Buy article online - an online subscription or single-article purchase is required to access this article.
In the title compound, [Na6(NO3)2(H2O)13][Ni(C14H18N2O8)]2, the edta-like tetraanionic unit uses two N and four O atoms to chelate to the Ni atom so that the [Ni(C14H18N2O8)]2- portion of the structure has the Ni atom in a cis-N2O4Ni octahedral geometry. The [Na6(NO3)2H2O)13]4+ portion exists as a chain consisting of edge-sharing NaO6 octahedra; there are four independent Na atoms in the asymmetric unit. The vertices are derived from the O atoms of water molecules, the O atom of the nitrate group as well as the O atoms of the [Ni(C14H18N2O8)]2- unit. The layer structure is consolidated by hydrogen bonds into a three-dimensional network. Two of the Na atoms and three of the water O atoms lie on special positions of site symmetry 2.
Supporting information
CCDC reference: 270252
Key indicators
- Single-crystal X-ray study
- T = 295 K
- Mean (C-C) = 0.006 Å
- R factor = 0.064
- wR factor = 0.182
- Data-to-parameter ratio = 15.8
checkCIF/PLATON results
No syntax errors found
Alert level A
PLAT220_ALERT_2_A Large Non-Solvent O Ueq(max)/Ueq(min) ... 4.82 Ratio
| Author Response: There is a larger than usual U~eq~ range for the oxygen atoms
in the cationic [(H~2~O)~13~(NO~3~)~2~Na~6~] part because some of the water
molecules form strong hydrogen bonds and others weak hydrogen bonds. One
of the water molecules (O1w) forms only one hydrogen bond, and the bond is
weak. There is a large residual peak near O1w but this peak could not be
modeled as a disorder component of O1w.
|
The nitrate group, which interacts with only one Na atom, shows larger
vibrations in the O atoms, and some restraints were applied to the group. It
could not be refined as two groups sharing a common O atom.
PLAT242_ALERT_2_A Check Low Ueq as Compared to Neighbors for Na1
| Author Response: The atom having the large U~eq~ that is linked to Na1 is the O1w
water molecule. The reason for the large U~eq~ is explained above.
|
Alert level B
PLAT222_ALERT_3_B Large Non-Solvent H Ueq(max)/Ueq(min) ... 4.82 Ratio
PLAT241_ALERT_2_B Check High Ueq as Compared to Neighbors for O9
PLAT242_ALERT_2_B Check Low Ueq as Compared to Neighbors for N3
| Author Response: The atom having the large U~eq~ that is linked to Na1 is the O1w
water molecule. The reason for the large U~eq~ is explained above.
|
PLAT415_ALERT_2_B Short Inter D-H..H-X H1W2 .. H4A .. 2.04 Ang.
PLAT733_ALERT_1_B Torsion Calc -1.9(4), Rep -1.90(7) ...... 5.71 su-Rat
O2W -NA1 -O2W -NA2 2.556 1.555 1.555 1.555
Alert level C
PLAT029_ALERT_3_C _diffrn_measured_fraction_theta_full Low ....... 0.97
PLAT042_ALERT_1_C Calc. and Rep. MoietyFormula Strings Differ .... ?
PLAT094_ALERT_2_C Ratio of Maximum / Minimum Residual Density .... 2.31
PLAT152_ALERT_1_C Supplied and Calc Volume s.u. Inconsistent ..... ?
PLAT220_ALERT_2_C Large Non-Solvent N Ueq(max)/Ueq(min) ... 3.32 Ratio
| Author Response: There is a larger than usual U~eq~ range for the oxygen atoms
in the cationic [(H~2~O)~13~(NO~3~)~2~Na~6~] part because some of the water
molecules form strong hydrogen bonds and others weak hydrogen bonds. One
of the water molecules (O1w) forms only one hydrogen bond, and the bond is
weak. There is a large residual peak near O1w but this peak could not be
modeled as a disorder component of O1w.
|
The nitrate group, which interacts with only one Na atom, shows larger
vibrations in the O atoms, and some restraints were applied to the group. It
could not be refined as two groups sharing a common O atom.
PLAT242_ALERT_2_C Check Low Ueq as Compared to Neighbors for Na4
| Author Response: The atom having the large U~eq~ that is linked to Na1 is the O1w
water molecule. The reason for the large U~eq~ is explained above.
|
PLAT410_ALERT_2_C Short Intra H...H Contact H4B .. H6A .. 1.96 Ang.
PLAT410_ALERT_2_C Short Intra H...H Contact H9B .. H14B .. 1.96 Ang.
PLAT720_ALERT_4_C Number of Unusual/Non-Standard Label(s) ........ 11
PLAT726_ALERT_1_C H...A Calc 2.28279, Rep 2.27000 Dev... 0.01 Ang.
H1# -O4 1.555 4.546
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: C28 H62 N6 Na6 Ni2 O35
Atom count from _chemical_formula_moiety:C28 H62 N6 Na6 O35
2 ALERT level A = In general: serious problem
5 ALERT level B = Potentially serious problem
10 ALERT level C = Check and explain
1 ALERT level G = General alerts; check
5 ALERT type 1 CIF construction/syntax error, inconsistent or missing data
10 ALERT type 2 Indicator that the structure model may be wrong or deficient
2 ALERT type 3 Indicator that the structure quality may be low
1 ALERT type 4 Improvement, methodology, query or suggestion
Data collection: SAINT (Bruker, 2002); cell refinement: SMART (Bruker, 2002); data reduction: SAINT; program(s) used to solve structure: SHELXS97 (Sheldrick, 1997); program(s) used to refine structure: SHELXL97 (Sheldrick, 1997); molecular graphics: ORTEPII (Johnson, 1976); software used to prepare material for publication: SHELXL97.
