Bis[trans-di-fluorido-tetra-kis-(pyridine-κN)chromium(III)] sodium tetra-chlorido-zincate perchlorate from synchrotron data.

The title salt, Na[CrF2(C5H5N)4]2[ZnCl4]ClO4, consists of two cationic Cr(III) complexes, an Na(+) cation, one [ZnCl4](2-) anion and one ClO4 (-) anion. The Cr(III) atoms are coordinated by four pyridine (py) N atoms and two F atoms in a trans arrangement, displaying a distorted octa-hedral geometry. The mean Cr-N(py) and Cr-F bond lengths are 2.086 (8) and 1.864 (14) Å, respectively. The [ZnCl4](2-) anion has a distorted tetra-hedral geometry. The most notable feature of the crystal packing is the formation of weak pyridine-perchlorate C-H⋯O hydrogen bonds, resulting in supra-molecular chains along the b-axis direction. The perchlorate anion was disordered over two sets of sites in a 0.868 (3):0.132 (3) ratio.

Related literature

For the synthesis of trans-[Cr(py)4F2]NO3, see: Glerup et al. (1970 ▶). For the structures of trans-[Cr(py)4F2]ClO4 and trans-[Cr(py)4F2]PF6, see: Moon & Choi (2013 ▶); Fochi et al. (1991 ▶). Chromium(III)-doped crystals are promising materials for tunable solid state lasers in the spectral region between 600 and 1100 nm, see: Powell (1998 ▶).

Experimental

Crystal data

Na[CrF2(C5H5N)4]2[ZnCl4]ClO4

M = 1142.41

Orthorhombic,

a = 25.397 (5) Å

b = 14.600 (3) Å

c = 25.510 (5) Å

V = 9459 (3) Å3

Z = 8

Synchrotron radiation

λ = 0.62998 Å

μ = 0.94 mm−1

T = 100 K

0.20 × 0.15 × 0.10 mm

Data collection

ADSC Q210 CCD area-detector diffractometer

Absorption correction: empirical (HKL3000sm; Otwinowski & Minor, 1997 ▶) T min = 0.835, T max = 0.912

86381 measured reflections

13152 independent reflections

12355 reflections with I > 2σ(I)

R int = 0.050

Refinement

R[F 2 > 2σ(F 2)] = 0.047

wR(F 2) = 0.136

S = 1.05

13152 reflections

605 parameters

6 restraints

H-atom parameters constrained

Δρmax = 1.25 e Å−3

Δρmin = −1.99 e Å−3

Data collection: PAL ADSC Quantum-210 ADX (Arvai & Nielsen, 1983 ▶); cell refinement: HKL3000sm (Otwinowski & Minor, 1997 ▶); data reduction: HKL3000sm; program(s) used to solve structure: XS in SHELXS2014 (Sheldrick, 2008 ▶); program(s) used to refine structure: XL in SHELXL2014 (Sheldrick, 2008 ▶); molecular graphics: DIAMOND (Brandenburg, 2007 ▶); software used to prepare material for publication: WinGX (Farrugia, 2012 ▶).

Crystal structure: contains datablock(s) I, 70. DOI: 10.1107/S1600536814014408/tk5321sup1.cif

Structure factors: contains datablock(s) I. DOI: 10.1107/S1600536814014408/tk5321Isup2.hkl

CCDC reference: 1009068

Additional supporting information: crystallographic information; 3D view; checkCIF report

Na[CrF2(C5H5N)4]2[ZnCl4]ClO4	Dx = 1.604 Mg m−3
Mr = 1142.41	Synchrotron radiation, λ = 0.62998 Å
Orthorhombic, Pbca	Cell parameters from 237022 reflections
a = 25.397 (5) Å	θ = 0.4–33.6°
b = 14.600 (3) Å	µ = 0.94 mm−1
c = 25.510 (5) Å	T = 100 K
V = 9459 (3) Å3	Block, purple
Z = 8	0.20 × 0.15 × 0.10 mm
F(000) = 4624

ADSC Q210 CCD area-detector diffractometer	12355 reflections with I > 2σ(I)
Radiation source: PLSII 2D bending magnet	Rint = 0.050
ω scan	θmax = 26.0°, θmin = 2.0°
Absorption correction: empirical (using intensity measurements) (HKL3000sm; Otwinowski & Minor, 1997)	h = −35→35
Tmin = 0.835, Tmax = 0.912	k = −19→19
86381 measured reflections	l = −35→35
13152 independent reflections

Refinement on F2	6 restraints
Least-squares matrix: full	Hydrogen site location: inferred from neighbouring sites
R[F2 > 2σ(F2)] = 0.047	H-atom parameters constrained
wR(F2) = 0.136	w = 1/[σ2(Fo2) + (0.0773P)2 + 19.7848P] where P = (Fo2 + 2Fc2)/3
S = 1.05	(Δ/σ)max = 0.002
13152 reflections	Δρmax = 1.25 e Å−3
605 parameters	Δρmin = −1.99 e Å−3

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.

