Entrance and diffusion pathway of CO₂ and dimethyl ether in silicalite-1 zeolite channels as determined by single-crystal XRD structural analysis

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.

Computing details

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.

Figures

(str05h_twin_f_co2)

Crystal data

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) Å^3	Coffin shape, colorless
Z = 4	0.15 × 0.10 × 0.08 mm

Data collection

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

Refinement on F^2	4 restraints
Least-squares matrix: full	Primary atom site location: structure-invariant direct methods
R[F^2 > 2σ(F^2)] = 0.092	Secondary atom site location: difference Fourier map
wR(F^2) = 0.186	w = 1/[σ^2(Fo^2) + (0.0366P)^2 + 44.8067P] where P = (Fo^2 + 2Fc^2)/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

Special details

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 (Ų)

	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 (Ų)

	U^11	U^22	U^33	U^12	U^13	U^23
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)

C200—O202	1.1601	Si14—O28	1.599 (8)
C200—O201	1.1601	Si14—O32	1.607 (9)
O202—O202^i	1.00 (11)	Si15—O19^iv	1.577 (9)
C500—O502	1.1604	Si15—O28	1.580 (8)
C500—O501	1.1604	Si15—O20^iv	1.585 (9)
Si1—O15	1.567 (9)	Si15—O29	1.601 (9)
Si1—O47^ii	1.569 (8)	Si16—O16^iv	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—O17^iv	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—O45^iii	1.601 (8)	Si18—O44	1.601 (9)
Si4—O4	1.576 (9)	Si18—O32	1.601 (9)
Si4—O43^iii	1.589 (9)	Si19—O23	1.579 (10)
Si4—O42^iii	1.594 (9)	Si19—O33	1.580 (9)
Si4—O3	1.605 (8)	Si19—O22^ii	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—O18^iv	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—O48^ii	1.602 (9)	Si22—O26	1.600 (10)
Si8—O12	1.578 (9)	Si22—O15^iv	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—O44^iii	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—O46^v	1.600 (9)
Si10—O10	1.591 (9)	O15—Si22^vi	1.601 (9)
Si10—O9	1.591 (9)	O16—Si16^vi	1.572 (9)
Si10—O41^iii	1.593 (9)	O17—Si16^vi	1.585 (9)
Si11—O10	1.581 (9)	O18—Si21^vi	1.580 (8)
Si11—O14	1.587 (10)	O19—Si15^vi	1.577 (9)
Si11—O11	1.594 (9)	O20—Si15^vi	1.585 (9)
Si11—O22	1.596 (9)	O21—Si13^vii	1.599 (8)
Si12—O11	1.576 (9)	O22—Si19^vii	1.585 (9)
Si12—O24	1.585 (9)	O41—Si10^v	1.593 (9)
Si12—O20	1.601 (8)	O42—Si4^v	1.594 (9)
Si12—O12	1.602 (9)	O43—Si4^v	1.590 (9)
Si13—O41	1.590 (10)	O44—Si9^v	1.583 (8)
Si13—O42	1.592 (9)	O45—Si3^v	1.601 (8)
Si13—O27	1.596 (8)	O46—Si24^iii	1.600 (9)
Si13—O21^ii	1.599 (8)	O47—Si1^vii	1.570 (8)
Si14—O27	1.590 (9)	O48—Si7^vii	1.602 (9)
Si14—O39	1.590 (10)
O202—C200—O201	180.00 (9)	O30—Si16—O17^iv	107.7 (5)
O202^i—O202—C200	128 (10)	O40—Si17—O30	109.4 (5)
O502—C500—O501	180 (10)	O40—Si17—O31	109.3 (5)
O15—Si1—O47^ii	109.2 (5)	O30—Si17—O31	109.6 (5)
O15—Si1—O1	108.2 (6)	O40—Si17—O47	111.3 (5)
O47^ii—Si1—O1	108.0 (4)	O30—Si17—O47	107.1 (4)
O15—Si1—O16	111.3 (5)	O31—Si17—O47	110.1 (5)
O47^ii—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—O22^ii	110.4 (4)
O46—Si3—O3	111.1 (5)	O33—Si19—O22^ii	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—O45^iii	109.2 (5)	O22^ii—Si19—O43	110.5 (5)
O3—Si3—O45^iii	108.3 (5)	O39—Si20—O33	110.2 (5)
O2—Si3—O45^iii	109.4 (5)	O39—Si20—O34	110.9 (5)
O4—Si4—O43^iii	109.2 (5)	O33—Si20—O34	108.7 (5)
O4—Si4—O42^iii	109.4 (5)	O39—Si20—O38	107.9 (5)
O43^iii—Si4—O42^iii	109.9 (5)	O33—Si20—O38	110.4 (5)
O4—Si4—O3	109.6 (5)	O34—Si20—O38	108.6 (4)
O43^iii—Si4—O3	110.6 (5)	O18^iv—Si21—O25	107.2 (4)
O42^iii—Si4—O3	108.1 (5)	O18^iv—Si21—O35	109.6 (5)
O21—Si5—O5	106.9 (4)	O25—Si21—O35	110.0 (4)
O21—Si5—O14	110.5 (5)	O18^iv—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—O15^iv	110.2 (5)
O18—Si6—O19	108.1 (5)	O35—Si22—O15^iv	110.3 (5)
O6—Si6—O5	109.2 (5)	O26—Si22—O15^iv	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—O48^ii	110.1 (5)	O40—Si23—O37	108.4 (5)
O23—Si7—O48^ii	110.7 (5)	O24—Si24—O38	108.9 (5)
O7—Si7—O48^ii	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—O46^v	108.5 (5)
O7—Si8—O13	109.8 (5)	O38—Si24—O46^v	110.2 (5)
O12—Si8—O8	110.7 (5)	O37—Si24—O46^v	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—O44^iii	110.6 (5)	Si3—O3—Si4	158.6 (7)
O8—Si9—O25	107.4 (4)	Si4—O4—Si5	147.2 (5)
O44^iii—Si9—O25	109.3 (4)	Si5—O5—Si6	147.6 (6)
O8—Si9—O9	108.5 (5)	Si2—O6—Si6	163.2 (6)
O44^iii—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—O41^iii	108.9 (5)	Si8—O12—Si12	167.5 (7)
O10—Si10—O41^iii	110.6 (5)	Si2—O13—Si8	160.5 (6)
O9—Si10—O41^iii	109.1 (5)	Si11—O14—Si5	158.3 (6)
O10—Si11—O14	108.2 (5)	Si1—O15—Si22^vi	149.3 (7)
O10—Si11—O11	110.3 (5)	Si16^vi—O16—Si1	171.9 (7)
O14—Si11—O11	109.9 (5)	Si16^vi—O17—Si7	146.4 (6)
O10—Si11—O22	109.6 (5)	Si21^vi—O18—Si6	142.3 (6)
O14—Si11—O22	110.2 (5)	Si15^vi—O19—Si6	167.9 (6)
O11—Si11—O22	108.7 (5)	Si15^vi—O20—Si12	142.2 (6)
O11—Si12—O24	110.7 (5)	Si5—O21—Si13^vii	145.5 (6)
O11—Si12—O20	109.5 (5)	Si19^vii—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—O21^ii	108.3 (5)	Si16—O30—Si17	155.7 (6)
O42—Si13—O21^ii	108.4 (5)	Si18—O31—Si17	147.3 (6)
O27—Si13—O21^ii	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)
O19^iv—Si15—O28	110.3 (5)	Si20—O39—Si14	163.3 (7)
O19^iv—Si15—O20^iv	111.4 (5)	Si23—O40—Si17	159.3 (5)
O28—Si15—O20^iv	107.4 (5)	Si13—O41—Si10^v	151.3 (6)
O19^iv—Si15—O29	108.3 (5)	Si13—O42—Si4^v	156.8 (6)
O28—Si15—O29	109.4 (5)	Si4^v—O43—Si19	150.5 (6)
O20^iv—Si15—O29	110.0 (5)	Si9^v—O44—Si18	150.2 (6)
O16^iv—Si16—O29	110.0 (5)	Si18—O45—Si3^v	153.4 (6)
O16^iv—Si16—O30	110.2 (5)	Si3—O46—Si24^iii	156.1 (7)
O29—Si16—O30	110.2 (5)	Si1^vii—O47—Si17	150.4 (6)
O16^iv—Si16—O17^iv	108.9 (5)	Si23—O48—Si7^vii	148.0 (7)
O29—Si16—O17^iv	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.

