3-(4-Pyridyl)-acetylacetone – a fully featured substituted pyridine and a flexible linker for complex materials

Merkens, C.; Truong, K.-N.; Englert, U.

doi:10.1107/S2052520614006210

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3-(4-Pyridyl)-acetylacetone – a fully featured substituted pyridine and a flexible linker for complex materials

C. Merkens, K.-N. Truong and U. Englert

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 Fe^III, and the resulting complex Fe(acacPy)₃ reacts analogously to a bridging polypyridine ligand towards the same Cd halides as the molecule HacacPy itself. With 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.

Keywords: coordination polymers; extended bimetallic structures; solid-state reactivity.

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Supporting information

	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
	Structure factor file (CIF format) https://doi.org/10.1107/S2052520614006210/bm50631sup2.hkl Contains datablock 1
	Structure factor file (CIF format) https://doi.org/10.1107/S2052520614006210/bm50632sup3.hkl Contains datablock 2
	Structure factor file (CIF format) https://doi.org/10.1107/S2052520614006210/bm50633asup4.hkl Contains datablock 3a
	Structure factor file (CIF format) https://doi.org/10.1107/S2052520614006210/bm50633bsup5.hkl Contains datablock 3b
	Structure factor file (CIF format) https://doi.org/10.1107/S2052520614006210/bm50634sup6.hkl Contains datablock 4
	Structure factor file (CIF format) https://doi.org/10.1107/S2052520614006210/bm50635sup7.hkl Contains datablock 5
	Structure factor file (CIF format) https://doi.org/10.1107/S2052520614006210/bm50636_squeezesup8.hkl Contains datablock 6_squeeze
	Structure factor file (CIF format) https://doi.org/10.1107/S2052520614006210/bm50636_without_squeezesup9.hkl Contains datablock 6_without_squeeze
	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

(1) top

Crystal data top

C₃₀H₃₃Cd₂Cl₄N₃O₆	Z = 2
M_r = 898.21	F(000) = 892
Triclinic, P1	D_x = 1.677 Mg m⁻³
a = 9.8304 (8) Å	Mo Kα radiation, λ = 0.71073 Å
b = 13.7388 (11) Å	Cell parameters from 3427 reflections
c = 14.8816 (12) Å	θ = 2.5–28.3°
α = 63.4935 (11)°	µ = 1.54 mm⁻¹
β = 84.0016 (13)°	T = 100 K
γ = 81.8575 (12)°	Needle, colorless
V = 1778.5 (2) Å³	0.29 × 0.08 × 0.06 mm

Data collection top

CCD area detector diffractometer	7972 reflections with I > 2σ(I)
Radiation source: Incoatec microsource, multilayer optics	R_int = 0.048
ω scans	θ_max = 29.9°, θ_min = 2.1°
Absorption correction: multi-scan SADABS	h = −13→13
T_min = 0.632, T_max = 0.746	k = −19→19
26747 measured reflections	l = −20→20
9968 independent reflections

Refinement top

Refinement on F²	Primary atom site location: heavy-atom method
Least-squares matrix: full	Hydrogen site location: mixed
R[F² > 2σ(F²)] = 0.037	H atoms treated by a mixture of independent and constrained refinement
wR(F²) = 0.079	w = 1/[σ²(F_o²) + (0.0241P)²] where P = (F_o² + 2F_c²)/3
S = 1.03	(Δ/σ)_max = 0.001
9968 reflections	Δρ_max = 0.74 e Å⁻³
421 parameters	Δρ_min = −0.54 e Å⁻³
3 restraints

Crystal data top

C₃₀H₃₃Cd₂Cl₄N₃O₆	γ = 81.8575 (12)°
M_r = 898.21	V = 1778.5 (2) Å³
Triclinic, P1	Z = 2
a = 9.8304 (8) Å	Mo Kα radiation
b = 13.7388 (11) Å	µ = 1.54 mm⁻¹
c = 14.8816 (12) Å	T = 100 K
α = 63.4935 (11)°	0.29 × 0.08 × 0.06 mm
β = 84.0016 (13)°

Data collection top

CCD area detector diffractometer	9968 independent reflections
Absorption correction: multi-scan SADABS	7972 reflections with I > 2σ(I)
T_min = 0.632, T_max = 0.746	R_int = 0.048
26747 measured reflections

Refinement top

R[F² > 2σ(F²)] = 0.037	3 restraints
wR(F²) = 0.079	H atoms treated by a mixture of independent and constrained refinement
S = 1.03	Δρ_max = 0.74 e Å⁻³
9968 reflections	Δρ_min = −0.54 e Å⁻³
421 parameters

Special details top

Geometry. All e.s.d.'s (except the e.s.d. in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell e.s.d.'s are taken into account individually in the estimation of e.s.d.'s in distances, angles and torsion angles; correlations between e.s.d.'s in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell e.s.d.'s is used for estimating e.s.d.'s involving l.s. planes.

Fractional atomic coordinates and isotropic or equivalent isotropic displacement parameters (Å²) top

	x	y	z	U_iso*/U_eq
Cd1	0.50443 (2)	0.05368 (2)	0.35685 (2)	0.01277 (5)
Cd2	0.15023 (2)	0.07845 (2)	0.49986 (2)	0.01286 (5)
Cl1	0.35930 (7)	−0.08333 (5)	0.51401 (5)	0.01328 (13)
Cl2	0.30590 (7)	0.20222 (5)	0.35240 (5)	0.01551 (14)
Cl3	0.28795 (7)	0.08664 (6)	0.63691 (5)	0.01653 (14)
Cl4	0.01156 (7)	0.05557 (5)	0.36904 (5)	0.01549 (14)
O1	0.1299 (2)	−0.10925 (19)	−0.06145 (17)	0.0307 (6)
O2	−0.0320 (3)	−0.1808 (2)	0.08470 (18)	0.0306 (6)
H2D	0.009 (3)	−0.162 (3)	0.0278 (17)	0.037*
O3	0.8559 (3)	0.5588 (2)	−0.18904 (19)	0.0452 (7)
H3D	0.868 (4)	0.600 (3)	−0.160 (3)	0.054*
O4	0.8571 (3)	0.6459 (2)	−0.0755 (2)	0.0465 (7)
O5	−0.5520 (2)	0.55950 (18)	0.32619 (19)	0.0301 (6)
H5D	−0.533 (4)	0.601 (2)	0.351 (2)	0.036*
O6	−0.4417 (2)	0.66111 (17)	0.39087 (18)	0.0283 (5)
N1	0.3871 (2)	0.00479 (19)	0.25611 (17)	0.0143 (5)
N2	0.6033 (3)	0.19701 (19)	0.21866 (18)	0.0177 (5)
N3	−0.0091 (2)	0.23090 (18)	0.48202 (17)	0.0147 (5)
C1	−0.0101 (4)	−0.1713 (3)	0.2366 (3)	0.0330 (8)
H1A	−0.0990	−0.2010	0.2512	0.049*
H1B	−0.0205	−0.1033	0.2441	0.049*
H1C	0.0569	−0.2245	0.2835	0.049*
C2	0.0389 (3)	−0.1487 (3)	0.1319 (2)	0.0226 (7)
C3	0.1587 (3)	−0.0961 (2)	0.0873 (2)	0.0185 (6)
C4	0.1994 (3)	−0.0771 (3)	−0.0116 (2)	0.0230 (7)
C5	0.3214 (4)	−0.0197 (3)	−0.0668 (3)	0.0337 (8)
H5A	0.3186	−0.0006	−0.1384	0.050*
H5B	0.4057	−0.0678	−0.0400	0.050*
H5C	0.3203	0.0472	−0.0582	0.050*
C6	0.2393 (3)	−0.0607 (2)	0.1451 (2)	0.0164 (6)
C7	0.2049 (3)	0.0395 (3)	0.1478 (2)	0.0241 (7)
H7	0.1303	0.0881	0.1111	0.029*
C8	0.2800 (3)	0.0681 (2)	0.2044 (2)	0.0206 (7)
H8	0.2537	0.1364	0.2064	0.025*
C9	0.4215 (3)	−0.0925 (2)	0.2543 (2)	0.0194 (6)
H9	0.4976	−0.1388	0.2909	0.023*
C10	0.3497 (3)	−0.1273 (2)	0.2007 (2)	0.0220 (7)
H10	0.3760	−0.1972	0.2020	0.026*
C11	0.7779 (4)	0.3892 (3)	−0.1410 (3)	0.0438 (10)
H11A	0.6994	0.4150	−0.1843	0.066*
H11B	0.7577	0.3235	−0.0799	0.066*
H11C	0.8597	0.3717	−0.1770	0.066*
C12	0.8038 (4)	0.4762 (3)	−0.1133 (3)	0.0328 (8)
C13	0.7788 (3)	0.4731 (3)	−0.0195 (2)	0.0255 (7)
C14	0.8102 (4)	0.5627 (3)	−0.0036 (3)	0.0370 (9)
C15	0.7880 (5)	0.5631 (3)	0.0974 (3)	0.0508 (12)
H15A	0.8072	0.6338	0.0917	0.076*
H15B	0.8498	0.5045	0.1448	0.076*
H15C	0.6923	0.5514	0.1217	0.076*
C16	0.7194 (3)	0.3772 (2)	0.0642 (2)	0.0235 (7)
C17	0.7965 (3)	0.3002 (3)	0.1439 (2)	0.0252 (7)
H17	0.8902	0.3077	0.1472	0.030*
C18	0.7346 (3)	0.2121 (3)	0.2185 (2)	0.0221 (7)
H18	0.7886	0.1600	0.2722	0.027*
C19	0.5291 (3)	0.2716 (3)	0.1418 (2)	0.0245 (7)
H19	0.4351	0.2628	0.1412	0.029*
C20	0.5826 (3)	0.3599 (3)	0.0642 (2)	0.0283 (8)
H20	0.5267	0.4092	0.0106	0.034*
C21	−0.2290 (3)	0.6006 (3)	0.4710 (3)	0.0273 (7)
H21A	−0.2407	0.6760	0.4631	0.041*
H21B	−0.1388	0.5860	0.4420	0.041*
H21C	−0.2352	0.5499	0.5426	0.041*
C22	−0.3392 (3)	0.5852 (3)	0.4182 (2)	0.0236 (7)
C23	−0.3380 (3)	0.4930 (2)	0.4003 (2)	0.0182 (6)
C24	−0.4495 (3)	0.4833 (2)	0.3537 (2)	0.0232 (7)
C25	−0.4587 (4)	0.3874 (3)	0.3338 (3)	0.0342 (9)
H25A	−0.4937	0.3280	0.3948	0.051*
H25B	−0.3672	0.3624	0.3140	0.051*
H25C	−0.5213	0.4085	0.2794	0.051*
C26	−0.2210 (3)	0.4037 (2)	0.4311 (2)	0.0169 (6)
C27	−0.2391 (3)	0.3009 (2)	0.5084 (2)	0.0186 (6)
H27	−0.3248	0.2875	0.5454	0.022*
C28	−0.1315 (3)	0.2180 (2)	0.5311 (2)	0.0165 (6)
H28	−0.1458	0.1483	0.5845	0.020*
C29	0.0094 (3)	0.3313 (2)	0.4081 (2)	0.0197 (6)
H29	0.0965	0.3430	0.3731	0.024*
C30	−0.0933 (3)	0.4178 (2)	0.3811 (2)	0.0195 (6)
H30	−0.0761	0.4870	0.3282	0.023*

Atomic displacement parameters (Å²) top

	U¹¹	U²²	U³³	U¹²	U¹³	U²³
Cd1	0.01101 (11)	0.01454 (10)	0.01177 (10)	−0.00073 (8)	−0.00071 (8)	−0.00502 (8)
Cd2	0.00964 (10)	0.01305 (10)	0.01458 (11)	−0.00053 (8)	−0.00095 (8)	−0.00500 (8)
Cl1	0.0121 (3)	0.0132 (3)	0.0141 (3)	−0.0014 (3)	−0.0011 (3)	−0.0055 (3)
Cl2	0.0121 (3)	0.0143 (3)	0.0174 (3)	−0.0008 (3)	0.0012 (3)	−0.0051 (3)
Cl3	0.0133 (3)	0.0197 (3)	0.0186 (3)	0.0013 (3)	−0.0035 (3)	−0.0106 (3)
Cl4	0.0132 (3)	0.0164 (3)	0.0146 (3)	−0.0029 (3)	−0.0010 (3)	−0.0044 (3)
O1	0.0319 (14)	0.0429 (14)	0.0270 (13)	0.0038 (11)	−0.0119 (11)	−0.0240 (11)
O2	0.0268 (14)	0.0389 (14)	0.0338 (14)	−0.0058 (11)	−0.0041 (11)	−0.0217 (12)
O3	0.0498 (18)	0.0362 (16)	0.0269 (14)	0.0024 (14)	0.0129 (13)	0.0014 (12)
O4	0.0450 (18)	0.0296 (14)	0.0456 (17)	−0.0136 (13)	−0.0016 (14)	0.0033 (12)
O5	0.0235 (13)	0.0208 (12)	0.0476 (16)	0.0070 (10)	−0.0153 (11)	−0.0164 (11)
O6	0.0232 (13)	0.0181 (11)	0.0440 (15)	0.0063 (9)	−0.0080 (11)	−0.0150 (11)
N1	0.0120 (12)	0.0160 (12)	0.0140 (12)	−0.0026 (10)	−0.0004 (9)	−0.0055 (10)
N2	0.0167 (13)	0.0198 (12)	0.0144 (12)	−0.0010 (10)	−0.0010 (10)	−0.0057 (10)
N3	0.0135 (13)	0.0150 (12)	0.0148 (12)	0.0008 (10)	−0.0028 (10)	−0.0059 (10)
C1	0.0250 (19)	0.044 (2)	0.032 (2)	−0.0085 (16)	0.0048 (15)	−0.0187 (17)
C2	0.0188 (17)	0.0269 (17)	0.0268 (17)	0.0005 (13)	−0.0043 (13)	−0.0162 (14)
C3	0.0130 (15)	0.0245 (15)	0.0219 (16)	0.0019 (12)	−0.0060 (12)	−0.0136 (13)
C4	0.0227 (17)	0.0264 (17)	0.0205 (16)	0.0043 (14)	−0.0067 (13)	−0.0116 (14)
C5	0.031 (2)	0.048 (2)	0.0241 (18)	−0.0061 (18)	0.0001 (15)	−0.0180 (17)
C6	0.0170 (16)	0.0206 (15)	0.0131 (14)	−0.0012 (12)	−0.0016 (12)	−0.0087 (12)
C7	0.0199 (17)	0.0290 (17)	0.0272 (17)	0.0080 (13)	−0.0146 (14)	−0.0159 (14)
C8	0.0223 (17)	0.0217 (15)	0.0207 (16)	0.0037 (13)	−0.0076 (13)	−0.0122 (13)
C9	0.0166 (16)	0.0194 (15)	0.0222 (16)	0.0028 (12)	−0.0069 (12)	−0.0092 (13)
C10	0.0227 (17)	0.0175 (15)	0.0269 (17)	−0.0003 (13)	−0.0066 (14)	−0.0100 (13)
C11	0.057 (3)	0.038 (2)	0.028 (2)	0.011 (2)	0.0002 (19)	−0.0116 (17)
C12	0.030 (2)	0.0257 (18)	0.0231 (18)	0.0052 (15)	0.0031 (15)	0.0030 (14)
C13	0.0239 (18)	0.0200 (16)	0.0204 (16)	−0.0022 (13)	−0.0009 (14)	0.0020 (13)
C14	0.031 (2)	0.0286 (19)	0.037 (2)	−0.0079 (16)	−0.0019 (17)	0.0000 (16)
C15	0.068 (3)	0.038 (2)	0.046 (3)	−0.020 (2)	−0.008 (2)	−0.014 (2)
C16	0.0246 (18)	0.0205 (16)	0.0215 (16)	−0.0015 (13)	0.0002 (13)	−0.0064 (13)
C17	0.0185 (17)	0.0260 (17)	0.0254 (17)	−0.0063 (14)	0.0002 (14)	−0.0055 (14)
C18	0.0180 (16)	0.0241 (16)	0.0187 (15)	0.0021 (13)	−0.0021 (13)	−0.0055 (13)
C19	0.0127 (16)	0.0317 (18)	0.0245 (17)	−0.0012 (13)	−0.0031 (13)	−0.0082 (14)
C20	0.0258 (19)	0.0269 (17)	0.0222 (17)	−0.0007 (15)	−0.0059 (14)	−0.0014 (14)
C21	0.0262 (19)	0.0206 (16)	0.038 (2)	0.0003 (14)	−0.0073 (15)	−0.0152 (15)
C22	0.0193 (17)	0.0207 (16)	0.0291 (18)	−0.0017 (13)	0.0005 (14)	−0.0098 (14)
C23	0.0161 (16)	0.0139 (14)	0.0215 (15)	0.0031 (12)	−0.0025 (12)	−0.0060 (12)
C24	0.0173 (16)	0.0157 (15)	0.0333 (18)	0.0019 (12)	−0.0047 (14)	−0.0081 (14)
C25	0.034 (2)	0.0270 (18)	0.046 (2)	0.0034 (16)	−0.0158 (18)	−0.0193 (17)
C26	0.0147 (15)	0.0171 (14)	0.0232 (16)	0.0019 (12)	−0.0057 (12)	−0.0127 (13)
C27	0.0153 (15)	0.0168 (14)	0.0228 (16)	−0.0031 (12)	0.0030 (12)	−0.0084 (12)
C28	0.0149 (15)	0.0151 (14)	0.0192 (15)	−0.0019 (11)	0.0003 (12)	−0.0075 (12)
C29	0.0173 (16)	0.0201 (15)	0.0203 (15)	−0.0037 (12)	0.0018 (12)	−0.0079 (13)
C30	0.0210 (17)	0.0131 (14)	0.0202 (15)	0.0004 (12)	0.0000 (13)	−0.0043 (12)

Geometric parameters (Å, º) top

Cd1—N1	2.347 (2)	C7—H7	0.9500
Cd1—N2	2.358 (2)	C8—H8	0.9500
Cd1—Cl3ⁱ	2.5800 (7)	C9—C10	1.385 (4)
Cd1—Cl2	2.5992 (7)	C9—H9	0.9500
Cd1—Cl1ⁱ	2.6542 (7)	C10—H10	0.9500
Cd1—Cl1	2.6800 (7)	C11—C12	1.487 (5)
Cd2—N3	2.360 (2)	C11—H11A	0.9800
Cd2—Cl4ⁱⁱ	2.5885 (7)	C11—H11B	0.9800
Cd2—Cl2	2.5987 (7)	C11—H11C	0.9800
Cd2—Cl3	2.6135 (7)	C12—C13	1.375 (5)
Cd2—Cl4	2.6400 (7)	C13—C14	1.432 (5)
Cd2—Cl1	2.7544 (7)	C13—C16	1.493 (4)
Cl1—Cd1ⁱ	2.6542 (7)	C14—C15	1.498 (5)
Cl3—Cd1ⁱ	2.5800 (7)	C15—H15A	0.9800
Cl4—Cd2ⁱⁱ	2.5885 (7)	C15—H15B	0.9800
O1—C4	1.302 (4)	C15—H15C	0.9800
O2—C2	1.281 (4)	C16—C17	1.394 (4)
O2—H2D	0.841 (18)	C16—C20	1.398 (4)
O3—C12	1.313 (4)	C17—C18	1.390 (4)
O3—H3D	0.880 (18)	C17—H17	0.9500
O4—C14	1.272 (4)	C18—H18	0.9500
O5—C24	1.297 (3)	C19—C20	1.373 (4)
O5—H5D	0.859 (18)	C19—H19	0.9500
O6—C22	1.295 (4)	C20—H20	0.9500
N1—C8	1.331 (4)	C21—C22	1.493 (4)
N1—C9	1.343 (3)	C21—H21A	0.9800
N2—C18	1.336 (4)	C21—H21B	0.9800
N2—C19	1.344 (4)	C21—H21C	0.9800
N3—C28	1.332 (4)	C22—C23	1.405 (4)
N3—C29	1.349 (3)	C23—C24	1.408 (4)
C1—C2	1.486 (4)	C23—C26	1.499 (4)
C1—H1A	0.9800	C24—C25	1.491 (4)
C1—H1B	0.9800	C25—H25A	0.9800
C1—H1C	0.9800	C25—H25B	0.9800
C2—C3	1.414 (4)	C25—H25C	0.9800
C3—C4	1.400 (4)	C26—C30	1.382 (4)
C3—C6	1.493 (4)	C26—C27	1.389 (4)
C4—C5	1.490 (5)	C27—C28	1.386 (4)
C5—H5A	0.9800	C27—H27	0.9500
C5—H5B	0.9800	C28—H28	0.9500
C5—H5C	0.9800	C29—C30	1.382 (4)
C6—C7	1.387 (4)	C29—H29	0.9500
C6—C10	1.390 (4)	C30—H30	0.9500
C7—C8	1.384 (4)

N1—Cd1—N2	93.94 (8)	N1—C9—C10	122.1 (3)
N1—Cd1—Cl3ⁱ	91.38 (6)	N1—C9—H9	118.9
N2—Cd1—Cl3ⁱ	92.61 (6)	C10—C9—H9	118.9
N1—Cd1—Cl2	91.88 (6)	C9—C10—C6	120.4 (3)
N2—Cd1—Cl2	85.55 (6)	C9—C10—H10	119.8
Cl3ⁱ—Cd1—Cl2	176.36 (2)	C6—C10—H10	119.8
N1—Cd1—Cl1ⁱ	173.05 (6)	C12—C11—H11A	109.5
N2—Cd1—Cl1ⁱ	91.79 (6)	C12—C11—H11B	109.5
Cl3ⁱ—Cd1—Cl1ⁱ	84.42 (2)	H11A—C11—H11B	109.5
Cl2—Cd1—Cl1ⁱ	92.48 (2)	C12—C11—H11C	109.5
N1—Cd1—Cl1	86.84 (6)	H11A—C11—H11C	109.5
N2—Cd1—Cl1	170.48 (6)	H11B—C11—H11C	109.5
Cl3ⁱ—Cd1—Cl1	96.86 (2)	O3—C12—C13	122.1 (3)
Cl2—Cd1—Cl1	84.94 (2)	O3—C12—C11	112.5 (3)
Cl1ⁱ—Cd1—Cl1	88.16 (2)	C13—C12—C11	125.4 (3)
N3—Cd2—Cl4ⁱⁱ	91.69 (6)	C12—C13—C14	119.2 (3)
N3—Cd2—Cl2	91.04 (6)	C12—C13—C16	119.9 (3)
Cl4ⁱⁱ—Cd2—Cl2	172.39 (2)	C14—C13—C16	120.9 (3)
N3—Cd2—Cl3	94.90 (6)	O4—C14—C13	120.9 (4)
Cl4ⁱⁱ—Cd2—Cl3	93.40 (2)	O4—C14—C15	117.4 (3)
Cl2—Cd2—Cl3	93.45 (2)	C13—C14—C15	121.7 (3)
N3—Cd2—Cl4	87.86 (6)	C14—C15—H15A	109.5
Cl4ⁱⁱ—Cd2—Cl4	83.73 (2)	C14—C15—H15B	109.5
Cl2—Cd2—Cl4	89.28 (2)	H15A—C15—H15B	109.5
Cl3—Cd2—Cl4	176.08 (2)	C14—C15—H15C	109.5
N3—Cd2—Cl1	173.39 (6)	H15A—C15—H15C	109.5
Cl4ⁱⁱ—Cd2—Cl1	94.23 (2)	H15B—C15—H15C	109.5
Cl2—Cd2—Cl1	83.46 (2)	C17—C16—C20	117.0 (3)
Cl3—Cd2—Cl1	81.83 (2)	C17—C16—C13	122.4 (3)
Cl4—Cd2—Cl1	95.70 (2)	C20—C16—C13	120.6 (3)
Cd1ⁱ—Cl1—Cd1	91.84 (2)	C18—C17—C16	119.2 (3)
Cd1ⁱ—Cl1—Cd2	94.11 (2)	C18—C17—H17	120.4
Cd1—Cl1—Cd2	92.96 (2)	C16—C17—H17	120.4
Cd2—Cl2—Cd1	98.61 (2)	N2—C18—C17	123.5 (3)
Cd1ⁱ—Cl3—Cd2	99.36 (2)	N2—C18—H18	118.3
Cd2ⁱⁱ—Cl4—Cd2	96.27 (2)	C17—C18—H18	118.3
C2—O2—H2D	105 (3)	N2—C19—C20	123.1 (3)
C12—O3—H3D	101 (3)	N2—C19—H19	118.5
C24—O5—H5D	102 (2)	C20—C19—H19	118.5
C8—N1—C9	117.8 (2)	C19—C20—C16	120.0 (3)
C8—N1—Cd1	121.87 (19)	C19—C20—H20	120.0
C9—N1—Cd1	120.23 (19)	C16—C20—H20	120.0
C18—N2—C19	117.3 (3)	C22—C21—H21A	109.5
C18—N2—Cd1	120.26 (19)	C22—C21—H21B	109.5
C19—N2—Cd1	122.2 (2)	H21A—C21—H21B	109.5
C28—N3—C29	117.1 (3)	C22—C21—H21C	109.5
C28—N3—Cd2	120.99 (18)	H21A—C21—H21C	109.5
C29—N3—Cd2	120.74 (19)	H21B—C21—H21C	109.5
C2—C1—H1A	109.5	O6—C22—C23	120.0 (3)
C2—C1—H1B	109.5	O6—C22—C21	116.4 (3)
H1A—C1—H1B	109.5	C23—C22—C21	123.5 (3)
C2—C1—H1C	109.5	C22—C23—C24	119.5 (3)
H1A—C1—H1C	109.5	C22—C23—C26	121.2 (3)
H1B—C1—H1C	109.5	C24—C23—C26	119.3 (3)
O2—C2—C3	121.7 (3)	O5—C24—C23	120.5 (3)
O2—C2—C1	116.5 (3)	O5—C24—C25	116.3 (3)
C3—C2—C1	121.8 (3)	C23—C24—C25	123.3 (3)
C4—C3—C2	119.1 (3)	C24—C25—H25A	109.5
C4—C3—C6	120.8 (3)	C24—C25—H25B	109.5
C2—C3—C6	120.1 (3)	H25A—C25—H25B	109.5
O1—C4—C3	120.7 (3)	C24—C25—H25C	109.5
O1—C4—C5	115.8 (3)	H25A—C25—H25C	109.5
C3—C4—C5	123.5 (3)	H25B—C25—H25C	109.5
C4—C5—H5A	109.5	C30—C26—C27	117.1 (3)
C4—C5—H5B	109.5	C30—C26—C23	122.0 (3)
H5A—C5—H5B	109.5	C27—C26—C23	120.8 (3)
C4—C5—H5C	109.5	C28—C27—C26	119.5 (3)
H5A—C5—H5C	109.5	C28—C27—H27	120.2
H5B—C5—H5C	109.5	C26—C27—H27	120.2
C7—C6—C10	116.8 (3)	N3—C28—C27	123.4 (3)
C7—C6—C3	121.4 (3)	N3—C28—H28	118.3
C10—C6—C3	121.8 (3)	C27—C28—H28	118.3
C8—C7—C6	119.6 (3)	N3—C29—C30	122.7 (3)
C8—C7—H7	120.2	N3—C29—H29	118.6
C6—C7—H7	120.2	C30—C29—H29	118.6
N1—C8—C7	123.3 (3)	C26—C30—C29	120.1 (3)
N1—C8—H8	118.4	C26—C30—H30	119.9
C7—C8—H8	118.4	C29—C30—H30	119.9

Symmetry codes: (i) −x+1, −y, −z+1; (ii) −x, −y, −z+1.

