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The structure of the title compound, [Mo(η6-C4Me4B2F2)2(CO)2], (II), was determined by X-ray crystallography at 173 K and has two independent mol­ecules of (II) in the asymmetric unit. The six-membered diboracycles are η6-coordinated [Mo—Calkene = 2.4157 (18)–2.6008 (19); Mo—B = 2.538 (2)–2.621 (2) Å].

Supporting information

cif

Crystallographic Information File (CIF) https://doi.org/10.1107/S1600536801014167/wn6036sup1.cif
Contains datablocks I, global

hkl

Structure factor file (CIF format) https://doi.org/10.1107/S1600536801014167/wn6036Isup2.hkl
Contains datablock I

CCDC reference: 175320

Key indicators

  • Single-crystal X-ray study
  • T = 173 K
  • Mean [sigma](C-C) = 0.003 Å
  • R factor = 0.023
  • wR factor = 0.053
  • Data-to-parameter ratio = 16.7

checkCIF results

No syntax errors found

ADDSYM reports no extra symmetry

General Notes

ABSTM_02 When printed, the submitted absorption T values will be replaced by the scaled T values. Since the ratio of scaled T's is identical to the ratio of reported T values, the scaling does not imply a change to the absorption corrections used in the study. Ratio of Tmax expected/reported 1.106 Tmax scaled 0.807 Tmin scaled 0.634

Comment top

The reaction of boron monofluoride with but-2-yne at low temperatures yields 1,4-difluoro-2,3,5,6-tetramethyl-1,4-diboracyclohexa-2,5-diene, (I) (Timms, 1968).

Reaction of (I), which is an analogue of duroquinone, with metal–carbonyl complexes displaces carbon monoxide thermally or under photolysis to yield complexes such as [Ni(CO)2(η6-C4Me4B2F2)] and [Ni(η6-C4Me4B2F2)2] (Maddren et al., 1975). The title compound, [Mo(CO)2(C4Me4B2F2)2], (II) (Fig. 1), was prepared by a sequential photolysis from [Mo(CO)6] and (I); photolysis of a mixture of [Mo(CO)6] with 1.5 equivalents of (I) yielded [Mo(CO)4(η6-C4Me4B2F2)] (Hawker, 1981) which, after further photolysis with another equivalent of (I), gave (II). Single crystals were grown from a solution of (II) in dichloromethane at 279 K.

Compound (II) crystallizes in space group P21/n with the asymmetric unit containing two independent molecules, each having C2 symmetry (Fig. 1). The complex consists of one Mo atom in a distorted pseudo-tetrahedral environment bonded to two carbonyl units and two conversely oriented η6-rings (angles between the MoB2 units = 45.4/70.7°). Each six-membered diboracycle acts as a 4 e- donor through two alkene entities, with Mo—Calkene bond lengths ranging between 2.415 (2) and 2.601 (2) Å. Back donation to the B—F units also occurs, leading to Mo—B contacts in the range 2.538 (2)–2.621 (2) Å. The rings are almost flat with the B atoms deviating from the Mo atom by between -0.172 and -0.165 Å (Mo deviations between 1.986 and 1.994 Å).

Experimental top

Analysis of compound (II) showed the following: IR (CD2Cl2 solution, cm-1): 2001 (s), 1955 (s), ν(CO). Mass spectrum (EI, m/z): M+ 481–493 (487, most intense). NMR 1H (300 MHz, CD2Cl2, p.p.m.): δ 1.59; 11B (96 MHz, CD2Cl2, p.p.m.): δ 21.6; 19F (282 MHz, CD2Cl2, p.p.m.): δ -152.5 (very broad signal); 13C (75 MHz, CD2Cl2, p.p.m.): δ 13.7 (CH3); 13C signals for the CO and ring C atoms not observed.

Computing details top

Data collection: SMART (Bruker, 1998); cell refinement: SMART; data reduction: SAINT (Bruker, 1998); program(s) used to solve structure: SHELXTL (Bruker, 1998); program(s) used to refine structure: SHELXTL; molecular graphics: SHELXTL; software used to prepare material for publication: SHELXTL.

