# Supplementary Material (ESI) for Chemical Communications # This journal is © The Royal Society of Chemistry 2003 data_global _journal_name_full Chem.Commun. _journal_coden_Cambridge 0182 loop_ _publ_author_name 'Markus Albrecht' 'Marita deGroot' 'Roland Frohlich' 'Soren Schmid' 'Patrick Weis' _publ_contact_author_name 'Prof Markus Albrecht' _publ_contact_author_address ; Aachen GERMANY ; _publ_contact_author_email MARKUS.ALBRECHT@OC.RWTH-AACHEN.DE _publ_section_title ; Self-assembly of an unpolar enantiomerically pure helicate-type metalla-cryptand ; data_fro2333 _database_code_CSD 215037 _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C69 H54 Br6 Fe2 O18' _chemical_formula_weight 1762.28 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' O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Fe Fe 0.3463 0.8444 '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' _symmetry_cell_setting orthorhombic _symmetry_space_group_name_H-M P212121 loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x+1/2, -y, z+1/2' '-x, y+1/2, -z+1/2' 'x+1/2, -y+1/2, -z' _cell_length_a 13.353(8) _cell_length_b 17.002(6) _cell_length_c 33.065(17) _cell_angle_alpha 90.00 _cell_angle_beta 90.00 _cell_angle_gamma 90.00 _cell_volume 7507(6) _cell_formula_units_Z 4 _cell_measurement_temperature 198(2) _cell_measurement_reflns_used ? _cell_measurement_theta_min ? _cell_measurement_theta_max ? _exptl_crystal_description plate _exptl_crystal_colour red _exptl_crystal_size_max 0.45 _exptl_crystal_size_mid 0.20 _exptl_crystal_size_min 0.05 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.559 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 3496 _exptl_absorpt_coefficient_mu 3.644 _exptl_absorpt_correction_type none _exptl_absorpt_correction_T_min 0.2909 _exptl_absorpt_correction_T_max 0.8388 _exptl_absorpt_process_details ? _exptl_special_details ; ? ; _diffrn_ambient_temperature 198(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'rotating anode Nonius FR591' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'Nonius KappaCCD' _diffrn_measurement_method '\w and \f scans' _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 8311 _diffrn_reflns_av_R_equivalents 0.0907 _diffrn_reflns_av_sigmaI/netI 0.1028 _diffrn_reflns_limit_h_min -15 _diffrn_reflns_limit_h_max 12 _diffrn_reflns_limit_k_min -21 _diffrn_reflns_limit_k_max 21 _diffrn_reflns_limit_l_min -40 _diffrn_reflns_limit_l_max 40 _diffrn_reflns_theta_min 1.35 _diffrn_reflns_theta_max 26.30 _reflns_number_total 7324 _reflns_number_gt 3617 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'Collect (Nonius B.V., 1998)' _computing_cell_refinement 'Collect (Nonius B.V., 1998)' _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 'SCHAKAL (Keller, 1997)' _computing_publication_material 'SHELXL-97 (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. Crystals were of very poor quality, analysis only done to confirm the presence of the metalla-cryptand. Dur to the limited amount of data carbon atoms were refined with isotropic thermal