Supporting information
Crystallographic Information File (CIF) https://doi.org/10.1107/S1600536807052191/ci2489sup1.cif | |
Structure factor file (CIF format) https://doi.org/10.1107/S1600536807052191/ci2489Isup2.hkl |
CCDC reference: 667244
Key indicators
- Single-crystal X-ray study
- T = 295 K
- Mean (C-C) = 0.004 Å
- R factor = 0.034
- wR factor = 0.086
- Data-to-parameter ratio = 15.8
checkCIF/PLATON results
No syntax errors found
Alert level C ABSTM02_ALERT_3_C The ratio of expected to reported Tmax/Tmin(RR') is < 0.90 Tmin and Tmax reported: 0.546 0.854 Tmin(prime) and Tmax expected: 0.690 0.850 RR(prime) = 0.787 Please check that your absorption correction is appropriate. STRVA01_ALERT_4_C Flack test results are ambiguous. From the CIF: _refine_ls_abs_structure_Flack 0.470 From the CIF: _refine_ls_abs_structure_Flack_su 0.020 PLAT033_ALERT_2_C Flack Parameter Value Deviates 2 * su from zero. 0.47 PLAT061_ALERT_3_C Tmax/Tmin Range Test RR' too Large ............. 0.78 PLAT222_ALERT_3_C Large Non-Solvent H Ueq(max)/Ueq(min) ... 3.49 Ratio PLAT242_ALERT_2_C Check Low Ueq as Compared to Neighbors for C1 PLAT415_ALERT_2_C Short Inter D-H..H-X H1W1 .. H8 .. 2.12 Ang. PLAT720_ALERT_4_C Number of Unusual/Non-Standard Label(s) ........ 2 PLAT731_ALERT_1_C Bond Calc 0.86(4), Rep 0.850(10) ...... 4.00 su-Ra O1W -H1W1 1.555 1.555 PLAT735_ALERT_1_C D-H Calc 0.86(4), Rep 0.850(10) ...... 4.00 su-Ra O1W -H1# 1.555 1.555
Alert level G REFLT03_ALERT_4_G 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. From the CIF: _diffrn_reflns_theta_max 27.45 From the CIF: _reflns_number_total 4282 Count of symmetry unique reflns 2468 Completeness (_total/calc) 173.50% TEST3: Check Friedels for noncentro structure Estimate of Friedel pairs measured 1814 Fraction of Friedel pairs measured 0.735 Are heavy atom types Z>Si present yes PLAT794_ALERT_5_G Check Predicted Bond Valency for Co1 (9) 1.36 PLAT860_ALERT_3_G Note: Number of Least-Squares Restraints ....... 2
0 ALERT level A = In general: serious problem 0 ALERT level B = Potentially serious problem 10 ALERT level C = Check and explain 3 ALERT level G = General alerts; check 2 ALERT type 1 CIF construction/syntax error, inconsistent or missing data 3 ALERT type 2 Indicator that the structure model may be wrong or deficient 4 ALERT type 3 Indicator that the structure quality may be low 3 ALERT type 4 Improvement, methodology, query or suggestion 1 ALERT type 5 Informative message, check
checkCIF publication errors
Alert level G PUBL013_ALERT_1_G The _publ_section_comment (discussion of study) is missing. This is required for a full paper submission (but is optional for an electronic paper).
0 ALERT level A = Data missing that is essential or data in wrong format 1 ALERT level G = General alerts. Data that may be required is missing
Cobalt dichloride hexahydrate (2 mmol), 3-(4-carboxylatophenoxy)propionic acid (2 mmol) and 2,2'-bipyridine (2 mmol) were dissolved in a 3:1 ethanol–water solution. Aqueous 0.1 M sodium hydroxide was added until the solution registered a pH of 7. The solution was set aside for the growth of crystals over several days. CH&N analysis. Calc. for C20H18N2O6Co: C 54.43, H 4.11, N 6.35%. Found: C 54.45, H 4.10, N 6.36%.
