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3-(4-Pyridyl)-acetylacetone (HacacPy) acts as a pyridine-type ligand towards CdX2 (X = Cl, Br, I). Chain polymers with six-coordinated metal cations are obtained from CdCl2 and with alternating five- and six-coordinated Cd centers from CdBr2. 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 CdI2, namely a ligand-rich molecular complex CdI2(HacacPy)2 and a ligand-deficient one-dimensional polymer [CdI2(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 FeIII, 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 CdCl2 and CdBr2, isomorphous chain polymers are obtained in which the Cd cations adopt distorted octahedral coordination and one of the peripheric pyridyl groups remains uncoordinated. With CdI2, the iron complex acts as a \mu _{{3}}-Fe(acacPy)3 bridge between tetrahedral Cd centers and gives rise to a ladder structure.

Supporting information

cif

Crystallographic Information File (CIF) https://doi.org/10.1107/S2052520614006210/bm5063sup1.cif
Contains datablocks 1, 2, 3a, 3b, 4, 5, 6_squeeze, 6_without_squeeze, global

hkl

Structure factor file (CIF format) https://doi.org/10.1107/S2052520614006210/bm50631sup2.hkl
Contains datablock 1

hkl

Structure factor file (CIF format) https://doi.org/10.1107/S2052520614006210/bm50632sup3.hkl
Contains datablock 2

hkl

Structure factor file (CIF format) https://doi.org/10.1107/S2052520614006210/bm50633asup4.hkl
Contains datablock 3a

hkl

Structure factor file (CIF format) https://doi.org/10.1107/S2052520614006210/bm50633bsup5.hkl
Contains datablock 3b

hkl

Structure factor file (CIF format) https://doi.org/10.1107/S2052520614006210/bm50634sup6.hkl
Contains datablock 4

hkl

Structure factor file (CIF format) https://doi.org/10.1107/S2052520614006210/bm50635sup7.hkl
Contains datablock 5

hkl

Structure factor file (CIF format) https://doi.org/10.1107/S2052520614006210/bm50636_squeezesup8.hkl
Contains datablock 6_squeeze

hkl

Structure factor file (CIF format) https://doi.org/10.1107/S2052520614006210/bm50636_without_squeezesup9.hkl
Contains datablock 6_without_squeeze

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Portable Document Format (PDF) file https://doi.org/10.1107/S2052520614006210/bm5063sup10.pdf
Displacement ellipsoid plots, comparison of refinement results and intensity plots

CCDC references: 992992; 992993; 992994; 992995

Experimental top

Refinement top

Crystal data, data collection and structure refinement details are summarized in Table 1.

Results and discussion top

Computing details 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).

