Crystal structure of hepta­guanidinium nona­hydrogen bis­[α-hexa­molybdoplatinate(IV)] hepta­hydrate

A compound, (CH₆N₃)₇H₉[PtMo₆O₂₄]₂·7H₂O, containing the well-known Anderson-structure heteropolyoxomolybdate, was obtained by recrystallization of its powdered guanidinium salt. The protonated O atoms in the polyanion were confirmed by electron-density maps, inter­polyanion hydrogen bonds and bond-valance sums (BVS).

Key indicators

• Single-crystal X-ray study
• T = 173 K
• Mean [sigma](N-C) = 0.008 Å
• Disorder in solvent or counterion
• R factor = 0.028
• wR factor = 0.073
• Data-to-parameter ratio = 14.1

checkCIF/PLATON results

No syntax errors found



Alert level B
PLAT416_ALERT_2_B Short Intra D-H..H-D       H10A   ..  H12A    ..       1.77 Ang.

Author Response: No problem. Because each other disordered Atoms.

PLAT417_ALERT_2_B Short Inter D-H..H-D       H3     ..  H2AW    ..       2.06 Ang.

Author Response: Because of strong H3...O2w HY bond (2.622 \%A) and disorder.

PLAT417_ALERT_2_B Short Inter D-H..H-D       H3     ..  H2BW    ..       2.06 Ang.

Author Response: Because of strong H3...O2w HY bond (2.622 \%A) and disorder.

PLAT417_ALERT_2_B Short Inter D-H..H-D       H2AW   ..  H3A     ..       1.98 Ang.

Author Response: Because of strong H3...O2w HY bond (2.622 \%A) and disorder.

PLAT417_ALERT_2_B Short Inter D-H..H-D       H3BW   ..  H4BW    ..       1.94 Ang.

Author Response: Because of strong H3...O2w HY bond (2.622 \%A) and disorder.

PLAT420_ALERT_2_B D-H Without Acceptor        O2W    -   H2AW   ..     Please Check

Author Response: Because the acceptor atoms were disorder atom.

Alert level C
PLAT244_ALERT_4_C Low   'Solvent' Ueq as Compared to Neighbors of          C1 Check
PLAT244_ALERT_4_C Low   'Solvent' Ueq as Compared to Neighbors of          C3 Check
PLAT303_ALERT_2_C Full Occupancy H-Atom  H6     with # Connections       2.00 Check

Author Response: Because H6 has half occupation number.

PLAT420_ALERT_2_C D-H Without Acceptor        N9     -   H9B    ..     Please Check

Author Response: Because the acceptor atoms were disorder atom.

PLAT751_ALERT_4_C Bond    Calc     1.27000, Rep    1.266(3) ......  Senseless su
              O6C  -H6      1.555   1.555                #         47
PLAT752_ALERT_4_C Angle   Calc      121.00, Rep    120.8(2) ......  Senseless su
              PT1  -O6C  -H6      1.555   1.555   1.555      #        142
PLAT752_ALERT_4_C Angle   Calc      121.00, Rep  121.27(19) ......  Senseless su
              MO6  -O6C  -H6      1.555   1.555   1.555      #        143
PLAT752_ALERT_4_C Angle   Calc      121.00, Rep  120.85(19) ......  Senseless su
              MO1  -O6C  -H6      1.555   1.555   1.555      #        144
PLAT911_ALERT_3_C Missing # FCF Refl Between THmin & STh/L=  0.600          3 Report
PLAT971_ALERT_2_C Check Calcd Residual Density  1.10A From     Pt1       2.36 eA-3
PLAT971_ALERT_2_C Check Calcd Residual Density  1.36A From     O2C       1.51 eA-3
PLAT975_ALERT_2_C Check Calcd Residual Density  0.84A From      N1       1.44 eA-3
PLAT975_ALERT_2_C Check Calcd Residual Density  1.05A From      N3       1.24 eA-3
PLAT975_ALERT_2_C Check Calcd Residual Density  1.05A From    O16T       0.83 eA-3
PLAT975_ALERT_2_C Check Calcd Residual Density  1.07A From     O8B       0.82 eA-3
PLAT975_ALERT_2_C Check Calcd Residual Density  0.76A From     O2W       0.68 eA-3
PLAT976_ALERT_2_C Check Calcd Residual Density  0.46A From      N3      -1.13 eA-3
PLAT976_ALERT_2_C Check Calcd Residual Density  0.44A From      N1      -1.09 eA-3

Alert level G
PLAT002_ALERT_2_G Number of Distance or Angle Restraints on AtSite         28 Note
PLAT005_ALERT_5_G No _iucr_refine_instructions_details  in the CIF     Please Do !
PLAT007_ALERT_5_G Number of Unrefined Donor-H Atoms ..............         19 Report
PLAT042_ALERT_1_G Calc. and Reported MoietyFormula Strings  Differ     Please Check
PLAT083_ALERT_2_G SHELXL Second Parameter in WGHT Unusually Large.      47.91 Why ?
PLAT128_ALERT_4_G Alternate Setting for Input Space Group     C2/c       I2/a Note
PLAT232_ALERT_2_G Hirshfeld Test Diff (M-X)  Mo6    --  O24T    ..        6.3 su
PLAT300_ALERT_4_G Atom Site Occupancy of *O4W    is Constrained at      0.500 Check
PLAT300_ALERT_4_G Atom Site Occupancy of *N12    is Constrained at      0.500 Check
PLAT300_ALERT_4_G Atom Site Occupancy of *C4     is Constrained at      0.500 Check
PLAT300_ALERT_4_G Atom Site Occupancy of *H4AW   is Constrained at      0.500 Check
PLAT300_ALERT_4_G Atom Site Occupancy of *H4BW   is Constrained at      0.500 Check
PLAT300_ALERT_4_G Atom Site Occupancy of *H12A   is Constrained at      0.500 Check
PLAT300_ALERT_4_G Atom Site Occupancy of *H12B   is Constrained at      0.500 Check
PLAT300_ALERT_4_G Atom Site Occupancy of *O4W_b  is Constrained at      0.500 Check
PLAT300_ALERT_4_G Atom Site Occupancy of *N12_b  is Constrained at      0.500 Check
PLAT300_ALERT_4_G Atom Site Occupancy of *C4_b   is Constrained at      0.500 Check
PLAT300_ALERT_4_G Atom Site Occupancy of *H4AW_b is Constrained at      0.500 Check
PLAT300_ALERT_4_G Atom Site Occupancy of *H4BW_b is Constrained at      0.500 Check
PLAT300_ALERT_4_G Atom Site Occupancy of *H12A_b is Constrained at      0.500 Check
PLAT300_ALERT_4_G Atom Site Occupancy of *H12B_b is Constrained at      0.500 Check
PLAT302_ALERT_4_G Anion/Solvent Disorder ............ Percentage =         15 Note
PLAT720_ALERT_4_G Number of Unusual/Non-Standard Labels ..........          8 Note
PLAT779_ALERT_4_G Suspect or Irrelevant (Bond) Angle in CIF .... #        145 Check
              O6C  -O6C  -H6      7.656   1.555   1.555              0.00 Deg.
PLAT779_ALERT_4_G Suspect or Irrelevant (Bond) Angle in CIF .... #        191 Check
              H12B -N12  -H4AW    1.555   1.555   1.555             20.00 Deg.
PLAT790_ALERT_4_G Centre of Gravity not Within Unit Cell: Resd.  #          3 Note
              C H6 N3
PLAT790_ALERT_4_G Centre of Gravity not Within Unit Cell: Resd.  #          8 Note
              H2 O
PLAT860_ALERT_3_G Number of Least-Squares Restraints .............         22 Note
PLAT912_ALERT_4_G Missing # of FCF Reflections Above STh/L=  0.600          3 Note

