Supplementary Material (ESI) for Perkin Transactions This journal is © The Royal Society of Chemistry 2001 data_global _journal_coden_Cambridge 207 _audit_creation_method Xtal3.6 _audit_creation_date 00-09-07 _audit_update_record ? #============================================================================== # 1. SUBMISSION DETAILS #---------------------- _publ_contact_author_name 'Prof J H Bowie' _publ_contact_author_address ; Prof J H Bowie Department of Organic Chemistry University of Adelaide South Australia 5001 AUSTRALIA ; _publ_contact_author_email bws@crystal.uwa.edu.au _publ_contact_author_fax (+61)_08_9380_1118 _publ_contact_author_phone (+61)_08-9380_3481 _publ_contact_letter ; ? #<< contact letter ; _publ_requested_journal 'Perkin Transactions 1' _publ_requested_category ? _publ_section_title ; ? #<< paper title text ; _publ_section_title_footnote ; ? #<< paper footnote text ; loop_ _publ_author_name 'Bowie, J. H.' 'Pyke, Simon M.' 'Rozek, Thomas' 'Skelton, Brian W.' 'White, Allan H.' _publ_section_synopsis ; ? #<< synopsis if FI,CI,CM,CO papers ; _publ_section_abstract ; ? #<< abstract text ; _publ_section_comment ; ? #<< scientific commentary text ; _publ_section_exptl_prep ; ? #<< material & crystal preparation text ; _publ_section_exptl_refinement ; ? #<< crystallographic methods used ; _publ_section_acknowledgements ; ? #<< acknowledgements text ; _publ_section_references ; Sheldrick, G M. (1996). SADABS. Pogram for Empirical Absorption Correction of Area Detector Data. University of Gottingen, Germany. Siemens (1995). SMART and SAINT. Area-Detector Control and Integration Software. Siemens Analytical X-ray Systems Inc., Madison, Wisconsin, USA. Hall, S.R., King, G.S.D., and Stewart., J.M. (1995). The Xtal 3.5 User's Manual. University of Western Australia, Lamb: Perth. ; _publ_section_figure_captions ; ? #<< figure captions ; #======================================================================= # Data block for single structure (one for each study in the paper) #======================================================================= data_jbtr1 _database_code_CSD 159020 # 2. EXPERIMENTAL DATA #--------------------- _chemical_formula_sum 'C24 H23 Br1 O6' _chemical_formula_moiety ? _chemical_formula_weight 487.35 _chemical_melting_point ? _symmetry_cell_setting monoclinic _symmetry_space_group_name_H-M P_1_21/c_1 _symmetry_space_group_name_Hall -p_2ybc 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 8.8741(4) _cell_length_b 20.1040(10) _cell_length_c 12.2989(6) _cell_angle_alpha 90.00000 _cell_angle_beta 101.6370(10) _cell_angle_gamma 90.00000 _cell_volume 2149.08(18) _cell_formula_units_Z 4 _exptl_crystal_density_diffrn 1.506 _exptl_crystal_density_meas ? _exptl_crystal_density_method ? _diffrn_radiation_type 'Mo K\a' _diffrn_radiation_wavelength .71073 _cell_measurement_reflns_used 8192 _cell_measurement_theta_min 3.2 _cell_measurement_theta_max 