Supporting information
Crystallographic Information File (CIF) https://doi.org/10.1107/S0108270102018474/na1580sup1.cif | |
Structure factor file (CIF format) https://doi.org/10.1107/S0108270102018474/na1580Isup2.hkl |
CCDC reference: 199411
Crystals of the title compound were obtained from a solution in cyanobenzene–water as described elsewhere (Janczak & Idemori, 2002).
The water H atoms wererefined, while the H atoms of the benzene rings of the Pc2- system were treated as riding.
Data collection: COLLECT (Nonius, 1997-2000); cell refinement: COLLECT; data reduction: COLLECT; program(s) used to solve structure: SHELXS97 (Sheldrick, 1990a); program(s) used to refine structure: SHELXL97 (Sheldrick, 1997); molecular graphics: SHELXTL (Sheldrick, 1990b); software used to prepare material for publication: SHELXL97.
Fig. 1. A view of both independent molecules in (I), shown with 50% probability displacement ellipsoids. H atoms are shown as spheres of arbitrary radii. |
[Mg(C32H16MgN8)(H2O)] | Z = 4 |
Mr = 554.86 | F(000) = 1144 |
Triclinic, P1 | Dx = 1.474 Mg m−3 Dm = 1.47 Mg m−3 Dm measured by flotation |
Hall symbol: -P 1 | Melting point: dehydratated K |
a = 12.955 (2) Å | Mo Kα radiation, λ = 0.71073 Å |
b = 13.293 (3) Å | Cell parameters from 4680 reflections |
c = 16.202 (3) Å | θ = 3–27° |
α = 65.03 (2)° | µ = 0.12 mm−1 |
β = 81.91 (2)° | T = 200 K |
γ = 83.73 (2)° | Parallelepiped, violet |
V = 2500.3 (9) Å3 | 0.25 × 0.22 × 0.16 mm |
Nonius CCD area-detector diffractometer | 11221 independent reflections |
Radiation source: fine-focus sealed tube | 8172 reflections with I > 2σ(I) |
Graphite monochromator | Rint = 0.040 |
Detector resolution: 1024x1024 pixels mm-1 | θmax = 27.4°, θmin = 1.4° |
ω scans | h = −16→16 |
Absorption correction: analytical face-indexed (SHELXTL; Sheldrick, 1990) | k = −17→16 |
Tmin = 0.966, Tmax = 0.982 | l = −20→20 |
47310 measured reflections |
Refinement on F2 | Primary atom site location: structure-invariant direct methods |
Least-squares matrix: full | Secondary atom site location: difference Fourier map |
R[F2 > 2σ(F2)] = 0.049 | Hydrogen site location: inferred from neighbouring sites |
wR(F2) = 0.099 | H atoms treated by a mixture of independent and constrained refinement |
S = 1.04 | w = 1/[σ2(Fo2) + (0.0301P)2 + 0.8806P] where P = (Fo2 + 2Fc2)/3 |
11221 reflections | (Δ/σ)max = 0.001 |
769 parameters | Δρmax = 0.37 e Å−3 |
0 restraints | Δρmin = −0.29 e Å−3 |
[Mg(C32H16MgN8)(H2O)] | γ = 83.73 (2)° |
Mr = 554.86 | V = 2500.3 (9) Å3 |
Triclinic, P1 | Z = 4 |
a = 12.955 (2) Å | Mo Kα radiation |
b = 13.293 (3) Å | µ = 0.12 mm−1 |
c = 16.202 (3) Å | T = 200 K |
α = 65.03 (2)° | 0.25 × 0.22 × 0.16 mm |
β = 81.91 (2)° |
Nonius CCD area-detector diffractometer | 11221 independent reflections |
Absorption correction: analytical face-indexed (SHELXTL; Sheldrick, 1990) | 8172 reflections with I > 2σ(I) |
Tmin = 0.966, Tmax = 0.982 | Rint = 0.040 |
47310 measured reflections |
R[F2 > 2σ(F2)] = 0.049 | 0 restraints |
wR(F2) = 0.099 | H atoms treated by a mixture of independent and constrained refinement |
S = 1.04 | Δρmax = 0.37 e Å−3 |
11221 reflections | Δρmin = −0.29 e Å−3 |
769 parameters |
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. |
Refinement. Refinement of F2 against ALL reflections. The weighted R-factor wR and goodness of fit S are based on F2, conventional R-factors R are based on F, with F set to zero for negative F2. The threshold expression of F2 > σ(F2) is used only for calculating R-factors(gt) etc. and is not relevant to the choice of reflections for refinement. R-factors based on F2 are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger. |
x | y | z | Uiso*/Ueq | ||
Mg1 | 0.55455 (4) | 0.25395 (4) | 0.45874 (4) | 0.01876 (13) | |
O1 | 0.55054 (11) | 0.23121 (11) | 0.34308 (9) | 0.0257 (3) | |
H1O1 | 0.5402 (16) | 0.1700 (19) | 0.3425 (15) | 0.038* | |
H2O1 | 0.5621 (16) | 0.2793 (18) | 0.2899 (15) | 0.038* | |
N1 | 0.68829 (11) | 0.33569 (11) | 0.42990 (9) | 0.0204 (3) | |
N2 | 0.61982 (11) | 0.52844 (11) | 0.36974 (9) | 0.0214 (3) | |