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

   1 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
   2 ALERT type 3 Indicator that the structure quality may be low
  28 ALERT type 4 Improvement, methodology, query or suggestion
   2 ALERT type 5 Informative message, check

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S1. Chemical context

The α (planar structure)-β (bent structure)-α geometrical isomerization, according to the stepwise protonation in the [PtMo₆O₂₄]^8- polyoxometalate (POM) species, viz. ([H_3.5α-PtMo₆O₂₄]^4.5- (Lee & Sasaki, 1994), [H₄β-PtMo₆O₂₄]^4- (Lee & Sasaki, 1994; Joo et al., 1994) and [H_4.5α-PtMo₆O₂₄]^3.5- (Lee & Sasaki, 1994; Lee et al., 2010) is an unprecedented phenomenon in the Anderson-structure heteropolyanion (Anderson, 1937), as well as in the chemistry of polyoxometalates.

As a result of the insolubility of the guanidinium salt, replaceable counter-cations in POMs can be exchanged by guanidinium ions. It is thus possible to obtain stable POMs by precipitation from aqueous solution with guanidinium salts. The guanidinium salts of platinum-containing POM species, viz. (CH₆N₃)₈[PtW₆O₂₄] (Lee et al., 2003), (CH₆N₃)₅[H₂PtV₉O₂₈] (Joo et al., 2011) and (CH₆N₃)₈[α-SiPt₂W₁₀O₄₀]·6H₂O (Lee et al., 2003) have been reported our group. The position of the protonated O atoms in the {[H_4.5α-PtMo₆O₂₄]₂}^7- polyanion were reconfirmed in the present study.

Sometimes a relatively short hydrogen bond, O···O distance < 2.60 Å, in which the H atom lies on a crystallographic center of symmetry, occurs in this class of structure. The H atom of the central hydrogen bond, O6C—H6—O6Cⁱ (Fig. 2) in the title compound lies on a crystallographic center of symmetry (space group C2/c : 3/4, 1/4, 1/2), and thus has half-occupancy in the asymmetric unit.

S2. Structural commentary

The structure of the title compound POM anion has been discussed in detail (Lee et al., 2010). Fig. 1 shows the structure of the title compound and selected geometrical parameters are given in Table 1. The complete polyanion has C₁ (1) symmetry. The O atoms of the cluster have been designated as OT (terminal Mo═O atom), OB (bridged µ₂-O atom), and OC (centered µ₃-O atom). The protonated O atoms in the polyanion were confirmed in electron density maps, inter­polyanion hydrogen bonds (Table 2) and by bond-valence sums (BVS; Brown & Altermatt, 1985; Brese & O'Keeffe, 1991). Fig. 2 shows a symmetric electron-density map around the position of atom H6. The heteropolyanions form inversion-generated dimers, {[H_4.5PtMo₆O₂₄]₂}^-7 held together by each of the four µ₃-O–H···µ₁-O (terminal O atom), two µ₂-O–H···µ₂-O and one centrosymmetric µ₃-O–H–µ₃-O hydrogen bonds (Table 2). The H atom's occupancy, which is 0.5 in the polyanion, is due to the centrosymmetry of this latter hydrogen bond (Figs. 2 and 3). The H atom of the centrosymmetric hydrogen bond in the compound lies on a crystallographic centre of symmetry (space group C2/c : 3/4, 1/4, 1/2). The O6C—H6 and O6C···O6Cⁱ distances are 1.266 and 2.532 (6) Å, and the O6C—H6—O6Cⁱ angle is 180° (Table 2 and Fig. 3). Atom H3 does not contribute to dimer formation because it is located on the other side of the polyanion.

Confirmation of the protonated O atoms was strongly supported by the BVS analysis. The calculated BVS for atoms O2C, O3C, O4C, O6C and O11B are 1.40, 1.36, 1.38, 1.41 and 1.30 valence units (v.u.), respectively, if the valence of the O—H bond is not included. Since the BVS value around the µ₂-O atom should be 2.0 v.u., the missing valences of O2C, O3C, O4C, O6C and O11B are 0.60, 0.64, 0.62, 0.59 and 0.70 v.u., respectively, which corresponds to the valence of the O–H bonds. The BVS value range for the unprotonated OC and OB atoms is 1.68–1.90 v.u. As a result, the protonated O atoms were O2C, O3C, O4C, O11B and O6C. The protonated features of both the {[H_4.5PtMo₆O₂₄]₂}^7- polyanion in the title compound and in K₇[H_4.5PtMo₆O₂₄]₂.11H₂O (space group P1) are exactly the same. The bond lengths and bond angles of protonated and unprotonated O atoms in the {[H_4.5PtMo₆O₂₄]₂}^7- polyanion are compared in Table 1. The Pt—OC bond lengths were not affected by protonation of the OC atoms.

