data_C:\structs\Terry\dmc4abr\DMC4ABR.CIF _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common 'dmc4abr' _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C48 H60 Br4 Cl4' _chemical_formula_weight 1098.40 loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source 'C' 'C' 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'H' 'H' 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'Br' 'Br' -0.2901 2.4595 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'Cl' 'Cl' 0.1484 0.1585 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting monoclinic _symmetry_space_group_name_H-M I2/a loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x+1/2, y, -z' 'x+1/2, y+1/2, z+1/2' '-x+1, y+1/2, -z+1/2' '-x, -y, -z' 'x-1/2, -y, z' '-x+1/2, -y+1/2, -z+1/2' 'x, -y+1/2, z+1/2' _cell_length_a 15.3492(3) _cell_length_b 17.7650(4) _cell_length_c 34.5444(7) _cell_angle_alpha 90.00 _cell_angle_beta 90.0280(10) _cell_angle_gamma 90.00 _cell_volume 9419.5(3) _cell_formula_units_Z 8 _cell_measurement_temperature 120(2) _cell_measurement_reflns_used ? _cell_measurement_theta_min ? _cell_measurement_theta_max ? _exptl_crystal_description 'block' _exptl_crystal_colour 'yellow' _exptl_crystal_size_max 0.80 _exptl_crystal_size_mid 0.70 _exptl_crystal_size_min 0.60 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.549 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 4448 _exptl_absorpt_coefficient_mu 3.678 _exptl_absorpt_correction_type empirical _exptl_absorpt_correction_T_min 0.1569 _exptl_absorpt_correction_T_max 0.2163 _exptl_absorpt_process_details ? _exptl_special_details ; Data were corrected for decay and absorption using the program Scalepack Z. Otwinowski and W. Minor, in Methods in Enzymology, ed. C. W. Carter and R. M. Sweet, Academic Press: London, 1997, vol. 276, pp 307. ; _diffrn_ambient_temperature 120(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator 'graphite' _diffrn_measurement_device_type 'Nonius KappaCCD' _diffrn_measurement_method ? _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% 0.0 _diffrn_reflns_number 28185 _diffrn_reflns_av_R_equivalents 0.1505 _diffrn_reflns_av_sigmaI/netI 0.1391 _diffrn_reflns_limit_h_min -18 _diffrn_reflns_limit_h_max 18 _diffrn_reflns_limit_k_min -21 _diffrn_reflns_limit_k_max 21 _diffrn_reflns_limit_l_min -42 _diffrn_reflns_limit_l_max 37 _diffrn_reflns_theta_min 1.18 _diffrn_reflns_theta_max 26.00 _reflns_number_total 9239 _reflns_number_gt 5365 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'Collect (Hooft, 1999)' _computing_cell_refinement 'DENZO-SMN (Otwinowski & Minor, 