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metal-organic compounds
Both carboxylate groups chelate to the Cd atom in the title compound, [Cd(C9H7O3)2(C6H12N4)2(H2O)]·3H2O. The four O atoms involved in chelation and one water molecule form a pentagonal plane around the Cd atom, while the N atoms of the hexamethylenetetramine ligands occupy the axial sites of the pentagonal bipyramid. Hydrogen bonds link the molecules of the complex with the solvent water molecules to form a three-dimensional network.
Supporting information
Crystallographic Information File (CIF) https://doi.org/10.1107/S1600536805016545/ac6174sup1.cif | |
Structure factor file (CIF format) https://doi.org/10.1107/S1600536805016545/ac6174Isup2.hkl |
CCDC reference: 274319
Key indicators
- Single-crystal X-ray study
- T = 295 K
- Mean (C-C) = 0.006 Å
- Disorder in solvent or counterion
- R factor = 0.042
- wR factor = 0.103
- Data-to-parameter ratio = 15.9
checkCIF/PLATON results
No syntax errors found
Alert level A PLAT305_ALERT_2_A Isolated Hydrogen Atom (Outside Bond Range ??) <H3'1 PLAT305_ALERT_2_A Isolated Hydrogen Atom (Outside Bond Range ??) <H3'2
Alert level B ABSTM02_ALERT_3_B The ratio of expected to reported Tmax/Tmin(RR') is < 0.75 Tmin and Tmax reported: 0.585 0.901 Tmin' and Tmax expected: 0.782 0.899 RR' = 0.746 Please check that your absorption correction is appropriate. PLAT061_ALERT_3_B Tmax/Tmin Range Test RR' too Large ............. 0.74 PLAT430_ALERT_2_B Short Inter D...A Contact O1 .. O3' .. 2.79 Ang. PLAT731_ALERT_1_B Bond Calc 0.87(7), Rep 0.860(10) ...... 7.00 su-Rat O4W -H4W1 1.555 1.555 PLAT731_ALERT_1_B Bond Calc 0.86(6), Rep 0.860(10) ...... 6.00 su-Rat O4W -H4W2 1.555 1.555 PLAT732_ALERT_1_B Angle Calc 127(2), Rep 127.2(3) ...... 6.67 su-Rat C11 -C12 -C13 1.555 1.555 1.555 PLAT735_ALERT_1_B D-H Calc 0.87(7), Rep 0.860(10) ...... 7.00 su-Rat O4W -H9# 1.555 1.555 PLAT735_ALERT_1_B D-H Calc 0.86(6), Rep 0.860(10) ...... 6.00 su-Rat O4W -H10# 1.555 1.555 PLAT736_ALERT_1_B H...A Calc 1.86(7), Rep 1.860(10) ...... 7.00 su-Rat H9# -O4 1.555 1.555 PLAT736_ALERT_1_B H...A Calc 2.08(7), Rep 2.080(10) ...... 7.00 su-Rat H10# -N4 1.555 4.575
Alert level C PLAT041_ALERT_1_C Calc. and Rep. SumFormula Strings Differ .... ? PLAT042_ALERT_1_C Calc. and Rep. MoietyFormula Strings Differ .... ? PLAT068_ALERT_1_C Reported F000 Differs from Calcd (or Missing)... ? PLAT302_ALERT_4_C Anion/Solvent Disorder ......................... 25.00 Perc. PLAT311_ALERT_2_C Isolated Disordered Oxygen Atom (No H's ?) ..... <O3' PLAT720_ALERT_4_C Number of Unusual/Non-Standard Label(s) ........ 10 PLAT731_ALERT_1_C Bond Calc 1.309(16), Rep 1.309(4) ...... 4.00 su-Rat C11 -C12 1.555 1.555 PLAT731_ALERT_1_C Bond Calc 1.466(11), Rep 1.466(4) ...... 2.75 su-Rat C12 -C13 1.555 1.555 PLAT731_ALERT_1_C Bond Calc 0.85(3), Rep 0.850(10) ...... 3.00 su-Rat O3 -H3O 1.555 1.555 PLAT731_ALERT_1_C Bond Calc 0.85(3), Rep 0.850(10) ...... 3.00 su-Rat O6 -H6O 1.555 1.555 PLAT732_ALERT_1_C Angle Calc 123.9(12), Rep 123.9(3) ...... 4.00 su-Rat C12 -C11 -C10 1.555 1.555 1.555 PLAT732_ALERT_1_C Angle Calc 119.2(11), Rep 119.2(3) ...... 3.67 su-Rat C14 -C13 -C12 1.555 1.555 1.555 PLAT732_ALERT_1_C Angle Calc 122.9(12), Rep 122.9(3) ...... 4.00 su-Rat C18 -C13 -C12 1.555 1.555 1.555 PLAT732_ALERT_1_C Angle Calc 109(6), Rep 109(2) ...... 3.00 su-Rat H4W1 -O4W -H4W2 1.555 1.555 1.555 PLAT735_ALERT_1_C D-H Calc 0.85(3), Rep 0.850(10) ...... 3.00 su-Rat O3 -H3O 1.555 1.555 PLAT735_ALERT_1_C D-H Calc 0.85(3), Rep 0.850(10) ...... 3.00 su-Rat O6 -H6O 1.555 1.555 PLAT736_ALERT_1_C H...A Calc 1.98(3), Rep 1.990(10) ...... 3.00 su-Rat H3O -N7 1.555 3.767 PLAT736_ALERT_1_C H...A Calc 1.88(4), Rep 1.870(10) ...... 4.00 su-Rat H6O -O5 1.555 3.566
2 ALERT level A = In general: serious problem 10 ALERT level B = Potentially serious problem 18 ALERT level C = Check and explain 0 ALERT level G = General alerts; check 22 ALERT type 1 CIF construction/syntax error, inconsistent or missing data 4 ALERT type 2 Indicator that the structure model may be wrong or deficient 2 ALERT type 3 Indicator that the structure quality may be low 2 ALERT type 4 Improvement, methodology, query or suggestion
Computing details top
Data collection: SMART (Bruker, 2002); cell refinement: SAINT (Bruker, 2002); data reduction: SAINT; program(s) used to solve structure: SHELXS97 (Sheldrick, 1997); program(s) used to refine structure: SHELXL97 (Sheldrick, 1997); molecular graphics: ORTEPII (Johnson, 1976); software used to prepare material for publication: SHELXL97.
