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The solvothermal reaction of gallium oxide with phosphoric acid in water/ethylene glycol in the presence of piperazine gave the title compound, bis(piperazinium) bis(dihydrogenphosphato)tetra-μ2-hydrogenphosphato-di-μ3-hydroxo-di-μ3-phosphato-tetragallate(III), (C4H12N2)3[Ga4(OH)2(H2PO4)2(HPO4)4(PO4)2]. The compound is isostructural with its FeIII analogue, and contains one-dimensional anionic chains with piperazinium cations lying between them. The tetranuclear anionic building blocks and the piperazinium cations lie on inversion centres.
Supporting information
CCDC reference: 629434
Key indicators
- Single-crystal X-ray study
- T = 295 K
- Mean (C-C) = 0.006 Å
- R factor = 0.029
- wR factor = 0.078
- Data-to-parameter ratio = 13.7
checkCIF/PLATON results
No syntax errors found
Alert level B
PLAT420_ALERT_2_B D-H Without Acceptor O17 - H17 ... ?
Alert level C
PLAT041_ALERT_1_C Calc. and Rep. SumFormula Strings Differ .... ?
PLAT042_ALERT_1_C Calc. and Rep. MoietyFormula Strings Differ .... ?
PLAT045_ALERT_1_C Calculated and Reported Z Differ by ............ 2.00 Ratio
PLAT244_ALERT_4_C Low 'Solvent' Ueq as Compared to Neighbors for N1
PLAT731_ALERT_1_C Bond Calc 0.81(4), Rep 0.820(10) ...... 4.00 su-Ra
O8 -H8 1.555 1.555
PLAT731_ALERT_1_C Bond Calc 0.82(3), Rep 0.820(10) ...... 3.00 su-Ra
O12 -H12 1.555 1.555
PLAT731_ALERT_1_C Bond Calc 0.81(4), Rep 0.810(10) ...... 4.00 su-Ra
O15 -H15 1.555 1.555
PLAT735_ALERT_1_C D-H Calc 0.81(4), Rep 0.820(10) ...... 4.00 su-Ra
O8 -H8 1.555 1.555
PLAT735_ALERT_1_C D-H Calc 0.82(3), Rep 0.820(10) ...... 3.00 su-Ra
O12 -H12 1.555 1.555
PLAT735_ALERT_1_C D-H Calc 0.81(4), Rep 0.810(10) ...... 4.00 su-Ra
O15 -H15 1.555 1.555
PLAT736_ALERT_1_C H...A Calc 1.88(4), Rep 1.880(10) ...... 4.00 su-Ra
H8 -O4 1.555 1.455
PLAT736_ALERT_1_C H...A Calc 1.73(4), Rep 1.730(10) ...... 4.00 su-Ra
H12 -O16 1.555 2.555
PLAT736_ALERT_1_C H...A Calc 2.04(3), Rep 2.030(10) ...... 3.00 su-Ra
H15 -O3 1.555 2.566
PLAT764_ALERT_4_C Overcomplete CIF Bond List Detected (Rep/Expd) . 1.19 Ratio
Alert level G
FORMU01_ALERT_1_G There is a discrepancy between the atom counts in the
_chemical_formula_sum and _chemical_formula_moiety. This is
usually due to the moiety formula being in the wrong format.
Atom count from _chemical_formula_sum: C12 H46 Ga4 N6 O34 P8
Atom count from _chemical_formula_moiety:C120 H360 N6300 O1020 P240
0 ALERT level A = In general: serious problem
1 ALERT level B = Potentially serious problem
14 ALERT level C = Check and explain
1 ALERT level G = General alerts; check
13 ALERT type 1 CIF construction/syntax error, inconsistent or missing data
1 ALERT type 2 Indicator that the structure model may be wrong or deficient
0 ALERT type 3 Indicator that the structure quality may be low
2 ALERT type 4 Improvement, methodology, query or suggestion
0 ALERT type 5 Informative message, check
Data collection: SMART (Bruker, 1997); cell refinement: SAINT (Bruker, 1997); data reduction: SAINT; program(s) used to solve structure: SHELXTL (Bruker, 2001); program(s) used to refine structure: SHELXTL; molecular graphics: SHELXTL; software used to prepare material for publication: SHELXTL.
