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3-(4-Pyridyl)-acetylacetone (HacacPy) acts as a pyridine-type ligand towards Cd
X2 (
X = Cl, Br, I). Chain polymers with six-coordinated metal cations are obtained from CdCl
2 and with alternating five- and six-coordinated Cd centers from CdBr
2. In either case, the formation of these compounds does not depend on the precise stoichiometry. In contrast, two different reaction products form with the heavier congener CdI
2, namely a ligand-rich molecular complex CdI
2(HacacPy)
2 and a ligand-deficient one-dimensional polymer [CdI
2(HacacPy)]
1∞. Interconversion between these two iodo derivatives is possible
via thermal degradation and mechanochemical synthesis. The acetylacetone moiety in HacacPy may be deprotonated and chelated to Fe
III, and the resulting complex Fe(acacPy)
3 reacts analogously to a bridging polypyridine ligand towards the same Cd halides as the molecule HacacPy itself. With CdCl
2 and CdBr
2, isomorphous chain polymers are obtained in which the Cd cations adopt distorted octahedral coordination and one of the peripheric pyridyl groups remains uncoordinated. With CdI
2, the iron complex acts as a
-Fe(acacPy)
3 bridge between tetrahedral Cd centers and gives rise to a ladder structure.
Supporting information
CCDC references: 992992; 992993; 992994; 992995
Crystal data, data collection and structure refinement details are summarized
in Table 1.
S2. Results and discussion
top
Data collection: Bruker SAMRT for (1), (3a), 6_squeeze, 6_without_squeeze; Bruker SMART for (2), (3b), (4), (5). Cell refinement: Bruker SAINT for (1), (4); Bruker SAINT 2009 for (2), (3a), (3b), (5), 6_squeeze, 6_without_squeeze. Data reduction: Bruker SAINT for (1), (4); Bruker SAINT 2009 for (2), (3a), (3b), (5), 6_squeeze, 6_without_squeeze. Program(s) used to solve structure: SHELXS97 for (1), (2), (3a), (3b), (5), 6_squeeze, 6_without_squeeze; SHELXL97 for (4). For all compounds, program(s) used to refine structure: SHELXL2013 (Sheldrick, 2013).
Crystal data top
C30H33Cd2Cl4N3O6 | Z = 2 |
Mr = 898.21 | F(000) = 892 |
Triclinic, P1 | Dx = 1.677 Mg m−3 |
a = 9.8304 (8) Å | Mo Kα radiation, λ = 0.71073 Å |
b = 13.7388 (11) Å | Cell parameters from 3427 reflections |
c = 14.8816 (12) Å | θ = 2.5–28.3° |
α = 63.4935 (11)° | µ = 1.54 mm−1 |
β = 84.0016 (13)° | T = 100 K |
γ = 81.8575 (12)° | Needle, colorless |
V = 1778.5 (2) Å3 | 0.29 × 0.08 × 0.06 mm |
Data collection top
CCD area detector diffractometer | 7972 reflections with I > 2σ(I) |
Radiation source: Incoatec microsource, multilayer optics | Rint = 0.048 |
ω scans | θmax = 29.9°, θmin = 2.1° |
Absorption correction: multi-scan SADABS | h = −13→13 |
Tmin = 0.632, Tmax = 0.746 | k = −19→19 |
26747 measured reflections | l = −20→20 |
9968 independent reflections | |
Refinement top
Refinement on F2 | Primary atom site location: heavy-atom method |
Least-squares matrix: full | Hydrogen site location: mixed |
R[F2 > 2σ(F2)] = 0.037 | H atoms treated by a mixture of independent and constrained refinement |
wR(F2) = 0.079 | w = 1/[σ2(Fo2) + (0.0241P)2]
where P = (Fo2 + 2Fc2)/3 |
S = 1.03 | (Δ/σ)max = 0.001 |
9968 reflections | Δρmax = 0.74 e Å−3 |
421 parameters | Δρmin = −0.54 e Å−3 |
3 restraints | |
Crystal data top
C30H33Cd2Cl4N3O6 | γ = 81.8575 (12)° |
Mr = 898.21 | V = 1778.5 (2) Å3 |
Triclinic, P1 | Z = 2 |
a = 9.8304 (8) Å | Mo Kα radiation |
b = 13.7388 (11) Å | µ = 1.54 mm−1 |
c = 14.8816 (12) Å | T = 100 K |
α = 63.4935 (11)° | 0.29 × 0.08 × 0.06 mm |
β = 84.0016 (13)° | |
Data collection top
CCD area detector diffractometer | 9968 independent reflections |
Absorption correction: multi-scan SADABS | 7972 reflections with I > 2σ(I) |
Tmin = 0.632, Tmax = 0.746 | Rint = 0.048 |
26747 measured reflections | |
Refinement top
R[F2 > 2σ(F2)] = 0.037 | 3 restraints |
wR(F2) = 0.079 | H atoms treated by a mixture of independent and constrained refinement |
S = 1.03 | Δρmax = 0.74 e Å−3 |
9968 reflections | Δρmin = −0.54 e Å−3 |
421 parameters | |
Special details top
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. |
Fractional atomic coordinates and isotropic or equivalent isotropic displacement parameters (Å2) top | x | y | z | Uiso*/Ueq | |
Cd1 | 0.50443 (2) | 0.05368 (2) | 0.35685 (2) | 0.01277 (5) | |
Cd2 | 0.15023 (2) | 0.07845 (2) | 0.49986 (2) | 0.01286 (5) | |
Cl1 | 0.35930 (7) | −0.08333 (5) | 0.51401 (5) | 0.01328 (13) | |
Cl2 | 0.30590 (7) | 0.20222 (5) | 0.35240 (5) | 0.01551 (14) | |
Cl3 | 0.28795 (7) | 0.08664 (6) | 0.63691 (5) | 0.01653 (14) | |
Cl4 | 0.01156 (7) | 0.05557 (5) | 0.36904 (5) | 0.01549 (14) | |
O1 | 0.1299 (2) | −0.10925 (19) | −0.06145 (17) | 0.0307 (6) | |
O2 | −0.0320 (3) | −0.1808 (2) | 0.08470 (18) | 0.0306 (6) | |
H2D | 0.009 (3) | −0.162 (3) | 0.0278 (17) | 0.037* | |
O3 | 0.8559 (3) | 0.5588 (2) | −0.18904 (19) | 0.0452 (7) | |
H3D | 0.868 (4) | 0.600 (3) | −0.160 (3) | 0.054* | |
O4 | 0.8571 (3) | 0.6459 (2) | −0.0755 (2) | 0.0465 (7) | |
O5 | −0.5520 (2) | 0.55950 (18) | 0.32619 (19) | 0.0301 (6) | |
H5D | −0.533 (4) | 0.601 (2) | 0.351 (2) | 0.036* | |
O6 | −0.4417 (2) | 0.66111 (17) | 0.39087 (18) | 0.0283 (5) | |
N1 | 0.3871 (2) | 0.00479 (19) | 0.25611 (17) | 0.0143 (5) | |
N2 | 0.6033 (3) | 0.19701 (19) | 0.21866 (18) | 0.0177 (5) | |
N3 | −0.0091 (2) | 0.23090 (18) | 0.48202 (17) | 0.0147 (5) | |
C1 | −0.0101 (4) | −0.1713 (3) | 0.2366 (3) | 0.0330 (8) | |
H1A | −0.0990 | −0.2010 | 0.2512 | 0.049* | |
H1B | −0.0205 | −0.1033 | 0.2441 | 0.049* | |
H1C | 0.0569 | −0.2245 | 0.2835 | 0.049* | |
C2 | 0.0389 (3) | −0.1487 (3) | 0.1319 (2) | 0.0226 (7) | |
C3 | 0.1587 (3) | −0.0961 (2) | 0.0873 (2) | 0.0185 (6) | |
C4 | 0.1994 (3) | −0.0771 (3) | −0.0116 (2) | 0.0230 (7) | |
C5 | 0.3214 (4) | −0.0197 (3) | −0.0668 (3) | 0.0337 (8) | |
H5A | 0.3186 | −0.0006 | −0.1384 | 0.050* | |
H5B | 0.4057 | −0.0678 | −0.0400 | 0.050* | |
H5C | 0.3203 | 0.0472 | −0.0582 | 0.050* | |
C6 | 0.2393 (3) | −0.0607 (2) | 0.1451 (2) | 0.0164 (6) | |
C7 | 0.2049 (3) | 0.0395 (3) | 0.1478 (2) | 0.0241 (7) | |
H7 | 0.1303 | 0.0881 | 0.1111 | 0.029* | |
C8 | 0.2800 (3) | 0.0681 (2) | 0.2044 (2) | 0.0206 (7) | |
H8 | 0.2537 | 0.1364 | 0.2064 | 0.025* | |
C9 | 0.4215 (3) | −0.0925 (2) | 0.2543 (2) | 0.0194 (6) | |
H9 | 0.4976 | −0.1388 | 0.2909 | 0.023* | |
C10 | 0.3497 (3) | −0.1273 (2) | 0.2007 (2) | 0.0220 (7) | |
H10 | 0.3760 | −0.1972 | 0.2020 | 0.026* | |
C11 | 0.7779 (4) | 0.3892 (3) | −0.1410 (3) | 0.0438 (10) | |
H11A | 0.6994 | 0.4150 | −0.1843 | 0.066* | |
H11B | 0.7577 | 0.3235 | −0.0799 | 0.066* | |
H11C | 0.8597 | 0.3717 | −0.1770 | 0.066* | |
C12 | 0.8038 (4) | 0.4762 (3) | −0.1133 (3) | 0.0328 (8) | |
C13 | 0.7788 (3) | 0.4731 (3) | −0.0195 (2) | 0.0255 (7) | |
C14 | 0.8102 (4) | 0.5627 (3) | −0.0036 (3) | 0.0370 (9) | |
C15 | 0.7880 (5) | 0.5631 (3) | 0.0974 (3) | 0.0508 (12) | |
H15A | 0.8072 | 0.6338 | 0.0917 | 0.076* | |
H15B | 0.8498 | 0.5045 | 0.1448 | 0.076* | |
H15C | 0.6923 | 0.5514 | 0.1217 | 0.076* | |
C16 | 0.7194 (3) | 0.3772 (2) | 0.0642 (2) | 0.0235 (7) | |
C17 | 0.7965 (3) | 0.3002 (3) | 0.1439 (2) | 0.0252 (7) | |
H17 | 0.8902 | 0.3077 | 0.1472 | 0.030* | |
C18 | 0.7346 (3) | 0.2121 (3) | 0.2185 (2) | 0.0221 (7) | |
H18 | 0.7886 | 0.1600 | 0.2722 | 0.027* | |
C19 | 0.5291 (3) | 0.2716 (3) | 0.1418 (2) | 0.0245 (7) | |
H19 | 0.4351 | 0.2628 | 0.1412 | 0.029* | |
C20 | 0.5826 (3) | 0.3599 (3) | 0.0642 (2) | 0.0283 (8) | |
H20 | 0.5267 | 0.4092 | 0.0106 | 0.034* | |
C21 | −0.2290 (3) | 0.6006 (3) | 0.4710 (3) | 0.0273 (7) | |
H21A | −0.2407 | 0.6760 | 0.4631 | 0.041* | |
H21B | −0.1388 | 0.5860 | 0.4420 | 0.041* | |
H21C | −0.2352 | 0.5499 | 0.5426 | 0.041* | |
C22 | −0.3392 (3) | 0.5852 (3) | 0.4182 (2) | 0.0236 (7) | |
C23 | −0.3380 (3) | 0.4930 (2) | 0.4003 (2) | 0.0182 (6) | |
C24 | −0.4495 (3) | 0.4833 (2) | 0.3537 (2) | 0.0232 (7) | |
C25 | −0.4587 (4) | 0.3874 (3) | 0.3338 (3) | 0.0342 (9) | |
H25A | −0.4937 | 0.3280 | 0.3948 | 0.051* | |
H25B | −0.3672 | 0.3624 | 0.3140 | 0.051* | |
H25C | −0.5213 | 0.4085 | 0.2794 | 0.051* | |
C26 | −0.2210 (3) | 0.4037 (2) | 0.4311 (2) | 0.0169 (6) | |
C27 | −0.2391 (3) | 0.3009 (2) | 0.5084 (2) | 0.0186 (6) | |
H27 | −0.3248 | 0.2875 | 0.5454 | 0.022* | |
C28 | −0.1315 (3) | 0.2180 (2) | 0.5311 (2) | 0.0165 (6) | |
H28 | −0.1458 | 0.1483 | 0.5845 | 0.020* | |
C29 | 0.0094 (3) | 0.3313 (2) | 0.4081 (2) | 0.0197 (6) | |
H29 | 0.0965 | 0.3430 | 0.3731 | 0.024* | |
C30 | −0.0933 (3) | 0.4178 (2) | 0.3811 (2) | 0.0195 (6) | |
H30 | −0.0761 | 0.4870 | 0.3282 | 0.023* | |
Atomic displacement parameters (Å2) top | U11 | U22 | U33 | U12 | U13 | U23 |
Cd1 | 0.01101 (11) | 0.01454 (10) | 0.01177 (10) | −0.00073 (8) | −0.00071 (8) | −0.00502 (8) |
Cd2 | 0.00964 (10) | 0.01305 (10) | 0.01458 (11) | −0.00053 (8) | −0.00095 (8) | −0.00500 (8) |
Cl1 | 0.0121 (3) | 0.0132 (3) | 0.0141 (3) | −0.0014 (3) | −0.0011 (3) | −0.0055 (3) |
Cl2 | 0.0121 (3) | 0.0143 (3) | 0.0174 (3) | −0.0008 (3) | 0.0012 (3) | −0.0051 (3) |
Cl3 | 0.0133 (3) | 0.0197 (3) | 0.0186 (3) | 0.0013 (3) | −0.0035 (3) | −0.0106 (3) |
Cl4 | 0.0132 (3) | 0.0164 (3) | 0.0146 (3) | −0.0029 (3) | −0.0010 (3) | −0.0044 (3) |
O1 | 0.0319 (14) | 0.0429 (14) | 0.0270 (13) | 0.0038 (11) | −0.0119 (11) | −0.0240 (11) |
O2 | 0.0268 (14) | 0.0389 (14) | 0.0338 (14) | −0.0058 (11) | −0.0041 (11) | −0.0217 (12) |
O3 | 0.0498 (18) | 0.0362 (16) | 0.0269 (14) | 0.0024 (14) | 0.0129 (13) | 0.0014 (12) |
O4 | 0.0450 (18) | 0.0296 (14) | 0.0456 (17) | −0.0136 (13) | −0.0016 (14) | 0.0033 (12) |
O5 | 0.0235 (13) | 0.0208 (12) | 0.0476 (16) | 0.0070 (10) | −0.0153 (11) | −0.0164 (11) |
O6 | 0.0232 (13) | 0.0181 (11) | 0.0440 (15) | 0.0063 (9) | −0.0080 (11) | −0.0150 (11) |
N1 | 0.0120 (12) | 0.0160 (12) | 0.0140 (12) | −0.0026 (10) | −0.0004 (9) | −0.0055 (10) |
N2 | 0.0167 (13) | 0.0198 (12) | 0.0144 (12) | −0.0010 (10) | −0.0010 (10) | −0.0057 (10) |
N3 | 0.0135 (13) | 0.0150 (12) | 0.0148 (12) | 0.0008 (10) | −0.0028 (10) | −0.0059 (10) |
C1 | 0.0250 (19) | 0.044 (2) | 0.032 (2) | −0.0085 (16) | 0.0048 (15) | −0.0187 (17) |
C2 | 0.0188 (17) | 0.0269 (17) | 0.0268 (17) | 0.0005 (13) | −0.0043 (13) | −0.0162 (14) |
C3 | 0.0130 (15) | 0.0245 (15) | 0.0219 (16) | 0.0019 (12) | −0.0060 (12) | −0.0136 (13) |
C4 | 0.0227 (17) | 0.0264 (17) | 0.0205 (16) | 0.0043 (14) | −0.0067 (13) | −0.0116 (14) |
C5 | 0.031 (2) | 0.048 (2) | 0.0241 (18) | −0.0061 (18) | 0.0001 (15) | −0.0180 (17) |
C6 | 0.0170 (16) | 0.0206 (15) | 0.0131 (14) | −0.0012 (12) | −0.0016 (12) | −0.0087 (12) |
C7 | 0.0199 (17) | 0.0290 (17) | 0.0272 (17) | 0.0080 (13) | −0.0146 (14) | −0.0159 (14) |
C8 | 0.0223 (17) | 0.0217 (15) | 0.0207 (16) | 0.0037 (13) | −0.0076 (13) | −0.0122 (13) |
C9 | 0.0166 (16) | 0.0194 (15) | 0.0222 (16) | 0.0028 (12) | −0.0069 (12) | −0.0092 (13) |
C10 | 0.0227 (17) | 0.0175 (15) | 0.0269 (17) | −0.0003 (13) | −0.0066 (14) | −0.0100 (13) |
C11 | 0.057 (3) | 0.038 (2) | 0.028 (2) | 0.011 (2) | 0.0002 (19) | −0.0116 (17) |
C12 | 0.030 (2) | 0.0257 (18) | 0.0231 (18) | 0.0052 (15) | 0.0031 (15) | 0.0030 (14) |
C13 | 0.0239 (18) | 0.0200 (16) | 0.0204 (16) | −0.0022 (13) | −0.0009 (14) | 0.0020 (13) |
C14 | 0.031 (2) | 0.0286 (19) | 0.037 (2) | −0.0079 (16) | −0.0019 (17) | 0.0000 (16) |
C15 | 0.068 (3) | 0.038 (2) | 0.046 (3) | −0.020 (2) | −0.008 (2) | −0.014 (2) |
C16 | 0.0246 (18) | 0.0205 (16) | 0.0215 (16) | −0.0015 (13) | 0.0002 (13) | −0.0064 (13) |
C17 | 0.0185 (17) | 0.0260 (17) | 0.0254 (17) | −0.0063 (14) | 0.0002 (14) | −0.0055 (14) |
C18 | 0.0180 (16) | 0.0241 (16) | 0.0187 (15) | 0.0021 (13) | −0.0021 (13) | −0.0055 (13) |
C19 | 0.0127 (16) | 0.0317 (18) | 0.0245 (17) | −0.0012 (13) | −0.0031 (13) | −0.0082 (14) |
C20 | 0.0258 (19) | 0.0269 (17) | 0.0222 (17) | −0.0007 (15) | −0.0059 (14) | −0.0014 (14) |
C21 | 0.0262 (19) | 0.0206 (16) | 0.038 (2) | 0.0003 (14) | −0.0073 (15) | −0.0152 (15) |
C22 | 0.0193 (17) | 0.0207 (16) | 0.0291 (18) | −0.0017 (13) | 0.0005 (14) | −0.0098 (14) |
C23 | 0.0161 (16) | 0.0139 (14) | 0.0215 (15) | 0.0031 (12) | −0.0025 (12) | −0.0060 (12) |
C24 | 0.0173 (16) | 0.0157 (15) | 0.0333 (18) | 0.0019 (12) | −0.0047 (14) | −0.0081 (14) |
C25 | 0.034 (2) | 0.0270 (18) | 0.046 (2) | 0.0034 (16) | −0.0158 (18) | −0.0193 (17) |
C26 | 0.0147 (15) | 0.0171 (14) | 0.0232 (16) | 0.0019 (12) | −0.0057 (12) | −0.0127 (13) |
C27 | 0.0153 (15) | 0.0168 (14) | 0.0228 (16) | −0.0031 (12) | 0.0030 (12) | −0.0084 (12) |
C28 | 0.0149 (15) | 0.0151 (14) | 0.0192 (15) | −0.0019 (11) | 0.0003 (12) | −0.0075 (12) |
C29 | 0.0173 (16) | 0.0201 (15) | 0.0203 (15) | −0.0037 (12) | 0.0018 (12) | −0.0079 (13) |
C30 | 0.0210 (17) | 0.0131 (14) | 0.0202 (15) | 0.0004 (12) | 0.0000 (13) | −0.0043 (12) |
Geometric parameters (Å, º) top
Cd1—N1 | 2.347 (2) | C7—H7 | 0.9500 |
Cd1—N2 | 2.358 (2) | C8—H8 | 0.9500 |
Cd1—Cl3i | 2.5800 (7) | C9—C10 | 1.385 (4) |
Cd1—Cl2 | 2.5992 (7) | C9—H9 | 0.9500 |
Cd1—Cl1i | 2.6542 (7) | C10—H10 | 0.9500 |
Cd1—Cl1 | 2.6800 (7) | C11—C12 | 1.487 (5) |
Cd2—N3 | 2.360 (2) | C11—H11A | 0.9800 |
Cd2—Cl4ii | 2.5885 (7) | C11—H11B | 0.9800 |
Cd2—Cl2 | 2.5987 (7) | C11—H11C | 0.9800 |
Cd2—Cl3 | 2.6135 (7) | C12—C13 | 1.375 (5) |
Cd2—Cl4 | 2.6400 (7) | C13—C14 | 1.432 (5) |
Cd2—Cl1 | 2.7544 (7) | C13—C16 | 1.493 (4) |
Cl1—Cd1i | 2.6542 (7) | C14—C15 | 1.498 (5) |
Cl3—Cd1i | 2.5800 (7) | C15—H15A | 0.9800 |
Cl4—Cd2ii | 2.5885 (7) | C15—H15B | 0.9800 |
O1—C4 | 1.302 (4) | C15—H15C | 0.9800 |
O2—C2 | 1.281 (4) | C16—C17 | 1.394 (4) |
O2—H2D | 0.841 (18) | C16—C20 | 1.398 (4) |
O3—C12 | 1.313 (4) | C17—C18 | 1.390 (4) |
O3—H3D | 0.880 (18) | C17—H17 | 0.9500 |
O4—C14 | 1.272 (4) | C18—H18 | 0.9500 |
O5—C24 | 1.297 (3) | C19—C20 | 1.373 (4) |
O5—H5D | 0.859 (18) | C19—H19 | 0.9500 |
O6—C22 | 1.295 (4) | C20—H20 | 0.9500 |
N1—C8 | 1.331 (4) | C21—C22 | 1.493 (4) |
N1—C9 | 1.343 (3) | C21—H21A | 0.9800 |
N2—C18 | 1.336 (4) | C21—H21B | 0.9800 |
N2—C19 | 1.344 (4) | C21—H21C | 0.9800 |
N3—C28 | 1.332 (4) | C22—C23 | 1.405 (4) |
N3—C29 | 1.349 (3) | C23—C24 | 1.408 (4) |
C1—C2 | 1.486 (4) | C23—C26 | 1.499 (4) |
C1—H1A | 0.9800 | C24—C25 | 1.491 (4) |
C1—H1B | 0.9800 | C25—H25A | 0.9800 |
C1—H1C | 0.9800 | C25—H25B | 0.9800 |
C2—C3 | 1.414 (4) | C25—H25C | 0.9800 |
C3—C4 | 1.400 (4) | C26—C30 | 1.382 (4) |
C3—C6 | 1.493 (4) | C26—C27 | 1.389 (4) |
C4—C5 | 1.490 (5) | C27—C28 | 1.386 (4) |
C5—H5A | 0.9800 | C27—H27 | 0.9500 |
C5—H5B | 0.9800 | C28—H28 | 0.9500 |
C5—H5C | 0.9800 | C29—C30 | 1.382 (4) |
C6—C7 | 1.387 (4) | C29—H29 | 0.9500 |
C6—C10 | 1.390 (4) | C30—H30 | 0.9500 |
C7—C8 | 1.384 (4) | | |
| | | |
N1—Cd1—N2 | 93.94 (8) | N1—C9—C10 | 122.1 (3) |
N1—Cd1—Cl3i | 91.38 (6) | N1—C9—H9 | 118.9 |
N2—Cd1—Cl3i | 92.61 (6) | C10—C9—H9 | 118.9 |
N1—Cd1—Cl2 | 91.88 (6) | C9—C10—C6 | 120.4 (3) |
N2—Cd1—Cl2 | 85.55 (6) | C9—C10—H10 | 119.8 |
Cl3i—Cd1—Cl2 | 176.36 (2) | C6—C10—H10 | 119.8 |
N1—Cd1—Cl1i | 173.05 (6) | C12—C11—H11A | 109.5 |
N2—Cd1—Cl1i | 91.79 (6) | C12—C11—H11B | 109.5 |
Cl3i—Cd1—Cl1i | 84.42 (2) | H11A—C11—H11B | 109.5 |
Cl2—Cd1—Cl1i | 92.48 (2) | C12—C11—H11C | 109.5 |
N1—Cd1—Cl1 | 86.84 (6) | H11A—C11—H11C | 109.5 |
N2—Cd1—Cl1 | 170.48 (6) | H11B—C11—H11C | 109.5 |
Cl3i—Cd1—Cl1 | 96.86 (2) | O3—C12—C13 | 122.1 (3) |
Cl2—Cd1—Cl1 | 84.94 (2) | O3—C12—C11 | 112.5 (3) |
Cl1i—Cd1—Cl1 | 88.16 (2) | C13—C12—C11 | 125.4 (3) |
N3—Cd2—Cl4ii | 91.69 (6) | C12—C13—C14 | 119.2 (3) |
N3—Cd2—Cl2 | 91.04 (6) | C12—C13—C16 | 119.9 (3) |
Cl4ii—Cd2—Cl2 | 172.39 (2) | C14—C13—C16 | 120.9 (3) |
N3—Cd2—Cl3 | 94.90 (6) | O4—C14—C13 | 120.9 (4) |
Cl4ii—Cd2—Cl3 | 93.40 (2) | O4—C14—C15 | 117.4 (3) |
Cl2—Cd2—Cl3 | 93.45 (2) | C13—C14—C15 | 121.7 (3) |
N3—Cd2—Cl4 | 87.86 (6) | C14—C15—H15A | 109.5 |
Cl4ii—Cd2—Cl4 | 83.73 (2) | C14—C15—H15B | 109.5 |
Cl2—Cd2—Cl4 | 89.28 (2) | H15A—C15—H15B | 109.5 |
Cl3—Cd2—Cl4 | 176.08 (2) | C14—C15—H15C | 109.5 |
N3—Cd2—Cl1 | 173.39 (6) | H15A—C15—H15C | 109.5 |
Cl4ii—Cd2—Cl1 | 94.23 (2) | H15B—C15—H15C | 109.5 |
Cl2—Cd2—Cl1 | 83.46 (2) | C17—C16—C20 | 117.0 (3) |
Cl3—Cd2—Cl1 | 81.83 (2) | C17—C16—C13 | 122.4 (3) |
Cl4—Cd2—Cl1 | 95.70 (2) | C20—C16—C13 | 120.6 (3) |
Cd1i—Cl1—Cd1 | 91.84 (2) | C18—C17—C16 | 119.2 (3) |
Cd1i—Cl1—Cd2 | 94.11 (2) | C18—C17—H17 | 120.4 |
Cd1—Cl1—Cd2 | 92.96 (2) | C16—C17—H17 | 120.4 |
Cd2—Cl2—Cd1 | 98.61 (2) | N2—C18—C17 | 123.5 (3) |
Cd1i—Cl3—Cd2 | 99.36 (2) | N2—C18—H18 | 118.3 |
Cd2ii—Cl4—Cd2 | 96.27 (2) | C17—C18—H18 | 118.3 |
C2—O2—H2D | 105 (3) | N2—C19—C20 | 123.1 (3) |
