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Low-energy contamination caused by focusing multilayer optics has been known for a long time. So far, the only method to avoid this problem is attenuation by interposition of a low-density material foil into the beam. However, attenuation lowers the intensity, which might be crucial, especially for charge density data collection, and is of course not possible for already measured data. In this article, an empirical correction is proposed as an alternative or addition. The low-energy contamination mainly affects the reflections with indices 3h 3k 3l. In the program SADABS, a 3λ correction in analogy to the earlier 2/λ correction is now implemented. The correction factor can be determined from the model, but for most cases, a default value depending on the experimental settings is acceptable. Alternatively, the correction can be refined in SHELXL, similarly to a twin refinement. An investigation of several data sets collected with and without attenuation revealed that the empirical correction and attenuation lead to similar improvements. The empirical correction is of special interest for charge density investigations, where the loss of intensity could hinder the data collection up to very high resolution. Here, the improvements in the model, especially for the noise level of the residual density, are even more pronounced.

Supporting information

cif

Crystallographic Information File (CIF) https://doi.org/10.1107/S1600576715020440/ks5494sup1.cif
Contains datablocks global, 1_corr, 1_filter, 1_uncorr, 2_corr, 2_filter, 2_uncorr, 3_corr, 3_filter, 3_uncorr, 4_corr, 4_filter, 4_uncorr, 5_corr, 5_filter, 5_uncorr, spanh_3lcorr, spanh_3lnocorr

hkl

Structure factor file (CIF format) https://doi.org/10.1107/S1600576715020440/ks54941_corrsup2.hkl
Contains datablock 1_corr

hkl

Structure factor file (CIF format) https://doi.org/10.1107/S1600576715020440/ks54941_filtersup3.hkl
Contains datablock 1_filter

hkl

Structure factor file (CIF format) https://doi.org/10.1107/S1600576715020440/ks54941_uncorrsup4.hkl
Contains datablock 1_uncorr

hkl

Structure factor file (CIF format) https://doi.org/10.1107/S1600576715020440/ks54942_corrsup5.hkl
Contains datablock 2_corr

hkl

Structure factor file (CIF format) https://doi.org/10.1107/S1600576715020440/ks54942_filtersup6.hkl
Contains datablock 2_filter

hkl

Structure factor file (CIF format) https://doi.org/10.1107/S1600576715020440/ks54942_uncorrsup7.hkl
Contains datablock 2_uncorr

hkl

Structure factor file (CIF format) https://doi.org/10.1107/S1600576715020440/ks54943_corrsup8.hkl
Contains datablock 3_corr

hkl

Structure factor file (CIF format) https://doi.org/10.1107/S1600576715020440/ks54943_filtersup9.hkl
Contains datablock 3_filter

hkl

Structure factor file (CIF format) https://doi.org/10.1107/S1600576715020440/ks54943_uncorrsup10.hkl
Contains datablock 3_uncorr

hkl

Structure factor file (CIF format) https://doi.org/10.1107/S1600576715020440/ks54944_corrsup11.hkl
Contains datablock 4_corr

hkl

Structure factor file (CIF format) https://doi.org/10.1107/S1600576715020440/ks54944_filtersup12.hkl
Contains datablock 4_filter

hkl

Structure factor file (CIF format) https://doi.org/10.1107/S1600576715020440/ks54944_uncorrsup13.hkl
Contains datablock 4_uncorr

hkl

Structure factor file (CIF format) https://doi.org/10.1107/S1600576715020440/ks54945_corrsup14.hkl
Contains datablock 5_corr

hkl

Structure factor file (CIF format) https://doi.org/10.1107/S1600576715020440/ks54945_filtersup15.hkl
Contains datablock 5_filter

hkl

Structure factor file (CIF format) https://doi.org/10.1107/S1600576715020440/ks54945_uncorrsup16.hkl
Contains datablock 5_uncorr

hkl

Structure factor file (CIF format) https://doi.org/10.1107/S1600576715020440/ks5494spanh_3lnocorrsup18.hkl
Contains datablock SPANH_3lnocorr

hkl

Structure factor file (CIF format) https://doi.org/10.1107/S1600576715020440/ks5494spanh_3lcorrsup17.hkl
Contains datablock SPANH_3lcorr

pdf

Portable Document Format (PDF) file https://doi.org/10.1107/S1600576715020440/ks5494sup19.pdf
Supporting information file

CCDC references: 1433805; 1433806; 1433807; 1433808; 1433809; 1433810; 1433811; 1433812; 1433813; 1433814; 1433815; 1433816; 1433817; 1433818; 1433819; 1433820; 1433821

Computing details top

Data collection: APEX2 v2012.2 for 1_corr, 1_filter, 1_uncorr, 2_corr, 2_filter, 2_uncorr, 3_corr, 3_filter, 3_uncorr, 4_corr, 4_filter, 4_uncorr, 5_corr, 5_filter, 5_uncorr. Cell refinement: SAINT V8.30C for 1_corr, 1_filter, 1_uncorr, 2_corr, 2_filter, 2_uncorr, 3_corr, 3_filter, 3_uncorr, 5_corr, 5_filter, 5_uncorr; SAINT V8.34A for 4_corr, 4_filter, 4_uncorr. Data reduction: SAINT V8.30C for 1_corr, 1_filter, 1_uncorr, 2_corr, 2_filter, 2_uncorr, 3_corr, 3_filter, 3_uncorr, 5_corr, 5_filter, 5_uncorr; SAINT V8.34A for 4_corr, 4_filter, 4_uncorr. Program(s) used to solve structure: SHELXT (G.M.Sheldrick,Acta Cryst.(2015)A71,3-8) for 1_corr, 1_filter, 1_uncorr, 2_corr, 2_filter, 2_uncorr, 3_corr, 3_filter, 3_uncorr, 4_corr, 4_filter, 4_uncorr, 5_corr, 5_filter, 5_uncorr. Program(s) used to refine structure: SHELXL2014/7 (Sheldrick, 2014) for 1_corr, 1_filter, 1_uncorr, 2_corr, 2_filter, 2_uncorr, 3_corr, 3_filter, 3_uncorr, 4_corr, 4_filter, 4_uncorr, 5_corr, 5_filter, 5_uncorr; Volkov et al., (2006) for spanh_3lcorr, spanh_3lnocorr. Molecular graphics: Mercury CSD 3.3 (Build RC5) for 1_corr, 1_filter, 1_uncorr, 2_corr, 2_filter, 2_uncorr, 3_corr, 3_filter, 3_uncorr, 4_corr, 4_filter, 4_uncorr, 5_corr, 5_filter, 5_uncorr; Volkov et al., (2006) for spanh_3lcorr, spanh_3lnocorr. Software used to prepare material for publication: Mercury CSD 3.3 (Build RC5) for 1_corr, 1_filter, 1_uncorr, 2_corr, 2_filter, 2_uncorr, 3_corr, 3_filter, 3_uncorr, 4_corr, 4_filter, 4_uncorr, 5_corr, 5_filter, 5_uncorr; Volkov et al., (2006) for spanh_3lcorr, spanh_3lnocorr.

(1_corr) top
Crystal data top
C28H18N2F(000) = 800
Mr = 382.44Dx = 1.383 Mg m3
Monoclinic, C2/cMo Kα radiation, λ = 0.71073 Å
a = 13.5559 (13) ÅCell parameters from 7097 reflections
b = 12.2134 (12) Åθ = 2.4–25.5°
c = 12.6643 (12) ŵ = 0.08 mm1
β = 118.8339 (17)°T = 100 K
V = 1836.8 (3) Å3Block
Z = 40.32 × 0.25 × 0.10 mm
Data collection top
Bruker Smart APEX II Quazar
diffractometer
1697 independent reflections
Radiation source: INCOATEC Microsource1530 reflections with I > 2σ(I)
ω scansθmax = 25.5°, θmin = 2.4°
Absorption correction: multi-scan
SADABS2015/1
h = 1614
Tmin = 0.709, Tmax = 0.745k = 014
1697 measured reflectionsl = 015
Refinement top
Refinement on F2123 restraints
Least-squares matrix: fullHydrogen site location: inferred from neighbouring sites
R[F2 > 2σ(F2)] = 0.040H-atom parameters constrained
wR(F2) = 0.111 w = 1/[σ2(Fo2) + (0.0483P)2 + 1.9011P]
where P = (Fo2 + 2Fc2)/3
S = 1.09(Δ/σ)max < 0.001
1697 reflectionsΔρmax = 0.27 e Å3
137 parametersΔρmin = 0.18 e Å3
Crystal data top
C28H18N2V = 1836.8 (3) Å3
Mr = 382.44Z = 4
Monoclinic, C2/cMo Kα radiation
a = 13.5559 (13) ŵ = 0.08 mm1
b = 12.2134 (12) ÅT = 100 K
c = 12.6643 (12) Å0.32 × 0.25 × 0.10 mm
β = 118.8339 (17)°
Data collection top
Bruker Smart APEX II Quazar
diffractometer
1697 measured reflections
Absorption correction: multi-scan
SADABS2015/1
1697 independent reflections
Tmin = 0.709, Tmax = 0.7451530 reflections with I > 2σ(I)
Refinement top
R[F2 > 2σ(F2)] = 0.040123 restraints
wR(F2) = 0.111H-atom parameters constrained
S = 1.09Δρmax = 0.27 e Å3
1697 reflectionsΔρmin = 0.18 e Å3
137 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. Refined as a 2-component twin.

Fractional atomic coordinates and isotropic or equivalent isotropic displacement parameters (Å2) top
xyzUiso*/Ueq
N10.89762 (10)0.62822 (10)0.48827 (10)0.0234 (3)
C10.83923 (12)0.55154 (11)0.51140 (12)0.0222 (3)
C20.90131 (13)0.46550 (12)0.59283 (13)0.0266 (3)
H20.98120.46550.63050.032*
C40.72737 (13)0.38271 (12)0.56227 (13)0.0294 (4)
H40.69050.32550.58050.035*
C30.84716 (13)0.38365 (12)0.61693 (13)0.0298 (4)
H30.88950.32650.67070.036*
C50.66564 (12)0.46320 (12)0.48433 (13)0.0258 (3)
H50.58590.46150.44850.031*
C60.71872 (12)0.55042 (11)0.45539 (12)0.0220 (3)
C70.65798 (12)0.63304 (11)0.37060 (12)0.0214 (3)
C80.71820 (12)0.71355 (11)0.34557 (12)0.0219 (3)
C90.66656 (12)0.80336 (12)0.26418 (13)0.0245 (3)
H90.58700.81090.22430.029*
C100.72952 (13)0.87772 (12)0.24322 (13)0.0272 (3)
H100.69370.93670.18920.033*
C110.84938 (13)0.86773 (12)0.30207 (13)0.0274 (3)
H110.89250.91880.28480.033*
C120.90181 (12)0.78648 (12)0.38182 (13)0.0260 (3)
H120.98170.78220.42170.031*
C130.83917 (12)0.70670 (11)0.40729 (12)0.0218 (3)
C140.53291 (12)0.63329 (11)0.30970 (13)0.0237 (3)
H140.49760.63350.35880.028*
Atomic displacement parameters (Å2) top
U11U22U33U12U13U23
N10.0229 (6)0.0253 (6)0.0207 (6)0.0002 (5)0.0094 (5)0.0019 (5)
C10.0252 (7)0.0230 (7)0.0175 (7)0.0001 (6)0.0096 (6)0.0037 (5)
C20.0262 (7)0.0295 (8)0.0215 (7)0.0041 (6)0.0094 (6)0.0005 (6)
C40.0376 (9)0.0248 (8)0.0268 (8)0.0043 (6)0.0162 (7)0.0005 (6)
C30.0362 (8)0.0266 (8)0.0230 (7)0.0060 (6)0.0114 (7)0.0042 (6)
C50.0258 (7)0.0268 (7)0.0233 (7)0.0029 (6)0.0107 (6)0.0023 (6)
C60.0263 (7)0.0217 (7)0.0185 (7)0.0001 (5)0.0113 (6)0.0035 (5)
C70.0231 (7)0.0221 (7)0.0179 (7)0.0001 (6)0.0090 (6)0.0032 (5)
C80.0254 (7)0.0222 (7)0.0176 (6)0.0003 (6)0.0100 (6)0.0033 (5)
C90.0247 (7)0.0246 (7)0.0221 (7)0.0011 (6)0.0096 (6)0.0008 (6)
C100.0335 (8)0.0241 (8)0.0234 (7)0.0006 (6)0.0133 (6)0.0031 (6)
C110.0309 (8)0.0269 (8)0.0281 (8)0.0062 (6)0.0171 (6)0.0017 (6)
C120.0237 (7)0.0286 (8)0.0264 (7)0.0043 (6)0.0127 (6)0.0046 (6)
C130.0248 (7)0.0216 (7)0.0190 (7)0.0001 (5)0.0105 (6)0.0045 (5)
C140.0229 (7)0.0225 (7)0.0254 (7)0.0000 (6)0.0113 (6)0.0004 (6)
Geometric parameters (Å, º) top
N1—C11.3465 (19)C7—C141.486 (2)
N1—C131.3470 (18)C8—C91.435 (2)
C1—C21.428 (2)C8—C131.439 (2)
C1—C61.433 (2)C9—C101.357 (2)
C2—C31.359 (2)C9—H90.9500
C2—H20.9500C10—C111.429 (2)
C4—C51.358 (2)C10—H100.9500
C4—C31.425 (2)C11—C121.348 (2)
C4—H40.9500C11—H110.9500
C3—H30.9500C12—C131.428 (2)
C5—C61.429 (2)C12—H120.9500
C5—H50.9500C14—C14i1.335 (3)
C6—C71.413 (2)C14—H140.9500
C7—C81.408 (2)
C1—N1—C13117.96 (12)C7—C8—C9124.08 (13)
N1—C1—C2117.74 (13)C7—C8—C13118.01 (13)
N1—C1—C6123.25 (13)C9—C8—C13117.90 (13)
C2—C1—C6118.97 (13)C10—C9—C8121.13 (13)
C3—C2—C1120.63 (14)C10—C9—H9119.4
C3—C2—H2119.7C8—C9—H9119.4
C1—C2—H2119.7C9—C10—C11120.32 (14)
C5—C4—C3120.36 (14)C9—C10—H10119.8
C5—C4—H4119.8C11—C10—H10119.8
C3—C4—H4119.8C12—C11—C10120.63 (14)
C2—C3—C4120.59 (14)C12—C11—H11119.7
C2—C3—H3119.7C10—C11—H11119.7
C4—C3—H3119.7C11—C12—C13121.03 (14)
C4—C5—C6121.08 (14)C11—C12—H12119.5
C4—C5—H5119.5C13—C12—H12119.5
C6—C5—H5119.5N1—C13—C12117.52 (13)
C7—C6—C5123.13 (13)N1—C13—C8123.55 (13)
C7—C6—C1118.46 (13)C12—C13—C8118.93 (13)
C5—C6—C1118.36 (13)C14i—C14—C7124.05 (17)
C8—C7—C6118.76 (13)C14i—C14—H14118.0
C8—C7—C14121.46 (12)C7—C14—H14118.0
C6—C7—C14119.78 (12)
Symmetry code: (i) x+1, y, z+1/2.
(1_filter) top
Crystal data top
C28H18N2F(000) = 800
Mr = 382.44Dx = 1.384 Mg m3
Monoclinic, C2/cMo Kα radiation, λ = 0.71073 Å
a = 13.5537 (16) ÅCell parameters from 7384 reflections
b = 12.2132 (15) Åθ = 2.4–25.5°
c = 12.6619 (15) ŵ = 0.08 mm1
β = 118.836 (2)°T = 100 K
V = 1836.1 (4) Å3Block
Z = 40.32 × 0.25 × 0.10 mm
Data collection top
Bruker Smart APEX II Quazar
diffractometer
1549 reflections with I > 2σ(I)
Radiation source: INCOATEC MicrosourceRint = 0.026
ω scansθmax = 25.6°, θmin = 2.4°
Absorption correction: multi-scan
SADABS2015/1
h = 1616
Tmin = 0.706, Tmax = 0.745k = 1414
14259 measured reflectionsl = 1515
1707 independent reflections
Refinement top
Refinement on F2123 restraints
Least-squares matrix: fullHydrogen site location: inferred from neighbouring sites
R[F2 > 2σ(F2)] = 0.039H-atom parameters constrained
wR(F2) = 0.111 w = 1/[σ2(Fo2) + (0.0515P)2 + 1.5638P]
where P = (Fo2 + 2Fc2)/3
S = 1.10(Δ/σ)max < 0.001
1707 reflectionsΔρmax = 0.27 e Å3
136 parametersΔρmin = 0.19 e Å3
Crystal data top
C28H18N2V = 1836.1 (4) Å3
Mr = 382.44Z = 4
Monoclinic, C2/cMo Kα radiation
a = 13.5537 (16) ŵ = 0.08 mm1
b = 12.2132 (15) ÅT = 100 K
c = 12.6619 (15) Å0.32 × 0.25 × 0.10 mm
β = 118.836 (2)°
Data collection top
Bruker Smart APEX II Quazar
diffractometer
1707 independent reflections
Absorption correction: multi-scan
SADABS2015/1
1549 reflections with I > 2σ(I)
Tmin = 0.706, Tmax = 0.745Rint = 0.026
14259 measured reflections
Refinement top
R[F2 > 2σ(F2)] = 0.039123 restraints
wR(F2) = 0.111H-atom parameters constrained
S = 1.10Δρmax = 0.27 e Å3
1707 reflectionsΔρmin = 0.19 e Å3
136 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
N10.89769 (9)0.62822 (9)0.48827 (10)0.0233 (3)
C10.83933 (11)0.55148 (11)0.51141 (11)0.0219 (3)
C20.90133 (12)0.46548 (11)0.59291 (12)0.0267 (3)
H20.98130.46540.63070.032*
C40.72732 (13)0.38276 (11)0.56223 (12)0.0291 (3)
H40.69040.32550.58040.035*
C30.84708 (12)0.38361 (12)0.61691 (12)0.0297 (3)
H30.88940.32650.67060.036*
C50.66557 (12)0.46325 (11)0.48434 (12)0.0258 (3)
H50.58580.46150.44860.031*
C60.71858 (11)0.55046 (11)0.45529 (11)0.0217 (3)
C70.65796 (11)0.63307 (10)0.37061 (11)0.0214 (3)
C80.71815 (11)0.71360 (10)0.34543 (11)0.0215 (3)
C90.66659 (11)0.80344 (11)0.26419 (12)0.0243 (3)
H90.58700.81100.22440.029*
C100.72948 (12)0.87779 (11)0.24314 (12)0.0271 (3)
H100.69360.93670.18900.033*
C110.84939 (12)0.86781 (11)0.30200 (12)0.0272 (3)
H110.89250.91900.28480.033*
C120.90194 (12)0.78632 (11)0.38186 (12)0.0261 (3)
H120.98180.78200.42170.031*
C130.83922 (11)0.70664 (10)0.40729 (11)0.0217 (3)
C140.53290 (11)0.63330 (10)0.30971 (12)0.0233 (3)
H140.49760.63350.35880.028*
Atomic displacement parameters (Å2) top
U11U22U33U12U13U23
N10.0230 (6)0.0251 (6)0.0206 (6)0.0002 (4)0.0095 (5)0.0020 (4)
C10.0247 (7)0.0231 (7)0.0170 (6)0.0003 (5)0.0092 (5)0.0038 (5)
C20.0266 (7)0.0293 (7)0.0213 (6)0.0041 (6)0.0093 (6)0.0000 (5)
C40.0372 (8)0.0242 (7)0.0268 (7)0.0042 (6)0.0160 (6)0.0007 (6)
C30.0354 (8)0.0262 (7)0.0234 (7)0.0059 (6)0.0110 (6)0.0043 (6)
C50.0252 (7)0.0266 (7)0.0236 (7)0.0029 (5)0.0102 (6)0.0024 (5)
C60.0254 (7)0.0216 (7)0.0184 (6)0.0000 (5)0.0108 (5)0.0032 (5)
C70.0230 (7)0.0225 (7)0.0173 (6)0.0000 (5)0.0087 (5)0.0033 (5)
C80.0237 (7)0.0223 (7)0.0176 (6)0.0003 (5)0.0093 (5)0.0033 (5)
C90.0247 (7)0.0247 (7)0.0216 (6)0.0011 (5)0.0095 (5)0.0007 (5)
C100.0330 (8)0.0241 (7)0.0234 (7)0.0009 (6)0.0129 (6)0.0030 (5)
C110.0303 (7)0.0269 (7)0.0278 (7)0.0063 (6)0.0168 (6)0.0018 (6)
C120.0239 (7)0.0294 (7)0.0257 (7)0.0043 (5)0.0125 (6)0.0047 (5)
C130.0248 (7)0.0217 (6)0.0186 (6)0.0000 (5)0.0104 (5)0.0042 (5)
C140.0228 (7)0.0218 (7)0.0251 (6)0.0001 (5)0.0114 (5)0.0004 (5)
Geometric parameters (Å, º) top
N1—C131.3464 (17)C7—C141.4855 (18)
N1—C11.3467 (17)C8—C91.4343 (19)
C1—C21.4275 (19)C8—C131.4400 (18)
C1—C61.4359 (18)C9—C101.3569 (19)
C2—C31.359 (2)C9—H90.9500
C2—H20.9500C10—C111.430 (2)
C4—C51.358 (2)C10—H100.9500
C4—C31.425 (2)C11—C121.351 (2)
C4—H40.9500C11—H110.9500
C3—H30.9500C12—C131.4273 (19)
C5—C61.4286 (19)C12—H120.9500
C5—H50.9500C14—C14i1.334 (3)
C6—C71.4117 (18)C14—H140.9500
C7—C81.4090 (18)
C13—N1—C1117.97 (11)C7—C8—C9124.14 (12)
N1—C1—C2117.81 (12)C7—C8—C13117.91 (12)
N1—C1—C6123.18 (12)C9—C8—C13117.94 (12)
C2—C1—C6118.98 (12)C10—C9—C8121.19 (13)
C3—C2—C1120.63 (13)C10—C9—H9119.4
C3—C2—H2119.7C8—C9—H9119.4
C1—C2—H2119.7C9—C10—C11120.30 (13)
C5—C4—C3120.42 (13)C9—C10—H10119.9
C5—C4—H4119.8C11—C10—H10119.9
C3—C4—H4119.8C12—C11—C10120.62 (13)
C2—C3—C4120.59 (13)C12—C11—H11119.7
C2—C3—H3119.7C10—C11—H11119.7
C4—C3—H3119.7C11—C12—C13120.98 (13)
C4—C5—C6121.10 (13)C11—C12—H12119.5
C4—C5—H5119.4C13—C12—H12119.5
C6—C5—H5119.4N1—C13—C12117.45 (12)
C7—C6—C5123.21 (12)N1—C13—C8123.64 (12)
C7—C6—C1118.46 (12)C12—C13—C8118.91 (12)
C5—C6—C1118.28 (12)C14i—C14—C7124.05 (16)
C8—C7—C6118.84 (12)C14i—C14—H14118.0
C8—C7—C14121.43 (11)C7—C14—H14118.0
C6—C7—C14119.74 (12)
Symmetry code: (i) x+1, y, z+1/2.
(1_uncorr) top
Crystal data top
C28H18N2F(000) = 800
Mr = 382.44Dx = 1.383 Mg m3
Monoclinic, C2/cMo Kα radiation, λ = 0.71073 Å
a = 13.5559 (13) ÅCell parameters from 7097 reflections
b = 12.2134 (12) Åθ = 2.4–25.5°
c = 12.6643 (12) ŵ = 0.08 mm1
β = 118.8339 (17)°T = 100 K
V = 1836.8 (3) Å3Block
Z = 40.32 × 0.25 × 0.10 mm
Data collection top
Bruker Smart APEX II Quazar
diffractometer
1547 reflections with I > 2σ(I)
Radiation source: INCOATEC MicrosourceRint = 0.025
ω scansθmax = 25.5°, θmin = 2.4°
Absorption correction: multi-scan
SADABS2015/1
h = 1616
Tmin = 0.709, Tmax = 0.745k = 1414
14302 measured reflectionsl = 1515
1697 independent reflections
Refinement top
Refinement on F2123 restraints
Least-squares matrix: fullHydrogen site location: inferred from neighbouring sites
R[F2 > 2σ(F2)] = 0.043H-atom parameters constrained
wR(F2) = 0.127 w = 1/[σ2(Fo2) + (0.0538P)2 + 2.3981P]
where P = (Fo2 + 2Fc2)/3
S = 1.12(Δ/σ)max < 0.001
1697 reflectionsΔρmax = 0.24 e Å3
136 parametersΔρmin = 0.20 e Å3
Crystal data top
C28H18N2V = 1836.8 (3) Å3
Mr = 382.44Z = 4
Monoclinic, C2/cMo Kα radiation
a = 13.5559 (13) ŵ = 0.08 mm1
b = 12.2134 (12) ÅT = 100 K
c = 12.6643 (12) Å0.32 × 0.25 × 0.10 mm
β = 118.8339 (17)°
Data collection top
Bruker Smart APEX II Quazar
diffractometer
1697 independent reflections
Absorption correction: multi-scan
SADABS2015/1
1547 reflections with I > 2σ(I)
Tmin = 0.709, Tmax = 0.745Rint = 0.025
14302 measured reflections
Refinement top
R[F2 > 2σ(F2)] = 0.043123 restraints
wR(F2) = 0.127H-atom parameters constrained
S = 1.12Δρmax = 0.24 e Å3
1697 reflectionsΔρmin = 0.20 e Å3
136 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
N10.89762 (11)0.62827 (11)0.48822 (12)0.0234 (3)
C10.83927 (13)0.55158 (13)0.51147 (13)0.0223 (4)
C20.90123 (14)0.46544 (14)0.59281 (14)0.0266 (4)
H20.98110.46540.63050.032*
C40.72735 (15)0.38273 (14)0.56217 (15)0.0294 (4)
H40.69050.32550.58030.035*
C30.84713 (15)0.38358 (14)0.61687 (15)0.0298 (4)
H30.88950.32640.67060.036*
C50.66569 (14)0.46312 (14)0.48435 (14)0.0258 (4)
H50.58590.46140.44850.031*
C60.71866 (13)0.55038 (13)0.45544 (13)0.0219 (4)
C70.65794 (13)0.63308 (13)0.37064 (13)0.0214 (4)
C80.71819 (13)0.71357 (13)0.34545 (14)0.0220 (4)
C90.66659 (14)0.80336 (13)0.26419 (14)0.0244 (4)
H90.58700.81090.22430.029*
C100.72955 (15)0.87777 (13)0.24332 (15)0.0274 (4)
H100.69380.93680.18940.033*
C110.84941 (15)0.86770 (14)0.30202 (15)0.0274 (4)
H110.89250.91870.28470.033*
C120.90182 (14)0.78644 (14)0.38179 (15)0.0259 (4)
H120.98170.78220.42170.031*
C130.83915 (13)0.70666 (13)0.40729 (14)0.0218 (4)
C140.53296 (13)0.63330 (13)0.30967 (14)0.0236 (4)
H140.49770.63350.35880.028*
Atomic displacement parameters (Å2) top
U11U22U33U12U13U23
N10.0228 (7)0.0256 (7)0.0207 (7)0.0001 (5)0.0094 (6)0.0019 (5)
C10.0254 (8)0.0232 (8)0.0174 (7)0.0002 (6)0.0095 (6)0.0041 (6)
C20.0264 (8)0.0294 (9)0.0213 (8)0.0039 (7)0.0094 (7)0.0002 (7)
C40.0377 (10)0.0247 (9)0.0266 (9)0.0043 (7)0.0160 (8)0.0004 (7)
C30.0360 (10)0.0266 (9)0.0230 (8)0.0057 (7)0.0113 (7)0.0040 (7)
C50.0254 (8)0.0269 (8)0.0234 (8)0.0026 (7)0.0103 (7)0.0025 (7)
C60.0262 (8)0.0219 (8)0.0185 (7)0.0002 (6)0.0114 (6)0.0037 (6)
C70.0233 (8)0.0223 (8)0.0176 (7)0.0003 (6)0.0091 (6)0.0030 (6)
C80.0254 (8)0.0225 (8)0.0176 (7)0.0000 (6)0.0100 (6)0.0029 (6)
C90.0245 (8)0.0245 (8)0.0222 (8)0.0011 (6)0.0097 (7)0.0007 (6)
C100.0340 (9)0.0240 (8)0.0238 (8)0.0007 (7)0.0137 (7)0.0029 (6)
C110.0310 (9)0.0272 (9)0.0277 (8)0.0062 (7)0.0172 (7)0.0016 (7)
C120.0236 (8)0.0287 (9)0.0259 (8)0.0042 (7)0.0123 (7)0.0046 (7)
C130.0247 (8)0.0216 (8)0.0191 (7)0.0001 (6)0.0106 (6)0.0044 (6)
C140.0231 (8)0.0226 (8)0.0251 (8)0.0003 (6)0.0115 (7)0.0004 (6)
Geometric parameters (Å, º) top
N1—C131.346 (2)C7—C141.485 (2)
N1—C11.347 (2)C8—C91.434 (2)
C1—C21.428 (2)C8—C131.439 (2)
C1—C61.435 (2)C9—C101.357 (2)
C2—C31.359 (2)C9—H90.9500
C2—H20.9500C10—C111.429 (2)
C4—C51.356 (2)C10—H100.9500
C4—C31.425 (3)C11—C121.348 (2)
C4—H40.9500C11—H110.9500
C3—H30.9500C12—C131.428 (2)
C5—C61.428 (2)C12—H120.9500
C5—H50.9500C14—C14i1.334 (3)
C6—C71.414 (2)C14—H140.9500
C7—C81.410 (2)
C13—N1—C1117.96 (14)C7—C8—C9124.08 (15)
N1—C1—C2117.83 (15)C7—C8—C13117.94 (14)
N1—C1—C6123.25 (14)C9—C8—C13117.96 (14)
C2—C1—C6118.87 (15)C10—C9—C8121.12 (15)
C3—C2—C1120.70 (15)C10—C9—H9119.4
C3—C2—H2119.6C8—C9—H9119.4
C1—C2—H2119.6C9—C10—C11120.34 (15)
C5—C4—C3120.41 (16)C9—C10—H10119.8
C5—C4—H4119.8C11—C10—H10119.8
C3—C4—H4119.8C12—C11—C10120.60 (15)
C2—C3—C4120.53 (15)C12—C11—H11119.7
C2—C3—H3119.7C10—C11—H11119.7
C4—C3—H3119.7C11—C12—C13121.04 (15)
C4—C5—C6121.12 (16)C11—C12—H12119.5
C4—C5—H5119.4C13—C12—H12119.5
C6—C5—H5119.4N1—C13—C12117.47 (14)
C7—C6—C5123.19 (15)N1—C13—C8123.65 (14)
C7—C6—C1118.40 (14)C12—C13—C8118.87 (14)
C5—C6—C1118.35 (15)C14i—C14—C7124.20 (19)
C8—C7—C6118.79 (14)C14i—C14—H14117.9
C8—C7—C14121.43 (14)C7—C14—H14117.9
C6—C7—C14119.78 (14)
Symmetry code: (i) x+1, y, z+1/2.
(2_corr) top
Crystal data top
C12H4N4F(000) = 416
Mr = 204.19Dx = 1.356 Mg m3
Monoclinic, C2/cMo Kα radiation, λ = 0.71073 Å
a = 8.896 (2) ÅCell parameters from 6323 reflections
b = 6.9130 (19) Åθ = 2.5–30.7°
c = 16.439 (5) ŵ = 0.09 mm1
β = 98.290 (3)°T = 100 K
V = 1000.5 (5) Å3Plate
Z = 40.18 × 0.13 × 0.06 mm
Data collection top
Bruker Smart APEX II Quazar
diffractometer
1543 independent reflections
Radiation source: INCOATEC Microsource1442 reflections with I > 2σ(I)
ω scansθmax = 30.7°, θmin = 2.5°
Absorption correction: multi-scan
SADABS2015/1
h = 1212
Tmin = 0.718, Tmax = 0.746k = 09
1543 measured reflectionsl = 023
Refinement top
Refinement on F20 restraints
Least-squares matrix: fullHydrogen site location: inferred from neighbouring sites
R[F2 > 2σ(F2)] = 0.034H-atom parameters constrained
wR(F2) = 0.096 w = 1/[σ2(Fo2) + (0.0517P)2 + 0.5563P]
where P = (Fo2 + 2Fc2)/3
S = 1.09(Δ/σ)max < 0.001
1543 reflectionsΔρmax = 0.46 e Å3
74 parametersΔρmin = 0.17 e Å3
Crystal data top
C12H4N4V = 1000.5 (5) Å3
Mr = 204.19Z = 4
Monoclinic, C2/cMo Kα radiation
a = 8.896 (2) ŵ = 0.09 mm1
b = 6.9130 (19) ÅT = 100 K
c = 16.439 (5) Å0.18 × 0.13 × 0.06 mm
β = 98.290 (3)°
Data collection top
Bruker Smart APEX II Quazar
diffractometer
1543 measured reflections
Absorption correction: multi-scan
SADABS2015/1
1543 independent reflections
Tmin = 0.718, Tmax = 0.7461442 reflections with I > 2σ(I)
Refinement top
R[F2 > 2σ(F2)] = 0.0340 restraints
wR(F2) = 0.096H-atom parameters constrained
S = 1.09Δρmax = 0.46 e Å3
1543 reflectionsΔρmin = 0.17 e Å3
74 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. Refined as a 2-component twin.

