# Supplementary Material (ESI) for Perkin Transactions # This journal is © The Royal Society of Chemistry 2002 data_General #---------------------------------------------------------------------- _journal_coden_Cambridge 188 _journal_volume ? _journal_year ? _journal_page_first ? #----------------------------------------------------------------------- #SUBMISSION DETAILS _publ_contact_author_name 'Prof Takanori Suzuki' _publ_contact_author_address ; Prof Takanori Suzuki Division of Chemistry Hokkaido University Graduate School of Science, N10 W8 Sapporo 060-0810 JAPAN ; _publ_contact_author_email ' TAK@SCI.HOKUDAI.AC.JP ' _publ_contact_letter ; ENTER TEXT OF LETTER ; _publ_requested_journal ' Perkins Trans 2' #----------------------------------------------------------------------- #TITLE AND AUTHOR LIST _publ_section_title ; ENTER SECTION TITLE ; _publ_section_title_footnote ; ENTER FOOTNOTE TO TITLE OF PAPER ; loop_ _publ_author_name 'Suzuki, Takanori' 'Higuchi, Hiroki' 'Hirota, Erika' 'Ohkita, Masakazu' 'Tsuji, Takashi' 'Yamamoto, Rie' _publ_section_synopsis ; ENTER SYNOPSIS ; #---------------------------------------------------------------------- #TEXT _publ_section_abstract ; ENTER ABSTRACT ; _publ_section_comment ; ENTER TEXT ; _publ_section_acknowledgements ; ENTER ACKNOWLEDGEMENTS ; _publ_section_references ; ENTER OTHER REFERENCES Molecular Structure Corporation, Rigaku Corporation. (2000). teXsan. Single Crystal Structure Analysis Software. Version 1.11. MSC, 3200 Research Forest Drive, The Woodlands, TX 77381, USA. Rigaku, 3-9-12 Akishima, Tokyo, Japan. ; _publ_section_figure_captions ; ENTER FIGURE CAPTIONS ; _publ_section_exptl_prep ; ENTER COMPOUND PREPARATION DETAILS ; _publ_section_exptl_refinement ; ENTER SPECIAL DETAILS OF THE REFINEMENT ; #------------------------------------------------------------------------ #***Data of 1a*** data_011025 _database_code_CSD 185682 _audit_creation_date 'Tue Feb 12 15:48:50 2002' _audit_creation_method 'by teXsan' _audit_update_record ? #------------------------------------------------------------------------ # CHEMICAL DATA _chemical_formula_sum 'C38 H22 Br2 O2 ' _chemical_formula_moiety 'C38 H22 Br2 O2 ' _chemical_formula_weight 670.40 _chemical_melting_point ? #------------------------------------------------------------------------ # CRYSTAL DATA _symmetry_cell_setting monoclinic _symmetry_space_group_name_H-M 'P 1 21/c 1' _symmetry_Int_Tables_number 14 loop_ _symmetry_equiv_pos_as_xyz x,y,z -x,1/2+y,1/2-z -x,-y,-z x,1/2-y,1/2+z _cell_length_a 12.462(6) _cell_length_b 15.613(7) _cell_length_c 15.042(7) _cell_angle_alpha 90 _cell_angle_beta 111.351(8) _cell_angle_gamma 90 _cell_volume 2725(2) _cell_formula_units_Z 4 _cell_measurement_reflns_used 7265 _cell_measurement_theta_min 3.1 _cell_measurement_theta_max 27.5 _cell_measurement_temperature 153.1 #-------------------------------------------------------------------- _exptl_crystal_description 'Needle' _exptl_crystal_colour 'Colorless' _exptl_crystal_size_max 0.400 _exptl_crystal_size_mid 0.150 _exptl_crystal_size_min 0.150 _exptl_crystal_size_rad ? _exptl_crystal_density_diffrn 1.633 _exptl_crystal_density_meas ? _exptl_crystal_density_method 'not measured' _exptl_absorpt_coefficient_mu 3.019 _exptl_absorpt_correction_type none _exptl_absorpt_process_details ? _exptl_absorpt_correction_T_min 0.636 _exptl_absorpt_correction_T_max 0.636 #-------------------------------------------------------------------- #EXPERIMENTAL DATA _diffrn_radiation_type 'Mo K\a' _diffrn_radiation_wavelength 0.7107 _diffrn_measurement_device_type 'Rigaku/MSC Mercury CCD' _diffrn_measurement_method \w _diffrn_detector_area_resol_mean 14.62 _diffrn_reflns_number 352 _diffrn_reflns_av_R_equivalents 0.044 _diffrn_reflns_theta_max 27.49 _diffrn_measured_fraction_theta_max 0.9877 _diffrn_reflns_theta_full 27.49 _diffrn_measured_fraction_theta_full 0.9877 _diffrn_reflns_limit_h_min -16 _diffrn_reflns_limit_h_max 12 _diffrn_reflns_limit_k_min -20 _diffrn_reflns_limit_k_max 19 _diffrn_reflns_limit_l_min -19 _diffrn_reflns_limit_l_max 19 #------------------------------------------------------------------- #REFINEMENT DATA _refine_special_details ; Refinement using reflections with F^2^ > 3.0 sigma(F^2^). The weighted R-factor (wR), goodness of fit (S) and R-factor (gt) are based on F, with F set to zero for negative F. The threshold expression of F^2^ > 3.0 sigma(F^2^) is used only for calculating R-factor (gt). ; _reflns_number_total 6174 _reflns_number_gt 3567 _reflns_threshold_expression F^2^>3.0\s(F^2^) _refine_ls_structure_factor_coef F _refine_ls_R_factor_gt 0.0361 _refine_ls_wR_factor_ref 0.0426 _refine_ls_hydrogen_treatment noref _refine_ls_number_reflns 3567 _refine_ls_number_parameters 379 _refine_ls_goodness_of_fit_ref 0.950 _refine_ls_weighting_scheme calc _refine_ls_weighting_details 'w = 1/[\s^2^(Fo) + 0.00063|Fo|^2^]' _refine_ls_shift/su_max 0.0009 _refine_diff_density_max 0.46 _refine_diff_density_min -0.45 _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_abs_structure_details ? _refine_ls_abs_structure_Flack ? loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source 'C' 'C' 0.003 0.002 ;International Tables for Crystallography (1992, Vol. C, Tables 4.2.6.8 and 6.1.1.1) ; 'H' 'H' 0.000 0.000 ;International Tables for Crystallography (1992, Vol. C, Table 6.1.1.2) ; 'Br' 'Br' -0.290 2.459 ;International Tables for Crystallography (1992, Vol. C, Tables 4.2.6.8 and 6.1.1.1) ; 'O' 'O' 0.011 0.006 ;International Tables for Crystallography (1992, Vol. C, Tables 4.2.6.8 and 6.1.1.1) ; #----------------------------------------------------------------------- #ATOMIC COORDINATES AND DISPLACEMENT PARAMETERS loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_occupancy _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group Br(1) Br 0.62954(4) 0.30791(3) 0.48846(3) 0.0276(1) Uani 1.00 d . . . Br(2) Br 0.46070(4) 0.46513(3) 0.34703(3) 0.0279(1) Uani 1.00 d . . . O(1) O 0.0221(2) 0.1164(2) 0.1048(2) 0.0211(8) Uani 1.00 d . . . O(2) O 0.1139(2) 0.0190(2) 0.3587(2) 0.0227(8) Uani 1.00 d . . . C(1) C 0.4184(3) 0.2594(3) 0.3354(3) 0.013(1) Uani 1.00 d . . . C(2) C 0.3636(3) 0.2010(3) 0.2631(3) 0.015(1) Uani 1.00 d . . . C(3) C 0.4219(4) 0.1680(3) 0.2072(3) 0.018(1) Uani 1.00 d . . . C(4) C 0.5377(4) 0.1838(3) 0.2310(3) 0.021(1) Uani 1.00 d . . . C(5) C 0.5986(3) 0.2275(3) 0.3144(3) 0.021(1) Uani 1.00 d . . . C(6) C 0.5395(3) 0.2640(3) 0.3659(3) 0.018(1) Uani 1.00 d . . . C(7) C 0.3467(3) 0.3116(3) 0.3748(3) 0.015(1) Uani 1.00 d . . . C(8) C 0.2497(3) 0.2746(3) 0.3848(3) 0.014(1) Uani 1.00 d . . . C(9) C 0.1918(3) 0.3189(3) 0.4347(3) 0.017(1) Uani 1.00 d . . . C(10) C 0.2233(4) 0.4017(3) 0.4653(3) 0.022(1) Uani 1.00 d . . . C(11) C 0.3063(4) 0.4439(3) 0.4420(3) 0.022(1) Uani 1.00 d . . . C(12) C 0.3660(3) 0.3994(3) 0.3957(3) 0.016(1) Uani 1.00 d . . . C(13) C 0.2386(3) 0.1765(3) 0.2443(3) 0.014(1) Uani 1.00 d . . . C(14) C 0.2168(3) 0.0835(3) 0.2122(3) 0.014(1) Uani 1.00 d . . . C(15) C 0.2976(4) 0.0181(3) 0.2491(3) 0.019(1) Uani 1.00 d . . . C(16) C 0.2724(4) -0.0669(3) 0.2239(3) 0.025(1) Uani 1.00 d . . . C(17) C 0.1644(4) -0.0888(3) 0.1613(3) 0.027(1) Uani 1.00 d . . . C(18) C 0.0821(4) -0.0266(3) 0.1227(3) 0.024(1) Uani 1.00 d . . . C(19) C 0.1091(4) 0.0591(3) 0.1481(3) 0.017(1) Uani 1.00 d . . . C(20) C 0.0533(3) 0.2013(3) 0.1035(3) 0.018(1) Uani 1.00 d . . . C(21) C -0.0265(4) 0.2528(3) 0.0365(3) 0.025(1) Uani 1.00 d . . . C(22) C -0.0003(4) 0.3371(3) 0.0261(3) 0.028(1) Uani 1.00 d . . . C(23) C 0.1059(4) 0.3700(3) 0.0825(3) 0.025(1) Uani 1.00 d . . . C(24) C 0.1845(4) 0.3183(3) 0.1511(3) 0.019(1) Uani 1.00 d . . . C(25) C 0.1579(3) 0.2331(3) 0.1651(3) 0.015(1) Uani 1.00 d . . . C(26) C 0.2109(3) 0.1856(3) 0.3435(3) 0.013(1) Uani 1.00 d . . . C(27) C 0.2746(3) 0.1179(3) 0.4192(3) 0.016(1) Uani 1.00 d . . . C(28) C 0.3806(4) 0.1329(3) 0.4917(3) 0.023(1) Uani 1.00 d . . . C(29) C 