data_global _publ_requested_journal 'Organometallics' _publ_requested_category FM _publ_contact_letter ; Please consider this CIF submission for deposition. The paper will be submitted to Organometallics. Kind regards! Ferdinand Belaj ; _publ_section_title ; Silanetriols as powerful starting materials for the selective condensation to bulky POSS cages ; loop_ _publ_author_name _publ_author_address 'Natascha Hurkes' ; University Kassel, Institut f. Chemie und CINSaT, Heinrich-Plett-Straße 40, 34132 Kassel, Germany ; 'Clemens Bruhn' ; University Kassel, Institut f. Chemie und CINSaT, Heinrich-Plett-Straße 40, 34132 Kassel, Germany ; 'Ferdinand Belaj' ; Institute of Chemistry, Karl-Franzens University Graz, Schubertstr. 1, A-8010 Graz, Austria ; 'Rudolf Pietschnig' ; University Kassel, Institut f. Chemie und CINSaT, Heinrich-Plett-Straße 40, 34132 Kassel, Germany ; _publ_contact_author_name 'Ferdinand Belaj' _publ_contact_author_address ; Institute of Chemistry, Karl-Franzens University Graz, Schubertstr. 1, A-8010 Graz, Austria ; _publ_contact_author_email 'ferdinand.belaj@uni-graz.at' _publ_contact_author_fax '43(316)3809835' _publ_contact_author_phone '43(316)3805288' #---------------------------------------------------------------------------- data_2b_NH156 _audit_author_name 'Ferdinand Belaj' _audit_creation_method 'manual edited SHELXL-97 .cif file' _chemical_compound_source 'synthetical product' _chemical_name_systematic ; 1,3-bis(1,1-dimethylpropyl)-1,1,3,3-tetrahydroxydisiloxane ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety 'C10 H26 O5 Si2' _chemical_formula_sum 'C10 H26 O5 Si2' _chemical_formula_weight 282.49 loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source 'C' 'C' 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'H' 'H' 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'O' 'O' 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'Si' 'Si' 0.0817 0.0704 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting monoclinic _symmetry_space_group_name_H-M 'C 2/m' _symmetry_space_group_name_Hall '-C 2y' loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' 'x, -y, z' 'x+1/2, y+1/2, z' 'x+1/2, -y+1/2, z' '-x, -y, -z' '-x, y, -z' '-x+1/2, -y+1/2, -z' '-x+1/2, y+1/2, -z' _cell_length_a 7.2163(4) _cell_length_b 10.1628(5) _cell_length_c 10.6832(5) _cell_angle_alpha 90.00 _cell_angle_beta 98.4520(10) _cell_angle_gamma 90.00 _cell_volume 774.97(7) _cell_formula_units_Z 2 _cell_measurement_temperature 100(2) _cell_measurement_reflns_used 2261 _cell_measurement_theta_min 3.49 _cell_measurement_theta_max 30.48 _exptl_crystal_description 'plate' _exptl_crystal_colour 'colourless' _exptl_crystal_size_max 0.40 _exptl_crystal_size_mid 0.38 _exptl_crystal_size_min 0.18 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.211 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 308 _exptl_absorpt_coefficient_mu 0.236 _exptl_absorpt_correction_type 'multi-scan' _exptl_absorpt_correction_T_min 0.827 _exptl_absorpt_correction_T_max 1.000 _exptl_absorpt_process_details 'Bruker SADABS' _exptl_special_details ; ? ; _diffrn_ambient_temperature 100(2) _diffrn_measurement_device_type 'Bruker APEX-II CCD' _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_type 'MoK\a' _diffrn_radiation_monochromator 'graphite' _diffrn_radiation_wavelength 0.71073 _diffrn_measurement_method '\f and \w scans' _diffrn_detector_area_resol_mean ? _diffrn_standards_number 0 _diffrn_standards_interval_count ? _diffrn_standards_decay_% ? _diffrn_reflns_number 2799 _diffrn_reflns_av_R_equivalents 0.0167 _diffrn_reflns_av_sigmaI/netI 0.0160 _diffrn_reflns_limit_h_min -10 _diffrn_reflns_limit_h_max 7 _diffrn_reflns_limit_k_min -14 _diffrn_reflns_limit_k_max 12 _diffrn_reflns_limit_l_min -15 _diffrn_reflns_limit_l_max 15 _diffrn_reflns_theta_min 3.49 _diffrn_reflns_theta_max 30.00 _reflns_number_total 1164 _reflns_number_gt 1095 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'Bruker APEX2' _computing_cell_refinement 'Bruker SAINT' _computing_data_reduction 'Bruker SAINT' _computing_structure_solution 'SHELXS-97 (Sheldrick, 2008)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 2008)' _computing_molecular_graphics 'modified ORTEP (Johnson, 1965)' _computing_publication_material 'SHELXL-97 (Sheldrick, 2008)' _refine_special_details ; Refinement of F^2^ against ALL reflections. The weighted R-factor wR and goodness of fit S are based on F^2^, conventional R-factors R are based on F, with F set to zero for negative F^2^. The threshold expression of F^2^ > 2sigma(F^2^) is used only for calculating R-factors(gt) etc. and is not relevant to the choice of reflections for refinement. R-factors based on F^2^ are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger. The H atoms of the OH group are disordered over two sites. They were refined with a common isotropic displacement parameter and with site occupation factors of 0.5. Only the bond length was fixed to be 0.84 \%A (DFIX of SHELXL-97), no angular or conformational constraints were applied. The 2-methyl-2-butyl group is disordered over two sites: The central C atom and one methyl group lie on the crystallographic mirror plane, the methyl group on one side and the ethyl group on the other side of that plane are disordered and were refined with site occupation factors of 0.5. The non-hydrogen atoms were refined with anisotropic displacement parameters without any constraints. The H atoms of the disordered CH~2~ group were included at calculated positions at C-H distances of 0.99 \%A with their isotropic displacement parameters fixed to 1.2 times U~eq~ of the C atom they are bonded to (AFIX 23 of SHELXL-97). The H atoms of the ordered methyl group were refined with a common isotropic displacement parameter and idealized geometry with tetrahedral angles, staggered conformation, and C-H distances of 0.98 \%A. The H atoms of the disordered methyl group were included at calculated positions at C-H distances of 0.98 \%A with their isotropic displacement parameters fixed to 1.3 times U~eq~ of the C atom they are bonded to (AFIX 23 of SHELXL-97). ; _refine_ls_structure_factor_coef Fsqd _refine_ls_matrix_type full _refine_ls_weighting_scheme calc _refine_ls_weighting_details 'calc w=1/[\s^2^(Fo^2^)+(0.0563P)^2^+0.5737P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment refU _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 1164 _refine_ls_number_parameters 67 _refine_ls_number_restraints 2 _refine_ls_R_factor_all 0.0369 _refine_ls_R_factor_gt 0.0348 _refine_ls_wR_factor_ref 0.0967 _refine_ls_wR_factor_gt 0.0940 _refine_ls_goodness_of_fit_ref 1.082 _refine_ls_restrained_S_all 1.081 _refine_ls_shift/su_max 0.001 _refine_ls_shift/su_mean 0.000 loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_occupancy _atom_site_symmetry_multiplicity _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group O1 O 1.0000 0.5000 1.0000 0.0240(3) Uani 1 4 d S . . Si1 Si 0.78370(5) 0.5000 0.93746(4) 0.01463(14) Uani 1 2 d S . . O2 O 0.68097(11) 0.62840(8) 0.98862(9) 0.0233(2) Uani 1 1 d D . . H1 H 0.5655(9) 0.627(3) 0.992(3) 0.023(5) Uiso 0.50 1 d PD . . H2 H 0.728(4) 0.7041(13) 0.998(3) 0.023(5) Uiso 0.50 1 d PD . . C1 C 0.7648(3) 0.5000 0.76238(17) 0.0315(4) Uani 1 2 d S . . C2 C 0.5493(4) 0.5000 0.7087(2) 0.0509(6) Uani 1 2 d S A . H21 H 0.5329 0.5000 0.6160 0.077(6) Uiso 1 2 calc SR . . H22 H 0.4905 0.5787 0.7384 0.077(6) Uiso 1 1 calc PR . . C3 C 0.8487(9) 0.3751(9) 0.7187(9) 0.0338(16) Uani 0.50 1 d P A 1 H31 H 0.8487 0.3790 0.6270 0.044 Uiso 0.50 1 calc PR A 1 H32 H 0.7742 0.2995 0.7390 0.044 Uiso 0.50 1 calc PR A 1 H33 H 0.9776 0.3656 0.7617 0.044 Uiso 0.50 1 calc PR A 1 C4 C 0.8741(16) 0.6251(10) 0.7245(10) 0.064(3) Uani 0.50 1 d P A 2 H41 H 0.8319 0.7032 0.7679 0.077 Uiso 0.50 1 calc PR A 2 H42 H 1.0096 0.6131 0.7542 0.077 Uiso 0.50 1 calc PR A 2 C5 C 0.8441(9) 0.6504(5) 0.5799(4) 0.0766(16) Uani 0.50 1 d P A 2 H51 H 0.9146 0.7287 0.5616 0.100 Uiso 0.50 1 calc PR A 2 H52 H 0.7105 0.6643 0.5503 0.100 Uiso 0.50 1 calc PR A 2 H53 H 0.8882 0.5742 0.5365 0.100 Uiso 0.50 1 calc PR A 2 loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 O1 0.0086(6) 0.0247(8) 0.0382(9) 0.000 0.0022(6) 0.000 Si1 0.0094(2) 0.0093(2) 0.0250(2) 0.000 0.00191(14) 0.000 O2 0.0158(4) 0.0121(4) 0.0429(5) -0.0035(3) 0.0074(3) 0.0013(3) C1 0.0481(11) 0.0195(8) 0.0257(8) 0.000 0.0015(7) 0.000 C2 0.0601(16) 0.0451(13) 0.0412(12) 0.000 -0.0132(11) 0.000 C3 0.0316(16) 0.033(3) 0.039(3) -0.011(2) 0.0117(15) -0.0030(17) C4 0.126(7) 0.038(4) 0.031(3) 0.003(3) 0.019(4) -0.036(4) C5 0.133(5) 0.058(3) 0.0436(19) 0.0101(18) 0.027(2) -0.019(3) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag O1 Si1 1.6050(4) . ? Si1 O2 1.6340(8) . ? Si1 C1 1.8553(19) . ? O2 H1 0.84 . ? O2 H2 0.84 . ? C1 C3 1.510(9) . ? C1 C2 1.577(3) . ? C1 C4 1.580(11) . ? C2 H21 0.98 . ? C2 H22 0.98 . ? C3 H31 0.98 . ? C3 H32 0.98 . ? C3 H33 0.98 . ? C4 C5 1.549(11) . ? C4 H41 0.99 . ? C4 H42 0.99 . ? C5 H51 0.98 . ? C5 H52 0.98 . ? C5 H53 0.98 . ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag Si1 O1 Si1 180.0 5_767 . ? O1 Si1 O2 108.79(3) . . ? O2 Si1 O2 105.99(6) 2_565 . ? O1 Si1 C1 110.03(7) . . ? O2 Si1 C1 111.56(5) . . ? Si1 O2 H1 121(2) . . ? Si1 O2 H2 125(2) . . ? H1 O2 H2 113(3) . . ? C3 C1 C3 114.5(6) . 2_565 ? C3 C1 C2 107.8(3) . . ? C3 C1 C4 111.1(3) . . ? C2 C1 C4 114.2(4) . . ? C4 C1 C4 107.2(8) 2_565 . ? C3 C1 Si1 109.8(4) . . ? C2 C1 Si1 106.81(16) . . ? C4 C1 Si1 107.0(4) . . ? C1 C2 H21 109.5 . . ? C1 C2 H22 109.5 . . ? H21 C2 H22 109.5 . . ? H22 C2 H22 109.5 . 2_565 ? C1 C3 H31 109.5 . . ? C1 C3 H32 109.5 . . ? H31 C3 H32 109.5 . . ? C1 C3 H33 109.5 . . ? H31 C3 H33 109.5 . . ? H32 C3 H33 109.5 . . ? C5 C4 C1 112.8(7) . . ? C5 C4 H41 109.0 . . ? C1 C4 H41 109.0 . . ? C5 C4 H42 109.0 . . ? C1 C4 H42 109.0 . . ? H41 C4 H42 107.8 . . ? C4 C5 H51 109.5 . . ? C4 C5 H52 109.5 . . ? H51 C5 H52 109.5 . . ? C4 C5 H53 109.5 . . ? H51 C5 H53 109.5 . . ? H52 C5 H53 109.5 . . ? loop_ _geom_torsion_atom_site_label_1 _geom_torsion_atom_site_label_2 _geom_torsion_atom_site_label_3 _geom_torsion_atom_site_label_4 _geom_torsion _geom_torsion_site_symmetry_1 _geom_torsion_site_symmetry_2 _geom_torsion_site_symmetry_3 _geom_torsion_site_symmetry_4 _geom_torsion_publ_flag O1 Si1 C1 C3 63.3(2) . . . . ? O2 Si1 C1 C3 -57.5(3) 2_565 . . . ? O2 Si1 C1 C3 -175.8(2) . . . . ? O1 Si1 C1 C3 -63.3(2) . . . 2_565 ? O2 Si1 C1 C3 175.8(2) 2_565 . . 2_565 ? O2 Si1 C1 C3 57.5(3) . . . 2_565 ? O1 Si1 C1 C2 180.0 . . . . ? O2 Si1 C1 C2 59.16(4) 2_565 . . . ? O2 Si1 C1 C2 -59.16(4) . . . . ? O1 Si1 C1 C4 57.3(4) . . . 2_565 ? O2 Si1 C1 C4 -63.5(4) 2_565 . . 2_565 ? O2 Si1 C1 C4 178.1(4) . . . 2_565 ? O1 Si1 C1 C4 -57.3(4) . . . . ? O2 Si1 C1 C4 -178.1(4) 2_565 . . . ? O2 Si1 C1 C4 63.5(4) . . . . ? C3 C1 C4 C5 69.3(8) . . . . ? C3 C1 C4 C5 -54(6) 2_565 . . . ? C2 C1 C4 C5 -52.9(7) . . . . ? C4 C1 C4 C5 74.6(9) 2_565 . . . ? Si1 C1 C4 C5 -170.9(5) . . . . ? loop_ _geom_hbond_atom_site_label_D _geom_hbond_atom_site_label_H _geom_hbond_atom_site_label_A _geom_hbond_distance_DH _geom_hbond_distance_HA _geom_hbond_distance_DA _geom_hbond_angle_DHA _geom_hbond_site_symmetry_A O2 H1 O2 0.84 1.820(3) 2.6585(15) 176(3) 6_657 O2 H2 O2 0.84 1.824(2) 2.6626(16) 177(3) 7_667 _diffrn_measured_fraction_theta_max 0.981 _diffrn_reflns_theta_full 30.00 _diffrn_measured_fraction_theta_full 0.981 _refine_diff_density_max 0.627 _refine_diff_density_min -0.280 _refine_diff_density_rms 0.064 _iucr_refine_instructions_details ; TITL NH156_0m in C2/m N.Hurkes [C2H5-C(CH3)2-Si-]2-O farblos 100K CELL 0.71073 7.2163 10.1628 10.6832 90.000 98.452 90.000 ZERR 2.00 0.0004 0.0005 0.0005 0.000 0.001 0.000 LATT 7 SYMM X,-Y, Z EQIV $1 1-X,Y,2-Z EQIV $2 1.5-X,1.5-Y,2-Z SFAC C H O SI UNIT 20 52 10 4 TEMP -173.150 SIZE 0.18 0.38 0.40 ACTA MERG 2 OMIT -2 60.009 OMIT -2 6 4 OMIT 3 1 0 OMIT 5 1 2 OMIT 2 0 3 OMIT 6 0 1 OMIT -3 1 3 OMIT -2 0 1 OMIT -2 4 1 OMIT -3 1 2 OMIT -2 0 3 OMIT 1 3 4 OMIT 2 4 2 L.S. 4 BOND $H CONF HTAB O2 O2_$1 HTAB O2 O2_$2 FMAP 2 PLAN 10 DFIX 0.84 0.0001 O2 H1 O2 H2 WGHT 0.056300 0.573700 FVAR 0.28497 0.02334 0.07748 O1 3 11.000000 10.500000 11.000000 10.25000 0.00859 0.02469 = 0.03823 0.00000 0.00216 0.00000 SI1 4 0.783703 0.500000 0.937463 10.50000 0.00943 0.00928 = 0.02499 0.00000 0.00191 0.00000 O2 3 0.680972 0.628398 0.988619 11.00000 0.01576 0.01212 = 0.04285 -0.00354 0.00740 0.00131 H1 2 0.565550 0.627383 0.992461 10.50000 21.00000 H2 2 0.727784 0.704063 0.998075 10.50000 21.00000 C1 1 0.764811 0.500000 0.762385 10.50000 0.04808 0.01950 = 0.02574 0.00000 0.00150 0.00000 C2 1 0.549280 0.500000 0.708696 10.50000 0.06015 0.04512 = 0.04122 0.00000 -0.01319 0.00000 AFIX 33 H21 2 0.532946 0.500000 0.615993 10.50000 31.00000 H22 2 0.490464 0.578735 0.738362 10.50000 31.00000 H23 2 0.490463 0.421265 0.738361 10.50000 31.00000 AFIX 0 PART 1 10.5 C3 1 0.848685 0.375076 0.718702 10.50000 0.03155 0.03332 = 0.03856 -0.01063 0.01173 -0.00300 AFIX 33 H31 2 0.848678 0.379020 0.627045 10.50000 -1.30000 H32 2 0.774212 0.299463 0.738969 10.50000 -1.30000 H33 2 0.977613 0.365648 0.761734 10.50000 -1.30000 AFIX 0 PART 2 10.5 C4 1 0.874108 0.625085 0.724534 10.50000 0.12646 0.03751 = 0.03100 0.00281 0.01941 -0.03641 AFIX 23 H41 2 0.831913 0.703238 0.767941 10.50000 -1.20000 H42 2 1.009605 0.613137 0.754186 10.50000 -1.20000 AFIX 0 C5 1 0.844072 0.650393 0.579938 10.50000 0.13262 0.05787 = 0.04359 0.01011 0.02747 -0.01893 AFIX 33 H51 2 0.914582 0.728736 0.561615 10.50000 -1.30000 H52 2 0.710451 0.664290 0.550254 10.50000 -1.30000 H53 2 0.888187 0.574161 0.536495 10.50000 -1.30000 HKLF 4 END ; #---------------------------------------------------------------------------- data_2d_i1044 _audit_author_name 'Clemens Bruhn' _audit_creation_method 'manual edited SHELXL-97 .cif file' _chemical_compound_source 'synthetical product' _chemical_name_systematic ; 1,3-bis(1,1-dimethylpentyl)-1,1,3,3-tetrahydroxydisiloxane ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C14 H34 O5 Si2' _chemical_formula_weight 338.59 loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source 'C' 'C' 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'H' 'H' 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'O' 'O' 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'Si' 'Si' 0.0817 0.0704 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting orthorhombic _symmetry_space_group_name_H-M 'C 2 2 21' _symmetry_Int_Tables_number 20 loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, -y, z+1/2' 'x, -y, -z' '-x, y, -z+1/2' 'x+1/2, y+1/2, z' '-x+1/2, -y+1/2, z+1/2' 'x+1/2, -y+1/2, -z' '-x+1/2, y+1/2, -z+1/2' _cell_length_a 7.2991(8) _cell_length_b 10.1695(11) _cell_length_c 27.408(4) _cell_angle_alpha 90.00 _cell_angle_beta 90.00 _cell_angle_gamma 90.00 _cell_volume 2034.4(4) _cell_formula_units_Z 4 _cell_measurement_temperature 100(2) _cell_measurement_reflns_used 8885 _cell_measurement_theta_min 1.49 _cell_measurement_theta_max 25.55 _exptl_crystal_description 'plate' _exptl_crystal_colour 'colorless' _exptl_crystal_size_max 0.58 _exptl_crystal_size_mid 0.31 _exptl_crystal_size_min 0.01 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.105 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 744 _exptl_absorpt_coefficient_mu 0.190 _exptl_absorpt_correction_type integration _exptl_absorpt_correction_T_min 0.9012 _exptl_absorpt_correction_T_max 0.9972 _exptl_absorpt_process_details 'X-red ver. 1.58 (Stoe & Cie. 2012)' _exptl_special_details ; ? ; _diffrn_ambient_temperature 100(2) _diffrn_measurement_device '2-circle goniometer' _diffrn_measurement_device_type 'STOE IPDS 2' _diffrn_detector 'image plate (34 cm diameter)' _diffrn_detector_type 'STOE' _diffrn_detector_area_resol_mean 6.67 _diffrn_source 'sealed X-ray tube, 12 x 0.4 mm long-fine focus' _diffrn_source_voltage 0 _diffrn_source_current 0.000 _diffrn_source_power 0.000 _diffrn_radiation_type 'Mo K\a' _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_monochromator 'plane graphite' _diffrn_radiation_polarisn_norm 0 _diffrn_radiation_collimation '0.5 mm diameter, multiple pinhole' _diffrn_measurement_method 'rotation method' _diffrn_measurement_details ; 180 frames, detector distance = 135 mm ; _diffrn_standards_decay_% 0 _diffrn_reflns_number 6611 _diffrn_reflns_av_R_equivalents 0.1641 _diffrn_reflns_av_sigmaI/netI 0.0699 _diffrn_reflns_limit_h_min -7 _diffrn_reflns_limit_h_max 8 _diffrn_reflns_limit_k_min -12 _diffrn_reflns_limit_k_max 12 _diffrn_reflns_limit_l_min -32 _diffrn_reflns_limit_l_max 32 _diffrn_reflns_theta_min 1.49 _diffrn_reflns_theta_max 24.99 _reflns_number_total 1051 _reflns_number_gt 982 _reflns_threshold_expression >2sigma(I) _computing_data_collection ? _computing_cell_refinement ? _computing_data_reduction ? _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics ? _computing_publication_material ? _refine_special_details ; Refinement of F^2^ against ALL reflections. The weighted R-factor wR and goodness of fit S are based on F^2^, conventional R-factors R are based on F, with F set to zero for negative F^2^. The threshold expression of F^2^ > 2sigma(F^2^) is used only for calculating R-factors(gt) etc. and is not relevant to the choice of reflections for refinement. R-factors based on F^2^ are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger. ; _refine_ls_structure_factor_coef Fsqd _refine_ls_matrix_type full _refine_ls_weighting_scheme calc _refine_ls_weighting_details 'calc w=1/[\s^2^(Fo^2^)+(0.0819P)^2^+5.5852P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment mixed _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_abs_structure_details 'Flack H D (1983), Acta Cryst. A39, 876-881' _refine_ls_abs_structure_Flack -0.2(5) _refine_ls_number_reflns 1051 _refine_ls_number_parameters 111 _refine_ls_number_restraints 5 _refine_ls_R_factor_all 0.0711 _refine_ls_R_factor_gt 0.0685 _refine_ls_wR_factor_ref 0.1752 _refine_ls_wR_factor_gt 0.1733 _refine_ls_goodness_of_fit_ref 1.089 _refine_ls_restrained_S_all 1.086 _refine_ls_shift/su_max 0.000 _refine_ls_shift/su_mean 0.000 loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_occupancy _atom_site_symmetry_multiplicity _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group Si1 Si 0.70457(19) 0.39553(13) 0.77304(5) 0.0290(4) Uani 1 1 d D . . O1 O 0.5000 0.4025(6) 0.7500 0.0368(12) Uani 1 2 d S . . O2 O 0.8176(6) 0.5275(3) 0.75625(15) 0.0342(9) Uani 1 1 d D . . H2F H 0.933(8) 0.521(13) 0.744(5) 0.051 Uiso 0.50 1 d PD . . H2G H 0.740(14) 0.596(8) 0.756(5) 0.051 Uiso 0.50 1 d PD . . O3 O 0.8148(6) 0.2703(3) 0.74887(15) 0.0351(9) Uani 1 1 d D . . H3F H 0.930(7) 0.257(8) 0.759(4) 0.053 Uiso 0.50 1 d PD . . H3G H 0.724(13) 0.277(14) 0.727(4) 0.053 Uiso 0.50 1 d PD . . C1 C 0.6934(8) 0.3808(5) 0.84135(19) 0.0334(11) Uani 1 1 d . . . C2 C 0.8943(8) 0.3803(6) 0.8605(2) 0.0379(13) Uani 1 1 d . . . H2A H 0.9643 0.3154 0.8411 0.045 Uiso 1 1 calc R . . H2B H 0.9480 0.4679 0.8537 0.045 Uiso 1 1 calc R . . C3 C 0.9247(9) 0.3495(6) 0.9143(2) 0.0457(15) Uani 1 1 d . . . H3A H 0.8846 0.2582 0.9209 0.055 Uiso 1 1 calc R . . H3B H 0.8481 0.4091 0.9343 0.055 Uiso 1 1 calc R . . C4 C 1.1251(10) 0.3647(8) 0.9296(2) 0.0540(17) Uani 1 1 d . . . H4A H 1.2024 0.3124 0.9071 0.065 Uiso 1 1 calc R . . H4B H 1.1608 0.4581 0.9260 0.065 Uiso 1 1 calc R . . C5 C 1.1638(13) 0.3215(8) 0.9814(3) 0.072(2) Uani 1 1 d . . . H5A H 1.0818 0.3682 1.0038 0.087 Uiso 1 1 calc R . . H5B H 1.2913 0.3418 0.9897 0.087 Uiso 1 1 calc R . . H5C H 1.1434 0.2266 0.9843 0.087 Uiso 1 1 calc R . . C6 C 0.5838(10) 0.4978(6) 0.8624(2) 0.0452(15) Uani 1 1 d . . . H6A H 0.6451 0.5804 0.8538 0.054 Uiso 1 1 calc R . . H6B H 0.5772 0.4899 0.8980 0.054 Uiso 1 1 calc R . . H6C H 0.4597 0.4975 0.8488 0.054 Uiso 1 1 calc R . . C7 C 0.5959(9) 0.2503(5) 0.8545(2) 0.0384(13) Uani 1 1 d . . . H7C H 0.5830 0.2438 0.8900 0.046 Uiso 1 1 calc R . . H7A H 0.6686 0.1761 0.8425 0.046 Uiso 1 1 calc R . . H7B H 0.4744 0.2486 0.8393 0.046 Uiso 1 1 calc R . . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 Si1 0.0177(7) 0.0202(6) 0.0492(8) 0.0000(6) -0.0010(6) -0.0015(6) O1 0.021(3) 0.032(3) 0.058(3) 0.000 -0.004(2) 0.000 O2 0.021(2) 0.0214(17) 0.060(2) 0.0026(16) 0.0021(19) -0.0001(17) O3 0.029(2) 0.0233(16) 0.053(2) -0.0036(17) -0.001(2) 0.0043(19) C1 0.026(3) 0.022(2) 0.052(3) 0.000(2) -0.001(2) -0.002(3) C2 0.031(3) 0.032(3) 0.050(3) -0.003(3) 0.002(2) -0.007(3) C3 0.039(3) 0.043(3) 0.055(4) 0.002(3) -0.001(3) -0.001(3) C4 0.046(4) 0.059(4) 0.057(4) 0.001(3) -0.006(3) -0.005(4) C5 0.062(6) 0.082(6) 0.073(5) 0.014(4) -0.023(4) -0.012(5) C6 0.040(3) 0.037(3) 0.058(4) -0.005(3) 0.005(3) 0.005(3) C7 0.024(3) 0.033(3) 0.058(3) 0.006(3) 0.003(3) -0.005(3) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag Si1 O1 1.6227(14) . ? Si1 O2 1.642(4) . ? Si1 O3 1.646(4) . ? Si1 C1 1.880(6) . ? Si1 H3G 1.75(13) . ? O1 Si1 1.6227(14) 4_656 ? O2 H2F 0.90(2) . ? O2 H2G 0.90(2) . ? O3 H3F 0.90(2) . ? O3 H3G 0.90(2) . ? C1 C6 1.546(8) . ? C1 C7 1.548(7) . ? C1 C2 1.557(8) . ? C2 C3 1.525(9) . ? C2 H2A 0.9900 . ? C2 H2B 0.9900 . ? C3 C4 1.529(9) . ? C3 H3A 0.9900 . ? C3 H3B 0.9900 . ? C4 C5 1.514(10) . ? C4 H4A 0.9900 . ? C4 H4B 0.9900 . ? C5 H5A 0.9800 . ? C5 H5B 0.9800 . ? C5 H5C 0.9800 . ? C6 H6A 0.9800 . ? C6 H6B 0.9800 . ? C6 H6C 0.9800 . ? C7 H7C 0.9800 . ? C7 H7A 0.9800 . ? C7 H7B 0.9800 . ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag O1 Si1 O2 108.5(2) . . ? O1 Si1 O3 109.1(2) . . ? O2 Si1 O3 105.9(2) . . ? O1 Si1 C1 110.56(19) . . ? O2 Si1 C1 111.5(2) . . ? O3 Si1 C1 111.1(2) . . ? O1 Si1 H3G 80(2) . . ? O2 Si1 H3G 109(5) . . ? O3 Si1 H3G 30.6(18) . . ? C1 Si1 H3G 132(4) . . ? Si1 O1 Si1 175.0(4) . 4_656 ? Si1 O2 H2F 121(8) . . ? Si1 O2 H2G 109(8) . . ? H2F O2 H2G 130(10) . . ? Si1 O3 H3F 116(2) . . ? Si1 O3 H3G 81(9) . . ? H3F O3 H3G 156(10) . . ? C6 C1 C7 109.6(5) . . ? C6 C1 C2 111.3(5) . . ? C7 C1 C2 110.6(5) . . ? C6 C1 Si1 109.4(4) . . ? C7 C1 Si1 108.7(4) . . ? C2 C1 Si1 107.1(4) . . ? C3 C2 C1 117.6(5) . . ? C3 C2 H2A 107.9 . . ? C1 C2 H2A 107.9 . . ? C3 C2 H2B 107.9 . . ? C1 C2 H2B 107.9 . . ? H2A C2 H2B 107.2 . . ? C2 C3 C4 112.5(5) . . ? C2 C3 H3A 109.1 . . ? C4 C3 H3A 109.1 . . ? C2 C3 H3B 109.1 . . ? C4 C3 H3B 109.1 . . ? H3A C3 H3B 107.8 . . ? C5 C4 C3 113.9(6) . . ? C5 C4 H4A 108.8 . . ? C3 C4 H4A 108.8 . . ? C5 C4 H4B 108.8 . . ? C3 C4 H4B 108.8 . . ? H4A C4 H4B 107.7 . . ? C4 C5 H5A 109.5 . . ? C4 C5 H5B 109.5 . . ? H5A C5 H5B 109.5 . . ? C4 C5 H5C 109.5 . . ? H5A C5 H5C 109.5 . . ? H5B C5 H5C 109.5 . . ? C1 C6 H6A 109.5 . . ? C1 C6 H6B 109.5 . . ? H6A C6 H6B 109.5 . . ? C1 C6 H6C 109.5 . . ? H6A C6 H6C 109.5 . . ? H6B C6 H6C 109.5 . . ? C1 C7 H7C 109.5 . . ? C1 C7 H7A 109.5 . . ? H7C C7 H7A 109.5 . . ? C1 C7 H7B 109.5 . . ? H7C C7 H7B 109.5 . . ? H7A C7 H7B 109.5 . . ? _diffrn_measured_fraction_theta_max 1.000 _diffrn_reflns_theta_full 24.99 _diffrn_measured_fraction_theta_full 1.000 _refine_diff_density_max 1.049 _refine_diff_density_min -0.319 _refine_diff_density_rms 0.080 _iucr_refine_instructions_details ; TITL NATASCHA HURKES 141, -173DEGC, AP CELL 0.71073 7.29910 10.16950 27.40800 90.00000 90.00000 90.00000 ZERR 4 0.00080 0.00110 0.00400 0.00000 0.00000 0.00000 LATT -7 SYMM -X, -Y, Z+ 0.50000 SYMM X, -Y, -Z SYMM -X, Y, -Z+ 0.50000 SFAC C H O SI UNIT 56 136 20 8 TEMP -173 L.S. 150 FMAP 2 MERG 3 SIZE 0.010 0.310 0.580 PLAN -20 OMIT -6 50 DFIX 0.9 O2 H2F O2 H2G O3 H3F O3 H3G DFIX 2.2 SI1 H3F ACTA BOND $H WGHT 0.081900 5.585200 FVAR 0.40847 SI1 4 0.704566 0.395533 0.773035 11.00000 0.01767 0.02016 = 0.04916 -0.00002 -0.00100 -0.00148 O1 3 0.500000 0.402517 0.750000 10.50000 0.02118 0.03166 = 0.05754 0.00000 -0.00411 0.00000 O2 3 0.817647 0.527544 0.756249 11.00000 0.02145 0.02140 = 0.05980 0.00264 0.00208 -0.00014 H2F 2 0.932510 0.521253 0.744402 10.50000 -1.50000 H2G 2 0.740265 0.596165 0.756469 10.50000 -1.50000 O3 3 0.814769 0.270260 0.748871 11.00000 0.02943 0.02327 = 0.05271 -0.00359 -0.00089 0.00435 H3F 2 0.930178 0.257434 0.759200 10.50000 -1.50000 H3G 2 0.723575 0.277240 0.726848 10.50000 -1.50000 C1 1 0.693436 0.380753 0.841349 11.00000 0.02631 0.02229 = 0.05171 0.00016 -0.00118 -0.00178 C2 1 0.894295 0.380319 0.860469 11.00000 0.03149 0.03230 = 0.04995 -0.00287 0.00199 -0.00744 AFIX 23 H2A 2 0.964339 0.315381 0.841072 11.00000 -1.20000 H2B 2 0.947966 0.467869 0.853749 11.00000 -1.20000 AFIX 0 C3 1 0.924671 0.349480 0.914323 11.00000 0.03866 0.04318 = 0.05522 0.00183 -0.00121 -0.00123 AFIX 23 H3A 2 0.884602 0.258202 0.920942 11.00000 -1.20000 H3B 2 0.848101 0.409128 0.934300 11.00000 -1.20000 AFIX 0 C4 1 1.125064 0.364651 0.929560 11.00000 0.04565 0.05923 = 0.05722 0.00118 -0.00642 -0.00540 AFIX 23 H4A 2 1.202430 0.312415 0.907098 11.00000 -1.20000 H4B 2 1.160771 0.458073 0.925990 11.00000 -1.20000 AFIX 0 C5 1 1.163802 0.321520 0.981400 11.00000 0.06214 0.08211 = 0.07306 0.01421 -0.02273 -0.01212 AFIX 137 H5A 2 1.081791 0.368208 1.003792 11.00000 -1.20000 H5B 2 1.291328 0.341827 0.989665 11.00000 -1.20000 H5C 2 1.143367 0.226599 0.984308 11.00000 -1.20000 AFIX 0 C6 1 0.583787 0.497830 0.862402 11.00000 0.04028 0.03737 = 0.05803 -0.00505 0.00534 0.00507 AFIX 137 H6A 2 0.645054 0.580370 0.853779 11.00000 -1.20000 H6B 2 0.577160 0.489866 0.897992 11.00000 -1.20000 H6C 2 0.459655 0.497455 0.848776 11.00000 -1.20000 AFIX 0 C7 1 0.595923 0.250332 0.854479 11.00000 0.02405 0.03288 = 0.05839 0.00599 0.00319 -0.00471 AFIX 137 H7C 2 0.583016 0.243787 0.889987 11.00000 -1.20000 H7A 2 0.668620 0.176064 0.842467 11.00000 -1.20000 H7B 2 0.474385 0.248561 0.839299 11.00000 -1.20000 HKLF 4 1 0.0000 1.0000 0.0000 -1.0000 0.0000 0.0000 0.0000 0.0000 1.0000 REM NATASCHA HURKES 141, -173DEGC, AP REM R1 = 0.0685 for 982 Fo > 4sig(Fo) and 0.0711 for all 1051 data REM 111 parameters refined using 5 restraints END ; #---------------------------------------------------------------------------- data_2g_NH231A _audit_author_name 'Ferdinand Belaj' _audit_creation_method 'manual edited SHELXL-97 .cif file' _chemical_compound_source 'synthetical product' _chemical_name_systematic ; 1,3-bis(1,1-dimethyloctyl)-1,1,3,3-tetrahydroxydisiloxane ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety 'C20 H46 O5 Si2' _chemical_formula_sum 'C20 H46 O5 Si2' _chemical_formula_weight 422.75 loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source 'C' 'C' 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'H' 'H' 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'O' 'O' 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'Si' 'Si' 0.0817 0.0704 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting monoclinic _symmetry_space_group_name_H-M 'C 2/c' _symmetry_space_group_name_Hall '-C 2yc' loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' 'x, -y, z+1/2' 'x+1/2, y+1/2, z' 'x+1/2, -y+1/2, z+1/2' '-x, -y, -z' '-x, y, -z-1/2' '-x+1/2, -y+1/2, -z' '-x+1/2, y+1/2, -z-1/2' _cell_length_a 7.2195(4) _cell_length_b 10.0508(5) _cell_length_c 35.0554(17) _cell_angle_alpha 90.00 _cell_angle_beta 92.856(2) _cell_angle_gamma 90.00 _cell_volume 2540.5(2) _cell_formula_units_Z 4 _cell_measurement_temperature 100(2) _cell_measurement_reflns_used 8860 _cell_measurement_theta_min 3.48 _cell_measurement_theta_max 31.18 _exptl_crystal_description 'needles' _exptl_crystal_colour 'colourless' _exptl_crystal_size_max 0.38 _exptl_crystal_size_mid 0.32 _exptl_crystal_size_min 0.20 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.105 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 936 _exptl_absorpt_coefficient_mu 0.164 _exptl_absorpt_correction_type 'multi-scan' _exptl_absorpt_correction_T_min 0.6163 _exptl_absorpt_correction_T_max 0.7462 _exptl_absorpt_process_details 'Bruker SADABS' _exptl_special_details ; ? ; _diffrn_ambient_temperature 100(2) _diffrn_measurement_device_type 'Bruker APEX-II CCD' _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_type 'MoK\a' _diffrn_radiation_monochromator 'graphite' _diffrn_radiation_wavelength 0.71073 _diffrn_measurement_method '\f and \w scans' _diffrn_detector_area_resol_mean ? _diffrn_standards_number 0 _diffrn_standards_interval_count ? _diffrn_standards_decay_% ? _diffrn_reflns_number 7769 _diffrn_reflns_av_R_equivalents 0.0232 _diffrn_reflns_av_sigmaI/netI 0.0281 _diffrn_reflns_limit_h_min -8 _diffrn_reflns_limit_h_max 8 _diffrn_reflns_limit_k_min -12 _diffrn_reflns_limit_k_max 12 _diffrn_reflns_limit_l_min -43 _diffrn_reflns_limit_l_max 43 _diffrn_reflns_theta_min 2.33 _diffrn_reflns_theta_max 26.00 _reflns_number_total 2471 _reflns_number_gt 2417 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'Bruker APEX2' _computing_cell_refinement 'Bruker SAINT' _computing_data_reduction 'Bruker SAINT' _computing_structure_solution 'SHELXS-97 (Sheldrick, 2008)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 2008)' _computing_molecular_graphics 'modified ORTEP (Johnson, 1965)' _computing_publication_material 'SHELXL-97 (Sheldrick, 2008)' _refine_special_details ; Refinement of F^2^ against ALL reflections. The weighted R-factor wR and goodness of fit S are based on F^2^, conventional R-factors R are based on F, with F set to zero for negative F^2^. The threshold expression of F^2^ > 2sigma(F^2^) is used only for calculating R-factors(gt) etc. and is not relevant to the choice of reflections for refinement. R-factors based on F^2^ are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger. The non-hydrogen atoms were refined with anisotropic displacement parameters without any constraints. Since twinning was detected a twin matrix (-1 0 0 / 0 1 0 / 1 0 -1) was applied and a scale factor was refined [0.0123(9)] between the two unequal components (TWIN, BASF instruction of SHELXL-97). The H atoms of the OH groups are disordered over two sites. They were refined with site occupation factors of 0.5 and with common isotropic displacement parameters for the H atoms bonded to the same O atom. Only the bond lengths were fixed to be 0.88 \%A (DFIX of SHELXL-97), no angular or conformational constraints were applied. The H atoms of the CH~2~ groups were included at calculated positions with their isotropic displacement parameters fixed to 1.2 times U~eq~ of the C atom they are bonded to. The H atoms of the methyl groups were refined with common isotropic displacement parameters for the H atoms of the same group and idealized geometries with tetrahedral angles, enabling rotation around the C-C bond, and C-H distances of 0.98 \%A (AFIX 137 of SHELXL-97). ; _refine_ls_structure_factor_coef Fsqd _refine_ls_matrix_type full _refine_ls_weighting_scheme calc _refine_ls_weighting_details 'calc w=1/[\s^2^(Fo^2^)+(0.0187P)^2^+18.3663P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment refU _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 2471 _refine_ls_number_parameters 144 _refine_ls_number_restraints 4 _refine_ls_R_factor_all 0.0755 _refine_ls_R_factor_gt 0.0745 _refine_ls_wR_factor_ref 0.1649 _refine_ls_wR_factor_gt 0.1643 _refine_ls_goodness_of_fit_ref 1.169 _refine_ls_restrained_S_all 1.168 _refine_ls_shift/su_max 0.001 _refine_ls_shift/su_mean 0.000 loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_occupancy _atom_site_symmetry_multiplicity _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group Si1 Si 0.80222(11) 0.48508(7) 0.76917(2) 0.0113(2) Uani 1 1 d . . . O1 O 1.0000 0.4764(3) 0.7500 0.0176(7) Uani 1 2 d S . . O2 O 0.6818(3) 0.35256(19) 0.75777(7) 0.0179(5) Uani 1 1 d D . . H21 H 0.5600(8) 0.350(7) 0.755(2) 0.021(14) Uiso 0.50 1 d PD . . H22 H 0.725(10) 0.272(3) 0.755(2) 0.021(14) Uiso 0.50 1 d PD . . O3 O 0.6845(3) 0.60970(19) 0.75024(7) 0.0182(5) Uani 1 1 d D . . H31 H 0.731(9) 0.687(3) 0.744(2) 0.021(14) Uiso 0.50 1 d PD . . H32 H 0.5629(11) 0.608(7) 0.751(2) 0.021(14) Uiso 0.50 1 d PD . . C11 C 0.8381(5) 0.5027(4) 0.82184(10) 0.0227(7) Uani 1 1 d . . . C12 C 0.6447(5) 0.5089(4) 0.83911(10) 0.0260(8) Uani 1 1 d . . . H121 H 0.5696 0.5767 0.8249 0.031 Uiso 1 1 calc R . . H122 H 0.5828 0.4220 0.8348 0.031 Uiso 1 1 calc R . . C13 C 0.6429(5) 0.5416(4) 0.88187(10) 0.0308(9) Uani 1 1 d . . . H131 H 0.7229 0.4770 0.8963 0.037 Uiso 1 1 calc R . . H132 H 0.6964 0.6313 0.8863 0.037 Uiso 1 1 calc R . . C14 C 0.4489(5) 0.5378(4) 0.89735(11) 0.0323(9) Uani 1 1 d . . . H141 H 0.3940 0.4488 0.8925 0.039 Uiso 1 1 calc R . . H142 H 0.3696 0.6041 0.8835 0.039 Uiso 1 1 calc R . . C15 C 0.4510(6) 0.5670(5) 0.94017(12) 0.0428(11) Uani 1 1 d . . . H151 H 0.5101 0.6548 0.9449 0.051 Uiso 1 1 calc R . . H152 H 0.5291 0.4994 0.9538 0.051 Uiso 1 1 calc R . . C16 C 0.2594(6) 0.5680(5) 0.95734(12) 0.0444(11) Uani 1 1 d . . . H161 H 0.1911 0.4871 0.9487 0.053 Uiso 1 1 calc R . . H162 H 0.2766 0.5634 0.9855 0.053 Uiso 1 1 calc R . . C17 C 0.1429(6) 0.6883(6) 0.94687(13) 0.0455(12) Uani 1 1 d . . . H171 H 0.1178 0.6900 0.9189 0.055 Uiso 1 1 calc R . . H172 H 0.2132 0.7697 0.9541 0.055 Uiso 1 1 calc R . . C18 C -0.0424(6) 0.6886(6) 0.96671(14) 0.0525(13) Uani 1 1 d . . . H181 H -0.1162 0.7657 0.9581 0.077(11) Uiso 1 1 calc R . . H182 H -0.0183 0.6936 0.9944 0.077(11) Uiso 1 1 calc R . . H183 H -0.1107 0.6067 0.9603 0.077(11) Uiso 1 1 calc R . . C19 C 0.9529(6) 0.3875(4) 0.83853(11) 0.0334(9) Uani 1 1 d . . . H191 H 1.0745 0.3866 0.8273 0.037(7) Uiso 1 1 calc R . . H192 H 0.8887 0.3034 0.8328 0.037(7) Uiso 1 1 calc R . . H193 H 0.9693 0.3983 0.8663 0.037(7) Uiso 1 1 calc R . . C20 C 0.9442(5) 0.6353(4) 0.82942(10) 0.0292(8) Uani 1 1 d . . . H201 H 0.8677 0.7099 0.8199 0.032(6) Uiso 1 1 calc R . . H202 H 1.0607 0.6338 0.8162 0.032(6) Uiso 1 1 calc R . . H203 H 0.9711 0.6458 0.8569 0.032(6) Uiso 1 1 calc R . . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 Si1 0.0053(4) 0.0041(4) 0.0245(4) -0.0002(3) 0.0012(3) 0.0004(3) O1 0.0067(14) 0.0174(15) 0.0291(17) 0.000 0.0034(12) 0.000 O2 0.0077(11) 0.0072(10) 0.0390(14) -0.0046(9) 0.0021(9) -0.0028(8) O3 0.0079(11) 0.0129(11) 0.0337(13) 0.0023(9) 0.0011(9) 0.0008(8) C11 0.0140(16) 0.0274(18) 0.0266(17) 0.0005(14) -0.0002(12) -0.0024(14) C12 0.0170(17) 0.033(2) 0.0280(18) -0.0003(15) 0.0033(13) -0.0014(15) C13 0.0197(19) 0.044(2) 0.0293(19) -0.0028(17) 0.0039(14) -0.0005(16) C14 0.022(2) 0.044(2) 0.031(2) 0.0018(17) 0.0066(15) 0.0000(17) C15 0.027(2) 0.071(3) 0.031(2) -0.001(2) 0.0079(17) 0.005(2) C16 0.031(2) 0.072(3) 0.030(2) 0.001(2) 0.0090(17) 0.002(2) C17 0.026(2) 0.075(3) 0.035(2) -0.005(2) 0.0050(17) 0.000(2) C18 0.025(2) 0.080(4) 0.053(3) -0.014(3) 0.008(2) -0.001(2) C19 0.024(2) 0.048(2) 0.0284(19) 0.0090(17) -0.0008(15) 0.0113(18) C20 0.0193(18) 0.046(2) 0.0222(17) -0.0089(16) -0.0013(13) -0.0099(16) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag Si1 O1 1.6104(8) . ? Si1 O2 1.630(2) . ? Si1 O3 1.636(2) . ? Si1 C11 1.860(3) . ? O2 H21 0.88 . ? O2 H22 0.88 . ? O3 H31 0.88 . ? O3 H32 0.88 . ? C11 C19 1.524(5) . ? C11 C12 1.551(5) . ? C11 C20 1.553(5) . ? C12 C13 1.535(5) . ? C12 H121 0.99 . ? C12 H122 0.99 . ? C13 C14 1.528(5) . ? C13 H131 0.99 . ? C13 H132 0.99 . ? C14 C15 1.529(5) . ? C14 H141 0.99 . ? C14 H142 0.99 . ? C15 C16 1.536(6) . ? C15 H151 0.99 . ? C15 H152 0.99 . ? C16 C17 1.508(7) . ? C16 H161 0.99 . ? C16 H162 0.99 . ? C17 C18 1.538(6) . ? C17 H171 0.99 . ? C17 H172 0.99 . ? C18 H181 0.98 . ? C18 H182 0.98 . ? C18 H183 0.98 . ? C19 H191 0.98 . ? C19 H192 0.98 . ? C19 H193 0.98 . ? C20 H201 0.98 . ? C20 H202 0.98 . ? C20 H203 0.98 . ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag O1 Si1 O2 109.07(13) . . ? O1 Si1 O3 109.03(12) . . ? O2 Si1 O3 105.44(11) . . ? O1 Si1 C11 109.67(11) . . ? O2 Si1 C11 111.56(15) . . ? O3 Si1 C11 111.94(15) . . ? Si1 O1 Si1 173.8(2) . 