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In the title compound, C26H24, the central cyclo­octa­tetra­ene ring has a boat conformation, and the mol­ecule is saddle shaped. The seat is defined by the mean plane of the four-atom attachment points (r.m.s. deviation = 0.014 Å) of the two bicyclo­heptane substituents. These substituents comprise the pommel and cantle, with each mean plane defined by four atoms proximate to the seat (r.m.s. deviations = 0.001 and 0.000 Å). Relative to the seat, the pommel and cantle bend up 33.36 (5) and 34.22 (4)°, while the benzo units (flaps, r.m.s. deviations = 0.008 and 0.013 Å) bend down 33.48 (4) and 36.58 (4)°.

Supporting information

cif

Crystallographic Information File (CIF) https://doi.org/10.1107/S160053681104493X/mw2032sup1.cif
Contains datablocks global, I

hkl

Structure factor file (CIF format) https://doi.org/10.1107/S160053681104493X/mw2032Isup2.hkl
Contains datablock I

cdx

Chemdraw file https://doi.org/10.1107/S160053681104493X/mw2032Isup3.cdx
Supplementary material

CCDC reference: 858326

Key indicators

  • Single-crystal X-ray study
  • T = 90 K, P = 0.0 kPa
  • Mean [sigma](C-C) = 0.002 Å
  • R factor = 0.045
  • wR factor = 0.121
  • Data-to-parameter ratio = 21.3

checkCIF/PLATON results

No syntax errors found



Alert level B PLAT934_ALERT_3_B Number of (Iobs-Icalc)/SigmaW .gt. 10 Outliers . 1
Alert level C PLAT910_ALERT_3_C Missing # of FCF Reflections Below Th(Min) ..... 4 PLAT911_ALERT_3_C Missing # FCF Refl Between THmin & STh/L= 0.600 2 PLAT912_ALERT_4_C Missing # of FCF Reflections Above STh/L= 0.600 14 PLAT913_ALERT_3_C Missing # of Very Strong Reflections in FCF .... 1
Alert level G PLAT005_ALERT_5_G No _iucr_refine_instructions_details in CIF .... ? PLAT153_ALERT_1_G The su's on the Cell Axes are Equal .......... 0.00040 Ang. PLAT154_ALERT_1_G The su's on the Cell Angles are Equal .......... 0.00200 Deg. PLAT720_ALERT_4_G Number of Unusual/Non-Standard Labels .......... 13 PLAT793_ALERT_4_G The Model has Chirality at C17 (Verify) .... R PLAT793_ALERT_4_G The Model has Chirality at C19 (Verify) .... S PLAT793_ALERT_4_G The Model has Chirality at C22 (Verify) .... R PLAT793_ALERT_4_G The Model has Chirality at C24 (Verify) .... S
0 ALERT level A = Most likely a serious problem - resolve or explain 1 ALERT level B = A potentially serious problem, consider carefully 4 ALERT level C = Check. Ensure it is not caused by an omission or oversight 8 ALERT level G = General information/check it is not something unexpected 2 ALERT type 1 CIF construction/syntax error, inconsistent or missing data 0 ALERT type 2 Indicator that the structure model may be wrong or deficient 4 ALERT type 3 Indicator that the structure quality may be low 6 ALERT type 4 Improvement, methodology, query or suggestion 1 ALERT type 5 Informative message, check

Comment top

The central 8-ring of the title compound adopts the boat configuration, and the overall shape of the molecule is that of a saddle. Relative to the mean plane of the saddle seat (C07, C08, C15, C16, δr.m.s. = 0.014 Å), the two bicycloheptane moieties (mean planes C07, C08, C22, C24, δr.m.s. = 0.001 Å, and C15, C16, C17, C19, δr.m.s. = 0.000 Å) bend up 33.36 (5)° and 34.22 (4)°, while the mean planes of the benzo moieties (C01 – C06, δr.m.s. = 0.008. and C09 – C14, δr.m.s. = 0.013 Å) bend down 33.48 (4)° and 36.58 (4)°.

Related literature top

For related structures, see: Cambridge Structural Database(Allen, 2002) reference codes BUPDOF and BUPDUL (Durr et al., 1983) and RIBCAH (Sygula et al., 2007). For the synthesis of the title compound, see: Schaller (1994).

Experimental top

The preparation is described by Schaller (1994). Suitable crystals were obtained by recrystallization from benzene.