1997)' _computing_data_reduction 'DENZO-SMN (Otwinowski & Minor, 1997)' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'X-Seed (Barbour, 1999)' _computing_publication_material 'CIFTAB (Sheldrick, 1997)' _refine_special_details ; Refinement of F^2^ against ALL reflections. The weighted R-factor wR and goodness of fit S are based on F^2^, conventional R-factors R are based on F, with F set to zero for negative F^2^. The threshold expression of F^2^ > 2sigma(F^2^) is used only for calculating R-factors(gt) etc. and is not relevant to the choice of reflections for refinement. R-factors based on F^2^ are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger. ; _refine_ls_structure_factor_coef Fsqd _refine_ls_matrix_type full _refine_ls_weighting_scheme calc _refine_ls_weighting_details 'calc w=1/[\s^2^(Fo^2^)+(0.0499P)^2^+33.3609P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment mixed _refine_ls_extinction_method SHELXL _refine_ls_extinction_coef 0.00015(4) _refine_ls_extinction_expression 'Fc^*^=kFc[1+0.001xFc^2^\l^3^/sin(2\q)]^-1/4^' _refine_ls_number_reflns 9239 _refine_ls_number_parameters 518 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.1365 _refine_ls_R_factor_gt 0.0642 _refine_ls_wR_factor_ref 0.1537 _refine_ls_wR_factor_gt 0.1291 _refine_ls_goodness_of_fit_ref 1.013 _refine_ls_restrained_S_all 1.013 _refine_ls_shift/su_max 0.021 _refine_ls_shift/su_mean 0.000 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_symmetry_multiplicity _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group Br1 Br 0.86538(4) 0.22975(4) 0.202135(19) 0.0331(2) Uani 1 1 d . . . C1 C 0.8851(4) 0.2043(4) 0.25766(18) 0.0295(16) Uani 1 1 d . . . H1A H 0.8377 0.2263 0.2734 0.035 Uiso 1 1 calc R . . H1B H 0.8831 0.1490 0.2609 0.035 Uiso 1 1 calc R . . Br2 Br 1.22844(6) 0.67766(4) 0.39746(2) 0.0567(3) Uani 1 1 d . . . C2 C 0.9715(4) 0.2332(3) 0.27232(16) 0.0217(14) Uani 1 1 d . . . Br3 Br 0.86295(4) 0.14811(5) 0.53445(2) 0.0497(3) Uani 1 1 d . . . C3 C 0.9786(4) 0.3095(3) 0.28262(16) 0.0191(13) Uani 1 1 d . . . Br4 Br 1.53571(4) 0.06396(4) 0.36662(2) 0.0394(2) Uani 1 1 d . . . C4 C 1.0580(3) 0.3364(3) 0.29679(15) 0.0167(13) Uani 1 1 d . . . C5 C 1.1306(3) 0.2883(3) 0.29991(15) 0.0148(12) Uani 1 1 d . . . C6 C 1.1223(3) 0.2113(3) 0.29070(15) 0.0178(13) Uani 1 1 d . . . C7 C 1.0429(4) 0.1842(3) 0.27483(16) 0.0230(14) Uani 1 1 d . . . C8 C 0.9012(4) 0.3624(4) 0.2772(2) 0.0389(19) Uani 1 1 d . . . H8A H 0.9174 0.4132 0.2856 0.058 Uiso 1 1 calc R . . H8B H 0.8520 0.3444 0.2927 0.058 Uiso 1 1 calc R . . H8C H 0.8846 0.3635 0.2498 0.058 Uiso 1 1 calc R . . C9 C 1.2181(4) 0.3197(3) 