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The title binuclear manganese(II) complex, [Mn2(C2H3O2)2(C12H8N2)4](ClO4)2, has been synthesized by the reaction of manganese(II) acetate and tetra-n-butyl­ammonium manganate(VII) with 1,10-phenanthroline in a mixed solvent of acetic acid, ethanol and pyridine. In the centrosymmetric cation, the two MnII atoms are linked to each other by the four O atoms of two acetate ions. Each MnII atom adopts a six-coordinate geometry and the six coordinating atoms form a distorted octa­hedron.

Supporting information

cif

Crystallographic Information File (CIF) https://doi.org/10.1107/S1600536805027479/is6113sup1.cif
Contains datablocks I, global

hkl

Structure factor file (CIF format) https://doi.org/10.1107/S1600536805027479/is6113Isup2.hkl
Contains datablock I

CCDC reference: 268810

Key indicators

  • Single-crystal X-ray study
  • T = 293 K
  • Mean [sigma](C-C) = 0.005 Å
  • R factor = 0.044
  • wR factor = 0.132
  • Data-to-parameter ratio = 12.9

checkCIF/PLATON results

No syntax errors found




Alert level C HYDTR01_ALERT_1_C The hydrogen treatment should only be one of the following keywords * refall * refxyz * refU * noref * undef * constr * none * mixed Hydrogen treatment given as geom PLAT042_ALERT_1_C Calc. and Rep. MoietyFormula Strings Differ .... ? PLAT125_ALERT_4_C No _symmetry_space_group_name_Hall Given ....... ? PLAT199_ALERT_1_C Check the Reported _cell_measurement_temperature 293 K PLAT200_ALERT_1_C Check the Reported _diffrn_ambient_temperature . 293 K PLAT230_ALERT_2_C Hirshfeld Test Diff for C5 - C6 .. 5.04 su PLAT241_ALERT_2_C Check High Ueq as Compared to Neighbors for C21 PLAT242_ALERT_2_C Check Low Ueq as Compared to Neighbors for C25 PLAT244_ALERT_4_C Low 'Solvent' Ueq as Compared to Neighbors for Cl1
0 ALERT level A = In general: serious problem 0 ALERT level B = Potentially serious problem 9 ALERT level C = Check and explain 0 ALERT level G = General alerts; check 4 ALERT type 1 CIF construction/syntax error, inconsistent or missing data 3 ALERT type 2 Indicator that the structure model may be wrong or deficient 0 ALERT type 3 Indicator that the structure quality may be low 2 ALERT type 4 Improvement, methodology, query or suggestion

Comment top

The photosystem II oxygen-evolving complex (PSII OEC) found in the chloroplast thylakoid membranes of higher plants and algae catalyzes the splitting of water. The process is generally believed to occur on four or two manganese aggregates (Arulsamy et al., 1994). Owing to their relevance to the catalytic center of the photosystem, binuclear manganese complexes have become the subjects of intensive research. Some binuclear manganese complexes have been synthesized, such as two O atoms bridge (Tan et al., 1996; Goodwin et al., 2004), O atom and Ac (CH3COO) mixed bridge (Arulsamy et al., 1994; Oberhausen et al., 1993; Sheats et al., 1987; Wieghardt et al., 1985), isophthalate bridge (Tan et al., 1997) and two Ac anions bridge binuclear manganese complexes (Oshio et al., 1993; Ishida et al., 2001; Iriller et al., 2002). We report here the title binuclear manganese(II) complex [Mn2(µ-Ac)2(phen)4]·(ClO4)2 (phen = 1,10-phenanthroline), (I).

The molecular structure and the packing diagram of (I) in are shown in Figs. 1 and 2, respectively. The manganese complex is a centrosymmetric anion with an Mn···Mn separation of 4.588 (2) Å. The two MnII atoms are bridged by two Ac ligends. Four N atoms of two phen ligands and two O atoms from two Ac anions coordinate each MnII atom to form a distorted octahedron. Atoms N1, N2, O1 and N4 form the equatorial plane, the N2—Mn1—N1, N1—Mn1—O1, O1—Mn1—N4 and N4—Mn1—N2 bond angles being 72.62 (9), 162.44 (9), 102.61 (8) and 163.76 (9)°, respectively. Atoms N3 and O2 lie in the axial positions with an N3—Mn1—O2 angle of 166.39 (8)°.

