Download citation
Download citation
link to html
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

cif

Crystallographic Information File (CIF) https://doi.org/10.1107/S1600536803024875/cf6280sup1.cif
Contains datablocks global, I

hkl

Structure factor file (CIF format) https://doi.org/10.1107/S1600536803024875/cf6280Isup2.hkl
Contains datablock I

CCDC reference: 211910

Key indicators

  • Single-crystal X-ray study
  • T = 293 K
  • Mean [sigma](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

Computing details top

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·H2OF(000) = 2832
Mr = 681.19Dx = 1.741 Mg m3
Monoclinic, P21/cMo Kα radiation, λ = 0.71073 Å
Hall symbol: -P 2ybcCell parameters from 765 reflections
a = 27.976 (5) Åθ = 1.5–25.5°
b = 13.333 (3) ŵ = 1.62 mm1
c = 14.070 (3) ÅT = 293 K
β = 97.896 (3)°Prism, red
V = 5198.4 (19) Å30.3 × 0.2 × 0.2 mm
Z = 8
Data collection top
Bruker SMART CCD area detector
diffractometer
9189 independent reflections
Radiation source: fine-focus sealed tube7533 reflections with I > 2σ(I)
Graphite monochromatorRint = 0.036
φ and ω scansθmax = 25.0°, θmin = 0.7°
Absorption correction: multi-scan
(SADABS; Sheldrick, 1996)
h = 3332
Tmin = 0.623, Tmax = 0.738k = 1515
37222 measured reflectionsl = 1616
Refinement top
Refinement on F2Primary atom site location: structure-invariant direct methods
Least-squares matrix: fullSecondary atom site location: difference Fourier map
R[F2 > 2σ(F2)] = 0.048Hydrogen site location: inferred from neighbouring sites
wR(F2) = 0.130H 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 parametersΔρmax = 1.09 e Å3
0 restraintsΔρmin = 0.77 e Å3
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
xyzUiso*/UeqOcc. (<1)
Ni10.391568 (16)0.54262 (3)0.22787 (3)0.02279 (13)
O20.37522 (9)0.5989 (2)0.09286 (17)0.0307 (6)
O10.31993 (11)0.5474 (2)0.2475 (2)0.0380 (7)
O40.46151 (10)0.5342 (2)0.1984 (2)0.0375 (7)
O30.39802 (11)0.6851 (2)0.2800 (2)0.0350 (7)
O50.41085 (13)0.4915 (2)0.3666 (2)0.0387 (8)
N50.46481 (11)0.1781 (2)0.0534 (2)0.0318 (7)
O60.38135 (10)0.3976 (2)0.1796 (2)0.0329 (7)
N100.28675 (11)0.1747 (2)0.6107 (2)0.0306 (7)
N90.26780 (11)0.2955 (2)0.4808 (2)0.0330 (8)
N70.52548 (11)0.2290 (2)0.0788 (2)0.0299 (7)
N60.50356 (11)0.3420 (2)0.0560 (2)0.0282 (7)
O140.32397 (13)0.3747 (2)0.3544 (2)0.0479 (9)
N120.21580 (11)0.2820 (2)0.6051 (2)0.0336 (8)
C100.54259 (13)0.3047 (3)0.0161 (3)0.0323 (9)
H10A0.56780.27590.01620.039*
H10B0.55640.36040.05470.039*
N80.44630 (11)0.3093 (2)0.0575 (2)0.0293 (7)
C150.25677 (14)0.1004 (3)0.5522 (3)0.0354 (9)
H15A0.27680.06300.51380.043*
H15B0.24350.05350.59420.043*
N110.21708 (12)0.1477 (2)0.4885 (2)0.0349 (8)
C90.50491 (14)0.1449 (3)0.0178 (3)0.0321 (9)
