 (10)
H2	0.554428	0.182003	0.203335	0.013*
C3	0.6425 (5)	0.0233 (5)	0.2991 (5)	0.0162 (11)
H3A	0.580025	0.047163	0.376761	0.019*
H3B	0.667484	−0.066948	0.302642	0.019*
C4	0.0445 (5)	0.1009 (4)	0.3328 (5)	0.0147 (11)
H4A	0.135127	0.100118	0.299111	0.018*
H4B	0.008737	0.113215	0.415968	0.018*
C5	−0.0397 (5)	0.2030 (4)	0.2660 (4)	0.0127 (10)
H5	−0.122474	0.187396	0.290152	0.015*
C6	0.0209 (5)	0.2060 (5)	0.1362 (5)	0.0187 (11)
H6A	0.041210	0.124953	0.115096	0.022*
H6B	−0.041824	0.270265	0.098737	0.022*
O30B	0.9054 (14)	0.105 (2)	−0.080 (3)	0.048 (6)	0.48 (5)
O30A	0.8950 (11)	0.1308 (12)	−0.026 (2)	0.035 (5)	0.52 (5)

Atomic displacement parameters (Å²) top

	U¹¹	U²²	U³³	U¹²	U¹³	U²³
W1	0.00509 (9)	0.00748 (9)	0.00526 (10)	−0.00281 (7)	−0.00147 (7)	0.00021 (7)
W2	0.00343 (9)	0.00618 (9)	0.00481 (10)	−0.00225 (7)	−0.00065 (7)	−0.00056 (7)
W3	0.00345 (9)	0.00601 (9)	0.00437 (10)	−0.00258 (7)	−0.00026 (7)	−0.00063 (7)
W4	0.00401 (9)	0.00709 (9)	0.00488 (10)	−0.00339 (7)	0.00000 (7)	−0.00063 (7)
W5	0.00430 (9)	0.00760 (9)	0.00575 (10)	−0.00427 (7)	−0.00078 (7)	−0.00051 (7)
W6	0.00366 (9)	0.00720 (9)	0.00671 (10)	−0.00237 (7)	−0.00130 (7)	−0.00083 (7)
Na1	0.0206 (11)	0.0287 (12)	0.0124 (10)	−0.0171 (10)	−0.0008 (9)	−0.0044 (9)
Na2	0.0148 (10)	0.0173 (10)	0.0248 (12)	−0.0047 (9)	−0.0068 (9)	−0.0020 (9)
Na3	0.0135 (10)	0.0150 (10)	0.0215 (11)	−0.0074 (8)	−0.0073 (9)	0.0029 (8)
O1	0.0080 (16)	0.0132 (17)	0.0082 (17)	−0.0048 (14)	0.0000 (13)	−0.0018 (13)
O2	0.0094 (16)	0.0104 (16)	0.0090 (17)	−0.0048 (14)	−0.0031 (14)	−0.0011 (13)
O3	0.0143 (18)	0.0096 (16)	0.0126 (18)	−0.0055 (14)	−0.0058 (15)	0.0012 (13)
O4	0.0070 (16)	0.0101 (16)	0.0045 (16)	−0.0027 (13)	−0.0010 (13)	−0.0010 (13)
O5	0.0052 (15)	0.0071 (15)	0.0071 (16)	−0.0013 (13)	−0.0026 (13)	−0.0001 (12)
O6	0.0111 (17)	0.0153 (17)	0.0043 (16)	−0.0079 (14)	−0.0004 (13)	−0.0017 (13)
O7	0.0098 (17)	0.0085 (16)	0.0120 (18)	−0.0016 (14)	−0.0022 (14)	−0.0008 (13)
