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The title compound, tetra­butyl­ammonium chloro­hepta­iso­butyl­dodeca-μ-oxo-hepta­siliconiron, [(C4H9)4N][FeSi7ClO12(C4H9)7], is an ionic species consisting of a tetra­butyl­ammonium cation and an isobutyl silsesquioxane monochloro­ferrate(III) anion. The FeIII atom in the anion is tetra­hedrally coordinated by a single Cl atom and three silanoxides from the tridentate isobutyl silsesquioxane ligand, while the cation exists also in a tetra­hedral arrangement.

Supporting information

cif

Crystallographic Information File (CIF) https://doi.org/10.1107/S1600536807000360/bt2233sup1.cif
Contains datablocks I, global

hkl

Structure factor file (CIF format) https://doi.org/10.1107/S1600536807000360/bt2233Isup2.hkl
Contains datablock I

CCDC reference: 636165

Key indicators

  • Single-crystal X-ray study
  • T = 150 K
  • Mean [sigma](C-C) = 0.008 Å
  • R factor = 0.067
  • wR factor = 0.170
  • Data-to-parameter ratio = 20.6

checkCIF/PLATON results

No syntax errors found



Alert level A PLAT220_ALERT_2_A Large Non-Solvent C Ueq(max)/Ueq(min) ... 7.27 Ratio
Author Response: There is some significant disorder within the isobutyl groups.
PLAT222_ALERT_3_A Large Non-Solvent    H     Ueq(max)/Ueq(min) ...       9.20 Ratio
Author Response: There is some significant disorder within the isobutyl groups.
PLAT222_ALERT_3_A Large Non-Solvent    H     Ueq(max)/Ueq(min) ...       5.02 Ratio
Author Response: There is some significant disorder within the isobutyl groups.
PLAT242_ALERT_2_A Check Low       Ueq as Compared to Neighbors for        C22
Author Response: There is some significant disorder within the isobutyl groups.

Alert level B PLAT220_ALERT_2_B Large Non-Solvent C Ueq(max)/Ueq(min) ... 4.03 Ratio
Author Response: There is some significant disorder within the isobutyl groups.
PLAT242_ALERT_2_B Check Low       Ueq as Compared to Neighbors for        C26
Author Response: There is some significant disorder within the isobutyl groups.

Alert level C PLAT042_ALERT_1_C Calc. and Rep. MoietyFormula Strings Differ .... ? PLAT094_ALERT_2_C Ratio of Maximum / Minimum Residual Density .... 2.74 PLAT230_ALERT_2_C Hirshfeld Test Diff for C34 - C35 .. 5.56 su PLAT230_ALERT_2_C Hirshfeld Test Diff for C35 - C36 .. 5.63 su PLAT242_ALERT_2_C Check Low Ueq as Compared to Neighbors for Si6
Author Response: There is some significant disorder within the isobutyl groups.
PLAT242_ALERT_2_C Check Low       Ueq as Compared to Neighbors for         C2
Author Response: There is some significant disorder within the isobutyl groups.
PLAT242_ALERT_2_C Check Low       Ueq as Compared to Neighbors for         C6
Author Response: There is some significant disorder within the isobutyl groups.
PLAT242_ALERT_2_C Check Low       Ueq as Compared to Neighbors for        C18
Author Response: There is some significant disorder within the isobutyl groups.
PLAT242_ALERT_2_C Check Low       Ueq as Compared to Neighbors for        C30
Author Response: There is some significant disorder within the isobutyl groups.
PLAT341_ALERT_3_C Low Bond Precision on C-C bonds (x 1000) Ang ...          8
PLAT360_ALERT_2_C Short  C(sp3)-C(sp3) Bond  C21    -   C22    ...       1.38 Ang.
PLAT360_ALERT_2_C Short  C(sp3)-C(sp3) Bond  C31    -   C32    ...       1.39 Ang.
PLAT360_ALERT_2_C Short  C(sp3)-C(sp3) Bond  C35    -   C36    ...       1.41 Ang.
PLAT396_ALERT_2_C Deviating Si-O-Si Angle from 150 Deg for      O4     160.90 Deg.
PLAT396_ALERT_2_C Deviating Si-O-Si Angle from 150 Deg for      O8     161.80 Deg.
PLAT396_ALERT_2_C Deviating Si-O-Si Angle from 150 Deg for      O9     160.50 Deg.

4 ALERT level A = In general: serious problem 2 ALERT level B = Potentially serious problem 16 ALERT level C = Check and explain 0 ALERT level G = General alerts; check 1 ALERT type 1 CIF construction/syntax error, inconsistent or missing data 18 ALERT type 2 Indicator that the structure model may be wrong or deficient 3 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: SMART (Bruker, 2001); cell refinement: SAINT (Bruker, 2001); data reduction: SAINT; program(s) used to solve structure: SHELXTL (Bruker, 2001); program(s) used to refine structure: SHELXTL; molecular graphics: SHELXTL; software used to prepare material for publication: SHELXTL.