Figures top
[Figure 1] Fig. 1. The structure of (II) showing 50% probability displacement ellipsoids. H atoms have been omitted for clarity.
(I) top
Crystal data top
[Mo(C8H12B2F2)2(CO)2]F(000) = 1968
Mr = 487.55Dx = 1.643 Mg m3
Monoclinic, P21/nMo Kα radiation, λ = 0.71073 Å
a = 14.9106 (10) ÅCell parameters from 494 reflections
b = 8.9361 (6) Åθ = 3–50°
c = 30.252 (2) ŵ = 0.71 mm1
β = 102.074 (9)°T = 173 K
V = 3941.7 (5) Å3Block, yellow
Z = 80.5 × 0.3 × 0.3 mm
Data collection top
Siemens CCD area-detector
diffractometer
9039 independent reflections
Radiation source: fine-focus sealed tube7446 reflections with I > 2σ(I)
Graphite monochromatorRint = 0.026
ω scans with narrow framesθmax = 27.5°, θmin = 1.7°
Absorption correction: multi-scan
(SADABS; Sheldrick, 1996)
h = 1919
Tmin = 0.573, Tmax = 0.730k = 811
24739 measured reflectionsl = 3938
Refinement top
Refinement on F2Secondary atom site location: difference Fourier map
Least-squares matrix: fullHydrogen site location: inferred from neighbouring sites
R[F2 > 2σ(F2)] = 0.023H-atom parameters constrained
wR(F2) = 0.053 w = 1/[σ2(Fo2) + (0.0259P)2]
where P = (Fo2 + 2Fc2)/3
S = 0.98(Δ/σ)max = 0.004
9039 reflectionsΔρmax = 0.50 e Å3
540 parametersΔρmin = 0.61 e Å3
0 restraintsExtinction correction: SHELXL97, Fc*=kFc[1+0.001xFc2λ3/sin(2θ)]-1/4
Primary atom site location: structure-invariant direct methodsExtinction coefficient: 0.00059 (5)
Crystal data top
[Mo(C8H12B2F2)2(CO)2]V = 3941.7 (5) Å3
Mr = 487.55Z = 8
Monoclinic, P21/nMo Kα radiation
a = 14.9106 (10) ŵ = 0.71 mm1
b = 8.9361 (6) ÅT = 173 K
c = 30.252 (2) Å0.5 × 0.3 × 0.3 mm
β = 102.074 (9)°
Data collection top
Siemens CCD area-detector
diffractometer
9039 independent reflections
Absorption correction: multi-scan
(SADABS; Sheldrick, 1996)
7446 reflections with I > 2σ(I)
Tmin = 0.573, Tmax = 0.730Rint = 0.026
24739 measured reflections
Refinement top
R[F2 > 2σ(F2)] = 0.0230 restraints
wR(F2) = 0.053H-atom parameters constrained
S = 0.98Δρmax = 0.50 e Å3
9039 reflectionsΔρmin = 0.61 e Å3
540 parameters
Special details top