0.4333(4) 0.0716(3) 0.5591(3) 0.033(1) Uani 1.00 d . . . C(30) C 0.3818(4) -0.0084(3) 0.5554(3) 0.032(1) Uani 1.00 d . . . C(31) C 0.2769(4) -0.0241(3) 0.4870(3) 0.027(1) Uani 1.00 d . . . C(32) C 0.2232(4) 0.0389(3) 0.4209(3) 0.020(1) Uani 1.00 d . . . C(33) C 0.0425(4) 0.0863(3) 0.3192(3) 0.018(1) Uani 1.00 d . . . C(34) C -0.0738(4) 0.0661(3) 0.2822(3) 0.025(1) Uani 1.00 d . . . C(35) C -0.1538(4) 0.1289(4) 0.2411(3) 0.030(1) Uani 1.00 d . . . C(36) C -0.1181(4) 0.2127(3) 0.2391(3) 0.024(1) Uani 1.00 d . . . C(37) C -0.0025(4) 0.2328(3) 0.2752(3) 0.019(1) Uani 1.00 d . . . C(38) C 0.0818(3) 0.1701(3) 0.3158(3) 0.015(1) Uani 1.00 d . . . H(1) H 0.3805 0.1341 0.1520 0.0218 Uiso 1.00 calc . . . H(2) H 0.5757 0.1646 0.1893 0.0264 Uiso 1.00 calc . . . H(3) H 0.6813 0.2314 0.3363 0.0248 Uiso 1.00 calc . . . H(4) H 0.1296 0.2913 0.4476 0.0209 Uiso 1.00 calc . . . H(5) H 0.1863 0.4302 0.5037 0.0267 Uiso 1.00 calc . . . H(6) H 0.3219 0.5036 0.4577 0.0268 Uiso 1.00 calc . . . H(7) H 0.3731 0.0325 0.2943 0.0228 Uiso 1.00 calc . . . H(8) H 0.3307 -0.1102 0.2502 0.0328 Uiso 1.00 calc . . . H(9) H 0.1460 -0.1483 0.1447 0.0311 Uiso 1.00 calc . . . H(10) H 0.0064 -0.0418 0.0789 0.0300 Uiso 1.00 calc . . . H(11) H -0.1004 0.2296 -0.0026 0.0316 Uiso 1.00 calc . . . H(12) H -0.0558 0.3733 -0.0198 0.0347 Uiso 1.00 calc . . . H(13) H 0.1271 0.4281 0.0747 0.0310 Uiso 1.00 calc . . . H(14) H 0.2581 0.3410 0.1890 0.0235 Uiso 1.00 calc . . . H(15) H 0.4185 0.1875 0.4938 0.0284 Uiso 1.00 calc . . . H(16) H 0.5064 0.0845 0.6096 0.0398 Uiso 1.00 calc . . . H(17) H 0.4215 -0.0524 0.6007 0.0395 Uiso 1.00 calc . . . H(18) H 0.2401 -0.0789 0.4846 0.0325 Uiso 1.00 calc . . . H(19) H -0.0986 0.0084 0.2857 0.0301 Uiso 1.00 calc . . . H(20) H -0.2340 0.1147 0.2128 0.0374 Uiso 1.00 calc . . . H(21) H -0.1741 0.2574 0.2122 0.0294 Uiso 1.00 calc . . . H(22) H 0.0213 0.2911 0.2733 0.0230 Uiso 1.00 calc . . . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_12 _atom_site_aniso_U_13 _atom_site_aniso_U_23 Br(1) 0.0189(2) 0.0313(3) 0.0265(2) -0.0039(2) 0.0008(2) -0.0073(2) Br(2) 0.0327(3) 0.0187(2) 0.0348(3) -0.0074(2) 0.0153(2) -0.0008(2) O(1) 0.013(1) 0.029(2) 0.020(2) -0.006(1) 0.003(1) -0.001(1) O(2) 0.021(2) 0.020(2) 0.025(2) -0.006(1) 0.006(1) 0.002(1) C(1) 0.013(2) 0.013(2) 0.014(2) -0.002(2) 0.006(2) 0.002(2) C(2) 0.013(2) 0.014(2) 0.018(2) 0.000(2) 0.005(2) 0.002(2) C(3) 0.017(2) 0.014(2) 0.023(2) -0.002(2) 0.009(2) -0.005(2) C(4) 0.020(2) 0.020(2) 0.030(2) 0.000(2) 0.016(2) 0.000(2) C(5) 0.012(2) 0.018(2) 0.031(3) 0.004(2) 0.007(2) 0.002(2) C(6) 0.014(2) 0.016(2) 0.021(2) -0.003(2) 0.005(2) -0.001(2) C(7) 0.015(2) 0.017(2) 0.009(2) 0.002(2) 0.002(2) 0.001(2) C(8) 0.012(2) 0.016(2) 0.010(2) 0.002(2) -0.001(2) 0.001(2) C(9) 0.016(2) 0.025(2) 0.010(2) 0.003(2) 0.003(2) -0.001(2) C(10) 0.018(2) 0.030(3) 0.018(2) 0.008(2) 0.008(2) -0.008(2) C(11) 0.023(2) 0.020(3) 0.016(2) 0.002(2) -0.001(2) -0.005(2) C(12) 0.018(2) 0.014(2) 0.017(2) 0.000(2) 0.007(2) -0.001(2) C(13) 0.010(2) 0.022(2) 0.010(2) -0.002(2) 0.003(2) -0.004(2) C(14) 0.015(2) 0.017(2) 0.013(2) -0.003(2) 0.008(2) -0.002(2) C(15) 0.017(2) 0.022(3) 0.018(2) -0.004(2) 0.008(2) -0.004(2) C(16) 0.027(3) 0.022(3) 0.026(2) 0.000(2) 0.008(2) -0.002(2) C(17) 0.043(3) 0.017(2) 0.020(2) -0.010(2) 0.011(2) -0.005(2) C(18) 0.026(2) 0.025(3) 0.017(2) -0.012(2) 0.004(2) -0.003(2) C(19) 0.019(2) 0.018(2) 0.015(2) -0.002(2) 0.008(2) 0.001(2) C(20) 0.018(2) 0.025(3) 0.011(2) 0.000(2) 0.005(2) 0.003(2) C(21) 0.018(2) 0.044(3) 0.016(2) 0.005(2) 0.008(2) -0.001(2) C(22) 0.033(3) 0.036(3) 0.016(2) 0.020(2) 0.009(2) 0.008(2) C(23) 0.037(3) 0.021(3) 0.020(2) 0.005(2) 0.015(2) 0.003(2) C(24) 0.023(2) 0.022(2) 0.015(2) 0.002(2) 0.011(2) -0.001(2) C(25) 0.016(2) 0.018(2) 0.012(2) 0.003(2) 0.006(2) -0.001(2) C(26) 0.012(2) 0.017(2) 0.011(2) -0.001(2) 0.006(2) -0.002(2) C(27) 0.014(2) 0.021(2) 0.015(2) 0.001(2) 0.009(2) 0.002(2) C(28) 0.020(2) 0.026(3) 0.021(2) 0.001(2) 0.004(2) 0.002(2) C(29) 0.026(3) 0.038(3) 0.027(3) 0.000(2) -0.001(2) 0.009(2) C(30) 0.026(3) 0.035(3) 0.030(3) 0.003(2) 0.005(2) 0.015(2) C(31) 0.027(3) 0.024(3) 0.029(3) -0.002(2) 0.010(2) 0.006(2) C(32) 0.016(2) 0.026(3) 0.018(2) -0.001(2) 0.006(2) -0.004(2) C(33) 0.018(2) 0.024(3) 0.015(2) -0.003(2) 0.010(2) -0.002(2) C(34) 0.023(2) 0.034(3) 0.020(2) -0.008(2) 0.011(2) -0.003(2) C(35) 0.013(2) 0.051(3) 0.026(3) -0.009(2) 0.007(2) -0.011(2) C(36) 0.015(2) 0.037(3) 0.021(2) 0.007(2) 0.007(2) -0.006(2) C(37) 0.018(2) 0.022(2) 0.017(2) 0.001(2) 0.008(2) -0.003(2) C(38) 0.013(2) 0.025(2) 0.010(2) -0.002(2) 0.006(2) -0.003(2) #--------------------------------------------------------------------- _computing_data_collection 'CRYSTALCLEAR' _computing_cell_refinement 'CRYSTALCLEAR' _computing_data_reduction 'teXsan Ver. 1.11' _computing_structure_solution SIR92 _computing_structure_refinement 'teXsan Ver. 1.10' _computing_publication_material 'teXsan Ver. 1.11' _computing_molecular_graphics ? #--------------------------------------------------------------------- _geom_special_details ; ? ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_1 _geom_bond_site_symmetry_2 _geom_bond_publ_flag Br(1) C(6) 1.903(4) . . yes Br(2) C(12) 1.901(4) . . yes O(1) C(19) 1.374(5) . . yes O(1) C(20) 1.384(5) . . yes O(2) C(32) 1.378(5) . . yes O(2) C(33) 1.364(5) . . yes C(1) C(2) 1.393(6) . . yes C(1) C(6) 1.410(6) . . yes C(1) C(7) 1.483(5) . . yes C(2) C(3) 1.394(5) . . yes C(2) C(13) 1.528(5) . . yes C(3) C(4) 1.377(6) . . yes C(4) C(5) 1.385(6) . . yes C(5) C(6) 1.374(6) . . yes C(7) C(8) 1.396(6) . . yes C(7) C(12) 1.408(6) . . yes C(8) C(9) 1.399(5) . . yes C(8) C(26) 1.527(6) . . yes C(9) C(10) 1.380(6) . . yes C(10) C(11) 1.375(6) . . yes C(11) C(12) 1.379(6) . . yes C(13) C(14) 1.522(6) . . yes C(13) C(25) 1.530(6) . . yes C(13) C(26) 1.656(5) . . yes C(14) C(15) 1.399(6) . . yes C(14) C(19) 1.391(5) . . yes C(15) C(16) 1.385(6) . . yes C(16) C(17) 1.376(6) . . yes C(17) C(18) 1.377(7) . . yes C(18) C(19) 1.398(6) . . yes C(20) C(21) 1.386(6) . . yes C(20) C(25) 1.388(6) . . yes C(21) C(22) 1.379(7) . . yes C(22) C(23) 1.385(7) . . yes C(23) C(24) 1.393(6) . . yes C(24) C(25) 1.404(6) . . yes C(26) C(27) 1.545(6) . . yes C(26) C(38) 1.527(5) . . yes C(27) C(28) 1.393(6) . . yes C(27) C(32) 1.394(6) . . yes C(28) C(29) 1.375(6) . . yes C(29) C(30) 1.395(7) . . yes C(30) C(31) 1.359(6) . . yes C(31) C(32) 1.386(6) . . yes C(33) C(34) 1.386(6) . . yes C(33) C(38) 1.405(6) . . yes C(34) C(35) 1.375(7) . . yes C(35) C(36) 1.386(7) . . yes C(36) C(37) 1.378(6) . . yes C(37) C(38) 1.403(6) . . yes #---------------------------------------------------------------------- loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_2 _geom_angle_site_symmetry_3 _geom_angle_publ_flag C(19) O(1) C(20) 117.0(3) . . . yes C(32) O(2) C(33) 116.7(3) . . . yes C(2) C(1) C(6) 116.7(4) . . . yes C(2) C(1) C(7) 118.4(3) . . . yes C(6) C(1) C(7) 124.8(4) . . . yes C(1) C(2) C(3) 119.8(4) . . . yes C(1) C(2) C(13) 119.1(3) . . . yes C(3) C(2) C(13) 121.0(4) . . . yes C(2) C(3) C(4) 120.3(4) . . . yes C(3) C(4) C(5) 120.1(4) . . . yes C(4) C(5) C(6) 119.0(4) . . . yes Br(1) C(6) C(1) 121.2(3) . . . yes Br(1) C(6) C(5) 116.6(3) . . . yes C(1) C(6) C(5) 121.7(4) . . . yes C(1) C(7) C(8) 119.2(4) . . . yes C(1) C(7) C(12) 123.0(4) . . . yes C(8) C(7) C(12) 117.6(4) . . . yes C(7) C(8) C(9) 119.3(4) . . . yes C(7) C(8) C(26) 119.4(3) . . . yes C(9) C(8) C(26) 121.3(4) . . . yes C(8) C(9) C(10) 120.1(4) . . . yes C(9) C(10) C(11) 120.9(4) . . . yes C(10) C(11) C(12) 118.7(4) . . . yes Br(2) C(12) C(7) 121.3(3) . . . yes Br(2) C(12) C(11) 116.6(3) . . . yes C(7) C(12) C(11) 121.6(4) . . . yes C(2) C(13) C(14) 110.5(3) . . . yes C(2) C(13) C(25) 109.7(3) . . . yes C(2) C(13) C(26) 110.1(3) . . . yes C(14) C(13) C(25) 108.3(3) . . . yes C(14) C(13) C(26) 107.2(3) . . . yes C(25) C(13) C(26) 111.0(3) . . . yes C(13) C(14) C(15) 123.4(4) . . . yes