H9A0.52990.11580.01500.039*
H9B0.49360.09340.05780.039*
C160.30591 (14)0.2445 (3)0.5454 (3)0.0351 (9)
H16A0.32650.20820.50730.042*
H16B0.32550.29440.58260.042*
C120.48661 (14)0.2726 (3)0.1265 (2)0.0324 (9)
H12A0.47480.22220.16710.039*
H12B0.49950.32760.16720.039*
C110.48290 (14)0.2558 (3)0.1131 (2)0.0333 (9)
H11A0.45670.27890.16020.040*
H11B0.50740.22700.14720.040*
C140.18707 (14)0.2056 (3)0.5470 (3)0.0362 (9)
H14A0.17270.16050.58900.043*
H14B0.16120.23820.50530.043*
C80.42749 (13)0.2239 (3)0.0028 (3)0.0337 (9)
H8A0.40100.24650.04950.040*
H8B0.41510.17360.03720.040*
C70.46556 (14)0.3832 (3)0.0046 (3)0.0329 (9)
H7A0.47860.43940.03420.039*
H7B0.43940.40800.05100.039*
C170.25544 (14)0.2309 (3)0.6672 (3)0.0359 (9)
H17A0.27450.28030.70610.043*
H17B0.24190.18530.71000.043*
C130.23753 (15)0.3503 (3)0.5401 (3)0.0388 (10)
H13A0.21210.38490.49900.047*
H13B0.25690.40030.57780.047*
C180.23812 (15)0.2185 (3)0.4256 (3)0.0394 (10)
H18A0.21240.25100.38350.047*
H18B0.25790.18190.38600.047*
Ni20.137658 (17)0.98700 (4)0.22775 (3)0.02490 (14)
O100.17281 (13)0.9822 (3)0.3656 (2)0.0484 (9)
O70.07458 (11)1.0278 (2)0.2712 (2)0.0378 (7)
O80.10453 (13)0.9836 (3)0.0885 (2)0.0520 (9)
O90.20288 (12)0.9469 (3)0.1849 (2)0.0442 (8)
N30.04400 (13)0.8370 (3)0.0155 (2)0.0443 (9)
O110.11698 (16)0.8451 (3)0.2437 (3)0.0691 (13)
O120.15619 (13)1.1326 (2)0.2179 (3)0.0482 (9)
N20.01971 (12)0.8356 (3)0.1517 (2)0.0360 (8)
C10.04583 (14)0.7607 (3)0.1025 (3)0.0414 (10)
H1A0.06500.71900.14970.050*
H1B0.06760.79450.06510.050*
N10.01254 (13)0.6973 (3)0.0391 (2)0.0442 (9)
N40.04745 (13)0.7192 (3)0.1467 (2)0.0423 (9)
C40.00977 (16)0.8976 (3)0.0781 (3)0.0446 (11)
H4A0.02710.94760.10960.053*
H4B0.01130.93220.03990.053*
C30.07477 (15)0.7831 (4)0.0737 (3)0.0472 (11)
H3A0.09720.74180.03220.057*
H3B0.09340.83110.10510.057*
C50.01652 (18)0.7623 (4)0.0315 (3)0.0555 (13)
H5A0.00460.79640.07000.067*
H5B0.03870.72130.07400.067*
C20.02000 (18)0.6474 (3)0.0975 (4)0.0543 (12)
H2A0.04220.60490.05660.065*
H2B0.00130.60500.14460.065*
C60.01305 (15)0.7832 (3)0.2068 (3)0.0437 (11)
H6A0.03070.83210.23920.052*
H6B0.00560.74230.25530.052*
Cr30.40602 (2)0.95943 (5)0.17023 (4)0.03159 (17)
Cr40.34395 (2)1.04621 (5)0.32500 (4)0.03467 (18)
Cr20.11436 (3)0.41461 (6)0.32677 (5)0.0516 (2)
O260.1245 (9)0.504 (2)0.0964 (14)0.133 (3)0.312 (6)
O290.1221 (7)0.6759 (14)0.148 (2)0.166 (4)0.312 (6)
O310.2033 (8)0.584 (2)0.1732 (16)0.133 (4)0.312 (6)
O26A0.1481 (4)0.5340 (8)0.0720 (6)0.133 (3)0.688 (6)
O29A0.1507 (3)0.6754 (6)0.1982 (9)0.166 (4)0.688 (6)
O31A0.2039 (3)0.5202 (8)0.2268 (7)0.133 (4)0.688 (6)
Cr10.14826 (4)0.56434 (6)0.17715 (6)0.0649 (3)
O230.0630 (7)0.4352 (15)0.2913 (16)0.091 (3)0.312 (6)
O300.1282 (6)0.4192 (13)0.4414 (12)0.0650 (18)0.312 (6)