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

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

Fractional atomic coordinates and isotropic or equivalent isotropic displacement parameters (Å2) top
xyzUiso*/Ueq
Mo10.118430 (10)0.895528 (16)0.106372 (5)0.01529 (4)
C10.06972 (13)0.8590 (2)0.04129 (7)0.0240 (4)
O10.04511 (10)0.83535 (17)0.00340 (5)0.0352 (3)
C20.11510 (13)1.1090 (2)0.08756 (6)0.0243 (4)
O20.11014 (10)1.23185 (16)0.07697 (5)0.0356 (3)
B10.05369 (15)0.8163 (3)0.17645 (7)0.0248 (5)
B20.05420 (14)0.8603 (2)0.08570 (7)0.0230 (5)
B30.25254 (15)0.7275 (3)0.14741 (8)0.0292 (5)
B40.27317 (15)1.0012 (2)0.09956 (8)0.0249 (5)
F10.08575 (8)0.79000 (14)0.22113 (4)0.0342 (3)
F20.11559 (7)0.87392 (13)0.04538 (4)0.0303 (3)
F30.26152 (8)0.59715 (14)0.17107 (4)0.0428 (3)
F40.29780 (8)1.12666 (13)0.07880 (4)0.0352 (3)
C30.04805 (14)1.1077 (2)0.19211 (7)0.0300 (4)
H3A0.00821.13890.20140.045*
H3B0.07161.19110.17680.045*
H3C0.09411.07840.21880.045*
C40.02729 (12)0.9752 (2)0.15986 (6)0.0223 (4)
C50.03158 (12)0.9939 (2)0.11720 (6)0.0221 (4)
C60.07795 (13)1.1433 (2)0.10365 (7)0.0270 (4)
H6A0.12741.15850.12000.040*
H6B0.10351.14360.07110.040*
H6C0.03291.22410.11110.040*
C70.02945 (14)0.5775 (2)0.06584 (7)0.0308 (5)
H7A0.07350.50990.07540.046*
H7B0.02720.52280.06520.046*
H7C0.05560.61610.03560.046*
C80.00847 (12)0.7073 (2)0.09890 (6)0.0226 (4)
C90.04192 (13)0.6850 (2)0.14312 (6)0.0235 (4)
C100.06966 (14)0.5283 (2)0.15980 (7)0.0321 (5)
H10J0.01490.47130.16250.048*
H10K0.11150.53400.18940.048*
H10L0.10060.47830.13830.048*
C110.27131 (15)0.8797 (3)0.22355 (7)0.0439 (6)
H11A0.33570.90210.23680.066*
H11B0.25520.78190.23430.066*
H11C0.23200.95700.23260.066*
C120.25755 (13)0.8770 (2)0.17253 (6)0.0283 (4)
C130.26427 (13)1.0092 (2)0.14884 (6)0.0264 (4)
C140.27648 (15)1.1597 (3)0.17300 (8)0.0392 (5)
H14A0.33791.16510.19240.059*
H14B0.23031.17040.19160.059*
H14C0.26911.24040.15060.059*
C150.22395 (15)0.5757 (2)0.07059 (8)0.0371 (5)
H15A0.28020.54920.06050.056*
H15B0.17320.58520.04430.056*
H15C0.20960.49730.09070.056*
C160.23771 (12)0.7236 (2)0.09588 (7)0.0249 (4)
C170.25451 (12)0.8563 (2)0.07290 (6)0.0221 (4)
C180.25990 (13)0.8541 (2)0.02343 (6)0.0310 (5)
H18A0.32210.82650.02070.047*
H18B0.24500.95360.01030.047*
H18C0.21610.78080.00730.047*
Mo20.635253 (10)0.667490 (16)0.144034 (5)0.01456 (4)
C1010.64875 (12)0.7194 (2)0.20863 (6)0.0229 (4)
O1010.66209 (10)0.74962 (17)0.24640 (4)0.0341 (4)
C1020.66101 (13)0.4597 (2)0.16570 (6)0.0250 (4)
O1020.66956 (10)0.33844 (16)0.17830 (5)0.0365 (4)
B1010.48716 (14)0.7310 (3)0.17005 (7)0.0236 (5)
B1020.49326 (14)0.6813 (3)0.07644 (7)0.0253 (5)
B1030.72851 (15)0.8539 (3)0.10422 (8)0.0293 (5)
B1040.79139 (15)0.5618 (3)0.13769 (8)0.0269 (5)
F1010.46801 (8)0.75863 (13)0.21132 (4)0.0324 (3)
