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The structure of the cation in [Cr(C12H8N2)3](ClO4)3·H2O consists of the Cr atom bonded to the N atoms of the three 1,10-phenanthroline (phen) ligands, resulting in a distorted octahedral arrangement with the six Cr-N distances ranging from 2.040 (4) to 2.055 (4) Å. One of the perchlorate anions is disordered and is located around two special positions.

Supporting information

cif

Crystallographic Information File (CIF) https://doi.org/10.1107/S0108270100006107/qb0212sup1.cif
Contains datablocks global, I

hkl

Structure factor file (CIF format) https://doi.org/10.1107/S0108270100006107/qb0212Isup2.hkl
Contains datablock I

CCDC reference: 146083

Computing details top

Data collection: KappaCCD Software (Nonius, 1999); cell refinement: DENZO and SCALEPAK (Otwinowski & Minor, 1997); data reduction: DENZO and SCALEPAK; program(s) used to solve structure: SIR97 (Altomare et al., 1998); program(s) used to refine structure: SHELXL97 (Sheldrick, 1997); software used to prepare material for publication: WinGX (Farrugia, 1998).

(I) top
Crystal data top
[Cr(C12H8N2)3](ClO4)3·H2OF(000) = 3704
Mr = 908.98Dx = 1.629 Mg m3
Monoclinic, C2/cMo Kα radiation, λ = 0.71073 Å
a = 17.6320 (4) ÅCell parameters from 47108 reflections
b = 18.2840 (4) Åθ = 1.0–30.0°
c = 22.9980 (4) ŵ = 0.60 mm1
β = 91.2700 (14)°T = 100 K
V = 7412.4 (3) Å3Fragment, red–yellow
Z = 80.20 × 0.17 × 0.10 mm
Data collection top
KappaCCD
diffractometer
10833 independent reflections
Radiation source: fine-focus sealed tube4967 reflections with I > 2σ(I)
Graphite monochromatorRint = 0.049
φ and ω scans with κ offsetsθmax = 30.1°, θmin = 1.6°
Absorption correction: multi-scan
(SORTAV; Blessing, 1995)
h = 2424
Tmin = 0.79, Tmax = 0.94k = 2525
47108 measured reflectionsl = 3232
Refinement top
Refinement on F240 restraints
Least-squares matrix: fullH-atom parameters constrained
R[F2 > 2σ(F2)] = 0.075 w = 1/[σ2(Fo2) + (0.1132*P)2],
where P = (max(Fo2,0) + 2*Fc2)/3
wR(F2) = 0.241(Δ/σ)max = 0.001
S = 1.03Δρmax = 1.14 e Å3
10833 reflectionsΔρmin = 0.58 e Å3
586 parameters
Special details top