O8	0.0032 (15)	0.0079 (15)	0.0069 (16)	−0.0031 (13)	−0.0001 (13)	−0.0012 (12)
O9	0.0036 (15)	0.0071 (15)	0.0088 (16)	−0.0021 (13)	−0.0003 (13)	−0.0013 (12)
O10	0.0017 (15)	0.0078 (15)	0.0059 (16)	−0.0012 (12)	0.0006 (12)	−0.0019 (12)
O11	0.0103 (17)	0.0112 (16)	0.0078 (17)	−0.0075 (14)	−0.0010 (14)	0.0006 (13)
O12	0.0072 (16)	0.0120 (16)	0.0103 (18)	−0.0029 (14)	−0.0008 (14)	−0.0017 (13)
O13	0.0056 (16)	0.0111 (16)	0.0066 (16)	−0.0041 (13)	−0.0014 (13)	−0.0009 (13)
O14	0.0071 (16)	0.0094 (16)	0.0085 (17)	−0.0042 (13)	−0.0022 (13)	−0.0011 (13)
O15	0.0125 (17)	0.0122 (17)	0.0109 (17)	−0.0074 (14)	−0.0018 (14)	−0.0011 (13)
O16	0.0040 (15)	0.0124 (16)	0.0095 (17)	−0.0036 (13)	0.0010 (13)	−0.0029 (13)
O17	0.0076 (16)	0.0137 (16)	0.0076 (17)	−0.0069 (14)	−0.0009 (13)	−0.0027 (13)
O18	0.0126 (17)	0.0139 (17)	0.0102 (17)	−0.0105 (15)	−0.0005 (14)	−0.0012 (14)
O19	0.0063 (16)	0.0088 (16)	0.0090 (17)	−0.0021 (13)	−0.0022 (13)	0.0011 (13)
O20	0.0071 (16)	0.0113 (16)	0.0126 (18)	−0.0037 (14)	−0.0027 (14)	−0.0018 (13)
O21	0.0102 (17)	0.0154 (17)	0.0099 (17)	−0.0070 (14)	−0.0016 (14)	−0.0026 (14)
O22	0.0098 (19)	0.033 (2)	0.015 (2)	−0.0058 (18)	0.0002 (16)	−0.0137 (18)
O23	0.0132 (19)	0.026 (2)	0.0117 (19)	−0.0114 (17)	−0.0014 (16)	−0.0046 (16)
O24	0.027 (2)	0.024 (2)	0.019 (2)	−0.0165 (19)	−0.0117 (18)	0.0022 (18)
O25	0.019 (2)	0.0128 (18)	0.028 (2)	−0.0040 (16)	−0.0139 (17)	−0.0027 (16)
O26	0.031 (2)	0.039 (2)	0.013 (2)	−0.024 (2)	0.0030 (18)	−0.0063 (18)
O27	0.013 (2)	0.012 (2)	0.052 (3)	−0.0004 (16)	−0.010 (2)	−0.0046 (19)
O28	0.013 (2)	0.028 (2)	0.033 (2)	−0.0048 (18)	−0.0076 (19)	−0.0059 (19)
O29	0.0168 (19)	0.0132 (18)	0.032 (2)	−0.0031 (16)	−0.0137 (17)	−0.0076 (16)
N1	0.018 (2)	0.010 (2)	0.010 (2)	−0.0072 (18)	−0.0023 (18)	0.0010 (16)
N2	0.008 (2)	0.015 (2)	0.011 (2)	−0.0023 (17)	−0.0015 (17)	−0.0014 (17)
C1	0.014 (3)	0.022 (3)	0.015 (3)	−0.008 (2)	−0.005 (2)	−0.002 (2)