Crystal data top
[Cd(C9H7O3)2(C6H12N4)2(H2O)]·3H2O | F(000) = 1640 |
Mr = 791.15 | Dx = 1.538 Mg m−3 |
Monoclinic, P21/c | Mo Kα radiation, λ = 0.71073 Å |
Hall symbol: -P 2ybc | Cell parameters from 5924 reflections |
a = 11.1249 (6) Å | θ = 2.2–26.7° |
b = 21.926 (1) Å | µ = 0.71 mm−1 |
c = 14.6557 (7) Å | T = 295 K |
β = 107.096 (1)° | Block, colourless |
V = 3416.9 (3) Å3 | 0.34 × 0.25 × 0.15 mm |
Z = 4 |
Data collection top
Bruker APEX area-detector diffractometer | 7680 independent reflections |
Radiation source: fine-focus sealed tube | 6442 reflections with I > 2σ(I) |
Graphite monochromator | Rint = 0.031 |
φ and ω scans | θmax = 27.5°, θmin = 1.7° |
Absorption correction: multi-scan (SADABS; Bruker, 2002) | h = −14→14 |
Tmin = 0.585, Tmax = 0.901 | k = −24→28 |
21045 measured reflections | l = −17→18 |
Refinement top
Refinement on F2 | Primary atom site location: structure-invariant direct methods |
Least-squares matrix: full | Secondary atom site location: difference Fourier map |
R[F2 > 2σ(F2)] = 0.042 | Hydrogen site location: inferred from neighbouring sites |
wR(F2) = 0.103 | H atoms treated by a mixture of independent and constrained refinement |
S = 1.03 | w = 1/[σ2(Fo2) + (0.0538P)2 + 1.0651P] where P = (Fo2 + 2Fc2)/3 |
7680 reflections | (Δ/σ)max = 0.001 |
482 parameters | Δρmax = 0.70 e Å−3 |
17 restraints | Δρmin = −0.46 e Å−3 |
Fractional atomic coordinates and isotropic or equivalent isotropic displacement parameters (Å2) top
x | y | z | Uiso*/Ueq | Occ. (<1) | |
Cd1 | 0.48061 (2) | 0.58514 (1) | 0.79186 (1) | 0.02887 (8) | |
O1 | 0.5960 (2) | 0.6730 (1) | 0.8734 (1) | 0.0413 (5) | |
O2 | 0.6538 (2) | 0.5819 (1) | 0.9326 (2) | 0.0410 (5) | |
O3 | 1.0148 (2) | 0.5560 (1) | 1.1987 (2) | 0.0453 (5) | |
O4 | 0.3594 (2) | 0.6482 (1) | 0.6789 (2) | 0.0488 (5) | |
O5 | 0.2852 (2) | 0.5552 (1) | 0.6530 (2) | 0.0474 (5) | |
O6 | −0.0950 (2) | 0.5264 (1) | 0.3902 (2) | 0.0571 (6) | |
O1W | 0.4938 (2) | 0.4812 (1) | 0.8077 (1) | 0.0359 (4) | |
O2W | 0.4998 (3) | 0.4136 (1) | 0.6524 (2) | 0.0557 (6) | |
O3W | 0.4825 (5) | 0.2923 (2) | 0.6023 (5) | 0.0815 (15) | 0.564 (6) |
O3' | 0.5023 (7) | 0.2836 (3) | 0.7094 (6) | 0.0815 (15) | 0.44 |
O4W | 0.4380 (5) | 0.7312 (2) | 0.5705 (6) | 0.179 (2) | |
N1 | 0.3363 (2) | 0.5948 (1) | 0.8884 (2) | 0.0283 (5) | |
N2 | 0.1259 (2) | 0.5867 (1) | 0.9082 (2) | 0.0402 (6) | |
N3 | 0.3094 (2) | 0.5690 (1) | 1.0440 (2) | 0.0388 (6) | |
N4 | 0.2619 (2) | 0.6719 (1) | 0.9802 (2) | 0.0424 (6) | |
N5 | 0.6340 (2) | 0.5811 (1) | 0.7002 (2) | 0.0311 (5) | |
N6 | 0.8007 (3) | 0.6368 (1) | 0.6573 (2) | 0.0486 (7) | |
N7 | 0.8165 (2) | 0.5264 (1) | 0.6792 (2) | 0.0422 (6) | |
N8 | 0.6607 (3) | 0.5695 (1) | 0.5407 (2) | 0.0434 (6) | |
C1 | 0.6704 (3) | 0.6387 (1) | 0.9332 (2) | 0.0336 (6) | |
C2 | 0.7797 (3) | 0.6669 (1) | 1.0036 (2) | 0.0390 (7) | |
C3 | 0.8626 (3) | 0.6351 (1) | 1.0678 (2) | 0.0357 (6) | |
C4 | 0.9776 (3) | 0.6565 (1) | 1.1386 (2) | 0.0335 (6) | |
C5 | 1.0528 (3) | 0.6153 (1) | 1.2035 (2) | 0.0347 (6) | |
C6 | 1.1631 (3) | 0.6351 (2) | 1.2697 (2) | 0.0428 (7) | |
C7 | 1.1991 (3) | 0.6943 (2) | 1.2717 (2) | 0.0515 (8) | |
C8 | 1.1265 (3) | 0.7356 (2) | 1.2082 (2) | 0.0538 (9) | |