Experimental top

Mn(Ac)2·4H2O (0.815 mmol) was dissolved in a mixed solvent (3 ml pyridine, 12 ml acetic acid, 20 ml EtOH); fresh (C4H9)4NMnO4 (0.315 mmol) was added slowly with continuous stirring and then NaClO4 (0.565 mmol) was added. After 1 h, solid phen (2.0 mmol) was added to the reaction solution with continuous stirring. The final mixture was filtered, and the filtrate was allowed to layer with ether. After three weeks, a red pole-shaped [yellow block?] crystal of (I) was obtained. M.p. >573 K. Analysis calculated for C52H38Cl2Mn2N8O12: C 54.37, H 3.31, N 9.76%; found: C 54.23, H 3.25, N 9.71%. Selected FT–IR (KBr, cm−1): υ 3072 (m), 3000 (s), 1625 (m), 1567 (s), 1516 (s), 1494 (m), 1094 (s), 865 (w), 848 (s), 770 (w), 728 (s).

Refinement top

The H atoms on the ligands were positioned geometrically and refined as riding [C—H = 0.93 Å and Uiso(H) = 1.2Ueq(C) for aromatic H atoms, and C—H = 0.96 Å and Uiso(H) = 1.5Ueq(C) for methyl H atoms]. Please check added text.

Computing details top

Data collection: SMART (Siemens, 1996); cell refinement: SAINT (Siemens, 1996); data reduction: SAINT; program(s) used to solve structure: SHELXS97 (Sheldrick, 1997); program(s) used to refine structure: SHELXL97 (Sheldrick, 1997); molecular graphics: SHELXTL (Bruker, 1997); software used to prepare material for publication: SHELXTL.

Figures top
[Figure 1] Fig. 1. The title complex, with the atomic numbering scheme and displacement ellipsoids at the 30% probability level. H atoms have been omitted for clarity.
[Figure 2] Fig. 2. The packing of the title complex viewed along the a axis. H atoms have been omitted.
di-µ-acetato-κ4O:O'-bis[bis(1,10-phenanthroline-κ2N,N')manganese(II)] bis(perchlorate) top
Crystal data top
[Mn2(C2H3O2)2(C12H8N2)4](ClO4)2Dx = 1.506 Mg m3
Mr = 1147.68Melting point > 300 K
Monoclinic, P21/cMo Kα radiation, λ = 0.71073 Å
a = 9.5474 (12) ÅCell parameters from 5713 reflections
b = 14.1858 (18) Åθ = 2.6–27.6°
c = 18.802 (2) ŵ = 0.68 mm1
β = 96.224 (2)°T = 293 K
V = 2531.5 (5) Å3Block, yellow
Z = 20.45 × 0.38 × 0.31 mm
F(000) = 1172
Data collection top
Siemens SMART CCD area-detector
diffractometer
4444 independent reflections
Radiation source: fine-focus sealed tube3681 reflections with I > 2σ(I)
Graphite monochromatorRint = 0.031
ϕ and ω scansθmax = 25.0°, θmin = 1.8°
Absorption correction: multi-scan
(SADABS; Sheldrick, 1996)
h = 1011
Tmin = 0.751, Tmax = 0.818k = 1613
12909 measured reflectionsl = 2222
Refinement top
Refinement on F2Primary atom site location: structure-invariant direct methods
Least-squares matrix: fullSecondary atom site location: difference Fourier map
R[F2 > 2σ(F2)] = 0.044Hydrogen site location: inferred from neighbouring sites
wR(F2) = 0.132H-atom parameters constrained
S = 1.01 w = 1/[σ2(Fo2) + (0.0794P)2 + 1.191P]
where P = (Fo2 + 2Fc2)/3
4444 reflections(Δ/σ)max < 0.001
344 parametersΔρmax = 0.64 e Å3
0 restraintsΔρmin = 0.33 e Å3
Crystal data top
[Mn2(C2H3O2)2(C12H8N2)4](ClO4)2V = 2531.5 (5) Å3
Mr = 1147.68Z = 2
Monoclinic, P21/cMo Kα radiation
a = 9.5474 (12) ŵ = 0.68 mm1
b = 14.1858 (18) ÅT = 293 K
c = 18.802 (2) Å0.45 × 0.38 × 0.31 mm
β = 96.224 (2)°
Data collection top
Siemens SMART CCD area-detector
diffractometer
4444 independent reflections
Absorption correction: multi-scan
(SADABS; Sheldrick, 1996)
3681 reflections with I > 2σ(I)
Tmin = 0.751, Tmax = 0.818Rint = 0.031
12909 measured reflections
Refinement top
R[F2 > 2σ(F2)] = 0.0440 restraints
wR(F2) = 0.132H-atom parameters constrained
S = 1.01Δρmax = 0.64 e Å3
4444 reflectionsΔρmin = 0.33 e Å3
344 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.

