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In the title compound, (C8H20N)[Mo(O2CCH2NH2)(NCCH3)(CO)3], obtained from the ligand substitution reaction of [Et4N]3[Mo3(CO)9(OMe)3] with glycine in the solvent acetonitrile the Mo center is in an approximately octahedral geometry.

Supporting information

cif

Crystallographic Information File (CIF) https://doi.org/10.1107/S1600536806047684/ez2049sup1.cif
Contains datablocks I, KK049

hkl

Structure factor file (CIF format) https://doi.org/10.1107/S1600536806047684/ez2049Isup2.hkl
Contains datablock I

CCDC reference: 629658

Key indicators

  • Single-crystal X-ray study
  • T = 110 K
  • Mean [sigma](C-C) = 0.002 Å
  • R factor = 0.023
  • wR factor = 0.057
  • Data-to-parameter ratio = 20.9

checkCIF/PLATON results

No syntax errors found



Alert level B PLAT232_ALERT_2_B Hirshfeld Test Diff (M-X) Mo1 - C3 .. 10.58 su PLAT232_ALERT_2_B Hirshfeld Test Diff (M-X) Mo1 - C4 .. 10.58 su PLAT232_ALERT_2_B Hirshfeld Test Diff (M-X) Mo1 - C5 .. 12.48 su
Alert level C PLAT230_ALERT_2_C Hirshfeld Test Diff for O3 - C3 .. 5.03 su PLAT230_ALERT_2_C Hirshfeld Test Diff for O5 - C5 .. 5.95 su PLAT232_ALERT_2_C Hirshfeld Test Diff (M-X) Mo1 - N2 .. 8.12 su PLAT420_ALERT_2_C D-H Without Acceptor N1 - H1B ... ?
0 ALERT level A = In general: serious problem 3 ALERT level B = Potentially serious problem 4 ALERT level C = Check and explain 0 ALERT level G = General alerts; check 0 ALERT type 1 CIF construction/syntax error, inconsistent or missing data 7 ALERT type 2 Indicator that the structure model may be wrong or deficient 0 ALERT type 3 Indicator that the structure quality may be low 0 ALERT type 4 Improvement, methodology, query or suggestion 0 ALERT type 5 Informative message, check

Computing details top

Data collection: APEX2 (Bruker, 2003); cell refinement: APEX2; data reduction: SAINTPLUS (Bruker, 2003); program(s) used to solve structure: SHELXS97 (Sheldrick, 1997); program(s) used to refine structure: SHELXL97 (Sheldrick, 1997); molecular graphics: SHELXTL (Bruker, 2000); software used to prepare material for publication: SHELXTL.