(2) top

Crystal data top

C₃₀H₃₃Br₄Cd₂N₃O₆	V = 1796.0 (4) Å³
M_r = 1076.03	Z = 2
Triclinic, P1	F(000) = 1036
a = 7.1262 (9) Å	D_x = 1.990 Mg m⁻³
b = 15.519 (2) Å	Mo Kα radiation, λ = 0.71073 Å
c = 16.597 (2) Å	µ = 5.68 mm⁻¹
α = 91.247 (3)°	T = 100 K
β = 97.889 (3)°	Plate, colorless
γ = 98.609 (3)°	0.18 × 0.13 × 0.04 mm

Data collection top

CCD area detector diffractometer	5914 reflections with I > 2σ(I)
Radiation source: Incoatec microsource	R_int = 0.084
ω scans	θ_max = 26.4°, θ_min = 1.2°
Absorption correction: multi-scan TWINABS	h = −8→8
T_min = 0.522, T_max = 0.746	k = −19→19
7336 measured reflections	l = 0→20
7336 independent reflections

Refinement top

Refinement on F²	11 restraints
Least-squares matrix: full	Hydrogen site location: mixed
R[F² > 2σ(F²)] = 0.056	H atoms treated by a mixture of independent and constrained refinement
wR(F²) = 0.103	w = 1/[σ²(F_o²) + (0.0199P)² + 4.2083P] where P = (F_o² + 2F_c²)/3
S = 1.14	(Δ/σ)_max = 0.001
7336 reflections	Δρ_max = 0.99 e Å⁻³
423 parameters	Δρ_min = −0.91 e Å⁻³

Crystal data top

C₃₀H₃₃Br₄Cd₂N₃O₆	γ = 98.609 (3)°
M_r = 1076.03	V = 1796.0 (4) Å³
Triclinic, P1	Z = 2
a = 7.1262 (9) Å	Mo Kα radiation
b = 15.519 (2) Å	µ = 5.68 mm⁻¹
c = 16.597 (2) Å	T = 100 K
α = 91.247 (3)°	0.18 × 0.13 × 0.04 mm
β = 97.889 (3)°

Data collection top

CCD area detector diffractometer	7336 independent reflections
Absorption correction: multi-scan TWINABS	5914 reflections with I > 2σ(I)
T_min = 0.522, T_max = 0.746	R_int = 0.084
7336 measured reflections

Refinement top

R[F² > 2σ(F²)] = 0.056	11 restraints
wR(F²) = 0.103	H atoms treated by a mixture of independent and constrained refinement
S = 1.14	Δρ_max = 0.99 e Å⁻³
7336 reflections	Δρ_min = −0.91 e Å⁻³
423 parameters

Special details top

Refinement. Refined as a 2-component twin.

Fractional atomic coordinates and isotropic or equivalent isotropic displacement parameters (Å²) top

	x	y	z	U_iso*/U_eq	Occ. (<1)
Cd1	0.79198 (10)	0.62721 (3)	0.25945 (4)	0.01556 (14)
Cd2	0.25939 (10)	0.53220 (3)	0.25449 (4)	0.01486 (14)
Br1	0.60807 (13)	0.53188 (6)	0.36106 (5)	0.0176 (2)
Br2	0.45375 (13)	0.65869 (5)	0.17413 (5)	0.0179 (2)
Br3	−0.08678 (13)	0.53698 (6)	0.14634 (5)	0.0177 (2)
Br4	0.14362 (13)	0.64469 (6)	0.35535 (5)	0.0187 (2)
O1	1.0537 (13)	1.1873 (5)	0.1974 (5)	0.047 (2)
H1D	1.156 (11)	1.184 (8)	0.229 (7)	0.071*
O2	1.3530 (11)	1.1631 (4)	0.2822 (4)	0.041 (2)
O3	−0.2057 (10)	0.0872 (4)	0.5199 (5)	0.0393 (19)
O4	−0.4688 (11)	0.1715 (4)	0.5194 (4)	0.0326 (18)
H4D	−0.398 (13)	0.133 (5)	0.524 (7)	0.049*
O5	0.7676 (10)	0.1848 (4)	−0.0443 (4)	0.0276 (16)
H5D	0.661 (8)	0.151 (6)	−0.054 (7)	0.041*
O6	0.4521 (11)	0.1011 (4)	−0.0559 (5)	0.042 (2)
N1	0.8823 (11)	0.7761 (4)	0.2520 (5)	0.0215 (18)
N2	0.1016 (11)	0.4196 (4)	0.3242 (4)	0.0189 (17)
N3	0.3468 (10)	0.4274 (4)	0.1689 (4)	0.0149 (16)
C1	0.7914 (18)	1.0759 (6)	0.1580 (8)	0.053 (4)
H1A	0.7006	1.1040	0.1847	0.079*
H1B	0.7572	1.0124	0.1586	0.079*
H1C	0.7866	1.0937	0.1015	0.079*
C2	0.9908 (17)	1.1032 (6)	0.2025 (6)	0.037 (3)
C3	1.0967 (16)	1.0481 (6)	0.2453 (6)	0.030 (2)
C4	1.2892 (16)	1.0843 (6)	0.2844 (6)	0.029 (2)
C5	1.4084 (15)	1.0280 (6)	0.3344 (6)	0.038 (3)
H5A	1.4370	0.9813	0.2994	0.056*
H5B	1.3379	1.0023	0.3770	0.056*
H5C	1.5286	1.0633	0.3596	0.056*
C6	1.0238 (14)	0.9527 (5)	0.2482 (5)	0.0212 (18)
C7	1.1014 (16)	0.8911 (6)	0.2087 (6)	0.034 (3)
H7	1.2034	0.9084	0.1784	0.040*
C8	1.0298 (16)	0.8030 (6)	0.2134 (6)	0.032 (2)
H8	1.0889	0.7608	0.1880	0.038*
C9	0.8082 (14)	0.8368 (6)	0.2889 (7)	0.033 (2)
H9	0.7025	0.8183	0.3169	0.039*
C10	0.8731 (14)	0.9235 (6)	0.2895 (7)	0.031 (2)
H10	0.8153	0.9637	0.3181	0.037*
C11	0.0715 (15)	0.1332 (7)	0.4622 (8)	0.043 (3)
H11A	0.1703	0.1630	0.5048	0.064*
H11B	0.0929	0.1565	0.4093	0.064*
H11C	0.0782	0.0705	0.4610	0.064*
C12	−0.1170 (16)	0.1471 (6)	0.4795 (7)	0.033 (3)
C13	−0.1977 (14)	0.2205 (5)	0.4578 (5)	0.022 (2)
C14	−0.3749 (14)	0.2287 (6)	0.4788 (6)	0.022 (2)
C15	−0.4769 (13)	0.3058 (5)	0.4583 (6)	0.022 (2)
H15A	−0.5735	0.2905	0.4102	0.033*
H15B	−0.3837	0.3556	0.4471	0.033*
H15C	−0.5396	0.3211	0.5044	0.033*
C16	−0.0932 (13)	0.2901 (5)	0.4113 (5)	0.0155 (19)
C17	−0.1302 (14)	0.2923 (6)	0.3276 (5)	0.024 (2)
H17	−0.2247	0.2496	0.2976	0.029*
C18	−0.0297 (14)	0.3568 (6)	0.2879 (6)	0.028 (2)
H18	−0.0568	0.3560	0.2302	0.034*
C19	0.1390 (12)	0.4175 (6)	0.4061 (5)	0.018 (2)
H19	0.2369	0.4603	0.4341	0.022*
C20	0.0430 (13)	0.3568 (6)	0.4512 (5)	0.021 (2)
H20	0.0692	0.3603	0.5090	0.025*
C21	0.8654 (14)	0.3226 (6)	0.0267 (6)	0.026 (2)
H21A	0.9619	0.3053	0.0686	0.039*
H21B	0.8044	0.3683	0.0494	0.039*
H21C	0.9273	0.3448	−0.0195	0.039*
C22	0.7181 (14)	0.2459 (5)	−0.0012 (5)	0.019 (2)
C23	0.5285 (13)	0.2351 (5)	0.0194 (5)	0.0155 (19)
C24	0.3999 (15)	0.1602 (6)	−0.0107 (7)	0.033 (3)
C25A	0.187 (3)	0.159 (3)	−0.008 (3)	0.036 (10)*	0.40 (7)
H25A	0.1164	0.1021	−0.0281	0.053*	0.40 (7)
H25B	0.1417	0.2046	−0.0422	0.053*	0.40 (7)
H25C	0.1666	0.1703	0.0483	0.053*	0.40 (7)
C25B	0.205 (3)	0.1342 (17)	0.0178 (17)	0.029 (6)*	0.60 (7)
H25D	0.1050	0.1219	−0.0296	0.043*	0.60 (7)
H25E	0.1768	0.1821	0.0515	0.043*	0.60 (7)
H25F	0.2071	0.0820	0.0499	0.043*	0.60 (7)
C26	0.4665 (12)	0.3030 (6)	0.0703 (6)	0.018 (2)
C27	0.4847 (14)	0.2987 (6)	0.1546 (5)	0.023 (2)
H27	0.5378	0.2520	0.1804	0.028*
C28	0.4274 (14)	0.3606 (6)	0.2001 (6)	0.025 (2)
H28	0.4453	0.3564	0.2576	0.030*
C29	0.3335 (13)	0.4330 (6)	0.0888 (6)	0.020 (2)
H29	0.2820	0.4811	0.0651	0.024*
C30	0.3894 (13)	0.3737 (6)	0.0376 (5)	0.021 (2)
H30	0.3753	0.3811	−0.0194	0.025*

Atomic displacement parameters (Å²) top

	U¹¹	U²²	U³³	U¹²	U¹³	U²³
Cd1	0.0144 (3)	0.0157 (3)	0.0173 (3)	0.0039 (3)	0.0031 (2)	0.0010 (3)
Cd2	0.0145 (3)	0.0175 (3)	0.0135 (3)	0.0039 (3)	0.0033 (2)	0.0007 (3)
Br1	0.0146 (5)	0.0223 (4)	0.0152 (4)	0.0017 (4)	0.0007 (4)	0.0043 (4)
Br2	0.0155 (5)	0.0208 (4)	0.0181 (4)	0.0039 (4)	0.0034 (4)	0.0060 (4)
Br3	0.0165 (5)	0.0218 (4)	0.0153 (4)	0.0061 (4)	0.0005 (4)	−0.0011 (4)
Br4	0.0154 (5)	0.0246 (4)	0.0158 (5)	0.0043 (4)	0.0011 (4)	−0.0040 (4)
O1	0.071 (7)	0.018 (3)	0.047 (5)	0.006 (4)	−0.013 (4)	0.006 (3)
O2	0.063 (6)	0.018 (3)	0.034 (4)	−0.004 (3)	−0.008 (4)	0.003 (3)
O3	0.031 (5)	0.037 (4)	0.050 (5)	−0.002 (3)	0.011 (4)	0.021 (4)
O4	0.029 (4)	0.034 (4)	0.033 (4)	−0.003 (3)	0.004 (4)	0.015 (3)
O5	0.028 (4)	0.030 (4)	0.027 (4)	0.008 (3)	0.009 (3)	−0.009 (3)
O6	0.035 (5)	0.028 (4)	0.062 (6)	0.006 (3)	0.002 (4)	−0.026 (4)
N1	0.027 (5)	0.017 (3)	0.021 (4)	0.008 (3)	0.001 (4)	0.001 (3)
N2	0.018 (4)	0.022 (4)	0.015 (4)	−0.002 (3)	0.001 (3)	0.003 (3)
N3	0.019 (4)	0.014 (3)	0.015 (4)	0.002 (3)	0.010 (3)	0.004 (3)
C1	0.069 (9)	0.023 (5)	0.057 (8)	0.004 (6)	−0.023 (7)	0.011 (5)
C2	0.058 (8)	0.022 (5)	0.027 (6)	0.004 (5)	−0.006 (5)	−0.006 (4)
C3	0.035 (6)	0.027 (5)	0.028 (6)	0.002 (5)	0.004 (5)	0.005 (4)
C4	0.044 (7)	0.027 (5)	0.016 (5)	0.006 (5)	0.000 (5)	0.002 (4)
C5	0.037 (7)	0.035 (6)	0.037 (6)	−0.010 (5)	0.009 (5)	0.003 (5)
C6	0.030 (5)	0.014 (3)	0.020 (5)	0.011 (3)	−0.005 (4)	0.004 (3)
C7	0.051 (7)	0.018 (4)	0.035 (6)	−0.005 (4)	0.029 (5)	−0.004 (4)
C8	0.047 (7)	0.018 (3)	0.033 (6)	0.004 (5)	0.022 (5)	−0.001 (4)
C9	0.024 (6)	0.023 (4)	0.052 (7)	0.008 (4)	0.006 (5)	−0.005 (5)
C10	0.021 (5)	0.022 (4)	0.052 (7)	0.011 (4)	0.008 (4)	−0.012 (4)
C11	0.023 (6)	0.034 (6)	0.072 (9)	0.012 (5)	−0.002 (6)	0.012 (6)
C12	0.031 (6)	0.022 (5)	0.047 (7)	0.002 (4)	0.010 (5)	0.004 (5)
C13	0.034 (6)	0.018 (4)	0.014 (5)	0.007 (4)	0.000 (4)	0.001 (4)
C14	0.026 (6)	0.019 (4)	0.023 (5)	0.006 (4)	0.007 (4)	0.001 (4)
C15	0.023 (5)	0.021 (5)	0.020 (5)	−0.003 (4)	0.002 (4)	0.002 (4)
C16	0.022 (5)	0.007 (4)	0.018 (5)	0.005 (3)	0.002 (4)	0.000 (3)
C17	0.023 (6)	0.028 (5)	0.016 (5)	−0.009 (4)	−0.005 (4)	0.006 (4)
C18	0.033 (6)	0.036 (6)	0.011 (5)	−0.001 (5)	−0.004 (4)	0.001 (4)
C19	0.008 (4)	0.022 (4)	0.023 (5)	−0.006 (4)	0.004 (4)	−0.004 (4)
C20	0.025 (5)	0.028 (5)	0.009 (4)	0.001 (4)	0.005 (4)	0.002 (4)
C21	0.025 (6)	0.030 (5)	0.026 (5)	0.009 (4)	0.010 (4)	−0.004 (4)
C22	0.028 (6)	0.013 (4)	0.018 (5)	0.008 (4)	0.001 (4)	0.004 (4)
C23	0.024 (5)	0.009 (4)	0.016 (4)	0.007 (4)	0.007 (4)	0.001 (3)
C24	0.018 (6)	0.031 (5)	0.049 (7)	0.009 (4)	−0.004 (5)	−0.014 (5)
C26	0.004 (4)	0.024 (5)	0.025 (5)	0.003 (4)	0.000 (4)	−0.001 (4)
C27	0.033 (6)	0.022 (5)	0.014 (5)	0.012 (4)	−0.008 (4)	−0.001 (4)
C28	0.031 (6)	0.026 (5)	0.019 (5)	0.006 (4)	0.000 (4)	0.004 (4)
C29	0.016 (5)	0.019 (4)	0.025 (5)	0.009 (4)	0.001 (4)	0.000 (4)
C30	0.026 (6)	0.025 (5)	0.014 (5)	0.011 (4)	0.004 (4)	0.008 (4)

Geometric parameters (Å, º) top

Cd1—N1	2.315 (7)	C9—H9	0.9500
Cd1—Br1	2.6240 (11)	C10—H10	0.9500
Cd1—Br3ⁱ	2.6314 (11)	C11—C12	1.457 (14)
Cd1—Br2	2.7384 (12)	C11—H11A	0.9800
Cd1—Br4ⁱ	2.7512 (12)	C11—H11B	0.9800
Cd2—N3	2.345 (7)	C11—H11C	0.9800
Cd2—N2	2.349 (7)	C12—C13	1.383 (13)
Cd2—Br4	2.6858 (11)	C13—C14	1.378 (13)
Cd2—Br2	2.7124 (10)	C13—C16	1.507 (12)
Cd2—Br1	2.8461 (12)	C14—C15	1.512 (12)
Cd2—Br3	2.8562 (12)	C15—H15A	0.9800
Br3—Cd1ⁱⁱ	2.6314 (11)	C15—H15B	0.9800
Br4—Cd1ⁱⁱ	2.7512 (12)	C15—H15C	0.9800
O1—C2	1.323 (12)	C16—C17	1.379 (12)
O1—H1D	0.84 (2)	C16—C20	1.396 (12)
O2—C4	1.242 (11)	C17—C18	1.376 (12)
O3—C12	1.297 (11)	C17—H17	0.9500
O4—C14	1.289 (11)	C18—H18	0.9500
O4—H4D	0.84 (2)	C19—C20	1.376 (11)
O5—C22	1.296 (10)	C19—H19	0.9500
O5—H5D	0.85 (2)	C20—H20	0.9500
O6—C24	1.301 (11)	C21—C22	1.484 (12)
N1—C8	1.324 (12)	C21—H21A	0.9800
N1—C9	1.325 (11)	C21—H21B	0.9800
N2—C18	1.317 (11)	C21—H21C	0.9800
N2—C19	1.351 (11)	C22—C23	1.425 (12)
N3—C29	1.325 (11)	C23—C24	1.403 (12)
N3—C28	1.339 (11)	C23—C26	1.491 (11)
C1—C2	1.504 (15)	C24—C25A	1.520 (19)
C1—H1A	0.9800	C24—C25B	1.531 (16)
C1—H1B	0.9800	C25A—H25A	0.9800
C1—H1C	0.9800	C25A—H25B	0.9800
C2—C3	1.371 (14)	C25A—H25C	0.9800
C3—C4	1.458 (15)	C25B—H25D	0.9800
C3—C6	1.497 (11)	C25B—H25E	0.9800
C4—C5	1.495 (14)	C25B—H25F	0.9800
C5—H5A	0.9800	C26—C30	1.387 (12)
C5—H5B	0.9800	C26—C27	1.391 (12)
C5—H5C	0.9800	C27—C28	1.353 (12)
C6—C7	1.371 (12)	C27—H27	0.9500
C6—C10	1.378 (13)	C28—H28	0.9500
C7—C8	1.394 (12)	C29—C30	1.376 (12)
C7—H7	0.9500	C29—H29	0.9500
C8—H8	0.9500	C30—H30	0.9500
C9—C10	1.355 (12)

N1—Cd1—Br1	132.91 (18)	H11A—C11—H11B	109.5
N1—Cd1—Br3ⁱ	112.59 (18)	C12—C11—H11C	109.5
Br1—Cd1—Br3ⁱ	114.44 (3)	H11A—C11—H11C	109.5
N1—Cd1—Br2	83.7 (2)	H11B—C11—H11C	109.5
Br1—Cd1—Br2	91.20 (4)	O3—C12—C13	120.5 (10)
Br3ⁱ—Cd1—Br2	99.21 (4)	O3—C12—C11	115.9 (9)
N1—Cd1—Br4ⁱ	81.2 (2)	C13—C12—C11	123.6 (9)
Br1—Cd1—Br4ⁱ	95.13 (4)	C14—C13—C12	119.2 (9)
Br3ⁱ—Cd1—Br4ⁱ	91.55 (4)	C14—C13—C16	120.6 (8)
Br2—Cd1—Br4ⁱ	163.98 (3)	C12—C13—C16	120.2 (9)
N3—Cd2—N2	89.4 (2)	O4—C14—C13	123.0 (9)
N3—Cd2—Br4	176.55 (16)	O4—C14—C15	113.2 (8)
N2—Cd2—Br4	87.25 (18)	C13—C14—C15	123.8 (8)
N3—Cd2—Br2	88.95 (16)	C14—C15—H15A	109.5
N2—Cd2—Br2	177.7 (2)	C14—C15—H15B	109.5
Br4—Cd2—Br2	94.40 (3)	H15A—C15—H15B	109.5
N3—Cd2—Br1	89.62 (19)	C14—C15—H15C	109.5
N2—Cd2—Br1	91.23 (19)	H15A—C15—H15C	109.5
Br4—Cd2—Br1	91.39 (3)	H15B—C15—H15C	109.5
Br2—Cd2—Br1	87.13 (3)	C17—C16—C20	116.7 (8)
N3—Cd2—Br3	90.89 (19)	C17—C16—C13	121.9 (8)
N2—Cd2—Br3	90.18 (19)	C20—C16—C13	121.4 (8)
Br4—Cd2—Br3	88.19 (3)	C18—C17—C16	119.7 (8)
Br2—Cd2—Br3	91.47 (3)	C18—C17—H17	120.1
Br1—Cd2—Br3	178.51 (3)	C16—C17—H17	120.1
Cd1—Br1—Cd2	89.36 (3)	N2—C18—C17	124.6 (9)
Cd2—Br2—Cd1	89.86 (3)	N2—C18—H18	117.7
Cd1ⁱⁱ—Br3—Cd2	88.98 (3)	C17—C18—H18	117.7
Cd2—Br4—Cd1ⁱⁱ	90.13 (3)	N2—C19—C20	123.5 (8)
C2—O1—H1D	92 (9)	N2—C19—H19	118.2
C14—O4—H4D	102 (8)	C20—C19—H19	118.2
C22—O5—H5D	100 (7)	C19—C20—C16	119.4 (8)
C8—N1—C9	117.1 (8)	C19—C20—H20	120.3
C8—N1—Cd1	117.7 (6)	C16—C20—H20	120.3
C9—N1—Cd1	125.0 (6)	C22—C21—H21A	109.5
C18—N2—C19	116.0 (7)	C22—C21—H21B	109.5
C18—N2—Cd2	123.4 (6)	H21A—C21—H21B	109.5
C19—N2—Cd2	120.6 (5)	C22—C21—H21C	109.5
C29—N3—C28	115.9 (8)	H21A—C21—H21C	109.5
C29—N3—Cd2	123.3 (6)	H21B—C21—H21C	109.5
C28—N3—Cd2	120.6 (6)	O5—C22—C23	118.8 (8)
C2—C1—H1A	109.5	O5—C22—C21	117.7 (8)
C2—C1—H1B	109.5	C23—C22—C21	123.4 (8)
H1A—C1—H1B	109.5	C24—C23—C22	118.8 (8)
C2—C1—H1C	109.5	C24—C23—C26	120.6 (8)
H1A—C1—H1C	109.5	C22—C23—C26	120.6 (7)
H1B—C1—H1C	109.5	O6—C24—C23	121.0 (9)
O1—C2—C3	122.9 (10)	O6—C24—C25A	118.6 (13)
O1—C2—C1	112.7 (9)	C23—C24—C25A	118.6 (15)
C3—C2—C1	124.4 (9)	O6—C24—C25B	114.8 (10)
C2—C3—C4	117.7 (9)	C23—C24—C25B	123.4 (10)
C2—C3—C6	121.6 (10)	C24—C25A—H25A	109.5
C4—C3—C6	120.5 (9)	C24—C25A—H25B	109.5
O2—C4—C3	121.5 (10)	H25A—C25A—H25B	109.5
O2—C4—C5	118.2 (10)	C24—C25A—H25C	109.5
C3—C4—C5	120.0 (9)	H25A—C25A—H25C	109.5
C4—C5—H5A	109.5	H25B—C25A—H25C	109.5
C4—C5—H5B	109.5	C24—C25B—H25D	109.5
H5A—C5—H5B	109.5	C24—C25B—H25E	109.5
C4—C5—H5C	109.5	H25D—C25B—H25E	109.5
H5A—C5—H5C	109.5	C24—C25B—H25F	109.5
H5B—C5—H5C	109.5	H25D—C25B—H25F	109.5
C7—C6—C10	117.2 (8)	H25E—C25B—H25F	109.5
C7—C6—C3	121.6 (9)	C30—C26—C27	116.1 (8)
C10—C6—C3	121.2 (8)	C30—C26—C23	122.9 (8)
C6—C7—C8	119.7 (9)	C27—C26—C23	120.9 (8)
C6—C7—H7	120.1	C28—C27—C26	120.4 (9)
C8—C7—H7	120.1	C28—C27—H27	119.8
N1—C8—C7	122.2 (9)	C26—C27—H27	119.8
N1—C8—H8	118.9	N3—C28—C27	123.8 (9)
C7—C8—H8	118.9	N3—C28—H28	118.1
N1—C9—C10	124.3 (10)	C27—C28—H28	118.1
N1—C9—H9	117.8	N3—C29—C30	124.4 (8)
C10—C9—H9	117.8	N3—C29—H29	117.8
C9—C10—C6	119.4 (8)	C30—C29—H29	117.8
C9—C10—H10	120.3	C29—C30—C26	119.3 (8)
C6—C10—H10	120.3	C29—C30—H30	120.4
C12—C11—H11A	109.5	C26—C30—H30	120.4
C12—C11—H11B	109.5

Symmetry codes: (i) x+1, y, z; (ii) x−1, y, z.