Figures top
[Figure 1]
[Figure 2]
[Figure 3]
[Figure 4]
[Figure 5]
[Figure 6]
[Figure 7]
[Figure 8]
[Figure 9]
(1) top
Crystal data top
C30H33Cd2Cl4N3O6Z = 2
Mr = 898.21F(000) = 892
Triclinic, P1Dx = 1.677 Mg m3
a = 9.8304 (8) ÅMo Kα radiation, λ = 0.71073 Å
b = 13.7388 (11) ÅCell parameters from 3427 reflections
c = 14.8816 (12) Åθ = 2.5–28.3°
α = 63.4935 (11)°µ = 1.54 mm1
β = 84.0016 (13)°T = 100 K
γ = 81.8575 (12)°Needle, colorless
V = 1778.5 (2) Å30.29 × 0.08 × 0.06 mm
Data collection top
CCD area detector
diffractometer
7972 reflections with I > 2σ(I)
Radiation source: Incoatec microsource, multilayer opticsRint = 0.048
ω scansθmax = 29.9°, θmin = 2.1°
Absorption correction: multi-scan
SADABS
h = 1313
Tmin = 0.632, Tmax = 0.746k = 1919
26747 measured reflectionsl = 2020
9968 independent reflections
Refinement top
Refinement on F2Primary atom site location: heavy-atom method
Least-squares matrix: fullHydrogen site location: mixed
R[F2 > 2σ(F2)] = 0.037H 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 reflectionsΔρmax = 0.74 e Å3
421 parametersΔρmin = 0.54 e Å3
3 restraints
Crystal data top
C30H33Cd2Cl4N3O6γ = 81.8575 (12)°
Mr = 898.21V = 1778.5 (2) Å3
Triclinic, P1Z = 2
a = 9.8304 (8) ÅMo Kα radiation
b = 13.7388 (11) ŵ = 1.54 mm1
c = 14.8816 (12) ÅT = 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 = 0.746Rint = 0.048
26747 measured reflections
Refinement top
R[F2 > 2σ(F2)] = 0.0373 restraints
wR(F2) = 0.079H atoms treated by a mixture of independent and constrained refinement
S = 1.03Δρmax = 0.74 e Å3
9968 reflectionsΔρmin = 0.54 e Å3
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
xyzUiso*/Ueq
Cd10.50443 (2)0.05368 (2)0.35685 (2)0.01277 (5)
Cd20.15023 (2)0.07845 (2)0.49986 (2)0.01286 (5)
Cl10.35930 (7)0.08333 (5)0.51401 (5)0.01328 (13)
Cl20.30590 (7)0.20222 (5)0.35240 (5)0.01551 (14)
Cl30.28795 (7)0.08664 (6)0.63691 (5)0.01653 (14)
Cl40.01156 (7)0.05557 (5)0.36904 (5)0.01549 (14)
O10.1299 (2)0.10925 (19)0.06145 (17)0.0307 (6)
O20.0320 (3)0.1808 (2)0.08470 (18)0.0306 (6)
H2D0.009 (3)0.162 (3)0.0278 (17)0.037*
O30.8559 (3)0.5588 (2)0.18904 (19)0.0452 (7)
H3D0.868 (4)0.600 (3)0.160 (3)0.054*
O40.8571 (3)0.6459 (2)0.0755 (2)0.0465 (7)
O50.5520 (2)0.55950 (18)0.32619 (19)0.0301 (6)
H5D0.533 (4)0.601 (2)0.351 (2)0.036*
O60.4417 (2)0.66111 (17)0.39087 (18)0.0283 (5)
N10.3871 (2)0.00479 (19)0.25611 (17)0.0143 (5)
N20.6033 (3)0.19701 (19)0.21866 (18)0.0177 (5)
N30.0091 (2)0.23090 (18)0.48202 (17)0.0147 (5)
C10.0101 (4)0.1713 (3)0.2366 (3)0.0330 (8)
H1A0.09900.20100.25120.049*
H1B0.02050.10330.24410.049*
H1C0.05690.22450.28350.049*
C20.0389 (3)0.1487 (3)0.1319 (2)0.0226 (7)
C30.1587 (3)0.0961 (2)0.0873 (2)0.0185 (6)
C40.1994 (3)0.0771 (3)0.0116 (2)0.0230 (7)
C50.3214 (4)0.0197 (3)0.0668 (3)0.0337 (8)
H5A0.31860.00060.13840.050*
H5B0.40570.06780.04000.050*
H5C0.32030.04720.05820.050*
C60.2393 (3)0.0607 (2)0.1451 (2)0.0164 (6)
C70.2049 (3)0.0395 (3)0.1478 (2)0.0241 (7)
H70.13030.08810.11110.029*
C80.2800 (3)0.0681 (2)0.2044 (2)0.0206 (7)
H80.25370.13640.20640.025*
C90.4215 (3)0.0925 (2)0.2543 (2)0.0194 (6)
H90.49760.13880.29090.023*
C100.3497 (3)0.1273 (2)0.2007 (2)0.0220 (7)
H100.37600.19720.20200.026*
C110.7779 (4)0.3892 (3)0.1410 (3)0.0438 (10)
H11A0.69940.41500.18430.066*
H11B0.75770.32350.07990.066*
H11C0.85970.37170.17700.066*
C120.8038 (4)0.4762 (3)0.1133 (3)0.0328 (8)
C130.7788 (3)0.4731 (3)0.0195 (2)0.0255 (7)
C140.8102 (4)0.5627 (3)0.0036 (3)0.0370 (9)
C150.7880 (5)0.5631 (3)0.0974 (3)0.0508 (12)
H15A0.80720.63380.09170.076*
H15B0.84980.50450.14480.076*
H15C0.69230.55140.12170.076*
C160.7194 (3)0.3772 (2)0.0642 (2)0.0235 (7)
C170.7965 (3)0.3002 (3)0.1439 (2)0.0252 (7)
H170.89020.30770.14720.030*
C180.7346 (3)0.2121 (3)0.2185 (2)0.0221 (7)
H180.78860.16000.27220.027*
C190.5291 (3)0.2716 (3)0.1418 (2)0.0245 (7)
H190.43510.26280.14120.029*
C200.5826 (3)0.3599 (3)0.0642 (2)0.0283 (8)
H200.52670.40920.01060.034*
C210.2290 (3)0.6006 (3)0.4710 (3)0.0273 (7)
H21A0.24070.67600.46310.041*
H21B0.13880.58600.44200.041*
H21C0.23520.54990.54260.041*
C220.3392 (3)0.5852 (3)0.4182 (2)0.0236 (7)
C230.3380 (3)0.4930 (2)0.4003 (2)0.0182 (6)
C240.4495 (3)0.4833 (2)0.3537 (2)0.0232 (7)
C250.4587 (4)0.3874 (3)0.3338 (3)0.0342 (9)
H25A0.49370.32800.39480.051*
H25B0.36720.36240.31400.051*
H25C0.52130.40850.27940.051*
C260.2210 (3)0.4037 (2)0.4311 (2)0.0169 (6)
C270.2391 (3)0.3009 (2)0.5084 (2)0.0186 (6)
H270.32480.28750.54540.022*
C280.1315 (3)0.2180 (2)0.5311 (2)0.0165 (6)
H280.14580.14830.58450.020*
C290.0094 (3)0.3313 (2)0.4081 (2)0.0197 (6)
H290.09650.34300.37310.024*
C300.0933 (3)0.4178 (2)0.3811 (2)0.0195 (6)
H300.07610.48700.32820.023*
Atomic displacement parameters (Å2) top
U11U22U33U12U13U23
Cd10.01101 (11)0.01454 (10)0.01177 (10)0.00073 (8)0.00071 (8)0.00502 (8)
Cd20.00964 (10)0.01305 (10)0.01458 (11)0.00053 (8)0.00095 (8)0.00500 (8)
Cl10.0121 (3)0.0132 (3)0.0141 (3)0.0014 (3)0.0011 (3)0.0055 (3)
Cl20.0121 (3)0.0143 (3)0.0174 (3)0.0008 (3)0.0012 (3)0.0051 (3)
Cl30.0133 (3)0.0197 (3)0.0186 (3)0.0013 (3)0.0035 (3)0.0106 (3)
Cl40.0132 (3)0.0164 (3)0.0146 (3)0.0029 (3)0.0010 (3)0.0044 (3)
O10.0319 (14)0.0429 (14)0.0270 (13)0.0038 (11)0.0119 (11)0.0240 (11)
O20.0268 (14)0.0389 (14)0.0338 (14)0.0058 (11)0.0041 (11)0.0217 (12)
O30.0498 (18)0.0362 (16)0.0269 (14)0.0024 (14)0.0129 (13)0.0014 (12)
O40.0450 (18)0.0296 (14)0.0456 (17)0.0136 (13)0.0016 (14)0.0033 (12)
O50.0235 (13)0.0208 (12)0.0476 (16)0.0070 (10)0.0153 (11)0.0164 (11)
O60.0232 (13)0.0181 (11)0.0440 (15)0.0063 (9)0.0080 (11)0.0150 (11)
N10.0120 (12)0.0160 (12)0.0140 (12)0.0026 (10)0.0004 (9)0.0055 (10)
N20.0167 (13)0.0198 (12)0.0144 (12)0.0010 (10)0.0010 (10)0.0057 (10)
N30.0135 (13)0.0150 (12)0.0148 (12)0.0008 (10)0.0028 (10)0.0059 (10)
C10.0250 (19)0.044 (2)0.032 (2)0.0085 (16)0.0048 (15)0.0187 (17)
C20.0188 (17)0.0269 (17)0.0268 (17)0.0005 (13)0.0043 (13)0.0162 (14)
C30.0130 (15)0.0245 (15)0.0219 (16)0.0019 (12)0.0060 (12)0.0136 (13)
C40.0227 (17)0.0264 (17)0.0205 (16)0.0043 (14)0.0067 (13)0.0116 (14)
C50.031 (2)0.048 (2)0.0241 (18)0.0061 (18)0.0001 (15)0.0180 (17)
C60.0170 (16)0.0206 (15)0.0131 (14)0.0012 (12)0.0016 (12)0.0087 (12)
C70.0199 (17)0.0290 (17)0.0272 (17)0.0080 (13)0.0146 (14)0.0159 (14)
C80.0223 (17)0.0217 (15)0.0207 (16)0.0037 (13)0.0076 (13)0.0122 (13)
C90.0166 (16)0.0194 (15)0.0222 (16)0.0028 (12)0.0069 (12)0.0092 (13)
C100.0227 (17)0.0175 (15)0.0269 (17)0.0003 (13)0.0066 (14)0.0100 (13)
C110.057 (3)0.038 (2)0.028 (2)0.011 (2)0.0002 (19)0.0116 (17)
C120.030 (2)0.0257 (18)0.0231 (18)0.0052 (15)0.0031 (15)0.0030 (14)
C130.0239 (18)0.0200 (16)0.0204 (16)0.0022 (13)0.0009 (14)0.0020 (13)
C140.031 (2)0.0286 (19)0.037 (2)0.0079 (16)0.0019 (17)0.0000 (16)
C150.068 (3)0.038 (2)0.046 (3)0.020 (2)0.008 (2)0.014 (2)
C160.0246 (18)0.0205 (16)0.0215 (16)0.0015 (13)0.0002 (13)0.0064 (13)
C170.0185 (17)0.0260 (17)0.0254 (17)0.0063 (14)0.0002 (14)0.0055 (14)
C180.0180 (16)0.0241 (16)0.0187 (15)0.0021 (13)0.0021 (13)0.0055 (13)
C190.0127 (16)0.0317 (18)0.0245 (17)0.0012 (13)0.0031 (13)0.0082 (14)
C200.0258 (19)0.0269 (17)0.0222 (17)0.0007 (15)0.0059 (14)0.0014 (14)
C210.0262 (19)0.0206 (16)0.038 (2)0.0003 (14)0.0073 (15)0.0152 (15)
C220.0193 (17)0.0207 (16)0.0291 (18)0.0017 (13)0.0005 (14)0.0098 (14)
C230.0161 (16)0.0139 (14)0.0215 (15)0.0031 (12)0.0025 (12)0.0060 (12)
C240.0173 (16)0.0157 (15)0.0333 (18)0.0019 (12)0.0047 (14)0.0081 (14)
C250.034 (2)0.0270 (18)0.046 (2)0.0034 (16)0.0158 (18)0.0193 (17)
C260.0147 (15)0.0171 (14)0.0232 (16)0.0019 (12)0.0057 (12)0.0127 (13)
C270.0153 (15)0.0168 (14)0.0228 (16)0.0031 (12)0.0030 (12)0.0084 (12)
C280.0149 (15)0.0151 (14)0.0192 (15)0.0019 (11)0.0003 (12)0.0075 (12)
C290.0173 (16)0.0201 (15)0.0203 (15)0.0037 (12)0.0018 (12)0.0079 (13)
C300.0210 (17)0.0131 (14)0.0202 (15)0.0004 (12)0.0000 (13)0.0043 (12)
Geometric parameters (Å, º) top
Cd1—N12.347 (2)C7—H70.9500
Cd1—N22.358 (2)C8—H80.9500
Cd1—Cl3i2.5800 (7)C9—C101.385 (4)
Cd1—Cl22.5992 (7)C9—H90.9500
Cd1—Cl1i2.6542 (7)C10—H100.9500
Cd1—Cl12.6800 (7)C11—C121.487 (5)
Cd2—N32.360 (2)C11—H11A0.9800
Cd2—Cl4ii2.5885 (7)C11—H11B0.9800
Cd2—Cl22.5987 (7)C11—H11C0.9800
Cd2—Cl32.6135 (7)C12—C131.375 (5)
Cd2—Cl42.6400 (7)C13—C141.432 (5)
Cd2—Cl12.7544 (7)C13—C161.493 (4)
Cl1—Cd1i2.6542 (7)C14—C151.498 (5)
Cl3—Cd1i2.5800 (7)C15—H15A0.9800
Cl4—Cd2ii2.5885 (7)C15—H15B0.9800
O1—C41.302 (4)C15—H15C0.9800
O2—C21.281 (4)C16—C171.394 (4)
O2—H2D0.841 (18)C16—C201.398 (4)
O3—C121.313 (4)C17—C181.390 (4)
O3—H3D0.880 (18)C17—H170.9500
O4—C141.272 (4)C18—H180.9500
O5—C241.297 (3)C19—C201.373 (4)
O5—H5D0.859 (18)C19—H190.9500
O6—C221.295 (4)C20—H200.9500
N1—C81.331 (4)C21—C221.493 (4)
N1—C91.343 (3)C21—H21A0.9800
N2—C181.336 (4)C21—H21B0.9800
N2—C191.344 (4)C21—H21C0.9800
N3—C281.332 (4)C22—C231.405 (4)
N3—C291.349 (3)C23—C241.408 (4)
C1—C21.486 (4)C23—C261.499 (4)
C1—H1A0.9800C24—C251.491 (4)
C1—H1B0.9800C25—H25A0.9800
C1—H1C0.9800C25—H25B0.9800
C2—C31.414 (4)C25—H25C0.9800
C3—C41.400 (4)C26—C301.382 (4)
C3—C61.493 (4)C26—C271.389 (4)
C4—C51.490 (5)C27—C281.386 (4)
C5—H5A0.9800C27—H270.9500
C5—H5B0.9800C28—H280.9500
C5—H5C0.9800C29—C301.382 (4)
C6—C71.387 (4)C29—H290.9500
C6—C101.390 (4)C30—H300.9500
C7—C81.384 (4)
N1—Cd1—N293.94 (8)N1—C9—C10122.1 (3)
N1—Cd1—Cl3i91.38 (6)N1—C9—H9118.9
N2—Cd1—Cl3i92.61 (6)C10—C9—H9118.9
N1—Cd1—Cl291.88 (6)C9—C10—C6120.4 (3)
N2—Cd1—Cl285.55 (6)C9—C10—H10119.8
Cl3i—Cd1—Cl2176.36 (2)C6—C10—H10119.8
N1—Cd1—Cl1i173.05 (6)C12—C11—H11A109.5
N2—Cd1—Cl1i91.79 (6)C12—C11—H11B109.5
Cl3i—Cd1—Cl1i84.42 (2)H11A—C11—H11B109.5
Cl2—Cd1—Cl1i92.48 (2)C12—C11—H11C109.5
N1—Cd1—Cl186.84 (6)H11A—C11—H11C109.5
N2—Cd1—Cl1170.48 (6)H11B—C11—H11C109.5
Cl3i—Cd1—Cl196.86 (2)O3—C12—C13122.1 (3)
Cl2—Cd1—Cl184.94 (2)O3—C12—C11112.5 (3)
Cl1i—Cd1—Cl188.16 (2)C13—C12—C11125.4 (3)
N3—Cd2—Cl4ii91.69 (6)C12—C13—C14119.2 (3)
N3—Cd2—Cl291.04 (6)C12—C13—C16119.9 (3)
Cl4ii—Cd2—Cl2172.39 (2)C14—C13—C16120.9 (3)
N3—Cd2—Cl394.90 (6)O4—C14—C13120.9 (4)
Cl4ii—Cd2—Cl393.40 (2)O4—C14—C15117.4 (3)
Cl2—Cd2—Cl393.45 (2)C13—C14—C15121.7 (3)
N3—Cd2—Cl487.86 (6)C14—C15—H15A109.5
Cl4ii—Cd2—Cl483.73 (2)C14—C15—H15B109.5
Cl2—Cd2—Cl489.28 (2)H15A—C15—H15B109.5
Cl3—Cd2—Cl4176.08 (2)C14—C15—H15C109.5
N3—Cd2—Cl1173.39 (6)H15A—C15—H15C109.5
Cl4ii—Cd2—Cl194.23 (2)H15B—C15—H15C109.5
Cl2—Cd2—Cl183.46 (2)C17—C16—C20117.0 (3)
Cl3—Cd2—Cl181.83 (2)C17—C16—C13122.4 (3)
Cl4—Cd2—Cl195.70 (2)C20—C16—C13120.6 (3)
Cd1i—Cl1—Cd191.84 (2)C18—C17—C16119.2 (3)
Cd1i—Cl1—Cd294.11 (2)C18—C17—H17120.4
Cd1—Cl1—Cd292.96 (2)C16—C17—H17120.4
Cd2—Cl2—Cd198.61 (2)N2—C18—C17123.5 (3)
Cd1i—Cl3—Cd299.36 (2)N2—C18—H18118.3
Cd2ii—Cl4—Cd296.27 (2)C17—C18—H18118.3
C2—O2—H2D105 (3)N2—C19—C20123.1 (3)
C12—O3—H3D101 (3)N2—C19—H19118.5
C24—O5—H5D102 (2)C20—C19—H19118.5
C8—N1—C9117.8 (2)C19—C20—C16120.0 (3)
C8—N1—Cd1121.87 (19)C19—C20—H20120.0
C9—N1—Cd1120.23 (19)C16—C20—H20120.0
C18—N2—C19117.3 (3)C22—C21—H21A109.5
C18—N2—Cd1120.26 (19)C22—C21—H21B109.5
C19—N2—Cd1122.2 (2)H21A—C21—H21B109.5
C28—N3—C29117.1 (3)C22—C21—H21C109.5
C28—N3—Cd2120.99 (18)H21A—C21—H21C109.5
C29—N3—Cd2120.74 (19)H21B—C21—H21C109.5
C2—C1—H1A109.5O6—C22—C23120.0 (3)
C2—C1—H1B109.5O6—C22—C21116.4 (3)
H1A—C1—H1B109.5C23—C22—C21123.5 (3)
C2—C1—H1C109.5C22—C23—C24119.5 (3)
H1A—C1—H1C109.5C22—C23—C26121.2 (3)
H1B—C1—H1C109.5C24—C23—C26119.3 (3)
O2—C2—C3121.7 (3)O5—C24—C23120.5 (3)
O2—C2—C1116.5 (3)O5—C24—C25116.3 (3)
C3—C2—C1121.8 (3)C23—C24—C25123.3 (3)
C4—C3—C2119.1 (3)C24—C25—H25A109.5
C4—C3—C6120.8 (3)C24—C25—H25B109.5
C2—C3—C6120.1 (3)H25A—C25—H25B109.5
O1—C4—C3120.7 (3)C24—C25—H25C109.5
O1—C4—C5115.8 (3)H25A—C25—H25C109.5
C3—C4—C5123.5 (3)H25B—C25—H25C109.5
C4—C5—H5A109.5C30—C26—C27117.1 (3)
C4—C5—H5B109.5C30—C26—C23122.0 (3)
H5A—C5—H5B109.5C27—C26—C23120.8 (3)
C4—C5—H5C109.5C28—C27—C26119.5 (3)
H5A—C5—H5C109.5C28—C27—H27120.2
H5B—C5—H5C109.5C26—C27—H27120.2
C7—C6—C10116.8 (3)N3—C28—C27123.4 (3)
C7—C6—C3121.4 (3)N3—C28—H28118.3
C10—C6—C3121.8 (3)C27—C28—H28118.3
C8—C7—C6119.6 (3)N3—C29—C30122.7 (3)
C8—C7—H7120.2N3—C29—H29118.6
C6—C7—H7120.2C30—C29—H29118.6
N1—C8—C7123.3 (3)C26—C30—C29120.1 (3)
N1—C8—H8118.4C26—C30—H30119.9
C7—C8—H8118.4C29—C30—H30119.9
Symmetry codes: (i) x+1, y, z+1; (ii) x, y, z+1.
(2) top
Crystal data top
C30H33Br4Cd2N3O6V = 1796.0 (4) Å3
Mr = 1076.03Z = 2
Triclinic, P1F(000) = 1036
a = 7.1262 (9) ÅDx = 1.990 Mg m3
b = 15.519 (2) ÅMo Kα radiation, λ = 0.71073 Å
c = 16.597 (2) ŵ = 5.68 mm1
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 microsourceRint = 0.084
ω scansθmax = 26.4°, θmin = 1.2°
Absorption correction: multi-scan
TWINABS
h = 88
Tmin = 0.522, Tmax = 0.746k = 1919
7336 measured reflectionsl = 020
7336 independent reflections
Refinement top
Refinement on F211 restraints
Least-squares matrix: fullHydrogen site location: mixed
R[F2 > 2σ(F2)] = 0.056H 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 reflectionsΔρmax = 0.99 e Å3
423 parametersΔρmin = 0.91 e Å3
Crystal data top
C30H33Br4Cd2N3O6γ = 98.609 (3)°
Mr = 1076.03V = 1796.0 (4) Å3
Triclinic, P1Z = 2
a = 7.1262 (9) ÅMo Kα radiation
b = 15.519 (2) ŵ = 5.68 mm1
c = 16.597 (2) ÅT = 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 = 0.746Rint = 0.084
7336 measured reflections
Refinement top
R[F2 > 2σ(F2)] = 0.05611 restraints
wR(F2) = 0.103H atoms treated by a mixture of independent and constrained refinement
S = 1.14Δρmax = 0.99 e Å3
7336 reflectionsΔρmin = 0.91 e Å3
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
xyzUiso*/UeqOcc. (<1)
Cd10.79198 (10)0.62721 (3)0.25945 (4)0.01556 (14)
Cd20.25939 (10)0.53220 (3)0.25449 (4)0.01486 (14)
Br10.60807 (13)0.53188 (6)0.36106 (5)0.0176 (2)
Br20.45375 (13)0.65869 (5)0.17413 (5)0.0179 (2)
Br30.08678 (13)0.53698 (6)0.14634 (5)0.0177 (2)
Br40.14362 (13)0.64469 (6)0.35535 (5)0.0187 (2)
O11.0537 (13)1.1873 (5)0.1974 (5)0.047 (2)
H1D1.156 (11)1.184 (8)0.229 (7)0.071*
O21.3530 (11)1.1631 (4)0.2822 (4)0.041 (2)
O30.2057 (10)0.0872 (4)0.5199 (5)0.0393 (19)
O40.4688 (11)0.1715 (4)0.5194 (4)0.0326 (18)
H4D0.398 (13)0.133 (5)0.524 (7)0.049*
O50.7676 (10)0.1848 (4)0.0443 (4)0.0276 (16)
H5D0.661 (8)0.151 (6)0.054 (7)0.041*
O60.4521 (11)0.1011 (4)0.0559 (5)0.042 (2)
N10.8823 (11)0.7761 (4)0.2520 (5)0.0215 (18)
N20.1016 (11)0.4196 (4)0.3242 (4)0.0189 (17)
N30.3468 (10)0.4274 (4)0.1689 (4)0.0149 (16)
C10.7914 (18)1.0759 (6)0.1580 (8)0.053 (4)
H1A0.70061.10400.18470.079*
H1B0.75721.01240.15860.079*
H1C0.78661.09370.10150.079*
C20.9908 (17)1.1032 (6)0.2025 (6)0.037 (3)
C31.0967 (16)1.0481 (6)0.2453 (6)0.030 (2)
C41.2892 (16)1.0843 (6)0.2844 (6)0.029 (2)
C51.4084 (15)1.0280 (6)0.3344 (6)0.038 (3)
H5A1.43700.98130.29940.056*
H5B1.33791.00230.37700.056*
H5C1.52861.06330.35960.056*
C61.0238 (14)0.9527 (5)0.2482 (5)0.0212 (18)
C71.1014 (16)0.8911 (6)0.2087 (6)0.034 (3)
H71.20340.90840.17840.040*
C81.0298 (16)0.8030 (6)0.2134 (6)0.032 (2)
H81.08890.76080.18800.038*
C90.8082 (14)0.8368 (6)0.2889 (7)0.033 (2)
H90.70250.81830.31690.039*
C100.8731 (14)0.9235 (6)0.2895 (7)0.031 (2)
H100.81530.96370.31810.037*
C110.0715 (15)0.1332 (7)0.4622 (8)0.043 (3)
H11A0.17030.16300.50480.064*
H11B0.09290.15650.40930.064*
H11C0.07820.07050.46100.064*
C120.1170 (16)0.1471 (6)0.4795 (7)0.033 (3)
C130.1977 (14)0.2205 (5)0.4578 (5)0.022 (2)
C140.3749 (14)0.2287 (6)0.4788 (6)0.022 (2)
C150.4769 (13)0.3058 (5)0.4583 (6)0.022 (2)