Bis(piperazinium) bis(dihydrogenphosphato)tetra-µ
2-hydrogenphosphato-
di-µ
3-hydroxo-di-µ
3-phosphato-tetragallate(III)
top
Crystal data top
(C4H12N2)3[Ga4(OH)2(H2PO4)2(HPO4)4(PO4)2] | Z = 1 |
Mr = 1345.19 | F(000) = 676 |
Triclinic, P1 | Dx = 2.298 Mg m−3 |
Hall symbol: -P 1 | Mo Kα radiation, λ = 0.71073 Å |
a = 6.2754 (3) Å | Cell parameters from 6645 reflections |
b = 13.0604 (5) Å | θ = 3.0–28.1° |
c = 13.6268 (6) Å | µ = 3.20 mm−1 |
α = 117.208 (1)° | T = 295 K |
β = 98.796 (1)° | Needle, colourless |
γ = 93.053 (1)° | 0.50 × 0.15 × 0.10 mm |
V = 971.90 (7) Å3 | |
Data collection top
Bruker SMART 1K CCD diffractometer | 4155 independent reflections |
Radiation source: fine-focus sealed tube | 3742 reflections with I > 2σ(I) |
Graphite monochromator | Rint = 0.037 |
ω scans | θmax = 28.1°, θmin = 1.7° |
Absorption correction: multi-scan (SADABS; Sheldrick, 1996) | h = −8→8 |
Tmin = 0.512, Tmax = 0.726 | k = −16→16 |
9405 measured reflections | l = −17→17 |
Refinement top
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)] = 0.029 | Hydrogen site location: inferred from neighbouring sites |
wR(F2) = 0.078 | H atoms treated by a mixture of independent and constrained refinement |
S = 1.03 | w = 1/[σ2(Fo2) + (0.0443P)2 + 0.7591P] where P = (Fo2 + 2Fc2)/3 |
4155 reflections | (Δ/σ)max = 0.001 |
304 parameters | Δρmax = 0.76 e Å−3 |
5 restraints | Δρmin = −0.73 e Å−3 |
Special details top
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. |
Fractional atomic coordinates and isotropic or equivalent isotropic displacement parameters (Å2) top | x | y | z | Uiso*/Ueq | |
Ga1 | 0.17098 (4) | 0.35530 (2) | 0.23964 (2) | 0.01109 (9) | |
Ga2 | 0.51621 (4) | 0.61654 (2) | 0.49250 (2) | 0.01162 (9) | |
P1 | 0.67664 (10) | 0.39526 (5) | 0.31399 (5) | 0.01054 (14) | |
P2 | 0.17618 (11) | 0.62581 (5) | 0.29816 (5) | 0.01215 (14) | |
P3 | −0.08049 (11) | 0.24252 (6) | −0.02624 (6) | 0.01387 (15) | |
P4 | 0.14848 (11) | 0.16429 (5) | 0.32991 (6) | 0.01353 (14) | |
O1 | 0.4732 (3) | 0.34862 (15) | 0.21935 (15) | 0.0132 (4) | |
O2 | −0.1219 (3) | 0.36538 (17) | 0.26491 (16) | 0.0187 (4) | |
