A novel compound consisting of a hydrated metal cation, an organic molecule, an inorganic complex anion and water of crystallization has been synthesized and is found to crystallize in the monoclinic space group P21/c. The structure of the title compound, [Ni(H2O)6][Cr2O7]·2C6H12N4·H2O, contains octahedrally coordinated nickel ions and discrete dichromate anions. The hexamethylenetetramine molecules have no direct coordination to the metal ions. There are two cations, two anions, four tetramine molecules and two uncoordinated water molecules in the asymmetric unit. The structure is stabilized by extensive intra- and intermolecular hydrogen bonding.
Supporting information
CCDC reference: 211910
Key indicators
- Single-crystal X-ray study
- T = 293 K
- Mean (Cr-O) = 0.004 Å
- R factor = 0.048
- wR factor = 0.130
- Data-to-parameter ratio = 11.8
checkCIF/PLATON results
No syntax errors found
Alert level A
PLAT241_ALERT_2_A Check High U(eq) as Compared to Neighbors .... O28
| Author Response: One of the dichromate ions is disordered. We have used EADP to
locate and refine the disordered moiety. O28 belongs to this and hence has
a high U(eq) as compared to Neighbors.
|
PLAT242_ALERT_2_A Check Low U(eq) as Compared to Neighbors .... Cr1
| Author Response: Cr1 is also a part of the disordered dichromate ion
|
Alert level B
PLAT241_ALERT_2_B Check High U(eq) as Compared to Neighbors .... O28A
| Author Response: One of the dichromate ions is disordered. We have used EADP to
locate and refine the disordered moiety. O28 belongs to this and hence has
a high U(eq) as compared to Neighbors.
|
PLAT241_ALERT_2_B Check High U(eq) as Compared to Neighbors .... O17
| Author Response: One of the dichromate ions is disordered. We have used EADP to
locate and refine the disordered moiety. O28 belongs to this and hence has
a high U(eq) as compared to Neighbors.
|
PLAT242_ALERT_2_B Check Low U(eq) as Compared to Neighbors .... Cr2
| Author Response: Cr1 is also a part of the disordered dichromate ion
|
PLAT242_ALERT_2_B Check Low U(eq) as Compared to Neighbors .... Cr3
| Author Response: Cr1 is also a part of the disordered dichromate ion
|
PLAT242_ALERT_2_B Check Low U(eq) as Compared to Neighbors .... Cr4
| Author Response: Cr1 is also a part of the disordered dichromate ion
|
PLAT354_ALERT_3_B Short O-H Bond (0.82A) O9 - H59 = 0.61 Ang.
Alert level C
PLAT042_ALERT_1_C Calc. and Rep. MoietyFormula Strings Differ .... ?
PLAT062_ALERT_4_C Rescale T(min) & T(max) by ..................... 0.98
PLAT213_ALERT_2_C Atom O29A has ADP max/min Ratio ............. 3.40 prolat
PLAT213_ALERT_2_C Atom O29 has ADP max/min Ratio ............. 3.40 prolat
PLAT220_ALERT_2_C Large Non-Solvent O Ueq(max)/Ueq(min) ... 2.57 Ratio
PLAT242_ALERT_2_C Check Low U(eq) as Compared to Neighbors .... Ni2
| Author Response: Cr1 is also a part of the disordered dichromate ion
|
PLAT301_ALERT_3_C Main Residue Disorder ......................... 9.00 Perc.
PLAT354_ALERT_3_C Short O-H Bond (0.82A) O1 - H67 = 0.69 Ang.
PLAT354_ALERT_3_C Short O-H Bond (0.82A) O4 - H53 = 0.71 Ang.
PLAT354_ALERT_3_C Short O-H Bond (0.82A) O5 - H5O = 0.68 Ang.
PLAT354_ALERT_3_C Short O-H Bond (0.82A) O5 - H77 = 0.67 Ang.
PLAT354_ALERT_3_C Short O-H Bond (0.82A) O6 - H51 = 0.68 Ang.
PLAT354_ALERT_3_C Short O-H Bond (0.82A) O11 - H65 = 0.70 Ang.
PLAT354_ALERT_3_C Short O-H Bond (0.82A) O22 - H70 = 0.62 Ang.
PLAT355_ALERT_3_C Long O-H Bond (0.82A) O2 - H57 = 1.06 Ang.
PLAT701_ALERT_1_C Bond Calc 2.035(2), Rep 2.038(2), Dev.. 1.50 Sigma
NI1 -O2 1.555 1.555
PLAT707_ALERT_1_C D...A Calc 2.869(4), Rep 2.874(4), Dev.. 1.25 Sigma
O4 -N6 1.555 3.665
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 H38 Cr2 N8 Ni1 O14
Atom count from _chemical_formula_moiety:H12 Ni1 O62
2 ALERT level A = In general: serious problem
6 ALERT level B = Potentially serious problem
17 ALERT level C = Check and explain
1 ALERT level G = General alerts; check
4 ALERT type 1 CIF construction/syntax error, inconsistent or missing data
11 ALERT type 2 Indicator that the structure model may be wrong or deficient
10 ALERT type 3 Indicator that the structure quality may be low
1 ALERT type 4 Improvement, methodology, query or suggestion
Data collection: SMART (Bruker, 1998); cell refinement: SMART; data reduction: SAINT (Bruker, 1998); program(s) used to solve structure: SIR92 (Altomare et al., 1993); program(s) used to refine structure: SHELXL97 (Sheldrick, 1997); molecular graphics: ORTEP-3 for Windows (Farrugia, 1997) and CAMERON (Watkin et al., 1993); software used to prepare material for publication: PLATON (Spek, 1990).