N3 | 0.47523 (11) | 0.40472 (11) | 0.43323 (9) | 0.0205 (3) | |
N4 | 0.29989 (11) | 0.34250 (11) | 0.48821 (9) | 0.0208 (3) | |
N5 | 0.42404 (11) | 0.18021 (11) | 0.53993 (9) | 0.0205 (3) | |
N6 | 0.49296 (11) | −0.01077 (11) | 0.61993 (9) | 0.0207 (3) | |
N7 | 0.63492 (11) | 0.10997 (11) | 0.53602 (9) | 0.0201 (3) | |
N8 | 0.81195 (11) | 0.17568 (11) | 0.48734 (9) | 0.0211 (3) | |
C1 | 0.78614 (12) | 0.28291 (14) | 0.44611 (11) | 0.0184 (3) | |
C2 | 0.86376 (13) | 0.36922 (14) | 0.41301 (12) | 0.0207 (4) | |
C3 | 0.97031 (14) | 0.36158 (15) | 0.41600 (12) | 0.0247 (4) | |
H3 | 1.0069 | 0.2930 | 0.4401 | 0.030* | |
C4 | 1.02110 (14) | 0.46080 (15) | 0.38147 (13) | 0.0286 (4) | |
H4 | 1.0932 | 0.4583 | 0.3806 | 0.034* | |
C5 | 0.96585 (15) | 0.56336 (16) | 0.34825 (14) | 0.0323 (4) | |
H5 | 1.0020 | 0.6279 | 0.3260 | 0.039* | |
C6 | 0.85762 (14) | 0.57191 (15) | 0.34752 (12) | 0.0266 (4) | |
H6 | 0.8210 | 0.6407 | 0.3268 | 0.032* | |
C7 | 0.80651 (13) | 0.47346 (14) | 0.37898 (11) | 0.0202 (4) | |
C8 | 0.69703 (13) | 0.44882 (13) | 0.39154 (11) | 0.0196 (3) | |
C9 | 0.51844 (13) | 0.50650 (13) | 0.39006 (11) | 0.0202 (4) | |
C10 | 0.43459 (14) | 0.59491 (14) | 0.37127 (11) | 0.0213 (4) | |
C11 | 0.43585 (14) | 0.71035 (14) | 0.33009 (11) | 0.0243 (4) | |
H11 | 0.4984 | 0.7458 | 0.3084 | 0.029* | |
C12 | 0.34051 (15) | 0.77079 (15) | 0.32246 (12) | 0.0263 (4) | |
H12 | 0.3392 | 0.8480 | 0.2948 | 0.032* | |
C13 | 0.24628 (15) | 0.71758 (14) | 0.35568 (12) | 0.0251 (4) | |
H13 | 0.1835 | 0.7600 | 0.3489 | 0.030* | |
C14 | 0.24514 (14) | 0.60224 (14) | 0.39871 (11) | 0.0230 (4) | |
H14 | 0.1826 | 0.5672 | 0.4222 | 0.028* | |
C15 | 0.34062 (13) | 0.54055 (14) | 0.40565 (12) | 0.0212 (4) | |
C16 | 0.36951 (13) | 0.42047 (14) | 0.44562 (11) | 0.0204 (4) | |
C17 | 0.32611 (13) | 0.23327 (13) | 0.53226 (11) | 0.0190 (3) | |
C18 | 0.24783 (13) | 0.15059 (14) | 0.58105 (11) | 0.0209 (4) | |
C19 | 0.13917 (13) | 0.16190 (15) | 0.59202 (12) | 0.0232 (4) | |
H19 | 0.1040 | 0.2313 | 0.5679 | 0.028* | |
C20 | 0.08513 (14) | 0.06569 (15) | 0.64031 (12) | 0.0260 (4) | |
H20 | 0.0125 | 0.0704 | 0.6473 | 0.031* | |
C21 | 0.13921 (14) | −0.03898 (15) | 0.67887 (12) | 0.0255 (4) | |
H21 | 0.1014 | −0.1022 | 0.7106 | 0.031* | |
C22 | 0.24802 (14) | −0.04970 (15) | 0.67043 (12) | 0.0243 (4) | |
H22 | 0.2830 | −0.1187 | 0.6975 | 0.029* | |
C23 | 0.30294 (13) | 0.04619 (14) | 0.62010 (11) | 0.0217 (4) | |
C24 | 0.41423 (13) | 0.06828 (13) | 0.59362 (11) | 0.0192 (3) | |
C25 | 0.59505 (13) | 0.01017 (13) | 0.59352 (11) | 0.0201 (4) | |
C26 | 0.68085 (13) | −0.07496 (14) | 0.62551 (11) | 0.0216 (4) | |
C27 | 0.68699 (14) | −0.18959 (15) | 0.68366 (12) | 0.0266 (4) | |
H27 | 0.6268 | −0.2280 | 0.7111 | 0.032* | |
C28 | 0.78528 (14) | −0.24350 (15) | 0.69878 (12) | 0.0280 (4) | |
H28 | 0.7907 | −0.3191 | 0.7363 | 0.034* | |
C29 | 0.87633 (14) | −0.18558 (14) | 0.65831 (12) | 0.0244 (4) | |
H29 | 0.9410 | −0.2233 | 0.6710 | 0.029* | |
C30 | 0.87246 (14) | −0.07365 (14) | 0.59992 (11) | 0.0231 (4) | |
H30 | 0.9331 | −0.0362 | 0.5723 | 0.028* | |
C31 | 0.77400 (13) | −0.01922 (14) | 0.58418 (11) | 0.0212 (4) | |
C32 | 0.74198 (13) | 0.09735 (13) | 0.53001 (11) | 0.0191 (3) | |
Mg2 | 0.54172 (4) | 0.20995 (5) | 0.04847 (4) | 0.01931 (13) | |
O2 | 0.50146 (10) | 0.07052 (11) | 0.16324 (9) | 0.0257 (3) | |
H1O2 | 0.4881 (17) | 0.0569 (18) | 0.2151 (16) | 0.039* | |
H2O2 | 0.4953 (17) | 0.0145 (18) | 0.1553 (15) | 0.039* | |
N9 | 0.45513 (11) | 0.33878 (11) | 0.06780 (9) | 0.0203 (3) | |
N10 | 0.57527 (11) | 0.39078 (12) | 0.14498 (9) | 0.0219 (3) | |
N11 | 0.66561 (11) | 0.26524 (11) | 0.08028 (9) | 0.0209 (3) | |
N12 | 0.80748 (11) | 0.16949 (11) | 0.02153 (9) | 0.0218 (3) | |
N13 | 0.64498 (11) | 0.14388 (11) | −0.02647 (9) | 0.0201 (3) | |
N14 | 0.52632 (12) | 0.09250 (11) | −0.10507 (9) | 0.0203 (3) | |
N15 | 0.43582 (12) | 0.21533 (11) | −0.03685 (9) | 0.0210 (3) | |
N16 | 0.29831 (11) | 0.33419 (11) | 0.00292 (9) | 0.0207 (3) | |
C33 | 0.35355 (13) | 0.36932 (13) | 0.04871 (11) | 0.0204 (4) | |
C34 | 0.31147 (13) | 0.44932 (13) | 0.08770 (11) | 0.0195 (4) | |
