Supporting information
Crystallographic Information File (CIF) https://doi.org/10.1107/S160053680301643X/bt6314sup1.cif | |
Structure factor file (CIF format) https://doi.org/10.1107/S160053680301643X/bt6314Isup2.hkl |
CCDC reference: 221666
Key indicators
- Single-crystal X-ray study
- T = 150 K
- Mean (C-C) = 0.008 Å
- R factor = 0.067
- wR factor = 0.153
- Data-to-parameter ratio = 16.1
checkCIF results
No syntax errors found ADDSYM reports no extra symmetry
Alert Level C:
RINTA_01 Alert C The value of Rint is greater than 0.10 Rint given 0.102 General Notes
REFLT_03 From the CIF: _diffrn_reflns_theta_max 27.47 From the CIF: _reflns_number_total 4948 Count of symmetry unique reflns 2955 Completeness (_total/calc) 167.45% TEST3: Check Friedels for noncentro structure Estimate of Friedel pairs measured 1993 Fraction of Friedel pairs measured 0.674 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: COLLECT (Nonius BV, 1997-2002); cell refinement: DENZO-SMN (Otwinowski & Minor, 1997); data reduction: DENZO-SMN; program(s) used to solve structure: SHELXTL (Sheldrick, 2001); program(s) used to refine structure: SHELXTL; molecular graphics: SHELXTL; software used to prepare material for publication: SHELXTL.
[Co(NO2)3(C17H25N3O6)]·H2O | F(000) = 1072 |
Mr = 516.36 | Dx = 1.523 Mg m−3 |
Orthorhombic, P212121 | Mo Kα radiation, λ = 0.71073 Å |
Hall symbol: P 2ac 2ab | Cell parameters from 2747 reflections |
a = 6.7185 (3) Å | θ = 2.6–27.5° |
b = 16.5766 (8) Å | µ = 0.82 mm−1 |
c = 20.2149 (10) Å | T = 150 K |
V = 2251.33 (19) Å3 | Needle, colourless |
Z = 4 | 0.10 × 0.04 × 0.03 mm |
Nonius KappaCCD diffractometer | 4948 independent reflections |
Radiation source: fine-focus sealed tube | 3621 reflections with I > 2σ(I) |
Graphite monochromator | Rint = 0.102 |
Detector resolution: 9 pixels mm-1 | θmax = 27.5°, θmin = 3.2° |
φ scans, and ω scans with κ offsets | h = −8→8 |
Absorption correction: multi-scan (DENZO-SMN; Otwinowski & Minor, 1997) | k = −21→21 |
Tmin = 0.922, Tmax = 0.976 | l = −26→26 |
9702 measured reflections |
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)] = 0.067 | H-atom parameters constrained |
wR(F2) = 0.153 | w = 1/[σ2(Fo2) + 0.7005P] where P = (Fo2 + 2Fc2)/3 |
S = 1.06 | (Δ/σ)max = 0.001 |
4948 reflections | Δρmax = 0.71 e Å−3 |
308 parameters | Δρmin = −0.71 e Å−3 |
2 restraints | Absolute structure: Flack (1983); 2017 Friedel pairs |
Primary atom site location: structure-invariant direct methods | Absolute structure parameter: −0.02 (3) |