Hexaaquanickel(II) dichromate bis(hexamethylenetetramine) monohydrate
top
Crystal data top
[Ni(H2O)6][Cr2O7]·2C6H12N4·H2O | F(000) = 2832 |
Mr = 681.19 | Dx = 1.741 Mg m−3 |
Monoclinic, P21/c | Mo Kα radiation, λ = 0.71073 Å |
Hall symbol: -P 2ybc | Cell parameters from 765 reflections |
a = 27.976 (5) Å | θ = 1.5–25.5° |
b = 13.333 (3) Å | µ = 1.62 mm−1 |
c = 14.070 (3) Å | T = 293 K |
β = 97.896 (3)° | Prism, red |
V = 5198.4 (19) Å3 | 0.3 × 0.2 × 0.2 mm |
Z = 8 | |
Data collection top
Bruker SMART CCD area detector diffractometer | 9189 independent reflections |
Radiation source: fine-focus sealed tube | 7533 reflections with I > 2σ(I) |
Graphite monochromator | Rint = 0.036 |
φ and ω scans | θmax = 25.0°, θmin = 0.7° |
Absorption correction: multi-scan (SADABS; Sheldrick, 1996) | h = −33→32 |
Tmin = 0.623, Tmax = 0.738 | k = −15→15 |
37222 measured reflections | l = −16→16 |
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)] = 0.048 | Hydrogen site location: inferred from neighbouring sites |
wR(F2) = 0.130 | H atoms treated by a mixture of independent and constrained refinement |
S = 1.34 | w = 1/[σ2(Fo2) + (0.0611P)2] where P = (Fo2 + 2Fc2)/3 |
9189 reflections | (Δ/σ)max = 0.001 |
779 parameters | Δρmax = 1.09 e Å−3 |
0 restraints | Δρmin = −0.77 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 | Occ. (<1) |
Ni1 | 0.391568 (16) | 0.54262 (3) | 0.22787 (3) | 0.02279 (13) | |
O2 | 0.37522 (9) | 0.5989 (2) | 0.09286 (17) | 0.0307 (6) | |
O1 | 0.31993 (11) | 0.5474 (2) | 0.2475 (2) | 0.0380 (7) | |
O4 | 0.46151 (10) | 0.5342 (2) | 0.1984 (2) | 0.0375 (7) | |
O3 | 0.39802 (11) | 0.6851 (2) | 0.2800 (2) | 0.0350 (7) | |
O5 | 0.41085 (13) | 0.4915 (2) | 0.3666 (2) | 0.0387 (8) | |
N5 | 0.46481 (11) | 0.1781 (2) | −0.0534 (2) | 0.0318 (7) | |
O6 | 0.38135 (10) | 0.3976 (2) | 0.1796 (2) | 0.0329 (7) | |
N10 | 0.28675 (11) | 0.1747 (2) | 0.6107 (2) | 0.0306 (7) | |
N9 | 0.26780 (11) | 0.2955 (2) | 0.4808 (2) | 0.0330 (8) | |
N7 | 0.52548 (11) | 0.2290 (2) | 0.0788 (2) | 0.0299 (7) | |
N6 | 0.50356 (11) | 0.3420 (2) | −0.0560 (2) | 0.0282 (7) | |
O14 | 0.32397 (13) | 0.3747 (2) | 0.3544 (2) | 0.0479 (9) | |
N12 | 0.21580 (11) | 0.2820 (2) | 0.6051 (2) | 0.0336 (8) | |
C10 | 0.54259 (13) | 0.3047 (3) | 0.0161 (3) | 0.0323 (9) | |
H10A | 0.5678 | 0.2759 | −0.0162 | 0.039* | |
H10B | 0.5564 | 0.3604 | 0.0547 | 0.039* | |
N8 | 0.44630 (11) | 0.3093 (2) | 0.0575 (2) | 0.0293 (7) | |
C15 | 0.25677 (14) | 0.1004 (3) | 0.5522 (3) | 0.0354 (9) | |
H15A | 0.2768 | 0.0630 | 0.5138 | 0.043* | |
H15B | 0.2435 | 0.0535 | 0.5942 | 0.043* | |
N11 | 0.21708 (12) | 0.1477 (2) | 0.4885 (2) | 0.0349 (8) | |
C9 | 0.50491 (14) | 0.1449 (3) | 0.0178 (3) | 0.0321 (9) | |
H9A | 0.5299 | 0.1158 | −0.0150 | 0.039* | |
H9B | 0.4936 | 0.0934 | 0.0578 | 0.039* | |
C16 | 0.30591 (14) | 0.2445 (3) | 0.5454 (3) | 0.0351 (9) | |
H16A | 0.3265 | 0.2082 | 0.5073 | 0.042* | |
H16B | 0.3255 | 0.2944 | 0.5826 | 0.042* | |
C12 | 0.48661 (14) | 0.2726 (3) | 0.1265 (2) | 0.0324 (9) | |
H12A | 0.4748 | 0.2222 | 0.1671 | 0.039* | |
H12B | 0.4995 | 0.3276 | 0.1672 | 0.039* | |
C11 | 0.48290 (14) | 0.2558 (3) | −0.1131 (2) | 0.0333 (9) | |
H11A | 0.4567 | 0.2789 | −0.1602 | 0.040* | |
H11B | 0.5074 | 0.2270 | −0.1472 | 0.040* | |
C14 | 0.18707 (14) | 0.2056 (3) | 0.5470 (3) | 0.0362 (9) | |
H14A | 0.1727 | 0.1605 | 0.5890 | 0.043* | |
H14B | 0.1612 | 0.2382 | 0.5053 | 0.043* | |
C8 | 0.42749 (13) | 0.2239 (3) | −0.0028 (3) | 0.0337 (9) | |
H8A | 0.4010 | 0.2465 | −0.0495 | 0.040* | |
H8B | 0.4151 | 0.1736 | 0.0372 | 0.040* | |
C7 | 0.46556 (14) | 0.3832 (3) | −0.0046 (3) | 0.0329 (9) | |
H7A | 0.4786 | 0.4394 | 0.0342 | 0.039* | |
H7B | 0.4394 | 0.4080 | −0.0510 | 0.039* | |
C17 | 0.25544 (14) | 0.2309 (3) | 0.6672 (3) | 0.0359 (9) | |
H17A | 0.2745 | 0.2803 | 0.7061 | 0.043* | |
H17B | 0.2419 | 0.1853 | 0.7100 | 0.043* | |
C13 | 0.23753 (15) | 0.3503 (3) | 0.5401 (3) | 0.0388 (10) | |
H13A | 0.2121 | 0.3849 | 0.4990 | 0.047* | |
H13B | 0.2569 | 0.4003 | 0.5778 | 0.047* | |