C12—O3—H3D | 101 (3) | N2—C19—H19 | 118.5 |
C24—O5—H5D | 102 (2) | C20—C19—H19 | 118.5 |
C8—N1—C9 | 117.8 (2) | C19—C20—C16 | 120.0 (3) |
C8—N1—Cd1 | 121.87 (19) | C19—C20—H20 | 120.0 |
C9—N1—Cd1 | 120.23 (19) | C16—C20—H20 | 120.0 |
C18—N2—C19 | 117.3 (3) | C22—C21—H21A | 109.5 |
C18—N2—Cd1 | 120.26 (19) | C22—C21—H21B | 109.5 |
C19—N2—Cd1 | 122.2 (2) | H21A—C21—H21B | 109.5 |
C28—N3—C29 | 117.1 (3) | C22—C21—H21C | 109.5 |
C28—N3—Cd2 | 120.99 (18) | H21A—C21—H21C | 109.5 |
C29—N3—Cd2 | 120.74 (19) | H21B—C21—H21C | 109.5 |
C2—C1—H1A | 109.5 | O6—C22—C23 | 120.0 (3) |
C2—C1—H1B | 109.5 | O6—C22—C21 | 116.4 (3) |
H1A—C1—H1B | 109.5 | C23—C22—C21 | 123.5 (3) |
C2—C1—H1C | 109.5 | C22—C23—C24 | 119.5 (3) |
H1A—C1—H1C | 109.5 | C22—C23—C26 | 121.2 (3) |
H1B—C1—H1C | 109.5 | C24—C23—C26 | 119.3 (3) |
O2—C2—C3 | 121.7 (3) | O5—C24—C23 | 120.5 (3) |
O2—C2—C1 | 116.5 (3) | O5—C24—C25 | 116.3 (3) |
C3—C2—C1 | 121.8 (3) | C23—C24—C25 | 123.3 (3) |
C4—C3—C2 | 119.1 (3) | C24—C25—H25A | 109.5 |
C4—C3—C6 | 120.8 (3) | C24—C25—H25B | 109.5 |
C2—C3—C6 | 120.1 (3) | H25A—C25—H25B | 109.5 |
O1—C4—C3 | 120.7 (3) | C24—C25—H25C | 109.5 |
O1—C4—C5 | 115.8 (3) | H25A—C25—H25C | 109.5 |
C3—C4—C5 | 123.5 (3) | H25B—C25—H25C | 109.5 |
C4—C5—H5A | 109.5 | C30—C26—C27 | 117.1 (3) |
C4—C5—H5B | 109.5 | C30—C26—C23 | 122.0 (3) |
H5A—C5—H5B | 109.5 | C27—C26—C23 | 120.8 (3) |
C4—C5—H5C | 109.5 | C28—C27—C26 | 119.5 (3) |
H5A—C5—H5C | 109.5 | C28—C27—H27 | 120.2 |
H5B—C5—H5C | 109.5 | C26—C27—H27 | 120.2 |
C7—C6—C10 | 116.8 (3) | N3—C28—C27 | 123.4 (3) |
C7—C6—C3 | 121.4 (3) | N3—C28—H28 | 118.3 |
C10—C6—C3 | 121.8 (3) | C27—C28—H28 | 118.3 |
C8—C7—C6 | 119.6 (3) | N3—C29—C30 | 122.7 (3) |
C8—C7—H7 | 120.2 | N3—C29—H29 | 118.6 |
C6—C7—H7 | 120.2 | C30—C29—H29 | 118.6 |
N1—C8—C7 | 123.3 (3) | C26—C30—C29 | 120.1 (3) |
N1—C8—H8 | 118.4 | C26—C30—H30 | 119.9 |
C7—C8—H8 | 118.4 | C29—C30—H30 | 119.9 |
Symmetry codes: (i) −x+1, −y, −z+1; (ii) −x, −y, −z+1. |
Crystal data top
C30H33Br4Cd2N3O6 | V = 1796.0 (4) Å3 |
Mr = 1076.03 | Z = 2 |
Triclinic, P1 | F(000) = 1036 |
a = 7.1262 (9) Å | Dx = 1.990 Mg m−3 |
b = 15.519 (2) Å | Mo Kα radiation, λ = 0.71073 Å |
c = 16.597 (2) Å | µ = 5.68 mm−1 |
α = 91.247 (3)° | T = 100 K |
β = 97.889 (3)° | Plate, colorless |
γ = 98.609 (3)° | 0.18 × 0.13 × 0.04 mm |
Data collection top
CCD area detector diffractometer | 5914 reflections with I > 2σ(I) |
Radiation source: Incoatec microsource | Rint = 0.084 |
ω scans | θmax = 26.4°, θmin = 1.2° |
Absorption correction: multi-scan TWINABS | h = −8→8 |
Tmin = 0.522, Tmax = 0.746 | k = −19→19 |
7336 measured reflections | l = 0→20 |
7336 independent reflections | |
Refinement top
Refinement on F2 | 11 restraints |
Least-squares matrix: full | Hydrogen site location: mixed |
R[F2 > 2σ(F2)] = 0.056 | H atoms treated by a mixture of independent and constrained refinement |
wR(F2) = 0.103 | w = 1/[σ2(Fo2) + (0.0199P)2 + 4.2083P]
where P = (Fo2 + 2Fc2)/3 |
S = 1.14 | (Δ/σ)max = 0.001 |
7336 reflections | Δρmax = 0.99 e Å−3 |
423 parameters | Δρmin = −0.91 e Å−3 |
Crystal data top
C30H33Br4Cd2N3O6 | γ = 98.609 (3)° |
Mr = 1076.03 | V = 1796.0 (4) Å3 |
Triclinic, P1 | Z = 2 |
a = 7.1262 (9) Å | Mo Kα radiation |
b = 15.519 (2) Å | µ = 5.68 mm−1 |
c = 16.597 (2) Å | T = 100 K |
α = 91.247 (3)° | 0.18 × 0.13 × 0.04 mm |
β = 97.889 (3)° | |
Data collection top
CCD area detector diffractometer | 7336 independent reflections |
Absorption correction: multi-scan TWINABS | 5914 reflections with I > 2σ(I) |
Tmin = 0.522, Tmax = 0.746 | Rint = 0.084 |
7336 measured reflections | |
Refinement top
R[F2 > 2σ(F2)] = 0.056 | 11 restraints |
wR(F2) = 0.103 | H atoms treated by a mixture of independent and constrained refinement |
S = 1.14 | Δρmax = 0.99 e Å−3 |
7336 reflections | Δρmin = −0.91 e Å−3 |
423 parameters | |
Special details top
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. Refined as a 2-component twin. |
Fractional atomic coordinates and isotropic or equivalent isotropic displacement parameters (Å2) top | x | y | z | Uiso*/Ueq | Occ. (<1) |
Cd1 | 0.79198 (10) | 0.62721 (3) | 0.25945 (4) | 0.01556 (14) | |
Cd2 | 0.25939 (10) | 0.53220 (3) | 0.25449 (4) | 0.01486 (14) | |
Br1 | 0.60807 (13) | 0.53188 (6) | 0.36106 (5) | 0.0176 (2) | |
Br2 | 0.45375 (13) | 0.65869 (5) | 0.17413 (5) | 0.0179 (2) | |
Br3 | −0.08678 (13) | 0.53698 (6) | 0.14634 (5) | 0.0177 (2) | |
Br4 | 0.14362 (13) | 0.64469 (6) | 0.35535 (5) | 0.0187 (2) | |
O1 | 1.0537 (13) | 1.1873 (5) | 0.1974 (5) | 0.047 (2) | |
H1D | 1.156 (11) | 1.184 (8) | 0.229 (7) | 0.071* | |
O2 | 1.3530 (11) | 1.1631 (4) | 0.2822 (4) | 0.041 (2) | |
O3 | −0.2057 (10) | 0.0872 (4) | 0.5199 (5) | 0.0393 (19) | |
O4 | −0.4688 (11) | 0.1715 (4) | 0.5194 (4) | 0.0326 (18) | |
H4D | −0.398 (13) | 0.133 (5) | 0.524 (7) | 0.049* | |
O5 | 0.7676 (10) | 0.1848 (4) | −0.0443 (4) | 0.0276 (16) | |
H5D | 0.661 (8) | 0.151 (6) | −0.054 (7) | 0.041* | |
O6 | 0.4521 (11) | 0.1011 (4) | −0.0559 (5) | 0.042 (2) | |
N1 | 0.8823 (11) | 0.7761 (4) | 0.2520 (5) | 0.0215 (18) | |
N2 | 0.1016 (11) | 0.4196 (4) | 0.3242 (4) | 0.0189 (17) | |
N3 | 0.3468 (10) | 0.4274 (4) | 0.1689 (4) | 0.0149 (16) | |
C1 | 0.7914 (18) | 1.0759 (6) | 0.1580 (8) | 0.053 (4) | |
H1A | 0.7006 | 1.1040 | 0.1847 | 0.079* | |
H1B | 0.7572 | 1.0124 | 0.1586 | 0.079* | |
H1C | 0.7866 | 1.0937 | 0.1015 | 0.079* | |
C2 | 0.9908 (17) | 1.1032 (6) | 0.2025 (6) | 0.037 (3) | |
C3 | 1.0967 (16) | 1.0481 (6) | 0.2453 (6) | 0.030 (2) | |
C4 | 1.2892 (16) | 1.0843 (6) | 0.2844 (6) | 0.029 (2) | |
C5 | 1.4084 (15) | 1.0280 (6) | 0.3344 (6) | 0.038 (3) | |
H5A | 1.4370 | 0.9813 | 0.2994 | 0.056* | |
H5B | 1.3379 | 1.0023 | 0.3770 | 0.056* | |
H5C | 1.5286 | 1.0633 | 0.3596 | 0.056* | |
C6 | 1.0238 (14) | 0.9527 (5) | 0.2482 (5) | 0.0212 (18) | |
C7 | 1.1014 (16) | 0.8911 (6) | 0.2087 (6) | 0.034 (3) | |
H7 | 1.2034 | 0.9084 | 0.1784 | 0.040* | |
C8 | 1.0298 (16) | 0.8030 (6) | 0.2134 (6) | 0.032 (2) | |
H8 | 1.0889 | 0.7608 | 0.1880 | 0.038* | |
C9 | 0.8082 (14) | 0.8368 (6) | 0.2889 (7) | 0.033 (2) | |
H9 | 0.7025 | 0.8183 | 0.3169 | 0.039* | |
C10 | 0.8731 (14) | 0.9235 (6) | 0.2895 (7) | 0.031 (2) | |
H10 | 0.8153 | 0.9637 | 0.3181 | 0.037* | |
C11 | 0.0715 (15) | 0.1332 (7) | 0.4622 (8) | 0.043 (3) | |
H11A | 0.1703 | 0.1630 | 0.5048 | 0.064* | |
H11B | 0.0929 | 0.1565 | 0.4093 | 0.064* | |
H11C | 0.0782 | 0.0705 | 0.4610 | 0.064* | |
C12 | −0.1170 (16) | 0.1471 (6) | 0.4795 (7) | 0.033 (3) | |
C13 | −0.1977 (14) | 0.2205 (5) | 0.4578 (5) | 0.022 (2) | |
C14 | −0.3749 (14) | 0.2287 (6) | 0.4788 (6) | 0.022 (2) | |
C15 | −0.4769 (13) | 0.3058 (5) | 0.4583 (6) | 0.022 (2) | |
H15A | −0.5735 | 0.2905 | 0.4102 | 0.033* | |
H15B | −0.3837 | 0.3556 | 0.4471 | 0.033* | |
H15C | −0.5396 | 0.3211 | 0.5044 | 0.033* | |
C16 | −0.0932 (13) | 0.2901 (5) | 0.4113 (5) | 0.0155 (19) | |
C17 | −0.1302 (14) | 0.2923 (6) | 0.3276 (5) | 0.024 (2) | |
H17 | −0.2247 | 0.2496 | 0.2976 | 0.029* | |
C18 | −0.0297 (14) | 0.3568 (6) | 0.2879 (6) | 0.028 (2) | |
H18 | −0.0568 | 0.3560 | 0.2302 | 0.034* | |
C19 | 0.1390 (12) | 0.4175 (6) | 0.4061 (5) | 0.018 (2) | |
H19 | 0.2369 | 0.4603 | 0.4341 | 0.022* | |
C20 | 0.0430 (13) | 0.3568 (6) | 0.4512 (5) | 0.021 (2) | |
H20 | 0.0692 | 0.3603 | 0.5090 | 0.025* | |
C21 | 0.8654 (14) | 0.3226 (6) | 0.0267 (6) | 0.026 (2) | |
H21A | 0.9619 | 0.3053 | 0.0686 | 0.039* | |
H21B | 0.8044 | 0.3683 | 0.0494 | 0.039* | |
H21C | 0.9273 | 0.3448 | −0.0195 | 0.039* | |
C22 | 0.7181 (14) | 0.2459 (5) | −0.0012 (5) | 0.019 (2) | |
C23 | 0.5285 (13) | 0.2351 (5) | 0.0194 (5) | 0.0155 (19) | |
C24 | 0.3999 (15) | 0.1602 (6) | −0.0107 (7) | 0.033 (3) | |
C25A | 0.187 (3) | 0.159 (3) | −0.008 (3) | 0.036 (10)* | 0.40 (7) |
H25A | 0.1164 | 0.1021 | −0.0281 | 0.053* | 0.40 (7) |
H25B | 0.1417 | 0.2046 | −0.0422 | 0.053* | 0.40 (7) |
H25C | 0.1666 | 0.1703 | 0.0483 | 0.053* | 0.40 (7) |
C25B | 0.205 (3) | 0.1342 (17) | 0.0178 (17) | 0.029 (6)* | 0.60 (7) |
H25D | 0.1050 | 0.1219 | −0.0296 | 0.043* | 0.60 (7) |
H25E | 0.1768 | 0.1821 | 0.0515 | 0.043* | 0.60 (7) |
H25F | 0.2071 | 0.0820 | 0.0499 | 0.043* | 0.60 (7) |
C26 | 0.4665 (12) | 0.3030 (6) | 0.0703 (6) | 0.018 (2) | |
C27 | 0.4847 (14) | 0.2987 (6) | 0.1546 (5) | 0.023 (2) | |
H27 | 0.5378 | 0.2520 | 0.1804 | 0.028* | |
C28 | 0.4274 (14) | 0.3606 (6) | 0.2001 (6) | 0.025 (2) | |
H28 | 0.4453 | 0.3564 | 0.2576 | 0.030* | |
C29 | 0.3335 (13) | 0.4330 (6) | 0.0888 (6) | 0.020 (2) | |
H29 | 0.2820 | 0.4811 | 0.0651 | 0.024* | |
C30 | 0.3894 (13) | 0.3737 (6) | 0.0376 (5) | 0.021 (2) | |
H30 | 0.3753 | 0.3811 | −0.0194 | 0.025* | |
Atomic displacement parameters (Å2) top | U11 | U22 | U33 | U12 | U13 | U23 |
Cd1 | 0.0144 (3) | 0.0157 (3) | 0.0173 (3) | 0.0039 (3) | 0.0031 (2) | 0.0010 (3) |
Cd2 | 0.0145 (3) | 0.0175 (3) | 0.0135 (3) | 0.0039 (3) | 0.0033 (2) | 0.0007 (3) |
Br1 | 0.0146 (5) | 0.0223 (4) | 0.0152 (4) | 0.0017 (4) | 0.0007 (4) | 0.0043 (4) |
Br2 | 0.0155 (5) | 0.0208 (4) | 0.0181 (4) | 0.0039 (4) | 0.0034 (4) | 0.0060 (4) |
Br3 | 0.0165 (5) | 0.0218 (4) | 0.0153 (4) | 0.0061 (4) | 0.0005 (4) | −0.0011 (4) |
Br4 | 0.0154 (5) | 0.0246 (4) | 0.0158 (5) | 0.0043 (4) | 0.0011 (4) | −0.0040 (4) |
O1 | 0.071 (7) | 0.018 (3) | 0.047 (5) | 0.006 (4) | −0.013 (4) | 0.006 (3) |
O2 | 0.063 (6) | 0.018 (3) | 0.034 (4) | −0.004 (3) | −0.008 (4) | 0.003 (3) |
O3 | 0.031 (5) | 0.037 (4) | 0.050 (5) | −0.002 (3) | 0.011 (4) | 0.021 (4) |
O4 | 0.029 (4) | 0.034 (4) | 0.033 (4) | −0.003 (3) | 0.004 (4) | 0.015 (3) |
O5 | 0.028 (4) | 0.030 (4) | 0.027 (4) | 0.008 (3) | 0.009 (3) | −0.009 (3) |
O6 | 0.035 (5) | 0.028 (4) | 0.062 (6) | 0.006 (3) | 0.002 (4) | −0.026 (4) |
N1 | 0.027 (5) | 0.017 (3) | 0.021 (4) | 0.008 (3) | 0.001 (4) | 0.001 (3) |
N2 | 0.018 (4) | 0.022 (4) | 0.015 (4) | −0.002 (3) | 0.001 (3) | 0.003 (3) |
N3 | 0.019 (4) | 0.014 (3) | 0.015 (4) | 0.002 (3) | 0.010 (3) | 0.004 (3) |
C1 | 0.069 (9) | 0.023 (5) | 0.057 (8) | 0.004 (6) | −0.023 (7) | 0.011 (5) |
C2 | 0.058 (8) | 0.022 (5) | 0.027 (6) | 0.004 (5) | −0.006 (5) | −0.006 (4) |
C3 | 0.035 (6) | 0.027 (5) | 0.028 (6) | 0.002 (5) | 0.004 (5) | 0.005 (4) |
C4 | 0.044 (7) | 0.027 (5) | 0.016 (5) | 0.006 (5) | 0.000 (5) | 0.002 (4) |
C5 | 0.037 (7) | 0.035 (6) | 0.037 (6) | −0.010 (5) | 0.009 (5) | 0.003 (5) |
C6 | 0.030 (5) | 0.014 (3) | 0.020 (5) | 0.011 (3) | −0.005 (4) | 0.004 (3) |
C7 | 0.051 (7) | 0.018 (4) | 0.035 (6) | −0.005 (4) | 0.029 (5) | −0.004 (4) |
C8 | 0.047 (7) | 0.018 (3) | 0.033 (6) | 0.004 (5) | 0.022 (5) | −0.001 (4) |
C9 | 0.024 (6) | 0.023 (4) | 0.052 (7) | 0.008 (4) | 0.006 (5) | −0.005 (5) |
C10 | 0.021 (5) | 0.022 (4) | 0.052 (7) | 0.011 (4) | 0.008 (4) | −0.012 (4) |
C11 | 0.023 (6) | 0.034 (6) | 0.072 (9) | 0.012 (5) | −0.002 (6) | 0.012 (6) |
C12 | 0.031 (6) | 0.022 (5) | 0.047 (7) | 0.002 (4) | 0.010 (5) | 0.004 (5) |
C13 | 0.034 (6) | 0.018 (4) | 0.014 (5) | 0.007 (4) | 0.000 (4) | 0.001 (4) |
C14 | 0.026 (6) | 0.019 (4) | 0.023 (5) | 0.006 (4) | 0.007 (4) | 0.001 (4) |
C15 | 0.023 (5) | 0.021 (5) | 0.020 (5) | −0.003 (4) | 0.002 (4) | 0.002 (4) |
C16 | 0.022 (5) | 0.007 (4) | 0.018 (5) | 0.005 (3) | 0.002 (4) | 0.000 (3) |
C17 | 0.023 (6) | 0.028 (5) | 0.016 (5) | −0.009 (4) | −0.005 (4) | 0.006 (4) |
C18 | 0.033 (6) | 0.036 (6) | 0.011 (5) | −0.001 (5) | −0.004 (4) | 0.001 (4) |
C19 | 0.008 (4) | 0.022 (4) | 0.023 (5) | −0.006 (4) | 0.004 (4) | −0.004 (4) |
C20 | 0.025 (5) | 0.028 (5) | 0.009 (4) | 0.001 (4) | 0.005 (4) | 0.002 (4) |
C21 | 0.025 (6) | 0.030 (5) | 0.026 (5) | 0.009 (4) | 0.010 (4) | −0.004 (4) |
C22 | 0.028 (6) | 0.013 (4) | 0.018 (5) | 0.008 (4) | 0.001 (4) | 0.004 (4) |
C23 | 0.024 (5) | 0.009 (4) | 0.016 (4) | 0.007 (4) | 0.007 (4) | 0.001 (3) |
C24 | 0.018 (6) | 0.031 (5) | 0.049 (7) | 0.009 (4) | −0.004 (5) | −0.014 (5) |
C26 | 0.004 (4) | 0.024 (5) | 0.025 (5) | 0.003 (4) | 0.000 (4) | −0.001 (4) |
C27 | 0.033 (6) | 0.022 (5) | 0.014 (5) | 0.012 (4) | −0.008 (4) | −0.001 (4) |
C28 | 0.031 (6) | 0.026 (5) | 0.019 (5) | 0.006 (4) | 0.000 (4) | 0.004 (4) |
C29 | 0.016 (5) | 0.019 (4) | 0.025 (5) | 0.009 (4) | 0.001 (4) | 0.000 (4) |
C30 | 0.026 (6) | 0.025 (5) | 0.014 (5) | 0.011 (4) | 0.004 (4) | 0.008 (4) |
Geometric parameters (Å, º) top
Cd1—N1 | 2.315 (7) | C9—H9 | 0.9500 |
Cd1—Br1 | 2.6240 (11) | C10—H10 | 0.9500 |
Cd1—Br3i | 2.6314 (11) | C11—C12 | 1.457 (14) |
Cd1—Br2 | 2.7384 (12) | C11—H11A | 0.9800 |
Cd1—Br4i | 2.7512 (12) | C11—H11B | 0.9800 |
Cd2—N3 | 2.345 (7) | C11—H11C | 0.9800 |
Cd2—N2 | 2.349 (7) | C12—C13 | 1.383 (13) |
Cd2—Br4 | 2.6858 (11) | C13—C14 | 1.378 (13) |
Cd2—Br2 | 2.7124 (10) | C13—C16 | 1.507 (12) |
Cd2—Br1 | 2.8461 (12) | C14—C15 | 1.512 (12) |
Cd2—Br3 | 2.8562 (12) | C15—H15A | 0.9800 |
Br3—Cd1ii | 2.6314 (11) | C15—H15B | 0.9800 |
Br4—Cd1ii | 2.7512 (12) | C15—H15C | 0.9800 |
O1—C2 | 1.323 (12) | C16—C17 | 1.379 (12) |
O1—H1D | 0.84 (2) | C16—C20 | 1.396 (12) |
O2—C4 | 1.242 (11) | C17—C18 | 1.376 (12) |
O3—C12 | 1.297 (11) | C17—H17 | 0.9500 |
O4—C14 | 1.289 (11) | C18—H18 | 0.9500 |
O4—H4D | 0.84 (2) | C19—C20 | 1.376 (11) |
O5—C22 | 1.296 (10) | C19—H19 | 0.9500 |
O5—H5D | 0.85 (2) | C20—H20 | 0.9500 |
O6—C24 | 1.301 (11) | C21—C22 | 1.484 (12) |
N1—C8 | 1.324 (12) | C21—H21A | 0.9800 |
N1—C9 | 1.325 (11) | C21—H21B | 0.9800 |
N2—C18 | 1.317 (11) | C21—H21C | 0.9800 |
N2—C19 | 1.351 (11) | C22—C23 | 1.425 (12) |
N3—C29 | 1.325 (11) | C23—C24 | 1.403 (12) |
N3—C28 | 1.339 (11) | C23—C26 | 1.491 (11) |
C1—C2 | 1.504 (15) | C24—C25A | 1.520 (19) |
C1—H1A | 0.9800 | C24—C25B | 1.531 (16) |
C1—H1B | 0.9800 | C25A—H25A | 0.9800 |
C1—H1C | 0.9800 | C25A—H25B | 0.9800 |
C2—C3 | 1.371 (14) | C25A—H25C | 0.9800 |
C3—C4 | 1.458 (15) | C25B—H25D | 0.9800 |
C3—C6 | 1.497 (11) | C25B—H25E | 0.9800 |
C4—C5 | 1.495 (14) | C25B—H25F | 0.9800 |
C5—H5A | 0.9800 | C26—C30 | 1.387 (12) |
C5—H5B | 0.9800 | C26—C27 | 1.391 (12) |
C5—H5C | 0.9800 | C27—C28 | 1.353 (12) |
C6—C7 | 1.371 (12) | C27—H27 | 0.9500 |
C6—C10 | 1.378 (13) | C28—H28 | 0.9500 |
C7—C8 | 1.394 (12) | C29—C30 | 1.376 (12) |
C7—H7 | 0.9500 | C29—H29 | 0.9500 |
C8—H8 | 0.9500 | C30—H30 | 0.9500 |
C9—C10 | 1.355 (12) | | |
| | | |
N1—Cd1—Br1 | 132.91 (18) | H11A—C11—H11B | 109.5 |
N1—Cd1—Br3i | 112.59 (18) | C12—C11—H11C | 109.5 |
Br1—Cd1—Br3i | 114.44 (3) | H11A—C11—H11C | 109.5 |
N1—Cd1—Br2 | 83.7 (2) | H11B—C11—H11C | 109.5 |
Br1—Cd1—Br2 | 91.20 (4) | O3—C12—C13 | 120.5 (10) |
Br3i—Cd1—Br2 | 99.21 (4) | O3—C12—C11 | 115.9 (9) |
N1—Cd1—Br4i | 81.2 (2) | C13—C12—C11 | 123.6 (9) |
Br1—Cd1—Br4i | 95.13 (4) | C14—C13—C12 | 119.2 (9) |
Br3i—Cd1—Br4i | 91.55 (4) | C14—C13—C16 | 120.6 (8) |
Br2—Cd1—Br4i | 163.98 (3) | C12—C13—C16 | 120.2 (9) |
N3—Cd2—N2 | 89.4 (2) | O4—C14—C13 | 123.0 (9) |
N3—Cd2—Br4 | 176.55 (16) | O4—C14—C15 | 113.2 (8) |
N2—Cd2—Br4 | 87.25 (18) | C13—C14—C15 | 123.8 (8) |
N3—Cd2—Br2 | 88.95 (16) | C14—C15—H15A | 109.5 |
N2—Cd2—Br2 | 177.7 (2) | C14—C15—H15B | 109.5 |
Br4—Cd2—Br2 | 94.40 (3) | H15A—C15—H15B | 109.5 |
N3—Cd2—Br1 | 89.62 (19) | C14—C15—H15C | 109.5 |
N2—Cd2—Br1 | 91.23 (19) | H15A—C15—H15C | 109.5 |
Br4—Cd2—Br1 | 91.39 (3) | H15B—C15—H15C | 109.5 |
Br2—Cd2—Br1 | 87.13 (3) | C17—C16—C20 | 116.7 (8) |
N3—Cd2—Br3 | 90.89 (19) | C17—C16—C13 | 121.9 (8) |
N2—Cd2—Br3 | 90.18 (19) | C20—C16—C13 | 121.4 (8) |
Br4—Cd2—Br3 | 88.19 (3) | C18—C17—C16 | 119.7 (8) |
Br2—Cd2—Br3 | 91.47 (3) | C18—C17—H17 | 120.1 |
Br1—Cd2—Br3 | 178.51 (3) | C16—C17—H17 | 120.1 |
Cd1—Br1—Cd2 | 89.36 (3) | N2—C18—C17 | 124.6 (9) |
Cd2—Br2—Cd1 | 89.86 (3) | N2—C18—H18 | 117.7 |
Cd1ii—Br3—Cd2 | 88.98 (3) | C17—C18—H18 | 117.7 |
Cd2—Br4—Cd1ii | 90.13 (3) | N2—C19—C20 | 123.5 (8) |
C2—O1—H1D | 92 (9) | N2—C19—H19 | 118.2 |
C14—O4—H4D | 102 (8) | C20—C19—H19 | 118.2 |
C22—O5—H5D | 100 (7) | C19—C20—C16 | 119.4 (8) |
C8—N1—C9 | 117.1 (8) | C19—C20—H20 | 120.3 |
C8—N1—Cd1 | 117.7 (6) | C16—C20—H20 | 120.3 |
C9—N1—Cd1 | 125.0 (6) | C22—C21—H21A | 109.5 |
C18—N2—C19 | 116.0 (7) | C22—C21—H21B | 109.5 |
C18—N2—Cd2 | 123.4 (6) | H21A—C21—H21B | 109.5 |
C19—N2—Cd2 | 120.6 (5) | C22—C21—H21C | 109.5 |
C29—N3—C28 | 115.9 (8) | H21A—C21—H21C | 109.5 |
C29—N3—Cd2 | 123.3 (6) | H21B—C21—H21C | 109.5 |
C28—N3—Cd2 | 120.6 (6) | O5—C22—C23 | 118.8 (8) |
C2—C1—H1A | 109.5 | O5—C22—C21 | 117.7 (8) |
C2—C1—H1B | 109.5 | C23—C22—C21 | 123.4 (8) |
H1A—C1—H1B | 109.5 | C24—C23—C22 | 118.8 (8) |
C2—C1—H1C | 109.5 | C24—C23—C26 | 120.6 (8) |
H1A—C1—H1C | 109.5 | C22—C23—C26 | 120.6 (7) |