(3a) top

Crystal data top

C₁₀H₁₁CdI₂NO₂	D_x = 2.573 Mg m⁻³
M_r = 543.41	Mo Kα radiation, λ = 0.71073 Å
Orthorhombic, Pbca	Cell parameters from 7521 reflections
a = 7.1002 (9) Å	θ = 2.8–28.3°
b = 14.3490 (18) Å	µ = 5.94 mm⁻¹
c = 27.540 (4) Å	T = 100 K
V = 2805.7 (6) Å³	Rod, colorless
Z = 8	0.27 × 0.07 × 0.03 mm
F(000) = 1984

Data collection top

CCD area detector diffractometer	3748 reflections with I > 2σ(I)
Radiation source: Incoatec microsource, multilayer optics	R_int = 0.047
ωs scans	θ_max = 30.9°, θ_min = 2.8°
Absorption correction: multi-scan SADABS	h = −9→9
T_min = 0.474, T_max = 0.746	k = −20→20
39565 measured reflections	l = −38→37
4234 independent reflections

Refinement top

Refinement on F²	Primary atom site location: heavy-atom method
Least-squares matrix: full	Hydrogen site location: mixed
R[F² > 2σ(F²)] = 0.024	H-atom parameters constrained
wR(F²) = 0.051	w = 1/[σ²(F_o²) + (0.0191P)² + 2.0764P] where P = (F_o² + 2F_c²)/3
S = 1.11	(Δ/σ)_max = 0.001
4234 reflections	Δρ_max = 0.69 e Å⁻³
147 parameters	Δρ_min = −0.59 e Å⁻³
0 restraints

Crystal data top

C₁₀H₁₁CdI₂NO₂	V = 2805.7 (6) Å³
M_r = 543.41	Z = 8
Orthorhombic, Pbca	Mo Kα radiation
a = 7.1002 (9) Å	µ = 5.94 mm⁻¹
b = 14.3490 (18) Å	T = 100 K
c = 27.540 (4) Å	0.27 × 0.07 × 0.03 mm

Data collection top

CCD area detector diffractometer	4234 independent reflections
Absorption correction: multi-scan SADABS	3748 reflections with I > 2σ(I)
T_min = 0.474, T_max = 0.746	R_int = 0.047
39565 measured reflections

Refinement top

R[F² > 2σ(F²)] = 0.024	0 restraints
wR(F²) = 0.051	H-atom parameters constrained
S = 1.11	Δρ_max = 0.69 e Å⁻³
4234 reflections	Δρ_min = −0.59 e Å⁻³
147 parameters

Special details top

Fractional atomic coordinates and isotropic or equivalent isotropic displacement parameters (Å²) top

	x	y	z	U_iso*/U_eq
Cd1	0.69629 (3)	0.49466 (2)	0.21095 (2)	0.01580 (5)
I1	0.57192 (2)	0.44443 (2)	0.30413 (2)	0.01675 (5)
I2	0.55761 (3)	0.66218 (2)	0.18766 (2)	0.02204 (5)
O1	−0.0032 (3)	0.14714 (17)	0.02937 (8)	0.0315 (5)
O2	0.2705 (4)	0.04421 (15)	0.03192 (8)	0.0288 (5)
H2A	0.1606	0.0785	0.0273	0.035*
N1	0.5538 (3)	0.38827 (16)	0.16261 (9)	0.0171 (5)
C1	−0.0167 (5)	0.2973 (2)	0.06472 (12)	0.0292 (7)
H1A	−0.0018	0.3130	0.0991	0.044*
H1B	−0.1508	0.2896	0.0573	0.044*
H1C	0.0357	0.3475	0.0447	0.044*
C2	0.0851 (4)	0.2083 (2)	0.05408 (11)	0.0237 (6)
C3	0.2730 (4)	0.1909 (2)	0.07071 (10)	0.0204 (6)
C4	0.3580 (5)	0.1074 (2)	0.05812 (10)	0.0220 (6)
C5	0.5572 (5)	0.0814 (2)	0.07039 (12)	0.0267 (7)
H5A	0.6217	0.1353	0.0845	0.040*
H5B	0.6230	0.0618	0.0408	0.040*
H5C	0.5569	0.0300	0.0938	0.040*
C6	0.3708 (4)	0.25965 (19)	0.10214 (10)	0.0164 (5)
C7	0.4242 (4)	0.23656 (19)	0.14947 (10)	0.0166 (5)
H7	0.3983	0.1762	0.1620	0.020*
C8	0.5147 (4)	0.30172 (19)	0.17803 (10)	0.0166 (5)
H8	0.5509	0.2845	0.2100	0.020*
C9	0.5022 (4)	0.4111 (2)	0.11701 (10)	0.0189 (6)
H9	0.5287	0.4723	0.1057	0.023*
C10	0.4126 (4)	0.3497 (2)	0.08606 (10)	0.0196 (6)
H10	0.3796	0.3686	0.0541	0.024*

Atomic displacement parameters (Å²) top

	U¹¹	U²²	U³³	U¹²	U¹³	U²³
Cd1	0.01426 (10)	0.01552 (10)	0.01762 (10)	0.00023 (7)	0.00036 (7)	−0.00089 (7)
I1	0.01327 (9)	0.02015 (9)	0.01684 (9)	0.00166 (7)	−0.00018 (7)	0.00260 (6)
I2	0.01971 (10)	0.01640 (9)	0.03001 (11)	0.00180 (7)	−0.00241 (8)	0.00231 (7)
O1	0.0297 (13)	0.0426 (14)	0.0223 (11)	−0.0082 (11)	−0.0041 (10)	−0.0091 (10)
O2	0.0389 (14)	0.0226 (11)	0.0248 (11)	−0.0087 (10)	0.0041 (10)	−0.0083 (9)
N1	0.0154 (12)	0.0163 (11)	0.0197 (11)	0.0020 (9)	0.0012 (9)	−0.0018 (9)
C1	0.0275 (17)	0.0362 (18)	0.0239 (16)	0.0031 (15)	−0.0097 (13)	0.0005 (13)
C2	0.0250 (16)	0.0302 (16)	0.0159 (13)	−0.0052 (13)	−0.0012 (12)	−0.0013 (12)
C3	0.0247 (15)	0.0214 (14)	0.0150 (13)	−0.0050 (12)	0.0009 (11)	−0.0020 (11)
C4	0.0297 (16)	0.0225 (14)	0.0139 (13)	−0.0064 (13)	0.0041 (12)	−0.0016 (11)
C5	0.0353 (19)	0.0216 (15)	0.0234 (15)	0.0016 (13)	0.0058 (14)	−0.0038 (12)
C6	0.0165 (13)	0.0166 (12)	0.0162 (13)	0.0005 (11)	0.0034 (10)	−0.0026 (10)
C7	0.0174 (13)	0.0140 (12)	0.0183 (13)	0.0015 (10)	0.0020 (11)	−0.0008 (10)
C8	0.0178 (14)	0.0162 (13)	0.0158 (12)	0.0030 (11)	−0.0013 (10)	−0.0005 (10)
C9	0.0193 (14)	0.0172 (13)	0.0201 (14)	−0.0012 (11)	0.0032 (11)	0.0001 (11)
C10	0.0244 (15)	0.0195 (14)	0.0150 (13)	−0.0020 (11)	0.0002 (11)	0.0003 (11)

Geometric parameters (Å, º) top

Cd1—N1	2.264 (2)	C3—C4	1.386 (4)
Cd1—I2	2.6756 (4)	C3—C6	1.484 (4)
Cd1—I1ⁱ	2.7938 (4)	C4—C5	1.502 (5)
Cd1—I1	2.8079 (4)	C5—H5A	0.9800
I1—Cd1ⁱⁱ	2.7938 (4)	C5—H5B	0.9800
O1—C2	1.275 (4)	C5—H5C	0.9800
O2—C4	1.315 (4)	C6—C7	1.397 (4)
O2—H2A	0.9311	C6—C10	1.398 (4)
N1—C8	1.341 (4)	C7—C8	1.381 (4)
N1—C9	1.349 (4)	C7—H7	0.9500
C1—C2	1.496 (5)	C8—H8	0.9500
C1—H1A	0.9800	C9—C10	1.381 (4)
C1—H1B	0.9800	C9—H9	0.9500
C1—H1C	0.9800	C10—H10	0.9500
C2—C3	1.433 (4)

N1—Cd1—I2	107.48 (6)	O2—C4—C5	113.4 (3)
N1—Cd1—I1ⁱ	99.50 (6)	C3—C4—C5	124.7 (3)
I2—Cd1—I1ⁱ	123.193 (9)	C4—C5—H5A	109.5
N1—Cd1—I1	102.93 (6)	C4—C5—H5B	109.5
I2—Cd1—I1	109.508 (9)	H5A—C5—H5B	109.5
I1ⁱ—Cd1—I1	111.711 (9)	C4—C5—H5C	109.5
Cd1ⁱⁱ—I1—Cd1	95.629 (8)	H5A—C5—H5C	109.5
C4—O2—H2A	96.1	H5B—C5—H5C	109.5
C8—N1—C9	117.6 (2)	C7—C6—C10	117.2 (3)
C8—N1—Cd1	122.05 (19)	C7—C6—C3	120.9 (2)
C9—N1—Cd1	120.33 (19)	C10—C6—C3	121.9 (3)
C2—C1—H1A	109.5	C8—C7—C6	119.8 (3)
C2—C1—H1B	109.5	C8—C7—H7	120.1
H1A—C1—H1B	109.5	C6—C7—H7	120.1
C2—C1—H1C	109.5	N1—C8—C7	122.9 (3)
H1A—C1—H1C	109.5	N1—C8—H8	118.6
H1B—C1—H1C	109.5	C7—C8—H8	118.6
O1—C2—C3	120.6 (3)	N1—C9—C10	123.0 (3)
O1—C2—C1	117.0 (3)	N1—C9—H9	118.5
C3—C2—C1	122.4 (3)	C10—C9—H9	118.5
C4—C3—C2	118.4 (3)	C9—C10—C6	119.5 (3)
C4—C3—C6	121.1 (3)	C9—C10—H10	120.3
C2—C3—C6	120.4 (3)	C6—C10—H10	120.3
O2—C4—C3	121.9 (3)

Symmetry codes: (i) x+1/2, y, −z+1/2; (ii) x−1/2, y, −z+1/2.

(3b) top

Crystal data top

C₂₀H₂₂CdI₂N₂O₄	D_x = 2.031 Mg m⁻³
M_r = 720.59	Mo Kα radiation, λ = 0.71073 Å
Orthorhombic, Pca2₁	Cell parameters from 9971 reflections
a = 13.5307 (3) Å	θ = 3.0–27.5°
b = 7.0913 (7) Å	µ = 3.57 mm⁻¹
c = 49.110 (2) Å	T = 100 K
V = 4712.1 (5) Å³	Block, colorless
Z = 8	0.25 × 0.13 × 0.11 mm
F(000) = 2736

Data collection top

CCD area detector diffractometer	12009 reflections with I > 2σ(I)
Radiation source: Incoatec microsource	R_int = 0.051
ω scans	θ_max = 31.0°, θ_min = 0.8°
Absorption correction: multi-scan SADABS	h = −19→19
T_min = 0.522, T_max = 0.746	k = −9→10
67491 measured reflections	l = −69→69
14053 independent reflections

Refinement top

Refinement on F²	Hydrogen site location: mixed
Least-squares matrix: full	H atoms treated by a mixture of independent and constrained refinement
R[F² > 2σ(F²)] = 0.038	w = 1/[σ²(F_o²) + (0.0227P)² + 4.6056P] where P = (F_o² + 2F_c²)/3
wR(F²) = 0.076	(Δ/σ)_max = 0.003
S = 1.09	Δρ_max = 1.29 e Å⁻³
14053 reflections	Δρ_min = −1.11 e Å⁻³
545 parameters	Absolute structure: Refined as an inversion twin.
5 restraints	Absolute structure parameter: 0.41 (3)
Primary atom site location: heavy-atom method

Crystal data top

C₂₀H₂₂CdI₂N₂O₄	V = 4712.1 (5) Å³
M_r = 720.59	Z = 8
Orthorhombic, Pca2₁	Mo Kα radiation
a = 13.5307 (3) Å	µ = 3.57 mm⁻¹
b = 7.0913 (7) Å	T = 100 K
c = 49.110 (2) Å	0.25 × 0.13 × 0.11 mm

Data collection top

CCD area detector diffractometer	14053 independent reflections
Absorption correction: multi-scan SADABS	12009 reflections with I > 2σ(I)
T_min = 0.522, T_max = 0.746	R_int = 0.051
67491 measured reflections

Refinement top

R[F² > 2σ(F²)] = 0.038	H atoms treated by a mixture of independent and constrained refinement
wR(F²) = 0.076	Δρ_max = 1.29 e Å⁻³
S = 1.09	Δρ_min = −1.11 e Å⁻³
14053 reflections	Absolute structure: Refined as an inversion twin.
545 parameters	Absolute structure parameter: 0.41 (3)
5 restraints

Special details top

Refinement. Refined as a 2-component inversion twin.

Fractional atomic coordinates and isotropic or equivalent isotropic displacement parameters (Å²) top

	x	y	z	U_iso*/U_eq
Cd1	0.30627 (4)	0.36841 (8)	0.64474 (2)	0.02432 (12)
Cd2	0.28575 (4)	0.87015 (8)	0.89541 (2)	0.02364 (12)
I1	0.43978 (4)	0.55273 (8)	0.67561 (2)	0.03312 (13)
I2	0.17999 (4)	0.56014 (9)	0.61261 (2)	0.03726 (14)
I3	0.41806 (4)	1.05371 (8)	0.86404 (2)	0.03288 (13)
I4	0.15884 (4)	1.06226 (9)	0.92741 (2)	0.03673 (14)
O1	0.6759 (5)	−0.2054 (11)	0.52992 (16)	0.0421 (17)
H2D	0.611 (7)	−0.405 (14)	0.532 (2)	0.063*
O2	0.5705 (5)	−0.4815 (11)	0.53894 (16)	0.0404 (18)
O3	−0.0596 (4)	−0.3191 (10)	0.75141 (15)	0.0394 (17)
O4	0.0988 (5)	−0.4791 (9)	0.75788 (15)	0.0382 (16)
H4D	0.037 (2)	−0.468 (13)	0.7594 (19)	0.03 (3)*
O5	0.6556 (5)	0.2950 (11)	1.00989 (15)	0.0408 (17)
O6	0.5501 (6)	0.0203 (11)	1.00127 (16)	0.0434 (19)
H6D	0.597 (6)	0.086 (16)	1.007 (3)	0.065*
O7	0.0672 (5)	0.0308 (9)	0.78276 (16)	0.0328 (15)
O8	−0.0892 (4)	0.1927 (10)	0.79063 (15)	0.0359 (15)
H8D	−0.042 (5)	0.120 (12)	0.787 (2)	0.054*
N1	0.3794 (5)	0.1445 (9)	0.61770 (14)	0.0241 (14)
N2	0.2219 (4)	0.1639 (9)	0.67232 (15)	0.0217 (14)
N3	0.3581 (5)	0.6455 (10)	0.92216 (15)	0.0256 (15)
N4	0.2018 (4)	0.6680 (9)	0.86758 (16)	0.0222 (14)
C1	0.6432 (7)	0.1010 (14)	0.5479 (2)	0.038 (2)
H1A	0.5812	0.1698	0.5450	0.057*
H1B	0.6912	0.1380	0.5339	0.057*
H1C	0.6696	0.1311	0.5660	0.057*
C2	0.6240 (7)	−0.1082 (14)	0.5460 (2)	0.037 (2)
C3	0.5440 (6)	−0.1901 (13)	0.56074 (18)	0.0281 (18)
C4	0.5199 (7)	−0.3763 (14)	0.55600 (19)	0.034 (2)
C5	0.4363 (7)	−0.4761 (15)	0.5697 (3)	0.044 (3)
H5A	0.3922	−0.5294	0.5559	0.067*
H5B	0.3995	−0.3866	0.5810	0.067*
H5C	0.4625	−0.5777	0.5811	0.067*
C6	0.4846 (6)	−0.0776 (12)	0.58078 (18)	0.0269 (18)
C7	0.3939 (7)	−0.0039 (16)	0.5746 (2)	0.040 (2)
H7	0.3650	−0.0290	0.5574	0.048*
C8	0.3441 (6)	0.1059 (16)	0.5931 (2)	0.036 (2)
H8	0.2816	0.1565	0.5881	0.043*
C9	0.4664 (7)	0.0725 (16)	0.6240 (2)	0.044 (3)
H9	0.4929	0.0999	0.6415	0.052*
C10	0.5207 (8)	−0.0394 (16)	0.60691 (19)	0.045 (3)
H10	0.5822	−0.0903	0.6127	0.054*
C11	−0.0823 (6)	−0.0549 (14)	0.7223 (2)	0.041 (2)
H11A	−0.0834	0.0565	0.7341	0.062*
H11B	−0.1496	−0.1036	0.7202	0.062*
H11C	−0.0557	−0.0204	0.7044	0.062*
C12	−0.0180 (5)	−0.2046 (12)	0.73495 (19)	0.0297 (19)
C13	0.0834 (5)	−0.2189 (11)	0.72850 (18)	0.0248 (17)
C14	0.1399 (6)	−0.3549 (11)	0.74132 (17)	0.0244 (16)
C15	0.2504 (6)	−0.3671 (12)	0.74015 (18)	0.0301 (17)
H15A	0.2739	−0.3127	0.7230	0.045*
H15B	0.2708	−0.4995	0.7412	0.045*
H15C	0.2789	−0.2971	0.7555	0.045*
C16	0.1296 (5)	−0.0851 (11)	0.70889 (16)	0.0208 (15)
C17	0.1676 (5)	−0.1466 (12)	0.68429 (18)	0.0249 (17)
H17	0.1625	−0.2759	0.6794	0.030*
C18	0.2130 (6)	−0.0205 (12)	0.66659 (17)	0.0264 (17)
H18	0.2387	−0.0664	0.6498	0.032*
C19	0.1833 (5)	0.2249 (12)	0.69609 (19)	0.0251 (17)
H19	0.1877	0.3557	0.7001	0.030*
C20	0.1378 (5)	0.1087 (11)	0.71490 (18)	0.0241 (16)
H20	0.1126	0.1583	0.7315	0.029*
C21	0.6219 (8)	0.5991 (14)	0.9920 (2)	0.040 (2)
H21A	0.6805	0.6298	1.0029	0.060*
H21B	0.5649	0.6691	0.9990	0.060*
H21C	0.6336	0.6340	0.9730	0.060*
C22	0.6020 (7)	0.3943 (13)	0.99381 (18)	0.033 (2)
C23	0.5232 (7)	0.3076 (14)	0.97888 (18)	0.0307 (19)
C24	0.4990 (7)	0.1203 (13)	0.98374 (19)	0.033 (2)
C25	0.4174 (7)	0.0185 (15)	0.9707 (2)	0.040 (2)
H25A	0.4234	0.0293	0.9509	0.060*
H25B	0.3544	0.0730	0.9766	0.060*
H25C	0.4200	−0.1147	0.9760	0.060*
C26	0.4647 (6)	0.4231 (12)	0.9592 (2)	0.0294 (19)
C27	0.5001 (8)	0.4609 (16)	0.9336 (2)	0.048 (3)
H27	0.5621	0.4112	0.9280	0.058*
C28	0.4453 (7)	0.5719 (17)	0.9157 (2)	0.042 (3)
H28	0.4715	0.5960	0.8981	0.051*
C29	0.3233 (7)	0.6063 (14)	0.94684 (19)	0.033 (2)
H29	0.2608	0.6568	0.9518	0.040*
C30	0.3725 (7)	0.4962 (18)	0.96585 (19)	0.041 (2)
H30	0.3437	0.4712	0.9831	0.049*
C31	0.2210 (5)	0.1418 (11)	0.7982 (2)	0.0302 (18)
H31A	0.2485	0.2437	0.7871	0.045*
H31B	0.2420	0.0198	0.7908	0.045*
H31C	0.2449	0.1543	0.8170	0.045*
C32	0.1109 (5)	0.1532 (11)	0.79793 (17)	0.0248 (16)
C33	0.0576 (5)	0.2933 (11)	0.81165 (18)	0.0204 (15)
C34	−0.0449 (6)	0.3086 (12)	0.80657 (18)	0.0265 (17)
C35	−0.1065 (6)	0.4602 (13)	0.8180 (2)	0.038 (2)
H35A	−0.1757	0.4390	0.8130	0.057*
H35B	−0.0846	0.5820	0.8108	0.057*
H35C	−0.1003	0.4605	0.8379	0.057*
C36	0.1069 (5)	0.4259 (11)	0.83073 (16)	0.0194 (15)
C37	0.1160 (5)	0.6178 (11)	0.82572 (17)	0.0216 (15)
H37	0.0900	0.6701	0.8094	0.026*
C38	0.1625 (5)	0.7324 (12)	0.84434 (17)	0.0225 (16)
H38	0.1669	0.8635	0.8405	0.027*
C39	0.1927 (6)	0.4820 (12)	0.87278 (19)	0.0277 (19)
H39	0.2197	0.4334	0.8892	0.033*
C40	0.1458 (5)	0.3598 (12)	0.85521 (18)	0.0236 (17)
H40	0.1399	0.2301	0.8598	0.028*

