Supporting information
Crystallographic Information File (CIF) https://doi.org/10.1107/S1600536807057352/cv2346sup1.cif | |
Structure factor file (CIF format) https://doi.org/10.1107/S1600536807057352/cv2346Isup2.hkl |
CCDC reference: 672652
Key indicators
- Single-crystal X-ray study
- T = 298 K
- Mean (C-C) = 0.008 Å
- R factor = 0.052
- wR factor = 0.145
- Data-to-parameter ratio = 13.7
checkCIF/PLATON results
No syntax errors found
Alert level B PLAT420_ALERT_2_B D-H Without Acceptor O1 - H38 ... ?
Alert level C RINTA01_ALERT_3_C The value of Rint is greater than 0.10 Rint given 0.133 PLAT020_ALERT_3_C The value of Rint is greater than 0.10 ......... 0.13 PLAT026_ALERT_3_C Ratio Observed / Unique Reflections too Low .... 47 Perc. PLAT042_ALERT_1_C Calc. and Rep. MoietyFormula Strings Differ .... ? PLAT063_ALERT_3_C Crystal Probably too Large for Beam Size ....... 0.66 mm PLAT125_ALERT_4_C No _symmetry_space_group_name_Hall Given ....... ? PLAT152_ALERT_1_C Supplied and Calc Volume s.u. Inconsistent ..... ? PLAT341_ALERT_3_C Low Bond Precision on C-C Bonds (x 1000) Ang ... 8
0 ALERT level A = In general: serious problem 1 ALERT level B = Potentially serious problem 8 ALERT level C = Check and explain 0 ALERT level G = General alerts; check 2 ALERT type 1 CIF construction/syntax error, inconsistent or missing data 1 ALERT type 2 Indicator that the structure model may be wrong or deficient 5 ALERT type 3 Indicator that the structure quality may be low 1 ALERT type 4 Improvement, methodology, query or suggestion 0 ALERT type 5 Informative message, check
For related sodium complexes with 1,10-phenanthroline, see: Qian et al. (1994).
The title compound was prepared by the reaction of sodium(I) bromide (102.9 mg, 1 mmol) with 1,10-phenanthroline (198.2 mg, 1 mmol), in absolute ethanol. After stirring for 5 h at room temperature, the yellow paste was obtained and then filtered. Yellow crystals suitable for X-ray analysis were obtained by slow evaporation of ethanol/dichloromethane (1:1 v/v) solution over a period of two weeks (yield 82%. m.p. 452k).
All H atoms were placed in calculated positions, with C—H = 0.93 Å for aromatic H atoms, O—H = 0.85 Å, and treated as riding on their parent atoms, with Uiso(H) = 1.2 Ueq(C, O).
Data collection: SMART (Siemens, 1996); cell refinement: SAINT (Siemens, 1996); data reduction: SAINT (Siemens, 1996); program(s) used to solve structure: SHELXS97 (Sheldrick, 1997a); program(s) used to refine structure: SHELXL97 (Sheldrick, 1997a); molecular graphics: SHELXTL (Sheldrick, 1997b); software used to prepare material for publication: SHELXTL (Sheldrick, 1997b).
Fig. 1. View of (I) showing 30% probability displacement ellipsoids and the atom-numbering scheme [symmetry code: (A) -x + 1, y + 1/2, -z + 1/2]. H atoms have been omitted for clarity. |
[Na2(C12H8N2)2(H2O)5]Br2·C12H8N2 | F(000) = 1696 |
