# Supplementary Material (ESI) for New Journal of Chemistry # This journal is © The Royal Society of Chemistry and # The Centre National de la Recherche Scientifique, 2003 data_global #=============================================================================== _audit_creation_date 08-09-02 _journal_coden_Cambridge 440 loop_ _publ_author_name 'Le Floch,Pascal' 'Christian Defieber' 'Nicolas Maigrot' 'Nicolas Mezailles' 'Audrey Moores' 'Louis Ricard' _publ_contact_author_name 'Dr Pascal Le Floch' _publ_contact_author_address ; Department de Chimie Ecole Polytechnique Laboratoire Heteroelements et Coord UMR CNRS 7653 (DCPH) Palaiseau cedex 91128 FRANCE ; _publ_contact_author_email LEFLOCH@POLY.POLYTECHNIQUE.FR _publ_requested_journal 'New Journal of Chemistry' _publ_section_title ; Siloxa-bridged-cyclophanes featuring benzene, thiophene and pyridine units ; _publ_section_exptl_prep ; All structures were solved using SIR97 (Altomare et al.) and refined with SHELXL97 (Sheldrick). Figures were drawn with Platon (Spek, 1990). ; _publ_section_references ; Altomare, A., Cascarano, G., Giacovazzo, C. & Guagliardi, A. (1993) J. Appl. Cryst. 26, 343-350. Sheldrick, G.M. SHELXL97. Program for crystal structure refinement. University of G\\"ottingen, Germany, 1997. Sluis, P. v.d., Spek, A.L. (1990). Acta Cryst. A46, 194-201. Spek, A.L. (1990). Acta Cryst. A46, C-34. ; #=============================================================================== data_compound_2 _database_code_CSD 203273 _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C20 H32 O2 Si4' _chemical_formula_weight 416.82 loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source C C .0033 .0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' H H .0000 .0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' O O .0106 .0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Si Si .0817 .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 ' loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, -y, -z' _cell_length_a 8.7122(2) _cell_length_b 12.4992(2) _cell_length_c 12.9229(3) _cell_angle_alpha 63.9270(10) _cell_angle_beta 71.7420(10) _cell_angle_gamma 73.1410(10) _cell_volume 1181.11(4) _cell_formula_units_Z 2 _cell_measurement_temperature 150.0(10) _cell_measurement_reflns_used 251 _cell_measurement_theta_min 3.0 _cell_measurement_theta_max 20.0 _exptl_crystal_description cube _exptl_crystal_colour colorless _exptl_crystal_size_max 0.20 _exptl_crystal_size_mid 0.20 _exptl_crystal_size_min 0.20 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.172 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 448 _exptl_absorpt_coefficient_mu 0.263 _exptl_absorpt_correction_type ? _exptl_absorpt_correction_T_min 0.9492 _exptl_absorpt_correction_T_max 0.9492 _exptl_absorpt_process_details ? _exptl_special_details ; ? ; _diffrn_ambient_temperature 150.0(10) _diffrn_radiation_wavelength 0.71069 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type KappaCCD _diffrn_measurement_method 'phi and omega scans' _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 7700 _diffrn_reflns_av_R_equivalents 0.0188 _diffrn_reflns_av_sigmaI/netI 0.0366 _diffrn_reflns_limit_h_min -10 _diffrn_reflns_limit_h_max 11 _diffrn_reflns_limit_k_min -15 _diffrn_reflns_limit_k_max 16 _diffrn_reflns_limit_l_min -16 _diffrn_reflns_limit_l_max 16 _diffrn_reflns_theta_min 2.50 _diffrn_reflns_theta_max 27.46 _reflns_number_total 5298 _reflns_number_gt 4730 _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^)+(0.0528P)^2^+0.3568P] 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_number_reflns 5298 _refine_ls_number_parameters 243 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0361 _refine_ls_R_factor_gt 0.0317 _refine_ls_wR_factor_ref 0.0990 _refine_ls_wR_factor_gt 0.0949 _refine_ls_goodness_of_fit_ref 1.034 _refine_ls_restrained_S_all 1.034 _refine_ls_shift/su_max 0.002 _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 0.59188(4) 1.11661(3) 0.18033(3) 0.02061(10) Uani 1 1 d . . . Si2 Si 0.71981(4) 1.24797(3) 0.28914(3) 0.02004(10) Uani 1 1 d . . . Si3 Si 0.17944(4) 0.76436(3) 0.28130(3) 0.01836(10) Uani 1 1 d . . . Si4 Si 0.03154(4) 0.63555(3) 0.18221(3) 0.01942(10) Uani 1 1 d . . . O1 O 0.69877(13) 1.18516(9) 0.20800(8) 0.0300(2) Uani 1 1 d . . . O2 O 0.08837(13) 0.73545(9) 0.20557(8) 0.0286(2) Uani 1 1 d . . . C1 C 0.49554(16) 1.00468(11) 0.32285(11) 0.0201(2) Uani 1 1 d . . . C2 C 0.34952(16) 1.04327(12) 0.39196(12) 0.0255(3) Uani 1 1 d . . . H2 H 0.2942 1.1246 0.3618 0.031 Uiso 1 1 calc R . . C3 C 0.28387(16) 0.96568(12) 0.50337(12) 0.0262(3) Uani 1 1 d . . . H3 H 0.1845 0.9952 0.5476 0.031 Uiso 1 1 calc R . . C4 C 0.35978(15) 0.84516(11) 0.55251(11) 0.0207(3) Uani 