C18 | 0.23812 (15) | 0.2185 (3) | 0.4256 (3) | 0.0394 (10) | |
H18A | 0.2124 | 0.2510 | 0.3835 | 0.047* | |
H18B | 0.2579 | 0.1819 | 0.3860 | 0.047* | |
Ni2 | 0.137658 (17) | 0.98700 (4) | 0.22775 (3) | 0.02490 (14) | |
O10 | 0.17281 (13) | 0.9822 (3) | 0.3656 (2) | 0.0484 (9) | |
O7 | 0.07458 (11) | 1.0278 (2) | 0.2712 (2) | 0.0378 (7) | |
O8 | 0.10453 (13) | 0.9836 (3) | 0.0885 (2) | 0.0520 (9) | |
O9 | 0.20288 (12) | 0.9469 (3) | 0.1849 (2) | 0.0442 (8) | |
N3 | 0.04400 (13) | 0.8370 (3) | −0.0155 (2) | 0.0443 (9) | |
O11 | 0.11698 (16) | 0.8451 (3) | 0.2437 (3) | 0.0691 (13) | |
O12 | 0.15619 (13) | 1.1326 (2) | 0.2179 (3) | 0.0482 (9) | |
N2 | −0.01971 (12) | 0.8356 (3) | −0.1517 (2) | 0.0360 (8) | |
C1 | −0.04583 (14) | 0.7607 (3) | −0.1025 (3) | 0.0414 (10) | |
H1A | −0.0650 | 0.7190 | −0.1497 | 0.050* | |
H1B | −0.0676 | 0.7945 | −0.0651 | 0.050* | |
N1 | −0.01254 (13) | 0.6973 (3) | −0.0391 (2) | 0.0442 (9) | |
N4 | 0.04745 (13) | 0.7192 (3) | −0.1467 (2) | 0.0423 (9) | |
C4 | 0.00977 (16) | 0.8976 (3) | −0.0781 (3) | 0.0446 (11) | |
H4A | 0.0271 | 0.9476 | −0.1096 | 0.053* | |
H4B | −0.0113 | 0.9322 | −0.0399 | 0.053* | |
C3 | 0.07477 (15) | 0.7831 (4) | −0.0737 (3) | 0.0472 (11) | |
H3A | 0.0972 | 0.7418 | −0.0322 | 0.057* | |
H3B | 0.0934 | 0.8311 | −0.1051 | 0.057* | |
C5 | 0.01652 (18) | 0.7623 (4) | 0.0315 (3) | 0.0555 (13) | |
H5A | −0.0046 | 0.7964 | 0.0700 | 0.067* | |
H5B | 0.0387 | 0.7213 | 0.0740 | 0.067* | |
C2 | 0.02000 (18) | 0.6474 (3) | −0.0975 (4) | 0.0543 (12) | |
H2A | 0.0422 | 0.6049 | −0.0566 | 0.065* | |
H2B | 0.0013 | 0.6050 | −0.1446 | 0.065* | |
C6 | 0.01305 (15) | 0.7832 (3) | −0.2068 (3) | 0.0437 (11) | |
H6A | 0.0307 | 0.8321 | −0.2392 | 0.052* | |
H6B | −0.0056 | 0.7423 | −0.2553 | 0.052* | |
Cr3 | 0.40602 (2) | 0.95943 (5) | 0.17023 (4) | 0.03159 (17) | |
Cr4 | 0.34395 (2) | 1.04621 (5) | 0.32500 (4) | 0.03467 (18) | |
Cr2 | 0.11436 (3) | 0.41461 (6) | 0.32677 (5) | 0.0516 (2) | |
O26 | 0.1245 (9) | 0.504 (2) | 0.0964 (14) | 0.133 (3) | 0.312 (6) |
O29 | 0.1221 (7) | 0.6759 (14) | 0.148 (2) | 0.166 (4) | 0.312 (6) |
O31 | 0.2033 (8) | 0.584 (2) | 0.1732 (16) | 0.133 (4) | 0.312 (6) |
O26A | 0.1481 (4) | 0.5340 (8) | 0.0720 (6) | 0.133 (3) | 0.688 (6) |
O29A | 0.1507 (3) | 0.6754 (6) | 0.1982 (9) | 0.166 (4) | 0.688 (6) |
O31A | 0.2039 (3) | 0.5202 (8) | 0.2268 (7) | 0.133 (4) | 0.688 (6) |
Cr1 | 0.14826 (4) | 0.56434 (6) | 0.17715 (6) | 0.0649 (3) | |
O23 | 0.0630 (7) | 0.4352 (15) | 0.2913 (16) | 0.091 (3) | 0.312 (6) |
O30 | 0.1282 (6) | 0.4192 (13) | 0.4414 (12) | 0.0650 (18) | 0.312 (6) |
O24 | 0.1284 (9) | 0.2970 (17) | 0.3231 (13) | 0.082 (2) | 0.312 (6) |
O23A | 0.0572 (3) | 0.3931 (6) | 0.3363 (6) | 0.091 (3) | 0.688 (6) |
O30A | 0.1428 (3) | 0.4625 (5) | 0.4232 (5) | 0.0650 (18) | 0.688 (6) |
O24A | 0.1396 (4) | 0.3217 (7) | 0.2865 (5) | 0.082 (2) | 0.688 (6) |
N14 | 0.30194 (11) | 0.7274 (2) | 0.0302 (2) | 0.0330 (8) | |
N15 | 0.22491 (12) | 0.7065 (3) | −0.0722 (2) | 0.0397 (8) | |
N13 | 0.28276 (12) | 0.8311 (2) | −0.1122 (2) | 0.0352 (8) | |
N16 | 0.24063 (11) | 0.8566 (3) | 0.0262 (2) | 0.0344 (8) | |
C20 | 0.32067 (14) | 0.7778 (3) | −0.0495 (3) | 0.0361 (9) | |
H20A | 0.3354 | 0.7284 | −0.0869 | 0.043* | |
H20B | 0.3454 | 0.8251 | −0.0240 | 0.043* | |
C22 | 0.20422 (14) | 0.7825 (3) | −0.0157 (3) | 0.0442 (11) | |
H22A | 0.1902 | 0.7501 | 0.0355 | 0.053* | |
H22B | 0.1786 | 0.8172 | −0.0562 | 0.053* | |
C24 | 0.27917 (14) | 0.8024 (3) | 0.0855 (3) | 0.0351 (9) | |
H24A | 0.2660 | 0.7694 | 0.1375 | 0.042* | |
H24B | 0.3034 | 0.8497 | 0.1134 | 0.042* | |
C19 | 0.26051 (15) | 0.9050 (3) | −0.0530 (3) | 0.0391 (10) | |
H19A | 0.2846 | 0.9537 | −0.0274 | 0.047* | |
H19B | 0.2350 | 0.9404 | −0.0930 | 0.047* | |
C21 | 0.26412 (15) | 0.6566 (3) | −0.0106 (3) | 0.0404 (10) | |
H21A | 0.2784 | 0.6062 | −0.0476 | 0.048* | |
H21B | 0.2511 | 0.6229 | 0.0411 | 0.048* | |
C23 | 0.24573 (16) | 0.7568 (3) | −0.1492 (3) | 0.0428 (11) | |
H23A | 0.2203 | 0.7902 | −0.1912 | 0.051* | |
H23B | 0.2601 | 0.7071 | −0.1868 | 0.051* | |
