Crystal structure of cis-aqua­chlorido­bis­(1,10-phenanthroline-κ2N,N′)chromium(III) tetra­chlorido­zincate monohydrate from synchrotron data

Moon, D.; Choi, J.-H.

doi:10.1107/S2056989015003266

Crystal structure of cis-aquachloridobis(1,10-phenanthroline-κ²N,N′)chromium(III) tetrachloridozincate monohydrate from synchrotron data

The Cr^III ion in the title complex is coordinated by two 1,10-phenanthroline (phen) ligands, one water molecule and a chloride in a cis geometry, displaying a distorted octahedral environment. The [ZnCl₄]²⁻ anion has a slightly distorted tetrahedral coordination geometry.

Keywords: crystal structure; synchrotron radiation; 1,10-phenanthroline; chloride ligand; aqua ligand; cis-geometry; chromium(III) complex.

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Supporting information

	Crystallographic Information File (CIF) https://doi.org/10.1107/S2056989015003266/wm5123sup1.cif Contains datablock I
	Structure factor file (CIF format) https://doi.org/10.1107/S2056989015003266/wm5123Isup2.hkl Contains datablock I

CCDC reference: 1049598

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Key indicators

Single-crystal synchrotron study
T = 100 K
Mean (C-C) = 0.003 Å
R factor = 0.040
wR factor = 0.107
Data-to-parameter ratio = 21.7

checkCIF/PLATON results

No syntax errors found



Alert level C
PLAT094_ALERT_2_C Ratio of Maximum / Minimum Residual Density ....       2.26 Report
PLAT911_ALERT_3_C Missing # FCF Refl Between THmin & STh/L=  0.600         32 Report
PLAT913_ALERT_3_C Missing # of Very Strong Reflections in FCF ....          7 Note
PLAT926_ALERT_1_C Reported and Calculated   R1 Differ by .........    -0.0013 Check
PLAT927_ALERT_1_C Reported and Calculated  wR2 Differ by .........    -0.0033 Check
PLAT971_ALERT_2_C Check Calcd Residual Density  0.87A From     O1A       1.66 eA-3
PLAT976_ALERT_2_C Check Calcd Residual Density  0.54A From     O1W      -0.61 eA-3

Alert level G
ABSMU01_ALERT_1_G  Calculation of _exptl_absorpt_correction_mu
                not performed for this radiation type.
PLAT002_ALERT_2_G Number of Distance or Angle Restraints on AtSite          6 Note
PLAT066_ALERT_1_G Predicted and Reported Tmin&Tmax Range Identical          ? Check
PLAT083_ALERT_2_G SHELXL Second Parameter in WGHT Unusually Large.       5.83 Why ?
PLAT172_ALERT_4_G The CIF-Embedded .res File Contains DFIX Records          2 Report
PLAT173_ALERT_4_G The CIF-Embedded .res File Contains DANG Records          2 Report
PLAT232_ALERT_2_G Hirshfeld Test Diff (M-X)  Cr1A   --  Cl1A    ..        7.0 su
PLAT232_ALERT_2_G Hirshfeld Test Diff (M-X)  Cr1A   --  O1A     ..       12.4 su
PLAT720_ALERT_4_G Number of Unusual/Non-Standard Labels ..........          4 Note
PLAT794_ALERT_5_G Tentative Bond Valency for Zn1B    (II)    .....       1.97 Note
PLAT860_ALERT_3_G Number of Least-Squares Restraints .............          6 Note
PLAT910_ALERT_3_G Missing # of FCF Reflection(s) Below Th(Min) ...          3 Report
PLAT912_ALERT_4_G Missing # of FCF Reflections Above STh/L=  0.600          9 Note
PLAT984_ALERT_1_G The Zn-f'=     0.348 Deviates from the B&C-Value      0.326 Check

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

   5 ALERT type 1 CIF construction/syntax error, inconsistent or missing data
   7 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
   4 ALERT type 4 Improvement, methodology, query or suggestion
   1 ALERT type 5 Informative message, check

Chemical context top

Chromium(III) complexes with polypyridine ligands are particularly interesting because of their long lifetimes, thermal stabilities and tunable excited states. These complexes are promising materials for the development of new molecule-based magnets, solar energy storage media or tunable solid state lasers (Powell, 1998; Dreiser et al., 2012; Scarborough et al., 2012). As a prerequisite for these applications, a detailed study of the structural and spectroscopic properties is needed. Therefore, we have been interested in the preparation, crystal structure and spectroscopic properties of chromium(III) complexes containing mixed various ligands (Choi et al., 2004a,b, 2007; Choi, 2009; Choi & Lee, 2009; Moon & Choi, 2014, 2015).

We report here on the synthesis and crystal structure of the title compound, [CrCl(phen)₂(H₂O)][ZnCl₄]·H₂O (phen = 1,10-phenanthroline), (I).

Structural commentary top

In the molecular structure of (I), there is one chlorine atom and one water molecule coordinating to the Cr^III ion in a cis arrangement with an O1A—Cr1A—Cl1A bond angle of 89.79 (5)°. The other coordination sites are occupied by four nitrogen atoms from two phen ligands, displaying an overall distorted octahedral coordination environment (Fig. 1).

