The entrance and diffusion pathway of CO2 and dimethyl ether (DME) in MFI-type zeolite channels were investigated by a selective sealing method using large silicalite-1 crystals. The MFI-type zeolite has two kinds of orthogonal channels: straight channels and sinusoidal channels. The mouths of the straight channels are on (010) crystal faces, while those of the sinusoidal channels are on (100) faces. The channel mouths are directly sealed by silicone resin on the (100) and (010) faces so as to restrict the entrance and diffusion pathways to straight and sinusoidal channel pathways, respectively. The locations and loadings of the guest CO2 and DME molecules are determined by single-crystal X-ray diffraction structural analysis. The loadings show the difference of the adsorption rates between the pathways. The straight channel pathway is 4.2 times faster than the sinusoidal channel pathway for the CO2, and the sinusoidal channel pathway is 5.1 times faster than the straight channel pathway for the DME. It reveals their dominant pathways and the anisotropy of adsorption. The dominant pathway correlates to the stability of the channel as adsorption sites.
Supporting information
CCDC references: 1042360; 1044716; 1044717; 1044718; 1044719; 1044720; 1044721; 1044722
Data collection: Bruker XSCANS for sin12h3_twin_f_dme, sin24h3_twin_f_dme; Bruker SMART for str12h_twin_f_dme, str24h_twin_f_dme. Cell refinement: Bruker XSCANS for sin12h3_twin_f_dme, sin24h3_twin_f_dme; Bruker SMART for str12h_twin_f_dme, str24h_twin_f_dme. Data reduction: Bruker SHELXTL for sin12h3_twin_f_dme, sin24h3_twin_f_dme; Bruker SAINT for str12h_twin_f_dme, str24h_twin_f_dme. For all compounds, program(s) used to solve structure: SHELXS97 (Sheldrick, 1990); program(s) used to refine structure: SHELXL97 (Sheldrick, 1997). Molecular graphics: Bruker SHELXTL for sin12h3_twin_f_dme, sin24h3_twin_f_dme, str12h_twin_f_dme, str24h_twin_f_dme. Software used to prepare material for publication: Bruker SHELXTL for sin12h3_twin_f_dme, sin24h3_twin_f_dme, str12h_twin_f_dme, str24h_twin_f_dme.
Crystal data top
C0.6O49.2Si24 | F(000) = 2968 |
Mr = 1467.7 | Dx = 1.859 Mg m−3 |
Monoclinic, P21/n | Mo Kα radiation, λ = 0.71073 Å |
a = 13.376 (2) Å | Cell parameters from 138 reflections |
b = 20.111 (3) Å | θ = 2.1–23.3° |
c = 19.878 (3) Å | µ = 0.68 mm−1 |
β = 90.003 (2)° | T = 296 K |
V = 5347.3 (14) Å3 | Coffin shape, colorless |
Z = 4 | 0.15 × 0.10 × 0.08 mm |
Data collection top
CCD area detector diffractometer | 12765 independent reflections |
Radiation source: fine-focus sealed tube | 6435 reflections with I > 2σ(I) |
Graphite monochromator | Rint = 0.175 |
phi and ω scans | θmax = 28.6°, θmin = 1.0° |
Absorption correction: analytical ? | h = −17→17 |
Tmin = 0.904, Tmax = 0.950 | k = −26→26 |
61406 measured reflections | l = −26→26 |
Refinement top
Refinement on F2 | 4 restraints |
Least-squares matrix: full | Primary atom site location: structure-invariant direct methods |
R[F2 > 2σ(F2)] = 0.092 | Secondary atom site location: difference Fourier map |
wR(F2) = 0.186 | w = 1/[σ2(Fo2) + (0.0366P)2 + 44.8067P] where P = (Fo2 + 2Fc2)/3 |
S = 1.01 | (Δ/σ)max = 0.007 |
12765 reflections | Δρmax = 0.89 e Å−3 |
664 parameters | Δρmin = −1.10 e Å−3 |
Crystal data top
C0.6O49.2Si24 | V = 5347.3 (14) Å3 |
Mr = 1467.7 | Z = 4 |
Monoclinic, P21/n | Mo Kα radiation |
a = 13.376 (2) Å | µ = 0.68 mm−1 |
b = 20.111 (3) Å | T = 296 K |
c = 19.878 (3) Å | 0.15 × 0.10 × 0.08 mm |
β = 90.003 (2)° | |
Data collection top
CCD area detector diffractometer | 12765 independent reflections |
Absorption correction: analytical ? | 6435 reflections with I > 2σ(I) |
Tmin = 0.904, Tmax = 0.950 | Rint = 0.175 |
61406 measured reflections | |
Refinement top
R[F2 > 2σ(F2)] = 0.092 | 4 restraints |
wR(F2) = 0.186 | w = 1/[σ2(Fo2) + (0.0366P)2 + 44.8067P] where P = (Fo2 + 2Fc2)/3 |
S = 1.01 | Δρmax = 0.89 e Å−3 |
12765 reflections | Δρmin = −1.10 e Å−3 |
664 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 | x | y | z | Uiso*/Ueq | Occ. (<1) |
C200 | 0.998 (5) | 0.497 (3) | 0.077 (3) | 0.16 (4)* | 0.20 (2) |
O201 | 0.993 (9) | 0.510 (2) | 0.134 (3) | 0.30 (7)* | 0.20 (2) |
O202 | 1.004 (6) | 0.484 (3) | 0.020 (3) | 0.11 (3)* | 0.20 (2) |
C500 | 0.987 (7) | 0.506 (4) | 0.339 (3) | 0.74 (13)* | 0.38 (4) |
O501 | 0.993 (10) | 0.507 (6) | 0.397 (3) | 0.78 (14)* | 0.38 (4) |
O502 | 0.980 (5) | 0.506 (4) | 0.280 (3) | 0.56 (11)* | 0.38 (4) |
Si1 | 0.3222 (2) | 0.42029 (14) | −0.05539 (18) | 0.0112 (6) | |
Si2 | 0.1672 (2) | 0.31317 (16) | −0.03061 (15) | 0.0129 (7) | |
Si3 | −0.0506 (2) | 0.27950 (15) | −0.06253 (17) | 0.0127 (7) | |
Si4 | −0.0357 (2) | 0.12395 (14) | −0.06274 (17) | 0.0106 (6) | |
Si5 | 0.1773 (2) | 0.07651 (15) | −0.02827 (15) | 0.0106 (7) | |
Si6 | 0.3154 (2) | 0.19482 (15) | −0.05580 (17) | 0.0120 (6) | |
Si7 | 0.3202 (3) | 0.42517 (15) | 0.17150 (16) | 0.0121 (7) | |
Si8 | 0.1752 (2) | 0.31140 (16) | 0.12675 (16) | 0.0132 (6) | |
Si9 | −0.0357 (2) | 0.27319 (15) | 0.17580 (15) | 0.0110 (7) | |
Si10 | −0.0330 (2) | 0.11918 (15) | 0.17608 (16) | 0.0113 (7) | |
Si11 | 0.1765 (2) | 0.07132 (15) | 0.12923 (17) | 0.0126 (7) | |
Si12 | 0.3148 (2) | 0.19012 (16) | 0.16597 (15) | 0.0128 (6) | |
Si13 | 0.3352 (2) | 0.42800 (14) | 0.55737 (18) | 0.0113 (6) | |
Si14 | 0.1885 (2) | 0.31193 (16) | 0.52706 (15) | 0.0134 (7) | |
Si15 | −0.0293 (2) | 0.27768 (15) | 0.56105 (17) | 0.0123 (7) | |
Si16 | −0.0330 (2) | 0.12176 (15) | 0.56425 (17) | 0.0118 (7) | |
Si17 | 0.1798 (2) | 0.07073 (15) | 0.52698 (15) | 0.0106 (7) | |
Si18 | 0.3186 (2) | 0.18668 (14) | 0.56232 (16) | 0.0125 (6) | |
Si19 | 0.3155 (2) | 0.42370 (15) | 0.32806 (16) | 0.0124 (7) | |
Si20 | 0.1711 (2) | 0.31223 (16) | 0.36900 (17) | 0.0133 (6) | |
Si21 | −0.0438 (2) | 0.27322 (16) | 0.33109 (16) | 0.0122 (7) | |
Si22 | −0.0372 (2) | 0.11870 (16) | 0.32972 (16) | 0.0123 (7) | |
Si23 | 0.1778 (2) | 0.07214 (14) | 0.36947 (17) | 0.0116 (6) | |
Si24 | 0.3005 (2) | 0.19358 (16) | 0.31969 (14) | 0.0122 (6) | |
O1 | 0.2226 (6) | 0.3766 (4) | −0.0592 (5) | 0.031 (2) | |
O2 | 0.0595 (6) | 0.3097 (4) | −0.0657 (4) | 0.0226 (19) | |
O3 | −0.0450 (7) | 0.2023 (4) | −0.0478 (5) | 0.036 (2) | |
O4 | 0.0783 (6) | 0.1040 (4) | −0.0674 (4) | 0.023 (2) | |
O5 | 0.2716 (6) | 0.1216 (4) | −0.0452 (5) | 0.024 (2) | |
O6 | 0.2280 (6) | 0.2473 (4) | −0.0465 (5) | 0.030 (2) | |
O7 | 0.2290 (7) | 0.3763 (4) | 0.1542 (5) | 0.032 (2) | |
O8 | 0.0718 (6) | 0.3042 (4) | 0.1667 (4) | 0.029 (2) | |
O9 | −0.0308 (7) | 0.1959 (4) | 0.1561 (4) | 0.026 (2) | |
O10 | 0.0768 (7) | 0.0894 (5) | 0.1682 (4) | 0.030 (2) | |
O11 | 0.2645 (7) | 0.1207 (5) | 0.1507 (5) | 0.032 (2) | |
O12 | 0.2433 (6) | 0.2481 (4) | 0.1381 (5) | 0.035 (2) | |
O13 | 0.1539 (7) | 0.3190 (4) | 0.0483 (4) | 0.038 (2) | |
O14 | 0.1553 (6) | 0.0778 (4) | 0.0507 (4) | 0.0258 (19) | |
O15 | 0.3774 (7) | 0.4147 (5) | −0.1249 (4) | 0.033 (2) | |
O16 | 0.3917 (7) | 0.3940 (4) | 0.0053 (4) | 0.033 (2) | |
O17 | 0.4194 (6) | 0.4023 (4) | 0.1333 (4) | 0.022 (2) | |
O18 | 0.3612 (5) | 0.2008 (4) | −0.1294 (4) | 0.0212 (18) | |
O19 | 0.4027 (6) | 0.2089 (4) | −0.0027 (4) | 0.028 (2) | |
O20 | 0.4202 (6) | 0.1948 (4) | 0.1278 (4) | 0.0249 (19) | |
O21 | 0.2036 (6) | 0.0032 (3) | −0.0521 (4) | 0.0212 (19) | |
O22 | 0.2092 (7) | −0.0030 (4) | 0.1472 (4) | 0.025 (2) | |
O23 | 0.3433 (5) | 0.4237 (4) | 0.2507 (5) | 0.0287 (17) | |
O24 | 0.3376 (5) | 0.1977 (4) | 0.2441 (4) | 0.0240 (17) | |
O25 | −0.0663 (5) | 0.2824 (3) | 0.2530 (4) | 0.0180 (15) | |
O26 | −0.0680 (5) | 0.1103 (3) | 0.2521 (5) | 0.0203 (16) | |
O27 | 0.2416 (6) | 0.3789 (4) | 0.5506 (6) | 0.032 (2) | |
O28 | 0.0752 (5) | 0.3138 (4) | 0.5530 (5) | 0.0251 (19) | |
O29 | −0.0117 (6) | 0.1991 (4) | 0.5673 (4) | 0.032 (2) | |
O30 | 0.0685 (5) | 0.0821 (4) | 0.5538 (5) | 0.029 (2) | |
O31 | 0.2546 (6) | 0.1201 (4) | 0.5652 (4) | 0.023 (2) | |
O32 | 0.2444 (6) | 0.2493 (4) | 0.5609 (5) | 0.030 (2) | |
O33 | 0.2202 (7) | 0.3789 (4) | 0.3412 (5) | 0.030 (2) | |
O34 | 0.0537 (6) | 0.3144 (4) | 0.3546 (4) | 0.0211 (19) | |
O35 | −0.0261 (7) | 0.1959 (4) | 0.3478 (4) | 0.023 (2) | |
O36 | 0.0671 (7) | 0.0835 (5) | 0.3431 (5) | 0.037 (3) | |
O37 | 0.2530 (7) | 0.1221 (4) | 0.3327 (4) | 0.027 (2) | |
O38 | 0.2173 (6) | 0.2490 (4) | 0.3316 (4) | 0.029 (2) | |
O39 | 0.1929 (6) | 0.3046 (5) | 0.4472 (5) | 0.043 (2) | |
O40 | 0.1834 (7) | 0.0853 (4) | 0.4482 (5) | 0.030 (2) | |
O41 | 0.3902 (7) | 0.4189 (4) | 0.6280 (5) | 0.030 (2) | |
O42 | 0.4132 (6) | 0.4152 (4) | 0.4981 (4) | 0.024 (2) | |
O43 | 0.4099 (6) | 0.3944 (4) | 0.3683 (4) | 0.024 (2) | |
O44 | 0.3853 (6) | 0.1896 (4) | 0.6295 (4) | 0.0224 (18) | |
O45 | 0.3887 (6) | 0.1858 (4) | 0.4975 (4) | 0.028 (2) | |
O46 | −0.1057 (6) | 0.2938 (5) | −0.1316 (4) | 0.036 (2) | |
O47 | 0.2090 (6) | −0.0053 (4) | 0.5433 (4) | 0.020 (2) | |
O48 | 0.2114 (7) | −0.0015 (4) | 0.3522 (5) | 0.028 (2) | |
Atomic displacement parameters (Å2) top | U11 | U22 | U33 | U12 | U13 | U23 |
Si1 | 0.0156 (15) | 0.0086 (13) | 0.0095 (14) | 0.0001 (12) | 0.0013 (15) | 0.0001 (13) |
Si2 | 0.0175 (16) | 0.0077 (15) | 0.0136 (14) | −0.0013 (13) | −0.0010 (12) | 0.0021 (12) |
Si3 | 0.0162 (16) | 0.0104 (14) | 0.0114 (16) | −0.0007 (12) | 0.0022 (13) | −0.0023 (12) |
Si4 | 0.0129 (15) | 0.0084 (15) | 0.0104 (16) | −0.0006 (12) | 0.0015 (14) | 0.0005 (13) |
Si5 | 0.0111 (15) | 0.0096 (15) | 0.0110 (15) | 0.0001 (13) | 0.0018 (13) | 0.0012 (12) |
Si6 | 0.0152 (15) | 0.0076 (13) | 0.0132 (14) | −0.0040 (13) | 0.0053 (14) | −0.0014 (14) |
Si7 | 0.0199 (17) | 0.0088 (15) | 0.0077 (16) | −0.0022 (13) | 0.0040 (15) | −0.0003 (12) |
Si8 | 0.0130 (15) | 0.0125 (15) | 0.0143 (15) | −0.0014 (14) | 0.0010 (14) | 0.0011 (15) |
Si9 | 0.0157 (16) | 0.0106 (15) | 0.0069 (16) | −0.0007 (12) | 0.0023 (13) | 0.0027 (12) |
Si10 | 0.0178 (17) | 0.0082 (15) | 0.0080 (16) | −0.0024 (13) | 0.0040 (14) | −0.0040 (12) |
Si11 | 0.0186 (17) | 0.0090 (15) | 0.0103 (15) | 0.0003 (13) | 0.0027 (15) | 0.0004 (13) |
Si12 | 0.0179 (15) | 0.0119 (14) | 0.0086 (14) | −0.0007 (14) | 0.0014 (12) | −0.0009 (13) |
Si13 | 0.0158 (16) | 0.0072 (13) | 0.0110 (14) | 0.0001 (12) | 0.0010 (14) | 0.0009 (13) |
Si14 | 0.0170 (16) | 0.0102 (15) | 0.0132 (14) | −0.0006 (14) | 0.0039 (12) | 0.0021 (13) |
Si15 | 0.0169 (16) | 0.0096 (14) | 0.0105 (16) | 0.0015 (11) | 0.0039 (14) | 0.0015 (13) |
Si16 | 0.0126 (15) | 0.0118 (16) | 0.0112 (17) | 0.0033 (12) | 0.0017 (14) | 0.0004 (13) |
Si17 | 0.0141 (16) | 0.0050 (15) | 0.0127 (16) | −0.0011 (12) | 0.0017 (13) | 0.0016 (12) |
Si18 | 0.0176 (15) | 0.0090 (14) | 0.0110 (15) | −0.0035 (13) | 0.0002 (13) | 0.0011 (13) |
Si19 | 0.0141 (16) | 0.0111 (16) | 0.0121 (17) | −0.0007 (13) | 0.0014 (15) | 0.0014 (12) |
Si20 | 0.0132 (15) | 0.0127 (15) | 0.0142 (15) | −0.0024 (13) | 0.0007 (14) | 0.0021 (15) |
Si21 | 0.0157 (16) | 0.0105 (16) | 0.0105 (16) | 0.0002 (12) | 0.0020 (14) | −0.0009 (12) |
Si22 | 0.0165 (16) | 0.0107 (16) | 0.0098 (16) | 0.0008 (13) | 0.0015 (14) | −0.0004 (13) |
Si23 | 0.0186 (16) | 0.0051 (14) | 0.0112 (15) | 0.0006 (13) | 0.0017 (15) | 0.0024 (13) |
Si24 | 0.0160 (15) | 0.0093 (14) | 0.0113 (14) | 0.0000 (14) | 0.0025 (12) | −0.0005 (13) |
O1 | 0.029 (5) | 0.011 (4) | 0.052 (6) | −0.005 (4) | −0.009 (5) | 0.006 (5) |
O2 | 0.022 (4) | 0.023 (4) | 0.023 (4) | −0.006 (4) | 0.008 (3) | 0.014 (4) |
O3 | 0.050 (5) | 0.013 (4) | 0.046 (5) | 0.002 (4) | 0.003 (5) | −0.002 (4) |
O4 | 0.022 (4) | 0.030 (5) | 0.018 (5) | 0.005 (4) | 0.004 (4) | 0.009 (4) |
O5 | 0.017 (4) | 0.011 (4) | 0.044 (6) | −0.002 (3) | 0.014 (4) | 0.002 (4) |
O6 | 0.031 (5) | 0.013 (4) | 0.047 (6) | 0.002 (4) | 0.008 (5) | −0.010 (4) |
O7 | 0.038 (6) | 0.014 (5) | 0.043 (6) | −0.018 (4) | 0.005 (5) | −0.007 (4) |
O8 | 0.019 (4) | 0.042 (5) | 0.025 (4) | −0.011 (4) | 0.012 (4) | −0.003 (4) |
O9 | 0.049 (6) | 0.015 (4) | 0.015 (4) | 0.000 (4) | 0.007 (4) | −0.001 (4) |
O10 | 0.024 (5) | 0.040 (6) | 0.026 (5) | 0.012 (4) | 0.011 (4) | 0.014 (4) |
O11 | 0.034 (5) | 0.023 (5) | 0.039 (6) | −0.008 (4) | −0.009 (4) | −0.008 (4) |
O12 | 0.028 (5) | 0.029 (5) | 0.047 (6) | 0.016 (4) | 0.000 (5) | 0.005 (5) |
O13 | 0.052 (6) | 0.050 (6) | 0.012 (4) | 0.009 (5) | −0.003 (4) | −0.003 (4) |
O14 | 0.030 (5) | 0.032 (5) | 0.016 (4) | −0.001 (4) | 0.000 (4) | −0.003 (4) |
O15 | 0.045 (6) | 0.039 (6) | 0.015 (5) | 0.012 (5) | 0.017 (5) | −0.004 (4) |
O16 | 0.034 (5) | 0.042 (6) | 0.024 (5) | 0.012 (4) | −0.013 (4) | 0.006 (4) |
O17 | 0.015 (4) | 0.037 (5) | 0.015 (4) | 0.003 (4) | 0.009 (4) | −0.003 (4) |
O18 | 0.011 (4) | 0.037 (5) | 0.015 (4) | −0.003 (4) | 0.005 (3) | −0.005 (4) |
O19 | 0.021 (4) | 0.044 (6) | 0.020 (4) | −0.008 (4) | −0.002 (4) | −0.003 (4) |
O20 | 0.024 (4) | 0.031 (5) | 0.020 (4) | 0.006 (4) | 0.010 (4) | 0.006 (4) |
O21 | 0.029 (5) | 0.006 (3) | 0.029 (5) | −0.001 (3) | 0.005 (4) | −0.003 (4) |
O22 | 0.025 (5) | 0.019 (5) | 0.029 (5) | −0.001 (4) | 0.000 (4) | −0.001 (4) |
O23 | 0.035 (4) | 0.042 (4) | 0.009 (3) | 0.005 (4) | 0.002 (5) | 0.003 (5) |
O24 | 0.033 (4) | 0.030 (4) | 0.008 (4) | −0.012 (4) | 0.012 (4) | −0.001 (4) |
O25 | 0.020 (4) | 0.021 (3) | 0.013 (3) | 0.001 (3) | 0.003 (4) | 0.005 (4) |
O26 | 0.019 (4) | 0.028 (4) | 0.014 (3) | −0.006 (3) | 0.006 (4) | −0.004 (4) |
O27 | 0.017 (4) | 0.019 (4) | 0.058 (6) | −0.011 (3) | −0.006 (5) | −0.004 (5) |
O28 | 0.016 (4) | 0.017 (4) | 0.043 (5) | 0.000 (3) | 0.009 (4) | 0.002 (4) |
O29 | 0.051 (6) | 0.012 (4) | 0.033 (5) | −0.003 (4) | −0.003 (4) | 0.005 (4) |
O30 | 0.011 (4) | 0.021 (4) | 0.054 (6) | 0.010 (3) | 0.011 (4) | −0.004 (5) |
O31 | 0.035 (5) | 0.018 (4) | 0.016 (4) | −0.011 (4) | −0.005 (4) | 0.009 (4) |
O32 | 0.037 (5) | 0.020 (4) | 0.032 (5) | 0.011 (4) | 0.000 (5) | 0.009 (4) |
O33 | 0.024 (5) | 0.011 (4) | 0.055 (7) | −0.010 (4) | 0.012 (4) | 0.005 (4) |
O34 | 0.024 (4) | 0.009 (4) | 0.030 (5) | 0.004 (3) | −0.002 (3) | −0.010 (3) |
O35 | 0.036 (5) | 0.007 (4) | 0.025 (4) | −0.004 (4) | 0.000 (4) | 0.002 (4) |
O36 | 0.030 (5) | 0.036 (6) | 0.044 (6) | 0.021 (5) | −0.019 (5) | −0.008 (5) |
O37 | 0.042 (6) | 0.014 (4) | 0.024 (5) | −0.010 (4) | 0.017 (4) | 0.003 (4) |
O38 | 0.031 (5) | 0.016 (4) | 0.039 (5) | 0.011 (4) | 0.006 (4) | −0.006 (4) |
O39 | 0.041 (5) | 0.066 (6) | 0.021 (4) | 0.002 (5) | 0.010 (5) | 0.001 (5) |
O40 | 0.052 (6) | 0.018 (4) | 0.020 (4) | −0.006 (4) | 0.001 (5) | 0.002 (4) |
O41 | 0.040 (5) | 0.025 (5) | 0.023 (5) | 0.022 (4) | −0.014 (5) | −0.003 (4) |
O42 | 0.028 (5) | 0.021 (5) | 0.023 (4) | 0.006 (4) | 0.011 (4) | 0.000 (4) |
O43 | 0.020 (4) | 0.035 (5) | 0.018 (4) | 0.008 (4) | −0.003 (4) | 0.000 (4) |
O44 | 0.025 (4) | 0.021 (4) | 0.022 (4) | −0.005 (4) | −0.015 (4) | −0.001 (4) |
O45 | 0.039 (5) | 0.021 (5) | 0.023 (4) | −0.001 (4) | 0.016 (4) | 0.006 (4) |
O46 | 0.026 (5) | 0.063 (7) | 0.018 (4) | 0.000 (5) | −0.015 (4) | 0.003 (5) |
O47 | 0.009 (4) | 0.014 (4) | 0.035 (5) | −0.003 (3) | 0.009 (4) | 0.008 (4) |
O48 | 0.030 (5) | 0.007 (4) | 0.046 (6) | 0.001 (4) | −0.002 (5) | −0.008 (4) |
Geometric parameters (Å, º) top
C200—O202 | 1.1601 | Si14—O28 | 1.599 (8) |
C200—O201 | 1.1601 | Si14—O32 | 1.607 (9) |
O202—O202i | 1.00 (11) | Si15—O19iv | 1.577 (9) |
C500—O502 | 1.1604 | Si15—O28 | 1.580 (8) |
C500—O501 | 1.1604 | Si15—O20iv | 1.585 (9) |
Si1—O15 | 1.567 (9) | Si15—O29 | 1.601 (9) |
Si1—O47ii | 1.569 (8) | Si16—O16iv | 1.572 (9) |
Si1—O1 | 1.594 (8) | Si16—O29 | 1.579 (9) |
Si1—O16 | 1.606 (9) | Si16—O30 | 1.585 (8) |
Si2—O1 | 1.579 (9) | Si16—O17iv | 1.585 (9) |
Si2—O13 | 1.579 (9) | Si17—O40 | 1.590 (10) |
Si2—O6 | 1.583 (9) | Si17—O30 | 1.594 (8) |
Si2—O2 | 1.597 (8) | Si17—O31 | 1.596 (8) |
Si3—O46 | 1.579 (9) | Si17—O47 | 1.609 (8) |
Si3—O3 | 1.580 (8) | Si18—O31 | 1.588 (8) |
Si3—O2 | 1.590 (8) | Si18—O45 | 1.590 (9) |
Si3—O45iii | 1.601 (8) | Si18—O44 | 1.601 (9) |
Si4—O4 | 1.576 (9) | Si18—O32 | 1.601 (9) |
Si4—O43iii | 1.589 (9) | Si19—O23 | 1.579 (10) |
Si4—O42iii | 1.594 (9) | Si19—O33 | 1.580 (9) |
Si4—O3 | 1.605 (8) | Si19—O22ii | 1.585 (9) |
Si5—O21 | 1.586 (8) | Si19—O43 | 1.601 (9) |
Si5—O5 | 1.587 (8) | Si20—O39 | 1.584 (10) |
Si5—O14 | 1.593 (10) | Si20—O33 | 1.589 (9) |
Si5—O4 | 1.626 (8) | Si20—O34 | 1.591 (9) |
Si6—O6 | 1.583 (9) | Si20—O38 | 1.595 (8) |
Si6—O18 | 1.586 (9) | Si21—O18iv | 1.580 (8) |
Si6—O19 | 1.593 (9) | Si21—O25 | 1.587 (9) |
Si6—O5 | 1.596 (8) | Si21—O35 | 1.604 (9) |
Si7—O17 | 1.593 (8) | Si21—O34 | 1.610 (8) |
Si7—O23 | 1.599 (10) | Si22—O36 | 1.582 (9) |
Si7—O7 | 1.600 (9) | Si22—O35 | 1.599 (9) |
Si7—O48ii | 1.602 (9) | Si22—O26 | 1.600 (10) |
Si8—O12 | 1.578 (9) | Si22—O15iv | 1.601 (9) |
Si8—O7 | 1.583 (9) | Si23—O48 | 1.582 (9) |
Si8—O13 | 1.587 (9) | Si23—O36 | 1.583 (10) |
Si8—O8 | 1.600 (8) | Si23—O40 | 1.584 (10) |
Si9—O8 | 1.574 (8) | Si23—O37 | 1.595 (9) |
Si9—O44iii | 1.583 (8) | Si24—O24 | 1.580 (9) |
Si9—O25 | 1.595 (9) | Si24—O38 | 1.590 (8) |
Si9—O9 | 1.602 (9) | Si24—O37 | 1.591 (9) |
Si10—O26 | 1.589 (10) | Si24—O46v | 1.600 (9) |
Si10—O10 | 1.591 (9) | O15—Si22vi | 1.601 (9) |
Si10—O9 | 1.591 (9) | O16—Si16vi | 1.572 (9) |
Si10—O41iii | 1.593 (9) | O17—Si16vi | 1.585 (9) |
Si11—O10 | 1.581 (9) | O18—Si21vi | 1.580 (8) |
Si11—O14 | 1.587 (10) | O19—Si15vi | 1.577 (9) |
Si11—O11 | 1.594 (9) | O20—Si15vi | 1.585 (9) |
Si11—O22 | 1.596 (9) | O21—Si13vii | 1.599 (8) |
Si12—O11 | 1.576 (9) | O22—Si19vii | 1.585 (9) |
Si12—O24 | 1.585 (9) | O41—Si10v | 1.593 (9) |
Si12—O20 | 1.601 (8) | O42—Si4v | 1.594 (9) |
Si12—O12 | 1.602 (9) | O43—Si4v | 1.590 (9) |
Si13—O41 | 1.590 (10) | O44—Si9v | 1.583 (8) |
Si13—O42 | 1.592 (9) | O45—Si3v | 1.601 (8) |
Si13—O27 | 1.596 (8) | O46—Si24iii | 1.600 (9) |
Si13—O21ii | 1.599 (8) | O47—Si1vii | 1.570 (8) |
Si14—O27 | 1.590 (9) | O48—Si7vii | 1.602 (9) |
Si14—O39 | 1.590 (10) | | |
| | | |
O202—C200—O201 | 180.00 (9) | O30—Si16—O17iv | 107.7 (5) |
O202i—O202—C200 | 128 (10) | O40—Si17—O30 | 109.4 (5) |
O502—C500—O501 | 180 (10) | O40—Si17—O31 | 109.3 (5) |
O15—Si1—O47ii | 109.2 (5) | O30—Si17—O31 | 109.6 (5) |
O15—Si1—O1 | 108.2 (6) | O40—Si17—O47 | 111.3 (5) |
O47ii—Si1—O1 | 108.0 (4) | O30—Si17—O47 | 107.1 (4) |
O15—Si1—O16 | 111.3 (5) | O31—Si17—O47 | 110.1 (5) |
O47ii—Si1—O16 | 110.5 (5) | O31—Si18—O45 | 109.6 (5) |
O1—Si1—O16 | 109.6 (5) | O31—Si18—O44 | 107.4 (5) |
O1—Si2—O13 | 110.5 (5) | O45—Si18—O44 | 110.2 (5) |
O1—Si2—O6 | 111.3 (5) | O31—Si18—O32 | 109.2 (5) |
O13—Si2—O6 | 108.5 (5) | O45—Si18—O32 | 111.0 (5) |
O1—Si2—O2 | 107.5 (5) | O44—Si18—O32 | 109.2 (5) |
O13—Si2—O2 | 109.4 (5) | O23—Si19—O33 | 110.6 (5) |
O6—Si2—O2 | 109.7 (5) | O23—Si19—O22ii | 110.4 (4) |
O46—Si3—O3 | 111.1 (5) | O33—Si19—O22ii | 108.1 (5) |
O46—Si3—O2 | 108.9 (5) | O23—Si19—O43 | 107.3 (5) |
O3—Si3—O2 | 109.8 (5) | O33—Si19—O43 | 109.9 (5) |
O46—Si3—O45iii | 109.2 (5) | O22ii—Si19—O43 | 110.5 (5) |
O3—Si3—O45iii | 108.3 (5) | O39—Si20—O33 | 110.2 (5) |
O2—Si3—O45iii | 109.4 (5) | O39—Si20—O34 | 110.9 (5) |
O4—Si4—O43iii | 109.2 (5) | O33—Si20—O34 | 108.7 (5) |
O4—Si4—O42iii | 109.4 (5) | O39—Si20—O38 | 107.9 (5) |
O43iii—Si4—O42iii | 109.9 (5) | O33—Si20—O38 | 110.4 (5) |
O4—Si4—O3 | 109.6 (5) | O34—Si20—O38 | 108.6 (4) |
O43iii—Si4—O3 | 110.6 (5) | O18iv—Si21—O25 | 107.2 (4) |
O42iii—Si4—O3 | 108.1 (5) | O18iv—Si21—O35 | 109.6 (5) |
O21—Si5—O5 | 106.9 (4) | O25—Si21—O35 | 110.0 (4) |
O21—Si5—O14 | 110.5 (5) | O18iv—Si21—O34 | 109.6 (4) |
O5—Si5—O14 | 110.2 (5) | O25—Si21—O34 | 111.9 (4) |
O21—Si5—O4 | 110.6 (5) | O35—Si21—O34 | 108.5 (5) |
O5—Si5—O4 | 110.4 (4) | O36—Si22—O35 | 108.4 (5) |
O14—Si5—O4 | 108.2 (4) | O36—Si22—O26 | 109.8 (5) |
O6—Si6—O18 | 110.0 (5) | O35—Si22—O26 | 110.0 (4) |
O6—Si6—O19 | 110.0 (5) | O36—Si22—O15iv | 110.2 (5) |
O18—Si6—O19 | 108.1 (5) | O35—Si22—O15iv | 110.3 (5) |
O6—Si6—O5 | 109.2 (5) | O26—Si22—O15iv | 108.3 (5) |
O18—Si6—O5 | 109.4 (5) | O48—Si23—O36 | 109.1 (5) |
O19—Si6—O5 | 110.1 (5) | O48—Si23—O40 | 110.9 (5) |
O17—Si7—O23 | 107.6 (4) | O36—Si23—O40 | 110.1 (5) |
O17—Si7—O7 | 110.7 (5) | O48—Si23—O37 | 108.1 (5) |
O23—Si7—O7 | 110.1 (5) | O36—Si23—O37 | 110.3 (5) |
O17—Si7—O48ii | 110.1 (5) | O40—Si23—O37 | 108.4 (5) |
O23—Si7—O48ii | 110.7 (5) | O24—Si24—O38 | 108.9 (5) |
O7—Si7—O48ii | 107.6 (5) | O24—Si24—O37 | 109.1 (4) |
O12—Si8—O7 | 110.7 (5) | O38—Si24—O37 | 109.2 (5) |
O12—Si8—O13 | 108.6 (5) | O24—Si24—O46v | 108.5 (5) |
O7—Si8—O13 | 109.8 (5) | O38—Si24—O46v | 110.2 (5) |
O12—Si8—O8 | 110.7 (5) | O37—Si24—O46v | 110.9 (5) |
O7—Si8—O8 | 107.1 (5) | Si2—O1—Si1 | 144.9 (6) |
O13—Si8—O8 | 109.9 (5) | Si3—O2—Si2 | 146.0 (5) |
O8—Si9—O44iii | 110.6 (5) | Si3—O3—Si4 | 158.6 (7) |
O8—Si9—O25 | 107.4 (4) | Si4—O4—Si5 | 147.2 (5) |
O44iii—Si9—O25 | 109.3 (4) | Si5—O5—Si6 | 147.6 (6) |
O8—Si9—O9 | 108.5 (5) | Si2—O6—Si6 | 163.2 (6) |
O44iii—Si9—O9 | 110.1 (5) | Si8—O7—Si7 | 157.2 (7) |
O25—Si9—O9 | 110.9 (4) | Si9—O8—Si8 | 151.6 (6) |
O26—Si10—O10 | 108.8 (4) | Si10—O9—Si9 | 151.2 (5) |
O26—Si10—O9 | 110.6 (4) | Si11—O10—Si10 | 155.5 (6) |
O10—Si10—O9 | 108.7 (5) | Si12—O11—Si11 | 156.1 (7) |
O26—Si10—O41iii | 108.9 (5) | Si8—O12—Si12 | 167.5 (7) |
O10—Si10—O41iii | 110.6 (5) | Si2—O13—Si8 | 160.5 (6) |
O9—Si10—O41iii | 109.1 (5) | Si11—O14—Si5 | 158.3 (6) |
O10—Si11—O14 | 108.2 (5) | Si1—O15—Si22vi | 149.3 (7) |
O10—Si11—O11 | 110.3 (5) | Si16vi—O16—Si1 | 171.9 (7) |
O14—Si11—O11 | 109.9 (5) | Si16vi—O17—Si7 | 146.4 (6) |
O10—Si11—O22 | 109.6 (5) | Si21vi—O18—Si6 | 142.3 (6) |
O14—Si11—O22 | 110.2 (5) | Si15vi—O19—Si6 | 167.9 (6) |
O11—Si11—O22 | 108.7 (5) | Si15vi—O20—Si12 | 142.2 (6) |
O11—Si12—O24 | 110.7 (5) | Si5—O21—Si13vii | 145.5 (6) |
O11—Si12—O20 | 109.5 (5) | Si19vii—O22—Si11 | 151.7 (6) |
O24—Si12—O20 | 106.8 (4) | Si19—O23—Si7 | 155.2 (5) |
O11—Si12—O12 | 108.9 (5) | Si24—O24—Si12 | 149.4 (5) |
O24—Si12—O12 | 112.3 (5) | Si21—O25—Si9 | 150.9 (5) |
O20—Si12—O12 | 108.5 (5) | Si10—O26—Si22 | 145.6 (5) |
O41—Si13—O42 | 109.2 (5) | Si14—O27—Si13 | 153.6 (7) |
O41—Si13—O27 | 111.3 (6) | Si15—O28—Si14 | 148.9 (6) |
O42—Si13—O27 | 110.5 (5) | Si16—O29—Si15 | 160.1 (6) |
O41—Si13—O21ii | 108.3 (5) | Si16—O30—Si17 | 155.7 (6) |
O42—Si13—O21ii | 108.4 (5) | Si18—O31—Si17 | 147.3 (6) |
O27—Si13—O21ii | 109.0 (5) | Si18—O32—Si14 | 155.3 (7) |