displacement parameters only. ; _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^)+(0.1102P)^2^+161.8092P] 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 'refined as riding atoms' _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_abs_structure_details 'Flack H D (1983), Acta Cryst. A39, 876-881' _refine_ls_abs_structure_Flack 0.02(4) _refine_ls_number_reflns 7324 _refine_ls_number_parameters 517 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.2219 _refine_ls_R_factor_gt 0.1354 _refine_ls_wR_factor_ref 0.3624 _refine_ls_wR_factor_gt 0.3017 _refine_ls_goodness_of_fit_ref 1.055 _refine_ls_restrained_S_all 1.055 _refine_ls_shift/su_max 0.000 _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 Fe1 Fe 0.7403(4) 0.4556(3) 1.14168(13) 0.0739(14) Uani 1 1 d . . . Fe2 Fe 0.9115(4) 0.5083(3) 0.99815(15) 0.0778(15) Uani 1 1 d . . . O11 O 0.7999(16) 0.4550(11) 1.1947(5) 0.061(6) Uani 1 1 d . . . C11 C 0.890(3) 0.4435(19) 1.2042(9) 0.061(8) Uiso 1 1 d . . . C111 C 0.916(3) 0.469(2) 1.2456(10) 0.079(10) Uiso 1 1 d . . . C112 C 0.842(4) 0.504(3) 1.2699(14) 0.130(17) Uiso 1 1 d . . . H112 H 0.7763 0.5071 1.2594 0.156 Uiso 1 1 calc R . . C113 C 0.861(4) 0.535(3) 1.3106(13) 0.114(15) Uiso 1 1 d . . . H113 H 0.8084 0.5525 1.3274 0.137 Uiso 1 1 calc R . . C114 C 0.961(3) 0.537(2) 1.3232(9) 0.073(9) Uiso 1 1 d . . . C115 C 1.037(3) 0.501(2) 1.3008(11) 0.098(12) Uiso 1 1 d . . . H115 H 1.1020 0.4932 1.3122 0.117 Uiso 1 1 calc R . . C116 C 1.015(3) 0.476(2) 1.2593(11) 0.095(12) Uiso 1 1 d . . . H116 H 1.0687 0.4641 1.2414 0.114 Uiso 1 1 calc R . . Br11 Br 0.9877(4) 0.5649(3) 1.37527(11) 0.1043(15) Uani 1 1 d . . . C12 C 0.964(2) 0.4088(16) 1.1801(8) 0.059(8) Uiso 1 1 d . . . H12 H 1.0285 0.3992 1.1908 0.071 Uiso 1 1 calc R . . C13 C 0.942(3) 0.3891(19) 1.1413(10) 0.068(9) Uiso 1 1 d . . . O13 O 0.8588(19) 0.3959(13) 1.1213(7) 0.083(7) Uani 1 1 d . . . C14 C 1.016(3) 0.3406(19) 1.1139(9) 0.074(9) Uiso 1 1 d . . . H14 H 0.9820 0.3020 1.0958 0.088 Uiso 1 1 calc R . . O14 O 1.0868(19) 0.3047(18) 1.1414(6) 0.099(8) Uani 1 1 d . . . C19 C 1.179(3) 0.304(2) 1.1194(10) 0.074(9) Uiso 1 1 d . . . C19A C 1.203(4) 0.226(3) 1.1003(13) 0.130(17) Uiso 1 1 d . . . H19A H 1.2120 0.1860 1.1214 0.195 Uiso 1 1 calc R . . H19B H 1.2650 0.2303 1.0845 0.195 Uiso 1 1 calc R . . H19C H 1.1481 0.2102 1.0824 0.195 Uiso 1 1 calc R . . C19B C 1.262(3) 0.323(2) 1.1487(11) 0.099(12) Uiso 1 1 d . . . H19D H 1.2433 0.3698 1.1645 0.149 Uiso 1 1 calc R . . H19E H 1.3239 0.3340 1.1338 0.149 Uiso 1 1 calc R . . H19F H 1.2727 0.2787 1.1670 0.149 Uiso 1 1 calc R . . O15 O 1.1802(19) 0.3651(18) 1.0899(7) 0.104(9) Uani 1 1 d . . . C15 C 1.082(3) 0.408(2) 1.0892(9) 0.071(9) Uiso 1 1 d . . . H15 H 1.0850 0.4588 1.1041 0.085 Uiso 1 1 calc R . . C16 C 1.044(3) 0.4176(19) 1.0472(9) 0.067(9) Uiso 1 1 d . . . O16 O 0.9626(19) 0.452(2) 1.0450(6) 0.110(10) Uani 1 1 d . . . C17 C 1.095(3) 0.389(2) 1.0129(10) 0.083(11) Uiso 1 1 d . . . H17 H 1.1552 0.3612 1.0179 0.100 Uiso 1 1 calc R . . C18 C 1.068(3) 0.397(2) 0.9730(10) 0.069(9) Uiso 1 