C9 | 1.0173 (3) | 0.7170 (1) | 1.1431 (2) | 0.0460 (8) | |
C10 | 0.2788 (3) | 0.6105 (2) | 0.6311 (2) | 0.0408 (7) | |
C11 | 0.1768 (3) | 0.6367 (2) | 0.5507 (2) | 0.0462 (7) | |
C12 | 0.0808 (3) | 0.6053 (14) | 0.4989 (2) | 0.0382 (7) | |
C13 | −0.0251 (3) | 0.6280 (1) | 0.4210 (2) | 0.0363 (6) | |
C14 | −0.1141 (3) | 0.5867 (1) | 0.3684 (2) | 0.0397 (7) | |
C15 | −0.2172 (3) | 0.6070 (2) | 0.2954 (2) | 0.0491 (8) | |
C16 | −0.2321 (3) | 0.6676 (2) | 0.2750 (2) | 0.0607 (10) | |
C17 | −0.1444 (4) | 0.7095 (2) | 0.3255 (3) | 0.0629 (10) | |
C18 | −0.0424 (3) | 0.6896 (2) | 0.3973 (2) | 0.0468 (8) | |
C19 | 0.2036 (3) | 0.5767 (1) | 0.8442 (2) | 0.0360 (6) | |
C20 | 0.3841 (3) | 0.5589 (1) | 0.9774 (2) | 0.0367 (6) | |
C21 | 0.3377 (3) | 0.6598 (1) | 0.9154 (2) | 0.0386 (7) | |
C22 | 0.1790 (3) | 0.5516 (1) | 0.9956 (2) | 0.0402 (7) | |
C23 | 0.1322 (3) | 0.6516 (1) | 0.9327 (2) | 0.0455 (8) | |
C24 | 0.3120 (3) | 0.6344 (1) | 1.0656 (2) | 0.0461 (8) | |
C25 | 0.5710 (3) | 0.5723 (1) | 0.5967 (2) | 0.0352 (6) | |
C26 | 0.7235 (3) | 0.5301 (1) | 0.7324 (2) | 0.0378 (6) | |
C27 | 0.7085 (3) | 0.6382 (1) | 0.7109 (2) | 0.0422 (7) | |
C28 | 0.7328 (3) | 0.6271 (2) | 0.5566 (2) | 0.0507 (8) | |
C29 | 0.8840 (3) | 0.5849 (2) | 0.6908 (3) | 0.0528 (9) | |
C30 | 0.7478 (3) | 0.5191 (2) | 0.5776 (2) | 0.0457 (7) | |
H3O | 1.065 (3) | 0.532 (1) | 1.237 (2) | 0.054* | |
H6O | −0.162 (2) | 0.506 (2) | 0.369 (3) | 0.069* | |
H1W1 | 0.486 (2) | 0.464 (1) | 0.754 (1) | 0.043* | |
H1W2 | 0.561 (2) | 0.468 (1) | 0.848 (1) | 0.043* | |
H2W1 | 0.493 (3) | 0.376 (1) | 0.661 (2) | 0.067* | |
H2W2 | 0.453 (3) | 0.424 (1) | 0.598 (1) | 0.067* | |
H3W1 | 0.426 (6) | 0.268 (3) | 0.611 (5) | 0.098* | 0.564 (6) |
H3W2 | 0.494 (7) | 0.284 (3) | 0.549 (3) | 0.098* | 0.564 (6) |
H3'1 | 0.444 (7) | 0.262 (4) | 0.672 (5) | 0.098* | 0.436 (6) |
H3'2 | 0.520 (9) | 0.268 (4) | 0.765 (3) | 0.098* | 0.436 (6) |
H4W1 | 0.409 (6) | 0.705 (3) | 0.603 (5) | 0.215* | |
H4W2 | 0.381 (5) | 0.758 (3) | 0.547 (5) | 0.215* | |
H2 | 0.7899 | 0.7089 | 1.0021 | 0.047* | |
H3 | 0.8465 | 0.5935 | 1.0687 | 0.043* | |
H6 | 1.2125 | 0.6075 | 1.3129 | 0.051* | |
H7 | 1.2731 | 0.7070 | 1.3162 | 0.062* | |
H8 | 1.1517 | 0.7762 | 1.2095 | 0.065* | |
H9 | 0.9684 | 0.7454 | 1.1010 | 0.055* | |
H11 | 0.1816 | 0.6778 | 0.5364 | 0.055* | |
H12 | 0.0797 | 0.5640 | 0.5132 | 0.046* | |
H15 | −0.2759 | 0.5792 | 0.2606 | 0.059* | |
H16 | −0.3018 | 0.6810 | 0.2268 | 0.073* | |
H17 | −0.1545 | 0.7508 | 0.3108 | 0.076* | |
H18 | 0.0165 | 0.7178 | 0.4309 | 0.056* | |
H19A | 0.1692 | 0.6000 | 0.7861 | 0.043* | |
H19B | 0.2005 | 0.5339 | 0.8271 | 0.043* | |
H20A | 0.3822 | 0.5159 | 0.9615 | 0.044* | |
H20B | 0.4709 | 0.5701 | 1.0084 | 0.044* | |
H21A | 0.4238 | 0.6722 | 0.9460 | 0.046* | |
H21B | 0.3057 | 0.6841 | 0.8581 | 0.046* | |
H22A | 0.1759 | 0.5085 | 0.9800 | 0.048* | |
H22B | 0.1283 | 0.5580 | 1.0385 | 0.048* | |
H23A | 0.0806 | 0.6592 | 0.9745 | 0.055* | |
H23B | 0.0981 | 0.6752 | 0.8750 | 0.055* | |
H24A | 0.2630 | 0.6417 | 1.1095 | 0.055* | |
H24B | 0.3980 | 0.6466 | 1.0972 | 0.055* | |
H25A | 0.5226 | 0.5348 | 0.5875 | 0.042* | |
H25B | 0.5129 | 0.6057 | 0.5734 | 0.042* | |
H26A | 0.7670 | 0.5351 | 0.7998 | 0.045* | |