tetrabutylammonium chloroheptaisobutyldodeca-µ-oxo-heptasiliconferrate top
Crystal data top
(C16H36N)[FeSi7ClO12(C4H9)7]F(000) = 4856
Mr = 1122.17Dx = 1.196 Mg m3
Monoclinic, C2/cMo Kα radiation, λ = 0.71073 Å
Hall symbol: -C 2ycCell parameters from 8154 reflections
a = 23.6451 (11) Åθ = 2.2–30.0°
b = 32.1149 (15) ŵ = 0.47 mm1
c = 18.3528 (9) ÅT = 150 K
β = 116.586 (1)°Block, yellow
V = 12462.8 (10) Å30.36 × 0.28 × 0.14 mm
Z = 8
Data collection top
Bruker SMART APEX CCD
diffractometer
12260 independent reflections
Radiation source: fine-focus sealed tube8887 reflections with I > 2σ(I)
Graphite monochromatorRint = 0.050
ω scansθmax = 26.0°, θmin = 1.8°
Absorption correction: multi-scan
(SADABS; Bruker, 2001)
h = 2929
Tmin = 0.849, Tmax = 0.937k = 3939
54262 measured reflectionsl = 2222
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)] = 0.067Hydrogen site location: inferred from neighbouring sites
wR(F2) = 0.170H-atom parameters constrained
S = 1.29 w = 1/[σ2(Fo2) + (0.078P)2]
where P = (Fo2 + 2Fc2)/3
12260 reflections(Δ/σ)max = 0.011
595 parametersΔρmax = 1.06 e Å3
0 restraintsΔρmin = 0.39 e Å3
Special details top

Experimental. IR [KBr, \n (cm-1)]: 2953 (vs), 2872 (s), 1477 (m), 1466 (m), 1402 (w), 1383(w), 1365(w), 1331 (w), 1230 (m), 1170 (s), 1101(vs), 1035(s), 939 (s), 835 (m), 738 (m), 470 (s). Analysis calculated for C44H99FeClNO12Si7: C 47.09, H 8.89, N 1.25%; found: C 46.87, H 9.17, N 1.32%.