C(13) C(14) C(19) 119.8(4) . . . yes C(15) C(14) C(19) 116.6(4) . . . yes C(14) C(15) C(16) 122.2(4) . . . yes C(15) C(16) C(17) 119.5(4) . . . yes C(16) C(17) C(18) 120.4(4) . . . yes C(17) C(18) C(19) 119.5(4) . . . yes O(1) C(19) C(14) 123.1(4) . . . yes O(1) C(19) C(18) 115.1(4) . . . yes C(14) C(19) C(18) 121.8(4) . . . yes O(1) C(20) C(21) 115.8(4) . . . yes O(1) C(20) C(25) 122.3(4) . . . yes C(21) C(20) C(25) 122.0(4) . . . yes C(20) C(21) C(22) 119.9(4) . . . yes C(21) C(22) C(23) 119.8(4) . . . yes C(22) C(23) C(24) 119.8(4) . . . yes C(23) C(24) C(25) 121.3(4) . . . yes C(13) C(25) C(20) 120.3(4) . . . yes C(13) C(25) C(24) 122.7(4) . . . yes C(20) C(25) C(24) 117.0(4) . . . yes C(8) C(26) C(13) 107.8(3) . . . yes C(8) C(26) C(27) 108.8(3) . . . yes C(8) C(26) C(38) 113.6(3) . . . yes C(13) C(26) C(27) 112.7(3) . . . yes C(13) C(26) C(38) 106.5(3) . . . yes C(27) C(26) C(38) 107.5(3) . . . yes C(26) C(27) C(28) 123.2(4) . . . yes C(26) C(27) C(32) 120.1(4) . . . yes C(28) C(27) C(32) 116.5(4) . . . yes C(27) C(28) C(29) 121.5(4) . . . yes C(28) C(29) C(30) 120.3(4) . . . yes C(29) C(30) C(31) 119.6(4) . . . yes C(30) C(31) C(32) 119.7(4) . . . yes O(2) C(32) C(27) 122.3(4) . . . yes O(2) C(32) C(31) 115.3(4) . . . yes C(27) C(32) C(31) 122.4(4) . . . yes O(2) C(33) C(34) 114.9(4) . . . yes O(2) C(33) C(38) 123.5(4) . . . yes C(34) C(33) C(38) 121.6(4) . . . yes C(33) C(34) C(35) 120.0(4) . . . yes C(34) C(35) C(36) 119.8(4) . . . yes C(35) C(36) C(37) 120.3(4) . . . yes C(36) C(37) C(38) 121.5(4) . . . yes C(26) C(38) C(33) 119.0(4) . . . yes C(26) C(38) C(37) 123.7(4) . . . yes C(33) C(38) C(37) 116.8(4) . . . yes #------------------------------------------------------------------------- loop_ _geom_torsion_atom_site_label_1 _geom_torsion_atom_site_label_2 _geom_torsion_atom_site_label_3 _geom_torsion_atom_site_label_4 _geom_torsion _geom_torsion_site_symmetry_1 _geom_torsion_site_symmetry_2 _geom_torsion_site_symmetry_3 _geom_torsion_site_symmetry_4 _geom_torsion_publ_flag Br(1) C(6) C(1) C(2) -157.9(3) . . . . yes Br(1) C(6) C(1) C(7) 21.8(6) . . . . yes Br(1) C(6) C(5) C(4) 171.0(3) . . . . yes Br(2) C(12) C(7) C(1) 15.5(5) . . . . yes Br(2) C(12) C(7) C(8) -159.1(3) . . . . yes Br(2) C(12) C(11) C(10) 170.0(3) . . . . yes O(1) C(19) C(14) C(13) 5.9(6) . . . . yes O(1) C(19) C(14) C(15) -178.7(3) . . . . yes O(1) C(19) C(18) C(17) 179.0(4) . . . . yes O(1) C(20) C(21) C(22) -176.2(4) . . . . yes O(1) C(20) C(25) C(13) -6.0(6) . . . . yes O(1) C(20) C(25) C(24) 174.2(3) . . . . yes O(2) C(32) C(27) C(26) -2.4(6) . . . . yes O(2) C(32) C(27) C(28) 173.9(4) . . . . yes O(2) C(32) C(31) C(30) -175.7(4) . . . . yes O(2) C(33) C(34) C(35) 179.6(4) . . . . yes O(2) C(33) C(38) C(26) 9.6(6) . . . . yes O(2) C(33) C(38) C(37) -178.3(3) . . . . yes C(1) C(2) C(3) C(4) 8.8(6) . . . . yes C(1) C(2) C(13) C(14) -146.4(4) . . . . yes C(1) C(2) C(13) C(25) 94.2(4) . . . . yes C(1) C(2) C(13) C(26) -28.2(5) . . . . yes C(1) C(6) C(5) C(4) -1.1(7) . . . . yes C(1) C(7) C(8) C(9) 170.5(3) . . . . yes C(1) C(7) C(8) C(26) -7.6(5) . . . . yes C(1) C(7) C(12) C(11) -172.7(4) . . . . yes C(2) C(1) C(6) C(5) 13.9(6) . . . . yes C(2) C(1) C(7) C(8) 36.5(5) . . . . yes C(2) C(1) C(7) C(12) -138.0(4) . . . . yes C(2) C(3) C(4) C(5) 4.5(7) . . . . yes C(2) C(13) C(14) C(15) 37.4(5) . . . . yes C(2) C(13) C(14) C(19) -147.5(4) . . . . yes C(2) C(13) C(25) C(20) 148.2(4) . . . . yes C(2) C(13) C(25) C(24) -32.1(5) . . . . yes C(2) C(13) C(26) C(8) 51.3(4) . . . . yes C(2) C(13) C(26) C(27) -68.8(4) . . . . yes C(2) C(13) C(26) C(38) 173.6(3) . . . . yes C(3) C(2) C(1) C(6) -17.5(6) . . . . yes C(3) C(2) C(1) C(7) 162.9(4) . . . . yes C(3) C(2) C(13) C(14) 35.7(5) . . . . yes C(3) C(2) C(13) C(25) -83.6(5) . . . . yes C(3) C(2) C(13) C(26) 154.0(4) . . . . yes C(3) C(4) C(5) C(6) -8.3(7) . . . . yes C(4) C(3) C(2) C(13) -173.4(4) . . . . yes C(5) C(6) C(1) C(7) -166.5(4) . . . . yes C(6) C(1) C(2) C(13) 164.7(4) . . . . yes C(6) C(1) C(7) C(8) -143.1(4) . . . . yes C(6) C(1) C(7) C(12) 42.4(6) . . . . yes C(7) C(1) C(2) C(13) -14.9(5) . . . . yes C(7) C(8) C(9) C(10) 6.6(6) . . . . yes C(7) C(8) C(26) C(13) -34.6(5) . . . . yes C(7) C(8) C(26) C(27) 88.0(4) . . . . yes C(7) C(8) C(26) C(38) -152.4(4) . . . . yes C(7) C(12) C(11) C(10) -2.2(6) . . . . yes C(8) C(7) C(12) C(11) 12.7(6) . . . . yes C(8) C(9) C(10) C(11) 4.3(6) . . . . yes C(8) C(26) C(13) C(14) 171.6(3) . . . . yes C(8) C(26) C(13) C(25) -70.3(4) . . . . yes C(8) C(26) C(27) C(28) -25.1(5) . . . . yes C(8) C(26) C(27) C(32) 150.9(4) . . . . yes C(8) C(26) C(38) C(33) -151.2(4) . . . . yes C(8) C(26) C(38) C(37) 37.4(5) . . . . yes C(9) C(8) C(7) C(12) -14.7(6) . . . . yes C(9) C(8) C(26) C(13) 147.4(3) . . . . yes C(9) C(8) C(26) C(27) -90.1(4) . . . . yes C(9) C(8) C(26) C(38) 29.5(5) . . . . yes C(9) C(10) C(11) C(12) -6.5(6) . . . . yes C(10) C(9) C(8) C(26) -175.4(4) . . . . yes C(12) C(7) C(8) C(26) 167.2(3) . . . . yes C(13) C(14) C(15) C(16) 175.1(4) . . . . yes C(13) C(14) C(19) C(18) -174.6(4) . . . . yes C(13) C(25) C(20) C(21) 174.2(3) . . . . yes C(13) C(25) C(24) C(23) -175.7(4) . . . . yes C(13) C(26) C(27) C(28) 94.4(4) . . . . yes C(13) C(26) C(27) C(32) -89.6(4) . . . . yes C(13) C(26) C(38) C(33) 90.3(4) . . . . yes C(13) C(26) C(38) C(37) -81.2(5) . . . . yes C(14) C(13) C(25) C(20) 27.6(5) . . . . yes C(14) C(13) C(25) C(24) -152.7(4) . . . . yes C(14) C(13) C(26) C(27) 51.5(4) . . . . yes C(14) C(13) C(26) C(38) -66.2(4) . . . . yes C(14) C(15) C(16) C(17) -0.8(7) . . . . yes C(14) C(19) O(1) C(20) 18.9(5) . . . . yes C(14) C(19) C(18) C(17) -0.5(6) . . . . yes C(15) C(14) C(13) C(25) 157.6(4) . . . . yes C(15) C(14) C(13) C(26) -82.6(4) . . . . yes C(15) C(14) C(19) C(18) 0.8(6) . . . . yes C(15) C(16) C(17) C(18) 1.0(7) . . . . yes C(16) C(15) C(14) C(19) -0.1(6) . . . . yes C(16) C(17) C(18) C(19) -0.4(7) . . . . yes C(18) C(19) O(1) C(20) -160.6(3) . . . . yes C(19) O(1) C(20) C(21) 161.0(3) . . . . yes C(19) O(1) C(20) C(25) -18.8(5) . . . . yes C(19) C(14) C(13) C(25) -27.4(5) . . . . yes C(19) C(14) C(13) C(26) 92.5(4) . . . . yes C(20) C(21) C(22) C(23) 0.3(6) . . . . yes C(20) C(25) C(13) C(26) -89.9(4) . . . . yes C(20) C(25) C(24) C(23) 4.0(6) . . . . yes C(21) C(20) C(25) C(24) -5.6(6) . . . . yes C(21) C(22) C(23) C(24) -1.7(6) . . . . yes C(22) C(21) C(20) C(25) 3.5(6) . . . . yes C(22) C(23) C(24) C(25) -0.5(6) . . . . yes C(24) C(25) C(13) C(26) 89.8(4) . . . . yes C(25) C(13) C(26) C(27) 169.6(3) . . . . yes C(25) C(13) C(26) C(38) 52.0(4) . . . . yes C(26) C(27) C(28) C(29) 178.4(4) . . . . yes C(26) C(27) C(32) C(31) 179.8(4) . . . . yes C(26) C(38) C(33) C(34) -170.6(4) . . . . yes C(26) C(38) C(37) C(36) 170.7(4) . . . . yes C(27) C(26) C(38) C(33) -30.7(5) . . . . yes C(27) C(26) C(38) C(37) 157.8(4) . . . . yes C(27) C(28) C(29) C(30) 1.1(7) . . . . yes C(27) C(32) O(2) C(33) -22.6(5) . . . . yes C(27) C(32) C(31) C(30) 2.3(7) . . . . yes C(28) C(27) C(26) C(38) -148.5(4) . . . . yes C(28) C(27) C(32) C(31) -3.9(6) . . . . yes C(28) C(29) C(30) C(31) -2.8(8) . . . . yes C(29) C(28) C(27) C(32) 2.2(6) . . . . yes C(29) C(30) C(31) C(32) 1.1(7) . . . . yes C(31) C(32) O(2) C(33) 155.4(4) . . . . yes C(32) O(2) C(33) C(34) -160.8(3) . . . . yes C(32) O(2) C(33) C(38) 19.0(5) . . . . yes C(32) C(27) C(26) C(38) 27.5(5) . . . . yes C(33) C(34) C(35) C(36) -1.6(6) . . . . yes C(33) C(38) C(37) C(36) -0.9(6) . . . . yes C(34) C(33) C(38) C(37) 1.5(6) . . . . yes C(34) C(35) C(36) C(37) 2.1(6) . . . . yes C(35) C(34) C(33) C(38) -0.3(6) . . . . yes C(35) C(36) C(37) C(38) -0.8(6) . . . . yes C(35) C(36) C(37) C(38) -0.8(6) . . . . yes #------------------------------------------------------------------------- loop_ _geom_contact_atom_site_label_1 _geom_contact_atom_site_label_2 _geom_contact_distance _geom_contact_site_symmetry_1 _geom_contact_site_symmetry_2 _geom_contact_publ_flag O(1) C(18) 3.482(5) . 