The Cr—N(phen) bond lengths are in the range of 2.0495 (18) to 2.0831 (18) Å and are in good agreement with those observed in [Cr(phen)₃](ClO₄)₃·H₂O (Luck et al., 2000), cis-[CrF₂(phen)₂]ClO₄·H₂O (Birk et al., 2008) or cis-[CrCl₂(phen)₂]Cl (Gao, 2011). The Cr—Cl and Cr—(OH₂) bond lengths in (I) are 2.2734 (7) and 1.9986 (17) Å, respectively. The Cr—(OH₂) bond length is comparable to those of 1.947 (4), 1.9579 (10) and 1.996 (4) Å found in cis-[Cr(dpp)(phen)₂(H₂O)](NO₃)₂·H₂O·CH₃CN [Hdpp = (C₆H₅O)₂·PO₂H] (Ferreira et al., 1998), cis-[CrF(bpy)₂(H₂O)](ClO₄)₂·2H₂O (Birk & Bendix, 2010) and trans-[CrF(3,2,3-tet)(H₂O)](ClO₄)₂·H₂O (3,2,3-tet = 1,5,8,12-tetraazaundecane) (Choi & Lee, 2008), respectively. The Cr—Cl bond length in (I) is somewhat shorter than those of 2.2941 (15) and 2.3253 (7) Å found in cis-[CrCl₂(phen)₂]Cl (Gao, 2011) or trans-[Cr(Me₂tn)₂Cl₂]Cl (Me₂tn = 2,2-dimethylpropane-1,3-diamine) (Choi et al., 2007), respectively. The Cl1A—Cr1A—N2A and N1A—Cr1A—N3A angles in (I) are 171.72 (5) and 169.79 (7)°, respectively. The bite angles N1A—Cr1A—N2A and N3A—Cr1A—N4A are 79.76 (5) and 80.23 (7)°.

The [ZnCl₄]^2- anion and the second water molecule remain outside the coordination sphere. The Zn^II atom in the complex anion exhibits a slightly distorted tetrahedral coordination sphere caused by the influence of hydrogen bonding on the Zn—Cl bond lengths and the Cl—Zn—Cl angles. The Zn—Cl bond lengths range from 2.2443 (7) to 2.2854 (7) Å and the Cl—Zn—Cl angles from 107.54 (4) to 111.57 (3)°.

Supramolecular features top

The supramolecular architecture involves hydrogen bonds including the O—H groups of coordinating and non-coordinating water molecules as donors, and the Cl atoms of the complex anion and the O atom of the solvent water molecule as acceptors. Atom Cl3B of the [ZnCl₄]^2- anion and the Cl1A ligand atom are not involved in hydrogen bonding. An extensive array of O—H—O and O—H···Cl contacts (Table 1) generates a three-dimensional network of molecules stacked along the a axis direction (Fig. 2). These hydrogen-bonded networks help to stabilize the crystal structure.

Database survey top

A search of the Cambridge Structural Database (Version 5.35, May 2014 with one update; Groom & Allen, 2014) indicates a total of 36 hits for Cr^III complexes containing two bidentate 1,10-phenanthroline ligands. The crystal structures of cis-[Cr(dpp)(phen)₂(H₂O)](NO₃)₂·H₂O·CH₃CN (Ferreira et al., 1998), [Cr(phen)₃](ClO₄)₃·H₂O (Luck et al., 2000), cis-[CrF₂(phen)₂]ClO₄ (Birk et al., 2008) and cis-[CrCl₂(phen)₂]Cl (Gao, 2011) have been reported previously. However, no structures of complexes of [CrCl(phen)₂(H₂O)]²⁺ with any anions have been deposited.

Synthesis and crystallization top

All chemicals were reagent-grade materials and used without further purification. The starting material, cis-[CrF₂(phen)₂]ClO₄·H₂O was prepared according to a literature procedure (Glerup et al., 1970). Crude cis-[CrF₂(phen)₂]ClO₄·H₂O (0.2 g) was dissolved in 10 mL of 0.01 M HCl at 313 K, and 5 mL of 1 M HCl containing 1.2 g of solid ZnCl₂ were added to this solution. The mixture was refluxed at 328 K for 30 min and then cooled to room temperature. The resulting solution was filtered and allowed to stand at room temperature for 3–5 days, giving purple crystals of (I) suitable for X-ray structural analysis.

Refinement top

Crystal data, data collection and structure refinement details are summarized in Table 2. C-bound H atoms were placed in calculated positions (C—H = 0.95 Å) and were included in the refinement in a riding-model approximation with U_iso(H) set to 1.2U_eq(C). The H atoms of water molecules (H1O1 and H2O1: H atoms of coordinating water; H1OW and H2OW: H atoms of solvent water) were located from difference Fourier maps and refined with restraints and an O—H distance of 0.84 (1) Å, with U_iso(H) values of 1.2 U_eq(O1A, O1W).