Mr = 836.49 | Dx = 1.523 Mg m−3 |
Monoclinic, P21/c | Mo Kα radiation, λ = 0.71073 Å |
a = 12.833 (5) Å | Cell parameters from 2683 reflections |
b = 11.445 (5) Å | θ = 2.4–20.9° |
c = 24.888 (10) Å | µ = 2.30 mm−1 |
β = 93.696 (6)° | T = 298 K |
V = 3648 (2) Å3 | Block, yellow |
Z = 4 | 0.66 × 0.32 × 0.10 mm |
CCD area-detector diffractometer | 6336 independent reflections |
Radiation source: fine-focus sealed tube | 3007 reflections with I > 2σ(I) |
Graphite monochromator | Rint = 0.134 |
ϕ and ω scans | θmax = 25.0°, θmin = 1.6° |
Absorption correction: multi-scan (SADABS; Sheldrick, 1996) | h = −12→15 |
Tmin = 0.313, Tmax = 0.803 | k = −13→13 |
18042 measured reflections | l = −29→27 |
Refinement on F2 | Secondary atom site location: difference Fourier map |
Least-squares matrix: full | Hydrogen site location: inferred from neighbouring sites |
R[F2 > 2σ(F2)] = 0.052 | H-atom parameters constrained |
wR(F2) = 0.145 | w = 1/[σ2(Fo2)] |
S = 0.85 | (Δ/σ)max = 0.001 |
6336 reflections | Δρmax = 0.44 e Å−3 |
461 parameters | Δρmin = −0.45 e Å−3 |
0 restraints | Extinction correction: SHELXL, Fc*=kFc[1+0.001xFc2λ3/sin(2θ)]-1/4 |
Primary atom site location: structure-invariant direct methods | Extinction coefficient: 0.0046 (4) |
[Na2(C12H8N2)2(H2O)5]Br2·C12H8N2 | V = 3648 (2) Å3 |
Mr = 836.49 | Z = 4 |
Monoclinic, P21/c | Mo Kα radiation |
a = 12.833 (5) Å | µ = 2.30 mm−1 |
b = 11.445 (5) Å | T = 298 K |
c = 24.888 (10) Å | 0.66 × 0.32 × 0.10 mm |
β = 93.696 (6)° |
CCD area-detector diffractometer | 6336 independent reflections |
Absorption correction: multi-scan (SADABS; Sheldrick, 1996) | 3007 reflections with I > 2σ(I) |
Tmin = 0.313, Tmax = 0.803 | Rint = 0.134 |
18042 measured reflections |
R[F2 > 2σ(F2)] = 0.052 | 0 restraints |
wR(F2) = 0.145 | H-atom parameters constrained |
S = 0.85 | Δρmax = 0.44 e Å−3 |
6336 reflections | Δρmin = −0.45 e Å−3 |
461 parameters |
x | y | z | Uiso*/Ueq | ||
Na1 | 0.39048 (15) | 0.29514 (18) | 0.25029 (8) | 0.0471 (6) | |
Na2 | 0.69832 (15) | 0.45126 (19) | 0.26998 (9) | 0.0512 (6) | |
Br1 | 0.27305 (5) | 0.09245 (6) | 0.39440 (3) | 0.0635 (3) | |
Br2 | 0.72128 (5) | 0.12723 (6) | 0.14815 (3) | 0.0717 (3) | |
N1 | 0.2206 (3) | 0.2379 (4) | 0.20115 (18) | 0.0458 (12) | |
N2 | 0.3897 (3) | 0.3228 (4) | 0.15218 (17) | 0.0405 (11) | |
N3 | 0.6562 (3) | 0.4975 (4) | 0.36179 (18) | 0.0439 (12) | |
N4 | 0.8426 (3) | 0.4056 (4) | 0.33425 (19) | 0.0440 (12) | |
N5 | 0.6283 (3) | 0.1801 (4) | 0.37083 (17) | 0.0407 (11) | |
N6 | 0.7845 (3) | 0.0744 (4) | 0.31736 (18) | 0.0394 (11) | |
O1 | 0.5907 (2) | 0.2818 (3) | 0.26352 (15) | 0.0534 (11) | |
H37 | 0.6010 | 0.2396 | 0.2915 | 0.064* | |
H38 | 0.6015 | 0.2375 | 0.2370 | 0.064* | |
O2 | 0.3959 (2) | 0.5093 (3) | 0.24641 (14) | 0.0487 (10) | |
H39 | 0.3860 | 0.5352 | 0.2777 | 0.058* | |
H40 | 0.3525 | 0.5385 | 0.2229 | 0.058* | |
O3 | 0.4043 (2) | 0.0894 (3) | 0.27973 (14) | 0.0471 (10) | |