(sin05h_twin_f_co2)

Crystal data

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) Å^3	Coffin shape, colorless
Z = 4	0.17 × 0.09 × 0.07 mm

Data collection

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

Refinement on F^2	2 restraints
Least-squares matrix: full	Primary atom site location: structure-invariant direct methods
R[F^2 > 2σ(F^2)] = 0.058	Secondary atom site location: difference Fourier map
wR(F^2) = 0.159	w = 1/[σ^2(Fo^2) + (0.0652P)^2] where P = (Fo^2 + 2Fc^2)/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

Special details

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 (Ų)

	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 (Ų)

	U^11	U^22	U^33	U^12	U^13	U^23
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)

C200—O202	1.1602	Si14—O32	1.597 (6)
C200—O201	1.1602	Si15—O28	1.590 (6)
O202—O202^i	1.38 (9)	Si15—O20^iv	1.585 (7)
Si1—O15	1.566 (7)	Si15—O19^iv	1.586 (7)
Si1—O47^ii	1.584 (7)	Si15—O29	1.602 (7)
Si1—O1	1.600 (6)	Si16—O16^iv	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—O17^iv	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—O45^iii	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—O42^iii	1.588 (6)	Si18—O45	1.606 (7)
Si4—O43^iii	1.599 (6)	Si19—O23	1.573 (8)
Si4—O3	1.598 (7)	Si19—O33	1.589 (7)
Si5—O5	1.589 (6)	Si19—O22^ii	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—O18^iv	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—O48^ii	1.598 (7)	Si22—O36	1.603 (7)
Si8—O12	1.580 (6)	Si22—O15^iv	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—O44^iii	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—O41^iii	1.592 (6)	Si24—O46^v	1.597 (6)
Si10—O10	1.594 (6)	Si24—O38	1.596 (6)
Si10—O9	1.587 (7)	O15—Si22^vi	1.595 (6)
Si10—O26	1.604 (6)	O16—Si16^vi	1.567 (7)
Si11—O22	1.586 (7)	O17—Si16^vi	1.593 (7)
Si11—O10	1.590 (6)	O18—Si21^vi	1.586 (6)
Si11—O11	1.597 (7)	O19—Si15^vi	1.586 (7)
Si11—O14	1.602 (6)	O20—Si15^vi	1.585 (7)
Si12—O11	1.573 (7)	O21—Si13^vii	1.585 (7)
Si12—O20	1.597 (6)	O22—Si19^vii	1.592 (7)
Si12—O24	1.591 (7)	O41—Si10^v	1.592 (6)
Si12—O12	1.599 (6)	O42—Si4^v	1.588 (6)
Si13—O27	1.584 (6)	O43—Si4^v	1.599 (6)
Si13—O21^ii	1.585 (7)	O44—Si9^v	1.594 (6)
Si13—O42	1.587 (7)	O45—Si3^v	1.581 (6)
Si13—O41	1.606 (6)	O46—Si24^iii	1.597 (6)
Si14—O39	1.588 (6)	O47—Si1^vii	1.584 (7)
Si14—O28	1.598 (6)	O48—Si7^vii	1.598 (7)
Si14—O27	1.592 (7)
O202—C200—O201	180.0	O30—Si16—O17^iv	107.8 (4)
C200—O202—O202^i	135 (8)	O40—Si17—O30	109.5 (3)
O15—Si1—O47^ii	109.9 (3)	O40—Si17—O47	111.2 (3)
O15—Si1—O1	108.3 (4)	O30—Si17—O47	107.8 (3)
O47^ii—Si1—O1	108.2 (4)	O40—Si17—O31	109.5 (3)
O15—Si1—O16	110.8 (4)	O30—Si17—O31	109.5 (4)
O47^ii—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—O45^iii	109.0 (4)	O23—Si19—O22^ii	110.2 (3)
O3—Si3—O46	109.9 (4)	O33—Si19—O22^ii	107.9 (4)
O45^iii—Si3—O46	109.4 (4)	O23—Si19—O43	107.8 (3)
O3—Si3—O2	110.6 (3)	O33—Si19—O43	110.1 (4)
O45^iii—Si3—O2	109.0 (3)	O22^ii—Si19—O43	110.4 (4)
O46—Si3—O2	108.9 (3)	O33—Si20—O34	109.1 (3)
O4—Si4—O42^iii	109.9 (3)	O33—Si20—O39	109.8 (4)
O4—Si4—O43^iii	108.8 (3)	O34—Si20—O39	110.3 (3)
O42^iii—Si4—O43^iii	110.6 (4)	O33—Si20—O38	110.5 (4)
O4—Si4—O3	109.5 (3)	O34—Si20—O38	108.5 (3)
O42^iii—Si4—O3	108.2 (4)	O39—Si20—O38	108.6 (4)
O43^iii—Si4—O3	109.9 (3)	O18^iv—Si21—O25	106.9 (3)
O5—Si5—O14	110.3 (3)	O18^iv—Si21—O35	110.3 (3)
O5—Si5—O21	107.0 (3)	O25—Si21—O35	110.0 (3)
O14—Si5—O21	110.3 (3)	O18^iv—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—O15^iv	108.3 (3)
O19—Si6—O18	108.4 (4)	O36—Si22—O15^iv	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)	O15^iv—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—O48^ii	107.7 (4)	O48—Si23—O37	108.4 (4)
O17—Si7—O48^ii	110.4 (3)	O40—Si23—O37	108.1 (3)
O23—Si7—O48^ii	110.7 (3)	O24—Si24—O37	109.8 (3)
O12—Si8—O13	108.5 (3)	O24—Si24—O46^v	108.4 (4)
O12—Si8—O7	110.8 (4)	O37—Si24—O46^v	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)	O46^v—Si24—O38	110.3 (4)
O7—Si8—O8	107.3 (3)	Si2—O1—Si1	146.9 (4)
O8—Si9—O44^iii	109.5 (4)	Si3—O2—Si2	145.4 (4)
O8—Si9—O25	107.3 (3)	Si3—O3—Si4	160.8 (5)
O44^iii—Si9—O25	109.6 (3)	Si4—O4—Si5	147.1 (4)
O8—Si9—O9	109.3 (4)	Si5—O5—Si6	147.5 (4)
O44^iii—Si9—O9	110.2 (3)	Si2—O6—Si6	163.8 (4)
O25—Si9—O9	110.8 (3)	Si8—O7—Si7	157.6 (5)
O41^iii—Si10—O10	111.3 (4)	Si9—O8—Si8	151.6 (4)
O41^iii—Si10—O9	109.5 (3)	Si10—O9—Si9	151.6 (4)
O10—Si10—O9	109.1 (3)	Si10—O10—Si11	155.5 (4)
O41^iii—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—Si22^vi	150.0 (4)
O10—Si11—O11	110.5 (4)	Si16^vi—O16—Si1	173.1 (5)
O22—Si11—O14	109.9 (3)	Si7—O17—Si16^vi	145.9 (4)
O10—Si11—O14	107.9 (4)	Si21^vi—O18—Si6	141.6 (4)
O11—Si11—O14	110.2 (3)	Si6—O19—Si15^vi	168.3 (5)
O11—Si12—O20	110.0 (3)	Si15^vi—O20—Si12	142.4 (4)
O11—Si12—O24	110.9 (3)	Si13^vii—O21—Si5	146.2 (4)
O20—Si12—O24	106.5 (3)	Si11—O22—Si19^vii	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—O21^ii	109.8 (4)	Si22—O26—Si10	145.8 (3)
O27—Si13—O42	110.4 (4)	Si13—O27—Si14	154.3 (5)
O21^ii—Si13—O42	108.5 (3)	Si15—O28—Si14	149.2 (4)
O27—Si13—O41	110.1 (4)	Si16—O29—Si15	159.7 (4)
O21^ii—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—O20^iv	107.6 (3)	Si24—O38—Si20	154.0 (4)
O28—Si15—O19^iv	110.5 (4)	Si14—O39—Si20	165.2 (5)
O20^iv—Si15—O19^iv	111.5 (4)	Si23—O40—Si17	159.8 (4)
O28—Si15—O29	108.7 (3)	Si10^v—O41—Si13	150.0 (4)
O20^iv—Si15—O29	110.2 (3)	Si13—O42—Si4^v	157.7 (4)
O19^iv—Si15—O29	108.4 (3)	Si4^v—O43—Si19	150.0 (4)
O16^iv—Si16—O29	110.5 (3)	Si9^v—O44—Si18	149.5 (4)
O16^iv—Si16—O30	110.1 (4)	Si3^v—O45—Si18	153.4 (4)
O29—Si16—O30	109.4 (3)	Si3—O46—Si24^iii	156.1 (5)
O16^iv—Si16—O17^iv	109.6 (4)	Si1^vii—O47—Si17	149.5 (4)
O29—Si16—O17^iv	109.4 (3)	Si23—O48—Si7^vii	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.