The C4 guanidinium ion and O4W water molecule are equally disordered about a twofold rotation axis.

S3. Supra­molecular features

The heteropolyanions form inversion-generated dimers, {[H_4.5PtMo₆O₂₄]₂}^-7 held together by each of the four µ₃-O–H···µ₁-O (terminal O atom), two µ₂-O–H···µ₂-O and one centrosymmetric µ₃-O–H–µ₃-O hydrogen bonds (Table2 and Fig. 3). Furthermore, the polyanions are linked in three dimensions via N—H···O hydrogen bonds (Table 2). All water molecules form hydrogen bonds with O atoms of the polyanions except for the O2W water molecule (Table 2).

S4. Database survey

A number of Anderson-structure platinum(IV)-containing heteropolyoxomolybdates have been reported: [H_4.5PtMo₆O₂₄]^3.5- and [H₄PtMo₆O₂₄]^4-, [H_3.5PtMo₆O₂₄]^4.5- (Lee & Sasaki, 1994); [H₄β-PtM0₆0₂₄]^4- (Joo et al., 1994); [H₂PtMo₆O₂₄]^6- (Lee & Joo, 2000, 2004); [H_4.5PtMo₆O₂₄]^3.5- (Lee et al., 2010); [H₆PtMo₆O₂₄]^2- (Lee & Joo, 2010); [(PtMo₆O₂₄)₄H₂₃]^9-, [(PtMo₆O₂₄)₃H₁₆]^8- and [(PtMo₆O₂₄)₃H₁₄]^14- (Day et al., 2009).

S5. Synthesis and crystallization

A pale-yellow powder of the title compound was obtained by addition of a small excess of the stoichiometric qu­antity of guanidinium chloride, CH₆N₃Cl, to a solution of the sodium salt of hexamolybdoplatinate hydrate. Single crystals were obtained by recrystallization from a hot aqueous solution of the crude sample in an insulating chamber.

S6. Refinement

All the H atoms in the polyanion and all water H atoms were positioned using difference Fourier maps. All H atoms of the polyanion were refined with a distance restraint of O–H = 0.95 (3) Å using the DFIX command (Sheldrick, 2008). All H atoms of the guanidinium ions were positioned geometrically and refined using a riding model, with U_iso(H) = 1.5U_eq(N). The C4 guanidinium ion and O4W water molecule are equally disordered about a twofold rotation axis. Refinement of the site occupation factors (s.o.f) converged at values close to half occupancy. In the final refinement, the s.o.f.s were constrained to 0.5 and reasonable displacement parameters were obtained. The C—N and N—H bond lengths were restrained to 1.30 (2) and 0.90 (2) Å, respectively, and the H—N—H angles were restrained by restraining the H···H distance to 1.55 (2) Å in the disordered C4 guanidinium ion using the DFIX command. The H atoms of all water molecules (OW) were refined with a distance restraint of O—H = 0.95 (3) Å using the DFIX, and were included in the refinement with U_iso(H) = 1.5U_eq(O). The highest peak in the difference map is 0.98 Å from atom Pt1 and the largest hole is 0.36 Å from N3.

Related literature

For related literature, see: Anderson (1937); Brese & O'Keeffe (1991); Brown & Altermatt (1985); Day et al. (2009); Joo et al. (1994, 2011); Lee & Joo (2000, 2004, 2010); Lee & Sasaki (1994); Lee, Jang, Joo & Park (2003); Lee, Joo & Park (2010); Lee, Joo, Park & Ozeki (2003); Sheldrick (2008).

Computing details

Data collection: APEX2 (Bruker, 2009); cell refinement: SAINT (Bruker, 2009); data reduction: SAINT; program(s) used to solve structure: SHELXS97 (Sheldrick, 2008); program(s) used to refine structure: SHELXL97 (Sheldrick, 2008); molecular graphics: ORTEP-3 for Windows (Farrugia, 2012), PLATON (Spek, 2009) and DIAMOND (Brandenburg,1998); software used to prepare material for publication: SHELXL97.

Figures

	Fig. 1. The molecular structure of the title compound, showing the atom-numbering scheme. Displacement ellipsoids are drawn at the 50% probability level. H atoms are presented as small spheres of arbitrary radius. Disordered parts have been omitted for clarity.
	Fig. 2. Difference-Fourier map around atom H6 (calculated with atom H6 absent from the model).
	Fig. 3. Polyhedral view of the heteropolyanion in the title compound with O—H···O contacts of the interanion hydrogen bonds shown as red dashed lines. [Symmetry code: (i) -x + 3/2, -y + 1/2, -z + 1.]

Heptaguanidinium nonahydrogen bis[α-hexamolybdoplatinate(IV)] heptahydrate

Crystal data

(CH6N3)7H9[PtMo6O24]2·7H2O	F(000) = 5416
Mr = 2865.26	Dx = 2.917 Mg m^−3
Monoclinic, C2/c	Mo Kα radiation, λ = 0.71073 Å
Hall symbol: -C 2yc	Cell parameters from 9569 reflections
a = 31.413 (10) Å	θ = 2.2–28.2°
b = 10.073 (3) Å	µ = 6.62 mm^−1
c = 23.677 (7) Å	T = 173 K
β = 119.451 (14)°	Block, yellow
V = 6524 (3) Å^3	0.30 × 0.12 × 0.05 mm
Z = 4

Data collection

Bruker SMART APEXII CCD diffractometer	7107 independent reflections
Radiation source: Rotating Anode	6050 reflections with I > 2σ(I)
Graphite multilayer monochromator	Rint = 0.033
Detector resolution: 10.0 pixels mm^-1	θmax = 27.0°, θmin = 1.5°
ϕ and ω scans	h = −40→36
Absorption correction: multi-scan (SADABS; Sheldrick, 2008)	k = −12→12
Tmin = 0.241, Tmax = 0.729	l = −30→30
56606 measured reflections

Refinement

Refinement on F^2	Primary atom site location: structure-invariant direct methods
Least-squares matrix: full	Secondary atom site location: difference Fourier map
R[F^2 > 2σ(F^2)] = 0.028	Hydrogen site location: difference Fourier map
wR(F^2) = 0.073	H atoms treated by a mixture of independent and constrained refinement
S = 1.03	w = 1/[σ^2(Fo^2) + (0.0337P)^2 + 47.9084P] where P = (Fo^2 + 2Fc^2)/3
7107 reflections	(Δ/σ)max = 0.002
505 parameters	Δρmax = 2.50 e Å^−3
22 restraints	Δρmin = −1.30 e Å^−3

Special details

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. 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 > 2sigma(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.

