Supporting information
Crystallographic Information File (CIF) https://doi.org/10.1107/S0108270110001393/sq3227sup1.cif | |
Structure factor file (CIF format) https://doi.org/10.1107/S0108270110001393/sq3227Isup2.hkl |
Single crystals of the title compound were prepared from a mixture of NH4VO3 (2 mmol, 0.234 g), BaCl2 (2 mmol, 0.4886 g), H3BO3 (2.5 mmol, 0.1758 g), H3PO4 (2 ml) and H2O (2 ml). The mixture was sealed in a 30 ml Teflon-lined stainless steel vessel and heated at 443 K for 6 d under autogenous pressure, then cooled to room temperature. The resulting dark-green crystals were collected and dried in air at ambient temperature.
The H atoms were located in a difference map and included in the model with O—H constrained to 0.85 Å and Uiso(H) = 1.2Ueq(O). The highest peak in the difference map is 1.63 e Å-3, 1.82 Å from atom H11, and the deepest hole is -1.2 e Å-3, 0.66 Å from atom Ba1.
Data collection: APEX2 (Bruker, 2007); cell refinement: SAINT (Bruker, 2007); data reduction: SAINT (Bruker, 2007); program(s) used to solve structure: SHELXS97 (Sheldrick, 2008); program(s) used to refine structure: SHELXL97 (Sheldrick, 2008); molecular graphics: SHELXTL (Sheldrick, 2008); software used to prepare material for publication: SHELXTL (Sheldrick, 2008).
Ba5Cl4(H2O)8(VPO5)8 | F(000) = 4208 |
Mr = 2267.91 | Dx = 3.539 Mg m−3 |
Orthorhombic, Cmca | Mo Kα radiation, λ = 0.71073 Å |
Hall symbol: -C 2bc 2 | Cell parameters from 1819 reflections |
a = 13.5073 (8) Å | θ = 2.3–27.4° |
b = 8.8803 (5) Å | µ = 6.90 mm−1 |
c = 35.482 (2) Å | T = 295 K |
V = 4256.1 (4) Å3 | Block, green |
Z = 4 | 0.20 × 0.12 × 0.12 mm |
Bruker APEXII CCD area-detector diffractometer | 1993 independent reflections |
Radiation source: fine-focus sealed tube | 1614 reflections with I > 2σ(I) |
Graphite monochromator | Rint = 0.046 |
ϕ and ω scans | θmax = 25.1°, θmin = 1.2° |
Absorption correction: multi-scan (SADABS; Bruker, 2007) | h = −16→8 |
Tmin = 0.339, Tmax = 0.492 | k = −10→10 |
10601 measured reflections | l = −42→39 |
Refinement on F2 | Primary atom site location: structure-invariant direct methods |
Least-squares matrix: full | Secondary atom site location: difference Fourier map |
R[F2 > 2σ(F2)] = 0.031 | Hydrogen site location: constr |
wR(F2) = 0.078 | H-atom parameters constrained |
S = 1.04 | w = 1/[σ2(Fo2) + (0.0283P)2 + 42.1779P] where P = (Fo2 + 2Fc2)/3 |
1993 reflections | (Δ/σ)max = 0.001 |
180 parameters | Δρmax = 1.63 e Å−3 |
0 restraints | Δρmin = −1.20 e Å−3 |
Ba5Cl4(H2O)8(VPO5)8 | V = 4256.1 (4) Å3 |
Mr = 2267.91 | Z = 4 |
Orthorhombic, Cmca | Mo Kα radiation |
a = 13.5073 (8) Å | µ = 6.90 mm−1 |
b = 8.8803 (5) Å | T = 295 K |
c = 35.482 (2) Å | 0.20 × 0.12 × 0.12 mm |
Bruker APEXII CCD area-detector diffractometer | 1993 independent reflections |
Absorption correction: multi-scan (SADABS; Bruker, 2007) | 1614 reflections with I > 2σ(I) |
Tmin = 0.339, Tmax = 0.492 | Rint = 0.046 |
10601 measured reflections |
R[F2 > 2σ(F2)] = 0.031 | 0 restraints |
wR(F2) = 0.078 | H-atom parameters constrained |
S = 1.04 | w = 1/[σ2(Fo2) + (0.0283P)2 + 42.1779P] where P = (Fo2 + 2Fc2)/3 |
1993 reflections | Δρmax = 1.63 e Å−3 |
180 parameters | Δρmin = −1.20 e Å−3 |
Geometry. All e.s.d.'s (except the e.s.d. in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell e.s.d.'s are taken into account individually in the estimation of e.s.d.'s in distances, angles and torsion angles; correlations between e.s.d.'s in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell e.s.d.'s is used for estimating e.s.d.'s involving l.s. planes. |
Refinement. 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 > σ(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. |
x | y | z | Uiso*/Ueq | ||
Ba1 | 0.0000 | 0.90019 (6) | 0.273505 (16) | 0.01910 (17) | |
Ba2 | 0.0000 | 1.11287 (6) | 0.399827 (15) | 0.01737 (16) | |
Ba3 | 0.0000 | 0.5000 | 0.5000 | 0.0212 (2) | |
V2 | −0.29225 (7) | 0.75070 (10) | 0.31245 (3) | 0.0059 (2) | |
V1 | −0.20641 (7) | 0.75085 (10) | 0.43692 (3) | 0.0060 (2) | |
Cl1 | 0.0000 | 1.2307 (2) | 0.31120 (6) | 0.0131 (4) | |
Cl2 | 0.0000 | 0.7680 (2) | 0.43684 (6) | 0.0126 (4) | |
P1 | 0.2500 | 0.9938 (2) | 0.2500 | 0.0057 (4) | |
P2 | 0.25414 (11) | 1.00478 (15) | 0.37464 (4) | 0.0066 (3) | |
P3 | −0.25119 (15) | 0.5000 | 0.5000 | 0.0051 (4) | |
O1 | −0.3239 (3) | 0.7444 (4) | 0.43569 (12) | 0.0152 (10) | |
O2 | −0.1750 (3) | 0.7565 (4) | 0.31098 (12) | 0.0143 (10) | |
O3 | 0.1765 (3) | 0.8948 (4) | 0.22787 (11) | 0.0095 (9) | |
O4 | 0.1837 (3) | 1.0867 (4) | 0.27602 (11) | 0.0106 (9) | |