H41 | 0.4668 | 0.0645 | 0.2822 | 0.056* | |
H42 | 0.3934 | 0.0904 | 0.3131 | 0.056* | |
O4 | 0.3149 (3) | 0.3385 (4) | 0.33216 (17) | 0.0831 (14) | |
H43 | 0.2852 | 0.2771 | 0.3428 | 0.100* | |
H44 | 0.2891 | 0.4022 | 0.3428 | 0.100* | |
O5 | 0.7918 (3) | 0.3920 (4) | 0.19641 (17) | 0.0718 (13) | |
H45 | 0.7634 | 0.3287 | 0.1852 | 0.086* | |
H46 | 0.7714 | 0.4131 | 0.1647 | 0.086* | |
C1 | 0.1379 (5) | 0.1980 (5) | 0.2253 (3) | 0.0556 (16) | |
H1 | 0.1443 | 0.1824 | 0.2621 | 0.067* | |
C2 | 0.0410 (4) | 0.1790 (5) | 0.1967 (3) | 0.0614 (18) | |
H2A | −0.0154 | 0.1515 | 0.2147 | 0.074* | |
C3 | 0.0295 (4) | 0.2006 (5) | 0.1431 (3) | 0.0560 (17) | |
H3 | −0.0345 | 0.1881 | 0.1243 | 0.067* | |
C4 | 0.1144 (4) | 0.2419 (5) | 0.1165 (2) | 0.0403 (14) | |
C5 | 0.2100 (4) | 0.2599 (4) | 0.1478 (2) | 0.0353 (13) | |
C6 | 0.2977 (4) | 0.3069 (4) | 0.1214 (2) | 0.0331 (13) | |
C7 | 0.2886 (4) | 0.3349 (4) | 0.0668 (2) | 0.0378 (13) | |
C8 | 0.3746 (4) | 0.3851 (5) | 0.0433 (2) | 0.0476 (15) | |
H8 | 0.3701 | 0.4057 | 0.0071 | 0.057* | |
C9 | 0.4642 (4) | 0.4031 (5) | 0.0740 (3) | 0.0540 (17) | |
H9 | 0.5219 | 0.4371 | 0.0595 | 0.065* | |
C10 | 0.4678 (4) | 0.3695 (5) | 0.1279 (3) | 0.0496 (16) | |
H10 | 0.5302 | 0.3809 | 0.1483 | 0.060* | |
C11 | 0.1097 (4) | 0.2689 (5) | 0.0603 (2) | 0.0522 (17) | |
H11 | 0.0482 | 0.2545 | 0.0396 | 0.063* | |
C12 | 0.1908 (4) | 0.3140 (5) | 0.0370 (2) | 0.0459 (15) | |
H12 | 0.1841 | 0.3324 | 0.0006 | 0.055* | |
C13 | 0.5678 (4) | 0.5410 (5) | 0.3758 (3) | 0.0530 (17) | |
H13 | 0.5160 | 0.5541 | 0.3486 | 0.064* | |
C14 | 0.5449 (5) | 0.5694 (5) | 0.4282 (3) | 0.0562 (17) | |
H14 | 0.4809 | 0.6017 | 0.4355 | 0.067* | |
C15 | 0.6198 (5) | 0.5479 (5) | 0.4681 (3) | 0.0557 (17) | |
H15 | 0.6072 | 0.5649 | 0.5036 | 0.067* | |
C16 | 0.7162 (4) | 0.5002 (5) | 0.4557 (2) | 0.0443 (15) | |
C17 | 0.7323 (4) | 0.4761 (4) | 0.4011 (2) | 0.0390 (14) | |
C18 | 0.8299 (4) | 0.4284 (4) | 0.3866 (2) | 0.0383 (14) | |
C19 | 0.9086 (4) | 0.4064 (5) | 0.4284 (2) | 0.0441 (15) | |
C20 | 1.0038 (5) | 0.3614 (5) | 0.4122 (3) | 0.0618 (19) | |
H20 | 1.0580 | 0.3460 | 0.4378 | 0.074* | |
C21 | 1.0167 (4) | 0.3404 (5) | 0.3599 (3) | 0.0645 (19) | |
H21 | 1.0796 | 0.3110 | 0.3491 | 0.077* | |
C22 | 0.9332 (5) | 0.3640 (5) | 0.3217 (3) | 0.0550 (17) | |
H22 | 0.9430 | 0.3493 | 0.2856 | 0.066* | |
C23 | 0.7965 (5) | 0.4725 (5) | 0.4960 (2) | 0.0561 (17) | |
H23 | 0.7852 | 0.4851 | 0.5321 | 0.067* | |
C24 | 0.8876 (5) | 0.4289 (5) | 0.4826 (3) | 0.0571 (18) | |
H24 | 0.9389 | 0.4127 | 0.5097 | 0.069* | |
C25 | 0.5517 (4) | 0.2223 (5) | 0.3984 (3) | 0.0533 (16) | |
H25 | 0.4899 | 0.2447 | 0.3796 | 0.064* | |
C26 | 0.5591 (5) | 0.2346 (5) | 0.4542 (3) | 0.0595 (18) | |
H26 | 0.5020 | 0.2608 | 0.4720 | 0.071* | |
C27 | 0.6503 (5) | 0.2081 (5) | 0.4823 (2) | 0.0581 (17) | |
H27 | 0.6571 | 0.2193 | 0.5193 | 0.070* | |