	x	y	z	Uiso*/Ueq	Occ. (<1)
Cr1	0.35117 (2)	0.76013 (2)	0.12316 (2)	0.00754 (8)
F1	0.30651 (4)	0.70701 (9)	0.17189 (5)	0.0118 (2)
F2	0.39507 (5)	0.81430 (9)	0.07234 (5)	0.0134 (2)
N1	0.37558 (7)	0.63065 (12)	0.09803 (7)	0.0116 (3)
N2	0.28923 (7)	0.75603 (12)	0.06915 (6)	0.0105 (3)
N3	0.32920 (6)	0.89005 (12)	0.14979 (6)	0.0099 (3)
N4	0.41194 (6)	0.75688 (12)	0.17755 (7)	0.0107 (3)
C1	0.35464 (10)	0.55497 (16)	0.12003 (9)	0.0188 (4)
H1	0.3272	0.5618	0.1451	0.023*
C2	0.37167 (12)	0.46750 (17)	0.10742 (10)	0.0258 (5)
H2	0.3556	0.4154	0.1230	0.031*
C3	0.41235 (11)	0.45702 (18)	0.07181 (10)	0.0268 (5)
H3	0.4258	0.3980	0.0637	0.032*
C4	0.43310 (10)	0.53502 (19)	0.04820 (11)	0.0252 (5)
H4	0.4603	0.5298	0.0228	0.030*
C5	0.41370 (9)	0.62005 (17)	0.06204 (9)	0.0180 (4)
H5	0.4278	0.6729	0.0455	0.022*
C6	0.29780 (8)	0.75294 (15)	0.01708 (8)	0.0143 (4)
H6	0.3330	0.7565	0.0045	0.017*
C7	0.25712 (9)	0.74470 (17)	−0.01887 (8)	0.0188 (4)
H7	0.2644	0.7426	−0.0554	0.023*
C8	0.20558 (9)	0.73955 (16)	−0.00069 (9)	0.0183 (4)
H8	0.1771	0.7332	−0.0246	0.022*
C9	0.19644 (8)	0.74378 (16)	0.05288 (9)	0.0165 (4)
H9	0.1616	0.7412	0.0663	0.020*
C10	0.23912 (8)	0.75180 (15)	0.08642 (8)	0.0133 (4)
H10	0.2328	0.7544	0.1231	0.016*
C11	0.35537 (8)	0.96612 (14)	0.13505 (8)	0.0125 (3)
H11	0.3854	0.9599	0.1132	0.015*
C12	0.33995 (9)	1.05350 (15)	0.15071 (8)	0.0165 (4)
H12	0.3592	1.1058	0.1397	0.020*
C13	0.29607 (9)	1.06300 (16)	0.18269 (9)	0.0177 (4)
H13	0.2845	1.1219	0.1935	0.021*
C14	0.26955 (9)	0.98475 (16)	0.19856 (9)	0.0173 (4)
H14	0.2395	0.9892	0.2206	0.021*
C15	0.28738 (8)	0.89998 (15)	0.18182 (8)	0.0137 (4)
H15	0.2694	0.8466	0.1934	0.016*
C16	0.40251 (9)	0.7286 (2)	0.22661 (9)	0.0259 (5)
H16	0.3673	0.7145	0.2362	0.031*
C17	0.44161 (10)	0.7191 (2)	0.26391 (10)	0.0288 (6)
H17	0.4332	0.6992	0.2984	0.035*
C18	0.49271 (9)	0.7387 (2)	0.25044 (10)	0.0245 (5)
H18	0.5204	0.7316	0.2751	0.029*
C19	0.50286 (10)	0.7688 (3)	0.20023 (11)	0.0441 (9)
H19	0.5378	0.7838	0.1899	0.053*
C20	0.46157 (9)	0.7770 (2)	0.16487 (9)	0.0301 (6)
H20	0.4689	0.7977	0.1303	0.036*
Cr2	0.65746 (2)	0.50377 (2)	0.11947 (2)	0.00778 (8)
F3	0.61676 (5)	0.45700 (9)	0.06534 (4)	0.0118 (2)
F4	0.70069 (5)	0.55143 (9)	0.17181 (5)	0.0130 (2)
N5	0.63053 (6)	0.63505 (12)	0.10134 (7)	0.0103 (3)
N6	0.59384 (6)	0.49421 (12)	0.17052 (6)	0.0098 (3)
N7	0.67945 (7)	0.37247 (12)	0.14187 (7)	0.0126 (3)
N8	0.72058 (7)	0.50992 (12)	0.06649 (6)	0.0104 (3)
C21	0.64820 (9)	0.70809 (15)	0.12802 (8)	0.0143 (4)
H21	0.6759	0.6999	0.1526	0.017*
C22	0.62733 (10)	0.79550 (16)	0.12082 (9)	0.0187 (4)
