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Each K+ ion in [K(CH3NO2)(H2O)4]Br·H2O, (I), has an eightfold coordination, with the coordination sphere containing four water mol­ecules and four O atoms from the nitro­methane mol­ecules. The coordination polyhedra share two O atoms from two different nitro­methane mol­ecules and, in this way, form chains running parallel to the (100) direction. Hydro­gen bonding involving the Br- ion and the fifth water mol­ecule tie the chains together.

Supporting information

cif

Crystallographic Information File (CIF) https://doi.org/10.1107/S1600536800020791/cf6016sup1.cif
Contains datablocks global, I

hkl

Structure factor file (CIF format) https://doi.org/10.1107/S1600536800020791/cf6016Isup2.hkl
Contains datablock I

CCDC reference: 159701

Key indicators

  • Single-crystal X-ray study
  • T = 293 K
  • Mean [sigma](N-C) = 0.008 Å
  • R factor = 0.037
  • wR factor = 0.092
  • Data-to-parameter ratio = 9.5

checkCIF results

No syntax errors found

ADDSYM reports no extra symmetry


Amber Alert Alert Level B:
THETM_01 Alert B The value of sine(theta_max)/wavelength is less than 0.575 Calculated sin(theta_max)/wavelength = 0.5565
Author response: The observed value represents the limit of theta_max for the crystal to CCD detector length chosen.

Yellow Alert Alert Level C:
REFNR_01 Alert C Ratio of reflections to parameters is < 10 for a centrosymmetric structure sine(theta)/lambda 0.5565 Proportion of unique data used 1.0000 Ratio reflections to parameters 9.4510 PLAT_030 Alert C Refined Extinction parameter within range .... 2.57 Sigma
0 Alert Level A = Potentially serious problem
1 Alert Level B = Potential problem
2 Alert Level C = Please check

Comment top

NO Comment

Experimental top

The title material was found as a side product in the attempted preparation of the linear chain compound Cu(14ane)CuBr4 (where 14ane is 1,4,8,11-tetraazacyclotetradecane), similar to the corresponding chloride material (Wang et al., 1996). The process involved slow crystallization of a solution of CuBr2 and 14ane in an organic solvent contained in a sealed vial. The major product obtained was the mixed valence compound Cu(14ane)CuBr3 (Willett, 2001). Further examination of the solid material obtained revealed a few small colorless crystals. With the possibility that this was a further product containing only the CuI metal ion, a crystal was selected for single-crystal structure determination.

Refinement top

H atoms were located via difference syntheses and their positions were loosely constrained to expected geometry via the DFIX instruction in the SHELXL97 program XL. Their isotropic displacement parameters were not constrained.

Computing details top

Data collection: SMART (Bruker, 1996); cell refinement: SAINT (Bruker, 1996); data reduction: SAINT; program(s) used to solve structure: SHELXS97 (Sheldrick, 1997a); program(s) used to refine structure: SHELXL97 (Sheldrick, 1997a); molecular graphics: SHELXTL (Sheldrick, 1997b); software used to prepare material for publication: SHELXL97.