F1020.47775 (8)0.66100 (14)0.03081 (4)0.0369 (3)
F1030.71376 (9)0.99352 (14)0.08663 (5)0.0467 (4)
F1040.83624 (8)0.43080 (14)0.15060 (4)0.0422 (3)
C1030.46876 (15)0.4454 (2)0.18314 (8)0.0371 (5)
H10G0.40260.43290.18050.056*
H10H0.49760.46960.21450.056*
H10I0.49490.35230.17430.056*
C1040.48612 (12)0.5716 (2)0.15234 (6)0.0243 (4)
C1050.49431 (12)0.5463 (2)0.10709 (7)0.0254 (4)
C1060.48646 (15)0.3889 (2)0.08730 (7)0.0349 (5)
H10A0.42390.35170.08510.052*
H10B0.52980.32260.10690.052*
H10C0.50070.39120.05710.052*
C1070.52507 (14)1.0166 (2)0.16278 (7)0.0318 (5)
H10D0.47011.07650.15130.048*
H10E0.57841.06490.15460.048*
H10F0.53471.00870.19570.048*
C1080.51282 (12)0.8618 (2)0.14215 (6)0.0219 (4)
C1090.51141 (12)0.8392 (2)0.09610 (6)0.0233 (4)
C1100.51134 (15)0.9726 (2)0.06517 (7)0.0347 (5)
H11M0.45391.02840.06280.052*
H11N0.51670.93780.03510.052*
H11O0.56331.03790.07760.052*
C1110.66774 (16)0.7386 (3)0.02298 (7)0.0487 (7)
H11G0.71840.73160.00700.073*
H11H0.63880.83720.01760.073*
H11I0.62230.66070.01180.073*
C1120.70439 (13)0.7171 (3)0.07328 (6)0.0299 (5)
C1130.73057 (13)0.5740 (2)0.09058 (6)0.0281 (4)
C1140.71287 (16)0.4355 (3)0.06088 (8)0.0484 (7)
H11P0.75780.43080.04150.073*
H11Q0.65090.44050.04200.073*
H11R0.71840.34600.08000.073*
C1150.78149 (15)0.9703 (2)0.18572 (8)0.0384 (5)
H11J0.84700.99490.19270.058*
H11K0.76130.94750.21380.058*
H11L0.74661.05570.17070.058*
C1160.76526 (12)0.8348 (2)0.15459 (7)0.0251 (4)
C1170.80070 (12)0.6928 (2)0.17047 (6)0.0240 (4)
C1180.85520 (14)0.6700 (3)0.21833 (7)0.0360 (5)
H11D0.91940.69780.21990.054*
H11E0.85190.56470.22690.054*
H11F0.82950.73280.23920.054*
Atomic displacement parameters (Å2) top
U11U22U33U12U13U23
Mo10.01401 (7)0.01448 (8)0.01732 (8)0.00037 (6)0.00318 (5)0.00074 (6)
C10.0188 (9)0.0246 (11)0.0291 (10)0.0000 (8)0.0061 (8)0.0002 (8)
O10.0292 (8)0.0525 (10)0.0224 (7)0.0037 (7)0.0021 (6)0.0057 (7)
C20.0205 (9)0.0242 (11)0.0282 (10)0.0030 (8)0.0053 (8)0.0015 (8)
O20.0329 (8)0.0212 (8)0.0528 (10)0.0011 (6)0.0097 (7)0.0054 (7)
B10.0207 (11)0.0299 (13)0.0252 (11)0.0018 (9)0.0081 (9)0.0034 (9)
B20.0152 (10)0.0270 (12)0.0281 (11)0.0016 (8)0.0078 (8)0.0006 (9)
B30.0161 (11)0.0334 (13)0.0381 (13)0.0042 (9)0.0055 (10)0.0104 (11)
B40.0183 (10)0.0257 (12)0.0309 (12)0.0019 (9)0.0057 (9)0.0021 (9)
F10.0393 (7)0.0380 (7)0.0254 (6)0.0013 (6)0.0068 (5)0.0049 (5)
F20.0223 (6)0.0341 (7)0.0318 (6)0.0027 (5)0.0007 (5)0.0026 (5)
F30.0328 (7)0.0416 (8)0.0525 (8)0.0080 (6)0.0053 (6)0.0225 (6)
F40.0337 (7)0.0289 (7)0.0470 (7)0.0082 (5)0.0178 (6)0.0005 (5)
C30.0311 (11)0.0288 (11)0.0322 (11)0.0008 (9)0.0112 (9)0.0074 (9)
C40.0209 (9)0.0237 (10)0.0247 (9)0.0022 (8)0.0102 (8)0.0027 (8)
C50.0187 (9)0.0216 (10)0.0283 (10)0.0010 (7)0.0099 (8)0.0009 (8)
C60.0253 (10)0.0214 (10)0.0354 (11)0.0047 (8)0.0090 (9)0.0004 (8)