Refinement top

All H atoms were placed in calculated positions, guided by difference maps, with C—H bond distances 0.95 (aromatic C) and 0.99 (alkyl C) Å, and Uiso=1.2Ueq, thereafter refined as riding.

Structure description top

The central 8-ring of the title compound adopts the boat configuration, and the overall shape of the molecule is that of a saddle. Relative to the mean plane of the saddle seat (C07, C08, C15, C16, δr.m.s. = 0.014 Å), the two bicycloheptane moieties (mean planes C07, C08, C22, C24, δr.m.s. = 0.001 Å, and C15, C16, C17, C19, δr.m.s. = 0.000 Å) bend up 33.36 (5)° and 34.22 (4)°, while the mean planes of the benzo moieties (C01 – C06, δr.m.s. = 0.008. and C09 – C14, δr.m.s. = 0.013 Å) bend down 33.48 (4)° and 36.58 (4)°.

For related structures, see: Cambridge Structural Database(Allen, 2002) reference codes BUPDOF and BUPDUL (Durr et al., 1983) and RIBCAH (Sygula et al., 2007). For the synthesis of the title compound, see: Schaller (1994).

Computing details top

Data collection: COLLECT (Nonius, 2000); cell refinement: SCALEPACK (Otwinowski & Minor, 1997); data reduction: DENZO and SCALEPACK (Otwinowski & Minor, 1997); program(s) used to solve structure: SHELXS86 (Sheldrick, 2008); program(s) used to refine structure: SHELXL97 (Sheldrick, 2008); molecular graphics: ORTEP-3 for Windows (Farrugia, 1997); software used to prepare material for publication: WinGX (Farrugia, 1999).