C2	0.010 (2)	0.007 (2)	0.013 (3)	−0.0018 (19)	−0.003 (2)	−0.0036 (19)
C3	0.019 (3)	0.013 (2)	0.017 (3)	−0.005 (2)	−0.008 (2)	−0.001 (2)
C4	0.014 (3)	0.013 (2)	0.016 (3)	−0.003 (2)	−0.005 (2)	−0.003 (2)
C5	0.005 (2)	0.016 (2)	0.018 (3)	−0.006 (2)	−0.002 (2)	−0.003 (2)
C6	0.016 (3)	0.021 (3)	0.022 (3)	−0.004 (2)	−0.012 (2)	−0.003 (2)
O30B	0.048 (7)	0.092 (10)	0.028 (11)	−0.052 (7)	−0.011 (7)	0.000 (9)
O30A	0.046 (6)	0.048 (7)	0.027 (10)	−0.030 (5)	−0.017 (5)	0.001 (5)

Geometric parameters (Å, º) top

W1—O1	1.743 (3)	Na2—O25	2.321 (4)
W1—O2	1.906 (3)	Na2—O26	2.328 (5)
W1—O3	1.742 (3)	Na3—O7^iv	2.684 (4)
W1—O4	1.914 (3)	Na3—O18^v	2.411 (4)
W1—O5	2.274 (3)	Na3—O20^vi	2.458 (4)
W1—O13ⁱ	2.270 (3)	Na3—O27	2.375 (5)
W2—O5	1.905 (3)	Na3—O28	2.522 (5)
W2—O6	1.818 (3)	Na3—O29^vii	2.434 (4)
W2—O7	1.723 (3)	O22—H22A	0.68 (7)
W2—O8	2.259 (3)	O22—H22B	0.90 (7)
W2—O9	2.047 (3)	O23—H23A	0.78 (7)
W2—O10	1.956 (3)	O23—H23B	0.91 (7)
W3—O8	2.255 (3)	O24—H24A	0.86 (7)
W3—O10	1.953 (3)	O24—H24B	0.63 (7)
W3—O11	1.807 (3)	O25—H25	0.73 (7)
W3—O12	1.723 (3)	O25—C1	1.422 (7)
W3—O13	1.896 (3)	O26—H26	0.89 (7)
W3—O14	2.052 (3)	O26—C6	1.420 (7)
W4—O4	1.957 (3)	O27—H27	0.67 (7)
W4—O5	2.227 (3)	O27—C4	1.418 (6)
W4—O11ⁱ	2.140 (3)	O28—H28A	0.75 (8)
W4—O15	1.761 (3)	O28—H28B	0.79 (8)
W4—O16	1.757 (3)	O29—H29	0.81 (7)
W4—O17	1.858 (3)	O29—C3	1.432 (6)
W5—O8	2.251 (3)	N1—H1A	0.9100
W5—O9	1.845 (3)	N1—H1B	0.9100
W5—O14	1.856 (3)	N1—H1C	0.9100
W5—O17	1.980 (3)	N1—C2	1.489 (6)
W5—O18	1.734 (3)	N2—H2A	0.9100
W5—O19	1.965 (3)	N2—H2B	0.9100
W6—O2ⁱ	1.966 (3)	N2—H2C	0.9100
W6—O6ⁱ	2.189 (3)	N2—C5	1.498 (6)
W6—O13	2.228 (3)	C1—H1D	0.9900
W6—O19	1.864 (3)	C1—H1E	0.9900
W6—O20	1.731 (3)	C1—C2	1.525 (7)
W6—O21	1.765 (3)	C2—H2	1.0000
Na1—Na2	3.513 (3)	C2—C3	1.502 (7)
Na1—O1	2.365 (4)	C3—H3A	0.9900
Na1—O12ⁱⁱ	2.360 (4)	C3—H3B	0.9900
Na1—O21ⁱ	2.440 (4)	C4—H4A	0.9900
Na1—O22	2.339 (5)	C4—H4B	0.9900
Na1—O23	2.365 (4)	C4—C5	1.517 (7)