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
Fe0.81780 (2)0.067978 (15)0.29531 (3)0.03476 (15)
Cl0.89193 (4)0.01816 (3)0.32439 (6)0.0471 (2)
Si10.80387 (4)0.14999 (3)0.18230 (6)0.0323 (2)
Si20.66048 (5)0.13932 (4)0.09519 (6)0.0411 (3)
Si30.64464 (5)0.19551 (3)0.22278 (6)0.0358 (2)
Si40.65241 (4)0.11514 (3)0.32700 (6)0.0351 (2)
Si50.79642 (4)0.12701 (3)0.42399 (5)0.0313 (2)
Si60.66679 (5)0.05883 (3)0.19917 (6)0.0412 (3)
Si70.78663 (4)0.20513 (3)0.31330 (5)0.0303 (2)
O10.82846 (12)0.10636 (7)0.22764 (15)0.0423 (6)
O20.73251 (12)0.14612 (9)0.10870 (14)0.0484 (7)
O30.64127 (12)0.17641 (9)0.13948 (15)0.0471 (7)
O40.63902 (11)0.15815 (8)0.27761 (15)0.0454 (6)
O50.72278 (11)0.11668 (7)0.40158 (13)0.0379 (6)
O60.82626 (11)0.09050 (8)0.39236 (14)0.0421 (6)
O70.73938 (12)0.04430 (8)0.24068 (17)0.0487 (7)
O80.65606 (12)0.09535 (9)0.13426 (16)0.0530 (7)
O90.79843 (11)0.17079 (8)0.38206 (14)0.0424 (6)
O100.71223 (11)0.21848 (7)0.27195 (14)0.0399 (6)
O110.80275 (11)0.18543 (7)0.24413 (13)0.0383 (6)
O120.64778 (12)0.07694 (8)0.26745 (15)0.0486 (7)
C10.85801 (18)0.17004 (12)0.1427 (2)0.0446 (9)
H1A0.90030.17330.18950.054*
H1B0.86180.14850.10660.054*
C20.8411 (2)0.21106 (14)0.0958 (3)0.0674 (13)
H2A0.81810.22890.11860.081*
C30.7978 (3)0.20295 (18)0.0077 (3)0.0915 (18)
H3A0.78620.22940.02190.137*
H3B0.75950.18890.00290.137*
H3C0.81930.18520.01560.137*
C40.9004 (4)0.2341 (2)0.1058 (4)0.124 (3)
H4A0.88850.26060.07620.186*
H4B0.92360.21700.08370.186*
H4C0.92740.23950.16370.186*
C50.60607 (18)0.14124 (14)0.0145 (2)0.0518 (10)
H5A0.56480.12980.02250.062*
H5B0.59910.17080.03130.062*
C60.6261 (2)0.11837 (16)0.0718 (2)0.0605 (12)
H6A0.66820.12960.06270.073*
C70.5793 (3)0.1271 (2)0.1602 (3)0.0959 (19)
H7A0.57580.15730.16960.144*
H7B0.53770.11580.17110.144*
H7C0.59420.11390.19650.144*
C80.6337 (3)0.07215 (18)0.0543 (3)0.0841 (17)
H8A0.66400.06760.00280.126*
H8B0.64910.05870.08990.126*
H8C0.59270.06010.06440.126*
C90.57889 (17)0.23212 (12)0.2007 (2)0.0451 (9)
H9A0.54310.21610.20050.054*
H9B0.59250.25210.24650.054*
C100.5538 (2)0.25734 (14)0.1216 (3)0.0572 (11)
H10A0.53990.23710.07540.069*
C110.6033 (2)0.28458 (18)0.1172 (3)0.0799 (16)
H11A0.63930.26750.12270.120*
H11B0.61740.30510.16150.120*
H11C0.58570.29910.06470.120*
C120.4957 (2)0.28238 (17)0.1115 (4)0.0902 (18)
H12A0.47960.29820.06050.135*
H12B0.50750.30170.15740.135*
H12C0.46290.26340.11020.135*
C130.59168 (17)0.10727 (12)0.3626 (2)0.0444 (9)
H13A0.55470.09400.31770.053*
H13B0.60870.08700.40800.053*
C140.5681 (2)0.14421 (15)0.3909 (3)0.0680 (13)
H14A0.54570.16170.34100.082*
C150.6155 (3)0.17173 (19)0.4494 (4)0.098 (2)
H15A0.64670.17900.43010.148*
H15B0.63670.15760.50220.148*
H15C0.59500.19720.45540.148*
C160.5172 (2)0.13231 (17)0.4165 (3)0.0738 (14)
H16A0.50310.15730.43450.111*
H16B0.53450.11220.46140.111*
H16C0.48120.11980.37020.111*
C170.84048 (17)0.13345 (11)0.53571 (19)0.0369 (8)
H17A0.84780.10540.56090.044*
H17B0.88240.14540.54820.044*
C180.80981 (18)0.16067 (12)0.5770 (2)0.0450 (9)
H18A0.76580.15020.55950.054*
C190.8054 (2)0.20575 (14)0.5536 (3)0.0696 (13)
H19A0.78160.20840.49430.104*
H19B0.84810.21710.57150.104*