Fractional atomic coordinates and isotropic or equivalent isotropic displacement parameters (Ų)

	x	y	z	Uiso*/Ueq	Occ. (<1)
Pt1	0.652431 (6)	0.176198 (17)	0.467608 (8)	0.01525 (6)
Mo1	0.743430 (14)	−0.00319 (4)	0.57409 (2)	0.02093 (10)
Mo2	0.682566 (15)	0.17866 (4)	0.624195 (19)	0.02035 (10)
Mo3	0.583929 (15)	0.34871 (4)	0.51759 (2)	0.02171 (10)
Mo4	0.552026 (14)	0.34729 (4)	0.359683 (19)	0.01849 (9)
Mo5	0.618484 (14)	0.17217 (4)	0.311229 (19)	0.01901 (10)
Mo6	0.712270 (14)	−0.01255 (4)	0.42001 (2)	0.02259 (10)
O1C	0.66821 (11)	0.0483 (3)	0.53959 (14)	0.0194 (7)
O2C	0.66214 (11)	0.3107 (3)	0.53597 (15)	0.0187 (7)
H2	0.6862 (17)	0.378 (5)	0.544 (3)	0.050 (18)*
O3C	0.58105 (11)	0.1962 (3)	0.44249 (15)	0.0178 (7)
H3	0.568 (2)	0.109 (3)	0.439 (3)	0.07 (2)*
O4C	0.63463 (11)	0.3099 (3)	0.39634 (15)	0.0184 (7)
H4	0.656 (3)	0.379 (6)	0.398 (4)	0.10 (3)*
O5C	0.64084 (11)	0.0488 (3)	0.39683 (14)	0.0191 (7)
O6C	0.72274 (11)	0.1511 (3)	0.49205 (15)	0.0190 (7)
H6	0.7500	0.2500	0.5000	0.06 (3)*
O7B	0.74507 (12)	0.1539 (3)	0.62431 (16)	0.0229 (7)
O8B	0.61194 (12)	0.2010 (3)	0.57683 (16)	0.0243 (7)
O9B	0.57705 (11)	0.4420 (3)	0.44128 (15)	0.0226 (7)
O10B	0.55913 (11)	0.1971 (3)	0.31241 (15)	0.0212 (7)
O11B	0.69300 (12)	0.1458 (3)	0.35603 (16)	0.0235 (7)
H11	0.713 (3)	0.222 (7)	0.362 (5)	0.15 (4)*
O12B	0.71759 (12)	−0.1040 (3)	0.49309 (17)	0.0262 (8)
O13T	0.80360 (12)	0.0093 (3)	0.59080 (17)	0.0285 (8)
O14T	0.74286 (12)	−0.1258 (3)	0.62346 (17)	0.0305 (8)
O15T	0.68520 (13)	0.0508 (4)	0.67282 (16)	0.0299 (8)
O16T	0.69977 (13)	0.3193 (3)	0.67096 (17)	0.0312 (8)
O17T	0.52417 (13)	0.3226 (4)	0.49587 (19)	0.0371 (9)
O18T	0.60285 (14)	0.4814 (4)	0.56903 (17)	0.0370 (9)
O19T	0.49288 (12)	0.3228 (3)	0.34110 (17)	0.0275 (8)
O20T	0.55233 (12)	0.4783 (3)	0.31420 (16)	0.0283 (8)
O21T	0.62270 (13)	0.3112 (4)	0.27214 (17)	0.0292 (8)
O22T	0.60336 (13)	0.0433 (4)	0.25787 (17)	0.0315 (8)
O23T	0.69102 (12)	−0.1349 (3)	0.36251 (18)	0.0304 (8)
O24T	0.77302 (12)	0.0093 (3)	0.44119 (17)	0.0290 (8)
C1	0.5886 (2)	−0.1669 (7)	0.5871 (3)	0.0536 (18)
N1	0.6167 (2)	−0.1725 (5)	0.5534 (3)	0.0611 (18)
H1A	0.6273	−0.2493	0.5476	0.073*
H1B	0.6230	−0.0991	0.5388	0.073*
N2	0.57817 (17)	−0.2673 (5)	0.6092 (2)	0.0446 (13)
H2A	0.5879	−0.3464	0.6046	0.053*
H2B	0.5611	−0.2586	0.6293	0.053*
N3	0.5678 (3)	−0.0394 (7)	0.5888 (4)	0.106 (3)
H3A	0.5480	−0.0333	0.6052	0.127*
H3B	0.5748	0.0317	0.5735	0.127*
C2	0.69992 (17)	0.6537 (5)	0.7035 (2)	0.0252 (11)
N4	0.7180 (2)	0.6254 (5)	0.6658 (3)	0.0482 (14)
H4A	0.7210	0.5420	0.6571	0.058*
H4B	0.7273	0.6896	0.6490	0.058*
N5	0.68617 (16)	0.5573 (4)	0.7284 (2)	0.0310 (10)
H5A	0.6892	0.4741	0.7196	0.037*
H5B	0.6739	0.5760	0.7538	0.037*
N6	0.69567 (17)	0.7785 (5)	0.7166 (2)	0.0355 (11)
H6A	0.7050	0.8426	0.6999	0.043*
H6B	0.6835	0.7976	0.7420	0.043*
C3	0.4036 (2)	0.6616 (5)	0.2726 (3)	0.0290 (11)
N7	0.43204 (15)	0.5625 (4)	0.3073 (2)	0.0324 (10)
H7A	0.4546	0.5757	0.3479	0.039*
H7B	0.4284	0.4834	0.2898	0.039*
N8	0.36976 (18)	0.6419 (5)	0.2123 (2)	0.0444 (13)
H8A	0.3507	0.7078	0.1894	0.053*
H8B	0.3661	0.5628	0.1947	0.053*
N9	0.4097 (3)	0.7778 (5)	0.2998 (3)	0.075 (2)
H9A	0.3910	0.8448	0.2775	0.090*
H9B	0.4326	0.7894	0.3403	0.090*
C4	0.5228 (3)	0.8412 (9)	0.2828 (4)	0.028 (2)	0.50
N10	0.5000	0.7313 (6)	0.2500	0.0368 (16)
H10A	0.4775 (14)	0.686 (4)	0.2159 (13)	0.044*
N11	0.5000	0.9567 (6)	0.2500	0.0471 (19)
H11A	0.5223 (16)	1.002 (4)	0.2844 (14)	0.057*
N12	0.5653 (4)	0.8331 (14)	0.3368 (6)	0.039 (3)	0.50
H12A	0.579 (3)	0.753 (5)	0.343 (6)	0.046*	0.50
H12B	0.584 (3)	0.905 (6)	0.355 (6)	0.046*	0.50
O1W	0.51593 (15)	0.6741 (4)	0.42228 (19)	0.0400 (10)
H1AW	0.5475 (12)	0.638 (6)	0.446 (3)	0.060*
H1BW	0.507 (2)	0.678 (6)	0.456 (2)	0.060*
O2W	0.52988 (18)	−0.0205 (5)	0.4254 (3)	0.0609 (13)
H2AW	0.508 (3)	−0.006 (8)	0.3811 (14)	0.091*
H2BW	0.553 (2)	−0.091 (6)	0.435 (4)	0.091*
O3W	0.6421 (2)	−0.3187 (6)	0.4650 (3)	0.0764 (17)
H3AW	0.6747 (13)	−0.346 (9)	0.487 (4)	0.115*
H3BW	0.632 (4)	−0.398 (6)	0.441 (4)	0.115*
O4W	0.5802 (4)	0.8321 (11)	0.3704 (5)	0.036 (2)	0.50
H4AW	0.599 (4)	0.911 (8)	0.381 (6)	0.055*	0.50
H4BW	0.602 (4)	0.770 (10)	0.402 (5)	0.055*	0.50