O3 | 0.3361 (3) | 0.65857 (15) | 0.60594 (15) | 0.0142 (4) | |
O4 | 0.6940 (3) | 0.52964 (15) | 0.38366 (15) | 0.0150 (4) | |
O5 | 0.1689 (3) | 0.49589 (16) | 0.22294 (16) | 0.0172 (4) | |
O6 | 0.2284 (3) | 0.69390 (16) | 0.23761 (16) | 0.0193 (4) | |
O7 | 0.3379 (3) | 0.67140 (16) | 0.40864 (17) | 0.0222 (4) | |
O8 | −0.0531 (3) | 0.65631 (18) | 0.3263 (2) | 0.0251 (5) | |
H8 | −0.113 (6) | 0.621 (3) | 0.353 (3) | 0.038* | |
O9 | −0.0432 (3) | 0.35564 (17) | −0.03871 (17) | 0.0199 (4) | |
H9 | −0.090 (6) | 0.340 (3) | −0.1039 (13) | 0.030* | |
O10 | 0.0858 (3) | 0.26177 (16) | 0.07626 (15) | 0.0160 (4) | |
O11 | −0.3140 (3) | 0.21481 (19) | −0.0259 (2) | 0.0272 (5) | |
O12 | −0.0017 (4) | 0.14770 (19) | −0.12953 (18) | 0.0297 (5) | |
H12 | −0.076 (6) | 0.086 (2) | −0.176 (3) | 0.045* | |
O13 | 0.1649 (3) | 0.20857 (16) | 0.24506 (16) | 0.0169 (4) | |
O14 | 0.7171 (3) | 0.75314 (16) | 0.55420 (16) | 0.0190 (4) | |
O15 | −0.0965 (3) | 0.15218 (18) | 0.3437 (2) | 0.0249 (5) | |
H15 | −0.157 (6) | 0.209 (2) | 0.370 (3) | 0.037* | |
O16 | 0.2094 (4) | 0.04272 (16) | 0.28906 (17) | 0.0228 (4) | |
O17 | 0.3037 (3) | 0.45211 (15) | 0.41223 (15) | 0.0127 (4) | |
H17 | 0.195 (3) | 0.465 (3) | 0.439 (3) | 0.019* | |
N1 | −0.5940 (4) | 0.1043 (2) | 0.0372 (2) | 0.0278 (6) | |
H1C | −0.5025 | 0.1483 | 0.0222 | 0.033* | |
H1D | −0.6982 | 0.1465 | 0.0671 | 0.033* | |
N2 | 0.5715 (4) | 0.5805 (2) | −0.0373 (2) | 0.0253 (5) | |
H2C | 0.6989 | 0.5583 | −0.0562 | 0.030* | |
H2D | 0.5487 | 0.6412 | −0.0501 | 0.030* | |
N3 | 0.3831 (5) | −0.0810 (2) | 0.3895 (2) | 0.0298 (6) | |
H3C | 0.3342 | −0.1544 | 0.3354 | 0.036* | |
H3D | 0.3359 | −0.0326 | 0.3633 | 0.036* | |
C1 | −0.4750 (8) | 0.0736 (3) | 0.1180 (3) | 0.0507 (12) | |
H1A | −0.5750 | 0.0302 | 0.1378 | 0.061* | |
H1B | −0.4073 | 0.1437 | 0.1860 | 0.061* | |
C2 | −0.6957 (7) | −0.0018 (3) | −0.0690 (4) | 0.0552 (13) | |
H2A | −0.7715 | 0.0203 | −0.1224 | 0.066* | |
H2B | −0.8012 | −0.0469 | −0.0537 | 0.066* | |
C3 | 0.5857 (5) | 0.6180 (3) | 0.0849 (3) | 0.0222 (6) | |
H3A | 0.4558 | 0.6512 | 0.1076 | 0.027* | |
H3B | 0.7102 | 0.6777 | 0.1283 | 0.027* | |
C4 | 0.2930 (6) | −0.0589 (3) | 0.4915 (3) | 0.0353 (8) | |