O240.1284 (9)0.2970 (17)0.3231 (13)0.082 (2)0.312 (6)
O23A0.0572 (3)0.3931 (6)0.3363 (6)0.091 (3)0.688 (6)
O30A0.1428 (3)0.4625 (5)0.4232 (5)0.0650 (18)0.688 (6)
O24A0.1396 (4)0.3217 (7)0.2865 (5)0.082 (2)0.688 (6)
N140.30194 (11)0.7274 (2)0.0302 (2)0.0330 (8)
N150.22491 (12)0.7065 (3)0.0722 (2)0.0397 (8)
N130.28276 (12)0.8311 (2)0.1122 (2)0.0352 (8)
N160.24063 (11)0.8566 (3)0.0262 (2)0.0344 (8)
C200.32067 (14)0.7778 (3)0.0495 (3)0.0361 (9)
H20A0.33540.72840.08690.043*
H20B0.34540.82510.02400.043*
C220.20422 (14)0.7825 (3)0.0157 (3)0.0442 (11)
H22A0.19020.75010.03550.053*
H22B0.17860.81720.05620.053*
C240.27917 (14)0.8024 (3)0.0855 (3)0.0351 (9)
H24A0.26600.76940.13750.042*
H24B0.30340.84970.11340.042*
C190.26051 (15)0.9050 (3)0.0530 (3)0.0391 (10)
H19A0.28460.95370.02740.047*
H19B0.23500.94040.09300.047*
C210.26412 (15)0.6566 (3)0.0106 (3)0.0404 (10)
H21A0.27840.60620.04760.048*
H21B0.25110.62290.04110.048*
C230.24573 (16)0.7568 (3)0.1492 (3)0.0428 (11)
H23A0.22030.79020.19120.051*
H23B0.26010.70710.18680.051*
O200.40292 (13)0.8424 (2)0.1497 (2)0.0603 (9)
O180.34977 (13)1.1619 (2)0.3047 (3)0.0665 (10)
O220.08147 (17)1.0902 (4)0.4498 (3)0.0808 (14)
O150.35058 (13)1.0301 (3)0.4396 (2)0.0630 (10)
O190.37035 (14)1.0176 (3)0.0935 (3)0.0761 (12)
O210.46026 (14)0.9971 (3)0.1711 (3)0.0843 (14)
O170.39211 (15)0.9777 (3)0.2875 (3)0.0814 (13)
O160.29273 (14)1.0079 (4)0.2783 (3)0.0985 (15)
O280.1337 (5)0.5321 (8)0.2814 (9)0.132 (4)0.50
O28A0.1061 (4)0.4884 (9)0.2251 (7)0.115 (4)0.50
H5O0.4263 (18)0.453 (4)0.379 (4)0.050*
H510.3960 (18)0.372 (4)0.153 (3)0.050*
H520.4854 (17)0.522 (3)0.232 (3)0.050*
H530.4700 (18)0.563 (4)0.162 (3)0.050*
H540.4214 (16)0.690 (3)0.318 (3)0.050*
H550.3985 (16)0.730 (4)0.242 (3)0.050*
H560.3716 (16)0.550 (3)0.050 (3)0.050*
H570.3474 (16)0.653 (3)0.082 (3)0.050*
H580.3127 (16)0.588 (4)0.286 (3)0.050*
H590.2073 (19)0.932 (4)0.146 (3)0.050*
H600.2265 (17)0.967 (3)0.222 (3)0.050*
H610.1681 (17)1.151 (3)0.172 (3)0.050*
H620.0781 (16)1.053 (3)0.329 (3)0.050*
H630.0592 (17)1.063 (4)0.241 (3)0.050*
H640.0980 (17)0.836 (3)0.280 (3)0.050*
H650.1253 (18)0.799 (4)0.229 (3)0.050*
H660.1157 (18)1.019 (3)0.051 (3)0.050*
H670.3177 (19)0.500 (4)0.266 (4)0.050*
H680.3554 (16)0.383 (4)0.171 (3)0.050*
H690.0983 (17)1.050 (3)0.498 (3)0.050*
H700.0672 (19)1.111 (4)0.473 (4)0.050*
H710.1448 (18)1.170 (4)0.245 (3)0.050*
H720.1787 (18)1.026 (4)0.396 (3)0.050*
H730.1706 (17)0.924 (3)0.385 (3)0.050*
H740.3059 (16)0.359 (3)0.398 (3)0.050*
H750.3306 (18)0.332 (4)0.327 (3)0.050*
H760.0890 (17)0.930 (4)0.077 (3)0.050*
H770.3926 (18)0.497 (4)0.392 (4)0.050*
Atomic displacement parameters (Å2) top
U11U22U33U12U13U23
Ni10.0211 (3)0.0232 (3)0.0237 (2)0.00153 (19)0.00187 (18)0.00110 (18)