Figures top
[Figure 1] Fig. 1. Illustration of the chain structure of the title compound. Displacement ellipsoids are shown at the 50% probability level.
(I) top
Crystal data top
[K(CH3NO2)(H2O)5]Br·H2OF(000) = 544
Mr = 270.13Dx = 1.772 Mg m3
Monoclinic, P21/nMo Kα radiation, λ = 0.71073 Å
a = 6.8004 (3) ÅCell parameters from 4394 reflections
b = 13.8358 (5) Åθ = 2.4–23.3°
c = 10.8658 (4) ŵ = 4.47 mm1
β = 97.896 (1)°T = 293 K
V = 1012.66 (7) Å3Needle, colorless
Z = 40.50 × 0.05 × 0.05 mm
Data collection top
SMART 1000 area detector
diffractometer
1446 independent reflections
Radiation source: fine-focus sealed tube1362 reflections with I > 2σ(I)
Graphite monochromatorRint = 0.045
ϕ and ω scansθmax = 23.3°, θmin = 2.4°
Absorption correction: multi-scan
(XPREP in SHELXTL; Sheldrick, 1997b)
h = 77
Tmin = 0.718, Tmax = 0.800k = 1515
4394 measured reflectionsl = 1112
Refinement top
Refinement on F2Secondary atom site location: difference Fourier map
Least-squares matrix: fullHydrogen site location: inferred from neighbouring sites
R[F2 > 2σ(F2)] = 0.037All H-atom parameters refined
wR(F2) = 0.092 w = 1/[σ2(Fo2) + (0.0367P)2 + 2.7724P]
where P = (Fo2 + 2Fc2)/3
S = 1.10(Δ/σ)max = 0.001
1446 reflectionsΔρmax = 0.44 e Å3
153 parametersΔρmin = 0.52 e Å3
17 restraintsExtinction correction: SHELXL97, Fc*=kFc[1+0.001xFc2λ3/sin(2θ)]-1/4
Primary atom site location: structure-invariant direct methodsExtinction coefficient: 0.0036 (14)
Crystal data top
[K(CH3NO2)(H2O)5]Br·H2OV = 1012.66 (7) Å3
Mr = 270.13Z = 4
Monoclinic, P21/nMo Kα radiation
a = 6.8004 (3) ŵ = 4.47 mm1
b = 13.8358 (5) ÅT = 293 K
c = 10.8658 (4) Å0.50 × 0.05 × 0.05 mm
β = 97.896 (1)°
Data collection top
SMART 1000 area detector
diffractometer
1446 independent reflections
Absorption correction: multi-scan
(XPREP in SHELXTL; Sheldrick, 1997b)
1362 reflections with I > 2σ(I)
Tmin = 0.718, Tmax = 0.800Rint = 0.045
4394 measured reflectionsθmax = 23.3°
Refinement top
R[F2 > 2σ(F2)] = 0.03717 restraints
wR(F2) = 0.092All H-atom parameters refined
S = 1.10Δρmax = 0.44 e Å3
1446 reflectionsΔρmin = 0.52 e Å3
153 parameters
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*/Ueq
Br0.10631 (8)0.66576 (4)0.03113 (5)0.0476 (3)
K0.23119 (12)0.52923 (6)0.41211 (8)0.0212 (3)
O70.1569 (6)0.3550 (3)0.3808 (4)0.0460 (9)
O60.2101 (6)0.4895 (3)0.1846 (3)0.0446 (9)
O50.2141 (7)0.6833 (3)0.3017 (4)0.0569 (11)
O40.4731 (6)0.6512 (3)0.1998 (4)0.0564 (11)
O30.2656 (6)0.6654 (3)0.5625 (4)0.0496 (10)
O20.4316 (4)0.4578 (2)0.6055 (3)0.0325 (8)
N10.2844 (6)0.4423 (3)0.6622 (4)0.0468 (11)
C10.3134 (10)0.3942 (5)0.7861 (6)0.0512 (16)
O10.1123 (4)0.4671 (3)0.6151 (3)0.0386 (8)
H1A0.313 (16)0.325 (8)0.766 (10)0.15 (4)*
H1B0.214 (10)0.398 (5)0.830 (6)0.07 (2)*
H1C0.420 (13)0.399 (6)0.830 (8)0.10 (3)*
H3A0.333 (9)0.655 (4)0.640 (4)0.062 (19)*
H3B0.323 (10)0.717 (4)0.531 (6)0.08 (2)*
H4A0.570 (8)0.601 (4)0.177 (6)0.08 (2)*
H4B0.377 (9)0.646 (5)0.144 (6)0.09 (2)*
H5A0.105 (9)0.723 (5)0.288 (7)0.11 (3)*
H5C0.331 (11)0.721 (7)0.302 (14)0.27 (8)*
H6A0.192 (10)0.541 (4)0.136 (5)0.07 (2)*
H6C0.118 (9)0.441 (4)0.154 (6)0.08 (2)*
H7A0.025 (6)0.348 (4)0.381 (6)0.07 (2)*
H7C0.222 (8)0.310 (4)0.431 (5)0.060 (18)*
Atomic displacement parameters (Å2) top
U11U22U33U12U13U23
Br0.0514 (4)0.0424 (4)0.0487 (4)0.0064 (2)0.0060 (3)0.0060 (2)