H19C0.78370.22120.57980.104*
C200.8453 (3)0.15651 (17)0.6694 (3)0.0835 (16)
H20A0.82480.17390.69460.125*
H20B0.88910.16560.68810.125*
H20C0.84470.12740.68480.125*
C210.6125 (3)0.01651 (16)0.1409 (3)0.0783 (16)
H21A0.57060.02960.10890.094*
H21B0.62700.00660.10100.094*
C220.6022 (4)0.0185 (2)0.1767 (4)0.119 (2)
H22A0.64320.03130.21580.143*
C230.5601 (4)0.0515 (2)0.1097 (6)0.170 (4)
H23A0.57800.05620.07140.256*
H23B0.51690.04090.08010.256*
H23C0.55950.07790.13630.256*
C240.5615 (6)0.0070 (3)0.2204 (7)0.270 (8)
H24A0.58320.01460.26130.405*
H24B0.55520.03170.24720.405*
H24C0.52040.00360.18050.405*
C250.83946 (18)0.24976 (12)0.3605 (2)0.0434 (9)
H25A0.81800.26870.38280.052*
H25B0.87800.23920.40720.052*
C260.8601 (2)0.27529 (15)0.3070 (3)0.0650 (13)
H26A0.87650.25510.27940.078*
C270.9138 (3)0.3048 (2)0.3554 (4)0.127 (3)
H27A0.92530.32050.31820.191*
H27B0.95050.28880.39350.191*
H27C0.90050.32420.38590.191*
C280.8067 (3)0.2975 (2)0.2419 (4)0.121 (3)
H28A0.77310.27760.21070.182*
H28B0.82130.31110.20550.182*
H28C0.79040.31850.26610.182*
N0.87882 (14)0.02840 (10)0.05273 (17)0.0416 (7)
C290.83980 (19)0.04428 (13)0.0331 (2)0.0540 (11)
H29A0.86890.05050.05720.065*
H29B0.81160.02150.06560.065*
C300.7998 (2)0.08234 (14)0.0425 (3)0.0584 (11)
H30A0.82740.10630.01460.070*
H30B0.77150.07730.01680.070*
C310.7605 (3)0.0925 (2)0.1320 (3)0.096 (2)
H31A0.73090.06910.15730.115*
H31B0.73460.11730.13560.115*
C320.7920 (4)0.1001 (3)0.1787 (4)0.158 (4)
H32A0.76110.10570.23510.236*
H32B0.81720.07560.17730.236*
H32C0.81990.12420.15670.236*
C330.8373 (2)0.01577 (13)0.0925 (3)0.0538 (11)
H33A0.86480.00380.14660.065*
H33B0.81780.04120.10170.065*
C340.7854 (2)0.01497 (14)0.0465 (3)0.0698 (13)
H34A0.80180.03790.02520.084*
H34B0.75050.00110.00010.084*
C350.7602 (3)0.0330 (2)0.1079 (4)0.106 (2)
H35A0.79460.04880.15180.127*
H35B0.74840.00960.13340.127*
C360.7076 (3)0.0592 (2)0.0680 (5)0.133 (3)
H36A0.69290.06910.10710.199*
H36B0.71960.08310.04470.199*
H36C0.67360.04370.02430.199*
C370.91541 (18)0.00811 (11)0.0440 (2)0.0431 (9)
H37A0.88490.02700.00210.052*
H37B0.94430.00250.02240.052*
C380.95395 (17)0.03370 (11)0.1182 (2)0.0391 (8)
H38A0.92580.04790.13720.047*
H38B0.98320.01550.16260.047*
C390.99108 (18)0.06563 (11)0.0968 (2)0.0441 (9)
H39A0.96120.08290.05100.053*
H39B1.01890.05100.07790.053*
C401.0310 (2)0.09383 (14)0.1666 (3)0.0686 (13)
H40A1.05380.11360.14860.103*
H40B1.00370.10910.18470.103*
H40C1.06150.07710.21180.103*
C410.92316 (18)0.06185 (11)0.1074 (2)0.0443 (9)
H41A0.89740.08250.11930.053*
H41B0.95190.04870.15970.053*
C420.96273 (18)0.08474 (13)0.0758 (2)0.0510 (10)
H42A0.93480.09920.02460.061*
H42B0.98900.06460.06360.061*
C431.00501 (19)0.11618 (13)0.1371 (3)0.0511 (10)
H43A1.03760.10120.18440.061*
H43B0.97940.13280.15690.061*
C441.0373 (2)0.14524 (16)0.1026 (3)0.0710 (13)
H44A1.06550.16400.14560.107*
H44B1.00540.16160.05820.107*
H44C1.06200.12890.08180.107*
Atomic displacement parameters (Å2) top
U11U22U33U12U13U23
Fe0.0404 (3)0.0268 (3)0.0408 (3)0.0051 (2)0.0215 (2)0.0007 (2)
Cl0.0503 (6)0.0370 (5)0.0559 (6)0.0144 (4)0.0255 (5)0.0029 (4)
Si10.0329 (5)0.0340 (5)0.0334 (5)0.0024 (4)0.0177 (4)0.0005 (4)