1 1 d . . . C5 C 0.50261(16) 0.80520(12) 0.48227(11) 0.0246(3) Uani 1 1 d . . . H5 H 0.5559 0.7232 0.5116 0.030 Uiso 1 1 calc R . . C6 C 0.56855(16) 0.88304(12) 0.37024(12) 0.0245(3) Uani 1 1 d . . . H6 H 0.6657 0.8527 0.3248 0.029 Uiso 1 1 calc R . . C7 C 0.73608(19) 1.04011(13) 0.08307(12) 0.0309(3) Uani 1 1 d . . . H7A H 0.7894 1.1001 0.0112 0.046 Uiso 1 1 calc R . . H7B H 0.6753 1.0005 0.0620 0.046 Uiso 1 1 calc R . . H7C H 0.8196 0.9794 0.1246 0.046 Uiso 1 1 calc R . . C8 C 0.42794(19) 1.23012(14) 0.10664(13) 0.0362(3) Uani 1 1 d . . . H8A H 0.3541 1.2697 0.1594 0.054 Uiso 1 1 calc R . . H8B H 0.3655 1.1896 0.0879 0.054 Uiso 1 1 calc R . . H8C H 0.4778 1.2910 0.0337 0.054 Uiso 1 1 calc R . . C9 C 0.60047(18) 1.40463(12) 0.24862(13) 0.0317(3) Uani 1 1 d . . . H9A H 0.6394 1.4514 0.1647 0.048 Uiso 1 1 calc R . . H9B H 0.6153 1.4429 0.2959 0.048 Uiso 1 1 calc R . . H9C H 0.4838 1.4023 0.2639 0.048 Uiso 1 1 calc R . . C10 C 0.94129(17) 1.24903(13) 0.25984(14) 0.0307(3) Uani 1 1 d . . . H10A H 1.0022 1.1658 0.2810 0.046 Uiso 1 1 calc R . . H10B H 0.9586 1.2862 0.3071 0.046 Uiso 1 1 calc R . . H10C H 0.9804 1.2957 0.1759 0.046 Uiso 1 1 calc R . . C11 C 0.12999(15) 0.65864(11) 0.43941(11) 0.0194(2) Uani 1 1 d . . . C12 C 0.24579(16) 0.56468(12) 0.49571(12) 0.0246(3) Uani 1 1 d . . . H12 H 0.3580 0.5585 0.4559 0.030 Uiso 1 1 calc R . . C13 C 0.20031(16) 0.47949(12) 0.60936(12) 0.0241(3) Uani 1 1 d . . . H13 H 0.2822 0.4164 0.6449 0.029 Uiso 1 1 calc R . . C14 C 0.03714(15) 0.48506(11) 0.67177(11) 0.0194(2) Uani 1 1 d . . . C15 C -0.07739(16) 0.58157(12) 0.61586(12) 0.0254(3) Uani 1 1 d . . . H15 H -0.1892 0.5894 0.6564 0.030 Uiso 1 1 calc R . . C16 C -0.03256(16) 0.66596(12) 0.50324(11) 0.0248(3) Uani 1 1 d . . . H16 H -0.1141 0.7303 0.4686 0.030 Uiso 1 1 calc R . . C17 C 0.09791(19) 0.92359(12) 0.26594(13) 0.0309(3) Uani 1 1 d . . . H17A H 0.1266 0.9773 0.1829 0.046 Uiso 1 1 calc R . . H17B H 0.1458 0.9428 0.3136 0.046 Uiso 1 1 calc R . . H17C H -0.0219 0.9350 0.2931 0.046 Uiso 1 1 calc R . . C18 C 0.40452(16) 0.74327(13) 0.22281(12) 0.0295(3) Uani 1 1 d . . . H18A H 0.4451 0.6609 0.2242 0.044 Uiso 1 1 calc R . . H18B H 0.4583 0.7558 0.2718 0.044 Uiso 1 1 calc R . . H18C H 0.4292 0.8019 0.1415 0.044 Uiso 1 1 calc R . . C19 C 0.20600(19) 0.56915(14) 0.08947(13) 0.0344(3) Uani 1 1 d . . . H19A H 0.2355 0.6322 0.0115 0.052 Uiso 1 1 calc R . . H19B H 0.1742 0.5049 0.0809 0.052 Uiso 1 1 calc R . . H19C H 0.3005 0.5352 0.1270 0.052 Uiso 1 1 calc R . . C20 C -0.13804(18) 0.71472(13) 0.10269(13) 0.0300(3) Uani 1 1 d . . . H20A H -0.2300 0.7510 0.1509 0.045 Uiso 1 1 calc R . . H20B H -0.1743 0.6567 0.0876 0.045 Uiso 1 1 calc R . . H20C H -0.0995 0.7784 0.0275 0.045 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 0.0253(2) 0.02262(18) 0.01591(18) -0.00711(14) -0.00464(14) -0.00744(14) Si2 0.02178(18) 0.02223(18) 0.01807(19) -0.00791(14) -0.00273(14) -0.00814(14) Si3 0.01995(18) 0.01941(17) 0.01645(18) -0.00583(13) -0.00366(13) -0.00653(13) Si4 0.02165(19) 0.02171(18) 0.01553(18) -0.00474(14) -0.00539(13) -0.00716(14) O1 0.0400(6) 0.0369(5) 0.0200(5) -0.0114(4) -0.0009(4) -0.0220(4) O2 0.0405(6) 0.0294(5) 0.0201(5) -0.0027(4) -0.0105(4) -0.0189(4) C1 0.0238(6) 0.0234(6) 0.0173(6) -0.0081(5) -0.0058(5) -0.0081(5) C2 0.0267(7) 0.0235(6) 0.0243(7) -0.0081(5) -0.0061(5) -0.0029(5) C3 0.0239(6) 0.0292(7) 0.0230(7) -0.0109(5) -0.0021(5) -0.0028(5) C4 0.0237(6) 0.0240(6) 0.0189(6) -0.0092(5) -0.0051(5) -0.0085(5) C5 0.0282(7) 0.0222(6) 0.0220(6) -0.0086(5) -0.0038(5) -0.0042(5) C6 0.0245(6) 0.0268(6) 0.0214(6) -0.0111(5) -0.0014(5) -0.0044(5) C7 0.0399(8) 0.0307(7) 0.0211(7) -0.0107(6) -0.0027(6) -0.0076(6) C8 0.0370(8) 0.0352(8) 0.0269(8) -0.0027(6) -0.0104(6) -0.0040(6) C9 0.0322(7) 0.0294(7) 0.0268(7) -0.0070(6) -0.0050(6) -0.0035(6) C10 0.0249(7) 0.0325(7) 0.0368(8) -0.0150(6) -0.0025(6) -0.0097(6) C11 0.0218(6) 0.0215(6) 0.0169(6) -0.0066(5) -0.0045(5) -0.0078(5) C12 0.0192(6) 0.0294(7) 0.0213(6) -0.0062(5) -0.0032(5) -0.0058(5) C13 0.0218(6) 0.0255(6) 0.0222(6) -0.0056(5) -0.0068(5) -0.0037(5) C14 0.0228(6) 0.0218(6) 0.0165(6) -0.0071(5) -0.0047(5) -0.0079(5) C15 0.0204(6) 0.0299(7) 0.0210(6) -0.0056(5) -0.0027(5) -0.0063(5) C16 0.0211(6) 0.0268(6) 0.0218(6) -0.0050(5) -0.0057(5) -0.0032(5) C17 0.0391(8) 0.0242(6) 0.0271(7) -0.0100(6) -0.0058(6) -0.0038(6) C18 0.0234(6) 0.0354(7) 0.0239(7) -0.0071(6) -0.0023(5) -0.0066(5) C19 0.0360(8) 0.0330(7) 0.0228(7) -0.0063(6) -0.0001(6) -0.0036(6) C20 0.0305(7) 0.0326(7) 0.0265(7) -0.0047(6) -0.0130(6) -0.0085(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 O1 1.6339(10) . ? Si1 C7 1.8555(14) . ? Si1 C8 1.8572(15) . ? Si1 C1 1.8712(13) . ? Si2 O1 1.6362(9) . ? Si2 C10 1.8491(14) . ? Si2 C9 1.8570(14) . ? Si2 C4 1.8731(13) 2_676 ? Si3 O2 1.6375(9) . ? Si3 C17 1.8510(13) . ? Si3 C18 1.8528(14) . ? Si3 C11 1.8740(13) . ? Si4 O2 1.6368(9) . ? Si4 C20 1.8513(14) . ? Si4 C19 1.8537(15) . ? Si4 C14 1.8727(13) 2_566 ? C1 C6 1.3986(18) . ? C1 C2 1.3998(18) . ? C2 C3 1.3852(19) . ? C3 C4 1.3980(18) . ? C4 C5 1.3971(18) . ? C4 Si2 1.8731(13) 2_676 ? C5 C6 1.3919(19) . ? C11 C12 1.3958(18) . ? C11 C16 1.3977(17) . ? C12 C13 1.3975(18) . ? C13 C14 1.3963(18) . ? C14 C15 1.4001(18) . ? C14 Si4 1.8727(13) 2_566 ? C15 C16 1.3844(18) . ? 