Supporting information
Crystallographic Information File (CIF) https://doi.org/10.1107/S1600536807040214/lh2456sup1.cif | |
Structure factor file (CIF format) https://doi.org/10.1107/S1600536807040214/lh2456Isup2.hkl |
CCDC reference: 660146
A solution of (2-Carboxymethyl-phenyl)-acetic acid(2 mmol,0.388 g), phenanthroline(3 mmol,0.594 g),cadmium chloride(3 mmol,0.37 g) in the mixture solution of ethanol-water. The mixture solution was stirred for 30 min at room temperature,then filtered. The filtrate were added to 30 ml sealed teflon-lined stainless steel vessels, and the teflon-lined stainless steel vessels was placed at 413 K vacuum case for 4 d under autogenous pressure. After cooled to room temperature, colorless crystals were produced(yield: 48.8%, based on Cd).
The crystal contains various partial occupancy solvent molecules, namely a 0.79 occupancy ethanol molecule and in addition to the two full occupancy water solvent molecules there are two more sites for water atoms adding to a further occupancy of 1.05. The H atoms of the partial occupancy water atoms were not located and were not included in the refinement. The contribution of these H atoms is included in the molecular formula.
H atoms boned to C and N atoms were positioned geometrically and refined in a riding-model approximation, with C—H distances of 0.95–0.99 Å, N—H distances of 0.92 Å, and with Uiso(H) = 1.2Ueq(C & N). The H atom of the partially occupied ethanol solvent was included in a calculated position with O—H = 0.84Å and Uiso(H) = 1.1Ueq(O). The H atoms of the water molecules were located in difference Fourier maps and were refined with a distance restraint of 0.84 (2)Å and their isotropic displacement parameters were refined.
Many complexes containing phenanthroline have been reported (e.g. Yam, et al.,1999; Harvey et al., 2000; Ding, et al.,2005) and these include dinuclear complexes containing phenanthroline bridged by carboxylate ligands (Tan, et al.,2006; Shi, et al.,2005). In this report we used phenanthroline, (2-Carboxymethyl-phenyl)-acetic acid and cadmium chloride to construct the title one-dimensional chain polymer.
The asymmetric unit contains two independent CdII atoms, two L2- ligands, three phenanthroline ligands, 3.05 H2O molecules and one partial occupancy C2H5OH molecule. The two CdII atoms have different coordination modes. Atom Cd1 is coordinated by four O atoms from two different L2- ligands, two N atoms from one phenanthroline ligand and by atom O9 from a water molecule, forming a distorted monocapped octahedral geometry. Atom Cd2 is coordinated by four N atoms from two different phenanthroline ligands and two O atoms from a two bridging L2-, ligands, forming a distorted octahedral geometry. The two independent CdII atoms are bridged by a L2- ligand forming a one-dimensional chain structure. Part of the one dimensional chain structure is shown in Fig. 1. A l l bond distances and angles are as expected. In the crystal structure, intermolecular O—H···O hydrogen bonds connect molecules to form a two-dimensional network (Fig. 2).
For related literature, see: Yam et al. (1999); Harvey et al. (2000); Ding et al. (2005); Shi et al. (2005); Tan et al. (2006).
Data collection: RAPID-AUTO (Rigaku, 2004); cell refinement: RAPID-AUTO (Rigaku, 2004); data reduction: RAPID-AUTO (Rigaku, 2004); program(s) used to solve structure: SHELXS97 (Sheldrick, 1997a); program(s) used to refine structure: SHELXL97 (Sheldrick, 1997a); molecular graphics: SHELXTL (Sheldrick, 1997b); software used to prepare material for publication: SHELXTL (Sheldrick, 1997b).
[Cd2(C10H8O4)2(C12H8N2)3(H2O)]·0.79C2H6O·3.05H2O | Z = 2 |
Mr = 1257.16 | F(000) = 1274 |
Triclinic, P1 | Dx = 1.625 Mg m−3 |
Hall symbol: -P 1 | Mo Kα radiation, λ = 0.71073 Å |
a = 12.6568 (2) Å | Cell parameters from 21913 reflections |
b = 14.7729 (3) Å | θ = 3.0–27.5° |
c = 15.0674 (3) Å | µ = 0.90 mm−1 |
α = 68.710 (1)° | T = 153 K |
β = 83.896 (1)° | Block, colorless |
γ = 78.303 (1)° | 0.20 × 0.16 × 0.11 mm |
V = 2568.84 (9) Å3 |
Rigaku R-AXIS RAPID diffractometer | 10285 reflections with I > 2σ(I) |
Radiation source: Rotating Anode | Rint = 0.016 |
