#------------------------------------------------------------------------------ #$Date: 2011-09-17 22:27:16 +0200 (Sat, 17 Sep 2011) $ #$Revision: 26029 $ #$URL: svn://www.crystallography.net/cod/cif/2/2003375.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_2003375 _journal_name_full 'Acta Crystallographica C' _journal_volume 51 _journal_year 1995 _journal_page_first 741 _journal_page_last 743 _publ_section_title ; p-Nitrobenzyl Trichloroacetimidate ; _chemical_formula_sum 'C9 H7 Cl3 N2 O3' _chemical_formula_weight 297.52 loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x+1/2, -y, z+1/2' 'x+1/2, -y+1/2, -z' '-x, y+1/2, -z+1/2' _symmetry_space_group_name_H-M 'P 21 21 21' _cell_length_a 7.0278(3) _cell_length_b 10.8550(5) _cell_length_c 15.6339(7) _cell_angle_alpha 90.00 _cell_angle_beta 90.00 _cell_angle_gamma 90.00 _cell_volume 1192.66(9) _cell_formula_units_Z 4 _exptl_crystal_density_diffrn 1.657 _exptl_crystal_density_meas ? _exptl_crystal_density_method ? _diffrn_radiation_type MoK\a _diffrn_radiation_wavelength 0.71073 _cell_measurement_reflns_used 32 _cell_measurement_theta_min 11.57 _cell_measurement_theta_max 12.17 _exptl_absorpt_coefficient_mu 0.764 _cell_measurement_temperature 295(2) _exptl_crystal_description block _exptl_crystal_size_max 0.52 _exptl_crystal_size_mid 0.40 _exptl_crystal_size_min 0.32 _exptl_crystal_colour colourless _chemical_compound_source ? _diffrn_measurement_device 'Stoe Siemens diffractometer' _diffrn_measurement_method '\w/\q scans with on-line profile fitting (Clegg,' _exptl_absorpt_correction_type none _exptl_absorpt_correction_T_min ? _exptl_absorpt_correction_T_max ? _diffrn_reflns_number 3906 _reflns_number_total 2098 _reflns_number_observed 1992 _reflns_observed_criterion >2sigma(I) _diffrn_reflns_av_R_equivalents 0.0239 _diffrn_reflns_theta_max 24.98 _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 -18 _diffrn_reflns_limit_l_max 18 _diffrn_standards_number 3 _diffrn_standards_interval_count ? _diffrn_standards_interval_time 60 _diffrn_standards_decay_% 0 _refine_ls_structure_factor_coef Fsqd _refine_ls_R_factor_obs 0.0228 _refine_ls_wR_factor_obs 0.0597 _refine_ls_wR_factor_all 0.0623 _refine_ls_goodness_of_fit_obs 1.031 _refine_ls_goodness_of_fit_all 1.041 _refine_ls_number_reflns 2097 _refine_ls_number_parameters 183 _refine_ls_hydrogen_treatment ? _refine_ls_weighting_scheme ; calc w = 1/[\s^2^(F~o~^2^) + (0.0320P)^2^ + 0.2219P] where P = (F~o~^2^ + 2F~c~^2^)/3 ; _refine_ls_shift/esd_max 0.001 _refine_diff_density_max .170 _refine_diff_density_min -.191 _refine_ls_extinction_method 'SHELXL93 (Sheldrick, 1994)' _refine_ls_extinction_coef 0.0170(16) 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' .0033 .0016 'H' 'H' 