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Reaction of alkaline earth metal salts with diphenylphosphinic acid in dimethylformamide solvent afforded four coordination polymers: [Mg3(O2PPh2)6(DMF)2]·2DMF (I), [Ca(O2PPh2)2(DMF)2] (II), [Sr(O2PPh2)2(DMF)2] (III) and [Ba(O2PPh2)2(DMF)2] (IV) (where DMF is N,N-dimethylformamide). Single-crystal X-ray diffraction revealed that all four compounds produce linear chain structures in the solid state, with the Ca, Sr and Ba forming isostructural crystals. The bulk materials were characterized by FT-IR and 1H NMR spectroscopy and elemental analyses.

Supporting information

cif

Crystallographic Information File (CIF) https://doi.org/10.1107/S2052520614004247/ry5058sup1.cif
Contains datablocks jre01_0m, jret56, etc013, jr65b

hkl

Structure factor file (CIF format) https://doi.org/10.1107/S2052520614004247/ry5058jre01_0msup2.hkl
Contains datablock jre01_0m

hkl

Structure factor file (CIF format) https://doi.org/10.1107/S2052520614004247/ry5058jret56sup3.hkl
Contains datablock jret56

hkl

Structure factor file (CIF format) https://doi.org/10.1107/S2052520614004247/ry5058etc013sup4.hkl
Contains datablock etc013

hkl

Structure factor file (CIF format) https://doi.org/10.1107/S2052520614004247/ry5058jr65bsup5.hkl
Contains datablock jr65b

pdf

Portable Document Format (PDF) file https://doi.org/10.1107/S2052520614004247/ry5058sup6.pdf
Chemical Line Diagrams 1 and 2

CCDC references: 956948; 956949; 956950; 956951

Computing details top

Data collection: APEX2 (Bruker, 2004) for jre01_0m, jr65b; CrysAlis PRO, Agilent Technologies, Version 1.171.35.21 (release 20-01-2012 CrysAlis171 .NET) (compiled Jan 23 2012,18:06:46) for jret56; Bruker APEX2 v2010.3.0 for etc013. Cell refinement: APEX2/SAINT (Bruker, 2004) for jre01_0m, jr65b; CrysAlis PRO, Agilent Technologies, Version 1.171.35.21 (release 20-01-2012 CrysAlis171 .NET) (compiled Jan 23 2012,18:06:46) for jret56; Bruker SAINT v7.60A for etc013. Data reduction: SAINT/XPREP (Bruker, 2004; Sheldrick, 2003) for jre01_0m, jr65b; CrysAlis PRO, Agilent Technologies, Version 1.171.35.21 (release 20-01-2012 CrysAlis171 .NET) (compiled Jan 23 2012,18:0 for jret56; Bruker SAINT v7.60A for etc013. Program(s) used to solve structure: XS (Sheldrick, 2001) for jre01_0m, jret56, jr65b; Bruker SHELXTL v6.14 for etc013. Program(s) used to refine structure: XL (Sheldrick, 2001) for jre01_0m, jret56, jr65b; SHELXL2012 for etc013. Molecular graphics: XP (Sheldrick, 1998) for jre01_0m, jret56, jr65b; Bruker SHELXTL v6.14 for etc013. Software used to prepare material for publication: XCIF (Sheldrick, 2001)/enCIFer (CCDC, 2004) for jre01_0m, jret56, jr65b; Bruker SHELXTL v6.14 for etc013.

(jre01_0m) top
Crystal data top
C78H74Mg3N2O14P6·2(C3H7NO)F(000) = 1748
Mr = 1668.33Dx = 1.331 Mg m3
Monoclinic, P21/nMo Kα radiation, λ = 0.71073 Å
Hall symbol: -P 2ynCell parameters from 9929 reflections
a = 12.7538 (5) Åθ = 2.3–26.3°
b = 22.3294 (9) ŵ = 0.22 mm1
c = 15.0157 (6) ÅT = 150 K
β = 103.175 (2)°Plate, colorless
V = 4163.7 (3) Å30.34 × 0.15 × 0.14 mm
Z = 2
Data collection top
Bruker X8 - ApexII CCD Diffractometer8517 independent reflections
Radiation source: fine-focus sealed tube6996 reflections with I > 2σ(I)
Graphite monochromatorRint = 0.038
Detector resolution: 8.33 pixels mm-1θmax = 26.4°, θmin = 1.7°
φ and ω scansh = 1515
Absorption correction: multi-scan
Blessing, R.H. (1995) Acta Cryst. A51, 33-38.
Sheldrick, G.M. (2004) SADABS, University of G\:ottingen, Germany
k = 2727
Tmin = 0.96, Tmax = 0.97l = 1817
57065 measured reflections
Refinement top
Refinement on F2Primary atom site location: structure-invariant direct methods
Least-squares matrix: fullSecondary atom site location: difference Fourier map
R[F2 > 2σ(F2)] = 0.036Hydrogen site location: inferred from neighbouring sites
wR(F2) = 0.095H-atom parameters constrained
S = 1.03 w = 1/[σ2(Fo2) + (0.0431P)2 + 2.5214P]
where P = (Fo2 + 2Fc2)/3
8517 reflections(Δ/σ)max = 0.001
515 parametersΔρmax = 0.69 e Å3
0 restraintsΔρmin = 0.43 e Å3
Special details top

Geometry. All e.s.d.'s (except the e.s.d. in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell e.s.d.'s are taken into account individually in the estimation of e.s.d.'s in distances, angles and torsion angles; correlations between e.s.d.'s in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell e.s.d.'s is used for estimating e.s.d.'s involving l.s. planes.

Refinement. Refinement of F2 against ALL reflections. The weighted R-factor wR and goodness of fit S are based on F2, conventional R-factors R are based on F, with F set to zero for negative F2. The threshold expression of F2 > σ(F2) is used only for calculating R-factors(gt) etc. and is not relevant to the choice of reflections for refinement. R-factors based on F2 are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger.