Fractional atomic coordinates and isotropic or equivalent isotropic displacement parameters (Å2) top
xyzUiso*/Ueq
N10.30688 (9)0.75618 (12)0.23989 (4)0.02159 (18)
C10.65124 (8)0.52594 (11)0.48397 (4)0.01337 (16)
H10.75320.54220.47430.016*
N20.02032 (8)0.56592 (12)0.40011 (5)0.02133 (18)
C20.53550 (8)0.57996 (11)0.42556 (4)0.01349 (16)
H20.55720.63380.37540.016*
C40.26081 (8)0.61022 (11)0.37927 (5)0.01357 (16)
C30.37907 (8)0.55637 (10)0.43887 (4)0.01240 (16)
C60.10475 (9)0.58526 (11)0.39042 (5)0.01540 (16)
C50.28657 (9)0.69138 (11)0.30188 (5)0.01578 (17)
Atomic displacement parameters (Å2) top
U11U22U33U12U13U23
N10.0225 (4)0.0240 (4)0.0184 (3)0.0010 (3)0.0030 (3)0.0031 (3)
C10.0128 (3)0.0143 (3)0.0137 (3)0.0011 (2)0.0040 (2)0.0005 (2)
N20.0165 (3)0.0264 (4)0.0211 (3)0.0001 (3)0.0029 (2)0.0000 (3)
C20.0133 (3)0.0145 (3)0.0133 (3)0.0012 (2)0.0041 (2)0.0004 (2)
C40.0135 (3)0.0139 (3)0.0135 (3)0.0006 (2)0.0025 (2)0.0008 (2)
C30.0127 (3)0.0121 (3)0.0128 (3)0.0005 (2)0.0031 (2)0.0011 (2)
C60.0156 (3)0.0162 (3)0.0141 (3)0.0003 (3)0.0010 (2)0.0003 (2)
C50.0146 (3)0.0166 (3)0.0158 (3)0.0004 (3)0.0010 (2)0.0006 (3)
Geometric parameters (Å, º) top
N1—C51.1509 (11)C2—H20.9500
C1—C21.3552 (11)C4—C31.3813 (11)
C1—C3i1.4504 (11)C4—C61.4368 (11)
C1—H10.9500C4—C51.4388 (11)
N2—C61.1543 (11)C3—C1i1.4505 (11)
C2—C31.4489 (11)
C2—C1—C3i120.64 (7)C3—C4—C5122.02 (7)
C2—C1—H1119.7C6—C4—C5116.09 (7)
C3i—C1—H1119.7C4—C3—C2120.83 (7)
C1—C2—C3120.67 (7)C4—C3—C1i120.49 (7)
C1—C2—H2119.7C2—C3—C1i118.68 (6)
C3—C2—H2119.7N2—C6—C4179.36 (8)
C3—C4—C6121.89 (7)N1—C5—C4179.86 (10)
Symmetry code: (i) x+1, y+1, z+1.
(2_filter) top
Crystal data top
C12H4N4F(000) = 416
Mr = 204.19Dx = 1.361 Mg m3
Monoclinic, C2/cMo Kα radiation, λ = 0.71073 Å
a = 8.8840 (12) ÅCell parameters from 6067 reflections
b = 6.9036 (9) Åθ = 2.5–30.7°
c = 16.421 (2) ŵ = 0.09 mm1
β = 98.241 (2)°T = 100 K
V = 996.7 (2) Å3Plate
Z = 40.18 × 0.13 × 0.06 mm
Data collection top
Bruker Smart APEX II Quazar
diffractometer
1432 reflections with I > 2σ(I)
Radiation source: INCOATEC MicrosourceRint = 0.016
ω scansθmax = 30.7°, θmin = 2.5°
Absorption correction: multi-scan
SADABS2015/1
h = 1212
Tmin = 0.718, Tmax = 0.746k = 99
10375 measured reflectionsl = 2323
1545 independent reflections
Refinement top
Refinement on F20 restraints
Least-squares matrix: fullHydrogen site location: inferred from neighbouring sites
R[F2 > 2σ(F2)] = 0.034H-atom parameters constrained
wR(F2) = 0.099 w = 1/[σ2(Fo2) + (0.0567P)2 + 0.4831P]
where P = (Fo2 + 2Fc2)/3
S = 1.08(Δ/σ)max < 0.001
1545 reflectionsΔρmax = 0.47 e Å3
73 parametersΔρmin = 0.19 e Å3
Crystal data top
C12H4N4V = 996.7 (2) Å3
Mr = 204.19Z = 4
Monoclinic, C2/cMo Kα radiation
a = 8.8840 (12) ŵ = 0.09 mm1
b = 6.9036 (9) ÅT = 100 K
c = 16.421 (2) Å0.18 × 0.13 × 0.06 mm
β = 98.241 (2)°
Data collection top
Bruker Smart APEX II Quazar
diffractometer
1545 independent reflections
Absorption correction: multi-scan
SADABS2015/1
1432 reflections with I > 2σ(I)
Tmin = 0.718, Tmax = 0.746Rint = 0.016
10375 measured reflections
Refinement top
R[F2 > 2σ(F2)] = 0.0340 restraints
wR(F2) = 0.099H-atom parameters constrained
S = 1.08Δρmax = 0.47 e Å3
1545 reflectionsΔρmin = 0.19 e Å3
73 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
N10.30687 (8)0.24383 (11)0.23988 (4)0.02160 (18)
C10.65123 (8)0.47404 (11)0.48395 (4)0.01331 (16)
H10.75330.45780.47420.016*
N20.02033 (8)0.43413 (11)0.40011 (5)0.02135 (18)
C20.53546 (8)0.42002 (11)0.42555 (4)0.01347 (16)
H20.55720.36610.37530.016*
C40.26078 (8)0.38973 (11)0.37923 (4)0.01353 (16)
C30.37905 (8)0.44364 (10)0.43889 (4)0.01239 (16)
C60.10468 (9)0.41472 (11)0.39038 (5)0.01544 (17)
C50.28653 (8)0.30871 (11)0.30187 (5)0.01573 (17)
Atomic displacement parameters (Å2) top
U11U22U33U12U13U23
N10.0224 (4)0.0239 (4)0.0185 (3)0.0009 (3)0.0029 (3)0.0033 (3)
C10.0128 (3)0.0141 (3)0.0137 (3)0.0011 (2)0.0041 (2)0.0005 (2)
N20.0163 (3)0.0267 (4)0.0212 (3)0.0002 (3)0.0029 (2)0.0001 (3)
C20.0134 (3)0.0144 (3)0.0133 (3)0.0011 (2)0.0042 (2)0.0005 (2)
C40.0135 (3)0.0137 (3)0.0136 (3)0.0006 (2)0.0026 (2)0.0008 (2)
C30.0128 (3)0.0120 (3)0.0127 (3)0.0006 (2)0.0030 (2)0.0011 (2)
C60.0155 (3)0.0161 (3)0.0144 (3)0.0003 (2)0.0013 (2)0.0004 (2)
C50.0147 (3)0.0164 (3)0.0158 (3)0.0006 (3)0.0011 (2)0.0003 (3)
Geometric parameters (Å, º) top
N1—C51.1499 (11)C2—H20.9500
C1—C21.3541 (10)C4—C31.3809 (10)
C1—C3i1.4486 (10)C4—C61.4350 (10)
C1—H10.9500C4—C51.4360 (10)
N2—C61.1522 (11)C3—C1i1.4486 (10)
C2—C31.4466 (10)
C2—C1—C3i120.67 (6)C3—C4—C5122.07 (7)
C2—C1—H1119.7C6—C4—C5116.04 (6)
C3i—C1—H1119.7C4—C3—C2120.79 (7)
C1—C2—C3120.68 (6)C4—C3—C1i120.56 (7)
C1—C2—H2119.7C2—C3—C1i118.65 (6)
C3—C2—H2119.7N2—C6—C4179.33 (8)
C3—C4—C6121.87 (7)N1—C5—C4179.88 (9)
Symmetry code: (i) x+1, y+1, z+1.
(2_uncorr) top
Crystal data top
C12H4N4F(000) = 416
Mr = 204.19Dx = 1.356 Mg m3
Monoclinic, C2/cMo Kα radiation, λ = 0.71073 Å
a = 8.896 (2) ÅCell parameters from 6323 reflections
b = 6.9130 (19) Åθ = 2.5–30.7°
c = 16.439 (5) ŵ = 0.09 mm1
β = 98.290 (3)°T = 100 K
V = 1000.5 (5) Å3Plate
Z = 40.18 × 0.13 × 0.06 mm
Data collection top
Bruker Smart APEX II Quazar
diffractometer
1447 reflections with I > 2σ(I)
Radiation source: INCOATEC MicrosourceRint = 0.015
ω scansθmax = 30.7°, θmin = 2.5°
Absorption correction: multi-scan
SADABS2015/1
h = 1212
Tmin = 0.718, Tmax = 0.746k = 99
10353 measured reflectionsl = 2323
1543 independent reflections
Refinement top
Refinement on F20 restraints
Least-squares matrix: fullHydrogen site location: inferred from neighbouring sites
R[F2 > 2σ(F2)] = 0.036H-atom parameters constrained
wR(F2) = 0.108 w = 1/[σ2(Fo2) + (0.0523P)2 + 0.8725P]
where P = (Fo2 + 2Fc2)/3
S = 1.09(Δ/σ)max < 0.001
1543 reflectionsΔρmax = 0.47 e Å3
73 parametersΔρmin = 0.16 e Å3
Crystal data top
C12H4N4V = 1000.5 (5) Å3
Mr = 204.19Z = 4
Monoclinic, C2/cMo Kα radiation
a = 8.896 (2) ŵ = 0.09 mm1
b = 6.9130 (19) ÅT = 100 K
c = 16.439 (5) Å0.18 × 0.13 × 0.06 mm
β = 98.290 (3)°
Data collection top
Bruker Smart APEX II Quazar
diffractometer
1543 independent reflections
Absorption correction: multi-scan
SADABS2015/1
1447 reflections with I > 2σ(I)
Tmin = 0.718, Tmax = 0.746Rint = 0.015
10353 measured reflections
Refinement top
R[F2 > 2σ(F2)] = 0.0360 restraints
wR(F2) = 0.108H-atom parameters constrained
S = 1.09Δρmax = 0.47 e Å3
1543 reflectionsΔρmin = 0.16 e Å3
73 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
N10.30686 (10)0.75641 (14)0.23988 (5)0.0216 (2)
C10.65130 (10)0.52600 (13)0.48403 (5)0.01344 (18)
H10.75330.54230.47440.016*
N20.02033 (10)0.56574 (14)0.40012 (5)0.0213 (2)
C20.53555 (10)0.57991 (13)0.42558 (5)0.01354 (18)
H20.55720.63380.37540.016*
C40.26081 (10)0.61020 (13)0.37929 (5)0.01372 (18)
C30.37903 (9)0.55627 (12)0.43884 (5)0.01240 (18)
C60.10476 (10)0.58520 (13)0.39044 (5)0.01544 (19)
C50.28658 (10)0.69132 (14)0.30189 (6)0.01588 (19)
Atomic displacement parameters (Å2) top
U11U22U33U12U13U23
N10.0225 (4)0.0240 (4)0.0184 (4)0.0010 (3)0.0030 (3)0.0031 (3)
C10.0126 (4)0.0144 (4)0.0139 (4)0.0012 (3)0.0039 (3)0.0004 (3)
N20.0167 (4)0.0262 (4)0.0211 (4)0.0001 (3)0.0029 (3)0.0002 (3)
C20.0134 (4)0.0144 (4)0.0135 (4)0.0012 (3)0.0041 (3)0.0005 (3)
C40.0137 (4)0.0140 (4)0.0136 (4)0.0005 (3)0.0025 (3)0.0009 (3)
C30.0129 (4)0.0120 (4)0.0127 (4)0.0005 (3)0.0031 (3)0.0011 (3)
C60.0156 (4)0.0163 (4)0.0141 (4)0.0002 (3)0.0009 (3)0.0004 (3)
C50.0148 (4)0.0166 (4)0.0160 (4)0.0006 (3)0.0010 (3)0.0004 (3)
Geometric parameters (Å, º) top
N1—C51.1521 (13)C2—H20.9500
C1—C21.3555 (12)C4—C31.3808 (12)
C1—C3i1.4499 (12)C4—C61.4367 (13)
C1—H10.9500C4—C51.4387 (13)
N2—C61.1546 (13)C3—C1i1.4500 (12)
C2—C31.4494 (12)
C2—C1—C3i120.64 (8)C3—C4—C5122.01 (8)
C2—C1—H1119.7C6—C4—C5116.09 (8)
C3i—C1—H1119.7C4—C3—C2120.86 (8)
C1—C2—C3120.70 (8)C4—C3—C1i120.47 (8)
C1—C2—H2119.7C2—C3—C1i118.67 (7)
C3—C2—H2119.7N2—C6—C4179.38 (10)
C3—C4—C6121.89 (8)N1—C5—C4179.84 (11)
Symmetry code: (i) x+1, y+1, z+1.
(3_corr) top
Crystal data top
C18H17CuO6F(000) = 1616
Mr = 392.86Dx = 1.538 Mg m3
Monoclinic, C2/cMo Kα radiation, λ = 0.71073 Å
a = 9.7935 (7) ÅCell parameters from 9918 reflections
b = 19.0055 (13) Åθ = 2.2–28.4°
c = 18.2997 (13) ŵ = 1.32 mm1
β = 94.7996 (11)°T = 100 K
V = 3394.2 (4) Å3Block
Z = 80.14 × 0.10 × 0.05 mm
Data collection top
Bruker Smart APEX II Quazar
diffractometer
4282 independent reflections
Radiation source: INCOATEC Microsource3719 reflections with I > 2σ(I)
ω scansθmax = 28.4°, θmin = 2.1°
Absorption correction: multi-scan
SADABS2015/1
h = 1313
Tmin = 0.695, Tmax = 0.746k = 025
4282 measured reflectionsl = 024
Refinement top
Refinement on F2652 restraints
Least-squares matrix: fullHydrogen site location: inferred from neighbouring sites
R[F2 > 2σ(F2)] = 0.026H-atom parameters constrained
wR(F2) = 0.065 w = 1/[σ2(Fo2) + (0.0269P)2 + 4.5951P]
where P = (Fo2 + 2Fc2)/3
S = 1.03(Δ/σ)max = 0.002
4282 reflectionsΔρmax = 0.36 e Å3
301 parametersΔρmin = 0.30 e Å3
Crystal data top
C18H17CuO6V = 3394.2 (4) Å3
Mr = 392.86Z = 8
Monoclinic, C2/cMo Kα radiation
a = 9.7935 (7) ŵ = 1.32 mm1
b = 19.0055 (13) ÅT = 100 K
c = 18.2997 (13) Å0.14 × 0.10 × 0.05 mm
β = 94.7996 (11)°
Data collection top
Bruker Smart APEX II Quazar
diffractometer
4282 measured reflections
Absorption correction: multi-scan
SADABS2015/1
4282 independent reflections
Tmin = 0.695, Tmax = 0.7463719 reflections with I > 2σ(I)
Refinement top
R[F2 > 2σ(F2)] = 0.026652 restraints
wR(F2) = 0.065H-atom parameters constrained
S = 1.03Δρmax = 0.36 e Å3
4282 reflectionsΔρmin = 0.30 e Å3
301 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. Refined as a 2-component twin.