Tridecaaquadinitratohexasodium(I)
bis[(
trans-cyclohexane-1,2-diyldinitrilotetraacetato)nickellate(II)]
top
Crystal data top
[Na6(NO3)2(H2O)13][Ni(C14H18N2O8)]2 | F(000) = 2696 |
Mr = 1298.20 | Dx = 1.700 Mg m−3 |
Monoclinic, C2/c | Mo Kα radiation, λ = 0.71073 Å |
Hall symbol: -C 2yc | Cell parameters from 8026 reflections |
a = 16.9182 (7) Å | θ = 2.5–28.3° |
b = 29.388 (1) Å | µ = 0.90 mm−1 |
c = 10.6777 (4) Å | T = 295 K |
β = 107.174 (1)° | Block, light green |
V = 5072.2 (4) Å3 | 0.40 × 0.25 × 0.20 mm |
Z = 4 | |
Data collection top
Bruker APEX area-detector diffractometer | 5669 independent reflections |
Radiation source: fine-focus sealed tube | 4889 reflections with I > 2σ(I) |
Graphite monochromator | Rint = 0.034 |
φ and ω scans | θmax = 27.5°, θmin = 1.4° |
Absorption correction: multi-scan SADABS (Bruker, 2002) | h = −21→9 |
Tmin = 0.641, Tmax = 0.840 | k = −36→38 |
14674 measured reflections | l = −13→13 |
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)] = 0.064 | Hydrogen site location: inferred from neighbouring sites |
wR(F2) = 0.182 | H-atom parameters constrained |
S = 1.10 | w = 1/[σ2(Fo2) + (0.0885P)2 + 18.9719P] where P = (Fo2 + 2Fc2)/3 |
5669 reflections | (Δ/σ)max = 0.001 |
358 parameters | Δρmax = 1.60 e Å−3 |
11 restraints | Δρmin = −0.69 e Å−3 |
Fractional atomic coordinates and isotropic or equivalent isotropic displacement parameters (Å2) top | x | y | z | Uiso*/Ueq | |
Ni1 | 0.27571 (3) | 0.350103 (17) | 0.75842 (4) | 0.02723 (16) | |
Na1 | 0.0000 | 0.07747 (10) | 0.7500 | 0.0524 (7) | |
Na2 | 0.08442 (10) | 0.17461 (6) | 0.70260 (16) | 0.0366 (4) | |
Na3 | 0.27968 (10) | 0.21892 (6) | 0.70554 (16) | 0.0383 (4) | |
Na4 | 0.5000 | 0.22418 (12) | 0.7500 | 0.0608 (8) | |
O1 | 0.39036 (17) | 0.33740 (10) | 0.8943 (3) | 0.0355 (6) | |
O2 | 0.45521 (17) | 0.35951 (11) | 1.0986 (3) | 0.0397 (7) | |
O3 | 0.32443 (19) | 0.37353 (11) | 0.6178 (3) | 0.0408 (7) | |
O4 | 0.3944 (3) | 0.43143 (17) | 0.5696 (4) | 0.0759 (13) | |
O5 | 0.22657 (17) | 0.29525 (9) | 0.6399 (3) | 0.0332 (6) | |
O6 | 0.13491 (19) | 0.28215 (10) | 0.4445 (3) | 0.0378 (6) | |
O7 | 0.22547 (18) | 0.32511 (10) | 0.8961 (3) | 0.0361 (6) | |
O8 | 0.1047 (2) | 0.29760 (13) | 0.8984 (3) | 0.0529 (9) | |
O9 | 0.3178 (4) | 0.13851 (18) | 0.7601 (5) | 0.108 (2) | |
O10 | 0.4069 (4) | 0.1118 (2) | 0.9314 (8) | 0.160 (4) | |
O11 | 0.2845 (4) | 0.0877 (2) | 0.8734 (6) | 0.122 (2) | |
O1w | 0.0239 (5) | 0.0100 (2) | 0.8939 (11) | 0.152 (3) | |
H1w1 | 0.0680 | 0.0050 | 0.95110 | 0.183* | |
H1w2 | 0.0000 | −0.0144 | 0.8730 | 0.183* | |
O2w | 0.1275 (2) | 0.09535 (13) | 0.6918 (4) | 0.0573 (9) | |
H2w1 | 0.1706 | 0.0883 | 0.7477 | 0.069* | |
H2w2 | 0.1273 | 0.0868 | 0.6186 | 0.069* | |
O3w | 0.0000 | 0.23382 (15) | 0.7500 | 0.0463 (11) | |
H3w1 | 0.0236 | 0.2496 | 0.8135 | 0.056* | |
O4w | 0.15342 (19) | 0.19456 (10) | 0.5525 (3) | 0.0386 (7) | |
H4w1 | 0.1301 | 0.2152 | 0.5039 | 0.046* | |
H4w2 | 0.1601 | 0.1728 | 0.5088 | 0.046* | |
O5w | 0.19866 (18) | 0.21267 (11) | 0.8594 (3) | 0.0383 (7) | |
H5w1 | 0.2210 | 0.1969 | 0.9233 | 0.046* | |
H5w2 | 0.1858 | 0.2375 | 0.8828 | 0.046* | |