1 d . . . O18 O 0.9919(19) 0.4343(12) 0.9641(6) 0.080(7) Uani 1 1 d . . . C181 C 1.142(3) 0.370(2) 0.9395(10) 0.072(9) Uiso 1 1 d . . . C182 C 1.189(2) 0.3037(19) 0.9416(9) 0.064(8) Uiso 1 1 d . . . H182 H 1.1837 0.2715 0.9649 0.077 Uiso 1 1 calc R . . C183 C 1.247(3) 0.280(2) 0.9076(10) 0.089(11) Uiso 1 1 d . . . H183 H 1.2858 0.2333 0.9084 0.107 Uiso 1 1 calc R . . C184 C 1.245(3) 0.3250(19) 0.8748(9) 0.069(9) Uiso 1 1 d . . . C185 C 1.203(2) 0.3946(17) 0.8722(9) 0.062(8) Uiso 1 1 d . . . H185 H 1.2173 0.4281 0.8499 0.074 Uiso 1 1 calc R . . C186 C 1.136(3) 0.419(2) 0.9034(10) 0.085(11) Uiso 1 1 d . . . H186 H 1.0923 0.4625 0.9008 0.102 Uiso 1 1 calc R . . Br18 Br 1.3287(3) 0.2953(3) 0.83004(11) 0.0962(13) Uani 1 1 d . . . O21 O 0.6654(18) 0.3600(11) 1.1529(6) 0.070(6) Uani 1 1 d . . . C21 C 0.585(3) 0.337(2) 1.1322(11) 0.078(10) Uiso 1 1 d . . . C211 C 0.541(3) 0.2633(19) 1.1519(9) 0.068(9) Uiso 1 1 d . . . C212 C 0.477(3) 0.217(2) 1.1313(12) 0.100(12) Uiso 1 1 d . . . H212 H 0.4540 0.2321 1.1052 0.119 Uiso 1 1 calc R . . C213 C 0.442(4) 0.143(3) 1.1485(14) 0.116(15) Uiso 1 1 d . . . H213 H 0.4072 0.1045 1.1333 0.139 Uiso 1 1 calc R . . C214 C 0.465(4) 0.133(3) 1.1902(15) 0.118(15) Uiso 1 1 d . . . C215 C 0.520(4) 0.178(3) 1.2090(14) 0.123(16) Uiso 1 1 d . . . H215 H 0.5370 0.1639 1.2359 0.148 Uiso 1 1 calc R . . C216 C 0.562(3) 0.254(2) 1.1932(11) 0.089(11) Uiso 1 1 d . . . H216 H 0.5982 0.2907 1.2090 0.107 Uiso 1 1 calc R . . Br21 Br 0.4209(6) 0.0380(4) 1.2146(2) 0.180(3) Uani 1 1 d . . . C22 C 0.550(3) 0.362(2) 1.0974(10) 0.081(10) Uiso 1 1 d . . . H22 H 0.4921 0.3386 1.0857 0.097 Uiso 1 1 calc R . . C23 C 0.600(3) 0.429(2) 1.0766(11) 0.079(11) Uiso 1 1 d . . . O23 O 0.687(2) 0.4524(12) 1.0865(6) 0.077(7) Uani 1 1 d . . . C24 C 0.562(3) 0.451(2) 1.0357(9) 0.066(9) Uiso 1 1 d . . . H24 H 0.5683 0.5090 1.0322 0.079 Uiso 1 1 calc R . . O24 O 0.4646(17) 0.4287(15) 1.0289(6) 0.081(7) Uani 1 1 d . . . C29 C 0.448(3) 0.3953(19) 0.9903(10) 0.067(9) Uiso 1 1 d . . . C29B C 0.367(3) 0.430(2) 0.9675(10) 0.083(10) Uiso 1 1 d . . . H29A H 0.3033 0.4103 0.9779 0.125 Uiso 1 1 calc R . . H29B H 0.3740 0.4149 0.9389 0.125 Uiso 1 1 calc R . . H29C H 0.3699 0.4870 0.9700 0.125 Uiso 1 1 calc R . . C29A C 0.429(3) 0.305(2) 0.9944(10) 0.091(11) Uiso 1 1 d . . . H29D H 0.4852 0.2806 1.0085 0.136 Uiso 1 1 calc R . . H29E H 0.4215 0.2819 0.9675 0.136 Uiso 1 1 calc R . . H29F H 0.3671 0.2967 1.0100 0.136 Uiso 1 1 calc R . . O25 O 0.5419(18) 0.408(2) 0.9697(6) 0.113(11) Uani 1 1 d . . . C25 C 0.617(3) 0.409(2) 1.0008(10) 0.078(10) Uiso 1 1 d . . . H25 H 0.6387 0.3550 1.0085 0.094 Uiso 1 1 calc R . . C26 C 0.703(3) 0.456(2) 0.9831(10) 0.073(9) Uiso 1 1 d . . . O26 O 0.7862(17) 0.4460(17) 1.0012(5) 0.092(8) Uani 1 1 d . . . C27 C 0.692(3) 0.516(2) 0.9516(9) 0.077(10) Uiso 1 1 d . . . H27 H 0.6263 0.5291 0.9426 0.093 Uiso 1 1 calc R . . C28 C 0.773(3) 0.552(2) 0.9345(10) 0.077(10) Uiso 1 1 d . . . O28 O 0.8582(19) 0.5495(15) 0.9474(5) 0.083(8) Uani 1 1 d . . . C281 C 0.756(4) 0.604(2) 0.8966(12) 0.096(12) Uiso 1 