H15A0.57350.29050.41020.033*
H15B0.38370.35560.44710.033*
H15C0.53960.32110.50440.033*
C160.0932 (13)0.2901 (5)0.4113 (5)0.0155 (19)
C170.1302 (14)0.2923 (6)0.3276 (5)0.024 (2)
H170.22470.24960.29760.029*
C180.0297 (14)0.3568 (6)0.2879 (6)0.028 (2)
H180.05680.35600.23020.034*
C190.1390 (12)0.4175 (6)0.4061 (5)0.018 (2)
H190.23690.46030.43410.022*
C200.0430 (13)0.3568 (6)0.4512 (5)0.021 (2)
H200.06920.36030.50900.025*
C210.8654 (14)0.3226 (6)0.0267 (6)0.026 (2)
H21A0.96190.30530.06860.039*
H21B0.80440.36830.04940.039*
H21C0.92730.34480.01950.039*
C220.7181 (14)0.2459 (5)0.0012 (5)0.019 (2)
C230.5285 (13)0.2351 (5)0.0194 (5)0.0155 (19)
C240.3999 (15)0.1602 (6)0.0107 (7)0.033 (3)
C25A0.187 (3)0.159 (3)0.008 (3)0.036 (10)*0.40 (7)
H25A0.11640.10210.02810.053*0.40 (7)
H25B0.14170.20460.04220.053*0.40 (7)
H25C0.16660.17030.04830.053*0.40 (7)
C25B0.205 (3)0.1342 (17)0.0178 (17)0.029 (6)*0.60 (7)
H25D0.10500.12190.02960.043*0.60 (7)
H25E0.17680.18210.05150.043*0.60 (7)
H25F0.20710.08200.04990.043*0.60 (7)
C260.4665 (12)0.3030 (6)0.0703 (6)0.018 (2)
C270.4847 (14)0.2987 (6)0.1546 (5)0.023 (2)
H270.53780.25200.18040.028*
C280.4274 (14)0.3606 (6)0.2001 (6)0.025 (2)
H280.44530.35640.25760.030*
C290.3335 (13)0.4330 (6)0.0888 (6)0.020 (2)
H290.28200.48110.06510.024*
C300.3894 (13)0.3737 (6)0.0376 (5)0.021 (2)
H300.37530.38110.01940.025*
Atomic displacement parameters (Å2) top
U11U22U33U12U13U23
Cd10.0144 (3)0.0157 (3)0.0173 (3)0.0039 (3)0.0031 (2)0.0010 (3)
Cd20.0145 (3)0.0175 (3)0.0135 (3)0.0039 (3)0.0033 (2)0.0007 (3)
Br10.0146 (5)0.0223 (4)0.0152 (4)0.0017 (4)0.0007 (4)0.0043 (4)
Br20.0155 (5)0.0208 (4)0.0181 (4)0.0039 (4)0.0034 (4)0.0060 (4)
Br30.0165 (5)0.0218 (4)0.0153 (4)0.0061 (4)0.0005 (4)0.0011 (4)
Br40.0154 (5)0.0246 (4)0.0158 (5)0.0043 (4)0.0011 (4)0.0040 (4)
O10.071 (7)0.018 (3)0.047 (5)0.006 (4)0.013 (4)0.006 (3)
O20.063 (6)0.018 (3)0.034 (4)0.004 (3)0.008 (4)0.003 (3)
O30.031 (5)0.037 (4)0.050 (5)0.002 (3)0.011 (4)0.021 (4)
O40.029 (4)0.034 (4)0.033 (4)0.003 (3)0.004 (4)0.015 (3)
O50.028 (4)0.030 (4)0.027 (4)0.008 (3)0.009 (3)0.009 (3)
O60.035 (5)0.028 (4)0.062 (6)0.006 (3)0.002 (4)0.026 (4)
N10.027 (5)0.017 (3)0.021 (4)0.008 (3)0.001 (4)0.001 (3)
N20.018 (4)0.022 (4)0.015 (4)0.002 (3)0.001 (3)0.003 (3)
N30.019 (4)0.014 (3)0.015 (4)0.002 (3)0.010 (3)0.004 (3)
C10.069 (9)0.023 (5)0.057 (8)0.004 (6)0.023 (7)0.011 (5)
C20.058 (8)0.022 (5)0.027 (6)0.004 (5)0.006 (5)0.006 (4)
C30.035 (6)0.027 (5)0.028 (6)0.002 (5)0.004 (5)0.005 (4)
C40.044 (7)0.027 (5)0.016 (5)0.006 (5)0.000 (5)0.002 (4)
C50.037 (7)0.035 (6)0.037 (6)0.010 (5)0.009 (5)0.003 (5)
C60.030 (5)0.014 (3)0.020 (5)0.011 (3)0.005 (4)0.004 (3)
C70.051 (7)0.018 (4)0.035 (6)0.005 (4)0.029 (5)0.004 (4)
C80.047 (7)0.018 (3)0.033 (6)0.004 (5)0.022 (5)0.001 (4)
C90.024 (6)0.023 (4)0.052 (7)0.008 (4)0.006 (5)0.005 (5)
C100.021 (5)0.022 (4)0.052 (7)0.011 (4)0.008 (4)0.012 (4)
C110.023 (6)0.034 (6)0.072 (9)0.012 (5)0.002 (6)0.012 (6)
C120.031 (6)0.022 (5)0.047 (7)0.002 (4)0.010 (5)0.004 (5)
C130.034 (6)0.018 (4)0.014 (5)0.007 (4)0.000 (4)0.001 (4)
C140.026 (6)0.019 (4)0.023 (5)0.006 (4)0.007 (4)0.001 (4)
C150.023 (5)0.021 (5)0.020 (5)0.003 (4)0.002 (4)0.002 (4)
C160.022 (5)0.007 (4)0.018 (5)0.005 (3)0.002 (4)0.000 (3)
C170.023 (6)0.028 (5)0.016 (5)0.009 (4)0.005 (4)0.006 (4)
C180.033 (6)0.036 (6)0.011 (5)0.001 (5)0.004 (4)0.001 (4)
C190.008 (4)0.022 (4)0.023 (5)0.006 (4)0.004 (4)0.004 (4)
C200.025 (5)0.028 (5)0.009 (4)0.001 (4)0.005 (4)0.002 (4)
C210.025 (6)0.030 (5)0.026 (5)0.009 (4)0.010 (4)0.004 (4)
C220.028 (6)0.013 (4)0.018 (5)0.008 (4)0.001 (4)0.004 (4)
C230.024 (5)0.009 (4)0.016 (4)0.007 (4)0.007 (4)0.001 (3)
C240.018 (6)0.031 (5)0.049 (7)0.009 (4)0.004 (5)0.014 (5)
C260.004 (4)0.024 (5)0.025 (5)0.003 (4)0.000 (4)0.001 (4)
C270.033 (6)0.022 (5)0.014 (5)0.012 (4)0.008 (4)0.001 (4)
C280.031 (6)0.026 (5)0.019 (5)0.006 (4)0.000 (4)0.004 (4)
C290.016 (5)0.019 (4)0.025 (5)0.009 (4)0.001 (4)0.000 (4)
C300.026 (6)0.025 (5)0.014 (5)0.011 (4)0.004 (4)0.008 (4)
Geometric parameters (Å, º) top
Cd1—N12.315 (7)C9—H90.9500
Cd1—Br12.6240 (11)C10—H100.9500
Cd1—Br3i2.6314 (11)C11—C121.457 (14)
Cd1—Br22.7384 (12)C11—H11A0.9800
Cd1—Br4i2.7512 (12)C11—H11B0.9800
Cd2—N32.345 (7)C11—H11C0.9800
Cd2—N22.349 (7)C12—C131.383 (13)
Cd2—Br42.6858 (11)C13—C141.378 (13)
Cd2—Br22.7124 (10)C13—C161.507 (12)
Cd2—Br12.8461 (12)C14—C151.512 (12)
Cd2—Br32.8562 (12)C15—H15A0.9800
Br3—Cd1ii2.6314 (11)C15—H15B0.9800
Br4—Cd1ii2.7512 (12)C15—H15C0.9800
O1—C21.323 (12)C16—C171.379 (12)
O1—H1D0.84 (2)C16—C201.396 (12)
O2—C41.242 (11)C17—C181.376 (12)
O3—C121.297 (11)C17—H170.9500
O4—C141.289 (11)C18—H180.9500
O4—H4D0.84 (2)C19—C201.376 (11)
O5—C221.296 (10)C19—H190.9500
O5—H5D0.85 (2)C20—H200.9500
O6—C241.301 (11)C21—C221.484 (12)
N1—C81.324 (12)C21—H21A0.9800
N1—C91.325 (11)C21—H21B0.9800
N2—C181.317 (11)C21—H21C0.9800
N2—C191.351 (11)C22—C231.425 (12)
N3—C291.325 (11)C23—C241.403 (12)
N3—C281.339 (11)C23—C261.491 (11)
C1—C21.504 (15)C24—C25A1.520 (19)
C1—H1A0.9800C24—C25B1.531 (16)
C1—H1B0.9800C25A—H25A0.9800
C1—H1C0.9800C25A—H25B0.9800
C2—C31.371 (14)C25A—H25C0.9800
C3—C41.458 (15)C25B—H25D0.9800
C3—C61.497 (11)C25B—H25E0.9800
C4—C51.495 (14)C25B—H25F0.9800
C5—H5A0.9800C26—C301.387 (12)
C5—H5B0.9800C26—C271.391 (12)
C5—H5C0.9800C27—C281.353 (12)
C6—C71.371 (12)C27—H270.9500
C6—C101.378 (13)C28—H280.9500
C7—C81.394 (12)C29—C301.376 (12)
C7—H70.9500C29—H290.9500
C8—H80.9500C30—H300.9500
C9—C101.355 (12)
N1—Cd1—Br1132.91 (18)H11A—C11—H11B109.5
N1—Cd1—Br3i112.59 (18)C12—C11—H11C109.5
Br1—Cd1—Br3i114.44 (3)H11A—C11—H11C109.5
N1—Cd1—Br283.7 (2)H11B—C11—H11C109.5
Br1—Cd1—Br291.20 (4)O3—C12—C13120.5 (10)
Br3i—Cd1—Br299.21 (4)O3—C12—C11115.9 (9)
N1—Cd1—Br4i81.2 (2)C13—C12—C11123.6 (9)
Br1—Cd1—Br4i95.13 (4)C14—C13—C12119.2 (9)
Br3i—Cd1—Br4i91.55 (4)C14—C13—C16120.6 (8)
Br2—Cd1—Br4i163.98 (3)C12—C13—C16120.2 (9)
N3—Cd2—N289.4 (2)O4—C14—C13123.0 (9)
N3—Cd2—Br4176.55 (16)O4—C14—C15113.2 (8)
N2—Cd2—Br487.25 (18)C13—C14—C15123.8 (8)
N3—Cd2—Br288.95 (16)C14—C15—H15A109.5
N2—Cd2—Br2177.7 (2)C14—C15—H15B109.5
Br4—Cd2—Br294.40 (3)H15A—C15—H15B109.5
N3—Cd2—Br189.62 (19)C14—C15—H15C109.5
N2—Cd2—Br191.23 (19)H15A—C15—H15C109.5
Br4—Cd2—Br191.39 (3)H15B—C15—H15C109.5
Br2—Cd2—Br187.13 (3)C17—C16—C20116.7 (8)
N3—Cd2—Br390.89 (19)C17—C16—C13121.9 (8)
N2—Cd2—Br390.18 (19)C20—C16—C13121.4 (8)
Br4—Cd2—Br388.19 (3)C18—C17—C16119.7 (8)
Br2—Cd2—Br391.47 (3)C18—C17—H17120.1
Br1—Cd2—Br3178.51 (3)C16—C17—H17120.1
Cd1—Br1—Cd289.36 (3)N2—C18—C17124.6 (9)
Cd2—Br2—Cd189.86 (3)N2—C18—H18117.7
Cd1ii—Br3—Cd288.98 (3)C17—C18—H18117.7
Cd2—Br4—Cd1ii90.13 (3)N2—C19—C20123.5 (8)
C2—O1—H1D92 (9)N2—C19—H19118.2
C14—O4—H4D102 (8)C20—C19—H19118.2
C22—O5—H5D100 (7)C19—C20—C16119.4 (8)
C8—N1—C9117.1 (8)C19—C20—H20120.3
C8—N1—Cd1117.7 (6)C16—C20—H20120.3
C9—N1—Cd1125.0 (6)C22—C21—H21A109.5
C18—N2—C19116.0 (7)C22—C21—H21B109.5
C18—N2—Cd2123.4 (6)H21A—C21—H21B109.5
C19—N2—Cd2120.6 (5)C22—C21—H21C109.5
C29—N3—C28115.9 (8)H21A—C21—H21C109.5
C29—N3—Cd2123.3 (6)H21B—C21—H21C109.5
C28—N3—Cd2120.6 (6)O5—C22—C23118.8 (8)
C2—C1—H1A109.5O5—C22—C21117.7 (8)
C2—C1—H1B109.5C23—C22—C21123.4 (8)
H1A—C1—H1B109.5C24—C23—C22118.8 (8)
C2—C1—H1C109.5C24—C23—C26120.6 (8)
H1A—C1—H1C109.5C22—C23—C26120.6 (7)
H1B—C1—H1C109.5O6—C24—C23121.0 (9)
O1—C2—C3122.9 (10)O6—C24—C25A118.6 (13)
O1—C2—C1112.7 (9)C23—C24—C25A118.6 (15)
C3—C2—C1124.4 (9)O6—C24—C25B114.8 (10)
C2—C3—C4117.7 (9)C23—C24—C25B123.4 (10)
C2—C3—C6121.6 (10)C24—C25A—H25A109.5
C4—C3—C6120.5 (9)C24—C25A—H25B109.5
O2—C4—C3121.5 (10)H25A—C25A—H25B109.5
O2—C4—C5118.2 (10)C24—C25A—H25C109.5
C3—C4—C5120.0 (9)H25A—C25A—H25C109.5
C4—C5—H5A109.5H25B—C25A—H25C109.5
C4—C5—H5B109.5C24—C25B—H25D109.5
H5A—C5—H5B109.5C24—C25B—H25E109.5
C4—C5—H5C109.5H25D—C25B—H25E109.5
H5A—C5—H5C109.5C24—C25B—H25F109.5
H5B—C5—H5C109.5H25D—C25B—H25F109.5
C7—C6—C10117.2 (8)H25E—C25B—H25F109.5
C7—C6—C3121.6 (9)C30—C26—C27116.1 (8)
C10—C6—C3121.2 (8)C30—C26—C23122.9 (8)
C6—C7—C8119.7 (9)C27—C26—C23120.9 (8)
C6—C7—H7120.1C28—C27—C26120.4 (9)
C8—C7—H7120.1C28—C27—H27119.8
N1—C8—C7122.2 (9)C26—C27—H27119.8
N1—C8—H8118.9N3—C28—C27123.8 (9)
C7—C8—H8118.9N3—C28—H28118.1
N1—C9—C10124.3 (10)C27—C28—H28118.1
N1—C9—H9117.8N3—C29—C30124.4 (8)
C10—C9—H9117.8N3—C29—H29117.8
C9—C10—C6119.4 (8)C30—C29—H29117.8
C9—C10—H10120.3C29—C30—C26119.3 (8)
C6—C10—H10120.3C29—C30—H30120.4
C12—C11—H11A109.5C26—C30—H30120.4
C12—C11—H11B109.5
Symmetry codes: (i) x+1, y, z; (ii) x1, y, z.
(3a) top
Crystal data top
C10H11CdI2NO2Dx = 2.573 Mg m3
Mr = 543.41Mo Kα radiation, λ = 0.71073 Å
Orthorhombic, PbcaCell parameters from 7521 reflections
a = 7.1002 (9) Åθ = 2.8–28.3°
b = 14.3490 (18) ŵ = 5.94 mm1
c = 27.540 (4) ÅT = 100 K
V = 2805.7 (6) Å3Rod, colorless
Z = 80.27 × 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 opticsRint = 0.047
ωs scansθmax = 30.9°, θmin = 2.8°
Absorption correction: multi-scan
SADABS
h = 99
Tmin = 0.474, Tmax = 0.746k = 2020
39565 measured reflectionsl = 3837
4234 independent reflections
Refinement top
Refinement on F2Primary atom site location: heavy-atom method
Least-squares matrix: fullHydrogen site location: mixed
R[F2 > 2σ(F2)] = 0.024H-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 reflectionsΔρmax = 0.69 e Å3
147 parametersΔρmin = 0.59 e Å3
0 restraints
Crystal data top
C10H11CdI2NO2V = 2805.7 (6) Å3
Mr = 543.41Z = 8
Orthorhombic, PbcaMo Kα radiation
a = 7.1002 (9) ŵ = 5.94 mm1
b = 14.3490 (18) ÅT = 100 K
c = 27.540 (4) Å0.27 × 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 = 0.746Rint = 0.047
39565 measured reflections
Refinement top
R[F2 > 2σ(F2)] = 0.0240 restraints
wR(F2) = 0.051H-atom parameters constrained
S = 1.11Δρmax = 0.69 e Å3
4234 reflectionsΔρmin = 0.59 e Å3
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
xyzUiso*/Ueq
Cd10.69629 (3)0.49466 (2)0.21095 (2)0.01580 (5)
I10.57192 (2)0.44443 (2)0.30413 (2)0.01675 (5)
I20.55761 (3)0.66218 (2)0.18766 (2)0.02204 (5)
O10.0032 (3)0.14714 (17)0.02937 (8)0.0315 (5)
O20.2705 (4)0.04421 (15)0.03192 (8)0.0288 (5)
H2A0.16060.07850.02730.035*
N10.5538 (3)0.38827 (16)0.16261 (9)0.0171 (5)
C10.0167 (5)0.2973 (2)0.06472 (12)0.0292 (7)
H1A0.00180.31300.09910.044*
H1B0.15080.28960.05730.044*
H1C0.03570.34750.04470.044*
C20.0851 (4)0.2083 (2)0.05408 (11)0.0237 (6)
C30.2730 (4)0.1909 (2)0.07071 (10)0.0204 (6)
C40.3580 (5)0.1074 (2)0.05812 (10)0.0220 (6)
C50.5572 (5)0.0814 (2)0.07039 (12)0.0267 (7)
H5A0.62170.13530.08450.040*
H5B0.62300.06180.04080.040*
H5C0.55690.03000.09380.040*
C60.3708 (4)0.25965 (19)0.10214 (10)0.0164 (5)
C70.4242 (4)0.23656 (19)0.14947 (10)0.0166 (5)
H70.39830.17620.16200.020*
C80.5147 (4)0.30172 (19)0.17803 (10)0.0166 (5)
H80.55090.28450.21000.020*
C90.5022 (4)0.4111 (2)0.11701 (10)0.0189 (6)
H90.52870.47230.10570.023*
C100.4126 (4)0.3497 (2)0.08606 (10)0.0196 (6)
H100.37960.36860.05410.024*
Atomic displacement parameters (Å2) top
U11U22U33U12U13U23
Cd10.01426 (10)0.01552 (10)0.01762 (10)0.00023 (7)0.00036 (7)0.00089 (7)
I10.01327 (9)0.02015 (9)0.01684 (9)0.00166 (7)0.00018 (7)0.00260 (6)
I20.01971 (10)0.01640 (9)0.03001 (11)0.00180 (7)0.00241 (8)0.00231 (7)
O10.0297 (13)0.0426 (14)0.0223 (11)0.0082 (11)0.0041 (10)0.0091 (10)
O20.0389 (14)0.0226 (11)0.0248 (11)0.0087 (10)0.0041 (10)0.0083 (9)
N10.0154 (12)0.0163 (11)0.0197 (11)0.0020 (9)0.0012 (9)0.0018 (9)
C10.0275 (17)0.0362 (18)0.0239 (16)0.0031 (15)0.0097 (13)0.0005 (13)
C20.0250 (16)0.0302 (16)0.0159 (13)0.0052 (13)0.0012 (12)0.0013 (12)
C30.0247 (15)0.0214 (14)0.0150 (13)0.0050 (12)0.0009 (11)0.0020 (11)
C40.0297 (16)0.0225 (14)0.0139 (13)0.0064 (13)0.0041 (12)0.0016 (11)
C50.0353 (19)0.0216 (15)0.0234 (15)0.0016 (13)0.0058 (14)0.0038 (12)
C60.0165 (13)0.0166 (12)0.0162 (13)0.0005 (11)0.0034 (10)0.0026 (10)
C70.0174 (13)0.0140 (12)0.0183 (13)0.0015 (10)0.0020 (11)0.0008 (10)
C80.0178 (14)0.0162 (13)0.0158 (12)0.0030 (11)0.0013 (10)0.0005 (10)
C90.0193 (14)0.0172 (13)0.0201 (14)0.0012 (11)0.0032 (11)0.0001 (11)
C100.0244 (15)0.0195 (14)0.0150 (13)0.0020 (11)0.0002 (11)0.0003 (11)
Geometric parameters (Å, º) top
Cd1—N12.264 (2)C3—C41.386 (4)
Cd1—I22.6756 (4)C3—C61.484 (4)
Cd1—I1i2.7938 (4)C4—C51.502 (5)
Cd1—I12.8079 (4)C5—H5A0.9800
I1—Cd1ii2.7938 (4)C5—H5B0.9800
O1—C21.275 (4)C5—H5C0.9800
O2—C41.315 (4)C6—C71.397 (4)
O2—H2A0.9311C6—C101.398 (4)
N1—C81.341 (4)C7—C81.381 (4)
N1—C91.349 (4)C7—H70.9500
C1—C21.496 (5)C8—H80.9500
C1—H1A0.9800C9—C101.381 (4)
C1—H1B0.9800C9—H90.9500
C1—H1C0.9800C10—H100.9500
C2—C31.433 (4)
N1—Cd1—I2107.48 (6)O2—C4—C5113.4 (3)
N1—Cd1—I1i99.50 (6)C3—C4—C5124.7 (3)
I2—Cd1—I1i123.193 (9)C4—C5—H5A109.5
N1—Cd1—I1102.93 (6)C4—C5—H5B109.5
I2—Cd1—I1109.508 (9)H5A—C5—H5B109.5
I1i—Cd1—I1111.711 (9)C4—C5—H5C109.5
Cd1ii—I1—Cd195.629 (8)H5A—C5—H5C109.5
C4—O2—H2A96.1H5B—C5—H5C109.5
C8—N1—C9117.6 (2)C7—C6—C10117.2 (3)
C8—N1—Cd1122.05 (19)C7—C6—C3120.9 (2)
C9—N1—Cd1120.33 (19)C10—C6—C3121.9 (3)
C2—C1—H1A109.5C8—C7—C6119.8 (3)
C2—C1—H1B109.5C8—C7—H7120.1
H1A—C1—H1B109.5C6—C7—H7120.1
C2—C1—H1C109.5N1—C8—C7122.9 (3)
H1A—C1—H1C109.5N1—C8—H8118.6
H1B—C1—H1C109.5C7—C8—H8118.6
O1—C2—C3120.6 (3)N1—C9—C10123.0 (3)
O1—C2—C1117.0 (3)N1—C9—H9118.5
C3—C2—C1122.4 (3)C10—C9—H9118.5
C4—C3—C2118.4 (3)C9—C10—C6119.5 (3)
C4—C3—C6121.1 (3)C9—C10—H10120.3
C2—C3—C6120.4 (3)C6—C10—H10120.3
O2—C4—C3121.9 (3)
Symmetry codes: (i) x+1/2, y, z+1/2; (ii) x1/2, y, z+1/2.
(3b) top
Crystal data top
C20H22CdI2N2O4Dx = 2.031 Mg m3
Mr = 720.59Mo Kα radiation, λ = 0.71073 Å
Orthorhombic, Pca21Cell parameters from 9971 reflections
a = 13.5307 (3) Åθ = 3.0–27.5°
b = 7.0913 (7) ŵ = 3.57 mm1
c = 49.110 (2) ÅT = 100 K
V = 4712.1 (5) Å3Block, colorless
Z = 80.25 × 0.13 × 0.11 mm
F(000) = 2736
Data collection top
CCD area detector
diffractometer
12009 reflections with I > 2σ(I)
Radiation source: Incoatec microsourceRint = 0.051
ω scansθmax = 31.0°, θmin = 0.8°
Absorption correction: multi-scan
SADABS
h = 1919
Tmin = 0.522, Tmax = 0.746k = 910
67491 measured reflectionsl = 6969
14053 independent reflections
Refinement top
Refinement on F2Hydrogen site location: mixed
Least-squares matrix: fullH 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 = 1.09Δρmax = 1.29 e Å3
14053 reflectionsΔρmin = 1.11 e Å3
545 parametersAbsolute structure: Refined as an inversion twin.
5 restraintsAbsolute structure parameter: 0.41 (3)
Primary atom site location: heavy-atom method
Crystal data top
C20H22CdI2N2O4V = 4712.1 (5) Å3
Mr = 720.59Z = 8
Orthorhombic, Pca21Mo Kα radiation
a = 13.5307 (3) ŵ = 3.57 mm1
b = 7.0913 (7) ÅT = 100 K
c = 49.110 (2) Å0.25 × 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 = 0.746Rint = 0.051
67491 measured reflections
Refinement top
R[F2 > 2σ(F2)] = 0.038H atoms treated by a mixture of independent and constrained refinement
wR(F2) = 0.076Δρmax = 1.29 e Å3
S = 1.09Δρmin = 1.11 e Å3
14053 reflectionsAbsolute structure: Refined as an inversion twin.
545 parametersAbsolute 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
xyzUiso*/Ueq
Cd10.30627 (4)0.36841 (8)0.64474 (2)0.02432 (12)
Cd20.28575 (4)0.87015 (8)0.89541 (2)0.02364 (12)
I10.43978 (4)0.55273 (8)0.67561 (2)0.03312 (13)
I20.17999 (4)0.56014 (9)0.61261 (2)0.03726 (14)
I30.41806 (4)1.05371 (8)0.86404 (2)0.03288 (13)
I40.15884 (4)1.06226 (9)0.92741 (2)0.03673 (14)
O10.6759 (5)0.2054 (11)0.52992 (16)0.0421 (17)