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

Fractional atomic coordinates and isotropic or equivalent isotropic displacement parameters (Å2) top
xyzUiso*/UeqOcc. (<1)
Cr10.72094 (4)0.02683 (4)0.37656 (3)0.0319 (2)
Cl10.45649 (7)0.13697 (7)0.46656 (5)0.0437 (3)
O110.4854 (2)0.0804 (2)0.42957 (16)0.0548 (10)
O120.4731 (2)0.2052 (2)0.4394 (2)0.0821 (15)
O130.37564 (18)0.12992 (19)0.47144 (15)0.0473 (9)
O140.4923 (3)0.1334 (4)0.52229 (18)0.117 (2)
Cl20.68383 (7)0.21587 (9)0.73064 (5)0.0518 (4)
O210.73669 (19)0.2070 (2)0.77732 (14)0.0485 (9)
O220.7216 (2)0.2423 (2)0.67984 (14)0.0539 (10)
O230.6226 (3)0.2614 (3)0.74633 (18)0.114 (2)
O240.6506 (2)0.1442 (3)0.71789 (18)0.0873 (16)
Cl30.94375 (16)0.01916 (18)0.07176 (12)0.0576 (8)0.486 (2)
O310.9015 (4)0.0778 (4)0.0919 (3)0.0521 (19)0.486 (2)
O320.8897 (5)0.0247 (5)0.0480 (3)0.078 (3)0.486 (2)
O330.9956 (6)0.0391 (6)0.0297 (4)0.102 (4)0.486 (2)
O340.9809 (8)0.0114 (7)0.1190 (5)0.130 (5)0.486 (2)
Cl41.00489 (17)0.09442 (19)0.16678 (13)0.0676 (9)0.514 (2)
O411.0516 (4)0.1485 (4)0.1726 (3)0.0483 (17)*0.514 (2)
O420.9398 (4)0.1160 (4)0.1338 (3)0.071 (2)0.514 (2)
O431.0366 (6)0.0317 (5)0.1411 (7)0.128 (5)0.514 (2)
O440.9820 (7)0.0740 (9)0.2218 (4)0.168 (7)0.514 (2)
O500.5873 (6)0.3942 (6)0.7921 (5)0.075 (3)0.53
O5010.5519 (7)0.4069 (9)0.7690 (5)0.100 (5)0.47
N10.69576 (19)0.0595 (2)0.45918 (15)0.0325 (8)
N20.8119 (2)0.0935 (2)0.39209 (14)0.0309 (8)
C10.8698 (2)0.1095 (3)0.35823 (19)0.0363 (10)
H10.87230.08670.32120.054*
C20.9268 (3)0.1584 (3)0.3748 (2)0.0443 (12)
H20.9670.16840.34920.067*
C30.9251 (3)0.1921 (3)0.4283 (2)0.0402 (11)
H30.96410.22540.43990.06*
C40.8646 (2)0.1767 (3)0.46594 (18)0.0338 (10)
C50.8575 (3)0.2061 (3)0.5229 (2)0.0406 (11)
H50.89460.23970.5370.061*
C60.7999 (3)0.1878 (3)0.5574 (2)0.0413 (11)
H60.79730.20860.59520.062*
C70.7422 (3)0.1373 (3)0.53808 (19)0.0362 (10)
C80.6833 (3)0.1125 (3)0.57227 (19)0.0384 (11)
H80.67760.13080.61060.058*
C90.6334 (3)0.0612 (3)0.55017 (19)0.0398 (11)
H90.59430.04240.57370.06*
C100.6404 (3)0.0370 (3)0.49325 (19)0.0367 (10)
H100.60430.00310.47810.055*
C110.7475 (2)0.1078 (2)0.48176 (17)0.0308 (9)
C120.8096 (2)0.1276 (3)0.44603 (17)0.0332 (10)
N30.6650 (2)0.1100 (2)0.33495 (15)0.0338 (8)
N40.7536 (2)0.0046 (2)0.29317 (16)0.0392 (9)
C130.6209 (3)0.1617 (3)0.3571 (2)0.0414 (11)