Na1—O30Bⁱⁱⁱ	2.96 (3)	C5—H5	1.0000
Na1—O30Aⁱⁱⁱ	2.668 (12)	C5—C6	1.496 (7)
Na2—O4ⁱⁱⁱ	2.606 (4)	C6—H6A	0.9900
Na2—O22	2.299 (4)	C6—H6B	0.9900
Na2—O23	2.471 (4)	O30B—O30A	0.772 (14)
Na2—O24	2.409 (5)

O1—W1—O2	99.34 (14)	O24—Na2—Na1	82.89 (12)
O1—W1—O4	97.41 (14)	O24—Na2—O4ⁱⁱⁱ	163.49 (15)
O1—W1—O5	165.62 (13)	O24—Na2—H22A	99.6 (17)
O1—W1—O13ⁱ	90.34 (13)	O24—Na2—O23	83.19 (15)
O2—W1—O4	152.13 (14)	O24—Na2—H23A	99.9 (16)
O2—W1—O5	85.31 (13)	O24—Na2—H24B	14.0 (16)
O2—W1—O13ⁱ	72.81 (12)	O25—Na2—Na1	141.81 (13)
O3—W1—O1	101.50 (15)	O25—Na2—O4ⁱⁱⁱ	95.66 (14)
O3—W1—O2	97.16 (15)	O25—Na2—H22A	91.2 (16)
O3—W1—O4	101.13 (15)	O25—Na2—O23	175.41 (17)
O3—W1—O5	91.33 (14)	O25—Na2—H23A	158.6 (16)
O3—W1—O13ⁱ	165.73 (14)	O25—Na2—O24	99.07 (17)
O4—W1—O5	73.49 (12)	O25—Na2—H24B	107.6 (17)
O4—W1—O13ⁱ	85.00 (12)	O25—Na2—O26	84.84 (16)
O13ⁱ—W1—O5	77.96 (11)	O26—Na2—Na1	133.01 (14)
O5—W2—O8	85.93 (12)	O26—Na2—O4ⁱⁱⁱ	91.27 (14)
O5—W2—O9	84.55 (13)	O26—Na2—H22A	162.9 (17)
O5—W2—O10	155.42 (13)	O26—Na2—O23	90.92 (16)
O6—W2—O5	95.34 (14)	O26—Na2—H23A	82.9 (15)
O6—W2—O8	88.22 (13)	O26—Na2—O24	97.41 (16)
O6—W2—O9	160.42 (14)	O26—Na2—H24B	108.9 (17)
O6—W2—O10	91.33 (13)	O18^v—Na3—O7^iv	99.45 (13)
O7—W2—O5	104.66 (15)	O18^v—Na3—O20^vi	82.68 (13)
O7—W2—O6	103.57 (16)	O18^v—Na3—O28	79.23 (14)
O7—W2—O8	163.09 (14)	O18^v—Na3—O29^vii	104.03 (14)
O7—W2—O9	95.34 (14)	O20^vi—Na3—O7^iv	118.30 (13)
O7—W2—O10	96.66 (14)	O20^vi—Na3—O28	82.88 (14)
O9—W2—O8	72.23 (11)	O27—Na3—O7^iv	88.69 (14)
O10—W2—O8	70.63 (12)	O27—Na3—O18^v	162.22 (16)
O10—W2—O9	81.39 (13)	O27—Na3—O20^vi	79.54 (14)
O10—W3—O8	70.79 (12)	O27—Na3—O28	98.85 (17)
O10—W3—O14	82.41 (13)	O27—Na3—O29^vii	92.51 (16)
O11—W3—O8	87.05 (13)	O28—Na3—O7^iv	158.61 (15)
O11—W3—O10	92.51 (14)	O29^vii—Na3—O7^iv	83.56 (13)
O11—W3—O13	94.39 (14)	O29^vii—Na3—O20^vi	156.19 (16)
O11—W3—O14	160.06 (14)	O29^vii—Na3—O28	76.17 (15)
O12—W3—O8	164.22 (13)	W1—O1—Na1	135.79 (18)