1 d . . . C282 C 0.665(3) 0.620(2) 0.8820(11) 0.091(12) Uiso 1 1 d . . . H282 H 0.6077 0.6009 0.8962 0.109 Uiso 1 1 calc R . . C283 C 0.650(4) 0.664(2) 0.8458(12) 0.102(13) Uiso 1 1 d . . . H283 H 0.5869 0.6855 0.8384 0.122 Uiso 1 1 calc R . . C285 C 0.823(4) 0.652(3) 0.8350(15) 0.132(17) Uiso 1 1 d . . . H285 H 0.8794 0.6690 0.8197 0.158 Uiso 1 1 calc R . . C284 C 0.735(4) 0.673(3) 0.8225(13) 0.108(14) Uiso 1 1 d . . . C286 C 0.842(4) 0.605(2) 0.8705(12) 0.105(13) Uiso 1 1 d . . . H286 H 0.9033 0.5788 0.8760 0.126 Uiso 1 1 calc R . . Br28 Br 0.7222(5) 0.7203(3) 0.77049(12) 0.129(2) Uani 1 1 d . . . O31 O 0.6158(17) 0.5080(12) 1.1633(6) 0.070(6) Uani 1 1 d . . . C31 C 0.585(3) 0.581(2) 1.1536(10) 0.082(10) Uiso 1 1 d . . . C311 C 0.469(3) 0.577(2) 1.1550(11) 0.089(11) Uiso 1 1 d . . . C312 C 0.417(3) 0.646(2) 1.1427(11) 0.093(11) Uiso 1 1 d . . . H312 H 0.4555 0.6893 1.1332 0.111 Uiso 1 1 calc R . . C313 C 0.319(3) 0.653(3) 1.1438(11) 0.097(12) Uiso 1 1 d . . . H313 H 0.2882 0.6982 1.1327 0.117 Uiso 1 1 calc R . . C314 C 0.261(4) 0.594(3) 1.1611(15) 0.129(16) Uiso 1 1 d . . . C315 C 0.314(5) 0.536(4) 1.1828(17) 0.17(2) Uiso 1 1 d . . . H315 H 0.2801 0.4953 1.1970 0.208 Uiso 1 1 calc R . . C316 C 0.424(5) 0.540(3) 1.1824(15) 0.141(18) Uiso 1 1 d . . . H316 H 0.4608 0.5145 1.2031 0.170 Uiso 1 1 calc R . . Br31 Br 0.1271(4) 0.5951(3) 1.1625(2) 0.146(2) Uani 1 1 d . . . C32 C 0.641(3) 0.631(2) 1.1363(10) 0.089(11) Uiso 1 1 d . . . H32 H 0.6087 0.6775 1.1272 0.107 Uiso 1 1 calc R . . C33 C 0.747(3) 0.6278(18) 1.1285(9) 0.060(8) Uiso 1 1 d . . . O33 O 0.7870(18) 0.5610(14) 1.1307(5) 0.086(8) Uani 1 1 d . . . C34 C 0.803(2) 0.6921(16) 1.1154(7) 0.052(7) Uiso 1 1 d . . . H34 H 0.8725 0.6889 1.1267 0.063 Uiso 1 1 calc R . . O34 O 0.760(2) 0.7652(12) 1.1255(8) 0.095(8) Uani 1 1 d . . . C39 C 0.782(3) 0.831(2) 1.1006(11) 0.089(11) Uiso 1 1 d . . . C39B C 0.866(4) 0.877(3) 1.1142(13) 0.123(16) Uiso 1 1 d . . . H39A H 0.8421 0.9198 1.1316 0.184 Uiso 1 1 calc R . . H39B H 0.9012 0.8991 1.0908 0.184 Uiso 1 1 calc R . . H39C H 0.9117 0.8433 1.1296 0.184 Uiso 1 1 calc R . . C39A C 0.695(4) 0.860(3) 1.0842(14) 0.131(17) Uiso 1 1 d . . . H39D H 0.6411 0.8218 1.0878 0.197 Uiso 1 1 calc R . . H39E H 0.7045 0.8705 1.0553 0.197 Uiso 1 1 calc R . . H39F H 0.6766 0.9095 1.0979 0.197 Uiso 1 1 calc R . . O35 O 0.831(2) 0.7841(14) 1.0653(8) 0.101(8) Uani 1 1 d . . . C35 C 0.808(3) 0.6994(18) 1.0695(8) 0.063(8) Uiso 1 1 d . . . H35 H 0.7403 0.6888 1.0581 0.076 Uiso 1 1 calc R . . C36 C 0.882(3) 0.658(2) 1.0457(10) 0.082(11) Uiso 1 1 d . . . O36 O 0.8432(15) 0.5914(11) 1.0297(6) 0.067(6) Uani 1 1 d . . . C37 C 0.982(3) 0.671(2) 1.0487(11) 0.091(11) Uiso 1 1 d . . . H37 H 1.0053 0.7079 1.0682 0.110 Uiso 1 1 calc R . . C38 C 1.051(3) 0.632(2) 1.0240(11) 0.082(11) Uiso 1 1 d . . . O38 O 1.0331(18) 0.5754(13) 1.0012(7) 0.084(7) Uani 1 1 d . . . C381 C 1.165(3) 0.6519(18) 1.0285(8) 0.059(8) Uiso 1 1 d . . . C382 C 1.190(3) 0.731(2) 1.0349(9) 0.078(10) Uiso 1 1 d . . . H382 H 1.1427 0.7718 1.0380 0.093 Uiso 1 1 calc R . . C383 