research communications
Double salt α-hexamolybdoplatinate(IV) heminonahydrogen α-hexamolybdoplatinate(IV) nonacosahydrate: dihydrogen disordered-mixture double salt
of hexasodium hemiundecahydrogenaDepartment of Chemistry, Pukyong National University, 599-1 Daeyeon 3-dong, Nam-gu, Busan 608-737, Republic of Korea, and bResearch Institute of Natural Science, Gyeongsang National University, 501, Jinju-daero, Jinju, 660-701, Republic of Korea
*Correspondence e-mail: uklee@pknu.ac.kr
The title double salt containing two distinct, differently protonated hexamolybdoplatinate(IV) polyanions, Na6[H5.5α-PtMo6O24][H4.5α-PtMo6O24]·29H2O, has been synthesized by a hydrothermal reaction at ca pH 1.80. The positions of the H atoms in the polyanions were established from difference Fourier maps and confirmed by the interpolyanion hydrogen bonds, bond-distance elongation, and bond-valence sum (BVS) calculations. The fractional numbers of H atoms in each polyanion are required for charge balance and in order to avoid unrealistically short H⋯H distances in the interpolyanion hydrogen bonds. Considering the disorder, the refined formula of the title polyanion, {[H5.5α-PtMo6O24]; polyanion (A) and [H4.5α-PtMo6O24]; polyanion (B)}6−, can be rewritten as a set of real formula, viz. {[H6α-PtMo6O24]; polyanion (A). [H4α-PtMo6O24]; polyanion (B)}6− and {[H5α-PtMo6O24]; polyanion (A). [H5α-PtMo6O24]; polyanion (B)}6−. The polyanion pairs both form dimers of the same formula, viz. {[H10α-Pt2Mo12O48]}6− connected by seven interpolyanion O—H⋯O hydrogen bonds.
Keywords: crystal structure; platinium containing polyoxomolybdate; double salt-type heteropolyoxometalate; hexamolybdoplatinate(IV); multihydrogen bond.
CCDC reference: 1426214
1. Chemical context
The α (planar structure) – β (bent structure) – α geometrical isomerization, according to stepwise protonation in the [PtMo6O24]8− polyoxometalate (POM) species, viz. ([H3.5α-PtMo6O24]4.5− (Lee & Sasaki, 1994; Lee, 1988) , [H4β-PtMo6O24]4− (Lee & Sasaki, 1994; Joo et al., 1994) and [H4.5α-PtMo6O24]3.5− (Lee & Sasaki, 1994; Lee et al., 2010; Joo et al., 2015a) is an unprecedented phenomenon in the Anderson-type heteropolyanion (Anderson, 1937) and as well as in the chemistry of POMs. In addition, differently protonated polyanion species have been reported, viz. [H2α-PtMo6O24]6− (Lee & Joo, 2000; Lee & Joo, 2004), and [H6α-PtMo6O24]2− (Lee & Joo, 2006a; Lee & Joo, 2006b; Lee & Joo, 2010). These polyanions form dimers by effective interpolyanion hydrogen bonds. Recently, a hydrogen-bonded hexamolybdoplatinate(IV) tetramer, [(α-PtMo6O24)4H23]9−, and the trimers, [(α-PtMo6O24)3H16]8− and [(α-PtMo6O24)3H14]10− were reported as tetra-n-butylammonium, and tetra-n-butylammonium/triethylammonium salts, respectively (Day et al., 2009).
In our studies of Anderson-type heteropolyoxotungstates containing PtIV, [Hnα-PtIVW6O24](8–n)– n = 0, 2, 2.5, 3, 3.5), we have found out that the gradual protonation is also a typical character of these compounds (Izarova et al., 2012). Furthermore, we have reported the stepwise protonation species in the nonavanadoplatinate(IV) series, viz. [HnPtV9O28](7−n)− (n = 2 and 3) (Lee et al., 2008; Joo et al., 2011; Joo & Lee, 2015; Joo et al., 2015b). As well as the PtIV a Keggin-type (Keggin, 1934) heteropolyoxometalate was formed, [α-SiPtIV2W10O40]8− (Lee et al., 2003).
The PtIV ion shows a very rich chemical behavior when it forms POMs with Mo, W and V systems. We assume that the diversity of the PtIV-containing POMs is caused by the starting material of the heteroatom, [PtIV(OH)6]2−, and the similarities in the oxidation states and the ionic radii of addenda atoms (Pt4+; 0.76, Mo6+; 0.73, W6+; 0.74 & V5+; 0.68 Å; Shannon, 1976) and the of Pt4+ (5d6) that preferentially forms the six-coordinated octahedra. In particular, the selective protonation of the μ3-O atoms around Pt atom in the POMs is an important factor to the formation of POMs because the geometries of M—μ3-O (bond distance) and M—μ3-O—M (bond angle) (M = Mo, W and V) are changeable by the partial protonation of the μ3-O and μ2-O atoms.
2. Structural commentary
The title compound contains two statistically different protonated hexamolybdoplatinate(IV) polyanions, [H5.5α-PtIVMo5O24]2.5− (A), and [H4.5α-PtIVMo5O24]3.5− (B). Figs. 1 and 2 show the structures of the title compound and polyanions, respectively. The O atoms of the clusters were designated as OT (terminal Mo=O atom), OB (bridging μ2-OB atom; Mo—O—Mo), and OC (centered μ3-O atom; Mo2—OC—Pt).
The H atoms of the protonated O atoms were found in difference Fourier maps and confirmed by bond-length elongation of Mo—O, and change of angles of Mo—OB—Mo and Mo—OC—Mo (Table 1), the interpolyanion hydrogen bonds (Table 2 and Fig. 4), and the bond-valence sums (BVSs; Brown & Altermatt, 1985; Brese & O'Keeffe, 1991). The protonated O atoms in the hexamolybdoplatinates(IV), polyanion (A) and (B), are five (Pt and Mo2)-bound μ3-O (O2C—O6C) and one Mo2-bound μ2-O (O7B) [for polyanion (A)], and four (Pt and Mo2)-bound μ3-O (O26C—O28C and O30C) and one Mo2-bound μ2-O (O31B) [for polyanion (B)] atoms. One (Pt and Mo2)-bound μ3-O atom in each polanion [O2C for polyanion (A) and O30C for polyanion (B)] is half-number protonated by disorder (Fig. 2). The residues of the two disordered H atoms, H2 and H30, were confirmed in the difference Fourier map (Fig. 3). This disorder is necessary for charge-balance of the polyanions and in order to avoid unreasonably short H⋯H distances in the interpolyanion hydrogen bonds.
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Two discrete heteropolyanions, (A) and (B), form a dimer, {[H10α-Pt2Mo12O48]6−, held together by two strong pairs of (Pt and Mo2)-bound μ3-OC—H⋯(Mo)-bound μ1-OT, normally a pair of (Mo2)-bound μ2-OB—H⋯(Mo2)-bound μ2-OB, and a single disordered strong (Pt and Mo2)-bound μ3-OC—H⋯(Pt and Mo2)-bound μ3-OC hydrogen bonds (Fig. 4 and Table 2). Considering the disorder, the statistically refined formula of the title polyanion, {[H5.5α-PtMo6O24]·[H4.5α-PtMo6O24]}6−, can be rewritten as mixture of dimers of {[H6α-PtMo6O24]; polyanion (A)}·[H4α-PtMo6O24]; polyanion (B)}6− and {[H5α-PtMo6O24]; polyanion (A)}·[H5α-PtMo6O24]; polyanion (B)}6− (Fig. 5). In other words, a set of polyanion (A), [H5.5α-PtMo6O24]2.5−, and polyanion (B), [H4.5α-PtMo6O24]3.5−, are the average disordered formulae of {[H6α-PtMo6O24]2·[H4α-PtMo6O24]4−} and {[H5α-PtMo6O24]3−·[H5α-PtMo6O24]3−} (Fig. 5).
The previously reported [β-H4PtMo6O24]4− polyanion (Lee & Sasaki, 1994; Joo et al., 1994) showed a bent structure (C2v) but the present polyanion shows a near planar structure. The protonated O atoms of [H6PtMo6O24]2− in the present structure show the same protonation scheme as one previously reported (Lee & Joo, 2006a,b), viz. four μ3-OC and two μ2-OB atoms are protonated. However, the protonation scheme of the previously reported polyanion in [H6PtMo6O24]2− (Lee & Joo, 2010) was different, consisting of five μ3-OC and one μ2-OB protonated O atoms. Five protonated polyanion species (A) and (B) were confirmed for the first time in the title compound. Four μ3-O and one μ2-O atoms are protonated in both polyanions, but the position of the unprotonated μ3-O atom differs (Fig. 2).
Confirmation of the protonated O atoms was strongly supported by the BVS analysis. The BVSs for protonated atoms O2C–O6C and O7B in polyanion (A) are 1.58, 1.45, 1.43, 1.36, 1.42 and 1.24, and O26C–O28C, O30C and O31B in the polyanion (B) are 1.41, 1.41, 1.39, 1.33 and 1.24 valence units (v.u.), respectively, if the valence of the O—H bond is not included. As the BVS value around the O atoms in the polyanion should be 2.0 v.u., the missing valences for each of the O atoms are 0.42 (for O2C), 0.55 (for O3C), 0.57 (for O4C), 0.64 (for O5C), 0.58 (for O6C) and 0.76 (for O7B) v.u. in polyanion (A), and 0.59 (for O26C), 0.59 (for O27C), 0.61 (for O28C), 0.67 (for O30C) and 0.76 (for O31B) in polyanion (B), respectively, corresponding to the valence of the O—H bonds. The BVSs around the other unprotonated atoms, O1C and O8B–O12B in the polyanion (A) and O25C, O29C and O32B–O36B in polyanion (B) are 1.82, 1.93, 1.84, 1.85, 1.90 and 1.90, and 1.82, 1.80, 1.94, 1.80, 1.81, 1.70 and 1.94 v.u., respectively, if the valence of the OB and the C⋯H—OW hydrogen bonds and (OB and C)⋯Na+ interactions are not included.
All Na+ cations are located on general positions of the P. The calculated BVSs for the Na1–Na6 ions are 1.22, 1.19, 1.32, 1.10, 1.21 and 1.18 v.u., respectively (Na+⋯O distance 〈 2.50 Å; total v.u = 7.22). The Na+ ions are variously coordinated by O atoms as [Na1(OT)2(OW)4]+, [Na2(OT)(OW)5]+, [Na3(OT)2(OW)4]+, [Na4(OT)(OW)4]+, [Na5(OT)2(OW)4]+ and [Na6(OT)2(OW)4]+.
3. Supramolecular features
The dimerized polyanions (A) + (B), {[H10α-Pt2Mo12O48]6−, are connected three-dimensionally by O atoms of the polyanion coordinated to Na+ ions. Two discrete heteropolyanions, (A) and (B), form a dimer, {[H10α-Pt2Mo12O48]6−, held together by two strong pairs of (Pt and Mo2)-bound μ3-OC—H⋯(Mo)-bound μ1-OT, normally a pair of (Mo2)-bound μ2-OB—H⋯(Mo2)-bound μ2-OB, and a single disordered strong (Pt and Mo2)-bound μ3O-C—H0.5⋯(Pt & Mo2)-bound μ3-OC hydrogen bond (Fig. 4 and Table 2). It is notable that the water molecules O21W–O29W, do not show any interaction with the metal atoms and are bonded to other O atoms only by O—H⋯O hydrogen bonds. The other H atoms of the polyanion (H3, H5 and H27) form hydrogen bonds with water molecules (Table 2).
4. Synthesis and crystallization
Crystals of title compound were prepared by the reaction of Na2MoO4·2H2O and Na2Pt(OH)6 at ca pH 1.80 as described in a previous report (Lee & Sasaki, 1994).
5. Refinement
The crystal data, the data collection and the structure . Atoms O5C and O30C, and O2C and O25C sets required an ISOR restraint in SHELXL2014/7 (Sheldrick, 2015) with reduced deviation s = 0.004 and st = 0.008, and s = 0.002 and st = 0.004, respectively. All H atoms of polyanions were located in difference Fourier maps, and were refined with a distance restraint of O—H = 0.85 (3) Å using the command DFIX in SHELXL2014/7, and included in the with Uiso(H) = 1.5Ueq(O). The occupancies of atoms H2 and H30 were reduced to 0.5 because of disorder. All H atoms of the water molecules, except O12W–O15W, were located in difference Fourier maps, and were refined using a distance restraint of O—H = 0.85 (3) Å and an angle restraint of HA—HB = 1.40 (3) Å using the command DFIX in SHELXL2014/7, and included in the with Uiso(H) = 1.5Ueq(O). An angle restraint of 1.35 (3) Å for O5W, O18W and O19W, and 1.30 (3) Å for O7W was applied. The H atoms of O12W–O13W were positioned geometrically and refined using a riding model (HFIX 137), with OW—H = 0.98 Å and Uiso(H) = 1.5Ueq(O). The H atoms of O14W were refined using a riding model (HFIX 23), with OW—H = 0.99 Å and Uiso(H) = 1.5Ueq(O). All invalid H atoms were removed in the final step of The highest peak in the difference map is 0.82 Å from Pt1 and the deepest hole is 0.98 Å from Pt2.
details are summarized in Table 3
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Supporting information
CCDC reference: 1426214
10.1107/S2056989015017703/hb7461sup1.cif
contains datablocks New_Global_Publ_Block, I. DOI:Structure factors: contains datablock I. DOI: 10.1107/S2056989015017703/hb7461Isup2.hkl
The α (planar structure) –β (bent structure) –α geometrical isomerization, according to stepwise protonation in the [PtMo6O24]8- polyoxometalate (POM) species, viz. ([H3.5α-PtMo6O24]4.5- (Lee & Sasaki, 1994; Lee, 1988 ), [H4β-PtMo6O24]4- (Lee & Sasaki, 1994; Joo et al., 1994) and [H4.5α-PtMo6O24]3.5- (Lee & Sasaki, 1994; Lee et al., 2010; Joo et al., 2015a) is an unprecedented phenomenon in the Anderson-type heteropolyanion (Anderson, 1937) and as well as in the chemistry of POMs. In addition, differently protonated polyanion species have been reported, viz. [H2α-PtMo6O24]6- (Lee & Joo, 2000; Lee & Joo, 2004), and [H6α-PtMo6O24]2- (Lee & Joo, 2006a; Lee & Joo, 2006b; Lee & Joo, 2010). These polyanions form dimers by effective interpolyanion hydrogen bonds. Recently, a hydrogen-bonded hexamolybdoplatinate(IV) tetramer, [(α-PtMo6O24)4H23]9-, and the trimers, [(α-PtMo6O24)3H16]8- and [(α-PtMo6O24)3H14]10- were reported as tetra-n-butylammonium, and tetra-n-butylammonium/triethylammonium salts, respectively (Day et al., 2009).