Fractional atomic coordinates and isotropic or equivalent isotropic displacement parameters (Å2) top
xyzUiso*/Ueq
Mg10.99869 (4)0.00794 (2)0.16290 (4)0.01457 (12)
Mg21.00000.00000.50000.01783 (17)
O11.09739 (10)0.02028 (6)0.41398 (8)0.0225 (3)
O21.13107 (9)0.00336 (5)0.25361 (8)0.0197 (3)
O30.88239 (10)0.02296 (6)0.39026 (9)0.0283 (3)
O40.88641 (10)0.03338 (6)0.22003 (8)0.0246 (3)
O50.95821 (10)0.06232 (5)0.08776 (8)0.0218 (3)
O60.97650 (10)0.06932 (5)0.07971 (8)0.0212 (3)
O70.94997 (11)0.09176 (6)0.49545 (9)0.0286 (3)
P10.94361 (3)0.097757 (19)0.00052 (3)0.01614 (10)
P21.17315 (3)0.023039 (19)0.35201 (3)0.01561 (10)
P30.82370 (4)0.03419 (2)0.29418 (3)0.02022 (11)
N10.95680 (15)0.17377 (8)0.58609 (14)0.0381 (4)
C11.01919 (14)0.16639 (8)0.02643 (13)0.0223 (4)
C21.04539 (17)0.18888 (9)0.11533 (16)0.0350 (5)
H21.02370.16790.16320.042*
C31.10332 (19)0.24203 (11)0.1342 (2)0.0510 (7)
H31.12120.25710.19490.061*
C41.13479 (19)0.27277 (10)0.0655 (2)0.0535 (8)
H41.17350.30930.07870.064*
C51.11031 (19)0.25081 (11)0.0225 (2)0.0514 (7)
H51.13260.27210.06980.062*
C61.05285 (17)0.19741 (9)0.04236 (16)0.0359 (5)
H61.03670.18220.10310.043*
C70.80305 (13)0.11749 (7)0.03526 (12)0.0169 (3)
C80.75298 (14)0.12187 (8)0.12785 (12)0.0209 (4)
H80.79350.11520.17270.025*
C90.64410 (15)0.13586 (8)0.15485 (13)0.0245 (4)
H90.61070.13920.21800.029*
C100.58410 (15)0.14499 (8)0.08968 (14)0.0249 (4)
H100.50970.15440.10820.030*
C110.63287 (15)0.14033 (8)0.00225 (14)0.0269 (4)
H110.59170.14640.04680.032*
C120.74190 (15)0.12677 (8)0.02984 (13)0.0229 (4)
H120.77490.12380.09310.028*
C131.22130 (14)0.09937 (8)0.35160 (12)0.0202 (4)
C141.1696 (2)0.14429 (10)0.38895 (19)0.0471 (6)
H141.10830.13500.41230.056*
C151.2073 (3)0.20293 (10)0.3923 (2)0.0680 (10)
H151.17100.23350.41760.082*
C161.2963 (2)0.21716 (10)0.35961 (18)0.0473 (6)
H161.32160.25730.36240.057*
C171.34815 (17)0.17336 (9)0.32300 (14)0.0309 (4)
H171.40980.18300.30030.037*
C181.31117 (15)0.11474 (8)0.31882 (13)0.0243 (4)
H181.34790.08460.29310.029*
C191.29135 (13)0.02099 (7)0.39901 (11)0.0159 (3)
C201.31658 (14)0.03485 (8)0.49216 (12)0.0200 (4)
H201.26940.02290.52950.024*
C211.41057 (15)0.06608 (8)0.53055 (12)0.0233 (4)
H211.42710.07560.59390.028*
C221.48013 (14)0.08324 (8)0.47623 (13)0.0227 (4)
H221.54470.10410.50260.027*
C231.45542 (14)0.06998 (8)0.38358 (12)0.0218 (4)
H231.50300.08180.34650.026*
C241.36133 (14)0.03940 (7)0.34483 (12)0.0186 (3)
H241.34430.03090.28120.022*
C250.71970 (14)0.02247 (8)0.26557 (11)0.0211 (4)
C260.61237 (15)0.01006 (9)0.22486 (12)0.0241 (4)
H260.58960.03020.21270.029*
C270.53852 (16)0.05658 (10)0.20208 (13)0.0317 (5)
H270.46540.04790.17440.038*
C280.57063 (18)0.11505 (10)0.21929 (14)0.0360 (5)
H280.52010.14660.20230.043*
C290.67656 (19)0.12803 (10)0.26134 (14)0.0355 (5)
H290.69840.16840.27380.043*
C300.75092 (17)0.08200 (9)0.28527 (13)0.0292 (4)
H300.82320.09100.31510.035*
C310.75918 (14)0.10653 (9)0.28811 (13)0.0249 (4)
C320.74700 (16)0.14253 (9)0.21063 (14)0.0314 (4)
H320.77190.12860.15930.038*
C330.69879 (18)0.19871 (10)0.20749 (18)0.0419 (6)
H330.69090.22290.15430.050*
C340.66265 (19)0.21911 (11)0.2816 (2)0.0490 (7)
H340.62970.25740.27940.059*
C350.6741 (2)0.18437 (11)0.3587 (2)0.0510 (7)
H350.64860.19880.40950.061*
C360.72264 (18)0.12813 (10)0.36308 (17)0.0384 (5)
H360.73090.10450.41690.046*
C370.94214 (16)0.11632 (9)0.56687 (14)0.0278 (4)
H370.92380.09160.61250.033*
C380.9992 (4)0.21335 (12)0.5266 (3)0.1033 (16)
H38A1.07810.21320.54450.155*
H38B0.97270.25410.53180.155*
H38C0.97570.19960.46320.155*
C390.9491 (2)0.19871 (11)0.67293 (19)0.0534 (7)
H39A0.92680.16740.71050.080*
H39B0.89580.23110.66290.080*
H39C1.01940.21460.70450.080*
O1S0.87614 (12)0.33669 (6)0.51849 (12)0.0409 (4)
N1S0.79771 (11)0.42513 (7)0.54072 (10)0.0203 (3)
C1S0.81493 (14)0.36639 (8)0.55259 (13)0.0250 (4)
H1S0.77640.34600.59060.030*
C2S0.72425 (15)0.45667 (8)0.58514 (13)0.0255 (4)
H2S10.69460.42860.62320.038*
H2S20.66550.47400.53860.038*
H2S30.76310.48870.62360.038*
C3S0.85001 (17)0.46022 (9)0.48178 (14)0.0307 (4)
H3S10.90000.43470.45820.046*
H3S20.88980.49330.51680.046*
H3S30.79550.47630.43060.046*
Atomic displacement parameters (Å2) top
U11U22U33U12U13U23
Mg10.0124 (3)0.0183 (3)0.0129 (3)0.0007 (2)0.0029 (2)0.0007 (2)