Fractional atomic coordinates and isotropic or equivalent isotropic displacement parameters (Å2) top
xyzUiso*/UeqOcc. (<1)
Cu010.59102 (2)0.33936 (2)0.30514 (2)0.01672 (6)
O10.33475 (11)0.25803 (5)0.24597 (6)0.0215 (2)
O20.46737 (12)0.27545 (6)0.35097 (6)0.0219 (2)
O30.68917 (11)0.40204 (6)0.24291 (6)0.0218 (2)
O40.51062 (11)0.41946 (5)0.15900 (6)0.0214 (2)
O60.82001 (13)0.25017 (7)0.48742 (7)0.0317 (3)
C1A0.37280 (16)0.24432 (8)0.31215 (8)0.0192 (3)
C2A0.2995 (11)0.1838 (4)0.3449 (4)0.0199 (10)0.77 (3)
C3A0.2243 (9)0.1351 (4)0.3009 (4)0.0239 (10)0.77 (3)
H3A0.20860.14290.24960.029*0.77 (3)
C4A0.1725 (8)0.0755 (3)0.3323 (5)0.0307 (11)0.77 (3)
H4A0.12170.04220.30240.037*0.77 (3)
C5A0.1942 (7)0.0642 (3)0.4070 (5)0.0367 (12)0.77 (3)
H5A0.16100.02240.42770.044*0.77 (3)
C6A0.2643 (8)0.1135 (4)0.4521 (4)0.0372 (12)0.77 (3)
H6A0.27660.10640.50360.045*0.77 (3)
C7A0.3159 (9)0.1735 (3)0.4206 (4)0.0293 (11)0.77 (3)
H7A0.36290.20780.45090.035*0.77 (3)
C2B0.312 (4)0.1886 (16)0.3560 (12)0.020 (3)0.23 (3)
C3B0.239 (3)0.1373 (13)0.3165 (12)0.021 (3)0.23 (3)
H3B0.22830.13980.26450.025*0.23 (3)
C4B0.181 (2)0.0814 (13)0.3530 (14)0.032 (4)0.23 (3)
H4B0.13030.04570.32630.039*0.23 (3)
C5B0.199 (2)0.0794 (15)0.4282 (13)0.042 (4)0.23 (3)
H5B0.16370.04070.45370.051*0.23 (3)
C6B0.266 (3)0.1327 (16)0.4670 (12)0.045 (4)0.23 (3)
H6B0.26870.13280.51900.054*0.23 (3)
C7B0.331 (3)0.1861 (14)0.4317 (11)0.026 (3)0.23 (3)
H7B0.38580.21990.45860.031*0.23 (3)
C8A0.63135 (16)0.43156 (7)0.18624 (8)0.0194 (3)
C9A0.71345 (17)0.48569 (8)0.14993 (9)0.0213 (3)
C10A0.84604 (18)0.50182 (9)0.17833 (10)0.0290 (4)
H10A0.88600.47720.21990.035*
C11A0.9198 (2)0.55385 (10)0.14592 (12)0.0374 (4)
H11A1.01070.56450.16500.045*
C12A0.8611 (2)0.59023 (10)0.08580 (12)0.0373 (4)
H12A0.91130.62640.06430.045*
C13A0.7296 (2)0.57431 (10)0.05677 (11)0.0360 (4)
H13A0.68980.59930.01530.043*
C14A0.65638 (19)0.52172 (9)0.08861 (10)0.0292 (4)
H14A0.56660.51020.06840.035*
O50.76258 (12)0.33161 (6)0.39320 (7)0.0266 (3)
C150.80171 (19)0.26024 (9)0.41093 (10)0.0294 (4)
H150.73400.22600.38750.035*
C16A0.9401 (8)0.2492 (4)0.3851 (5)0.0438 (15)0.767 (10)
H16A0.93930.21000.34960.053*0.767 (10)
H16B1.00830.23900.42680.053*0.767 (10)
C17A0.9723 (4)0.31899 (19)0.3486 (2)0.0491 (10)0.767 (10)
H17A1.07090.33060.35720.059*0.767 (10)
H17B0.94700.31710.29520.059*0.767 (10)
C16B0.9458 (19)0.2469 (11)0.3743 (15)0.027 (3)0.233 (10)
H16C0.99980.20890.40010.033*0.233 (10)
H16D0.92990.23480.32170.033*0.233 (10)
C17B1.0173 (10)0.3183 (5)0.3851 (7)0.037 (3)0.233 (10)
H17C1.07530.32880.34470.044*0.233 (10)
H17D1.07390.32060.43250.044*0.233 (10)
C180.8883 (2)0.37061 (11)0.38405 (12)0.0402 (5)
H18A0.93320.38570.43200.048*
H18B0.87000.41250.35260.048*
Atomic displacement parameters (Å2) top
U11U22U33U12U13U23
Cu010.02037 (10)0.01302 (9)0.01592 (9)0.00030 (7)0.00349 (6)0.00042 (7)
O10.0262 (6)0.0171 (5)0.0203 (5)0.0031 (4)0.0025 (4)0.0016 (4)
O20.0273 (6)0.0187 (5)0.0192 (5)0.0026 (4)0.0011 (4)0.0013 (4)
O30.0247 (6)0.0186 (5)0.0214 (6)0.0016 (4)0.0025 (4)0.0027 (4)
O40.0228 (5)0.0173 (5)0.0233 (6)0.0009 (4)0.0028 (4)0.0034 (4)
O60.0352 (7)0.0318 (6)0.0259 (6)0.0052 (5)0.0112 (5)0.0027 (5)
C1A0.0216 (7)0.0153 (6)0.0206 (7)0.0022 (5)0.0016 (6)0.0001 (5)
C2A0.021 (3)0.0181 (16)0.0205 (18)0.0003 (13)0.0001 (17)0.0019 (14)
C3A0.026 (2)0.0203 (13)0.025 (2)0.0042 (13)0.0028 (18)0.0014 (15)
C4A0.034 (2)0.0238 (13)0.034 (3)0.0090 (12)0.001 (2)0.0024 (16)
C5A0.039 (2)0.0306 (17)0.040 (3)0.0150 (13)0.002 (2)0.0064 (17)
C6A0.045 (2)0.037 (2)0.029 (2)0.0128 (17)0.0035 (18)0.0080 (16)
C7A0.033 (3)0.0286 (19)0.026 (2)0.0108 (14)0.0017 (17)0.0026 (14)
C2B0.013 (5)0.023 (5)0.023 (5)0.007 (4)0.009 (4)0.001 (4)
C3B0.015 (5)0.028 (5)0.018 (6)0.001 (3)0.010 (5)0.006 (4)
C4B0.029 (5)0.036 (6)0.028 (7)0.018 (4)0.019 (5)0.011 (5)
C5B0.045 (6)0.052 (8)0.025 (6)0.030 (6)0.020 (5)0.020 (5)
C6B0.043 (7)0.059 (9)0.029 (6)0.035 (7)0.012 (5)0.008 (5)
C7B0.020 (5)0.040 (8)0.015 (5)0.020 (5)0.010 (4)0.009 (4)
C8A0.0255 (8)0.0129 (6)0.0200 (7)0.0014 (5)0.0021 (6)0.0018 (5)
C9A0.0261 (8)0.0151 (6)0.0227 (8)0.0003 (6)0.0026 (6)0.0007 (6)
C10A0.0282 (9)0.0251 (8)0.0329 (9)0.0039 (7)0.0031 (7)0.0058 (7)
C11A0.0302 (9)0.0333 (9)0.0479 (12)0.0101 (8)0.0023 (8)0.0081 (8)
C12A0.0383 (10)0.0266 (9)0.0475 (12)0.0069 (8)0.0061 (9)0.0101 (8)
C13A0.0417 (11)0.0296 (9)0.0363 (10)0.0012 (8)0.0008 (8)0.0128 (8)
C14A0.0300 (9)0.0259 (8)0.0310 (9)0.0018 (7)0.0007 (7)0.0054 (7)
O50.0312 (6)0.0206 (5)0.0257 (6)0.0009 (5)0.0109 (5)0.0025 (5)
C150.0389 (10)0.0228 (8)0.0243 (8)0.0053 (7)0.0107 (7)0.0000 (6)
C16A0.045 (3)0.052 (2)0.032 (3)0.0162 (18)0.0071 (17)0.0097 (19)
C17A0.0353 (17)0.075 (2)0.036 (2)0.0010 (14)0.0013 (15)0.0032 (15)
C16B0.020 (5)0.036 (5)0.025 (6)0.007 (4)0.003 (4)0.005 (4)
C17B0.031 (4)0.048 (4)0.029 (6)0.004 (3)0.007 (4)0.008 (3)
C180.0354 (10)0.0410 (10)0.0412 (11)0.0097 (8)0.0153 (8)0.0061 (9)
Geometric parameters (Å, º) top
Cu01—O21.9532 (11)C6B—C7B1.383 (13)
Cu01—O31.9552 (11)C6B—H6B0.9500
Cu01—O4i1.9616 (11)C7B—H7B0.9500
Cu01—O1i1.9765 (11)C8A—C9A1.495 (2)
Cu01—O52.2335 (11)C9A—C14A1.391 (2)
Cu01—Cu01i2.5785 (4)C9A—C10A1.392 (2)
O1—C1A1.2641 (19)C10A—C11A1.387 (2)
O1—Cu01i1.9765 (11)C10A—H10A0.9500
O2—C1A1.2659 (18)C11A—C12A1.383 (3)
O3—C8A1.2699 (18)C11A—H11A0.9500
O4—C8A1.2652 (19)C12A—C13A1.385 (3)
O4—Cu01i1.9616 (11)C12A—H12A0.9500
O6—C151.409 (2)C13A—C14A1.387 (2)
O6—O6ii1.483 (3)C13A—H13A0.9500
C1A—C2B1.48 (2)C14A—H14A0.9500
C1A—C2A1.507 (6)O5—C151.4390 (19)
C2A—C3A1.395 (5)O5—C181.459 (2)
C2A—C7A1.395 (5)C15—C16A1.487 (7)
C3A—C4A1.386 (4)C15—C16B1.632 (16)
C3A—H3A0.9500C15—H151.0000
C4A—C5A1.382 (5)C16A—C17A1.529 (9)
C4A—H4A0.9500C16A—H16A0.9900
C5A—C6A1.392 (4)C16A—H16B0.9900
C5A—H5A0.9500C17A—C181.466 (4)
C6A—C7A1.392 (5)C17A—H17A0.9900
C6A—H6A0.9500C17A—H17B0.9900
C7A—H7A0.9500C16B—C17B1.53 (2)
C2B—C3B1.377 (13)C16B—H16C0.9900
C2B—C7B1.383 (13)C16B—H16D0.9900
C3B—C4B1.401 (13)C17B—C181.606 (10)
C3B—H3B0.9500C17B—H17C0.9900
C4B—C5B1.373 (11)C17B—H17D0.9900
C4B—H4B0.9500C18—H18A0.9900
C5B—C6B1.375 (11)C18—H18B0.9900
C5B—H5B0.9500
O2—Cu01—O3169.00 (5)O4—C8A—C9A118.01 (13)
O2—Cu01—O4i89.36 (5)O3—C8A—C9A116.57 (14)
O3—Cu01—O4i90.57 (5)C14A—C9A—C10A119.48 (15)
O2—Cu01—O1i89.01 (5)C14A—C9A—C8A120.16 (15)
O3—Cu01—O1i89.01 (5)C10A—C9A—C8A120.34 (14)
O4i—Cu01—O1i169.19 (4)C11A—C10A—C9A120.04 (16)
O2—Cu01—O596.04 (5)C11A—C10A—H10A120.0
O3—Cu01—O594.79 (5)C9A—C10A—H10A120.0
O4i—Cu01—O5100.49 (4)C12A—C11A—C10A119.97 (18)
O1i—Cu01—O590.32 (4)C12A—C11A—H11A120.0
O2—Cu01—Cu01i85.59 (3)C10A—C11A—H11A120.0
O3—Cu01—Cu01i83.43 (3)C11A—C12A—C13A120.49 (17)
O4i—Cu01—Cu01i85.69 (3)C11A—C12A—H12A119.8
O1i—Cu01—Cu01i83.53 (3)C13A—C12A—H12A119.8
O5—Cu01—Cu01i173.61 (3)C12A—C13A—C14A119.55 (17)
C1A—O1—Cu01i121.60 (10)C12A—C13A—H13A120.2
C1A—O2—Cu01120.04 (10)C14A—C13A—H13A120.2
C8A—O3—Cu01122.51 (10)C13A—C14A—C9A120.45 (17)
C8A—O4—Cu01i119.53 (10)C13A—C14A—H14A119.8
C15—O6—O6ii105.37 (14)C9A—C14A—H14A119.8
O1—C1A—O2125.76 (14)C15—O5—C18107.06 (14)
O1—C1A—C2B124.5 (9)C15—O5—Cu01113.26 (9)
O2—C1A—C2B109.8 (9)C18—O5—Cu01118.35 (10)
O1—C1A—C2A115.2 (3)O6—C15—O5111.18 (14)
O2—C1A—C2A119.0 (3)O6—C15—C16A104.6 (4)
C3A—C2A—C7A119.5 (4)O5—C15—C16A107.1 (3)
C3A—C2A—C1A121.5 (4)O6—C15—C16B110.1 (10)
C7A—C2A—C1A118.8 (4)O5—C15—C16B106.1 (8)
C4A—C3A—C2A119.7 (4)O6—C15—H15111.2
C4A—C3A—H3A120.1O5—C15—H15111.2
C2A—C3A—H3A120.1C16A—C15—H15111.2
C5A—C4A—C3A120.4 (3)C15—C16A—C17A104.1 (4)
C5A—C4A—H4A119.8C15—C16A—H16A110.9
C3A—C4A—H4A119.8C17A—C16A—H16A110.9
C4A—C5A—C6A120.6 (3)C15—C16A—H16B110.9
C4A—C5A—H5A119.7C17A—C16A—H16B110.9
C6A—C5A—H5A119.7H16A—C16A—H16B109.0
C7A—C6A—C5A118.9 (4)C18—C17A—C16A104.1 (3)
C7A—C6A—H6A120.5C18—C17A—H17A110.9
C5A—C6A—H6A120.5C16A—C17A—H17A110.9
C6A—C7A—C2A120.7 (4)C18—C17A—H17B110.9
C6A—C7A—H7A119.6C16A—C17A—H17B110.9
C2A—C7A—H7A119.6H17A—C17A—H17B109.0
C3B—C2B—C7B121.4 (15)C17B—C16B—C15102.1 (11)
C3B—C2B—C1A115.8 (15)C17B—C16B—H16C111.3
C7B—C2B—C1A122.8 (15)C15—C16B—H16C111.3
C2B—C3B—C4B120.0 (13)C17B—C16B—H16D111.3
C2B—C3B—H3B120.0C15—C16B—H16D111.3
C4B—C3B—H3B120.0H16C—C16B—H16D109.2
C5B—C4B—C3B118.4 (12)C16B—C17B—C18101.3 (8)
C5B—C4B—H4B120.8C16B—C17B—H17C111.5
C3B—C4B—H4B120.8C18—C17B—H17C111.5
C4B—C5B—C6B120.9 (12)C16B—C17B—H17D111.5
C4B—C5B—H5B119.6C18—C17B—H17D111.5
C6B—C5B—H5B119.6H17C—C17B—H17D109.3
C5B—C6B—C7B121.2 (12)O5—C18—C17A102.76 (19)
C5B—C6B—H6B119.4O5—C18—C17B110.8 (4)
C7B—C6B—H6B119.4O5—C18—H18A111.2
C6B—C7B—C2B117.8 (13)C17A—C18—H18A111.2
C6B—C7B—H7B121.1O5—C18—H18B111.2
C2B—C7B—H7B121.1C17A—C18—H18B111.2
O4—C8A—O3125.42 (14)H18A—C18—H18B109.1
Symmetry codes: (i) x+1, y, z+1/2; (ii) x+3/2, y+1/2, z+1.
(3_filter) top
Crystal data top
C18H17CuO6F(000) = 1616
Mr = 392.86Dx = 1.538 Mg m3
Monoclinic, C2/cMo Kα radiation, λ = 0.71073 Å
a = 9.7936 (7) ÅCell parameters from 9174 reflections
b = 18.9973 (12) Åθ = 2.2–28.3°
c = 18.2982 (12) ŵ = 1.32 mm1
β = 94.840 (1)°T = 100 K
V = 3392.3 (4) Å3Block
Z = 80.14 × 0.10 × 0.05 mm
Data collection top
Bruker Smart APEX II Quazar
diffractometer
3574 reflections with I > 2σ(I)
Radiation source: INCOATEC MicrosourceRint = 0.033
ω scansθmax = 28.3°, θmin = 2.1°
Absorption correction: multi-scan
SADABS2015/1
h = 1313
Tmin = 0.694, Tmax = 0.746k = 2525
29137 measured reflectionsl = 2324
4233 independent reflections
Refinement top
Refinement on F2652 restraints
Least-squares matrix: fullHydrogen site location: inferred from neighbouring sites
R[F2 > 2σ(F2)] = 0.028H-atom parameters constrained
wR(F2) = 0.068 w = 1/[σ2(Fo2) + (0.030P)2 + 3.6174P]
where P = (Fo2 + 2Fc2)/3
S = 1.03(Δ/σ)max = 0.001
4233 reflectionsΔρmax = 0.34 e Å3
300 parametersΔρmin = 0.29 e Å3
Crystal data top
C18H17CuO6V = 3392.3 (4) Å3
Mr = 392.86Z = 8
Monoclinic, C2/cMo Kα radiation
a = 9.7936 (7) ŵ = 1.32 mm1
b = 18.9973 (12) ÅT = 100 K
c = 18.2982 (12) Å0.14 × 0.10 × 0.05 mm
β = 94.840 (1)°
Data collection top
Bruker Smart APEX II Quazar
diffractometer
4233 independent reflections
Absorption correction: multi-scan
SADABS2015/1
3574 reflections with I > 2σ(I)
Tmin = 0.694, Tmax = 0.746Rint = 0.033
29137 measured reflections
Refinement top
R[F2 > 2σ(F2)] = 0.028652 restraints
wR(F2) = 0.068H-atom parameters constrained
S = 1.03Δρmax = 0.34 e Å3
4233 reflectionsΔρmin = 0.29 e Å3
300 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)
Cu010.59102 (2)0.33935 (2)0.30513 (2)0.01757 (6)
O10.33470 (12)0.25799 (6)0.24597 (6)0.0222 (2)
O20.46752 (12)0.27546 (6)0.35100 (6)0.0227 (2)
O30.68907 (12)0.40206 (6)0.24299 (6)0.0223 (2)
O40.51060 (12)0.41946 (6)0.15903 (6)0.0221 (2)
O60.82008 (13)0.25014 (7)0.48747 (7)0.0336 (3)
C1A0.37271 (17)0.24419 (8)0.31215 (9)0.0200 (3)
C2A0.3003 (12)0.1825 (5)0.3452 (4)0.0212 (12)0.74 (3)
C3A0.2247 (11)0.1347 (4)0.3005 (5)0.0244 (12)0.74 (3)
H3A0.20930.14280.24930.029*0.74 (3)
C4A0.1722 (9)0.0752 (3)0.3319 (5)0.0312 (12)0.74 (3)
H4A0.12120.04190.30190.037*0.74 (3)
C5A0.1941 (7)0.0640 (3)0.4067 (5)0.0355 (13)0.74 (3)
H5A0.16020.02230.42740.043*0.74 (3)
C6A0.2648 (8)0.1130 (4)0.4521 (4)0.0358 (12)0.74 (3)
H6A0.27750.10560.50360.043*0.74 (3)
C7A0.3165 (11)0.1727 (4)0.4207 (4)0.0297 (12)0.74 (3)
H7A0.36330.20720.45100.036*0.74 (3)
C2B0.308 (3)0.1915 (14)0.3534 (12)0.021 (3)0.26 (3)
C3B0.235 (3)0.1389 (13)0.3155 (12)0.024 (3)0.26 (3)
H3B0.22160.14130.26350.028*0.26 (3)
C4B0.179 (2)0.0822 (13)0.3519 (14)0.037 (4)0.26 (3)
H4B0.12820.04640.32520.044*0.26 (3)
C5B0.199 (2)0.0795 (15)0.4266 (13)0.050 (4)0.26 (3)
H5B0.16650.04020.45220.060*0.26 (3)
C6B0.265 (3)0.1334 (16)0.4649 (12)0.052 (5)0.26 (3)
H6B0.26740.13380.51700.062*0.26 (3)
C7B0.328 (3)0.1867 (14)0.4297 (11)0.029 (4)0.26 (3)
H7B0.38490.21970.45690.035*0.26 (3)
C8A0.63139 (17)0.43158 (8)0.18634 (9)0.0202 (3)
C9A0.71326 (18)0.48566 (8)0.14995 (9)0.0222 (3)
C10A0.84551 (19)0.50186 (9)0.17827 (11)0.0302 (4)
H10A0.88540.47720.21990.036*
C11A0.9194 (2)0.55379 (10)0.14601 (12)0.0384 (5)
H11A1.01030.56440.16520.046*
C12A0.8607 (2)0.59020 (10)0.08580 (12)0.0390 (5)
H12A0.91090.62640.06430.047*
C13A0.7295 (2)0.57426 (10)0.05677 (12)0.0376 (5)
H13A0.68970.59920.01530.045*
C14A0.6565 (2)0.52176 (10)0.08859 (10)0.0301 (4)
H14A0.56670.51030.06830.036*
O50.76250 (13)0.33154 (6)0.39327 (7)0.0273 (3)
C150.8014 (2)0.26029 (9)0.41088 (10)0.0312 (4)
H150.73330.22620.38760.037*
C16A0.9395 (10)0.2488 (5)0.3849 (7)0.0455 (17)0.753 (12)
H16A0.93810.20960.34920.055*0.753 (12)
H16B1.00790.23830.42650.055*0.753 (12)
C17A0.9717 (4)0.3188 (2)0.3485 (3)0.0499 (11)0.753 (12)
H17A1.07040.33030.35690.060*0.753 (12)
H17B0.94610.31710.29500.060*0.753 (12)
C16B0.947 (2)0.2485 (13)0.376 (2)0.033 (3)0.247 (12)
H16C1.00220.21200.40390.040*0.247 (12)
H16D0.93310.23420.32420.040*0.247 (12)
C17B1.0154 (12)0.3183 (5)0.3837 (8)0.043 (3)0.247 (12)
H17C1.07040.32790.34180.051*0.247 (12)
H17D1.07530.32170.43000.051*0.247 (12)
C180.8883 (2)0.37061 (12)0.38401 (12)0.0424 (5)
H18A0.93340.38570.43190.051*
H18B0.86990.41250.35250.051*
Atomic displacement parameters (Å2) top
U11U22U33U12U13U23
Cu010.02138 (11)0.01346 (10)0.01695 (10)0.00031 (7)0.00373 (7)0.00031 (7)
O10.0275 (6)0.0170 (5)0.0213 (6)0.0031 (4)0.0028 (5)0.0012 (4)
O20.0287 (6)0.0194 (5)0.0192 (6)0.0026 (5)0.0020 (5)0.0018 (4)
O30.0246 (6)0.0201 (5)0.0213 (6)0.0021 (4)0.0030 (5)0.0027 (5)
O40.0242 (6)0.0180 (5)0.0233 (6)0.0013 (4)0.0030 (5)0.0028 (5)
O60.0374 (7)0.0338 (7)0.0270 (7)0.0055 (6)0.0120 (6)0.0022 (6)
C1A0.0226 (8)0.0149 (7)0.0223 (8)0.0029 (6)0.0012 (6)0.0003 (6)
C2A0.024 (3)0.015 (2)0.025 (2)0.0013 (15)0.0045 (19)0.0019 (16)
C3A0.027 (3)0.0196 (15)0.026 (2)0.0047 (14)0.001 (2)0.0039 (17)
C4A0.034 (2)0.0255 (16)0.034 (3)0.0102 (13)0.002 (2)0.0036 (17)
C5A0.037 (2)0.0274 (18)0.042 (3)0.0145 (14)0.003 (2)0.0056 (18)
C6A0.045 (2)0.034 (3)0.029 (2)0.0132 (19)0.0037 (17)0.0077 (17)
C7A0.034 (3)0.026 (2)0.029 (2)0.0105 (16)0.0004 (18)0.0014 (16)
C2B0.015 (5)0.018 (5)0.028 (5)0.002 (4)0.010 (3)0.004 (4)
C3B0.024 (5)0.023 (5)0.022 (6)0.001 (4)0.009 (5)0.004 (4)
C4B0.035 (5)0.032 (6)0.039 (7)0.018 (4)0.019 (5)0.010 (5)
C5B0.057 (7)0.056 (8)0.032 (7)0.031 (6)0.018 (5)0.020 (5)
C6B0.052 (7)0.059 (9)0.040 (6)0.033 (7)0.012 (5)0.010 (5)
C7B0.025 (5)0.038 (8)0.022 (5)0.017 (6)0.008 (4)0.006 (4)
C8A0.0258 (8)0.0137 (7)0.0210 (8)0.0006 (6)0.0008 (6)0.0022 (6)
C9A0.0276 (8)0.0152 (7)0.0241 (8)0.0006 (6)0.0033 (7)0.0013 (6)
C10A0.0305 (9)0.0262 (9)0.0328 (10)0.0035 (7)0.0036 (8)0.0055 (7)
C11A0.0321 (10)0.0333 (10)0.0487 (13)0.0100 (8)0.0025 (9)0.0073 (9)
C12A0.0396 (11)0.0281 (10)0.0496 (13)0.0067 (8)0.0055 (9)0.0106 (9)
C13A0.0422 (11)0.0315 (10)0.0387 (11)0.0011 (8)0.0005 (9)0.0136 (9)
C14A0.0305 (9)0.0282 (9)0.0309 (10)0.0016 (7)0.0015 (7)0.0067 (8)
O50.0318 (7)0.0216 (6)0.0262 (7)0.0010 (5)0.0111 (5)0.0027 (5)
C150.0400 (10)0.0243 (9)0.0268 (9)0.0054 (7)0.0115 (8)0.0004 (7)
C16A0.043 (3)0.055 (3)0.036 (4)0.015 (2)0.008 (2)0.006 (2)
C17A0.0349 (19)0.080 (2)0.034 (2)0.0000 (15)0.0019 (16)0.0037 (16)
C16B0.026 (5)0.042 (6)0.030 (7)0.006 (4)0.003 (5)0.001 (4)
C17B0.041 (4)0.052 (5)0.033 (6)0.004 (3)0.008 (4)0.009 (4)
C180.0373 (11)0.0437 (11)0.0428 (12)0.0105 (9)0.0162 (9)0.0077 (10)
Geometric parameters (Å, º) top
Cu01—O21.9524 (12)C6B—C7B1.375 (13)
Cu01—O31.9540 (12)C6B—H6B0.9500
Cu01—O4i1.9612 (11)C7B—H7B0.9500
Cu01—O1i1.9768 (11)C8A—C9A1.494 (2)
Cu01—O52.2330 (12)C9A—C10A1.388 (2)
Cu01—Cu01i2.5773 (4)C9A—C14A1.391 (2)
O1—C1A1.2640 (19)C10A—C11A1.385 (3)
O1—Cu01i1.9768 (11)C10A—H10A0.9500
O2—C1A1.2685 (19)C11A—C12A1.384 (3)
O3—C8A1.2685 (19)C11A—H11A0.9500
O4—C8A1.2659 (19)C12A—C13A1.382 (3)
O4—Cu01i1.9613 (11)C12A—H12A0.9500
O6—C151.411 (2)C13A—C14A1.384 (3)
O6—O6ii1.484 (3)C13A—H13A0.9500
C1A—C2B1.43 (2)C14A—H14A0.9500
C1A—C2A1.521 (7)O5—C151.435 (2)
C2A—C7A1.390 (5)O5—C181.460 (2)
C2A—C3A1.392 (5)C15—C16A1.487 (7)
C3A—C4A1.386 (5)C15—C16B1.625 (18)
C3A—H3A0.9500C15—H151.0000
C4A—C5A1.385 (5)C16A—C17A1.532 (11)
C4A—H4A0.9500C16A—H16A0.9900
C5A—C6A1.392 (5)C16A—H16B0.9900
C5A—H5A0.9500C17A—C181.465 (4)
C6A—C7A1.388 (5)C17A—H17A0.9900
C6A—H6A0.9500C17A—H17B0.9900
C7A—H7A0.9500C16B—C17B1.49 (3)
C2B—C3B1.384 (12)C16B—H16C0.9900
C2B—C7B1.398 (13)C16B—H16D0.9900
C3B—C4B1.402 (13)C17B—C181.593 (11)
C3B—H3B0.9500C17B—H17C0.9900
C4B—C5B1.366 (12)C17B—H17D0.9900
C4B—H4B0.9500C18—H18A0.9900
C5B—C6B1.372 (11)C18—H18B0.9900
C5B—H5B0.9500
O2—Cu01—O3169.06 (5)O4—C8A—C9A117.89 (14)
O2—Cu01—O4i89.33 (5)O3—C8A—C9A116.71 (14)
O3—Cu01—O4i90.56 (5)C10A—C9A—C14A119.27 (16)
O2—Cu01—O1i89.04 (5)C10A—C9A—C8A120.32 (15)
O3—Cu01—O1i89.02 (5)C14A—C9A—C8A120.38 (16)
O4i—Cu01—O1i169.20 (5)C11A—C10A—C9A120.23 (17)
O2—Cu01—O595.95 (5)C11A—C10A—H10A119.9
O3—Cu01—O594.83 (5)C9A—C10A—H10A119.9
O4i—Cu01—O5100.49 (5)C12A—C11A—C10A119.87 (19)
O1i—Cu01—O590.30 (5)C12A—C11A—H11A120.1
O2—Cu01—Cu01i85.63 (3)C10A—C11A—H11A120.1
O3—Cu01—Cu01i83.45 (3)C13A—C12A—C11A120.46 (18)
O4i—Cu01—Cu01i85.68 (3)C13A—C12A—H12A119.8
O1i—Cu01—Cu01i83.54 (3)C11A—C12A—H12A119.8
O5—Cu01—Cu01i173.63 (4)C12A—C13A—C14A119.54 (18)
C1A—O1—Cu01i121.66 (10)C12A—C13A—H13A120.2
C1A—O2—Cu01120.06 (10)C14A—C13A—H13A120.2
C8A—O3—Cu01122.56 (11)C13A—C14A—C9A120.61 (18)
C8A—O4—Cu01i119.52 (10)C13A—C14A—H14A119.7
C15—O6—O6ii105.17 (14)C9A—C14A—H14A119.7
O1—C1A—O2125.61 (15)C15—O5—C18107.15 (15)
O1—C1A—C2B122.8 (10)C15—O5—Cu01113.21 (10)
O2—C1A—C2B111.6 (9)C18—O5—Cu01118.22 (11)
O1—C1A—C2A115.5 (4)O6—C15—O5111.20 (15)
O2—C1A—C2A118.8 (4)O6—C15—C16A104.6 (5)
C7A—C2A—C3A120.4 (4)O5—C15—C16A107.3 (4)
C7A—C2A—C1A118.7 (5)O6—C15—C16B108.8 (14)
C3A—C2A—C1A120.8 (5)O5—C15—C16B105.6 (9)
C4A—C3A—C2A119.1 (5)O6—C15—H15111.2
C4A—C3A—H3A120.4O5—C15—H15111.2
C2A—C3A—H3A120.4C16A—C15—H15111.2
C5A—C4A—C3A120.1 (4)C15—C16A—C17A103.7 (5)
C5A—C4A—H4A119.9C15—C16A—H16A111.0
C3A—C4A—H4A119.9C17A—C16A—H16A111.0
C4A—C5A—C6A121.1 (4)C15—C16A—H16B111.0
C4A—C5A—H5A119.5C17A—C16A—H16B111.0
C6A—C5A—H5A119.5H16A—C16A—H16B109.0
C7A—C6A—C5A118.7 (4)C18—C17A—C16A104.3 (3)
C7A—C6A—H6A120.7C18—C17A—H17A110.9
C5A—C6A—H6A120.7C16A—C17A—H17A110.9
C6A—C7A—C2A120.4 (4)C18—C17A—H17B110.9
C6A—C7A—H7A119.8C16A—C17A—H17B110.9
C2A—C7A—H7A119.8H17A—C17A—H17B108.9
C3B—C2B—C7B118.5 (14)C17B—C16B—C15104.1 (13)
C3B—C2B—C1A118.4 (15)C17B—C16B—H16C110.9
C7B—C2B—C1A122.7 (15)C15—C16B—H16C110.9
C2B—C3B—C4B121.6 (13)C17B—C16B—H16D110.9
C2B—C3B—H3B119.2C15—C16B—H16D110.9
C4B—C3B—H3B119.2H16C—C16B—H16D108.9
C5B—C4B—C3B118.4 (12)C16B—C17B—C18102.2 (9)
C5B—C4B—H4B120.8C16B—C17B—H17C111.3
C3B—C4B—H4B120.8C18—C17B—H17C111.3
C4B—C5B—C6B120.4 (13)C16B—C17B—H17D111.3
C4B—C5B—H5B119.8C18—C17B—H17D111.3
C6B—C5B—H5B119.8H17C—C17B—H17D109.2
C5B—C6B—C7B121.5 (13)O5—C18—C17A102.6 (2)
C5B—C6B—H6B119.3O5—C18—C17B110.5 (4)
C7B—C6B—H6B119.3O5—C18—H18A111.3
C6B—C7B—C2B119.0 (13)C17A—C18—H18A111.3
C6B—C7B—H7B120.5O5—C18—H18B111.3
C2B—C7B—H7B120.5C17A—C18—H18B111.3
O4—C8A—O3125.39 (15)H18A—C18—H18B109.2
Symmetry codes: (i) x+1, y, z+1/2; (ii) x+3/2, y+1/2, z+1.
(3_uncorr) top
Crystal data top
C18H17CuO6F(000) = 1616
Mr = 392.86Dx = 1.538 Mg m3
Monoclinic, C2/cMo Kα radiation, λ = 0.71073 Å
a = 9.7935 (7) ÅCell parameters from 9918 reflections
b = 19.0055 (13) Åθ = 2.2–28.4°
c = 18.2997 (13) ŵ = 1.32 mm1
β = 94.7996 (11)°T = 100 K
V = 3394.2 (4) Å3Block
Z = 80.14 × 0.10 × 0.05 mm
Data collection top
Bruker Smart APEX II Quazar
diffractometer
3723 reflections with I > 2σ(I)
Radiation source: INCOATEC MicrosourceRint = 0.028
ω scansθmax = 28.4°, θmin = 2.1°
Absorption correction: multi-scan
SADABS2015/1
h = 1313
Tmin = 0.695, Tmax = 0.746k = 2525
29203 measured reflectionsl = 2324
4282 independent reflections
Refinement top
Refinement on F2652 restraints
Least-squares matrix: fullHydrogen site location: inferred from neighbouring sites
R[F2 > 2σ(F2)] = 0.027H-atom parameters constrained
wR(F2) = 0.070 w = 1/[σ2(Fo2) + (0.025P)2 + 6.0544P]
where P = (Fo2 + 2Fc2)/3
S = 1.07(Δ/σ)max = 0.001
4282 reflectionsΔρmax = 0.39 e Å3
300 parametersΔρmin = 0.28 e Å3
Crystal data top
C18H17CuO6V = 3394.2 (4) Å3
Mr = 392.86Z = 8
Monoclinic, C2/cMo Kα radiation
a = 9.7935 (7) ŵ = 1.32 mm1
b = 19.0055 (13) ÅT = 100 K
c = 18.2997 (13) Å0.14 × 0.10 × 0.05 mm
β = 94.7996 (11)°
Data collection top
Bruker Smart APEX II Quazar
diffractometer
4282 independent reflections
Absorption correction: multi-scan
SADABS2015/1
3723 reflections with I > 2σ(I)
Tmin = 0.695, Tmax = 0.746Rint = 0.028
29203 measured reflections
Refinement top
R[F2 > 2σ(F2)] = 0.027652 restraints
wR(F2) = 0.070H-atom parameters constrained
S = 1.07Δρmax = 0.39 e Å3
4282 reflectionsΔρmin = 0.28 e Å3
300 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)
Cu010.59101 (2)0.33937 (2)0.30514 (2)0.01673 (6)
O10.33471 (13)0.25803 (6)0.24597 (7)0.0214 (3)
O20.46739 (13)0.27545 (6)0.35094 (7)0.0218 (3)
O30.68924 (13)0.40206 (6)0.24288 (7)0.0218 (3)
O40.51069 (12)0.41946 (6)0.15900 (7)0.0214 (3)
O60.82003 (14)0.25019 (7)0.48743 (8)0.0319 (3)
C1A0.37285 (17)0.24429 (8)0.31215 (9)0.0192 (3)
C2A0.2992 (11)0.1840 (4)0.3450 (4)0.0203 (11)0.78 (3)
C3A0.2241 (10)0.1352 (4)0.3010 (4)0.0246 (12)0.78 (3)
H3A0.20840.14290.24970.030*0.78 (3)
C4A0.1726 (8)0.0755 (3)0.3324 (5)0.0312 (11)0.78 (3)
H4A0.12200.04220.30240.037*0.78 (3)
C5A0.1943 (7)0.0642 (3)0.4071 (5)0.0367 (13)0.78 (3)
H5A0.16120.02240.42780.044*0.78 (3)
C6A0.2645 (8)0.1136 (4)0.4523 (4)0.0371 (12)0.78 (3)
H6A0.27650.10650.50380.044*0.78 (3)
C7A0.3168 (10)0.1736 (4)0.4207 (4)0.0288 (11)0.78 (3)
H7A0.36480.20760.45100.035*0.78 (3)
C2B0.313 (4)0.1877 (17)0.3561 (14)0.019 (3)0.22 (3)
C3B0.240 (3)0.1367 (14)0.3162 (13)0.020 (3)0.22 (3)
H3B0.22840.13930.26420.024*0.22 (3)
C4B0.181 (3)0.0811 (14)0.3532 (15)0.031 (4)0.22 (3)
H4B0.13090.04520.32670.037*0.22 (3)
C5B0.198 (3)0.0797 (17)0.4286 (14)0.042 (4)0.22 (3)
H5B0.16260.04120.45420.051*0.22 (3)
C6B0.266 (3)0.1333 (18)0.4676 (13)0.045 (5)0.22 (3)
H6B0.26910.13310.51960.054*0.22 (3)
C7B0.328 (3)0.1874 (16)0.4322 (13)0.028 (4)0.22 (3)
H7B0.37920.22290.45890.033*0.22 (3)
C8A0.63128 (18)0.43150 (8)0.18617 (9)0.0195 (3)
C9A0.71369 (19)0.48566 (9)0.14992 (10)0.0213 (3)
C10A0.8460 (2)0.50180 (10)0.17825 (11)0.0291 (4)
H10A0.88600.47710.21990.035*
C11A0.9198 (2)0.55389 (11)0.14586 (13)0.0373 (5)
H11A1.01070.56460.16490.045*
C12A0.8611 (2)0.59018 (11)0.08586 (13)0.0373 (5)
H12A0.91130.62640.06440.045*
C13A0.7297 (2)0.57433 (11)0.05671 (12)0.0360 (5)
H13A0.69000.59920.01520.043*
C14A0.6563 (2)0.52173 (10)0.08865 (11)0.0292 (4)
H14A0.56650.51030.06860.035*
O50.76263 (14)0.33161 (6)0.39318 (7)0.0267 (3)
C150.8017 (2)0.26021 (10)0.41085 (11)0.0292 (4)
H150.73370.22600.38750.035*
C16A0.9397 (9)0.2490 (5)0.3848 (6)0.0437 (16)0.766 (11)
H16A0.93830.20990.34900.052*0.766 (11)
H16B1.00800.23840.42630.052*0.766 (11)
C17A0.9721 (4)0.3190 (2)0.3485 (3)0.0490 (11)0.766 (11)
H17A1.07070.33050.35720.059*0.766 (11)
H17B0.94690.31740.29500.059*0.766 (11)
C16B0.947 (2)0.2475 (12)0.3752 (18)0.030 (3)0.234 (11)
H16C1.00120.21000.40160.036*0.234 (11)
H16D0.93190.23470.32270.036*0.234 (11)
C17B1.0173 (11)0.3184 (5)0.3849 (8)0.038 (3)0.234 (11)
H17C1.07460.32860.34420.045*0.234 (11)
H17D1.07460.32100.43210.045*0.234 (11)
C180.8883 (2)0.37061 (12)0.38404 (13)0.0400 (5)
H18A0.93320.38560.43200.048*
H18B0.87000.41250.35260.048*
Atomic displacement parameters (Å2) top
U11U22U33U12U13U23
Cu010.02037 (11)0.01304 (10)0.01594 (10)0.00031 (7)0.00349 (7)0.00043 (7)
O10.0263 (6)0.0169 (6)0.0204 (6)0.0031 (5)0.0020 (5)0.0017 (5)
O20.0275 (6)0.0185 (6)0.0189 (6)0.0026 (5)0.0012 (5)0.0011 (5)
O30.0249 (6)0.0186 (6)0.0213 (6)0.0016 (5)0.0029 (5)0.0025 (5)
O40.0231 (6)0.0173 (6)0.0230 (6)0.0007 (5)0.0029 (5)0.0031 (5)
O60.0352 (7)0.0321 (7)0.0260 (7)0.0055 (6)0.0117 (6)0.0026 (6)
C1A0.0218 (8)0.0154 (7)0.0204 (8)0.0026 (6)0.0017 (6)0.0004 (6)
C2A0.021 (3)0.0191 (16)0.0207 (19)0.0009 (14)0.0001 (18)0.0027 (15)
C3A0.026 (3)0.0208 (14)0.026 (2)0.0039 (15)0.0029 (19)0.0005 (16)
C4A0.035 (2)0.0247 (15)0.034 (3)0.0088 (13)0.000 (2)0.0014 (17)
C5A0.039 (2)0.0311 (19)0.040 (3)0.0140 (14)0.002 (2)0.0066 (19)
C6A0.045 (2)0.037 (2)0.030 (2)0.0126 (18)0.0042 (19)0.0083 (17)
C7A0.034 (3)0.027 (2)0.025 (2)0.0101 (15)0.0004 (18)0.0018 (15)
C2B0.010 (5)0.021 (5)0.024 (6)0.007 (4)0.009 (4)0.000 (4)
C3B0.011 (5)0.027 (5)0.020 (6)0.000 (3)0.010 (5)0.008 (5)
C4B0.030 (6)0.034 (6)0.027 (7)0.019 (5)0.017 (5)0.012 (5)
C5B0.048 (7)0.051 (9)0.024 (7)0.030 (7)0.019 (5)0.018 (5)
C6B0.043 (8)0.058 (9)0.031 (6)0.033 (8)0.013 (5)0.008 (6)
C7B0.023 (5)0.041 (8)0.018 (5)0.020 (6)0.010 (4)0.007 (5)
C8A0.0254 (8)0.0130 (7)0.0200 (8)0.0016 (6)0.0020 (7)0.0018 (6)
C9A0.0264 (9)0.0153 (7)0.0222 (8)0.0003 (6)0.0023 (7)0.0008 (6)
C10A0.0289 (10)0.0249 (9)0.0325 (10)0.0037 (7)0.0027 (8)0.0056 (8)
C11A0.0295 (10)0.0332 (11)0.0483 (13)0.0101 (8)0.0022 (9)0.0082 (9)
C12A0.0384 (11)0.0264 (10)0.0476 (13)0.0064 (8)0.0065 (10)0.0104 (9)
C13A0.0414 (12)0.0299 (10)0.0362 (11)0.0012 (9)0.0006 (9)0.0130 (9)
C14A0.0299 (10)0.0259 (9)0.0312 (10)0.0020 (8)0.0013 (8)0.0058 (8)
O50.0313 (7)0.0207 (6)0.0260 (7)0.0010 (5)0.0106 (5)0.0026 (5)
C150.0385 (11)0.0228 (9)0.0242 (9)0.0049 (8)0.0104 (8)0.0003 (7)
C16A0.044 (3)0.052 (3)0.034 (3)0.015 (2)0.008 (2)0.009 (2)
C17A0.0356 (19)0.075 (2)0.035 (2)0.0006 (16)0.0017 (17)0.0036 (16)
C16B0.021 (5)0.038 (6)0.030 (7)0.008 (4)0.003 (5)0.005 (4)
C17B0.034 (4)0.049 (5)0.028 (6)0.005 (3)0.008 (4)0.010 (4)
C180.0352 (11)0.0410 (12)0.0406 (12)0.0092 (9)0.0157 (9)0.0055 (10)
Geometric parameters (Å, º) top
Cu01—O21.9529 (12)C6B—C7B1.386 (13)
Cu01—O31.9562 (12)C6B—H6B0.9500
Cu01—O4i1.9620 (12)C7B—H7B0.9500
Cu01—O1i1.9768 (12)C8A—C9A1.497 (2)
Cu01—O52.2336 (12)C9A—C10A1.389 (3)
Cu01—Cu01i2.5787 (4)C9A—C14A1.392 (3)
O1—C1A1.264 (2)C10A—C11A1.388 (3)
O1—Cu01i1.9768 (12)C10A—H10A0.9500
O2—C1A1.266 (2)C11A—C12A1.381 (3)
O3—C8A1.270 (2)C11A—H11A0.9500
O4—C8A1.263 (2)C12A—C13A1.384 (3)
O4—Cu01i1.9620 (12)C12A—H12A0.9500
O6—C151.411 (2)C13A—C14A1.388 (3)
O6—O6ii1.483 (3)C13A—H13A0.9500
C1A—C2B1.49 (2)C14A—H14A0.9500
C1A—C2A1.505 (6)O5—C151.439 (2)
C2A—C3A1.396 (5)O5—C181.458 (2)
C2A—C7A1.396 (5)C15—C16A1.486 (7)
C3A—C4A1.385 (5)C15—C16B1.632 (18)
C3A—H3A0.9500C15—H151.0000
C4A—C5A1.383 (5)C16A—C17A1.531 (10)
C4A—H4A0.9500C16A—H16A0.9900
C5A—C6A1.394 (5)C16A—H16B0.9900
C5A—H5A0.9500C17A—C181.465 (4)
C6A—C7A1.395 (5)C17A—H17A0.9900
C6A—H6A0.9500C17A—H17B0.9900
C7A—H7A0.9500C16B—C17B1.52 (3)
C2B—C3B1.380 (13)C16B—H16C0.9900
C2B—C7B1.388 (13)C16B—H16D0.9900
C3B—C4B1.403 (13)C17B—C181.606 (11)
C3B—H3B0.9500C17B—H17C0.9900
C4B—C5B1.376 (12)C17B—H17D0.9900
C4B—H4B0.9500C18—H18A0.9900
C5B—C6B1.381 (12)C18—H18B0.9900
C5B—H5B0.9500
O2—Cu01—O3168.99 (5)O4—C8A—C9A118.11 (15)
O2—Cu01—O4i89.36 (5)O3—C8A—C9A116.38 (15)
O3—Cu01—O4i90.59 (5)C10A—C9A—C14A119.53 (17)
O2—Cu01—O1i89.00 (5)C10A—C9A—C8A120.48 (16)
O3—Cu01—O1i88.99 (5)C14A—C9A—C8A119.97 (16)
O4i—Cu01—O1i169.18 (5)C11A—C10A—C9A120.08 (18)
O2—Cu01—O596.06 (5)C11A—C10A—H10A120.0
O3—Cu01—O594.78 (5)C9A—C10A—H10A120.0
O4i—Cu01—O5100.51 (5)C12A—C11A—C10A119.9 (2)
O1i—Cu01—O590.30 (5)C12A—C11A—H11A120.0
O2—Cu01—Cu01i85.59 (4)C10A—C11A—H11A120.0
O3—Cu01—Cu01i83.43 (4)C11A—C12A—C13A120.65 (19)
O4i—Cu01—Cu01i85.68 (4)C11A—C12A—H12A119.7
O1i—Cu01—Cu01i83.53 (4)C13A—C12A—H12A119.7
O5—Cu01—Cu01i173.59 (4)C12A—C13A—C14A119.44 (19)
C1A—O1—Cu01i121.59 (11)C12A—C13A—H13A120.3
C1A—O2—Cu01120.07 (11)C14A—C13A—H13A120.3
C8A—O3—Cu01122.43 (11)C13A—C14A—C9A120.38 (19)
C8A—O4—Cu01i119.54 (11)C13A—C14A—H14A119.8
C15—O6—O6ii105.33 (15)C9A—C14A—H14A119.8
O1—C1A—O2125.75 (16)C15—O5—C18107.10 (16)
O1—C1A—C2B124.6 (10)C15—O5—Cu01113.21 (10)
O2—C1A—C2B109.6 (10)C18—O5—Cu01118.36 (11)
O1—C1A—C2A115.2 (3)O6—C15—O5111.09 (15)
O2—C1A—C2A119.0 (3)O6—C15—C16A104.8 (5)
C3A—C2A—C7A119.5 (4)O5—C15—C16A107.1 (4)
C3A—C2A—C1A121.5 (4)O6—C15—C16B109.5 (12)
C7A—C2A—C1A118.8 (4)O5—C15—C16B105.9 (9)
C4A—C3A—C2A119.9 (4)O6—C15—H15111.2
C4A—C3A—H3A120.1O5—C15—H15111.2
C2A—C3A—H3A120.1C16A—C15—H15111.2
C5A—C4A—C3A120.4 (4)C15—C16A—C17A104.0 (5)
C5A—C4A—H4A119.8C15—C16A—H16A111.0
C3A—C4A—H4A119.8C17A—C16A—H16A111.0
C4A—C5A—C6A120.6 (3)C15—C16A—H16B111.0
C4A—C5A—H5A119.7C17A—C16A—H16B111.0
C6A—C5A—H5A119.7H16A—C16A—H16B109.0
C5A—C6A—C7A118.9 (4)C18—C17A—C16A104.2 (3)
C5A—C6A—H6A120.5C18—C17A—H17A110.9
C7A—C6A—H6A120.5C16A—C17A—H17A110.9
C6A—C7A—C2A120.6 (4)C18—C17A—H17B110.9
C6A—C7A—H7A119.7C16A—C17A—H17B110.9
C2A—C7A—H7A119.7H17A—C17A—H17B108.9
C3B—C2B—C7B122.3 (16)C17B—C16B—C15102.9 (12)
C3B—C2B—C1A115.6 (15)C17B—C16B—H16C111.2
C7B—C2B—C1A122.0 (16)C15—C16B—H16C111.2
C2B—C3B—C4B119.4 (14)C17B—C16B—H16D111.2
C2B—C3B—H3B120.3C15—C16B—H16D111.2
C4B—C3B—H3B120.3H16C—C16B—H16D109.1
C5B—C4B—C3B118.6 (12)C16B—C17B—C18101.5 (9)
C5B—C4B—H4B120.7C16B—C17B—H17C111.5
C3B—C4B—H4B120.7C18—C17B—H17C111.5
C4B—C5B—C6B121.1 (13)C16B—C17B—H17D111.5
C4B—C5B—H5B119.5C18—C17B—H17D111.5
C6B—C5B—H5B119.5H17C—C17B—H17D109.3
C5B—C6B—C7B121.2 (13)O5—C18—C17A102.7 (2)
C5B—C6B—H6B119.4O5—C18—C17B110.8 (4)
C7B—C6B—H6B119.4O5—C18—H18A111.2
C6B—C7B—C2B117.3 (13)C17A—C18—H18A111.2
C6B—C7B—H7B121.4O5—C18—H18B111.2
C2B—C7B—H7B121.4C17A—C18—H18B111.2
O4—C8A—O3125.51 (16)H18A—C18—H18B109.1
Symmetry codes: (i) x+1, y, z+1/2; (ii) x+3/2, y+1/2, z+1.
(4_corr) top
Crystal data top
C34H26MgN4O4F(000) = 1208
Mr = 578.90Dx = 1.361 Mg m3
Monoclinic, P21/nMo Kα radiation, λ = 0.71073 Å
a = 11.3068 (12) ÅCell parameters from 9953 reflections
b = 14.9595 (16) Åθ = 2.3–30.7°
c = 16.7252 (17) ŵ = 0.11 mm1
β = 93.0500 (15)°T = 100 K
V = 2825.0 (5) Å3Block
Z = 40.19 × 0.15 × 0.11 mm
Data collection top
Bruker Smart APEX II Ultra
diffractometer
8694 independent reflections
Radiation source: BRUKER Rotating Anode7486 reflections with I > 2σ(I)
ω scansθmax = 30.6°, θmin = 1.8°
Absorption correction: multi-scan
SADABS2015/1
h = 1616
Tmin = 0.688, Tmax = 0.746k = 021
8694 measured reflectionsl = 023
Refinement top
Refinement on F2408 restraints
Least-squares matrix: fullHydrogen site location: inferred from neighbouring sites
R[F2 > 2σ(F2)] = 0.040H-atom parameters constrained
wR(F2) = 0.109 w = 1/[σ2(Fo2) + (0.0572P)2 + 1.1587P]
where P = (Fo2 + 2Fc2)/3
S = 1.02(Δ/σ)max = 0.001
8694 reflectionsΔρmax = 0.53 e Å3
393 parametersΔρmin = 0.25 e Å3
Crystal data top
C34H26MgN4O4V = 2825.0 (5) Å3
Mr = 578.90Z = 4
Monoclinic, P21/nMo Kα radiation
a = 11.3068 (12) ŵ = 0.11 mm1
b = 14.9595 (16) ÅT = 100 K
c = 16.7252 (17) Å0.19 × 0.15 × 0.11 mm
β = 93.0500 (15)°
Data collection top
Bruker Smart APEX II Ultra
diffractometer
8694 measured reflections
Absorption correction: multi-scan
SADABS2015/1
8694 independent reflections
Tmin = 0.688, Tmax = 0.7467486 reflections with I > 2σ(I)
Refinement top
R[F2 > 2σ(F2)] = 0.040408 restraints
wR(F2) = 0.109H-atom parameters constrained
S = 1.02Δρmax = 0.53 e Å3
8694 reflectionsΔρmin = 0.25 e Å3
393 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. Refined as a 2-component twin.