3_555 ? C(9) C(20) 3.566(5) . 4_555 ? C(10) C(19) 3.580(6) . 4_555 ? C(17) C(36) 3.580(6) . 2_545 ? C(22) C(33) 3.550(6) . 4_554 ? C(23) C(32) 3.558(6) . 4_554 ? C(29) C(30) 3.485(7) . 3_656 ? #----------------------------------------------------------------------- #------------------------------------- #===END #***Data of 1b*** #------------------------------------------------------------------------ data_011026_1b _database_code_CSD 185683 #----------------------------------------------------------------------- _audit_creation_date 'Mon Apr 8 15:46:22 2002' _audit_creation_method 'by teXsan' _audit_update_record ? # CHEMICAL DATA _chemical_formula_sum 'C40 H28 O2 ' _chemical_formula_moiety 'C40 H28 O2 ' _chemical_formula_weight 540.66 _chemical_melting_point ? #------------------------------------------------------------------------ # CRYSTAL DATA _symmetry_cell_setting monoclinic _symmetry_space_group_name_H-M 'P 1 21/n 1' _symmetry_Int_Tables_number 14 loop_ _symmetry_equiv_pos_as_xyz x,y,z 1/2-x,1/2+y,1/2-z -x,-y,-z 1/2+x,1/2-y,1/2+z _cell_length_a 10.059(5) _cell_length_b 14.309(7) _cell_length_c 19.109(10) _cell_angle_alpha 90 _cell_angle_beta 97.049(7) _cell_angle_gamma 90 _cell_volume 2729(2) _cell_formula_units_Z 4 _cell_measurement_reflns_used 6588 _cell_measurement_theta_min 3.1 _cell_measurement_theta_max 27.5 _cell_measurement_temperature 153.2 #------------------------------------------------------------------------ _exptl_crystal_description 'plate' _exptl_crystal_colour 'Colorless' _exptl_crystal_size_max 0.400 _exptl_crystal_size_mid 0.200 _exptl_crystal_size_min 0.050 _exptl_crystal_size_rad ? _exptl_crystal_density_diffrn 1.315 _exptl_crystal_density_meas ? _exptl_crystal_density_method 'not measured' _exptl_absorpt_coefficient_mu 0.079 _exptl_absorpt_correction_type none _exptl_absorpt_process_details ? _exptl_absorpt_correction_T_min 0.996 _exptl_absorpt_correction_T_max 0.996 #------------------------------------------------------------------------ # EXPERIMENTAL DATA _diffrn_radiation_type 'Mo K\a' _diffrn_radiation_wavelength 0.7107 _diffrn_measurement_device_type 'Rigaku/MSC Mercury CCD' _diffrn_measurement_method \w _diffrn_detector_area_resol_mean 14.62 _diffrn_reflns_number 352 _diffrn_reflns_av_R_equivalents 0.038 _diffrn_reflns_theta_max 27.49 _diffrn_measured_fraction_theta_max 0.9634 _diffrn_reflns_theta_full 27.49 _diffrn_measured_fraction_theta_full 0.9634 _diffrn_reflns_limit_h_min -7 _diffrn_reflns_limit_h_max 13 _diffrn_reflns_limit_k_min -17 _diffrn_reflns_limit_k_max 17 _diffrn_reflns_limit_l_min -24 _diffrn_reflns_limit_l_max 24 #------------------------------------------------------------------------- # REFINEMENT DATA _refine_special_details ; Refinement using reflections with F^2^ > 3.0 sigma(F^2^). The weighted R-factor (wR), goodness of fit (S) and R-factor (gt) are based on F, with F set to zero for negative F. The threshold expression of F^2^ > 3.0 sigma(F^2^) is used only for calculating R-factor (gt). ; _reflns_number_total 6033 _reflns_number_gt 2925 _reflns_threshold_expression F^2^>3.0\s(F^2^) _refine_ls_structure_factor_coef F _refine_ls_R_factor_gt 0.0567 _refine_ls_wR_factor_ref 0.0642 _refine_ls_hydrogen_treatment noref _refine_ls_number_reflns 2925 _refine_ls_number_parameters 379 _refine_ls_goodness_of_fit_ref 1.410 _refine_ls_weighting_scheme calc _refine_ls_weighting_details 'w = 1/[\s^2^(Fo) + 0.00063|Fo|^2^]' _refine_ls_shift/su_max 0.0014 _refine_diff_density_max 0.33 _refine_diff_density_min -0.34 _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_abs_structure_details ? _refine_ls_abs_structure_Flack ? loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source 'O' 'O' 0.011 0.006 ; International Tables for Crystallography (1992, Vol. C, Tables 4.2.6.8 and 6.1.1.1) ; 'C' 'C' 0.003 0.002 ; International Tables for Crystallography (1992, Vol. C, Tables 4.2.6.8 and 6.1.1.1) ; 'H' 'H' 0.000 0.000 ; International Tables for Crystallography (1992, Vol. C, Table 6.1.1.2) ; #------------------------------------------------------------------------- #ATOMIC COORDINATES AND DISPLACEMENT PARAMETERS loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_occupancy _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group O(1) O -0.2232(2) -0.3317(2) -1.2840(1) 0.0364(7) Uani 1.00 d . . . O(2) O -0.5776(2) -0.2858(1) -1.4011(1) 0.0290(6) Uani 1.00 d . . . C(1) C -0.6241(3) -0.4411(2) -1.1416(2) 0.0280(9) Uani 1.00 d . . . C(2) C -0.5314(3) -0.4693(2) -1.1868(2) 0.0243(9) Uani 1.00 d . . . C(3) C -0.5051(3) -0.5639(2) -1.1939(2) 0.0294(9) Uani 1.00 d . . . C(4) C -0.5778(4) -0.6301(2) -1.1622(2) 0.039(1) Uani 1.00 d . . . C(5) C -0.6803(4) -0.6019(3) -1.1254(2) 0.043(1) Uani 1.00 d . . . C(6) C -0.7068(4) -0.5083(2) -1.1149(2) 0.039(1) Uani 1.00 d . . . C(7) C -0.6402(3) -0.3399(2) -1.1277(2) 0.0272(9) Uani 1.00 d . . . C(8) C -0.6300(3) -0.2768(2) -1.1829(2) 0.0227(8) Uani 1.00 d . . . C(9) C -0.6719(3) -0.1850(2) -1.1766(2) 0.0313(10) Uani 1.00 d . . . C(10) C -0.7099(4) -0.1536(2) -1.1134(2) 0.042(1) Uani 1.00 d . . . C(11) C -0.6995(4) -0.2114(3) -1.0559(2) 0.045(1) Uani 1.00 d . . . C(12) C -0.6625(4) -0.3045(3) -1.0610(2) 0.039(1) Uani 1.00 d . . . C(13) C -0.4640(3) -0.3948(2) -1.2275(2) 0.0224(8) Uani 1.00 d . . . C(14) C -0.4202(3) -0.4311(2) -1.2962(2) 0.0251(9) Uani 1.00 d . . . C(15) C -0.4945(4) -0.4963(2) -1.3393(2) 0.0311(10) Uani 1.00 d . . . C(16) C -0.4568(4) -0.5239(2) -1.4033(2) 0.042(1) Uani 1.00 d . . . C(17) C -0.3443(5) -0.4861(3) -1.4263(2) 0.050(1) Uani 1.00 d . . . C(18) C -0.2688(4) -0.4211(3) -1.3857(2) 0.040(1) Uani 1.00 d . . . C(19) C -0.3074(3) -0.3955(2) -1.3213(2) 0.0306(10) Uani 1.00 d . . . C(20) C -0.2274(3) -0.3278(2) -1.2120(2) 0.0296(10) Uani 1.00 d . . . C(21) C -0.1134(3) -0.2913(2) -1.1737(2) 0.039(1) Uani 1.00 d . . . C(22) C -0.1071(4) -0.2863(2) -1.1007(2) 0.040(1) Uani 1.00 d . . . C(23) C -0.2118(4) -0.3197(2) -1.0682(2) 0.0343(10) Uani 1.00 d . . . C(24) C -0.3246(3) -0.3556(2) -1.1078(2) 0.0288(9) Uani 1.00 d . . . C(25) C -0.3376(3) -0.3581(2) -1.1813(2) 0.0217(8) Uani 1.00 d . . . C(26) C -0.5730(3) -0.3101(2) -1.2489(2) 0.0209(8) Uani 1.00 d . . . C(27) C -0.6874(3) -0.3442(2) -1.3034(2) 0.0224(9) Uani 1.00 d . . . C(28) C -0.8031(3) -0.3873(2) -1.2850(2) 0.0266(9) Uani 1.00 d . . . C(29) C -0.9036(3) -0.4189(2) -1.3346(2) 0.0320(10) Uani 1.00 d . . . C(30) C -0.8940(3) -0.4063(2) -1.4059(2) 0.0331(10) Uani 1.00 d . . . C(31) C -0.7837(3) -0.3615(2) -1.4261(2) 0.0284(9) Uani 1.00 d . . . C(32) C -0.6827(3) -0.3313(2) -1.3753(2) 0.0241(9) Uani 1.00 d . . . C(33) C -0.5004(3) -0.2269(2) -1.3548(2) 0.0283(9) Uani 1.00 d . . . C(34) C -0.4256(4) -0.1622(2) -1.3871(2) 0.038(1) Uani 1.00 d . . . C(35) C -0.3482(4) -0.0987(3) -1.3462(2) 0.046(1) Uani 1.00 d . . . C(36) C -0.3472(4) -0.1002(2) -1.2737(2) 0.039(1) Uani 1.00 d . . . C(37) C -0.4201(3) -0.1659(2) -1.2421(2) 0.0302(10) Uani 1.00 d . . . C(38) C -0.4993(3) -0.2324(2) -1.2826(2) 0.0234(9) Uani 1.00 d . . . C(39) C -0.8317(5) -0.4828(3) -1.0811(3) 0.072(2) Uani 1.00 d . . . C(40) C -0.6314(5) -0.3599(3) -0.9940(2) 0.067(2) Uani 1.00 d . . . H(1) H -0.4352 -0.5834 -1.2214 0.0366 Uiso 1.00 calc . . . H(2) H -0.5559 -0.6957 -1.1655 0.0500 Uiso 1.00 calc . . . H(3) H -0.7351 -0.6488 -1.1060 0.0521 Uiso 1.00 calc . . . H(4) H -0.6751 -0.1430 -1.2175 0.0408 Uiso 1.00 calc . . . H(5) H -0.7442 -0.0901 -1.1095 0.0529 Uiso 1.00 calc . . . H(6) H -0.7168 -0.1878 -1.0108 0.0568 Uiso 1.00 calc . . . H(7) H -0.5751 -0.5219 -1.3237 0.0395 Uiso 1.00 calc . . . H(8) H -0.5096 -0.5702 -1.4314 0.0514 Uiso 1.00 calc . . . H(9) H -0.3201 -0.5053 -1.4711 0.0593 Uiso 1.00 calc . . . H(10) H -0.1909 -0.3935 -1.4021 0.0481 Uiso 1.00 calc . . . H(11) H -0.0393 -0.2707 -1.1980 0.0466 Uiso 1.00 calc . . . H(12) H -0.0298 -0.2590 -1.0730 0.0489 Uiso 1.00 calc . . . H(13) H -0.2059 -0.3182 -1.0174 0.0416 Uiso 1.00 calc . . . H(14) H -0.3972 -0.3793 -1.0843 0.0350 Uiso 1.00 calc . . . H(15) H -0.8121 -0.3933 -1.2353 0.0326 Uiso 1.00 calc . . . H(16) H -0.9810 -0.4504 -1.3199 0.0415 Uiso 1.00 calc . . . H(17) H -0.9638 -0.4288 -1.4406 0.0391 Uiso 1.00 calc . . . H(18) H -0.7757 -0.3514 -1.4753 0.0343 Uiso 1.00 calc . . . H(19) H -0.4288 -0.1616 -1.4378 0.0442 Uiso 1.00 calc . . . H(20) H -0.2942 -0.0541 -1.3686 0.0538 Uiso 1.00 calc . . . H(21) H -0.2965 -0.0537 -1.2449 0.0475 Uiso 1.00 calc . . . H(22) H -0.4172 -0.1669 -1.1917 0.0381 Uiso 1.00 calc . . . H(23) H -0.8388 -0.4150 -1.0773 0.0873 Uiso 1.00 calc . . . H(24) H -0.9110 -0.5039 -1.1090 0.0873 Uiso 1.00 calc . . . H(25) H -0.8288 -0.5077 -1.0349 0.0873 Uiso 1.00 calc . . . H(26) H -0.7067 -0.3624 -0.9680 0.0809 Uiso 1.00 calc . . . H(27) H -0.6063 -0.4231 -1.0035 0.0809 Uiso 1.00 calc . . . H(28) H -0.5578 -0.3324 -0.9639 0.0809 Uiso 1.00 calc . . . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_12 _atom_site_aniso_U_13 _atom_site_aniso_U_23 O(1) 0.025(1) 0.053(2) 0.032(1) 0.000(1) 0.005(1) 0.006(1) O(2) 0.027(1) 0.031(1) 0.029(1) -0.006(1) 0.002(1) 0.003(1) C(1) 0.025(2) 0.031(2) 0.027(2) 0.000(1) -0.001(2) 0.007(2) C(2) 0.024(2) 0.023(2) 0.025(2) -0.002(1) -0.004(2) 0.002(1) C(3) 0.032(2) 0.026(2) 0.029(2) 0.000(2) 0.000(2) -0.001(2) C(4) 0.048(2) 0.029(2) 0.038(2) -0.005(2) -0.007(2) 0.002(2) C(5) 0.044(2) 0.036(2) 0.048(3) -0.015(2) 0.002(2) 0.014(2) C(6) 0.031(2) 0.043(2) 0.041(2) -0.003(2) 0.003(2) 0.013(2) C(7) 0.019(2) 0.037(2) 0.027(2) 0.003(1) 0.004(1) -0.004(2) C(8) 0.016(2) 0.026(2) 0.025(2) -0.002(1) 0.001(1) -0.005(1) C(9) 0.028(2) 0.026(2) 0.040(2) -0.001(1) 0.007(2) -0.006(2) C(10) 0.036(2) 0.042(2) 0.048(2) 0.008(2) 0.007(2) -0.015(2) C(11) 0.041(2) 0.064(3) 0.030(2) 0.012(2) 0.007(2) -0.016(2) C(12) 0.035(2) 0.053(2) 0.029(2) 0.010(2) 0.004(2) -0.002(2) C(13) 0.022(2) 0.021(2) 0.024(2) 0.001(1) 0.004(1) 0.000(1) C(14) 0.025(2) 0.025(2) 0.024(2) 0.007(1) 0.000(2) 0.002(1) C(15) 0.036(2) 0.028(2) 0.029(2) 0.009(2) 0.000(2) -0.002(2) C(16) 0.051(3) 0.043(2) 0.030(2) 0.018(2) -0.006(2) -0.009(2) C(17) 0.059(3) 0.070(3) 0.021(2) 0.033(2) 0.005(2) -0.002(2) C(18) 0.029(2) 0.063(3) 0.028(2) 0.020(2) 0.007(2) 0.012(2) C(19) 0.025(2) 0.041(2) 0.025(2) 0.013(2) 0.001(2) 0.003(2) C(20) 0.024(2) 0.035(2) 0.029(2) 0.002(2) 0.000(2) 0.006(2) C(21) 0.022(2) 0.043(2) 0.049(2) -0.005(2) -0.004(2) 0.007(2) C(22) 0.032(2) 0.038(2) 0.047(2) -0.006(2) -0.012(2) 0.002(2) C(23) 0.037(2) 0.035(2) 0.029(2) 0.005(2) -0.007(2) -0.003(2) C(24) 0.024(2) 0.029(2) 0.032(2) 0.002(1) 0.000(2) -0.001(2) C(25) 0.022(2) 0.018(1) 0.024(2) 0.000(1) -0.001(1) 0.000(1) C(26) 0.019(2) 0.019(1) 0.023(2) 0.000(1) -0.001(1) 0.000(1) C(27) 0.022(2) 0.018(2) 0.026(2) 0.003(1) -0.001(1) -0.001(1) C(28) 0.023(2) 0.026(2) 0.030(2) 0.002(1) 0.002(2) 0.002(1) C(29) 0.023(2) 0.033(2) 0.039(2) -0.006(1) -0.001(2) 0.001(2) C(30) 0.026(2) 0.030(2) 0.041(2) -0.004(2) -0.006(2) -0.003(2) C(31) 0.033(2) 0.026(2) 0.025(2) 0.002(2) -0.002(2) -0.001(1) C(32) 0.023(2) 0.019(2) 0.030(2) 0.004(1) 0.003(2) 0.001(1) C(33) 0.021(2) 0.030(2) 0.033(2) -0.001(2) 0.000(2) 0.004(2) C(34) 0.034(2) 0.043(2) 0.038(2) -0.008(2) 0.005(2) 0.010(2) C(35) 0.043(2) 0.043(2) 0.052(3) -0.018(2) 0.008(2) 0.010(2) C(36) 0.031(2) 0.033(2) 0.054(3) -0.012(2) 0.004(2) -0.005(2) C(37) 0.027(2) 0.027(2) 0.037(2) -0.002(2) 0.003(2) -0.002(2) C(38) 0.019(2) 0.021(2) 0.031(2) 0.003(1) 0.004(1) 0.001(1) C(39) 0.048(3) 0.070(3) 0.103(4) -0.001(2) 0.033(3) 0.029(3) C(40) 0.068(3) 0.105(4) 0.031(2) 0.033(3) 0.014(2) 0.008(2) #------------------------------------------------------------------------ _computing_data_collection 'CRYSTALCLEAR' _computing_cell_refinement 'CRYSTALCLEAR' _computing_data_reduction 'teXsan Ver. 1.11' _computing_structure_solution SAPI91 _computing_structure_refinement 'teXsan Ver. 1.10' _computing_publication_material 'teXsan Ver. 1.11' _computing_molecular_graphics ? #------------------------------------------------------------------------ _geom_special_details ; ? ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_1 _geom_bond_site_symmetry_2 _geom_bond_publ_flag O(1) C(19) 1.383(4) . . yes O(1) C(20) 1.381(4) . . yes O(2) C(32) 1.383(4) . . yes O(2) C(33) 1.388(4) . . yes C(1) C(2) 1.406(4) . . yes C(1) C(6) 1.408(4) . . yes C(1) C(7) 1.485(4) . . yes C(2) C(3) 1.388(4) . . yes C(2) C(13) 1.526(4) . . yes C(3) C(4) 1.381(5) . . yes C(4) C(5) 1.377(5) . . yes C(5) C(6) 1.386(5) . . yes C(6) C(39) 1.526(6) . . yes C(7) C(8) 1.402(4) . . yes C(7) C(12) 1.415(4) . . yes C(8) C(9) 1.390(4) . . yes C(8) C(26) 1.525(4) . . yes C(9) C(10) 1.384(5) . . yes C(10) C(11) 1.369(5) . . yes C(11) C(12) 1.388(5) . . yes C(12) C(40) 1.506(5) . . yes C(13) C(14) 1.525(4) . . yes C(13) C(25) 1.548(4) . . yes C(13) C(26) 1.652(4) . . yes C(14) C(15) 1.400(4) . . yes C(14) C(19) 1.383(4) . . yes C(15) C(16) 1.381(5) . . yes C(16) C(17) 1.375(6) . . yes C(17) C(18) 1.378(5) . . yes C(18) C(19) 1.385(5) . . yes C(20) C(21) 1.386(5) . . yes C(20) C(25) 1.385(4) . . yes C(21) C(22) 1.390(5) . . yes C(22) C(23) 1.372(5) . . yes C(23) C(24) 1.383(5) . . yes C(24) C(25) 1.395(4) . . yes C(26) C(27) 1.534(4) . . yes C(26) C(38) 1.522(4) . . yes C(27) C(28) 1.400(4) . . yes C(27) C(32) 1.392(4) . . yes C(28) C(29) 1.376(4) . . yes C(29) C(30) 1.388(5) . . yes C(30) C(31) 1.377(5) . . yes C(31) C(32) 1.386(4) . . yes C(33) C(34) 1.385(4) . . yes C(33) C(38) 1.379(4) . . yes C(34) C(35) 1.376(5) . . yes C(35) C(36) 1.385(5) . . yes C(36) C(37) 1.377(5) . . yes C(37) C(38) 1.411(4) . . yes #----------------------------------------------------------------------- loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_2 _geom_angle_site_symmetry_3 _geom_angle_publ_flag C(19) O(1) C(20) 116.6(3) . . . yes C(32) O(2) C(33) 116.8(2) . . . yes C(2) C(1) C(6) 119.6(3) . . . yes C(2) C(1) C(7) 119.0(3) . . . yes C(6) C(1) C(7) 121.2(3) . . . yes C(1) C(2) C(3) 119.2(3) . . . yes C(1) C(2) C(13) 118.8(3) . . . yes C(3) C(2) C(13) 121.9(3) . . . yes C(2) C(3) C(4) 120.5(3) . . . yes C(3) C(4) C(5) 119.6(3) . . . yes C(4) C(5) C(6) 121.8(3) . . . yes C(1) C(6) C(5) 118.3(3) . . . yes C(1) C(6) C(39) 123.0(3) . . . yes C(5) C(6) C(39) 118.5(3) . . . yes C(1) C(7) C(8) 118.3(3) . . . yes C(1) C(7) C(12) 123.0(3) . . . yes C(8) C(7) C(12) 118.8(3) . . . yes C(7) C(8) C(9) 119.5(3) . . . yes C(7) C(8) C(26) 119.4(3) . . . yes C(9) C(8) C(26) 121.1(3) . . . yes C(8) C(9) C(10) 120.1(3) . . . yes C(9) C(10) C(11) 120.2(3) . . . yes C(10) C(11) C(12) 121.2(3) . . . yes C(7) C(12) C(11) 118.7(3) . . . yes C(7) C(12) C(40) 122.5(3) . . . yes C(11) C(12) C(40) 118.4(3) . . . yes C(2) C(13) C(14) 113.2(2) . . . yes C(2) C(13) C(25) 109.4(2) . . . yes C(2) C(13) C(26) 108.4(2) . . . yes C(14) C(13) C(25) 107.6(3) . . . yes C(14) C(13) C(26) 106.8(2) . . . yes C(25) C(13) C(26) 111.5(2) . . . yes C(13) C(14) C(15) 123.0(3) . . . yes C(13) C(14) C(19) 120.6(3) . . . yes C(15) C(14) C(19) 116.3(3) . . . yes C(14) C(15) C(16) 121.8(3) . . . yes C(15) C(16) C(17) 119.8(4) . . . yes C(16) C(17) C(18) 120.2(3) . . . yes C(17) C(18) C(19) 118.9(3) . . . yes O(1) C(19) C(14) 122.7(3) . . . yes O(1) C(19) C(18) 114.4(3) . . . yes C(14) C(19) C(18) 122.9(3) . . . yes O(1) C(20) C(21) 114.6(3) . . . yes O(1) C(20) C(25) 122.2(3) . . . yes C(21) C(20) C(25) 123.2(3) . . . yes C(20) C(21) C(22) 118.9(3) . . . yes C(21) C(22) C(23) 119.5(3) . . . yes C(22) C(23) C(24) 120.3(3) . . . yes C(23) C(24) C(25) 122.0(3) . . . yes C(13) C(25) C(20) 120.6(3) . . . yes C(13) C(25) C(24) 123.4(3) . . . yes C(20) C(25) C(24) 115.9(3) . . . yes C(8) C(26) C(13) 109.2(2) . . . yes C(8) C(26) C(27) 109.5(2) . . . yes C(8) C(26) C(38) 112.0(2) . . . yes C(13) C(26) C(27) 110.8(2) . . . yes C(13) C(26) C(38) 107.3(2) . . . yes C(27) C(26) C(38) 108.0(2) . . . yes C(26) C(27) C(28) 123.2(3) . . . yes C(26) C(27) C(32) 120.9(3) . . . yes C(28) C(27) C(32) 