Si20.0329 (5)0.0573 (7)0.0313 (5)0.0032 (5)0.0129 (4)0.0067 (5)
Si30.0329 (5)0.0397 (6)0.0353 (5)0.0074 (4)0.0158 (4)0.0009 (4)
Si40.0346 (5)0.0360 (5)0.0394 (5)0.0036 (4)0.0209 (5)0.0054 (4)
Si50.0336 (5)0.0310 (5)0.0295 (5)0.0025 (4)0.0143 (4)0.0010 (4)
Si60.0388 (6)0.0392 (6)0.0493 (6)0.0096 (4)0.0231 (5)0.0155 (5)
Si70.0330 (5)0.0274 (5)0.0313 (5)0.0004 (4)0.0152 (4)0.0000 (4)
O10.0490 (15)0.0338 (13)0.0490 (14)0.0025 (11)0.0264 (13)0.0052 (11)
O20.0413 (15)0.0696 (19)0.0359 (13)0.0003 (13)0.0188 (12)0.0074 (13)
O30.0405 (15)0.0594 (17)0.0418 (14)0.0062 (12)0.0189 (12)0.0072 (12)
O40.0434 (15)0.0493 (16)0.0469 (14)0.0005 (12)0.0231 (13)0.0009 (12)
O50.0393 (14)0.0417 (14)0.0366 (13)0.0024 (11)0.0206 (11)0.0009 (11)
O60.0450 (15)0.0404 (14)0.0419 (14)0.0051 (11)0.0203 (12)0.0074 (11)
O70.0440 (15)0.0357 (14)0.0667 (17)0.0036 (11)0.0249 (14)0.0115 (13)
O80.0500 (16)0.0601 (18)0.0475 (15)0.0021 (13)0.0206 (13)0.0078 (14)
O90.0452 (15)0.0424 (15)0.0374 (13)0.0030 (12)0.0165 (12)0.0087 (11)
O100.0353 (13)0.0368 (14)0.0459 (14)0.0062 (11)0.0164 (12)0.0011 (11)
O110.0408 (14)0.0394 (14)0.0366 (13)0.0008 (11)0.0190 (12)0.0039 (11)
O120.0494 (16)0.0520 (16)0.0513 (15)0.0094 (12)0.0286 (14)0.0196 (13)
C10.048 (2)0.044 (2)0.056 (2)0.0041 (18)0.036 (2)0.0018 (18)
C20.101 (4)0.053 (3)0.078 (3)0.013 (3)0.067 (3)0.012 (2)
C30.129 (5)0.088 (4)0.072 (3)0.036 (4)0.058 (4)0.033 (3)
C40.182 (7)0.085 (5)0.147 (6)0.051 (5)0.110 (6)0.001 (4)
C50.040 (2)0.073 (3)0.037 (2)0.003 (2)0.0114 (18)0.003 (2)
C60.051 (3)0.092 (4)0.037 (2)0.008 (2)0.019 (2)0.012 (2)
C70.098 (4)0.138 (5)0.037 (3)0.008 (4)0.018 (3)0.019 (3)
C80.078 (4)0.112 (5)0.060 (3)0.013 (3)0.029 (3)0.023 (3)
C90.040 (2)0.048 (2)0.050 (2)0.0128 (17)0.0224 (19)0.0030 (18)
C100.055 (3)0.055 (3)0.056 (3)0.020 (2)0.019 (2)0.007 (2)
C110.086 (4)0.093 (4)0.072 (3)0.018 (3)0.046 (3)0.034 (3)
C120.065 (3)0.084 (4)0.113 (4)0.033 (3)0.032 (3)0.030 (3)
C130.037 (2)0.047 (2)0.055 (2)0.0043 (17)0.0257 (19)0.0004 (19)
C140.065 (3)0.070 (3)0.090 (3)0.008 (2)0.054 (3)0.016 (3)
C150.088 (4)0.106 (5)0.129 (5)0.024 (3)0.074 (4)0.059 (4)
C160.066 (3)0.088 (4)0.091 (4)0.001 (3)0.057 (3)0.004 (3)
C170.042 (2)0.0330 (19)0.0314 (17)0.0044 (15)0.0122 (16)0.0039 (15)
C180.046 (2)0.052 (2)0.0349 (19)0.0018 (18)0.0161 (18)0.0046 (17)
C190.096 (4)0.051 (3)0.070 (3)0.021 (3)0.045 (3)0.001 (2)
C200.112 (4)0.091 (4)0.041 (2)0.010 (3)0.029 (3)0.011 (3)
C210.096 (4)0.067 (3)0.102 (4)0.041 (3)0.071 (3)0.049 (3)
C220.164 (7)0.072 (4)0.127 (6)0.030 (4)0.071 (5)0.016 (4)
C230.190 (8)0.119 (6)0.261 (11)0.109 (6)0.154 (8)0.116 (7)
C240.48 (2)0.186 (10)0.343 (15)0.208 (12)0.364 (16)0.170 (10)
C250.048 (2)0.041 (2)0.043 (2)0.0098 (17)0.0221 (19)0.0089 (17)
C260.079 (3)0.055 (3)0.061 (3)0.022 (2)0.031 (3)0.001 (2)
C270.155 (7)0.136 (6)0.109 (5)0.101 (5)0.076 (5)0.031 (4)
C280.122 (5)0.087 (4)0.139 (6)0.005 (4)0.044 (5)0.065 (4)
N0.0477 (18)0.0421 (18)0.0389 (16)0.0040 (14)0.0229 (15)0.0052 (14)
C290.050 (2)0.060 (3)0.044 (2)0.009 (2)0.015 (2)0.007 (2)
C300.057 (3)0.061 (3)0.055 (2)0.018 (2)0.024 (2)0.007 (2)
C310.102 (4)0.116 (5)0.072 (3)0.054 (4)0.042 (3)0.031 (3)
