Download citation
Download citation
link to html
The new generation of X-ray detectors, the hybrid pixel area detectors or `pixel detectors', is based on direct detection and single-photon counting processes. A large linearity range, high dynamic and extremely low noise leading to an unprecedented high signal-to-noise ratio, fast readout time (high frame rates) and an electronic shutter are among their intrinsic characteristics which render them very attractive. First used on synchrotron beamlines, these detectors are also promising in the laboratory, in particular for pump-probe or quasi-static experiments and accurate electron density measurements, as explained in this paper. An original laboratory diffractometer made from a Nonius Mach3 goniometer equipped with an Incoatec Mo microsource and an XPAD pixel area detector has been developed at the CRM2 laboratory. Mo Kα accurate charge density quality data up to 1.21 Å−1 resolution have been collected on a sodium nitroprusside crystal using this home-made diffractometer. Data quality for charge density analysis based on multipolar modelling are discussed in this paper. Deformation electron densities are compared to those already published (based on data collected with CCD APEXII and CAD4 diffractometers).

Supporting information

cif

Crystallographic Information File (CIF) https://doi.org/10.1107/S2052520614017338/gw5033sup1.cif
Contains datablock I

hkl

Structure factor file (CIF format) https://doi.org/10.1107/S2052520614017338/gw5033Isup2.hkl
Contains datablock I

txt

Text file https://doi.org/10.1107/S2052520614017338/gw5033sup3.txt
Output file of multipolar model refinement software

CCDC reference: 1016354

Computing details top

Data collection: CAD4, Bruker-Nonius; cell refinement: CrysAlis PRO, Agilent Technologies, Version 1.171.37.31 (release 14-01-2014 CrysAlis171 .NET) (compiled Jan 14 2014,18:38:05); data reduction: CrysAlis PRO, Agilent Technologies, Version 1.171.37.31 (release 14-01-2014 CrysAlis171 .NET) (compiled Jan 14 2014,18:38:05); program(s) used to solve structure: SIR92; program(s) used to refine structure: SHELXL2013 (Sheldrick, 2013); molecular graphics: ORTEP-3 for Windows (Farrugia, 1997); software used to prepare material for publication: ShelXle, C. B. Hubschle, G. M. Sheldrick and B. Dittrich.

Figures top
[Figure 1]
[Figure 2]
[Figure 3]
[Figure 4]
[Figure 5]
[Figure 6]
[Figure 7]
[Figure 8]
[Figure 9]
[Figure 10]
(I) top
Crystal data top
C5H4FeN6Na2O3Dx = 1.750 Mg m3
Mr = 297.97Mo Kα radiation, λ = 0.71073 Å
Orthorhombic, PnnmCell parameters from 213934 reflections
a = 6.14102 (7) Åθ = 2.2–59.4°
b = 11.84510 (16) ŵ = 1.41 mm1
c = 15.5509 (3) ÅT = 100 K
V = 1131.19 (3) Å3Prismatic, red
Z = 40.22 × 0.19 × 0.17 mm
F(000) = 592
Data collection top
Pixel detector XPAD 3.2
diffractometer
6059 reflections with I > 2σ(I)
ω scansRint = 0.034
Absorption correction: multi-scan
CrysAlis PRO, Agilent Technologies, Version 1.171.36.32 (release 02-08-2013 CrysAlis171 .NET) (compiled Aug 2 2013,16:46:58) Empirical absorption correction using spherical harmonics, implemented in SCALE3 ABSPACK scaling algorithm.
θmax = 59.4°, θmin = 2.2°
Tmin = 0.741, Tmax = 0.785h = 014
213934 measured reflectionsk = 028
8273 independent reflectionsl = 037
Refinement top
Refinement on F23 restraints
Least-squares matrix: fullHydrogen site location: difference Fourier map
R[F2 > 2σ(F2)] = 0.025All H-atom parameters refined
wR(F2) = 0.062 w = 1/[σ2(Fo2)]
where P = (Fo2 + 2Fc2)/3
S = 0.90(Δ/σ)max = 0.001
8273 reflectionsΔρmax = 0.97 e Å3
95 parametersΔρmin = 1.15 e Å3
Crystal data top
C5H4FeN6Na2O3V = 1131.19 (3) Å3
Mr = 297.97Z = 4
Orthorhombic, PnnmMo Kα radiation
a = 6.14102 (7) ŵ = 1.41 mm1
b = 11.84510 (16) ÅT = 100 K
c = 15.5509 (3) Å0.22 × 0.19 × 0.17 mm
Data collection top
Pixel detector XPAD 3.2
diffractometer
8273 independent reflections
Absorption correction: multi-scan
CrysAlis PRO, Agilent Technologies, Version 1.171.36.32 (release 02-08-2013 CrysAlis171 .NET) (compiled Aug 2 2013,16:46:58) Empirical absorption correction using spherical harmonics, implemented in SCALE3 ABSPACK scaling algorithm.
6059 reflections with I > 2σ(I)
Tmin = 0.741, Tmax = 0.785Rint = 0.034
213934 measured reflections
Refinement top
R[F2 > 2σ(F2)] = 0.0253 restraints
wR(F2) = 0.062All H-atom parameters refined
S = 0.90Δρmax = 0.97 e Å3
8273 reflectionsΔρmin = 1.15 e Å3
95 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.