O5 | 0.1827 (3) | 1.1072 (4) | 0.35273 (11) | 0.0097 (9) | |
O6 | 0.1848 (3) | 0.9093 (4) | 0.39913 (11) | 0.0112 (9) | |
O7 | 0.3185 (3) | 0.9110 (4) | 0.34854 (12) | 0.0109 (9) | |
O8 | 0.3251 (3) | 1.0986 (4) | 0.39872 (11) | 0.0100 (9) | |
O9 | −0.3193 (3) | 0.6002 (4) | 0.52346 (11) | 0.0109 (9) | |
O10 | −0.1808 (3) | 0.5936 (4) | 0.47527 (11) | 0.0092 (9) | |
O11 | 0.0000 | 0.5878 (6) | 0.29195 (19) | 0.0210 (15) | |
H11 | −0.0412 | 0.5376 | 0.3050 | 0.025* | |
O12 | 0.0000 | 0.8572 (8) | 0.35111 (17) | 0.0217 (15) | |
H12 | −0.0386 | 0.8103 | 0.3660 | 0.026* | |
O13 | 0.0000 | 1.1692 (8) | 0.47768 (18) | 0.0258 (16) | |
H13 | 0.0496 | 1.1374 | 0.4901 | 0.031* | |
O14 | 0.0000 | 1.4209 (6) | 0.4153 (2) | 0.0241 (16) | |
H14 | 0.0520 | 1.4746 | 0.4139 | 0.029* |
U11 | U22 | U33 | U12 | U13 | U23 | |
Ba1 | 0.0190 (3) | 0.0198 (3) | 0.0186 (3) | 0.000 | 0.000 | 0.0002 (2) |
Ba2 | 0.0179 (3) | 0.0198 (3) | 0.0144 (3) | 0.000 | 0.000 | −0.0032 (2) |
Ba3 | 0.0081 (4) | 0.0269 (5) | 0.0286 (5) | 0.000 | 0.000 | 0.0163 (4) |
V2 | 0.0081 (5) | 0.0050 (5) | 0.0045 (5) | −0.0003 (4) | −0.0002 (4) | −0.0001 (4) |
V1 | 0.0075 (5) | 0.0057 (5) | 0.0048 (5) | 0.0005 (4) | 0.0001 (4) | −0.0002 (4) |
Cl1 | 0.0104 (11) | 0.0129 (10) | 0.0161 (11) | 0.000 | 0.000 | 0.0020 (8) |
Cl2 | 0.0104 (10) | 0.0143 (10) | 0.0132 (11) | 0.000 | 0.000 | 0.0018 (8) |
P1 | 0.0075 (10) | 0.0035 (9) | 0.0061 (10) | 0.000 | −0.0009 (8) | 0.000 |
P2 | 0.0106 (8) | 0.0047 (7) | 0.0046 (7) | −0.0002 (6) | −0.0007 (6) | −0.0001 (5) |
P3 | 0.0062 (10) | 0.0047 (10) | 0.0045 (10) | 0.000 | 0.000 | −0.0002 (8) |
O1 | 0.012 (2) | 0.015 (2) | 0.018 (3) | 0.0009 (18) | −0.0013 (18) | −0.0004 (18) |
O2 | 0.007 (2) | 0.017 (2) | 0.019 (3) | −0.0006 (17) | −0.0023 (18) | −0.0014 (18) |
O3 | 0.007 (2) | 0.012 (2) | 0.009 (2) | −0.0024 (17) | −0.0018 (16) | −0.0019 (17) |
O4 | 0.014 (2) | 0.010 (2) | 0.008 (2) | 0.0014 (17) | 0.0024 (17) | −0.0039 (16) |
O5 | 0.011 (2) | 0.007 (2) | 0.011 (2) | 0.0016 (16) | 0.0000 (17) | 0.0031 (17) |
O6 | 0.014 (2) | 0.010 (2) | 0.009 (2) | −0.0037 (17) | 0.0019 (17) | 0.0066 (17) |
O7 | 0.013 (2) | 0.009 (2) | 0.010 (2) | 0.0037 (17) | 0.0013 (18) | −0.0027 (17) |
O8 | 0.012 (2) | 0.009 (2) | 0.009 (2) | −0.0001 (17) | −0.0023 (16) | −0.0041 (17) |
O9 | 0.013 (2) | 0.010 (2) | 0.010 (2) | 0.0021 (17) | 0.0008 (17) | −0.0035 (17) |
O10 | 0.010 (2) | 0.007 (2) | 0.010 (2) | 0.0000 (16) | 0.0010 (16) | 0.0033 (17) |
O11 | 0.019 (4) | 0.007 (3) | 0.037 (4) | 0.000 | 0.000 | −0.002 (3) |
O12 | 0.018 (3) | 0.045 (4) | 0.003 (3) | 0.000 | 0.000 | −0.006 (3) |
O13 | 0.015 (4) | 0.042 (4) | 0.021 (4) | 0.000 | 0.000 | 0.007 (3) |
O14 | 0.014 (3) | 0.007 (3) | 0.052 (5) | 0.000 | 0.000 | 0.004 (3) |
Ba1—O12 | 2.780 (6) | V2—O3iv | 1.965 (4) |
Ba1—O11 | 2.850 (6) | V2—O4xi | 1.974 (4) |
Ba1—O11i | 2.858 (6) | V1—O1 | 1.589 (4) |
Ba1—O3ii | 2.882 (4) | V1—O8xi | 1.961 (4) |
Ba1—O3 | 2.882 (4) | V1—O9xii | 1.962 (4) |
Ba1—O4 | 2.984 (4) | V1—O6ii | 1.966 (4) |
Ba1—O4ii | 2.984 (4) | V1—O10 | 1.980 (4) |
Ba1—O2 | 2.997 (4) | V1—Cl2 | 2.7922 (10) |
Ba1—O2ii | 2.997 (4) | Cl1—Ba1i | 3.362 (2) |
Ba1—Cl1 | 3.225 (2) | Cl2—V1ii | 2.7922 (10) |
Ba1—Cl1iii | 3.362 (2) | P1—O4xiii | 1.529 (4) |
Ba1—P1iv | 3.5762 (5) | P1—O4 | 1.529 (4) |
Ba2—O14 | 2.790 (6) | P1—O3 | 1.541 (4) |
Ba2—O13 | 2.807 (7) | P1—O3xiii | 1.541 (4) |
Ba2—O12 | 2.854 (6) | P1—Ba1xiv | 3.5762 (5) |
Ba2—O1v | 2.939 (4) | P2—O7 | 1.519 (4) |
Ba2—O1vi | 2.939 (4) | P2—O8 | 1.530 (4) |
Ba2—O5ii | 2.981 (4) | P2—O6 | 1.533 (4) |
Ba2—O5 | 2.981 (4) | P2—O5 | 1.537 (4) |
Ba2—O6ii | 3.082 (4) | P3—O9vii | 1.526 (4) |
Ba2—O6 | 3.082 (4) | P3—O9 | 1.526 (4) |
Ba2—Cl1 | 3.314 (2) | P3—O10 | 1.538 (4) |
Ba2—Cl2 | 3.332 (2) | P3—O10vii | 1.538 (4) |
Ba2—P2ii | 3.6748 (15) | O1—Ba2xi | 2.939 (4) |
Ba3—O10vii | 2.725 (4) | O3—V2xiv | 1.965 (4) |
Ba3—O10 | 2.725 (4) | O4—V2v | 1.974 (4) |
Ba3—O10ii | 2.725 (4) | O5—V2v | 1.945 (4) |
Ba3—O10viii | 2.725 (4) | O6—V1ii | 1.966 (4) |
Ba3—O13ix | 3.043 (7) | O7—V2ii | 1.947 (4) |
Ba3—O13x | 3.043 (7) | O8—V1v | 1.961 (4) |
Ba3—O14ix | 3.086 (7) | O9—V1xii | 1.962 (4) |
Ba3—O14x | 3.086 (7) | O11—Ba1iii | 2.858 (6) |
Ba3—Cl2 | 3.269 (2) | O11—H11 | 0.8500 |
Ba3—Cl2viii | 3.269 (2) | O12—H12 | 0.8499 |
Ba3—P3viii | 3.393 (2) | O13—Ba3xv | 3.043 (7) |
Ba3—P3 | 3.393 (2) | O13—H13 | 0.8499 |
V2—O2 | 1.585 (4) | O14—Ba3xv | 3.086 (7) |
V2—O7ii | 1.947 (4) | O14—H14 | 0.8500 |
V2—O5xi | 1.945 (4) | ||
O12—Ba1—O11 | 68.83 (19) | O10viii—Ba3—O14ix | 104.13 (9) |
O12—Ba1—O11i | 152.24 (19) | O13ix—Ba3—O14ix | 61.76 (16) |
