#------------------------------------------------------------------------------ #$Date: 2008-01-26 14:05:32 +0100 (Sat, 26 Jan 2008) $ #$Revision: 19 $ #$URL: svn://www.crystallography.net/cod/cif/2/2003402.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_2003402 _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 16.154(3) _cell_length_b 16.483(6) _cell_length_c 11.454(6) _cell_angle_alpha 90.00 _cell_angle_beta 90.00 _cell_angle_gamma 90.00 _cell_volume 3050(2) _cell_formula_units_Z 4 _exptl_crystal_density_diffrn 1.223 _exptl_crystal_density_meas ? _diffrn_radiation_type 'MoK\a' _diffrn_radiation_wavelength 0.71069 _cell_measurement_reflns_used 59 _cell_measurement_theta_min 5 _cell_measurement_theta_max 20 _exptl_absorpt_coefficient_mu 0.329 _cell_measurement_temperature 293(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 a 0.01 molar solution of N-ethyl-N,N-dimethyl-3-(pentamethyldisiloxanyl)propylammonium bromide in 0.5 mol l^-1^ of sodium perchlorate in the presence of a phosphate buffer to keep the pH value at 7, white needles spontaneously began to crystallize. These white needles were isolated and recrystallized from acetone. ; _diffrn_measurement_device 'Huber 4-circle diffractometer' _diffrn_measurement_method 2\q-\w _exptl_absorpt_correction_type none _exptl_absorpt_correction_T_min ? _exptl_absorpt_correction_T_max ? _diffrn_reflns_number 2319 _reflns_number_total 2291 _reflns_number_observed 928 _reflns_observed_criterion '>\s(I)' _diffrn_reflns_av_R_equivalents ? _diffrn_reflns_theta_max 23.5 _diffrn_reflns_limit_h_min 0 _diffrn_reflns_limit_h_max 16 _diffrn_reflns_limit_k_min 0 _diffrn_reflns_limit_k_max 18 _diffrn_reflns_limit_l_min 0 _diffrn_reflns_limit_l_max 12 _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 90 _diffrn_standards_decay_% -4.0 _refine_ls_structure_factor_coef F _refine_ls_R_factor_obs 0.082 _refine_ls_wR_factor_obs 0.062 _refine_ls_wR_factor_all ? _refine_ls_goodness_of_fit_obs 4.02 _refine_ls_goodness_of_fit_all ? _refine_ls_number_reflns 928 _refine_ls_number_parameters 150 _refine_ls_hydrogen_treatment noref _refine_ls_weighting_scheme 'sigma' _refine_ls_shift/esd_max 0.27 _refine_diff_density_max 0.30 _refine_diff_density_min -0.34 _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 ? ; GENEV, GENSIN and GENTAN of the XTAL2.2 program system (Hall & Stewart, 1987) ; ; PLUTON92 (Spek, 1992) and SCHAKAL92 (Keller, 1992) ; loop_ _atom_site_label _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv Si 0.2807(2) 0.16140(17) 0.4637(3) 0.0885(10) O1 0.25 0.25 0.5069(6) 0.081(3) N4 0.1088(5) -0.1146(4) 0.3481(6) 0.086(3) C1 0.1849(6) 0.0981(5) 0.4517(9) 0.102(4) C2 0.1946(6) 0.0124(5) 0.4036(9) 0.099(5) C3 0.1135(6) -0.0318(6) 0.4011(8) 0.085(4) C5 0.1231(7) -0.1061(9) 0.2193(8) 0.165(6) C6 0.1062(11) -0.1491(12) 0.1453(10) 0.308(12) C11 0.3507(7) 0.1188(7) 0.5740(10) 0.143(6) C12 0.3328(7) 0.1712(7) 0.3198(9) 0.126(5) C41 0.1705(7) -0.1673(6) 0.4047(10) 0.112(5) C42 0.0245(6) -0.1501(7) 0.3728(9) 0.118(5) Cl 0.09239(16) 0.59656(15) 0.2538(2) 0.0919(9) O11 0.1111(6) 0.6317(6) 0.3508(7) 0.212(5) O12 0.0307(5) 0.6343(6) 0.1932(7) 0.185(5) O13 0.0735(7) 0.5229(5) 0.2675(13) 0.297(7) O14 0.1580(6) 0.5982(9) 0.1931(7) 0.291(7) H11 0.14380 0.12803 0.40411 0.2624 H12 0.15824 0.09566 0.52964 0.2624 H21 0.23627 -0.01662 0.45027 0.2677 H22 0.21962 0.01543 0.32511 0.2677 H31 0.09416 -0.03398 0.48154 0.2228 H32 0.07481 0.00337 0.36025 0.2228 H51 0.18394 -0.09774 0.21384 0.4505 H52 0.10035 -0.05218 0.20164 0.4505 H61 0.12378 -0.13719 0.07123 0.7051 H62 0.15182 -0.19588 0.16945 0.7051 H63 0.05893 -0.17392 0.15599 0.7051 H111 0.40205 0.14820 0.57888 0.3155 H112 0.32648 0.11681 0.64921 0.3155 H113 0.3664 0.06254 0.55394 0.3155 H121 0.38529 0.20086 0.32868 0.3009 H122 0.35015 0.11717 0.29151 0.3009 H123 0.30097 0.19576 0.26426 0.3009 H411 0.17168 -0.2215 0.37681 0.2907 H412 0.22675 -0.14561 0.39641 0.2907 H413 0.16259 -0.17097 0.49035 0.2907 H421 0.01884 -0.20508 0.34013 0.275 H422 0.0123 -0.15533 0.45473 0.275 H423 -0.01966 -0.11887 0.33829 0.275 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 0.109(2) 0.004(2) 0.000(2) 0.0612(15) 0.008(2) 0.0953(18) O1 0.117(7) 0 0 0.046(4) 0.000(6) 0.080(6) N4 0.073(6) -0.015(5) -0.012(5) 0.080(6) -0.003(5) 0.104(6) C1 0.116(9) -0.002(8) 0.030(7) 0.053(6) -0.009(7) 0.136(8) C2 0.088(8) 0.011(7) 0.009(7) 0.059(7) 0.005(7) 0.150(9) C3 0.081(8) 0.000(6) 0.003(6) 0.076(7) 0.009(7) 0.099(7) C5 0.148(11) -0.081(8) 0.028(7) 0.281(14) -0.089(10) 0.067(7) C6 0.36(2) -0.035(13) -0.001(11) 0.50(3) -0.235(18) 0.064(8) C11 0.145(10) 0.014(9) -0.050(9) 0.141(11) 0.035(9) 0.143(10) C12 0.114(9) 0.001(9) 0.042(8) 0.113(9) 0.002(9) 0.152(10) C41 0.113(9) -0.008(8) -0.004(8) 0.048(6) 0.017(8) 0.175(10) C42 0.065(8) -0.027(9) -0.010(7) 0.138(10) -0.024(8) 0.150(9) Cl 0.0992(18) -0.0072(19) -0.0104(19) 0.0800(15) -0.003(2) 0.0966(15) O11 0.261(11) -0.099(6) -0.045(7) 0.239(10) -0.007(9) 0.135(6) O12 0.146(7) 0.038(7) -0.065(6) 0.226(10) 0.051(7) 0.183(7) O13 0.270(10) 0.028(10) -0.159(12) 0.065(5) -0.022(8) 0.556(17) O14 0.114(7) 0.054(11) 0.010(6) 0.64(2) 0.018(12) 0.120(7)