Mg20.0118 (4)0.0294 (4)0.0131 (4)0.0015 (3)0.0043 (3)0.0013 (3)
O10.0183 (6)0.0308 (7)0.0204 (7)0.0001 (5)0.0086 (5)0.0011 (5)
O20.0148 (6)0.0284 (7)0.0154 (6)0.0002 (5)0.0021 (5)0.0008 (5)
O30.0165 (6)0.0497 (8)0.0183 (7)0.0014 (6)0.0032 (5)0.0006 (6)
O40.0187 (6)0.0373 (7)0.0194 (7)0.0049 (5)0.0079 (5)0.0026 (6)
O50.0221 (7)0.0222 (6)0.0203 (7)0.0049 (5)0.0036 (5)0.0037 (5)
O60.0203 (6)0.0232 (6)0.0206 (7)0.0022 (5)0.0061 (5)0.0039 (5)
O70.0285 (7)0.0362 (8)0.0226 (7)0.0076 (6)0.0093 (6)0.0032 (6)
P10.0165 (2)0.0158 (2)0.0157 (2)0.00207 (16)0.00290 (16)0.00014 (16)
P20.0127 (2)0.0205 (2)0.0140 (2)0.00007 (16)0.00391 (16)0.00070 (17)
P30.0124 (2)0.0328 (3)0.0160 (2)0.00171 (18)0.00432 (17)0.00138 (19)
N10.0441 (11)0.0255 (9)0.0522 (12)0.0078 (8)0.0267 (9)0.0038 (8)
C10.0162 (9)0.0173 (8)0.0309 (10)0.0040 (7)0.0001 (7)0.0002 (7)
C20.0287 (11)0.0337 (11)0.0419 (13)0.0001 (9)0.0068 (9)0.0166 (9)
C30.0352 (13)0.0399 (13)0.0735 (19)0.0007 (10)0.0033 (12)0.0329 (13)
C40.0290 (12)0.0214 (11)0.100 (2)0.0004 (9)0.0063 (13)0.0073 (13)
C50.0335 (13)0.0343 (12)0.079 (2)0.0069 (10)0.0027 (12)0.0246 (13)
C60.0303 (11)0.0329 (11)0.0384 (12)0.0059 (9)0.0044 (9)0.0119 (9)
C70.0170 (8)0.0137 (8)0.0198 (9)0.0010 (6)0.0040 (7)0.0008 (6)
C80.0217 (9)0.0213 (9)0.0199 (9)0.0017 (7)0.0051 (7)0.0009 (7)
C90.0243 (10)0.0225 (9)0.0234 (10)0.0023 (7)0.0017 (7)0.0003 (7)
C100.0175 (9)0.0200 (9)0.0363 (11)0.0020 (7)0.0040 (8)0.0030 (8)
C110.0233 (10)0.0286 (10)0.0322 (11)0.0039 (8)0.0133 (8)0.0032 (8)
C120.0232 (9)0.0263 (9)0.0198 (9)0.0032 (7)0.0063 (7)0.0032 (7)
C130.0211 (9)0.0212 (9)0.0175 (9)0.0030 (7)0.0027 (7)0.0022 (7)
C140.0573 (15)0.0259 (11)0.0722 (18)0.0074 (10)0.0443 (14)0.0048 (11)
C150.101 (2)0.0220 (12)0.104 (3)0.0085 (13)0.071 (2)0.0022 (13)
C160.0677 (17)0.0193 (10)0.0618 (17)0.0062 (10)0.0287 (14)0.0004 (10)
C170.0303 (11)0.0254 (10)0.0369 (12)0.0041 (8)0.0074 (9)0.0045 (8)
C180.0229 (10)0.0212 (9)0.0283 (10)0.0004 (7)0.0051 (8)0.0002 (7)
C190.0130 (8)0.0167 (8)0.0170 (9)0.0032 (6)0.0014 (6)0.0004 (6)
C200.0197 (9)0.0232 (9)0.0175 (9)0.0026 (7)0.0048 (7)0.0008 (7)
C210.0245 (10)0.0270 (9)0.0159 (9)0.0023 (7)0.0002 (7)0.0030 (7)
C220.0184 (9)0.0207 (9)0.0256 (10)0.0021 (7)0.0016 (7)0.0022 (7)
C230.0192 (9)0.0236 (9)0.0228 (10)0.0018 (7)0.0054 (7)0.0022 (7)
C240.0202 (9)0.0200 (8)0.0154 (9)0.0009 (7)0.0039 (7)0.0001 (7)
C250.0194 (9)0.0331 (10)0.0114 (8)0.0001 (7)0.0050 (7)0.0033 (7)
C260.0214 (9)0.0369 (10)0.0147 (9)0.0021 (8)0.0051 (7)0.0005 (8)
C270.0257 (10)0.0522 (13)0.0167 (10)0.0094 (9)0.0037 (8)0.0032 (9)
C280.0455 (13)0.0421 (12)0.0224 (11)0.0186 (10)0.0117 (9)0.0095 (9)
C290.0533 (14)0.0305 (11)0.0264 (11)0.0011 (10)0.0165 (10)0.0030 (9)
C300.0314 (11)0.0354 (11)0.0215 (10)0.0061 (9)0.0077 (8)0.0009 (8)
C310.0123 (9)0.0317 (10)0.0310 (11)0.0035 (7)0.0057 (7)0.0081 (8)
C320.0256 (10)0.0331 (11)0.0312 (11)0.0008 (8)0.0026 (8)0.0064 (9)
C330.0362 (13)0.0296 (11)0.0533 (15)0.0012 (9)0.0038 (11)0.0022 (10)
C340.0335 (13)0.0296 (12)0.084 (2)0.0008 (9)0.0147 (13)0.0132 (12)
C350.0461 (15)0.0392 (13)0.079 (2)0.0053 (11)0.0381 (14)0.0209 (13)
C360.0364 (12)0.0360 (12)0.0500 (14)0.0068 (9)0.0249 (11)0.0106 (10)
C370.0275 (10)0.0309 (10)0.0257 (11)0.0028 (8)0.0073 (8)0.0021 (8)
C380.175 (4)0.0287 (14)0.150 (4)0.0251 (19)0.128 (3)0.0228 (18)
C390.0628 (17)0.0410 (14)0.0567 (17)0.0056 (12)0.0144 (13)0.0172 (12)
O1S0.0317 (8)0.0315 (8)0.0612 (11)0.0085 (6)0.0140 (7)0.0092 (7)
N1S0.0175 (7)0.0236 (8)0.0204 (8)0.0009 (6)0.0057 (6)0.0015 (6)
C1S0.0191 (9)0.0257 (9)0.0285 (10)0.0007 (7)0.0021 (7)0.0020 (8)
C2S0.0214 (9)0.0282 (10)0.0275 (10)0.0045 (8)0.0069 (8)0.0049 (8)
C3S0.0321 (11)0.0345 (11)0.0273 (11)0.0023 (9)0.0104 (8)0.0027 (8)
Geometric parameters (Å, º) top
Mg1—O41.9155 (13)C7—C121.398 (2)
Mg1—O6i1.9286 (13)C8—C91.391 (2)
Mg1—O21.9290 (13)C9—C101.388 (3)
Mg1—O51.9327 (13)C10—C111.383 (3)
Mg2—O3ii2.0252 (13)C11—C121.391 (3)
Mg2—O32.0252 (13)C13—C141.387 (3)
Mg2—O1ii2.0365 (11)C13—C181.390 (2)
Mg2—O12.0365 (11)C14—C151.392 (3)
Mg2—O72.1424 (13)C15—C161.373 (4)
Mg2—O7ii2.1424 (13)C16—C171.365 (3)
O1—P21.4877 (12)C17—C181.388 (3)
O2—P21.5175 (12)C19—C201.397 (2)
O3—P31.4873 (13)C19—C241.399 (2)
O4—P31.5118 (12)C20—C211.393 (3)
O5—P11.5052 (13)C21—C221.389 (3)