In our studies of Anderson-type heteropolyoxotungstates containing PtIV, [Hnα-PtIVW6O24](8-n)- n = 0, 2, 2.5, 3, 3.5), we have found out that the gradual protonation is also a typical character of these compounds (Izarova et al., 2012). Furthermore, we have reported the stepwise protonation species in the nonavanadoplatinate(IV), viz. [HnPtV9O28](7-n)- (n = 2 and 3) (Lee et al., 2008; Joo et al., 2011; Joo & Lee, 2015; Joo et al., 2015b). As well as the PtIV a Keggin-type (Keggin, 1934) heteropolyoxometalate was formed, [α-SiPtIV2W10O40]8- (Lee et al., 2003).
The PtIV ion shows a very rich chemical behavior when it forms POMs with Mo, W and V systems. We assume that the diversity of the PtIV-containing POMs is caused by the starting material of the heteroatom, [PtIV(OH)6]2-, and the similarities in the oxidation states and the ionic radii of addenda atoms (Pt4+; 0.76, Mo6+; 0.73, W6+; 0.74 & V5+; 0.68 Å; Shannon, 1976) and the
of Pt4+ (5d6) that preferentially forms the six-coordinated octahedra. In particular, the selective protonation of the µ3-O atoms around Pt atom in the POMs is an important factor to the formation of POMs because the geometries of M—µ3-O (bond distance) and M—µ3-O—M (bond angle) (M = Mo, W and V) are changeable by the partial protonation of the µ3-O and µ2-O atoms.The title compound contains two statistically different protonated hexamolybdoplatinate(IV) polyanions, [H5.5α-PtIVMo5O24]2.5- (A), and [H4.5α-PtIVMo5O24]3.5- (B). Figs. 1 and 2 show the structures of the title compound and polyanions, respectively. The O atoms of the clusters were designated as OT (terminal Mo═O atom), OB (bridging µ2-OB atom; Mo—O—Mo), and OC (centered µ3-O atom; Mo2—OC—Pt).
The H atoms of the protonated O atoms were found in difference Fourier maps and confirmed by bond-length elongation of Mo—O, and change of angles of Mo—OB—Mo and Mo—OC—Mo (Table 1), the interpolyanion hydrogen bonds (Table 2 and Fig. 4), and the bond-valence sums (BVSs; Brown & Altermatt, 1985; Brese & O'Keeffe, 1991). The protonated O atoms in the hexamolybdoplatinates(IV), polyanion (A) and (B), are five (Pt and Mo2)-bound µ3-O (O2C—O6C) and one Mo2-bound µ2-O (O7B) [for polyanion (A)], and four (Pt and Mo2)-bound µ3-O (O26C—O28C and O30C) and one Mo2-bound µ2-O (O31B) [for polyanion (B)] atoms. In addition, one (Pt and Mo2)-bound µ3-O atom [O2C for polyanion (A) and O30C for polyanion (B)] atoms are half-number protonated by disorder (Fig. 2). The residues of the two disordered H atoms, H2 and H30, were confirmed in the difference Fourier map (Fig. 3). This disorder is necessary for charge-balance of the polyanions and in order to avoid unreasonably short H···H distances in the interpolyanion hydrogen bonds.
Two discrete heteropolyanions, (A) and (B), form a dimer, {[H10α-Pt2Mo12O48]6-, held together by two strong pairs of (Pt and Mo2)-bound µ3-OC—H···(Mo)-bound µ1-OT, normally a pair of (Mo2)-bound µ2-OB—H···(Mo2)-bound µ2-OB, and single disordered strong (Pt and Mo2)-bound µ3-OC—H···(Pt and Mo2)-bound µ3-OC hydrogen bonds (Fig. 4 and Table 2). Considering the disorder, the statistically refined formula of the title polyanion, {[H5.5α-PtMo6O24]·[H4.5α-PtMo6O24]}6-, can be rewritten as mixture of dimers of {[H6α-PtMo6O24]; polyanion (A)}·[H4α-PtMo6O24]; polyanion (B)}6- and {[H5α-PtMo6O24]; polyanion (A)}·[H5α-PtMo6O24]; polyanion (B)}6- (Fig. 5). In other words, a set of polyanion (A), [H5.5α-PtMo6O24]2.5-, and polyanion (B), [H4.5α-PtMo6O24]3.5-, are the average disordered formulae of {[H6α-PtMo6O24]2·[H4α-PtMo6O24]4-} and {[H5α-PtMo6O24]3-·[H5α-PtMo6O24]3-} (Fig. 5).
The previously reported [β-H4PtMo6O24]4- polyanion (Lee & Sasaki, 1994; Joo et al., 1994) showed a bent structure (C2v) but the present polyanion shows a near planar structure. The protonated O atoms of [H6PtMo6O24]2- in the present structure show the same protonation scheme as one previously reported (Lee & Joo, 2006a,b), viz. four µ3-OC and two µ2-OB atoms are protonated. However, the protonation scheme of the previously reported polyanion in [H6PtMo6O24]2- (Lee & Joo, 2010) was different, consisting of five µ3-OC and one µ2-OB protonated O atoms. Five protonated polyanion species (A) and (B) were confirmed for the first time in the title compound. Four µ3-O and one µ2-O atoms are protonated in both polyanions, but the position of the unprotonated µ3-O atom differs (Fig. 2).
Confirmation of the protonated O atoms was strongly supported by the BVS analysis. The BVSs for protonated atoms O2C–O6C and O7B in polyanion (A) are 1.58, 1.45, 1.43, 1.36, 1.42 and 1.24, and O26C–O28C, O30C and O31B in the polyanion (B) are 1.41, 1.41, 1.39, 1.33 and 1.24 valence units (v.u.), respectively, if the valence of the O—H bond is not included. As the BVS value around the O atoms in the polyanion should be 2.0 v.u., the missing valences for each of the O atoms are 0.42 (for O2C), 0.55 (for O3C), 0.57 (for O4C), 0.64 (for O5C), 0.58 (for O6C) and 0.76 (for O7B) v.u. in polyanion (A), and 0.59 (for O26C), 0.59 (for O27C), 0.61 (for O28C), 0.67 (for O30C) and 0.76 (for O31B) in polyanion (B), respectively, corresponding to the valence of the O—H bonds. The BVSs around the other unprotonated atoms, O1C and O8B–O12B in the polyanion (A) and O25C, O29C and O32B–O36B in polyanion (B) are 1.82, 1.93, 1.84, 1.85, 1.90 and 1.90, and 1.82, 1.80, 1.94, 1.80, 1.81, 1.70 and 1.94 v.u., respectively, if the valence of the OB and the C···H—OW hydrogen bonds and (OB and C)···Na+ interactions are not included.
All Na+ cations are located on general positions of the 1. The calculated BVSs for the Na1–Na6 ions are 1.22, 1.19, 1.32, 1.10, 1.21 and 1.18 v.u., respectively (Na+···O distance 〈 2.50 Å; total v.u = 7.22). The Na+ ions are variously coordinated by O atoms as [Na1(OT)2(OW)4]+, [Na2(OT)(OW)5]+, [Na3(OT)2(OW)4]+, [Na4(OT)(OW)4]+, [Na5(OT)2(OW)4]+ and [Na6(OT)2(OW)4]+.
PThe dimerized polyanions (A) + (B), {[H10α-Pt2Mo12O48]6-, are connected three-dimensionally by O atoms of the polyanion coordinated to Na+ ions. Two discrete heteropolyanions, (A) and (B), form a dimer, {[H10α-Pt2Mo12O48]6-, held together by two strong pairs of (Pt and Mo2)-bound µ3-OC—H···(Mo)-bound µ1-OT, normally a pair of (Mo2)-bound µ2-OB—H···(Mo2)-bound µ2-OB, and a single disordered strong (Pt and Mo2)-bound µ3O-C—H0.5···(Pt & Mo2)-bound µ3-OC hydrogen bond (Fig. 4 and Table 2). It is notable that the water molecules O21W–O29W, do not show any interaction with the metal atoms and are bonded to other O atoms only by O—H···O hydrogen bonds. The other H atoms of the polyanion (H3, H5 and H27) form hydrogen bonds with water molecules (Table 2).
Crystals of title compound were prepared by the reaction of Na2MoO4·2H2O and Na2Pt(OH)6 at ca pH 1.80 as described in a previous report (Lee & Sasaki, 1994).
The crystal data, the data collection and the structure
details are summarized in Table 3. Atoms O5C and O30C, and O2C and O25C sets required an ISOR restraint in SHELXL2014/7 (Sheldrick, 2015) with reduced deviation s = 0.004 and st = 0.008, and s =0.002 and st = 0.004, respectively. All H atoms of polyanions were located in difference Fourier maps, and were refined a distance restraint of O—H = 0.85 (3) Å using the command DFIX in SHELXL2014/7, and included in the with Uiso(H) = 1.5Ueq(O). The occupancies of atoms H2 and H30 were reduced to 0.5 because of disorder. All H atoms of the water molecules, except O12W–O15W, were located in difference Fourier maps, and were refined using distance restraint of O—H = 0.85 (3) Å and an angle [OK?] restraint of HA—HB = 1.40 (3) Å using the command DFIX in SHELXL2014/7 , and included in the with Uiso(H) = 1.5Ueq(O). An angle restraint of 1.35 (3) Å for O5W, O18W and O19W, and 1.30 (3) Å for O7W was applied. The H atoms of O12W–O13W were positioned geometrically and refined using a riding model (HFIX 137), with OW—H = 0.98 Å and Uiso(H) = 1.5Ueq(O). The H atoms of O14W were refined using a riding model (HFIX 23), with OW—H = 0.99 Å and Uiso(H) = 1.5Ueq(O). All invalid H atoms were removed in the final step of The highest peak in the difference map is 0.82 Å from Pt1 and the deepest hole is 0.98 Å from Pt2.Data collection: APEX2 (Bruker, 2009); cell