O12—W3—O10	97.08 (14)	W1—O2—W6ⁱ	117.99 (16)
O12—W3—O11	103.95 (15)	W1—O4—W4	117.48 (16)
O12—W3—O13	103.07 (15)	W1—O4—Na2ⁱⁱⁱ	116.67 (15)
O12—W3—O14	95.83 (14)	W4—O4—Na2ⁱⁱⁱ	116.38 (15)
O13—W3—O8	87.06 (13)	W2—O5—W1	125.33 (15)
O13—W3—O10	156.41 (13)	W2—O5—W4	137.59 (16)
O13—W3—O14	83.45 (13)	W4—O5—W1	94.63 (12)
O14—W3—O8	73.06 (12)	W2—O6—W6ⁱ	139.38 (17)
O4—W4—O5	73.85 (12)	W2—O7—Na3^iv	137.29 (18)
O4—W4—O11ⁱ	81.97 (13)	W3—O8—W2	97.22 (12)
O11ⁱ—W4—O5	77.76 (12)	W5—O8—W2	94.75 (11)
O15—W4—O4	92.61 (14)	W5—O8—W3	94.52 (12)
O15—W4—O5	96.44 (14)	W5—O9—W2	116.91 (15)
O15—W4—O11ⁱ	172.94 (14)	W3—O10—W2	120.08 (15)
O15—W4—O17	96.69 (15)	W3—O11—W4ⁱ	136.32 (18)
O16—W4—O4	96.54 (14)	W3—O12—Na1^viii	170.67 (19)
O16—W4—O5	160.85 (13)	W3—O13—W1ⁱ	126.28 (15)
O16—W4—O11ⁱ	84.60 (13)	W3—O13—W6	137.29 (16)
O16—W4—O15	100.58 (15)	W6—O13—W1ⁱ	95.12 (12)
O16—W4—O17	99.46 (15)	W5—O14—W3	115.64 (16)
O17—W4—O4	159.66 (14)	W4—O17—W5	148.36 (18)
O17—W4—O5	87.12 (13)	W5—O18—Na3^ix	150.89 (19)
O17—W4—O11ⁱ	87.11 (13)	W6—O19—W5	146.16 (18)
O9—W5—O8	76.09 (12)	W6—O20—Na3^vi	132.86 (18)
O9—W5—O14	93.33 (14)	W6—O21—Na1ⁱ	135.54 (18)
O9—W5—O17	86.47 (14)	Na1—O22—H22A	122 (6)
O9—W5—O19	154.74 (14)	Na1—O22—H22B	114 (4)
O14—W5—O8	76.78 (12)	Na2—O22—Na1	98.47 (16)
O14—W5—O17	156.72 (13)	Na2—O22—H22A	104 (6)
O14—W5—O19	87.83 (14)	Na2—O22—H22B	113 (4)
O17—W5—O8	80.60 (12)	H22A—O22—H22B	104 (7)
O18—W5—O8	178.51 (14)	Na1—O23—Na2	93.15 (15)
O18—W5—O9	102.80 (15)	Na1—O23—H23A	113 (5)
O18—W5—O14	102.35 (15)	Na1—O23—H23B	138 (4)
O18—W5—O17	100.38 (14)	Na2—O23—H23A	88 (5)
O18—W5—O19	101.57 (15)	Na2—O23—H23B	113 (4)
O19—W5—O8	79.64 (12)	H23A—O23—H23B	101 (6)
O19—W5—O17	82.74 (13)	Na2—O24—H24A	126 (5)
O2ⁱ—W6—O6ⁱ	77.66 (13)	Na2—O24—H24B	98 (7)
O2ⁱ—W6—O13	72.73 (12)	H24A—O24—H24B	101 (8)
O6ⁱ—W6—O13	76.98 (12)	Na2—O25—H25	118 (5)
O19—W6—O2ⁱ	156.59 (14)	C1—O25—Na2	130.9 (3)
O19—W6—O6ⁱ	84.75 (13)	C1—O25—H25	107 (5)
O19—W6—O13	88.45 (13)	Na2—O26—H26	106 (4)
