Crystal structure of di-μ-chlorido-bis­[di­chlorido(L-histidinium-κO)cadmium(II)]

In the bimetallic title compound, [Cd₂(C₆N₃O₂H₉)₂Cl₆], both cadmium atoms adopt a distorted CdCl₄O trigonal–bipyramidal coordination geometry.

Key indicators

• Single-crystal X-ray study
• T = 100 K
• Mean [sigma](C-C) = 0.008 Å
• R factor = 0.024
• wR factor = 0.057
• Data-to-parameter ratio = 17.7

checkCIF/PLATON results

No syntax errors found



Alert level C
PLAT094_ALERT_2_C Ratio of Maximum / Minimum Residual Density ....       3.05 Report
PLAT342_ALERT_3_C Low Bond Precision on  C-C Bonds ...............    0.00813 Ang.
PLAT420_ALERT_2_C D-H Without Acceptor       N1       --H1B      .     Please Check
PLAT911_ALERT_3_C Missing FCF Refl Between Thmin & STh/L=    0.600          5 Report
PLAT915_ALERT_3_C No Flack x Check Done: Low Friedel Pair Coverage         82 %
PLAT978_ALERT_2_C Number C-C Bonds with Positive Residual Density.          0 Info

Alert level G
PLAT007_ALERT_5_G Number of Unrefined Donor-H Atoms ..............         10 Report
PLAT012_ALERT_1_G N.O.K.   _shelx_res_checksum Found in CIF ......     Please Check
PLAT013_ALERT_1_G No       _shelx_hkl_checksum Found in CIF ......     Please Check
PLAT066_ALERT_1_G Predicted and Reported Tmin&Tmax Range Identical          ? Check
PLAT111_ALERT_2_G ADDSYM Detects New (Pseudo) Centre of Symmetry .         80 %Fit
PLAT113_ALERT_2_G ADDSYM Suggests Possible Pseudo/New  Space Group        P-1 Check
PLAT154_ALERT_1_G The s.u.'s on the Cell Angles are Equal ..(Note)      0.002 Degree
PLAT791_ALERT_4_G Model has Chirality at C2          (Chiral SPGR)          S Verify
PLAT791_ALERT_4_G Model has Chirality at C8          (Chiral SPGR)          S Verify
PLAT794_ALERT_5_G Tentative Bond Valency for Cd1       (II)      .       1.94 Info
PLAT794_ALERT_5_G Tentative Bond Valency for Cd2       (II)      .       1.97 Info
PLAT910_ALERT_3_G Missing # of FCF Reflection(s) Below Theta(Min).          1 Note
PLAT912_ALERT_4_G Missing # of FCF Reflections Above STh/L=  0.600         20 Note
PLAT933_ALERT_2_G Number of OMIT Records in Embedded .res File ...          2 Note
PLAT961_ALERT_5_G Dataset Contains no Negative Intensities .......     Please Check

   0 ALERT level A = Most likely a serious problem - resolve or explain
   0 ALERT level B = A potentially serious problem, consider carefully
   6 ALERT level C = Check. Ensure it is not caused by an omission or oversight
  15 ALERT level G = General information/check it is not something unexpected

   4 ALERT type 1 CIF construction/syntax error, inconsistent or missing data
   6 ALERT type 2 Indicator that the structure model may be wrong or deficient
   4 ALERT type 3 Indicator that the structure quality may be low
   3 ALERT type 4 Improvement, methodology, query or suggestion
   4 ALERT type 5 Informative message, check

---

Computing details

Data collection: COLLECT(Nonius, 2002); cell refinement: DENZO and SCALEPACK (Otwinowski & Minor, 1997); data reduction: DENZO and SCALEPACK (Otwinowski & Minor, 1997); program(s) used to solve structure: SIR2014 (Burla et al., 2015); program(s) used to refine structure: SHELXL2018 (Sheldrick, 2015); molecular graphics: Mercury (Macrae et al., 2006); software used to prepare material for publication: WinGX (Farrugia, 2012) and PARST (Nardelli, 1995).