The carbon-bound H atoms were placed in calculated positions [C—H = 0.93–0.97 Å and Uiso(H) = 1.2–1.5Ueq(C)], and were included in the refinement in the riding-model approximation. The water H-atoms were located in a difference Fourier map, and were refined with a distance restraint of O—H = 0.85 (1) Å; their Uiso(H) values were freely refined.
Data collection: RAPID-AUTO (Rigaku, 1998); cell refinement: RAPID-AUTO (Rigaku, 1998); data reduction: CrystalStructure (Rigaku/MSC, 2002); program(s) used to solve structure: SHELXS97 (Sheldrick, 1997); program(s) used to refine structure: SHELXL97 (Sheldrick, 1997); molecular graphics: X-SEED (Barbour, 2001); software used to prepare material for publication: publCIF (Westrip, 2007).
[Co(C10H8O5)(C10H8N2)(H2O)] | F(000) = 908 |
Mr = 441.29 | Dx = 1.565 Mg m−3 |
Orthorhombic, P212121 | Mo Kα radiation, λ = 0.71073 Å |
Hall symbol: P 2ac 2ab | Cell parameters from 14469 reflections |
a = 6.7193 (2) Å | θ = 3.0–27.5° |
b = 16.1369 (5) Å | µ = 0.96 mm−1 |
c = 17.2762 (7) Å | T = 295 K |
V = 1873.2 (1) Å3 | Block, pink |
Z = 4 | 0.38 × 0.25 × 0.17 mm |
Rigaku R-AXIS RAPID diffractometer | 4282 independent reflections |
Radiation source: fine-focus sealed tube | 3233 reflections with I > 2σ(I) |
Graphite monochromator | Rint = 0.041 |
Detector resolution: 10.000 pixels mm-1 | θmax = 27.5°, θmin = 3.3° |
ω scans | h = −8→8 |
Absorption correction: multi-scan (ABSCOR; Higashi, 1995) | k = −20→20 |
Tmin = 0.546, Tmax = 0.854 | l = −22→22 |
18344 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)] = 0.034 | H atoms treated by a mixture of independent and constrained refinement |
wR(F2) = 0.087 | w = 1/[σ2(Fo2) + (0.0503P)2] where P = (Fo2 + 2Fc2)/3 |
S = 1.00 | (Δ/σ)max = 0.001 |
4282 reflections | Δρmax = 0.33 e Å−3 |
271 parameters | Δρmin = −0.35 e Å−3 |
2 restraints | Absolute structure: Flack (1983), with 1820 Friedel pairs |
Primary atom site location: structure-invariant direct methods | Absolute structure parameter: 0.47 (2) |
[Co(C10H8O5)(C10H8N2)(H2O)] | V = 1873.2 (1) Å3 |
Mr = 441.29 | Z = 4 |
Orthorhombic, P212121 | Mo Kα radiation |
a = 6.7193 (2) Å | µ = 0.96 mm−1 |
b = 16.1369 (5) Å | T = 295 K |