O6w | 0.4026 (2) | 0.24156 (11) | 0.8674 (3) | 0.0430 (7) | |
H6w1 | 0.4110 | 0.2265 | 0.9348 | 0.052* | |
H6w2 | 0.4023 | 0.2687 | 0.8848 | 0.052* | |
O7w | 0.5000 | 0.1488 (3) | 0.7500 | 0.121 (3) | |
H7w | 0.5411 | 0.1395 | 0.7321 | 0.146* | |
O8w | 0.5000 | 0.3051 (2) | 0.7500 | 0.0763 (18) | |
H8w | 0.4733 | 0.3144 | 0.7976 | 0.092* | |
N1 | 0.3038 (2) | 0.41479 (11) | 0.8352 (3) | 0.0303 (7) | |
N2 | 0.15816 (18) | 0.37473 (11) | 0.6714 (3) | 0.0265 (6) | |
N3 | 0.3393 (4) | 0.11366 (17) | 0.8553 (5) | 0.088 (2) | |
C1 | 0.4029 (2) | 0.36442 (14) | 0.9903 (4) | 0.0315 (8) | |
C2 | 0.3471 (3) | 0.40598 (14) | 0.9742 (4) | 0.0356 (9) | |
H2a | 0.3076 | 0.4013 | 1.0204 | 0.043* | |
H2b | 0.3795 | 0.4318 | 1.0110 | 0.043* | |
C3 | 0.3591 (3) | 0.41152 (17) | 0.6416 (4) | 0.0442 (10) | |
C4 | 0.3594 (3) | 0.43513 (16) | 0.7673 (4) | 0.0402 (9) | |
H4a | 0.4142 | 0.4348 | 0.8251 | 0.048* | |
H4b | 0.3440 | 0.4660 | 0.7481 | 0.048* | |
C5 | 0.2224 (2) | 0.43814 (13) | 0.8139 (4) | 0.0316 (8) | |
H5 | 0.1979 | 0.4256 | 0.8756 | 0.038* | |
C6 | 0.2282 (3) | 0.48939 (16) | 0.8380 (5) | 0.0491 (12) | |
H6a | 0.2569 | 0.5031 | 0.7837 | 0.059* | |
H6b | 0.2585 | 0.4952 | 0.9268 | 0.059* | |
C7 | 0.1417 (4) | 0.51015 (18) | 0.8084 (5) | 0.0553 (13) | |
H7a | 0.1136 | 0.4972 | 0.8646 | 0.066* | |
H7b | 0.1461 | 0.5420 | 0.8241 | 0.066* | |
C8 | 0.0933 (3) | 0.50122 (16) | 0.6667 (5) | 0.0489 (11) | |
H8a | 0.1214 | 0.5143 | 0.6106 | 0.059* | |
H8b | 0.0403 | 0.5151 | 0.6480 | 0.059* | |
C9 | 0.0832 (3) | 0.45050 (15) | 0.6408 (5) | 0.0429 (10) | |
H9a | 0.0554 | 0.4457 | 0.5505 | 0.051* | |
H9b | 0.0496 | 0.4382 | 0.6899 | 0.051* | |
C10 | 0.1658 (2) | 0.42542 (14) | 0.6772 (4) | 0.0316 (8) | |
H10 | 0.1935 | 0.4342 | 0.6155 | 0.038* | |
C11 | 0.1676 (2) | 0.30703 (13) | 0.5409 (4) | 0.0298 (8) | |
C12 | 0.1352 (3) | 0.35545 (14) | 0.5379 (4) | 0.0338 (8) | |
H12a | 0.1577 | 0.3737 | 0.4835 | 0.041* | |
H12b | 0.0767 | 0.3555 | 0.5021 | 0.041* | |
C13 | 0.1476 (2) | 0.32353 (14) | 0.8549 (4) | 0.0323 (8) | |
C14 | 0.1045 (2) | 0.35590 (14) | 0.7458 (4) | 0.0321 (8) | |
H14a | 0.0596 | 0.3404 | 0.6865 | 0.039* | |
H14b | 0.0822 | 0.3804 | 0.7825 | 0.039* | |
Atomic displacement parameters (Å2) top | U11 | U22 | U33 | U12 | U13 | U23 |
Ni1 | 0.0242 (3) | 0.0303 (3) | 0.0233 (2) | 0.00208 (18) | 0.00099 (18) | −0.00342 (17) |
Na1 | 0.0527 (15) | 0.0554 (17) | 0.0424 (14) | 0.000 | 0.0036 (12) | 0.000 |
Na2 | 0.0292 (8) | 0.0406 (9) | 0.0386 (9) | −0.0039 (7) | 0.0078 (6) | −0.0029 (7) |
Na3 | 0.0325 (8) | 0.0448 (9) | 0.0360 (8) | −0.0052 (7) | 0.0075 (7) | −0.0018 (7) |
Na4 | 0.0505 (16) | 0.081 (2) | 0.0543 (17) | 0.000 | 0.0211 (13) | 0.000 |
O1 | 0.0306 (14) | 0.0370 (15) | 0.0325 (14) | 0.0057 (11) | −0.0004 (11) | −0.0082 (11) |
O2 | 0.0289 (14) | 0.0512 (18) | 0.0304 (14) | 0.0056 (12) | −0.0044 (11) | −0.0031 (12) |
O3 | 0.0425 (16) | 0.0491 (18) | 0.0328 (14) | −0.0048 (14) | 0.0138 (12) | −0.0087 (13) |
O4 | 0.101 (3) | 0.082 (3) | 0.059 (2) | −0.027 (3) | 0.046 (2) | −0.004 (2) |
O5 | 0.0319 (13) | 0.0304 (14) | 0.0327 (13) | 0.0030 (11) | 0.0024 (11) | −0.0039 (11) |