Di-µ-chlorido-bis[dichlorido(L-histidinium-κO)cadmium(II)]

Crystal data

[Cd2(C6H9N3O2)2Cl6]	Z = 1
Mr = 749.87	F(000) = 364
Triclinic, P1	Dx = 2.163 Mg m^−3
Hall symbol: P 1	Mo Kα radiation, λ = 0.71073 Å
a = 7.1540 (6) Å	Cell parameters from 6833 reflections
b = 8.2591 (6) Å	θ = 2.6–27.6°
c = 10.4459 (8) Å	µ = 2.58 mm^−1
α = 108.502 (2)°	T = 100 K
β = 97.499 (2)°	Block, colourless
γ = 94.512 (2)°	0.08 × 0.03 × 0.02 mm
V = 575.54 (8) Å^3

Data collection

Bruker Nonius KappaCCD diffractometer	4856 independent reflections
Radiation source: fine-focus sealed tube	4799 reflections with I > 2σ(I)
Graphite monochromator	Rint = 0.025
Detector resolution: 8.2632 pixels mm^-1	θmax = 27.6°, θmin = 2.6°
ω scans	h = −9→9
Absorption correction: multi-scan (SADABS; Sheldrick, 2003)	k = −10→10
Tmin = 0.820, Tmax = 0.950	l = −13→13
7735 measured reflections

Refinement

Refinement on F^2	Hydrogen site location: inferred from neighbouring sites
Least-squares matrix: full	H-atom parameters constrained
R[F^2 > 2σ(F^2)] = 0.024	w = 1/[σ^2(Fo^2) + (0.0263P)^2] where P = (Fo^2 + 2Fc^2)/3
wR(F^2) = 0.057	(Δ/σ)max < 0.001
S = 1.08	Δρmax = 1.33 e Å^−3
4856 reflections	Δρmin = −0.43 e Å^−3
274 parameters	Absolute structure: Flack & Bernardinelli (2000)
3 restraints	Absolute structure parameter: 0.02 (2)

Special details

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

Fractional atomic coordinates and isotropic or equivalent isotropic displacement parameters (Ų)