O27—Si14—O39 | 110.7 (6) | Si19—O33—Si20 | 150.4 (7) |
O27—Si14—O28 | 107.9 (5) | Si20—O34—Si21 | 146.3 (5) |
O39—Si14—O28 | 111.1 (5) | Si22—O35—Si21 | 151.4 (6) |
O27—Si14—O32 | 109.4 (5) | Si22—O36—Si23 | 160.0 (7) |
O39—Si14—O32 | 108.9 (5) | Si24—O37—Si23 | 153.2 (6) |
O28—Si14—O32 | 108.8 (5) | Si24—O38—Si20 | 153.8 (6) |
O19iv—Si15—O28 | 110.3 (5) | Si20—O39—Si14 | 163.3 (7) |
O19iv—Si15—O20iv | 111.4 (5) | Si23—O40—Si17 | 159.3 (5) |
O28—Si15—O20iv | 107.4 (5) | Si13—O41—Si10v | 151.3 (6) |
O19iv—Si15—O29 | 108.3 (5) | Si13—O42—Si4v | 156.8 (6) |
O28—Si15—O29 | 109.4 (5) | Si4v—O43—Si19 | 150.5 (6) |
O20iv—Si15—O29 | 110.0 (5) | Si9v—O44—Si18 | 150.2 (6) |
O16iv—Si16—O29 | 110.0 (5) | Si18—O45—Si3v | 153.4 (6) |
O16iv—Si16—O30 | 110.2 (5) | Si3—O46—Si24iii | 156.1 (7) |
O29—Si16—O30 | 110.2 (5) | Si1vii—O47—Si17 | 150.4 (6) |
O16iv—Si16—O17iv | 108.9 (5) | Si23—O48—Si7vii | 148.0 (7) |
O29—Si16—O17iv | 109.8 (5) | | |
Symmetry codes: (i) −x+2, −y+1, −z; (ii) −x+1/2, y+1/2, −z+1/2; (iii) x−1/2, −y+1/2, z−1/2; (iv) x−1/2, −y+1/2, z+1/2; (v) x+1/2, −y+1/2, z+1/2; (vi) x+1/2, −y+1/2, z−1/2; (vii) −x+1/2, y−1/2, −z+1/2. |
Crystal data top
C0.14O48.27Si24 | F(000) = 2968 |
Mr = 1448.2 | Dx = 1.867 Mg m−3 |
Monoclinic, P21/n | Mo Kα radiation, λ = 0.71073 Å |
a = 13.383 (3) Å | Cell parameters from 293 reflections |
b = 20.118 (4) Å | θ = 2.9–22.2° |
c = 19.887 (4) Å | µ = 0.69 mm−1 |
β = 90.049 (3)° | T = 296 K |
V = 5354.4 (19) Å3 | Coffin shape, colorless |
Z = 4 | 0.17 × 0.09 × 0.07 mm |
Data collection top
CCD area detector diffractometer | 12808 independent reflections |
Radiation source: fine-focus sealed tube | 6047 reflections with I > 2σ(I) |
Graphite monochromator | Rint = 0.123 |
phi and ω scans | θmax = 28.7°, θmin = 1.0° |
Absorption correction: analytical ? | h = −17→17 |
Tmin = 0.893, Tmax = 0.954 | k = −26→26 |
61320 measured reflections | l = −25→26 |
Refinement top
Refinement on F2 | 2 restraints |
Least-squares matrix: full | Primary atom site location: structure-invariant direct methods |
R[F2 > 2σ(F2)] = 0.058 | Secondary atom site location: difference Fourier map |
wR(F2) = 0.159 | w = 1/[σ2(Fo2) + (0.0652P)2] where P = (Fo2 + 2Fc2)/3 |
S = 0.92 | (Δ/σ)max = 0.001 |
12808 reflections | Δρmax = 0.89 e Å−3 |
660 parameters | Δρmin = −0.84 e Å−3 |
Crystal data top
C0.14O48.27Si24 | V = 5354.4 (19) Å3 |
Mr = 1448.2 | Z = 4 |
Monoclinic, P21/n | Mo Kα radiation |
a = 13.383 (3) Å | µ = 0.69 mm−1 |
b = 20.118 (4) Å | T = 296 K |
c = 19.887 (4) Å | 0.17 × 0.09 × 0.07 mm |
β = 90.049 (3)° | |
Data collection top
CCD area detector diffractometer | 12808 independent reflections |
Absorption correction: analytical ? | 6047 reflections with I > 2σ(I) |
Tmin = 0.893, Tmax = 0.954 | Rint = 0.123 |
61320 measured reflections | |
Refinement top
R[F2 > 2σ(F2)] = 0.058 | 660 parameters |
wR(F2) = 0.159 | 2 restraints |
S = 0.92 | Δρmax = 0.89 e Å−3 |
12808 reflections | Δρmin = −0.84 e Å−3 |
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 | x | y | z | Uiso*/Ueq | Occ. (<1) |
C200 | 0.508 (3) | 0.001 (2) | 0.913 (2) | 0.10 (3)* | 0.137 (11) |
O201 | 0.510 (5) | −0.015 (3) | 0.857 (3) | 0.13 (3)* | 0.137 (11) |
O202 | 0.507 (4) | 0.017 (3) | 0.970 (2) | 0.08 (2)* | 0.137 (11) |
Si1 | 0.32260 (17) | 0.42062 (10) | −0.05549 (12) | 0.0144 (5) | |
Si2 | 0.16793 (18) | 0.31273 (11) | −0.03037 (10) | 0.0173 (5) | |
Si3 | −0.04946 (18) | 0.27950 (11) | −0.06247 (12) | 0.0169 (5) | |
Si4 | −0.03547 (17) | 0.12367 (10) | −0.06279 (11) | 0.0155 (5) | |
Si5 | 0.17725 (18) | 0.07612 (10) | −0.02815 (10) | 0.0141 (5) | |
Si6 | 0.31572 (16) | 0.19430 (10) | −0.05575 (12) | 0.0151 (4) | |
Si7 | 0.32035 (18) | 0.42517 (10) | 0.17154 (11) | 0.0147 (5) | |
Si8 | 0.17564 (17) | 0.31122 (11) | 0.12698 (11) | 0.0159 (5) | |
Si9 | −0.03549 (17) | 0.27323 (10) | 0.17579 (10) | 0.0141 (5) | |
Si10 | −0.03320 (18) | 0.11920 (11) | 0.17581 (11) | 0.0147 (5) | |
Si11 | 0.17719 (18) | 0.07124 (10) | 0.12951 (11) | 0.0153 (5) | |
Si12 | 0.31503 (18) | 0.19003 (11) | 0.16611 (10) | 0.0153 (5) | |
Si13 | 0.33506 (17) | 0.42775 (9) | 0.55733 (13) | 0.0148 (5) | |
Si14 | 0.18850 (18) | 0.31199 (11) | 0.52733 (10) | 0.0164 (5) | |
Si15 | −0.02954 (16) | 0.27758 (10) | 0.56122 (12) | 0.0157 (5) | |
Si16 | −0.03280 (16) | 0.12176 (10) | 0.56401 (12) | 0.0148 (5) | |
Si17 | 0.18004 (18) | 0.07088 (10) | 0.52719 (10) | 0.0136 (5) | |
Si18 | 0.31921 (18) | 0.18704 (10) | 0.56219 (11) | 0.0157 (5) | |
Si19 | 0.31600 (19) | 0.42364 (10) | 0.32795 (11) | 0.0159 (5) | |
Si20 | 0.17143 (17) | 0.31207 (11) | 0.36893 (11) | 0.0160 (5) | |
Si21 | −0.04305 (18) | 0.27337 (11) | 0.33111 (11) | 0.0159 (5) | |
Si22 | −0.03694 (18) | 0.11893 (11) | 0.32952 (11) | 0.0162 (5) | |
Si23 | 0.17775 (18) | 0.07205 (10) | 0.36953 (11) | 0.0154 (5) | |
Si24 | 0.30147 (17) | 0.19327 (11) | 0.32010 (10) | 0.0153 (5) | |
O1 | 0.2237 (4) | 0.3760 (3) | −0.0577 (3) | 0.0295 (14) | |
O2 | 0.0606 (4) | 0.3100 (3) | −0.0657 (3) | 0.0250 (13) | |
O3 | −0.0450 (5) | 0.2020 (2) | −0.0494 (3) | 0.0402 (16) | |
O4 | 0.0788 (4) | 0.1040 (3) | −0.0673 (3) | 0.0285 (15) | |
O5 | 0.2715 (4) | 0.1209 (2) | −0.0456 (3) | 0.0239 (14) | |
O6 | 0.2287 (4) | 0.2476 (3) | −0.0466 (3) | 0.0366 (16) | |
O7 | 0.2299 (5) | 0.3765 (3) | 0.1541 (3) | 0.0362 (18) | |
O8 | 0.0706 (4) | 0.3049 (3) | 0.1663 (3) | 0.0323 (15) | |
O9 | −0.0311 (5) | 0.1959 (3) | 0.1562 (2) | 0.0296 (15) | |
O10 | 0.0765 (4) | 0.0893 (3) | 0.1683 (3) | 0.0320 (15) | |
O11 | 0.2652 (5) | 0.1204 (3) | 0.1512 (3) | 0.0340 (17) | |
O12 | 0.2437 (4) | 0.2480 (3) | 0.1383 (3) | 0.0357 (16) | |
O13 | 0.1543 (5) | 0.3186 (3) | 0.0489 (3) | 0.0439 (17) | |
O14 | 0.1559 (4) | 0.0777 (3) | 0.0505 (3) | 0.0276 (13) | |
O15 | 0.3775 (5) | 0.4139 (3) | −0.1250 (3) | 0.0352 (17) | |
O16 | 0.3930 (5) | 0.3948 (3) | 0.0049 (3) | 0.0386 (17) | |
O17 | 0.4195 (4) | 0.4016 (3) | 0.1338 (3) | 0.0261 (14) | |
O18 | 0.3621 (4) | 0.1995 (3) | −0.1298 (3) | 0.0251 (13) | |
O19 | 0.4019 (5) | 0.2086 (3) | −0.0028 (3) | 0.0335 (16) | |
O20 | 0.4199 (4) | 0.1953 (3) | 0.1282 (3) | 0.0284 (14) | |
O21 | 0.2030 (4) | 0.0024 (2) | −0.0518 (3) | 0.0234 (13) | |
O22 | 0.2098 (5) | −0.0028 (3) | 0.1472 (3) | 0.0300 (15) | |
O23 | 0.3426 (4) | 0.4241 (2) | 0.2506 (3) | 0.0337 (13) | |
O24 | 0.3383 (4) | 0.1983 (2) | 0.2444 (3) | 0.0272 (12) | |
O25 | −0.0654 (3) | 0.2825 (2) | 0.2529 (3) | 0.0205 (11) | |
O26 | −0.0675 (3) | 0.1100 (2) | 0.2525 (3) | 0.0229 (11) | |
O27 | 0.2431 (4) | 0.3785 (3) | 0.5514 (4) | 0.0384 (16) | |
O28 | 0.0756 (4) | 0.3135 (2) | 0.5534 (3) | 0.0290 (14) | |
O29 | −0.0111 (5) | 0.1988 (3) | 0.5668 (3) | 0.0351 (15) | |
O30 | 0.0690 (4) | 0.0829 (3) | 0.5542 (3) | 0.0319 (14) | |
O31 | 0.2558 (4) | 0.1203 (3) | 0.5653 (3) | 0.0256 (14) | |
O32 | 0.2455 (4) | 0.2497 (3) | 0.5599 (3) | 0.0299 (14) | |
O33 | 0.2209 (5) | 0.3783 (3) | 0.3416 (3) | 0.0304 (16) | |
O34 | 0.0548 (4) | 0.3140 (2) | 0.3543 (3) | 0.0251 (14) | |
O35 | −0.0255 (5) | 0.1961 (2) | 0.3480 (2) | 0.0276 (15) | |
O36 | 0.0683 (5) | 0.0834 (3) | 0.3432 (3) | 0.0418 (18) | |
O37 | 0.2536 (5) | 0.1221 (3) | 0.3332 (3) | 0.0364 (17) | |
O38 | 0.2180 (4) | 0.2487 (3) | 0.3320 (3) | 0.0329 (15) | |
O39 | 0.1915 (5) | 0.3053 (3) | 0.4478 (3) | 0.0478 (17) | |
O40 | 0.1837 (5) | 0.0850 (3) | 0.4482 (3) | 0.0340 (15) | |
O41 | 0.3891 (4) | 0.4188 (3) | 0.6289 (3) | 0.0295 (15) | |
O42 | 0.4132 (5) | 0.4144 (3) | 0.4984 (3) | 0.0284 (14) | |
O43 | 0.4109 (4) | 0.3952 (3) | 0.3679 (3) | 0.0286 (15) | |
O44 | 0.3857 (4) | 0.1891 (3) | 0.6293 (3) | 0.0273 (14) | |
O45 | 0.3910 (5) | 0.1861 (3) | 0.4971 (3) | 0.0309 (15) | |
O46 | −0.1050 (4) | 0.2940 (3) | −0.1317 (3) | 0.0391 (17) | |
O47 | 0.2099 (4) | −0.0043 (2) | 0.5437 (3) | 0.0248 (14) | |
O48 | 0.2107 (5) | −0.0016 (3) | 0.3524 (3) | 0.0292 (15) | |
Atomic displacement parameters (Å2) top | U11 | U22 | U33 | U12 | U13 | U23 |
Si1 | 0.0211 (12) | 0.0118 (10) | 0.0102 (10) | −0.0002 (9) | 0.0037 (11) | −0.0009 (9) |
Si2 | 0.0237 (13) | 0.0126 (11) | 0.0157 (10) | −0.0015 (10) | 0.0021 (9) | −0.0002 (9) |
Si3 | 0.0237 (13) | 0.0148 (10) | 0.0122 (11) | 0.0002 (9) | 0.0010 (10) | −0.0017 (9) |
Si4 | 0.0208 (12) | 0.0128 (11) | 0.0129 (12) | −0.0008 (9) | 0.0000 (11) | −0.0003 (9) |
Si5 | 0.0182 (13) | 0.0120 (11) | 0.0122 (11) | −0.0029 (10) | 0.0022 (10) | −0.0011 (8) |
Si6 | 0.0194 (12) | 0.0124 (10) | 0.0136 (9) | −0.0054 (10) | 0.0049 (10) | −0.0003 (10) |
Si7 | 0.0224 (13) | 0.0119 (11) | 0.0100 (11) | −0.0016 (10) | 0.0034 (11) | −0.0004 (9) |
Si8 | 0.0179 (12) | 0.0154 (11) | 0.0144 (10) | −0.0006 (10) | 0.0014 (10) | 0.0003 (10) |
Si9 | 0.0213 (13) | 0.0132 (11) | 0.0079 (11) | −0.0003 (9) | 0.0036 (10) | 0.0023 (8) |
Si10 | 0.0218 (13) | 0.0134 (11) | 0.0088 (11) | −0.0013 (10) | 0.0029 (10) | −0.0019 (9) |
Si11 | 0.0203 (13) | 0.0128 (11) | 0.0127 (11) | 0.0016 (10) | 0.0022 (11) | −0.0009 (9) |
Si12 | 0.0212 (11) | 0.0137 (10) | 0.0108 (9) | −0.0019 (10) | 0.0028 (9) | −0.0001 (9) |
Si13 | 0.0206 (13) | 0.0093 (9) | 0.0145 (10) | 0.0010 (9) | 0.0004 (11) | 0.0000 (9) |
Si14 | 0.0220 (12) | 0.0117 (11) | 0.0156 (10) | −0.0014 (10) | 0.0037 (9) | 0.0011 (9) |
Si15 | 0.0217 (13) | 0.0123 (10) | 0.0132 (11) | 0.0003 (9) | 0.0041 (10) | 0.0002 (9) |
Si16 | 0.0163 (12) | 0.0134 (11) | 0.0147 (12) | 0.0014 (9) | 0.0021 (11) | −0.0008 (9) |
Si17 | 0.0198 (13) | 0.0083 (10) | 0.0126 (11) | −0.0006 (9) | 0.0026 (10) | 0.0004 (8) |
Si18 | 0.0221 (12) | 0.0123 (10) | 0.0127 (10) | −0.0025 (10) | 0.0001 (10) | 0.0010 (9) |
Si19 | 0.0237 (13) | 0.0113 (11) | 0.0128 (12) | −0.0010 (10) | 0.0017 (11) | 0.0018 (9) |
Si20 | 0.0190 (12) | 0.0144 (11) | 0.0146 (10) | −0.0032 (10) | 0.0033 (10) | 0.0002 (10) |
Si21 | 0.0210 (13) | 0.0146 (11) | 0.0120 (11) | −0.0002 (9) | 0.0007 (10) | −0.0011 (9) |
Si22 | 0.0220 (13) | 0.0147 (11) | 0.0117 (11) | 0.0013 (10) | −0.0002 (11) | 0.0002 (9) |
Si23 | 0.0226 (13) | 0.0099 (10) | 0.0137 (11) | 0.0013 (10) | 0.0006 (11) | 0.0001 (9) |
Si24 | 0.0213 (12) | 0.0140 (10) | 0.0106 (10) | −0.0006 (10) | 0.0062 (9) | −0.0013 (9) |
O1 | 0.029 (3) | 0.018 (3) | 0.042 (4) | −0.008 (3) | 0.000 (3) | 0.006 (3) |
O2 | 0.021 (3) | 0.027 (3) | 0.027 (3) | −0.006 (3) | 0.007 (2) | 0.005 (3) |
O3 | 0.057 (4) | 0.010 (3) | 0.054 (4) | 0.002 (3) | 0.008 (4) | −0.006 (3) |
O4 | 0.023 (3) | 0.041 (3) | 0.022 (3) | 0.005 (3) | 0.007 (3) | 0.007 (3) |
O5 | 0.021 (3) | 0.014 (3) | 0.036 (4) | −0.006 (2) | 0.008 (3) | 0.003 (3) |
O6 | 0.034 (4) | 0.018 (3) | 0.058 (4) | 0.012 (3) | 0.007 (4) | −0.006 (3) |
O7 | 0.036 (4) | 0.018 (3) | 0.055 (4) | −0.018 (3) | 0.004 (3) | −0.004 (3) |
O8 | 0.024 (3) | 0.038 (4) | 0.035 (3) | −0.011 (3) | 0.016 (3) | −0.011 (3) |
O9 | 0.055 (4) | 0.014 (3) | 0.020 (3) | 0.006 (3) | 0.004 (3) | −0.002 (3) |
O10 | 0.025 (4) | 0.044 (4) | 0.028 (3) | 0.017 (3) | 0.017 (3) | 0.013 (3) |
O11 | 0.034 (4) | 0.020 (3) | 0.047 (4) | −0.009 (3) | −0.011 (3) | −0.011 (3) |
O12 | 0.036 (4) | 0.025 (3) | 0.046 (4) | 0.018 (3) | 0.003 (3) | 0.002 (3) |
O13 | 0.060 (5) | 0.060 (4) | 0.012 (3) | 0.009 (3) | 0.000 (3) | −0.007 (3) |
O14 | 0.033 (3) | 0.035 (3) | 0.015 (3) | 0.003 (3) | 0.001 (3) | −0.003 (3) |
O15 | 0.051 (4) | 0.042 (4) | 0.013 (3) | 0.013 (3) | 0.021 (3) | −0.002 (3) |
O16 | 0.045 (4) | 0.053 (4) | 0.018 (3) | 0.016 (3) | −0.009 (3) | 0.004 (3) |
O17 | 0.020 (3) | 0.043 (4) | 0.016 (3) | 0.007 (3) | 0.009 (3) | −0.006 (3) |
O18 | 0.016 (3) | 0.042 (3) | 0.018 (3) | −0.003 (3) | 0.006 (2) | −0.001 (3) |
O19 | 0.036 (4) | 0.044 (4) | 0.020 (3) | −0.009 (3) | −0.009 (3) | −0.005 (3) |
O20 | 0.026 (3) | 0.037 (3) | 0.022 (3) | 0.005 (3) | 0.012 (3) | 0.007 (3) |
O21 | 0.022 (3) | 0.016 (3) | 0.032 (3) | −0.005 (2) | 0.008 (3) | −0.005 (3) |
O22 | 0.031 (4) | 0.020 (3) | 0.039 (4) | −0.001 (3) | 0.001 (3) | 0.007 (3) |
O23 | 0.045 (3) | 0.046 (3) | 0.011 (2) | 0.001 (3) | 0.006 (4) | 0.000 (3) |
O24 | 0.036 (3) | 0.036 (3) | 0.010 (2) | −0.012 (3) | 0.009 (3) | −0.004 (3) |
O25 | 0.024 (3) | 0.027 (2) | 0.010 (2) | 0.004 (2) | 0.003 (3) | 0.005 (3) |
O26 | 0.028 (3) | 0.031 (3) | 0.010 (2) | −0.002 (2) | 0.009 (3) | −0.002 (3) |
O27 | 0.028 (4) | 0.019 (3) | 0.068 (4) | −0.012 (3) | −0.005 (4) | −0.005 (4) |
O28 | 0.022 (3) | 0.020 (3) | 0.045 (3) | 0.000 (3) | 0.014 (3) | −0.006 (3) |
O29 | 0.052 (4) | 0.014 (3) | 0.039 (4) | −0.005 (3) | 0.001 (3) | 0.005 (3) |
O30 | 0.014 (3) | 0.031 (3) | 0.051 (4) | 0.012 (3) | 0.013 (3) | 0.005 (3) |
O31 | 0.039 (4) | 0.025 (3) | 0.013 (3) | −0.007 (3) | −0.008 (3) | 0.004 (2) |
O32 | 0.033 (3) | 0.021 (3) | 0.036 (3) | 0.009 (3) | 0.003 (3) | 0.008 (3) |
O33 | 0.031 (4) | 0.012 (3) | 0.048 (4) | −0.011 (3) | 0.010 (3) | 0.004 (3) |
O34 | 0.029 (3) | 0.015 (3) | 0.032 (3) | 0.001 (3) | −0.005 (3) | −0.006 (2) |
O35 | 0.052 (4) | 0.007 (3) | 0.024 (3) | −0.004 (3) | −0.008 (3) | −0.001 (2) |
O36 | 0.037 (4) | 0.040 (4) | 0.049 (4) | 0.022 (3) | −0.012 (3) | −0.007 (3) |
O37 | 0.058 (5) | 0.022 (3) | 0.029 (3) | −0.011 (3) | 0.019 (3) | 0.001 (3) |
O38 | 0.037 (4) | 0.020 (3) | 0.042 (4) | 0.008 (3) | 0.004 (3) | −0.008 (3) |
O39 | 0.052 (4) | 0.076 (4) | 0.015 (3) | −0.005 (4) | 0.002 (3) | −0.003 (4) |
O40 | 0.057 (4) | 0.027 (3) | 0.018 (3) | −0.006 (3) | 0.001 (3) | 0.002 (3) |
O41 | 0.031 (4) | 0.032 (3) | 0.025 (3) | 0.014 (3) | −0.012 (3) | −0.004 (3) |
O42 | 0.032 (4) | 0.028 (3) | 0.025 (3) | 0.011 (3) | 0.014 (3) | −0.004 (3) |
O43 | 0.024 (3) | 0.043 (4) | 0.018 (3) | 0.007 (3) | −0.004 (3) | 0.004 (3) |
O44 | 0.035 (3) | 0.023 (3) | 0.024 (3) | −0.005 (3) | −0.007 (3) | 0.000 (3) |
O45 | 0.039 (4) | 0.026 (3) | 0.028 (3) | −0.003 (3) | 0.014 (3) | 0.008 (3) |
O46 | 0.028 (4) | 0.065 (5) | 0.024 (3) | 0.005 (3) | −0.015 (3) | 0.008 (3) |
O47 | 0.025 (4) | 0.009 (3) | 0.040 (4) | −0.002 (2) | 0.005 (3) | 0.009 (3) |
O48 | 0.034 (4) | 0.013 (3) | 0.040 (4) | 0.006 (3) | 0.002 (3) | −0.002 (3) |
Geometric parameters (Å, º) top
C200—O202 | 1.1602 | Si14—O32 | 1.597 (6) |
C200—O201 | 1.1602 | Si15—O28 | 1.590 (6) |
O202—O202i | 1.38 (9) | Si15—O20iv | 1.585 (7) |
Si1—O15 | 1.566 (7) | Si15—O19iv | 1.586 (7) |
Si1—O47ii | 1.584 (7) | Si15—O29 | 1.602 (7) |
Si1—O1 | 1.600 (6) | Si16—O16iv | 1.567 (7) |
Si1—O16 | 1.612 (7) | Si16—O29 | 1.573 (7) |
Si2—O1 | 1.567 (6) | Si16—O30 | 1.583 (6) |
Si2—O6 | 1.570 (7) | Si16—O17iv | 1.599 (6) |
Si2—O13 | 1.592 (6) | Si17—O40 | 1.597 (6) |
Si2—O2 | 1.599 (6) | Si17—O30 | 1.599 (6) |
Si3—O3 | 1.582 (5) | Si17—O47 | 1.593 (7) |
Si3—O45iii | 1.580 (6) | Si17—O31 | 1.609 (6) |
Si3—O46 | 1.585 (7) | Si18—O31 | 1.590 (6) |
Si3—O2 | 1.597 (6) | Si18—O32 | 1.595 (6) |
Si4—O4 | 1.582 (6) | Si18—O44 | 1.604 (6) |
Si4—O42iii | 1.588 (6) | Si18—O45 | 1.606 (7) |
Si4—O43iii | 1.599 (6) | Si19—O23 | 1.573 (8) |
Si4—O3 | 1.598 (7) | Si19—O33 | 1.589 (7) |
Si5—O5 | 1.589 (6) | Si19—O22ii | 1.592 (7) |
Si5—O14 | 1.585 (8) | Si19—O43 | 1.603 (6) |
Si5—O21 | 1.594 (5) | Si20—O33 | 1.579 (7) |
Si5—O4 | 1.629 (6) | Si20—O34 | 1.588 (6) |
Si6—O19 | 1.587 (7) | Si20—O39 | 1.591 (8) |
Si6—O6 | 1.594 (6) | Si20—O38 | 1.593 (6) |
Si6—O18 | 1.596 (7) | Si21—O18iv | 1.586 (6) |
Si6—O5 | 1.604 (5) | Si21—O25 | 1.588 (7) |
Si7—O7 | 1.588 (7) | Si21—O35 | 1.608 (5) |
Si7—O17 | 1.597 (6) | Si21—O34 | 1.611 (6) |
Si7—O23 | 1.594 (8) | Si22—O26 | 1.589 (8) |
Si7—O48ii | 1.598 (7) | Si22—O36 | 1.603 (7) |
Si8—O12 | 1.580 (6) | Si22—O15iv | 1.595 (6) |
Si8—O13 | 1.580 (7) | Si22—O35 | 1.598 (7) |
Si8—O7 | 1.595 (7) | Si23—O36 | 1.572 (7) |
Si8—O8 | 1.614 (6) | Si23—O48 | 1.577 (7) |
Si9—O8 | 1.568 (6) | Si23—O40 | 1.582 (8) |
Si9—O44iii | 1.594 (6) | Si23—O37 | 1.596 (7) |
Si9—O25 | 1.590 (7) | Si24—O24 | 1.588 (6) |
Si9—O9 | 1.599 (7) | Si24—O37 | 1.584 (7) |
Si10—O41iii | 1.592 (6) | Si24—O46v | 1.597 (6) |
Si10—O10 | 1.594 (6) | Si24—O38 | 1.596 (6) |
Si10—O9 | 1.587 (7) | O15—Si22vi | 1.595 (6) |
Si10—O26 | 1.604 (6) | O16—Si16vi | 1.567 (7) |
Si11—O22 | 1.586 (7) | O17—Si16vi | 1.593 (7) |
Si11—O10 | 1.590 (6) | O18—Si21vi | 1.586 (6) |
Si11—O11 | 1.597 (7) | O19—Si15vi | 1.586 (7) |
Si11—O14 | 1.602 (6) | O20—Si15vi | 1.585 (7) |
Si12—O11 | 1.573 (7) | O21—Si13vii | 1.585 (7) |
Si12—O20 | 1.597 (6) | O22—Si19vii | 1.592 (7) |
Si12—O24 | 1.591 (7) | O41—Si10v | 1.592 (6) |
Si12—O12 | 1.599 (6) | O42—Si4v | 1.588 (6) |
Si13—O27 | 1.584 (6) | O43—Si4v | 1.599 (6) |
Si13—O21ii | 1.585 (7) | O44—Si9v | 1.594 (6) |
Si13—O42 | 1.587 (7) | O45—Si3v | 1.581 (6) |
Si13—O41 | 1.606 (6) | O46—Si24iii | 1.597 (6) |
Si14—O39 | 1.588 (6) | O47—Si1vii | 1.584 (7) |
Si14—O28 | 1.598 (6) | O48—Si7vii | 1.598 (7) |
Si14—O27 | 1.592 (7) | | |
| | | |
O202—C200—O201 | 180.0 | O30—Si16—O17iv | 107.8 (4) |
C200—O202—O202i | 135 (8) | O40—Si17—O30 | 109.5 (3) |
O15—Si1—O47ii | 109.9 (3) | O40—Si17—O47 | 111.2 (3) |
O15—Si1—O1 | 108.3 (4) | O30—Si17—O47 | 107.8 (3) |
O47ii—Si1—O1 | 108.2 (4) | O40—Si17—O31 | 109.5 (3) |
O15—Si1—O16 | 110.8 (4) | O30—Si17—O31 | 109.5 (4) |
O47ii—Si1—O16 | 110.9 (3) | O47—Si17—O31 | 109.4 (4) |
O1—Si1—O16 | 108.7 (4) | O31—Si18—O32 | 109.8 (4) |
O1—Si2—O6 | 111.0 (4) | O31—Si18—O44 | 106.5 (3) |
O1—Si2—O13 | 109.7 (4) | O32—Si18—O44 | 110.1 (3) |
O6—Si2—O13 | 108.9 (3) | O31—Si18—O45 | 109.8 (3) |
O1—Si2—O2 | 107.6 (3) | O32—Si18—O45 | 110.6 (3) |
O6—Si2—O2 | 110.1 (3) | O44—Si18—O45 | 109.8 (4) |
O13—Si2—O2 | 109.5 (4) | O23—Si19—O33 | 110.5 (3) |
O3—Si3—O45iii | 109.0 (4) | O23—Si19—O22ii | 110.2 (3) |
O3—Si3—O46 | 109.9 (4) | O33—Si19—O22ii | 107.9 (4) |
O45iii—Si3—O46 | 109.4 (4) | O23—Si19—O43 | 107.8 (3) |
O3—Si3—O2 | 110.6 (3) | O33—Si19—O43 | 110.1 (4) |
O45iii—Si3—O2 | 109.0 (3) | O22ii—Si19—O43 | 110.4 (4) |
O46—Si3—O2 | 108.9 (3) | O33—Si20—O34 | 109.1 (3) |
O4—Si4—O42iii | 109.9 (3) | O33—Si20—O39 | 109.8 (4) |
O4—Si4—O43iii | 108.8 (3) | O34—Si20—O39 | 110.3 (3) |
O42iii—Si4—O43iii | 110.6 (4) | O33—Si20—O38 | 110.5 (4) |
O4—Si4—O3 | 109.5 (3) | O34—Si20—O38 | 108.5 (3) |
O42iii—Si4—O3 | 108.2 (4) | O39—Si20—O38 | 108.6 (4) |
O43iii—Si4—O3 | 109.9 (3) | O18iv—Si21—O25 | 106.9 (3) |
O5—Si5—O14 | 110.3 (3) | O18iv—Si21—O35 | 110.3 (3) |
O5—Si5—O21 | 107.0 (3) | O25—Si21—O35 | 110.0 (3) |
O14—Si5—O21 | 110.3 (3) | O18iv—Si21—O34 | 109.5 (3) |
O5—Si5—O4 | 109.9 (4) | O25—Si21—O34 | 111.9 (3) |
O14—Si5—O4 | 108.6 (3) | O35—Si21—O34 | 108.2 (3) |
O21—Si5—O4 | 110.7 (3) | O26—Si22—O36 | 109.7 (3) |
O19—Si6—O6 | 109.4 (4) | O26—Si22—O15iv | 108.3 (3) |
O19—Si6—O18 | 108.4 (4) | O36—Si22—O15iv | 110.4 (4) |
O6—Si6—O18 | 110.2 (4) | O26—Si22—O35 | 110.7 (3) |
O19—Si6—O5 | 110.6 (3) | O36—Si22—O35 | 108.1 (4) |
O6—Si6—O5 | 109.7 (4) | O15iv—Si22—O35 | 109.8 (3) |
O18—Si6—O5 | 108.6 (3) | O36—Si23—O48 | 108.9 (4) |
O7—Si7—O17 | 110.2 (4) | O36—Si23—O40 | 110.5 (4) |
O7—Si7—O23 | 110.2 (3) | O48—Si23—O40 | 110.6 (3) |
O17—Si7—O23 | 107.7 (3) | O36—Si23—O37 | 110.3 (4) |
O7—Si7—O48ii | 107.7 (4) | O48—Si23—O37 | 108.4 (4) |
O17—Si7—O48ii | 110.4 (3) | O40—Si23—O37 | 108.1 (3) |
O23—Si7—O48ii | 110.7 (3) | O24—Si24—O37 | 109.8 (3) |
O12—Si8—O13 | 108.5 (3) | O24—Si24—O46v | 108.4 (4) |
O12—Si8—O7 | 110.8 (4) | O37—Si24—O46v | 111.1 (4) |
O13—Si8—O7 | 109.5 (4) | O24—Si24—O38 | 108.3 (3) |
O12—Si8—O8 | 111.6 (4) | O37—Si24—O38 | 108.9 (4) |
O13—Si8—O8 | 109.1 (4) | O46v—Si24—O38 | 110.3 (4) |
O7—Si8—O8 | 107.3 (3) | Si2—O1—Si1 | 146.9 (4) |
O8—Si9—O44iii | 109.5 (4) | Si3—O2—Si2 | 145.4 (4) |
O8—Si9—O25 | 107.3 (3) | Si3—O3—Si4 | 160.8 (5) |
O44iii—Si9—O25 | 109.6 (3) | Si4—O4—Si5 | 147.1 (4) |
O8—Si9—O9 | 109.3 (4) | Si5—O5—Si6 | 147.5 (4) |
O44iii—Si9—O9 | 110.2 (3) | Si2—O6—Si6 | 163.8 (4) |
O25—Si9—O9 | 110.8 (3) | Si8—O7—Si7 | 157.6 (5) |
O41iii—Si10—O10 | 111.3 (4) | Si9—O8—Si8 | 151.6 (4) |
O41iii—Si10—O9 | 109.5 (3) | Si10—O9—Si9 | 151.6 (4) |
O10—Si10—O9 | 109.1 (3) | Si10—O10—Si11 | 155.5 (4) |
O41iii—Si10—O26 | 108.4 (3) | Si12—O11—Si11 | 155.7 (5) |
O10—Si10—O26 | 108.1 (3) | Si8—O12—Si12 | 167.5 (4) |
O9—Si10—O26 | 110.5 (3) | Si8—O13—Si2 | 160.5 (5) |
O22—Si11—O10 | 109.7 (3) | Si5—O14—Si11 | 158.7 (4) |
O22—Si11—O11 | 108.6 (4) | Si1—O15—Si22vi | 150.0 (4) |
O10—Si11—O11 | 110.5 (4) | Si16vi—O16—Si1 | 173.1 (5) |
O22—Si11—O14 | 109.9 (3) | Si7—O17—Si16vi | 145.9 (4) |
O10—Si11—O14 | 107.9 (4) | Si21vi—O18—Si6 | 141.6 (4) |
O11—Si11—O14 | 110.2 (3) | Si6—O19—Si15vi | 168.3 (5) |
O11—Si12—O20 | 110.0 (3) | Si15vi—O20—Si12 | 142.4 (4) |
O11—Si12—O24 | 110.9 (3) | Si13vii—O21—Si5 | 146.2 (4) |
O20—Si12—O24 | 106.5 (3) | Si11—O22—Si19vii | 151.2 (5) |
O11—Si12—O12 | 109.3 (4) | Si19—O23—Si7 | 156.2 (4) |
O20—Si12—O12 | 108.1 (3) | Si24—O24—Si12 | 149.1 (4) |
O24—Si12—O12 | 112.0 (3) | Si21—O25—Si9 | 151.3 (3) |
O27—Si13—O21ii | 109.8 (4) | Si22—O26—Si10 | 145.8 (3) |
O27—Si13—O42 | 110.4 (4) | Si13—O27—Si14 | 154.3 (5) |
O21ii—Si13—O42 | 108.5 (3) | Si15—O28—Si14 | 149.2 (4) |
O27—Si13—O41 | 110.1 (4) | Si16—O29—Si15 | 159.7 (4) |
O21ii—Si13—O41 | 108.1 (3) | Si16—O30—Si17 | 156.3 (4) |
O42—Si13—O41 | 109.8 (4) | Si18—O31—Si17 | 147.1 (4) |
O39—Si14—O28 | 110.6 (3) | Si18—O32—Si14 | 156.9 (4) |
O39—Si14—O27 | 110.9 (4) | Si20—O33—Si19 | 151.2 (5) |
O28—Si14—O27 | 108.5 (3) | Si20—O34—Si21 | 147.0 (4) |
O39—Si14—O32 | 108.9 (4) | Si22—O35—Si21 | 151.0 (4) |
O28—Si14—O32 | 109.4 (3) | Si23—O36—Si22 | 160.1 (5) |
O27—Si14—O32 | 108.5 (4) | Si24—O37—Si23 | 153.6 (4) |
O28—Si15—O20iv | 107.6 (3) | Si24—O38—Si20 | 154.0 (4) |
O28—Si15—O19iv | 110.5 (4) | Si14—O39—Si20 | 165.2 (5) |
O20iv—Si15—O19iv | 111.5 (4) | Si23—O40—Si17 | 159.8 (4) |
O28—Si15—O29 | 108.7 (3) | Si10v—O41—Si13 | 150.0 (4) |
O20iv—Si15—O29 | 110.2 (3) | Si13—O42—Si4v | 157.7 (4) |
O19iv—Si15—O29 | 108.4 (3) | Si4v—O43—Si19 | 150.0 (4) |
O16iv—Si16—O29 | 110.5 (3) | Si9v—O44—Si18 | 149.5 (4) |
O16iv—Si16—O30 | 110.1 (4) | Si3v—O45—Si18 | 153.4 (4) |
O29—Si16—O30 | 109.4 (3) | Si3—O46—Si24iii | 156.1 (5) |
O16iv—Si16—O17iv | 109.6 (4) | Si1vii—O47—Si17 | 149.5 (4) |
O29—Si16—O17iv | 109.4 (3) | Si23—O48—Si7vii | 148.5 (5) |
Symmetry codes: (i) −x+1, −y, −z+2; (ii) −x+1/2, y+1/2, −z+1/2; (iii) x−1/2, −y+1/2, z−1/2; (iv) x−1/2, −y+1/2, z+1/2; (v) x+1/2, −y+1/2, z+1/2; (vi) x+1/2, −y+1/2, z−1/2; (vii) −x+1/2, y−1/2, −z+1/2. |
Crystal data top