H26B | 0.6769 | 0.4921 | 0.7247 | 0.045* | |
H27A | 0.6519 | 0.6723 | 0.6889 | 0.051* | |
H27B | 0.7521 | 0.6447 | 0.7780 | 0.051* | |
H28A | 0.7924 | 0.6265 | 0.5198 | 0.061* | |
H28B | 0.6756 | 0.6609 | 0.5339 | 0.061* | |
H29A | 0.9291 | 0.5907 | 0.7577 | 0.063* | |
H29B | 0.9455 | 0.5834 | 0.6557 | 0.063* | |
H30A | 0.8077 | 0.5166 | 0.5412 | 0.055* | |
H30B | 0.7011 | 0.4812 | 0.5688 | 0.055* |
Atomic displacement parameters (Å2) top
U11 | U22 | U33 | U12 | U13 | U23 | |
Cd1 | 0.0258 (1) | 0.0348 (1) | 0.0239 (1) | 0.0010 (1) | 0.0040 (1) | 0.0004 (1) |
O1 | 0.036 (1) | 0.046 (1) | 0.036 (1) | 0.003 (1) | 0.001 (1) | 0.000 (1) |
O2 | 0.040 (1) | 0.037 (1) | 0.039 (1) | −0.004 (1) | 0.000 (1) | −0.005 (1) |
O3 | 0.040 (1) | 0.038 (1) | 0.049 (1) | 0.003 (1) | 0.000 (1) | 0.002 (1) |
O4 | 0.043 (1) | 0.056 (1) | 0.038 (1) | 0.004 (1) | −0.003 (1) | 0.007 (1) |
O5 | 0.046 (1) | 0.052 (1) | 0.038 (1) | 0.007 (1) | 0.003 (1) | 0.008 (1) |
O6 | 0.056 (2) | 0.055 (2) | 0.053 (1) | −0.009 (1) | 0.004 (1) | 0.014 (1) |
O1W | 0.037 (1) | 0.036 (1) | 0.028 (1) | 0.001 (1) | 0.001 (1) | 0.002 (1) |
O2W | 0.062 (2) | 0.056 (2) | 0.042 (1) | −0.012 (1) | 0.005 (1) | −0.012 (1) |
O3W | 0.069 (3) | 0.050 (2) | 0.118 (4) | −0.007 (2) | 0.016 (3) | −0.012 (3) |
O3' | 0.069 (3) | 0.050 (2) | 0.118 (4) | −0.007 (2) | 0.016 (3) | −0.012 (3) |
O4W | 0.134 (4) | 0.123 (4) | 0.303 (8) | 0.035 (3) | 0.097 (5) | 0.107 (4) |
N1 | 0.029 (1) | 0.030 (1) | 0.024 (1) | 0.005 (1) | 0.005 (1) | 0.0022 (1) |
N2 | 0.032 (1) | 0.051 (2) | 0.039 (1) | 0.002 (1) | 0.012 (1) | −0.003 (1) |
N3 | 0.043 (2) | 0.044 (1) | 0.032 (1) | 0.005 (1) | 0.014 (1) | 0.007 (1) |
N4 | 0.054 (2) | 0.034 (1) | 0.045 (2) | 0.000 (1) | 0.024 (1) | −0.004 (1) |
N5 | 0.028 (1) | 0.036 (1) | 0.029 (1) | −0.002 (1) | 0.007 (1) | −0.001 (1) |
N6 | 0.044 (2) | 0.058 (2) | 0.049 (2) | −0.016 (1) | 0.023 (1) | −0.008 (1) |
N7 | 0.031 (1) | 0.055 (2) | 0.042 (1) | 0.004 (1) | 0.013 (1) | −0.005 (1) |
N8 | 0.044 (2) | 0.056 (2) | 0.032 (1) | −0.002 (1) | 0.014 (1) | −0.003 (1) |
C1 | 0.030 (2) | 0.045 (2) | 0.025 (1) | −0.001 (1) | 0.007 (1) | −0.004 (1) |
C2 | 0.040 (2) | 0.033 (1) | 0.039 (2) | −0.005 (1) | 0.003 (1) | −0.004 (1) |
C3 | 0.036 (2) | 0.032 (1) | 0.037 (2) | −0.005 (1) | 0.006 (1) | −0.005 (1) |
C4 | 0.033 (2) | 0.040 (2) | 0.027 (1) | −0.003 (2) | 0.008 (1) | −0.002 (1) |
C5 | 0.031 (2) | 0.044 (2) | 0.030 (1) | 0.000 (1) | 0.012 (1) | −0.004 (1) |
C6 | 0.034 (2) | 0.055 (2) | 0.035 (2) | 0.004 (1) | 0.005 (1) | −0.006 (1) |
C7 | 0.038 (2) | 0.063 (2) | 0.045 (2) | −0.014 (2) | 0.000 (1) | −0.013 (2) |
C8 | 0.060 (2) | 0.048 (2) | 0.046 (2) | −0.022 (2) | 0.004 (2) | −0.010 (2) |
C9 | 0.049 (2) | 0.045 (2) | 0.037 (2) | −0.010 (1) | 0.001 (1) | −0.003 (1) |
C10 | 0.034 (2) | 0.063 (2) | 0.026 (1) | 0.015 (2) | 0.010 (1) | 0.005 (1) |
C11 | 0.045 (2) | 0.050 (2) | 0.037 (2) | 0.007 (2) | 0.003 (1) | 0.008 (1) |
C12 | 0.038 (2) | 0.048 (2) | 0.030 (2) | 0.010 (1) | 0.011 (1) | 0.006 (1) |
C13 | 0.031 (2) | 0.051 (2) | 0.028 (1) | 0.008 (1) | 0.011 (1) | 0.004 (1) |
C14 | 0.034 (2) | 0.056 (2) | 0.031 (2) | 0.002 (1) | 0.012 (1) | 0.007 (1) |