	x	y	z	Uiso*/Ueq
Cd2	0.32732 (4)	0.13067 (3)	0.53489 (3)	0.00958 (10)
Cd1	0.21319 (4)	−0.04006 (3)	0.13444 (3)	0.00944 (10)
Cl2	0.5118 (2)	0.10427 (15)	0.34159 (13)	0.0111 (3)
Cl4	0.38809 (19)	−0.29705 (15)	0.05541 (13)	0.0118 (2)
Cl5	0.0240 (2)	0.02992 (15)	0.32637 (13)	0.0107 (3)
Cl1	0.25293 (19)	0.42775 (14)	0.63993 (13)	0.0131 (3)
Cl6	0.18541 (19)	−0.11633 (15)	0.59302 (13)	0.0138 (3)
Cl3	0.2694 (2)	0.17319 (16)	0.01896 (15)	0.0161 (3)
O3	0.5872 (5)	0.1400 (4)	0.6964 (4)	0.0117 (7)
C4	−0.3126 (9)	−0.3001 (7)	−0.4445 (6)	0.0096 (12)
O4	0.7438 (5)	0.3680 (4)	0.6649 (4)	0.0133 (8)
O1	−0.0490 (5)	−0.2181 (4)	−0.0211 (4)	0.0115 (7)
N1	−0.4829 (6)	−0.1360 (5)	−0.1962 (4)	0.0126 (9)
H1A	−0.447402	−0.043754	−0.218017	0.019*
H1B	−0.522967	−0.102932	−0.115773	0.019*
H1C	−0.576801	−0.202840	−0.260150	0.019*
O2	−0.2172 (6)	0.0068 (4)	0.0144 (4)	0.0133 (8)
C8	0.8474 (9)	0.3019 (6)	0.8662 (6)	0.0101 (11)
H22	0.891581	0.194267	0.870762	0.012*
N5	0.8879 (7)	0.3255 (6)	1.1983 (5)	0.0115 (10)
H22A	0.860404	0.215366	1.170454	0.014*
N2	−0.4575 (7)	−0.3273 (6)	−0.6510 (5)	0.0124 (10)
H2	−0.502332	−0.302327	−0.721887	0.015*
N3	−0.3875 (7)	−0.4694 (6)	−0.5153 (5)	0.0130 (10)
H3	−0.378659	−0.553255	−0.483665	0.016*
N4	1.0146 (6)	0.4309 (5)	0.8826 (4)	0.0107 (9)
H11A	1.054037	0.413115	0.802492	0.013*
H11B	1.108038	0.420170	0.943384	0.013*
H11C	0.981433	0.536510	0.911830	0.013*
C3	−0.2016 (8)	−0.2381 (6)	−0.3028 (5)	0.0097 (11)
H3A	−0.138831	−0.122866	−0.284998	0.012*
H3B	−0.103314	−0.311671	−0.298755	0.012*
C6	−0.4754 (9)	−0.4837 (7)	−0.6399 (6)	0.0135 (12)
H6	−0.537559	−0.584164	−0.706536	0.016*
C9	0.7299 (8)	0.3710 (6)	0.9811 (6)	0.0097 (11)
H33A	0.669343	0.465858	0.966065	0.012*
H33B	0.630052	0.280691	0.974320	0.012*
C1	−0.1857 (10)	−0.1393 (7)	−0.0503 (6)	0.0117 (13)
C5	−0.3564 (9)	−0.2120 (7)	−0.5316 (6)	0.0147 (13)
H5	−0.323972	−0.094758	−0.513781	0.018*
C2	−0.3185 (8)	−0.2340 (6)	−0.1874 (6)	0.0090 (11)
H2A	−0.362841	−0.351433	−0.192256	0.011*
C10	0.8396 (9)	0.4311 (7)	1.1223 (6)	0.0095 (12)
N6	0.9961 (7)	0.5842 (6)	1.3260 (5)	0.0129 (10)
H33	1.051801	0.670205	1.395165	0.015*
C12	0.9823 (9)	0.4198 (7)	1.3198 (6)	0.0137 (12)
H66	1.030715	0.378824	1.388932	0.016*
C7	0.7185 (9)	0.2673 (7)	0.7288 (6)	0.0086 (12)
C11	0.9078 (9)	0.5944 (6)	1.2053 (6)	0.0136 (12)
H55	0.896359	0.694526	1.183723	0.016*

Atomic displacement parameters (Ų)