C0.6O49.2Si24 | F(000) = 2968 |
Mr = 1468.2 | Dx = 1.866 Mg m−3 |
Monoclinic, P21/n | Mo Kα radiation, λ = 0.71073 Å |
a = 13.388 (2) Å | Cell parameters from 211 reflections |
b = 20.132 (3) Å | θ = 2.1–22.5° |
c = 19.902 (3) Å | µ = 0.69 mm−1 |
β = 90.040 (2)° | T = 296 K |
V = 5364.1 (14) Å3 | Coffin shape, colorless |
Z = 4 | 0.14 × 0.08 × 0.07 mm |
Data collection top
CCD area detector diffractometer | 12862 independent reflections |
Radiation source: fine-focus sealed tube | 5397 reflections with I > 2σ(I) |
Graphite monochromator | Rint = 0.143 |
phi and ω scans | θmax = 28.7°, θmin = 1.0° |
Absorption correction: analytical ? | h = −17→17 |
Tmin = 0.908, Tmax = 0.955 | k = −26→26 |
62011 measured reflections | l = −25→25 |
Refinement top
Refinement on F2 | 4 restraints |
Least-squares matrix: full | Primary atom site location: structure-invariant direct methods |
R[F2 > 2σ(F2)] = 0.053 | Secondary atom site location: difference Fourier map |
wR(F2) = 0.122 | w = 1/[σ2(Fo2) + (0.0374P)2] where P = (Fo2 + 2Fc2)/3 |
S = 0.83 | (Δ/σ)max = 0.001 |
12862 reflections | Δρmax = 0.56 e Å−3 |
664 parameters | Δρmin = −0.62 e Å−3 |
Crystal data top
C0.6O49.2Si24 | V = 5364.1 (14) Å3 |
Mr = 1468.2 | Z = 4 |
Monoclinic, P21/n | Mo Kα radiation |
a = 13.388 (2) Å | µ = 0.69 mm−1 |
b = 20.132 (3) Å | T = 296 K |
c = 19.902 (3) Å | 0.14 × 0.08 × 0.07 mm |
β = 90.040 (2)° | |
Data collection top
CCD area detector diffractometer | 12862 independent reflections |
Absorption correction: analytical ? | 5397 reflections with I > 2σ(I) |
Tmin = 0.908, Tmax = 0.955 | Rint = 0.143 |
62011 measured reflections | |
Refinement top
R[F2 > 2σ(F2)] = 0.053 | 664 parameters |
wR(F2) = 0.122 | 4 restraints |
S = 0.83 | Δρmax = 0.56 e Å−3 |
12862 reflections | Δρmin = −0.62 e Å−3 |
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 | x | y | z | Uiso*/Ueq | Occ. (<1) |
C200 | 0.993 (2) | 0.4860 (18) | 0.419 (3) | 0.27 (4)* | 0.281 (15) |
O201 | 0.978 (2) | 0.491 (3) | 0.361 (3) | 0.62 (8)* | 0.281 (15) |
O202 | 1.007 (2) | 0.481 (2) | 0.476 (3) | 0.24 (3)* | 0.281 (15) |
C500 | 0.006 (2) | 0.508 (2) | 0.187 (4) | 0.73 (9)* | 0.31 (2) |
O501 | 0.014 (3) | 0.517 (3) | 0.130 (4) | 0.72 (10)* | 0.31 (2) |
O502 | −0.003 (2) | 0.499 (3) | 0.245 (4) | 0.64 (8)* | 0.31 (2) |
Si1 | 0.32242 (18) | 0.42049 (10) | −0.05565 (13) | 0.0131 (5) | |
Si2 | 0.16770 (19) | 0.31296 (12) | −0.03045 (11) | 0.0163 (5) | |
Si3 | −0.04992 (19) | 0.27965 (11) | −0.06243 (13) | 0.0162 (6) | |
Si4 | −0.03530 (18) | 0.12384 (11) | −0.06301 (13) | 0.0149 (6) | |
Si5 | 0.1773 (2) | 0.07614 (11) | −0.02826 (11) | 0.0136 (6) | |
Si6 | 0.31558 (17) | 0.19452 (11) | −0.05589 (13) | 0.0150 (5) | |
Si7 | 0.3202 (2) | 0.42530 (11) | 0.17173 (12) | 0.0145 (6) | |
Si8 | 0.17551 (17) | 0.31115 (12) | 0.12699 (11) | 0.0143 (5) | |
Si9 | −0.03541 (19) | 0.27329 (11) | 0.17558 (12) | 0.0135 (6) | |
Si10 | −0.03273 (19) | 0.11941 (12) | 0.17579 (12) | 0.0147 (6) | |
Si11 | 0.17716 (19) | 0.07131 (11) | 0.12922 (13) | 0.0147 (5) | |
Si12 | 0.31518 (19) | 0.19021 (12) | 0.16625 (11) | 0.0145 (5) | |
Si13 | 0.33516 (18) | 0.42784 (10) | 0.55736 (14) | 0.0135 (5) | |
Si14 | 0.18836 (18) | 0.31191 (12) | 0.52717 (11) | 0.0146 (5) | |
Si15 | −0.02945 (18) | 0.27746 (11) | 0.56118 (13) | 0.0141 (5) | |
Si16 | −0.03281 (18) | 0.12165 (11) | 0.56410 (13) | 0.0134 (5) | |
Si17 | 0.1796 (2) | 0.07075 (11) | 0.52723 (11) | 0.0140 (6) | |
Si18 | 0.31890 (19) | 0.18707 (11) | 0.56220 (12) | 0.0150 (5) | |
Si19 | 0.3158 (2) | 0.42357 (11) | 0.32812 (12) | 0.0148 (6) | |
Si20 | 0.17082 (18) | 0.31212 (12) | 0.36883 (12) | 0.0163 (5) | |
Si21 | −0.04344 (19) | 0.27331 (11) | 0.33104 (12) | 0.0144 (6) | |
Si22 | −0.0368 (2) | 0.11864 (12) | 0.32947 (12) | 0.0155 (6) | |
Si23 | 0.1775 (2) | 0.07217 (10) | 0.36937 (13) | 0.0137 (5) | |
Si24 | 0.30113 (18) | 0.19327 (12) | 0.32031 (11) | 0.0152 (5) | |
O1 | 0.2233 (4) | 0.3770 (3) | −0.0582 (4) | 0.0296 (15) | |
O2 | 0.0599 (4) | 0.3103 (3) | −0.0655 (3) | 0.0235 (14) | |
O3 | −0.0455 (5) | 0.2021 (3) | −0.0491 (3) | 0.0369 (15) | |
O4 | 0.0788 (4) | 0.1035 (2) | −0.0673 (3) | 0.0251 (15) | |
O5 | 0.2712 (4) | 0.1211 (3) | −0.0457 (3) | 0.0246 (15) | |
O6 | 0.2279 (4) | 0.2471 (3) | −0.0471 (4) | 0.0350 (17) | |
O7 | 0.2297 (5) | 0.3759 (3) | 0.1548 (3) | 0.037 (2) | |
O8 | 0.0707 (4) | 0.3041 (3) | 0.1657 (3) | 0.0308 (15) | |
O9 | −0.0309 (5) | 0.1957 (3) | 0.1557 (2) | 0.0276 (16) | |
O10 | 0.0764 (5) | 0.0890 (3) | 0.1677 (3) | 0.0304 (16) | |
O11 | 0.2651 (5) | 0.1210 (3) | 0.1513 (3) | 0.0312 (18) | |
O12 | 0.2427 (5) | 0.2478 (3) | 0.1390 (3) | 0.0343 (16) | |
O13 | 0.1548 (5) | 0.3182 (3) | 0.0484 (3) | 0.0421 (18) | |
O14 | 0.1570 (4) | 0.0779 (3) | 0.0504 (3) | 0.0273 (15) | |
O15 | 0.3786 (5) | 0.4140 (3) | −0.1250 (3) | 0.0331 (18) | |
O16 | 0.3927 (5) | 0.3949 (3) | 0.0044 (3) | 0.0382 (19) | |
O17 | 0.4196 (4) | 0.4022 (3) | 0.1341 (3) | 0.0251 (15) | |
O18 | 0.3611 (4) | 0.1998 (3) | −0.1298 (3) | 0.0232 (14) | |
O19 | 0.4031 (5) | 0.2079 (3) | −0.0029 (3) | 0.0315 (16) | |
O20 | 0.4195 (4) | 0.1956 (3) | 0.1278 (3) | 0.0249 (14) | |
O21 | 0.2031 (4) | 0.0028 (2) | −0.0524 (3) | 0.0225 (14) | |
O22 | 0.2093 (5) | −0.0028 (3) | 0.1476 (3) | 0.0263 (16) | |
O23 | 0.3427 (3) | 0.4237 (2) | 0.2505 (3) | 0.0294 (12) | |
O24 | 0.3384 (3) | 0.1980 (2) | 0.2445 (3) | 0.0262 (12) | |
O25 | −0.0654 (3) | 0.28263 (19) | 0.2519 (3) | 0.0239 (12) | |
O26 | −0.0679 (3) | 0.1097 (2) | 0.2521 (3) | 0.0224 (12) | |
O27 | 0.2430 (4) | 0.3780 (3) | 0.5514 (4) | 0.0346 (17) | |
O28 | 0.0747 (4) | 0.3134 (2) | 0.5540 (3) | 0.0257 (14) | |
O29 | −0.0112 (4) | 0.1993 (3) | 0.5670 (3) | 0.0337 (16) | |
O30 | 0.0687 (4) | 0.0827 (2) | 0.5543 (3) | 0.0297 (15) | |
O31 | 0.2566 (4) | 0.1202 (3) | 0.5648 (3) | 0.0253 (15) | |
O32 | 0.2457 (4) | 0.2490 (3) | 0.5600 (3) | 0.0308 (16) | |
O33 | 0.2204 (5) | 0.3792 (3) | 0.3418 (3) | 0.0286 (17) | |
O34 | 0.0549 (4) | 0.3143 (2) | 0.3538 (2) | 0.0197 (13) | |
O35 | −0.0265 (5) | 0.1963 (3) | 0.3480 (3) | 0.0292 (16) | |
O36 | 0.0681 (5) | 0.0830 (3) | 0.3433 (3) | 0.0377 (18) | |
O37 | 0.2539 (5) | 0.1219 (3) | 0.3335 (3) | 0.0335 (18) | |
O38 | 0.2184 (5) | 0.2489 (3) | 0.3318 (3) | 0.0290 (15) | |
O39 | 0.1922 (4) | 0.3061 (3) | 0.4472 (3) | 0.0452 (16) | |
O40 | 0.1833 (5) | 0.0848 (3) | 0.4486 (3) | 0.0313 (15) | |
O41 | 0.3903 (5) | 0.4193 (3) | 0.6287 (3) | 0.0323 (17) | |
O42 | 0.4130 (5) | 0.4144 (3) | 0.4984 (3) | 0.0310 (16) | |
O43 | 0.4103 (5) | 0.3949 (3) | 0.3680 (3) | 0.0270 (16) | |
O44 | 0.3850 (4) | 0.1901 (3) | 0.6288 (3) | 0.0243 (14) | |
O45 | 0.3895 (5) | 0.1860 (3) | 0.4970 (3) | 0.0290 (15) | |
O46 | −0.1047 (4) | 0.2944 (3) | −0.1316 (3) | 0.0372 (17) | |
O47 | 0.2102 (4) | −0.0046 (2) | 0.5427 (3) | 0.0194 (15) | |
O48 | 0.2107 (5) | −0.0022 (3) | 0.3523 (3) | 0.0309 (17) | |
Atomic displacement parameters (Å2) top | U11 | U22 | U33 | U12 | U13 | U23 |
Si1 | 0.0209 (13) | 0.0086 (10) | 0.0098 (11) | 0.0010 (10) | −0.0012 (12) | −0.0007 (10) |
Si2 | 0.0227 (14) | 0.0099 (12) | 0.0164 (11) | −0.0017 (11) | 0.0010 (10) | 0.0001 (10) |
Si3 | 0.0217 (14) | 0.0115 (11) | 0.0154 (13) | −0.0021 (9) | 0.0006 (11) | −0.0041 (10) |
Si4 | 0.0198 (14) | 0.0132 (12) | 0.0116 (13) | −0.0011 (10) | −0.0031 (12) | −0.0015 (10) |
Si5 | 0.0199 (14) | 0.0081 (12) | 0.0127 (12) | −0.0021 (11) | 0.0002 (11) | 0.0002 (9) |
Si6 | 0.0201 (13) | 0.0115 (10) | 0.0135 (10) | −0.0064 (11) | 0.0050 (11) | 0.0003 (12) |
Si7 | 0.0227 (15) | 0.0104 (12) | 0.0105 (13) | −0.0026 (11) | 0.0021 (12) | −0.0017 (10) |
Si8 | 0.0153 (12) | 0.0129 (11) | 0.0148 (11) | −0.0013 (11) | 0.0005 (11) | −0.0021 (11) |
Si9 | 0.0193 (14) | 0.0122 (12) | 0.0090 (12) | 0.0000 (10) | −0.0004 (11) | 0.0014 (9) |
Si10 | 0.0232 (15) | 0.0119 (12) | 0.0089 (13) | −0.0024 (11) | 0.0008 (12) | −0.0013 (10) |
Si11 | 0.0204 (14) | 0.0107 (12) | 0.0129 (12) | 0.0016 (11) | 0.0009 (13) | −0.0005 (10) |
Si12 | 0.0197 (12) | 0.0129 (11) | 0.0111 (10) | −0.0002 (12) | 0.0027 (10) | −0.0005 (10) |
Si13 | 0.0205 (14) | 0.0089 (10) | 0.0112 (11) | 0.0005 (9) | 0.0005 (11) | 0.0001 (10) |
Si14 | 0.0197 (13) | 0.0114 (12) | 0.0128 (11) | −0.0026 (11) | 0.0032 (9) | 0.0007 (10) |
Si15 | 0.0215 (14) | 0.0101 (11) | 0.0106 (12) | 0.0008 (9) | 0.0030 (11) | −0.0019 (10) |
Si16 | 0.0171 (14) | 0.0104 (12) | 0.0127 (13) | 0.0006 (10) | −0.0004 (12) | −0.0007 (10) |
Si17 | 0.0198 (15) | 0.0097 (12) | 0.0125 (12) | −0.0015 (11) | 0.0008 (11) | 0.0009 (9) |
Si18 | 0.0224 (13) | 0.0098 (11) | 0.0130 (11) | −0.0026 (11) | −0.0011 (11) | 0.0013 (10) |
Si19 | 0.0208 (15) | 0.0113 (12) | 0.0122 (13) | −0.0019 (11) | 0.0007 (12) | 0.0002 (9) |
Si20 | 0.0226 (14) | 0.0132 (12) | 0.0131 (11) | −0.0008 (12) | 0.0027 (11) | −0.0020 (12) |
Si21 | 0.0208 (15) | 0.0114 (12) | 0.0109 (13) | 0.0001 (10) | 0.0002 (11) | −0.0009 (9) |
Si22 | 0.0222 (15) | 0.0124 (12) | 0.0121 (13) | 0.0010 (11) | −0.0006 (12) | 0.0003 (10) |
Si23 | 0.0234 (14) | 0.0057 (11) | 0.0119 (12) | −0.0002 (10) | 0.0000 (13) | −0.0015 (10) |
Si24 | 0.0230 (13) | 0.0102 (10) | 0.0123 (11) | −0.0019 (12) | 0.0040 (10) | −0.0019 (10) |
O1 | 0.026 (4) | 0.016 (3) | 0.047 (4) | −0.005 (3) | −0.004 (4) | 0.014 (3) |
O2 | 0.019 (3) | 0.026 (3) | 0.025 (3) | −0.004 (3) | 0.007 (3) | 0.008 (3) |
O3 | 0.057 (4) | 0.010 (3) | 0.044 (4) | 0.002 (3) | 0.008 (4) | −0.004 (3) |
O4 | 0.021 (3) | 0.032 (3) | 0.022 (3) | 0.005 (3) | 0.009 (3) | 0.009 (3) |
O5 | 0.025 (3) | 0.012 (3) | 0.037 (4) | −0.006 (2) | 0.007 (3) | 0.006 (3) |
O6 | 0.036 (4) | 0.011 (3) | 0.059 (4) | 0.008 (3) | 0.012 (4) | −0.004 (3) |
O7 | 0.045 (5) | 0.017 (3) | 0.049 (5) | −0.019 (3) | 0.003 (4) | −0.008 (3) |
O8 | 0.022 (3) | 0.033 (3) | 0.037 (3) | −0.006 (3) | 0.019 (3) | −0.006 (3) |
O9 | 0.055 (5) | 0.011 (3) | 0.016 (3) | 0.003 (3) | 0.000 (3) | 0.000 (3) |
O10 | 0.028 (4) | 0.040 (4) | 0.023 (3) | 0.014 (3) | 0.016 (3) | 0.012 (3) |
O11 | 0.040 (4) | 0.016 (3) | 0.038 (4) | −0.010 (3) | −0.009 (3) | −0.010 (3) |
O12 | 0.037 (4) | 0.027 (3) | 0.038 (4) | 0.016 (3) | 0.000 (3) | 0.001 (3) |
O13 | 0.060 (5) | 0.052 (4) | 0.014 (3) | 0.003 (3) | −0.009 (3) | −0.004 (3) |
O14 | 0.039 (4) | 0.031 (3) | 0.012 (3) | 0.004 (3) | −0.002 (3) | −0.006 (3) |
O15 | 0.045 (5) | 0.041 (4) | 0.013 (4) | 0.011 (3) | 0.015 (3) | 0.003 (3) |
O16 | 0.047 (5) | 0.050 (4) | 0.018 (3) | 0.016 (4) | −0.019 (3) | 0.006 (3) |
O17 | 0.020 (4) | 0.039 (4) | 0.016 (3) | 0.004 (3) | 0.006 (3) | −0.001 (3) |
O18 | 0.017 (3) | 0.039 (4) | 0.014 (3) | −0.004 (3) | 0.005 (3) | 0.004 (3) |
O19 | 0.031 (4) | 0.044 (4) | 0.020 (3) | −0.013 (3) | −0.008 (3) | 0.001 (3) |
O20 | 0.026 (3) | 0.032 (3) | 0.017 (3) | 0.002 (3) | 0.005 (3) | 0.005 (3) |
O21 | 0.023 (4) | 0.012 (3) | 0.033 (3) | −0.004 (2) | 0.003 (3) | −0.005 (3) |
O22 | 0.031 (4) | 0.013 (3) | 0.035 (4) | −0.006 (3) | 0.004 (3) | 0.006 (3) |
O23 | 0.042 (3) | 0.041 (3) | 0.005 (2) | 0.007 (3) | 0.004 (4) | 0.000 (3) |
O24 | 0.034 (3) | 0.034 (3) | 0.011 (3) | −0.011 (3) | 0.005 (3) | −0.001 (3) |
O25 | 0.033 (3) | 0.028 (3) | 0.011 (2) | 0.006 (2) | 0.003 (4) | 0.004 (3) |
O26 | 0.020 (3) | 0.031 (3) | 0.017 (3) | −0.006 (2) | 0.012 (4) | −0.009 (3) |
O27 | 0.023 (4) | 0.017 (3) | 0.063 (5) | −0.013 (3) | −0.004 (4) | −0.001 (4) |
O28 | 0.016 (3) | 0.021 (3) | 0.040 (3) | −0.002 (3) | 0.011 (3) | 0.000 (3) |
O29 | 0.051 (4) | 0.013 (3) | 0.037 (4) | −0.004 (3) | 0.000 (3) | 0.006 (3) |
O30 | 0.019 (3) | 0.025 (3) | 0.046 (4) | 0.008 (3) | 0.009 (4) | 0.002 (3) |
O31 | 0.041 (4) | 0.022 (3) | 0.012 (3) | −0.012 (3) | −0.006 (3) | 0.006 (3) |
O32 | 0.043 (4) | 0.016 (3) | 0.034 (4) | 0.008 (3) | 0.010 (4) | 0.009 (3) |
O33 | 0.023 (4) | 0.009 (3) | 0.054 (5) | −0.006 (3) | 0.009 (3) | 0.008 (3) |
O34 | 0.021 (3) | 0.010 (3) | 0.029 (3) | 0.002 (3) | −0.005 (2) | −0.008 (2) |
O35 | 0.047 (4) | 0.009 (3) | 0.032 (3) | −0.007 (3) | −0.005 (3) | 0.001 (3) |
O36 | 0.033 (4) | 0.038 (4) | 0.042 (4) | 0.019 (3) | −0.017 (3) | −0.006 (3) |
O37 | 0.052 (5) | 0.022 (3) | 0.027 (4) | −0.012 (3) | 0.021 (3) | −0.002 (3) |
O38 | 0.038 (4) | 0.017 (3) | 0.031 (3) | 0.008 (3) | 0.001 (3) | −0.009 (3) |
O39 | 0.041 (4) | 0.080 (4) | 0.015 (3) | −0.004 (4) | 0.003 (3) | 0.003 (4) |
O40 | 0.051 (4) | 0.028 (3) | 0.015 (3) | −0.012 (3) | 0.001 (4) | 0.000 (3) |
O41 | 0.050 (5) | 0.027 (4) | 0.020 (4) | 0.017 (3) | −0.013 (4) | 0.003 (3) |
O42 | 0.034 (4) | 0.034 (4) | 0.026 (3) | 0.011 (3) | 0.012 (3) | −0.003 (3) |
O43 | 0.026 (4) | 0.035 (4) | 0.020 (3) | 0.004 (3) | −0.009 (3) | 0.011 (3) |
O44 | 0.029 (3) | 0.022 (3) | 0.022 (3) | −0.010 (3) | −0.015 (3) | −0.003 (3) |
O45 | 0.039 (4) | 0.021 (3) | 0.027 (3) | −0.004 (3) | 0.011 (3) | 0.008 (3) |
O46 | 0.025 (4) | 0.066 (5) | 0.021 (3) | 0.002 (3) | −0.012 (3) | 0.008 (4) |
O47 | 0.022 (4) | 0.007 (3) | 0.029 (4) | −0.001 (2) | 0.003 (3) | 0.008 (3) |
O48 | 0.035 (4) | 0.012 (3) | 0.045 (4) | 0.005 (3) | 0.000 (4) | −0.005 (3) |
Geometric parameters (Å, º) top
C200—O202 | 1.1603 | Si14—O28 | 1.613 (6) |
C200—O201 | 1.1604 | Si14—O32 | 1.619 (6) |
O202—O202i | 1.24 (9) | Si15—O28 | 1.578 (6) |
C500—O502 | 1.1598 | Si15—O20iv | 1.588 (6) |
C500—O501 | 1.1598 | Si15—O19iv | 1.590 (7) |
Si1—O15 | 1.578 (7) | Si15—O29 | 1.597 (6) |
Si1—O1 | 1.591 (6) | Si16—O30 | 1.581 (6) |
Si1—O47ii | 1.586 (6) | Si16—O16iv | 1.586 (7) |
Si1—O16 | 1.605 (7) | Si16—O29 | 1.585 (7) |
Si2—O13 | 1.582 (6) | Si16—O17iv | 1.606 (6) |
Si2—O6 | 1.587 (6) | Si17—O40 | 1.591 (6) |
Si2—O1 | 1.581 (6) | Si17—O30 | 1.598 (6) |
Si2—O2 | 1.603 (6) | Si17—O47 | 1.601 (5) |
Si3—O3 | 1.585 (6) | Si17—O31 | 1.616 (6) |
Si3—O46 | 1.587 (6) | Si18—O31 | 1.585 (6) |
Si3—O45iii | 1.593 (7) | Si18—O32 | 1.581 (6) |
Si3—O2 | 1.596 (6) | Si18—O44 | 1.594 (6) |
Si4—O4 | 1.578 (7) | Si18—O45 | 1.606 (7) |
Si4—O43iii | 1.599 (7) | Si19—O33 | 1.575 (7) |
Si4—O42iii | 1.602 (7) | Si19—O23 | 1.587 (6) |
Si4—O3 | 1.606 (6) | Si19—O22ii | 1.595 (6) |
Si5—O5 | 1.588 (6) | Si19—O43 | 1.601 (7) |
Si5—O14 | 1.590 (6) | Si20—O34 | 1.581 (6) |
Si5—O21 | 1.591 (5) | Si20—O39 | 1.590 (6) |
Si5—O4 | 1.626 (6) | Si20—O33 | 1.592 (6) |
Si6—O6 | 1.590 (6) | Si20—O38 | 1.596 (6) |
Si6—O18 | 1.596 (6) | Si21—O18iv | 1.586 (6) |
Si6—O19 | 1.599 (7) | Si21—O35 | 1.597 (6) |
Si6—O5 | 1.600 (6) | Si21—O25 | 1.613 (6) |
Si7—O48ii | 1.591 (6) | Si21—O34 | 1.618 (6) |
Si7—O23 | 1.597 (6) | Si22—O15iv | 1.586 (7) |
Si7—O17 | 1.597 (6) | Si22—O36 | 1.601 (7) |
Si7—O7 | 1.597 (7) | Si22—O26 | 1.605 (6) |
Si8—O12 | 1.572 (6) | Si22—O35 | 1.605 (7) |
Si8—O7 | 1.591 (7) | Si23—O36 | 1.562 (7) |
Si8—O13 | 1.595 (6) | Si23—O40 | 1.599 (7) |
Si8—O8 | 1.608 (6) | Si23—O37 | 1.600 (7) |
Si9—O8 | 1.563 (6) | Si23—O48 | 1.592 (7) |
Si9—O25 | 1.583 (6) | Si24—O24 | 1.592 (6) |
Si9—O44iii | 1.595 (6) | Si24—O38 | 1.585 (6) |
Si9—O9 | 1.607 (7) | Si24—O37 | 1.586 (7) |
Si10—O9 | 1.587 (6) | Si24—O46v | 1.602 (6) |
Si10—O10 | 1.585 (7) | O15—Si22vi | 1.586 (7) |
Si10—O41iii | 1.596 (7) | O16—Si16vi | 1.586 (7) |
Si10—O26 | 1.602 (6) | O17—Si16vi | 1.606 (6) |
Si11—O10 | 1.586 (7) | O18—Si21vi | 1.586 (6) |
Si11—O14 | 1.597 (6) | O19—Si15vi | 1.590 (7) |
Si11—O22 | 1.589 (7) | O20—Si15vi | 1.588 (6) |
Si11—O11 | 1.599 (7) | O21—Si13vii | 1.597 (5) |
Si12—O11 | 1.568 (7) | O22—Si19vii | 1.595 (6) |
Si12—O24 | 1.596 (6) | O41—Si10v | 1.596 (7) |
Si12—O20 | 1.597 (6) | O42—Si4v | 1.602 (7) |
Si12—O12 | 1.599 (6) | O43—Si4v | 1.599 (7) |
Si13—O42 | 1.586 (7) | O44—Si9v | 1.595 (6) |
Si13—O27 | 1.595 (6) | O45—Si3v | 1.593 (7) |
Si13—O21ii | 1.597 (5) | O46—Si24iii | 1.602 (6) |
Si13—O41 | 1.609 (7) | O47—Si1vii | 1.586 (6) |
Si14—O27 | 1.586 (6) | O48—Si7vii | 1.591 (6) |
Si14—O39 | 1.597 (6) | | |
| | | |
O202—C200—O201 | 180.0 | O29—Si16—O17iv | 109.5 (3) |
C200—O202—O202i | 132 (8) | O40—Si17—O30 | 109.5 (4) |
O502—C500—O501 | 180 (3) | O40—Si17—O47 | 110.4 (3) |
O15—Si1—O1 | 109.0 (4) | O30—Si17—O47 | 108.5 (3) |
O15—Si1—O47ii | 110.6 (3) | O40—Si17—O31 | 108.9 (3) |
O1—Si1—O47ii | 107.3 (3) | O30—Si17—O31 | 110.1 (4) |
O15—Si1—O16 | 110.1 (4) | O47—Si17—O31 | 109.4 (4) |
O1—Si1—O16 | 109.6 (4) | O31—Si18—O32 | 110.1 (4) |
O47ii—Si1—O16 | 110.2 (3) | O31—Si18—O44 | 107.2 (3) |
O13—Si2—O6 | 108.5 (4) | O32—Si18—O44 | 109.6 (4) |
O13—Si2—O1 | 110.0 (4) | O31—Si18—O45 | 109.0 (3) |
O6—Si2—O1 | 111.6 (4) | O32—Si18—O45 | 110.6 (3) |
O13—Si2—O2 | 109.5 (3) | O44—Si18—O45 | 110.2 (4) |
O6—Si2—O2 | 109.8 (4) | O33—Si19—O23 | 110.6 (3) |
O1—Si2—O2 | 107.4 (3) | O33—Si19—O22ii | 107.6 (4) |
O3—Si3—O46 | 110.3 (4) | O23—Si19—O22ii | 109.9 (3) |
O3—Si3—O45iii | 108.9 (4) | O33—Si19—O43 | 110.5 (4) |
O46—Si3—O45iii | 109.0 (4) | O23—Si19—O43 | 107.6 (3) |
O3—Si3—O2 | 110.6 (3) | O22ii—Si19—O43 | 110.6 (4) |
O46—Si3—O2 | 108.7 (3) | O34—Si20—O39 | 111.3 (3) |
O45iii—Si3—O2 | 109.3 (3) | O34—Si20—O33 | 108.7 (3) |
O4—Si4—O43iii | 109.4 (3) | O39—Si20—O33 | 108.7 (4) |
O4—Si4—O42iii | 109.5 (3) | O34—Si20—O38 | 109.0 (3) |
O43iii—Si4—O42iii | 110.1 (4) | O39—Si20—O38 | 108.5 (4) |
O4—Si4—O3 | 110.2 (3) | O33—Si20—O38 | 110.6 (4) |
O43iii—Si4—O3 | 109.9 (3) | O18iv—Si21—O35 | 109.9 (3) |
O42iii—Si4—O3 | 107.7 (3) | O18iv—Si21—O25 | 107.0 (3) |
O5—Si5—O14 | 109.8 (3) | O35—Si21—O25 | 110.1 (3) |
O5—Si5—O21 | 106.9 (3) | O18iv—Si21—O34 | 110.1 (3) |
O14—Si5—O21 | 110.8 (3) | O35—Si21—O34 | 108.6 (3) |
O5—Si5—O4 | 110.2 (3) | O25—Si21—O34 | 111.2 (3) |
O14—Si5—O4 | 108.8 (3) | O15iv—Si22—O36 | 110.0 (4) |
O21—Si5—O4 | 110.3 (3) | O15iv—Si22—O26 | 108.3 (3) |
O6—Si6—O18 | 109.9 (4) | O36—Si22—O26 | 110.0 (3) |
O6—Si6—O19 | 110.8 (4) | O15iv—Si22—O35 | 109.3 (3) |
O18—Si6—O19 | 108.3 (4) | O36—Si22—O35 | 108.7 (4) |
O6—Si6—O5 | 109.0 (4) | O26—Si22—O35 | 110.5 (3) |
O18—Si6—O5 | 108.6 (3) | O36—Si23—O40 | 110.3 (4) |
O19—Si6—O5 | 110.1 (3) | O36—Si23—O37 | 111.3 (4) |
O48ii—Si7—O23 | 111.3 (3) | O40—Si23—O37 | 108.0 (3) |
O48ii—Si7—O17 | 110.1 (4) | O36—Si23—O48 | 108.7 (4) |
O23—Si7—O17 | 107.3 (3) | O40—Si23—O48 | 110.2 (3) |
O48ii—Si7—O7 | 108.1 (4) | O37—Si23—O48 | 108.3 (4) |
O23—Si7—O7 | 109.6 (3) | O24—Si24—O38 | 108.3 (3) |
O17—Si7—O7 | 110.5 (4) | O24—Si24—O37 | 109.6 (3) |
O12—Si8—O7 | 110.5 (4) | O38—Si24—O37 | 109.6 (4) |
O12—Si8—O13 | 108.6 (3) | O24—Si24—O46v | 108.0 (3) |
O7—Si8—O13 | 110.3 (4) | O38—Si24—O46v | 110.6 (4) |
O12—Si8—O8 | 110.7 (4) | O37—Si24—O46v | 110.8 (4) |
O7—Si8—O8 | 107.7 (4) | Si2—O1—Si1 | 145.8 (4) |
O13—Si8—O8 | 109.0 (3) | Si3—O2—Si2 | 145.7 (4) |
O8—Si9—O25 | 107.8 (3) | Si3—O3—Si4 | 160.3 (5) |
O8—Si9—O44iii | 110.5 (4) | Si4—O4—Si5 | 147.5 (4) |
O25—Si9—O44iii | 109.5 (3) | Si5—O5—Si6 | 147.7 (4) |
O8—Si9—O9 | 108.6 (4) | Si2—O6—Si6 | 162.6 (5) |
O25—Si9—O9 | 111.1 (3) | Si8—O7—Si7 | 157.8 (5) |
O44iii—Si9—O9 | 109.3 (3) | Si9—O8—Si8 | 152.8 (4) |
O9—Si10—O10 | 109.4 (4) | Si10—O9—Si9 | 151.1 (4) |
O9—Si10—O41iii | 109.6 (3) | Si10—O10—Si11 | 155.9 (4) |
O10—Si10—O41iii | 110.2 (4) | Si12—O11—Si11 | 156.2 (5) |
O9—Si10—O26 | 111.2 (3) | Si8—O12—Si12 | 168.1 (4) |
O10—Si10—O26 | 108.6 (3) | Si2—O13—Si8 | 161.4 (4) |
O41iii—Si10—O26 | 107.8 (3) | Si5—O14—Si11 | 159.5 (4) |
O10—Si11—O14 | 108.1 (4) | Si1—O15—Si22vi | 150.6 (4) |
O10—Si11—O22 | 109.1 (4) | Si16vi—O16—Si1 | 173.2 (5) |
O14—Si11—O22 | 110.4 (3) | Si7—O17—Si16vi | 145.6 (4) |
O10—Si11—O11 | 110.6 (4) | Si21vi—O18—Si6 | 141.4 (4) |
O14—Si11—O11 | 109.8 (3) | Si15vi—O19—Si6 | 167.4 (5) |
O22—Si11—O11 | 108.8 (4) | Si15vi—O20—Si12 | 143.2 (4) |
O11—Si12—O24 | 110.8 (3) | Si5—O21—Si13vii | 145.7 (4) |
O11—Si12—O20 | 110.0 (4) | Si19vii—O22—Si11 | 151.8 (5) |
O24—Si12—O20 | 106.9 (3) | Si19—O23—Si7 | 155.9 (3) |
O11—Si12—O12 | 108.6 (4) | Si24—O24—Si12 | 149.1 (3) |
O24—Si12—O12 | 112.0 (3) | Si9—O25—Si21 | 151.2 (3) |
O20—Si12—O12 | 108.6 (3) | Si10—O26—Si22 | 145.0 (3) |
O42—Si13—O27 | 110.2 (4) | Si14—O27—Si13 | 154.6 (5) |
O42—Si13—O21ii | 109.0 (3) | Si15—O28—Si14 | 148.8 (4) |
O27—Si13—O21ii | 110.0 (4) | Si16—O29—Si15 | 159.7 (4) |
O42—Si13—O41 | 109.3 (4) | Si16—O30—Si17 | 156.3 (4) |
O27—Si13—O41 | 110.6 (4) | Si18—O31—Si17 | 147.5 (4) |
O21ii—Si13—O41 | 107.6 (3) | Si18—O32—Si14 | 156.8 (5) |
O27—Si14—O39 | 110.3 (4) | Si19—O33—Si20 | 150.5 (5) |
O27—Si14—O28 | 108.5 (3) | Si20—O34—Si21 | 146.9 (4) |
O39—Si14—O28 | 111.2 (3) | Si21—O35—Si22 | 151.4 (4) |
O27—Si14—O32 | 108.3 (4) | Si23—O36—Si22 | 159.7 (5) |
O39—Si14—O32 | 109.2 (4) | Si24—O37—Si23 | 153.2 (4) |
O28—Si14—O32 | 109.2 (3) | Si24—O38—Si20 | 154.4 (4) |
O28—Si15—O20iv | 107.5 (3) | Si20—O39—Si14 | 165.0 (5) |
O28—Si15—O19iv | 110.1 (4) | Si17—O40—Si23 | 160.0 (4) |
O20iv—Si15—O19iv | 111.2 (3) | Si10v—O41—Si13 | 150.0 (4) |
O28—Si15—O29 | 108.9 (3) | Si13—O42—Si4v | 157.9 (5) |
O20iv—Si15—O29 | 110.0 (3) | Si4v—O43—Si19 | 150.5 (5) |
O19iv—Si15—O29 | 109.1 (3) | Si18—O44—Si9v | 150.7 (4) |
O30—Si16—O16iv | 110.1 (4) | Si3v—O45—Si18 | 153.4 (4) |
O30—Si16—O29 | 109.6 (3) | Si3—O46—Si24iii | 155.5 (5) |
O16iv—Si16—O29 | 110.4 (3) | Si1vii—O47—Si17 | 149.2 (4) |
O30—Si16—O17iv | 107.5 (4) | Si7vii—O48—Si23 | 148.3 (5) |
O16iv—Si16—O17iv | 109.7 (4) | | |
Symmetry codes: (i) −x+2, −y+1, −z+1; (ii) −x+1/2, y+1/2, −z+1/2; (iii) x−1/2, −y+1/2, z−1/2; (iv) x−1/2, −y+1/2, z+1/2; (v) x+1/2, −y+1/2, z+1/2; (vi) x+1/2, −y+1/2, z−1/2; (vii) −x+1/2, y−1/2, −z+1/2. |
(str3h6_2_twin_f_co2)
top
Crystal data top
C1.1O50.2Si24 | F(000) = 2968 |
Mr = 1491.1 | Dx = 1.854 Mg m−3 |
Monoclinic, P21/n | Mo Kα radiation, λ = 0.71073 Å |
a = 13.383 (3) Å | Cell parameters from 328 reflections |
b = 20.121 (4) Å | θ = 3.4–26.7° |
c = 19.881 (4) Å | µ = 0.68 mm−1 |
β = 90.057 (3)° | T = 296 K |
V = 5353.5 (19) Å3 | Coffin shape, colorless |
Z = 4 | 0.13 × 0.09 × 0.08 mm |
Data collection top
CCD area detector diffractometer | 12802 independent reflections |
Radiation source: fine-focus sealed tube | 6968 reflections with I > 2σ(I) |
Graphite monochromator | Rint = 0.130 |
phi and ω scans | θmax = 28.7°, θmin = 1.0° |
Absorption correction: analytical ? | h = −17→17 |
Tmin = 0.914, Tmax = 0.950 | k = −26→25 |
61855 measured reflections | l = −26→25 |
Refinement top
Refinement on F2 | 9 restraints |
Least-squares matrix: full | Primary atom site location: structure-invariant direct methods |