Figures top
[Figure 1] Fig. 1. View of (I) (50% probability displacement ellipsoids)
Dibenzo[a,e]pentacyclo[12.2.1.16,9.02,13.05.10]octadeca- 2(13),5(10)-diene top
Crystal data top
C26H24Z = 2
Mr = 336.45F(000) = 360
Triclinic, P1Dx = 1.296 Mg m3
Hall symbol: -P 1Mo Kα radiation, λ = 0.71073 Å
a = 9.6962 (4) ÅCell parameters from 4596 reflections
b = 9.7754 (4) Åθ = 2.6–30.0°
c = 10.3676 (4) ŵ = 0.07 mm1
α = 77.896 (2)°T = 90 K
β = 63.781 (2)°Prism, colorless
γ = 85.497 (2)°0.48 × 0.48 × 0.22 mm
V = 861.87 (6) Å3
Data collection top
Nonius KappaCCD
diffractometer
5019 independent reflections
Radiation source: sealed tube4347 reflections with I > 2σ(I)
Horizonally mounted graphite crystal monochromatorRint = 0.024
Detector resolution: 9 pixels mm-1θmax = 30.0°, θmin = 2.8°
CCD rotation images, thick slices scansh = 1313
Absorption correction: multi-scan
(SCALEPACK; Otwinowski & Minor, 1997)
k = 1313
Tmin = 0.966, Tmax = 0.984l = 1414
8966 measured reflections
Refinement top
Refinement on F2Secondary atom site location: difference Fourier map
Least-squares matrix: fullHydrogen site location: inferred from neighbouring sites
R[F2 > 2σ(F2)] = 0.045H-atom parameters constrained
wR(F2) = 0.121 w = 1/[σ2(Fo2) + (0.0535P)2 + 0.4358P]
where P = (Fo2 + 2Fc2)/3
S = 1.05(Δ/σ)max = 0.001
5019 reflectionsΔρmax = 0.41 e Å3
236 parametersΔρmin = 0.25 e Å3
0 restraintsExtinction correction: SHELXL97 (Sheldrick, 2008), Fc*=kFc[1+0.001xFc2λ3/sin(2θ)]-1/4
0 constraintsExtinction coefficient: 0.015 (4)
Primary atom site location: structure-invariant direct methods
Crystal data top
C26H24γ = 85.497 (2)°
Mr = 336.45V = 861.87 (6) Å3
Triclinic, P1Z = 2
a = 9.6962 (4) ÅMo Kα radiation
b = 9.7754 (4) ŵ = 0.07 mm1
c = 10.3676 (4) ÅT = 90 K
α = 77.896 (2)°0.48 × 0.48 × 0.22 mm
β = 63.781 (2)°
Data collection top
Nonius KappaCCD
diffractometer
5019 independent reflections
Absorption correction: multi-scan
(SCALEPACK; Otwinowski & Minor, 1997)
4347 reflections with I > 2σ(I)
Tmin = 0.966, Tmax = 0.984Rint = 0.024
8966 measured reflections
Refinement top
R[F2 > 2σ(F2)] = 0.0450 restraints
wR(F2) = 0.121H-atom parameters constrained
S = 1.05Δρmax = 0.41 e Å3
5019 reflectionsΔρmin = 0.25 e Å3
236 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*/Ueq
C010.28621 (12)0.39958 (11)0.15111 (11)0.0134 (2)
C020.25832 (13)0.47525 (12)0.26849 (12)0.0164 (2)
H020.29060.43770.35460.020*
C030.18494 (13)0.60324 (12)0.26193 (13)0.0182 (2)
H030.16480.65090.34150.022*
C040.14123 (13)0.66103 (11)0.13797 (13)0.0172 (2)
H040.09170.74890.13250.021*
C050.17053 (12)0.58930 (11)0.02231 (12)0.0153 (2)
H050.14240.63020.06110.018*
C060.24068 (12)0.45787 (11)0.02517 (11)0.01283 (19)
C070.27322 (12)0.39265 (11)0.10023 (11)0.01297 (19)
C080.24073 (12)0.26227 (11)0.18361 (11)0.01301 (19)
C090.16507 (12)0.14103 (11)0.17577 (11)0.0130 (2)
C100.04120 (12)0.07520 (11)0.30452 (12)0.0153 (2)
H100.00770.11170.39140.018*
C110.03322 (13)0.04209 (12)0.30719 (13)0.0175 (2)
H110.11940.08240.39400.021*
C120.01873 (14)0.10005 (12)0.18273 (13)0.0187 (2)
H120.03110.18050.18400.022*
C130.14420 (13)0.03930 (11)0.05642 (12)0.0169 (2)
H130.18190.08140.02730.020*
C140.21718 (12)0.08297 (11)0.04893 (12)0.0137 (2)
C150.35046 (12)0.14034 (11)0.08965 (12)0.0137 (2)
C160.37693 (12)0.27080 (11)0.17235 (11)0.0134 (2)
C170.51686 (12)0.26307 (11)0.31741 (12)0.0151 (2)
H170.57250.35380.37430.018*
C180.61003 (13)0.15005 (12)0.26337 (13)0.0171 (2)
H18A0.69670.11500.34430.021*
H18B0.64650.18030.19820.021*
C190.47281 (12)0.04601 (11)0.17980 (12)0.0155 (2)
H190.49170.04320.12260.019*
C200.43547 (14)0.03038 (12)0.30813 (13)0.0179 (2)
H20A0.50390.03800.36450.021*
H20B0.32710.00060.27110.021*