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 | ||
Co1 | 0.72694 (9) | 0.13797 (4) | 0.77949 (3) | 0.02465 (19) | |
O1 | 0.4723 (6) | −0.0247 (2) | 0.89840 (18) | 0.0355 (9) | |
O2 | 1.0154 (6) | 0.0784 (3) | 0.61241 (17) | 0.0352 (9) | |
O3 | 0.3666 (7) | 0.0876 (3) | 0.7214 (3) | 0.0555 (12) | |
O4 | 0.4164 (6) | 0.2136 (2) | 0.7134 (2) | 0.0435 (10) | |
O5 | 0.8068 (6) | 0.3004 (2) | 0.77423 (19) | 0.0412 (10) | |
O6 | 0.6007 (7) | 0.2694 (3) | 0.85087 (19) | 0.0410 (10) | |
O7 | 1.0786 (7) | 0.1856 (3) | 0.8416 (2) | 0.0539 (13) | |
O8 | 1.0434 (8) | 0.0589 (3) | 0.8380 (3) | 0.0598 (14) | |
N1 | 0.5900 (7) | 0.0909 (3) | 0.8551 (2) | 0.0278 (10) | |
N2 | 0.7368 (7) | 0.0273 (3) | 0.75423 (18) | 0.0263 (9) | |
N3 | 0.8723 (6) | 0.1487 (3) | 0.69513 (19) | 0.0250 (9) | |
N4 | 0.9814 (7) | 0.1274 (3) | 0.8245 (2) | 0.0307 (10) | |
N5 | 0.7125 (7) | 0.2486 (3) | 0.8041 (2) | 0.0300 (10) | |
N6 | 0.4726 (6) | 0.1471 (3) | 0.73255 (19) | 0.0294 (10) | |
C1 | 0.5074 (8) | 0.1164 (3) | 0.9199 (2) | 0.0297 (12) | |
H1A | 0.4114 | 0.1617 | 0.9131 | 0.036* | |
C2 | 0.3938 (9) | 0.0408 (4) | 0.9414 (3) | 0.0342 (13) | |
H2A | 0.4188 | 0.0286 | 0.9886 | 0.041* | |
H2B | 0.2489 | 0.0478 | 0.9347 | 0.041* | |
C3 | 0.5661 (8) | 0.0138 (3) | 0.8502 (2) | 0.0273 (11) | |
C4 | 0.6529 (8) | −0.0278 (3) | 0.7933 (2) | 0.0274 (11) | |
C5 | 0.6561 (8) | −0.1091 (3) | 0.7761 (3) | 0.0350 (12) | |
H5A | 0.5892 | −0.1481 | 0.8024 | 0.042* | |
C6 | 0.7588 (8) | −0.1315 (3) | 0.7202 (3) | 0.0372 (11) | |
H6A | 0.7656 | −0.1868 | 0.7083 | 0.045* | |
C7 | 0.8533 (9) | −0.0736 (4) | 0.6807 (3) | 0.0339 (13) | |
H7A | 0.9267 | −0.0890 | 0.6426 | 0.041* | |
C8 | 0.8364 (8) | 0.0066 (3) | 0.6989 (3) | 0.0299 (12) | |
C9 | 0.9108 (8) | 0.0800 (4) | 0.6680 (2) | 0.0290 (12) | |
C10 | 1.0855 (9) | 0.1628 (4) | 0.6038 (3) | 0.0340 (13) | |
H10A | 1.0618 | 0.1816 | 0.5580 | 0.041* | |
H10B | 1.2295 | 0.1671 | 0.6136 | 0.041* | |
C11 | 0.9619 (8) | 0.2133 (3) | 0.6538 (3) | 0.0288 (12) | |
H11A | 1.0540 | 0.2464 | 0.6816 | 0.035* | |
C12 | 0.6738 (8) | 0.1436 (4) | 0.9676 (2) | 0.0326 (12) | |
H12A | 0.7625 | 0.1812 | 0.9426 | 0.039* | |
C13 | 0.8029 (9) | 0.0734 (4) | 0.9917 (3) | 0.0436 (15) | |
H13A | 0.9166 | 0.0945 | 1.0167 | 0.065* | |
H13B | 0.8512 | 0.0426 | 0.9536 | 0.065* | |
H13C | 0.7236 | 0.0381 | 1.0203 | 0.065* | |
C14 | 0.5855 (10) | 0.1907 (4) | 1.0242 (3) | 0.0437 (15) | |
H14A | 0.6884 | 0.2009 | 1.0575 | 0.066* | |
H14B | 0.4770 | 0.1595 | 1.0442 | 0.066* | |