H1B—C1—H1C | 109.5 | O6—C24—C23 | 121.0 (9) |
O1—C2—C3 | 122.9 (10) | O6—C24—C25A | 118.6 (13) |
O1—C2—C1 | 112.7 (9) | C23—C24—C25A | 118.6 (15) |
C3—C2—C1 | 124.4 (9) | O6—C24—C25B | 114.8 (10) |
C2—C3—C4 | 117.7 (9) | C23—C24—C25B | 123.4 (10) |
C2—C3—C6 | 121.6 (10) | C24—C25A—H25A | 109.5 |
C4—C3—C6 | 120.5 (9) | C24—C25A—H25B | 109.5 |
O2—C4—C3 | 121.5 (10) | H25A—C25A—H25B | 109.5 |
O2—C4—C5 | 118.2 (10) | C24—C25A—H25C | 109.5 |
C3—C4—C5 | 120.0 (9) | H25A—C25A—H25C | 109.5 |
C4—C5—H5A | 109.5 | H25B—C25A—H25C | 109.5 |
C4—C5—H5B | 109.5 | C24—C25B—H25D | 109.5 |
H5A—C5—H5B | 109.5 | C24—C25B—H25E | 109.5 |
C4—C5—H5C | 109.5 | H25D—C25B—H25E | 109.5 |
H5A—C5—H5C | 109.5 | C24—C25B—H25F | 109.5 |
H5B—C5—H5C | 109.5 | H25D—C25B—H25F | 109.5 |
C7—C6—C10 | 117.2 (8) | H25E—C25B—H25F | 109.5 |
C7—C6—C3 | 121.6 (9) | C30—C26—C27 | 116.1 (8) |
C10—C6—C3 | 121.2 (8) | C30—C26—C23 | 122.9 (8) |
C6—C7—C8 | 119.7 (9) | C27—C26—C23 | 120.9 (8) |
C6—C7—H7 | 120.1 | C28—C27—C26 | 120.4 (9) |
C8—C7—H7 | 120.1 | C28—C27—H27 | 119.8 |
N1—C8—C7 | 122.2 (9) | C26—C27—H27 | 119.8 |
N1—C8—H8 | 118.9 | N3—C28—C27 | 123.8 (9) |
C7—C8—H8 | 118.9 | N3—C28—H28 | 118.1 |
N1—C9—C10 | 124.3 (10) | C27—C28—H28 | 118.1 |
N1—C9—H9 | 117.8 | N3—C29—C30 | 124.4 (8) |
C10—C9—H9 | 117.8 | N3—C29—H29 | 117.8 |
C9—C10—C6 | 119.4 (8) | C30—C29—H29 | 117.8 |
C9—C10—H10 | 120.3 | C29—C30—C26 | 119.3 (8) |
C6—C10—H10 | 120.3 | C29—C30—H30 | 120.4 |
C12—C11—H11A | 109.5 | C26—C30—H30 | 120.4 |
C12—C11—H11B | 109.5 | | |
Symmetry codes: (i) x+1, y, z; (ii) x−1, y, z. |
Crystal data top
C10H11CdI2NO2 | Dx = 2.573 Mg m−3 |
Mr = 543.41 | Mo Kα radiation, λ = 0.71073 Å |
Orthorhombic, Pbca | Cell parameters from 7521 reflections |
a = 7.1002 (9) Å | θ = 2.8–28.3° |
b = 14.3490 (18) Å | µ = 5.94 mm−1 |
c = 27.540 (4) Å | T = 100 K |
V = 2805.7 (6) Å3 | Rod, colorless |
Z = 8 | 0.27 × 0.07 × 0.03 mm |
F(000) = 1984 | |
Data collection top
CCD area detector diffractometer | 3748 reflections with I > 2σ(I) |
Radiation source: Incoatec microsource, multilayer optics | Rint = 0.047 |
ωs scans | θmax = 30.9°, θmin = 2.8° |
Absorption correction: multi-scan SADABS | h = −9→9 |
Tmin = 0.474, Tmax = 0.746 | k = −20→20 |
39565 measured reflections | l = −38→37 |
4234 independent reflections | |
Refinement top
Refinement on F2 | Primary atom site location: heavy-atom method |
Least-squares matrix: full | Hydrogen site location: mixed |
R[F2 > 2σ(F2)] = 0.024 | H-atom parameters constrained |
wR(F2) = 0.051 | w = 1/[σ2(Fo2) + (0.0191P)2 + 2.0764P]
where P = (Fo2 + 2Fc2)/3 |
S = 1.11 | (Δ/σ)max = 0.001 |
4234 reflections | Δρmax = 0.69 e Å−3 |
147 parameters | Δρmin = −0.59 e Å−3 |
0 restraints | |
Crystal data top
C10H11CdI2NO2 | V = 2805.7 (6) Å3 |
Mr = 543.41 | Z = 8 |
Orthorhombic, Pbca | Mo Kα radiation |
a = 7.1002 (9) Å | µ = 5.94 mm−1 |
b = 14.3490 (18) Å | T = 100 K |
c = 27.540 (4) Å | 0.27 × 0.07 × 0.03 mm |
Data collection top
CCD area detector diffractometer | 4234 independent reflections |
Absorption correction: multi-scan SADABS | 3748 reflections with I > 2σ(I) |
Tmin = 0.474, Tmax = 0.746 | Rint = 0.047 |
39565 measured reflections | |
Refinement top
R[F2 > 2σ(F2)] = 0.024 | 0 restraints |
wR(F2) = 0.051 | H-atom parameters constrained |
S = 1.11 | Δρmax = 0.69 e Å−3 |
4234 reflections | Δρmin = −0.59 e Å−3 |
147 parameters | |
Special details top
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. |
Fractional atomic coordinates and isotropic or equivalent isotropic displacement parameters (Å2) top | x | y | z | Uiso*/Ueq | |
Cd1 | 0.69629 (3) | 0.49466 (2) | 0.21095 (2) | 0.01580 (5) | |
I1 | 0.57192 (2) | 0.44443 (2) | 0.30413 (2) | 0.01675 (5) | |
I2 | 0.55761 (3) | 0.66218 (2) | 0.18766 (2) | 0.02204 (5) | |
O1 | −0.0032 (3) | 0.14714 (17) | 0.02937 (8) | 0.0315 (5) | |
O2 | 0.2705 (4) | 0.04421 (15) | 0.03192 (8) | 0.0288 (5) | |
H2A | 0.1606 | 0.0785 | 0.0273 | 0.035* | |
N1 | 0.5538 (3) | 0.38827 (16) | 0.16261 (9) | 0.0171 (5) | |
C1 | −0.0167 (5) | 0.2973 (2) | 0.06472 (12) | 0.0292 (7) | |
H1A | −0.0018 | 0.3130 | 0.0991 | 0.044* | |
H1B | −0.1508 | 0.2896 | 0.0573 | 0.044* | |
H1C | 0.0357 | 0.3475 | 0.0447 | 0.044* | |
C2 | 0.0851 (4) | 0.2083 (2) | 0.05408 (11) | 0.0237 (6) | |
C3 | 0.2730 (4) | 0.1909 (2) | 0.07071 (10) | 0.0204 (6) | |
C4 | 0.3580 (5) | 0.1074 (2) | 0.05812 (10) | 0.0220 (6) | |
C5 | 0.5572 (5) | 0.0814 (2) | 0.07039 (12) | 0.0267 (7) | |
H5A | 0.6217 | 0.1353 | 0.0845 | 0.040* | |
H5B | 0.6230 | 0.0618 | 0.0408 | 0.040* | |
H5C | 0.5569 | 0.0300 | 0.0938 | 0.040* | |
C6 | 0.3708 (4) | 0.25965 (19) | 0.10214 (10) | 0.0164 (5) | |
C7 | 0.4242 (4) | 0.23656 (19) | 0.14947 (10) | 0.0166 (5) | |
H7 | 0.3983 | 0.1762 | 0.1620 | 0.020* | |
C8 | 0.5147 (4) | 0.30172 (19) | 0.17803 (10) | 0.0166 (5) | |
H8 | 0.5509 | 0.2845 | 0.2100 | 0.020* | |
C9 | 0.5022 (4) | 0.4111 (2) | 0.11701 (10) | 0.0189 (6) | |
H9 | 0.5287 | 0.4723 | 0.1057 | 0.023* | |
C10 | 0.4126 (4) | 0.3497 (2) | 0.08606 (10) | 0.0196 (6) | |
H10 | 0.3796 | 0.3686 | 0.0541 | 0.024* | |
Atomic displacement parameters (Å2) top | U11 | U22 | U33 | U12 | U13 | U23 |
Cd1 | 0.01426 (10) | 0.01552 (10) | 0.01762 (10) | 0.00023 (7) | 0.00036 (7) | −0.00089 (7) |
I1 | 0.01327 (9) | 0.02015 (9) | 0.01684 (9) | 0.00166 (7) | −0.00018 (7) | 0.00260 (6) |
I2 | 0.01971 (10) | 0.01640 (9) | 0.03001 (11) | 0.00180 (7) | −0.00241 (8) | 0.00231 (7) |
O1 | 0.0297 (13) | 0.0426 (14) | 0.0223 (11) | −0.0082 (11) | −0.0041 (10) | −0.0091 (10) |
O2 | 0.0389 (14) | 0.0226 (11) | 0.0248 (11) | −0.0087 (10) | 0.0041 (10) | −0.0083 (9) |
N1 | 0.0154 (12) | 0.0163 (11) | 0.0197 (11) | 0.0020 (9) | 0.0012 (9) | −0.0018 (9) |
C1 | 0.0275 (17) | 0.0362 (18) | 0.0239 (16) | 0.0031 (15) | −0.0097 (13) | 0.0005 (13) |
C2 | 0.0250 (16) | 0.0302 (16) | 0.0159 (13) | −0.0052 (13) | −0.0012 (12) | −0.0013 (12) |
C3 | 0.0247 (15) | 0.0214 (14) | 0.0150 (13) | −0.0050 (12) | 0.0009 (11) | −0.0020 (11) |
C4 | 0.0297 (16) | 0.0225 (14) | 0.0139 (13) | −0.0064 (13) | 0.0041 (12) | −0.0016 (11) |
C5 | 0.0353 (19) | 0.0216 (15) | 0.0234 (15) | 0.0016 (13) | 0.0058 (14) | −0.0038 (12) |
C6 | 0.0165 (13) | 0.0166 (12) | 0.0162 (13) | 0.0005 (11) | 0.0034 (10) | −0.0026 (10) |
C7 | 0.0174 (13) | 0.0140 (12) | 0.0183 (13) | 0.0015 (10) | 0.0020 (11) | −0.0008 (10) |
C8 | 0.0178 (14) | 0.0162 (13) | 0.0158 (12) | 0.0030 (11) | −0.0013 (10) | −0.0005 (10) |
C9 | 0.0193 (14) | 0.0172 (13) | 0.0201 (14) | −0.0012 (11) | 0.0032 (11) | 0.0001 (11) |
C10 | 0.0244 (15) | 0.0195 (14) | 0.0150 (13) | −0.0020 (11) | 0.0002 (11) | 0.0003 (11) |
Geometric parameters (Å, º) top
Cd1—N1 | 2.264 (2) | C3—C4 | 1.386 (4) |
Cd1—I2 | 2.6756 (4) | C3—C6 | 1.484 (4) |
Cd1—I1i | 2.7938 (4) | C4—C5 | 1.502 (5) |
Cd1—I1 | 2.8079 (4) | C5—H5A | 0.9800 |
I1—Cd1ii | 2.7938 (4) | C5—H5B | 0.9800 |
O1—C2 | 1.275 (4) | C5—H5C | 0.9800 |
O2—C4 | 1.315 (4) | C6—C7 | 1.397 (4) |
O2—H2A | 0.9311 | C6—C10 | 1.398 (4) |
N1—C8 | 1.341 (4) | C7—C8 | 1.381 (4) |
N1—C9 | 1.349 (4) | C7—H7 | 0.9500 |
C1—C2 | 1.496 (5) | C8—H8 | 0.9500 |
C1—H1A | 0.9800 | C9—C10 | 1.381 (4) |
C1—H1B | 0.9800 | C9—H9 | 0.9500 |
C1—H1C | 0.9800 | C10—H10 | 0.9500 |
C2—C3 | 1.433 (4) | | |
| | | |
N1—Cd1—I2 | 107.48 (6) | O2—C4—C5 | 113.4 (3) |
N1—Cd1—I1i | 99.50 (6) | C3—C4—C5 | 124.7 (3) |
I2—Cd1—I1i | 123.193 (9) | C4—C5—H5A | 109.5 |
N1—Cd1—I1 | 102.93 (6) | C4—C5—H5B | 109.5 |
I2—Cd1—I1 | 109.508 (9) | H5A—C5—H5B | 109.5 |
I1i—Cd1—I1 | 111.711 (9) | C4—C5—H5C | 109.5 |
Cd1ii—I1—Cd1 | 95.629 (8) | H5A—C5—H5C | 109.5 |
C4—O2—H2A | 96.1 | H5B—C5—H5C | 109.5 |
C8—N1—C9 | 117.6 (2) | C7—C6—C10 | 117.2 (3) |
C8—N1—Cd1 | 122.05 (19) | C7—C6—C3 | 120.9 (2) |
C9—N1—Cd1 | 120.33 (19) | C10—C6—C3 | 121.9 (3) |
C2—C1—H1A | 109.5 | C8—C7—C6 | 119.8 (3) |
C2—C1—H1B | 109.5 | C8—C7—H7 | 120.1 |
H1A—C1—H1B | 109.5 | C6—C7—H7 | 120.1 |
C2—C1—H1C | 109.5 | N1—C8—C7 | 122.9 (3) |
H1A—C1—H1C | 109.5 | N1—C8—H8 | 118.6 |
H1B—C1—H1C | 109.5 | C7—C8—H8 | 118.6 |
O1—C2—C3 | 120.6 (3) | N1—C9—C10 | 123.0 (3) |
O1—C2—C1 | 117.0 (3) | N1—C9—H9 | 118.5 |
C3—C2—C1 | 122.4 (3) | C10—C9—H9 | 118.5 |
C4—C3—C2 | 118.4 (3) | C9—C10—C6 | 119.5 (3) |
C4—C3—C6 | 121.1 (3) | C9—C10—H10 | 120.3 |
C2—C3—C6 | 120.4 (3) | C6—C10—H10 | 120.3 |
O2—C4—C3 | 121.9 (3) | | |
Symmetry codes: (i) x+1/2, y, −z+1/2; (ii) x−1/2, y, −z+1/2. |
Crystal data top
C20H22CdI2N2O4 | Dx = 2.031 Mg m−3 |
Mr = 720.59 | Mo Kα radiation, λ = 0.71073 Å |
Orthorhombic, Pca21 | Cell parameters from 9971 reflections |
a = 13.5307 (3) Å | θ = 3.0–27.5° |
b = 7.0913 (7) Å | µ = 3.57 mm−1 |
c = 49.110 (2) Å | T = 100 K |
V = 4712.1 (5) Å3 | Block, colorless |
Z = 8 | 0.25 × 0.13 × 0.11 mm |
F(000) = 2736 | |
Data collection top
CCD area detector diffractometer | 12009 reflections with I > 2σ(I) |
Radiation source: Incoatec microsource | Rint = 0.051 |
ω scans | θmax = 31.0°, θmin = 0.8° |
Absorption correction: multi-scan SADABS | h = −19→19 |
Tmin = 0.522, Tmax = 0.746 | k = −9→10 |
67491 measured reflections | l = −69→69 |
14053 independent reflections | |
Refinement top
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)] = 0.038 | w = 1/[σ2(Fo2) + (0.0227P)2 + 4.6056P]
where P = (Fo2 + 2Fc2)/3 |
wR(F2) = 0.076 | (Δ/σ)max = 0.003 |
S = 1.09 | Δρmax = 1.29 e Å−3 |
14053 reflections | Δρmin = −1.11 e Å−3 |
545 parameters | Absolute structure: Refined as an inversion twin. |
5 restraints | Absolute structure parameter: 0.41 (3) |
Primary atom site location: heavy-atom method | |
Crystal data top
C20H22CdI2N2O4 | V = 4712.1 (5) Å3 |
Mr = 720.59 | Z = 8 |
Orthorhombic, Pca21 | Mo Kα radiation |
a = 13.5307 (3) Å | µ = 3.57 mm−1 |
b = 7.0913 (7) Å | T = 100 K |
c = 49.110 (2) Å | 0.25 × 0.13 × 0.11 mm |
Data collection top
CCD area detector diffractometer | 14053 independent reflections |
Absorption correction: multi-scan SADABS | 12009 reflections with I > 2σ(I) |
Tmin = 0.522, Tmax = 0.746 | Rint = 0.051 |
67491 measured reflections | |
Refinement top
R[F2 > 2σ(F2)] = 0.038 | H atoms treated by a mixture of independent and constrained refinement |
wR(F2) = 0.076 | Δρmax = 1.29 e Å−3 |
S = 1.09 | Δρmin = −1.11 e Å−3 |
14053 reflections | Absolute structure: Refined as an inversion twin. |
545 parameters | Absolute structure parameter: 0.41 (3) |
5 restraints | |
Special details top
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. Refined as a 2-component inversion twin. |
Fractional atomic coordinates and isotropic or equivalent isotropic displacement parameters (Å2) top | x | y | z | Uiso*/Ueq | |
Cd1 | 0.30627 (4) | 0.36841 (8) | 0.64474 (2) | 0.02432 (12) | |
Cd2 | 0.28575 (4) | 0.87015 (8) | 0.89541 (2) | 0.02364 (12) | |
I1 | 0.43978 (4) | 0.55273 (8) | 0.67561 (2) | 0.03312 (13) | |
I2 | 0.17999 (4) | 0.56014 (9) | 0.61261 (2) | 0.03726 (14) | |
I3 | 0.41806 (4) | 1.05371 (8) | 0.86404 (2) | 0.03288 (13) | |
I4 | 0.15884 (4) | 1.06226 (9) | 0.92741 (2) | 0.03673 (14) | |
O1 | 0.6759 (5) | −0.2054 (11) | 0.52992 (16) | 0.0421 (17) | |
H2D | 0.611 (7) | −0.405 (14) | 0.532 (2) | 0.063* | |
O2 | 0.5705 (5) | −0.4815 (11) | 0.53894 (16) | 0.0404 (18) | |
O3 | −0.0596 (4) | −0.3191 (10) | 0.75141 (15) | 0.0394 (17) | |
O4 | 0.0988 (5) | −0.4791 (9) | 0.75788 (15) | 0.0382 (16) | |
H4D | 0.037 (2) | −0.468 (13) | 0.7594 (19) | 0.03 (3)* | |
O5 | 0.6556 (5) | 0.2950 (11) | 1.00989 (15) | 0.0408 (17) | |
O6 | 0.5501 (6) | 0.0203 (11) | 1.00127 (16) | 0.0434 (19) | |
H6D | 0.597 (6) | 0.086 (16) | 1.007 (3) | 0.065* | |
O7 | 0.0672 (5) | 0.0308 (9) | 0.78276 (16) | 0.0328 (15) | |
O8 | −0.0892 (4) | 0.1927 (10) | 0.79063 (15) | 0.0359 (15) | |
H8D | −0.042 (5) | 0.120 (12) | 0.787 (2) | 0.054* | |
N1 | 0.3794 (5) | 0.1445 (9) | 0.61770 (14) | 0.0241 (14) | |
N2 | 0.2219 (4) | 0.1639 (9) | 0.67232 (15) | 0.0217 (14) | |
N3 | 0.3581 (5) | 0.6455 (10) | 0.92216 (15) | 0.0256 (15) | |
N4 | 0.2018 (4) | 0.6680 (9) | 0.86758 (16) | 0.0222 (14) | |
C1 | 0.6432 (7) | 0.1010 (14) | 0.5479 (2) | 0.038 (2) | |
H1A | 0.5812 | 0.1698 | 0.5450 | 0.057* | |
H1B | 0.6912 | 0.1380 | 0.5339 | 0.057* | |
H1C | 0.6696 | 0.1311 | 0.5660 | 0.057* | |
C2 | 0.6240 (7) | −0.1082 (14) | 0.5460 (2) | 0.037 (2) | |
C3 | 0.5440 (6) | −0.1901 (13) | 0.56074 (18) | 0.0281 (18) | |
C4 | 0.5199 (7) | −0.3763 (14) | 0.55600 (19) | 0.034 (2) | |
C5 | 0.4363 (7) | −0.4761 (15) | 0.5697 (3) | 0.044 (3) | |
H5A | 0.3922 | −0.5294 | 0.5559 | 0.067* | |
H5B | 0.3995 | −0.3866 | 0.5810 | 0.067* | |
H5C | 0.4625 | −0.5777 | 0.5811 | 0.067* | |
C6 | 0.4846 (6) | −0.0776 (12) | 0.58078 (18) | 0.0269 (18) | |
C7 | 0.3939 (7) | −0.0039 (16) | 0.5746 (2) | 0.040 (2) | |
H7 | 0.3650 | −0.0290 | 0.5574 | 0.048* | |
C8 | 0.3441 (6) | 0.1059 (16) | 0.5931 (2) | 0.036 (2) | |
H8 | 0.2816 | 0.1565 | 0.5881 | 0.043* | |
C9 | 0.4664 (7) | 0.0725 (16) | 0.6240 (2) | 0.044 (3) | |
H9 | 0.4929 | 0.0999 | 0.6415 | 0.052* | |
C10 | 0.5207 (8) | −0.0394 (16) | 0.60691 (19) | 0.045 (3) | |
H10 | 0.5822 | −0.0903 | 0.6127 | 0.054* | |
C11 | −0.0823 (6) | −0.0549 (14) | 0.7223 (2) | 0.041 (2) | |
H11A | −0.0834 | 0.0565 | 0.7341 | 0.062* | |
H11B | −0.1496 | −0.1036 | 0.7202 | 0.062* | |
H11C | −0.0557 | −0.0204 | 0.7044 | 0.062* | |
C12 | −0.0180 (5) | −0.2046 (12) | 0.73495 (19) | 0.0297 (19) | |
C13 | 0.0834 (5) | −0.2189 (11) | 0.72850 (18) | 0.0248 (17) | |
C14 | 0.1399 (6) | −0.3549 (11) | 0.74132 (17) | 0.0244 (16) | |
C15 | 0.2504 (6) | −0.3671 (12) | 0.74015 (18) | 0.0301 (17) | |
H15A | 0.2739 | −0.3127 | 0.7230 | 0.045* | |
H15B | 0.2708 | −0.4995 | 0.7412 | 0.045* | |
H15C | 0.2789 | −0.2971 | 0.7555 | 0.045* | |
C16 | 0.1296 (5) | −0.0851 (11) | 0.70889 (16) | 0.0208 (15) | |
C17 | 0.1676 (5) | −0.1466 (12) | 0.68429 (18) | 0.0249 (17) | |
H17 | 0.1625 | −0.2759 | 0.6794 | 0.030* | |
C18 | 0.2130 (6) | −0.0205 (12) | 0.66659 (17) | 0.0264 (17) | |
H18 | 0.2387 | −0.0664 | 0.6498 | 0.032* | |
C19 | 0.1833 (5) | 0.2249 (12) | 0.69609 (19) | 0.0251 (17) | |
H19 | 0.1877 | 0.3557 | 0.7001 | 0.030* | |
C20 | 0.1378 (5) | 0.1087 (11) | 0.71490 (18) | 0.0241 (16) | |
H20 | 0.1126 | 0.1583 | 0.7315 | 0.029* | |
C21 | 0.6219 (8) | 0.5991 (14) | 0.9920 (2) | 0.040 (2) | |
H21A | 0.6805 | 0.6298 | 1.0029 | 0.060* | |
H21B | 0.5649 | 0.6691 | 0.9990 | 0.060* | |
H21C | 0.6336 | 0.6340 | 0.9730 | 0.060* | |
C22 | 0.6020 (7) | 0.3943 (13) | 0.99381 (18) | 0.033 (2) | |
C23 | 0.5232 (7) | 0.3076 (14) | 0.97888 (18) | 0.0307 (19) | |
C24 | 0.4990 (7) | 0.1203 (13) | 0.98374 (19) | 0.033 (2) | |
C25 | 0.4174 (7) | 0.0185 (15) | 0.9707 (2) | 0.040 (2) | |
H25A | 0.4234 | 0.0293 | 0.9509 | 0.060* | |
H25B | 0.3544 | 0.0730 | 0.9766 | 0.060* | |
H25C | 0.4200 | −0.1147 | 0.9760 | 0.060* | |
C26 | 0.4647 (6) | 0.4231 (12) | 0.9592 (2) | 0.0294 (19) | |
C27 | 0.5001 (8) | 0.4609 (16) | 0.9336 (2) | 0.048 (3) | |
H27 | 0.5621 | 0.4112 | 0.9280 | 0.058* | |
C28 | 0.4453 (7) | 0.5719 (17) | 0.9157 (2) | 0.042 (3) | |
H28 | 0.4715 | 0.5960 | 0.8981 | 0.051* | |
C29 | 0.3233 (7) | 0.6063 (14) | 0.94684 (19) | 0.033 (2) | |
H29 | 0.2608 | 0.6568 | 0.9518 | 0.040* | |
C30 | 0.3725 (7) | 0.4962 (18) | 0.96585 (19) | 0.041 (2) | |
H30 | 0.3437 | 0.4712 | 0.9831 | 0.049* | |
C31 | 0.2210 (5) | 0.1418 (11) | 0.7982 (2) | 0.0302 (18) | |
H31A | 0.2485 | 0.2437 | 0.7871 | 0.045* | |
H31B | 0.2420 | 0.0198 | 0.7908 | 0.045* | |
H31C | 0.2449 | 0.1543 | 0.8170 | 0.045* | |
C32 | 0.1109 (5) | 0.1532 (11) | 0.79793 (17) | 0.0248 (16) | |
C33 | 0.0576 (5) | 0.2933 (11) | 0.81165 (18) | 0.0204 (15) | |
C34 | −0.0449 (6) | 0.3086 (12) | 0.80657 (18) | 0.0265 (17) | |
C35 | −0.1065 (6) | 0.4602 (13) | 0.8180 (2) | 0.038 (2) | |
H35A | −0.1757 | 0.4390 | 0.8130 | 0.057* | |
H35B | −0.0846 | 0.5820 | 0.8108 | 0.057* | |
H35C | −0.1003 | 0.4605 | 0.8379 | 0.057* | |
C36 | 0.1069 (5) | 0.4259 (11) | 0.83073 (16) | 0.0194 (15) | |
C37 | 0.1160 (5) | 0.6178 (11) | 0.82572 (17) | 0.0216 (15) | |
H37 | 0.0900 | 0.6701 | 0.8094 | 0.026* | |
C38 | 0.1625 (5) | 0.7324 (12) | 0.84434 (17) | 0.0225 (16) | |
H38 | 0.1669 | 0.8635 | 0.8405 | 0.027* | |
C39 | 0.1927 (6) | 0.4820 (12) | 0.87278 (19) | 0.0277 (19) | |
H39 | 0.2197 | 0.4334 | 0.8892 | 0.033* | |
C40 | 0.1458 (5) | 0.3598 (12) | 0.85521 (18) | 0.0236 (17) | |
H40 | 0.1399 | 0.2301 | 0.8598 | 0.028* | |
Atomic displacement parameters (Å2) top | U11 | U22 | U33 | U12 | U13 | U23 |
Cd1 | 0.0314 (3) | 0.0157 (3) | 0.0259 (3) | −0.0011 (2) | 0.0030 (2) | 0.0001 (3) |