Atomic displacement parameters (Å²) top

	U¹¹	U²²	U³³	U¹²	U¹³	U²³
Cd1	0.0314 (3)	0.0157 (3)	0.0259 (3)	−0.0011 (2)	0.0030 (2)	0.0001 (3)
Cd2	0.0304 (3)	0.0157 (3)	0.0248 (3)	−0.0014 (2)	−0.0037 (2)	−0.0009 (3)
I1	0.0279 (2)	0.0268 (3)	0.0447 (4)	−0.00334 (19)	−0.0004 (2)	−0.0056 (3)
I2	0.0508 (3)	0.0254 (3)	0.0356 (4)	0.0062 (2)	−0.0060 (3)	0.0057 (3)
I3	0.0273 (2)	0.0267 (3)	0.0446 (4)	−0.00326 (19)	0.0006 (2)	0.0056 (3)
I4	0.0498 (3)	0.0259 (3)	0.0345 (3)	0.0060 (2)	0.0057 (3)	−0.0059 (3)
O1	0.059 (4)	0.037 (4)	0.030 (4)	0.007 (3)	0.019 (3)	0.005 (3)
O2	0.066 (5)	0.027 (4)	0.029 (4)	0.002 (3)	0.014 (3)	−0.006 (3)
O3	0.037 (3)	0.035 (4)	0.046 (4)	−0.017 (3)	0.015 (3)	−0.006 (3)
O4	0.043 (4)	0.030 (4)	0.042 (4)	−0.011 (3)	0.006 (3)	0.009 (3)
O5	0.060 (4)	0.034 (4)	0.029 (4)	0.005 (3)	−0.019 (3)	0.000 (3)
O6	0.080 (5)	0.025 (4)	0.025 (4)	0.006 (3)	−0.015 (3)	0.002 (3)
O7	0.044 (3)	0.021 (3)	0.034 (4)	−0.005 (3)	−0.006 (3)	−0.005 (3)
O8	0.024 (3)	0.036 (4)	0.048 (4)	−0.009 (2)	−0.010 (3)	0.000 (3)
N1	0.042 (4)	0.014 (3)	0.015 (3)	−0.005 (3)	0.002 (3)	0.002 (3)
N2	0.025 (3)	0.017 (3)	0.024 (4)	0.000 (2)	0.001 (2)	0.001 (3)
N3	0.032 (3)	0.021 (4)	0.024 (4)	0.003 (3)	−0.004 (3)	−0.001 (3)
N4	0.021 (3)	0.014 (3)	0.032 (4)	−0.002 (2)	−0.003 (2)	0.001 (3)
C1	0.046 (5)	0.029 (5)	0.038 (6)	−0.003 (4)	0.015 (4)	0.005 (4)
C2	0.051 (5)	0.034 (5)	0.025 (5)	−0.003 (4)	0.005 (4)	0.010 (4)
C3	0.044 (5)	0.019 (4)	0.021 (4)	−0.001 (3)	0.007 (3)	0.002 (3)
C4	0.056 (6)	0.029 (5)	0.017 (4)	−0.001 (4)	0.006 (4)	0.008 (4)
C5	0.067 (7)	0.024 (6)	0.042 (7)	−0.011 (4)	0.011 (5)	−0.005 (5)
C6	0.047 (5)	0.016 (4)	0.017 (4)	−0.002 (3)	0.004 (3)	0.005 (3)
C7	0.049 (5)	0.050 (7)	0.021 (5)	0.002 (5)	0.002 (4)	−0.010 (5)
C8	0.026 (4)	0.052 (7)	0.028 (5)	0.002 (4)	−0.003 (3)	−0.007 (5)
C9	0.046 (5)	0.051 (7)	0.034 (6)	0.021 (4)	−0.011 (4)	−0.021 (5)
C10	0.062 (6)	0.054 (7)	0.019 (5)	0.023 (5)	−0.006 (4)	−0.011 (4)
C11	0.021 (4)	0.039 (6)	0.063 (7)	−0.003 (4)	0.008 (4)	−0.008 (5)
C12	0.018 (4)	0.030 (5)	0.041 (5)	−0.012 (3)	0.002 (3)	−0.012 (4)
C13	0.026 (4)	0.017 (4)	0.031 (5)	−0.007 (3)	0.001 (3)	−0.006 (3)
C14	0.032 (4)	0.015 (4)	0.026 (4)	−0.005 (3)	0.003 (3)	0.000 (3)
C15	0.033 (4)	0.025 (4)	0.032 (4)	0.003 (3)	−0.002 (3)	0.005 (4)
C16	0.015 (3)	0.019 (4)	0.028 (4)	0.001 (3)	−0.002 (3)	0.001 (3)
C17	0.030 (4)	0.019 (4)	0.026 (4)	0.002 (3)	0.001 (3)	0.000 (3)
C18	0.039 (4)	0.021 (4)	0.020 (4)	−0.004 (3)	0.001 (3)	0.003 (3)
C19	0.020 (3)	0.019 (4)	0.037 (5)	−0.001 (3)	0.005 (3)	−0.004 (3)
C20	0.022 (3)	0.020 (4)	0.031 (4)	−0.003 (3)	0.002 (3)	−0.007 (3)
C21	0.056 (6)	0.028 (5)	0.037 (6)	−0.012 (4)	−0.015 (4)	−0.003 (4)
C22	0.052 (5)	0.025 (5)	0.021 (4)	0.009 (4)	−0.008 (4)	0.001 (4)
C23	0.048 (5)	0.027 (5)	0.017 (4)	0.000 (4)	−0.008 (3)	0.000 (3)
C24	0.056 (6)	0.022 (5)	0.020 (5)	0.002 (4)	−0.008 (4)	0.003 (4)
C25	0.065 (6)	0.024 (5)	0.031 (6)	−0.013 (4)	−0.008 (4)	0.002 (4)
C26	0.043 (5)	0.019 (5)	0.026 (5)	−0.001 (3)	−0.009 (4)	−0.003 (4)
C27	0.052 (6)	0.051 (7)	0.042 (6)	0.027 (5)	0.004 (5)	0.012 (5)
C28	0.055 (6)	0.055 (7)	0.017 (5)	0.018 (5)	0.006 (4)	0.006 (5)
C29	0.042 (5)	0.040 (6)	0.017 (4)	0.002 (4)	0.001 (3)	−0.004 (4)
C30	0.043 (5)	0.061 (7)	0.017 (4)	0.004 (5)	0.000 (3)	0.008 (5)
C31	0.025 (4)	0.022 (4)	0.043 (5)	0.005 (3)	0.003 (3)	−0.004 (4)
C32	0.030 (4)	0.017 (4)	0.028 (4)	−0.005 (3)	−0.003 (3)	0.004 (3)
C33	0.015 (3)	0.017 (4)	0.029 (4)	−0.004 (3)	−0.004 (3)	0.001 (3)
C34	0.028 (4)	0.021 (4)	0.031 (4)	−0.004 (3)	0.000 (3)	0.005 (3)
C35	0.018 (4)	0.032 (5)	0.064 (7)	0.001 (3)	0.007 (4)	−0.001 (5)
C36	0.013 (3)	0.019 (4)	0.026 (4)	0.001 (2)	0.002 (3)	0.002 (3)
C37	0.020 (3)	0.016 (4)	0.029 (4)	−0.001 (3)	−0.003 (3)	−0.001 (3)
C38	0.021 (3)	0.019 (4)	0.028 (4)	−0.002 (3)	−0.004 (3)	−0.001 (3)
C39	0.030 (4)	0.021 (4)	0.032 (5)	0.004 (3)	−0.004 (3)	0.009 (4)
C40	0.024 (4)	0.014 (4)	0.033 (5)	−0.004 (3)	−0.006 (3)	0.002 (3)

Geometric parameters (Å, º) top

Cd1—N2	2.289 (7)	C13—C14	1.382 (11)
Cd1—N1	2.294 (7)	C13—C16	1.489 (11)
Cd1—I2	2.6941 (9)	C14—C15	1.499 (11)
Cd1—I1	2.6962 (8)	C15—H15A	0.9800
Cd2—N4	2.283 (7)	C15—H15B	0.9800
Cd2—N3	2.285 (7)	C15—H15C	0.9800
Cd2—I3	2.6966 (8)	C16—C17	1.384 (11)
Cd2—I4	2.6973 (8)	C16—C20	1.410 (11)
O1—C2	1.260 (12)	C17—C18	1.391 (11)
O2—C4	1.314 (11)	C17—H17	0.9500
O2—H2D	0.84 (3)	C18—H18	0.9500
O3—C12	1.277 (11)	C19—C20	1.383 (12)
O4—C14	1.322 (10)	C19—H19	0.9500
O4—H4D	0.84 (3)	C20—H20	0.9500
O5—C22	1.282 (11)	C21—C22	1.480 (13)
O6—C24	1.313 (11)	C21—H21A	0.9800
O6—H6D	0.84 (3)	C21—H21B	0.9800
O7—C32	1.288 (10)	C21—H21C	0.9800
O8—C34	1.284 (11)	C22—C23	1.433 (12)
O8—H8D	0.85 (3)	C23—C24	1.389 (13)
N1—C9	1.320 (11)	C23—C26	1.494 (12)
N1—C8	1.328 (12)	C24—C25	1.465 (13)
N2—C18	1.343 (11)	C25—H25A	0.9800
N2—C19	1.350 (11)	C25—H25B	0.9800
N3—C28	1.329 (11)	C25—H25C	0.9800
N3—C29	1.330 (11)	C26—C27	1.374 (14)
N4—C38	1.339 (11)	C26—C30	1.389 (14)
N4—C39	1.349 (11)	C27—C28	1.393 (13)
C1—C2	1.509 (13)	C27—H27	0.9500
C1—H1A	0.9800	C28—H28	0.9500
C1—H1B	0.9800	C29—C30	1.387 (14)
C1—H1C	0.9800	C29—H29	0.9500
C2—C3	1.427 (12)	C30—H30	0.9500
C3—C4	1.380 (13)	C31—C32	1.492 (11)
C3—C6	1.500 (12)	C31—H31A	0.9800
C4—C5	1.493 (13)	C31—H31B	0.9800
C5—H5A	0.9800	C31—H31C	0.9800
C5—H5B	0.9800	C32—C33	1.400 (11)
C5—H5C	0.9800	C33—C34	1.414 (10)
C6—C7	1.369 (14)	C33—C36	1.486 (11)
C6—C10	1.400 (12)	C34—C35	1.472 (12)
C7—C8	1.373 (14)	C35—H35A	0.9800
C7—H7	0.9500	C35—H35B	0.9800
C8—H8	0.9500	C35—H35C	0.9800
C9—C10	1.370 (13)	C36—C37	1.389 (10)
C9—H9	0.9500	C36—C40	1.393 (11)
C10—H10	0.9500	C37—C38	1.376 (11)
C11—C12	1.506 (13)	C37—H37	0.9500
C11—H11A	0.9800	C38—H38	0.9500
C11—H11B	0.9800	C39—C40	1.378 (12)
C11—H11C	0.9800	C39—H39	0.9500
C12—C13	1.412 (10)	C40—H40	0.9500

N2—Cd1—N1	96.8 (2)	C17—C16—C13	121.3 (7)
N2—Cd1—I2	110.49 (15)	C20—C16—C13	121.2 (7)
N1—Cd1—I2	106.49 (18)	C16—C17—C18	120.5 (8)
N2—Cd1—I1	107.98 (17)	C16—C17—H17	119.8
N1—Cd1—I1	111.83 (17)	C18—C17—H17	119.8
I2—Cd1—I1	120.64 (3)	N2—C18—C17	122.3 (8)
N4—Cd2—N3	96.9 (2)	N2—C18—H18	118.8
N4—Cd2—I3	106.95 (18)	C17—C18—H18	118.8
N3—Cd2—I3	112.36 (17)	N2—C19—C20	124.0 (8)
N4—Cd2—I4	110.44 (16)	N2—C19—H19	118.0
N3—Cd2—I4	106.84 (18)	C20—C19—H19	118.0
I3—Cd2—I4	120.78 (3)	C19—C20—C16	118.4 (8)
C4—O2—H2D	104 (9)	C19—C20—H20	120.8
C14—O4—H4D	114 (6)	C16—C20—H20	120.8
C24—O6—H6D	109 (10)	C22—C21—H21A	109.5
C34—O8—H8D	100 (7)	C22—C21—H21B	109.5
C9—N1—C8	117.1 (8)	H21A—C21—H21B	109.5
C9—N1—Cd1	121.0 (6)	C22—C21—H21C	109.5
C8—N1—Cd1	120.9 (6)	H21A—C21—H21C	109.5
C18—N2—C19	117.3 (7)	H21B—C21—H21C	109.5
C18—N2—Cd1	122.5 (5)	O5—C22—C23	120.0 (9)
C19—N2—Cd1	120.1 (5)	O5—C22—C21	118.2 (9)
C28—N3—C29	116.8 (8)	C23—C22—C21	121.8 (8)
C28—N3—Cd2	121.1 (6)	C24—C23—C22	119.9 (8)
C29—N3—Cd2	121.2 (6)	C24—C23—C26	120.7 (8)
C38—N4—C39	117.3 (7)	C22—C23—C26	119.4 (8)
C38—N4—Cd2	119.6 (5)	O6—C24—C23	120.3 (9)
C39—N4—Cd2	123.1 (6)	O6—C24—C25	114.6 (9)
C2—C1—H1A	109.5	C23—C24—C25	125.0 (8)
C2—C1—H1B	109.5	C24—C25—H25A	109.5
H1A—C1—H1B	109.5	C24—C25—H25B	109.5
C2—C1—H1C	109.5	H25A—C25—H25B	109.5
H1A—C1—H1C	109.5	C24—C25—H25C	109.5
H1B—C1—H1C	109.5	H25A—C25—H25C	109.5
O1—C2—C3	121.2 (9)	H25B—C25—H25C	109.5
O1—C2—C1	118.8 (8)	C27—C26—C30	117.1 (8)
C3—C2—C1	119.9 (9)	C27—C26—C23	121.0 (8)
C4—C3—C2	118.9 (8)	C30—C26—C23	121.9 (9)
C4—C3—C6	119.5 (8)	C26—C27—C28	120.2 (9)
C2—C3—C6	121.6 (8)	C26—C27—H27	119.9
O2—C4—C3	121.8 (8)	C28—C27—H27	119.9
O2—C4—C5	114.3 (9)	N3—C28—C27	122.9 (9)
C3—C4—C5	123.8 (9)	N3—C28—H28	118.6
C4—C5—H5A	109.5	C27—C28—H28	118.6
C4—C5—H5B	109.5	N3—C29—C30	124.1 (9)
H5A—C5—H5B	109.5	N3—C29—H29	117.9
C4—C5—H5C	109.5	C30—C29—H29	117.9
H5A—C5—H5C	109.5	C29—C30—C26	118.9 (9)
H5B—C5—H5C	109.5	C29—C30—H30	120.6
C7—C6—C10	116.2 (8)	C26—C30—H30	120.6
C7—C6—C3	122.6 (8)	C32—C31—H31A	109.5
C10—C6—C3	121.2 (8)	C32—C31—H31B	109.5
C6—C7—C8	120.7 (9)	H31A—C31—H31B	109.5
C6—C7—H7	119.6	C32—C31—H31C	109.5
C8—C7—H7	119.6	H31A—C31—H31C	109.5
N1—C8—C7	122.8 (8)	H31B—C31—H31C	109.5
N1—C8—H8	118.6	O7—C32—C33	121.4 (7)
C7—C8—H8	118.6	O7—C32—C31	115.3 (7)
N1—C9—C10	123.9 (9)	C33—C32—C31	123.2 (7)
N1—C9—H9	118.1	C32—C33—C34	118.3 (7)
C10—C9—H9	118.1	C32—C33—C36	121.4 (6)
C9—C10—C6	119.2 (9)	C34—C33—C36	120.2 (7)
C9—C10—H10	120.4	O8—C34—C33	121.1 (8)
C6—C10—H10	120.4	O8—C34—C35	115.9 (7)
C12—C11—H11A	109.5	C33—C34—C35	123.0 (8)
C12—C11—H11B	109.5	C34—C35—H35A	109.5
H11A—C11—H11B	109.5	C34—C35—H35B	109.5
C12—C11—H11C	109.5	H35A—C35—H35B	109.5
H11A—C11—H11C	109.5	C34—C35—H35C	109.5
H11B—C11—H11C	109.5	H35A—C35—H35C	109.5
O3—C12—C13	121.7 (9)	H35B—C35—H35C	109.5
O3—C12—C11	117.0 (7)	C37—C36—C40	116.7 (7)
C13—C12—C11	121.3 (8)	C37—C36—C33	123.2 (7)
C14—C13—C12	119.0 (8)	C40—C36—C33	120.0 (7)
C14—C13—C16	120.4 (6)	C38—C37—C36	120.1 (8)
C12—C13—C16	120.5 (8)	C38—C37—H37	120.0
O4—C14—C13	120.8 (7)	C36—C37—H37	120.0
O4—C14—C15	113.9 (7)	N4—C38—C37	123.2 (8)
C13—C14—C15	125.1 (7)	N4—C38—H38	118.4
C14—C15—H15A	109.5	C37—C38—H38	118.4
C14—C15—H15B	109.5	N4—C39—C40	122.6 (8)
H15A—C15—H15B	109.5	N4—C39—H39	118.7
C14—C15—H15C	109.5	C40—C39—H39	118.7
H15A—C15—H15C	109.5	C39—C40—C36	120.1 (8)
H15B—C15—H15C	109.5	C39—C40—H40	119.9
C17—C16—C20	117.5 (7)	C36—C40—H40	119.9

(4) top

Crystal data top

C₆₀H₆₀CdCl₂Fe₂N₆O₁₂·6(CH₄O)·6(H₂O)	Z = 1
M_r = 1652.50	F(000) = 860
Triclinic, P1	D_x = 1.364 Mg m⁻³
a = 12.1351 (13) Å	Mo Kα radiation, λ = 0.71073 Å
b = 13.2343 (14) Å	Cell parameters from 4039 reflections
c = 13.8728 (15) Å	θ = 2.3–25.2°
α = 91.809 (2)°	µ = 0.76 mm⁻¹
β = 109.675 (2)°	T = 100 K
γ = 104.825 (2)°	Block, red
V = 2011.0 (4) Å³	0.25 × 0.23 × 0.08 mm

Data collection top

CCD area detector diffractometer	6746 reflections with I > 2σ(I)
Radiation source: Incoatec microsource	R_int = 0.050
ω scans	θ_max = 26.6°, θ_min = 2.1°
Absorption correction: multi-scan SADABS	h = −15→15
T_min = 0.640, T_max = 0.745	k = −16→16
24575 measured reflections	l = −17→17
8416 independent reflections

Refinement top

Refinement on F²	Primary atom site location: heavy-atom method
Least-squares matrix: full	Hydrogen site location: mixed
R[F² > 2σ(F²)] = 0.049	H-atom parameters constrained
wR(F²) = 0.130	w = 1/[σ²(F_o²) + (0.0498P)² + 4.8255P] where P = (F_o² + 2F_c²)/3
S = 1.04	(Δ/σ)_max = 0.001
8416 reflections	Δρ_max = 1.12 e Å⁻³
456 parameters	Δρ_min = −0.92 e Å⁻³
0 restraints

Crystal data top

C₆₀H₆₀CdCl₂Fe₂N₆O₁₂·6(CH₄O)·6(H₂O)	γ = 104.825 (2)°
M_r = 1652.50	V = 2011.0 (4) Å³
Triclinic, P1	Z = 1
a = 12.1351 (13) Å	Mo Kα radiation
b = 13.2343 (14) Å	µ = 0.76 mm⁻¹
c = 13.8728 (15) Å	T = 100 K
α = 91.809 (2)°	0.25 × 0.23 × 0.08 mm
β = 109.675 (2)°

Data collection top

CCD area detector diffractometer	8416 independent reflections
Absorption correction: multi-scan SADABS	6746 reflections with I > 2σ(I)
T_min = 0.640, T_max = 0.745	R_int = 0.050
24575 measured reflections

Refinement top

R[F² > 2σ(F²)] = 0.049	0 restraints
wR(F²) = 0.130	H-atom parameters constrained
S = 1.04	Δρ_max = 1.12 e Å⁻³
8416 reflections	Δρ_min = −0.92 e Å⁻³
456 parameters

Special details top

Fractional atomic coordinates and isotropic or equivalent isotropic displacement parameters (Å²) top

	x	y	z	U_iso*/U_eq
Cd1	0.5000	1.0000	0.0000	0.01625 (11)
Fe1	0.04526 (5)	0.39589 (4)	0.25295 (4)	0.01632 (13)
Cl1	0.66071 (9)	1.03831 (7)	0.18977 (7)	0.0242 (2)
O1	−0.1302 (2)	0.3878 (2)	0.20690 (19)	0.0203 (5)
O2	0.0389 (2)	0.3848 (2)	0.39246 (19)	0.0194 (5)
O3	0.0580 (2)	0.41432 (19)	0.11412 (18)	0.0179 (5)
O4	0.1003 (2)	0.55232 (19)	0.27828 (19)	0.0209 (6)
O5	−0.0013 (2)	0.24041 (19)	0.2114 (2)	0.0202 (5)
O6	0.2166 (2)	0.38829 (19)	0.30313 (19)	0.0202 (5)
N1	−0.4459 (3)	0.3006 (3)	0.5008 (3)	0.0297 (8)
N2	0.4054 (3)	0.8368 (2)	0.0417 (2)	0.0190 (6)
N3	0.3676 (3)	0.0662 (2)	0.0592 (2)	0.0202 (7)
C1	−0.3358 (4)	0.3574 (4)	0.1891 (3)	0.0301 (9)
H1A	−0.3399	0.3819	0.1224	0.045*
H1B	−0.3699	0.3997	0.2244	0.045*
H1C	−0.3830	0.2831	0.1780	0.045*
C2	−0.2051 (4)	0.3690 (3)	0.2544 (3)	0.0208 (8)
C3	−0.1727 (3)	0.3581 (3)	0.3599 (3)	0.0187 (7)
C4	−0.0521 (3)	0.3649 (3)	0.4234 (3)	0.0188 (8)
C5	−0.0220 (4)	0.3478 (3)	0.5346 (3)	0.0253 (8)
H5A	0.0665	0.3621	0.5681	0.038*
H5B	−0.0621	0.2747	0.5390	0.038*
H5C	−0.0508	0.3955	0.5694	0.038*
C6	−0.2693 (3)	0.3375 (3)	0.4073 (3)	0.0210 (8)
C7	−0.3505 (4)	0.2385 (3)	0.3943 (3)	0.0264 (9)
H7	−0.3475	0.1813	0.3531	0.032*
C8	−0.4360 (4)	0.2240 (3)	0.4421 (3)	0.0304 (9)
H8	−0.4907	0.1557	0.4324	0.037*
C9	−0.3676 (4)	0.3957 (3)	0.5136 (3)	0.0284 (9)
H9	−0.3725	0.4513	0.5556	0.034*
C10	−0.2797 (4)	0.4172 (3)	0.4689 (3)	0.0249 (8)
H10	−0.2263	0.4864	0.4801	0.030*
C11	0.1586 (4)	0.4620 (3)	−0.0029 (3)	0.0209 (8)
H11A	0.1041	0.3928	−0.0384	0.031*
H11B	0.2435	0.4603	0.0173	0.031*
H11C	0.1451	0.5155	−0.0494	0.031*
C12	0.1324 (3)	0.4885 (3)	0.0912 (3)	0.0163 (7)
C13	0.1878 (3)	0.5892 (3)	0.1493 (3)	0.0191 (8)
C14	0.1625 (3)	0.6173 (3)	0.2368 (3)	0.0200 (8)
C15	0.2056 (4)	0.7299 (3)	0.2846 (3)	0.0327 (10)
H15A	0.1835	0.7352	0.3459	0.049*
H15B	0.1671	0.7727	0.2346	0.049*
H15C	0.2945	0.7557	0.3044	0.049*
C16	0.2647 (3)	0.6728 (3)	0.1107 (3)	0.0189 (8)
C17	0.2112 (4)	0.7224 (3)	0.0283 (3)	0.0221 (8)
H17	0.1251	0.7019	−0.0055	0.027*
C18	0.2842 (4)	0.8022 (3)	−0.0045 (3)	0.0218 (8)
H18	0.2462	0.8336	−0.0625	0.026*
C19	0.4569 (4)	0.7887 (3)	0.1207 (3)	0.0224 (8)
H19	0.5432	0.8116	0.1537	0.027*
C20	0.3913 (4)	0.7069 (3)	0.1570 (3)	0.0220 (8)
H20	0.4323	0.6745	0.2128	0.026*
C21	−0.0097 (4)	0.0817 (3)	0.1240 (4)	0.0325 (10)
H21A	−0.0873	0.0591	0.1353	0.049*
H21B	0.0382	0.0323	0.1496	0.049*
H21C	−0.0256	0.0829	0.0500	0.049*
C22	0.0605 (4)	0.1903 (3)	0.1808 (3)	0.0203 (8)
C23	0.1848 (3)	0.2323 (3)	0.1958 (3)	0.0203 (8)
C24	0.2557 (3)	0.3292 (3)	0.2559 (3)	0.0200 (8)
C25	0.3877 (4)	0.3725 (3)	0.2671 (3)	0.0271 (9)
H25A	0.3926	0.4073	0.2068	0.041*
H25B	0.4254	0.3147	0.2723	0.041*
H25C	0.4308	0.4236	0.3297	0.041*
C26	0.2444 (4)	0.1708 (3)	0.1471 (3)	0.0216 (8)
C27	0.3045 (4)	0.1011 (3)	0.1989 (3)	0.0274 (9)
H27	0.3039	0.0876	0.2656	0.033*
C28	0.3647 (4)	0.0517 (3)	0.1535 (3)	0.0282 (9)
H28	0.4062	0.0051	0.1907	0.034*
C29	0.3046 (4)	0.1279 (3)	0.0069 (3)	0.0236 (8)
H29	0.3021	0.1359	−0.0616	0.028*
C30	0.2425 (4)	0.1812 (3)	0.0473 (3)	0.0254 (9)
H30	0.1987	0.2247	0.0070	0.031*
O7	0.5547 (3)	0.9488 (3)	0.3692 (2)	0.0441 (8)
H7D	0.5713	0.8912	0.3786	0.066*
H7E	0.5921	0.9728	0.3299	0.066*
O8	0.3377 (4)	0.9766 (3)	0.4157 (3)	0.0560 (10)
H8D	0.3583	0.9891	0.4837	0.084*
H8E	0.3892	0.9665	0.3877	0.084*
O9	0.0765 (6)	0.9115 (5)	0.3225 (5)	0.133 (3)
H9D	0.1535	0.9307	0.3500	0.199*
H9E	0.0234	0.9379	0.3297	0.199*
C31	0.7300 (6)	0.7744 (6)	0.4712 (5)	0.076 (2)
H31A	0.7890	0.8078	0.4397	0.114*
H31B	0.7406	0.7055	0.4887	0.114*
H31C	0.7433	0.8193	0.5340	0.114*
O10	0.6090 (3)	0.7609 (3)	0.3999 (2)	0.0360 (7)
H10D	0.5633	0.7402	0.4321	0.054*
O11	−0.0971 (6)	0.9975 (5)	0.3463 (5)	0.1045 (18)
H11D	−0.1606	1.0082	0.3052	0.157*
C32	−0.0730 (7)	1.0923 (6)	0.4115 (6)	0.086 (2)
H32A	−0.0059	1.0955	0.4763	0.130*
H32B	−0.1462	1.0932	0.4262	0.130*
H32C	−0.0502	1.1532	0.3767	0.130*
O12	−0.1019 (6)	0.7605 (5)	0.1721 (5)	0.117 (2)*
H12D	−0.0541	0.8153	0.2124	0.175*
C33	−0.1876 (9)	0.6941 (8)	0.2100 (8)	0.122 (3)*
H33A	−0.1542	0.6385	0.2425	0.183*
H33B	−0.2644	0.6622	0.1524	0.183*
H33C	−0.2028	0.7364	0.2609	0.183*