C35 | 0.21362 (14) | 0.50439 (13) | 0.08877 (11) | 0.0225 (4) | |
H35 | 0.1605 | 0.4953 | 0.0598 | 0.027* | |
C36 | 0.19838 (15) | 0.57419 (14) | 0.13525 (12) | 0.0270 (4) | |
H36 | 0.1335 | 0.6109 | 0.1380 | 0.032* | |
C37 | 0.27930 (15) | 0.58996 (15) | 0.17790 (12) | 0.0297 (4) | |
H37 | 0.2670 | 0.6372 | 0.2077 | 0.036* | |
C38 | 0.37716 (15) | 0.53585 (15) | 0.17602 (12) | 0.0265 (4) | |
H38 | 0.4308 | 0.5464 | 0.2036 | 0.032* | |
C39 | 0.39197 (14) | 0.46435 (14) | 0.13076 (11) | 0.0222 (4) | |
C40 | 0.48213 (13) | 0.39454 (14) | 0.11602 (11) | 0.0217 (4) | |
C41 | 0.66034 (13) | 0.33556 (14) | 0.12325 (11) | 0.0212 (4) | |
C42 | 0.76513 (13) | 0.34830 (14) | 0.14035 (11) | 0.0217 (4) | |
C43 | 0.80216 (15) | 0.41365 (15) | 0.17820 (12) | 0.0262 (4) | |
H43 | 0.7567 | 0.4560 | 0.2023 | 0.031* | |
C44 | 0.91003 (15) | 0.41205 (16) | 0.17795 (13) | 0.0316 (4) | |
H44 | 0.9373 | 0.4529 | 0.2035 | 0.038* | |
C45 | 0.97874 (15) | 0.34914 (15) | 0.13932 (12) | 0.0285 (4) | |
H45 | 1.0503 | 0.3496 | 0.1401 | 0.034* | |
C46 | 0.94137 (14) | 0.28625 (15) | 0.09999 (12) | 0.0253 (4) | |
H46 | 0.9869 | 0.2466 | 0.0733 | 0.030* | |
C47 | 0.83364 (13) | 0.28536 (14) | 0.10230 (11) | 0.0217 (4) | |
C48 | 0.76885 (13) | 0.23266 (13) | 0.06486 (11) | 0.0201 (4) | |
C49 | 0.75068 (13) | 0.13011 (13) | −0.02086 (11) | 0.0197 (4) | |
C50 | 0.79811 (13) | 0.06508 (14) | −0.07115 (11) | 0.0219 (4) | |
C51 | 0.90271 (14) | 0.03322 (15) | −0.08808 (12) | 0.0254 (4) | |
H51 | 0.9556 | 0.0534 | −0.0657 | 0.031* | |
C52 | 0.92522 (14) | −0.02945 (15) | −0.13941 (12) | 0.0278 (4) | |
H52 | 0.9942 | −0.0506 | −0.1524 | 0.033* | |
C53 | 0.84492 (15) | −0.06118 (15) | −0.17190 (12) | 0.0288 (4) | |
H53 | 0.8616 | −0.1049 | −0.2046 | 0.035* | |
C54 | 0.74116 (14) | −0.02865 (14) | −0.15631 (12) | 0.0254 (4) | |
H54 | 0.6886 | −0.0498 | −0.1784 | 0.030* | |
C55 | 0.71704 (14) | 0.03752 (14) | −0.10610 (12) | 0.0215 (4) | |
C56 | 0.62139 (14) | 0.09160 (13) | −0.07841 (12) | 0.0203 (4) | |
C57 | 0.44173 (13) | 0.15183 (13) | −0.08654 (12) | 0.0183 (3) | |
C58 | 0.33810 (13) | 0.15730 (14) | −0.11797 (12) | 0.0217 (4) | |
C59 | 0.29750 (14) | 0.10739 (15) | −0.16661 (12) | 0.0252 (4) | |
H59 | 0.3396 | 0.0613 | −0.1891 | 0.030* | |
C60 | 0.19253 (14) | 0.12906 (15) | −0.18000 (12) | 0.0271 (4) | |
H60 | 0.1639 | 0.0961 | −0.2114 | 0.032* | |
C61 | 0.12850 (14) | 0.19942 (15) | −0.14739 (12) | 0.0271 (4) | |
H61 | 0.0584 | 0.2122 | −0.1576 | 0.033* | |
C62 | 0.16820 (13) | 0.25098 (14) | −0.09962 (12) | 0.0240 (4) | |
H62 | 0.1263 | 0.2984 | −0.0785 | 0.029* | |
C63 | 0.27304 (13) | 0.22771 (14) | −0.08543 (12) | 0.0211 (4) | |
C64 | 0.33661 (12) | 0.26470 (13) | −0.03595 (12) | 0.0183 (3) |
U11 | U22 | U33 | U12 | U13 | U23 | |
Mg1 | 0.0188 (3) | 0.0171 (3) | 0.0188 (3) | −0.0012 (2) | −0.0020 (2) | −0.0057 (2) |
O1 | 0.0337 (7) | 0.0199 (7) | 0.0212 (6) | −0.0041 (6) | −0.0033 (5) | −0.0056 (5) |
N1 | 0.0230 (8) | 0.0170 (7) | 0.0206 (7) | 0.0004 (6) | −0.0031 (6) | −0.0074 (6) |
N2 | 0.0225 (8) | 0.0201 (7) | 0.0215 (7) | −0.0014 (6) | −0.0027 (6) | −0.0082 (6) |
N3 | 0.0221 (8) | 0.0185 (7) | 0.0200 (7) | −0.0018 (6) | −0.0027 (6) | −0.0067 (6) |
N4 | 0.0218 (8) | 0.0200 (7) | 0.0213 (7) | −0.0009 (6) | −0.0028 (6) | −0.0092 (6) |
N5 | 0.0204 (7) | 0.0185 (7) | 0.0215 (7) | 0.0001 (6) | −0.0024 (6) | −0.0075 (6) |
N6 | 0.0213 (7) | 0.0196 (7) | 0.0211 (7) | −0.0019 (6) | −0.0008 (6) | −0.0087 (6) |
N7 | 0.0207 (7) | 0.0181 (7) | 0.0215 (7) | −0.0001 (6) | −0.0025 (6) | −0.0082 (6) |
N8 | 0.0212 (7) | 0.0190 (7) | 0.0222 (7) | −0.0010 (6) | −0.0017 (6) | −0.0079 (6) |
C1 | 0.0157 (8) | 0.0254 (9) | 0.0163 (8) | −0.0003 (7) | −0.0023 (6) | −0.0109 (7) |
C2 | 0.0227 (9) | 0.0213 (9) | 0.0182 (8) | −0.0011 (7) | −0.0016 (7) | −0.0084 (7) |
C3 | 0.0238 (9) | 0.0245 (9) | 0.0253 (9) | 0.0011 (7) | −0.0042 (7) | −0.0100 (8) |
C4 | 0.0219 (9) | 0.0332 (10) | 0.0339 (10) | −0.0052 (8) | −0.0039 (8) | −0.0159 (9) |
C5 | 0.0277 (10) | 0.0282 (10) | 0.0397 (11) | −0.0101 (8) | 0.0009 (8) | −0.0123 (9) |