O6—P11.5035 (12)C22—C231.387 (3)
O6—Mg1i1.9286 (13)C23—C241.388 (2)
O7—C371.229 (2)C25—C261.394 (3)
P1—C11.8049 (18)C25—C301.400 (3)
P1—C71.8048 (17)C26—C271.391 (3)
P2—C191.8034 (17)C27—C281.375 (3)
P2—C131.8121 (18)C28—C291.385 (3)
P3—C311.8057 (19)C29—C301.389 (3)
P3—C251.8124 (19)C31—C321.393 (3)
N1—C371.319 (3)C31—C361.399 (3)
N1—C381.446 (3)C32—C331.393 (3)
N1—C391.442 (3)C33—C341.375 (4)
C1—C21.394 (3)C34—C351.374 (4)
C1—C61.391 (3)C35—C361.395 (3)
C2—C31.393 (3)O1S—C1S1.222 (2)
C3—C41.373 (4)N1S—C1S1.335 (2)
C4—C51.376 (4)N1S—C2S1.450 (2)
C5—C61.396 (3)N1S—C3S1.453 (2)
C7—C81.395 (2)
O4—Mg1—O6i109.21 (6)C6—C1—P1120.19 (15)
O4—Mg1—O2110.24 (6)C1—C2—C3120.1 (2)
O6i—Mg1—O2107.69 (6)C4—C3—C2120.4 (2)
O4—Mg1—O5112.01 (6)C3—C4—C5120.1 (2)
O6i—Mg1—O5105.08 (6)C4—C5—C6120.2 (2)
O2—Mg1—O5112.36 (6)C1—C6—C5120.2 (2)
O3ii—Mg2—O3180.0C8—C7—C12119.01 (16)
O3ii—Mg2—O1ii89.19 (5)C8—C7—P1120.79 (13)
O3—Mg2—O1ii90.81 (5)C12—C7—P1120.17 (13)
O3ii—Mg2—O190.81 (5)C7—C8—C9120.42 (16)
O3—Mg2—O189.19 (5)C10—C9—C8120.12 (17)
O1ii—Mg2—O1180.0C11—C10—C9119.87 (17)
O3ii—Mg2—O786.78 (5)C10—C11—C12120.36 (17)
O3—Mg2—O793.22 (5)C11—C12—C7120.21 (17)
O1ii—Mg2—O790.72 (5)C14—C13—C18118.10 (18)
O1—Mg2—O789.28 (5)C14—C13—P2119.09 (15)
O3ii—Mg2—O7ii93.22 (5)C18—C13—P2122.75 (13)
O3—Mg2—O7ii86.78 (5)C13—C14—C15120.2 (2)
O1ii—Mg2—O7ii89.28 (5)C16—C15—C14120.8 (2)
O1—Mg2—O7ii90.72 (5)C17—C16—C15119.6 (2)
O7—Mg2—O7ii180.0C16—C17—C18120.20 (19)
P2—O1—Mg2169.39 (9)C17—C18—C13121.07 (18)
P2—O2—Mg1141.60 (8)C20—C19—C24119.03 (15)
P3—O3—Mg2161.36 (8)C20—C19—P2119.60 (13)
P3—O4—Mg1155.27 (9)C24—C19—P2121.31 (13)
P1—O5—Mg1153.95 (8)C19—C20—C21120.36 (16)
P1—O6—Mg1i159.39 (8)C22—C21—C20119.98 (17)
C37—O7—Mg2118.81 (13)C23—C22—C21120.05 (16)
O5—P1—O6118.26 (7)C22—C23—C24120.18 (16)
O5—P1—C1107.74 (8)C23—C24—C19120.38 (16)
O6—P1—C1107.37 (8)C26—C25—C30119.01 (18)
O5—P1—C7107.75 (7)C26—C25—P3123.90 (15)
O6—P1—C7107.71 (8)C30—C25—P3117.08 (14)
C1—P1—C7107.59 (8)C27—C26—C25120.10 (19)
O1—P2—O2117.45 (7)C28—C27—C26120.44 (19)
O1—P2—C19109.68 (8)C27—C28—C29120.13 (19)
O2—P2—C19107.56 (7)C28—C29—C30120.0 (2)
O1—P2—C13108.06 (8)C29—C30—C25120.23 (19)
O2—P2—C13108.30 (8)C32—C31—C36118.61 (19)
C19—P2—C13105.10 (8)C32—C31—P3121.40 (14)
O3—P3—O4118.60 (7)C36—C31—P3119.97 (16)
O3—P3—C31108.82 (9)C31—C32—C33120.8 (2)
O4—P3—C31106.56 (8)C34—C33—C32119.8 (2)
O3—P3—C25106.96 (8)C33—C34—C35120.3 (2)
O4—P3—C25107.37 (8)C34—C35—C36120.5 (2)
C31—P3—C25108.18 (8)C35—C36—C31119.9 (2)
C37—N1—C38120.9 (2)O7—C37—N1126.11 (19)
C37—N1—C39122.56 (19)C1S—N1S—C2S121.30 (16)
C38—N1—C39115.8 (2)C1S—N1S—C3S121.78 (16)
C2—C1—C6118.99 (18)C2S—N1S—C3S116.91 (15)
C2—C1—P1120.81 (15)O1S—C1S—N1S125.34 (19)
Symmetry codes: (i) x+2, y, z; (ii) x+2, y, z+1.
(jret56) top
Crystal data top
C30H34CaN2O6P2F(000) = 652
Mr = 620.61Dx = 1.425 Mg m3
Monoclinic, P21/cMo Kα radiation, λ = 0.7107 Å
a = 9.7975 (2) ÅCell parameters from 3858 reflections
b = 5.79149 (16) Åθ = 3.2–29.3°
c = 25.7052 (7) ŵ = 0.38 mm1
β = 97.272 (3)°T = 120 K
V = 1446.84 (7) Å3Plate, colorless
Z = 20.38 × 0.21 × 0.19 mm
Data collection top
SuperNova, Dual, Cu at zero, Atlas
diffractometer
3496 independent reflections
Radiation source: SuperNova (Mo) X-ray Source2745 reflections with I > 2σ(I)
Mirror monochromatorRint = 0.033
Detector resolution: 10.3875 pixels mm-1θmax = 29.3°, θmin = 3.2°
ω scansh = 913
Absorption correction: multi-scan
Blessing, R.H. (1995) Acta Cryst. A51, 33-38.
Sheldrick, G.M. (2004) SADABS, University of G\:ottingen, Germany
k = 77
Tmin = 0.98, Tmax = 1.00l = 3433
9758 measured reflections
Refinement top
Refinement on F2Primary atom site location: structure-invariant direct methods
Least-squares matrix: fullSecondary atom site location: difference Fourier map
R[F2 > 2σ(F2)] = 0.039Hydrogen site location: inferred from neighbouring sites
wR(F2) = 0.095H-atom parameters constrained
S = 1.06 w = 1/[σ2(Fo2) + (0.0307P)2 + 1.1211P]
where P = (Fo2 + 2Fc2)/3
3496 reflections(Δ/σ)max = 0.002
189 parametersΔρmax = 0.45 e Å3
0 restraintsΔρmin = 0.35 e Å3
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
Ca10.50000.50000.00000.01064 (13)
O10.56664 (13)0.2130 (2)0.06063 (5)0.0159 (3)
O20.50062 (13)0.2178 (2)0.06460 (5)0.0154 (3)
O30.26819 (13)0.3792 (2)0.00791 (5)0.0182 (3)