c = 17.2762 (7) Å | 0.38 × 0.25 × 0.17 mm |
Rigaku R-AXIS RAPID diffractometer | 4282 independent reflections |
Absorption correction: multi-scan (ABSCOR; Higashi, 1995) | 3233 reflections with I > 2σ(I) |
Tmin = 0.546, Tmax = 0.854 | Rint = 0.041 |
18344 measured reflections |
R[F2 > 2σ(F2)] = 0.034 | H atoms treated by a mixture of independent and constrained refinement |
wR(F2) = 0.087 | Δρmax = 0.33 e Å−3 |
S = 1.00 | Δρmin = −0.35 e Å−3 |
4282 reflections | Absolute structure: Flack (1983), with 1820 Friedel pairs |
271 parameters | Absolute structure parameter: 0.47 (2) |
2 restraints |
x | y | z | Uiso*/Ueq | ||
Co1 | 0.76489 (5) | 0.398602 (19) | 0.855061 (19) | 0.03280 (11) | |
O1 | 0.8432 (3) | 0.51878 (12) | 0.86177 (15) | 0.0497 (5) | |
O2 | 0.5641 (3) | 0.58949 (13) | 0.84844 (18) | 0.0748 (8) | |
O3 | 0.9850 (3) | 0.64927 (14) | 0.98563 (12) | 0.0493 (6) | |
O4 | 1.4181 (3) | 0.62191 (12) | 1.31063 (11) | 0.0381 (5) | |
O5 | 1.6780 (3) | 0.60698 (13) | 1.23548 (11) | 0.0392 (4) | |
O1W | 0.4572 (3) | 0.43293 (15) | 0.86584 (15) | 0.0471 (5) | |
H1W1 | 0.351 (5) | 0.421 (3) | 0.841 (3) | 0.13 (2)* | |
H1W2 | 0.472 (10) | 0.4855 (10) | 0.858 (3) | 0.15 (2)* | |
N1 | 0.7355 (3) | 0.26736 (12) | 0.86476 (13) | 0.0380 (5) | |
N2 | 0.7761 (3) | 0.37846 (13) | 0.97567 (12) | 0.0372 (5) | |
C1 | 0.7464 (5) | 0.58424 (15) | 0.85589 (15) | 0.0405 (6) | |
C2 | 0.8697 (5) | 0.66325 (17) | 0.85777 (19) | 0.0478 (7) | |
H2A | 0.7878 | 0.7080 | 0.8774 | 0.057* | |
H2B | 0.9084 | 0.6774 | 0.8053 | 0.057* | |
C3 | 1.0561 (5) | 0.65662 (19) | 0.90742 (18) | 0.0468 (8) | |
H3A | 1.1336 | 0.6083 | 0.8930 | 0.056* | |
H3B | 1.1384 | 0.7056 | 0.9016 | 0.056* | |
C4 | 1.1199 (4) | 0.63966 (18) | 1.04414 (19) | 0.0400 (8) | |
C5 | 1.3226 (4) | 0.62954 (18) | 1.03432 (18) | 0.0382 (7) | |
H5 | 1.3781 | 0.6289 | 0.9850 | 0.046* | |
C6 | 1.4423 (4) | 0.62027 (17) | 1.09954 (18) | 0.0358 (7) | |
H6 | 1.5785 | 0.6128 | 1.0932 | 0.043* | |
C7 | 1.3635 (4) | 0.62183 (18) | 1.17393 (17) | 0.0325 (6) | |
C8 | 1.1589 (4) | 0.6321 (2) | 1.18138 (19) | 0.0407 (8) | |
H8 | 1.1024 | 0.6334 | 1.2305 | 0.049* | |
C9 | 1.0378 (5) | 0.6405 (2) | 1.11728 (19) | 0.0464 (8) | |