Atomic displacement parameters (Ų)

	U^11	U^22	U^33	U^12	U^13	U^23
Pt1	0.01074 (9)	0.01946 (10)	0.01597 (9)	−0.00051 (6)	0.00690 (7)	−0.00191 (7)
Mo1	0.01368 (19)	0.0186 (2)	0.0308 (2)	0.00080 (15)	0.01116 (17)	0.00340 (17)
Mo2	0.0199 (2)	0.0212 (2)	0.0193 (2)	−0.00066 (16)	0.00908 (17)	0.00091 (16)
Mo3	0.0190 (2)	0.0282 (2)	0.0213 (2)	0.00438 (17)	0.01255 (17)	−0.00020 (17)
Mo4	0.01413 (19)	0.0230 (2)	0.01809 (19)	0.00203 (15)	0.00773 (16)	0.00188 (16)
Mo5	0.0170 (2)	0.0242 (2)	0.01814 (19)	−0.00386 (16)	0.01039 (17)	−0.00427 (16)
Mo6	0.01442 (19)	0.0212 (2)	0.0358 (2)	−0.00414 (16)	0.01523 (18)	−0.01035 (18)
O1C	0.0188 (16)	0.0194 (17)	0.0189 (15)	0.0004 (13)	0.0083 (13)	−0.0001 (13)
O2C	0.0175 (16)	0.0200 (17)	0.0203 (16)	−0.0025 (13)	0.0107 (14)	−0.0044 (13)
O3C	0.0110 (15)	0.0224 (17)	0.0212 (16)	0.0003 (13)	0.0089 (13)	−0.0007 (13)
O4C	0.0157 (16)	0.0218 (17)	0.0194 (16)	−0.0030 (13)	0.0099 (13)	−0.0016 (13)
O5C	0.0160 (15)	0.0227 (17)	0.0195 (15)	−0.0018 (13)	0.0093 (13)	−0.0053 (13)
O6C	0.0086 (14)	0.0223 (17)	0.0225 (16)	0.0019 (12)	0.0049 (13)	−0.0056 (13)
O7B	0.0182 (16)	0.0249 (18)	0.0228 (17)	−0.0009 (14)	0.0077 (14)	0.0004 (14)
O8B	0.0213 (17)	0.0329 (19)	0.0235 (17)	−0.0006 (15)	0.0149 (15)	0.0021 (15)
O9B	0.0224 (17)	0.0214 (17)	0.0241 (16)	0.0033 (14)	0.0116 (14)	0.0006 (14)
O10B	0.0144 (15)	0.0283 (18)	0.0201 (16)	−0.0035 (13)	0.0079 (13)	−0.0024 (14)
O11B	0.0180 (16)	0.0287 (18)	0.0271 (17)	−0.0031 (14)	0.0135 (15)	−0.0036 (15)
O12B	0.0200 (17)	0.0226 (18)	0.041 (2)	−0.0029 (14)	0.0185 (16)	−0.0060 (15)
O13T	0.0204 (17)	0.0244 (18)	0.038 (2)	−0.0017 (14)	0.0124 (16)	0.0006 (15)
O14T	0.0245 (18)	0.0262 (19)	0.038 (2)	0.0018 (15)	0.0131 (16)	0.0075 (16)
O15T	0.0318 (19)	0.032 (2)	0.0264 (18)	0.0031 (16)	0.0144 (16)	0.0078 (16)
O16T	0.030 (2)	0.029 (2)	0.0307 (19)	0.0001 (15)	0.0115 (17)	−0.0062 (15)
O17T	0.0255 (19)	0.057 (3)	0.037 (2)	0.0066 (17)	0.0210 (18)	0.0066 (18)
O18T	0.048 (2)	0.036 (2)	0.0266 (19)	0.0097 (18)	0.0184 (18)	−0.0030 (17)
O19T	0.0159 (16)	0.033 (2)	0.0313 (19)	0.0022 (14)	0.0099 (15)	0.0011 (15)
O20T	0.0261 (18)	0.031 (2)	0.0254 (17)	0.0023 (15)	0.0112 (15)	0.0051 (15)
O21T	0.0292 (19)	0.038 (2)	0.0257 (18)	−0.0018 (16)	0.0173 (16)	0.0027 (15)
O22T	0.0311 (19)	0.038 (2)	0.0292 (18)	−0.0069 (17)	0.0176 (16)	−0.0152 (16)
O23T	0.0255 (18)	0.0244 (18)	0.044 (2)	−0.0039 (15)	0.0197 (17)	−0.0126 (17)
O24T	0.0257 (18)	0.0280 (19)	0.040 (2)	0.0018 (15)	0.0208 (17)	−0.0045 (16)
C1	0.035 (3)	0.063 (5)	0.052 (4)	−0.005 (3)	0.013 (3)	−0.013 (3)
N1	0.035 (3)	0.035 (3)	0.100 (5)	−0.006 (2)	0.024 (3)	0.000 (3)
N2	0.035 (3)	0.049 (3)	0.057 (3)	−0.003 (2)	0.029 (3)	0.012 (3)
N3	0.134 (7)	0.078 (5)	0.185 (9)	−0.068 (5)	0.140 (7)	−0.066 (5)
C2	0.019 (2)	0.030 (3)	0.021 (2)	−0.002 (2)	0.006 (2)	0.000 (2)
N4	0.075 (4)	0.040 (3)	0.063 (3)	−0.011 (3)	0.059 (3)	−0.005 (3)
N5	0.038 (3)	0.029 (2)	0.035 (2)	−0.002 (2)	0.026 (2)	−0.003 (2)
N6	0.038 (3)	0.032 (3)	0.038 (3)	0.000 (2)	0.021 (2)	0.003 (2)
C3	0.034 (3)	0.030 (3)	0.028 (3)	0.004 (2)	0.019 (2)	0.005 (2)
N7	0.031 (2)	0.032 (2)	0.026 (2)	0.003 (2)	0.0069 (19)	0.0025 (19)
N8	0.038 (3)	0.044 (3)	0.036 (3)	0.005 (2)	0.006 (2)	0.010 (2)
N9	0.154 (7)	0.029 (3)	0.045 (3)	0.016 (4)	0.050 (4)	0.004 (3)
C4	0.022 (5)	0.039 (6)	0.031 (6)	−0.007 (4)	0.019 (5)	−0.002 (5)
N10	0.033 (4)	0.022 (3)	0.045 (4)	0.000	0.012 (3)	0.000
N11	0.042 (4)	0.019 (3)	0.083 (6)	0.000	0.033 (4)	0.000
N12	0.035 (8)	0.030 (6)	0.043 (7)	0.007 (5)	0.013 (6)	0.011 (7)
O1W	0.039 (2)	0.055 (3)	0.031 (2)	0.0063 (19)	0.0207 (19)	0.0038 (18)
O2W	0.051 (3)	0.037 (3)	0.091 (4)	0.000 (2)	0.032 (3)	0.006 (3)
O3W	0.069 (4)	0.072 (4)	0.097 (5)	0.027 (3)	0.048 (4)	0.009 (3)
O4W	0.025 (6)	0.034 (6)	0.050 (7)	−0.010 (4)	0.018 (5)	0.001 (6)