0.31170(16) 0.0205(14) Uani 1 1 d . . . H9A H 1.2212 0.3228 0.3400 0.031 Uiso 1 1 calc R . . H9B H 1.2254 0.3700 0.3006 0.031 Uiso 1 1 calc R . . H9C H 1.2644 0.2866 0.3022 0.031 Uiso 1 1 calc R . . C10 C 1.0350(4) 0.1040(3) 0.2607(2) 0.0353(17) Uani 1 1 d . . . H10A H 1.0168 0.0715 0.2822 0.053 Uiso 1 1 calc R . . H10B H 1.0915 0.0869 0.2509 0.053 Uiso 1 1 calc R . . H10C H 0.9916 0.1015 0.2399 0.053 Uiso 1 1 calc R . . C11 C 1.0686(4) 0.4196(3) 0.30619(16) 0.0205(14) Uani 1 1 d . . . H11A H 1.0109 0.4439 0.3033 0.025 Uiso 1 1 calc R . . H11B H 1.1073 0.4419 0.2863 0.025 Uiso 1 1 calc R . . C12 C 1.2743(4) 0.5754(4) 0.3868(2) 0.0368(18) Uani 1 1 d . . . H12A H 1.3069 0.5759 0.3621 0.044 Uiso 1 1 calc R . . H12B H 1.3152 0.5608 0.4076 0.044 Uiso 1 1 calc R . . C13 C 1.2018(4) 0.5183(3) 0.38440(18) 0.0261(15) Uani 1 1 d . . . C14 C 1.1704(4) 0.4971(3) 0.34769(16) 0.0196(13) Uani 1 1 d . . . C15 C 1.1046(3) 0.4411(3) 0.34577(16) 0.0162(13) Uani 1 1 d . . . C16 C 1.0703(4) 0.4103(3) 0.37988(16) 0.0178(13) Uani 1 1 d . . . C17 C 1.1047(4) 0.4304(3) 0.41627(16) 0.0190(13) Uani 1 1 d . . . C18 C 1.1687(4) 0.4857(3) 0.41824(17) 0.0235(14) Uani 1 1 d . . . C19 C 1.2054(4) 0.5338(4) 0.31145(19) 0.0334(16) Uani 1 1 d . . . H19A H 1.2482 0.5004 0.2992 0.050 Uiso 1 1 calc R . . H19B H 1.2334 0.5816 0.3182 0.050 Uiso 1 1 calc R . . H19C H 1.1574 0.5432 0.2934 0.050 Uiso 1 1 calc R . . C20 C 0.9929(4) 0.3576(3) 0.37777(17) 0.0251(15) Uani 1 1 d . . . H20A H 1.0135 0.3054 0.3766 0.038 Uiso 1 1 calc R . . H20B H 0.9587 0.3689 0.3545 0.038 Uiso 1 1 calc R . . H20C H 0.9564 0.3644 0.4008 0.038 Uiso 1 1 calc R . . C21 C 1.2018(4) 0.5132(4) 0.45677(18) 0.0368(17) Uani 1 1 d . . . H21A H 1.1527 0.5198 0.4745 0.055 Uiso 1 1 calc R . . H21B H 1.2318 0.5615 0.4533 0.055 Uiso 1 1 calc R . . H21C H 1.2426 0.4763 0.4676 0.055 Uiso 1 1 calc R . . C22 C 1.0674(4) 0.3971(4) 0.45310(17) 0.0265(15) Uani 1 1 d . . . H22A H 1.0096 0.4204 0.4573 0.032 Uiso 1 1 calc R . . H22B H 1.1052 0.4136 0.4747 0.032 Uiso 1 1 calc R . . C23 C 0.8759(4) 0.1726(4) 0.47902(19) 0.0353(17) Uani 1 1 d . . . H23A H 0.8660 0.1265 0.4635 0.042 Uiso 1 1 calc R . . H23B H 0.8309 0.2098 0.4716 0.042 Uiso 1 1 calc R . . C24 C 0.9642(4) 0.2039(4) 0.46940(17) 0.0251(15) Uani 1 1 d . . . C25 C 0.9760(4) 0.2823(4) 0.46901(16) 0.0245(15) Uani 1 1 d . . . C26 C 1.0559(4) 0.3125(3) 0.45683(15) 0.0209(14) Uani 1 1 d . . . C27 C 1.1258(3) 0.2639(3) 0.44887(15) 0.0170(13) Uani 1 1 d . . . C28 C 1.1145(3) 0.1854(3) 0.44980(15) 0.0186(13) Uani 1 1 d . . . C29 C 1.0332(4) 0.1553(3) 0.46009(17) 0.0229(14) Uani 1 1 d . . . C30 C 