K0.0131 (5)0.0239 (5)0.0266 (5)0.0003 (3)0.0033 (3)0.0015 (4)
O70.044 (2)0.035 (2)0.057 (2)0.0036 (17)0.0019 (19)0.0020 (18)
O60.045 (2)0.046 (2)0.041 (2)0.0068 (18)0.0015 (17)0.0035 (18)
O50.068 (3)0.044 (2)0.063 (3)0.010 (2)0.022 (2)0.0158 (19)
O40.051 (2)0.054 (2)0.067 (3)0.002 (2)0.018 (2)0.005 (2)
O30.058 (3)0.037 (2)0.055 (3)0.0034 (18)0.007 (2)0.0037 (18)
O20.0165 (15)0.0436 (19)0.0389 (19)0.0022 (13)0.0089 (13)0.0101 (14)
N10.041 (3)0.041 (3)0.058 (3)0.004 (2)0.005 (2)0.003 (2)
C10.034 (3)0.076 (5)0.044 (3)0.002 (3)0.006 (3)0.024 (3)
O10.0128 (16)0.058 (2)0.044 (2)0.0069 (14)0.0013 (14)0.0144 (16)
Geometric parameters (Å, º) top
K—O1i2.315 (3)O5—H5C0.95 (5)
K—O2ii2.334 (3)O4—H4A0.96 (4)
K—O52.441 (4)O4—H4B0.95 (4)
K—O72.477 (4)O3—H3A0.91 (4)
K—O32.484 (4)O3—H3B0.90 (4)
K—O62.517 (4)O2—N11.263 (5)
K—O22.543 (3)O2—Kii2.334 (3)
K—O12.598 (3)N1—O11.259 (5)
O7—H7A0.90 (4)N1—C11.491 (7)
O7—H7C0.90 (4)C1—H1A0.98 (11)
O6—H6A0.88 (4)C1—H1B0.88 (7)
O6—H6C0.94 (4)C1—H1C0.81 (9)
O5—H5A0.92 (4)O1—Ki2.315 (3)
O1i—K—O2ii166.78 (12)K—O7—H7A107 (4)
O1i—K—O586.50 (14)K—O7—H7C121 (4)
O2ii—K—O582.73 (13)H7A—O7—H7C109 (5)
O1i—K—O779.67 (13)K—O6—H6A113 (4)
O2ii—K—O7104.35 (12)K—O6—H6C116 (4)
O5—K—O7141.94 (15)H6A—O6—H6C109 (6)
O1i—K—O393.98 (13)K—O5—H5A126 (5)
O2ii—K—O389.47 (13)K—O5—H5C120 (6)
O5—K—O369.79 (15)H5A—O5—H5C109 (7)
O7—K—O3145.87 (14)H4A—O4—H4B107 (5)
O1i—K—O687.64 (12)K—O3—H3A118 (4)
O2ii—K—O681.98 (12)K—O3—H3B111 (5)
O5—K—O673.49 (14)H3A—O3—H3B106 (6)
O7—K—O670.69 (13)N1—O2—Kii155.0 (3)
O3—K—O6143.06 (14)N1—O2—K95.6 (3)
O1i—K—O2122.08 (11)Kii—O2—K108.86 (11)
O2ii—K—O271.14 (11)O1—N1—O2120.7 (4)
O5—K—O2136.86 (14)O1—N1—C1119.3 (4)
O7—K—O279.11 (12)O2—N1—C1120.0 (4)
O3—K—O276.11 (13)N1—C1—H1A104 (7)
O6—K—O2132.73 (12)N1—C1—H1B117 (4)
O1i—K—O171.90 (12)H1A—C1—H1B101 (8)
O2ii—K—O1121.27 (10)N1—C1—H1C119 (6)
O5—K—O1134.98 (13)H1A—C1—H1C101 (8)
O7—K—O173.34 (13)H1B—C1—H1C112 (7)
O3—K—O172.82 (13)N1—O1—Ki157.5 (3)
O6—K—O1141.18 (12)N1—O1—K93.1 (3)
O2—K—O150.47 (9)Ki—O1—K108.10 (12)
O1i—K—O2—N15.5 (3)O1i—K—N1—O2175.3 (3)
O2ii—K—O2—N1174.8 (3)O2ii—K—N1—O25.0 (3)
O5—K—O2—N1118.8 (3)O5—K—N1—O291.2 (3)
O7—K—O2—N175.8 (3)O7—K—N1—O298.2 (3)
O3—K—O2—N180.5 (3)O3—K—N1—O292.5 (3)
O6—K—O2—N1126.3 (3)O6—K—N1—O280.0 (3)
O1—K—O2—N11.5 (3)O1—K—N1—O2177.3 (5)
Kii—K—O2—N1174.8 (3)Kii—K—N1—O23.4 (2)
Ki—K—O2—N11.9 (3)Ki—K—N1—O2177.7 (3)
O1i—K—O2—Kii179.78 (13)O2—N1—O1—Ki163.4 (6)
O5—K—O2—Kii55.9 (2)C1—N1—O1—Ki16.6 (12)
O7—K—O2—Kii109.41 (15)K—N1—O1—Ki160.7 (9)
O3—K—O2—Kii94.27 (15)O2—N1—O1—K2.7 (5)
O6—K—O2—Kii58.9 (2)C1—N1—O1—K177.3 (5)
O1—K—O2—Kii173.3 (2)O1i—K—O1—N1172.3 (4)
N1—K—O2—Kii174.8 (3)O2ii—K—O1—N18.9 (3)
Ki—K—O2—Kii176.72 (12)O5—K—O1—N1122.3 (3)
Kii—O2—N1—O1165.5 (5)O7—K—O1—N188.0 (3)
K—O2—N1—O12.8 (5)O3—K—O1—N187.4 (3)
Kii—O2—N1—C114.5 (10)O6—K—O1—N1110.7 (3)
K—O2—N1—C1177.3 (5)O2—K—O1—N11.5 (3)
Kii—O2—N1—K168.2 (7)Kii—K—O1—N15.2 (3)
O1i—K—N1—O17.3 (3)Ki—K—O1—N1172.3 (4)
O2ii—K—N1—O1172.3 (3)O2ii—K—O1—Ki178.74 (13)
O5—K—N1—O186.1 (3)O5—K—O1—Ki65.3 (2)
O7—K—N1—O184.5 (3)O7—K—O1—Ki84.31 (16)
O3—K—N1—O184.8 (3)O3—K—O1—Ki100.22 (16)
O6—K—N1—O1102.7 (3)O6—K—O1—Ki61.6 (2)
O2—K—N1—O1177.3 (5)O2—K—O1—Ki173.8 (2)
Kii—K—N1—O1173.9 (3)N1—K—O1—Ki172.3 (4)
Ki—K—N1—O15.0 (2)Kii—K—O1—Ki177.57 (13)
Symmetry codes: (i) x, y+1, z+1; (ii) x+1, y+1, z+1.