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.

Fractional atomic coordinates and isotropic or equivalent isotropic displacement parameters (Å2) top
xyzUiso*/Ueq
Mn10.48252 (4)0.15506 (3)0.032485 (19)0.04150 (16)
Cl10.03229 (9)0.37814 (6)0.17235 (5)0.0707 (3)
N10.3818 (3)0.29822 (16)0.00123 (12)0.0525 (6)
N20.6458 (3)0.24196 (16)0.01692 (12)0.0538 (6)
N30.5281 (2)0.21402 (15)0.14617 (11)0.0438 (5)
N40.3037 (3)0.10828 (17)0.09445 (12)0.0540 (6)
O10.6298 (2)0.04504 (13)0.05213 (10)0.0516 (5)
O20.3895 (2)0.10793 (13)0.06989 (9)0.0572 (5)
O30.0446 (4)0.3325 (3)0.1156 (2)0.1570 (17)
O40.1779 (3)0.35989 (19)0.17173 (15)0.0811 (7)
O50.0092 (4)0.3485 (3)0.2389 (2)0.1319 (14)
O60.0119 (4)0.4779 (2)0.1681 (2)0.1208 (11)
C10.2537 (4)0.3264 (2)0.01140 (19)0.0703 (9)
H10.20010.28920.03890.084*
C20.1952 (5)0.4109 (3)0.0179 (2)0.0918 (14)
H20.10450.42890.01000.110*
C30.2732 (6)0.4653 (3)0.0576 (2)0.0958 (15)
H30.23550.52120.07720.115*
C40.4084 (5)0.4390 (2)0.06941 (18)0.0786 (12)
C50.4606 (4)0.35334 (18)0.03781 (15)0.0570 (8)
C60.5988 (4)0.3231 (2)0.04834 (15)0.0547 (7)
C70.6839 (5)0.3771 (2)0.09080 (17)0.0759 (11)
C80.8167 (5)0.3440 (3)0.0992 (2)0.0936 (14)
H80.87460.37760.12690.112*
C90.8632 (4)0.2624 (4)0.0672 (2)0.0960 (13)
H90.95250.23930.07290.115*
C100.7755 (4)0.2142 (3)0.0261 (2)0.0720 (9)
H100.80920.15910.00350.086*
C110.4992 (7)0.4902 (3)0.1130 (2)0.0986 (17)
H110.46570.54570.13500.118*
C120.6265 (7)0.4619 (3)0.1227 (2)0.0975 (16)
H120.68040.49770.15090.117*
C130.6391 (3)0.2643 (2)0.17166 (15)0.0522 (7)
H130.71110.27370.14280.063*
C140.6526 (3)0.3038 (2)0.23998 (16)0.0602 (8)
H140.73260.33820.25620.072*
C150.5490 (3)0.2917 (2)0.28235 (15)0.0581 (8)
H150.55650.31880.32760.070*
C160.4295 (3)0.23786 (19)0.25805 (13)0.0476 (6)
C170.4250 (3)0.20005 (17)0.18895 (13)0.0410 (6)
C180.3074 (3)0.14250 (18)0.16192 (14)0.0454 (6)
C190.2001 (3)0.1237 (2)0.20575 (16)0.0563 (7)
C200.0901 (4)0.0656 (3)0.1780 (2)0.0811 (11)
H200.01880.04980.20570.097*
C210.0874 (4)0.0321 (3)0.1100 (2)0.0965 (14)
H210.01270.00510.09060.116*
C220.1962 (4)0.0539 (3)0.07023 (19)0.0801 (11)
H220.19400.02920.02430.096*
C230.3173 (3)0.2200 (2)0.29973 (14)0.0568 (7)
H230.31900.24720.34480.068*
C240.2096 (4)0.1650 (2)0.27562 (16)0.0630 (8)
H240.13890.15320.30480.076*
C250.6348 (3)0.02586 (18)0.09172 (13)0.0446 (6)
C260.6739 (4)0.0126 (2)0.17081 (16)0.0753 (10)
H26A0.59000.00270.19380.113*
H26B0.73460.04110.17870.113*
H26C0.72180.06780.19040.113*
Atomic displacement parameters (Å2) top
U11U22U33U12U13U23
Mn10.0545 (3)0.0347 (2)0.0354 (2)0.00482 (16)0.00554 (17)0.00263 (15)
Cl10.0550 (5)0.0691 (5)0.0876 (6)0.0028 (4)0.0054 (4)0.0115 (4)
N10.0657 (15)0.0389 (12)0.0498 (13)0.0029 (11)0.0076 (11)0.0070 (10)