C70.0289 (11)0.0233 (11)0.0400 (12)0.0041 (8)0.0069 (9)0.0054 (9)
C80.0193 (9)0.0201 (10)0.0299 (10)0.0027 (8)0.0087 (8)0.0018 (8)
C90.0208 (9)0.0205 (10)0.0313 (10)0.0014 (7)0.0098 (8)0.0033 (8)
C100.0318 (11)0.0223 (11)0.0429 (12)0.0003 (9)0.0092 (9)0.0063 (9)
C110.0310 (12)0.0742 (18)0.0256 (11)0.0063 (11)0.0036 (9)0.0016 (11)
C120.0155 (9)0.0436 (13)0.0242 (10)0.0005 (8)0.0005 (8)0.0004 (9)
C130.0169 (9)0.0349 (12)0.0266 (10)0.0039 (8)0.0026 (8)0.0081 (8)
C140.0303 (12)0.0454 (14)0.0418 (13)0.0112 (10)0.0073 (10)0.0209 (11)
C150.0309 (12)0.0273 (12)0.0549 (14)0.0034 (9)0.0129 (10)0.0082 (10)
C160.0169 (9)0.0229 (10)0.0350 (11)0.0027 (8)0.0058 (8)0.0032 (8)
C170.0150 (9)0.0278 (11)0.0237 (9)0.0020 (7)0.0043 (7)0.0011 (8)
C180.0238 (10)0.0431 (13)0.0277 (10)0.0004 (9)0.0087 (8)0.0048 (9)
Mo20.01347 (7)0.01412 (8)0.01569 (7)0.00063 (6)0.00209 (5)0.00011 (6)
C1010.0184 (9)0.0243 (10)0.0259 (10)0.0007 (8)0.0047 (8)0.0018 (8)
O1010.0312 (8)0.0481 (10)0.0225 (8)0.0013 (7)0.0043 (6)0.0048 (6)
C1020.0202 (9)0.0260 (11)0.0281 (10)0.0008 (8)0.0036 (8)0.0017 (8)
O1020.0348 (8)0.0234 (8)0.0489 (9)0.0046 (6)0.0036 (7)0.0099 (7)
B1010.0162 (10)0.0274 (12)0.0272 (11)0.0016 (9)0.0046 (9)0.0013 (9)
B1020.0159 (10)0.0329 (14)0.0254 (11)0.0010 (9)0.0003 (9)0.0017 (9)
B1030.0192 (11)0.0305 (13)0.0391 (13)0.0026 (9)0.0082 (10)0.0095 (10)
B1040.0186 (11)0.0302 (13)0.0339 (12)0.0018 (9)0.0099 (9)0.0003 (10)
F1010.0316 (7)0.0393 (8)0.0293 (6)0.0048 (5)0.0134 (5)0.0005 (5)
F1020.0363 (7)0.0472 (8)0.0236 (6)0.0008 (6)0.0020 (5)0.0045 (5)
F1030.0339 (7)0.0379 (8)0.0663 (9)0.0061 (6)0.0056 (6)0.0240 (7)
F1040.0321 (7)0.0335 (7)0.0621 (9)0.0118 (6)0.0124 (6)0.0008 (6)
C1030.0302 (11)0.0290 (12)0.0560 (14)0.0010 (9)0.0178 (10)0.0099 (10)
C1040.0152 (9)0.0238 (10)0.0340 (10)0.0008 (7)0.0057 (8)0.0041 (8)
C1050.0180 (9)0.0225 (10)0.0330 (10)0.0018 (8)0.0010 (8)0.0035 (8)
C1060.0322 (12)0.0252 (11)0.0435 (12)0.0045 (9)0.0007 (10)0.0089 (9)
C1070.0317 (11)0.0231 (11)0.0396 (12)0.0014 (9)0.0051 (9)0.0027 (9)
C1080.0172 (9)0.0171 (10)0.0301 (10)0.0030 (7)0.0021 (8)0.0007 (7)
C1090.0182 (9)0.0232 (10)0.0273 (10)0.0027 (8)0.0022 (8)0.0063 (8)
C1100.0374 (12)0.0293 (12)0.0377 (12)0.0065 (9)0.0085 (10)0.0122 (9)
C1110.0335 (13)0.090 (2)0.0223 (11)0.0091 (13)0.0057 (10)0.0077 (11)
C1120.0189 (10)0.0507 (13)0.0213 (10)0.0047 (9)0.0069 (8)0.0003 (9)
C1130.0227 (10)0.0365 (12)0.0279 (10)0.0038 (9)0.0117 (8)0.0106 (9)
C1140.0394 (13)0.0594 (17)0.0492 (14)0.0103 (12)0.0157 (11)0.0323 (13)
C1150.0343 (12)0.0326 (13)0.0518 (14)0.0128 (10)0.0170 (11)0.0142 (10)
C1160.0170 (9)0.0287 (11)0.0317 (10)0.0064 (8)0.0098 (8)0.0034 (8)
C1170.0143 (9)0.0327 (12)0.0257 (10)0.0024 (8)0.0055 (7)0.0018 (8)
C1180.0232 (11)0.0544 (15)0.0290 (11)0.0001 (10)0.0023 (9)0.0007 (10)
Geometric parameters (Å, º) top