Related literature top

For related literature, see: Birk & Bendix (2010); Birk et al. (2008); Choi (2009); Choi & Lee (2008, 2009); Choi & Moon (2014, 2015); Choi et al. (2004a, 2004b, 2007); Dreiser et al. (2012); Ferreira et al. (1998); Gao (2011); Glerup et al. (1970); Groom & Allen (2014); Luck et al. (2000); Powell (1998); Scarborough et al. (2012).

Computing details top

Data collection: PAL ADSC Quantum-210 ADX (Arvai & Nielsen, 1983); cell refinement: HKL3000sm (Otwinowski & Minor, 1997); data reduction: HKL3000sm (Otwinowski & Minor, 1997); program(s) used to solve structure: SHELXT2014/5 (Sheldrick, 2015a); program(s) used to refine structure: SHELXL2014/7 (Sheldrick, 2015b); molecular graphics: DIAMOND (Putz & Brandenburg, 2014); software used to prepare material for publication: publCIF (Westrip, 2010).

Figures top

	Fig. 1. The structure of the molecular components in (I), showing the atom-numbering scheme. Non-H atoms are shown as displacement ellipsoids at the 50% probability level.
	Fig. 2. The crystal packing in (I), viewed along [100]. Dashed lines represent O—H···O (purple) and O—H···Cl (blue) hydrogen-bonding interactions.

cis-Aquachloridobis(1,10-phenanthroline-κ²N,N')chromium(III) tetrachloridozincate monohydrate top

Crystal data top

[CrCl(C₁₂H₈N₂)₂(H₂O)][ZnCl₄]·H₂O	F(000) = 1388
M_r = 691.06	D_x = 1.706 Mg m⁻³
Monoclinic, P2₁/c	Synchrotron radiation, λ = 0.62998 Å
a = 8.2710 (17) Å	Cell parameters from 65318 reflections
b = 19.535 (4) Å	θ = 0.4–33.6°
c = 16.934 (3) Å	µ = 1.30 mm⁻¹
β = 100.55 (3)°	T = 100 K
V = 2689.8 (10) Å³	Block, purple
Z = 4	0.10 × 0.08 × 0.05 mm

Data collection top

ADSC Q210 CCD area-detector diffractometer	7016 reflections with I > 2σ(I)
Radiation source: PLSII 2D bending magnet	R_int = 0.045
ω scan	θ_max = 26.0°, θ_min = 2.2°
Absorption correction: empirical (using intensity measurements) (HKL3000sm SCALEPACK; Otwinowski & Minor, 1997)	h = −11→11
T_min = 0.881, T_max = 0.938	k = −27→27
25530 measured reflections	l = −23→23
7554 independent reflections

Refinement top

Refinement on F²	6 restraints
Least-squares matrix: full	Hydrogen site location: mixed
R[F² > 2σ(F²)] = 0.040	H atoms treated by a mixture of independent and constrained refinement
wR(F²) = 0.107	w = 1/[σ²(F_o²) + (0.0492P)² + 5.8256P] where P = (F_o² + 2F_c²)/3
S = 1.02	(Δ/σ)_max = 0.001
7554 reflections	Δρ_max = 1.96 e Å⁻³
348 parameters	Δρ_min = −0.87 e Å⁻³

Crystal data top

[CrCl(C₁₂H₈N₂)₂(H₂O)][ZnCl₄]·H₂O	V = 2689.8 (10) Å³
M_r = 691.06	Z = 4
Monoclinic, P2₁/c	Synchrotron radiation, λ = 0.62998 Å
a = 8.2710 (17) Å	µ = 1.30 mm⁻¹
b = 19.535 (4) Å	T = 100 K
c = 16.934 (3) Å	0.10 × 0.08 × 0.05 mm
β = 100.55 (3)°

Data collection top

ADSC Q210 CCD area-detector diffractometer	7554 independent reflections
Absorption correction: empirical (using intensity measurements) (HKL3000sm SCALEPACK; Otwinowski & Minor, 1997)	7016 reflections with I > 2σ(I)
T_min = 0.881, T_max = 0.938	R_int = 0.045
25530 measured reflections

