Supporting information
Crystallographic Information File (CIF) https://doi.org/10.1107/S2053229621011347/op3014sup1.cif | |
Structure factor file (CIF format) https://doi.org/10.1107/S2053229621011347/op3014Isup2.hkl | |
Portable Document Format (PDF) file https://doi.org/10.1107/S2053229621011347/op3014sup3.pdf |
CCDC reference: 2051249
Data collection: APEX3 (Bruker, 2018); cell refinement: SAINT (Bruker, 2017); data reduction: SAINT (Bruker 2017); program(s) used to solve structure: SHELXS2017 (Sheldrick, 2008); program(s) used to refine structure: SHELXL2017 (Sheldrick, 2015); molecular graphics: X-SEED (Barbour, 2020); software used to prepare material for publication: SHELXL2017 (Sheldrick, 2015).
[Co(C3H6NO3)2] | F(000) = 274 |
Mr = 267.11 | Dx = 1.891 Mg m−3 |
Monoclinic, P21 | Mo Kα radiation, λ = 0.71073 Å |
a = 5.5666 (4) Å | Cell parameters from 11159 reflections |
b = 8.7105 (6) Å | θ = 2.1–28.4° |
c = 9.8314 (7) Å | µ = 1.84 mm−1 |
β = 100.311 (1)° | T = 173 K |
V = 469.01 (6) Å3 | Block, red purple |
Z = 2 | 0.24 × 0.24 × 0.22 mm |
Bruker Kappa DUO APEXII diffractometer | 2293 reflections with I > 2σ(I) |
Radiation source: fine-focus sealed tube | Rint = 0.034 |
1.2°φ scans and ω scans | θmax = 28.4°, θmin = 2.1° |
Absorption correction: multi-scan (SADABS; Krause et al., 2015) | h = −7→7 |
k = −11→11 | |
11159 measured reflections | l = −13→13 |
2353 independent reflections |
Refinement on F2 | Hydrogen site location: mixed |
Least-squares matrix: full | H atoms treated by a mixture of independent and constrained refinement |
R[F2 > 2σ(F2)] = 0.021 | w = 1/[σ2(Fo2) + (0.0277P)2] where P = (Fo2 + 2Fc2)/3 |
wR(F2) = 0.048 | (Δ/σ)max < 0.001 |
S = 1.03 | Δρmax = 0.23 e Å−3 |
2353 reflections | Δρmin = −0.20 e Å−3 |
140 parameters | Absolute structure: Flack x determined using 1028 quotients [(I+)-(I-)]/[(I+)+(I-)] (Parsons et al., 2013) |
1 restraint | Absolute structure parameter: −0.001 (11) |
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. For single-crystal structure refinement, data collections were performed on a Bruker KAPPA APEXII Duo diffractometer using Mo <i.Kα (λ = 0.71069 Å). Unit-cell refinement and data reduction were performed using the program SAINT (Bruker, 2017). Data were corrected for Lorentz polarisation effects and for absorption using the program SADABS (Krause et al., 2015). The structure was solved by direct methods and refined by full-matrix least squares on F2 in the SHELX (Sheldrick, 2008) suite of programs within the X-SEED (Barbour, 2020) interface. All non-H atoms were refined with anisotropic displacement parameters |
x | y | z | Uiso*/Ueq | ||
Co1 | 0.48448 (5) | 0.83382 (4) | 0.19408 (3) | 0.01158 (9) | |
O1B | 0.2501 (3) | 0.9135 (2) | 0.32539 (18) | 0.0174 (4) | |
N1A | 0.2297 (4) | 0.6561 (2) | 0.1290 (2) | 0.0128 (4) | |
H1A1 | 0.215527 | 0.595708 | 0.202630 | 0.015* | |
H1A2 | 0.080814 | 0.698107 | 0.096482 | 0.015* | |
O2A | 0.6827 (3) | 0.4777 (2) | −0.03844 (19) | 0.0173 (4) | |
O2B | 0.1688 (4) | 0.9107 (3) | 0.5386 (2) | 0.0252 (4) | |
C2B | 0.5014 (5) | 0.7575 (3) | 0.4964 (3) | 0.0164 (5) | |
H2B | 0.425786 | 0.654164 | 0.502740 | 0.020* | |
C1B | 0.2929 (5) | 0.8712 (3) | 0.4518 (3) | 0.0155 (5) | |
C2A | 0.3049 (4) | 0.5612 (3) | 0.0202 (3) | 0.0128 (5) | |
H2A | 0.261472 | 0.451547 | 0.033510 | 0.015* | |
O3B | 0.7553 (4) | 0.9428 (2) | 0.6409 (2) | 0.0254 (5) | |
H3B | 0.880303 | 0.937581 | 0.604197 | 0.030* | |