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 C7 107.16(6) . . ? O1 Si1 C8 109.25(7) . . ? C7 Si1 C8 111.03(7) . . ? O1 Si1 C1 108.92(5) . . ? C7 Si1 C1 111.18(6) . . ? C8 Si1 C1 109.25(6) . . ? O1 Si2 C10 107.20(6) . . ? O1 Si2 C9 109.52(6) . . ? C10 Si2 C9 110.67(7) . . ? O1 Si2 C4 107.95(5) . 2_676 ? C10 Si2 C4 111.29(6) . 2_676 ? C9 Si2 C4 110.12(6) . 2_676 ? O2 Si3 C17 107.32(6) . . ? O2 Si3 C18 110.16(6) . . ? C17 Si3 C18 110.01(7) . . ? O2 Si3 C11 108.29(5) . . ? C17 Si3 C11 110.79(6) . . ? C18 Si3 C11 110.22(6) . . ? O2 Si4 C20 107.89(6) . . ? O2 Si4 C19 109.73(7) . . ? C20 Si4 C19 109.13(7) . . ? O2 Si4 C14 108.46(5) . 2_566 ? C20 Si4 C14 111.17(6) . 2_566 ? C19 Si4 C14 110.42(6) . 2_566 ? Si1 O1 Si2 150.23(7) . . ? Si4 O2 Si3 148.71(7) . . ? C6 C1 C2 116.67(12) . . ? C6 C1 Si1 123.17(10) . . ? C2 C1 Si1 119.98(9) . . ? C3 C2 C1 121.54(12) . . ? C2 C3 C4 121.83(12) . . ? C5 C4 C3 116.80(12) . . ? C5 C4 Si2 123.61(10) . 2_676 ? C3 C4 Si2 119.27(9) . 2_676 ? C6 C5 C4 121.39(12) . . ? C5 C6 C1 121.71(12) . . ? C12 C11 C16 116.99(11) . . ? C12 C11 Si3 123.26(10) . . ? C16 C11 Si3 119.53(9) . . ? C11 C12 C13 121.46(12) . . ? C14 C13 C12 121.44(12) . . ? C13 C14 C15 116.67(11) . . ? C13 C14 Si4 122.60(10) . 2_566 ? C15 C14 Si4 120.56(9) . 2_566 ? C16 C15 C14 121.94(12) . . ? C15 C16 C11 121.45(12) . . ? _diffrn_measured_fraction_theta_max .981 _diffrn_reflns_theta_full 27.46 _diffrn_measured_fraction_theta_full .981 _refine_diff_density_max .411 _refine_diff_density_min -.324 _refine_diff_density_rms .047 #===END data_compound_3 _database_code_CSD 203274 _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C24 H42 O3 Si6' _chemical_formula_weight 547.12 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 'P21/c ' loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, y+1/2, -z+1/2' '-x, -y, -z' 'x, -y-1/2, z-1/2' _cell_length_a 17.0411(3) _cell_length_b 12.0953(2) _cell_length_c 16.9900(2) _cell_angle_alpha 90.00 _cell_angle_beta 114.0700(10) _cell_angle_gamma 90.00 _cell_volume 3197.43(9) _cell_formula_units_Z 4 _cell_measurement_temperature 150.0(10) _cell_measurement_reflns_used 251 _cell_measurement_theta_min 3.0 _cell_measurement_theta_max 20.0 _exptl_crystal_description cube _exptl_crystal_colour colorless _exptl_crystal_size_max 0.20 _exptl_crystal_size_mid 0.20 _exptl_crystal_size_min 0.20 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.137 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1176 _exptl_absorpt_coefficient_mu 0.283 _exptl_absorpt_correction_type ? _exptl_absorpt_correction_T_min 0.9456 _exptl_absorpt_correction_T_max 0.9456 _exptl_absorpt_process_details ? _exptl_special_details ; ? ; _diffrn_ambient_temperature 150.0(10) _diffrn_radiation_wavelength 0.71069 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type KappaCCD _diffrn_measurement_method 'phi and omega scans' _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 15394 _diffrn_reflns_av_R_equivalents 0.0212 _diffrn_reflns_av_sigmaI/netI 0.0420 _diffrn_reflns_limit_h_min -23 _diffrn_reflns_limit_h_max 23 _diffrn_reflns_limit_k_min -16 _diffrn_reflns_limit_k_max 14 _diffrn_reflns_limit_l_min -23 _diffrn_reflns_limit_l_max 23 _diffrn_reflns_theta_min 2.77 _diffrn_reflns_theta_max 29.98 _reflns_number_total 9244 _reflns_number_gt 7331 _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^)+(0.0530P)^2^+0.9174P] 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_number_reflns 9244 _refine_ls_number_parameters 310 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0529 _refine_ls_R_factor_gt 0.0388 _refine_ls_wR_factor_ref 0.1104 _refine_ls_wR_factor_gt 0.1027 _refine_ls_goodness_of_fit_ref 1.022 _refine_ls_restrained_S_all 1.022 _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 0.32872(3) -0.08695(3) 0.33809(2) 0.02640(9) Uani 1 1 d . . . Si2 Si 0.25813(2) -0.08823(3) 0.48282(2) 0.02426(9) Uani 1 1 d . . . Si3 Si 0.32581(2) 0.37076(3) 0.53923(2) 0.02409(9) Uani 1 1 d . . . Si4 Si 0.39923(2) 0.37480(3) 0.39692(2) 0.02392(9) Uani 1 1 d . . . Si5 Si 0.08186(2) 0.23503(3) 0.14116(2) 0.02312(9) Uani 1 1 d . . . Si6 Si 0.00625(2) 0.22783(3) 0.28352(2) 0.02407(9) Uani 