H130.61250.16210.39770.062*
C140.5864 (3)0.2160 (3)0.3216 (2)0.0524 (13)
H140.55540.25250.33840.079*
C150.5980 (3)0.2154 (3)0.2632 (2)0.0549 (15)
H150.57540.25230.23940.082*
C160.6426 (3)0.1613 (3)0.2377 (2)0.0478 (13)
C170.6566 (3)0.1531 (4)0.1765 (2)0.0584 (16)
H170.63450.18690.14980.088*
C180.7007 (4)0.0979 (4)0.1561 (2)0.0613 (17)
H180.70810.09370.11540.092*
C190.7357 (3)0.0469 (3)0.1944 (2)0.0523 (15)
C200.7831 (3)0.0103 (4)0.1769 (2)0.0623 (18)
H200.79360.0160.13680.094*
C210.8143 (4)0.0578 (4)0.2162 (3)0.0631 (17)
H210.84680.0960.2040.095*
C220.7980 (3)0.0497 (3)0.2738 (2)0.0495 (13)
H220.81890.08350.30110.074*
C230.7224 (3)0.0523 (3)0.25373 (19)0.0415 (12)
C240.6761 (3)0.1085 (3)0.2753 (2)0.0434 (12)
N50.6305 (2)0.0423 (2)0.36434 (15)0.0314 (8)
N60.7685 (2)0.0666 (2)0.40930 (16)0.0371 (9)
C250.5617 (2)0.0295 (3)0.34095 (17)0.0342 (10)
H250.54820.01960.3320.051*
C260.5090 (3)0.0842 (3)0.32908 (19)0.0381 (11)
H260.46090.07260.31210.057*
C270.5275 (3)0.1547 (3)0.34218 (19)0.0437 (12)
H270.49220.19270.33360.065*
C280.5980 (3)0.1721 (3)0.36824 (19)0.0384 (11)
C290.6222 (3)0.2429 (3)0.3854 (2)0.0475 (13)
H290.58930.28340.37870.071*
C300.6900 (3)0.2540 (3)0.4107 (2)0.0483 (13)
H300.70330.30210.42280.072*
C310.7432 (3)0.1964 (3)0.4203 (2)0.0433 (12)
C320.8150 (3)0.2049 (3)0.4456 (2)0.0510 (13)
H320.83190.25190.45770.077*
C330.8614 (3)0.1451 (3)0.4528 (2)0.0561 (15)
H330.91010.15070.47070.084*
C340.8371 (3)0.0758 (3)0.4339 (2)0.0475 (12)
H340.86990.03490.43860.071*
C350.7219 (3)0.1254 (3)0.40331 (19)0.0364 (11)
C360.6487 (3)0.1130 (3)0.37809 (18)0.0365 (11)
Atomic displacement parameters (Å2) top
U11U22U33U12U13U23
Cr10.0309 (4)0.0389 (4)0.0259 (3)0.0015 (3)0.0005 (3)0.0012 (3)
Cl10.0402 (6)0.0529 (8)0.0379 (6)0.0115 (6)0.0024 (5)0.0098 (5)
O110.052 (2)0.056 (2)0.057 (2)0.0093 (18)0.0141 (18)0.0136 (19)
O120.051 (2)0.045 (2)0.151 (5)0.0030 (19)0.024 (3)0.003 (3)
O130.0392 (19)0.046 (2)0.058 (2)0.0030 (16)0.0100 (16)0.0026 (17)
O140.086 (3)0.219 (7)0.045 (2)0.094 (4)0.021 (2)0.035 (3)
Cl20.0452 (7)0.0801 (10)0.0301 (6)0.0153 (7)0.0036 (5)0.0037 (6)
O210.052 (2)0.052 (2)0.0404 (18)0.0090 (17)0.0039 (16)0.0010 (16)
O220.059 (2)0.067 (3)0.0364 (18)0.0066 (19)0.0073 (16)0.0023 (17)
O230.125 (4)0.165 (5)0.051 (3)0.100 (4)0.034 (3)0.036 (3)
O240.062 (3)0.140 (5)0.060 (3)0.053 (3)0.004 (2)0.022 (3)