O6 | 0.0427 (16) | 0.0381 (16) | 0.0289 (13) | −0.0081 (13) | 0.0050 (12) | −0.0088 (12) |
O7 | 0.0359 (15) | 0.0409 (16) | 0.0272 (13) | 0.0040 (12) | 0.0025 (11) | 0.0074 (11) |
O8 | 0.056 (2) | 0.056 (2) | 0.0388 (17) | −0.0233 (17) | 0.0016 (15) | 0.0138 (15) |
O9 | 0.168 (6) | 0.067 (3) | 0.084 (4) | 0.014 (4) | 0.029 (4) | 0.025 (3) |
O10 | 0.128 (6) | 0.141 (7) | 0.160 (7) | 0.027 (5) | −0.034 (5) | −0.054 (6) |
O11 | 0.115 (5) | 0.156 (6) | 0.120 (5) | 0.025 (4) | 0.073 (4) | 0.036 (5) |
O1w | 0.121 (6) | 0.081 (4) | 0.226 (10) | −0.032 (4) | 0.007 (6) | 0.023 (5) |
O2w | 0.064 (2) | 0.064 (2) | 0.0453 (19) | 0.0108 (18) | 0.0178 (17) | 0.0003 (16) |
O3w | 0.041 (2) | 0.038 (2) | 0.050 (3) | 0.000 | −0.002 (2) | 0.000 |
O4w | 0.0470 (16) | 0.0364 (16) | 0.0314 (14) | −0.0042 (13) | 0.0100 (13) | −0.0041 (12) |
O5w | 0.0369 (15) | 0.0435 (17) | 0.0303 (14) | 0.0021 (12) | 0.0031 (12) | 0.0043 (12) |
O6w | 0.0517 (18) | 0.0421 (17) | 0.0339 (15) | −0.0029 (14) | 0.0107 (13) | 0.0015 (13) |
O7w | 0.118 (8) | 0.115 (7) | 0.100 (7) | 0.000 | −0.016 (6) | 0.000 |
O8w | 0.088 (5) | 0.066 (4) | 0.099 (5) | 0.000 | 0.065 (4) | 0.000 |
N1 | 0.0303 (15) | 0.0324 (16) | 0.0234 (14) | 0.0016 (13) | 0.0006 (12) | −0.0019 (12) |
N2 | 0.0255 (14) | 0.0287 (16) | 0.0215 (14) | −0.0001 (12) | 0.0011 (11) | −0.0002 (11) |
N3 | 0.112 (5) | 0.088 (4) | 0.065 (3) | 0.047 (4) | 0.028 (4) | −0.006 (3) |
C1 | 0.0224 (17) | 0.038 (2) | 0.0302 (18) | 0.0009 (15) | 0.0012 (14) | 0.0006 (15) |
C2 | 0.038 (2) | 0.037 (2) | 0.0225 (17) | 0.0061 (17) | −0.0048 (15) | −0.0055 (15) |
C3 | 0.043 (2) | 0.053 (3) | 0.038 (2) | −0.004 (2) | 0.0133 (19) | −0.002 (2) |
C4 | 0.040 (2) | 0.040 (2) | 0.038 (2) | −0.0079 (18) | 0.0088 (18) | −0.0056 (18) |
C5 | 0.0343 (19) | 0.0312 (19) | 0.0255 (17) | 0.0034 (15) | 0.0030 (15) | 0.0000 (14) |
C6 | 0.056 (3) | 0.034 (2) | 0.046 (2) | 0.008 (2) | −0.002 (2) | −0.0085 (19) |
C7 | 0.069 (3) | 0.043 (3) | 0.046 (3) | 0.020 (2) | 0.005 (2) | −0.003 (2) |
C8 | 0.055 (3) | 0.039 (2) | 0.045 (2) | 0.015 (2) | 0.003 (2) | 0.008 (2) |
C9 | 0.038 (2) | 0.039 (2) | 0.043 (2) | 0.0096 (18) | −0.0015 (18) | 0.0061 (18) |
C10 | 0.0315 (19) | 0.034 (2) | 0.0255 (17) | 0.0021 (15) | 0.0021 (15) | 0.0021 (14) |
C11 | 0.0279 (18) | 0.034 (2) | 0.0263 (17) | −0.0065 (15) | 0.0066 (14) | −0.0046 (14) |
C12 | 0.034 (2) | 0.038 (2) | 0.0231 (17) | 0.0013 (16) | −0.0023 (15) | −0.0009 (15) |
C13 | 0.036 (2) | 0.033 (2) | 0.0246 (17) | −0.0032 (16) | 0.0052 (15) | −0.0012 (15) |
C14 | 0.0275 (18) | 0.034 (2) | 0.0332 (19) | −0.0008 (15) | 0.0068 (15) | 0.0035 (15) |
Geometric parameters (Å, º) top
Ni1—O1 | 2.085 (3) | O3w—H3w1 | 0.8200 |
Ni1—O3 | 2.034 (3) | O4w—H4w1 | 0.8200 |
Ni1—O5 | 2.066 (3) | O4w—H4w2 | 0.8200 |
Ni1—O7 | 2.040 (3) | O5w—H5w1 | 0.8200 |
Ni1—N1 | 2.069 (3) | O5w—H5w2 | 0.8200 |
Ni1—N2 | 2.062 (3) | O6w—H6w1 | 0.8200 |
Na1—O2i | 2.428 (4) | O6w—H6w2 | 0.8200 |
Na1—O2ii | 2.428 (4) | O7w—H7w | 0.8200 |
Na1—O1w | 2.468 (8) | O8w—H8w | 0.8200 |
Na1—O1wiii | 2.468 (8) | N1—C2 | 1.471 (5) |
Na1—O2w | 2.472 (4) | N1—C4 | 1.474 (6) |
Na1—O2wiii | 2.472 (4) | N1—C5 | 1.494 (5) |