24.6 _cell_measurement_temperature 153 _exptl_absorpt_coefficient_mu 1.952 _exptl_crystal_description prism _exptl_crystal_size_max .3 _exptl_crystal_size_mid .25 _exptl_crystal_size_min .2 _exptl_crystal_size_rad ? _exptl_crystal_colour colourless _diffrn_measurement_device_type ; Bruker SMART CCD diffractometer ; _diffrn_measurement_method '\w scans' _diffrn_detector_area_resol_mean ? _exptl_absorpt_correction_type multi-scan _exptl_absorpt_process_details ; SADABS; Sheldrick, 1996 ; _exptl_absorpt_correction_T_min .71 _exptl_absorpt_correction_T_max .80 _diffrn_reflns_number 40562 _reflns_number_total 10667 _reflns_Friedel_coverage 0 _reflns_number_gt 6875 _reflns_threshold_expression 'F > 4.00 sig(F )' _diffrn_reflns_theta_max 37.16 _diffrn_reflns_theta_full ? _diffrn_measured_fraction_theta_max ? _diffrn_measured_fraction_theta_full ? _diffrn_reflns_av_R_equivalents .036 _diffrn_reflns_limit_h_min -15 _diffrn_reflns_limit_h_max 14 _diffrn_reflns_limit_k_min 0 _diffrn_reflns_limit_k_max 34 _diffrn_reflns_limit_l_min 0 _diffrn_reflns_limit_l_max 20 _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% 0 _refine_ls_structure_factor_coef F _refine_ls_R_factor_gt .03 _refine_ls_wR_factor_ref .028 _refine_ls_goodness_of_fit_ref 1.02 _refine_ls_number_reflns 6875 _refine_ls_number_parameters 372 _refine_ls_weighting_scheme calc _refine_ls_weighting_details ? _refine_ls_hydrogen_treatment refall _refine_ls_shift/su_max .077 _refine_diff_density_min -.629 _refine_diff_density_max .688 _refine_ls_extinction_method ? _refine_ls_extinction_coef ? _refine_ls_abs_structure_details ? _refine_ls_abs_structure_Flack ? # 3. Information for the "methods" section #----------------------------------------- _computing_data_collection 'Siemens SMART (Siemens, 1995)' _computing_cell_refinement 'Siemens SAINT (Siemens, 1995)' _computing_data_reduction 'xtal ADDREF SORTRF' _computing_structure_solution xtal _computing_structure_refinement 'xtal CRYLSQ' _computing_molecular_graphics xtal _computing_publication_material 'xtal BONDLA CIFIO' # 4. Supplementary data for validation and tables #------------------------------------------------ loop_ _atom_type_symbol _atom_type_description _atom_type_oxidation_number _atom_type_number_in_cell _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source C ? 0 96 .002 .002 'Int Tables Vol IV Tables 2.2B and 2.3.1' H ? 0 92 0 0 'Int Tables Vol IV Tables 2.2B and 2.3.1' Br ? 0 4 -.374 2.456 'Int Tables Vol IV Tables 2.2B and 2.3.1' O ? 0 24 .008 .006 'Int Tables Vol IV Tables 2.2B and 2.3.1' loop_ _atom_site_label _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_calc_flag _atom_site_calc_attached_atom _atom_site_occupancy _atom_site_disorder_assembly _atom_site_disorder_group C1 .07430(14) .90493(6) .19172(10) .0165(5) Uani ? ? 1.00000 ? ? O111 .17721(10) .94013(4) .13924(7) .0189(4) Uani ? ? 1.00000 ? ? C111 .14239(15) .94445(6) .02656(11) .0192(5) Uani ? ? 