6_757 ? Si1 O2 H21 125(5) . . ? Si1 O2 H22 127(5) . . ? H21 O2 H22 109(7) . . ? Si1 O3 H31 126(5) . . ? Si1 O3 H32 118(5) . . ? H31 O3 H32 115(7) . . ? C19 C11 C12 111.3(3) . . ? C19 C11 C20 109.4(3) . . ? C12 C11 C20 110.2(3) . . ? C19 C11 Si1 110.8(3) . . ? C12 C11 Si1 107.9(2) . . ? C20 C11 Si1 107.1(2) . . ? C13 C12 C11 116.2(3) . . ? C13 C12 H121 108.2 . . ? C11 C12 H121 108.2 . . ? C13 C12 H122 108.2 . . ? C11 C12 H122 108.2 . . ? H121 C12 H122 107.4 . . ? C14 C13 C12 113.2(3) . . ? C14 C13 H131 108.9 . . ? C12 C13 H131 108.9 . . ? C14 C13 H132 108.9 . . ? C12 C13 H132 108.9 . . ? H131 C13 H132 107.8 . . ? C13 C14 C15 112.3(3) . . ? C13 C14 H141 109.1 . . ? C15 C14 H141 109.1 . . ? C13 C14 H142 109.1 . . ? C15 C14 H142 109.1 . . ? H141 C14 H142 107.9 . . ? C14 C15 C16 114.9(4) . . ? C14 C15 H151 108.5 . . ? C16 C15 H151 108.5 . . ? C14 C15 H152 108.5 . . ? C16 C15 H152 108.5 . . ? H151 C15 H152 107.5 . . ? C17 C16 C15 114.3(4) . . ? C17 C16 H161 108.7 . . ? C15 C16 H161 108.7 . . ? C17 C16 H162 108.7 . . ? C15 C16 H162 108.7 . . ? H161 C16 H162 107.6 . . ? C16 C17 C18 112.3(4) . . ? C16 C17 H171 109.2 . . ? C18 C17 H171 109.2 . . ? C16 C17 H172 109.2 . . ? C18 C17 H172 109.2 . . ? H171 C17 H172 107.9 . . ? C17 C18 H181 109.5 . . ? C17 C18 H182 109.5 . . ? H181 C18 H182 109.5 . . ? C17 C18 H183 109.5 . . ? H181 C18 H183 109.5 . . ? H182 C18 H183 109.5 . . ? C11 C19 H191 109.5 . . ? C11 C19 H192 109.5 . . ? H191 C19 H192 109.5 . . ? C11 C19 H193 109.5 . . ? H191 C19 H193 109.5 . . ? H192 C19 H193 109.5 . . ? C11 C20 H201 109.5 . . ? C11 C20 H202 109.5 . . ? H201 C20 H202 109.5 . . ? C11 C20 H203 109.5 . . ? H201 C20 H203 109.5 . . ? H202 C20 H203 109.5 . . ? loop_ _geom_torsion_atom_site_label_1 _geom_torsion_atom_site_label_2 _geom_torsion_atom_site_label_3 _geom_torsion_atom_site_label_4 _geom_torsion _geom_torsion_site_symmetry_1 _geom_torsion_site_symmetry_2 _geom_torsion_site_symmetry_3 _geom_torsion_site_symmetry_4 _geom_torsion_publ_flag O1 Si1 C11 C19 -57.2(3) . . . . ? O2 Si1 C11 C19 63.8(3) . . . . ? O3 Si1 C11 C19 -178.3(2) . . . . ? O1 Si1 C11 C12 -179.3(2) . . . . ? O2 Si1 C11 C12 -58.3(3) . . . . ? O3 Si1 C11 C12 59.5(3) . . . . ? O1 Si1 C11 C20 62.1(3) . . . . ? O2 Si1 C11 C20 -176.9(2) . . . . ? O3 Si1 C11 C20 -59.1(3) . . . . ? C19 C11 C12 C13 65.8(4) . . . . ? C20 C11 C12 C13 -55.7(4) . . . . ? Si1 C11 C12 C13 -172.4(3) . . . . ? C11 C12 C13 C14 -176.6(3) . . . . ? C12 C13 C14 C15 178.5(4) . . . . ? C13 C14 C15 C16 178.6(4) . . . . ? C14 C15 C16 C17 -73.4(6) . . . . ? C15 C16 C17 C18 -176.5(4) . . . . ? loop_ _geom_hbond_atom_site_label_D _geom_hbond_atom_site_label_H _geom_hbond_atom_site_label_A _geom_hbond_distance_DH _geom_hbond_distance_HA _geom_hbond_distance_DA _geom_hbond_angle_DHA _geom_hbond_site_symmetry_A O2 H21 O2 0.88 1.780(12) 2.654(4) 172(8) 6_657 O2 H22 O3 0.88 1.765(3) 2.645(3) 179(8) 8_647 O3 H31 O2 0.88 1.781(17) 2.645(3) 167(7) 8_657 O3 H32 O3 0.88 1.784(7) 2.663(4) 176(8) 6_657 _diffrn_measured_fraction_theta_max 0.986 _diffrn_reflns_theta_full 26.00 _diffrn_measured_fraction_theta_full 0.986 _refine_diff_density_max 0.654 _refine_diff_density_min -0.736 _refine_diff_density_rms 0.086 _iucr_refine_instructions_details ; TITL NH231A_0m in C 2/c N.Hurkes [C7H16-C(Me)2Si(OH)2]O farblos 100K CELL 0.71073 7.2195 10.0508 35.0554 90.000 92.856 90.000 ZERR 4.00 0.0004 0.0005 0.0017 0.000 0.002 0.000 LATT 7 SYMM X, -Y, 0.5+Z EQIV $1 1-X, Y, 1.5-Z EQIV $2 1.5-X, Y-0.5, 1.5-Z EQIV $3 1.5-X, Y+0.5, 1.5-Z SFAC C H O SI UNIT 80 184 20 8 TEMP -173.170 SIZE 0.20 0.32 0.38 ACTA MERG 2 OMIT -2 52.002 OMIT -1 3 3 OMIT -6 8 4 OMIT 1 9 10 OMIT -5 3 3 OMIT -3 9 14 L.S. 3 BOND $H CONF FMAP 2 PLAN 20 HTAB O2 O2_$1 HTAB O2 O3_$2 HTAB O3 O2_$3 HTAB O3 O3_$1 TWIN -1 0 0 0 1 0 1 0 -1 DFIX 0.88 0.0001 O2 H21 O2 H22 O3 H31 O3 H32 WGHT 0.0187 18.3663 BASF 0.01225 FVAR 0.11636 0.02061 0.02053 0.07677 0.03684 0.03177 SI1 4 0.802222 0.485084 0.769167 11.00000 0.00530 0.00411 = 0.02449 -0.00021 0.00124 0.00044 O1 3 1.000000 0.476379 0.750000 10.50000 0.00671 0.01739 = 0.02907 0.00000 0.00342 0.00000 O2 3 0.681762 0.352565 0.757770 11.00000 0.00768 0.00722 = 0.03903 -0.00457 0.00213 -0.00276 H21 2 0.560018 0.349883 0.754939 10.50000 21.00000 H22 2 0.725336 0.271684 0.754740 10.50000 21.00000 O3 3 0.684459 0.609700 0.750243 11.00000 0.00793 0.01295 = 0.03370 0.00230 0.00109 0.00083 H31 2 0.731134 0.686970 0.743852 10.50000 31.00000 H32 2 0.562920 0.608111 0.751229 10.50000 31.00000 C11 1 0.838142 0.502719 0.821837 11.00000 0.01400 0.02738 = 0.02655 0.00051 -0.00016 -0.00235 C12 1 0.644738 0.508920 0.839112 11.00000 0.01704 0.03305 = 0.02800 -0.00034 0.00329 -0.00137 AFIX 23 H121 2 0.569558 0.576720 0.824904 11.00000 -1.20000 H122 2 0.582836 0.421951 0.834777 11.00000 -1.20000 AFIX 0 C13 1 0.642937 0.541578 0.881871 11.00000 0.01966 0.04377 = 0.02933 -0.00277 0.00389 -0.00050 AFIX 23 H131 2 0.722942 0.477035 0.896267 11.00000 -1.20000 H132 2 0.696351 0.631322 0.886264 11.00000 -1.20000 AFIX 0 C14 1 0.448929 0.537771 0.897347 11.00000 0.02245 0.04375 = 0.03123 0.00184 0.00661 0.00000 AFIX 23 H141 2 0.393953 0.448783 0.892455 11.00000 -1.20000 H142 2 0.369575 0.604143 0.883533 11.00000 -1.20000 AFIX 0 C15 1 0.450990 0.566996 0.940166 11.00000 0.02703 0.07101 = 0.03114 -0.00143 0.00786 0.00507 AFIX 23 H151 2 0.510070 0.654750 0.944877 11.00000 -1.20000 H152 2 0.529069 0.499358 0.953756 11.00000 -1.20000 AFIX 0 C16 1 0.259423 0.567952 0.957339 11.00000 0.03102 0.07248 = 0.03043 0.00077 0.00900 0.00178 AFIX 23 H161 2 0.191054 0.487125 0.948716 11.00000 -1.20000 H162 2 0.276590 0.563420 0.985504 11.00000 -1.20000 AFIX 0 C17 1 0.142929 0.688270 0.946870 11.00000 0.02648 0.07492 = 0.03548 -0.00523 0.00500 -0.00043 AFIX 23 H171 2 0.117794 0.690012 0.918852 11.00000 -1.20000 H172 2 0.213238 0.769737 0.954135 11.00000 -1.20000 AFIX 0 C18 1 -0.042364 0.688612 0.966715 11.00000 0.02506 0.07996 = 0.05302 -0.01449 0.00797 -0.00139 AFIX 137 H181 2 -0.116180 0.765698 0.958051 11.00000 41.00000 H182 2 -0.018289 0.693648 0.994437 11.00000 41.00000 H183 2 -0.110671 0.606706 0.960299 11.00000 41.00000 AFIX 0 C19 1 0.952916 0.387487 0.838533 11.00000 0.02360 0.04812 = 0.02839 0.00896 -0.00083 0.01128 AFIX 137 H191 2 1.074528 0.386620 0.827302 11.00000 51.00000 H192 2 0.888706 0.303424 0.832757 11.00000 51.00000 H193 2 0.969324 0.398313 0.866279 11.00000 51.00000 AFIX 0 C20 1 0.944186 0.635278 0.829420 11.00000 0.01929 0.04569 = 0.02225 -0.00891 -0.00131 -0.00991 AFIX 137 H201 2 0.867683 0.709872 0.819889 11.00000 61.00000 H202 2 1.060693 0.633768 0.816227 11.00000 61.00000 H203 2 0.971102 0.645846 0.856930 11.00000 61.00000 HKLF 4 END ; #---------------------------------------------------------------------------- data_4a_i1154 _audit_author_name 'Clemens Bruhn' _audit_creation_method 'manual edited SHELXL-97 .cif file' _chemical_compound_source 'synthetical product' _chemical_name_systematic ; octakis(tert-butyl)octasilsesquioxane ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C32 H72 O12 Si8' _chemical_formula_weight 873.62 loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source 'C' 'C' 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'H' 'H' 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'O' 'O' 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'Si' 'Si' 0.0817 0.0704 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting triclinic _symmetry_space_group_name_H-M 'P -1' _symmetry_Int_Tables_number 2 loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, -y, -z' _cell_length_a 10.7426(14) _cell_length_b 11.0102(13) _cell_length_c 11.8640(14) _cell_angle_alpha 111.291(9) _cell_angle_beta 72.229(9) _cell_angle_gamma 94.686(10) _cell_volume 1244.4(3) _cell_formula_units_Z 1 _cell_measurement_temperature 100(2) _cell_measurement_reflns_used 9973 _cell_measurement_theta_min 1.93 _cell_measurement_theta_max 25.29 _exptl_crystal_description 'plate' _exptl_crystal_colour 'colorless' _exptl_crystal_size_max 0.52 _exptl_crystal_size_mid 0.33 _exptl_crystal_size_min 0.07 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.166 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 472 _exptl_absorpt_coefficient_mu 0.264 _exptl_absorpt_correction_type integration _exptl_absorpt_correction_T_min 0.8894 _exptl_absorpt_correction_T_max 0.9812 _exptl_absorpt_process_details 'X-red ver. 1.31 (Stoe & Cie. 2005)' _exptl_special_details ; ? ; _diffrn_ambient_temperature 100(2) _diffrn_measurement_device '2-circle goniometer' _diffrn_measurement_device_type 'STOE IPDS 2' _diffrn_detector 'image plate (34 cm diameter)' _diffrn_detector_type 'STOE' _diffrn_detector_area_resol_mean 6.67 _diffrn_source 'sealed X-ray tube, 12 x 0.4 mm long-fine focus' _diffrn_source_voltage 50 _diffrn_source_current 30 _diffrn_source_power 1.50 _diffrn_radiation_type 'Mo K\a' _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_monochromator 'plane graphite' _diffrn_radiation_polarisn_norm 0 _diffrn_radiation_collimation '0.5 mm diameter, multiple pinhole' _diffrn_measurement_method 'rotation method' _diffrn_measurement_details ; 190 frames, detector distance = 138 mm ; _diffrn_standards_decay_% 0 _diffrn_reflns_number 8177 _diffrn_reflns_av_R_equivalents 0.0537 _diffrn_reflns_av_sigmaI/netI 0.0450 _diffrn_reflns_limit_h_min -12 _diffrn_reflns_limit_h_max 12 _diffrn_reflns_limit_k_min -13 _diffrn_reflns_limit_k_max 11 _diffrn_reflns_limit_l_min -13 _diffrn_reflns_limit_l_max 13 _diffrn_reflns_theta_min 1.93 _diffrn_reflns_theta_max 24.84 _reflns_number_total 4199 _reflns_number_gt 3352 _reflns_threshold_expression >2sigma(I) _computing_data_collection ? _computing_cell_refinement ? _computing_data_reduction ? _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics ? _computing_publication_material ? _refine_special_details ; Refinement of F^2^ against ALL reflections. The weighted R-factor wR and goodness of fit S are based on F^2^, conventional R-factors R are based on F, with F set to zero for negative F^2^. The threshold expression of F^2^ > 2sigma(F^2^) is used only for calculating R-factors(gt) etc. and is not relevant to the choice of reflections for refinement. R-factors based on F^2^ are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger. ; _refine_ls_structure_factor_coef Fsqd _refine_ls_matrix_type full _refine_ls_weighting_scheme calc _refine_ls_weighting_details 'calc w=1/[\s^2^(Fo^2^)+(0.0934P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment constr _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 4199 _refine_ls_number_parameters 247 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0534 _refine_ls_R_factor_gt 0.0454 _refine_ls_wR_factor_ref 0.1334 _refine_ls_wR_factor_gt 0.1293 _refine_ls_goodness_of_fit_ref 1.013 _refine_ls_restrained_S_all 1.013 _refine_ls_shift/su_max 0.000 _refine_ls_shift/su_mean 0.000 loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_occupancy _atom_site_symmetry_multiplicity _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group C1 C 0.1763(2) 0.2379(2) 0.3513(2) 0.0479(5) Uani 1 1 d . . . C2 C 0.0419(3) 0.1786(3) 0.3504(3) 0.0703(8) Uani 1 1 d . . . H2A H 0.0226 0.1756 0.2739 0.084 Uiso 1 1 calc R . . H2B H -0.0254 0.2324 0.4255 0.084 Uiso 1 1 calc R . . H2C H 0.0429 0.0900 0.3512 0.084 Uiso 1 1 calc R . . C3 C 0.1720(3) 0.3793(3) 0.3554(3) 0.0699(8) Uani 1 1 d . . . H3A H 0.1085 0.4319 0.4344 0.084 Uiso 1 1 calc R . . H3B H 0.1461 0.3796 0.2831 0.084 Uiso 1 1 calc R . . H3C H 0.2588 0.4161 0.3512 0.084 Uiso 1 1 calc R . . C4 C 0.2096(3) 0.2391(3) 0.4690(2) 0.0705(8) Uani 1 1 d . . . H4C H 0.2978 0.2717 0.4661 0.085 Uiso 1 1 calc R . . H4B H 0.2060 0.1504 0.4703 0.085 Uiso 1 1 calc R . . H4A H 0.1463 0.2961 0.5456 0.085 Uiso 1 1 calc R . . C5 C 0.6734(2) 0.3423(2) 0.2583(2) 0.0476(5) Uani 1 1 d . . . C6 C 0.6030(3) 0.4686(3) 0.2814(3) 0.0693(8) Uani 1 1 d . . . H6A H 0.6184 0.4813 0.2007 0.083 Uiso 1 1 calc R . . H6B H 0.6367 0.5425 0.3391 0.083 Uiso 1 1 calc R . . H6C H 0.5089 0.4628 0.3192 0.083 Uiso 1 1 calc R . . C7 C 0.8207(3) 0.3516(3) 0.1976(3) 0.0698(8) Uani 1 1 d . . . H7A H 0.8554 0.4241 0.2558 0.084 Uiso 1 1 calc R . . H7B H 0.8349 0.3666 0.1182 0.084 Uiso 1 1 calc R . . H7C H 0.8658 0.2700 0.1802 0.084 Uiso 1 1 calc R . . C8 C 0.6529(3) 0.3223(3) 0.3846(2) 0.0722(8) Uani 1 1 d . . . H8C H 0.7019 0.2437 0.3692 0.087 Uiso 1 1 calc R . . H8B H 0.5596 0.3123 0.4224 0.087 Uiso 1 1 calc R . . H8A H 0.6840 0.3980 0.4427 0.087 Uiso 1 1 calc R . . C9 C 0.7909(2) -0.1593(2) 0.1303(2) 0.0491(6) Uani 1 1 d . . . C10 C 0.7419(4) -0.1195(4) 0.2756(3) 0.0858(10) Uani 1 1 d . . . H10A H 0.7305 -0.0244 0.3147 0.103 Uiso 1 1 calc R . . H10B H 0.8060 -0.1491 0.3045 0.103 Uiso 1 1 calc R . . H10C H 0.6580 -0.1598 0.3000 0.103 Uiso 1 1 calc R . . C11 C 0.9261(3) -0.1036(3) 0.0924(3) 0.0654(7) Uani 1 1 d . . . H11A H 0.9874 -0.1393 0.1199 0.078 Uiso 1 1 calc R . . H11B H 0.9202 -0.0084 0.1329 0.078 Uiso 1 1 calc R . . H11C H 0.9571 -0.1276 0.0002 0.078 Uiso 1 1 calc R . . C12 C 0.8030(3) -0.3088(3) 0.0677(3) 0.0753(8) Uani 1 1 d . . . H12C H 0.8399 -0.3333 -0.0242 0.090 Uiso 1 1 calc R . . H12B H 0.7162 -0.3456 0.0872 0.090 Uiso 1 1 calc R . . H12A H 0.8604 -0.3429 0.1003 0.090 Uiso 1 1 calc R . . C13 C 0.2956(2) -0.2656(2) 0.2182(2) 0.0511(6) Uani 1 1 d . . . C14 C 0.3082(4) -0.2100(4) 0.3533(3) 0.0812(10) Uani 1 1 d . . . H14A H 0.4009 -0.2052 0.3491 0.097 Uiso 1 1 calc R . . H14B H 0.2646 -0.2669 0.3997 0.097 Uiso 1 1 calc R . . H14C H 0.2670 -0.1224 0.3970 0.097 Uiso 1 1 calc R . . C15 C 0.3659(3) -0.3996(3) 0.1473(3) 0.0766(9) Uani 1 1 d . . . H15A H 0.3262 -0.4589 0.1921 0.092 Uiso 1 1 calc R . . H15B H 0.4586 -0.3908 0.1431 0.092 Uiso 1 1 calc R . . H15C H 0.3579 -0.4348 0.0612 0.092 Uiso 1 1 calc R . . C16 C 0.1502(3) -0.2795(3) 0.2253(3) 0.0721(8) Uani 1 1 d . . . H16C H 0.1418 -0.3120 0.1394 0.087 Uiso 1 1 calc R . . H16B H 0.1047 -0.1944 0.2732 0.087 Uiso 1 1 calc R . . H16A H 0.1116 -0.3412 0.2677 0.087 Uiso 1 1 calc R . . O1 O 0.44811(15) 0.19981(16) 0.21000(14) 0.0462(4) Uani 1 1 d . . . O2 O 0.67088(16) 0.06497(15) 0.13396(14) 0.0464(4) Uani 1 1 d . . . O3 O 0.52935(15) -0.14516(16) 0.12078(14) 0.0472(4) Uani 1 1 d . . . O4 O 0.30558(16) -0.01048(15) 0.20041(14) 0.0474(4) Uani 1 1 d . . . O5 O 0.27652(16) 0.14136(16) 0.07931(13) 0.0466(4) Uani 1 1 d . . . O6 O 0.63908(16) 0.21563(16) 0.01293(13) 0.0469(4) Uani 1 1 d . . . Si1 Si 0.30536(6) 0.13950(6) 0.20581(5) 0.03925(18) Uani 1 1 d . . . Si2 Si 0.60603(6) 0.20159(6) 0.15106(5) 0.03839(18) Uani 1 1 d . . . Si3 Si 0.67517(6) -0.09369(6) 0.07490(5) 0.03865(18) Uani 1 1 d . . . Si4 Si 0.37450(6) -0.15555(6) 0.12959(5) 0.03870(18) Uani 1 1 d . . . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 C1 0.0509(13) 0.0511(14) 0.0340(11) 0.0089(10) -0.0080(9) 0.0044(10) C2 0.0525(16) 0.082(2) 0.0559(16) 0.0084(14) -0.0058(12) 0.0023(14) C3 0.0724(18) 0.0562(16) 0.0619(17) 0.0098(13) -0.0015(14) 0.0201(13) C4 0.0763(19) 0.091(2) 0.0310(12) 0.0106(13) -0.0079(12) 0.0123(16) C5 0.0537(13) 0.0473(13) 0.0385(11) 0.0075(10) -0.0174(10) 0.0026(10) C6 0.0824(19) 0.0418(14) 0.0757(19) 0.0010(13) -0.0352(15) 0.0041(13) C7 0.0585(16) 0.0653(18) 0.0723(18) 0.0057(14) -0.0250(14) -0.0068(13) C8 0.099(2) 0.077(2) 0.0422(14) 0.0105(13) -0.0379(14) -0.0117(16) C9 0.0540(14) 0.0534(14) 0.0475(13) 0.0214(11) -0.0200(11) 0.0027(10) C10 0.091(2) 0.131(3) 0.0571(17) 0.0484(19) -0.0283(16) 0.019(2) C11 0.0597(16) 0.0683(18) 0.0813(19) 0.0314(15) -0.0335(14) -0.0032(13) C12 0.079(2) 0.0624(18) 0.107(2) 0.0411(17) -0.0441(18) 0.0026(14) C13 0.0548(14) 0.0579(15) 0.0492(14) 0.0298(12) -0.0135(11) 0.0010(11) C14 0.095(2) 0.111(3) 0.0529(16) 0.0519(18) -0.0205(15) -0.0185(19) C15 0.081(2) 0.0612(18) 0.098(2) 0.0514(17) -0.0114(17) 0.0013(15) C16 0.0593(17) 0.090(2) 0.082(2) 0.0545(18) -0.0151(14) -0.0085(15) O1 0.0449(9) 0.0509(9) 0.0380(8) 0.0107(7) -0.0109(6) 0.0029(7) O2 0.0570(9) 0.0414(9) 0.0415(8) 0.0094(7) -0.0198(7) 0.0074(7) O3 0.0463(9) 0.0555(10) 0.0450(8) 0.0234(7) -0.0142(7) -0.0014(7) O4 0.0561(9) 0.0446(9) 0.0384(8) 0.0148(7) -0.0077(7) 0.0062(7) O5 0.0544(9) 0.0535(9) 0.0313(8) 0.0120(7) -0.0119(6) 0.0120(7) O6 0.0610(10) 0.0481(9) 0.0339(8) 0.0154(7) -0.0170(7) -0.0040(7) Si1 0.0461(4) 0.0408(3) 0.0287(3) 0.0093(2) -0.0101(2) 0.0060(2) Si2 0.0467(4) 0.0378(3) 0.0298(3) 0.0086(2) -0.0131(2) 0.0029(2) Si3 0.0471(4) 0.0406(3) 0.0313(3) 0.0133(2) -0.0138(2) 0.0042(2) Si4 0.0473(4) 0.0400(3) 0.0311(3) 0.0146(2) -0.0115(3) 0.0021(2) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag C1 C2 1.537(4) . ? C1 C4 1.539(3) . ? C1 C3 1.543(4) . ? C1 Si1 1.871(2) . ? C2 H2A 0.9800 . ? C2 H2B 0.9800 . ? C2 H2C 0.9800 . ? C3 H3A 0.9800 . ? C3 H3B 0.9800 . ? C3 H3C 0.9800 . ? C4 H4C 0.9800 . ? C4 H4B 0.9800 . ? C4 H4A 0.9800 . ? C5 C6 1.532(4) . ? C5 C7 1.538(4) . ? C5 C8 1.541(3) . ? C5 Si2 1.868(2) . ? C6 H6A 0.9800 . ? C6 H6B 0.9800 . ? C6 H6C 0.9800 . ? C7 H7A 0.9800 . ? C7 H7B 0.9800 . ? C7 H7C 0.9800 . ? C8 H8C 0.9800 . ? C8 H8B 0.9800 . ? C8 H8A 0.9800 . ? C9 C11 1.530(4) . ? C9 C12 1.539(4) . ? C9 C10 1.541(4) . ? C9 Si3 1.868(2) . ? C10 H10A 0.9800 . ? C10 H10B 0.9800 . ? C10 H10C 0.9800 . ? C11 H11A 0.9800 . ? C11 H11B 0.9800 . ? C11 H11C 0.9800 . ? C12 H12C 0.9800 . ? C12 H12B 0.9800 . ? C12 H12A 0.9800 . ? C13 C15 1.532(4) . ? C13 C16 1.535(4) . ? C13 C14 1.539(4) . ? C13 Si4 1.872(2) . ? C14 H14A 0.9800 . ? C14 H14B 0.9800 . ? C14 H14C 0.9800 . ? C15 H15A 0.9800 . ? C15 H15B 0.9800 . ? C15 H15C 0.9800 . ? C16 H16C 0.9800 . ? C16 H16B 0.9800 . ? C16 H16A 0.9800 . ? O1 Si2 1.6272(16) . ? O1 Si1 1.6283(17) . ? O2 Si3 1.6277(16) . ? O2 Si2 1.6286(16) . ? O3 Si3 1.6217(16) . ? O3 Si4 1.6318(16) . ? O4 Si4 1.6262(16) . ? O4 Si1 1.6293(17) . ? O5 Si1 1.6297(15) . ? O5 Si3 1.6308(15) 2_655 ? O6 Si4 1.6248(15) 2_655 ? O6 Si2 1.6296(15) . ? Si3 O5 1.6308(15) 2_655 ? Si4 O6 1.6248(15) 2_655 ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag C2 C1 C4 109.9(2) . . ? C2 C1 C3 109.0(2) . . ? C4 C1 C3 109.1(2) . . ? C2 C1 Si1 110.05(17) . . ? C4 C1 Si1 109.02(18) . . ? C3 C1 Si1 109.74(17) . . ? C1 C2 H2A 109.5 . . ? C1 C2 H2B 109.5 . . ? H2A C2 H2B 109.5 . . ? C1 C2 H2C 109.5 . . ? H2A C2 H2C 109.5 . . ? H2B C2 H2C 109.5 . . ? C1 C3 H3A 109.5 . . ? C1 C3 H3B 109.5 . . ? H3A C3 H3B 109.5 . . ? C1 C3 H3C 109.5 . . ? H3A C3 H3C 109.5 . . ? H3B C3 H3C 109.5 . . ? C1 C4 H4C 109.5 . . ? C1 C4 H4B 109.5 . . ? H4C C4 H4B 109.5 . . ? C1 C4 H4A 109.5 . . ? H4C C4 H4A 109.5 . . ? H4B C4 H4A 109.5 . . ? C6 C5 C7 109.2(2) . . ? C6 C5 C8 110.2(2) . . ? C7 C5 C8 108.7(2) . . ? C6 C5 Si2 109.17(17) . . ? C7 C5 Si2 110.26(16) . . ? C8 C5 Si2 109.28(18) . . ? C5 C6 H6A 109.5 . . ? C5 C6 H6B 109.5 . . ? H6A C6 H6B 109.5 . . ? C5 C6 H6C 109.5 . . ? H6A C6 H6C 109.5 . . ? H6B C6 H6C 109.5 . . ? C5 C7 H7A 109.5 . . ? C5 C7 H7B 109.5 . . ? H7A C7 H7B 109.5 . . ? C5 C7 H7C 109.5 . . ? H7A C7 H7C 109.5 . . ? H7B C7 H7C 109.5 . . ? C5 C8 H8C 109.5 . . ? C5 C8 H8B 109.5 . . ? H8C C8 H8B 109.5 . . ? C5 C8 H8A 109.5 . . ? H8C C8 H8A 109.5 . . ? H8B C8 H8A 109.5 . . ? C11 C9 C12 108.5(2) . . ? C11 C9 C10 109.1(2) . . ? C12 C9 C10 109.9(2) . . ? C11 C9 Si3 109.33(17) . . ? C12 C9 Si3 109.92(17) . . ? C10 C9 Si3 109.95(18) . . ? C9 C10 H10A 109.5 . . ? C9 C10 H10B 109.5 . . ? H10A C10 H10B 109.5 . . ? C9 C10 H10C 109.5 . . ? H10A C10 H10C 109.5 . . ? H10B C10 H10C 109.5 . . ? C9 C11 H11A 109.5 . . ? C9 C11 H11B 109.5 . . ? H11A C11 H11B 109.5 . . ? C9 C11 H11C 109.5 . . ? H11A C11 H11C 109.5 . . ? H11B C11 H11C 109.5 . . ? C9 C12 H12C 109.5 . . ? C9 C12 H12B 109.5 . . ? H12C C12 H12B 109.5 . . ? C9 C12 H12A 109.5 . . ? H12C C12 H12A 109.5 . . ? H12B C12 H12A 109.5 . . ? C15 C13 C16 109.5(2) . . ? C15 C13 C14 109.6(2) . . ? C16 C13 C14 109.3(2) . . ? C15 C13 Si4 108.04(17) . . ? C16 C13 Si4 110.48(17) . . ? C14 C13 Si4 109.95(19) . . ? C13 C14 H14A 109.5 . . ? C13 C14 H14B 109.5 . . ? H14A C14 H14B 109.5 . . ? C13 C14 H14C 109.5 . . ? H14A C14 H14C 109.5 . . ? H14B C14 H14C 109.5 . . ? C13 C15 H15A 109.5 . . ? C13 C15 H15B 109.5 . . ? H15A C15 H15B 109.5 . . ? C13 C15 H15C 109.5 . . ? H15A C15 H15C 109.5 . . ? H15B C15 H15C 109.5 . . ? C13 C16 H16C 109.5 . . ? C13 C16 H16B 109.5 . . ? H16C C16 H16B 109.5 . . ? C13 C16 H16A 109.5 . . ? H16C C16 H16A 109.5 . . ? H16B C16 H16A 109.5 . . ? Si2 O1 Si1 152.59(11) . . ? Si3 O2 Si2 147.83(11) . . ? Si3 O3 Si4 152.81(11) . . ? Si4 O4 Si1 147.61(11) . . ? Si1 O5 Si3 146.76(11) . 2_655 ? Si4 O6 Si2 147.33(11) 2_655 . ? O1 Si1 O4 109.24(9) . . ? O1 Si1 O5 109.08(9) . . ? O4 Si1 O5 109.23(9) . . ? O1 Si1 C1 109.75(10) . . ? O4 Si1 C1 109.19(10) . . ? O5 Si1 C1 110.33(10) . . ? O1 Si2 O2 109.11(9) . . ? O1 Si2 O6 108.83(9) . . ? O2 Si2 O6 109.18(8) . . ? O1 Si2 C5 110.03(10) . . ? O2 Si2 C5 110.17(10) . . ? O6 Si2 C5 109.50(10) . . ? O3 Si3 O2 108.99(9) . . ? O3 Si3 O5 109.12(9) . 