O11—Ba1—O11i | 138.93 (13) | O13x—Ba3—O14ix | 118.24 (16) |
O12—Ba1—O3ii | 123.65 (8) | O10vii—Ba3—O14x | 75.87 (9) |
O11—Ba1—O3ii | 96.48 (11) | O10—Ba3—O14x | 104.13 (9) |
O11i—Ba1—O3ii | 63.46 (9) | O10ii—Ba3—O14x | 104.13 (9) |
O12—Ba1—O3 | 123.65 (8) | O10viii—Ba3—O14x | 75.87 (9) |
O11—Ba1—O3 | 96.48 (11) | O13ix—Ba3—O14x | 118.24 (16) |
O11i—Ba1—O3 | 63.46 (9) | O13x—Ba3—O14x | 61.76 (16) |
O3ii—Ba1—O3 | 111.61 (15) | O14ix—Ba3—O14x | 180.000 (1) |
O12—Ba1—O4 | 92.67 (11) | O10vii—Ba3—Cl2 | 116.28 (8) |
O11—Ba1—O4 | 122.23 (8) | O10—Ba3—Cl2 | 63.72 (8) |
O11i—Ba1—O4 | 72.59 (10) | O10ii—Ba3—Cl2 | 63.72 (8) |
O3ii—Ba1—O4 | 135.53 (11) | O10viii—Ba3—Cl2 | 116.28 (8) |
O3—Ba1—O4 | 48.58 (10) | O13ix—Ba3—Cl2 | 121.64 (13) |
O12—Ba1—O4ii | 92.67 (11) | O13x—Ba3—Cl2 | 58.36 (13) |
O11—Ba1—O4ii | 122.23 (8) | O14ix—Ba3—Cl2 | 59.88 (11) |
O11i—Ba1—O4ii | 72.59 (10) | O14x—Ba3—Cl2 | 120.12 (11) |
O3ii—Ba1—O4ii | 48.58 (10) | O10vii—Ba3—Cl2viii | 63.72 (8) |
O3—Ba1—O4ii | 135.53 (11) | O10—Ba3—Cl2viii | 116.28 (8) |
O4—Ba1—O4ii | 112.46 (15) | O10ii—Ba3—Cl2viii | 116.28 (8) |
O12—Ba1—O2 | 60.14 (10) | O10viii—Ba3—Cl2viii | 63.72 (8) |
O11—Ba1—O2 | 58.92 (9) | O13ix—Ba3—Cl2viii | 58.36 (13) |
O11i—Ba1—O2 | 127.49 (8) | O13x—Ba3—Cl2viii | 121.64 (13) |
O3ii—Ba1—O2 | 65.79 (11) | O14ix—Ba3—Cl2viii | 120.12 (11) |
O3—Ba1—O2 | 153.43 (11) | O14x—Ba3—Cl2viii | 59.88 (11) |
O4—Ba1—O2 | 151.48 (11) | Cl2—Ba3—Cl2viii | 180.0 |
O4ii—Ba1—O2 | 64.37 (11) | O10vii—Ba3—P3viii | 153.67 (8) |
O12—Ba1—O2ii | 60.14 (10) | O10—Ba3—P3viii | 153.67 (8) |
O11—Ba1—O2ii | 58.92 (9) | O10ii—Ba3—P3viii | 26.33 (8) |
O11i—Ba1—O2ii | 127.49 (8) | O10viii—Ba3—P3viii | 26.33 (8) |
O3ii—Ba1—O2ii | 153.43 (11) | O13ix—Ba3—P3viii | 90.000 (1) |
O3—Ba1—O2ii | 65.79 (11) | O13x—Ba3—P3viii | 90.000 (1) |
O4—Ba1—O2ii | 64.37 (11) | O14ix—Ba3—P3viii | 90.000 (1) |
O4ii—Ba1—O2ii | 151.48 (11) | O14x—Ba3—P3viii | 90.000 (1) |
O2—Ba1—O2ii | 104.11 (16) | Cl2—Ba3—P3viii | 90.0 |
O12—Ba1—Cl1 | 73.39 (14) | Cl2viii—Ba3—P3viii | 90.0 |
O11—Ba1—Cl1 | 142.22 (14) | O10vii—Ba3—P3 | 26.33 (8) |
O11i—Ba1—Cl1 | 78.85 (13) | O10—Ba3—P3 | 26.33 (8) |
O3ii—Ba1—Cl1 | 104.37 (8) | O10ii—Ba3—P3 | 153.67 (8) |
O3—Ba1—Cl1 | 104.37 (8) | O10viii—Ba3—P3 | 153.67 (8) |
O4—Ba1—Cl1 | 58.84 (7) | O13ix—Ba3—P3 | 90.000 (1) |
O4ii—Ba1—Cl1 | 58.84 (7) | O13x—Ba3—P3 | 90.000 (1) |
O2—Ba1—Cl1 | 101.74 (8) | O14ix—Ba3—P3 | 90.000 (1) |
O2ii—Ba1—Cl1 | 101.74 (8) | O14x—Ba3—P3 | 90.000 (1) |
O12—Ba1—Cl1iii | 145.50 (14) | Cl2—Ba3—P3 | 90.0 |
O11—Ba1—Cl1iii | 76.67 (14) | Cl2viii—Ba3—P3 | 90.0 |
O11i—Ba1—Cl1iii | 62.26 (13) | P3viii—Ba3—P3 | 180.0 |
O3ii—Ba1—Cl1iii | 59.35 (8) | O2—V2—O7ii | 100.4 (2) |
O3—Ba1—Cl1iii | 59.35 (8) | O2—V2—O5xi | 102.7 (2) |
O4—Ba1—Cl1iii | 105.98 (8) | O7ii—V2—O5xi | 87.96 (17) |
O4ii—Ba1—Cl1iii | 105.98 (8) | O2—V2—O3iv | 99.8 (2) |
O2—Ba1—Cl1iii | 101.88 (8) | O7ii—V2—O3iv | 87.91 (17) |
O2ii—Ba1—Cl1iii | 101.88 (8) | O5xi—V2—O3iv | 157.58 (17) |
Cl1—Ba1—Cl1iii | 141.11 (5) | O2—V2—O4xi | 99.6 (2) |
O12—Ba1—P1iv | 105.24 (3) | O7ii—V2—O4xi | 160.02 (18) |
O11—Ba1—P1iv | 106.25 (4) | O5xi—V2—O4xi | 88.22 (17) |
O11i—Ba1—P1iv | 71.04 (2) | O3iv—V2—O4xi | 88.18 (17) |
O3ii—Ba1—P1iv | 24.75 (8) | O1—V1—O8xi | 100.0 (2) |
O3—Ba1—P1iv | 130.83 (8) | O1—V1—O9xii | 102.8 (2) |
O4—Ba1—P1iv | 131.52 (8) | O8xi—V1—O9xii | 157.21 (18) |
O4ii—Ba1—P1iv | 24.91 (8) | O1—V1—O6ii | 99.0 (2) |
O2—Ba1—P1iv | 57.16 (8) | O8xi—V1—O6ii | 89.43 (17) |
O2ii—Ba1—P1iv | 161.27 (8) | O9xii—V1—O6ii | 88.84 (17) |
Cl1—Ba1—P1iv | 83.41 (3) | O1—V1—O10 | 99.7 (2) |
Cl1iii—Ba1—P1iv | 84.01 (2) | O8xi—V1—O10 | 87.18 (16) |
O14—Ba2—O13 | 68.4 (2) | O9xii—V1—O10 | 87.26 (17) |
O14—Ba2—O12 | 154.1 (2) | O6ii—V1—O10 | 161.39 (18) |
O13—Ba2—O12 | 137.54 (19) | O1—V1—Cl2 | 178.06 (18) |
O14—Ba2—O1v | 61.65 (10) | O8xi—V1—Cl2 | 79.65 (13) |
O13—Ba2—O1v | 60.21 (10) | O9xii—V1—Cl2 | 77.71 (13) |
O12—Ba2—O1v | 125.34 (8) | O6ii—V1—Cl2 | 79.16 (13) |
O14—Ba2—O1vi | 61.65 (10) | O10—V1—Cl2 | 82.23 (12) |
O13—Ba2—O1vi | 60.21 (10) | Ba1—Cl1—Ba2 | 96.11 (5) |
O12—Ba2—O1vi | 125.34 (8) | Ba1—Cl1—Ba1i | 92.10 (5) |
O1v—Ba2—O1vi | 108.02 (17) | Ba2—Cl1—Ba1i | 171.79 (7) |
O14—Ba2—O5ii | 97.30 (11) | V1ii—Cl2—V1 | 173.74 (9) |
O13—Ba2—O5ii | 123.69 (8) | V1ii—Cl2—Ba3 | 87.68 (5) |
O12—Ba2—O5ii | 69.32 (10) | V1—Cl2—Ba3 | 87.68 (5) |
O1v—Ba2—O5ii | 156.83 (11) | V1ii—Cl2—Ba2 | 92.90 (5) |
O1vi—Ba2—O5ii | 65.14 (11) | V1—Cl2—Ba2 | 92.90 (5) |
O14—Ba2—O5 | 97.30 (11) | Ba3—Cl2—Ba2 | 159.94 (7) |
O13—Ba2—O5 | 123.69 (8) | O4xiii—P1—O4 | 114.7 (3) |
O12—Ba2—O5 | 69.32 (10) | O4xiii—P1—O3 | 112.2 (2) |