C15 | 0.031 (2) | 0.075 (2) | 0.039 (2) | 0.000 (2) | 0.008 (1) | 0.001 (2) |
C16 | 0.041 (2) | 0.084 (3) | 0.047 (2) | 0.024 (2) | −0.002 (2) | 0.009 (2) |
C17 | 0.066 (3) | 0.056 (2) | 0.058 (2) | 0.028 (2) | 0.004 (2) | 0.009 (2) |
C18 | 0.046 (2) | 0.050 (2) | 0.040 (2) | 0.010 (2) | 0.005 (1) | 0.001 (1) |
C19 | 0.031 (2) | 0.047 (2) | 0.029 (1) | 0.001 (1) | 0.006 (1) | −0.003 (1) |
C20 | 0.034 (2) | 0.045 (2) | 0.030 (1) | 0.010 (1) | 0.007 (1) | 0.007 (1) |
C21 | 0.043 (2) | 0.035 (2) | 0.040 (2) | −0.002 (1) | 0.010 (1) | 0.002 (1) |
C22 | 0.044 (2) | 0.039 (2) | 0.042 (2) | 0.000 (1) | 0.020 (1) | 0.004 (1) |
C23 | 0.046 (2) | 0.051 (2) | 0.046 (2) | 0.018 (2) | 0.023 (2) | 0.008 (2) |
C24 | 0.052 (2) | 0.056 (2) | 0.033 (2) | −0.004 (2) | 0.017 (1) | −0.011 (1) |
C25 | 0.031 (2) | 0.046 (2) | 0.027 (1) | −0.001 (1) | 0.007 (1) | −0.004 (1) |
C26 | 0.031 (2) | 0.049 (2) | 0.033 (2) | 0.004 (1) | 0.008 (1) | 0.002 (1) |
C27 | 0.042 (2) | 0.043 (2) | 0.045 (2) | −0.013 (1) | 0.016 (1) | −0.010 (1) |
C28 | 0.052 (2) | 0.063 (2) | 0.045 (2) | −0.006 (2) | 0.027 (2) | 0.003 (2) |
C29 | 0.028 (2) | 0.083 (3) | 0.048 (2) | −0.007 (2) | 0.011 (1) | −0.007 (2) |
C30 | 0.042 (2) | 0.058 (2) | 0.041 (2) | 0.004 (2) | 0.018 (1) | −0.008 (2) |
Geometric parameters (Å, º) top
Cd1—O1 | 2.426 (2) | C15—C16 | 1.361 (5) |
Cd1—O2 | 2.375 (2) | C16—C17 | 1.386 (5) |
Cd1—O4 | 2.272 (2) | C17—C18 | 1.373 (5) |
Cd1—O5 | 2.588 (2) | O3—H3O | 0.85 (1) |
Cd1—O1W | 2.290 (2) | O6—H6O | 0.85 (1) |
Cd1—N1 | 2.441 (2) | O1W—H1W1 | 0.85 (1) |
Cd1—N5 | 2.465 (2) | O1W—H1W2 | 0.85 (1) |
O1—C1 | 1.262 (3) | O2W—H2W1 | 0.85 (1) |
O2—C1 | 1.258 (3) | O2W—H2W2 | 0.85 (1) |
O3—C5 | 1.363 (4) | O3W—H3W1 | 0.86 (1) |
O4—C10 | 1.269 (4) | O3W—H3W2 | 0.85 (1) |
O5—C10 | 1.250 (4) | O3'—H3'1 | 0.86 (1) |
O6—C14 | 1.362 (4) | O3'—H3'2 | 0.86 (1) |
N1—C21 | 1.477 (3) | O4W—H4W1 | 0.86 (1) |
N1—C19 | 1.481 (4) | O4W—H4W2 | 0.86 (1) |
N1—C20 | 1.483 (3) | C2—H2 | 0.93 |
N2—C23 | 1.463 (4) | C3—H3 | 0.93 |
N2—C22 | 1.462 (4) | C6—H6 | 0.93 |
N2—C19 | 1.467 (4) | C7—H7 | 0.93 |
N3—C22 | 1.466 (4) | C8—H8 | 0.93 |
N3—C24 | 1.466 (4) | C9—H9 | 0.93 |
N3—C20 | 1.473 (3) | C11—H11 | 0.93 |
N4—C24 | 1.465 (4) | C12—H12 | 0.93 |
N4—C21 | 1.469 (3) | C15—H15 | 0.93 |
N4—C23 | 1.475 (4) | C16—H16 | 0.93 |
N5—C26 | 1.479 (3) | C17—H17 | 0.93 |
N5—C25 | 1.484 (3) | C18—H18 | 0.93 |
N5—C27 | 1.485 (3) | C19—H19A | 0.97 |
N6—C29 | 1.459 (4) | C19—H19B | 0.97 |
N6—C27 | 1.464 (4) | C20—H20A | 0.97 |
N6—C28 | 1.462 (4) | C20—H20B | 0.97 |
N7—C26 | 1.469 (4) | C21—H21A | 0.97 |
N7—C29 | 1.469 (4) | C21—H21B | 0.97 |
N7—C30 | 1.469 (4) | C22—H22A | 0.97 |
N8—C30 | 1.463 (4) | C22—H22B | 0.97 |
N8—C25 | 1.468 (4) | C23—H23A | 0.97 |
N8—C28 | 1.479 (4) | C23—H23B | 0.97 |
C1—C2 | 1.479 (4) | C24—H24A | 0.97 |
C2—C3 | 1.309 (4) | C24—H24B | 0.97 |
C3—C4 | 1.468 (4) | C25—H25A | 0.97 |
C4—C9 | 1.394 (4) | C25—H25B | 0.97 |
C4—C5 | 1.397 (4) | C26—H26A | 0.97 |
C5—C6 | 1.392 (4) | C26—H26B | 0.97 |
C6—C7 | 1.356 (4) | C27—H27A | 0.97 |
C7—C8 | 1.379 (5) | C27—H27B | 0.97 |
C8—C9 | 1.367 (4) | C28—H28A | 0.97 |
C10—C11 | 1.490 (4) | C28—H28B | 0.97 |
C11—C12 | 1.309 (4) | C29—H29A | 0.97 |
C12—C13 | 1.466 (4) | C29—H29B | 0.97 |