H4A | 0.3361 | −0.1143 | 0.5172 | 0.042* | |
H4B | 0.1352 | −0.0695 | 0.4727 | 0.042* | |
C5 | 0.3920 (5) | 0.4822 (3) | −0.1097 (3) | 0.0243 (6) | |
H5A | 0.3957 | 0.4565 | −0.1884 | 0.029* | |
H5B | 0.2527 | 0.5089 | −0.0965 | 0.029* | |
C6 | 0.6242 (6) | −0.0636 (3) | 0.4152 (3) | 0.0345 (8) | |
H6A | 0.6789 | −0.0761 | 0.3484 | 0.041* | |
H6B | 0.6761 | −0.1193 | 0.4386 | 0.041* | |
Atomic displacement parameters (Å2) top | U11 | U22 | U33 | U12 | U13 | U23 |
Ga1 | 0.01051 (15) | 0.01008 (14) | 0.01066 (15) | 0.00174 (10) | 0.00143 (10) | 0.00337 (11) |
Ga2 | 0.01470 (16) | 0.00928 (14) | 0.00940 (14) | 0.00181 (10) | 0.00160 (10) | 0.00340 (11) |
P1 | 0.0093 (3) | 0.0102 (3) | 0.0099 (3) | 0.0013 (2) | 0.0018 (2) | 0.0029 (2) |
P2 | 0.0143 (3) | 0.0104 (3) | 0.0108 (3) | 0.0017 (2) | 0.0009 (2) | 0.0048 (3) |
P3 | 0.0141 (3) | 0.0120 (3) | 0.0116 (3) | 0.0008 (2) | −0.0011 (2) | 0.0034 (3) |
P4 | 0.0162 (3) | 0.0086 (3) | 0.0124 (3) | 0.0001 (2) | −0.0005 (2) | 0.0032 (3) |
O1 | 0.0109 (8) | 0.0151 (9) | 0.0105 (8) | 0.0024 (7) | 0.0024 (7) | 0.0032 (7) |
O2 | 0.0123 (9) | 0.0223 (10) | 0.0186 (10) | 0.0034 (7) | 0.0058 (7) | 0.0063 (8) |
O3 | 0.0164 (9) | 0.0144 (9) | 0.0135 (9) | 0.0039 (7) | 0.0054 (7) | 0.0072 (7) |
O4 | 0.0173 (9) | 0.0105 (9) | 0.0135 (9) | 0.0007 (7) | 0.0057 (7) | 0.0019 (7) |
O5 | 0.0254 (10) | 0.0109 (9) | 0.0133 (9) | 0.0034 (7) | 0.0017 (8) | 0.0046 (8) |
O6 | 0.0269 (11) | 0.0160 (9) | 0.0156 (10) | 0.0000 (8) | 0.0021 (8) | 0.0088 (8) |
O7 | 0.0316 (12) | 0.0123 (9) | 0.0158 (10) | 0.0025 (8) | −0.0075 (8) | 0.0047 (8) |
O8 | 0.0181 (10) | 0.0231 (11) | 0.0375 (13) | 0.0049 (8) | 0.0118 (9) | 0.0151 (10) |
O9 | 0.0233 (11) | 0.0195 (10) | 0.0167 (10) | 0.0002 (8) | −0.0007 (8) | 0.0101 (9) |
O10 | 0.0184 (10) | 0.0158 (9) | 0.0099 (9) | 0.0050 (7) | −0.0011 (7) | 0.0036 (7) |
O11 | 0.0170 (11) | 0.0306 (12) | 0.0385 (13) | −0.0024 (9) | 0.0003 (9) | 0.0221 (11) |
O12 | 0.0315 (12) | 0.0227 (11) | 0.0165 (10) | 0.0057 (9) | −0.0014 (9) | −0.0045 (9) |
O13 | 0.0228 (10) | 0.0118 (9) | 0.0133 (9) | 0.0023 (7) | 0.0007 (7) | 0.0044 (8) |