C210.46571 (14)0.18041 (12)0.40311 (12)0.0183 (2)
H21A0.37130.21990.40960.022*
H21B0.54790.18110.50330.022*
C220.27239 (12)0.26323 (11)0.31521 (12)0.0142 (2)
H220.28990.16950.36630.017*
C230.40970 (12)0.36642 (12)0.24377 (12)0.0158 (2)
H23A0.50240.33090.16870.019*
H23B0.43500.39680.31620.019*
C240.32682 (12)0.47954 (11)0.17707 (12)0.0146 (2)
H240.38920.56550.11380.018*
C250.18178 (13)0.50237 (12)0.31881 (12)0.0170 (2)
H25A0.20460.56840.36760.020*
H25B0.09490.53820.29620.020*
C260.14585 (13)0.35287 (12)0.41540 (12)0.0163 (2)
H26A0.04160.32060.43910.020*
H26B0.15450.34950.50770.020*
Atomic displacement parameters (Å2) top
U11U22U33U12U13U23
C010.0133 (4)0.0118 (4)0.0146 (5)0.0001 (3)0.0060 (4)0.0017 (4)
C020.0187 (5)0.0156 (5)0.0160 (5)0.0007 (4)0.0090 (4)0.0022 (4)
C030.0195 (5)0.0166 (5)0.0198 (5)0.0010 (4)0.0116 (4)0.0003 (4)
C040.0165 (5)0.0129 (5)0.0225 (5)0.0023 (4)0.0099 (4)0.0017 (4)
C050.0150 (5)0.0124 (5)0.0177 (5)0.0012 (4)0.0065 (4)0.0030 (4)
C060.0122 (4)0.0114 (4)0.0141 (4)0.0002 (3)0.0055 (4)0.0014 (3)
C070.0125 (4)0.0125 (5)0.0136 (4)0.0016 (3)0.0053 (4)0.0034 (4)
C080.0126 (4)0.0134 (5)0.0129 (4)0.0017 (3)0.0054 (4)0.0028 (4)
C090.0140 (4)0.0112 (4)0.0145 (5)0.0016 (3)0.0076 (4)0.0009 (3)
C100.0165 (5)0.0141 (5)0.0151 (5)0.0005 (4)0.0075 (4)0.0008 (4)
C110.0174 (5)0.0149 (5)0.0183 (5)0.0020 (4)0.0077 (4)0.0016 (4)
C120.0212 (5)0.0137 (5)0.0222 (5)0.0026 (4)0.0111 (4)0.0006 (4)
C130.0204 (5)0.0136 (5)0.0182 (5)0.0005 (4)0.0098 (4)0.0033 (4)
C140.0151 (4)0.0117 (4)0.0153 (5)0.0017 (3)0.0080 (4)0.0019 (4)
C150.0145 (4)0.0134 (5)0.0147 (5)0.0020 (4)0.0073 (4)0.0046 (4)
C160.0138 (4)0.0142 (5)0.0138 (4)0.0018 (4)0.0068 (4)0.0043 (4)
C170.0150 (5)0.0157 (5)0.0141 (5)0.0016 (4)0.0055 (4)0.0043 (4)
C180.0144 (5)0.0185 (5)0.0191 (5)0.0034 (4)0.0071 (4)0.0063 (4)
C190.0169 (5)0.0138 (5)0.0170 (5)0.0033 (4)0.0081 (4)0.0049 (4)
C200.0207 (5)0.0164 (5)0.0191 (5)0.0028 (4)0.0096 (4)0.0076 (4)
C210.0221 (5)0.0189 (5)0.0157 (5)0.0018 (4)0.0089 (4)0.0057 (4)
C220.0146 (4)0.0142 (5)0.0136 (4)0.0006 (4)0.0063 (4)0.0024 (4)
C230.0149 (5)0.0174 (5)0.0159 (5)0.0007 (4)0.0074 (4)0.0027 (4)
C240.0156 (5)0.0136 (5)0.0148 (5)0.0002 (4)0.0067 (4)0.0029 (4)
C250.0191 (5)0.0154 (5)0.0169 (5)0.0019 (4)0.0075 (4)0.0057 (4)
C260.0173 (5)0.0169 (5)0.0139 (5)0.0005 (4)0.0058 (4)0.0038 (4)
Geometric parameters (Å, º) top
C01—C021.4082 (14)C15—C191.5301 (15)
C01—C061.4099 (15)C16—C171.5287 (15)
C01—C161.4758 (14)C17—C181.5433 (15)
C02—C031.3891 (15)C17—C211.5626 (15)
C02—H020.9500C17—H171.0000
C03—C041.3914 (16)C18—C191.5426 (16)
C03—H030.9500C18—H18A0.9900
C04—C051.3883 (15)C18—H18B0.9900
C04—H040.9500C19—C201.5634 (15)
C05—C061.4054 (14)C19—H191.0000
C05—H050.9500C20—C211.5534 (16)
C06—C071.4763 (14)C20—H20A0.9900
C07—C081.3532 (14)C20—H20B0.9900
C07—C241.5314 (15)C21—H21A0.9900
C08—C091.4762 (14)C21—H21B0.9900
C08—C221.5270 (15)C22—C231.5378 (15)
C09—C101.4082 (15)C22—C261.5617 (15)
C09—C141.4098 (15)C22—H221.0000
C10—C111.3910 (15)C23—C241.5420 (15)
C10—H100.9500C23—H23A0.9900
C11—C121.3883 (17)C23—H23B0.9900
C11—H110.9500C24—C251.5650 (15)
C12—C131.3882 (16)C24—H241.0000
C12—H120.9500C25—C261.5550 (15)
C13—C141.4073 (15)C25—H25A0.9900
C13—H130.9500C25—H25B0.9900
C14—C151.4779 (15)C26—H26A0.9900
C15—C161.3512 (15)C26—H26B0.9900
C02—C01—C06118.50 (10)C19—C18—C1793.53 (8)
C02—C01—C16118.22 (9)C19—C18—H18A113.0
C06—C01—C16122.92 (9)C17—C18—H18A113.0
C03—C02—C01121.88 (10)C19—C18—H18B113.0
C03—C02—H02119.1C17—C18—H18B113.0
C01—C02—H02119.1H18A—C18—H18B110.4
C02—C03—C04119.48 (10)C15—C19—C18100.09 (8)
C02—C03—H03120.3C15—C19—C20107.17 (9)
C04—C03—H03120.3C18—C19—C20100.24 (9)
C05—C04—C03119.47 (10)C15—C19—H19115.7
C05—C04—H04120.3C18—C19—H19115.7