O20.0291 (15)0.0368 (17)0.0255 (13)0.0026 (13)0.0007 (11)0.0033 (11)
O10.0282 (16)0.043 (2)0.0451 (18)0.0049 (15)0.0139 (13)0.0082 (14)
O40.0205 (15)0.053 (2)0.0382 (17)0.0008 (13)0.0027 (12)0.0161 (14)
O30.0437 (18)0.0236 (15)0.0351 (15)0.0025 (13)0.0038 (13)0.0013 (12)
O50.052 (2)0.0357 (19)0.0284 (15)0.0042 (15)0.0063 (14)0.0070 (13)
N50.0311 (18)0.037 (2)0.0291 (16)0.0016 (15)0.0097 (14)0.0083 (14)
O60.0283 (16)0.0294 (16)0.0431 (16)0.0037 (13)0.0124 (13)0.0102 (12)
N100.0273 (18)0.0323 (19)0.0334 (17)0.0045 (14)0.0088 (14)0.0038 (14)
N90.0316 (19)0.0313 (19)0.0371 (17)0.0009 (14)0.0087 (15)0.0040 (14)
N70.0304 (18)0.0305 (18)0.0282 (15)0.0017 (14)0.0022 (13)0.0038 (13)
N60.0251 (17)0.0325 (19)0.0279 (16)0.0006 (14)0.0064 (13)0.0064 (13)
O140.054 (2)0.043 (2)0.050 (2)0.0075 (17)0.0207 (16)0.0055 (15)
N120.0326 (19)0.0306 (19)0.0400 (18)0.0043 (15)0.0133 (15)0.0040 (14)
C100.026 (2)0.036 (2)0.035 (2)0.0024 (17)0.0036 (16)0.0018 (17)
N80.0272 (17)0.0292 (18)0.0329 (16)0.0001 (14)0.0091 (13)0.0007 (13)
C150.039 (2)0.022 (2)0.048 (2)0.0018 (18)0.0146 (19)0.0002 (17)
N110.0333 (19)0.036 (2)0.0362 (17)0.0068 (15)0.0076 (15)0.0079 (15)
C90.033 (2)0.032 (2)0.0313 (19)0.0055 (18)0.0068 (17)0.0022 (16)
C160.029 (2)0.036 (2)0.043 (2)0.0037 (18)0.0111 (17)0.0000 (18)
C120.040 (2)0.035 (2)0.0231 (17)0.0008 (18)0.0085 (16)0.0006 (16)
C110.029 (2)0.050 (3)0.0210 (17)0.0029 (19)0.0063 (15)0.0009 (17)
C140.025 (2)0.042 (3)0.043 (2)0.0003 (18)0.0109 (17)0.0000 (19)
C80.026 (2)0.039 (2)0.037 (2)0.0052 (18)0.0091 (17)0.0059 (17)
C70.033 (2)0.030 (2)0.036 (2)0.0031 (17)0.0056 (17)0.0047 (17)
C170.037 (2)0.040 (2)0.0310 (19)0.0042 (19)0.0048 (17)0.0044 (17)
C130.039 (2)0.030 (2)0.049 (2)0.0042 (19)0.012 (2)0.0016 (18)
C180.038 (2)0.051 (3)0.0295 (19)0.001 (2)0.0055 (18)0.0027 (18)
Ni20.0234 (3)0.0263 (3)0.0258 (2)0.0016 (2)0.00625 (19)0.00049 (19)
O100.064 (2)0.043 (2)0.0337 (17)0.0107 (18)0.0092 (15)0.0040 (14)
O70.0329 (17)0.0464 (19)0.0352 (16)0.0115 (13)0.0091 (13)0.0094 (13)
O80.051 (2)0.071 (3)0.0325 (16)0.0223 (18)0.0008 (14)0.0020 (16)
O90.0274 (17)0.063 (2)0.0433 (19)0.0000 (15)0.0104 (14)0.0182 (17)
N30.038 (2)0.061 (3)0.0335 (18)0.0058 (18)0.0002 (15)0.0086 (17)
O110.085 (3)0.0293 (19)0.110 (3)0.0145 (19)0.071 (2)0.009 (2)
O120.062 (2)0.0290 (18)0.062 (2)0.0071 (16)0.0383 (17)0.0044 (15)
N20.0319 (19)0.041 (2)0.0347 (17)0.0036 (15)0.0013 (14)0.0008 (15)
C10.028 (2)0.049 (3)0.047 (2)0.001 (2)0.0058 (18)0.005 (2)
N10.039 (2)0.047 (2)0.049 (2)0.0015 (18)0.0121 (17)0.0141 (18)
N40.040 (2)0.042 (2)0.049 (2)0.0068 (17)0.0193 (17)0.0036 (17)
C40.046 (3)0.037 (3)0.053 (3)0.002 (2)0.012 (2)0.011 (2)
C30.027 (2)0.060 (3)0.055 (3)0.004 (2)0.004 (2)0.011 (2)