(sin3h4_twin_f_co2)

Crystal data

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) Å^3	Coffin shape, colorless
Z = 4	0.14 × 0.08 × 0.07 mm

Data collection

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

Refinement on F^2	4 restraints
Least-squares matrix: full	Primary atom site location: structure-invariant direct methods
R[F^2 > 2σ(F^2)] = 0.053	Secondary atom site location: difference Fourier map
wR(F^2) = 0.122	w = 1/[σ^2(Fo^2) + (0.0374P)^2] where P = (Fo^2 + 2Fc^2)/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

Special details

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 (Ų)

	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 (Ų)

	U^11	U^22	U^33	U^12	U^13	U^23
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)

C200—O202	1.1603	Si14—O28	1.613 (6)
C200—O201	1.1604	Si14—O32	1.619 (6)
O202—O202^i	1.24 (9)	Si15—O28	1.578 (6)
C500—O502	1.1598	Si15—O20^iv	1.588 (6)
C500—O501	1.1598	Si15—O19^iv	1.590 (7)
Si1—O15	1.578 (7)	Si15—O29	1.597 (6)
Si1—O1	1.591 (6)	Si16—O30	1.581 (6)
Si1—O47^ii	1.586 (6)	Si16—O16^iv	1.586 (7)
Si1—O16	1.605 (7)	Si16—O29	1.585 (7)
Si2—O13	1.582 (6)	Si16—O17^iv	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—O45^iii	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—O43^iii	1.599 (7)	Si19—O33	1.575 (7)
Si4—O42^iii	1.602 (7)	Si19—O23	1.587 (6)
Si4—O3	1.606 (6)	Si19—O22^ii	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—O18^iv	1.586 (6)
Si6—O19	1.599 (7)	Si21—O35	1.597 (6)
Si6—O5	1.600 (6)	Si21—O25	1.613 (6)
Si7—O48^ii	1.591 (6)	Si21—O34	1.618 (6)
Si7—O23	1.597 (6)	Si22—O15^iv	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—O44^iii	1.595 (6)	Si24—O38	1.585 (6)
Si9—O9	1.607 (7)	Si24—O37	1.586 (7)
Si10—O9	1.587 (6)	Si24—O46^v	1.602 (6)
Si10—O10	1.585 (7)	O15—Si22^vi	1.586 (7)
Si10—O41^iii	1.596 (7)	O16—Si16^vi	1.586 (7)
Si10—O26	1.602 (6)	O17—Si16^vi	1.606 (6)
Si11—O10	1.586 (7)	O18—Si21^vi	1.586 (6)
Si11—O14	1.597 (6)	O19—Si15^vi	1.590 (7)
Si11—O22	1.589 (7)	O20—Si15^vi	1.588 (6)
Si11—O11	1.599 (7)	O21—Si13^vii	1.597 (5)
Si12—O11	1.568 (7)	O22—Si19^vii	1.595 (6)
Si12—O24	1.596 (6)	O41—Si10^v	1.596 (7)
Si12—O20	1.597 (6)	O42—Si4^v	1.602 (7)
Si12—O12	1.599 (6)	O43—Si4^v	1.599 (7)
Si13—O42	1.586 (7)	O44—Si9^v	1.595 (6)
Si13—O27	1.595 (6)	O45—Si3^v	1.593 (7)
Si13—O21^ii	1.597 (5)	O46—Si24^iii	1.602 (6)
Si13—O41	1.609 (7)	O47—Si1^vii	1.586 (6)
Si14—O27	1.586 (6)	O48—Si7^vii	1.591 (6)
Si14—O39	1.597 (6)
O202—C200—O201	180.0	O29—Si16—O17^iv	109.5 (3)
C200—O202—O202^i	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—O47^ii	110.6 (3)	O40—Si17—O31	108.9 (3)
O1—Si1—O47^ii	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)
O47^ii—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—O22^ii	107.6 (4)
O3—Si3—O46	110.3 (4)	O23—Si19—O22^ii	109.9 (3)
O3—Si3—O45^iii	108.9 (4)	O33—Si19—O43	110.5 (4)
O46—Si3—O45^iii	109.0 (4)	O23—Si19—O43	107.6 (3)
O3—Si3—O2	110.6 (3)	O22^ii—Si19—O43	110.6 (4)
O46—Si3—O2	108.7 (3)	O34—Si20—O39	111.3 (3)
O45^iii—Si3—O2	109.3 (3)	O34—Si20—O33	108.7 (3)
O4—Si4—O43^iii	109.4 (3)	O39—Si20—O33	108.7 (4)
O4—Si4—O42^iii	109.5 (3)	O34—Si20—O38	109.0 (3)
O43^iii—Si4—O42^iii	110.1 (4)	O39—Si20—O38	108.5 (4)
O4—Si4—O3	110.2 (3)	O33—Si20—O38	110.6 (4)
O43^iii—Si4—O3	109.9 (3)	O18^iv—Si21—O35	109.9 (3)
O42^iii—Si4—O3	107.7 (3)	O18^iv—Si21—O25	107.0 (3)
O5—Si5—O14	109.8 (3)	O35—Si21—O25	110.1 (3)
O5—Si5—O21	106.9 (3)	O18^iv—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)	O15^iv—Si22—O36	110.0 (4)
O21—Si5—O4	110.3 (3)	O15^iv—Si22—O26	108.3 (3)
O6—Si6—O18	109.9 (4)	O36—Si22—O26	110.0 (3)
O6—Si6—O19	110.8 (4)	O15^iv—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)
O48^ii—Si7—O23	111.3 (3)	O40—Si23—O37	108.0 (3)
O48^ii—Si7—O17	110.1 (4)	O36—Si23—O48	108.7 (4)
O23—Si7—O17	107.3 (3)	O40—Si23—O48	110.2 (3)
O48^ii—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—O46^v	108.0 (3)
O7—Si8—O13	110.3 (4)	O38—Si24—O46^v	110.6 (4)
O12—Si8—O8	110.7 (4)	O37—Si24—O46^v	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—O44^iii	110.5 (4)	Si4—O4—Si5	147.5 (4)
O25—Si9—O44^iii	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)
O44^iii—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—O41^iii	109.6 (3)	Si10—O10—Si11	155.9 (4)
O10—Si10—O41^iii	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)
O41^iii—Si10—O26	107.8 (3)	Si5—O14—Si11	159.5 (4)
O10—Si11—O14	108.1 (4)	Si1—O15—Si22^vi	150.6 (4)
O10—Si11—O22	109.1 (4)	Si16^vi—O16—Si1	173.2 (5)
O14—Si11—O22	110.4 (3)	Si7—O17—Si16^vi	145.6 (4)
O10—Si11—O11	110.6 (4)	Si21^vi—O18—Si6	141.4 (4)
O14—Si11—O11	109.8 (3)	Si15^vi—O19—Si6	167.4 (5)
O22—Si11—O11	108.8 (4)	Si15^vi—O20—Si12	143.2 (4)
O11—Si12—O24	110.8 (3)	Si5—O21—Si13^vii	145.7 (4)
O11—Si12—O20	110.0 (4)	Si19^vii—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—O21^ii	109.0 (3)	Si15—O28—Si14	148.8 (4)
O27—Si13—O21^ii	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)
O21^ii—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—O20^iv	107.5 (3)	Si20—O39—Si14	165.0 (5)
O28—Si15—O19^iv	110.1 (4)	Si17—O40—Si23	160.0 (4)
O20^iv—Si15—O19^iv	111.2 (3)	Si10^v—O41—Si13	150.0 (4)
O28—Si15—O29	108.9 (3)	Si13—O42—Si4^v	157.9 (5)
O20^iv—Si15—O29	110.0 (3)	Si4^v—O43—Si19	150.5 (5)
O19^iv—Si15—O29	109.1 (3)	Si18—O44—Si9^v	150.7 (4)
O30—Si16—O16^iv	110.1 (4)	Si3^v—O45—Si18	153.4 (4)
O30—Si16—O29	109.6 (3)	Si3—O46—Si24^iii	155.5 (5)
O16^iv—Si16—O29	110.4 (3)	Si1^vii—O47—Si17	149.2 (4)
O30—Si16—O17^iv	107.5 (4)	Si7^vii—O48—Si23	148.3 (5)
O16^iv—Si16—O17^iv	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)

Crystal data

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) Å^3	Coffin shape, colorless
Z = 4	0.13 × 0.09 × 0.08 mm