R[F2 > 2σ(F2)] = 0.074 | Secondary atom site location: difference Fourier map |
wR(F2) = 0.172 | w = 1/[σ2(Fo2) + (0.0712P)2] where P = (Fo2 + 2Fc2)/3 |
S = 0.99 | (Δ/σ)max = 0.001 |
12802 reflections | Δρmax = 0.88 e Å−3 |
672 parameters | Δρmin = −0.96 e Å−3 |
Crystal data top
C1.1O50.2Si24 | V = 5353.5 (19) Å3 |
Mr = 1491.1 | Z = 4 |
Monoclinic, P21/n | Mo Kα radiation |
a = 13.383 (3) Å | µ = 0.68 mm−1 |
b = 20.121 (4) Å | T = 296 K |
c = 19.881 (4) Å | 0.13 × 0.09 × 0.08 mm |
β = 90.057 (3)° | |
Data collection top
CCD area detector diffractometer | 12802 independent reflections |
Absorption correction: analytical ? | 6968 reflections with I > 2σ(I) |
Tmin = 0.914, Tmax = 0.950 | Rint = 0.130 |
61855 measured reflections | |
Refinement top
R[F2 > 2σ(F2)] = 0.074 | 672 parameters |
wR(F2) = 0.172 | 9 restraints |
S = 0.99 | Δρmax = 0.88 e Å−3 |
12802 reflections | Δρmin = −0.96 e Å−3 |
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 | x | y | z | Uiso*/Ueq | Occ. (<1) |
C100 | 0.521 (4) | 0.992 (2) | 0.5278 (18) | 0.24 (4)* | 0.202 (12) |
O101 | 0.515 (4) | 0.988 (2) | 0.4752 (18) | 0.13 (3)* | 0.202 (12) |
O102 | 0.527 (3) | 0.9948 (17) | 0.5804 (18) | 0.31 (5)* | 0.202 (12) |
C200 | 0.492 (2) | 0.9984 (15) | 0.9010 (18) | 0.25 (4)* | 0.37 (2) |
O201 | 0.476 (2) | 0.9815 (13) | 0.8460 (18) | 0.49 (5)* | 0.37 (2) |
O202 | 0.509 (3) | 1.0143 (18) | 0.9521 (18) | 0.40 (5)* | 0.37 (2) |
C300 | 0.146 (13) | 0.274 (3) | 0.731 (6) | 0.6 (2)* | 0.10 (3) |
O301 | 0.161 (12) | 0.329 (3) | 0.719 (6) | 0.6 (2)* | 0.10 (3) |
O302 | 0.130 (14) | 0.219 (3) | 0.744 (7) | 0.5 (2)* | 0.10 (3) |
C400 | 0.4845 (18) | 1.0015 (11) | 0.7135 (18) | 0.50 (7)* | 0.44 (3) |
O401 | 0.470 (2) | 1.0248 (13) | 0.6608 (18) | 0.61 (7)* | 0.44 (3) |
O402 | 0.4985 (17) | 0.9781 (11) | 0.7661 (18) | 0.56 (5)* | 0.44 (3) |
Si1 | 0.32304 (17) | 0.42065 (10) | −0.05565 (12) | 0.0125 (5) | |
Si2 | 0.16829 (18) | 0.31273 (10) | −0.03048 (11) | 0.0138 (5) | |
Si3 | −0.04921 (18) | 0.27971 (10) | −0.06254 (12) | 0.0146 (5) | |
Si4 | −0.03518 (17) | 0.12373 (10) | −0.06306 (11) | 0.0123 (5) | |
Si5 | 0.17775 (19) | 0.07632 (10) | −0.02817 (10) | 0.0119 (5) | |
Si6 | 0.31626 (17) | 0.19419 (10) | −0.05606 (12) | 0.0134 (5) | |
Si7 | 0.32045 (19) | 0.42505 (10) | 0.17166 (11) | 0.0129 (5) | |
Si8 | 0.17627 (18) | 0.31107 (11) | 0.12696 (11) | 0.0143 (5) | |
Si9 | −0.03488 (18) | 0.27326 (10) | 0.17568 (11) | 0.0130 (5) | |
Si10 | −0.03267 (19) | 0.11925 (10) | 0.17569 (11) | 0.0140 (5) | |
Si11 | 0.17731 (18) | 0.07115 (10) | 0.12929 (11) | 0.0132 (5) | |
Si12 | 0.31558 (19) | 0.18974 (11) | 0.16622 (11) | 0.0145 (5) | |
Si13 | 0.33555 (17) | 0.42790 (9) | 0.55746 (13) | 0.0125 (5) | |
Si14 | 0.18933 (18) | 0.31173 (11) | 0.52748 (11) | 0.0143 (5) | |
Si15 | −0.02893 (17) | 0.27770 (10) | 0.56129 (12) | 0.0132 (5) | |
Si16 | −0.03248 (17) | 0.12170 (10) | 0.56385 (12) | 0.0134 (5) | |
Si17 | 0.17997 (19) | 0.07064 (10) | 0.52735 (10) | 0.0120 (5) | |
Si18 | 0.31980 (18) | 0.18660 (10) | 0.56218 (12) | 0.0140 (5) | |
Si19 | 0.31630 (19) | 0.42364 (10) | 0.32804 (11) | 0.0137 (5) | |
Si20 | 0.17166 (18) | 0.31180 (10) | 0.36903 (12) | 0.0146 (5) | |
Si21 | −0.04307 (18) | 0.27330 (10) | 0.33094 (11) | 0.0140 (5) | |
Si22 | −0.03630 (19) | 0.11888 (10) | 0.32951 (11) | 0.0139 (5) | |
Si23 | 0.17839 (19) | 0.07201 (9) | 0.36948 (11) | 0.0131 (5) | |
Si24 | 0.30154 (18) | 0.19307 (10) | 0.32018 (10) | 0.0129 (5) | |
O1 | 0.2244 (4) | 0.3768 (3) | −0.0580 (3) | 0.0302 (15) | |
O2 | 0.0605 (4) | 0.3094 (3) | −0.0655 (3) | 0.0233 (13) | |
O3 | −0.0450 (5) | 0.2016 (3) | −0.0490 (3) | 0.0375 (16) | |
O4 | 0.0799 (4) | 0.1038 (3) | −0.0675 (3) | 0.0247 (14) | |
O5 | 0.2723 (4) | 0.1211 (2) | −0.0461 (3) | 0.0221 (14) | |
O6 | 0.2280 (5) | 0.2469 (3) | −0.0463 (3) | 0.0357 (16) | |
O7 | 0.2304 (5) | 0.3761 (3) | 0.1545 (3) | 0.0341 (18) | |
O8 | 0.0716 (4) | 0.3044 (3) | 0.1659 (3) | 0.0311 (15) | |
O9 | −0.0306 (5) | 0.1960 (3) | 0.1561 (3) | 0.0277 (16) | |
O10 | 0.0783 (5) | 0.0894 (3) | 0.1687 (3) | 0.0286 (15) | |
O11 | 0.2660 (5) | 0.1205 (3) | 0.1514 (3) | 0.0307 (17) | |
O12 | 0.2439 (5) | 0.2475 (3) | 0.1391 (3) | 0.0334 (16) | |
O13 | 0.1549 (5) | 0.3181 (3) | 0.0489 (3) | 0.0400 (17) | |
O14 | 0.1561 (4) | 0.0781 (3) | 0.0510 (3) | 0.0277 (14) | |
O15 | 0.3781 (5) | 0.4147 (3) | −0.1254 (3) | 0.0317 (16) | |
O16 | 0.3927 (5) | 0.3943 (3) | 0.0044 (3) | 0.0355 (17) | |
O17 | 0.4202 (4) | 0.4018 (3) | 0.1342 (3) | 0.0250 (14) | |
O18 | 0.3627 (4) | 0.1987 (3) | −0.1300 (3) | 0.0240 (13) | |
O19 | 0.4038 (5) | 0.2079 (3) | −0.0028 (3) | 0.0339 (16) | |
O20 | 0.4200 (4) | 0.1955 (3) | 0.1280 (3) | 0.0259 (14) | |
O21 | 0.2044 (4) | 0.0028 (2) | −0.0517 (3) | 0.0210 (13) | |
O22 | 0.2086 (5) | −0.0030 (3) | 0.1477 (3) | 0.0266 (15) | |
O23 | 0.3438 (4) | 0.4238 (2) | 0.2506 (3) | 0.0293 (13) | |
O24 | 0.3394 (4) | 0.1977 (2) | 0.2447 (3) | 0.0251 (12) | |
O25 | −0.0648 (4) | 0.2823 (2) | 0.2527 (3) | 0.0214 (12) | |
O26 | −0.0671 (3) | 0.1099 (2) | 0.2527 (3) | 0.0216 (12) | |
O27 | 0.2433 (4) | 0.3776 (3) | 0.5517 (4) | 0.0348 (16) | |
O28 | 0.0757 (4) | 0.3139 (2) | 0.5535 (3) | 0.0253 (13) | |
O29 | −0.0105 (5) | 0.1993 (3) | 0.5669 (3) | 0.0352 (16) | |
O30 | 0.0688 (4) | 0.0832 (3) | 0.5546 (3) | 0.0306 (15) | |
O31 | 0.2564 (4) | 0.1200 (3) | 0.5648 (3) | 0.0236 (14) | |
O32 | 0.2466 (4) | 0.2493 (3) | 0.5598 (3) | 0.0292 (15) | |
O33 | 0.2204 (5) | 0.3782 (3) | 0.3416 (3) | 0.0288 (16) | |
O34 | 0.0547 (4) | 0.3140 (2) | 0.3546 (3) | 0.0217 (14) | |
O35 | −0.0256 (5) | 0.1960 (3) | 0.3479 (3) | 0.0253 (15) | |
O36 | 0.0668 (5) | 0.0836 (3) | 0.3433 (3) | 0.0368 (17) | |
O37 | 0.2535 (5) | 0.1220 (3) | 0.3336 (3) | 0.0318 (17) | |
O38 | 0.2196 (5) | 0.2485 (3) | 0.3321 (3) | 0.0306 (15) | |
O39 | 0.1928 (5) | 0.3059 (3) | 0.4480 (3) | 0.0434 (17) | |
O40 | 0.1832 (5) | 0.0845 (3) | 0.4486 (3) | 0.0317 (15) | |
O41 | 0.3903 (5) | 0.4187 (3) | 0.6288 (3) | 0.0297 (16) | |
O42 | 0.4139 (4) | 0.4148 (3) | 0.4986 (3) | 0.0229 (14) | |
O43 | 0.4106 (5) | 0.3951 (3) | 0.3683 (3) | 0.0260 (15) | |
O44 | 0.3854 (4) | 0.1896 (3) | 0.6296 (3) | 0.0241 (14) | |
O45 | 0.3905 (5) | 0.1861 (3) | 0.4971 (3) | 0.0269 (15) | |
O46 | −0.1041 (5) | 0.2947 (3) | −0.1323 (3) | 0.0377 (17) | |
O47 | 0.2089 (4) | −0.0049 (2) | 0.5441 (3) | 0.0215 (14) | |
O48 | 0.2115 (5) | −0.0017 (3) | 0.3526 (3) | 0.0282 (16) | |
Atomic displacement parameters (Å2) top | U11 | U22 | U33 | U12 | U13 | U23 |
Si1 | 0.0190 (12) | 0.0079 (9) | 0.0106 (10) | 0.0001 (9) | 0.0041 (11) | −0.0001 (9) |
Si2 | 0.0198 (13) | 0.0076 (10) | 0.0141 (10) | −0.0017 (10) | 0.0001 (9) | −0.0005 (8) |
Si3 | 0.0202 (13) | 0.0136 (10) | 0.0101 (11) | 0.0016 (9) | 0.0007 (10) | −0.0031 (9) |
Si4 | 0.0164 (13) | 0.0089 (10) | 0.0116 (12) | 0.0000 (9) | 0.0007 (11) | 0.0014 (9) |
Si5 | 0.0168 (13) | 0.0083 (10) | 0.0105 (11) | −0.0020 (10) | 0.0021 (10) | 0.0010 (8) |
Si6 | 0.0198 (12) | 0.0084 (9) | 0.0122 (10) | −0.0038 (9) | 0.0040 (11) | −0.0004 (10) |
Si7 | 0.0210 (13) | 0.0081 (10) | 0.0096 (11) | −0.0005 (10) | 0.0057 (11) | −0.0010 (8) |
Si8 | 0.0170 (12) | 0.0146 (10) | 0.0114 (10) | −0.0035 (10) | 0.0007 (11) | −0.0005 (10) |
Si9 | 0.0185 (14) | 0.0134 (10) | 0.0073 (11) | −0.0003 (9) | 0.0027 (10) | 0.0031 (8) |
Si10 | 0.0222 (14) | 0.0128 (11) | 0.0070 (11) | −0.0002 (10) | 0.0016 (11) | −0.0001 (9) |
Si11 | 0.0196 (13) | 0.0106 (10) | 0.0094 (11) | −0.0019 (10) | 0.0062 (12) | −0.0009 (9) |
Si12 | 0.0217 (12) | 0.0133 (10) | 0.0085 (10) | −0.0020 (10) | 0.0021 (10) | 0.0000 (9) |
Si13 | 0.0192 (13) | 0.0083 (9) | 0.0102 (10) | 0.0013 (9) | 0.0022 (11) | −0.0009 (9) |
Si14 | 0.0184 (13) | 0.0124 (11) | 0.0120 (10) | 0.0001 (10) | 0.0041 (9) | 0.0012 (9) |
Si15 | 0.0191 (13) | 0.0107 (9) | 0.0098 (11) | 0.0008 (9) | 0.0044 (11) | 0.0003 (9) |
Si16 | 0.0161 (13) | 0.0127 (10) | 0.0114 (12) | −0.0002 (9) | 0.0026 (11) | 0.0020 (9) |
Si17 | 0.0186 (14) | 0.0069 (10) | 0.0106 (11) | −0.0007 (9) | 0.0038 (10) | −0.0004 (8) |
Si18 | 0.0200 (13) | 0.0090 (9) | 0.0131 (11) | −0.0026 (9) | −0.0001 (10) | 0.0007 (9) |
Si19 | 0.0203 (14) | 0.0113 (10) | 0.0095 (11) | −0.0013 (10) | 0.0032 (11) | 0.0004 (8) |
Si20 | 0.0200 (13) | 0.0120 (10) | 0.0117 (10) | −0.0014 (10) | 0.0041 (10) | 0.0000 (10) |
Si21 | 0.0218 (14) | 0.0108 (10) | 0.0095 (11) | 0.0012 (9) | 0.0029 (11) | −0.0015 (8) |
Si22 | 0.0218 (14) | 0.0107 (10) | 0.0091 (11) | 0.0004 (10) | 0.0014 (11) | 0.0036 (9) |
Si23 | 0.0212 (13) | 0.0070 (10) | 0.0113 (11) | 0.0028 (9) | 0.0040 (12) | 0.0001 (9) |
Si24 | 0.0202 (13) | 0.0094 (9) | 0.0092 (10) | 0.0009 (10) | 0.0046 (9) | −0.0010 (8) |
O1 | 0.033 (4) | 0.018 (3) | 0.039 (4) | −0.006 (3) | −0.003 (4) | 0.011 (3) |
O2 | 0.019 (3) | 0.023 (3) | 0.028 (3) | −0.008 (3) | 0.002 (3) | 0.004 (3) |
O3 | 0.052 (4) | 0.011 (3) | 0.050 (4) | −0.003 (3) | 0.009 (4) | −0.003 (3) |
O4 | 0.024 (3) | 0.031 (3) | 0.019 (3) | 0.005 (3) | 0.005 (3) | 0.006 (3) |
O5 | 0.018 (3) | 0.012 (3) | 0.036 (4) | −0.007 (2) | 0.009 (3) | 0.001 (3) |
O6 | 0.035 (4) | 0.019 (3) | 0.053 (4) | 0.007 (3) | 0.009 (4) | −0.011 (3) |
O7 | 0.033 (4) | 0.018 (3) | 0.051 (4) | −0.023 (3) | 0.002 (3) | −0.008 (3) |
O8 | 0.022 (4) | 0.036 (3) | 0.036 (3) | −0.005 (3) | 0.016 (3) | −0.007 (3) |
O9 | 0.056 (5) | 0.007 (3) | 0.021 (3) | 0.003 (3) | 0.004 (3) | 0.000 (2) |
O10 | 0.019 (3) | 0.040 (4) | 0.027 (3) | 0.010 (3) | 0.011 (3) | 0.006 (3) |
O11 | 0.025 (4) | 0.022 (3) | 0.044 (4) | −0.007 (3) | −0.007 (3) | −0.008 (3) |
O12 | 0.037 (4) | 0.021 (3) | 0.042 (4) | 0.015 (3) | −0.006 (3) | 0.003 (3) |
O13 | 0.054 (5) | 0.056 (4) | 0.011 (3) | 0.007 (3) | 0.004 (3) | −0.006 (3) |
O14 | 0.035 (4) | 0.037 (3) | 0.011 (3) | 0.004 (3) | 0.000 (3) | −0.002 (3) |
O15 | 0.041 (4) | 0.039 (4) | 0.016 (3) | 0.012 (3) | 0.016 (3) | 0.000 (3) |
O16 | 0.045 (4) | 0.044 (4) | 0.018 (3) | 0.016 (3) | −0.010 (3) | 0.003 (3) |
O17 | 0.019 (3) | 0.039 (4) | 0.017 (3) | 0.006 (3) | 0.013 (3) | −0.006 (3) |
O18 | 0.017 (3) | 0.039 (3) | 0.016 (3) | −0.003 (3) | 0.007 (3) | 0.003 (3) |
O19 | 0.033 (4) | 0.048 (4) | 0.020 (3) | −0.015 (3) | −0.010 (3) | −0.003 (3) |
O20 | 0.020 (3) | 0.036 (3) | 0.022 (3) | 0.001 (3) | 0.013 (3) | 0.005 (3) |
O21 | 0.026 (4) | 0.008 (2) | 0.029 (3) | −0.002 (2) | 0.014 (3) | 0.002 (3) |
O22 | 0.030 (4) | 0.016 (3) | 0.034 (4) | −0.003 (3) | 0.004 (3) | 0.004 (3) |
O23 | 0.042 (4) | 0.041 (3) | 0.006 (2) | 0.006 (3) | 0.011 (3) | 0.003 (3) |
O24 | 0.036 (3) | 0.034 (3) | 0.005 (2) | −0.007 (3) | 0.010 (3) | 0.002 (3) |
O25 | 0.030 (3) | 0.023 (2) | 0.011 (2) | 0.005 (2) | 0.005 (3) | 0.004 (3) |
O26 | 0.026 (3) | 0.033 (3) | 0.006 (2) | −0.004 (2) | 0.005 (3) | −0.004 (3) |
O27 | 0.022 (4) | 0.021 (3) | 0.062 (4) | −0.011 (3) | −0.005 (4) | −0.003 (3) |
O28 | 0.015 (3) | 0.021 (3) | 0.040 (3) | 0.000 (2) | 0.010 (3) | −0.004 (3) |
O29 | 0.050 (4) | 0.013 (3) | 0.042 (4) | −0.003 (3) | −0.001 (3) | 0.003 (3) |
O30 | 0.012 (3) | 0.026 (3) | 0.054 (4) | 0.006 (3) | 0.012 (3) | 0.002 (3) |
O31 | 0.035 (4) | 0.022 (3) | 0.014 (3) | −0.014 (3) | −0.002 (3) | 0.007 (2) |
O32 | 0.036 (4) | 0.020 (3) | 0.032 (3) | 0.012 (3) | 0.004 (3) | 0.006 (3) |
O33 | 0.024 (4) | 0.015 (3) | 0.047 (4) | −0.010 (3) | 0.011 (3) | 0.004 (3) |
O34 | 0.019 (3) | 0.010 (3) | 0.036 (4) | 0.000 (2) | −0.001 (3) | −0.004 (2) |
O35 | 0.041 (4) | 0.014 (3) | 0.021 (3) | −0.004 (3) | −0.003 (3) | −0.002 (3) |
O36 | 0.026 (4) | 0.037 (4) | 0.047 (4) | 0.020 (3) | −0.009 (3) | −0.009 (3) |
O37 | 0.051 (5) | 0.016 (3) | 0.029 (3) | −0.013 (3) | 0.024 (3) | 0.000 (3) |
O38 | 0.032 (4) | 0.022 (3) | 0.039 (4) | 0.008 (3) | 0.006 (3) | −0.011 (3) |
O39 | 0.043 (4) | 0.073 (4) | 0.015 (3) | 0.001 (4) | 0.007 (3) | 0.004 (3) |
O40 | 0.055 (4) | 0.026 (3) | 0.014 (3) | −0.004 (3) | −0.005 (3) | 0.000 (3) |
O41 | 0.039 (4) | 0.026 (3) | 0.024 (3) | 0.014 (3) | −0.010 (3) | −0.001 (3) |
O42 | 0.019 (3) | 0.027 (3) | 0.023 (3) | 0.004 (3) | 0.014 (3) | −0.007 (3) |
O43 | 0.028 (4) | 0.037 (3) | 0.013 (3) | 0.008 (3) | −0.002 (3) | 0.004 (3) |
O44 | 0.032 (4) | 0.023 (3) | 0.017 (3) | −0.008 (3) | −0.010 (3) | 0.001 (3) |
O45 | 0.036 (4) | 0.021 (3) | 0.024 (3) | −0.004 (3) | 0.014 (3) | 0.006 (3) |
O46 | 0.035 (4) | 0.064 (5) | 0.014 (3) | 0.004 (3) | −0.016 (3) | 0.009 (3) |
O47 | 0.020 (3) | 0.009 (3) | 0.035 (4) | −0.004 (2) | 0.007 (3) | 0.007 (2) |
O48 | 0.032 (4) | 0.011 (3) | 0.042 (4) | 0.001 (3) | 0.000 (3) | −0.007 (3) |
Geometric parameters (Å, º) top
C100—O101i | 0.63 (9) | Si13—O27 | 1.599 (6) |
C100—O101 | 1.0478 | Si13—O41 | 1.600 (7) |
C100—O102 | 1.0480 | Si13—O21ii | 1.602 (6) |
C100—C100i | 1.28 (8) | Si14—O27 | 1.580 (6) |
O101—C100i | 0.63 (9) | Si14—O39 | 1.581 (7) |
O101—O101i | 1.16 (7) | Si14—O32 | 1.601 (6) |
O101—O102i | 1.28 (9) | Si14—O28 | 1.607 (6) |
O102—O101i | 1.28 (8) | Si15—O19iv | 1.579 (6) |
C200—O202 | 1.0843 | Si15—O28 | 1.585 (6) |
C200—O201 | 1.1606 | Si15—O20iv | 1.586 (6) |
C300—O302 | 1.1596 | Si15—O29 | 1.599 (6) |
C300—O301 | 1.1596 | Si16—O30 | 1.571 (6) |
C400—O401 | 1.1594 | Si16—O16iv | 1.574 (7) |
C400—O402 | 1.1596 | Si16—O29 | 1.588 (6) |
Si1—O47ii | 1.574 (6) | Si16—O17iv | 1.606 (6) |
Si1—O15 | 1.575 (6) | Si17—O40 | 1.588 (7) |
Si1—O1 | 1.586 (6) | Si17—O47 | 1.601 (6) |
Si1—O16 | 1.597 (6) | Si17—O30 | 1.603 (6) |
Si2—O6 | 1.577 (6) | Si17—O31 | 1.604 (6) |
Si2—O1 | 1.588 (6) | Si18—O31 | 1.585 (6) |
Si2—O13 | 1.589 (7) | Si18—O44 | 1.603 (6) |
Si2—O2 | 1.597 (6) | Si18—O32 | 1.597 (6) |
Si3—O2 | 1.583 (6) | Si18—O45 | 1.604 (6) |
Si3—O45iii | 1.590 (6) | Si19—O23 | 1.581 (7) |
Si3—O46 | 1.592 (6) | Si19—O22ii | 1.587 (6) |
Si3—O3 | 1.593 (6) | Si19—O43 | 1.594 (7) |
Si4—O43iii | 1.584 (6) | Si19—O33 | 1.598 (6) |
Si4—O4 | 1.591 (7) | Si20—O33 | 1.582 (6) |
Si4—O3 | 1.596 (6) | Si20—O34 | 1.588 (7) |
Si4—O42iii | 1.602 (6) | Si20—O39 | 1.595 (7) |
Si5—O21 | 1.590 (6) | Si20—O38 | 1.603 (6) |
Si5—O5 | 1.592 (6) | Si21—O18iv | 1.586 (6) |
Si5—O14 | 1.598 (7) | Si21—O25 | 1.587 (7) |
Si5—O4 | 1.616 (6) | Si21—O35 | 1.606 (6) |
Si6—O5 | 1.595 (6) | Si21—O34 | 1.608 (6) |
Si6—O19 | 1.596 (7) | Si22—O36 | 1.572 (7) |
Si6—O18 | 1.597 (7) | Si22—O26 | 1.587 (7) |
Si6—O6 | 1.598 (6) | Si22—O35 | 1.599 (6) |
Si7—O7 | 1.590 (6) | Si22—O15iv | 1.605 (6) |
Si7—O23 | 1.594 (7) | Si23—O48 | 1.583 (6) |
Si7—O17 | 1.599 (6) | Si23—O40 | 1.589 (7) |
Si7—O48ii | 1.606 (6) | Si23—O37 | 1.591 (6) |
Si8—O13 | 1.579 (7) | Si23—O36 | 1.593 (7) |
Si8—O12 | 1.582 (6) | Si24—O38 | 1.581 (6) |
Si8—O7 | 1.589 (6) | Si24—O24 | 1.585 (6) |
Si8—O8 | 1.607 (6) | Si24—O46v | 1.588 (7) |
Si9—O8 | 1.567 (7) | Si24—O37 | 1.589 (6) |
Si9—O44iii | 1.586 (6) | O15—Si22vi | 1.605 (6) |
Si9—O25 | 1.592 (6) | O16—Si16vi | 1.574 (7) |
Si9—O9 | 1.601 (6) | O17—Si16vi | 1.606 (6) |
Si10—O41iii | 1.580 (6) | O18—Si21vi | 1.586 (6) |
Si10—O9 | 1.592 (6) | O19—Si15vi | 1.579 (6) |
Si10—O10 | 1.607 (7) | O20—Si15vi | 1.586 (6) |
Si10—O26 | 1.607 (7) | O21—Si13vii | 1.602 (6) |
Si11—O10 | 1.583 (7) | O22—Si19vii | 1.587 (6) |
Si11—O14 | 1.584 (7) | O41—Si10v | 1.580 (6) |
Si11—O22 | 1.589 (6) | O42—Si4v | 1.602 (6) |
Si11—O11 | 1.604 (7) | O43—Si4v | 1.584 (6) |
Si12—O11 | 1.569 (7) | O44—Si9v | 1.586 (6) |
Si12—O20 | 1.596 (6) | O45—Si3v | 1.590 (6) |
Si12—O24 | 1.596 (6) | O46—Si24iii | 1.588 (7) |
Si12—O12 | 1.596 (6) | O47—Si1vii | 1.574 (6) |
Si13—O42 | 1.594 (6) | O48—Si7vii | 1.606 (6) |
| | | |
O101i—C100—O101 | 84 (6) | O28—Si15—O29 | 108.9 (3) |
O101i—C100—O102 | 96 (6) | O20iv—Si15—O29 | 110.1 (3) |
O101—C100—O102 | 180 (10) | O30—Si16—O16iv | 110.8 (4) |
O101i—C100—C100i | 55 (6) | O30—Si16—O29 | 109.2 (3) |
O101—C100—C100i | 29 (4) | O16iv—Si16—O29 | 110.2 (3) |
O102—C100—C100i | 151 (4) | O30—Si16—O17iv | 107.5 (4) |
C100i—O101—C100 | 96 (6) | O16iv—Si16—O17iv | 109.8 (4) |
C100i—O101—O101i | 64 (6) | O29—Si16—O17iv | 109.2 (3) |
C100—O101—O101i | 32 (4) | O40—Si17—O47 | 111.2 (3) |
C100i—O101—O102i | 55 (6) | O40—Si17—O30 | 109.5 (4) |
C100—O101—O102i | 151 (5) | O47—Si17—O30 | 107.6 (3) |
O101i—O101—O102i | 118 (8) | O40—Si17—O31 | 109.0 (3) |
C100—O102—O101i | 29 (4) | O47—Si17—O31 | 109.8 (3) |
O202—C200—O201 | 178.9 (3) | O30—Si17—O31 | 109.6 (3) |
O302—C300—O301 | 180.0 | O31—Si18—O44 | 107.2 (3) |
O401—C400—O402 | 180 (5) | O31—Si18—O32 | 109.9 (4) |
O47ii—Si1—O15 | 109.2 (3) | O44—Si18—O32 | 109.2 (3) |
O47ii—Si1—O1 | 107.9 (3) | O31—Si18—O45 | 109.8 (3) |
O15—Si1—O1 | 108.9 (4) | O44—Si18—O45 | 110.6 (4) |
O47ii—Si1—O16 | 111.3 (3) | O32—Si18—O45 | 110.2 (3) |
O15—Si1—O16 | 110.9 (4) | O23—Si19—O22ii | 110.1 (3) |
O1—Si1—O16 | 108.5 (4) | O23—Si19—O43 | 107.4 (3) |
O6—Si2—O1 | 111.8 (4) | O22ii—Si19—O43 | 110.4 (3) |
O6—Si2—O13 | 108.3 (4) | O23—Si19—O33 | 110.8 (3) |
O1—Si2—O13 | 109.9 (4) | O22ii—Si19—O33 | 108.1 (4) |
O6—Si2—O2 | 109.5 (3) | O43—Si19—O33 | 110.0 (4) |
O1—Si2—O2 | 108.1 (3) | O33—Si20—O34 | 108.8 (3) |
O13—Si2—O2 | 109.1 (4) | O33—Si20—O39 | 109.2 (4) |
O2—Si3—O45iii | 109.7 (3) | O34—Si20—O39 | 110.3 (3) |
O2—Si3—O46 | 108.6 (3) | O33—Si20—O38 | 110.3 (4) |
O45iii—Si3—O46 | 109.4 (4) | O34—Si20—O38 | 109.6 (3) |
O2—Si3—O3 | 110.2 (3) | O39—Si20—O38 | 108.7 (4) |
O45iii—Si3—O3 | 108.6 (3) | O18iv—Si21—O25 | 107.2 (3) |
O46—Si3—O3 | 110.4 (4) | O18iv—Si21—O35 | 110.8 (3) |
O43iii—Si4—O4 | 109.2 (3) | O25—Si21—O35 | 109.9 (3) |
O43iii—Si4—O3 | 110.3 (3) | O18iv—Si21—O34 | 108.8 (3) |
O4—Si4—O3 | 109.7 (3) | O25—Si21—O34 | 111.8 (3) |
O43iii—Si4—O42iii | 110.3 (3) | O35—Si21—O34 | 108.2 (3) |
O4—Si4—O42iii | 109.6 (3) | O36—Si22—O26 | 109.8 (3) |
O3—Si4—O42iii | 107.8 (3) | O36—Si22—O35 | 108.7 (4) |
O21—Si5—O5 | 106.3 (3) | O26—Si22—O35 | 110.6 (3) |
O21—Si5—O14 | 110.6 (3) | O36—Si22—O15iv | 109.9 (4) |
O5—Si5—O14 | 110.8 (3) | O26—Si22—O15iv | 107.8 (3) |
O21—Si5—O4 | 111.0 (3) | O35—Si22—O15iv | 110.1 (3) |
O5—Si5—O4 | 109.9 (3) | O48—Si23—O40 | 110.3 (3) |
O14—Si5—O4 | 108.4 (3) | O48—Si23—O37 | 108.6 (4) |
O5—Si6—O19 | 110.2 (3) | O40—Si23—O37 | 108.7 (3) |
O5—Si6—O18 | 108.1 (3) | O48—Si23—O36 | 109.3 (4) |
O19—Si6—O18 | 108.1 (4) | O40—Si23—O36 | 109.3 (3) |
O5—Si6—O6 | 108.9 (4) | O37—Si23—O36 | 110.7 (4) |
O19—Si6—O6 | 110.1 (4) | O38—Si24—O24 | 109.0 (3) |
O18—Si6—O6 | 111.3 (4) | O38—Si24—O46v | 110.5 (4) |
O7—Si7—O23 | 110.1 (3) | O24—Si24—O46v | 107.1 (4) |
O7—Si7—O17 | 110.6 (4) | O38—Si24—O37 | 109.1 (4) |
O23—Si7—O17 | 107.0 (3) | O24—Si24—O37 | 110.0 (3) |
O7—Si7—O48ii | 107.7 (4) | O46v—Si24—O37 | 111.1 (4) |
O23—Si7—O48ii | 111.1 (3) | Si1—O1—Si2 | 146.5 (4) |
O17—Si7—O48ii | 110.4 (3) | Si3—O2—Si2 | 146.3 (4) |
O13—Si8—O12 | 108.8 (3) | Si3—O3—Si4 | 160.1 (5) |
O13—Si8—O7 | 110.0 (4) | Si4—O4—Si5 | 147.0 (4) |
O12—Si8—O7 | 110.7 (4) | Si5—O5—Si6 | 147.3 (4) |
O13—Si8—O8 | 109.0 (4) | Si2—O6—Si6 | 162.7 (5) |
O12—Si8—O8 | 110.9 (3) | Si8—O7—Si7 | 157.7 (5) |
O7—Si8—O8 | 107.4 (3) | Si9—O8—Si8 | 152.4 (4) |
O8—Si9—O44iii | 110.3 (4) | Si10—O9—Si9 | 151.6 (4) |
O8—Si9—O25 | 107.9 (3) | Si11—O10—Si10 | 154.6 (4) |
O44iii—Si9—O25 | 109.1 (3) | Si12—O11—Si11 | 155.5 (5) |
O8—Si9—O9 | 108.9 (4) | Si8—O12—Si12 | 168.4 (4) |
O44iii—Si9—O9 | 110.0 (3) | Si8—O13—Si2 | 160.8 (5) |
O25—Si9—O9 | 110.7 (3) | Si11—O14—Si5 | 158.3 (4) |
O41iii—Si10—O9 | 109.7 (3) | Si1—O15—Si22vi | 149.2 (4) |
O41iii—Si10—O10 | 111.5 (4) | Si16vi—O16—Si1 | 172.1 (5) |
O9—Si10—O10 | 108.9 (3) | Si7—O17—Si16vi | 145.4 (4) |
O41iii—Si10—O26 | 108.3 (3) | Si21vi—O18—Si6 | 141.5 (4) |
O9—Si10—O26 | 110.5 (3) | Si15vi—O19—Si6 | 167.5 (5) |
O10—Si10—O26 | 107.9 (3) | Si15vi—O20—Si12 | 143.4 (4) |
O10—Si11—O14 | 108.5 (3) | Si5—O21—Si13vii | 145.1 (4) |
O10—Si11—O22 | 108.8 (3) | Si19vii—O22—Si11 | 152.3 (5) |
O14—Si11—O22 | 110.7 (3) | Si19—O23—Si7 | 155.3 (4) |
O10—Si11—O11 | 109.9 (4) | Si24—O24—Si12 | 148.5 (4) |
O14—Si11—O11 | 110.0 (3) | Si21—O25—Si9 | 151.6 (4) |
O22—Si11—O11 | 108.9 (4) | Si22—O26—Si10 | 145.6 (3) |
O11—Si12—O20 | 110.2 (3) | Si14—O27—Si13 | 154.5 (5) |
O11—Si12—O24 | 110.7 (3) | Si15—O28—Si14 | 148.7 (4) |
O20—Si12—O24 | 106.6 (3) | Si16—O29—Si15 | 159.6 (5) |
O11—Si12—O12 | 109.3 (4) | Si16—O30—Si17 | 156.5 (4) |
O20—Si12—O12 | 108.2 (3) | Si18—O31—Si17 | 147.9 (4) |
O24—Si12—O12 | 111.8 (3) | Si18—O32—Si14 | 157.2 (4) |
O42—Si13—O27 | 110.6 (4) | Si20—O33—Si19 | 150.7 (5) |
O42—Si13—O41 | 109.3 (4) | Si20—O34—Si21 | 146.7 (4) |
O27—Si13—O41 | 109.8 (4) | Si22—O35—Si21 | 151.3 (4) |
O42—Si13—O21ii | 108.9 (3) | Si22—O36—Si23 | 160.1 (5) |
O27—Si13—O21ii | 109.5 (3) | Si24—O37—Si23 | 154.0 (4) |
O41—Si13—O21ii | 108.8 (3) | Si24—O38—Si20 | 155.0 (4) |
O27—Si14—O39 | 110.4 (4) | Si14—O39—Si20 | 165.4 (5) |
O27—Si14—O32 | 108.6 (4) | Si17—O40—Si23 | 160.4 (4) |
O39—Si14—O32 | 108.9 (3) | Si10v—O41—Si13 | 150.4 (4) |
O27—Si14—O28 | 108.0 (3) | Si13—O42—Si4v | 157.3 (4) |
O39—Si14—O28 | 110.8 (3) | Si4v—O43—Si19 | 150.7 (4) |
O32—Si14—O28 | 110.0 (3) | Si9v—O44—Si18 | 149.8 (4) |
O19iv—Si15—O28 | 109.6 (4) | Si3v—O45—Si18 | 154.0 (4) |
O19iv—Si15—O20iv | 111.3 (4) | Si24iii—O46—Si3 | 154.8 (5) |
O28—Si15—O20iv | 108.0 (3) | Si1vii—O47—Si17 | 150.1 (4) |
O19iv—Si15—O29 | 108.9 (3) | Si23—O48—Si7vii | 147.9 (5) |
Symmetry codes: (i) −x+1, −y+2, −z+1; (ii) −x+1/2, y+1/2, −z+1/2; (iii) x−1/2, −y+1/2, z−1/2; (iv) x−1/2, −y+1/2, z+1/2; (v) x+1/2, −y+1/2, z+1/2; (vi) x+1/2, −y+1/2, z−1/2; (vii) −x+1/2, y−1/2, −z+1/2. |
Crystal data top
C1.1O48.5Si24 | Z = 4 |
Mr = 1463.65 | F(000) = 2960 |
Monoclinic, P21/n | Dx = 1.855 Mg m−3 |
a = 13.386 (2) Å | Mo Kα radiation, λ = 0.71073 Å |
b = 20.106 (3) Å | µ = 0.68 mm−1 |
c = 19.881 (3) Å | T = 296 K |
β = 90.020 (2)° | Coffin shaped, colorless |
V = 5350.8 (14) Å3 | 0.23 × 0.08 × 0.06 mm |
Data collection top
Bruker P4 diffractometer | 12821 independent reflections |
Radiation source: fine-focus sealed tube | 5131 reflections with I > 2σ(I) |
Graphite monochromator | Rint = 0.113 |
ω scans | θmax = 28.7°, θmin = 1.0° |
Absorption correction: analytical ? | h = −17→17 |
Tmin = 0.861, Tmax = 0.962 | k = −25→27 |
61647 measured reflections | l = −26→26 |
Refinement top
Refinement on F2 | 2 restraints |
Least-squares matrix: full | Primary atom site location: structure-invariant direct methods |