C50.058 (3)0.080 (4)0.028 (2)0.004 (3)0.006 (2)0.007 (2)
C20.058 (3)0.036 (3)0.072 (3)0.008 (2)0.020 (3)0.005 (2)
C60.054 (3)0.050 (3)0.029 (2)0.005 (2)0.0110 (19)0.0039 (19)
Cr30.0288 (4)0.0324 (4)0.0343 (3)0.0023 (3)0.0070 (3)0.0006 (3)
Cr40.0278 (4)0.0420 (4)0.0349 (3)0.0028 (3)0.0066 (3)0.0022 (3)
Cr20.0663 (6)0.0474 (5)0.0390 (4)0.0133 (4)0.0001 (4)0.0049 (3)
O260.157 (10)0.186 (9)0.064 (5)0.049 (6)0.044 (4)0.035 (5)
O290.105 (8)0.064 (4)0.314 (14)0.027 (5)0.031 (7)0.088 (6)
O310.086 (5)0.188 (11)0.124 (8)0.039 (6)0.010 (5)0.028 (6)
O26A0.157 (10)0.186 (9)0.064 (5)0.049 (6)0.044 (4)0.035 (5)
O29A0.105 (8)0.064 (4)0.314 (14)0.027 (5)0.031 (7)0.088 (6)
O31A0.086 (5)0.188 (11)0.124 (8)0.039 (6)0.010 (5)0.028 (6)
Cr10.0900 (7)0.0467 (5)0.0630 (5)0.0152 (5)0.0280 (5)0.0216 (4)
O230.054 (3)0.087 (7)0.136 (8)0.014 (4)0.030 (4)0.031 (5)
O300.063 (5)0.076 (6)0.056 (3)0.001 (3)0.009 (3)0.024 (3)
O240.115 (6)0.066 (5)0.065 (6)0.035 (4)0.016 (4)0.021 (4)
O23A0.054 (3)0.087 (7)0.136 (8)0.014 (4)0.030 (4)0.031 (5)
O30A0.063 (5)0.076 (6)0.056 (3)0.001 (3)0.009 (3)0.024 (3)
O24A0.115 (6)0.066 (5)0.065 (6)0.035 (4)0.016 (4)0.021 (4)
N140.0307 (18)0.037 (2)0.0316 (16)0.0041 (15)0.0034 (14)0.0010 (14)
N150.034 (2)0.044 (2)0.0381 (18)0.0093 (16)0.0027 (15)0.0038 (16)
N130.036 (2)0.034 (2)0.0360 (18)0.0041 (15)0.0085 (15)0.0053 (14)
N160.0277 (18)0.039 (2)0.0379 (18)0.0022 (15)0.0078 (14)0.0046 (14)
C200.026 (2)0.043 (3)0.040 (2)0.0049 (18)0.0073 (17)0.0033 (18)
C220.023 (2)0.059 (3)0.051 (2)0.001 (2)0.0040 (19)0.000 (2)
C240.033 (2)0.042 (2)0.0308 (19)0.0015 (19)0.0044 (17)0.0058 (17)
C190.038 (2)0.032 (2)0.047 (2)0.0055 (19)0.0086 (19)0.0041 (19)
C210.047 (3)0.032 (2)0.041 (2)0.0018 (19)0.003 (2)0.0028 (18)
C230.046 (3)0.049 (3)0.031 (2)0.001 (2)0.0038 (18)0.0013 (19)
O200.078 (3)0.038 (2)0.065 (2)0.0050 (17)0.0104 (18)0.0039 (16)
O180.078 (3)0.042 (2)0.075 (2)0.0035 (18)0.006 (2)0.0054 (17)
O220.075 (3)0.108 (4)0.060 (3)0.033 (3)0.013 (2)0.027 (2)
O150.062 (2)0.080 (3)0.0489 (19)0.0076 (19)0.0149 (17)0.0128 (17)
O190.082 (3)0.062 (2)0.076 (3)0.000 (2)0.016 (2)0.021 (2)
O210.058 (2)0.133 (4)0.059 (2)0.053 (2)0.0042 (19)0.010 (2)
O170.088 (3)0.104 (3)0.057 (2)0.046 (2)0.027 (2)0.008 (2)
O160.054 (3)0.127 (4)0.105 (3)0.031 (3)0.024 (2)0.009 (3)
O280.213 (15)0.080 (8)0.114 (9)0.005 (8)0.063 (9)0.004 (6)
O28A0.098 (8)0.162 (11)0.075 (6)0.064 (7)0.029 (5)0.058 (6)
Geometric parameters (Å, º) top
Ni1—O22.038 (2)O9—H600.83 (4)
Ni1—O32.038 (3)N3—C41.455 (5)
Ni1—O62.059 (3)N3—C31.459 (5)
Ni1—O42.061 (3)N3—C51.472 (6)
Ni1—O12.064 (3)O11—H640.79 (5)
Ni1—O52.070 (3)O11—H650.71 (5)
O2—H560.89 (5)O12—H610.81 (5)
O2—H571.05 (4)O12—H710.73 (5)
O1—H580.82 (5)N2—C61.459 (5)
O1—H670.69 (5)N2—C11.467 (5)