O14 | 0.0254 (11) | 0.0137 (9) | 0.0124 (9) | −0.0054 (8) | −0.0020 (8) | 0.0041 (8) |
O15 | 0.0191 (11) | 0.0220 (11) | 0.0344 (12) | 0.0010 (8) | 0.0055 (9) | 0.0141 (10) |
O16 | 0.0336 (12) | 0.0100 (9) | 0.0193 (10) | 0.0048 (8) | −0.0013 (9) | 0.0041 (8) |
O17 | 0.0124 (9) | 0.0135 (9) | 0.0114 (8) | 0.0028 (7) | 0.0038 (7) | 0.0045 (7) |
N1 | 0.0234 (13) | 0.0160 (12) | 0.0433 (17) | 0.0095 (10) | 0.0145 (12) | 0.0103 (12) |
N2 | 0.0270 (13) | 0.0250 (13) | 0.0275 (14) | −0.0018 (10) | 0.0028 (11) | 0.0168 (12) |
N3 | 0.0444 (17) | 0.0153 (12) | 0.0239 (13) | 0.0017 (11) | −0.0041 (12) | 0.0079 (11) |
C1 | 0.100 (4) | 0.0215 (17) | 0.0202 (17) | 0.017 (2) | 0.0047 (19) | 0.0027 (14) |
C2 | 0.042 (2) | 0.0233 (18) | 0.075 (3) | 0.0031 (16) | −0.029 (2) | 0.014 (2) |
C3 | 0.0189 (14) | 0.0197 (14) | 0.0224 (14) | 0.0016 (11) | 0.0024 (11) | 0.0059 (12) |
C4 | 0.0373 (19) | 0.0249 (16) | 0.0372 (19) | −0.0021 (14) | 0.0041 (15) | 0.0109 (15) |
C5 | 0.0213 (15) | 0.0285 (16) | 0.0214 (14) | 0.0004 (12) | −0.0009 (11) | 0.0121 (13) |
C6 | 0.040 (2) | 0.0243 (16) | 0.0314 (18) | 0.0051 (14) | 0.0067 (15) | 0.0064 (14) |
Geometric parameters (Å, º) top
Ga1—O2 | 1.9212 (19) | O15—H15 | 0.81 (1) |
Ga1—O13 | 1.9499 (18) | O17—Ga2i | 2.1190 (18) |
Ga1—O5 | 1.9512 (18) | O17—H17 | 0.81 (1) |
Ga1—O10 | 1.9530 (18) | N1—C1 | 1.454 (5) |
Ga1—O1 | 1.9586 (18) | N1—C2 | 1.487 (5) |
Ga1—O17 | 2.0959 (18) | N1—H1C | 0.900 |
Ga2—O7 | 1.8746 (19) | N1—H1D | 0.900 |
Ga2—O14 | 1.8823 (19) | N2—C3 | 1.491 (4) |
Ga2—O3 | 1.9474 (18) | N2—C5 | 1.496 (4) |
Ga2—O4 | 1.9583 (18) | N2—H2C | 0.900 |
Ga2—O17i | 2.1191 (18) | N2—H2D | 0.900 |
Ga2—O17 | 2.1651 (18) | N3—C6 | 1.481 (5) |
P1—O2ii | 1.5069 (19) | N3—C4 | 1.492 (5) |
P1—O1 | 1.5362 (18) | N3—H3C | 0.900 |
P1—O3i | 1.5535 (19) | N3—H3D | 0.900 |
P1—O4 | 1.5549 (18) | C1—C2iv | 1.492 (6) |
P2—O7 | 1.517 (2) | C1—H1A | 0.970 |
P2—O6 | 1.517 (2) | C1—H1B | 0.970 |
P2—O5 | 1.5228 (19) | C2—C1iv | 1.492 (6) |
P2—O8 | 1.570 (2) | C2—H2A | 0.970 |
P3—O11 | 1.492 (2) | C2—H2B | 0.970 |
P3—O10 | 1.5192 (18) | C3—C5v | 1.503 (4) |
P3—O12 | 1.563 (2) | C3—H3A | 0.970 |
P3—O9 | 1.572 (2) | C3—H3B | 0.970 |