Fractional atomic coordinates and isotropic or equivalent isotropic displacement parameters (Å2) top
xyzUiso*/Ueq
Mg010.27303 (3)0.33004 (2)0.35532 (2)0.01280 (8)
O0020.05820 (7)0.12031 (5)0.43101 (5)0.01754 (15)
O0030.36933 (7)0.59101 (5)0.42444 (5)0.01845 (15)
O0040.64247 (6)0.36193 (5)0.38294 (5)0.01863 (15)
O0050.02141 (7)0.25127 (5)0.17526 (5)0.02009 (16)
N0060.17719 (7)0.24066 (6)0.41889 (5)0.01393 (16)
N0070.45367 (7)0.31500 (6)0.35926 (5)0.01408 (16)
N0080.17564 (7)0.30678 (6)0.25064 (5)0.01439 (16)
N0090.27790 (8)0.46110 (6)0.39094 (5)0.01437 (16)
C00A0.09846 (9)0.18576 (6)0.38134 (6)0.01502 (18)
C00B0.18575 (9)0.21132 (6)0.49863 (6)0.01419 (17)
C00C0.24555 (9)0.24707 (7)0.56621 (6)0.01589 (18)
C00D0.53110 (9)0.24423 (7)0.34385 (6)0.01441 (18)
C00E0.16953 (9)0.35065 (7)0.17618 (6)0.01568 (18)
C00F0.19109 (9)0.52678 (7)0.40187 (6)0.01533 (18)
C00G0.38171 (9)0.50288 (6)0.40451 (6)0.01558 (18)
C00H0.52430 (9)0.38363 (7)0.38140 (6)0.01554 (18)
C00I0.08659 (9)0.24836 (7)0.24655 (6)0.01574 (18)
C00J0.50888 (9)0.15750 (7)0.31659 (6)0.01638 (18)
C00K0.24873 (10)0.60625 (7)0.42211 (6)0.01747 (19)
C00L0.11440 (9)0.13648 (7)0.50501 (6)0.01641 (19)
C00M0.05149 (9)0.18663 (7)0.30316 (6)0.01741 (19)
H00M0.00690.14350.28750.021*
C00N0.07359 (10)0.31671 (8)0.13094 (6)0.0194 (2)
C00O0.49687 (9)0.47091 (7)0.40126 (7)0.01804 (19)
H00O0.56030.51110.41330.022*
C00P0.64632 (9)0.27359 (7)0.35954 (6)0.01691 (19)
C00Q0.31476 (10)0.33241 (7)0.56302 (6)0.0189 (2)
H00A0.38370.32330.53080.028*
H00B0.34140.35020.61740.028*
H00C0.26440.37950.53870.028*
C00R0.06758 (10)0.52332 (7)0.39427 (6)0.0187 (2)
C00S0.74566 (10)0.22162 (8)0.35228 (7)0.0215 (2)
H00S0.82340.24340.36450.026*
C00T0.24330 (9)0.41462 (7)0.14515 (6)0.01751 (19)
C00U0.38542 (10)0.12440 (7)0.29747 (7)0.0212 (2)
H00D0.34780.16110.25480.032*
H00E0.33950.12840.34540.032*
H00F0.38830.06200.27970.032*
C00V0.10169 (11)0.08936 (7)0.57453 (7)0.0221 (2)
H00V0.05420.03710.57650.027*
C00W0.21198 (11)0.44281 (8)0.06727 (7)0.0231 (2)
H00W0.25980.48640.04320.028*
C00X0.19257 (11)0.68605 (7)0.43532 (7)0.0220 (2)
H00X0.23460.73910.45000.026*
C00Y0.23244 (10)0.20083 (8)0.63780 (6)0.0205 (2)
H00Y0.27190.22270.68540.025*
C00Z0.72358 (10)0.13471 (8)0.32567 (7)0.0232 (2)
H00Z0.78840.09530.31940.028*
C0100.60855 (10)0.10408 (7)0.30797 (7)0.0207 (2)
H0100.59770.04450.28930.025*
C0110.06969 (11)0.68338 (8)0.42566 (8)0.0255 (2)
H0110.02560.73660.43260.031*
C0120.00064 (10)0.43936 (8)0.37277 (8)0.0241 (2)
H01A0.01510.42260.31750.036*
H01B0.08430.44950.37780.036*
H01C0.02740.39110.40900.036*
C0130.34921 (10)0.45009 (8)0.19231 (7)0.0222 (2)
H01D0.39330.49050.15870.033*
H01E0.40040.40030.21010.033*
H01F0.32340.48270.23910.033*
C0140.00984 (10)0.60436 (8)0.40605 (8)0.0241 (2)
H0140.07420.60570.40040.029*
C0150.04090 (11)0.34451 (9)0.05433 (7)0.0260 (2)
H0150.02620.32090.02490.031*
C0160.16357 (11)0.12379 (8)0.64201 (7)0.0236 (2)
H0160.15870.09410.69200.028*
C0170.11320 (12)0.40952 (9)0.02343 (7)0.0272 (2)
H0170.09500.43190.02890.033*
Atomic displacement parameters (Å2) top
U11U22U33U12U13U23
Mg010.01083 (15)0.01178 (15)0.01581 (16)0.00159 (11)0.00077 (12)0.00026 (11)
O0020.0203 (4)0.0143 (3)0.0184 (3)0.0060 (3)0.0055 (3)0.0006 (3)
O0030.0183 (4)0.0118 (3)0.0253 (4)0.0002 (3)0.0005 (3)0.0024 (3)
O0040.0108 (3)0.0180 (3)0.0271 (4)0.0003 (3)0.0002 (3)0.0034 (3)
O0050.0176 (4)0.0245 (4)0.0178 (3)0.0051 (3)0.0029 (3)0.0010 (3)
N0060.0129 (4)0.0126 (4)0.0164 (4)0.0009 (3)0.0021 (3)0.0001 (3)
N0070.0127 (4)0.0126 (4)0.0169 (4)0.0003 (3)0.0005 (3)0.0006 (3)
N0080.0129 (4)0.0145 (4)0.0159 (4)0.0014 (3)0.0015 (3)0.0005 (3)
N0090.0137 (4)0.0127 (4)0.0168 (4)0.0011 (3)0.0019 (3)0.0005 (3)
C00A0.0132 (4)0.0125 (4)0.0198 (4)0.0020 (3)0.0048 (3)0.0002 (3)
C00B0.0141 (4)0.0118 (4)0.0171 (4)0.0010 (3)0.0048 (3)0.0003 (3)
C00C0.0147 (4)0.0145 (4)0.0186 (4)0.0006 (3)0.0020 (3)0.0005 (3)
C00D0.0128 (4)0.0158 (4)0.0147 (4)0.0014 (3)0.0018 (3)0.0009 (3)
C00E0.0158 (4)0.0167 (4)0.0145 (4)0.0006 (3)0.0011 (3)0.0000 (3)
C00F0.0176 (5)0.0131 (4)0.0155 (4)0.0024 (3)0.0032 (3)0.0014 (3)
C00G0.0182 (5)0.0113 (4)0.0173 (4)0.0006 (3)0.0009 (3)0.0004 (3)
C00H0.0109 (4)0.0170 (4)0.0186 (4)0.0006 (3)0.0000 (3)0.0001 (3)
C00I0.0127 (4)0.0173 (4)0.0171 (4)0.0007 (3)0.0000 (3)0.0025 (3)
C00J0.0166 (4)0.0161 (4)0.0166 (4)0.0002 (4)0.0029 (3)0.0007 (3)
C00K0.0191 (5)0.0150 (4)0.0185 (4)0.0012 (4)0.0025 (4)0.0006 (3)
C00L0.0182 (5)0.0131 (4)0.0184 (4)0.0011 (3)0.0052 (4)0.0024 (3)
C00M0.0146 (4)0.0172 (4)0.0204 (5)0.0051 (3)0.0008 (4)0.0013 (4)
C00N0.0173 (5)0.0224 (5)0.0184 (5)0.0020 (4)0.0001 (4)0.0005 (4)
C00O0.0145 (4)0.0144 (4)0.0251 (5)0.0026 (3)0.0001 (4)0.0024 (4)
C00P0.0144 (4)0.0172 (4)0.0193 (4)0.0003 (4)0.0013 (3)0.0007 (4)
C00Q0.0191 (5)0.0169 (4)0.0205 (5)0.0036 (4)0.0016 (4)0.0012 (4)
C00R0.0171 (5)0.0178 (5)0.0215 (5)0.0022 (4)0.0049 (4)0.0018 (4)
C00S0.0131 (4)0.0250 (5)0.0265 (5)0.0027 (4)0.0014 (4)0.0012 (4)
C00T0.0179 (5)0.0175 (5)0.0173 (4)0.0008 (4)0.0031 (4)0.0005 (3)
C00U0.0176 (5)0.0173 (5)0.0288 (5)0.0018 (4)0.0030 (4)0.0058 (4)
C00V0.0289 (6)0.0160 (5)0.0224 (5)0.0050 (4)0.0093 (4)0.0005 (4)
C00W0.0273 (6)0.0241 (5)0.0183 (5)0.0026 (4)0.0031 (4)0.0037 (4)
C00X0.0270 (6)0.0144 (5)0.0252 (5)0.0025 (4)0.0060 (4)0.0004 (4)
C00Y0.0237 (5)0.0202 (5)0.0178 (5)0.0014 (4)0.0021 (4)0.0007 (4)
C00Z0.0184 (5)0.0231 (5)0.0284 (5)0.0061 (4)0.0052 (4)0.0018 (4)
C0100.0213 (5)0.0172 (5)0.0236 (5)0.0032 (4)0.0035 (4)0.0024 (4)
C0110.0263 (6)0.0182 (5)0.0330 (6)0.0074 (4)0.0102 (5)0.0004 (4)
C0120.0156 (5)0.0214 (5)0.0357 (6)0.0005 (4)0.0034 (4)0.0012 (4)
C0130.0213 (5)0.0249 (5)0.0206 (5)0.0072 (4)0.0020 (4)0.0033 (4)
C0140.0191 (5)0.0220 (5)0.0320 (6)0.0060 (4)0.0076 (4)0.0017 (4)
C0150.0247 (6)0.0338 (6)0.0189 (5)0.0033 (5)0.0046 (4)0.0023 (4)
C0160.0323 (6)0.0200 (5)0.0191 (5)0.0032 (4)0.0068 (4)0.0035 (4)
C0170.0304 (6)0.0331 (6)0.0180 (5)0.0019 (5)0.0014 (4)0.0055 (4)
Geometric parameters (Å, º) top
Mg01—N0082.0480 (9)C00N—C0151.3788 (15)
Mg01—N0092.0490 (9)C00O—H00O0.9500
Mg01—N0072.0525 (9)C00P—C00S1.3766 (15)
Mg01—N0062.0531 (9)C00Q—H00A0.9800
O002—C00A1.3770 (12)C00Q—H00B0.9800
O002—C00L1.3821 (13)C00Q—H00C0.9800
O003—C00G1.3688 (12)C00R—C0141.3958 (15)
O003—C00K1.3811 (13)C00R—C0121.5003 (16)
O004—C00H1.3739 (12)C00S—C00Z1.3925 (17)
O004—C00P1.3796 (13)C00S—H00S0.9500
O005—C00I1.3686 (12)C00T—C00W1.3967 (15)
O005—C00N1.3793 (13)C00T—C0131.4957 (15)
N006—C00A1.3424 (13)C00U—H00D0.9800
N006—C00B1.4024 (13)C00U—H00E0.9800
N007—C00H1.3408 (13)C00U—H00F0.9800
N007—C00D1.4062 (13)C00V—C0161.3946 (17)
N008—C00I1.3322 (13)C00V—H00V0.9500
N008—C00E1.4061 (13)C00W—C0171.3949 (17)
N009—C00G1.3385 (13)C00W—H00W0.9500
N009—C00F1.4076 (13)C00X—C0111.3907 (17)
C00A—C00M1.3850 (14)C00X—H00X0.9500
C00B—C00L1.3873 (14)C00Y—C0161.3949 (16)
C00B—C00C1.3927 (14)C00Y—H00Y0.9500
C00C—C00Y1.3975 (14)C00Z—C0101.3958 (16)
C00C—C00Q1.4998 (14)C00Z—H00Z0.9500
C00D—C00P1.3866 (14)C010—H0100.9500
C00D—C00J1.3935 (14)C011—C0141.3926 (17)
C00E—C00N1.3855 (14)C011—H0110.9500
C00E—C00T1.3881 (14)C012—H01A0.9800
C00F—C00K1.3890 (14)C012—H01B0.9800
C00F—C00R1.3965 (15)C012—H01C0.9800
C00G—C00O1.3909 (15)C013—H01D0.9800
C00H—C00O1.3864 (14)C013—H01E0.9800
C00I—C00M1.3952 (14)C013—H01F0.9800
C00J—C0101.3953 (15)C014—H0140.9500
C00J—C00U1.4995 (15)C015—C0171.3879 (18)
C00K—C00X1.3755 (14)C015—H0150.9500
C00L—C00V1.3738 (15)C016—H0160.9500
C00M—H00M0.9500C017—H0170.9500
N008—Mg01—N009114.59 (4)C00S—C00P—C00D124.55 (10)
N008—Mg01—N007119.84 (4)O004—C00P—C00D108.28 (9)
N009—Mg01—N00794.84 (4)C00C—C00Q—H00A109.5
N008—Mg01—N00693.29 (4)C00C—C00Q—H00B109.5
N009—Mg01—N006118.64 (4)H00A—C00Q—H00B109.5
N007—Mg01—N006117.63 (4)C00C—C00Q—H00C109.5
C00A—O002—C00L105.36 (8)H00A—C00Q—H00C109.5
C00G—O003—C00K105.41 (8)H00B—C00Q—H00C109.5
C00H—O004—C00P105.45 (8)C014—C00R—C00F115.34 (10)
C00I—O005—C00N105.36 (8)C014—C00R—C012121.82 (10)
C00A—N006—C00B105.30 (8)C00F—C00R—C012122.82 (10)
C00A—N006—Mg01120.75 (7)C00P—C00S—C00Z114.98 (10)
C00B—N006—Mg01133.21 (7)C00P—C00S—H00S122.5
C00H—N007—C00D105.05 (8)C00Z—C00S—H00S122.5
C00H—N007—Mg01120.13 (7)C00E—C00T—C00W115.42 (10)
C00D—N007—Mg01134.82 (7)C00E—C00T—C013121.84 (9)
C00I—N008—C00E105.03 (8)C00W—C00T—C013122.74 (10)
C00I—N008—Mg01121.72 (7)C00J—C00U—H00D109.5
C00E—N008—Mg01132.59 (7)C00J—C00U—H00E109.5
C00G—N009—C00F105.27 (8)H00D—C00U—H00E109.5
C00G—N009—Mg01120.39 (7)C00J—C00U—H00F109.5
C00F—N009—Mg01134.23 (7)H00D—C00U—H00F109.5
N006—C00A—O002112.64 (9)H00E—C00U—H00F109.5
N006—C00A—C00M130.34 (9)C00L—C00V—C016115.15 (10)
O002—C00A—C00M116.99 (9)C00L—C00V—H00V122.4
C00L—C00B—C00C120.44 (9)C016—C00V—H00V122.4
C00L—C00B—N006108.35 (9)C017—C00W—C00T122.59 (11)
C00C—C00B—N006131.11 (9)C017—C00W—H00W118.7
C00B—C00C—C00Y115.86 (9)C00T—C00W—H00W118.7
C00B—C00C—C00Q121.99 (9)C00K—C00X—C011115.04 (11)
C00Y—C00C—C00Q122.08 (10)C00K—C00X—H00X122.5
C00P—C00D—C00J120.54 (9)C011—C00X—H00X122.5
C00P—C00D—N007108.34 (9)C016—C00Y—C00C122.49 (10)
C00J—C00D—N007131.12 (9)C016—C00Y—H00Y118.8
C00N—C00E—C00T121.14 (10)C00C—C00Y—H00Y118.8
C00N—C00E—N008108.22 (9)C00S—C00Z—C010121.56 (10)
C00T—C00E—N008130.59 (9)C00S—C00Z—H00Z119.2
C00K—C00F—C00R120.52 (10)C010—C00Z—H00Z119.2
C00K—C00F—N009107.92 (9)C00J—C010—C00Z122.59 (10)
C00R—C00F—N009131.55 (10)C00J—C010—H010118.7
N009—C00G—O003113.01 (9)C00Z—C010—H010118.7
N009—C00G—C00O130.32 (9)C00X—C011—C014121.45 (10)
O003—C00G—C00O116.67 (9)C00X—C011—H011119.3
N007—C00H—O004112.86 (9)C014—C011—H011119.3
N007—C00H—C00O130.53 (9)C00R—C012—H01A109.5
O004—C00H—C00O116.60 (9)C00R—C012—H01B109.5
N008—C00I—O005113.22 (9)H01A—C012—H01B109.5
N008—C00I—C00M129.85 (9)C00R—C012—H01C109.5
O005—C00I—C00M116.92 (9)H01A—C012—H01C109.5
C00D—C00J—C010115.75 (10)H01B—C012—H01C109.5
C00D—C00J—C00U121.79 (9)C00T—C013—H01D109.5
C010—C00J—C00U122.46 (10)C00T—C013—H01E109.5
C00X—C00K—O003127.03 (10)H01D—C013—H01E109.5
C00X—C00K—C00F124.57 (10)C00T—C013—H01F109.5
O003—C00K—C00F108.38 (9)H01D—C013—H01F109.5
C00V—C00L—O002127.18 (10)H01E—C013—H01F109.5
C00V—C00L—C00B124.52 (10)C011—C014—C00R123.05 (11)
O002—C00L—C00B108.29 (9)C011—C014—H014118.5
C00A—C00M—C00I122.57 (9)C00R—C014—H014118.5
C00A—C00M—H00M118.7C00N—C015—C017115.04 (11)
C00I—C00M—H00M118.7C00N—C015—H015122.5
C015—C00N—O005127.76 (10)C017—C015—H015122.5
C015—C00N—C00E124.08 (11)C00V—C016—C00Y121.45 (10)
O005—C00N—C00E108.15 (9)C00V—C016—H016119.3
C00H—C00O—C00G123.71 (9)C00Y—C016—H016119.3
C00H—C00O—H00O118.1C015—C017—C00W121.70 (11)
C00G—C00O—H00O118.1C015—C017—H017119.1
C00S—C00P—O004127.17 (10)C00W—C017—H017119.1
(4_filter) top
Crystal data top
C34H26MgN4O4F(000) = 1208
Mr = 578.90Dx = 1.357 Mg m3
Monoclinic, P21/nMo Kα radiation, λ = 0.71073 Å
a = 11.3182 (14) ÅCell parameters from 9930 reflections
b = 14.9745 (18) Åθ = 2.2–30.6°
c = 16.744 (2) ŵ = 0.11 mm1
β = 93.044 (2)°T = 100 K
V = 2833.9 (6) Å3Block
Z = 40.19 × 0.15 × 0.11 mm
Data collection top
Bruker Smart APEX II Ultra
diffractometer
7421 reflections with I > 2σ(I)
Radiation source: BRUKER Rotating AnodeRint = 0.031
ω scansθmax = 30.8°, θmin = 1.8°
Absorption correction: multi-scan
SADABS2015/1
h = 1616
Tmin = 0.679, Tmax = 0.746k = 2121
36495 measured reflectionsl = 2424
8866 independent reflections
Refinement top
Refinement on F2408 restraints
Least-squares matrix: fullHydrogen site location: inferred from neighbouring sites
R[F2 > 2σ(F2)] = 0.040H-atom parameters constrained
wR(F2) = 0.111 w = 1/[σ2(Fo2) + (0.0582P)2 + 0.8513P]
where P = (Fo2 + 2Fc2)/3
S = 1.03(Δ/σ)max < 0.001
8866 reflectionsΔρmax = 0.45 e Å3
392 parametersΔρmin = 0.26 e Å3
Crystal data top
C34H26MgN4O4V = 2833.9 (6) Å3
Mr = 578.90Z = 4
Monoclinic, P21/nMo Kα radiation
a = 11.3182 (14) ŵ = 0.11 mm1
b = 14.9745 (18) ÅT = 100 K
c = 16.744 (2) Å0.19 × 0.15 × 0.11 mm
β = 93.044 (2)°
Data collection top
Bruker Smart APEX II Ultra
diffractometer
8866 independent reflections
Absorption correction: multi-scan
SADABS2015/1
7421 reflections with I > 2σ(I)
Tmin = 0.679, Tmax = 0.746Rint = 0.031
36495 measured reflections
Refinement top
R[F2 > 2σ(F2)] = 0.040408 restraints
wR(F2) = 0.111H-atom parameters constrained
S = 1.03Δρmax = 0.45 e Å3
8866 reflectionsΔρmin = 0.26 e Å3
392 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
Mg010.27308 (3)0.33005 (2)0.35534 (2)0.01305 (8)
O0020.05821 (7)0.12026 (5)0.43094 (4)0.01763 (15)
O0030.36932 (7)0.59096 (5)0.42442 (5)0.01854 (15)
O0040.64246 (7)0.36195 (5)0.38294 (5)0.01880 (16)
O0050.02151 (7)0.25130 (5)0.17522 (5)0.02027 (16)
N0060.17719 (8)0.24073 (6)0.41883 (5)0.01414 (16)
N0070.45369 (8)0.31493 (6)0.35926 (5)0.01436 (16)
N0080.17556 (8)0.30673 (6)0.25062 (5)0.01442 (16)
N0090.27790 (8)0.46115 (6)0.39100 (5)0.01435 (16)
C00A0.09842 (9)0.18575 (6)0.38132 (6)0.01488 (18)
C00B0.24554 (9)0.24707 (7)0.56621 (6)0.01593 (19)
C00C0.18572 (9)0.21132 (7)0.49862 (6)0.01444 (18)
C00D0.53109 (9)0.24424 (7)0.34383 (6)0.01451 (18)
C00E0.52438 (9)0.38366 (7)0.38137 (6)0.01551 (18)
C00F0.08657 (9)0.24837 (7)0.24648 (6)0.01584 (19)
C00G0.19122 (9)0.52685 (7)0.40182 (6)0.01565 (19)
C00H0.38175 (9)0.50281 (6)0.40460 (6)0.01554 (19)
C00I0.16944 (9)0.35062 (7)0.17617 (6)0.01600 (19)
C00J0.24870 (10)0.60625 (7)0.42200 (6)0.01741 (19)
C00K0.50887 (9)0.15751 (7)0.31656 (6)0.01665 (19)
C00L0.05149 (9)0.18672 (7)0.30318 (6)0.01742 (19)
H00L0.00690.14370.28750.021*
C00M0.49681 (9)0.47082 (7)0.40122 (7)0.0182 (2)
H00M0.56020.51110.41320.022*
C00N0.11442 (9)0.13650 (7)0.50502 (6)0.01636 (19)
C00O0.07358 (10)0.31670 (8)0.13092 (6)0.0195 (2)
C00P0.64636 (9)0.27364 (7)0.35964 (6)0.01691 (19)
C00Q0.06765 (10)0.52335 (7)0.39426 (6)0.0187 (2)
C00R0.31472 (10)0.33236 (7)0.56297 (6)0.0192 (2)
H00A0.26450.37930.53850.029*
H00B0.38370.32320.53100.029*
H00C0.34110.35030.61730.029*
C00S0.24327 (10)0.41469 (7)0.14517 (6)0.01762 (19)
C00T0.74561 (10)0.22166 (8)0.35229 (7)0.0218 (2)
H00T0.82330.24340.36440.026*
C00U0.38554 (10)0.12434 (7)0.29750 (7)0.0213 (2)
H00D0.38850.06210.27970.032*
H00E0.34780.16110.25490.032*
H00F0.33970.12820.34540.032*
C00V0.10169 (11)0.08934 (7)0.57452 (7)0.0224 (2)
H00V0.05420.03720.57650.027*
C00W0.23229 (10)0.20076 (8)0.63776 (6)0.0208 (2)
H00W0.27160.22270.68530.025*
C00X0.21204 (11)0.44285 (8)0.06726 (7)0.0232 (2)
H00X0.25990.48630.04320.028*
C00Y0.19263 (11)0.68599 (7)0.43525 (7)0.0223 (2)
H00Y0.23470.73890.44990.027*
C00Z0.60864 (10)0.10419 (7)0.30801 (7)0.0209 (2)
H00Z0.59790.04470.28940.025*
C0100.06969 (11)0.68337 (8)0.42565 (8)0.0259 (2)
H0100.02570.73660.43260.031*
C0110.72346 (10)0.13474 (8)0.32575 (7)0.0232 (2)
H0110.78810.09530.31960.028*
C0120.00060 (10)0.43936 (8)0.37285 (8)0.0241 (2)
H01A0.01480.42260.31760.036*
H01B0.08420.44960.37800.036*
H01C0.02740.39110.40900.036*
C0130.34922 (10)0.45013 (8)0.19225 (7)0.0221 (2)
H01D0.39310.49060.15870.033*
H01E0.40050.40040.20980.033*
H01F0.32350.48260.23910.033*
C0140.16369 (11)0.12372 (8)0.64197 (7)0.0239 (2)
H0140.15900.09400.69180.029*
C0150.00983 (11)0.60425 (8)0.40605 (7)0.0241 (2)
H0150.07410.60550.40050.029*
C0160.04091 (11)0.34450 (9)0.05432 (7)0.0262 (2)
H0160.02600.32090.02490.031*
C0170.11321 (12)0.40959 (9)0.02339 (7)0.0275 (2)
H0170.09490.43200.02890.033*
Atomic displacement parameters (Å2) top
U11U22U33U12U13U23
Mg010.01099 (16)0.01193 (16)0.01623 (16)0.00143 (12)0.00078 (12)0.00025 (12)
O0020.0201 (4)0.0145 (3)0.0187 (3)0.0060 (3)0.0052 (3)0.0007 (3)
O0030.0180 (4)0.0119 (3)0.0257 (4)0.0003 (3)0.0004 (3)0.0025 (3)
O0040.0113 (3)0.0175 (4)0.0274 (4)0.0007 (3)0.0003 (3)0.0032 (3)
O0050.0179 (4)0.0248 (4)0.0178 (3)0.0051 (3)0.0027 (3)0.0012 (3)
N0060.0128 (4)0.0125 (4)0.0172 (4)0.0008 (3)0.0018 (3)0.0001 (3)
N0070.0131 (4)0.0129 (4)0.0170 (4)0.0001 (3)0.0004 (3)0.0005 (3)
N0080.0126 (4)0.0142 (4)0.0165 (4)0.0015 (3)0.0013 (3)0.0004 (3)
N0090.0134 (4)0.0123 (4)0.0174 (4)0.0009 (3)0.0018 (3)0.0003 (3)
C00A0.0131 (4)0.0122 (4)0.0197 (4)0.0017 (3)0.0048 (3)0.0006 (3)
C00B0.0143 (4)0.0143 (4)0.0193 (5)0.0004 (3)0.0022 (4)0.0003 (3)
C00C0.0144 (4)0.0120 (4)0.0174 (4)0.0013 (3)0.0049 (3)0.0003 (3)
C00D0.0127 (4)0.0156 (4)0.0153 (4)0.0010 (3)0.0015 (3)0.0009 (3)
C00E0.0107 (4)0.0167 (4)0.0192 (4)0.0006 (3)0.0006 (3)0.0004 (3)
C00F0.0128 (4)0.0172 (4)0.0174 (4)0.0003 (3)0.0000 (3)0.0022 (3)
C00G0.0177 (5)0.0136 (4)0.0159 (4)0.0028 (3)0.0031 (3)0.0018 (3)
C00H0.0188 (5)0.0108 (4)0.0169 (4)0.0011 (3)0.0003 (4)0.0003 (3)
C00I0.0158 (5)0.0171 (4)0.0152 (4)0.0010 (4)0.0009 (3)0.0003 (3)
C00J0.0184 (5)0.0150 (4)0.0190 (4)0.0012 (4)0.0028 (4)0.0008 (3)
C00K0.0169 (5)0.0162 (4)0.0170 (4)0.0005 (4)0.0026 (4)0.0006 (3)
C00L0.0150 (5)0.0163 (4)0.0209 (5)0.0045 (4)0.0006 (4)0.0014 (4)
C00M0.0151 (5)0.0140 (4)0.0254 (5)0.0029 (4)0.0005 (4)0.0024 (4)
C00N0.0179 (5)0.0130 (4)0.0186 (4)0.0009 (4)0.0054 (4)0.0026 (3)
C00O0.0170 (5)0.0225 (5)0.0189 (5)0.0019 (4)0.0001 (4)0.0005 (4)
C00P0.0146 (5)0.0162 (4)0.0199 (4)0.0005 (4)0.0008 (4)0.0009 (4)
C00Q0.0176 (5)0.0174 (5)0.0214 (5)0.0017 (4)0.0045 (4)0.0019 (4)
C00R0.0196 (5)0.0176 (5)0.0201 (5)0.0035 (4)0.0014 (4)0.0009 (4)
C00S0.0180 (5)0.0175 (5)0.0175 (4)0.0001 (4)0.0025 (4)0.0005 (4)
C00T0.0134 (5)0.0245 (5)0.0276 (5)0.0027 (4)0.0016 (4)0.0012 (4)
C00U0.0180 (5)0.0172 (5)0.0289 (5)0.0018 (4)0.0026 (4)0.0054 (4)
C00V0.0295 (6)0.0159 (5)0.0227 (5)0.0048 (4)0.0092 (4)0.0003 (4)
C00W0.0233 (5)0.0209 (5)0.0183 (5)0.0007 (4)0.0019 (4)0.0009 (4)
C00X0.0276 (6)0.0237 (5)0.0186 (5)0.0025 (4)0.0030 (4)0.0038 (4)
C00Y0.0272 (6)0.0145 (5)0.0257 (5)0.0027 (4)0.0061 (4)0.0003 (4)
C00Z0.0217 (5)0.0176 (5)0.0238 (5)0.0037 (4)0.0035 (4)0.0021 (4)
C0100.0268 (6)0.0177 (5)0.0339 (6)0.0073 (4)0.0097 (5)0.0001 (4)
C0110.0185 (5)0.0224 (5)0.0291 (6)0.0066 (4)0.0050 (4)0.0015 (4)
C0120.0155 (5)0.0209 (5)0.0360 (6)0.0004 (4)0.0039 (4)0.0007 (4)
C0130.0209 (5)0.0248 (5)0.0206 (5)0.0070 (4)0.0021 (4)0.0034 (4)
C0140.0323 (6)0.0202 (5)0.0198 (5)0.0031 (4)0.0064 (4)0.0036 (4)
C0150.0184 (5)0.0226 (5)0.0320 (6)0.0055 (4)0.0075 (4)0.0011 (4)
C0160.0240 (6)0.0336 (6)0.0203 (5)0.0033 (5)0.0043 (4)0.0026 (4)
C0170.0315 (6)0.0325 (6)0.0183 (5)0.0017 (5)0.0015 (4)0.0060 (4)
Geometric parameters (Å, º) top
Mg01—N0082.0516 (9)C00N—C00V1.3753 (15)
Mg01—N0092.0518 (9)C00O—C0161.3802 (15)
Mg01—N0062.0542 (9)C00P—C00T1.3775 (15)
Mg01—N0072.0543 (10)C00Q—C0151.3958 (15)
O002—C00A1.3781 (12)C00Q—C0121.5025 (16)
O002—C00N1.3852 (13)C00R—H00A0.9800
O003—C00H1.3701 (12)C00R—H00B0.9800
O003—C00J1.3827 (13)C00R—H00C0.9800
O004—C00E1.3743 (12)C00S—C00X1.3985 (15)
O004—C00P1.3801 (13)C00S—C0131.4968 (15)
O005—C00F1.3692 (12)C00T—C0111.3937 (17)
O005—C00O1.3795 (13)C00T—H00T0.9500
N006—C00A1.3446 (13)C00U—H00D0.9800
N006—C00C1.4052 (13)C00U—H00E0.9800
N007—C00E1.3435 (13)C00U—H00F0.9800
N007—C00D1.4067 (13)C00V—C0141.3960 (17)
N008—C00F1.3325 (13)C00V—H00V0.9500
N008—C00I1.4076 (13)C00W—C0141.3945 (16)
N009—C00H1.3395 (13)C00W—H00W0.9500
N009—C00G1.4078 (13)C00X—C0171.3970 (17)
C00A—C00L1.3857 (14)C00X—H00X0.9500
C00B—C00C1.3944 (14)C00Y—C0101.3928 (18)
C00B—C00W1.3991 (15)C00Y—H00Y0.9500
C00B—C00R1.5006 (15)C00Z—C0111.3947 (16)
C00C—C00N1.3882 (14)C00Z—H00Z0.9500
C00D—C00P1.3890 (14)C010—C0151.3953 (17)
C00D—C00K1.3951 (14)C010—H0100.9500
C00E—C00M1.3865 (14)C011—H0110.9500
C00F—C00L1.3970 (14)C012—H01A0.9800
C00G—C00J1.3884 (15)C012—H01B0.9800
C00G—C00Q1.3986 (15)C012—H01C0.9800
C00H—C00M1.3916 (15)C013—H01D0.9800
C00I—C00O1.3863 (15)C013—H01E0.9800
C00I—C00S1.3908 (15)C013—H01F0.9800
C00J—C00Y1.3758 (15)C014—H0140.9500
C00K—C00Z1.3965 (15)C015—H0150.9500
C00K—C00U1.5000 (15)C016—C0171.3902 (18)
C00L—H00L0.9500C016—H0160.9500
C00M—H00M0.9500C017—H0170.9500
N008—Mg01—N009114.60 (4)C00T—C00P—C00D124.47 (10)
N008—Mg01—N00693.24 (4)O004—C00P—C00D108.28 (9)
N009—Mg01—N006118.62 (4)C015—C00Q—C00G115.39 (10)
N008—Mg01—N007119.85 (4)C015—C00Q—C012121.71 (10)
N009—Mg01—N00794.88 (4)C00G—C00Q—C012122.88 (10)
N006—Mg01—N007117.64 (4)C00B—C00R—H00A109.5
C00A—O002—C00N105.33 (8)C00B—C00R—H00B109.5
C00H—O003—C00J105.45 (8)H00A—C00R—H00B109.5
C00E—O004—C00P105.48 (8)C00B—C00R—H00C109.5
C00F—O005—C00O105.42 (8)H00A—C00R—H00C109.5
C00A—N006—C00C105.22 (8)H00B—C00R—H00C109.5
C00A—N006—Mg01120.82 (7)C00I—C00S—C00X115.41 (10)
C00C—N006—Mg01133.21 (7)C00I—C00S—C013121.90 (9)
C00E—N007—C00D105.04 (8)C00X—C00S—C013122.69 (10)
C00E—N007—Mg01120.09 (7)C00P—C00T—C011114.99 (10)
C00D—N007—Mg01134.86 (7)C00P—C00T—H00T122.5
C00F—N008—C00I104.99 (8)C011—C00T—H00T122.5
C00F—N008—Mg01121.80 (7)C00K—C00U—H00D109.5
C00I—N008—Mg01132.56 (7)C00K—C00U—H00E109.5
C00H—N009—C00G105.30 (8)H00D—C00U—H00E109.5
C00H—N009—Mg01120.31 (7)C00K—C00U—H00F109.5
C00G—N009—Mg01134.28 (7)H00D—C00U—H00F109.5
N006—C00A—O002112.71 (9)H00E—C00U—H00F109.5
N006—C00A—C00L130.25 (9)C00N—C00V—C014115.12 (10)
O002—C00A—C00L117.02 (9)C00N—C00V—H00V122.4
C00C—C00B—C00W115.79 (10)C014—C00V—H00V122.4
C00C—C00B—C00R121.95 (9)C014—C00W—C00B122.59 (10)
C00W—C00B—C00R122.19 (10)C014—C00W—H00W118.7
C00N—C00C—C00B120.43 (9)C00B—C00W—H00W118.7
C00N—C00C—N006108.39 (9)C017—C00X—C00S122.59 (11)
C00B—C00C—N006131.08 (9)C017—C00X—H00X118.7
C00P—C00D—C00K120.57 (9)C00S—C00X—H00X118.7
C00P—C00D—N007108.32 (9)C00J—C00Y—C010115.06 (11)
C00K—C00D—N007131.11 (9)C00J—C00Y—H00Y122.5
N007—C00E—O004112.85 (9)C010—C00Y—H00Y122.5
N007—C00E—C00M130.46 (10)C011—C00Z—C00K122.68 (10)
O004—C00E—C00M116.69 (9)C011—C00Z—H00Z118.7
N008—C00F—O005113.23 (9)C00K—C00Z—H00Z118.7
N008—C00F—C00L129.75 (9)C00Y—C010—C015121.38 (10)
O005—C00F—C00L117.02 (9)C00Y—C010—H010119.3
C00J—C00G—C00Q120.49 (10)C015—C010—H010119.3
C00J—C00G—N009108.00 (9)C00T—C011—C00Z121.60 (10)
C00Q—C00G—N009131.49 (10)C00T—C011—H011119.2
N009—C00H—O003112.92 (9)C00Z—C011—H011119.2
N009—C00H—C00M130.34 (9)C00Q—C012—H01A109.5
O003—C00H—C00M116.74 (9)C00Q—C012—H01B109.5
C00O—C00I—C00S121.14 (10)H01A—C012—H01B109.5
C00O—C00I—N008108.26 (9)C00Q—C012—H01C109.5
C00S—C00I—N008130.56 (9)H01A—C012—H01C109.5
C00Y—C00J—O003127.03 (10)H01B—C012—H01C109.5
C00Y—C00J—C00G124.63 (11)C00S—C013—H01D109.5
O003—C00J—C00G108.32 (9)C00S—C013—H01E109.5
C00D—C00K—C00Z115.66 (10)H01D—C013—H01E109.5
C00D—C00K—C00U121.84 (9)C00S—C013—H01F109.5
C00Z—C00K—C00U122.50 (10)H01D—C013—H01F109.5
C00A—C00L—C00F122.69 (9)H01E—C013—H01F109.5
C00A—C00L—H00L118.7C00W—C014—C00V121.43 (10)
C00F—C00L—H00L118.7C00W—C014—H014119.3
C00E—C00M—C00H123.84 (9)C00V—C014—H014119.3
C00E—C00M—H00M118.1C010—C015—C00Q123.01 (11)
C00H—C00M—H00M118.1C010—C015—H015118.5
C00V—C00N—O002127.14 (10)C00Q—C015—H015118.5
C00V—C00N—C00C124.55 (10)C00O—C016—C017115.07 (11)
O002—C00N—C00C108.29 (9)C00O—C016—H016122.5
O005—C00O—C016127.79 (10)C017—C016—H016122.5
O005—C00O—C00I108.09 (9)C016—C017—C00X121.66 (11)
C016—C00O—C00I124.10 (11)C016—C017—H017119.2
C00T—C00P—O004127.25 (10)C00X—C017—H017119.2
(4_uncorr) top
Crystal data top
C34H26MgN4O4F(000) = 1208
Mr = 578.90Dx = 1.361 Mg m3
Monoclinic, P21/nMo Kα radiation, λ = 0.71073 Å
a = 11.3068 (12) ÅCell parameters from 9953 reflections
b = 14.9595 (16) Åθ = 2.3–30.7°
c = 16.7252 (17) ŵ = 0.11 mm1
β = 93.0500 (15)°T = 100 K
V = 2825.0 (5) Å3Block
Z = 40.19 × 0.15 × 0.11 mm
Data collection top
Bruker Smart APEX II Ultra
diffractometer
7463 reflections with I > 2σ(I)
Radiation source: BRUKER Rotating AnodeRint = 0.027
ω scansθmax = 30.6°, θmin = 1.8°
Absorption correction: multi-scan
SADABS2015/1
h = 1616
Tmin = 0.688, Tmax = 0.746k = 2121
36155 measured reflectionsl = 2323
8694 independent reflections
Refinement top
Refinement on F2408 restraints
Least-squares matrix: fullHydrogen site location: inferred from neighbouring sites
R[F2 > 2σ(F2)] = 0.041H-atom parameters constrained
wR(F2) = 0.115 w = 1/[σ2(Fo2) + (0.0609P)2 + 1.1405P]
where P = (Fo2 + 2Fc2)/3
S = 1.03(Δ/σ)max = 0.001
8694 reflectionsΔρmax = 0.53 e Å3
392 parametersΔρmin = 0.25 e Å3
Crystal data top
C34H26MgN4O4V = 2825.0 (5) Å3
Mr = 578.90Z = 4
Monoclinic, P21/nMo Kα radiation
a = 11.3068 (12) ŵ = 0.11 mm1
b = 14.9595 (16) ÅT = 100 K
c = 16.7252 (17) Å0.19 × 0.15 × 0.11 mm
β = 93.0500 (15)°
Data collection top
Bruker Smart APEX II Ultra
diffractometer
8694 independent reflections
Absorption correction: multi-scan
SADABS2015/1
7463 reflections with I > 2σ(I)
Tmin = 0.688, Tmax = 0.746Rint = 0.027
36155 measured reflections
Refinement top
R[F2 > 2σ(F2)] = 0.041408 restraints
wR(F2) = 0.115H-atom parameters constrained
S = 1.03Δρmax = 0.53 e Å3
8694 reflectionsΔρmin = 0.25 e Å3
392 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
Mg010.27304 (3)0.33006 (2)0.35532 (2)0.01282 (8)
O0020.05823 (7)0.12031 (5)0.43100 (5)0.01756 (16)
O0030.36933 (7)0.59101 (5)0.42443 (5)0.01842 (16)
O0040.64249 (7)0.36193 (5)0.38293 (5)0.01856 (16)
O0050.02145 (7)0.25129 (6)0.17528 (5)0.02010 (17)
N0060.17714 (8)0.24066 (6)0.41890 (5)0.01395 (16)
N0070.45364 (8)0.31500 (6)0.35925 (5)0.01412 (16)
N0080.17567 (8)0.30678 (6)0.25060 (5)0.01442 (17)
N0090.27788 (8)0.46112 (6)0.39094 (5)0.01437 (16)
C00A0.09843 (9)0.18575 (7)0.38137 (6)0.01504 (19)
C00B0.18576 (9)0.21131 (7)0.49862 (6)0.01418 (18)
C00C0.24554 (9)0.24709 (7)0.56622 (6)0.01587 (19)
C00D0.53114 (9)0.24422 (7)0.34386 (6)0.01442 (18)
C00E0.16958 (9)0.35065 (7)0.17615 (6)0.01568 (19)
C00F0.19106 (9)0.52678 (7)0.40185 (6)0.01533 (19)
C00G0.38172 (10)0.50288 (7)0.40452 (6)0.01553 (19)
C00H0.52429 (9)0.38365 (7)0.38140 (6)0.01557 (19)
C00I0.08660 (9)0.24836 (7)0.24657 (6)0.01573 (19)
C00J0.50888 (10)0.15747 (7)0.31658 (6)0.01644 (19)
C00K0.24873 (10)0.60626 (7)0.42212 (6)0.0175 (2)
C00L0.11442 (10)0.13650 (7)0.50502 (6)0.01637 (19)
C00M0.05154 (10)0.18665 (7)0.30319 (7)0.0174 (2)
H00M0.00680.14350.28750.021*
C00N0.07366 (10)0.31672 (8)0.13093 (7)0.0195 (2)
C00O0.49685 (10)0.47089 (7)0.40126 (7)0.0180 (2)
H00O0.56030.51110.41330.022*
C00P0.64633 (9)0.27356 (7)0.35952 (6)0.01693 (19)
C00Q0.31478 (10)0.33239 (7)0.56302 (7)0.0189 (2)
H00A0.38350.32340.53060.028*
H00B0.34180.35000.61740.028*
H00C0.26430.37950.53900.028*
C00R0.06758 (10)0.52331 (8)0.39428 (7)0.0187 (2)
C00S0.74561 (10)0.22163 (8)0.35228 (7)0.0215 (2)
H00S0.82340.24340.36450.026*
C00T0.24327 (10)0.41464 (7)0.14515 (6)0.0175 (2)
C00U0.38538 (10)0.12438 (8)0.29754 (7)0.0212 (2)
H00D0.34780.16090.25470.032*
H00E0.33940.12870.34540.032*
H00F0.38820.06190.28010.032*
C00V0.10166 (11)0.08936 (8)0.57452 (7)0.0222 (2)
H00V0.05420.03710.57650.027*
C00W0.21199 (11)0.44284 (8)0.06727 (7)0.0232 (2)
H00W0.25990.48640.04320.028*
C00X0.19251 (11)0.68604 (8)0.43533 (7)0.0220 (2)
H00X0.23450.73910.45000.026*
C00Y0.23248 (11)0.20082 (8)0.63779 (7)0.0206 (2)
H00Y0.27210.22260.68540.025*
C00Z0.72351 (11)0.13471 (8)0.32568 (8)0.0231 (2)
H00Z0.78830.09530.31940.028*
C0100.60862 (10)0.10410 (8)0.30797 (7)0.0207 (2)
H0100.59780.04450.28930.025*
C0110.06969 (12)0.68337 (8)0.42565 (8)0.0256 (2)
H0110.02560.73660.43250.031*
C0120.00064 (10)0.43935 (8)0.37273 (8)0.0242 (2)
H01A0.01490.42270.31740.036*
H01B0.08420.44950.37790.036*
H01C0.02750.39100.40890.036*
C0130.34921 (11)0.45009 (8)0.19236 (7)0.0222 (2)
H01D0.39330.49050.15870.033*
H01E0.40040.40020.21010.033*
H01F0.32330.48270.23910.033*
C0140.00987 (11)0.60432 (8)0.40609 (8)0.0242 (2)
H0140.07420.60560.40050.029*
C0150.04086 (12)0.34453 (9)0.05432 (7)0.0260 (2)
H0150.02620.32090.02490.031*
C0160.16354 (12)0.12381 (8)0.64201 (7)0.0237 (2)
H0160.15860.09420.69200.028*
C0170.11313 (12)0.40953 (9)0.02346 (7)0.0273 (3)
H0170.09480.43200.02890.033*
Atomic displacement parameters (Å2) top
U11U22U33U12U13U23
Mg010.01087 (16)0.01179 (16)0.01580 (16)0.00154 (12)0.00073 (12)0.00024 (12)
O0020.0203 (4)0.0144 (3)0.0184 (4)0.0059 (3)0.0055 (3)0.0005 (3)
O0030.0182 (4)0.0118 (3)0.0251 (4)0.0003 (3)0.0005 (3)0.0023 (3)
O0040.0106 (3)0.0180 (4)0.0270 (4)0.0003 (3)0.0003 (3)0.0034 (3)
O0050.0176 (4)0.0245 (4)0.0178 (4)0.0050 (3)0.0028 (3)0.0009 (3)
N0060.0129 (4)0.0127 (4)0.0164 (4)0.0009 (3)0.0022 (3)0.0000 (3)
N0070.0127 (4)0.0127 (4)0.0169 (4)0.0002 (3)0.0005 (3)0.0006 (3)
N0080.0129 (4)0.0145 (4)0.0159 (4)0.0015 (3)0.0015 (3)0.0005 (3)
N0090.0136 (4)0.0127 (4)0.0170 (4)0.0010 (3)0.0018 (3)0.0005 (3)
C00A0.0132 (4)0.0126 (4)0.0198 (5)0.0020 (3)0.0050 (4)0.0002 (3)
C00B0.0142 (4)0.0118 (4)0.0169 (4)0.0009 (3)0.0047 (3)0.0003 (3)
C00C0.0146 (4)0.0145 (4)0.0187 (5)0.0005 (3)0.0019 (4)0.0006 (4)
C00D0.0128 (4)0.0159 (4)0.0146 (4)0.0014 (3)0.0018 (3)0.0010 (3)
C00E0.0158 (5)0.0168 (4)0.0145 (4)0.0008 (4)0.0011 (3)0.0000 (3)
C00F0.0177 (5)0.0132 (4)0.0154 (4)0.0024 (4)0.0032 (4)0.0014 (3)
C00G0.0181 (5)0.0113 (4)0.0172 (4)0.0007 (3)0.0009 (4)0.0004 (3)
C00H0.0109 (4)0.0171 (5)0.0186 (5)0.0006 (3)0.0001 (3)0.0003 (4)
C00I0.0127 (4)0.0172 (5)0.0172 (4)0.0006 (4)0.0001 (3)0.0025 (4)
C00J0.0167 (5)0.0161 (4)0.0167 (4)0.0003 (4)0.0029 (4)0.0007 (4)
C00K0.0191 (5)0.0152 (5)0.0184 (5)0.0012 (4)0.0027 (4)0.0008 (4)
C00L0.0181 (5)0.0132 (4)0.0183 (5)0.0010 (4)0.0052 (4)0.0024 (3)
C00M0.0146 (5)0.0171 (5)0.0205 (5)0.0051 (4)0.0007 (4)0.0014 (4)
C00N0.0174 (5)0.0224 (5)0.0186 (5)0.0021 (4)0.0002 (4)0.0005 (4)
C00O0.0146 (5)0.0146 (5)0.0247 (5)0.0027 (4)0.0001 (4)0.0024 (4)
C00P0.0147 (5)0.0170 (5)0.0192 (5)0.0003 (4)0.0013 (4)0.0006 (4)
C00Q0.0190 (5)0.0171 (5)0.0203 (5)0.0035 (4)0.0016 (4)0.0012 (4)
C00R0.0172 (5)0.0179 (5)0.0214 (5)0.0022 (4)0.0049 (4)0.0018 (4)
C00S0.0132 (5)0.0248 (5)0.0267 (5)0.0026 (4)0.0014 (4)0.0011 (4)
C00T0.0179 (5)0.0176 (5)0.0172 (5)0.0007 (4)0.0029 (4)0.0004 (4)
C00U0.0175 (5)0.0173 (5)0.0290 (6)0.0018 (4)0.0029 (4)0.0058 (4)
C00V0.0290 (6)0.0159 (5)0.0225 (5)0.0049 (4)0.0093 (4)0.0003 (4)
C00W0.0275 (6)0.0242 (5)0.0180 (5)0.0027 (4)0.0030 (4)0.0036 (4)
C00X0.0272 (6)0.0144 (5)0.0249 (5)0.0025 (4)0.0060 (4)0.0003 (4)
C00Y0.0236 (5)0.0202 (5)0.0182 (5)0.0015 (4)0.0020 (4)0.0006 (4)
C00Z0.0185 (5)0.0231 (5)0.0280 (6)0.0061 (4)0.0051 (4)0.0017 (4)
C0100.0216 (5)0.0170 (5)0.0236 (5)0.0031 (4)0.0035 (4)0.0023 (4)
C0110.0264 (6)0.0182 (5)0.0331 (6)0.0072 (4)0.0102 (5)0.0004 (4)
C0120.0155 (5)0.0214 (5)0.0357 (6)0.0005 (4)0.0034 (4)0.0013 (5)
C0130.0214 (5)0.0249 (5)0.0205 (5)0.0073 (4)0.0020 (4)0.0033 (4)
C0140.0189 (5)0.0221 (5)0.0323 (6)0.0060 (4)0.0077 (4)0.0018 (4)
C0150.0248 (6)0.0336 (6)0.0191 (5)0.0035 (5)0.0045 (4)0.0024 (5)
C0160.0322 (6)0.0201 (5)0.0193 (5)0.0032 (4)0.0067 (4)0.0035 (4)
C0170.0303 (6)0.0330 (6)0.0182 (5)0.0019 (5)0.0014 (4)0.0055 (5)
Geometric parameters (Å, º) top
Mg01—N0082.0484 (9)C00N—C0151.3791 (16)
Mg01—N0092.0490 (10)C00O—H00O0.9500
Mg01—N0072.0521 (10)C00P—C00S1.3757 (15)
Mg01—N0062.0536 (9)C00Q—H00A0.9800
O002—C00A1.3761 (12)C00Q—H00B0.9800
O002—C00L1.3825 (13)C00Q—H00C0.9800
O003—C00G1.3689 (12)C00R—C0141.3955 (16)
O003—C00K1.3811 (14)C00R—C0121.5005 (16)
O004—C00H1.3743 (13)C00S—C00Z1.3926 (17)
O004—C00P1.3801 (13)C00S—H00S0.9500
O005—C00I1.3685 (13)C00T—C00W1.3967 (15)
O005—C00N1.3795 (14)C00T—C0131.4963 (16)
N006—C00A1.3421 (13)C00U—H00D0.9800
N006—C00B1.4023 (13)C00U—H00E0.9800
N007—C00H1.3411 (13)C00U—H00F0.9800
N007—C00D1.4067 (13)C00V—C0161.3946 (17)
N008—C00I1.3324 (13)C00V—H00V0.9500
N008—C00E1.4061 (13)C00W—C0171.3954 (18)
N009—C00G1.3386 (14)C00W—H00W0.9500
N009—C00F1.4074 (13)C00X—C0111.3902 (18)
C00A—C00M1.3847 (15)C00X—H00X0.9500
C00B—C00L1.3870 (14)C00Y—C0161.3948 (16)
C00B—C00C1.3929 (15)C00Y—H00Y0.9500
C00C—C00Y1.3975 (15)C00Z—C0101.3942 (17)
C00C—C00Q1.4994 (15)C00Z—H00Z0.9500
C00D—C00P1.3861 (14)C010—H0100.9500
C00D—C00J1.3941 (15)C011—C0141.3926 (18)
C00E—C00N1.3851 (15)C011—H0110.9500
C00E—C00T1.3875 (15)C012—H01A0.9800
C00F—C00K1.3893 (15)C012—H01B0.9800
C00F—C00R1.3961 (15)C012—H01C0.9800
C00G—C00O1.3907 (15)C013—H01D0.9800
C00H—C00O1.3860 (15)C013—H01E0.9800
C00I—C00M1.3950 (15)C013—H01F0.9800
C00J—C0101.3954 (15)C014—H0140.9500
C00J—C00U1.4997 (15)C015—C0171.3874 (18)
C00K—C00X1.3756 (15)C015—H0150.9500
C00L—C00V1.3737 (15)C016—H0160.9500
C00M—H00M0.9500C017—H0170.9500
N008—Mg01—N009114.59 (4)C00S—C00P—C00D124.58 (10)
N008—Mg01—N007119.83 (4)O004—C00P—C00D108.27 (9)
N009—Mg01—N00794.85 (4)C00C—C00Q—H00A109.5
N008—Mg01—N00693.29 (4)C00C—C00Q—H00B109.5
N009—Mg01—N006118.64 (4)H00A—C00Q—H00B109.5
N007—Mg01—N006117.63 (4)C00C—C00Q—H00C109.5
C00A—O002—C00L105.35 (8)H00A—C00Q—H00C109.5
C00G—O003—C00K105.42 (8)H00B—C00Q—H00C109.5
C00H—O004—C00P105.45 (8)C014—C00R—C00F115.33 (11)
C00I—O005—C00N105.38 (8)C014—C00R—C012121.82 (10)
C00A—N006—C00B105.29 (9)C00F—C00R—C012122.83 (10)
C00A—N006—Mg01120.78 (7)C00P—C00S—C00Z114.96 (11)
C00B—N006—Mg01133.18 (7)C00P—C00S—H00S122.5
C00H—N007—C00D105.02 (9)C00Z—C00S—H00S122.5
C00H—N007—Mg01120.12 (7)C00E—C00T—C00W115.44 (10)
C00D—N007—Mg01134.85 (7)C00E—C00T—C013121.81 (10)
C00I—N008—C00E105.07 (9)C00W—C00T—C013122.75 (10)
C00I—N008—Mg01121.68 (7)C00J—C00U—H00D109.5
C00E—N008—Mg01132.58 (7)C00J—C00U—H00E109.5
C00G—N009—C00F105.30 (9)H00D—C00U—H00E109.5
C00G—N009—Mg01120.36 (7)C00J—C00U—H00F109.5
C00F—N009—Mg01134.22 (7)H00D—C00U—H00F109.5
N006—C00A—O002112.67 (9)H00E—C00U—H00F109.5
N006—C00A—C00M130.29 (10)C00L—C00V—C016115.11 (10)
O002—C00A—C00M117.03 (9)C00L—C00V—H00V122.4
C00L—C00B—C00C120.43 (10)C016—C00V—H00V122.4
C00L—C00B—N006108.34 (9)C017—C00W—C00T122.54 (11)
C00C—C00B—N006131.12 (10)C017—C00W—H00W118.7
C00B—C00C—C00Y115.85 (10)C00T—C00W—H00W118.7
C00B—C00C—C00Q122.00 (10)C00K—C00X—C011115.06 (11)
C00Y—C00C—C00Q122.09 (10)C00K—C00X—H00X122.5
C00P—C00D—C00J120.53 (10)C011—C00X—H00X122.5
C00P—C00D—N007108.38 (9)C016—C00Y—C00C122.49 (11)
C00J—C00D—N007131.08 (10)C016—C00Y—H00Y118.8
C00N—C00E—C00T121.14 (10)C00C—C00Y—H00Y118.8
C00N—C00E—N008108.21 (9)C00S—C00Z—C010121.59 (11)
C00T—C00E—N008130.61 (10)C00S—C00Z—H00Z119.2
C00K—C00F—C00R120.53 (10)C010—C00Z—H00Z119.2
C00K—C00F—N009107.90 (9)C00Z—C010—C00J122.62 (11)
C00R—C00F—N009131.56 (10)C00Z—C010—H010118.7
N009—C00G—O003112.99 (9)C00J—C010—H010118.7
N009—C00G—C00O130.33 (10)C00X—C011—C014121.43 (11)
O003—C00G—C00O116.68 (9)C00X—C011—H011119.3
N007—C00H—O004112.86 (9)C014—C011—H011119.3
N007—C00H—C00O130.52 (10)C00R—C012—H01A109.5
O004—C00H—C00O116.62 (9)C00R—C012—H01B109.5
N008—C00I—O005113.17 (9)H01A—C012—H01B109.5
N008—C00I—C00M129.86 (10)C00R—C012—H01C109.5
O005—C00I—C00M116.96 (9)H01A—C012—H01C109.5
C00D—C00J—C010115.70 (10)H01B—C012—H01C109.5
C00D—C00J—C00U121.77 (10)C00T—C013—H01D109.5
C010—C00J—C00U122.52 (10)C00T—C013—H01E109.5
C00X—C00K—O003127.07 (10)H01D—C013—H01E109.5
C00X—C00K—C00F124.53 (11)C00T—C013—H01F109.5
O003—C00K—C00F108.39 (9)H01D—C013—H01F109.5
C00V—C00L—O002127.15 (10)H01E—C013—H01F109.5
C00V—C00L—C00B124.55 (10)C011—C014—C00R123.08 (11)
O002—C00L—C00B108.28 (9)C011—C014—H014118.5
C00A—C00M—C00I122.63 (10)C00R—C014—H014118.5
C00A—C00M—H00M118.7C00N—C015—C017115.00 (11)
C00I—C00M—H00M118.7C00N—C015—H015122.5
C015—C00N—O005127.73 (11)C017—C015—H015122.5
C015—C00N—C00E124.11 (11)C00V—C016—C00Y121.46 (11)
O005—C00N—C00E108.16 (9)C00V—C016—H016119.3
C00H—C00O—C00G123.73 (10)C00Y—C016—H016119.3
C00H—C00O—H00O118.1C015—C017—C00W121.74 (11)
C00G—C00O—H00O118.1C015—C017—H017119.1
C00S—C00P—O004127.16 (10)C00W—C017—H017119.1
(5_corr) top
Crystal data top
C11H10O2SDx = 1.381 Mg m3
Mr = 206.25Mo Kα radiation, λ = 0.71073 Å
Orthorhombic, P212121Cell parameters from 9037 reflections
a = 5.9633 (1) Åθ = 2.5–28.3°
b = 9.0417 (2) ŵ = 0.29 mm1
c = 18.4007 (4) ÅT = 293 K
V = 992.14 (3) Å3Sphere
Z = 40.25 mm (radius)
F(000) = 432
Data collection top
Bruker Smart APEX II Quazar
diffractometer
2456 independent reflections
Radiation source: INCOATEC Microsource2398 reflections with I > 2σ(I)
ω scansθmax = 28.3°, θmin = 2.2°
Absorption correction: multi-scan
SADABS2015/1
h = 77
Tmin = 0.710, Tmax = 0.746k = 012
2456 measured reflectionsl = 024
Refinement top
Refinement on F2Hydrogen site location: inferred from neighbouring sites
Least-squares matrix: fullH-atom parameters constrained
R[F2 > 2σ(F2)] = 0.025 w = 1/[σ2(Fo2) + (0.0398P)2 + 0.0978P]
where P = (Fo2 + 2Fc2)/3
wR(F2) = 0.067(Δ/σ)max = 0.001
S = 1.08Δρmax = 0.22 e Å3
2456 reflectionsΔρmin = 0.18 e Å3
130 parametersAbsolute structure: Flack x determined using 978 quotients [(I+)-(I-)]/[(I+)+(I-)] (Parsons, Flack and Wagner, Acta Cryst. B69 (2013) 249-259).
0 restraintsAbsolute structure parameter: 0.035 (15)
Crystal data top
C11H10O2SV = 992.14 (3) Å3
Mr = 206.25Z = 4
Orthorhombic, P212121Mo Kα radiation
a = 5.9633 (1) ŵ = 0.29 mm1
b = 9.0417 (2) ÅT = 293 K
c = 18.4007 (4) Å0.25 mm (radius)
Data collection top
Bruker Smart APEX II Quazar
diffractometer
2456 measured reflections
Absorption correction: multi-scan
SADABS2015/1
2456 independent reflections
Tmin = 0.710, Tmax = 0.7462398 reflections with I > 2σ(I)
Refinement top
R[F2 > 2σ(F2)] = 0.025H-atom parameters constrained
wR(F2) = 0.067Δρmax = 0.22 e Å3
S = 1.08Δρmin = 0.18 e Å3
2456 reflectionsAbsolute structure: Flack x determined using 978 quotients [(I+)-(I-)]/[(I+)+(I-)] (Parsons, Flack and Wagner, Acta Cryst. B69 (2013) 249-259).
130 parametersAbsolute structure parameter: 0.035 (15)
0 restraints
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. Refined as a 2-component twin.