Data collection

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

Refinement on F^2	9 restraints
Least-squares matrix: full	Primary atom site location: structure-invariant direct methods
R[F^2 > 2σ(F^2)] = 0.074	Secondary atom site location: difference Fourier map
wR(F^2) = 0.172	w = 1/[σ^2(Fo^2) + (0.0712P)^2] where P = (Fo^2 + 2Fc^2)/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

Special details

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 (Ų)

	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 (Ų)

	U^11	U^22	U^33	U^12	U^13	U^23
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)

C100—O101^i	0.63 (9)	Si13—O27	1.599 (6)
C100—O101	1.0478	Si13—O41	1.600 (7)
C100—O102	1.0480	Si13—O21^ii	1.602 (6)
C100—C100^i	1.28 (8)	Si14—O27	1.580 (6)
O101—C100^i	0.63 (9)	Si14—O39	1.581 (7)
O101—O101^i	1.16 (7)	Si14—O32	1.601 (6)
O101—O102^i	1.28 (9)	Si14—O28	1.607 (6)
O102—O101^i	1.28 (8)	Si15—O19^iv	1.579 (6)
C200—O202	1.0843	Si15—O28	1.585 (6)
C200—O201	1.1606	Si15—O20^iv	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—O16^iv	1.574 (7)
C400—O402	1.1596	Si16—O29	1.588 (6)
Si1—O47^ii	1.574 (6)	Si16—O17^iv	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—O45^iii	1.590 (6)	Si19—O23	1.581 (7)
Si3—O46	1.592 (6)	Si19—O22^ii	1.587 (6)
Si3—O3	1.593 (6)	Si19—O43	1.594 (7)
Si4—O43^iii	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—O42^iii	1.602 (6)	Si20—O39	1.595 (7)
Si5—O21	1.590 (6)	Si20—O38	1.603 (6)
Si5—O5	1.592 (6)	Si21—O18^iv	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—O15^iv	1.605 (6)
Si7—O23	1.594 (7)	Si23—O48	1.583 (6)
Si7—O17	1.599 (6)	Si23—O40	1.589 (7)
Si7—O48^ii	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—O46^v	1.588 (7)
Si9—O8	1.567 (7)	Si24—O37	1.589 (6)
Si9—O44^iii	1.586 (6)	O15—Si22^vi	1.605 (6)
Si9—O25	1.592 (6)	O16—Si16^vi	1.574 (7)
Si9—O9	1.601 (6)	O17—Si16^vi	1.606 (6)
Si10—O41^iii	1.580 (6)	O18—Si21^vi	1.586 (6)
Si10—O9	1.592 (6)	O19—Si15^vi	1.579 (6)
Si10—O10	1.607 (7)	O20—Si15^vi	1.586 (6)
Si10—O26	1.607 (7)	O21—Si13^vii	1.602 (6)
Si11—O10	1.583 (7)	O22—Si19^vii	1.587 (6)
Si11—O14	1.584 (7)	O41—Si10^v	1.580 (6)
Si11—O22	1.589 (6)	O42—Si4^v	1.602 (6)
Si11—O11	1.604 (7)	O43—Si4^v	1.584 (6)
Si12—O11	1.569 (7)	O44—Si9^v	1.586 (6)
Si12—O20	1.596 (6)	O45—Si3^v	1.590 (6)
Si12—O24	1.596 (6)	O46—Si24^iii	1.588 (7)
Si12—O12	1.596 (6)	O47—Si1^vii	1.574 (6)
Si13—O42	1.594 (6)	O48—Si7^vii	1.606 (6)
O101^i—C100—O101	84 (6)	O28—Si15—O29	108.9 (3)
O101^i—C100—O102	96 (6)	O20^iv—Si15—O29	110.1 (3)
O101—C100—O102	180 (10)	O30—Si16—O16^iv	110.8 (4)
O101^i—C100—C100^i	55 (6)	O30—Si16—O29	109.2 (3)
O101—C100—C100^i	29 (4)	O16^iv—Si16—O29	110.2 (3)
O102—C100—C100^i	151 (4)	O30—Si16—O17^iv	107.5 (4)
C100^i—O101—C100	96 (6)	O16^iv—Si16—O17^iv	109.8 (4)
C100^i—O101—O101^i	64 (6)	O29—Si16—O17^iv	109.2 (3)
C100—O101—O101^i	32 (4)	O40—Si17—O47	111.2 (3)
C100^i—O101—O102^i	55 (6)	O40—Si17—O30	109.5 (4)
C100—O101—O102^i	151 (5)	O47—Si17—O30	107.6 (3)
O101^i—O101—O102^i	118 (8)	O40—Si17—O31	109.0 (3)
C100—O102—O101^i	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)
O47^ii—Si1—O15	109.2 (3)	O44—Si18—O32	109.2 (3)
O47^ii—Si1—O1	107.9 (3)	O31—Si18—O45	109.8 (3)
O15—Si1—O1	108.9 (4)	O44—Si18—O45	110.6 (4)
O47^ii—Si1—O16	111.3 (3)	O32—Si18—O45	110.2 (3)
O15—Si1—O16	110.9 (4)	O23—Si19—O22^ii	110.1 (3)
O1—Si1—O16	108.5 (4)	O23—Si19—O43	107.4 (3)
O6—Si2—O1	111.8 (4)	O22^ii—Si19—O43	110.4 (3)
O6—Si2—O13	108.3 (4)	O23—Si19—O33	110.8 (3)
O1—Si2—O13	109.9 (4)	O22^ii—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—O45^iii	109.7 (3)	O34—Si20—O39	110.3 (3)
O2—Si3—O46	108.6 (3)	O33—Si20—O38	110.3 (4)
O45^iii—Si3—O46	109.4 (4)	O34—Si20—O38	109.6 (3)
O2—Si3—O3	110.2 (3)	O39—Si20—O38	108.7 (4)
O45^iii—Si3—O3	108.6 (3)	O18^iv—Si21—O25	107.2 (3)
O46—Si3—O3	110.4 (4)	O18^iv—Si21—O35	110.8 (3)
O43^iii—Si4—O4	109.2 (3)	O25—Si21—O35	109.9 (3)
O43^iii—Si4—O3	110.3 (3)	O18^iv—Si21—O34	108.8 (3)
O4—Si4—O3	109.7 (3)	O25—Si21—O34	111.8 (3)
O43^iii—Si4—O42^iii	110.3 (3)	O35—Si21—O34	108.2 (3)
O4—Si4—O42^iii	109.6 (3)	O36—Si22—O26	109.8 (3)
O3—Si4—O42^iii	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—O15^iv	109.9 (4)
O5—Si5—O14	110.8 (3)	O26—Si22—O15^iv	107.8 (3)
O21—Si5—O4	111.0 (3)	O35—Si22—O15^iv	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—O46^v	110.5 (4)
O7—Si7—O23	110.1 (3)	O24—Si24—O46^v	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—O48^ii	107.7 (4)	O46^v—Si24—O37	111.1 (4)
O23—Si7—O48^ii	111.1 (3)	Si1—O1—Si2	146.5 (4)
O17—Si7—O48^ii	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—O44^iii	110.3 (4)	Si10—O9—Si9	151.6 (4)
O8—Si9—O25	107.9 (3)	Si11—O10—Si10	154.6 (4)
O44^iii—Si9—O25	109.1 (3)	Si12—O11—Si11	155.5 (5)
O8—Si9—O9	108.9 (4)	Si8—O12—Si12	168.4 (4)
O44^iii—Si9—O9	110.0 (3)	Si8—O13—Si2	160.8 (5)
O25—Si9—O9	110.7 (3)	Si11—O14—Si5	158.3 (4)
O41^iii—Si10—O9	109.7 (3)	Si1—O15—Si22^vi	149.2 (4)
O41^iii—Si10—O10	111.5 (4)	Si16^vi—O16—Si1	172.1 (5)
O9—Si10—O10	108.9 (3)	Si7—O17—Si16^vi	145.4 (4)
O41^iii—Si10—O26	108.3 (3)	Si21^vi—O18—Si6	141.5 (4)
O9—Si10—O26	110.5 (3)	Si15^vi—O19—Si6	167.5 (5)
O10—Si10—O26	107.9 (3)	Si15^vi—O20—Si12	143.4 (4)
O10—Si11—O14	108.5 (3)	Si5—O21—Si13^vii	145.1 (4)
O10—Si11—O22	108.8 (3)	Si19^vii—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—O21^ii	108.9 (3)	Si22—O36—Si23	160.1 (5)
O27—Si13—O21^ii	109.5 (3)	Si24—O37—Si23	154.0 (4)
O41—Si13—O21^ii	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)	Si10^v—O41—Si13	150.4 (4)
O27—Si14—O28	108.0 (3)	Si13—O42—Si4^v	157.3 (4)
O39—Si14—O28	110.8 (3)	Si4^v—O43—Si19	150.7 (4)
O32—Si14—O28	110.0 (3)	Si9^v—O44—Si18	149.8 (4)
O19^iv—Si15—O28	109.6 (4)	Si3^v—O45—Si18	154.0 (4)
O19^iv—Si15—O20^iv	111.3 (4)	Si24^iii—O46—Si3	154.8 (5)
O28—Si15—O20^iv	108.0 (3)	Si1^vii—O47—Si17	150.1 (4)
O19^iv—Si15—O29	108.9 (3)	Si23—O48—Si7^vii	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.