O20—W6—O2ⁱ	94.54 (14)	C6—O26—Na2	150.9 (3)
O20—W6—O6ⁱ	90.10 (14)	C6—O26—H26	100 (4)
O20—W6—O13	163.39 (13)	Na3—O27—H27	110 (6)
O20—W6—O19	100.87 (15)	C4—O27—Na3	131.5 (3)
O20—W6—O21	101.60 (16)	C4—O27—H27	112 (6)
O21—W6—O2ⁱ	95.80 (14)	Na3—O28—H28A	110 (6)
O21—W6—O6ⁱ	167.09 (14)	Na3—O28—H28B	107 (6)
O21—W6—O13	90.50 (14)	H28A—O28—H28B	108 (8)
O21—W6—O19	98.20 (15)	Na3^x—O29—H29	108 (5)
O1—Na1—Na2	130.03 (12)	C3—O29—Na3^x	107.8 (3)
O1—Na1—O21ⁱ	87.94 (13)	C3—O29—H29	109 (5)
O1—Na1—O30Bⁱⁱⁱ	75.4 (4)	H1A—N1—H1B	109.5
O1—Na1—O30Aⁱⁱⁱ	82.9 (4)	H1A—N1—H1C	109.5
O12ⁱⁱ—Na1—Na2	90.80 (11)	H1B—N1—H1C	109.5
O12ⁱⁱ—Na1—O1	91.95 (13)	C2—N1—H1A	109.5
O12ⁱⁱ—Na1—O21ⁱ	169.87 (16)	C2—N1—H1B	109.5
O12ⁱⁱ—Na1—O23	87.84 (14)	C2—N1—H1C	109.5
O12ⁱⁱ—Na1—O30Bⁱⁱⁱ	106.9 (5)	H2A—N2—H2B	109.5
O12ⁱⁱ—Na1—O30Aⁱⁱⁱ	94.4 (6)	H2A—N2—H2C	109.5
O21ⁱ—Na1—Na2	81.56 (10)	H2B—N2—H2C	109.5
O21ⁱ—Na1—O30Bⁱⁱⁱ	82.9 (6)	C5—N2—H2A	109.5
O21ⁱ—Na1—O30Aⁱⁱⁱ	95.6 (6)	C5—N2—H2B	109.5
O22—Na1—Na2	40.33 (11)	C5—N2—H2C	109.5
O22—Na1—O1	89.70 (15)	O25—C1—H1D	109.6
O22—Na1—O12ⁱⁱ	92.67 (15)	O25—C1—H1E	109.6
O22—Na1—O21ⁱ	77.19 (14)	O25—C1—C2	110.2 (4)
O22—Na1—O23	84.94 (15)	H1D—C1—H1E	108.1
O22—Na1—O30Bⁱⁱⁱ	155.5 (6)	C2—C1—H1D	109.6
O22—Na1—O30Aⁱⁱⁱ	169.9 (6)	C2—C1—H1E	109.6
O23—Na1—Na2	44.61 (11)	N1—C2—C1	108.4 (4)
O23—Na1—O1	174.62 (17)	N1—C2—H2	109.3
O23—Na1—O21ⁱ	91.32 (14)	N1—C2—C3	110.2 (4)
O23—Na1—O30Bⁱⁱⁱ	109.8 (4)	C1—C2—H2	109.3
O23—Na1—O30Aⁱⁱⁱ	102.5 (4)	C3—C2—C1	110.2 (4)
O30Bⁱⁱⁱ—Na1—Na2	149.3 (2)	C3—C2—H2	109.3
O30Aⁱⁱⁱ—Na1—Na2	146.5 (3)	O29—C3—C2	112.1 (4)
O30Aⁱⁱⁱ—Na1—O30Bⁱⁱⁱ	14.6 (2)	O29—C3—H3A	109.2
Na1—Na2—H22A	51.3 (16)	O29—C3—H3B	109.2
Na1—Na2—H23A	51.3 (15)	C2—C3—H3A	109.2
Na1—Na2—H24B	69.2 (17)	C2—C3—H3B	109.2
O4ⁱⁱⁱ—Na2—Na1	80.92 (9)	H3A—C3—H3B	107.9
O4ⁱⁱⁱ—Na2—H22A	72.6 (17)	O27—C4—H4A	110.5
O4ⁱⁱⁱ—Na2—H23A	67.2 (16)	O27—C4—H4B	110.5
O4ⁱⁱⁱ—Na2—H24B	150.2 (17)	O27—C4—C5	106.2 (4)
O22—Na2—Na1	41.20 (11)	H4A—C4—H4B	108.7