115.9(3) . . . yes C(27) C(28) C(29) 122.3(3) . . . yes C(28) C(29) C(30) 120.0(3) . . . yes C(29) C(30) C(31) 119.4(3) . . . yes C(30) C(31) C(32) 119.7(3) . . . yes O(2) C(32) C(27) 122.3(3) . . . yes O(2) C(32) C(31) 115.1(3) . . . yes C(27) C(32) C(31) 122.6(3) . . . yes O(2) C(33) C(34) 114.4(3) . . . yes O(2) C(33) C(38) 122.5(3) . . . yes C(34) C(33) C(38) 123.0(3) . . . yes C(33) C(34) C(35) 119.3(3) . . . yes C(34) C(35) C(36) 119.5(3) . . . yes C(35) C(36) C(37) 120.7(3) . . . yes C(36) C(37) C(38) 121.0(3) . . . yes C(26) C(38) C(33) 121.3(3) . . . yes C(26) C(38) C(37) 122.1(3) . . . yes C(33) C(38) C(37) 116.4(3) . . . yes #------------------------------------------------------------------------- loop_ _geom_torsion_atom_site_label_1 _geom_torsion_atom_site_label_2 _geom_torsion_atom_site_label_3 _geom_torsion_atom_site_label_4 _geom_torsion _geom_torsion_site_symmetry_1 _geom_torsion_site_symmetry_2 _geom_torsion_site_symmetry_3 _geom_torsion_site_symmetry_4 _geom_torsion_publ_flag O(1) C(19) C(14) C(13) 5.1(5) . . . . yes O(1) C(19) C(14) C(15) -178.9(3) . . . . yes O(1) C(19) C(18) C(17) 178.5(3) . . . . yes O(1) C(20) C(21) C(22) -178.8(3) . . . . yes O(1) C(20) C(25) C(13) -2.1(5) . . . . yes O(1) C(20) C(25) C(24) 176.1(3) . . . . yes O(2) C(32) C(27) C(26) -1.5(4) . . . . yes O(2) C(32) C(27) C(28) 176.8(3) . . . . yes O(2) C(32) C(31) C(30) -178.9(3) . . . . yes O(2) C(33) C(34) C(35) 178.2(3) . . . . yes O(2) C(33) C(38) C(26) 6.0(5) . . . . yes O(2) C(33) C(38) C(37) -177.6(3) . . . . yes C(1) C(2) C(3) C(4) 5.9(5) . . . . yes C(1) C(2) C(13) C(14) -153.3(3) . . . . yes C(1) C(2) C(13) C(25) 86.8(3) . . . . yes C(1) C(2) C(13) C(26) -35.0(4) . . . . yes C(1) C(6) C(5) C(4) -1.3(6) . . . . yes C(1) C(7) C(8) C(9) 166.5(3) . . . . yes C(1) C(7) C(8) C(26) -13.6(4) . . . . yes C(1) C(7) C(12) C(11) -168.8(3) . . . . yes C(1) C(7) C(12) C(40) 19.0(6) . . . . yes C(2) C(1) C(6) C(5) 9.6(5) . . . . yes C(2) C(1) C(6) C(39) -164.5(4) . . . . yes C(2) C(1) C(7) C(8) 36.2(5) . . . . yes C(2) C(1) C(7) C(12) -142.6(3) . . . . yes C(2) C(3) C(4) C(5) 2.4(5) . . . . yes C(2) C(13) C(14) C(15) 36.7(4) . . . . yes C(2) C(13) C(14) C(19) -147.6(3) . . . . yes C(2) C(13) C(25) C(20) 148.7(3) . . . . yes C(2) C(13) C(25) C(24) -29.5(4) . . . . yes C(2) C(13) C(26) C(8) 52.6(3) . . . . yes C(2) C(13) C(26) C(27) -68.0(3) . . . . yes C(2) C(13) C(26) C(38) 174.3(2) . . . . yes C(3) C(2) C(1) C(6) -11.9(5) . . . . yes C(3) C(2) C(1) C(7) 172.9(3) . . . . yes C(3) C(2) C(13) C(14) 25.8(4) . . . . yes C(3) C(2) C(13) C(25) -94.2(3) . . . . yes C(3) C(2) C(13) C(26) 144.1(3) . . . . yes C(3) C(4) C(5) C(6) -4.7(6) . . . . yes C(4) C(3) C(2) C(13) -173.2(3) . . . . yes C(4) C(5) C(6) C(39) 173.0(4) . . . . yes C(5) C(6) C(1) C(7) -175.3(3) . . . . yes C(6) C(1) C(2) C(13) 167.2(3) . . . . yes C(6) C(1) C(7) C(8) -139.0(3) . . . . yes C(6) C(1) C(7) C(12) 42.3(5) . . . . yes C(7) C(1) C(2) C(13) -8.0(4) . . . . yes C(7) C(1) C(6) C(39) 10.6(6) . . . . yes C(7) C(8) C(9) C(10) 6.8(5) . . . . yes C(7) C(8) C(26) C(13) -29.8(4) . . . . yes C(7) C(8) C(26) C(27) 91.7(3) . . . . yes C(7) C(8) C(26) C(38) -148.5(3) . . . . yes C(7) C(12) C(11) C(10) -2.3(6) . . . . yes C(8) C(7) C(12) C(11) 12.4(5) . . . . yes C(8) C(7) C(12) C(40) -159.8(4) . . . . yes C(8) C(9) C(10) C(11) 3.5(5) . . . . yes C(8) C(26) C(13) C(14) 174.9(2) . . . . yes C(8) C(26) C(13) C(25) -67.8(3) . . . . yes C(8) C(26) C(27) C(28) -32.9(4) . . . . yes C(8) C(26) C(27) C(32) 145.3(3) . . . . yes C(8) C(26) C(38) C(33) -146.0(3) . . . . yes C(8) C(26) C(38) C(37) 37.9(4) . . . . yes C(9) C(8) C(7) C(12) -14.7(5) . . . . yes C(9) C(8) C(26) C(13) 150.1(3) . . . . yes C(9) C(8) C(26) C(27) -88.4(3) . . . . yes C(9) C(8) C(26) C(38) 31.4(4) . . . . yes C(9) C(10) C(11) C(12) -5.7(6) . . . . yes C(10) C(9) C(8) C(26) -173.1(3) . . . . yes C(10) C(11) C(12) C(40) 170.2(4) . . . . yes C(12) C(7) C(8) C(26) 165.2(3) . . . . yes C(13) C(14) C(15) C(16) 176.2(3) . . . . yes C(13) C(14) C(19) C(18) -175.3(3) . . . . yes C(13) C(25) C(20) C(21) 177.7(3) . . . . yes C(13) C(25) C(24) C(23) -178.0(3) . . . . yes C(13) C(26) C(27) C(28) 87.7(3) . . . . yes C(13) C(26) C(27) C(32) -94.2(3) . . . . yes C(13) C(26) C(38) C(33) 94.1(3) . . . . yes C(13) C(26) C(38) C(37) -82.0(3) . . . . yes C(14) C(13) C(25) C(20) 25.3(4) . . . . yes C(14) C(13) C(25) C(24) -152.8(3) . . . . yes C(14) C(13) C(26) C(27) 54.3(3) . . . . yes C(14) C(13) C(26) C(38) -63.4(3) . . . . yes C(14) C(15) C(16) C(17) -0.8(5) . . . . yes C(14) C(19) O(1) C(20) 21.4(4) . . . . yes C(14) C(19) C(18) C(17) -1.2(5) . . . . yes C(15) C(14) C(13) C(25) 157.6(3) . . . . yes C(15) C(14) C(13) C(26) -82.6(3) . . . . yes C(15) C(14) C(19) C(18) 0.7(5) . . . . yes C(15) C(16) C(17) C(18) 0.3(6) . . . . yes C(16) C(15) C(14) C(19) 0.3(5) . . . . yes C(16) C(17) C(18) C(19) 0.7(5) . . . . yes C(18) C(19) O(1) C(20) -158.2(3) . . . . yes C(19) O(1) C(20) C(21) 157.4(3) . . . . yes C(19) O(1) C(20) C(25) -22.7(4) . . . . yes C(19) C(14) C(13) C(25) -26.7(4) . . . . yes C(19) C(14) C(13) C(26) 93.1(3) . . . . yes C(20) C(21) C(22) C(23) 1.7(5) . . . . yes C(20) C(25) C(13) C(26) -91.4(3) . . . . yes C(20) C(25) C(24) C(23) 3.8(5) . . . . yes C(21) C(20) C(25) C(24) -4.0(5) . . . . yes C(21) C(22) C(23) C(24) -1.9(5) . . . . yes C(22) C(21) C(20) C(25) 1.4(5) . . . . yes C(22) C(23) C(24) C(25) -0.9(5) . . . . yes C(24) C(25) C(13) C(26) 90.5(3) . . . . yes C(25) C(13) C(26) C(27) 171.5(2) . . . . yes C(25) C(13) C(26) C(38) 53.8(3) . . . . yes C(26) C(27) C(28) C(29) -178.8(3) . . . . yes C(26) C(27) C(32) C(31) 179.7(3) . . . . yes C(26) C(38) C(33) C(34) -174.4(3) . . . . yes C(26) C(38) C(37) C(36) 175.6(3) . . . . yes C(27) C(26) C(38) C(33) -25.4(4) . . . . yes C(27) C(26) C(38) C(37) 158.5(3) . . . . yes C(27) C(28) C(29) C(30) -1.8(5) . . . . yes C(27) C(32) O(2) C(33) -20.9(4) . . . . yes C(27) C(32) C(31) C(30) -0.1(5) . . . . yes C(28) C(27) C(26) C(38) -155.1(3) . . . . yes C(28) C(27) C(32) C(31) -2.0(4) . . . . yes C(28) C(29) C(30) C(31) -0.4(5) . . . . yes C(29) C(28) C(27) C(32) 2.9(5) . . . . yes C(29) C(30) C(31) C(32) 1.3(5) . . . . yes C(31) C(32) O(2) C(33) 158.0(3) . . . . yes C(32) O(2) C(33) C(34) -160.9(3) . . . . yes C(32) O(2) C(33) C(38) 18.7(4) . . . . yes C(32) C(27) C(26) C(38) 23.1(4) . . . . yes C(33) C(34) C(35) C(36) -0.5(6) . . . . yes C(33) C(38) C(37) C(36) -0.7(5) . . . . yes C(34) C(33) C(38) C(37) 2.0(5) . . . . yes C(34) C(35) C(36) C(37) 1.7(6) . . . . yes C(35) C(34) C(33) C(38) -1.4(5) . . . . yes C(35) C(36) C(37) C(38) -1.1(5) . . . . yes C(35) C(36) C(37) C(38) -1.1(5) . . . . yes #------------------------------------------------------------------------ loop_ _geom_contact_atom_site_label_1 _geom_contact_atom_site_label_2 _geom_contact_distance _geom_contact_site_symmetry_1 _geom_contact_site_symmetry_2 _geom_contact_publ_flag C(3) C(35) 3.577(5) . 2_442 ? C(4) C(40) 3.437(6) . 3_443 ? C(5) C(32) 3.561(4) . 2_342 ? C(34) C(39) 3.543(6) . 