#------------------------------------------------------------------------------ #$Date: 2008-01-13 23:15:36 +0100 (Sun, 13 Jan 2008) $ #$Revision: 14 $ #$URL: svn://www.crystallography.net/cod/cif/2/2003403.cif $ #------------------------------------------------------------------------------ # # This file is available in the Crystallography Open Database (COD), # http://www.crystallography.net/ # # All data on this site have been placed in the public domain by the # contributors. # data_2003403 _journal_name_full 'Acta Crystallographica' _journal_year 1995 _journal_volume C51 _journal_page_first 763 _journal_page_last 766 _publ_section_title ; 1,3-Bis[(3-dimethylethylammonium)propyl]- 1,1,3,3-tetramethyldisiloxane diperchlorate at 163 K and Room Temperature ; _chemical_formula_moiety 'C18 H46 N2 O1 Si2 2+, 2(Cl1 O4 1-)' _chemical_formula_sum 'C18 H46 Cl2 N2 O9 Si2' _chemical_formula_weight 561.6 loop_ _symmetry_equiv_pos_as_xyz 'x,y,z' '1/2-x,y,1/2+z' 'x,1/2-y,1/2+z' '1/2-x,1/2-y,z' '-x,-y,-z' '1/2+x,-y,1/2-z' '-x,1/2+y,1/2-z' '1/2+x,1/2+y,-z' _symmetry_space_group_name_H-M 'P c c n' _cell_length_a 15.676(3) _cell_length_b 16.433(5) _cell_length_c 11.316(3) _cell_angle_alpha 90 _cell_angle_beta 90 _cell_angle_gamma 90 _cell_volume 2915(1) _cell_formula_units_Z 4 _exptl_crystal_density_diffrn 1.280 _exptl_crystal_density_meas ? _diffrn_radiation_type CuK\a _diffrn_radiation_wavelength 1.54178 _cell_measurement_reflns_used 25 _cell_measurement_theta_min 18 _cell_measurement_theta_max 21 _exptl_absorpt_coefficient_mu 3.22 _cell_measurement_temperature 163(2) _exptl_crystal_description needle _exptl_crystal_size_max 0.33 _exptl_crystal_size_mid 0.10 _exptl_crystal_size_min 0.08 _exptl_crystal_colour colourless _chemical_compound_source ; From 0.01 molar solution of N-ethyl-N,N-dimethyl-3-(pentamethyl-disiloxanyl)propylammonium bromide in 0.5 mol/L of sodium perchlorate in the presence of a phosphate buffer to keep the pH value at 7 spontaneously white needles began to crystallize. These white needles were isolated and recrystallized from acetone. ; _diffrn_measurement_device CAD-4 _diffrn_measurement_method 2\q-\w _exptl_absorpt_correction_type refdelf _exptl_absorpt_correction_T_min 0.768 _exptl_absorpt_correction_T_max 1.326 _diffrn_reflns_number 1905 _reflns_number_total 1754 _reflns_number_observed 1384 _reflns_observed_criterion >\s(I) _diffrn_reflns_av_R_equivalents 0.027 _diffrn_reflns_theta_max 54 _diffrn_reflns_limit_h_min 0 _diffrn_reflns_limit_h_max 15 _diffrn_reflns_limit_k_min -1 _diffrn_reflns_limit_k_max 17 _diffrn_reflns_limit_l_min 0 _diffrn_reflns_limit_l_max 11 _reflns_limit_h_min ? _reflns_limit_h_max ? _reflns_limit_k_min ? _reflns_limit_k_max ? _reflns_limit_l_min ? _reflns_limit_l_max ? _diffrn_standards_number 2 _diffrn_standards_interval_time 30 _diffrn_standards_decay_% -9.0 _refine_ls_structure_factor_coef F _refine_ls_R_factor_obs 0.060 _refine_ls_wR_factor_obs 0.045 _refine_ls_wR_factor_all ? _refine_ls_goodness_of_fit_obs 2.69 _refine_ls_goodness_of_fit_all ? _refine_ls_number_reflns 1384 _refine_ls_number_parameters 206 _refine_ls_hydrogen_treatment refall _refine_ls_weighting_scheme sigma _refine_ls_shift/esd_max 0.17 _refine_diff_density_max 0.45 _refine_diff_density_min -0.32 _refine_ls_extinction_method 'none' _refine_ls_extinction_coef ? _atom_type_symbol ? _atom_type_scat_source 'IntTabC' _atom_type_scat_dispersion_real ? _atom_type_scat_dispersion_imag ? _refine_ls_abs_structure_details ? _refine_ls_abs_structure_Flack ? loop_ _atom_site_label _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv Si 0.28358(10) 0.16194(9) 0.48136(14) 0.0395(5) O1 0.25 0.25 0.5285(4) 0.0370(16) N4 0.1098(3) -0.1132(2) 0.3475(4) 0.0313(16) C1 0.1857(3) 0.0972(3) 0.4661(5) 0.046(2) C2 0.1990(3) 0.0120(3) 0.4124(5) 0.039(2) C3 0.1127(3) -0.0293(3) 0.4059(5) 0.0367(19) C5 0.1231(3) -0.1016(3) 0.2169(4) 0.0430(19) C6 0.1251(4) -0.1765(4) 0.1476(5) 0.072(3) C11 0.3567(4) 0.1177(3) 0.5924(6) 0.066(3) C12 0.3399(4) 0.1736(3) 0.3371(6) 0.065(3) C41 0.1768(3) -0.1667(3) 0.4026(5) 0.044(2) C42 0.0241(3) -0.1492(3) 0.3710(5) 0.047(2) Cl 0.09065(8) 0.59475(8) 0.25081(12) 0.0374(4) O11 0.10327 0.64153 0.35620 0.0823(19) O12 0.02468 0.63184 0.17896 0.0643(17) O13 0.06576 0.51342 0.27803 0.105(2) O14 0.17051 0.59501 0.18613 0.104(2) H11 0.144(2) 0.131(2) 0.410(4) 0.09(3) H12 0.160(3) 0.099(3) 0.545(4) 0.16(4) H21 0.254(4) -0.016(3) 0.477(4) 0.20(4) H22 0.221(3) 0.014(3) 0.317(4) 0.15(4) H31 0.091(2) -0.034(2) 0.479(3) 0.07(3) H32 0.066(3) 0.011(3) 0.341(4) 0.13(3) H51 0.158(3) -0.055(3) 0.183(4) 0.19(4) H52 0.077(3) -0.073(2) 0.163(4) 0.11(3) H61 0.16964 -0.21002 0.17533 0.195 H62 0.07169 -0.20541 0.15913 0.195 H63 0.13146 -0.16529 0.06686 0.195 H111 0.37847 0.06527 0.56424 0.1405 H112 0.40680 0.15177 0.60229 0.1405 H113 0.33093 0.10985 0.66547 0.1405 H121 0.36305 0.12345 0.31035 0.1435 H122 0.30569 0.19714 0.27895 0.1435 H123 0.39001 0.21049 0.34765 0.1435 H411 0.165(2) -0.220(2) 0.382(3) 0.06(3) H412 0.232(3) -0.147(3) 0.377(4) 0.17(4) H413 0.173(3) -0.172(3) 0.499(4) 0.12(3) H421 0.019(3) -0.218(3) 0.329(4) 0.21(4) H422 0.015(2) -0.163(2) 0.440(3) 0.06(3) H423 -0.020(3) -0.115(2) 0.326(4) 0.12(3) loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_12 _atom_site_aniso_U_13 _atom_site_aniso_U_22 _atom_site_aniso_U_23 _atom_site_aniso_U_33 Si 0.0455(10) 0.0007(8) -0.0018(9) 0.0329(8) 0.0019(8) 0.0400(9) O1 0.049(3) 0 0 0.026(2) 0.000(3) 0.036(3) N4 0.026(3) 0.001(2) 0.001(2) 0.032(2) 0.000(2) 0.036(3) C1 0.050(4) -0.004(3) 0.007(3) 0.037(3) -0.001(3) 0.050(4) C2 0.038(4) 0.001(3) 0.002(3) 0.032(3) -0.005(3) 0.046(4) C3 0.039(4) -0.002(3) 0.006(3) 0.035(3) 0.002(3) 0.036(3) C5 0.058(4) -0.001(3) 0.004(3) 0.043(3) -0.006(3) 0.028(3) C6 0.087(5) -0.010(4) -0.005(4) 0.084(5) -0.012(5) 0.044(4) C11 0.073(5) 0.007(4) -0.020(4) 0.057(4) 0.012(4) 0.068(4) C12 0.073(5) -0.002(4) 0.032(4) 0.049(4) 0.011(4) 0.074(4) C41 0.044(4) -0.002(3) -0.005(3) 0.025(3) 0.003(3) 0.064(4) C42 0.036(4) 0.005(3) 0.002(3) 0.061(4) -0.008(3) 0.044(4) Cl 0.0358(7) -0.0047(8) -0.0045(7) 0.0421(6) -0.0057(7) 0.0343(7) O11 0.105(4) -0.028(3) -0.018(3) 0.086(3) -0.012(3) 0.056(3) O12 0.050(3) 0.018(2) -0.014(2) 0.078(3) 0.004(2) 0.065(3) O13 0.091(4) 0.023(3) -0.059(4) 0.039(2) -0.009(3) 0.185(5) O14 0.052(3) 0.008(4) -0.004(3) 0.209(5) 0.014(4) 0.052(3)