H22	0.6408	0.8459	0.1402	0.022*
C23	0.58692 (9)	0.80824 (16)	0.08526 (9)	0.0200 (4)
H23	0.5721	0.8672	0.0798	0.024*
C24	0.56850 (9)	0.73228 (17)	0.05761 (10)	0.0198 (4)
H24	0.5409	0.7387	0.0328	0.024*
C25	0.59096 (8)	0.64744 (15)	0.06679 (9)	0.0153 (4)
H25	0.5780	0.5959	0.0480	0.018*
C26	0.54766 (8)	0.45919 (16)	0.15431 (8)	0.0162 (4)
H26	0.5448	0.4377	0.1193	0.019*
C27	0.50407 (9)	0.4532 (2)	0.18677 (9)	0.0241 (5)
H27	0.4721	0.4272	0.1744	0.029*
C28	0.50789 (9)	0.4858 (2)	0.23773 (9)	0.0227 (5)
H28	0.4784	0.4837	0.2606	0.027*
C29	0.55529 (9)	0.52141 (19)	0.25454 (9)	0.0214 (5)
H29	0.5590	0.5435	0.2894	0.026*
C30	0.59751 (8)	0.52459 (16)	0.22017 (8)	0.0156 (4)
H30	0.6301	0.5490	0.2320	0.019*
C31	0.71928 (9)	0.35834 (16)	0.17617 (8)	0.0177 (4)
H31	0.7389	0.4096	0.1883	0.021*
C32	0.73252 (10)	0.27212 (18)	0.19426 (9)	0.0222 (5)
H32	0.7609	0.2642	0.2180	0.027*
C33	0.70374 (10)	0.19765 (18)	0.17718 (10)	0.0248 (5)
H33	0.7118	0.1378	0.1893	0.030*
C34	0.66268 (10)	0.21171 (16)	0.14187 (11)	0.0229 (5)
H34	0.6425	0.1614	0.1296	0.027*
C35	0.65162 (9)	0.29982 (16)	0.12486 (9)	0.0169 (4)
H35	0.6237	0.3092	0.1006	0.020*
C36	0.77078 (8)	0.51247 (15)	0.08380 (8)	0.0136 (4)
H36	0.7771	0.5151	0.1205	0.016*
C37	0.81361 (8)	0.51134 (16)	0.04979 (9)	0.0164 (4)
H37	0.8486	0.5123	0.0631	0.020*
C38	0.80443 (8)	0.50876 (16)	−0.00376 (9)	0.0174 (4)
H38	0.8330	0.5078	−0.0278	0.021*
C39	0.75289 (9)	0.50755 (16)	−0.02167 (8)	0.0171 (4)
H39	0.7457	0.5069	−0.0582	0.020*
C40	0.71206 (8)	0.50729 (15)	0.01433 (8)	0.0137 (4)
H40	0.6768	0.5052	0.0018	0.016*
Cl1P	0.63013 (3)	−0.20630 (5)	0.28660 (3)	0.01264 (18)	0.868 (3)
O1P	0.60224 (9)	−0.23420 (16)	0.33334 (8)	0.0262 (5)	0.868 (3)
O2P	0.68283 (8)	−0.1857 (2)	0.30024 (11)	0.0374 (7)	0.868 (3)
O3P	0.62633 (11)	−0.2764 (3)	0.24867 (13)	0.0354 (7)	0.868 (3)
O4P	0.60397 (9)	−0.12621 (15)	0.26743 (10)	0.0370 (5)	0.868 (3)
Cl2P	0.6450 (2)	−0.1831 (4)	0.2710 (2)	0.0221 (12)	0.132 (3)
O5P	0.6630 (6)	−0.2113 (10)	0.3260 (5)	0.0221 (12)	0.132 (3)
O6P	0.6833 (5)	−0.1475 (10)	0.2396 (5)	0.0221 (12)	0.132 (3)
O7P	0.6415 (8)	−0.2796 (17)	0.2504 (9)	0.0221 (12)	0.132 (3)
O8P	0.60397 (9)	−0.12621 (15)	0.26743 (10)	0.0370 (5)	0.132 (3)
Zn1	0.51089 (2)	0.13481 (2)	0.06065 (2)	0.01240 (7)
Cl1	0.52526 (2)	0.28484 (4)	0.05651 (2)	0.02034 (12)
Cl2	0.42603 (2)	0.10088 (4)	0.04318 (2)	0.02115 (12)
Cl3	0.55209 (11)	0.09300 (14)	−0.00286 (9)	0.1300 (9)
Cl4	0.54386 (3)	0.04804 (5)	0.12572 (2)	0.03005 (14)
Na1P	0.65188 (10)	−0.00419 (16)	0.19280 (11)	0.0856 (7)