1.00000 ? ? O112 .02627(11) .92220(5) -.02944(8) .0240(4) Uani ? ? 1.00000 ? ? C112 .2670(2) .97986(9) -.01568(14) .0273(7) Uani ? ? 1.00000 ? ? C2 -.00600(15) .93956(7) .25178(11) .0206(5) Uani ? ? 1.00000 ? ? C3 -.11354(15) .90874(7) .31841(11) .0225(6) Uani ? ? 1.00000 ? ? C31 -.0281(2) .89794(9) .43887(12) .0294(7) Uani ? ? 1.00000 ? ? C32 -.2533(2) .95342(9) .31765(15) .0326(8) Uani ? ? 1.00000 ? ? C4 -.16736(15) .84209(7) .26308(12) .0226(6) Uani ? ? 1.00000 ? ? C4a -.03553(14) .79909(6) .24588(10) .0184(5) Uani ? ? 1.00000 ? ? C5 -.01547(15) .73813(7) .28759(11) .0217(6) Uani ? ? 1.00000 ? ? C6 .10875(15) .69142(7) .27205(12) .0226(6) Uani ? ? 1.00000 ? ? C6a .19852(14) .71757(6) .18612(10) .0171(5) Uani ? ? 1.00000 ? ? C7 .34805(14) .67919(6) .19886(10) .0187(5) Uani ? ? 1.00000 ? ? O7 .36122(12) .63350(5) .13715(8) .0292(5) Uani ? ? 1.00000 ? ? C7a .47022(14) .69850(6) .29638(10) .0156(5) Uani ? ? 1.00000 ? ? C8 .59173(14) .65594(6) .34122(10) .0164(5) Uani ? ? 1.00000 ? ? C81 .65971(14) .59114(7) .19892(11) .0202(6) Uani ? ? 1.00000 ? ? O81 .60193(10) .59310(4) .29498(7) .0197(4) Uani ? ? 1.00000 ? ? O82 .72230(12) .63791(5) .16780(8) .0291(5) Uani ? ? 1.00000 ? ? C82 .6312(2) .52510(8) .14388(13) .0275(7) Uani ? ? 1.00000 ? ? C9 .69844(15) .67253(7) .43600(10) .0190(5) Uani ? ? 1.00000 ? ? C10 .68670(15) .73342(7) .48766(10) .0192(5) Uani ? ? 1.00000 ? ? C11 .56866(14) .77689(6) .44475(10) .0166(5) Uani ? ? 1.00000 ? ? C11a .46071(13) .75995(6) .35045(10) .0148(5) Uani ? ? 1.00000 ? ? C12 .33474(13) .80900(6) .30929(9) .0154(5) Uani ? ? 1.00000 ? ? O12 .32197(11) .85978(5) .35955(8) .0252(4) Uani ? ? 1.00000 ? ? C12a .22567(14) .79259(6) .19983(9) .0148(5) Uani ? ? 1.00000 ? ? C12b .07071(14) .83006(6) .17639(10) .0154(5) Uani ? ? 1.00000 ? ? Br .354734(15) .815313(7) .089180(11) .02220(6) Uani ? ? 1.00000 ? ? H2 .0063(17) .9886(7) .2520(12) .020(4) Uiso ? ? 1.00000 ? ? H31A -.098(2) .8789(8) .4829(14) .035(5) Uiso ? ? 1.00000 ? ? H31B .060(2) .8683(8) .4410(14) .033(5) Uiso ? ? 1.00000 ? ? H31C .005(2) .9391(10) .4685(15) .046(5) Uiso ? ? 1.00000 ? ? H32A -.325(2) .9322(9) .3562(16) .048(5) Uiso ? ? 1.00000 ? ? H32B -.224(2) .9948(9) .3446(15) .041(5) Uiso ? ? 1.00000 ? ? H32C -.312(2) .9605(9) .2483(17) .047(5) Uiso ? ? 1.00000 ? ? H4A -.2294(19) .8184(7) .3066(13) .025(4) Uiso ? ? 1.00000 ? ? H4B -.234(2) .8512(8) .1914(15) .034(4) Uiso ? ? 1.00000 ? ? H5 -.089(2) .7225(8) .3285(14) .035(5) Uiso ? ? 1.00000 ? ? H6A .1785(18) .6844(7) .3428(13) .024(4) Uiso ? ? 1.00000 ? ? H6B .0673(18) .6479(8) .2476(13) .032(4) Uiso ? ? 1.00000 ? ? H6a .1412(17) .7098(7) .1172(12) .019(4) Uiso ? ? 1.00000 ? ? H82A .699(2) .5183(9) .0928(16) .050(6) Uiso ? ? 1.00000 ? ? H82B .637(2) .4900(9) .1947(16) .048(5) Uiso ? ? 1.00000 ? ? H82C .532(2) .5251(9) .1043(15) .043(5) Uiso ? ? 1.00000 ? ? H9 .7739(16) .6402(7) .4641(12) .018(4) Uiso ? ? 