Fractional atomic coordinates and isotropic or equivalent isotropic displacement parameters (Å2) top
xyzUiso*/Ueq
S10.80979 (7)0.31840 (4)0.25958 (2)0.03544 (12)
O10.3354 (2)0.19756 (15)0.32298 (7)0.0471 (3)
O20.8421 (3)0.58922 (14)0.37066 (7)0.0492 (3)
C0040.6893 (3)0.49876 (17)0.37460 (8)0.0345 (3)
C0050.3581 (3)0.38583 (18)0.41745 (9)0.0347 (3)
C0060.4328 (3)0.30465 (18)0.35007 (9)0.0336 (3)
C0070.5099 (3)0.49840 (18)0.43199 (9)0.0360 (4)
C0080.6356 (3)0.37592 (18)0.32789 (8)0.0336 (3)
C0090.1764 (4)0.3594 (2)0.46185 (10)0.0457 (4)
H0090.07540.28370.45180.055*
C00A0.4860 (4)0.5876 (2)0.49258 (10)0.0477 (5)
H00A0.58900.66170.50310.057*
C00B0.1497 (4)0.4507 (2)0.52253 (11)0.0543 (5)
H00B0.02800.43600.55330.065*
C00C0.8351 (4)0.12269 (19)0.27103 (11)0.0455 (4)
H00C0.68850.07910.27290.068*
H00D0.91360.10210.31550.068*
H00E0.91700.08180.23080.068*
C00D0.2993 (5)0.5614 (2)0.53755 (10)0.0568 (6)
H00F0.27710.62050.57830.068*
C00E0.6496 (5)0.3242 (3)0.17717 (10)0.0576 (5)
H00G0.62760.42520.16280.086*
H00H0.50660.27810.18500.086*
H00I0.72870.27230.13960.086*
Atomic displacement parameters (Å2) top
U11U22U33U12U13U23
S10.0377 (2)0.03170 (19)0.03691 (19)0.00493 (16)0.00840 (15)0.00391 (15)
O10.0407 (6)0.0466 (7)0.0541 (7)0.0099 (6)0.0018 (6)0.0120 (6)
O20.0569 (8)0.0418 (7)0.0490 (7)0.0160 (6)0.0079 (7)0.0088 (5)
C0040.0423 (8)0.0288 (7)0.0324 (7)0.0006 (8)0.0017 (7)0.0002 (5)
C0050.0371 (8)0.0340 (8)0.0330 (7)0.0072 (6)0.0027 (6)0.0026 (6)
C0060.0331 (7)0.0331 (8)0.0348 (7)0.0023 (7)0.0007 (6)0.0001 (6)
C0070.0472 (10)0.0300 (7)0.0308 (7)0.0047 (7)0.0036 (7)0.0029 (6)
C0080.0368 (8)0.0322 (7)0.0317 (7)0.0004 (6)0.0036 (6)0.0038 (6)
C0090.0433 (9)0.0485 (10)0.0452 (9)0.0046 (9)0.0086 (8)0.0037 (7)
C00A0.0705 (13)0.0367 (9)0.0358 (8)0.0015 (9)0.0063 (9)0.0029 (7)
C00B0.0620 (13)0.0550 (11)0.0457 (10)0.0124 (10)0.0235 (10)0.0068 (9)
C00C0.0459 (9)0.0327 (8)0.0580 (10)0.0082 (8)0.0119 (9)0.0010 (7)
C00D0.0879 (16)0.0459 (10)0.0365 (9)0.0136 (12)0.0180 (11)0.0007 (7)
C00E0.0850 (16)0.0534 (11)0.0345 (8)0.0048 (12)0.0058 (9)0.0027 (8)
Geometric parameters (Å, º) top
S1—C0081.7114 (16)C009—H0090.9300
S1—C00C1.7885 (17)C00A—C00D1.407 (3)
S1—C00E1.793 (2)C00A—H00A0.9300
O1—C0061.234 (2)C00B—C00D1.369 (3)
O2—C0041.226 (2)C00B—H00B0.9300
C004—C0081.440 (2)C00C—H00C0.9600
C004—C0071.503 (2)C00C—H00D0.9600
C005—C0091.378 (3)C00C—H00E0.9600
C005—C0071.388 (2)C00D—H00F0.9300
C005—C0061.508 (2)C00E—H00G0.9600
C006—C0081.430 (2)C00E—H00H0.9600
C007—C00A1.383 (2)C00E—H00I0.9600
C009—C00B1.398 (3)
C008—S1—C00C105.40 (9)C007—C00A—C00D117.25 (19)
C008—S1—C00E106.79 (10)C007—C00A—H00A121.4
C00C—S1—C00E99.98 (10)C00D—C00A—H00A121.4
O2—C004—C008130.08 (15)C00D—C00B—C009121.27 (19)
O2—C004—C007124.86 (15)C00D—C00B—H00B119.4
C008—C004—C007105.04 (14)C009—C00B—H00B119.4
C009—C005—C007121.73 (16)S1—C00C—H00C109.5
C009—C005—C006129.43 (17)S1—C00C—H00D109.5
C007—C005—C006108.82 (14)H00C—C00C—H00D109.5
O1—C006—C008129.52 (16)S1—C00C—H00E109.5
O1—C006—C005125.09 (16)H00C—C00C—H00E109.5
C008—C006—C005105.37 (14)H00D—C00C—H00E109.5
C00A—C007—C005121.02 (16)C00B—C00D—C00A121.30 (18)
C00A—C007—C004129.68 (17)C00B—C00D—H00F119.3
C005—C007—C004109.29 (14)C00A—C00D—H00F119.3
C006—C008—C004111.41 (14)S1—C00E—H00G109.5
C006—C008—S1125.87 (13)S1—C00E—H00H109.5
C004—C008—S1122.53 (12)H00G—C00E—H00H109.5
C005—C009—C00B117.4 (2)S1—C00E—H00I109.5
C005—C009—H009121.3H00G—C00E—H00I109.5
C00B—C009—H009121.3H00H—C00E—H00I109.5
C009—C005—C006—O10.8 (3)O2—C004—C008—C006176.12 (17)
C007—C005—C006—O1179.25 (17)C007—C004—C008—C0062.63 (19)
C009—C005—C006—C008177.80 (18)O2—C004—C008—S18.6 (3)
C007—C005—C006—C0080.68 (17)C007—C004—C008—S1172.70 (12)
C009—C005—C007—C00A0.9 (3)C00C—S1—C008—C00643.83 (18)
C006—C005—C007—C00A177.73 (16)C00E—S1—C008—C00661.89 (17)
C009—C005—C007—C004179.54 (16)C00C—S1—C008—C004130.80 (15)
C006—C005—C007—C0040.92 (18)C00E—S1—C008—C004123.48 (15)
O2—C004—C007—C00A4.8 (3)C007—C005—C009—C00B0.1 (3)
C008—C004—C007—C00A176.34 (18)C006—C005—C009—C00B178.41 (17)
O2—C004—C007—C005176.68 (17)C005—C007—C00A—C00D1.4 (3)
C008—C004—C007—C0052.15 (18)C004—C007—C00A—C00D179.77 (18)
O1—C006—C008—C004179.40 (18)C005—C009—C00B—C00D0.5 (3)
C005—C006—C008—C0042.10 (18)C009—C00B—C00D—C00A0.1 (3)
O1—C006—C008—S15.5 (3)C007—C00A—C00D—C00B1.0 (3)
C005—C006—C008—S1173.04 (12)
(5_filter) top
Crystal data top
C11H10O2SDx = 1.380 Mg m3
Mr = 206.25Mo Kα radiation, λ = 0.71073 Å
Orthorhombic, P212121Cell parameters from 8709 reflections
a = 5.9641 (2) Åθ = 2.5–28.3°
b = 9.0419 (2) ŵ = 0.29 mm1
c = 18.4027 (5) ÅT = 293 K
V = 992.40 (5) Å3Sphere
Z = 40.25 mm (radius)
F(000) = 432
Data collection top
Bruker Smart APEX II Quazar
diffractometer
2383 reflections with I > 2σ(I)
Radiation source: INCOATEC MicrosourceRint = 0.020
ω scansθmax = 28.3°, θmin = 2.2°
Absorption correction: multi-scan
SADABS2015/1
h = 77
Tmin = 0.712, Tmax = 0.746k = 1212
15101 measured reflectionsl = 2424
2453 independent reflections
Refinement top
Refinement on F2Hydrogen site location: inferred from neighbouring sites
Least-squares matrix: fullH-atom parameters constrained
R[F2 > 2σ(F2)] = 0.025 w = 1/[σ2(Fo2) + (0.0389P)2 + 0.0898P]
where P = (Fo2 + 2Fc2)/3
wR(F2) = 0.067(Δ/σ)max < 0.001
S = 1.11Δρmax = 0.21 e Å3
2453 reflectionsΔρmin = 0.19 e Å3
129 parametersAbsolute structure: Flack x determined using 969 quotients [(I+)-(I-)]/[(I+)+(I-)] (Parsons, Flack and Wagner, Acta Cryst. B69 (2013) 249-259).
0 restraintsAbsolute structure parameter: 0.049 (16)
Crystal data top
C11H10O2SV = 992.40 (5) Å3
Mr = 206.25Z = 4
Orthorhombic, P212121Mo Kα radiation
a = 5.9641 (2) ŵ = 0.29 mm1
b = 9.0419 (2) ÅT = 293 K
c = 18.4027 (5) Å0.25 mm (radius)
Data collection top
Bruker Smart APEX II Quazar
diffractometer
2453 independent reflections
Absorption correction: multi-scan
SADABS2015/1
2383 reflections with I > 2σ(I)
Tmin = 0.712, Tmax = 0.746Rint = 0.020
15101 measured reflections
Refinement top
R[F2 > 2σ(F2)] = 0.025H-atom parameters constrained
wR(F2) = 0.067Δρmax = 0.21 e Å3
S = 1.11Δρmin = 0.19 e Å3
2453 reflectionsAbsolute structure: Flack x determined using 969 quotients [(I+)-(I-)]/[(I+)+(I-)] (Parsons, Flack and Wagner, Acta Cryst. B69 (2013) 249-259).
129 parametersAbsolute structure parameter: 0.049 (16)
0 restraints
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
S10.80982 (7)0.31844 (4)0.25959 (2)0.03555 (12)
O10.3355 (2)0.19755 (15)0.32294 (7)0.0474 (3)
O20.8421 (3)0.58923 (15)0.37071 (7)0.0493 (3)
C0040.6894 (3)0.49883 (17)0.37462 (8)0.0344 (3)
C0050.3579 (3)0.38572 (18)0.41750 (9)0.0349 (3)
C0060.4329 (3)0.30487 (19)0.35004 (9)0.0338 (3)
C0070.5099 (3)0.49824 (19)0.43200 (9)0.0360 (4)
C0080.6358 (3)0.37592 (18)0.32793 (8)0.0338 (3)
C0090.1766 (4)0.3593 (2)0.46190 (10)0.0457 (4)
H0090.07580.28350.45190.055*
C00A0.4861 (4)0.5876 (2)0.49256 (10)0.0479 (5)
H00A0.58900.66180.50310.057*
C00B0.1498 (4)0.4507 (2)0.52251 (11)0.0544 (6)
H00B0.02790.43620.55320.065*
C00C0.8352 (4)0.12279 (19)0.27102 (11)0.0460 (4)
H00C0.68860.07920.27270.069*
H00D0.91320.10220.31550.069*
H00E0.91750.08200.23090.069*
C00D0.2996 (5)0.5613 (2)0.53753 (10)0.0566 (6)
H00F0.27760.62030.57830.068*
C00E0.6498 (5)0.3242 (3)0.17716 (10)0.0577 (5)
H00G0.62900.42520.16260.086*
H00H0.50630.27880.18510.086*
H00I0.72850.27160.13970.086*
Atomic displacement parameters (Å2) top
U11U22U33U12U13U23
S10.0378 (2)0.03167 (19)0.03714 (19)0.00497 (17)0.00837 (16)0.00396 (15)
O10.0412 (7)0.0467 (7)0.0543 (7)0.0101 (7)0.0019 (6)0.0118 (6)
O20.0569 (8)0.0414 (7)0.0495 (7)0.0159 (7)0.0084 (7)0.0082 (5)
C0040.0425 (8)0.0289 (7)0.0318 (7)0.0007 (8)0.0010 (7)0.0002 (5)
C0050.0371 (8)0.0343 (8)0.0332 (7)0.0071 (7)0.0027 (6)0.0030 (6)
C0060.0327 (8)0.0336 (8)0.0350 (7)0.0026 (7)0.0010 (6)0.0001 (7)
C0070.0479 (10)0.0298 (8)0.0304 (7)0.0048 (7)0.0035 (7)0.0027 (6)
C0080.0373 (8)0.0328 (7)0.0314 (7)0.0002 (6)0.0033 (6)0.0040 (6)
C0090.0426 (9)0.0487 (10)0.0457 (9)0.0045 (9)0.0083 (8)0.0040 (7)
C00A0.0715 (13)0.0361 (9)0.0360 (9)0.0012 (9)0.0063 (9)0.0037 (7)
C00B0.0625 (13)0.0549 (12)0.0458 (10)0.0120 (11)0.0236 (10)0.0068 (9)
C00C0.0457 (10)0.0331 (8)0.0591 (11)0.0081 (8)0.0122 (9)0.0005 (8)
C00D0.0879 (16)0.0456 (10)0.0365 (9)0.0139 (12)0.0187 (11)0.0005 (8)
C00E0.0863 (16)0.0522 (11)0.0345 (8)0.0045 (13)0.0053 (9)0.0024 (8)
Geometric parameters (Å, º) top
S1—C0081.7116 (16)C009—H0090.9300
S1—C00C1.7879 (18)C00A—C00D1.406 (3)
S1—C00E1.793 (2)C00A—H00A0.9300
O1—C0061.236 (2)C00B—C00D1.369 (3)
O2—C0041.226 (2)C00B—H00B0.9300
C004—C0081.441 (2)C00C—H00C0.9600
C004—C0071.503 (2)C00C—H00D0.9600
C005—C0091.376 (3)C00C—H00E0.9600
C005—C0071.389 (2)C00D—H00F0.9300
C005—C0061.509 (2)C00E—H00G0.9600
C006—C0081.429 (2)C00E—H00H0.9600
C007—C00A1.384 (2)C00E—H00I0.9600
C009—C00B1.397 (3)
C008—S1—C00C105.39 (9)C007—C00A—C00D117.2 (2)
C008—S1—C00E106.86 (10)C007—C00A—H00A121.4
C00C—S1—C00E99.97 (11)C00D—C00A—H00A121.4
O2—C004—C008130.10 (15)C00D—C00B—C009121.21 (19)
O2—C004—C007124.93 (15)C00D—C00B—H00B119.4
C008—C004—C007104.96 (14)C009—C00B—H00B119.4
C009—C005—C007121.73 (16)S1—C00C—H00C109.5
C009—C005—C006129.62 (17)S1—C00C—H00D109.5
C007—C005—C006108.64 (14)H00C—C00C—H00D109.5
O1—C006—C008129.51 (16)S1—C00C—H00E109.5
O1—C006—C005124.95 (16)H00C—C00C—H00E109.5
C008—C006—C005105.51 (14)H00D—C00C—H00E109.5
C00A—C007—C005121.02 (17)C00B—C00D—C00A121.36 (18)
C00A—C007—C004129.55 (17)C00B—C00D—H00F119.3
C005—C007—C004109.41 (14)C00A—C00D—H00F119.3
C006—C008—C004111.40 (14)S1—C00E—H00G109.5
C006—C008—S1125.89 (13)S1—C00E—H00H109.5
C004—C008—S1122.54 (13)H00G—C00E—H00H109.5
C005—C009—C00B117.5 (2)S1—C00E—H00I109.5
C005—C009—H009121.3H00G—C00E—H00I109.5
C00B—C009—H009121.3H00H—C00E—H00I109.5
C009—C005—C006—O10.7 (3)O2—C004—C008—C006176.07 (18)
C007—C005—C006—O1179.15 (17)C007—C004—C008—C0062.77 (19)
C009—C005—C006—C008177.70 (18)O2—C004—C008—S18.4 (3)
C007—C005—C006—C0080.79 (18)C007—C004—C008—S1172.72 (12)
C009—C005—C007—C00A0.8 (3)C00C—S1—C008—C00643.97 (18)
C006—C005—C007—C00A177.84 (16)C00E—S1—C008—C00661.77 (18)
C009—C005—C007—C004179.53 (16)C00C—S1—C008—C004130.85 (15)
C006—C005—C007—C0040.90 (18)C00E—S1—C008—C004123.42 (16)
O2—C004—C007—C00A4.7 (3)C007—C005—C009—C00B0.2 (3)
C008—C004—C007—C00A176.38 (19)C006—C005—C009—C00B178.54 (17)
O2—C004—C007—C005176.70 (17)C005—C007—C00A—C00D1.3 (3)
C008—C004—C007—C0052.22 (18)C004—C007—C00A—C00D179.77 (18)
O1—C006—C008—C004179.47 (18)C005—C009—C00B—C00D0.7 (3)
C005—C006—C008—C0042.26 (18)C009—C00B—C00D—C00A0.1 (3)
O1—C006—C008—S15.2 (3)C007—C00A—C00D—C00B0.9 (3)
C005—C006—C008—S1173.04 (13)
(5_uncorr) top
Crystal data top
C11H10O2SDx = 1.381 Mg m3
Mr = 206.25Mo Kα radiation, λ = 0.71073 Å
Orthorhombic, P212121Cell parameters from 9037 reflections
a = 5.9633 (1) Åθ = 2.5–28.3°
b = 9.0417 (2) ŵ = 0.29 mm1
c = 18.4007 (4) ÅT = 293 K
V = 992.14 (3) Å3Sphere
Z = 40.25 mm (radius)
F(000) = 432
Data collection top
Bruker Smart APEX II Quazar
diffractometer
2397 reflections with I > 2σ(I)
Radiation source: INCOATEC MicrosourceRint = 0.020
ω scansθmax = 28.3°, θmin = 2.2°
Absorption correction: multi-scan
SADABS2015/1
h = 77
Tmin = 0.710, Tmax = 0.746k = 1212
15091 measured reflectionsl = 2424
2456 independent reflections
Refinement top
Refinement on F2Hydrogen site location: inferred from neighbouring sites
Least-squares matrix: fullH-atom parameters constrained
R[F2 > 2σ(F2)] = 0.025 w = 1/[σ2(Fo2) + (0.0392P)2 + 0.1061P]
where P = (Fo2 + 2Fc2)/3
wR(F2) = 0.068(Δ/σ)max < 0.001
S = 1.09Δρmax = 0.22 e Å3
2456 reflectionsΔρmin = 0.20 e Å3
129 parametersAbsolute structure: Flack x determined using 976 quotients [(I+)-(I-)]/[(I+)+(I-)] (Parsons, Flack and Wagner, Acta Cryst. B69 (2013) 249-259).
0 restraintsAbsolute structure parameter: 0.034 (14)
Crystal data top
C11H10O2SV = 992.14 (3) Å3
Mr = 206.25Z = 4
Orthorhombic, P212121Mo Kα radiation
a = 5.9633 (1) ŵ = 0.29 mm1
b = 9.0417 (2) ÅT = 293 K
c = 18.4007 (4) Å0.25 mm (radius)
Data collection top
Bruker Smart APEX II Quazar
diffractometer
2456 independent reflections
Absorption correction: multi-scan
SADABS2015/1
2397 reflections with I > 2σ(I)
Tmin = 0.710, Tmax = 0.746Rint = 0.020
15091 measured reflections
Refinement top
R[F2 > 2σ(F2)] = 0.025H-atom parameters constrained
wR(F2) = 0.068Δρmax = 0.22 e Å3
S = 1.09Δρmin = 0.20 e Å3
2456 reflectionsAbsolute structure: Flack x determined using 976 quotients [(I+)-(I-)]/[(I+)+(I-)] (Parsons, Flack and Wagner, Acta Cryst. B69 (2013) 249-259).
129 parametersAbsolute structure parameter: 0.034 (14)
0 restraints
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
S10.80978 (7)0.31840 (4)0.25958 (2)0.03544 (12)
O10.3354 (2)0.19755 (15)0.32298 (8)0.0473 (3)
O20.8420 (3)0.58921 (15)0.37067 (7)0.0492 (3)
C0040.6893 (3)0.49880 (18)0.37460 (9)0.0345 (3)
C0050.3580 (3)0.38579 (19)0.41747 (9)0.0346 (3)
C0060.4327 (3)0.30467 (19)0.35007 (9)0.0337 (3)
C0070.5102 (3)0.49836 (19)0.43199 (9)0.0359 (4)
C0080.6356 (3)0.37590 (18)0.32792 (9)0.0337 (3)
C0090.1767 (4)0.3594 (2)0.46188 (10)0.0457 (4)
H0090.07590.28360.45190.055*
C00A0.4859 (4)0.5875 (2)0.49258 (10)0.0478 (5)
H00A0.58880.66170.50320.057*
C00B0.1496 (4)0.4507 (2)0.52255 (11)0.0542 (6)
H00B0.02770.43600.55330.065*
C00C0.8351 (4)0.1227 (2)0.27098 (11)0.0457 (4)
H00C0.68840.07920.27290.069*
H00D0.91370.10210.31540.069*
H00E0.91680.08180.23080.069*
C00D0.2993 (5)0.5614 (2)0.53756 (10)0.0569 (6)
H00F0.27720.62050.57830.068*
C00E0.6495 (5)0.3240 (3)0.17716 (10)0.0577 (6)
H00G0.62730.42510.16280.087*
H00H0.50660.27790.18500.087*
H00I0.72870.27220.13960.087*
Atomic displacement parameters (Å2) top
U11U22U33U12U13U23
S10.0377 (2)0.03168 (19)0.03696 (19)0.00496 (17)0.00844 (16)0.00390 (15)
O10.0409 (7)0.0469 (7)0.0541 (7)0.0101 (7)0.0019 (6)0.0120 (6)
O20.0570 (8)0.0415 (7)0.0491 (7)0.0157 (7)0.0081 (7)0.0086 (6)
C0040.0422 (8)0.0288 (7)0.0323 (7)0.0008 (8)0.0013 (7)0.0001 (6)
C0050.0369 (9)0.0341 (8)0.0328 (7)0.0072 (7)0.0028 (6)0.0025 (6)
C0060.0330 (8)0.0332 (8)0.0348 (7)0.0025 (7)0.0005 (6)0.0002 (7)
C0070.0473 (10)0.0299 (8)0.0306 (8)0.0045 (7)0.0036 (7)0.0029 (6)
C0080.0370 (8)0.0324 (7)0.0317 (7)0.0003 (6)0.0035 (6)0.0038 (6)
C0090.0432 (9)0.0486 (10)0.0453 (9)0.0046 (9)0.0085 (9)0.0038 (7)
C00A0.0710 (14)0.0366 (9)0.0358 (9)0.0016 (9)0.0065 (9)0.0028 (7)
C00B0.0619 (13)0.0554 (12)0.0454 (10)0.0122 (11)0.0231 (10)0.0071 (9)
C00C0.0460 (10)0.0328 (8)0.0583 (11)0.0086 (8)0.0116 (9)0.0012 (8)
C00D0.0882 (17)0.0457 (10)0.0367 (9)0.0132 (13)0.0185 (11)0.0009 (8)
C00E0.0852 (16)0.0534 (11)0.0344 (9)0.0051 (13)0.0056 (10)0.0026 (9)
Geometric parameters (Å, º) top
S1—C0081.7118 (17)C009—H0090.9300
S1—C00C1.7882 (18)C00A—C00D1.407 (3)
S1—C00E1.793 (2)C00A—H00A0.9300
O1—C0061.234 (2)C00B—C00D1.370 (4)
O2—C0041.226 (2)C00B—H00B0.9300
C004—C0081.441 (2)C00C—H00C0.9600
C004—C0071.502 (2)C00C—H00D0.9600
C005—C0091.376 (3)C00C—H00E0.9600
C005—C0071.389 (3)C00D—H00F0.9300
C005—C0061.508 (2)C00E—H00G0.9600
C006—C0081.430 (2)C00E—H00H0.9600
C007—C00A1.383 (3)C00E—H00I0.9600
C009—C00B1.398 (3)
C008—S1—C00C105.40 (9)C007—C00A—C00D117.3 (2)
C008—S1—C00E106.81 (10)C007—C00A—H00A121.3
C00C—S1—C00E99.93 (11)C00D—C00A—H00A121.3
O2—C004—C008130.12 (16)C00D—C00B—C009121.1 (2)
O2—C004—C007124.86 (15)C00D—C00B—H00B119.4
C008—C004—C007105.01 (14)C009—C00B—H00B119.4
C009—C005—C007121.73 (16)S1—C00C—H00C109.5
C009—C005—C006129.51 (17)S1—C00C—H00D109.5
C007—C005—C006108.75 (14)H00C—C00C—H00D109.5
O1—C006—C008129.52 (16)S1—C00C—H00E109.5
O1—C006—C005125.08 (16)H00C—C00C—H00E109.5
C008—C006—C005105.39 (14)H00D—C00C—H00E109.5
C00A—C007—C005120.89 (17)C00B—C00D—C00A121.31 (18)
C00A—C007—C004129.75 (18)C00B—C00D—H00F119.3
C005—C007—C004109.35 (14)C00A—C00D—H00F119.3
C006—C008—C004111.44 (15)S1—C00E—H00G109.5
C006—C008—S1125.87 (13)S1—C00E—H00H109.5
C004—C008—S1122.51 (13)H00G—C00E—H00H109.5
C005—C009—C00B117.6 (2)S1—C00E—H00I109.5
C005—C009—H009121.2H00G—C00E—H00I109.5
C00B—C009—H009121.2H00H—C00E—H00I109.5
C009—C005—C006—O10.8 (3)O2—C004—C008—C006176.09 (18)
C007—C005—C006—O1179.19 (17)C007—C004—C008—C0062.72 (19)
C009—C005—C006—C008177.74 (18)O2—C004—C008—S18.5 (3)
C007—C005—C006—C0080.69 (18)C007—C004—C008—S1172.69 (12)
C009—C005—C007—C00A0.8 (3)C00C—S1—C008—C00643.87 (18)
C006—C005—C007—C00A177.80 (17)C00E—S1—C008—C00661.80 (18)
C009—C005—C007—C004179.54 (16)C00C—S1—C008—C004130.86 (16)
C006—C005—C007—C0040.96 (18)C00E—S1—C008—C004123.48 (16)
O2—C004—C007—C00A4.7 (3)C007—C005—C009—C00B0.2 (3)
C008—C004—C007—C00A176.40 (19)C006—C005—C009—C00B178.47 (18)
O2—C004—C007—C005176.66 (17)C005—C007—C00A—C00D1.3 (3)
C008—C004—C007—C0052.22 (19)C004—C007—C00A—C00D179.82 (18)
O1—C006—C008—C004179.42 (18)C005—C009—C00B—C00D0.6 (3)
C005—C006—C008—C0042.17 (19)C009—C00B—C00D—C00A0.0 (3)
O1—C006—C008—S15.4 (3)C007—C00A—C00D—C00B1.0 (3)
C005—C006—C008—S1173.05 (13)
(spanh_3lcorr) top
Crystal data top
C26H19PSV = 1972.2 (7) Å3
Mr = 394.44Z = 4
Triclinic, P1F(000) = 824
a = 10.215 (2) ÅDx = 1.328 Mg m3
b = 12.322 (2) ÅMo Kα radiation, λ = 0.71073 Å
c = 17.351 (3) ŵ = 0.25 mm1
α = 101.57 (2)°T = 100 K
β = 91.25 (2)°Block, yellow
γ = 112.02 (2)°0.15 × 0.10 × 0.10 mm
Data collection top
Bruker Smart APEX II Quazar
diffractometer
45758 independent reflections
Radiation source: INCOATEC MicrosourceRint = 0.021
ω scansθmax = 53.0°, θmin = 1.2°
Absorption correction: multi-scan
SADABS2015/1
h = 2222
Tmin = 0.716, Tmax = 0.750k = 2726
272253 measured reflectionsl = 3838
Refinement top
Refinement on F20 restraints
Least-squares matrix: fullH-atom parameters constrained
R[F2 > 2σ(F2)] = 0.02 w2 = 1/[s2(Fo2)]
wR(F2) = 0.021(Δ/σ)max = 0.011
S = 1.40Δρmax = 0.30 e Å3
43155 reflectionsΔρmin = 0.21 e Å3
815 parameters
Crystal data top
C26H19PSγ = 112.02 (2)°
Mr = 394.44V = 1972.2 (7) Å3
Triclinic, P1Z = 4
a = 10.215 (2) ÅMo Kα radiation
b = 12.322 (2) ŵ = 0.25 mm1
c = 17.351 (3) ÅT = 100 K
α = 101.57 (2)°0.15 × 0.10 × 0.10 mm
β = 91.25 (2)°
Data collection top
Bruker Smart APEX II Quazar
diffractometer
272253 measured reflections
Absorption correction: multi-scan
SADABS2015/1
45758 independent reflections
Tmin = 0.716, Tmax = 0.750Rint = 0.021
Refinement top
R[F2 > 2σ(F2)] = 0.020 restraints
wR(F2) = 0.021H-atom parameters constrained
S = 1.40Δρmax = 0.30 e Å3
43155 reflectionsΔρmin = 0.21 e Å3
815 parameters
Fractional atomic coordinates and isotropic or equivalent isotropic displacement parameters (Å2) top
xyzUiso*/Ueq
S(1)0.338686 (8)0.550091 (7)0.771206 (4)0.017
S(2)0.790744 (10)0.537378 (7)0.663518 (5)0.022
P(1)0.240527 (7)0.387161 (6)0.786524 (4)0.012
P(2)0.897382 (8)0.702440 (6)0.655799 (4)0.014
C(1)0.170981 (13)0.374949 (11)0.881897 (8)0.013
C(2)0.039051 (14)0.387504 (11)0.891267 (7)0.013
C(3)0.021087 (14)0.439064 (12)0.840390 (7)0.015
C(4)0.151143 (15)0.444518 (13)0.849780 (8)0.017
C(5)0.23219 (3)0.39760 (3)0.909811 (18)0.02
C(6)0.176487 (14)0.353062 (13)0.961954 (8)0.018
C(7)0.038956 (14)0.349042 (12)0.955350 (8)0.014
C(8)0.021322 (14)0.309885 (12)1.011336 (8)0.015
C(9)0.159539 (14)0.313808 (11)1.009094 (7)0.013
C(10)0.224306 (14)0.287385 (12)1.072617 (8)0.016
C(11)0.361259 (15)0.295582 (13)1.073693 (8)0.018
C(12)0.440580 (15)0.332303 (14)1.010753 (9)0.02
C(13)0.381422 (14)0.356680 (13)0.948099 (8)0.017
C(14)0.237492 (13)0.347351 (11)0.943819 (7)0.013
C(15)0.347465 (13)0.296771 (11)0.767164 (7)0.013
C(16)0.295458 (14)0.177786 (13)0.775880 (8)0.016
C(17)0.375819 (15)0.108390 (13)0.757707 (9)0.018
C(18)0.507383 (15)0.156452 (13)0.729308 (8)0.018
C(19)0.558891 (14)0.274218 (12)0.720109 (8)0.017
C(20)0.479739 (14)0.345083 (12)0.739679 (7)0.014
C(21)0.084042 (14)0.298725 (11)0.715641 (7)0.013
C(22)0.067492 (15)0.337722 (13)0.647498 (8)0.016
C(23)0.054490 (16)0.274602 (14)0.594421 (8)0.021
C(24)0.15908 (3)0.17224 (3)0.609076 (17)0.021
C(25)0.141496 (15)0.131060 (13)0.676255 (8)0.018
C(26)0.020446 (15)0.194248 (12)0.729444 (8)0.016
C(27)0.925939 (13)0.813261 (12)0.748504 (8)0.013
C(28)1.048349 (14)0.847201 (11)0.802881 (8)0.013
C(29)1.140802 (14)0.783006 (12)0.798730 (8)0.015
C(30)1.255460 (15)0.818697 (13)0.853837 (8)0.018
C(31)1.288767 (15)0.922224 (14)0.916387 (9)0.019
C(32)1.201634 (14)0.984209 (13)0.924262 (8)0.017
C(33)1.077617 (14)0.946351 (12)0.869837 (8)0.014
C(34)0.981939 (14)1.003067 (12)0.883010 (8)0.015
C(35)0.852139 (14)0.959323 (12)0.836352 (8)0.014
C(36)0.748740 (16)1.009485 (13)0.857054 (8)0.018
C(37)0.616543 (16)0.960135 (14)0.816406 (9)0.02
C(38)0.581388 (15)0.857958 (14)0.752551 (9)0.019
C(39)0.680041 (14)0.810973 (13)0.728829 (8)0.017
C(40)0.820938 (14)0.860918 (12)0.768821 (7)0.013
C(41)0.815945 (14)0.746879 (12)0.579333 (8)0.015
C(42)0.869477 (15)0.864424 (13)0.568406 (8)0.018
C(43)0.81300 (3)0.89174 (3)0.504695 (17)0.021
C(44)0.70279 (3)0.80303 (3)0.451996 (17)0.023
C(45)0.64739 (3)0.68640 (3)0.463494 (17)0.023
C(46)0.70378 (3)0.65835 (3)0.526965 (17)0.019
C(47)1.07132 (3)0.72517 (2)0.621503 (15)0.016
C(48)1.10178 (4)0.62451 (3)0.591660 (17)0.022
C(49)1.23152 (4)0.63812 (4)0.562201 (19)0.03
C(50)1.33114 (4)0.75168 (4)0.562461 (19)0.03
C(51)1.30120 (3)0.85259 (3)0.592624 (18)0.025
C(52)1.17202 (3)0.83988 (3)0.621966 (16)0.019
H(3)0.0398680.4787950.7957170.01790 (2)
H(4)0.1920020.4869950.8117880.02063 (3)
H(5)0.3347380.4037570.9152240.02386 (3)
H(6)0.2303680.3227731.0113880.02183 (3)
H(8)0.0392710.2818991.0593230.01761 (2)
H(10)0.1627480.2651131.121360.01870 (3)
H(11)0.4124440.2799071.1232530.02166 (3)
H(12)0.5515020.3449081.0141870.02382 (3)
H(13)0.4465320.3907050.9030910.02009 (3)
H(16)0.1937590.1393470.7980390.01986 (3)
H(17)0.3354010.0169560.7655050.02187 (3)
H(18)0.5695670.1019960.7155070.02188 (3)
H(19)0.6607560.3118080.6979320.02030 (3)
H(20)0.5200590.4372750.7333890.01742 (2)
H(22)0.1486540.4191970.6378290.01983 (3)
H(23)0.068210.3065870.5422640.02497 (3)
H(24)0.2551910.1242320.56870.02508 (3)
H(25)0.2218950.0501640.687190.02227 (3)
H(26)0.0108130.1650230.783380.01888 (3)
H(29)1.1172790.7013980.7537970.01827 (2)
H(30)1.3202070.765880.8500880.02107 (3)
H(31)1.3807890.9498270.9589050.02295 (3)
H(32)1.2204771.061450.9722030.02103 (3)
H(34)1.0049891.0786880.9327630.01827 (2)
H(36)0.7779861.0859410.9067820.02126 (3)
H(37)0.5358610.9950580.8328640.02367 (3)
H(38)0.4744290.81550.7227620.02317 (3)
H(39)0.6486730.7300030.6824380.02008 (3)
H(42)0.9540780.9361750.6088610.02132 (3)
H(43)0.8559480.9832510.4970660.02524 (3)
H(44)0.6598780.8255460.4026330.02739 (3)
H(45)0.5612640.6165020.4229240.02740 (3)
H(46)0.6615580.5680230.5367630.02272 (3)
H(48)1.0235560.5361570.5918350.02700 (3)
H(49)1.2530310.5589020.5386340.03577 (4)
H(50)1.432180.7629510.5396950.03599 (4)
H(51)1.3785470.9418280.5937540.02988 (4)
H(52)1.1527940.9196830.6471730.02265 (3)
Atomic displacement parameters (Å2) top
U11U22U33U12U13U23
S(1)0.017993 (14)0.012410 (13)0.020556 (15)0.004656 (10)0.003206 (11)0.005743 (10)
S(2)0.03104 (4)0.01392 (3)0.01918 (4)0.00414 (3)0.00277 (3)0.00579 (3)
P(1)0.012330 (13)0.011859 (13)0.011219 (12)0.004868 (10)0.002247 (9)0.003795 (9)
P(2)0.017417 (14)0.012215 (13)0.010859 (13)0.005598 (11)0.001920 (10)0.002790 (10)
C(1)0.01271 (4)0.01547 (5)0.01088 (4)0.00660 (4)0.00201 (4)0.00383 (4)
C(2)0.01301 (5)0.01592 (5)0.01151 (4)0.00699 (4)0.00189 (4)0.00338 (4)
C(3)0.01595 (5)0.01858 (5)0.01287 (5)0.00950 (4)0.00190 (4)0.00421 (4)
C(4)0.01635 (5)0.02273 (6)0.01559 (5)0.01103 (4)0.00123 (4)0.00468 (4)
C(5)0.01454 (5)0.02913 (7)0.01972 (6)0.01156 (5)0.00337 (4)0.00798 (5)
C(6)0.01381 (5)0.02570 (6)0.01781 (5)0.00939 (5)0.00453 (4)0.00762 (5)
C(7)0.01279 (5)0.01781 (5)0.01282 (5)0.00679 (4)0.00268 (4)0.00439 (4)
C(8)0.01366 (5)0.01819 (5)0.01333 (5)0.00644 (4)0.00336 (4)0.00582 (4)
C(9)0.01319 (5)0.01479 (5)0.01156 (4)0.00541 (4)0.00193 (4)0.00428 (4)
C(10)0.01600 (5)0.01850 (5)0.01334 (5)0.00643 (4)0.00176 (4)0.00686 (4)
C(11)0.01631 (5)0.02383 (6)0.01580 (5)0.00795 (4)0.00047 (4)0.00866 (4)
C(12)0.01417 (5)0.03092 (7)0.01737 (5)0.00974 (5)0.00149 (4)0.01028 (5)
C(13)0.01261 (5)0.02504 (6)0.01428 (5)0.00779 (4)0.00203 (4)0.00753 (4)
C(14)0.01207 (4)0.01508 (5)0.01125 (4)0.00543 (4)0.00143 (4)0.00403 (4)
C(15)0.01308 (4)0.01328 (4)0.01395 (5)0.00556 (4)0.00330 (4)0.00460 (4)
C(16)0.01567 (5)0.01459 (5)0.02189 (6)0.00678 (4)0.00584 (4)0.00789 (4)
C(17)0.01807 (5)0.01542 (5)0.02420 (6)0.00851 (4)0.00477 (4)0.00745 (4)
C(18)0.01701 (5)0.01809 (5)0.02267 (6)0.00977 (4)0.00402 (4)0.00559 (4)
C(19)0.01394 (5)0.01777 (5)0.02005 (5)0.00705 (4)0.00438 (4)0.00483 (4)
C(20)0.01314 (5)0.01440 (5)0.01604 (5)0.00502 (4)0.00361 (4)0.00430 (4)
C(21)0.01436 (5)0.01375 (4)0.01110 (4)0.00551 (4)0.00147 (4)0.00375 (4)
C(22)0.01904 (5)0.01868 (5)0.01256 (5)0.00696 (4)0.00121 (4)0.00615 (4)
C(23)0.02347 (6)0.02420 (6)0.01415 (5)0.00825 (5)0.00242 (4)0.00572 (5)
C(24)0.02013 (6)0.02227 (6)0.01718 (5)0.00642 (5)0.00408 (5)0.00201 (5)
C(25)0.01696 (5)0.01693 (5)0.01819 (5)0.00346 (4)0.00125 (4)0.00297 (4)
C(26)0.01616 (5)0.01474 (5)0.01464 (5)0.00364 (4)0.00024 (4)0.00491 (4)
C(27)0.01457 (5)0.01396 (5)0.01105 (4)0.00607 (4)0.00193 (4)0.00266 (4)
C(28)0.01393 (5)0.01391 (5)0.01149 (4)0.00570 (4)0.00201 (4)0.00271 (4)
C(29)0.01673 (5)0.01767 (5)0.01320 (5)0.00887 (4)0.00241 (4)0.00354 (4)
C(30)0.01623 (5)0.02231 (6)0.01615 (5)0.00961 (4)0.00214 (4)0.00477 (4)
C(31)0.01482 (5)0.02355 (6)0.01714 (5)0.00659 (5)0.00046 (4)0.00257 (5)
C(32)0.01531 (5)0.01829 (5)0.01547 (5)0.00442 (4)0.00025 (4)0.00064 (4)
C(33)0.01418 (5)0.01363 (5)0.01292 (5)0.00461 (4)0.00176 (4)0.00177 (4)