Atomic displacement parameters (Å²) top

	U¹¹	U²²	U³³	U¹²	U¹³	U²³
Cd1	0.0179 (2)	0.01283 (18)	0.0212 (2)	0.00305 (14)	0.01184 (16)	0.00333 (14)
Fe1	0.0181 (3)	0.0154 (3)	0.0187 (3)	0.0032 (2)	0.0118 (2)	0.0032 (2)
Cl1	0.0265 (5)	0.0221 (5)	0.0213 (4)	0.0026 (4)	0.0087 (4)	0.0027 (4)
O1	0.0227 (14)	0.0230 (13)	0.0205 (13)	0.0058 (11)	0.0144 (11)	0.0052 (10)
O2	0.0194 (13)	0.0215 (13)	0.0208 (13)	0.0044 (11)	0.0124 (11)	0.0038 (10)
O3	0.0181 (13)	0.0167 (12)	0.0184 (13)	0.0002 (10)	0.0095 (11)	0.0020 (10)
O4	0.0286 (15)	0.0190 (13)	0.0198 (13)	0.0051 (11)	0.0154 (12)	0.0041 (10)
O5	0.0206 (14)	0.0175 (12)	0.0261 (14)	0.0033 (10)	0.0144 (11)	0.0031 (10)
O6	0.0189 (13)	0.0201 (13)	0.0214 (13)	0.0033 (10)	0.0090 (11)	−0.0011 (10)
N1	0.0235 (18)	0.040 (2)	0.0255 (18)	0.0026 (16)	0.0135 (15)	0.0028 (15)
N2	0.0193 (16)	0.0148 (15)	0.0233 (16)	0.0000 (12)	0.0116 (13)	0.0027 (12)
N3	0.0221 (17)	0.0185 (15)	0.0248 (16)	0.0071 (13)	0.0132 (14)	0.0041 (13)
C1	0.023 (2)	0.047 (3)	0.025 (2)	0.0101 (19)	0.0139 (18)	0.0042 (18)
C2	0.022 (2)	0.0189 (18)	0.0249 (19)	0.0039 (15)	0.0145 (16)	0.0030 (15)
C3	0.0194 (19)	0.0171 (17)	0.0206 (18)	0.0019 (14)	0.0111 (15)	0.0008 (14)
C4	0.024 (2)	0.0151 (17)	0.0201 (18)	0.0016 (14)	0.0141 (16)	0.0005 (14)
C5	0.025 (2)	0.034 (2)	0.0206 (19)	0.0084 (17)	0.0135 (17)	0.0041 (16)
C6	0.0174 (19)	0.0259 (19)	0.0189 (18)	0.0022 (15)	0.0086 (15)	0.0000 (15)
C7	0.029 (2)	0.026 (2)	0.025 (2)	0.0000 (17)	0.0166 (18)	0.0000 (16)
C8	0.025 (2)	0.034 (2)	0.029 (2)	−0.0024 (18)	0.0131 (18)	0.0006 (18)
C9	0.024 (2)	0.038 (2)	0.023 (2)	0.0050 (18)	0.0131 (17)	−0.0036 (17)
C10	0.020 (2)	0.026 (2)	0.027 (2)	−0.0006 (16)	0.0124 (17)	−0.0023 (16)
C11	0.024 (2)	0.0192 (18)	0.0222 (19)	0.0047 (15)	0.0131 (16)	0.0037 (15)
C12	0.0150 (17)	0.0165 (17)	0.0194 (18)	0.0032 (14)	0.0093 (14)	0.0070 (14)
C13	0.0211 (19)	0.0169 (17)	0.0188 (18)	0.0009 (15)	0.0096 (15)	0.0046 (14)
C14	0.0206 (19)	0.0145 (17)	0.0227 (19)	−0.0004 (14)	0.0088 (16)	0.0018 (14)
C15	0.050 (3)	0.019 (2)	0.028 (2)	−0.0012 (19)	0.021 (2)	−0.0009 (16)
C16	0.024 (2)	0.0159 (17)	0.0179 (18)	−0.0003 (15)	0.0126 (16)	0.0003 (14)
C17	0.021 (2)	0.0205 (18)	0.0235 (19)	0.0008 (15)	0.0101 (16)	0.0033 (15)
C18	0.024 (2)	0.0194 (18)	0.0188 (18)	0.0015 (15)	0.0075 (16)	0.0030 (14)
C19	0.021 (2)	0.0188 (18)	0.028 (2)	0.0038 (15)	0.0105 (16)	0.0058 (15)
C20	0.022 (2)	0.0219 (19)	0.0217 (19)	0.0049 (15)	0.0077 (16)	0.0070 (15)
C21	0.030 (2)	0.023 (2)	0.046 (3)	0.0034 (18)	0.019 (2)	−0.0053 (18)
C22	0.024 (2)	0.0173 (18)	0.0226 (19)	0.0050 (15)	0.0119 (16)	0.0043 (14)
C23	0.023 (2)	0.0212 (18)	0.0224 (19)	0.0086 (15)	0.0125 (16)	0.0046 (15)
C24	0.0197 (19)	0.0216 (18)	0.0203 (18)	0.0067 (15)	0.0084 (15)	0.0054 (14)
C25	0.021 (2)	0.028 (2)	0.033 (2)	0.0065 (17)	0.0119 (18)	0.0035 (17)
C26	0.022 (2)	0.0198 (18)	0.026 (2)	0.0042 (15)	0.0133 (16)	0.0010 (15)
C27	0.035 (2)	0.032 (2)	0.023 (2)	0.0151 (18)	0.0145 (18)	0.0073 (16)
C28	0.037 (2)	0.033 (2)	0.026 (2)	0.0210 (19)	0.0170 (19)	0.0119 (17)
C29	0.028 (2)	0.025 (2)	0.0217 (19)	0.0095 (17)	0.0125 (17)	0.0064 (15)
C30	0.033 (2)	0.024 (2)	0.027 (2)	0.0132 (17)	0.0163 (18)	0.0078 (16)
O7	0.066 (2)	0.0371 (18)	0.0358 (18)	0.0145 (17)	0.0268 (17)	0.0089 (14)
O8	0.069 (3)	0.049 (2)	0.045 (2)	0.0092 (19)	0.020 (2)	0.0024 (17)
O9	0.096 (5)	0.122 (5)	0.166 (6)	0.045 (4)	0.022 (4)	−0.038 (5)
C31	0.058 (4)	0.106 (6)	0.079 (5)	0.031 (4)	0.036 (4)	0.027 (4)
O10	0.0265 (16)	0.0488 (19)	0.0375 (17)	0.0063 (14)	0.0196 (14)	0.0172 (15)
O11	0.108 (5)	0.107 (4)	0.108 (4)	0.052 (4)	0.034 (4)	0.020 (4)
C32	0.082 (5)	0.064 (4)	0.098 (6)	0.019 (4)	0.017 (4)	−0.018 (4)

Geometric parameters (Å, º) top

Cd1—N2ⁱ	2.361 (3)	C15—H15A	0.9800
Cd1—N2	2.361 (3)	C15—H15B	0.9800
Cd1—N3ⁱⁱ	2.363 (3)	C15—H15C	0.9800
Cd1—N3ⁱⁱⁱ	2.363 (3)	C16—C17	1.387 (5)
Cd1—Cl1ⁱ	2.6351 (9)	C16—C20	1.393 (5)
Cd1—Cl1	2.6351 (9)	C17—C18	1.390 (5)
Fe1—O2	1.971 (2)	C17—H17	0.9500
Fe1—O1	1.979 (3)	C18—H18	0.9500
Fe1—O4	1.986 (3)	C19—C20	1.386 (5)
Fe1—O6	1.989 (3)	C19—H19	0.9500
Fe1—O5	1.999 (3)	C20—H20	0.9500
Fe1—O3	2.001 (2)	C21—C22	1.505 (5)
O1—C2	1.274 (4)	C21—H21A	0.9800
O2—C4	1.284 (4)	C21—H21B	0.9800
O3—C12	1.281 (4)	C21—H21C	0.9800
O4—C14	1.278 (4)	C22—C23	1.406 (5)
O5—C22	1.279 (4)	C23—C24	1.402 (5)
O6—C24	1.277 (4)	C23—C26	1.495 (5)
N1—C9	1.334 (5)	C24—C25	1.508 (5)
N1—C8	1.334 (5)	C25—H25A	0.9800
N2—C18	1.336 (5)	C25—H25B	0.9800
N2—C19	1.336 (5)	C25—H25C	0.9800
N3—C29	1.327 (5)	C26—C30	1.389 (5)
N3—C28	1.340 (5)	C26—C27	1.391 (6)
N3—Cd1^iv	2.363 (3)	C27—C28	1.373 (6)
C1—C2	1.503 (6)	C27—H27	0.9500
C1—H1A	0.9800	C28—H28	0.9500
C1—H1B	0.9800	C29—C30	1.382 (5)
C1—H1C	0.9800	C29—H29	0.9500
C2—C3	1.404 (5)	C30—H30	0.9500
C3—C4	1.408 (5)	O7—H7D	0.8400
C3—C6	1.500 (5)	O7—H7E	0.8418
C4—C5	1.501 (5)	O8—H8D	0.8880
C5—H5A	0.9800	O8—H8E	0.8730
C5—H5B	0.9800	O9—H9D	0.8455
C5—H5C	0.9800	O9—H9E	0.8380
C6—C7	1.388 (5)	C31—O10	1.429 (7)
C6—C10	1.393 (5)	C31—H31A	0.9800
C7—C8	1.387 (6)	C31—H31B	0.9800
C7—H7	0.9500	C31—H31C	0.9800
C8—H8	0.9500	O10—H10D	0.8242
C9—C10	1.380 (5)	O11—C32	1.428 (8)
C9—H9	0.9500	O11—H11D	0.8400
C10—H10	0.9500	C32—H32A	0.9800
C11—C12	1.496 (5)	C32—H32B	0.9800
C11—H11A	0.9800	C32—H32C	0.9800
C11—H11B	0.9800	O12—C33	1.435 (10)
C11—H11C	0.9800	O12—H12D	0.8458
C12—C13	1.409 (5)	C33—H33A	0.9800
C13—C14	1.410 (5)	C33—H33B	0.9800
C13—C16	1.492 (5)	C33—H33C	0.9800
C14—C15	1.497 (5)

N2ⁱ—Cd1—N2	180.0	C12—C13—C14	122.1 (3)
N2ⁱ—Cd1—N3ⁱⁱ	85.20 (10)	C12—C13—C16	119.2 (3)
N2—Cd1—N3ⁱⁱ	94.80 (10)	C14—C13—C16	118.3 (3)
N2ⁱ—Cd1—N3ⁱⁱⁱ	94.80 (10)	O4—C14—C13	124.1 (3)
N2—Cd1—N3ⁱⁱⁱ	85.20 (10)	O4—C14—C15	115.9 (3)
N3ⁱⁱ—Cd1—N3ⁱⁱⁱ	180.0	C13—C14—C15	120.0 (3)
N2ⁱ—Cd1—Cl1ⁱ	87.95 (8)	C14—C15—H15A	109.5
N2—Cd1—Cl1ⁱ	92.05 (8)	C14—C15—H15B	109.5
N3ⁱⁱ—Cd1—Cl1ⁱ	89.60 (8)	H15A—C15—H15B	109.5
N3ⁱⁱⁱ—Cd1—Cl1ⁱ	90.40 (8)	C14—C15—H15C	109.5
N2ⁱ—Cd1—Cl1	92.05 (8)	H15A—C15—H15C	109.5
N2—Cd1—Cl1	87.95 (8)	H15B—C15—H15C	109.5
N3ⁱⁱ—Cd1—Cl1	90.40 (8)	C17—C16—C20	117.2 (3)
N3ⁱⁱⁱ—Cd1—Cl1	89.60 (8)	C17—C16—C13	120.5 (3)
Cl1ⁱ—Cd1—Cl1	180.0	C20—C16—C13	122.2 (3)
O2—Fe1—O1	86.53 (10)	C16—C17—C18	119.6 (4)
O2—Fe1—O4	92.33 (10)	C16—C17—H17	120.2
O1—Fe1—O4	94.13 (11)	C18—C17—H17	120.2
O2—Fe1—O6	90.75 (11)	N2—C18—C17	123.1 (4)
O1—Fe1—O6	173.81 (10)	N2—C18—H18	118.4
O4—Fe1—O6	91.54 (11)	C17—C18—H18	118.4
O2—Fe1—O5	95.20 (10)	N2—C19—C20	123.5 (4)
O1—Fe1—O5	88.89 (11)	N2—C19—H19	118.3
O4—Fe1—O5	172.05 (10)	C20—C19—H19	118.3
O6—Fe1—O5	85.82 (10)	C19—C20—C16	119.3 (3)
O2—Fe1—O3	177.07 (10)	C19—C20—H20	120.3
O1—Fe1—O3	94.87 (10)	C16—C20—H20	120.3
O4—Fe1—O3	85.01 (10)	C22—C21—H21A	109.5
O6—Fe1—O3	88.11 (10)	C22—C21—H21B	109.5
O5—Fe1—O3	87.41 (10)	H21A—C21—H21B	109.5
C2—O1—Fe1	131.1 (2)	C22—C21—H21C	109.5
C4—O2—Fe1	130.8 (2)	H21A—C21—H21C	109.5
C12—O3—Fe1	127.5 (2)	H21B—C21—H21C	109.5
C14—O4—Fe1	129.2 (2)	O5—C22—C23	123.7 (3)
C22—O5—Fe1	126.2 (2)	O5—C22—C21	115.3 (3)
C24—O6—Fe1	123.4 (2)	C23—C22—C21	120.9 (3)
C9—N1—C8	116.9 (3)	C24—C23—C22	122.5 (3)
C18—N2—C19	117.2 (3)	C24—C23—C26	118.5 (3)
C18—N2—Cd1	115.7 (2)	C22—C23—C26	119.0 (3)
C19—N2—Cd1	125.6 (2)	O6—C24—C23	124.8 (3)
C29—N3—C28	117.5 (3)	O6—C24—C25	114.7 (3)
C29—N3—Cd1^iv	122.3 (2)	C23—C24—C25	120.5 (3)
C28—N3—Cd1^iv	119.9 (3)	C24—C25—H25A	109.5
C2—C1—H1A	109.5	C24—C25—H25B	109.5
C2—C1—H1B	109.5	H25A—C25—H25B	109.5
H1A—C1—H1B	109.5	C24—C25—H25C	109.5
C2—C1—H1C	109.5	H25A—C25—H25C	109.5
H1A—C1—H1C	109.5	H25B—C25—H25C	109.5
H1B—C1—H1C	109.5	C30—C26—C27	116.7 (4)
O1—C2—C3	124.3 (4)	C30—C26—C23	121.2 (3)
O1—C2—C1	115.3 (3)	C27—C26—C23	122.1 (3)
C3—C2—C1	120.4 (3)	C28—C27—C26	120.0 (4)
C2—C3—C4	122.4 (3)	C28—C27—H27	120.0
C2—C3—C6	119.3 (3)	C26—C27—H27	120.0
C4—C3—C6	118.3 (3)	N3—C28—C27	122.9 (4)
O2—C4—C3	124.1 (3)	N3—C28—H28	118.5
O2—C4—C5	115.0 (3)	C27—C28—H28	118.5
C3—C4—C5	120.8 (3)	N3—C29—C30	123.1 (4)
C4—C5—H5A	109.5	N3—C29—H29	118.4
C4—C5—H5B	109.5	C30—C29—H29	118.4
H5A—C5—H5B	109.5	C29—C30—C26	119.6 (4)
C4—C5—H5C	109.5	C29—C30—H30	120.2
H5A—C5—H5C	109.5	C26—C30—H30	120.2
H5B—C5—H5C	109.5	H7D—O7—H7E	102.0
C7—C6—C10	116.8 (3)	H8D—O8—H8E	121.9
C7—C6—C3	122.0 (3)	H9D—O9—H9E	131.6
C10—C6—C3	121.2 (3)	O10—C31—H31A	109.5
C8—C7—C6	119.3 (4)	O10—C31—H31B	109.5
C8—C7—H7	120.4	H31A—C31—H31B	109.5
C6—C7—H7	120.4	O10—C31—H31C	109.5
N1—C8—C7	123.8 (4)	H31A—C31—H31C	109.5
N1—C8—H8	118.1	H31B—C31—H31C	109.5
C7—C8—H8	118.1	C31—O10—H10D	106.0
N1—C9—C10	123.2 (4)	C32—O11—H11D	90.8
N1—C9—H9	118.4	O11—C32—H32A	109.5
C10—C9—H9	118.4	O11—C32—H32B	109.5
C9—C10—C6	120.1 (4)	H32A—C32—H32B	109.5
C9—C10—H10	120.0	O11—C32—H32C	109.5
C6—C10—H10	120.0	H32A—C32—H32C	109.5
C12—C11—H11A	109.5	H32B—C32—H32C	109.5
C12—C11—H11B	109.5	C33—O12—H12D	115.7
H11A—C11—H11B	109.5	O12—C33—H33A	109.5
C12—C11—H11C	109.5	O12—C33—H33B	109.5
H11A—C11—H11C	109.5	H33A—C33—H33B	109.5
H11B—C11—H11C	109.5	O12—C33—H33C	109.5
O3—C12—C13	123.6 (3)	H33A—C33—H33C	109.5
O3—C12—C11	115.5 (3)	H33B—C33—H33C	109.5
C13—C12—C11	120.9 (3)

Fe1—O1—C2—C3	6.1 (5)	C12—C13—C16—C20	−107.6 (4)
Fe1—O1—C2—C1	−173.3 (3)	C14—C13—C16—C20	79.2 (5)
O1—C2—C3—C4	−1.4 (6)	C20—C16—C17—C18	0.2 (5)
C1—C2—C3—C4	177.9 (4)	C13—C16—C17—C18	178.1 (3)
O1—C2—C3—C6	179.1 (3)	C19—N2—C18—C17	2.4 (5)
C1—C2—C3—C6	−1.6 (5)	Cd1—N2—C18—C17	−164.3 (3)
Fe1—O2—C4—C3	−7.9 (5)	C16—C17—C18—N2	−2.1 (6)
Fe1—O2—C4—C5	171.6 (2)	C18—N2—C19—C20	−0.9 (6)
C2—C3—C4—O2	2.4 (6)	Cd1—N2—C19—C20	164.3 (3)
C6—C3—C4—O2	−178.1 (3)	N2—C19—C20—C16	−0.9 (6)
C2—C3—C4—C5	−177.1 (3)	C17—C16—C20—C19	1.2 (5)
C6—C3—C4—C5	2.4 (5)	C13—C16—C20—C19	−176.7 (3)
C2—C3—C6—C7	77.8 (5)	Fe1—O5—C22—C23	16.6 (5)
C4—C3—C6—C7	−101.7 (4)	Fe1—O5—C22—C21	−161.9 (3)
C2—C3—C6—C10	−103.7 (4)	O5—C22—C23—C24	7.2 (6)
C4—C3—C6—C10	76.8 (5)	C21—C22—C23—C24	−174.4 (4)
C10—C6—C7—C8	0.0 (6)	O5—C22—C23—C26	−173.7 (3)
C3—C6—C7—C8	178.6 (4)	C21—C22—C23—C26	4.8 (6)
C9—N1—C8—C7	−0.4 (6)	Fe1—O6—C24—C23	−30.7 (5)
C6—C7—C8—N1	0.2 (7)	Fe1—O6—C24—C25	148.1 (3)
C8—N1—C9—C10	0.5 (6)	C22—C23—C24—O6	0.6 (6)
N1—C9—C10—C6	−0.3 (7)	C26—C23—C24—O6	−178.6 (3)
C7—C6—C10—C9	0.1 (6)	C22—C23—C24—C25	−178.2 (4)
C3—C6—C10—C9	−178.5 (4)	C26—C23—C24—C25	2.6 (5)
Fe1—O3—C12—C13	−24.3 (5)	C24—C23—C26—C30	−93.1 (5)
Fe1—O3—C12—C11	155.5 (2)	C22—C23—C26—C30	87.7 (5)
O3—C12—C13—C14	−1.8 (6)	C24—C23—C26—C27	86.7 (5)
C11—C12—C13—C14	178.4 (4)	C22—C23—C26—C27	−92.5 (5)
O3—C12—C13—C16	−174.8 (3)	C30—C26—C27—C28	4.1 (6)
C11—C12—C13—C16	5.4 (5)	C23—C26—C27—C28	−175.7 (4)
Fe1—O4—C14—C13	11.4 (6)	C29—N3—C28—C27	−2.9 (6)
Fe1—O4—C14—C15	−170.8 (3)	Cd1^iv—N3—C28—C27	169.9 (3)
C12—C13—C14—O4	8.7 (6)	C26—C27—C28—N3	−0.9 (7)
C16—C13—C14—O4	−178.3 (4)	C28—N3—C29—C30	3.5 (6)
C12—C13—C14—C15	−169.1 (4)	Cd1^iv—N3—C29—C30	−169.2 (3)
C16—C13—C14—C15	4.0 (6)	N3—C29—C30—C26	−0.2 (6)
C12—C13—C16—C17	74.5 (5)	C27—C26—C30—C29	−3.6 (6)
C14—C13—C16—C17	−98.7 (4)	C23—C26—C30—C29	176.2 (4)

Symmetry codes: (i) −x+1, −y+2, −z; (ii) −x+1, −y+1, −z; (iii) x, y+1, z; (iv) x, y−1, z.