(sin12h3_twin_f_dme)

Crystal data

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) Å^3	0.23 × 0.08 × 0.06 mm

Data collection

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

Refinement on F^2	2 restraints
Least-squares matrix: full	Primary atom site location: structure-invariant direct methods
R[F^2 > 2σ(F^2)] = 0.055	Secondary atom site location: difference Fourier map
wR(F^2) = 0.148	w = 1/[σ^2(Fo^2) + (0.051P)^2] where P = (Fo^2 + 2Fc^2)/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

Special details

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 (Ų)

	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 (Ų)

	U^11	U^22	U^33	U^12	U^13	U^23
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)

C301—O303	1.4006	Si14—O27	1.600 (6)
C302—O303	1.4002	Si15—O19^iii	1.578 (6)
Si1—O47^i	1.573 (6)	Si15—O29	1.592 (6)
Si1—O15	1.574 (7)	Si15—O28	1.595 (6)
Si1—O1	1.586 (6)	Si15—O20^iii	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—O16^iii	1.579 (7)
Si2—O1	1.583 (6)	Si16—O17^iii	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—O45^ii	1.593 (7)	Si18—O31	1.582 (6)
Si4—O4	1.578 (6)	Si18—O32	1.589 (6)
Si4—O43^ii	1.595 (7)	Si18—O44	1.594 (6)
Si4—O42^ii	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—O22^i	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—O18^iii	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—O48^i	1.596 (7)	Si22—O15^iii	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—O44^ii	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—O41^ii	1.593 (7)	Si24—O46^iv	1.604 (6)
Si10—O26	1.597 (7)	O15—Si22^v	1.583 (7)
Si11—O10	1.581 (7)	O16—Si16^v	1.579 (7)
Si11—O11	1.584 (7)	O17—Si16^v	1.595 (7)
Si11—O14	1.592 (7)	O18—Si21^v	1.581 (6)
Si11—O22	1.593 (6)	O19—Si15^v	1.578 (6)
Si12—O11	1.584 (7)	O20—Si15^v	1.595 (6)
Si12—O20	1.587 (6)	O21—Si13^vi	1.597 (6)
Si12—O24	1.588 (7)	O22—Si19^vi	1.581 (6)
Si12—O12	1.601 (6)	O41—Si10^iv	1.593 (7)
Si13—O42	1.581 (7)	O42—Si4^iv	1.597 (7)
Si13—O27	1.583 (6)	O43—Si4^iv	1.594 (7)
Si13—O41	1.597 (7)	O44—Si9^iv	1.595 (6)
Si13—O21^i	1.597 (6)	O45—Si3^iv	1.593 (7)
Si14—O39	1.582 (7)	O46—Si24^ii	1.604 (6)
Si14—O28	1.590 (6)	O47—Si1^vi	1.573 (6)
Si14—O32	1.592 (6)	O48—Si7^vi	1.596 (7)
C302—O303—C301	111.6	O40—Si17—O47	110.7 (3)
O47^i—Si1—O15	109.9 (4)	O40—Si17—O31	109.1 (3)
O47^i—Si1—O1	108.1 (4)	O47—Si17—O31	109.9 (4)
O15—Si1—O1	109.1 (4)	O40—Si17—O30	108.6 (4)
O47^i—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—O22^i	110.6 (3)
O3—Si3—O2	110.6 (4)	O33—Si19—O22^i	107.9 (4)
O46—Si3—O2	108.2 (4)	O23—Si19—O43	107.5 (3)
O3—Si3—O45^ii	109.2 (4)	O33—Si19—O43	110.5 (4)
O46—Si3—O45^ii	109.6 (4)	O22^i—Si19—O43	110.2 (4)
O2—Si3—O45^ii	108.7 (4)	O34—Si20—O39	110.6 (3)
O4—Si4—O43^ii	109.6 (4)	O34—Si20—O33	109.1 (4)
O4—Si4—O42^ii	109.5 (4)	O39—Si20—O33	109.8 (4)
O43^ii—Si4—O42^ii	110.7 (4)	O34—Si20—O38	109.2 (4)
O4—Si4—O3	109.5 (4)	O39—Si20—O38	107.8 (4)
O43^ii—Si4—O3	110.2 (4)	O33—Si20—O38	110.3 (4)
O42^ii—Si4—O3	107.3 (4)	O18^iii—Si21—O25	107.0 (3)
O14—Si5—O21	110.9 (3)	O18^iii—Si21—O34	109.2 (3)
O14—Si5—O5	110.1 (4)	O25—Si21—O34	111.7 (3)
O21—Si5—O5	105.9 (3)	O18^iii—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)	O15^iii—Si22—O36	109.9 (4)
O6—Si6—O19	111.0 (4)	O15^iii—Si22—O26	108.1 (3)
O6—Si6—O18	109.3 (4)	O36—Si22—O26	110.3 (3)
O19—Si6—O18	108.5 (4)	O15^iii—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—O48^i	108.1 (4)	O40—Si23—O37	109.4 (4)
O17—Si7—O48^i	111.2 (4)	O48—Si23—O37	107.9 (4)
O23—Si7—O48^i	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—O46^iv	111.3 (4)
O12—Si8—O8	110.9 (4)	O38—Si24—O46^iv	110.9 (4)
O13—Si8—O8	109.8 (4)	O24—Si24—O46^iv	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—O44^ii	110.0 (4)	Si5—O5—Si6	146.5 (4)
O25—Si9—O44^ii	108.9 (3)	Si2—O6—Si6	162.4 (5)
O9—Si9—O44^ii	109.4 (4)	Si7—O7—Si8	158.2 (5)
O9—Si10—O10	109.6 (4)	Si9—O8—Si8	152.7 (5)
O9—Si10—O41^ii	109.2 (4)	Si10—O9—Si9	151.7 (4)
O10—Si10—O41^ii	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)
O41^ii—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—Si22^v	149.7 (5)
O11—Si11—O14	109.6 (4)	Si16^v—O16—Si1	175.3 (6)
O10—Si11—O22	109.5 (4)	Si7—O17—Si16^v	146.6 (5)
O11—Si11—O22	108.9 (4)	Si21^v—O18—Si6	142.4 (4)
O14—Si11—O22	110.0 (3)	Si15^v—O19—Si6	168.6 (5)
O11—Si12—O20	110.4 (4)	Si12—O20—Si15^v	142.5 (4)
O11—Si12—O24	111.0 (3)	Si5—O21—Si13^vi	145.1 (4)
O20—Si12—O24	106.7 (3)	Si19^vi—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—O21^i	109.9 (4)	Si16—O29—Si15	162.6 (5)
O27—Si13—O21^i	109.6 (4)	Si16—O30—Si17	157.0 (5)
O41—Si13—O21^i	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)
O19^iii—Si15—O29	108.7 (4)	Si24—O38—Si20	155.7 (5)
O19^iii—Si15—O28	110.8 (4)	Si14—O39—Si20	166.0 (5)
O29—Si15—O28	109.5 (3)	Si23—O40—Si17	161.2 (4)
O19^iii—Si15—O20^iii	111.0 (3)	Si10^iv—O41—Si13	150.4 (4)
O29—Si15—O20^iii	109.8 (4)	Si13—O42—Si4^iv	159.8 (5)
O28—Si15—O20^iii	107.1 (3)	Si19—O43—Si4^iv	150.4 (5)
O29—Si16—O30	110.6 (3)	Si18—O44—Si9^iv	149.4 (4)
O29—Si16—O16^iii	110.7 (4)	Si3^iv—O45—Si18	154.4 (5)
O30—Si16—O16^iii	109.8 (4)	Si3—O46—Si24^ii	153.8 (5)
O29—Si16—O17^iii	108.6 (4)	Si1^vi—O47—Si17	150.0 (5)
O30—Si16—O17^iii	108.1 (4)	Si23—O48—Si7^vi	148.6 (5)
O16^iii—Si16—O17^iii	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.

