Supporting information
Crystallographic Information File (CIF) https://doi.org/10.1107/S1600536800020791/cf6016sup1.cif | |
Structure factor file (CIF format) https://doi.org/10.1107/S1600536800020791/cf6016Isup2.hkl |
CCDC reference: 159701
Key indicators
- Single-crystal X-ray study
- T = 293 K
- Mean (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
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. |
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
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.
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.
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.
Fig. 1. Illustration of the chain structure of the title compound. Displacement ellipsoids are shown at the 50% probability level. |
[K(CH3NO2)(H2O)5]Br·H2O | F(000) = 544 |
Mr = 270.13 | Dx = 1.772 Mg m−3 |
Monoclinic, P21/n | Mo Kα radiation, λ = 0.71073 Å |
a = 6.8004 (3) Å | Cell parameters from 4394 reflections |
b = 13.8358 (5) Å | θ = 2.4–23.3° |
c = 10.8658 (4) Å | µ = 4.47 mm−1 |
β = 97.896 (1)° | T = 293 K |
V = 1012.66 (7) Å3 | Needle, colorless |
Z = 4 | 0.50 × 0.05 × 0.05 mm |
SMART 1000 area detector diffractometer | 1446 independent reflections |
Radiation source: fine-focus sealed tube | 1362 reflections with I > 2σ(I) |
Graphite monochromator | Rint = 0.045 |
ϕ and ω scans | θmax = 23.3°, θmin = 2.4° |
Absorption correction: multi-scan (XPREP in SHELXTL; Sheldrick, 1997b) | h = −7→7 |
Tmin = 0.718, Tmax = 0.800 | k = −15→15 |
4394 measured reflections | l = −11→12 |
Refinement on F2 | Secondary atom site location: difference Fourier map |
Least-squares matrix: full | Hydrogen site location: inferred from neighbouring sites |
R[F2 > 2σ(F2)] = 0.037 | All 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 reflections | Δρmax = 0.44 e Å−3 |
153 parameters | Δρmin = −0.52 e Å−3 |
17 restraints | Extinction correction: SHELXL97, Fc*=kFc[1+0.001xFc2λ3/sin(2θ)]-1/4 |
Primary atom site location: structure-invariant direct methods | Extinction coefficient: 0.0036 (14) |
[K(CH3NO2)(H2O)5]Br·H2O | V = 1012.66 (7) Å3 |
Mr = 270.13 | Z = 4 |
Monoclinic, P21/n | Mo Kα radiation |
a = 6.8004 (3) Å | µ = 4.47 mm−1 |
b = 13.8358 (5) Å | T = 293 K |
c = 10.8658 (4) Å | 0.50 × 0.05 × 0.05 mm |
β = 97.896 (1)° |
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 = 0.800 | Rint = 0.045 |