Graphite monochromator | θmax = 27.5°, θmin = 3.0° |
ω scans | h = −16→16 |
25428 measured reflections | k = −19→19 |
11681 independent reflections | l = −19→19 |
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)] = 0.025 | H atoms treated by a mixture of independent and constrained refinement |
wR(F2) = 0.093 | w = 1/[σ2(Fo2) + (0.0676P)2 + 0.93P] where P = (Fo2 + 2Fc2)/3 |
S = 1.01 | (Δ/σ)max = 0.001 |
11681 reflections | Δρmax = 0.82 e Å−3 |
744 parameters | Δρmin = −0.85 e Å−3 |
9 restraints | Extinction correction: SHELXL97 (Sheldrick, 1997a), Fc*=kFc[1+0.001xFc2λ3/sin(2θ)]-1/4 |
Primary atom site location: structure-invariant direct methods | Extinction coefficient: 0.0017 (3) |
[Cd2(C10H8O4)2(C12H8N2)3(H2O)]·0.79C2H6O·3.05H2O | γ = 78.303 (1)° |
Mr = 1257.16 | V = 2568.84 (9) Å3 |
Triclinic, P1 | Z = 2 |
a = 12.6568 (2) Å | Mo Kα radiation |
b = 14.7729 (3) Å | µ = 0.90 mm−1 |
c = 15.0674 (3) Å | T = 153 K |
α = 68.710 (1)° | 0.20 × 0.16 × 0.11 mm |
β = 83.896 (1)° |
Rigaku R-AXIS RAPID diffractometer | 10285 reflections with I > 2σ(I) |
25428 measured reflections | Rint = 0.016 |
11681 independent reflections |
R[F2 > 2σ(F2)] = 0.025 | 9 restraints |
wR(F2) = 0.093 | H atoms treated by a mixture of independent and constrained refinement |
S = 1.01 | Δρmax = 0.82 e Å−3 |
11681 reflections | Δρmin = −0.85 e Å−3 |
744 parameters |
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 | Occ. (<1) | |
Cd1 | 0.689294 (11) | 0.421799 (11) | 0.608438 (11) | 0.02153 (6) | |
Cd2 | 0.053959 (11) | 0.793489 (11) | 0.773349 (10) | 0.02087 (6) | |
O1 | 0.49865 (13) | 0.49043 (12) | 0.63061 (12) | 0.0290 (3) | |
O2 | 0.61249 (13) | 0.45434 (12) | 0.74444 (12) | 0.0296 (3) | |
O3 | 0.22400 (12) | 0.79301 (12) | 0.71617 (11) | 0.0253 (3) | |
O4 | 0.20909 (13) | 0.70938 (13) | 0.62286 (13) | 0.0324 (4) | |
O5 | 0.78141 (15) | 0.26364 (13) | 0.67143 (16) | 0.0418 (5) | |
O6 | 0.60941 (16) | 0.26266 (14) | 0.66945 (18) | 0.0471 (5) | |
O7 | 0.98151 (13) | −0.07694 (12) | 0.65385 (12) | 0.0287 (3) | |
O8 | 1.02815 (15) | 0.03295 (15) | 0.70485 (15) | 0.0399 (4) | |
O9 | 0.68968 (15) | 0.41970 (15) | 0.45880 (14) | 0.0365 (4) | |
N1 | 0.85996 (15) | 0.45969 (14) | 0.61669 (13) | 0.0243 (4) | |
N2 | 0.69086 (15) | 0.59301 (14) | 0.51893 (14) | 0.0253 (4) | |
N3 | −0.08039 (15) | 0.72071 (13) | 0.74069 (13) | 0.0233 (4) | |
N4 | 0.09081 (15) | 0.61537 (14) | 0.85106 (14) | 0.0249 (4) | |
N5 | −0.08516 (17) | 0.84413 (15) | 0.88096 (15) | 0.0304 (4) | |
N6 | 0.13219 (18) | 0.80485 (15) | 0.90742 (14) | 0.0301 (4) | |
C1 | 0.51985 (18) | 0.48876 (16) | 0.71056 (17) | 0.0249 (4) | |
C2 | 0.43193 (19) | 0.52965 (17) | 0.77025 (17) | 0.0293 (5) | |
H2A | 0.3641 | 0.5545 | 0.7351 | 0.035* | |
H2B | 0.4186 | 0.4758 | 0.8304 | 0.035* | |
C3 | 0.46247 (17) | 0.61267 (18) | 0.79344 (17) | 0.0274 (5) | |
C4 | 0.5117 (2) | 0.5908 (2) | 0.8791 (2) | 0.0435 (7) | |
H4 | 0.5267 | 0.5242 | 0.9213 | 0.052* | |
C5 | 0.5390 (2) | 0.6647 (3) | 0.9037 (3) | 0.0588 (11) | |
H5 | 0.5712 | 0.6488 | 0.9629 | 0.071* | |
C6 | 0.5195 (2) | 0.7610 (3) | 0.8422 (3) | 0.0551 (10) | |
H6 | 0.5383 | 0.8118 | 0.8587 | 0.066* | |
C7 | 0.47280 (19) | 0.7833 (2) | 0.7570 (2) | 0.0399 (6) | |
H7 | 0.4602 | 0.8499 | 0.7146 | 0.048* | |
C8 | 0.44330 (16) | 0.71033 (17) | 0.73112 (17) | 0.0264 (5) | |
C9 | 0.38516 (17) | 0.73898 (17) | 0.64020 (16) | 0.0258 (4) | |
H9A | 0.4114 | 0.6891 | 0.6097 | 0.031* | |
H9B | 0.4012 | 0.8033 | 0.5957 | 0.031* | |
C10 | 0.26244 (17) | 0.74676 (16) | 0.65953 (15) | 0.0232 (4) | |
C11 | 0.7039 (2) | 0.21884 (17) | 0.68541 (18) | 0.0291 (5) | |
C12 | 0.7269 (2) | 0.10595 (17) | 0.72501 (18) | 0.0295 (5) | |
H12A | 0.8017 | 0.0827 | 0.7475 | 0.035* | |
H12B | 0.6771 | 0.0819 | 0.7802 | 0.035* | |
C13 | 0.71312 (17) | 0.06376 (15) | 0.64981 (16) | 0.0237 (4) | |
C14 | 0.61860 (18) | 0.02941 (17) | 0.65013 (17) | 0.0283 (5) | |
H14 | 0.5647 | 0.0302 | 0.6989 | 0.034* | |
C15 | 0.60195 (19) | −0.00598 (17) | 0.58005 (18) | 0.0299 (5) | |
H15 | 0.5368 | −0.0288 | 0.5809 | 0.036* | |
C16 | 0.6798 (2) | −0.00801 (17) | 0.50930 (18) | 0.0306 (5) | |
H16 | 0.6682 | −0.0315 | 0.4608 | 0.037* | |