N20.0643 (16)0.0470 (13)0.0497 (13)0.0127 (11)0.0045 (11)0.0060 (11)
N30.0512 (13)0.0391 (11)0.0405 (11)0.0021 (9)0.0023 (9)0.0014 (9)
N40.0601 (14)0.0561 (14)0.0467 (13)0.0170 (12)0.0095 (11)0.0075 (11)
O10.0663 (12)0.0409 (10)0.0479 (10)0.0019 (9)0.0079 (9)0.0083 (8)
O20.0910 (15)0.0383 (11)0.0386 (10)0.0012 (10)0.0096 (9)0.0019 (8)
O30.104 (3)0.202 (4)0.160 (4)0.051 (3)0.008 (2)0.056 (3)
O40.0597 (14)0.0900 (18)0.0942 (18)0.0091 (12)0.0109 (13)0.0184 (14)
O50.096 (2)0.165 (4)0.143 (3)0.015 (2)0.051 (2)0.057 (3)
O60.127 (3)0.082 (2)0.156 (3)0.0319 (18)0.026 (2)0.019 (2)
C10.074 (2)0.061 (2)0.071 (2)0.0090 (17)0.0110 (17)0.0186 (16)
C20.087 (3)0.073 (3)0.106 (3)0.029 (2)0.035 (2)0.031 (2)
C30.131 (4)0.049 (2)0.092 (3)0.016 (2)0.055 (3)0.011 (2)
C40.128 (3)0.0372 (16)0.0594 (19)0.0003 (19)0.040 (2)0.0032 (14)
C50.092 (2)0.0329 (14)0.0408 (14)0.0097 (14)0.0183 (14)0.0004 (11)
C60.079 (2)0.0409 (15)0.0418 (14)0.0196 (14)0.0043 (14)0.0009 (12)
C70.117 (3)0.059 (2)0.0482 (17)0.043 (2)0.0051 (19)0.0080 (15)
C80.101 (3)0.103 (3)0.080 (3)0.050 (3)0.023 (2)0.007 (2)
C90.074 (3)0.114 (4)0.102 (3)0.030 (2)0.023 (2)0.005 (3)
C100.062 (2)0.074 (2)0.081 (2)0.0114 (17)0.0158 (17)0.0067 (18)
C110.180 (5)0.0388 (19)0.066 (2)0.026 (3)0.040 (3)0.0239 (17)
C120.159 (5)0.065 (3)0.064 (2)0.046 (3)0.012 (3)0.0191 (19)
C130.0530 (16)0.0508 (16)0.0525 (16)0.0042 (13)0.0038 (13)0.0004 (13)
C140.0620 (19)0.0602 (19)0.0548 (17)0.0080 (15)0.0098 (14)0.0076 (15)
C150.071 (2)0.0590 (18)0.0408 (14)0.0046 (15)0.0075 (14)0.0056 (13)
C160.0613 (17)0.0445 (15)0.0356 (13)0.0111 (13)0.0013 (12)0.0038 (11)
C170.0500 (15)0.0354 (13)0.0369 (12)0.0040 (11)0.0016 (11)0.0054 (10)
C180.0557 (16)0.0427 (14)0.0387 (13)0.0000 (11)0.0085 (11)0.0051 (11)
C190.0629 (18)0.0588 (17)0.0487 (16)0.0061 (14)0.0132 (13)0.0070 (13)
C200.074 (2)0.100 (3)0.074 (2)0.033 (2)0.0283 (18)0.004 (2)
C210.089 (3)0.117 (3)0.088 (3)0.059 (3)0.028 (2)0.029 (2)
C220.086 (2)0.090 (3)0.067 (2)0.040 (2)0.0233 (18)0.0246 (19)
C230.074 (2)0.0631 (18)0.0338 (13)0.0098 (16)0.0059 (13)0.0042 (13)
C240.072 (2)0.075 (2)0.0445 (16)0.0077 (17)0.0201 (15)0.0118 (15)
C250.0535 (16)0.0412 (15)0.0380 (13)0.0013 (12)0.0001 (11)0.0028 (11)
C260.120 (3)0.0570 (19)0.0439 (16)0.0063 (19)0.0151 (17)0.0021 (14)
Geometric parameters (Å, º) top
Mn1—O12.1061 (19)C8—H80.9300
Mn1—O22.1376 (18)C9—C101.381 (5)
Mn1—N22.264 (2)C9—H90.9300
Mn1—N42.268 (2)C10—H100.9300
Mn1—N32.293 (2)C11—C121.312 (7)
Mn1—N12.296 (2)C11—H110.9300
Cl1—O31.388 (4)C12—H120.9300
Cl1—O41.416 (3)C13—C141.394 (4)
Cl1—O51.417 (3)C13—H130.9300
Cl1—O61.430 (3)C14—C151.346 (4)
N1—C11.320 (4)C14—H140.9300
N1—C51.355 (4)C15—C161.407 (4)
N2—C101.329 (4)C15—H150.9300