0.9032(4) 0.3337(4) 0.48367(19) 0.0343(17) Uani 1 1 d . . . H30A H 0.9287 0.3763 0.4977 0.051 Uiso 1 1 calc R . . H30B H 0.8650 0.3054 0.5011 0.051 Uiso 1 1 calc R . . H30C H 0.8693 0.3525 0.4616 0.051 Uiso 1 1 calc R . . C31 C 1.2157(4) 0.2965(3) 0.44154(18) 0.0249(14) Uani 1 1 d . . . H31A H 1.2248 0.3022 0.4136 0.037 Uiso 1 1 calc R . . H31B H 1.2600 0.2626 0.4522 0.037 Uiso 1 1 calc R . . H31C H 1.2204 0.3458 0.4541 0.037 Uiso 1 1 calc R . . C32 C 1.0161(4) 0.0708(4) 0.4623(2) 0.0377(17) Uani 1 1 d . . . H32A H 0.9911 0.0535 0.4378 0.056 Uiso 1 1 calc R . . H32B H 0.9753 0.0604 0.4834 0.056 Uiso 1 1 calc R . . H32C H 1.0711 0.0443 0.4671 0.056 Uiso 1 1 calc R . . C33 C 1.1908(4) 0.1332(3) 0.44213(16) 0.0230(14) Uani 1 1 d . . . H33A H 1.1683 0.0810 0.4426 0.028 Uiso 1 1 calc R . . H33B H 1.2318 0.1382 0.4641 0.028 Uiso 1 1 calc R . . C34 C 1.4791(4) 0.1631(3) 0.37343(19) 0.0258(15) Uani 1 1 d . . . H34A H 1.4964 0.1848 0.3987 0.031 Uiso 1 1 calc R . . H34B H 1.4988 0.1977 0.3528 0.031 Uiso 1 1 calc R . . C35 C 1.3810(4) 0.1555(3) 0.37182(17) 0.0212(14) Uani 1 1 d . . . C36 C 1.3340(4) 0.1452(3) 0.40619(16) 0.0211(14) Uani 1 1 d . . . C37 C 1.2429(4) 0.1428(3) 0.40498(16) 0.0205(14) Uani 1 1 d . . . C38 C 1.2003(3) 0.1462(3) 0.36896(16) 0.0174(13) Uani 1 1 d . . . C39 C 1.2472(4) 0.1562(3) 0.33456(16) 0.0180(13) Uani 1 1 d . . . C40 C 1.3389(4) 0.1603(3) 0.33581(16) 0.0207(14) Uani 1 1 d . . . C41 C 1.3833(4) 0.1336(4) 0.44454(18) 0.0353(17) Uani 1 1 d . . . H41A H 1.3868 0.1815 0.4585 0.053 Uiso 1 1 calc R . . H41B H 1.4423 0.1152 0.4391 0.053 Uiso 1 1 calc R . . H41C H 1.3523 0.0966 0.4604 0.053 Uiso 1 1 calc R . . C42 C 1.1023(4) 0.1317(3) 0.36694(17) 0.0224(14) Uani 1 1 d . . . H42A H 1.0712 0.1799 0.3658 0.034 Uiso 1 1 calc R . . H42B H 1.0838 0.1038 0.3900 0.034 Uiso 1 1 calc R . . H42C H 1.0889 0.1022 0.3437 0.034 Uiso 1 1 calc R . . C43 C 1.3918(4) 0.1644(4) 0.29879(17) 0.0295(16) Uani 1 1 d . . . H43A H 1.3957 0.2168 0.2902 0.044 Uiso 1 1 calc R . . H43B H 1.3635 0.1341 0.2787 0.044 Uiso 1 1 calc R . . H43C H 1.4505 0.1448 0.3036 0.044 Uiso 1 1 calc R . . C44 C 1.1998(4) 0.1581(3) 0.29571(16) 0.0204(14) Uani 1 1 d . . . H44A H 1.1792 0.1065 0.2902 0.024 Uiso 1 1 calc R . . H44B H 1.2432 0.1710 0.2756 0.024 Uiso 1 1 calc R . . Cl1S Cl 1.40387(14) 0.42575(15) 0.34551(6) 0.0714(7) Uani 1 1 d . . . C1S C 1.4639(6) 0.3553(5) 0.4126(3) 0.073(3) Uani 1 1 d . . . H1S1 H 1.5149 0.3320 0.4254 0.087 Uiso 1 1 calc R . . H1S2 H 1.4195 0.3156 0.4085 0.087 Uiso 1 1 calc R . . Cl2S Cl 1.42065(14) 0.42568(12) 0.44275(6) 0.0581(6) Uani 1 1 d . . . C2S C 1.4903(5) 