N10.14769 (16)0.0960 (3)0.04314 (6)0.0167 (4)
P10.55442 (5)0.00177 (8)0.09251 (2)0.01133 (12)
C10.72208 (18)0.0666 (3)0.12838 (7)0.0136 (4)
C20.78373 (19)0.2812 (4)0.12452 (7)0.0166 (4)
H20.73820.39610.10380.020*
C30.9136 (2)0.3246 (4)0.15161 (8)0.0198 (4)
H30.95460.46800.14870.024*
C40.9816 (2)0.1552 (4)0.18272 (8)0.0205 (4)
H41.06860.18460.20050.025*
C50.9205 (2)0.0581 (4)0.18743 (8)0.0205 (4)
H50.96590.17150.20860.025*
C60.79095 (19)0.1024 (4)0.16042 (7)0.0179 (4)
H60.74990.24550.16370.021*
C70.45072 (18)0.0660 (3)0.14430 (7)0.0133 (4)
C80.43920 (19)0.0978 (4)0.18341 (7)0.0180 (4)
H80.48170.24080.18190.022*
C90.3647 (2)0.0481 (4)0.22449 (8)0.0223 (5)
H90.35910.15680.25080.027*
C100.2986 (2)0.1621 (4)0.22651 (8)0.0222 (5)
H100.24750.19410.25380.027*
C110.3087 (2)0.3244 (4)0.18779 (8)0.0235 (5)
H110.26370.46530.18890.028*
C120.3862 (2)0.2784 (4)0.14701 (8)0.0186 (4)
H120.39460.39000.12160.022*
C130.24714 (19)0.1720 (4)0.01700 (7)0.0160 (4)
H130.30500.06320.00460.019*
C140.0570 (2)0.2556 (4)0.06567 (9)0.0249 (5)
H14A0.09180.28390.10170.037*
H14B0.03350.19000.06360.037*
H14C0.05280.39840.04660.037*
C150.1415 (2)0.1445 (4)0.05827 (9)0.0237 (5)
H15A0.20180.23380.03950.036*
H15B0.04900.20000.05010.036*
H15C0.16980.15900.09530.036*
Atomic displacement parameters (Å2) top
U11U22U33U12U13U23
Ca10.0140 (2)0.0094 (3)0.0088 (2)0.0000 (2)0.00239 (19)0.0003 (2)
O10.0216 (7)0.0140 (7)0.0123 (6)0.0010 (6)0.0028 (5)0.0022 (5)
O20.0194 (7)0.0144 (7)0.0122 (6)0.0002 (6)0.0013 (5)0.0018 (5)
O30.0178 (7)0.0178 (8)0.0196 (7)0.0009 (6)0.0048 (6)0.0009 (6)
N10.0174 (8)0.0144 (9)0.0195 (8)0.0001 (7)0.0068 (7)0.0004 (7)
P10.0150 (2)0.0104 (2)0.0086 (2)0.00131 (19)0.00170 (18)0.00010 (18)
C10.0152 (9)0.0160 (10)0.0102 (9)0.0001 (8)0.0040 (7)0.0025 (7)
C20.0193 (9)0.0161 (10)0.0148 (9)0.0008 (8)0.0033 (8)0.0007 (8)
C30.0194 (9)0.0208 (11)0.0201 (10)0.0064 (9)0.0055 (8)0.0037 (8)
C40.0148 (9)0.0288 (12)0.0179 (10)0.0024 (9)0.0020 (8)0.0050 (9)
C50.0211 (10)0.0246 (12)0.0155 (10)0.0069 (9)0.0015 (8)0.0011 (8)
C60.0200 (9)0.0168 (10)0.0173 (10)0.0014 (8)0.0041 (8)0.0005 (8)
C70.0133 (8)0.0160 (10)0.0104 (9)0.0012 (7)0.0008 (7)0.0030 (7)
C80.0186 (9)0.0188 (11)0.0167 (10)0.0003 (8)0.0023 (8)0.0008 (8)
C90.0211 (10)0.0314 (13)0.0150 (10)0.0053 (9)0.0052 (8)0.0023 (9)
C100.0168 (9)0.0330 (13)0.0180 (10)0.0052 (9)0.0071 (8)0.0094 (9)
C110.0222 (10)0.0242 (12)0.0248 (11)0.0034 (9)0.0055 (9)0.0076 (9)
C120.0216 (10)0.0176 (11)0.0169 (10)0.0006 (8)0.0035 (8)0.0013 (8)
C130.0155 (9)0.0182 (10)0.0140 (9)0.0004 (8)0.0004 (7)0.0020 (8)
C140.0253 (11)0.0219 (12)0.0299 (12)0.0016 (9)0.0133 (9)0.0023 (9)
C150.0235 (10)0.0178 (11)0.0309 (12)0.0020 (9)0.0073 (9)0.0027 (9)
Geometric parameters (Å, º) top
Ca1—O12.3152 (13)P1—C71.8168 (19)
Ca1—O1i2.3152 (13)P1—C11.8182 (19)
Ca1—O2ii2.3294 (13)C1—C21.391 (3)
Ca1—O2iii2.3294 (13)C1—C61.396 (3)
Ca1—O32.4095 (13)C2—C31.393 (3)
Ca1—O3i2.4095 (13)C3—C41.382 (3)
Ca1—C13i3.1955 (19)C4—C51.385 (3)
O1—P11.5027 (14)C5—C61.391 (3)
O2—P11.5041 (14)C7—C121.389 (3)
O2—Ca1iv2.3294 (13)C7—C81.397 (3)
O3—C131.245 (2)C8—C91.388 (3)
N1—C131.327 (2)C9—C101.383 (3)
N1—C151.449 (3)C10—C111.382 (3)
N1—C141.453 (3)C11—C121.395 (3)
O1—Ca1—O1i180.0C13—N1—C14121.09 (17)
O1—Ca1—O2ii87.21 (5)C15—N1—C14117.14 (16)
O1i—Ca1—O2ii92.79 (5)O1—P1—O2118.42 (7)
O1—Ca1—O2iii92.79 (5)O1—P1—C7108.14 (8)
O1i—Ca1—O2iii87.21 (5)O2—P1—C7109.53 (8)
O2ii—Ca1—O2iii180.00 (6)O1—P1—C1108.55 (8)
O1—Ca1—O385.60 (5)O2—P1—C1108.04 (8)
O1i—Ca1—O394.40 (5)C7—P1—C1103.07 (8)
O2ii—Ca1—O386.50 (5)C2—C1—C6119.10 (17)
O2iii—Ca1—O393.50 (5)C2—C1—P1121.39 (15)
O1—Ca1—O3i94.40 (5)C6—C1—P1119.51 (15)
O1i—Ca1—O3i85.60 (5)C1—C2—C3120.17 (18)
O2ii—Ca1—O3i93.50 (5)C4—C3—C2120.28 (19)
O2iii—Ca1—O3i86.50 (5)C3—C4—C5120.07 (18)
O3—Ca1—O3i180.00 (6)C4—C5—C6119.88 (19)
O1—Ca1—C13i111.19 (5)C5—C6—C1120.49 (19)
O1i—Ca1—C13i68.81 (5)C12—C7—C8119.10 (17)
O2ii—Ca1—C13i104.58 (5)C12—C7—P1121.90 (15)
O2iii—Ca1—C13i75.42 (5)C8—C7—P1118.97 (15)
O3—Ca1—C13i159.96 (5)C9—C8—C7120.3 (2)
O3i—Ca1—C13i20.04 (5)C10—C9—C8120.3 (2)
P1—O1—Ca1157.86 (8)C11—C10—C9119.68 (19)
P1—O2—Ca1iv153.22 (8)C10—C11—C12120.4 (2)
C13—O3—Ca1118.43 (12)C7—C12—C11120.09 (19)
C13—N1—C15120.85 (17)O3—C13—N1124.37 (18)