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' .0000 .0000 'N' 'N' 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' .0061 .0033 'O' 'O' 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' .0106 .0060 'Cl' 'Cl' 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' .1484 .158 _refine_ls_abs_structure_details 'Flack (1983)' _refine_ls_abs_structure_Flack -0.03(6) 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 Cl1 1 0.99911(9) 0.31196(5) 0.57317(4) 0.0624(2) Cl2 1 1.22786(7) 0.48565(5) 0.47767(4) 0.0581(2) Cl3 1 0.96329(10) 0.32843(6) 0.39029(4) 0.0684(2) N1 1 0.7031(3) 0.5310(2) 0.45281(13) 0.0556(5) H1 1 0.6964(35) 0.4821(23) 0.4069(16) 0.062(7) N2 1 0.0801(3) 0.5283(2) 0.76184(11) 0.0533(4) O1 1 0.8898(2) 0.57606(13) 0.56784(9) 0.0480(3) O2 1 0.0589(3) 0.4194(2) 0.77976(12) 0.0759(5) O3 1 -0.0354(3) 0.6082(2) 0.77958(12) 0.0718(5) C1 1 1.0016(3) 0.4134(2) 0.48483(12) 0.0438(4) C2 1 0.8467(3) 0.5116(2) 0.49717(11) 0.0410(4) C3 1 0.7617(3) 0.6749(2) 0.5893(2) 0.0516(5) H3A 1 0.7269(32) 0.7149(22) 0.5428(15) 0.053(6) H3B 1 0.8422(37) 0.7282(24) 0.6277(16) 0.061(7) C4 1 0.5844(3) 0.6314(2) 0.63425(12) 0.0416(4) C5 1 0.4401(3) 0.7166(2) 0.64829(14) 0.0476(5) H5 1 0.4578(36) 0.7851(26) 0.6268(17) 0.060(7) C6 1 0.2749(3) 0.6847(2) 0.69002(13) 0.0478(5) H6 1 0.1889(38) 0.7404(23) 0.6991(16) 0.060(7) C7 1 0.2555(3) 0.5647(2) 0.71759(11) 0.0429(4) C8 1 0.3950(3) 0.4779(2) 0.70470(13) 0.0497(5) H8 1 0.3715(37) 0.3999(24) 0.7255(15) 0.057(6) C9 1 0.5609(3) 0.5125(2) 0.66406(14) 0.0503(5) H9 1 0.6596(40) 0.4598(26) 0.6544(16) 0.067(8) 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 Cl1 0.0681(4) 0.0067(3) 0.0075(3) 0.0506(3) 0.0159(2) 0.0687(3) Cl2 0.0382(2) -0.0069(2) 0.0091(2) 0.0570(3) -0.0054(3) 0.0791(4) Cl3 0.0680(4) -0.0091(3) 0.0080(3) 0.0737(4) -0.0265(3) 0.0633(3) N1 0.0475(10) -0.0012(9) -0.0103(8) 0.0642(11) 0.0023(9) 0.0549(10) N2 0.0528(10) -0.0084(10) 0.0020(8) 0.0650(11) -0.0049(8) 0.0420(8) O1 0.0393(7) 0.0048(6) -0.0034(7) 0.0498(7) -0.0112(7) 0.0551(8) O2 0.0847(13) -0.0168(10) 0.0226(10) 0.0661(11) 0.0019(9) 0.0768(11) O3 0.0569(10) 0.0080(10) 0.0190(9) 0.0859(12) -0.0038(9) 0.0725(10) C1 0.0404(9) -0.0034(8) 0.0040(9) 0.0430(9) -0.0017(8) 0.0481(10) C2 0.0384(9) -0.0052(8) 0.0039(8) 0.0407(9) 0.0049(8) 0.0438(9) C3 0.0455(11) 0.0012(9) 0.0037(10) 0.0412(10) -0.0070(10) 0.0681(14) C4 0.0399(10) 0.0010(8) -0.0058(8) 0.0411(9) -0.0022(8) 0.0438(9) C5 0.0495(11) 0.0024(9) -0.0029(10) 0.0365(10) 0.0035(9) 0.0567(11) C6 0.0436(11) 0.0107(10) -0.0025(9) 0.0462(10) -0.0038(9) 0.0535(11) C7 0.0451(10) -0.0024(9) -0.0013(9) 0.0468(10) -0.0054(8) 0.0368(8) C8 0.0621(13) 0.0025(10) 0.0040(9) 0.0375(10) 0.0020(9) 0.0494(10) C9 0.0507(11) 0.0094(9) 0.0033(10) 0.0393(10) -0.0021(9) 0.0610(11) _cod_database_code 2003375