C6 | 0.0266 (10) | 0.0254 (9) | 0.0242 (9) | −0.0038 (8) | 0.0000 (7) | −0.0071 (8) |
C7 | 0.0242 (9) | 0.0188 (8) | 0.0182 (8) | −0.0013 (7) | −0.0001 (7) | −0.0088 (7) |
C8 | 0.0238 (9) | 0.0176 (8) | 0.0180 (8) | −0.0002 (7) | −0.0036 (7) | −0.0077 (7) |
C9 | 0.0261 (9) | 0.0173 (8) | 0.0160 (8) | −0.0027 (7) | −0.0036 (7) | −0.0051 (7) |
C10 | 0.0267 (9) | 0.0199 (8) | 0.0169 (8) | −0.0007 (7) | −0.0023 (7) | −0.0076 (7) |
C11 | 0.0304 (10) | 0.0211 (9) | 0.0208 (9) | −0.0001 (7) | −0.0034 (7) | −0.0081 (7) |
C12 | 0.0397 (11) | 0.0182 (9) | 0.0210 (9) | 0.0030 (8) | −0.0079 (8) | −0.0076 (7) |
C13 | 0.0315 (10) | 0.0242 (9) | 0.0225 (9) | 0.0091 (8) | −0.0100 (7) | −0.0126 (7) |
C14 | 0.0247 (9) | 0.0266 (9) | 0.0214 (9) | 0.0019 (7) | −0.0044 (7) | −0.0137 (7) |
C15 | 0.0263 (9) | 0.0194 (8) | 0.0188 (8) | 0.0002 (7) | −0.0052 (7) | −0.0082 (7) |
C16 | 0.0228 (9) | 0.0213 (9) | 0.0182 (8) | −0.0003 (7) | −0.0020 (7) | −0.0094 (7) |
C17 | 0.0175 (8) | 0.0197 (8) | 0.0183 (8) | −0.0009 (7) | −0.0029 (6) | −0.0061 (7) |
C18 | 0.0239 (9) | 0.0243 (9) | 0.0168 (8) | −0.0020 (7) | −0.0033 (7) | −0.0102 (7) |
C19 | 0.0237 (9) | 0.0257 (9) | 0.0199 (8) | 0.0001 (7) | −0.0037 (7) | −0.0091 (7) |
C20 | 0.0205 (9) | 0.0323 (10) | 0.0245 (9) | −0.0043 (8) | −0.0015 (7) | −0.0107 (8) |
C21 | 0.0268 (10) | 0.0267 (9) | 0.0244 (9) | −0.0096 (8) | 0.0030 (7) | −0.0117 (8) |
C22 | 0.0258 (9) | 0.0218 (9) | 0.0238 (9) | −0.0036 (7) | −0.0020 (7) | −0.0076 (7) |
C23 | 0.0223 (9) | 0.0237 (9) | 0.0197 (8) | −0.0018 (7) | 0.0006 (7) | −0.0102 (7) |
C24 | 0.0205 (9) | 0.0184 (8) | 0.0190 (8) | −0.0017 (7) | −0.0040 (6) | −0.0072 (7) |
C25 | 0.0236 (9) | 0.0174 (8) | 0.0198 (8) | −0.0007 (7) | −0.0024 (7) | −0.0083 (7) |
C26 | 0.0220 (9) | 0.0212 (9) | 0.0207 (8) | 0.0009 (7) | −0.0022 (7) | −0.0084 (7) |
C27 | 0.0260 (10) | 0.0231 (9) | 0.0250 (9) | −0.0037 (7) | −0.0006 (7) | −0.0046 (8) |
C28 | 0.0299 (10) | 0.0219 (9) | 0.0260 (9) | 0.0040 (8) | −0.0026 (8) | −0.0055 (8) |
C29 | 0.0254 (9) | 0.0243 (9) | 0.0237 (9) | 0.0086 (7) | −0.0073 (7) | −0.0108 (8) |
C30 | 0.0240 (9) | 0.0244 (9) | 0.0212 (8) | 0.0017 (7) | −0.0017 (7) | −0.0107 (7) |
C31 | 0.0246 (9) | 0.0183 (8) | 0.0210 (8) | −0.0001 (7) | −0.0048 (7) | −0.0079 (7) |
C32 | 0.0194 (8) | 0.0194 (8) | 0.0195 (8) | −0.0002 (7) | −0.0020 (6) | −0.0094 (7) |
Mg2 | 0.0195 (3) | 0.0198 (3) | 0.0196 (3) | −0.0009 (2) | −0.0026 (2) | −0.0090 (2) |
O2 | 0.0342 (7) | 0.0220 (7) | 0.0213 (6) | −0.0039 (6) | −0.0009 (6) | −0.0093 (6) |
N9 | 0.0213 (7) | 0.0184 (7) | 0.0214 (7) | −0.0008 (6) | −0.0022 (6) | −0.0085 (6) |
N10 | 0.0224 (8) | 0.0227 (8) | 0.0191 (7) | −0.0005 (6) | −0.0025 (6) | −0.0071 (6) |
N11 | 0.0239 (8) | 0.0192 (7) | 0.0187 (7) | −0.0013 (6) | −0.0024 (6) | −0.0070 (6) |
N12 | 0.0220 (8) | 0.0193 (7) | 0.0218 (7) | −0.0018 (6) | −0.0032 (6) | −0.0058 (6) |
N13 | 0.0213 (7) | 0.0186 (7) | 0.0193 (7) | −0.0006 (6) | −0.0031 (6) | −0.0066 (6) |
N14 | 0.0212 (7) | 0.0199 (7) | 0.0181 (7) | −0.0031 (6) | −0.0009 (6) | −0.0060 (6) |
N15 | 0.0205 (7) | 0.0209 (7) | 0.0227 (7) | −0.0008 (6) | −0.0024 (6) | −0.0103 (6) |
N16 | 0.0221 (8) | 0.0192 (7) | 0.0200 (7) | −0.0022 (6) | −0.0023 (6) | −0.0069 (6) |
C33 | 0.0209 (9) | 0.0187 (8) | 0.0201 (8) | −0.0017 (7) | −0.0005 (7) | −0.0067 (7) |
C34 | 0.0217 (9) | 0.0162 (8) | 0.0170 (8) | −0.0034 (7) | 0.0012 (6) | −0.0037 (7) |
C35 | 0.0250 (9) | 0.0178 (8) | 0.0201 (8) | −0.0013 (7) | 0.0015 (7) | −0.0044 (7) |
C36 | 0.0297 (10) | 0.0205 (9) | 0.0235 (9) | 0.0043 (7) | 0.0019 (7) | −0.0048 (7) |
C37 | 0.0413 (12) | 0.0248 (9) | 0.0228 (9) | 0.0047 (8) | −0.0010 (8) | −0.0120 (8) |
C38 | 0.0360 (11) | 0.0255 (9) | 0.0198 (9) | −0.0013 (8) | −0.0052 (7) | −0.0103 (7) |
C39 | 0.0270 (9) | 0.0185 (8) | 0.0183 (8) | −0.0007 (7) | −0.0001 (7) | −0.0058 (7) |
C40 | 0.0254 (9) | 0.0199 (9) | 0.0186 (8) | −0.0054 (7) | −0.0004 (7) | −0.0064 (7) |
C41 | 0.0235 (9) | 0.0202 (9) | 0.0181 (8) | −0.0035 (7) | −0.0026 (7) | −0.0056 (7) |
C42 | 0.0264 (9) | 0.0187 (8) | 0.0159 (8) | −0.0050 (7) | −0.0029 (7) | −0.0021 (7) |