	U^11	U^22	U^33	U^12	U^13	U^23
Cd2	0.0101 (2)	0.00984 (15)	0.0073 (2)	−0.00029 (13)	−0.00021 (15)	0.00184 (13)
Cd1	0.0105 (2)	0.00944 (15)	0.0071 (2)	0.00022 (13)	−0.00009 (15)	0.00171 (13)
Cl2	0.0106 (7)	0.0129 (5)	0.0080 (6)	−0.0004 (5)	−0.0004 (5)	0.0020 (5)
Cl4	0.0112 (7)	0.0124 (5)	0.0097 (6)	0.0026 (5)	0.0001 (5)	0.0013 (4)
Cl5	0.0106 (7)	0.0127 (5)	0.0071 (6)	0.0004 (5)	0.0007 (5)	0.0016 (5)
Cl1	0.0155 (7)	0.0120 (5)	0.0111 (6)	0.0024 (5)	0.0040 (6)	0.0021 (5)
Cl6	0.0123 (7)	0.0171 (5)	0.0111 (6)	−0.0051 (5)	−0.0026 (5)	0.0069 (5)
Cl3	0.0145 (7)	0.0195 (5)	0.0185 (7)	0.0018 (5)	0.0022 (6)	0.0123 (5)
O3	0.012 (2)	0.0110 (14)	0.0090 (18)	−0.0013 (13)	−0.0035 (15)	0.0016 (13)
C4	0.008 (3)	0.013 (2)	0.007 (3)	0.001 (2)	0.002 (2)	0.001 (2)
O4	0.015 (2)	0.0168 (16)	0.0083 (19)	0.0010 (15)	−0.0007 (16)	0.0057 (14)
O1	0.012 (2)	0.0102 (14)	0.0091 (18)	0.0019 (14)	−0.0026 (15)	0.0000 (13)
N1	0.012 (2)	0.0147 (18)	0.011 (2)	0.0012 (17)	0.0015 (19)	0.0044 (17)
O2	0.016 (2)	0.0105 (14)	0.0098 (19)	0.0018 (13)	−0.0032 (16)	0.0005 (13)
C8	0.012 (3)	0.009 (2)	0.009 (3)	−0.003 (2)	−0.002 (2)	0.004 (2)
N5	0.011 (3)	0.0110 (18)	0.010 (3)	0.0024 (17)	0.003 (2)	0.0005 (17)
N2	0.014 (3)	0.019 (2)	0.006 (2)	0.0066 (19)	0.004 (2)	0.0040 (19)
N3	0.011 (3)	0.017 (2)	0.012 (2)	0.0009 (17)	0.001 (2)	0.0072 (18)
N4	0.014 (2)	0.0109 (16)	0.007 (2)	0.0009 (16)	0.0019 (18)	0.0030 (15)
C3	0.010 (3)	0.012 (2)	0.006 (3)	0.0005 (19)	0.001 (2)	0.0022 (19)
C6	0.010 (3)	0.016 (2)	0.012 (3)	−0.002 (2)	0.001 (2)	0.003 (2)
C9	0.009 (3)	0.009 (2)	0.010 (3)	0.0004 (18)	0.003 (2)	0.0012 (19)
C1	0.013 (3)	0.010 (2)	0.012 (3)	−0.001 (2)	0.001 (2)	0.005 (2)
C5	0.017 (3)	0.014 (2)	0.013 (3)	0.004 (2)	0.002 (3)	0.004 (2)
C2	0.009 (3)	0.012 (2)	0.006 (3)	0.003 (2)	0.002 (2)	0.002 (2)
C10	0.009 (3)	0.010 (2)	0.009 (3)	0.001 (2)	0.003 (2)	0.003 (2)
N6	0.012 (3)	0.015 (2)	0.008 (3)	−0.0009 (19)	0.001 (2)	−0.0014 (19)
C12	0.014 (3)	0.016 (3)	0.009 (3)	0.002 (2)	0.001 (2)	0.002 (2)
C7	0.010 (3)	0.008 (2)	0.006 (3)	0.001 (2)	0.002 (2)	−0.001 (2)
C11	0.017 (3)	0.012 (2)	0.012 (3)	0.000 (2)	0.003 (2)	0.004 (2)

Geometric parameters (Å, º)