Mo1—C11.9780 (19)Mo2—C1011.9772 (19)
Mo1—C21.988 (2)Mo2—C1021.980 (2)
Mo1—C162.4208 (18)Mo2—C1162.4160 (18)
Mo1—C42.4272 (17)Mo2—C1052.4199 (18)
Mo1—C172.4749 (18)Mo2—C1172.4395 (18)
Mo1—C52.4881 (18)Mo2—C1042.4446 (18)
Mo1—C132.4983 (18)Mo2—C1132.5089 (18)
Mo1—C82.5064 (18)Mo2—C1082.5113 (18)
Mo1—B22.538 (2)Mo2—B1042.556 (2)
Mo1—B42.541 (2)Mo2—B1012.558 (2)
Mo1—C122.5689 (19)Mo2—C1092.5976 (18)
Mo1—C92.5703 (18)Mo2—C1122.6009 (18)
C1—O11.148 (2)C101—O1011.150 (2)
C2—O21.141 (2)C102—O1021.147 (2)
B1—F11.357 (2)B101—F1011.360 (2)
B1—C41.530 (3)B101—C1041.521 (3)
B1—C91.533 (3)B101—C1081.536 (3)
B2—F21.369 (2)B102—F1021.363 (2)
B2—C51.521 (3)B102—C1051.520 (3)
B2—C81.543 (3)B102—C1091.533 (3)
B3—F31.359 (3)B103—F1031.356 (3)
B3—C161.528 (3)B103—C1161.517 (3)
B3—C121.531 (3)B103—C1121.536 (3)
B4—F41.372 (2)B104—F1041.364 (3)
B4—C171.520 (3)B104—C1171.521 (3)
B4—C131.526 (3)B104—C1131.525 (3)
C3—C41.524 (3)C103—C1041.519 (3)
C4—C51.411 (3)C104—C1051.418 (3)
C5—C61.519 (2)C105—C1061.523 (3)
C7—C81.521 (3)C107—C1081.513 (3)
C8—C91.405 (3)C108—C1091.403 (3)
C9—C101.517 (3)C109—C1101.515 (3)
C11—C121.514 (3)C111—C1121.518 (3)
C12—C131.396 (3)C112—C1131.406 (3)
C13—C141.524 (3)C113—C1141.520 (3)
C15—C161.519 (3)C115—C1161.521 (3)
C16—C171.423 (3)C116—C1171.420 (3)
C17—C181.516 (2)C117—C1181.518 (3)
C1—Mo1—C283.77 (8)C101—Mo2—C10285.42 (8)
C1—Mo1—C1683.78 (7)C101—Mo2—C11679.12 (7)
C2—Mo1—C16123.12 (7)C102—Mo2—C116116.23 (7)
C1—Mo1—C4124.87 (7)C101—Mo2—C105117.41 (7)
C2—Mo1—C485.71 (7)C102—Mo2—C10579.80 (7)
C16—Mo1—C4143.39 (7)C116—Mo2—C105158.96 (7)
C1—Mo1—C1774.40 (7)C101—Mo2—C11776.55 (7)
C2—Mo1—C1789.57 (7)C102—Mo2—C11782.26 (7)
C16—Mo1—C1733.77 (6)C116—Mo2—C11734.00 (6)
C4—Mo1—C17159.32 (6)C105—Mo2—C117156.04 (6)
C1—Mo1—C592.08 (7)C101—Mo2—C10483.53 (7)
C2—Mo1—C574.29 (7)C102—Mo2—C10475.81 (7)
C16—Mo1—C5161.25 (6)C116—Mo2—C104157.72 (6)
C4—Mo1—C533.33 (6)C105—Mo2—C10433.88 (6)
C17—Mo1—C5160.15 (6)C117—Mo2—C104151.40 (6)
C1—Mo1—C13132.68 (7)C101—Mo2—C113139.54 (7)
C2—Mo1—C1373.99 (7)C102—Mo2—C11378.72 (7)
C16—Mo1—C1374.99 (6)C116—Mo2—C11375.18 (6)
C4—Mo1—C1394.96 (6)C105—Mo2—C11396.18 (6)
C17—Mo1—C1364.41 (6)C117—Mo2—C11364.64 (6)
C5—Mo1—C13119.90 (6)C104—Mo2—C113126.85 (6)
C1—Mo1—C871.72 (7)C101—Mo2—C10877.50 (7)
C2—Mo1—C8130.16 (7)C102—Mo2—C108138.22 (7)
C16—Mo1—C897.10 (6)C116—Mo2—C10897.72 (6)
C4—Mo1—C874.91 (6)C105—Mo2—C10875.05 (6)
C17—Mo1—C8122.41 (6)C117—Mo2—C108128.60 (6)
C5—Mo1—C864.32 (6)C104—Mo2—C10864.67 (6)
C13—Mo1—C8151.47 (6)C113—Mo2—C108136.27 (7)
C1—Mo1—B265.92 (7)C101—Mo2—B104104.76 (7)
C2—Mo1—B294.88 (7)C102—Mo2—B10464.01 (8)
C16—Mo1—B2128.62 (7)C116—Mo2—B10461.34 (7)
C4—Mo1—B261.33 (7)C105—Mo2—B104121.10 (7)
C17—Mo1—B2139.26 (6)C117—Mo2—B10435.36 (7)
C5—Mo1—B235.21 (6)C104—Mo2—B104137.77 (7)
C13—Mo1—B2154.94 (7)C113—Mo2—B10435.02 (7)