O20 | 0.40292 (13) | 0.8424 (2) | 0.1497 (2) | 0.0603 (9) | |
O18 | 0.34977 (13) | 1.1619 (2) | 0.3047 (3) | 0.0665 (10) | |
O22 | 0.08147 (17) | 1.0902 (4) | 0.4498 (3) | 0.0808 (14) | |
O15 | 0.35058 (13) | 1.0301 (3) | 0.4396 (2) | 0.0630 (10) | |
O19 | 0.37035 (14) | 1.0176 (3) | 0.0935 (3) | 0.0761 (12) | |
O21 | 0.46026 (14) | 0.9971 (3) | 0.1711 (3) | 0.0843 (14) | |
O17 | 0.39211 (15) | 0.9777 (3) | 0.2875 (3) | 0.0814 (13) | |
O16 | 0.29273 (14) | 1.0079 (4) | 0.2783 (3) | 0.0985 (15) | |
O28 | 0.1337 (5) | 0.5321 (8) | 0.2814 (9) | 0.132 (4) | 0.50 |
O28A | 0.1061 (4) | 0.4884 (9) | 0.2251 (7) | 0.115 (4) | 0.50 |
H5O | 0.4263 (18) | 0.453 (4) | 0.379 (4) | 0.050* | |
H51 | 0.3960 (18) | 0.372 (4) | 0.153 (3) | 0.050* | |
H52 | 0.4854 (17) | 0.522 (3) | 0.232 (3) | 0.050* | |
H53 | 0.4700 (18) | 0.563 (4) | 0.162 (3) | 0.050* | |
H54 | 0.4214 (16) | 0.690 (3) | 0.318 (3) | 0.050* | |
H55 | 0.3985 (16) | 0.730 (4) | 0.242 (3) | 0.050* | |
H56 | 0.3716 (16) | 0.550 (3) | 0.050 (3) | 0.050* | |
H57 | 0.3474 (16) | 0.653 (3) | 0.082 (3) | 0.050* | |
H58 | 0.3127 (16) | 0.588 (4) | 0.286 (3) | 0.050* | |
H59 | 0.2073 (19) | 0.932 (4) | 0.146 (3) | 0.050* | |
H60 | 0.2265 (17) | 0.967 (3) | 0.222 (3) | 0.050* | |
H61 | 0.1681 (17) | 1.151 (3) | 0.172 (3) | 0.050* | |
H62 | 0.0781 (16) | 1.053 (3) | 0.329 (3) | 0.050* | |
H63 | 0.0592 (17) | 1.063 (4) | 0.241 (3) | 0.050* | |
H64 | 0.0980 (17) | 0.836 (3) | 0.280 (3) | 0.050* | |
H65 | 0.1253 (18) | 0.799 (4) | 0.229 (3) | 0.050* | |
H66 | 0.1157 (18) | 1.019 (3) | 0.051 (3) | 0.050* | |
H67 | 0.3177 (19) | 0.500 (4) | 0.266 (4) | 0.050* | |
H68 | 0.3554 (16) | 0.383 (4) | 0.171 (3) | 0.050* | |
H69 | 0.0983 (17) | 1.050 (3) | 0.498 (3) | 0.050* | |
H70 | 0.0672 (19) | 1.111 (4) | 0.473 (4) | 0.050* | |
H71 | 0.1448 (18) | 1.170 (4) | 0.245 (3) | 0.050* | |
H72 | 0.1787 (18) | 1.026 (4) | 0.396 (3) | 0.050* | |
H73 | 0.1706 (17) | 0.924 (3) | 0.385 (3) | 0.050* | |
H74 | 0.3059 (16) | 0.359 (3) | 0.398 (3) | 0.050* | |
H75 | 0.3306 (18) | 0.332 (4) | 0.327 (3) | 0.050* | |
H76 | 0.0890 (17) | 0.930 (4) | 0.077 (3) | 0.050* | |
H77 | 0.3926 (18) | 0.497 (4) | 0.392 (4) | 0.050* | |
Atomic displacement parameters (Å2) top | U11 | U22 | U33 | U12 | U13 | U23 |
Ni1 | 0.0211 (3) | 0.0232 (3) | 0.0237 (2) | −0.00153 (19) | 0.00187 (18) | 0.00110 (18) |
O2 | 0.0291 (15) | 0.0368 (17) | 0.0255 (13) | 0.0026 (13) | 0.0007 (11) | 0.0033 (11) |
O1 | 0.0282 (16) | 0.043 (2) | 0.0451 (18) | −0.0049 (15) | 0.0139 (13) | −0.0082 (14) |
O4 | 0.0205 (15) | 0.053 (2) | 0.0382 (17) | −0.0008 (13) | 0.0027 (12) | 0.0161 (14) |
O3 | 0.0437 (18) | 0.0236 (15) | 0.0351 (15) | −0.0025 (13) | −0.0038 (13) | 0.0013 (12) |
O5 | 0.052 (2) | 0.0357 (19) | 0.0284 (15) | 0.0042 (15) | 0.0063 (14) | 0.0070 (13) |
N5 | 0.0311 (18) | 0.037 (2) | 0.0291 (16) | −0.0016 (15) | 0.0097 (14) | −0.0083 (14) |
O6 | 0.0283 (16) | 0.0294 (16) | 0.0431 (16) | −0.0037 (13) | 0.0124 (13) | −0.0102 (12) |
N10 | 0.0273 (18) | 0.0323 (19) | 0.0334 (17) | 0.0045 (14) | 0.0088 (14) | 0.0038 (14) |
N9 | 0.0316 (19) | 0.0313 (19) | 0.0371 (17) | −0.0009 (14) | 0.0087 (15) | 0.0040 (14) |
N7 | 0.0304 (18) | 0.0305 (18) | 0.0282 (15) | 0.0017 (14) | 0.0022 (13) | 0.0038 (13) |
N6 | 0.0251 (17) | 0.0325 (19) | 0.0279 (16) | 0.0006 (14) | 0.0064 (13) | 0.0064 (13) |
O14 | 0.054 (2) | 0.043 (2) | 0.050 (2) | −0.0075 (17) | 0.0207 (16) | 0.0055 (15) |
N12 | 0.0326 (19) | 0.0306 (19) | 0.0400 (18) | 0.0043 (15) | 0.0133 (15) | −0.0040 (14) |
C10 | 0.026 (2) | 0.036 (2) | 0.035 (2) | −0.0024 (17) | 0.0036 (16) | 0.0018 (17) |
N8 | 0.0272 (17) | 0.0292 (18) | 0.0329 (16) | 0.0001 (14) | 0.0091 (13) | −0.0007 (13) |
C15 | 0.039 (2) | 0.022 (2) | 0.048 (2) | 0.0018 (18) | 0.0146 (19) | −0.0002 (17) |
N11 | 0.0333 (19) | 0.036 (2) | 0.0362 (17) | −0.0068 (15) | 0.0076 (15) | −0.0079 (15) |
C9 | 0.033 (2) | 0.032 (2) | 0.0313 (19) | 0.0055 (18) | 0.0068 (17) | −0.0022 (16) |
C16 | 0.029 (2) | 0.036 (2) | 0.043 (2) | −0.0037 (18) | 0.0111 (17) | 0.0000 (18) |