C320.197 (8)0.190 (9)0.124 (6)0.123 (7)0.106 (6)0.092 (6)
C330.064 (3)0.043 (2)0.071 (3)0.006 (2)0.046 (2)0.005 (2)
C340.071 (3)0.052 (3)0.099 (4)0.000 (2)0.049 (3)0.016 (3)
C350.099 (4)0.098 (4)0.164 (6)0.045 (4)0.097 (5)0.079 (4)
C360.134 (6)0.123 (6)0.181 (7)0.030 (5)0.106 (6)0.069 (6)
C370.051 (2)0.044 (2)0.0393 (19)0.0045 (18)0.0245 (18)0.0055 (17)
C380.042 (2)0.039 (2)0.0404 (19)0.0030 (16)0.0218 (17)0.0062 (16)
C390.047 (2)0.036 (2)0.054 (2)0.0019 (17)0.026 (2)0.0046 (17)
C400.080 (3)0.050 (3)0.083 (3)0.016 (2)0.043 (3)0.006 (2)
C410.055 (2)0.039 (2)0.039 (2)0.0059 (18)0.0210 (19)0.0032 (16)
C420.042 (2)0.062 (3)0.046 (2)0.0056 (19)0.0165 (19)0.003 (2)
C430.046 (2)0.050 (2)0.058 (2)0.0039 (19)0.024 (2)0.003 (2)
C440.052 (3)0.074 (3)0.079 (3)0.002 (2)0.022 (3)0.011 (3)
Geometric parameters (Å, º) top
Fe—O71.832 (2)C18—C201.524 (5)
Fe—O11.846 (2)C18—H18A1.0000
Fe—O61.848 (2)C19—H19A0.9800
Fe—Cl2.2537 (10)C19—H19B0.9800
Si1—O11.600 (2)C19—H19C0.9800
Si1—O111.616 (2)C20—H20A0.9800
Si1—O21.627 (3)C20—H20B0.9800
Si1—C11.848 (4)C20—H20C0.9800
Si2—O81.608 (3)C21—C221.379 (8)
Si2—O31.617 (3)C21—H21A0.9900
Si2—O21.622 (3)C21—H21B0.9900
Si2—C51.842 (4)C22—C241.549 (11)
Si3—O41.609 (3)C22—C231.590 (8)
Si3—O31.616 (3)C22—H22A1.0000
Si3—O101.619 (3)C23—H23A0.9800
Si3—C91.844 (4)C23—H23B0.9800
Si4—O41.604 (3)C23—H23C0.9800
Si4—O51.614 (2)C24—H24A0.9800
Si4—O121.614 (3)C24—H24B0.9800
Si4—C131.842 (4)C24—H24C0.9800
Si5—O61.605 (2)C25—C261.518 (5)
Si5—O91.614 (2)C25—H25A0.9900
Si5—O51.634 (2)C25—H25B0.9900
Si5—C171.849 (3)C26—C281.476 (7)
Si6—O71.604 (3)C26—C271.514 (7)
Si6—O81.609 (3)C26—H26A1.0000
Si6—O121.617 (3)C27—H27A0.9800
Si6—C211.847 (4)C27—H27B0.9800
Si7—O91.604 (2)C27—H27C0.9800
Si7—O111.609 (2)C28—H28A0.9800
Si7—O101.631 (2)C28—H28B0.9800
Si7—C251.843 (4)C28—H28C0.9800
C1—C21.526 (6)N—C371.508 (4)
C1—H1A0.9900N—C291.515 (5)
C1—H1B0.9900N—C331.516 (5)
C2—C31.500 (7)N—C411.523 (5)
C2—C41.523 (7)C29—C301.508 (6)
C2—H2A1.0000C29—H29A0.9900
C3—H3A0.9800C29—H29B0.9900
C3—H3B0.9800C30—C311.517 (6)
C3—H3C0.9800C30—H30A0.9900
C4—H4A0.9800C30—H30B0.9900
C4—H4B0.9800C31—C321.385 (8)
C4—H4C0.9800C31—H31A0.9900
C5—C61.521 (5)C31—H31B0.9900
C5—H5A0.9900C32—H32A0.9800
C5—H5B0.9900C32—H32B0.9800
C6—C81.513 (7)C32—H32C0.9800
C6—C71.526 (6)C33—C341.506 (6)
C6—H6A1.0000C33—H33A0.9900
C7—H7A0.9800C33—H33B0.9900
C7—H7B0.9800C34—C351.600 (8)
C7—H7C0.9800C34—H34A0.9900
C8—H8A0.9800C34—H34B0.9900
C8—H8B0.9800C35—C361.405 (8)
C8—H8C0.9800C35—H35A0.9900
C9—C101.530 (5)C35—H35B0.9900
C9—H9A0.9900C36—H36A0.9800
C9—H9B0.9900C36—H36B0.9800
C10—C111.493 (7)C36—H36C0.9800
C10—C121.528 (6)C37—C381.500 (5)
C10—H10A1.0000C37—H37A0.9900
C11—H11A0.9800C37—H37B0.9900
C11—H11B0.9800C38—C391.512 (5)
C11—H11C0.9800C38—H38A0.9900
C12—H12A0.9800C38—H38B0.9900
C12—H12B0.9800C39—C401.507 (6)
C12—H12C0.9800C39—H39A0.9900
C13—C141.499 (6)C39—H39B0.9900
C13—H13A0.9900C40—H40A0.9800
C13—H13B0.9900C40—H40B0.9800
C14—C151.453 (7)C40—H40C0.9800
C14—C161.525 (6)C41—C421.495 (5)
C14—H14A1.0000C41—H41A0.9900
C15—H15A0.9800C41—H41B0.9900
C15—H15B0.9800C42—C431.509 (5)
C15—H15C0.9800C42—H42A0.9900
C16—H16A0.9800C42—H42B0.9900
