Supporting information
Crystallographic Information File (CIF) https://doi.org/10.1107/S1600536803016489/ww6100sup1.cif | |
Structure factor file (CIF format) https://doi.org/10.1107/S1600536803016489/ww6100Isup2.hkl |
CCDC reference: 221664
Key indicators
- Single-crystal X-ray study
- T = 223 K
- Mean (C-C) = 0.003 Å
- R factor = 0.033
- wR factor = 0.082
- Data-to-parameter ratio = 18.0
checkCIF results
No syntax errors found ADDSYM reports no extra symmetry
Alert Level C:
ABSTM_02 Alert C The ratio of expected to reported Tmax/Tmin(RR') is < 0.90 Tmin and Tmax reported: 0.739 0.960 Tmin' and Tmax expected: 0.822 0.959 RR' = 0.898 Please check that your absorption correction is appropriate. General Notes
REFLT_03 From the CIF: _diffrn_reflns_theta_max 30.00 From the CIF: _reflns_number_total 3200 Count of symmetry unique reflns 1689 Completeness (_total/calc) 189.46% TEST3: Check Friedels for noncentro structure Estimate of Friedel pairs measured 1511 Fraction of Friedel pairs measured 0.895 Are heavy atom types Z>Si present yes Please check that the estimate of the number of Friedel pairs is correct. If it is not, please give the correct count in the _publ_section_exptl_refinement section of the submitted CIF.
0 Alert Level A = Potentially serious problem
0 Alert Level B = Potential problem
1 Alert Level C = Please check
Data collection: SMART (Bruker, 2000); cell refinement: SAINT (Bruker, 2000); data reduction: SHELXTL (Bruker, 2000); program(s) used to solve structure: PATTY in DIRDIF92 (Beurskens et al., 1992); program(s) used to refine structure: SHELXL97 (Sheldrick, 1997); molecular graphics: ORTEPII (Johnson, 1976); software used to prepare material for publication: SHELXL97.
[Co(C12H8N2)2(N3)2]NO3 | F(000) = 1152 |
Mr = 565.41 | Dx = 1.686 Mg m−3 |
Orthorhombic, Iba2 | Mo Kα radiation, λ = 0.71069 Å |
Hall symbol: I 2 -2c | Cell parameters from 3743 reflections |
a = 15.4858 (6) Å | θ = 2.5–29.0° |
b = 9.7359 (4) Å | µ = 0.83 mm−1 |
c = 14.7769 (8) Å | T = 223 K |
V = 2227.89 (17) Å3 | Block, brown |
Z = 4 | 0.23 × 0.23 × 0.05 mm |
Bruker AXS SMART CCD diffractometer | 3200 independent reflections |
Radiation source: fine-focus sealed tube | 2868 reflections with I > 2σ(I) |
Graphite monochromator | Rint = 0.037 |
ω scans | θmax = 30.0°, θmin = 2.5° |
Absorption correction: multi-scan (SADABS, Bruker, 2000; Blessing, 1995) | h = −16→21 |
Tmin = 0.739, Tmax = 0.960 | k = −13→11 |
8877 measured reflections | l = −20→20 |
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)] = 0.033 | H-atom parameters constrained |
wR(F2) = 0.082 | w = 1/[σ2(Fo2) + (0.0514P)2] where P = (Fo2 + 2Fc2)/3 |
S = 1.00 | (Δ/σ)max < 0.001 |
3200 reflections | Δρmax = 0.56 e Å−3 |
178 parameters | Δρmin = −0.25 e Å−3 |
1 restraint | Absolute structure: Flack (1983), 0000 Friedel pairs |
Primary atom site location: structure-invariant direct methods | Absolute structure parameter: −0.033 (14) |