N2—C61.348 (4)C16—C171.402 (4)
N3—C131.324 (3)C16—C231.417 (4)
N3—C171.351 (3)C17—C181.436 (4)
N4—C221.325 (4)C18—C191.408 (4)
N4—C181.355 (3)C19—C201.391 (5)
O1—C251.249 (3)C19—C241.432 (4)
O2—C25i1.248 (3)C20—C211.361 (5)
C1—C21.409 (5)C20—H200.9300
C1—H10.9300C21—C221.379 (5)
C2—C31.352 (6)C21—H210.9300
C2—H20.9300C22—H220.9300
C3—C41.385 (7)C23—C241.330 (5)
C3—H30.9300C23—H230.9300
C4—C51.419 (4)C24—H240.9300
C4—C111.451 (7)C25—O2i1.248 (3)
C5—C61.422 (5)C25—C261.505 (4)
C6—C71.423 (5)C26—H26A0.9600
C7—C81.377 (6)C26—H26B0.9600
C7—C121.426 (6)C26—H26C0.9600
C8—C91.358 (6)
O1—Mn1—O297.49 (8)C7—C8—H8120.0
O1—Mn1—N289.96 (8)C8—C9—C10118.8 (4)
O2—Mn1—N292.18 (8)C8—C9—H9120.6
O1—Mn1—N4102.61 (8)C10—C9—H9120.6
O2—Mn1—N496.25 (8)N2—C10—C9123.8 (4)
N2—Mn1—N4163.76 (9)N2—C10—H10118.1
O1—Mn1—N392.94 (7)C9—C10—H10118.1
O2—Mn1—N3166.39 (8)C12—C11—C4123.0 (4)
N2—Mn1—N396.57 (8)C12—C11—H11118.5
N4—Mn1—N372.84 (8)C4—C11—H11118.5
O1—Mn1—N1162.44 (9)C11—C12—C7121.3 (4)
O2—Mn1—N185.68 (7)C11—C12—H12119.3
N2—Mn1—N172.62 (9)C7—C12—H12119.3
N4—Mn1—N194.16 (9)N3—C13—C14122.7 (3)
N3—Mn1—N187.00 (8)N3—C13—H13118.7
O3—Cl1—O4110.3 (2)C14—C13—H13118.7
O3—Cl1—O5111.4 (3)C15—C14—C13119.6 (3)
O4—Cl1—O5108.78 (19)C15—C14—H14120.2
O3—Cl1—O6111.2 (3)C13—C14—H14120.2
O4—Cl1—O6107.97 (19)C14—C15—C16119.9 (3)
O5—Cl1—O6107.1 (2)C14—C15—H15120.0
C1—N1—C5118.7 (3)C16—C15—H15120.0
C1—N1—Mn1126.9 (2)C17—C16—C15116.8 (3)
C5—N1—Mn1114.0 (2)C17—C16—C23119.7 (3)
C10—N2—C6117.8 (3)C15—C16—C23123.5 (3)
C10—N2—Mn1125.8 (2)N3—C17—C16123.0 (2)
C6—N2—Mn1115.7 (2)N3—C17—C18117.7 (2)
C13—N3—C17118.0 (2)C16—C17—C18119.3 (2)
C13—N3—Mn1126.70 (18)N4—C18—C19122.2 (3)
C17—N3—Mn1115.14 (16)N4—C18—C17118.3 (2)
C22—N4—C18118.1 (3)C19—C18—C17119.4 (2)
C22—N4—Mn1126.3 (2)C20—C19—C18117.4 (3)
C18—N4—Mn1115.58 (18)C20—C19—C24123.8 (3)
C25—O1—Mn1133.10 (18)C18—C19—C24118.8 (3)
C25i—O2—Mn1129.23 (16)C21—C20—C19119.8 (3)
N1—C1—C2122.4 (4)C21—C20—H20120.1
N1—C1—H1118.8C19—C20—H20120.1
C2—C1—H1118.8C20—C21—C22119.5 (3)
C3—C2—C1118.9 (4)C20—C21—H21120.3
C3—C2—H2120.6C22—C21—H21120.3
C1—C2—H2120.6N4—C22—C21123.0 (3)
C2—C3—C4120.8 (4)N4—C22—H22118.5
C2—C3—H3119.6C21—C22—H22118.5
C4—C3—H3119.6C24—C23—C16121.3 (3)
C3—C4—C5117.1 (4)C24—C23—H23119.4
C3—C4—C11125.4 (4)C16—C23—H23119.4
C5—C4—C11117.5 (4)C23—C24—C19121.5 (3)
N1—C5—C4122.0 (4)C23—C24—H24119.3
N1—C5—C6118.7 (2)C19—C24—H24119.3
C4—C5—C6119.3 (3)O2i—C25—O1124.1 (2)
N2—C6—C5117.8 (3)O2i—C25—C26117.3 (2)
N2—C6—C7121.5 (3)O1—C25—C26118.5 (2)
C5—C6—C7120.7 (3)C25—C26—H26A109.5
C8—C7—C6118.0 (4)C25—C26—H26B109.5
C8—C7—C12123.8 (4)H26A—C26—H26B109.5
C6—C7—C12118.2 (4)C25—C26—H26C109.5
C9—C8—C7120.1 (4)H26A—C26—H26C109.5
C9—C8—H8120.0H26B—C26—H26C109.5
Symmetry code: (i) x+1, y, z.