C 1.300(3) 0.742(2) 1.0361(9) 0.076(10) Uiso 1 1 d . . . H383 H 1.3279 0.7934 1.0371 0.091 Uiso 1 1 calc R . . C384 C 1.361(3) 0.677(2) 1.0359(10) 0.080(10) Uiso 1 1 d . . . C385 C 1.332(4) 0.603(3) 1.0320(11) 0.105(13) Uiso 1 1 d . . . H385 H 1.3786 0.5612 1.0303 0.126 Uiso 1 1 calc R . . C386 C 1.226(3) 0.589(2) 1.0303(9) 0.073(9) Uiso 1 1 d . . . H386 H 1.2000 0.5374 1.0305 0.088 Uiso 1 1 calc R . . Br38 Br 1.5014(4) 0.6952(3) 1.03781(13) 0.1126(16) Uani 1 1 d . . . 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 Fe1 0.072(4) 0.088(3) 0.061(3) -0.002(2) -0.007(2) 0.006(3) Fe2 0.063(4) 0.091(4) 0.080(4) -0.001(3) -0.003(3) 0.001(3) O11 0.062(16) 0.048(11) 0.073(13) -0.008(9) 0.022(11) -0.011(11) Br11 0.119(4) 0.136(4) 0.058(2) -0.006(2) -0.004(2) -0.009(3) O13 0.074(19) 0.089(17) 0.085(17) 0.003(12) 0.024(13) 0.020(15) O14 0.08(2) 0.16(2) 0.055(14) 0.004(14) -0.012(13) 0.008(19) O15 0.059(18) 0.15(3) 0.101(19) 0.026(16) 0.019(14) 0.015(18) O16 0.058(18) 0.23(3) 0.044(13) 0.014(15) 0.000(10) -0.01(2) O18 0.078(18) 0.070(14) 0.091(16) -0.002(11) -0.014(13) 0.038(14) Br18 0.094(3) 0.118(3) 0.077(2) -0.012(2) 0.014(2) -0.004(3) O21 0.092(19) 0.054(12) 0.063(13) -0.004(9) -0.023(12) 0.009(13) Br21 0.143(6) 0.164(6) 0.234(7) 0.077(5) -0.021(5) -0.055(5) O23 0.09(2) 0.062(13) 0.077(14) 0.021(10) 0.023(13) -0.003(14) O24 0.046(16) 0.13(2) 0.066(14) -0.002(13) -0.004(10) 0.008(14) O25 0.060(17) 0.25(3) 0.025(10) -0.009(14) -0.001(10) -0.01(2) O26 0.072(18) 0.18(2) 0.020(10) 0.010(12) 0.006(9) 0.015(18) O28 0.084(19) 0.13(2) 0.032(11) -0.010(11) -0.002(10) -0.044(17) Br28 0.165(5) 0.154(5) 0.068(3) 0.023(3) -0.005(3) 0.007(4) O31 0.073(17) 0.067(13) 0.071(14) -0.009(10) -0.003(11) 0.017(12) Br31 0.077(4) 0.122(4) 0.239(7) -0.024(4) 0.013(4) 0.001(3) O33 0.11(2) 0.121(19) 0.027(10) -0.024(10) -0.029(10) 0.053(17) O34 0.09(2) 0.046(12) 0.14(2) -0.023(12) 0.015(16) 0.017(14) O35 0.09(2) 0.077(17) 0.13(2) 0.017(15) -0.004(16) 0.016(17) O36 0.043(14) 0.045(11) 0.113(17) 0.008(11) -0.007(12) 0.004(11) O38 0.066(18) 0.082(16) 0.105(18) -0.012(13) 0.007(13) 0.016(14) Br38 0.073(3) 0.145(4) 0.120(3) 0.017(3) -0.007(3) -0.013(3) _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 Fe1 O11 1.93(2) . ? Fe1 O33 1.93(3) . ? Fe1 O21 1.94(2) . ? Fe1 O23 1.96(2) . ? Fe1 O13 2.00(2) . ? Fe1 O31 2.02(2) . ? Fe2 O16 1.94(3) . ? Fe2 O28 1.95(2) . ? Fe2 O36 1.98(2) . ? Fe2 O26 1.98(3) . ? Fe2 O38 1.99(3) . ? Fe2 O18 2.00(2) . ? O11 C11 1.25(4) . ? C11 C12 1.40(4) . ? C11 C111 1.48(4) . ? C111 C112 1.40(6) . ? C111 C116 1.41(5) . ? C112 C113 1.47(5) . ? C113 C114 1.39(5) . ? C114 C115 1.41(5) . ? C114 Br11 1.82(3) . ? C115 C116 1.47(5) . ? C12 C13 1.36(4) . ? C13 O13 1.30(4) . ? C13 C14 1.58(5) . ? C14 O14 1.45(4) . ? C14 C15 1.66(4) . ? O14 C19 1.43(4) . ? C19 O15 1.43(4) . ? C19 C19A 1.50(5) . ? C19 C19B 1.51(5) . ? O15 C15 1.50(4) . ? C15 C16 1.49(4) . ? C16 O16 1.23(4) . ? C16 C17 1.41(5) . ? C17 C18 1.38(4) . ? C18 O18 1.22(4) . ? C18 C181 1.56(5) . ? C181 C182 1.29(4) . ? C181 C186 1.45(4) . ? C182 