C43 | 0.0322 (10) | 0.0255 (9) | 0.0212 (9) | −0.0032 (8) | −0.0059 (7) | −0.0085 (7) |
C44 | 0.0358 (11) | 0.0342 (11) | 0.0263 (10) | −0.0110 (9) | −0.0090 (8) | −0.0100 (8) |
C45 | 0.0274 (10) | 0.0261 (10) | 0.0271 (9) | −0.0101 (8) | −0.0081 (8) | −0.0026 (8) |
C46 | 0.0238 (9) | 0.0231 (9) | 0.0239 (9) | −0.0023 (7) | −0.0037 (7) | −0.0044 (7) |
C47 | 0.0231 (9) | 0.0210 (9) | 0.0188 (8) | −0.0040 (7) | −0.0042 (7) | −0.0049 (7) |
C48 | 0.0186 (8) | 0.0180 (8) | 0.0187 (8) | −0.0052 (7) | −0.0034 (6) | −0.0012 (7) |
C49 | 0.0187 (8) | 0.0169 (8) | 0.0209 (8) | 0.0002 (7) | −0.0018 (7) | −0.0056 (7) |
C50 | 0.0234 (9) | 0.0202 (9) | 0.0171 (8) | 0.0016 (7) | −0.0022 (7) | −0.0036 (7) |
C51 | 0.0215 (9) | 0.0263 (9) | 0.0238 (9) | 0.0008 (7) | −0.0022 (7) | −0.0063 (8) |
C52 | 0.0262 (10) | 0.0286 (10) | 0.0249 (9) | 0.0040 (8) | 0.0028 (7) | −0.0104 (8) |
C53 | 0.0338 (11) | 0.0278 (10) | 0.0250 (9) | 0.0030 (8) | 0.0019 (8) | −0.0135 (8) |
C54 | 0.0290 (10) | 0.0241 (9) | 0.0224 (9) | 0.0007 (8) | −0.0040 (7) | −0.0092 (7) |
C55 | 0.0239 (9) | 0.0194 (8) | 0.0186 (8) | 0.0002 (7) | −0.0013 (7) | −0.0061 (7) |
C56 | 0.0231 (9) | 0.0175 (8) | 0.0174 (8) | −0.0040 (7) | −0.0013 (7) | −0.0038 (7) |
C57 | 0.0202 (8) | 0.0147 (8) | 0.0180 (8) | −0.0006 (6) | −0.0031 (6) | −0.0046 (6) |
C58 | 0.0236 (9) | 0.0207 (9) | 0.0192 (8) | −0.0026 (7) | −0.0042 (7) | −0.0056 (7) |
C59 | 0.0281 (10) | 0.0238 (9) | 0.0237 (9) | −0.0026 (7) | −0.0046 (7) | −0.0088 (8) |
C60 | 0.0297 (10) | 0.0283 (10) | 0.0237 (9) | −0.0044 (8) | −0.0086 (7) | −0.0088 (8) |
C61 | 0.0217 (9) | 0.0284 (10) | 0.0293 (10) | −0.0007 (8) | −0.0098 (7) | −0.0080 (8) |
C62 | 0.0227 (9) | 0.0242 (9) | 0.0227 (9) | −0.0003 (7) | −0.0028 (7) | −0.0073 (7) |
C63 | 0.0236 (9) | 0.0186 (8) | 0.0193 (8) | −0.0026 (7) | −0.0030 (7) | −0.0056 (7) |
C64 | 0.0164 (8) | 0.0169 (8) | 0.0205 (8) | 0.0001 (6) | −0.0031 (6) | −0.0067 (7) |
Mg1—O1 | 2.029 (2) | C29—C30 | 1.386 (2) |
Mg1—N1 | 2.039 (2) | C29—H29 | 0.9300 |
Mg1—N5 | 2.049 (2) | C30—C31 | 1.396 (2) |
Mg1—N3 | 2.053 (2) | C30—H30 | 0.9300 |
Mg1—N7 | 2.055 (2) | C31—C32 | 1.469 (2) |
Mg2—O2 | 2.048 (2) | O2—H1O2 | 0.78 (2) |
Mg2—N9 | 2.055 (2) | O2—H2O2 | 0.82 (2) |
Mg2—N13 | 2.055 (2) | N9—C33 | 1.373 (2) |
Mg2—N11 | 2.048 (2) | N9—C40 | 1.380 (2) |
Mg2—N15 | 2.056 (2) | N10—C40 | 1.343 (2) |
O1—H1O1 | 0.84 (2) | N10—C41 | 1.345 (2) |
O1—H2O1 | 0.83 (2) | N11—C41 | 1.373 (2) |
N1—C8 | 1.374 (2) | N11—C48 | 1.382 (2) |
N1—C1 | 1.383 (2) | N12—C48 | 1.325 (2) |
N2—C8 | 1.341 (2) | N12—C49 | 1.348 (2) |
N2—C9 | 1.341 (2) | N13—C49 | 1.372 (2) |
N3—C16 | 1.362 (2) | N13—C56 | 1.377 (2) |
N3—C9 | 1.375 (2) | N14—C57 | 1.353 (2) |
N4—C16 | 1.338 (2) | N14—C56 | 1.359 (2) |
N4—C17 | 1.349 (2) | N15—C64 | 1.379 (2) |
N5—C17 | 1.378 (2) | N15—C57 | 1.382 (2) |
N5—C24 | 1.380 (2) | N16—C33 | 1.340 (2) |
N6—C25 | 1.353 (2) | N16—C64 | 1.341 (2) |
N6—C24 | 1.355 (2) | C33—C34 | 1.473 (2) |
N7—C25 | 1.366 (2) | C34—C35 | 1.395 (2) |
N7—C32 | 1.374 (2) | C34—C39 | 1.408 (2) |
N8—C1 | 1.321 (2) | C35—C36 | 1.405 (3) |
N8—C32 | 1.344 (2) | C35—H35 | 0.9300 |
C1—C2 | 1.482 (2) | C36—C37 | 1.412 (3) |
C2—C3 | 1.379 (2) | C36—H36 | 0.9300 |
C2—C7 | 1.421 (2) | C37—C38 | 1.391 (3) |
C3—C4 | 1.396 (2) | C37—H37 | 0.9300 |
C3—H3 | 0.9300 | C38—C39 | 1.410 (2) |
C4—C5 | 1.392 (3) | C38—H38 | 0.9300 |
C4—H4 | 0.9300 | C39—C40 | 1.468 (2) |
C5—C6 | 1.396 (3) | C41—C42 | 1.464 (2) |
C5—H5 | 0.9300 | C42—C43 | 1.409 (2) |
C6—C7 | 1.394 (2) | C42—C47 | 1.410 (3) |
C6—H6 | 0.9300 | C43—C44 | 1.395 (3) |
C7—C8 | 1.458 (2) | C43—H43 | 0.9300 |
C9—C10 | 1.472 (2) | C44—C45 | 1.416 (3) |
C10—C11 | 1.392 (2) | C44—H44 | 0.9300 |
C10—C15 | 1.406 (2) | C45—C46 | 1.402 (3) |
C11—C12 | 1.389 (3) | C45—H45 | 0.9300 |
C11—H11 | 0.9300 | C46—C47 | 1.392 (2) |
C12—C13 | 1.401 (3) | C46—H46 | 0.9300 |
C12—H12 | 0.9300 | C47—C48 | 1.481 (2) |
C13—C14 | 1.392 (2) | C49—C50 | 1.458 (2) |
C13—H13 | 0.9300 | C50—C51 | 1.400 (2) |
C14—C15 | 1.398 (2) | C50—C55 | 1.409 (2) |
C14—H14 | 0.9300 | C51—C52 | 1.391 (3) |
C15—C16 | 1.474 (2) | C51—H51 | 0.9300 |
C17—C18 | 1.465 (2) | C52—C53 | 1.405 (3) |