C16—H16B0.9800C43—C441.512 (6)
C16—H16C0.9800C43—H43A0.9900
C17—C181.535 (5)C43—H43B0.9900
C17—H17A0.9900C44—H44A0.9800
C17—H17B0.9900C44—H44B0.9800
C18—C191.500 (6)C44—H44C0.9800
O7—Fe—O1108.57 (12)C19—C18—H18A107.7
O7—Fe—O6109.65 (11)C20—C18—H18A107.7
O1—Fe—O6113.50 (11)C17—C18—H18A107.7
O7—Fe—Cl108.93 (8)C18—C19—H19A109.5
O1—Fe—Cl107.91 (8)C18—C19—H19B109.5
O6—Fe—Cl108.19 (8)H19A—C19—H19B109.5
O1—Si1—O11111.60 (13)C18—C19—H19C109.5
O1—Si1—O2111.43 (14)H19A—C19—H19C109.5
O11—Si1—O2107.46 (13)H19B—C19—H19C109.5
O1—Si1—C1110.79 (16)C18—C20—H20A109.5
O11—Si1—C1105.22 (16)C18—C20—H20B109.5
O2—Si1—C1110.11 (16)H20A—C20—H20B109.5
O8—Si2—O3109.49 (14)C18—C20—H20C109.5
O8—Si2—O2108.86 (15)H20A—C20—H20C109.5
O3—Si2—O2109.62 (14)H20B—C20—H20C109.5
O8—Si2—C5111.33 (18)C22—C21—Si6123.4 (5)
O3—Si2—C5107.99 (17)C22—C21—H21A106.5
O2—Si2—C5109.53 (16)Si6—C21—H21A106.5
O4—Si3—O3109.02 (14)C22—C21—H21B106.5
O4—Si3—O10109.17 (13)Si6—C21—H21B106.5
O3—Si3—O10108.59 (14)H21A—C21—H21B106.5
O4—Si3—C9108.39 (16)C21—C22—C24109.5 (7)
O3—Si3—C9110.75 (16)C21—C22—C23111.0 (6)
O10—Si3—C9110.89 (16)C24—C22—C23104.0 (7)
O4—Si4—O5108.70 (13)C21—C22—H22A110.7
O4—Si4—O12109.60 (14)C24—C22—H22A110.7
O5—Si4—O12109.22 (14)C23—C22—H22A110.7
O4—Si4—C13109.31 (16)C22—C23—H23A109.5
O5—Si4—C13112.01 (15)C22—C23—H23B109.5
O12—Si4—C13107.97 (16)H23A—C23—H23B109.5
O6—Si5—O9110.64 (13)C22—C23—H23C109.5
O6—Si5—O5110.61 (13)H23A—C23—H23C109.5
O9—Si5—O5108.20 (13)H23B—C23—H23C109.5
O6—Si5—C17111.21 (14)C22—C24—H24A109.5
O9—Si5—C17108.01 (15)C22—C24—H24B109.5
O5—Si5—C17108.06 (14)H24A—C24—H24B109.5
O7—Si6—O8110.14 (15)C22—C24—H24C109.5
O7—Si6—O12110.24 (14)H24A—C24—H24C109.5
O8—Si6—O12107.78 (15)H24B—C24—H24C109.5
O7—Si6—C21112.3 (2)C26—C25—Si7117.5 (3)
O8—Si6—C21105.6 (2)C26—C25—H25A107.9
O12—Si6—C21110.56 (18)Si7—C25—H25A107.9
O9—Si7—O11109.35 (13)C26—C25—H25B107.9
O9—Si7—O10108.57 (13)Si7—C25—H25B107.9
O11—Si7—O10108.86 (13)H25A—C25—H25B107.2
O9—Si7—C25108.80 (15)C28—C26—C27111.2 (5)
O11—Si7—C25109.06 (15)C28—C26—C25112.3 (4)
O10—Si7—C25112.16 (16)C27—C26—C25112.7 (4)
Si1—O1—Fe143.84 (16)C28—C26—H26A106.7
Si2—O2—Si1139.90 (16)C27—C26—H26A106.7
Si3—O3—Si2148.10 (18)C25—C26—H26A106.7
Si4—O4—Si3160.86 (18)C26—C27—H27A109.5
Si4—O5—Si5142.90 (15)C26—C27—H27B109.5
Si5—O6—Fe139.36 (15)H27A—C27—H27B109.5
Si6—O7—Fe138.14 (16)C26—C27—H27C109.5
Si2—O8—Si6161.81 (19)H27A—C27—H27C109.5
Si7—O9—Si5160.49 (17)H27B—C27—H27C109.5
Si3—O10—Si7136.84 (16)C26—C28—H28A109.5
Si7—O11—Si1156.20 (17)C26—C28—H28B109.5
Si4—O12—Si6147.15 (18)H28A—C28—H28B109.5
C2—C1—Si1118.0 (3)C26—C28—H28C109.5
C2—C1—H1A107.8H28A—C28—H28C109.5
Si1—C1—H1A107.8H28B—C28—H28C109.5
C2—C1—H1B107.8C37—N—C29105.2 (3)
Si1—C1—H1B107.8C37—N—C33111.7 (3)
H1A—C1—H1B107.1C29—N—C33111.5 (3)
C3—C2—C4111.2 (5)C37—N—C41111.1 (3)
C3—C2—C1109.8 (4)C29—N—C41111.5 (3)
C4—C2—C1110.9 (4)C33—N—C41105.9 (3)
C3—C2—H2A108.3C30—C29—N116.8 (3)
C4—C2—H2A108.3C30—C29—H29A108.1
C1—C2—H2A108.3N—C29—H29A108.1
C2—C3—H3A109.5C30—C29—H29B108.1
C2—C3—H3B109.5N—C29—H29B108.1
H3A—C3—H3B109.5H29A—C29—H29B107.3
C2—C3—H3C109.5C29—C30—C31110.3 (4)
H3A—C3—H3C109.5C29—C30—H30A109.6
H3B—C3—H3C109.5C31—C30—H30A109.6