1 1 d . . . O1 O 0.28837(9) -0.12337(10) 0.40647(8) 0.0498(3) Uani 1 1 d . . . O2 O 0.38896(6) 0.38223(9) 0.48826(6) 0.0298(2) Uani 1 1 d . . . O3 O 0.02465(7) 0.24657(12) 0.19792(6) 0.0468(3) Uani 1 1 d . . . C1 C 0.30009(9) 0.06093(11) 0.30542(8) 0.0226(2) Uani 1 1 d . . . C2 C 0.22057(9) 0.08850(11) 0.23918(8) 0.0230(3) Uani 1 1 d . . . H2 H 0.1834 0.0305 0.2078 0.028 Uiso 1 1 calc R . . C3 C 0.19377(8) 0.19787(11) 0.21735(8) 0.0215(2) Uani 1 1 d . . . C4 C 0.25057(8) 0.28135(11) 0.26410(8) 0.0232(3) Uani 1 1 d . . . H4 H 0.2340 0.3562 0.2498 0.028 Uiso 1 1 calc R . . C5 C 0.33032(9) 0.25975(11) 0.33065(8) 0.0228(3) Uani 1 1 d . . . C6 C 0.35335(9) 0.14846(12) 0.35000(8) 0.0237(3) Uani 1 1 d . . . H6 H 0.4074 0.1318 0.3953 0.028 Uiso 1 1 calc R . . C7 C 0.21809(8) 0.05782(11) 0.46357(8) 0.0223(2) Uani 1 1 d . . . C8 C 0.13730(8) 0.08360(11) 0.39871(8) 0.0222(3) Uani 1 1 d . . . H8 H 0.1002 0.0249 0.3686 0.027 Uiso 1 1 calc R . . C9 C 0.10935(8) 0.19260(11) 0.37678(8) 0.0212(2) Uani 1 1 d . . . C10 C 0.16591(8) 0.27713(11) 0.42288(8) 0.0228(3) Uani 1 1 d . . . H10 H 0.1482 0.3518 0.4091 0.027 Uiso 1 1 calc R . . C11 C 0.24693(8) 0.25635(11) 0.48803(8) 0.0221(3) Uani 1 1 d . . . C12 C 0.27094(8) 0.14558(11) 0.50711(8) 0.0229(3) Uani 1 1 d . . . H12 H 0.3256 0.1296 0.5516 0.027 Uiso 1 1 calc R . . C13 C 0.28308(11) -0.18054(14) 0.24376(11) 0.0392(4) Uani 1 1 d . . . H13A H 0.2971 -0.2573 0.2628 0.059 Uiso 1 1 calc R . . H13B H 0.3075 -0.1622 0.2022 0.059 Uiso 1 1 calc R . . H13C H 0.2205 -0.1716 0.2165 0.059 Uiso 1 1 calc R . . C14 C 0.44704(11) -0.10447(16) 0.38820(12) 0.0470(4) Uani 1 1 d . . . H14A H 0.4716 -0.0583 0.4400 0.070 Uiso 1 1 calc R . . H14B H 0.4710 -0.0822 0.3471 0.070 Uiso 1 1 calc R . . H14C H 0.4610 -0.1822 0.4040 0.070 Uiso 1 1 calc R . . C15 C 0.34904(11) -0.09985(15) 0.58975(11) 0.0428(4) Uani 1 1 d . . . H15A H 0.3670 -0.1773 0.6009 0.064 Uiso 1 1 calc R . . H15B H 0.3310 -0.0735 0.6344 0.064 Uiso 1 1 calc R . . H15C H 0.3972 -0.0549 0.5906 0.064 Uiso 1 1 calc R . . C16 C 0.17197(10) -0.18467(14) 0.47838(11) 0.0388(4) Uani 1 1 d . . . H16A H 0.1235 -0.1791 0.4219 0.058 Uiso 1 1 calc R . . H16B H 0.1526 -0.1654 0.5236 0.058 Uiso 1 1 calc R . . H16C H 0.1942 -0.2605 0.4873 0.058 Uiso 1 1 calc R . . C17 C 0.39581(10) 0.33928(15) 0.65279(9) 0.0361(3) Uani 1 1 d . . . H17A H 0.4277 0.2709 0.6556 0.054 Uiso 1 1 calc R . . H17B H 0.3605 0.3300 0.6856 0.054 Uiso 1 1 calc R . . H17C H 0.4364 0.4002 0.6774 0.054 Uiso 1 1 calc R . . C18 C 0.26650(11) 0.50275(13) 0.53000(12) 0.0396(4) Uani 1 1 d . . . H18A H 0.3074 0.5620 0.5586 0.059 Uiso 1 1 calc R . . H18B H 0.2263 0.4944 0.5575 0.059 Uiso 1 1 calc R . . H18C H 0.2346 0.5213 0.4690 0.059 Uiso 1 1 calc R . . C19 C 0.51370(10) 0.34773(16) 0.42149(11) 0.0405(4) Uani 1 1 d . . . H19A H 0.5487 0.4095 0.4548 0.061 Uiso 1 1 calc R . . H19B H 0.5212 0.3399 0.3675 0.061 Uiso 1 1 calc R . . H19C H 0.5318 0.2794 0.4551 0.061 Uiso 1 1 calc R . . C20 C 0.36597(13) 0.50866(14) 0.33930(11) 0.0461(4) Uani 1 1 d . . . H20A H 0.3071 0.5261 0.3316 0.069 Uiso 1 1 calc R . . H20B H 0.3684 0.5033 0.2828 0.069 Uiso 1 1 calc R . . H20C H 0.4048 0.5672 0.3731 0.069 Uiso 1 1 calc R . . C21 C 0.03418(11) 0.12659(14) 0.05874(10) 0.0397(4) Uani 1 1 d . . . H21A H 0.0373 0.0552 0.0872 0.060 Uiso 1 1 calc R . . H21B H 0.0660 0.1222 0.0221 0.060 Uiso 1 1 calc R . . H21C H -0.0260 0.1448 0.0232 0.060 Uiso 1 1 calc R . . C22 C 0.08031(10) 0.36988(13) 0.08901(10) 0.0349(3) Uani 1 1 d . . . H22A H 0.0211 0.3885 0.0504 0.052 Uiso 1 1 calc R . . H22B H 0.1156 0.3653 0.0558 0.052 Uiso 1 1 calc R . . H22C H 0.1035 0.4272 0.1333 0.052 Uiso 1 1 calc R . . C23 C -0.03809(11) 0.35909(14) 0.30484(11) 0.0378(3) Uani 1 1 d . . . H23A H 0.0056 0.4172 0.3192 0.057 Uiso 1 1 calc R . . H23B H -0.0547 0.3487 0.3532 0.057 Uiso 1 1 calc R . . H23C H -0.0886 0.3807 0.2533 0.057 Uiso 1 1 calc R . . C24 C -0.07574(11) 0.11805(15) 0.26253(12) 0.0441(4) Uani 1 1 d . . . H24A H -0.1258 0.1348 0.2091 0.066 Uiso 1 1 calc R . . H24B H -0.0934 0.1146 0.3106 0.066 Uiso 1 1 calc R . . H24C H -0.0514 0.0467 0.2567 0.066 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 0.0358(2) 0.02066(19) 0.02866(19) 0.00064(14) 0.01918(17) 0.00306(15) Si2 0.0302(2) 0.02005(19) 0.02665(18) 0.00246(14) 0.01579(16) 0.00221(14) Si3 0.02755(19) 0.0239(2) 0.02455(17) -0.00613(14) 0.01444(15) -0.00488(14) Si4 0.03011(19) 0.02263(19) 0.02233(17) -0.00459(14) 0.01406(15) -0.00688(15) Si5 0.02504(18) 0.0278(2) 0.01788(16) -0.00039(14) 0.01013(14) -0.00145(14) Si6 0.02213(18) 0.0321(2) 0.02025(17) 0.00224(14) 0.01100(14) 0.00087(15) O1 0.0929(10) 0.0251(6) 0.0602(8) 0.0106(5) 0.0607(8) 0.0151(6) O2 0.0346(5) 0.0339(6) 0.0264(5) -0.0097(4) 