C13—C14 | 1.394 (4) | C30—H30A | 0.97 |
C13—C18 | 1.395 (4) | C30—H30B | 0.97 |
C14—C15 | 1.391 (4) | ||
O1—Cd1—O2 | 54.48 (6) | N6—C29—N7 | 112.8 (3) |
O1—Cd1—O4 | 89.43 (8) | N8—C30—N7 | 112.5 (2) |
O1—Cd1—O5 | 142.11 (7) | C5—O3—H3O | 115 (2) |
O1—Cd1—O1W | 136.98 (7) | C14—O6—H6O | 112 (3) |
O1—Cd1—N1 | 89.36 (7) | Cd1—O1W—H1W1 | 111 (2) |
O1—Cd1—N5 | 86.90 (7) | Cd1—O1W—H1W2 | 116 (2) |
O2—Cd1—O4 | 143.87 (7) | H1W1—O1W—H1W2 | 108 (2) |
O2—Cd1—O5 | 162.81 (7) | H2W1—O2W—H2W2 | 110 (2) |
O2—Cd1—O1W | 82.56 (7) | H3W1—O3W—H3W2 | 109 (2) |
O2—Cd1—N1 | 90.19 (8) | H3'1—O3'—H3'2 | 108 (2) |
O2—Cd1—N5 | 87.56 (8) | H4W1—O4W—H4W2 | 109 (2) |
O4—Cd1—O5 | 53.12 (7) | C3—C2—H2 | 118.7 |
O4—Cd1—O1W | 133.34 (8) | C1—C2—H2 | 118.7 |
O4—Cd1—N1 | 91.09 (8) | C2—C3—H3 | 115.8 |
O4—Cd1—N5 | 88.97 (8) | C4—C3—H3 | 115.8 |
O5—Cd1—N1 | 86.22 (7) | C7—C6—H6 | 119.7 |
O5—Cd1—N5 | 96.79 (7) | C5—C6—H6 | 119.7 |
O5—Cd1—O1W | 80.89 (7) | C6—C7—H7 | 119.9 |
O1W—Cd1—N1 | 93.50 (7) | C8—C7—H7 | 119.9 |
O1W—Cd1—N5 | 89.17 (7) | C9—C8—H8 | 120.0 |
N1—Cd1—N5 | 176.26 (7) | C7—C8—H8 | 120.0 |
C1—O1—Cd1 | 90.70 (17) | C8—C9—H9 | 119.3 |
C1—O2—Cd1 | 93.20 (17) | C4—C9—H9 | 119.3 |
C10—O4—Cd1 | 100.18 (18) | C12—C11—H11 | 118.1 |
C10—O5—Cd1 | 85.81 (18) | C10—C11—H11 | 118.1 |
C21—N1—C19 | 107.8 (2) | C11—C12—H12 | 116.4 |
C21—N1—C20 | 107.7 (2) | C13—C12—H12 | 116.4 |
C19—N1—C20 | 107.2 (2) | C16—C15—H15 | 120.0 |
C21—N1—Cd1 | 106.40 (15) | C14—C15—H15 | 120.0 |
C19—N1—Cd1 | 117.69 (16) | C15—C16—H16 | 119.7 |
C20—N1—Cd1 | 109.69 (15) | C17—C16—H16 | 119.7 |
C23—N2—C22 | 108.6 (2) | C18—C17—H17 | 120.3 |
C23—N2—C19 | 107.9 (2) | C16—C17—H17 | 120.3 |
C22—N2—C19 | 108.6 (2) | C17—C18—H18 | 119.3 |
C22—N3—C24 | 108.3 (2) | C13—C18—H18 | 119.3 |
C22—N3—C20 | 108.1 (2) | N2—C19—H19A | 109.1 |
C24—N3—C20 | 108.2 (2) | N1—C19—H19A | 109.1 |
C24—N4—C21 | 107.7 (2) | N2—C19—H19B | 109.1 |
C24—N4—C23 | 107.9 (2) | N1—C19—H19B | 109.1 |
C21—N4—C23 | 107.9 (2) | H19A—C19—H19B | 107.9 |
C26—N5—C25 | 107.4 (2) | N3—C20—H20A | 109.2 |
C26—N5—C27 | 107.6 (2) | N1—C20—H20A | 109.2 |
C25—N5—C27 | 107.4 (2) | N3—C20—H20B | 109.2 |
C26—N5—Cd1 | 111.20 (15) | N1—C20—H20B | 109.2 |
C25—N5—Cd1 | 111.50 (16) | H20A—C20—H20B | 107.9 |
C27—N5—Cd1 | 111.46 (16) | N4—C21—H21A | 109.1 |
C29—N6—C27 | 108.2 (3) | N1—C21—H21A | 109.1 |
C29—N6—C28 | 108.4 (3) | N4—C21—H21B | 109.1 |
C27—N6—C28 | 108.1 (2) | N1—C21—H21B | 109.1 |
C26—N7—C29 | 107.9 (2) | H21A—C21—H21B | 107.8 |
C26—N7—C30 | 107.8 (2) | N2—C22—H22A | 109.2 |
C29—N7—C30 | 107.9 (3) | N3—C22—H22A | 109.2 |
C30—N8—C25 | 108.1 (2) | N2—C22—H22B | 109.2 |
C30—N8—C28 | 108.5 (3) | N3—C22—H22B | 109.2 |
C25—N8—C28 | 107.6 (2) | H22A—C22—H22B | 107.9 |
O2—C1—O1 | 121.4 (3) | N2—C23—H23A | 109.1 |
O2—C1—C2 | 120.5 (3) | N4—C23—H23A | 109.1 |
O1—C1—C2 | 118.1 (3) | N2—C23—H23B | 109.1 |
C3—C2—C1 | 122.7 (3) | N4—C23—H23B | 109.1 |
C2—C3—C4 | 128.4 (3) | H23A—C23—H23B | 107.9 |
C9—C4—C5 | 117.8 (3) | N4—C24—H24A | 109.1 |
C9—C4—C3 | 122.4 (3) | N3—C24—H24A | 109.1 |
C5—C4—C3 | 119.8 (3) | N4—C24—H24B | 109.1 |
O3—C5—C6 | 122.0 (3) | N3—C24—H24B | 109.1 |
O3—C5—C4 | 117.9 (2) | H24A—C24—H24B | 107.8 |
C6—C5—C4 | 120.1 (3) | N8—C25—H25A | 109.1 |