1.00000 ? ? H10 .7591(17) .7457(7) .5505(12) .022(4) Uiso ? ? 1.00000 ? ? H11 .5605(17) .8193(7) .4798(12) .020(4) Uiso ? ? 1.00000 ? ? H12b .0280(17) .8215(7) .0995(12) .018(4) Uiso ? ? 1.00000 ? ? H112A .225(3) 1.0165(13) -.047(2) .088(8) Uiso ? ? 1.00000 ? ? H112B .349(2) .9897(10) .0365(18) .055(6) Uiso ? ? 1.00000 ? ? H112C .292(3) .9536(12) -.071(2) .070(7) Uiso ? ? 1.00000 ? ? 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 C1 .0144(5) .0201(6) .0147(5) .0007(5) .0021(4) .0023(5) O111 .0183(4) .0216(5) .0172(4) -.0015(4) .0045(3) .0014(4) C111 .0217(6) .0173(6) .0194(6) .0032(5) .0060(5) .0028(5) O112 .0245(5) .0268(5) .0198(5) -.0004(4) .0020(4) .0031(4) C112 .0281(8) .0287(8) .0274(8) -.0018(6) .0110(6) .0063(6) C2 .0205(6) .0221(6) .0189(6) .0038(5) .0036(5) .0006(5) C3 .0234(6) .0270(7) .0188(6) .0063(5) .0085(5) .0010(5) C31 .0359(8) .0341(8) .0194(7) .0049(7) .0085(6) -.0022(6) C32 .0309(8) .0372(9) .0337(9) .0128(7) .0164(7) .0037(7) C4 .0161(6) .0315(7) .0219(6) .0015(5) .0077(5) .0010(6) C4a .0145(5) .0239(6) .0170(6) -.0022(5) .0038(4) -.0016(5) C5 .0179(6) .0250(7) .0230(6) -.0049(5) .0060(5) .0002(5) C6 .0192(6) .0189(7) .0289(7) -.0040(5) .0035(5) .0012(5) C6a .0152(5) .0186(6) .0156(6) .0003(5) -.0013(4) -.0034(5) C7 .0191(5) .0189(6) .0168(5) .0001(5) .0007(4) -.0004(5) O7 .0283(5) .0280(5) .0274(5) .0077(4) -.0036(4) -.0121(4) C7a .0157(5) .0177(6) .0134(5) -.0001(4) .0030(4) .0005(4) C8 .0173(5) .0162(6) .0157(5) -.0001(5) .0034(4) .0025(4) C81 .0174(6) .0230(6) .0188(6) .0047(5) .0007(5) .0005(5) O81 .0235(5) .0164(4) .0196(4) .0032(4) .0052(4) .0016(3) O82 .0343(6) .0292(5) .0264(5) -.0060(4) .0122(4) -.0020(4) C82 .0297(8) .0245(7) .0266(7) .0034(6) .0020(6) -.0047(6) C9 .0152(5) .0233(7) .0178(6) .0021(5) .0019(4) .0062(5) C10 .0157(6) .0258(7) .0148(6) -.0023(5) .0003(5) .0022(5) C11 .0164(5) .0201(6) .0134(5) -.0022(5) .0034(4) .0001(4) C11a .0137(5) .0176(6) .0135(5) -.0003(4) .0035(4) .0015(4) C12 .0148(5) .0175(6) .0137(5) -.0007(4) .0024(4) .0005(4) O12 .0267(5) .0229(5) .0225(5) .0056(4) -.0031(4) -.0074(4) C12a .0144(5) .0189(5) .0115(5) .0007(4) .0032(4) -.0003(4) C12b .0137(5) .0198(6) .0124(5) .0009(4) .0018(4) -.0001(4) Br .02195(6) .02968(7) .01763(6) .00794(6) .01031(4) .00564(6) # 5. Molecular Geometry #---------------------- loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_site_symmetry_1 _geom_bond_site_symmetry_2 _geom_bond_distance _geom_bond_publ_flag #<< enter YES for value to be published C1 O111 . . 1.4104(16) ? C1 C2 . . 1.323(2) ? C1 C12b . . 1.5166(17) ? O111 C111 . . 1.3605(15) ? C111 O112 . . 1.2041(15) ? C111 C112 . . 1.494(2) ? C112 H112A . . .88(3) ? C112 H112B . . .89(2) ? C112 H112C . . .92(2) ? C2 C3 . . 1.510(2) ? C2 H2 . . .991(15) ? C3 C31 . . 1.5375(19) ? C3 C32 . . 1.530(2) ? C3 C4 . . 1.535(2) ? C31 H31A . . .978(19) ? C31 H31B . . .978(18) ? C31 H31C . . .928(19) ? C32 H32A . . .97(2) ? C32 H32B . . .914(19) ? C32 H32C . . .92(2) ? C4 C4a . . 