Experimental details

Crystal data
Chemical formula[K(CH3NO2)(H2O)5]Br·H2O
Mr270.13
Crystal system, space groupMonoclinic, P21/n
Temperature (K)293
a, b, c (Å)6.8004 (3), 13.8358 (5), 10.8658 (4)
β (°) 97.896 (1)
V3)1012.66 (7)
Z4
Radiation typeMo Kα
µ (mm1)4.47
Crystal size (mm)0.50 × 0.05 × 0.05
Data collection
DiffractometerSMART 1000 area detector
diffractometer
Absorption correctionMulti-scan
(XPREP in SHELXTL; Sheldrick, 1997b)
Tmin, Tmax0.718, 0.800
No. of measured, independent and
observed [I > 2σ(I)] reflections
4394, 1446, 1362
Rint0.045
θmax (°)23.3
(sin θ/λ)max1)0.557
Refinement
R[F2 > 2σ(F2)], wR(F2), S 0.037, 0.092, 1.10
No. of reflections1446
No. of parameters153
No. of restraints17
H-atom treatmentAll H-atom parameters refined
Δρmax, Δρmin (e Å3)0.44, 0.52

Computer programs: SMART (Bruker, 1996), SAINT (Bruker, 1996), SAINT, SHELXS97 (Sheldrick, 1997a), SHELXL97 (Sheldrick, 1997a), SHELXTL (Sheldrick, 1997b), SHELXL97.

 

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