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XIPHOS has been developed to expand home laboratory facilities closer to those found at central facilities, offering extremes of sample environment and flux densities far greater than standard laboratory sources. The system has a minimum operating temperature of 1.9 K, and has a direct-drive molybdenum rotating-anode generator coupled with the latest multilayer optics. XIPHOS has been specifically designed to accommodate various sample environments and is now operational. Furthermore, it has been calibrated with structural phase transitions from 14 to 148 K. Results are also presented from a full low-temperature data collection of m-nitroaniline to demonstrate the quality of results attainable from XIPHOS.

Supporting information

cif

Crystallographic Information File (CIF) https://doi.org/10.1107/S0021889810041282/hx5107sup1.cif
Contains datablocks global, mna_2_K

hkl

Structure factor file (CIF format) https://doi.org/10.1107/S0021889810041282/hx5107sup2.hkl
Contains datablock sad_2_orient

pdf

Portable Document Format (PDF) file https://doi.org/10.1107/S0021889810041282/hx5107sup3.pdf
Supplementary information

Computing details top

Data collection: Bruker APEXII v2010.1-2 (Bruker, 2010); cell refinement: Bruker SAINT version 7.68a (Bruker, 2010); data reduction: Bruker SAINT version 7.68a (Bruker, 2010); program(s) used to solve structure: A short history of SHELX (Sheldrick, 2007)/Bruker; program(s) used to refine structure: SHELXL97 (Sheldrick, 2008); molecular graphics: OLEX2: a complete structure solution, refinement and analysis program. Dolomanov et al., J. Appl. Cryst. (2009). 42, 339-341; software used to prepare material for publication: OLEX2: a complete structure solution, refinement and analysis program. Dolomanov et al., J. Appl. Cryst. (2009). 42, 339-341.

m-nitroaniline top
Crystal data top
C6H6N2O2Dx = 1.503 Mg m3
Mr = 138.13Mo Kα radiation, λ = 0.71073 Å
Orthorhombic, Pca21Cell parameters from 3128 reflections
a = 18.7169 (4) Åθ = 3.3–30.4°
b = 6.5215 (2) ŵ = 0.12 mm1
c = 5.0014 (1) ÅT = 2 K
V = 610.48 (3) Å3Block, clear yellowish yellow
Z = 40.27 × 0.1 × 0.08 mm
F(000) = 288
Data collection top
Bruker APEX-II CCD
diffractometer
993 independent reflections
Radiation source: Bruker TXS with Helios Optics935 reflections with I > 2σ(I)
Multilayer optics monochromatorRint = 0.034
φ and ω scansθmax = 30.4°, θmin = 2.2°
Absorption correction: multi-scan
SADABS-2008/1 (Bruker,2008) was used for absorption correction. R(int) was 0.0670 before and 0.0419 after correction. The Ratio of minimum to maximum transmission is 0.818632707775. The λ/2 correction factor is Not present
h = 2626
Tmin = 0.611, Tmax = 0.746k = 99
9614 measured reflectionsl = 77
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)] = 0.033H atoms treated by a mixture of independent and constrained refinement
wR(F2) = 0.088 w = 1/[σ2(Fo2) + (0.0542P)2 + 0.2014P]
where P = (Fo2 + 2Fc2)/3
S = 1.07(Δ/σ)max < 0.001
993 reflectionsΔρmax = 0.33 e Å3
115 parametersΔρmin = 0.22 e Å3
1 restraintAbsolute structure: not refined as all light atom structure
Primary atom site location: structure-invariant direct methods
Special details top