1.504(2) ? C4 H4A . . .967(17) ? C4 H4B . . .975(16) ? C4a C5 . . 1.3266(19) ? C4a C12b . . 1.5271(19) ? C5 C6 . . 1.490(2) ? C5 H5 . . .951(18) ? C6 C6a . . 1.539(2) ? C6 H6A . . .971(15) ? C6 H6B . . .974(17) ? C6a C7 . . 1.5155(18) ? C6a C12a . . 1.5313(18) ? C6a H6a . . .910(14) ? C7 O7 . . 1.2122(17) ? C7 C7a . . 1.4967(16) ? C7a C8 . . 1.3996(16) ? C7a C11a . . 1.4136(17) ? C8 O81 . . 1.3959(15) ? C8 C9 . . 1.3862(16) ? C81 O81 . . 1.3800(17) ? C81 O82 . . 1.1937(17) ? C81 C82 . . 1.489(2) ? C82 H82A . . .96(2) ? C82 H82B . . .94(2) ? C82 H82C . . .918(18) ? C9 C10 . . 1.393(2) ? C9 H9 . . .947(14) ? C10 C11 . . 1.3845(17) ? C10 H10 . . .933(14) ? C11 C11a . . 1.3895(15) ? C11 H11 . . .964(15) ? C11a C12 . . 1.4999(16) ? C12 O12 . . 1.2107(16) ? C12 C12a . . 1.5272(15) ? C12a C12b . . 1.5433(17) ? C12a Br . . 2.0002(13) ? C12b H12b . . .960(14) ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_2 _geom_angle_site_symmetry_3 _geom_angle _geom_angle_publ_flag #<< enter YES for value to be published O111 C1 C2 . . . 117.58(11) ? O111 C1 C12b . . . 116.13(11) ? C2 C1 C12b . . . 126.26(12) ? C1 O111 C111 . . . 117.59(9) ? O111 C111 O112 . . . 123.46(13) ? O111 C111 C112 . . . 110.66(11) ? O112 C111 C112 . . . 125.88(13) ? C111 C112 H112A . . . 105.7(18) ? C111 C112 H112B . . . 114.2(15) ? C111 C112 H112C . . . 106.7(15) ? H112A C112 H112B . . . 110(2) ? H112A C112 H112C . . . 107(2) ? H112B C112 H112C . . . 112(2) ? C1 C2 C3 . . . 123.89(13) ? C1 C2 H2 . . . 117.0(9) ? C3 C2 H2 . . . 119.2(9) ? C2 C3 C31 . . . 109.74(11) ? C2 C3 C32 . . . 110.86(12) ? C2 C3 C4 . . . 106.96(12) ? C31 C3 C32 . . . 109.31(13) ? C31 C3 C4 . . . 110.66(12) ? C32 C3 C4 . . . 109.30(11) ? C3 C31 H31A . . . 110.2(9) ? C3 C31 H31B . . . 110.4(10) ? C3 C31 H31C . . . 107.8(11) ? H31A C31 H31B . . . 109.6(14) ? H31A C31 H31C . . . 108.4(16) ? H31B C31 H31C . . . 110.4(15) ? C3 C32 H32A . . . 110.6(11) ? C3 C32 H32B . . . 110.9(12) ? C3 C32 H32C . . . 113.8(13) ? H32A C32 H32B . . . 113.2(17) ? H32A C32 H32C . . . 102.7(17) ? H32B C32 H32C . . . 105.3(16) ? C3 C4 C4a . . . 112.52(11) ? C3 C4 H4A . . . 110.3(9) ? C3 C4 H4B . . . 108.4(10) ? C4a C4 H4A . . . 109.9(9) ? C4a C4 H4B . . . 109.2(11) ? H4A C4 H4B . . . 106.4(14) ? C4 C4a C5 . . . 121.62(13) ? C4 C4a C12b . . . 115.47(11) ? C5 C4a C12b . . . 122.91(12) ? C4a C5 C6 . . . 125.30(14) ? C4a C5 H5 . . . 117.2(10) ? C6 C5 H5 . . . 117.5(10) ? C5 C6 C6a . . . 111.83(11) ? C5 C6 H6A . . . 109.3(10) ? C5 C6 H6B . . . 111.3(10) ? C6a C6 H6A . . . 109.9(10) ? C6a C6 H6B . . . 108.1(10) ? H6A C6 H6B . . . 106.2(12) ? C6 C6a C7 . . . 108.59(10) ? C6 C6a C12a . . . 110.66(11) ? C6 C6a H6a . . . 108.1(10) ? C7 C6a C12a . . . 112.02(10) ? C7 C6a H6a . . . 108.8(10) ? C12a C6a H6a . . . 108.5(9) ? C6a C7 O7 . . . 120.93(11) ? C6a C7 C7a . . . 115.37(11) ? O7 C7 C7a . . . 123.54(11) ? C7 C7a C8 . . . 122.22(11) ? C7 C7a C11a . . . 