C17 | 0.77596 (19) | 0.02477 (17) | 0.50944 (16) | 0.0280 (5) | |
H17 | 0.8300 | 0.0227 | 0.4610 | 0.034* | |
C18 | 0.79385 (17) | 0.06027 (15) | 0.57926 (16) | 0.0244 (4) | |
C19 | 0.90071 (18) | 0.09020 (16) | 0.58026 (18) | 0.0282 (5) | |
H19A | 0.8879 | 0.1513 | 0.5956 | 0.034* | |
H19B | 0.9360 | 0.1047 | 0.5160 | 0.034* | |
C20 | 0.97616 (17) | 0.00966 (17) | 0.65299 (17) | 0.0260 (4) | |
C21 | 0.94063 (19) | 0.39586 (18) | 0.66638 (17) | 0.0296 (5) | |
H21 | 0.9310 | 0.3296 | 0.6995 | 0.035* | |
C22 | 1.03977 (19) | 0.4216 (2) | 0.67239 (18) | 0.0340 (5) | |
H22 | 1.0952 | 0.3738 | 0.7097 | 0.041* | |
C23 | 1.05560 (19) | 0.5164 (2) | 0.62381 (18) | 0.0344 (5) | |
H23 | 1.1221 | 0.5352 | 0.6271 | 0.041* | |
C24 | 0.97165 (19) | 0.58586 (19) | 0.56868 (17) | 0.0295 (5) | |
C25 | 0.9833 (2) | 0.6857 (2) | 0.5142 (2) | 0.0354 (5) | |
H25 | 1.0487 | 0.7071 | 0.5157 | 0.042* | |
C26 | 0.9022 (2) | 0.74954 (19) | 0.4609 (2) | 0.0358 (5) | |
H26 | 0.9125 | 0.8146 | 0.4230 | 0.043* | |
C27 | 0.8011 (2) | 0.72061 (17) | 0.46086 (17) | 0.0290 (5) | |
C28 | 0.7118 (2) | 0.78729 (18) | 0.41059 (19) | 0.0359 (5) | |
H28 | 0.7185 | 0.8533 | 0.3726 | 0.043* | |
C29 | 0.6160 (2) | 0.7556 (2) | 0.4174 (2) | 0.0391 (6) | |
H29 | 0.5549 | 0.7998 | 0.3856 | 0.047* | |
C30 | 0.6090 (2) | 0.65751 (19) | 0.47168 (19) | 0.0320 (5) | |
H30 | 0.5424 | 0.6361 | 0.4748 | 0.038* | |
C31 | 0.78632 (18) | 0.62377 (16) | 0.51401 (16) | 0.0237 (4) | |
C32 | 0.87444 (17) | 0.55413 (17) | 0.56788 (16) | 0.0237 (4) | |
C33 | −0.16356 (18) | 0.77187 (17) | 0.68545 (16) | 0.0263 (4) | |
H33 | −0.1626 | 0.8391 | 0.6479 | 0.032* | |
C34 | −0.25225 (19) | 0.73094 (19) | 0.68023 (18) | 0.0297 (5) | |
H34 | −0.3102 | 0.7702 | 0.6405 | 0.036* | |
C35 | −0.25462 (19) | 0.63431 (19) | 0.73267 (17) | 0.0292 (5) | |
H35 | −0.3149 | 0.6058 | 0.7308 | 0.035* | |
C36 | −0.16710 (19) | 0.57734 (17) | 0.78951 (16) | 0.0262 (4) | |
C37 | −0.1615 (2) | 0.47415 (19) | 0.84237 (18) | 0.0329 (5) | |
H37 | −0.2200 | 0.4428 | 0.8422 | 0.040* | |
C38 | −0.0735 (2) | 0.42123 (18) | 0.89247 (18) | 0.0349 (5) | |
H38 | −0.0706 | 0.3526 | 0.9262 | 0.042* | |
C39 | 0.0153 (2) | 0.46562 (17) | 0.89621 (17) | 0.0294 (5) | |
C40 | 0.1087 (2) | 0.41219 (18) | 0.9472 (2) | 0.0383 (6) | |
H40 | 0.1154 | 0.3431 | 0.9805 | 0.046* | |
C41 | 0.1895 (2) | 0.4603 (2) | 0.9484 (2) | 0.0391 (6) | |
H41 | 0.2532 | 0.4250 | 0.9820 | 0.047* | |
C42 | 0.17758 (19) | 0.56245 (19) | 0.89955 (18) | 0.0320 (5) | |
H42 | 0.2342 | 0.5952 | 0.9013 | 0.038* | |
C43 | 0.01141 (18) | 0.56768 (16) | 0.84802 (15) | 0.0232 (4) | |
C44 | −0.08122 (17) | 0.62421 (16) | 0.79162 (15) | 0.0221 (4) | |
C45 | −0.1902 (2) | 0.8629 (2) | 0.8677 (2) | 0.0384 (6) | |
H45 | −0.2145 | 0.8535 | 0.8146 | 0.046* | |
C46 | −0.2673 (3) | 0.8960 (2) | 0.9283 (2) | 0.0487 (7) | |
H46 | −0.3421 | 0.9087 | 0.9166 | 0.058* | |
C47 | −0.2321 (3) | 0.9095 (3) | 1.0047 (2) | 0.0544 (8) | |
H47 | −0.2829 | 0.9325 | 1.0463 | 0.065* | |
C48 | −0.1213 (3) | 0.8896 (2) | 1.0217 (2) | 0.0448 (7) | |
C49 | −0.0793 (3) | 0.8993 (3) | 1.1015 (2) | 0.0560 (9) | |
H49 | −0.1279 | 0.9225 | 1.1443 | 0.067* | |
C50 | 0.0272 (3) | 0.8765 (3) | 1.1178 (2) | 0.0528 (8) | |
H50 | 0.0526 | 0.8825 | 1.1722 | 0.063* | |
C51 | 0.1025 (3) | 0.8431 (2) | 1.0527 (2) | 0.0421 (6) | |
C52 | 0.2130 (3) | 0.8170 (3) | 1.0670 (2) | 0.0517 (8) | |
H52 | 0.2413 | 0.8204 | 1.1214 | 0.062* | |
C53 | 0.2808 (3) | 0.7866 (3) | 1.0024 (2) | 0.0490 (7) | |
H53 | 0.3564 | 0.7687 | 1.0113 | 0.059* | |
C54 | 0.2367 (2) | 0.7823 (2) | 0.92304 (19) | 0.0370 (6) | |
H54 | 0.2844 | 0.7621 | 0.8780 | 0.044* | |
C55 | 0.0641 (2) | 0.83559 (17) | 0.97167 (17) | 0.0307 (5) | |
C56 | −0.0501 (2) | 0.85692 (17) | 0.95655 (18) | 0.0325 (5) | |
O11 | 1.24607 (16) | −0.02220 (14) | 0.72639 (15) | 0.0380 (4) | |
O12 | −0.3976 (3) | 0.9918 (3) | 1.1718 (3) | 0.0813 (9) | |
O13 | −0.4695 (4) | 1.0800 (4) | 0.9987 (4) | 0.112 (2) | 0.846 (12) |
O10 | −0.4680 (3) | 0.8163 (3) | 1.1848 (3) | 0.0728 (10) | 0.792 (4) |
H10 | −0.5096 | 0.7944 | 1.2318 | 0.080* | 0.792 (4) |
C58 | −0.4086 (5) | 0.7355 (4) | 1.1573 (5) | 0.115 (3) | 0.792 (4) |
H58A | −0.3846 | 0.7615 | 1.0895 | 0.137* | 0.792 (4) |
