#------------------------------------------------------------------------------ #$Date: 2008-03-02 13:24:56 +0000 (Sun, 02 Mar 2008) $ #$Revision: 199 $ #$URL: svn://www.crystallography.net/cod/cif/2/2003522.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_2003522 _journal_name_full 'Acta Crystallographica' _journal_year 1995 _journal_volume C51 _journal_page_first 1148 _journal_page_last 1152 _publ_section_title ; Two Conformational Isomers of 2-Bromo-2,3-dihydro-2,3-(bibenzyl-2,2'-diyl)methano-1,4-naphthoquinone ; _chemical_formula_moiety 'C25 H17 Br O2' _chemical_formula_sum 'C25 H17 Br O2' _chemical_formula_weight 429.31 loop_ _symmetry_equiv_pos_as_xyz ' +x, +y, +z' ' -x, -y, -z' _symmetry_space_group_name_H-M 'P -1' _cell_length_a 9.165(1) _cell_length_b 13.155(1) _cell_length_c 8.850(1) _cell_angle_alpha 101.58(1) _cell_angle_beta 116.59(1) _cell_angle_gamma 80.77(1) _cell_volume 931.7(2) _cell_formula_units_Z 2.00 _exptl_crystal_density_diffrn 1.530 _exptl_crystal_density_meas 1.53 _exptl_crystal_density_method ? _diffrn_radiation_type 'Mo K\a' _diffrn_radiation_wavelength 0.7107 _cell_measurement_reflns_used 25 _cell_measurement_theta_min 10.015 _cell_measurement_theta_max 12.785 _exptl_absorpt_coefficient_mu 2.20 _cell_measurement_temperature 296 _exptl_crystal_description 'prismatic' _exptl_crystal_size_max 0.40 _exptl_crystal_size_mid 0.20 _exptl_crystal_size_min 0.20 _exptl_crystal_colour 'colorless' _diffrn_measurement_device 'Rigaku AFC5R diffractometer' _diffrn_measurement_method '\q/2\q scans' _exptl_absorpt_correction_type 'empirical, \y scan' _exptl_absorpt_correction_T_min 0.817 _exptl_absorpt_correction_T_max 1.000 _diffrn_reflns_number 4271 _reflns_number_total 3955 _reflns_number_observed 2401 _reflns_observed_criterion '|Fo|>3\s(|Fo|)' _diffrn_reflns_av_R_equivalents 0.021 _diffrn_reflns_theta_max 30.07 _diffrn_reflns_limit_h_min -10 _diffrn_reflns_limit_h_max 0 _diffrn_reflns_limit_k_min -18 _diffrn_reflns_limit_k_max 16 _diffrn_reflns_limit_l_min -11 _diffrn_reflns_limit_l_max 12 _diffrn_standards_number 3 _diffrn_standards_interval_count 100 _diffrn_standards_decay_% -1.66 _refine_ls_structure_factor_coef F _refine_ls_R_factor_obs 0.037 _refine_ls_wR_factor_obs 0.040 _refine_ls_wR_factor_all ? _refine_ls_goodness_of_fit_obs 1.48 _refine_ls_goodness_of_fit_all ? _refine_ls_number_reflns 2401 _refine_ls_number_parameters 313 _refine_ls_hydrogen_treatment 'refall except H8, H9, which were not refined' _refine_ls_weighting_scheme sigma _refine_ls_shift/esd_max 0.46 _refine_diff_density_max 0.355 _refine_diff_density_min -0.433 _refine_ls_extinction_method 'none' _refine_ls_extinction_coef ? loop_ _atom_type_symbol _atom_type_scat_source _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag C IntTabIV_Table_2.2A 0.003 0.002 H IntTabIV_Table_2.2A 0.000 0.000 O IntTabIV_Table_2.2A 0.011 0.006 Br IntTabIV_Table_2.2A -0.290 2.459 _refine_ls_abs_structure_details ? _refine_ls_abs_structure_Flack ? ##;MSC/AFC Diffractometer Control Software ##(Molecular Structure Corporation, 1988) ##; ##;PROCESS TEXSAN (Molecular Structure Corporation, 1992) ##; loop_ _atom_site_label _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv Br(1) -0.19896(5) 0.63672(4) 0.02386(6) 0.0549(1) O(1) -0.1413(3) 0.8371(2) -0.0528(4) 0.0617(9) O(2) 0.4021(3) 0.5830(2) 0.1761(4) 0.067(1) C(1) -0.0123(4) 0.7893(3) 0.0228(4) 0.041(1) C(2) -0.0021(4) 0.7075(3) 0.1237(4) 0.037(1) C(3) 0.1537(4) 