Refinement top

R[F² > 2σ(F²)] = 0.040	6 restraints
wR(F²) = 0.107	H atoms treated by a mixture of independent and constrained refinement
S = 1.02	Δρ_max = 1.96 e Å⁻³
7554 reflections	Δρ_min = −0.87 e Å⁻³
348 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
Cr1A	0.77359 (4)	0.46841 (2)	0.23994 (2)	0.01080 (10)
Cl1A	0.60790 (7)	0.54226 (3)	0.29174 (3)	0.02194 (13)
O1A	0.58493 (19)	0.40363 (9)	0.21135 (9)	0.0188 (3)
H1O1	0.586 (4)	0.3627 (7)	0.1986 (18)	0.023*
H2O1	0.517 (3)	0.4046 (14)	0.2425 (16)	0.023*
N1A	0.7218 (2)	0.51346 (9)	0.12699 (10)	0.0116 (3)
N2A	0.9036 (2)	0.40349 (9)	0.17655 (10)	0.0130 (3)
N3A	0.8666 (2)	0.42150 (9)	0.34777 (10)	0.0127 (3)
N4A	0.9743 (2)	0.52941 (9)	0.27805 (10)	0.0129 (3)
C1A	0.6368 (3)	0.57069 (11)	0.10513 (12)	0.0160 (4)
H1A	0.5964	0.5966	0.1448	0.019*
C2A	0.6054 (3)	0.59364 (11)	0.02519 (13)	0.0183 (4)
H2A	0.5463	0.6349	0.0115	0.022*
C3A	0.6605 (3)	0.55611 (12)	−0.03309 (13)	0.0180 (4)
H3A	0.6377	0.5708	−0.0875	0.022*
C4A	0.7514 (2)	0.49553 (11)	−0.01165 (12)	0.0145 (4)
C5A	0.8122 (3)	0.45241 (12)	−0.06790 (13)	0.0201 (4)
H5A	0.7896	0.4637	−0.1234	0.024*
C6A	0.9019 (3)	0.39541 (12)	−0.04308 (13)	0.0205 (4)
H6A	0.9400	0.3673	−0.0816	0.025*
C7A	0.9397 (3)	0.37714 (11)	0.04016 (13)	0.0163 (4)
C8A	1.0386 (3)	0.32049 (12)	0.07004 (14)	0.0215 (4)
H8A	1.0858	0.2922	0.0347	0.026*
C9A	1.0656 (3)	0.30693 (12)	0.15110 (15)	0.0241 (5)
H9A	1.1320	0.2691	0.1722	0.029*
C10A	0.9944 (3)	0.34918 (11)	0.20257 (13)	0.0190 (4)
H10A	1.0120	0.3385	0.2582	0.023*
C11A	0.8769 (2)	0.41770 (10)	0.09595 (11)	0.0117 (3)
C12A	0.7805 (2)	0.47693 (10)	0.06979 (11)	0.0115 (3)
C13A	0.8073 (3)	0.36762 (11)	0.38182 (13)	0.0169 (4)
H13A	0.7095	0.3464	0.3546	0.020*
C14A	0.8845 (3)	0.34138 (12)	0.45623 (13)	0.0199 (4)
H14A	0.8392	0.3029	0.4787	0.024*
C15A	1.0265 (3)	0.37163 (12)	0.49676 (12)	0.0186 (4)
H15A	1.0802	0.3540	0.5470	0.022*
C16A	1.0910 (3)	0.42887 (11)	0.46279 (12)	0.0155 (4)
C17A	1.2356 (3)	0.46545 (12)	0.49998 (13)	0.0209 (4)
H17A	1.2952	0.4500	0.5502	0.025*
C18A	1.2888 (3)	0.52137 (12)	0.46518 (14)	0.0209 (4)
H18A	1.3837	0.5450	0.4918	0.025*
C19A	1.2040 (2)	0.54558 (11)	0.38867 (13)	0.0164 (4)
C20A	1.2508 (3)	0.60401 (12)	0.34946 (15)	0.0208 (4)
H20A	1.3461	0.6291	0.3725	0.025*
C21A	1.1571 (3)	0.62439 (12)	0.27744 (15)	0.0226 (4)
H21A	1.1858	0.6643	0.2510	0.027*
C22A	1.0188 (3)	0.58561 (11)	0.24359 (13)	0.0182 (4)
H22A	0.9546	0.6002	0.1941	0.022*
C23A	1.0641 (2)	0.50980 (10)	0.35036 (12)	0.0123 (3)
C24A	1.0064 (2)	0.45161 (10)	0.38781 (11)	0.0125 (3)
Zn1B	0.36987 (3)	0.28015 (2)	0.39019 (2)	0.01831 (10)
Cl1B	0.35510 (7)	0.38494 (3)	0.32928 (4)	0.02700 (15)
Cl2B	0.57258 (8)	0.21748 (3)	0.35055 (5)	0.03248 (17)
Cl3B	0.12374 (6)	0.22928 (3)	0.35577 (3)	0.01971 (13)
Cl4B	0.42194 (10)	0.29190 (4)	0.52663 (4)	0.03734 (18)
O1W	0.6215 (3)	0.27775 (11)	0.18258 (15)	0.0383 (5)
H1OW	0.575 (5)	0.2623 (19)	0.1371 (10)	0.046*
H2OW	0.589 (5)	0.2513 (17)	0.2168 (16)	0.046*