C12 | 0.040 (2) | 0.035 (2) | 0.0231 (17) | 0.0008 (18) | 0.0085 (16) | −0.0006 (16) |
C11 | 0.029 (2) | 0.050 (3) | 0.0210 (17) | 0.0029 (19) | 0.0063 (15) | 0.0009 (17) |
C14 | 0.025 (2) | 0.042 (3) | 0.043 (2) | −0.0003 (18) | 0.0109 (17) | 0.0000 (19) |
C8 | 0.026 (2) | 0.039 (2) | 0.037 (2) | −0.0052 (18) | 0.0091 (17) | −0.0059 (17) |
C7 | 0.033 (2) | 0.030 (2) | 0.036 (2) | 0.0031 (17) | 0.0056 (17) | 0.0047 (17) |
C17 | 0.037 (2) | 0.040 (2) | 0.0310 (19) | −0.0042 (19) | 0.0048 (17) | −0.0044 (17) |
C13 | 0.039 (2) | 0.030 (2) | 0.049 (2) | 0.0042 (19) | 0.012 (2) | 0.0016 (18) |
C18 | 0.038 (2) | 0.051 (3) | 0.0295 (19) | −0.001 (2) | 0.0055 (18) | 0.0027 (18) |
Ni2 | 0.0234 (3) | 0.0263 (3) | 0.0258 (2) | −0.0016 (2) | 0.00625 (19) | −0.00049 (19) |
O10 | 0.064 (2) | 0.043 (2) | 0.0337 (17) | 0.0107 (18) | −0.0092 (15) | −0.0040 (14) |
O7 | 0.0329 (17) | 0.0464 (19) | 0.0352 (16) | 0.0115 (13) | 0.0091 (13) | 0.0094 (13) |
O8 | 0.051 (2) | 0.071 (3) | 0.0325 (16) | −0.0223 (18) | 0.0008 (14) | −0.0020 (16) |
O9 | 0.0274 (17) | 0.063 (2) | 0.0433 (19) | 0.0000 (15) | 0.0104 (14) | −0.0182 (17) |
N3 | 0.038 (2) | 0.061 (3) | 0.0335 (18) | −0.0058 (18) | 0.0002 (15) | −0.0086 (17) |
O11 | 0.085 (3) | 0.0293 (19) | 0.110 (3) | −0.0145 (19) | 0.071 (2) | −0.009 (2) |
O12 | 0.062 (2) | 0.0290 (18) | 0.062 (2) | −0.0071 (16) | 0.0383 (17) | −0.0044 (15) |
N2 | 0.0319 (19) | 0.041 (2) | 0.0347 (17) | 0.0036 (15) | 0.0013 (14) | 0.0008 (15) |
C1 | 0.028 (2) | 0.049 (3) | 0.047 (2) | −0.001 (2) | 0.0058 (18) | −0.005 (2) |
N1 | 0.039 (2) | 0.047 (2) | 0.049 (2) | 0.0015 (18) | 0.0121 (17) | 0.0141 (18) |
N4 | 0.040 (2) | 0.042 (2) | 0.049 (2) | 0.0068 (17) | 0.0193 (17) | −0.0036 (17) |
C4 | 0.046 (3) | 0.037 (3) | 0.053 (3) | −0.002 (2) | 0.012 (2) | −0.011 (2) |
C3 | 0.027 (2) | 0.060 (3) | 0.055 (3) | 0.004 (2) | 0.004 (2) | 0.011 (2) |
C5 | 0.058 (3) | 0.080 (4) | 0.028 (2) | 0.004 (3) | 0.006 (2) | 0.007 (2) |
C2 | 0.058 (3) | 0.036 (3) | 0.072 (3) | 0.008 (2) | 0.020 (3) | 0.005 (2) |
C6 | 0.054 (3) | 0.050 (3) | 0.029 (2) | −0.005 (2) | 0.0110 (19) | −0.0039 (19) |
Cr3 | 0.0288 (4) | 0.0324 (4) | 0.0343 (3) | −0.0023 (3) | 0.0070 (3) | 0.0006 (3) |
Cr4 | 0.0278 (4) | 0.0420 (4) | 0.0349 (3) | 0.0028 (3) | 0.0066 (3) | −0.0022 (3) |
Cr2 | 0.0663 (6) | 0.0474 (5) | 0.0390 (4) | 0.0133 (4) | 0.0001 (4) | −0.0049 (3) |
O26 | 0.157 (10) | 0.186 (9) | 0.064 (5) | −0.049 (6) | 0.044 (4) | −0.035 (5) |
O29 | 0.105 (8) | 0.064 (4) | 0.314 (14) | 0.027 (5) | −0.031 (7) | −0.088 (6) |
O31 | 0.086 (5) | 0.188 (11) | 0.124 (8) | 0.039 (6) | 0.010 (5) | −0.028 (6) |
O26A | 0.157 (10) | 0.186 (9) | 0.064 (5) | −0.049 (6) | 0.044 (4) | −0.035 (5) |
O29A | 0.105 (8) | 0.064 (4) | 0.314 (14) | 0.027 (5) | −0.031 (7) | −0.088 (6) |
O31A | 0.086 (5) | 0.188 (11) | 0.124 (8) | 0.039 (6) | 0.010 (5) | −0.028 (6) |
Cr1 | 0.0900 (7) | 0.0467 (5) | 0.0630 (5) | −0.0152 (5) | 0.0280 (5) | −0.0216 (4) |
O23 | 0.054 (3) | 0.087 (7) | 0.136 (8) | −0.014 (4) | 0.030 (4) | −0.031 (5) |
O30 | 0.063 (5) | 0.076 (6) | 0.056 (3) | −0.001 (3) | 0.009 (3) | −0.024 (3) |
O24 | 0.115 (6) | 0.066 (5) | 0.065 (6) | 0.035 (4) | 0.016 (4) | −0.021 (4) |
O23A | 0.054 (3) | 0.087 (7) | 0.136 (8) | −0.014 (4) | 0.030 (4) | −0.031 (5) |
O30A | 0.063 (5) | 0.076 (6) | 0.056 (3) | −0.001 (3) | 0.009 (3) | −0.024 (3) |
O24A | 0.115 (6) | 0.066 (5) | 0.065 (6) | 0.035 (4) | 0.016 (4) | −0.021 (4) |
N14 | 0.0307 (18) | 0.037 (2) | 0.0316 (16) | 0.0041 (15) | 0.0034 (14) | 0.0010 (14) |
N15 | 0.034 (2) | 0.044 (2) | 0.0381 (18) | −0.0093 (16) | −0.0027 (15) | −0.0038 (16) |
N13 | 0.036 (2) | 0.034 (2) | 0.0360 (18) | 0.0041 (15) | 0.0085 (15) | 0.0053 (14) |
N16 | 0.0277 (18) | 0.039 (2) | 0.0379 (18) | 0.0022 (15) | 0.0078 (14) | −0.0046 (14) |
C20 | 0.026 (2) | 0.043 (3) | 0.040 (2) | 0.0049 (18) | 0.0073 (17) | −0.0033 (18) |
C22 | 0.023 (2) | 0.059 (3) | 0.051 (2) | −0.001 (2) | 0.0040 (19) | 0.000 (2) |
C24 | 0.033 (2) | 0.042 (2) | 0.0308 (19) | −0.0015 (19) | 0.0044 (17) | −0.0058 (17) |