H58B | −0.4571 | 0.6885 | 1.1636 | 0.137* | 0.792 (4) |
C57 | −0.3117 (5) | 0.6815 (5) | 1.2168 (6) | 0.121 (3) | 0.792 (4) |
H57A | −0.2627 | 0.7274 | 1.2099 | 0.133* | 0.792 (4) |
H57B | −0.2741 | 0.6278 | 1.1953 | 0.133* | 0.792 (4) |
H57C | −0.3351 | 0.6541 | 1.2838 | 0.133* | 0.792 (4) |
O10W | −0.4956 (12) | 0.7129 (10) | 1.1176 (10) | 0.0728 (10) | 0.208 (4) |
H9AO | 0.720 (2) | 0.3728 (16) | 0.444 (2) | 0.035 (8)* | |
H9BO | 0.6380 (19) | 0.454 (2) | 0.428 (2) | 0.046 (9)* | |
H01A | 1.1821 (14) | 0.001 (3) | 0.716 (3) | 0.090 (16)* | |
H01B | 1.255 (3) | −0.0762 (14) | 0.720 (3) | 0.055 (10)* | |
H02A | −0.388 (3) | 0.9327 (8) | 1.194 (2) | 0.035 (9)* | |
H02B | −0.363 (4) | 1.013 (4) | 1.201 (4) | 0.12 (2)* |
U11 | U22 | U33 | U12 | U13 | U23 | |
Cd1 | 0.02012 (9) | 0.01939 (9) | 0.02826 (10) | −0.00338 (6) | −0.00033 (6) | −0.01231 (7) |
Cd2 | 0.02013 (9) | 0.01867 (9) | 0.02286 (9) | −0.00310 (6) | 0.00037 (6) | −0.00666 (6) |
O1 | 0.0257 (7) | 0.0303 (8) | 0.0330 (9) | −0.0016 (7) | −0.0018 (6) | −0.0150 (7) |
O2 | 0.0261 (8) | 0.0292 (8) | 0.0339 (9) | 0.0007 (7) | −0.0021 (6) | −0.0142 (7) |
O3 | 0.0217 (7) | 0.0269 (8) | 0.0292 (8) | −0.0026 (6) | 0.0023 (6) | −0.0137 (7) |
O4 | 0.0250 (8) | 0.0390 (9) | 0.0403 (10) | −0.0025 (7) | −0.0031 (7) | −0.0234 (8) |
O5 | 0.0389 (10) | 0.0234 (8) | 0.0653 (13) | −0.0052 (8) | −0.0126 (9) | −0.0155 (9) |
O6 | 0.0359 (10) | 0.0292 (9) | 0.0783 (15) | 0.0020 (8) | −0.0095 (10) | −0.0233 (10) |
O7 | 0.0275 (8) | 0.0199 (7) | 0.0335 (9) | −0.0013 (6) | −0.0038 (7) | −0.0042 (7) |
O8 | 0.0361 (9) | 0.0392 (10) | 0.0492 (11) | −0.0002 (8) | −0.0122 (8) | −0.0218 (9) |
O9 | 0.0324 (9) | 0.0444 (10) | 0.0418 (10) | 0.0077 (8) | −0.0110 (8) | −0.0307 (9) |
N1 | 0.0229 (8) | 0.0278 (9) | 0.0242 (9) | −0.0046 (7) | −0.0009 (7) | −0.0112 (8) |
N2 | 0.0256 (9) | 0.0238 (9) | 0.0289 (10) | −0.0055 (7) | −0.0011 (7) | −0.0112 (8) |
N3 | 0.0236 (8) | 0.0215 (8) | 0.0251 (9) | −0.0042 (7) | −0.0017 (7) | −0.0080 (7) |
N4 | 0.0245 (9) | 0.0233 (9) | 0.0244 (9) | −0.0007 (7) | 0.0000 (7) | −0.0075 (8) |
N5 | 0.0377 (11) | 0.0227 (9) | 0.0291 (10) | −0.0059 (8) | 0.0061 (8) | −0.0089 (8) |
N6 | 0.0409 (11) | 0.0250 (9) | 0.0253 (10) | −0.0108 (8) | 0.0032 (8) | −0.0082 (8) |
C1 | 0.0258 (10) | 0.0164 (9) | 0.0318 (11) | −0.0054 (8) | 0.0040 (9) | −0.0081 (9) |
C2 | 0.0290 (11) | 0.0248 (11) | 0.0314 (12) | −0.0053 (9) | 0.0081 (9) | −0.0089 (9) |
C3 | 0.0214 (10) | 0.0338 (12) | 0.0288 (11) | −0.0002 (9) | 0.0024 (8) | −0.0167 (10) |
C4 | 0.0361 (13) | 0.0577 (18) | 0.0336 (13) | 0.0140 (13) | −0.0068 (11) | −0.0226 (13) |
C5 | 0.0310 (13) | 0.105 (3) | 0.059 (2) | 0.0126 (17) | −0.0159 (13) | −0.060 (2) |
C6 | 0.0233 (12) | 0.083 (2) | 0.089 (3) | −0.0018 (14) | −0.0059 (14) | −0.069 (2) |
C7 | 0.0214 (10) | 0.0419 (14) | 0.0691 (19) | −0.0071 (10) | 0.0031 (11) | −0.0348 (14) |
C8 | 0.0162 (9) | 0.0288 (11) | 0.0392 (13) | −0.0021 (8) | 0.0024 (8) | −0.0195 (10) |
C9 | 0.0218 (10) | 0.0245 (10) | 0.0293 (11) | −0.0029 (8) | 0.0049 (8) | −0.0097 (9) |
C10 | 0.0230 (9) | 0.0197 (9) | 0.0239 (10) | −0.0006 (8) | 0.0010 (8) | −0.0065 (8) |
C11 | 0.0337 (12) | 0.0251 (11) | 0.0328 (12) | −0.0030 (9) | −0.0051 (9) | −0.0153 (10) |
C12 | 0.0342 (12) | 0.0249 (11) | 0.0312 (12) | −0.0048 (9) | −0.0037 (9) | −0.0116 (10) |
C13 | 0.0255 (10) | 0.0166 (9) | 0.0277 (11) | −0.0021 (8) | −0.0037 (8) | −0.0066 (8) |
C14 | 0.0244 (10) | 0.0231 (10) | 0.0342 (12) | −0.0033 (9) | 0.0002 (9) | −0.0072 (9) |
C15 | 0.0281 (11) | 0.0254 (11) | 0.0358 (12) | −0.0077 (9) | −0.0075 (9) | −0.0069 (10) |
C16 | 0.0371 (12) | 0.0237 (11) | 0.0319 (12) | −0.0020 (9) | −0.0119 (10) | −0.0098 (10) |
C17 | 0.0301 (11) | 0.0227 (10) | 0.0264 (11) | 0.0004 (9) | 0.0002 (9) | −0.0062 (9) |
C18 | 0.0222 (9) | 0.0153 (9) | 0.0315 (11) | −0.0014 (8) | −0.0034 (8) | −0.0034 (8) |
C19 | 0.0251 (10) | 0.0185 (10) | 0.0360 (12) | −0.0054 (8) | −0.0017 (9) | −0.0028 (9) |
C20 | 0.0200 (9) | 0.0251 (10) | 0.0293 (11) | −0.0044 (8) | 0.0027 (8) | −0.0062 (9) |
C21 | 0.0275 (11) | 0.0306 (11) | 0.0306 (12) | −0.0050 (9) | −0.0018 (9) | −0.0106 (10) |