Cd2 | 0.0304 (3) | 0.0157 (3) | 0.0248 (3) | −0.0014 (2) | −0.0037 (2) | −0.0009 (3) |
I1 | 0.0279 (2) | 0.0268 (3) | 0.0447 (4) | −0.00334 (19) | −0.0004 (2) | −0.0056 (3) |
I2 | 0.0508 (3) | 0.0254 (3) | 0.0356 (4) | 0.0062 (2) | −0.0060 (3) | 0.0057 (3) |
I3 | 0.0273 (2) | 0.0267 (3) | 0.0446 (4) | −0.00326 (19) | 0.0006 (2) | 0.0056 (3) |
I4 | 0.0498 (3) | 0.0259 (3) | 0.0345 (3) | 0.0060 (2) | 0.0057 (3) | −0.0059 (3) |
O1 | 0.059 (4) | 0.037 (4) | 0.030 (4) | 0.007 (3) | 0.019 (3) | 0.005 (3) |
O2 | 0.066 (5) | 0.027 (4) | 0.029 (4) | 0.002 (3) | 0.014 (3) | −0.006 (3) |
O3 | 0.037 (3) | 0.035 (4) | 0.046 (4) | −0.017 (3) | 0.015 (3) | −0.006 (3) |
O4 | 0.043 (4) | 0.030 (4) | 0.042 (4) | −0.011 (3) | 0.006 (3) | 0.009 (3) |
O5 | 0.060 (4) | 0.034 (4) | 0.029 (4) | 0.005 (3) | −0.019 (3) | 0.000 (3) |
O6 | 0.080 (5) | 0.025 (4) | 0.025 (4) | 0.006 (3) | −0.015 (3) | 0.002 (3) |
O7 | 0.044 (3) | 0.021 (3) | 0.034 (4) | −0.005 (3) | −0.006 (3) | −0.005 (3) |
O8 | 0.024 (3) | 0.036 (4) | 0.048 (4) | −0.009 (2) | −0.010 (3) | 0.000 (3) |
N1 | 0.042 (4) | 0.014 (3) | 0.015 (3) | −0.005 (3) | 0.002 (3) | 0.002 (3) |
N2 | 0.025 (3) | 0.017 (3) | 0.024 (4) | 0.000 (2) | 0.001 (2) | 0.001 (3) |
N3 | 0.032 (3) | 0.021 (4) | 0.024 (4) | 0.003 (3) | −0.004 (3) | −0.001 (3) |
N4 | 0.021 (3) | 0.014 (3) | 0.032 (4) | −0.002 (2) | −0.003 (2) | 0.001 (3) |
C1 | 0.046 (5) | 0.029 (5) | 0.038 (6) | −0.003 (4) | 0.015 (4) | 0.005 (4) |
C2 | 0.051 (5) | 0.034 (5) | 0.025 (5) | −0.003 (4) | 0.005 (4) | 0.010 (4) |
C3 | 0.044 (5) | 0.019 (4) | 0.021 (4) | −0.001 (3) | 0.007 (3) | 0.002 (3) |
C4 | 0.056 (6) | 0.029 (5) | 0.017 (4) | −0.001 (4) | 0.006 (4) | 0.008 (4) |
C5 | 0.067 (7) | 0.024 (6) | 0.042 (7) | −0.011 (4) | 0.011 (5) | −0.005 (5) |
C6 | 0.047 (5) | 0.016 (4) | 0.017 (4) | −0.002 (3) | 0.004 (3) | 0.005 (3) |
C7 | 0.049 (5) | 0.050 (7) | 0.021 (5) | 0.002 (5) | 0.002 (4) | −0.010 (5) |
C8 | 0.026 (4) | 0.052 (7) | 0.028 (5) | 0.002 (4) | −0.003 (3) | −0.007 (5) |
C9 | 0.046 (5) | 0.051 (7) | 0.034 (6) | 0.021 (4) | −0.011 (4) | −0.021 (5) |
C10 | 0.062 (6) | 0.054 (7) | 0.019 (5) | 0.023 (5) | −0.006 (4) | −0.011 (4) |
C11 | 0.021 (4) | 0.039 (6) | 0.063 (7) | −0.003 (4) | 0.008 (4) | −0.008 (5) |
C12 | 0.018 (4) | 0.030 (5) | 0.041 (5) | −0.012 (3) | 0.002 (3) | −0.012 (4) |
C13 | 0.026 (4) | 0.017 (4) | 0.031 (5) | −0.007 (3) | 0.001 (3) | −0.006 (3) |
C14 | 0.032 (4) | 0.015 (4) | 0.026 (4) | −0.005 (3) | 0.003 (3) | 0.000 (3) |
C15 | 0.033 (4) | 0.025 (4) | 0.032 (4) | 0.003 (3) | −0.002 (3) | 0.005 (4) |
C16 | 0.015 (3) | 0.019 (4) | 0.028 (4) | 0.001 (3) | −0.002 (3) | 0.001 (3) |
C17 | 0.030 (4) | 0.019 (4) | 0.026 (4) | 0.002 (3) | 0.001 (3) | 0.000 (3) |
C18 | 0.039 (4) | 0.021 (4) | 0.020 (4) | −0.004 (3) | 0.001 (3) | 0.003 (3) |
C19 | 0.020 (3) | 0.019 (4) | 0.037 (5) | −0.001 (3) | 0.005 (3) | −0.004 (3) |
C20 | 0.022 (3) | 0.020 (4) | 0.031 (4) | −0.003 (3) | 0.002 (3) | −0.007 (3) |
C21 | 0.056 (6) | 0.028 (5) | 0.037 (6) | −0.012 (4) | −0.015 (4) | −0.003 (4) |
C22 | 0.052 (5) | 0.025 (5) | 0.021 (4) | 0.009 (4) | −0.008 (4) | 0.001 (4) |
C23 | 0.048 (5) | 0.027 (5) | 0.017 (4) | 0.000 (4) | −0.008 (3) | 0.000 (3) |
C24 | 0.056 (6) | 0.022 (5) | 0.020 (5) | 0.002 (4) | −0.008 (4) | 0.003 (4) |
C25 | 0.065 (6) | 0.024 (5) | 0.031 (6) | −0.013 (4) | −0.008 (4) | 0.002 (4) |
C26 | 0.043 (5) | 0.019 (5) | 0.026 (5) | −0.001 (3) | −0.009 (4) | −0.003 (4) |
C27 | 0.052 (6) | 0.051 (7) | 0.042 (6) | 0.027 (5) | 0.004 (5) | 0.012 (5) |
C28 | 0.055 (6) | 0.055 (7) | 0.017 (5) | 0.018 (5) | 0.006 (4) | 0.006 (5) |
C29 | 0.042 (5) | 0.040 (6) | 0.017 (4) | 0.002 (4) | 0.001 (3) | −0.004 (4) |
C30 | 0.043 (5) | 0.061 (7) | 0.017 (4) | 0.004 (5) | 0.000 (3) | 0.008 (5) |
C31 | 0.025 (4) | 0.022 (4) | 0.043 (5) | 0.005 (3) | 0.003 (3) | −0.004 (4) |
C32 | 0.030 (4) | 0.017 (4) | 0.028 (4) | −0.005 (3) | −0.003 (3) | 0.004 (3) |
C33 | 0.015 (3) | 0.017 (4) | 0.029 (4) | −0.004 (3) | −0.004 (3) | 0.001 (3) |
C34 | 0.028 (4) | 0.021 (4) | 0.031 (4) | −0.004 (3) | 0.000 (3) | 0.005 (3) |
C35 | 0.018 (4) | 0.032 (5) | 0.064 (7) | 0.001 (3) | 0.007 (4) | −0.001 (5) |
C36 | 0.013 (3) | 0.019 (4) | 0.026 (4) | 0.001 (2) | 0.002 (3) | 0.002 (3) |
C37 | 0.020 (3) | 0.016 (4) | 0.029 (4) | −0.001 (3) | −0.003 (3) | −0.001 (3) |
C38 | 0.021 (3) | 0.019 (4) | 0.028 (4) | −0.002 (3) | −0.004 (3) | −0.001 (3) |
C39 | 0.030 (4) | 0.021 (4) | 0.032 (5) | 0.004 (3) | −0.004 (3) | 0.009 (4) |
C40 | 0.024 (4) | 0.014 (4) | 0.033 (5) | −0.004 (3) | −0.006 (3) | 0.002 (3) |
Geometric parameters (Å, º) top
Cd1—N2 | 2.289 (7) | C13—C14 | 1.382 (11) |
Cd1—N1 | 2.294 (7) | C13—C16 | 1.489 (11) |
Cd1—I2 | 2.6941 (9) | C14—C15 | 1.499 (11) |
Cd1—I1 | 2.6962 (8) | C15—H15A | 0.9800 |
Cd2—N4 | 2.283 (7) | C15—H15B | 0.9800 |
Cd2—N3 | 2.285 (7) | C15—H15C | 0.9800 |
Cd2—I3 | 2.6966 (8) | C16—C17 | 1.384 (11) |
Cd2—I4 | 2.6973 (8) | C16—C20 | 1.410 (11) |
O1—C2 | 1.260 (12) | C17—C18 | 1.391 (11) |
O2—C4 | 1.314 (11) | C17—H17 | 0.9500 |
O2—H2D | 0.84 (3) | C18—H18 | 0.9500 |
O3—C12 | 1.277 (11) | C19—C20 | 1.383 (12) |
O4—C14 | 1.322 (10) | C19—H19 | 0.9500 |
O4—H4D | 0.84 (3) | C20—H20 | 0.9500 |
O5—C22 | 1.282 (11) | C21—C22 | 1.480 (13) |
O6—C24 | 1.313 (11) | C21—H21A | 0.9800 |
O6—H6D | 0.84 (3) | C21—H21B | 0.9800 |
O7—C32 | 1.288 (10) | C21—H21C | 0.9800 |
O8—C34 | 1.284 (11) | C22—C23 | 1.433 (12) |
O8—H8D | 0.85 (3) | C23—C24 | 1.389 (13) |
N1—C9 | 1.320 (11) | C23—C26 | 1.494 (12) |
N1—C8 | 1.328 (12) | C24—C25 | 1.465 (13) |
N2—C18 | 1.343 (11) | C25—H25A | 0.9800 |
N2—C19 | 1.350 (11) | C25—H25B | 0.9800 |
N3—C28 | 1.329 (11) | C25—H25C | 0.9800 |
N3—C29 | 1.330 (11) | C26—C27 | 1.374 (14) |
N4—C38 | 1.339 (11) | C26—C30 | 1.389 (14) |
N4—C39 | 1.349 (11) | C27—C28 | 1.393 (13) |
C1—C2 | 1.509 (13) | C27—H27 | 0.9500 |
C1—H1A | 0.9800 | C28—H28 | 0.9500 |
C1—H1B | 0.9800 | C29—C30 | 1.387 (14) |
C1—H1C | 0.9800 | C29—H29 | 0.9500 |
C2—C3 | 1.427 (12) | C30—H30 | 0.9500 |
C3—C4 | 1.380 (13) | C31—C32 | 1.492 (11) |
C3—C6 | 1.500 (12) | C31—H31A | 0.9800 |
C4—C5 | 1.493 (13) | C31—H31B | 0.9800 |
C5—H5A | 0.9800 | C31—H31C | 0.9800 |
C5—H5B | 0.9800 | C32—C33 | 1.400 (11) |
C5—H5C | 0.9800 | C33—C34 | 1.414 (10) |
C6—C7 | 1.369 (14) | C33—C36 | 1.486 (11) |
C6—C10 | 1.400 (12) | C34—C35 | 1.472 (12) |
C7—C8 | 1.373 (14) | C35—H35A | 0.9800 |
C7—H7 | 0.9500 | C35—H35B | 0.9800 |
C8—H8 | 0.9500 | C35—H35C | 0.9800 |
C9—C10 | 1.370 (13) | C36—C37 | 1.389 (10) |
C9—H9 | 0.9500 | C36—C40 | 1.393 (11) |
C10—H10 | 0.9500 | C37—C38 | 1.376 (11) |
C11—C12 | 1.506 (13) | C37—H37 | 0.9500 |
C11—H11A | 0.9800 | C38—H38 | 0.9500 |
C11—H11B | 0.9800 | C39—C40 | 1.378 (12) |
C11—H11C | 0.9800 | C39—H39 | 0.9500 |
C12—C13 | 1.412 (10) | C40—H40 | 0.9500 |
| | | |
N2—Cd1—N1 | 96.8 (2) | C17—C16—C13 | 121.3 (7) |
N2—Cd1—I2 | 110.49 (15) | C20—C16—C13 | 121.2 (7) |
N1—Cd1—I2 | 106.49 (18) | C16—C17—C18 | 120.5 (8) |
N2—Cd1—I1 | 107.98 (17) | C16—C17—H17 | 119.8 |
N1—Cd1—I1 | 111.83 (17) | C18—C17—H17 | 119.8 |
I2—Cd1—I1 | 120.64 (3) | N2—C18—C17 | 122.3 (8) |
N4—Cd2—N3 | 96.9 (2) | N2—C18—H18 | 118.8 |
N4—Cd2—I3 | 106.95 (18) | C17—C18—H18 | 118.8 |
N3—Cd2—I3 | 112.36 (17) | N2—C19—C20 | 124.0 (8) |
N4—Cd2—I4 | 110.44 (16) | N2—C19—H19 | 118.0 |
N3—Cd2—I4 | 106.84 (18) | C20—C19—H19 | 118.0 |
I3—Cd2—I4 | 120.78 (3) | C19—C20—C16 | 118.4 (8) |
C4—O2—H2D | 104 (9) | C19—C20—H20 | 120.8 |
C14—O4—H4D | 114 (6) | C16—C20—H20 | 120.8 |
C24—O6—H6D | 109 (10) | C22—C21—H21A | 109.5 |
C34—O8—H8D | 100 (7) | C22—C21—H21B | 109.5 |
C9—N1—C8 | 117.1 (8) | H21A—C21—H21B | 109.5 |
C9—N1—Cd1 | 121.0 (6) | C22—C21—H21C | 109.5 |
C8—N1—Cd1 | 120.9 (6) | H21A—C21—H21C | 109.5 |
C18—N2—C19 | 117.3 (7) | H21B—C21—H21C | 109.5 |
C18—N2—Cd1 | 122.5 (5) | O5—C22—C23 | 120.0 (9) |
C19—N2—Cd1 | 120.1 (5) | O5—C22—C21 | 118.2 (9) |
C28—N3—C29 | 116.8 (8) | C23—C22—C21 | 121.8 (8) |
C28—N3—Cd2 | 121.1 (6) | C24—C23—C22 | 119.9 (8) |
C29—N3—Cd2 | 121.2 (6) | C24—C23—C26 | 120.7 (8) |
C38—N4—C39 | 117.3 (7) | C22—C23—C26 | 119.4 (8) |
C38—N4—Cd2 | 119.6 (5) | O6—C24—C23 | 120.3 (9) |
C39—N4—Cd2 | 123.1 (6) | O6—C24—C25 | 114.6 (9) |
C2—C1—H1A | 109.5 | C23—C24—C25 | 125.0 (8) |
C2—C1—H1B | 109.5 | C24—C25—H25A | 109.5 |
H1A—C1—H1B | 109.5 | C24—C25—H25B | 109.5 |
C2—C1—H1C | 109.5 | H25A—C25—H25B | 109.5 |
H1A—C1—H1C | 109.5 | C24—C25—H25C | 109.5 |
H1B—C1—H1C | 109.5 | H25A—C25—H25C | 109.5 |
O1—C2—C3 | 121.2 (9) | H25B—C25—H25C | 109.5 |
O1—C2—C1 | 118.8 (8) | C27—C26—C30 | 117.1 (8) |
C3—C2—C1 | 119.9 (9) | C27—C26—C23 | 121.0 (8) |
C4—C3—C2 | 118.9 (8) | C30—C26—C23 | 121.9 (9) |
C4—C3—C6 | 119.5 (8) | C26—C27—C28 | 120.2 (9) |
C2—C3—C6 | 121.6 (8) | C26—C27—H27 | 119.9 |
O2—C4—C3 | 121.8 (8) | C28—C27—H27 | 119.9 |
O2—C4—C5 | 114.3 (9) | N3—C28—C27 | 122.9 (9) |
C3—C4—C5 | 123.8 (9) | N3—C28—H28 | 118.6 |
C4—C5—H5A | 109.5 | C27—C28—H28 | 118.6 |
C4—C5—H5B | 109.5 | N3—C29—C30 | 124.1 (9) |
H5A—C5—H5B | 109.5 | N3—C29—H29 | 117.9 |
C4—C5—H5C | 109.5 | C30—C29—H29 | 117.9 |
H5A—C5—H5C | 109.5 | C29—C30—C26 | 118.9 (9) |
H5B—C5—H5C | 109.5 | C29—C30—H30 | 120.6 |
C7—C6—C10 | 116.2 (8) | C26—C30—H30 | 120.6 |
C7—C6—C3 | 122.6 (8) | C32—C31—H31A | 109.5 |
C10—C6—C3 | 121.2 (8) | C32—C31—H31B | 109.5 |
C6—C7—C8 | 120.7 (9) | H31A—C31—H31B | 109.5 |
C6—C7—H7 | 119.6 | C32—C31—H31C | 109.5 |
C8—C7—H7 | 119.6 | H31A—C31—H31C | 109.5 |
N1—C8—C7 | 122.8 (8) | H31B—C31—H31C | 109.5 |
N1—C8—H8 | 118.6 | O7—C32—C33 | 121.4 (7) |
C7—C8—H8 | 118.6 | O7—C32—C31 | 115.3 (7) |
N1—C9—C10 | 123.9 (9) | C33—C32—C31 | 123.2 (7) |
N1—C9—H9 | 118.1 | C32—C33—C34 | 118.3 (7) |
C10—C9—H9 | 118.1 | C32—C33—C36 | 121.4 (6) |
C9—C10—C6 | 119.2 (9) | C34—C33—C36 | 120.2 (7) |
C9—C10—H10 | 120.4 | O8—C34—C33 | 121.1 (8) |
C6—C10—H10 | 120.4 | O8—C34—C35 | 115.9 (7) |
C12—C11—H11A | 109.5 | C33—C34—C35 | 123.0 (8) |
C12—C11—H11B | 109.5 | C34—C35—H35A | 109.5 |
H11A—C11—H11B | 109.5 | C34—C35—H35B | 109.5 |
C12—C11—H11C | 109.5 | H35A—C35—H35B | 109.5 |
H11A—C11—H11C | 109.5 | C34—C35—H35C | 109.5 |
H11B—C11—H11C | 109.5 | H35A—C35—H35C | 109.5 |
O3—C12—C13 | 121.7 (9) | H35B—C35—H35C | 109.5 |
O3—C12—C11 | 117.0 (7) | C37—C36—C40 | 116.7 (7) |
C13—C12—C11 | 121.3 (8) | C37—C36—C33 | 123.2 (7) |
C14—C13—C12 | 119.0 (8) | C40—C36—C33 | 120.0 (7) |
C14—C13—C16 | 120.4 (6) | C38—C37—C36 | 120.1 (8) |
C12—C13—C16 | 120.5 (8) | C38—C37—H37 | 120.0 |
O4—C14—C13 | 120.8 (7) | C36—C37—H37 | 120.0 |
O4—C14—C15 | 113.9 (7) | N4—C38—C37 | 123.2 (8) |
C13—C14—C15 | 125.1 (7) | N4—C38—H38 | 118.4 |
C14—C15—H15A | 109.5 | C37—C38—H38 | 118.4 |
C14—C15—H15B | 109.5 | N4—C39—C40 | 122.6 (8) |
H15A—C15—H15B | 109.5 | N4—C39—H39 | 118.7 |
C14—C15—H15C | 109.5 | C40—C39—H39 | 118.7 |
H15A—C15—H15C | 109.5 | C39—C40—C36 | 120.1 (8) |
H15B—C15—H15C | 109.5 | C39—C40—H40 | 119.9 |
C17—C16—C20 | 117.5 (7) | C36—C40—H40 | 119.9 |
Crystal data top
C60H60CdCl2Fe2N6O12·6(CH4O)·6(H2O) | Z = 1 |
Mr = 1652.50 | F(000) = 860 |
Triclinic, P1 | Dx = 1.364 Mg m−3 |
a = 12.1351 (13) Å | Mo Kα radiation, λ = 0.71073 Å |
b = 13.2343 (14) Å | Cell parameters from 4039 reflections |
c = 13.8728 (15) Å | θ = 2.3–25.2° |
α = 91.809 (2)° | µ = 0.76 mm−1 |
β = 109.675 (2)° | T = 100 K |
γ = 104.825 (2)° | Block, red |
V = 2011.0 (4) Å3 | 0.25 × 0.23 × 0.08 mm |
Data collection top
CCD area detector diffractometer | 6746 reflections with I > 2σ(I) |
Radiation source: Incoatec microsource | Rint = 0.050 |
ω scans | θmax = 26.6°, θmin = 2.1° |
Absorption correction: multi-scan SADABS | h = −15→15 |
Tmin = 0.640, Tmax = 0.745 | k = −16→16 |
24575 measured reflections | l = −17→17 |
8416 independent reflections | |
Refinement top
Refinement on F2 | Primary atom site location: heavy-atom method |
Least-squares matrix: full | Hydrogen site location: mixed |
R[F2 > 2σ(F2)] = 0.049 | H-atom parameters constrained |
wR(F2) = 0.130 | w = 1/[σ2(Fo2) + (0.0498P)2 + 4.8255P]
where P = (Fo2 + 2Fc2)/3 |
S = 1.04 | (Δ/σ)max = 0.001 |
8416 reflections | Δρmax = 1.12 e Å−3 |
456 parameters | Δρmin = −0.92 e Å−3 |
0 restraints | |
Crystal data top
C60H60CdCl2Fe2N6O12·6(CH4O)·6(H2O) | γ = 104.825 (2)° |
Mr = 1652.50 | V = 2011.0 (4) Å3 |
Triclinic, P1 | Z = 1 |
a = 12.1351 (13) Å | Mo Kα radiation |
b = 13.2343 (14) Å | µ = 0.76 mm−1 |
c = 13.8728 (15) Å | T = 100 K |
α = 91.809 (2)° | 0.25 × 0.23 × 0.08 mm |
β = 109.675 (2)° | |
Data collection top
CCD area detector diffractometer | 8416 independent reflections |
Absorption correction: multi-scan SADABS | 6746 reflections with I > 2σ(I) |
Tmin = 0.640, Tmax = 0.745 | Rint = 0.050 |
24575 measured reflections | |
Refinement top
R[F2 > 2σ(F2)] = 0.049 | 0 restraints |
wR(F2) = 0.130 | H-atom parameters constrained |
S = 1.04 | Δρmax = 1.12 e Å−3 |
8416 reflections | Δρmin = −0.92 e Å−3 |
456 parameters | |
Special details top
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. |
Fractional atomic coordinates and isotropic or equivalent isotropic displacement parameters (Å2) top | x | y | z | Uiso*/Ueq | |
Cd1 | 0.5000 | 1.0000 | 0.0000 | 0.01625 (11) | |
Fe1 | 0.04526 (5) | 0.39589 (4) | 0.25295 (4) | 0.01632 (13) | |
Cl1 | 0.66071 (9) | 1.03831 (7) | 0.18977 (7) | 0.0242 (2) | |
O1 | −0.1302 (2) | 0.3878 (2) | 0.20690 (19) | 0.0203 (5) | |
O2 | 0.0389 (2) | 0.3848 (2) | 0.39246 (19) | 0.0194 (5) | |
O3 | 0.0580 (2) | 0.41432 (19) | 0.11412 (18) | 0.0179 (5) | |
O4 | 0.1003 (2) | 0.55232 (19) | 0.27828 (19) | 0.0209 (6) | |
O5 | −0.0013 (2) | 0.24041 (19) | 0.2114 (2) | 0.0202 (5) | |
O6 | 0.2166 (2) | 0.38829 (19) | 0.30313 (19) | 0.0202 (5) | |
N1 | −0.4459 (3) | 0.3006 (3) | 0.5008 (3) | 0.0297 (8) | |
N2 | 0.4054 (3) | 0.8368 (2) | 0.0417 (2) | 0.0190 (6) | |
N3 | 0.3676 (3) | 0.0662 (2) | 0.0592 (2) | 0.0202 (7) | |
C1 | −0.3358 (4) | 0.3574 (4) | 0.1891 (3) | 0.0301 (9) | |
H1A | −0.3399 | 0.3819 | 0.1224 | 0.045* | |
H1B | −0.3699 | 0.3997 | 0.2244 | 0.045* | |
H1C | −0.3830 | 0.2831 | 0.1780 | 0.045* | |
C2 | −0.2051 (4) | 0.3690 (3) | 0.2544 (3) | 0.0208 (8) | |
C3 | −0.1727 (3) | 0.3581 (3) | 0.3599 (3) | 0.0187 (7) | |
C4 | −0.0521 (3) | 0.3649 (3) | 0.4234 (3) | 0.0188 (8) | |
C5 | −0.0220 (4) | 0.3478 (3) | 0.5346 (3) | 0.0253 (8) | |
H5A | 0.0665 | 0.3621 | 0.5681 | 0.038* | |
H5B | −0.0621 | 0.2747 | 0.5390 | 0.038* | |
H5C | −0.0508 | 0.3955 | 0.5694 | 0.038* | |
C6 | −0.2693 (3) | 0.3375 (3) | 0.4073 (3) | 0.0210 (8) | |
C7 | −0.3505 (4) | 0.2385 (3) | 0.3943 (3) | 0.0264 (9) | |
H7 | −0.3475 | 0.1813 | 0.3531 | 0.032* | |
C8 | −0.4360 (4) | 0.2240 (3) | 0.4421 (3) | 0.0304 (9) | |
H8 | −0.4907 | 0.1557 | 0.4324 | 0.037* | |
C9 | −0.3676 (4) | 0.3957 (3) | 0.5136 (3) | 0.0284 (9) | |
H9 | −0.3725 | 0.4513 | 0.5556 | 0.034* | |
C10 | −0.2797 (4) | 0.4172 (3) | 0.4689 (3) | 0.0249 (8) | |
H10 | −0.2263 | 0.4864 | 0.4801 | 0.030* | |
C11 | 0.1586 (4) | 0.4620 (3) | −0.0029 (3) | 0.0209 (8) | |
H11A | 0.1041 | 0.3928 | −0.0384 | 0.031* | |
H11B | 0.2435 | 0.4603 | 0.0173 | 0.031* | |
H11C | 0.1451 | 0.5155 | −0.0494 | 0.031* | |
C12 | 0.1324 (3) | 0.4885 (3) | 0.0912 (3) | 0.0163 (7) | |
C13 | 0.1878 (3) | 0.5892 (3) | 0.1493 (3) | 0.0191 (8) | |
C14 | 0.1625 (3) | 0.6173 (3) | 0.2368 (3) | 0.0200 (8) | |
C15 | 0.2056 (4) | 0.7299 (3) | 0.2846 (3) | 0.0327 (10) | |
H15A | 0.1835 | 0.7352 | 0.3459 | 0.049* | |
H15B | 0.1671 | 0.7727 | 0.2346 | 0.049* | |
H15C | 0.2945 | 0.7557 | 0.3044 | 0.049* | |
C16 | 0.2647 (3) | 0.6728 (3) | 0.1107 (3) | 0.0189 (8) | |
C17 | 0.2112 (4) | 0.7224 (3) | 0.0283 (3) | 0.0221 (8) | |
H17 | 0.1251 | 0.7019 | −0.0055 | 0.027* | |
C18 | 0.2842 (4) | 0.8022 (3) | −0.0045 (3) | 0.0218 (8) | |
H18 | 0.2462 | 0.8336 | −0.0625 | 0.026* | |
C19 | 0.4569 (4) | 0.7887 (3) | 0.1207 (3) | 0.0224 (8) | |
H19 | 0.5432 | 0.8116 | 0.1537 | 0.027* | |
C20 | 0.3913 (4) | 0.7069 (3) | 0.1570 (3) | 0.0220 (8) | |
H20 | 0.4323 | 0.6745 | 0.2128 | 0.026* | |
C21 | −0.0097 (4) | 0.0817 (3) | 0.1240 (4) | 0.0325 (10) | |
H21A | −0.0873 | 0.0591 | 0.1353 | 0.049* | |
H21B | 0.0382 | 0.0323 | 0.1496 | 0.049* | |
H21C | −0.0256 | 0.0829 | 0.0500 | 0.049* | |
C22 | 0.0605 (4) | 0.1903 (3) | 0.1808 (3) | 0.0203 (8) | |
C23 | 0.1848 (3) | 0.2323 (3) | 0.1958 (3) | 0.0203 (8) | |
C24 | 0.2557 (3) | 0.3292 (3) | 0.2559 (3) | 0.0200 (8) | |
C25 | 0.3877 (4) | 0.3725 (3) | 0.2671 (3) | 0.0271 (9) | |
H25A | 0.3926 | 0.4073 | 0.2068 | 0.041* | |
H25B | 0.4254 | 0.3147 | 0.2723 | 0.041* | |
H25C | 0.4308 | 0.4236 | 0.3297 | 0.041* | |