C18—C19 | 1.393 (2) | C52—H52 | 0.9300 |
C18—C23 | 1.416 (2) | C53—C54 | 1.388 (3) |
C19—C20 | 1.391 (2) | C53—H53 | 0.9300 |
C19—H19 | 0.9300 | C54—C55 | 1.416 (2) |
C20—C21 | 1.412 (3) | C54—H54 | 0.9300 |
C20—H20 | 0.9300 | C55—C56 | 1.475 (2) |
C21—C22 | 1.394 (2) | C57—C58 | 1.486 (2) |
C21—H21 | 0.9300 | C58—C59 | 1.404 (2) |
C22—C23 | 1.398 (2) | C58—C63 | 1.408 (2) |
C22—H22 | 0.9300 | C59—C60 | 1.387 (3) |
C23—C24 | 1.470 (2) | C59—H59 | 0.9300 |
C25—C26 | 1.475 (2) | C60—C61 | 1.402 (3) |
C26—C27 | 1.414 (2) | C60—H60 | 0.9300 |
C26—C31 | 1.415 (2) | C61—C62 | 1.404 (3) |
C27—C28 | 1.391 (3) | C61—H61 | 0.9300 |
C27—H27 | 0.9300 | C62—C63 | 1.389 (2) |
C28—C29 | 1.403 (3) | C62—H62 | 0.9300 |
C28—H28 | 0.9300 | C63—C64 | 1.473 (2) |
O1—Mg1—N1 | 102.00 (6) | C28—C29—H29 | 119.1 |
O1—Mg1—N5 | 103.58 (6) | C29—C30—C31 | 117.5 (2) |
N1—Mg1—N5 | 154.41 (6) | C29—C30—H30 | 121.3 |
O1—Mg1—N3 | 104.09 (6) | C31—C30—H30 | 121.3 |
N1—Mg1—N3 | 86.85 (6) | C30—C31—C26 | 122.0 (2) |
N5—Mg1—N3 | 87.80 (6) | C30—C31—C32 | 131.7 (2) |
O1—Mg1—N7 | 100.71 (6) | C26—C31—C32 | 106.3 (2) |
N1—Mg1—N7 | 88.78 (6) | N8—C32—N7 | 128.5 (2) |
N5—Mg1—N7 | 85.66 (6) | N8—C32—C31 | 121.8 (2) |
N3—Mg1—N7 | 155.18 (6) | N7—C32—C31 | 109.5 (2) |
O2—Mg2—N9 | 105.07 (6) | Mg2—O2—H1O2 | 135 (2) |
O2—Mg2—N13 | 101.63 (6) | Mg2—O2—H2O2 | 116 (2) |
N13—Mg2—N9 | 153.24 (6) | H1O2—O2—H2O2 | 109 (2) |
O2—Mg2—N11 | 104.53 (6) | C33—N9—C40 | 108.9 (2) |
N11—Mg2—N9 | 86.06 (6) | C33—N9—Mg2 | 124.5 (2) |
N11—Mg2—N13 | 88.85 (6) | C40—N9—Mg2 | 125.6 (2) |
O2—Mg2—N15 | 101.42 (6) | C40—N10—C41 | 122.6 (2) |
N9—Mg2—N15 | 88.22 (6) | C41—N11—C48 | 109.2 (2) |
N13—Mg2—N15 | 84.94 (6) | C41—N11—Mg2 | 126.4 (2) |
N11—Mg2—N15 | 154.03 (6) | C48—N11—Mg2 | 124.4 (2) |
Mg1—O1—H1O1 | 124 (2) | C48—N12—C49 | 124.6 (2) |
Mg1—O1—H2O1 | 125 (2) | C49—N13—C56 | 108.3 (2) |
H1O1—O1—H2O1 | 111 (2) | C49—N13—Mg2 | 123.8 (2) |
C8—N1—C1 | 109.4 (2) | C56—N13—Mg2 | 127.3 (1) |
C8—N1—Mg1 | 126.8 (1) | C57—N14—C56 | 122.7 (2) |
C1—N1—Mg1 | 123.8 (1) | C64—N15—C57 | 109.1 (2) |
C8—N2—C9 | 122.9 (2) | C64—N15—Mg2 | 123.1 (1) |
C16—N3—C9 | 109.0 (2) | C57—N15—Mg2 | 126.3 (1) |
C16—N3—Mg1 | 125.0 (1) | C33—N16—C64 | 124.4 (2) |
C9—N3—Mg1 | 125.5 (2) | N16—C33—N9 | 127.5 (2) |
C16—N4—C17 | 123.8 (2) | N16—C33—C34 | 123.7 (2) |
C17—N5—C24 | 108.9 (2) | N9—C33—C34 | 108.8 (2) |
C17—N5—Mg1 | 122.9 (1) | C35—C34—C39 | 121.1 (2) |
C24—N5—Mg1 | 126.7 (1) | C35—C34—C33 | 132.1 (2) |
C25—N6—C24 | 123.5 (2) | C39—C34—C33 | 106.8 (2) |
C25—N7—C32 | 108.6 (2) | C34—C35—C36 | 117.4 (2) |
C25—N7—Mg1 | 127.7 (1) | C34—C35—H35 | 121.3 |
C32—N7—Mg1 | 123.4 (1) | C36—C35—H35 | 121.3 |
C1—N8—C32 | 123.7 (2) | C35—C36—C37 | 121.6 (2) |
N8—C1—N1 | 129.1 (2) | C35—C36—H36 | 119.2 |
N8—C1—C2 | 122.7 (2) | C37—C36—H36 | 119.2 |
N1—C1—C2 | 108.2 (2) | C38—C37—C36 | 121.0 (2) |
C3—C2—C7 | 121.9 (2) | C38—C37—H37 | 119.5 |
C3—C2—C1 | 131.6 (2) | C36—C37—H37 | 119.5 |
C7—C2—C1 | 106.4 (2) | C37—C38—C39 | 117.5 (2) |
C2—C3—C4 | 117.4 (2) | C37—C38—H38 | 121.2 |
C2—C3—H3 | 121.3 | C39—C38—H38 | 121.2 |
C4—C3—H3 | 121.3 | C34—C39—C38 | 121.5 (2) |
C5—C4—C3 | 121.3 (2) | C34—C39—C40 | 106.1 (2) |
C5—C4—H4 | 119.4 | C38—C39—C40 | 132.5 (2) |
C3—C4—H4 | 119.4 | N10—C40—N9 | 127.7 (2) |
C4—C5—C6 | 121.8 (2) | N10—C40—C39 | 123.0 (2) |
C4—C5—H5 | 119.1 | N9—C40—C39 | 109.3 (2) |
C6—C5—H5 | 119.1 | N10—C41—N11 | 127.8 (2) |
C7—C6—C5 | 117.5 (2) | N10—C41—C42 | 122.2 (2) |
C7—C6—H6 | 121.3 | N11—C41—C42 | 109.9 (2) |
C5—C6—H6 | 121.3 | C43—C42—C47 | 121.8 (2) |
C6—C7—C2 | 120.2 (2) | C43—C42—C41 | 132.3 (2) |
C6—C7—C8 | 133.4 (2) | C47—C42—C41 | 105.7 (2) |
C2—C7—C8 | 106.3 (2) | C44—C43—C42 | 117.1 (2) |
N2—C8—N1 | 127.7 (2) | C44—C43—H43 | 121.5 |
N2—C8—C7 | 122.6 (2) | C42—C43—H43 | 121.5 |
N1—C8—C7 | 109.7 (2) | C43—C44—C45 | 121.0 (2) |
N2—C9—N3 | 128.3 (2) | C43—C44—H44 | 119.5 |
N2—C9—C10 | 122.4 (2) | C45—C44—H44 | 119.5 |
N3—C9—C10 | 109.3 (2) | C46—C45—C44 | 121.6 (2) |
C11—C10—C15 | 121.6 (2) | C46—C45—H45 | 119.2 |
C11—C10—C9 | 132.4 (2) | C44—C45—H45 | 119.2 |