Na2—O2i | 2.608 (4) | N2—C12 | 1.475 (5) |
Na2—O2ii | 2.363 (3) | N2—C14 | 1.479 (5) |
Na2—O2w | 2.454 (4) | N2—C10 | 1.495 (5) |
Na2—O3w | 2.398 (4) | C1—C2 | 1.522 (5) |
Na2—O4w | 2.319 (3) | C2—H2a | 0.9500 |
Na2—O5w | 2.425 (3) | C2—H2b | 0.9500 |
Na3—O5 | 2.441 (3) | C3—C4 | 1.510 (6) |
Na3—O6iv | 2.455 (3) | C4—H4a | 0.9500 |
Na3—O9 | 2.474 (5) | C4—H4b | 0.9500 |
Na3—O4w | 2.384 (3) | C5—C6 | 1.527 (6) |
Na3—O5w | 2.438 (3) | C5—C10 | 1.537 (5) |
Na3—O6w | 2.373 (3) | C5—H5 | 0.9500 |
Na4—O6iv | 2.600 (3) | C6—C7 | 1.530 (7) |
Na4—O6v | 2.600 (3) | C6—H6a | 0.9500 |
Na4—O6w | 2.401 (3) | C6—H6b | 0.9500 |
Na4—O6wvi | 2.401 (3) | C7—C8 | 1.516 (7) |
Na4—O7w | 2.22 (1) | C7—H7a | 0.9500 |
Na4—O8w | 2.378 (7) | C7—H7b | 0.9500 |
O1—C1 | 1.264 (5) | C8—C9 | 1.517 (7) |
O2—C1 | 1.240 (5) | C8—H8a | 0.9500 |
O3—C3 | 1.252 (6) | C8—H8b | 0.9500 |
O4—C3 | 1.249 (6) | C9—C10 | 1.526 (6) |
O5—C11 | 1.268 (5) | C9—H9a | 0.9500 |
O6—C11 | 1.251 (4) | C9—H9b | 0.9500 |
O7—C13 | 1.261 (5) | C10—H10 | 0.9500 |
O8—C13 | 1.234 (5) | C11—C12 | 1.522 (6) |
O9—N3 | 1.216 (6) | C12—H12a | 0.9500 |
O10—N3 | 1.192 (6) | C12—H12b | 0.9500 |
O11—N3 | 1.258 (6) | C13—C14 | 1.514 (5) |
O1w—H1w1 | 0.8200 | C14—H14a | 0.9500 |
O2w—H2w1 | 0.8200 | C14—H14b | 0.9500 |
O2w—H2w2 | 0.8200 | | |
| | | |
O1—Ni1—O3 | 94.5 (1) | Na2—O4w—H4w2 | 112.2 |
O1—Ni1—O5 | 114.2 (1) | Na3—O4w—H4w2 | 112.2 |
O1—Ni1—O7 | 86.2 (1) | H4w1—O4w—H4w2 | 109.8 |
O1—Ni1—N1 | 80.3 (1) | Na2—O5w—Na3 | 93.52 (11) |
O1—Ni1—N2 | 162.2 (1) | Na2—O5w—H5w1 | 113.0 |
O3—Ni1—O7 | 178.4 (1) | Na3—O5w—H5w1 | 113.0 |
O3—Ni1—O5 | 89.4 (1) | Na2—O5w—H5w2 | 113.0 |
O3—Ni1—N1 | 83.5 (1) | Na3—O5w—H5w2 | 113.0 |
O3—Ni1—N2 | 95.5 (1) | H5w1—O5w—H5w2 | 110.4 |
O5—Ni1—O7 | 89.0 (1) | Na3—O6w—Na4 | 98.58 (12) |
O5—Ni1—N1 | 164.4 (1) | Na3—O6w—H6w1 | 112.1 |
O5—Ni1—N2 | 80.7 (1) | Na4—O6w—H6w1 | 112.1 |
O7—Ni1—N1 | 98.1 (1) | Na3—O6w—H6w2 | 112.1 |
O7—Ni1—N2 | 84.2 (1) | Na4—O6w—H6w2 | 112.1 |
N1—Ni1—N2 | 86.2 (1) | H6w1—O6w—H6w2 | 109.7 |
O2i—Na1—O2ii | 80.6 (2) | Na4—O7w—H7w | 109.5 |
O2i—Na1—O1w | 103.7 (2) | Na4—O8w—H8w | 109.5 |
O2i—Na1—O1wiii | 171.6 (2) | C2—N1—C4 | 111.6 (3) |
O2i—Na1—O2w | 83.2 (1) | C2—N1—C5 | 113.4 (3) |
O2i—Na1—O2wiii | 78.1 (1) | C4—N1—C5 | 115.6 (3) |
O2ii—Na1—O1w | 171.6 (2) | C2—N1—Ni1 | 103.1 (2) |
O2ii—Na1—O1wiii | 103.7 (2) | C4—N1—Ni1 | 106.4 (2) |
O2ii—Na1—O2w | 78.1 (1) | C5—N1—Ni1 | 105.5 (2) |
O2ii—Na1—O2wiii | 83.2 (1) | C12—N2—C14 | 110.3 (3) |
O1w—Na1—O1wiii | 73.1 (5) | C12—N2—C10 | 114.7 (3) |
O1w—Na1—O2w | 109.4 (2) | C14—N2—C10 | 114.2 (3) |
O1w—Na1—O2wiii | 90.5 (3) | C12—N2—Ni1 | 104.1 (2) |
O1wiii—Na1—O2w | 90.5 (3) | C14—N2—Ni1 | 106.9 (2) |
O1wiii—Na1—O2wiii | 109.4 (2) | C10—N2—Ni1 | 105.7 (2) |
O2w—Na1—O2wiii | 155.4 (2) | O10—N3—O9 | 125.9 (6) |
O2i—Na2—O2ii | 78.2 (1) | O10—N3—O11 | 118.0 (6) |
O2i—Na2—O2w | 79.9 (1) | O9—N3—O11 | 116.1 (5) |
O2i—Na2—O3w | 78.2 (1) | O2—C1—O1 | 125.9 (4) |
O2i—Na2—O4w | 164.2 (1) | O2—C1—C2 | 116.6 (4) |
O2i—Na2—O5w | 87.7 (1) | O1—C1—C2 | 117.6 (3) |
O2ii—Na2—O2w | 79.7 (1) | N1—C2—C1 | 111.3 (3) |
O2ii—Na2—O3w | 83.2 (1) | N1—C2—H2a | 109.4 |