Atomic displacement parameters (Å²) top

	U¹¹	U²²	U³³	U¹²	U¹³	U²³
Cr1A	0.01239 (16)	0.01388 (16)	0.00571 (15)	0.00007 (10)	0.00052 (10)	0.00026 (10)
Cl1A	0.0241 (3)	0.0262 (3)	0.0161 (2)	0.0080 (2)	0.00524 (19)	−0.00103 (19)
O1A	0.0145 (7)	0.0292 (8)	0.0123 (7)	0.0010 (6)	0.0014 (5)	0.0026 (6)
N1A	0.0131 (7)	0.0132 (7)	0.0076 (7)	−0.0004 (6)	−0.0002 (6)	0.0008 (6)
N2A	0.0166 (8)	0.0130 (7)	0.0089 (7)	0.0009 (6)	0.0014 (6)	0.0011 (6)
N3A	0.0155 (7)	0.0147 (7)	0.0076 (7)	0.0011 (6)	0.0013 (6)	0.0009 (6)
N4A	0.0129 (7)	0.0147 (8)	0.0108 (7)	0.0005 (6)	0.0013 (6)	−0.0025 (6)
C1A	0.0161 (9)	0.0165 (9)	0.0142 (9)	0.0027 (7)	−0.0004 (7)	0.0009 (7)
C2A	0.0180 (9)	0.0179 (9)	0.0167 (9)	0.0011 (7)	−0.0028 (7)	0.0036 (7)
C3A	0.0184 (9)	0.0211 (10)	0.0126 (9)	−0.0025 (8)	−0.0019 (7)	0.0050 (7)
C4A	0.0155 (8)	0.0188 (9)	0.0088 (8)	−0.0034 (7)	0.0009 (7)	0.0011 (7)
C5A	0.0259 (10)	0.0262 (11)	0.0087 (8)	−0.0029 (8)	0.0042 (7)	−0.0006 (8)
C6A	0.0261 (11)	0.0238 (10)	0.0130 (9)	−0.0024 (8)	0.0074 (8)	−0.0047 (8)
C7A	0.0200 (9)	0.0153 (9)	0.0147 (9)	−0.0013 (7)	0.0061 (7)	−0.0035 (7)
C8A	0.0271 (11)	0.0168 (9)	0.0223 (10)	0.0032 (8)	0.0090 (9)	−0.0029 (8)
C9A	0.0310 (12)	0.0177 (10)	0.0240 (11)	0.0086 (9)	0.0062 (9)	0.0015 (8)
C10A	0.0245 (10)	0.0163 (9)	0.0156 (9)	0.0052 (8)	0.0021 (8)	0.0022 (7)
C11A	0.0143 (8)	0.0127 (8)	0.0082 (8)	−0.0029 (6)	0.0021 (6)	−0.0005 (6)
C12A	0.0116 (8)	0.0143 (8)	0.0080 (8)	−0.0028 (6)	0.0005 (6)	−0.0001 (6)
C13A	0.0198 (9)	0.0171 (9)	0.0141 (9)	−0.0004 (7)	0.0038 (7)	0.0018 (7)
C14A	0.0258 (10)	0.0196 (10)	0.0151 (9)	0.0046 (8)	0.0057 (8)	0.0052 (8)
C15A	0.0241 (10)	0.0213 (10)	0.0101 (8)	0.0100 (8)	0.0025 (7)	0.0026 (7)
C16A	0.0156 (9)	0.0192 (9)	0.0108 (8)	0.0075 (7)	0.0002 (7)	−0.0021 (7)
C17A	0.0169 (9)	0.0282 (11)	0.0148 (9)	0.0087 (8)	−0.0046 (7)	−0.0052 (8)
C18A	0.0140 (9)	0.0252 (11)	0.0207 (10)	0.0050 (8)	−0.0039 (8)	−0.0090 (8)
C19A	0.0123 (8)	0.0186 (9)	0.0176 (9)	0.0020 (7)	0.0011 (7)	−0.0063 (7)
C20A	0.0162 (9)	0.0193 (10)	0.0267 (11)	−0.0033 (8)	0.0030 (8)	−0.0063 (8)
C21A	0.0220 (10)	0.0189 (10)	0.0274 (11)	−0.0062 (8)	0.0054 (9)	−0.0004 (8)
C22A	0.0193 (9)	0.0191 (9)	0.0158 (9)	−0.0020 (8)	0.0025 (7)	0.0005 (7)
C23A	0.0118 (8)	0.0142 (8)	0.0106 (8)	0.0024 (6)	0.0017 (6)	−0.0028 (7)
C24A	0.0128 (8)	0.0155 (8)	0.0092 (8)	0.0040 (7)	0.0015 (6)	−0.0010 (6)
Zn1B	0.01505 (14)	0.01295 (14)	0.02733 (16)	−0.00137 (8)	0.00488 (10)	−0.00108 (9)
Cl1B	0.0273 (3)	0.0157 (2)	0.0436 (4)	0.00190 (19)	0.0212 (3)	0.0037 (2)
Cl2B	0.0238 (3)	0.0158 (3)	0.0623 (5)	0.00274 (19)	0.0199 (3)	0.0013 (3)
Cl3B	0.0182 (2)	0.0157 (2)	0.0243 (3)	−0.00401 (17)	0.00131 (19)	0.00362 (18)
Cl4B	0.0441 (4)	0.0316 (3)	0.0282 (3)	0.0039 (3)	−0.0148 (3)	−0.0057 (2)
O1W	0.0443 (12)	0.0256 (10)	0.0421 (12)	−0.0001 (8)	0.0005 (10)	−0.0081 (8)