R[F2 > 2σ(F2)] = 0.055 | Secondary atom site location: difference Fourier map |
wR(F2) = 0.148 | w = 1/[σ2(Fo2) + (0.051P)2] where P = (Fo2 + 2Fc2)/3 |
S = 0.82 | (Δ/σ)max = 0.001 |
12821 reflections | Δρmax = 0.90 e Å−3 |
660 parameters | Δρmin = −0.69 e Å−3 |
Crystal data top
C1.1O48.5Si24 | V = 5350.8 (14) Å3 |
Mr = 1463.65 | Z = 4 |
Monoclinic, P21/n | Mo Kα radiation |
a = 13.386 (2) Å | µ = 0.68 mm−1 |
b = 20.106 (3) Å | T = 296 K |
c = 19.881 (3) Å | 0.23 × 0.08 × 0.06 mm |
β = 90.020 (2)° | |
Data collection top
Bruker P4 diffractometer | 12821 independent reflections |
Absorption correction: analytical ? | 5131 reflections with I > 2σ(I) |
Tmin = 0.861, Tmax = 0.962 | Rint = 0.113 |
61647 measured reflections | |
Refinement top
R[F2 > 2σ(F2)] = 0.055 | 660 parameters |
wR(F2) = 0.148 | 2 restraints |
S = 0.82 | Δρmax = 0.90 e Å−3 |
12821 reflections | Δρmin = −0.69 e Å−3 |
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 | x | y | z | Uiso*/Ueq | Occ. (<1) |
C301 | 0.665 (4) | 0.2321 (16) | 0.259 (4) | 0.35 (3)* | 0.537 (15) |
C302 | 0.641 (5) | 0.3463 (17) | 0.265 (4) | 0.43 (4)* | 0.537 (15) |
O303 | 0.610 (3) | 0.287 (2) | 0.235 (3) | 0.45 (3)* | 0.537 (15) |
Si1 | 0.32420 (19) | 0.42060 (11) | −0.05615 (14) | 0.0167 (5) | |
Si2 | 0.1694 (2) | 0.31214 (13) | −0.03041 (12) | 0.0197 (6) | |
Si3 | −0.04836 (19) | 0.27962 (12) | −0.06255 (14) | 0.0190 (6) | |
Si4 | −0.03457 (19) | 0.12352 (12) | −0.06310 (13) | 0.0177 (6) | |
Si5 | 0.1783 (2) | 0.07558 (11) | −0.02785 (12) | 0.0150 (6) | |
Si6 | 0.31690 (19) | 0.19356 (12) | −0.05585 (14) | 0.0180 (5) | |
Si7 | 0.3209 (2) | 0.42465 (12) | 0.17134 (13) | 0.0163 (6) | |
Si8 | 0.17687 (19) | 0.31063 (13) | 0.12709 (12) | 0.0178 (5) | |
Si9 | −0.03436 (19) | 0.27338 (12) | 0.17549 (12) | 0.0158 (6) | |
Si10 | −0.0318 (2) | 0.11951 (12) | 0.17566 (12) | 0.0177 (6) | |
Si11 | 0.1779 (2) | 0.07110 (11) | 0.12960 (13) | 0.0178 (6) | |
Si12 | 0.3163 (2) | 0.18962 (13) | 0.16691 (12) | 0.0171 (5) | |
Si13 | 0.33533 (19) | 0.42734 (11) | 0.55756 (15) | 0.0162 (6) | |
Si14 | 0.1895 (2) | 0.31124 (13) | 0.52761 (12) | 0.0181 (6) | |
Si15 | −0.02898 (18) | 0.27759 (12) | 0.56141 (13) | 0.0168 (6) | |
Si16 | −0.03224 (19) | 0.12196 (12) | 0.56379 (14) | 0.0175 (6) | |
Si17 | 0.1808 (2) | 0.07054 (12) | 0.52774 (12) | 0.0165 (6) | |
Si18 | 0.31994 (19) | 0.18678 (11) | 0.56219 (13) | 0.0175 (6) | |
Si19 | 0.3173 (2) | 0.42371 (12) | 0.32771 (12) | 0.0172 (6) | |
Si20 | 0.17275 (19) | 0.31183 (12) | 0.36929 (13) | 0.0178 (5) | |
Si21 | −0.0416 (2) | 0.27348 (13) | 0.33081 (13) | 0.0189 (6) | |
Si22 | −0.0357 (2) | 0.11874 (13) | 0.32930 (13) | 0.0187 (6) | |
Si23 | 0.1790 (2) | 0.07196 (11) | 0.36961 (13) | 0.0161 (6) | |
Si24 | 0.30240 (19) | 0.19251 (12) | 0.32102 (11) | 0.0178 (6) | |
O1 | 0.2265 (5) | 0.3756 (3) | −0.0581 (4) | 0.0374 (17) | |
O2 | 0.0611 (4) | 0.3103 (3) | −0.0646 (3) | 0.0275 (15) | |
O3 | −0.0439 (5) | 0.2020 (3) | −0.0507 (4) | 0.0456 (18) | |
O4 | 0.0796 (4) | 0.1033 (3) | −0.0659 (3) | 0.0292 (16) | |
O5 | 0.2731 (4) | 0.1199 (3) | −0.0463 (3) | 0.0293 (16) | |
O6 | 0.2296 (5) | 0.2466 (3) | −0.0483 (4) | 0.0400 (18) | |
O7 | 0.2317 (5) | 0.3756 (3) | 0.1547 (3) | 0.038 (2) | |
O8 | 0.0718 (4) | 0.3050 (3) | 0.1647 (3) | 0.0352 (17) | |
O9 | −0.0315 (5) | 0.1963 (3) | 0.1559 (3) | 0.0310 (17) | |
O10 | 0.0783 (5) | 0.0900 (3) | 0.1682 (3) | 0.0330 (17) | |
O11 | 0.2653 (5) | 0.1200 (3) | 0.1515 (3) | 0.0349 (19) | |
O12 | 0.2429 (5) | 0.2470 (3) | 0.1404 (3) | 0.0395 (19) | |
O13 | 0.1594 (5) | 0.3169 (3) | 0.0484 (3) | 0.050 (2) | |
O14 | 0.1592 (4) | 0.0774 (3) | 0.0506 (3) | 0.0324 (16) | |
O15 | 0.3802 (5) | 0.4147 (3) | −0.1257 (3) | 0.0367 (19) | |
O16 | 0.3941 (6) | 0.3963 (3) | 0.0043 (3) | 0.047 (2) | |
O17 | 0.4191 (5) | 0.4009 (3) | 0.1335 (3) | 0.0329 (18) | |
O18 | 0.3642 (4) | 0.1990 (3) | −0.1297 (3) | 0.0285 (15) | |
O19 | 0.4033 (5) | 0.2067 (3) | −0.0019 (3) | 0.0364 (18) | |
O20 | 0.4206 (4) | 0.1953 (3) | 0.1290 (3) | 0.0273 (15) | |
O21 | 0.2043 (5) | 0.0023 (2) | −0.0521 (3) | 0.0263 (15) | |
O22 | 0.2093 (5) | −0.0033 (3) | 0.1481 (3) | 0.0295 (17) | |
O23 | 0.3443 (4) | 0.4233 (2) | 0.2503 (4) | 0.0335 (13) | |
O24 | 0.3391 (4) | 0.1975 (2) | 0.2451 (3) | 0.0311 (13) | |
O25 | −0.0638 (4) | 0.2832 (2) | 0.2524 (3) | 0.0271 (13) | |
O26 | −0.0663 (3) | 0.1095 (2) | 0.2522 (3) | 0.0251 (12) | |
O27 | 0.2436 (5) | 0.3775 (3) | 0.5540 (4) | 0.0402 (18) | |
O28 | 0.0774 (4) | 0.3131 (3) | 0.5548 (3) | 0.0315 (15) | |
O29 | −0.0137 (5) | 0.1990 (3) | 0.5665 (3) | 0.0405 (18) | |
O30 | 0.0694 (4) | 0.0835 (3) | 0.5547 (4) | 0.0328 (16) | |
O31 | 0.2583 (5) | 0.1194 (3) | 0.5641 (3) | 0.0294 (16) | |
O32 | 0.2457 (5) | 0.2487 (3) | 0.5593 (3) | 0.0374 (17) | |
O33 | 0.2230 (5) | 0.3780 (3) | 0.3411 (3) | 0.0306 (18) | |
O34 | 0.0561 (4) | 0.3138 (3) | 0.3541 (3) | 0.0253 (15) | |
O35 | −0.0235 (5) | 0.1960 (3) | 0.3479 (3) | 0.0298 (17) | |
O36 | 0.0690 (5) | 0.0844 (3) | 0.3437 (3) | 0.043 (2) | |
O37 | 0.2560 (6) | 0.1217 (3) | 0.3328 (3) | 0.039 (2) | |
O38 | 0.2206 (5) | 0.2476 (3) | 0.3336 (3) | 0.0385 (18) | |
O39 | 0.1927 (5) | 0.3057 (4) | 0.4481 (3) | 0.0531 (19) | |
O40 | 0.1831 (5) | 0.0840 (3) | 0.4486 (3) | 0.0359 (16) | |
O41 | 0.3912 (5) | 0.4191 (3) | 0.6283 (3) | 0.0350 (18) | |
O42 | 0.4129 (5) | 0.4129 (3) | 0.4992 (3) | 0.0336 (17) | |
O43 | 0.4122 (5) | 0.3964 (3) | 0.3678 (3) | 0.0314 (17) | |
O44 | 0.3852 (4) | 0.1893 (3) | 0.6295 (3) | 0.0285 (15) | |
O45 | 0.3912 (5) | 0.1865 (3) | 0.4977 (3) | 0.0364 (18) | |
O46 | −0.1017 (5) | 0.2957 (3) | −0.1317 (3) | 0.0382 (18) | |
O47 | 0.2089 (5) | −0.0051 (3) | 0.5438 (3) | 0.0248 (16) | |
O48 | 0.2111 (5) | −0.0021 (3) | 0.3518 (3) | 0.0307 (17) | |
Atomic displacement parameters (Å2) top | U11 | U22 | U33 | U12 | U13 | U23 |
Si1 | 0.0265 (14) | 0.0110 (11) | 0.0126 (12) | 0.0020 (10) | 0.0028 (13) | −0.0007 (11) |
Si2 | 0.0284 (15) | 0.0131 (13) | 0.0174 (12) | −0.0017 (12) | 0.0032 (11) | −0.0015 (11) |
Si3 | 0.0269 (14) | 0.0150 (12) | 0.0151 (14) | 0.0007 (10) | −0.0007 (12) | −0.0034 (11) |
Si4 | 0.0213 (14) | 0.0159 (13) | 0.0158 (14) | −0.0023 (11) | 0.0005 (13) | 0.0019 (12) |
Si5 | 0.0204 (15) | 0.0112 (13) | 0.0134 (13) | −0.0015 (11) | 0.0014 (12) | −0.0011 (10) |
Si6 | 0.0247 (13) | 0.0153 (12) | 0.0139 (11) | −0.0069 (12) | 0.0035 (12) | 0.0010 (12) |
Si7 | 0.0199 (14) | 0.0153 (13) | 0.0136 (14) | −0.0021 (12) | 0.0038 (13) | −0.0034 (11) |
Si8 | 0.0190 (13) | 0.0191 (13) | 0.0153 (12) | −0.0012 (12) | 0.0001 (12) | −0.0004 (12) |
Si9 | 0.0219 (15) | 0.0156 (13) | 0.0098 (13) | 0.0014 (11) | 0.0023 (11) | 0.0020 (10) |
Si10 | 0.0271 (16) | 0.0171 (14) | 0.0091 (13) | −0.0008 (11) | 0.0020 (12) | −0.0026 (11) |
Si11 | 0.0260 (15) | 0.0138 (13) | 0.0136 (13) | −0.0004 (11) | 0.0063 (13) | −0.0015 (11) |
Si12 | 0.0231 (13) | 0.0161 (12) | 0.0121 (11) | −0.0002 (12) | 0.0034 (10) | 0.0007 (11) |
Si13 | 0.0251 (15) | 0.0099 (11) | 0.0135 (12) | 0.0006 (10) | 0.0023 (12) | −0.0001 (11) |
Si14 | 0.0227 (14) | 0.0164 (13) | 0.0153 (12) | −0.0012 (12) | 0.0033 (10) | 0.0015 (11) |
Si15 | 0.0219 (14) | 0.0162 (12) | 0.0124 (13) | −0.0002 (10) | 0.0038 (12) | −0.0017 (11) |
Si16 | 0.0219 (14) | 0.0142 (13) | 0.0164 (14) | 0.0015 (11) | 0.0021 (13) | 0.0019 (12) |
Si17 | 0.0235 (15) | 0.0101 (13) | 0.0157 (13) | −0.0021 (11) | 0.0014 (12) | 0.0021 (10) |
Si18 | 0.0243 (14) | 0.0140 (12) | 0.0141 (12) | −0.0025 (11) | −0.0006 (11) | 0.0017 (11) |
Si19 | 0.0280 (16) | 0.0126 (13) | 0.0109 (13) | −0.0011 (12) | 0.0016 (13) | −0.0004 (10) |
Si20 | 0.0244 (14) | 0.0139 (12) | 0.0151 (12) | −0.0024 (12) | 0.0029 (12) | −0.0016 (12) |
Si21 | 0.0250 (15) | 0.0177 (14) | 0.0141 (14) | −0.0002 (11) | 0.0025 (12) | −0.0018 (11) |
Si22 | 0.0254 (15) | 0.0169 (14) | 0.0139 (14) | 0.0001 (12) | 0.0020 (13) | −0.0001 (11) |
Si23 | 0.0264 (15) | 0.0088 (12) | 0.0130 (13) | 0.0005 (11) | 0.0018 (13) | −0.0002 (11) |
Si24 | 0.0265 (14) | 0.0135 (12) | 0.0134 (12) | −0.0021 (12) | 0.0034 (10) | −0.0025 (10) |
O1 | 0.043 (4) | 0.017 (3) | 0.052 (4) | −0.013 (3) | 0.000 (4) | 0.009 (4) |
O2 | 0.015 (3) | 0.028 (4) | 0.039 (4) | −0.007 (3) | 0.000 (3) | 0.001 (3) |
O3 | 0.070 (5) | 0.009 (3) | 0.058 (4) | 0.000 (3) | 0.005 (4) | −0.007 (4) |
O4 | 0.017 (3) | 0.046 (4) | 0.025 (4) | 0.007 (3) | 0.003 (3) | 0.006 (3) |
O5 | 0.022 (3) | 0.018 (3) | 0.049 (4) | −0.011 (3) | 0.006 (3) | 0.006 (3) |
O6 | 0.030 (4) | 0.019 (3) | 0.070 (5) | 0.010 (3) | 0.019 (4) | −0.006 (4) |
O7 | 0.034 (4) | 0.030 (4) | 0.049 (5) | −0.017 (3) | 0.002 (4) | −0.016 (3) |
O8 | 0.021 (4) | 0.042 (4) | 0.042 (4) | −0.009 (4) | 0.020 (3) | −0.005 (3) |
O9 | 0.054 (5) | 0.015 (3) | 0.023 (3) | 0.005 (3) | 0.000 (3) | 0.000 (3) |
O10 | 0.028 (4) | 0.046 (4) | 0.025 (4) | 0.019 (3) | 0.016 (3) | 0.008 (3) |
O11 | 0.037 (4) | 0.021 (4) | 0.047 (5) | −0.005 (3) | −0.013 (3) | −0.012 (3) |
O12 | 0.044 (4) | 0.028 (4) | 0.047 (4) | 0.022 (3) | −0.005 (4) | 0.000 (3) |
O13 | 0.069 (5) | 0.063 (5) | 0.017 (3) | 0.004 (4) | −0.004 (4) | −0.004 (4) |
O14 | 0.040 (4) | 0.041 (4) | 0.015 (3) | 0.006 (3) | 0.003 (3) | −0.004 (3) |
O15 | 0.057 (5) | 0.041 (4) | 0.012 (4) | 0.017 (4) | 0.017 (4) | −0.001 (3) |
O16 | 0.051 (5) | 0.066 (5) | 0.025 (4) | 0.024 (4) | −0.021 (4) | 0.003 (4) |
O17 | 0.026 (4) | 0.049 (5) | 0.024 (4) | 0.005 (3) | 0.014 (4) | −0.006 (4) |
O18 | 0.023 (3) | 0.046 (4) | 0.016 (3) | −0.009 (3) | 0.007 (3) | 0.001 (3) |
O19 | 0.040 (4) | 0.053 (5) | 0.017 (3) | −0.016 (4) | −0.010 (3) | −0.004 (3) |
O20 | 0.020 (3) | 0.041 (4) | 0.021 (3) | 0.000 (3) | 0.008 (3) | 0.009 (3) |
O21 | 0.034 (4) | 0.015 (3) | 0.031 (3) | −0.006 (3) | 0.010 (4) | −0.006 (3) |
O22 | 0.033 (4) | 0.014 (3) | 0.041 (4) | −0.001 (3) | 0.000 (4) | 0.005 (3) |
O23 | 0.047 (4) | 0.045 (3) | 0.008 (2) | 0.001 (3) | 0.003 (4) | −0.002 (4) |
O24 | 0.042 (3) | 0.038 (3) | 0.013 (3) | −0.014 (3) | 0.005 (3) | −0.003 (4) |
O25 | 0.035 (3) | 0.028 (3) | 0.018 (3) | 0.006 (2) | 0.005 (4) | 0.007 (3) |
O26 | 0.028 (3) | 0.033 (3) | 0.015 (3) | −0.004 (2) | 0.008 (4) | −0.003 (4) |
O27 | 0.036 (4) | 0.022 (4) | 0.063 (5) | −0.016 (3) | 0.004 (4) | −0.004 (4) |
O28 | 0.018 (3) | 0.029 (4) | 0.047 (4) | −0.002 (3) | 0.008 (3) | −0.009 (4) |
O29 | 0.060 (5) | 0.014 (3) | 0.047 (4) | −0.001 (3) | 0.008 (4) | 0.000 (3) |
O30 | 0.017 (3) | 0.030 (3) | 0.052 (4) | 0.010 (3) | 0.015 (4) | 0.002 (4) |
O31 | 0.046 (4) | 0.021 (3) | 0.021 (4) | −0.015 (3) | −0.009 (3) | 0.004 (3) |
O32 | 0.042 (4) | 0.022 (3) | 0.048 (4) | 0.015 (3) | 0.011 (4) | 0.015 (3) |
O33 | 0.027 (4) | 0.013 (3) | 0.052 (5) | −0.006 (3) | 0.009 (3) | 0.004 (3) |
O34 | 0.019 (3) | 0.022 (3) | 0.035 (4) | −0.004 (3) | −0.005 (3) | −0.003 (3) |
O35 | 0.052 (5) | 0.012 (3) | 0.026 (3) | −0.003 (3) | −0.013 (3) | −0.001 (3) |
O36 | 0.038 (5) | 0.042 (4) | 0.050 (5) | 0.022 (4) | −0.014 (4) | −0.009 (4) |
O37 | 0.063 (5) | 0.023 (4) | 0.030 (4) | −0.006 (4) | 0.019 (4) | −0.002 (3) |
O38 | 0.049 (5) | 0.020 (3) | 0.046 (4) | 0.011 (3) | 0.015 (4) | −0.008 (3) |
O39 | 0.044 (4) | 0.100 (5) | 0.015 (3) | −0.007 (4) | 0.006 (3) | 0.000 (4) |
O40 | 0.064 (5) | 0.025 (3) | 0.018 (3) | −0.015 (3) | 0.003 (4) | 0.000 (3) |
O41 | 0.052 (5) | 0.032 (4) | 0.021 (4) | 0.016 (4) | −0.013 (4) | −0.002 (3) |
O42 | 0.031 (4) | 0.041 (4) | 0.029 (4) | 0.008 (3) | 0.011 (3) | −0.007 (3) |
O43 | 0.031 (4) | 0.047 (4) | 0.016 (3) | 0.010 (3) | −0.004 (4) | 0.007 (3) |
O44 | 0.031 (4) | 0.030 (3) | 0.024 (3) | −0.012 (3) | −0.017 (3) | −0.003 (3) |
O45 | 0.043 (4) | 0.036 (4) | 0.031 (4) | −0.009 (4) | 0.017 (3) | 0.002 (3) |
O46 | 0.030 (4) | 0.065 (5) | 0.020 (3) | 0.010 (4) | −0.011 (3) | 0.007 (4) |
O47 | 0.030 (4) | 0.011 (3) | 0.033 (4) | 0.002 (3) | 0.007 (3) | 0.009 (3) |
O48 | 0.029 (4) | 0.016 (3) | 0.048 (5) | 0.001 (3) | −0.002 (4) | −0.008 (3) |
Geometric parameters (Å, º) top
C301—O303 | 1.4006 | Si14—O27 | 1.600 (6) |
C302—O303 | 1.4002 | Si15—O19iii | 1.578 (6) |
Si1—O47i | 1.573 (6) | Si15—O29 | 1.592 (6) |
Si1—O15 | 1.574 (7) | Si15—O28 | 1.595 (6) |
Si1—O1 | 1.586 (6) | Si15—O20iii | 1.595 (6) |
Si1—O16 | 1.594 (7) | Si16—O29 | 1.567 (6) |
Si2—O13 | 1.572 (7) | Si16—O30 | 1.571 (6) |
Si2—O6 | 1.581 (6) | Si16—O16iii | 1.579 (7) |
Si2—O1 | 1.583 (6) | Si16—O17iii | 1.595 (7) |
Si2—O2 | 1.598 (6) | Si17—O40 | 1.593 (7) |
Si3—O3 | 1.577 (6) | Si17—O47 | 1.595 (6) |
Si3—O46 | 1.578 (6) | Si17—O31 | 1.598 (6) |
Si3—O2 | 1.586 (6) | Si17—O30 | 1.601 (6) |
Si3—O45ii | 1.593 (7) | Si18—O31 | 1.582 (6) |
Si4—O4 | 1.578 (6) | Si18—O32 | 1.589 (6) |
Si4—O43ii | 1.595 (7) | Si18—O44 | 1.594 (6) |
Si4—O42ii | 1.597 (7) | Si18—O45 | 1.595 (7) |
Si4—O3 | 1.597 (6) | Si19—O23 | 1.577 (7) |
Si5—O14 | 1.576 (7) | Si19—O33 | 1.579 (7) |
Si5—O21 | 1.585 (6) | Si19—O22i | 1.580 (6) |
Si5—O5 | 1.589 (6) | Si19—O43 | 1.592 (7) |
Si5—O4 | 1.617 (6) | Si20—O34 | 1.586 (6) |
Si6—O6 | 1.585 (6) | Si20—O39 | 1.589 (7) |
Si6—O19 | 1.595 (6) | Si20—O33 | 1.589 (6) |
Si6—O18 | 1.599 (7) | Si20—O38 | 1.602 (6) |
Si6—O5 | 1.601 (6) | Si21—O18iii | 1.581 (6) |
Si7—O7 | 1.579 (7) | Si21—O25 | 1.594 (7) |
Si7—O17 | 1.584 (7) | Si21—O34 | 1.602 (6) |
Si7—O23 | 1.596 (7) | Si21—O35 | 1.609 (6) |
Si7—O48i | 1.596 (7) | Si22—O15iii | 1.583 (7) |
Si8—O12 | 1.573 (6) | Si22—O36 | 1.584 (7) |
Si8—O13 | 1.582 (7) | Si22—O26 | 1.594 (7) |
Si8—O7 | 1.591 (7) | Si22—O35 | 1.601 (6) |
Si8—O8 | 1.592 (6) | Si23—O36 | 1.576 (7) |
Si9—O8 | 1.568 (6) | Si23—O40 | 1.586 (7) |
Si9—O25 | 1.587 (7) | Si23—O48 | 1.587 (7) |
Si9—O9 | 1.594 (6) | Si23—O37 | 1.608 (7) |
Si9—O44ii | 1.595 (6) | Si24—O37 | 1.567 (7) |
Si10—O9 | 1.589 (6) | Si24—O38 | 1.574 (6) |
Si10—O10 | 1.592 (7) | Si24—O24 | 1.586 (7) |
Si10—O41ii | 1.593 (7) | Si24—O46iv | 1.604 (6) |
Si10—O26 | 1.597 (7) | O15—Si22v | 1.583 (7) |
Si11—O10 | 1.581 (7) | O16—Si16v | 1.579 (7) |
Si11—O11 | 1.584 (7) | O17—Si16v | 1.595 (7) |
Si11—O14 | 1.592 (7) | O18—Si21v | 1.581 (6) |
Si11—O22 | 1.593 (6) | O19—Si15v | 1.578 (6) |
Si12—O11 | 1.584 (7) | O20—Si15v | 1.595 (6) |
Si12—O20 | 1.587 (6) | O21—Si13vi | 1.597 (6) |
Si12—O24 | 1.588 (7) | O22—Si19vi | 1.581 (6) |
Si12—O12 | 1.601 (6) | O41—Si10iv | 1.593 (7) |
Si13—O42 | 1.581 (7) | O42—Si4iv | 1.597 (7) |
Si13—O27 | 1.583 (6) | O43—Si4iv | 1.594 (7) |
Si13—O41 | 1.597 (7) | O44—Si9iv | 1.595 (6) |
Si13—O21i | 1.597 (6) | O45—Si3iv | 1.593 (7) |
Si14—O39 | 1.582 (7) | O46—Si24ii | 1.604 (6) |
Si14—O28 | 1.590 (6) | O47—Si1vi | 1.573 (6) |
Si14—O32 | 1.592 (6) | O48—Si7vi | 1.596 (7) |
| | | |
C302—O303—C301 | 111.6 | O40—Si17—O47 | 110.7 (3) |
O47i—Si1—O15 | 109.9 (4) | O40—Si17—O31 | 109.1 (3) |
O47i—Si1—O1 | 108.1 (4) | O47—Si17—O31 | 109.9 (4) |
O15—Si1—O1 | 109.1 (4) | O40—Si17—O30 | 108.6 (4) |
O47i—Si1—O16 | 109.7 (4) | O47—Si17—O30 | 107.9 (3) |
O15—Si1—O16 | 110.9 (4) | O31—Si17—O30 | 110.5 (4) |
O1—Si1—O16 | 109.0 (4) | O31—Si18—O32 | 110.1 (4) |
O13—Si2—O6 | 108.5 (4) | O31—Si18—O44 | 106.9 (3) |
O13—Si2—O1 | 109.7 (4) | O32—Si18—O44 | 110.2 (4) |
O6—Si2—O1 | 110.2 (4) | O31—Si18—O45 | 109.1 (4) |
O13—Si2—O2 | 110.3 (4) | O32—Si18—O45 | 110.3 (4) |
O6—Si2—O2 | 110.2 (4) | O44—Si18—O45 | 110.2 (4) |
O1—Si2—O2 | 107.9 (4) | O23—Si19—O33 | 110.1 (3) |
O3—Si3—O46 | 110.4 (4) | O23—Si19—O22i | 110.6 (3) |
O3—Si3—O2 | 110.6 (4) | O33—Si19—O22i | 107.9 (4) |
O46—Si3—O2 | 108.2 (4) | O23—Si19—O43 | 107.5 (3) |
O3—Si3—O45ii | 109.2 (4) | O33—Si19—O43 | 110.5 (4) |
O46—Si3—O45ii | 109.6 (4) | O22i—Si19—O43 | 110.2 (4) |
O2—Si3—O45ii | 108.7 (4) | O34—Si20—O39 | 110.6 (3) |
O4—Si4—O43ii | 109.6 (4) | O34—Si20—O33 | 109.1 (4) |
O4—Si4—O42ii | 109.5 (4) | O39—Si20—O33 | 109.8 (4) |
O43ii—Si4—O42ii | 110.7 (4) | O34—Si20—O38 | 109.2 (4) |
O4—Si4—O3 | 109.5 (4) | O39—Si20—O38 | 107.8 (4) |
O43ii—Si4—O3 | 110.2 (4) | O33—Si20—O38 | 110.3 (4) |
O42ii—Si4—O3 | 107.3 (4) | O18iii—Si21—O25 | 107.0 (3) |
O14—Si5—O21 | 110.9 (3) | O18iii—Si21—O34 | 109.2 (3) |
O14—Si5—O5 | 110.1 (4) | O25—Si21—O34 | 111.7 (3) |
O21—Si5—O5 | 105.9 (3) | O18iii—Si21—O35 | 110.6 (4) |
O14—Si5—O4 | 108.7 (3) | O25—Si21—O35 | 110.5 (3) |
O21—Si5—O4 | 110.9 (4) | O34—Si21—O35 | 107.8 (4) |
O5—Si5—O4 | 110.4 (3) | O15iii—Si22—O36 | 109.9 (4) |
O6—Si6—O19 | 111.0 (4) | O15iii—Si22—O26 | 108.1 (3) |
O6—Si6—O18 | 109.3 (4) | O36—Si22—O26 | 110.3 (3) |
O19—Si6—O18 | 108.5 (4) | O15iii—Si22—O35 | 110.6 (4) |
O6—Si6—O5 | 109.9 (4) | O36—Si22—O35 | 106.8 (4) |
O19—Si6—O5 | 109.7 (4) | O26—Si22—O35 | 111.1 (3) |
O18—Si6—O5 | 108.4 (4) | O36—Si23—O40 | 109.2 (4) |
O7—Si7—O17 | 109.7 (4) | O36—Si23—O48 | 109.1 (4) |
O7—Si7—O23 | 110.0 (3) | O40—Si23—O48 | 110.7 (3) |
O17—Si7—O23 | 107.3 (3) | O36—Si23—O37 | 110.5 (4) |
O7—Si7—O48i | 108.1 (4) | O40—Si23—O37 | 109.4 (4) |
O17—Si7—O48i | 111.2 (4) | O48—Si23—O37 | 107.9 (4) |
O23—Si7—O48i | 110.5 (3) | O37—Si24—O38 | 109.8 (4) |
O12—Si8—O13 | 108.2 (4) | O37—Si24—O24 | 108.8 (3) |
O12—Si8—O7 | 110.4 (4) | O38—Si24—O24 | 108.7 (3) |
O13—Si8—O7 | 110.0 (4) | O37—Si24—O46iv | 111.3 (4) |
O12—Si8—O8 | 110.9 (4) | O38—Si24—O46iv | 110.9 (4) |
O13—Si8—O8 | 109.8 (4) | O24—Si24—O46iv | 107.3 (3) |
O7—Si8—O8 | 107.6 (4) | Si2—O1—Si1 | 147.7 (5) |
O8—Si9—O25 | 107.7 (3) | Si3—O2—Si2 | 146.2 (4) |
O8—Si9—O9 | 109.7 (4) | Si3—O3—Si4 | 162.4 (5) |
O25—Si9—O9 | 111.1 (3) | Si4—O4—Si5 | 149.1 (4) |
O8—Si9—O44ii | 110.0 (4) | Si5—O5—Si6 | 146.5 (4) |
O25—Si9—O44ii | 108.9 (3) | Si2—O6—Si6 | 162.4 (5) |
O9—Si9—O44ii | 109.4 (4) | Si7—O7—Si8 | 158.2 (5) |
O9—Si10—O10 | 109.6 (4) | Si9—O8—Si8 | 152.7 (5) |
O9—Si10—O41ii | 109.2 (4) | Si10—O9—Si9 | 151.7 (4) |
O10—Si10—O41ii | 111.1 (4) | Si11—O10—Si10 | 155.7 (5) |
O9—Si10—O26 | 110.8 (3) | Si12—O11—Si11 | 156.2 (5) |
O10—Si10—O26 | 107.9 (3) | Si8—O12—Si12 | 169.0 (5) |
O41ii—Si10—O26 | 108.2 (3) | Si2—O13—Si8 | 164.4 (5) |
O10—Si11—O11 | 109.8 (4) | Si5—O14—Si11 | 160.7 (4) |
O10—Si11—O14 | 109.0 (4) | Si1—O15—Si22v | 149.7 (5) |
O11—Si11—O14 | 109.6 (4) | Si16v—O16—Si1 | 175.3 (6) |
O10—Si11—O22 | 109.5 (4) | Si7—O17—Si16v | 146.6 (5) |
O11—Si11—O22 | 108.9 (4) | Si21v—O18—Si6 | 142.4 (4) |
O14—Si11—O22 | 110.0 (3) | Si15v—O19—Si6 | 168.6 (5) |
O11—Si12—O20 | 110.4 (4) | Si12—O20—Si15v | 142.5 (4) |
O11—Si12—O24 | 111.0 (3) | Si5—O21—Si13vi | 145.1 (4) |
O20—Si12—O24 | 106.7 (3) | Si19vi—O22—Si11 | 151.5 (5) |
O11—Si12—O12 | 108.0 (4) | Si19—O23—Si7 | 155.4 (4) |
O20—Si12—O12 | 109.2 (3) | Si24—O24—Si12 | 149.4 (4) |
O24—Si12—O12 | 111.5 (3) | Si9—O25—Si21 | 151.1 (3) |
O42—Si13—O27 | 111.0 (4) | Si22—O26—Si10 | 145.4 (3) |
O42—Si13—O41 | 108.6 (4) | Si13—O27—Si14 | 152.7 (5) |
O27—Si13—O41 | 109.5 (4) | Si14—O28—Si15 | 148.8 (4) |
O42—Si13—O21i | 109.9 (4) | Si16—O29—Si15 | 162.6 (5) |
O27—Si13—O21i | 109.6 (4) | Si16—O30—Si17 | 157.0 (5) |
O41—Si13—O21i | 108.2 (4) | Si18—O31—Si17 | 148.2 (4) |
O39—Si14—O28 | 111.4 (4) | Si18—O32—Si14 | 157.5 (5) |
O39—Si14—O32 | 109.0 (4) | Si19—O33—Si20 | 151.7 (5) |
O28—Si14—O32 | 109.1 (4) | Si20—O34—Si21 | 147.2 (4) |
O39—Si14—O27 | 111.8 (4) | Si22—O35—Si21 | 150.6 (4) |
O28—Si14—O27 | 107.1 (4) | Si23—O36—Si22 | 161.8 (5) |
O32—Si14—O27 | 108.2 (4) | Si24—O37—Si23 | 152.0 (5) |
O19iii—Si15—O29 | 108.7 (4) | Si24—O38—Si20 | 155.7 (5) |
O19iii—Si15—O28 | 110.8 (4) | Si14—O39—Si20 | 166.0 (5) |
O29—Si15—O28 | 109.5 (3) | Si23—O40—Si17 | 161.2 (4) |
O19iii—Si15—O20iii | 111.0 (3) | Si10iv—O41—Si13 | 150.4 (4) |
O29—Si15—O20iii | 109.8 (4) | Si13—O42—Si4iv | 159.8 (5) |
O28—Si15—O20iii | 107.1 (3) | Si19—O43—Si4iv | 150.4 (5) |
O29—Si16—O30 | 110.6 (3) | Si18—O44—Si9iv | 149.4 (4) |
O29—Si16—O16iii | 110.7 (4) | Si3iv—O45—Si18 | 154.4 (5) |
O30—Si16—O16iii | 109.8 (4) | Si3—O46—Si24ii | 153.8 (5) |
O29—Si16—O17iii | 108.6 (4) | Si1vi—O47—Si17 | 150.0 (5) |
O30—Si16—O17iii | 108.1 (4) | Si23—O48—Si7vi | 148.6 (5) |
O16iii—Si16—O17iii | 109.1 (4) | | |
Symmetry codes: (i) −x+1/2, y+1/2, −z+1/2; (ii) x−1/2, −y+1/2, z−1/2; (iii) x−1/2, −y+1/2, z+1/2; (iv) x+1/2, −y+1/2, z+1/2; (v) x+1/2, −y+1/2, z−1/2; (vi) −x+1/2, y−1/2, −z+1/2. |
Crystal data top
C2O49Si24 | Z = 4 |
Mr = 1481.3 | F(000) = 2984 |
Monoclinic, P21/n | Dx = 1.891 Mg m−3 |
a = 13.381 (2) Å | Mo Kα radiation, λ = 0.71073 Å |
b = 20.107 (4) Å | µ = 0.69 mm−1 |
c = 19.875 (4) Å | T = 296 K |
β = 90.023 (3)° | Coffin shaped, colorless |
V = 5347.4 (17) Å3 | 0.18 × 0.08 × 0.05 mm |
Data collection top
Bruker P4 diffractometer | 12898 independent reflections |
Radiation source: fine-focus sealed tube | 5103 reflections with I > 2σ(I) |
Graphite monochromator | Rint = 0.144 |
ω scans | θmax = 29.0°, θmin = 1.0° |
Absorption correction: analytical ? | h = −17→18 |
Tmin = 0.885, Tmax = 0.969 | k = −27→25 |
61933 measured reflections | l = −26→25 |
Refinement top
Refinement on F2 | 6 restraints |
Least-squares matrix: full | Primary atom site location: structure-invariant direct methods |
R[F2 > 2σ(F2)] = 0.059 | Secondary atom site location: difference Fourier map |
wR(F2) = 0.139 | w = 1/[σ2(Fo2) + (0.0415P)2] where P = (Fo2 + 2Fc2)/3 |
S = 0.84 | (Δ/σ)max < 0.001 |
12898 reflections | Δρmax = 0.77 e Å−3 |
668 parameters | Δρmin = −0.73 e Å−3 |
Crystal data top
C2O49Si24 | V = 5347.4 (17) Å3 |
Mr = 1481.3 | Z = 4 |
Monoclinic, P21/n | Mo Kα radiation |
a = 13.381 (2) Å | µ = 0.69 mm−1 |
b = 20.107 (4) Å | T = 296 K |
c = 19.875 (4) Å | 0.18 × 0.08 × 0.05 mm |
β = 90.023 (3)° | |
Data collection top
Bruker P4 diffractometer | 12898 independent reflections |
Absorption correction: analytical ? | 5103 reflections with I > 2σ(I) |
Tmin = 0.885, Tmax = 0.969 | Rint = 0.144 |
61933 measured reflections | |
Refinement top
R[F2 > 2σ(F2)] = 0.059 | 668 parameters |
wR(F2) = 0.139 | 6 restraints |
S = 0.84 | Δρmax = 0.77 e Å−3 |
12898 reflections | Δρmin = −0.73 e Å−3 |
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 | x | y | z | Uiso*/Ueq | Occ. (<1) |
C101 | −0.002 (2) | 0.4830 (16) | 0.090 (2) | 0.12 (4)* | 0.119 (9) |
C102 | 0.009 (3) | 0.5109 (17) | −0.025 (2) | 0.05 (3)* | 0.119 (9) |
O103 | 0.063 (3) | 0.5009 (15) | 0.036 (2) | 0.07 (2)* | 0.119 (9) |
C201 | 0.508 (2) | 0.0341 (13) | 0.0014 (17) | 0.12 (2)* | 0.282 (12) |
C202 | 0.4889 (19) | 0.0092 (9) | 0.1161 (18) | 0.16 (3)* | 0.282 (12) |