120.08(10) ? C8 C7a C11a . . . 117.60(10) ? C7a C8 O81 . . . 120.06(10) ? C7a C8 C9 . . . 121.71(11) ? O81 C8 C9 . . . 118.09(10) ? O81 C81 O82 . . . 121.95(12) ? O81 C81 C82 . . . 110.89(12) ? O82 C81 C82 . . . 127.16(14) ? C8 O81 C81 . . . 116.13(10) ? C81 C82 H82A . . . 110.6(11) ? C81 C82 H82B . . . 112.8(12) ? C81 C82 H82C . . . 107.3(11) ? H82A C82 H82B . . . 111.8(17) ? H82A C82 H82C . . . 108.4(17) ? H82B C82 H82C . . . 105.6(16) ? C8 C9 C10 . . . 119.59(11) ? C8 C9 H9 . . . 117.1(8) ? C10 C9 H9 . . . 123.3(8) ? C9 C10 C11 . . . 120.10(11) ? C9 C10 H10 . . . 120.6(9) ? C11 C10 H10 . . . 119.3(9) ? C10 C11 C11a . . . 120.31(12) ? C10 C11 H11 . . . 120.4(8) ? C11a C11 H11 . . . 119.3(8) ? C7a C11a C11 . . . 120.69(11) ? C7a C11a C12 . . . 121.80(10) ? C11 C11a C12 . . . 117.52(11) ? C11a C12 O12 . . . 121.48(10) ? C11a C12 C12a . . . 116.88(10) ? O12 C12 C12a . . . 121.62(10) ? C6a C12a C12 . . . 111.56(9) ? C6a C12a C12b . . . 110.22(10) ? C6a C12a Br . . . 104.42(8) ? C12 C12a C12b . . . 116.21(10) ? C12 C12a Br . . . 101.68(8) ? C12b C12a Br . . . 111.86(8) ? C1 C12b C4a . . . 109.57(11) ? C1 C12b C12a . . . 117.75(10) ? C1 C12b H12b . . . 107.1(8) ? C4a C12b C12a . . . 108.90(10) ? C4a C12b H12b . . . 108.2(9) ? C12a C12b H12b . . . 104.8(9) ? 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_site_symmetry_1 _geom_torsion_site_symmetry_2 _geom_torsion_site_symmetry_3 _geom_torsion_site_symmetry_4 _geom_torsion _geom_torsion_publ_flag #<< enter YES for value to be published ? ? ? ? ? ? ? ? ? ? loop_ _geom_hbond_atom_site_label_D _geom_hbond_atom_site_label_H _geom_hbond_atom_site_label_A _geom_hbond_site_symmetry_D _geom_hbond_site_symmetry_H _geom_hbond_site_symmetry_A _geom_hbond_distance_DH _geom_hbond_distance_HA _geom_hbond_distance_DA _geom_hbond_angle_DHA _geom_hbond_publ_flag #<< enter YES for value to be published ? ? ? ? ? ? ? ? ? ? ? #-------------------------------------------------------------------------- # Special items requested by author for inclusion in paper #-------------------------------------------------------------------------- loop_ _publ_manuscript_incl_extra_item _publ_manuscript_incl_extra_defn ? ? #-------------------------------------------------------------------------- # Items which are non-mandatory for Acta C submissions #-------------------------------------------------------------------------- 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 C1 C111 2.3702(19) . . ? C1 O112 2.6895(15) . . ? C1 C3 2.502(2) . . ? C1 C4 2.779(2) . . ? C1 C4a 2.4866(18) . . ? C1 O12 2.8434(14) . . ? C1 C12a 2.6194(18) . . ? C1 Br 3.5066(13) . . ? C1 H2 1.980(15) . . ? C1 H12b 2.020(14) . . ? O111 O112 2.2599(12) . . ? O111 C112 2.348(2) . . ? O111 C2 2.3382(18) . . ? O111 C12b 2.4846(15) . . ? O111 Br 3.0902(9) . . ? O111 H2 2.454(16) . . ? O111 H82B 2.557(18) . '2 655' ? O111 H112B 2.39(2) . . ? C111 Br 3.2091(13) . . ? C111 H112A 