H2D0.611 (7)0.405 (14)0.532 (2)0.063*
O20.5705 (5)0.4815 (11)0.53894 (16)0.0404 (18)
O30.0596 (4)0.3191 (10)0.75141 (15)0.0394 (17)
O40.0988 (5)0.4791 (9)0.75788 (15)0.0382 (16)
H4D0.037 (2)0.468 (13)0.7594 (19)0.03 (3)*
O50.6556 (5)0.2950 (11)1.00989 (15)0.0408 (17)
O60.5501 (6)0.0203 (11)1.00127 (16)0.0434 (19)
H6D0.597 (6)0.086 (16)1.007 (3)0.065*
O70.0672 (5)0.0308 (9)0.78276 (16)0.0328 (15)
O80.0892 (4)0.1927 (10)0.79063 (15)0.0359 (15)
H8D0.042 (5)0.120 (12)0.787 (2)0.054*
N10.3794 (5)0.1445 (9)0.61770 (14)0.0241 (14)
N20.2219 (4)0.1639 (9)0.67232 (15)0.0217 (14)
N30.3581 (5)0.6455 (10)0.92216 (15)0.0256 (15)
N40.2018 (4)0.6680 (9)0.86758 (16)0.0222 (14)
C10.6432 (7)0.1010 (14)0.5479 (2)0.038 (2)
H1A0.58120.16980.54500.057*
H1B0.69120.13800.53390.057*
H1C0.66960.13110.56600.057*
C20.6240 (7)0.1082 (14)0.5460 (2)0.037 (2)
C30.5440 (6)0.1901 (13)0.56074 (18)0.0281 (18)
C40.5199 (7)0.3763 (14)0.55600 (19)0.034 (2)
C50.4363 (7)0.4761 (15)0.5697 (3)0.044 (3)
H5A0.39220.52940.55590.067*
H5B0.39950.38660.58100.067*
H5C0.46250.57770.58110.067*
C60.4846 (6)0.0776 (12)0.58078 (18)0.0269 (18)
C70.3939 (7)0.0039 (16)0.5746 (2)0.040 (2)
H70.36500.02900.55740.048*
C80.3441 (6)0.1059 (16)0.5931 (2)0.036 (2)
H80.28160.15650.58810.043*
C90.4664 (7)0.0725 (16)0.6240 (2)0.044 (3)
H90.49290.09990.64150.052*
C100.5207 (8)0.0394 (16)0.60691 (19)0.045 (3)
H100.58220.09030.61270.054*
C110.0823 (6)0.0549 (14)0.7223 (2)0.041 (2)
H11A0.08340.05650.73410.062*
H11B0.14960.10360.72020.062*
H11C0.05570.02040.70440.062*
C120.0180 (5)0.2046 (12)0.73495 (19)0.0297 (19)
C130.0834 (5)0.2189 (11)0.72850 (18)0.0248 (17)
C140.1399 (6)0.3549 (11)0.74132 (17)0.0244 (16)
C150.2504 (6)0.3671 (12)0.74015 (18)0.0301 (17)
H15A0.27390.31270.72300.045*
H15B0.27080.49950.74120.045*
H15C0.27890.29710.75550.045*
C160.1296 (5)0.0851 (11)0.70889 (16)0.0208 (15)
C170.1676 (5)0.1466 (12)0.68429 (18)0.0249 (17)
H170.16250.27590.67940.030*
C180.2130 (6)0.0205 (12)0.66659 (17)0.0264 (17)
H180.23870.06640.64980.032*
C190.1833 (5)0.2249 (12)0.69609 (19)0.0251 (17)
H190.18770.35570.70010.030*
C200.1378 (5)0.1087 (11)0.71490 (18)0.0241 (16)
H200.11260.15830.73150.029*
C210.6219 (8)0.5991 (14)0.9920 (2)0.040 (2)
H21A0.68050.62981.00290.060*
H21B0.56490.66910.99900.060*
H21C0.63360.63400.97300.060*
C220.6020 (7)0.3943 (13)0.99381 (18)0.033 (2)
C230.5232 (7)0.3076 (14)0.97888 (18)0.0307 (19)
C240.4990 (7)0.1203 (13)0.98374 (19)0.033 (2)
C250.4174 (7)0.0185 (15)0.9707 (2)0.040 (2)
H25A0.42340.02930.95090.060*
H25B0.35440.07300.97660.060*
H25C0.42000.11470.97600.060*
C260.4647 (6)0.4231 (12)0.9592 (2)0.0294 (19)
C270.5001 (8)0.4609 (16)0.9336 (2)0.048 (3)
H270.56210.41120.92800.058*
C280.4453 (7)0.5719 (17)0.9157 (2)0.042 (3)
H280.47150.59600.89810.051*
C290.3233 (7)0.6063 (14)0.94684 (19)0.033 (2)
H290.26080.65680.95180.040*
C300.3725 (7)0.4962 (18)0.96585 (19)0.041 (2)
H300.34370.47120.98310.049*
C310.2210 (5)0.1418 (11)0.7982 (2)0.0302 (18)
H31A0.24850.24370.78710.045*
H31B0.24200.01980.79080.045*
H31C0.24490.15430.81700.045*
C320.1109 (5)0.1532 (11)0.79793 (17)0.0248 (16)
C330.0576 (5)0.2933 (11)0.81165 (18)0.0204 (15)
C340.0449 (6)0.3086 (12)0.80657 (18)0.0265 (17)
C350.1065 (6)0.4602 (13)0.8180 (2)0.038 (2)
H35A0.17570.43900.81300.057*
H35B0.08460.58200.81080.057*
H35C0.10030.46050.83790.057*
C360.1069 (5)0.4259 (11)0.83073 (16)0.0194 (15)
C370.1160 (5)0.6178 (11)0.82572 (17)0.0216 (15)
H370.09000.67010.80940.026*
C380.1625 (5)0.7324 (12)0.84434 (17)0.0225 (16)
H380.16690.86350.84050.027*
C390.1927 (6)0.4820 (12)0.87278 (19)0.0277 (19)
H390.21970.43340.88920.033*
C400.1458 (5)0.3598 (12)0.85521 (18)0.0236 (17)
H400.13990.23010.85980.028*
Atomic displacement parameters (Å2) top
U11U22U33U12U13U23
Cd10.0314 (3)0.0157 (3)0.0259 (3)0.0011 (2)0.0030 (2)0.0001 (3)
Cd20.0304 (3)0.0157 (3)0.0248 (3)0.0014 (2)0.0037 (2)0.0009 (3)
I10.0279 (2)0.0268 (3)0.0447 (4)0.00334 (19)0.0004 (2)0.0056 (3)
I20.0508 (3)0.0254 (3)0.0356 (4)0.0062 (2)0.0060 (3)0.0057 (3)
I30.0273 (2)0.0267 (3)0.0446 (4)0.00326 (19)0.0006 (2)0.0056 (3)
I40.0498 (3)0.0259 (3)0.0345 (3)0.0060 (2)0.0057 (3)0.0059 (3)
O10.059 (4)0.037 (4)0.030 (4)0.007 (3)0.019 (3)0.005 (3)
O20.066 (5)0.027 (4)0.029 (4)0.002 (3)0.014 (3)0.006 (3)
O30.037 (3)0.035 (4)0.046 (4)0.017 (3)0.015 (3)0.006 (3)
O40.043 (4)0.030 (4)0.042 (4)0.011 (3)0.006 (3)0.009 (3)
O50.060 (4)0.034 (4)0.029 (4)0.005 (3)0.019 (3)0.000 (3)
O60.080 (5)0.025 (4)0.025 (4)0.006 (3)0.015 (3)0.002 (3)
O70.044 (3)0.021 (3)0.034 (4)0.005 (3)0.006 (3)0.005 (3)
O80.024 (3)0.036 (4)0.048 (4)0.009 (2)0.010 (3)0.000 (3)
N10.042 (4)0.014 (3)0.015 (3)0.005 (3)0.002 (3)0.002 (3)
N20.025 (3)0.017 (3)0.024 (4)0.000 (2)0.001 (2)0.001 (3)
N30.032 (3)0.021 (4)0.024 (4)0.003 (3)0.004 (3)0.001 (3)
N40.021 (3)0.014 (3)0.032 (4)0.002 (2)0.003 (2)0.001 (3)
C10.046 (5)0.029 (5)0.038 (6)0.003 (4)0.015 (4)0.005 (4)
C20.051 (5)0.034 (5)0.025 (5)0.003 (4)0.005 (4)0.010 (4)
C30.044 (5)0.019 (4)0.021 (4)0.001 (3)0.007 (3)0.002 (3)
C40.056 (6)0.029 (5)0.017 (4)0.001 (4)0.006 (4)0.008 (4)
C50.067 (7)0.024 (6)0.042 (7)0.011 (4)0.011 (5)0.005 (5)
C60.047 (5)0.016 (4)0.017 (4)0.002 (3)0.004 (3)0.005 (3)
C70.049 (5)0.050 (7)0.021 (5)0.002 (5)0.002 (4)0.010 (5)
C80.026 (4)0.052 (7)0.028 (5)0.002 (4)0.003 (3)0.007 (5)
C90.046 (5)0.051 (7)0.034 (6)0.021 (4)0.011 (4)0.021 (5)
C100.062 (6)0.054 (7)0.019 (5)0.023 (5)0.006 (4)0.011 (4)
C110.021 (4)0.039 (6)0.063 (7)0.003 (4)0.008 (4)0.008 (5)
C120.018 (4)0.030 (5)0.041 (5)0.012 (3)0.002 (3)0.012 (4)
C130.026 (4)0.017 (4)0.031 (5)0.007 (3)0.001 (3)0.006 (3)
C140.032 (4)0.015 (4)0.026 (4)0.005 (3)0.003 (3)0.000 (3)
C150.033 (4)0.025 (4)0.032 (4)0.003 (3)0.002 (3)0.005 (4)
C160.015 (3)0.019 (4)0.028 (4)0.001 (3)0.002 (3)0.001 (3)
C170.030 (4)0.019 (4)0.026 (4)0.002 (3)0.001 (3)0.000 (3)
C180.039 (4)0.021 (4)0.020 (4)0.004 (3)0.001 (3)0.003 (3)
C190.020 (3)0.019 (4)0.037 (5)0.001 (3)0.005 (3)0.004 (3)
C200.022 (3)0.020 (4)0.031 (4)0.003 (3)0.002 (3)0.007 (3)
C210.056 (6)0.028 (5)0.037 (6)0.012 (4)0.015 (4)0.003 (4)
C220.052 (5)0.025 (5)0.021 (4)0.009 (4)0.008 (4)0.001 (4)
C230.048 (5)0.027 (5)0.017 (4)0.000 (4)0.008 (3)0.000 (3)
C240.056 (6)0.022 (5)0.020 (5)0.002 (4)0.008 (4)0.003 (4)
C250.065 (6)0.024 (5)0.031 (6)0.013 (4)0.008 (4)0.002 (4)
C260.043 (5)0.019 (5)0.026 (5)0.001 (3)0.009 (4)0.003 (4)
C270.052 (6)0.051 (7)0.042 (6)0.027 (5)0.004 (5)0.012 (5)
C280.055 (6)0.055 (7)0.017 (5)0.018 (5)0.006 (4)0.006 (5)
C290.042 (5)0.040 (6)0.017 (4)0.002 (4)0.001 (3)0.004 (4)
C300.043 (5)0.061 (7)0.017 (4)0.004 (5)0.000 (3)0.008 (5)
C310.025 (4)0.022 (4)0.043 (5)0.005 (3)0.003 (3)0.004 (4)
C320.030 (4)0.017 (4)0.028 (4)0.005 (3)0.003 (3)0.004 (3)
C330.015 (3)0.017 (4)0.029 (4)0.004 (3)0.004 (3)0.001 (3)
C340.028 (4)0.021 (4)0.031 (4)0.004 (3)0.000 (3)0.005 (3)
C350.018 (4)0.032 (5)0.064 (7)0.001 (3)0.007 (4)0.001 (5)
C360.013 (3)0.019 (4)0.026 (4)0.001 (2)0.002 (3)0.002 (3)
C370.020 (3)0.016 (4)0.029 (4)0.001 (3)0.003 (3)0.001 (3)
C380.021 (3)0.019 (4)0.028 (4)0.002 (3)0.004 (3)0.001 (3)
C390.030 (4)0.021 (4)0.032 (5)0.004 (3)0.004 (3)0.009 (4)
C400.024 (4)0.014 (4)0.033 (5)0.004 (3)0.006 (3)0.002 (3)
Geometric parameters (Å, º) top
Cd1—N22.289 (7)C13—C141.382 (11)
Cd1—N12.294 (7)C13—C161.489 (11)
Cd1—I22.6941 (9)C14—C151.499 (11)
Cd1—I12.6962 (8)C15—H15A0.9800
Cd2—N42.283 (7)C15—H15B0.9800
Cd2—N32.285 (7)C15—H15C0.9800
Cd2—I32.6966 (8)C16—C171.384 (11)
Cd2—I42.6973 (8)C16—C201.410 (11)
O1—C21.260 (12)C17—C181.391 (11)
O2—C41.314 (11)C17—H170.9500
O2—H2D0.84 (3)C18—H180.9500
O3—C121.277 (11)C19—C201.383 (12)
O4—C141.322 (10)C19—H190.9500
O4—H4D0.84 (3)C20—H200.9500
O5—C221.282 (11)C21—C221.480 (13)
O6—C241.313 (11)C21—H21A0.9800
O6—H6D0.84 (3)C21—H21B0.9800
O7—C321.288 (10)C21—H21C0.9800
O8—C341.284 (11)C22—C231.433 (12)
O8—H8D0.85 (3)C23—C241.389 (13)
N1—C91.320 (11)C23—C261.494 (12)
N1—C81.328 (12)C24—C251.465 (13)
N2—C181.343 (11)C25—H25A0.9800
N2—C191.350 (11)C25—H25B0.9800
N3—C281.329 (11)C25—H25C0.9800
N3—C291.330 (11)C26—C271.374 (14)
N4—C381.339 (11)C26—C301.389 (14)
N4—C391.349 (11)C27—C281.393 (13)
C1—C21.509 (13)C27—H270.9500
C1—H1A0.9800C28—H280.9500
C1—H1B0.9800C29—C301.387 (14)
C1—H1C0.9800C29—H290.9500
C2—C31.427 (12)C30—H300.9500
C3—C41.380 (13)C31—C321.492 (11)
C3—C61.500 (12)C31—H31A0.9800
C4—C51.493 (13)C31—H31B0.9800
C5—H5A0.9800C31—H31C0.9800
C5—H5B0.9800C32—C331.400 (11)
C5—H5C0.9800C33—C341.414 (10)
C6—C71.369 (14)C33—C361.486 (11)
C6—C101.400 (12)C34—C351.472 (12)
C7—C81.373 (14)C35—H35A0.9800
C7—H70.9500C35—H35B0.9800
C8—H80.9500C35—H35C0.9800
C9—C101.370 (13)C36—C371.389 (10)
C9—H90.9500C36—C401.393 (11)
C10—H100.9500C37—C381.376 (11)
C11—C121.506 (13)C37—H370.9500
C11—H11A0.9800C38—H380.9500
C11—H11B0.9800C39—C401.378 (12)
C11—H11C0.9800C39—H390.9500
C12—C131.412 (10)C40—H400.9500
N2—Cd1—N196.8 (2)C17—C16—C13121.3 (7)
N2—Cd1—I2110.49 (15)C20—C16—C13121.2 (7)
N1—Cd1—I2106.49 (18)C16—C17—C18120.5 (8)
N2—Cd1—I1107.98 (17)C16—C17—H17119.8
N1—Cd1—I1111.83 (17)C18—C17—H17119.8
I2—Cd1—I1120.64 (3)N2—C18—C17122.3 (8)
N4—Cd2—N396.9 (2)N2—C18—H18118.8
N4—Cd2—I3106.95 (18)C17—C18—H18118.8
N3—Cd2—I3112.36 (17)N2—C19—C20124.0 (8)
N4—Cd2—I4110.44 (16)N2—C19—H19118.0
N3—Cd2—I4106.84 (18)C20—C19—H19118.0
I3—Cd2—I4120.78 (3)C19—C20—C16118.4 (8)
C4—O2—H2D104 (9)C19—C20—H20120.8
C14—O4—H4D114 (6)C16—C20—H20120.8
C24—O6—H6D109 (10)C22—C21—H21A109.5
C34—O8—H8D100 (7)C22—C21—H21B109.5
C9—N1—C8117.1 (8)H21A—C21—H21B109.5
C9—N1—Cd1121.0 (6)C22—C21—H21C109.5
C8—N1—Cd1120.9 (6)H21A—C21—H21C109.5
C18—N2—C19117.3 (7)H21B—C21—H21C109.5
C18—N2—Cd1122.5 (5)O5—C22—C23120.0 (9)
C19—N2—Cd1120.1 (5)O5—C22—C21118.2 (9)
C28—N3—C29116.8 (8)C23—C22—C21121.8 (8)
C28—N3—Cd2121.1 (6)C24—C23—C22119.9 (8)
C29—N3—Cd2121.2 (6)C24—C23—C26120.7 (8)
C38—N4—C39117.3 (7)C22—C23—C26119.4 (8)
C38—N4—Cd2119.6 (5)O6—C24—C23120.3 (9)
C39—N4—Cd2123.1 (6)O6—C24—C25114.6 (9)
C2—C1—H1A109.5C23—C24—C25125.0 (8)
C2—C1—H1B109.5C24—C25—H25A109.5
H1A—C1—H1B109.5C24—C25—H25B109.5
C2—C1—H1C109.5H25A—C25—H25B109.5
H1A—C1—H1C109.5C24—C25—H25C109.5
H1B—C1—H1C109.5H25A—C25—H25C109.5
O1—C2—C3121.2 (9)H25B—C25—H25C109.5
O1—C2—C1118.8 (8)C27—C26—C30117.1 (8)
C3—C2—C1119.9 (9)C27—C26—C23121.0 (8)
C4—C3—C2118.9 (8)C30—C26—C23121.9 (9)
C4—C3—C6119.5 (8)C26—C27—C28120.2 (9)
C2—C3—C6121.6 (8)C26—C27—H27119.9
O2—C4—C3121.8 (8)C28—C27—H27119.9
O2—C4—C5114.3 (9)N3—C28—C27122.9 (9)
C3—C4—C5123.8 (9)N3—C28—H28118.6
C4—C5—H5A109.5C27—C28—H28118.6
C4—C5—H5B109.5N3—C29—C30124.1 (9)
H5A—C5—H5B109.5N3—C29—H29117.9
C4—C5—H5C109.5C30—C29—H29117.9
H5A—C5—H5C109.5C29—C30—C26118.9 (9)
H5B—C5—H5C109.5C29—C30—H30120.6
C7—C6—C10116.2 (8)C26—C30—H30120.6
C7—C6—C3122.6 (8)C32—C31—H31A109.5
C10—C6—C3121.2 (8)C32—C31—H31B109.5
C6—C7—C8120.7 (9)H31A—C31—H31B109.5
C6—C7—H7119.6C32—C31—H31C109.5
C8—C7—H7119.6H31A—C31—H31C109.5
N1—C8—C7122.8 (8)H31B—C31—H31C109.5
N1—C8—H8118.6O7—C32—C33121.4 (7)
C7—C8—H8118.6O7—C32—C31115.3 (7)
N1—C9—C10123.9 (9)C33—C32—C31123.2 (7)
N1—C9—H9118.1C32—C33—C34118.3 (7)
C10—C9—H9118.1C32—C33—C36121.4 (6)
C9—C10—C6119.2 (9)C34—C33—C36120.2 (7)
C9—C10—H10120.4O8—C34—C33121.1 (8)
C6—C10—H10120.4O8—C34—C35115.9 (7)
C12—C11—H11A109.5C33—C34—C35123.0 (8)
C12—C11—H11B109.5C34—C35—H35A109.5
H11A—C11—H11B109.5C34—C35—H35B109.5
C12—C11—H11C109.5H35A—C35—H35B109.5
H11A—C11—H11C109.5C34—C35—H35C109.5
H11B—C11—H11C109.5H35A—C35—H35C109.5
O3—C12—C13121.7 (9)H35B—C35—H35C109.5
O3—C12—C11117.0 (7)C37—C36—C40116.7 (7)
C13—C12—C11121.3 (8)C37—C36—C33123.2 (7)
C14—C13—C12119.0 (8)C40—C36—C33120.0 (7)
C14—C13—C16120.4 (6)C38—C37—C36120.1 (8)
C12—C13—C16120.5 (8)C38—C37—H37120.0
O4—C14—C13120.8 (7)C36—C37—H37120.0
O4—C14—C15113.9 (7)N4—C38—C37123.2 (8)
C13—C14—C15125.1 (7)N4—C38—H38118.4
C14—C15—H15A109.5C37—C38—H38118.4
C14—C15—H15B109.5N4—C39—C40122.6 (8)
H15A—C15—H15B109.5N4—C39—H39118.7
C14—C15—H15C109.5C40—C39—H39118.7
H15A—C15—H15C109.5C39—C40—C36120.1 (8)
H15B—C15—H15C109.5C39—C40—H40119.9
C17—C16—C20117.5 (7)C36—C40—H40119.9
(4) top
Crystal data top
C60H60CdCl2Fe2N6O12·6(CH4O)·6(H2O)Z = 1
Mr = 1652.50F(000) = 860
Triclinic, P1Dx = 1.364 Mg m3
a = 12.1351 (13) ÅMo Kα radiation, λ = 0.71073 Å
b = 13.2343 (14) ÅCell parameters from 4039 reflections
c = 13.8728 (15) Åθ = 2.3–25.2°
α = 91.809 (2)°µ = 0.76 mm1
β = 109.675 (2)°T = 100 K
γ = 104.825 (2)°Block, red
V = 2011.0 (4) Å30.25 × 0.23 × 0.08 mm
Data collection top
CCD area detector
diffractometer
6746 reflections with I > 2σ(I)
Radiation source: Incoatec microsourceRint = 0.050
ω scansθmax = 26.6°, θmin = 2.1°
Absorption correction: multi-scan
SADABS
h = 1515
Tmin = 0.640, Tmax = 0.745k = 1616
24575 measured reflectionsl = 1717
8416 independent reflections
Refinement top
Refinement on F2Primary atom site location: heavy-atom method
Least-squares matrix: fullHydrogen site location: mixed
R[F2 > 2σ(F2)] = 0.049H-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 reflectionsΔρmax = 1.12 e Å3
456 parametersΔρmin = 0.92 e Å3
0 restraints
Crystal data top
C60H60CdCl2Fe2N6O12·6(CH4O)·6(H2O)γ = 104.825 (2)°
Mr = 1652.50V = 2011.0 (4) Å3
Triclinic, P1Z = 1
a = 12.1351 (13) ÅMo Kα radiation
b = 13.2343 (14) ŵ = 0.76 mm1
c = 13.8728 (15) ÅT = 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 = 0.745Rint = 0.050
24575 measured reflections
Refinement top
R[F2 > 2σ(F2)] = 0.0490 restraints
wR(F2) = 0.130H-atom parameters constrained
S = 1.04Δρmax = 1.12 e Å3
8416 reflectionsΔρmin = 0.92 e Å3
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
xyzUiso*/Ueq
Cd10.50001.00000.00000.01625 (11)
Fe10.04526 (5)0.39589 (4)0.25295 (4)0.01632 (13)
Cl10.66071 (9)1.03831 (7)0.18977 (7)0.0242 (2)
O10.1302 (2)0.3878 (2)0.20690 (19)0.0203 (5)
O20.0389 (2)0.3848 (2)0.39246 (19)0.0194 (5)
O30.0580 (2)0.41432 (19)0.11412 (18)0.0179 (5)
O40.1003 (2)0.55232 (19)0.27828 (19)0.0209 (6)
O50.0013 (2)0.24041 (19)0.2114 (2)0.0202 (5)
O60.2166 (2)0.38829 (19)0.30313 (19)0.0202 (5)
N10.4459 (3)0.3006 (3)0.5008 (3)0.0297 (8)
N20.4054 (3)0.8368 (2)0.0417 (2)0.0190 (6)
N30.3676 (3)0.0662 (2)0.0592 (2)0.0202 (7)
C10.3358 (4)0.3574 (4)0.1891 (3)0.0301 (9)
H1A0.33990.38190.12240.045*
H1B0.36990.39970.22440.045*
H1C0.38300.28310.17800.045*
C20.2051 (4)0.3690 (3)0.2544 (3)0.0208 (8)
C30.1727 (3)0.3581 (3)0.3599 (3)0.0187 (7)
C40.0521 (3)0.3649 (3)0.4234 (3)0.0188 (8)
C50.0220 (4)0.3478 (3)0.5346 (3)0.0253 (8)
H5A0.06650.36210.56810.038*
H5B0.06210.27470.53900.038*
H5C0.05080.39550.56940.038*
C60.2693 (3)0.3375 (3)0.4073 (3)0.0210 (8)
C70.3505 (4)0.2385 (3)0.3943 (3)0.0264 (9)
H70.34750.18130.35310.032*
C80.4360 (4)0.2240 (3)0.4421 (3)0.0304 (9)
H80.49070.15570.43240.037*
C90.3676 (4)0.3957 (3)0.5136 (3)0.0284 (9)
H90.37250.45130.55560.034*
C100.2797 (4)0.4172 (3)0.4689 (3)0.0249 (8)
H100.22630.48640.48010.030*
C110.1586 (4)0.4620 (3)0.0029 (3)0.0209 (8)
H11A0.10410.39280.03840.031*
H11B0.24350.46030.01730.031*
H11C0.14510.51550.04940.031*
C120.1324 (3)0.4885 (3)0.0912 (3)0.0163 (7)
C130.1878 (3)0.5892 (3)0.1493 (3)0.0191 (8)
C140.1625 (3)0.6173 (3)0.2368 (3)0.0200 (8)
C150.2056 (4)0.7299 (3)0.2846 (3)0.0327 (10)
H15A0.18350.73520.34590.049*
H15B0.16710.77270.23460.049*
H15C0.29450.75570.30440.049*
C160.2647 (3)0.6728 (3)0.1107 (3)0.0189 (8)
C170.2112 (4)0.7224 (3)0.0283 (3)0.0221 (8)
H170.12510.70190.00550.027*
C180.2842 (4)0.8022 (3)0.0045 (3)0.0218 (8)