C26 | 0.2444 (4) | 0.1708 (3) | 0.1471 (3) | 0.0216 (8) | |
C27 | 0.3045 (4) | 0.1011 (3) | 0.1989 (3) | 0.0274 (9) | |
H27 | 0.3039 | 0.0876 | 0.2656 | 0.033* | |
C28 | 0.3647 (4) | 0.0517 (3) | 0.1535 (3) | 0.0282 (9) | |
H28 | 0.4062 | 0.0051 | 0.1907 | 0.034* | |
C29 | 0.3046 (4) | 0.1279 (3) | 0.0069 (3) | 0.0236 (8) | |
H29 | 0.3021 | 0.1359 | −0.0616 | 0.028* | |
C30 | 0.2425 (4) | 0.1812 (3) | 0.0473 (3) | 0.0254 (9) | |
H30 | 0.1987 | 0.2247 | 0.0070 | 0.031* | |
O7 | 0.5547 (3) | 0.9488 (3) | 0.3692 (2) | 0.0441 (8) | |
H7D | 0.5713 | 0.8912 | 0.3786 | 0.066* | |
H7E | 0.5921 | 0.9728 | 0.3299 | 0.066* | |
O8 | 0.3377 (4) | 0.9766 (3) | 0.4157 (3) | 0.0560 (10) | |
H8D | 0.3583 | 0.9891 | 0.4837 | 0.084* | |
H8E | 0.3892 | 0.9665 | 0.3877 | 0.084* | |
O9 | 0.0765 (6) | 0.9115 (5) | 0.3225 (5) | 0.133 (3) | |
H9D | 0.1535 | 0.9307 | 0.3500 | 0.199* | |
H9E | 0.0234 | 0.9379 | 0.3297 | 0.199* | |
C31 | 0.7300 (6) | 0.7744 (6) | 0.4712 (5) | 0.076 (2) | |
H31A | 0.7890 | 0.8078 | 0.4397 | 0.114* | |
H31B | 0.7406 | 0.7055 | 0.4887 | 0.114* | |
H31C | 0.7433 | 0.8193 | 0.5340 | 0.114* | |
O10 | 0.6090 (3) | 0.7609 (3) | 0.3999 (2) | 0.0360 (7) | |
H10D | 0.5633 | 0.7402 | 0.4321 | 0.054* | |
O11 | −0.0971 (6) | 0.9975 (5) | 0.3463 (5) | 0.1045 (18) | |
H11D | −0.1606 | 1.0082 | 0.3052 | 0.157* | |
C32 | −0.0730 (7) | 1.0923 (6) | 0.4115 (6) | 0.086 (2) | |
H32A | −0.0059 | 1.0955 | 0.4763 | 0.130* | |
H32B | −0.1462 | 1.0932 | 0.4262 | 0.130* | |
H32C | −0.0502 | 1.1532 | 0.3767 | 0.130* | |
O12 | −0.1019 (6) | 0.7605 (5) | 0.1721 (5) | 0.117 (2)* | |
H12D | −0.0541 | 0.8153 | 0.2124 | 0.175* | |
C33 | −0.1876 (9) | 0.6941 (8) | 0.2100 (8) | 0.122 (3)* | |
H33A | −0.1542 | 0.6385 | 0.2425 | 0.183* | |
H33B | −0.2644 | 0.6622 | 0.1524 | 0.183* | |
H33C | −0.2028 | 0.7364 | 0.2609 | 0.183* | |
Atomic displacement parameters (Å2) top | U11 | U22 | U33 | U12 | U13 | U23 |
Cd1 | 0.0179 (2) | 0.01283 (18) | 0.0212 (2) | 0.00305 (14) | 0.01184 (16) | 0.00333 (14) |
Fe1 | 0.0181 (3) | 0.0154 (3) | 0.0187 (3) | 0.0032 (2) | 0.0118 (2) | 0.0032 (2) |
Cl1 | 0.0265 (5) | 0.0221 (5) | 0.0213 (4) | 0.0026 (4) | 0.0087 (4) | 0.0027 (4) |
O1 | 0.0227 (14) | 0.0230 (13) | 0.0205 (13) | 0.0058 (11) | 0.0144 (11) | 0.0052 (10) |
O2 | 0.0194 (13) | 0.0215 (13) | 0.0208 (13) | 0.0044 (11) | 0.0124 (11) | 0.0038 (10) |
O3 | 0.0181 (13) | 0.0167 (12) | 0.0184 (13) | 0.0002 (10) | 0.0095 (11) | 0.0020 (10) |
O4 | 0.0286 (15) | 0.0190 (13) | 0.0198 (13) | 0.0051 (11) | 0.0154 (12) | 0.0041 (10) |
O5 | 0.0206 (14) | 0.0175 (12) | 0.0261 (14) | 0.0033 (10) | 0.0144 (11) | 0.0031 (10) |
O6 | 0.0189 (13) | 0.0201 (13) | 0.0214 (13) | 0.0033 (10) | 0.0090 (11) | −0.0011 (10) |
N1 | 0.0235 (18) | 0.040 (2) | 0.0255 (18) | 0.0026 (16) | 0.0135 (15) | 0.0028 (15) |
N2 | 0.0193 (16) | 0.0148 (15) | 0.0233 (16) | 0.0000 (12) | 0.0116 (13) | 0.0027 (12) |
N3 | 0.0221 (17) | 0.0185 (15) | 0.0248 (16) | 0.0071 (13) | 0.0132 (14) | 0.0041 (13) |
C1 | 0.023 (2) | 0.047 (3) | 0.025 (2) | 0.0101 (19) | 0.0139 (18) | 0.0042 (18) |
C2 | 0.022 (2) | 0.0189 (18) | 0.0249 (19) | 0.0039 (15) | 0.0145 (16) | 0.0030 (15) |
C3 | 0.0194 (19) | 0.0171 (17) | 0.0206 (18) | 0.0019 (14) | 0.0111 (15) | 0.0008 (14) |
C4 | 0.024 (2) | 0.0151 (17) | 0.0201 (18) | 0.0016 (14) | 0.0141 (16) | 0.0005 (14) |
C5 | 0.025 (2) | 0.034 (2) | 0.0206 (19) | 0.0084 (17) | 0.0135 (17) | 0.0041 (16) |
C6 | 0.0174 (19) | 0.0259 (19) | 0.0189 (18) | 0.0022 (15) | 0.0086 (15) | 0.0000 (15) |
C7 | 0.029 (2) | 0.026 (2) | 0.025 (2) | 0.0000 (17) | 0.0166 (18) | 0.0000 (16) |
C8 | 0.025 (2) | 0.034 (2) | 0.029 (2) | −0.0024 (18) | 0.0131 (18) | 0.0006 (18) |
C9 | 0.024 (2) | 0.038 (2) | 0.023 (2) | 0.0050 (18) | 0.0131 (17) | −0.0036 (17) |
C10 | 0.020 (2) | 0.026 (2) | 0.027 (2) | −0.0006 (16) | 0.0124 (17) | −0.0023 (16) |
C11 | 0.024 (2) | 0.0192 (18) | 0.0222 (19) | 0.0047 (15) | 0.0131 (16) | 0.0037 (15) |
C12 | 0.0150 (17) | 0.0165 (17) | 0.0194 (18) | 0.0032 (14) | 0.0093 (14) | 0.0070 (14) |
C13 | 0.0211 (19) | 0.0169 (17) | 0.0188 (18) | 0.0009 (15) | 0.0096 (15) | 0.0046 (14) |
C14 | 0.0206 (19) | 0.0145 (17) | 0.0227 (19) | −0.0004 (14) | 0.0088 (16) | 0.0018 (14) |
C15 | 0.050 (3) | 0.019 (2) | 0.028 (2) | −0.0012 (19) | 0.021 (2) | −0.0009 (16) |
C16 | 0.024 (2) | 0.0159 (17) | 0.0179 (18) | −0.0003 (15) | 0.0126 (16) | 0.0003 (14) |
C17 | 0.021 (2) | 0.0205 (18) | 0.0235 (19) | 0.0008 (15) | 0.0101 (16) | 0.0033 (15) |
C18 | 0.024 (2) | 0.0194 (18) | 0.0188 (18) | 0.0015 (15) | 0.0075 (16) | 0.0030 (14) |
C19 | 0.021 (2) | 0.0188 (18) | 0.028 (2) | 0.0038 (15) | 0.0105 (16) | 0.0058 (15) |
C20 | 0.022 (2) | 0.0219 (19) | 0.0217 (19) | 0.0049 (15) | 0.0077 (16) | 0.0070 (15) |
C21 | 0.030 (2) | 0.023 (2) | 0.046 (3) | 0.0034 (18) | 0.019 (2) | −0.0053 (18) |
C22 | 0.024 (2) | 0.0173 (18) | 0.0226 (19) | 0.0050 (15) | 0.0119 (16) | 0.0043 (14) |
C23 | 0.023 (2) | 0.0212 (18) | 0.0224 (19) | 0.0086 (15) | 0.0125 (16) | 0.0046 (15) |
C24 | 0.0197 (19) | 0.0216 (18) | 0.0203 (18) | 0.0067 (15) | 0.0084 (15) | 0.0054 (14) |
C25 | 0.021 (2) | 0.028 (2) | 0.033 (2) | 0.0065 (17) | 0.0119 (18) | 0.0035 (17) |
C26 | 0.022 (2) | 0.0198 (18) | 0.026 (2) | 0.0042 (15) | 0.0133 (16) | 0.0010 (15) |
C27 | 0.035 (2) | 0.032 (2) | 0.023 (2) | 0.0151 (18) | 0.0145 (18) | 0.0073 (16) |
C28 | 0.037 (2) | 0.033 (2) | 0.026 (2) | 0.0210 (19) | 0.0170 (19) | 0.0119 (17) |
C29 | 0.028 (2) | 0.025 (2) | 0.0217 (19) | 0.0095 (17) | 0.0125 (17) | 0.0064 (15) |
C30 | 0.033 (2) | 0.024 (2) | 0.027 (2) | 0.0132 (17) | 0.0163 (18) | 0.0078 (16) |
O7 | 0.066 (2) | 0.0371 (18) | 0.0358 (18) | 0.0145 (17) | 0.0268 (17) | 0.0089 (14) |
O8 | 0.069 (3) | 0.049 (2) | 0.045 (2) | 0.0092 (19) | 0.020 (2) | 0.0024 (17) |
O9 | 0.096 (5) | 0.122 (5) | 0.166 (6) | 0.045 (4) | 0.022 (4) | −0.038 (5) |
C31 | 0.058 (4) | 0.106 (6) | 0.079 (5) | 0.031 (4) | 0.036 (4) | 0.027 (4) |
O10 | 0.0265 (16) | 0.0488 (19) | 0.0375 (17) | 0.0063 (14) | 0.0196 (14) | 0.0172 (15) |
O11 | 0.108 (5) | 0.107 (4) | 0.108 (4) | 0.052 (4) | 0.034 (4) | 0.020 (4) |
C32 | 0.082 (5) | 0.064 (4) | 0.098 (6) | 0.019 (4) | 0.017 (4) | −0.018 (4) |
Geometric parameters (Å, º) top
Cd1—N2i | 2.361 (3) | C15—H15A | 0.9800 |
Cd1—N2 | 2.361 (3) | C15—H15B | 0.9800 |
Cd1—N3ii | 2.363 (3) | C15—H15C | 0.9800 |
Cd1—N3iii | 2.363 (3) | C16—C17 | 1.387 (5) |
Cd1—Cl1i | 2.6351 (9) | C16—C20 | 1.393 (5) |
Cd1—Cl1 | 2.6351 (9) | C17—C18 | 1.390 (5) |
Fe1—O2 | 1.971 (2) | C17—H17 | 0.9500 |
Fe1—O1 | 1.979 (3) | C18—H18 | 0.9500 |
Fe1—O4 | 1.986 (3) | C19—C20 | 1.386 (5) |
Fe1—O6 | 1.989 (3) | C19—H19 | 0.9500 |
Fe1—O5 | 1.999 (3) | C20—H20 | 0.9500 |
Fe1—O3 | 2.001 (2) | C21—C22 | 1.505 (5) |
O1—C2 | 1.274 (4) | C21—H21A | 0.9800 |
O2—C4 | 1.284 (4) | C21—H21B | 0.9800 |
O3—C12 | 1.281 (4) | C21—H21C | 0.9800 |
O4—C14 | 1.278 (4) | C22—C23 | 1.406 (5) |
O5—C22 | 1.279 (4) | C23—C24 | 1.402 (5) |
O6—C24 | 1.277 (4) | C23—C26 | 1.495 (5) |
N1—C9 | 1.334 (5) | C24—C25 | 1.508 (5) |
N1—C8 | 1.334 (5) | C25—H25A | 0.9800 |
N2—C18 | 1.336 (5) | C25—H25B | 0.9800 |
N2—C19 | 1.336 (5) | C25—H25C | 0.9800 |
N3—C29 | 1.327 (5) | C26—C30 | 1.389 (5) |
N3—C28 | 1.340 (5) | C26—C27 | 1.391 (6) |
N3—Cd1iv | 2.363 (3) | C27—C28 | 1.373 (6) |
C1—C2 | 1.503 (6) | C27—H27 | 0.9500 |
C1—H1A | 0.9800 | C28—H28 | 0.9500 |
C1—H1B | 0.9800 | C29—C30 | 1.382 (5) |
C1—H1C | 0.9800 | C29—H29 | 0.9500 |
C2—C3 | 1.404 (5) | C30—H30 | 0.9500 |
C3—C4 | 1.408 (5) | O7—H7D | 0.8400 |
C3—C6 | 1.500 (5) | O7—H7E | 0.8418 |
C4—C5 | 1.501 (5) | O8—H8D | 0.8880 |
C5—H5A | 0.9800 | O8—H8E | 0.8730 |
C5—H5B | 0.9800 | O9—H9D | 0.8455 |
C5—H5C | 0.9800 | O9—H9E | 0.8380 |
C6—C7 | 1.388 (5) | C31—O10 | 1.429 (7) |
C6—C10 | 1.393 (5) | C31—H31A | 0.9800 |
C7—C8 | 1.387 (6) | C31—H31B | 0.9800 |
C7—H7 | 0.9500 | C31—H31C | 0.9800 |
C8—H8 | 0.9500 | O10—H10D | 0.8242 |
C9—C10 | 1.380 (5) | O11—C32 | 1.428 (8) |
C9—H9 | 0.9500 | O11—H11D | 0.8400 |
C10—H10 | 0.9500 | C32—H32A | 0.9800 |
C11—C12 | 1.496 (5) | C32—H32B | 0.9800 |
C11—H11A | 0.9800 | C32—H32C | 0.9800 |
C11—H11B | 0.9800 | O12—C33 | 1.435 (10) |
C11—H11C | 0.9800 | O12—H12D | 0.8458 |
C12—C13 | 1.409 (5) | C33—H33A | 0.9800 |
C13—C14 | 1.410 (5) | C33—H33B | 0.9800 |
C13—C16 | 1.492 (5) | C33—H33C | 0.9800 |
C14—C15 | 1.497 (5) | | |
| | | |
N2i—Cd1—N2 | 180.0 | C12—C13—C14 | 122.1 (3) |
N2i—Cd1—N3ii | 85.20 (10) | C12—C13—C16 | 119.2 (3) |
N2—Cd1—N3ii | 94.80 (10) | C14—C13—C16 | 118.3 (3) |
N2i—Cd1—N3iii | 94.80 (10) | O4—C14—C13 | 124.1 (3) |
N2—Cd1—N3iii | 85.20 (10) | O4—C14—C15 | 115.9 (3) |
N3ii—Cd1—N3iii | 180.0 | C13—C14—C15 | 120.0 (3) |
N2i—Cd1—Cl1i | 87.95 (8) | C14—C15—H15A | 109.5 |
N2—Cd1—Cl1i | 92.05 (8) | C14—C15—H15B | 109.5 |
N3ii—Cd1—Cl1i | 89.60 (8) | H15A—C15—H15B | 109.5 |
N3iii—Cd1—Cl1i | 90.40 (8) | C14—C15—H15C | 109.5 |
N2i—Cd1—Cl1 | 92.05 (8) | H15A—C15—H15C | 109.5 |
N2—Cd1—Cl1 | 87.95 (8) | H15B—C15—H15C | 109.5 |
N3ii—Cd1—Cl1 | 90.40 (8) | C17—C16—C20 | 117.2 (3) |
N3iii—Cd1—Cl1 | 89.60 (8) | C17—C16—C13 | 120.5 (3) |
Cl1i—Cd1—Cl1 | 180.0 | C20—C16—C13 | 122.2 (3) |
O2—Fe1—O1 | 86.53 (10) | C16—C17—C18 | 119.6 (4) |
O2—Fe1—O4 | 92.33 (10) | C16—C17—H17 | 120.2 |
O1—Fe1—O4 | 94.13 (11) | C18—C17—H17 | 120.2 |
O2—Fe1—O6 | 90.75 (11) | N2—C18—C17 | 123.1 (4) |
O1—Fe1—O6 | 173.81 (10) | N2—C18—H18 | 118.4 |
O4—Fe1—O6 | 91.54 (11) | C17—C18—H18 | 118.4 |
O2—Fe1—O5 | 95.20 (10) | N2—C19—C20 | 123.5 (4) |
O1—Fe1—O5 | 88.89 (11) | N2—C19—H19 | 118.3 |
O4—Fe1—O5 | 172.05 (10) | C20—C19—H19 | 118.3 |
O6—Fe1—O5 | 85.82 (10) | C19—C20—C16 | 119.3 (3) |
O2—Fe1—O3 | 177.07 (10) | C19—C20—H20 | 120.3 |
O1—Fe1—O3 | 94.87 (10) | C16—C20—H20 | 120.3 |
O4—Fe1—O3 | 85.01 (10) | C22—C21—H21A | 109.5 |
O6—Fe1—O3 | 88.11 (10) | C22—C21—H21B | 109.5 |
O5—Fe1—O3 | 87.41 (10) | H21A—C21—H21B | 109.5 |
C2—O1—Fe1 | 131.1 (2) | C22—C21—H21C | 109.5 |
C4—O2—Fe1 | 130.8 (2) | H21A—C21—H21C | 109.5 |
C12—O3—Fe1 | 127.5 (2) | H21B—C21—H21C | 109.5 |
C14—O4—Fe1 | 129.2 (2) | O5—C22—C23 | 123.7 (3) |
C22—O5—Fe1 | 126.2 (2) | O5—C22—C21 | 115.3 (3) |
C24—O6—Fe1 | 123.4 (2) | C23—C22—C21 | 120.9 (3) |
C9—N1—C8 | 116.9 (3) | C24—C23—C22 | 122.5 (3) |
C18—N2—C19 | 117.2 (3) | C24—C23—C26 | 118.5 (3) |
C18—N2—Cd1 | 115.7 (2) | C22—C23—C26 | 119.0 (3) |
C19—N2—Cd1 | 125.6 (2) | O6—C24—C23 | 124.8 (3) |
C29—N3—C28 | 117.5 (3) | O6—C24—C25 | 114.7 (3) |
C29—N3—Cd1iv | 122.3 (2) | C23—C24—C25 | 120.5 (3) |
C28—N3—Cd1iv | 119.9 (3) | C24—C25—H25A | 109.5 |
C2—C1—H1A | 109.5 | C24—C25—H25B | 109.5 |
C2—C1—H1B | 109.5 | H25A—C25—H25B | 109.5 |
H1A—C1—H1B | 109.5 | C24—C25—H25C | 109.5 |
C2—C1—H1C | 109.5 | H25A—C25—H25C | 109.5 |
H1A—C1—H1C | 109.5 | H25B—C25—H25C | 109.5 |
H1B—C1—H1C | 109.5 | C30—C26—C27 | 116.7 (4) |
O1—C2—C3 | 124.3 (4) | C30—C26—C23 | 121.2 (3) |
O1—C2—C1 | 115.3 (3) | C27—C26—C23 | 122.1 (3) |
C3—C2—C1 | 120.4 (3) | C28—C27—C26 | 120.0 (4) |
C2—C3—C4 | 122.4 (3) | C28—C27—H27 | 120.0 |
C2—C3—C6 | 119.3 (3) | C26—C27—H27 | 120.0 |
C4—C3—C6 | 118.3 (3) | N3—C28—C27 | 122.9 (4) |
O2—C4—C3 | 124.1 (3) | N3—C28—H28 | 118.5 |
O2—C4—C5 | 115.0 (3) | C27—C28—H28 | 118.5 |
C3—C4—C5 | 120.8 (3) | N3—C29—C30 | 123.1 (4) |
C4—C5—H5A | 109.5 | N3—C29—H29 | 118.4 |
C4—C5—H5B | 109.5 | C30—C29—H29 | 118.4 |
H5A—C5—H5B | 109.5 | C29—C30—C26 | 119.6 (4) |
C4—C5—H5C | 109.5 | C29—C30—H30 | 120.2 |
H5A—C5—H5C | 109.5 | C26—C30—H30 | 120.2 |
H5B—C5—H5C | 109.5 | H7D—O7—H7E | 102.0 |
C7—C6—C10 | 116.8 (3) | H8D—O8—H8E | 121.9 |
C7—C6—C3 | 122.0 (3) | H9D—O9—H9E | 131.6 |
C10—C6—C3 | 121.2 (3) | O10—C31—H31A | 109.5 |
C8—C7—C6 | 119.3 (4) | O10—C31—H31B | 109.5 |
C8—C7—H7 | 120.4 | H31A—C31—H31B | 109.5 |
C6—C7—H7 | 120.4 | O10—C31—H31C | 109.5 |
N1—C8—C7 | 123.8 (4) | H31A—C31—H31C | 109.5 |
N1—C8—H8 | 118.1 | H31B—C31—H31C | 109.5 |
C7—C8—H8 | 118.1 | C31—O10—H10D | 106.0 |
N1—C9—C10 | 123.2 (4) | C32—O11—H11D | 90.8 |
N1—C9—H9 | 118.4 | O11—C32—H32A | 109.5 |
C10—C9—H9 | 118.4 | O11—C32—H32B | 109.5 |
C9—C10—C6 | 120.1 (4) | H32A—C32—H32B | 109.5 |
C9—C10—H10 | 120.0 | O11—C32—H32C | 109.5 |
C6—C10—H10 | 120.0 | H32A—C32—H32C | 109.5 |
C12—C11—H11A | 109.5 | H32B—C32—H32C | 109.5 |
C12—C11—H11B | 109.5 | C33—O12—H12D | 115.7 |
H11A—C11—H11B | 109.5 | O12—C33—H33A | 109.5 |
C12—C11—H11C | 109.5 | O12—C33—H33B | 109.5 |
H11A—C11—H11C | 109.5 | H33A—C33—H33B | 109.5 |
H11B—C11—H11C | 109.5 | O12—C33—H33C | 109.5 |
O3—C12—C13 | 123.6 (3) | H33A—C33—H33C | 109.5 |
O3—C12—C11 | 115.5 (3) | H33B—C33—H33C | 109.5 |
C13—C12—C11 | 120.9 (3) | | |
| | | |
Fe1—O1—C2—C3 | 6.1 (5) | C12—C13—C16—C20 | −107.6 (4) |
Fe1—O1—C2—C1 | −173.3 (3) | C14—C13—C16—C20 | 79.2 (5) |
O1—C2—C3—C4 | −1.4 (6) | C20—C16—C17—C18 | 0.2 (5) |
C1—C2—C3—C4 | 177.9 (4) | C13—C16—C17—C18 | 178.1 (3) |
O1—C2—C3—C6 | 179.1 (3) | C19—N2—C18—C17 | 2.4 (5) |
C1—C2—C3—C6 | −1.6 (5) | Cd1—N2—C18—C17 | −164.3 (3) |
Fe1—O2—C4—C3 | −7.9 (5) | C16—C17—C18—N2 | −2.1 (6) |
Fe1—O2—C4—C5 | 171.6 (2) | C18—N2—C19—C20 | −0.9 (6) |
C2—C3—C4—O2 | 2.4 (6) | Cd1—N2—C19—C20 | 164.3 (3) |
C6—C3—C4—O2 | −178.1 (3) | N2—C19—C20—C16 | −0.9 (6) |
C2—C3—C4—C5 | −177.1 (3) | C17—C16—C20—C19 | 1.2 (5) |
C6—C3—C4—C5 | 2.4 (5) | C13—C16—C20—C19 | −176.7 (3) |
C2—C3—C6—C7 | 77.8 (5) | Fe1—O5—C22—C23 | 16.6 (5) |
C4—C3—C6—C7 | −101.7 (4) | Fe1—O5—C22—C21 | −161.9 (3) |
C2—C3—C6—C10 | −103.7 (4) | O5—C22—C23—C24 | 7.2 (6) |
C4—C3—C6—C10 | 76.8 (5) | C21—C22—C23—C24 | −174.4 (4) |
C10—C6—C7—C8 | 0.0 (6) | O5—C22—C23—C26 | −173.7 (3) |
C3—C6—C7—C8 | 178.6 (4) | C21—C22—C23—C26 | 4.8 (6) |
C9—N1—C8—C7 | −0.4 (6) | Fe1—O6—C24—C23 | −30.7 (5) |
C6—C7—C8—N1 | 0.2 (7) | Fe1—O6—C24—C25 | 148.1 (3) |
C8—N1—C9—C10 | 0.5 (6) | C22—C23—C24—O6 | 0.6 (6) |
N1—C9—C10—C6 | −0.3 (7) | C26—C23—C24—O6 | −178.6 (3) |
C7—C6—C10—C9 | 0.1 (6) | C22—C23—C24—C25 | −178.2 (4) |
C3—C6—C10—C9 | −178.5 (4) | C26—C23—C24—C25 | 2.6 (5) |
Fe1—O3—C12—C13 | −24.3 (5) | C24—C23—C26—C30 | −93.1 (5) |
Fe1—O3—C12—C11 | 155.5 (2) | C22—C23—C26—C30 | 87.7 (5) |
O3—C12—C13—C14 | −1.8 (6) | C24—C23—C26—C27 | 86.7 (5) |
C11—C12—C13—C14 | 178.4 (4) | C22—C23—C26—C27 | −92.5 (5) |
O3—C12—C13—C16 | −174.8 (3) | C30—C26—C27—C28 | 4.1 (6) |
C11—C12—C13—C16 | 5.4 (5) | C23—C26—C27—C28 | −175.7 (4) |
Fe1—O4—C14—C13 | 11.4 (6) | C29—N3—C28—C27 | −2.9 (6) |
Fe1—O4—C14—C15 | −170.8 (3) | Cd1iv—N3—C28—C27 | 169.9 (3) |
C12—C13—C14—O4 | 8.7 (6) | C26—C27—C28—N3 | −0.9 (7) |
C16—C13—C14—O4 | −178.3 (4) | C28—N3—C29—C30 | 3.5 (6) |
C12—C13—C14—C15 | −169.1 (4) | Cd1iv—N3—C29—C30 | −169.2 (3) |
C16—C13—C14—C15 | 4.0 (6) | N3—C29—C30—C26 | −0.2 (6) |
C12—C13—C16—C17 | 74.5 (5) | C27—C26—C30—C29 | −3.6 (6) |
C14—C13—C16—C17 | −98.7 (4) | C23—C26—C30—C29 | 176.2 (4) |
Symmetry codes: (i) −x+1, −y+2, −z; (ii) −x+1, −y+1, −z; (iii) x, y+1, z; (iv) x, y−1, z. |
Crystal data top
C60H60Br2CdFe2N6O12·0.24(C2H8O2)·4.75(CH4O)·6(H2O) | Z = 1 |
Mr = 1716.66 | F(000) = 882.1 |
Triclinic, P1 | Dx = 1.385 Mg m−3 |
a = 12.2603 (15) Å | Mo Kα radiation, λ = 0.71073 Å |
b = 13.3560 (16) Å | Cell parameters from 4766 reflections |
c = 13.9326 (16) Å | θ = 2.3–24.8° |
α = 92.055 (2)° | µ = 1.64 mm−1 |
β = 109.196 (2)° | T = 100 K |
γ = 105.345 (2)° | Plate, red |
V = 2058.8 (4) Å3 | 0.36 × 0.10 × 0.03 mm |
Data collection top
CCD area detector diffractometer | 6555 reflections with I > 2σ(I) |
Radiation source: Incoatec microsource | Rint = 0.052 |
ω scans | θmax = 26.5°, θmin = 2.1° |
Absorption correction: multi-scan SADABS | h = −15→15 |
Tmin = 0.595, Tmax = 0.745 | k = −16→16 |
24811 measured reflections | l = −17→17 |
8482 independent reflections | |
Refinement top
Refinement on F2 | Primary atom site location: heavy-atom method |
Least-squares matrix: full | Hydrogen site location: mixed |
R[F2 > 2σ(F2)] = 0.054 | H-atom parameters constrained |
wR(F2) = 0.157 | w = 1/[σ2(Fo2) + (0.0753P)2 + 3.957P]
where P = (Fo2 + 2Fc2)/3 |
S = 1.05 | (Δ/σ)max = 0.001 |
8482 reflections | Δρmax = 1.30 e Å−3 |
441 parameters | Δρmin = −1.05 e Å−3 |
2 restraints | |
Crystal data top
C60H60Br2CdFe2N6O12·0.24(C2H8O2)·4.75(CH4O)·6(H2O) | γ = 105.345 (2)° |
Mr = 1716.66 | V = 2058.8 (4) Å3 |
Triclinic, P1 | Z = 1 |
a = 12.2603 (15) Å | Mo Kα radiation |
b = 13.3560 (16) Å | µ = 1.64 mm−1 |
c = 13.9326 (16) Å | T = 100 K |
α = 92.055 (2)° | 0.36 × 0.10 × 0.03 mm |
β = 109.196 (2)° | |
Data collection top
CCD area detector diffractometer | 8482 independent reflections |
Absorption correction: multi-scan SADABS | 6555 reflections with I > 2σ(I) |