(sin24h3_twin_f_dme)

Crystal data

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) Å^3	0.18 × 0.08 × 0.05 mm

Data collection

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

Refinement on F^2	6 restraints
Least-squares matrix: full	Primary atom site location: structure-invariant direct methods
R[F^2 > 2σ(F^2)] = 0.059	Secondary atom site location: difference Fourier map
wR(F^2) = 0.139	w = 1/[σ^2(Fo^2) + (0.0415P)^2] where P = (Fo^2 + 2Fc^2)/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

Special details

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 (Ų)

	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 (Ų)

	U^11	U^22	U^33	U^12	U^13	U^23
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)

C101—C102^i	1.29 (9)	Si13—O41	1.590 (8)
C101—O103	1.4125	Si13—O21^iii	1.592 (7)
C102—O103^i	1.01 (8)	Si13—O42	1.590 (7)
C102—C102^i	1.10 (10)	Si14—O27	1.597 (7)
C102—C101^i	1.29 (9)	Si14—O32	1.602 (7)
C102—O103	1.4047	Si14—O28	1.605 (6)
O103—C102^i	1.01 (7)	Si14—O39	1.607 (6)
C201—O203^ii	1.07 (5)	Si15—O19^v	1.574 (7)
C201—C201^ii	1.38 (5)	Si15—O29	1.581 (7)
C201—O203	1.4098	Si15—O20^v	1.585 (6)
C202—O203	1.4080	Si15—O28	1.587 (6)
O203—C201^ii	1.07 (7)	Si16—O30	1.565 (6)
C301—O303	1.3933	Si16—O16^v	1.581 (7)
C302—O303	1.3912	Si16—O29	1.591 (7)
Si1—O15	1.567 (7)	Si16—O17^v	1.610 (7)
Si1—O1	1.581 (7)	Si17—O40	1.577 (7)
Si1—O47^iii	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—O22^iii	1.587 (7)
Si3—O45^iv	1.620 (7)	Si19—O23	1.588 (8)
Si4—O43^iv	1.575 (7)	Si19—O43	1.612 (7)
Si4—O4	1.586 (7)	Si20—O39	1.570 (7)
Si4—O42^iv	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—O18^v	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—O15^v	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—O48^iii	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—O46^vi	1.617 (7)
Si9—O44^iv	1.598 (7)	O15—Si22^vii	1.578 (8)
Si9—O25	1.597 (6)	O16—Si16^vii	1.581 (7)
Si9—O9	1.606 (7)	O17—Si16^vii	1.610 (7)
Si10—O10	1.578 (7)	O18—Si21^vii	1.592 (7)
Si10—O9	1.589 (7)	O19—Si15^vii	1.574 (7)
Si10—O41^iv	1.614 (7)	O20—Si15^vii	1.585 (6)
Si10—O26	1.618 (8)	O21—Si13^viii	1.592 (7)
Si11—O11	1.573 (8)	O22—Si19^viii	1.587 (7)
Si11—O14	1.581 (7)	O41—Si10^vi	1.614 (7)
Si11—O10	1.594 (7)	O42—Si4^vi	1.590 (7)
Si11—O22	1.605 (7)	O43—Si4^vi	1.575 (7)
Si12—O24	1.581 (6)	O44—Si9^vi	1.598 (7)
Si12—O12	1.589 (7)	O45—Si3^vi	1.620 (7)
Si12—O20	1.597 (6)	O46—Si24^iv	1.617 (7)
Si12—O11	1.607 (7)	O47—Si1^viii	1.586 (6)
Si13—O27	1.583 (7)	O48—Si7^viii	1.601 (7)
C102^i—C101—O103	44 (4)	O29—Si15—O28	109.1 (4)
O103^i—C102—C102^i	83 (8)	O20^v—Si15—O28	107.3 (4)
O103^i—C102—C101^i	75 (5)	O30—Si16—O16^v	109.4 (4)
C102^i—C102—C101^i	155 (8)	O30—Si16—O29	110.6 (4)
O103^i—C102—O103	129 (6)	O16^v—Si16—O29	110.5 (4)
C102^i—C102—O103	46 (4)	O30—Si16—O17^v	108.2 (4)
C101^i—C102—O103	154 (3)	O16^v—Si16—O17^v	108.7 (4)
C102^i—O103—C102	51 (6)	O29—Si16—O17^v	109.5 (4)
C102^i—O103—C101	62 (6)	O40—Si17—O47	111.3 (4)
C102—O103—C101	111.7	O40—Si17—O31	109.0 (4)
O203^ii—C201—C201^ii	69 (2)	O47—Si17—O31	109.6 (4)
O203^ii—C201—O203	114 (4)	O40—Si17—O30	108.8 (4)
C201^ii—C201—O203	45 (3)	O47—Si17—O30	108.0 (4)
C201^ii—O203—C202	171 (3)	O31—Si17—O30	110.1 (4)
C201^ii—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—O47^iii	110.6 (4)	O45—Si18—O44	110.9 (4)
O1—Si1—O47^iii	108.3 (4)	O32—Si18—O44	110.3 (4)
O15—Si1—O16	110.4 (4)	O33—Si19—O22^iii	107.4 (4)
O1—Si1—O16	109.0 (4)	O33—Si19—O23	110.7 (4)
O47^iii—Si1—O16	109.8 (4)	O22^iii—Si19—O23	111.0 (3)
O13—Si2—O6	108.7 (4)	O33—Si19—O43	109.7 (4)
O13—Si2—O1	109.8 (4)	O22^iii—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—O45^iv	110.3 (4)	O25—Si21—O18^v	106.9 (3)
O3—Si3—O45^iv	108.9 (4)	O25—Si21—O35	110.6 (3)
O46—Si3—O45^iv	109.5 (4)	O18^v—Si21—O35	109.4 (4)
O43^iv—Si4—O4	109.5 (4)	O25—Si21—O34	111.0 (3)
O43^iv—Si4—O42^iv	110.0 (4)	O18^v—Si21—O34	110.0 (4)
O4—Si4—O42^iv	109.3 (4)	O35—Si21—O34	108.8 (4)
O43^iv—Si4—O3	109.9 (4)	O15^v—Si22—O26	108.6 (4)
O4—Si4—O3	110.0 (4)	O15^v—Si22—O36	110.3 (4)
O42^iv—Si4—O3	108.2 (4)	O26—Si22—O36	110.3 (4)
O5—Si5—O21	107.2 (4)	O15^v—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—O46^vi	111.5 (4)
O17—Si7—O48^iii	110.2 (4)	O38—Si24—O46^vi	110.2 (4)
O23—Si7—O48^iii	110.5 (4)	O24—Si24—O46^vi	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)
O48^iii—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—O44^iv	110.6 (4)	Si10—O10—Si11	156.7 (5)
O8—Si9—O25	108.2 (3)	Si11—O11—Si12	154.7 (5)
O44^iv—Si9—O25	109.0 (3)	Si8—O12—Si12	168.8 (5)
O8—Si9—O9	108.5 (4)	Si2—O13—Si8	163.7 (5)
O44^iv—Si9—O9	109.2 (4)	Si11—O14—Si5	160.2 (5)
O25—Si9—O9	111.3 (3)	Si1—O15—Si22^vii	150.8 (5)
O10—Si10—O9	109.6 (4)	Si16^vii—O16—Si1	174.8 (6)
O10—Si10—O41^iv	110.4 (4)	Si7—O17—Si16^vii	146.8 (5)
O9—Si10—O41^iv	109.7 (4)	Si21^vii—O18—Si6	142.2 (5)
O10—Si10—O26	109.0 (3)	Si15^vii—O19—Si6	167.0 (5)
O9—Si10—O26	110.8 (3)	Si15^vii—O20—Si12	142.8 (4)
O41^iv—Si10—O26	107.3 (4)	Si5—O21—Si13^viii	146.3 (5)
O11—Si11—O14	109.8 (4)	Si19^viii—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—O21^iii	110.5 (4)	Si21—O35—Si22	151.2 (4)
O41—Si13—O21^iii	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)
O21^iii—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—Si10^vi	149.3 (5)
O32—Si14—O28	109.3 (4)	Si4^vi—O42—Si13	158.5 (5)
O27—Si14—O39	111.1 (4)	Si4^vi—O43—Si19	151.2 (5)
O32—Si14—O39	108.1 (4)	Si18—O44—Si9^vi	150.2 (5)
O28—Si14—O39	111.5 (4)	Si18—O45—Si3^vi	154.9 (5)
O19^v—Si15—O29	109.2 (4)	Si3—O46—Si24^iv	153.6 (5)
O19^v—Si15—O20^v	111.5 (4)	Si1^viii—O47—Si17	149.8 (5)
O29—Si15—O20^v	110.1 (4)	Si23—O48—Si7^viii	149.0 (6)
O19^v—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.