4394 measured reflections | θmax = 23.3° |
R[F2 > 2σ(F2)] = 0.037 | 17 restraints |
wR(F2) = 0.092 | All H-atom parameters refined |
S = 1.10 | Δρmax = 0.44 e Å−3 |
1446 reflections | Δρmin = −0.52 e Å−3 |
153 parameters |
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. |
x | y | z | Uiso*/Ueq | ||
Br | 0.10631 (8) | 0.66576 (4) | −0.03113 (5) | 0.0476 (3) | |
K | 0.23119 (12) | 0.52923 (6) | 0.41211 (8) | 0.0212 (3) | |
O7 | 0.1569 (6) | 0.3550 (3) | 0.3808 (4) | 0.0460 (9) | |
O6 | 0.2101 (6) | 0.4895 (3) | 0.1846 (3) | 0.0446 (9) | |
O5 | 0.2141 (7) | 0.6833 (3) | 0.3017 (4) | 0.0569 (11) | |
O4 | 0.4731 (6) | 0.6512 (3) | −0.1998 (4) | 0.0564 (11) | |
O3 | 0.2656 (6) | 0.6654 (3) | 0.5625 (4) | 0.0496 (10) | |
O2 | 0.4316 (4) | 0.4578 (2) | 0.6055 (3) | 0.0325 (8) | |
N1 | 0.2844 (6) | 0.4423 (3) | 0.6622 (4) | 0.0468 (11) | |
C1 | 0.3134 (10) | 0.3942 (5) | 0.7861 (6) | 0.0512 (16) | |
O1 | 0.1123 (4) | 0.4671 (3) | 0.6151 (3) | 0.0386 (8) | |
H1A | 0.313 (16) | 0.325 (8) | 0.766 (10) | 0.15 (4)* | |
H1B | 0.214 (10) | 0.398 (5) | 0.830 (6) | 0.07 (2)* | |
H1C | 0.420 (13) | 0.399 (6) | 0.830 (8) | 0.10 (3)* | |
H3A | 0.333 (9) | 0.655 (4) | 0.640 (4) | 0.062 (19)* | |
H3B | 0.323 (10) | 0.717 (4) | 0.531 (6) | 0.08 (2)* | |
H4A | 0.570 (8) | 0.601 (4) | −0.177 (6) | 0.08 (2)* | |
H4B | 0.377 (9) | 0.646 (5) | −0.144 (6) | 0.09 (2)* | |
H5A | 0.105 (9) | 0.723 (5) | 0.288 (7) | 0.11 (3)* | |
H5C | 0.331 (11) | 0.721 (7) | 0.302 (14) | 0.27 (8)* | |
H6A | 0.192 (10) | 0.541 (4) | 0.136 (5) | 0.07 (2)* | |
H6C | 0.118 (9) | 0.441 (4) | 0.154 (6) | 0.08 (2)* | |
H7A | 0.025 (6) | 0.348 (4) | 0.381 (6) | 0.07 (2)* | |
H7C | 0.222 (8) | 0.310 (4) | 0.431 (5) | 0.060 (18)* |
U11 | U22 | U33 | U12 | U13 | U23 | |
Br | 0.0514 (4) | 0.0424 (4) | 0.0487 (4) | −0.0064 (2) | 0.0060 (3) | −0.0060 (2) |
K | 0.0131 (5) | 0.0239 (5) | 0.0266 (5) | 0.0003 (3) | 0.0033 (3) | 0.0015 (4) |
O7 | 0.044 (2) | 0.035 (2) | 0.057 (2) | 0.0036 (17) | 0.0019 (19) | 0.0020 (18) |
O6 | 0.045 (2) | 0.046 (2) | 0.041 (2) | −0.0068 (18) | −0.0015 (17) | 0.0035 (18) |
O5 | 0.068 (3) | 0.044 (2) | 0.063 (3) | 0.010 (2) | 0.022 (2) | 0.0158 (19) |
O4 | 0.051 (2) | 0.054 (2) | 0.067 (3) | −0.002 (2) | 0.018 (2) | −0.005 (2) |
O3 | 0.058 (3) | 0.037 (2) | 0.055 (3) | −0.0034 (18) | 0.007 (2) | −0.0037 (18) |