H180.24620.83360.06250.026*
C190.4569 (4)0.7887 (3)0.1207 (3)0.0224 (8)
H190.54320.81160.15370.027*
C200.3913 (4)0.7069 (3)0.1570 (3)0.0220 (8)
H200.43230.67450.21280.026*
C210.0097 (4)0.0817 (3)0.1240 (4)0.0325 (10)
H21A0.08730.05910.13530.049*
H21B0.03820.03230.14960.049*
H21C0.02560.08290.05000.049*
C220.0605 (4)0.1903 (3)0.1808 (3)0.0203 (8)
C230.1848 (3)0.2323 (3)0.1958 (3)0.0203 (8)
C240.2557 (3)0.3292 (3)0.2559 (3)0.0200 (8)
C250.3877 (4)0.3725 (3)0.2671 (3)0.0271 (9)
H25A0.39260.40730.20680.041*
H25B0.42540.31470.27230.041*
H25C0.43080.42360.32970.041*
C260.2444 (4)0.1708 (3)0.1471 (3)0.0216 (8)
C270.3045 (4)0.1011 (3)0.1989 (3)0.0274 (9)
H270.30390.08760.26560.033*
C280.3647 (4)0.0517 (3)0.1535 (3)0.0282 (9)
H280.40620.00510.19070.034*
C290.3046 (4)0.1279 (3)0.0069 (3)0.0236 (8)
H290.30210.13590.06160.028*
C300.2425 (4)0.1812 (3)0.0473 (3)0.0254 (9)
H300.19870.22470.00700.031*
O70.5547 (3)0.9488 (3)0.3692 (2)0.0441 (8)
H7D0.57130.89120.37860.066*
H7E0.59210.97280.32990.066*
O80.3377 (4)0.9766 (3)0.4157 (3)0.0560 (10)
H8D0.35830.98910.48370.084*
H8E0.38920.96650.38770.084*
O90.0765 (6)0.9115 (5)0.3225 (5)0.133 (3)
H9D0.15350.93070.35000.199*
H9E0.02340.93790.32970.199*
C310.7300 (6)0.7744 (6)0.4712 (5)0.076 (2)
H31A0.78900.80780.43970.114*
H31B0.74060.70550.48870.114*
H31C0.74330.81930.53400.114*
O100.6090 (3)0.7609 (3)0.3999 (2)0.0360 (7)
H10D0.56330.74020.43210.054*
O110.0971 (6)0.9975 (5)0.3463 (5)0.1045 (18)
H11D0.16061.00820.30520.157*
C320.0730 (7)1.0923 (6)0.4115 (6)0.086 (2)
H32A0.00591.09550.47630.130*
H32B0.14621.09320.42620.130*
H32C0.05021.15320.37670.130*
O120.1019 (6)0.7605 (5)0.1721 (5)0.117 (2)*
H12D0.05410.81530.21240.175*
C330.1876 (9)0.6941 (8)0.2100 (8)0.122 (3)*
H33A0.15420.63850.24250.183*
H33B0.26440.66220.15240.183*
H33C0.20280.73640.26090.183*
Atomic displacement parameters (Å2) top
U11U22U33U12U13U23
Cd10.0179 (2)0.01283 (18)0.0212 (2)0.00305 (14)0.01184 (16)0.00333 (14)
Fe10.0181 (3)0.0154 (3)0.0187 (3)0.0032 (2)0.0118 (2)0.0032 (2)
Cl10.0265 (5)0.0221 (5)0.0213 (4)0.0026 (4)0.0087 (4)0.0027 (4)
O10.0227 (14)0.0230 (13)0.0205 (13)0.0058 (11)0.0144 (11)0.0052 (10)
O20.0194 (13)0.0215 (13)0.0208 (13)0.0044 (11)0.0124 (11)0.0038 (10)
O30.0181 (13)0.0167 (12)0.0184 (13)0.0002 (10)0.0095 (11)0.0020 (10)
O40.0286 (15)0.0190 (13)0.0198 (13)0.0051 (11)0.0154 (12)0.0041 (10)
O50.0206 (14)0.0175 (12)0.0261 (14)0.0033 (10)0.0144 (11)0.0031 (10)
O60.0189 (13)0.0201 (13)0.0214 (13)0.0033 (10)0.0090 (11)0.0011 (10)
N10.0235 (18)0.040 (2)0.0255 (18)0.0026 (16)0.0135 (15)0.0028 (15)
N20.0193 (16)0.0148 (15)0.0233 (16)0.0000 (12)0.0116 (13)0.0027 (12)
N30.0221 (17)0.0185 (15)0.0248 (16)0.0071 (13)0.0132 (14)0.0041 (13)
C10.023 (2)0.047 (3)0.025 (2)0.0101 (19)0.0139 (18)0.0042 (18)
C20.022 (2)0.0189 (18)0.0249 (19)0.0039 (15)0.0145 (16)0.0030 (15)
C30.0194 (19)0.0171 (17)0.0206 (18)0.0019 (14)0.0111 (15)0.0008 (14)
C40.024 (2)0.0151 (17)0.0201 (18)0.0016 (14)0.0141 (16)0.0005 (14)
C50.025 (2)0.034 (2)0.0206 (19)0.0084 (17)0.0135 (17)0.0041 (16)
C60.0174 (19)0.0259 (19)0.0189 (18)0.0022 (15)0.0086 (15)0.0000 (15)
C70.029 (2)0.026 (2)0.025 (2)0.0000 (17)0.0166 (18)0.0000 (16)
C80.025 (2)0.034 (2)0.029 (2)0.0024 (18)0.0131 (18)0.0006 (18)
C90.024 (2)0.038 (2)0.023 (2)0.0050 (18)0.0131 (17)0.0036 (17)
C100.020 (2)0.026 (2)0.027 (2)0.0006 (16)0.0124 (17)0.0023 (16)
C110.024 (2)0.0192 (18)0.0222 (19)0.0047 (15)0.0131 (16)0.0037 (15)
C120.0150 (17)0.0165 (17)0.0194 (18)0.0032 (14)0.0093 (14)0.0070 (14)
C130.0211 (19)0.0169 (17)0.0188 (18)0.0009 (15)0.0096 (15)0.0046 (14)
C140.0206 (19)0.0145 (17)0.0227 (19)0.0004 (14)0.0088 (16)0.0018 (14)
C150.050 (3)0.019 (2)0.028 (2)0.0012 (19)0.021 (2)0.0009 (16)
C160.024 (2)0.0159 (17)0.0179 (18)0.0003 (15)0.0126 (16)0.0003 (14)
C170.021 (2)0.0205 (18)0.0235 (19)0.0008 (15)0.0101 (16)0.0033 (15)
C180.024 (2)0.0194 (18)0.0188 (18)0.0015 (15)0.0075 (16)0.0030 (14)
C190.021 (2)0.0188 (18)0.028 (2)0.0038 (15)0.0105 (16)0.0058 (15)
C200.022 (2)0.0219 (19)0.0217 (19)0.0049 (15)0.0077 (16)0.0070 (15)
C210.030 (2)0.023 (2)0.046 (3)0.0034 (18)0.019 (2)0.0053 (18)
C220.024 (2)0.0173 (18)0.0226 (19)0.0050 (15)0.0119 (16)0.0043 (14)
C230.023 (2)0.0212 (18)0.0224 (19)0.0086 (15)0.0125 (16)0.0046 (15)
C240.0197 (19)0.0216 (18)0.0203 (18)0.0067 (15)0.0084 (15)0.0054 (14)
C250.021 (2)0.028 (2)0.033 (2)0.0065 (17)0.0119 (18)0.0035 (17)
C260.022 (2)0.0198 (18)0.026 (2)0.0042 (15)0.0133 (16)0.0010 (15)
C270.035 (2)0.032 (2)0.023 (2)0.0151 (18)0.0145 (18)0.0073 (16)
C280.037 (2)0.033 (2)0.026 (2)0.0210 (19)0.0170 (19)0.0119 (17)
C290.028 (2)0.025 (2)0.0217 (19)0.0095 (17)0.0125 (17)0.0064 (15)
C300.033 (2)0.024 (2)0.027 (2)0.0132 (17)0.0163 (18)0.0078 (16)
O70.066 (2)0.0371 (18)0.0358 (18)0.0145 (17)0.0268 (17)0.0089 (14)
O80.069 (3)0.049 (2)0.045 (2)0.0092 (19)0.020 (2)0.0024 (17)
O90.096 (5)0.122 (5)0.166 (6)0.045 (4)0.022 (4)0.038 (5)
C310.058 (4)0.106 (6)0.079 (5)0.031 (4)0.036 (4)0.027 (4)
O100.0265 (16)0.0488 (19)0.0375 (17)0.0063 (14)0.0196 (14)0.0172 (15)
O110.108 (5)0.107 (4)0.108 (4)0.052 (4)0.034 (4)0.020 (4)
C320.082 (5)0.064 (4)0.098 (6)0.019 (4)0.017 (4)0.018 (4)
Geometric parameters (Å, º) top
Cd1—N2i2.361 (3)C15—H15A0.9800
Cd1—N22.361 (3)C15—H15B0.9800
Cd1—N3ii2.363 (3)C15—H15C0.9800
Cd1—N3iii2.363 (3)C16—C171.387 (5)
Cd1—Cl1i2.6351 (9)C16—C201.393 (5)
Cd1—Cl12.6351 (9)C17—C181.390 (5)
Fe1—O21.971 (2)C17—H170.9500
Fe1—O11.979 (3)C18—H180.9500
Fe1—O41.986 (3)C19—C201.386 (5)
Fe1—O61.989 (3)C19—H190.9500
Fe1—O51.999 (3)C20—H200.9500
Fe1—O32.001 (2)C21—C221.505 (5)
O1—C21.274 (4)C21—H21A0.9800
O2—C41.284 (4)C21—H21B0.9800
O3—C121.281 (4)C21—H21C0.9800
O4—C141.278 (4)C22—C231.406 (5)
O5—C221.279 (4)C23—C241.402 (5)
O6—C241.277 (4)C23—C261.495 (5)
N1—C91.334 (5)C24—C251.508 (5)
N1—C81.334 (5)C25—H25A0.9800
N2—C181.336 (5)C25—H25B0.9800
N2—C191.336 (5)C25—H25C0.9800
N3—C291.327 (5)C26—C301.389 (5)
N3—C281.340 (5)C26—C271.391 (6)
N3—Cd1iv2.363 (3)C27—C281.373 (6)
C1—C21.503 (6)C27—H270.9500
C1—H1A0.9800C28—H280.9500
C1—H1B0.9800C29—C301.382 (5)
C1—H1C0.9800C29—H290.9500
C2—C31.404 (5)C30—H300.9500
C3—C41.408 (5)O7—H7D0.8400
C3—C61.500 (5)O7—H7E0.8418
C4—C51.501 (5)O8—H8D0.8880
C5—H5A0.9800O8—H8E0.8730
C5—H5B0.9800O9—H9D0.8455
C5—H5C0.9800O9—H9E0.8380
C6—C71.388 (5)C31—O101.429 (7)
C6—C101.393 (5)C31—H31A0.9800
C7—C81.387 (6)C31—H31B0.9800
C7—H70.9500C31—H31C0.9800
C8—H80.9500O10—H10D0.8242
C9—C101.380 (5)O11—C321.428 (8)
C9—H90.9500O11—H11D0.8400
C10—H100.9500C32—H32A0.9800
C11—C121.496 (5)C32—H32B0.9800
C11—H11A0.9800C32—H32C0.9800
C11—H11B0.9800O12—C331.435 (10)
C11—H11C0.9800O12—H12D0.8458
C12—C131.409 (5)C33—H33A0.9800
C13—C141.410 (5)C33—H33B0.9800
C13—C161.492 (5)C33—H33C0.9800
C14—C151.497 (5)
N2i—Cd1—N2180.0C12—C13—C14122.1 (3)
N2i—Cd1—N3ii85.20 (10)C12—C13—C16119.2 (3)
N2—Cd1—N3ii94.80 (10)C14—C13—C16118.3 (3)
N2i—Cd1—N3iii94.80 (10)O4—C14—C13124.1 (3)
N2—Cd1—N3iii85.20 (10)O4—C14—C15115.9 (3)
N3ii—Cd1—N3iii180.0C13—C14—C15120.0 (3)
N2i—Cd1—Cl1i87.95 (8)C14—C15—H15A109.5
N2—Cd1—Cl1i92.05 (8)C14—C15—H15B109.5
N3ii—Cd1—Cl1i89.60 (8)H15A—C15—H15B109.5
N3iii—Cd1—Cl1i90.40 (8)C14—C15—H15C109.5
N2i—Cd1—Cl192.05 (8)H15A—C15—H15C109.5
N2—Cd1—Cl187.95 (8)H15B—C15—H15C109.5
N3ii—Cd1—Cl190.40 (8)C17—C16—C20117.2 (3)
N3iii—Cd1—Cl189.60 (8)C17—C16—C13120.5 (3)
Cl1i—Cd1—Cl1180.0C20—C16—C13122.2 (3)
O2—Fe1—O186.53 (10)C16—C17—C18119.6 (4)
O2—Fe1—O492.33 (10)C16—C17—H17120.2
O1—Fe1—O494.13 (11)C18—C17—H17120.2
O2—Fe1—O690.75 (11)N2—C18—C17123.1 (4)
O1—Fe1—O6173.81 (10)N2—C18—H18118.4
O4—Fe1—O691.54 (11)C17—C18—H18118.4
O2—Fe1—O595.20 (10)N2—C19—C20123.5 (4)
O1—Fe1—O588.89 (11)N2—C19—H19118.3
O4—Fe1—O5172.05 (10)C20—C19—H19118.3
O6—Fe1—O585.82 (10)C19—C20—C16119.3 (3)
O2—Fe1—O3177.07 (10)C19—C20—H20120.3
O1—Fe1—O394.87 (10)C16—C20—H20120.3
O4—Fe1—O385.01 (10)C22—C21—H21A109.5
O6—Fe1—O388.11 (10)C22—C21—H21B109.5
O5—Fe1—O387.41 (10)H21A—C21—H21B109.5
C2—O1—Fe1131.1 (2)C22—C21—H21C109.5
C4—O2—Fe1130.8 (2)H21A—C21—H21C109.5
C12—O3—Fe1127.5 (2)H21B—C21—H21C109.5
C14—O4—Fe1129.2 (2)O5—C22—C23123.7 (3)
C22—O5—Fe1126.2 (2)O5—C22—C21115.3 (3)
C24—O6—Fe1123.4 (2)C23—C22—C21120.9 (3)
C9—N1—C8116.9 (3)C24—C23—C22122.5 (3)
C18—N2—C19117.2 (3)C24—C23—C26118.5 (3)
C18—N2—Cd1115.7 (2)C22—C23—C26119.0 (3)
C19—N2—Cd1125.6 (2)O6—C24—C23124.8 (3)
C29—N3—C28117.5 (3)O6—C24—C25114.7 (3)
C29—N3—Cd1iv122.3 (2)C23—C24—C25120.5 (3)
C28—N3—Cd1iv119.9 (3)C24—C25—H25A109.5
C2—C1—H1A109.5C24—C25—H25B109.5
C2—C1—H1B109.5H25A—C25—H25B109.5
H1A—C1—H1B109.5C24—C25—H25C109.5
C2—C1—H1C109.5H25A—C25—H25C109.5
H1A—C1—H1C109.5H25B—C25—H25C109.5
H1B—C1—H1C109.5C30—C26—C27116.7 (4)
O1—C2—C3124.3 (4)C30—C26—C23121.2 (3)
O1—C2—C1115.3 (3)C27—C26—C23122.1 (3)
C3—C2—C1120.4 (3)C28—C27—C26120.0 (4)
C2—C3—C4122.4 (3)C28—C27—H27120.0
C2—C3—C6119.3 (3)C26—C27—H27120.0
C4—C3—C6118.3 (3)N3—C28—C27122.9 (4)
O2—C4—C3124.1 (3)N3—C28—H28118.5
O2—C4—C5115.0 (3)C27—C28—H28118.5
C3—C4—C5120.8 (3)N3—C29—C30123.1 (4)
C4—C5—H5A109.5N3—C29—H29118.4
C4—C5—H5B109.5C30—C29—H29118.4
H5A—C5—H5B109.5C29—C30—C26119.6 (4)
C4—C5—H5C109.5C29—C30—H30120.2
H5A—C5—H5C109.5C26—C30—H30120.2
H5B—C5—H5C109.5H7D—O7—H7E102.0
C7—C6—C10116.8 (3)H8D—O8—H8E121.9
C7—C6—C3122.0 (3)H9D—O9—H9E131.6
C10—C6—C3121.2 (3)O10—C31—H31A109.5
C8—C7—C6119.3 (4)O10—C31—H31B109.5
C8—C7—H7120.4H31A—C31—H31B109.5
C6—C7—H7120.4O10—C31—H31C109.5
N1—C8—C7123.8 (4)H31A—C31—H31C109.5
N1—C8—H8118.1H31B—C31—H31C109.5
C7—C8—H8118.1C31—O10—H10D106.0
N1—C9—C10123.2 (4)C32—O11—H11D90.8
N1—C9—H9118.4O11—C32—H32A109.5
C10—C9—H9118.4O11—C32—H32B109.5
C9—C10—C6120.1 (4)H32A—C32—H32B109.5
C9—C10—H10120.0O11—C32—H32C109.5
C6—C10—H10120.0H32A—C32—H32C109.5
C12—C11—H11A109.5H32B—C32—H32C109.5
C12—C11—H11B109.5C33—O12—H12D115.7
H11A—C11—H11B109.5O12—C33—H33A109.5
C12—C11—H11C109.5O12—C33—H33B109.5
H11A—C11—H11C109.5H33A—C33—H33B109.5
H11B—C11—H11C109.5O12—C33—H33C109.5
O3—C12—C13123.6 (3)H33A—C33—H33C109.5
O3—C12—C11115.5 (3)H33B—C33—H33C109.5
C13—C12—C11120.9 (3)
Fe1—O1—C2—C36.1 (5)C12—C13—C16—C20107.6 (4)
Fe1—O1—C2—C1173.3 (3)C14—C13—C16—C2079.2 (5)
O1—C2—C3—C41.4 (6)C20—C16—C17—C180.2 (5)
C1—C2—C3—C4177.9 (4)C13—C16—C17—C18178.1 (3)
O1—C2—C3—C6179.1 (3)C19—N2—C18—C172.4 (5)
C1—C2—C3—C61.6 (5)Cd1—N2—C18—C17164.3 (3)
Fe1—O2—C4—C37.9 (5)C16—C17—C18—N22.1 (6)
Fe1—O2—C4—C5171.6 (2)C18—N2—C19—C200.9 (6)
C2—C3—C4—O22.4 (6)Cd1—N2—C19—C20164.3 (3)
C6—C3—C4—O2178.1 (3)N2—C19—C20—C160.9 (6)
C2—C3—C4—C5177.1 (3)C17—C16—C20—C191.2 (5)
C6—C3—C4—C52.4 (5)C13—C16—C20—C19176.7 (3)
C2—C3—C6—C777.8 (5)Fe1—O5—C22—C2316.6 (5)
C4—C3—C6—C7101.7 (4)Fe1—O5—C22—C21161.9 (3)
C2—C3—C6—C10103.7 (4)O5—C22—C23—C247.2 (6)
C4—C3—C6—C1076.8 (5)C21—C22—C23—C24174.4 (4)
C10—C6—C7—C80.0 (6)O5—C22—C23—C26173.7 (3)
C3—C6—C7—C8178.6 (4)C21—C22—C23—C264.8 (6)
C9—N1—C8—C70.4 (6)Fe1—O6—C24—C2330.7 (5)
C6—C7—C8—N10.2 (7)Fe1—O6—C24—C25148.1 (3)
C8—N1—C9—C100.5 (6)C22—C23—C24—O60.6 (6)
N1—C9—C10—C60.3 (7)C26—C23—C24—O6178.6 (3)
C7—C6—C10—C90.1 (6)C22—C23—C24—C25178.2 (4)
C3—C6—C10—C9178.5 (4)C26—C23—C24—C252.6 (5)
Fe1—O3—C12—C1324.3 (5)C24—C23—C26—C3093.1 (5)
Fe1—O3—C12—C11155.5 (2)C22—C23—C26—C3087.7 (5)
O3—C12—C13—C141.8 (6)C24—C23—C26—C2786.7 (5)
C11—C12—C13—C14178.4 (4)C22—C23—C26—C2792.5 (5)
O3—C12—C13—C16174.8 (3)C30—C26—C27—C284.1 (6)
C11—C12—C13—C165.4 (5)C23—C26—C27—C28175.7 (4)
Fe1—O4—C14—C1311.4 (6)C29—N3—C28—C272.9 (6)
Fe1—O4—C14—C15170.8 (3)Cd1iv—N3—C28—C27169.9 (3)
C12—C13—C14—O48.7 (6)C26—C27—C28—N30.9 (7)
C16—C13—C14—O4178.3 (4)C28—N3—C29—C303.5 (6)
C12—C13—C14—C15169.1 (4)Cd1iv—N3—C29—C30169.2 (3)
C16—C13—C14—C154.0 (6)N3—C29—C30—C260.2 (6)
C12—C13—C16—C1774.5 (5)C27—C26—C30—C293.6 (6)
C14—C13—C16—C1798.7 (4)C23—C26—C30—C29176.2 (4)
Symmetry codes: (i) x+1, y+2, z; (ii) x+1, y+1, z; (iii) x, y+1, z; (iv) x, y1, z.
(5) top
Crystal data top
C60H60Br2CdFe2N6O12·0.24(C2H8O2)·4.75(CH4O)·6(H2O)Z = 1
Mr = 1716.66F(000) = 882.1
Triclinic, P1Dx = 1.385 Mg m3
a = 12.2603 (15) ÅMo Kα radiation, λ = 0.71073 Å
b = 13.3560 (16) ÅCell parameters from 4766 reflections
c = 13.9326 (16) Åθ = 2.3–24.8°
α = 92.055 (2)°µ = 1.64 mm1
β = 109.196 (2)°T = 100 K
γ = 105.345 (2)°Plate, red
V = 2058.8 (4) Å30.36 × 0.10 × 0.03 mm
Data collection top
CCD area detector
diffractometer
6555 reflections with I > 2σ(I)
Radiation source: Incoatec microsourceRint = 0.052
ω scansθmax = 26.5°, θmin = 2.1°
Absorption correction: multi-scan
SADABS
h = 1515
Tmin = 0.595, Tmax = 0.745k = 1616
24811 measured reflectionsl = 1717
8482 independent reflections
Refinement top
Refinement on F2Primary atom site location: heavy-atom method
Least-squares matrix: fullHydrogen site location: mixed
R[F2 > 2σ(F2)] = 0.054H-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 reflectionsΔρmax = 1.30 e Å3
441 parametersΔρmin = 1.05 e Å3
2 restraints
Crystal data top
C60H60Br2CdFe2N6O12·0.24(C2H8O2)·4.75(CH4O)·6(H2O)γ = 105.345 (2)°
Mr = 1716.66V = 2058.8 (4) Å3
Triclinic, P1Z = 1
a = 12.2603 (15) ÅMo Kα radiation
b = 13.3560 (16) ŵ = 1.64 mm1
c = 13.9326 (16) ÅT = 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 = 0.745Rint = 0.052
24811 measured reflections
Refinement top
R[F2 > 2σ(F2)] = 0.0542 restraints
wR(F2) = 0.157H-atom parameters constrained
S = 1.05Δρmax = 1.30 e Å3
8482 reflectionsΔρmin = 1.05 e Å3
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
xyzUiso*/UeqOcc. (<1)
Cd10.50001.00000.00000.02037 (14)
Fe10.04644 (6)0.39445 (5)0.25163 (5)0.01918 (17)
Br10.67335 (5)1.03674 (4)0.19520 (4)0.02738 (15)
O10.1281 (3)0.3808 (3)0.2063 (2)0.0226 (7)
O20.0395 (3)0.3827 (3)0.3904 (2)0.0228 (7)
O30.0586 (3)0.4140 (2)0.1132 (2)0.0216 (7)
O40.0972 (3)0.5497 (2)0.2766 (2)0.0250 (7)
O50.0059 (3)0.2404 (2)0.2101 (3)0.0246 (7)
O60.2181 (3)0.3927 (2)0.3015 (2)0.0231 (7)
N10.4387 (4)0.3016 (4)0.5023 (3)0.0393 (12)
N20.3981 (4)0.8397 (3)0.0426 (3)0.0230 (9)
N30.3790 (4)0.0749 (3)0.0639 (3)0.0252 (9)
C10.3317 (5)0.3468 (5)0.1891 (4)0.0339 (12)
H1A0.33570.37320.12370.051*
H1B0.36790.38520.22510.051*
H1C0.37610.27200.17620.051*
C20.2028 (4)0.3617 (4)0.2537 (4)0.0235 (10)
C30.1699 (4)0.3542 (3)0.3593 (3)0.0214 (10)
C40.0503 (4)0.3630 (4)0.4215 (4)0.0226 (10)
C50.0197 (5)0.3472 (4)0.5333 (4)0.0309 (12)
H5A0.06720.35670.56450.046*
H5B0.06440.27610.53840.046*
H5C0.04210.39840.56930.046*
C60.2645 (4)0.3348 (4)0.4075 (4)0.0258 (11)
C70.3468 (5)0.2372 (4)0.3954 (4)0.0334 (12)
H70.34510.17960.35430.040*
C80.4317 (5)0.2238 (5)0.4435 (4)0.0402 (15)
H80.48720.15620.43420.048*
C90.3592 (5)0.3950 (5)0.5148 (4)0.0397 (14)
H90.36230.45080.55710.048*
C100.2718 (5)0.4152 (4)0.4695 (4)0.0330 (12)
H100.21730.48350.48060.040*
C110.1567 (5)0.4653 (4)0.0050 (4)0.0241 (10)
H11A0.10390.39600.04080.036*
H11B0.24130.46570.01450.036*
H11C0.14230.51840.05040.036*
C120.1299 (4)0.4893 (3)0.0898 (3)0.0190 (9)
C130.1834 (4)0.5900 (4)0.1477 (3)0.0216 (10)
C140.1578 (4)0.6155 (4)0.2348 (4)0.0246 (10)
C150.2015 (6)0.7280 (4)0.2848 (4)0.0408 (15)
H15A0.18520.73130.34900.061*
H15B0.15920.76990.23840.061*
H15C0.28860.75570.29950.061*
C160.2583 (4)0.6752 (3)0.1095 (3)0.0225 (10)
C170.2049 (5)0.7267 (4)0.0313 (4)0.0250 (10)
H170.11950.70690.00060.030*
C180.2770 (4)0.8075 (4)0.0001 (4)0.0248 (10)
H180.23900.84170.05430.030*
C190.4494 (5)0.7889 (4)0.1176 (4)0.0270 (11)
H190.53490.81030.14840.032*
C200.3834 (5)0.7066 (4)0.1526 (4)0.0275 (11)
H200.42360.67220.20550.033*