C22 | 0.0247 (11) | 0.0445 (14) | 0.0332 (12) | −0.0025 (10) | −0.0035 (9) | −0.0152 (11) |
C23 | 0.0231 (10) | 0.0506 (15) | 0.0350 (13) | −0.0109 (10) | 0.0033 (9) | −0.0203 (12) |
C24 | 0.0271 (11) | 0.0372 (13) | 0.0289 (11) | −0.0108 (10) | 0.0054 (9) | −0.0160 (10) |
C25 | 0.0323 (12) | 0.0377 (13) | 0.0430 (14) | −0.0183 (11) | 0.0055 (10) | −0.0178 (12) |
C26 | 0.0435 (14) | 0.0293 (12) | 0.0394 (14) | −0.0183 (11) | 0.0058 (11) | −0.0134 (11) |
C27 | 0.0342 (12) | 0.0254 (11) | 0.0313 (12) | −0.0094 (9) | 0.0040 (9) | −0.0137 (10) |
C28 | 0.0466 (14) | 0.0212 (11) | 0.0379 (13) | −0.0061 (10) | −0.0002 (11) | −0.0083 (10) |
C29 | 0.0366 (13) | 0.0293 (12) | 0.0463 (15) | 0.0000 (11) | −0.0068 (11) | −0.0091 (12) |
C30 | 0.0278 (11) | 0.0283 (12) | 0.0382 (13) | −0.0026 (10) | −0.0049 (10) | −0.0099 (10) |
C31 | 0.0271 (10) | 0.0242 (10) | 0.0241 (10) | −0.0062 (8) | 0.0013 (8) | −0.0134 (9) |
C32 | 0.0242 (10) | 0.0279 (11) | 0.0242 (10) | −0.0094 (9) | 0.0022 (8) | −0.0136 (9) |
C33 | 0.0272 (10) | 0.0224 (10) | 0.0279 (11) | −0.0010 (9) | −0.0036 (8) | −0.0083 (9) |
C34 | 0.0245 (10) | 0.0342 (12) | 0.0324 (12) | −0.0010 (9) | −0.0042 (9) | −0.0155 (10) |
C35 | 0.0261 (10) | 0.0359 (12) | 0.0323 (12) | −0.0092 (10) | 0.0015 (9) | −0.0185 (10) |
C36 | 0.0328 (11) | 0.0267 (11) | 0.0229 (10) | −0.0110 (9) | 0.0040 (8) | −0.0113 (9) |
C37 | 0.0427 (13) | 0.0299 (12) | 0.0309 (12) | −0.0175 (10) | 0.0025 (10) | −0.0112 (10) |
C38 | 0.0518 (15) | 0.0201 (10) | 0.0315 (12) | −0.0128 (10) | 0.0007 (11) | −0.0048 (9) |
C39 | 0.0396 (12) | 0.0207 (10) | 0.0265 (11) | −0.0043 (9) | 0.0000 (9) | −0.0075 (9) |
C40 | 0.0480 (15) | 0.0199 (11) | 0.0378 (14) | 0.0028 (10) | −0.0048 (11) | −0.0029 (10) |
C41 | 0.0354 (13) | 0.0343 (13) | 0.0387 (14) | 0.0091 (11) | −0.0084 (11) | −0.0085 (11) |
C42 | 0.0253 (11) | 0.0318 (12) | 0.0360 (13) | 0.0007 (10) | −0.0035 (9) | −0.0107 (10) |
C43 | 0.0277 (10) | 0.0206 (10) | 0.0200 (10) | −0.0025 (8) | 0.0021 (8) | −0.0075 (8) |
C44 | 0.0265 (10) | 0.0209 (9) | 0.0203 (10) | −0.0054 (8) | 0.0016 (8) | −0.0089 (8) |
C45 | 0.0406 (14) | 0.0369 (13) | 0.0382 (14) | −0.0075 (11) | 0.0071 (11) | −0.0159 (12) |
C46 | 0.0420 (15) | 0.0547 (18) | 0.0521 (18) | −0.0080 (14) | 0.0146 (13) | −0.0268 (15) |
C47 | 0.0562 (18) | 0.060 (2) | 0.0553 (19) | −0.0157 (16) | 0.0265 (15) | −0.0350 (17) |
C48 | 0.0592 (18) | 0.0409 (15) | 0.0430 (15) | −0.0206 (14) | 0.0193 (13) | −0.0246 (13) |
C49 | 0.076 (2) | 0.065 (2) | 0.0465 (17) | −0.0284 (18) | 0.0256 (16) | −0.0413 (17) |
C50 | 0.077 (2) | 0.061 (2) | 0.0393 (16) | −0.0317 (18) | 0.0136 (15) | −0.0335 (15) |
C51 | 0.0629 (18) | 0.0391 (14) | 0.0341 (14) | −0.0238 (13) | 0.0078 (12) | −0.0191 (12) |
C52 | 0.066 (2) | 0.065 (2) | 0.0375 (15) | −0.0264 (17) | −0.0035 (14) | −0.0253 (15) |
C53 | 0.0491 (16) | 0.065 (2) | 0.0400 (16) | −0.0140 (15) | −0.0048 (13) | −0.0233 (15) |
C54 | 0.0410 (13) | 0.0420 (14) | 0.0295 (12) | −0.0111 (12) | 0.0003 (10) | −0.0128 (11) |
C55 | 0.0483 (14) | 0.0223 (10) | 0.0256 (11) | −0.0158 (10) | 0.0070 (10) | −0.0104 (9) |
C56 | 0.0494 (14) | 0.0226 (11) | 0.0285 (12) | −0.0154 (10) | 0.0106 (10) | −0.0111 (9) |
O11 | 0.0382 (10) | 0.0286 (9) | 0.0483 (11) | −0.0083 (8) | 0.0015 (8) | −0.0143 (8) |
O12 | 0.088 (2) | 0.087 (2) | 0.100 (2) | −0.0421 (19) | 0.0266 (18) | −0.065 (2) |
O13 | 0.098 (3) | 0.112 (4) | 0.133 (4) | −0.023 (3) | −0.035 (3) | −0.039 (3) |
O10 | 0.083 (2) | 0.067 (2) | 0.073 (2) | −0.0356 (18) | 0.0166 (18) | −0.0234 (18) |
C58 | 0.165 (8) | 0.113 (6) | 0.091 (5) | −0.092 (6) | 0.021 (5) | −0.036 (5) |
C57 | 0.088 (5) | 0.176 (9) | 0.155 (8) | −0.045 (5) | 0.036 (5) | −0.122 (7) |
O10W | 0.083 (2) | 0.067 (2) | 0.073 (2) | −0.0356 (18) | 0.0166 (18) | −0.0234 (18) |
Cd1—O9 | 2.2656 (18) | C21—C22 | 1.404 (3) |
Cd1—O5 | 2.2891 (18) | C21—H21 | 0.9500 |
Cd1—O2 | 2.3404 (16) | C22—C23 | 1.369 (4) |
Cd1—N1 | 2.3649 (19) | C22—H22 | 0.9500 |
Cd1—N2 | 2.399 (2) | C23—C24 | 1.414 (3) |
Cd1—O1 | 2.4586 (15) | C23—H23 | 0.9500 |
Cd1—O6 | 2.567 (2) | C24—C32 | 1.405 (3) |
Cd1—C1 | 2.737 (2) | C24—C25 | 1.433 (4) |
Cd2—O7i | 2.2098 (16) | C25—C26 | 1.349 (4) |
Cd2—O3 | 2.2312 (15) | C25—H25 | 0.9500 |