2_655 ? O2 Si3 O5 109.09(8) . 2_655 ? O3 Si3 C9 110.18(10) . . ? O2 Si3 C9 109.50(10) . . ? O5 Si3 C9 109.94(10) 2_655 . ? O6 Si4 O4 109.07(9) 2_655 . ? O6 Si4 O3 108.91(8) 2_655 . ? O4 Si4 O3 109.16(9) . . ? O6 Si4 C13 109.44(10) 2_655 . ? O4 Si4 C13 110.83(10) . . ? O3 Si4 C13 109.41(10) . . ? _diffrn_measured_fraction_theta_max 0.977 _diffrn_reflns_theta_full 24.84 _diffrn_measured_fraction_theta_full 0.977 _refine_diff_density_max 0.349 _refine_diff_density_min -0.458 _refine_diff_density_rms 0.063 _iucr_refine_instructions_details ; TITL NATASCHA HURKES, -100DEGC, AP CELL 0.71073 10.74260 11.01020 11.86400 68.70900 72.22900 85.31400 ZERR 1 0.00140 0.00130 0.00140 0.00900 0.00900 0.01000 LATT 1 SFAC C H O SI UNIT 32 72 12 8 TEMP -100 L.S. 15 ACTA BOND $H SIZE 0.070 0.330 0.520 OMIT -6 50 FMAP 2 PLAN 25 WGHT 0.094000 FVAR 0.89108 C1 1 0.673418 0.157742 0.758246 11.00000 0.05449 0.04670 = 0.03796 -0.00786 -0.01657 -0.00347 C2 1 0.652854 0.177757 0.884652 11.00000 0.10054 0.07656 = 0.04161 -0.01064 -0.03712 0.01010 AFIX 137 H2A 2 0.701462 0.256648 0.869144 11.00000 -1.20000 H2B 2 0.684517 0.102212 0.942512 11.00000 -1.20000 H2C 2 0.559511 0.187135 0.922662 11.00000 -1.20000 AFIX 0 C3 1 0.820748 0.148380 0.697748 11.00000 0.05958 0.06445 = 0.07203 -0.00549 -0.02417 0.00598 AFIX 137 H3A 2 0.855148 0.075356 0.755665 11.00000 -1.20000 H3B 2 0.865971 0.229680 0.681105 11.00000 -1.20000 H3C 2 0.835022 0.134138 0.617917 11.00000 -1.20000 AFIX 0 C4 1 0.602971 0.031435 0.781503 11.00000 0.08317 0.04142 = 0.07504 -0.00118 -0.03363 -0.00507 AFIX 137 H4C 2 0.618455 0.018589 0.700856 11.00000 -1.20000 H4B 2 0.508877 0.037380 0.819162 11.00000 -1.20000 H4A 2 0.636532 -0.042435 0.839363 11.00000 -1.20000 AFIX 0 C5 1 0.176396 0.262108 0.851180 11.00000 0.05166 0.05097 = 0.03346 -0.00905 -0.00701 -0.00524 C6 1 0.209474 0.260918 0.968984 11.00000 0.07746 0.09028 = 0.03021 -0.01060 -0.00657 -0.01319 AFIX 137 H6A 2 0.297659 0.228455 0.966185 11.00000 -1.20000 H6B 2 0.146111 0.203889 1.045503 11.00000 -1.20000 H6C 2 0.205712 0.349653 0.970273 11.00000 -1.20000 AFIX 0 C7 1 0.171949 0.120621 0.855155 11.00000 0.07313 0.05580 = 0.06118 -0.00982 -0.00035 -0.02071 AFIX 137 H7A 2 0.108376 0.067997 0.934178 11.00000 -1.20000 H7B 2 0.258691 0.083707 0.850917 11.00000 -1.20000 H7C 2 0.145959 0.120444 0.782891 11.00000 -1.20000 AFIX 0 C8 1 0.042040 0.321402 0.850421 11.00000 0.05364 0.08208 = 0.05516 -0.00848 -0.00439 -0.00341 AFIX 137 H8C 2 0.022624 0.324539 0.773906 11.00000 -1.20000 H8B 2 0.042985 0.409946 0.851385 11.00000 -1.20000 H8A 2 -0.025211 0.267554 0.925490 11.00000 -1.20000 AFIX 0 C9 1 0.295462 0.765568 0.718101 11.00000 0.05587 0.05774 = 0.04836 -0.02991 -0.01230 -0.00190 C10 1 0.150325 0.779466 0.725374 11.00000 0.06047 0.08986 = 0.08110 -0.05416 -0.01382 0.00734 AFIX 137 H10A 2 0.141740 0.812178 0.639558 11.00000 -1.20000 H10B 2 0.111660 0.840859 0.768072 11.00000 -1.20000 H10C 2 0.104798 0.694245 0.773142 11.00000 -1.20000 AFIX 0 C11 1 0.366030 0.899566 0.647204 11.00000 0.08131 0.06025 = 0.09694 -0.05075 -0.01072 -0.00208 AFIX 137 H11A 2 0.326297 0.958968 0.691979 11.00000 -1.20000 H11B 2 0.358258 0.934748 0.561080 11.00000 -1.20000 H11C 2 0.458636 0.890625 0.643241 11.00000 -1.20000 AFIX 0 C12 1 0.308178 0.709964 0.853310 11.00000 0.09627 0.11063 = 0.05226 -0.05160 -0.01965 0.01661 AFIX 137 H12C 2 0.400911 0.704988 0.849063 11.00000 -1.20000 H12B 2 0.266809 0.622507 0.897212 11.00000 -1.20000 H12A 2 0.264901 0.767026 0.899663 11.00000 -1.20000 AFIX 0 C13 1 0.790959 0.659186 0.630312 11.00000 0.05538 0.05326 = 0.04593 -0.02089 -0.01895 -0.00376 C14 1 0.803000 0.808734 0.567778 11.00000 0.08059 0.06202 = 0.10639 -0.04143 -0.04378 -0.00340 AFIX 137 H14A 2 0.861100 0.842702 0.599834 11.00000 -1.20000 H14B 2 0.716372 0.845545 0.587930 11.00000 -1.20000 H14C 2 0.839199 0.833205 0.475741 11.00000 -1.20000 AFIX 0 C15 1 0.742043 0.619544 0.775620 11.00000 0.09179 0.13089 = 0.05645 -0.04807 -0.02752 -0.02041 AFIX 137 H15A 2 0.657944 0.659377 0.800079 11.00000 -1.20000 H15B 2 0.805995 0.649654 0.804357 11.00000 -1.20000 H15C 2 0.731094 0.524400 0.814794 11.00000 -1.20000 AFIX 0 C16 1 0.925959 0.603721 0.592410 11.00000 0.06057 0.06848 = 0.08031 -0.03099 -0.03258 0.00215 AFIX 137 H16C 2 0.920255 0.508524 0.633108 11.00000 -1.20000 H16B 2 0.987306 0.639666 0.619620 11.00000 -1.20000 H16A 2 0.956896 0.627403 0.500196 11.00000 -1.20000 AFIX 0 O1 3 0.448102 0.300304 0.709886 11.00000 0.04606 0.05077 = 0.03727 -0.01100 -0.00984 -0.00395 O2 3 0.305591 0.510493 0.700387 11.00000 0.05683 0.04424 = 0.03780 -0.01484 -0.00684 -0.00721 O3 3 0.529320 0.645142 0.620700 11.00000 0.04761 0.05502 = 0.04378 -0.02314 -0.01310 0.00030 O4 3 0.670842 0.435031 0.633927 11.00000 0.05802 0.04062 = 0.04111 -0.00941 -0.01872 -0.00849 O5 3 0.639070 0.284391 0.512906 11.00000 0.06173 0.04757 = 0.03336 -0.01535 -0.01600 0.00271 O6 3 0.276586 0.358635 0.579333 11.00000 0.05545 0.05362 = 0.03058 -0.01194 -0.01112 -0.01293 SI1 4 0.606028 0.298393 0.651069 11.00000 0.04751 0.03740 = 0.02921 -0.00861 -0.01217 -0.00379 SI2 4 0.305366 0.360490 0.705822 11.00000 0.04693 0.04061 = 0.02809 -0.00938 -0.00910 -0.00693 SI3 4 0.374495 0.655537 0.629591 11.00000 0.04814 0.03972 = 0.03048 -0.01462 -0.01056 -0.00311 SI4 4 0.675177 0.593731 0.574897 11.00000 0.04788 0.04032 = 0.03065 -0.01325 -0.01277 -0.00504 HKLF 4 REM NATASCHA HURKES, -100DEGC, AP REM R1 = 0.0449 for 3353 Fo > 4sig(Fo) and 0.0528 for all 4199 data REM 247 parameters refined using 0 restraints END WGHT 0.0940 0.0000 REM Highest difference peak 0.412, deepest hole -0.409, 1-sigma level 0.060 Q1 1 0.6527 0.2261 0.7057 11.00000 0.05 0.41 Q2 1 0.6620 0.5559 0.6803 11.00000 0.05 0.29 Q3 1 0.3090 0.7365 0.6772 11.00000 0.05 0.27 Q4 1 0.3245 0.4768 0.6562 11.00000 0.05 0.27 Q5 1 0.6268 0.3310 0.4513 11.00000 0.05 0.26 Q6 1 0.6622 0.4866 0.6094 11.00000 0.05 0.26 Q7 1 0.6575 0.3788 0.6910 11.00000 0.05 0.25 Q8 1 0.7674 0.6389 0.5999 11.00000 0.05 0.25 Q9 1 0.2700 0.3000 0.7885 11.00000 0.05 0.24 Q10 1 0.4580 0.3429 0.6666 11.00000 0.05 0.23 Q11 1 0.2882 0.2978 0.6393 11.00000 0.05 0.22 Q12 1 0.3013 0.4531 0.7312 11.00000 0.05 0.22 Q13 1 0.6628 0.2356 0.5569 11.00000 0.05 0.21 Q14 1 0.5229 0.6130 0.5809 11.00000 0.05 0.21 Q15 1 0.4712 0.2463 0.7653 11.00000 0.05 0.21 Q16 1 0.7747 0.7127 0.6071 11.00000 0.05 0.20 Q17 1 0.5305 0.7056 0.5790 11.00000 0.05 0.20 Q18 1 0.4815 0.5639 0.7391 11.00000 0.05 0.19 Q19 1 0.4438 0.3371 0.7346 11.00000 0.05 0.19 Q20 1 0.1693 0.4982 0.7002 11.00000 0.05 0.19 Q21 1 0.2759 0.3236 0.5477 11.00000 0.05 0.18 Q22 1 0.2936 0.9783 0.5807 11.00000 0.05 0.18 Q23 1 0.6426 0.3558 0.5334 11.00000 0.05 0.18 Q24 1 0.5920 0.2414 0.9357 11.00000 0.05 0.18 Q25 1 0.1995 0.2843 0.8970 11.00000 0.05 0.18 ; #---------------------------------------------------------------------------- data_4b_NH235B _audit_author_name 'Ferdinand Belaj' _audit_creation_method 'manual edited SHELXL-97 .cif file' _chemical_compound_source 'synthetical product' _chemical_name_systematic ; octakis(1,1-dimethylpropyl)octasilsesquioxane ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety 'C40 H88 O12 Si8' _chemical_formula_sum 'C40 H88 O12 Si8' _chemical_formula_weight 985.81 loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source 'C' 'C' 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'H' 'H' 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'O' 'O' 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'Si' 'Si' 0.0817 0.0704 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting 'trigonal' _symmetry_space_group_name_H-M 'R -3 c' _symmetry_space_group_name_Hall '-R 3 2"c' loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-y, x-y, z' '-x+y, -x, z' 'y, x, -z+1/2' 'x-y, -y, -z+1/2' '-x, -x+y, -z+1/2' 'x+2/3, y+1/3, z+1/3' '-y+2/3, x-y+1/3, z+1/3' '-x+y+2/3, -x+1/3, z+1/3' 'y+2/3, x+1/3, -z+5/6' 'x-y+2/3, -y+1/3, -z+5/6' '-x+2/3, -x+y+1/3, -z+5/6' 'x+1/3, y+2/3, z+2/3' '-y+1/3, x-y+2/3, z+2/3' '-x+y+1/3, -x+2/3, z+2/3' 'y+1/3, x+2/3, -z+7/6' 'x-y+1/3, -y+2/3, -z+7/6' '-x+1/3, -x+y+2/3, -z+7/6' '-x, -y, -z' 'y, -x+y, -z' 'x-y, x, -z' '-y, -x, z-1/2' '-x+y, y, z-1/2' 'x, x-y, z-1/2' '-x+2/3, -y+1/3, -z+1/3' 'y+2/3, -x+y+1/3, -z+1/3' 'x-y+2/3, x+1/3, -z+1/3' '-y+2/3, -x+1/3, z-1/6' '-x+y+2/3, y+1/3, z-1/6' 'x+2/3, x-y+1/3, z-1/6' '-x+1/3, -y+2/3, -z+2/3' 'y+1/3, -x+y+2/3, -z+2/3' 'x-y+1/3, x+2/3, -z+2/3' '-y+1/3, -x+2/3, z+1/6' '-x+y+1/3, y+2/3, z+1/6' 'x+1/3, x-y+2/3, z+1/6' _cell_length_a 13.2192(4) _cell_length_b 13.2192(4) _cell_length_c 53.3347(18) _cell_angle_alpha 90.00 _cell_angle_beta 90.00 _cell_angle_gamma 120.00 _cell_volume 8071.4(5) _cell_formula_units_Z 6 _cell_measurement_temperature 100(2) _cell_measurement_reflns_used 9715 _cell_measurement_theta_min 2.34 _cell_measurement_theta_max 31.03 _exptl_crystal_description 'block' _exptl_crystal_colour 'colourless' _exptl_crystal_size_max 0.30 _exptl_crystal_size_mid 0.26 _exptl_crystal_size_min 0.25 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.217 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 3216 _exptl_absorpt_coefficient_mu 0.252 _exptl_absorpt_correction_type 'multi-scan' _exptl_absorpt_correction_T_min 0.5440 _exptl_absorpt_correction_T_max 0.7462 _exptl_absorpt_process_details 'Bruker SADABS' _exptl_special_details ; ? ; _diffrn_ambient_temperature 100(2) _diffrn_measurement_device_type 'Bruker APEX-II CCD' _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_type 'MoK\a' _diffrn_radiation_monochromator 'graphite' _diffrn_radiation_wavelength 0.71073 _diffrn_measurement_method '\f and \w scans' _diffrn_detector_area_resol_mean ? _diffrn_standards_number 0 _diffrn_standards_interval_count ? _diffrn_standards_decay_% ? _diffrn_reflns_number 14563 _diffrn_reflns_av_R_equivalents 0.0238 _diffrn_reflns_av_sigmaI/netI 0.0172 _diffrn_reflns_limit_h_min -17 _diffrn_reflns_limit_h_max 13 _diffrn_reflns_limit_k_min -14 _diffrn_reflns_limit_k_max 18 _diffrn_reflns_limit_l_min -75 _diffrn_reflns_limit_l_max 54 _diffrn_reflns_theta_min 2.34 _diffrn_reflns_theta_max 30.00 _reflns_number_total 2623 _reflns_number_gt 2265 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'Bruker APEX2' _computing_cell_refinement 'Bruker SAINT' _computing_data_reduction 'Bruker SAINT' _computing_structure_solution 'SHELXS-97 (Sheldrick, 2008)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 2008)' _computing_molecular_graphics 'modified ORTEP (Johnson, 1965)' _computing_publication_material 'SHELXL-97 (Sheldrick, 2008)' _refine_special_details ; Refinement of F^2^ against ALL reflections. The weighted R-factor wR and goodness of fit S are based on F^2^, conventional R-factors R are based on F, with F set to zero for negative F^2^. The threshold expression of F^2^ > 2sigma(F^2^) is used only for calculating R-factors(gt) etc. and is not relevant to the choice of reflections for refinement. R-factors based on F^2^ are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger. The tert. pentyl group bonded to the atom Si1, which lies on a three-fold rotation axis, is disordered over three orientations and was refined with site occupation factors of 1/3 and 2/3, respectively. The tert. pentyl group bonded to the atom Si2, which lies on a general position, is also disordered over three orientations and was refined with site occupation factors adding to unity. The ordered non-hydrogen atoms were refined with anisotropic displacement parameters without any constraints. Due to disorder the C-C distances were fixed to be equal in length (DFIX of SHELXL-97) but this C-C bond length was enabled to refine resulting in a value of 1.538(2) \%A. The bonds within the tert. pentyl groups were subjected to a rigid bond restraint (DELU instruction of SHELXL-97). The H atoms of the CH~2~ groups were refined with one common isotropic displacement parameter for these H atoms and idealized geometry with approximately tetrahedral angles and C-H distances of 0.99 \%A (AFIX 23 of SHELXL-97). The H atoms of the methyl groups were refined with one common isotropic displacement parameter for these H atoms and idealized geometry with tetrahedral angles, staggered conformation, and C-H distances of 0.98 \%A (AFIX 33 of SHELXL-97). ; _refine_ls_structure_factor_coef Fsqd _refine_ls_matrix_type full _refine_ls_weighting_scheme calc _refine_ls_weighting_details 'calc w=1/[\s^2^(Fo^2^)+(0.0725P)^2^+12.2905P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment refU _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 2623 _refine_ls_number_parameters 157 _refine_ls_number_restraints 125 _refine_ls_R_factor_all 0.0482 _refine_ls_R_factor_gt 0.0416 _refine_ls_wR_factor_ref 0.1280 _refine_ls_wR_factor_gt 0.1200 _refine_ls_goodness_of_fit_ref 1.064 _refine_ls_restrained_S_all 1.172 _refine_ls_shift/su_max 0.001 _refine_ls_shift/su_mean 0.000 loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_occupancy _atom_site_symmetry_multiplicity _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group Si1 Si 0.6667 0.3333 0.282618(15) 0.02474(18) Uani 1 3 d S . . Si2 Si 0.74593(3) 0.55322(3) 0.316449(8) 0.02359(15) Uani 1 1 d . B . O1 O 0.71725(11) 0.46502(10) 0.29307(2) 0.0311(3) Uani 1 1 d . . . O2 O 0.62762(10) 0.51057(10) 0.33262(2) 0.0296(3) Uani 1 1 d . . . C11 C 0.6667 0.3333 0.24764(6) 0.0405(6) Uani 1 3 d SDU . . C12 C 0.6153(5) 0.4089(6) 0.23836(15) 0.0608(14) Uani 0.66667 1 d PDU A 1 H121 H 0.5346 0.3751 0.2443 0.078(4) Uiso 0.66667 1 calc PR A 1 H122 H 0.6166 0.4111 0.2200 0.078(4) Uiso 0.66667 1 calc PR A 1 H123 H 0.6621 0.4884 0.2449 0.078(4) Uiso 0.66667 1 calc PR A 1 C13 C 0.6433(8) 0.4278(8) 0.2371(3) 0.0468(18) Uani 0.33333 1 d PDU A 2 H131 H 0.6578 0.4358 0.2188 0.060(9) Uiso 0.33333 1 calc PR A 2 H132 H 0.6966 0.5039 0.2451 0.060(9) Uiso 0.33333 1 calc PR A 2 C14 C 0.5159(7) 0.3934(8) 0.24245(16) 0.0576(18) Uani 0.33333 1 d PDU A 2 H141 H 0.5006 0.4536 0.2358 0.078(4) Uiso 0.33333 1 calc PR A 2 H142 H 0.5022 0.3862 0.2606 0.078(4) Uiso 0.33333 1 calc PR A 2 H143 H 0.4636 0.3185 0.2344 0.078(4) Uiso 0.33333 1 calc PR A 2 C21 C 0.79990(15) 0.70412(14) 0.30437(4) 0.0364(3) Uani 1 1 d DU . . C22 C 0.6984(2) 0.70702(19) 0.29107(5) 0.0532(6) Uani 1 1 d DU B . H221 H 0.7252 0.7858 0.2846 0.078(4) Uiso 1 1 calc R . . H222 H 0.6345 0.6860 0.3030 0.078(4) Uiso 1 1 calc R . . H223 H 0.6706 0.6511 0.2772 0.078(4) Uiso 1 1 calc R . . C23 C 0.8303(6) 0.7850(4) 0.32772(10) 0.0549(15) Uani 0.575(4) 1 d PDU B 1 H231 H 0.8953 0.7862 0.3369 0.078(4) Uiso 0.575(4) 1 calc PR B 1 H232 H 0.7620 0.7552 0.3387 0.078(4) Uiso 0.575(4) 1 calc PR B 1 H233 H 0.8530 0.8643 0.3223 0.078(4) Uiso 0.575(4) 1 calc PR B 1 C24 C 0.8647(5) 0.8033(6) 0.32282(13) 0.0436(12) Uani 0.425(4) 1 d PDU B 2 H241 H 0.9327 0.8004 0.3297 0.060(9) Uiso 0.425(4) 1 calc PR B 2 H242 H 0.8936 0.8792 0.3142 0.060(9) Uiso 0.425(4) 1 calc PR B 2 C25 C 0.7827(5) 0.7919(5) 0.34380(12) 0.0565(13) Uani 0.425(4) 1 d PDU B 2 H251 H 0.8240 0.8562 0.3557 0.078(4) Uiso 0.425(4) 1 calc PR B 2 H252 H 0.7553 0.7172 0.3524 0.078(4) Uiso 0.425(4) 1 calc PR B 2 H253 H 0.7156 0.7950 0.3368 0.078(4) Uiso 0.425(4) 1 calc PR B 2 C26 C 0.8979(5) 0.7331(7) 0.28477(12) 0.0391(10) Uani 0.425(4) 1 d PDU B 2 H261 H 0.8677 0.6741 0.2715 0.078(4) Uiso 0.425(4) 1 calc PR B 2 H262 H 0.9642 0.7333 0.2930 0.078(4) Uiso 0.425(4) 1 calc PR B 2 H263 H 0.9234 0.8103 0.2775 0.078(4) Uiso 0.425(4) 1 calc PR B 2 C27 C 0.9231(6) 0.7598(9) 0.2932(2) 0.0503(18) Uani 0.274(6) 1 d PDU B 3 H271 H 0.9332 0.6999 0.2842 0.060(9) Uiso 0.274(6) 1 calc PR B 3 H272 H 0.9819 0.7925 0.3068 0.060(9) Uiso 0.274(6) 1 calc PR B 3 C28 C 0.9413(7) 0.8585(6) 0.27481(14) 0.0426(17) Uani 0.274(6) 1 d PDU B 3 H281 H 1.0213 0.8970 0.2683 0.078(4) Uiso 0.274(6) 1 calc PR B 3 H282 H 0.9279 0.9158 0.2836 0.078(4) Uiso 0.274(6) 1 calc PR B 3 H283 H 0.8860 0.8249 0.2608 0.078(4) Uiso 0.274(6) 1 calc PR B 3 C29 C 0.8785(9) 0.7248(16) 0.28109(14) 0.050(2) Uani 0.301(5) 1 d PDU B 4 H291 H 0.8326 0.6650 0.2683 0.060(9) Uiso 0.301(5) 1 calc PR B 4 H292 H 0.9010 0.8022 0.2739 0.060(9) Uiso 0.301(5) 1 calc PR B 4 C30 C 0.9891(7) 0.7198(9) 0.2869(2) 0.068(3) Uani 0.301(5) 1 d PDU B 4 H301 H 1.0357 0.7361 0.2715 0.078(4) Uiso 0.301(5) 1 calc PR B 4 H302 H 0.9676 0.6419 0.2931 0.078(4) Uiso 0.301(5) 1 calc PR B 4 H303 H 1.0349 0.7784 0.2996 0.078(4) Uiso 0.301(5) 1 calc PR B 4 loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 Si1 0.0194(2) 0.0194(2) 0.0354(4) 0.000 0.000 0.00971(11) Si2 0.0157(2) 0.0130(2) 0.0416(3) 0.00275(15) 0.00193(15) 0.00684(15) O1 0.0294(6) 0.0197(5) 0.0428(6) 0.0020(4) 0.0044(5) 0.0112(4) O2 0.0193(5) 0.0196(5) 0.0502(7) 0.0007(5) 0.0057(5) 0.0101(4) C11 0.0418(9) 0.0418(9) 0.0380(14) 0.000 0.000 0.0209(4) C12 0.058(3) 0.064(3) 0.058(3) 0.028(2) -0.007(2) 0.029(2) C13 0.048(3) 0.040(3) 0.053(4) 0.006(2) 0.007(3) 0.022(3) C14 0.055(3) 0.065(4) 0.064(4) 0.023(3) 0.014(3) 0.038(3) C21 0.0286(7) 0.0174(6) 0.0605(9) 0.0069(6) -0.0063(6) 0.0096(6) C22 0.0454(10) 0.0316(9) 0.0830(16) 0.0070(9) -0.0218(9) 0.0195(8) C23 0.068(4) 0.0115(16) 0.073(3) -0.0009(18) -0.021(2) 0.011(2) C24 0.028(2) 0.019(2) 0.074(2) 0.002(2) -0.0074(14) 0.0053(18) C25 0.057(3) 0.038(2) 0.066(3) -0.003(2) -0.002(2) 0.017(2) C26 0.0241(17) 0.021(2) 0.045(2) 0.0140(18) -0.0105(15) -0.0099(19) C27 0.0385(17) 0.036(3) 0.068(4) 0.016(3) 0.007(2) 0.012(3) C28 0.039(3) 0.030(3) 0.048(3) 0.004(2) -0.002(2) 0.009(2) C29 0.046(3) 0.043(4) 0.051(3) 0.014(3) -0.003(2) 0.013(3) C30 0.054(3) 0.061(5) 0.096(6) 0.035(4) 0.030(3) 0.034(4) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag Si1 O1 1.6199(12) . ? Si1 C11 1.865(4) . ? Si2 O1 1.6175(13) . ? Si2 O2 1.6194(12) 32 ? Si2 O2 1.6203(12) . ? Si2 C21 1.8655(17) . ? C11 C13 1.535(5) . ? C11 C12 1.544(3) . ? C12 H121 0.98 . ? C12 H122 0.98 . ? C12 H123 0.98 . ? C13 C14 1.535(5) . ? C13 H131 0.99 . ? C13 H132 0.99 . ? C14 H141 0.98 . ? C14 H142 0.98 . ? C14 H143 0.98 . ? C21 C24 1.516(4) . ? C21 C27 1.532(4) . ? C21 C22 1.535(2) . ? C21 C29 1.553(5) . ? C21 C26 1.556(4) . ? C21 C23 1.557(4) . ? C22 H221 0.98 . ? C22 H222 0.98 . ? C22 H223 0.98 . ? C23 H231 0.98 . ? C23 H232 0.98 . ? C23 H233 0.98 . ? C24 C25 1.512(4) . ? C24 H241 0.99 . ? C24 H242 0.99 . ? C25 H251 0.98 . ? C25 H252 0.98 . ? C25 H253 0.98 . ? C26 H261 0.98 . ? C26 H262 0.98 . ? C26 H263 0.98 . ? C27 C28 1.553(5) . ? C27 H271 0.99 . ? C27 H272 0.99 . ? C28 H281 0.98 . ? C28 H282 0.98 . ? C28 H283 0.98 . ? C29 C30 1.527(5) . ? C29 H291 0.99 . ? C29 H292 0.99 . ? C30 H301 0.98 . ? C30 H302 0.98 . ? C30 H303 0.98 . ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag O1 Si1 O1 108.82(5) 2_655 . ? O1 Si1 C11 110.12(5) . . ? O1 Si2 O2 109.17(7) . 