Cl30.0560 (16)0.075 (2)0.0421 (14)0.0114 (15)0.0002 (12)0.0105 (14)
O310.047 (4)0.042 (4)0.068 (5)0.006 (3)0.009 (4)0.024 (4)
O320.126 (8)0.061 (6)0.048 (5)0.053 (6)0.015 (5)0.006 (4)
O330.104 (8)0.124 (9)0.078 (7)0.045 (7)0.017 (6)0.004 (6)
O340.122 (11)0.139 (12)0.126 (10)0.004 (10)0.031 (9)0.064 (9)
Cl40.0550 (17)0.083 (2)0.0648 (18)0.0136 (16)0.0089 (14)0.0168 (16)
O420.071 (5)0.072 (6)0.069 (5)0.001 (4)0.005 (4)0.021 (4)
O430.077 (7)0.046 (6)0.261 (17)0.019 (5)0.033 (9)0.002 (8)
O440.116 (10)0.32 (2)0.061 (6)0.030 (13)0.014 (6)0.032 (10)
O500.062 (6)0.075 (6)0.085 (7)0.015 (5)0.013 (5)0.002 (6)
O5010.072 (8)0.171 (14)0.056 (7)0.027 (9)0.002 (5)0.026 (8)
N10.0290 (18)0.041 (2)0.0273 (17)0.0021 (16)0.0005 (15)0.0027 (16)
N20.0321 (19)0.034 (2)0.0265 (17)0.0010 (16)0.0014 (14)0.0017 (15)
C10.034 (2)0.043 (3)0.032 (2)0.001 (2)0.0031 (18)0.002 (2)
C20.035 (3)0.060 (3)0.039 (3)0.002 (2)0.004 (2)0.008 (2)
C30.030 (2)0.049 (3)0.042 (3)0.003 (2)0.0024 (19)0.006 (2)
C40.034 (2)0.037 (3)0.031 (2)0.0020 (19)0.0005 (18)0.0020 (19)
C50.042 (3)0.041 (3)0.039 (2)0.002 (2)0.003 (2)0.008 (2)
C60.047 (3)0.042 (3)0.035 (2)0.005 (2)0.004 (2)0.011 (2)
C70.037 (2)0.039 (3)0.033 (2)0.007 (2)0.0002 (19)0.002 (2)
C80.037 (2)0.049 (3)0.029 (2)0.006 (2)0.0016 (19)0.002 (2)
C90.036 (2)0.055 (3)0.029 (2)0.005 (2)0.0022 (19)0.004 (2)
C100.035 (2)0.043 (3)0.033 (2)0.000 (2)0.0014 (18)0.002 (2)
C110.032 (2)0.032 (2)0.029 (2)0.0042 (19)0.0030 (17)0.0004 (18)
C120.034 (2)0.041 (3)0.025 (2)0.005 (2)0.0002 (17)0.0009 (19)
N30.0333 (19)0.040 (2)0.0279 (18)0.0038 (17)0.0015 (15)0.0023 (16)
N40.036 (2)0.048 (2)0.034 (2)0.0102 (18)0.0048 (16)0.0059 (18)
C130.037 (3)0.048 (3)0.038 (2)0.003 (2)0.001 (2)0.001 (2)
C140.043 (3)0.049 (3)0.064 (4)0.003 (2)0.010 (3)0.009 (3)
C150.045 (3)0.065 (4)0.054 (3)0.012 (3)0.018 (2)0.031 (3)
C160.040 (3)0.064 (4)0.039 (3)0.014 (3)0.008 (2)0.016 (3)
C170.064 (4)0.068 (4)0.042 (3)0.030 (3)0.017 (3)0.019 (3)
C180.070 (4)0.078 (5)0.036 (3)0.036 (4)0.001 (3)0.007 (3)
C190.052 (3)0.075 (4)0.030 (2)0.032 (3)0.003 (2)0.006 (3)
C200.072 (4)0.076 (4)0.040 (3)0.037 (3)0.023 (3)0.022 (3)
C210.071 (4)0.070 (4)0.050 (3)0.023 (3)0.023 (3)0.025 (3)
C220.047 (3)0.052 (3)0.049 (3)0.015 (2)0.012 (2)0.016 (2)
C230.041 (3)0.052 (3)0.031 (2)0.018 (2)0.000 (2)0.003 (2)
C240.041 (3)0.057 (3)0.032 (2)0.020 (2)0.004 (2)0.004 (2)