O2ii—Na2—O4w | 111.5 (1) | C1—C2—H2a | 109.4 |
O2ii—Na2—O5w | 163.4 (1) | N1—C2—H2b | 109.4 |
O2w—Na2—O3w | 154.5 (1) | C1—C2—H2b | 109.4 |
O2w—Na2—O4w | 89.4 (1) | H2a—C2—H2b | 108.0 |
O2w—Na2—O5w | 106.4 (1) | O4—C3—O3 | 125.0 (5) |
O3w—Na2—O4w | 114.5 (1) | O4—C3—C4 | 117.1 (4) |
O3w—Na2—O5w | 85.6 (1) | O3—C3—C4 | 117.9 (4) |
O4w—Na2—O5w | 84.2 (1) | N1—C4—C3 | 114.6 (4) |
O5—Na3—O6iv | 93.6 (1) | N1—C4—H4a | 108.6 |
O5—Na3—O9 | 173.7 (2) | C3—C4—H4a | 108.6 |
O5—Na3—O4w | 84.3 (1) | N1—C4—H4b | 108.6 |
O5—Na3—O5w | 91.7 (1) | C3—C4—H4b | 108.6 |
O5—Na3—O6w | 96.9 (1) | H4a—C4—H4b | 107.6 |
O6iv—Na3—O9 | 88.8 (2) | N1—C5—C6 | 114.7 (3) |
O6iv—Na3—O4w | 97.5 (1) | N1—C5—C10 | 108.7 (3) |
O6iv—Na3—O5w | 174.7 (1) | C6—C5—C10 | 113.0 (3) |
O6iv—Na3—O6w | 85.5 (1) | N1—C5—H5 | 106.6 |
O9—Na3—O4w | 89.6 (2) | C6—C5—H5 | 106.6 |
O9—Na3—O5w | 85.9 (2) | C10—C5—H5 | 106.6 |
O9—Na3—O6w | 89.1 (2) | C5—C6—C7 | 110.4 (4) |
O4w—Na3—O5w | 82.6 (1) | C5—C6—H6a | 109.6 |
O4w—Na3—O6w | 176.8 (1) | C7—C6—H6a | 109.6 |
O5w—Na3—O6w | 94.4 (1) | C5—C6—H6b | 109.6 |
O6iv—Na4—O6v | 171.8 (2) | C7—C6—H6b | 109.6 |
O6iv—Na4—O6w | 81.8 (1) | H6a—C6—H6b | 108.1 |
O6iv—Na4—O6wvi | 100.0 (1) | C8—C7—C6 | 109.9 (4) |
O6iv—Na4—O7w | 85.9 (1) | C8—C7—H7a | 109.7 |
O6iv—Na4—O8w | 94.1 (1) | C6—C7—H7a | 109.7 |
O6v—Na4—O6w | 100.0 (1) | C8—C7—H7b | 109.7 |
O6v—Na4—O6wvi | 81.8 (1) | C6—C7—H7b | 109.7 |
O6v—Na4—O7w | 85.9 (1) | H7a—C7—H7b | 108.2 |
O6v—Na4—O8w | 94.1 (1) | C7—C8—C9 | 110.5 (4) |
O6w—Na4—O6wvi | 155.4 (2) | C7—C8—H8a | 109.5 |
O6w—Na4—O7w | 102.3 (1) | C9—C8—H8a | 109.5 |
O6w—Na4—O8w | 77.7 (1) | C7—C8—H8b | 109.5 |
O6wvi—Na4—O7w | 102.3 (1) | C9—C8—H8b | 109.5 |
O6wvi—Na4—O8w | 77.7 (1) | H8a—C8—H8b | 108.1 |
O7w—Na4—O8w | 180 | C8—C9—C10 | 112.5 (4) |
C1—O1—Ni1 | 110.5 (2) | C8—C9—H9a | 109.1 |
C1—O2—Na2v | 142.6 (3) | C10—C9—H9a | 109.1 |
C1—O2—Na1i | 121.9 (3) | C8—C9—H9b | 109.1 |
Na2v—O2—Na1i | 86.98 (10) | C10—C9—H9b | 109.1 |
C1—O2—Na2i | 121.3 (3) | H9a—C9—H9b | 107.8 |
Na2v—O2—Na2i | 83.04 (11) | N2—C10—C9 | 114.2 (3) |
Na1i—O2—Na2i | 81.73 (10) | N2—C10—C5 | 107.7 (3) |
C3—O3—Ni1 | 114.8 (3) | C9—C10—C5 | 113.0 (3) |
C11—O5—Ni1 | 111.9 (2) | N2—C10—H10 | 107.2 |
C11—O5—Na3 | 128.5 (2) | C9—C10—H10 | 107.2 |
Ni1—O5—Na3 | 119.58 (12) | C5—C10—H10 | 107.2 |
C11—O6—Na3iv | 110.0 (2) | O6—C11—O5 | 125.0 (4) |
C11—O6—Na4iv | 140.4 (3) | O6—C11—C12 | 117.4 (3) |
Na3iv—O6—Na4iv | 91.41 (10) | O5—C11—C12 | 117.6 (3) |
C13—O7—Ni1 | 112.1 (2) | N2—C12—C11 | 110.4 (3) |
N3—O9—Na3 | 139.7 (4) | N2—C12—H12a | 109.6 |
Na1—O1w—H1w1 | 124 | C11—C12—H12a | 109.6 |
Na2—O2w—Na1 | 84.06 (14) | N2—C12—H12b | 109.6 |
Na2—O2w—H2w1 | 114.6 | C11—C12—H12b | 109.6 |
Na1—O2w—H2w1 | 114.6 | H12a—C12—H12b | 108.1 |
Na2—O2w—H2w2 | 114.6 | O8—C13—O7 | 124.2 (4) |
Na1—O2w—H2w2 | 114.6 | O8—C13—C14 | 118.3 (4) |
H2w1—O2w—H2w2 | 111.7 | O7—C13—C14 | 117.5 (3) |
Na2iii—O3w—Na2 | 86.96 (17) | N2—C14—C13 | 114.6 (3) |
Na2iii—O3w—H3w1 | 114.2 | N2—C14—H14a | 108.6 |
Na2—O3w—H3w1 | 114.2 | C13—C14—H14a | 108.6 |
Na2—O4w—Na3 | 97.72 (12) | N2—C14—H14b | 108.6 |
Na2—O4w—H4w1 | 112.2 | C13—C14—H14b | 108.6 |