	U11	U22	U33	U12	U13	U23
Cr1	0.00589 (14)	0.00984 (15)	0.00688 (14)	−0.00199 (10)	0.00172 (9)	0.00211 (10)
F1	0.0085 (5)	0.0164 (6)	0.0106 (5)	−0.0028 (4)	0.0025 (4)	0.0051 (4)
F2	0.0136 (5)	0.0156 (6)	0.0110 (5)	−0.0050 (4)	0.0066 (4)	0.0024 (4)
N1	0.0108 (7)	0.0129 (8)	0.0111 (7)	0.0001 (6)	−0.0006 (6)	0.0004 (6)
N2	0.0108 (7)	0.0113 (8)	0.0093 (7)	−0.0014 (6)	−0.0008 (6)	0.0016 (6)
N3	0.0088 (7)	0.0130 (8)	0.0079 (7)	−0.0006 (6)	−0.0003 (5)	0.0010 (6)
N4	0.0066 (7)	0.0150 (8)	0.0106 (7)	−0.0008 (6)	0.0008 (5)	0.0003 (6)
C1	0.0266 (11)	0.0125 (10)	0.0173 (9)	−0.0004 (8)	0.0012 (8)	0.0049 (7)
C2	0.0433 (15)	0.0134 (10)	0.0208 (11)	0.0032 (10)	−0.0058 (10)	0.0040 (8)
C3	0.0364 (14)	0.0183 (11)	0.0258 (11)	0.0116 (10)	−0.0128 (10)	−0.0055 (9)
C4	0.0216 (11)	0.0263 (13)	0.0279 (12)	0.0073 (9)	−0.0003 (9)	−0.0106 (10)
C5	0.0152 (9)	0.0196 (11)	0.0192 (10)	−0.0004 (8)	0.0036 (7)	−0.0043 (8)
C6	0.0157 (9)	0.0166 (9)	0.0107 (8)	−0.0003 (7)	−0.0004 (7)	0.0011 (7)
C7	0.0217 (10)	0.0238 (11)	0.0110 (9)	0.0020 (8)	−0.0039 (8)	−0.0011 (8)
C8	0.0183 (10)	0.0188 (10)	0.0179 (10)	0.0003 (8)	−0.0083 (8)	0.0003 (8)
C9	0.0124 (9)	0.0179 (10)	0.0193 (10)	−0.0018 (7)	−0.0036 (7)	0.0026 (8)
C10	0.0108 (8)	0.0169 (9)	0.0121 (8)	−0.0023 (7)	−0.0009 (7)	0.0023 (7)
C11	0.0143 (8)	0.0125 (9)	0.0107 (8)	−0.0023 (7)	−0.0007 (7)	0.0015 (7)
C12	0.0221 (10)	0.0116 (9)	0.0157 (9)	−0.0014 (7)	−0.0031 (7)	0.0010 (7)
C13	0.0216 (10)	0.0156 (10)	0.0157 (9)	0.0058 (8)	−0.0048 (8)	−0.0015 (7)
C14	0.0149 (9)	0.0210 (10)	0.0160 (9)	0.0048 (8)	0.0013 (7)	−0.0020 (8)
C15	0.0115 (8)	0.0174 (10)	0.0122 (8)	0.0003 (7)	0.0023 (7)	0.0005 (7)
C16	0.0096 (9)	0.0503 (16)	0.0177 (10)	−0.0052 (9)	−0.0016 (8)	0.0148 (10)
C17	0.0160 (10)	0.0515 (17)	0.0188 (11)	−0.0053 (10)	−0.0057 (8)	0.0147 (11)
C18	0.0106 (9)	0.0430 (15)	0.0197 (10)	0.0016 (9)	−0.0049 (8)	−0.0003 (10)
C19	0.0085 (10)	0.104 (3)	0.0196 (12)	−0.0125 (14)	−0.0014 (9)	0.0057 (15)
C20	0.0097 (9)	0.067 (2)	0.0133 (10)	−0.0130 (11)	0.0004 (8)	0.0044 (11)
Cr2	0.00645 (14)	0.01014 (15)	0.00675 (14)	−0.00042 (10)	−0.00057 (9)	−0.00142 (10)
F3	0.0122 (5)	0.0140 (6)	0.0091 (5)	−0.0032 (4)	−0.0019 (4)	−0.0029 (4)
F4	0.0099 (5)	0.0185 (6)	0.0107 (5)	−0.0007 (4)	−0.0030 (4)	−0.0032 (4)
N5	0.0089 (7)	0.0115 (8)	0.0104 (7)	−0.0010 (5)	0.0010 (6)	−0.0006 (6)
N6	0.0087 (7)	0.0121 (8)	0.0087 (7)	0.0002 (5)	0.0001 (5)	−0.0011 (5)
N7	0.0129 (7)	0.0142 (8)	0.0108 (7)	0.0039 (6)	0.0027 (6)	0.0009 (6)
N8	0.0084 (7)	0.0135 (8)	0.0093 (7)	0.0004 (6)	0.0001 (5)	−0.0008 (6)
C21	0.0181 (9)	0.0131 (10)	0.0118 (8)	−0.0020 (7)	0.0016 (7)	−0.0024 (7)