1.93(3) . . ? C111 H112B 2.03(2) . . ? C111 H112C 1.97(3) . . ? O112 C112 2.406(2) . . ? O112 Br 3.6779(9) . . ? O112 H9 2.554(15) . '4 464' ? O112 H12b 2.569(14) . . ? O112 H112A 2.63(3) . . ? O112 H112C 2.59(2) . . ? C112 Br 3.5788(17) . . ? C2 C31 2.493(2) . . ? C2 C32 2.504(2) . . ? C2 C4 2.447(2) . . ? C2 C4a 2.836(2) . . ? C2 C12b 2.5345(19) . . ? C2 H31B 2.695(16) . . ? C2 H31C 2.65(2) . . ? C2 H32B 2.67(2) . . ? C2 H4B 2.684(17) . . ? C3 C4a 2.527(2) . . ? C3 H2 2.173(16) . . ? C3 H31A 2.088(17) . . ? C3 H31B 2.090(16) . . ? C3 H31C 2.024(18) . . ? C3 H32A 2.08(2) . . ? C3 H32B 2.04(2) . . ? C3 H32C 2.076(18) . . ? C3 H4A 2.078(15) . . ? C3 H4B 2.062(16) . . ? C31 C32 2.502(2) . . ? C31 C4 2.527(2) . . ? C31 H4A 2.688(15) . . ? C32 C4 2.500(2) . . ? C32 H2 2.685(16) . . ? C32 H31A 2.675(16) . . ? C32 H31C 2.655(17) . . ? C32 H4B 2.603(18) . . ? C4 C5 2.472(2) . . ? C4 C12b 2.563(2) . . ? C4 H32A 2.68(2) . . ? C4 H32C 2.693(18) . . ? C4 H5 2.586(16) . . ? C4a C6 2.5024(19) . . ? C4a C6a 2.8558(19) . . ? C4a C12a 2.4981(18) . . ? C4a H4A 2.046(18) . . ? C4a H4B 2.043(17) . . ? C4a H5 1.954(17) . . ? C4a H12b 2.043(16) . . ? C5 C6a 2.508(2) . . ? C5 C12a 2.806(2) . . ? C5 C12b 2.509(2) . . ? C5 H4A 2.538(16) . . ? C5 H6A 2.030(15) . . ? C5 H6B 2.055(17) . . ? C6 C7 2.480(2) . . ? C6 C12a 2.525(2) . . ? C6 H5 2.105(18) . . ? C6 H6a 2.017(16) . . ? C6a O7 2.3780(17) . . ? C6a C7a 2.5457(16) . . ? C6a C11a 2.8856(16) . . ? C6a C12 2.5289(17) . . ? C6a C12b 2.5220(18) . . ? C6a Br 2.8056(13) . . ? C6a H6A 2.080(17) . . ? C6a H6B 2.061(17) . . ? C6a H12b 2.672(13) . . ? C7 C8 2.5363(16) . . ? C7 O81 2.8974(15) . . ? C7 C11a 2.5218(17) . . ? C7 C12 2.9552(18) . . ? C7 C12a 2.5262(18) . . ? C7 Br 3.0568(13) . . ? C7 H6A 2.546(18) . . ? C7 H6a 2.004(14) . . ? O7 C7a 2.3905(15) . . ? O7 C8 2.9354(15) . . ? O7 C81 2.7399(16) . . ? O7 O81 2.7052(12) . . ? O7 Br 3.7010(10) . . ? O7 H6a 2.456(15) . . ? C7a O81 2.4216(15) . . ? C7a C9 2.4331(16) . . ? C7a C10 2.8097(16) . . ? C7a C11 2.4359(17) . . ? C7a C12 2.5461(17) . . ? C7a C12a 2.9425(16) . . ? C7a Br 3.4650(12) . . ? C7a Br 3.9477(13) . '4 565' ? C8 C81 2.3558(19) . . ? C8 O82 2.6495(18) . . ? C8 C10 2.4016(17) . . ? C8 C11 2.7715(18) . . ? C8 C11a 2.4063(17) . . ? C8 H9 2.003(13) . . ? C81 H82A 2.04(2) . . ? C81 H82B 2.04(2) . . ? C81 H82C 1.968(18) . . ? O81 O82 2.2524(15) . . ? O81 C82 2.363(2) . . ? O81 C9 2.3858(15) . . ? O81 H82B 2.46(2) . . ? O81 H82C 2.677(18) . . ? O81 H9 2.505(13) . . ? O82 C82 2.4057(19) . . ? O82 H82A 2.569(19) . . ? O82 H11 2.609(14) . '4 564' ? C9 C11 2.4063(19) . . ? C9 C11a 2.7841(17) . . ? C9 Br 3.9026(14) . '4 565' ? C9 H10 2.033(15) . . ? C10 C11a 2.4061(16) . . ? C10 Br 3.5611(14) . '4 565' ? C10 H9 2.070(15) . . ? C10 H11 2.049(14) . . ? C11 C12 2.4711(15) . . ? C11 O12 2.7824(15) . . ? C11 Br 3.3994(13) . '4 565' ? C11 H10 2.013(14) . . ? C11a O12 2.3690(16) . . ? C11a C12a 2.5795(15) . . ? C11a