N50.035 (2)0.035 (2)0.0249 (17)0.0040 (16)0.0050 (15)0.0040 (15)
N60.0305 (19)0.045 (2)0.036 (2)0.0073 (17)0.0005 (16)0.0030 (18)
C250.034 (2)0.043 (3)0.026 (2)0.001 (2)0.0018 (17)0.000 (2)
C260.036 (2)0.044 (3)0.034 (2)0.005 (2)0.0042 (19)0.005 (2)
C270.043 (3)0.054 (3)0.034 (2)0.015 (2)0.011 (2)0.012 (2)
C280.046 (3)0.036 (3)0.033 (2)0.003 (2)0.013 (2)0.004 (2)
C290.058 (3)0.041 (3)0.045 (3)0.004 (2)0.014 (3)0.005 (2)
C300.070 (4)0.033 (3)0.043 (3)0.008 (3)0.020 (3)0.003 (2)
C310.049 (3)0.045 (3)0.036 (2)0.010 (2)0.011 (2)0.007 (2)
C320.060 (3)0.049 (3)0.045 (3)0.017 (3)0.006 (3)0.003 (3)
C330.050 (3)0.068 (4)0.050 (3)0.023 (3)0.005 (2)0.003 (3)
C340.046 (3)0.050 (3)0.046 (3)0.008 (2)0.007 (2)0.004 (2)
C350.045 (3)0.036 (3)0.028 (2)0.006 (2)0.0075 (19)0.0056 (19)
C360.039 (2)0.044 (3)0.026 (2)0.004 (2)0.0095 (19)0.008 (2)
Geometric parameters (Å, º) top
Cr1—N22.040 (4)C7—C81.393 (6)
Cr1—N62.040 (4)C7—C111.407 (6)
Cr1—N32.040 (4)C8—C91.375 (7)
Cr1—N52.049 (4)C9—C101.390 (6)
Cr1—N12.050 (3)C11—C121.429 (6)
Cr1—N42.055 (4)N3—C131.331 (6)
Cl1—O141.418 (4)N3—C241.391 (6)
Cl1—O121.429 (4)N4—C221.346 (6)
Cl1—O131.438 (3)N4—C231.365 (6)
Cl1—O111.440 (3)C13—C141.413 (7)
Cl2—O211.415 (3)C14—C151.363 (8)
Cl2—O231.416 (4)C15—C161.401 (8)
Cl2—O221.441 (3)C16—C241.415 (7)
Cl2—O241.463 (5)C16—C171.443 (7)
Cl3—O321.352 (8)C17—C181.364 (9)
Cl3—O341.376 (10)C18—C191.415 (8)
Cl3—O311.391 (7)C19—C231.393 (6)
Cl3—O331.394 (9)C19—C201.404 (9)
O34—O431.156 (14)C20—C211.362 (9)
O34—Cl41.915 (11)C21—C221.369 (7)
Cl4—O411.292 (7)C23—C241.409 (7)
Cl4—O441.388 (10)N5—C251.337 (5)
Cl4—O431.411 (9)N5—C361.368 (6)
Cl4—O421.418 (8)N6—C341.335 (6)
O44—O44i1.432 (19)N6—C351.359 (6)
O50—O5010.843 (13)C25—C261.388 (6)
N1—C101.330 (5)C26—C271.363 (7)
N1—C111.365 (6)C27—C281.405 (7)
N2—C11.330 (5)C28—C361.416 (7)
N2—C121.390 (5)C28—C291.417 (7)
C1—C21.392 (7)C29—C301.334 (8)
C2—C31.378 (6)C30—C311.424 (7)
C3—C41.416 (6)C31—C321.390 (7)
C4—C121.392 (6)C31—C351.404 (7)
C4—C51.425 (6)C32—C331.373 (8)
C5—C61.344 (6)C33—C341.404 (8)
C6—C71.438 (7)C35—C361.421 (7)
N2—Cr1—N696.94 (15)C8—C7—C6124.5 (4)
N2—Cr1—N390.38 (15)C11—C7—C6118.0 (4)
N6—Cr1—N3171.23 (15)C9—C8—C7119.5 (4)
N2—Cr1—N5177.53 (14)C8—C9—C10119.7 (4)
N6—Cr1—N581.15 (15)N1—C10—C9122.6 (4)
N3—Cr1—N591.65 (15)N1—C11—C7122.7 (4)
N2—Cr1—N181.31 (14)N1—C11—C12117.3 (4)