C22	0.0269 (11)	0.0132 (10)	0.0159 (9)	−0.0014 (8)	0.0053 (8)	−0.0030 (7)
C23	0.0223 (10)	0.0151 (10)	0.0225 (10)	0.0050 (8)	0.0086 (8)	0.0032 (8)
C24	0.0147 (9)	0.0181 (11)	0.0264 (11)	0.0019 (8)	−0.0014 (8)	0.0056 (8)
C25	0.0135 (9)	0.0147 (10)	0.0178 (9)	−0.0017 (7)	−0.0042 (7)	0.0016 (7)
C26	0.0122 (9)	0.0231 (11)	0.0134 (9)	−0.0065 (7)	0.0014 (7)	−0.0047 (7)
C27	0.0134 (9)	0.0409 (15)	0.0180 (10)	−0.0110 (9)	0.0028 (8)	−0.0065 (10)
C28	0.0137 (10)	0.0383 (14)	0.0160 (10)	−0.0030 (9)	0.0048 (7)	−0.0036 (9)
C29	0.0149 (9)	0.0369 (13)	0.0125 (9)	−0.0013 (9)	0.0033 (7)	−0.0077 (9)
C30	0.0114 (8)	0.0246 (11)	0.0110 (8)	−0.0010 (7)	0.0004 (7)	−0.0056 (8)
C31	0.0187 (10)	0.0213 (11)	0.0133 (9)	0.0069 (8)	0.0002 (7)	0.0007 (7)
C32	0.0254 (11)	0.0253 (12)	0.0160 (9)	0.0129 (9)	0.0025 (8)	0.0037 (8)
C33	0.0292 (12)	0.0207 (11)	0.0244 (11)	0.0121 (9)	0.0109 (9)	0.0073 (9)
C34	0.0245 (11)	0.0129 (10)	0.0312 (12)	0.0022 (8)	0.0087 (9)	0.0006 (9)
C35	0.0154 (9)	0.0139 (10)	0.0214 (10)	0.0021 (7)	0.0051 (7)	0.0000 (7)
C36	0.0094 (8)	0.0194 (10)	0.0121 (8)	0.0003 (7)	−0.0004 (7)	−0.0005 (7)
C37	0.0087 (8)	0.0232 (11)	0.0172 (9)	0.0015 (7)	0.0011 (7)	0.0013 (8)
C38	0.0135 (9)	0.0224 (11)	0.0162 (9)	0.0036 (8)	0.0060 (7)	0.0009 (8)
C39	0.0168 (9)	0.0239 (11)	0.0104 (8)	0.0016 (8)	0.0033 (7)	0.0007 (7)
C40	0.0120 (8)	0.0185 (10)	0.0105 (8)	0.0009 (7)	−0.0001 (7)	0.0001 (7)
Cl1P	0.0113 (3)	0.0140 (3)	0.0127 (3)	0.0026 (2)	−0.0047 (2)	−0.0003 (2)
O1P	0.0341 (11)	0.0252 (11)	0.0193 (9)	−0.0025 (9)	0.0063 (8)	0.0046 (8)
O2P	0.0090 (9)	0.0603 (17)	0.0430 (14)	−0.0026 (10)	−0.0084 (9)	−0.0126 (12)
O3P	0.0316 (15)	0.0470 (16)	0.0276 (12)	0.0024 (15)	−0.0071 (13)	−0.0239 (11)
O4P	0.0288 (10)	0.0346 (12)	0.0476 (13)	0.0188 (9)	0.0081 (9)	0.0216 (10)
Cl2P	0.0194 (14)	0.0263 (14)	0.0205 (14)	−0.0016 (9)	−0.0010 (9)	−0.0038 (9)
O5P	0.0194 (14)	0.0263 (14)	0.0205 (14)	−0.0016 (9)	−0.0010 (9)	−0.0038 (9)
O6P	0.0194 (14)	0.0263 (14)	0.0205 (14)	−0.0016 (9)	−0.0010 (9)	−0.0038 (9)
O7P	0.0194 (14)	0.0263 (14)	0.0205 (14)	−0.0016 (9)	−0.0010 (9)	−0.0038 (9)
O8P	0.0288 (10)	0.0346 (12)	0.0476 (13)	0.0188 (9)	0.0081 (9)	0.0216 (10)
Zn1	0.01514 (13)	0.01067 (13)	0.01138 (12)	−0.00326 (8)	0.00344 (8)	−0.00087 (8)
Cl1	0.0246 (3)	0.0112 (2)	0.0252 (3)	−0.00530 (19)	−0.0023 (2)	−0.00346 (18)
Cl2	0.0145 (2)	0.0141 (2)	0.0348 (3)	−0.00498 (17)	0.0031 (2)	0.0015 (2)
Cl3	0.173 (2)	0.0881 (13)	0.1291 (17)	−0.0183 (13)	0.0785 (16)	−0.0087 (11)
Cl4	0.0477 (4)	0.0215 (3)	0.0209 (3)	0.0029 (3)	−0.0073 (2)	0.0041 (2)
Na1P	0.0897 (16)	0.0696 (14)	0.0974 (17)	−0.0081 (12)	0.0211 (13)	0.0102 (12)