0.0182(4) -0.0128(4) O3 0.0240(5) 0.0973(11) 0.0213(5) 0.0106(6) 0.0114(4) 0.0083(6) C1 0.0286(6) 0.0211(6) 0.0218(6) -0.0009(5) 0.0141(5) -0.0010(5) C2 0.0276(6) 0.0220(6) 0.0227(6) -0.0033(5) 0.0138(5) -0.0036(5) C3 0.0253(6) 0.0227(6) 0.0202(5) -0.0022(5) 0.0129(5) -0.0019(5) C4 0.0288(7) 0.0216(6) 0.0232(6) -0.0018(5) 0.0146(5) -0.0008(5) C5 0.0286(6) 0.0227(6) 0.0208(6) -0.0035(5) 0.0138(5) -0.0037(5) C6 0.0267(6) 0.0257(7) 0.0210(6) -0.0015(5) 0.0121(5) -0.0017(5) C7 0.0271(6) 0.0213(6) 0.0227(6) 0.0000(5) 0.0144(5) 0.0010(5) C8 0.0266(6) 0.0222(6) 0.0209(6) -0.0016(5) 0.0128(5) -0.0012(5) C9 0.0242(6) 0.0236(6) 0.0187(5) 0.0003(5) 0.0118(5) 0.0002(5) C10 0.0280(6) 0.0204(6) 0.0242(6) 0.0011(5) 0.0148(5) 0.0010(5) C11 0.0249(6) 0.0220(6) 0.0232(6) -0.0026(5) 0.0138(5) -0.0025(5) C12 0.0229(6) 0.0246(7) 0.0230(6) -0.0003(5) 0.0113(5) 0.0010(5) C13 0.0466(9) 0.0261(8) 0.0446(9) -0.0066(7) 0.0183(8) 0.0008(7) C14 0.0413(9) 0.0387(10) 0.0515(10) 0.0013(8) 0.0093(8) 0.0088(8) C15 0.0330(8) 0.0377(9) 0.0464(9) 0.0044(7) 0.0047(7) 0.0051(7) C16 0.0377(8) 0.0279(8) 0.0468(9) 0.0046(7) 0.0131(7) -0.0037(6) C17 0.0369(8) 0.0484(10) 0.0250(6) -0.0050(7) 0.0148(6) -0.0071(7) C18 0.0407(9) 0.0264(8) 0.0559(10) -0.0116(7) 0.0239(8) -0.0045(7) C19 0.0336(8) 0.0474(10) 0.0468(9) -0.0163(8) 0.0230(7) -0.0120(7) C20 0.0695(12) 0.0267(8) 0.0363(8) 0.0007(7) 0.0156(8) -0.0094(8) C21 0.0474(9) 0.0324(9) 0.0277(7) -0.0022(6) 0.0036(7) -0.0051(7) C22 0.0379(8) 0.0288(8) 0.0391(8) 0.0041(6) 0.0169(7) 0.0034(6) C23 0.0382(8) 0.0350(9) 0.0386(8) 0.0065(7) 0.0140(7) 0.0096(7) C24 0.0322(8) 0.0403(10) 0.0559(10) -0.0024(8) 0.0141(8) -0.0045(7) _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 1.6335(11) . ? Si1 C14 1.8533(18) . ? Si1 C13 1.8543(16) . ? Si1 C1 1.8774(14) . ? Si2 O1 1.6353(11) . ? Si2 C15 1.8506(17) . ? Si2 C16 1.8525(16) . ? Si2 C7 1.8737(14) . ? Si3 O2 1.6393(9) . ? Si3 C17 1.8475(15) . ? Si3 C18 1.8617(17) . ? Si3 C11 1.8774(13) . ? Si4 O2 1.6335(9) . ? Si4 C19 1.8500(16) . ? Si4 C20 1.8569(17) . ? Si4 C5 1.8720(14) . ? Si5 O3 1.6331(10) . ? Si5 C21 1.8475(16) . ? Si5 C22 1.8512(16) . ? Si5 C3 1.8711(14) . ? Si6 O3 1.6238(10) . ? Si6 C24 1.8536(17) . ? Si6 C23 1.8563(17) . ? Si6 C9 1.8731(13) . ? C1 C6 1.3991(19) . ? C1 C2 1.4036(19) . ? C2 C3 1.3992(19) . ? C3 C4 1.4001(18) . ? C4 C5 1.3929(19) . ? C5 C6 1.4032(19) . ? C7 C12 1.3934(19) . ? C7 C8 1.4035(18) . ? C8 C9 1.3996(19) . ? C9 C10 1.4043(19) . ? C10 C11 1.3958(19) . ? C11 C12 1.3998(18) . ? 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 C14 109.70(8) . . ? O1 Si1 C13 107.47(8) . . ? C14 Si1 C13 108.75(8) . . ? O1 Si1 C1 109.47(6) . . ? C14 Si1 C1 110.34(8) . . ? C13 Si1 C1 111.05(7) . . ? O1 Si2 C15 110.52(8) . . ? O1 Si2 C16 107.76(8) . . ? C15 Si2 C16 108.93(8) . . ? O1 Si2 C7 108.46(6) . . ? C15 Si2 C7 110.02(7) . . ? C16 Si2 C7 111.13(7) . . ? O2 Si3 C17 106.60(6) . . ? O2 Si3 C18 109.49(7) . . ? C17 Si3 C18 111.21(8) . . ? O2 Si3 C11 108.53(5) . . ? C17 Si3 C11 111.55(7) . . ? C18 Si3 C11 109.36(7) . . ? O2 Si4 C19 107.88(7) . . ? O2 Si4 C20 108.96(7) . . ? C19 Si4 C20 109.89(9) . . ? O2 Si4 C5 109.17(5) . . ? C19 Si4 C5 110.43(7) . . ? C20 Si4 C5 110.45(7) . . ? O3 Si5 C21 108.92(8) . . ? O3 Si5 C22 108.17(7) . . ? C21 Si5 C22 110.29(7) . . ? O3 Si5 C3 107.30(5) . . ? C21 Si5 C3 111.28(7) . . ? C22 Si5 C3 110.75(7) . . ? O3 Si6 C24 109.48(8) . . ? O3 Si6 C23 107.34(7) . . ? C24 Si6 C23 108.38(8) . . ? O3 Si6 C9 109.40(5) . . ? C24 Si6 C9 111.91(7) . . ? C23 Si6 C9 110.21(7) . . ? Si1 O1 Si2 148.68(8) . . ? Si4 O2 Si3 147.66(7) . . ? Si6 O3 Si5 153.75(8) . . ? C6 C1 C2 117.08(12) . . ? C6 C1 Si1 121.86(10) . . ? C2 C1 Si1 120.86(10) . . ? C3 C2 C1 122.77(12) . . ? C2 C3 C4 117.13(12) . . ? C2 C3 Si5 122.74(10) . . ? C4 C3 Si5 119.54(10) . . ? C5 C4 C3 123.03(13) . . ? C4 C5 C6 117.20(12) . . ? C4 C5 Si4 120.92(10) . . ? C6 C5 Si4 121.69(10) . . ? C1 C6 C5 122.79(13) . . ? C12 C7 C8 117.53(12) . . ? C12 C7 Si2 121.00(10) . . ? C8 C7 Si2 121.15(10) . . ? C9 C8 C7 122.45(12) . . ? C8 C9 C10 117.12(12) . . ? C8 C9 Si6 122.64(10) . . ? C10 C9 Si6 119.98(10) . . ? C11 C10 C9 122.89(12) . . ? C10 C11 C12 117.21(12) . . ? C10 C11 Si3 121.63(10) . . ? C12 C11 Si3 120.79(10) . . ? C7 C12 C11 122.80(13) . . ? _diffrn_measured_fraction_theta_max 0.995 _diffrn_reflns_theta_full 29.98 _diffrn_measured_fraction_theta_full 0.995 _refine_diff_density_max 0.668 _refine_diff_density_min -0.453 _refine_diff_density_rms 0.053 #===END data_compound_11 _database_code_CSD 203275 _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C16 H28 O2 S2 Si4' _chemical_formula_weight 428.86 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' S S 0.1246 0.1234 '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 loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, -y, -z' _cell_length_a 6.7411(2) _cell_length_b 8.2744(2) _cell_length_c 11.44040(10) _cell_angle_alpha 72.939(2) _cell_angle_beta 72.984(2) _cell_angle_gamma 73.3800(10) _cell_volume 569.18(2) _cell_formula_units_Z 1 _cell_measurement_temperature 150.0(10) _cell_measurement_reflns_used 251 _cell_measurement_theta_min 3.0 _cell_measurement_theta_max 20.0 _exptl_crystal_description needle _exptl_crystal_colour colorless _exptl_crystal_size_max 0.22 _exptl_crystal_size_mid 0.16 _exptl_crystal_size_min 0.16 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.251 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 228 _exptl_absorpt_coefficient_mu 0.452 _exptl_absorpt_correction_type ? _exptl_absorpt_correction_T_min 0.9072 _exptl_absorpt_correction_T_max 0.9312 _exptl_absorpt_process_details ? _exptl_special_details ; ? ; _diffrn_ambient_temperature 150.0(10) _diffrn_radiation_wavelength 0.71069 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type KappaCCD _diffrn_measurement_method 'phi and omega scans' _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 4544 _diffrn_reflns_av_R_equivalents 0.0277 _diffrn_reflns_av_sigmaI/netI 0.0523 _diffrn_reflns_limit_h_min -9 _diffrn_reflns_limit_h_max 6 _diffrn_reflns_limit_k_min -11 _diffrn_reflns_limit_k_max 11 _diffrn_reflns_limit_l_min -16 _diffrn_reflns_limit_l_max 16 _diffrn_reflns_theta_min 3.37 _diffrn_reflns_theta_max 30.01 _reflns_number_total 3296 _reflns_number_gt 2782 _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^)+(0.0445P)^2^+0.1347P] 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_number_reflns 3296 _refine_ls_number_parameters 113 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0429 _refine_ls_R_factor_gt 0.0346 _refine_ls_wR_factor_ref 0.0967 _refine_ls_wR_factor_gt 0.0893 _refine_ls_goodness_of_fit_ref 1.026 _refine_ls_restrained_S_all 1.026 _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 S1 S 0.07138(6) 0.27490(4) 0.55029(3) 0.01894(10) Uani 1 1 d . . . Si1 Si 0.03042(6) 0.34478(5) 0.81490(3) 0.01894(11) Uani 1 1 d . . . Si2 Si 0.12536(6) 0.70936(5) 0.67371(3) 0.01759(11) Uani 1 1 d . . . O1 O 0.14716(17) 0.50876(12) 0.75733(9) 0.0216(2) Uani 1 1 d . . . C1 C -0.1441(2) 0.29150(17) 0.49214(12) 0.0187(3) Uani 1 1 d . . . C2 C -0.3264(2) 0.32571(18) 0.58199(13) 0.0220(3) Uani 1 1 d . . . H2 H -0.4641 0.3379 0.5701 0.026 Uiso 1 1 calc R . . C3 C -0.2917(2) 0.34128(18) 0.69416(13) 0.0218(3) Uani 1 1 d . . . H3 H -0.4036 0.3658 0.7639 0.026 Uiso 1 1 calc R . . C4 C -0.0804(2) 0.31744(17) 0.69247(12) 0.0191(3) Uani 1 1 d . . . C5 C 0.2322(3) 0.1498(2) 0.86454(15) 0.0305(4) Uani 1 1 d . . . H5A H 0.3459 0.1267 0.7913 0.046 Uiso 1 1 calc R . . H5B H 0.1653 0.0501 0.9023 0.046 Uiso 1 1 calc R . . H5C H 0.2921 0.1695 0.9263 0.046 Uiso 1 1 calc R . . C6 C -0.1960(3) 0.3886(2) 0.94862(14) 0.0315(4) Uani 1 1 d . . . H6A H -0.1429 0.4005 1.0161 0.047 Uiso 1 1 calc R . . H6B H -0.2692 0.2923 0.9798 0.047 Uiso 1 1 calc R . . H6C H -0.2955 0.4960 0.9206 0.047 Uiso 1 1 calc R . . C7 C 0.3561(3) 0.78508(19) 0.67742(14) 0.0243(3) Uani 1 1 d . . . H7A H 0.3538 0.7798 0.7645 0.037 Uiso 1 1 calc R . . H7B H 0.3486 0.9048 0.6284 0.037 Uiso 1 1 calc R . . H7C H 0.4879 0.7108 0.6413 0.037 Uiso 1 1 calc R . . C8 C -0.1322(2) 0.8431(2) 0.73874(14) 0.0258(3) Uani 1 1 d . . . H8A H -0.2485 0.8015 0.7304 0.039 Uiso 1 1 calc R . . H8B H -0.1408 0.9642 0.6926 0.039 Uiso 1 1 calc R . . H8C H -0.1437 0.8344 0.8277 0.039 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 S1 0.01832(18) 0.02082(18) 0.01830(17) -0.00543(12) -0.00376(13) -0.00466(13) Si1 0.0237(2) 0.01772(19) 0.01605(18) -0.00298(14) -0.00467(15) -0.00618(16) Si2 0.0193(2) 0.01699(19) 0.01827(18) -0.00445(14) -0.00495(15) -0.00550(15) O1 0.0270(6) 0.0190(5) 0.0208(5) -0.0028(4) -0.0078(4) -0.0074(4) C1 0.0205(7) 0.0167(6) 0.0199(6) -0.0026(5) -0.0068(5) -0.0049(5) C2 0.0196(7) 0.0229(7) 0.0233(6) -0.0033(5) -0.0054(5) -0.0058(6) C3 0.0213(7) 0.0222(7) 0.0200(6) -0.0052(5) -0.0021(5) -0.0044(6) C4 0.0215(7) 0.0166(6) 0.0189(6) -0.0047(5) -0.0029(5) -0.0045(5) C5 0.0366(9) 0.0233(7) 0.0305(8) 0.0007(6) -0.0138(7) -0.0056(7) C6 0.0359(10) 0.0370(9) 0.0219(7) -0.0095(6) 0.0003(6) -0.0125(7) C7 0.0245(8) 0.0238(7) 0.0273(7) -0.0066(5) -0.0066(6) -0.0076(6) C8 0.0237(8) 0.0254(7) 0.0281(7) -0.0085(6) -0.0044(6) -0.0043(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 S1 C1 1.7229(14) . ? S1 C4 1.7240(14) . ? Si1 O1 1.6362(10) . ? Si1 C5 1.8534(16) . ? Si1 C6 1.8556(16) . ? Si1 C4 1.8617(14) . ? Si2 O1 1.6440(10) . ? Si2 C8 1.8492(16) . ? Si2 C7 1.8505(15) . ? Si2 C1 1.8664(13) 2_566 ? C1 C2 1.371(2) . ? C1 Si2 1.8665(13) 2_566 ? C2 C3 1.417(2) . ? C2 H2 0.9500 . ? C3 C4 1.376(2) . ? C3 H3 0.9500 . ? 