O1v—Ba2—O5 | 65.14 (11) | O4—P1—O3 | 103.8 (2) |
O1vi—Ba2—O5 | 156.83 (11) | O4xiii—P1—O3xiii | 103.8 (2) |
O5ii—Ba2—O5 | 111.76 (15) | O4—P1—O3xiii | 112.2 (2) |
O14—Ba2—O6ii | 125.21 (8) | O3—P1—O3xiii | 110.4 (3) |
O13—Ba2—O6ii | 96.45 (11) | O4xiii—P1—Ba1 | 145.08 (16) |
O12—Ba2—O6ii | 61.86 (9) | O4—P1—Ba1 | 55.32 (15) |
O1v—Ba2—O6ii | 153.10 (11) | O3—P1—Ba1 | 51.53 (15) |
O1vi—Ba2—O6ii | 65.24 (11) | O3xiii—P1—Ba1 | 110.91 (16) |
O5ii—Ba2—O6ii | 46.77 (10) | O4xiii—P1—Ba1xiv | 55.32 (15) |
O5—Ba2—O6ii | 131.00 (11) | O4—P1—Ba1xiv | 145.08 (16) |
O14—Ba2—O6 | 125.21 (8) | O3—P1—Ba1xiv | 110.91 (15) |
O13—Ba2—O6 | 96.45 (11) | O3xiii—P1—Ba1xiv | 51.53 (15) |
O12—Ba2—O6 | 61.86 (9) | Ba1—P1—Ba1xiv | 153.12 (6) |
O1v—Ba2—O6 | 65.24 (11) | O7—P2—O8 | 106.3 (2) |
O1vi—Ba2—O6 | 153.10 (11) | O7—P2—O6 | 113.1 (2) |
O5ii—Ba2—O6 | 131.00 (11) | O8—P2—O6 | 111.5 (2) |
O5—Ba2—O6 | 46.77 (10) | O7—P2—O5 | 112.0 (2) |
O6ii—Ba2—O6 | 108.18 (14) | O8—P2—O5 | 110.7 (2) |
O14—Ba2—Cl1 | 82.96 (15) | O6—P2—O5 | 103.3 (2) |
O13—Ba2—Cl1 | 151.34 (14) | O7—P2—Ba2 | 145.71 (17) |
O12—Ba2—Cl1 | 71.12 (14) | O8—P2—Ba2 | 107.88 (16) |
O1v—Ba2—Cl1 | 106.59 (9) | O6—P2—Ba2 | 55.66 (16) |
O1vi—Ba2—Cl1 | 106.59 (9) | O5—P2—Ba2 | 51.83 (15) |
O5ii—Ba2—Cl1 | 58.22 (8) | O9vii—P3—O9 | 105.9 (3) |
O5—Ba2—Cl1 | 58.22 (7) | O9vii—P3—O10 | 112.1 (2) |
O6ii—Ba2—Cl1 | 100.22 (8) | O9—P3—O10 | 111.6 (2) |
O6—Ba2—Cl1 | 100.22 (8) | O9vii—P3—O10vii | 111.6 (2) |
O14—Ba2—Cl2 | 145.43 (16) | O9—P3—O10vii | 112.1 (2) |
O13—Ba2—Cl2 | 77.05 (15) | O10—P3—O10vii | 103.6 (3) |
O12—Ba2—Cl2 | 60.49 (14) | O9vii—P3—Ba3 | 127.06 (16) |
O1v—Ba2—Cl2 | 101.22 (8) | O9—P3—Ba3 | 127.06 (16) |
O1vi—Ba2—Cl2 | 101.22 (8) | O10—P3—Ba3 | 51.82 (15) |
O5ii—Ba2—Cl2 | 101.85 (7) | O10vii—P3—Ba3 | 51.82 (16) |
O5—Ba2—Cl2 | 101.85 (7) | V1—O1—Ba2xi | 146.6 (2) |
O6ii—Ba2—Cl2 | 57.60 (7) | V2—O2—Ba1 | 144.7 (2) |
O6—Ba2—Cl2 | 57.60 (7) | P1—O3—V2xiv | 127.2 (2) |
Cl1—Ba2—Cl2 | 131.61 (5) | P1—O3—Ba1 | 103.72 (18) |
O14—Ba2—P2ii | 107.70 (4) | V2xiv—O3—Ba1 | 126.69 (17) |
O13—Ba2—P2ii | 106.61 (4) | P1—O4—V2v | 134.2 (2) |
O12—Ba2—P2ii | 69.20 (2) | P1—O4—Ba1 | 99.77 (18) |
O1v—Ba2—P2ii | 164.78 (9) | V2v—O4—Ba1 | 124.48 (17) |
O1vi—Ba2—P2ii | 56.86 (8) | P2—O5—V2v | 130.6 (2) |
O5ii—Ba2—P2ii | 23.92 (8) | P2—O5—Ba2 | 104.25 (19) |
O5—Ba2—P2ii | 129.24 (8) | V2v—O5—Ba2 | 123.02 (16) |
O6ii—Ba2—P2ii | 24.25 (7) | P2—O6—V1ii | 133.8 (3) |
O6—Ba2—P2ii | 126.97 (8) | P2—O6—Ba2 | 100.09 (18) |
Cl1—Ba2—P2ii | 81.47 (3) | V1ii—O6—Ba2 | 122.33 (17) |
Cl2—Ba2—P2ii | 81.71 (3) | P2—O7—V2ii | 134.2 (3) |
O10vii—Ba3—O10 | 52.66 (16) | P2—O8—V1v | 128.7 (2) |
O10vii—Ba3—O10ii | 180.00 (7) | P3—O9—V1xii | 132.6 (3) |
O10—Ba3—O10ii | 127.34 (16) | P3—O10—V1 | 131.7 (2) |
O10vii—Ba3—O10viii | 127.34 (16) | P3—O10—Ba3 | 101.85 (19) |
O10—Ba3—O10viii | 180.00 (16) | V1—O10—Ba3 | 126.36 (17) |
O10ii—Ba3—O10viii | 52.66 (16) | Ba1—O11—Ba1iii | 112.4 (2) |
O10vii—Ba3—O13ix | 77.84 (9) | Ba1—O11—H11 | 129.5 |
O10—Ba3—O13ix | 102.16 (9) | Ba1iii—O11—H11 | 97.8 |
O10ii—Ba3—O13ix | 102.16 (9) | Ba1—O12—Ba2 | 119.4 (2) |
O10viii—Ba3—O13ix | 77.84 (9) | Ba1—O12—H12 | 132.9 |
O10vii—Ba3—O13x | 102.16 (9) | Ba2—O12—H12 | 90.8 |
O10—Ba3—O13x | 77.84 (9) | Ba2—O13—Ba3xv | 115.3 (2) |
O10ii—Ba3—O13x | 77.84 (9) | Ba2—O13—H13 | 116.8 |
O10viii—Ba3—O13x | 102.16 (9) | Ba3xv—O13—H13 | 100.7 |
O13ix—Ba3—O13x | 180.0 (2) | Ba2—O14—Ba3xv | 114.5 (2) |
O10vii—Ba3—O14ix | 104.13 (9) | Ba2—O14—H14 | 122.6 |
O10—Ba3—O14ix | 75.87 (9) | Ba3xv—O14—H14 | 85.9 |
O10ii—Ba3—O14ix | 75.87 (9) | ||
O3ii—Ba1—Cl1—Ba2 | 121.37 (8) | O13ix—Ba3—P3—O10vii | 61.6 (2) |
O3—Ba1—Cl1—Ba2 | −121.37 (8) | O13x—Ba3—P3—O10vii | −118.4 (2) |
O4—Ba1—Cl1—Ba2 | −103.72 (9) | O14ix—Ba3—P3—O10vii | 123.4 (2) |
O4ii—Ba1—Cl1—Ba2 | 103.72 (9) | O14x—Ba3—P3—O10vii | −56.6 (2) |
O2—Ba1—Cl1—Ba2 | 53.66 (8) | Cl2—Ba3—P3—O10vii | −176.72 (19) |
O2ii—Ba1—Cl1—Ba2 | −53.66 (8) | Cl2viii—Ba3—P3—O10vii | 3.28 (19) |
P1iv—Ba1—Cl1—Ba2 | 108.099 (15) | O8xi—V1—O1—Ba2xi | −3.2 (4) |
O3ii—Ba1—Cl1—Ba1i | −58.63 (8) | O9xii—V1—O1—Ba2xi | 178.7 (4) |
O3—Ba1—Cl1—Ba1i | 58.63 (8) | O6ii—V1—O1—Ba2xi | 87.8 (4) |
O4—Ba1—Cl1—Ba1i | 76.28 (9) | O10—V1—O1—Ba2xi | −92.0 (4) |
O4ii—Ba1—Cl1—Ba1i | −76.28 (9) | Cl2—V1—O1—Ba2xi | 75 (5) |
O2—Ba1—Cl1—Ba1i | −126.34 (8) | O7ii—V2—O2—Ba1 | −87.7 (4) |
O2ii—Ba1—Cl1—Ba1i | 126.34 (8) | O5xi—V2—O2—Ba1 | −177.9 (3) |
P1iv—Ba1—Cl1—Ba1i | −71.901 (15) | O3iv—V2—O2—Ba1 | 2.0 (4) |
O1v—Ba2—Cl1—Ba1 | 122.41 (8) | O4xi—V2—O2—Ba1 | 91.8 (4) |
O1vi—Ba2—Cl1—Ba1 | −122.41 (8) | O12—Ba1—O2—V2 | 137.5 (4) |