C7—C6—C5 | 120.5 (3) | N5—C25—H25A | 109.1 |
C6—C7—C8 | 120.3 (3) | N8—C25—H25B | 109.1 |
C9—C8—C7 | 119.9 (3) | N5—C25—H25B | 109.1 |
C8—C9—C4 | 121.4 (3) | H25A—C25—H25B | 107.9 |
O5—C10—O4 | 120.9 (3) | N7—C26—H26A | 109.1 |
O5—C10—C11 | 123.3 (3) | N5—C26—H26A | 109.1 |
O4—C10—C11 | 115.8 (3) | N7—C26—H26B | 109.1 |
C12—C11—C10 | 123.9 (3) | N5—C26—H26B | 109.1 |
C11—C12—C13 | 127.2 (3) | H26A—C26—H26B | 107.8 |
C14—C13—C18 | 117.8 (3) | N6—C27—H27A | 109.1 |
C14—C13—C12 | 119.2 (3) | N5—C27—H27A | 109.1 |
C18—C13—C12 | 122.9 (3) | N6—C27—H27B | 109.1 |
O6—C14—C15 | 121.8 (3) | N5—C27—H27B | 109.1 |
O6—C14—C13 | 117.6 (3) | H27A—C27—H27B | 107.9 |
C15—C14—C13 | 120.6 (3) | N6—C28—H28A | 109.2 |
C16—C15—C14 | 120.1 (3) | N8—C28—H28A | 109.2 |
C15—C16—C17 | 120.6 (3) | N6—C28—H28B | 109.2 |
C18—C17—C16 | 119.5 (3) | N8—C28—H28B | 109.2 |
C17—C18—C13 | 121.5 (3) | H28A—C28—H28B | 107.9 |
N2—C19—N1 | 112.3 (2) | N6—C29—H29A | 109.0 |
N3—C20—N1 | 112.1 (2) | N7—C29—H29A | 109.0 |
N4—C21—N1 | 112.7 (2) | N6—C29—H29B | 109.0 |
N2—C22—N3 | 111.9 (2) | N7—C29—H29B | 109.0 |
N2—C23—N4 | 112.3 (2) | H29A—C29—H29B | 107.8 |
N4—C24—N3 | 112.7 (2) | N8—C30—H30A | 109.1 |
N8—C25—N5 | 112.4 (2) | N7—C30—H30A | 109.1 |
N7—C26—N5 | 112.6 (2) | N8—C30—H30B | 109.1 |
N6—C27—N5 | 112.4 (2) | N7—C30—H30B | 109.1 |
N6—C28—N8 | 112.2 (2) | H30A—C30—H30B | 107.8 |
O4—Cd1—O1—C1 | −175.6 (2) | Cd1—O5—C10—O4 | 1.0 (3) |
O1W—Cd1—O1—C1 | −1.1 (2) | Cd1—O5—C10—C11 | −177.3 (3) |
O2—Cd1—O1—C1 | 2.6 (2) | Cd1—O4—C10—O5 | −1.2 (3) |
N1—Cd1—O1—C1 | 93.3 (2) | Cd1—O4—C10—C11 | 177.3 (2) |
N5—Cd1—O1—C1 | −86.6 (2) | O5—C10—C11—C12 | 4.0 (5) |
O5—Cd1—O1—C1 | 176.3 (2) | O4—C10—C11—C12 | −174.5 (3) |
O4—Cd1—O2—C1 | 0.4 (2) | C10—C11—C12—C13 | 177.8 (3) |
O1W—Cd1—O2—C1 | 174.8 (2) | C11—C12—C13—C14 | 174.8 (3) |
O1—Cd1—O2—C1 | −2.6 (2) | C11—C12—C13—C18 | −6.0 (5) |
N1—Cd1—O2—C1 | −91.7 (2) | C18—C13—C14—O6 | 178.3 (3) |
N5—Cd1—O2—C1 | 85.3 (2) | C12—C13—C14—O6 | −2.5 (4) |
O5—Cd1—O2—C1 | −169.5 (2) | C18—C13—C14—C15 | −0.7 (4) |
O1W—Cd1—O4—C10 | 12.0 (2) | C12—C13—C14—C15 | 178.6 (3) |
O2—Cd1—O4—C10 | −175.7 (2) | O6—C14—C15—C16 | −179.1 (3) |
O1—Cd1—O4—C10 | −173.2 (2) | C13—C14—C15—C16 | −0.2 (5) |
N1—Cd1—O4—C10 | −83.8 (2) | C14—C15—C16—C17 | 0.9 (5) |
N5—Cd1—O4—C10 | 99.9 (2) | C15—C16—C17—C18 | −0.7 (6) |
O5—Cd1—O4—C10 | 0.6 (2) | C16—C17—C18—C13 | −0.2 (5) |
O4—Cd1—O5—C10 | −0.6 (2) | C14—C13—C18—C17 | 0.9 (5) |
O1W—Cd1—O5—C10 | −172.3 (2) | C12—C13—C18—C17 | −178.3 (3) |
O2—Cd1—O5—C10 | 171.9 (2) | C23—N2—C19—N1 | 58.9 (3) |
O1—Cd1—O5—C10 | 9.5 (2) | C22—N2—C19—N1 | −58.7 (3) |
N1—Cd1—O5—C10 | 93.6 (2) | C21—N1—C19—N2 | −57.7 (3) |
N5—Cd1—O5—C10 | −84.2 (2) | C20—N1—C19—N2 | 57.9 (3) |
O4—Cd1—N1—C21 | −62.7 (2) | Cd1—N1—C19—N2 | −178.0 (2) |
O1W—Cd1—N1—C21 | 163.8 (2) | C22—N3—C20—N1 | 59.1 (3) |
O2—Cd1—N1—C21 | 81.2 (2) | C24—N3—C20—N1 | −58.0 (3) |
O1—Cd1—N1—C21 | 26.7 (2) | C21—N1—C20—N3 | 57.5 (3) |
O5—Cd1—N1—C21 | −115.6 (2) | C19—N1—C20—N3 | −58.2 (3) |
O4—Cd1—N1—C19 | 58.3 (2) | Cd1—N1—C20—N3 | 172.9 (2) |
O1W—Cd1—N1—C19 | −75.3 (2) | C24—N4—C21—N1 | 58.5 (3) |
O2—Cd1—N1—C19 | −157.8 (2) | C23—N4—C21—N1 | −57.8 (3) |
O1—Cd1—N1—C19 | 147.7 (2) | C19—N1—C21—N4 | 57.3 (3) |