Geometric parameters (Å, º)

Pt1—O1C	1.995 (3)	O6C—O6C^i	2.532 (6)
Pt1—O2C	2.015 (3)	O6C—H6	1.266 (3)
Pt1—O3C	2.027 (3)	O11B—H11	0.95 (2)
Pt1—O4C	2.011 (3)	C1—N2	1.254 (8)
Pt1—O5C	1.997 (3)	C1—N1	1.451 (10)
Pt1—O6C	2.005 (3)	C1—N3	1.451 (10)
Mo1—O1C	2.150 (3)	N1—H1A	0.8800
Mo1—O6C	2.317 (3)	N1—H1B	0.8800
Mo2—O1C	2.248 (3)	N2—H2A	0.8800
Mo2—O2C	2.286 (3)	N2—H2B	0.8800
Mo3—O2C	2.307 (3)	N3—H3A	0.8800
Mo3—O3C	2.318 (3)	N3—H3B	0.8800
Mo4—O3C	2.287 (3)	C2—N4	1.304 (7)
Mo4—O4C	2.327 (3)	C2—N5	1.314 (6)
Mo5—O4C	2.289 (3)	C2—N6	1.317 (7)
Mo5—O5C	2.178 (3)	N4—H4A	0.8800
Mo6—O5C	2.123 (3)	N4—H4B	0.8800
Mo6—O6C	2.277 (3)	N5—H5A	0.8800
Mo1—O7B	1.965 (3)	N5—H5B	0.8800
Mo1—O12B	1.959 (3)	N6—H6A	0.8800
Mo2—O7B	1.978 (3)	N6—H6B	0.8800
Mo2—O8B	1.945 (3)	C3—N9	1.303 (7)
Mo3—O8B	1.934 (3)	C3—N8	1.310 (7)
Mo3—O9B	1.952 (3)	C3—N7	1.322 (6)
Mo4—O9B	1.941 (3)	N7—H7A	0.8800
Mo4—O10B	1.959 (3)	N7—H7B	0.8800
Mo5—O10B	1.895 (3)	N8—H8A	0.8800
Mo5—O11B	2.058 (3)	N8—H8B	0.8800
Mo6—O11B	2.075 (4)	N9—H9A	0.8800
Mo6—O12B	1.894 (4)	N9—H9B	0.8800
Mo1—O14T	1.706 (3)	C4—N12	1.320 (12)
Mo1—O13T	1.735 (3)	C4—N10	1.340 (10)
Mo2—O15T	1.702 (3)	C4—N11	1.387 (10)
Mo2—O16T	1.713 (3)	N10—H10A	0.893 (17)
Mo3—O17T	1.705 (4)	N11—H11A	0.898 (18)
Mo3—O18T	1.706 (4)	N12—H12A	0.90 (2)
Mo4—O19T	1.704 (3)	N12—H12B	0.90 (2)
Mo4—O20T	1.706 (3)	O1W—H1AW	0.94 (2)
Mo5—O22T	1.708 (3)	O1W—H1BW	0.95 (2)
Mo5—O21T	1.719 (3)	O2W—H2AW	0.94 (2)
Mo6—O23T	1.710 (3)	O2W—H2BW	0.95 (2)
Mo6—O24T	1.732 (3)	O3W—H3AW	0.93 (2)
O2C—H2	0.96 (2)	O3W—H3BW	0.94 (2)
O3C—H3	0.96 (2)	O4W—H4AW	0.95 (2)
O4C—H4	0.95 (2)	O4W—H4BW	0.95 (2)
Mo1—O1C—Mo2	95.79 (12)	O21T—Mo5—O4C	86.44 (14)
Mo2—O2C—Mo3	93.64 (11)	O10B—Mo5—O4C	72.56 (12)
Mo4—O3C—Mo3	93.75 (12)	O11B—Mo5—O4C	85.46 (12)
Mo5—O4C—Mo4	92.64 (11)	O5C—Mo5—O4C	72.30 (12)
Mo6—O5C—Mo5	102.87 (13)	O23T—Mo6—O24T	105.40 (16)
Mo6—O6C—Mo1	91.14 (12)	O23T—Mo6—O12B	101.61 (17)
Mo1—O7B—Mo2	111.71 (15)	O24T—Mo6—O12B	101.99 (16)
Mo3—O8B—Mo2	119.36 (16)	O23T—Mo6—O11B	96.50 (16)
Mo4—O9B—Mo3	119.39 (17)	O24T—Mo6—O11B	89.87 (15)
Mo5—O10B—Mo4	120.02 (16)	O12B—Mo6—O11B	154.72 (14)
Mo5—O11B—Mo6	108.97 (15)	O23T—Mo6—O5C	93.14 (14)
Mo6—O12B—Mo1	116.75 (17)	O24T—Mo6—O5C	155.73 (14)
O1C—Pt1—O5C	99.68 (14)	O12B—Mo6—O5C	89.14 (13)
O1C—Pt1—O6C	84.05 (13)	O11B—Mo6—O5C	72.28 (12)
O5C—Pt1—O6C	83.21 (12)	O23T—Mo6—O6C	166.99 (14)
O1C—Pt1—O4C	177.35 (12)	O24T—Mo6—O6C	87.60 (14)
O5C—Pt1—O4C	82.27 (13)	O12B—Mo6—O6C	75.67 (13)
O6C—Pt1—O4C	97.99 (13)	O11B—Mo6—O6C	82.71 (13)
O1C—Pt1—O2C	82.64 (13)	O5C—Mo6—O6C	74.21 (11)
O5C—Pt1—O2C	177.41 (13)	Pt1—O1C—Mo1	104.21 (13)
O6C—Pt1—O2C	98.20 (13)	Pt1—O1C—Mo2	103.95 (14)
O4C—Pt1—O2C	95.37 (13)	Pt1—O2C—Mo2	101.92 (13)
O1C—Pt1—O3C	95.12 (13)	Pt1—O2C—Mo3	103.51 (13)
O5C—Pt1—O3C	95.66 (12)	Pt1—O2C—H2	116 (4)
O6C—Pt1—O3C	178.46 (12)	Mo2—O2C—H2	113 (4)
O4C—Pt1—O3C	82.87 (13)	Mo3—O2C—H2	125 (4)
O2C—Pt1—O3C	82.96 (13)	Pt1—O3C—Mo4	103.59 (13)
O14T—Mo1—O13T	105.87 (16)	Pt1—O3C—Mo3	102.74 (13)
O14T—Mo1—O12B	99.01 (16)	Pt1—O3C—H3	108 (4)