O203 | 0.483 (2) | −0.0157 (11) | 0.0493 (19) | 0.16 (2)* | 0.282 (12) |
C301 | 0.6756 (16) | 0.2272 (11) | 0.2500 (14) | 0.31 (3)* | 0.577 (16) |
C302 | 0.6442 (18) | 0.3407 (11) | 0.2431 (16) | 0.35 (3)* | 0.577 (16) |
O303 | 0.6023 (16) | 0.2768 (11) | 0.2435 (13) | 0.47 (3)* | 0.577 (16) |
Si1 | 0.3243 (2) | 0.42077 (12) | −0.05612 (15) | 0.0150 (6) | |
Si2 | 0.1697 (2) | 0.31246 (14) | −0.03064 (12) | 0.0182 (6) | |
Si3 | −0.0477 (2) | 0.27957 (13) | −0.06245 (14) | 0.0177 (6) | |
Si4 | −0.0344 (2) | 0.12356 (12) | −0.06301 (14) | 0.0147 (6) | |
Si5 | 0.1781 (2) | 0.07577 (12) | −0.02813 (12) | 0.0149 (6) | |
Si6 | 0.3173 (2) | 0.19361 (13) | −0.05549 (14) | 0.0180 (6) | |
Si7 | 0.3210 (2) | 0.42459 (13) | 0.17154 (13) | 0.0154 (6) | |
Si8 | 0.1766 (2) | 0.31041 (14) | 0.12706 (13) | 0.0161 (6) | |
Si9 | −0.0343 (2) | 0.27343 (13) | 0.17577 (13) | 0.0160 (6) | |
Si10 | −0.0314 (2) | 0.11950 (13) | 0.17539 (13) | 0.0158 (6) | |
Si11 | 0.1783 (2) | 0.07137 (12) | 0.12938 (14) | 0.0149 (6) | |
Si12 | 0.3162 (2) | 0.18983 (14) | 0.16668 (12) | 0.0160 (6) | |
Si13 | 0.3356 (2) | 0.42728 (11) | 0.55740 (16) | 0.0158 (6) | |
Si14 | 0.1892 (2) | 0.31132 (14) | 0.52759 (12) | 0.0168 (6) | |
Si15 | −0.0293 (2) | 0.27774 (12) | 0.56131 (14) | 0.0156 (6) | |
Si16 | −0.0319 (2) | 0.12194 (13) | 0.56369 (14) | 0.0158 (6) | |
Si17 | 0.1809 (2) | 0.07042 (12) | 0.52725 (13) | 0.0150 (6) | |
Si18 | 0.3199 (2) | 0.18668 (12) | 0.56248 (13) | 0.0134 (6) | |
Si19 | 0.3173 (2) | 0.42359 (12) | 0.32785 (13) | 0.0155 (6) | |
Si20 | 0.1729 (2) | 0.31175 (13) | 0.36938 (14) | 0.0175 (6) | |
Si21 | −0.0413 (2) | 0.27345 (13) | 0.33108 (13) | 0.0152 (6) | |
Si22 | −0.0359 (2) | 0.11829 (13) | 0.32937 (14) | 0.0174 (6) | |
Si23 | 0.1789 (2) | 0.07183 (12) | 0.36935 (14) | 0.0148 (6) | |
Si24 | 0.3025 (2) | 0.19270 (13) | 0.32069 (12) | 0.0166 (6) | |
O1 | 0.2275 (5) | 0.3758 (3) | −0.0589 (4) | 0.0323 (18) | |
O2 | 0.0611 (4) | 0.3097 (3) | −0.0652 (3) | 0.0251 (15) | |
O3 | −0.0438 (5) | 0.2020 (3) | −0.0506 (4) | 0.0419 (18) | |
O4 | 0.0798 (5) | 0.1027 (3) | −0.0661 (3) | 0.0248 (16) | |
O5 | 0.2715 (5) | 0.1204 (3) | −0.0463 (3) | 0.0238 (16) | |
O6 | 0.2294 (5) | 0.2470 (3) | −0.0480 (4) | 0.0387 (19) | |
O7 | 0.2292 (6) | 0.3759 (3) | 0.1545 (4) | 0.035 (2) | |
O8 | 0.0724 (5) | 0.3042 (3) | 0.1650 (3) | 0.0319 (18) | |
O9 | −0.0304 (5) | 0.1961 (3) | 0.1558 (3) | 0.0303 (18) | |
O10 | 0.0770 (5) | 0.0896 (3) | 0.1673 (3) | 0.0325 (19) | |
O11 | 0.2660 (6) | 0.1189 (3) | 0.1509 (3) | 0.0318 (19) | |
O12 | 0.2433 (5) | 0.2465 (3) | 0.1403 (3) | 0.0374 (19) | |
O13 | 0.1595 (5) | 0.3179 (3) | 0.0481 (3) | 0.042 (2) | |
O14 | 0.1587 (5) | 0.0776 (3) | 0.0512 (3) | 0.0297 (16) | |
O15 | 0.3808 (6) | 0.4145 (3) | −0.1253 (3) | 0.036 (2) | |
O16 | 0.3943 (6) | 0.3961 (4) | 0.0043 (3) | 0.045 (2) | |
O17 | 0.4193 (5) | 0.4021 (3) | 0.1336 (3) | 0.0280 (18) | |
O18 | 0.3639 (5) | 0.1990 (3) | −0.1294 (3) | 0.0277 (16) | |
O19 | 0.4046 (5) | 0.2063 (4) | −0.0022 (3) | 0.0302 (18) | |
O20 | 0.4207 (4) | 0.1954 (3) | 0.1283 (3) | 0.0264 (16) | |
O21 | 0.2029 (5) | 0.0020 (3) | −0.0517 (3) | 0.0221 (15) | |
O22 | 0.2099 (6) | −0.0035 (3) | 0.1476 (4) | 0.0301 (19) | |
O23 | 0.3447 (4) | 0.4232 (2) | 0.2501 (4) | 0.0306 (13) | |
O24 | 0.3392 (4) | 0.1976 (3) | 0.2443 (3) | 0.0292 (13) | |
O25 | −0.0638 (4) | 0.2832 (2) | 0.2530 (3) | 0.0227 (13) | |
O26 | −0.0671 (3) | 0.1095 (2) | 0.2525 (4) | 0.0216 (13) | |
O27 | 0.2448 (5) | 0.3770 (3) | 0.5529 (4) | 0.0371 (19) | |
O28 | 0.0762 (4) | 0.3132 (3) | 0.5545 (4) | 0.0265 (15) | |
O29 | −0.0130 (5) | 0.2000 (3) | 0.5662 (3) | 0.0368 (18) | |
O30 | 0.0690 (5) | 0.0837 (3) | 0.5541 (4) | 0.0336 (17) | |
O31 | 0.2587 (5) | 0.1195 (3) | 0.5647 (3) | 0.0275 (17) | |
O32 | 0.2455 (5) | 0.2481 (3) | 0.5588 (4) | 0.0346 (18) | |
O33 | 0.2234 (6) | 0.3780 (3) | 0.3416 (3) | 0.0279 (18) | |
O34 | 0.0572 (5) | 0.3137 (3) | 0.3535 (3) | 0.0239 (16) | |
O35 | −0.0257 (6) | 0.1961 (3) | 0.3485 (3) | 0.0282 (18) | |
O36 | 0.0700 (6) | 0.0838 (4) | 0.3434 (4) | 0.043 (2) | |
O37 | 0.2562 (6) | 0.1218 (3) | 0.3333 (3) | 0.034 (2) | |
O38 | 0.2216 (5) | 0.2483 (3) | 0.3329 (3) | 0.0368 (19) | |
O39 | 0.1927 (5) | 0.3054 (4) | 0.4470 (3) | 0.0476 (19) | |
O40 | 0.1836 (5) | 0.0845 (3) | 0.4492 (3) | 0.0339 (17) | |
O41 | 0.3903 (5) | 0.4197 (3) | 0.6280 (4) | 0.0324 (19) | |
O42 | 0.4137 (5) | 0.4138 (3) | 0.4982 (3) | 0.0302 (18) | |
O43 | 0.4123 (5) | 0.3958 (3) | 0.3691 (3) | 0.0279 (18) | |
O44 | 0.3849 (5) | 0.1899 (3) | 0.6296 (3) | 0.0255 (16) | |
O45 | 0.3893 (5) | 0.1864 (3) | 0.4980 (3) | 0.0336 (18) | |
O46 | −0.1011 (5) | 0.2944 (4) | −0.1320 (3) | 0.039 (2) | |
O47 | 0.2091 (5) | −0.0046 (3) | 0.5434 (3) | 0.0220 (17) | |
O48 | 0.2106 (6) | −0.0021 (3) | 0.3516 (4) | 0.033 (2) | |
Atomic displacement parameters (Å2) top | U11 | U22 | U33 | U12 | U13 | U23 |
Si1 | 0.0243 (15) | 0.0114 (12) | 0.0094 (12) | −0.0004 (11) | 0.0019 (14) | −0.0011 (12) |
Si2 | 0.0264 (16) | 0.0118 (13) | 0.0165 (12) | −0.0012 (13) | 0.0041 (11) | 0.0001 (11) |
Si3 | 0.0255 (16) | 0.0142 (13) | 0.0135 (14) | 0.0003 (11) | −0.0007 (12) | −0.0039 (11) |
Si4 | 0.0207 (15) | 0.0109 (13) | 0.0125 (14) | −0.0016 (11) | −0.0009 (14) | −0.0005 (11) |
Si5 | 0.0208 (16) | 0.0108 (13) | 0.0129 (13) | −0.0002 (12) | 0.0010 (12) | −0.0005 (10) |
Si6 | 0.0274 (15) | 0.0118 (12) | 0.0150 (12) | −0.0063 (13) | 0.0032 (13) | −0.0001 (13) |
Si7 | 0.0220 (16) | 0.0142 (14) | 0.0102 (14) | −0.0015 (13) | 0.0049 (13) | −0.0009 (11) |
Si8 | 0.0153 (14) | 0.0187 (14) | 0.0143 (12) | −0.0026 (13) | 0.0029 (12) | −0.0008 (13) |
Si9 | 0.0208 (16) | 0.0173 (14) | 0.0100 (14) | −0.0002 (12) | 0.0025 (12) | 0.0023 (11) |
Si10 | 0.0219 (17) | 0.0171 (14) | 0.0084 (14) | −0.0019 (12) | 0.0017 (13) | −0.0035 (11) |
Si11 | 0.0214 (16) | 0.0106 (13) | 0.0130 (13) | 0.0001 (12) | 0.0069 (14) | 0.0005 (11) |
Si12 | 0.0204 (14) | 0.0162 (13) | 0.0116 (11) | −0.0004 (13) | 0.0036 (11) | 0.0000 (11) |
Si13 | 0.0242 (16) | 0.0102 (12) | 0.0130 (12) | 0.0012 (11) | −0.0015 (13) | 0.0022 (12) |
Si14 | 0.0223 (15) | 0.0116 (13) | 0.0165 (12) | −0.0017 (13) | 0.0045 (11) | 0.0022 (11) |
Si15 | 0.0237 (16) | 0.0126 (12) | 0.0105 (13) | −0.0015 (10) | 0.0018 (13) | −0.0036 (11) |
Si16 | 0.0189 (16) | 0.0149 (14) | 0.0135 (14) | 0.0021 (11) | 0.0013 (13) | 0.0008 (12) |
Si17 | 0.0225 (17) | 0.0069 (13) | 0.0157 (14) | −0.0001 (12) | 0.0017 (12) | −0.0001 (10) |
Si18 | 0.0169 (14) | 0.0122 (12) | 0.0110 (12) | −0.0025 (11) | 0.0018 (11) | 0.0032 (11) |
Si19 | 0.0248 (17) | 0.0093 (13) | 0.0123 (14) | −0.0007 (12) | 0.0008 (14) | 0.0024 (10) |
Si20 | 0.0246 (15) | 0.0130 (13) | 0.0152 (12) | −0.0033 (13) | 0.0058 (13) | 0.0003 (13) |
Si21 | 0.0227 (16) | 0.0122 (14) | 0.0106 (14) | 0.0005 (11) | 0.0016 (12) | −0.0010 (10) |
Si22 | 0.0237 (17) | 0.0138 (14) | 0.0147 (15) | −0.0005 (12) | 0.0013 (14) | −0.0011 (11) |
Si23 | 0.0232 (16) | 0.0085 (13) | 0.0127 (13) | −0.0005 (12) | 0.0035 (14) | 0.0007 (11) |
Si24 | 0.0256 (15) | 0.0111 (12) | 0.0132 (12) | −0.0039 (13) | 0.0067 (11) | −0.0026 (11) |
O1 | 0.034 (4) | 0.015 (3) | 0.048 (4) | −0.011 (3) | −0.003 (4) | 0.011 (4) |
O2 | 0.011 (3) | 0.033 (4) | 0.030 (4) | 0.000 (3) | 0.007 (3) | 0.007 (3) |
O3 | 0.064 (5) | 0.008 (3) | 0.054 (4) | −0.004 (3) | 0.014 (4) | −0.003 (4) |
O4 | 0.015 (4) | 0.037 (4) | 0.022 (4) | 0.007 (3) | 0.008 (3) | 0.008 (3) |
O5 | 0.020 (4) | 0.013 (3) | 0.039 (4) | −0.008 (3) | 0.005 (3) | 0.003 (3) |
O6 | 0.027 (4) | 0.020 (4) | 0.069 (5) | 0.008 (3) | 0.014 (4) | −0.011 (4) |
O7 | 0.039 (5) | 0.017 (4) | 0.051 (5) | −0.017 (4) | −0.003 (4) | −0.011 (4) |
O8 | 0.018 (4) | 0.037 (4) | 0.042 (4) | −0.010 (4) | 0.025 (3) | −0.011 (4) |
O9 | 0.053 (5) | 0.015 (4) | 0.023 (3) | 0.006 (4) | 0.005 (3) | 0.000 (3) |
O10 | 0.023 (4) | 0.048 (5) | 0.026 (4) | 0.020 (4) | 0.018 (3) | 0.015 (3) |
O11 | 0.037 (5) | 0.017 (4) | 0.041 (5) | −0.008 (3) | −0.013 (3) | −0.013 (3) |
O12 | 0.041 (5) | 0.024 (4) | 0.048 (5) | 0.018 (3) | −0.004 (4) | −0.001 (3) |
O13 | 0.050 (5) | 0.059 (5) | 0.017 (3) | 0.008 (4) | −0.004 (4) | −0.001 (4) |
O14 | 0.042 (4) | 0.031 (4) | 0.016 (3) | 0.005 (3) | 0.003 (3) | −0.003 (3) |
O15 | 0.052 (5) | 0.045 (5) | 0.011 (4) | 0.019 (4) | 0.013 (4) | 0.002 (3) |
O16 | 0.060 (6) | 0.055 (5) | 0.021 (4) | 0.027 (4) | −0.024 (4) | 0.003 (4) |
O17 | 0.017 (4) | 0.048 (5) | 0.019 (4) | 0.004 (3) | 0.009 (3) | −0.010 (4) |
O18 | 0.026 (4) | 0.045 (4) | 0.013 (3) | −0.007 (3) | 0.007 (3) | −0.001 (3) |
O19 | 0.025 (4) | 0.051 (5) | 0.014 (3) | −0.008 (4) | −0.004 (3) | −0.004 (3) |
O20 | 0.023 (4) | 0.036 (4) | 0.020 (3) | 0.004 (4) | 0.008 (3) | 0.008 (3) |
O21 | 0.024 (4) | 0.009 (3) | 0.033 (4) | −0.002 (3) | 0.003 (4) | −0.007 (3) |
O22 | 0.038 (5) | 0.015 (4) | 0.038 (4) | −0.006 (4) | 0.003 (4) | 0.004 (3) |
O23 | 0.044 (4) | 0.041 (3) | 0.007 (2) | 0.000 (3) | −0.001 (4) | −0.004 (4) |
O24 | 0.041 (4) | 0.036 (3) | 0.010 (3) | −0.011 (3) | 0.003 (3) | −0.004 (4) |
O25 | 0.028 (3) | 0.030 (3) | 0.010 (2) | 0.000 (2) | 0.000 (4) | 0.008 (3) |
O26 | 0.023 (3) | 0.028 (3) | 0.013 (3) | −0.002 (2) | 0.003 (4) | −0.001 (4) |
O27 | 0.034 (4) | 0.018 (4) | 0.060 (5) | −0.014 (3) | −0.003 (5) | −0.004 (4) |
O28 | 0.016 (3) | 0.018 (3) | 0.045 (4) | −0.002 (3) | 0.012 (3) | −0.004 (4) |
O29 | 0.063 (5) | 0.009 (3) | 0.038 (4) | −0.001 (3) | 0.002 (3) | 0.000 (3) |
O30 | 0.015 (4) | 0.031 (4) | 0.054 (4) | 0.011 (3) | 0.015 (4) | 0.001 (4) |
O31 | 0.046 (5) | 0.024 (4) | 0.013 (3) | −0.015 (3) | −0.007 (3) | 0.006 (3) |
O32 | 0.044 (4) | 0.020 (3) | 0.040 (4) | 0.014 (3) | 0.006 (4) | 0.007 (4) |
O33 | 0.023 (4) | 0.015 (4) | 0.045 (5) | −0.007 (3) | 0.009 (4) | 0.004 (3) |
O34 | 0.026 (4) | 0.011 (3) | 0.035 (4) | −0.005 (3) | −0.006 (3) | −0.008 (3) |
O35 | 0.054 (5) | 0.005 (3) | 0.026 (4) | −0.003 (4) | −0.002 (3) | 0.001 (3) |
O36 | 0.039 (5) | 0.032 (4) | 0.059 (5) | 0.021 (4) | −0.023 (4) | −0.004 (4) |
O37 | 0.061 (6) | 0.019 (4) | 0.023 (4) | −0.007 (4) | 0.019 (4) | 0.002 (3) |
O38 | 0.047 (5) | 0.016 (3) | 0.047 (4) | 0.010 (3) | 0.012 (4) | −0.010 (3) |
O39 | 0.040 (4) | 0.088 (5) | 0.015 (3) | 0.002 (4) | 0.000 (4) | −0.004 (5) |
O40 | 0.056 (5) | 0.036 (4) | 0.011 (3) | −0.011 (3) | 0.001 (4) | −0.001 (3) |
O41 | 0.045 (5) | 0.026 (4) | 0.026 (4) | 0.015 (4) | −0.019 (4) | 0.000 (3) |
O42 | 0.028 (4) | 0.035 (4) | 0.028 (4) | 0.014 (3) | 0.012 (3) | −0.006 (3) |
O43 | 0.033 (4) | 0.041 (4) | 0.010 (3) | 0.008 (4) | −0.005 (4) | 0.006 (3) |
O44 | 0.035 (4) | 0.025 (3) | 0.016 (3) | −0.009 (3) | −0.015 (3) | −0.002 (3) |
O45 | 0.039 (4) | 0.028 (4) | 0.034 (4) | −0.008 (4) | 0.017 (3) | 0.007 (3) |
O46 | 0.025 (4) | 0.070 (5) | 0.022 (4) | 0.006 (4) | −0.008 (3) | 0.010 (4) |
O47 | 0.019 (4) | 0.013 (3) | 0.034 (4) | −0.001 (3) | 0.007 (3) | 0.010 (3) |
O48 | 0.038 (5) | 0.011 (4) | 0.050 (5) | 0.006 (4) | −0.003 (4) | −0.005 (3) |
Geometric parameters (Å, º) top
C101—C102i | 1.29 (9) | Si13—O41 | 1.590 (8) |
C101—O103 | 1.4125 | Si13—O21iii | 1.592 (7) |
C102—O103i | 1.01 (8) | Si13—O42 | 1.590 (7) |
C102—C102i | 1.10 (10) | Si14—O27 | 1.597 (7) |
C102—C101i | 1.29 (9) | Si14—O32 | 1.602 (7) |
C102—O103 | 1.4047 | Si14—O28 | 1.605 (6) |
O103—C102i | 1.01 (7) | Si14—O39 | 1.607 (6) |
C201—O203ii | 1.07 (5) | Si15—O19v | 1.574 (7) |
C201—C201ii | 1.38 (5) | Si15—O29 | 1.581 (7) |
C201—O203 | 1.4098 | Si15—O20v | 1.585 (6) |
C202—O203 | 1.4080 | Si15—O28 | 1.587 (6) |
O203—C201ii | 1.07 (7) | Si16—O30 | 1.565 (6) |
C301—O303 | 1.3933 | Si16—O16v | 1.581 (7) |
C302—O303 | 1.3912 | Si16—O29 | 1.591 (7) |
Si1—O15 | 1.567 (7) | Si16—O17v | 1.610 (7) |
Si1—O1 | 1.581 (7) | Si17—O40 | 1.577 (7) |
Si1—O47iii | 1.586 (7) | Si17—O47 | 1.588 (7) |
Si1—O16 | 1.601 (8) | Si17—O31 | 1.616 (7) |
Si2—O13 | 1.575 (6) | Si17—O30 | 1.612 (7) |
Si2—O6 | 1.578 (7) | Si18—O31 | 1.580 (7) |
Si2—O1 | 1.593 (7) | Si18—O45 | 1.583 (7) |
Si2—O2 | 1.608 (6) | Si18—O32 | 1.588 (7) |
Si3—O2 | 1.578 (6) | Si18—O44 | 1.594 (7) |
Si3—O3 | 1.578 (7) | Si19—O33 | 1.579 (8) |
Si3—O46 | 1.584 (7) | Si19—O22iii | 1.587 (7) |
Si3—O45iv | 1.620 (7) | Si19—O23 | 1.588 (8) |
Si4—O43iv | 1.575 (7) | Si19—O43 | 1.612 (7) |
Si4—O4 | 1.586 (7) | Si20—O39 | 1.570 (7) |
Si4—O42iv | 1.590 (7) | Si20—O34 | 1.580 (7) |
Si4—O3 | 1.601 (7) | Si20—O33 | 1.593 (7) |
Si5—O5 | 1.581 (7) | Si20—O38 | 1.606 (7) |
Si5—O21 | 1.591 (6) | Si21—O25 | 1.593 (6) |
Si5—O14 | 1.598 (6) | Si21—O18v | 1.592 (7) |
Si5—O4 | 1.610 (7) | Si21—O35 | 1.607 (7) |
Si6—O19 | 1.597 (7) | Si21—O34 | 1.609 (7) |
Si6—O6 | 1.599 (7) | Si22—O15v | 1.578 (8) |
Si6—O18 | 1.600 (7) | Si22—O26 | 1.594 (8) |
Si6—O5 | 1.605 (7) | Si22—O36 | 1.602 (8) |
Si7—O17 | 1.582 (7) | Si22—O35 | 1.616 (7) |
Si7—O23 | 1.593 (8) | Si23—O36 | 1.564 (8) |
Si7—O48iii | 1.601 (7) | Si23—O48 | 1.586 (7) |
Si7—O7 | 1.607 (8) | Si23—O40 | 1.609 (7) |
Si8—O12 | 1.587 (7) | Si23—O37 | 1.610 (7) |
Si8—O7 | 1.590 (7) | Si24—O37 | 1.575 (7) |
Si8—O13 | 1.593 (7) | Si24—O38 | 1.575 (7) |
Si8—O8 | 1.590 (7) | Si24—O24 | 1.599 (6) |
Si9—O8 | 1.571 (7) | Si24—O46vi | 1.617 (7) |
Si9—O44iv | 1.598 (7) | O15—Si22vii | 1.578 (8) |
Si9—O25 | 1.597 (6) | O16—Si16vii | 1.581 (7) |
Si9—O9 | 1.606 (7) | O17—Si16vii | 1.610 (7) |
Si10—O10 | 1.578 (7) | O18—Si21vii | 1.592 (7) |
Si10—O9 | 1.589 (7) | O19—Si15vii | 1.574 (7) |
Si10—O41iv | 1.614 (7) | O20—Si15vii | 1.585 (6) |
Si10—O26 | 1.618 (8) | O21—Si13viii | 1.592 (7) |
Si11—O11 | 1.573 (8) | O22—Si19viii | 1.587 (7) |
Si11—O14 | 1.581 (7) | O41—Si10vi | 1.614 (7) |
Si11—O10 | 1.594 (7) | O42—Si4vi | 1.590 (7) |
Si11—O22 | 1.605 (7) | O43—Si4vi | 1.575 (7) |
Si12—O24 | 1.581 (6) | O44—Si9vi | 1.598 (7) |
Si12—O12 | 1.589 (7) | O45—Si3vi | 1.620 (7) |
Si12—O20 | 1.597 (6) | O46—Si24iv | 1.617 (7) |
Si12—O11 | 1.607 (7) | O47—Si1viii | 1.586 (6) |
Si13—O27 | 1.583 (7) | O48—Si7viii | 1.601 (7) |
| | | |
C102i—C101—O103 | 44 (4) | O29—Si15—O28 | 109.1 (4) |
O103i—C102—C102i | 83 (8) | O20v—Si15—O28 | 107.3 (4) |
O103i—C102—C101i | 75 (5) | O30—Si16—O16v | 109.4 (4) |
C102i—C102—C101i | 155 (8) | O30—Si16—O29 | 110.6 (4) |
O103i—C102—O103 | 129 (6) | O16v—Si16—O29 | 110.5 (4) |
C102i—C102—O103 | 46 (4) | O30—Si16—O17v | 108.2 (4) |
C101i—C102—O103 | 154 (3) | O16v—Si16—O17v | 108.7 (4) |
C102i—O103—C102 | 51 (6) | O29—Si16—O17v | 109.5 (4) |
C102i—O103—C101 | 62 (6) | O40—Si17—O47 | 111.3 (4) |
C102—O103—C101 | 111.7 | O40—Si17—O31 | 109.0 (4) |
O203ii—C201—C201ii | 69 (2) | O47—Si17—O31 | 109.6 (4) |
O203ii—C201—O203 | 114 (4) | O40—Si17—O30 | 108.8 (4) |
C201ii—C201—O203 | 45 (3) | O47—Si17—O30 | 108.0 (4) |
C201ii—O203—C202 | 171 (3) | O31—Si17—O30 | 110.1 (4) |
C201ii—O203—C201 | 66 (4) | O31—Si18—O45 | 109.0 (4) |
C202—O203—C201 | 111.7 | O31—Si18—O32 | 110.0 (4) |
C302—O303—C301 | 111.8 | O45—Si18—O32 | 109.6 (4) |
O15—Si1—O1 | 108.7 (4) | O31—Si18—O44 | 107.0 (4) |
O15—Si1—O47iii | 110.6 (4) | O45—Si18—O44 | 110.9 (4) |
O1—Si1—O47iii | 108.3 (4) | O32—Si18—O44 | 110.3 (4) |
O15—Si1—O16 | 110.4 (4) | O33—Si19—O22iii | 107.4 (4) |
O1—Si1—O16 | 109.0 (4) | O33—Si19—O23 | 110.7 (4) |
O47iii—Si1—O16 | 109.8 (4) | O22iii—Si19—O23 | 111.0 (3) |
O13—Si2—O6 | 108.7 (4) | O33—Si19—O43 | 109.7 (4) |
O13—Si2—O1 | 109.8 (4) | O22iii—Si19—O43 | 110.3 (4) |
O6—Si2—O1 | 110.0 (4) | O23—Si19—O43 | 107.9 (4) |
O13—Si2—O2 | 110.1 (4) | O39—Si20—O34 | 111.0 (4) |
O6—Si2—O2 | 109.7 (4) | O39—Si20—O33 | 109.8 (4) |
O1—Si2—O2 | 108.5 (4) | O34—Si20—O33 | 109.1 (4) |
O2—Si3—O3 | 110.8 (4) | O39—Si20—O38 | 108.2 (4) |
O2—Si3—O46 | 108.0 (4) | O34—Si20—O38 | 109.2 (4) |
O3—Si3—O46 | 109.4 (4) | O33—Si20—O38 | 109.5 (4) |
O2—Si3—O45iv | 110.3 (4) | O25—Si21—O18v | 106.9 (3) |
O3—Si3—O45iv | 108.9 (4) | O25—Si21—O35 | 110.6 (3) |
O46—Si3—O45iv | 109.5 (4) | O18v—Si21—O35 | 109.4 (4) |
O43iv—Si4—O4 | 109.5 (4) | O25—Si21—O34 | 111.0 (3) |
O43iv—Si4—O42iv | 110.0 (4) | O18v—Si21—O34 | 110.0 (4) |
O4—Si4—O42iv | 109.3 (4) | O35—Si21—O34 | 108.8 (4) |
O43iv—Si4—O3 | 109.9 (4) | O15v—Si22—O26 | 108.6 (4) |
O4—Si4—O3 | 110.0 (4) | O15v—Si22—O36 | 110.3 (4) |
O42iv—Si4—O3 | 108.2 (4) | O26—Si22—O36 | 110.3 (4) |
O5—Si5—O21 | 107.2 (4) | O15v—Si22—O35 | 109.2 (4) |
O5—Si5—O14 | 110.2 (4) | O26—Si22—O35 | 110.8 (3) |
O21—Si5—O14 | 110.3 (4) | O36—Si22—O35 | 107.8 (4) |
O5—Si5—O4 | 110.3 (4) | O36—Si23—O48 | 108.7 (4) |
O21—Si5—O4 | 110.4 (4) | O36—Si23—O40 | 109.4 (4) |
O14—Si5—O4 | 108.5 (4) | O48—Si23—O40 | 111.1 (4) |
O19—Si6—O6 | 111.6 (4) | O36—Si23—O37 | 110.9 (4) |
O19—Si6—O18 | 108.0 (4) | O48—Si23—O37 | 108.2 (4) |
O6—Si6—O18 | 109.3 (4) | O40—Si23—O37 | 108.5 (4) |
O19—Si6—O5 | 110.5 (4) | O37—Si24—O38 | 110.2 (4) |
O6—Si6—O5 | 108.9 (4) | O37—Si24—O24 | 109.3 (3) |
O18—Si6—O5 | 108.5 (4) | O38—Si24—O24 | 108.5 (4) |
O17—Si7—O23 | 107.5 (4) | O37—Si24—O46vi | 111.5 (4) |
O17—Si7—O48iii | 110.2 (4) | O38—Si24—O46vi | 110.2 (4) |
O23—Si7—O48iii | 110.5 (4) | O24—Si24—O46vi | 107.1 (4) |
O17—Si7—O7 | 111.2 (4) | Si1—O1—Si2 | 147.6 (5) |
O23—Si7—O7 | 110.1 (4) | Si3—O2—Si2 | 146.2 (4) |
O48iii—Si7—O7 | 107.5 (4) | Si3—O3—Si4 | 162.3 (5) |
O12—Si8—O7 | 111.6 (4) | Si4—O4—Si5 | 149.0 (4) |
O12—Si8—O13 | 108.5 (4) | Si5—O5—Si6 | 148.1 (5) |
O7—Si8—O13 | 108.7 (4) | Si2—O6—Si6 | 162.4 (5) |
O12—Si8—O8 | 110.5 (4) | Si8—O7—Si7 | 156.2 (6) |
O7—Si8—O8 | 106.8 (4) | Si9—O8—Si8 | 153.2 (5) |
O13—Si8—O8 | 110.7 (4) | Si10—O9—Si9 | 151.4 (4) |
O8—Si9—O44iv | 110.6 (4) | Si10—O10—Si11 | 156.7 (5) |
O8—Si9—O25 | 108.2 (3) | Si11—O11—Si12 | 154.7 (5) |
O44iv—Si9—O25 | 109.0 (3) | Si8—O12—Si12 | 168.8 (5) |
O8—Si9—O9 | 108.5 (4) | Si2—O13—Si8 | 163.7 (5) |
O44iv—Si9—O9 | 109.2 (4) | Si11—O14—Si5 | 160.2 (5) |
O25—Si9—O9 | 111.3 (3) | Si1—O15—Si22vii | 150.8 (5) |
O10—Si10—O9 | 109.6 (4) | Si16vii—O16—Si1 | 174.8 (6) |
O10—Si10—O41iv | 110.4 (4) | Si7—O17—Si16vii | 146.8 (5) |
O9—Si10—O41iv | 109.7 (4) | Si21vii—O18—Si6 | 142.2 (5) |
O10—Si10—O26 | 109.0 (3) | Si15vii—O19—Si6 | 167.0 (5) |
O9—Si10—O26 | 110.8 (3) | Si15vii—O20—Si12 | 142.8 (4) |
O41iv—Si10—O26 | 107.3 (4) | Si5—O21—Si13viii | 146.3 (5) |
O11—Si11—O14 | 109.8 (4) | Si19viii—O22—Si11 | 151.1 (5) |
O11—Si11—O10 | 111.5 (4) | Si19—O23—Si7 | 155.2 (4) |
O14—Si11—O10 | 108.0 (4) | Si12—O24—Si24 | 149.4 (4) |
O11—Si11—O22 | 108.3 (4) | Si21—O25—Si9 | 151.0 (3) |
O14—Si11—O22 | 109.8 (4) | Si22—O26—Si10 | 144.7 (3) |
O10—Si11—O22 | 109.4 (4) | Si13—O27—Si14 | 154.5 (5) |
O24—Si12—O12 | 111.6 (4) | Si15—O28—Si14 | 149.0 (4) |
O24—Si12—O20 | 107.0 (3) | Si15—O29—Si16 | 162.1 (5) |
O12—Si12—O20 | 109.2 (4) | Si16—O30—Si17 | 157.4 (5) |
O24—Si12—O11 | 110.9 (4) | Si18—O31—Si17 | 147.4 (4) |
O12—Si12—O11 | 108.6 (4) | Si18—O32—Si14 | 158.2 (5) |
O20—Si12—O11 | 109.5 (4) | Si19—O33—Si20 | 152.1 (5) |
O27—Si13—O41 | 109.8 (4) | Si20—O34—Si21 | 147.6 (4) |
O27—Si13—O21iii | 110.5 (4) | Si21—O35—Si22 | 151.2 (4) |
O41—Si13—O21iii | 107.5 (4) | Si23—O36—Si22 | 161.4 (5) |
O27—Si13—O42 | 110.8 (4) | Si24—O37—Si23 | 152.7 (5) |
O41—Si13—O42 | 109.5 (4) | Si24—O38—Si20 | 155.9 (5) |
O21iii—Si13—O42 | 108.7 (4) | Si20—O39—Si14 | 165.5 (5) |
O27—Si14—O32 | 108.5 (4) | Si17—O40—Si23 | 160.2 (4) |
O27—Si14—O28 | 108.3 (4) | Si13—O41—Si10vi | 149.3 (5) |
O32—Si14—O28 | 109.3 (4) | Si4vi—O42—Si13 | 158.5 (5) |
O27—Si14—O39 | 111.1 (4) | Si4vi—O43—Si19 | 151.2 (5) |
O32—Si14—O39 | 108.1 (4) | Si18—O44—Si9vi | 150.2 (5) |
O28—Si14—O39 | 111.5 (4) | Si18—O45—Si3vi | 154.9 (5) |
O19v—Si15—O29 | 109.2 (4) | Si3—O46—Si24iv | 153.6 (5) |
O19v—Si15—O20v | 111.5 (4) | Si1viii—O47—Si17 | 149.8 (5) |
O29—Si15—O20v | 110.1 (4) | Si23—O48—Si7viii | 149.0 (6) |
O19v—Si15—O28 | 109.6 (4) | | |
Symmetry codes: (i) −x, −y+1, −z; (ii) −x+1, −y, −z; (iii) −x+1/2, y+1/2, −z+1/2; (iv) x−1/2, −y+1/2, z−1/2; (v) x−1/2, −y+1/2, z+1/2; (vi) x+1/2, −y+1/2, z+1/2; (vii) x+1/2, −y+1/2, z−1/2; (viii) −x+1/2, y−1/2, −z+1/2. |
Crystal data top
C0.4O48.2Si24 | F(000) = 2984 |
Mr = 1449.1 | Dx = 1.843 Mg m−3 |
Monoclinic, P21/n | Mo Kα radiation, λ = 0.71073 Å |
a = 13.383 (2) Å | Cell parameters from 7648 reflections |
b = 20.108 (3) Å | θ = 2.3–27.6° |
c = 19.877 (3) Å | µ = 0.68 mm−1 |
β = 90.003 (2)° | T = 296 K |
V = 5349.0 (14) Å3 | Coffin shape, colorless |
Z = 4 | 0.23 × 0.13 × 0.08 mm |
Data collection top
CCD area detector diffractometer | 12004 independent reflections |
Radiation source: fine-focus sealed tube | 9577 reflections with I > 2σ(I) |
Graphite monochromator | Rint = 0.115 |
phi and ω scans | θmax = 27.8°, θmin = 1.0° |
Absorption correction: analytical ? | h = −17→17 |
Tmin = 0.860, Tmax = 0.948 | k = −26→26 |
58608 measured reflections | l = −26→26 |
Refinement top
Refinement on F2 | 2 restraints |
Least-squares matrix: full | Primary atom site location: structure-invariant direct methods |
R[F2 > 2σ(F2)] = 0.060 | Secondary atom site location: difference Fourier map |
wR(F2) = 0.198 | w = 1/[σ2(Fo2) + (0.1204P)2] where P = (Fo2 + 2Fc2)/3 |
S = 1.11 | (Δ/σ)max = 0.001 |
12004 reflections | Δρmax = 0.94 e Å−3 |
660 parameters | Δρmin = −1.00 e Å−3 |
Crystal data top
C0.4O48.2Si24 | V = 5349.0 (14) Å3 |
Mr = 1449.1 | Z = 4 |
Monoclinic, P21/n | Mo Kα radiation |
a = 13.383 (2) Å | µ = 0.68 mm−1 |
b = 20.108 (3) Å | T = 296 K |
c = 19.877 (3) Å | 0.23 × 0.13 × 0.08 mm |
β = 90.003 (2)° | |
Data collection top
CCD area detector diffractometer | 12004 independent reflections |
Absorption correction: analytical ? | 9577 reflections with I > 2σ(I) |
Tmin = 0.860, Tmax = 0.948 | Rint = 0.115 |
58608 measured reflections | |
Refinement top
R[F2 > 2σ(F2)] = 0.060 | 660 parameters |
wR(F2) = 0.198 | 2 restraints |
S = 1.11 | Δρmax = 0.94 e Å−3 |
12004 reflections | Δρmin = −1.00 e Å−3 |
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 | x | y | z | Uiso*/Ueq | Occ. (<1) |
C301 | 0.159 (9) | 0.262 (4) | 0.746 (7) | 0.29 (7)* | 0.174 (16) |
C302 | 0.143 (9) | 0.147 (4) | 0.737 (6) | 0.27 (6)* | 0.174 (16) |
O303 | 0.095 (6) | 0.207 (5) | 0.754 (5) | 0.30 (5)* | 0.174 (16) |
Si1 | 0.32240 (11) | 0.42074 (5) | −0.05594 (6) | 0.0211 (3) | |
Si2 | 0.16808 (12) | 0.31244 (6) | −0.03029 (7) | 0.0232 (3) | |
Si3 | −0.04987 (11) | 0.27969 (6) | −0.06242 (6) | 0.0230 (3) | |