C210.0026 (5)0.0846 (4)0.1239 (5)0.0399 (14)
H21A0.07150.05770.13940.060*
H21B0.05400.03860.14550.060*
H21C0.01830.08690.05000.060*
C220.0696 (5)0.1938 (4)0.1809 (4)0.0249 (10)
C230.1928 (4)0.2383 (4)0.1967 (4)0.0249 (10)
C240.2608 (4)0.3353 (4)0.2569 (3)0.0230 (10)
C250.3923 (5)0.3802 (4)0.2709 (4)0.0336 (12)
H25A0.39960.40120.20600.050*
H25B0.43420.32710.29180.050*
H25C0.42870.44150.32390.050*
C260.2552 (4)0.1785 (4)0.1502 (4)0.0246 (10)
C270.3129 (5)0.1106 (5)0.2015 (4)0.0358 (13)
H270.31080.09740.26760.043*
C280.3745 (5)0.0611 (5)0.1565 (4)0.0362 (13)
H280.41500.01540.19390.043*
C290.3162 (6)0.1363 (4)0.0121 (4)0.0378 (14)
H290.31330.14360.05620.045*
C300.2559 (6)0.1892 (5)0.0522 (4)0.0412 (15)
H300.21460.23320.01270.049*
O70.5522 (5)0.9407 (4)0.3744 (4)0.0661 (15)
H7D0.56880.88310.38380.099*
H7E0.58960.96470.33500.099*
O80.3369 (5)0.9792 (4)0.4121 (4)0.0744 (16)
H8D0.35750.99170.48000.112*
H8E0.38840.96910.38410.112*
O90.0948 (12)0.9314 (10)0.3331 (10)0.207 (5)*
H9D0.17180.95050.36070.310*
H9E0.04170.95770.34030.310*
C310.7117 (13)0.7387 (11)0.4633 (11)0.145 (5)*
H31A0.77420.77150.43530.218*
H31B0.70960.66540.46930.218*
H31C0.73020.77620.53110.218*
O100.5971 (4)0.7432 (4)0.3964 (4)0.0539 (12)*
H10D0.55130.72250.42860.081*
O110.071 (2)1.0021 (19)0.3528 (19)0.136 (10)*0.374 (14)
H11D0.13491.01290.31170.204*0.374 (14)
C320.041 (2)1.0978 (19)0.4101 (19)0.077 (7)*0.374 (14)
H32A0.07901.09050.46200.116*0.374 (14)
H32B0.06811.14780.36520.116*0.374 (14)
H32C0.04731.12350.44400.116*0.374 (14)
O120.0824 (10)0.7742 (9)0.1722 (9)0.168 (4)*
H12D0.03450.82900.21250.253*
C330.1788 (15)0.7116 (14)0.2044 (14)0.202 (8)*
H33A0.16240.64610.22470.304*
H33B0.25630.69570.14760.304*
H33C0.18240.75210.26280.304*
C340.502 (3)0.491 (2)0.021 (2)0.051 (8)*0.240 (11)
H34A0.56090.54960.02980.076*0.240 (11)
H34B0.45260.51850.07860.076*0.240 (11)
H34C0.54490.45000.04650.076*0.240 (11)
O130.428 (3)0.428 (3)0.023 (3)0.140 (15)*0.240 (11)
H13D0.46780.41640.08170.168*0.240 (11)
Atomic displacement parameters (Å2) top
U11U22U33U12U13U23
Cd10.0238 (3)0.0150 (2)0.0258 (3)0.00228 (18)0.0163 (2)0.00085 (18)
Fe10.0224 (3)0.0185 (3)0.0188 (3)0.0028 (3)0.0128 (3)0.0008 (2)
Br10.0300 (3)0.0234 (3)0.0248 (3)0.0009 (2)0.0106 (2)0.00190 (19)
O10.0259 (17)0.0261 (17)0.0202 (16)0.0075 (14)0.0139 (14)0.0032 (13)
O20.0218 (17)0.0261 (17)0.0229 (17)0.0034 (14)0.0140 (14)0.0006 (13)
O30.0231 (17)0.0189 (16)0.0201 (16)0.0000 (13)0.0097 (14)0.0038 (13)
O40.0362 (19)0.0187 (16)0.0243 (17)0.0023 (14)0.0210 (15)0.0011 (13)
O50.0282 (18)0.0202 (16)0.0297 (18)0.0041 (14)0.0185 (15)0.0004 (14)
O60.0255 (17)0.0230 (17)0.0199 (16)0.0046 (14)0.0096 (14)0.0052 (13)
N10.026 (2)0.057 (3)0.029 (2)0.003 (2)0.017 (2)0.012 (2)
N20.024 (2)0.019 (2)0.024 (2)0.0002 (16)0.0116 (17)0.0027 (16)
N30.028 (2)0.026 (2)0.027 (2)0.0107 (18)0.0161 (18)0.0014 (17)
C10.023 (3)0.051 (3)0.027 (3)0.010 (2)0.011 (2)0.000 (2)
C20.026 (2)0.018 (2)0.028 (3)0.0036 (19)0.014 (2)0.0029 (19)
C30.026 (2)0.018 (2)0.021 (2)0.0015 (19)0.013 (2)0.0040 (18)
C40.030 (3)0.018 (2)0.022 (2)0.0014 (19)0.017 (2)0.0022 (18)
C50.033 (3)0.042 (3)0.022 (2)0.009 (2)0.016 (2)0.002 (2)
C60.022 (2)0.030 (3)0.023 (2)0.000 (2)0.011 (2)0.004 (2)
C70.035 (3)0.033 (3)0.031 (3)0.002 (2)0.020 (2)0.009 (2)
C80.031 (3)0.046 (3)0.031 (3)0.013 (3)0.014 (2)0.006 (2)
C90.030 (3)0.055 (4)0.031 (3)0.001 (3)0.017 (2)0.015 (3)
C100.027 (3)0.039 (3)0.029 (3)0.001 (2)0.015 (2)0.012 (2)
C110.031 (3)0.020 (2)0.021 (2)0.003 (2)0.014 (2)0.0019 (18)
C120.020 (2)0.019 (2)0.019 (2)0.0033 (18)0.0103 (19)0.0018 (17)
C130.022 (2)0.022 (2)0.019 (2)0.0018 (19)0.0112 (19)0.0015 (18)
C140.030 (3)0.019 (2)0.024 (2)0.000 (2)0.014 (2)0.0031 (19)
C150.066 (4)0.023 (3)0.031 (3)0.004 (3)0.028 (3)0.007 (2)
C160.026 (3)0.017 (2)0.022 (2)0.0015 (19)0.012 (2)0.0043 (18)
C170.025 (2)0.022 (2)0.025 (2)0.000 (2)0.011 (2)0.0027 (19)
C180.028 (3)0.024 (2)0.021 (2)0.002 (2)0.011 (2)0.0015 (19)
C190.026 (3)0.023 (2)0.030 (3)0.001 (2)0.013 (2)0.003 (2)
C200.026 (3)0.027 (3)0.024 (3)0.002 (2)0.007 (2)0.004 (2)
C210.039 (3)0.026 (3)0.053 (4)0.005 (2)0.018 (3)0.011 (3)
C220.031 (3)0.022 (2)0.025 (2)0.008 (2)0.015 (2)0.0010 (19)
C230.030 (3)0.028 (3)0.025 (2)0.011 (2)0.018 (2)0.004 (2)
C240.027 (3)0.027 (2)0.018 (2)0.008 (2)0.012 (2)0.0037 (19)
C250.023 (3)0.038 (3)0.039 (3)0.007 (2)0.013 (2)0.002 (2)
C260.028 (3)0.024 (2)0.027 (2)0.009 (2)0.016 (2)0.0008 (19)
C270.045 (3)0.053 (4)0.030 (3)0.032 (3)0.025 (3)0.014 (3)
C280.046 (3)0.048 (3)0.034 (3)0.030 (3)0.024 (3)0.015 (3)
C290.063 (4)0.043 (3)0.028 (3)0.030 (3)0.030 (3)0.012 (2)
C300.073 (4)0.040 (3)0.037 (3)0.039 (3)0.035 (3)0.017 (3)
O70.113 (4)0.040 (3)0.054 (3)0.009 (3)0.052 (3)0.006 (2)
O80.102 (4)0.065 (3)0.043 (3)0.003 (3)0.026 (3)0.002 (2)
Geometric parameters (Å, º) top
Cd1—N3i2.363 (4)C15—H15C0.9800
Cd1—N3ii2.363 (4)C16—C171.382 (7)
Cd1—N22.379 (4)C16—C201.388 (7)
Cd1—N2iii2.379 (4)C17—C181.386 (6)
Cd1—Br12.7759 (6)C17—H170.9500
Cd1—Br1iii2.7759 (6)C18—H180.9500
Fe1—O21.973 (3)C19—C201.388 (6)
Fe1—O11.977 (3)C19—H190.9500
Fe1—O41.982 (3)C20—H200.9500
Fe1—O61.994 (3)C21—C221.512 (7)
Fe1—O52.000 (3)C21—H21A0.9800
Fe1—O32.005 (3)C21—H21B0.9800
O1—C21.275 (5)C21—H21C0.9800
O2—C41.280 (5)C22—C231.407 (7)
O3—C121.275 (5)C23—C241.402 (7)
O4—C141.281 (5)C23—C261.503 (6)
O5—C221.269 (6)C24—C251.507 (7)
O6—C241.280 (6)C25—H25A0.9800
N1—C91.329 (7)C25—H25B0.9800
N1—C81.338 (7)C25—H25C0.9800
N2—C191.339 (6)C26—C271.374 (7)
N2—C181.344 (6)C26—C301.379 (7)
N3—C281.328 (6)C27—C281.395 (7)
N3—C291.341 (7)C27—H270.9500
N3—Cd1iv2.363 (4)C28—H280.9500
C1—C21.494 (7)C29—C301.371 (7)
C1—H1A0.9800C29—H290.9500
C1—H1B0.9800C30—H300.9500
C1—H1C0.9800O7—H7D0.8501
C2—C31.407 (7)O7—H7E0.8447
C3—C41.407 (7)O8—H8D0.8926
C3—C61.493 (6)O8—H8E0.8787
C4—C51.514 (6)O9—H9D0.8545
C5—H5A0.9800O9—H9E0.8478
C5—H5B0.9800C31—O101.426 (14)
C5—H5C0.9800C31—H31A0.9800
C6—C71.386 (7)C31—H31B0.9800
C6—C101.393 (7)C31—H31C0.9800
C7—C81.391 (7)O10—H10D0.8272
C7—H70.9500O11—C321.37 (3)
C8—H80.9500O11—H11D0.8530
C9—C101.387 (7)C32—H32A0.9800
C9—H90.9500C32—H32B0.9800
C10—H100.9500C32—H32C0.9800
C11—C121.506 (6)O12—C331.467 (9)
C11—H11A0.9800O12—H12D0.8492
C11—H11B0.9800C33—H33A0.9800
C11—H11C0.9800C33—H33B0.9800
C12—C131.413 (6)C33—H33C0.9800
C13—C141.402 (6)C34—O131.387 (19)
C13—C161.494 (6)C34—H34A0.9800
C14—C151.511 (7)C34—H34B0.9800
C15—H15A0.9800C34—H34C0.9800
C15—H15B0.9800O13—H13D0.8400
N3i—Cd1—N3ii180.00 (17)O4—C14—C13124.7 (4)
N3i—Cd1—N294.41 (14)O4—C14—C15115.6 (4)
N3ii—Cd1—N285.59 (14)C13—C14—C15119.7 (4)
N3i—Cd1—N2iii85.59 (14)C14—C15—H15A109.5
N3ii—Cd1—N2iii94.41 (14)C14—C15—H15B109.5
N2—Cd1—N2iii180.0H15A—C15—H15B109.5
N3i—Cd1—Br189.82 (10)C14—C15—H15C109.5
N3ii—Cd1—Br190.18 (10)H15A—C15—H15C109.5
N2—Cd1—Br188.49 (10)H15B—C15—H15C109.5
N2iii—Cd1—Br191.51 (10)C17—C16—C20117.8 (4)
N3i—Cd1—Br1iii90.18 (10)C17—C16—C13121.0 (4)
N3ii—Cd1—Br1iii89.82 (10)C20—C16—C13121.2 (4)
N2—Cd1—Br1iii91.51 (10)C16—C17—C18119.4 (5)
N2iii—Cd1—Br1iii88.49 (10)C16—C17—H17120.3
Br1—Cd1—Br1iii180.0C18—C17—H17120.3
O2—Fe1—O186.34 (13)N2—C18—C17123.1 (5)
O2—Fe1—O492.35 (13)N2—C18—H18118.5
O1—Fe1—O494.42 (14)C17—C18—H18118.5
O2—Fe1—O690.85 (13)N2—C19—C20123.1 (5)
O1—Fe1—O6173.82 (14)N2—C19—H19118.4
O4—Fe1—O691.20 (14)C20—C19—H19118.4
O2—Fe1—O595.54 (13)C19—C20—C16119.3 (5)
O1—Fe1—O589.22 (14)C19—C20—H20120.4
O4—Fe1—O5171.51 (13)C16—C20—H20120.4
O6—Fe1—O585.56 (13)C22—C21—H21A109.5
O2—Fe1—O3177.07 (13)C22—C21—H21B109.5
O1—Fe1—O394.74 (13)H21A—C21—H21B109.5
O4—Fe1—O384.86 (13)C22—C21—H21C109.5
O6—Fe1—O388.33 (13)H21A—C21—H21C109.5
O5—Fe1—O387.20 (13)H21B—C21—H21C109.5
C2—O1—Fe1131.6 (3)O5—C22—C23124.2 (4)
C4—O2—Fe1130.9 (3)O5—C22—C21115.0 (4)
C12—O3—Fe1127.7 (3)C23—C22—C21120.8 (4)
C14—O4—Fe1129.0 (3)C24—C23—C22122.6 (4)
C22—O5—Fe1126.5 (3)C24—C23—C26118.5 (4)
C24—O6—Fe1124.6 (3)C22—C23—C26119.0 (4)
C9—N1—C8117.2 (4)O6—C24—C23124.2 (4)
C19—N2—C18117.2 (4)O6—C24—C25115.2 (4)
C19—N2—Cd1124.8 (3)C23—C24—C25120.6 (4)
C18—N2—Cd1116.9 (3)C24—C25—H25A109.5
C28—N3—C29116.5 (4)C24—C25—H25B109.5
C28—N3—Cd1iv120.5 (3)H25A—C25—H25B109.5
C29—N3—Cd1iv122.9 (3)C24—C25—H25C109.5
C2—C1—H1A109.5H25A—C25—H25C109.5
C2—C1—H1B109.5H25B—C25—H25C109.5
H1A—C1—H1B109.5C27—C26—C30116.9 (5)
C2—C1—H1C109.5C27—C26—C23122.3 (4)
H1A—C1—H1C109.5C30—C26—C23120.7 (5)
H1B—C1—H1C109.5C26—C27—C28119.9 (5)
O1—C2—C3123.9 (4)C26—C27—H27120.1
O1—C2—C1115.4 (4)C28—C27—H27120.1
C3—C2—C1120.6 (4)N3—C28—C27122.9 (5)
C2—C3—C4122.2 (4)N3—C28—H28118.5
C2—C3—C6119.4 (4)C27—C28—H28118.5
C4—C3—C6118.4 (4)N3—C29—C30123.6 (5)
O2—C4—C3124.6 (4)N3—C29—H29118.2
O2—C4—C5114.7 (4)C30—C29—H29118.2
C3—C4—C5120.7 (4)C29—C30—C26119.9 (5)
C4—C5—H5A109.5C29—C30—H30120.0
C4—C5—H5B109.5C26—C30—H30120.0
H5A—C5—H5B109.5H7D—O7—H7E101.9
C4—C5—H5C109.5H8D—O8—H8E121.4
H5A—C5—H5C109.5H9D—O9—H9E132.0
H5B—C5—H5C109.5O10—C31—H31A109.5
C7—C6—C10116.8 (4)O10—C31—H31B109.5
C7—C6—C3122.5 (4)H31A—C31—H31B109.5
C10—C6—C3120.7 (4)O10—C31—H31C109.5
C6—C7—C8119.8 (5)H31A—C31—H31C109.5
C6—C7—H7120.1H31B—C31—H31C109.5
C8—C7—H7120.1C31—O10—H10D104.0
N1—C8—C7123.0 (5)C32—O11—H11D91.0
N1—C8—H8118.5O11—C32—H32A109.5
C7—C8—H8118.5O11—C32—H32B109.5
N1—C9—C10123.4 (5)H32A—C32—H32B109.5
N1—C9—H9118.3O11—C32—H32C109.5
C10—C9—H9118.3H32A—C32—H32C109.5
C9—C10—C6119.6 (5)H32B—C32—H32C109.5
C9—C10—H10120.2C33—O12—H12D116.6
C6—C10—H10120.2O12—C33—H33A110.1
C12—C11—H11A109.5O12—C33—H33B109.5
C12—C11—H11B109.5H33A—C33—H33B109.5
H11A—C11—H11B109.5O12—C33—H33C108.8
C12—C11—H11C109.5H33A—C33—H33C109.5
H11A—C11—H11C109.5H33B—C33—H33C109.5
H11B—C11—H11C109.5O13—C34—H34A109.5
O3—C12—C13123.8 (4)O13—C34—H34B109.5
O3—C12—C11115.9 (4)H34A—C34—H34B109.5
C13—C12—C11120.2 (4)O13—C34—H34C109.5
C14—C13—C12121.5 (4)H34A—C34—H34C109.5
C14—C13—C16118.5 (4)H34B—C34—H34C109.5
C12—C13—C16119.6 (4)C34—O13—H13D112.1
Symmetry codes: (i) x+1, y+1, z; (ii) x, y+1, z; (iii) x+1, y+2, z; (iv) x, y1, z.
(6_squeeze) top
Crystal data top
C64.09H68.18Cd3Cl8.18Fe2I6N6O12F(000) = 4975
Mr = 2614.57Dx = 1.726 Mg m3
Monoclinic, C2/cMo Kα radiation, λ = 0.71073 Å
a = 32.186 (3) ÅCell parameters from 3756 reflections
b = 13.7863 (15) Åθ = 2.4–19.7°
c = 27.721 (2) ŵ = 3.01 mm1
β = 125.118 (8)°T = 100 K
V = 10061.4 (18) Å3Block, red
Z = 40.15 × 0.08 × 0.07 mm
Data collection top
CCD area detector
diffractometer
3817 reflections with I > 2σ(I)
Radiation source: Incoatec microsourceRint = 0.085
ω scansθmax = 22.0°, θmin = 1.8°
Absorption correction: multi-scan
SADABS
h = 3333
Tmin = 0.587, Tmax = 0.745k = 1414
41442 measured reflectionsl = 2929
6166 independent reflections
Refinement top
Refinement on F2Primary atom site location: heavy-atom method
Least-squares matrix: fullHydrogen site location: inferred from neighbouring sites
R[F2 > 2σ(F2)] = 0.066H-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 reflectionsΔρmax = 2.31 e Å3
259 parametersΔρmin = 1.52 e Å3
2 restraints
Crystal data top
C64.09H68.18Cd3Cl8.18Fe2I6N6O12V = 10061.4 (18) Å3
Mr = 2614.57Z = 4
Monoclinic, C2/cMo Kα radiation
a = 32.186 (3) ŵ = 3.01 mm1
b = 13.7863 (15) ÅT = 100 K
c = 27.721 (2) Å0.15 × 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 = 0.745Rint = 0.085
41442 measured reflectionsθmax = 22.0°
Refinement top
R[F2 > 2σ(F2)] = 0.0662 restraints
wR(F2) = 0.163H-atom parameters constrained
S = 0.95Δρmax = 2.31 e Å3
6166 reflectionsΔρmin = 1.52 e Å3
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
xyzUiso*/UeqOcc. (<1)
I10.81336 (5)0.16305 (8)0.18575 (6)0.0648 (4)
I20.89618 (5)0.36766 (9)0.11898 (5)0.0548 (4)
I30.41195 (4)0.19416 (8)0.16986 (5)0.0445 (3)
Cd10.85709 (4)0.32463 (8)0.18033 (5)0.0348 (3)
Cd20.50000.28300 (11)0.25000.0322 (5)
Fe10.56602 (8)0.74825 (14)0.02682 (9)0.0270 (6)
O10.6075 (3)0.7195 (7)0.0035 (4)0.031 (3)*
O20.6323 (4)0.7596 (7)0.1046 (4)0.038 (3)*
O30.5634 (3)0.6034 (6)0.0322 (4)0.026 (2)*
O40.5302 (3)0.7505 (7)0.0658 (4)0.033 (3)*
O50.5019 (3)0.7476 (7)0.0543 (4)0.029 (3)*
O60.5645 (3)0.8919 (6)0.0185 (4)0.023 (2)*
N10.7969 (4)0.4404 (9)0.1542 (5)0.032 (3)*
N20.5136 (4)0.3896 (8)0.1977 (5)0.026 (3)*
N30.4110 (4)1.1032 (8)0.2309 (5)0.025 (3)*
C10.6574 (6)0.6183 (11)0.0164 (7)0.046 (5)*
H1A0.64170.55400.02650.069*
H1B0.69420.61150.00400.069*
H1C0.64340.65630.05250.069*
C20.6468 (5)0.6686 (10)0.0226 (6)0.029 (4)*
C30.6779 (5)0.6536 (10)0.0825 (6)0.032 (4)*
C40.6705 (6)0.7022 (12)0.1205 (7)0.047 (5)*
C50.7092 (7)0.7025 (15)0.1872 (9)0.092 (7)*
H5A0.71730.76960.20140.138*
H5B0.74020.66950.19740.138*
H5C0.69500.66880.20580.138*
C60.7216 (6)0.5837 (11)0.1097 (6)0.032 (4)*
C70.7649 (6)0.5994 (13)0.1169 (7)0.048 (5)*
H70.77060.66150.10680.057*
C80.8029 (6)0.5309 (12)0.1383 (7)0.052 (5)*
H80.83340.54650.14210.062*
C90.7541 (6)0.4264 (12)0.1487 (6)0.040 (4)*
H90.74940.36570.16120.048*
C100.7163 (6)0.4918 (11)0.1266 (6)0.041 (4)*
H100.68570.47530.12250.049*
C110.5706 (5)0.4464 (9)0.0694 (6)0.030 (4)*
H11A0.54140.40510.05780.045*
H11B0.59870.43160.11020.045*
H11C0.58120.43410.04320.045*
C120.5558 (5)0.5515 (10)0.0650 (6)0.021 (3)*
C130.5381 (5)0.5882 (10)0.0968 (6)0.023 (4)*
C140.5234 (5)0.6850 (11)0.0944 (6)0.030 (4)*
C150.5009 (5)0.7201 (11)0.1239 (7)0.041 (4)*
H15A0.48980.78740.11220.061*
H15B0.52610.71710.16670.061*
H15C0.47160.67960.11270.061*
C160.5300 (5)0.5187 (10)0.1320 (6)0.024 (4)*
C170.4871 (5)0.4617 (10)0.1059 (6)0.026 (4)*
H170.46150.46650.06480.032*
C180.4814 (6)0.3969 (11)0.1405 (7)0.038 (4)*
H180.45250.35560.12130.046*
C190.5536 (6)0.4429 (11)0.2214 (7)0.037 (4)*
H190.57820.43570.26260.045*
C200.5642 (6)0.5101 (11)0.1924 (7)0.039 (4)*
H200.59400.54890.21360.046*
C210.4340 (5)0.7873 (11)0.1507 (6)0.037 (4)*
H21A0.42900.71710.15090.056*
H21B0.43850.80390.18180.056*
H21C0.40430.82140.15770.056*
C220.4796 (5)0.8164 (11)0.0929 (6)0.030 (4)*
C230.4961 (5)0.9139 (10)0.0820 (6)0.021 (4)*
C240.5364 (5)0.9470 (10)0.0274 (6)0.022 (4)*
C250.5533 (5)1.0513 (10)0.0162 (6)0.033 (4)*
H25A0.57701.06220.02640.050*
H25B0.52371.09370.03210.050*
H25C0.57031.06590.03550.050*
C260.4676 (5)0.9843 (10)0.1325 (6)0.026 (4)*
C270.4303 (5)1.0422 (10)0.1394 (6)0.034 (4)*
H270.42261.04110.11100.041*
C280.4035 (6)1.1029 (11)0.1881 (6)0.035 (4)*
H280.37891.14580.19120.042*
C290.4488 (5)1.0488 (10)0.2232 (6)0.032 (4)*
H290.45621.05150.25180.039*
C300.4777 (5)0.9886 (11)0.1746 (6)0.033 (4)*
H300.50430.95060.17030.040*
Cl10.6931 (3)0.0075 (7)0.0560 (4)0.121 (3)0.7735
Cl20.7184 (3)0.1501 (5)0.0114 (3)0.082 (2)0.7735
C310.6737 (8)0.0766 (15)0.0090 (9)0.053 (7)*0.7735
H31A0.65270.04690.03070.063*0.7735
H31B0.65100.11880.01310.063*0.7735
Cl30.7165 (3)0.3660 (6)0.0005 (3)0.097 (3)*0.7703
Cl40.6454 (3)0.2964 (6)0.0262 (4)0.110 (3)*0.7703
C320.6954 (9)0.2687 (19)0.0213 (12)0.083 (9)*0.7703
H32A0.68470.21560.00760.100*0.7703
H32B0.72420.24450.06010.100*0.7703
Cl50.6784 (7)0.3269 (15)0.3041 (9)0.196 (8)*0.5
Cl60.7041 (6)0.4057 (13)0.2401 (8)0.166 (7)*0.5
C330.7268 (12)0.403 (3)0.3133 (11)0.079 (13)*0.5
H33A0.72690.46820.32870.095*0.5
H33B0.76100.37360.33840.095*0.5
Atomic displacement parameters (Å2) top
U11U22U33U12U13U23
I10.0710 (10)0.0301 (7)0.0745 (10)0.0025 (7)0.0310 (8)0.0104 (7)
I20.0718 (9)0.0591 (9)0.0536 (8)0.0092 (7)0.0476 (8)0.0165 (7)
I30.0653 (8)0.0276 (7)0.0477 (8)0.0121 (6)0.0365 (7)0.0022 (5)
Cd10.0420 (8)0.0295 (7)0.0310 (7)0.0009 (6)0.0199 (7)0.0040 (6)
Cd20.0611 (12)0.0170 (9)0.0348 (10)0.0000.0369 (10)0.000