C2—C4—H4A109.5C29—C30—H30B109.6
C2—C4—H4B109.5C31—C30—H30B109.6
H4A—C4—H4B109.5H30A—C30—H30B108.1
C2—C4—H4C109.5C32—C31—C30118.0 (6)
H4A—C4—H4C109.5C32—C31—H31A107.8
H4B—C4—H4C109.5C30—C31—H31A107.8
C6—C5—Si2117.3 (3)C32—C31—H31B107.8
C6—C5—H5A108.0C30—C31—H31B107.8
Si2—C5—H5A108.0H31A—C31—H31B107.1
C6—C5—H5B108.0C31—C32—H32A109.5
Si2—C5—H5B108.0C31—C32—H32B109.5
H5A—C5—H5B107.2H32A—C32—H32B109.5
C8—C6—C5111.8 (4)C31—C32—H32C109.5
C8—C6—C7111.5 (4)H32A—C32—H32C109.5
C5—C6—C7110.1 (4)H32B—C32—H32C109.5
C8—C6—H6A107.8C34—C33—N116.5 (3)
C5—C6—H6A107.8C34—C33—H33A108.2
C7—C6—H6A107.8N—C33—H33A108.2
C6—C7—H7A109.5C34—C33—H33B108.2
C6—C7—H7B109.5N—C33—H33B108.2
H7A—C7—H7B109.5H33A—C33—H33B107.3
C6—C7—H7C109.5C33—C34—C35108.1 (4)
H7A—C7—H7C109.5C33—C34—H34A110.1
H7B—C7—H7C109.5C35—C34—H34A110.1
C6—C8—H8A109.5C33—C34—H34B110.1
C6—C8—H8B109.5C35—C34—H34B110.1
H8A—C8—H8B109.5H34A—C34—H34B108.4
C6—C8—H8C109.5C36—C35—C34111.8 (6)
H8A—C8—H8C109.5C36—C35—H35A109.3
H8B—C8—H8C109.5C34—C35—H35A109.3
C10—C9—Si3118.5 (3)C36—C35—H35B109.3
C10—C9—H9A107.7C34—C35—H35B109.3
Si3—C9—H9A107.7H35A—C35—H35B107.9
C10—C9—H9B107.7C35—C36—H36A109.5
Si3—C9—H9B107.7C35—C36—H36B109.5
H9A—C9—H9B107.1H36A—C36—H36B109.5
C11—C10—C12111.6 (4)C35—C36—H36C109.5
C11—C10—C9112.3 (4)H36A—C36—H36C109.5
C12—C10—C9109.9 (4)H36B—C36—H36C109.5
C11—C10—H10A107.6C38—C37—N118.2 (3)
C12—C10—H10A107.6C38—C37—H37A107.7
C9—C10—H10A107.6N—C37—H37A107.7
C10—C11—H11A109.5C38—C37—H37B107.7
C10—C11—H11B109.5N—C37—H37B107.7
H11A—C11—H11B109.5H37A—C37—H37B107.1
C10—C11—H11C109.5C37—C38—C39108.8 (3)
H11A—C11—H11C109.5C37—C38—H38A109.9
H11B—C11—H11C109.5C39—C38—H38A109.9
C10—C12—H12A109.5C37—C38—H38B109.9
C10—C12—H12B109.5C39—C38—H38B109.9
H12A—C12—H12B109.5H38A—C38—H38B108.3
C10—C12—H12C109.5C40—C39—C38113.7 (3)
H12A—C12—H12C109.5C40—C39—H39A108.8
H12B—C12—H12C109.5C38—C39—H39A108.8
C14—C13—Si4118.9 (3)C40—C39—H39B108.8
C14—C13—H13A107.6C38—C39—H39B108.8
Si4—C13—H13A107.6H39A—C39—H39B107.7
C14—C13—H13B107.6C39—C40—H40A109.5
Si4—C13—H13B107.6C39—C40—H40B109.5
H13A—C13—H13B107.0H40A—C40—H40B109.5
C15—C14—C13117.0 (4)C39—C40—H40C109.5
C15—C14—C16112.3 (4)H40A—C40—H40C109.5
C13—C14—C16112.1 (4)H40B—C40—H40C109.5
C15—C14—H14A104.7C42—C41—N117.2 (3)
C13—C14—H14A104.7C42—C41—H41A108.0
C16—C14—H14A104.7N—C41—H41A108.0
C14—C15—H15A109.5C42—C41—H41B108.0
C14—C15—H15B109.5N—C41—H41B108.0
H15A—C15—H15B109.5H41A—C41—H41B107.2
C14—C15—H15C109.5C41—C42—C43111.2 (3)
H15A—C15—H15C109.5C41—C42—H42A109.4
H15B—C15—H15C109.5C43—C42—H42A109.4
C14—C16—H16A109.5C41—C42—H42B109.4
C14—C16—H16B109.5C43—C42—H42B109.4
H16A—C16—H16B109.5H42A—C42—H42B108.0
C14—C16—H16C109.5C42—C43—C44113.0 (4)
H16A—C16—H16C109.5C42—C43—H43A109.0
H16B—C16—H16C109.5C44—C43—H43A109.0
C18—C17—Si5117.1 (2)C42—C43—H43B109.0
C18—C17—H17A108.0C44—C43—H43B109.0
Si5—C17—H17A108.0H43A—C43—H43B107.8
C18—C17—H17B108.0C43—C44—H44A109.5
Si5—C17—H17B108.0C43—C44—H44B109.5
H17A—C17—H17B107.3H44A—C44—H44B109.5
C19—C18—C20109.6 (4)C43—C44—H44C109.5
C19—C18—C17113.3 (3)H44A—C44—H44C109.5
C20—C18—C17110.7 (3)H44B—C44—H44C109.5
 

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