Na3—O4w—H4w1 | 112.2 | H14a—C14—H14b | 107.6 |
| | | |
O3—Ni1—O1—C1 | 112.1 (3) | O1—Ni1—N1—C4 | 81.8 (3) |
O7—Ni1—O1—C1 | −69.4 (3) | O3—Ni1—N1—C5 | 109.5 (2) |
N2—Ni1—O1—C1 | −11.7 (6) | O7—Ni1—N1—C5 | −70.1 (2) |
O5—Ni1—O1—C1 | −156.6 (3) | N2—Ni1—N1—C5 | 13.5 (2) |
N1—Ni1—O1—C1 | 29.5 (3) | O5—Ni1—N1—C5 | 46.3 (6) |
N2—Ni1—O3—C3 | 94.5 (3) | O1—Ni1—N1—C5 | −154.9 (2) |
O5—Ni1—O3—C3 | 175.0 (3) | O3—Ni1—N2—C12 | 54.7 (2) |
N1—Ni1—O3—C3 | 8.9 (3) | O7—Ni1—N2—C12 | −123.7 (2) |
O1—Ni1—O3—C3 | −70.7 (3) | O5—Ni1—N2—C12 | −33.8 (2) |
O3—Ni1—O5—C11 | −70.3 (3) | N1—Ni1—N2—C12 | 137.7 (2) |
O7—Ni1—O5—C11 | 109.7 (3) | O1—Ni1—N2—C12 | 178.4 (4) |
N2—Ni1—O5—C11 | 25.4 (3) | O3—Ni1—N2—C14 | 171.4 (2) |
N1—Ni1—O5—C11 | −7.8 (6) | O7—Ni1—N2—C14 | −7.0 (2) |
O1—Ni1—O5—C11 | −164.9 (3) | O5—Ni1—N2—C14 | 83.0 (2) |
O3—Ni1—O5—Na3 | 112.52 (16) | N1—Ni1—N2—C14 | −105.5 (2) |
O7—Ni1—O5—Na3 | −67.49 (15) | O1—Ni1—N2—C14 | −64.9 (5) |
N2—Ni1—O5—Na3 | −151.80 (17) | O3—Ni1—N2—C10 | −66.5 (2) |
N1—Ni1—O5—Na3 | 175.0 (4) | O7—Ni1—N2—C10 | 115.1 (2) |
O1—Ni1—O5—Na3 | 17.90 (19) | O5—Ni1—N2—C10 | −155.0 (2) |
O6w—Na3—O5—C11 | 167.8 (3) | N1—Ni1—N2—C10 | 16.5 (2) |
O4w—Na3—O5—C11 | −15.2 (3) | O1—Ni1—N2—C10 | 57.2 (5) |
O5w—Na3—O5—C11 | −97.6 (3) | Na3—O9—N3—O10 | −77.6 (8) |
O6iv—Na3—O5—C11 | 81.9 (3) | Na3—O9—N3—O11 | 102.6 (7) |
O6w—Na3—O5—Ni1 | −15.53 (17) | Na2v—O2—C1—O1 | 26.5 (8) |
O4w—Na3—O5—Ni1 | 161.47 (16) | Na1i—O2—C1—O1 | 161.9 (3) |
O5w—Na3—O5—Ni1 | 79.10 (15) | Na2i—O2—C1—O1 | −97.7 (4) |
O6iv—Na3—O5—Ni1 | −101.38 (15) | Na2v—O2—C1—C2 | −155.7 (4) |
N2—Ni1—O7—C13 | 18.1 (3) | Na1i—O2—C1—C2 | −20.3 (5) |
O5—Ni1—O7—C13 | −62.6 (3) | Na2i—O2—C1—C2 | 80.1 (4) |
N1—Ni1—O7—C13 | 103.4 (3) | Ni1—O1—C1—O2 | 163.1 (4) |
O1—Ni1—O7—C13 | −177.0 (3) | Ni1—O1—C1—C2 | −14.7 (5) |
O6w—Na3—O9—N3 | 50.7 (8) | C4—N1—C2—C1 | −75.5 (4) |
O4w—Na3—O9—N3 | −126.4 (8) | C5—N1—C2—C1 | 151.9 (3) |
O5w—Na3—O9—N3 | −43.8 (8) | Ni1—N1—C2—C1 | 38.3 (4) |
O6iv—Na3—O9—N3 | 136.1 (8) | O2—C1—C2—N1 | 165.0 (4) |
O4w—Na2—O2w—Na1 | −152.39 (11) | O1—C1—C2—N1 | −17.1 (5) |
O2ii—Na2—O2w—Na1 | −40.37 (11) | Ni1—O3—C3—O4 | 178.4 (5) |
O3w—Na2—O2w—Na1 | 8.3 (3) | Ni1—O3—C3—C4 | −1.0 (5) |
O5w—Na2—O2w—Na1 | 123.80 (11) | C2—N1—C4—C3 | 129.1 (4) |
O2i—Na2—O2w—Na1 | 39.29 (9) | C5—N1—C4—C3 | −99.5 (4) |
O2i—Na1—O2w—Na2 | −42.40 (11) | Ni1—N1—C4—C3 | 17.4 (4) |
O2ii—Na1—O2w—Na2 | 39.33 (11) | O4—C3—C4—N1 | 168.7 (5) |
O2wiii—Na1—O2w—Na2 | −1.90 (7) | O3—C3—C4—N1 | −11.9 (6) |
O1wiii—Na1—O2w—Na2 | 143.2 (2) | C2—N1—C5—C6 | 79.6 (4) |
O1w—Na1—O2w—Na2 | −144.6 (3) | C4—N1—C5—C6 | −51.0 (5) |
O4w—Na2—O3w—Na2iii | 152.24 (12) | Ni1—N1—C5—C6 | −168.3 (3) |
O2ii—Na2—O3w—Na2iii | 41.63 (8) | C2—N1—C5—C10 | −152.8 (3) |
O5w—Na2—O3w—Na2iii | −126.19 (10) | C4—N1—C5—C10 | 76.6 (4) |
O2w—Na2—O3w—Na2iii | −6.4 (2) | Ni1—N1—C5—C10 | −40.7 (3) |
O2i—Na2—O3w—Na2iii | −37.64 (7) | N1—C5—C6—C7 | 177.8 (4) |
O2ii—Na2—O4w—Na3 | −174.51 (12) | C10—C5—C6—C7 | 52.4 (5) |
O3w—Na2—O4w—Na3 | 93.22 (12) | C5—C6—C7—C8 | −59.6 (6) |
O5w—Na2—O4w—Na3 | 10.79 (12) | C6—C7—C8—C9 | 61.2 (6) |
O2w—Na2—O4w—Na3 | −95.80 (14) | C7—C8—C9—C10 | −55.5 (6) |