O5ii—Ba2—Cl1—Ba1 | −76.87 (9) | O11—Ba1—O2—V2 | −140.6 (4) |
O5—Ba2—Cl1—Ba1 | 76.87 (9) | O11i—Ba1—O2—V2 | −10.3 (5) |
O6ii—Ba2—Cl1—Ba1 | −55.38 (7) | O3ii—Ba1—O2—V2 | −26.0 (4) |
O6—Ba2—Cl1—Ba1 | 55.38 (7) | O3—Ba1—O2—V2 | −116.2 (4) |
P2ii—Ba2—Cl1—Ba1 | −70.84 (2) | O4—Ba1—O2—V2 | 118.2 (4) |
O1v—Ba2—Cl1—Ba1i | −57.59 (8) | O4ii—Ba1—O2—V2 | 27.9 (4) |
O1vi—Ba2—Cl1—Ba1i | 57.59 (8) | O2ii—Ba1—O2—V2 | −179.9 (3) |
O5ii—Ba2—Cl1—Ba1i | 103.13 (9) | Cl1—Ba1—O2—V2 | 74.6 (4) |
O5—Ba2—Cl1—Ba1i | −103.13 (9) | Cl1iii—Ba1—O2—V2 | −74.3 (4) |
O6ii—Ba2—Cl1—Ba1i | 124.62 (7) | P1iv—Ba1—O2—V2 | 0.5 (3) |
O6—Ba2—Cl1—Ba1i | −124.62 (7) | O4xiii—P1—O3—V2xiv | 53.2 (4) |
P2ii—Ba2—Cl1—Ba1i | 109.16 (2) | O4—P1—O3—V2xiv | 177.5 (3) |
O1—V1—Cl2—V1ii | −124 (5) | O3xiii—P1—O3—V2xiv | −62.1 (2) |
O8xi—V1—Cl2—V1ii | −45.6 (9) | Ba1—P1—O3—V2xiv | −163.0 (4) |
O9xii—V1—Cl2—V1ii | 131.8 (9) | Ba1xiv—P1—O3—V2xiv | −6.7 (3) |
O6ii—V1—Cl2—V1ii | −137.0 (9) | O4xiii—P1—O3—Ba1 | −143.79 (19) |
O10—V1—Cl2—V1ii | 42.9 (9) | O4—P1—O3—Ba1 | −19.5 (2) |
O1—V1—Cl2—Ba3 | −166 (5) | O3xiii—P1—O3—Ba1 | 100.97 (17) |
O8xi—V1—Cl2—Ba3 | −87.93 (12) | Ba1xiv—P1—O3—Ba1 | 156.35 (7) |
O9xii—V1—Cl2—Ba3 | 89.48 (13) | O12—Ba1—O3—P1 | −46.4 (3) |
O6ii—V1—Cl2—Ba3 | −179.34 (13) | O11—Ba1—O3—P1 | −115.2 (2) |
O10—V1—Cl2—Ba3 | 0.61 (12) | O11i—Ba1—O3—P1 | 102.5 (2) |
O1—V1—Cl2—Ba2 | 34 (5) | O3ii—Ba1—O3—P1 | 145.15 (12) |
O8xi—V1—Cl2—Ba2 | 112.15 (13) | O4—Ba1—O3—P1 | 12.76 (16) |
O9xii—V1—Cl2—Ba2 | −70.44 (13) | O4ii—Ba1—O3—P1 | 92.9 (2) |
O6ii—V1—Cl2—Ba2 | 20.73 (13) | O2—Ba1—O3—P1 | −136.1 (2) |
O10—V1—Cl2—Ba2 | −159.32 (13) | O2ii—Ba1—O3—P1 | −63.60 (19) |
O10vii—Ba3—Cl2—V1ii | −179.51 (10) | Cl1—Ba1—O3—P1 | 33.0 (2) |
O10—Ba3—Cl2—V1ii | −176.27 (11) | Cl1iii—Ba1—O3—P1 | 174.5 (2) |
O10ii—Ba3—Cl2—V1ii | 0.49 (10) | P1iv—Ba1—O3—P1 | 126.72 (17) |
O10viii—Ba3—Cl2—V1ii | 3.73 (11) | O12—Ba1—O3—V2xiv | 116.8 (2) |
O13ix—Ba3—Cl2—V1ii | −87.89 (5) | O11—Ba1—O3—V2xiv | 47.9 (2) |
O13x—Ba3—Cl2—V1ii | 92.11 (5) | O11i—Ba1—O3—V2xiv | −94.4 (2) |
O14ix—Ba3—Cl2—V1ii | −87.89 (5) | O3ii—Ba1—O3—V2xiv | −51.7 (3) |
O14x—Ba3—Cl2—V1ii | 92.11 (5) | O4—Ba1—O3—V2xiv | 175.9 (3) |
Cl2viii—Ba3—Cl2—V1ii | −87.9 (6) | O4ii—Ba1—O3—V2xiv | −103.9 (2) |
P3viii—Ba3—Cl2—V1ii | 2.11 (5) | O2—Ba1—O3—V2xiv | 27.1 (4) |
P3—Ba3—Cl2—V1ii | −177.89 (5) | O2ii—Ba1—O3—V2xiv | 99.6 (2) |
O10vii—Ba3—Cl2—V1 | −3.73 (11) | Cl1—Ba1—O3—V2xiv | −163.84 (18) |
O10—Ba3—Cl2—V1 | −0.49 (10) | Cl1iii—Ba1—O3—V2xiv | −22.38 (16) |
O10ii—Ba3—Cl2—V1 | 176.27 (11) | P1iv—Ba1—O3—V2xiv | −70.1 (2) |
O10viii—Ba3—Cl2—V1 | 179.51 (10) | O4xiii—P1—O4—V2v | −53.2 (3) |
O13ix—Ba3—Cl2—V1 | 87.89 (5) | O3—P1—O4—V2v | −175.9 (3) |
O13x—Ba3—Cl2—V1 | −92.11 (5) | O3xiii—P1—O4—V2v | 64.8 (4) |
O14ix—Ba3—Cl2—V1 | 87.89 (5) | Ba1—P1—O4—V2v | 165.6 (4) |
O14x—Ba3—Cl2—V1 | −92.11 (5) | Ba1xiv—P1—O4—V2v | 10.9 (5) |
Cl2viii—Ba3—Cl2—V1 | 87.9 (7) | O4xiii—P1—O4—Ba1 | 141.21 (19) |
P3viii—Ba3—Cl2—V1 | 177.89 (5) | O3—P1—O4—Ba1 | 18.5 (2) |
P3—Ba3—Cl2—V1 | −2.11 (5) | O3xiii—P1—O4—Ba1 | −100.7 (2) |
O10vii—Ba3—Cl2—Ba2 | 88.38 (9) | Ba1xiv—P1—O4—Ba1 | −154.65 (17) |
O10—Ba3—Cl2—Ba2 | 91.62 (9) | O12—Ba1—O4—P1 | 121.6 (2) |
O10ii—Ba3—Cl2—Ba2 | −91.62 (9) | O11—Ba1—O4—P1 | 55.1 (3) |
O10viii—Ba3—Cl2—Ba2 | −88.38 (9) | O11i—Ba1—O4—P1 | −82.3 (2) |
P3viii—Ba3—Cl2—Ba2 | −90.0 | O3ii—Ba1—O4—P1 | −91.3 (2) |
P3—Ba3—Cl2—Ba2 | 90.0 | O3—Ba1—O4—P1 | −12.69 (15) |
O14—Ba2—Cl2—V1ii | −91.18 (5) | O4ii—Ba1—O4—P1 | −144.37 (10) |
O13—Ba2—Cl2—V1ii | −91.18 (5) | O2—Ba1—O4—P1 | 138.3 (2) |
O12—Ba2—Cl2—V1ii | 88.82 (5) | O2ii—Ba1—O4—P1 | 66.75 (18) |
O1v—Ba2—Cl2—V1ii | −35.61 (10) | Cl1—Ba1—O4—P1 | −169.6 (2) |
O1vi—Ba2—Cl2—V1ii | −146.76 (10) | Cl1iii—Ba1—O4—P1 | −29.01 (19) |
O5ii—Ba2—Cl2—V1ii | 146.59 (9) | P1iv—Ba1—O4—P1 | −125.24 (14) |
O5—Ba2—Cl2—V1ii | 31.05 (9) | O12—Ba1—O4—V2v | −45.9 (2) |
O6ii—Ba2—Cl2—V1ii | 162.40 (11) | O11—Ba1—O4—V2v | −112.4 (2) |
O6—Ba2—Cl2—V1ii | 15.23 (9) | O11i—Ba1—O4—V2v | 110.2 (2) |
Cl1—Ba2—Cl2—V1ii | 88.82 (5) | O3ii—Ba1—O4—V2v | 101.2 (2) |
P2ii—Ba2—Cl2—V1ii | 159.55 (6) | O3—Ba1—O4—V2v | 179.8 (3) |
O14—Ba2—Cl2—V1 | 91.18 (5) | O4ii—Ba1—O4—V2v | 48.1 (3) |
O13—Ba2—Cl2—V1 | 91.18 (5) | O2—Ba1—O4—V2v | −29.2 (4) |
O12—Ba2—Cl2—V1 | −88.82 (5) | O2ii—Ba1—O4—V2v | −100.7 (2) |
O1v—Ba2—Cl2—V1 | 146.76 (10) | Cl1—Ba1—O4—V2v | 22.89 (16) |
O1vi—Ba2—Cl2—V1 | 35.61 (10) | Cl1iii—Ba1—O4—V2v | 163.51 (18) |
O5ii—Ba2—Cl2—V1 | −31.05 (9) | P1iv—Ba1—O4—V2v | 67.3 (2) |
O5—Ba2—Cl2—V1 | −146.59 (9) | O7—P2—O5—V2v | −52.1 (4) |
O6ii—Ba2—Cl2—V1 | −15.23 (9) | O8—P2—O5—V2v | 66.3 (4) |
O6—Ba2—Cl2—V1 | −162.40 (11) | O6—P2—O5—V2v | −174.2 (3) |