(5) top

Crystal data top

C₆₀H₆₀Br₂CdFe₂N₆O₁₂·0.24(C₂H₈O₂)·4.75(CH₄O)·6(H₂O)	Z = 1
M_r = 1716.66	F(000) = 882.1
Triclinic, P1	D_x = 1.385 Mg m⁻³
a = 12.2603 (15) Å	Mo Kα radiation, λ = 0.71073 Å
b = 13.3560 (16) Å	Cell parameters from 4766 reflections
c = 13.9326 (16) Å	θ = 2.3–24.8°
α = 92.055 (2)°	µ = 1.64 mm⁻¹
β = 109.196 (2)°	T = 100 K
γ = 105.345 (2)°	Plate, red
V = 2058.8 (4) Å³	0.36 × 0.10 × 0.03 mm

Data collection top

CCD area detector diffractometer	6555 reflections with I > 2σ(I)
Radiation source: Incoatec microsource	R_int = 0.052
ω scans	θ_max = 26.5°, θ_min = 2.1°
Absorption correction: multi-scan SADABS	h = −15→15
T_min = 0.595, T_max = 0.745	k = −16→16
24811 measured reflections	l = −17→17
8482 independent reflections

Refinement top

Refinement on F²	Primary atom site location: heavy-atom method
Least-squares matrix: full	Hydrogen site location: mixed
R[F² > 2σ(F²)] = 0.054	H-atom parameters constrained
wR(F²) = 0.157	w = 1/[σ²(F_o²) + (0.0753P)² + 3.957P] where P = (F_o² + 2F_c²)/3
S = 1.05	(Δ/σ)_max = 0.001
8482 reflections	Δρ_max = 1.30 e Å⁻³
441 parameters	Δρ_min = −1.05 e Å⁻³
2 restraints

Crystal data top

C₆₀H₆₀Br₂CdFe₂N₆O₁₂·0.24(C₂H₈O₂)·4.75(CH₄O)·6(H₂O)	γ = 105.345 (2)°
M_r = 1716.66	V = 2058.8 (4) Å³
Triclinic, P1	Z = 1
a = 12.2603 (15) Å	Mo Kα radiation
b = 13.3560 (16) Å	µ = 1.64 mm⁻¹
c = 13.9326 (16) Å	T = 100 K
α = 92.055 (2)°	0.36 × 0.10 × 0.03 mm
β = 109.196 (2)°

Data collection top

CCD area detector diffractometer	8482 independent reflections
Absorption correction: multi-scan SADABS	6555 reflections with I > 2σ(I)
T_min = 0.595, T_max = 0.745	R_int = 0.052
24811 measured reflections

Refinement top

R[F² > 2σ(F²)] = 0.054	2 restraints
wR(F²) = 0.157	H-atom parameters constrained
S = 1.05	Δρ_max = 1.30 e Å⁻³
8482 reflections	Δρ_min = −1.05 e Å⁻³
441 parameters

Special details top

Fractional atomic coordinates and isotropic or equivalent isotropic displacement parameters (Å²) top

	x	y	z	U_iso*/U_eq	Occ. (<1)
Cd1	0.5000	1.0000	0.0000	0.02037 (14)
Fe1	0.04644 (6)	0.39445 (5)	0.25163 (5)	0.01918 (17)
Br1	0.67335 (5)	1.03674 (4)	0.19520 (4)	0.02738 (15)
O1	−0.1281 (3)	0.3808 (3)	0.2063 (2)	0.0226 (7)
O2	0.0395 (3)	0.3827 (3)	0.3904 (2)	0.0228 (7)
O3	0.0586 (3)	0.4140 (2)	0.1132 (2)	0.0216 (7)
O4	0.0972 (3)	0.5497 (2)	0.2766 (2)	0.0250 (7)
O5	0.0059 (3)	0.2404 (2)	0.2101 (3)	0.0246 (7)
O6	0.2181 (3)	0.3927 (2)	0.3015 (2)	0.0231 (7)
N1	−0.4387 (4)	0.3016 (4)	0.5023 (3)	0.0393 (12)
N2	0.3981 (4)	0.8397 (3)	0.0426 (3)	0.0230 (9)
N3	0.3790 (4)	0.0749 (3)	0.0639 (3)	0.0252 (9)
C1	−0.3317 (5)	0.3468 (5)	0.1891 (4)	0.0339 (12)
H1A	−0.3357	0.3732	0.1237	0.051*
H1B	−0.3679	0.3852	0.2251	0.051*
H1C	−0.3761	0.2720	0.1762	0.051*
C2	−0.2028 (4)	0.3617 (4)	0.2537 (4)	0.0235 (10)
C3	−0.1699 (4)	0.3542 (3)	0.3593 (3)	0.0214 (10)
C4	−0.0503 (4)	0.3630 (4)	0.4215 (4)	0.0226 (10)
C5	−0.0197 (5)	0.3472 (4)	0.5333 (4)	0.0309 (12)
H5A	0.0672	0.3567	0.5645	0.046*
H5B	−0.0644	0.2761	0.5384	0.046*
H5C	−0.0421	0.3984	0.5693	0.046*
C6	−0.2645 (4)	0.3348 (4)	0.4075 (4)	0.0258 (11)
C7	−0.3468 (5)	0.2372 (4)	0.3954 (4)	0.0334 (12)
H7	−0.3451	0.1796	0.3543	0.040*
C8	−0.4317 (5)	0.2238 (5)	0.4435 (4)	0.0402 (15)
H8	−0.4872	0.1562	0.4342	0.048*
C9	−0.3592 (5)	0.3950 (5)	0.5148 (4)	0.0397 (14)
H9	−0.3623	0.4508	0.5571	0.048*
C10	−0.2718 (5)	0.4152 (4)	0.4695 (4)	0.0330 (12)
H10	−0.2173	0.4835	0.4806	0.040*
C11	0.1567 (5)	0.4653 (4)	−0.0050 (4)	0.0241 (10)
H11A	0.1039	0.3960	−0.0408	0.036*
H11B	0.2413	0.4657	0.0145	0.036*
H11C	0.1423	0.5184	−0.0504	0.036*
C12	0.1299 (4)	0.4893 (3)	0.0898 (3)	0.0190 (9)
C13	0.1834 (4)	0.5900 (4)	0.1477 (3)	0.0216 (10)
C14	0.1578 (4)	0.6155 (4)	0.2348 (4)	0.0246 (10)
C15	0.2015 (6)	0.7280 (4)	0.2848 (4)	0.0408 (15)
H15A	0.1852	0.7313	0.3490	0.061*
H15B	0.1592	0.7699	0.2384	0.061*
H15C	0.2886	0.7557	0.2995	0.061*
C16	0.2583 (4)	0.6752 (3)	0.1095 (3)	0.0225 (10)
C17	0.2049 (5)	0.7267 (4)	0.0313 (4)	0.0250 (10)
H17	0.1195	0.7069	−0.0006	0.030*
C18	0.2770 (4)	0.8075 (4)	−0.0001 (4)	0.0248 (10)
H18	0.2390	0.8417	−0.0543	0.030*
C19	0.4494 (5)	0.7889 (4)	0.1176 (4)	0.0270 (11)
H19	0.5349	0.8103	0.1484	0.032*
C20	0.3834 (5)	0.7066 (4)	0.1526 (4)	0.0275 (11)
H20	0.4236	0.6722	0.2055	0.033*
C21	0.0026 (5)	0.0846 (4)	0.1239 (5)	0.0399 (14)
H21A	−0.0715	0.0577	0.1394	0.060*
H21B	0.0540	0.0386	0.1455	0.060*
H21C	−0.0183	0.0869	0.0500	0.060*
C22	0.0696 (5)	0.1938 (4)	0.1809 (4)	0.0249 (10)
C23	0.1928 (4)	0.2383 (4)	0.1967 (4)	0.0249 (10)
C24	0.2608 (4)	0.3353 (4)	0.2569 (3)	0.0230 (10)
C25	0.3923 (5)	0.3802 (4)	0.2709 (4)	0.0336 (12)
H25A	0.3996	0.4012	0.2060	0.050*
H25B	0.4342	0.3271	0.2918	0.050*
H25C	0.4287	0.4415	0.3239	0.050*
C26	0.2552 (4)	0.1785 (4)	0.1502 (4)	0.0246 (10)
C27	0.3129 (5)	0.1106 (5)	0.2015 (4)	0.0358 (13)
H27	0.3108	0.0974	0.2676	0.043*
C28	0.3745 (5)	0.0611 (5)	0.1565 (4)	0.0362 (13)
H28	0.4150	0.0154	0.1939	0.043*
C29	0.3162 (6)	0.1363 (4)	0.0121 (4)	0.0378 (14)
H29	0.3133	0.1436	−0.0562	0.045*
C30	0.2559 (6)	0.1892 (5)	0.0522 (4)	0.0412 (15)
H30	0.2146	0.2332	0.0127	0.049*
O7	0.5522 (5)	0.9407 (4)	0.3744 (4)	0.0661 (15)
H7D	0.5688	0.8831	0.3838	0.099*
H7E	0.5896	0.9647	0.3350	0.099*
O8	0.3369 (5)	0.9792 (4)	0.4121 (4)	0.0744 (16)
H8D	0.3575	0.9917	0.4800	0.112*
H8E	0.3884	0.9691	0.3841	0.112*
O9	0.0948 (12)	0.9314 (10)	0.3331 (10)	0.207 (5)*
H9D	0.1718	0.9505	0.3607	0.310*
H9E	0.0417	0.9577	0.3403	0.310*
C31	0.7117 (13)	0.7387 (11)	0.4633 (11)	0.145 (5)*
H31A	0.7742	0.7715	0.4353	0.218*
H31B	0.7096	0.6654	0.4693	0.218*
H31C	0.7302	0.7762	0.5311	0.218*
O10	0.5971 (4)	0.7432 (4)	0.3964 (4)	0.0539 (12)*
H10D	0.5513	0.7225	0.4286	0.081*
O11	−0.071 (2)	1.0021 (19)	0.3528 (19)	0.136 (10)*	0.374 (14)
H11D	−0.1349	1.0129	0.3117	0.204*	0.374 (14)
C32	−0.041 (2)	1.0978 (19)	0.4101 (19)	0.077 (7)*	0.374 (14)
H32A	−0.0790	1.0905	0.4620	0.116*	0.374 (14)
H32B	−0.0681	1.1478	0.3652	0.116*	0.374 (14)
H32C	0.0473	1.1235	0.4440	0.116*	0.374 (14)
O12	−0.0824 (10)	0.7742 (9)	0.1722 (9)	0.168 (4)*
H12D	−0.0345	0.8290	0.2125	0.253*
C33	−0.1788 (15)	0.7116 (14)	0.2044 (14)	0.202 (8)*
H33A	−0.1624	0.6461	0.2247	0.304*
H33B	−0.2563	0.6957	0.1476	0.304*
H33C	−0.1824	0.7521	0.2628	0.304*
C34	0.502 (3)	0.491 (2)	−0.021 (2)	0.051 (8)*	0.240 (11)
H34A	0.5609	0.5496	0.0298	0.076*	0.240 (11)
H34B	0.4526	0.5185	−0.0786	0.076*	0.240 (11)
H34C	0.5449	0.4500	−0.0465	0.076*	0.240 (11)
O13	0.428 (3)	0.428 (3)	0.023 (3)	0.140 (15)*	0.240 (11)
H13D	0.4678	0.4164	0.0817	0.168*	0.240 (11)

Atomic displacement parameters (Å²) top

	U¹¹	U²²	U³³	U¹²	U¹³	U²³
Cd1	0.0238 (3)	0.0150 (2)	0.0258 (3)	0.00228 (18)	0.0163 (2)	−0.00085 (18)
Fe1	0.0224 (3)	0.0185 (3)	0.0188 (3)	0.0028 (3)	0.0128 (3)	−0.0008 (2)
Br1	0.0300 (3)	0.0234 (3)	0.0248 (3)	0.0009 (2)	0.0106 (2)	−0.00190 (19)
O1	0.0259 (17)	0.0261 (17)	0.0202 (16)	0.0075 (14)	0.0139 (14)	0.0032 (13)
O2	0.0218 (17)	0.0261 (17)	0.0229 (17)	0.0034 (14)	0.0140 (14)	−0.0006 (13)
O3	0.0231 (17)	0.0189 (16)	0.0201 (16)	0.0000 (13)	0.0097 (14)	−0.0038 (13)
O4	0.0362 (19)	0.0187 (16)	0.0243 (17)	0.0023 (14)	0.0210 (15)	−0.0011 (13)
O5	0.0282 (18)	0.0202 (16)	0.0297 (18)	0.0041 (14)	0.0185 (15)	0.0004 (14)
O6	0.0255 (17)	0.0230 (17)	0.0199 (16)	0.0046 (14)	0.0096 (14)	−0.0052 (13)
N1	0.026 (2)	0.057 (3)	0.029 (2)	−0.003 (2)	0.017 (2)	−0.012 (2)
N2	0.024 (2)	0.019 (2)	0.024 (2)	−0.0002 (16)	0.0116 (17)	−0.0027 (16)
N3	0.028 (2)	0.026 (2)	0.027 (2)	0.0107 (18)	0.0161 (18)	0.0014 (17)
C1	0.023 (3)	0.051 (3)	0.027 (3)	0.010 (2)	0.011 (2)	0.000 (2)
C2	0.026 (2)	0.018 (2)	0.028 (3)	0.0036 (19)	0.014 (2)	−0.0029 (19)
C3	0.026 (2)	0.018 (2)	0.021 (2)	0.0015 (19)	0.013 (2)	−0.0040 (18)
C4	0.030 (3)	0.018 (2)	0.022 (2)	0.0014 (19)	0.017 (2)	−0.0022 (18)
C5	0.033 (3)	0.042 (3)	0.022 (2)	0.009 (2)	0.016 (2)	0.002 (2)
C6	0.022 (2)	0.030 (3)	0.023 (2)	0.000 (2)	0.011 (2)	−0.004 (2)
C7	0.035 (3)	0.033 (3)	0.031 (3)	−0.002 (2)	0.020 (2)	−0.009 (2)
C8	0.031 (3)	0.046 (3)	0.031 (3)	−0.013 (3)	0.014 (2)	−0.006 (2)
C9	0.030 (3)	0.055 (4)	0.031 (3)	0.001 (3)	0.017 (2)	−0.015 (3)
C10	0.027 (3)	0.039 (3)	0.029 (3)	−0.001 (2)	0.015 (2)	−0.012 (2)
C11	0.031 (3)	0.020 (2)	0.021 (2)	0.003 (2)	0.014 (2)	−0.0019 (18)
C12	0.020 (2)	0.019 (2)	0.019 (2)	0.0033 (18)	0.0103 (19)	0.0018 (17)
C13	0.022 (2)	0.022 (2)	0.019 (2)	−0.0018 (19)	0.0112 (19)	0.0015 (18)
C14	0.030 (3)	0.019 (2)	0.024 (2)	0.000 (2)	0.014 (2)	−0.0031 (19)
C15	0.066 (4)	0.023 (3)	0.031 (3)	−0.004 (3)	0.028 (3)	−0.007 (2)
C16	0.026 (3)	0.017 (2)	0.022 (2)	−0.0015 (19)	0.012 (2)	−0.0043 (18)
C17	0.025 (2)	0.022 (2)	0.025 (2)	0.000 (2)	0.011 (2)	−0.0027 (19)
C18	0.028 (3)	0.024 (2)	0.021 (2)	0.002 (2)	0.011 (2)	0.0015 (19)
C19	0.026 (3)	0.023 (2)	0.030 (3)	−0.001 (2)	0.013 (2)	0.003 (2)
C20	0.026 (3)	0.027 (3)	0.024 (3)	0.002 (2)	0.007 (2)	0.004 (2)
C21	0.039 (3)	0.026 (3)	0.053 (4)	0.005 (2)	0.018 (3)	−0.011 (3)
C22	0.031 (3)	0.022 (2)	0.025 (2)	0.008 (2)	0.015 (2)	−0.0010 (19)
C23	0.030 (3)	0.028 (3)	0.025 (2)	0.011 (2)	0.018 (2)	0.004 (2)
C24	0.027 (3)	0.027 (2)	0.018 (2)	0.008 (2)	0.012 (2)	0.0037 (19)
C25	0.023 (3)	0.038 (3)	0.039 (3)	0.007 (2)	0.013 (2)	−0.002 (2)
C26	0.028 (3)	0.024 (2)	0.027 (2)	0.009 (2)	0.016 (2)	−0.0008 (19)
C27	0.045 (3)	0.053 (4)	0.030 (3)	0.032 (3)	0.025 (3)	0.014 (3)
C28	0.046 (3)	0.048 (3)	0.034 (3)	0.030 (3)	0.024 (3)	0.015 (3)
C29	0.063 (4)	0.043 (3)	0.028 (3)	0.030 (3)	0.030 (3)	0.012 (2)
C30	0.073 (4)	0.040 (3)	0.037 (3)	0.039 (3)	0.035 (3)	0.017 (3)
O7	0.113 (4)	0.040 (3)	0.054 (3)	0.009 (3)	0.052 (3)	0.006 (2)
O8	0.102 (4)	0.065 (3)	0.043 (3)	0.003 (3)	0.026 (3)	0.002 (2)

Geometric parameters (Å, º) top

Cd1—N3ⁱ	2.363 (4)	C15—H15C	0.9800
Cd1—N3ⁱⁱ	2.363 (4)	C16—C17	1.382 (7)
Cd1—N2	2.379 (4)	C16—C20	1.388 (7)
Cd1—N2ⁱⁱⁱ	2.379 (4)	C17—C18	1.386 (6)
Cd1—Br1	2.7759 (6)	C17—H17	0.9500
Cd1—Br1ⁱⁱⁱ	2.7759 (6)	C18—H18	0.9500
Fe1—O2	1.973 (3)	C19—C20	1.388 (6)
Fe1—O1	1.977 (3)	C19—H19	0.9500
Fe1—O4	1.982 (3)	C20—H20	0.9500
Fe1—O6	1.994 (3)	C21—C22	1.512 (7)
Fe1—O5	2.000 (3)	C21—H21A	0.9800
Fe1—O3	2.005 (3)	C21—H21B	0.9800
O1—C2	1.275 (5)	C21—H21C	0.9800
O2—C4	1.280 (5)	C22—C23	1.407 (7)
O3—C12	1.275 (5)	C23—C24	1.402 (7)
O4—C14	1.281 (5)	C23—C26	1.503 (6)
O5—C22	1.269 (6)	C24—C25	1.507 (7)
O6—C24	1.280 (6)	C25—H25A	0.9800
N1—C9	1.329 (7)	C25—H25B	0.9800
N1—C8	1.338 (7)	C25—H25C	0.9800
N2—C19	1.339 (6)	C26—C27	1.374 (7)
N2—C18	1.344 (6)	C26—C30	1.379 (7)
N3—C28	1.328 (6)	C27—C28	1.395 (7)
N3—C29	1.341 (7)	C27—H27	0.9500
N3—Cd1^iv	2.363 (4)	C28—H28	0.9500
C1—C2	1.494 (7)	C29—C30	1.371 (7)
C1—H1A	0.9800	C29—H29	0.9500
C1—H1B	0.9800	C30—H30	0.9500
C1—H1C	0.9800	O7—H7D	0.8501
C2—C3	1.407 (7)	O7—H7E	0.8447
C3—C4	1.407 (7)	O8—H8D	0.8926
C3—C6	1.493 (6)	O8—H8E	0.8787
C4—C5	1.514 (6)	O9—H9D	0.8545
C5—H5A	0.9800	O9—H9E	0.8478
C5—H5B	0.9800	C31—O10	1.426 (14)
C5—H5C	0.9800	C31—H31A	0.9800
C6—C7	1.386 (7)	C31—H31B	0.9800
C6—C10	1.393 (7)	C31—H31C	0.9800
C7—C8	1.391 (7)	O10—H10D	0.8272
C7—H7	0.9500	O11—C32	1.37 (3)
C8—H8	0.9500	O11—H11D	0.8530
C9—C10	1.387 (7)	C32—H32A	0.9800
C9—H9	0.9500	C32—H32B	0.9800
C10—H10	0.9500	C32—H32C	0.9800
C11—C12	1.506 (6)	O12—C33	1.467 (9)
C11—H11A	0.9800	O12—H12D	0.8492
C11—H11B	0.9800	C33—H33A	0.9800
C11—H11C	0.9800	C33—H33B	0.9800
C12—C13	1.413 (6)	C33—H33C	0.9800
C13—C14	1.402 (6)	C34—O13	1.387 (19)
C13—C16	1.494 (6)	C34—H34A	0.9800
C14—C15	1.511 (7)	C34—H34B	0.9800
C15—H15A	0.9800	C34—H34C	0.9800
C15—H15B	0.9800	O13—H13D	0.8400

N3ⁱ—Cd1—N3ⁱⁱ	180.00 (17)	O4—C14—C13	124.7 (4)
N3ⁱ—Cd1—N2	94.41 (14)	O4—C14—C15	115.6 (4)
N3ⁱⁱ—Cd1—N2	85.59 (14)	C13—C14—C15	119.7 (4)
N3ⁱ—Cd1—N2ⁱⁱⁱ	85.59 (14)	C14—C15—H15A	109.5
N3ⁱⁱ—Cd1—N2ⁱⁱⁱ	94.41 (14)	C14—C15—H15B	109.5
N2—Cd1—N2ⁱⁱⁱ	180.0	H15A—C15—H15B	109.5
N3ⁱ—Cd1—Br1	89.82 (10)	C14—C15—H15C	109.5
N3ⁱⁱ—Cd1—Br1	90.18 (10)	H15A—C15—H15C	109.5
N2—Cd1—Br1	88.49 (10)	H15B—C15—H15C	109.5
N2ⁱⁱⁱ—Cd1—Br1	91.51 (10)	C17—C16—C20	117.8 (4)
N3ⁱ—Cd1—Br1ⁱⁱⁱ	90.18 (10)	C17—C16—C13	121.0 (4)
N3ⁱⁱ—Cd1—Br1ⁱⁱⁱ	89.82 (10)	C20—C16—C13	121.2 (4)
N2—Cd1—Br1ⁱⁱⁱ	91.51 (10)	C16—C17—C18	119.4 (5)
N2ⁱⁱⁱ—Cd1—Br1ⁱⁱⁱ	88.49 (10)	C16—C17—H17	120.3
Br1—Cd1—Br1ⁱⁱⁱ	180.0	C18—C17—H17	120.3
O2—Fe1—O1	86.34 (13)	N2—C18—C17	123.1 (5)
O2—Fe1—O4	92.35 (13)	N2—C18—H18	118.5
O1—Fe1—O4	94.42 (14)	C17—C18—H18	118.5
O2—Fe1—O6	90.85 (13)	N2—C19—C20	123.1 (5)
O1—Fe1—O6	173.82 (14)	N2—C19—H19	118.4
O4—Fe1—O6	91.20 (14)	C20—C19—H19	118.4
O2—Fe1—O5	95.54 (13)	C19—C20—C16	119.3 (5)
O1—Fe1—O5	89.22 (14)	C19—C20—H20	120.4
O4—Fe1—O5	171.51 (13)	C16—C20—H20	120.4
O6—Fe1—O5	85.56 (13)	C22—C21—H21A	109.5
O2—Fe1—O3	177.07 (13)	C22—C21—H21B	109.5
O1—Fe1—O3	94.74 (13)	H21A—C21—H21B	109.5
O4—Fe1—O3	84.86 (13)	C22—C21—H21C	109.5
O6—Fe1—O3	88.33 (13)	H21A—C21—H21C	109.5
O5—Fe1—O3	87.20 (13)	H21B—C21—H21C	109.5
C2—O1—Fe1	131.6 (3)	O5—C22—C23	124.2 (4)
C4—O2—Fe1	130.9 (3)	O5—C22—C21	115.0 (4)
C12—O3—Fe1	127.7 (3)	C23—C22—C21	120.8 (4)
C14—O4—Fe1	129.0 (3)	C24—C23—C22	122.6 (4)
C22—O5—Fe1	126.5 (3)	C24—C23—C26	118.5 (4)
C24—O6—Fe1	124.6 (3)	C22—C23—C26	119.0 (4)
C9—N1—C8	117.2 (4)	O6—C24—C23	124.2 (4)
C19—N2—C18	117.2 (4)	O6—C24—C25	115.2 (4)
C19—N2—Cd1	124.8 (3)	C23—C24—C25	120.6 (4)
C18—N2—Cd1	116.9 (3)	C24—C25—H25A	109.5
C28—N3—C29	116.5 (4)	C24—C25—H25B	109.5
C28—N3—Cd1^iv	120.5 (3)	H25A—C25—H25B	109.5
C29—N3—Cd1^iv	122.9 (3)	C24—C25—H25C	109.5
C2—C1—H1A	109.5	H25A—C25—H25C	109.5
C2—C1—H1B	109.5	H25B—C25—H25C	109.5
H1A—C1—H1B	109.5	C27—C26—C30	116.9 (5)
C2—C1—H1C	109.5	C27—C26—C23	122.3 (4)
H1A—C1—H1C	109.5	C30—C26—C23	120.7 (5)
H1B—C1—H1C	109.5	C26—C27—C28	119.9 (5)
O1—C2—C3	123.9 (4)	C26—C27—H27	120.1
O1—C2—C1	115.4 (4)	C28—C27—H27	120.1
C3—C2—C1	120.6 (4)	N3—C28—C27	122.9 (5)
C2—C3—C4	122.2 (4)	N3—C28—H28	118.5
C2—C3—C6	119.4 (4)	C27—C28—H28	118.5
C4—C3—C6	118.4 (4)	N3—C29—C30	123.6 (5)
O2—C4—C3	124.6 (4)	N3—C29—H29	118.2
O2—C4—C5	114.7 (4)	C30—C29—H29	118.2
C3—C4—C5	120.7 (4)	C29—C30—C26	119.9 (5)
C4—C5—H5A	109.5	C29—C30—H30	120.0
C4—C5—H5B	109.5	C26—C30—H30	120.0
H5A—C5—H5B	109.5	H7D—O7—H7E	101.9
C4—C5—H5C	109.5	H8D—O8—H8E	121.4
H5A—C5—H5C	109.5	H9D—O9—H9E	132.0
H5B—C5—H5C	109.5	O10—C31—H31A	109.5
C7—C6—C10	116.8 (4)	O10—C31—H31B	109.5
C7—C6—C3	122.5 (4)	H31A—C31—H31B	109.5
C10—C6—C3	120.7 (4)	O10—C31—H31C	109.5
C6—C7—C8	119.8 (5)	H31A—C31—H31C	109.5
C6—C7—H7	120.1	H31B—C31—H31C	109.5
C8—C7—H7	120.1	C31—O10—H10D	104.0
N1—C8—C7	123.0 (5)	C32—O11—H11D	91.0
N1—C8—H8	118.5	O11—C32—H32A	109.5
C7—C8—H8	118.5	O11—C32—H32B	109.5
N1—C9—C10	123.4 (5)	H32A—C32—H32B	109.5
N1—C9—H9	118.3	O11—C32—H32C	109.5
C10—C9—H9	118.3	H32A—C32—H32C	109.5
C9—C10—C6	119.6 (5)	H32B—C32—H32C	109.5
C9—C10—H10	120.2	C33—O12—H12D	116.6
C6—C10—H10	120.2	O12—C33—H33A	110.1
C12—C11—H11A	109.5	O12—C33—H33B	109.5
C12—C11—H11B	109.5	H33A—C33—H33B	109.5
H11A—C11—H11B	109.5	O12—C33—H33C	108.8
C12—C11—H11C	109.5	H33A—C33—H33C	109.5
H11A—C11—H11C	109.5	H33B—C33—H33C	109.5
H11B—C11—H11C	109.5	O13—C34—H34A	109.5
O3—C12—C13	123.8 (4)	O13—C34—H34B	109.5
O3—C12—C11	115.9 (4)	H34A—C34—H34B	109.5
C13—C12—C11	120.2 (4)	O13—C34—H34C	109.5
C14—C13—C12	121.5 (4)	H34A—C34—H34C	109.5
C14—C13—C16	118.5 (4)	H34B—C34—H34C	109.5
C12—C13—C16	119.6 (4)	C34—O13—H13D	112.1

Symmetry codes: (i) −x+1, −y+1, −z; (ii) x, y+1, z; (iii) −x+1, −y+2, −z; (iv) x, y−1, z.