Si4 | −0.03521 (10) | 0.12365 (6) | −0.06277 (6) | 0.0220 (3) | |
Si5 | 0.17758 (11) | 0.07591 (6) | −0.02821 (6) | 0.0203 (3) | |
Si6 | 0.31602 (12) | 0.19390 (5) | −0.05614 (7) | 0.0226 (3) | |
Si7 | 0.32036 (12) | 0.42498 (6) | 0.17153 (6) | 0.0218 (3) | |
Si8 | 0.17549 (12) | 0.31142 (5) | 0.12726 (7) | 0.0219 (3) | |
Si9 | −0.03521 (11) | 0.27358 (6) | 0.17561 (6) | 0.0212 (3) | |
Si10 | −0.03273 (11) | 0.11929 (6) | 0.17567 (6) | 0.0229 (3) | |
Si11 | 0.17695 (11) | 0.07147 (6) | 0.12946 (6) | 0.0214 (3) | |
Si12 | 0.31544 (12) | 0.19019 (5) | 0.16655 (7) | 0.0219 (3) | |
Si13 | 0.33551 (11) | 0.42748 (5) | 0.55742 (6) | 0.0207 (3) | |
Si14 | 0.18859 (12) | 0.31177 (6) | 0.52760 (7) | 0.0235 (3) | |
Si15 | −0.02929 (10) | 0.27755 (6) | 0.56132 (6) | 0.0210 (3) | |
Si16 | −0.03272 (10) | 0.12167 (6) | 0.56403 (6) | 0.0212 (3) | |
Si17 | 0.17970 (11) | 0.07081 (5) | 0.52754 (6) | 0.0204 (3) | |
Si18 | 0.31959 (12) | 0.18725 (5) | 0.56202 (7) | 0.0227 (3) | |
Si19 | 0.31598 (11) | 0.42397 (6) | 0.32787 (6) | 0.0215 (3) | |
Si20 | 0.17168 (12) | 0.31206 (6) | 0.36934 (7) | 0.0232 (3) | |
Si21 | −0.04318 (11) | 0.27334 (6) | 0.33071 (6) | 0.0223 (3) | |
Si22 | −0.03687 (11) | 0.11893 (6) | 0.32941 (6) | 0.0227 (3) | |
Si23 | 0.17850 (12) | 0.07206 (5) | 0.36965 (6) | 0.0220 (3) | |
Si24 | 0.30149 (12) | 0.19306 (5) | 0.32080 (6) | 0.0218 (3) | |
O1 | 0.2240 (3) | 0.37691 (16) | −0.0581 (2) | 0.0440 (10) | |
O2 | 0.0611 (3) | 0.30984 (16) | −0.06558 (19) | 0.0366 (9) | |
O3 | −0.0430 (4) | 0.20109 (15) | −0.0495 (2) | 0.0479 (12) | |
O4 | 0.0796 (3) | 0.10269 (18) | −0.06668 (17) | 0.0357 (8) | |
O5 | 0.2712 (3) | 0.12151 (15) | −0.04626 (18) | 0.0346 (9) | |
O6 | 0.2293 (3) | 0.24733 (17) | −0.0478 (2) | 0.0470 (11) | |
O7 | 0.2298 (3) | 0.37654 (18) | 0.1535 (2) | 0.0465 (11) | |
O8 | 0.0726 (3) | 0.30536 (17) | 0.1650 (2) | 0.0427 (11) | |
O9 | −0.0311 (4) | 0.19582 (15) | 0.15593 (19) | 0.0417 (11) | |
O10 | 0.0777 (3) | 0.08964 (19) | 0.1686 (2) | 0.0448 (10) | |
O11 | 0.2656 (3) | 0.12017 (18) | 0.15168 (19) | 0.0442 (11) | |
O12 | 0.2431 (3) | 0.24789 (19) | 0.1401 (2) | 0.0489 (11) | |
O13 | 0.1538 (4) | 0.3173 (2) | 0.0488 (2) | 0.0571 (13) | |
O14 | 0.1563 (3) | 0.07806 (17) | 0.05067 (17) | 0.0401 (9) | |
O15 | 0.3786 (3) | 0.41497 (18) | −0.12571 (17) | 0.0412 (10) | |
O16 | 0.3928 (3) | 0.3947 (2) | 0.00394 (18) | 0.0468 (10) | |
O17 | 0.4191 (3) | 0.40122 (18) | 0.13383 (17) | 0.0360 (9) | |
O18 | 0.3625 (3) | 0.19891 (17) | −0.12977 (19) | 0.0328 (9) | |
O19 | 0.4025 (4) | 0.2071 (2) | −0.00185 (19) | 0.0448 (10) | |
O20 | 0.4197 (3) | 0.19565 (17) | 0.12860 (19) | 0.0371 (10) | |
O21 | 0.2043 (3) | 0.00237 (14) | −0.05178 (17) | 0.0308 (8) | |
O22 | 0.2096 (3) | −0.00269 (16) | 0.14745 (18) | 0.0385 (9) | |
O23 | 0.3438 (3) | 0.42372 (18) | 0.25025 (17) | 0.0413 (9) | |
O24 | 0.3386 (3) | 0.19730 (15) | 0.24468 (17) | 0.0360 (9) | |
O25 | −0.0658 (3) | 0.28277 (16) | 0.25273 (17) | 0.0338 (8) | |
O26 | −0.0675 (3) | 0.11022 (15) | 0.25229 (16) | 0.0320 (8) | |
O27 | 0.2425 (3) | 0.37850 (17) | 0.5513 (2) | 0.0473 (11) | |
O28 | 0.0759 (3) | 0.31395 (15) | 0.5530 (2) | 0.0370 (10) | |
O29 | −0.0105 (4) | 0.19865 (15) | 0.5663 (2) | 0.0447 (11) | |
O30 | 0.0696 (3) | 0.08322 (18) | 0.5549 (2) | 0.0433 (10) | |
O31 | 0.2568 (3) | 0.11938 (16) | 0.56444 (16) | 0.0343 (9) | |
O32 | 0.2458 (3) | 0.24965 (17) | 0.5593 (2) | 0.0436 (10) | |
O33 | 0.2207 (3) | 0.37888 (17) | 0.34191 (19) | 0.0400 (10) | |
O34 | 0.0548 (3) | 0.31404 (16) | 0.35410 (19) | 0.0340 (9) | |
O35 | −0.0258 (4) | 0.19600 (14) | 0.34814 (18) | 0.0377 (10) | |
O36 | 0.0677 (4) | 0.0835 (2) | 0.3437 (2) | 0.0521 (12) | |
O37 | 0.2530 (4) | 0.12172 (17) | 0.33361 (19) | 0.0466 (11) | |
O38 | 0.2202 (3) | 0.24879 (18) | 0.3331 (2) | 0.0472 (11) | |
O39 | 0.1920 (4) | 0.3058 (2) | 0.4485 (2) | 0.0562 (13) | |
O40 | 0.1830 (3) | 0.08423 (17) | 0.44890 (17) | 0.0438 (10) | |
O41 | 0.3902 (3) | 0.41850 (18) | 0.62854 (17) | 0.0427 (10) | |
O42 | 0.4137 (3) | 0.41417 (18) | 0.49893 (17) | 0.0378 (9) | |
O43 | 0.4109 (3) | 0.39549 (19) | 0.36843 (17) | 0.0384 (9) | |
O44 | 0.3854 (3) | 0.18978 (16) | 0.62968 (19) | 0.0354 (10) | |
O45 | 0.3901 (4) | 0.18733 (17) | 0.4981 (2) | 0.0405 (10) | |
O46 | −0.1056 (4) | 0.2954 (2) | −0.1318 (2) | 0.0496 (11) | |
O47 | 0.2102 (3) | −0.00449 (15) | 0.54394 (18) | 0.0341 (9) | |
O48 | 0.2116 (3) | −0.00200 (16) | 0.35182 (18) | 0.0378 (9) | |
Atomic displacement parameters (Å2) top | U11 | U22 | U33 | U12 | U13 | U23 |
Si1 | 0.0383 (8) | 0.0111 (5) | 0.0139 (5) | −0.0001 (5) | 0.0058 (6) | −0.0018 (4) |
Si2 | 0.0394 (9) | 0.0139 (6) | 0.0163 (6) | −0.0023 (5) | 0.0040 (6) | −0.0011 (4) |
Si3 | 0.0399 (8) | 0.0148 (6) | 0.0142 (6) | 0.0002 (5) | 0.0024 (6) | −0.0007 (5) |
Si4 | 0.0375 (8) | 0.0129 (6) | 0.0157 (6) | −0.0004 (5) | 0.0026 (6) | 0.0002 (5) |
Si5 | 0.0359 (8) | 0.0114 (5) | 0.0138 (6) | −0.0019 (5) | 0.0037 (6) | 0.0006 (4) |
Si6 | 0.0384 (8) | 0.0128 (6) | 0.0165 (6) | −0.0041 (5) | 0.0080 (6) | 0.0000 (4) |
Si7 | 0.0419 (8) | 0.0114 (5) | 0.0123 (6) | −0.0019 (5) | 0.0051 (6) | −0.0009 (4) |
Si8 | 0.0356 (8) | 0.0147 (6) | 0.0154 (6) | −0.0022 (5) | 0.0035 (6) | 0.0001 (4) |
Si9 | 0.0368 (8) | 0.0149 (6) | 0.0120 (6) | 0.0006 (5) | 0.0036 (6) | 0.0014 (4) |
Si10 | 0.0417 (8) | 0.0144 (6) | 0.0127 (6) | 0.0004 (5) | 0.0047 (6) | −0.0018 (4) |
Si11 | 0.0383 (8) | 0.0122 (5) | 0.0137 (6) | −0.0003 (5) | 0.0042 (6) | −0.0006 (4) |
Si12 | 0.0389 (8) | 0.0143 (6) | 0.0125 (6) | −0.0016 (5) | 0.0044 (6) | 0.0001 (4) |
Si13 | 0.0383 (8) | 0.0099 (5) | 0.0139 (6) | 0.0006 (5) | 0.0033 (6) | 0.0003 (4) |
Si14 | 0.0383 (8) | 0.0150 (6) | 0.0172 (6) | −0.0012 (5) | 0.0058 (6) | 0.0013 (4) |
Si15 | 0.0336 (7) | 0.0146 (6) | 0.0149 (6) | 0.0007 (5) | 0.0058 (6) | 0.0011 (5) |
Si16 | 0.0351 (7) | 0.0131 (6) | 0.0154 (6) | −0.0005 (5) | 0.0050 (6) | 0.0002 (5) |
Si17 | 0.0371 (8) | 0.0090 (5) | 0.0151 (6) | −0.0010 (5) | 0.0049 (6) | −0.0004 (4) |
Si18 | 0.0406 (8) | 0.0131 (5) | 0.0144 (6) | −0.0033 (5) | 0.0018 (6) | 0.0011 (4) |
Si19 | 0.0394 (8) | 0.0132 (6) | 0.0120 (6) | −0.0019 (5) | 0.0033 (6) | 0.0005 (4) |
Si20 | 0.0389 (8) | 0.0151 (6) | 0.0155 (6) | −0.0017 (5) | 0.0049 (6) | −0.0002 (5) |
Si21 | 0.0375 (8) | 0.0159 (6) | 0.0137 (6) | −0.0008 (5) | 0.0043 (6) | −0.0017 (5) |
Si22 | 0.0410 (8) | 0.0142 (6) | 0.0128 (6) | −0.0002 (5) | 0.0038 (6) | 0.0019 (4) |
Si23 | 0.0421 (8) | 0.0103 (5) | 0.0136 (6) | −0.0005 (5) | 0.0028 (6) | 0.0002 (4) |
Si24 | 0.0392 (8) | 0.0152 (6) | 0.0112 (6) | −0.0012 (5) | 0.0053 (6) | −0.0015 (4) |
O1 | 0.058 (3) | 0.0213 (17) | 0.053 (2) | −0.0149 (17) | −0.002 (2) | 0.0057 (17) |
O2 | 0.039 (2) | 0.036 (2) | 0.034 (2) | −0.0075 (15) | 0.0023 (18) | 0.0053 (15) |
O3 | 0.075 (3) | 0.0133 (17) | 0.055 (3) | −0.0017 (17) | 0.009 (3) | −0.0021 (16) |
O4 | 0.040 (2) | 0.044 (2) | 0.0235 (18) | 0.0059 (18) | 0.0048 (16) | 0.0036 (15) |
O5 | 0.043 (2) | 0.0164 (16) | 0.044 (2) | −0.0059 (15) | 0.0069 (18) | 0.0029 (15) |
O6 | 0.056 (3) | 0.0193 (17) | 0.066 (3) | 0.0087 (17) | 0.015 (2) | −0.0031 (18) |
O7 | 0.056 (3) | 0.0259 (19) | 0.058 (3) | −0.0154 (19) | 0.002 (2) | −0.0089 (17) |
O8 | 0.040 (2) | 0.043 (2) | 0.045 (3) | −0.0076 (17) | 0.017 (2) | −0.0045 (17) |
O9 | 0.080 (3) | 0.0160 (18) | 0.029 (2) | 0.0016 (17) | 0.010 (2) | 0.0011 (13) |
O10 | 0.051 (3) | 0.048 (2) | 0.036 (2) | 0.017 (2) | 0.019 (2) | 0.0075 (17) |
O11 | 0.061 (3) | 0.0228 (18) | 0.049 (2) | −0.0113 (18) | −0.007 (2) | −0.0069 (16) |
O12 | 0.060 (3) | 0.029 (2) | 0.057 (3) | 0.0161 (19) | 0.002 (2) | 0.0053 (18) |
O13 | 0.089 (4) | 0.066 (3) | 0.0162 (19) | 0.008 (2) | 0.005 (2) | −0.0004 (18) |
O14 | 0.063 (3) | 0.040 (2) | 0.0173 (17) | 0.0009 (18) | 0.0030 (19) | −0.0009 (15) |
O15 | 0.061 (3) | 0.042 (2) | 0.0206 (18) | 0.0183 (19) | 0.0177 (19) | 0.0000 (16) |
O16 | 0.056 (3) | 0.059 (3) | 0.0256 (19) | 0.010 (2) | −0.0087 (19) | 0.0060 (18) |
O17 | 0.045 (2) | 0.041 (2) | 0.0223 (17) | 0.0053 (18) | 0.0134 (17) | −0.0084 (15) |
O18 | 0.035 (2) | 0.044 (2) | 0.0196 (18) | −0.0054 (16) | 0.0114 (17) | 0.0039 (14) |
O19 | 0.053 (3) | 0.055 (2) | 0.026 (2) | −0.017 (2) | −0.0068 (19) | −0.0039 (17) |
O20 | 0.046 (3) | 0.043 (2) | 0.0220 (19) | −0.0006 (17) | 0.0159 (19) | 0.0090 (15) |
O21 | 0.047 (2) | 0.0129 (15) | 0.0324 (18) | −0.0016 (14) | 0.0059 (18) | −0.0047 (13) |
O22 | 0.051 (2) | 0.0179 (17) | 0.047 (2) | 0.0002 (17) | 0.0050 (19) | 0.0063 (15) |
O23 | 0.058 (2) | 0.053 (2) | 0.0130 (15) | 0.0038 (18) | 0.007 (2) | 0.0014 (16) |
O24 | 0.054 (3) | 0.039 (2) | 0.0149 (17) | −0.0139 (16) | 0.0113 (19) | −0.0014 (14) |
O25 | 0.054 (2) | 0.0340 (17) | 0.0141 (15) | 0.0051 (16) | 0.0086 (18) | 0.0010 (14) |
O26 | 0.048 (2) | 0.0345 (17) | 0.0131 (14) | −0.0016 (15) | 0.0088 (17) | −0.0002 (14) |
O27 | 0.043 (2) | 0.0242 (19) | 0.074 (3) | −0.0114 (17) | 0.008 (2) | −0.0100 (19) |
O28 | 0.042 (2) | 0.0241 (18) | 0.045 (2) | −0.0071 (15) | 0.017 (2) | −0.0039 (16) |
O29 | 0.065 (3) | 0.0145 (17) | 0.054 (3) | −0.0055 (16) | 0.004 (2) | 0.0050 (16) |
O30 | 0.038 (2) | 0.0354 (19) | 0.056 (3) | 0.0096 (17) | 0.019 (2) | 0.0048 (18) |
O31 | 0.060 (3) | 0.0208 (17) | 0.0225 (18) | −0.0158 (16) | −0.0050 (18) | 0.0037 (14) |
O32 | 0.059 (3) | 0.0255 (18) | 0.046 (2) | 0.0106 (17) | 0.010 (2) | 0.0104 (17) |
O33 | 0.051 (2) | 0.0225 (18) | 0.047 (2) | −0.0131 (17) | 0.006 (2) | 0.0069 (16) |
O34 | 0.041 (2) | 0.0211 (17) | 0.040 (2) | −0.0037 (15) | −0.0040 (18) | −0.0032 (14) |
O35 | 0.072 (3) | 0.0147 (17) | 0.026 (2) | −0.0027 (16) | −0.001 (2) | −0.0006 (13) |
O36 | 0.057 (3) | 0.050 (2) | 0.050 (3) | 0.022 (2) | −0.021 (2) | −0.010 (2) |
O37 | 0.078 (3) | 0.0220 (18) | 0.040 (2) | −0.0113 (19) | 0.024 (2) | 0.0030 (16) |
O38 | 0.060 (3) | 0.0251 (19) | 0.057 (2) | 0.0103 (18) | 0.013 (2) | −0.0124 (17) |
O39 | 0.065 (3) | 0.085 (4) | 0.019 (2) | −0.001 (2) | 0.007 (2) | 0.0024 (18) |
O40 | 0.084 (3) | 0.0331 (19) | 0.0148 (16) | −0.003 (2) | 0.004 (2) | 0.0008 (14) |
O41 | 0.071 (3) | 0.039 (2) | 0.0177 (18) | 0.019 (2) | −0.0072 (19) | 0.0009 (15) |
O42 | 0.048 (2) | 0.039 (2) | 0.0269 (19) | 0.0037 (17) | 0.0156 (17) | −0.0066 (15) |
O43 | 0.045 (2) | 0.046 (2) | 0.0247 (18) | 0.0062 (18) | −0.0025 (18) | 0.0018 (16) |
O44 | 0.057 (3) | 0.0283 (19) | 0.0205 (18) | −0.0086 (16) | −0.0096 (19) | 0.0014 (13) |
O45 | 0.061 (3) | 0.031 (2) | 0.030 (2) | −0.0042 (17) | 0.020 (2) | 0.0059 (15) |
O46 | 0.057 (3) | 0.072 (3) | 0.0195 (19) | 0.003 (2) | −0.006 (2) | 0.0058 (18) |
O47 | 0.046 (2) | 0.0117 (15) | 0.045 (2) | −0.0006 (14) | 0.0114 (19) | 0.0043 (14) |
O48 | 0.057 (3) | 0.0143 (16) | 0.042 (2) | 0.0012 (17) | 0.0009 (19) | −0.0071 (14) |
Geometric parameters (Å, º) top
C301—O303 | 1.4069 | Si14—O27 | 1.595 (4) |
C302—O303 | 1.4077 | Si15—O19iii | 1.582 (4) |
Si1—O47i | 1.585 (3) | Si15—O28 | 1.597 (4) |
Si1—O15 | 1.586 (4) | Si15—O20iii | 1.599 (4) |
Si1—O1 | 1.586 (4) | Si15—O29 | 1.610 (3) |
Si1—O16 | 1.605 (4) | Si16—O29 | 1.578 (3) |
Si2—O6 | 1.585 (4) | Si16—O30 | 1.584 (4) |
Si2—O13 | 1.590 (4) | Si16—O16iii | 1.589 (4) |
Si2—O2 | 1.595 (4) | Si16—O17iii | 1.602 (3) |
Si2—O1 | 1.598 (4) | Si17—O40 | 1.590 (4) |
Si3—O45ii | 1.591 (4) | Si17—O30 | 1.593 (4) |
Si3—O46 | 1.599 (4) | Si17—O31 | 1.598 (3) |
Si3—O3 | 1.605 (3) | Si17—O47 | 1.603 (3) |
Si3—O2 | 1.606 (4) | Si18—O45 | 1.587 (4) |
Si4—O3 | 1.584 (3) | Si18—O32 | 1.598 (4) |
Si4—O43ii | 1.593 (4) | Si18—O31 | 1.605 (3) |
Si4—O4 | 1.597 (4) | Si18—O44 | 1.608 (4) |
Si4—O42ii | 1.601 (4) | Si19—O23 | 1.591 (4) |
Si5—O21 | 1.594 (3) | Si19—O33 | 1.591 (4) |
Si5—O5 | 1.595 (4) | Si19—O22i | 1.593 (3) |
Si5—O14 | 1.598 (4) | Si19—O43 | 1.609 (4) |
Si5—O4 | 1.609 (4) | Si20—O33 | 1.594 (3) |
Si6—O5 | 1.588 (3) | Si20—O34 | 1.594 (5) |
Si6—O6 | 1.591 (4) | Si20—O38 | 1.602 (4) |
Si6—O18 | 1.598 (4) | Si20—O39 | 1.604 (4) |
Si6—O19 | 1.603 (4) | Si21—O18iii | 1.591 (4) |
Si7—O7 | 1.595 (4) | Si21—O25 | 1.592 (4) |
Si7—O17 | 1.596 (4) | Si21—O35 | 1.611 (3) |
Si7—O23 | 1.597 (4) | Si21—O34 | 1.613 (4) |
Si7—O48i | 1.599 (3) | Si22—O36 | 1.596 (4) |
Si8—O8 | 1.577 (4) | Si22—O26 | 1.597 (3) |
Si8—O7 | 1.586 (4) | Si22—O15iii | 1.598 (4) |
Si8—O12 | 1.587 (4) | Si22—O35 | 1.602 (3) |
Si8—O13 | 1.592 (4) | Si23—O37 | 1.586 (4) |
Si9—O44ii | 1.582 (4) | Si23—O36 | 1.586 (5) |
Si9—O8 | 1.593 (4) | Si23—O48 | 1.595 (3) |
Si9—O25 | 1.601 (3) | Si23—O40 | 1.598 (4) |
Si9—O9 | 1.614 (3) | Si24—O46iv | 1.576 (5) |
Si10—O41ii | 1.586 (4) | Si24—O38 | 1.583 (4) |
Si10—O9 | 1.590 (3) | Si24—O37 | 1.596 (4) |
Si10—O10 | 1.601 (4) | Si24—O24 | 1.599 (4) |
Si10—O26 | 1.603 (3) | O15—Si22v | 1.598 (4) |
Si11—O10 | 1.586 (4) | O16—Si16v | 1.589 (4) |
Si11—O22 | 1.595 (3) | O17—Si16v | 1.602 (3) |
Si11—O14 | 1.597 (4) | O18—Si21v | 1.591 (4) |
Si11—O11 | 1.600 (4) | O19—Si15v | 1.582 (4) |
Si12—O11 | 1.587 (4) | O20—Si15v | 1.595 (4) |
Si12—O24 | 1.591 (4) | O21—Si13vi | 1.602 (3) |
Si12—O20 | 1.594 (4) | O22—Si19vi | 1.593 (3) |
Si12—O12 | 1.600 (4) | O41—Si10iv | 1.587 (4) |
Si13—O42 | 1.587 (4) | O42—Si4iv | 1.600 (4) |
Si13—O27 | 1.593 (4) | O43—Si4iv | 1.593 (4) |
Si13—O41 | 1.602 (4) | O44—Si9iv | 1.582 (4) |
Si13—O21i | 1.602 (3) | O45—Si3iv | 1.591 (4) |
Si14—O39 | 1.580 (4) | O46—Si24ii | 1.576 (5) |
Si14—O28 | 1.594 (4) | O47—Si1vi | 1.585 (3) |
Si14—O32 | 1.595 (4) | O48—Si7vi | 1.599 (3) |
| | | |
C301—O303—C302 | 111.7 | O40—Si17—O30 | 109.8 (2) |
O47i—Si1—O15 | 109.48 (19) | O40—Si17—O31 | 109.2 (2) |
O47i—Si1—O1 | 107.6 (2) | O30—Si17—O31 | 110.1 (2) |
O15—Si1—O1 | 109.4 (2) | O40—Si17—O47 | 110.69 (19) |
O47i—Si1—O16 | 111.1 (2) | O30—Si17—O47 | 108.3 (2) |
O15—Si1—O16 | 110.3 (2) | O31—Si17—O47 | 108.7 (2) |
O1—Si1—O16 | 108.9 (2) | O45—Si18—O32 | 110.0 (2) |
O6—Si2—O13 | 109.4 (2) | O45—Si18—O31 | 109.8 (2) |
O6—Si2—O2 | 109.9 (2) | O32—Si18—O31 | 110.2 (2) |
O13—Si2—O2 | 109.1 (3) | O45—Si18—O44 | 110.2 (3) |
O6—Si2—O1 | 110.6 (2) | O32—Si18—O44 | 109.9 (2) |
O13—Si2—O1 | 110.6 (2) | O31—Si18—O44 | 106.71 (18) |
O2—Si2—O1 | 107.2 (2) | O23—Si19—O33 | 111.1 (2) |
O45ii—Si3—O46 | 109.6 (3) | O23—Si19—O22i | 110.7 (2) |
O45ii—Si3—O3 | 108.5 (2) | O33—Si19—O22i | 107.5 (2) |
O46—Si3—O3 | 111.0 (2) | O23—Si19—O43 | 107.4 (2) |
O45ii—Si3—O2 | 109.9 (2) | O33—Si19—O43 | 110.0 (2) |
O46—Si3—O2 | 108.7 (2) | O22i—Si19—O43 | 110.2 (2) |
O3—Si3—O2 | 109.0 (2) | O33—Si20—O34 | 108.6 (2) |
O3—Si4—O43ii | 110.6 (2) | O33—Si20—O38 | 110.4 (2) |
O3—Si4—O4 | 109.4 (2) | O34—Si20—O38 | 109.5 (2) |
O43ii—Si4—O4 | 109.1 (2) | O33—Si20—O39 | 109.5 (2) |
O3—Si4—O42ii | 108.1 (2) | O34—Si20—O39 | 110.6 (2) |
O43ii—Si4—O42ii | 110.6 (2) | O38—Si20—O39 | 108.2 (2) |
O4—Si4—O42ii | 109.0 (2) | O18iii—Si21—O25 | 107.0 (2) |
O21—Si5—O5 | 106.91 (19) | O18iii—Si21—O35 | 110.3 (2) |
O21—Si5—O14 | 110.82 (18) | O25—Si21—O35 | 110.60 (19) |
O5—Si5—O14 | 110.4 (2) | O18iii—Si21—O34 | 109.0 (2) |
O21—Si5—O4 | 110.7 (2) | O25—Si21—O34 | 111.9 (2) |
O5—Si5—O4 | 109.86 (19) | O35—Si21—O34 | 108.2 (2) |
O14—Si5—O4 | 108.1 (2) | O36—Si22—O26 | 110.1 (2) |
O5—Si6—O6 | 109.3 (2) | O36—Si22—O15iii | 109.4 (2) |
O5—Si6—O18 | 108.69 (19) | O26—Si22—O15iii | 108.1 (2) |
O6—Si6—O18 | 109.9 (2) | O36—Si22—O35 | 108.1 (2) |
O5—Si6—O19 | 109.9 (2) | O26—Si22—O35 | 110.68 (19) |
O6—Si6—O19 | 110.1 (2) | O15iii—Si22—O35 | 110.4 (2) |
O18—Si6—O19 | 109.0 (2) | O37—Si23—O36 | 110.5 (2) |
O7—Si7—O17 | 110.0 (2) | O37—Si23—O48 | 108.2 (2) |
O7—Si7—O23 | 110.9 (2) | O36—Si23—O48 | 108.9 (2) |
O17—Si7—O23 | 107.3 (2) | O37—Si23—O40 | 109.2 (2) |
O7—Si7—O48i | 107.1 (2) | O36—Si23—O40 | 109.3 (2) |
O17—Si7—O48i | 111.1 (2) | O48—Si23—O40 | 110.7 (2) |
O23—Si7—O48i | 110.6 (2) | O46iv—Si24—O38 | 110.1 (2) |
O8—Si8—O7 | 107.9 (2) | O46iv—Si24—O37 | 111.0 (2) |
O8—Si8—O12 | 111.1 (2) | O38—Si24—O37 | 109.4 (2) |
O7—Si8—O12 | 110.6 (3) | O46iv—Si24—O24 | 108.2 (2) |
O8—Si8—O13 | 108.5 (3) | O38—Si24—O24 | 109.0 (2) |
O7—Si8—O13 | 110.1 (2) | O37—Si24—O24 | 109.12 (19) |
O12—Si8—O13 | 108.6 (2) | Si1—O1—Si2 | 146.3 (3) |
O44ii—Si9—O8 | 110.1 (2) | Si2—O2—Si3 | 145.6 (3) |
O44ii—Si9—O25 | 109.1 (2) | Si4—O3—Si3 | 161.2 (3) |
O8—Si9—O25 | 108.4 (2) | Si4—O4—Si5 | 148.1 (2) |
O44ii—Si9—O9 | 109.6 (2) | Si6—O5—Si5 | 148.6 (3) |
O8—Si9—O9 | 109.0 (2) | Si2—O6—Si6 | 163.7 (3) |
O25—Si9—O9 | 110.72 (19) | Si8—O7—Si7 | 157.8 (3) |
O41ii—Si10—O9 | 109.1 (2) | Si8—O8—Si9 | 152.6 (3) |
O41ii—Si10—O10 | 111.6 (2) | Si10—O9—Si9 | 151.5 (3) |
O9—Si10—O10 | 109.0 (2) | Si11—O10—Si10 | 154.8 (3) |
O41ii—Si10—O26 | 108.5 (2) | Si12—O11—Si11 | 155.1 (3) |
O9—Si10—O26 | 110.43 (19) | Si8—O12—Si12 | 169.1 (3) |
O10—Si10—O26 | 108.2 (2) | Si2—O13—Si8 | 160.9 (4) |
O10—Si11—O22 | 109.5 (2) | Si11—O14—Si5 | 158.8 (3) |
O10—Si11—O14 | 108.7 (2) | Si1—O15—Si22v | 149.3 (3) |
O22—Si11—O14 | 110.14 (19) | Si16v—O16—Si1 | 172.7 (3) |
O10—Si11—O11 | 110.2 (2) | Si7—O17—Si16v | 146.2 (3) |
O22—Si11—O11 | 108.0 (2) | Si21v—O18—Si6 | 142.0 (3) |
O14—Si11—O11 | 110.2 (2) | Si15v—O19—Si6 | 169.0 (3) |
O11—Si12—O24 | 110.04 (19) | Si12—O20—Si15v | 142.9 (3) |
O11—Si12—O20 | 110.0 (2) | Si5—O21—Si13vi | 145.0 (3) |
O24—Si12—O20 | 106.8 (2) | Si19vi—O22—Si11 | 151.3 (3) |
O11—Si12—O12 | 109.2 (2) | Si19—O23—Si7 | 155.1 (3) |
O24—Si12—O12 | 111.9 (2) | Si12—O24—Si24 | 149.5 (3) |
O20—Si12—O12 | 108.9 (2) | Si21—O25—Si9 | 150.8 (3) |
O42—Si13—O27 | 110.9 (2) | Si22—O26—Si10 | 145.7 (2) |
O42—Si13—O41 | 109.1 (2) | Si13—O27—Si14 | 153.7 (3) |
O27—Si13—O41 | 110.6 (2) | Si14—O28—Si15 | 148.9 (2) |
O42—Si13—O21i | 109.05 (19) | Si16—O29—Si15 | 159.5 (4) |
O27—Si13—O21i | 108.5 (2) | Si16—O30—Si17 | 156.5 (3) |
O41—Si13—O21i | 108.59 (19) | Si17—O31—Si18 | 147.6 (2) |
O39—Si14—O28 | 110.5 (3) | Si14—O32—Si18 | 157.7 (3) |
O39—Si14—O32 | 108.6 (2) | Si19—O33—Si20 | 150.8 (3) |
O28—Si14—O32 | 110.5 (2) | Si20—O34—Si21 | 147.0 (2) |
O39—Si14—O27 | 110.1 (2) | Si22—O35—Si21 | 150.7 (3) |
O28—Si14—O27 | 108.1 (2) | Si23—O36—Si22 | 160.4 (3) |
O32—Si14—O27 | 109.1 (3) | Si23—O37—Si24 | 153.6 (3) |
O19iii—Si15—O28 | 109.6 (2) | Si24—O38—Si20 | 156.0 (3) |
O19iii—Si15—O20iii | 110.6 (2) | Si14—O39—Si20 | 165.6 (4) |
O28—Si15—O20iii | 108.1 (2) | Si17—O40—Si23 | 161.0 (3) |
O19iii—Si15—O29 | 109.3 (2) | Si10iv—O41—Si13 | 150.6 (3) |
O28—Si15—O29 | 108.7 (2) | Si13—O42—Si4iv | 157.7 (3) |
O20iii—Si15—O29 | 110.4 (2) | Si4iv—O43—Si19 | 150.7 (3) |
O29—Si16—O30 | 108.6 (2) | Si9iv—O44—Si18 | 149.8 (2) |
O29—Si16—O16iii | 110.0 (2) | Si18—O45—Si3iv | 155.3 (3) |
O30—Si16—O16iii | 110.7 (2) | Si24ii—O46—Si3 | 155.6 (3) |
O29—Si16—O17iii | 109.5 (2) | Si1vi—O47—Si17 | 149.1 (3) |
O30—Si16—O17iii | 108.1 (2) | Si23—O48—Si7vi | 148.1 (3) |
O16iii—Si16—O17iii | 109.9 (2) | | |
Symmetry codes: (i) −x+1/2, y+1/2, −z+1/2; (ii) x−1/2, −y+1/2, z−1/2; (iii) x−1/2, −y+1/2, z+1/2; (iv) x+1/2, −y+1/2, z+1/2; (v) x+1/2, −y+1/2, z−1/2; (vi) −x+1/2, y−1/2, −z+1/2. |
Crystal data top
C0.5O48.2Si24 | F(000) = 2984 |
Mr = 1451.8 | Dx = 1.853 Mg m−3 |
Monoclinic, P21/n | Mo Kα radiation, λ = 0.71073 Å |
a = 13.385 (2) Å | Cell parameters from 8115 reflections |
b = 20.110 (3) Å | θ = 2.3–27.4° |
c = 19.881 (3) Å | µ = 0.68 mm−1 |
β = 90.041 (2)° | T = 296 K |
V = 5351.4 (14) Å3 | Coffin shape, colorless |
Z = 4 | 0.25 × 0.09 × 0.09 mm |
Data collection top
CCD area detector diffractometer | 11904 independent reflections |
Radiation source: fine-focus sealed tube | 10178 reflections with I > 2σ(I) |
Graphite monochromator | Rint = 0.111 |
phi and ω scans | θmax = 27.6°, θmin = 1.0° |
Absorption correction: analytical ? | h = −17→17 |
Tmin = 0.849, Tmax = 0.941 | k = −26→26 |
58291 measured reflections | l = −25→25 |
Refinement top
Refinement on F2 | 2 restraints |
Least-squares matrix: full | Primary atom site location: structure-invariant direct methods |
R[F2 > 2σ(F2)] = 0.059 | Secondary atom site location: difference Fourier map |
wR(F2) = 0.192 | w = 1/[σ2(Fo2) + (0.1189P)2 + 2.6558P] where P = (Fo2 + 2Fc2)/3 |
S = 1.10 | (Δ/σ)max < 0.001 |
11904 reflections | Δρmax = 0.87 e Å−3 |
660 parameters | Δρmin = −0.98 e Å−3 |
Crystal data top
C0.5O48.2Si24 | V = 5351.4 (14) Å3 |
Mr = 1451.8 | Z = 4 |
Monoclinic, P21/n | Mo Kα radiation |
a = 13.385 (2) Å | µ = 0.68 mm−1 |
b = 20.110 (3) Å | T = 296 K |
c = 19.881 (3) Å | 0.25 × 0.09 × 0.09 mm |
β = 90.041 (2)° | |
Data collection top
CCD area detector diffractometer | 11904 independent reflections |
Absorption correction: analytical ? | 10178 reflections with I > 2σ(I) |
Tmin = 0.849, Tmax = 0.941 | Rint = 0.111 |
58291 measured reflections | |
Refinement top
R[F2 > 2σ(F2)] = 0.059 | 660 parameters |
wR(F2) = 0.192 | 2 restraints |
S = 1.10 | Δρmax = 0.87 e Å−3 |
11904 reflections | Δρmin = −0.98 e Å−3 |
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 | x | y | z | Uiso*/Ueq | Occ. (<1) |
C301 | 0.152 (9) | 0.262 (4) | 0.737 (7) | 0.35 (7)* | 0.24 (2) |
C302 | 0.142 (9) | 0.147 (3) | 0.734 (6) | 0.35 (7)* | 0.24 (2) |
O303 | 0.093 (6) | 0.206 (4) | 0.752 (4) | 0.34 (5)* | 0.24 (2) |
Si1 | 0.32257 (10) | 0.42081 (5) | −0.05596 (6) | 0.0191 (2) | |
Si2 | 0.16841 (11) | 0.31235 (5) | −0.03023 (6) | 0.0217 (3) | |
Si3 | −0.04936 (10) | 0.27961 (5) | −0.06222 (6) | 0.0206 (3) | |
Si4 | −0.03506 (9) | 0.12359 (5) | −0.06277 (6) | 0.0198 (3) | |
Si5 | 0.17766 (10) | 0.07579 (5) | −0.02828 (5) | 0.0189 (3) | |
Si6 | 0.31616 (10) | 0.19378 (5) | −0.05620 (7) | 0.0202 (3) | |
Si7 | 0.32033 (10) | 0.42491 (5) | 0.17155 (5) | 0.0197 (3) | |
Si8 | 0.17577 (11) | 0.31138 (5) | 0.12729 (6) | 0.0203 (3) | |
Si9 | −0.03502 (10) | 0.27355 (5) | 0.17564 (5) | 0.0195 (3) | |
Si10 | −0.03262 (10) | 0.11928 (5) | 0.17574 (5) | 0.0206 (3) | |
Si11 | 0.17715 (10) | 0.07142 (5) | 0.12939 (6) | 0.0193 (2) | |
Si12 | 0.31570 (11) | 0.19013 (5) | 0.16677 (6) | 0.0201 (3) | |
Si13 | 0.33546 (10) | 0.42737 (5) | 0.55739 (6) | 0.0189 (3) | |
Si14 | 0.18865 (11) | 0.31169 (5) | 0.52768 (6) | 0.0209 (3) | |
Si15 | −0.02929 (9) | 0.27759 (5) | 0.56149 (6) | 0.0193 (2) | |
Si16 | −0.03265 (9) | 0.12166 (5) | 0.56418 (6) | 0.0191 (2) | |
Si17 | 0.17982 (10) | 0.07082 (5) | 0.52762 (5) | 0.0177 (2) | |
Si18 | 0.31966 (11) | 0.18725 (5) | 0.56205 (6) | 0.0207 (3) | |