Cl1—Ba2—Cl2—V1 | −88.82 (5) | Ba2—P2—O5—V2v | 163.2 (4) |
P2ii—Ba2—Cl2—V1 | −18.08 (5) | O7—P2—O5—Ba2 | 144.64 (19) |
O1v—Ba2—Cl2—Ba3 | 55.57 (9) | O8—P2—O5—Ba2 | −96.9 (2) |
O1vi—Ba2—Cl2—Ba3 | −55.57 (9) | O6—P2—O5—Ba2 | 22.6 (2) |
O5ii—Ba2—Cl2—Ba3 | −122.23 (8) | O14—Ba2—O5—P2 | 117.8 (2) |
O5—Ba2—Cl2—Ba3 | 122.23 (8) | O13—Ba2—O5—P2 | 49.0 (3) |
O6ii—Ba2—Cl2—Ba3 | −106.41 (9) | O12—Ba2—O5—P2 | −85.1 (2) |
O6—Ba2—Cl2—Ba3 | 106.41 (9) | O1v—Ba2—O5—P2 | 63.79 (18) |
Cl1—Ba2—Cl2—Ba3 | 180.0 | O1vi—Ba2—O5—P2 | 141.3 (3) |
P2ii—Ba2—Cl2—Ba3 | −109.26 (2) | O5ii—Ba2—O5—P2 | −141.25 (12) |
O12—Ba1—P1—O4xiii | −145.8 (3) | O6ii—Ba2—O5—P2 | −90.3 (2) |
O11—Ba1—P1—O4xiii | 142.3 (3) | O6—Ba2—O5—P2 | −14.80 (15) |
O11i—Ba1—P1—O4xiii | 5.4 (3) | Cl1—Ba2—O5—P2 | −165.1 (2) |
O3ii—Ba1—P1—O4xiii | 28.2 (3) | Cl2—Ba2—O5—P2 | −33.21 (19) |
O3—Ba1—P1—O4xiii | 72.8 (3) | P2ii—Ba2—O5—P2 | −122.13 (17) |
O4—Ba1—P1—O4xiii | −84.0 (5) | O14—Ba2—O5—V2v | −47.0 (2) |
O4ii—Ba1—P1—O4xiii | −38.0 (4) | O13—Ba2—O5—V2v | −115.8 (2) |
O2—Ba1—P1—O4xiii | 177.6 (4) | O12—Ba2—O5—V2v | 110.0 (2) |
O2ii—Ba1—P1—O4xiii | 176.4 (3) | O1v—Ba2—O5—V2v | −101.1 (2) |
Cl1—Ba1—P1—O4xiii | −75.1 (3) | O1vi—Ba2—O5—V2v | −23.5 (4) |
Cl1iii—Ba1—P1—O4xiii | 68.1 (3) | O5ii—Ba2—O5—V2v | 53.9 (3) |
P1iv—Ba1—P1—O4xiii | −4.4 (3) | O6ii—Ba2—O5—V2v | 104.8 (2) |
O12—Ba1—P1—O4 | −61.8 (2) | O6—Ba2—O5—V2v | −179.6 (3) |
O11—Ba1—P1—O4 | −133.7 (2) | Cl1—Ba2—O5—V2v | 30.01 (16) |
O11i—Ba1—P1—O4 | 89.4 (2) | Cl2—Ba2—O5—V2v | 161.93 (18) |
O3ii—Ba1—P1—O4 | 112.2 (2) | P2ii—Ba2—O5—V2v | 73.0 (2) |
O3—Ba1—P1—O4 | 156.8 (3) | O7—P2—O6—V1ii | 59.9 (4) |
O4ii—Ba1—P1—O4 | 45.98 (15) | O8—P2—O6—V1ii | −59.8 (4) |
O2—Ba1—P1—O4 | −98.4 (3) | O5—P2—O6—V1ii | −178.7 (3) |
O2ii—Ba1—P1—O4 | −99.6 (2) | Ba2—P2—O6—V1ii | −157.3 (4) |
Cl1—Ba1—P1—O4 | 8.92 (19) | O7—P2—O6—Ba2 | −142.79 (19) |
Cl1iii—Ba1—P1—O4 | 152.05 (19) | O8—P2—O6—Ba2 | 97.5 (2) |
P1iv—Ba1—P1—O4 | 79.58 (19) | O5—P2—O6—Ba2 | −21.5 (2) |
O12—Ba1—P1—O3 | 141.3 (2) | O14—Ba2—O6—P2 | −48.7 (3) |
O11—Ba1—P1—O3 | 69.4 (2) | O13—Ba2—O6—P2 | −116.7 (2) |
O11i—Ba1—P1—O3 | −67.5 (2) | O12—Ba2—O6—P2 | 101.9 (2) |
O3ii—Ba1—P1—O3 | −44.60 (17) | O1v—Ba2—O6—P2 | −63.76 (19) |
O4—Ba1—P1—O3 | −156.8 (3) | O1vi—Ba2—O6—P2 | −144.8 (2) |
O4ii—Ba1—P1—O3 | −110.9 (2) | O5ii—Ba2—O6—P2 | 96.4 (2) |
O2—Ba1—P1—O3 | 104.8 (3) | O5—Ba2—O6—P2 | 14.60 (15) |
O2ii—Ba1—P1—O3 | 103.5 (2) | O6ii—Ba2—O6—P2 | 144.32 (11) |
Cl1—Ba1—P1—O3 | −147.9 (2) | Cl1—Ba2—O6—P2 | 39.90 (19) |
Cl1iii—Ba1—P1—O3 | −4.79 (19) | Cl2—Ba2—O6—P2 | 173.1 (2) |
P1iv—Ba1—P1—O3 | −77.3 (2) | P2ii—Ba2—O6—P2 | 126.87 (16) |
O12—Ba1—P1—O3xiii | 41.3 (2) | O14—Ba2—O6—V1ii | 112.1 (3) |
O11—Ba1—P1—O3xiii | −30.6 (2) | O13—Ba2—O6—V1ii | 44.0 (2) |
O11i—Ba1—P1—O3xiii | −167.5 (2) | O12—Ba2—O6—V1ii | −97.4 (2) |
O3ii—Ba1—P1—O3xiii | −144.6 (2) | O1v—Ba2—O6—V1ii | 97.0 (2) |
O3—Ba1—P1—O3xiii | −100.0 (3) | O1vi—Ba2—O6—V1ii | 15.9 (4) |
O4—Ba1—P1—O3xiii | 103.1 (2) | O5ii—Ba2—O6—V1ii | −102.9 (2) |
O4ii—Ba1—P1—O3xiii | 149.13 (19) | O5—Ba2—O6—V1ii | 175.3 (3) |
O2—Ba1—P1—O3xiii | 4.8 (3) | O6ii—Ba2—O6—V1ii | −55.0 (3) |
O2ii—Ba1—P1—O3xiii | 3.51 (18) | Cl1—Ba2—O6—V1ii | −159.38 (18) |
Cl1—Ba1—P1—O3xiii | 112.07 (17) | Cl2—Ba2—O6—V1ii | −26.17 (15) |
Cl1iii—Ba1—P1—O3xiii | −104.80 (17) | P2ii—Ba2—O6—V1ii | −72.4 (2) |
P1iv—Ba1—P1—O3xiii | −177.28 (16) | O8—P2—O7—V2ii | 173.5 (3) |
O12—Ba1—P1—Ba1xiv | 85.34 (14) | O6—P2—O7—V2ii | 50.8 (4) |
O11—Ba1—P1—Ba1xiv | 13.42 (14) | O5—P2—O7—V2ii | −65.4 (4) |
O11i—Ba1—P1—Ba1xiv | −123.48 (13) | Ba2—P2—O7—V2ii | −11.6 (6) |
O3ii—Ba1—P1—Ba1xiv | −100.60 (11) | O7—P2—O8—V1v | 177.2 (3) |
O3—Ba1—P1—Ba1xiv | −56.00 (19) | O6—P2—O8—V1v | −59.1 (4) |
O4—Ba1—P1—Ba1xiv | 147.17 (19) | O5—P2—O8—V1v | 55.3 (4) |
O4ii—Ba1—P1—Ba1xiv | −166.86 (10) | Ba2—P2—O8—V1v | 0.2 (3) |
O2—Ba1—P1—Ba1xiv | 48.8 (3) | O9vii—P3—O9—V1xii | 175.1 (4) |
O2ii—Ba1—P1—Ba1xiv | 47.53 (9) | O10—P3—O9—V1xii | −62.6 (4) |
Cl1—Ba1—P1—Ba1xiv | 156.09 (4) | O10vii—P3—O9—V1xii | 53.2 (4) |
Cl1iii—Ba1—P1—Ba1xiv | −60.79 (3) | Ba3—P3—O9—V1xii | −4.9 (4) |
P1iv—Ba1—P1—Ba1xiv | −133.26 (7) | O9vii—P3—O10—V1 | 62.5 (4) |
O14—Ba2—P2—O7 | −139.2 (3) | O9—P3—O10—V1 | −56.1 (4) |
O13—Ba2—P2—O7 | 148.8 (3) | O10vii—P3—O10—V1 | −177.0 (4) |
O12—Ba2—P2—O7 | 13.5 (3) | Ba3—P3—O10—V1 | −177.0 (4) |
O1v—Ba2—P2—O7 | −175.7 (3) | O9vii—P3—O10—Ba3 | −120.5 (2) |
O1vi—Ba2—P2—O7 | 177.3 (4) | O9—P3—O10—Ba3 | 120.8 (2) |
O5ii—Ba2—P2—O7 | −23.6 (3) | O10vii—P3—O10—Ba3 | 0.0 |
O5—Ba2—P2—O7 | −72.2 (3) | O1—V1—O10—P3 | −5.0 (4) |
O6ii—Ba2—P2—O7 | 37.0 (3) | O8xi—V1—O10—P3 | −104.7 (3) |