P4—O16 | 1.5160 (19) | C4—C6vi | 1.515 (5) |
P4—O14i | 1.5190 (19) | C4—H4A | 0.970 |
P4—O13 | 1.524 (2) | C4—H4B | 0.970 |
P4—O15 | 1.585 (2) | C5—C3v | 1.503 (4) |
O2—P1iii | 1.5069 (19) | C5—H5A | 0.970 |
O3—P1i | 1.5535 (19) | C5—H5B | 0.970 |
O8—H8 | 0.82 (1) | C6—C4vi | 1.515 (5) |
O9—H9 | 0.82 (1) | C6—H6A | 0.970 |
O12—H12 | 0.82 (1) | C6—H6B | 0.970 |
O14—P4i | 1.5190 (19) | | |
| | | |
O2—Ga1—O13 | 90.37 (8) | P4—O13—Ga1 | 138.52 (12) |
O2—Ga1—O5 | 89.56 (8) | P4i—O14—Ga2 | 135.72 (12) |
O13—Ga1—O5 | 176.00 (8) | P4—O15—H15 | 120 (3) |
O2—Ga1—O10 | 95.07 (8) | Ga1—O17—Ga2i | 123.73 (8) |
O13—Ga1—O10 | 86.64 (8) | Ga1—O17—Ga2 | 125.78 (9) |
O5—Ga1—O10 | 89.38 (8) | Ga2i—O17—Ga2 | 94.30 (7) |
O2—Ga1—O1 | 178.05 (8) | Ga1—O17—H17 | 101 (2) |
O13—Ga1—O1 | 89.92 (8) | Ga2i—O17—H17 | 103 (2) |
O5—Ga1—O1 | 90.29 (8) | Ga2—O17—H17 | 106 (2) |
O10—Ga1—O1 | 86.87 (8) | C1—N1—C2 | 110.7 (3) |
O2—Ga1—O17 | 92.28 (8) | C1—N1—H1C | 109.5 |
O13—Ga1—O17 | 92.40 (7) | C2—N1—H1C | 109.5 |
O5—Ga1—O17 | 91.60 (7) | C1—N1—H1D | 109.5 |
O10—Ga1—O17 | 172.60 (7) | C2—N1—H1D | 109.5 |
O1—Ga1—O17 | 85.78 (7) | H1C—N1—H1D | 108.1 |
O7—Ga2—O14 | 90.22 (9) | C3—N2—C5 | 112.1 (2) |
O7—Ga2—O3 | 92.91 (9) | C3—N2—H2C | 109.2 |
O14—Ga2—O3 | 101.00 (8) | C5—N2—H2C | 109.2 |
O7—Ga2—O4 | 100.09 (9) | C3—N2—H2D | 109.2 |
O14—Ga2—O4 | 91.66 (8) | C5—N2—H2D | 109.2 |
O3—Ga2—O4 | 161.83 (8) | H2C—N2—H2D | 107.9 |
O7—Ga2—O17i | 175.71 (8) | C6—N3—C4 | 111.3 (3) |
O14—Ga2—O17i | 93.46 (8) | C6—N3—H3C | 109.4 |
O3—Ga2—O17i | 84.22 (7) | C4—N3—H3C | 109.4 |
O4—Ga2—O17i | 82.03 (7) | C6—N3—H3D | 109.4 |
O7—Ga2—O17 | 90.81 (8) | C4—N3—H3D | 109.4 |
O14—Ga2—O17 | 175.17 (8) | H3C—N3—H3D | 108.0 |
O3—Ga2—O17 | 83.66 (7) | N1—C1—C2iv | 110.2 (3) |
O4—Ga2—O17 | 83.52 (7) | N1—C1—H1A | 109.6 |
O17i—Ga2—O17 | 85.70 (7) | C2iv—C1—H1A | 109.6 |
O2ii—P1—O1 | 110.15 (11) | N1—C1—H1B | 109.6 |
O2ii—P1—O3i | 108.70 (11) | C2iv—C1—H1B | 109.6 |
O1—P1—O3i | 110.62 (10) | H1A—C1—H1B | 108.1 |
O2ii—P1—O4 | 109.04 (11) | N1—C2—C1iv | 110.0 (3) |
O1—P1—O4 | 109.66 (10) | N1—C2—H2A | 109.7 |
O3i—P1—O4 | 108.64 (10) | C1iv—C2—H2A | 109.7 |
O7—P2—O6 | 109.64 (12) | N1—C2—H2B | 109.7 |