(str12h_twin_f_dme)

Crystal data

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) Å^3	Coffin shape, colorless
Z = 4	0.23 × 0.13 × 0.08 mm

Data collection

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

Refinement on F^2	2 restraints
Least-squares matrix: full	Primary atom site location: structure-invariant direct methods
R[F^2 > 2σ(F^2)] = 0.060	Secondary atom site location: difference Fourier map
wR(F^2) = 0.198	w = 1/[σ^2(Fo^2) + (0.1204P)^2] where P = (Fo^2 + 2Fc^2)/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

Special details

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 (Ų)

	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 (Ų)

	U^11	U^22	U^33	U^12	U^13	U^23
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)

C301—O303	1.4069	Si14—O27	1.595 (4)
C302—O303	1.4077	Si15—O19^iii	1.582 (4)
Si1—O47^i	1.585 (3)	Si15—O28	1.597 (4)
Si1—O15	1.586 (4)	Si15—O20^iii	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—O16^iii	1.589 (4)
Si2—O2	1.595 (4)	Si16—O17^iii	1.602 (3)
Si2—O1	1.598 (4)	Si17—O40	1.590 (4)
Si3—O45^ii	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—O43^ii	1.593 (4)	Si18—O31	1.605 (3)
Si4—O4	1.597 (4)	Si18—O44	1.608 (4)
Si4—O42^ii	1.601 (4)	Si19—O23	1.591 (4)
Si5—O21	1.594 (3)	Si19—O33	1.591 (4)
Si5—O5	1.595 (4)	Si19—O22^i	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—O18^iii	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—O48^i	1.599 (3)	Si22—O36	1.596 (4)
Si8—O8	1.577 (4)	Si22—O26	1.597 (3)
Si8—O7	1.586 (4)	Si22—O15^iii	1.598 (4)
Si8—O12	1.587 (4)	Si22—O35	1.602 (3)
Si8—O13	1.592 (4)	Si23—O37	1.586 (4)
Si9—O44^ii	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—O46^iv	1.576 (5)
Si10—O41^ii	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—Si22^v	1.598 (4)
Si11—O10	1.586 (4)	O16—Si16^v	1.589 (4)
Si11—O22	1.595 (3)	O17—Si16^v	1.602 (3)
Si11—O14	1.597 (4)	O18—Si21^v	1.591 (4)
Si11—O11	1.600 (4)	O19—Si15^v	1.582 (4)
Si12—O11	1.587 (4)	O20—Si15^v	1.595 (4)
Si12—O24	1.591 (4)	O21—Si13^vi	1.602 (3)
Si12—O20	1.594 (4)	O22—Si19^vi	1.593 (3)
Si12—O12	1.600 (4)	O41—Si10^iv	1.587 (4)
Si13—O42	1.587 (4)	O42—Si4^iv	1.600 (4)
Si13—O27	1.593 (4)	O43—Si4^iv	1.593 (4)
Si13—O41	1.602 (4)	O44—Si9^iv	1.582 (4)
Si13—O21^i	1.602 (3)	O45—Si3^iv	1.591 (4)
Si14—O39	1.580 (4)	O46—Si24^ii	1.576 (5)
Si14—O28	1.594 (4)	O47—Si1^vi	1.585 (3)
Si14—O32	1.595 (4)	O48—Si7^vi	1.599 (3)
C301—O303—C302	111.7	O40—Si17—O30	109.8 (2)
O47^i—Si1—O15	109.48 (19)	O40—Si17—O31	109.2 (2)
O47^i—Si1—O1	107.6 (2)	O30—Si17—O31	110.1 (2)
O15—Si1—O1	109.4 (2)	O40—Si17—O47	110.69 (19)
O47^i—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)
O45^ii—Si3—O46	109.6 (3)	O23—Si19—O22^i	110.7 (2)
O45^ii—Si3—O3	108.5 (2)	O33—Si19—O22^i	107.5 (2)
O46—Si3—O3	111.0 (2)	O23—Si19—O43	107.4 (2)
O45^ii—Si3—O2	109.9 (2)	O33—Si19—O43	110.0 (2)
O46—Si3—O2	108.7 (2)	O22^i—Si19—O43	110.2 (2)
O3—Si3—O2	109.0 (2)	O33—Si20—O34	108.6 (2)
O3—Si4—O43^ii	110.6 (2)	O33—Si20—O38	110.4 (2)
O3—Si4—O4	109.4 (2)	O34—Si20—O38	109.5 (2)
O43^ii—Si4—O4	109.1 (2)	O33—Si20—O39	109.5 (2)
O3—Si4—O42^ii	108.1 (2)	O34—Si20—O39	110.6 (2)
O43^ii—Si4—O42^ii	110.6 (2)	O38—Si20—O39	108.2 (2)
O4—Si4—O42^ii	109.0 (2)	O18^iii—Si21—O25	107.0 (2)
O21—Si5—O5	106.91 (19)	O18^iii—Si21—O35	110.3 (2)
O21—Si5—O14	110.82 (18)	O25—Si21—O35	110.60 (19)
O5—Si5—O14	110.4 (2)	O18^iii—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—O15^iii	109.4 (2)
O5—Si6—O18	108.69 (19)	O26—Si22—O15^iii	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)	O15^iii—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—O48^i	107.1 (2)	O36—Si23—O40	109.3 (2)
O17—Si7—O48^i	111.1 (2)	O48—Si23—O40	110.7 (2)
O23—Si7—O48^i	110.6 (2)	O46^iv—Si24—O38	110.1 (2)
O8—Si8—O7	107.9 (2)	O46^iv—Si24—O37	111.0 (2)
O8—Si8—O12	111.1 (2)	O38—Si24—O37	109.4 (2)
O7—Si8—O12	110.6 (3)	O46^iv—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)
O44^ii—Si9—O8	110.1 (2)	Si2—O2—Si3	145.6 (3)
O44^ii—Si9—O25	109.1 (2)	Si4—O3—Si3	161.2 (3)
O8—Si9—O25	108.4 (2)	Si4—O4—Si5	148.1 (2)
O44^ii—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)
O41^ii—Si10—O9	109.1 (2)	Si8—O8—Si9	152.6 (3)
O41^ii—Si10—O10	111.6 (2)	Si10—O9—Si9	151.5 (3)
O9—Si10—O10	109.0 (2)	Si11—O10—Si10	154.8 (3)
O41^ii—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—Si22^v	149.3 (3)
O22—Si11—O14	110.14 (19)	Si16^v—O16—Si1	172.7 (3)
O10—Si11—O11	110.2 (2)	Si7—O17—Si16^v	146.2 (3)
O22—Si11—O11	108.0 (2)	Si21^v—O18—Si6	142.0 (3)
O14—Si11—O11	110.2 (2)	Si15^v—O19—Si6	169.0 (3)
O11—Si12—O24	110.04 (19)	Si12—O20—Si15^v	142.9 (3)
O11—Si12—O20	110.0 (2)	Si5—O21—Si13^vi	145.0 (3)
O24—Si12—O20	106.8 (2)	Si19^vi—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—O21^i	109.05 (19)	Si16—O29—Si15	159.5 (4)
O27—Si13—O21^i	108.5 (2)	Si16—O30—Si17	156.5 (3)
O41—Si13—O21^i	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)
O19^iii—Si15—O28	109.6 (2)	Si24—O38—Si20	156.0 (3)
O19^iii—Si15—O20^iii	110.6 (2)	Si14—O39—Si20	165.6 (4)
O28—Si15—O20^iii	108.1 (2)	Si17—O40—Si23	161.0 (3)
O19^iii—Si15—O29	109.3 (2)	Si10^iv—O41—Si13	150.6 (3)
O28—Si15—O29	108.7 (2)	Si13—O42—Si4^iv	157.7 (3)
O20^iii—Si15—O29	110.4 (2)	Si4^iv—O43—Si19	150.7 (3)
O29—Si16—O30	108.6 (2)	Si9^iv—O44—Si18	149.8 (2)
O29—Si16—O16^iii	110.0 (2)	Si18—O45—Si3^iv	155.3 (3)
O30—Si16—O16^iii	110.7 (2)	Si24^ii—O46—Si3	155.6 (3)
O29—Si16—O17^iii	109.5 (2)	Si1^vi—O47—Si17	149.1 (3)
O30—Si16—O17^iii	108.1 (2)	Si23—O48—Si7^vi	148.1 (3)
O16^iii—Si16—O17^iii	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.