O4—H520.78 (4)N2—C41.485 (5)
O4—H530.72 (5)C1—N11.468 (5)
O3—H540.79 (4)C1—H1A0.970
O3—H550.80 (5)C1—H1B0.970
O5—H5O0.68 (5)N1—C21.469 (6)
O5—H770.67 (5)N1—C51.477 (6)
N5—C91.468 (5)N4—C21.462 (6)
N5—C111.468 (5)N4—C61.466 (5)
N5—C81.476 (5)N4—C31.468 (5)
O6—H510.69 (5)C4—H4A0.970
O6—H680.75 (4)C4—H4B0.970
N10—C161.463 (5)C3—H3A0.970
N10—C171.469 (5)C3—H3B0.970
N10—C151.477 (5)C5—H5A0.970
N9—C131.466 (5)C5—H5B0.970
N9—C161.471 (5)C2—H2A0.970
N9—C181.475 (5)C2—H2B0.970
N7—C101.466 (5)C6—H6A0.970
N7—C121.475 (5)C6—H6B0.970
N7—C91.483 (5)Cr3—O191.573 (3)
N6—C101.473 (4)Cr3—O201.590 (3)
N6—C71.474 (5)Cr3—O211.599 (3)
N6—C111.476 (5)Cr3—O171.765 (4)
O14—H740.87 (5)Cr4—O161.579 (4)
O14—H750.73 (5)Cr4—O181.583 (3)
N12—C141.475 (5)Cr4—O151.615 (3)
N12—C131.481 (5)Cr4—O171.770 (4)
N12—C171.482 (5)Cr2—O231.48 (2)
C10—H10A0.970Cr2—O24A1.572 (8)
C10—H10B0.970Cr2—O301.609 (16)
N8—C71.468 (5)Cr2—O30A1.609 (6)
N8—C121.470 (5)Cr2—O241.62 (2)
N8—C81.476 (5)Cr2—O23A1.652 (7)
C15—N111.472 (5)Cr2—O28A1.728 (8)
C15—H15A0.970Cr2—O281.804 (11)
C15—H15B0.970O26—Cr11.48 (2)
N11—C181.473 (5)O29—Cr11.69 (2)
N11—C141.475 (5)O31—Cr11.57 (2)
C9—H9A0.970O26A—Cr11.536 (8)
C9—H9B0.970O29A—Cr11.511 (7)
C16—H16A0.970O31A—Cr11.724 (9)
C16—H16B0.970Cr1—O281.635 (11)
C12—H12A0.970Cr1—O28A1.761 (9)
C12—H12B0.970O23—O28A1.77 (2)
C11—H11A0.970N14—C201.467 (5)
C11—H11B0.970N14—C241.467 (5)
C14—H14A0.970N14—C211.476 (5)
C14—H14B0.970N15—C221.458 (5)
C8—H8A0.970N15—C211.463 (5)
C8—H8B0.970N15—C231.464 (5)
C7—H7A0.970N13—C201.468 (5)
C7—H7B0.970N13—C231.477 (5)
C17—H17A0.970N13—C191.484 (5)
C17—H17B0.970N16—C241.463 (5)
C13—H13A0.970N16—C191.464 (5)
C13—H13B0.970N16—C221.484 (5)
C18—H18A0.970C20—H20A0.970
C18—H18B0.970C20—H20B0.970
Ni2—O112.002 (3)C22—H22A0.970
Ni2—O122.022 (3)C22—H22B0.970
Ni2—O72.023 (3)C24—H24A0.970
Ni2—O82.052 (3)C24—H24B0.970
Ni2—O102.054 (3)C19—H19A0.970
Ni2—O92.072 (3)C19—H19B0.970
O10—H720.73 (5)C21—H21A0.970
O10—H730.82 (4)C21—H21B0.970
O7—H620.87 (5)C23—H23A0.970
O7—H630.73 (5)C23—H23B0.970
O8—H660.81 (5)O22—H690.94 (4)
O8—H760.85 (5)O22—H700.62 (5)
O9—H590.61 (5)O28—O28A1.184 (14)
O2—Ni1—O389.39 (12)H62—O7—H63106 (5)
O2—Ni1—O692.01 (12)Ni2—O8—H66117 (3)
O3—Ni1—O6176.43 (12)Ni2—O8—H76111 (3)
O2—Ni1—O485.99 (11)H66—O8—H76128 (5)
O3—Ni1—O494.81 (13)Ni2—O9—H59130 (5)
O6—Ni1—O488.56 (12)Ni2—O9—H60113 (3)
O2—Ni1—O190.91 (12)H59—O9—H60115 (6)
O3—Ni1—O187.86 (12)C4—N3—C3108.9 (3)
O6—Ni1—O188.84 (12)C4—N3—C5107.9 (4)
O4—Ni1—O1175.88 (13)C3—N3—C5107.7 (4)
O2—Ni1—O5176.94 (13)Ni2—O11—H64116 (3)
O3—Ni1—O588.22 (12)Ni2—O11—H65133 (4)
O6—Ni1—O590.48 (13)H64—O11—H65110 (5)
O4—Ni1—O592.31 (13)Ni2—O12—H61120 (3)
O1—Ni1—O590.91 (13)Ni2—O12—H71119 (4)
Ni1—O2—H56110 (3)H61—O12—H71118 (5)