O2 | 0.0165 (15) | 0.0436 (19) | 0.0389 (19) | −0.0022 (13) | 0.0089 (13) | 0.0101 (14) |
N1 | 0.041 (3) | 0.041 (3) | 0.058 (3) | −0.004 (2) | 0.005 (2) | 0.003 (2) |
C1 | 0.034 (3) | 0.076 (5) | 0.044 (3) | −0.002 (3) | 0.006 (3) | 0.024 (3) |
O1 | 0.0128 (16) | 0.058 (2) | 0.044 (2) | 0.0069 (14) | 0.0013 (14) | 0.0144 (16) |
K—O1i | 2.315 (3) | O5—H5C | 0.95 (5) |
K—O2ii | 2.334 (3) | O4—H4A | 0.96 (4) |
K—O5 | 2.441 (4) | O4—H4B | 0.95 (4) |
K—O7 | 2.477 (4) | O3—H3A | 0.91 (4) |
K—O3 | 2.484 (4) | O3—H3B | 0.90 (4) |
K—O6 | 2.517 (4) | O2—N1 | 1.263 (5) |
K—O2 | 2.543 (3) | O2—Kii | 2.334 (3) |
K—O1 | 2.598 (3) | N1—O1 | 1.259 (5) |
O7—H7A | 0.90 (4) | N1—C1 | 1.491 (7) |
O7—H7C | 0.90 (4) | C1—H1A | 0.98 (11) |
O6—H6A | 0.88 (4) | C1—H1B | 0.88 (7) |
O6—H6C | 0.94 (4) | C1—H1C | 0.81 (9) |
O5—H5A | 0.92 (4) | O1—Ki | 2.315 (3) |
O1i—K—O2ii | 166.78 (12) | K—O7—H7A | 107 (4) |
O1i—K—O5 | 86.50 (14) | K—O7—H7C | 121 (4) |
O2ii—K—O5 | 82.73 (13) | H7A—O7—H7C | 109 (5) |
O1i—K—O7 | 79.67 (13) | K—O6—H6A | 113 (4) |
O2ii—K—O7 | 104.35 (12) | K—O6—H6C | 116 (4) |
O5—K—O7 | 141.94 (15) | H6A—O6—H6C | 109 (6) |
O1i—K—O3 | 93.98 (13) | K—O5—H5A | 126 (5) |
O2ii—K—O3 | 89.47 (13) | K—O5—H5C | 120 (6) |
O5—K—O3 | 69.79 (15) | H5A—O5—H5C | 109 (7) |
O7—K—O3 | 145.87 (14) | H4A—O4—H4B | 107 (5) |
O1i—K—O6 | 87.64 (12) | K—O3—H3A | 118 (4) |
O2ii—K—O6 | 81.98 (12) | K—O3—H3B | 111 (5) |
O5—K—O6 | 73.49 (14) | H3A—O3—H3B | 106 (6) |
O7—K—O6 | 70.69 (13) | N1—O2—Kii | 155.0 (3) |
O3—K—O6 | 143.06 (14) | N1—O2—K | 95.6 (3) |
O1i—K—O2 | 122.08 (11) | Kii—O2—K | 108.86 (11) |
O2ii—K—O2 | 71.14 (11) | O1—N1—O2 | 120.7 (4) |
O5—K—O2 | 136.86 (14) | O1—N1—C1 | 119.3 (4) |
O7—K—O2 | 79.11 (12) | O2—N1—C1 | 120.0 (4) |
O3—K—O2 | 76.11 (13) | N1—C1—H1A | 104 (7) |
O6—K—O2 | 132.73 (12) | N1—C1—H1B | 117 (4) |
O1i—K—O1 | 71.90 (12) | H1A—C1—H1B | 101 (8) |
O2ii—K—O1 | 121.27 (10) | N1—C1—H1C | 119 (6) |
O5—K—O1 | 134.98 (13) | H1A—C1—H1C | 101 (8) |
O7—K—O1 | 73.34 (13) | H1B—C1—H1C | 112 (7) |
O3—K—O1 | 72.82 (13) | N1—O1—Ki | 157.5 (3) |
O6—K—O1 | 141.18 (12) | N1—O1—K | 93.1 (3) |
O2—K—O1 | 50.47 (9) | Ki—O1—K | 108.10 (12) |
O1i—K—O2—N1 | −5.5 (3) | O1i—K—N1—O2 | 175.3 (3) |
O2ii—K—O2—N1 | 174.8 (3) | O2ii—K—N1—O2 | −5.0 (3) |
O5—K—O2—N1 | 118.8 (3) | O5—K—N1—O2 | −91.2 (3) |
O7—K—O2—N1 | −75.8 (3) | O7—K—N1—O2 | 98.2 (3) |