0.3865(5) 0.3752(3) 0.064(2) Uani 1 1 d . . . H2S1 H 1.5194 0.3461 0.3602 0.076 Uiso 1 1 calc R . . H2S2 H 1.5340 0.4264 0.3799 0.076 Uiso 1 1 calc R . . Cl3S Cl 0.87779(16) 0.15768(17) 0.35987(9) 0.0927(9) Uani 1 1 d . . . C3S C 0.7805(6) 0.1134(5) 0.3664(3) 0.085(3) Uani 1 1 d . . . H3S1 H 0.7690 0.1079 0.3945 0.102 Uiso 1 1 calc R . . H3S2 H 0.7333 0.1445 0.3551 0.102 Uiso 1 1 calc R . . Cl4S Cl 0.77997(18) 0.03607(13) 0.29554(7) 0.0806(8) Uani 1 1 d . . . C4S C 0.7799(6) 0.0377(5) 0.3479(3) 0.069(3) Uani 1 1 d . . . H4S1 H 0.7277 0.0102 0.3571 0.082 Uiso 1 1 calc R . . H4S2 H 0.8317 0.0096 0.3571 0.082 Uiso 1 1 calc R . . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 Br1 0.0277(4) 0.0392(4) 0.0324(4) -0.0028(3) -0.0093(3) -0.0056(3) C1 0.027(4) 0.029(4) 0.033(4) 0.006(3) 0.001(3) -0.011(3) Br2 0.0777(6) 0.0271(4) 0.0651(6) 0.0001(4) -0.0325(4) -0.0140(4) C2 0.014(3) 0.030(4) 0.020(3) 0.003(3) 0.001(2) -0.001(3) Br3 0.0195(4) 0.0814(6) 0.0483(5) 0.0226(4) 0.0122(3) 0.0050(4) C3 0.017(3) 0.025(4) 0.015(3) 0.001(3) 0.001(2) 0.004(3) Br4 0.0303(4) 0.0404(5) 0.0476(5) 0.0040(3) 0.0044(3) 0.0179(3) C4 0.016(3) 0.021(3) 0.013(3) -0.001(2) -0.001(2) -0.001(3) C5 0.014(3) 0.018(3) 0.012(3) 0.000(2) -0.001(2) 0.000(2) C6 0.015(3) 0.025(4) 0.013(3) -0.001(3) 0.001(2) 0.004(3) C7 0.037(4) 0.021(3) 0.011(3) -0.001(3) 0.000(3) -0.002(3) C8 0.026(4) 0.042(5) 0.049(5) -0.021(4) -0.015(3) 0.010(3) C9 0.023(3) 0.021(3) 0.018(3) 0.000(3) -0.002(2) 0.003(3) C10 0.037(4) 0.025(4) 0.044(4) 0.002(3) -0.013(3) -0.003(3) C11 0.021(3) 0.019(3) 0.021(3) 0.001(3) -0.005(3) 0.001(3) C12 0.032(4) 0.043(5) 0.036(4) -0.011(3) -0.007(3) -0.004(3) C13 0.022(4) 0.018(4) 0.038(4) -0.004(3) -0.010(3) 0.004(3) C14 0.017(3) 0.017(3) 0.026(3) 0.001(3) 0.002(3) 0.002(3) C15 0.015(3) 0.015(3) 0.019(3) -0.002(2) -0.003(2) 0.008(2) C16 0.016(3) 0.015(3) 0.022(3) -0.003(3) 0.000(2) 0.004(2) C17 0.023(3) 0.012(3) 0.022(3) -0.003(3) -0.001(3) 0.006(3) C18 0.027(4) 0.022(4) 0.021(3) -0.008(3) -0.008(3) 0.006(3) C19 0.035(4) 0.027(4) 0.038(4) 0.000(3) 0.000(3) -0.013(3) C20 0.019(3) 0.031(4) 0.025(3) 0.002(3) 0.004(3) -0.001(3) C21 0.051(5) 0.033(4) 0.027(4) -0.007(3) -0.013(3) -0.003(3) C22 0.025(4) 0.033(4) 0.021(3) -0.010(3) 0.001(3) -0.002(3) C23 0.021(4) 0.050(5) 0.035(4) 0.008(3) -0.002(3) 0.002(3) C24 0.015(3) 0.036(4) 0.023(3) 0.004(3) -0.001(3) 0.001(3) C25 0.013(3) 0.046(5) 0.014(3) 0.004(3) -0.002(2) 0.007(3) C26 0.027(4) 0.028(4) 0.008(3) 0.002(3) -0.007(2) 0.002(3) C27 0.011(3) 0.028(4) 0.012(3) 0.004(3) 0.003(2) 0.003(3) C28 0.011(3) 0.031(4) 0.013(3) 0.006(3) -0.001(2) 0.005(3) C29 