#------------------------------------------------------------------------------ #$Date: 2008-01-26 14:05:32 +0100 (Sat, 26 Jan 2008) $ #$Revision: 19 $ #$URL: svn://www.crystallography.net/cod/cif/2/2003255.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_2003255 _journal_name_full 'Acta Crystallographica' _journal_year 1995 _journal_volume C51 _journal_page_first 471 _journal_page_last 473 _publ_section_title ; 4-[(Trimethylsilyl)methyl]tetracyclo[5.4.0.0^6,10^.0^9,11^]undec-3-yl 3,5-Dinitrobenzoate ; _chemical_formula_sum 'C22 H28 N2 O6 Si' _chemical_formula_weight 444.55 loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x+1/2, -y, z+1/2' '-x, y+1/2, -z+1/2' 'x+1/2, -y+1/2, -z' _symmetry_space_group_name_H-M 'P 21 21 21' _cell_length_a 11.408(2) _cell_length_b 11.495(2) _cell_length_c 17.672(4) _cell_angle_alpha 90.00 _cell_angle_beta 90.00 _cell_angle_gamma 90.00 _cell_volume 2317.4(8) _cell_formula_units_Z 4 _exptl_crystal_density_diffrn 1.274 _exptl_crystal_density_meas ? _exptl_crystal_density_method ? _diffrn_radiation_type MoK\a _diffrn_radiation_wavelength 0.71073 _cell_measurement_reflns_used 22 _cell_measurement_theta_min 20.0 _cell_measurement_theta_max 26.5 _exptl_absorpt_coefficient_mu 0.141 _cell_measurement_temperature 293(2) _exptl_crystal_description 'plate' _exptl_crystal_size_max 0.35 _exptl_crystal_size_mid 0.30 _exptl_crystal_size_min 0.12 _exptl_crystal_colour 'colourless' _chemical_compound_source ? _diffrn_measurement_device 'Enraf-Nonius CAD4' _diffrn_measurement_method '\w-2\q scans' _exptl_absorpt_correction_type 'none' _exptl_absorpt_correction_T_min ? _exptl_absorpt_correction_T_max ? _diffrn_reflns_number 5019 _reflns_number_total 4552 _reflns_number_observed 2909 _reflns_observed_criterion >2sigma(I) _diffrn_reflns_av_R_equivalents 0.0247 _diffrn_reflns_theta_max 26.0 _diffrn_reflns_limit_h_min -14 _diffrn_reflns_limit_h_max 14 _diffrn_reflns_limit_k_min 0 _diffrn_reflns_limit_k_max 14 _diffrn_reflns_limit_l_min 0 _diffrn_reflns_limit_l_max 21 _diffrn_standards_number 3 _diffrn_standards_interval_count ? _diffrn_standards_interval_time '120 min' _diffrn_standards_decay_% '<3' _refine_ls_structure_factor_coef Fsqd _refine_ls_R_factor_obs 0.0483 _refine_ls_wR_factor_obs 0.1092 _refine_ls_wR_factor_all 0.1279 _refine_ls_goodness_of_fit_obs 1.113 _refine_ls_goodness_of_fit_all 1.024 _refine_ls_number_reflns 4551 _refine_ls_number_parameters 282 _refine_ls_hydrogen_treatment 'riding model' _refine_ls_weighting_scheme 'calc w=1/[\s^2^(Fo^2^)+(0.0581P)^2^+0.3272P] wh _refine_ls_shift/esd_max 0.024 _refine_diff_density_max 0.187 _refine_diff_density_min -0.144 _refine_ls_extinction_method 'SHELXL93 (Sheldrick, 1993)' _refine_ls_extinction_coef 0.0026(10) loop_ _atom_type_symbol _atom_type_description _atom_type_scat_source _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag 'C' 'C' 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 0.0033 0.001 'H' 'H' 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 0.0000 0.000 'N' 'N' 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 0.0061 0.003 'O' 'O' 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 0.0106 0.006 'Si' 'Si' 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 0.0817 0.0 _refine_ls_abs_structure_details 'Flack H D (1983), Acta Cryst. A39, 876-881 _refine_ls_abs_structure_Flack 0.08(19) loop_ _atom_site_label _atom_site_occupancy _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv Si 1 0.87003(10) 0.79301(9) 0.02493(5) 0.0595(3) N1 1 0.9005(3) 0.0838(3) 0.1916(2) 0.0665(8) N2 1 1.2294(3) 0.3515(3) 0.1588(2) 0.0736(9) O1 1 0.9614(2) 0.4334(2) -0.05923(12) 0.0543(6) O2 1 0.8018(2) 0.3231(3) -0.0420(2) 0.0938(10) O3 1 0.8048(2) 0.0522(2) 0.1712(2) 0.0835(9) O4 1 0.9515(3) 0.0436(3) 0.2462(2) 0.1035(11) O5 1 1.2752(2) 0.3051(3) 0.2130(2) 0.0932(10) O6 1 1.2702(3) 0.4325(3) 0.1250(2) 0.1171(14) C1 1 0.8682(3) 0.6432(3) -0.0165(2) 0.0620(9) H1A 1 0.7916 0.6115 -0.0074 0.091(2) H1B 1 0.9226 0.5969 0.0120 0.091(2) C2 1 0.8955(3) 0.6247(3) -0.1003(2) 0.0513(8) H2A 1 0.9686 0.6627 -0.1107 0.091(2) C3 1 0.8033(3) 0.6845(4) -0.1500(2) 0.0719(11) H3A 1 0.7295 0.6521 -0.1346 0.091(2) H3B 1 0.8026 0.7652 -0.1360 0.091(2) C4 1 0.8121(3) 0.6754(3) -0.2369(2) 0.0606(9) H4A 1 0.7808 0.7460 -0.2577 0.091(2) C5 1 0.9293(3) 0.6535(3) -0.2750(2) 0.0582(9) H5A 1 0.9920 0.7039 -0.2595 0.091(2) C6 1 0.9514(3) 0.5237(3) -0.2647(2) 0.0591(9) H6A 1 1.0086 0.5009 -0.3017 0.091(2) C7 1 0.9909(3) 0.4767(3) -0.1882(2) 0.0618(10) H7A 1 1.0073 0.3951 -0.1927 0.091(2) H7B 1 1.0629 0.5150 -0.1753 0.091(2) C8 1 0.9088(3) 0.4973(3) -0.1230(2) 0.0538(8) H8A 1 0.8337 0.4647 -0.1353 0.091(2) C9 1 0.8921(4) 0.6573(3) -0.3580(2) 0.0775(12) H9A 1 0.8613 0.7322 -0.3714 0.091(2) H9B 1 0.9546 0.6360 -0.3916 0.091(2) C10 1 0.7978(4) 0.5671(4) -0.3524(2) 0.0787(12) H10A 1 0.7498 0.5450 -0.3946 0.091(2) C11 1 0.7490(3) 0.5763(4) -0.2740(2) 0.0759(11) H11A 1 0.6680 0.5600 -0.2639 0.091(2) C12 1 0.8354(4) 0.4831(4) -0.2915(2) 0.0751(12) H12A 1 0.8126 0.4027 -0.2923 0.091(2) C13 1 0.8987(3) 0.3540(3) -0.0241(2) 0.0513(8) C21 1 0.9606(3) 0.3052(3) 0.0432(2) 0.0449(7) C22 1 0.9065(3) 0.2175(3) 0.0832(2) 0.0508(8) H22A 1 0.8326 0.1868 0.0667 0.091(2) C23 1 0.9605(3) 0.1755(3) 0.1476(2) 