Cd2—N3 | 2.3650 (19) | C26—C27 | 1.430 (4) |
Cd2—N6 | 2.414 (2) | C26—H26 | 0.9500 |
Cd2—N4 | 2.4277 (19) | C27—C31 | 1.403 (3) |
Cd2—N5 | 2.455 (2) | C27—C28 | 1.417 (4) |
O1—C1 | 1.252 (3) | C28—C29 | 1.367 (4) |
O2—C1 | 1.261 (3) | C28—H28 | 0.9500 |
O3—C10 | 1.278 (3) | C29—C30 | 1.397 (4) |
O4—C10 | 1.232 (3) | C29—H29 | 0.9500 |
O5—C11 | 1.251 (3) | C30—H30 | 0.9500 |
O6—C11 | 1.241 (3) | C31—C32 | 1.443 (3) |
O7—C20 | 1.263 (3) | C33—C34 | 1.400 (3) |
O7—Cd2ii | 2.2099 (16) | C33—H33 | 0.9500 |
O8—C20 | 1.248 (3) | C34—C35 | 1.362 (4) |
O9—H9AO | 0.81 (3) | C34—H34 | 0.9500 |
O9—H9BO | 0.81 (3) | C35—C36 | 1.403 (3) |
N1—C21 | 1.324 (3) | C35—H35 | 0.9500 |
N1—C32 | 1.360 (3) | C36—C44 | 1.411 (3) |
N2—C30 | 1.324 (3) | C36—C37 | 1.432 (3) |
N2—C31 | 1.360 (3) | C37—C38 | 1.349 (4) |
N3—C33 | 1.334 (3) | C37—H37 | 0.9500 |
N3—C44 | 1.353 (3) | C38—C39 | 1.427 (4) |
N4—C42 | 1.326 (3) | C38—H38 | 0.9500 |
N4—C43 | 1.352 (3) | C39—C43 | 1.409 (3) |
N5—C45 | 1.324 (4) | C39—C40 | 1.409 (4) |
N5—C56 | 1.352 (3) | C40—C41 | 1.364 (4) |
N6—C54 | 1.322 (3) | C40—H40 | 0.9500 |
N6—C55 | 1.367 (3) | C41—C42 | 1.402 (4) |
C1—C2 | 1.524 (3) | C41—H41 | 0.9500 |
C2—C3 | 1.519 (3) | C42—H42 | 0.9500 |
C2—H2A | 0.9900 | C43—C44 | 1.447 (3) |
C2—H2B | 0.9900 | C45—C46 | 1.402 (4) |
C3—C8 | 1.394 (3) | C45—H45 | 0.9500 |
C3—C4 | 1.395 (3) | C46—C47 | 1.369 (5) |
C4—C5 | 1.387 (5) | C46—H46 | 0.9500 |
C4—H4 | 0.9500 | C47—C48 | 1.406 (5) |
C5—C6 | 1.376 (6) | C47—H47 | 0.9500 |
C5—H5 | 0.9500 | C48—C56 | 1.410 (3) |
C6—C7 | 1.372 (5) | C48—C49 | 1.428 (5) |
C6—H6 | 0.9500 | C49—C50 | 1.348 (5) |
C7—C8 | 1.398 (3) | C49—H49 | 0.9500 |
C7—H7 | 0.9500 | C50—C51 | 1.441 (4) |
C8—C9 | 1.505 (3) | C50—H50 | 0.9500 |
C9—C10 | 1.538 (3) | C51—C52 | 1.392 (5) |
C9—H9A | 0.9900 | C51—C55 | 1.409 (4) |
C9—H9B | 0.9900 | C52—C53 | 1.367 (4) |
C11—C12 | 1.529 (3) | C52—H52 | 0.9500 |
C12—C13 | 1.517 (3) | C53—C54 | 1.399 (4) |
C12—H12A | 0.9900 | C53—H53 | 0.9500 |
C12—H12B | 0.9900 | C54—H54 | 0.9500 |
C13—C14 | 1.390 (3) | C55—C56 | 1.439 (4) |
C13—C18 | 1.401 (3) | O11—H01A | 0.82 (3) |
C14—C15 | 1.388 (3) | O11—H01B | 0.82 (3) |
C14—H14 | 0.9500 | O12—O13 | 2.624 (6) |
C15—C16 | 1.377 (4) | O12—H02A | 0.80 (3) |
C15—H15 | 0.9500 | O12—H02B | 0.83 (6) |
C16—C17 | 1.399 (4) | O10—C58 | 1.446 (3) |
C16—H16 | 0.9500 | O10—H10 | 0.8400 |
C17—C18 | 1.390 (3) | C58—C57 | 1.504 (3) |
C17—H17 | 0.9500 | C58—H58A | 0.9900 |
C18—C19 | 1.509 (3) | C58—H58B | 0.9900 |
C19—C20 | 1.531 (3) | C57—H57A | 0.9800 |
C19—H19A | 0.9900 | C57—H57B | 0.9800 |
C19—H19B | 0.9900 | C57—H57C | 0.9800 |
O9—Cd1—O5 | 94.96 (7) | C16—C17—H17 | 119.4 |
O9—Cd1—O2 | 155.26 (6) | C17—C18—C13 | 118.9 (2) |
O5—Cd1—O2 | 102.44 (7) | C17—C18—C19 | 119.8 (2) |
O9—Cd1—N1 | 103.79 (7) | C13—C18—C19 | 121.3 (2) |
O5—Cd1—N1 | 81.95 (7) | C18—C19—C20 | 112.13 (18) |
O2—Cd1—N1 | 96.01 (6) | C18—C19—H19A | 109.2 |
O9—Cd1—N2 | 80.43 (7) | C20—C19—H19A | 109.2 |
O5—Cd1—N2 | 149.43 (7) | C18—C19—H19B | 109.2 |
O2—Cd1—N2 | 92.79 (6) | C20—C19—H19B | 109.2 |
N1—Cd1—N2 | 70.09 (6) | H19A—C19—H19B | 107.9 |
O9—Cd1—O1 | 100.71 (6) | O8—C20—O7 | 125.1 (2) |
O5—Cd1—O1 | 130.02 (7) | O8—C20—C19 | 119.4 (2) |
O2—Cd1—O1 | 54.58 (5) | O7—C20—C19 | 115.5 (2) |
N1—Cd1—O1 | 137.32 (6) | N1—C21—C22 | 123.0 (2) |
N2—Cd1—O1 | 80.34 (6) | N1—C21—H21 | 118.5 |
O9—Cd1—O6 | 88.46 (8) | C22—C21—H21 | 118.5 |
O5—Cd1—O6 | 53.06 (6) | C23—C22—C21 | 119.2 (2) |
O2—Cd1—O6 | 88.12 (7) | C23—C22—H22 | 120.4 |
N1—Cd1—O6 | 134.45 (6) | C21—C22—H22 | 120.4 |
N2—Cd1—O6 | 155.23 (6) | C22—C23—C24 | 119.1 (2) |
O1—Cd1—O6 | 80.08 (6) | C22—C23—H23 | 120.4 |
O9—Cd1—C1 | 127.90 (7) | C24—C23—H23 | 120.4 |
O5—Cd1—C1 | 119.58 (7) | C32—C24—C23 | 117.8 (2) |
O2—Cd1—C1 | 27.37 (6) | C32—C24—C25 | 119.9 (2) |
N1—Cd1—C1 | 117.77 (7) | C23—C24—C25 | 122.3 (2) |
N2—Cd1—C1 | 85.39 (6) | C26—C25—C24 | 120.7 (2) |
O1—Cd1—C1 | 27.23 (6) | C26—C25—H25 | 119.6 |
O6—Cd1—C1 | 84.13 (7) | C24—C25—H25 | 119.6 |
O7i—Cd2—O3 | 96.07 (6) | C25—C26—C27 | 120.8 (2) |
O7i—Cd2—N3 | 82.72 (6) | C25—C26—H26 | 119.6 |
O3—Cd2—N3 | 128.91 (6) | C27—C26—H26 | 119.6 |
O7i—Cd2—N6 | 123.74 (7) | C31—C27—C28 | 117.4 (2) |