O13T—Mo1—O12B	98.14 (15)	Mo4—O3C—H3	124 (4)
O14T—Mo1—O7B	100.03 (16)	Mo3—O3C—H3	122 (4)
O13T—Mo1—O7B	95.86 (15)	Pt1—O4C—Mo5	100.53 (13)
O12B—Mo1—O7B	152.25 (14)	Pt1—O4C—Mo4	102.74 (13)
O14T—Mo1—O1C	93.17 (14)	Pt1—O4C—H4	124 (5)
O13T—Mo1—O1C	160.02 (14)	Mo5—O4C—H4	109 (5)
O12B—Mo1—O1C	84.50 (12)	Mo4—O4C—H4	122 (5)
O7B—Mo1—O1C	74.48 (12)	Pt1—O5C—Mo6	103.69 (13)
O14T—Mo1—O6C	165.12 (14)	Pt1—O5C—Mo5	104.87 (14)
O13T—Mo1—O6C	88.14 (14)	Pt1—O6C—Mo6	98.17 (12)
O12B—Mo1—O6C	73.55 (13)	Pt1—O6C—Mo1	98.14 (13)
O7B—Mo1—O6C	83.11 (12)	Pt1—O6C—O6C^i	120.8 (2)
O1C—Mo1—O6C	73.54 (11)	Mo6—O6C—O6C^i	121.27 (19)
O15T—Mo2—O16T	107.06 (18)	Mo1—O6C—O6C^i	120.85 (19)
O15T—Mo2—O8B	98.04 (15)	Pt1—O6C—H6	120.8 (2)
O16T—Mo2—O8B	100.65 (16)	Mo6—O6C—H6	121.27 (19)
O15T—Mo2—O7B	100.70 (15)	Mo1—O6C—H6	120.85 (19)
O16T—Mo2—O7B	96.07 (16)	O6C^i—O6C—H6	0.00 (18)
O8B—Mo2—O7B	149.93 (14)	Mo5—O11B—H11	118 (7)
O15T—Mo2—O1C	94.74 (15)	Mo6—O11B—H11	125 (7)
O16T—Mo2—O1C	156.95 (15)	N2—C1—N1	123.5 (6)
O8B—Mo2—O1C	83.19 (13)	N2—C1—N3	119.2 (7)
O7B—Mo2—O1C	72.05 (12)	N1—C1—N3	117.0 (6)
O15T—Mo2—O2C	163.07 (14)	C1—N1—H1A	120.0
O16T—Mo2—O2C	88.12 (15)	C1—N1—H1B	120.0
O8B—Mo2—O2C	71.19 (12)	H1A—N1—H1B	120.0
O7B—Mo2—O2C	84.67 (12)	C1—N2—H2A	120.0
O1C—Mo2—O2C	71.47 (12)	C1—N2—H2B	120.0
O17T—Mo3—O18T	106.36 (19)	H2A—N2—H2B	120.0
O17T—Mo3—O8B	98.10 (16)	C1—N3—H3A	120.0
O18T—Mo3—O8B	102.14 (16)	C1—N3—H3B	120.0
O17T—Mo3—O9B	100.99 (16)	H3A—N3—H3B	120.0
O18T—Mo3—O9B	97.16 (16)	N4—C2—N5	119.7 (5)
O8B—Mo3—O9B	147.71 (13)	N4—C2—N6	120.0 (5)
O17T—Mo3—O2C	160.66 (16)	N5—C2—N6	120.3 (5)
O18T—Mo3—O2C	91.76 (16)	C2—N4—H4A	120.0
O8B—Mo3—O2C	70.90 (12)	C2—N4—H4B	120.0
O9B—Mo3—O2C	82.96 (12)	H4A—N4—H4B	120.0
O17T—Mo3—O3C	92.54 (15)	C2—N5—H5A	120.0
O18T—Mo3—O3C	159.28 (16)	C2—N5—H5B	120.0
O8B—Mo3—O3C	83.03 (13)	H5A—N5—H5B	120.0
O9B—Mo3—O3C	70.38 (13)	C2—N6—H6A	120.0
O2C—Mo3—O3C	70.78 (11)	C2—N6—H6B	120.0
O19T—Mo4—O20T	107.04 (16)	H6A—N6—H6B	120.0
O19T—Mo4—O9B	100.65 (15)	N9—C3—N8	121.1 (5)
O20T—Mo4—O9B	97.05 (15)	N9—C3—N7	118.8 (5)
O19T—Mo4—O10B	99.01 (15)	N8—C3—N7	120.1 (5)
O20T—Mo4—O10B	101.47 (15)	C3—N7—H7A	120.0
O9B—Mo4—O10B	147.60 (13)	C3—N7—H7B	120.0
O19T—Mo4—O3C	92.83 (14)	H7A—N7—H7B	120.0
O20T—Mo4—O3C	158.72 (14)	C3—N8—H8A	120.0
O9B—Mo4—O3C	71.24 (13)	C3—N8—H8B	120.0
O10B—Mo4—O3C	82.34 (13)	H8A—N8—H8B	120.0
O19T—Mo4—O4C	161.33 (14)	C3—N9—H9A	120.0
O20T—Mo4—O4C	90.53 (14)	C3—N9—H9B	120.0
O9B—Mo4—O4C	82.92 (12)	H9A—N9—H9B	120.0
O10B—Mo4—O4C	70.65 (12)	N12—C4—N10	120.6 (9)
O3C—Mo4—O4C	70.80 (11)	N12—C4—N11	126.3 (9)
O22T—Mo5—O21T	106.73 (18)	N10—C4—N11	112.7 (7)
O22T—Mo5—O10B	101.18 (15)	C4—N10—H10A	155 (2)
O21T—Mo5—O10B	103.69 (15)	C4—N12—H12A	113 (7)
O22T—Mo5—O11B	96.63 (15)	C4—N12—H12B	122 (8)
O21T—Mo5—O11B	90.77 (15)	H12A—N12—H4AW	106 (10)
O10B—Mo5—O11B	152.59 (14)	H12B—N12—H4AW	20 (10)
O22T—Mo5—O5C	95.73 (15)	H1AW—O1W—H1BW	100 (6)
O21T—Mo5—O5C	152.95 (14)	H2AW—O2W—H2BW	116 (8)
O10B—Mo5—O5C	86.07 (13)	H3AW—O3W—H3BW	92 (8)
O11B—Mo5—O5C	71.47 (12)	H4AW—O4W—H4BW	103 (10)
O22T—Mo5—O4C	166.58 (15)