(I) top
Crystal data top
C8H20N·C7H7MoN2O5F(000) = 1760
Mr = 425.34Dx = 1.563 Mg m3
Monoclinic, C2/cMo Kα radiation, λ = 0.71073 Å
Hall symbol: -C 2ycCell parameters from 7575 reflections
a = 12.0407 (8) Åθ = 2.4–28.2°
b = 12.8897 (8) ŵ = 0.76 mm1
c = 23.4746 (14) ÅT = 110 K
β = 97.177 (1)°Plate, yellow
V = 3614.7 (4) Å30.18 × 0.14 × 0.10 mm
Z = 8
Data collection top
Bruker X8 Apex
diffractometer
4538 independent reflections
Radiation source: fine-focus sealed tube3956 reflections with I > 2σ(I)
Graphite monochromatorRint = 0.036
φ and ω scansθmax = 28.5°, θmin = 2.3°
Absorption correction: multi-scan
(SADABS; Bruker, 2002)
h = 1616
Tmin = 0.877, Tmax = 0.928k = 1717
24788 measured reflectionsl = 3131
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)] = 0.023Hydrogen site location: inferred from neighbouring sites
wR(F2) = 0.057H-atom parameters constrained
S = 1.04 w = 1/[σ2(Fo2) + (0.0281P)2 + 3.1028P]
where P = (Fo2 + 2Fc2)/3
4538 reflections(Δ/σ)max = 0.004
217 parametersΔρmax = 0.40 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
Mo10.757171 (10)1.110459 (10)0.580094 (5)0.01194 (5)
O10.72614 (9)0.94861 (9)0.54995 (5)0.0153 (2)
O20.61288 (10)0.84434 (9)0.49299 (5)0.0191 (2)
O30.93071 (10)1.05991 (10)0.68641 (5)0.0247 (3)
O40.57005 (11)1.13770 (10)0.65824 (5)0.0250 (3)
O50.78205 (11)1.33504 (10)0.62824 (5)0.0242 (3)
N10.62992 (11)1.12327 (10)0.49838 (6)0.0142 (3)
H1A0.56121.14240.50830.017*
H1B0.65291.17370.47470.017*
N20.87662 (11)1.11385 (10)0.51291 (6)0.0151 (3)
N30.72649 (11)0.72615 (10)0.67705 (5)0.0135 (3)
C10.65411 (13)0.93069 (12)0.50632 (7)0.0142 (3)
C20.61941 (13)1.02290 (12)0.46738 (6)0.0156 (3)
H2A0.66671.02460.43580.019*
H2B0.54081.01350.45010.019*
C30.86567 (14)1.07823 (13)0.64624 (7)0.0161 (3)
C40.64064 (14)1.12040 (12)0.62949 (7)0.0161 (3)
C50.77636 (13)1.25166 (13)0.60716 (7)0.0164 (3)
C60.93163 (13)1.12365 (12)0.47699 (7)0.0149 (3)
C71.00322 (14)1.13859 (13)0.43192 (7)0.0187 (3)
H7A0.95681.14320.39460.028*
H7B1.05471.07980.43170.028*
H7C1.04621.20280.43910.028*
C80.61405 (13)0.77087 (13)0.68780 (7)0.0177 (3)
H8A0.55750.71480.68280.021*
H8B0.61980.79410.72830.021*
C90.57237 (16)0.86078 (15)0.64949 (9)0.0271 (4)
H9A0.49980.88410.65940.041*
H9B0.56410.83840.60930.041*
H9C0.62630.91800.65500.041*
C100.72682 (14)0.69573 (13)0.61450 (7)0.0177 (3)
H10A0.71370.75870.59050.021*
H10B0.80200.66880.60940.021*
C110.64011 (15)0.61475 (15)0.59289 (8)0.0242 (4)