Ni1—O2—H57117 (2)C6—N2—C1108.4 (3)
H56—O2—H57113 (4)C6—N2—C4108.0 (3)
Ni1—O1—H58116 (3)C1—N2—C4108.4 (3)
Ni1—O1—H6799 (5)N2—C1—N1111.3 (3)
H58—O1—H67109 (6)N2—C1—H1A109.4
Ni1—O4—H52131 (4)N1—C1—H1A109.4
Ni1—O4—H53122 (4)N2—C1—H1B109.4
H52—O4—H53102 (5)N1—C1—H1B109.4
Ni1—O3—H54110 (3)H1A—C1—H1B108.0
Ni1—O3—H55117 (3)C1—N1—C2108.2 (3)
H54—O3—H55108 (5)C1—N1—C5108.5 (4)
Ni1—O5—H5O124 (4)C2—N1—C5108.5 (4)
Ni1—O5—H77111 (5)C2—N4—C6108.0 (3)
H5O—O5—H77117 (6)C2—N4—C3107.9 (4)
C9—N5—C11108.2 (3)C6—N4—C3107.7 (3)
C9—N5—C8108.8 (3)N3—C4—N2111.7 (3)
C11—N5—C8107.9 (3)N3—C4—H4A109.3
Ni1—O6—H51126 (4)N2—C4—H4A109.3
Ni1—O6—H68113 (4)N3—C4—H4B109.3
H51—O6—H68115 (6)N2—C4—H4B109.3
C16—N10—C17108.3 (3)H4A—C4—H4B107.9
C16—N10—C15107.8 (3)N3—C3—N4112.9 (3)
C17—N10—C15108.0 (3)N3—C3—H3A109.0
C13—N9—C16107.8 (3)N4—C3—H3A109.0
C13—N9—C18108.7 (3)N3—C3—H3B109.0
C16—N9—C18108.2 (3)N4—C3—H3B109.0
C10—N7—C12109.0 (3)H3A—C3—H3B107.8
C10—N7—C9107.8 (3)N3—C5—N1111.6 (3)
C12—N7—C9108.1 (3)N3—C5—H5A109.3
C10—N6—C7107.8 (3)N1—C5—H5A109.3
C10—N6—C11108.1 (3)N3—C5—H5B109.3
C7—N6—C11107.7 (3)N1—C5—H5B109.3
H74—O14—H75113 (5)H5A—C5—H5B108.0
C14—N12—C13108.8 (3)N4—C2—N1112.0 (4)
C14—N12—C17108.5 (3)N4—C2—H2A109.2
C13—N12—C17108.1 (3)N1—C2—H2A109.2
N7—C10—N6112.0 (3)N4—C2—H2B109.2
N7—C10—H10A109.2N1—C2—H2B109.2
N6—C10—H10A109.2H2A—C2—H2B107.9
N7—C10—H10B109.2N2—C6—N4112.6 (3)
N6—C10—H10B109.2N2—C6—H6A109.1
H10A—C10—H10B107.9N4—C6—H6A109.1
C7—N8—C12107.8 (3)N2—C6—H6B109.1
C7—N8—C8108.0 (3)N4—C6—H6B109.1
C12—N8—C8107.7 (3)H6A—C6—H6B107.8
N11—C15—N10112.1 (3)O19—Cr3—O20110.27 (19)
N11—C15—H15A109.2O19—Cr3—O21111.3 (2)
N10—C15—H15A109.2O20—Cr3—O21109.8 (2)
N11—C15—H15B109.2O19—Cr3—O17112.0 (2)
N10—C15—H15B109.2O20—Cr3—O17107.03 (19)
H15A—C15—H15B107.9O21—Cr3—O17106.3 (2)
C15—N11—C18108.1 (3)O16—Cr4—O18110.5 (2)
C15—N11—C14109.0 (3)O16—Cr4—O15110.3 (2)
C18—N11—C14107.8 (3)O18—Cr4—O15108.07 (19)
N5—C9—N7111.5 (3)O16—Cr4—O17113.3 (2)
N5—C9—H9A109.3O18—Cr4—O17110.4 (2)
N7—C9—H9A109.3O15—Cr4—O17104.01 (18)
N5—C9—H9B109.3O23—Cr2—O30114.8 (10)
N7—C9—H9B109.3O24A—Cr2—O30A115.1 (4)
H9A—C9—H9B108.0O23—Cr2—O24113.4 (12)
N10—C16—N9112.7 (3)O30—Cr2—O2492.5 (9)
N10—C16—H16A109.0O24A—Cr2—O23A112.4 (5)
N9—C16—H16A109.0O30A—Cr2—O23A111.9 (4)
N10—C16—H16B109.0O24A—Cr2—O28A99.6 (5)
N9—C16—H16B109.0O30A—Cr2—O28A117.9 (4)
H16A—C16—H16B107.8O23A—Cr2—O28A98.3 (4)
N8—C12—N7112.2 (3)O23—Cr2—O2892.6 (9)
N8—C12—H12A109.2O30—Cr2—O28106.2 (7)
N7—C12—H12A109.2O24—Cr2—O28138.1 (8)
N8—C12—H12B109.2O29A—Cr1—O26A116.2 (6)
N7—C12—H12B109.2O26—Cr1—O31113.8 (12)
H12A—C12—H12B107.9O26—Cr1—O28114.0 (9)
N5—C11—N6112.3 (3)O31—Cr1—O28116.2 (9)
N5—C11—H11A109.2O26—Cr1—O2999.2 (14)
N6—C11—H11A109.2O31—Cr1—O29103.9 (12)
N5—C11—H11B109.2O28—Cr1—O29107.4 (11)