C8—Mo1—B235.62 (6)C108—Mo2—B104157.33 (7)
C1—Mo1—B497.54 (7)C101—Mo2—B10163.89 (7)
C2—Mo1—B465.74 (7)C102—Mo2—B101103.08 (7)
C16—Mo1—B461.36 (7)C116—Mo2—B101122.84 (7)
C4—Mo1—B4126.13 (7)C105—Mo2—B10161.27 (7)
C17—Mo1—B435.25 (6)C117—Mo2—B101139.23 (7)
C5—Mo1—B4137.39 (7)C104—Mo2—B10135.30 (7)
C13—Mo1—B435.24 (6)C113—Mo2—B101156.06 (7)
C8—Mo1—B4157.40 (7)C108—Mo2—B10135.27 (7)
B2—Mo1—B4156.54 (7)B104—Mo2—B101164.42 (7)
C1—Mo1—C12146.45 (7)C101—Mo2—C109109.07 (7)
C2—Mo1—C12104.64 (7)C102—Mo2—C109143.61 (7)
C16—Mo1—C1264.24 (6)C116—Mo2—C10999.51 (6)
C4—Mo1—C1288.45 (6)C105—Mo2—C10963.85 (6)
C17—Mo1—C1273.27 (6)C117—Mo2—C109132.87 (6)
C5—Mo1—C12121.46 (6)C104—Mo2—C10973.07 (6)
C13—Mo1—C1231.95 (6)C113—Mo2—C109105.62 (6)
C8—Mo1—C12119.88 (6)C108—Mo2—C10931.83 (6)
B2—Mo1—C12142.75 (7)B104—Mo2—C109136.76 (7)
B4—Mo1—C1259.22 (7)B101—Mo2—C10958.82 (6)
C1—Mo1—C9101.88 (7)C101—Mo2—C112142.89 (7)
C2—Mo1—C9147.05 (7)C102—Mo2—C112110.46 (7)
C16—Mo1—C989.82 (6)C116—Mo2—C11263.78 (6)
C4—Mo1—C964.24 (6)C105—Mo2—C11298.72 (6)
C17—Mo1—C9123.31 (6)C117—Mo2—C11272.92 (6)
C5—Mo1—C973.09 (6)C104—Mo2—C112132.07 (6)
C13—Mo1—C9119.50 (6)C113—Mo2—C11231.87 (7)
C8—Mo1—C932.09 (6)C108—Mo2—C112105.95 (7)
B2—Mo1—C959.80 (6)B104—Mo2—C11258.48 (7)
B4—Mo1—C9143.10 (7)B101—Mo2—C112137.03 (7)
C12—Mo1—C988.56 (6)C109—Mo2—C11278.33 (6)
O1—C1—Mo1177.02 (16)O101—C101—Mo2175.97 (16)
O2—C2—Mo1177.63 (17)O102—C102—Mo2175.21 (17)
F1—B1—C4120.05 (18)F101—B101—C104120.32 (18)
F1—B1—C9119.38 (18)F101—B101—C108119.36 (18)
C4—B1—C9120.55 (17)C104—B101—C108120.29 (17)
F1—B1—Mo1138.13 (14)F101—B101—Mo2133.09 (14)
C4—B1—Mo166.07 (10)C104—B101—Mo268.27 (10)
C9—B1—Mo171.55 (10)C108—B101—Mo270.70 (10)
F2—B2—C5120.54 (18)F102—B102—C105119.32 (18)
F2—B2—C8119.09 (17)F102—B102—C109119.63 (18)
C5—B2—C8120.37 (17)C105—B102—C109121.04 (18)
F2—B2—Mo1131.55 (13)F102—B102—Mo2136.23 (14)
C5—B2—Mo170.60 (10)C105—B102—Mo265.35 (10)
C8—B2—Mo171.07 (10)C109—B102—Mo272.09 (11)
F3—B3—C16119.7 (2)F103—B103—C116119.5 (2)
F3—B3—C12119.8 (2)F103—B103—C112119.7 (2)
C16—B3—C12120.52 (19)C116—B103—C112120.82 (19)
F3—B3—Mo1136.71 (14)F103—B103—Mo2135.02 (15)
C16—B3—Mo166.00 (11)C116—B103—Mo265.27 (10)
C12—B3—Mo171.69 (11)C112—B103—Mo272.25 (11)
F4—B4—C17119.35 (18)F104—B104—C117120.07 (19)
F4—B4—C13119.69 (18)F104—B104—C113119.27 (19)
C17—B4—C13120.96 (18)C117—B104—C113120.64 (19)
F4—B4—Mo1132.47 (14)F104—B104—Mo2134.04 (14)
C17—B4—Mo170.00 (10)C117—B104—Mo268.12 (10)
C13—B4—Mo170.86 (11)C113—B104—Mo270.79 (11)
C5—C4—C3119.85 (17)C105—C104—C103122.29 (18)
C5—C4—B1118.58 (17)C105—C104—B101119.53 (17)
C3—C4—B1120.46 (17)C103—C104—B101118.01 (18)
C5—C4—Mo175.70 (10)C105—C104—Mo272.10 (10)
C3—C4—Mo1125.99 (12)C103—C104—Mo2126.77 (13)
B1—C4—Mo178.75 (11)B101—C104—Mo276.43 (11)
C4—C5—C6120.79 (16)C104—C105—B102118.07 (18)