C183 1.42(4) . ? C183 C184 1.33(4) . ? C184 C185 1.31(4) . ? C184 Br18 1.92(3) . ? C185 C186 1.43(4) . ? O21 C21 1.34(4) . ? C21 C22 1.32(4) . ? C21 C211 1.52(5) . ? C211 C212 1.35(5) . ? C211 C216 1.40(4) . ? C212 C213 1.45(5) . ? C213 C214 1.42(5) . ? C214 C215 1.23(6) . ? C214 Br21 1.90(5) . ? C215 C216 1.50(6) . ? C22 C23 1.48(5) . ? C23 O23 1.28(4) . ? C23 C24 1.49(4) . ? C24 O24 1.38(4) . ? C24 C25 1.54(4) . ? O24 C29 1.42(4) . ? C29 C29B 1.44(4) . ? C29 O25 1.44(4) . ? C29 C29A 1.56(5) . ? O25 C25 1.44(4) . ? C25 C26 1.52(5) . ? C26 O26 1.27(4) . ? C26 C27 1.46(4) . ? C27 C28 1.38(5) . ? C28 O28 1.21(4) . ? C28 C281 1.55(5) . ? C281 C282 1.34(5) . ? C281 C286 1.44(5) . ? C282 C283 1.43(5) . ? C283 C284 1.38(6) . ? C285 C284 1.29(6) . ? C285 C286 1.44(6) . ? C284 Br28 1.91(4) . ? O31 C31 1.34(4) . ? C31 C32 1.27(5) . ? C31 C311 1.56(5) . ? C311 C316 1.26(6) . ? C311 C312 1.41(5) . ? C312 C313 1.31(5) . ? C313 C314 1.39(6) . ? C314 C315 1.41(7) . ? C314 Br31 1.79(5) . ? C315 C316 1.46(7) . ? C32 C33 1.44(5) . ? C33 O33 1.26(3) . ? C33 C34 1.39(4) . ? C34 O34 1.41(3) . ? C34 C35 1.52(3) . ? O34 C39 1.43(4) . ? C39 C39A 1.38(6) . ? C39 C39B 1.43(5) . ? C39 O35 1.56(4) . ? O35 C35 1.48(4) . ? C35 C36 1.44(4) . ? C36 O36 1.35(4) . ? C36 C37 1.35(5) . ? C37 C38 1.41(5) . ? C38 O38 1.24(4) . ? C38 C381 1.56(5) . ? C381 C386 1.34(4) . ? C381 C382 1.40(4) . ? C382 C383 1.48(5) . ? C383 C384 1.36(4) . ? C384 C385 1.33(5) . ? C384 Br38 1.90(4) . ? C385 C386 1.43(5) . ? 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 O11 Fe1 O33 92.4(8) . . ? O11 Fe1 O21 92.0(8) . . ? O33 Fe1 O21 167.8(10) . . ? O11 Fe1 O23 176.3(10) . . ? O33 Fe1 O23 88.1(8) . . ? O21 Fe1 O23 88.2(9) . . ? O11 Fe1 O13 88.7(9) . . ? O33 Fe1 O13 98.8(10) . . ? O21 Fe1 O13 92.7(10) . . ? O23 Fe1 O13 87.6(10) . . ? O11 Fe1 O31 91.2(8) . . ? O33 Fe1 O31 85.6(9) . . ? O21 Fe1 O31 83.0(9) . . ? O23 Fe1 O31 92.5(9) . . ? O13 Fe1 O31 175.6(10) . . ? O16 Fe2 O28 171.7(13) . . ? O16 Fe2 O36 95.2(11) . . ? O28 Fe2 O36 91.6(10) . . ? O16 Fe2 O26 89.7(10) . . ? O28 Fe2 O26 85.8(9) . . ? O36 Fe2 O26 88.1(10) . . ? O16 Fe2 O38 87.4(11) . . ? O28 Fe2 O38 97.8(10) . . ? O36 Fe2 O38 86.5(9) . . ? O26 Fe2 O38 173.6(9) . . ? O16 Fe2 O18 87.3(11) . . ? O28 Fe2 O18 86.4(10) . . ? O36 Fe2 O18 173.1(10) . . ? O26 Fe2 O18 98.3(10) . . ? O38 Fe2 O18 87.2(10) . . ? C11 O11 Fe1 128.6(19) . . ? O11 C11 C12 127(3) . . ? O11 C11 C111 114(3) . . ? C12 C11 C111 119(3) . . ? C112 C111 C116 116(4) . . ? C112 C111 C11 119(4) . . ? C116 C111 C11 123(3) . . ? C111 C112 C113 124(5) . . ? C114 C113 C112 117(4) . . ? C113 C114 C115 122(4) . . ? C113 C114 Br11 119(3) . . ? C115 C114 Br11 118(3) . . ? C114 C115 C116 118(4) . . ? C111 C116 C115 121(4) . . ? C13 C12 C11 119(3) . . ? O13 C13 C12 130(3) . . ? O13 C13 C14 107(3) . . ? C12 C13 C14 122(3) . . ? C13 O13 Fe1 123(2) . . ? O14 C14 C13 106(3) . . ? O14 C14 C15 105(3) . . ? C13 C14 C15 105(3) . . ? C19 O14 C14 104(2) . . ? O14 C19 O15 110(3) . . ? O14 C19 C19A 114(3) . . ? O15 C19 C19A 111(3) . . ? O14 C19 C19B 