Fe10.0444 (15)0.0116 (12)0.0329 (14)0.0042 (11)0.0268 (12)0.0053 (10)
Cl10.102 (7)0.118 (8)0.111 (7)0.011 (6)0.042 (6)0.035 (6)
Cl20.090 (5)0.078 (5)0.109 (6)0.001 (4)0.076 (5)0.012 (4)
Geometric parameters (Å, º) top
I1—Cd12.6850 (17)C11—H11B0.9800
I2—Cd12.6997 (16)C11—H11C0.9800
I3—Cd22.6876 (13)C12—C131.392 (17)
Cd1—N3i2.268 (11)C13—C141.404 (18)
Cd1—N12.282 (12)C13—C161.492 (18)
Cd2—N2ii2.276 (11)C14—C151.453 (18)
Cd2—N22.276 (11)C15—H15A0.9800
Cd2—I3ii2.6876 (13)C15—H15B0.9800
Fe1—O41.982 (9)C15—H15C0.9800
Fe1—O21.982 (10)C16—C171.380 (17)
Fe1—O11.984 (9)C16—C201.383 (18)
Fe1—O61.991 (9)C17—C181.395 (18)
Fe1—O51.994 (9)C17—H170.9500
Fe1—O32.008 (9)C18—H180.9500
O1—C21.251 (15)C19—C201.391 (19)
O2—C41.308 (17)C19—H190.9500
O3—C121.287 (14)C20—H200.9500
O4—C141.301 (16)C21—C221.475 (18)
O5—C221.295 (15)C21—H21A0.9800
O6—C241.300 (14)C21—H21B0.9800
N1—C91.311 (17)C21—H21C0.9800
N1—C81.373 (18)C22—C231.412 (18)
N2—C191.286 (16)C23—C241.386 (17)
N2—C181.309 (17)C23—C261.505 (18)
N3—C291.338 (16)C24—C251.506 (18)
N3—C281.341 (16)C25—H25A0.9800
N3—Cd1iii2.268 (11)C25—H25B0.9800
C1—C21.480 (19)C25—H25C0.9800
C1—H1A0.9800C26—C271.361 (18)
C1—H1B0.9800C26—C301.383 (18)
C1—H1C0.9800C27—C281.390 (19)
C2—C31.373 (19)C27—H270.9500
C3—C41.38 (2)C28—H280.9500
C3—C61.504 (19)C29—C301.388 (18)
C4—C51.52 (2)C29—H290.9500
C5—H5A0.9800C30—H300.9500
C5—H5B0.9800Cl1—C311.58 (2)
C5—H5C0.9800Cl2—C311.73 (2)
C6—C71.307 (19)C31—H31A0.9900
C6—C101.396 (19)C31—H31B0.9900
C7—C81.38 (2)Cl3—C321.75 (2)
C7—H70.9500Cl4—C321.73 (2)
C8—H80.9500C32—H32A0.9900
C9—C101.347 (19)C32—H32B0.9900
C9—H90.9500Cl5—C331.775 (18)
C10—H100.9500Cl6—C331.717 (18)
C11—C121.507 (17)C33—H33A0.9900
C11—H11A0.9800C33—H33B0.9900
N3i—Cd1—N191.0 (4)O3—C12—C13123.9 (12)
N3i—Cd1—I1113.7 (3)O3—C12—C11114.4 (12)
N1—Cd1—I1102.8 (3)C13—C12—C11121.6 (12)
N3i—Cd1—I2104.1 (3)C12—C13—C14124.5 (13)
N1—Cd1—I2105.3 (3)C12—C13—C16117.9 (12)
I1—Cd1—I2131.82 (6)C14—C13—C16117.5 (12)
N2ii—Cd2—N299.6 (6)O4—C14—C13121.2 (13)
N2ii—Cd2—I3108.8 (3)O4—C14—C15115.2 (13)
N2—Cd2—I3105.4 (3)C13—C14—C15123.6 (14)
N2ii—Cd2—I3ii105.4 (3)C14—C15—H15A109.5
N2—Cd2—I3ii108.8 (3)C14—C15—H15B109.5
I3—Cd2—I3ii125.78 (7)H15A—C15—H15B109.5
O4—Fe1—O290.3 (4)C14—C15—H15C109.5
O4—Fe1—O1167.9 (4)H15A—C15—H15C109.5
O2—Fe1—O184.9 (4)H15B—C15—H15C109.5
O4—Fe1—O693.7 (4)C17—C16—C20116.3 (14)
O2—Fe1—O689.2 (4)C17—C16—C13121.5 (12)
O1—Fe1—O697.3 (4)C20—C16—C13122.1 (13)
O4—Fe1—O593.8 (4)C16—C17—C18119.5 (14)
O2—Fe1—O5174.0 (4)C16—C17—H17120.2
O1—Fe1—O591.9 (4)C18—C17—H17120.2
O6—Fe1—O586.2 (4)N2—C18—C17123.8 (14)
O4—Fe1—O385.0 (4)N2—C18—H18118.1
O2—Fe1—O393.6 (4)C17—C18—H18118.1
O1—Fe1—O384.3 (4)N2—C19—C20126.3 (15)
O6—Fe1—O3176.8 (4)N2—C19—H19116.9
O5—Fe1—O391.1 (4)C20—C19—H19116.9
C2—O1—Fe1124.7 (9)C16—C20—C19117.9 (14)
C4—O2—Fe1122.2 (10)C16—C20—H20121.0
C12—O3—Fe1129.7 (8)C19—C20—H20121.0
C14—O4—Fe1132.5 (9)C22—C21—H21A109.5
C22—O5—Fe1130.6 (9)C22—C21—H21B109.5
C24—O6—Fe1130.6 (8)H21A—C21—H21B109.5
C9—N1—C8115.3 (14)C22—C21—H21C109.5
C9—N1—Cd1125.3 (11)H21A—C21—H21C109.5
C8—N1—Cd1119.2 (10)H21B—C21—H21C109.5
C19—N2—C18115.9 (14)O5—C22—C23123.9 (13)
C19—N2—Cd2123.2 (10)O5—C22—C21115.5 (13)
C18—N2—Cd2120.9 (10)C23—C22—C21120.6 (13)
C29—N3—C28117.9 (13)C24—C23—C22123.2 (13)
C29—N3—Cd1iii118.5 (9)C24—C23—C26119.4 (12)
C28—N3—Cd1iii123.1 (10)C22—C23—C26117.4 (12)
C2—C1—H1A109.5O6—C24—C23124.3 (12)
C2—C1—H1B109.5O6—C24—C25113.0 (12)
H1A—C1—H1B109.5C23—C24—C25122.7 (12)
C2—C1—H1C109.5C24—C25—H25A109.5
H1A—C1—H1C109.5C24—C25—H25B109.5
H1B—C1—H1C109.5H25A—C25—H25B109.5
O1—C2—C3125.1 (14)C24—C25—H25C109.5
O1—C2—C1114.9 (13)H25A—C25—H25C109.5
C3—C2—C1119.9 (14)H25B—C25—H25C109.5
C2—C3—C4121.6 (14)C27—C26—C30118.3 (14)
C2—C3—C6121.6 (13)C27—C26—C23121.7 (13)
C4—C3—C6116.8 (14)C30—C26—C23120.0 (13)
O2—C4—C3125.3 (15)C26—C27—C28119.6 (15)
O2—C4—C5111.2 (15)C26—C27—H27120.2
C3—C4—C5123.3 (16)C28—C27—H27120.2
C4—C5—H5A109.5N3—C28—C27122.3 (15)
C4—C5—H5B109.5N3—C28—H28118.8
H5A—C5—H5B109.5C27—C28—H28118.8
C4—C5—H5C109.5N3—C29—C30122.0 (14)
H5A—C5—H5C109.5N3—C29—H29119.0
H5B—C5—H5C109.5C30—C29—H29119.0
C7—C6—C10115.2 (15)C26—C30—C29119.6 (14)
C7—C6—C3125.4 (15)C26—C30—H30120.2
C10—C6—C3119.3 (14)C29—C30—H30120.2
C6—C7—C8123.7 (17)Cl1—C31—Cl2118.2 (13)
C6—C7—H7118.2Cl1—C31—H31A107.8
C8—C7—H7118.2Cl2—C31—H31A107.8
N1—C8—C7120.5 (16)Cl1—C31—H31B107.8
N1—C8—H8119.7Cl2—C31—H31B107.8
C7—C8—H8119.7H31A—C31—H31B107.1
N1—C9—C10124.7 (16)Cl4—C32—Cl3114.4 (15)
N1—C9—H9117.6Cl4—C32—H32A108.7
C10—C9—H9117.6Cl3—C32—H32A108.7
C9—C10—C6120.4 (15)Cl4—C32—H32B108.7
C9—C10—H10119.8Cl3—C32—H32B108.7
C6—C10—H10119.8H32A—C32—H32B107.6
C12—C11—H11A109.5Cl6—C33—Cl595.7 (15)
C12—C11—H11B109.5Cl6—C33—H33A112.6
H11A—C11—H11B109.5Cl5—C33—H33A112.6
C12—C11—H11C109.5Cl6—C33—H33B112.6
H11A—C11—H11C109.5Cl5—C33—H33B112.6
H11B—C11—H11C109.5H33A—C33—H33B110.1
Symmetry codes: (i) x+1/2, y+3/2, z+1/2; (ii) x+1, y, z+1/2; (iii) x1/2, y+3/2, z1/2.
(6_without_squeeze) top
Crystal data top
C64.09H68.18Cd3Cl8.18Fe2I6N6O12F(000) = 4975
Mr = 2614.57Dx = 1.726 Mg m3
Monoclinic, C2/cMo Kα radiation, λ = 0.71073 Å
a = 32.186 (3) ÅCell parameters from 3756 reflections
b = 13.7863 (15) Åθ = 2.4–19.7°
c = 27.721 (2) ŵ = 3.01 mm1
β = 125.118 (8)°T = 100 K
V = 10061.4 (18) Å3Block, red
Z = 40.15 × 0.08 × 0.07 mm
Data collection top
CCD area detector
diffractometer
3835 reflections with I > 2σ(I)
Radiation source: Incoatec microsourceRint = 0.090
ω scansθmax = 22.0°, θmin = 1.8°
Absorption correction: multi-scan
SADABS
h = 3333
Tmin = 0.587, Tmax = 0.745k = 1414
41442 measured reflectionsl = 2929
6166 independent reflections
Refinement top
Refinement on F2Primary atom site location: heavy-atom method
Least-squares matrix: fullHydrogen site location: inferred from neighbouring sites
R[F2 > 2σ(F2)] = 0.073H-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 reflectionsΔρmax = 2.43 e Å3
259 parametersΔρmin = 1.56 e Å3
2 restraints
Crystal data top
C64.09H68.18Cd3Cl8.18Fe2I6N6O12V = 10061.4 (18) Å3
Mr = 2614.57Z = 4
Monoclinic, C2/cMo Kα radiation
a = 32.186 (3) ŵ = 3.01 mm1
b = 13.7863 (15) ÅT = 100 K
c = 27.721 (2) Å0.15 × 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 = 0.745Rint = 0.090
41442 measured reflectionsθmax = 22.0°
Refinement top
R[F2 > 2σ(F2)] = 0.0732 restraints
wR(F2) = 0.210H-atom parameters constrained
S = 1.00Δρmax = 2.43 e Å3
6166 reflectionsΔρmin = 1.56 e Å3
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
xyzUiso*/UeqOcc. (<1)
I10.81334 (6)0.16302 (10)0.18587 (7)0.0639 (5)
I20.89629 (6)0.36744 (11)0.11910 (6)0.0539 (5)
I30.41197 (5)0.19408 (9)0.16984 (6)0.0444 (4)
Cd10.85707 (5)0.32468 (10)0.18031 (6)0.0345 (4)
Cd20.50000.28294 (12)0.25000.0321 (5)
Fe10.56591 (9)0.74831 (16)0.02682 (11)0.0268 (6)
O10.6074 (4)0.7195 (8)0.0037 (5)0.032 (3)*
O20.6321 (4)0.7596 (8)0.1049 (5)0.036 (3)*
O30.5632 (4)0.6035 (7)0.0321 (4)0.025 (3)*
O40.5302 (4)0.7513 (8)0.0652 (5)0.033 (3)*
O50.5018 (4)0.7475 (8)0.0540 (5)0.029 (3)*
O60.5645 (4)0.8915 (7)0.0188 (4)0.023 (3)*
N10.7967 (5)0.4412 (10)0.1540 (6)0.034 (4)*
N20.5132 (5)0.3896 (9)0.1977 (6)0.026 (3)*
N30.4110 (5)1.1025 (10)0.2312 (6)0.028 (3)*
C10.6581 (7)0.6182 (14)0.0159 (8)0.049 (5)*
H1A0.64440.55210.02400.073*
H1B0.69490.61560.00390.073*
H1C0.64240.65390.05310.073*
C20.6468 (6)0.6684 (12)0.0228 (7)0.031 (4)*
C30.6781 (6)0.6529 (12)0.0834 (7)0.031 (5)*
C40.6700 (7)0.7026 (14)0.1208 (9)0.047 (5)*
C50.7091 (9)0.7046 (18)0.1865 (10)0.089 (8)*
H5A0.71450.77170.20050.134*
H5B0.74110.67770.19580.134*
H5C0.69710.66580.20580.134*
C60.7209 (6)0.5833 (12)0.1096 (7)0.031 (4)*
C70.7651 (7)0.5989 (15)0.1165 (8)0.048 (5)*
H70.77040.66110.10610.058*
C80.8036 (8)0.5310 (15)0.1376 (8)0.054 (6)*
H80.83380.54590.14070.065*
C90.7539 (7)0.4282 (14)0.1484 (8)0.043 (5)*
H90.74930.36730.16070.052*
C100.7158 (7)0.4925 (13)0.1269 (8)0.041 (5)*
H100.68560.47590.12370.050*
C110.5703 (6)0.4461 (11)0.0698 (7)0.029 (4)*
H11A0.54040.40540.05560.044*
H11B0.59650.43060.11130.044*
H11C0.58350.43360.04620.044*
C120.5558 (6)0.5513 (11)0.0646 (7)0.020 (4)*
C130.5379 (6)0.5882 (11)0.0963 (7)0.024 (4)*
C140.5240 (6)0.6845 (12)0.0941 (7)0.030 (4)*
C150.5007 (7)0.7204 (13)0.1244 (8)0.042 (5)*
H15A0.48900.78740.11220.063*
H15B0.52600.71820.16720.063*
H15C0.47170.67920.11360.063*
C160.5294 (6)0.5184 (11)0.1316 (7)0.024 (4)*
C170.4873 (6)0.4616 (11)0.1058 (7)0.028 (4)*
H170.46200.46570.06460.034*
C180.4814 (7)0.3961 (13)0.1409 (8)0.039 (5)*
H180.45260.35470.12170.047*
C190.5527 (7)0.4429 (13)0.2220 (8)0.039 (5)*
H190.57690.43680.26340.047*
C200.5631 (7)0.5105 (13)0.1919 (8)0.040 (5)*
H200.59270.54980.21290.049*
C210.4335 (6)0.7867 (13)0.1503 (7)0.037 (5)*
H21A0.42670.71770.14910.056*
H21B0.43850.79770.18140.056*
H21C0.40450.82520.15830.056*
C220.4795 (6)0.8157 (12)0.0930 (7)0.030 (4)*
C230.4955 (6)0.9135 (11)0.0823 (7)0.023 (4)*
C240.5368 (6)0.9465 (12)0.0265 (7)0.024 (4)*
C250.5536 (6)1.0512 (12)0.0163 (7)0.034 (5)*
H25A0.57941.06190.02590.051*
H25B0.52431.09340.02970.051*
H25C0.56801.06630.03830.051*
C260.4669 (6)0.9835 (12)0.1326 (7)0.028 (4)*
C270.4295 (6)1.0413 (12)0.1392 (7)0.035 (5)*
H270.42151.03940.11110.042*
C280.4032 (6)1.1028 (13)0.1875 (7)0.035 (5)*
H280.37911.14660.19030.042*
C290.4486 (6)1.0483 (12)0.2241 (7)0.033 (5)*
H290.45571.05090.25290.039*
C300.4776 (7)0.9877 (13)0.1751 (7)0.037 (5)*
H300.50430.94980.17060.044*
Cl10.6933 (4)0.0074 (8)0.0561 (5)0.121 (4)0.7735
Cl20.7182 (3)0.1508 (6)0.0107 (4)0.079 (3)0.7735
C310.6732 (9)0.0769 (18)0.0081 (11)0.052 (7)*0.7735
H31A0.65250.04670.03140.063*0.7735
H31B0.65030.11890.01190.063*0.7735
Cl30.7167 (3)0.3657 (7)0.0003 (4)0.095 (3)*0.7703
Cl40.6458 (4)0.2956 (7)0.0264 (5)0.108 (3)*0.7703
C320.6951 (11)0.267 (2)0.0186 (14)0.082 (10)*0.7703
H32A0.72390.23930.05620.098*0.7703
H32B0.68280.21700.01230.098*0.7703
Cl50.6784 (9)0.3268 (18)0.3045 (11)0.192 (10)*0.5
Cl60.7025 (8)0.4047 (17)0.2388 (9)0.167 (8)*0.5
C330.7266 (15)0.402 (3)0.3124 (13)0.093 (18)*0.5
H33A0.72750.46710.32820.112*0.5
H33B0.76070.37180.33670.112*0.5
Atomic displacement parameters (Å2) top
U11U22U33U12U13U23
I10.0698 (11)0.0301 (9)0.0734 (11)0.0023 (7)0.0305 (9)0.0104 (7)
I20.0699 (10)0.0582 (10)0.0526 (9)0.0088 (8)0.0463 (9)0.0160 (7)
I30.0646 (10)0.0281 (8)0.0471 (8)0.0122 (7)0.0360 (8)0.0024 (6)
Cd10.0419 (9)0.0294 (8)0.0305 (8)0.0010 (7)0.0198 (7)0.0039 (6)
Cd20.0606 (14)0.0170 (10)0.0349 (12)0.0000.0368 (11)0.000
Fe10.0441 (16)0.0114 (13)0.0329 (15)0.0044 (12)0.0267 (14)0.0054 (11)
Cl10.101 (8)0.111 (9)0.114 (8)0.010 (6)0.040 (7)0.039 (7)
Cl20.090 (6)0.073 (6)0.108 (7)0.002 (5)0.076 (6)0.009 (5)
Geometric parameters (Å, º) top
I1—Cd12.687 (2)C11—H11B0.9800
I2—Cd12.6989 (19)C11—H11C0.9800
I3—Cd22.6874 (15)C12—C131.40 (2)
Cd1—N3i2.267 (13)C13—C141.39 (2)
Cd1—N12.293 (14)C13—C161.51 (2)
Cd2—N2ii2.269 (13)C14—C151.50 (2)
Cd2—N22.269 (13)C15—H15A0.9800
Cd2—I3ii2.6874 (15)C15—H15B0.9800
Fe1—O41.966 (11)C15—H15C0.9800
Fe1—O61.984 (10)C16—C171.36 (2)
Fe1—O21.986 (11)C16—C201.38 (2)
Fe1—O11.987 (11)C17—C181.42 (2)
Fe1—O51.989 (10)C17—H170.9500
Fe1—O32.007 (10)C18—H180.9500
O1—C21.255 (18)C19—C201.41 (2)
O2—C41.30 (2)C19—H190.9500
O3—C121.277 (17)C20—H200.9500
O4—C141.307 (18)C21—C221.47 (2)
O5—C221.295 (18)C21—H21A0.9800
O6—C241.288 (17)C21—H21B0.9800
N1—C91.31 (2)C21—H21C0.9800
N1—C81.38 (2)C22—C231.41 (2)
N2—C191.28 (2)C23—C241.42 (2)
N2—C181.30 (2)C23—C261.50 (2)
N3—C291.336 (19)C24—C251.51 (2)
N3—C281.371 (19)C25—H25A0.9800
N3—Cd1iii2.267 (13)C25—H25B0.9800
C1—C21.49 (2)C25—H25C0.9800
C1—H1A0.9800C26—C271.37 (2)
C1—H1B0.9800C26—C301.41 (2)
C1—H1C0.9800C27—C281.39 (2)
C2—C31.39 (2)C27—H270.9500
C3—C41.39 (2)C28—H280.9500
C3—C61.48 (2)C29—C301.40 (2)
C4—C51.50 (3)C29—H290.9500
C5—H5A0.9800C30—H300.9500
C5—H5B0.9800Cl1—C311.60 (2)
C5—H5C0.9800Cl2—C311.74 (2)
C6—C71.34 (2)C31—H31A0.9900
C6—C101.38 (2)C31—H31B0.9900
C7—C81.39 (2)Cl3—C321.73 (3)
C7—H70.9500Cl4—C321.76 (3)
C8—H80.9500C32—H32A0.9900
C9—C101.34 (2)C32—H32B0.9900
C9—H90.9500Cl5—C331.774 (19)
C10—H100.9500Cl6—C331.717 (19)
C11—C121.50 (2)C33—H33A0.9900
C11—H11A0.9800C33—H33B0.9900
N3i—Cd1—N190.9 (5)O3—C12—C13123.3 (14)
N3i—Cd1—I1113.9 (3)O3—C12—C11116.1 (13)
N1—Cd1—I1102.9 (4)C13—C12—C11120.5 (14)
N3i—Cd1—I2103.9 (3)C14—C13—C12124.0 (15)
N1—Cd1—I2105.3 (4)C14—C13—C16117.7 (14)
I1—Cd1—I2131.84 (7)C12—C13—C16118.2 (14)
N2ii—Cd2—N299.3 (7)O4—C14—C13122.8 (15)
N2ii—Cd2—I3109.1 (3)O4—C14—C15114.4 (15)
N2—Cd2—I3105.2 (3)C13—C14—C15122.9 (15)
N2ii—Cd2—I3ii105.2 (3)C14—C15—H15A109.5
N2—Cd2—I3ii109.1 (3)C14—C15—H15B109.5
I3—Cd2—I3ii125.76 (9)H15A—C15—H15B109.5
O4—Fe1—O693.2 (4)C14—C15—H15C109.5
O4—Fe1—O290.1 (5)H15A—C15—H15C109.5
O6—Fe1—O289.1 (4)H15B—C15—H15C109.5
O4—Fe1—O1168.3 (5)C17—C16—C20116.3 (16)
O6—Fe1—O197.4 (4)C17—C16—C13121.6 (14)
O2—Fe1—O185.3 (5)C20—C16—C13122.0 (15)
O4—Fe1—O593.3 (4)C16—C17—C18119.5 (16)
O6—Fe1—O586.4 (4)C16—C17—H17120.3
O2—Fe1—O5174.5 (5)C18—C17—H17120.3
O1—Fe1—O592.1 (4)N2—C18—C17123.7 (17)
O4—Fe1—O385.3 (4)N2—C18—H18118.1
O6—Fe1—O3176.8 (4)C17—C18—H18118.1
O2—Fe1—O393.6 (4)N2—C19—C20124.8 (18)
O1—Fe1—O384.3 (4)N2—C19—H19117.6
O5—Fe1—O390.9 (4)C20—C19—H19117.6
C2—O1—Fe1124.3 (11)C16—C20—C19118.7 (17)
C4—O2—Fe1122.1 (12)C16—C20—H20120.6
C12—O3—Fe1130.2 (10)C19—C20—H20120.6
C14—O4—Fe1131.2 (11)C22—C21—H21A109.5
C22—O5—Fe1130.8 (11)C22—C21—H21B109.5
C24—O6—Fe1130.8 (10)H21A—C21—H21B109.5
C9—N1—C8116.2 (16)C22—C21—H21C109.5
C9—N1—Cd1125.8 (13)H21A—C21—H21C109.5
C8—N1—Cd1117.8 (12)H21B—C21—H21C109.5
C19—N2—C18116.8 (16)O5—C22—C23124.0 (15)
C19—N2—Cd2122.1 (12)O5—C22—C21115.7 (15)
C18—N2—Cd2121.0 (12)C23—C22—C21120.3 (15)
C29—N3—C28118.7 (15)C22—C23—C24122.4 (15)
C29—N3—Cd1iii118.1 (11)C22—C23—C26117.7 (14)
C28—N3—Cd1iii122.7 (11)C24—C23—C26119.9 (14)
C2—C1—H1A109.5O6—C24—C23124.4 (15)
C2—C1—H1B109.5O6—C24—C25114.0 (14)
H1A—C1—H1B109.5C23—C24—C25121.5 (14)
C2—C1—H1C109.5C24—C25—H25A109.5
H1A—C1—H1C109.5C24—C25—H25B109.5
H1B—C1—H1C109.5H25A—C25—H25B109.5
O1—C2—C3125.4 (16)C24—C25—H25C109.5
O1—C2—C1115.0 (15)H25A—C25—H25C109.5
C3—C2—C1119.5 (16)H25B—C25—H25C109.5
C4—C3—C2120.7 (16)C27—C26—C30119.1 (16)
C4—C3—C6118.4 (16)C27—C26—C23121.5 (15)
C2—C3—C6120.9 (16)C30—C26—C23119.4 (15)
O2—C4—C3126.3 (18)C26—C27—C28119.1 (17)
O2—C4—C5111.5 (18)C26—C27—H27120.4
C3—C4—C5121.9 (18)C28—C27—H27120.4
C4—C5—H5A109.5N3—C28—C27122.1 (17)
C4—C5—H5B109.5N3—C28—H28118.9
H5A—C5—H5B109.5C27—C28—H28118.9
C4—C5—H5C109.5N3—C29—C30121.3 (16)
H5A—C5—H5C109.5N3—C29—H29119.3
H5B—C5—H5C109.5C30—C29—H29119.3
C7—C6—C10115.2 (17)C29—C30—C26119.3 (17)
C7—C6—C3125.3 (17)C29—C30—H30120.4
C10—C6—C3119.4 (16)C26—C30—H30120.4
C6—C7—C8125 (2)Cl1—C31—Cl2117.6 (16)
C6—C7—H7117.6Cl1—C31—H31A107.9
C8—C7—H7117.6Cl2—C31—H31A107.9
N1—C8—C7118.1 (19)Cl1—C31—H31B107.9
N1—C8—H8120.9Cl2—C31—H31B107.9
C7—C8—H8120.9H31A—C31—H31B107.2
N1—C9—C10126.4 (19)Cl3—C32—Cl4113.9 (18)
N1—C9—H9116.8Cl3—C32—H32A108.8
C10—C9—H9116.8Cl4—C32—H32A108.8
C9—C10—C6119.3 (18)Cl3—C32—H32B108.8
C9—C10—H10120.4Cl4—C32—H32B108.8
C6—C10—H10120.4H32A—C32—H32B107.7
C12—C11—H11A109.5Cl6—C33—Cl595.8 (18)
C12—C11—H11B109.5Cl6—C33—H33A112.6
H11A—C11—H11B109.5Cl5—C33—H33A112.6
C12—C11—H11C109.5Cl6—C33—H33B112.6
H11A—C11—H11C109.5Cl5—C33—H33B112.6
H11B—C11—H11C109.5H33A—C33—H33B110.1
Symmetry codes: (i) x+1/2, y+3/2, z+1/2; (ii) x+1, y, z+1/2; (iii) x1/2, y+3/2, z1/2.