H11A0.64510.60020.55230.036*
H11B0.56510.64090.59710.036*
H11C0.65410.55090.61530.036*
C120.81975 (13)0.80628 (13)0.68920 (7)0.0176 (3)
H12A0.88970.77600.67840.021*
H12B0.80080.86710.66410.021*
C130.84208 (15)0.84370 (14)0.75062 (7)0.0228 (4)
H13A0.90370.89380.75410.034*
H13B0.86230.78450.77600.034*
H13C0.77460.87700.76150.034*
C140.74489 (14)0.63300 (12)0.71691 (7)0.0163 (3)
H14A0.75020.65780.75710.020*
H14B0.67850.58720.71010.020*
C150.84839 (14)0.56937 (14)0.71016 (8)0.0219 (4)
H15A0.85410.51160.73750.033*
H15B0.91500.61340.71760.033*
H15C0.84290.54200.67100.033*
Atomic displacement parameters (Å2) top
U11U22U33U12U13U23
Mo10.01195 (7)0.01341 (7)0.01059 (7)0.00176 (5)0.00186 (5)0.00013 (5)
O10.0158 (5)0.0146 (6)0.0149 (5)0.0004 (4)0.0001 (4)0.0002 (4)
O20.0178 (6)0.0153 (6)0.0239 (6)0.0012 (5)0.0012 (5)0.0034 (5)
O30.0231 (6)0.0317 (7)0.0181 (6)0.0056 (5)0.0030 (5)0.0060 (5)
O40.0235 (6)0.0319 (7)0.0214 (6)0.0021 (5)0.0097 (5)0.0020 (5)
O50.0333 (7)0.0191 (6)0.0217 (6)0.0070 (5)0.0091 (5)0.0049 (5)
N10.0147 (6)0.0140 (7)0.0140 (6)0.0003 (5)0.0020 (5)0.0005 (5)
N20.0139 (6)0.0165 (7)0.0148 (6)0.0009 (5)0.0008 (5)0.0011 (5)
N30.0128 (6)0.0148 (6)0.0134 (6)0.0006 (5)0.0029 (5)0.0015 (5)
C10.0126 (7)0.0157 (8)0.0153 (7)0.0010 (6)0.0054 (6)0.0016 (6)
C20.0178 (7)0.0159 (8)0.0128 (7)0.0003 (6)0.0013 (6)0.0010 (6)
C30.0168 (7)0.0159 (8)0.0164 (8)0.0045 (6)0.0054 (6)0.0005 (6)
C40.0178 (7)0.0157 (8)0.0143 (7)0.0037 (6)0.0005 (6)0.0004 (6)
C50.0158 (7)0.0205 (8)0.0134 (7)0.0020 (6)0.0045 (6)0.0033 (6)
C60.0142 (7)0.0128 (7)0.0168 (7)0.0002 (6)0.0014 (6)0.0014 (6)
C70.0193 (8)0.0186 (8)0.0193 (8)0.0011 (6)0.0067 (6)0.0011 (6)
C80.0141 (7)0.0194 (8)0.0205 (8)0.0005 (6)0.0053 (6)0.0005 (7)
C90.0231 (9)0.0258 (9)0.0337 (10)0.0083 (7)0.0086 (8)0.0069 (8)
C100.0182 (8)0.0220 (8)0.0131 (7)0.0001 (6)0.0028 (6)0.0011 (6)
C110.0209 (8)0.0305 (10)0.0206 (9)0.0031 (7)0.0001 (7)0.0062 (7)
C120.0162 (7)0.0169 (8)0.0201 (8)0.0049 (6)0.0042 (6)0.0012 (6)
C130.0258 (9)0.0210 (9)0.0218 (9)0.0057 (7)0.0032 (7)0.0030 (7)
C140.0170 (7)0.0153 (8)0.0165 (8)0.0016 (6)0.0022 (6)0.0032 (6)
C150.0203 (8)0.0217 (9)0.0233 (9)0.0044 (7)0.0007 (7)0.0028 (7)
Geometric parameters (Å, º) top
Mo1—C51.9320 (17)C7—H7C0.9800
Mo1—C41.9329 (17)C8—C91.514 (2)
Mo1—C31.9452 (17)C8—H8A0.9900
Mo1—O12.2195 (11)C8—H8B0.9900
Mo1—N22.2637 (14)C9—H9A0.9800
Mo1—N12.3066 (13)C9—H9B0.9800
O1—C11.2778 (19)C9—H9C0.9800