H9 | 0.9011 | 0.6466 | 1.1234 | 0.056* | |
C10 | 1.4924 (4) | 0.61640 (16) | 1.24370 (16) | 0.0315 (6) | |
C11 | 0.7263 (5) | 0.21451 (17) | 0.80494 (18) | 0.0465 (7) | |
H11 | 0.7152 | 0.2359 | 0.7551 | 0.056* | |
C12 | 0.7325 (6) | 0.12974 (18) | 0.8145 (2) | 0.0577 (9) | |
H12 | 0.7225 | 0.0946 | 0.7720 | 0.069* | |
C13 | 0.7535 (5) | 0.09824 (18) | 0.8873 (2) | 0.0597 (8) | |
H13 | 0.7629 | 0.0413 | 0.8949 | 0.072* | |
C14 | 0.7608 (5) | 0.15235 (17) | 0.9502 (2) | 0.0512 (8) | |
H14 | 0.7712 | 0.1320 | 1.0004 | 0.061* | |
C15 | 0.7525 (4) | 0.23639 (15) | 0.93690 (16) | 0.0372 (6) | |
C16 | 0.7603 (4) | 0.29919 (16) | 0.99980 (15) | 0.0362 (6) | |
C17 | 0.7481 (5) | 0.2795 (2) | 1.07764 (16) | 0.0496 (7) | |
H17 | 0.7364 | 0.2246 | 1.0935 | 0.059* | |
C18 | 0.7535 (5) | 0.3428 (2) | 1.13136 (17) | 0.0583 (8) | |
H18 | 0.7468 | 0.3308 | 1.1839 | 0.070* | |
C19 | 0.7688 (5) | 0.4237 (2) | 1.10691 (18) | 0.0569 (8) | |
H19 | 0.7711 | 0.4669 | 1.1426 | 0.068* | |
C20 | 0.7804 (5) | 0.43962 (19) | 1.02912 (17) | 0.0471 (7) | |
H20 | 0.7917 | 0.4943 | 1.0126 | 0.056* |
U11 | U22 | U33 | U12 | U13 | U23 | |
Co1 | 0.03360 (18) | 0.03556 (17) | 0.02925 (18) | −0.00088 (17) | 0.00086 (18) | 0.00136 (15) |
O1 | 0.0485 (12) | 0.0362 (10) | 0.0644 (15) | −0.0022 (9) | 0.0008 (12) | −0.0018 (11) |
O2 | 0.0542 (14) | 0.0514 (14) | 0.119 (3) | 0.0054 (11) | −0.0266 (16) | −0.0056 (16) |
O3 | 0.0396 (12) | 0.0774 (15) | 0.0309 (12) | −0.0002 (10) | −0.0106 (9) | −0.0001 (10) |
O4 | 0.0337 (10) | 0.0499 (11) | 0.0308 (11) | 0.0015 (9) | 0.0002 (8) | −0.0032 (9) |
O5 | 0.0267 (9) | 0.0581 (11) | 0.0328 (10) | 0.0010 (9) | −0.0034 (7) | −0.0006 (10) |
O1W | 0.0331 (11) | 0.0588 (13) | 0.0495 (14) | 0.0017 (10) | −0.0034 (11) | −0.0037 (11) |
N1 | 0.0351 (12) | 0.0369 (10) | 0.0420 (13) | −0.0033 (11) | 0.0067 (14) | 0.0017 (9) |
N2 | 0.0335 (13) | 0.0472 (12) | 0.0310 (12) | 0.0040 (12) | −0.0005 (11) | 0.0013 (9) |
C1 | 0.0499 (16) | 0.0399 (13) | 0.0317 (13) | 0.0009 (14) | −0.0089 (19) | −0.0005 (11) |
C2 | 0.063 (2) | 0.0423 (15) | 0.0385 (17) | −0.0063 (14) | −0.0131 (18) | 0.0071 (15) |
C3 | 0.0505 (18) | 0.0504 (17) | 0.0396 (18) | −0.0072 (15) | −0.0044 (15) | 0.0055 (14) |