0.019(3) 0.026(4) 0.024(3) 0.005(3) -0.002(3) 0.001(3) C30 0.019(4) 0.043(4) 0.041(4) 0.006(3) 0.006(3) 0.011(3) C31 0.015(3) 0.028(4) 0.032(4) 0.007(3) 0.005(3) 0.001(3) C32 0.031(4) 0.044(5) 0.039(4) 0.004(4) 0.013(3) -0.001(3) C33 0.027(4) 0.024(4) 0.018(3) 0.007(3) 0.003(3) 0.007(3) C34 0.019(3) 0.022(4) 0.036(4) 0.002(3) 0.003(3) 0.002(3) C35 0.019(3) 0.017(3) 0.028(4) 0.006(3) 0.001(3) 0.009(3) C36 0.019(3) 0.024(4) 0.020(3) 0.007(3) -0.002(3) 0.008(3) C37 0.020(3) 0.019(3) 0.022(3) 0.010(3) 0.007(2) 0.005(3) C38 0.018(3) 0.010(3) 0.025(3) 0.006(3) 0.000(2) -0.001(2) C39 0.020(3) 0.015(3) 0.019(3) 0.004(3) 0.000(2) 0.005(3) C40 0.025(4) 0.016(3) 0.021(3) 0.001(3) 0.006(3) 0.005(3) C41 0.023(4) 0.058(5) 0.025(4) 0.010(3) -0.001(3) 0.013(3) C42 0.021(3) 0.018(3) 0.028(4) 0.002(3) 0.003(3) -0.001(3) C43 0.023(4) 0.039(4) 0.027(4) 0.005(3) 0.003(3) 0.009(3) C44 0.026(4) 0.017(3) 0.018(3) 0.001(3) 0.000(3) 0.010(3) Cl1S 0.0474(13) 0.111(2) 0.0559(14) -0.0096(13) -0.0093(10) -0.0109(13) C1S 0.068(6) 0.048(6) 0.102(8) -0.014(5) 0.008(6) 0.001(5) Cl2S 0.0693(15) 0.0630(14) 0.0420(12) -0.0035(10) 0.0077(10) 0.0013(11) C2S 0.052(6) 0.048(5) 0.092(7) 0.007(5) 0.020(5) 0.009(4) Cl3S 0.0559(16) 0.113(2) 0.109(2) -0.0388(18) 0.0013(14) -0.0210(15) C3S 0.064(7) 0.060(7) 0.131(10) -0.010(6) 0.012(6) -0.003(5) Cl4S 0.119(2) 0.0480(14) 0.0744(17) 0.0075(12) 0.0012(14) -0.0421(14) C4S 0.077(7) 0.035(5) 0.094(7) -0.001(5) 0.012(5) 0.007(5) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag Br1 C1 1.994(6) . ? C1 C2 1.509(8) . ? Br2 C12 1.983(7) . ? C2 C7 1.401(8) . ? C2 C3 1.406(8) . ? Br3 C23 1.974(6) . ? C3 C4 1.396(7) . ? C3 C8 1.526(8) . ? Br4 C34 1.978(6) . ? C4 C5 1.410(7) . ? C4 C11 1.522(8) . ? C5 C6 1.409(8) . ? C5 C9 1.510(7) . ? C6 C7 1.420(8) . ? C6 C44 1.529(7) . ? C7 C10 1.512(8) . ? C11 C15 1.523(7) . ? C12 C13 1.508(9) . ? C13 C18 1.400(9) . ? C13 C14 1.408(8) . ? C14 C15 1.419(8) . ? C14 C19 1.511(8) . ? C15 C16 1.403(8) . ? C16 C17 1.410(8) . ? C16 C20 1.514(8) . ? C17 C18 1.391(8) . ? C17 C22 1.515(8) . ? C18 C21 1.506(8) . ? C22 C26 1.519(8) . ? C23 C24 1.502(8) . ? C24 C29 1.404(8) . ? C24 C25 1.405(9) . ? C25 C26 1.403(8) . ? C25 C30 1.530(8) . ? C26 C27 1.405(8) . ? C27 C28 1.406(8) . ? C27 C31 1.518(8) . ? C28 C29 1.404(8) . ? C28 C33 1.516(8) . ? C29 C32 1.525(9) . ? C33 C37 1.523(8) . ? C34 C35 1.512(8) . ? C35 C36 1.402(8) . ? C35 C40 1.404(8) . ? C36 C37 1.398(8) . ? C36 C41 1.540(8) . ? C37 C38 1.407(8) . ? C38 C39 1.401(8) . ? C38 C42 1.529(7) . ? C39 C40 1.409(8) . ? C39 C44 1.527(7) . ? C40 C43 1.518(8) . ? Cl1S C2S 1.815(9) . ? C1S C2S 1.465(12) . ? C1S Cl2S 1.757(9) . ? Cl3S C3S 1.703(9) . ? C3S C4S 1.489(11) . ? Cl4S C4S 1.809(10) . ? 