H14C | 0.5335 | 0.2421 | 1.0078 | 0.066* | |
C15 | 0.8066 (8) | 0.2685 (3) | 0.6219 (3) | 0.0358 (13) | |
H15A | 0.7197 | 0.2895 | 0.6582 | 0.043* | |
C16 | 0.6732 (9) | 0.2259 (5) | 0.5730 (3) | 0.0504 (18) | |
H16A | 0.6203 | 0.1766 | 0.5932 | 0.076* | |
H16B | 0.7499 | 0.2120 | 0.5334 | 0.076* | |
H16C | 0.5628 | 0.2615 | 0.5607 | 0.076* | |
C17 | 0.9122 (11) | 0.3412 (4) | 0.5909 (3) | 0.0554 (19) | |
H17A | 0.8145 | 0.3749 | 0.5679 | 0.083* | |
H17B | 1.0124 | 0.3222 | 0.5593 | 0.083* | |
H17C | 0.9771 | 0.3728 | 0.6257 | 0.083* | |
O1W | 0.6804 (11) | 0.4392 (4) | 0.8881 (3) | 0.095 (2) | |
H1W | 0.715 | 0.471 | 0.858 | 0.114* | |
H2W | 0.668 | 0.393 | 0.871 | 0.114* |
U11 | U22 | U33 | U12 | U13 | U23 | |
Co1 | 0.0240 (3) | 0.0252 (3) | 0.0248 (3) | 0.0001 (3) | −0.0008 (3) | 0.0002 (3) |
O1 | 0.036 (2) | 0.031 (2) | 0.040 (2) | −0.0048 (17) | 0.0065 (17) | 0.0071 (18) |
O2 | 0.039 (2) | 0.038 (2) | 0.0282 (19) | 0.0024 (18) | 0.0045 (17) | −0.0029 (17) |
O3 | 0.044 (3) | 0.039 (3) | 0.084 (3) | −0.010 (2) | −0.031 (3) | 0.008 (2) |
O4 | 0.039 (2) | 0.032 (2) | 0.059 (3) | 0.0048 (17) | −0.011 (2) | 0.002 (2) |
O5 | 0.044 (2) | 0.033 (2) | 0.046 (2) | −0.0069 (17) | 0.008 (2) | −0.0034 (19) |
O6 | 0.052 (3) | 0.033 (2) | 0.038 (2) | 0.0011 (19) | 0.008 (2) | −0.0075 (18) |
O7 | 0.046 (3) | 0.040 (3) | 0.075 (3) | −0.006 (2) | −0.027 (3) | −0.002 (2) |
O8 | 0.047 (3) | 0.042 (3) | 0.090 (4) | 0.011 (2) | −0.034 (3) | −0.001 (3) |
N1 | 0.024 (2) | 0.029 (3) | 0.030 (2) | 0.0017 (18) | 0.0034 (18) | −0.0005 (19) |
N2 | 0.020 (2) | 0.032 (2) | 0.0263 (18) | 0.002 (2) | −0.0026 (18) | 0.0021 (17) |
N3 | 0.021 (2) | 0.029 (2) | 0.0249 (18) | −0.0016 (19) | −0.0005 (16) | 0.0011 (19) |
N4 | 0.027 (2) | 0.036 (3) | 0.029 (2) | −0.004 (2) | 0.0030 (17) | 0.000 (2) |
N5 | 0.028 (2) | 0.032 (2) | 0.030 (2) | −0.006 (2) | −0.0012 (18) | −0.0002 (19) |
N6 | 0.033 (2) | 0.028 (2) | 0.027 (2) | 0.001 (2) | 0.0028 (17) | 0.001 (2) |
C1 | 0.027 (3) | 0.039 (3) | 0.024 (2) | 0.005 (2) | 0.006 (2) | −0.004 (2) |
C2 | 0.027 (3) | 0.041 (3) | 0.034 (3) | −0.002 (2) | 0.006 (2) | −0.004 (2) |
C3 | 0.019 (3) | 0.032 (3) | 0.030 (3) | 0.000 (2) | −0.001 (2) | 0.004 (2) |
C4 | 0.026 (3) | 0.028 (3) | 0.028 (3) | −0.003 (2) | −0.005 (2) | 0.004 (2) |
C5 | 0.036 (3) | 0.027 (3) | 0.041 (3) | −0.004 (2) | −0.003 (3) | 0.003 (3) |
C6 | 0.042 (3) | 0.025 (3) | 0.044 (3) | 0.003 (3) | 0.003 (3) | −0.007 (3) |
C7 | 0.034 (3) | 0.036 (3) | 0.032 (3) | 0.004 (2) | −0.001 (2) | −0.008 (2) |