32 ? O1 Si2 O2 108.78(7) . . ? O2 Si2 O2 109.17(5) 32 . ? O1 Si2 C21 109.33(8) . . ? O2 Si2 C21 110.35(7) 32 . ? O2 Si2 C21 110.02(7) . . ? Si2 O1 Si1 149.53(9) . . ? Si2 O2 Si2 148.96(8) 33_545 . ? C13 C11 C13 107.4(6) 2_655 . ? C13 C11 C12 118.9(5) 2_655 3_665 ? C13 C11 C12 98.1(4) . 3_665 ? C13 C11 C12 98.1(4) 3_665 2_655 ? C13 C11 C12 118.9(5) . 2_655 ? C12 C11 C12 110.2(3) 3_665 2_655 ? C13 C11 C12 118.9(5) 3_665 . ? C13 C11 C12 98.1(4) 2_655 . ? C12 C11 C12 110.2(3) 3_665 . ? C12 C11 C12 110.2(3) 2_655 . ? C13 C11 Si1 111.4(6) . . ? C12 C11 Si1 108.7(3) . . ? C11 C12 H121 109.5 . . ? C11 C12 H122 109.5 . . ? H121 C12 H122 109.5 . . ? C11 C12 H123 109.5 . . ? H121 C12 H123 109.5 . . ? H122 C12 H123 109.5 . . ? C11 C13 C14 109.2(5) . . ? C11 C13 H131 109.8 . . ? C14 C13 H131 109.8 . . ? C11 C13 H132 109.8 . . ? C14 C13 H132 109.8 . . ? H131 C13 H132 108.3 . . ? C13 C14 H141 109.5 . . ? C13 C14 H142 109.5 . . ? H141 C14 H142 109.5 . . ? C13 C14 H143 109.5 . . ? H141 C14 H143 109.5 . . ? H142 C14 H143 109.5 . . ? C24 C21 C27 80.3(6) . . ? C24 C21 C22 113.6(4) . . ? C27 C21 C22 122.8(4) . . ? C24 C21 C29 109.1(7) . . ? C22 C21 C29 98.2(4) . . ? C24 C21 C26 100.5(4) . . ? C22 C21 C26 108.3(3) . . ? C27 C21 C23 97.6(6) . . ? C22 C21 C23 106.3(3) . . ? C29 C21 C23 126.7(7) . . ? C26 C21 C23 118.1(4) . . ? C24 C21 Si2 116.7(4) . . ? C27 C21 Si2 113.2(3) . . ? C22 C21 Si2 108.33(12) . . ? C29 C21 Si2 109.2(7) . . ? C26 C21 Si2 108.8(3) . . ? C23 C21 Si2 106.7(3) . . ? C21 C22 H221 109.5 . . ? C21 C22 H222 109.5 . . ? H221 C22 H222 109.5 . . ? C21 C22 H223 109.5 . . ? H221 C22 H223 109.5 . . ? H222 C22 H223 109.5 . . ? C21 C23 H231 109.5 . . ? C21 C23 H232 109.5 . . ? H231 C23 H232 109.5 . . ? C21 C23 H233 109.5 . . ? H231 C23 H233 109.5 . . ? H232 C23 H233 109.5 . . ? C25 C24 C21 109.1(4) . . ? C25 C24 H241 109.9 . . ? C21 C24 H241 109.9 . . ? C25 C24 H242 109.9 . . ? C21 C24 H242 109.9 . . ? H241 C24 H242 108.3 . . ? C24 C25 H251 109.5 . . ? C24 C25 H252 109.5 . . ? H251 C25 H252 109.5 . . ? C24 C25 H253 109.5 . . ? H251 C25 H253 109.5 . . ? H252 C25 H253 109.5 . . ? C21 C26 H261 109.5 . . ? C21 C26 H262 109.5 . . ? H261 C26 H262 109.5 . . ? C21 C26 H263 109.5 . . ? H261 C26 H263 109.5 . . ? H262 C26 H263 109.5 . . ? C21 C27 C28 109.3(5) . . ? C21 C27 H271 109.8 . . ? C28 C27 H271 109.8 . . ? C21 C27 H272 109.8 . . ? C28 C27 H272 109.8 . . ? H271 C27 H272 108.3 . . ? C27 C28 H281 109.5 . . ? C27 C28 H282 109.5 . . ? H281 C28 H282 109.5 . . ? C27 C28 H283 109.5 . . ? H281 C28 H283 109.5 . . ? H282 C28 H283 109.5 . . ? C30 C29 C21 113.7(6) . . ? C30 C29 H291 108.8 . . ? C21 C29 H291 108.8 . . ? C30 C29 H292 108.8 . . ? C21 C29 H292 108.8 . . ? H291 C29 H292 107.7 . . ? C29 C30 H301 109.5 . . ? C29 C30 H302 109.5 . . ? H301 C30 H302 109.5 . . ? C29 C30 H303 109.5 . . ? H301 C30 H303 109.5 . . ? H302 C30 H303 109.5 . . ? loop_ _geom_torsion_atom_site_label_1 _geom_torsion_atom_site_label_2 _geom_torsion_atom_site_label_3 _geom_torsion_atom_site_label_4 _geom_torsion _geom_torsion_site_symmetry_1 _geom_torsion_site_symmetry_2 _geom_torsion_site_symmetry_3 _geom_torsion_site_symmetry_4 _geom_torsion_publ_flag O2 Si2 O1 Si1 64.16(18) 32 . . . ? O2 Si2 O1 Si1 -54.87(18) . . . . ? C21 Si2 O1 Si1 -175.03(16) . . . . ? O1 Si1 O1 Si2 -63.98(16) 3_665 . . . ? O1 Si1 O1 Si2 54.45(17) 2_655 . . . ? C11 Si1 O1 Si2 175.24(15) . . . . ? O1 Si2 O2 Si2 64.90(18) . . . 33_545 ? O2 Si2 O2 Si2 -54.14(16) 32 . . 33_545 ? C21 Si2 O2 Si2 -175.37(16) . . . 33_545 ? O1 Si1 C11 C13 -33.2(4) 3_665 . . 3_665 ? O1 Si1 C11 C13 -153.2(4) 2_655 . . 3_665 ? O1 Si1 C11 C13 86.8(4) . . . 3_665 ? O1 Si1 C11 C13 86.8(4) 3_665 . . 2_655 ? O1 Si1 C11 C13 -33.2(4) 2_655 . . 2_655 ? O1 Si1 C11 C13 -153.2(4) . . . 2_655 ? O1 Si1 C11 C13 -153.2(4) 3_665 . . . ? O1 Si1 C11 C13 86.8(4) 2_655 . . . ? O1 Si1 C11 C13 -33.2(4) . . . . ? O1 Si1 C11 C12 -46.1(3) 3_665 . . 3_665 ? O1 Si1 C11 C12 -166.1(3) 2_655 . . 3_665 ? O1 Si1 C11 C12 73.9(3) . . . 3_665 ? O1 Si1 C11 C12 73.9(3) 3_665 . . 2_655 ? O1 Si1 C11 C12 -46.1(3) 2_655 . . 2_655 ? O1 Si1 C11 C12 -166.1(3) . . . 2_655 ? O1 Si1 C11 C12 -166.1(3) 3_665 . . . ? O1 Si1 C11 C12 73.9(3) 2_655 . . . ? O1 Si1 C11 C12 -46.1(3) . . . . ? C13 C11 C13 C14 168.0(5) 3_665 . . . ? C13 C11 C13 C14 52.6(16) 2_655 . . . ? C12 C11 C13 C14 176.5(10) 3_665 . . . ? C12 C11 C13 C14 57.9(9) 2_655 . . . ? C12 C11 C13 C14 10(3) . . . . ? Si1 C11 C13 C14 -69.7(10) . . . . ? O1 Si2 C21 C24 -162.2(3) . . . . ? O2 Si2 C21 C24 -42.1(3) 32 . . . ? O2 Si2 C21 C24 78.4(3) . . . . ? O1 Si2 C21 C27 -71.6(6) . . . . ? O2 Si2 C21 C27 48.4(6) 32 . . . ? O2 Si2 C21 C27 169.0(6) . . . . ? O1 Si2 C21 C22 68.03(17) . . . . ? O2 Si2 C21 C22 -171.89(15) 32 . . . ? O2 Si2 C21 C22 -51.37(17) . . . . ? O1 Si2 C21 C29 -37.9(4) . . . . ? O2 Si2 C21 C29 82.2(4) 32 . . . ? O2 Si2 C21 C29 -157.3(4) . . . . ? O1 Si2 C21 C26 -49.5(3) . . . . ? O2 Si2 C21 C26 70.6(3) 32 . . . ? O2 Si2 C21 C26 -168.9(3) . . . . ? O1 Si2 C21 C23 -177.8(3) . . . . ? O2 Si2 C21 C23 -57.7(3) 32 . . . ? O2 Si2 C21 C23 62.8(3) . . . . ? C27 C21 C24 C25 -174.3(7) . . . . ? C22 C21 C24 C25 64.0(7) . . . . ? C29 C21 C24 C25 172.5(7) . . . . ? C26 C21 C24 C25 179.5(7) . . . . ? C23 C21 C24 C25 -4.6(16) . . . . ? Si2 C21 C24 C25 -63.2(7) . . . . ? C24 C21 C27 C28 -87.3(9) . . . . ? C22 C21 C27 C28 24.6(11) . . . . ? C29 C21 C27 C28 68.4(14) . . . . ? C26 C21 C27 C28 75.6(12) . . . . ? C23 C21 C27 C28 -90.5(9) . . . . ? Si2 C21 C27 C28 157.7(6) . . . . ? C24 C21 C29 C30 65.1(13) . . . . ? C27 C21 C29 C30 39.7(9) . . . . ? C22 C21 C29 C30 -176.3(11) . . . . ? C26 C21 C29 C30 26(4) . . . . ? C23 C21 C29 C30 66.2(15) . . . . ? Si2 C21 C29 C30 -63.6(13) . . . . ? _diffrn_measured_fraction_theta_max 0.997 _diffrn_reflns_theta_full 30.00 _diffrn_measured_fraction_theta_full 0.997 _refine_diff_density_max 0.744 _refine_diff_density_min -0.408 _refine_diff_density_rms 0.061 _iucr_refine_instructions_details ; TITL NH235B_0m in R-3c CELL 0.71073 13.2192 13.2192 53.3347 90.000 90.000 120.000 ZERR 6.00 0.0004 0.0004 0.0018 0.000 0.000 0.000 LATT 3 SYMM -Y, X-Y, Z SYMM -X+Y, -X, Z SYMM Y, X, 0.5-Z SYMM X-Y, -Y, 0.5-Z SYMM -X, -X+Y, 0.5-Z SFAC C H O SI UNIT 240 528 72 48 TEMP -173.170 SIZE 0.25 0.26 0.30 ACTA MERG 2 OMIT -2 60.005 OMIT -4 5 15 OMIT -3 7 29 OMIT -2 4 18 OMIT 0 5 4 OMIT -3 8 13 OMIT -1 6 5 L.S. 3 BOND $H CONF FMAP 2 PLAN 4 WGHT 0.0725 12.2905 FVAR 0.05614 1.53794 0.42542 0.27391 0.30067 0.05973 0.07755 SI1 4 0.666667 0.333333 0.282618 10.33333 0.01941 0.01941 = 0.03539 0.00000 0.00000 0.00971 SI2 4 0.745931 0.553217 0.316449 11.00000 0.01572 0.01297 = 0.04164 0.00275 0.00193 0.00684 O1 3 0.717252 0.465021 0.293066 11.00000 0.02945 0.01967 = 0.04275 0.00204 0.00438 0.01122 O2 3 0.627622 0.510573 0.332615 11.00000 0.01929 0.01962 = 0.05020 0.00072 0.00565 0.01007 DELU .0001 .0002 C11 > C30 ISOR .004 .008 C11 > C30 SIMU .004 .008 C26 C29 DFIX 21 .004 C11 C12 C11 C13 C13 C14 C11 1 0.666667 0.333333 0.247643 10.33333 0.04176 0.04176 = 0.03803 0.00000 0.00000 0.02088 PART 1 10.666667 C12 1 0.615297 0.408900 0.238358 10.66667 0.05849 0.06399 = 0.05759 0.02778 -0.00667 0.02878 AFIX 33 H121 2 0.534590 0.375147 0.244261 10.66667 71.00000 H122 2 0.616573 0.411103 0.219990 10.66667 71.00000 H123 2 0.662112 0.488428 0.244929 10.66667 71.00000 AFIX 0 PART 2 10.333333 C13 1 0.643315 0.427834 0.237124 10.33333 0.04763 0.03985 = 0.05326 0.00590 0.00736 0.02213 AFIX 23 H131 2 0.657833 0.435785 0.218826 10.33333 61.00000 H132 2 0.696608 0.503928 0.245092 10.33333 61.00000 AFIX 0 C14 1 0.515917 0.393418 0.242450 10.33333 0.05476 0.06487 = 0.06426 0.02297 0.01351 0.03831 AFIX 33 H141 2 0.500626 0.453595 0.235797 10.33333 71.00000 H142 2 0.502222 0.386205 0.260588 10.33333 71.00000 H143 2 0.463594 0.318486 0.234365 10.33333 71.00000 AFIX 0 PART 0 DFIX 21 .004 C21 C22 C21 C23 C21 C24 C24 C25 DFIX 21 .004 C21 C26 C21 C27 C21 C29 C27 C28 C29 C30 SUMP 1.0 .00001 1.0 3 1.0 4 1.0 5 C21 1 0.799900 0.704124 0.304372 11.00000 0.02860 0.01738 = 0.06051 0.00693 -0.00630 0.00956 C22 1 0.698378 0.707023 0.291074 11.00000 0.04539 0.03158 = 0.08304 0.00702 -0.02181 0.01950 AFIX 33 H221 2 0.725202 0.785775 0.284578 11.00000 71.00000 H222 2 0.634488 0.686011 0.302999 11.00000 71.00000 H223 2 0.670640 0.651133 0.277156 11.00000 71.00000 AFIX 0 PART 1 -31 C23 1 0.830347 0.784975 0.327716 -31.00000 0.06797 0.01153 = 0.07325 -0.00088 -0.02093 0.01098 AFIX 33 H231 2 0.895273 0.786245 0.336861 -31.00000 71.00000 H232 2 0.761964 0.755248 0.338714 -31.00000 71.00000 H233 2 0.852968 0.864320 0.322266 -31.00000 71.00000 AFIX 0 PART 2 31 C24 1 0.864677 0.803314 0.322817 31.00000 0.02849 0.01948 = 0.07389 0.00161 -0.00745 0.00529 AFIX 23 H241 2 0.932684 0.800428 0.329736 31.00000 61.00000 H242 2 0.893630 0.879178 0.314190 31.00000 61.00000 AFIX 0 C25 1 0.782685 0.791924 0.343805 31.00000 0.05724 0.03790 = 0.06565 -0.00284 -0.00244 0.01727 AFIX 33 H251 2 0.823963 0.856193 0.355729 31.00000 71.00000 H252 2 0.755324 0.717249 0.352441 31.00000 71.00000 H253 2 0.715638 0.794951 0.336845 31.00000 71.00000 AFIX 0 C26 1 0.897854 0.733133 0.284771 31.00000 0.02409 0.02054 = 0.04456 0.01402 -0.01047 -0.00986 AFIX 33 H261 2 0.867694 0.674116 0.271462 31.00000 71.00000 H262 2 0.964201 0.733263 0.293001 31.00000 71.00000 H263 2 0.923373 0.810293 0.277502 31.00000 71.00000 AFIX 0 PART 3 41 C27 1 0.923099 0.759825 0.293235 41.00000 0.03851 0.03576 = 0.06803 0.01588 0.00708 0.01205 AFIX 23 H271 2 0.933184 0.699930 0.284245 41.00000 61.00000 H272 2 0.981852 0.792476 0.306831 41.00000 61.00000 AFIX 0 C28 1 0.941264 0.858503 0.274808 41.00000 0.03859 0.03026 = 0.04814 0.00351 -0.00161 0.00907 AFIX 33 H281 2 1.021333 0.897041 0.268319 41.00000 71.00000 H282 2 0.927874 0.915791 0.283633 41.00000 71.00000 H283 2 0.886047 0.824946 0.260845 41.00000 71.00000 AFIX 0 PART 4 51 C29 1 0.878456 0.724787 0.281094 51.00000 0.04562 0.04284 = 0.05125 0.01443 -0.00336 0.01343 AFIX 23 H291 2 0.832565 0.665025 0.268278 51.00000 61.00000 H292 2 0.901026 0.802222 0.273865 51.00000 61.00000 AFIX 0 C30 1 0.989064 0.719845 0.286859 51.00000 0.05360 0.06129 = 0.09628 0.03497 0.03037 0.03409 AFIX 33 H301 2 1.035663 0.736073 0.271545 51.00000 71.00000 H302 2 0.967609 0.641921 0.293106 51.00000 71.00000 H303 2 1.034898 0.778369 0.299624 51.00000 71.00000 HKLF 4 END ; #---------------------------------------------------------------------------- data_4c_NH260 _audit_author_name 'Ferdinand Belaj' _audit_creation_method 'manual edited SHELXL-97 .cif file' _chemical_compound_source 'synthetical product' _chemical_name_systematic ; octakis(1,1-dimethylbutyl)octasilsesquioxane ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety 'C48 H104 O12 Si8' _chemical_formula_sum 'C48 H104 O12 Si8' _chemical_formula_weight 1098.03 loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source 'C' 'C' 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'H' 'H' 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'O' 'O' 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'Si' 'Si' 0.0817 0.0704 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting triclinic _symmetry_space_group_name_H-M 'P -1' _symmetry_space_group_name_Hall '-P 1' loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, -y, -z' _cell_length_a 10.8944(4) _cell_length_b 12.6042(4) _cell_length_c 13.4936(5) _cell_angle_alpha 68.8952(11) _cell_angle_beta 87.8745(12) _cell_angle_gamma 66.4831(11) _cell_volume 1572.67(10) _cell_formula_units_Z 1 _cell_measurement_temperature 100(2) _cell_measurement_reflns_used 9989 _cell_measurement_theta_min 3.25 _cell_measurement_theta_max 31.13 _exptl_crystal_description 'block' _exptl_crystal_colour 'colourless' _exptl_crystal_size_min 0.36 _exptl_crystal_size_mid 0.36 _exptl_crystal_size_max 0.38 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.159 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 600 _exptl_absorpt_coefficient_mu 0.222 _exptl_absorpt_correction_type 'multi-scan' _exptl_absorpt_correction_T_min 0.6812 _exptl_absorpt_correction_T_max 0.7462 _exptl_absorpt_process_details 'Bruker SADABS' _exptl_special_details ; ? ; _diffrn_ambient_temperature 100(2) _diffrn_measurement_device_type 'Bruker APEX-II CCD' _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_type 'MoK\a' _diffrn_radiation_monochromator 'graphite' _diffrn_radiation_wavelength 0.71073 _diffrn_measurement_method '\f and \w scans' _diffrn_detector_area_resol_mean ? _diffrn_standards_number 0 _diffrn_standards_interval_count ? _diffrn_standards_decay_% ? _diffrn_reflns_number 26387 _diffrn_reflns_av_R_equivalents 0.0168 _diffrn_reflns_av_sigmaI/netI 0.0159 _diffrn_reflns_limit_h_min -15 _diffrn_reflns_limit_h_max 15 _diffrn_reflns_limit_k_min -17 _diffrn_reflns_limit_k_max 17 _diffrn_reflns_limit_l_min -18 _diffrn_reflns_limit_l_max 18 _diffrn_reflns_theta_min 1.98 _diffrn_reflns_theta_max 30.00 _reflns_number_total 9065 _reflns_number_gt 8236 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'Bruker APEX2' _computing_cell_refinement 'Bruker SAINT' _computing_data_reduction 'Bruker SAINT' _computing_structure_solution 'SHELXS-97 (Sheldrick, 2008)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 2008)' _computing_molecular_graphics 'modified ORTEP (Johnson, 1965)' _computing_publication_material 'SHELXL-97 (Sheldrick, 2008)' _refine_special_details ; Refinement of F^2^ against ALL reflections. The weighted R-factor wR and goodness of fit S are based on F^2^, conventional R-factors R are based on F, with F set to zero for negative F^2^. The threshold expression of F^2^ > 2sigma(F^2^) is used only for calculating R-factors(gt) etc. and is not relevant to the choice of reflections for refinement. R-factors based on F^2^ are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger. The non-hydrogen atoms were refined with anisotropic displacement parameters without any constraints. The H atoms of the CH~2~ groups were refined with common isotropic displacement parameters for the H atoms of the same group and idealized geometry with approximately tetrahedral angles and C-H distances of 0.99 \%A (AFIX 23 of SHELXL-97). The H atoms of the methyl groups were refined with common isotropic displacement parameters for the H atoms of the same group and idealized geometries with tetrahedral angles, enabling rotation around the C-C bond, and C-H distances of 0.98 \%A (AFIX 137 of SHELXL-97). ; _refine_ls_structure_factor_coef Fsqd _refine_ls_matrix_type full _refine_ls_weighting_scheme calc _refine_ls_weighting_details 'calc w=1/[\s^2^(Fo^2^)+(0.0397P)^2^+0.5414P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment refU _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 9065 _refine_ls_number_parameters 339 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0300 _refine_ls_R_factor_gt 0.0264 _refine_ls_wR_factor_ref 0.0783 _refine_ls_wR_factor_gt 0.0742 _refine_ls_goodness_of_fit_ref 1.055 _refine_ls_restrained_S_all 1.055 _refine_ls_shift/su_max 0.001 _refine_ls_shift/su_mean 0.000 loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_occupancy _atom_site_symmetry_multiplicity _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group Si1 Si 0.59859(2) 0.61403(2) 0.326282(17) 0.00906(5) Uani 1 1 d . . . O1 O 0.66028(6) 0.46547(6) 0.34929(5) 0.01360(12) Uani 1 1 d . . . Si2 Si 0.65442(2) 0.33197(2) 0.416723(17) 0.00933(5) Uani 1 1 d . . . O2 O 0.70818(6) 0.28909(6) 0.54155(5) 0.01446(12) Uani 1 1 d . . . Si3 Si 0.70694(2) 0.31801(2) 0.649487(17) 0.00941(5) Uani 1 1 d . . . O3 O 0.72229(6) 0.44856(6) 0.62050(5) 0.01388(12) Uani 1 1 d . . . Si4 Si 0.65101(2) 0.59944(2) 0.559612(17) 0.00952(5) Uani 1 1 d . . . O4 O 0.63865(7) 0.63363(6) 0.43117(5) 0.01456(12) Uani 1 1 d . . . O5 O 0.43537(6) 0.66959(6) 0.30345(5) 0.01391(12) Uani 1 1 d . . . O6 O 0.49945(6) 0.34796(6) 0.40660(5) 0.01400(12) Uani 1 1 d . . . C11 C 0.66943(9) 0.69300(8) 0.20812(7) 0.01384(15) Uani 1 1 d . . . C12 C 0.66449(10) 0.81750(9) 0.20744(8) 0.01973(18) Uani 1 1 d . . . H121 H 0.7217 0.7986 0.2722 0.026(2) Uiso 1 1 calc R . . H122 H 0.7059 0.8527 0.1446 0.026(2) Uiso 1 1 calc R . . C13 C 0.52677(12) 0.91780(10) 0.20423(10) 0.0267(2) Uani 1 1 d . . . H131 H 0.4837 0.8844 0.2667 0.038(3) Uiso 1 1 calc R . . H132 H 0.4691 0.9401 0.1386 0.038(3) Uiso 1 1 calc R . . C14 C 0.53584(17) 1.03503(12) 0.20571(13) 0.0435(3) Uani 1 1 d . . . H141 H 0.5887 1.0143 0.2725 0.060(3) Uiso 1 1 calc R . . H142 H 0.4449 1.0984 0.2010 0.060(3) Uiso 1 1 calc R . . H143 H 0.5797 1.0677 0.1447 0.060(3) Uiso 1 1 calc R . . C15 C 0.59280(11) 0.71448(10) 0.10411(7) 0.02115(18) Uani 1 1 d . . . H151 H 0.6327 0.7522 0.0425 0.032(2) Uiso 1 1 calc R . . H152 H 0.4978 0.7705 0.0987 0.032(2) Uiso 1 1 calc R . . H153 H 0.5992 0.6343 0.1050 0.032(2) Uiso 1 1 calc R . . C16 C 0.81882(10) 0.60609(10) 0.21455(9) 0.0259(2) Uani 1 1 d . . . H161 H 0.8251 0.5283 0.2098 0.036(2) Uiso 1 1 calc R . . H162 H 0.8674 0.5872 0.2827 0.036(2) Uiso 1 1 calc R . . H163 H 0.8590 0.6475 0.1552 0.036(2) Uiso 1 1 calc R . . C21 C 0.76195(8) 0.20693(8) 0.36880(7) 0.01274(15) Uani 1 1 d . . . C22 C 0.70063(9) 0.22100(8) 0.26115(7) 0.01527(16) Uani 1 1 d . . . H221 H 0.7593 0.1478 0.2444 0.021(2) Uiso 1 1 calc R . . H222 H 0.6119 0.2170 0.2712 0.021(2) Uiso 1 1 calc R . . C23 C 0.68024(11) 0.33846(10) 0.16340(7) 0.02262(19) Uani 1 1 d . . . H231 H 0.7668 0.3469 0.1535 0.030(3) Uiso 1 1 calc R . . H232 H 0.6145 0.4129 0.1751 0.030(3) Uiso 1 1 calc R . . C24 C 0.62866(13) 0.33174(12) 0.06301(8) 0.0296(2) Uani 1 1 d . . . H241 H 0.6949 0.2592 0.0505 0.044(3) Uiso 1 1 calc R . . H242 H 0.6152 0.4081 0.0013 0.044(3) Uiso 1 1 calc R . . H243 H 0.5428 0.3236 0.0729 0.044(3) Uiso 1 1 calc R . . C25 C 0.77104(11) 0.08116(8) 0.45257(8) 0.02085(18) Uani 1 1 d . . . H251 H 0.8256 0.0132 0.4292 0.029(2) Uiso 1 1 calc R . . H252 H 0.6802 0.0836 0.4597 0.029(2) Uiso 1 1 calc R . . H253 H 0.8130 0.0669 0.5218 0.029(2) Uiso 1 1 calc R . . C26 C 0.90510(9) 0.20281(10) 0.36188(8) 0.02016(18) Uani 1 1 d . . . H261 H 0.9616 0.1351 0.3390 0.028(2) Uiso 1 1 calc R . . H262 H 0.9442 0.1882 0.4323 0.028(2) Uiso 1 1 calc R . . H263 H 0.9006 0.2826 0.3099 0.028(2) Uiso 1 1 calc R . . C31 C 0.84943(8) 0.19016(8) 0.75177(7) 0.01355(15) Uani 1 1 d . . . C32 C 0.83041(10) 0.06756(9) 0.78221(7) 0.01867(17) Uani 1 1 d . . . H321 H 0.7408 0.0816 0.8074 0.033(3) Uiso 1 1 calc R . . H322 H 0.8288 0.0501 0.7165 0.033(3) Uiso 1 1 calc R . . C33 C 0.93555(12) -0.04866(10) 0.86731(9) 0.0302(2) Uani 1 1 d . . . H331 H 1.0251 -0.0671 0.8414 0.050(3) Uiso 1 1 calc R . . H332 H 0.9402 -0.0320 0.9331 0.050(3) Uiso 1 1 calc R . . C34 C 0.90337(15) -0.16216(11) 0.89424(11) 0.0387(3) Uani 1 1 d . . . H341 H 0.8152 -0.1448 0.9207 0.058(3) Uiso 1 1 calc R . . H342 H 0.9729 -0.2342 0.9495 0.058(3) Uiso 1 1 calc R . . H343 H 0.9013 -0.1805 0.8298 0.058(3) Uiso 1 1 calc R . . C35 C 0.84658(13) 0.22631(11) 0.84955(8) 0.0301(2) Uani 1 1 d . . . H351 H 0.9240 0.1630 0.9029 0.044(3) Uiso 1 1 calc R . . H352 H 0.7628 0.2313 0.8809 0.044(3) Uiso 1 1 calc R . . H353 H 0.8511 0.3076 0.8271 0.044(3) Uiso 1 1 calc R . . C36 C 0.98293(10) 0.17804(10) 0.70489(9) 0.0260(2) Uani 1 1 d . . . H361 H 0.9896 0.2585 0.6816 0.040(2) Uiso 1 1 calc R . . H362 H 0.9856 0.1534 0.6435 0.040(2) Uiso 1 1 calc R . . H363 H 1.0587 0.1145 0.7597 0.040(2) Uiso 1 1 calc R . . C41 C 0.75495(9) 0.67077(9) 0.59507(7) 0.01619(16) Uani 1 1 d . . . C42 C 0.81538(10) 0.60668(9) 0.71421(7) 0.01862(17) Uani 1 1 d . . . H421 H 0.8761 0.5186 0.7277 0.024(2) Uiso 1 1 calc R . . H422 H 0.8720 0.6472 0.7256 0.024(2) Uiso 1 1 calc R . . C43 C 0.71836(10) 0.60692(10) 0.79850(8) 0.02079(18) Uani 1 1 d . . . H431 H 0.6672 0.5588 0.7940 0.030(3) Uiso 1 1 calc R . . H432 H 0.6530 0.6938 0.7844 0.030(3) Uiso 1 1 calc R . . C44 C 0.79478(13) 0.54930(12) 0.91090(8) 0.0299(2) Uani 1 1 d . . . H441 H 0.8566 0.4621 0.9261 0.035(2) Uiso 1 1 calc R . . H442 H 0.7303 0.5526 0.9636 0.035(2) Uiso 1 1 calc R . . H443 H 0.8463 0.5962 0.9151 0.035(2) Uiso 1 1 calc R . . C45 C 0.67058(14) 0.81176(10) 0.56577(9) 0.0300(2) Uani 1 1 d . . . H451 H 0.7267 0.8489 0.5827 0.041(3) Uiso 1 1 calc R . . H452 H 0.5936 0.8242 0.6069 0.041(3) Uiso 1 1 calc R . . H453 H 0.6378 0.8519 0.4891 0.041(3) Uiso 1 1 calc R . . C46 C 0.87520(13) 0.65242(15) 0.52927(9) 0.0347(3) Uani 1 1 d . . . H461 H 0.8416 0.6947 0.4527 0.046(3) Uiso 1 1 calc R . . H462 H 0.9279 0.5630 0.5460 0.046(3) Uiso 1 1 calc R . . H463 H 0.9325 0.6879 0.5472 0.046(3) Uiso 1 1 calc R . . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 Si1 0.00957(10) 0.00960(10) 0.00815(9) -0.00293(7) 0.00107(7) -0.00444(8) O1 0.0156(3) 0.0104(3) 0.0140(3) -0.0045(2) 0.0036(2) -0.0049(2) Si2 0.00992(10) 0.00906(10) 0.00854(10) -0.00376(8) 0.00071(7) -0.00304(8) O2 0.0167(3) 0.0148(3) 0.0101(3) -0.0052(2) -0.0008(2) -0.0040(2) Si3 0.00879(10) 0.00988(10) 0.00796(9) -0.00274(8) -0.00038(7) -0.00275(8) O3 0.0131(3) 0.0114(3) 0.0156(3) -0.0037(2) -0.0015(2) -0.0044(2) Si4 0.00987(10) 0.01063(10) 0.00926(10) -0.00391(8) 0.00055(7) -0.00520(8) O4 0.0190(3) 0.0175(3) 0.0104(3) -0.0054(2) 0.0011(2) -0.0104(2) O5 0.0101(3) 0.0162(3) 0.0127(3) -0.0034(2) 0.0010(2) -0.0046(2) O6 0.0113(3) 0.0156(3) 0.0169(3) -0.0086(2) 0.0021(2) -0.0052(2) C11 0.0148(4) 0.0149(4) 0.0120(3) -0.0037(3) 0.0031(3) -0.0076(3) C12 0.0248(4) 0.0191(4) 0.0180(4) -0.0037(3) 0.0021(3) -0.0147(4) C13 0.0315(5) 0.0171(4) 0.0327(5) -0.0094(4) 0.0030(4) -0.0111(4) C14 0.0648(9) 0.0220(5) 0.0486(8) -0.0141(5) 0.0046(7) -0.0218(6) C15 0.0312(5) 0.0243(4) 0.0112(4) -0.0060(3) 0.0036(3) -0.0153(4) C16 0.0176(4) 0.0259(5) 0.0283(5) -0.0053(4) 0.0104(4) -0.0084(4) C21 0.0129(3) 0.0118(3) 0.0120(3) -0.0052(3) 0.0011(3) -0.0031(3) C22 0.0175(4) 0.0158(4) 0.0144(4) -0.0085(3) 0.0022(3) -0.0061(3) C23 0.0328(5) 0.0241(5) 0.0133(4) -0.0054(3) -0.0002(3) -0.0152(4) C24 0.0413(6) 0.0346(6) 0.0142(4) -0.0097(4) -0.0003(4) -0.0162(5) C25 0.0277(5) 0.0108(4) 0.0186(4) -0.0046(3) 0.0022(3) -0.0035(3) C26 0.0126(4) 0.0246(4) 0.0230(4) -0.0132(4) 0.0019(3) -0.0037(3) C31 0.0121(3) 0.0132(4) 0.0113(3) -0.0030(3) -0.0021(3) -0.0025(3) C32 0.0183(4) 0.0139(4) 0.0163(4) 0.0003(3) -0.0023(3) -0.0044(3) C33 0.0322(6) 0.0163(4) 0.0264(5) 0.0022(4) -0.0086(4) -0.0029(4) C34 0.0473(7) 0.0174(5) 0.0349(6) 0.0033(4) 0.0033(5) -0.0088(5) C35 0.0401(6) 0.0234(5) 0.0169(4) -0.0079(4) -0.0123(4) -0.0021(4) C36 0.0115(4) 0.0227(5) 0.0320(5) -0.0008(4) 0.0002(4) -0.0041(3) C41 0.0198(4) 0.0217(4) 0.0134(4) -0.0068(3) 0.0019(3) -0.0146(3) C42 0.0191(4) 0.0248(4) 0.0158(4) -0.0090(3) 0.0001(3) -0.0114(4) C43 0.0230(4) 0.0233(4) 0.0161(4) -0.0087(3) 0.0027(3) -0.0086(4) C44 0.0396(6) 0.0360(6) 0.0159(4) -0.0101(4) 0.0011(4) -0.0170(5) C45 0.0492(7) 0.0189(5) 0.0253(5) -0.0029(4) -0.0071(5) -0.0213(5) C46 0.0317(6) 0.0700(9) 0.0247(5) -0.0228(6) 0.0125(4) -0.0389(6) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag Si1 O4 1.6243(7) . ? Si1 O5 1.6244(6) . ? Si1 O1 1.6269(7) . ? Si1 C11 1.8727(8) . ? O1 Si2 1.6255(6) . ? Si2 O6 1.6234(7) . ? Si2 O2 1.6239(6) . ? Si2 C21 1.8651(9) . ? O2 Si3 1.6222(7) . ? Si3 O5 1.6237(6) 2_666 ? Si3 O3 1.6248(7) . ? Si3 C31 1.8634(8) . ? O3 Si4 1.6242(7) . ? Si4 O6 1.6215(6) 2_666 ? Si4 O4 1.6250(6) . ? Si4 C41 1.8660(9) . ? O5 Si3 1.6237(6) 2_666 ? O6 Si4 1.6215(6) 2_666 ? C11 C15 1.5405(13) . ? C11 C16 1.5413(13) . ? C11 C12 1.5452(13) . ? C12 C13 1.5175(15) . ? C12 H121 0.99 . ? C12 H122 0.99 . ? C13 C14 1.5269(16) . ? C13 H131 0.99 . ? C13 H132 0.99 . ? C14 H141 0.98 . ? C14 H142 0.98 . ? C14 H143 0.98 . ? C15 H151 0.98 . ? C15 H152 0.98 . ? C15 H153 0.98 . ? C16 H161 0.98 . ? C16 H162 0.98 . ? C16 H163 0.98 . ? C21 C26 1.5400(12) . ? C21 C22 1.5426(12) . ? C21 C25 1.5469(12) . ? C22 C23 1.5277(13) . ? C22 H221 0.99 . ? C22 H222 0.99 . ? C23 C24 1.5282(14) . ? C23 H231 0.99 . ? C23 H232 0.99 . ? C24 H241 0.98 . ? C24 H242 0.98 . ? C24 H243 0.98 . ? C25 H251 0.98 . ? C25 H252 0.98 . ? C25 H253 0.98 . ? C26 H261 0.98 . ? C26 H262 0.98 . ? C26 H263 0.98 . ? C31 C36 1.5371(13) . ? C31 C35 1.5389(13) . ? C31 C32 1.5465(13) . ? C32 C33 1.5243(13) . ? C32 H321 0.99 . ? C32 H322 0.99 . ? C33 C34 1.5225(18) . ? C33 H331 0.99 . ? C33 H332 0.99 . ? C34 H341 0.98 . ? C34 H342 0.98 . ? C34 H343 0.98 . ? C35 H351 0.98 . ? C35 H352 0.98 . ? C35 H353 0.98 . ? C36 H361 0.98 . ? C36 H362 0.98 . ? C36 H363 0.98 . ? C41 C45 1.5417(15) . ? C41 C46 1.5420(14) . ? C41 C42 1.5458(12) . ? C42 C43 1.5237(13) . ? C42 H421 0.99 . ? C42 H422 0.99 . ? C43 C44 1.5293(14) . ? C43 H431 0.99 . ? C43 H432 0.99 . ? C44 H441 0.98 . ? C44 H442 0.98 . ? C44 H443 0.98 . ? C45 H451 0.98 . ? C45 H452 0.98 . ? C45 H453 0.98 . ? C46 H461 0.98 . ? C46 H462 0.98 . ? C46 H463 0.98 . ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag O4 Si1 O5 109.05(3) . . ? O4 Si1 O1 109.36(3) . . ? O5 Si1 O1 108.25(3) . . ? O4 Si1 C11 110.08(4) . . ? O5 Si1 C11 111.01(4) . . ? O1 Si1 C11 109.05(4) . . ? Si2 O1 Si1 146.58(4) . . ? O6 Si2 O2 109.41(3) . . ? O6 Si2 O1 109.14(3) . . ? O2 Si2 O1 108.63(4) . . ? O6 Si2 C21 109.00(4) . . ? O2 Si2 C21 108.14(4) . . ? O1 Si2 C21 112.48(4) . . ? Si3 O2 Si2 151.04(4) . . ? O2 Si3 O5 109.01(4) . 2_666 ? O2 Si3 O3 109.14(3) . . ? O5 Si3 O3 109.43(3) 2_666 . ? O2 Si3 C31 110.44(4) . . ? O5 Si3 C31 109.74(4) 2_666 . ? O3 Si3 C31 109.07(4) . . ? Si4 O3 Si3 146.06(4) . . ? O6 Si4 O3 109.12(3) 2_666 . ? O6 Si4 O4 108.62(3) 2_666 . ? O3 Si4 O4 108.83(3) . . ? O6 Si4 C41 110.88(4) 2_666 . ? O3 Si4 C41 109.89(4) . . ? O4 Si4 C41 109.45(4) . . ? Si1 O4 Si4 151.20(4) . . ? Si3 O5 Si1 148.34(4) 2_666 . ? Si4 O6 Si2 148.33(4) 2_666 . ? C15 C11 C16 108.71(8) . . ? C15 C11 C12 110.58(7) . . ? C16 C11 C12 107.42(8) . . ? C15 C11 Si1 109.55(6) . . ? C16 C11 Si1 108.22(6) . . ? C12 C11 Si1 112.25(6) . . ? C13 C12 C11 117.16(8) . . ? C13 C12 H121 108.0 . . ? C11 C12 H121 108.0 . . ? C13 C12 H122 108.0 . . ? C11 C12 H122 108.0 . . ? H121 C12 H122 107.3 . . ? C12 C13 C14 112.03(10) . . ? C12 C13 H131 109.2 . . ? C14 C13 H131 109.2 . . ? C12 C13 H132 109.2 . . ? C14 C13 H132 109.2 . . ? H131 C13 H132 107.9 . . ? C13 C14 H141 109.5 . . ? C13 C14 H142 109.5 . . ? H141 C14 H142 109.5 . . ? C13 C14 H143 109.5 . . ? H141 C14 H143 109.5 . . ? H142 C14 H143 109.5 . . ? C11 C15 H151 109.5 . . ? C11 C15 H152 109.5 . . ? H151 C15 H152 109.5 . . ? C11 C15 H153 109.5 . . ? H151 C15 H153 109.5 . . ? H152 C15 H153 109.5 . . ? C11 C16 H161 109.5 . . ? C11 C16 H162 109.5 . . ? H161 C16 H162 109.5 . . ? C11 C16 H163 109.5 . . ? H161 C16 H163 109.5 . . ? H162 C16 H163 109.5 . . ? C26 C21 C22 111.01(7) . . ? C26 C21 C25 108.61(7) . . ? C22 C21 C25 106.85(7) . . ? C26 C21 Si2 110.11(6) . . ? C22 C21 Si2 112.82(6) . . ? C25 C21 Si2 107.23(6) . . ? C23 C22 C21 117.90(8) . . ? C23 C22 H221 107.8 . . ? C21 C22 H221 107.8 . . ? C23 C22 H222 107.8 . . ? C21 C22 H222 107.8 . . ? H221 C22 H222 107.2 . . ? C22 C23 C24 110.52(9) . . ? C22 C23 H231 109.5 . . ? C24 C23 H231 109.5 . . ? C22 C23 H232 109.5 . . ? C24 C23 H232 109.5 . . ? H231 C23 H232 108.1 . . ? C23 C24 H241 109.5 . . ? C23 C24 H242 109.5 . . ? H241 C24 H242 109.5 . . ? C23 C24 H243 109.5 . . ? H241 C24 H243 109.5 . . ? H242 C24 H243 109.5 . . ? C21 C25 H251 109.5 . . ? C21 C25 H252 109.5 . . ? H251 C25 H252 109.5 . . ? C21 C25 H253 109.5 . . ? H251 C25 H253 109.5 . . ? H252 C25 H253 109.5 . . ? C21 C26 H261 109.5 . . ? C21 C26 H262 109.5 . . ? H261 C26 H262 109.5 . . ? C21 C26 H263 109.5 . . ? H261 C26 H263 109.5 . . ? H262 C26 H263 109.5 . . ? C36 C31 C35 109.44(9) . . ? C36 C31 C32 111.02(8) . . ? C35 C31 C32 110.97(8) . . ? C36 C31 Si3 108.95(6) . . ? C35 C31 Si3 107.79(6) . . ? C32 C31 Si3 108.58(6) . . ? C33 C32 C31 116.88(8) . . ? C33 C32 H321 108.1 . . ? C31 C32 H321 108.1 . . ? C33 C32 H322 108.1 . . ? C31 C32 H322 108.1 . . ? H321 C32 H322 107.3 . . ? C34 C33 C32 112.27(10) . . ? C34 C33 H331 109.1 . . ? C32 C33 H331 109.1 . . ? C34 C33 H332 109.1 . . ? C32 C33 H332 109.1 . . ? H331 C33 H332 107.9 . . ? C33 C34 H341 109.5 . . ? C33 C34 H342 109.5 . . ? H341 C34 H342 109.5 . . ? C33 C34 H343 109.5 . . ? H341 C34 H343 109.5 . . ? H342 C34 H343 109.5 . . ? C31 C35 H351 109.5 . . ? C31 C35 H352 109.5 . . ? H351 C35 H352 109.5 . . ? C31 C35 H353 109.5 . . ? H351 C35 H353 109.5 . . ? H352 C35 H353 109.5 . . ? C31 C36 H361 109.5 . . ? C31 C36 H362 109.5 . . ? H361 C36 H362 109.5 . . ? C31 C36 H363 109.5 . . ? H361 C36 H363 109.5 . . ? H362 C36 H363 109.5 . . ? C45 C41 C46 109.02(9) . . ? C45 C41 C42 110.48(8) . . ? C46 C41 C42 106.58(8) . . ? C45 C41 Si4 110.05(7) . . ? C46 C41 Si4 107.70(7) . . ? C42 C41 Si4 112.85(6) . . ? C43 C42 C41 118.05(8) . . ? C43 C42 H421 107.8 . . ? C41 C42 H421 107.8 . . ? C43 C42 H422 107.8 . . ? C41 C42 H422 107.8 . . ? H421 C42 H422 107.1 . . ? C42 C43 C44 110.87(9) . . ? C42 C43 H431 109.5 . . ? C44 C43 H431 109.5 . . ? C42 C43 H432 109.5 . . ? C44 C43 H432 109.5 . . ? H431 C43 H432 108.1 . . ? C43 C44 H441 109.5 . . ? C43 C44 H442 109.5 . . ? H441 C44 H442 109.5 . . ? C43 C44 H443 109.5 . . ? H441 C44 H443 109.5 . . ? H442 C44 H443 109.5 . . ? C41 C45 H451 109.5 . . ? C41 C45 H452 109.5 . . ? H451 C45 H452 109.5 . . ? C41 C45 H453 109.5 . . ? H451 C45 H453 109.5 . . ? H452 C45 H453 109.5 . . ? C41 C46 H461 109.5 . . ? C41 C46 H462 109.5 . . ? H461 C46 H462 109.5 . . ? C41 C46 H463 109.5 . . ? H461 C46 H463 109.5 . . ? H462 C46 H463 109.5 . . ? loop_ _geom_torsion_atom_site_label_1 _geom_torsion_atom_site_label_2 _geom_torsion_atom_site_label_3 _geom_torsion_atom_site_label_4 _geom_torsion _geom_torsion_site_symmetry_1 _geom_torsion_site_symmetry_2 _geom_torsion_site_symmetry_3 _geom_torsion_site_symmetry_4 _geom_torsion_publ_flag O4 Si1 O1 Si2 68.18(9) . . . . ? O5 Si1 O1 Si2 -50.52(9) . . . . ? C11 Si1 O1 Si2 -171.41(8) . . . . ? Si1 O1 Si2 O6 50.74(9) . . . . ? Si1 O1 Si2 O2 -68.49(9) . . . . ? Si1 O1 Si2 C21 171.84(7) . . . . ? O6 Si2 O2 Si3 -69.91(10) . . . . ? O1 Si2 O2 Si3 49.14(10) . . . . ? C21 Si2 O2 Si3 171.48(9) . . . . ? Si2 O2 Si3 O5 69.89(10) . . . 2_666 ? Si2 O2 Si3 O3 -49.57(10) . . . . ? Si2 O2 Si3 C31 -169.47(9) . . . . ? O2 Si3 O3 Si4 69.59(8) . . . . ? O5 Si3 O3 Si4 -49.62(9) 2_666 . . . ? C31 Si3 O3 Si4 -169.68(7) . . . . ? Si3 O3 Si4 O6 49.31(9) . . . 2_666 ? Si3 O3 Si4 O4 -69.07(8) . . . . ? Si3 O3 Si4 C41 171.09(7) . . . . ? O5 Si1 O4 Si4 70.94(10) . . . . ? O1 Si1 O4 Si4 -47.26(10) . . . . ? C11 Si1 O4 Si4 -167.05(9) . . . . ? O6 Si4 O4 Si1 -71.10(10) 2_666 . . . ? O3 Si4 O4 Si1 47.60(10) . . . . ? C41 Si4 O4 Si1 167.71(9) . . . . ? O4 Si1 O5 Si3 -44.51(10) . . . 2_666 ? O1 Si1 O5 Si3 74.38(9) . . . 2_666 ? C11 Si1 O5 Si3 -165.96(8) . . . 2_666 ? O2 Si2 O6 Si4 44.88(9) . . . 2_666 ? O1 Si2 O6 Si4 -73.86(9) . . . 2_666 ? C21 Si2 O6 Si4 162.94(8) . . . 2_666 ? O4 Si1 C11 C15 -160.30(6) . . . . ? O5 Si1 C11 C15 -39.46(7) . . . . ? O1 Si1 C11 C15 79.72(7) . . . . ? O4 Si1 C11 C16 81.31(7) . . . . ? O5 Si1 C11 C16 -157.84(7) . . . . ? O1 Si1 C11 C16 -38.66(8) . . . . ? O4 Si1 C11 C12 -37.05(7) . . . . ? O5 Si1 C11 C12 83.79(7) . . . . ? O1 Si1 C11 C12 -157.03(6) . . . . ? C15 C11 C12 C13 63.01(11) . . . . ? C16 C11 C12 C13 -178.51(9) . . . . ? Si1 C11 C12 C13 -59.66(10) . . . . ? C11 C12 C13 C14 179.06(10) . . . . ? O6 Si2 C21 C26 171.74(6) . . . . ? O2 Si2 C21 C26 -69.39(7) . . . . ? O1 Si2 C21 C26 50.57(7) . . . . ? O6 Si2 C21 C22 47.11(7) . . . . ? O2 Si2 C21 C22 165.97(6) . . . . ? O1 Si2 C21 C22 -74.07(7) . . . . ? O6 Si2 C21 C25 -70.26(7) . . . . ? O2 Si2 C21 C25 48.60(7) . . . . ? O1 Si2 C21 C25 168.56(6) . . . . ? C26 C21 C22 C23 -61.71(10) . . . . ? C25 C21 C22 C23 -179.97(8) . . . . ? Si2 C21 C22 C23 62.43(9) . . . . ? C21 C22 C23 C24 175.81(8) . . . . ? O2 Si3 C31 C36 58.60(8) . . . . ? O5 Si3 C31 C36 178.80(7) 2_666 . . . ? O3 Si3 C31 C36 -61.34(7) . . . . ? O2 Si3 C31 C35 177.28(7) . . . . ? O5 Si3 C31 C35 -62.53(8) 2_666 . . . ? O3 Si3 C31 C35 57.34(8) . . . . ? O2 Si3 C31 C32 -62.44(7) . . . . ? O5 Si3 C31 C32 57.76(7) 2_666 . . . ? O3 Si3 C31 C32 177.62(6) . . . . ? C36 C31 C32 C33 61.56(11) . . . . ? C35 C31 C32 C33 -60.39(11) . . . . ? Si3 C31 C32 C33 -178.69(8) . . . . ? C31 C32 C33 C34 177.52(10) . . . . ? O6 Si4 C41 C45 -42.77(8) 2_666 . . . ? O3 Si4 C41 C45 -163.50(7) . . . . ? O4 Si4 C41 C45 77.04(7) . . . . ? O6 Si4 C41 C46 -161.50(7) 2_666 . . . ? O3 Si4 C41 C46 77.77(8) . . . . ? O4 Si4 C41 C46 -41.69(8) . . . . ? O6 Si4 C41 C42 81.14(7) 2_666 . . . ? O3 Si4 C41 C42 -39.59(8) . . . . ? O4 Si4 C41 C42 -159.05(6) . . . . ? C45 C41 C42 C43 63.48(11) . . . . ? C46 C41 C42 C43 -178.21(9) . . . . ? Si4 C41 C42 C43 -60.19(10) . . . . ? C41 C42 C43 C44 -175.37(9) . . . . ? _diffrn_measured_fraction_theta_max 0.987 _diffrn_reflns_theta_full 30.00 _diffrn_measured_fraction_theta_full 0.987 _refine_diff_density_max 0.519 _refine_diff_density_min -0.365 _refine_diff_density_rms 0.047 _iucr_refine_instructions_details ; TITL NH260_0m in P-1 N.Hurkes [C3H7-C(CH3)2-]8Si8O12 (T8) farblos 100K CELL 0.71073 10.8944 12.6042 13.4936 68.8952 87.8745 66.4831 ZERR 1.00 0.0004 0.0004 0.0005 0.0011 0.0012 0.0011 LATT 1 SFAC C H O SI UNIT 48 104 12 8 TEMP -173.140 ACTA MERG 2 OMIT -2 60.005 OMIT -4 0 1 OMIT -5 -3 1 L.S. 4 BOND $H CONF FMAP 2 PLAN 20 WGHT 0.0397 0.5414 FVAR 0.19793 0.02572 0.02088 0.03266 0.02442 0.03783 0.03016 FVAR 0.04968 0.02988 0.06005 0.04414 0.05769 0.03543 0.03202 FVAR 0.02949 0.04449 0.04096 0.03641 0.02832 0.03987 0.04643 SI1 4 0.598594 0.614030 0.326282 11.00000 0.00957 0.00960 = 0.00815 -0.00293 0.00107 -0.00444 O1 3 0.660285 0.465472 0.349294 11.00000 0.01556 0.01045 = 0.01402 -0.00447 0.00362 -0.00490 SI2 4 0.654424 0.331970 0.416723 11.00000 0.00992 0.00906 = 0.00854 -0.00376 0.00071 -0.00304 O2 3 0.708181 0.289086 0.541550 11.00000 0.01668 0.01476 = 0.01006 -0.00523 -0.00078 -0.00399 SI3 4 0.706937 0.318012 0.649487 11.00000 0.00879 0.00988 = 0.00796 -0.00274 -0.00038 -0.00275 O3 3 0.722288 0.448565 0.620497 11.00000 0.01306 0.01140 = 0.01557 -0.00373 -0.00151 -0.00441 SI4 4 0.651006 0.599441 0.559612 11.00000 0.00987 0.01063 = 0.00926 -0.00391 0.00055 -0.00520 O4 3 0.638654 0.633632 0.431169 11.00000 0.01897 0.01750 = 0.01038 -0.00540 0.00112 -0.01043 O5 3 0.435373 0.669589 0.303451 11.00000 0.01013 0.01618 = 0.01267 -0.00340 0.00097 -0.00455 O6 3 0.499450 0.347955 0.406598 11.00000 0.01131 0.01559 = 0.01690 -0.00855 0.00205 -0.00519 C11 1 0.669431 0.692998 0.208124 11.00000 0.01475 0.01490 = 0.01198 -0.00367 0.00311 -0.00761 C12 1 0.664488 0.817502 0.207439 11.00000 0.02482 0.01911 = 0.01804 -0.00366 0.00206 -0.01470 AFIX 23 H121 2 0.721654 0.798648 0.272173 11.00000 21.00000 H122 2 0.705929 0.852661 0.144587 11.00000 21.00000 AFIX 0 C13 1 0.526773 0.917803 0.204232 11.00000 0.03148 0.01707 = 0.03272 -0.00945 0.00305 -0.01107 AFIX 23 H131 2 0.483718 0.884376 0.266668 11.00000 61.00000 H132 2 0.469058 0.940096 0.138582 11.00000 61.00000 AFIX 0 C14 1 0.535838 1.035034 0.205711 11.00000 0.06481 0.02201 = 0.04859 -0.01406 0.00460 -0.02178 AFIX 137 H141 2 0.588724 1.014274 0.272473 11.00000 101.00000 H142 2 0.444865 1.098405 0.200951 11.00000 101.00000 H143 2 0.579744 1.067668 0.144660 11.00000 101.00000 AFIX 0 C15 1 0.592800 0.714477 0.104106 11.00000 0.03119 0.02433 = 0.01120 -0.00604 0.00359 -0.01530 AFIX 137 H151 2 0.632695 0.752242 0.042469 11.00000 141.00000 H152 2 0.497795 0.770507 0.098671 11.00000 141.00000 H153 2 0.599161 0.634346 0.105007 11.00000 141.00000 AFIX 0 C16 1 0.818825 0.606090 0.214553 11.00000 0.01759 0.02590 = 0.02827 -0.00526 0.01042 -0.00836 AFIX 137 H161 2 0.825077 0.528342 0.209829 11.00000 181.00000 H162 2 0.867421 0.587151 0.282717 11.00000 181.00000 H163 2 0.858965 0.647520 0.155200 11.00000 181.00000 AFIX 0 C21 1 0.761950 0.206929 0.368804 11.00000 0.01291 0.01179 = 0.01205 -0.00518 0.00109 -0.00306 C22 1 0.700625 0.221004 0.261151 11.00000 0.01746 0.01576 = 0.01437 -0.00852 0.00218 -0.00608 AFIX 23 H221 2 0.759297 0.147751 0.244444 11.00000 31.00000 H222 2 0.611858 0.217046 0.271247 11.00000 31.00000 AFIX 0 C23 1 0.680244 0.338462 0.163403 11.00000 0.03280 0.02411 = 0.01328 -0.00540 -0.00023 -0.01522 AFIX 23 H231 2 0.766841 0.346932 0.153473 11.00000 71.00000 H232 2 0.614470 0.412897 0.175081 11.00000 71.00000 AFIX 0 C24 1 0.628661 0.331745 0.063006 11.00000 0.04133 0.03458 = 0.01419 -0.00974 -0.00035 -0.01619 AFIX 137 H241 2 0.694916 0.259234 0.050496 11.00000 111.00000 H242 2 0.615164 0.408102 0.001287 11.00000 111.00000 H243 2 0.542821 0.323591 0.072852 11.00000 111.00000 AFIX 0 C25 1 0.771036 0.081162 0.452566 11.00000 0.02773 0.01084 = 0.01858 -0.00462 0.00224 -0.00350 AFIX 137 H251 2 0.825646 0.013216 0.429220 11.00000 151.00000 H252 2 0.680180 0.083649 0.459726 11.00000 151.00000 H253 2 0.813040 0.066945 0.521818 11.00000 151.00000 AFIX 0 C26 1 0.905100 0.202812 0.361881 11.00000 0.01259 0.02461 = 0.02303 -0.01315 0.00195 -0.00374 AFIX 137 H261 2 0.961578 0.135055 0.338957 11.00000 191.00000 H262 2 0.944174 0.188190 0.432344 11.00000 191.00000 H263 2 0.900643 0.282572 0.309938 11.00000 191.00000 AFIX 0 C31 1 0.849427 0.190163 0.751771 11.00000 0.01208 0.01325 = 0.01132 -0.00304 -0.00210 -0.00247 C32 1 0.830406 0.067562 0.782211 11.00000 0.01833 0.01392 = 0.01631 0.00031 -0.00229 -0.00440 AFIX 23 H321 2 0.740845 0.081591 0.807430 11.00000 41.00000 H322 2 0.828834 0.050132 0.716464 11.00000 41.00000 AFIX 0 C33 1 0.935546 -0.048657 0.867310 11.00000 0.03222 0.01629 = 0.02644 0.00220 -0.00861 -0.00289 AFIX 23 H331 2 1.025101 -0.067057 0.841430 11.00000 81.00000 H332 2 0.940244 -0.032028 0.933082 11.00000 81.00000 AFIX 0 C34 1 0.903366 -0.162157 0.894239 11.00000 0.04734 0.01738 = 0.03492 0.00326 0.00327 -0.00882 AFIX 137 H341 2 0.815229 -0.144762 0.920693 11.00000 121.00000 H342 2 0.972886 -0.234237 0.949537 11.00000 121.00000 H343 2 0.901269 -0.180530 0.829820 11.00000 121.00000 AFIX 0 C35 1 0.846583 0.226310 0.849554 11.00000 0.04014 0.02344 = 0.01685 -0.00788 -0.01229 -0.00208 AFIX 137 H351 2 0.924031 0.163038 0.902874 11.00000 161.00000 H352 2 0.762840 0.231266 0.880929 11.00000 161.00000 H353 2 0.851066 0.307646 0.827131 11.00000 161.00000 AFIX 0 C36 1 0.982928 0.178041 0.704894 11.00000 0.01152 0.02275 = 0.03201 -0.00076 0.00023 -0.00409 AFIX 137 H361 2 0.989650 0.258492 0.681592 11.00000 201.00000 H362 2 0.985569 0.153360 0.643506 11.00000 201.00000 H363 2 1.058678 0.114542 0.759697 11.00000 201.00000 AFIX 0 C41 1 0.754955 0.670767 0.595065 11.00000 0.01981 0.02170 = 0.01341 -0.00679 0.00193 -0.01457 C42 1 0.815385 0.606684 0.714209 11.00000 0.01907 0.02476 = 0.01582 -0.00898 0.00005 -0.01139 AFIX 23 H421 2 0.876133 0.518645 0.727659 11.00000 51.00000 H422 2 0.872020 0.647195 0.725608 11.00000 51.00000 AFIX 0 C43 1 0.718364 0.606917 0.798504 11.00000 0.02303 0.02329 = 0.01611 -0.00865 0.00272 -0.00856 AFIX 23 H431 2 0.667246 0.558820 0.793962 11.00000 91.00000 H432 2 0.652995 0.693791 0.784414 11.00000 91.00000 AFIX 0 C44 1 0.794778 0.549299 0.910904 11.00000 0.03961 0.03602 = 0.01590 -0.01014 0.00110 -0.01703 AFIX 137 H441 2 0.856625 0.462138 0.926063 11.00000 131.00000 H442 2 0.730335 0.552610 0.963558 11.00000 131.00000 H443 2 0.846342 0.596225 0.915120 11.00000 131.00000 AFIX 0 C45 1 0.670583 0.811765 0.565770 11.00000 0.04925 0.01889 = 0.02526 -0.00285 -0.00712 -0.02133 AFIX 137 H451 2 0.726734 0.848874 0.582662 11.00000 171.00000 H452 2 0.593565 0.824160 0.606942 11.00000 171.00000 H453 2 0.637819 0.851886 0.489083 11.00000 171.00000 AFIX 0 C46 1 0.875200 0.652415 0.529270 11.00000 0.03167 0.07001 = 0.02468 -0.02284 0.01253 -0.03894 AFIX 137 H461 2 0.841588 0.694701 0.452744 11.00000 211.00000 H462 2 0.927906 0.563015 0.546016 11.00000 211.00000 H463 2 0.932528 0.687866 0.547233 11.00000 211.00000 HKLF 4 END ; #---------------------------------------------------------------------------- data_4d_i1113 _audit_author_name 'Clemens Bruhn' _audit_creation_method 'manual edited SHELXL-97 .cif file' _chemical_compound_source 'synthetical product' _chemical_name_systematic ; octakis(1,1-dimethylpentyl)octasilsesquioxane ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C56 H120 O12 Si8' _chemical_formula_weight 1210.24 loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source 'C' 'C' 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'H' 'H' 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'O' 'O' 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'Si' 'Si' 0.0817 0.0704 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting monoclinic _symmetry_space_group_name_H-M 'P 21/n' _symmetry_Int_Tables_number 14 loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x+1/2, y+1/2, -z+1/2' '-x, -y, -z' 'x-1/2, -y-1/2, z-1/2' _cell_length_a 14.1192(9) _cell_length_b 12.8237(5) _cell_length_c 20.1991(12) _cell_angle_alpha 90.00 _cell_angle_beta 97.065(5) _cell_angle_gamma 90.00 _cell_volume 3629.5(3) _cell_formula_units_Z 2 _cell_measurement_temperature 173(2) _cell_measurement_reflns_used 19393 _cell_measurement_theta_min 1.67 _cell_measurement_theta_max 25.49 _exptl_crystal_description 'needle' _exptl_crystal_colour 'colorless' _exptl_crystal_size_max 0.60 _exptl_crystal_size_mid 0.60 _exptl_crystal_size_min 0.07 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.107 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1328 _exptl_absorpt_coefficient_mu 0.198 _exptl_absorpt_correction_type integration _exptl_absorpt_correction_T_min 0.8735 _exptl_absorpt_correction_T_max 0.9868 _exptl_absorpt_process_details 'X-red ver.1.31 (Stoe & Cie. 2005)' _exptl_special_details ; ? ; _diffrn_ambient_temperature 173(2) _diffrn_measurement_device '2-circle goniometer' _diffrn_measurement_device_type 'STOE IPDS 2' _diffrn_detector 'image plate (34 cm diameter)' _diffrn_detector_type 'STOE' _diffrn_detector_area_resol_mean 6.67 _diffrn_source 'sealed X-ray tube, 12 x 0.4 mm long-fine focus' _diffrn_source_voltage 50 _diffrn_source_current 30 _diffrn_source_power 1.50 _diffrn_radiation_type 'Mo K\a' _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_monochromator 'plane graphite' _diffrn_radiation_polarisn_norm 0 _diffrn_radiation_collimation '0.5 mm diameter, multiple pinhole' _diffrn_measurement_method 'rotation method' _diffrn_measurement_details ; 178 frames, detector distance = 135 mm ; _diffrn_standards_decay_% 0 _diffrn_reflns_number 22786 _diffrn_reflns_av_R_equivalents 0.1663 _diffrn_reflns_av_sigmaI/netI 0.1091 _diffrn_reflns_limit_h_min -16 _diffrn_reflns_limit_h_max 16 _diffrn_reflns_limit_k_min -14 _diffrn_reflns_limit_k_max 15 _diffrn_reflns_limit_l_min -24 _diffrn_reflns_limit_l_max 24 _diffrn_reflns_theta_min 1.67 _diffrn_reflns_theta_max 25.00 _reflns_number_total 6395 _reflns_number_gt 4615 _reflns_threshold_expression >2sigma(I) _computing_data_collection ? _computing_cell_refinement ? _computing_data_reduction ? _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics ? _computing_publication_material ? _refine_special_details ; Refinement of F^2^ against ALL reflections. The weighted R-factor wR and goodness of fit S are based on F^2^, conventional R-factors R are based on F, with F set to zero for negative F^2^. The threshold expression of F^2^ > 2sigma(F^2^) is used only for calculating R-factors(gt) etc. and is not relevant to the choice of reflections for refinement. R-factors based on F^2^ are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger. ; _refine_ls_structure_factor_coef Fsqd _refine_ls_matrix_type full _refine_ls_weighting_scheme calc _refine_ls_weighting_details 'calc w=1/[\s^2^(Fo^2^)+(0.1166P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment constr _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 6395 _refine_ls_number_parameters 431 _refine_ls_number_restraints 370 _refine_ls_R_factor_all 0.0951 _refine_ls_R_factor_gt 0.0745 _refine_ls_wR_factor_ref 0.2028 _refine_ls_wR_factor_gt 0.1887 _refine_ls_goodness_of_fit_ref 1.003 _refine_ls_restrained_S_all 0.989 _refine_ls_shift/su_max 0.000 _refine_ls_shift/su_mean 0.000 loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_occupancy _atom_site_symmetry_multiplicity _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group C1 C 0.2215(2) -0.0013(3) 0.18540(17) 0.0532(8) Uani 1 1 d U . . C2 C 0.3177(3) 0.0443(3) 0.1710(2) 0.0650(10) Uani 1 1 d U . . H2A H 0.3621 0.0426 0.2129 0.078 Uiso 1 1 calc R . . H2B H 0.3443 -0.0023 0.1389 0.078 Uiso 1 1 calc R . . C3 C 0.3168(3) 0.1547(3) 0.1434(2) 0.0661(10) Uani 1 1 d U . . H3A H 0.2735 0.1572 0.1011 0.079 Uiso 1 1 calc R . . H3B H 0.2909 0.2023 0.1754 0.079 Uiso 1 1 calc R . . C4 C 0.4143(3) 0.1934(4) 0.1309(3) 0.0879(15) Uani 1 1 d U . . H4B H 0.4569 0.1942 0.1737 0.105 Uiso 1 1 calc R . . H4A H 0.4416 0.1440 0.1007 0.105 Uiso 1 1 calc R . . C5 C 0.4124(5) 0.3005(5) 0.1007(4) 0.123(2) Uani 1 1 d U . . H5A H 0.3845 0.3497 0.1300 0.147 Uiso 1 1 calc R . . H5B H 0.3739 0.2994 0.0569 0.147 Uiso 1 1 calc R . . H5C H 0.4776 0.3223 0.0956 0.147 Uiso 1 1 calc R . . C6 C 0.1833(3) 0.0555(4) 0.24407(19) 0.0750(12) Uani 1 1 d U . . H6A H 0.1749 0.1298 0.2334 0.090 Uiso 1 1 calc R . . H6B H 0.2290 0.0476 0.2844 0.090 Uiso 1 1 calc R . . H6C H 0.1219 0.0253 0.2517 0.090 Uiso 1 1 calc R . . C7 C 0.2386(3) -0.1177(4) 0.2064(2) 0.0770(12) Uani 1 1 d U . . H7A H 0.2847 -0.1210 0.2468 0.092 Uiso 1 1 calc R . . H7B H 0.2637 -0.1559 0.1704 0.092 Uiso 1 1 calc R . . H7C H 0.1782 -0.1491 0.2153 0.092 Uiso 1 1 calc R . . C8 C -0.2960(3) 0.0761(3) 0.0589(2) 0.0631(10) Uani 1 1 d DU . . C9 C -0.3543(6) 0.1467(8) 0.0063(5) 0.088(3) Uani 0.580(10) 1 d PDU A 3 H9A H -0.3672 0.1078 -0.0362 0.105 Uiso 0.580(10) 1 calc PR A 3 H9B H -0.4164 0.1633 0.0218 0.105 Uiso 0.580(10) 1 calc PR A 3 C10 C -0.3050(10) 0.2444(13) -0.0058(9) 0.098(5) Uani 0.580(10) 1 d PDU A 3 H10A H -0.2541 0.2304 -0.0343 0.117 Uiso 0.580(10) 1 calc PR A 3 H10B H -0.2749 0.2734 0.0371 0.117 Uiso 0.580(10) 1 calc PR A 3 C11 C -0.3759(10) 0.3235(12) -0.0403(9) 0.130(5) Uani 0.580(10) 1 d PDU A 3 H11A H -0.4230 0.2842 -0.0711 0.156 Uiso 0.580(10) 1 calc PR A 3 H11B H -0.4112 0.3542 -0.0056 0.156 Uiso 0.580(10) 1 calc PR A 3 C12 C -0.3422(13) 0.4080(11) -0.0773(8) 0.150(6) Uani 0.580(10) 1 d PDU A 3 H12C H -0.3783 0.4102 -0.1220 0.180 Uiso 0.580(10) 1 calc PR A 3 H12B H -0.2743 0.3979 -0.0812 0.180 Uiso 0.580(10) 1 calc PR A 3 H12A H -0.3509 0.4738 -0.0542 0.180 Uiso 0.580(10) 1 calc PR A 3 C9X C -0.3211(7) 0.1944(7) 0.0504(5) 0.065(3) Uani 0.420(10) 1 d PDU A 4 H9C H -0.3814 0.2057 0.0697 0.079 Uiso 0.420(10) 1 calc PR A 4 H9D H -0.2709 0.2336 0.0786 0.079 Uiso 0.420(10) 1 calc PR A 4 C10X C -0.3326(13) 0.2452(19) -0.0170(11) 0.092(5) Uani 0.420(10) 1 d PDU A 4 H10C H -0.3927 0.2125 -0.0374 0.110 Uiso 0.420(10) 1 calc PR A 4 H10D H -0.2821 0.2090 -0.0382 0.110 Uiso 0.420(10) 1 calc PR A 4 C11X C -0.3370(16) 0.3517(17) -0.0549(14) 0.129(7) Uani 0.420(10) 1 d PDU A 4 H11C H -0.2845 0.3984 -0.0365 0.155 Uiso 0.420(10) 1 calc PR A 4 H11D H -0.3339 0.3414 -0.1032 0.155 Uiso 0.420(10) 1 calc PR A 4 C12X C -0.4292(14) 0.393(2) -0.0429(11) 0.162(9) Uani 0.420(10) 1 d PDU A 4 H12D H -0.4228 0.4292 0.0001 0.195 Uiso 0.420(10) 1 calc PR A 4 H12E H -0.4749 0.3355 -0.0422 0.195 Uiso 0.420(10) 1 calc PR A 4 H12F H -0.4522 0.4419 -0.0785 0.195 Uiso 0.420(10) 1 calc PR A 4 C13 C -0.2895(3) 0.0938(6) 0.1328(3) 0.118(2) Uani 1 1 d U A . H13A H -0.3525 0.1125 0.1447 0.142 Uiso 1 1 calc R . . H13B H -0.2445 0.1506 0.1456 0.142 Uiso 1 1 calc R . . H13C H -0.2671 0.0299 0.1564 0.142 Uiso 1 1 calc R . . C14 C -0.3589(4) -0.0154(6) 0.0412(3) 0.121(3) Uani 1 1 d U A . H14A H -0.3628 -0.0286 -0.0069 0.145 Uiso 1 1 calc R . . H14B H -0.4229 -0.0011 0.0530 0.145 Uiso 1 1 calc R . . H14C H -0.3325 -0.0769 0.0656 0.145 Uiso 1 1 calc R . . C15 C 0.0102(3) 0.3263(3) 0.09265(17) 0.0507(8) Uani 1 1 d DU . . C16 C 0.0119(6) 0.3276(8) 0.1707(4) 0.060(2) Uani 0.650(11) 1 d PDU B 1 H16A H 0.0657 0.2840 0.1909 0.072 Uiso 0.650(11) 1 calc PR B 1 H16B H 0.0236 0.3999 0.1869 0.072 Uiso 0.650(11) 1 calc PR B 1 C17 C -0.0824(8) 0.2870(8) 0.1944(4) 0.085(3) Uani 0.650(11) 1 d PDU B 1 H17A H -0.1368 0.3097 0.1619 0.102 Uiso 0.650(11) 1 calc PR B 1 H17B H -0.0814 0.2098 0.1941 0.102 Uiso 0.650(11) 1 calc PR B 1 C18 C -0.0995(8) 0.3241(12) 0.2641(5) 0.116(4) Uani 0.650(11) 1 d PDU B 1 H18A H -0.1004 0.4013 0.2650 0.139 Uiso 0.650(11) 1 calc PR B 1 H18B H -0.1625 0.2988 0.2740 0.139 Uiso 0.650(11) 1 calc PR B 1 C19 C -0.0265(10) 0.2865(15) 0.3141(8) 0.148(5) Uani 0.650(11) 1 d PDU B 1 H19C H -0.0483 0.2927 0.3581 0.177 Uiso 0.650(11) 1 calc PR B 1 H19B H 0.0316 0.3280 0.3131 0.177 Uiso 0.650(11) 1 calc PR B 1 H19A H -0.0129 0.2132 0.3052 0.177 Uiso 0.650(11) 1 calc PR B 1 C16X C -0.0343(18) 0.3336(16) 0.1577(8) 0.090(5) Uani 0.350(11) 1 d PDU B 2 H16C H -0.0117 0.4001 0.1790 0.108 Uiso 0.350(11) 1 calc PR B 2 H16D H -0.1039 0.3415 0.1449 0.108 Uiso 0.350(11) 1 calc PR B 2 C17X C -0.0226(18) 0.2556(13) 0.2093(8) 0.096(5) Uani 0.350(11) 1 d PDU B 2 H17C H 0.0470 0.2437 0.2186 0.116 Uiso 0.350(11) 1 calc PR B 2 H17D H -0.0498 0.1908 0.1881 0.116 Uiso 0.350(11) 1 calc PR B 2 C18X C -0.0575(18) 0.2598(13) 0.2753(8) 0.095(5) Uani 0.350(11) 1 d PDU B 2 H18C H -0.0152 0.2163 0.3069 0.114 Uiso 0.350(11) 1 calc PR B 2 H18D H -0.1222 0.2289 0.2714 0.114 Uiso 0.350(11) 1 calc PR B 2 C19X C -0.0618(17) 0.3691(15) 0.3045(10) 0.107(6) Uani 0.350(11) 1 d PDU B 2 H19D H -0.0474 0.3657 0.3532 0.128 Uiso 0.350(11) 1 calc PR B 2 H19E H -0.1259 0.3981 0.2927 0.128 Uiso 0.350(11) 1 calc PR B 2 H19F H -0.0149 0.4139 0.2865 0.128 Uiso 0.350(11) 1 calc PR B 2 C20 C -0.0674(4) 0.3940(3) 0.0539(3) 0.0834(14) Uani 1 1 d U B . H20A H -0.0650 0.4644 0.0728 0.100 Uiso 1 1 calc R . . H20B H -0.1302 0.3632 0.0572 0.100 Uiso 1 1 calc R . . H20C H -0.0567 0.3975 0.0069 0.100 Uiso 1 1 calc R . . C21 C 0.1069(3) 0.3746(3) 0.0849(3) 0.0835(14) Uani 1 1 d U B . H21A H 0.1574 0.3351 0.1116 0.100 Uiso 1 1 calc R . . H21B H 0.1081 0.4471 0.1003 0.100 Uiso 1 1 calc R . . H21C H 0.1174 0.3727 0.0379 0.100 Uiso 1 1 calc R . . C22 C 0.0812(2) 0.2442(2) -0.14765(17) 0.0487(7) Uani 1 1 d U . . C23 C 0.1727(3) 0.2995(3) -0.11477(19) 0.0596(9) Uani 1 1 d U . . H23A H 0.1588 0.3299 -0.0720 0.072 Uiso 1 1 calc R . . H23B H 0.2228 0.2459 -0.1042 0.072 Uiso 1 1 calc R . . C24 C 0.2134(3) 0.3855(3) -0.1552(2) 0.0653(10) Uani 1 1 d U . . H24A H 0.2306 0.3556 -0.1974 0.078 Uiso 1 1 calc R . . H24B H 0.1639 0.4393 -0.1669 0.078 Uiso 1 1 calc R . . C25 C 0.3000(4) 0.4357(4) -0.1178(3) 0.0910(15) Uani 1 1 d U . . H25B H 0.3482 0.3812 -0.1044 0.109 Uiso 1 1 calc R . . H25A H 0.2820 0.4681 -0.0767 0.109 Uiso 1 1 calc R . . C26 C 0.3448(5) 0.5192(5) -0.1590(3) 0.113(2) Uani 1 1 d U . . H26A H 0.2982 0.5748 -0.1711 0.135 Uiso 1 1 calc R . . H26B H 0.3635 0.4875 -0.1996 0.135 Uiso 1 1 calc R . . H26C H 0.4013 0.5487 -0.1324 0.135 Uiso 1 1 calc R . . C27 C 0.0991(3) 0.1898(3) -0.21288(18) 0.0611(9) Uani 1 1 d U . . H27A H 0.1543 0.1433 -0.2042 0.073 Uiso 1 1 calc R . . H27B H 0.1117 0.2424 -0.2459 0.073 Uiso 1 1 calc R . . H27C H 0.0426 0.1490 -0.2301 0.073 Uiso 1 1 calc R . . C28 C -0.0015(3) 0.3218(3) -0.1617(2) 0.0627(10) Uani 1 1 d U . . H28C H -0.0598 0.2842 -0.1788 0.075 Uiso 1 1 calc R . . H28B H 0.0138 0.3729 -0.1949 0.075 Uiso 1 1 calc R . . H28A H -0.0113 0.3579 -0.1203 0.075 Uiso 1 1 calc R . . O1 O 0.08295(16) 0.11692(17) 0.09955(11) 0.0480(5) Uani 1 1 d U . . O2 O -0.10099(16) 0.14170(17) 0.05803(11) 0.0478(5) Uani 1 1 d U . . O3 O -0.17921(15) 0.03059(18) -0.04472(11) 0.0483(5) Uani 1 1 d U . . O4 O -0.13486(16) -0.05901(18) 0.07231(12) 0.0498(5) Uani 1 1 d U . . O5 O 0.02774(17) 0.19739(17) -0.01942(11) 0.0505(6) Uani 1 1 d U . . O6 O -0.04616(16) 0.08064(17) -0.12037(11) 0.0497(5) Uani 1 1 d U . . Si1 Si 0.13041(6) 0.00204(7) 0.11047(4) 0.0416(2) Uani 1 1 d U . . Si2 Si -0.17442(6) 0.04739(7) 0.03523(4) 0.0429(2) Uani 1 1 d U A . Si3 Si 0.00473(6) 0.19179(6) 0.05740(4) 0.0416(2) Uani 1 1 d U A . Si4 Si 0.04834(6) 0.14228(7) -0.08822(4) 0.0427(2) Uani 1 1 d U . . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 C1 0.0472(18) 0.068(2) 0.0432(17) -0.0010(16) -0.0014(14) 0.0001(16) C2 0.051(2) 0.082(3) 0.060(2) -0.0105(19) -0.0031(17) -0.0036(19) C3 0.049(2) 0.077(3) 0.072(3) -0.013(2) 0.0062(18) -0.0146(18) C4 0.067(3) 0.111(4) 0.086(3) -0.020(3) 0.011(2) -0.035(3) C5 0.098(4) 0.117(5) 0.160(7) 0.005(4) 0.043(4) -0.043(4) C6 0.073(3) 0.109(3) 0.042(2) -0.009(2) 0.0035(18) -0.006(2) C7 0.073(3) 0.086(3) 0.066(3) 0.018(2) -0.015(2) 0.003(2) C8 0.0431(18) 0.079(2) 0.068(2) -0.007(2) 0.0120(17) 0.0061(18) C9 0.054(4) 0.116(7) 0.092(6) -0.015(5) 0.004(4) 0.029(4) C10 0.072(10) 0.114(8) 0.103(8) 0.015(6) -0.006(7) 0.057(7) C11 0.094(9) 0.124(9) 0.180(12) 0.085(8) 0.046(8) 0.058(8) C12 0.203(16) 0.111(9) 0.138(11) 0.076(8) 0.035(10) 0.039(10) C9X 0.046(5) 0.083(6) 0.067(6) -0.017(5) 0.006(4) 0.009(4) C10X 0.033(7) 0.114(10) 0.125(12) 0.045(8) -0.004(7) 0.023(7) C11X 0.118(15) 0.120(15) 0.156(16) 0.034(13) 0.041(12) 0.039(12) C12X 0.151(17) 0.184(19) 0.142(17) 0.014(14) -0.022(14) 0.064(16) C13 0.055(3) 0.215(7) 0.089(4) -0.065(4) 0.030(2) -0.026(4) C14 0.057(3) 0.179(6) 0.134(5) -0.081(5) 0.041(3) -0.038(3) C15 0.0564(19) 0.0458(16) 0.0498(19) -0.0031(14) 0.0062(15) -0.0024(15) C16 0.066(4) 0.064(4) 0.047(4) -0.012(3) -0.004(3) -0.006(4) C17 0.094(6) 0.107(6) 0.061(4) -0.022(4) 0.031(4) -0.022(5) C18 0.107(8) 0.150(10) 0.096(8) -0.013(8) 0.034(6) -0.025(7) C19 0.122(10) 0.208(16) 0.111(10) -0.021(11) 0.007(8) -0.003(10) C16X 0.124(14) 0.082(9) 0.069(10) -0.019(8) 0.028(10) -0.001(12) C17X 0.111(12) 0.107(11) 0.080(10) -0.022(8) 0.044(9) 0.005(10) C18X 0.115(13) 0.107(11) 0.056(8) -0.022(8) -0.009(8) -0.002(10) C19X 0.118(14) 0.136(15) 0.066(10) -0.045(11) 0.012(9) 0.017(12) C20 0.082(3) 0.053(2) 0.108(4) -0.012(2) -0.015(3) 0.013(2) C21 0.071(3) 0.055(2) 0.125(4) -0.018(2) 0.014(3) -0.011(2) C22 0.0534(19) 0.0490(17) 0.0439(17) -0.0002(14) 0.0064(14) -0.0061(15) C23 0.064(2) 0.066(2) 0.050(2) 0.0045(16) 0.0131(17) -0.0194(18) C24 0.073(2) 0.062(2) 0.064(2) 0.0065(18) 0.0197(19) -0.0128(19) C25 0.095(4) 0.097(3) 0.081(3) 0.004(3) 0.015(3) -0.048(3) C26 0.107(4) 0.102(4) 0.135(5) 0.015(4) 0.036(4) -0.047(3) C27 0.077(3) 0.064(2) 0.0438(19) -0.0002(16) 0.0135(17) -0.0050(19) C28 0.074(2) 0.057(2) 0.058(2) 0.0121(16) 0.0104(19) 0.0032(18) O1 0.0451(12) 0.0489(12) 0.0490(13) -0.0020(10) 0.0017(10) -0.0010(10) O2 0.0442(12) 0.0505(12) 0.0492(13) -0.0054(10) 0.0079(10) -0.0008(10) O3 0.0416(11) 0.0611(13) 0.0416(12) -0.0043(10) 0.0033(9) 0.0044(10) O4 0.0430(12) 0.0557(13) 0.0522(13) 0.0076(10) 0.0112(10) -0.0006(10) O5 0.0589(14) 0.0512(12) 0.0431(13) -0.0027(9) 0.0131(10) -0.0051(10) O6 0.0488(13) 0.0534(12) 0.0462(12) 0.0037(10) 0.0035(10) -0.0077(10) Si1 0.0377(4) 0.0479(5) 0.0385(4) -0.0001(3) 0.0025(3) -0.0004(3) Si2 0.0350(4) 0.0506(5) 0.0435(5) -0.0018(4) 0.0071(3) 0.0012(3) Si3 0.0426(5) 0.0425(4) 0.0403(5) -0.0019(3) 0.0072(4) -0.0010(3) Si4 0.0443(5) 0.0455(5) 0.0389(5) 0.0018(3) 0.0075(3) -0.0035(4) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag C1 C2 1.539(5) . ? C1 C6 1.543(5) . ? C1 C7 1.563(6) . ? C1 Si1 1.862(3) . ? C2 C3 1.520(6) . ? C2 H2A 0.9900 . ? C2 H2B 0.9900 . ? C3 C4 1.514(6) . ? C3 H3A 0.9900 . ? C3 H3B 0.9900 . ? C4 C5 1.501(8) . ? C4 H4B 0.9900 . ? C4 H4A 0.9900 . ? C5 H5A 0.9800 . ? C5 H5B 0.9800 . ? C5 H5C 0.9800 . ? C6 H6A 0.9800 . ? C6 H6B 0.9800 . ? C6 H6C 0.9800 . ? C7 H7A 0.9800 . ? C7 H7B 0.9800 . ? C7 H7C 0.9800 . ? C8 C14 1.489(7) . ? C8 C13 1.502(6) . ? C8 C9 1.553(9) . ? C8 C9X 1.563(10) . ? C8 Si2 1.875(4) . ? C9 C10 1.468(15) . ? C9 H9A 0.9900 . ? C9 H9B 0.9900 . ? C10 C11 1.532(13) . ? C10 H10A 0.9900 . ? C10 H10B 0.9900 . ? C11 C12 1.430(13) . ? C11 H11A 0.9900 . ? C11 H11B 0.9900 . ? C12 H12C 0.9800 . ? C12 H12B 0.9800 . ? C12 H12A 0.9800 . ? C9X C10X 1.499(16) . ? C9X H9C 0.9900 . ? C9X H9D 0.9900 . ? C10X C11X 1.563(17) . ? C10X H10C 0.9900 . ? C10X H10D 0.9900 . ? C11X C12X 1.453(17) . ? C11X H11C 0.9900 . ? C11X H11D 0.9900 . ? C12X H12D 0.9800 . ? C12X H12E 0.9800 . ? C12X H12F 0.9800 . ? C13 H13A 0.9800 . ? C13 H13B 0.9800 . ? C13 H13C 0.9800 . ? C14 H14A 0.9800 . ? C14 H14B 0.9800 . ? C14 H14C 0.9800 . ? C15 C21 1.524(6) . ? C15 C16X 1.527(14) . ? C15 C20 1.535(5) . ? C15 C16 1.573(8) . ? C15 Si3 1.865(3) . ? C16 C17 1.560(10) . ? C16 H16A 0.9900 . ? C16 H16B 0.9900 . ? C17 C18 1.532(12) . ? C17 H17A 0.9900 . ? C17 H17B 0.9900 . ? C18 C19 1.435(14) . ? C18 H18A 0.9900 . ? C18 H18B 0.9900 . ? C19 H19C 0.9800 . ? C19 H19B 0.9800 . ? C19 H19A 0.9800 . ? C16X C17X 1.440(17) . ? C16X H16C 0.9900 . ? C16X H16D 0.9900 . ? C17X C18X 1.479(15) . ? C17X H17C 0.9900 . ? C17X H17D 0.9900 . ? C18X C19X 1.525(16) . ? C18X H18C 0.9900 . ? C18X H18D 0.9900 . ? C19X H19D 0.9800 . ? C19X H19E 0.9800 . ? C19X H19F 0.9800 . ? C20 H20A 0.9800 . ? C20 H20B 0.9800 . ? C20 H20C 0.9800 . ? C21 H21A 0.9800 . ? C21 H21B 0.9800 . ? C21 H21C 0.9800 . ? C22 C28 1.534(5) . ? C22 C27 1.539(5) . ? C22 C23 1.550(5) . ? C22 Si4 1.871(3) . ? C23 C24 1.527(5) . ? C23 H23A 0.9900 . ? C23 H23B 0.9900 . ? C24 C25 1.501(6) . ? C24 H24A 0.9900 . ? C24 H24B 0.9900 . ? C25 C26 1.539(6) . ? C25 H25B 0.9900 . ? C25 H25A 0.9900 . ? C26 H26A 0.9800 . ? C26 H26B 0.9800 . ? C26 H26C 0.9800 . ? C27 H27A 0.9800 . ? C27 H27B 0.9800 . ? C27 H27C 0.9800 . ? C28 H28C 0.9800 . ? C28 H28B 0.9800 . ? C28 H28A 0.9800 . ? O1 Si1 1.622(2) . ? O1 Si3 1.623(2) . ? O2 Si2 1.622(2) . ? O2 Si3 1.627(2) . ? O3 Si2 1.622(2) . ? O3 Si1 1.624(2) 3 ? O4 Si2 1.622(2) . ? O4 Si4 1.625(2) 3 ? O5 Si4 1.617(2) . ? O5 Si3 1.626(2) . ? O6 Si4 1.617(2) . ? O6 Si1 1.624(2) 3 ? Si1 O6 1.624(2) 3 ? Si1 O3 1.624(2) 3 ? Si4 O4 1.625(2) 3 ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag C2 C1 C6 111.4(3) . . ? C2 C1 C7 107.7(3) . . ? C6 C1 C7 107.4(3) . . ? C2 C1 Si1 112.0(3) . . ? C6 C1 Si1 110.0(3) . . ? C7 C1 Si1 108.1(3) . . ? C3 C2 C1 117.1(3) . . ? C3 C2 H2A 108.0 . . ? C1 C2 H2A 108.0 . . ? C3 C2 H2B 108.0 . . ? C1 C2 H2B 108.0 . . ? H2A C2 H2B 107.3 . . ? C4 C3 C2 113.6(4) . . ? C4 C3 H3A 108.8 . . ? C2 C3 H3A 108.8 . . ? C4 C3 H3B 108.8 . . ? C2 C3 H3B 108.8 . . ? H3A C3 H3B 107.7 . . ? C5 C4 C3 113.4(5) . . ? C5 C4 H4B 108.9 . . ? C3 C4 H4B 108.9 . . ? C5 C4 H4A 108.9 . . ? C3 C4 H4A 108.9 . . ? H4B C4 H4A 107.7 . . ? C4 C5 H5A 109.5 . . ? C4 C5 H5B 109.5 . . ? H5A C5 H5B 109.5 . . ? C4 C5 H5C 109.5 . . ? H5A C5 H5C 109.5 . . ? H5B C5 H5C 109.5 . . ? C1 C6 H6A 109.5 . . ? C1 C6 H6B 109.5 . . ? H6A C6 H6B 109.5 . . ? C1 C6 H6C 109.5 . . ? H6A C6 H6C 109.5 . . ? H6B C6 H6C 109.5 . . ? C1 C7 H7A 109.5 . . ? C1 C7 H7B 109.5 . . ? H7A C7 H7B 109.5 . . ? C1 C7 H7C 109.5 . . ? H7A C7 H7C 109.5 . . ? H7B C7 H7C 109.5 . . ? C14 C8 C13 108.7(4) . . ? C14 C8 C9 92.5(5) . . ? C13 C8 C9 123.7(5) . . ? C14 C8 C9X 128.2(5) . . ? C13 C8 C9X 87.1(5) . . ? C9 C8 C9X 42.7(5) . . ? C14 C8 Si2 108.7(3) . . ? C13 C8 Si2 109.7(3) . . ? C9 C8 Si2 111.4(4) . . ? C9X C8 Si2 111.4(4) . . ? C10 C9 C8 112.9(8) . . ? C10 C9 H9A 109.0 . . ? C8 C9 H9A 109.0 . . ? C10 C9 H9B 109.0 . . ? C8 C9 H9B 109.0 . . ? H9A C9 H9B 107.8 . . ? C9 C10 C11 110.2(12) . . ? C9 C10 H10A 109.6 . . ? C11 C10 H10A 109.6 . . ? C9 C10 H10B 109.6 . . ? C11 C10 H10B 109.6 . . ? H10A C10 H10B 108.1 . . ? C12 C11 C10 119.9(14) . . ? C12 C11 H11A 107.3 . . ? C10 C11 H11A 107.3 . . ? C12 C11 H11B 107.3 . . ? C10 C11 H11B 107.3 . . ? H11A C11 H11B 106.9 . . ? C10X C9X C8 121.3(13) . . ? C10X C9X H9C 107.0 . . ? C8 C9X H9C 107.0 . . ? C10X C9X H9D 107.0 . . ? C8 C9X H9D 107.0 . . ? H9C C9X H9D 106.7 . . ? C9X C10X C11X 145(2) . . ? C9X C10X H10C 100.7 . . ? C11X C10X H10C 100.7 . . ? C9X C10X H10D 100.7 . . ? C11X C10X H10D 100.7 . . ? H10C C10X H10D 104.4 . . ? C12X C11X C10X 103(2) . . ? C12X C11X H11C 111.2 . . ? C10X C11X H11C 111.2 . . ? C12X C11X H11D 111.2 . . ? C10X C11X H11D 111.2 . . ? H11C C11X H11D 109.1 . . ? C8 C13 H13A 109.5 . . ? C8 C13 H13B 109.5 . . ? H13A C13 H13B 109.5 . . ? C8 C13 H13C 109.5 . . ? H13A C13 H13C 109.5 . . ? H13B C13 H13C 109.5 . . ? C8 C14 H14A 109.5 . . ? C8 C14 H14B 109.5 . . ? H14A C14 H14B 109.5 . . ? C8 C14 H14C 109.5 . . ? H14A C14 H14C 109.5 . . ? H14B C14 H14C 109.5 . . ? C21 C15 C16X 122.1(11) . . ? C21 C15 C20 108.1(4) . . ? C16X C15 C20 93.5(9) . . ? C21 C15 C16 101.2(4) . . ? C16X C15 C16 25.2(9) . . ? C20 C15 C16 115.3(5) . . ? C21 C15 Si3 109.4(3) . . ? C16X C15 Si3 112.5(8) . . ? C20 C15 Si3 109.6(2) . . ? C16 C15 Si3 112.8(4) . . ? C17 C16 C15 113.3(6) . . ? C17 C16 H16A 108.9 . . ? C15 C16 H16A 108.9 . . ? C17 C16 H16B 108.9 . . ? C15 C16 H16B 108.9 . . ? H16A C16 H16B 107.7 . . ? C18 C17 C16 114.5(7) . . ? C18 C17 H17A 108.6 . . ? C16 C17 H17A 108.6 . . ? C18 C17 H17B 108.6 . . ? C16 C17 H17B 108.6 . . ? H17A C17 H17B 107.6 . . ? C19 C18 C17 111.2(14) . . ? C19 C18 H18A 109.4 . . ? C17 C18 H18A 109.4 . . ? C19 C18 H18B 109.4 . . ? C17 C18 H18B 109.4 . . ? H18A C18 H18B 108.0 . . ? C17X C16X C15 123.9(15) . . ? C17X C16X H16C 106.4 . . ? C15 C16X H16C 106.4 . . ? C17X C16X H16D 106.4 . . ? C15 C16X H16D 106.4 . . ? H16C C16X H16D 106.4 . . ? C16X C17X C18X 127.3(16) . . ? C16X C17X H17C 105.5 . . ? C18X C17X H17C 105.5 . . ? C16X C17X H17D 105.5 . . ? C18X C17X H17D 105.5 . . ? H17C C17X H17D 106.1 . . ? C17X C18X C19X 114.6(15) . . ? C17X C18X H18C 108.6 . . ? C19X C18X H18C 108.6 . . ? C17X C18X H18D 108.6 . . ? C19X C18X H18D 108.6 . . ? H18C C18X H18D 107.6 . . ? C18X C19X H19D 109.5 . . ? C18X C19X H19E 109.5 . . ? H19D C19X H19E 109.5 . . ? C18X C19X H19F 109.5 . . ? H19D C19X H19F 109.5 . . ? H19E C19X H19F 109.5 . . ? C15 C20 H20A 109.5 . . ? C15 C20 H20B 109.5 . . ? H20A C20 H20B 109.5 . . ? C15 C20 H20C 109.5 . . ? H20A C20 H20C 109.5 . . ? H20B C20 H20C 109.5 . . ? C15 C21 H21A 109.5 . . ? C15 C21 H21B 109.5 . . ? H21A C21 H21B 109.5 . . ? C15 C21 H21C 109.5 . . ? H21A C21 H21C 109.5 . . ? H21B C21 H21C 109.5 . . ? C28 C22 C27 109.7(3) . . ? C28 C22 C23 110.9(3) . . ? C27 C22 C23 111.0(3) . . ? C28 C22 Si4 109.2(2) . . ? C27 C22 Si4 108.2(2) . . ? C23 C22 Si4 107.7(2) . . ? C24 C23 C22 116.8(3) . . ? C24 C23 H23A 108.1 . . ? C22 C23 H23A 108.1 . . ? C24 C23 H23B 108.1 . . ? C22 C23 H23B 108.1 . . ? H23A C23 H23B 107.3 . . ? C25 C24 C23 112.2(4) . . ? C25 C24 H24A 109.2 . . ? C23 C24 H24A 109.2 . . ? C25 C24 H24B 109.2 . . ? C23 C24 H24B 109.2 . . ? H24A C24 H24B 107.9 . . ? C24 C25 C26 113.0(5) . . ? C24 C25 H25B 109.0 . . ? C26 C25 H25B 109.0 . . ? C24 C25 H25A 109.0 . . ? C26 C25 H25A 109.0 . . ? H25B C25 H25A 107.8 . . ? C25 C26 H26A 109.5 . . ? C25 C26 H26B 109.5 . . ? H26A C26 H26B 109.5 . . ? C25 C26 H26C 109.5 . . ? H26A C26 H26C 109.5 . . ? H26B C26 H26C 109.5 . . ? C22 C27 H27A 109.5 . . ? C22 C27 H27B 109.5 . . ? H27A C27 H27B 109.5 . . ? C22 C27 H27C 109.5 . . ? H27A C27 H27C 109.5 . . ? H27B C27 H27C 109.5 . . ? C22 C28 H28C 109.5 . . ? C22 C28 H28B 109.5 . . ? H28C C28 H28B 109.5 . . ? C22 C28 H28A 109.5 . . ? H28C C28 H28A 109.5 . . ? H28B C28 H28A 109.5 . . ? Si1 O1 Si3 148.38(15) . . ? Si2 O2 Si3 147.91(15) . . ? Si2 O3 Si1 151.41(15) . 3 ? Si2 O4 Si4 148.43(15) . 3 ? Si4 O5 Si3 151.55(16) . . ? Si4 O6 Si1 148.27(16) . 3 ? O1 Si1 O6 108.24(12) . 3 ? O1 Si1 O3 109.41(12) . 3 ? O6 Si1 O3 108.86(12) 3 3 ? O1 Si1 C1 111.32(15) . . ? O6 Si1 C1 109.16(15) 3 . ? O3 Si1 C1 109.80(14) 3 . ? O4 Si2 O2 108.92(12) . . ? O4 Si2 O3 108.52(13) . . ? O2 Si2 O3 109.17(12) . . ? O4 Si2 C8 108.75(16) . . ? O2 Si2 C8 110.76(15) . . ? O3 Si2 C8 110.67(15) . . ? O1 Si3 O5 108.89(12) . . ? O1 Si3 O2 109.16(12) . . ? O5 Si3 O2 108.43(12) . . ? O1 Si3 C15 110.70(14) . . ? O5 Si3 C15 108.65(14) . . ? O2 Si3 C15 110.95(14) . . ? O6 Si4 O5 109.40(13) . . ? O6 Si4 O4 108.75(13) . 3 ? O5 Si4 O4 109.12(13) . 3 ? O6 Si4 C22 109.95(14) . . ? O5 Si4 C22 109.35(14) . . ? O4 Si4 C22 110.25(14) 3 . ? _diffrn_measured_fraction_theta_max 1.000 _diffrn_reflns_theta_full 25.00 _diffrn_measured_fraction_theta_full 1.000 _refine_diff_density_max 0.515 _refine_diff_density_min -0.547 _refine_diff_density_rms 0.089 _iucr_refine_instructions_details ; TITL N. HURKES, -100DEGC, CB CELL 0.71073 14.11920 12.82370 20.19910 90.00000 97.06500 90.00000 ZERR 2 0.00090 0.00050 0.00120 0.00000 0.00500 0.00000 LATT 1 SYMM -X+ 0.50000, Y+ 0.50000, -Z+ 0.50000 SFAC C H O SI UNIT 112 240 24 16 TEMP -100 MERG 2 OMIT -6 50 ACTA BOND $H SIZE 0.07 0.60 0.60 DFIX 1.52 C15 C16 C16 C17 C17 C18 C18 C19 DFIX 1.52 C15 C16X C16X C17X C17X C18X C18X C19X DFIX 1.52 C8 C9 C9 C10 C10 C11 C11 C12 DFIX 1.52 C8 C9X C9X C10X C10X C11X C11X C12X SIMU L.S. 25 FMAP 2 PLAN 25 WGHT 0.116600 FVAR 0.28984 0.64998 0.58019 C1 1 0.221489 -0.001257 0.185400 11.00000 0.04716 0.06758 = 0.04316 -0.00104 -0.00145 0.00015 C2 1 0.317716 0.044307 0.170980 11.00000 0.05075 0.08186 = 0.05982 -0.01054 -0.00308 -0.00356 AFIX 23 H2A 2 0.362054 0.042606 0.212936 11.00000 -1.20000 H2B 2 0.344325 -0.002349 0.138856 11.00000 -1.20000 AFIX 0 C3 1 0.316833 0.154667 0.143448 11.00000 0.04862 0.07741 = 0.07207 -0.01300 0.00622 -0.01460 AFIX 23 H3A 2 0.273462 0.157182 0.101061 11.00000 -1.20000 H3B 2 0.290916 0.202280 0.175355 11.00000 -1.20000 AFIX 0 C4 1 0.414337 0.193406 0.130907 11.00000 0.06702 0.11118 = 0.08577 -0.02015 0.01065 -0.03455 AFIX 23 H4B 2 0.456884 0.194188 0.173691 11.00000 -1.20000 H4A 2 0.441609 0.144010 0.100682 11.00000 -1.20000 AFIX 0 C5 1 0.412402 0.300479 0.100736 11.00000 0.09784 0.11703 = 0.15975 0.00479 0.04295 -0.04317 AFIX 137 H5A 2 0.384466 0.349722 0.129972 11.00000 -1.20000 H5B 2 0.373853 0.299355 0.056946 11.00000 -1.20000 H5C 2 0.477626 0.322260 0.095593 11.00000 -1.20000 AFIX 0 C6 1 0.183344 0.055549 0.244070 11.00000 0.07268 0.10950 = 0.04187 -0.00924 0.00346 -0.00629 AFIX 137 H6A 2 0.174933 0.129770 0.233371 11.00000 -1.20000 H6B 2 0.229010 0.047638 0.284398 11.00000 -1.20000 H6C 2 0.121867 0.025308 0.251693 11.00000 -1.20000 AFIX 0 C7 1 0.238605 -0.117652 0.206431 11.00000 0.07329 0.08625 = 0.06559 0.01824 -0.01543 0.00316 AFIX 137 H7A 2 0.284669 -0.121038 0.246835 11.00000 -1.20000 H7B 2 0.263723 -0.155852 0.170352 11.00000 -1.20000 H7C 2 0.178156 -0.149069 0.215295 11.00000 -1.20000 AFIX 0 C8 1 -0.296037 0.076099 0.058938 11.00000 0.04314 0.07937 = 0.06807 -0.00687 0.01200 0.00606 PART 3 C9 1 -0.354288 0.146690 0.006320 31.00000 0.05424 0.11556 = 0.09218 -0.01535 0.00412 0.02885 AFIX 23 H9A 2 -0.367225 0.107803 -0.036170 31.00000 -1.20000 H9B 2 -0.416440 0.163326 0.021756 31.00000 -1.20000 AFIX 0 C10 1 -0.305019 0.244350 -0.005833 31.00000 0.07197 0.11390 = 0.10273 0.01476 -0.00605 0.05688 AFIX 23 H10A 2 -0.254138 0.230418 -0.034294 31.00000 -1.20000 H10B 2 -0.274853 0.273352 0.037075 31.00000 -1.20000 AFIX 0 C11 1 -0.375935 0.323550 -0.040330 31.00000 0.09356 0.12419 = 0.18025 0.08504 0.04571 0.05832 AFIX 23 H11A 2 -0.422961 0.284220 -0.071104 31.00000 -1.20000 H11B 2 -0.411151 0.354226 -0.005593 31.00000 -1.20000 AFIX 0 C12 1 -0.342215 0.407993 -0.077346 31.00000 0.20310 0.11116 = 0.13839 0.07600 0.03534 0.03921 AFIX 137 H12C 2 -0.378326 0.410157 -0.121978 31.00000 -1.20000 H12B 2 -0.274325 0.397866 -0.081236 31.00000 -1.20000 H12A 2 -0.350890 0.473814 -0.054185 31.00000 -1.20000 PART 4 AFIX 0 C9X 1 -0.321068 0.194416 0.050380 -31.00000 0.04563 0.08344 = 0.06707 -0.01714 0.00592 0.00924 AFIX 23 H9C 2 -0.381355 0.205729 0.069725 -31.00000 -1.20000 H9D 2 -0.270852 0.233556 0.078599 -31.00000 -1.20000 AFIX 0 C10X 1 -0.332558 0.245181 -0.017000 -31.00000 0.03330 0.11370 = 0.12469 0.04532 -0.00417 0.02307 AFIX 23 H10C 2 -0.392695 0.212508 -0.037388 -31.00000 -1.20000 H10D 2 -0.282101 0.209027 -0.038162 -31.00000 -1.20000 AFIX 0 C11X 1 -0.337000 0.351684 -0.054905 -31.00000 0.11786 0.11959 = 0.15643 0.03418 0.04056 0.03946 AFIX 23 H11C 2 -0.284456 0.398436 -0.036507 -31.00000 -1.20000 H11D 2 -0.333875 0.341422 -0.103165 -31.00000 -1.20000 AFIX 0 C12X 1 -0.429230 0.392965 -0.042890 -31.00000 0.15050 0.18381 = 0.14248 0.01408 -0.02171 0.06449 AFIX 137 H12D 2 -0.422768 0.429238 0.000133 -31.00000 -1.20000 H12E 2 -0.474894 0.335543 -0.042180 -31.00000 -1.20000 H12F 2 -0.452213 0.441946 -0.078521 -31.00000 -1.20000 PART 0 AFIX 0 C13 1 -0.289471 0.093808 0.132844 11.00000 0.05501 0.21548 = 0.08886 -0.06474 0.03034 -0.02588 AFIX 137 H13A 2 -0.352546 0.112467 0.144715 11.00000 -1.20000 H13B 2 -0.244465 0.150589 0.145641 11.00000 -1.20000 H13C 2 -0.267116 0.029925 0.156412 11.00000 -1.20000 AFIX 0 C14 1 -0.358947 -0.015446 0.041155 11.00000 0.05657 0.17869 = 0.13429 -0.08122 0.04114 -0.03842 AFIX 137 H14A 2 -0.362848 -0.028555 -0.006902 11.00000 -1.20000 H14B 2 -0.422918 -0.001100 0.053025 11.00000 -1.20000 H14C 2 -0.332476 -0.076927 0.065639 11.00000 -1.20000 AFIX 0 C15 1 0.010211 0.326337 0.092652 11.00000 0.05638 0.04578 = 0.04975 -0.00308 0.00620 -0.00242 PART 1 C16 1 0.011918 0.327642 0.170654 21.00000 0.06569 0.06372 = 0.04671 -0.01172 -0.00434 -0.00642 AFIX 23 H16A 2 0.065666 0.283985 0.190889 21.00000 -1.20000 H16B 2 0.023556 0.399888 0.186929 21.00000 -1.20000 AFIX 0 C17 1 -0.082409 0.286956 0.194394 21.00000 0.09381 0.10679 = 0.06099 -0.02211 0.03136 -0.02201 AFIX 23 H17A 2 -0.136761 0.309725 0.161942 21.00000 -1.20000 H17B 2 -0.081394 0.209766 0.194143 21.00000 -1.20000 AFIX 0 C18 1 -0.099514 0.324091 0.264052 21.00000 0.10724 0.15016 = 0.09611 -0.01284 0.03385 -0.02509 AFIX 23 H18A 2 -0.100429 0.401269 0.264986 21.00000 -1.20000 H18B 2 -0.162483 0.298823 0.274027 21.00000 -1.20000 AFIX 0 C19 1 -0.026496 0.286525 0.314095 21.00000 0.12191 0.20768 = 0.11145 -0.02092 0.00668 -0.00338 AFIX 137 H19C 2 -0.048343 0.292667 0.358141 21.00000 -1.20000 H19B 2 0.031594 0.328014 0.313065 21.00000 -1.20000 H19A 2 -0.012887 0.213245 0.305245 21.00000 -1.20000 PART 2 AFIX 0 C16X 1 -0.034299 0.333616 0.157674 -21.00000 0.12387 0.08189 = 0.06858 -0.01870 0.02840 -0.00099 AFIX 23 H16C 2 -0.011662 0.400083 0.178984 -21.00000 -1.20000 H16D 2 -0.103893 0.341473 0.144859 -21.00000 -1.20000 AFIX 0 C17X 1 -0.022623 0.255553 0.209291 -21.00000 0.11096 0.10660 = 0.07994 -0.02248 0.04400 0.00495 AFIX 23 H17C 2 0.047032 0.243736 0.218625 -21.00000 -1.20000 H17D 2 -0.049767 0.190752 0.188111 -21.00000 -1.20000 AFIX 0 C18X 1 -0.057474 0.259819 0.275345 -21.00000 0.11549 0.10750 = 0.05602 -0.02198 -0.00886 -0.00162 AFIX 23 H18C 2 -0.015245 0.216275 0.306901 -21.00000 -1.20000 H18D 2 -0.122156 0.228862 0.271429 -21.00000 -1.20000 AFIX 0 C19X 1 -0.061796 0.369144 0.304541 -21.00000 0.11803 0.13555 = 0.06616 -0.04516 0.01176 0.01663 AFIX 137 H19D 2 -0.047369 0.365714 0.353205 -21.00000 -1.20000 H19E 2 -0.125889 0.398070 0.292711 -21.00000 -1.20000 H19F 2 -0.014908 0.413900 0.286467 -21.00000 -1.20000 PART 0 AFIX 0 C20 1 -0.067446 0.393963 0.053902 11.00000 0.08239 0.05329 = 0.10794 -0.01196 -0.01492 0.01329 AFIX 137 H20A 2 -0.065032 0.464406 0.072846 11.00000 -1.20000 H20B 2 -0.130227 0.363175 0.057173 11.00000 -1.20000 H20C 2 -0.056661 0.397487 0.006944 11.00000 -1.20000 AFIX 0 C21 1 0.106882 0.374637 0.084907 11.00000 0.07083 0.05468 = 0.12526 -0.01793 0.01361 -0.01058 AFIX 137 H21A 2 0.157359 0.335130 0.111579 11.00000 -1.20000 H21B 2 0.108052 0.447149 0.100303 11.00000 -1.20000 H21C 2 0.117385 0.372682 0.037859 11.00000 -1.20000 AFIX 0 C22 1 0.081201 0.244153 -0.147652 11.00000 0.05339 0.04897 = 0.04393 -0.00015 0.00641 -0.00609 C23 1 0.172679 0.299456 -0.114769 11.00000 0.06415 0.06596 = 0.05031 0.00452 0.01314 -0.01937 AFIX 23 H23A 2 0.158797 0.329910 -0.071966 11.00000 -1.20000 H23B 2 0.222753 0.245906 -0.104157 11.00000 -1.20000 AFIX 0 C24 1 0.213445 0.385468 -0.155243 11.00000 0.07293 0.06225 = 0.06365 0.00645 0.01971 -0.01280 AFIX 23 H24A 2 0.230612 0.355554 -0.197352 11.00000 -1.20000 H24B 2 0.163897 0.439271 -0.166856 11.00000 -1.20000 AFIX 0 C25 1 0.300022 0.435680 -0.117848 11.00000 0.09547 0.09731 = 0.08145 0.00393 0.01549 -0.04813 AFIX 23 H25B 2 0.348237 0.381186 -0.104395 11.00000 -1.20000 H25A 2 0.282009 0.468130 -0.076716 11.00000 -1.20000 AFIX 0 C26 1 0.344822 0.519247 -0.158962 11.00000 0.10708 0.10192 = 0.13456 0.01461 0.03558 -0.04719 AFIX 137 H26A 2 0.298225 0.574774 -0.171113 11.00000 -1.20000 H26B 2 0.363491 0.487535 -0.199557 11.00000 -1.20000 H26C 2 0.401285 0.548659 -0.132403 11.00000 -1.20000 AFIX 0 C27 1 0.099077 0.189775 -0.212883 11.00000 0.07734 0.06364 = 0.04381 -0.00021 0.01354 -0.00504 AFIX 137 H27A 2 0.154291 0.143277 -0.204211 11.00000 -1.20000 H27B 2 0.111682 0.242372 -0.245893 11.00000 -1.20000 H27C 2 0.042641 0.149045 -0.230088 11.00000 -1.20000 AFIX 0 C28 1 -0.001473 0.321822 -0.161677 11.00000 0.07421 0.05656 = 0.05796 0.01207 0.01039 0.00317 AFIX 137 H28C 2 -0.059807 0.284243 -0.178828 11.00000 -1.20000 H28B 2 0.013836 0.372892 -0.194856 11.00000 -1.20000 H28A 2 -0.011262 0.357946 -0.120307 11.00000 -1.20000 AFIX 0 O1 3 0.082946 0.116922 0.099545 11.00000 0.04514 0.04885 = 0.04902 -0.00197 0.00166 -0.00095 O2 3 -0.100995 0.141696 0.058029 11.00000 0.04419 0.05048 = 0.04919 -0.00537 0.00787 -0.00077 O3 3 -0.179206 0.030592 -0.044724 11.00000 0.04163 0.06110 = 0.04161 -0.00431 0.00334 0.00443 O4 3 -0.134858 -0.059012 0.072306 11.00000 0.04298 0.05566 = 0.05224 0.00759 0.01123 -0.00061 O5 3 0.027738 0.197391 -0.019418 11.00000 0.05890 0.05118 = 0.04308 -0.00268 0.01309 -0.00508 O6 3 -0.046160 0.080645 -0.120371 11.00000 0.04877 0.05336 = 0.04622 0.00365 0.00346 -0.00767 SI1 4 0.130409 0.002041 0.110470 11.00000 0.03770 0.04793 = 0.03852 -0.00008 0.00247 -0.00038 SI2 4 -0.174418 0.047387 0.035231 11.00000 0.03504 0.05056 = 0.04352 -0.00176 0.00708 0.00119 SI3 4 0.004734 0.191789 0.057403 11.00000 0.04263 0.04246 = 0.04030 -0.00185 0.00724 -0.00103 SI4 4 0.048337 0.142283 -0.088222 11.00000 0.04428 0.04546 = 0.03889 0.00182 0.00746 -0.00355 HKLF 4 REM N. HURKES, -100DEGC, CB REM R1 = 0.0745 for 4615 Fo > 4sig(Fo) and 0.0951 for all 6395 data REM 431 parameters refined using 370 restraints END WGHT 0.1165 0.0000 REM Highest difference peak 0.515, deepest hole -0.547, 1-sigma level 0.089 Q1 1 0.1058 0.0989 0.1093 11.00000 0.05 0.52 Q2 1 0.1818 0.0024 0.1496 11.00000 0.05 0.49 Q3 1 0.0097 0.2696 0.0628 11.00000 0.05 0.47 Q4 1 0.0740 0.1422 0.0930 11.00000 0.05 0.46 Q5 1 0.0165 0.1082 0.0640 11.00000 0.05 0.40 Q6 1 -0.1638 -0.0393 0.0407 11.00000 0.05 0.38 Q7 1 -0.1234 -0.0121 0.0752 11.00000 0.05 0.38 Q8 1 -0.1056 0.0759 0.0623 11.00000 0.05 0.37 Q9 1 -0.1100 -0.0438 0.0913 11.00000 0.05 0.35 Q10 1 0.0274 0.0487 -0.0955 11.00000 0.05 0.34 Q11 1 -0.0152 0.0021 -0.0925 11.00000 0.05 0.30 Q12 1 0.2257 -0.0425 0.1867 11.00000 0.05 0.29 Q13 1 0.0608 0.2021 -0.1467 11.00000 0.05 0.29 Q14 1 -0.1669 -0.0971 0.0668 11.00000 0.05 0.26 Q15 1 -0.0296 0.0303 0.0795 11.00000 0.05 0.26 Q16 1 -0.0208 0.3524 0.0752 11.00000 0.05 0.26 Q17 1 -0.3584 0.1841 -0.0608 11.00000 0.05 0.26 Q18 1 0.1183 0.2728 -0.1338 11.00000 0.05 0.26 Q19 1 0.2961 -0.0609 0.1877 11.00000 0.05 0.25 Q20 1 -0.0606 0.4640 -0.1721 11.00000 0.05 0.25 Q21 1 0.1044 0.0563 0.0518 11.00000 0.05 0.25 Q22 1 -0.1187 0.1187 -0.1396 11.00000 0.05 0.25 Q23 1 -0.3791 0.4659 -0.0970 11.00000 0.05 0.25 Q24 1 -0.1984 0.1745 0.0336 11.00000 0.05 0.24 Q25 1 0.2988 0.1520 0.0899 11.00000 0.05 0.24 ; #---------------------------------- END OF FILE -------------------------