O2—C11.243 (2)C10—C111.518 (2)
O3—C31.172 (2)C10—H10A0.9900
O4—C41.171 (2)C10—H10B0.9900
O5—C51.182 (2)C11—H11A0.9800
N1—C21.482 (2)C11—H11B0.9800
N1—H1A0.9200C11—H11C0.9800
N1—H1B0.9200C12—C131.512 (2)
N2—C61.142 (2)C12—H12A0.9900
N3—C101.520 (2)C12—H12B0.9900
N3—C81.521 (2)C13—H13A0.9800
N3—C141.521 (2)C13—H13B0.9800
N3—C121.526 (2)C13—H13C0.9800
C1—C21.526 (2)C14—C151.517 (2)
C2—H2A0.9900C14—H14A0.9900
C2—H2B0.9900C14—H14B0.9900
C6—C71.459 (2)C15—H15A0.9800
C7—H7A0.9800C15—H15B0.9800
C7—H7B0.9800C15—H15C0.9800
C5—Mo1—C478.83 (7)C9—C8—N3115.31 (13)
C5—Mo1—C384.14 (7)C9—C8—H8A108.4
C4—Mo1—C390.04 (7)N3—C8—H8A108.4
C5—Mo1—O1177.08 (5)C9—C8—H8B108.4
C4—Mo1—O198.49 (6)N3—C8—H8B108.4
C3—Mo1—O197.08 (6)H8A—C8—H8B107.5
C5—Mo1—N298.66 (6)C8—C9—H9A109.5
C4—Mo1—N2171.36 (6)C8—C9—H9B109.5
C3—Mo1—N297.96 (6)H9A—C9—H9B109.5
O1—Mo1—N283.82 (4)C8—C9—H9C109.5
C5—Mo1—N1104.22 (6)H9A—C9—H9C109.5
C4—Mo1—N192.15 (6)H9B—C9—H9C109.5
C3—Mo1—N1171.62 (6)C11—C10—N3114.54 (13)
O1—Mo1—N174.59 (4)C11—C10—H10A108.6
N2—Mo1—N180.39 (5)N3—C10—H10A108.6
C1—O1—Mo1119.72 (10)C11—C10—H10B108.6
C2—N1—Mo1110.66 (9)N3—C10—H10B108.6
C2—N1—H1A109.5H10A—C10—H10B107.6
Mo1—N1—H1A109.5C10—C11—H11A109.5
C2—N1—H1B109.5C10—C11—H11B109.5
Mo1—N1—H1B109.5H11A—C11—H11B109.5
H1A—N1—H1B108.1C10—C11—H11C109.5
C6—N2—Mo1173.57 (13)H11A—C11—H11C109.5
C10—N3—C8111.58 (12)H11B—C11—H11C109.5
C10—N3—C14111.88 (12)C13—C12—N3115.66 (13)
C8—N3—C14105.15 (12)C13—C12—H12A108.4
C10—N3—C12105.33 (12)N3—C12—H12A108.4
C8—N3—C12111.21 (12)C13—C12—H12B108.4
C14—N3—C12111.84 (12)N3—C12—H12B108.4
O2—C1—O1125.00 (15)H12A—C12—H12B107.4
O2—C1—C2118.43 (14)C12—C13—H13A109.5
O1—C1—C2116.56 (14)C12—C13—H13B109.5
N1—C2—C1112.69 (12)H13A—C13—H13B109.5
N1—C2—H2A109.1C12—C13—H13C109.5
C1—C2—H2A109.1H13A—C13—H13C109.5
N1—C2—H2B109.1H13B—C13—H13C109.5
C1—C2—H2B109.1C15—C14—N3114.90 (13)
H2A—C2—H2B107.8C15—C14—H14A108.5
O3—C3—Mo1179.19 (16)N3—C14—H14A108.5
O4—C4—Mo1172.76 (14)C15—C14—H14B108.5
O5—C5—Mo1173.14 (13)N3—C14—H14B108.5
N2—C6—C7178.48 (18)H14A—C14—H14B107.5
C6—C7—H7A109.5C14—C15—H15A109.5
C6—C7—H7B109.5C14—C15—H15B109.5
H7A—C7—H7B109.5H15A—C15—H15B109.5
C6—C7—H7C109.5C14—C15—H15C109.5
H7A—C7—H7C109.5H15A—C15—H15C109.5
H7B—C7—H7C109.5H15B—C15—H15C109.5
Hydrogen-bond geometry (Å, º) top
D—H···AD—HH···AD···AD—H···A
N1—H1A···O2i0.922.102.9849 (17)161
Symmetry code: (i) x+1, y+2, z+1.
 

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