(6_squeeze) top

Crystal data top

C_64.09H_68.18Cd₃Cl_8.18Fe₂I₆N₆O₁₂	F(000) = 4975
M_r = 2614.57	D_x = 1.726 Mg m⁻³
Monoclinic, C2/c	Mo Kα radiation, λ = 0.71073 Å
a = 32.186 (3) Å	Cell parameters from 3756 reflections
b = 13.7863 (15) Å	θ = 2.4–19.7°
c = 27.721 (2) Å	µ = 3.01 mm⁻¹
β = 125.118 (8)°	T = 100 K
V = 10061.4 (18) Å³	Block, red
Z = 4	0.15 × 0.08 × 0.07 mm

Data collection top

CCD area detector diffractometer	3817 reflections with I > 2σ(I)
Radiation source: Incoatec microsource	R_int = 0.085
ω scans	θ_max = 22.0°, θ_min = 1.8°
Absorption correction: multi-scan SADABS	h = −33→33
T_min = 0.587, T_max = 0.745	k = −14→14
41442 measured reflections	l = −29→29
6166 independent reflections

Refinement top

Refinement on F²	Primary atom site location: heavy-atom method
Least-squares matrix: full	Hydrogen site location: inferred from neighbouring sites
R[F² > 2σ(F²)] = 0.066	H-atom parameters constrained
wR(F²) = 0.163	w = 1/[σ²(F_o²) + (0.0555P)²] where P = (F_o² + 2F_c²)/3
S = 0.95	(Δ/σ)_max = 0.001
6166 reflections	Δρ_max = 2.31 e Å⁻³
259 parameters	Δρ_min = −1.52 e Å⁻³
2 restraints

Crystal data top

C_64.09H_68.18Cd₃Cl_8.18Fe₂I₆N₆O₁₂	V = 10061.4 (18) Å³
M_r = 2614.57	Z = 4
Monoclinic, C2/c	Mo Kα radiation
a = 32.186 (3) Å	µ = 3.01 mm⁻¹
b = 13.7863 (15) Å	T = 100 K
c = 27.721 (2) Å	0.15 × 0.08 × 0.07 mm
β = 125.118 (8)°

Data collection top

CCD area detector diffractometer	6166 independent reflections
Absorption correction: multi-scan SADABS	3817 reflections with I > 2σ(I)
T_min = 0.587, T_max = 0.745	R_int = 0.085
41442 measured reflections	θ_max = 22.0°

Refinement top

R[F² > 2σ(F²)] = 0.066	2 restraints
wR(F²) = 0.163	H-atom parameters constrained
S = 0.95	Δρ_max = 2.31 e Å⁻³
6166 reflections	Δρ_min = −1.52 e Å⁻³
259 parameters

Special details top

Fractional atomic coordinates and isotropic or equivalent isotropic displacement parameters (Å²) top

	x	y	z	U_iso*/U_eq	Occ. (<1)
I1	0.81336 (5)	0.16305 (8)	0.18575 (6)	0.0648 (4)
I2	0.89618 (5)	0.36766 (9)	0.11898 (5)	0.0548 (4)
I3	0.41195 (4)	0.19416 (8)	0.16986 (5)	0.0445 (3)
Cd1	0.85709 (4)	0.32463 (8)	0.18033 (5)	0.0348 (3)
Cd2	0.5000	0.28300 (11)	0.2500	0.0322 (5)
Fe1	0.56602 (8)	0.74825 (14)	0.02682 (9)	0.0270 (6)
O1	0.6075 (3)	0.7195 (7)	−0.0035 (4)	0.031 (3)*
O2	0.6323 (4)	0.7596 (7)	0.1046 (4)	0.038 (3)*
O3	0.5634 (3)	0.6034 (6)	0.0322 (4)	0.026 (2)*
O4	0.5302 (3)	0.7505 (7)	0.0658 (4)	0.033 (3)*
O5	0.5019 (3)	0.7476 (7)	−0.0543 (4)	0.029 (3)*
O6	0.5645 (3)	0.8919 (6)	0.0185 (4)	0.023 (2)*
N1	0.7969 (4)	0.4404 (9)	0.1542 (5)	0.032 (3)*
N2	0.5136 (4)	0.3896 (8)	0.1977 (5)	0.026 (3)*
N3	0.4110 (4)	1.1032 (8)	−0.2309 (5)	0.025 (3)*
C1	0.6574 (6)	0.6183 (11)	−0.0164 (7)	0.046 (5)*
H1A	0.6417	0.5540	−0.0265	0.069*
H1B	0.6942	0.6115	0.0040	0.069*
H1C	0.6434	0.6563	−0.0525	0.069*
C2	0.6468 (5)	0.6686 (10)	0.0226 (6)	0.029 (4)*
C3	0.6779 (5)	0.6536 (10)	0.0825 (6)	0.032 (4)*
C4	0.6705 (6)	0.7022 (12)	0.1205 (7)	0.047 (5)*
C5	0.7092 (7)	0.7025 (15)	0.1872 (9)	0.092 (7)*
H5A	0.7173	0.7696	0.2014	0.138*
H5B	0.7402	0.6695	0.1974	0.138*
H5C	0.6950	0.6688	0.2058	0.138*
C6	0.7216 (6)	0.5837 (11)	0.1097 (6)	0.032 (4)*
C7	0.7649 (6)	0.5994 (13)	0.1169 (7)	0.048 (5)*
H7	0.7706	0.6615	0.1068	0.057*
C8	0.8029 (6)	0.5309 (12)	0.1383 (7)	0.052 (5)*
H8	0.8334	0.5465	0.1421	0.062*
C9	0.7541 (6)	0.4264 (12)	0.1487 (6)	0.040 (4)*
H9	0.7494	0.3657	0.1612	0.048*
C10	0.7163 (6)	0.4918 (11)	0.1266 (6)	0.041 (4)*
H10	0.6857	0.4753	0.1225	0.049*
C11	0.5706 (5)	0.4464 (9)	0.0694 (6)	0.030 (4)*
H11A	0.5414	0.4051	0.0578	0.045*
H11B	0.5987	0.4316	0.1102	0.045*
H11C	0.5812	0.4341	0.0432	0.045*
C12	0.5558 (5)	0.5515 (10)	0.0650 (6)	0.021 (3)*
C13	0.5381 (5)	0.5882 (10)	0.0968 (6)	0.023 (4)*
C14	0.5234 (5)	0.6850 (11)	0.0944 (6)	0.030 (4)*
C15	0.5009 (5)	0.7201 (11)	0.1239 (7)	0.041 (4)*
H15A	0.4898	0.7874	0.1122	0.061*
H15B	0.5261	0.7171	0.1667	0.061*
H15C	0.4716	0.6796	0.1127	0.061*
C16	0.5300 (5)	0.5187 (10)	0.1320 (6)	0.024 (4)*
C17	0.4871 (5)	0.4617 (10)	0.1059 (6)	0.026 (4)*
H17	0.4615	0.4665	0.0648	0.032*
C18	0.4814 (6)	0.3969 (11)	0.1405 (7)	0.038 (4)*
H18	0.4525	0.3556	0.1213	0.046*
C19	0.5536 (6)	0.4429 (11)	0.2214 (7)	0.037 (4)*
H19	0.5782	0.4357	0.2626	0.045*
C20	0.5642 (6)	0.5101 (11)	0.1924 (7)	0.039 (4)*
H20	0.5940	0.5489	0.2136	0.046*
C21	0.4340 (5)	0.7873 (11)	−0.1507 (6)	0.037 (4)*
H21A	0.4290	0.7171	−0.1509	0.056*
H21B	0.4385	0.8039	−0.1818	0.056*
H21C	0.4043	0.8214	−0.1577	0.056*
C22	0.4796 (5)	0.8164 (11)	−0.0929 (6)	0.030 (4)*
C23	0.4961 (5)	0.9139 (10)	−0.0820 (6)	0.021 (4)*
C24	0.5364 (5)	0.9470 (10)	−0.0274 (6)	0.022 (4)*
C25	0.5533 (5)	1.0513 (10)	−0.0162 (6)	0.033 (4)*
H25A	0.5770	1.0622	0.0264	0.050*
H25B	0.5237	1.0937	−0.0321	0.050*
H25C	0.5703	1.0659	−0.0355	0.050*
C26	0.4676 (5)	0.9843 (10)	−0.1325 (6)	0.026 (4)*
C27	0.4303 (5)	1.0422 (10)	−0.1394 (6)	0.034 (4)*
H27	0.4226	1.0411	−0.1110	0.041*
C28	0.4035 (6)	1.1029 (11)	−0.1881 (6)	0.035 (4)*
H28	0.3789	1.1458	−0.1912	0.042*
C29	0.4488 (5)	1.0488 (10)	−0.2232 (6)	0.032 (4)*
H29	0.4562	1.0515	−0.2518	0.039*
C30	0.4777 (5)	0.9886 (11)	−0.1746 (6)	0.033 (4)*
H30	0.5043	0.9506	−0.1703	0.040*
Cl1	0.6931 (3)	0.0075 (7)	0.0560 (4)	0.121 (3)	0.7735
Cl2	0.7184 (3)	−0.1501 (5)	0.0114 (3)	0.082 (2)	0.7735
C31	0.6737 (8)	−0.0766 (15)	0.0090 (9)	0.053 (7)*	0.7735
H31A	0.6527	−0.0469	−0.0307	0.063*	0.7735
H31B	0.6510	−0.1188	0.0131	0.063*	0.7735
Cl3	0.7165 (3)	0.3660 (6)	0.0005 (3)	0.097 (3)*	0.7703
Cl4	0.6454 (3)	0.2964 (6)	0.0262 (4)	0.110 (3)*	0.7703
C32	0.6954 (9)	0.2687 (19)	0.0213 (12)	0.083 (9)*	0.7703
H32A	0.6847	0.2156	−0.0076	0.100*	0.7703
H32B	0.7242	0.2445	0.0601	0.100*	0.7703
Cl5	0.6784 (7)	0.3269 (15)	0.3041 (9)	0.196 (8)*	0.5
Cl6	0.7041 (6)	0.4057 (13)	0.2401 (8)	0.166 (7)*	0.5
C33	0.7268 (12)	0.403 (3)	0.3133 (11)	0.079 (13)*	0.5
H33A	0.7269	0.4682	0.3287	0.095*	0.5
H33B	0.7610	0.3736	0.3384	0.095*	0.5

Atomic displacement parameters (Å²) top

	U¹¹	U²²	U³³	U¹²	U¹³	U²³
I1	0.0710 (10)	0.0301 (7)	0.0745 (10)	−0.0025 (7)	0.0310 (8)	0.0104 (7)
I2	0.0718 (9)	0.0591 (9)	0.0536 (8)	−0.0092 (7)	0.0476 (8)	−0.0165 (7)
I3	0.0653 (8)	0.0276 (7)	0.0477 (8)	−0.0121 (6)	0.0365 (7)	−0.0022 (5)
Cd1	0.0420 (8)	0.0295 (7)	0.0310 (7)	0.0009 (6)	0.0199 (7)	−0.0040 (6)
Cd2	0.0611 (12)	0.0170 (9)	0.0348 (10)	0.000	0.0369 (10)	0.000
Fe1	0.0444 (15)	0.0116 (12)	0.0329 (14)	0.0042 (11)	0.0268 (12)	0.0053 (10)
Cl1	0.102 (7)	0.118 (8)	0.111 (7)	0.011 (6)	0.042 (6)	−0.035 (6)
Cl2	0.090 (5)	0.078 (5)	0.109 (6)	−0.001 (4)	0.076 (5)	0.012 (4)

Geometric parameters (Å, º) top

I1—Cd1	2.6850 (17)	C11—H11B	0.9800
I2—Cd1	2.6997 (16)	C11—H11C	0.9800
I3—Cd2	2.6876 (13)	C12—C13	1.392 (17)
Cd1—N3ⁱ	2.268 (11)	C13—C14	1.404 (18)
Cd1—N1	2.282 (12)	C13—C16	1.492 (18)
Cd2—N2ⁱⁱ	2.276 (11)	C14—C15	1.453 (18)
Cd2—N2	2.276 (11)	C15—H15A	0.9800
Cd2—I3ⁱⁱ	2.6876 (13)	C15—H15B	0.9800
Fe1—O4	1.982 (9)	C15—H15C	0.9800
Fe1—O2	1.982 (10)	C16—C17	1.380 (17)
Fe1—O1	1.984 (9)	C16—C20	1.383 (18)
Fe1—O6	1.991 (9)	C17—C18	1.395 (18)
Fe1—O5	1.994 (9)	C17—H17	0.9500
Fe1—O3	2.008 (9)	C18—H18	0.9500
O1—C2	1.251 (15)	C19—C20	1.391 (19)
O2—C4	1.308 (17)	C19—H19	0.9500
O3—C12	1.287 (14)	C20—H20	0.9500
O4—C14	1.301 (16)	C21—C22	1.475 (18)
O5—C22	1.295 (15)	C21—H21A	0.9800
O6—C24	1.300 (14)	C21—H21B	0.9800
N1—C9	1.311 (17)	C21—H21C	0.9800
N1—C8	1.373 (18)	C22—C23	1.412 (18)
N2—C19	1.286 (16)	C23—C24	1.386 (17)
N2—C18	1.309 (17)	C23—C26	1.505 (18)
N3—C29	1.338 (16)	C24—C25	1.506 (18)
N3—C28	1.341 (16)	C25—H25A	0.9800
N3—Cd1ⁱⁱⁱ	2.268 (11)	C25—H25B	0.9800
C1—C2	1.480 (19)	C25—H25C	0.9800
C1—H1A	0.9800	C26—C27	1.361 (18)
C1—H1B	0.9800	C26—C30	1.383 (18)
C1—H1C	0.9800	C27—C28	1.390 (19)
C2—C3	1.373 (19)	C27—H27	0.9500
C3—C4	1.38 (2)	C28—H28	0.9500
C3—C6	1.504 (19)	C29—C30	1.388 (18)
C4—C5	1.52 (2)	C29—H29	0.9500
C5—H5A	0.9800	C30—H30	0.9500
C5—H5B	0.9800	Cl1—C31	1.58 (2)
C5—H5C	0.9800	Cl2—C31	1.73 (2)
C6—C7	1.307 (19)	C31—H31A	0.9900
C6—C10	1.396 (19)	C31—H31B	0.9900
C7—C8	1.38 (2)	Cl3—C32	1.75 (2)
C7—H7	0.9500	Cl4—C32	1.73 (2)
C8—H8	0.9500	C32—H32A	0.9900
C9—C10	1.347 (19)	C32—H32B	0.9900
C9—H9	0.9500	Cl5—C33	1.775 (18)
C10—H10	0.9500	Cl6—C33	1.717 (18)
C11—C12	1.507 (17)	C33—H33A	0.9900
C11—H11A	0.9800	C33—H33B	0.9900

N3ⁱ—Cd1—N1	91.0 (4)	O3—C12—C13	123.9 (12)
N3ⁱ—Cd1—I1	113.7 (3)	O3—C12—C11	114.4 (12)
N1—Cd1—I1	102.8 (3)	C13—C12—C11	121.6 (12)
N3ⁱ—Cd1—I2	104.1 (3)	C12—C13—C14	124.5 (13)
N1—Cd1—I2	105.3 (3)	C12—C13—C16	117.9 (12)
I1—Cd1—I2	131.82 (6)	C14—C13—C16	117.5 (12)
N2ⁱⁱ—Cd2—N2	99.6 (6)	O4—C14—C13	121.2 (13)
N2ⁱⁱ—Cd2—I3	108.8 (3)	O4—C14—C15	115.2 (13)
N2—Cd2—I3	105.4 (3)	C13—C14—C15	123.6 (14)
N2ⁱⁱ—Cd2—I3ⁱⁱ	105.4 (3)	C14—C15—H15A	109.5
N2—Cd2—I3ⁱⁱ	108.8 (3)	C14—C15—H15B	109.5
I3—Cd2—I3ⁱⁱ	125.78 (7)	H15A—C15—H15B	109.5
O4—Fe1—O2	90.3 (4)	C14—C15—H15C	109.5
O4—Fe1—O1	167.9 (4)	H15A—C15—H15C	109.5
O2—Fe1—O1	84.9 (4)	H15B—C15—H15C	109.5
O4—Fe1—O6	93.7 (4)	C17—C16—C20	116.3 (14)
O2—Fe1—O6	89.2 (4)	C17—C16—C13	121.5 (12)
O1—Fe1—O6	97.3 (4)	C20—C16—C13	122.1 (13)
O4—Fe1—O5	93.8 (4)	C16—C17—C18	119.5 (14)
O2—Fe1—O5	174.0 (4)	C16—C17—H17	120.2
O1—Fe1—O5	91.9 (4)	C18—C17—H17	120.2
O6—Fe1—O5	86.2 (4)	N2—C18—C17	123.8 (14)
O4—Fe1—O3	85.0 (4)	N2—C18—H18	118.1
O2—Fe1—O3	93.6 (4)	C17—C18—H18	118.1
O1—Fe1—O3	84.3 (4)	N2—C19—C20	126.3 (15)
O6—Fe1—O3	176.8 (4)	N2—C19—H19	116.9
O5—Fe1—O3	91.1 (4)	C20—C19—H19	116.9
C2—O1—Fe1	124.7 (9)	C16—C20—C19	117.9 (14)
C4—O2—Fe1	122.2 (10)	C16—C20—H20	121.0
C12—O3—Fe1	129.7 (8)	C19—C20—H20	121.0
C14—O4—Fe1	132.5 (9)	C22—C21—H21A	109.5
C22—O5—Fe1	130.6 (9)	C22—C21—H21B	109.5
C24—O6—Fe1	130.6 (8)	H21A—C21—H21B	109.5
C9—N1—C8	115.3 (14)	C22—C21—H21C	109.5
C9—N1—Cd1	125.3 (11)	H21A—C21—H21C	109.5
C8—N1—Cd1	119.2 (10)	H21B—C21—H21C	109.5
C19—N2—C18	115.9 (14)	O5—C22—C23	123.9 (13)
C19—N2—Cd2	123.2 (10)	O5—C22—C21	115.5 (13)
C18—N2—Cd2	120.9 (10)	C23—C22—C21	120.6 (13)
C29—N3—C28	117.9 (13)	C24—C23—C22	123.2 (13)
C29—N3—Cd1ⁱⁱⁱ	118.5 (9)	C24—C23—C26	119.4 (12)
C28—N3—Cd1ⁱⁱⁱ	123.1 (10)	C22—C23—C26	117.4 (12)
C2—C1—H1A	109.5	O6—C24—C23	124.3 (12)
C2—C1—H1B	109.5	O6—C24—C25	113.0 (12)
H1A—C1—H1B	109.5	C23—C24—C25	122.7 (12)
C2—C1—H1C	109.5	C24—C25—H25A	109.5
H1A—C1—H1C	109.5	C24—C25—H25B	109.5
H1B—C1—H1C	109.5	H25A—C25—H25B	109.5
O1—C2—C3	125.1 (14)	C24—C25—H25C	109.5
O1—C2—C1	114.9 (13)	H25A—C25—H25C	109.5
C3—C2—C1	119.9 (14)	H25B—C25—H25C	109.5
C2—C3—C4	121.6 (14)	C27—C26—C30	118.3 (14)
C2—C3—C6	121.6 (13)	C27—C26—C23	121.7 (13)
C4—C3—C6	116.8 (14)	C30—C26—C23	120.0 (13)
O2—C4—C3	125.3 (15)	C26—C27—C28	119.6 (15)
O2—C4—C5	111.2 (15)	C26—C27—H27	120.2
C3—C4—C5	123.3 (16)	C28—C27—H27	120.2
C4—C5—H5A	109.5	N3—C28—C27	122.3 (15)
C4—C5—H5B	109.5	N3—C28—H28	118.8
H5A—C5—H5B	109.5	C27—C28—H28	118.8
C4—C5—H5C	109.5	N3—C29—C30	122.0 (14)
H5A—C5—H5C	109.5	N3—C29—H29	119.0
H5B—C5—H5C	109.5	C30—C29—H29	119.0
C7—C6—C10	115.2 (15)	C26—C30—C29	119.6 (14)
C7—C6—C3	125.4 (15)	C26—C30—H30	120.2
C10—C6—C3	119.3 (14)	C29—C30—H30	120.2
C6—C7—C8	123.7 (17)	Cl1—C31—Cl2	118.2 (13)
C6—C7—H7	118.2	Cl1—C31—H31A	107.8
C8—C7—H7	118.2	Cl2—C31—H31A	107.8
N1—C8—C7	120.5 (16)	Cl1—C31—H31B	107.8
N1—C8—H8	119.7	Cl2—C31—H31B	107.8
C7—C8—H8	119.7	H31A—C31—H31B	107.1
N1—C9—C10	124.7 (16)	Cl4—C32—Cl3	114.4 (15)
N1—C9—H9	117.6	Cl4—C32—H32A	108.7
C10—C9—H9	117.6	Cl3—C32—H32A	108.7
C9—C10—C6	120.4 (15)	Cl4—C32—H32B	108.7
C9—C10—H10	119.8	Cl3—C32—H32B	108.7
C6—C10—H10	119.8	H32A—C32—H32B	107.6
C12—C11—H11A	109.5	Cl6—C33—Cl5	95.7 (15)
C12—C11—H11B	109.5	Cl6—C33—H33A	112.6
H11A—C11—H11B	109.5	Cl5—C33—H33A	112.6
C12—C11—H11C	109.5	Cl6—C33—H33B	112.6
H11A—C11—H11C	109.5	Cl5—C33—H33B	112.6
H11B—C11—H11C	109.5	H33A—C33—H33B	110.1

Symmetry codes: (i) x+1/2, −y+3/2, z+1/2; (ii) −x+1, y, −z+1/2; (iii) x−1/2, −y+3/2, z−1/2.