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 | ||
Co | 0.0000 | 0.0000 | −0.00392 (3) | 0.01734 (8) | |
O1 | −0.5000 | 0.0000 | −0.5083 (3) | 0.0612 (8) | |
O2 | −0.56843 (13) | −0.0141 (2) | −0.38222 (17) | 0.0564 (6) | |
N1 | −0.03337 (12) | −0.13482 (19) | 0.08542 (13) | 0.0275 (4) | |
N2 | −0.08184 (10) | −0.10418 (18) | 0.14527 (10) | 0.0254 (3) | |
N3 | −0.12953 (15) | −0.0837 (2) | 0.20354 (14) | 0.0444 (5) | |
N4 | 0.11657 (8) | −0.07178 (13) | −0.00368 (13) | 0.0200 (3) | |
N5 | 0.04371 (10) | 0.12165 (17) | −0.09839 (10) | 0.0203 (3) | |
N6 | −0.5000 | 0.0000 | −0.4248 (2) | 0.0349 (6) | |
C1 | 0.14995 (12) | −0.1709 (2) | 0.04744 (13) | 0.0258 (4) | |
H1 | 0.1131 | −0.2253 | 0.0831 | 0.031* | |
C2 | 0.23908 (13) | −0.1956 (2) | 0.04898 (14) | 0.0292 (4) | |
H2 | 0.2614 | −0.2648 | 0.0866 | 0.035* | |
C3 | 0.29422 (10) | −0.11938 (19) | −0.00410 (16) | 0.0275 (3) | |
H3 | 0.3541 | −0.1348 | −0.0022 | 0.033* | |
C4 | 0.25943 (12) | −0.01814 (19) | −0.06115 (16) | 0.0245 (4) | |
C5 | 0.17009 (12) | 0.00255 (17) | −0.05818 (14) | 0.0205 (3) | |
C6 | 0.13025 (11) | 0.10457 (18) | −0.11180 (12) | 0.0207 (3) | |
C7 | 0.17810 (12) | 0.1817 (2) | −0.17410 (13) | 0.0244 (4) | |
C8 | 0.13255 (13) | 0.2782 (2) | −0.22603 (13) | 0.0278 (4) | |
H8 | 0.1616 | 0.3322 | −0.2691 | 0.033* | |
C9 | 0.04523 (14) | 0.2931 (2) | −0.21343 (14) | 0.0288 (4) | |
H9 | 0.0140 | 0.3563 | −0.2486 | 0.035* | |
C10 | 0.00285 (11) | 0.2142 (2) | −0.14820 (15) | 0.0246 (4) | |
H10 | −0.0567 | 0.2271 | −0.1394 | 0.030* | |
C11 | 0.30841 (12) | 0.0648 (2) | −0.12395 (16) | 0.0309 (4) | |
H11 | 0.3687 | 0.0541 | −0.1270 | 0.037* | |
C12 | 0.26935 (14) | 0.1572 (2) | −0.17825 (15) | 0.0317 (4) | |
H12 | 0.3029 | 0.2070 | −0.2200 | 0.038* |
U11 | U22 | U33 | U12 | U13 | U23 | |
Co | 0.01613 (13) | 0.01956 (14) | 0.01633 (13) | 0.00045 (10) | 0.000 | 0.000 |
O1 | 0.0437 (13) | 0.103 (2) | 0.0365 (14) | 0.0159 (12) | 0.000 | 0.000 |
O2 | 0.0390 (10) | 0.0718 (15) | 0.0584 (14) | 0.0093 (9) | 0.0117 (10) | 0.0319 (10) |
N1 | 0.0288 (8) | 0.0280 (9) | 0.0258 (9) | 0.0019 (7) | 0.0050 (7) | 0.0059 (7) |
N2 | 0.0276 (8) | 0.0249 (8) | 0.0238 (8) | −0.0028 (6) | 0.0015 (6) | 0.0037 (6) |
N3 | 0.0540 (12) | 0.0436 (11) | 0.0355 (11) | 0.0025 (10) | 0.0213 (9) | 0.0042 (9) |
N4 | 0.0185 (6) | 0.0224 (7) | 0.0191 (6) | 0.0001 (5) | −0.0008 (7) | 0.0007 (7) |
N5 | 0.0218 (8) | 0.0210 (8) | 0.0182 (8) | −0.0014 (6) | −0.0005 (6) | −0.0009 (6) |
N6 | 0.0341 (14) | 0.0342 (15) | 0.0364 (15) | 0.0090 (10) | 0.000 | 0.000 |
C1 | 0.0269 (9) | 0.0275 (10) | 0.0230 (9) | 0.0035 (7) | −0.0019 (7) | 0.0024 (7) |
C2 | 0.0290 (9) | 0.0321 (10) | 0.0266 (9) | 0.0072 (8) | −0.0067 (8) | −0.0013 (8) |
C3 | 0.0195 (7) | 0.0304 (9) | 0.0325 (9) | 0.0043 (6) | −0.0047 (9) | −0.0095 (10) |
C4 | 0.0176 (8) | 0.0256 (10) | 0.0304 (10) | −0.0024 (6) | 0.0004 (7) | −0.0087 (7) |
C5 | 0.0190 (8) | 0.0207 (8) | 0.0219 (8) | −0.0012 (6) | 0.0002 (6) | −0.0044 (6) |