C4 | 0.0359 (16) | 0.0460 (18) | 0.0380 (19) | −0.0072 (13) | −0.0068 (14) | 0.0012 (14) |
C5 | 0.0383 (16) | 0.0469 (17) | 0.0295 (16) | 0.0001 (12) | 0.0008 (12) | −0.0038 (13) |
C6 | 0.0270 (14) | 0.0418 (16) | 0.0385 (17) | 0.0002 (12) | 0.0006 (12) | −0.0029 (13) |
C7 | 0.0291 (13) | 0.0356 (15) | 0.0328 (16) | −0.0032 (11) | −0.0033 (12) | −0.0006 (12) |
C8 | 0.0317 (15) | 0.060 (2) | 0.0301 (17) | −0.0012 (13) | 0.0019 (12) | 0.0024 (14) |
C9 | 0.0300 (15) | 0.070 (2) | 0.0388 (19) | −0.0044 (14) | 0.0002 (14) | 0.0043 (15) |
C10 | 0.0296 (14) | 0.0310 (13) | 0.0338 (15) | −0.0004 (11) | −0.0019 (11) | −0.0017 (11) |
C11 | 0.0461 (18) | 0.0483 (15) | 0.0451 (17) | −0.0067 (15) | 0.0103 (17) | −0.0053 (13) |
C12 | 0.052 (2) | 0.0440 (15) | 0.077 (2) | −0.0061 (17) | 0.009 (2) | −0.0126 (16) |
C13 | 0.0485 (17) | 0.0352 (14) | 0.095 (3) | −0.002 (2) | 0.005 (2) | −0.0002 (16) |
C14 | 0.0350 (16) | 0.0498 (16) | 0.069 (2) | −0.0011 (17) | −0.004 (2) | 0.0180 (14) |
C15 | 0.0249 (12) | 0.0419 (13) | 0.0448 (15) | 0.0003 (14) | 0.0014 (16) | 0.0085 (11) |
C16 | 0.0224 (12) | 0.0503 (14) | 0.0358 (14) | 0.0015 (14) | 0.0008 (14) | 0.0079 (11) |
C17 | 0.0361 (15) | 0.0694 (17) | 0.0432 (17) | 0.0053 (18) | 0.0027 (18) | 0.0180 (14) |
C18 | 0.0426 (17) | 0.102 (3) | 0.0300 (16) | 0.007 (2) | 0.0007 (19) | 0.0098 (15) |
C19 | 0.0479 (19) | 0.085 (2) | 0.0381 (17) | 0.0034 (19) | 0.0011 (18) | −0.0131 (16) |
C20 | 0.0482 (19) | 0.0572 (16) | 0.0358 (16) | 0.0035 (16) | −0.0003 (15) | −0.0056 (13) |
Co1—O1 | 2.013 (2) | C5—C6 | 1.392 (4) |
Co1—O5i | 2.103 (2) | C5—H5 | 0.93 |
Co1—N2 | 2.110 (2) | C6—C7 | 1.390 (4) |
Co1—N1 | 2.134 (2) | C6—H6 | 0.93 |
Co1—O1W | 2.148 (2) | C7—C8 | 1.391 (4) |
Co1—O4i | 2.289 (2) | C7—C10 | 1.487 (4) |
O1—C1 | 1.245 (3) | C8—C9 | 1.380 (4) |
O2—C1 | 1.234 (4) | C8—H8 | 0.93 |
O3—C4 | 1.367 (4) | C9—H9 | 0.93 |
O3—C3 | 1.438 (4) | C11—C12 | 1.379 (4) |
O4—C10 | 1.263 (3) | C11—H11 | 0.93 |
O5—C10 | 1.265 (3) | C12—C13 | 1.364 (5) |
O1W—H1W1 | 0.85 (1) | C12—H12 | 0.93 |
O1W—H1W2 | 0.86 (1) | C13—C14 | 1.395 (5) |
N1—C11 | 1.341 (3) | C13—H13 | 0.93 |
N1—C15 | 1.348 (3) | C14—C15 | 1.377 (4) |
N2—C16 | 1.350 (3) | C14—H14 | 0.93 |