Experimental details

Crystal data
Chemical formula[Mn2(C2H3O2)2(C12H8N2)4](ClO4)2
Mr1147.68
Crystal system, space groupMonoclinic, P21/c
Temperature (K)293
a, b, c (Å)9.5474 (12), 14.1858 (18), 18.802 (2)
β (°) 96.224 (2)
V3)2531.5 (5)
Z2
Radiation typeMo Kα
µ (mm1)0.68
Crystal size (mm)0.45 × 0.38 × 0.31
Data collection
DiffractometerSiemens SMART CCD area-detector
diffractometer
Absorption correctionMulti-scan
(SADABS; Sheldrick, 1996)
Tmin, Tmax0.751, 0.818
No. of measured, independent and
observed [I > 2σ(I)] reflections
12909, 4444, 3681
Rint0.031
(sin θ/λ)max1)0.595
Refinement
R[F2 > 2σ(F2)], wR(F2), S 0.044, 0.132, 1.01
No. of reflections4444
No. of parameters344
H-atom treatmentH-atom parameters constrained
Δρmax, Δρmin (e Å3)0.64, 0.33

Computer programs: SMART (Siemens, 1996), SAINT (Siemens, 1996), SAINT, SHELXS97 (Sheldrick, 1997), SHELXL97 (Sheldrick, 1997), SHELXTL (Bruker, 1997), SHELXTL.

 

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