C03—C04—H04120.3C20—C19—H19115.7
C04—C05—C06121.88 (10)C21—C20—C19102.90 (9)
C04—C05—H05119.1C21—C20—H20A111.2
C06—C05—H05119.1C19—C20—H20A111.2
C05—C06—C01118.76 (10)C21—C20—H20B111.2
C05—C06—C07117.87 (9)C19—C20—H20B111.2
C01—C06—C07123.22 (9)H20A—C20—H20B109.1
C08—C07—C06130.51 (10)C20—C21—C17102.78 (9)
C08—C07—C24106.88 (9)C20—C21—H21A111.2
C06—C07—C24121.69 (9)C17—C21—H21A111.2
C07—C08—C09131.06 (10)C20—C21—H21B111.2
C07—C08—C22107.00 (9)C17—C21—H21B111.2
C09—C08—C22121.23 (9)H21A—C21—H21B109.1
C10—C09—C14118.74 (10)C08—C22—C23100.36 (8)
C10—C09—C08117.94 (9)C08—C22—C26107.65 (8)
C14—C09—C08123.18 (9)C23—C22—C26100.28 (9)
C11—C10—C09121.42 (10)C08—C22—H22115.5
C11—C10—H10119.3C23—C22—H22115.5
C09—C10—H10119.3C26—C22—H22115.5
C12—C11—C10119.87 (10)C22—C23—C2493.57 (8)
C12—C11—H11120.1C22—C23—H23A113.0
C10—C11—H11120.1C24—C23—H23A113.0
C13—C12—C11119.37 (10)C22—C23—H23B113.0
C13—C12—H12120.3C24—C23—H23B113.0
C11—C12—H12120.3H23A—C23—H23B110.4
C12—C13—C14121.84 (10)C07—C24—C23100.19 (8)
C12—C13—H13119.1C07—C24—C25106.63 (8)
C14—C13—H13119.1C23—C24—C25100.53 (8)
C13—C14—C09118.66 (10)C07—C24—H24115.8
C13—C14—C15118.30 (10)C23—C24—H24115.8
C09—C14—C15122.96 (9)C25—C24—H24115.8
C16—C15—C14129.94 (10)C26—C25—C24102.79 (8)
C16—C15—C19107.15 (9)C26—C25—H25A111.2
C14—C15—C19122.01 (9)C24—C25—H25A111.2
C15—C16—C01131.40 (10)C26—C25—H25B111.2
C15—C16—C17106.96 (9)C24—C25—H25B111.2
C01—C16—C17121.07 (9)H25A—C25—H25B109.1
C16—C17—C18100.22 (8)C25—C26—C22102.68 (8)
C16—C17—C21107.22 (9)C25—C26—H26A111.2
C18—C17—C21100.36 (9)C22—C26—H26A111.2
C16—C17—H17115.6C25—C26—H26B111.2
C18—C17—H17115.6C22—C26—H26B111.2
C21—C17—H17115.6H26A—C26—H26B109.1
C06—C01—C02—C031.34 (16)C14—C15—C16—C17169.06 (10)
C16—C01—C02—C03174.67 (10)C19—C15—C16—C170.00 (11)
C01—C02—C03—C041.86 (17)C02—C01—C16—C15130.46 (12)
C02—C03—C04—C050.52 (17)C06—C01—C16—C1556.53 (17)
C03—C04—C05—C061.31 (16)C02—C01—C16—C1739.74 (14)
C04—C05—C06—C011.81 (16)C06—C01—C16—C17133.27 (11)
C04—C05—C06—C07177.38 (10)C15—C16—C17—C1833.99 (11)
C02—C01—C06—C050.48 (15)C01—C16—C17—C18153.68 (9)
C16—C01—C06—C05172.52 (10)C15—C16—C17—C2170.33 (11)
C02—C01—C06—C07175.80 (10)C01—C16—C17—C21102.00 (11)
C16—C01—C06—C072.80 (16)C16—C17—C18—C1951.33 (9)
C05—C06—C07—C08130.07 (12)C21—C17—C18—C1958.47 (9)
C01—C06—C07—C0854.57 (16)C16—C15—C19—C1833.99 (11)
C05—C06—C07—C2437.51 (14)C14—C15—C19—C18155.89 (9)
C01—C06—C07—C24137.85 (10)C16—C15—C19—C2070.13 (11)
C06—C07—C08—C091.38 (19)C14—C15—C19—C2099.99 (11)
C24—C07—C08—C09170.36 (10)C17—C18—C19—C1551.23 (9)
C06—C07—C08—C22168.83 (10)C17—C18—C19—C2058.45 (9)
C24—C07—C08—C220.14 (11)C15—C19—C20—C2167.15 (10)
C07—C08—C09—C10128.15 (12)C18—C19—C20—C2136.87 (10)
C22—C08—C09—C1040.89 (14)C19—C20—C21—C170.10 (11)
C07—C08—C09—C1456.15 (16)C16—C17—C21—C2067.52 (10)
C22—C08—C09—C14134.80 (10)C18—C17—C21—C2036.70 (10)
C14—C09—C10—C112.22 (15)C07—C08—C22—C2334.13 (10)
C08—C09—C10—C11178.12 (10)C09—C08—C22—C23154.49 (9)
C09—C10—C11—C122.77 (17)C07—C08—C22—C2670.26 (10)
C10—C11—C12—C130.42 (17)C09—C08—C22—C26101.12 (11)
C11—C12—C13—C142.45 (17)C08—C22—C23—C2451.37 (9)
C12—C13—C14—C092.95 (16)C26—C22—C23—C2458.90 (9)
C12—C13—C14—C15179.75 (10)C08—C07—C24—C2333.77 (10)
C10—C09—C14—C130.60 (15)C06—C07—C24—C23156.07 (9)
C08—C09—C14—C13175.07 (10)C08—C07—C24—C2570.56 (10)
C10—C09—C14—C15177.24 (10)C06—C07—C24—C2599.60 (11)
C08—C09—C14—C151.58 (15)C22—C23—C24—C0751.19 (9)
C13—C14—C15—C16127.20 (12)C22—C23—C24—C2558.03 (9)
C09—C14—C15—C1656.14 (16)C07—C24—C25—C2668.46 (10)
C13—C14—C15—C1940.45 (14)C23—C24—C25—C2635.62 (10)
C09—C14—C15—C19136.20 (11)C24—C25—C26—C221.28 (10)
C14—C15—C16—C012.17 (19)C08—C22—C26—C2566.56 (10)
C19—C15—C16—C01171.23 (11)C23—C22—C26—C2537.88 (10)