(str24h_twin_f_dme)

Crystal data

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) Å^3	Coffin shape, colorless
Z = 4	0.25 × 0.09 × 0.09 mm

Data collection

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

Refinement on F^2	2 restraints
Least-squares matrix: full	Primary atom site location: structure-invariant direct methods
R[F^2 > 2σ(F^2)] = 0.059	Secondary atom site location: difference Fourier map
wR(F^2) = 0.192	w = 1/[σ^2(Fo^2) + (0.1189P)^2 + 2.6558P] where P = (Fo^2 + 2Fc^2)/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

Special details

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 (Ų)

	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 (Ų)

	U^11	U^22	U^33	U^12	U^13	U^23
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)

C301—O303	1.4048	Si14—O28	1.594 (4)
C302—O303	1.4055	Si15—O19^iii	1.589 (4)
Si1—O15	1.584 (4)	Si15—O20^iii	1.591 (4)
Si1—O1	1.585 (4)	Si15—O28	1.592 (4)
Si1—O47^i	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—O16^iii	1.597 (4)
Si2—O2	1.593 (4)	Si16—O17^iii	1.594 (3)
Si2—O1	1.594 (3)	Si17—O40	1.587 (3)
Si3—O46	1.591 (4)	Si17—O31	1.591 (3)
Si3—O45^ii	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—O43^ii	1.594 (3)	Si18—O44	1.602 (4)
Si4—O4	1.594 (3)	Si18—O31	1.604 (3)
Si4—O42^ii	1.602 (3)	Si19—O23	1.586 (3)
Si5—O21	1.593 (3)	Si19—O33	1.590 (4)
Si5—O5	1.594 (3)	Si19—O22^i	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—O18^iii	1.590 (4)
Si7—O7	1.594 (4)	Si21—O35	1.605 (3)
Si7—O48^i	1.595 (3)	Si21—O34	1.611 (4)
Si7—O17	1.596 (4)	Si22—O15^iii	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—O44^ii	1.593 (4)	Si23—O40	1.592 (3)
Si9—O25	1.595 (3)	Si23—O48	1.593 (3)
Si9—O9	1.608 (3)	Si24—O46^iv	1.590 (4)
Si10—O41^ii	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—Si22^v	1.592 (4)
Si11—O14	1.587 (3)	O16—Si16^v	1.597 (4)
Si11—O10	1.590 (4)	O17—Si16^v	1.594 (3)
Si11—O22	1.592 (3)	O18—Si21^v	1.590 (4)
Si11—O11	1.598 (4)	O19—Si15^v	1.589 (4)
Si12—O11	1.584 (3)	O20—Si15^v	1.591 (4)
Si12—O24	1.586 (3)	O21—Si13^vi	1.596 (3)
Si12—O12	1.594 (4)	O22—Si19^vi	1.591 (3)
Si12—O20	1.594 (4)	O41—Si10^iv	1.589 (4)
Si13—O42	1.584 (4)	O42—Si4^iv	1.602 (3)
Si13—O41	1.600 (4)	O43—Si4^iv	1.594 (3)
Si13—O21^i	1.596 (3)	O44—Si9^iv	1.593 (4)
Si13—O27	1.597 (4)	O45—Si3^iv	1.593 (4)
Si14—O39	1.580 (4)	O46—Si24^ii	1.590 (4)
Si14—O27	1.590 (3)	O47—Si1^vi	1.588 (3)
Si14—O32	1.591 (3)	O48—Si7^vi	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—O47^i	109.51 (19)	O31—Si17—O30	110.2 (2)
O1—Si1—O47^i	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)
O47^i—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—O45^ii	109.7 (2)	O23—Si19—O22^i	110.48 (19)
O46—Si3—O3	110.9 (2)	O33—Si19—O22^i	107.7 (2)
O45^ii—Si3—O3	108.4 (2)	O23—Si19—O43	107.3 (2)
O46—Si3—O2	108.3 (2)	O33—Si19—O43	110.1 (2)
O45^ii—Si3—O2	110.1 (2)	O22^i—Si19—O43	110.4 (2)
O3—Si3—O2	109.4 (2)	O34—Si20—O33	108.6 (2)
O3—Si4—O43^ii	110.6 (2)	O34—Si20—O39	110.7 (2)
O3—Si4—O4	109.8 (2)	O33—Si20—O39	109.7 (2)
O43^ii—Si4—O4	108.94 (19)	O34—Si20—O38	109.1 (2)
O3—Si4—O42^ii	108.0 (2)	O33—Si20—O38	110.2 (2)
O43^ii—Si4—O42^ii	110.3 (2)	O39—Si20—O38	108.5 (2)
O4—Si4—O42^ii	109.27 (19)	O25—Si21—O18^iii	107.02 (19)
O21—Si5—O5	107.00 (18)	O25—Si21—O35	110.60 (18)
O21—Si5—O14	110.83 (18)	O18^iii—Si21—O35	110.2 (2)
O5—Si5—O14	110.3 (2)	O25—Si21—O34	111.7 (2)
O21—Si5—O4	110.61 (18)	O18^iii—Si21—O34	109.18 (19)
O5—Si5—O4	109.98 (18)	O35—Si21—O34	108.2 (2)
O14—Si5—O4	108.2 (2)	O15^iii—Si22—O36	109.6 (2)
O5—Si6—O6	109.2 (2)	O15^iii—Si22—O26	108.12 (18)
O5—Si6—O18	108.76 (19)	O36—Si22—O26	109.8 (2)
O6—Si6—O18	110.2 (2)	O15^iii—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—O48^i	110.48 (19)	O37—Si23—O40	108.8 (2)
O7—Si7—O48^i	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)
O48^i—Si7—O17	110.9 (2)	O46^iv—Si24—O38	110.3 (2)
O7—Si8—O13	110.1 (2)	O46^iv—Si24—O37	111.0 (2)
O7—Si8—O12	110.9 (3)	O38—Si24—O37	109.4 (2)
O13—Si8—O12	108.6 (2)	O46^iv—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—O44^ii	110.4 (2)	Si2—O2—Si3	145.7 (2)
O8—Si9—O25	108.0 (2)	Si4—O3—Si3	161.3 (3)
O44^ii—Si9—O25	108.6 (2)	Si4—O4—Si5	148.0 (2)
O8—Si9—O9	109.2 (2)	Si6—O5—Si5	148.6 (2)
O44^ii—Si9—O9	109.5 (2)	Si2—O6—Si6	163.5 (3)
O25—Si9—O9	110.83 (18)	Si8—O7—Si7	157.4 (3)
O41^ii—Si10—O9	109.2 (2)	Si9—O8—Si8	152.4 (3)
O41^ii—Si10—O10	111.5 (2)	Si10—O9—Si9	151.4 (3)
O9—Si10—O10	108.9 (2)	Si11—O10—Si10	155.2 (3)
O41^ii—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—Si22^v	149.4 (2)
O10—Si11—O22	109.5 (2)	Si16^v—O16—Si1	173.0 (3)
O14—Si11—O11	110.3 (2)	Si16^v—O17—Si7	146.3 (2)
O10—Si11—O11	110.2 (2)	Si21^v—O18—Si6	142.3 (3)
O22—Si11—O11	107.9 (2)	Si15^v—O19—Si6	169.0 (3)
O11—Si12—O24	109.96 (19)	Si15^v—O20—Si12	143.0 (3)
O11—Si12—O12	109.0 (2)	Si5—O21—Si13^vi	145.1 (2)
O24—Si12—O12	111.7 (2)	Si19^vi—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—O21^i	108.99 (18)	Si14—O27—Si13	152.8 (3)
O41—Si13—O21^i	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)
O21^i—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)
O19^iii—Si15—O20^iii	110.4 (2)	Si24—O38—Si20	155.8 (3)
O19^iii—Si15—O28	109.5 (2)	Si14—O39—Si20	165.9 (4)
O20^iii—Si15—O28	108.1 (2)	Si17—O40—Si23	161.1 (2)
O19^iii—Si15—O29	109.2 (2)	Si10^iv—O41—Si13	150.3 (3)
O20^iii—Si15—O29	110.7 (2)	Si13—O42—Si4^iv	157.9 (3)
O28—Si15—O29	108.8 (2)	Si4^iv—O43—Si19	150.7 (3)
O29—Si16—O30	109.0 (2)	Si9^iv—O44—Si18	149.5 (2)
O29—Si16—O16^iii	109.8 (2)	Si18—O45—Si3^iv	155.5 (2)
O30—Si16—O16^iii	110.4 (2)	Si24^ii—O46—Si3	155.1 (3)
O29—Si16—O17^iii	109.7 (2)	Si1^vi—O47—Si17	148.9 (3)
O30—Si16—O17^iii	108.1 (2)	Si23—O48—Si7^vi	148.2 (3)
O16^iii—Si16—O17^iii	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.