Symmetry codes: (i) x+1, y+1, z; (ii) x+1, y, z; (iii) x, y+1, z; (iv) x, y1, z.
(etc013) top
Crystal data top
2(C12H10O2P)·2(C3H7NO)·SrF(000) = 688
Mr = 668.15Dx = 1.495 Mg m3
Monoclinic, P21/cSynchrotron radiation, λ = 0.77490 Å
a = 9.7098 (17) ÅCell parameters from 4537 reflections
b = 5.8964 (10) Åθ = 2.7–28.9°
c = 26.165 (5) ŵ = 0.57 mm1
β = 97.635 (2)°T = 150 K
V = 1484.8 (4) Å3Needle, colorless
Z = 20.16 × 0.01 × 0.01 mm
Data collection top
Bruker APEXII
diffractometer
2425 reflections with I > 2σ(I)
Radiation source: synchrotronRint = 0.054
Si-<111> channel cut crystal monochromatorθmax = 29.0°, θmin = 2.7°
Detector resolution: 8.33 pixels mm-1h = 1212
phi and ω scansk = 77
15927 measured reflectionsl = 3232
3020 independent reflections
Refinement top
Refinement on F20 restraints
Least-squares matrix: fullHydrogen site location: inferred from neighbouring sites
R[F2 > 2σ(F2)] = 0.030H-atom parameters constrained
wR(F2) = 0.079 w = 1/[σ2(Fo2) + (0.0296P)2 + 0.9012P]
where P = (Fo2 + 2Fc2)/3
S = 1.02(Δ/σ)max < 0.001
3020 reflectionsΔρmax = 0.40 e Å3
189 parametersΔρmin = 0.36 e Å3
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
Sr10.50000.00000.00000.01534 (10)
O10.49628 (14)0.2850 (2)0.06866 (5)0.0210 (3)
O20.57151 (15)0.7032 (2)0.06358 (5)0.0229 (3)
O30.25372 (14)0.1420 (2)0.00668 (6)0.0261 (3)
N10.14066 (18)0.4196 (3)0.04423 (7)0.0239 (4)
P10.55495 (5)0.49567 (8)0.09551 (2)0.01602 (13)
C10.7825 (2)0.2127 (4)0.12778 (8)0.0223 (4)
H10.73370.09810.10720.027*
C20.9134 (2)0.1666 (4)0.15441 (8)0.0258 (5)
H20.95330.02060.15190.031*
C30.9855 (2)0.3309 (4)0.18441 (8)0.0267 (5)
H31.07530.29910.20210.032*
C40.9263 (2)0.5430 (4)0.18873 (8)0.0263 (5)
H40.97510.65600.20980.032*
C50.7956 (2)0.5903 (4)0.16221 (8)0.0226 (4)
H50.75550.73580.16530.027*
C60.7230 (2)0.4254 (3)0.13116 (7)0.0176 (4)
C70.4513 (2)0.5714 (4)0.14590 (7)0.0190 (4)
C80.4369 (2)0.4144 (4)0.18473 (8)0.0239 (4)
H80.47880.26910.18380.029*
C90.3618 (2)0.4685 (4)0.22470 (9)0.0302 (5)
H90.35390.36130.25130.036*
C100.2988 (2)0.6779 (4)0.22584 (8)0.0310 (5)
H100.24660.71430.25300.037*
C110.3116 (2)0.8341 (4)0.18755 (9)0.0313 (5)
H110.26730.97750.18820.038*
C120.3894 (2)0.7829 (4)0.14791 (8)0.0250 (5)
H120.39990.89290.12220.030*
C130.2360 (2)0.3441 (4)0.01668 (8)0.0223 (4)
H130.29480.45250.00370.027*
C140.1366 (2)0.6570 (4)0.05934 (10)0.0336 (5)
H14A0.19640.74620.03960.050*
H14B0.04090.71320.05230.050*
H14C0.16970.67140.09620.050*
C150.0501 (2)0.2637 (4)0.06691 (10)0.0335 (5)
H15A0.08830.23390.10290.050*
H15B0.04260.33090.06570.050*
H15C0.04350.12100.04750.050*
Atomic displacement parameters (Å2) top
U11U22U33U12U13U23
Sr10.01987 (17)0.01225 (16)0.01414 (16)0.00024 (12)0.00317 (11)0.00011 (12)
O10.0260 (7)0.0184 (7)0.0177 (7)0.0006 (6)0.0001 (6)0.0037 (6)
O20.0319 (8)0.0186 (7)0.0184 (7)0.0026 (6)0.0034 (6)0.0035 (6)
O30.0239 (8)0.0240 (8)0.0312 (8)0.0033 (6)0.0066 (6)0.0027 (6)
N10.0258 (9)0.0202 (9)0.0273 (9)0.0010 (7)0.0093 (7)0.0002 (8)
P10.0210 (3)0.0140 (3)0.0130 (2)0.00167 (19)0.00185 (19)0.00028 (19)
C10.0254 (10)0.0201 (10)0.0215 (10)0.0013 (8)0.0029 (8)0.0001 (8)
C20.0244 (11)0.0241 (11)0.0298 (11)0.0062 (9)0.0063 (9)0.0038 (9)
C30.0181 (10)0.0381 (13)0.0236 (11)0.0006 (9)0.0016 (8)0.0062 (10)
C40.0255 (11)0.0292 (12)0.0238 (11)0.0060 (9)0.0019 (9)0.0022 (9)
C50.0263 (11)0.0199 (10)0.0219 (10)0.0007 (8)0.0047 (8)0.0011 (8)
C60.0214 (10)0.0177 (9)0.0140 (9)0.0009 (8)0.0040 (7)0.0012 (8)
C70.0189 (10)0.0212 (10)0.0162 (9)0.0008 (8)0.0000 (7)0.0034 (8)
C80.0228 (10)0.0261 (11)0.0230 (11)0.0006 (9)0.0041 (8)0.0011 (9)
C90.0273 (11)0.0439 (15)0.0199 (11)0.0068 (10)0.0054 (9)0.0013 (10)
C100.0231 (11)0.0467 (15)0.0245 (11)0.0068 (10)0.0081 (9)0.0144 (10)
C110.0286 (12)0.0287 (12)0.0377 (13)0.0038 (10)0.0082 (10)0.0129 (10)
C120.0282 (11)0.0232 (11)0.0240 (11)0.0032 (9)0.0046 (9)0.0025 (9)
C130.0212 (10)0.0243 (11)0.0214 (10)0.0002 (8)0.0024 (8)0.0010 (8)
C140.0319 (12)0.0238 (12)0.0457 (14)0.0037 (10)0.0071 (11)0.0086 (10)
C150.0347 (12)0.0295 (13)0.0403 (13)0.0035 (10)0.0191 (11)0.0058 (10)
Geometric parameters (Å, º) top
Sr1—O2i2.4505 (14)C4—C51.392 (3)
Sr1—O2ii2.4505 (14)C4—H40.9500
Sr1—O12.4637 (14)C5—C61.396 (3)
Sr1—O1iii2.4637 (14)C5—H50.9500
Sr1—O3iii2.5614 (14)C7—C121.388 (3)
Sr1—O32.5615 (14)C7—C81.395 (3)