Fractional atomic coordinates and isotropic or equivalent isotropic displacement parameters (Å2) top
xyzUiso*/Ueq
Fe0.50052 (2)0.28023 (2)0.50000.006290 (10)
N40.72604 (9)0.35805 (5)0.50000.00934 (7)
O0.88629 (11)0.40525 (6)0.50000.01922 (11)
C10.25010 (11)0.18273 (6)0.50000.01001 (8)
N10.10007 (11)0.12369 (6)0.50000.01481 (10)
C20.60742 (8)0.17946 (4)0.58803 (3)0.00994 (6)
N20.66722 (8)0.11964 (4)0.64187 (3)0.01474 (7)
C30.34548 (8)0.36188 (4)0.41087 (3)0.01034 (6)
N30.25007 (9)0.40533 (5)0.35576 (3)0.01647 (8)
Na10.50000.00000.24581 (2)0.01106 (4)
Na20.00000.00000.37803 (2)0.01295 (5)
OW10.17207 (8)0.12262 (4)0.26871 (3)0.01659 (7)
H10.1810 (19)0.1885 (9)0.2867 (7)0.048 (3)*
H20.061 (2)0.1216 (11)0.2352 (7)0.060 (4)*
Atomic displacement parameters (Å2) top
U11U22U33U12U13U23
Fe0.00623 (2)0.00685 (2)0.00578 (2)0.00032 (3)0.0000.000
N40.00840 (16)0.00878 (16)0.01084 (17)0.00104 (13)0.0000.000
O0.0119 (2)0.0174 (2)0.0284 (3)0.00698 (18)0.0000.000
C10.00975 (19)0.0106 (2)0.00964 (18)0.00186 (17)0.0000.000
N10.0129 (2)0.0152 (2)0.0164 (2)0.00550 (19)0.0000.000
C20.00949 (13)0.01097 (14)0.00936 (13)0.00046 (11)0.00012 (11)0.00144 (11)
N20.01433 (16)0.01660 (16)0.01328 (15)0.00205 (14)0.00008 (13)0.00578 (13)
C30.01007 (13)0.01224 (14)0.00871 (13)0.00117 (12)0.00002 (11)0.00114 (11)
N30.01589 (17)0.0215 (2)0.01200 (14)0.00383 (15)0.00158 (13)0.00469 (14)
Na10.01141 (11)0.01263 (11)0.00914 (9)0.00228 (10)0.0000.000
Na20.01227 (11)0.01454 (12)0.01205 (11)0.00094 (11)0.0000.000
OW10.01604 (16)0.01664 (16)0.01708 (15)0.00135 (13)0.00245 (13)0.00190 (13)
Geometric parameters (Å, º) top
Fe—N41.6636 (6)Na1—N2i2.4726 (5)
Fe—C11.9232 (7)Na1—N2iii2.4726 (5)
Fe—C21.9312 (5)Na1—OW12.5084 (5)
Fe—C2i1.9312 (5)Na1—OW1vii2.5084 (5)
Fe—C31.9399 (5)Na1—Na2viii3.6954 (3)
Fe—C3i1.9400 (5)Na1—Na23.6954 (3)
N4—O1.1319 (8)Na2—OW12.4731 (5)
C1—N11.1567 (9)Na2—OW1ix2.4732 (5)
N1—Na22.4742 (5)Na2—N1ii2.4743 (5)
N1—Na2ii2.4743 (5)Na2—N2x2.5061 (5)
C2—N21.1567 (6)Na2—N2iii2.5061 (5)
N2—Na1iii2.4727 (5)Na2—Na1xi3.6954 (3)
N2—Na2iii2.5061 (5)Na2—Na2ii3.7935 (7)
C3—N31.1586 (6)Na2—H22.673 (12)
N3—Na1iv2.4720 (5)OW1—H10.831 (11)
Na1—N3v2.4720 (5)OW1—H20.858 (12)
Na1—N3vi2.4720 (5)
N4—Fe—C1176.74 (3)Na2viii—Na1—Na2112.382 (12)
N4—Fe—C293.41 (2)OW1—Na2—OW1ix93.15 (3)
C1—Fe—C284.30 (2)OW1—Na2—N194.190 (16)
N4—Fe—C2i93.41 (2)OW1ix—Na2—N1168.770 (19)
C1—Fe—C2i84.30 (2)OW1—Na2—N1ii168.770 (19)