O22—Na2—O4ⁱⁱⁱ	83.35 (14)	C5—C4—H4A	110.5
O22—Na2—H22A	15.0 (16)	C5—C4—H4B	110.5
O22—Na2—O23	83.43 (15)	N2—C5—C4	110.1 (4)
O22—Na2—H23A	90.4 (15)	N2—C5—H5	107.2
O22—Na2—O24	86.63 (15)	C4—C5—H5	107.2
O22—Na2—H24B	74.3 (17)	C6—C5—N2	111.0 (4)
O22—Na2—O25	100.64 (16)	C6—C5—C4	113.9 (4)
O22—Na2—O26	172.64 (19)	C6—C5—H5	107.2
H22A—Na2—H23A	95 (2)	O26—C6—C5	110.7 (4)
H22A—Na2—H24B	88 (2)	O26—C6—H6A	109.5
O23—Na2—Na1	42.24 (10)	O26—C6—H6B	109.5
O23—Na2—O4ⁱⁱⁱ	82.65 (13)	C5—C6—H6A	109.5
O23—Na2—H22A	92.4 (16)	C5—C6—H6B	109.5
O23—Na2—H23A	17.7 (15)	H6A—C6—H6B	108.1
O23—Na2—H24B	75.5 (17)	O30A—O30B—Na1ⁱⁱⁱ	60.3 (18)
H23A—Na2—H24B	93 (2)	O30B—O30A—Na1ⁱⁱⁱ	105 (2)

Na2—O25—C1—C2	−81.3 (5)	O11ⁱ—W4—O17—W5	−70.5 (3)
Na2—O26—C6—C5	−28.2 (9)	O12—W3—O11—W4ⁱ	−55.6 (3)
Na3—O27—C4—C5	−70.6 (6)	O12—W3—O13—W1ⁱ	60.5 (2)
Na3^x—O29—C3—C2	−169.3 (3)	O12—W3—O13—W6	−136.2 (2)
O2—W1—O1—Na1	−25.9 (3)	O13ⁱ—W1—O1—Na1	46.8 (3)
O2ⁱ—W6—O19—W5	47.2 (6)	O13—W3—O11—W4ⁱ	49.1 (3)
O2ⁱ—W6—O20—Na3^vi	−50.9 (2)	O13—W6—O19—W5	11.3 (3)
O2ⁱ—W6—O21—Na1ⁱ	−30.6 (3)	O13—W6—O20—Na3^vi	−90.0 (5)
O3—W1—O1—Na1	−125.2 (3)	O13—W6—O21—Na1ⁱ	42.1 (3)
O4—W1—O1—Na1	131.8 (2)	O14—W3—O11—W4ⁱ	132.0 (3)
O4—W4—O17—W5	−13.1 (6)	O14—W3—O13—W1ⁱ	155.0 (2)
O5—W1—O1—Na1	82.1 (6)	O14—W3—O13—W6	−41.7 (2)
O5—W2—O6—W6ⁱ	−42.3 (3)	O14—W5—O9—W2	−76.39 (18)
O5—W2—O7—Na3^iv	−150.8 (2)	O14—W5—O18—Na3^ix	−153.2 (4)
O5—W4—O17—W5	7.4 (3)	O15—W4—O17—W5	103.5 (3)
O6—W2—O7—Na3^iv	109.9 (2)	O16—W4—O17—W5	−154.6 (3)
O6ⁱ—W6—O19—W5	88.4 (3)	O17—W5—O9—W2	80.29 (17)
O6ⁱ—W6—O20—Na3^vi	−128.5 (2)	O17—W5—O14—W3	−13.9 (4)
O6ⁱ—W6—O21—Na1ⁱ	28.1 (8)	O17—W5—O18—Na3^ix	31.8 (4)
O7—W2—O6—W6ⁱ	64.3 (3)	O18—W5—O9—W2	−179.85 (17)
O8—W2—O6—W6ⁱ	−128.0 (3)	O18—W5—O14—W3	178.84 (17)
O8—W2—O7—Na3^iv	−23.3 (6)	O19—W5—O9—W2	15.6 (4)
O8—W3—O11—W4ⁱ	135.9 (2)	O19—W5—O14—W3	−79.79 (17)
O8—W3—O13—W1ⁱ	−131.77 (19)	O19—W5—O18—Na3^ix	116.5 (4)
O8—W3—O13—W6	31.6 (2)	O19—W6—O20—Na3^vi	146.9 (2)