C(34)0.01661 (5)0.01325 (5)0.01481 (5)0.00576 (4)0.00235 (4)0.00125 (4)
C(35)0.01616 (5)0.01394 (5)0.01390 (5)0.00712 (4)0.00339 (4)0.00351 (4)
C(36)0.02010 (6)0.01814 (5)0.01858 (5)0.01104 (5)0.00551 (4)0.00501 (4)
C(37)0.01955 (6)0.02456 (6)0.02101 (6)0.01346 (5)0.00582 (5)0.00832 (5)
C(38)0.01619 (5)0.02639 (6)0.01826 (5)0.01031 (5)0.00287 (4)0.00746 (5)
C(39)0.01500 (5)0.02114 (6)0.01434 (5)0.00730 (4)0.00154 (4)0.00429 (4)
C(40)0.01443 (5)0.01465 (5)0.01233 (4)0.00633 (4)0.00244 (4)0.00374 (4)
C(41)0.01751 (5)0.01510 (5)0.01172 (4)0.00609 (4)0.00068 (4)0.00257 (4)
C(42)0.02112 (6)0.01635 (5)0.01560 (5)0.00661 (4)0.00047 (4)0.00495 (4)
C(43)0.02699 (7)0.02186 (6)0.01723 (6)0.01166 (5)0.00037 (5)0.00713 (5)
C(44)0.02834 (7)0.02837 (7)0.01512 (5)0.01526 (6)0.00180 (5)0.00440 (5)
C(45)0.02451 (6)0.02550 (7)0.01631 (5)0.00975 (5)0.00453 (5)0.00063 (5)
C(46)0.02070 (6)0.01825 (6)0.01490 (5)0.00585 (5)0.00163 (4)0.00109 (4)
C(47)0.02042 (6)0.01808 (6)0.01236 (5)0.01067 (4)0.00345 (4)0.00342 (4)
C(48)0.03180 (7)0.02423 (7)0.01809 (6)0.01882 (6)0.00527 (5)0.00355 (5)
C(49)0.03647 (9)0.04004 (9)0.02408 (7)0.02844 (8)0.00848 (6)0.00436 (6)
C(50)0.02570 (7)0.04908 (11)0.02208 (7)0.02282 (7)0.00775 (6)0.00658 (7)
C(51)0.01851 (6)0.03601 (8)0.02044 (6)0.01072 (6)0.00542 (5)0.00674 (6)
C(52)0.01788 (5)0.02163 (6)0.01775 (5)0.00826 (5)0.00449 (4)0.00470 (4)
Geometric parameters (Å, º) top
S(1)—P(1)1.9552 (1)C(24)—H(24)1.0830 (3)
S(2)—P(2)1.9482 (1)C(25)—C(26)1.3882 (2)
P(1)—C(1)1.8267 (2)C(25)—H(25)1.0830 (1)
P(1)—C(15)1.8234 (2)C(26)—H(26)1.0830 (1)
P(1)—C(21)1.8237 (2)C(27)—C(28)1.4236 (2)
P(2)—C(27)1.8267 (2)C(27)—C(40)1.4231 (2)
P(2)—C(41)1.8268 (2)C(28)—C(29)1.4363 (2)
P(2)—C(47)1.8247 (3)C(28)—C(33)1.4399 (2)
C(1)—C(2)1.4221 (2)C(29)—C(30)1.3695 (2)
C(1)—C(14)1.4211 (2)C(29)—H(29)1.0830 (1)
C(2)—C(3)1.4333 (2)C(30)—C(31)1.4227 (2)
C(2)—C(7)1.4362 (2)C(30)—H(30)1.0830 (1)
C(3)—C(4)1.3668 (2)C(31)—C(32)1.3665 (2)
C(3)—H(3)1.0830 (1)C(31)—H(31)1.0830 (1)
C(4)—C(5)1.4230 (3)C(32)—C(33)1.4291 (2)
C(4)—H(4)1.0830 (1)C(32)—H(32)1.0830 (1)
C(5)—C(6)1.3618 (3)C(33)—C(34)1.3978 (2)
C(5)—H(5)1.0830 (3)C(34)—C(35)1.3951 (2)
C(6)—C(7)1.4305 (2)C(34)—H(34)1.0830 (1)
C(6)—H(6)1.0830 (1)C(35)—C(36)1.4296 (2)
C(7)—C(8)1.3929 (2)C(35)—C(40)1.4383 (2)
C(8)—C(9)1.3962 (2)C(36)—C(37)1.3643 (2)
C(8)—H(8)1.0830 (1)C(36)—H(36)1.0830 (2)
C(9)—C(10)1.4256 (2)C(37)—C(38)1.4233 (2)
C(9)—C(14)1.4381 (2)C(37)—H(37)1.0830 (1)
C(10)—C(11)1.3638 (2)C(38)—C(39)1.3712 (2)
C(10)—H(10)1.0830 (1)C(38)—H(38)1.0830 (2)
C(11)—C(12)1.4198 (2)C(39)—C(40)1.4327 (2)
C(11)—H(11)1.0830 (1)C(39)—H(39)1.0830 (1)
C(12)—C(13)1.3695 (2)C(41)—C(42)1.3977 (2)
C(12)—H(12)1.0830 (1)C(41)—C(46)1.3957 (3)
C(13)—C(14)1.4302 (2)C(42)—C(43)1.3911 (3)
C(13)—H(13)1.0830 (1)C(42)—H(42)1.0830 (2)
C(15)—C(16)1.4011 (2)C(43)—C(44)1.3892 (4)
C(15)—C(20)1.3951 (2)C(43)—H(43)1.0830 (3)
C(16)—C(17)1.3907 (2)C(44)—C(45)1.3912 (5)
C(16)—H(16)1.0830 (1)C(44)—H(44)1.0830 (3)
C(17)—C(18)1.3960 (2)C(45)—C(46)1.3923 (4)
C(17)—H(17)1.0830 (1)C(45)—H(45)1.0830 (3)
C(18)—C(19)1.3900 (2)C(46)—H(46)1.0830 (3)
C(18)—H(18)1.0830 (1)C(47)—C(48)1.3935 (4)
C(19)—C(20)1.3978 (2)C(47)—C(52)1.4003 (4)
C(19)—H(19)1.0830 (1)C(48)—C(49)1.3940 (5)
C(20)—H(20)1.0830 (1)C(48)—H(48)1.0830 (4)
C(21)—C(22)1.3920 (2)C(49)—C(50)1.3867 (6)
C(21)—C(26)1.3994 (2)C(49)—H(49)1.0830 (3)
C(22)—C(23)1.3934 (2)C(50)—C(51)1.3946 (5)
C(22)—H(22)1.0830 (1)C(50)—H(50)1.0830 (3)
C(23)—C(24)1.3882 (3)C(51)—C(52)1.3897 (4)
C(23)—H(23)1.0830 (1)C(51)—H(51)1.0830 (4)
C(24)—C(25)1.3946 (3)C(52)—H(52)1.0830 (3)
S(1)—P(1)—C(1)116.214 (6)C(24)—C(25)—C(26)119.811 (17)
S(1)—P(1)—C(15)112.519 (5)C(24)—C(25)—H(25)120.335 (17)
S(1)—P(1)—C(21)113.049 (5)C(26)—C(25)—H(25)119.854 (13)
C(1)—P(1)—C(15)109.001 (6)C(21)—C(26)—C(25)120.187 (13)
C(1)—P(1)—C(21)103.063 (6)C(21)—C(26)—H(26)120.372 (12)
C(15)—P(1)—C(21)101.643 (6)C(25)—C(26)—H(26)119.333 (13)
S(2)—P(2)—C(27)113.915 (6)P(2)—C(27)—C(28)120.614 (10)
S(2)—P(2)—C(41)112.833 (6)P(2)—C(27)—C(40)119.759 (10)
S(2)—P(2)—C(47)112.932 (9)C(28)—C(27)—C(40)119.522 (12)
C(27)—P(2)—C(41)108.136 (6)C(27)—C(28)—C(29)123.990 (12)
C(27)—P(2)—C(47)107.147 (10)C(27)—C(28)—C(33)119.031 (12)
C(41)—P(2)—C(47)100.932 (9)C(29)—C(28)—C(33)116.821 (12)
P(1)—C(1)—C(2)116.845 (9)C(28)—C(29)—C(30)121.274 (13)
P(1)—C(1)—C(14)123.470 (9)C(28)—C(29)—H(29)120.389 (12)
C(2)—C(1)—C(14)119.587 (12)C(30)—C(29)—H(29)118.221 (12)
C(1)—C(2)—C(3)123.406 (12)C(29)—C(30)—C(31)121.077 (13)
C(1)—C(2)—C(7)119.461 (12)C(29)—C(30)—H(30)119.101 (14)
C(3)—C(2)—C(7)117.125 (12)C(31)—C(30)—H(30)119.811 (13)
C(2)—C(3)—C(4)121.196 (12)C(30)—C(31)—C(32)119.824 (13)
C(2)—C(3)—H(3)119.497 (12)C(30)—C(31)—H(31)120.021 (14)
C(4)—C(3)—H(3)119.224 (12)C(32)—C(31)—H(31)120.116 (14)
C(3)—C(4)—C(5)120.999 (16)C(31)—C(32)—C(33)120.536 (13)
C(3)—C(4)—H(4)119.445 (13)C(31)—C(32)—H(32)122.438 (13)
C(5)—C(4)—H(4)119.542 (16)C(33)—C(32)—H(32)116.997 (13)
C(4)—C(5)—C(6)119.85 (2)C(28)—C(33)—C(32)120.192 (12)
C(4)—C(5)—H(5)118.62 (3)C(28)—C(33)—C(34)119.824 (12)
C(6)—C(5)—H(5)121.40 (3)C(32)—C(33)—C(34)119.950 (12)
C(5)—C(6)—C(7)120.635 (17)C(33)—C(34)—C(35)121.250 (13)
C(5)—C(6)—H(6)122.684 (17)C(33)—C(34)—H(34)119.772 (12)
C(7)—C(6)—H(6)116.630 (13)C(35)—C(34)—H(34)118.839 (12)
C(2)—C(7)—C(6)119.911 (12)C(34)—C(35)—C(36)120.135 (13)
C(2)—C(7)—C(8)119.505 (12)C(34)—C(35)—C(40)119.711 (12)
C(6)—C(7)—C(8)120.575 (12)C(36)—C(35)—C(40)120.123 (12)
C(7)—C(8)—C(9)121.285 (13)C(35)—C(36)—C(37)120.667 (13)
C(7)—C(8)—H(8)118.138 (12)C(35)—C(36)—H(36)117.848 (13)
C(9)—C(8)—H(8)120.443 (12)C(37)—C(36)—H(36)121.464 (13)
C(8)—C(9)—C(10)119.804 (12)C(36)—C(37)—C(38)119.671 (13)
C(8)—C(9)—C(14)120.032 (12)C(36)—C(37)—H(37)121.465 (15)
C(10)—C(9)—C(14)120.146 (12)C(38)—C(37)—H(37)118.829 (14)
C(9)—C(10)—C(11)121.092 (12)C(37)—C(38)—C(39)121.145 (13)
C(9)—C(10)—H(10)117.614 (12)C(37)—C(38)—H(38)119.554 (14)
C(11)—C(10)—H(10)121.219 (12)C(39)—C(38)—H(38)119.293 (15)
C(10)—C(11)—C(12)119.188 (12)C(38)—C(39)—C(40)121.192 (13)
C(10)—C(11)—H(11)121.258 (13)C(38)—C(39)—H(39)119.553 (13)
C(12)—C(11)—H(11)119.448 (13)C(40)—C(39)—H(39)119.035 (12)
C(11)—C(12)—C(13)121.432 (12)C(27)—C(40)—C(35)119.306 (12)
C(11)—C(12)—H(12)118.701 (13)C(27)—C(40)—C(39)123.562 (12)
C(13)—C(12)—H(12)119.809 (13)C(35)—C(40)—C(39)116.988 (12)
C(12)—C(13)—C(14)121.306 (12)P(2)—C(41)—C(42)121.864 (11)
C(12)—C(13)—H(13)119.795 (12)P(2)—C(41)—C(46)118.490 (15)
C(14)—C(13)—H(13)118.708 (12)C(42)—C(41)—C(46)119.472 (18)
C(1)—C(14)—C(9)118.923 (11)C(41)—C(42)—C(43)119.949 (18)
C(1)—C(14)—C(13)124.203 (12)C(41)—C(42)—H(42)121.654 (13)
C(9)—C(14)—C(13)116.790 (12)C(43)—C(42)—H(42)118.394 (18)
P(1)—C(15)—C(16)120.795 (10)C(42)—C(43)—C(44)120.43 (3)
P(1)—C(15)—C(20)119.390 (10)C(42)—C(43)—H(43)118.95 (3)
C(16)—C(15)—C(20)119.742 (13)C(44)—C(43)—H(43)120.63 (3)
C(15)—C(16)—C(17)120.117 (13)C(43)—C(44)—C(45)119.82 (3)
C(15)—C(16)—H(16)120.686 (12)C(43)—C(44)—H(44)119.64 (3)
C(17)—C(16)—H(16)119.181 (13)C(45)—C(44)—H(44)120.54 (3)
C(16)—C(17)—C(18)120.038 (12)C(44)—C(45)—C(46)120.05 (3)
C(16)—C(17)—H(17)119.555 (13)C(44)—C(45)—H(45)120.52 (3)
C(18)—C(17)—H(17)120.407 (12)C(46)—C(45)—H(45)119.43 (3)
C(17)—C(18)—C(19)119.987 (12)C(41)—C(46)—C(45)120.27 (3)
C(17)—C(18)—H(18)119.624 (13)C(41)—C(46)—H(46)118.85 (2)
C(19)—C(18)—H(18)120.380 (13)C(45)—C(46)—H(46)120.88 (3)
C(18)—C(19)—C(20)120.206 (12)P(2)—C(47)—C(48)118.47 (2)
C(18)—C(19)—H(19)120.251 (12)P(2)—C(47)—C(52)121.91 (2)
C(20)—C(19)—H(19)119.542 (13)C(48)—C(47)—C(52)119.58 (3)
C(15)—C(20)—C(19)119.894 (13)C(47)—C(48)—C(49)120.11 (3)
C(15)—C(20)—H(20)119.613 (12)C(47)—C(48)—H(48)119.11 (3)
C(19)—C(20)—H(20)120.493 (12)C(49)—C(48)—H(48)120.78 (3)
P(1)—C(21)—C(22)119.087 (10)C(48)—C(49)—C(50)120.33 (3)
P(1)—C(21)—C(26)121.181 (10)C(48)—C(49)—H(49)119.17 (4)
C(22)—C(21)—C(26)119.718 (13)C(50)—C(49)—H(49)120.50 (3)
C(21)—C(22)—C(23)120.000 (13)C(49)—C(50)—C(51)119.68 (3)
C(21)—C(22)—H(22)118.958 (13)C(49)—C(50)—H(50)120.75 (3)
C(23)—C(22)—H(22)121.001 (13)C(51)—C(50)—H(50)119.57 (4)
C(22)—C(23)—C(24)120.078 (16)C(50)—C(51)—C(52)120.39 (3)
C(22)—C(23)—H(23)119.757 (14)C(50)—C(51)—H(51)120.41 (3)
C(24)—C(23)—H(23)120.156 (17)C(52)—C(51)—H(51)119.20 (3)
C(23)—C(24)—C(25)120.18 (2)C(47)—C(52)—C(51)119.91 (3)
C(23)—C(24)—H(24)120.27 (2)C(47)—C(52)—H(52)120.99 (3)
C(25)—C(24)—H(24)119.56 (3)C(51)—C(52)—H(52)119.05 (3)
(spanh_3lnocorr) top
Crystal data top
C26H19PSV = 1972.2 (7) Å3
Mr = 394.44Z = 4
Triclinic, P1F(000) = 824
a = 10.215 (2) ÅDx = 1.328 Mg m3
b = 12.322 (2) ÅMo Kα radiation, λ = 0.71073 Å
c = 17.351 (3) ŵ = 0.25 mm1
α = 101.57 (2)°T = 100 K
β = 91.25 (2)°Block, yellow
γ = 112.02 (2)°0.15 × 0.10 × 0.10 mm
Data collection top
Bruker Smart APEX II Quazar
diffractometer
45758 independent reflections
Radiation source: INCOATEC MicrosourceRint = 0.021
ω scansθmax = 53.0°, θmin = 1.2°
Absorption correction: multi-scan
SADABS2015/1
h = 2222
Tmin = 0.716, Tmax = 0.750k = 2726
272253 measured reflectionsl = 3838
Refinement top
Refinement on F20 restraints
Least-squares matrix: fullH-atom parameters constrained
R[F2 > 2σ(F2)] = 0.021 w2 = 1/[s2(Fo2)]
wR(F2) = 0.025(Δ/σ)max = 0.004
S = 1.67Δρmax = 0.29 e Å3
43292 reflectionsΔρmin = 0.21 e Å3
815 parameters
Crystal data top
C26H19PSγ = 112.02 (2)°
Mr = 394.44V = 1972.2 (7) Å3
Triclinic, P1Z = 4
a = 10.215 (2) ÅMo Kα radiation
b = 12.322 (2) ŵ = 0.25 mm1
c = 17.351 (3) ÅT = 100 K
α = 101.57 (2)°0.15 × 0.10 × 0.10 mm
β = 91.25 (2)°
Data collection top
Bruker Smart APEX II Quazar
diffractometer
272253 measured reflections
Absorption correction: multi-scan
SADABS2015/1
45758 independent reflections
Tmin = 0.716, Tmax = 0.750Rint = 0.021
Refinement top
R[F2 > 2σ(F2)] = 0.0210 restraints
wR(F2) = 0.025H-atom parameters constrained
S = 1.67Δρmax = 0.29 e Å3
43292 reflectionsΔρmin = 0.21 e Å3
815 parameters
Fractional atomic coordinates and isotropic or equivalent isotropic displacement parameters (Å2) top
xyzUiso*/Ueq
S(1)0.338679 (9)0.550091 (8)0.771200 (5)0.017
S(2)0.790753 (11)0.537383 (9)0.663517 (5)0.022
P(1)0.240533 (8)0.387168 (7)0.786528 (5)0.012
P(2)0.897388 (9)0.702438 (7)0.655799 (5)0.013
C(1)0.170984 (15)0.374947 (13)0.881893 (9)0.013
C(2)0.039047 (16)0.387497 (13)0.891266 (9)0.013
C(3)0.021085 (17)0.439060 (14)0.840384 (9)0.015
C(4)0.151135 (18)0.444520 (15)0.849770 (10)0.017
C(5)0.23219 (4)0.39759 (3)0.90981 (2)0.02
C(6)0.176488 (17)0.353067 (16)0.961959 (10)0.018
C(7)0.038965 (17)0.349043 (14)0.955359 (9)0.014
C(8)0.021340 (16)0.309890 (14)1.011341 (9)0.015
C(9)0.159544 (16)0.313800 (13)1.009096 (9)0.013
C(10)0.224281 (17)0.287383 (14)1.072614 (9)0.016
C(11)0.361261 (18)0.295576 (15)1.073689 (10)0.018
C(12)0.440575 (18)0.332296 (17)1.010741 (10)0.02
C(13)0.381426 (17)0.356675 (15)0.948101 (9)0.017
C(14)0.237498 (16)0.347358 (13)0.943813 (9)0.013
C(15)0.347469 (16)0.296765 (14)0.767167 (8)0.013
C(16)0.295468 (17)0.177786 (15)0.775874 (10)0.016
C(17)0.375817 (18)0.108369 (15)0.757709 (10)0.018
C(18)0.507373 (18)0.156462 (15)0.729319 (10)0.018
C(19)0.558884 (17)0.274225 (15)0.720112 (10)0.017
C(20)0.479736 (17)0.345080 (14)0.739677 (9)0.014
C(21)0.084035 (17)0.298731 (14)0.715646 (9)0.013
C(22)0.067474 (18)0.337701 (15)0.647491 (9)0.016
C(23)0.054457 (19)0.274586 (17)0.594402 (10)0.021
C(24)0.15906 (4)0.17222 (3)0.60906 (2)0.021
C(25)0.141480 (18)0.131062 (15)0.676259 (10)0.018
C(26)0.020458 (17)0.194254 (15)0.729448 (9)0.016
C(27)0.925936 (16)0.813269 (14)0.748506 (9)0.013
C(28)1.048357 (17)0.847206 (14)0.802881 (9)0.013
C(29)1.140802 (17)0.782998 (14)0.798725 (9)0.015
C(30)1.255449 (18)0.818692 (16)0.853843 (10)0.017
C(31)1.288780 (18)0.922248 (17)0.916390 (10)0.019
C(32)1.201637 (17)0.984221 (15)0.924277 (10)0.017
C(33)1.077623 (17)0.946338 (14)0.869847 (9)0.014
C(34)0.981940 (17)1.003069 (15)0.883003 (10)0.015
C(35)0.852133 (17)0.959319 (14)0.836357 (9)0.014
C(36)0.748754 (19)1.009498 (15)0.857055 (10)0.018
C(37)0.616523 (19)0.960126 (17)0.816404 (11)0.02
C(38)0.581363 (18)0.857945 (17)0.752548 (10)0.019
C(39)0.680061 (17)0.810989 (15)0.728829 (9)0.017
C(40)0.820946 (17)0.860912 (14)0.768814 (9)0.013
C(41)0.815946 (17)0.746875 (14)0.579332 (9)0.015
C(42)0.869462 (18)0.864416 (16)0.568405 (10)0.018
C(43)0.81298 (4)0.89172 (3)0.50469 (2)0.021
C(44)0.70279 (4)0.80305 (4)0.45201 (2)0.023
C(45)0.64744 (4)0.68643 (4)0.46350 (2)0.023
C(46)0.70376 (4)0.65832 (3)0.52694 (2)0.019
C(47)1.07130 (4)0.72513 (3)0.621494 (18)0.016
C(48)1.10178 (4)0.62447 (4)0.59164 (2)0.022
C(49)1.23152 (5)0.63812 (4)0.56220 (2)0.03
C(50)1.33111 (5)0.75167 (5)0.56245 (2)0.03
C(51)1.30112 (4)0.85253 (4)0.59262 (2)0.025
C(52)1.17205 (4)0.83989 (3)0.621964 (19)0.019
H(3)0.0398730.4787980.7957140.01788 (3)
H(4)0.1920060.4869990.8117850.02063 (3)
H(5)0.3347240.4037560.9152230.02387 (4)
H(6)0.2303710.3227711.0113910.02184 (3)
H(8)0.039270.28191.0593220.01761 (3)
H(10)0.1627440.2651111.1213630.01870 (3)
H(11)0.4124440.2799071.1232530.02165 (3)
H(12)0.5514990.3449081.0141870.02382 (4)
H(13)0.446530.3907050.9030930.02007 (3)
H(16)0.1937720.1393510.7980360.01986 (3)
H(17)0.3353920.0169350.7655070.02191 (3)
H(18)0.5695560.1020060.715510.02186 (3)
H(19)0.6607490.3118050.6979330.02028 (3)
H(20)0.5200590.4372740.7333890.01740 (3)
H(22)0.1486390.4191820.6378310.01982 (3)
H(23)0.0682110.3065890.542260.02496 (4)
H(24)0.2551930.124230.5686980.02505 (4)
H(25)0.221890.0501690.6871890.02222 (3)
H(26)0.0108130.1650230.7833790.01888 (3)
H(29)1.1172760.701390.7537930.01824 (3)
H(30)1.3202050.7658820.8500880.02104 (3)
H(31)1.3807960.9498290.9589080.02290 (3)
H(32)1.2204811.0614670.9722130.02101 (3)
H(34)1.0049881.0786850.9327610.01827 (3)
H(36)0.7779891.0859480.9067860.02125 (3)
H(37)0.5358530.9950610.8328660.02366 (4)
H(38)0.4744050.815490.7227550.02317 (4)
H(39)0.6486760.7300110.6824430.02009 (3)
H(42)0.9540690.9361670.6088570.02130 (3)
H(43)0.8559410.9832380.4970670.02520 (4)
H(44)0.6598820.8255430.4026380.02737 (4)
H(45)0.5612980.6165290.422940.02741 (4)
H(46)0.6615510.5680060.5367650.02275 (3)
H(48)1.023530.5361280.5918350.02701 (4)
H(49)1.2530290.5589080.5386360.03580 (5)
H(50)1.4321590.7629490.53970.03596 (5)
H(51)1.3784840.9417550.5937530.02988 (4)
H(52)1.1527940.919680.6471720.02267 (3)
Atomic displacement parameters (Å2) top
U11U22U33U12U13U23
S(1)0.017979 (17)0.012420 (15)0.020551 (18)0.004661 (12)0.003197 (13)0.005742 (12)
S(2)0.03104 (5)0.01392 (4)0.01919 (4)0.00412 (4)0.00276 (4)0.00581 (3)
P(1)0.012338 (15)0.011839 (15)0.011215 (15)0.004869 (12)0.002262 (11)0.003794 (11)
P(2)0.017404 (17)0.012214 (16)0.010846 (15)0.005593 (13)0.001916 (12)0.002781 (11)
C(1)0.01273 (5)0.01546 (6)0.01086 (5)0.00662 (5)0.00202 (4)0.00384 (4)
C(2)0.01299 (5)0.01593 (6)0.01147 (5)0.00699 (5)0.00191 (4)0.00334 (4)
C(3)0.01591 (6)0.01859 (6)0.01283 (5)0.00948 (5)0.00190 (5)0.00422 (5)
C(4)0.01635 (6)0.02278 (7)0.01558 (6)0.01107 (5)0.00123 (5)0.00470 (5)
C(5)0.01455 (6)0.02913 (8)0.01974 (7)0.01156 (6)0.00337 (5)0.00796 (6)
C(6)0.01380 (6)0.02571 (7)0.01784 (6)0.00940 (5)0.00455 (5)0.00761 (6)
C(7)0.01273 (5)0.01779 (6)0.01283 (5)0.00676 (5)0.00267 (4)0.00435 (5)
C(8)0.01366 (6)0.01819 (6)0.01335 (5)0.00644 (5)0.00340 (5)0.00589 (5)
C(9)0.01325 (6)0.01481 (6)0.01157 (5)0.00544 (4)0.00192 (4)0.00427 (4)
C(10)0.01602 (6)0.01846 (6)0.01337 (6)0.00643 (5)0.00177 (5)0.00686 (5)
C(11)0.01628 (6)0.02381 (7)0.01582 (6)0.00793 (5)0.00046 (5)0.00866 (5)
C(12)0.01413 (6)0.03103 (8)0.01731 (6)0.00977 (6)0.00148 (5)0.01027 (6)
C(13)0.01259 (6)0.02504 (7)0.01426 (6)0.00780 (5)0.00203 (5)0.00750 (5)
C(14)0.01209 (5)0.01511 (6)0.01120 (5)0.00550 (4)0.00147 (4)0.00404 (4)
C(15)0.01307 (5)0.01327 (5)0.01396 (6)0.00555 (5)0.00326 (4)0.00459 (4)
C(16)0.01567 (6)0.01462 (6)0.02189 (7)0.00681 (5)0.00583 (5)0.00793 (5)
C(17)0.01802 (6)0.01550 (6)0.02429 (7)0.00851 (5)0.00478 (5)0.00753 (5)
C(18)0.01699 (6)0.01800 (6)0.02272 (7)0.00975 (5)0.00407 (5)0.00558 (5)
C(19)0.01400 (6)0.01773 (6)0.02001 (6)0.00706 (5)0.00436 (5)0.00481 (5)
C(20)0.01319 (5)0.01437 (6)0.01600 (6)0.00503 (5)0.00366 (4)0.00428 (4)
C(21)0.01433 (5)0.01375 (5)0.01109 (5)0.00550 (5)0.00149 (4)0.00376 (4)
C(22)0.01903 (6)0.01863 (6)0.01257 (6)0.00694 (5)0.00124 (5)0.00616 (5)
C(23)0.02345 (7)0.02416 (7)0.01416 (6)0.00822 (6)0.00242 (5)0.00571 (5)
C(24)0.02009 (7)0.02221 (7)0.01719 (7)0.00638 (6)0.00408 (5)0.00199 (5)
C(25)0.01699 (6)0.01685 (6)0.01813 (6)0.00344 (5)0.00130 (5)0.00295 (5)
C(26)0.01614 (6)0.01471 (6)0.01466 (6)0.00363 (5)0.00026 (5)0.00493 (5)
C(27)0.01462 (6)0.01394 (6)0.01101 (5)0.00608 (4)0.00196 (4)0.00263 (5)
C(28)0.01395 (5)0.01393 (5)0.01144 (5)0.00572 (5)0.00201 (4)0.00275 (4)
C(29)0.01672 (6)0.01766 (6)0.01316 (6)0.00887 (5)0.00241 (5)0.00352 (5)
C(30)0.01625 (6)0.02225 (7)0.01614 (6)0.00962 (5)0.00219 (5)0.00473 (5)
C(31)0.01480 (6)0.02350 (7)0.01713 (6)0.00662 (5)0.00046 (5)0.00255 (6)
C(32)0.01528 (6)0.01828 (6)0.01547 (6)0.00442 (5)0.00022 (5)0.00065 (5)
C(33)0.01417 (6)0.01354 (5)0.01288 (5)0.00460 (5)0.00179 (5)0.00174 (4)
C(34)0.01662 (6)0.01326 (6)0.01482 (6)0.00576 (5)0.00240 (5)0.00126 (5)
C(35)0.01616 (6)0.01398 (6)0.01387 (6)0.00715 (5)0.00337 (5)0.00350 (5)
C(36)0.02006 (7)0.01815 (6)0.01857 (6)0.01101 (5)0.00551 (5)0.00499 (5)
C(37)0.01960 (7)0.02450 (7)0.02100 (7)0.01346 (6)0.00582 (6)0.00831 (6)
C(38)0.01617 (6)0.02643 (8)0.01826 (7)0.01034 (6)0.00283 (5)0.00748 (6)
C(39)0.01502 (6)0.02116 (7)0.01433 (6)0.00732 (5)0.00154 (5)0.00427 (5)
C(40)0.01440 (6)0.01465 (6)0.01231 (5)0.00632 (5)0.00245 (4)0.00373 (5)
C(41)0.01748 (6)0.01517 (6)0.01172 (5)0.00612 (5)0.00067 (5)0.00256 (4)
C(42)0.02110 (7)0.01638 (6)0.01560 (6)0.00666 (5)0.00046 (5)0.00495 (5)
C(43)0.02695 (8)0.02184 (7)0.01721 (7)0.01166 (6)0.00038 (6)0.00715 (6)
C(44)0.02836 (8)0.02845 (9)0.01502 (6)0.01533 (7)0.00182 (6)0.00443 (6)
C(45)0.02454 (8)0.02548 (8)0.01633 (7)0.00973 (6)0.00454 (6)0.00066 (6)
C(46)0.02077 (7)0.01831 (7)0.01486 (6)0.00591 (6)0.00164 (5)0.00109 (5)
C(47)0.02039 (7)0.01811 (7)0.01232 (6)0.01066 (5)0.00343 (5)0.00340 (5)
C(48)0.03183 (9)0.02425 (8)0.01806 (7)0.01884 (7)0.00521 (6)0.00351 (6)
C(49)0.03651 (10)0.04009 (11)0.02405 (8)0.02847 (10)0.00843 (7)0.00430 (7)
C(50)0.02559 (9)0.04909 (13)0.02204 (8)0.02273 (9)0.00772 (7)0.00662 (8)
C(51)0.01851 (7)0.03606 (10)0.02044 (7)0.01075 (7)0.00541 (6)0.00677 (7)
C(52)0.01785 (7)0.02166 (7)0.01780 (6)0.00828 (6)0.00449 (5)0.00470 (5)
Geometric parameters (Å, º) top
S(1)—P(1)1.9552 (1)C(24)—H(24)1.0830 (4)
S(2)—P(2)1.9481 (1)C(25)—C(26)1.3880 (2)
P(1)—C(1)1.8266 (2)C(25)—H(25)1.0830 (2)
P(1)—C(15)1.8235 (2)C(26)—H(26)1.0830 (2)
P(1)—C(21)1.8237 (2)C(27)—C(28)1.4237 (2)
P(2)—C(27)1.8268 (2)C(27)—C(40)1.4229 (2)
P(2)—C(41)1.8268 (2)C(28)—C(29)1.4364 (2)
P(2)—C(47)1.8245 (4)C(28)—C(33)1.4399 (2)
C(1)—C(2)1.4222 (2)C(29)—C(30)1.3696 (2)
C(1)—C(14)1.4210 (2)C(29)—H(29)1.0830 (2)
C(2)—C(3)1.4333 (2)C(30)—C(31)1.4229 (2)
C(2)—C(7)1.4364 (2)C(30)—H(30)1.0830 (2)
C(3)—C(4)1.3667 (2)C(31)—C(32)1.3665 (2)
C(3)—H(3)1.0830 (2)C(31)—H(31)1.0830 (2)
C(4)—C(5)1.4231 (4)C(32)—C(33)1.4290 (2)
C(4)—H(4)1.0830 (2)C(32)—H(32)1.0830 (2)
C(5)—C(6)1.3617 (4)C(33)—C(34)1.3979 (2)
C(5)—H(5)1.0830 (3)C(34)—C(35)1.3950 (2)
C(6)—C(7)1.4304 (2)C(34)—H(34)1.0830 (2)
C(6)—H(6)1.0830 (2)C(35)—C(36)1.4295 (2)
C(7)—C(8)1.3930 (2)C(35)—C(40)1.4385 (2)
C(8)—C(9)1.3961 (2)C(36)—C(37)1.3646 (3)
C(8)—H(8)1.0830 (2)C(36)—H(36)1.0830 (2)
C(9)—C(10)1.4253 (2)C(37)—C(38)1.4233 (3)
C(9)—C(14)1.4382 (2)C(37)—H(37)1.0830 (2)
C(10)—C(11)1.3640 (2)C(38)—C(39)1.3714 (2)
C(10)—H(10)1.0830 (2)C(38)—H(38)1.0830 (2)
C(11)—C(12)1.4199 (2)C(39)—C(40)1.4326 (2)
C(11)—H(11)1.0830 (2)C(39)—H(39)1.0830 (2)
C(12)—C(13)1.3693 (2)C(41)—C(42)1.3977 (2)
C(12)—H(12)1.0830 (2)C(41)—C(46)1.3961 (4)
C(13)—C(14)1.4302 (2)C(42)—C(43)1.3912 (4)
C(13)—H(13)1.0830 (2)C(42)—H(42)1.0830 (2)
C(15)—C(16)1.4010 (2)C(43)—C(44)1.3887 (5)
C(15)—C(20)1.3951 (2)C(43)—H(43)1.0830 (4)
C(16)—C(17)1.3908 (2)C(44)—C(45)1.3910 (6)
C(16)—H(16)1.0830 (2)C(44)—H(44)1.0830 (4)
C(17)—C(18)1.3959 (2)C(45)—C(46)1.3919 (5)
C(17)—H(17)1.0830 (2)C(45)—H(45)1.0830 (4)
C(18)—C(19)1.3900 (2)C(46)—H(46)1.0830 (4)
C(18)—H(18)1.0830 (2)C(47)—C(48)1.3938 (5)
C(19)—C(20)1.3977 (2)C(47)—C(52)1.4010 (5)
C(19)—H(19)1.0830 (2)C(48)—C(49)1.3937 (6)
C(20)—H(20)1.0830 (2)C(48)—H(48)1.0830 (4)
C(21)—C(22)1.3920 (2)C(49)—C(50)1.3865 (7)
C(21)—C(26)1.3994 (2)C(49)—H(49)1.0830 (4)
C(22)—C(23)1.3932 (2)C(50)—C(51)1.3942 (6)
C(22)—H(22)1.0830 (2)C(50)—H(50)1.0830 (4)
C(23)—C(24)1.3883 (4)C(51)—C(52)1.3889 (5)
C(23)—H(23)1.0830 (2)C(51)—H(51)1.0830 (4)
C(24)—C(25)1.3947 (4)C(52)—H(52)1.0830 (4)
S(1)—P(1)—C(1)116.221 (7)C(24)—C(25)—C(26)119.82 (2)
S(1)—P(1)—C(15)112.524 (6)C(24)—C(25)—H(25)120.32 (2)
S(1)—P(1)—C(21)113.043 (6)C(26)—C(25)—H(25)119.862 (16)
C(1)—P(1)—C(15)108.998 (7)C(21)—C(26)—C(25)120.189 (15)
C(1)—P(1)—C(21)103.057 (7)C(21)—C(26)—H(26)120.369 (15)
C(15)—P(1)—C(21)101.644 (7)C(25)—C(26)—H(26)119.336 (15)
S(2)—P(2)—C(27)113.916 (7)P(2)—C(27)—C(28)120.605 (12)
S(2)—P(2)—C(41)112.831 (7)P(2)—C(27)—C(40)119.759 (12)
S(2)—P(2)—C(47)112.920 (11)C(28)—C(27)—C(40)119.531 (14)
C(27)—P(2)—C(41)108.132 (8)C(27)—C(28)—C(29)123.988 (14)
C(27)—P(2)—C(47)107.162 (12)C(27)—C(28)—C(33)119.032 (14)
C(41)—P(2)—C(47)100.935 (11)C(29)—C(28)—C(33)116.819 (14)
P(1)—C(1)—C(2)116.848 (11)C(28)—C(29)—C(30)121.262 (15)
P(1)—C(1)—C(14)123.468 (11)C(28)—C(29)—H(29)120.393 (14)
C(2)—C(1)—C(14)119.586 (14)C(30)—C(29)—H(29)118.228 (15)
C(1)—C(2)—C(3)123.399 (14)C(29)—C(30)—C(31)121.083 (15)
C(1)—C(2)—C(7)119.466 (14)C(29)—C(30)—H(30)119.095 (16)
C(3)—C(2)—C(7)117.127 (14)C(31)—C(30)—H(30)119.811 (16)
C(2)—C(3)—C(4)121.196 (15)C(30)—C(31)—C(32)119.826 (15)
C(2)—C(3)—H(3)119.501 (14)C(30)—C(31)—H(31)120.011 (16)
C(4)—C(3)—H(3)119.219 (15)C(32)—C(31)—H(31)120.123 (17)
C(3)—C(4)—C(5)120.987 (19)C(31)—C(32)—C(33)120.522 (15)
C(3)—C(4)—H(4)119.458 (16)C(31)—C(32)—H(32)122.444 (16)
C(5)—C(4)—H(4)119.540 (19)C(33)—C(32)—H(32)117.007 (15)
C(4)—C(5)—C(6)119.86 (3)C(28)—C(33)—C(32)120.210 (15)
C(4)—C(5)—H(5)118.61 (3)C(28)—C(33)—C(34)119.811 (15)
C(6)—C(5)—H(5)121.39 (3)C(32)—C(33)—C(34)119.946 (15)
C(5)—C(6)—C(7)120.63 (2)C(33)—C(34)—C(35)121.258 (16)
C(5)—C(6)—H(6)122.69 (2)C(33)—C(34)—H(34)119.764 (15)
C(7)—C(6)—H(6)116.625 (15)C(35)—C(34)—H(34)118.838 (15)
C(2)—C(7)—C(6)119.910 (14)C(34)—C(35)—C(36)120.135 (15)
C(2)—C(7)—C(8)119.493 (14)C(34)—C(35)—C(40)119.703 (15)
C(6)—C(7)—C(8)120.590 (15)C(36)—C(35)—C(40)120.132 (15)
C(7)—C(8)—C(9)121.298 (16)C(35)—C(36)—C(37)120.661 (16)
C(7)—C(8)—H(8)118.118 (14)C(35)—C(36)—H(36)117.857 (16)
C(9)—C(8)—H(8)120.451 (14)C(37)—C(36)—H(36)121.461 (16)
C(8)—C(9)—C(10)119.796 (14)C(36)—C(37)—C(38)119.674 (15)
C(8)—C(9)—C(14)120.026 (14)C(36)—C(37)—H(37)121.457 (18)
C(10)—C(9)—C(14)120.160 (14)C(38)—C(37)—H(37)118.835 (17)
C(9)—C(10)—C(11)121.084 (15)C(37)—C(38)—C(39)121.128 (16)
C(9)—C(10)—H(10)117.636 (14)C(37)—C(38)—H(38)119.556 (16)
C(11)—C(10)—H(10)121.206 (15)C(39)—C(38)—H(38)119.307 (18)
C(10)—C(11)—C(12)119.183 (14)C(38)—C(39)—C(40)121.214 (16)
C(10)—C(11)—H(11)121.255 (16)C(38)—C(39)—H(39)119.530 (16)
C(12)—C(11)—H(11)119.456 (16)C(40)—C(39)—H(39)119.034 (15)
C(11)—C(12)—C(13)121.435 (15)C(27)—C(40)—C(35)119.306 (14)
C(11)—C(12)—H(12)118.688 (15)C(27)—C(40)—C(39)123.574 (15)
C(13)—C(12)—H(12)119.818 (16)C(35)—C(40)—C(39)116.975 (14)
C(12)—C(13)—C(14)121.316 (15)P(2)—C(41)—C(42)121.867 (13)
C(12)—C(13)—H(13)119.798 (15)P(2)—C(41)—C(46)118.492 (18)
C(14)—C(13)—H(13)118.696 (14)C(42)—C(41)—C(46)119.47 (2)
C(1)—C(14)—C(9)118.927 (14)C(41)—C(42)—C(43)119.95 (2)
C(1)—C(14)—C(13)124.213 (14)C(41)—C(42)—H(42)121.652 (15)
C(9)—C(14)—C(13)116.776 (14)C(43)—C(42)—H(42)118.40 (2)
P(1)—C(15)—C(16)120.801 (12)C(42)—C(43)—C(44)120.43 (3)
P(1)—C(15)—C(20)119.383 (12)C(42)—C(43)—H(43)118.93 (3)
C(16)—C(15)—C(20)119.742 (15)C(44)—C(43)—H(43)120.64 (3)
C(15)—C(16)—C(17)120.132 (15)C(43)—C(44)—C(45)119.81 (3)
C(15)—C(16)—H(16)120.681 (15)C(43)—C(44)—H(44)119.66 (4)
C(17)—C(16)—H(16)119.171 (15)C(45)—C(44)—H(44)120.53 (3)
C(16)—C(17)—C(18)120.010 (15)C(44)—C(45)—C(46)120.08 (3)
C(16)—C(17)—H(17)119.563 (15)C(44)—C(45)—H(45)120.52 (3)
C(18)—C(17)—H(17)120.427 (15)C(46)—C(45)—H(45)119.40 (4)
C(17)—C(18)—C(19)120.007 (14)C(41)—C(46)—C(45)120.24 (3)
C(17)—C(18)—H(18)119.611 (15)C(41)—C(46)—H(46)118.83 (3)
C(19)—C(18)—H(18)120.374 (15)C(45)—C(46)—H(46)120.93 (3)
C(18)—C(19)—C(20)120.202 (14)P(2)—C(47)—C(48)118.50 (3)
C(18)—C(19)—H(19)120.249 (14)P(2)—C(47)—C(52)121.89 (3)
C(20)—C(19)—H(19)119.549 (15)C(48)—C(47)—C(52)119.58 (4)
C(15)—C(20)—C(19)119.891 (15)C(47)—C(48)—C(49)120.09 (4)
C(15)—C(20)—H(20)119.616 (14)C(47)—C(48)—H(48)119.08 (4)
C(19)—C(20)—H(20)120.492 (15)C(49)—C(48)—H(48)120.83 (4)
P(1)—C(21)—C(22)119.096 (12)C(48)—C(49)—C(50)120.35 (4)
P(1)—C(21)—C(26)121.184 (12)C(48)—C(49)—H(49)119.14 (5)
C(22)—C(21)—C(26)119.707 (16)C(50)—C(49)—H(49)120.50 (4)
C(21)—C(22)—C(23)120.020 (16)C(49)—C(50)—C(51)119.66 (4)
C(21)—C(22)—H(22)118.942 (15)C(49)—C(50)—H(50)120.75 (4)
C(23)—C(22)—H(22)120.997 (15)C(51)—C(50)—H(50)119.60 (4)
C(22)—C(23)—C(24)120.067 (19)C(50)—C(51)—C(52)120.45 (4)
C(22)—C(23)—H(23)119.773 (17)C(50)—C(51)—H(51)120.37 (4)
C(24)—C(23)—H(23)120.15 (2)C(52)—C(51)—H(51)119.18 (4)
C(23)—C(24)—C(25)120.17 (3)C(47)—C(52)—C(51)119.87 (4)
C(23)—C(24)—H(24)120.27 (3)C(47)—C(52)—H(52)120.98 (3)
C(25)—C(24)—H(24)119.56 (3)C(51)—C(52)—H(52)119.10 (4)