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 H8A 0.9800 . ? C8 H8B 0.9800 . ? C8 H8C 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 C1 S1 C4 94.43(7) . . ? O1 Si1 C5 107.69(7) . . ? O1 Si1 C6 110.08(7) . . ? C5 Si1 C6 111.41(8) . . ? O1 Si1 C4 109.27(6) . . ? C5 Si1 C4 111.17(7) . . ? C6 Si1 C4 107.22(7) . . ? O1 Si2 C8 109.50(6) . . ? O1 Si2 C7 107.02(6) . . ? C8 Si2 C7 112.81(7) . . ? O1 Si2 C1 108.41(6) . 2_566 ? C8 Si2 C1 110.71(7) . 2_566 ? C7 Si2 C1 108.23(7) . 2_566 ? Si1 O1 Si2 144.49(7) . . ? C2 C1 S1 108.85(10) . . ? C2 C1 Si2 126.83(11) . 2_566 ? S1 C1 Si2 123.89(8) . 2_566 ? C1 C2 C3 114.17(13) . . ? C1 C2 H2 122.9 . . ? C3 C2 H2 122.9 . . ? C4 C3 C2 113.62(13) . . ? C4 C3 H3 123.2 . . ? C2 C3 H3 123.2 . . ? C3 C4 S1 108.92(10) . . ? C3 C4 Si1 126.94(11) . . ? S1 C4 Si1 123.93(8) . . ? Si1 C5 H5A 109.5 . . ? Si1 C5 H5B 109.5 . . ? H5A C5 H5B 109.5 . . ? Si1 C5 H5C 109.5 . . ? H5A C5 H5C 109.5 . . ? H5B C5 H5C 109.5 . . ? Si1 C6 H6A 109.5 . . ? Si1 C6 H6B 109.5 . . ? H6A C6 H6B 109.5 . . ? Si1 C6 H6C 109.5 . . ? H6A C6 H6C 109.5 . . ? H6B C6 H6C 109.5 . . ? Si2 C7 H7A 109.5 . . ? Si2 C7 H7B 109.5 . . ? H7A C7 H7B 109.5 . . ? Si2 C7 H7C 109.5 . . ? H7A C7 H7C 109.5 . . ? H7B C7 H7C 109.5 . . ? Si2 C8 H8A 109.5 . . ? Si2 C8 H8B 109.5 . . ? H8A C8 H8B 109.5 . . ? Si2 C8 H8C 109.5 . . ? H8A C8 H8C 109.5 . . ? H8B C8 H8C 109.5 . . ? _diffrn_measured_fraction_theta_max 0.990 _diffrn_reflns_theta_full 30.01 _diffrn_measured_fraction_theta_full 0.990 _refine_diff_density_max 0.405 _refine_diff_density_min -0.390 _refine_diff_density_rms 0.067 #===END data_compound_13 _database_code_CSD 203276 _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C22 H40 Br2 N2 O3 Si4' _chemical_formula_weight 652.74 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' Br Br -0.2901 2.4595 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' N N 0.0061 0.0033 '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' H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting Orthorhombic _symmetry_space_group_name_H-M 'Pnma ' loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x+1/2, -y, z+1/2' 'x+1/2, -y+1/2, -z+1/2' '-x, y+1/2, -z' '-x, -y, -z' 'x-1/2, y, -z-1/2' '-x-1/2, y-1/2, z-1/2' 'x, -y-1/2, z' _cell_length_a 23.444(5) _cell_length_b 12.699(5) _cell_length_c 10.521(5) _cell_angle_alpha 90.00 _cell_angle_beta 90.00 _cell_angle_gamma 90.00 _cell_volume 3132(2) _cell_formula_units_Z 4 _cell_measurement_temperature 150.0(10) _cell_measurement_reflns_used 251 _cell_measurement_theta_min 3.0 _cell_measurement_theta_max 20.0 _exptl_crystal_description needle _exptl_crystal_colour colorless _exptl_crystal_size_max 0.22 _exptl_crystal_size_mid 0.12 _exptl_crystal_size_min 0.12 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.384 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1344 _exptl_absorpt_coefficient_mu 2.765 _exptl_absorpt_correction_type ? _exptl_absorpt_correction_T_min 0.5814 _exptl_absorpt_correction_T_max 0.7326 _exptl_absorpt_process_details ? _exptl_special_details ; ? ; _diffrn_ambient_temperature 150.0(10) _diffrn_radiation_wavelength 0.71069 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type KappaCCD _diffrn_measurement_method 'phi and omega scans' _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 6591 _diffrn_reflns_av_R_equivalents 0.0249 _diffrn_reflns_av_sigmaI/netI 0.0435 _diffrn_reflns_limit_h_min -29 _diffrn_reflns_limit_h_max 29 _diffrn_reflns_limit_k_min -16 _diffrn_reflns_limit_k_max 16 _diffrn_reflns_limit_l_min -13 _diffrn_reflns_limit_l_max 13 _diffrn_reflns_theta_min 3.98 _diffrn_reflns_theta_max 27.08 _reflns_number_total 3592 _reflns_number_gt 2757 _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^)+(0.0705P)^2^+2.5812P] 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_number_reflns 3592 _refine_ls_number_parameters 140 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0621 _refine_ls_R_factor_gt 0.0455 _refine_ls_wR_factor_ref 0.1388 _refine_ls_wR_factor_gt 0.1331 _refine_ls_goodness_of_fit_ref 1.082 _refine_ls_restrained_S_all 1.082 _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 -0.05841(4) -0.12700(8) -0.19587(10) 0.0374(3) Uani 1 1 d . . . Si4 Si -0.26857(4) -0.12711(8) -0.45151(9) 0.0364(3) Uani 1 1 d . . . O1 O -0.07381(13) -0.2500 -0.2259(3) 0.0328(7) Uani 1 2 d S . . O2 O -0.24841(14) -0.2500 -0.4447(3) 0.0348(8) Uani 1 2 d S . . N1 N -0.16055(12) -0.0951(2) -0.3348(3) 0.0318(6) Uani 1 1 d . . . H1N H -0.1718(17) -0.148(3) -0.298(4) 0.038 Uiso 1 1 d . . . C1 C -0.10905(15) -0.0536(3) -0.3057(3) 0.0358(8) Uani 1 1 d . . . C2 C -0.0964(2) 