108(3) . . ? O15 C19 C19B 106(3) . . ? C19A C19 C19B 108(4) . . ? C19 O15 C15 111(3) . . ? C16 C15 O15 112(3) . . ? C16 C15 C14 111(3) . . ? O15 C15 C14 97(2) . . ? O16 C16 C17 123(3) . . ? O16 C16 C15 114(3) . . ? C17 C16 C15 123(4) . . ? C16 O16 Fe2 126(2) . . ? C18 C17 C16 127(4) . . ? O18 C18 C17 120(3) . . ? O18 C18 C181 121(3) . . ? C17 C18 C181 119(3) . . ? C18 O18 Fe2 129(2) . . ? C182 C181 C186 125(3) . . ? C182 C181 C18 122(3) . . ? C186 C181 C18 112(3) . . ? C181 C182 C183 118(3) . . ? C184 C183 C182 118(4) . . ? C185 C184 C183 125(3) . . ? C185 C184 Br18 116(2) . . ? C183 C184 Br18 118(3) . . ? C184 C185 C186 119(3) . . ? C185 C186 C181 113(3) . . ? C21 O21 Fe1 124(2) . . ? C22 C21 O21 129(4) . . ? C22 C21 C211 121(3) . . ? O21 C21 C211 110(3) . . ? C212 C211 C216 123(3) . . ? C212 C211 C21 121(3) . . ? C216 C211 C21 116(3) . . ? C211 C212 C213 121(4) . . ? C214 C213 C212 114(4) . . ? C215 C214 C213 123(5) . . ? C215 C214 Br21 120(4) . . ? C213 C214 Br21 116(4) . . ? C214 C215 C216 125(5) . . ? C211 C216 C215 111(4) . . ? C21 C22 C23 120(4) . . ? O23 C23 C22 122(3) . . ? O23 C23 C24 117(3) . . ? C22 C23 C24 117(3) . . ? C23 O23 Fe1 125(2) . . ? O24 C24 C23 114(3) . . ? O24 C24 C25 102(3) . . ? C23 C24 C25 114(3) . . ? C24 O24 C29 114(2) . . ? O24 C29 C29B 115(3) . . ? O24 C29 O25 103(3) . . ? C29B C29 O25 110(3) . . ? O24 C29 C29A 110(3) . . ? C29B C29 C29A 109(3) . . ? O25 C29 C29A 110(3) . . ? C25 O25 C29 106(2) . . ? O25 C25 C26 105(3) . . ? O25 C25 C24 102(3) . . ? C26 C25 C24 114(3) . . ? O26 C26 C27 122(3) . . ? O26 C26 C25 114(3) . . ? C27 C26 C25 124(3) . . ? C26 O26 Fe2 130(2) . . ? C28 C27 C26 121(4) . . ? O28 C28 C27 125(3) . . ? O28 C28 C281 117(4) . . ? C27 C28 C281 118(4) . . ? C28 O28 Fe2 131(2) . . ? C282 C281 C286 121(4) . . ? C282 C281 C28 123(4) . . ? C286 C281 C28 112(4) . . ? C281 C282 C283 122(4) . . ? C284 C283 C282 114(4) . . ? C284 C285 C286 125(5) . . ? C285 C284 C283 123(5) . . ? C285 C284 Br28 119(4) . . ? C283 C284 Br28 118(4) . . ? C281 C286 C285 111(5) . . ? C31 O31 Fe1 125(2) . . ? C32 C31 O31 123(4) . . ? C32 C31 C311 129(4) . . ? O31 C31 C311 105(3) . . ? C316 C311 C312 113(5) . . ? C316 C311 C31 121(4) . . ? C312 C311 C31 116(4) . . ? C313 C312 C311 123(4) . . ? C312 C313 C314 120(5) . . ? C313 C314 C315 115(6) . . ? C313 C314 Br31 124(4) . . ? C315 C314 Br31 120(5) . . ? C314 C315 C316 118(6) . . ? C311 C316 C315 121(6) . . ? C31 C32 C33 129(4) . . ? O33 C33 C34 120(3) . . ? O33 C33 C32 116(3) . . ? C34 C33 C32 124(3) . . ? C33 O33 Fe1 136(2) . . ? C33 C34 O34 113(3) . . ? C33 C34 C35 113(2) . . ? O34 C34 C35 101(2) . . ? C34 O34 C39 118(3) . . ? C39A C39 O34 109(4) . . ? C39A C39 C39B 126(5) . . ? O34 C39 C39B 114(4) . . ? C39A C39 O35 104(3) . . ? O34 C39 O35 96(3) . . ? C39B C39 O35 101(3) . . ? C35 O35 C39 110(2) . . ? C36 C35 O35 107(3) . . ? C36 C35 C34 122(3) . . ? O35 C35 C34 101(2) . . ? O36 C36 C37 123(4) . . ? O36 C36 C35 111(3) . . ? C37 C36 C35 123(4) . . ? C36 O36 Fe2 129(2) . . ? C36 C37 C38 122(4) . . ? O38 C38 C37 126(4) . . ? O38 C38 C381 115(3) . . ? C37 C38 C381 119(3) . . ? C38 O38 Fe2 129(3) . . ? C386 C381 C382 127(3) . . ? C386 C381 C38 115(3) . . ? C382 C381 C38 117(3) . . ? C381 C382 C383 112(3) . . ? C384 C383 C382 119(3) . . ? C385 C384 C383 126(4) . . ? C385 C384 Br38 116(3) . . ? C383 C384 Br38 117(3) . . ? C384 C385 C386 116(4) . . ? C381 C386 C385 118(4) . . ? 