C28 | 0.7335 (4) | 0.1641 (5) | 0.4552 (2) | 0.0440 (14) | |
C29 | 0.7192 (4) | 0.1479 (4) | 0.3996 (2) | 0.0375 (14) | |
C30 | 0.8015 (4) | 0.0986 (4) | 0.3698 (2) | 0.0360 (13) | |
C31 | 0.8991 (4) | 0.0763 (5) | 0.3987 (3) | 0.0435 (15) | |
C32 | 0.9783 (4) | 0.0304 (5) | 0.3684 (3) | 0.0536 (17) | |
H32 | 1.0435 | 0.0147 | 0.3853 | 0.064* | |
C33 | 0.9615 (4) | 0.0087 (5) | 0.3154 (3) | 0.0587 (18) | |
H33 | 1.0147 | −0.0198 | 0.2954 | 0.070* | |
C34 | 0.8624 (4) | 0.0300 (5) | 0.2914 (2) | 0.0523 (16) | |
H34 | 0.8501 | 0.0121 | 0.2550 | 0.063* | |
C35 | 0.8314 (5) | 0.1364 (5) | 0.4821 (2) | 0.0576 (18) | |
H35 | 0.8407 | 0.1462 | 0.5191 | 0.069* | |
C36 | 0.9105 (5) | 0.0961 (5) | 0.4546 (3) | 0.0605 (18) | |
H36 | 0.9746 | 0.0809 | 0.4729 | 0.073* |
U11 | U22 | U33 | U12 | U13 | U23 | |
Na1 | 0.0494 (12) | 0.0529 (15) | 0.0386 (14) | 0.0009 (10) | −0.0001 (10) | 0.0058 (11) |
Na2 | 0.0506 (13) | 0.0624 (16) | 0.0397 (15) | −0.0020 (11) | −0.0049 (11) | 0.0047 (11) |
Br1 | 0.0607 (4) | 0.0888 (6) | 0.0419 (4) | −0.0109 (4) | 0.0097 (3) | −0.0017 (3) |
Br2 | 0.0713 (5) | 0.0805 (6) | 0.0630 (5) | −0.0209 (4) | 0.0012 (4) | 0.0103 (4) |
N1 | 0.046 (3) | 0.054 (3) | 0.038 (3) | 0.005 (2) | 0.002 (2) | 0.007 (2) |
N2 | 0.039 (3) | 0.051 (3) | 0.032 (3) | −0.006 (2) | 0.001 (2) | −0.006 (2) |
N3 | 0.038 (3) | 0.051 (3) | 0.043 (3) | 0.003 (2) | −0.003 (2) | 0.002 (2) |
N4 | 0.043 (3) | 0.050 (3) | 0.039 (3) | 0.002 (2) | 0.004 (2) | 0.001 (2) |
N5 | 0.036 (2) | 0.049 (3) | 0.038 (3) | −0.002 (2) | 0.010 (2) | 0.002 (2) |
N6 | 0.038 (3) | 0.049 (3) | 0.031 (3) | −0.003 (2) | 0.006 (2) | −0.003 (2) |
O1 | 0.057 (2) | 0.052 (3) | 0.050 (3) | −0.0047 (19) | −0.002 (2) | 0.005 (2) |
O2 | 0.050 (2) | 0.063 (3) | 0.032 (2) | 0.0016 (19) | −0.0075 (18) | 0.0049 (19) |
O3 | 0.044 (2) | 0.063 (3) | 0.034 (2) | 0.0036 (18) | 0.0029 (17) | 0.0087 (19) |
O4 | 0.118 (4) | 0.067 (3) | 0.069 (3) | 0.015 (3) | 0.046 (3) | 0.004 (2) |
O5 | 0.081 (3) | 0.083 (4) | 0.052 (3) | −0.002 (2) | 0.010 (2) | −0.001 (2) |
C1 | 0.063 (4) | 0.056 (4) | 0.049 (4) | 0.002 (3) | 0.014 (3) | 0.005 (3) |
C2 | 0.045 (4) | 0.062 (5) | 0.080 (6) | −0.004 (3) | 0.026 (4) | 0.010 (4) |
C3 | 0.041 (3) | 0.054 (4) | 0.072 (5) | −0.005 (3) | 0.002 (3) | −0.001 (4) |
C4 | 0.034 (3) | 0.043 (4) | 0.043 (4) | 0.001 (3) | −0.002 (3) | −0.001 (3) |
C5 | 0.039 (3) | 0.029 (3) | 0.039 (4) | 0.007 (2) | 0.009 (3) | 0.004 (3) |
C6 | 0.040 (3) | 0.032 (3) | 0.028 (3) | 0.005 (2) | 0.006 (3) | −0.005 (2) |
C7 | 0.053 (3) | 0.032 (3) | 0.028 (3) | 0.007 (3) | 0.001 (3) | −0.005 (3) |
C8 | 0.059 (4) | 0.049 (4) | 0.036 (4) | 0.000 (3) | 0.014 (3) | 0.007 (3) |
C9 | 0.052 (4) | 0.058 (4) | 0.054 (5) | −0.013 (3) | 0.022 (3) | −0.004 (3) |
C10 | 0.045 (3) | 0.049 (4) | 0.055 (5) | −0.010 (3) | 0.003 (3) | −0.013 (3) |
C11 | 0.050 (4) | 0.052 (4) | 0.052 (5) | −0.001 (3) | −0.020 (3) | −0.003 (3) |