Sr1—C13iii3.343 (2)C8—C91.389 (3)
O1—P11.5018 (14)C8—H80.9500
O2—P11.5025 (14)C9—C101.380 (3)
O2—Sr1iv2.4505 (14)C9—H90.9500
O3—C131.237 (2)C10—C111.379 (3)
N1—C131.324 (3)C10—H100.9500
N1—C151.452 (3)C11—C121.394 (3)
N1—C141.457 (3)C11—H110.9500
P1—C61.816 (2)C12—H120.9500
P1—C71.817 (2)C13—H130.9500
C1—C61.389 (3)C14—H14A0.9800
C1—C21.392 (3)C14—H14B0.9800
C1—H10.9500C14—H14C0.9800
C2—C31.378 (3)C15—H15A0.9800
C2—H20.9500C15—H15B0.9800
C3—C41.387 (3)C15—H15C0.9800
C3—H30.9500
O2i—Sr1—O2ii180.00 (10)C3—C4—C5120.0 (2)
O2i—Sr1—O188.73 (5)C3—C4—H4120.0
O2ii—Sr1—O191.27 (5)C5—C4—H4120.0
O2i—Sr1—O1iii91.27 (5)C4—C5—C6120.5 (2)
O2ii—Sr1—O1iii88.73 (5)C4—C5—H5119.8
O1—Sr1—O1iii180.0C6—C5—H5119.8
O2i—Sr1—O3iii84.44 (5)C1—C6—C5118.92 (19)
O2ii—Sr1—O3iii95.56 (5)C1—C6—P1121.74 (15)
O1—Sr1—O3iii86.05 (5)C5—C6—P1119.33 (16)
O1iii—Sr1—O3iii93.95 (5)C12—C7—C8118.84 (19)
O2i—Sr1—O395.56 (5)C12—C7—P1122.19 (16)
O2ii—Sr1—O384.44 (5)C8—C7—P1118.95 (16)
O1—Sr1—O393.95 (5)C9—C8—C7120.6 (2)
O1iii—Sr1—O386.05 (5)C9—C8—H8119.7
O3iii—Sr1—O3180.0C7—C8—H8119.7
O2i—Sr1—C13iii68.35 (5)C10—C9—C8120.0 (2)
O2ii—Sr1—C13iii111.65 (5)C10—C9—H9120.0
O1—Sr1—C13iii76.54 (5)C8—C9—H9120.0
O1iii—Sr1—C13iii103.46 (5)C11—C10—C9119.9 (2)
O3iii—Sr1—C13iii18.85 (5)C11—C10—H10120.0
O3—Sr1—C13iii161.15 (5)C9—C10—H10120.0
P1—O1—Sr1149.77 (8)C10—C11—C12120.4 (2)
P1—O2—Sr1iv156.57 (9)C10—C11—H11119.8
C13—O3—Sr1119.14 (13)C12—C11—H11119.8
C13—N1—C15120.96 (19)C7—C12—C11120.2 (2)
C13—N1—C14121.16 (18)C7—C12—H12119.9
C15—N1—C14117.25 (18)C11—C12—H12119.9
O1—P1—O2118.40 (8)O3—C13—N1124.5 (2)
O1—P1—C6108.10 (9)O3—C13—H13117.7
O2—P1—C6108.42 (9)N1—C13—H13117.7
O1—P1—C7109.30 (9)N1—C14—H14A109.5
O2—P1—C7108.28 (9)N1—C14—H14B109.5
C6—P1—C7103.28 (9)H14A—C14—H14B109.5
C6—C1—C2120.26 (19)N1—C14—H14C109.5
C6—C1—H1119.9H14A—C14—H14C109.5
C2—C1—H1119.9H14B—C14—H14C109.5
C3—C2—C1120.6 (2)N1—C15—H15A109.5
C3—C2—H2119.7N1—C15—H15B109.5
C1—C2—H2119.7H15A—C15—H15B109.5
C2—C3—C4119.7 (2)N1—C15—H15C109.5
C2—C3—H3120.1H15A—C15—H15C109.5
C4—C3—H3120.1H15B—C15—H15C109.5
Sr1—O1—P1—O251.79 (19)C7—P1—C6—C560.31 (17)
Sr1—O1—P1—C671.90 (17)O1—P1—C7—C12123.87 (17)
Sr1—O1—P1—C7176.35 (15)O2—P1—C7—C126.4 (2)
Sr1iv—O2—P1—O151.2 (2)C6—P1—C7—C12121.24 (18)
Sr1iv—O2—P1—C6174.8 (2)O1—P1—C7—C858.08 (18)
Sr1iv—O2—P1—C773.8 (2)O2—P1—C7—C8171.65 (16)
C6—C1—C2—C30.0 (3)C6—P1—C7—C856.82 (18)
C1—C2—C3—C41.0 (3)C12—C7—C8—C90.0 (3)
C2—C3—C4—C51.0 (3)P1—C7—C8—C9178.15 (16)
C3—C4—C5—C60.0 (3)C7—C8—C9—C101.0 (3)
C2—C1—C6—C50.9 (3)C8—C9—C10—C110.7 (3)
C2—C1—C6—P1178.06 (15)C9—C10—C11—C120.7 (3)
C4—C5—C6—C10.9 (3)C8—C7—C12—C111.4 (3)
C4—C5—C6—P1178.11 (16)P1—C7—C12—C11179.48 (16)
O1—P1—C6—C14.94 (19)C10—C11—C12—C71.8 (3)
O2—P1—C6—C1124.58 (17)Sr1—O3—C13—N1146.19 (17)
C7—P1—C6—C1120.69 (17)C15—N1—C13—O32.2 (3)
O1—P1—C6—C5176.06 (15)C14—N1—C13—O3172.9 (2)
O2—P1—C6—C554.42 (17)
Symmetry codes: (i) x+1, y+1, z; (ii) x, y1, z; (iii) x+1, y, z; (iv) x, y+1, z.
(jr65b) top
Crystal data top
C30H34BaN2O6P2F(000) = 724
Mr = 717.85Dx = 1.565 Mg m3
Monoclinic, P21/cMo Kα radiation, λ = 0.71073 Å
Hall symbol: -P 2ybcCell parameters from 9198 reflections
a = 9.6068 (7) Åθ = 2.5–26.5°
b = 6.0118 (4) ŵ = 1.45 mm1
c = 26.6405 (19) ÅT = 120 K
β = 98.033 (1)°Rod, colorless
V = 1523.50 (19) Å30.67 × 0.12 × 0.05 mm
Z = 2
Data collection top
Bruker X8 - ApexII CCD Diffractometer3153 independent reflections
Radiation source: fine-focus sealed tube2694 reflections with I > 2σ(I)
Graphite monochromatorRint = 0.028
Detector resolution: 8.33 pixels mm-1θmax = 26.5°, θmin = 1.5°
φ and ω scansh = 1112
Absorption correction: multi-scan
Blessing, R.H. (1995) Acta Cryst. A51, 33-38.
Sheldrick, G.M. (2004) SADABS, University of G\:ottingen, Germany
k = 77
Tmin = 0.811, Tmax = 0.930l = 3333
22314 measured reflections
Refinement top
Refinement on F2Primary atom site location: structure-invariant direct methods
Least-squares matrix: fullSecondary atom site location: difference Fourier map
R[F2 > 2σ(F2)] = 0.018Hydrogen site location: inferred from neighbouring sites
wR(F2) = 0.041H-atom parameters constrained
S = 1.02 w = 1/[σ2(Fo2) + (0.0159P)2 + 1.3613P]
where P = (Fo2 + 2Fc2)/3
3153 reflections(Δ/σ)max < 0.001
189 parametersΔρmax = 0.44 e Å3
0 restraintsΔρmin = 0.38 e Å3
Special details top