O3—Cd2—N6 | 81.73 (6) | C31—C27—C26 | 120.0 (2) |
N3—Cd2—N6 | 139.90 (7) | C28—C27—C26 | 122.5 (2) |
O7i—Cd2—N4 | 148.45 (7) | C29—C28—C27 | 119.2 (2) |
O3—Cd2—N4 | 90.95 (6) | C29—C28—H28 | 120.4 |
N3—Cd2—N4 | 69.16 (6) | C27—C28—H28 | 120.4 |
N6—Cd2—N4 | 87.67 (7) | C28—C29—C30 | 119.3 (2) |
O7i—Cd2—N5 | 88.72 (7) | C28—C29—H29 | 120.3 |
O3—Cd2—N5 | 146.51 (7) | C30—C29—H29 | 120.3 |
N3—Cd2—N5 | 84.56 (7) | N2—C30—C29 | 123.1 (2) |
N6—Cd2—N5 | 68.34 (7) | N2—C30—H30 | 118.5 |
N4—Cd2—N5 | 102.12 (6) | C29—C30—H30 | 118.5 |
C1—O1—Cd1 | 88.85 (13) | N2—C31—C27 | 122.6 (2) |
C1—O2—Cd1 | 94.08 (14) | N2—C31—C32 | 118.2 (2) |
C10—O3—Cd2 | 120.91 (14) | C27—C31—C32 | 119.2 (2) |
C11—O5—Cd1 | 98.65 (15) | N1—C32—C24 | 122.3 (2) |
C11—O6—Cd1 | 85.81 (16) | N1—C32—C31 | 118.5 (2) |
C20—O7—Cd2ii | 121.04 (15) | C24—C32—C31 | 119.2 (2) |
Cd1—O9—H9AO | 122 (2) | N3—C33—C34 | 123.0 (2) |
Cd1—O9—H9BO | 115 (2) | N3—C33—H33 | 118.5 |
H9AO—O9—H9BO | 118 (3) | C34—C33—H33 | 118.5 |
C21—N1—C32 | 118.5 (2) | C35—C34—C33 | 119.4 (2) |
C21—N1—Cd1 | 124.41 (17) | C35—C34—H34 | 120.3 |
C32—N1—Cd1 | 117.07 (14) | C33—C34—H34 | 120.3 |
C30—N2—C31 | 118.3 (2) | C34—C35—C36 | 119.3 (2) |
C30—N2—Cd1 | 125.61 (17) | C34—C35—H35 | 120.4 |
C31—N2—Cd1 | 116.00 (14) | C36—C35—H35 | 120.4 |
C33—N3—C44 | 118.0 (2) | C35—C36—C44 | 117.9 (2) |
C33—N3—Cd2 | 123.73 (15) | C35—C36—C37 | 122.2 (2) |
C44—N3—Cd2 | 117.61 (14) | C44—C36—C37 | 119.8 (2) |
C42—N4—C43 | 118.0 (2) | C38—C37—C36 | 120.2 (2) |
C42—N4—Cd2 | 126.33 (18) | C38—C37—H37 | 119.9 |
C43—N4—Cd2 | 115.59 (14) | C36—C37—H37 | 119.9 |
C45—N5—C56 | 118.8 (2) | C37—C38—C39 | 121.7 (2) |
C45—N5—Cd2 | 124.48 (17) | C37—C38—H38 | 119.1 |
C56—N5—Cd2 | 116.65 (17) | C39—C38—H38 | 119.1 |
C54—N6—C55 | 118.0 (2) | C43—C39—C40 | 117.0 (2) |
C54—N6—Cd2 | 124.04 (16) | C43—C39—C38 | 119.9 (2) |
C55—N6—Cd2 | 117.99 (17) | C40—C39—C38 | 123.1 (2) |
O1—C1—O2 | 122.4 (2) | C41—C40—C39 | 119.6 (2) |
O1—C1—C2 | 119.8 (2) | C41—C40—H40 | 120.2 |
O2—C1—C2 | 117.8 (2) | C39—C40—H40 | 120.2 |
O1—C1—Cd1 | 63.93 (11) | C40—C41—C42 | 119.3 (2) |
O2—C1—Cd1 | 58.55 (11) | C40—C41—H41 | 120.4 |
C2—C1—Cd1 | 175.33 (17) | C42—C41—H41 | 120.4 |
C3—C2—C1 | 112.04 (19) | N4—C42—C41 | 123.0 (3) |
C3—C2—H2A | 109.2 | N4—C42—H42 | 118.5 |
C1—C2—H2A | 109.2 | C41—C42—H42 | 118.5 |
C3—C2—H2B | 109.2 | N4—C43—C39 | 123.1 (2) |
C1—C2—H2B | 109.2 | N4—C43—C44 | 118.24 (19) |
H2A—C2—H2B | 107.9 | C39—C43—C44 | 118.6 (2) |
C8—C3—C4 | 118.9 (2) | N3—C44—C36 | 122.5 (2) |
C8—C3—C2 | 121.8 (2) | N3—C44—C43 | 117.9 (2) |
C4—C3—C2 | 119.2 (2) | C36—C44—C43 | 119.6 (2) |
C5—C4—C3 | 121.0 (3) | N5—C45—C46 | 123.0 (3) |
C5—C4—H4 | 119.5 | N5—C45—H45 | 118.5 |
C3—C4—H4 | 119.5 | C46—C45—H45 | 118.5 |
C6—C5—C4 | 119.9 (3) | C47—C46—C45 | 118.5 (3) |
C6—C5—H5 | 120.1 | C47—C46—H46 | 120.8 |
C4—C5—H5 | 120.1 | C45—C46—H46 | 120.8 |
C7—C6—C5 | 119.7 (3) | C46—C47—C48 | 120.3 (3) |
C7—C6—H6 | 120.2 | C46—C47—H47 | 119.9 |
C5—C6—H6 | 120.2 | C48—C47—H47 | 119.9 |
C6—C7—C8 | 121.5 (3) | C47—C48—C56 | 117.0 (3) |
C6—C7—H7 | 119.2 | C47—C48—C49 | 123.2 (3) |
C8—C7—H7 | 119.2 | C56—C48—C49 | 119.7 (3) |
C3—C8—C7 | 119.0 (2) | C50—C49—C48 | 121.9 (3) |
C3—C8—C9 | 121.2 (2) | C50—C49—H49 | 119.0 |
C7—C8—C9 | 119.7 (2) | C48—C49—H49 | 119.0 |
C8—C9—C10 | 111.10 (18) | C49—C50—C51 | 119.9 (3) |
C8—C9—H9A | 109.4 | C49—C50—H50 | 120.0 |
C10—C9—H9A | 109.4 | C51—C50—H50 | 120.0 |
C8—C9—H9B | 109.4 | C52—C51—C55 | 118.1 (3) |
C10—C9—H9B | 109.4 | C52—C51—C50 | 122.4 (3) |
H9A—C9—H9B | 108.0 | C55—C51—C50 | 119.6 (3) |
O4—C10—O3 | 124.9 (2) | C53—C52—C51 | 119.8 (3) |
O4—C10—C9 | 120.84 (19) | C53—C52—H52 | 120.1 |
O3—C10—C9 | 114.27 (19) | C51—C52—H52 | 120.1 |
O6—C11—O5 | 122.4 (2) | C52—C53—C54 | 118.7 (3) |
O6—C11—C12 | 119.2 (2) | C52—C53—H53 | 120.6 |
O5—C11—C12 | 118.4 (2) | C54—C53—H53 | 120.6 |
C13—C12—C11 | 111.20 (19) | N6—C54—C53 | 123.5 (3) |
C13—C12—H12A | 109.4 | N6—C54—H54 | 118.2 |
C11—C12—H12A | 109.4 | C53—C54—H54 | 118.2 |
C13—C12—H12B | 109.4 | N6—C55—C51 | 121.9 (3) |
C11—C12—H12B | 109.4 | N6—C55—C56 | 118.0 (2) |
H12A—C12—H12B | 108.0 | C51—C55—C56 | 120.0 (2) |
C14—C13—C18 | 119.6 (2) | N5—C56—C48 | 122.4 (3) |