C12 | 0.052 (4) | 0.060 (4) | 0.025 (3) | 0.002 (3) | −0.004 (3) | 0.000 (3) |
C13 | 0.036 (3) | 0.050 (4) | 0.073 (5) | 0.006 (3) | −0.002 (3) | 0.004 (3) |
C14 | 0.051 (4) | 0.060 (5) | 0.058 (5) | 0.006 (3) | 0.013 (4) | −0.004 (4) |
C15 | 0.067 (4) | 0.054 (4) | 0.048 (4) | 0.000 (3) | 0.012 (4) | −0.009 (3) |
C16 | 0.048 (3) | 0.042 (4) | 0.043 (4) | −0.005 (3) | 0.002 (3) | −0.006 (3) |
C17 | 0.044 (3) | 0.033 (3) | 0.040 (4) | −0.009 (3) | 0.005 (3) | 0.003 (3) |
C18 | 0.036 (3) | 0.034 (3) | 0.043 (4) | 0.001 (2) | −0.005 (3) | 0.001 (3) |
C19 | 0.042 (3) | 0.044 (4) | 0.044 (4) | −0.004 (3) | −0.009 (3) | 0.003 (3) |
C20 | 0.044 (4) | 0.074 (5) | 0.066 (5) | 0.005 (3) | −0.004 (4) | −0.001 (4) |
C21 | 0.043 (4) | 0.069 (5) | 0.084 (6) | 0.010 (3) | 0.013 (4) | 0.007 (4) |
C22 | 0.057 (4) | 0.061 (4) | 0.049 (4) | 0.006 (3) | 0.014 (3) | 0.005 (3) |
C23 | 0.074 (4) | 0.059 (4) | 0.034 (4) | −0.006 (4) | −0.005 (3) | 0.002 (3) |
C24 | 0.062 (4) | 0.058 (4) | 0.047 (5) | 0.003 (3) | −0.025 (4) | 0.005 (3) |
C25 | 0.046 (4) | 0.059 (4) | 0.055 (5) | −0.007 (3) | 0.005 (3) | 0.001 (3) |
C26 | 0.054 (4) | 0.065 (5) | 0.063 (5) | −0.005 (3) | 0.030 (4) | −0.004 (4) |
C27 | 0.076 (4) | 0.062 (5) | 0.039 (4) | −0.013 (4) | 0.019 (4) | −0.005 (3) |
C28 | 0.055 (4) | 0.042 (4) | 0.036 (4) | −0.008 (3) | 0.004 (3) | 0.002 (3) |
C29 | 0.033 (3) | 0.039 (3) | 0.041 (4) | −0.006 (2) | 0.002 (3) | 0.010 (3) |
C30 | 0.032 (3) | 0.036 (3) | 0.039 (4) | −0.007 (2) | 0.002 (3) | −0.002 (3) |
C31 | 0.039 (3) | 0.040 (4) | 0.050 (4) | −0.003 (3) | −0.007 (3) | 0.009 (3) |
C32 | 0.032 (3) | 0.054 (4) | 0.075 (5) | 0.004 (3) | −0.005 (3) | 0.010 (4) |
C33 | 0.039 (4) | 0.066 (5) | 0.072 (5) | −0.001 (3) | 0.016 (4) | 0.003 (4) |
C34 | 0.051 (4) | 0.060 (4) | 0.047 (4) | −0.009 (3) | 0.013 (3) | −0.008 (3) |
C35 | 0.075 (5) | 0.064 (5) | 0.031 (4) | −0.014 (4) | −0.015 (4) | 0.004 (3) |
C36 | 0.054 (4) | 0.064 (5) | 0.061 (5) | 0.008 (3) | −0.017 (4) | 0.015 (4) |
Na1—O4 | 2.365 (5) | C8—C9 | 1.356 (7) |
Na1—O2 | 2.454 (4) | C8—H8 | 0.9300 |
Na1—N2 | 2.462 (5) | C9—C10 | 1.392 (8) |
Na1—O3 | 2.469 (4) | C9—H9 | 0.9300 |
Na1—N1 | 2.517 (5) | C10—H10 | 0.9300 |
Na1—O1 | 2.574 (4) | C11—C12 | 1.328 (7) |
Na1—Na2i | 4.119 (3) | C11—H11 | 0.9300 |
Na2—O5 | 2.353 (5) | C12—H12 | 0.9300 |
Na2—O3ii | 2.357 (4) | C13—C14 | 1.393 (8) |
Na2—O1 | 2.380 (4) | C13—H13 | 0.9300 |
Na2—N4 | 2.425 (5) | C14—C15 | 1.359 (7) |
Na2—N3 | 2.440 (5) | C14—H14 | 0.9300 |
Na2—Na1ii | 4.119 (3) | C15—C16 | 1.405 (7) |
N1—C1 | 1.334 (7) | C15—H15 | 0.9300 |
N1—C5 | 1.350 (6) | C16—C17 | 1.413 (7) |
N2—C10 | 1.317 (7) | C16—C23 | 1.427 (7) |
N2—C6 | 1.376 (6) | C17—C18 | 1.433 (7) |
N3—C13 | 1.306 (6) | C18—C19 | 1.424 (7) |
N3—C17 | 1.360 (6) | C19—C20 | 1.408 (8) |
N4—C22 | 1.312 (6) | C19—C24 | 1.417 (8) |
N4—C18 | 1.350 (7) | C20—C21 | 1.343 (9) |
N5—C25 | 1.326 (7) | C20—H20 | 0.9300 |