N1B | 0.6587 (4) | 0.7465 (3) | 0.3906 (2) | 0.0162 (5) | |
H1B1 | 0.699717 | 0.646471 | 0.380866 | 0.019* | |
H1B2 | 0.798857 | 0.799991 | 0.419787 | 0.019* | |
C3B | 0.6445 (5) | 0.7949 (3) | 0.6386 (3) | 0.0214 (6) | |
H3B1 | 0.533739 | 0.792153 | 0.706907 | 0.026* | |
H3B2 | 0.772685 | 0.716300 | 0.665458 | 0.026* | |
O1A | 0.6898 (3) | 0.6873 (2) | 0.09082 (19) | 0.0168 (4) | |
C1A | 0.5799 (5) | 0.5750 (3) | 0.0258 (3) | 0.0122 (5) | |
O3A | 0.2204 (4) | 0.5083 (2) | −0.22685 (19) | 0.0166 (4) | |
H3A2 | 0.099 (7) | 0.477 (4) | −0.251 (3) | 0.020* | |
C3A | 0.1783 (5) | 0.6157 (3) | −0.1223 (3) | 0.0150 (5) | |
H1 | 0.000691 | 0.625528 | −0.123775 | 0.018* | |
H2 | 0.242032 | 0.717924 | −0.141951 | 0.018* |
U11 | U22 | U33 | U12 | U13 | U23 | |
Co1 | 0.01072 (14) | 0.01198 (13) | 0.01185 (15) | 0.00105 (14) | 0.00152 (10) | 0.00012 (15) |
O1B | 0.0164 (9) | 0.0197 (9) | 0.0156 (9) | 0.0055 (7) | 0.0016 (7) | −0.0012 (7) |
N1A | 0.0112 (10) | 0.0148 (9) | 0.0128 (11) | 0.0003 (8) | 0.0031 (8) | 0.0003 (8) |
O2A | 0.0114 (8) | 0.0196 (9) | 0.0204 (9) | 0.0009 (7) | 0.0018 (7) | −0.0081 (8) |
O2B | 0.0215 (10) | 0.0339 (11) | 0.0222 (10) | 0.0010 (9) | 0.0097 (8) | −0.0048 (9) |
C2B | 0.0192 (12) | 0.0157 (12) | 0.0152 (12) | −0.0013 (10) | 0.0048 (10) | 0.0001 (10) |
C1B | 0.0150 (11) | 0.0150 (13) | 0.0167 (12) | −0.0023 (8) | 0.0032 (9) | −0.0031 (9) |
C2A | 0.0103 (11) | 0.0147 (11) | 0.0133 (12) | 0.0006 (9) | 0.0022 (9) | −0.0001 (9) |
O3B | 0.0195 (10) | 0.0284 (11) | 0.0287 (11) | −0.0030 (8) | 0.0057 (9) | −0.0141 (9) |
N1B | 0.0175 (10) | 0.0173 (11) | 0.0137 (11) | 0.0037 (9) | 0.0024 (8) | −0.0008 (8) |
C3B | 0.0247 (14) | 0.0257 (16) | 0.0132 (13) | 0.0015 (10) | 0.0016 (10) | 0.0016 (10) |
O1A | 0.0100 (8) | 0.0183 (8) | 0.0220 (10) | −0.0009 (7) | 0.0020 (7) | −0.0074 (7) |
C1A | 0.0103 (11) | 0.0148 (11) | 0.0113 (12) | 0.0016 (9) | 0.0015 (9) | 0.0004 (9) |
O3A | 0.0133 (9) | 0.0198 (9) | 0.0160 (9) | 0.0003 (8) | 0.0006 (7) | −0.0048 (7) |
C3A | 0.0133 (12) | 0.0163 (12) | 0.0148 (13) | 0.0023 (9) | 0.0008 (10) | −0.0013 (10) |
Co1—O1A | 2.0930 (19) | O2B—C1B | 1.239 (3) |
Co1—O1B | 2.1102 (19) | C2B—N1B | 1.478 (4) |
Co1—O2Ai | 2.0658 (18) | C2B—C3B | 1.515 (4) |
Co1—O3Ai | 2.2183 (19) | C2B—C1B | 1.530 (4) |
Co1—N1A | 2.119 (2) | C2A—C3A | 1.527 (3) |
Co1—N1B | 2.140 (2) | C2A—C1A | 1.527 (4) |
O1B—C1B | 1.277 (3) | O3B—C3B | 1.427 (3) |
N1A—C2A | 1.470 (3) | O1A—C1A | 1.265 (3) |
O2A—C1A | 1.255 (3) | O3A—C3A | 1.440 (3) |
O1A—Co1—N1A | 78.60 (8) | N1B—C2B—C3B | 112.5 (2) |
O1B—Co1—N1B | 78.14 (8) | N1B—C2B—C1B | 110.8 (2) |
O2Ai—Co1—O3Ai | 85.17 (7) | C3B—C2B—C1B | 111.8 (2) |
O1A—Co1—O1B | 161.50 (7) | O2B—C1B—O1B | 124.1 (2) |
N1A—Co1—O3Ai | 169.15 (8) | O2B—C1B—C2B | 118.0 (2) |
O2Ai—Co1—N1B | 162.83 (8) | O1B—C1B—C2B | 117.8 (2) |
O2Ai—Co1—O1A | 102.90 (7) | N1A—C2A—C3A | 110.4 (2) |
O2Ai—Co1—O1B | 90.45 (7) | N1A—C2A—C1A | 110.1 (2) |
O2Ai—Co1—N1A | 91.77 (8) | C3A—C2A—C1A | 107.7 (2) |
O1B—Co1—N1A | 88.37 (8) | C2B—N1B—Co1 | 112.50 (16) |
O1A—Co1—N1B | 91.29 (8) | O3B—C3B—C2B | 111.3 (2) |
N1A—Co1—N1B | 100.58 (8) | C1A—O1A—Co1 | 117.37 (17) |
O1A—Co1—O3Ai | 91.92 (7) | O2A—C1A—O1A | 123.7 (2) |
O1B—Co1—O3Ai | 102.04 (7) | O2A—C1A—C2A | 118.2 (2) |
N1B—Co1—O3Ai | 84.73 (8) | O1A—C1A—C2A | 118.1 (2) |
C1B—O1B—Co1 | 118.21 (16) | C3A—O3A—Co1ii | 123.54 (15) |
C2A—N1A—Co1 | 111.59 (15) | O3A—C3A—C2A | 110.21 (19) |
C1A—O2A—Co1ii | 126.67 (16) |
Symmetry codes: (i) −x+1, y+1/2, −z; (ii) −x+1, y−1/2, −z. |