SAINT (Bruker, 2009); data reduction: SAINT (Bruker, 2009); program(s) used to solve structure: SHELXS2014/7 (Sheldrick, 2008); program(s) used to refine structure: SHELXL2014/7 (Sheldrick, 2015); molecular graphics: ORTEP-3 for Windows (Farrugia, 2012), PLATON (Spek, 2009) and DIAMOND (Brandenburg, 1998); software used to prepare material for publication: SHELXL2014/7 (Sheldrick, 2015).Fig. 1. The molecular entities in the crystal structure of the title compound. Displacement ellipsoids are drawn at the 50% probability level. The H atoms of the polyanion are presented as small spheres of arbitrary radius and the H atoms of water molecules have been omitted for clarity. | |
Fig. 2. The polyanion structure in the title compound with the atomic numbering scheme and displacement ellipsoids at the 50% probability level for non-H atoms. H atoms are presented as small spheres of arbitrary radius. | |
Fig. 3. Difference-Fourier map around atoms H2 and H30. Calculated with atom H2 and H30 absent from the model. | |
Fig. 4. Polyhedral view of the heteropolyanion in the title compound, with O—H···O contacts of the interpolyanion hydrogen bonds shown as red dashed lines. Disordered H atoms are included. | |
Fig. 5. Polyhedral view of the unit-cell packing in the title compound, with O—H···O contacts of the interpolyanion hydrogen bonds shown as red dashed lines. Disordered H atoms have been omitted. [Symmetry code: (i) -x +1 , -y + 1, -z + 1.] |
H6Mo6O24Pt·H4Mo6O24Pt·29(H2O)·6(Na) | Z = 2 |
Mr = 2979.85 | F(000) = 2820 |
Triclinic, P1 | Dx = 2.891 Mg m−3 |
a = 14.0384 (6) Å | Mo Kα radiation, λ = 0.71073 Å |
b = 15.7969 (6) Å | Cell parameters from 9847 reflections |
c = 16.7235 (6) Å | θ = 2.2–28.3° |
α = 72.825 (2)° | µ = 6.36 mm−1 |
β = 75.522 (2)° | T = 173 K |
γ = 89.168 (2)° | Block, yellow |
V = 3423.7 (2) Å3 | 0.67 × 0.44 × 0.22 mm |
Bruker SMART APEXII CCD diffractometer | 14940 independent reflections |
Radiation source: Rotating Anode | 12688 reflections with I > 2σ(I) |
Graphite multilayer monochromator | Rint = 0.057 |
Detector resolution: 10.0 pixels mm-1 | θmax = 27.0°, θmin = 1.4° |
φ and ω scans | h = −16→17 |
Absorption correction: multi-scan (SADABS; Bruker, 2009) | k = −20→20 |
Tmin = 0.234, Tmax = 0.746 | l = −21→21 |
58415 measured reflections |
Refinement on F2 | Secondary atom site location: difference Fourier map |
Least-squares matrix: full | Hydrogen site location: difference Fourier map |
R[F2 > 2σ(F2)] = 0.036 | Only H-atom coordinates refined |
wR(F2) = 0.091 | w = 1/[σ2(Fo2) + (0.0223P)2 + 5.6226P] where P = (Fo2 + 2Fc2)/3 |
S = 1.06 | (Δ/σ)max = 0.002 |
14940 reflections | Δρmax = 1.73 e Å−3 |
1064 parameters | Δρmin = −2.25 e Å−3 |
114 restraints | Extinction correction: SHELXL2014/7 (Sheldrick 2014, Fc*=kFc[1+0.001xFc2λ3/sin(2θ)]-1/4 |
Primary atom site location: structure-invariant direct methods | Extinction coefficient: 0.00097 (2) |
H6Mo6O24Pt·H4Mo6O24Pt·29(H2O)·6(Na) | γ = 89.168 (2)° |
Mr = 2979.85 | V = 3423.7 (2) Å3 |
Triclinic, P1 | Z = 2 |
a = 14.0384 (6) Å | Mo Kα radiation |
b = 15.7969 (6) Å | µ = 6.36 mm−1 |
c = 16.7235 (6) Å | T = 173 K |
α = 72.825 (2)° | 0.67 × 0.44 × 0.22 mm |
β = 75.522 (2)° |
Bruker SMART APEXII CCD diffractometer | 14940 independent reflections |
Absorption correction: multi-scan (SADABS; Bruker, 2009) | 12688 reflections with I > 2σ(I) |
Tmin = 0.234, Tmax = 0.746 | Rint = 0.057 |
58415 measured reflections |
R[F2 > 2σ(F2)] = 0.036 | 114 restraints |
wR(F2) = 0.091 | Only H-atom coordinates refined |
S = 1.06 | Δρmax = 1.73 e Å−3 |
14940 reflections | Δρmin = −2.25 e Å−3 |
1064 parameters |
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. |
x | y | z | Uiso*/Ueq | Occ. (<1) | |
Pt1 | 0.37861 (2) | 0.80827 (2) | 0.33415 (2) | 0.00743 (6) | |
Pt2 | 0.13101 (2) | 0.69756 (2) | 0.15934 (2) | 0.00734 (6) | |
Mo1 | 0.48088 (3) | 0.73755 (3) | 0.17456 (2) | 0.01032 (9) | |
Mo2 | 0.38120 (3) | 0.92698 (3) | 0.13444 (2) | 0.01043 (9) | |
Mo3 | 0.27924 (3) | 1.00756 (3) | 0.29553 (3) | 0.01189 (9) | |
Mo4 | 0.27941 (3) | 0.89367 (3) | 0.49832 (2) | 0.01226 (9) | |
Mo5 | 0.37444 (3) | 0.69579 (3) | 0.54288 (2) | 0.01302 (9) | |
Mo6 | 0.47496 (3) | 0.61324 (3) | 0.38076 (3) | 0.01233 (9) | |
Mo7 | 0.02597 (3) | 0.89077 (3) | 0.11926 (3) | 0.01261 (9) | |
Mo8 | 0.12559 (3) | 0.81350 (3) | −0.04502 (2) | 0.01205 (9) | |
Mo9 | 0.22090 (3) | 0.61525 (3) | −0.00919 (2) | 0.01097 (9) | |
Mo10 | 0.21502 (3) | 0.49586 (3) | 0.19550 (2) | 0.01178 (9) | |
Mo11 | 0.12327 (3) | 0.56971 (3) | 0.35600 (2) | 0.01106 (9) | |
Mo12 | 0.02151 (3) | 0.76546 (3) | 0.32235 (2) | 0.01089 (9) | |
Na1 | 0.23742 (14) | 0.46059 (13) | 0.69299 (12) | 0.0204 (4) | |
Na2 | 0.23737 (13) | 0.33338 (13) | 0.89570 (12) | 0.0215 (4) | |
Na3 | 0.00711 (13) | 1.06967 (13) | 0.39992 (12) | 0.0207 (4) | |
Na4 | 0.02805 (15) | 1.23682 (14) | 0.20474 (13) | 0.0312 (5) | |
Na5 | 0.25851 (14) | 1.04851 (13) | −0.20594 (12) | 0.0197 (4) | |
Na6 | 0.50542 (14) | 0.56953 (15) | −0.10815 (14) | 0.0302 (5) | |
O1C | 0.4984 (2) | 0.7498 (2) | 0.29268 (19) | 0.0093 (6) | |
O2C | 0.3429 (2) | 0.7918 (2) | 0.2319 (2) | 0.0114 (7) | |
H2 | 0.302 (6) | 0.750 (4) | 0.236 (6) | 0.017* | 0.5 |
O3C | 0.4185 (2) | 0.9314 (2) | 0.25614 (19) | 0.0098 (7) | |
H3 | 0.470 (2) | 0.958 (3) | 0.260 (3) | 0.015* | |
O4C | 0.2544 (2) | 0.8638 (2) | 0.3794 (2) | 0.0116 (7) | |
H4 | 0.199 (2) | 0.840 (3) | 0.382 (3) | 0.017* | |
O5C | 0.4156 (2) | 0.8287 (2) | 0.43710 (19) | 0.0117 (7) | |
H5 | 0.471 (2) | 0.858 (3) | 0.423 (3) | 0.018* | |
O6C | 0.3372 (2) | 0.6876 (2) | 0.4153 (2) | 0.0115 (7) | |
H6 | 0.283 (2) | 0.664 (3) | 0.415 (3) | 0.017* | |
O7B | 0.4252 (2) | 0.6188 (2) | 0.2725 (2) | 0.0165 (7) | |
H7 | 0.372 (3) | 0.593 (3) | 0.275 (3) | 0.025* | |
O8B | 0.5009 (2) | 0.8611 (2) | 0.12156 (19) | 0.0137 (7) | |
O9B | 0.2635 (2) | 0.9556 (2) | 0.20675 (19) | 0.0146 (7) | |
O10B | 0.3285 (2) | 0.9949 (2) | 0.3959 (2) | 0.0157 (7) | |
O11B | 0.2613 (2) | 0.7673 (2) | 0.54830 (19) | 0.0155 (7) | |
O12B | 0.4894 (2) | 0.6608 (2) | 0.4697 (2) | 0.0144 (7) | |
O13T | 0.5925 (2) | 0.5883 (2) | 0.3436 (2) | 0.0215 (8) | |
O14T | 0.4079 (3) | 0.5158 (2) | 0.4360 (2) | 0.0232 (8) | |
O15T | 0.5986 (2) | 0.7061 (2) | 0.1477 (2) | 0.0187 (8) | |
O16T | 0.4206 (2) | 0.7054 (2) | 0.1085 (2) | 0.0165 (7) | |
O17T | 0.3308 (2) | 0.9010 (2) | 0.0596 (2) | 0.0163 (7) | |
O18T | 0.4392 (2) | 1.0292 (2) | 0.0834 (2) | 0.0199 (8) | |
O19T | 0.3365 (3) | 1.1085 (2) | 0.2315 (2) | 0.0230 (8) | |
O20T | 0.1590 (2) | 1.0260 (2) | 0.3325 (2) | 0.0228 (8) | |
O21T | 0.1608 (2) | 0.9179 (2) | 0.5323 (2) | 0.0250 (9) | |
O22T | 0.3430 (3) | 0.9230 (2) | 0.5618 (2) | 0.0225 (8) | |
O23T | 0.4295 (3) | 0.7258 (3) | 0.6111 (2) | 0.0262 (9) | |
O24T | 0.3127 (3) | 0.5959 (2) | 0.5988 (2) | 0.0247 (8) | |
O25C | 0.0097 (2) | 0.7540 (2) | 0.20418 (19) | 0.0101 (7) | |
O26C | 0.1662 (2) | 0.8208 (2) | 0.0782 (2) | 0.0107 (7) | |
H26 | 0.220 (2) | 0.846 (3) | 0.073 (3) | 0.016* | |
O27C | 0.0895 (2) | 0.6796 (2) | 0.05850 (19) | 0.0106 (7) | |
H27 | 0.030 (2) | 0.655 (3) | 0.075 (3) | 0.016* | |
O28C | 0.2520 (2) | 0.6413 (2) | 0.1108 (2) | 0.0103 (7) | |
H28 | 0.311 (2) | 0.654 (3) | 0.111 (3) | 0.015* | |
O29C | 0.0931 (2) | 0.5750 (2) | 0.23650 (19) | 0.0108 (7) | |
O30C | 0.1708 (2) | 0.7142 (2) | 0.26046 (19) | 0.0119 (7) | |
H30 | 0.224 (4) | 0.744 (5) | 0.250 (6) | 0.018* | 0.5 |
O31B | 0.0771 (2) | 0.8849 (2) | 0.2266 (2) | 0.0165 (7) | |
H31 | 0.129 (3) | 0.910 (3) | 0.223 (3) | 0.025* | |
O32B | 0.0110 (2) | 0.8455 (2) | 0.0295 (2) | 0.0150 (7) | |
O33B | 0.2413 (2) | 0.7429 (2) | −0.05672 (19) | 0.0144 (7) | |
O34B | 0.1690 (2) | 0.5144 (2) | 0.09047 (19) | 0.0141 (7) | |
O35B | 0.2443 (2) | 0.5361 (2) | 0.28926 (19) | 0.0147 (7) | |
O36B | 0.0079 (2) | 0.6417 (2) | 0.36859 (19) | 0.0132 (7) | |
O37T | −0.0955 (2) | 0.7942 (2) | 0.3539 (2) | 0.0219 (8) | |
O38T | 0.0849 (2) | 0.7958 (2) | 0.3885 (2) | 0.0180 (8) | |
O39T | −0.0918 (3) | 0.9120 (3) | 0.1604 (2) | 0.0251 (9) | |
O40T | 0.0901 (3) | 0.9901 (2) | 0.0659 (2) | 0.0265 (9) | |
O41T | 0.1871 (3) | 0.9132 (2) | −0.1021 (2) | 0.0230 (8) | |
O42T | 0.0681 (3) | 0.7831 (2) | −0.1111 (2) | 0.0219 (8) | |
O43T | 0.1597 (2) | 0.5900 (2) | −0.0772 (2) | 0.0198 (8) | |
O44T | 0.3380 (2) | 0.5884 (2) | −0.0418 (2) | 0.0210 (8) | |
O45T | 0.3332 (3) | 0.4717 (2) | 0.1580 (2) | 0.0233 (8) | |
O46T | 0.1507 (3) | 0.3978 (2) | 0.2531 (2) | 0.0264 (8) | |
O47T | 0.0646 (2) | 0.4688 (2) | 0.4142 (2) | 0.0200 (8) | |
O48T | 0.1785 (2) | 0.6017 (2) | 0.4253 (2) | 0.0169 (7) | |
O1W | 0.1853 (3) | 0.4397 (3) | 0.5748 (2) | 0.0277 (9) | |
H1A | 0.124 (2) | 0.419 (3) | 0.591 (3) | 0.042* | |
H1B | 0.195 (4) | 0.479 (3) | 0.527 (2) | 0.042* | |