C14—C13—C12 | 119.6 (2) | N5—C56—C55 | 118.9 (2) |
C18—C13—C12 | 120.8 (2) | C48—C56—C55 | 118.7 (2) |
C15—C14—C13 | 120.8 (2) | H01A—O11—H01B | 105 (4) |
C15—C14—H14 | 119.6 | O13—O12—H02A | 119 (3) |
C13—C14—H14 | 119.6 | O13—O12—H02B | 128 (5) |
C16—C15—C14 | 120.1 (2) | H02A—O12—H02B | 110 (5) |
C16—C15—H15 | 120.0 | O10—C58—C57 | 112.6 (3) |
C14—C15—H15 | 120.0 | O10—C58—H58A | 109.1 |
C15—C16—C17 | 119.4 (2) | C57—C58—H58A | 109.1 |
C15—C16—H16 | 120.3 | O10—C58—H58B | 109.1 |
C17—C16—H16 | 120.3 | C57—C58—H58B | 109.1 |
C18—C17—C16 | 121.1 (2) | H58A—C58—H58B | 107.8 |
C18—C17—H17 | 119.4 |
Symmetry codes: (i) x−1, y+1, z; (ii) x+1, y−1, z. |
D—H···A | D—H | H···A | D···A | D—H···A |
O9—H9BO···O1iii | 0.81 (3) | 1.92 (3) | 2.713 (2) | 167 (4) |
O9—H9AO···O4iii | 0.81 (3) | 1.88 (3) | 2.678 (2) | 164 (3) |
O11—H01B···O3ii | 0.82 (3) | 2.07 (3) | 2.860 (3) | 161 (4) |
O11—H01A···O8 | 0.82 (3) | 1.92 (3) | 2.732 (3) | 170 (5) |
O12—H02A···O10 | 0.80 (3) | 2.22 (3) | 2.844 (5) | 136 (3) |
O12—H02B···O11iv | 0.83 (6) | 1.98 (5) | 2.776 (4) | 161 (6) |
O10—H10···O6v | 0.84 | 1.91 | 2.745 (5) | 174 |
Symmetry codes: (ii) x+1, y−1, z; (iii) −x+1, −y+1, −z+1; (iv) −x+1, −y+1, −z+2; (v) −x, −y+1, −z+2. |
Experimental details
Crystal data | |
Chemical formula | [Cd2(C10H8O4)2(C12H8N2)3(H2O)]·0.79C2H6O·3.05H2O |
Mr | 1257.16 |
Crystal system, space group | Triclinic, P1 |
Temperature (K) | 153 |
a, b, c (Å) | 12.6568 (2), 14.7729 (3), 15.0674 (3) |
α, β, γ (°) | 68.710 (1), 83.896 (1), 78.303 (1) |
V (Å3) | 2568.84 (9) |
Z | 2 |
Radiation type | Mo Kα |
µ (mm−1) | 0.90 |
Crystal size (mm) | 0.20 × 0.16 × 0.11 |
Data collection | |
Diffractometer | Rigaku R-AXIS RAPID |
Absorption correction | – |
No. of measured, independent and observed [I > 2σ(I)] reflections | 25428, 11681, 10285 |
Rint | 0.016 |
(sin θ/λ)max (Å−1) | 0.649 |
Refinement | |
R[F2 > 2σ(F2)], wR(F2), S | 0.025, 0.093, 1.01 |
No. of reflections | 11681 |
No. of parameters | 744 |
No. of restraints | 9 |
H-atom treatment | H atoms treated by a mixture of independent and constrained refinement |
Δρmax, Δρmin (e Å−3) | 0.82, −0.85 |
Computer programs: RAPID-AUTO (Rigaku, 2004), SHELXS97 (Sheldrick, 1997a), SHELXL97 (Sheldrick, 1997a), SHELXTL (Sheldrick, 1997b).
D—H···A | D—H | H···A | D···A | D—H···A |
O9—H9BO···O1i | 0.81 (3) | 1.92 (3) | 2.713 (2) | 167 (4) |
O9—H9AO···O4i | 0.81 (3) | 1.88 (3) | 2.678 (2) | 164 (3) |
O11—H01B···O3ii | 0.82 (3) | 2.07 (3) | 2.860 (3) | 161 (4) |
O11—H01A···O8 | 0.82 (3) | 1.92 (3) | 2.732 (3) | 170 (5) |
O12—H02A···O10 | 0.80 (3) | 2.22 (3) | 2.844 (5) | 136 (3) |
O12—H02B···O11iii | 0.83 (6) | 1.98 (5) | 2.776 (4) | 161 (6) |
O10—H10···O6iv | 0.84 | 1.91 | 2.745 (5) | 174 |
Symmetry codes: (i) −x+1, −y+1, −z+1; (ii) x+1, y−1, z; (iii) −x+1, −y+1, −z+2; (iv) −x, −y+1, −z+2. |
Many complexes containing phenanthroline have been reported (e.g. Yam, et al.,1999; Harvey et al., 2000; Ding, et al.,2005) and these include dinuclear complexes containing phenanthroline bridged by carboxylate ligands (Tan, et al.,2006; Shi, et al.,2005). In this report we used phenanthroline, (2-Carboxymethyl-phenyl)-acetic acid and cadmium chloride to construct the title one-dimensional chain polymer.
The asymmetric unit contains two independent CdII atoms, two L2- ligands, three phenanthroline ligands, 3.05 H2O molecules and one partial occupancy C2H5OH molecule. The two CdII atoms have different coordination modes. Atom Cd1 is coordinated by four O atoms from two different L2- ligands, two N atoms from one phenanthroline ligand and by atom O9 from a water molecule, forming a distorted monocapped octahedral geometry. Atom Cd2 is coordinated by four N atoms from two different phenanthroline ligands and two O atoms from a two bridging L2-, ligands, forming a distorted octahedral geometry. The two independent CdII atoms are bridged by a L2- ligand forming a one-dimensional chain structure. Part of the one dimensional chain structure is shown in Fig. 1. A l l bond distances and angles are as expected. In the crystal structure, intermolecular O—H···O hydrogen bonds connect molecules to form a two-dimensional network (Fig. 2).