(6_without_squeeze) top

Crystal data top

C_64.09H_68.18Cd₃Cl_8.18Fe₂I₆N₆O₁₂	F(000) = 4975
M_r = 2614.57	D_x = 1.726 Mg m⁻³
Monoclinic, C2/c	Mo Kα radiation, λ = 0.71073 Å
a = 32.186 (3) Å	Cell parameters from 3756 reflections
b = 13.7863 (15) Å	θ = 2.4–19.7°
c = 27.721 (2) Å	µ = 3.01 mm⁻¹
β = 125.118 (8)°	T = 100 K
V = 10061.4 (18) Å³	Block, red
Z = 4	0.15 × 0.08 × 0.07 mm

Data collection top

CCD area detector diffractometer	3835 reflections with I > 2σ(I)
Radiation source: Incoatec microsource	R_int = 0.090
ω scans	θ_max = 22.0°, θ_min = 1.8°
Absorption correction: multi-scan SADABS	h = −33→33
T_min = 0.587, T_max = 0.745	k = −14→14
41442 measured reflections	l = −29→29
6166 independent reflections

Refinement top

Refinement on F²	Primary atom site location: heavy-atom method
Least-squares matrix: full	Hydrogen site location: inferred from neighbouring sites
R[F² > 2σ(F²)] = 0.073	H-atom parameters constrained
wR(F²) = 0.210	w = 1/[σ²(F_o²) + (0.0904P)²] where P = (F_o² + 2F_c²)/3
S = 1.00	(Δ/σ)_max < 0.001
6166 reflections	Δρ_max = 2.43 e Å⁻³
259 parameters	Δρ_min = −1.56 e Å⁻³
2 restraints

Crystal data top

C_64.09H_68.18Cd₃Cl_8.18Fe₂I₆N₆O₁₂	V = 10061.4 (18) Å³
M_r = 2614.57	Z = 4
Monoclinic, C2/c	Mo Kα radiation
a = 32.186 (3) Å	µ = 3.01 mm⁻¹
b = 13.7863 (15) Å	T = 100 K
c = 27.721 (2) Å	0.15 × 0.08 × 0.07 mm
β = 125.118 (8)°

Data collection top

CCD area detector diffractometer	6166 independent reflections
Absorption correction: multi-scan SADABS	3835 reflections with I > 2σ(I)
T_min = 0.587, T_max = 0.745	R_int = 0.090
41442 measured reflections	θ_max = 22.0°

Refinement top

R[F² > 2σ(F²)] = 0.073	2 restraints
wR(F²) = 0.210	H-atom parameters constrained
S = 1.00	Δρ_max = 2.43 e Å⁻³
6166 reflections	Δρ_min = −1.56 e Å⁻³
259 parameters

Special details top

Fractional atomic coordinates and isotropic or equivalent isotropic displacement parameters (Å²) top

	x	y	z	U_iso*/U_eq	Occ. (<1)
I1	0.81334 (6)	0.16302 (10)	0.18587 (7)	0.0639 (5)
I2	0.89629 (6)	0.36744 (11)	0.11910 (6)	0.0539 (5)
I3	0.41197 (5)	0.19408 (9)	0.16984 (6)	0.0444 (4)
Cd1	0.85707 (5)	0.32468 (10)	0.18031 (6)	0.0345 (4)
Cd2	0.5000	0.28294 (12)	0.2500	0.0321 (5)
Fe1	0.56591 (9)	0.74831 (16)	0.02682 (11)	0.0268 (6)
O1	0.6074 (4)	0.7195 (8)	−0.0037 (5)	0.032 (3)*
O2	0.6321 (4)	0.7596 (8)	0.1049 (5)	0.036 (3)*
O3	0.5632 (4)	0.6035 (7)	0.0321 (4)	0.025 (3)*
O4	0.5302 (4)	0.7513 (8)	0.0652 (5)	0.033 (3)*
O5	0.5018 (4)	0.7475 (8)	−0.0540 (5)	0.029 (3)*
O6	0.5645 (4)	0.8915 (7)	0.0188 (4)	0.023 (3)*
N1	0.7967 (5)	0.4412 (10)	0.1540 (6)	0.034 (4)*
N2	0.5132 (5)	0.3896 (9)	0.1977 (6)	0.026 (3)*
N3	0.4110 (5)	1.1025 (10)	−0.2312 (6)	0.028 (3)*
C1	0.6581 (7)	0.6182 (14)	−0.0159 (8)	0.049 (5)*
H1A	0.6444	0.5521	−0.0240	0.073*
H1B	0.6949	0.6156	0.0039	0.073*
H1C	0.6424	0.6539	−0.0531	0.073*
C2	0.6468 (6)	0.6684 (12)	0.0228 (7)	0.031 (4)*
C3	0.6781 (6)	0.6529 (12)	0.0834 (7)	0.031 (5)*
C4	0.6700 (7)	0.7026 (14)	0.1208 (9)	0.047 (5)*
C5	0.7091 (9)	0.7046 (18)	0.1865 (10)	0.089 (8)*
H5A	0.7145	0.7717	0.2005	0.134*
H5B	0.7411	0.6777	0.1958	0.134*
H5C	0.6971	0.6658	0.2058	0.134*
C6	0.7209 (6)	0.5833 (12)	0.1096 (7)	0.031 (4)*
C7	0.7651 (7)	0.5989 (15)	0.1165 (8)	0.048 (5)*
H7	0.7704	0.6611	0.1061	0.058*
C8	0.8036 (8)	0.5310 (15)	0.1376 (8)	0.054 (6)*
H8	0.8338	0.5459	0.1407	0.065*
C9	0.7539 (7)	0.4282 (14)	0.1484 (8)	0.043 (5)*
H9	0.7493	0.3673	0.1607	0.052*
C10	0.7158 (7)	0.4925 (13)	0.1269 (8)	0.041 (5)*
H10	0.6856	0.4759	0.1237	0.050*
C11	0.5703 (6)	0.4461 (11)	0.0698 (7)	0.029 (4)*
H11A	0.5404	0.4054	0.0556	0.044*
H11B	0.5965	0.4306	0.1113	0.044*
H11C	0.5835	0.4336	0.0462	0.044*
C12	0.5558 (6)	0.5513 (11)	0.0646 (7)	0.020 (4)*
C13	0.5379 (6)	0.5882 (11)	0.0963 (7)	0.024 (4)*
C14	0.5240 (6)	0.6845 (12)	0.0941 (7)	0.030 (4)*
C15	0.5007 (7)	0.7204 (13)	0.1244 (8)	0.042 (5)*
H15A	0.4890	0.7874	0.1122	0.063*
H15B	0.5260	0.7182	0.1672	0.063*
H15C	0.4717	0.6792	0.1136	0.063*
C16	0.5294 (6)	0.5184 (11)	0.1316 (7)	0.024 (4)*
C17	0.4873 (6)	0.4616 (11)	0.1058 (7)	0.028 (4)*
H17	0.4620	0.4657	0.0646	0.034*
C18	0.4814 (7)	0.3961 (13)	0.1409 (8)	0.039 (5)*
H18	0.4526	0.3547	0.1217	0.047*
C19	0.5527 (7)	0.4429 (13)	0.2220 (8)	0.039 (5)*
H19	0.5769	0.4368	0.2634	0.047*
C20	0.5631 (7)	0.5105 (13)	0.1919 (8)	0.040 (5)*
H20	0.5927	0.5498	0.2129	0.049*
C21	0.4335 (6)	0.7867 (13)	−0.1503 (7)	0.037 (5)*
H21A	0.4267	0.7177	−0.1491	0.056*
H21B	0.4385	0.7977	−0.1814	0.056*
H21C	0.4045	0.8252	−0.1583	0.056*
C22	0.4795 (6)	0.8157 (12)	−0.0930 (7)	0.030 (4)*
C23	0.4955 (6)	0.9135 (11)	−0.0823 (7)	0.023 (4)*
C24	0.5368 (6)	0.9465 (12)	−0.0265 (7)	0.024 (4)*
C25	0.5536 (6)	1.0512 (12)	−0.0163 (7)	0.034 (5)*
H25A	0.5794	1.0619	0.0259	0.051*
H25B	0.5243	1.0934	−0.0297	0.051*
H25C	0.5680	1.0663	−0.0383	0.051*
C26	0.4669 (6)	0.9835 (12)	−0.1326 (7)	0.028 (4)*
C27	0.4295 (6)	1.0413 (12)	−0.1392 (7)	0.035 (5)*
H27	0.4215	1.0394	−0.1111	0.042*
C28	0.4032 (6)	1.1028 (13)	−0.1875 (7)	0.035 (5)*
H28	0.3791	1.1466	−0.1903	0.042*
C29	0.4486 (6)	1.0483 (12)	−0.2241 (7)	0.033 (5)*
H29	0.4557	1.0509	−0.2529	0.039*
C30	0.4776 (7)	0.9877 (13)	−0.1751 (7)	0.037 (5)*
H30	0.5043	0.9498	−0.1706	0.044*
Cl1	0.6933 (4)	0.0074 (8)	0.0561 (5)	0.121 (4)	0.7735
Cl2	0.7182 (3)	−0.1508 (6)	0.0107 (4)	0.079 (3)	0.7735
C31	0.6732 (9)	−0.0769 (18)	0.0081 (11)	0.052 (7)*	0.7735
H31A	0.6525	−0.0467	−0.0314	0.063*	0.7735
H31B	0.6503	−0.1189	0.0119	0.063*	0.7735
Cl3	0.7167 (3)	0.3657 (7)	0.0003 (4)	0.095 (3)*	0.7703
Cl4	0.6458 (4)	0.2956 (7)	0.0264 (5)	0.108 (3)*	0.7703
C32	0.6951 (11)	0.267 (2)	0.0186 (14)	0.082 (10)*	0.7703
H32A	0.7239	0.2393	0.0562	0.098*	0.7703
H32B	0.6828	0.2170	−0.0123	0.098*	0.7703
Cl5	0.6784 (9)	0.3268 (18)	0.3045 (11)	0.192 (10)*	0.5
Cl6	0.7025 (8)	0.4047 (17)	0.2388 (9)	0.167 (8)*	0.5
C33	0.7266 (15)	0.402 (3)	0.3124 (13)	0.093 (18)*	0.5
H33A	0.7275	0.4671	0.3282	0.112*	0.5
H33B	0.7607	0.3718	0.3367	0.112*	0.5

Atomic displacement parameters (Å²) top

	U¹¹	U²²	U³³	U¹²	U¹³	U²³
I1	0.0698 (11)	0.0301 (9)	0.0734 (11)	−0.0023 (7)	0.0305 (9)	0.0104 (7)
I2	0.0699 (10)	0.0582 (10)	0.0526 (9)	−0.0088 (8)	0.0463 (9)	−0.0160 (7)
I3	0.0646 (10)	0.0281 (8)	0.0471 (8)	−0.0122 (7)	0.0360 (8)	−0.0024 (6)
Cd1	0.0419 (9)	0.0294 (8)	0.0305 (8)	0.0010 (7)	0.0198 (7)	−0.0039 (6)
Cd2	0.0606 (14)	0.0170 (10)	0.0349 (12)	0.000	0.0368 (11)	0.000
Fe1	0.0441 (16)	0.0114 (13)	0.0329 (15)	0.0044 (12)	0.0267 (14)	0.0054 (11)
Cl1	0.101 (8)	0.111 (9)	0.114 (8)	0.010 (6)	0.040 (7)	−0.039 (7)
Cl2	0.090 (6)	0.073 (6)	0.108 (7)	−0.002 (5)	0.076 (6)	0.009 (5)

Geometric parameters (Å, º) top

I1—Cd1	2.687 (2)	C11—H11B	0.9800
I2—Cd1	2.6989 (19)	C11—H11C	0.9800
I3—Cd2	2.6874 (15)	C12—C13	1.40 (2)
Cd1—N3ⁱ	2.267 (13)	C13—C14	1.39 (2)
Cd1—N1	2.293 (14)	C13—C16	1.51 (2)
Cd2—N2ⁱⁱ	2.269 (13)	C14—C15	1.50 (2)
Cd2—N2	2.269 (13)	C15—H15A	0.9800
Cd2—I3ⁱⁱ	2.6874 (15)	C15—H15B	0.9800
Fe1—O4	1.966 (11)	C15—H15C	0.9800
Fe1—O6	1.984 (10)	C16—C17	1.36 (2)
Fe1—O2	1.986 (11)	C16—C20	1.38 (2)
Fe1—O1	1.987 (11)	C17—C18	1.42 (2)
Fe1—O5	1.989 (10)	C17—H17	0.9500
Fe1—O3	2.007 (10)	C18—H18	0.9500
O1—C2	1.255 (18)	C19—C20	1.41 (2)
O2—C4	1.30 (2)	C19—H19	0.9500
O3—C12	1.277 (17)	C20—H20	0.9500
O4—C14	1.307 (18)	C21—C22	1.47 (2)
O5—C22	1.295 (18)	C21—H21A	0.9800
O6—C24	1.288 (17)	C21—H21B	0.9800
N1—C9	1.31 (2)	C21—H21C	0.9800
N1—C8	1.38 (2)	C22—C23	1.41 (2)
N2—C19	1.28 (2)	C23—C24	1.42 (2)
N2—C18	1.30 (2)	C23—C26	1.50 (2)
N3—C29	1.336 (19)	C24—C25	1.51 (2)
N3—C28	1.371 (19)	C25—H25A	0.9800
N3—Cd1ⁱⁱⁱ	2.267 (13)	C25—H25B	0.9800
C1—C2	1.49 (2)	C25—H25C	0.9800
C1—H1A	0.9800	C26—C27	1.37 (2)
C1—H1B	0.9800	C26—C30	1.41 (2)
C1—H1C	0.9800	C27—C28	1.39 (2)
C2—C3	1.39 (2)	C27—H27	0.9500
C3—C4	1.39 (2)	C28—H28	0.9500
C3—C6	1.48 (2)	C29—C30	1.40 (2)
C4—C5	1.50 (3)	C29—H29	0.9500
C5—H5A	0.9800	C30—H30	0.9500
C5—H5B	0.9800	Cl1—C31	1.60 (2)
C5—H5C	0.9800	Cl2—C31	1.74 (2)
C6—C7	1.34 (2)	C31—H31A	0.9900
C6—C10	1.38 (2)	C31—H31B	0.9900
C7—C8	1.39 (2)	Cl3—C32	1.73 (3)
C7—H7	0.9500	Cl4—C32	1.76 (3)
C8—H8	0.9500	C32—H32A	0.9900
C9—C10	1.34 (2)	C32—H32B	0.9900
C9—H9	0.9500	Cl5—C33	1.774 (19)
C10—H10	0.9500	Cl6—C33	1.717 (19)
C11—C12	1.50 (2)	C33—H33A	0.9900
C11—H11A	0.9800	C33—H33B	0.9900

N3ⁱ—Cd1—N1	90.9 (5)	O3—C12—C13	123.3 (14)
N3ⁱ—Cd1—I1	113.9 (3)	O3—C12—C11	116.1 (13)
N1—Cd1—I1	102.9 (4)	C13—C12—C11	120.5 (14)
N3ⁱ—Cd1—I2	103.9 (3)	C14—C13—C12	124.0 (15)
N1—Cd1—I2	105.3 (4)	C14—C13—C16	117.7 (14)
I1—Cd1—I2	131.84 (7)	C12—C13—C16	118.2 (14)
N2ⁱⁱ—Cd2—N2	99.3 (7)	O4—C14—C13	122.8 (15)
N2ⁱⁱ—Cd2—I3	109.1 (3)	O4—C14—C15	114.4 (15)
N2—Cd2—I3	105.2 (3)	C13—C14—C15	122.9 (15)
N2ⁱⁱ—Cd2—I3ⁱⁱ	105.2 (3)	C14—C15—H15A	109.5
N2—Cd2—I3ⁱⁱ	109.1 (3)	C14—C15—H15B	109.5
I3—Cd2—I3ⁱⁱ	125.76 (9)	H15A—C15—H15B	109.5
O4—Fe1—O6	93.2 (4)	C14—C15—H15C	109.5
O4—Fe1—O2	90.1 (5)	H15A—C15—H15C	109.5
O6—Fe1—O2	89.1 (4)	H15B—C15—H15C	109.5
O4—Fe1—O1	168.3 (5)	C17—C16—C20	116.3 (16)
O6—Fe1—O1	97.4 (4)	C17—C16—C13	121.6 (14)
O2—Fe1—O1	85.3 (5)	C20—C16—C13	122.0 (15)
O4—Fe1—O5	93.3 (4)	C16—C17—C18	119.5 (16)
O6—Fe1—O5	86.4 (4)	C16—C17—H17	120.3
O2—Fe1—O5	174.5 (5)	C18—C17—H17	120.3
O1—Fe1—O5	92.1 (4)	N2—C18—C17	123.7 (17)
O4—Fe1—O3	85.3 (4)	N2—C18—H18	118.1
O6—Fe1—O3	176.8 (4)	C17—C18—H18	118.1
O2—Fe1—O3	93.6 (4)	N2—C19—C20	124.8 (18)
O1—Fe1—O3	84.3 (4)	N2—C19—H19	117.6
O5—Fe1—O3	90.9 (4)	C20—C19—H19	117.6
C2—O1—Fe1	124.3 (11)	C16—C20—C19	118.7 (17)
C4—O2—Fe1	122.1 (12)	C16—C20—H20	120.6
C12—O3—Fe1	130.2 (10)	C19—C20—H20	120.6
C14—O4—Fe1	131.2 (11)	C22—C21—H21A	109.5
C22—O5—Fe1	130.8 (11)	C22—C21—H21B	109.5
C24—O6—Fe1	130.8 (10)	H21A—C21—H21B	109.5
C9—N1—C8	116.2 (16)	C22—C21—H21C	109.5
C9—N1—Cd1	125.8 (13)	H21A—C21—H21C	109.5
C8—N1—Cd1	117.8 (12)	H21B—C21—H21C	109.5
C19—N2—C18	116.8 (16)	O5—C22—C23	124.0 (15)
C19—N2—Cd2	122.1 (12)	O5—C22—C21	115.7 (15)
C18—N2—Cd2	121.0 (12)	C23—C22—C21	120.3 (15)
C29—N3—C28	118.7 (15)	C22—C23—C24	122.4 (15)
C29—N3—Cd1ⁱⁱⁱ	118.1 (11)	C22—C23—C26	117.7 (14)
C28—N3—Cd1ⁱⁱⁱ	122.7 (11)	C24—C23—C26	119.9 (14)
C2—C1—H1A	109.5	O6—C24—C23	124.4 (15)
C2—C1—H1B	109.5	O6—C24—C25	114.0 (14)
H1A—C1—H1B	109.5	C23—C24—C25	121.5 (14)
C2—C1—H1C	109.5	C24—C25—H25A	109.5
H1A—C1—H1C	109.5	C24—C25—H25B	109.5
H1B—C1—H1C	109.5	H25A—C25—H25B	109.5
O1—C2—C3	125.4 (16)	C24—C25—H25C	109.5
O1—C2—C1	115.0 (15)	H25A—C25—H25C	109.5
C3—C2—C1	119.5 (16)	H25B—C25—H25C	109.5
C4—C3—C2	120.7 (16)	C27—C26—C30	119.1 (16)
C4—C3—C6	118.4 (16)	C27—C26—C23	121.5 (15)
C2—C3—C6	120.9 (16)	C30—C26—C23	119.4 (15)
O2—C4—C3	126.3 (18)	C26—C27—C28	119.1 (17)
O2—C4—C5	111.5 (18)	C26—C27—H27	120.4
C3—C4—C5	121.9 (18)	C28—C27—H27	120.4
C4—C5—H5A	109.5	N3—C28—C27	122.1 (17)
C4—C5—H5B	109.5	N3—C28—H28	118.9
H5A—C5—H5B	109.5	C27—C28—H28	118.9
C4—C5—H5C	109.5	N3—C29—C30	121.3 (16)
H5A—C5—H5C	109.5	N3—C29—H29	119.3
H5B—C5—H5C	109.5	C30—C29—H29	119.3
C7—C6—C10	115.2 (17)	C29—C30—C26	119.3 (17)
C7—C6—C3	125.3 (17)	C29—C30—H30	120.4
C10—C6—C3	119.4 (16)	C26—C30—H30	120.4
C6—C7—C8	125 (2)	Cl1—C31—Cl2	117.6 (16)
C6—C7—H7	117.6	Cl1—C31—H31A	107.9
C8—C7—H7	117.6	Cl2—C31—H31A	107.9
N1—C8—C7	118.1 (19)	Cl1—C31—H31B	107.9
N1—C8—H8	120.9	Cl2—C31—H31B	107.9
C7—C8—H8	120.9	H31A—C31—H31B	107.2
N1—C9—C10	126.4 (19)	Cl3—C32—Cl4	113.9 (18)
N1—C9—H9	116.8	Cl3—C32—H32A	108.8
C10—C9—H9	116.8	Cl4—C32—H32A	108.8
C9—C10—C6	119.3 (18)	Cl3—C32—H32B	108.8
C9—C10—H10	120.4	Cl4—C32—H32B	108.8
C6—C10—H10	120.4	H32A—C32—H32B	107.7
C12—C11—H11A	109.5	Cl6—C33—Cl5	95.8 (18)
C12—C11—H11B	109.5	Cl6—C33—H33A	112.6
H11A—C11—H11B	109.5	Cl5—C33—H33A	112.6
C12—C11—H11C	109.5	Cl6—C33—H33B	112.6
H11A—C11—H11C	109.5	Cl5—C33—H33B	112.6
H11B—C11—H11C	109.5	H33A—C33—H33B	110.1

Symmetry codes: (i) x+1/2, −y+3/2, z+1/2; (ii) −x+1, y, −z+1/2; (iii) x−1/2, −y+3/2, z−1/2.

Experimental details

	(1)	(2)	(3a)	(3b)
Crystal data
Chemical formula	C₃₀H₃₃Cd₂Cl₄N₃O₆	C₃₀H₃₃Br₄Cd₂N₃O₆	C₁₀H₁₁CdI₂NO₂	C₂₀H₂₂CdI₂N₂O₄
M_r	898.21	1076.03	543.41	720.59
Crystal system, space group	Triclinic, P1	Triclinic, P1	Orthorhombic, Pbca	Orthorhombic, Pca2₁
Temperature (K)	100	100	100	100
a, b, c (Å)	9.8304 (8), 13.7388 (11), 14.8816 (12)	7.1262 (9), 15.519 (2), 16.597 (2)	7.1002 (9), 14.3490 (18), 27.540 (4)	13.5307 (3), 7.0913 (7), 49.110 (2)
α, β, γ (°)	63.4935 (11), 84.0016 (13), 81.8575 (12)	91.247 (3), 97.889 (3), 98.609 (3)	90, 90, 90	90, 90, 90
V (Å³)	1778.5 (2)	1796.0 (4)	2805.7 (6)	4712.1 (5)
Z	2	2	8	8
Radiation type	Mo Kα	Mo Kα	Mo Kα	Mo Kα
µ (mm⁻¹)	1.54	5.68	5.94	3.57
Crystal size (mm)	0.29 × 0.08 × 0.06	0.18 × 0.13 × 0.04	0.27 × 0.07 × 0.03	0.25 × 0.13 × 0.11

Data collection
Diffractometer	CCD area detector diffractometer	CCD area detector diffractometer	CCD area detector diffractometer	CCD area detector diffractometer
Absorption correction	Multi-scan SADABS	Multi-scan TWINABS	Multi-scan SADABS	Multi-scan SADABS
T_min, T_max	0.632, 0.746	0.522, 0.746	0.474, 0.746	0.522, 0.746
No. of measured, independent and observed [I > 2σ(I)] reflections	26747, 9968, 7972	7336, 7336, 5914	39565, 4234, 3748	67491, 14053, 12009
R_int	0.048	0.084	0.047	0.051
θ_max (°)	29.9	26.4	30.9	31.0
(sin θ/λ)_max (Å⁻¹)	0.701	0.625	0.723	0.724

Refinement
R[F² > 2σ(F²)], wR(F²), S	0.037, 0.079, 1.03	0.056, 0.103, 1.14	0.024, 0.051, 1.11	0.038, 0.076, 1.09
No. of reflections	9968	7336	4234	14053
No. of parameters	421	423	147	545
No. of restraints	3	11	0	5
H-atom treatment	H atoms treated by a mixture of independent and constrained refinement	H atoms treated by a mixture of independent and constrained refinement	H-atom parameters constrained	H atoms treated by a mixture of independent and constrained refinement
Δρ_max, Δρ_min (e Å⁻³)	0.74, −0.54	0.99, −0.91	0.69, −0.59	1.29, −1.11
Absolute structure	?	?	?	Refined as an inversion twin.
Absolute structure parameter	?	?	?	0.41 (3)

	(4)	(5)	(6_squeeze)	(6_without_squeeze)
Crystal data
Chemical formula	C₆₀H₆₀CdCl₂Fe₂N₆O₁₂·6(CH₄O)·6(H₂O)	C₆₀H₆₀Br₂CdFe₂N₆O₁₂·0.24(C₂H₈O₂)·4.75(CH₄O)·6(H₂O)	C_64.09H_68.18Cd₃Cl_8.18Fe₂I₆N₆O₁₂	C_64.09H_68.18Cd₃Cl_8.18Fe₂I₆N₆O₁₂
M_r	1652.50	1716.66	2614.57	2614.57
Crystal system, space group	Triclinic, P1	Triclinic, P1	Monoclinic, C2/c	Monoclinic, C2/c
Temperature (K)	100	100	100	100
a, b, c (Å)	12.1351 (13), 13.2343 (14), 13.8728 (15)	12.2603 (15), 13.3560 (16), 13.9326 (16)	32.186 (3), 13.7863 (15), 27.721 (2)	32.186 (3), 13.7863 (15), 27.721 (2)
α, β, γ (°)	91.809 (2), 109.675 (2), 104.825 (2)	92.055 (2), 109.196 (2), 105.345 (2)	90, 125.118 (8), 90	90, 125.118 (8), 90
V (Å³)	2011.0 (4)	2058.8 (4)	10061.4 (18)	10061.4 (18)
Z	1	1	4	4
Radiation type	Mo Kα	Mo Kα	Mo Kα	Mo Kα
µ (mm⁻¹)	0.76	1.64	3.01	3.01
Crystal size (mm)	0.25 × 0.23 × 0.08	0.36 × 0.10 × 0.03	0.15 × 0.08 × 0.07	0.15 × 0.08 × 0.07

Data collection
Diffractometer	CCD area detector diffractometer	CCD area detector diffractometer	CCD area detector diffractometer	CCD area detector diffractometer
Absorption correction	Multi-scan SADABS	Multi-scan SADABS	Multi-scan SADABS	Multi-scan SADABS
T_min, T_max	0.640, 0.745	0.595, 0.745	0.587, 0.745	0.587, 0.745
No. of measured, independent and observed [I > 2σ(I)] reflections	24575, 8416, 6746	24811, 8482, 6555	41442, 6166, 3817	41442, 6166, 3835
R_int	0.050	0.052	0.085	0.090
θ_max (°)	26.6	26.5	22.0	22.0
(sin θ/λ)_max (Å⁻¹)	0.630	0.627	0.527	0.527

Refinement
R[F² > 2σ(F²)], wR(F²), S	0.049, 0.130, 1.04	0.054, 0.157, 1.05	0.066, 0.163, 0.95	0.073, 0.210, 1.00
No. of reflections	8416	8482	6166	6166
No. of parameters	456	441	259	259
No. of restraints	0	2	2	2
H-atom treatment	H-atom parameters constrained	H-atom parameters constrained	H-atom parameters constrained	H-atom parameters constrained
Δρ_max, Δρ_min (e Å⁻³)	1.12, −0.92	1.30, −1.05	2.31, −1.52	2.43, −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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