O6—Ba2—P2—O7 | 80.9 (4) | O9xii—V1—O10—P3 | 97.5 (3) |
Cl1—Ba2—P2—O7 | −59.5 (3) | O6ii—V1—O10—P3 | 175.6 (4) |
Cl2—Ba2—P2—O7 | 75.0 (3) | Cl2—V1—O10—P3 | 175.4 (3) |
P2ii—Ba2—P2—O7 | 7.4 (3) | O1—V1—O10—Ba3 | 178.7 (2) |
O14—Ba2—P2—O8 | 35.6 (2) | O8xi—V1—O10—Ba3 | 79.0 (2) |
O13—Ba2—P2—O8 | −36.4 (2) | O9xii—V1—O10—Ba3 | −78.9 (2) |
O12—Ba2—P2—O8 | −171.7 (2) | O6ii—V1—O10—Ba3 | −0.7 (7) |
O1v—Ba2—P2—O8 | −0.89 (19) | Cl2—V1—O10—Ba3 | −0.90 (18) |
O1vi—Ba2—P2—O8 | −7.8 (4) | O10viii—Ba3—O10—P3 | −163 (100) |
O5ii—Ba2—P2—O8 | 151.28 (19) | O13ix—Ba3—O10—P3 | 64.2 (2) |
O5—Ba2—P2—O8 | 102.6 (3) | O13x—Ba3—O10—P3 | −115.8 (2) |
O6ii—Ba2—P2—O8 | −148.20 (18) | O14ix—Ba3—O10—P3 | 120.6 (2) |
O6—Ba2—P2—O8 | −104.3 (3) | O14x—Ba3—O10—P3 | −59.4 (2) |
Cl1—Ba2—P2—O8 | 115.38 (17) | Cl2—Ba3—O10—P3 | −176.3 (2) |
Cl2—Ba2—P2—O8 | −110.15 (17) | Cl2viii—Ba3—O10—P3 | 3.7 (2) |
P2ii—Ba2—P2—O8 | −177.73 (16) | P3viii—Ba3—O10—P3 | 180.0 |
O14—Ba2—P2—O6 | 139.9 (2) | O10vii—Ba3—O10—V1 | 177.2 (4) |
O13—Ba2—P2—O6 | 67.9 (2) | O10ii—Ba3—O10—V1 | −2.8 (4) |
O12—Ba2—P2—O6 | −67.4 (2) | O10viii—Ba3—O10—V1 | 14 (100) |
O1v—Ba2—P2—O6 | 103.4 (2) | O13ix—Ba3—O10—V1 | −118.6 (2) |
O1vi—Ba2—P2—O6 | 96.4 (4) | O13x—Ba3—O10—V1 | 61.4 (2) |
O5ii—Ba2—P2—O6 | −104.4 (2) | O14ix—Ba3—O10—V1 | −62.2 (2) |
O5—Ba2—P2—O6 | −153.1 (3) | O14x—Ba3—O10—V1 | 117.8 (2) |
O6ii—Ba2—P2—O6 | −43.92 (16) | Cl2—Ba3—O10—V1 | 0.85 (17) |
Cl1—Ba2—P2—O6 | −140.33 (19) | Cl2viii—Ba3—O10—V1 | −179.15 (17) |
Cl2—Ba2—P2—O6 | −5.87 (19) | P3viii—Ba3—O10—V1 | −2.8 (4) |
P2ii—Ba2—P2—O6 | −73.4 (2) | P3—Ba3—O10—V1 | 177.2 (4) |
O14—Ba2—P2—O5 | −67.0 (2) | O3ii—Ba1—O11—Ba1iii | 56.35 (8) |
O13—Ba2—P2—O5 | −139.0 (2) | O3—Ba1—O11—Ba1iii | −56.35 (8) |
O12—Ba2—P2—O5 | 85.7 (2) | O4—Ba1—O11—Ba1iii | −100.67 (12) |
O1v—Ba2—P2—O5 | −103.5 (2) | O4ii—Ba1—O11—Ba1iii | 100.67 (12) |
O1vi—Ba2—P2—O5 | −110.5 (4) | O2—Ba1—O11—Ba1iii | 112.95 (12) |
O5ii—Ba2—P2—O5 | 48.63 (17) | O2ii—Ba1—O11—Ba1iii | −112.95 (12) |
O6ii—Ba2—P2—O5 | 109.2 (2) | Cl1—Ba1—O11—Ba1iii | 180.0 |
O6—Ba2—P2—O5 | 153.1 (3) | Cl1iii—Ba1—O11—Ba1iii | 0.0 |
Cl1—Ba2—P2—O5 | 12.74 (19) | P1iv—Ba1—O11—Ba1iii | 79.58 (4) |
Cl2—Ba2—P2—O5 | 147.20 (19) | O3ii—Ba1—O12—Ba2 | −96.46 (13) |
P2ii—Ba2—P2—O5 | 79.6 (2) | O3—Ba1—O12—Ba2 | 96.46 (13) |
O10vii—Ba3—P3—O9vii | −89.7 (3) | O4—Ba1—O12—Ba2 | 56.32 (7) |
O10—Ba3—P3—O9vii | 90.3 (3) | O4ii—Ba1—O12—Ba2 | −56.32 (7) |
O10ii—Ba3—P3—O9vii | 90.3 (3) | O2—Ba1—O12—Ba2 | −114.58 (11) |
O10viii—Ba3—P3—O9vii | −89.7 (3) | O2ii—Ba1—O12—Ba2 | 114.58 (11) |
O13ix—Ba3—P3—O9vii | −28.0 (2) | P1iv—Ba1—O12—Ba2 | −78.15 (5) |
O13x—Ba3—P3—O9vii | 152.0 (2) | O1v—Ba2—O12—Ba1 | −97.31 (14) |
O14ix—Ba3—P3—O9vii | 33.7 (2) | O1vi—Ba2—O12—Ba1 | 97.31 (14) |
O14x—Ba3—P3—O9vii | −146.3 (2) | O5ii—Ba2—O12—Ba1 | 62.24 (9) |
Cl2—Ba3—P3—O9vii | 93.62 (19) | O5—Ba2—O12—Ba1 | −62.24 (9) |
Cl2viii—Ba3—P3—O9vii | −86.38 (19) | O6ii—Ba2—O12—Ba1 | 113.30 (10) |
P3viii—Ba3—P3—O9vii | 0 (85) | O6—Ba2—O12—Ba1 | −113.30 (10) |
O10vii—Ba3—P3—O9 | 90.3 (3) | P2ii—Ba2—O12—Ba1 | 87.84 (6) |
O10—Ba3—P3—O9 | −89.7 (3) | O1v—Ba2—O13—Ba3xv | 68.80 (12) |
O10ii—Ba3—P3—O9 | −89.7 (3) | O1vi—Ba2—O13—Ba3xv | −68.80 (12) |
O10viii—Ba3—P3—O9 | 90.3 (3) | O5ii—Ba2—O13—Ba3xv | −84.26 (13) |
O13ix—Ba3—P3—O9 | 152.0 (2) | O5—Ba2—O13—Ba3xv | 84.26 (13) |
O13x—Ba3—P3—O9 | −28.0 (2) | O6ii—Ba2—O13—Ba3xv | −125.40 (7) |
O14ix—Ba3—P3—O9 | −146.3 (2) | O6—Ba2—O13—Ba3xv | 125.40 (7) |
O14x—Ba3—P3—O9 | 33.7 (2) | P2ii—Ba2—O13—Ba3xv | −102.89 (5) |
Cl2—Ba3—P3—O9 | −86.38 (19) | O1v—Ba2—O14—Ba3xv | −66.83 (12) |
Cl2viii—Ba3—P3—O9 | 93.62 (19) | O1vi—Ba2—O14—Ba3xv | 66.83 (12) |
O13ix—Ba3—P3—O10 | −118.4 (2) | O5ii—Ba2—O14—Ba3xv | 123.42 (8) |
O13x—Ba3—P3—O10 | 61.6 (2) | O5—Ba2—O14—Ba3xv | −123.42 (8) |
O14ix—Ba3—P3—O10 | −56.6 (2) | O6ii—Ba2—O14—Ba3xv | 82.43 (14) |
O14x—Ba3—P3—O10 | 123.4 (2) | O6—Ba2—O14—Ba3xv | −82.43 (14) |
Cl2—Ba3—P3—O10 | 3.28 (19) | P2ii—Ba2—O14—Ba3xv | 101.32 (5) |
Cl2viii—Ba3—P3—O10 | −176.72 (19) |
Symmetry codes: (i) x, y+1/2, −z+1/2; (ii) −x, y, z; (iii) x, y−1/2, −z+1/2; (iv) x−1/2, y, −z+1/2; (v) x+1/2, y+1/2, z; (vi) −x−1/2, y+1/2, z; (vii) x, −y+1, −z+1; (viii) −x, −y+1, −z+1; (ix) x, y−1, z; (x) −x, −y+2, −z+1; (xi) x−1/2, y−1/2, z; (xii) −x−1/2, −y+3/2, −z+1; (xiii) −x+1/2, y, −z+1/2; (xiv) x+1/2, y, −z+1/2; (xv) x, y+1, z. |
Experimental details
Crystal data | |
Chemical formula | Ba5Cl4(H2O)8(VPO5)8 |
Mr | 2267.91 |
Crystal system, space group | Orthorhombic, Cmca |
Temperature (K) | 295 |
a, b, c (Å) | 13.5073 (8), 8.8803 (5), 35.482 (2) |
V (Å3) | 4256.1 (4) |
Z | 4 |