C8 | 0.026 (3) | 0.035 (3) | 0.028 (2) | 0.002 (2) | 0.001 (2) | −0.004 (2) |
C9 | 0.025 (3) | 0.038 (3) | 0.024 (2) | 0.000 (2) | 0.001 (2) | −0.003 (2) |
C10 | 0.029 (3) | 0.041 (4) | 0.031 (3) | −0.003 (2) | 0.004 (2) | 0.003 (2) |
C11 | 0.025 (3) | 0.034 (3) | 0.028 (3) | 0.001 (2) | 0.002 (2) | 0.003 (2) |
C12 | 0.034 (3) | 0.038 (3) | 0.026 (2) | −0.002 (3) | −0.0020 (19) | 0.003 (3) |
C13 | 0.036 (4) | 0.058 (4) | 0.036 (3) | 0.009 (3) | −0.008 (3) | −0.004 (3) |
C14 | 0.052 (4) | 0.049 (4) | 0.030 (3) | 0.006 (3) | −0.002 (3) | −0.001 (3) |
C15 | 0.034 (3) | 0.038 (3) | 0.036 (3) | 0.005 (2) | 0.006 (2) | 0.010 (2) |
C16 | 0.029 (4) | 0.081 (5) | 0.041 (3) | 0.007 (3) | −0.007 (3) | 0.008 (3) |
C17 | 0.060 (5) | 0.047 (4) | 0.059 (4) | 0.013 (3) | 0.023 (3) | 0.024 (3) |
O1W | 0.098 (6) | 0.081 (5) | 0.106 (5) | −0.029 (4) | 0.041 (4) | −0.024 (4) |
Co1—N5 | 1.903 (5) | C6—C7 | 1.400 (8) |
Co1—N2 | 1.905 (4) | C6—H6A | 0.9500 |
Co1—N4 | 1.945 (5) | C7—C8 | 1.384 (8) |
Co1—N1 | 1.946 (4) | C7—H7A | 0.9500 |
Co1—N6 | 1.960 (4) | C8—C9 | 1.457 (8) |
Co1—N3 | 1.973 (4) | C10—C11 | 1.553 (8) |
O1—C3 | 1.325 (6) | C10—H10A | 0.9900 |
O1—C2 | 1.487 (7) | C10—H10B | 0.9900 |
O2—C9 | 1.326 (6) | C11—C15 | 1.531 (7) |
O2—C10 | 1.486 (7) | C11—H11A | 1.0000 |
O3—N6 | 1.236 (6) | C12—C14 | 1.506 (8) |
O4—N6 | 1.228 (6) | C12—C13 | 1.532 (8) |
O5—N5 | 1.225 (6) | C12—H12A | 1.0000 |
O6—N5 | 1.256 (6) | C13—H13A | 0.9800 |
O7—N4 | 1.214 (6) | C13—H13B | 0.9800 |
O8—N4 | 1.240 (6) | C13—H13C | 0.9800 |
N1—C3 | 1.293 (7) | C14—H14A | 0.9800 |
N1—C1 | 1.485 (6) | C14—H14B | 0.9800 |
N2—C4 | 1.333 (6) | C14—H14C | 0.9800 |
N2—C8 | 1.347 (6) | C15—C16 | 1.509 (9) |
N3—C9 | 1.290 (7) | C15—C17 | 1.531 (9) |
N3—C11 | 1.486 (7) | C15—H15A | 1.0000 |
C1—C2 | 1.530 (8) | C16—H16A | 0.9800 |
C1—C12 | 1.544 (7) | C16—H16B | 0.9800 |
C1—H1A | 1.0000 | C16—H16C | 0.9800 |
C2—H2A | 0.9900 | C17—H17A | 0.9800 |
C2—H2B | 0.9900 | C17—H17B | 0.9800 |
C3—C4 | 1.462 (7) | C17—H17C | 0.9800 |
C4—C5 | 1.392 (7) | O1W—H1W | 0.8400 |
C5—C6 | 1.375 (8) | O1W—H2W | 0.8400 |
C5—H5A | 0.9500 | ||
N5—Co1—N2 | 179.0 (2) | C8—C7—C6 | 117.9 (5) |
N5—Co1—N4 | 90.5 (2) | C8—C7—H7A | 121.0 |
N2—Co1—N4 | 90.5 (2) | C6—C7—H7A | 121.0 |
N5—Co1—N1 | 99.03 (18) | N2—C8—C7 | 120.5 (5) |
N2—Co1—N1 | 80.86 (18) | N2—C8—C9 | 108.2 (5) |
N4—Co1—N1 | 90.71 (19) | C7—C8—C9 | 131.3 (5) |
N5—Co1—N6 | 90.45 (19) | N3—C9—O2 | 118.9 (5) |
N2—Co1—N6 | 88.55 (19) | N3—C9—C8 | 119.1 (5) |
N4—Co1—N6 | 178.8 (2) | O2—C9—C8 | 122.0 (5) |