Experimental details

(1_corr)(1_filter)(1_uncorr)(2_corr)
Crystal data
Chemical formulaC28H18N2C28H18N2C28H18N2C12H4N4
Mr382.44382.44382.44204.19
Crystal system, space groupMonoclinic, C2/cMonoclinic, C2/cMonoclinic, C2/cMonoclinic, C2/c
Temperature (K)100100100100
a, b, c (Å)13.5559 (13), 12.2134 (12), 12.6643 (12)13.5537 (16), 12.2132 (15), 12.6619 (15)13.5559 (13), 12.2134 (12), 12.6643 (12)8.896 (2), 6.9130 (19), 16.439 (5)
α, β, γ (°)90, 118.8339 (17), 9090, 118.836 (2), 9090, 118.8339 (17), 9090, 98.290 (3), 90
V3)1836.8 (3)1836.1 (4)1836.8 (3)1000.5 (5)
Z4444
Radiation typeMo KαMo KαMo KαMo Kα
µ (mm1)0.080.080.080.09
Crystal size (mm)0.32 × 0.25 × 0.100.32 × 0.25 × 0.100.32 × 0.25 × 0.100.18 × 0.13 × 0.06
Data collection
DiffractometerBruker Smart APEX II QuazarBruker Smart APEX II QuazarBruker Smart APEX II QuazarBruker Smart APEX II Quazar
Absorption correctionMulti-scan
SADABS2015/1
Multi-scan
SADABS2015/1
Multi-scan
SADABS2015/1
Multi-scan
SADABS2015/1
Tmin, Tmax0.709, 0.7450.706, 0.7450.709, 0.7450.718, 0.746
No. of measured, independent and
observed reflections
1697, 1697, 1530 [I > 2σ(I)]14259, 1707, 1549 [I > 2σ(I)]14302, 1697, 1547 [I > 2σ(I)]1543, 1543, 1442 [I > 2σ(I)]
Rint?0.0260.025?
(sin θ/λ)max1)0.6060.6070.6060.718
Refinement
R[F2 > 2σ(F2)], wR(F2), S 0.040, 0.111, 1.09 0.039, 0.111, 1.10 0.043, 0.127, 1.12 0.034, 0.096, 1.09
No. of reflections1697170716971543
No. of parameters13713613674
No. of restraints1231231230
H-atom treatmentH-atom parameters constrainedH-atom parameters constrainedH-atom parameters constrainedH-atom parameters constrained
Δρmax, Δρmin (e Å3)0.27, 0.180.27, 0.190.24, 0.200.46, 0.17
Absolute structure????
Absolute structure parameter????