Cr1—F1	1.8532 (12)	N6—C26	1.344 (3)
Cr1—F2	1.8838 (12)	N6—C30	1.345 (2)
Cr1—N4	2.0759 (17)	N7—C35	1.346 (3)
Cr1—N1	2.0902 (18)	N7—C31	1.353 (3)
Cr1—N3	2.0906 (18)	N8—C40	1.349 (2)
Cr1—N2	2.0920 (17)	N8—C36	1.350 (2)
N1—C5	1.343 (3)	C21—C22	1.394 (3)
N1—C1	1.349 (3)	C21—H21	0.9500
N2—C6	1.347 (3)	C22—C23	1.382 (3)
N2—C10	1.348 (2)	C22—H22	0.9500
N3—C11	1.348 (3)	C23—C24	1.395 (4)
N3—C15	1.348 (2)	C23—H23	0.9500
N4—C20	1.334 (3)	C24—C25	1.384 (3)
N4—C16	1.339 (3)	C24—H24	0.9500
C1—C2	1.386 (3)	C25—H25	0.9500
C1—H1	0.9500	C26—C27	1.385 (3)
C2—C3	1.384 (4)	C26—H26	0.9500
C2—H2	0.9500	C27—C28	1.388 (3)
C3—C4	1.392 (4)	C27—H27	0.9500
C3—H3	0.9500	C28—C29	1.380 (3)
C4—C5	1.382 (3)	C28—H28	0.9500
C4—H4	0.9500	C29—C30	1.386 (3)
C5—H5	0.9500	C29—H29	0.9500
C6—C7	1.387 (3)	C30—H30	0.9500
C6—H6	0.9500	C31—C32	1.382 (3)
C7—C8	1.391 (3)	C31—H31	0.9500
C7—H7	0.9500	C32—C33	1.381 (4)
C8—C9	1.388 (3)	C32—H32	0.9500
C8—H8	0.9500	C33—C34	1.393 (4)
C9—C10	1.386 (3)	C33—H33	0.9500
C9—H9	0.9500	C34—C35	1.386 (3)
C10—H10	0.9500	C34—H34	0.9500
C11—C12	1.393 (3)	C35—H35	0.9500
C11—H11	0.9500	C36—C37	1.391 (3)
C12—C13	1.388 (3)	C36—H36	0.9500
C12—H12	0.9500	C37—C38	1.386 (3)
C13—C14	1.387 (3)	C37—H37	0.9500
C13—H13	0.9500	C38—C39	1.387 (3)
C14—C15	1.385 (3)	C38—H38	0.9500
C14—H14	0.9500	C39—C40	1.385 (3)
C15—H15	0.9500	C39—H39	0.9500
C16—C17	1.382 (3)	C40—H40	0.9500
C16—H16	0.9500	Cl1P—O3P	1.412 (3)
C17—C18	1.372 (3)	Cl1P—O2P	1.415 (2)
C17—H17	0.9500	Cl1P—O4P	1.431 (2)
C18—C19	1.379 (4)	Cl1P—O1P	1.445 (2)
C18—H18	0.9500	O4P—Na1P	2.877 (3)
C19—C20	1.388 (3)	Cl2P—O6P	1.362 (15)
C19—H19	0.9500	Cl2P—O7P	1.51 (3)
C20—H20	0.9500	Cl2P—O5P	1.531 (15)
Cr2—F3	1.8552 (12)	Cl2P—Na1P	3.291 (8)
Cr2—F4	1.8634 (12)	O6P—Na1P	2.537 (15)
Cr2—N7	2.0769 (18)	Zn1—Cl3	2.0228 (19)
Cr2—N6	2.0801 (17)	Zn1—Cl1	2.2232 (7)
Cr2—N5	2.0868 (18)	Zn1—Cl4	2.2499 (7)
Cr2—N8	2.0986 (17)	Zn1—Cl2	2.2558 (7)
N5—C21	1.342 (3)	Cl4—Na1P	3.322 (3)
N5—C25	1.349 (3)
F1—Cr1—F2	178.47 (6)	N6—Cr2—N8	178.11 (7)
F1—Cr1—N4	89.83 (6)	N5—Cr2—N8	93.92 (7)
F2—Cr1—N4	91.70 (6)	C21—N5—C25	118.28 (19)
F1—Cr1—N1	90.50 (6)	C21—N5—Cr2	120.52 (14)
F2—Cr1—N1	89.61 (6)	C25—N5—Cr2	120.81 (14)
N4—Cr1—N1	87.93 (7)	C26—N6—C30	118.39 (18)
F1—Cr1—N3	89.90 (6)	C26—N6—Cr2	120.70 (14)
F2—Cr1—N3	90.04 (6)	C30—N6—Cr2	120.90 (14)
N4—Cr1—N3	90.12 (7)	C35—N7—C31	118.73 (19)
N1—Cr1—N3	178.00 (7)	C35—N7—Cr2	119.82 (15)
F1—Cr1—N2	88.25 (6)	C31—N7—Cr2	121.30 (15)
F2—Cr1—N2	90.22 (6)	C40—N8—C36	118.38 (17)
N4—Cr1—N2	176.95 (7)	C40—N8—Cr2	120.77 (14)
N1—Cr1—N2	89.72 (7)	C36—N8—Cr2	120.79 (13)
N3—Cr1—N2	92.25 (7)	N5—C21—C22	122.2 (2)
C5—N1—C1	118.3 (2)	N5—C21—H21	118.9