0.0422(3) -0.3615(4) 0.0537(11) Uani 1 1 d . . . H2 H -0.0609 0.0751 -0.3445 0.064 Uiso 1 1 calc R . . C3 C -0.1347(2) 0.0901(4) -0.4409(5) 0.0677(14) Uani 1 1 d . . . H3 H -0.1252 0.1557 -0.4789 0.081 Uiso 1 1 calc R . . C4 C -0.1867(2) 0.0445(3) -0.4665(4) 0.0511(10) Uani 1 1 d . . . H4 H -0.2131 0.0790 -0.5207 0.061 Uiso 1 1 calc R . . C5 C -0.20031(16) -0.0530(3) -0.4125(3) 0.0345(8) Uani 1 1 d . . . C6 C 0.01490(18) -0.0950(4) -0.2474(5) 0.0680(13) Uani 1 1 d . . . H6A H 0.0423 -0.1301 -0.1913 0.102 Uiso 1 1 calc R . . H6B H 0.0207 -0.0187 -0.2434 0.102 Uiso 1 1 calc R . . H6C H 0.0206 -0.1194 -0.3349 0.102 Uiso 1 1 calc R . . C7 C -0.0724(2) -0.0896(4) -0.0292(4) 0.0584(12) Uani 1 1 d . . . H7A H -0.1104 -0.1144 -0.0042 0.088 Uiso 1 1 calc R . . H7B H -0.0707 -0.0128 -0.0209 0.088 Uiso 1 1 calc R . . H7C H -0.0436 -0.1217 0.0260 0.088 Uiso 1 1 calc R . . C8 C -0.32426(18) -0.0969(4) -0.3342(4) 0.0566(11) Uani 1 1 d . . . H8A H -0.3611 -0.1230 -0.3650 0.085 Uiso 1 1 calc R . . H8B H -0.3264 -0.0205 -0.3218 0.085 Uiso 1 1 calc R . . H8C H -0.3150 -0.1310 -0.2533 0.085 Uiso 1 1 calc R . . C9 C -0.2896(2) -0.0906(4) -0.6143(4) 0.0592(12) Uani 1 1 d . . . H9A H -0.2593 -0.1111 -0.6737 0.089 Uiso 1 1 calc R . . H9B H -0.2955 -0.0143 -0.6190 0.089 Uiso 1 1 calc R . . H9C H -0.3250 -0.1269 -0.6369 0.089 Uiso 1 1 calc R . . Br1 Br -0.21586(2) -0.2500 -0.11578(5) 0.03730(17) Uani 1 2 d S . . Br2 Br -0.06388(3) -0.7500 -0.09296(7) 0.0637(2) Uani 1 2 d S . . 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 0.0260(5) 0.0395(5) 0.0465(6) -0.0028(4) -0.0072(4) -0.0045(4) Si4 0.0294(5) 0.0423(6) 0.0374(5) 0.0035(4) -0.0065(4) 0.0061(4) O1 0.0212(16) 0.0345(17) 0.0429(18) 0.000 -0.0033(14) 0.000 O2 0.0321(19) 0.0378(18) 0.0345(17) 0.000 -0.0057(14) 0.000 N1 0.0303(15) 0.0278(14) 0.0372(15) 0.0037(12) -0.0014(12) 0.0003(12) C1 0.0312(18) 0.0338(17) 0.0425(18) -0.0049(15) 0.0013(15) -0.0027(15) C2 0.053(3) 0.043(2) 0.065(3) 0.009(2) -0.006(2) -0.016(2) C3 0.080(4) 0.041(2) 0.082(3) 0.025(2) -0.009(3) -0.015(2) C4 0.060(3) 0.039(2) 0.054(2) 0.0127(19) -0.010(2) 0.004(2) C5 0.0375(19) 0.0340(17) 0.0319(16) 0.0011(14) -0.0004(14) 0.0048(15) C6 0.028(2) 0.070(3) 0.106(4) 0.007(3) -0.003(2) -0.017(2) C7 0.058(3) 0.070(3) 0.048(2) -0.015(2) -0.017(2) 0.009(2) C8 0.033(2) 0.074(3) 0.063(3) -0.005(2) 0.0012(19) 0.016(2) C9 0.055(3) 0.068(3) 0.054(2) 0.021(2) -0.022(2) -0.002(2) Br1 0.0334(3) 0.0408(3) 0.0378(3) 0.000 0.0048(2) 0.000 Br2 0.0457(4) 0.0642(4) 0.0813(5) 0.000 -0.0115(3) 0.000 _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 1.6339(15) . ? Si1 C7 1.846(4) . ? Si1 C6 1.848(4) . ? Si1 C1 1.901(4) . ? Si4 O2 1.6322(15) . ? Si4 C8 1.837(4) . ? Si4 C9 1.842(4) . ? Si4 C5 1.901(4) . ? O1 Si1 1.6339(15) 8 ? O2 Si4 1.6322(15) 8 ? N1 C5 1.351(4) . ? N1 C1 1.353(4) . ? N1 H1N 0.82(4) . ? C1 C2 1.382(5) . ? C2 C3 1.368(6) . ? C2 H2 0.9500 . ? C3 C4 1.376(6) . ? C3 H3 0.9500 . ? C4 C5 1.398(5) . ? C4 H4 0.9500 . ? 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 H8A 0.9800 . ? C8 H8B 0.9800 . ? C8 H8C 0.9800 . ? C9 H9A 0.9800 . ? C9 H9B 0.9800 . ? C9 H9C 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 C7 113.0(2) . . ? O1 Si1 C6 111.0(2) . . ? C7 Si1 C6 112.8(2) . . ? O1 Si1 C1 102.33(16) . . ? C7 Si1 C1 109.90(18) . . ? C6 Si1 C1 107.1(2) . . ? O2 Si4 C8 112.1(2) . . ? O2 Si4 C9 111.0(2) . . ? C8 Si4 C9 112.5(2) . . ? O2 Si4 C5 102.73(16) . . ? C8 Si4 C5 110.46(19) . . ? C9 Si4 C5 107.50(19) . . ? Si1 O1 Si1 145.9(2) . 8 ? Si4 O2 Si4 145.9(2) . 8 ? C5 N1 C1 126.7(3) . . ? C5 N1 H1N 113(3) . . ? C1 N1 H1N 120(3) . . ? N1 C1 C2 116.0(3) . . ? N1 C1 Si1 120.2(3) . . ? C2 C1 Si1 123.8(3) . . ? C3 C2 C1 120.7(4) . . ? C3 C2 H2 119.7 . . ? C1 C2 H2 119.7 . . ? C2 C3 C4 120.8(4) . . ? C2 C3 H3 119.6 . . ? C4 C3 H3 119.6 . . ? C3 C4 C5 119.7(4) . . ? C3 C4 H4 120.1 . . ? C5 C4 H4 120.1 . . ? N1 C5 C4 116.0(4) . . ? N1 C5 Si4 121.0(3) . . ? C4 C5 Si4 122.9(3) . . ? Si1 C6 H6A 109.5 . . ? Si1 C6 H6B 109.5 . . ? H6A C6 H6B 109.5 . . ? Si1 C6 H6C 109.5 . . ? H6A C6 H6C 109.5 . . ? H6B C6 H6C 109.5 . . ? Si1 C7 H7A 109.5 . . ? Si1 C7 H7B 109.5 . . ? H7A C7 H7B 109.5 . . ? Si1 C7 H7C 109.5 . . ? H7A C7 H7C 109.5 . . ? H7B C7 H7C 109.5 . . ? Si4 C8 H8A 109.5 . . ? Si4 C8 H8B 109.5 . . ? H8A C8 H8B 109.5 . . ? Si4 C8 H8C 109.5 . . ? H8A C8 H8C 109.5 . . ? H8B C8 H8C 109.5 . . ? Si4 C9 H9A 109.5 . . ? Si4 C9 H9B 109.5 . . ? H9A C9 H9B 109.5 . . ? Si4 C9 H9C 109.5 . . ? H9A C9 H9C 109.5 . . ? H9B C9 H9C 109.5 . . ? _diffrn_measured_fraction_theta_max 0.995 _diffrn_reflns_theta_full 27.08 _diffrn_measured_fraction_theta_full 0.995 _refine_diff_density_max 0.925 _refine_diff_density_min -0.601 _refine_diff_density_rms 0.086 #===END