Cd1—O1	2.361 (4)	N5—C10	1.388 (6)
Cd1—Cl3	2.4662 (12)	N5—H22A	0.8600
Cd1—Cl5	2.5061 (14)	N2—C6	1.331 (7)
Cd1—Cl4	2.5155 (12)	N2—C5	1.374 (8)
Cd1—Cl2	2.7244 (14)	N2—H2	0.8600
Cd2—O3	2.320 (3)	N3—C6	1.335 (7)
Cd2—Cl1	2.4812 (11)	N3—H3	0.8600
Cd2—Cl6	2.4864 (12)	N4—H11A	0.8900
Cd2—Cl2	2.5155 (14)	N4—H11B	0.8900
Cd2—Cl5	2.7344 (14)	N4—H11C	0.8900
Cd2—Cd1	3.9162 (5)	C3—C2	1.548 (8)
O3—C7	1.280 (7)	C3—H3A	0.9700
C4—C5	1.355 (7)	C3—H3B	0.9700
C4—N3	1.383 (7)	C6—H6	0.9300
C4—C3	1.494 (8)	C9—C10	1.486 (8)
O4—C7	1.236 (6)	C9—H33A	0.9700
O1—C1	1.274 (7)	C9—H33B	0.9700
N1—C2	1.489 (6)	C1—C2	1.543 (9)
N1—H1A	0.8900	C5—H5	0.9300
N1—H1B	0.8900	C2—H2A	0.9800
N1—H1C	0.8900	C10—C11	1.362 (8)
O2—C1	1.236 (7)	N6—C12	1.334 (7)
C8—N4	1.492 (7)	N6—C11	1.366 (7)
C8—C7	1.531 (8)	N6—H33	0.8600
C8—C9	1.542 (8)	C12—H66	0.9300
C8—H22	0.9800	C11—H55	0.9300
N5—C12	1.319 (8)
O1—Cd1—Cl3	99.31 (8)	C8—N4—H11A	109.5
O1—Cd1—Cl5	91.97 (9)	C8—N4—H11B	109.5
Cl3—Cd1—Cl5	118.96 (4)	H11A—N4—H11B	109.5
O1—Cd1—Cl4	84.88 (8)	C8—N4—H11C	109.5
Cl3—Cd1—Cl4	113.33 (4)	H11A—N4—H11C	109.5
Cl5—Cd1—Cl4	127.41 (4)	H11B—N4—H11C	109.5
O1—Cd1—Cl2	166.16 (8)	C4—C3—C2	115.5 (5)
Cl3—Cd1—Cl2	94.41 (4)	C4—C3—H3A	108.4
Cl5—Cd1—Cl2	82.99 (4)	C2—C3—H3A	108.4
Cl4—Cd1—Cl2	87.97 (4)	C4—C3—H3B	108.4
O3—Cd2—Cl1	97.93 (9)	C2—C3—H3B	108.4
O3—Cd2—Cl6	85.65 (9)	H3A—C3—H3B	107.5
Cl1—Cd2—Cl6	121.93 (4)	N2—C6—N3	107.2 (5)
O3—Cd2—Cl2	95.70 (10)	N2—C6—H6	126.4
Cl1—Cd2—Cl2	112.59 (4)	N3—C6—H6	126.4
Cl6—Cd2—Cl2	124.74 (4)	C10—C9—C8	115.2 (5)
O3—Cd2—Cl5	165.13 (8)	C10—C9—H33A	108.5
Cl1—Cd2—Cl5	96.33 (4)	C8—C9—H33A	108.5
Cl6—Cd2—Cl5	83.27 (4)	C10—C9—H33B	108.5
Cl2—Cd2—Cl5	82.61 (4)	C8—C9—H33B	108.5
Cd2—Cl2—Cd1	96.64 (5)	H33A—C9—H33B	107.5
Cd1—Cl5—Cd2	96.62 (5)	O2—C1—O1	127.5 (6)
C7—O3—Cd2	117.6 (3)	O2—C1—C2	116.9 (5)
C5—C4—N3	105.7 (5)	O1—C1—C2	115.5 (5)
C5—C4—C3	129.8 (5)	C4—C5—N2	107.6 (5)
N3—C4—C3	124.5 (4)	C4—C5—H5	126.2
C1—O1—Cd1	114.9 (3)	N2—C5—H5	126.2
C2—N1—H1A	109.5	N1—C2—C1	108.2 (4)
C2—N1—H1B	109.5	N1—C2—C3	110.9 (4)
H1A—N1—H1B	109.5	C1—C2—C3	107.0 (5)
C2—N1—H1C	109.5	N1—C2—H2A	110.2