O2W | 0.2834 (3) | 0.4879 (3) | 0.8111 (2) | 0.0258 (9) | |
H2A | 0.344 (2) | 0.506 (3) | 0.800 (3) | 0.039* | |
H2B | 0.251 (3) | 0.524 (3) | 0.837 (3) | 0.039* | |
O3W | −0.0402 (3) | 0.9185 (2) | 0.4682 (2) | 0.0248 (8) | |
H3A | −0.1018 (19) | 0.904 (4) | 0.473 (3) | 0.037* | |
H3B | −0.003 (3) | 0.883 (3) | 0.447 (4) | 0.037* | |
O4W | 0.0692 (3) | 0.2145 (3) | 0.3358 (3) | 0.0327 (9) | |
H4A | 0.131 (2) | 0.221 (4) | 0.336 (4) | 0.049* | |
H4B | 0.035 (3) | 0.245 (4) | 0.362 (4) | 0.049* | |
O5W | 0.5335 (3) | 0.5855 (3) | 0.0218 (3) | 0.0339 (10) | |
H5A | 0.500 (3) | 0.621 (3) | 0.046 (4) | 0.051* | |
H5B | 0.591 (2) | 0.601 (4) | 0.007 (4) | 0.051* | |
O6W | 0.1875 (3) | 0.3127 (2) | 0.7759 (2) | 0.0207 (8) | |
H6A | 0.1274 (19) | 0.292 (3) | 0.790 (3) | 0.031* | |
H6B | 0.225 (3) | 0.273 (3) | 0.760 (3) | 0.031* | |
O7W | 0.1841 (3) | 0.1846 (3) | 0.9808 (3) | 0.0267 (9) | |
H7A | 0.221 (3) | 0.151 (3) | 0.959 (4) | 0.040* | |
H7B | 0.126 (2) | 0.175 (4) | 0.982 (4) | 0.040* | |
O8W | 0.2657 (3) | 0.3672 (2) | 1.0195 (2) | 0.0254 (8) | |
H8A | 0.247 (4) | 0.411 (2) | 1.040 (3) | 0.038* | |
H8B | 0.239 (4) | 0.320 (2) | 1.061 (3) | 0.038* | |
O9W | 0.1896 (3) | 0.2051 (3) | 0.1354 (3) | 0.0366 (10) | |
H9A | 0.229 (4) | 0.180 (4) | 0.162 (3) | 0.055* | |
H9B | 0.184 (4) | 0.183 (4) | 0.096 (3) | 0.055* | |
O10W | 0.8819 (3) | 0.2975 (3) | 0.2745 (3) | 0.0474 (11) | |
H10A | 0.875 (4) | 0.287 (5) | 0.328 (2) | 0.071* | |
H10B | 0.832 (4) | 0.276 (5) | 0.263 (4) | 0.071* | |
O11W | 0.0385 (3) | 0.3872 (2) | 0.0928 (2) | 0.0261 (8) | |
H11A | 0.073 (3) | 0.420 (3) | 0.109 (3) | 0.039* | |
H11B | −0.022 (2) | 0.398 (4) | 0.103 (4) | 0.039* | |
O12W | 0.2141 (3) | 0.9781 (4) | 0.7002 (3) | 0.0618 (16) | |
H12A | 0.2596 | 0.9318 | 0.6923 | 0.093* | |
H12B | 0.2181 | 1.0222 | 0.6440 | 0.093* | |
O13W | −0.0165 (3) | 1.0739 (3) | 0.2621 (2) | 0.0315 (9) | |
H13A | −0.0853 | 1.0581 | 0.2644 | 0.047* | |
H13B | 0.0300 | 1.0386 | 0.2321 | 0.047* | |
O14W | 0.4187 (2) | 0.9806 (2) | 0.7644 (2) | 0.0233 (8) | |
H14A | 0.4196 | 0.9282 | 0.8133 | 0.035* | |
H14B | 0.4274 | 0.9631 | 0.7116 | 0.035* | |
O15W | 0.0789 (3) | 0.3932 (2) | 0.9223 (2) | 0.0219 (8) | |
H15A | 0.073 (4) | 0.439 (3) | 0.884 (2) | 0.033* | |
H15B | 0.075 (4) | 0.399 (3) | 0.9722 (19) | 0.033* | |
O16W | 0.4775 (3) | 0.5453 (4) | 0.7651 (3) | 0.0575 (15) | |
H16A | 0.461 (5) | 0.600 (3) | 0.762 (5) | 0.086* | |
H16B | 0.518 (4) | 0.550 (4) | 0.717 (3) | 0.086* | |
O17W | 0.3075 (3) | 1.0648 (3) | −0.0822 (2) | 0.0257 (9) | |
H17A | 0.362 (3) | 1.089 (3) | −0.098 (3) | 0.039* | |
H17B | 0.300 (4) | 1.015 (2) | −0.043 (3) | 0.039* | |
O18W | 0.3126 (3) | 0.1933 (3) | 0.7104 (2) | 0.0250 (9) | |
H18A | 0.308 (4) | 0.205 (4) | 0.660 (2) | 0.038* | |
H18B | 0.367 (3) | 0.208 (4) | 0.712 (3) | 0.038* | |
O19W | 0.0830 (3) | 0.5111 (3) | 0.7640 (3) | 0.0279 (9) | |
H19A | 0.032 (3) | 0.493 (3) | 0.754 (4) | 0.042* | |
H19B | 0.093 (4) | 0.5638 (18) | 0.744 (4) | 0.042* | |
O20W | 0.5152 (5) | 0.7241 (3) | 0.8036 (4) | 0.0765 (17) | |
H20A | 0.540 (7) | 0.731 (6) | 0.845 (5) | 0.115* | |
H20B | 0.483 (6) | 0.769 (4) | 0.785 (5) | 0.115* | |
O21W | 0.2843 (4) | 0.7843 (4) | 0.7520 (3) | 0.0685 (16) | |
H21A | 0.340 (4) | 0.771 (5) | 0.720 (4) | 0.103* | |
H21B | 0.290 (5) | 0.766 (6) | 0.804 (2) | 0.103* | |
O22W | −0.2460 (4) | 0.8598 (3) | 0.4844 (3) | 0.0504 (12) | |
H22A | −0.246 (5) | 0.824 (4) | 0.452 (3) | 0.076* | |
H22B | −0.257 (6) | 0.827 (4) | 0.5371 (19) | 0.076* | |
O23W | 0.5070 (3) | 0.8893 (3) | 0.6478 (3) | 0.0476 (12) | |
H23A | 0.487 (4) | 0.889 (5) | 0.603 (3) | 0.071* | |
H23B | 0.564 (3) | 0.917 (4) | 0.628 (4) | 0.071* | |
O24W | 0.3421 (3) | 0.3767 (3) | 0.3558 (3) | 0.0424 (11) | |
H24A | 0.339 (5) | 0.358 (4) | 0.409 (2) | 0.064* | |
H24B | 0.305 (4) | 0.423 (3) | 0.347 (4) | 0.064* | |
O25W | −0.0526 (4) | 0.3217 (3) | 0.4196 (3) | 0.0541 (14) | |
H25A | −0.097 (4) | 0.302 (4) | 0.465 (3) | 0.081* | |
H25B | −0.029 (5) | 0.373 (3) | 0.416 (4) | 0.081* | |
O26W | 0.2713 (3) | 0.2255 (3) | 0.3382 (3) | 0.0518 (12) | |
H26A | 0.277 (5) | 0.282 (2) | 0.335 (4) | 0.078* | |
H26B | 0.309 (5) | 0.219 (4) | 0.291 (3) | 0.078* | |
O27W | 0.4268 (3) | 0.8374 (3) | −0.0976 (3) | 0.0378 (10) | |
H27A | 0.465 (4) | 0.845 (4) | −0.067 (3) | 0.057* | |
H27B | 0.379 (3) | 0.799 (3) | −0.065 (3) | 0.057* | |
O28W | 0.3135 (3) | 0.3091 (3) | 0.5390 (3) | 0.0300 (9) | |
H28A | 0.373 (2) | 0.326 (4) | 0.533 (4) | 0.045* | |
H28B | 0.277 (3) | 0.348 (3) | 0.555 (4) | 0.045* | |
O29W | 0.5730 (3) | 0.9091 (3) | 0.4418 (3) | 0.0440 (12) | |
H29A | 0.573 (5) | 0.966 (2) | 0.420 (4) | 0.066* | |
H29B | 0.621 (4) | 0.896 (4) | 0.463 (4) | 0.066* |
U11 | U22 | U33 | U12 | U13 | U23 | |
Pt1 | 0.00954 (10) | 0.00867 (10) | 0.00598 (9) | −0.00002 (7) | −0.00068 (6) | −0.00612 (7) |
Pt2 | 0.00933 (10) | 0.00833 (10) | 0.00628 (9) | 0.00006 (7) | −0.00122 (6) | −0.00569 (7) |
Mo1 | 0.0110 (2) | 0.0139 (2) | 0.01004 (19) | 0.00019 (16) | −0.00179 (15) | −0.01018 (16) |
Mo2 | 0.0118 (2) | 0.0125 (2) | 0.00893 (19) | −0.00137 (16) | −0.00222 (14) | −0.00634 (16) |
Mo3 | 0.0139 (2) | 0.0111 (2) | 0.0126 (2) | 0.00246 (16) | −0.00246 (15) | −0.00733 (16) |
Mo4 | 0.0147 (2) | 0.0147 (2) | 0.00968 (19) | 0.00173 (16) | −0.00023 (15) | −0.00955 (17) |
Mo5 | 0.0176 (2) | 0.0135 (2) | 0.00813 (19) | 0.00016 (17) | −0.00184 (15) | −0.00471 (16) |
Mo6 | 0.0149 (2) | 0.0109 (2) | 0.0134 (2) | 0.00249 (16) | −0.00354 (15) | −0.00718 (17) |
Mo7 | 0.0148 (2) | 0.0111 (2) | 0.0145 (2) | 0.00282 (16) | −0.00414 (16) | −0.00732 (17) |
Mo8 | 0.0162 (2) | 0.0121 (2) | 0.00841 (19) | −0.00019 (16) | −0.00287 (15) | −0.00410 (16) |
Mo9 | 0.0123 (2) | 0.0136 (2) | 0.00969 (19) | 0.00170 (16) | −0.00127 (15) | −0.00888 (16) |
Mo10 | 0.0152 (2) | 0.0105 (2) | 0.0114 (2) | 0.00199 (16) | −0.00271 (15) | −0.00665 (16) |
Mo11 | 0.0133 (2) | 0.0140 (2) | 0.00731 (19) | −0.00197 (16) | −0.00172 (14) | −0.00598 (16) |
Mo12 | 0.0122 (2) | 0.0140 (2) | 0.01044 (19) | 0.00028 (16) | −0.00208 (15) | −0.01016 (17) |
Na1 | 0.0246 (11) | 0.0195 (10) | 0.0167 (10) | −0.0017 (8) | −0.0031 (8) | −0.0068 (8) |
Na2 | 0.0182 (10) | 0.0275 (11) | 0.0215 (10) | 0.0043 (8) | −0.0049 (8) | −0.0117 (9) |
Na3 | 0.0208 (11) | 0.0216 (11) | 0.0191 (10) | 0.0018 (9) | −0.0013 (8) | −0.0083 (9) |
Na4 | 0.0332 (12) | 0.0398 (13) | 0.0217 (11) | 0.0021 (10) | −0.0076 (9) | −0.0105 (10) |
Na5 | 0.0196 (10) | 0.0193 (10) | 0.0213 (10) | −0.0013 (8) | −0.0044 (8) | −0.0083 (8) |
Na6 | 0.0196 (11) | 0.0406 (14) | 0.0390 (13) | 0.0043 (10) | −0.0025 (9) | −0.0292 (11) |
O1C | 0.0109 (15) | 0.0103 (16) | 0.0102 (15) | 0.0030 (12) | −0.0029 (12) | −0.0083 (13) |
O2C | 0.0134 (13) | 0.0141 (14) | 0.0093 (13) | −0.0001 (11) | −0.0014 (10) | −0.0088 (11) |
O3C | 0.0123 (16) | 0.0073 (16) | 0.0114 (16) | −0.0029 (13) | −0.0031 (12) | −0.0049 (13) |
O4C | 0.0082 (16) | 0.0139 (17) | 0.0170 (17) | 0.0010 (13) | −0.0028 (13) | −0.0115 (14) |
O5C | 0.0134 (16) | 0.0147 (16) | 0.0107 (15) | 0.0002 (13) | −0.0019 (12) | −0.0106 (13) |
O6C | 0.0096 (16) | 0.0118 (17) | 0.0130 (16) | −0.0011 (13) | −0.0008 (12) | −0.0054 (14) |
O7B | 0.0179 (18) | 0.0164 (18) | 0.0179 (18) | −0.0008 (14) | −0.0056 (14) | −0.0083 (15) |
O8B | 0.0117 (16) | 0.0169 (17) | 0.0131 (16) | −0.0017 (13) | −0.0007 (12) | −0.0076 (14) |
O9B | 0.0162 (17) | 0.0183 (18) | 0.0122 (16) | −0.0005 (14) | −0.0028 (13) | −0.0098 (14) |
O10B | 0.0210 (18) | 0.0127 (17) | 0.0143 (17) | −0.0001 (14) | −0.0017 (13) | −0.0079 (14) |
O11B | 0.0175 (17) | 0.0145 (17) | 0.0120 (16) | 0.0014 (14) | 0.0016 (13) | −0.0046 (14) |
O12B | 0.0171 (17) | 0.0152 (17) | 0.0147 (17) | 0.0039 (14) | −0.0060 (13) | −0.0088 (14) |
O13T | 0.0180 (19) | 0.028 (2) | 0.0227 (19) | 0.0080 (16) | −0.0045 (14) | −0.0154 (16) |
O14T | 0.034 (2) | 0.0139 (18) | 0.0215 (19) | −0.0022 (16) | −0.0071 (16) | −0.0049 (15) |
O15T | 0.0132 (17) | 0.025 (2) | 0.0213 (18) | 0.0026 (15) | −0.0010 (14) | −0.0142 (16) |
O16T | 0.0179 (18) | 0.0210 (19) | 0.0146 (17) | 0.0004 (14) | −0.0025 (13) | −0.0125 (15) |
O17T | 0.0168 (17) | 0.0228 (19) | 0.0122 (16) | −0.0011 (14) | −0.0023 (13) | −0.0104 (15) |
O18T | 0.0229 (19) | 0.0205 (19) | 0.0144 (18) | −0.0061 (15) | −0.0014 (14) | −0.0051 (15) |
O19T | 0.031 (2) | 0.0169 (19) | 0.0208 (19) | −0.0033 (15) | −0.0048 (15) | −0.0063 (15) |
O20T | 0.0149 (18) | 0.029 (2) | 0.027 (2) | 0.0067 (16) | −0.0029 (15) | −0.0146 (17) |