2_352 ? #------------------------------------------------------------------------- #------------------------------------------------------------------------- #===END #***Data of 6*** data_1_3-butanediol_adduct_-150 _database_code_CSD 185684 _audit_creation_date 'Tue Feb 12 15:51:58 2002' _audit_creation_method 'by teXsan' _audit_update_record ? #------------------------------------------------------------------------ # CHEMICAL DATA _chemical_formula_sum 'C46 H40 Br2 O6 ' _chemical_formula_moiety 'C46 H40 Br2 O6 ' _chemical_formula_weight 848.63 _chemical_melting_point ? #------------------------------------------------------------------------ # CRYSTAL DATA _symmetry_cell_setting monoclinic _symmetry_space_group_name_H-M 'C 1 2 1' _symmetry_Int_Tables_number 5 loop_ _symmetry_equiv_pos_as_xyz x,y,z -x,y,-z 1/2+x,1/2+y,z 1/2-x,1/2+y,-z _cell_length_a 21.614(2) _cell_length_b 9.8916(8) _cell_length_c 9.6740(4) _cell_angle_alpha 90 _cell_angle_beta 113.459(2) _cell_angle_gamma 90 _cell_volume 1897.3(2) _cell_formula_units_Z 2 _cell_measurement_reflns_used ? _cell_measurement_theta_min ? _cell_measurement_theta_max ? _cell_measurement_temperature 123.2 #---------------------------------------------------------------------- _exptl_crystal_description 'plate' _exptl_crystal_colour 'colorless' _exptl_crystal_size_max 0.100 _exptl_crystal_size_mid 0.100 _exptl_crystal_size_min 0.030 _exptl_crystal_size_rad ? _exptl_crystal_density_diffrn 1.485 _exptl_crystal_density_meas ? _exptl_crystal_density_method 'not measured' _exptl_absorpt_coefficient_mu 2.193 _exptl_absorpt_correction_type none #----------------------------------------------------------------------- #EXPERIMENTAL DATA _diffrn_radiation_type 'Mo K\a' _diffrn_radiation_wavelength 0.7107 _diffrn_measurement_device_type 'Rigaku/MSC Mercury CCD' _diffrn_measurement_method \w _diffrn_detector_area_resol_mean ? _diffrn_reflns_number 5256 _diffrn_reflns_av_R_equivalents 0.038 _diffrn_reflns_theta_max 27.48 _diffrn_measured_fraction_theta_max 0.9835 _diffrn_reflns_theta_full 27.48 _diffrn_measured_fraction_theta_full 0.9835 _diffrn_reflns_limit_h_min -27 _diffrn_reflns_limit_h_max 26 _diffrn_reflns_limit_k_min -12 _diffrn_reflns_limit_k_max 12 _diffrn_reflns_limit_l_min -7 _diffrn_reflns_limit_l_max 12 #----------------------------------------------------------------------- #REFINEMENT DATA _refine_special_details ; Refinement using reflections with F^2^ > 3.0 sigma(F^2^). The weighted R-factor (wR), goodness of fit (S) and R-factor (gt) are based on F, with F set to zero for negative F. The threshold expression of F^2^ > 3.0 sigma(F^2^) is used only for calculating R-factor (gt). ; _reflns_number_total 2261 _reflns_number_gt 1777 _reflns_threshold_expression F^2^>3.0\s(F^2^) _refine_ls_structure_factor_coef F _refine_ls_R_factor_gt 0.0324 _refine_ls_wR_factor_ref 0.0412 _refine_ls_hydrogen_treatment noref _refine_ls_number_reflns 1777 _refine_ls_number_parameters 245 _refine_ls_goodness_of_fit_ref 1.007 _refine_ls_weighting_scheme calc _refine_ls_weighting_details 'w = 1/[\s^2^(Fo) + 0.00063|Fo|^2^]' _refine_ls_shift/su_max 0.0029 _refine_diff_density_max 0.37 _refine_diff_density_min -0.38 _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_abs_structure_details ? _refine_ls_abs_structure_Flack 0.40(4) loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source 'C' 'C' 0.003 0.002 ; International Tables for Crystallography (1992, Vol. C, Tables 4.2.6.8 and 6.1.1.1) ; 'H' 'H' 0.000 0.000 ; International Tables for Crystallography (1992, Vol. C, Table 6.1.1.2) ; 'O' 'O' 0.011 0.006 ; International Tables for Crystallography (1992, Vol. C, Tables 4.2.6.8 and 6.1.1.1) ; 'Br' 'Br' -0.290 2.459 ; International Tables for Crystallography (1992, Vol. C, Tables 4.2.6.8 and 6.1.1.1) ; #----------------------------------------------------------------------------- #ATOMIC COORDINATES AND DISPLACEMENT PARAMETERS loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_occupancy _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group Br(1) Br -0.09442(2) -0.012(2) -0.10717(6) 0.0278(1) Uani 1.00 d . . . O(1) O 0.1493(2) 0.574(2) 0.4923(6) 0.029(1) Uani 1.00 d . . . O(2) O 0.0999(2) 0.386(2) 0.1333(4) 0.0176(8) Uani 1.00 d . . . O(3) O 0.2772(2) 0.329(2) 0.3248(5) 0.034(1) Uani 1.00 d . . . C(1) C -0.0127(2) 0.209(2) 0.0619(6) 0.019(1) Uani 1.00 d . . . C(2) C 0.0112(2) 0.291(2) 0.1935(6) 0.017(1) Uani 1.00 d . . . C(3) C -0.0199(3) 0.283(2) 0.2952(6) 0.023(1) Uani 1.00 d . . . C(4) C -0.0727(3) 0.197(2) 0.2752(7) 0.028(1) Uani 1.00 d . . . C(5) C -0.0942(2) 0.110(2) 0.1531(7) 0.026(1) Uani 1.00 d . . . C(6) C -0.0647(2) 0.118(2) 0.0501(6) 0.023(1) Uani 1.00 d . . . C(7) C 0.0722(2) 0.390(2) 0.2474(6) 0.018(1) Uani 1.00 d . . . C(8) C 0.1259(3) 0.342(2) 0.3980(6) 0.020(1) Uani 1.00 d . . . C(9) C 0.1442(3) 0.207(2) 0.4256(6) 0.022(1) Uani 1.00 d . . . C(10) C 0.1982(3) 0.165(2) 0.5535(7) 0.026(1) Uani 1.00 d . . . C(11) C 0.2361(3) 0.264(2) 0.6585(6) 0.027(1) Uani 1.00 d . . . C(12) C 0.2186(3) 0.397(2) 0.6337(7) 0.030(1) Uani 1.00 d . . . C(13) C 0.1627(3) 0.435(2) 0.5057(7) 0.020(1) Uani 1.00 d . . . C(14) C 0.0886(3) 0.614(2) 0.3820(7) 0.024(1) Uani 1.00 d . . . C(15) C 0.0688(3) 0.745(2) 0.3993(7) 0.030(1) Uani 1.00 d . . . C(16) C 0.0093(3) 0.794(2) 0.2965(7) 0.031(2) Uani 1.00 d . . . C(17) C -0.0312(3) 0.714(2) 0.1767(7) 0.027(1) Uani 1.00 d . . . C(18) C -0.0121(3) 0.584(2) 0.1610(6) 0.023(1) Uani 1.00 d . . . C(19) C 0.0491(3) 0.531(2) 0.2643(6) 0.020(1) Uani 1.00 d . . . C(20) C 0.1549(2) 0.477(2) 0.1589(5) 0.021(1) Uani 1.00 d . . . C(21) C 0.2003(3) 0.413(2) 0.0915(6) 0.022(1) Uani 1.00 d . . . C(22) C 0.2368(3) 0.288(2) 0.1732(7) 0.027(1) Uani 1.00 d . . . C(23) C 0.2803(3) 0.227(2) 0.1006(9) 0.043(2) Uani 1.00 d . . . H(1) H -0.0034 0.3410 0.3830 0.0288 Uiso 1.00 calc . . . H(2) H -0.0945 0.1986 0.3448 0.0339 Uiso 1.00 calc . . . H(3) H -0.1301 0.0476 0.1386 0.0313 Uiso 1.00 calc . . . H(4) H 0.1181 0.1414 0.3534 0.0281 Uiso 1.00 calc . . . H(5) H 0.2100 0.0732 0.5738 0.0328 Uiso 1.00 calc . . . H(6) H 0.2744 0.2367 0.7448 0.0343 Uiso 1.00 calc . . . H(7) H 0.2452 0.4652 0.7050 0.0358 Uiso 1.00 calc . . . H(8) H 0.0976 0.8022 0.4813 0.0364 Uiso 1.00 calc . . . H(9) H -0.0048 0.8863 0.3064 0.0366 Uiso 1.00 calc . . . H(10) H -0.0736 0.7489 0.1032 0.0339 Uiso 1.00 calc . . . H(11) H -0.0411 0.5303 0.0792 0.0280 Uiso 1.00 calc . . . H(12) H 0.1380 0.5653 0.1113 0.0280 Uiso 1.00 calc . . . H(13) H 0.1792 0.4957 0.2642 0.0280 Uiso 1.00 calc . . . H(14) H 0.1732 0.3917 -0.0108 0.0275 Uiso 1.00 calc . . . H(15) H 0.2333 0.4792 0.0925 0.0275 Uiso 1.00 calc . . . H(16) H 0.2040 0.2234 0.1722 0.0336 Uiso 1.00 calc . . . H(17) H 0.3028 0.1516 0.1513 0.0514 Uiso 1.00 calc . . . H(18) H 0.2522 0.2041 -0.0036 0.0514 Uiso 1.00 calc . . . H(19) H 0.3119 0.2946 0.0962 0.0514 Uiso 1.00 calc . . . H(20) H 0.2899 0.2501 0.4061 0.0433 Uiso 1.00 calc . . . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_12 _atom_site_aniso_U_13 _atom_site_aniso_U_23 Br(1) 0.0255(2) 0.0211(2) 0.0297(3) -0.0061(3) 0.0035(2) 0.0009(4) O(1) 0.024(2) 0.023(2) 0.027(3) 0.004(2) -0.004(2) -0.005(2) O(2) 0.013(1) 0.023(2) 0.016(2) 0.000(1) 0.005(1) -0.001(1) O(3) 0.027(2) 0.031(2) 0.031(2) 0.007(2) -0.003(2) 0.004(2) C(1) 0.017(2) 0.016(2) 0.021(2) 0.004(2) 0.004(2) 0.005(2) C(2) 0.009(2) 0.022(3) 0.017(2) -0.001(2) 0.000(2) 0.005(2) C(3) 0.020(2) 0.032(3) 0.015(3) 0.005(2) 0.005(2) 0.001(2) C(4) 0.023(2) 0.037(3) 0.026(3) 0.000(2) 0.012(2) 0.007(2) C(5) 0.016(2) 0.028(3) 0.031(3) -0.001(2) 0.007(2) 0.008(2) C(6) 0.018(2) 0.020(2) 0.025(2) 0.002(2) 0.002(2) 0.007(2) C(7) 0.014(2) 0.020(2) 0.015(2) -0.005(2) 0.002(2) -0.002(2) C(8) 0.018(2) 0.023(2) 0.016(2) 0.004(2) 0.004(2) -0.001(2) C(9) 0.021(2) 0.022(2) 0.022(3) 0.001(2) 0.008(2) 0.001(2) C(10) 0.021(2) 0.025(3) 0.030(3) 0.010(2) 0.007(2) 0.009(2) C(11) 0.021(3) 0.039(2) 0.015(3) 0.010(2) 0.001(2) 0.006(2) C(12) 0.022(2) 0.039(2) 0.019(3) 0.007(2) -0.004(2) -0.006(2) C(13) 0.016(2) 0.023(2) 0.018(3) 0.002(2) 0.003(2) -0.002(2) C(14) 0.022(2) 0.021(2) 0.026(3) 0.004(2) 0.004(2) -0.001(2) C(15) 0.032(3) 0.025(3) 0.027(3) 0.007(2) 0.005(2) -0.008(2) C(16) 0.034(3) 0.030(3) 0.029(3) 0.012(2) 0.011(2) -0.001(2) C(17) 0.019(3) 0.031(2) 0.028(3) 0.010(2) 0.005(2) 0.009(2) C(18) 0.019(2) 0.029(2) 0.016(3) 0.001(2) 0.003(2) 0.003(2) C(19) 0.017(2) 0.023(2) 0.018(2) 0.003(2) 0.005(2) 0.002(2) C(20) 0.017(2) 0.018(3) 0.021(2) 0.000(2) 0.003(2) 0.000(3) C(21) 0.019(2) 0.026(3) 0.022(3) 0.000(2) 0.009(2) 0.002(2) C(22) 0.024(3) 0.018(2) 0.032(3) -0.007(2) 0.005(2) 0.000(2) C(23) 0.044(4) 0.036(3) 0.066(5) 0.003(3) 0.039(4) -0.010(4) #----------------------------------------------------------------------------- _computing_data_collection '.' _computing_cell_refinement '.' _computing_data_reduction 'teXsan Ver. 1.11' _computing_structure_solution 'DIRDIF94 (PATTY)' _computing_structure_refinement 'teXsan Ver. 1.10' _computing_publication_material 'teXsan Ver. 1.11' _computing_molecular_graphics ? #----------------------------------------------------------------------------- _geom_special_details ; ? ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_1 _geom_bond_site_symmetry_2 _geom_bond_publ_flag Br(1) C(6) 1.895(6) . . yes O(1) C(13) 1.399(7) . . yes O(1) C(14) 1.376(7) . . yes O(2) C(7) 1.450(6) . . yes O(2) C(20) 1.432(7) . . yes O(3) C(22) 1.432(7) . . yes C(1) C(1) 1.50(1) . 2_555 yes C(1) C(2) 1.419(7) . . yes C(1) C(6) 1.413(7) . . yes C(2) C(3) 1.396(7) . . yes C(2) C(7) 1.557(7) . . yes C(3) C(4) 1.374(8) . . yes C(4) C(5) 1.385(9) . . yes C(5) C(6) 1.384(8) . . yes C(7) C(8) 1.530(7) . . yes C(7) C(19) 1.517(8) . . yes C(8) C(9) 1.394(8) . . yes C(8) C(13) 1.379(8) . . yes C(9) C(10) 1.383(8) . . yes C(10) C(11) 1.407(9) . . yes C(11) C(12) 1.365(9) . . yes C(12) C(13) 1.395(8) . . yes C(14) C(15) 1.404(8) . . yes C(14) C(19) 1.384(8) . . yes C(15) C(16) 1.363(8) . . yes C(16) C(17) 1.393(9) . . yes C(17) C(18) 1.376(8) . . yes C(18) C(19) 1.401(7) . . yes C(20) C(21) 1.515(8) . . yes C(21) C(22) 1.511(8) . . yes C(22) C(23) 1.505(9) . . yes #----------------------------------------------------------------------------- loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_2 _geom_angle_site_symmetry_3 _geom_angle_publ_flag C(13) O(1) C(14) 116.7(5) . . 0_555 yes C(7) O(2) C(20) 114.7(4) . . 0_555 yes C(1) C(1) C(2) 126.7(4) 2_555 . 0_555 yes C(1) C(1) C(6) 117.8(5) 2_555 . 0_555 yes C(2) C(1) C(6) 115.5(5) . . 0_555 yes C(1) C(2) C(3) 119.8(5) . . 0_555 yes C(1) C(2) C(7) 127.9(5) . . 0_555 yes C(3) C(2) C(7) 112.2(5) . . 0_555 yes C(2) C(3) C(4) 122.7(5) . . 0_555 yes C(3) C(4) C(5) 119.0(5) . . 0_555 yes C(4) C(5) C(6) 119.0(5) . . 0_555 yes Br(1) C(6) C(1) 120.2(4) . . 0_555 yes Br(1) C(6) C(5) 115.7(4) . . 0_555 yes C(1) C(6) C(5) 123.9(5) . . 0_555 yes O(2) C(7) C(2) 106.2(4) . . 0_555 yes O(2) C(7) C(8) 109.3(4) . . 0_555 yes O(2) C(7) C(19) 111.1(4) . . 0_555 yes C(2) C(7) C(8) 110.3(4) . . 0_555 yes C(2) C(7) C(19) 110.1(4) . . 0_555 yes C(8) C(7) C(19) 109.7(4) . . 0_555 yes C(7) C(8) C(9) 121.7(5) . . 0_555 yes C(7) C(8) C(13) 120.5(5) . . 0_555 yes C(9) C(8) C(13) 117.5(5) . . 0_555 yes C(8) C(9) C(10) 122.0(5) . . 0_555 yes C(9) C(10) C(11) 118.9(5) . . 0_555 yes C(10) C(11) C(12) 119.9(5) . . 0_555 yes C(11) C(12) C(13) 120.0(5) . . 0_555 yes O(1) C(13) C(8) 123.2(6) . . 0_555 yes O(1) C(13) C(12) 115.1(5) . . 0_555 yes C(8) C(13) C(12) 121.7(6) . . 0_555 yes O(1) C(14) C(15) 114.4(5) . . 0_555 yes O(1) C(14) C(19) 123.8(5) . . 0_555 yes C(15) C(14) C(19) 121.8(5) . . 0_555 yes C(14) C(15) C(16) 119.2(6) . . 0_555 yes C(15) C(16) C(17) 120.0(5) . . 0_555 yes C(16) C(17) C(18) 120.7(5) . . 0_555 yes C(17) C(18) C(19) 120.4(5) . . 0_555 yes C(7) C(19) C(14) 120.6(5) . . 0_555 yes C(7) C(19) C(18) 121.5(5) . . 0_555 yes C(14) C(19) C(18) 117.9(5) . . 0_555 yes O(2) C(20) C(21) 107.5(5) . . 0_555 yes C(20) C(21) C(22) 114.1(5) . . 0_555 yes O(3) C(22) C(21) 106.6(4) . . 0_555 yes O(3) C(22) C(23) 110.5(5) . . 0_555 yes C(21) C(22) C(23) 112.1(5) . . 0_555 yes #----------------------------------------------------------------------------- loop_ _geom_torsion_atom_site_label_1 _geom_torsion_atom_site_label_2 _geom_torsion_atom_site_label_3 _geom_torsion_atom_site_label_4 _geom_torsion _geom_torsion_site_symmetry_1 _geom_torsion_site_symmetry_2 _geom_torsion_site_symmetry_3 _geom_torsion_site_symmetry_4 _geom_torsion_publ_flag Br(1) C(6) C(1) C(1) 6.0(6) 0_555 12_1 5_555 55_5 yes Br(1) C(6) C(1) C(2) -172.7(4) 0_555 12_1 5_555 55_5 yes Br(1) C(6) C(5) C(4) 177.0(4) 0_555 12_1 5_555 55_5 yes O(1) C(13) C(8) C(7) 6.8(10) 0_555 12_1 5_555 55_5 yes O(1) C(13) C(8) C(9) -179.5(6) 0_555 12_1 5_555 55_5 yes O(1) C(13) C(12) C(11) 179.6(6) 0_555 12_1 5_555 55_5 yes O(1) C(14) C(15) C(16) -179.7(6) 0_555 12_1 5_555 55_5 yes O(1) C(14) C(19) C(7) -1.9(9) 0_555 12_1 5_555 55_5 yes O(1) C(14) C(19) C(18) 179.0(6) 0_555 12_1 5_555 55_5 yes O(2) C(7) C(2) C(1) 1.5(7) 0_555 12_1 5_555 55_5 yes O(2) C(7) C(2) C(3) 179.2(4) 0_555 12_1 5_555 55_5 yes O(2) C(7) C(8) C(9) -73.8(6) 0_555 12_1 5_555 55_5 yes O(2) C(7) C(8) C(13) 99.7(6) 0_555 12_1 5_555 55_5 yes O(2) C(7) C(19) C(14) -100.9(6) 0_555 12_1 5_555 55_5 yes O(2) C(7) C(19) C(18) 78.1(6) 0_555 12_1 5_555 55_5 yes O(2) C(20) C(21) C(22) -68.2(5) 0_555 12_1 5_555 55_5 yes O(3) C(22) C(21) C(20) -60.0(6) 0_555 12_1 5_555 55_5 yes C(1) C(1) C(2) C(3) 177.1(5) 0_555 12_1 5_555 55_5 yes C(1) C(1) C(2) C(7) -5.4(8) 0_555 12_1 5_555 55_5 yes C(1) C(1) C(6) C(5) -177.8(5) 0_555 12_1 5_555 55_5 yes C(1) C(2) C(3) C(4) 1.3(8) 0_555 12_1 5_555 55_5 yes C(1) C(2) C(7) C(8) -116.9(6) 0_555 12_1 5_555 55_5 yes C(1) C(2) C(7) C(19) 121.9(5) 0_555 12_1 5_555 55_5 yes C(1) C(6) C(5) C(4) 0.7(8) 0_555 12_1 5_555 55_5 yes C(2) C(1) C(1) C(2) -89.8(9) 0_555 12_1 5_555 55_5 yes C(2) C(1) C(1) C(6) 91.6(3) 0_555 12_1 5_555 55_5 yes C(2) C(1) C(6) C(5) 3.4(7) 0_555 12_1 5_555 55_5 yes C(2) C(3) C(4) C(5) 3.0(9) 0_555 12_1 5_555 55_5 yes C(2) C(7) O(2) C(20) 176.7(4) 0_555 12_1 5_555 55_5 yes C(2) C(7) C(8) C(9) 42.7(7) 0_555 12_1 5_555 55_5 yes C(2) C(7) C(8) C(13) -143.8(5) 0_555 12_1 5_555 55_5 yes C(2) C(7) C(19) C(14) 141.7(5) 0_555 12_1 5_555 55_5 yes C(2) C(7) C(19) C(18) -39.3(7) 0_555 12_1 5_555 55_5 yes C(3) C(2) C(1) C(6) -4.3(7) 0_555 12_1 5_555 55_5 yes C(3) C(2) C(7) C(8) 60.8(6) 0_555 12_1 5_555 55_5 yes C(3) C(2) C(7) C(19) -60.5(6) 0_555 12_1 5_555 55_5 yes C(3) C(4) C(5) C(6) -3.9(8) 0_555 12_1 5_555 55_5 yes C(4) C(3) C(2) C(7) -176.6(5) 0_555 12_1 5_555 55_5 yes C(6) C(1) C(1) C(6) -87.0(8) 0_555 12_1 5_555 55_5 yes C(6) C(1) C(2) C(7) 173.2(5) 0_555 12_1 5_555 55_5 yes C(7) O(2) C(20) C(21) 149.6(4) 0_555 12_1 5_555 55_5 yes C(7) C(8) C(9) C(10) 171.8(5) 0_555 12_1 5_555 55_5 yes C(7) C(8) C(13) C(12) -170.1(5) 0_555 12_1 5_555 55_5 yes C(7) C(19) C(14) C(15) 179.3(5) 0_555 12_1 5_555 55_5 yes C(7) C(19) C(18) C(17) -178.4(5) 0_555 12_1 5_555 55_5 yes C(8) C(7) O(2) C(20) -64.2(6) 0_555 12_1 5_555 55_5 yes C(8) C(7) C(19) C(14) 20.1(6) 0_555 12_1 5_555 55_5 yes C(8) C(7) C(19) C(18) -160.9(5) 0_555 12_1 5_555 55_5 yes C(8) C(9) C(10) C(11) -0.3(8) 0_555 12_1 5_555 55_5 yes C(8) C(13) O(1) C(14) 13.5(10) 0_555 12_1 5_555 55_5 yes C(8) C(13) C(12) C(11) -3.3(10) 0_555 12_1 5_555 55_5 yes C(9) C(8) C(7) C(19) 164.2(5) 0_555 12_1 5_555 55_5 yes C(9) C(8) C(13) C(12) 3.7(9) 0_555 12_1 5_555 55_5 yes C(9) C(10) C(11) C(12) 0.8(9) 0_555 12_1 5_555 55_5 yes C(10) C(9) C(8) C(13) -1.9(9) 0_555 12_1 5_555 55_5 yes C(10) C(11) C(12) C(13) 1.0(9) 0_555 12_1 5_555 55_5 yes C(12) C(13) O(1) C(14) -169.5(5) 0_555 12_1 5_555 55_5 yes C(13) O(1) C(14) C(15) 162.9(6) 0_555 12_1 5_555 55_5 yes C(13) O(1) C(14) C(19) -16.0(10) 0_555 12_1 5_555 55_5 yes C(13) C(8) C(7) C(19) -22.3(7) 0_555 12_1 5_555 55_5 yes C(14) C(15) C(16) C(17) 0.5(10) 0_555 12_1 5_555 55_5 yes C(14) C(19) C(18) C(17) 0.6(8) 0_555 12_1 5_555 55_5 yes C(15) C(14) C(19) C(18) 0.2(9) 0_555 12_1 5_555 55_5 yes C(15) C(16) C(17) C(18) 0.3(9) 0_555 12_1 5_555 55_5 yes C(16) C(15) C(14) C(19) -0.8(10) 0_555 12_1 5_555 55_5 yes C(16) C(17) C(18) C(19) -0.9(9) 0_555 12_1 5_555 55_5 yes C(19) C(7) O(2) C(20) 57.0(5) 0_555 12_1 5_555 55_5 yes C(20) C(21) C(22) C(23) 179.0(5) 0_555 12_1 5_555 55_5 yes C(20) C(21) C(22) C(23) 179.0(5) 0_555 12_1 5_555 55_5 yes #----------------------------------------------------------------------------- loop_ _geom_contact_atom_site_label_1 _geom_contact_atom_site_label_2 _geom_contact_distance _geom_contact_site_symmetry_1 _geom_contact_site_symmetry_2 _geom_contact_publ_flag O(1) O(3) 3.124(6) . 4_556 ? O(3) C(15) 3.436(7) . 4_546 ? O(3) C(10) 3.504(7) . 4_556 ? #-----------------------------------------------------------------------------