C4—C5—B2119.61 (17)C104—C105—C106120.76 (18)
C6—C5—B2119.46 (17)B102—C105—C106120.21 (18)
C4—C5—Mo170.97 (10)C104—C105—Mo274.01 (10)
C6—C5—Mo1130.23 (12)B102—C105—Mo279.84 (11)
B2—C5—Mo174.19 (10)C106—C105—Mo2125.63 (13)
C9—C8—C7120.93 (17)C109—C108—C107121.08 (17)
C9—C8—B2119.43 (17)C109—C108—B101118.84 (17)
C7—C8—B2119.12 (17)C107—C108—B101119.44 (17)
C9—C8—Mo176.46 (11)C109—C108—Mo277.47 (11)
C7—C8—Mo1128.22 (12)C107—C108—Mo2126.76 (13)
B2—C8—Mo173.31 (10)B101—C108—Mo274.03 (11)
C8—C9—C10120.14 (17)C108—C109—C110119.86 (18)
C8—C9—B1118.87 (17)C108—C109—B102118.82 (17)
C10—C9—B1120.14 (17)C110—C109—B102120.48 (18)
C8—C9—Mo171.45 (10)C108—C109—Mo270.69 (10)
C10—C9—Mo1134.83 (13)C110—C109—Mo2135.90 (13)
B1—C9—Mo173.99 (11)B102—C109—Mo273.74 (11)
C13—C12—C11120.03 (19)C113—C112—C111120.1 (2)
C13—C12—B3118.99 (18)C113—C112—B103119.05 (18)
C11—C12—B3120.17 (19)C111—C112—B103120.0 (2)
C13—C12—Mo171.24 (11)C113—C112—Mo270.46 (11)
C11—C12—Mo1135.10 (14)C111—C112—Mo2136.48 (14)
B3—C12—Mo173.86 (11)B103—C112—Mo273.54 (11)
C12—C13—C14121.00 (18)C112—C113—C114121.36 (19)
C12—C13—B4119.49 (18)C112—C113—B104118.53 (18)
C14—C13—B4118.94 (18)C114—C113—B104119.3 (2)
C12—C13—Mo176.81 (11)C112—C113—Mo277.68 (11)
C14—C13—Mo1127.54 (13)C114—C113—Mo2126.90 (14)
B4—C13—Mo173.90 (11)B104—C113—Mo274.19 (11)
C17—C16—C15119.85 (18)C117—C116—B103118.08 (18)
C17—C16—B3118.47 (18)C117—C116—C115120.14 (19)
C15—C16—B3120.60 (19)B103—C116—C115120.65 (19)
C17—C16—Mo175.20 (11)C117—C116—Mo273.91 (10)
C15—C16—Mo1126.34 (13)B103—C116—Mo279.94 (11)
B3—C16—Mo178.78 (11)C115—C116—Mo2126.41 (13)
C16—C17—C18121.53 (17)C116—C117—C118121.97 (18)
C16—C17—B4118.82 (17)C116—C117—B104119.37 (18)
C18—C17—B4119.54 (17)C118—C117—B104118.44 (18)
C16—C17—Mo171.03 (10)C116—C117—Mo272.09 (10)
C18—C17—Mo1128.55 (12)C118—C117—Mo2127.09 (13)
B4—C17—Mo174.75 (11)B104—C117—Mo276.52 (11)

Experimental details

Crystal data
Chemical formula[Mo(C8H12B2F2)2(CO)2]
Mr487.55
Crystal system, space groupMonoclinic, P21/n
Temperature (K)173
a, b, c (Å)14.9106 (10), 8.9361 (6), 30.252 (2)
β (°) 102.074 (9)
V3)3941.7 (5)
Z8
Radiation typeMo Kα
µ (mm1)0.71
Crystal size (mm)0.5 × 0.3 × 0.3
Data collection
DiffractometerSiemens CCD area-detector
diffractometer
Absorption correctionMulti-scan
(SADABS; Sheldrick, 1996)
Tmin, Tmax0.573, 0.730
No. of measured, independent and
observed [I > 2σ(I)] reflections
24739, 9039, 7446
Rint0.026
(sin θ/λ)max1)0.650
Refinement
R[F2 > 2σ(F2)], wR(F2), S 0.023, 0.053, 0.98
No. of reflections9039
No. of parameters540
H-atom treatmentH-atom parameters constrained
Δρmax, Δρmin (e Å3)0.50, 0.61

Computer programs: SMART (Bruker, 1998), SMART, SAINT (Bruker, 1998), SHELXTL (Bruker, 1998), SHELXTL.

 

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