O21T | 0.0176 (19) | 0.029 (2) | 0.025 (2) | 0.0050 (16) | 0.0054 (15) | −0.0127 (17) |
O22T | 0.033 (2) | 0.024 (2) | 0.0157 (18) | −0.0011 (16) | −0.0057 (15) | −0.0140 (16) |
O23T | 0.032 (2) | 0.035 (2) | 0.0200 (19) | 0.0023 (17) | −0.0101 (16) | −0.0176 (17) |
O24T | 0.030 (2) | 0.0184 (19) | 0.0189 (19) | −0.0024 (16) | −0.0004 (15) | −0.0012 (16) |
O25C | 0.0109 (13) | 0.0106 (13) | 0.0118 (13) | 0.0017 (11) | −0.0010 (10) | −0.0095 (11) |
O26C | 0.0106 (16) | 0.0088 (16) | 0.0126 (16) | −0.0009 (13) | −0.0011 (13) | −0.0046 (13) |
O27C | 0.0116 (16) | 0.0128 (17) | 0.0118 (16) | 0.0008 (13) | −0.0036 (12) | −0.0097 (13) |
O28C | 0.0078 (16) | 0.0139 (17) | 0.0137 (16) | 0.0008 (13) | −0.0028 (12) | −0.0107 (13) |
O29C | 0.0149 (16) | 0.0083 (16) | 0.0090 (15) | −0.0016 (13) | −0.0019 (12) | −0.0033 (13) |
O30C | 0.0146 (16) | 0.0170 (16) | 0.0071 (14) | 0.0015 (13) | −0.0025 (12) | −0.0086 (13) |
O31B | 0.0172 (18) | 0.0169 (18) | 0.0187 (18) | −0.0032 (14) | −0.0050 (14) | −0.0098 (15) |
O32B | 0.0168 (17) | 0.0174 (18) | 0.0147 (17) | 0.0048 (14) | −0.0062 (13) | −0.0092 (14) |
O33B | 0.0142 (17) | 0.0170 (18) | 0.0115 (16) | −0.0008 (14) | −0.0005 (12) | −0.0060 (14) |
O34B | 0.0181 (17) | 0.0137 (17) | 0.0123 (16) | 0.0003 (14) | −0.0036 (13) | −0.0068 (14) |
O35B | 0.0151 (17) | 0.0201 (18) | 0.0122 (16) | 0.0034 (14) | −0.0029 (13) | −0.0104 (14) |
O36B | 0.0125 (16) | 0.0164 (17) | 0.0115 (16) | −0.0040 (13) | 0.0004 (12) | −0.0079 (14) |
O37T | 0.0159 (18) | 0.032 (2) | 0.0221 (19) | 0.0039 (16) | −0.0011 (14) | −0.0178 (17) |
O38T | 0.0196 (18) | 0.0205 (19) | 0.0149 (17) | −0.0046 (15) | −0.0007 (14) | −0.0097 (15) |
O39T | 0.0205 (19) | 0.033 (2) | 0.030 (2) | 0.0133 (17) | −0.0092 (16) | −0.0201 (18) |
O40T | 0.039 (2) | 0.0172 (19) | 0.025 (2) | −0.0015 (17) | −0.0113 (17) | −0.0063 (16) |
O41T | 0.030 (2) | 0.0172 (19) | 0.0171 (18) | −0.0043 (16) | −0.0003 (15) | −0.0032 (15) |
O42T | 0.028 (2) | 0.026 (2) | 0.0211 (19) | 0.0054 (16) | −0.0140 (15) | −0.0138 (16) |
O43T | 0.0244 (19) | 0.0236 (19) | 0.0180 (18) | 0.0016 (15) | −0.0083 (14) | −0.0135 (16) |
O44T | 0.0156 (18) | 0.027 (2) | 0.0215 (19) | 0.0048 (15) | −0.0002 (14) | −0.0134 (16) |
O45T | 0.0208 (19) | 0.031 (2) | 0.025 (2) | 0.0141 (16) | −0.0094 (15) | −0.0179 (17) |
O46T | 0.036 (2) | 0.0189 (19) | 0.025 (2) | −0.0033 (16) | −0.0065 (16) | −0.0082 (16) |
O47T | 0.026 (2) | 0.0193 (19) | 0.0133 (18) | −0.0052 (15) | −0.0020 (14) | −0.0045 (15) |
O48T | 0.0179 (18) | 0.0215 (19) | 0.0121 (17) | −0.0015 (14) | −0.0030 (13) | −0.0069 (15) |
O1W | 0.028 (2) | 0.034 (2) | 0.019 (2) | −0.0081 (18) | −0.0076 (16) | −0.0033 (17) |
O2W | 0.021 (2) | 0.032 (2) | 0.026 (2) | −0.0052 (17) | 0.0003 (16) | −0.0175 (18) |
O3W | 0.027 (2) | 0.027 (2) | 0.023 (2) | 0.0053 (17) | −0.0023 (16) | −0.0141 (17) |
O4W | 0.045 (3) | 0.027 (2) | 0.030 (2) | −0.0024 (19) | −0.0093 (19) | −0.0144 (18) |
O5W | 0.018 (2) | 0.044 (3) | 0.053 (3) | 0.0046 (19) | −0.0056 (19) | −0.039 (2) |
O6W | 0.0196 (19) | 0.021 (2) | 0.0224 (19) | −0.0023 (15) | −0.0023 (15) | −0.0101 (16) |
O7W | 0.022 (2) | 0.028 (2) | 0.035 (2) | 0.0009 (17) | −0.0071 (17) | −0.0165 (18) |
O8W | 0.029 (2) | 0.025 (2) | 0.024 (2) | −0.0001 (17) | −0.0029 (16) | −0.0139 (17) |
O9W | 0.046 (3) | 0.039 (3) | 0.026 (2) | 0.014 (2) | −0.0111 (18) | −0.0095 (19) |
O10W | 0.047 (3) | 0.062 (3) | 0.030 (2) | 0.006 (2) | −0.003 (2) | −0.015 (2) |
O11W | 0.0184 (19) | 0.032 (2) | 0.036 (2) | −0.0039 (17) | −0.0055 (16) | −0.0239 (18) |
O12W | 0.033 (3) | 0.122 (5) | 0.047 (3) | −0.013 (3) | 0.003 (2) | −0.059 (3) |
O13W | 0.031 (2) | 0.038 (2) | 0.029 (2) | 0.0038 (18) | −0.0092 (17) | −0.0140 (18) |
O14W | 0.0219 (19) | 0.026 (2) | 0.025 (2) | −0.0024 (16) | −0.0042 (15) | −0.0134 (17) |
O15W | 0.0180 (18) | 0.030 (2) | 0.0205 (19) | 0.0008 (16) | −0.0039 (15) | −0.0124 (17) |
O16W | 0.029 (3) | 0.104 (4) | 0.052 (3) | −0.008 (3) | −0.001 (2) | −0.050 (3) |
O17W | 0.025 (2) | 0.025 (2) | 0.023 (2) | −0.0075 (17) | −0.0051 (16) | −0.0021 (17) |
O18W | 0.024 (2) | 0.024 (2) | 0.028 (2) | −0.0037 (17) | −0.0076 (17) | −0.0068 (18) |
O19W | 0.022 (2) | 0.025 (2) | 0.036 (2) | −0.0005 (17) | −0.0053 (17) | −0.0087 (19) |
O20W | 0.086 (5) | 0.045 (3) | 0.084 (5) | −0.003 (3) | 0.015 (3) | −0.026 (3) |
O21W | 0.056 (3) | 0.109 (5) | 0.033 (3) | 0.002 (3) | 0.007 (2) | −0.024 (3) |
O22W | 0.051 (3) | 0.056 (3) | 0.063 (3) | 0.013 (2) | −0.022 (3) | −0.041 (3) |
O23W | 0.033 (2) | 0.077 (3) | 0.044 (3) | −0.017 (2) | −0.004 (2) | −0.037 (3) |
O24W | 0.065 (3) | 0.042 (3) | 0.029 (2) | 0.008 (2) | −0.023 (2) | −0.014 (2) |
O25W | 0.059 (3) | 0.052 (3) | 0.046 (3) | −0.027 (2) | 0.021 (2) | −0.033 (3) |
O26W | 0.047 (3) | 0.050 (3) | 0.069 (3) | 0.005 (2) | −0.011 (2) | −0.037 (3) |
O27W | 0.041 (3) | 0.038 (3) | 0.034 (2) | −0.007 (2) | −0.0026 (19) | −0.015 (2) |
O28W | 0.024 (2) | 0.036 (2) | 0.034 (2) | −0.0010 (18) | −0.0077 (18) | −0.0154 (19) |
O29W | 0.032 (3) | 0.036 (3) | 0.071 (3) | −0.003 (2) | −0.019 (2) | −0.022 (3) |
Mo1—O1C | 2.114 (3) | Na4—O10Wv | 2.428 (5) |
Mo6—O1C | 2.198 (3) | Na4—O13W | 2.495 (4) |
Mo1—O2C | 2.216 (3) | Na4—O11Wii | 2.534 (4) |
Mo2—O2C | 2.246 (3) | Na5—O18Wvi | 2.322 (4) |
Mo2—O3C | 2.245 (3) | Na5—O41T | 2.364 (4) |
Mo3—O3C | 2.336 (3) | Na5—O12Wvii | 2.373 (4) |
Mo3—O4C | 2.267 (3) | Na5—O39Tiv | 2.406 (4) |
Mo4—O4C | 2.283 (3) | Na5—O17W | 2.419 (4) |
Mo4—O5C | 2.312 (3) | Na5—O14Wvii | 2.478 (4) |
Mo5—O5C | 2.280 (3) | Na6—O45Tviii | 2.363 (4) |
Mo5—O6C | 2.358 (3) | Na6—O16Wvii | 2.386 (5) |
Mo6—O6C | 2.287 (3) | Na6—O5W | 2.387 (5) |
Mo7—O25C | 2.186 (3) | Na6—O44T | 2.390 (4) |
Mo12—O25C | 2.084 (3) | Na6—O5Wviii | 2.436 (5) |
Mo7—O26C | 2.297 (3) | Na6—O20Wvii | 2.437 (6) |
Mo8—O26C | 2.305 (3) | O2C—O30C | 2.595 (5) |
Mo8—O27C | 2.272 (3) | O2C—H2 | 0.86 (3) |
Mo9—O27C | 2.302 (3) | O3C—H3 | 0.86 (3) |
Mo9—O28C | 2.307 (3) | O4C—H4 | 0.85 (3) |
Mo10—O28C | 2.302 (3) | O5C—H5 | 0.86 (3) |
Mo10—O29C | 2.196 (3) | O6C—H6 | 0.86 (3) |
Mo11—O29C | 2.122 (3) | O7B—H7 | 0.84 (3) |
Mo11—O30C | 2.359 (3) | O13T—Na1i | 2.483 (4) |
Mo12—O30C | 2.340 (3) | O15T—Na2i | 2.369 (4) |
Mo1—O7B | 2.098 (3) | O21T—Na3iii | 2.379 (4) |
Mo6—O7B | 2.076 (3) | O26C—H26 | 0.82 (3) |
Mo1—O8B | 1.883 (3) | O27C—H27 | 0.87 (3) |
Mo2—O8B | 1.963 (3) | O28C—H28 | 0.86 (3) |
Mo2—O9B | 1.924 (3) | O30C—H30 | 0.84 (3) |
Mo3—O9B | 1.953 (3) | O31B—H31 | 0.82 (3) |
Mo3—O10B | 1.927 (3) | O39T—Na5iv | 2.406 (4) |
Mo4—O10B | 1.947 (3) | O42T—Na4iv | 2.394 (4) |
Mo4—O11B | 1.916 (3) | O45T—Na6viii | 2.363 (4) |
Mo5—O11B | 1.935 (3) | O1W—H1A | 0.87 (3) |
Mo5—O12B | 1.947 (3) | O1W—H1B | 0.84 (3) |
Mo6—O12B | 1.906 (3) | O2W—H2A | 0.86 (3) |
Mo7—O31B | 2.072 (3) | O2W—H2B | 0.87 (3) |
Mo12—O31B | 2.090 (3) | O3W—Na3iii | 2.424 (4) |
Mo7—O32B | 1.899 (3) | O3W—H3A | 0.87 (3) |
Mo8—O32B | 1.935 (3) | O3W—H3B | 0.86 (3) |
Mo8—O33B | 1.959 (3) | O4W—Na3ix | 2.299 (4) |
Mo9—O33B | 1.932 (3) | O4W—Na4ix | 2.330 (4) |
Mo9—O34B | 1.925 (3) | O4W—H4A | 0.88 (3) |
Mo10—O34B | 1.961 (3) | O4W—H4B | 0.82 (3) |
Mo10—O35B | 1.988 (3) | O5W—Na6viii | 2.436 (5) |
Mo11—O35B | 1.947 (3) | O5W—H5A | 0.85 (3) |
Mo11—O36B | 1.970 (3) | O5W—H5B | 0.81 (3) |
Mo12—O36B | 1.870 (3) | O6W—H6A | 0.86 (3) |
Pt1—O1C | 1.978 (3) | O6W—H6B | 0.87 (3) |
Pt1—O6C | 1.980 (3) | O7W—H7A | 0.82 (3) |
Pt1—O2C | 1.984 (3) | O7W—H7B | 0.82 (3) |
Pt1—O3C | 1.992 (3) | O8W—H8A | 0.87 (3) |
Pt1—O4C | 2.018 (3) | O8W—H8B | 0.87 (3) |
Pt1—O5C | 2.029 (3) | O9W—Na4ix | 2.395 (4) |
Pt1—Mo1 | 3.1985 (4) | O9W—H9A | 0.83 (3) |
Pt2—O29C | 1.977 (3) | O9W—H9B | 0.86 (3) |
Pt2—O25C | 1.993 (3) | O10W—Na4x | 2.428 (5) |
Pt2—O30C | 1.995 (3) | O10W—H10A | 0.84 (3) |
Pt2—O26C | 2.002 (3) | O10W—H10B | 0.86 (3) |
Pt2—O28C | 2.006 (3) | O11W—Na4ix | 2.534 (4) |
Pt2—O27C | 2.011 (3) | O11W—H11A | 0.85 (3) |
Mo1—O15T | 1.707 (3) | O11W—H11B | 0.85 (3) |
Mo1—O16T | 1.734 (3) | O12W—Na5xi | 2.373 (4) |
Mo2—O18T | 1.696 (3) | O12W—H12A | 0.9800 |
Mo2—O17T | 1.729 (3) | O12W—H12B | 0.9800 |
Mo3—O20T | 1.698 (3) | O13W—H13A | 0.9900 |
Mo3—O19T | 1.713 (3) | O13W—H13B | 0.9900 |
Mo4—O21T | 1.697 (3) | O14W—Na5xi | 2.478 (4) |
Mo4—O22T | 1.708 (3) | O14W—H14A | 0.9799 |
Mo5—O24T | 1.697 (3) | O14W—H14B | 0.9801 |
Mo5—O23T | 1.701 (3) | O15W—O11Wxi | 2.738 (5) |
Mo6—O13T | 1.696 (3) | O15W—O19W | 2.738 (5) |
Mo6—O14T | 1.696 (3) | O15W—H15A | 0.83 (3) |
Mo7—O39T | 1.695 (3) | O15W—H15B | 0.86 (3) |
Mo7—O40T | 1.697 (4) | O16W—Na6xi | 2.386 (5) |