Geometric parameters (Å, º) top

Cr1A—O1A	1.9986 (17)	C8A—H8A	0.9500
Cr1A—N4A	2.0495 (18)	C9A—C10A	1.405 (3)
Cr1A—N3A	2.0619 (17)	C9A—H9A	0.9500
Cr1A—N1A	2.0775 (17)	C10A—H10A	0.9500
Cr1A—N2A	2.0831 (18)	C11A—C12A	1.429 (3)
Cr1A—Cl1A	2.2734 (7)	C13A—C14A	1.401 (3)
O1A—H1O1	0.829 (10)	C13A—H13A	0.9500
O1A—H2O1	0.839 (10)	C14A—C15A	1.380 (3)
N1A—C1A	1.336 (3)	C14A—H14A	0.9500
N1A—C12A	1.362 (3)	C15A—C16A	1.406 (3)
N2A—C10A	1.328 (3)	C15A—H15A	0.9500
N2A—C11A	1.371 (2)	C16A—C24A	1.405 (3)
N3A—C13A	1.336 (3)	C16A—C17A	1.436 (3)
N3A—C24A	1.362 (3)	C17A—C18A	1.353 (4)
N4A—C22A	1.327 (3)	C17A—H17A	0.9500
N4A—C23A	1.366 (3)	C18A—C19A	1.436 (3)
C1A—C2A	1.404 (3)	C18A—H18A	0.9500
C1A—H1A	0.9500	C19A—C23A	1.405 (3)
C2A—C3A	1.372 (3)	C19A—C20A	1.410 (3)
C2A—H2A	0.9500	C20A—C21A	1.378 (3)
C3A—C4A	1.413 (3)	C20A—H20A	0.9500
C3A—H3A	0.9500	C21A—C22A	1.404 (3)
C4A—C12A	1.404 (3)	C21A—H21A	0.9500
C4A—C5A	1.430 (3)	C22A—H22A	0.9500
C5A—C6A	1.361 (3)	C23A—C24A	1.426 (3)
C5A—H5A	0.9500	Zn1B—Cl3B	2.2443 (7)
C6A—C7A	1.432 (3)	Zn1B—Cl2B	2.2744 (8)
C6A—H6A	0.9500	Zn1B—Cl4B	2.2830 (9)
C7A—C11A	1.404 (3)	Zn1B—Cl1B	2.2854 (7)
C7A—C8A	1.414 (3)	O1W—H1OW	0.851 (10)
C8A—C9A	1.376 (3)	O1W—H2OW	0.855 (10)

O1A—Cr1A—N4A	174.86 (7)	C8A—C9A—H9A	120.1
O1A—Cr1A—N3A	94.66 (7)	C10A—C9A—H9A	120.1
N4A—Cr1A—N3A	80.23 (7)	N2A—C10A—C9A	122.6 (2)
O1A—Cr1A—N1A	91.43 (7)	N2A—C10A—H10A	118.7
N4A—Cr1A—N1A	93.56 (7)	C9A—C10A—H10A	118.7
N3A—Cr1A—N1A	169.79 (7)	N2A—C11A—C7A	122.96 (19)
O1A—Cr1A—N2A	86.75 (7)	N2A—C11A—C12A	116.85 (17)
N4A—Cr1A—N2A	92.95 (7)	C7A—C11A—C12A	120.19 (18)
N3A—Cr1A—N2A	92.39 (7)	N1A—C12A—C4A	122.94 (18)
N1A—Cr1A—N2A	79.76 (7)	N1A—C12A—C11A	117.07 (17)
O1A—Cr1A—Cl1A	89.79 (5)	C4A—C12A—C11A	119.99 (18)
N4A—Cr1A—Cl1A	91.17 (5)	N3A—C13A—C14A	122.3 (2)
N3A—Cr1A—Cl1A	95.39 (5)	N3A—C13A—H13A	118.9
N1A—Cr1A—Cl1A	92.82 (5)	C14A—C13A—H13A	118.9
N2A—Cr1A—Cl1A	171.72 (5)	C15A—C14A—C13A	119.8 (2)
Cr1A—O1A—H1O1	129 (2)	C15A—C14A—H14A	120.1
Cr1A—O1A—H2O1	115 (2)	C13A—C14A—H14A	120.1
H1O1—O1A—H2O1	103 (2)	C14A—C15A—C16A	119.26 (19)
C1A—N1A—C12A	118.63 (17)	C14A—C15A—H15A	120.4
C1A—N1A—Cr1A	128.22 (14)	C16A—C15A—H15A	120.4
C12A—N1A—Cr1A	113.12 (13)	C24A—C16A—C15A	117.26 (19)
C10A—N2A—C11A	118.07 (18)	C24A—C16A—C17A	118.4 (2)
C10A—N2A—Cr1A	129.02 (15)	C15A—C16A—C17A	124.32 (19)
C11A—N2A—Cr1A	112.69 (13)	C18A—C17A—C16A	121.5 (2)
C13A—N3A—C24A	118.07 (17)	C18A—C17A—H17A	119.3
C13A—N3A—Cr1A	128.73 (14)	C16A—C17A—H17A	119.3
C24A—N3A—Cr1A	113.20 (13)	C17A—C18A—C19A	121.0 (2)
C22A—N4A—C23A	118.51 (18)	C17A—C18A—H18A	119.5
C22A—N4A—Cr1A	128.07 (15)	C19A—C18A—H18A	119.5
C23A—N4A—Cr1A	113.30 (14)	C23A—C19A—C20A	117.3 (2)
N1A—C1A—C2A	121.9 (2)	C23A—C19A—C18A	118.5 (2)
N1A—C1A—H1A	119.0	C20A—C19A—C18A	124.1 (2)
C2A—C1A—H1A	119.0	C21A—C20A—C19A	119.5 (2)
C3A—C2A—C1A	119.7 (2)	C21A—C20A—H20A	120.2
C3A—C2A—H2A	120.1	C19A—C20A—H20A	120.2
C1A—C2A—H2A	120.1	C20A—C21A—C22A	119.3 (2)
C2A—C3A—C4A	119.57 (19)	C20A—C21A—H21A	120.4
C2A—C3A—H3A	120.2	C22A—C21A—H21A	120.4
C4A—C3A—H3A	120.2	N4A—C22A—C21A	122.5 (2)
C12A—C4A—C3A	117.17 (19)	N4A—C22A—H22A	118.7
C12A—C4A—C5A	118.95 (19)	C21A—C22A—H22A	118.7
C3A—C4A—C5A	123.88 (19)	N4A—C23A—C19A	122.77 (19)
C6A—C5A—C4A	121.0 (2)	N4A—C23A—C24A	116.80 (17)
C6A—C5A—H5A	119.5	C19A—C23A—C24A	120.39 (18)
C4A—C5A—H5A	119.5	N3A—C24A—C16A	123.38 (19)
C5A—C6A—C7A	121.1 (2)	N3A—C24A—C23A	116.47 (17)
C5A—C6A—H6A	119.5	C16A—C24A—C23A	120.14 (18)
C7A—C6A—H6A	119.5	Cl3B—Zn1B—Cl2B	111.57 (3)
C11A—C7A—C8A	117.5 (2)	Cl3B—Zn1B—Cl4B	107.54 (4)
C11A—C7A—C6A	118.7 (2)	Cl2B—Zn1B—Cl4B	109.89 (4)
C8A—C7A—C6A	123.7 (2)	Cl3B—Zn1B—Cl1B	107.97 (3)
C9A—C8A—C7A	119.0 (2)	Cl2B—Zn1B—Cl1B	109.29 (3)
C9A—C8A—H8A	120.5	Cl4B—Zn1B—Cl1B	110.56 (3)
C7A—C8A—H8A	120.5	H1OW—O1W—H2OW	105 (2)
C8A—C9A—C10A	119.7 (2)