Tmin = 0.595, Tmax = 0.745 | Rint = 0.052 |
24811 measured reflections | |
Refinement top
R[F2 > 2σ(F2)] = 0.054 | 2 restraints |
wR(F2) = 0.157 | H-atom parameters constrained |
S = 1.05 | Δρmax = 1.30 e Å−3 |
8482 reflections | Δρmin = −1.05 e Å−3 |
441 parameters | |
Special details top
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. |
Fractional atomic coordinates and isotropic or equivalent isotropic displacement parameters (Å2) top | x | y | z | Uiso*/Ueq | Occ. (<1) |
Cd1 | 0.5000 | 1.0000 | 0.0000 | 0.02037 (14) | |
Fe1 | 0.04644 (6) | 0.39445 (5) | 0.25163 (5) | 0.01918 (17) | |
Br1 | 0.67335 (5) | 1.03674 (4) | 0.19520 (4) | 0.02738 (15) | |
O1 | −0.1281 (3) | 0.3808 (3) | 0.2063 (2) | 0.0226 (7) | |
O2 | 0.0395 (3) | 0.3827 (3) | 0.3904 (2) | 0.0228 (7) | |
O3 | 0.0586 (3) | 0.4140 (2) | 0.1132 (2) | 0.0216 (7) | |
O4 | 0.0972 (3) | 0.5497 (2) | 0.2766 (2) | 0.0250 (7) | |
O5 | 0.0059 (3) | 0.2404 (2) | 0.2101 (3) | 0.0246 (7) | |
O6 | 0.2181 (3) | 0.3927 (2) | 0.3015 (2) | 0.0231 (7) | |
N1 | −0.4387 (4) | 0.3016 (4) | 0.5023 (3) | 0.0393 (12) | |
N2 | 0.3981 (4) | 0.8397 (3) | 0.0426 (3) | 0.0230 (9) | |
N3 | 0.3790 (4) | 0.0749 (3) | 0.0639 (3) | 0.0252 (9) | |
C1 | −0.3317 (5) | 0.3468 (5) | 0.1891 (4) | 0.0339 (12) | |
H1A | −0.3357 | 0.3732 | 0.1237 | 0.051* | |
H1B | −0.3679 | 0.3852 | 0.2251 | 0.051* | |
H1C | −0.3761 | 0.2720 | 0.1762 | 0.051* | |
C2 | −0.2028 (4) | 0.3617 (4) | 0.2537 (4) | 0.0235 (10) | |
C3 | −0.1699 (4) | 0.3542 (3) | 0.3593 (3) | 0.0214 (10) | |
C4 | −0.0503 (4) | 0.3630 (4) | 0.4215 (4) | 0.0226 (10) | |
C5 | −0.0197 (5) | 0.3472 (4) | 0.5333 (4) | 0.0309 (12) | |
H5A | 0.0672 | 0.3567 | 0.5645 | 0.046* | |
H5B | −0.0644 | 0.2761 | 0.5384 | 0.046* | |
H5C | −0.0421 | 0.3984 | 0.5693 | 0.046* | |
C6 | −0.2645 (4) | 0.3348 (4) | 0.4075 (4) | 0.0258 (11) | |
C7 | −0.3468 (5) | 0.2372 (4) | 0.3954 (4) | 0.0334 (12) | |
H7 | −0.3451 | 0.1796 | 0.3543 | 0.040* | |
C8 | −0.4317 (5) | 0.2238 (5) | 0.4435 (4) | 0.0402 (15) | |
H8 | −0.4872 | 0.1562 | 0.4342 | 0.048* | |
C9 | −0.3592 (5) | 0.3950 (5) | 0.5148 (4) | 0.0397 (14) | |
H9 | −0.3623 | 0.4508 | 0.5571 | 0.048* | |
C10 | −0.2718 (5) | 0.4152 (4) | 0.4695 (4) | 0.0330 (12) | |
H10 | −0.2173 | 0.4835 | 0.4806 | 0.040* | |
C11 | 0.1567 (5) | 0.4653 (4) | −0.0050 (4) | 0.0241 (10) | |
H11A | 0.1039 | 0.3960 | −0.0408 | 0.036* | |
H11B | 0.2413 | 0.4657 | 0.0145 | 0.036* | |
H11C | 0.1423 | 0.5184 | −0.0504 | 0.036* | |
C12 | 0.1299 (4) | 0.4893 (3) | 0.0898 (3) | 0.0190 (9) | |
C13 | 0.1834 (4) | 0.5900 (4) | 0.1477 (3) | 0.0216 (10) | |
C14 | 0.1578 (4) | 0.6155 (4) | 0.2348 (4) | 0.0246 (10) | |
C15 | 0.2015 (6) | 0.7280 (4) | 0.2848 (4) | 0.0408 (15) | |
H15A | 0.1852 | 0.7313 | 0.3490 | 0.061* | |
H15B | 0.1592 | 0.7699 | 0.2384 | 0.061* | |
H15C | 0.2886 | 0.7557 | 0.2995 | 0.061* | |
C16 | 0.2583 (4) | 0.6752 (3) | 0.1095 (3) | 0.0225 (10) | |
C17 | 0.2049 (5) | 0.7267 (4) | 0.0313 (4) | 0.0250 (10) | |
H17 | 0.1195 | 0.7069 | −0.0006 | 0.030* | |
C18 | 0.2770 (4) | 0.8075 (4) | −0.0001 (4) | 0.0248 (10) | |
H18 | 0.2390 | 0.8417 | −0.0543 | 0.030* | |
C19 | 0.4494 (5) | 0.7889 (4) | 0.1176 (4) | 0.0270 (11) | |
H19 | 0.5349 | 0.8103 | 0.1484 | 0.032* | |
C20 | 0.3834 (5) | 0.7066 (4) | 0.1526 (4) | 0.0275 (11) | |
H20 | 0.4236 | 0.6722 | 0.2055 | 0.033* | |
C21 | 0.0026 (5) | 0.0846 (4) | 0.1239 (5) | 0.0399 (14) | |
H21A | −0.0715 | 0.0577 | 0.1394 | 0.060* | |
H21B | 0.0540 | 0.0386 | 0.1455 | 0.060* | |
H21C | −0.0183 | 0.0869 | 0.0500 | 0.060* | |
C22 | 0.0696 (5) | 0.1938 (4) | 0.1809 (4) | 0.0249 (10) | |
C23 | 0.1928 (4) | 0.2383 (4) | 0.1967 (4) | 0.0249 (10) | |
C24 | 0.2608 (4) | 0.3353 (4) | 0.2569 (3) | 0.0230 (10) | |
C25 | 0.3923 (5) | 0.3802 (4) | 0.2709 (4) | 0.0336 (12) | |
H25A | 0.3996 | 0.4012 | 0.2060 | 0.050* | |
H25B | 0.4342 | 0.3271 | 0.2918 | 0.050* | |
H25C | 0.4287 | 0.4415 | 0.3239 | 0.050* | |
C26 | 0.2552 (4) | 0.1785 (4) | 0.1502 (4) | 0.0246 (10) | |
C27 | 0.3129 (5) | 0.1106 (5) | 0.2015 (4) | 0.0358 (13) | |
H27 | 0.3108 | 0.0974 | 0.2676 | 0.043* | |
C28 | 0.3745 (5) | 0.0611 (5) | 0.1565 (4) | 0.0362 (13) | |
H28 | 0.4150 | 0.0154 | 0.1939 | 0.043* | |
C29 | 0.3162 (6) | 0.1363 (4) | 0.0121 (4) | 0.0378 (14) | |
H29 | 0.3133 | 0.1436 | −0.0562 | 0.045* | |
C30 | 0.2559 (6) | 0.1892 (5) | 0.0522 (4) | 0.0412 (15) | |
H30 | 0.2146 | 0.2332 | 0.0127 | 0.049* | |
O7 | 0.5522 (5) | 0.9407 (4) | 0.3744 (4) | 0.0661 (15) | |
H7D | 0.5688 | 0.8831 | 0.3838 | 0.099* | |
H7E | 0.5896 | 0.9647 | 0.3350 | 0.099* | |
O8 | 0.3369 (5) | 0.9792 (4) | 0.4121 (4) | 0.0744 (16) | |
H8D | 0.3575 | 0.9917 | 0.4800 | 0.112* | |
H8E | 0.3884 | 0.9691 | 0.3841 | 0.112* | |
O9 | 0.0948 (12) | 0.9314 (10) | 0.3331 (10) | 0.207 (5)* | |
H9D | 0.1718 | 0.9505 | 0.3607 | 0.310* | |
H9E | 0.0417 | 0.9577 | 0.3403 | 0.310* | |
C31 | 0.7117 (13) | 0.7387 (11) | 0.4633 (11) | 0.145 (5)* | |
H31A | 0.7742 | 0.7715 | 0.4353 | 0.218* | |
H31B | 0.7096 | 0.6654 | 0.4693 | 0.218* | |
H31C | 0.7302 | 0.7762 | 0.5311 | 0.218* | |
O10 | 0.5971 (4) | 0.7432 (4) | 0.3964 (4) | 0.0539 (12)* | |
H10D | 0.5513 | 0.7225 | 0.4286 | 0.081* | |
O11 | −0.071 (2) | 1.0021 (19) | 0.3528 (19) | 0.136 (10)* | 0.374 (14) |
H11D | −0.1349 | 1.0129 | 0.3117 | 0.204* | 0.374 (14) |
C32 | −0.041 (2) | 1.0978 (19) | 0.4101 (19) | 0.077 (7)* | 0.374 (14) |
H32A | −0.0790 | 1.0905 | 0.4620 | 0.116* | 0.374 (14) |
H32B | −0.0681 | 1.1478 | 0.3652 | 0.116* | 0.374 (14) |
H32C | 0.0473 | 1.1235 | 0.4440 | 0.116* | 0.374 (14) |
O12 | −0.0824 (10) | 0.7742 (9) | 0.1722 (9) | 0.168 (4)* | |
H12D | −0.0345 | 0.8290 | 0.2125 | 0.253* | |
C33 | −0.1788 (15) | 0.7116 (14) | 0.2044 (14) | 0.202 (8)* | |
H33A | −0.1624 | 0.6461 | 0.2247 | 0.304* | |
H33B | −0.2563 | 0.6957 | 0.1476 | 0.304* | |
H33C | −0.1824 | 0.7521 | 0.2628 | 0.304* | |
C34 | 0.502 (3) | 0.491 (2) | −0.021 (2) | 0.051 (8)* | 0.240 (11) |
H34A | 0.5609 | 0.5496 | 0.0298 | 0.076* | 0.240 (11) |
H34B | 0.4526 | 0.5185 | −0.0786 | 0.076* | 0.240 (11) |
H34C | 0.5449 | 0.4500 | −0.0465 | 0.076* | 0.240 (11) |
O13 | 0.428 (3) | 0.428 (3) | 0.023 (3) | 0.140 (15)* | 0.240 (11) |
H13D | 0.4678 | 0.4164 | 0.0817 | 0.168* | 0.240 (11) |
Atomic displacement parameters (Å2) top | U11 | U22 | U33 | U12 | U13 | U23 |
Cd1 | 0.0238 (3) | 0.0150 (2) | 0.0258 (3) | 0.00228 (18) | 0.0163 (2) | −0.00085 (18) |
Fe1 | 0.0224 (3) | 0.0185 (3) | 0.0188 (3) | 0.0028 (3) | 0.0128 (3) | −0.0008 (2) |
Br1 | 0.0300 (3) | 0.0234 (3) | 0.0248 (3) | 0.0009 (2) | 0.0106 (2) | −0.00190 (19) |
O1 | 0.0259 (17) | 0.0261 (17) | 0.0202 (16) | 0.0075 (14) | 0.0139 (14) | 0.0032 (13) |
O2 | 0.0218 (17) | 0.0261 (17) | 0.0229 (17) | 0.0034 (14) | 0.0140 (14) | −0.0006 (13) |
O3 | 0.0231 (17) | 0.0189 (16) | 0.0201 (16) | 0.0000 (13) | 0.0097 (14) | −0.0038 (13) |
O4 | 0.0362 (19) | 0.0187 (16) | 0.0243 (17) | 0.0023 (14) | 0.0210 (15) | −0.0011 (13) |
O5 | 0.0282 (18) | 0.0202 (16) | 0.0297 (18) | 0.0041 (14) | 0.0185 (15) | 0.0004 (14) |
O6 | 0.0255 (17) | 0.0230 (17) | 0.0199 (16) | 0.0046 (14) | 0.0096 (14) | −0.0052 (13) |
N1 | 0.026 (2) | 0.057 (3) | 0.029 (2) | −0.003 (2) | 0.017 (2) | −0.012 (2) |
N2 | 0.024 (2) | 0.019 (2) | 0.024 (2) | −0.0002 (16) | 0.0116 (17) | −0.0027 (16) |
N3 | 0.028 (2) | 0.026 (2) | 0.027 (2) | 0.0107 (18) | 0.0161 (18) | 0.0014 (17) |
C1 | 0.023 (3) | 0.051 (3) | 0.027 (3) | 0.010 (2) | 0.011 (2) | 0.000 (2) |
C2 | 0.026 (2) | 0.018 (2) | 0.028 (3) | 0.0036 (19) | 0.014 (2) | −0.0029 (19) |
C3 | 0.026 (2) | 0.018 (2) | 0.021 (2) | 0.0015 (19) | 0.013 (2) | −0.0040 (18) |
C4 | 0.030 (3) | 0.018 (2) | 0.022 (2) | 0.0014 (19) | 0.017 (2) | −0.0022 (18) |
C5 | 0.033 (3) | 0.042 (3) | 0.022 (2) | 0.009 (2) | 0.016 (2) | 0.002 (2) |
C6 | 0.022 (2) | 0.030 (3) | 0.023 (2) | 0.000 (2) | 0.011 (2) | −0.004 (2) |
C7 | 0.035 (3) | 0.033 (3) | 0.031 (3) | −0.002 (2) | 0.020 (2) | −0.009 (2) |
C8 | 0.031 (3) | 0.046 (3) | 0.031 (3) | −0.013 (3) | 0.014 (2) | −0.006 (2) |
C9 | 0.030 (3) | 0.055 (4) | 0.031 (3) | 0.001 (3) | 0.017 (2) | −0.015 (3) |
C10 | 0.027 (3) | 0.039 (3) | 0.029 (3) | −0.001 (2) | 0.015 (2) | −0.012 (2) |
C11 | 0.031 (3) | 0.020 (2) | 0.021 (2) | 0.003 (2) | 0.014 (2) | −0.0019 (18) |
C12 | 0.020 (2) | 0.019 (2) | 0.019 (2) | 0.0033 (18) | 0.0103 (19) | 0.0018 (17) |
C13 | 0.022 (2) | 0.022 (2) | 0.019 (2) | −0.0018 (19) | 0.0112 (19) | 0.0015 (18) |
C14 | 0.030 (3) | 0.019 (2) | 0.024 (2) | 0.000 (2) | 0.014 (2) | −0.0031 (19) |
C15 | 0.066 (4) | 0.023 (3) | 0.031 (3) | −0.004 (3) | 0.028 (3) | −0.007 (2) |
C16 | 0.026 (3) | 0.017 (2) | 0.022 (2) | −0.0015 (19) | 0.012 (2) | −0.0043 (18) |
C17 | 0.025 (2) | 0.022 (2) | 0.025 (2) | 0.000 (2) | 0.011 (2) | −0.0027 (19) |
C18 | 0.028 (3) | 0.024 (2) | 0.021 (2) | 0.002 (2) | 0.011 (2) | 0.0015 (19) |
C19 | 0.026 (3) | 0.023 (2) | 0.030 (3) | −0.001 (2) | 0.013 (2) | 0.003 (2) |
C20 | 0.026 (3) | 0.027 (3) | 0.024 (3) | 0.002 (2) | 0.007 (2) | 0.004 (2) |
C21 | 0.039 (3) | 0.026 (3) | 0.053 (4) | 0.005 (2) | 0.018 (3) | −0.011 (3) |
C22 | 0.031 (3) | 0.022 (2) | 0.025 (2) | 0.008 (2) | 0.015 (2) | −0.0010 (19) |
C23 | 0.030 (3) | 0.028 (3) | 0.025 (2) | 0.011 (2) | 0.018 (2) | 0.004 (2) |
C24 | 0.027 (3) | 0.027 (2) | 0.018 (2) | 0.008 (2) | 0.012 (2) | 0.0037 (19) |
C25 | 0.023 (3) | 0.038 (3) | 0.039 (3) | 0.007 (2) | 0.013 (2) | −0.002 (2) |
C26 | 0.028 (3) | 0.024 (2) | 0.027 (2) | 0.009 (2) | 0.016 (2) | −0.0008 (19) |
C27 | 0.045 (3) | 0.053 (4) | 0.030 (3) | 0.032 (3) | 0.025 (3) | 0.014 (3) |
C28 | 0.046 (3) | 0.048 (3) | 0.034 (3) | 0.030 (3) | 0.024 (3) | 0.015 (3) |
C29 | 0.063 (4) | 0.043 (3) | 0.028 (3) | 0.030 (3) | 0.030 (3) | 0.012 (2) |
C30 | 0.073 (4) | 0.040 (3) | 0.037 (3) | 0.039 (3) | 0.035 (3) | 0.017 (3) |
O7 | 0.113 (4) | 0.040 (3) | 0.054 (3) | 0.009 (3) | 0.052 (3) | 0.006 (2) |
O8 | 0.102 (4) | 0.065 (3) | 0.043 (3) | 0.003 (3) | 0.026 (3) | 0.002 (2) |
Geometric parameters (Å, º) top
Cd1—N3i | 2.363 (4) | C15—H15C | 0.9800 |
Cd1—N3ii | 2.363 (4) | C16—C17 | 1.382 (7) |
Cd1—N2 | 2.379 (4) | C16—C20 | 1.388 (7) |
Cd1—N2iii | 2.379 (4) | C17—C18 | 1.386 (6) |
Cd1—Br1 | 2.7759 (6) | C17—H17 | 0.9500 |
Cd1—Br1iii | 2.7759 (6) | C18—H18 | 0.9500 |
Fe1—O2 | 1.973 (3) | C19—C20 | 1.388 (6) |
Fe1—O1 | 1.977 (3) | C19—H19 | 0.9500 |
Fe1—O4 | 1.982 (3) | C20—H20 | 0.9500 |
Fe1—O6 | 1.994 (3) | C21—C22 | 1.512 (7) |
Fe1—O5 | 2.000 (3) | C21—H21A | 0.9800 |
Fe1—O3 | 2.005 (3) | C21—H21B | 0.9800 |
O1—C2 | 1.275 (5) | C21—H21C | 0.9800 |
O2—C4 | 1.280 (5) | C22—C23 | 1.407 (7) |
O3—C12 | 1.275 (5) | C23—C24 | 1.402 (7) |
O4—C14 | 1.281 (5) | C23—C26 | 1.503 (6) |
O5—C22 | 1.269 (6) | C24—C25 | 1.507 (7) |
O6—C24 | 1.280 (6) | C25—H25A | 0.9800 |
N1—C9 | 1.329 (7) | C25—H25B | 0.9800 |
N1—C8 | 1.338 (7) | C25—H25C | 0.9800 |
N2—C19 | 1.339 (6) | C26—C27 | 1.374 (7) |
N2—C18 | 1.344 (6) | C26—C30 | 1.379 (7) |
N3—C28 | 1.328 (6) | C27—C28 | 1.395 (7) |
N3—C29 | 1.341 (7) | C27—H27 | 0.9500 |
N3—Cd1iv | 2.363 (4) | C28—H28 | 0.9500 |
C1—C2 | 1.494 (7) | C29—C30 | 1.371 (7) |
C1—H1A | 0.9800 | C29—H29 | 0.9500 |
C1—H1B | 0.9800 | C30—H30 | 0.9500 |
C1—H1C | 0.9800 | O7—H7D | 0.8501 |
C2—C3 | 1.407 (7) | O7—H7E | 0.8447 |
C3—C4 | 1.407 (7) | O8—H8D | 0.8926 |
C3—C6 | 1.493 (6) | O8—H8E | 0.8787 |
C4—C5 | 1.514 (6) | O9—H9D | 0.8545 |
C5—H5A | 0.9800 | O9—H9E | 0.8478 |
C5—H5B | 0.9800 | C31—O10 | 1.426 (14) |
C5—H5C | 0.9800 | C31—H31A | 0.9800 |
C6—C7 | 1.386 (7) | C31—H31B | 0.9800 |
C6—C10 | 1.393 (7) | C31—H31C | 0.9800 |
C7—C8 | 1.391 (7) | O10—H10D | 0.8272 |
C7—H7 | 0.9500 | O11—C32 | 1.37 (3) |
C8—H8 | 0.9500 | O11—H11D | 0.8530 |
C9—C10 | 1.387 (7) | C32—H32A | 0.9800 |
C9—H9 | 0.9500 | C32—H32B | 0.9800 |
C10—H10 | 0.9500 | C32—H32C | 0.9800 |
C11—C12 | 1.506 (6) | O12—C33 | 1.467 (9) |
C11—H11A | 0.9800 | O12—H12D | 0.8492 |
C11—H11B | 0.9800 | C33—H33A | 0.9800 |
C11—H11C | 0.9800 | C33—H33B | 0.9800 |
C12—C13 | 1.413 (6) | C33—H33C | 0.9800 |
C13—C14 | 1.402 (6) | C34—O13 | 1.387 (19) |
C13—C16 | 1.494 (6) | C34—H34A | 0.9800 |
C14—C15 | 1.511 (7) | C34—H34B | 0.9800 |
C15—H15A | 0.9800 | C34—H34C | 0.9800 |
C15—H15B | 0.9800 | O13—H13D | 0.8400 |
| | | |
N3i—Cd1—N3ii | 180.00 (17) | O4—C14—C13 | 124.7 (4) |
N3i—Cd1—N2 | 94.41 (14) | O4—C14—C15 | 115.6 (4) |
N3ii—Cd1—N2 | 85.59 (14) | C13—C14—C15 | 119.7 (4) |
N3i—Cd1—N2iii | 85.59 (14) | C14—C15—H15A | 109.5 |
N3ii—Cd1—N2iii | 94.41 (14) | C14—C15—H15B | 109.5 |
N2—Cd1—N2iii | 180.0 | H15A—C15—H15B | 109.5 |
N3i—Cd1—Br1 | 89.82 (10) | C14—C15—H15C | 109.5 |
N3ii—Cd1—Br1 | 90.18 (10) | H15A—C15—H15C | 109.5 |
N2—Cd1—Br1 | 88.49 (10) | H15B—C15—H15C | 109.5 |
N2iii—Cd1—Br1 | 91.51 (10) | C17—C16—C20 | 117.8 (4) |
N3i—Cd1—Br1iii | 90.18 (10) | C17—C16—C13 | 121.0 (4) |
N3ii—Cd1—Br1iii | 89.82 (10) | C20—C16—C13 | 121.2 (4) |
N2—Cd1—Br1iii | 91.51 (10) | C16—C17—C18 | 119.4 (5) |
N2iii—Cd1—Br1iii | 88.49 (10) | C16—C17—H17 | 120.3 |
Br1—Cd1—Br1iii | 180.0 | C18—C17—H17 | 120.3 |
O2—Fe1—O1 | 86.34 (13) | N2—C18—C17 | 123.1 (5) |
O2—Fe1—O4 | 92.35 (13) | N2—C18—H18 | 118.5 |
O1—Fe1—O4 | 94.42 (14) | C17—C18—H18 | 118.5 |
O2—Fe1—O6 | 90.85 (13) | N2—C19—C20 | 123.1 (5) |
O1—Fe1—O6 | 173.82 (14) | N2—C19—H19 | 118.4 |
O4—Fe1—O6 | 91.20 (14) | C20—C19—H19 | 118.4 |
O2—Fe1—O5 | 95.54 (13) | C19—C20—C16 | 119.3 (5) |
O1—Fe1—O5 | 89.22 (14) | C19—C20—H20 | 120.4 |
O4—Fe1—O5 | 171.51 (13) | C16—C20—H20 | 120.4 |
O6—Fe1—O5 | 85.56 (13) | C22—C21—H21A | 109.5 |
O2—Fe1—O3 | 177.07 (13) | C22—C21—H21B | 109.5 |
O1—Fe1—O3 | 94.74 (13) | H21A—C21—H21B | 109.5 |
O4—Fe1—O3 | 84.86 (13) | C22—C21—H21C | 109.5 |
O6—Fe1—O3 | 88.33 (13) | H21A—C21—H21C | 109.5 |
O5—Fe1—O3 | 87.20 (13) | H21B—C21—H21C | 109.5 |
C2—O1—Fe1 | 131.6 (3) | O5—C22—C23 | 124.2 (4) |
C4—O2—Fe1 | 130.9 (3) | O5—C22—C21 | 115.0 (4) |
C12—O3—Fe1 | 127.7 (3) | C23—C22—C21 | 120.8 (4) |
C14—O4—Fe1 | 129.0 (3) | C24—C23—C22 | 122.6 (4) |
C22—O5—Fe1 | 126.5 (3) | C24—C23—C26 | 118.5 (4) |
C24—O6—Fe1 | 124.6 (3) | C22—C23—C26 | 119.0 (4) |
C9—N1—C8 | 117.2 (4) | O6—C24—C23 | 124.2 (4) |
C19—N2—C18 | 117.2 (4) | O6—C24—C25 | 115.2 (4) |
C19—N2—Cd1 | 124.8 (3) | C23—C24—C25 | 120.6 (4) |
C18—N2—Cd1 | 116.9 (3) | C24—C25—H25A | 109.5 |
C28—N3—C29 | 116.5 (4) | C24—C25—H25B | 109.5 |
C28—N3—Cd1iv | 120.5 (3) | H25A—C25—H25B | 109.5 |
C29—N3—Cd1iv | 122.9 (3) | C24—C25—H25C | 109.5 |
C2—C1—H1A | 109.5 | H25A—C25—H25C | 109.5 |
C2—C1—H1B | 109.5 | H25B—C25—H25C | 109.5 |
H1A—C1—H1B | 109.5 | C27—C26—C30 | 116.9 (5) |
C2—C1—H1C | 109.5 | C27—C26—C23 | 122.3 (4) |
H1A—C1—H1C | 109.5 | C30—C26—C23 | 120.7 (5) |
H1B—C1—H1C | 109.5 | C26—C27—C28 | 119.9 (5) |
O1—C2—C3 | 123.9 (4) | C26—C27—H27 | 120.1 |
O1—C2—C1 | 115.4 (4) | C28—C27—H27 | 120.1 |
C3—C2—C1 | 120.6 (4) | N3—C28—C27 | 122.9 (5) |
C2—C3—C4 | 122.2 (4) | N3—C28—H28 | 118.5 |
C2—C3—C6 | 119.4 (4) | C27—C28—H28 | 118.5 |
C4—C3—C6 | 118.4 (4) | N3—C29—C30 | 123.6 (5) |
O2—C4—C3 | 124.6 (4) | N3—C29—H29 | 118.2 |
O2—C4—C5 | 114.7 (4) | C30—C29—H29 | 118.2 |
C3—C4—C5 | 120.7 (4) | C29—C30—C26 | 119.9 (5) |
C4—C5—H5A | 109.5 | C29—C30—H30 | 120.0 |
C4—C5—H5B | 109.5 | C26—C30—H30 | 120.0 |
H5A—C5—H5B | 109.5 | H7D—O7—H7E | 101.9 |
C4—C5—H5C | 109.5 | H8D—O8—H8E | 121.4 |
H5A—C5—H5C | 109.5 | H9D—O9—H9E | 132.0 |
H5B—C5—H5C | 109.5 | O10—C31—H31A | 109.5 |
C7—C6—C10 | 116.8 (4) | O10—C31—H31B | 109.5 |
C7—C6—C3 | 122.5 (4) | H31A—C31—H31B | 109.5 |
C10—C6—C3 | 120.7 (4) | O10—C31—H31C | 109.5 |
C6—C7—C8 | 119.8 (5) | H31A—C31—H31C | 109.5 |
C6—C7—H7 | 120.1 | H31B—C31—H31C | 109.5 |
C8—C7—H7 | 120.1 | C31—O10—H10D | 104.0 |
N1—C8—C7 | 123.0 (5) | C32—O11—H11D | 91.0 |
N1—C8—H8 | 118.5 | O11—C32—H32A | 109.5 |
C7—C8—H8 | 118.5 | O11—C32—H32B | 109.5 |
N1—C9—C10 | 123.4 (5) | H32A—C32—H32B | 109.5 |
N1—C9—H9 | 118.3 | O11—C32—H32C | 109.5 |
C10—C9—H9 | 118.3 | H32A—C32—H32C | 109.5 |
C9—C10—C6 | 119.6 (5) | H32B—C32—H32C | 109.5 |
C9—C10—H10 | 120.2 | C33—O12—H12D | 116.6 |
C6—C10—H10 | 120.2 | O12—C33—H33A | 110.1 |
C12—C11—H11A | 109.5 | O12—C33—H33B | 109.5 |
C12—C11—H11B | 109.5 | H33A—C33—H33B | 109.5 |
H11A—C11—H11B | 109.5 | O12—C33—H33C | 108.8 |
C12—C11—H11C | 109.5 | H33A—C33—H33C | 109.5 |
H11A—C11—H11C | 109.5 | H33B—C33—H33C | 109.5 |
H11B—C11—H11C | 109.5 | O13—C34—H34A | 109.5 |
O3—C12—C13 | 123.8 (4) | O13—C34—H34B | 109.5 |
O3—C12—C11 | 115.9 (4) | H34A—C34—H34B | 109.5 |
C13—C12—C11 | 120.2 (4) | O13—C34—H34C | 109.5 |
C14—C13—C12 | 121.5 (4) | H34A—C34—H34C | 109.5 |