N6—C11—H11B109.2O29A—Cr1—O31A104.0 (5)
H11A—C11—H11B107.9O26A—Cr1—O31A100.6 (5)
N11—C14—N12111.3 (3)O29A—Cr1—O28A120.3 (6)
N11—C14—H14A109.4O26A—Cr1—O28A107.8 (5)
N12—C14—H14A109.4O31A—Cr1—O28A105.4 (5)
N11—C14—H14B109.4C20—N14—C24108.7 (3)
N12—C14—H14B109.4C20—N14—C21107.9 (3)
H14A—C14—H14B108.0C24—N14—C21107.6 (3)
N8—C8—N5112.2 (3)C22—N15—C21108.4 (3)
N8—C8—H8A109.2C22—N15—C23108.3 (3)
N5—C8—H8A109.2C21—N15—C23107.8 (3)
N8—C8—H8B109.2C20—N13—C23107.6 (3)
N5—C8—H8B109.2C20—N13—C19108.0 (3)
H8A—C8—H8B107.9C23—N13—C19108.4 (3)
N8—C7—N6113.0 (3)C24—N16—C19109.0 (3)
N8—C7—H7A109.0C24—N16—C22108.1 (3)
N6—C7—H7A109.0C19—N16—C22107.7 (3)
N8—C7—H7B109.0N14—C20—N13112.2 (3)
N6—C7—H7B109.0N14—C20—H20A109.2
H7A—C7—H7B107.8N13—C20—H20A109.2
N10—C17—N12111.7 (3)N14—C20—H20B109.2
N10—C17—H17A109.3N13—C20—H20B109.2
N12—C17—H17A109.3H20A—C20—H20B107.9
N10—C17—H17B109.3N15—C22—N16112.2 (3)
N12—C17—H17B109.3N15—C22—H22A109.2
H17A—C17—H17B107.9N16—C22—H22A109.2
N9—C13—N12111.3 (3)N15—C22—H22B109.2
N9—C13—H13A109.4N16—C22—H22B109.2
N12—C13—H13A109.4H22A—C22—H22B107.9
N9—C13—H13B109.4N16—C24—N14112.0 (3)
N12—C13—H13B109.4N16—C24—H24A109.2
H13A—C13—H13B108.0N14—C24—H24A109.2
N11—C18—N9111.9 (3)N16—C24—H24B109.2
N11—C18—H18A109.2N14—C24—H24B109.2
N9—C18—H18A109.2H24A—C24—H24B107.9
N11—C18—H18B109.2N16—C19—N13111.6 (3)
N9—C18—H18B109.2N16—C19—H19A109.3
H18A—C18—H18B107.9N13—C19—H19A109.3
O11—Ni2—O12176.57 (14)N16—C19—H19B109.3
O11—Ni2—O786.73 (14)N13—C19—H19B109.3
O12—Ni2—O790.28 (13)H19A—C19—H19B108.0
O11—Ni2—O889.23 (18)N15—C21—N14112.3 (3)
O12—Ni2—O892.43 (15)N15—C21—H21A109.1
O7—Ni2—O889.78 (14)N14—C21—H21A109.1
O11—Ni2—O1088.46 (17)N15—C21—H21B109.1
O12—Ni2—O1090.02 (15)N14—C21—H21B109.1
O7—Ni2—O1092.72 (13)H21A—C21—H21B107.9
O8—Ni2—O10176.49 (15)N15—C23—N13112.2 (3)
O11—Ni2—O993.91 (16)N15—C23—H23A109.2
O12—Ni2—O989.06 (14)N13—C23—H23A109.2
O7—Ni2—O9179.03 (14)N15—C23—H23B109.2
O8—Ni2—O990.97 (14)N13—C23—H23B109.2
O10—Ni2—O986.56 (14)H23A—C23—H23B107.9
Ni2—O10—H72124 (4)H69—O22—H70100 (6)
Ni2—O10—H73107 (3)Cr3—O17—Cr4128.8 (2)
H72—O10—H73126 (5)Cr1—O28—Cr2132.1 (7)
Ni2—O7—H62113 (3)Cr2—O28A—Cr1128.7 (5)
Ni2—O7—H63118 (4)
Hydrogen-bond geometry (Å, º) top
D—H···AD—HH···AD···AD—H···A
O4—H53···N6i0.72 (5)2.16 (5)2.874 (4)177 (3)
O11—H64···N4ii0.79 (5)2.01 (5)2.782 (6)166 (4)
O10—H73···N15ii0.82 (5)2.34 (5)2.982 (5)135 (4)
O1—H58···N13ii0.82 (5)2.06 (5)2.862 (5)168 (5)
O12—H61···N12iii0.81 (5)1.95 (5)2.710 (5)156 (4)
O7—H63···N2iv0.73 (5)2.06 (5)2.795 (4)176 (5)
O22—H70···N1v0.62 (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, z1/2; (iv) x, y+2, z; (v) x, y+1/2, z+1/2.
 

Follow Acta Cryst. E
Sign up for e-alerts
Follow Acta Cryst. on Twitter
Follow us on facebook
Sign up for RSS feeds