C12A—N1A—C1A—C2A	0.6 (3)	C24A—N3A—C13A—C14A	−0.4 (3)
Cr1A—N1A—C1A—C2A	−177.22 (15)	Cr1A—N3A—C13A—C14A	−179.76 (16)
N1A—C1A—C2A—C3A	1.1 (3)	N3A—C13A—C14A—C15A	0.1 (3)
C1A—C2A—C3A—C4A	−1.4 (3)	C13A—C14A—C15A—C16A	0.5 (3)
C2A—C3A—C4A—C12A	0.0 (3)	C14A—C15A—C16A—C24A	−0.8 (3)
C2A—C3A—C4A—C5A	179.1 (2)	C14A—C15A—C16A—C17A	178.6 (2)
C12A—C4A—C5A—C6A	−2.3 (3)	C24A—C16A—C17A—C18A	1.3 (3)
C3A—C4A—C5A—C6A	178.6 (2)	C15A—C16A—C17A—C18A	−178.1 (2)
C4A—C5A—C6A—C7A	−0.6 (4)	C16A—C17A—C18A—C19A	−1.2 (3)
C5A—C6A—C7A—C11A	2.5 (3)	C17A—C18A—C19A—C23A	−0.1 (3)
C5A—C6A—C7A—C8A	−176.9 (2)	C17A—C18A—C19A—C20A	179.0 (2)
C11A—C7A—C8A—C9A	1.4 (3)	C23A—C19A—C20A—C21A	1.6 (3)
C6A—C7A—C8A—C9A	−179.1 (2)	C18A—C19A—C20A—C21A	−177.5 (2)
C7A—C8A—C9A—C10A	0.2 (4)	C19A—C20A—C21A—C22A	−1.4 (4)
C11A—N2A—C10A—C9A	1.1 (3)	C23A—N4A—C22A—C21A	1.9 (3)
Cr1A—N2A—C10A—C9A	175.09 (18)	Cr1A—N4A—C22A—C21A	177.73 (17)
C8A—C9A—C10A—N2A	−1.5 (4)	C20A—C21A—C22A—N4A	−0.3 (4)
C10A—N2A—C11A—C7A	0.7 (3)	C22A—N4A—C23A—C19A	−1.7 (3)
Cr1A—N2A—C11A—C7A	−174.29 (16)	Cr1A—N4A—C23A—C19A	−178.16 (15)
C10A—N2A—C11A—C12A	−179.22 (19)	C22A—N4A—C23A—C24A	176.20 (18)
Cr1A—N2A—C11A—C12A	5.8 (2)	Cr1A—N4A—C23A—C24A	−0.2 (2)
C8A—C7A—C11A—N2A	−1.9 (3)	C20A—C19A—C23A—N4A	0.0 (3)
C6A—C7A—C11A—N2A	178.62 (19)	C18A—C19A—C23A—N4A	179.15 (19)
C8A—C7A—C11A—C12A	177.99 (19)	C20A—C19A—C23A—C24A	−177.84 (19)
C6A—C7A—C11A—C12A	−1.5 (3)	C18A—C19A—C23A—C24A	1.3 (3)
C1A—N1A—C12A—C4A	−2.0 (3)	C13A—N3A—C24A—C16A	0.0 (3)
Cr1A—N1A—C12A—C4A	176.07 (15)	Cr1A—N3A—C24A—C16A	179.48 (15)
C1A—N1A—C12A—C11A	177.33 (18)	C13A—N3A—C24A—C23A	−178.80 (18)
Cr1A—N1A—C12A—C11A	−4.6 (2)	Cr1A—N3A—C24A—C23A	0.7 (2)
C3A—C4A—C12A—N1A	1.7 (3)	C15A—C16A—C24A—N3A	0.6 (3)
C5A—C4A—C12A—N1A	−177.40 (19)	C17A—C16A—C24A—N3A	−178.90 (19)
C3A—C4A—C12A—C11A	−177.60 (18)	C15A—C16A—C24A—C23A	179.37 (18)
C5A—C4A—C12A—C11A	3.3 (3)	C17A—C16A—C24A—C23A	−0.1 (3)
N2A—C11A—C12A—N1A	−0.9 (3)	N4A—C23A—C24A—N3A	−0.3 (3)
C7A—C11A—C12A—N1A	179.23 (18)	C19A—C23A—C24A—N3A	177.69 (18)
N2A—C11A—C12A—C4A	178.51 (18)	N4A—C23A—C24A—C16A	−179.14 (18)
C7A—C11A—C12A—C4A	−1.4 (3)	C19A—C23A—C24A—C16A	−1.2 (3)