Experimental details

Crystal data
Chemical formulaC26H24
Mr336.45
Crystal system, space groupTriclinic, P1
Temperature (K)90
a, b, c (Å)9.6962 (4), 9.7754 (4), 10.3676 (4)
α, β, γ (°)77.896 (2), 63.781 (2), 85.497 (2)
V3)861.87 (6)
Z2
Radiation typeMo Kα
µ (mm1)0.07
Crystal size (mm)0.48 × 0.48 × 0.22
Data collection
DiffractometerNonius KappaCCD
Absorption correctionMulti-scan
(SCALEPACK; Otwinowski & Minor, 1997)
Tmin, Tmax0.966, 0.984
No. of measured, independent and
observed [I > 2σ(I)] reflections
8966, 5019, 4347
Rint0.024
(sin θ/λ)max1)0.704
Refinement
R[F2 > 2σ(F2)], wR(F2), S 0.045, 0.121, 1.05
No. of reflections5019
No. of parameters236
H-atom treatmentH-atom parameters constrained
Δρmax, Δρmin (e Å3)0.41, 0.25

Computer programs: COLLECT (Nonius, 2000), DENZO and SCALEPACK (Otwinowski & Minor, 1997), SHELXS86 (Sheldrick, 2008), SHELXL97 (Sheldrick, 2008), ORTEP-3 for Windows (Farrugia, 1997), WinGX (Farrugia, 1999).

 

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