N2—C20 | 1.352 (4) | C15—C16 | 1.487 (4) |
C1—C2 | 1.521 (4) | C16—C17 | 1.384 (4) |
C2—C3 | 1.522 (4) | C17—C18 | 1.381 (5) |
C2—H2A | 0.97 | C17—H17 | 0.93 |
C2—H2B | 0.97 | C18—C19 | 1.377 (5) |
C3—H3A | 0.97 | C18—H18 | 0.93 |
C3—H3B | 0.97 | C19—C20 | 1.370 (4) |
C4—C5 | 1.382 (4) | C19—H19 | 0.93 |
C4—C9 | 1.379 (4) | C20—H20 | 0.93 |
O1—Co1—O5i | 92.87 (9) | C4—C5—H5 | 120.6 |
O1—Co1—N2 | 94.72 (9) | C6—C5—H5 | 120.6 |
O5i—Co1—N2 | 163.10 (8) | C5—C6—C7 | 121.8 (3) |
O1—Co1—N1 | 167.43 (10) | C5—C6—H6 | 119.1 |
O5i—Co1—N1 | 92.95 (8) | C7—C6—H6 | 119.1 |
N2—Co1—N1 | 76.87 (9) | C6—C7—C8 | 117.7 (3) |
O1—Co1—O1W | 89.89 (9) | C6—C7—C10 | 121.8 (2) |
O5i—Co1—O1W | 105.76 (8) | C8—C7—C10 | 120.5 (3) |
N2—Co1—O1W | 89.35 (9) | C9—C8—C7 | 121.3 (3) |
N1—Co1—O1W | 99.22 (9) | C9—C8—H8 | 119.3 |
O1—Co1—O4i | 85.14 (8) | C7—C8—H8 | 119.3 |
O5i—Co1—O4i | 59.64 (7) | C8—C9—C4 | 119.9 (3) |
N2—Co1—O4i | 106.00 (8) | C8—C9—H9 | 120.0 |
N1—Co1—O4i | 88.21 (8) | C4—C9—H9 | 120.0 |
O1W—Co1—O4i | 164.19 (8) | O4—C10—O5 | 120.1 (3) |
C1—O1—Co1 | 132.6 (2) | O4—C10—C7 | 120.5 (2) |
C4—O3—C3 | 118.9 (2) | O5—C10—C7 | 119.4 (2) |
C10—O4—Co1ii | 85.92 (15) | N1—C11—C12 | 122.5 (3) |
C10—O5—Co1ii | 94.29 (17) | N1—C11—H11 | 118.8 |
Co1—O1W—H1W1 | 134 (4) | C12—C11—H11 | 118.8 |
Co1—O1W—H1W2 | 98 (5) | C13—C12—C11 | 118.9 (3) |
H1W1—O1W—H1W2 | 104 (5) | C13—C12—H12 | 120.5 |
C11—N1—C15 | 118.7 (2) | C11—C12—H12 | 120.5 |
C11—N1—Co1 | 125.10 (19) | C12—C13—C14 | 119.2 (3) |
C15—N1—Co1 | 115.65 (17) | C12—C13—H13 | 120.4 |
C16—N2—C20 | 118.9 (2) | C14—C13—H13 | 120.4 |
C16—N2—Co1 | 116.62 (17) | C15—C14—C13 | 119.0 (3) |
C20—N2—Co1 | 124.24 (19) | C15—C14—H14 | 120.5 |
O2—C1—O1 | 125.8 (3) | C13—C14—H14 | 120.5 |
O2—C1—C2 | 119.0 (2) | N1—C15—C14 | 121.5 (3) |
O1—C1—C2 | 115.1 (3) | N1—C15—C16 | 115.2 (2) |
C1—C2—C3 | 113.7 (2) | C14—C15—C16 | 123.2 (3) |
C1—C2—H2A | 108.8 | N2—C16—C17 | 121.5 (3) |
C3—C2—H2A | 108.8 | N2—C16—C15 | 115.0 (2) |
C1—C2—H2B | 108.8 | C17—C16—C15 | 123.5 (2) |
C3—C2—H2B | 108.8 | C18—C17—C16 | 118.8 (3) |
H2A—C2—H2B | 107.7 | C18—C17—H17 | 120.6 |
O3—C3—C2 | 105.2 (3) | C16—C17—H17 | 120.6 |
O3—C3—H3A | 110.7 | C19—C18—C17 | 119.9 (3) |
C2—C3—H3A | 110.7 | C19—C18—H18 | 120.1 |