O3—K—O2—N1 | 80.5 (3) | O3—K—N1—O2 | −92.5 (3) |
O6—K—O2—N1 | −126.3 (3) | O6—K—N1—O2 | 80.0 (3) |
O1—K—O2—N1 | 1.5 (3) | O1—K—N1—O2 | −177.3 (5) |
Kii—K—O2—N1 | 174.8 (3) | Kii—K—N1—O2 | −3.4 (2) |
Ki—K—O2—N1 | −1.9 (3) | Ki—K—N1—O2 | 177.7 (3) |
O1i—K—O2—Kii | 179.78 (13) | O2—N1—O1—Ki | 163.4 (6) |
O5—K—O2—Kii | −55.9 (2) | C1—N1—O1—Ki | −16.6 (12) |
O7—K—O2—Kii | 109.41 (15) | K—N1—O1—Ki | 160.7 (9) |
O3—K—O2—Kii | −94.27 (15) | O2—N1—O1—K | 2.7 (5) |
O6—K—O2—Kii | 58.9 (2) | C1—N1—O1—K | −177.3 (5) |
O1—K—O2—Kii | −173.3 (2) | O1i—K—O1—N1 | 172.3 (4) |
N1—K—O2—Kii | −174.8 (3) | O2ii—K—O1—N1 | −8.9 (3) |
Ki—K—O2—Kii | −176.72 (12) | O5—K—O1—N1 | −122.3 (3) |
Kii—O2—N1—O1 | 165.5 (5) | O7—K—O1—N1 | 88.0 (3) |
K—O2—N1—O1 | −2.8 (5) | O3—K—O1—N1 | −87.4 (3) |
Kii—O2—N1—C1 | −14.5 (10) | O6—K—O1—N1 | 110.7 (3) |
K—O2—N1—C1 | 177.3 (5) | O2—K—O1—N1 | −1.5 (3) |
Kii—O2—N1—K | 168.2 (7) | Kii—K—O1—N1 | −5.2 (3) |
O1i—K—N1—O1 | −7.3 (3) | Ki—K—O1—N1 | 172.3 (4) |
O2ii—K—N1—O1 | 172.3 (3) | O2ii—K—O1—Ki | 178.74 (13) |
O5—K—N1—O1 | 86.1 (3) | O5—K—O1—Ki | 65.3 (2) |
O7—K—N1—O1 | −84.5 (3) | O7—K—O1—Ki | −84.31 (16) |
O3—K—N1—O1 | 84.8 (3) | O3—K—O1—Ki | 100.22 (16) |
O6—K—N1—O1 | −102.7 (3) | O6—K—O1—Ki | −61.6 (2) |
O2—K—N1—O1 | 177.3 (5) | O2—K—O1—Ki | −173.8 (2) |
Kii—K—N1—O1 | 173.9 (3) | N1—K—O1—Ki | −172.3 (4) |
Ki—K—N1—O1 | −5.0 (2) | Kii—K—O1—Ki | −177.57 (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 |
Mr | 270.13 |
Crystal system, space group | Monoclinic, P21/n |
Temperature (K) | 293 |
a, b, c (Å) | 6.8004 (3), 13.8358 (5), 10.8658 (4) |
β (°) | 97.896 (1) |
V (Å3) | 1012.66 (7) |
Z | 4 |
Radiation type | Mo Kα |
µ (mm−1) | 4.47 |
Crystal size (mm) | 0.50 × 0.05 × 0.05 |
Data collection | |
Diffractometer | SMART 1000 area detector diffractometer |
Absorption correction | Multi-scan (XPREP in SHELXTL; Sheldrick, 1997b) |
Tmin, Tmax | 0.718, 0.800 |
No. of measured, independent and observed [I > 2σ(I)] reflections | 4394, 1446, 1362 |
Rint | 0.045 |
θmax (°) | 23.3 |
(sin θ/λ)max (Å−1) | 0.557 |
Refinement | |
R[F2 > 2σ(F2)], wR(F2), S | 0.037, 0.092, 1.10 |
No. of reflections | 1446 |
No. of parameters | 153 |
No. of restraints | 17 |
H-atom treatment | All H-atom parameters refined |
Δρmax, Δρmin (e Å−3) | 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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