Si19 | 0.31598 (10) | 0.42398 (5) | 0.32791 (5) | 0.0200 (3) | |
Si20 | 0.17177 (11) | 0.31196 (5) | 0.36941 (6) | 0.0213 (3) | |
Si21 | −0.04283 (10) | 0.27328 (5) | 0.33072 (6) | 0.0203 (3) | |
Si22 | −0.03676 (10) | 0.11887 (5) | 0.32947 (6) | 0.0207 (3) | |
Si23 | 0.17825 (10) | 0.07196 (5) | 0.36967 (6) | 0.0201 (3) | |
Si24 | 0.30169 (11) | 0.19284 (5) | 0.32091 (6) | 0.0197 (3) | |
O1 | 0.2244 (3) | 0.37663 (16) | −0.0582 (2) | 0.0401 (9) | |
O2 | 0.0612 (3) | 0.30969 (15) | −0.06544 (18) | 0.0335 (8) | |
O3 | −0.0433 (4) | 0.20119 (15) | −0.0495 (2) | 0.0454 (10) | |
O4 | 0.0796 (2) | 0.10238 (17) | −0.06686 (16) | 0.0328 (7) | |
O5 | 0.2713 (3) | 0.12142 (15) | −0.04633 (18) | 0.0330 (8) | |
O6 | 0.2293 (3) | 0.24723 (17) | −0.0477 (2) | 0.0452 (10) | |
O7 | 0.2296 (3) | 0.37656 (18) | 0.1535 (2) | 0.0439 (10) | |
O8 | 0.0718 (3) | 0.30551 (17) | 0.1652 (2) | 0.0402 (9) | |
O9 | −0.0307 (4) | 0.19596 (14) | 0.15590 (18) | 0.0384 (10) | |
O10 | 0.0772 (3) | 0.08957 (19) | 0.16841 (19) | 0.0430 (9) | |
O11 | 0.2656 (3) | 0.12018 (17) | 0.15187 (19) | 0.0433 (10) | |
O12 | 0.2432 (3) | 0.24763 (18) | 0.1405 (2) | 0.0462 (10) | |
O13 | 0.1547 (4) | 0.3170 (2) | 0.04888 (19) | 0.0548 (12) | |
O14 | 0.1566 (3) | 0.07812 (17) | 0.05091 (16) | 0.0375 (8) | |
O15 | 0.3788 (3) | 0.41488 (18) | −0.12577 (16) | 0.0393 (9) | |
O16 | 0.3928 (3) | 0.3950 (2) | 0.00372 (17) | 0.0466 (10) | |
O17 | 0.4193 (3) | 0.40126 (17) | 0.13376 (16) | 0.0346 (8) | |
O18 | 0.3630 (3) | 0.19878 (17) | −0.12964 (17) | 0.0324 (8) | |
O19 | 0.4023 (3) | 0.2068 (2) | −0.00193 (18) | 0.0438 (10) | |
O20 | 0.4199 (3) | 0.19539 (17) | 0.12844 (18) | 0.0362 (9) | |
O21 | 0.2042 (3) | 0.00208 (14) | −0.05178 (16) | 0.0289 (7) | |
O22 | 0.2098 (3) | −0.00260 (15) | 0.14772 (17) | 0.0355 (8) | |
O23 | 0.3437 (3) | 0.42377 (17) | 0.25031 (17) | 0.0388 (8) | |
O24 | 0.3386 (3) | 0.19719 (15) | 0.24492 (17) | 0.0342 (8) | |
O25 | −0.0654 (3) | 0.28277 (16) | 0.25269 (16) | 0.0313 (7) | |
O26 | −0.0673 (2) | 0.11009 (15) | 0.25203 (15) | 0.0294 (7) | |
O27 | 0.2416 (3) | 0.37853 (16) | 0.5516 (2) | 0.0462 (10) | |
O28 | 0.0758 (3) | 0.31380 (15) | 0.5532 (2) | 0.0340 (8) | |
O29 | −0.0111 (3) | 0.19888 (15) | 0.5661 (2) | 0.0433 (10) | |
O30 | 0.0695 (3) | 0.08325 (18) | 0.5550 (2) | 0.0414 (9) | |
O31 | 0.2567 (3) | 0.11932 (15) | 0.56426 (16) | 0.0335 (8) | |
O32 | 0.2453 (3) | 0.24935 (16) | 0.55933 (19) | 0.0398 (9) | |
O33 | 0.2207 (3) | 0.37865 (16) | 0.34169 (18) | 0.0376 (9) | |
O34 | 0.0556 (3) | 0.31364 (15) | 0.35385 (19) | 0.0331 (8) | |
O35 | −0.0260 (4) | 0.19606 (14) | 0.34813 (18) | 0.0374 (10) | |
O36 | 0.0679 (3) | 0.0833 (2) | 0.3435 (2) | 0.0500 (11) | |
O37 | 0.2534 (3) | 0.12176 (17) | 0.33393 (18) | 0.0451 (10) | |
O38 | 0.2200 (3) | 0.24890 (17) | 0.3332 (2) | 0.0448 (10) | |
O39 | 0.1917 (4) | 0.3059 (2) | 0.4483 (2) | 0.0564 (13) | |
O40 | 0.1830 (3) | 0.08411 (17) | 0.44886 (16) | 0.0418 (9) | |
O41 | 0.3898 (3) | 0.41861 (18) | 0.62855 (17) | 0.0405 (9) | |
O42 | 0.4133 (3) | 0.41422 (18) | 0.49901 (17) | 0.0369 (8) | |
O43 | 0.4108 (3) | 0.39572 (19) | 0.36828 (16) | 0.0369 (8) | |
O44 | 0.3842 (3) | 0.18991 (15) | 0.62986 (18) | 0.0339 (9) | |
O45 | 0.3904 (3) | 0.18749 (16) | 0.49828 (18) | 0.0386 (9) | |
O46 | −0.1043 (3) | 0.2954 (2) | −0.13161 (18) | 0.0457 (10) | |
O47 | 0.2104 (3) | −0.00418 (14) | 0.54412 (18) | 0.0321 (8) | |
O48 | 0.2114 (3) | −0.00212 (15) | 0.35187 (17) | 0.0363 (9) | |
Atomic displacement parameters (Å2) top | U11 | U22 | U33 | U12 | U13 | U23 |
Si1 | 0.0330 (6) | 0.0115 (5) | 0.0128 (5) | 0.0003 (4) | −0.0014 (5) | −0.0014 (4) |
Si2 | 0.0358 (7) | 0.0140 (5) | 0.0152 (6) | −0.0020 (4) | −0.0019 (5) | −0.0006 (4) |
Si3 | 0.0340 (7) | 0.0151 (5) | 0.0127 (5) | −0.0003 (5) | −0.0048 (5) | −0.0007 (4) |
Si4 | 0.0321 (6) | 0.0133 (5) | 0.0140 (5) | −0.0003 (4) | −0.0051 (5) | 0.0000 (4) |
Si5 | 0.0328 (7) | 0.0119 (5) | 0.0119 (5) | −0.0023 (4) | −0.0019 (5) | 0.0010 (4) |
Si6 | 0.0310 (7) | 0.0144 (5) | 0.0152 (6) | −0.0044 (4) | 0.0003 (6) | 0.0004 (4) |
Si7 | 0.0361 (7) | 0.0121 (5) | 0.0110 (5) | −0.0018 (5) | −0.0014 (5) | −0.0008 (4) |
Si8 | 0.0319 (7) | 0.0154 (5) | 0.0135 (6) | −0.0021 (4) | −0.0029 (5) | 0.0001 (4) |
Si9 | 0.0324 (6) | 0.0158 (5) | 0.0104 (5) | 0.0007 (4) | −0.0018 (5) | 0.0017 (4) |
Si10 | 0.0361 (7) | 0.0152 (5) | 0.0107 (5) | 0.0002 (5) | −0.0019 (5) | −0.0018 (4) |
Si11 | 0.0336 (6) | 0.0120 (5) | 0.0122 (5) | 0.0001 (4) | −0.0024 (5) | −0.0004 (4) |
Si12 | 0.0345 (7) | 0.0142 (5) | 0.0115 (5) | −0.0020 (4) | −0.0023 (5) | −0.0001 (4) |
Si13 | 0.0330 (7) | 0.0105 (5) | 0.0131 (5) | 0.0006 (4) | −0.0035 (5) | 0.0005 (4) |
Si14 | 0.0322 (7) | 0.0157 (5) | 0.0148 (6) | −0.0018 (4) | −0.0007 (5) | 0.0010 (4) |
Si15 | 0.0297 (6) | 0.0144 (5) | 0.0138 (5) | 0.0009 (4) | −0.0007 (5) | 0.0007 (4) |
Si16 | 0.0303 (6) | 0.0134 (5) | 0.0137 (5) | −0.0009 (4) | −0.0013 (5) | 0.0004 (4) |
Si17 | 0.0303 (6) | 0.0098 (5) | 0.0130 (5) | −0.0003 (4) | −0.0013 (5) | 0.0004 (4) |
Si18 | 0.0357 (7) | 0.0133 (5) | 0.0131 (5) | −0.0029 (4) | −0.0054 (5) | 0.0012 (4) |
Si19 | 0.0363 (7) | 0.0134 (5) | 0.0103 (5) | −0.0016 (4) | −0.0030 (5) | 0.0010 (4) |
Si20 | 0.0338 (7) | 0.0156 (5) | 0.0144 (6) | −0.0020 (5) | −0.0014 (5) | −0.0004 (4) |
Si21 | 0.0326 (7) | 0.0160 (5) | 0.0123 (5) | −0.0011 (5) | −0.0016 (5) | −0.0017 (4) |
Si22 | 0.0356 (7) | 0.0149 (5) | 0.0116 (5) | 0.0004 (5) | −0.0028 (5) | 0.0022 (4) |
Si23 | 0.0371 (7) | 0.0107 (5) | 0.0125 (5) | −0.0003 (4) | −0.0032 (5) | 0.0003 (4) |
Si24 | 0.0338 (7) | 0.0154 (5) | 0.0099 (5) | −0.0020 (4) | −0.0009 (5) | −0.0013 (4) |
O1 | 0.048 (2) | 0.0213 (16) | 0.051 (2) | −0.0134 (15) | −0.0085 (19) | 0.0064 (16) |
O2 | 0.033 (2) | 0.0372 (19) | 0.0305 (19) | −0.0070 (14) | −0.0055 (16) | 0.0055 (14) |
O3 | 0.067 (3) | 0.0141 (15) | 0.055 (3) | −0.0028 (16) | 0.002 (2) | −0.0044 (15) |
O4 | 0.0333 (17) | 0.0442 (19) | 0.0208 (16) | 0.0083 (16) | −0.0016 (14) | 0.0040 (14) |
O5 | 0.0395 (19) | 0.0168 (15) | 0.043 (2) | −0.0076 (14) | 0.0028 (16) | 0.0035 (14) |
O6 | 0.051 (2) | 0.0211 (17) | 0.063 (3) | 0.0080 (15) | 0.008 (2) | −0.0047 (17) |
O7 | 0.050 (2) | 0.0263 (18) | 0.056 (2) | −0.0149 (17) | −0.0035 (19) | −0.0087 (16) |
O8 | 0.030 (2) | 0.046 (2) | 0.044 (2) | −0.0103 (15) | 0.0117 (18) | −0.0056 (16) |
O9 | 0.072 (3) | 0.0167 (16) | 0.0269 (18) | 0.0014 (15) | 0.0054 (19) | 0.0006 (12) |
O10 | 0.046 (2) | 0.050 (2) | 0.0333 (19) | 0.0190 (19) | 0.0142 (17) | 0.0067 (16) |
O11 | 0.060 (3) | 0.0224 (17) | 0.048 (2) | −0.0122 (17) | −0.0134 (19) | −0.0075 (15) |
O12 | 0.054 (2) | 0.0309 (19) | 0.054 (2) | 0.0156 (18) | −0.006 (2) | 0.0065 (17) |
O13 | 0.084 (3) | 0.068 (3) | 0.0121 (17) | 0.009 (2) | −0.005 (2) | −0.0017 (16) |
O14 | 0.060 (2) | 0.0409 (19) | 0.0121 (14) | 0.0011 (17) | −0.0023 (16) | −0.0012 (13) |
O15 | 0.058 (2) | 0.041 (2) | 0.0186 (16) | 0.0196 (18) | 0.0112 (17) | 0.0010 (14) |
O16 | 0.056 (2) | 0.060 (2) | 0.0234 (17) | 0.010 (2) | −0.0151 (17) | 0.0053 (17) |
O17 | 0.043 (2) | 0.0392 (19) | 0.0213 (16) | 0.0059 (16) | 0.0064 (15) | −0.0084 (14) |
O18 | 0.036 (2) | 0.045 (2) | 0.0153 (16) | −0.0074 (15) | 0.0047 (15) | 0.0040 (13) |
O19 | 0.051 (2) | 0.056 (2) | 0.0235 (19) | −0.0148 (19) | −0.0138 (17) | −0.0032 (16) |
O20 | 0.041 (2) | 0.046 (2) | 0.0218 (18) | 0.0022 (15) | 0.0085 (17) | 0.0097 (14) |
O21 | 0.0412 (19) | 0.0145 (14) | 0.0310 (16) | −0.0023 (13) | −0.0004 (15) | −0.0040 (12) |
O22 | 0.045 (2) | 0.0189 (16) | 0.042 (2) | 0.0004 (15) | 0.0007 (17) | 0.0085 (14) |
O23 | 0.053 (2) | 0.052 (2) | 0.0117 (13) | 0.0066 (17) | −0.0002 (17) | 0.0021 (15) |
O24 | 0.050 (2) | 0.0399 (19) | 0.0129 (15) | −0.0131 (14) | 0.0042 (17) | −0.0017 (12) |
O25 | 0.0477 (19) | 0.0337 (16) | 0.0124 (13) | 0.0041 (15) | 0.0015 (16) | 0.0018 (13) |
O26 | 0.0428 (18) | 0.0347 (16) | 0.0107 (13) | −0.0013 (14) | 0.0015 (15) | −0.0009 (13) |
O27 | 0.039 (2) | 0.0234 (17) | 0.076 (3) | −0.0103 (15) | 0.004 (2) | −0.0116 (18) |
O28 | 0.036 (2) | 0.0266 (17) | 0.040 (2) | −0.0051 (13) | 0.0099 (17) | −0.0060 (14) |
O29 | 0.058 (3) | 0.0154 (16) | 0.057 (3) | −0.0031 (14) | −0.003 (2) | 0.0031 (15) |
O30 | 0.034 (2) | 0.0375 (19) | 0.053 (2) | 0.0102 (15) | 0.0122 (18) | 0.0030 (17) |
O31 | 0.058 (2) | 0.0214 (15) | 0.0211 (16) | −0.0155 (15) | −0.0101 (16) | 0.0028 (13) |
O32 | 0.050 (2) | 0.0254 (17) | 0.044 (2) | 0.0106 (15) | −0.0013 (19) | 0.0099 (16) |
O33 | 0.045 (2) | 0.0233 (16) | 0.044 (2) | −0.0116 (16) | 0.0003 (17) | 0.0074 (15) |
O34 | 0.037 (2) | 0.0221 (16) | 0.040 (2) | −0.0049 (14) | −0.0073 (17) | −0.0028 (13) |
O35 | 0.069 (3) | 0.0159 (16) | 0.0269 (19) | −0.0023 (15) | −0.0088 (18) | −0.0005 (12) |
O36 | 0.050 (2) | 0.047 (2) | 0.053 (3) | 0.0195 (19) | −0.023 (2) | −0.0102 (18) |
O37 | 0.076 (3) | 0.0201 (16) | 0.040 (2) | −0.0133 (18) | 0.022 (2) | 0.0016 (15) |
O38 | 0.055 (2) | 0.0262 (18) | 0.054 (2) | 0.0124 (17) | 0.004 (2) | −0.0128 (16) |
O39 | 0.069 (3) | 0.087 (3) | 0.0131 (18) | −0.001 (2) | −0.005 (2) | 0.0024 (17) |
O40 | 0.080 (3) | 0.0334 (17) | 0.0117 (14) | −0.0030 (18) | −0.0054 (18) | −0.0001 (13) |
O41 | 0.065 (3) | 0.0407 (19) | 0.0160 (16) | 0.0180 (18) | −0.0125 (17) | 0.0017 (14) |
O42 | 0.048 (2) | 0.0380 (19) | 0.0245 (17) | 0.0028 (16) | 0.0084 (16) | −0.0063 (14) |
O43 | 0.042 (2) | 0.046 (2) | 0.0230 (17) | 0.0084 (17) | −0.0105 (16) | 0.0035 (15) |
O44 | 0.051 (2) | 0.0302 (18) | 0.0200 (17) | −0.0111 (15) | −0.0158 (17) | 0.0008 (12) |
O45 | 0.058 (3) | 0.0322 (19) | 0.0262 (19) | −0.0044 (16) | 0.0118 (18) | 0.0057 (13) |
O46 | 0.044 (2) | 0.076 (3) | 0.0170 (17) | 0.0023 (19) | −0.0102 (17) | 0.0083 (17) |
O47 | 0.041 (2) | 0.0127 (14) | 0.0424 (19) | 0.0011 (13) | 0.0062 (16) | 0.0072 (13) |
O48 | 0.054 (2) | 0.0137 (14) | 0.042 (2) | 0.0024 (15) | −0.0027 (17) | −0.0064 (13) |
Geometric parameters (Å, º) top
C301—O303 | 1.4048 | Si14—O28 | 1.594 (4) |
C302—O303 | 1.4055 | Si15—O19iii | 1.589 (4) |
Si1—O15 | 1.584 (4) | Si15—O20iii | 1.591 (4) |
Si1—O1 | 1.585 (4) | Si15—O28 | 1.592 (4) |
Si1—O47i | 1.588 (3) | Si15—O29 | 1.603 (3) |
Si1—O16 | 1.596 (4) | Si16—O29 | 1.579 (3) |
Si2—O6 | 1.580 (4) | Si16—O30 | 1.580 (4) |
Si2—O13 | 1.585 (4) | Si16—O16iii | 1.597 (4) |
Si2—O2 | 1.593 (4) | Si16—O17iii | 1.594 (3) |
Si2—O1 | 1.594 (3) | Si17—O40 | 1.587 (3) |
Si3—O46 | 1.591 (4) | Si17—O31 | 1.591 (3) |
Si3—O45ii | 1.593 (4) | Si17—O30 | 1.595 (4) |
Si3—O3 | 1.598 (3) | Si17—O47 | 1.595 (3) |
Si3—O2 | 1.599 (4) | Si18—O45 | 1.584 (4) |
Si4—O3 | 1.585 (3) | Si18—O32 | 1.596 (3) |
Si4—O43ii | 1.594 (3) | Si18—O44 | 1.602 (4) |
Si4—O4 | 1.594 (3) | Si18—O31 | 1.604 (3) |
Si4—O42ii | 1.602 (3) | Si19—O23 | 1.586 (3) |
Si5—O21 | 1.593 (3) | Si19—O33 | 1.590 (4) |
Si5—O5 | 1.594 (3) | Si19—O22i | 1.591 (3) |
Si5—O14 | 1.599 (3) | Si19—O43 | 1.601 (3) |
Si5—O4 | 1.611 (3) | Si20—O34 | 1.583 (4) |
Si6—O5 | 1.585 (3) | Si20—O33 | 1.591 (3) |
Si6—O6 | 1.592 (4) | Si20—O39 | 1.593 (4) |
Si6—O18 | 1.593 (4) | Si20—O38 | 1.594 (4) |
Si6—O19 | 1.596 (4) | Si21—O25 | 1.592 (3) |
Si7—O23 | 1.593 (3) | Si21—O18iii | 1.590 (4) |
Si7—O7 | 1.594 (4) | Si21—O35 | 1.605 (3) |
Si7—O48i | 1.595 (3) | Si21—O34 | 1.611 (4) |
Si7—O17 | 1.596 (4) | Si22—O15iii | 1.592 (4) |
Si8—O7 | 1.581 (4) | Si22—O36 | 1.595 (4) |
Si8—O13 | 1.585 (4) | Si22—O26 | 1.599 (3) |
Si8—O12 | 1.588 (4) | Si22—O35 | 1.601 (3) |
Si8—O8 | 1.588 (4) | Si23—O36 | 1.579 (4) |
Si9—O8 | 1.580 (4) | Si23—O37 | 1.588 (4) |
Si9—O44ii | 1.593 (4) | Si23—O40 | 1.592 (3) |
Si9—O25 | 1.595 (3) | Si23—O48 | 1.593 (3) |
Si9—O9 | 1.608 (3) | Si24—O46iv | 1.590 (4) |
Si10—O41ii | 1.589 (4) | Si24—O38 | 1.589 (4) |
Si10—O9 | 1.590 (3) | Si24—O37 | 1.589 (3) |
Si10—O10 | 1.593 (4) | Si24—O24 | 1.592 (4) |
Si10—O26 | 1.597 (3) | O15—Si22v | 1.592 (4) |
Si11—O14 | 1.587 (3) | O16—Si16v | 1.597 (4) |
Si11—O10 | 1.590 (4) | O17—Si16v | 1.594 (3) |
Si11—O22 | 1.592 (3) | O18—Si21v | 1.590 (4) |
Si11—O11 | 1.598 (4) | O19—Si15v | 1.589 (4) |
Si12—O11 | 1.584 (3) | O20—Si15v | 1.591 (4) |
Si12—O24 | 1.586 (3) | O21—Si13vi | 1.596 (3) |
Si12—O12 | 1.594 (4) | O22—Si19vi | 1.591 (3) |
Si12—O20 | 1.594 (4) | O41—Si10iv | 1.589 (4) |
Si13—O42 | 1.584 (4) | O42—Si4iv | 1.602 (3) |
Si13—O41 | 1.600 (4) | O43—Si4iv | 1.594 (3) |
Si13—O21i | 1.596 (3) | O44—Si9iv | 1.593 (4) |
Si13—O27 | 1.597 (4) | O45—Si3iv | 1.593 (4) |
Si14—O39 | 1.580 (4) | O46—Si24ii | 1.590 (4) |
Si14—O27 | 1.590 (3) | O47—Si1vi | 1.588 (3) |
Si14—O32 | 1.591 (3) | O48—Si7vi | 1.595 (3) |
| | | |
C301—O303—C302 | 111.7 | O40—Si17—O31 | 109.12 (19) |
O15—Si1—O1 | 109.2 (2) | O40—Si17—O30 | 109.8 (2) |
O15—Si1—O47i | 109.51 (19) | O31—Si17—O30 | 110.2 (2) |
O1—Si1—O47i | 107.78 (19) | O40—Si17—O47 | 110.70 (19) |
O15—Si1—O16 | 110.2 (2) | O31—Si17—O47 | 108.68 (19) |
O1—Si1—O16 | 108.9 (2) | O30—Si17—O47 | 108.33 (19) |
O47i—Si1—O16 | 111.2 (2) | O45—Si18—O32 | 110.2 (2) |
O6—Si2—O13 | 109.2 (2) | O45—Si18—O44 | 110.6 (3) |
O6—Si2—O2 | 109.8 (2) | O32—Si18—O44 | 109.7 (2) |
O13—Si2—O2 | 109.2 (3) | O45—Si18—O31 | 109.86 (19) |
O6—Si2—O1 | 110.6 (2) | O32—Si18—O31 | 109.8 (2) |
O13—Si2—O1 | 110.8 (2) | O44—Si18—O31 | 106.70 (17) |
O2—Si2—O1 | 107.32 (19) | O23—Si19—O33 | 110.9 (2) |
O46—Si3—O45ii | 109.7 (2) | O23—Si19—O22i | 110.48 (19) |
O46—Si3—O3 | 110.9 (2) | O33—Si19—O22i | 107.7 (2) |
O45ii—Si3—O3 | 108.4 (2) | O23—Si19—O43 | 107.3 (2) |
O46—Si3—O2 | 108.3 (2) | O33—Si19—O43 | 110.1 (2) |
O45ii—Si3—O2 | 110.1 (2) | O22i—Si19—O43 | 110.4 (2) |
O3—Si3—O2 | 109.4 (2) | O34—Si20—O33 | 108.6 (2) |
O3—Si4—O43ii | 110.6 (2) | O34—Si20—O39 | 110.7 (2) |
O3—Si4—O4 | 109.8 (2) | O33—Si20—O39 | 109.7 (2) |
O43ii—Si4—O4 | 108.94 (19) | O34—Si20—O38 | 109.1 (2) |
O3—Si4—O42ii | 108.0 (2) | O33—Si20—O38 | 110.2 (2) |
O43ii—Si4—O42ii | 110.3 (2) | O39—Si20—O38 | 108.5 (2) |
O4—Si4—O42ii | 109.27 (19) | O25—Si21—O18iii | 107.02 (19) |
O21—Si5—O5 | 107.00 (18) | O25—Si21—O35 | 110.60 (18) |
O21—Si5—O14 | 110.83 (18) | O18iii—Si21—O35 | 110.2 (2) |
O5—Si5—O14 | 110.3 (2) | O25—Si21—O34 | 111.7 (2) |
O21—Si5—O4 | 110.61 (18) | O18iii—Si21—O34 | 109.18 (19) |
O5—Si5—O4 | 109.98 (18) | O35—Si21—O34 | 108.2 (2) |
O14—Si5—O4 | 108.2 (2) | O15iii—Si22—O36 | 109.6 (2) |
O5—Si6—O6 | 109.2 (2) | O15iii—Si22—O26 | 108.12 (18) |
O5—Si6—O18 | 108.76 (19) | O36—Si22—O26 | 109.8 (2) |
O6—Si6—O18 | 110.2 (2) | O15iii—Si22—O35 | 110.3 (2) |
O5—Si6—O19 | 109.8 (2) | O36—Si22—O35 | 108.4 (2) |
O6—Si6—O19 | 110.1 (2) | O26—Si22—O35 | 110.59 (18) |
O18—Si6—O19 | 108.8 (2) | O36—Si23—O37 | 110.8 (2) |
O23—Si7—O7 | 110.9 (2) | O36—Si23—O40 | 109.6 (2) |
O23—Si7—O48i | 110.48 (19) | O37—Si23—O40 | 108.8 (2) |
O7—Si7—O48i | 107.1 (2) | O36—Si23—O48 | 108.8 (2) |
O23—Si7—O17 | 107.33 (19) | O37—Si23—O48 | 108.2 (2) |
O7—Si7—O17 | 110.2 (2) | O40—Si23—O48 | 110.65 (19) |
O48i—Si7—O17 | 110.9 (2) | O46iv—Si24—O38 | 110.3 (2) |
O7—Si8—O13 | 110.1 (2) | O46iv—Si24—O37 | 111.0 (2) |
O7—Si8—O12 | 110.9 (3) | O38—Si24—O37 | 109.4 (2) |
O13—Si8—O12 | 108.6 (2) | O46iv—Si24—O24 | 107.9 (2) |
O7—Si8—O8 | 107.7 (2) | O38—Si24—O24 | 108.8 (2) |
O13—Si8—O8 | 108.5 (3) | O37—Si24—O24 | 109.35 (18) |
O12—Si8—O8 | 111.1 (2) | Si1—O1—Si2 | 146.6 (3) |
O8—Si9—O44ii | 110.4 (2) | Si2—O2—Si3 | 145.7 (2) |
O8—Si9—O25 | 108.0 (2) | Si4—O3—Si3 | 161.3 (3) |
O44ii—Si9—O25 | 108.6 (2) | Si4—O4—Si5 | 148.0 (2) |
O8—Si9—O9 | 109.2 (2) | Si6—O5—Si5 | 148.6 (2) |
O44ii—Si9—O9 | 109.5 (2) | Si2—O6—Si6 | 163.5 (3) |
O25—Si9—O9 | 110.83 (18) | Si8—O7—Si7 | 157.4 (3) |
O41ii—Si10—O9 | 109.2 (2) | Si9—O8—Si8 | 152.4 (3) |
O41ii—Si10—O10 | 111.5 (2) | Si10—O9—Si9 | 151.4 (3) |
O9—Si10—O10 | 108.9 (2) | Si11—O10—Si10 | 155.2 (3) |
O41ii—Si10—O26 | 108.19 (19) | Si12—O11—Si11 | 155.2 (3) |
O9—Si10—O26 | 110.61 (18) | Si8—O12—Si12 | 169.4 (3) |
O10—Si10—O26 | 108.36 (19) | Si8—O13—Si2 | 161.5 (4) |
O14—Si11—O10 | 108.4 (2) | Si11—O14—Si5 | 158.8 (3) |
O14—Si11—O22 | 110.48 (19) | Si1—O15—Si22v | 149.4 (2) |
O10—Si11—O22 | 109.5 (2) | Si16v—O16—Si1 | 173.0 (3) |
O14—Si11—O11 | 110.3 (2) | Si16v—O17—Si7 | 146.3 (2) |
O10—Si11—O11 | 110.2 (2) | Si21v—O18—Si6 | 142.3 (3) |
O22—Si11—O11 | 107.9 (2) | Si15v—O19—Si6 | 169.0 (3) |
O11—Si12—O24 | 109.96 (19) | Si15v—O20—Si12 | 143.0 (3) |
O11—Si12—O12 | 109.0 (2) | Si5—O21—Si13vi | 145.1 (2) |
O24—Si12—O12 | 111.7 (2) | Si19vi—O22—Si11 | 151.2 (3) |
O11—Si12—O20 | 109.8 (2) | Si19—O23—Si7 | 155.2 (3) |
O24—Si12—O20 | 107.2 (2) | Si12—O24—Si24 | 149.6 (3) |
O12—Si12—O20 | 109.1 (2) | Si21—O25—Si9 | 150.8 (2) |
O42—Si13—O41 | 109.4 (2) | Si10—O26—Si22 | 145.7 (2) |
O42—Si13—O21i | 108.99 (18) | Si14—O27—Si13 | 152.8 (3) |
O41—Si13—O21i | 108.39 (18) | Si15—O28—Si14 | 149.1 (2) |
O42—Si13—O27 | 111.3 (2) | Si16—O29—Si15 | 160.2 (3) |
O41—Si13—O27 | 110.5 (2) | Si16—O30—Si17 | 156.5 (3) |
O21i—Si13—O27 | 108.17 (19) | Si17—O31—Si18 | 147.9 (2) |
O39—Si14—O27 | 110.2 (2) | Si14—O32—Si18 | 157.5 (3) |
O39—Si14—O32 | 108.7 (2) | Si19—O33—Si20 | 150.8 (3) |
O27—Si14—O32 | 109.7 (2) | Si20—O34—Si21 | 147.6 (2) |
O39—Si14—O28 | 110.4 (2) | Si22—O35—Si21 | 151.0 (3) |
O27—Si14—O28 | 107.7 (2) | Si23—O36—Si22 | 160.1 (3) |
O32—Si14—O28 | 110.2 (2) | Si23—O37—Si24 | 153.8 (3) |
O19iii—Si15—O20iii | 110.4 (2) | Si24—O38—Si20 | 155.8 (3) |
O19iii—Si15—O28 | 109.5 (2) | Si14—O39—Si20 | 165.9 (4) |
O20iii—Si15—O28 | 108.1 (2) | Si17—O40—Si23 | 161.1 (2) |
O19iii—Si15—O29 | 109.2 (2) | Si10iv—O41—Si13 | 150.3 (3) |
O20iii—Si15—O29 | 110.7 (2) | Si13—O42—Si4iv | 157.9 (3) |
O28—Si15—O29 | 108.8 (2) | Si4iv—O43—Si19 | 150.7 (3) |
O29—Si16—O30 | 109.0 (2) | Si9iv—O44—Si18 | 149.5 (2) |
O29—Si16—O16iii | 109.8 (2) | Si18—O45—Si3iv | 155.5 (2) |
O30—Si16—O16iii | 110.4 (2) | Si24ii—O46—Si3 | 155.1 (3) |
O29—Si16—O17iii | 109.7 (2) | Si1vi—O47—Si17 | 148.9 (3) |
O30—Si16—O17iii | 108.1 (2) | Si23—O48—Si7vi | 148.2 (3) |
O16iii—Si16—O17iii | 109.8 (2) | | |
Symmetry codes: (i) −x+1/2, y+1/2, −z+1/2; (ii) x−1/2, −y+1/2, z−1/2; (iii) x−1/2, −y+1/2, z+1/2; (iv) x+1/2, −y+1/2, z+1/2; (v) x+1/2, −y+1/2, z−1/2; (vi) −x+1/2, y−1/2, −z+1/2. |
Experimental details
| (str05h_twin_f_co2) | (sin05h_twin_f_co2) | (sin3h4_twin_f_co2) | (str3h6_2_twin_f_co2) |
Crystal data |
Chemical formula | C0.6O49.2Si24 | C0.14O48.27Si24 | C0.6O49.2Si24 | C1.1O50.2Si24 |
Mr | 1467.7 | 1448.2 | 1468.2 | 1491.1 |
Crystal system, space group | Monoclinic, P21/n | Monoclinic, P21/n | Monoclinic, P21/n | Monoclinic, P21/n |
Temperature (K) | 296 | 296 | 296 | 296 |
a, b, c (Å) | 13.376 (2), 20.111 (3), 19.878 (3) | 13.383 (3), 20.118 (4), 19.887 (4) | 13.388 (2), 20.132 (3), 19.902 (3) | 13.383 (3), 20.121 (4), 19.881 (4) |
β (°) | 90.003 (2) | 90.049 (3) | 90.040 (2) | 90.057 (3) |
V (Å3) | 5347.3 (14) | 5354.4 (19) | 5364.1 (14) | 5353.5 (19) |
Z | 4 | 4 | 4 | 4 |
Radiation type | Mo Kα | Mo Kα | Mo Kα | Mo Kα |
µ (mm−1) | 0.68 | 0.69 | 0.69 | 0.68 |
Crystal size (mm) | 0.15 × 0.10 × 0.08 | 0.17 × 0.09 × 0.07 | 0.14 × 0.08 × 0.07 | 0.13 × 0.09 × 0.08 |
|
Data collection |
Diffractometer | CCD area detector diffractometer | CCD area detector diffractometer | CCD area detector diffractometer | CCD area detector diffractometer |
Absorption correction | Analytical | Analytical | Analytical | Analytical |
Tmin, Tmax | 0.904, 0.950 | 0.893, 0.954 | 0.908, 0.955 | 0.914, 0.950 |
No. of measured, independent and observed [I > 2σ(I)] reflections | 61406, 12765, 6435 | 61320, 12808, 6047 | 62011, 12862, 5397 | 61855, 12802, 6968 |
Rint | 0.175 | 0.123 | 0.143 | 0.130 |
(sin θ/λ)max (Å−1) | 0.674 | 0.675 | 0.675 | 0.675 |
|
Refinement |
R[F2 > 2σ(F2)], wR(F2), S | 0.092, 0.186, 1.01 | 0.058, 0.159, 0.92 | 0.053, 0.122, 0.83 | 0.074, 0.172, 0.99 |
No. of reflections | 12765 | 12808 | 12862 | 12802 |
No. of parameters | 664 | 660 | 664 | 672 |
No. of restraints | 4 | 2 | 4 | 9 |
| w = 1/[σ2(Fo2) + (0.0366P)2 + 44.8067P] where P = (Fo2 + 2Fc2)/3 | w = 1/[σ2(Fo2) + (0.0652P)2] where P = (Fo2 + 2Fc2)/3 | w = 1/[σ2(Fo2) + (0.0374P)2] where P = (Fo2 + 2Fc2)/3 | w = 1/[σ2(Fo2) + (0.0712P)2] where P = (Fo2 + 2Fc2)/3 |
Δρmax, Δρmin (e Å−3) | 0.89, −1.10 | 0.89, −0.84 | 0.56, −0.62 | 0.88, −0.96 |
| (sin12h3_twin_f_dme) | (sin24h3_twin_f_dme) | (str12h_twin_f_dme) | (str24h_twin_f_dme) |
Crystal data |
Chemical formula | C1.1O48.5Si24 | C2O49Si24 | C0.4O48.2Si24 | C0.5O48.2Si24 |
Mr | 1463.65 | 1481.3 | 1449.1 | 1451.8 |
Crystal system, space group | Monoclinic, P21/n | Monoclinic, P21/n | Monoclinic, P21/n | Monoclinic, P21/n |
Temperature (K) | 296 | 296 | 296 | 296 |
a, b, c (Å) | 13.386 (2), 20.106 (3), 19.881 (3) | 13.381 (2), 20.107 (4), 19.875 (4) | 13.383 (2), 20.108 (3), 19.877 (3) | 13.385 (2), 20.110 (3), 19.881 (3) |
β (°) | 90.020 (2) | 90.023 (3) | 90.003 (2) | 90.041 (2) |
V (Å3) | 5350.8 (14) | 5347.4 (17) | 5349.0 (14) | 5351.4 (14) |
Z | 4 | 4 | 4 | 4 |
Radiation type | Mo Kα | Mo Kα | Mo Kα | Mo Kα |
µ (mm−1) | 0.68 | 0.69 | 0.68 | 0.68 |
Crystal size (mm) | 0.23 × 0.08 × 0.06 | 0.18 × 0.08 × 0.05 | 0.23 × 0.13 × 0.08 | 0.25 × 0.09 × 0.09 |
|
Data collection |
Diffractometer | Bruker P4 diffractometer | Bruker P4 diffractometer | CCD area detector diffractometer | CCD area detector diffractometer |
Absorption correction | Analytical | Analytical | Analytical | Analytical |
Tmin, Tmax | 0.861, 0.962 | 0.885, 0.969 | 0.860, 0.948 | 0.849, 0.941 |
No. of measured, independent and observed [I > 2σ(I)] reflections | 61647, 12821, 5131 | 61933, 12898, 5103 | 58608, 12004, 9577 | 58291, 11904, 10178 |
Rint | 0.113 | 0.144 | 0.115 | 0.111 |
(sin θ/λ)max (Å−1) | 0.675 | 0.681 | 0.657 | 0.651 |
|
Refinement |
R[F2 > 2σ(F2)], wR(F2), S | 0.055, 0.148, 0.82 | 0.059, 0.139, 0.84 | 0.060, 0.198, 1.11 | 0.059, 0.192, 1.10 |
No. of reflections | 12821 | 12898 | 12004 | 11904 |
No. of parameters | 660 | 668 | 660 | 660 |
No. of restraints | 2 | 6 | 2 | 2 |
| w = 1/[σ2(Fo2) + (0.051P)2] where P = (Fo2 + 2Fc2)/3 | w = 1/[σ2(Fo2) + (0.0415P)2] where P = (Fo2 + 2Fc2)/3 | w = 1/[σ2(Fo2) + (0.1204P)2] where P = (Fo2 + 2Fc2)/3 | w = 1/[σ2(Fo2) + (0.1189P)2 + 2.6558P] where P = (Fo2 + 2Fc2)/3 |
Δρmax, Δρmin (e Å−3) | 0.90, −0.69 | 0.77, −0.73 | 0.94, −1.00 | 0.87, −0.98 |