Mo8—O42T | 1.696 (3) | O16W—O24Wi | 2.842 (6) |
Mo8—O41T | 1.696 (3) | O16W—O7Bi | 3.068 (6) |
Mo9—O44T | 1.688 (3) | O16W—H16A | 0.89 (3) |
Mo9—O43T | 1.719 (3) | O16W—H16B | 0.85 (3) |
Mo10—O46T | 1.693 (3) | O17W—H17A | 0.81 (3) |
Mo10—O45T | 1.701 (3) | O17W—H17B | 0.84 (3) |
Mo10—Mo11 | 3.2096 (5) | O18W—Na5xii | 2.322 (4) |
Mo11—O47T | 1.699 (3) | O18W—H18A | 0.83 (3) |
Mo11—O48T | 1.735 (3) | O18W—H18B | 0.81 (3) |
Mo12—O37T | 1.694 (3) | O19W—H19A | 0.85 (3) |
Mo12—O38T | 1.750 (3) | O19W—H19B | 0.80 (3) |
Na1—O24T | 2.326 (4) | O20W—Na6xi | 2.437 (6) |
Na1—O6W | 2.349 (4) | O20W—H20A | 0.88 (3) |
Na1—O2W | 2.377 (4) | O20W—H20B | 0.85 (3) |
Na1—O1W | 2.380 (4) | O21W—H21A | 0.89 (3) |
Na1—O19W | 2.443 (4) | O21W—H21B | 0.86 (3) |
Na1—O13Ti | 2.483 (4) | O22W—H22A | 0.88 (3) |
Na2—O15Ti | 2.369 (4) | O22W—H22B | 0.85 (3) |
Na2—O7W | 2.377 (4) | O23W—H23A | 0.87 (3) |
Na2—O6W | 2.388 (4) | O23W—H23B | 0.85 (3) |
Na2—O15W | 2.393 (4) | O24W—H24A | 0.84 (3) |
Na2—O8W | 2.408 (4) | O24W—H24B | 0.89 (3) |
Na2—O2W | 2.434 (4) | O25W—H25A | 0.83 (3) |
Na3—O4Wii | 2.299 (4) | O25W—H25B | 0.86 (3) |
Na3—O3W | 2.347 (4) | O26W—H26A | 0.87 (3) |
Na3—O20T | 2.348 (4) | O26W—H26B | 0.87 (3) |
Na3—O21Tiii | 2.379 (4) | O27W—H27A | 0.86 (3) |
Na3—O13W | 2.390 (4) | O27W—H27B | 0.87 (3) |
Na3—O3Wiii | 2.424 (4) | O28W—H28A | 0.86 (3) |
Na3—Na3iii | 3.379 (4) | O28W—H28B | 0.86 (3) |
Na4—O4Wii | 2.330 (4) | O29W—H29A | 0.86 (3) |
Na4—O42Tiv | 2.394 (4) | O29W—H29B | 0.84 (3) |
Na4—O9Wii | 2.395 (4) | ||
Mo1—O1C—Mo6 | 104.42 (13) | O46T—Mo10—O35B | 101.20 (15) |
Mo1—O2C—Mo2 | 93.27 (12) | O45T—Mo10—O35B | 94.06 (15) |
Mo2—O3C—Mo3 | 92.61 (11) | O34B—Mo10—O35B | 152.77 (13) |
Mo3—O4C—Mo4 | 94.36 (12) | O46T—Mo10—O29C | 93.58 (15) |
Mo5—O5C—Mo4 | 93.05 (11) | O45T—Mo10—O29C | 157.99 (15) |
Mo6—O6C—Mo5 | 91.98 (11) | O34B—Mo10—O29C | 86.01 (12) |
Mo6—O7B—Mo1 | 109.51 (15) | O35B—Mo10—O29C | 73.14 (12) |
Mo1—O8B—Mo2 | 115.01 (15) | O46T—Mo10—O28C | 161.08 (15) |
Mo2—O9B—Mo3 | 117.38 (16) | O45T—Mo10—O28C | 90.14 (15) |
Mo3—O10B—Mo4 | 118.97 (16) | O34B—Mo10—O28C | 70.72 (12) |
Mo4—O11B—Mo5 | 119.86 (16) | O35B—Mo10—O28C | 85.87 (12) |
Mo6—O12B—Mo5 | 120.24 (16) | O29C—Mo10—O28C | 71.49 (11) |
Mo12—O25C—Mo7 | 104.38 (13) | O46T—Mo10—Mo11 | 88.46 (12) |
Mo7—O26C—Mo8 | 92.23 (11) | O45T—Mo10—Mo11 | 128.96 (12) |
Mo8—O27C—Mo9 | 93.67 (11) | O34B—Mo10—Mo11 | 127.13 (9) |
Mo10—O28C—Mo9 | 93.85 (11) | O35B—Mo10—Mo11 | 34.92 (9) |
Mo11—O29C—Mo10 | 96.01 (12) | O29C—Mo10—Mo11 | 41.12 (8) |
Mo12—O30C—Mo11 | 90.63 (11) | O28C—Mo10—Mo11 | 87.55 (8) |
Mo7—O31B—Mo12 | 108.35 (15) | O47T—Mo11—O48T | 105.57 (15) |
Mo7—O32B—Mo8 | 119.84 (16) | O47T—Mo11—O35B | 101.45 (15) |
Mo9—O33B—Mo8 | 118.01 (15) | O48T—Mo11—O35B | 95.26 (14) |
Mo9—O34B—Mo10 | 120.01 (16) | O47T—Mo11—O36B | 97.92 (15) |
Mo11—O35B—Mo10 | 109.31 (15) | O48T—Mo11—O36B | 97.46 (14) |
Mo12—O36B—Mo11 | 120.93 (15) | O35B—Mo11—O36B | 153.01 (13) |
O1C—Pt1—O6C | 82.75 (13) | O47T—Mo11—O29C | 97.13 (14) |
O1C—Pt1—O2C | 83.08 (12) | O48T—Mo11—O29C | 156.88 (14) |
O6C—Pt1—O2C | 98.53 (13) | O35B—Mo11—O29C | 75.62 (12) |
O1C—Pt1—O3C | 98.76 (13) | O36B—Mo11—O29C | 83.51 (12) |
O6C—Pt1—O3C | 177.87 (12) | O47T—Mo11—O30C | 165.79 (14) |
O2C—Pt1—O3C | 83.17 (13) | O48T—Mo11—O30C | 86.13 (14) |
O1C—Pt1—O4C | 178.01 (12) | O35B—Mo11—O30C | 85.13 (12) |
O6C—Pt1—O4C | 95.27 (13) | O36B—Mo11—O30C | 72.13 (12) |
O2C—Pt1—O4C | 97.15 (13) | O29C—Mo11—O30C | 72.11 (11) |
O3C—Pt1—O4C | 83.22 (13) | O47T—Mo11—Mo10 | 90.36 (11) |
O1C—Pt1—O5C | 97.43 (12) | O48T—Mo11—Mo10 | 131.02 (11) |
O6C—Pt1—O5C | 82.98 (13) | O35B—Mo11—Mo10 | 35.77 (9) |
O2C—Pt1—O5C | 178.47 (12) | O36B—Mo11—Mo10 | 126.38 (9) |
O3C—Pt1—O5C | 95.32 (13) | O29C—Mo11—Mo10 | 42.87 (8) |
O4C—Pt1—O5C | 82.39 (13) | O30C—Mo11—Mo10 | 87.77 (7) |
O1C—Pt1—Mo1 | 40.13 (8) | O37T—Mo12—O38T | 105.28 (16) |
O6C—Pt1—Mo1 | 93.90 (9) | O37T—Mo12—O36B | 102.09 (16) |
O2C—Pt1—Mo1 | 43.18 (9) | O38T—Mo12—O36B | 102.12 (15) |
O3C—Pt1—Mo1 | 88.22 (9) | O37T—Mo12—O25C | 95.72 (14) |
O4C—Pt1—Mo1 | 140.25 (9) | O38T—Mo12—O25C | 152.97 (13) |
O5C—Pt1—Mo1 | 137.18 (9) | O36B—Mo12—O25C | 89.63 (12) |
O29C—Pt2—O25C | 97.99 (13) | O37T—Mo12—O31B | 97.63 (15) |
O29C—Pt2—O30C | 83.50 (13) | O38T—Mo12—O31B | 88.31 (14) |
O25C—Pt2—O30C | 83.64 (12) | O36B—Mo12—O31B | 154.25 (13) |
O29C—Pt2—O26C | 177.72 (12) | O25C—Mo12—O31B | 71.95 (12) |
O25C—Pt2—O26C | 81.67 (12) | O37T—Mo12—O30C | 168.56 (14) |
O30C—Pt2—O26C | 98.68 (13) | O38T—Mo12—O30C | 86.14 (14) |
O29C—Pt2—O28C | 82.62 (13) | O36B—Mo12—O30C | 74.22 (12) |
O25C—Pt2—O28C | 178.26 (11) | O25C—Mo12—O30C | 73.62 (11) |
O30C—Pt2—O28C | 98.06 (13) | O31B—Mo12—O30C | 83.21 (12) |
O26C—Pt2—O28C | 97.66 (13) | O24T—Na1—O6W | 169.39 (16) |
O29C—Pt2—O27C | 95.84 (13) | O24T—Na1—O2W | 91.74 (14) |
O25C—Pt2—O27C | 96.06 (12) | O6W—Na1—O2W | 90.55 (14) |
O30C—Pt2—O27C | 179.23 (13) | O24T—Na1—O1W | 87.12 (14) |
O26C—Pt2—O27C | 81.97 (13) | O6W—Na1—O1W | 91.11 (14) |
O28C—Pt2—O27C | 82.25 (12) | O2W—Na1—O1W | 176.82 (17) |
O15T—Mo1—O16T | 105.41 (15) | O24T—Na1—O19W | 99.77 (14) |
O15T—Mo1—O8B | 100.56 (15) | O6W—Na1—O19W | 90.84 (14) |
O16T—Mo1—O8B | 101.85 (15) | O2W—Na1—O19W | 79.87 (14) |
O15T—Mo1—O7B | 95.79 (15) | O1W—Na1—O19W | 97.40 (15) |
O16T—Mo1—O7B | 88.94 (15) | O24T—Na1—O13Ti | 82.35 (14) |
O8B—Mo1—O7B | 157.14 (13) | O6W—Na1—O13Ti | 87.56 (14) |
O15T—Mo1—O1C | 91.61 (14) | O2W—Na1—O13Ti | 84.58 (13) |
O16T—Mo1—O1C | 155.61 (13) | O1W—Na1—O13Ti | 98.20 (14) |
O8B—Mo1—O1C | 91.78 (13) | O19W—Na1—O13Ti | 164.35 (15) |
O7B—Mo1—O1C | 71.77 (12) | O15Ti—Na2—O7W | 91.66 (14) |
O15T—Mo1—O2C | 165.40 (14) | O15Ti—Na2—O6W | 95.56 (13) |
O16T—Mo1—O2C | 89.18 (14) | O7W—Na2—O6W | 91.55 (14) |
O8B—Mo1—O2C | 75.40 (12) | O15Ti—Na2—O15W | 171.51 (15) |
O7B—Mo1—O2C | 84.78 (13) | O7W—Na2—O15W | 96.52 (14) |
O1C—Mo1—O2C | 74.66 (11) | O6W—Na2—O15W | 82.00 (13) |
O15T—Mo1—Pt1 | 128.03 (11) | O15Ti—Na2—O8W | 92.83 (13) |
O16T—Mo1—Pt1 | 125.74 (11) | O7W—Na2—O8W | 90.84 (14) |
O8B—Mo1—Pt1 | 79.21 (9) | O6W—Na2—O8W | 171.21 (15) |
O7B—Mo1—Pt1 | 78.14 (9) | O15W—Na2—O8W | 89.33 (13) |
O1C—Mo1—Pt1 | 37.08 (8) | O15Ti—Na2—O2W | 91.24 (14) |
O2C—Mo1—Pt1 | 37.78 (8) | O7W—Na2—O2W | 177.09 (15) |
O18T—Mo2—O17T | 105.58 (15) | O6W—Na2—O2W | 88.28 (14) |
O18T—Mo2—O9B | 100.97 (15) | O15W—Na2—O2W | 80.57 (14) |
O17T—Mo2—O9B | 99.27 (14) | O8W—Na2—O2W | 88.91 (14) |
O18T—Mo2—O8B | 95.89 (15) | O4Wii—Na3—O3W | 174.07 (17) |
O17T—Mo2—O8B | 99.65 (14) | O4Wii—Na3—O20T | 87.99 (15) |
O9B—Mo2—O8B | 150.17 (13) | O3W—Na3—O20T | 87.55 (14) |
O18T—Mo2—O3C | 88.95 (14) | O4Wii—Na3—O21Tiii | 103.88 (16) |
O17T—Mo2—O3C | 164.86 (13) | O3W—Na3—O21Tiii | 80.97 (14) |
O9B—Mo2—O3C | 73.24 (12) | O20T—Na3—O21Tiii | 166.84 (15) |
O8B—Mo2—O3C | 82.72 (12) | O4Wii—Na3—O13W | 86.52 (14) |
O18T—Mo2—O2C | 158.87 (14) | O3W—Na3—O13W | 96.38 (14) |
O17T—Mo2—O2C | 94.25 (14) | O20T—Na3—O13W | 78.05 (13) |
O9B—Mo2—O2C | 82.57 (13) | O21Tiii—Na3—O13W | 96.75 (14) |
O8B—Mo2—O2C | 73.23 (12) | O4Wii—Na3—O3Wiii | 87.20 (14) |
O3C—Mo2—O2C | 71.99 (11) | O3W—Na3—O3Wiii | 89.82 (14) |
O20T—Mo3—O19T | 106.27 (17) | O20T—Na3—O3Wiii | 101.04 (14) |
O20T—Mo3—O10B | 101.86 (15) | O21Tiii—Na3—O3Wiii | 85.43 (14) |
O19T—Mo3—O10B | 99.45 (15) | O13W—Na3—O3Wiii | 173.68 (16) |
O20T—Mo3—O9B | 97.79 (15) | O4Wii—Na4—O42Tiv | 156.09 (16) |
O19T—Mo3—O9B | 100.12 (15) | O4Wii—Na4—O9Wii | 92.04 (16) |
O10B—Mo3—O9B | 147.01 (13) | O42Tiv—Na4—O9Wii | 102.56 (15) |
O20T—Mo3—O4C | 91.34 (15) | O4Wii—Na4—O10Wv | 83.94 (16) |
O19T—Mo3—O4C | 161.54 (14) | O42Tiv—Na4—O10Wv | 85.19 (15) |
O10B—Mo3—O4C | 70.87 (12) | O9Wii—Na4—O10Wv | 167.83 (18) |
O9B—Mo3—O4C | 82.51 (13) | O4Wii—Na4—O13W | 83.45 (14) |
O20T—Mo3—O3C | 159.41 (15) | O42Tiv—Na4—O13W | 78.16 (13) |
O19T—Mo3—O3C | 92.80 (14) | O9Wii—Na4—O13W | 88.64 (15) |
O10B—Mo3—O3C | 82.12 (12) | O10Wv—Na4—O13W | 102.26 (16) |
O9B—Mo3—O3C | 70.67 (12) | O4Wii—Na4—O11Wii | 123.93 (15) |
O4C—Mo3—O3C | 70.67 (11) | O42Tiv—Na4—O11Wii | 74.82 (13) |
O21T—Mo4—O22T | 106.64 (17) | O9Wii—Na4—O11Wii | 92.35 (14) |
O21T—Mo4—O11B | 97.82 (16) | O10Wv—Na4—O11Wii | 80.51 (15) |
O22T—Mo4—O11B | 102.09 (15) | O13W—Na4—O11Wii | 152.51 (14) |
O21T—Mo4—O10B | 101.48 (15) | O18Wvi—Na5—O41T | 169.60 (16) |
O22T—Mo4—O10B | 96.38 (15) | O18Wvi—Na5—O12Wvii | 106.16 (18) |
O11B—Mo4—O10B | 148.14 (13) | O41T—Na5—O12Wvii | 81.20 (16) |
O21T—Mo4—O4C | 93.57 (15) | O18Wvi—Na5—O39Tiv | 92.76 (15) |
O22T—Mo4—O4C | 157.85 (14) | O41T—Na5—O39Tiv | 79.54 (14) |