O3—C3—H3B | 110.7 | C17—C18—H18 | 120.1 |
C2—C3—H3B | 110.7 | C20—C19—C18 | 118.8 (3) |
H3A—C3—H3B | 108.8 | C20—C19—H19 | 120.6 |
O3—C4—C5 | 125.2 (3) | C18—C19—H19 | 120.6 |
O3—C4—C9 | 114.3 (3) | N2—C20—C19 | 122.2 (3) |
C5—C4—C9 | 120.5 (3) | N2—C20—H20 | 118.9 |
C4—C5—C6 | 118.8 (3) | C19—C20—H20 | 118.9 |
O5i—Co1—O1—C1 | 91.4 (3) | C10—C7—C8—C9 | 177.5 (3) |
N2—Co1—O1—C1 | −103.7 (3) | C7—C8—C9—C4 | −0.8 (5) |
N1—Co1—O1—C1 | −151.1 (4) | O3—C4—C9—C8 | −179.4 (3) |
O1W—Co1—O1—C1 | −14.4 (3) | C5—C4—C9—C8 | 0.8 (5) |
O4i—Co1—O1—C1 | 150.6 (3) | Co1ii—O4—C10—O5 | −2.4 (2) |
O1—Co1—N1—C11 | −127.3 (4) | Co1ii—O4—C10—C7 | 178.3 (2) |
O5i—Co1—N1—C11 | −9.8 (3) | Co1ii—O5—C10—O4 | 2.6 (3) |
N2—Co1—N1—C11 | −176.2 (3) | Co1ii—O5—C10—C7 | −178.0 (2) |
O1W—Co1—N1—C11 | 96.7 (3) | C6—C7—C10—O4 | 176.6 (3) |
O4i—Co1—N1—C11 | −69.3 (3) | C8—C7—C10—O4 | −0.7 (4) |
O1—Co1—N1—C15 | 44.2 (6) | C6—C7—C10—O5 | −2.7 (4) |
O5i—Co1—N1—C15 | 161.7 (2) | C8—C7—C10—O5 | 179.9 (3) |
N2—Co1—N1—C15 | −4.6 (2) | C15—N1—C11—C12 | 0.3 (5) |
O1W—Co1—N1—C15 | −91.8 (2) | Co1—N1—C11—C12 | 171.6 (3) |
O4i—Co1—N1—C15 | 102.2 (2) | N1—C11—C12—C13 | −1.6 (6) |
O1—Co1—N2—C16 | −170.7 (2) | C11—C12—C13—C14 | 2.3 (6) |
O5i—Co1—N2—C16 | −54.3 (4) | C12—C13—C14—C15 | −1.9 (5) |
N1—Co1—N2—C16 | −0.2 (2) | C11—N1—C15—C14 | 0.1 (5) |
O1W—Co1—N2—C16 | 99.5 (2) | Co1—N1—C15—C14 | −172.0 (2) |
O4i—Co1—N2—C16 | −84.4 (2) | C11—N1—C15—C16 | −179.6 (3) |
O1—Co1—N2—C20 | 15.3 (3) | Co1—N1—C15—C16 | 8.3 (3) |
O5i—Co1—N2—C20 | 131.7 (3) | C13—C14—C15—N1 | 0.7 (5) |
N1—Co1—N2—C20 | −174.2 (3) | C13—C14—C15—C16 | −179.7 (3) |
O1W—Co1—N2—C20 | −74.5 (3) | C20—N2—C16—C17 | 0.1 (5) |
O4i—Co1—N2—C20 | 101.6 (3) | Co1—N2—C16—C17 | −174.2 (2) |
Co1—O1—C1—O2 | 4.8 (5) | C20—N2—C16—C15 | 178.8 (3) |
Co1—O1—C1—C2 | −174.7 (2) | Co1—N2—C16—C15 | 4.5 (3) |
O2—C1—C2—C3 | 148.8 (3) | N1—C15—C16—N2 | −8.5 (4) |
O1—C1—C2—C3 | −31.6 (4) | C14—C15—C16—N2 | 171.9 (3) |
C4—O3—C3—C2 | 178.1 (2) | N1—C15—C16—C17 | 170.1 (3) |
C1—C2—C3—O3 | −67.7 (3) | C14—C15—C16—C17 | −9.5 (5) |
C3—O3—C4—C5 | −5.5 (4) | N2—C16—C17—C18 | −0.4 (5) |
C3—O3—C4—C9 | 174.6 (3) | C15—C16—C17—C18 | −178.9 (3) |