0.0479(8) C24 1 1.0663(3) 0.2160(3) 0.1732(2) 0.0529(8) H24A 1 1.1037 0.1848 0.2175 0.091(2) C25 1 1.1163(3) 0.3036(3) 0.1324(2) 0.0507(8) C26 1 1.0669(3) 0.3499(3) 0.0679(2) 0.0488(8) H26A 1 1.1046 0.4124 0.0413 0.091(2) C31 1 0.9106(5) 0.7725(4) 0.1255(2) 0.105(2) H31A 1 0.9855 0.7346 0.1282 0.091(2) H31B 1 0.8521 0.7240 0.1484 0.091(2) H31C 1 0.9143 0.8454 0.1519 0.091(2) C32 1 0.9790(4) 0.8891(4) -0.0201(3) 0.0883(13) H32A 1 1.0550 0.8535 -0.0176 0.091(2) H32B 1 0.9807 0.9623 0.0060 0.091(2) H32C 1 0.9579 0.9015 -0.0720 0.091(2) C33 1 0.7253(4) 0.8637(4) 0.0199(3) 0.0900(13) H33A 1 0.7062 0.8769 -0.0323 0.091(2) H33B 1 0.7285 0.9369 0.0460 0.091(2) H33C 1 0.6663 0.8154 0.0425 0.091(2) 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 0.0699(6) 0.0102(5) 0.0086(5) 0.0568(6) 0.0009(5) 0.0518(5) N1 0.067(2) -0.002(2) 0.004(2) 0.056(2) 0.007(2) 0.076(2) N2 0.046(2) -0.014(2) -0.014(2) 0.103(3) 0.020(2) 0.071(2) O1 0.0518(13) -0.0004(11) -0.0186(11) 0.0480(12) 0.0117(11) 0.0632(14) O2 0.065(2) -0.039(2) -0.0342(15) 0.128(2) 0.036(2) 0.089(2) O3 0.061(2) -0.0177(15) -0.006(2) 0.071(2) 0.016(2) 0.119(2) O4 0.104(2) -0.025(2) -0.017(2) 0.106(2) 0.052(2) 0.101(2) O5 0.063(2) -0.016(2) -0.0340(15) 0.133(3) 0.035(2) 0.084(2) O6 0.081(2) -0.062(2) -0.044(2) 0.141(3) 0.067(3) 0.129(3) C1 0.076(2) 0.013(2) 0.005(2) 0.056(2) 0.005(2) 0.054(2) C2 0.056(2) 0.012(2) -0.0044(15) 0.050(2) 0.0028(15) 0.049(2) C3 0.075(2) 0.032(2) 0.000(2) 0.075(3) 0.001(2) 0.065(2) C4 0.059(2) 0.014(2) -0.016(2) 0.059(2) 0.006(2) 0.064(2) C5 0.065(2) -0.007(2) -0.004(2) 0.050(2) 0.007(2) 0.059(2) C6 0.069(2) 0.007(2) -0.004(2) 0.058(2) -0.003(2) 0.050(2) C7 0.070(2) 0.021(2) -0.005(2) 0.053(2) -0.005(2) 0.063(2) C8 0.050(2) 0.003(2) -0.019(2) 0.055(2) 0.007(2) 0.056(2) C9 0.104(3) 0.005(3) -0.005(2) 0.068(2) 0.009(2) 0.060(2) C10 0.102(3) -0.008(3) -0.031(2) 0.075(3) 0.008(2) 0.059(2) C11 0.050(2) -0.017(2) -0.014(2) 0.099(3) 0.015(2) 0.079(3) C12 0.095(3) -0.017(2) -0.029(2) 0.057(2) 0.005(2) 0.073(2) C13 0.050(2) 0.003(2) -0.005(2) 0.053(2) -0.005(2) 0.051(2) C21 0.041(2) 0.0041(15) -0.0040(14) 0.043(2) -0.0046(14) 0.051(2) C22 0.050(2) 0.001(2) -0.0035(15) 0.043(2) -0.004(2) 0.060(2) C23 0.048(2) 0.0003(15) 0.0060(15) 0.042(2) 0.0028(15) 0.054(2) C24 0.050(2) 0.002(2) -0.0004(15) 0.060(2) 0.006(2) 0.049(2) C25 0.039(2) -0.003(2) -0.0043(15) 0.059(2) 0.004(2) 0.054(2) C26 0.049(2) 0.004(2) -0.0006(15) 0.050(2) 0.001(2) 0.047(2) C31 0.165(5) 0.018(3) -0.005(3) 0.093(3) -0.002(2) 0.058(2) C32 0.086(3) 0.001(2) 0.010(3) 0.074(3) 0.011(3) 0.105(3) C33 0.084(3) 0.017(2) 0.014(3) 0.077(3) -0.008(3) 0.109(3)