C19 | 0.038 (2) | 0.032 (2) | 0.047 (2) | 0.0055 (19) | 0.0086 (19) | 0.0041 (19) |
C21 | 0.047 (3) | 0.032 (2) | 0.041 (2) | −0.0018 (19) | 0.003 (2) | 0.0028 (18) |
C23 | 0.046 (3) | 0.049 (3) | 0.031 (2) | 0.001 (2) | −0.0038 (18) | −0.0013 (19) |
O20 | 0.078 (3) | 0.038 (2) | 0.065 (2) | 0.0050 (17) | 0.0104 (18) | 0.0039 (16) |
O18 | 0.078 (3) | 0.042 (2) | 0.075 (2) | 0.0035 (18) | −0.006 (2) | 0.0054 (17) |
O22 | 0.075 (3) | 0.108 (4) | 0.060 (3) | 0.033 (3) | 0.013 (2) | −0.027 (2) |
O15 | 0.062 (2) | 0.080 (3) | 0.0489 (19) | 0.0076 (19) | 0.0149 (17) | 0.0128 (17) |
O19 | 0.082 (3) | 0.062 (2) | 0.076 (3) | 0.000 (2) | −0.016 (2) | 0.021 (2) |
O21 | 0.058 (2) | 0.133 (4) | 0.059 (2) | −0.053 (2) | −0.0042 (19) | 0.010 (2) |
O17 | 0.088 (3) | 0.104 (3) | 0.057 (2) | 0.046 (2) | 0.027 (2) | 0.008 (2) |
O16 | 0.054 (3) | 0.127 (4) | 0.105 (3) | −0.031 (3) | −0.024 (2) | −0.009 (3) |
O28 | 0.213 (15) | 0.080 (8) | 0.114 (9) | −0.005 (8) | 0.063 (9) | −0.004 (6) |
O28A | 0.098 (8) | 0.162 (11) | 0.075 (6) | −0.064 (7) | −0.029 (5) | 0.058 (6) |
Geometric parameters (Å, º) top
Ni1—O2 | 2.038 (2) | O9—H60 | 0.83 (4) |
Ni1—O3 | 2.038 (3) | N3—C4 | 1.455 (5) |
Ni1—O6 | 2.059 (3) | N3—C3 | 1.459 (5) |
Ni1—O4 | 2.061 (3) | N3—C5 | 1.472 (6) |
Ni1—O1 | 2.064 (3) | O11—H64 | 0.79 (5) |
Ni1—O5 | 2.070 (3) | O11—H65 | 0.71 (5) |
O2—H56 | 0.89 (5) | O12—H61 | 0.81 (5) |
O2—H57 | 1.05 (4) | O12—H71 | 0.73 (5) |
O1—H58 | 0.82 (5) | N2—C6 | 1.459 (5) |
O1—H67 | 0.69 (5) | N2—C1 | 1.467 (5) |
O4—H52 | 0.78 (4) | N2—C4 | 1.485 (5) |
O4—H53 | 0.72 (5) | C1—N1 | 1.468 (5) |
O3—H54 | 0.79 (4) | C1—H1A | 0.970 |
O3—H55 | 0.80 (5) | C1—H1B | 0.970 |
O5—H5O | 0.68 (5) | N1—C2 | 1.469 (6) |
O5—H77 | 0.67 (5) | N1—C5 | 1.477 (6) |
N5—C9 | 1.468 (5) | N4—C2 | 1.462 (6) |
N5—C11 | 1.468 (5) | N4—C6 | 1.466 (5) |
N5—C8 | 1.476 (5) | N4—C3 | 1.468 (5) |
O6—H51 | 0.69 (5) | C4—H4A | 0.970 |
O6—H68 | 0.75 (4) | C4—H4B | 0.970 |
N10—C16 | 1.463 (5) | C3—H3A | 0.970 |
N10—C17 | 1.469 (5) | C3—H3B | 0.970 |
N10—C15 | 1.477 (5) | C5—H5A | 0.970 |
N9—C13 | 1.466 (5) | C5—H5B | 0.970 |
N9—C16 | 1.471 (5) | C2—H2A | 0.970 |
N9—C18 | 1.475 (5) | C2—H2B | 0.970 |
N7—C10 | 1.466 (5) | C6—H6A | 0.970 |
N7—C12 | 1.475 (5) | C6—H6B | 0.970 |
N7—C9 | 1.483 (5) | Cr3—O19 | 1.573 (3) |
N6—C10 | 1.473 (4) | Cr3—O20 | 1.590 (3) |
N6—C7 | 1.474 (5) | Cr3—O21 | 1.599 (3) |
N6—C11 | 1.476 (5) | Cr3—O17 | 1.765 (4) |
O14—H74 | 0.87 (5) | Cr4—O16 | 1.579 (4) |
O14—H75 | 0.73 (5) | Cr4—O18 | 1.583 (3) |
N12—C14 | 1.475 (5) | Cr4—O15 | 1.615 (3) |
N12—C13 | 1.481 (5) | Cr4—O17 | 1.770 (4) |
N12—C17 | 1.482 (5) | Cr2—O23 | 1.48 (2) |
C10—H10A | 0.970 | Cr2—O24A | 1.572 (8) |
C10—H10B | 0.970 | Cr2—O30 | 1.609 (16) |
N8—C7 | 1.468 (5) | Cr2—O30A | 1.609 (6) |
N8—C12 | 1.470 (5) | Cr2—O24 | 1.62 (2) |
N8—C8 | 1.476 (5) | Cr2—O23A | 1.652 (7) |
C15—N11 | 1.472 (5) | Cr2—O28A | 1.728 (8) |
C15—H15A | 0.970 | Cr2—O28 | 1.804 (11) |
C15—H15B | 0.970 | O26—Cr1 | 1.48 (2) |
N11—C18 | 1.473 (5) | O29—Cr1 | 1.69 (2) |
N11—C14 | 1.475 (5) | O31—Cr1 | 1.57 (2) |
C9—H9A | 0.970 | O26A—Cr1 | 1.536 (8) |
C9—H9B | 0.970 | O29A—Cr1 | 1.511 (7) |
C16—H16A | 0.970 | O31A—Cr1 | 1.724 (9) |
C16—H16B | 0.970 | Cr1—O28 | 1.635 (11) |
C12—H12A | 0.970 | Cr1—O28A | 1.761 (9) |
C12—H12B | 0.970 | O23—O28A | 1.77 (2) |
C11—H11A | 0.970 | N14—C20 | 1.467 (5) |
C11—H11B | 0.970 | N14—C24 | 1.467 (5) |
C14—H14A | 0.970 | N14—C21 | 1.476 (5) |
C14—H14B | 0.970 | N15—C22 | 1.458 (5) |
C8—H8A | 0.970 | N15—C21 | 1.463 (5) |
C8—H8B | 0.970 | N15—C23 | 1.464 (5) |
C7—H7A | 0.970 | N13—C20 | 1.468 (5) |
C7—H7B | 0.970 | N13—C23 | 1.477 (5) |
C17—H17A | 0.970 | N13—C19 | 1.484 (5) |
C17—H17B | 0.970 | N16—C24 | 1.463 (5) |
C13—H13A | 0.970 | N16—C19 | 1.464 (5) |
C13—H13B | 0.970 | N16—C22 | 1.484 (5) |
C18—H18A | 0.970 | C20—H20A | 0.970 |
C18—H18B | 0.970 | C20—H20B | 0.970 |
Ni2—O11 | 2.002 (3) | C22—H22A | 0.970 |
Ni2—O12 | 2.022 (3) | C22—H22B | 0.970 |
Ni2—O7 | 2.023 (3) | C24—H24A | 0.970 |
Ni2—O8 | 2.052 (3) | C24—H24B | 0.970 |
Ni2—O10 | 2.054 (3) | C19—H19A | 0.970 |