C5—N1—Cr1	121.84 (15)	C22—C21—H21	118.9
C1—N1—Cr1	119.77 (15)	C23—C22—C21	119.5 (2)
C6—N2—C10	118.25 (17)	C23—C22—H22	120.3
C6—N2—Cr1	121.93 (14)	C21—C22—H22	120.3
C10—N2—Cr1	119.74 (13)	C22—C23—C24	118.3 (2)
C11—N3—C15	117.97 (18)	C22—C23—H23	120.9
C11—N3—Cr1	121.69 (14)	C24—C23—H23	120.9
C15—N3—Cr1	120.33 (14)	C25—C24—C23	119.2 (2)
C20—N4—C16	117.59 (19)	C25—C24—H24	120.4
C20—N4—Cr1	122.37 (15)	C23—C24—H24	120.4
C16—N4—Cr1	119.92 (14)	N5—C25—C24	122.5 (2)
N1—C1—C2	122.4 (2)	N5—C25—H25	118.7
N1—C1—H1	118.8	C24—C25—H25	118.7
C2—C1—H1	118.8	N6—C26—C27	122.5 (2)
C3—C2—C1	119.1 (2)	N6—C26—H26	118.8
C3—C2—H2	120.4	C27—C26—H26	118.8
C1—C2—H2	120.4	C26—C27—C28	118.8 (2)
C2—C3—C4	118.4 (2)	C26—C27—H27	120.6
C2—C3—H3	120.8	C28—C27—H27	120.6
C4—C3—H3	120.8	C29—C28—C27	118.8 (2)
C5—C4—C3	119.3 (2)	C29—C28—H28	120.6
C5—C4—H4	120.3	C27—C28—H28	120.6
C3—C4—H4	120.3	C28—C29—C30	119.4 (2)
N1—C5—C4	122.4 (2)	C28—C29—H29	120.3
N1—C5—H5	118.8	C30—C29—H29	120.3
C4—C5—H5	118.8	N6—C30—C29	122.08 (19)
N2—C6—C7	122.3 (2)	N6—C30—H30	119.0
N2—C6—H6	118.8	C29—C30—H30	119.0
C7—C6—H6	118.8	N7—C31—C32	122.4 (2)
C6—C7—C8	119.1 (2)	N7—C31—H31	118.8
C6—C7—H7	120.5	C32—C31—H31	118.8
C8—C7—H7	120.5	C33—C32—C31	118.9 (2)
C9—C8—C7	118.90 (19)	C33—C32—H32	120.6
C9—C8—H8	120.5	C31—C32—H32	120.6
C7—C8—H8	120.5	C32—C33—C34	119.0 (2)
C10—C9—C8	118.8 (2)	C32—C33—H33	120.5
C10—C9—H9	120.6	C34—C33—H33	120.5
C8—C9—H9	120.6	C35—C34—C33	119.4 (2)
N2—C10—C9	122.72 (19)	C35—C34—H34	120.3
N2—C10—H10	118.6	C33—C34—H34	120.3
C9—C10—H10	118.6	N7—C35—C34	121.6 (2)
N3—C11—C12	122.42 (19)	N7—C35—H35	119.2
N3—C11—H11	118.8	C34—C35—H35	119.2
C12—C11—H11	118.8	N8—C36—C37	122.27 (19)
C13—C12—C11	119.1 (2)	N8—C36—H36	118.9
C13—C12—H12	120.5	C37—C36—H36	118.9
C11—C12—H12	120.5	C38—C37—C36	118.91 (19)
C14—C13—C12	118.6 (2)	C38—C37—H37	120.5
C14—C13—H13	120.7	C36—C37—H37	120.5
C12—C13—H13	120.7	C37—C38—C39	118.92 (19)
C15—C14—C13	119.2 (2)	C37—C38—H38	120.5
C15—C14—H14	120.4	C39—C38—H38	120.5
C13—C14—H14	120.4	C40—C39—C38	119.2 (2)
N3—C15—C14	122.7 (2)	C40—C39—H39	120.4
N3—C15—H15	118.6	C38—C39—H39	120.4
C14—C15—H15	118.6	N8—C40—C39	122.26 (19)
N4—C16—C17	123.1 (2)	N8—C40—H40	118.9
N4—C16—H16	118.5	C39—C40—H40	118.9
C17—C16—H16	118.5	O3P—Cl1P—O2P	112.79 (16)
C18—C17—C16	119.1 (2)	O3P—Cl1P—O4P	109.07 (18)
C18—C17—H17	120.5	O2P—Cl1P—O4P	110.45 (17)
C16—C17—H17	120.5	O3P—Cl1P—O1P	109.10 (19)
C17—C18—C19	118.4 (2)	O2P—Cl1P—O1P	108.70 (16)
C17—C18—H18	120.8	O4P—Cl1P—O1P	106.53 (13)
C19—C18—H18	120.8	Cl1P—O4P—Na1P	122.39 (13)
C18—C19—C20	119.3 (2)	O6P—Cl2P—O7P	101.2 (11)
C18—C19—H19	120.3	O6P—Cl2P—O5P	115.5 (9)
C20—C19—H19	120.3	O7P—Cl2P—O5P	94.8 (11)