N5—C29 | 1.380 (6) | C21—C22 | 1.412 (8) |
N6—C34 | 1.327 (7) | C21—H21 | 0.9300 |
N6—C30 | 1.338 (6) | C22—H22 | 0.9300 |
O1—H37 | 0.8500 | C23—C24 | 1.333 (8) |
O1—H38 | 0.8500 | C23—H23 | 0.9300 |
O2—H39 | 0.8500 | C24—H24 | 0.9300 |
O2—H40 | 0.8500 | C25—C26 | 1.391 (8) |
O3—Na2i | 2.357 (4) | C25—H25 | 0.9300 |
O3—H41 | 0.8500 | C26—C27 | 1.359 (7) |
O3—H42 | 0.8499 | C26—H26 | 0.9300 |
O4—H43 | 0.8499 | C27—C28 | 1.393 (7) |
O4—H44 | 0.8500 | C27—H27 | 0.9300 |
O5—H45 | 0.8501 | C28—C29 | 1.395 (7) |
O5—H46 | 0.8500 | C28—C35 | 1.421 (7) |
C1—C2 | 1.410 (8) | C29—C30 | 1.444 (7) |
C1—H1 | 0.9300 | C30—C31 | 1.427 (7) |
C2—C3 | 1.354 (8) | C31—C32 | 1.406 (8) |
C2—H2A | 0.9300 | C31—C36 | 1.408 (8) |
C3—C4 | 1.394 (7) | C32—C33 | 1.345 (8) |
C3—H3 | 0.9300 | C32—H32 | 0.9300 |
C4—C5 | 1.425 (6) | C33—C34 | 1.392 (7) |
C4—C11 | 1.428 (7) | C33—H33 | 0.9300 |
C5—C6 | 1.444 (7) | C34—H34 | 0.9300 |
C6—C7 | 1.394 (7) | C35—C36 | 1.342 (8) |
C7—C8 | 1.404 (7) | C35—H35 | 0.9300 |
C7—C12 | 1.436 (7) | C36—H36 | 0.9300 |
O4—Na1—O2 | 80.71 (15) | C6—C7—C12 | 118.7 (5) |
O4—Na1—N2 | 148.42 (17) | C8—C7—C12 | 122.5 (5) |
O2—Na1—N2 | 80.27 (14) | C9—C8—C7 | 119.3 (5) |
O4—Na1—O3 | 88.29 (15) | C9—C8—H8 | 120.4 |
O2—Na1—O3 | 164.26 (14) | C7—C8—H8 | 120.4 |
N2—Na1—O3 | 114.36 (15) | C8—C9—C10 | 118.3 (5) |
O4—Na1—N1 | 94.76 (17) | C8—C9—H9 | 120.8 |
O2—Na1—N1 | 105.47 (14) | C10—C9—H9 | 120.8 |
N2—Na1—N1 | 66.62 (15) | N2—C10—C9 | 125.1 (5) |
O3—Na1—N1 | 86.52 (14) | N2—C10—H10 | 117.4 |
O4—Na1—O1 | 111.33 (16) | C9—C10—H10 | 117.4 |
O2—Na1—O1 | 91.93 (12) | C12—C11—C4 | 121.8 (5) |
N2—Na1—O1 | 94.29 (14) | C12—C11—H11 | 119.1 |
O3—Na1—O1 | 81.57 (12) | C4—C11—H11 | 119.1 |
N1—Na1—O1 | 150.81 (16) | C11—C12—C7 | 121.5 (5) |
O4—Na1—Na2i | 100.40 (13) | C11—C12—H12 | 119.2 |
O2—Na1—Na2i | 163.28 (10) | C7—C12—H12 | 119.2 |
N2—Na1—Na2i | 91.01 (12) | N3—C13—C14 | 125.3 (6) |
O3—Na1—Na2i | 30.59 (8) | N3—C13—H13 | 117.4 |
N1—Na1—Na2i | 57.83 (11) | C14—C13—H13 | 117.4 |
O1—Na1—Na2i | 103.00 (10) | C15—C14—C13 | 117.4 (6) |
O5—Na2—O3ii | 94.63 (15) | C15—C14—H14 | 121.3 |
O5—Na2—O1 | 92.00 (16) | C13—C14—H14 | 121.3 |
O3ii—Na2—O1 | 102.07 (14) | C14—C15—C16 | 120.0 (6) |
O5—Na2—N4 | 92.58 (17) | C14—C15—H15 | 120.0 |
O3ii—Na2—N4 | 150.24 (17) | C16—C15—H15 | 120.0 |
O1—Na2—N4 | 106.50 (16) | C15—C16—C17 | 118.2 (5) |
O5—Na2—N3 | 161.14 (16) | C15—C16—C23 | 122.5 (6) |
O3ii—Na2—N3 | 101.31 (16) | C17—C16—C23 | 119.2 (5) |
O1—Na2—N3 | 94.43 (15) | N3—C17—C16 | 120.9 (5) |
N4—Na2—N3 | 68.60 (16) | N3—C17—C18 | 119.1 (5) |
O5—Na2—Na1ii | 109.34 (13) | C16—C17—C18 | 120.0 (5) |
O3ii—Na2—Na1ii | 32.22 (9) | N4—C18—C19 | 123.0 (5) |
O1—Na2—Na1ii | 127.99 (11) | N4—C18—C17 | 118.7 (5) |
N4—Na2—Na1ii | 118.71 (13) | C19—C18—C17 | 118.3 (5) |
N3—Na2—Na1ii | 80.29 (12) | C20—C19—C24 | 124.2 (5) |
C1—N1—C5 | 118.4 (4) | C20—C19—C18 | 116.3 (6) |