Ni2—O9 | 2.072 (3) | C19—H19B | 0.970 |
O10—H72 | 0.73 (5) | C21—H21A | 0.970 |
O10—H73 | 0.82 (4) | C21—H21B | 0.970 |
O7—H62 | 0.87 (5) | C23—H23A | 0.970 |
O7—H63 | 0.73 (5) | C23—H23B | 0.970 |
O8—H66 | 0.81 (5) | O22—H69 | 0.94 (4) |
O8—H76 | 0.85 (5) | O22—H70 | 0.62 (5) |
O9—H59 | 0.61 (5) | O28—O28A | 1.184 (14) |
| | | |
O2—Ni1—O3 | 89.39 (12) | H62—O7—H63 | 106 (5) |
O2—Ni1—O6 | 92.01 (12) | Ni2—O8—H66 | 117 (3) |
O3—Ni1—O6 | 176.43 (12) | Ni2—O8—H76 | 111 (3) |
O2—Ni1—O4 | 85.99 (11) | H66—O8—H76 | 128 (5) |
O3—Ni1—O4 | 94.81 (13) | Ni2—O9—H59 | 130 (5) |
O6—Ni1—O4 | 88.56 (12) | Ni2—O9—H60 | 113 (3) |
O2—Ni1—O1 | 90.91 (12) | H59—O9—H60 | 115 (6) |
O3—Ni1—O1 | 87.86 (12) | C4—N3—C3 | 108.9 (3) |
O6—Ni1—O1 | 88.84 (12) | C4—N3—C5 | 107.9 (4) |
O4—Ni1—O1 | 175.88 (13) | C3—N3—C5 | 107.7 (4) |
O2—Ni1—O5 | 176.94 (13) | Ni2—O11—H64 | 116 (3) |
O3—Ni1—O5 | 88.22 (12) | Ni2—O11—H65 | 133 (4) |
O6—Ni1—O5 | 90.48 (13) | H64—O11—H65 | 110 (5) |
O4—Ni1—O5 | 92.31 (13) | Ni2—O12—H61 | 120 (3) |
O1—Ni1—O5 | 90.91 (13) | Ni2—O12—H71 | 119 (4) |
Ni1—O2—H56 | 110 (3) | H61—O12—H71 | 118 (5) |
Ni1—O2—H57 | 117 (2) | C6—N2—C1 | 108.4 (3) |
H56—O2—H57 | 113 (4) | C6—N2—C4 | 108.0 (3) |
Ni1—O1—H58 | 116 (3) | C1—N2—C4 | 108.4 (3) |
Ni1—O1—H67 | 99 (5) | N2—C1—N1 | 111.3 (3) |
H58—O1—H67 | 109 (6) | N2—C1—H1A | 109.4 |
Ni1—O4—H52 | 131 (4) | N1—C1—H1A | 109.4 |
Ni1—O4—H53 | 122 (4) | N2—C1—H1B | 109.4 |
H52—O4—H53 | 102 (5) | N1—C1—H1B | 109.4 |
Ni1—O3—H54 | 110 (3) | H1A—C1—H1B | 108.0 |
Ni1—O3—H55 | 117 (3) | C1—N1—C2 | 108.2 (3) |
H54—O3—H55 | 108 (5) | C1—N1—C5 | 108.5 (4) |
Ni1—O5—H5O | 124 (4) | C2—N1—C5 | 108.5 (4) |
Ni1—O5—H77 | 111 (5) | C2—N4—C6 | 108.0 (3) |
H5O—O5—H77 | 117 (6) | C2—N4—C3 | 107.9 (4) |
C9—N5—C11 | 108.2 (3) | C6—N4—C3 | 107.7 (3) |
C9—N5—C8 | 108.8 (3) | N3—C4—N2 | 111.7 (3) |
C11—N5—C8 | 107.9 (3) | N3—C4—H4A | 109.3 |
Ni1—O6—H51 | 126 (4) | N2—C4—H4A | 109.3 |
Ni1—O6—H68 | 113 (4) | N3—C4—H4B | 109.3 |
H51—O6—H68 | 115 (6) | N2—C4—H4B | 109.3 |
C16—N10—C17 | 108.3 (3) | H4A—C4—H4B | 107.9 |
C16—N10—C15 | 107.8 (3) | N3—C3—N4 | 112.9 (3) |
C17—N10—C15 | 108.0 (3) | N3—C3—H3A | 109.0 |
C13—N9—C16 | 107.8 (3) | N4—C3—H3A | 109.0 |
C13—N9—C18 | 108.7 (3) | N3—C3—H3B | 109.0 |
C16—N9—C18 | 108.2 (3) | N4—C3—H3B | 109.0 |
C10—N7—C12 | 109.0 (3) | H3A—C3—H3B | 107.8 |
C10—N7—C9 | 107.8 (3) | N3—C5—N1 | 111.6 (3) |
C12—N7—C9 | 108.1 (3) | N3—C5—H5A | 109.3 |
C10—N6—C7 | 107.8 (3) | N1—C5—H5A | 109.3 |
C10—N6—C11 | 108.1 (3) | N3—C5—H5B | 109.3 |
C7—N6—C11 | 107.7 (3) | N1—C5—H5B | 109.3 |
H74—O14—H75 | 113 (5) | H5A—C5—H5B | 108.0 |
C14—N12—C13 | 108.8 (3) | N4—C2—N1 | 112.0 (4) |
C14—N12—C17 | 108.5 (3) | N4—C2—H2A | 109.2 |
C13—N12—C17 | 108.1 (3) | N1—C2—H2A | 109.2 |
N7—C10—N6 | 112.0 (3) | N4—C2—H2B | 109.2 |
N7—C10—H10A | 109.2 | N1—C2—H2B | 109.2 |
N6—C10—H10A | 109.2 | H2A—C2—H2B | 107.9 |
N7—C10—H10B | 109.2 | N2—C6—N4 | 112.6 (3) |
N6—C10—H10B | 109.2 | N2—C6—H6A | 109.1 |
H10A—C10—H10B | 107.9 | N4—C6—H6A | 109.1 |
C7—N8—C12 | 107.8 (3) | N2—C6—H6B | 109.1 |
C7—N8—C8 | 108.0 (3) | N4—C6—H6B | 109.1 |
C12—N8—C8 | 107.7 (3) | H6A—C6—H6B | 107.8 |
N11—C15—N10 | 112.1 (3) | O19—Cr3—O20 | 110.27 (19) |
N11—C15—H15A | 109.2 | O19—Cr3—O21 | 111.3 (2) |
N10—C15—H15A | 109.2 | O20—Cr3—O21 | 109.8 (2) |
N11—C15—H15B | 109.2 | O19—Cr3—O17 | 112.0 (2) |
N10—C15—H15B | 109.2 | O20—Cr3—O17 | 107.03 (19) |
H15A—C15—H15B | 107.9 | O21—Cr3—O17 | 106.3 (2) |
C15—N11—C18 | 108.1 (3) | O16—Cr4—O18 | 110.5 (2) |
C15—N11—C14 | 109.0 (3) | O16—Cr4—O15 | 110.3 (2) |
C18—N11—C14 | 107.8 (3) | O18—Cr4—O15 | 108.07 (19) |
N5—C9—N7 | 111.5 (3) | O16—Cr4—O17 | 113.3 (2) |
N5—C9—H9A | 109.3 | O18—Cr4—O17 | 110.4 (2) |
N7—C9—H9A | 109.3 | O15—Cr4—O17 | 104.01 (18) |
N5—C9—H9B | 109.3 | O23—Cr2—O30 | 114.8 (10) |
N7—C9—H9B | 109.3 | O24A—Cr2—O30A | 115.1 (4) |
H9A—C9—H9B | 108.0 | O23—Cr2—O24 | 113.4 (12) |
N10—C16—N9 | 112.7 (3) | O30—Cr2—O24 | 92.5 (9) |
N10—C16—H16A | 109.0 | O24A—Cr2—O23A | 112.4 (5) |
N9—C16—H16A | 109.0 | O30A—Cr2—O23A | 111.9 (4) |