N6—Cr1—N189.88 (14)C7—C11—C12120.0 (4)
N3—Cr1—N196.01 (14)N2—C12—C4123.3 (4)
N5—Cr1—N197.07 (14)N2—C12—C11115.9 (4)
N2—Cr1—N492.65 (14)C4—C12—C11120.8 (4)
N6—Cr1—N493.31 (16)C13—N3—C24119.2 (4)
N3—Cr1—N481.49 (16)C13—N3—Cr1129.1 (3)
N5—Cr1—N489.04 (14)C24—N3—Cr1111.7 (3)
N1—Cr1—N4173.48 (15)C22—N4—C23118.7 (4)
O14—Cl1—O12110.1 (4)C22—N4—Cr1129.1 (4)
O14—Cl1—O13110.4 (3)C23—N4—Cr1112.1 (3)
O12—Cl1—O13109.0 (2)N3—C13—C14121.7 (5)
O14—Cl1—O11110.1 (3)C15—C14—C13119.4 (5)
O12—Cl1—O11106.9 (2)C14—C15—C16121.0 (5)
O13—Cl1—O11110.3 (2)C15—C16—C24117.2 (5)
O21—Cl2—O23111.5 (3)C15—C16—C17126.2 (5)
O21—Cl2—O22110.2 (2)C24—C16—C17116.5 (5)
O23—Cl2—O22112.2 (3)C18—C17—C16121.6 (5)
O21—Cl2—O24107.7 (3)C17—C18—C19121.1 (5)
O23—Cl2—O24105.9 (3)C23—C19—C20116.6 (5)
O22—Cl2—O24109.2 (2)C23—C19—C18118.9 (6)
O32—Cl3—O34113.4 (7)C20—C19—C18124.5 (5)
O32—Cl3—O31102.4 (5)C21—C20—C19121.3 (5)
O34—Cl3—O31107.5 (7)C20—C21—C22118.9 (6)
O32—Cl3—O33110.0 (5)N4—C22—C21122.4 (6)
O34—Cl3—O33110.3 (7)N4—C23—C19122.1 (5)
O31—Cl3—O33113.2 (6)N4—C23—C24117.4 (4)
O43—O34—Cl3149.6 (14)C19—C23—C24120.5 (5)
O43—O34—Cl447.1 (6)N3—C24—C23117.2 (4)
Cl3—O34—Cl4150.5 (10)N3—C24—C16121.5 (5)
O41—Cl4—O44108.1 (7)C23—C24—C16121.3 (4)
O41—Cl4—O43114.0 (5)C25—N5—C36117.7 (4)
O44—Cl4—O43106.8 (8)C25—N5—Cr1130.1 (3)
O41—Cl4—O42110.4 (5)C36—N5—Cr1111.9 (3)
O44—Cl4—O42108.3 (6)C34—N6—C35119.0 (4)
O43—Cl4—O42109.0 (7)C34—N6—Cr1128.5 (4)
O41—Cl4—O34142.9 (6)C35—N6—Cr1112.5 (3)
O44—Cl4—O34104.1 (8)N5—C25—C26123.4 (4)
O43—Cl4—O3436.9 (6)C27—C26—C25118.9 (5)
O42—Cl4—O3475.4 (6)C26—C27—C28120.9 (5)
O34—O43—Cl496.0 (9)C27—C28—C36116.4 (4)
Cl4—O44—O44i133.9 (13)C27—C28—C29125.7 (5)
C10—N1—C11118.0 (4)C36—C28—C29117.9 (5)
C10—N1—Cr1129.2 (3)C30—C29—C28121.4 (5)
C11—N1—Cr1112.6 (3)C29—C30—C31122.4 (5)
C1—N2—C12117.5 (4)C32—C31—C35117.1 (5)
C1—N2—Cr1129.8 (3)C32—C31—C30124.9 (5)
C12—N2—Cr1112.7 (3)C35—C31—C30118.0 (5)
N2—C1—C2122.7 (4)C33—C32—C31119.8 (5)
C3—C2—C1120.2 (4)C32—C33—C34120.3 (5)
C2—C3—C4119.2 (4)N6—C34—C33120.8 (5)
C12—C4—C3117.2 (4)N6—C35—C31123.1 (4)
C12—C4—C5118.0 (4)N6—C35—C36117.2 (4)
C3—C4—C5124.8 (4)C31—C35—C36119.7 (5)
C6—C5—C4122.2 (4)N5—C36—C28122.7 (4)
C5—C6—C7121.0 (4)N5—C36—C35116.8 (4)
C8—C7—C11117.4 (4)C28—C36—C35120.5 (4)
Symmetry code: (i) x+2, y, z+1/2.
 

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