Geometry. All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds 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 > 2sigma(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
O10.39879 (6)1.06784 (19)0.0795 (3)0.0132 (3)
O20.30390 (6)0.89456 (19)0.0261 (3)0.0124 (3)
N10.30431 (7)0.2819 (2)0.5743 (3)0.0106 (3)
N20.35802 (7)0.9202 (2)0.1096 (3)0.0092 (3)
C50.37561 (8)0.7694 (2)0.3170 (3)0.0084 (3)
C60.33173 (9)0.5977 (2)0.3415 (3)0.0092 (3)
C10.34867 (8)0.4516 (2)0.5354 (3)0.0089 (3)
C20.40898 (8)0.4832 (3)0.6982 (3)0.0101 (3)
C30.45130 (8)0.6569 (3)0.6668 (3)0.0102 (3)
C40.43576 (8)0.8043 (3)0.4746 (4)0.0097 (3)
H60.2909 (12)0.582 (4)0.229 (6)0.015 (6)*
H40.4634 (12)0.926 (4)0.460 (7)0.018 (6)*
H20.4188 (14)0.387 (4)0.827 (7)0.020 (6)*
H1A0.2771 (11)0.259 (3)0.448 (6)0.009 (5)*
H30.4923 (12)0.677 (3)0.779 (5)0.011 (6)*
H1B0.3231 (12)0.176 (4)0.657 (6)0.015 (6)*
Atomic displacement parameters (Å2) top
U11U22U33U12U13U23
O10.0141 (6)0.0090 (5)0.0164 (6)0.0029 (4)0.0003 (5)0.0024 (5)
O20.0119 (5)0.0120 (6)0.0133 (6)0.0000 (4)0.0029 (5)0.0018 (5)
N10.0108 (6)0.0089 (6)0.0121 (6)0.0017 (5)0.0018 (6)0.0019 (6)
N20.0099 (6)0.0078 (6)0.0097 (6)0.0010 (4)0.0007 (6)0.0000 (5)
C50.0098 (7)0.0068 (7)0.0086 (6)0.0019 (5)0.0002 (6)0.0010 (6)
C60.0093 (7)0.0081 (7)0.0101 (6)0.0002 (5)0.0004 (6)0.0014 (6)
C10.0093 (6)0.0081 (7)0.0094 (7)0.0011 (5)0.0025 (5)0.0003 (6)
C20.0104 (7)0.0093 (7)0.0104 (7)0.0005 (6)0.0007 (6)0.0019 (6)
C30.0090 (6)0.0109 (7)0.0109 (7)0.0000 (5)0.0012 (6)0.0003 (6)
C40.0104 (6)0.0076 (6)0.0111 (7)0.0015 (5)0.0004 (6)0.0001 (6)
Geometric parameters (Å, º) top
O1—N21.2379 (17)C6—C11.396 (2)
O2—N21.2307 (18)C6—H60.96 (3)
N1—C11.397 (2)C1—C21.407 (2)
N1—H1A0.83 (3)C2—C31.391 (2)
N1—H1B0.88 (3)C2—H20.92 (3)
N2—C51.466 (2)C3—C41.390 (2)
C5—C61.394 (2)C3—H30.96 (2)
C5—C41.393 (2)C4—H40.95 (2)
O1—N2—C5117.99 (13)C1—C6—H6121.2 (16)
O2—N2—O1123.07 (14)C1—C2—H2117.7 (17)
O2—N2—C5118.94 (13)C2—C3—H3119.9 (14)
N1—C1—C2120.82 (15)C3—C2—C1120.73 (15)
C5—C6—C1118.41 (15)C3—C2—H2121.5 (17)
C5—C6—H6120.4 (16)C3—C4—C5116.59 (14)
C5—C4—H4122.2 (18)C3—C4—H4121.1 (18)
C6—C5—N2117.94 (14)C4—C5—N2118.18 (14)
C6—C1—N1120.18 (14)C4—C5—C6123.88 (15)
C6—C1—C2118.94 (15)C4—C3—C2121.46 (15)
C1—N1—H1A113.7 (16)C4—C3—H3118.7 (14)
C1—N1—H1B116.8 (15)H1A—N1—H1B118 (2)
O1—N2—C5—C6176.72 (14)C5—C6—C1—N1177.17 (14)
O1—N2—C5—C42.2 (2)C5—C6—C1—C20.1 (2)
O2—N2—C5—C63.2 (2)C6—C5—C4—C30.3 (2)
O2—N2—C5—C4177.92 (15)C6—C1—C2—C30.2 (2)
N1—C1—C2—C3177.16 (15)C1—C2—C3—C40.1 (3)
N2—C5—C6—C1178.97 (15)C2—C3—C4—C50.3 (2)
N2—C5—C4—C3179.20 (15)C4—C5—C6—C10.1 (2)
 

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