O7—P2—O5 | 112.67 (11) | C1iv—C2—H2B | 109.7 |
O6—P2—O5 | 110.90 (11) | H2A—C2—H2B | 108.2 |
O7—P2—O8 | 107.81 (13) | N2—C3—C5v | 111.4 (2) |
O6—P2—O8 | 104.07 (12) | N2—C3—H3A | 109.3 |
O5—P2—O8 | 111.36 (12) | C5v—C3—H3A | 109.3 |
O11—P3—O10 | 117.07 (12) | N2—C3—H3B | 109.3 |
O11—P3—O12 | 113.12 (14) | C5v—C3—H3B | 109.3 |
O10—P3—O12 | 105.33 (11) | H3A—C3—H3B | 108.0 |
O11—P3—O9 | 110.66 (12) | N3—C4—C6vi | 110.5 (3) |
O10—P3—O9 | 105.89 (11) | N3—C4—H4A | 109.6 |
O12—P3—O9 | 103.67 (13) | C6vi—C4—H4A | 109.6 |
O16—P4—O14i | 110.83 (11) | N3—C4—H4B | 109.6 |
O16—P4—O13 | 111.70 (12) | C6vi—C4—H4B | 109.6 |
O14i—P4—O13 | 112.09 (11) | H4A—C4—H4B | 108.1 |
O16—P4—O15 | 104.79 (12) | N2—C5—C3v | 111.0 (2) |
O14i—P4—O15 | 107.08 (12) | N2—C5—H5A | 109.4 |
O13—P4—O15 | 110.00 (11) | C3v—C5—H5A | 109.4 |
P1—O1—Ga1 | 125.91 (11) | N2—C5—H5B | 109.4 |
P1iii—O2—Ga1 | 165.68 (14) | C3v—C5—H5B | 109.4 |
P1i—O3—Ga2 | 126.09 (10) | H5A—C5—H5B | 108.0 |
P1—O4—Ga2 | 126.95 (11) | N3—C6—C4vi | 109.5 (3) |
P2—O5—Ga1 | 137.72 (12) | N3—C6—H6A | 109.8 |
P2—O7—Ga2 | 140.06 (12) | C4vi—C6—H6A | 109.8 |
P2—O8—H8 | 118 (3) | N3—C6—H6B | 109.8 |
P3—O9—H9 | 109 (3) | C4vi—C6—H6B | 109.8 |
P3—O10—Ga1 | 143.80 (12) | H6A—C6—H6B | 108.2 |
P3—O12—H12 | 124 (3) | | |
| | | |
O2ii—P1—O1—Ga1 | 175.43 (12) | O12—P3—O10—Ga1 | 175.8 (2) |
O3i—P1—O1—Ga1 | 55.23 (15) | O9—P3—O10—Ga1 | 66.4 (2) |
O4—P1—O1—Ga1 | −64.57 (15) | O2—Ga1—O10—P3 | 36.5 (2) |
O13—Ga1—O1—P1 | −87.38 (13) | O13—Ga1—O10—P3 | 126.6 (2) |
O5—Ga1—O1—P1 | 96.61 (13) | O5—Ga1—O10—P3 | −53.0 (2) |
O10—Ga1—O1—P1 | −174.02 (14) | O1—Ga1—O10—P3 | −143.3 (2) |
O17—Ga1—O1—P1 | 5.03 (13) | O16—P4—O13—Ga1 | −165.63 (16) |
O13—Ga1—O2—P1iii | 103.5 (5) | O14i—P4—O13—Ga1 | −40.6 (2) |
O5—Ga1—O2—P1iii | −80.5 (5) | O15—P4—O13—Ga1 | 78.4 (2) |
O10—Ga1—O2—P1iii | −169.9 (5) | O2—Ga1—O13—P4 | −64.95 (19) |
O17—Ga1—O2—P1iii | 11.1 (5) | O10—Ga1—O13—P4 | −160.01 (19) |
O7—Ga2—O3—P1i | 157.06 (14) | O1—Ga1—O13—P4 | 113.11 (18) |
O14—Ga2—O3—P1i | −112.15 (14) | O17—Ga1—O13—P4 | 27.34 (19) |
O4—Ga2—O3—P1i | 21.2 (3) | O7—Ga2—O14—P4i | 137.80 (19) |
O17i—Ga2—O3—P1i | −19.73 (13) | O3—Ga2—O14—P4i | 44.78 (19) |