N10—C16—H16B | 109.0 | O24A—Cr2—O28A | 99.6 (5) |
N9—C16—H16B | 109.0 | O30A—Cr2—O28A | 117.9 (4) |
H16A—C16—H16B | 107.8 | O23A—Cr2—O28A | 98.3 (4) |
N8—C12—N7 | 112.2 (3) | O23—Cr2—O28 | 92.6 (9) |
N8—C12—H12A | 109.2 | O30—Cr2—O28 | 106.2 (7) |
N7—C12—H12A | 109.2 | O24—Cr2—O28 | 138.1 (8) |
N8—C12—H12B | 109.2 | O29A—Cr1—O26A | 116.2 (6) |
N7—C12—H12B | 109.2 | O26—Cr1—O31 | 113.8 (12) |
H12A—C12—H12B | 107.9 | O26—Cr1—O28 | 114.0 (9) |
N5—C11—N6 | 112.3 (3) | O31—Cr1—O28 | 116.2 (9) |
N5—C11—H11A | 109.2 | O26—Cr1—O29 | 99.2 (14) |
N6—C11—H11A | 109.2 | O31—Cr1—O29 | 103.9 (12) |
N5—C11—H11B | 109.2 | O28—Cr1—O29 | 107.4 (11) |
N6—C11—H11B | 109.2 | O29A—Cr1—O31A | 104.0 (5) |
H11A—C11—H11B | 107.9 | O26A—Cr1—O31A | 100.6 (5) |
N11—C14—N12 | 111.3 (3) | O29A—Cr1—O28A | 120.3 (6) |
N11—C14—H14A | 109.4 | O26A—Cr1—O28A | 107.8 (5) |
N12—C14—H14A | 109.4 | O31A—Cr1—O28A | 105.4 (5) |
N11—C14—H14B | 109.4 | C20—N14—C24 | 108.7 (3) |
N12—C14—H14B | 109.4 | C20—N14—C21 | 107.9 (3) |
H14A—C14—H14B | 108.0 | C24—N14—C21 | 107.6 (3) |
N8—C8—N5 | 112.2 (3) | C22—N15—C21 | 108.4 (3) |
N8—C8—H8A | 109.2 | C22—N15—C23 | 108.3 (3) |
N5—C8—H8A | 109.2 | C21—N15—C23 | 107.8 (3) |
N8—C8—H8B | 109.2 | C20—N13—C23 | 107.6 (3) |
N5—C8—H8B | 109.2 | C20—N13—C19 | 108.0 (3) |
H8A—C8—H8B | 107.9 | C23—N13—C19 | 108.4 (3) |
N8—C7—N6 | 113.0 (3) | C24—N16—C19 | 109.0 (3) |
N8—C7—H7A | 109.0 | C24—N16—C22 | 108.1 (3) |
N6—C7—H7A | 109.0 | C19—N16—C22 | 107.7 (3) |
N8—C7—H7B | 109.0 | N14—C20—N13 | 112.2 (3) |
N6—C7—H7B | 109.0 | N14—C20—H20A | 109.2 |
H7A—C7—H7B | 107.8 | N13—C20—H20A | 109.2 |
N10—C17—N12 | 111.7 (3) | N14—C20—H20B | 109.2 |
N10—C17—H17A | 109.3 | N13—C20—H20B | 109.2 |
N12—C17—H17A | 109.3 | H20A—C20—H20B | 107.9 |
N10—C17—H17B | 109.3 | N15—C22—N16 | 112.2 (3) |
N12—C17—H17B | 109.3 | N15—C22—H22A | 109.2 |
H17A—C17—H17B | 107.9 | N16—C22—H22A | 109.2 |
N9—C13—N12 | 111.3 (3) | N15—C22—H22B | 109.2 |
N9—C13—H13A | 109.4 | N16—C22—H22B | 109.2 |
N12—C13—H13A | 109.4 | H22A—C22—H22B | 107.9 |
N9—C13—H13B | 109.4 | N16—C24—N14 | 112.0 (3) |
N12—C13—H13B | 109.4 | N16—C24—H24A | 109.2 |
H13A—C13—H13B | 108.0 | N14—C24—H24A | 109.2 |
N11—C18—N9 | 111.9 (3) | N16—C24—H24B | 109.2 |
N11—C18—H18A | 109.2 | N14—C24—H24B | 109.2 |
N9—C18—H18A | 109.2 | H24A—C24—H24B | 107.9 |
N11—C18—H18B | 109.2 | N16—C19—N13 | 111.6 (3) |
N9—C18—H18B | 109.2 | N16—C19—H19A | 109.3 |
H18A—C18—H18B | 107.9 | N13—C19—H19A | 109.3 |
O11—Ni2—O12 | 176.57 (14) | N16—C19—H19B | 109.3 |
O11—Ni2—O7 | 86.73 (14) | N13—C19—H19B | 109.3 |
O12—Ni2—O7 | 90.28 (13) | H19A—C19—H19B | 108.0 |
O11—Ni2—O8 | 89.23 (18) | N15—C21—N14 | 112.3 (3) |
O12—Ni2—O8 | 92.43 (15) | N15—C21—H21A | 109.1 |
O7—Ni2—O8 | 89.78 (14) | N14—C21—H21A | 109.1 |
O11—Ni2—O10 | 88.46 (17) | N15—C21—H21B | 109.1 |
O12—Ni2—O10 | 90.02 (15) | N14—C21—H21B | 109.1 |
O7—Ni2—O10 | 92.72 (13) | H21A—C21—H21B | 107.9 |
O8—Ni2—O10 | 176.49 (15) | N15—C23—N13 | 112.2 (3) |
O11—Ni2—O9 | 93.91 (16) | N15—C23—H23A | 109.2 |
O12—Ni2—O9 | 89.06 (14) | N13—C23—H23A | 109.2 |
O7—Ni2—O9 | 179.03 (14) | N15—C23—H23B | 109.2 |
O8—Ni2—O9 | 90.97 (14) | N13—C23—H23B | 109.2 |
O10—Ni2—O9 | 86.56 (14) | H23A—C23—H23B | 107.9 |
Ni2—O10—H72 | 124 (4) | H69—O22—H70 | 100 (6) |
Ni2—O10—H73 | 107 (3) | Cr3—O17—Cr4 | 128.8 (2) |
H72—O10—H73 | 126 (5) | Cr1—O28—Cr2 | 132.1 (7) |
Ni2—O7—H62 | 113 (3) | Cr2—O28A—Cr1 | 128.7 (5) |
Ni2—O7—H63 | 118 (4) | | |
Hydrogen-bond geometry (Å, º) top
D—H···A | D—H | H···A | D···A | D—H···A |
O4—H53···N6i | 0.72 (5) | 2.16 (5) | 2.874 (4) | 177 (3) |
O11—H64···N4ii | 0.79 (5) | 2.01 (5) | 2.782 (6) | 166 (4) |
O10—H73···N15ii | 0.82 (5) | 2.34 (5) | 2.982 (5) | 135 (4) |
O1—H58···N13ii | 0.82 (5) | 2.06 (5) | 2.862 (5) | 168 (5) |
O12—H61···N12iii | 0.81 (5) | 1.95 (5) | 2.710 (5) | 156 (4) |
O7—H63···N2iv | 0.73 (5) | 2.06 (5) | 2.795 (4) | 176 (5) |
O22—H70···N1v | 0.62 (6) | 2.22 (6) | 2.833 (6) | 172 (6) |
Symmetry codes: (i) −x+1, −y+1, −z; (ii) x, −y+3/2, z+1/2; (iii) x, −y+3/2, z−1/2; (iv) −x, −y+2, −z; (v) −x, y+1/2, −z+1/2. |