Experimental details

(1)(2)(3a)(3b)
Crystal data
Chemical formulaC30H33Cd2Cl4N3O6C30H33Br4Cd2N3O6C10H11CdI2NO2C20H22CdI2N2O4
Mr898.211076.03543.41720.59
Crystal system, space groupTriclinic, P1Triclinic, P1Orthorhombic, PbcaOrthorhombic, Pca21
Temperature (K)100100100100
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, 9090, 90, 90
V3)1778.5 (2)1796.0 (4)2805.7 (6)4712.1 (5)
Z2288
Radiation typeMo KαMo KαMo KαMo Kα
µ (mm1)1.545.685.943.57
Crystal size (mm)0.29 × 0.08 × 0.060.18 × 0.13 × 0.040.27 × 0.07 × 0.030.25 × 0.13 × 0.11
Data collection
DiffractometerCCD area detector
diffractometer
CCD area detector
diffractometer
CCD area detector
diffractometer
CCD area detector
diffractometer
Absorption correctionMulti-scan
SADABS
Multi-scan
TWINABS
Multi-scan
SADABS
Multi-scan
SADABS
Tmin, Tmax0.632, 0.7460.522, 0.7460.474, 0.7460.522, 0.746
No. of measured, independent and
observed [I > 2σ(I)] reflections
26747, 9968, 7972 7336, 7336, 5914 39565, 4234, 3748 67491, 14053, 12009
Rint0.0480.0840.0470.051
θmax (°)29.926.430.931.0
(sin θ/λ)max1)0.7010.6250.7230.724
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 reflections99687336423414053
No. of parameters421423147545
No. of restraints31105
H-atom treatmentH atoms treated by a mixture of independent and constrained refinementH atoms treated by a mixture of independent and constrained refinementH-atom parameters constrainedH atoms treated by a mixture of independent and constrained refinement
Δρmax, Δρmin (e Å3)0.74, 0.540.99, 0.910.69, 0.591.29, 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 formulaC60H60CdCl2Fe2N6O12·6(CH4O)·6(H2O)C60H60Br2CdFe2N6O12·0.24(C2H8O2)·4.75(CH4O)·6(H2O)C64.09H68.18Cd3Cl8.18Fe2I6N6O12C64.09H68.18Cd3Cl8.18Fe2I6N6O12
Mr1652.501716.662614.572614.57
Crystal system, space groupTriclinic, P1Triclinic, P1Monoclinic, C2/cMonoclinic, C2/c
Temperature (K)100100100100
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), 9090, 125.118 (8), 90
V3)2011.0 (4)2058.8 (4)10061.4 (18)10061.4 (18)
Z1144
Radiation typeMo KαMo KαMo KαMo Kα
µ (mm1)0.761.643.013.01
Crystal size (mm)0.25 × 0.23 × 0.080.36 × 0.10 × 0.030.15 × 0.08 × 0.070.15 × 0.08 × 0.07
Data collection
DiffractometerCCD area detector
diffractometer
CCD area detector
diffractometer
CCD area detector
diffractometer
CCD area detector
diffractometer
Absorption correctionMulti-scan
SADABS
Multi-scan
SADABS
Multi-scan
SADABS
Multi-scan
SADABS
Tmin, Tmax0.640, 0.7450.595, 0.7450.587, 0.7450.587, 0.745
No. of measured, independent and
observed [I > 2σ(I)] reflections
24575, 8416, 6746 24811, 8482, 6555 41442, 6166, 3817 41442, 6166, 3835
Rint0.0500.0520.0850.090
θmax (°)26.626.522.022.0
(sin θ/λ)max1)0.6300.6270.5270.527
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 reflections8416848261666166
No. of parameters456441259259
No. of restraints0222
H-atom treatmentH-atom parameters constrainedH-atom parameters constrainedH-atom parameters constrainedH-atom parameters constrained
Δρmax, Δρmin (e Å3)1.12, 0.921.30, 1.052.31, 1.522.43, 1.56
Absolute structure????
Absolute structure parameter????

Computer programs: Bruker SAMRT, Bruker SMART, Bruker SAINT 2009, SHELXS97, SHELXL97, SHELXL2013 (Sheldrick, 2013).

 

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