N4—C20—C19	122.5 (2)	O6P—Cl2P—Na1P	45.8 (6)
N4—C20—H20	118.7	O7P—Cl2P—Na1P	122.3 (10)
C19—C20—H20	118.7	O5P—Cl2P—Na1P	138.9 (6)
F3—Cr2—F4	177.55 (6)	Cl2P—O6P—Na1P	111.5 (8)
F3—Cr2—N7	90.85 (7)	Cl3—Zn1—Cl1	100.05 (6)
F4—Cr2—N7	89.38 (7)	Cl3—Zn1—Cl4	103.21 (9)
F3—Cr2—N6	90.48 (6)	Cl1—Zn1—Cl4	121.91 (3)
F4—Cr2—N6	91.96 (6)	Cl3—Zn1—Cl2	105.65 (9)
N7—Cr2—N6	88.54 (7)	Cl1—Zn1—Cl2	111.33 (2)
F3—Cr2—N5	89.46 (6)	Cl4—Zn1—Cl2	112.19 (3)
F4—Cr2—N5	90.51 (6)	Zn1—Cl4—Na1P	144.75 (5)
N7—Cr2—N5	175.43 (7)	O6P—Na1P—Cl2P	22.6 (3)
N6—Cr2—N5	86.89 (7)	O6P—Na1P—Cl4	133.7 (3)
F3—Cr2—N8	87.82 (6)	O4P—Na1P—Cl4	97.68 (9)
F4—Cr2—N8	89.74 (6)	Cl2P—Na1P—Cl4	116.80 (12)
N7—Cr2—N8	90.65 (7)
C5—N1—C1—C2	1.1 (3)	C21—C22—C23—C24	−0.1 (3)
Cr1—N1—C1—C2	−175.75 (19)	C22—C23—C24—C25	0.3 (3)
N1—C1—C2—C3	1.4 (4)	C21—N5—C25—C24	0.6 (3)
C1—C2—C3—C4	−2.8 (4)	Cr2—N5—C25—C24	173.43 (17)
C2—C3—C4—C5	1.9 (4)	C23—C24—C25—N5	−0.5 (3)
C1—N1—C5—C4	−2.1 (3)	C30—N6—C26—C27	−0.1 (4)
Cr1—N1—C5—C4	174.69 (18)	Cr2—N6—C26—C27	−178.8 (2)
C3—C4—C5—N1	0.6 (4)	N6—C26—C27—C28	1.0 (4)
C10—N2—C6—C7	−0.7 (3)	C26—C27—C28—C29	−1.3 (4)
Cr1—N2—C6—C7	176.06 (17)	C27—C28—C29—C30	0.7 (4)
N2—C6—C7—C8	0.1 (3)	C26—N6—C30—C29	−0.5 (3)
C6—C7—C8—C9	0.7 (3)	Cr2—N6—C30—C29	178.14 (19)
C7—C8—C9—C10	−0.8 (3)	C28—C29—C30—N6	0.2 (4)
C6—N2—C10—C9	0.5 (3)	C35—N7—C31—C32	0.2 (3)
Cr1—N2—C10—C9	−176.32 (17)	Cr2—N7—C31—C32	175.81 (17)
C8—C9—C10—N2	0.3 (3)	N7—C31—C32—C33	−0.7 (3)
C15—N3—C11—C12	−1.5 (3)	C31—C32—C33—C34	0.7 (3)
Cr1—N3—C11—C12	177.33 (15)	C32—C33—C34—C35	−0.2 (4)
N3—C11—C12—C13	0.0 (3)	C31—N7—C35—C34	0.3 (3)
C11—C12—C13—C14	0.9 (3)	Cr2—N7—C35—C34	−175.35 (17)
C12—C13—C14—C15	−0.4 (3)	C33—C34—C35—N7	−0.4 (3)
C11—N3—C15—C14	2.1 (3)	C40—N8—C36—C37	−0.8 (3)
Cr1—N3—C15—C14	−176.77 (16)	Cr2—N8—C36—C37	176.29 (17)
C13—C14—C15—N3	−1.2 (3)	N8—C36—C37—C38	0.9 (3)
C20—N4—C16—C17	−0.5 (4)	C36—C37—C38—C39	0.1 (3)
Cr1—N4—C16—C17	175.7 (2)	C37—C38—C39—C40	−1.2 (3)
N4—C16—C17—C18	−0.4 (5)	C36—N8—C40—C39	−0.3 (3)
C16—C17—C18—C19	1.1 (5)	Cr2—N8—C40—C39	−177.39 (17)
C17—C18—C19—C20	−1.0 (6)	C38—C39—C40—N8	1.3 (3)
C16—N4—C20—C19	0.6 (5)	O3P—Cl1P—O4P—Na1P	−79.1 (2)
Cr1—N4—C20—C19	−175.5 (3)	O2P—Cl1P—O4P—Na1P	45.3 (2)
C18—C19—C20—N4	0.1 (6)	O1P—Cl1P—O4P—Na1P	163.23 (16)
C25—N5—C21—C22	−0.5 (3)	O7P—Cl2P—O6P—Na1P	124.6 (10)
Cr2—N5—C21—C22	−173.30 (16)	O5P—Cl2P—O6P—Na1P	−134.5 (8)
N5—C21—C22—C23	0.2 (3)

D—H···A	D—H	H···A	D···A	D—H···A
C2—H2···O5Pi	0.95	2.31	3.237 (14)	165
C10—H10···O2Pii	0.95	2.49	3.352 (3)	151

Table 1

Hydrogen-bond geometry (Å, °)

D—H⋯A	D—H	H⋯A	D⋯A	D—H⋯A
C2—H2⋯O5P i	0.95	2.31	3.237 (14)	165
C10—H10⋯O2P ii	0.95	2.49	3.352 (3)	151

Symmetry codes: (i) ; (ii) .