Geometry. All e.s.d.'s (except the e.s.d. in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell e.s.d.'s are taken into account individually in the estimation of e.s.d.'s in distances, angles and torsion angles; correlations between e.s.d.'s in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell e.s.d.'s is used for estimating e.s.d.'s involving l.s. planes.

Refinement. Refinement of F2 against ALL reflections. The weighted R-factor wR and goodness of fit S are based on F2, conventional R-factors R are based on F, with F set to zero for negative F2. The threshold expression of F2 > σ(F2) is used only for calculating R-factors(gt) etc. and is not relevant to the choice of reflections for refinement. R-factors based on F2 are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger.

Fractional atomic coordinates and isotropic or equivalent isotropic displacement parameters (Å2) top
xyzUiso*/Ueq
Ba10.50000.00000.00000.00985 (5)
P10.55484 (4)0.49164 (8)0.099263 (16)0.01148 (9)
O20.57640 (14)0.3101 (2)0.06681 (5)0.0188 (3)
O10.23805 (14)0.1655 (2)0.00507 (5)0.0229 (3)
C150.43435 (19)0.4291 (3)0.18693 (7)0.0175 (4)
H150.47430.28460.18690.021*
C90.78006 (19)0.2039 (3)0.13199 (7)0.0167 (4)
H90.72770.09200.11250.020*
C30.1305 (2)0.6693 (4)0.06122 (9)0.0321 (5)
H3A0.18950.75730.04150.048*
H3B0.03380.72540.05530.048*
H3C0.16690.68140.09740.048*
C10.22361 (19)0.3630 (3)0.01658 (7)0.0195 (4)
H10.28230.46940.00360.023*
C20.0430 (2)0.2832 (4)0.06845 (9)0.0323 (5)
H2A0.08540.25010.10330.049*
H2B0.04980.35050.06880.049*
H2C0.03300.14530.04870.049*
N10.13248 (17)0.4370 (3)0.04566 (6)0.0199 (4)
C40.72381 (18)0.4165 (3)0.13468 (6)0.0117 (3)
C70.9891 (2)0.3164 (3)0.18651 (7)0.0200 (4)
H71.07990.28260.20390.024*
C50.80156 (19)0.5770 (3)0.16431 (7)0.0161 (4)
H50.76350.72170.16690.019*
C60.9337 (2)0.5282 (3)0.19005 (7)0.0201 (4)
H60.98580.63900.21000.024*
C80.9130 (2)0.1547 (3)0.15783 (7)0.0209 (4)
H80.95120.00980.15570.025*
C100.45226 (18)0.5782 (3)0.14816 (7)0.0131 (4)
C130.2986 (2)0.7000 (4)0.22532 (7)0.0248 (5)
H130.24640.74200.25160.030*
C140.3584 (2)0.4906 (4)0.22559 (7)0.0243 (4)
H140.34760.38900.25210.029*
C110.3928 (2)0.7891 (3)0.14870 (7)0.0190 (4)
H110.40560.89330.12290.023*
C120.3146 (2)0.8479 (4)0.18695 (8)0.0258 (5)
H120.27200.99070.18660.031*
O30.49009 (13)0.2861 (2)0.07381 (5)0.0166 (3)
Atomic displacement parameters (Å2) top
U11U22U33U12U13U23
Ba10.01305 (7)0.00808 (7)0.00865 (7)0.00054 (6)0.00230 (5)0.00008 (6)
P10.0144 (2)0.0111 (2)0.00871 (19)0.00202 (19)0.00078 (16)0.00049 (19)
O20.0242 (7)0.0178 (7)0.0151 (7)0.0047 (6)0.0048 (5)0.0054 (5)
O10.0186 (7)0.0231 (7)0.0277 (8)0.0049 (6)0.0056 (6)0.0043 (6)
C150.0155 (9)0.0207 (9)0.0161 (9)0.0010 (7)0.0017 (7)0.0004 (8)
C90.0176 (9)0.0153 (9)0.0172 (9)0.0004 (7)0.0019 (8)0.0014 (8)
C30.0262 (12)0.0269 (12)0.0429 (14)0.0065 (9)0.0040 (10)0.0143 (10)
C10.0122 (9)0.0260 (11)0.0197 (10)0.0018 (8)0.0006 (8)0.0001 (8)
C20.0335 (13)0.0344 (12)0.0330 (13)0.0076 (10)0.0183 (10)0.0102 (10)
N10.0183 (8)0.0202 (8)0.0219 (9)0.0050 (6)0.0051 (7)0.0006 (7)
C40.0123 (8)0.0140 (8)0.0095 (8)0.0008 (7)0.0042 (7)0.0032 (7)
C70.0118 (9)0.0287 (11)0.0194 (10)0.0017 (8)0.0015 (8)0.0058 (9)
C50.0180 (9)0.0144 (8)0.0164 (9)0.0010 (7)0.0043 (8)0.0007 (7)
C60.0169 (9)0.0252 (11)0.0180 (9)0.0064 (8)0.0022 (7)0.0022 (8)
C80.0192 (10)0.0181 (9)0.0257 (11)0.0052 (8)0.0045 (8)0.0029 (8)
C100.0110 (8)0.0158 (8)0.0117 (9)0.0011 (7)0.0004 (7)0.0038 (7)
C130.0133 (9)0.0418 (13)0.0202 (10)0.0069 (9)0.0060 (8)0.0154 (9)
C140.0184 (9)0.0391 (12)0.0158 (9)0.0070 (10)0.0035 (7)0.0004 (10)
C110.0197 (10)0.0169 (9)0.0204 (10)0.0024 (8)0.0026 (8)0.0027 (8)
C120.0210 (10)0.0253 (11)0.0316 (12)0.0020 (9)0.0056 (9)0.0127 (9)
O30.0178 (7)0.0168 (7)0.0145 (6)0.0017 (5)0.0004 (5)0.0054 (5)
Geometric parameters (Å, º) top
Ba1—O2i2.6111 (12)C9—C41.393 (3)
Ba1—O22.6111 (12)C9—C81.395 (3)
Ba1—O3i2.6241 (12)C3—N11.458 (3)
Ba1—O32.6241 (12)C1—N11.324 (2)
Ba1—O12.7268 (13)C2—N11.452 (3)
Ba1—O1i2.7268 (13)C4—C51.395 (3)
P1—O31.5019 (13)C7—C81.381 (3)
P1—O2ii1.5035 (13)C7—C61.388 (3)
P1—C101.8160 (18)C5—C61.387 (3)
P1—C41.8168 (18)C10—C111.391 (3)
O2—P1iii1.5035 (13)C13—C121.380 (3)
O1—C11.239 (2)C13—C141.383 (3)
C15—C141.393 (3)C11—C121.394 (3)
C15—C101.396 (3)
O2i—Ba1—O2180.00 (8)C1—O1—Ba1119.86 (12)
O2i—Ba1—O3i89.62 (4)C14—C15—C10120.55 (19)
O2—Ba1—O3i90.38 (4)C4—C9—C8120.26 (18)
O2i—Ba1—O390.38 (4)O1—C1—N1124.94 (19)
O2—Ba1—O389.62 (4)C1—N1—C2120.61 (17)
O3i—Ba1—O3180.00 (6)C1—N1—C3121.60 (18)
O2i—Ba1—O196.94 (4)C2—N1—C3117.33 (17)
O2—Ba1—O183.06 (4)C9—C4—C5118.84 (17)
O3i—Ba1—O185.89 (4)C9—C4—P1121.74 (14)
O3—Ba1—O194.11 (4)C5—C4—P1119.40 (14)
O2i—Ba1—O1i83.06 (4)C8—C7—C6120.29 (18)
O2—Ba1—O1i96.94 (4)C6—C5—C4120.94 (18)
O3i—Ba1—O1i94.11 (4)C5—C6—C7119.59 (18)
O3—Ba1—O1i85.89 (4)C7—C8—C9120.07 (18)
O1—Ba1—O1i180.00 (8)C11—C10—C15118.96 (17)
O3—P1—O2ii118.30 (8)C11—C10—P1122.21 (14)
O3—P1—C10109.13 (8)C15—C10—P1118.82 (14)
O2ii—P1—C10108.51 (8)C12—C13—C14120.08 (18)
O3—P1—C4108.28 (8)C13—C14—C15119.85 (19)
O2ii—P1—C4108.10 (8)C10—C11—C12120.17 (19)
C10—P1—C4103.52 (8)C13—C12—C11120.37 (19)
P1iii—O2—Ba1155.47 (8)P1—O3—Ba1145.23 (7)
Symmetry codes: (i) x+1, y, z; (ii) x, y+1, z; (iii) x, y1, z.
 

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