Symmetry code: (i) −x+3/2, −y+1/2, −z+1.

Hydrogen-bond geometry (Å, º)

D—H···A	D—H	H···A	D···A	D—H···A
O2C—H2···O24T^i	0.96 (2)	1.61 (2)	2.578 (5)	179 (6)
O3C—H3···O2W	0.96 (2)	1.69 (3)	2.622 (6)	164 (7)
O4C—H4···O13T^i	0.95 (2)	1.63 (2)	2.568 (5)	173 (9)
O6C—H6···O6C^i	1.27	1.27	2.532 (6)	180
O11B—H11···O7B^i	0.95 (2)	1.74 (2)	2.679 (5)	173 (10)
N1—H1B···O1C	0.88	2.05	2.864 (6)	154
N1—H1A···O3W	0.88	2.33	2.973 (9)	130
N2—H2A···O18T^ii	0.88	2.08	2.940 (7)	165
N2—H2B···O19T^iii	0.88	2.22	3.043 (6)	155
N3—H3B···O8B	0.88	2.04	2.874 (7)	157
N3—H3A···O2W^iii	0.88	2.25	2.979 (9)	140
N4—H4B···O14T^iv	0.88	2.09	2.944 (6)	164
N4—H4A···O24T^i	0.88	2.48	3.006 (6)	119
N5—H5A···O16T	0.88	2.06	2.890 (6)	157
N5—H5B···O21T^v	0.88	2.18	2.973 (5)	149
N6—H6A···O15T^iv	0.88	2.19	2.894 (6)	136
N6—H6B···O21T^v	0.88	2.59	3.281 (6)	136
N7—H7B···O19T	0.88	2.40	2.936 (5)	119
N7—H7A···O1W	0.88	2.11	2.927 (6)	154
N8—H8B···O13T^vi	0.88	2.39	3.006 (6)	128
N8—H8A···O23T^vii	0.88	2.04	2.918 (6)	178
N9—H9A···O22T^vii	0.88	2.21	2.938 (7)	140
O1W—H1AW···O9B	0.94 (2)	2.20 (5)	2.916 (5)	132 (5)
O1W—H1BW···O17T^viii	0.95 (2)	1.85 (3)	2.783 (5)	166 (6)
O2W—H2BW···O4W^ii	0.95 (2)	2.24 (7)	2.902 (12)	126 (6)
O3W—H3BW···O9B^ii	0.94 (2)	2.35 (8)	3.029 (7)	128 (8)

Symmetry codes: (i) −x+3/2, −y+1/2, −z+1; (ii) x, y−1, z; (iii) −x+1, −y, −z+1; (iv) x, y+1, z; (v) x, −y+1, z+1/2; (vi) x−1/2, −y+1/2, z−1/2; (vii) −x+1, y+1, −z+1/2; (viii) −x+1, −y+1, −z+1.