C14—C13—C16 | 118.5 (4) | H34B—C34—H34C | 109.5 |
C12—C13—C16 | 119.6 (4) | C34—O13—H13D | 112.1 |
Symmetry codes: (i) −x+1, −y+1, −z; (ii) x, y+1, z; (iii) −x+1, −y+2, −z; (iv) x, y−1, z. |
Crystal data top
C64.09H68.18Cd3Cl8.18Fe2I6N6O12 | F(000) = 4975 |
Mr = 2614.57 | Dx = 1.726 Mg m−3 |
Monoclinic, C2/c | Mo Kα radiation, λ = 0.71073 Å |
a = 32.186 (3) Å | Cell parameters from 3756 reflections |
b = 13.7863 (15) Å | θ = 2.4–19.7° |
c = 27.721 (2) Å | µ = 3.01 mm−1 |
β = 125.118 (8)° | T = 100 K |
V = 10061.4 (18) Å3 | Block, red |
Z = 4 | 0.15 × 0.08 × 0.07 mm |
Data collection top
CCD area detector diffractometer | 3817 reflections with I > 2σ(I) |
Radiation source: Incoatec microsource | Rint = 0.085 |
ω scans | θmax = 22.0°, θmin = 1.8° |
Absorption correction: multi-scan SADABS | h = −33→33 |
Tmin = 0.587, Tmax = 0.745 | k = −14→14 |
41442 measured reflections | l = −29→29 |
6166 independent reflections | |
Refinement top
Refinement on F2 | Primary atom site location: heavy-atom method |
Least-squares matrix: full | Hydrogen site location: inferred from neighbouring sites |
R[F2 > 2σ(F2)] = 0.066 | H-atom parameters constrained |
wR(F2) = 0.163 | w = 1/[σ2(Fo2) + (0.0555P)2]
where P = (Fo2 + 2Fc2)/3 |
S = 0.95 | (Δ/σ)max = 0.001 |
6166 reflections | Δρmax = 2.31 e Å−3 |
259 parameters | Δρmin = −1.52 e Å−3 |
2 restraints | |
Crystal data top
C64.09H68.18Cd3Cl8.18Fe2I6N6O12 | V = 10061.4 (18) Å3 |
Mr = 2614.57 | Z = 4 |
Monoclinic, C2/c | Mo Kα radiation |
a = 32.186 (3) Å | µ = 3.01 mm−1 |
b = 13.7863 (15) Å | T = 100 K |
c = 27.721 (2) Å | 0.15 × 0.08 × 0.07 mm |
β = 125.118 (8)° | |
Data collection top
CCD area detector diffractometer | 6166 independent reflections |
Absorption correction: multi-scan SADABS | 3817 reflections with I > 2σ(I) |
Tmin = 0.587, Tmax = 0.745 | Rint = 0.085 |
41442 measured reflections | θmax = 22.0° |
Refinement top
R[F2 > 2σ(F2)] = 0.066 | 2 restraints |
wR(F2) = 0.163 | H-atom parameters constrained |
S = 0.95 | Δρmax = 2.31 e Å−3 |
6166 reflections | Δρmin = −1.52 e Å−3 |
259 parameters | |
Special details top
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. |
Fractional atomic coordinates and isotropic or equivalent isotropic displacement parameters (Å2) top | x | y | z | Uiso*/Ueq | Occ. (<1) |
I1 | 0.81336 (5) | 0.16305 (8) | 0.18575 (6) | 0.0648 (4) | |
I2 | 0.89618 (5) | 0.36766 (9) | 0.11898 (5) | 0.0548 (4) | |
I3 | 0.41195 (4) | 0.19416 (8) | 0.16986 (5) | 0.0445 (3) | |
Cd1 | 0.85709 (4) | 0.32463 (8) | 0.18033 (5) | 0.0348 (3) | |
Cd2 | 0.5000 | 0.28300 (11) | 0.2500 | 0.0322 (5) | |
Fe1 | 0.56602 (8) | 0.74825 (14) | 0.02682 (9) | 0.0270 (6) | |
O1 | 0.6075 (3) | 0.7195 (7) | −0.0035 (4) | 0.031 (3)* | |
O2 | 0.6323 (4) | 0.7596 (7) | 0.1046 (4) | 0.038 (3)* | |
O3 | 0.5634 (3) | 0.6034 (6) | 0.0322 (4) | 0.026 (2)* | |
O4 | 0.5302 (3) | 0.7505 (7) | 0.0658 (4) | 0.033 (3)* | |
O5 | 0.5019 (3) | 0.7476 (7) | −0.0543 (4) | 0.029 (3)* | |
O6 | 0.5645 (3) | 0.8919 (6) | 0.0185 (4) | 0.023 (2)* | |
N1 | 0.7969 (4) | 0.4404 (9) | 0.1542 (5) | 0.032 (3)* | |
N2 | 0.5136 (4) | 0.3896 (8) | 0.1977 (5) | 0.026 (3)* | |
N3 | 0.4110 (4) | 1.1032 (8) | −0.2309 (5) | 0.025 (3)* | |
C1 | 0.6574 (6) | 0.6183 (11) | −0.0164 (7) | 0.046 (5)* | |
H1A | 0.6417 | 0.5540 | −0.0265 | 0.069* | |
H1B | 0.6942 | 0.6115 | 0.0040 | 0.069* | |
H1C | 0.6434 | 0.6563 | −0.0525 | 0.069* | |
C2 | 0.6468 (5) | 0.6686 (10) | 0.0226 (6) | 0.029 (4)* | |
C3 | 0.6779 (5) | 0.6536 (10) | 0.0825 (6) | 0.032 (4)* | |
C4 | 0.6705 (6) | 0.7022 (12) | 0.1205 (7) | 0.047 (5)* | |
C5 | 0.7092 (7) | 0.7025 (15) | 0.1872 (9) | 0.092 (7)* | |
H5A | 0.7173 | 0.7696 | 0.2014 | 0.138* | |
H5B | 0.7402 | 0.6695 | 0.1974 | 0.138* | |
H5C | 0.6950 | 0.6688 | 0.2058 | 0.138* | |
C6 | 0.7216 (6) | 0.5837 (11) | 0.1097 (6) | 0.032 (4)* | |
C7 | 0.7649 (6) | 0.5994 (13) | 0.1169 (7) | 0.048 (5)* | |
H7 | 0.7706 | 0.6615 | 0.1068 | 0.057* | |
C8 | 0.8029 (6) | 0.5309 (12) | 0.1383 (7) | 0.052 (5)* | |
H8 | 0.8334 | 0.5465 | 0.1421 | 0.062* | |
C9 | 0.7541 (6) | 0.4264 (12) | 0.1487 (6) | 0.040 (4)* | |
H9 | 0.7494 | 0.3657 | 0.1612 | 0.048* | |
C10 | 0.7163 (6) | 0.4918 (11) | 0.1266 (6) | 0.041 (4)* | |
H10 | 0.6857 | 0.4753 | 0.1225 | 0.049* | |
C11 | 0.5706 (5) | 0.4464 (9) | 0.0694 (6) | 0.030 (4)* | |
H11A | 0.5414 | 0.4051 | 0.0578 | 0.045* | |
H11B | 0.5987 | 0.4316 | 0.1102 | 0.045* | |
H11C | 0.5812 | 0.4341 | 0.0432 | 0.045* | |
C12 | 0.5558 (5) | 0.5515 (10) | 0.0650 (6) | 0.021 (3)* | |
C13 | 0.5381 (5) | 0.5882 (10) | 0.0968 (6) | 0.023 (4)* | |
C14 | 0.5234 (5) | 0.6850 (11) | 0.0944 (6) | 0.030 (4)* | |
C15 | 0.5009 (5) | 0.7201 (11) | 0.1239 (7) | 0.041 (4)* | |
H15A | 0.4898 | 0.7874 | 0.1122 | 0.061* | |
H15B | 0.5261 | 0.7171 | 0.1667 | 0.061* | |
H15C | 0.4716 | 0.6796 | 0.1127 | 0.061* | |
C16 | 0.5300 (5) | 0.5187 (10) | 0.1320 (6) | 0.024 (4)* | |
C17 | 0.4871 (5) | 0.4617 (10) | 0.1059 (6) | 0.026 (4)* | |
H17 | 0.4615 | 0.4665 | 0.0648 | 0.032* | |
C18 | 0.4814 (6) | 0.3969 (11) | 0.1405 (7) | 0.038 (4)* | |
H18 | 0.4525 | 0.3556 | 0.1213 | 0.046* | |
C19 | 0.5536 (6) | 0.4429 (11) | 0.2214 (7) | 0.037 (4)* | |
H19 | 0.5782 | 0.4357 | 0.2626 | 0.045* | |
C20 | 0.5642 (6) | 0.5101 (11) | 0.1924 (7) | 0.039 (4)* | |
H20 | 0.5940 | 0.5489 | 0.2136 | 0.046* | |
C21 | 0.4340 (5) | 0.7873 (11) | −0.1507 (6) | 0.037 (4)* | |
H21A | 0.4290 | 0.7171 | −0.1509 | 0.056* | |
H21B | 0.4385 | 0.8039 | −0.1818 | 0.056* | |
H21C | 0.4043 | 0.8214 | −0.1577 | 0.056* | |
C22 | 0.4796 (5) | 0.8164 (11) | −0.0929 (6) | 0.030 (4)* | |
C23 | 0.4961 (5) | 0.9139 (10) | −0.0820 (6) | 0.021 (4)* | |
C24 | 0.5364 (5) | 0.9470 (10) | −0.0274 (6) | 0.022 (4)* | |
C25 | 0.5533 (5) | 1.0513 (10) | −0.0162 (6) | 0.033 (4)* | |
H25A | 0.5770 | 1.0622 | 0.0264 | 0.050* | |
H25B | 0.5237 | 1.0937 | −0.0321 | 0.050* | |
H25C | 0.5703 | 1.0659 | −0.0355 | 0.050* | |
C26 | 0.4676 (5) | 0.9843 (10) | −0.1325 (6) | 0.026 (4)* | |
C27 | 0.4303 (5) | 1.0422 (10) | −0.1394 (6) | 0.034 (4)* | |
H27 | 0.4226 | 1.0411 | −0.1110 | 0.041* | |
C28 | 0.4035 (6) | 1.1029 (11) | −0.1881 (6) | 0.035 (4)* | |
H28 | 0.3789 | 1.1458 | −0.1912 | 0.042* | |
C29 | 0.4488 (5) | 1.0488 (10) | −0.2232 (6) | 0.032 (4)* | |
H29 | 0.4562 | 1.0515 | −0.2518 | 0.039* | |
C30 | 0.4777 (5) | 0.9886 (11) | −0.1746 (6) | 0.033 (4)* | |
H30 | 0.5043 | 0.9506 | −0.1703 | 0.040* | |
Cl1 | 0.6931 (3) | 0.0075 (7) | 0.0560 (4) | 0.121 (3) | 0.7735 |
Cl2 | 0.7184 (3) | −0.1501 (5) | 0.0114 (3) | 0.082 (2) | 0.7735 |
C31 | 0.6737 (8) | −0.0766 (15) | 0.0090 (9) | 0.053 (7)* | 0.7735 |
H31A | 0.6527 | −0.0469 | −0.0307 | 0.063* | 0.7735 |
H31B | 0.6510 | −0.1188 | 0.0131 | 0.063* | 0.7735 |
Cl3 | 0.7165 (3) | 0.3660 (6) | 0.0005 (3) | 0.097 (3)* | 0.7703 |
Cl4 | 0.6454 (3) | 0.2964 (6) | 0.0262 (4) | 0.110 (3)* | 0.7703 |
C32 | 0.6954 (9) | 0.2687 (19) | 0.0213 (12) | 0.083 (9)* | 0.7703 |
H32A | 0.6847 | 0.2156 | −0.0076 | 0.100* | 0.7703 |
H32B | 0.7242 | 0.2445 | 0.0601 | 0.100* | 0.7703 |
Cl5 | 0.6784 (7) | 0.3269 (15) | 0.3041 (9) | 0.196 (8)* | 0.5 |
Cl6 | 0.7041 (6) | 0.4057 (13) | 0.2401 (8) | 0.166 (7)* | 0.5 |
C33 | 0.7268 (12) | 0.403 (3) | 0.3133 (11) | 0.079 (13)* | 0.5 |
H33A | 0.7269 | 0.4682 | 0.3287 | 0.095* | 0.5 |
H33B | 0.7610 | 0.3736 | 0.3384 | 0.095* | 0.5 |
Atomic displacement parameters (Å2) top | U11 | U22 | U33 | U12 | U13 | U23 |
I1 | 0.0710 (10) | 0.0301 (7) | 0.0745 (10) | −0.0025 (7) | 0.0310 (8) | 0.0104 (7) |
I2 | 0.0718 (9) | 0.0591 (9) | 0.0536 (8) | −0.0092 (7) | 0.0476 (8) | −0.0165 (7) |
I3 | 0.0653 (8) | 0.0276 (7) | 0.0477 (8) | −0.0121 (6) | 0.0365 (7) | −0.0022 (5) |
Cd1 | 0.0420 (8) | 0.0295 (7) | 0.0310 (7) | 0.0009 (6) | 0.0199 (7) | −0.0040 (6) |
Cd2 | 0.0611 (12) | 0.0170 (9) | 0.0348 (10) | 0.000 | 0.0369 (10) | 0.000 |
Fe1 | 0.0444 (15) | 0.0116 (12) | 0.0329 (14) | 0.0042 (11) | 0.0268 (12) | 0.0053 (10) |
Cl1 | 0.102 (7) | 0.118 (8) | 0.111 (7) | 0.011 (6) | 0.042 (6) | −0.035 (6) |
Cl2 | 0.090 (5) | 0.078 (5) | 0.109 (6) | −0.001 (4) | 0.076 (5) | 0.012 (4) |
Geometric parameters (Å, º) top
I1—Cd1 | 2.6850 (17) | C11—H11B | 0.9800 |
I2—Cd1 | 2.6997 (16) | C11—H11C | 0.9800 |
I3—Cd2 | 2.6876 (13) | C12—C13 | 1.392 (17) |
Cd1—N3i | 2.268 (11) | C13—C14 | 1.404 (18) |
Cd1—N1 | 2.282 (12) | C13—C16 | 1.492 (18) |
Cd2—N2ii | 2.276 (11) | C14—C15 | 1.453 (18) |
Cd2—N2 | 2.276 (11) | C15—H15A | 0.9800 |
Cd2—I3ii | 2.6876 (13) | C15—H15B | 0.9800 |
Fe1—O4 | 1.982 (9) | C15—H15C | 0.9800 |
Fe1—O2 | 1.982 (10) | C16—C17 | 1.380 (17) |
Fe1—O1 | 1.984 (9) | C16—C20 | 1.383 (18) |
Fe1—O6 | 1.991 (9) | C17—C18 | 1.395 (18) |
Fe1—O5 | 1.994 (9) | C17—H17 | 0.9500 |
Fe1—O3 | 2.008 (9) | C18—H18 | 0.9500 |
O1—C2 | 1.251 (15) | C19—C20 | 1.391 (19) |
O2—C4 | 1.308 (17) | C19—H19 | 0.9500 |
O3—C12 | 1.287 (14) | C20—H20 | 0.9500 |
O4—C14 | 1.301 (16) | C21—C22 | 1.475 (18) |
O5—C22 | 1.295 (15) | C21—H21A | 0.9800 |
O6—C24 | 1.300 (14) | C21—H21B | 0.9800 |
N1—C9 | 1.311 (17) | C21—H21C | 0.9800 |
N1—C8 | 1.373 (18) | C22—C23 | 1.412 (18) |
N2—C19 | 1.286 (16) | C23—C24 | 1.386 (17) |
N2—C18 | 1.309 (17) | C23—C26 | 1.505 (18) |
N3—C29 | 1.338 (16) | C24—C25 | 1.506 (18) |
N3—C28 | 1.341 (16) | C25—H25A | 0.9800 |
N3—Cd1iii | 2.268 (11) | C25—H25B | 0.9800 |
C1—C2 | 1.480 (19) | C25—H25C | 0.9800 |
C1—H1A | 0.9800 | C26—C27 | 1.361 (18) |
C1—H1B | 0.9800 | C26—C30 | 1.383 (18) |
C1—H1C | 0.9800 | C27—C28 | 1.390 (19) |
C2—C3 | 1.373 (19) | C27—H27 | 0.9500 |
C3—C4 | 1.38 (2) | C28—H28 | 0.9500 |
C3—C6 | 1.504 (19) | C29—C30 | 1.388 (18) |
C4—C5 | 1.52 (2) | C29—H29 | 0.9500 |
C5—H5A | 0.9800 | C30—H30 | 0.9500 |
C5—H5B | 0.9800 | Cl1—C31 | 1.58 (2) |
C5—H5C | 0.9800 | Cl2—C31 | 1.73 (2) |
C6—C7 | 1.307 (19) | C31—H31A | 0.9900 |
C6—C10 | 1.396 (19) | C31—H31B | 0.9900 |
C7—C8 | 1.38 (2) | Cl3—C32 | 1.75 (2) |
C7—H7 | 0.9500 | Cl4—C32 | 1.73 (2) |
C8—H8 | 0.9500 | C32—H32A | 0.9900 |
C9—C10 | 1.347 (19) | C32—H32B | 0.9900 |
C9—H9 | 0.9500 | Cl5—C33 | 1.775 (18) |
C10—H10 | 0.9500 | Cl6—C33 | 1.717 (18) |
C11—C12 | 1.507 (17) | C33—H33A | 0.9900 |
C11—H11A | 0.9800 | C33—H33B | 0.9900 |
| | | |
N3i—Cd1—N1 | 91.0 (4) | O3—C12—C13 | 123.9 (12) |
N3i—Cd1—I1 | 113.7 (3) | O3—C12—C11 | 114.4 (12) |
N1—Cd1—I1 | 102.8 (3) | C13—C12—C11 | 121.6 (12) |
N3i—Cd1—I2 | 104.1 (3) | C12—C13—C14 | 124.5 (13) |
N1—Cd1—I2 | 105.3 (3) | C12—C13—C16 | 117.9 (12) |
I1—Cd1—I2 | 131.82 (6) | C14—C13—C16 | 117.5 (12) |
N2ii—Cd2—N2 | 99.6 (6) | O4—C14—C13 | 121.2 (13) |
N2ii—Cd2—I3 | 108.8 (3) | O4—C14—C15 | 115.2 (13) |
N2—Cd2—I3 | 105.4 (3) | C13—C14—C15 | 123.6 (14) |
N2ii—Cd2—I3ii | 105.4 (3) | C14—C15—H15A | 109.5 |
N2—Cd2—I3ii | 108.8 (3) | C14—C15—H15B | 109.5 |
I3—Cd2—I3ii | 125.78 (7) | H15A—C15—H15B | 109.5 |
O4—Fe1—O2 | 90.3 (4) | C14—C15—H15C | 109.5 |
O4—Fe1—O1 | 167.9 (4) | H15A—C15—H15C | 109.5 |
O2—Fe1—O1 | 84.9 (4) | H15B—C15—H15C | 109.5 |
O4—Fe1—O6 | 93.7 (4) | C17—C16—C20 | 116.3 (14) |
O2—Fe1—O6 | 89.2 (4) | C17—C16—C13 | 121.5 (12) |
O1—Fe1—O6 | 97.3 (4) | C20—C16—C13 | 122.1 (13) |
O4—Fe1—O5 | 93.8 (4) | C16—C17—C18 | 119.5 (14) |
O2—Fe1—O5 | 174.0 (4) | C16—C17—H17 | 120.2 |
O1—Fe1—O5 | 91.9 (4) | C18—C17—H17 | 120.2 |
O6—Fe1—O5 | 86.2 (4) | N2—C18—C17 | 123.8 (14) |
O4—Fe1—O3 | 85.0 (4) | N2—C18—H18 | 118.1 |
O2—Fe1—O3 | 93.6 (4) | C17—C18—H18 | 118.1 |
O1—Fe1—O3 | 84.3 (4) | N2—C19—C20 | 126.3 (15) |
O6—Fe1—O3 | 176.8 (4) | N2—C19—H19 | 116.9 |
O5—Fe1—O3 | 91.1 (4) | C20—C19—H19 | 116.9 |
C2—O1—Fe1 | 124.7 (9) | C16—C20—C19 | 117.9 (14) |
C4—O2—Fe1 | 122.2 (10) | C16—C20—H20 | 121.0 |
C12—O3—Fe1 | 129.7 (8) | C19—C20—H20 | 121.0 |
C14—O4—Fe1 | 132.5 (9) | C22—C21—H21A | 109.5 |
C22—O5—Fe1 | 130.6 (9) | C22—C21—H21B | 109.5 |
C24—O6—Fe1 | 130.6 (8) | H21A—C21—H21B | 109.5 |
C9—N1—C8 | 115.3 (14) | C22—C21—H21C | 109.5 |
C9—N1—Cd1 | 125.3 (11) | H21A—C21—H21C | 109.5 |
C8—N1—Cd1 | 119.2 (10) | H21B—C21—H21C | 109.5 |
C19—N2—C18 | 115.9 (14) | O5—C22—C23 | 123.9 (13) |
C19—N2—Cd2 | 123.2 (10) | O5—C22—C21 | 115.5 (13) |
C18—N2—Cd2 | 120.9 (10) | C23—C22—C21 | 120.6 (13) |
C29—N3—C28 | 117.9 (13) | C24—C23—C22 | 123.2 (13) |
C29—N3—Cd1iii | 118.5 (9) | C24—C23—C26 | 119.4 (12) |
C28—N3—Cd1iii | 123.1 (10) | C22—C23—C26 | 117.4 (12) |
C2—C1—H1A | 109.5 | O6—C24—C23 | 124.3 (12) |
C2—C1—H1B | 109.5 | O6—C24—C25 | 113.0 (12) |
H1A—C1—H1B | 109.5 | C23—C24—C25 | 122.7 (12) |
C2—C1—H1C | 109.5 | C24—C25—H25A | 109.5 |
H1A—C1—H1C | 109.5 | C24—C25—H25B | 109.5 |
H1B—C1—H1C | 109.5 | H25A—C25—H25B | 109.5 |
O1—C2—C3 | 125.1 (14) | C24—C25—H25C | 109.5 |
O1—C2—C1 | 114.9 (13) | H25A—C25—H25C | 109.5 |
C3—C2—C1 | 119.9 (14) | H25B—C25—H25C | 109.5 |
C2—C3—C4 | 121.6 (14) | C27—C26—C30 | 118.3 (14) |
C2—C3—C6 | 121.6 (13) | C27—C26—C23 | 121.7 (13) |
C4—C3—C6 | 116.8 (14) | C30—C26—C23 | 120.0 (13) |
O2—C4—C3 | 125.3 (15) | C26—C27—C28 | 119.6 (15) |
O2—C4—C5 | 111.2 (15) | C26—C27—H27 | 120.2 |
C3—C4—C5 | 123.3 (16) | C28—C27—H27 | 120.2 |
C4—C5—H5A | 109.5 | N3—C28—C27 | 122.3 (15) |
C4—C5—H5B | 109.5 | N3—C28—H28 | 118.8 |
H5A—C5—H5B | 109.5 | C27—C28—H28 | 118.8 |
C4—C5—H5C | 109.5 | N3—C29—C30 | 122.0 (14) |
H5A—C5—H5C | 109.5 | N3—C29—H29 | 119.0 |
H5B—C5—H5C | 109.5 | C30—C29—H29 | 119.0 |
C7—C6—C10 | 115.2 (15) | C26—C30—C29 | 119.6 (14) |
C7—C6—C3 | 125.4 (15) | C26—C30—H30 | 120.2 |
C10—C6—C3 | 119.3 (14) | C29—C30—H30 | 120.2 |
C6—C7—C8 | 123.7 (17) | Cl1—C31—Cl2 | 118.2 (13) |
C6—C7—H7 | 118.2 | Cl1—C31—H31A | 107.8 |
C8—C7—H7 | 118.2 | Cl2—C31—H31A | 107.8 |
N1—C8—C7 | 120.5 (16) | Cl1—C31—H31B | 107.8 |
N1—C8—H8 | 119.7 | Cl2—C31—H31B | 107.8 |
C7—C8—H8 | 119.7 | H31A—C31—H31B | 107.1 |
N1—C9—C10 | 124.7 (16) | Cl4—C32—Cl3 | 114.4 (15) |
N1—C9—H9 | 117.6 | Cl4—C32—H32A | 108.7 |
C10—C9—H9 | 117.6 | Cl3—C32—H32A | 108.7 |
C9—C10—C6 | 120.4 (15) | Cl4—C32—H32B | 108.7 |
C9—C10—H10 | 119.8 | Cl3—C32—H32B | 108.7 |
C6—C10—H10 | 119.8 | H32A—C32—H32B | 107.6 |
C12—C11—H11A | 109.5 | Cl6—C33—Cl5 | 95.7 (15) |
C12—C11—H11B | 109.5 | Cl6—C33—H33A | 112.6 |
H11A—C11—H11B | 109.5 | Cl5—C33—H33A | 112.6 |
C12—C11—H11C | 109.5 | Cl6—C33—H33B | 112.6 |
H11A—C11—H11C | 109.5 | Cl5—C33—H33B | 112.6 |
H11B—C11—H11C | 109.5 | H33A—C33—H33B | 110.1 |
Symmetry codes: (i) x+1/2, −y+3/2, z+1/2; (ii) −x+1, y, −z+1/2; (iii) x−1/2, −y+3/2, z−1/2. |
Crystal data top
C64.09H68.18Cd3Cl8.18Fe2I6N6O12 | F(000) = 4975 |
Mr = 2614.57 | Dx = 1.726 Mg m−3 |
Monoclinic, C2/c | Mo Kα radiation, λ = 0.71073 Å |
a = 32.186 (3) Å | Cell parameters from 3756 reflections |
b = 13.7863 (15) Å | θ = 2.4–19.7° |
c = 27.721 (2) Å | µ = 3.01 mm−1 |
β = 125.118 (8)° | T = 100 K |
V = 10061.4 (18) Å3 | Block, red |
Z = 4 | 0.15 × 0.08 × 0.07 mm |
Data collection top
CCD area detector diffractometer | 3835 reflections with I > 2σ(I) |
Radiation source: Incoatec microsource | Rint = 0.090 |
ω scans | θmax = 22.0°, θmin = 1.8° |
Absorption correction: multi-scan SADABS | h = −33→33 |
Tmin = 0.587, Tmax = 0.745 | k = −14→14 |
41442 measured reflections | l = −29→29 |
6166 independent reflections | |
Refinement top
Refinement on F2 | Primary atom site location: heavy-atom method |
Least-squares matrix: full | Hydrogen site location: inferred from neighbouring sites |
R[F2 > 2σ(F2)] = 0.073 | H-atom parameters constrained |
wR(F2) = 0.210 | w = 1/[σ2(Fo2) + (0.0904P)2]
where P = (Fo2 + 2Fc2)/3 |
S = 1.00 | (Δ/σ)max < 0.001 |
6166 reflections | Δρmax = 2.43 e Å−3 |
259 parameters | Δρmin = −1.56 e Å−3 |
2 restraints | |
Crystal data top
C64.09H68.18Cd3Cl8.18Fe2I6N6O12 | V = 10061.4 (18) Å3 |
Mr = 2614.57 | Z = 4 |
Monoclinic, C2/c | Mo Kα radiation |
a = 32.186 (3) Å | µ = 3.01 mm−1 |
b = 13.7863 (15) Å | T = 100 K |
c = 27.721 (2) Å | 0.15 × 0.08 × 0.07 mm |
β = 125.118 (8)° | |
Data collection top
CCD area detector diffractometer | 6166 independent reflections |
Absorption correction: multi-scan SADABS | 3835 reflections with I > 2σ(I) |
Tmin = 0.587, Tmax = 0.745 | Rint = 0.090 |
41442 measured reflections | θmax = 22.0° |
Refinement top
R[F2 > 2σ(F2)] = 0.073 | 2 restraints |
wR(F2) = 0.210 | H-atom parameters constrained |
S = 1.00 | Δρmax = 2.43 e Å−3 |
6166 reflections | Δρmin = −1.56 e Å−3 |
259 parameters | |
Special details top
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. |
Fractional atomic coordinates and isotropic or equivalent isotropic displacement parameters (Å2) top | x | y | z | Uiso*/Ueq | Occ. (<1) |
I1 | 0.81334 (6) | 0.16302 (10) | 0.18587 (7) | 0.0639 (5) | |