O5—Cd1—N1—C19 | 5.36 (18) | C20—N1—C21—N4 | −58.1 (3) |
O4—Cd1—N1—C20 | −178.9 (2) | Cd1—N1—C21—N4 | −175.6 (2) |
O1W—Cd1—N1—C20 | 47.6 (2) | C23—N2—C22—N3 | −58.4 (3) |
O2—Cd1—N1—C20 | −35.0 (2) | C19—N2—C22—N3 | 58.7 (3) |
O1—Cd1—N1—C20 | −89.5 (2) | C24—N3—C22—N2 | 58.2 (3) |
O5—Cd1—N1—C20 | 128.2 (2) | C20—N3—C22—N2 | −58.8 (3) |
O4—Cd1—N5—C26 | −164.7 (2) | C22—N2—C23—N4 | 58.2 (3) |
O1W—Cd1—N5—C26 | −31.3 (2) | C19—N2—C23—N4 | −59.4 (3) |
O2—Cd1—N5—C26 | 51.3 (2) | C24—N4—C23—N2 | −57.4 (3) |
O1—Cd1—N5—C26 | 105.8 (2) | C21—N4—C23—N2 | 58.8 (3) |
O5—Cd1—N5—C26 | −112.0 (2) | C21—N4—C24—N3 | −58.7 (3) |
O4—Cd1—N5—C25 | −44.8 (2) | C23—N4—C24—N3 | 57.6 (3) |
O1W—Cd1—N5—C25 | 88.6 (2) | C22—N3—C24—N4 | −58.2 (3) |
O2—Cd1—N5—C25 | 171.2 (2) | C20—N3—C24—N4 | 58.7 (3) |
O1—Cd1—N5—C25 | −134.3 (2) | C30—N8—C25—N5 | 58.3 (3) |
O5—Cd1—N5—C25 | 7.9 (2) | C28—N8—C25—N5 | −58.7 (3) |
O4—Cd1—N5—C27 | 75.3 (2) | C26—N5—C25—N8 | −57.6 (3) |
O1W—Cd1—N5—C27 | −151.4 (2) | C27—N5—C25—N8 | 57.9 (3) |
O2—Cd1—N5—C27 | −68.8 (2) | Cd1—N5—C25—N8 | −179.7 (2) |
O1—Cd1—N5—C27 | −14.2 (2) | C29—N7—C26—N5 | 57.8 (3) |
O5—Cd1—N5—C27 | 127.9 (2) | C30—N7—C26—N5 | −58.5 (3) |
Cd1—O2—C1—O1 | 4.9 (3) | C25—N5—C26—N7 | 57.9 (3) |
Cd1—O2—C1—C2 | −174.1 (2) | C27—N5—C26—N7 | −57.6 (3) |
Cd1—O1—C1—O2 | −4.7 (3) | Cd1—N5—C26—N7 | −179.9 (2) |
Cd1—O1—C1—C2 | 174.2 (2) | C29—N6—C27—N5 | −58.3 (3) |
O2—C1—C2—C3 | −0.4 (5) | C28—N6—C27—N5 | 58.9 (3) |
O1—C1—C2—C3 | −179.4 (3) | C26—N5—C27—N6 | 57.6 (3) |
C1—C2—C3—C4 | 177.0 (3) | C25—N5—C27—N6 | −57.8 (3) |
C2—C3—C4—C9 | −3.0 (5) | Cd1—N5—C27—N6 | 179.8 (2) |
C2—C3—C4—C5 | 178.2 (3) | C29—N6—C28—N8 | 57.6 (3) |
C9—C4—C5—O3 | −179.5 (2) | C27—N6—C28—N8 | −59.5 (3) |
C3—C4—C5—O3 | −0.6 (4) | C30—N8—C28—N6 | −57.4 (3) |
C9—C4—C5—C6 | 0.0 (4) | C25—N8—C28—N6 | 59.4 (3) |
C3—C4—C5—C6 | 178.9 (2) | C27—N6—C29—N7 | 58.7 (3) |
O3—C5—C6—C7 | 179.1 (3) | C28—N6—C29—N7 | −58.3 (3) |
C4—C5—C6—C7 | −0.3 (4) | C26—N7—C29—N6 | −58.3 (3) |
C5—C6—C7—C8 | 0.1 (5) | C30—N7—C29—N6 | 58.0 (3) |
C6—C7—C8—C9 | 0.4 (5) | C25—N8—C30—N7 | −58.9 (3) |
C7—C8—C9—C4 | −0.7 (5) | C28—N8—C30—N7 | 57.5 (3) |
C5—C4—C9—C8 | 0.5 (5) | C26—N7—C30—N8 | 58.8 (3) |
C3—C4—C9—C8 | −178.3 (3) | C29—N7—C30—N8 | −57.5 (3) |
Hydrogen-bond geometry (Å, º) top
D—H···A | D—H | H···A | D···A | D—H···A |
O3—H3O···N7i | 0.85 (1) | 1.99 (1) | 2.831 (3) | 176 (3) |
O6—H6O···O5ii | 0.85 (1) | 1.87 (1) | 2.701 (3) | 164 (4) |
O1W—H1W1···O2W | 0.85 (1) | 1.90 (1) | 2.735 (3) | 167 (2) |
O1W—H1W2···N3iii | 0.85 (1) | 1.98 (1) | 2.817 (3) | 168 (3) |
O2W—H2W1···O3W | 0.85 (1) | 2.01 (2) | 2.751 (5) | 145 (3) |
O2W—H2W2···N8iv | 0.85 (1) | 2.06 (1) | 2.892 (4) | 169 (3) |
O3W—H3W1···O1v | 0.86 (1) | 2.12 (6) | 2.812 (5) | 138 (7) |
O3W—H3W2···O4Wiv | 0.85 (1) | 2.12 (2) | 2.96 (1) | 168 (7) |
O3′—H3′1···O1v | 0.86 (1) | 2.07 (7) | 2.787 (7) | 141 (9) |
O4W—H4W1···O4 | 0.86 (1) | 1.86 (1) | 2.722 (5) | 176 (7) |
O4W—H4W2···N4vi | 0.86 (1) | 2.08 (1) | 2.929 (5) | 171 (6) |
Symmetry codes: (i) −x+2, −y+1, −z+2; (ii) −x, −y+1, −z+1; (iii) −x+1, −y+1, −z+2; (iv) −x+1, −y+1, −z+1; (v) −x+1, y−1/2, −z+3/2; (vi) x, −y+3/2, z−1/2. |
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