O3—C4—C5—C6 | −179.9 (3) | C16—C17—C18—C19 | 0.7 (5) |
C9—C4—C5—C6 | −0.1 (5) | C17—C18—C19—C20 | −0.7 (6) |
C4—C5—C6—C7 | −0.7 (4) | C16—N2—C20—C19 | −0.2 (5) |
C5—C6—C7—C8 | 0.7 (4) | Co1—N2—C20—C19 | 173.7 (2) |
C5—C6—C7—C10 | −176.7 (3) | C18—C19—C20—N2 | 0.4 (5) |
C6—C7—C8—C9 | 0.0 (5) |
Symmetry codes: (i) −x+5/2, −y+1, z−1/2; (ii) −x+5/2, −y+1, z+1/2. |
D—H···A | D—H | H···A | D···A | D—H···A |
O1W—H1W2···O2 | 0.86 (1) | 1.80 (2) | 2.644 (3) | 166 (6) |
O1W—H1W1···O4iii | 0.85 (1) | 2.01 (2) | 2.837 (3) | 164 (5) |
Symmetry code: (iii) −x+3/2, −y+1, z−1/2. |
Experimental details
Crystal data | |
Chemical formula | [Co(C10H8O5)(C10H8N2)(H2O)] |
Mr | 441.29 |
Crystal system, space group | Orthorhombic, P212121 |
Temperature (K) | 295 |
a, b, c (Å) | 6.7193 (2), 16.1369 (5), 17.2762 (7) |
V (Å3) | 1873.2 (1) |
Z | 4 |
Radiation type | Mo Kα |
µ (mm−1) | 0.96 |
Crystal size (mm) | 0.38 × 0.25 × 0.17 |
Data collection | |
Diffractometer | Rigaku R-AXIS RAPID |
Absorption correction | Multi-scan (ABSCOR; Higashi, 1995) |
Tmin, Tmax | 0.546, 0.854 |
No. of measured, independent and observed [I > 2σ(I)] reflections | 18344, 4282, 3233 |
Rint | 0.041 |
(sin θ/λ)max (Å−1) | 0.649 |
Refinement | |
R[F2 > 2σ(F2)], wR(F2), S | 0.034, 0.087, 1.00 |
No. of reflections | 4282 |
No. of parameters | 271 |
No. of restraints | 2 |
H-atom treatment | H atoms treated by a mixture of independent and constrained refinement |
Δρmax, Δρmin (e Å−3) | 0.33, −0.35 |
Absolute structure | Flack (1983), with 1820 Friedel pairs |
Absolute structure parameter | 0.47 (2) |
Computer programs: RAPID-AUTO (Rigaku, 1998), CrystalStructure (Rigaku/MSC, 2002), SHELXS97 (Sheldrick, 1997), SHELXL97 (Sheldrick, 1997), X-SEED (Barbour, 2001), publCIF (Westrip, 2007).
D—H···A | D—H | H···A | D···A | D—H···A |
O1W—H1W2···O2 | 0.86 (1) | 1.80 (2) | 2.644 (3) | 166 (6) |
O1W—H1W1···O4i | 0.85 (1) | 2.01 (2) | 2.837 (3) | 164 (5) |
Symmetry code: (i) −x+3/2, −y+1, z−1/2. |
Subscribe to Acta Crystallographica Section E: Crystallographic Communications
The full text of this article is available to subscribers to the journal.
- Information on subscribing
- Sample issue
- If you have already subscribed, you may need to register