C1—N1—Na1 | 124.0 (4) | C24—C19—C18 | 119.5 (5) |
C5—N1—Na1 | 117.3 (3) | C21—C20—C19 | 120.4 (6) |
C10—N2—C6 | 116.7 (5) | C21—C20—H20 | 119.8 |
C10—N2—Na1 | 123.6 (4) | C19—C20—H20 | 119.8 |
C6—N2—Na1 | 118.9 (3) | C20—C21—C22 | 118.8 (6) |
C13—N3—C17 | 118.2 (5) | C20—C21—H21 | 120.6 |
C13—N3—Na2 | 125.5 (4) | C22—C21—H21 | 120.6 |
C17—N3—Na2 | 116.3 (4) | N4—C22—C21 | 123.7 (6) |
C22—N4—C18 | 117.7 (5) | N4—C22—H22 | 118.2 |
C22—N4—Na2 | 124.9 (4) | C21—C22—H22 | 118.2 |
C18—N4—Na2 | 117.4 (3) | C24—C23—C16 | 120.8 (6) |
C25—N5—C29 | 117.3 (5) | C24—C23—H23 | 119.6 |
C34—N6—C30 | 118.3 (4) | C16—C23—H23 | 119.6 |
Na2—O1—Na1 | 122.02 (16) | C23—C24—C19 | 122.0 (5) |
Na2—O1—H37 | 110.4 | C23—C24—H24 | 119.0 |
Na1—O1—H37 | 103.9 | C19—C24—H24 | 119.0 |
Na2—O1—H38 | 114.6 | N5—C25—C26 | 123.3 (5) |
Na1—O1—H38 | 98.4 | N5—C25—H25 | 118.4 |
H37—O1—H38 | 105.8 | C26—C25—H25 | 118.4 |
Na1—O2—H39 | 107.8 | C27—C26—C25 | 119.5 (6) |
Na1—O2—H40 | 113.6 | C27—C26—H26 | 120.3 |
H39—O2—H40 | 111.3 | C25—C26—H26 | 120.3 |
Na2i—O3—Na1 | 117.19 (15) | C26—C27—C28 | 119.5 (6) |
Na2i—O3—H41 | 107.9 | C26—C27—H27 | 120.2 |
Na1—O3—H41 | 113.0 | C28—C27—H27 | 120.2 |
Na2i—O3—H42 | 113.6 | C27—C28—C29 | 118.2 (5) |
Na1—O3—H42 | 105.3 | C27—C28—C35 | 122.3 (6) |
H41—O3—H42 | 98.4 | C29—C28—C35 | 119.5 (6) |
Na1—O4—H43 | 108.2 | N5—C29—C28 | 122.1 (5) |
Na1—O4—H44 | 129.6 | N5—C29—C30 | 117.3 (5) |
H43—O4—H44 | 114.9 | C28—C29—C30 | 120.5 (5) |
Na2—O5—H45 | 105.8 | N6—C30—C31 | 122.4 (5) |
Na2—O5—H46 | 119.8 | N6—C30—C29 | 120.3 (4) |
H45—O5—H46 | 80.6 | C31—C30—C29 | 117.3 (5) |
N1—C1—C2 | 121.7 (6) | C32—C31—C36 | 123.9 (5) |
N1—C1—H1 | 119.1 | C32—C31—C30 | 116.0 (6) |
C2—C1—H1 | 119.1 | C36—C31—C30 | 120.1 (5) |
C3—C2—C1 | 120.4 (6) | C33—C32—C31 | 121.3 (5) |
C3—C2—H2A | 119.8 | C33—C32—H32 | 119.3 |
C1—C2—H2A | 119.8 | C31—C32—H32 | 119.3 |
C2—C3—C4 | 119.4 (5) | C32—C33—C34 | 118.2 (6) |
C2—C3—H3 | 120.3 | C32—C33—H33 | 120.9 |
C4—C3—H3 | 120.3 | C34—C33—H33 | 120.9 |
C3—C4—C5 | 117.4 (5) | N6—C34—C33 | 123.6 (6) |
C3—C4—C11 | 123.6 (5) | N6—C34—H34 | 118.2 |
C5—C4—C11 | 119.0 (5) | C33—C34—H34 | 118.2 |
N1—C5—C4 | 122.7 (5) | C36—C35—C28 | 120.8 (6) |
N1—C5—C6 | 119.0 (4) | C36—C35—H35 | 119.6 |
C4—C5—C6 | 118.3 (5) | C28—C35—H35 | 119.6 |
N2—C6—C7 | 121.8 (5) | C35—C36—C31 | 121.7 (5) |
N2—C6—C5 | 117.5 (5) | C35—C36—H36 | 119.2 |
C7—C6—C5 | 120.7 (4) | C31—C36—H36 | 119.2 |
C6—C7—C8 | 118.7 (5) |
Symmetry codes: (i) −x+1, y−1/2, −z+1/2; (ii) −x+1, y+1/2, −z+1/2. |
D—H···A | D—H | H···A | D···A | D—H···A |
O1—H37···N5 | 0.85 | 2.10 | 2.925 (6) | 164 |
O2—H39···Br2ii | 0.85 | 2.60 | 3.388 (4) | 156 |
O2—H40···N6ii | 0.85 | 2.01 | 2.821 (5) | 160 |
O3—H41···O2i | 0.85 | 2.04 | 2.838 (5) | 156 |
O3—H42···Br1 | 0.85 | 2.62 | 3.406 (4) | 153 |
O4—H43···Br1 | 0.85 | 2.48 | 3.275 (4) | 155 |
O4—H44···Br2ii | 0.85 | 2.59 | 3.377 (4) | 155 |
O5—H45···Br2 | 0.85 | 2.53 | 3.362 (4) | 167 |