C6 | 0.0210 (7) | 0.0211 (8) | 0.0198 (8) | −0.0036 (7) | 0.0008 (6) | −0.0030 (7) |
C7 | 0.0266 (9) | 0.0230 (9) | 0.0235 (9) | −0.0068 (7) | 0.0022 (7) | −0.0033 (7) |
C8 | 0.0374 (10) | 0.0252 (9) | 0.0207 (8) | −0.0086 (7) | 0.0020 (7) | 0.0007 (7) |
C9 | 0.0358 (10) | 0.0273 (10) | 0.0232 (9) | −0.0030 (8) | −0.0027 (8) | 0.0037 (8) |
C10 | 0.0248 (9) | 0.0253 (10) | 0.0237 (9) | 0.0012 (7) | −0.0032 (6) | 0.0014 (7) |
C11 | 0.0187 (8) | 0.0309 (11) | 0.0431 (11) | −0.0048 (7) | 0.0071 (8) | −0.0079 (9) |
C12 | 0.0294 (10) | 0.0313 (11) | 0.0345 (10) | −0.0098 (8) | 0.0103 (8) | −0.0049 (9) |
Co—N1i | 1.9320 (18) | C2—H2 | 0.9400 |
Co—N1 | 1.9320 (18) | C3—C4 | 1.404 (3) |
Co—N4i | 1.9358 (12) | C3—H3 | 0.9400 |
Co—N4 | 1.9358 (12) | C4—C5 | 1.399 (3) |
Co—N5i | 1.9518 (16) | C4—C11 | 1.445 (3) |
Co—N5 | 1.9518 (16) | C5—C6 | 1.412 (3) |
O1—N6 | 1.233 (6) | C6—C7 | 1.400 (3) |
O2—N6 | 1.240 (3) | C7—C8 | 1.403 (3) |
N1—N2 | 1.198 (2) | C7—C12 | 1.434 (3) |
N2—N3 | 1.152 (2) | C8—C9 | 1.373 (3) |
N4—C1 | 1.330 (2) | C8—H8 | 0.9400 |
N4—C5 | 1.364 (2) | C9—C10 | 1.397 (3) |
N5—C10 | 1.324 (3) | C9—H9 | 0.9400 |
N5—C6 | 1.365 (2) | C10—H10 | 0.9400 |
N6—O2ii | 1.240 (3) | C11—C12 | 1.349 (3) |
C1—C2 | 1.401 (3) | C11—H11 | 0.9400 |
C1—H1 | 0.9400 | C12—H12 | 0.9400 |
C2—C3 | 1.376 (3) | ||
N1—Co—N4 | 90.16 (7) | C1—C2—H2 | 119.7 |
N1—Co—N5 | 173.57 (8) | C2—C3—C4 | 118.83 (16) |
N1—Co—N1i | 93.80 (12) | C2—C3—H3 | 120.6 |
N1—Co—N4i | 89.69 (7) | C4—C3—H3 | 120.6 |
N1—Co—N5i | 89.06 (6) | C5—C4—C3 | 117.49 (18) |
N4—Co—N5 | 84.09 (7) | C5—C4—C11 | 117.30 (19) |
N4—Co—N4i | 179.79 (12) | C3—C4—C11 | 125.19 (18) |
N4—Co—N5i | 96.06 (7) | N4—C5—C4 | 122.90 (18) |
N5—Co—N5i | 88.68 (9) | N4—C5—C6 | 116.05 (16) |
N1i—Co—N4 | 89.69 (7) | C4—C5—C6 | 121.05 (18) |
N1i—Co—N4i | 90.16 (7) | N5—C6—C7 | 123.36 (17) |
N1i—Co—N5i | 173.57 (8) | N5—C6—C5 | 115.67 (16) |
N4i—Co—N5i | 84.09 (7) | C7—C6—C5 | 120.98 (16) |
N1i—Co—N5 | 89.06 (6) | C6—C7—C8 | 116.90 (17) |
N4i—Co—N5 | 96.06 (7) | C6—C7—C12 | 117.42 (18) |
Co—N1—N2 | 120.19 (15) | C8—C7—C12 | 125.67 (18) |
N1—N2—N3 | 175.6 (2) | C9—C8—C7 | 119.47 (18) |
C1—N4—C5 | 118.97 (15) | C9—C8—H8 | 120.3 |
C1—N4—Co | 128.71 (13) | C7—C8—H8 | 120.3 |
C5—N4—Co | 111.97 (12) | C8—C9—C10 | 119.89 (18) |
C10—N5—C6 | 118.12 (16) | C8—C9—H9 | 120.1 |
C10—N5—Co | 130.13 (13) | C10—C9—H9 | 120.1 |
C6—N5—Co | 111.74 (12) | N5—C10—C9 | 122.23 (17) |
O1—N6—O2ii | 120.48 (18) | N5—C10—H10 | 118.9 |
O1—N6—O2 | 120.48 (18) | C9—C10—H10 | 118.9 |
O2ii—N6—O2 | 119.0 (4) | C12—C11—C4 | 121.30 (17) |
N4—C1—C2 | 121.08 (18) | C12—C11—H11 | 119.4 |
N4—C1—H1 | 119.5 | C4—C11—H11 | 119.4 |
C2—C1—H1 | 119.5 | C11—C12—C7 | 121.81 (18) |
C3—C2—C1 | 120.64 (19) | C11—C12—H12 | 119.1 |
C3—C2—H2 | 119.7 | C7—C12—H12 | 119.1 |
Symmetry codes: (i) −x, −y, z; (ii) −x−1, −y, z. |
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