O11B—Mo4—O4C | 83.58 (13) | O12Wvii—Na5—O39Tiv | 91.39 (15) |
O10B—Mo4—O4C | 70.20 (12) | O18Wvi—Na5—O17W | 93.24 (15) |
O21T—Mo4—O5C | 161.20 (15) | O41T—Na5—O17W | 80.61 (13) |
O22T—Mo4—O5C | 90.59 (14) | O12Wvii—Na5—O17W | 159.22 (19) |
O11B—Mo4—O5C | 70.61 (12) | O39Tiv—Na5—O17W | 95.08 (14) |
O10B—Mo4—O5C | 83.57 (12) | O18Wvi—Na5—O14Wvii | 97.57 (14) |
O4C—Mo4—O5C | 70.91 (11) | O41T—Na5—O14Wvii | 90.15 (14) |
O24T—Mo5—O23T | 106.92 (18) | O12Wvii—Na5—O14Wvii | 86.13 (15) |
O24T—Mo5—O11B | 97.36 (16) | O39Tiv—Na5—O14Wvii | 169.66 (15) |
O23T—Mo5—O11B | 101.02 (16) | O17W—Na5—O14Wvii | 83.98 (13) |
O24T—Mo5—O12B | 101.20 (15) | O45Tviii—Na6—O16Wvii | 84.88 (15) |
O23T—Mo5—O12B | 99.38 (15) | O45Tviii—Na6—O5W | 94.17 (14) |
O11B—Mo5—O12B | 146.97 (13) | O16Wvii—Na6—O5W | 177.0 (2) |
O24T—Mo5—O5C | 157.91 (15) | O45Tviii—Na6—O44T | 171.00 (16) |
O23T—Mo5—O5C | 93.95 (15) | O16Wvii—Na6—O44T | 97.15 (15) |
O11B—Mo5—O5C | 71.01 (12) | O5W—Na6—O44T | 83.36 (14) |
O12B—Mo5—O5C | 81.93 (12) | O45Tviii—Na6—O5Wviii | 86.65 (14) |
O24T—Mo5—O6C | 90.40 (15) | O16Wvii—Na6—O5Wviii | 93.72 (18) |
O23T—Mo5—O6C | 161.60 (15) | O5W—Na6—O5Wviii | 83.36 (15) |
O11B—Mo5—O6C | 82.37 (12) | O44T—Na6—O5Wviii | 84.47 (14) |
O12B—Mo5—O6C | 70.49 (12) | O45Tviii—Na6—O20Wvii | 101.56 (18) |
O5C—Mo5—O6C | 69.85 (11) | O16Wvii—Na6—O20Wvii | 81.7 (2) |
O13T—Mo6—O14T | 107.19 (18) | O5W—Na6—O20Wvii | 101.3 (2) |
O13T—Mo6—O12B | 100.66 (15) | O44T—Na6—O20Wvii | 87.42 (18) |
O14T—Mo6—O12B | 103.65 (15) | O5Wviii—Na6—O20Wvii | 170.2 (2) |
O13T—Mo6—O7B | 98.18 (15) | Pt1—O1C—Mo1 | 102.79 (13) |
O14T—Mo6—O7B | 90.40 (15) | Pt1—O1C—Mo6 | 104.47 (13) |
O12B—Mo6—O7B | 151.86 (13) | Pt1—O2C—Mo1 | 99.04 (13) |
O13T—Mo6—O1C | 93.47 (15) | Pt1—O2C—Mo2 | 102.52 (14) |
O14T—Mo6—O1C | 153.85 (15) | Pt1—O2C—O30C | 116.35 (16) |
O12B—Mo6—O1C | 87.60 (12) | Pt1—O3C—Mo2 | 102.31 (13) |
O7B—Mo6—O1C | 70.51 (12) | Pt1—O3C—Mo3 | 102.23 (13) |
O13T—Mo6—O6C | 163.39 (15) | Pt1—O4C—Mo3 | 103.81 (13) |
O14T—Mo6—O6C | 89.30 (15) | Pt1—O4C—Mo4 | 104.05 (13) |
O12B—Mo6—O6C | 72.79 (12) | Pt1—O5C—Mo5 | 104.17 (14) |
O7B—Mo6—O6C | 83.29 (12) | Pt1—O5C—Mo4 | 102.66 (13) |
O1C—Mo6—O6C | 71.32 (11) | Pt1—O6C—Mo6 | 101.23 (13) |
O39T—Mo7—O40T | 107.31 (19) | Pt1—O6C—Mo5 | 103.00 (13) |
O39T—Mo7—O32B | 101.06 (15) | Pt2—O25C—Mo12 | 105.47 (13) |
O40T—Mo7—O32B | 104.07 (15) | Pt2—O25C—Mo7 | 105.62 (13) |
O39T—Mo7—O31B | 97.15 (15) | Mo1—O2C—O30C | 122.10 (17) |
O40T—Mo7—O31B | 89.78 (15) | Mo2—O2C—O30C | 119.13 (16) |
O32B—Mo7—O31B | 152.51 (13) | Pt2—O26C—Mo7 | 101.33 (13) |
O39T—Mo7—O25C | 93.78 (15) | Pt2—O26C—Mo8 | 103.45 (13) |
O40T—Mo7—O25C | 152.78 (15) | Pt2—O27C—Mo8 | 104.35 (13) |
O32B—Mo7—O25C | 88.06 (13) | Pt2—O27C—Mo9 | 103.89 (13) |
O31B—Mo7—O25C | 70.25 (12) | Pt2—O28C—Mo10 | 100.58 (13) |
O39T—Mo7—O26C | 163.50 (15) | Pt2—O28C—Mo9 | 103.89 (13) |
O40T—Mo7—O26C | 89.09 (15) | Pt2—O29C—Mo11 | 106.63 (14) |
O32B—Mo7—O26C | 72.35 (12) | Pt2—O29C—Mo10 | 105.30 (13) |
O31B—Mo7—O26C | 84.45 (12) | Pt2—O30C—Mo12 | 96.59 (13) |
O25C—Mo7—O26C | 71.22 (11) | Pt2—O30C—Mo11 | 97.72 (13) |
O42T—Mo8—O41T | 107.11 (17) | Pt2—O30C—O2C | 117.78 (16) |
O42T—Mo8—O32B | 98.16 (15) | Mo12—O30C—O2C | 124.51 (17) |
O41T—Mo8—O32B | 102.73 (15) | Mo11—O30C—O2C | 122.82 (16) |
O42T—Mo8—O33B | 99.95 (15) | H1A—O1W—H1B | 109 (4) |
O41T—Mo8—O33B | 96.08 (15) | H2A—O2W—H2B | 104 (3) |
O32B—Mo8—O33B | 148.67 (13) | H3A—O3W—H3B | 110 (4) |
O42T—Mo8—O27C | 93.34 (14) | H4A—O4W—H4B | 110 (4) |
O41T—Mo8—O27C | 157.72 (15) | H5A—O5W—H5B | 111 (4) |
O32B—Mo8—O27C | 82.48 (12) | H6A—O6W—H6B | 107 (3) |
O33B—Mo8—O27C | 71.16 (12) | H7A—O7W—H7B | 112 (4) |
O42T—Mo8—O26C | 161.29 (14) | H8A—O8W—H8B | 105 (3) |
O41T—Mo8—O26C | 90.66 (15) | H9A—O9W—H9B | 113 (4) |
O32B—Mo8—O26C | 71.58 (12) | H10A—O10W—H10B | 112 (4) |
O33B—Mo8—O26C | 83.51 (12) | H11A—O11W—H11B | 111 (4) |
O27C—Mo8—O26C | 70.22 (11) | H12A—O12W—H12B | 109.5 |
O44T—Mo9—O43T | 105.42 (16) | H13A—O13W—H13B | 110.8 |
O44T—Mo9—O34B | 101.22 (15) | H14A—O14W—H14B | 109.5 |
O43T—Mo9—O34B | 97.29 (15) | H15A—O15W—H15B | 115 (4) |
O44T—Mo9—O33B | 98.74 (15) | H16A—O16W—H16B | 105 (4) |
O43T—Mo9—O33B | 101.57 (15) | H17A—O17W—H17B | 115 (4) |
O34B—Mo9—O33B | 147.68 (13) | H18A—O18W—H18B | 112 (4) |
O44T—Mo9—O27C | 159.33 (14) | H19A—O19W—H19B | 112 (4) |
O43T—Mo9—O27C | 94.36 (14) | H20A—O20W—H20B | 111 (5) |
O34B—Mo9—O27C | 81.75 (12) | H21A—O21W—H21B | 105 (4) |
O33B—Mo9—O27C | 70.92 (12) | H22A—O22W—H22B | 108 (4) |
O44T—Mo9—O28C | 91.45 (14) | H23A—O23W—H23B | 106 (4) |
O43T—Mo9—O28C | 161.38 (14) | H24A—O24W—H24B | 108 (4) |
O34B—Mo9—O28C | 71.21 (12) | H25A—O25W—H25B | 111 (4) |
O33B—Mo9—O28C | 83.19 (12) | H26A—O26W—H26B | 107 (4) |
O27C—Mo9—O28C | 69.96 (11) | H27A—O27W—H27B | 109 (4) |
O46T—Mo10—O45T | 106.66 (18) | H28A—O28W—H28B | 107 (4) |
O46T—Mo10—O34B | 97.33 (15) | H29A—O29W—H29B | 110 (4) |
O45T—Mo10—O34B | 99.56 (15) |
Symmetry codes: (i) −x+1, −y+1, −z+1; (ii) x, y+1, z; (iii) −x, −y+2, −z+1; (iv) −x, −y+2, −z; (v) x−1, y+1, z; (vi) x, y+1, z−1; (vii) x, y, z−1; (viii) −x+1, −y+1, −z; (ix) x, y−1, z; (x) x+1, y−1, z; (xi) x, y, z+1; (xii) x, y−1, z+1. |
D—H···A | D—H | H···A | D···A | D—H···A |
O2C—H2···O30C | 0.86 (3) | 1.84 (6) | 2.595 (5) | 145 (9) |
O3C—H3···O14Wxiii | 0.86 (3) | 1.74 (3) | 2.586 (5) | 164 (4) |
O4C—H4···O38T | 0.85 (3) | 1.72 (3) | 2.576 (4) | 178 (5) |
O5C—H5···O29W | 0.86 (3) | 1.79 (3) | 2.595 (5) | 156 (5) |
O6C—H6···O48T | 0.86 (3) | 1.72 (3) | 2.569 (4) | 171 (5) |
O7B—H7···O35B | 0.84 (3) | 1.94 (3) | 2.785 (5) | 175 (5) |
O26C—H26···O17T | 0.82 (3) | 1.73 (3) | 2.556 (4) | 178 (5) |
O27C—H27···O15Wxiv | 0.87 (3) | 1.70 (3) | 2.548 (5) | 164 (5) |
O28C—H28···O16T | 0.86 (3) | 1.73 (3) | 2.575 (4) | 166 (5) |
O30C—H30···O2C | 0.84 (3) | 1.76 (3) | 2.595 (5) | 172 (9) |
O31B—H31···O9B | 0.82 (3) | 1.95 (3) | 2.763 (4) | 171 (5) |
O1W—H1A···O36Bxiv | 0.87 (3) | 1.96 (3) | 2.830 (5) | 173 (5) |
O1W—H1B···O48T | 0.84 (3) | 2.22 (3) | 3.023 (5) | 161 (5) |
O2W—H2A···O16W | 0.86 (3) | 1.87 (3) | 2.731 (6) | 175 (5) |
O2W—H2B···O43Txi | 0.87 (3) | 2.17 (3) | 3.031 (5) | 169 (5) |
O3W—H3A···O22W | 0.87 (3) | 2.10 (3) | 2.969 (6) | 175 (5) |
O3W—H3B···O38T | 0.86 (3) | 2.13 (3) | 2.980 (5) | 176 (5) |
O4W—H4A···O26W | 0.88 (3) | 1.98 (3) | 2.857 (6) | 175 (5) |
O4W—H4B···O25W | 0.82 (3) | 1.99 (3) | 2.806 (6) | 176 (6) |
O5W—H5A···O16T | 0.85 (3) | 2.08 (3) | 2.930 (5) | 178 (6) |
O6W—H6A···O25Cxiv | 0.86 (3) | 2.04 (3) | 2.880 (5) | 167 (5) |
O6W—H6B···O18W | 0.87 (3) | 1.97 (3) | 2.831 (6) | 173 (5) |
O7W—H7A···O17Wxii | 0.82 (3) | 1.98 (3) | 2.804 (5) | 175 (6) |
O7W—H7B···O32Bxiv | 0.82 (3) | 2.02 (3) | 2.842 (5) | 174 (5) |
O8W—H8A···O34Bxi | 0.87 (3) | 2.21 (3) | 3.064 (5) | 168 (5) |
O8W—H8B···O9Wxi | 0.87 (3) | 1.89 (3) | 2.750 (6) | 169 (5) |
O9W—H9A···O19Tix | 0.83 (3) | 2.22 (3) | 3.046 (5) | 178 (5) |
O9W—H9B···O7Wvii | 0.86 (3) | 1.91 (3) | 2.720 (5) | 156 (6) |
O10W—H10A···O25Wxv | 0.84 (3) | 2.23 (4) | 2.924 (7) | 140 (5) |
O10W—H10B···O21Wi | 0.86 (3) | 2.02 (3) | 2.874 (7) | 174 (7) |
O11W—H11A···O34B | 0.85 (3) | 1.93 (3) | 2.723 (5) | 155 (5) |
O11W—H11B···O43Txvi | 0.85 (3) | 2.08 (3) | 2.867 (5) | 154 (5) |
O12W—H12A···O22T | 0.98 | 2.25 | 2.904 (5) | 123 |
O12W—H12A···O21W | 0.98 | 2.31 | 3.141 (8) | 142 |
O13W—H13A···O12Wiii | 0.99 | 1.80 | 2.766 (6) | 164 |
O13W—H13B···O31B | 0.99 | 2.53 | 3.396 (5) | 146 |
O14W—H14A···O27Wxi | 0.98 | 1.76 | 2.737 (6) | 177 |
O14W—H14B···O23W | 0.98 | 1.96 | 2.796 (6) | 142 |
O15W—H15A···O19W | 0.83 (3) | 1.97 (3) | 2.738 (5) | 154 (5) |
O16W—H16A···O20W | 0.89 (3) | 2.45 (6) | 3.156 (7) | 137 (7) |
O16W—H16B···O24Wi | 0.85 (3) | 2.17 (6) | 2.842 (6) | 136 (6) |
O17W—H17A···O8Bxvii | 0.81 (3) | 1.98 (3) | 2.790 (5) | 173 (5) |
O17W—H17B···O17T | 0.84 (3) | 2.22 (3) | 3.027 (5) | 160 (5) |
O18W—H18A···O28W | 0.83 (3) | 2.18 (4) | 2.907 (5) | 146 (5) |
O18W—H18B···O1Ci | 0.81 (3) | 1.99 (3) | 2.798 (5) | 176 (5) |
O19W—H19A···O29Cxiv | 0.85 (3) | 2.01 (3) | 2.842 (5) | 164 (5) |
O19W—H19B···O10Wi | 0.80 (3) | 2.14 (3) | 2.920 (6) | 164 (6) |
O20W—H20B···O23W | 0.85 (3) | 2.46 (7) | 3.121 (8) | 135 (8) |
O21W—H21A···O23T | 0.89 (3) | 2.24 (4) | 3.064 (6) | 155 (7) |
O21W—H21B···O33Bxi | 0.86 (3) | 2.17 (3) | 2.972 (5) | 155 (6) |
O22W—H22A···O28Wxiv | 0.88 (3) | 2.28 (5) | 3.007 (6) | 140 (5) |
O22W—H22B···O26Wxiv | 0.85 (3) | 1.96 (3) | 2.805 (7) | 169 (6) |
O23W—H23A···O22T | 0.87 (3) | 2.30 (5) | 2.970 (6) | 134 (6) |