C15—C10—C9 | 106.0 (2) | C47—C46—C45 | 117.5 (2) |
C12—C11—C10 | 117.7 (2) | C47—C46—H46 | 121.2 |
C12—C11—H11 | 121.1 | C45—C46—H46 | 121.2 |
C10—C11—H11 | 121.1 | C46—C47—C42 | 121.0 (2) |
C11—C12—C13 | 121.2 (2) | C46—C47—C48 | 131.7 (2) |
C11—C12—H12 | 119.4 | C42—C47—C48 | 107.2 (2) |
C13—C12—H12 | 119.4 | N12—C48—N11 | 128.1 (2) |
C14—C13—C12 | 121.1 (2) | N12—C48—C47 | 123.9 (2) |
C14—C13—H13 | 119.5 | N11—C48—C47 | 107.9 (2) |
C12—C13—H13 | 119.5 | N12—C49—N13 | 128.3 (2) |
C13—C14—C15 | 118.2 (2) | N12—C49—C50 | 122.3 (2) |
C13—C14—H14 | 120.9 | N13—C49—C50 | 109.4 (2) |
C15—C14—H14 | 120.9 | C51—C50—C55 | 121.9 (2) |
C14—C15—C10 | 120.2 (2) | C51—C50—C49 | 130.8 (2) |
C14—C15—C16 | 133.3 (2) | C55—C50—C49 | 107.3 (2) |
C10—C15—C16 | 106.5 (2) | C52—C51—C50 | 118.0 (2) |
N4—C16—N3 | 127.4 (2) | C52—C51—H51 | 121.0 |
N4—C16—C15 | 123.4 (2) | C50—C51—H51 | 121.0 |
N3—C16—C15 | 109.3 (2) | C51—C52—C53 | 120.8 (2) |
N4—C17—N5 | 128.7 (2) | C51—C52—H52 | 119.6 |
N4—C17—C18 | 122.3 (2) | C53—C52—H52 | 119.6 |
N5—C17—C18 | 109.0 (2) | C54—C53—C52 | 121.4 (2) |
C19—C18—C23 | 122.1 (2) | C54—C53—H53 | 119.3 |
C19—C18—C17 | 131.1 (2) | C52—C53—H53 | 119.3 |
C23—C18—C17 | 106.9 (2) | C53—C54—C55 | 118.5 (2) |
C20—C19—C18 | 117.6 (2) | C53—C54—H54 | 120.7 |
C20—C19—H19 | 121.2 | C55—C54—H54 | 120.7 |
C18—C19—H19 | 121.2 | C50—C55—C54 | 119.2 (2) |
C19—C20—C21 | 120.8 (2) | C50—C55—C56 | 105.1 (2) |
C19—C20—H20 | 119.6 | C54—C55—C56 | 135.6 (2) |
C21—C20—H20 | 119.6 | N14—C56—N13 | 126.5 (2) |
C22—C21—C20 | 121.5 (2) | N14—C56—C55 | 123.7 (2) |
C22—C21—H21 | 119.3 | N13—C56—C55 | 109.8 (2) |
C20—C21—H21 | 119.3 | N14—C57—N15 | 127.2 (2) |
C21—C22—C23 | 118.1 (2) | N14—C57—C58 | 123.6 (2) |
C21—C22—H22 | 121.0 | N15—C57—C58 | 109.2 (2) |
C23—C22—H22 | 121.0 | C59—C58—C63 | 120.1 (2) |
C22—C23—C18 | 119.9 (2) | C59—C58—C57 | 134.3 (2) |
C22—C23—C24 | 134.2 (2) | C63—C58—C57 | 105.6 (2) |
C18—C23—C24 | 105.9 (2) | C60—C59—C58 | 117.8 (2) |
N6—C24—N5 | 126.7 (2) | C60—C59—H59 | 121.1 |
N6—C24—C23 | 124.0 (2) | C58—C59—H59 | 121.1 |
N5—C24—C23 | 109.3 (2) | C59—C60—C61 | 121.7 (2) |
N6—C25—N7 | 126.7 (2) | C59—C60—H60 | 119.2 |
N6—C25—C26 | 123.4 (2) | C61—C60—H60 | 119.2 |
N7—C25—C26 | 109.9 (2) | C60—C61—C62 | 121.2 (2) |
C27—C26—C31 | 119.4 (2) | C60—C61—H61 | 119.4 |
C27—C26—C25 | 135.0 (2) | C62—C61—H61 | 119.4 |
C31—C26—C25 | 105.6 (2) | C63—C62—C61 | 116.8 (2) |
C28—C27—C26 | 118.4 (2) | C63—C62—H62 | 121.6 |
C28—C27—H27 | 120.8 | C61—C62—H62 | 121.6 |
C26—C27—H27 | 120.8 | C62—C63—C58 | 122.5 (2) |
C27—C28—C29 | 121.0 (2) | C62—C63—C64 | 130.1 (2) |
C27—C28—H28 | 119.5 | C58—C63—C64 | 107.4 (2) |
C29—C28—H28 | 119.5 | N16—C64—N15 | 128.6 (2) |
C30—C29—C28 | 121.7 (2) | N16—C64—C63 | 122.7 (2) |
C30—C29—H29 | 119.1 | N15—C64—C63 | 108.7 (2) |
D—H···A | D—H | H···A | D···A | D—H···A |
O1—H1O1···N6i | 0.84 (2) | 2.02 (2) | 2.837 (3) | 164 (2) |
O2—H2O2···N14ii | 0.82 (2) | 1.97 (2) | 2.776 (3) | 166 (2) |
Symmetry codes: (i) −x+1, −y, −z+1; (ii) −x+1, −y, −z. |
Experimental details
Crystal data | |
Chemical formula | [Mg(C32H16MgN8)(H2O)] |
Mr | 554.86 |
Crystal system, space group | Triclinic, P1 |
Temperature (K) | 200 |
a, b, c (Å) | 12.955 (2), 13.293 (3), 16.202 (3) |
α, β, γ (°) | 65.03 (2), 81.91 (2), 83.73 (2) |
V (Å3) | 2500.3 (9) |
Z | 4 |
Radiation type | Mo Kα |
µ (mm−1) | 0.12 |
Crystal size (mm) | 0.25 × 0.22 × 0.16 |
Data collection | |
Diffractometer | Nonius CCD area-detector diffractometer |
Absorption correction | Analytical face-indexed (SHELXTL; Sheldrick, 1990) |
Tmin, Tmax | 0.966, 0.982 |
No. of measured, independent and observed [I > 2σ(I)] reflections | 47310, 11221, 8172 |
Rint | 0.040 |
(sin θ/λ)max (Å−1) | 0.648 |
Refinement | |
R[F2 > 2σ(F2)], wR(F2), S | 0.049, 0.099, 1.04 |
No. of reflections | 11221 |
No. of parameters | 769 |
H-atom treatment | H atoms treated by a mixture of independent and constrained refinement |
Δρmax, Δρmin (e Å−3) | 0.37, −0.29 |
Computer programs: COLLECT (Nonius, 1997-2000), COLLECT, SHELXS97 (Sheldrick, 1990a), SHELXL97 (Sheldrick, 1997), SHELXTL (Sheldrick, 1990b), SHELXL97.