Hydrogen-bond geometry (Å, º) top

D—H···A	D—H	H···A	D···A	D—H···A
O1A—H1O1···O1W	0.83 (1)	1.72 (1)	2.536 (3)	170 (3)
O1A—H2O1···Cl1B	0.84 (1)	2.20 (1)	3.0208 (19)	168 (3)
O1W—H2OW···Cl2B	0.86 (1)	2.39 (2)	3.172 (3)	153 (3)
O1W—H1OW···Cl4Bⁱ	0.85 (1)	2.31 (1)	3.155 (2)	170 (3)

Symmetry code: (i) x, −y+1/2, z−1/2.

Hydrogen-bond geometry (Å, º) top

D—H···A	D—H	H···A	D···A	D—H···A
O1A—H1O1···O1W	0.829 (10)	1.715 (11)	2.536 (3)	170 (3)
O1A—H2O1···Cl1B	0.839 (10)	2.195 (12)	3.0208 (19)	168 (3)
O1W—H2OW···Cl2B	0.855 (10)	2.388 (17)	3.172 (3)	153 (3)
O1W—H1OW···Cl4Bⁱ	0.851 (10)	2.314 (13)	3.155 (2)	170 (3)

Symmetry code: (i) x, −y+1/2, z−1/2.

Experimental details

Crystal data
Chemical formula	[CrCl(C₁₂H₈N₂)₂(H₂O)][ZnCl₄]·H₂O
M_r	691.06
Crystal system, space group	Monoclinic, P2₁/c
Temperature (K)	100
a, b, c (Å)	8.2710 (17), 19.535 (4), 16.934 (3)
β (°)	100.55 (3)
V (Å³)	2689.8 (10)
Z	4
Radiation type	Synchrotron, λ = 0.62998 Å
µ (mm⁻¹)	1.30
Crystal size (mm)	0.10 × 0.08 × 0.05

Data collection
Diffractometer	ADSC Q210 CCD area-detector diffractometer
Absorption correction	Empirical (using intensity measurements) (HKL3000sm SCALEPACK; Otwinowski & Minor, 1997)
T_min, T_max	0.881, 0.938
No. of measured, independent and observed [I > 2σ(I)] reflections	25530, 7554, 7016
R_int	0.045
(sin θ/λ)_max (Å⁻¹)	0.696

Refinement
R[F² > 2σ(F²)], wR(F²), S	0.040, 0.107, 1.02
No. of reflections	7554
No. of parameters	348
No. of restraints	6
H-atom treatment	H atoms treated by a mixture of independent and constrained refinement
Δρ_max, Δρ_min (e Å⁻³)	1.96, −0.87

Computer programs: PAL ADSC Quantum-210 ADX (Arvai & Nielsen, 1983), HKL3000sm (Otwinowski & Minor, 1997), SHELXT2014/5 (Sheldrick, 2015a), SHELXL2014/7 (Sheldrick, 2015b), DIAMOND (Putz & Brandenburg, 2014), publCIF (Westrip, 2010).

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Crystal structure of cis-aqua­chlorido­bis­(1,10-phenanthroline-κ2N,N′)chromium(III) tetra­chlorido­zincate monohydrate from synchrotron data

Supporting information

Key indicators

checkCIF/PLATON results

Crystal structure of cis-aquachloridobis(1,10-phenanthroline-κ²N,N′)chromium(III) tetrachloridozincate monohydrate from synchrotron data