C2—Fe—C2i90.28 (3)OW1ix—Na2—N1ii94.189 (16)
N4—Fe—C397.60 (2)N1—Na2—N1ii79.90 (3)
C1—Fe—C384.66 (2)OW1—Na2—N2x86.067 (17)
C2—Fe—C3168.95 (2)OW1ix—Na2—N2x84.193 (16)
C2i—Fe—C388.20 (2)N1—Na2—N2x87.84 (2)
N4—Fe—C3i97.60 (2)N1ii—Na2—N2x103.12 (2)
C1—Fe—C3i84.66 (2)OW1—Na2—N2iii84.192 (16)
C2—Fe—C3i88.20 (2)OW1ix—Na2—N2iii86.067 (17)
C2i—Fe—C3i168.95 (2)N1—Na2—N2iii103.12 (2)
C3—Fe—C3i91.21 (3)N1ii—Na2—N2iii87.84 (2)
O—N4—Fe175.96 (6)N2x—Na2—N2iii165.81 (3)
N1—C1—Fe179.70 (7)OW1—Na2—Na142.482 (11)
C1—N1—Na2123.77 (3)OW1ix—Na2—Na188.424 (14)
C1—N1—Na2ii123.77 (3)N1—Na2—Na1102.720 (15)
Na2—N1—Na2ii100.10 (3)N1ii—Na2—Na1129.265 (18)
N2—C2—Fe178.42 (5)N2x—Na2—Na1127.507 (15)
C2—N2—Na1iii136.94 (4)N2iii—Na2—Na141.731 (11)
C2—N2—Na2iii121.06 (4)OW1—Na2—Na1xi88.425 (14)
Na1iii—N2—Na2iii95.843 (16)OW1ix—Na2—Na1xi42.482 (11)
N3—C3—Fe176.46 (5)N1—Na2—Na1xi129.266 (18)
C3—N3—Na1iv171.19 (4)N1ii—Na2—Na1xi102.720 (15)
N3v—Na1—N3vi100.57 (3)N2x—Na2—Na1xi41.731 (11)
N3v—Na1—N2i165.785 (17)N2iii—Na2—Na1xi127.507 (15)
N3vi—Na1—N2i86.181 (17)Na1—Na2—Na1xi112.382 (12)
N3v—Na1—N2iii86.181 (17)OW1—Na2—Na2ii133.425 (13)
N3vi—Na1—N2iii165.785 (17)OW1ix—Na2—Na2ii133.425 (13)
N2i—Na1—N2iii90.11 (3)N1—Na2—Na2ii39.951 (13)
N3v—Na1—OW181.643 (17)N1ii—Na2—Na2ii39.952 (13)
N3vi—Na1—OW1109.075 (18)N2x—Na2—Na2ii97.093 (13)
N2i—Na1—OW184.333 (17)N2iii—Na2—Na2ii97.093 (13)
N2iii—Na1—OW184.153 (16)Na1—Na2—Na2ii123.809 (6)
N3v—Na1—OW1vii109.074 (18)Na1xi—Na2—Na2ii123.809 (6)
N3vi—Na1—OW1vii81.643 (17)OW1—Na2—H218.7 (3)
N2i—Na1—OW1vii84.154 (16)OW1ix—Na2—H278.8 (3)
N2iii—Na1—OW1vii84.333 (17)N1—Na2—H2106.4 (3)
OW1—Na1—OW1vii163.67 (3)N1ii—Na2—H2172.2 (3)
N3v—Na1—Na2viii150.659 (13)N2x—Na2—H273.0 (3)
N3vi—Na1—Na2viii80.755 (13)N2iii—Na2—H295.0 (3)
N2i—Na1—Na2viii42.425 (12)Na1—Na2—H254.6 (3)
N2iii—Na1—Na2viii87.249 (14)Na1xi—Na2—H269.8 (3)
OW1—Na1—Na2viii126.020 (14)Na2ii—Na2—H2146.2 (3)
OW1vii—Na1—Na2viii41.749 (11)Na2—OW1—Na195.771 (16)
N3v—Na1—Na280.755 (13)Na2—OW1—H1110.4 (8)
N3vi—Na1—Na2150.659 (13)Na1—OW1—H1122.6 (8)
N2i—Na1—Na287.248 (14)Na2—OW1—H294.0 (8)
N2iii—Na1—Na242.425 (12)Na1—OW1—H2122.9 (8)
OW1—Na1—Na241.748 (11)H1—OW1—H2105.7 (11)
OW1vii—Na1—Na2126.020 (14)
Symmetry codes: (i) x, y, z+1; (ii) x, y, z+1; (iii) x+1, y, z+1; (iv) x1/2, y+1/2, z+1/2; (v) x+1/2, y1/2, z+1/2; (vi) x+1/2, y+1/2, z+1/2; (vii) x+1, y, z; (viii) x+1, y, z; (ix) x, y, z; (x) x1, y, z+1; (xi) x1, y, z.