Br 3.3510(12) . . ? C11a Br 3.5929(13) . '4 565' ? C11a H11 2.042(14) . . ? C12 C12b 2.6068(15) . . ? C12 Br 2.7513(12) . . ? C12 H11 2.600(14) . . ? O12 C12a 2.3952(15) . . ? O12 C12b 2.8943(14) . . ? O12 Br 3.5116(10) . . ? O12 H11 2.463(14) . . ? C12a H6a 2.014(14) . . ? C12a H12b 2.016(14) . . ? C12b Br 2.9465(13) . . ? C12b H6a 2.636(15) . . ? Br H4B 3.682(17) . '1 655' ? Br H6A 3.117(15) . '4 564' ? Br H6a 2.911(15) . . ? Br H11 3.668(15) . '4 564' ? Br H12b 2.930(15) . . ? Br H112B 3.56(2) . . ? Br H112C 3.39(2) . . ? H31A H31B 1.60(3) . . ? H31A H31C 1.55(3) . . ? H31B H31C 1.56(3) . . ? H32A H32B 1.57(3) . . ? H32A H32C 1.47(3) . . ? H32B H32C 1.45(3) . . ? H4A H4B 1.56(2) . . ? H4A H5 2.28(2) . . ? H5 H6B 2.39(2) . . ? H6A H6B 1.56(2) . . ? H6B H6a 2.23(2) . . ? H82A H82B 1.57(3) . . ? H82A H82C 1.53(3) . . ? H82B H82C 1.48(2) . . ? H9 H10 2.39(2) . . ? H10 H11 2.33(2) . . ? H112A H112B 1.45(3) . . ? H112A H112C 1.45(4) . . ? H112B H112C 1.51(3) . . ? _atom_sites_solution_primary ? _atom_sites_solution_secondary ? _atom_sites_solution_hydrogens ? _geom_special_details ? _cell_special_details ; ? ; _exptl_special_details ; ? ; _diffrn_special_details ; ? ; _chemical_compound_source ? _chemical_name_systematic ? _chemical_name_common ? _chemical_formula_analytical ? _chemical_formula_structural ? _exptl_crystal_F_000 1000 loop_ _diffrn_standard_refln_index_h _diffrn_standard_refln_index_k _diffrn_standard_refln_index_l ? ? ? loop_ _diffrn_attenuator_code _diffrn_attenuator_scale ? ? _reflns_limit_h_min 0 _reflns_limit_h_max 15 _reflns_limit_k_min 0 _reflns_limit_k_max 34 _reflns_limit_l_min -20 _reflns_limit_l_max 20 _reflns_number_observed ? _reflns_d_resolution_high .588 _reflns_d_resolution_low 8.677 _diffrn_reflns_av_sigmaI/netI .117 _diffrn_reflns_theta_min 2.34 _diffrn_reflns_reduction_process ? _diffrn_ambient_temperature 153 _diffrn_radiation_source 'sealed tube' _diffrn_radiation_monochromator graphite _diffrn_radiation_detector 'CCD area detector' _refine_ls_extinction_expression ? _refine_ls_matrix_type full _refine_ls_number_restraints 0 _refine_ls_number_constraints 0 _refine_ls_R_factor_all .064 _refine_ls_wR_factor_all .031 _refine_ls_goodness_of_fit_all .894 _refine_ls_shift/su_mean .002 #========================================================================== # Structure Factor lists should be submitted as separate files #========================================================================== #data_ # but for xtal use the refln data is needed in same block loop_ _refln_index_h _refln_index_k _refln_index_l _refln_F_meas _refln_F_calc _refln_F_sigma _refln_F_squared_meas _refln_F_squared_calc _refln_F_squared_sigma _refln_observed_status _refln_F_meas_friedel _refln_F_sigma_friedel _refln_F_squared_meas_friedel _refln_F_squared_sigma_friedel ? ? ? ? ? ? ? ? ? ? ? ? ? ? #-end-end-end-end-end-end-end-end-end-end-end-end-end-end-end-end-end-end