O5—H46···Br1ii | 0.85 | 2.57 | 3.290 (4) | 143 |
Symmetry codes: (i) −x+1, y−1/2, −z+1/2; (ii) −x+1, y+1/2, −z+1/2. |
Experimental details
Crystal data | |
Chemical formula | [Na2(C12H8N2)2(H2O)5]Br2·C12H8N2 |
Mr | 836.49 |
Crystal system, space group | Monoclinic, P21/c |
Temperature (K) | 298 |
a, b, c (Å) | 12.833 (5), 11.445 (5), 24.888 (10) |
β (°) | 93.696 (6) |
V (Å3) | 3648 (2) |
Z | 4 |
Radiation type | Mo Kα |
µ (mm−1) | 2.30 |
Crystal size (mm) | 0.66 × 0.32 × 0.10 |
Data collection | |
Diffractometer | CCD area-detector diffractometer |
Absorption correction | Multi-scan (SADABS; Sheldrick, 1996) |
Tmin, Tmax | 0.313, 0.803 |
No. of measured, independent and observed [I > 2σ(I)] reflections | 18042, 6336, 3007 |
Rint | 0.134 |
(sin θ/λ)max (Å−1) | 0.595 |
Refinement | |
R[F2 > 2σ(F2)], wR(F2), S | 0.052, 0.145, 0.85 |
No. of reflections | 6336 |
No. of parameters | 461 |
H-atom treatment | H-atom parameters constrained |
Δρmax, Δρmin (e Å−3) | 0.44, −0.45 |
Computer programs: SMART (Siemens, 1996), SAINT (Siemens, 1996), SHELXS97 (Sheldrick, 1997a), SHELXL97 (Sheldrick, 1997a), SHELXTL (Sheldrick, 1997b).
D—H···A | D—H | H···A | D···A | D—H···A |
O1—H37···N5 | 0.85 | 2.10 | 2.925 (6) | 164.4 |
O2—H39···Br2i | 0.85 | 2.60 | 3.388 (4) | 155.5 |
O2—H40···N6i | 0.85 | 2.01 | 2.821 (5) | 159.6 |
O3—H41···O2ii | 0.85 | 2.04 | 2.838 (5) | 155.5 |
O3—H42···Br1 | 0.85 | 2.62 | 3.406 (4) | 153.4 |
O4—H43···Br1 | 0.85 | 2.48 | 3.275 (4) | 155.4 |
O4—H44···Br2i | 0.85 | 2.59 | 3.377 (4) | 154.6 |
O5—H45···Br2 | 0.85 | 2.53 | 3.362 (4) | 166.9 |
O5—H46···Br1i | 0.85 | 2.57 | 3.290 (4) | 143.4 |
Symmetry codes: (i) −x+1, y+1/2, −z+1/2; (ii) −x+1, y−1/2, −z+1/2. |
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The structural chemistry of sodium complexes with 1,10-phenanthroline has been explored (Qian et al., 1994). In continuation of our study of sodium complexes with 1,10-phenanthroline, we present here the synthesis and crystal structure of the title compound, (I).
In the title compound (Fig. 1), [(Na2L2(H2O)5)2+.2Br-.L]n, (L=1,10-phenanthroline), the NaI ions in polymeric chains adopt two different coordinate fashions. The NaI ions adopt different coordinate fashions. In one fashion, the NaI ion is coordinated by two N atoms from L and four water molecules in a distorted octahedral geometry, while in another fashion, the NaI ion is coordinated by two N atoms from L and three water molecules in a distorted trigonal-bipyramidal geometry. The coordinating bond lengths Na—N [2.425 (5)–2.517 (5) Å] and Na—O [2.353 (5)–2.574 (4) Å] are normal. The crystal packing exhibits an extensive hydrogen-bonding network formed by O—H···N, O—H···O and O—H···Br hydrogen bonds (Table 1) and π···π interactions, proved by short distances of 3.605 (4) and 3.821 (4) between the centroids of central and outer rings of L from neighbouring molecules.