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_3 _geom_angle_publ_flag C2 C1 Br1 112.3(4) . . ? C7 C2 C3 121.5(5) . . ? C7 C2 C1 119.8(5) . . ? C3 C2 C1 118.7(5) . . ? C4 C3 C2 119.1(5) . . ? C4 C3 C8 120.7(5) . . ? C2 C3 C8 120.1(5) . . ? C3 C4 C5 120.6(5) . . ? C3 C4 C11 120.1(5) . . ? C5 C4 C11 119.2(5) . . ? C6 C5 C4 120.0(5) . . ? C6 C5 C9 120.0(5) . . ? C4 C5 C9 120.0(5) . . ? C5 C6 C7 119.5(5) . . ? C5 C6 C44 120.2(5) . . ? C7 C6 C44 120.2(5) . . ? C2 C7 C6 119.0(5) . . ? C2 C7 C10 120.2(5) . . ? C6 C7 C10 120.8(5) . . ? C4 C11 C15 118.3(5) . . ? C13 C12 Br2 111.4(4) . . ? C18 C13 C14 121.1(5) . . ? C18 C13 C12 120.0(5) . . ? C14 C13 C12 118.8(6) . . ? C13 C14 C15 118.2(5) . . ? C13 C14 C19 120.6(5) . . ? C15 C14 C19 121.2(5) . . ? C16 C15 C14 120.2(5) . . ? C16 C15 C11 121.3(5) . . ? C14 C15 C11 118.4(5) . . ? C15 C16 C17 120.6(5) . . ? C15 C16 C20 119.8(5) . . ? C17 C16 C20 119.6(5) . . ? C18 C17 C16 119.2(5) . . ? C18 C17 C22 120.1(5) . . ? C16 C17 C22 120.5(5) . . ? C17 C18 C13 120.5(5) . . ? C17 C18 C21 120.7(6) . . ? C13 C18 C21 118.8(6) . . ? C17 C22 C26 120.1(5) . . ? C24 C23 Br3 112.8(4) . . ? C29 C24 C25 120.7(5) . . ? C29 C24 C23 120.3(6) . . ? C25 C24 C23 119.1(6) . . ? C26 C25 C24 119.7(5) . . ? C26 C25 C30 120.6(6) . . ? C24 C25 C30 119.6(5) . . ? C25 C26 C27 119.4(5) . . ? C25 C26 C22 120.4(5) . . ? C27 C26 C22 120.2(5) . . ? C26 C27 C28 120.8(5) . . ? C26 C27 C31 119.5(5) . . ? C28 C27 C31 119.6(5) . . ? C29 C28 C27 119.6(5) . . ? C29 C28 C33 119.9(5) . . ? C27 C28 C33 120.5(5) . . ? C24 C29 C28 119.7(6) . . ? C24 C29 C32 117.6(5) . . ? C28 C29 C32 122.7(5) . . ? C28 C33 C37 119.0(5) . . ? C35 C34 Br4 110.8(4) . . ? C36 C35 C40 121.4(5) . . ? C36 C35 C34 119.6(5) . . ? C40 C35 C34 119.0(5) . . ? C37 C36 C35 119.6(5) . . ? C37 C36 C41 120.9(5) . . ? C35 C36 C41 119.5(5) . . ? C36 C37 C38 119.3(5) . . ? C36 C37 C33 120.3(5) . . ? C38 C37 C33 120.4(5) . . ? C39 C38 C37 121.1(5) . . ? C39 C38 C42 119.3(5) . . ? C37 C38 C42 119.4(5) . . ? C38 C39 C40 119.6(5) . . ? C38 C39 C44 120.3(5) . . ? C40 C39 C44 120.1(5) . . ? C35 C40 C39 118.9(5) . . ? C35 C40 C43 120.2(5) . . ? C39 C40 C43 120.8(5) . . ? C39 C44 C6 118.9(5) . . ? C2S C1S Cl2S 111.0(7) . . ? C1S C2S Cl1S 116.2(6) . . ? C4S C3S Cl3S 111.4(7) . . ? C3S C4S Cl4S 116.3(7) . . ? _diffrn_measured_fraction_theta_max 0.997 _diffrn_reflns_theta_full 26.00 _diffrn_measured_fraction_theta_full 0.997 _refine_diff_density_max 1.803 _refine_diff_density_min -0.942 _refine_diff_density_rms 0.123