H1A—N1—H1C	109.5	C1—C2—H2A	110.2
H1B—N1—H1C	109.5	C3—C2—H2A	110.2
N4—C8—C7	110.6 (4)	C11—C10—N5	105.7 (5)
N4—C8—C9	109.8 (4)	C11—C10—C9	129.2 (4)
C7—C8—C9	108.1 (5)	N5—C10—C9	125.1 (5)
N4—C8—H22	109.4	C12—N6—C11	109.2 (5)
C7—C8—H22	109.4	C12—N6—H33	125.4
C9—C8—H22	109.4	C11—N6—H33	125.4
C12—N5—C10	109.6 (5)	N5—C12—N6	108.0 (5)
C12—N5—H22A	125.2	N5—C12—H66	126.0
C10—N5—H22A	125.2	N6—C12—H66	126.0
C6—N2—C5	109.5 (5)	O4—C7—O3	126.8 (6)
C6—N2—H2	125.3	O4—C7—C8	118.0 (5)
C5—N2—H2	125.3	O3—C7—C8	115.0 (4)
C6—N3—C4	110.1 (4)	C10—C11—N6	107.4 (4)
C6—N3—H3	125.0	C10—C11—H55	126.3
C4—N3—H3	125.0	N6—C11—H55	126.3
C5—C4—N3—C6	−0.7 (7)	C4—C3—C2—N1	−52.9 (6)
C3—C4—N3—C6	−178.8 (5)	C4—C3—C2—C1	−170.8 (4)
C5—C4—C3—C2	110.2 (7)	C12—N5—C10—C11	−0.8 (7)
N3—C4—C3—C2	−72.2 (7)	C12—N5—C10—C9	−179.0 (6)
C5—N2—C6—N3	0.1 (7)	C8—C9—C10—C11	99.8 (7)
C4—N3—C6—N2	0.4 (7)	C8—C9—C10—N5	−82.5 (7)
N4—C8—C9—C10	−52.3 (5)	C10—N5—C12—N6	0.5 (7)
C7—C8—C9—C10	−173.0 (4)	C11—N6—C12—N5	0.1 (7)
Cd1—O1—C1—O2	−18.4 (8)	Cd2—O3—C7—O4	−16.1 (8)
Cd1—O1—C1—C2	157.2 (3)	Cd2—O3—C7—C8	159.6 (4)
N3—C4—C5—N2	0.7 (7)	N4—C8—C7—O4	−13.9 (7)
C3—C4—C5—N2	178.7 (6)	C9—C8—C7—O4	106.4 (6)
C6—N2—C5—C4	−0.5 (7)	N4—C8—C7—O3	169.9 (4)
O2—C1—C2—N1	−11.4 (7)	C9—C8—C7—O3	−69.8 (5)
O1—C1—C2—N1	172.5 (5)	N5—C10—C11—N6	0.9 (7)
O2—C1—C2—C3	108.2 (6)	C9—C10—C11—N6	178.9 (6)
O1—C1—C2—C3	−67.8 (6)	C12—N6—C11—C10	−0.6 (7)

Hydrogen-bond geometry (Å, º)

D—H···A	D—H	H···A	D···A	D—H···A
N1—H1A···O3^i	0.89	2.01	2.881 (5)	167
N1—H1C···Cl6^i	0.89	2.44	3.070 (4)	128
N2—H2···Cl4^i	0.86	2.37	3.215 (5)	167
N3—H3···O4^ii	0.86	1.99	2.751 (6)	146
N4—H11A···Cl1^iii	0.89	2.38	3.229 (4)	160
N4—H11B···Cl3^iv	0.89	2.70	3.426 (5)	140
N4—H11C···O1^v	0.89	1.96	2.846 (6)	171
N5—H22A···O2^iv	0.86	1.94	2.699 (6)	147
N6—H33···Cl6^v	0.86	2.28	3.137 (5)	174
C2—H2A···O4^ii	0.98	2.56	3.252 (7)	128
C5—H5···Cl2^i	0.93	2.79	3.424 (6)	126
C9—H33B···Cl3^vi	0.97	2.81	3.686 (6)	151
C11—H55···Cl5^v	0.93	2.71	3.405 (6)	132
C11—H55···O1^v	0.93	2.53	3.245 (7)	134
C12—H66···Cl1^iv	0.93	2.78	3.618 (6)	151

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