Radiation type | Mo Kα |
µ (mm−1) | 6.90 |
Crystal size (mm) | 0.20 × 0.12 × 0.12 |
Data collection | |
Diffractometer | Bruker APEXII CCD area-detector diffractometer |
Absorption correction | Multi-scan (SADABS; Bruker, 2007) |
Tmin, Tmax | 0.339, 0.492 |
No. of measured, independent and observed [I > 2σ(I)] reflections | 10601, 1993, 1614 |
Rint | 0.046 |
(sin θ/λ)max (Å−1) | 0.597 |
Refinement | |
R[F2 > 2σ(F2)], wR(F2), S | 0.031, 0.078, 1.04 |
No. of reflections | 1993 |
No. of parameters | 180 |
H-atom treatment | H-atom parameters constrained |
w = 1/[σ2(Fo2) + (0.0283P)2 + 42.1779P] where P = (Fo2 + 2Fc2)/3 | |
Δρmax, Δρmin (e Å−3) | 1.63, −1.20 |
Computer programs: APEX2 (Bruker, 2007), SAINT (Bruker, 2007), SHELXS97 (Sheldrick, 2008), SHELXL97 (Sheldrick, 2008), SHELXTL (Sheldrick, 2008).
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The V–P–O system has received considerable attention, not only because of its application to catalysis, but also due to its rich and impressive structural chemistry associated with the ability of vanadium to have tetrahedral, square-pyramidal and octahedral coordination environments in various oxidation states. The introduction of pyridinium cations into the V–P–O system leads to rather complicated structures (Huang et al., 2001; Luan et al., 2001). Several structures have also been reported with the introduction of organic ammonium cations into the V–P–O system (Zhang et al., 1995; Soghomonian et al., 1996; Luan et al., 2003). A few structures with introduction of inorganic cations into the P—V—O system have also been reported (Soghomonian et al., 1998; Khan et al., 1996; Tian & Wu, 2002). In the present paper, we report a new compound, Ba5Cl4(H2O)8(PVO5)8, in which the oxovanadium phosphate framework is templated by an unusual cationic barium chloride hydrate cluster of composition Ba5Cl4(H2O)8.
Ba5Cl4(H2O)8(VPO5)8 crystallizes in the orthorhombic space group Cmca with a unit cell consisting of four asymmetric units. The coordination environments of the V, P and Ba atoms are shown in Fig. 1. Each of the two independent V sites in the asymmetric unit exhibits a distorted square-pyramidal [VO5] geometry. The basal positions are defined by O donors from four adjacent phosphate groups and the apical O atoms (O1 and O2) are coordinated to adjacent Ba2+ cations. Based on the stoichiometry of the compound and assuming normal oxidation states for Ba, Cl, P and O, the oxidation states of vanadium are VIV and VV in a ratio of 3:1, i.e. two of the eight V atoms are VV and six are VIV. The bond-valence sum calculations (Standard reference?) for V1 and V2 give values of 4.42 and 4.35, respectively. The mean valence, 4.385, is reasonably close to 4.25 for VIV:VV = 3:1. Similar mixed bond-valence sums for V atoms have been reported in other oxovanadium phosphates (Zhang et al., 1999; Le Fur et al., 2001). Atoms Ba1, Ba2, Cl1, Cl2 and O11–O14 are situated on the (100) mirror plane, while atom Ba3 is on the intersection of the (100) plane and the twofold axis parallel to a. Atom P1 is on the twofold axis parallel to b and atom P3 is on the twofold axis parallel to a. All other atoms, i.e. V1, V2, P2 and O1–10, are on general positions.
Atoms Ba1 and Ba2 are both 11-coordinate, with four phosphate O atoms, two vanadyl oxo atoms, three water molecules and two bridging Cl- anions. Atom Ba3 is ten-coordinate, with four phosphate O atoms, four water molecules and two bridging Cl- anions. The Ba—O bond lengths range from 2.725 (4) to 3.086 (7) Å, while the O—Ba—O angles span 46.72 (10)–180.00 (15)°. The Ba—Cl bond lengths vary from 3.224 (2) to 3.362 (2) Å, with the Cl—Ba—Cl angles in the range 131.61 (5)–180.00 (5)°.
There are two kinds of layer in the structure, namely anionic oxovanadium phosphate (VPO5) and cationic barium chloride hydrate, Ba5Cl4(H2O)8. The (VPO5) layers consist of a checkerboard pattern of corner-sharing VO5 square pyramids and PO4 tetrahedra in the bc plane, and are similar to those found in Na3V2O2F(PO4)2 (Massa et al., 2002) (Fig. 2). In the layers of barium chloride hydrate, clusters of three Ba2+ cations are linked via additional bridging of the Cl- anions and water molecules to form a two-dimensional network in the bc plane (Fig. 3). To our knowledge, this barium chloride hydrate structural unit is unprecedented. Adjacent VPO5 and Ba5Cl4(H2O)8 layers are connected by Ba—O bonds involving both phosphate and vanadyl O atoms of the anionic layers, and the layers alternate along the a axis to generate the three-dimensional structure (Fig. 4).