O8—W5—O9—W2	−0.89 (15)	O19—W6—O21—Na1ⁱ	130.6 (2)
O8—W5—O14—W3	0.08 (15)	O20—W6—O19—W5	177.5 (3)
O9—W2—O6—W6ⁱ	−131.0 (3)	O20—W6—O21—Na1ⁱ	−126.5 (3)
O9—W2—O7—Na3^iv	−65.0 (3)	O21—W6—O19—W5	−79.0 (3)
O9—W5—O14—W3	74.95 (18)	O21—W6—O20—Na3^vi	46.0 (3)
O9—W5—O18—Na3^ix	−56.9 (4)	O25—C1—C2—N1	−54.2 (5)
O10—W2—O6—W6ⁱ	161.4 (3)	O25—C1—C2—C3	−174.9 (4)
O10—W2—O7—Na3^iv	16.9 (3)	O27—C4—C5—N2	163.1 (4)
O10—W3—O11—W4ⁱ	−153.5 (2)	O27—C4—C5—C6	−71.6 (5)
O10—W3—O13—W1ⁱ	−151.6 (2)	N1—C2—C3—O29	63.4 (5)
O10—W3—O13—W6	11.8 (5)	N2—C5—C6—O26	61.3 (5)
O11—W3—O13—W1ⁱ	−45.0 (2)	C1—C2—C3—O29	−177.0 (4)
O11—W3—O13—W6	118.4 (2)	C4—C5—C6—O26	−63.6 (6)

Symmetry codes: (i) −x+1, −y+1, −z+1; (ii) x, y, z−1; (iii) −x+1, −y+1, −z; (iv) −x, −y+1, −z+1; (v) x−1, y−1, z; (vi) −x+1, −y, −z+1; (vii) x−1, y, z; (viii) x, y, z+1; (ix) x+1, y+1, z; (x) x+1, y, z.

Hydrogen-bond geometry (Å, º) top

D—H···A	D—H	H···A	D···A	D—H···A
O22—H22A···O1ⁱⁱⁱ	0.67 (7)	2.11 (7)	2.757 (5)	163 (8)
O23—H23A···O16ⁱⁱⁱ	0.78 (7)	2.04 (7)	2.802 (5)	165 (7)
O23—H23B···O16^vii	0.91 (7)	1.91 (7)	2.811 (5)	175 (6)
O25—H25···O3^xi	0.73 (6)	2.05 (7)	2.761 (5)	164 (7)
O26—H26···O15ⁱⁱⁱ	0.88 (7)	1.88 (7)	2.730 (5)	160 (6)
O27—H27···O2^xi	0.67 (7)	2.04 (7)	2.696 (5)	165 (8)
O28—H28A···O21^vi	0.75 (8)	2.01 (8)	2.735 (6)	160 (8)
O29—H29···O10ⁱ	0.81 (6)	1.91 (7)	2.692 (5)	163 (6)
N1—H1B···O15^xi	0.91	1.82	2.723 (5)	170
N2—H2B···O24	0.91	1.96	2.867 (6)	172

Symmetry codes: (i) −x+1, −y+1, −z+1; (iii) −x+1, −y+1, −z; (vi) −x+1, −y, −z+1; (vii) x−1, y, z; (xi) x, y−1, z.

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Crystal structure of hexa­sodium tetra­serinolium paratungstate B deca­hydrate, [Na6{(CH2OH)2CHNH3}4][W12O40(OH)2]·10H2O

Supporting information

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checkCIF/PLATON results

Crystal structure of hexasodium tetraserinolium paratungstate B decahydrate, [Na₆{(CH₂OH)₂CHNH₃}₄][W₁₂O₄₀(OH)₂]·10H₂O