O23W—H23B···O10Bxiii | 0.85 (3) | 1.95 (3) | 2.775 (5) | 162 (7) |
O24W—H24A···O28W | 0.84 (3) | 2.02 (3) | 2.854 (6) | 173 (6) |
O24W—H24B···O35B | 0.89 (3) | 2.05 (3) | 2.911 (5) | 163 (5) |
O25W—H25A···O38Txiv | 0.83 (3) | 2.52 (6) | 3.119 (6) | 130 (7) |
O25W—H25B···O47T | 0.86 (3) | 2.01 (3) | 2.834 (5) | 161 (7) |
O26W—H26A···O24W | 0.87 (3) | 1.93 (5) | 2.723 (6) | 150 (7) |
O26W—H26B···O19Tix | 0.87 (3) | 2.23 (4) | 2.920 (5) | 135 (5) |
O27W—H27A···O18Txvii | 0.86 (3) | 2.33 (5) | 2.945 (5) | 129 (5) |
O27W—H27B···O33B | 0.87 (3) | 2.10 (4) | 2.846 (5) | 144 (5) |
O28W—H28A···O12Bi | 0.86 (3) | 1.93 (3) | 2.775 (5) | 168 (6) |
O28W—H28B···O1W | 0.86 (3) | 1.96 (3) | 2.817 (6) | 171 (6) |
O29W—H29A···O22Txiii | 0.86 (3) | 2.26 (5) | 2.895 (5) | 131 (5) |
O29W—H29B···O22Wxv | 0.84 (3) | 2.03 (3) | 2.844 (6) | 165 (7) |
Symmetry codes: (i) −x+1, −y+1, −z+1; (iii) −x, −y+2, −z+1; (vii) x, y, z−1; (ix) x, y−1, z; (xi) x, y, z+1; (xii) x, y−1, z+1; (xiii) −x+1, −y+2, −z+1; (xiv) −x, −y+1, −z+1; (xv) x+1, y, z; (xvi) −x, −y+1, −z; (xvii) −x+1, −y+2, −z. |
Mo1—O1C | 2.114 (3) | Mo1—O7B | 2.098 (3) |
Mo6—O1C | 2.198 (3) | Mo6—O7B | 2.076 (3) |
Mo1—O2C | 2.216 (3) | Mo1—O8B | 1.883 (3) |
Mo2—O2C | 2.246 (3) | Mo2—O8B | 1.963 (3) |
Mo2—O3C | 2.245 (3) | Mo2—O9B | 1.924 (3) |
Mo3—O3C | 2.336 (3) | Mo3—O9B | 1.953 (3) |
Mo3—O4C | 2.267 (3) | Mo3—O10B | 1.927 (3) |
Mo4—O4C | 2.283 (3) | Mo4—O10B | 1.947 (3) |
Mo4—O5C | 2.312 (3) | Mo4—O11B | 1.916 (3) |
Mo5—O5C | 2.280 (3) | Mo5—O11B | 1.935 (3) |
Mo5—O6C | 2.358 (3) | Mo5—O12B | 1.947 (3) |
Mo6—O6C | 2.287 (3) | Mo6—O12B | 1.906 (3) |
Mo7—O25C | 2.186 (3) | Mo7—O31B | 2.072 (3) |
Mo12—O25C | 2.084 (3) | Mo12—O31B | 2.090 (3) |
Mo7—O26C | 2.297 (3) | Mo7—O32B | 1.899 (3) |
Mo8—O26C | 2.305 (3) | Mo8—O32B | 1.935 (3) |
Mo8—O27C | 2.272 (3) | Mo8—O33B | 1.959 (3) |
Mo9—O27C | 2.302 (3) | Mo9—O33B | 1.932 (3) |
Mo9—O28C | 2.307 (3) | Mo9—O34B | 1.925 (3) |
Mo10—O28C | 2.302 (3) | Mo10—O34B | 1.961 (3) |
Mo10—O29C | 2.196 (3) | Mo10—O35B | 1.988 (3) |
Mo11—O29C | 2.122 (3) | Mo11—O35B | 1.947 (3) |
Mo11—O30C | 2.359 (3) | Mo11—O36B | 1.970 (3) |
Mo12—O30C | 2.340 (3) | Mo12—O36B | 1.870 (3) |
Mo1—O1C—Mo6 | 104.42 (13) | Mo12—O25C—Mo7 | 104.38 (13) |
Mo1—O2C—Mo2 | 93.27 (12) | Mo7—O26C—Mo8 | 92.23 (11) |
Mo2—O3C—Mo3 | 92.61 (11) | Mo8—O27C—Mo9 | 93.67 (11) |
Mo3—O4C—Mo4 | 94.36 (12) | Mo10—O28C—Mo9 | 93.85 (11) |
Mo5—O5C—Mo4 | 93.05 (11) | Mo11—O29C—Mo10 | 96.01 (12) |
Mo6—O6C—Mo5 | 91.98 (11) | Mo12—O30C—Mo11 | 90.63 (11) |
Mo6—O7B—Mo1 | 109.51 (15) | Mo7—O31B—Mo12 | 108.35 (15) |
Mo1—O8B—Mo2 | 115.01 (15) | Mo7—O32B—Mo8 | 119.84 (16) |
Mo2—O9B—Mo3 | 117.38 (16) | Mo9—O33B—Mo8 | 118.01 (15) |
Mo3—O10B—Mo4 | 118.97 (16) | Mo9—O34B—Mo10 | 120.01 (16) |
Mo4—O11B—Mo5 | 119.86 (16) | Mo11—O35B—Mo10 | 109.31 (15) |
Mo6—O12B—Mo5 | 120.24 (16) | Mo12—O36B—Mo11 | 120.93 (15) |
D—H···A | D—H | H···A | D···A | D—H···A |
O2C—H2···O30C | 0.86 (3) | 1.84 (6) | 2.595 (5) | 145 (9) |
O3C—H3···O14Wi | 0.86 (3) | 1.74 (3) | 2.586 (5) | 164 (4) |
O4C—H4···O38T | 0.85 (3) | 1.72 (3) | 2.576 (4) | 178 (5) |
O5C—H5···O29W | 0.86 (3) | 1.79 (3) | 2.595 (5) | 156 (5) |
O6C—H6···O48T | 0.86 (3) | 1.72 (3) | 2.569 (4) | 171 (5) |
O7B—H7···O35B | 0.84 (3) | 1.94 (3) | 2.785 (5) | 175 (5) |
O26C—H26···O17T | 0.82 (3) | 1.73 (3) | 2.556 (4) | 178 (5) |
O27C—H27···O15Wii | 0.87 (3) | 1.70 (3) | 2.548 (5) | 164 (5) |
O28C—H28···O16T | 0.86 (3) | 1.73 (3) | 2.575 (4) | 166 (5) |
O30C—H30···O2C | 0.84 (3) | 1.76 (3) | 2.595 (5) | 172 (9) |
O31B—H31···O9B | 0.82 (3) | 1.95 (3) | 2.763 (4) | 171 (5) |
O1W—H1A···O36Bii | 0.87 (3) | 1.96 (3) | 2.830 (5) | 173 (5) |
O1W—H1B···O48T | 0.84 (3) | 2.22 (3) | 3.023 (5) | 161 (5) |
O2W—H2A···O16W | 0.86 (3) | 1.87 (3) | 2.731 (6) | 175 (5) |
O2W—H2B···O43Tiii | 0.87 (3) | 2.17 (3) | 3.031 (5) | 169 (5) |
O3W—H3A···O22W | 0.87 (3) | 2.10 (3) | 2.969 (6) | 175 (5) |
O3W—H3B···O38T | 0.86 (3) | 2.13 (3) | 2.980 (5) | 176 (5) |
O4W—H4A···O26W | 0.88 (3) | 1.98 (3) | 2.857 (6) | 175 (5) |
O4W—H4B···O25W | 0.82 (3) | 1.99 (3) | 2.806 (6) | 176 (6) |
O5W—H5A···O16T | 0.85 (3) | 2.08 (3) | 2.930 (5) | 178 (6) |
O6W—H6A···O25Cii | 0.86 (3) | 2.04 (3) | 2.880 (5) | 167 (5) |
O6W—H6B···O18W | 0.87 (3) | 1.97 (3) | 2.831 (6) | 173 (5) |
O7W—H7A···O17Wiv | 0.82 (3) | 1.98 (3) | 2.804 (5) | 175 (6) |
O7W—H7B···O32Bii | 0.82 (3) | 2.02 (3) | 2.842 (5) | 174 (5) |
O8W—H8A···O34Biii | 0.87 (3) | 2.21 (3) | 3.064 (5) | 168 (5) |
O8W—H8B···O9Wiii | 0.87 (3) | 1.89 (3) | 2.750 (6) | 169 (5) |
O9W—H9A···O19Tv | 0.83 (3) | 2.22 (3) | 3.046 (5) | 178 (5) |
O9W—H9B···O7Wvi | 0.86 (3) | 1.91 (3) | 2.720 (5) | 156 (6) |
O10W—H10A···O25Wvii | 0.84 (3) | 2.23 (4) | 2.924 (7) | 140 (5) |
O10W—H10B···O21Wviii | 0.86 (3) | 2.02 (3) | 2.874 (7) | 174 (7) |
O11W—H11A···O34B | 0.85 (3) | 1.93 (3) | 2.723 (5) | 155 (5) |
O11W—H11B···O43Tix | 0.85 (3) | 2.08 (3) | 2.867 (5) | 154 (5) |
O12W—H12A···O22T | 0.98 | 2.25 | 2.904 (5) | 123.4 |
O12W—H12A···O21W | 0.98 | 2.31 | 3.141 (8) | 142.4 |
O13W—H13A···O12Wx | 0.99 | 1.80 | 2.766 (6) | 164.3 |
O13W—H13B···O31B | 0.99 | 2.53 | 3.396 (5) | 146.2 |
O14W—H14A···O27Wiii | 0.98 | 1.76 | 2.737 (6) | 176.5 |
O14W—H14B···O23W | 0.98 | 1.96 | 2.796 (6) | 141.6 |
O15W—H15A···O19W | 0.83 (3) | 1.97 (3) | 2.738 (5) | 154 (5) |
O16W—H16A···O20W | 0.89 (3) | 2.45 (6) | 3.156 (7) | 137 (7) |
O16W—H16B···O24Wviii | 0.85 (3) | 2.17 (6) | 2.842 (6) | 136 (6) |
O17W—H17A···O8Bxi | 0.81 (3) | 1.98 (3) | 2.790 (5) | 173 (5) |
O17W—H17B···O17T | 0.84 (3) | 2.22 (3) | 3.027 (5) | 160 (5) |
O18W—H18A···O28W | 0.83 (3) | 2.18 (4) | 2.907 (5) | 146 (5) |
O18W—H18B···O1Cviii | 0.81 (3) | 1.99 (3) | 2.798 (5) | 176 (5) |
O19W—H19A···O29Cii | 0.85 (3) | 2.01 (3) | 2.842 (5) | 164 (5) |
O19W—H19B···O10Wviii | 0.80 (3) | 2.14 (3) | 2.920 (6) | 164 (6) |
O20W—H20B···O23W | 0.85 (3) | 2.46 (7) | 3.121 (8) | 135 (8) |
O21W—H21A···O23T | 0.89 (3) | 2.24 (4) | 3.064 (6) | 155 (7) |
O21W—H21B···O33Biii | 0.86 (3) | 2.17 (3) | 2.972 (5) | 155 (6) |
O22W—H22A···O28Wii | 0.88 (3) | 2.28 (5) | 3.007 (6) | 140 (5) |
O22W—H22B···O26Wii | 0.85 (3) | 1.96 (3) | 2.805 (7) | 169 (6) |
O23W—H23A···O22T | 0.87 (3) | 2.30 (5) | 2.970 (6) | 134 (6) |
O23W—H23B···O10Bi | 0.85 (3) | 1.95 (3) | 2.775 (5) | 162 (7) |
O24W—H24A···O28W | 0.84 (3) | 2.02 (3) | 2.854 (6) | 173 (6) |
O24W—H24B···O35B | 0.89 (3) | 2.05 (3) | 2.911 (5) | 163 (5) |
O25W—H25A···O38Tii | 0.83 (3) | 2.52 (6) | 3.119 (6) | 130 (7) |
O25W—H25B···O47T | 0.86 (3) | 2.01 (3) | 2.834 (5) | 161 (7) |
O26W—H26A···O24W | 0.87 (3) | 1.93 (5) | 2.723 (6) | 150 (7) |
O26W—H26B···O19Tv | 0.87 (3) | 2.23 (4) | 2.920 (5) | 135 (5) |
O27W—H27A···O18Txi | 0.86 (3) | 2.33 (5) | 2.945 (5) | 129 (5) |
O27W—H27B···O33B | 0.87 (3) | 2.10 (4) | 2.846 (5) | 144 (5) |
O28W—H28A···O12Bviii | 0.86 (3) | 1.93 (3) | 2.775 (5) | 168 (6) |
O28W—H28B···O1W | 0.86 (3) | 1.96 (3) | 2.817 (6) | 171 (6) |
O29W—H29A···O22Ti | 0.86 (3) | 2.26 (5) | 2.895 (5) | 131 (5) |
O29W—H29B···O22Wvii | 0.84 (3) | 2.03 (3) | 2.844 (6) | 165 (7) |
Symmetry codes: (i) −x+1, −y+2, −z+1; (ii) −x, −y+1, −z+1; (iii) x, y, z+1; (iv) x, y−1, z+1; (v) x, y−1, z; (vi) x, y, z−1; (vii) x+1, y, z; (viii) −x+1, −y+1, −z+1; (ix) −x, −y+1, −z; (x) −x, −y+2, −z+1; (xi) −x+1, −y+2, −z. |
Experimental details
Crystal data | |
Chemical formula | H6Mo6O24Pt·H4Mo6O24Pt·29(H2O)·6(Na) |
Mr | 2979.85 |
Crystal system, space group | Triclinic, P1 |
Temperature (K) | 173 |
a, b, c (Å) | 14.0384 (6), 15.7969 (6), 16.7235 (6) |
α, β, γ (°) | 72.825 (2), 75.522 (2), 89.168 (2) |
V (Å3) | 3423.7 (2) |
Z | 2 |
Radiation type | Mo Kα |
µ (mm−1) | 6.36 |
Crystal size (mm) | 0.67 × 0.44 × 0.22 |
Data collection | |
Diffractometer | Bruker SMART APEXII CCD diffractometer |
Absorption correction | Multi-scan (SADABS; Bruker, 2009) |
Tmin, Tmax | 0.234, 0.746 |
No. of measured, independent and observed [I > 2σ(I)] reflections | 58415, 14940, 12688 |
Rint | 0.057 |
(sin θ/λ)max (Å−1) | 0.639 |
Refinement | |
R[F2 > 2σ(F2)], wR(F2), S | 0.036, 0.091, 1.06 |
No. of reflections | 14940 |
No. of parameters | 1064 |
No. of restraints | 114 |
H-atom treatment | Only H-atom coordinates refined |
Δρmax, Δρmin (e Å−3) | 1.73, −2.25 |
Computer programs: APEX2 (Bruker, 2009), SAINT (Bruker, 2009), SHELXS2014/7 (Sheldrick, 2008), SHELXL2014/7 (Sheldrick, 2015), ORTEP-3 for Windows (Farrugia, 2012), PLATON (Spek, 2009) and DIAMOND (Brandenburg, 1998).
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