I2 | 0.89629 (6) | 0.36744 (11) | 0.11910 (6) | 0.0539 (5) | |
I3 | 0.41197 (5) | 0.19408 (9) | 0.16984 (6) | 0.0444 (4) | |
Cd1 | 0.85707 (5) | 0.32468 (10) | 0.18031 (6) | 0.0345 (4) | |
Cd2 | 0.5000 | 0.28294 (12) | 0.2500 | 0.0321 (5) | |
Fe1 | 0.56591 (9) | 0.74831 (16) | 0.02682 (11) | 0.0268 (6) | |
O1 | 0.6074 (4) | 0.7195 (8) | −0.0037 (5) | 0.032 (3)* | |
O2 | 0.6321 (4) | 0.7596 (8) | 0.1049 (5) | 0.036 (3)* | |
O3 | 0.5632 (4) | 0.6035 (7) | 0.0321 (4) | 0.025 (3)* | |
O4 | 0.5302 (4) | 0.7513 (8) | 0.0652 (5) | 0.033 (3)* | |
O5 | 0.5018 (4) | 0.7475 (8) | −0.0540 (5) | 0.029 (3)* | |
O6 | 0.5645 (4) | 0.8915 (7) | 0.0188 (4) | 0.023 (3)* | |
N1 | 0.7967 (5) | 0.4412 (10) | 0.1540 (6) | 0.034 (4)* | |
N2 | 0.5132 (5) | 0.3896 (9) | 0.1977 (6) | 0.026 (3)* | |
N3 | 0.4110 (5) | 1.1025 (10) | −0.2312 (6) | 0.028 (3)* | |
C1 | 0.6581 (7) | 0.6182 (14) | −0.0159 (8) | 0.049 (5)* | |
H1A | 0.6444 | 0.5521 | −0.0240 | 0.073* | |
H1B | 0.6949 | 0.6156 | 0.0039 | 0.073* | |
H1C | 0.6424 | 0.6539 | −0.0531 | 0.073* | |
C2 | 0.6468 (6) | 0.6684 (12) | 0.0228 (7) | 0.031 (4)* | |
C3 | 0.6781 (6) | 0.6529 (12) | 0.0834 (7) | 0.031 (5)* | |
C4 | 0.6700 (7) | 0.7026 (14) | 0.1208 (9) | 0.047 (5)* | |
C5 | 0.7091 (9) | 0.7046 (18) | 0.1865 (10) | 0.089 (8)* | |
H5A | 0.7145 | 0.7717 | 0.2005 | 0.134* | |
H5B | 0.7411 | 0.6777 | 0.1958 | 0.134* | |
H5C | 0.6971 | 0.6658 | 0.2058 | 0.134* | |
C6 | 0.7209 (6) | 0.5833 (12) | 0.1096 (7) | 0.031 (4)* | |
C7 | 0.7651 (7) | 0.5989 (15) | 0.1165 (8) | 0.048 (5)* | |
H7 | 0.7704 | 0.6611 | 0.1061 | 0.058* | |
C8 | 0.8036 (8) | 0.5310 (15) | 0.1376 (8) | 0.054 (6)* | |
H8 | 0.8338 | 0.5459 | 0.1407 | 0.065* | |
C9 | 0.7539 (7) | 0.4282 (14) | 0.1484 (8) | 0.043 (5)* | |
H9 | 0.7493 | 0.3673 | 0.1607 | 0.052* | |
C10 | 0.7158 (7) | 0.4925 (13) | 0.1269 (8) | 0.041 (5)* | |
H10 | 0.6856 | 0.4759 | 0.1237 | 0.050* | |
C11 | 0.5703 (6) | 0.4461 (11) | 0.0698 (7) | 0.029 (4)* | |
H11A | 0.5404 | 0.4054 | 0.0556 | 0.044* | |
H11B | 0.5965 | 0.4306 | 0.1113 | 0.044* | |
H11C | 0.5835 | 0.4336 | 0.0462 | 0.044* | |
C12 | 0.5558 (6) | 0.5513 (11) | 0.0646 (7) | 0.020 (4)* | |
C13 | 0.5379 (6) | 0.5882 (11) | 0.0963 (7) | 0.024 (4)* | |
C14 | 0.5240 (6) | 0.6845 (12) | 0.0941 (7) | 0.030 (4)* | |
C15 | 0.5007 (7) | 0.7204 (13) | 0.1244 (8) | 0.042 (5)* | |
H15A | 0.4890 | 0.7874 | 0.1122 | 0.063* | |
H15B | 0.5260 | 0.7182 | 0.1672 | 0.063* | |
H15C | 0.4717 | 0.6792 | 0.1136 | 0.063* | |
C16 | 0.5294 (6) | 0.5184 (11) | 0.1316 (7) | 0.024 (4)* | |
C17 | 0.4873 (6) | 0.4616 (11) | 0.1058 (7) | 0.028 (4)* | |
H17 | 0.4620 | 0.4657 | 0.0646 | 0.034* | |
C18 | 0.4814 (7) | 0.3961 (13) | 0.1409 (8) | 0.039 (5)* | |
H18 | 0.4526 | 0.3547 | 0.1217 | 0.047* | |
C19 | 0.5527 (7) | 0.4429 (13) | 0.2220 (8) | 0.039 (5)* | |
H19 | 0.5769 | 0.4368 | 0.2634 | 0.047* | |
C20 | 0.5631 (7) | 0.5105 (13) | 0.1919 (8) | 0.040 (5)* | |
H20 | 0.5927 | 0.5498 | 0.2129 | 0.049* | |
C21 | 0.4335 (6) | 0.7867 (13) | −0.1503 (7) | 0.037 (5)* | |
H21A | 0.4267 | 0.7177 | −0.1491 | 0.056* | |
H21B | 0.4385 | 0.7977 | −0.1814 | 0.056* | |
H21C | 0.4045 | 0.8252 | −0.1583 | 0.056* | |
C22 | 0.4795 (6) | 0.8157 (12) | −0.0930 (7) | 0.030 (4)* | |
C23 | 0.4955 (6) | 0.9135 (11) | −0.0823 (7) | 0.023 (4)* | |
C24 | 0.5368 (6) | 0.9465 (12) | −0.0265 (7) | 0.024 (4)* | |
C25 | 0.5536 (6) | 1.0512 (12) | −0.0163 (7) | 0.034 (5)* | |
H25A | 0.5794 | 1.0619 | 0.0259 | 0.051* | |
H25B | 0.5243 | 1.0934 | −0.0297 | 0.051* | |
H25C | 0.5680 | 1.0663 | −0.0383 | 0.051* | |
C26 | 0.4669 (6) | 0.9835 (12) | −0.1326 (7) | 0.028 (4)* | |
C27 | 0.4295 (6) | 1.0413 (12) | −0.1392 (7) | 0.035 (5)* | |
H27 | 0.4215 | 1.0394 | −0.1111 | 0.042* | |
C28 | 0.4032 (6) | 1.1028 (13) | −0.1875 (7) | 0.035 (5)* | |
H28 | 0.3791 | 1.1466 | −0.1903 | 0.042* | |
C29 | 0.4486 (6) | 1.0483 (12) | −0.2241 (7) | 0.033 (5)* | |
H29 | 0.4557 | 1.0509 | −0.2529 | 0.039* | |
C30 | 0.4776 (7) | 0.9877 (13) | −0.1751 (7) | 0.037 (5)* | |
H30 | 0.5043 | 0.9498 | −0.1706 | 0.044* | |
Cl1 | 0.6933 (4) | 0.0074 (8) | 0.0561 (5) | 0.121 (4) | 0.7735 |
Cl2 | 0.7182 (3) | −0.1508 (6) | 0.0107 (4) | 0.079 (3) | 0.7735 |
C31 | 0.6732 (9) | −0.0769 (18) | 0.0081 (11) | 0.052 (7)* | 0.7735 |
H31A | 0.6525 | −0.0467 | −0.0314 | 0.063* | 0.7735 |
H31B | 0.6503 | −0.1189 | 0.0119 | 0.063* | 0.7735 |
Cl3 | 0.7167 (3) | 0.3657 (7) | 0.0003 (4) | 0.095 (3)* | 0.7703 |
Cl4 | 0.6458 (4) | 0.2956 (7) | 0.0264 (5) | 0.108 (3)* | 0.7703 |
C32 | 0.6951 (11) | 0.267 (2) | 0.0186 (14) | 0.082 (10)* | 0.7703 |
H32A | 0.7239 | 0.2393 | 0.0562 | 0.098* | 0.7703 |
H32B | 0.6828 | 0.2170 | −0.0123 | 0.098* | 0.7703 |
Cl5 | 0.6784 (9) | 0.3268 (18) | 0.3045 (11) | 0.192 (10)* | 0.5 |
Cl6 | 0.7025 (8) | 0.4047 (17) | 0.2388 (9) | 0.167 (8)* | 0.5 |
C33 | 0.7266 (15) | 0.402 (3) | 0.3124 (13) | 0.093 (18)* | 0.5 |
H33A | 0.7275 | 0.4671 | 0.3282 | 0.112* | 0.5 |
H33B | 0.7607 | 0.3718 | 0.3367 | 0.112* | 0.5 |
Atomic displacement parameters (Å2) top | U11 | U22 | U33 | U12 | U13 | U23 |
I1 | 0.0698 (11) | 0.0301 (9) | 0.0734 (11) | −0.0023 (7) | 0.0305 (9) | 0.0104 (7) |
I2 | 0.0699 (10) | 0.0582 (10) | 0.0526 (9) | −0.0088 (8) | 0.0463 (9) | −0.0160 (7) |
I3 | 0.0646 (10) | 0.0281 (8) | 0.0471 (8) | −0.0122 (7) | 0.0360 (8) | −0.0024 (6) |
Cd1 | 0.0419 (9) | 0.0294 (8) | 0.0305 (8) | 0.0010 (7) | 0.0198 (7) | −0.0039 (6) |
Cd2 | 0.0606 (14) | 0.0170 (10) | 0.0349 (12) | 0.000 | 0.0368 (11) | 0.000 |
Fe1 | 0.0441 (16) | 0.0114 (13) | 0.0329 (15) | 0.0044 (12) | 0.0267 (14) | 0.0054 (11) |
Cl1 | 0.101 (8) | 0.111 (9) | 0.114 (8) | 0.010 (6) | 0.040 (7) | −0.039 (7) |
Cl2 | 0.090 (6) | 0.073 (6) | 0.108 (7) | −0.002 (5) | 0.076 (6) | 0.009 (5) |
Geometric parameters (Å, º) top
I1—Cd1 | 2.687 (2) | C11—H11B | 0.9800 |
I2—Cd1 | 2.6989 (19) | C11—H11C | 0.9800 |
I3—Cd2 | 2.6874 (15) | C12—C13 | 1.40 (2) |
Cd1—N3i | 2.267 (13) | C13—C14 | 1.39 (2) |
Cd1—N1 | 2.293 (14) | C13—C16 | 1.51 (2) |
Cd2—N2ii | 2.269 (13) | C14—C15 | 1.50 (2) |
Cd2—N2 | 2.269 (13) | C15—H15A | 0.9800 |
Cd2—I3ii | 2.6874 (15) | C15—H15B | 0.9800 |
Fe1—O4 | 1.966 (11) | C15—H15C | 0.9800 |
Fe1—O6 | 1.984 (10) | C16—C17 | 1.36 (2) |
Fe1—O2 | 1.986 (11) | C16—C20 | 1.38 (2) |
Fe1—O1 | 1.987 (11) | C17—C18 | 1.42 (2) |
Fe1—O5 | 1.989 (10) | C17—H17 | 0.9500 |
Fe1—O3 | 2.007 (10) | C18—H18 | 0.9500 |
O1—C2 | 1.255 (18) | C19—C20 | 1.41 (2) |
O2—C4 | 1.30 (2) | C19—H19 | 0.9500 |
O3—C12 | 1.277 (17) | C20—H20 | 0.9500 |
O4—C14 | 1.307 (18) | C21—C22 | 1.47 (2) |
O5—C22 | 1.295 (18) | C21—H21A | 0.9800 |
O6—C24 | 1.288 (17) | C21—H21B | 0.9800 |
N1—C9 | 1.31 (2) | C21—H21C | 0.9800 |
N1—C8 | 1.38 (2) | C22—C23 | 1.41 (2) |
N2—C19 | 1.28 (2) | C23—C24 | 1.42 (2) |
N2—C18 | 1.30 (2) | C23—C26 | 1.50 (2) |
N3—C29 | 1.336 (19) | C24—C25 | 1.51 (2) |
N3—C28 | 1.371 (19) | C25—H25A | 0.9800 |
N3—Cd1iii | 2.267 (13) | C25—H25B | 0.9800 |
C1—C2 | 1.49 (2) | C25—H25C | 0.9800 |
C1—H1A | 0.9800 | C26—C27 | 1.37 (2) |
C1—H1B | 0.9800 | C26—C30 | 1.41 (2) |
C1—H1C | 0.9800 | C27—C28 | 1.39 (2) |
C2—C3 | 1.39 (2) | C27—H27 | 0.9500 |
C3—C4 | 1.39 (2) | C28—H28 | 0.9500 |
C3—C6 | 1.48 (2) | C29—C30 | 1.40 (2) |
C4—C5 | 1.50 (3) | C29—H29 | 0.9500 |
C5—H5A | 0.9800 | C30—H30 | 0.9500 |
C5—H5B | 0.9800 | Cl1—C31 | 1.60 (2) |
C5—H5C | 0.9800 | Cl2—C31 | 1.74 (2) |
C6—C7 | 1.34 (2) | C31—H31A | 0.9900 |
C6—C10 | 1.38 (2) | C31—H31B | 0.9900 |
C7—C8 | 1.39 (2) | Cl3—C32 | 1.73 (3) |
C7—H7 | 0.9500 | Cl4—C32 | 1.76 (3) |
C8—H8 | 0.9500 | C32—H32A | 0.9900 |
C9—C10 | 1.34 (2) | C32—H32B | 0.9900 |
C9—H9 | 0.9500 | Cl5—C33 | 1.774 (19) |
C10—H10 | 0.9500 | Cl6—C33 | 1.717 (19) |
C11—C12 | 1.50 (2) | C33—H33A | 0.9900 |
C11—H11A | 0.9800 | C33—H33B | 0.9900 |
| | | |
N3i—Cd1—N1 | 90.9 (5) | O3—C12—C13 | 123.3 (14) |
N3i—Cd1—I1 | 113.9 (3) | O3—C12—C11 | 116.1 (13) |
N1—Cd1—I1 | 102.9 (4) | C13—C12—C11 | 120.5 (14) |
N3i—Cd1—I2 | 103.9 (3) | C14—C13—C12 | 124.0 (15) |
N1—Cd1—I2 | 105.3 (4) | C14—C13—C16 | 117.7 (14) |
I1—Cd1—I2 | 131.84 (7) | C12—C13—C16 | 118.2 (14) |
N2ii—Cd2—N2 | 99.3 (7) | O4—C14—C13 | 122.8 (15) |
N2ii—Cd2—I3 | 109.1 (3) | O4—C14—C15 | 114.4 (15) |
N2—Cd2—I3 | 105.2 (3) | C13—C14—C15 | 122.9 (15) |
N2ii—Cd2—I3ii | 105.2 (3) | C14—C15—H15A | 109.5 |
N2—Cd2—I3ii | 109.1 (3) | C14—C15—H15B | 109.5 |
I3—Cd2—I3ii | 125.76 (9) | H15A—C15—H15B | 109.5 |
O4—Fe1—O6 | 93.2 (4) | C14—C15—H15C | 109.5 |
O4—Fe1—O2 | 90.1 (5) | H15A—C15—H15C | 109.5 |
O6—Fe1—O2 | 89.1 (4) | H15B—C15—H15C | 109.5 |
O4—Fe1—O1 | 168.3 (5) | C17—C16—C20 | 116.3 (16) |
O6—Fe1—O1 | 97.4 (4) | C17—C16—C13 | 121.6 (14) |
O2—Fe1—O1 | 85.3 (5) | C20—C16—C13 | 122.0 (15) |
O4—Fe1—O5 | 93.3 (4) | C16—C17—C18 | 119.5 (16) |
O6—Fe1—O5 | 86.4 (4) | C16—C17—H17 | 120.3 |
O2—Fe1—O5 | 174.5 (5) | C18—C17—H17 | 120.3 |
O1—Fe1—O5 | 92.1 (4) | N2—C18—C17 | 123.7 (17) |
O4—Fe1—O3 | 85.3 (4) | N2—C18—H18 | 118.1 |
O6—Fe1—O3 | 176.8 (4) | C17—C18—H18 | 118.1 |
O2—Fe1—O3 | 93.6 (4) | N2—C19—C20 | 124.8 (18) |
O1—Fe1—O3 | 84.3 (4) | N2—C19—H19 | 117.6 |
O5—Fe1—O3 | 90.9 (4) | C20—C19—H19 | 117.6 |
C2—O1—Fe1 | 124.3 (11) | C16—C20—C19 | 118.7 (17) |
C4—O2—Fe1 | 122.1 (12) | C16—C20—H20 | 120.6 |
C12—O3—Fe1 | 130.2 (10) | C19—C20—H20 | 120.6 |
C14—O4—Fe1 | 131.2 (11) | C22—C21—H21A | 109.5 |
C22—O5—Fe1 | 130.8 (11) | C22—C21—H21B | 109.5 |
C24—O6—Fe1 | 130.8 (10) | H21A—C21—H21B | 109.5 |
C9—N1—C8 | 116.2 (16) | C22—C21—H21C | 109.5 |
C9—N1—Cd1 | 125.8 (13) | H21A—C21—H21C | 109.5 |
C8—N1—Cd1 | 117.8 (12) | H21B—C21—H21C | 109.5 |
C19—N2—C18 | 116.8 (16) | O5—C22—C23 | 124.0 (15) |
C19—N2—Cd2 | 122.1 (12) | O5—C22—C21 | 115.7 (15) |
C18—N2—Cd2 | 121.0 (12) | C23—C22—C21 | 120.3 (15) |
C29—N3—C28 | 118.7 (15) | C22—C23—C24 | 122.4 (15) |
C29—N3—Cd1iii | 118.1 (11) | C22—C23—C26 | 117.7 (14) |
C28—N3—Cd1iii | 122.7 (11) | C24—C23—C26 | 119.9 (14) |
C2—C1—H1A | 109.5 | O6—C24—C23 | 124.4 (15) |
C2—C1—H1B | 109.5 | O6—C24—C25 | 114.0 (14) |
H1A—C1—H1B | 109.5 | C23—C24—C25 | 121.5 (14) |
C2—C1—H1C | 109.5 | C24—C25—H25A | 109.5 |
H1A—C1—H1C | 109.5 | C24—C25—H25B | 109.5 |
H1B—C1—H1C | 109.5 | H25A—C25—H25B | 109.5 |
O1—C2—C3 | 125.4 (16) | C24—C25—H25C | 109.5 |
O1—C2—C1 | 115.0 (15) | H25A—C25—H25C | 109.5 |
C3—C2—C1 | 119.5 (16) | H25B—C25—H25C | 109.5 |
C4—C3—C2 | 120.7 (16) | C27—C26—C30 | 119.1 (16) |
C4—C3—C6 | 118.4 (16) | C27—C26—C23 | 121.5 (15) |
C2—C3—C6 | 120.9 (16) | C30—C26—C23 | 119.4 (15) |
O2—C4—C3 | 126.3 (18) | C26—C27—C28 | 119.1 (17) |
O2—C4—C5 | 111.5 (18) | C26—C27—H27 | 120.4 |
C3—C4—C5 | 121.9 (18) | C28—C27—H27 | 120.4 |
C4—C5—H5A | 109.5 | N3—C28—C27 | 122.1 (17) |
C4—C5—H5B | 109.5 | N3—C28—H28 | 118.9 |
H5A—C5—H5B | 109.5 | C27—C28—H28 | 118.9 |
C4—C5—H5C | 109.5 | N3—C29—C30 | 121.3 (16) |
H5A—C5—H5C | 109.5 | N3—C29—H29 | 119.3 |
H5B—C5—H5C | 109.5 | C30—C29—H29 | 119.3 |
C7—C6—C10 | 115.2 (17) | C29—C30—C26 | 119.3 (17) |
C7—C6—C3 | 125.3 (17) | C29—C30—H30 | 120.4 |
C10—C6—C3 | 119.4 (16) | C26—C30—H30 | 120.4 |
C6—C7—C8 | 125 (2) | Cl1—C31—Cl2 | 117.6 (16) |
C6—C7—H7 | 117.6 | Cl1—C31—H31A | 107.9 |
C8—C7—H7 | 117.6 | Cl2—C31—H31A | 107.9 |
N1—C8—C7 | 118.1 (19) | Cl1—C31—H31B | 107.9 |
N1—C8—H8 | 120.9 | Cl2—C31—H31B | 107.9 |
C7—C8—H8 | 120.9 | H31A—C31—H31B | 107.2 |
N1—C9—C10 | 126.4 (19) | Cl3—C32—Cl4 | 113.9 (18) |
N1—C9—H9 | 116.8 | Cl3—C32—H32A | 108.8 |
C10—C9—H9 | 116.8 | Cl4—C32—H32A | 108.8 |
C9—C10—C6 | 119.3 (18) | Cl3—C32—H32B | 108.8 |
C9—C10—H10 | 120.4 | Cl4—C32—H32B | 108.8 |
C6—C10—H10 | 120.4 | H32A—C32—H32B | 107.7 |
C12—C11—H11A | 109.5 | Cl6—C33—Cl5 | 95.8 (18) |
C12—C11—H11B | 109.5 | Cl6—C33—H33A | 112.6 |
H11A—C11—H11B | 109.5 | Cl5—C33—H33A | 112.6 |
C12—C11—H11C | 109.5 | Cl6—C33—H33B | 112.6 |
H11A—C11—H11C | 109.5 | Cl5—C33—H33B | 112.6 |
H11B—C11—H11C | 109.5 | H33A—C33—H33B | 110.1 |
Symmetry codes: (i) x+1/2, −y+3/2, z+1/2; (ii) −x+1, y, −z+1/2; (iii) x−1/2, −y+3/2, z−1/2. |
Experimental details
| (1) | (2) | (3a) | (3b) |
Crystal data |
Chemical formula | C30H33Cd2Cl4N3O6 | C30H33Br4Cd2N3O6 | C10H11CdI2NO2 | C20H22CdI2N2O4 |
Mr | 898.21 | 1076.03 | 543.41 | 720.59 |
Crystal system, space group | Triclinic, P1 | Triclinic, P1 | Orthorhombic, Pbca | Orthorhombic, Pca21 |
Temperature (K) | 100 | 100 | 100 | 100 |
a, b, c (Å) | 9.8304 (8), 13.7388 (11), 14.8816 (12) | 7.1262 (9), 15.519 (2), 16.597 (2) | 7.1002 (9), 14.3490 (18), 27.540 (4) | 13.5307 (3), 7.0913 (7), 49.110 (2) |
α, β, γ (°) | 63.4935 (11), 84.0016 (13), 81.8575 (12) | 91.247 (3), 97.889 (3), 98.609 (3) | 90, 90, 90 | 90, 90, 90 |
V (Å3) | 1778.5 (2) | 1796.0 (4) | 2805.7 (6) | 4712.1 (5) |
Z | 2 | 2 | 8 | 8 |
Radiation type | Mo Kα | Mo Kα | Mo Kα | Mo Kα |
µ (mm−1) | 1.54 | 5.68 | 5.94 | 3.57 |
Crystal size (mm) | 0.29 × 0.08 × 0.06 | 0.18 × 0.13 × 0.04 | 0.27 × 0.07 × 0.03 | 0.25 × 0.13 × 0.11 |
|
Data collection |
Diffractometer | CCD area detector diffractometer | CCD area detector diffractometer | CCD area detector diffractometer | CCD area detector diffractometer |
Absorption correction | Multi-scan SADABS | Multi-scan TWINABS | Multi-scan SADABS | Multi-scan SADABS |
Tmin, Tmax | 0.632, 0.746 | 0.522, 0.746 | 0.474, 0.746 | 0.522, 0.746 |
No. of measured, independent and observed [I > 2σ(I)] reflections | 26747, 9968, 7972 | 7336, 7336, 5914 | 39565, 4234, 3748 | 67491, 14053, 12009 |
Rint | 0.048 | 0.084 | 0.047 | 0.051 |
θmax (°) | 29.9 | 26.4 | 30.9 | 31.0 |
(sin θ/λ)max (Å−1) | 0.701 | 0.625 | 0.723 | 0.724 |
|
Refinement |
R[F2 > 2σ(F2)], wR(F2), S | 0.037, 0.079, 1.03 | 0.056, 0.103, 1.14 | 0.024, 0.051, 1.11 | 0.038, 0.076, 1.09 |
No. of reflections | 9968 | 7336 | 4234 | 14053 |
No. of parameters | 421 | 423 | 147 | 545 |
No. of restraints | 3 | 11 | 0 | 5 |
H-atom treatment | H atoms treated by a mixture of independent and constrained refinement | H atoms treated by a mixture of independent and constrained refinement | H-atom parameters constrained | H atoms treated by a mixture of independent and constrained refinement |
Δρmax, Δρmin (e Å−3) | 0.74, −0.54 | 0.99, −0.91 | 0.69, −0.59 | 1.29, −1.11 |
Absolute structure | ? | ? | ? | Refined as an inversion twin. |
Absolute structure parameter | ? | ? | ? | 0.41 (3) |
| (4) | (5) | (6_squeeze) | (6_without_squeeze) |
Crystal data |
Chemical formula | C60H60CdCl2Fe2N6O12·6(CH4O)·6(H2O) | C60H60Br2CdFe2N6O12·0.24(C2H8O2)·4.75(CH4O)·6(H2O) | C64.09H68.18Cd3Cl8.18Fe2I6N6O12 | C64.09H68.18Cd3Cl8.18Fe2I6N6O12 |
Mr | 1652.50 | 1716.66 | 2614.57 | 2614.57 |
Crystal system, space group | Triclinic, P1 | Triclinic, P1 | Monoclinic, C2/c | Monoclinic, C2/c |
Temperature (K) | 100 | 100 | 100 | 100 |
a, b, c (Å) | 12.1351 (13), 13.2343 (14), 13.8728 (15) | 12.2603 (15), 13.3560 (16), 13.9326 (16) | 32.186 (3), 13.7863 (15), 27.721 (2) | 32.186 (3), 13.7863 (15), 27.721 (2) |
α, β, γ (°) | 91.809 (2), 109.675 (2), 104.825 (2) | 92.055 (2), 109.196 (2), 105.345 (2) | 90, 125.118 (8), 90 | 90, 125.118 (8), 90 |
V (Å3) | 2011.0 (4) | 2058.8 (4) | 10061.4 (18) | 10061.4 (18) |
Z | 1 | 1 | 4 | 4 |
Radiation type | Mo Kα | Mo Kα | Mo Kα | Mo Kα |
µ (mm−1) | 0.76 | 1.64 | 3.01 | 3.01 |
Crystal size (mm) | 0.25 × 0.23 × 0.08 | 0.36 × 0.10 × 0.03 | 0.15 × 0.08 × 0.07 | 0.15 × 0.08 × 0.07 |
|
Data collection |
Diffractometer | CCD area detector diffractometer | CCD area detector diffractometer | CCD area detector diffractometer | CCD area detector diffractometer |
Absorption correction | Multi-scan SADABS | Multi-scan SADABS | Multi-scan SADABS | Multi-scan SADABS |
Tmin, Tmax | 0.640, 0.745 | 0.595, 0.745 | 0.587, 0.745 | 0.587, 0.745 |
No. of measured, independent and observed [I > 2σ(I)] reflections | 24575, 8416, 6746 | 24811, 8482, 6555 | 41442, 6166, 3817 | 41442, 6166, 3835 |
Rint | 0.050 | 0.052 | 0.085 | 0.090 |
θmax (°) | 26.6 | 26.5 | 22.0 | 22.0 |
(sin θ/λ)max (Å−1) | 0.630 | 0.627 | 0.527 | 0.527 |
|
Refinement |
R[F2 > 2σ(F2)], wR(F2), S | 0.049, 0.130, 1.04 | 0.054, 0.157, 1.05 | 0.066, 0.163, 0.95 | 0.073, 0.210, 1.00 |
No. of reflections | 8416 | 8482 | 6166 | 6166 |
No. of parameters | 456 | 441 | 259 | 259 |
No. of restraints | 0 | 2 | 2 | 2 |
H-atom treatment | H-atom parameters constrained | H-atom parameters constrained | H-atom parameters constrained | H-atom parameters constrained |
Δρmax, Δρmin (e Å−3) | 1.12, −0.92 | 1.30, −1.05 | 2.31, −1.52 | 2.43, −1.56 |
Absolute structure | ? | ? | ? | ? |
Absolute structure parameter | ? | ? | ? | ? |
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