O17—Ga2—O3—P1i | 66.57 (13) | O4—Ga2—O14—P4i | −122.11 (18) |
O2ii—P1—O4—Ga2 | −165.27 (13) | O17i—Ga2—O14—P4i | −39.99 (19) |
O1—P1—O4—Ga2 | 74.05 (15) | O2—Ga1—O17—Ga2i | 114.18 (11) |
O3i—P1—O4—Ga2 | −46.95 (16) | O13—Ga1—O17—Ga2i | 23.72 (11) |
O7—Ga2—O4—P1 | −105.99 (14) | O5—Ga1—O17—Ga2i | −156.20 (11) |
O14—Ga2—O4—P1 | 163.50 (14) | O1—Ga1—O17—Ga2i | −66.03 (10) |
O3—Ga2—O4—P1 | 29.0 (3) | O2—Ga1—O17—Ga2 | −119.51 (11) |
O17i—Ga2—O4—P1 | 70.23 (14) | O13—Ga1—O17—Ga2 | 150.03 (11) |
O17—Ga2—O4—P1 | −16.32 (13) | O5—Ga1—O17—Ga2 | −29.88 (11) |
O7—P2—O5—Ga1 | 41.8 (2) | O1—Ga1—O17—Ga2 | 60.29 (10) |
O6—P2—O5—Ga1 | 165.16 (16) | O7—Ga2—O17—Ga1 | 44.73 (12) |
O8—P2—O5—Ga1 | −79.5 (2) | O3—Ga2—O17—Ga1 | 137.58 (11) |
O2—Ga1—O5—P2 | 72.31 (19) | O4—Ga2—O17—Ga1 | −55.33 (11) |
O10—Ga1—O5—P2 | 167.38 (19) | O17i—Ga2—O17—Ga1 | −137.78 (13) |
O1—Ga1—O5—P2 | −105.75 (19) | O7—Ga2—O17—Ga2i | −177.49 (9) |
O17—Ga1—O5—P2 | −19.96 (19) | O3—Ga2—O17—Ga2i | −84.65 (7) |
O6—P2—O7—Ga2 | −133.0 (2) | O4—Ga2—O17—Ga2i | 82.45 (8) |
O5—P2—O7—Ga2 | −8.9 (3) | O17i—Ga2—O17—Ga2i | 0.0 |
O8—P2—O7—Ga2 | 114.4 (2) | C2—N1—C1—C2iv | 58.1 (5) |
O14—Ga2—O7—P2 | 149.9 (2) | C1—N1—C2—C1iv | −58.0 (5) |
O3—Ga2—O7—P2 | −109.1 (2) | C5—N2—C3—C5v | 54.9 (3) |
O4—Ga2—O7—P2 | 58.1 (2) | C6—N3—C4—C6vi | 58.2 (4) |
O17—Ga2—O7—P2 | −25.4 (2) | C3—N2—C5—C3v | −54.6 (4) |
O11—P3—O10—Ga1 | −57.5 (3) | C4—N3—C6—C4vi | −57.6 (4) |
Symmetry codes: (i) −x+1, −y+1, −z+1; (ii) x+1, y, z; (iii) x−1, y, z; (iv) −x−1, −y, −z; (v) −x+1, −y+1, −z; (vi) −x+1, −y, −z+1. |
Hydrogen-bond geometry (Å, º) top
D—H···A | D—H | H···A | D···A | D—H···A |
N1—H1D···O10iii | 0.90 | 2.05 | 2.884 (3) | 153 |
N1—H1C···O11 | 0.90 | 1.80 | 2.691 (3) | 171 |
N3—H3C···O6vii | 0.90 | 1.82 | 2.717 (3) | 174 |
N3—H3D···O16 | 0.90 | 1.84 | 2.726 (3) | 170 |
O8—H8···O4iii | 0.82 (1) | 1.88 (1) | 2.674 (3) | 166 (4) |
O12—H12···O16viii | 0.82 (1) | 1.73 (1) | 2.540 (3) | 171 (4) |
O15—H15···O3ix | 0.81 (1) | 2.03 (1) | 2.829 (3) | 166 (4) |
Symmetry codes: (iii) x−1, y, z; (vii) x, y−1, z; (viii) −x, −y, −z; (ix) −x, −y+1, −z+1. |
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