0.6386(3) 0.1915(4) 0.037(1) C(4) 0.2920(4) 0.6516(3) 0.1558(5) 0.046(1) C(5) 0.2853(4) 0.7459(3) 0.0850(4) 0.040(1) C(6) 0.1409(4) 0.8095(3) 0.0189(4) 0.041(1) C(7) 0.1371(7) 0.8915(4) -0.0606(6) 0.058(2) C(8) 0.2742(8) 0.9110(4) -0.0713(7) 0.074(2) C(9) 0.4169(7) 0.8484(4) -0.0050(6) 0.069(2) C(10) 0.4219(5) 0.7669(4) 0.0723(6) 0.054(1) C(11) 0.1046(4) 0.7190(3) 0.3160(4) 0.036(1) C(12) 0.0632(4) 0.6779(3) 0.4369(5) 0.039(1) C(13) 0.1893(5) 0.6246(3) 0.5604(5) 0.051(1) C(14) 0.3554(6) 0.6035(5) 0.5620(7) 0.071(2) C(15) 0.4459(6) 0.6958(5) 0.5875(6) 0.083(2) C(16) 0.3589(5) 0.7991(3) 0.5335(5) 0.050(1) C(17) 0.1990(4) 0.8131(3) 0.4064(4) 0.038(1) C(18) 0.1279(6) 0.9116(3) 0.3794(5) 0.053(1) C(19) 0.2114(8) 0.9981(4) 0.4674(7) 0.074(2) C(20) 0.3702(8) 0.9853(5) 0.5850(7) 0.081(2) C(21) 0.4420(6) 0.8890(5) 0.6188(6) 0.069(2) C(22) 0.1572(9) 0.5898(4) 0.6798(6) 0.074(2) C(23) 0.0078(11) 0.6108(5) 0.6808(8) 0.092(3) C(24) -0.1127(9) 0.6667(5) 0.5665(9) 0.083(2) C(25) -0.0858(5) 0.7014(4) 0.4429(6) 0.057(1) H(1) 0.149(4) 0.561(3) 0.197(4) 0.037(9) H(2) 0.048(5) 0.928(3) -0.099(5) 0.06(1) H(3) 0.275(6) 0.965(4) -0.121(7) 0.10(1) H(4) 0.508(6) 0.871(4) -0.012(6) 0.09(1) H(5) 0.509(5) 0.727(3) 0.117(5) 0.05(1) H(6) 0.345(5) 0.554(3) 0.454(6) 0.08(1) H(7) 0.411(6) 0.561(4) 0.642(6) 0.09(1) H(8) 0.5130 0.6742 0.5292 0.099 H(9) 0.5127 0.7099 0.7070 0.099 H(10) 0.016(5) 0.919(3) 0.304(5) 0.06(1) H(11) 0.161(5) 1.064(4) 0.447(6) 0.08(1) H(12) 0.423(6) 1.041(4) 0.632(6) 0.08(1) H(13) 0.558(5) 0.874(3) 0.702(5) 0.07(1) H(14) 0.252(7) 0.557(4) 0.772(7) 0.11(1) H(15) -0.011(7) 0.579(4) 0.760(7) 0.12(1) H(16) -0.212(6) 0.678(4) 0.553(6) 0.09(1) H(17) -0.161(3) 0.741(2) 0.367(4) 0.015(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 Br(1) 0.0386(2) -0.0115(2) 0.143(2) 0.0615(3) -0.0028(2) 0.0565(3) O(1) 0.044(2) 0.016(1) 0.010(1) 0.063(2) 0.028(2) 0.065(2) O(2) 0.051(2) 0.031(2) 0.038(2) 0.070(2) 0.036(2) 0.089(2) C(1) 0.040(2) 0.006(2) 0.010(2) 0.039(2) 0.004(2) 0.034(2) C(2) 0.028(2) 0.000(2) 0.010(2) 0.039(2) 0.004(2) 0.037(2) C(3) 0.038(2) 0.006(2) 0.014(2) 0.031(2) 0.010(2) 0.040(2) C(4) 0.039(2) 0.007(2) 0.018(2) 0.049(2) 0.011(2) 0.047(2) C(5) 0.042(2) -0.002(2) 0.016(2) 0.044(2) 0.000(2) 0.033(2) C(6) 0.047(2) 0.002(2) 0.016(2) 0.036(2) 0.005(2) 0.035(2) C(7) 0.072(3) 0.009(2) 0.035(3) 0.051(3) 0.019(2) 0.060(3) C(8) 0.103(4) -0.010(3) 0.053(3) 0.062(3) 0.017(3) 0.079(4) C(9) 0.081(4) -0.029(3) 0.043(3) 0.075(4) -0.001(3) 0.068(3) C(10) 0.047(3) -0.005(2) 0.025(2) 0.067(3) 0.007(2) 0.052(3) C(11) 0.033(2) 0.004(2) 0.013(2) 0.035(2) 0.006(2) 0.037(2) C(12) 0.049(2) -0.007(2) 0.025(2) 0.031(2) -0.003(2) 0.042(2) C(13) 0.071(3) -0.001(2) 0.026(2) 0.043(2) 0.008(2) 0.042(2) C(14) 0.069(3) 0.030(3) 0.023(3) 0.078(4) 0.034(3) 0.061(3) C(15) 0.048(3) 0.012(3) 0.012(2) 0.112(5) 0.029(3) 0.075(3) C(16) 0.041(2) -0.010(2) 0.019(2) 0.070(3) 0.010(2) 0.045(2) C(17) 0.044(2) -0.007(2) 0.019(2) 0.040(2) 0.005(2) 0.034(2) C(18) 0.064(3) -0.009(2) 0.018(2) 0.045(3) 0.004(2) 0.044(2) C(19) 0.123(5) -0.024(3) 0.041(3) 0.043(3) -0.004(2) 0.060(3) C(20) 0.120(5) -0.068(4) 0.043(3) 0.082(4) -0.017(3) 0.056(3) C(21) 0.056(3) -0.038(3) 0.018(2) 0.104(5) 0.002(3) 0.050(3) C(22) 0.121(5) -0.018(3) 0.037(3) 0.056(3) 0.003(2) 0.050(3) C(23) 0.157(7) -0.063(5) 0.069(5) 0.081(4) -0.020(3) 0.067(4) C(24) 0.090(4) -0.052(4) 0.067(4) 0.095(4) -0.038(4) 0.091(4) C(25) 0.054(3) -0.013(2) 0.029(2) 0.056(3) -0.011(2) 0.061(3)