O2i—Na2—O4w—Na3 | −48.6 (5) | C12—N2—C10—C9 | 76.7 (4) |
O5w—Na3—O4w—Na2 | −10.77 (12) | C14—N2—C10—C9 | −52.0 (4) |
O5—Na3—O4w—Na2 | −103.28 (13) | Ni1—N2—C10—C9 | −169.2 (3) |
O6iv—Na3—O4w—Na2 | 163.87 (12) | C12—N2—C10—C5 | −157.0 (3) |
O9—Na3—O4w—Na2 | 75.16 (18) | C14—N2—C10—C5 | 74.4 (4) |
O4w—Na2—O5w—Na3 | −10.47 (12) | Ni1—N2—C10—C5 | −42.8 (3) |
O2ii—Na2—O5w—Na3 | −172.9 (4) | C8—C9—C10—N2 | 171.7 (4) |
O3w—Na2—O5w—Na3 | −125.71 (11) | C8—C9—C10—C5 | 48.1 (5) |
O2w—Na2—O5w—Na3 | 77.23 (14) | N1—C5—C10—N2 | 57.6 (4) |
O2i—Na2—O5w—Na3 | 155.98 (12) | C6—C5—C10—N2 | −173.9 (4) |
O6w—Na3—O5w—Na2 | −168.72 (12) | N1—C5—C10—C9 | −175.4 (3) |
O4w—Na3—O5w—Na2 | 10.22 (12) | C6—C5—C10—C9 | −46.9 (5) |
O5—Na3—O5w—Na2 | 94.19 (11) | Na3iv—O6—C11—O5 | −80.6 (4) |
O9—Na3—O5w—Na2 | −79.92 (17) | Na4iv—O6—C11—O5 | 160.7 (3) |
O5w—Na3—O6w—Na4 | 161.22 (15) | Na3iv—O6—C11—C12 | 98.2 (3) |
O5—Na3—O6w—Na4 | −106.49 (14) | Na4iv—O6—C11—C12 | −20.5 (6) |
O6iv—Na3—O6w—Na4 | −13.45 (14) | Ni1—O5—C11—O6 | 169.3 (3) |
O9—Na3—O6w—Na4 | 75.39 (19) | Na3—O5—C11—O6 | −13.8 (6) |
O7w—Na4—O6w—Na3 | −71.16 (11) | Ni1—O5—C11—C12 | −9.5 (4) |
O8w—Na4—O6w—Na3 | 108.84 (11) | Na3—O5—C11—C12 | 167.3 (3) |
O6wvi—Na4—O6w—Na3 | 108.84 (11) | C14—N2—C12—C11 | −76.4 (4) |
O6v—Na4—O6w—Na3 | −159.10 (14) | C10—N2—C12—C11 | 153.0 (3) |
O6iv—Na4—O6w—Na3 | 12.78 (14) | Ni1—N2—C12—C11 | 38.0 (4) |
O3—Ni1—N1—C2 | −131.4 (3) | O6—C11—C12—N2 | 160.7 (3) |
O7—Ni1—N1—C2 | 49.0 (3) | O5—C11—C12—N2 | −20.3 (5) |
N2—Ni1—N1—C2 | 132.6 (3) | Ni1—O7—C13—O8 | 155.7 (4) |
O5—Ni1—N1—C2 | 165.4 (4) | Ni1—O7—C13—C14 | −24.8 (4) |
O1—Ni1—N1—C2 | −35.7 (2) | C12—N2—C14—C13 | 109.7 (4) |
O3—Ni1—N1—C4 | −13.9 (3) | C10—N2—C14—C13 | −119.5 (3) |
O7—Ni1—N1—C4 | 166.5 (2) | Ni1—N2—C14—C13 | −2.9 (4) |
N2—Ni1—N1—C4 | −109.9 (3) | O8—C13—C14—N2 | −161.4 (4) |
O5—Ni1—N1—C4 | −77.1 (5) | O7—C13—C14—N2 | 19.1 (5) |
Symmetry codes: (i) −x+1/2, −y+1/2, −z+2; (ii) x−1/2, −y+1/2, z−1/2; (iii) −x, y, −z+3/2; (iv) −x+1/2, −y+1/2, −z+1; (v) x+1/2, −y+1/2, z+1/2; (vi) −x+1, y, −z+3/2. |
Hydrogen-bond geometry (Å, º) top
D—H···A | D—H | H···A | D···A | D—H···A |
O1w—H1w1···O4vii | 0.82 | 2.27 | 2.660 (9) | 109 |
O2w—H2w1···O11 | 0.82 | 2.00 | 2.797 (8) | 165 |
O2w—H2w2···O4iv | 0.82 | 2.01 | 2.817 (6) | 170 |
O4w—H4w1···O6 | 0.82 | 2.08 | 2.800 (4) | 147 |
O4w—H4w2···O3iv | 0.82 | 1.99 | 2.803 (4) | 172 |
O5w—H5w1···O7i | 0.82 | 1.98 | 2.778 (4) | 164 |
O5w—H5w2···O8 | 0.82 | 2.27 | 3.053 (5) | 159 |
O6w—H6w1···O8i | 0.82 | 2.01 | 2.789 (4) | 159 |
O6w—H6w2···O1 | 0.82 | 2.03 | 2.845 (4) | 170 |
O7w—H7w···O9vi | 0.82 | 2.36 | 3.130 (7) | 156 |
O7w—H7w···O10vi | 0.82 | 2.32 | 3.04 (1) | 146 |
O8w—H8w···O1 | 0.82 | 2.09 | 2.899 (4) | 172 |
Symmetry codes: (i) −x+1/2, −y+1/2, −z+2; (iv) −x+1/2, −y+1/2, −z+1; (vi) −x+1, y, −z+3/2; (vii) −x+1/2, y−1/2, −z+3/2. |
Subscribe to Acta Crystallographica Section E: Crystallographic Communications
The full text of this article is available to subscribers to the journal.
If you have already registered and are using a computer listed in your registration details, please email
support@iucr.org for assistance.