Experimental details

Crystal data
Chemical formulaC5H4FeN6Na2O3
Mr297.97
Crystal system, space groupOrthorhombic, Pnnm
Temperature (K)100
a, b, c (Å)6.14102 (7), 11.84510 (16), 15.5509 (3)
V3)1131.19 (3)
Z4
Radiation typeMo Kα
µ (mm1)1.41
Crystal size (mm)0.22 × 0.19 × 0.17
Data collection
DiffractometerPixel detector XPAD 3.2
diffractometer
Absorption correctionMulti-scan
CrysAlis PRO, Agilent Technologies, Version 1.171.36.32 (release 02-08-2013 CrysAlis171 .NET) (compiled Aug 2 2013,16:46:58) Empirical absorption correction using spherical harmonics, implemented in SCALE3 ABSPACK scaling algorithm.
Tmin, Tmax0.741, 0.785
No. of measured, independent and
observed [I > 2σ(I)] reflections
213934, 8273, 6059
Rint0.034
(sin θ/λ)max1)1.210
Refinement
R[F2 > 2σ(F2)], wR(F2), S 0.025, 0.062, 0.90
No. of reflections8273
No. of parameters95
No. of restraints3
H-atom treatmentAll H-atom parameters refined
Δρmax, Δρmin (e Å3)0.97, 1.15

Computer programs: CAD4, Bruker-Nonius, CrysAlis PRO, Agilent Technologies, Version 1.171.37.31 (release 14-01-2014 CrysAlis171 .NET) (compiled Jan 14 2014,18:38:05), SIR92, SHELXL2013 (Sheldrick, 2013), ORTEP-3 for Windows (Farrugia, 1997), ShelXle, C. B. Hubschle, G. M. Sheldrick and B. Dittrich.

 

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