(2_filter)(2_uncorr)(3_corr)(3_filter)
Crystal data
Chemical formulaC12H4N4C12H4N4C18H17CuO6C18H17CuO6
Mr204.19204.19392.86392.86
Crystal system, space groupMonoclinic, C2/cMonoclinic, C2/cMonoclinic, C2/cMonoclinic, C2/c
Temperature (K)100100100100
a, b, c (Å)8.8840 (12), 6.9036 (9), 16.421 (2)8.896 (2), 6.9130 (19), 16.439 (5)9.7935 (7), 19.0055 (13), 18.2997 (13)9.7936 (7), 18.9973 (12), 18.2982 (12)
α, β, γ (°)90, 98.241 (2), 9090, 98.290 (3), 9090, 94.7996 (11), 9090, 94.840 (1), 90
V3)996.7 (2)1000.5 (5)3394.2 (4)3392.3 (4)
Z4488
Radiation typeMo KαMo KαMo KαMo Kα
µ (mm1)0.090.091.321.32
Crystal size (mm)0.18 × 0.13 × 0.060.18 × 0.13 × 0.060.14 × 0.10 × 0.050.14 × 0.10 × 0.05
Data collection
DiffractometerBruker Smart APEX II QuazarBruker Smart APEX II QuazarBruker Smart APEX II QuazarBruker Smart APEX II Quazar
Absorption correctionMulti-scan
SADABS2015/1
Multi-scan
SADABS2015/1
Multi-scan
SADABS2015/1
Multi-scan
SADABS2015/1
Tmin, Tmax0.718, 0.7460.718, 0.7460.695, 0.7460.694, 0.746
No. of measured, independent and
observed reflections
10375, 1545, 1432 [I > 2σ(I)]10353, 1543, 1447 [I > 2σ(I)]4282, 4282, 3719 [I > 2σ(I)]29137, 4233, 3574 [I > 2σ(I)]
Rint0.0160.015?0.033
(sin θ/λ)max1)0.7190.7180.6700.668
Refinement
R[F2 > 2σ(F2)], wR(F2), S 0.034, 0.099, 1.08 0.036, 0.108, 1.09 0.026, 0.065, 1.03 0.028, 0.068, 1.03
No. of reflections1545154342824233
No. of parameters7373301300
No. of restraints00652652
H-atom treatmentH-atom parameters constrainedH-atom parameters constrainedH-atom parameters constrainedH-atom parameters constrained
Δρmax, Δρmin (e Å3)0.47, 0.190.47, 0.160.36, 0.300.34, 0.29
Absolute structure????
Absolute structure parameter????


(3_uncorr)(4_corr)(4_filter)(4_uncorr)
Crystal data
Chemical formulaC18H17CuO6C34H26MgN4O4C34H26MgN4O4C34H26MgN4O4
Mr392.86578.90578.90578.90
Crystal system, space groupMonoclinic, C2/cMonoclinic, P21/nMonoclinic, P21/nMonoclinic, P21/n
Temperature (K)100100100100
a, b, c (Å)9.7935 (7), 19.0055 (13), 18.2997 (13)11.3068 (12), 14.9595 (16), 16.7252 (17)11.3182 (14), 14.9745 (18), 16.744 (2)11.3068 (12), 14.9595 (16), 16.7252 (17)
α, β, γ (°)90, 94.7996 (11), 9090, 93.0500 (15), 9090, 93.044 (2), 9090, 93.0500 (15), 90
V3)3394.2 (4)2825.0 (5)2833.9 (6)2825.0 (5)
Z8444
Radiation typeMo KαMo KαMo KαMo Kα
µ (mm1)1.320.110.110.11
Crystal size (mm)0.14 × 0.10 × 0.050.19 × 0.15 × 0.110.19 × 0.15 × 0.110.19 × 0.15 × 0.11
Data collection
DiffractometerBruker Smart APEX II QuazarBruker Smart APEX II UltraBruker Smart APEX II UltraBruker Smart APEX II Ultra
Absorption correctionMulti-scan
SADABS2015/1
Multi-scan
SADABS2015/1
Multi-scan
SADABS2015/1
Multi-scan
SADABS2015/1
Tmin, Tmax0.695, 0.7460.688, 0.7460.679, 0.7460.688, 0.746
No. of measured, independent and
observed reflections
29203, 4282, 3723 [I > 2σ(I)]8694, 8694, 7486 [I > 2σ(I)]36495, 8866, 7421 [I > 2σ(I)]36155, 8694, 7463 [I > 2σ(I)]
Rint0.028?0.0310.027
(sin θ/λ)max1)0.6700.7170.7210.717
Refinement
R[F2 > 2σ(F2)], wR(F2), S 0.027, 0.070, 1.07 0.040, 0.109, 1.02 0.040, 0.111, 1.03 0.041, 0.115, 1.03
No. of reflections4282869488668694
No. of parameters300393392392
No. of restraints652408408408
H-atom treatmentH-atom parameters constrainedH-atom parameters constrainedH-atom parameters constrainedH-atom parameters constrained
Δρmax, Δρmin (e Å3)0.39, 0.280.53, 0.250.45, 0.260.53, 0.25
Absolute structure????
Absolute structure parameter????


(5_corr)(5_filter)(5_uncorr)(spanh_3lcorr)
Crystal data
Chemical formulaC11H10O2SC11H10O2SC11H10O2SC26H19PS
Mr206.25206.25206.25394.44
Crystal system, space groupOrthorhombic, P212121Orthorhombic, P212121Orthorhombic, P212121Triclinic, P1
Temperature (K)293293293100
a, b, c (Å)5.9633 (1), 9.0417 (2), 18.4007 (4)5.9641 (2), 9.0419 (2), 18.4027 (5)5.9633 (1), 9.0417 (2), 18.4007 (4)10.215 (2), 12.322 (2), 17.351 (3)
α, β, γ (°)90, 90, 9090, 90, 9090, 90, 90101.57 (2), 91.25 (2), 112.02 (2)
V3)992.14 (3)992.40 (5)992.14 (3)1972.2 (7)
Z4444
Radiation typeMo KαMo KαMo KαMo Kα
µ (mm1)0.290.290.290.25
Crystal size (mm)0.25 (radius)0.25 (radius)0.25 (radius)0.15 × 0.10 × 0.10
Data collection
DiffractometerBruker Smart APEX II QuazarBruker Smart APEX II QuazarBruker Smart APEX II QuazarBruker Smart APEX II Quazar
Absorption correctionMulti-scan
SADABS2015/1
Multi-scan
SADABS2015/1
Multi-scan
SADABS2015/1
Multi-scan
SADABS2015/1
Tmin, Tmax0.710, 0.7460.712, 0.7460.710, 0.7460.716, 0.750
No. of measured, independent and
observed reflections
2456, 2456, 2398 [I > 2σ(I)]15101, 2453, 2383 [I > 2σ(I)]15091, 2456, 2397 [I > 2σ(I)]272253, 45758, 38346 (?)
Rint?0.0200.0200.021
(sin θ/λ)max1)0.6670.6670.6671.123
Refinement
R[F2 > 2σ(F2)], wR(F2), S 0.025, 0.067, 1.08 0.025, 0.067, 1.11 0.025, 0.068, 1.09 0.02, 0.021, 1.40
No. of reflections24562453245643155
No. of parameters130129129815
No. of restraints0000
H-atom treatmentH-atom parameters constrainedH-atom parameters constrainedH-atom parameters constrainedH-atom parameters constrained
Δρmax, Δρmin (e Å3)0.22, 0.180.21, 0.190.22, 0.200.30, 0.21
Absolute structureFlack x determined using 978 quotients [(I+)-(I-)]/[(I+)+(I-)] (Parsons, Flack and Wagner, Acta Cryst. B69 (2013) 249-259).Flack x determined using 969 quotients [(I+)-(I-)]/[(I+)+(I-)] (Parsons, Flack and Wagner, Acta Cryst. B69 (2013) 249-259).Flack x determined using 976 quotients [(I+)-(I-)]/[(I+)+(I-)] (Parsons, Flack and Wagner, Acta Cryst. B69 (2013) 249-259).?
Absolute structure parameter0.035 (15)0.049 (16)0.034 (14)?


(spanh_3lnocorr)
Crystal data
Chemical formulaC26H19PS
Mr394.44
Crystal system, space groupTriclinic, P1
Temperature (K)100
a, b, c (Å)10.215 (2), 12.322 (2), 17.351 (3)
α, β, γ (°)101.57 (2), 91.25 (2), 112.02 (2)
V3)1972.2 (7)
Z4
Radiation typeMo Kα
µ (mm1)0.25
Crystal size (mm)0.15 × 0.10 × 0.10
Data collection
DiffractometerBruker Smart APEX II Quazar
Absorption correctionMulti-scan
SADABS2015/1
Tmin, Tmax0.716, 0.750
No. of measured, independent and
observed reflections
272253, 45758, 38346 (?)
Rint0.021
(sin θ/λ)max1)1.123
Refinement
R[F2 > 2σ(F2)], wR(F2), S 0.021, 0.025, 1.67
No. of reflections43292
No. of parameters815
No. of restraints0
H-atom treatmentH-atom parameters constrained
Δρmax, Δρmin (e Å3)0.29, 0.21
Absolute structure?
Absolute structure parameter?

Computer programs: APEX2 v2012.2, SAINT V8.30C, SAINT V8.34A, SHELXT (G.M.Sheldrick, Acta Cryst.(2015)A71, 3-8), SHELXL2014/7 (Sheldrick, 2014), Volkov et al., (2006), Mercury CSD 3.3 (Build RC5).

Selected geometric parameters (Å, º) for (spanh_3lcorr) top
S(1)—P(1)1.9552 (1)C(24)—H(24)1.0830 (3)
S(2)—P(2)1.9482 (1)C(25)—C(26)1.3882 (2)
P(1)—C(1)1.8267 (2)C(25)—H(25)1.0830 (1)
P(1)—C(15)1.8234 (2)C(26)—H(26)1.0830 (1)
P(1)—C(21)1.8237 (2)C(27)—C(28)1.4236 (2)
P(2)—C(27)1.8267 (2)C(27)—C(40)1.4231 (2)
P(2)—C(41)1.8268 (2)C(28)—C(29)1.4363 (2)
P(2)—C(47)1.8247 (3)C(28)—C(33)1.4399 (2)
C(1)—C(2)1.4221 (2)C(29)—C(30)1.3695 (2)
C(1)—C(14)1.4211 (2)C(29)—H(29)1.0830 (1)
C(2)—C(3)1.4333 (2)C(30)—C(31)1.4227 (2)
C(2)—C(7)1.4362 (2)C(30)—H(30)1.0830 (1)
C(3)—C(4)1.3668 (2)C(31)—C(32)1.3665 (2)
C(3)—H(3)1.0830 (1)C(31)—H(31)1.0830 (1)
C(4)—C(5)1.4230 (3)C(32)—C(33)1.4291 (2)
C(4)—H(4)1.0830 (1)C(32)—H(32)1.0830 (1)
C(5)—C(6)1.3618 (3)C(33)—C(34)1.3978 (2)
C(5)—H(5)1.0830 (3)C(34)—C(35)1.3951 (2)
C(6)—C(7)1.4305 (2)C(34)—H(34)1.0830 (1)
C(6)—H(6)1.0830 (1)C(35)—C(36)1.4296 (2)
C(7)—C(8)1.3929 (2)C(35)—C(40)1.4383 (2)
C(8)—C(9)1.3962 (2)C(36)—C(37)1.3643 (2)
C(8)—H(8)1.0830 (1)C(36)—H(36)1.0830 (2)
C(9)—C(10)1.4256 (2)C(37)—C(38)1.4233 (2)
C(9)—C(14)1.4381 (2)C(37)—H(37)1.0830 (1)
C(10)—C(11)1.3638 (2)C(38)—C(39)1.3712 (2)
C(10)—H(10)1.0830 (1)C(38)—H(38)1.0830 (2)
C(11)—C(12)1.4198 (2)C(39)—C(40)1.4327 (2)
C(11)—H(11)1.0830 (1)C(39)—H(39)1.0830 (1)
C(12)—C(13)1.3695 (2)C(41)—C(42)1.3977 (2)
C(12)—H(12)1.0830 (1)C(41)—C(46)1.3957 (3)
C(13)—C(14)1.4302 (2)C(42)—C(43)1.3911 (3)
C(13)—H(13)1.0830 (1)C(42)—H(42)1.0830 (2)
C(15)—C(16)1.4011 (2)C(43)—C(44)1.3892 (4)
C(15)—C(20)1.3951 (2)C(43)—H(43)1.0830 (3)
C(16)—C(17)1.3907 (2)C(44)—C(45)1.3912 (5)
C(16)—H(16)1.0830 (1)C(44)—H(44)1.0830 (3)
C(17)—C(18)1.3960 (2)C(45)—C(46)1.3923 (4)
C(17)—H(17)1.0830 (1)C(45)—H(45)1.0830 (3)
C(18)—C(19)1.3900 (2)C(46)—H(46)1.0830 (3)
C(18)—H(18)1.0830 (1)C(47)—C(48)1.3935 (4)
C(19)—C(20)1.3978 (2)C(47)—C(52)1.4003 (4)
C(19)—H(19)1.0830 (1)C(48)—C(49)1.3940 (5)
C(20)—H(20)1.0830 (1)C(48)—H(48)1.0830 (4)
C(21)—C(22)1.3920 (2)C(49)—C(50)1.3867 (6)
C(21)—C(26)1.3994 (2)C(49)—H(49)1.0830 (3)
C(22)—C(23)1.3934 (2)C(50)—C(51)1.3946 (5)
C(22)—H(22)1.0830 (1)C(50)—H(50)1.0830 (3)
C(23)—C(24)1.3882 (3)C(51)—C(52)1.3897 (4)
C(23)—H(23)1.0830 (1)C(51)—H(51)1.0830 (4)
C(24)—C(25)1.3946 (3)C(52)—H(52)1.0830 (3)
S(1)—P(1)—C(1)116.214 (6)C(24)—C(25)—C(26)119.811 (17)
S(1)—P(1)—C(15)112.519 (5)C(24)—C(25)—H(25)120.335 (17)
S(1)—P(1)—C(21)113.049 (5)C(26)—C(25)—H(25)119.854 (13)
C(1)—P(1)—C(15)109.001 (6)C(21)—C(26)—C(25)120.187 (13)
C(1)—P(1)—C(21)103.063 (6)C(21)—C(26)—H(26)120.372 (12)
C(15)—P(1)—C(21)101.643 (6)C(25)—C(26)—H(26)119.333 (13)
S(2)—P(2)—C(27)113.915 (6)P(2)—C(27)—C(28)120.614 (10)
S(2)—P(2)—C(41)112.833 (6)P(2)—C(27)—C(40)119.759 (10)
S(2)—P(2)—C(47)112.932 (9)C(28)—C(27)—C(40)119.522 (12)
C(27)—P(2)—C(41)108.136 (6)C(27)—C(28)—C(29)123.990 (12)
C(27)—P(2)—C(47)107.147 (10)C(27)—C(28)—C(33)119.031 (12)
C(41)—P(2)—C(47)100.932 (9)C(29)—C(28)—C(33)116.821 (12)
P(1)—C(1)—C(2)116.845 (9)C(28)—C(29)—C(30)121.274 (13)
P(1)—C(1)—C(14)123.470 (9)C(28)—C(29)—H(29)120.389 (12)
C(2)—C(1)—C(14)119.587 (12)C(30)—C(29)—H(29)118.221 (12)
C(1)—C(2)—C(3)123.406 (12)C(29)—C(30)—C(31)121.077 (13)
C(1)—C(2)—C(7)119.461 (12)C(29)—C(30)—H(30)119.101 (14)
C(3)—C(2)—C(7)117.125 (12)C(31)—C(30)—H(30)119.811 (13)
C(2)—C(3)—C(4)121.196 (12)C(30)—C(31)—C(32)119.824 (13)
C(2)—C(3)—H(3)119.497 (12)C(30)—C(31)—H(31)120.021 (14)
C(4)—C(3)—H(3)119.224 (12)C(32)—C(31)—H(31)120.116 (14)
C(3)—C(4)—C(5)120.999 (16)C(31)—C(32)—C(33)120.536 (13)
C(3)—C(4)—H(4)119.445 (13)C(31)—C(32)—H(32)122.438 (13)
C(5)—C(4)—H(4)119.542 (16)C(33)—C(32)—H(32)116.997 (13)
C(4)—C(5)—C(6)119.85 (2)C(28)—C(33)—C(32)120.192 (12)
C(4)—C(5)—H(5)118.62 (3)C(28)—C(33)—C(34)119.824 (12)
C(6)—C(5)—H(5)121.40 (3)C(32)—C(33)—C(34)119.950 (12)
C(5)—C(6)—C(7)120.635 (17)C(33)—C(34)—C(35)121.250 (13)
C(5)—C(6)—H(6)122.684 (17)C(33)—C(34)—H(34)119.772 (12)
C(7)—C(6)—H(6)116.630 (13)C(35)—C(34)—H(34)118.839 (12)
C(2)—C(7)—C(6)119.911 (12)C(34)—C(35)—C(36)120.135 (13)
C(2)—C(7)—C(8)119.505 (12)C(34)—C(35)—C(40)119.711 (12)
C(6)—C(7)—C(8)120.575 (12)C(36)—C(35)—C(40)120.123 (12)
C(7)—C(8)—C(9)121.285 (13)C(35)—C(36)—C(37)120.667 (13)
C(7)—C(8)—H(8)118.138 (12)C(35)—C(36)—H(36)117.848 (13)
C(9)—C(8)—H(8)120.443 (12)C(37)—C(36)—H(36)121.464 (13)
C(8)—C(9)—C(10)119.804 (12)C(36)—C(37)—C(38)119.671 (13)
C(8)—C(9)—C(14)120.032 (12)C(36)—C(37)—H(37)121.465 (15)
C(10)—C(9)—C(14)120.146 (12)C(38)—C(37)—H(37)118.829 (14)
C(9)—C(10)—C(11)121.092 (12)C(37)—C(38)—C(39)121.145 (13)
C(9)—C(10)—H(10)117.614 (12)C(37)—C(38)—H(38)119.554 (14)
C(11)—C(10)—H(10)121.219 (12)C(39)—C(38)—H(38)119.293 (15)
C(10)—C(11)—C(12)119.188 (12)C(38)—C(39)—C(40)121.192 (13)
C(10)—C(11)—H(11)121.258 (13)C(38)—C(39)—H(39)119.553 (13)
C(12)—C(11)—H(11)119.448 (13)C(40)—C(39)—H(39)119.035 (12)
C(11)—C(12)—C(13)121.432 (12)C(27)—C(40)—C(35)119.306 (12)
C(11)—C(12)—H(12)118.701 (13)C(27)—C(40)—C(39)123.562 (12)
C(13)—C(12)—H(12)119.809 (13)C(35)—C(40)—C(39)116.988 (12)
C(12)—C(13)—C(14)121.306 (12)P(2)—C(41)—C(42)121.864 (11)
C(12)—C(13)—H(13)119.795 (12)P(2)—C(41)—C(46)118.490 (15)
C(14)—C(13)—H(13)118.708 (12)C(42)—C(41)—C(46)119.472 (18)
C(1)—C(14)—C(9)118.923 (11)C(41)—C(42)—C(43)119.949 (18)
C(1)—C(14)—C(13)124.203 (12)C(41)—C(42)—H(42)121.654 (13)
C(9)—C(14)—C(13)116.790 (12)C(43)—C(42)—H(42)118.394 (18)
P(1)—C(15)—C(16)120.795 (10)C(42)—C(43)—C(44)120.43 (3)
P(1)—C(15)—C(20)119.390 (10)C(42)—C(43)—H(43)118.95 (3)
C(16)—C(15)—C(20)119.742 (13)C(44)—C(43)—H(43)120.63 (3)
C(15)—C(16)—C(17)120.117 (13)C(43)—C(44)—C(45)119.82 (3)
C(15)—C(16)—H(16)120.686 (12)C(43)—C(44)—H(44)119.64 (3)
C(17)—C(16)—H(16)119.181 (13)C(45)—C(44)—H(44)120.54 (3)
C(16)—C(17)—C(18)120.038 (12)C(44)—C(45)—C(46)120.05 (3)
C(16)—C(17)—H(17)119.555 (13)C(44)—C(45)—H(45)120.52 (3)
C(18)—C(17)—H(17)120.407 (12)C(46)—C(45)—H(45)119.43 (3)
C(17)—C(18)—C(19)119.987 (12)C(41)—C(46)—C(45)120.27 (3)
C(17)—C(18)—H(18)119.624 (13)C(41)—C(46)—H(46)118.85 (2)
C(19)—C(18)—H(18)120.380 (13)C(45)—C(46)—H(46)120.88 (3)
C(18)—C(19)—C(20)120.206 (12)P(2)—C(47)—C(48)118.47 (2)
C(18)—C(19)—H(19)120.251 (12)P(2)—C(47)—C(52)121.91 (2)
C(20)—C(19)—H(19)119.542 (13)C(48)—C(47)—C(52)119.58 (3)
C(15)—C(20)—C(19)119.894 (13)C(47)—C(48)—C(49)120.11 (3)
C(15)—C(20)—H(20)119.613 (12)C(47)—C(48)—H(48)119.11 (3)
C(19)—C(20)—H(20)120.493 (12)C(49)—C(48)—H(48)120.78 (3)
P(1)—C(21)—C(22)119.087 (10)C(48)—C(49)—C(50)120.33 (3)
P(1)—C(21)—C(26)121.181 (10)C(48)—C(49)—H(49)119.17 (4)
C(22)—C(21)—C(26)119.718 (13)C(50)—C(49)—H(49)120.50 (3)
C(21)—C(22)—C(23)120.000 (13)C(49)—C(50)—C(51)119.68 (3)
C(21)—C(22)—H(22)118.958 (13)C(49)—C(50)—H(50)120.75 (3)
C(23)—C(22)—H(22)121.001 (13)C(51)—C(50)—H(50)119.57 (4)
C(22)—C(23)—C(24)120.078 (16)C(50)—C(51)—C(52)120.39 (3)
C(22)—C(23)—H(23)119.757 (14)C(50)—C(51)—H(51)120.41 (3)
C(24)—C(23)—H(23)120.156 (17)C(52)—C(51)—H(51)119.20 (3)
C(23)—C(24)—C(25)120.18 (2)C(47)—C(52)—C(51)119.91 (3)
C(23)—C(24)—H(24)120.27 (2)C(47)—C(52)—H(52)120.99 (3)
C(25)—C(24)—H(24)119.56 (3)C(51)—C(52)—H(52)119.05 (3)
Selected geometric parameters (Å, º) for (spanh_3lnocorr) top
S(1)—P(1)1.9552 (1)C(24)—H(24)1.0830 (4)
S(2)—P(2)1.9481 (1)C(25)—C(26)1.3880 (2)
P(1)—C(1)1.8266 (2)C(25)—H(25)1.0830 (2)
P(1)—C(15)1.8235 (2)C(26)—H(26)1.0830 (2)
P(1)—C(21)1.8237 (2)C(27)—C(28)1.4237 (2)
P(2)—C(27)1.8268 (2)C(27)—C(40)1.4229 (2)
P(2)—C(41)1.8268 (2)C(28)—C(29)1.4364 (2)
P(2)—C(47)1.8245 (4)C(28)—C(33)1.4399 (2)
C(1)—C(2)1.4222 (2)C(29)—C(30)1.3696 (2)
C(1)—C(14)1.4210 (2)C(29)—H(29)1.0830 (2)
C(2)—C(3)1.4333 (2)C(30)—C(31)1.4229 (2)
C(2)—C(7)1.4364 (2)C(30)—H(30)1.0830 (2)
C(3)—C(4)1.3667 (2)C(31)—C(32)1.3665 (2)
C(3)—H(3)1.0830 (2)C(31)—H(31)1.0830 (2)
C(4)—C(5)1.4231 (4)C(32)—C(33)1.4290 (2)
C(4)—H(4)1.0830 (2)C(32)—H(32)1.0830 (2)
C(5)—C(6)1.3617 (4)C(33)—C(34)1.3979 (2)
C(5)—H(5)1.0830 (3)C(34)—C(35)1.3950 (2)
C(6)—C(7)1.4304 (2)C(34)—H(34)1.0830 (2)
C(6)—H(6)1.0830 (2)C(35)—C(36)1.4295 (2)
C(7)—C(8)1.3930 (2)C(35)—C(40)1.4385 (2)
C(8)—C(9)1.3961 (2)C(36)—C(37)1.3646 (3)
C(8)—H(8)1.0830 (2)C(36)—H(36)1.0830 (2)
C(9)—C(10)1.4253 (2)C(37)—C(38)1.4233 (3)
C(9)—C(14)1.4382 (2)C(37)—H(37)1.0830 (2)
C(10)—C(11)1.3640 (2)C(38)—C(39)1.3714 (2)
C(10)—H(10)1.0830 (2)C(38)—H(38)1.0830 (2)
C(11)—C(12)1.4199 (2)C(39)—C(40)1.4326 (2)
C(11)—H(11)1.0830 (2)C(39)—H(39)1.0830 (2)
C(12)—C(13)1.3693 (2)C(41)—C(42)1.3977 (2)
C(12)—H(12)1.0830 (2)C(41)—C(46)1.3961 (4)
C(13)—C(14)1.4302 (2)C(42)—C(43)1.3912 (4)
C(13)—H(13)1.0830 (2)C(42)—H(42)1.0830 (2)
C(15)—C(16)1.4010 (2)C(43)—C(44)1.3887 (5)
C(15)—C(20)1.3951 (2)C(43)—H(43)1.0830 (4)
C(16)—C(17)1.3908 (2)C(44)—C(45)1.3910 (6)
C(16)—H(16)1.0830 (2)C(44)—H(44)1.0830 (4)
C(17)—C(18)1.3959 (2)C(45)—C(46)1.3919 (5)
C(17)—H(17)1.0830 (2)C(45)—H(45)1.0830 (4)
C(18)—C(19)1.3900 (2)C(46)—H(46)1.0830 (4)
C(18)—H(18)1.0830 (2)C(47)—C(48)1.3938 (5)
C(19)—C(20)1.3977 (2)C(47)—C(52)1.4010 (5)
C(19)—H(19)1.0830 (2)C(48)—C(49)1.3937 (6)
C(20)—H(20)1.0830 (2)C(48)—H(48)1.0830 (4)
C(21)—C(22)1.3920 (2)C(49)—C(50)1.3865 (7)
C(21)—C(26)1.3994 (2)C(49)—H(49)1.0830 (4)
C(22)—C(23)1.3932 (2)C(50)—C(51)1.3942 (6)
C(22)—H(22)1.0830 (2)C(50)—H(50)1.0830 (4)
C(23)—C(24)1.3883 (4)C(51)—C(52)1.3889 (5)
C(23)—H(23)1.0830 (2)C(51)—H(51)1.0830 (4)
C(24)—C(25)1.3947 (4)C(52)—H(52)1.0830 (4)
S(1)—P(1)—C(1)116.221 (7)C(24)—C(25)—C(26)119.82 (2)
S(1)—P(1)—C(15)112.524 (6)C(24)—C(25)—H(25)120.32 (2)
S(1)—P(1)—C(21)113.043 (6)C(26)—C(25)—H(25)119.862 (16)
C(1)—P(1)—C(15)108.998 (7)C(21)—C(26)—C(25)120.189 (15)
C(1)—P(1)—C(21)103.057 (7)C(21)—C(26)—H(26)120.369 (15)
C(15)—P(1)—C(21)101.644 (7)C(25)—C(26)—H(26)119.336 (15)
S(2)—P(2)—C(27)113.916 (7)P(2)—C(27)—C(28)120.605 (12)
S(2)—P(2)—C(41)112.831 (7)P(2)—C(27)—C(40)119.759 (12)
S(2)—P(2)—C(47)112.920 (11)C(28)—C(27)—C(40)119.531 (14)
C(27)—P(2)—C(41)108.132 (8)C(27)—C(28)—C(29)123.988 (14)
C(27)—P(2)—C(47)107.162 (12)C(27)—C(28)—C(33)119.032 (14)
C(41)—P(2)—C(47)100.935 (11)C(29)—C(28)—C(33)116.819 (14)
P(1)—C(1)—C(2)116.848 (11)C(28)—C(29)—C(30)121.262 (15)
P(1)—C(1)—C(14)123.468 (11)C(28)—C(29)—H(29)120.393 (14)
C(2)—C(1)—C(14)119.586 (14)C(30)—C(29)—H(29)118.228 (15)
C(1)—C(2)—C(3)123.399 (14)C(29)—C(30)—C(31)121.083 (15)
C(1)—C(2)—C(7)119.466 (14)C(29)—C(30)—H(30)119.095 (16)
C(3)—C(2)—C(7)117.127 (14)C(31)—C(30)—H(30)119.811 (16)
C(2)—C(3)—C(4)121.196 (15)C(30)—C(31)—C(32)119.826 (15)
C(2)—C(3)—H(3)119.501 (14)C(30)—C(31)—H(31)120.011 (16)
C(4)—C(3)—H(3)119.219 (15)C(32)—C(31)—H(31)120.123 (17)
C(3)—C(4)—C(5)120.987 (19)C(31)—C(32)—C(33)120.522 (15)
C(3)—C(4)—H(4)119.458 (16)C(31)—C(32)—H(32)122.444 (16)
C(5)—C(4)—H(4)119.540 (19)C(33)—C(32)—H(32)117.007 (15)
C(4)—C(5)—C(6)119.86 (3)C(28)—C(33)—C(32)120.210 (15)
C(4)—C(5)—H(5)118.61 (3)C(28)—C(33)—C(34)119.811 (15)
C(6)—C(5)—H(5)121.39 (3)C(32)—C(33)—C(34)119.946 (15)
C(5)—C(6)—C(7)120.63 (2)C(33)—C(34)—C(35)121.258 (16)
C(5)—C(6)—H(6)122.69 (2)C(33)—C(34)—H(34)119.764 (15)
C(7)—C(6)—H(6)116.625 (15)C(35)—C(34)—H(34)118.838 (15)
C(2)—C(7)—C(6)119.910 (14)C(34)—C(35)—C(36)120.135 (15)
C(2)—C(7)—C(8)119.493 (14)C(34)—C(35)—C(40)119.703 (15)
C(6)—C(7)—C(8)120.590 (15)C(36)—C(35)—C(40)120.132 (15)
C(7)—C(8)—C(9)121.298 (16)C(35)—C(36)—C(37)120.661 (16)
C(7)—C(8)—H(8)118.118 (14)C(35)—C(36)—H(36)117.857 (16)
C(9)—C(8)—H(8)120.451 (14)C(37)—C(36)—H(36)121.461 (16)
C(8)—C(9)—C(10)119.796 (14)C(36)—C(37)—C(38)119.674 (15)
C(8)—C(9)—C(14)120.026 (14)C(36)—C(37)—H(37)121.457 (18)
C(10)—C(9)—C(14)120.160 (14)C(38)—C(37)—H(37)118.835 (17)
C(9)—C(10)—C(11)121.084 (15)C(37)—C(38)—C(39)121.128 (16)
C(9)—C(10)—H(10)117.636 (14)C(37)—C(38)—H(38)119.556 (16)
C(11)—C(10)—H(10)121.206 (15)C(39)—C(38)—H(38)119.307 (18)
C(10)—C(11)—C(12)119.183 (14)C(38)—C(39)—C(40)121.214 (16)
C(10)—C(11)—H(11)121.255 (16)C(38)—C(39)—H(39)119.530 (16)
C(12)—C(11)—H(11)119.456 (16)C(40)—C(39)—H(39)119.034 (15)
C(11)—C(12)—C(13)121.435 (15)C(27)—C(40)—C(35)119.306 (14)
C(11)—C(12)—H(12)118.688 (15)C(27)—C(40)—C(39)123.574 (15)
C(13)—C(12)—H(12)119.818 (16)C(35)—C(40)—C(39)116.975 (14)
C(12)—C(13)—C(14)121.316 (15)P(2)—C(41)—C(42)121.867 (13)
C(12)—C(13)—H(13)119.798 (15)P(2)—C(41)—C(46)118.492 (18)
C(14)—C(13)—H(13)118.696 (14)C(42)—C(41)—C(46)119.47 (2)
C(1)—C(14)—C(9)118.927 (14)C(41)—C(42)—C(43)119.95 (2)
C(1)—C(14)—C(13)124.213 (14)C(41)—C(42)—H(42)121.652 (15)
C(9)—C(14)—C(13)116.776 (14)C(43)—C(42)—H(42)118.40 (2)
P(1)—C(15)—C(16)120.801 (12)C(42)—C(43)—C(44)120.43 (3)
P(1)—C(15)—C(20)119.383 (12)C(42)—C(43)—H(43)118.93 (3)
C(16)—C(15)—C(20)119.742 (15)C(44)—C(43)—H(43)120.64 (3)
C(15)—C(16)—C(17)120.132 (15)C(43)—C(44)—C(45)119.81 (3)
C(15)—C(16)—H(16)120.681 (15)C(43)—C(44)—H(44)119.66 (4)
C(17)—C(16)—H(16)119.171 (15)C(45)—C(44)—H(44)120.53 (3)
C(16)—C(17)—C(18)120.010 (15)C(44)—C(45)—C(46)120.08 (3)
C(16)—C(17)—H(17)119.563 (15)C(44)—C(45)—H(45)120.52 (3)
C(18)—C(17)—H(17)120.427 (15)C(46)—C(45)—H(45)119.40 (4)
C(17)—C(18)—C(19)120.007 (14)C(41)—C(46)—C(45)120.24 (3)
C(17)—C(18)—H(18)119.611 (15)C(41)—C(46)—H(46)118.83 (3)
C(19)—C(18)—H(18)120.374 (15)C(45)—C(46)—H(46)120.93 (3)
C(18)—C(19)—C(20)120.202 (14)P(2)—C(47)—C(48)118.50 (3)
C(18)—C(19)—H(19)120.249 (14)P(2)—C(47)—C(52)121.89 (3)
C(20)—C(19)—H(19)119.549 (15)C(48)—C(47)—C(52)119.58 (4)
C(15)—C(20)—C(19)119.891 (15)C(47)—C(48)—C(49)120.09 (4)
C(15)—C(20)—H(20)119.616 (14)C(47)—C(48)—H(48)119.08 (4)
C(19)—C(20)—H(20)120.492 (15)C(49)—C(48)—H(48)120.83 (4)
P(1)—C(21)—C(22)119.096 (12)C(48)—C(49)—C(50)120.35 (4)
P(1)—C(21)—C(26)121.184 (12)C(48)—C(49)—H(49)119.14 (5)
C(22)—C(21)—C(26)119.707 (16)C(50)—C(49)—H(49)120.50 (4)
C(21)—C(22)—C(23)120.020 (16)C(49)—C(50)—C(51)119.66 (4)
C(21)—C(22)—H(22)118.942 (15)C(49)—C(50)—H(50)120.75 (4)
C(23)—C(22)—H(22)120.997 (15)C(51)—C(50)—H(50)119.60 (4)
C(22)—C(23)—C(24)120.067 (19)C(50)—C(51)—C(52)120.45 (4)
C(22)—C(23)—H(23)119.773 (17)C(50)—C(51)—H(51)120.37 (4)
C(24)—C(23)—H(23)120.15 (2)C(52)—C(51)—H(51)119.18 (4)
C(23)—C(24)—C(25)120.17 (3)C(47)—C(52)—C(51)119.87 (4)
C(23)—C(24)—H(24)120.27 (3)C(47)—C(52)—H(52)120.98 (3)
C(25)—C(24)—H(24)119.56 (3)C(51)—C(52)—H(52)119.10 (4)
 

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