Mg1—O1 | 2.029 (2) | Mg2—O2 | 2.048 (2) |
Mg1—N1 | 2.039 (2) | Mg2—N9 | 2.055 (2) |
Mg1—N5 | 2.049 (2) | Mg2—N13 | 2.055 (2) |
Mg1—N3 | 2.053 (2) | Mg2—N11 | 2.048 (2) |
Mg1—N7 | 2.055 (2) | Mg2—N15 | 2.056 (2) |
O1—Mg1—N1 | 102.00 (6) | O2—Mg2—N9 | 105.07 (6) |
O1—Mg1—N5 | 103.58 (6) | O2—Mg2—N13 | 101.63 (6) |
N1—Mg1—N5 | 154.41 (6) | N13—Mg2—N9 | 153.24 (6) |
O1—Mg1—N3 | 104.09 (6) | O2—Mg2—N11 | 104.53 (6) |
N1—Mg1—N3 | 86.85 (6) | N11—Mg2—N9 | 86.06 (6) |
N5—Mg1—N3 | 87.80 (6) | N11—Mg2—N13 | 88.85 (6) |
O1—Mg1—N7 | 100.71 (6) | O2—Mg2—N15 | 101.42 (6) |
N1—Mg1—N7 | 88.78 (6) | N9—Mg2—N15 | 88.22 (6) |
N5—Mg1—N7 | 85.66 (6) | N13—Mg2—N15 | 84.94 (6) |
N3—Mg1—N7 | 155.18 (6) | N11—Mg2—N15 | 154.03 (6) |
D—H···A | D—H | H···A | D···A | D—H···A |
O1—H1O1···N6i | 0.84 (2) | 2.02 (2) | 2.837 (3) | 164 (2) |
O2—H2O2···N14ii | 0.82 (2) | 1.97 (2) | 2.776 (3) | 166 (2) |
Symmetry codes: (i) −x+1, −y, −z+1; (ii) −x+1, −y, −z. |
Our interest in magnesium phthalocyaninate, MgPc, and its 4 + 1- and 4 + 2-coordinated complexes (Kubiak et al., 1995; Janczak & Kubiak, 2001, 2002) is due to their optical properties in the solid state, especially the X-phase. The literature data related to this phase are inconsistent (Davidson, 1982; Hor & Loutfy, 1983; Krishankumer & Menon, 1997; Sakakibara et al., 2001). Endo et al. (1999) assigned the MgPc(H2O)2 composition to the X-phase. However, until now there is no evidence for the existence of this complex. Quite recently, we have determined the crystal structure of the β-modification of MgPc and, contrary to our expectations, the geometry of MgPc molecule was found to be different from that of other MIIPc compounds in that it is non-planar. The Mg atom in the crystal of MgPc is displaced by 0.557 (2) Å (at 120 K) from the plane defined by the four isoindole N atoms of the Pc2- ring due to the interaction with an azamethine N atom of a neighbouring MgPc molecule (Janczak & Kubiak, 2001).
In the asymmetric unit of the triclinic form of aqua(phthalocyaninato)magnesium, (I), there are two crystallographically independent MgPc(H2O) molecules (Fig. 1). The geometries of these independent molecules are very similar and neither are planar. The central Mg atom in (I) is significantly displaced [0.447 (1) for Mg1 and 0.468 (1) Å for Mg2] from the weighted least-squares plane defined by the four isoindole N atoms towards the water O atom. The displacement of the central Mg atom from the Pc2- plane is comparable to that observed in the other aqua(phthalocyaninato)magnesium complexes (Mizuguchi, 2002; Mizuguchi & Mochizuhi, 2002; Fischer et al., 1977). In the title crystal, the MgPc(H2O) molecules form dimers via intermolecular O—H···Nazamethine hydrogen bonds. These dimers are stacked along the b axis in a herring-bone fashion. The Pc···Pc distances between the benzo rings in the dimers are shorter than the distance of 3.4 Å between π-aromatic ring systems (Pauling, 1960) and indicate strong π–π interactions between the Pc rings. The face-to-face orientation of the MgPc(H2O) molecules in the dimers is similar to the orientation of the MgPc molecules in the crystal, in which, due to intermolecular Mg···Nazamethine interactions, the MgPc molecules also form a dimeric (MgPc)2 structure (Janczak & Kubiak, 2001).
The geometry of the MgPc(H2O) molecules in the triclinic crystals is similar to that of the monoclinic modification, although the refinement parameters of the latter are relatively large (R = 10.6% and wR = 20.9%; Mizuguchi, 2002). The difference between these two crystallographic modifications of MgPc(H2O) can be found only in the arrangements of the molecules in the crystals. In the triclinic crystals, the complex molecules form face-to-face hydrogen-bonded dimers, in contrast with the monoclinic crystals, in which the MgPc(H2O) molecules form a hydrogen-bonded polymeric structure (Mizuguchi, 2002). The differences in the arrangement of MgPc(H2O) molecules between these two crystallographic modifications implicate differences in the solid-state optical properties, the study of which is now in progress (Janczak & Idemori, 2002).