N1—Co1—N6 | 89.92 (18) | O2—C10—C11 | 105.2 (4) |
N5—Co1—N3 | 99.43 (19) | O2—C10—H10A | 110.7 |
N2—Co1—N3 | 80.69 (18) | C11—C10—H10A | 110.7 |
N4—Co1—N3 | 88.70 (17) | O2—C10—H10B | 110.7 |
N1—Co1—N3 | 161.53 (18) | C11—C10—H10B | 110.7 |
N6—Co1—N3 | 90.37 (16) | H10A—C10—H10B | 108.8 |
C3—O1—C2 | 104.3 (4) | N3—C11—C15 | 113.1 (4) |
C9—O2—C10 | 104.4 (4) | N3—C11—C10 | 101.2 (4) |
C3—N1—C1 | 107.6 (4) | C15—C11—C10 | 114.4 (4) |
C3—N1—Co1 | 113.3 (3) | N3—C11—H11A | 109.3 |
C1—N1—Co1 | 139.1 (4) | C15—C11—H11A | 109.3 |
C4—N2—C8 | 121.7 (5) | C10—C11—H11A | 109.3 |
C4—N2—Co1 | 119.1 (3) | C14—C12—C13 | 112.0 (4) |
C8—N2—Co1 | 119.1 (4) | C14—C12—C1 | 109.9 (5) |
C9—N3—C11 | 108.4 (4) | C13—C12—C1 | 112.7 (5) |
C9—N3—Co1 | 112.7 (4) | C14—C12—H12A | 107.3 |
C11—N3—Co1 | 138.7 (3) | C13—C12—H12A | 107.3 |
O7—N4—O8 | 118.9 (5) | C1—C12—H12A | 107.3 |
O7—N4—Co1 | 122.3 (4) | C12—C13—H13A | 109.5 |
O8—N4—Co1 | 118.7 (4) | C12—C13—H13B | 109.5 |
O5—N5—O6 | 119.2 (5) | H13A—C13—H13B | 109.5 |
O5—N5—Co1 | 121.3 (4) | C12—C13—H13C | 109.5 |
O6—N5—Co1 | 119.5 (4) | H13A—C13—H13C | 109.5 |
O4—N6—O3 | 118.7 (4) | H13B—C13—H13C | 109.5 |
O4—N6—Co1 | 119.3 (4) | C12—C14—H14A | 109.5 |
O3—N6—Co1 | 121.9 (4) | C12—C14—H14B | 109.5 |
N1—C1—C2 | 101.8 (4) | H14A—C14—H14B | 109.5 |
N1—C1—C12 | 111.4 (4) | C12—C14—H14C | 109.5 |
C2—C1—C12 | 115.1 (4) | H14A—C14—H14C | 109.5 |
N1—C1—H1A | 109.4 | H14B—C14—H14C | 109.5 |
C2—C1—H1A | 109.4 | C16—C15—C11 | 113.6 (5) |
C12—C1—H1A | 109.4 | C16—C15—C17 | 112.0 (5) |
O1—C2—C1 | 104.8 (4) | C11—C15—C17 | 109.1 (5) |
O1—C2—H2A | 110.8 | C16—C15—H15A | 107.3 |
C1—C2—H2A | 110.8 | C11—C15—H15A | 107.3 |
O1—C2—H2B | 110.8 | C17—C15—H15A | 107.3 |
C1—C2—H2B | 110.8 | C15—C16—H16A | 109.5 |
H2A—C2—H2B | 108.9 | C15—C16—H16B | 109.5 |
N1—C3—O1 | 118.7 (5) | H16A—C16—H16B | 109.5 |
N1—C3—C4 | 118.5 (5) | C15—C16—H16C | 109.5 |
O1—C3—C4 | 122.8 (5) | H16A—C16—H16C | 109.5 |
N2—C4—C5 | 120.7 (5) | H16B—C16—H16C | 109.5 |
N2—C4—C3 | 108.1 (4) | C15—C17—H17A | 109.5 |
C5—C4—C3 | 131.2 (5) | C15—C17—H17B | 109.5 |
C6—C5—C4 | 118.3 (5) | H17A—C17—H17B | 109.5 |
C6—C5—H5A | 120.9 | C15—C17—H17C | 109.5 |
C4—C5—H5A | 120.9 | H17A—C17—H17C | 109.5 |
C5—C6—C7 | 120.8 (5) | H17B—C17—H17C | 109.5 |
C5—C6—H6A | 119.6 | H1W—O1W—H2W | 107 |
C7—C6—H6A | 119.6 |
D—H···A | D—H | H···A | D···A | D—H···A |
O1W—H2W···O6 | 0.84 | 2.14 | 2.962 (8) | 165 |
O1W—H1W···O3i | 0.84 | 2.57 | 3.326 (10) | 150 |
Symmetry code: (i) −x+1, y+1/2, −z+3/2. |
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