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 O33 Fe1 O11 C11 -80(3) . . . . ? O21 Fe1 O11 C11 112(3) . . . . ? O23 Fe1 O11 C11 19(15) . . . . ? O13 Fe1 O11 C11 19(3) . . . . ? O31 Fe1 O11 C11 -165(3) . . . . ? Fe1 O11 C11 C12 -18(5) . . . . ? Fe1 O11 C11 C111 163(2) . . . . ? O11 C11 C111 C112 -1(5) . . . . ? C12 C11 C111 C112 -180(4) . . . . ? O11 C11 C111 C116 -167(3) . . . . ? C12 C11 C111 C116 14(5) . . . . ? C116 C111 C112 C113 -10(7) . . . . ? C11 C111 C112 C113 -177(4) . . . . ? C111 C112 C113 C114 7(7) . . . . ? C112 C113 C114 C115 -9(6) . . . . ? C112 C113 C114 Br11 -174(3) . . . . ? C113 C114 C115 C116 13(6) . . . . ? Br11 C114 C115 C116 178(3) . . . . ? C112 C111 C116 C115 14(6) . . . . ? C11 C111 C116 C115 -180(3) . . . . ? C114 C115 C116 C111 -16(6) . . . . ? O11 C11 C12 C13 5(5) . . . . ? C111 C11 C12 C13 -176(3) . . . . ? C11 C12 C13 O13 -1(5) . . . . ? C11 C12 C13 C14 -172(3) . . . . ? C12 C13 O13 Fe1 10(5) . . . . ? C14 C13 O13 Fe1 -177.9(18) . . . . ? O11 Fe1 O13 C13 -15(3) . . . . ? O33 Fe1 O13 C13 77(3) . . . . ? O21 Fe1 O13 C13 -107(3) . . . . ? O23 Fe1 O13 C13 165(3) . . . . ? O31 Fe1 O13 C13 -103(13) . . . . ? O13 C13 C14 O14 -155(3) . . . . ? C12 C13 C14 O14 17(4) . . . . ? O13 C13 C14 C15 94(3) . . . . ? C12 C13 C14 C15 -93(3) . . . . ? C13 C14 O14 C19 -146(3) . . . . ? C15 C14 O14 C19 -36(3) . . . . ? C14 O14 C19 O15 26(4) . . . . ? C14 O14 C19 C19A -99(4) . . . . ? C14 O14 C19 C19B 141(3) . . . . ? O14 C19 O15 C15 -4(4) . . . . ? C19A C19 O15 C15 123(4) . . . . ? C19B C19 O15 C15 -120(3) . . . . ? C19 O15 C15 C16 -132(3) . . . . ? C19 O15 C15 C14 -17(3) . . . . ? O14 C14 C15 C16 148(3) . . . . ? C13 C14 C15 C16 -101(3) . . . . ? O14 C14 C15 O15 32(3) . . . . ? C13 C14 C15 O15 143(3) . . . . ? O15 C15 C16 O16 180(3) . . . . ? C14 C15 C16 O16 73(4) . . . . ? O15 C15 C16 C17 0(4) . . . . ? C14 C15 C16 C17 -107(4) . . . . ? C17 C16 O16 Fe2 -24(5) . . . . ? C15 C16 O16 Fe2 157(2) . . . . ? O28 Fe2 O16 C16 69(8) . . . . ? O36 Fe2 O16 C16 -145(3) . . . . ? O26 Fe2 O16 C16 127(3) . . . . ? O38 Fe2 O16 C16 -59(3) . . . . ? O18 Fe2 O16 C16 29(3) . . . . ? O16 C16 C17 C18 3(6) . . . . ? C15 C16 C17 C18 -178(3) . . . . ? C16 C17 C18 O18 2(6) . . . . ? C16 C17 C18 C181 172(3) . . . . ? C17 C18 O18 Fe2 15(5) . . . . ? C181 C18 O18 Fe2 -155(2) . . . . ? O16 Fe2 O18 C18 -25(3) . . . . ? O28 Fe2 O18 C18 160(3) . . . . ? O36 Fe2 O18 C18 86(8) . . . . ? O26 Fe2 O18 C18 -114(3) . . . . ? O38 Fe2 O18 C18 62(3) . . . . ? O18 C18 C181 C182 -143(4) . . . . ? C17 C18 C181 C182 46(5) . . . . ? O18 C18 C181 C186 24(5) . . . . ? C17 C18 C181 C186 -147(3) . . . . ? C186 C181 C182 C183 8(6) . . . . ? C18 C181 C182 C183 173(3) . . . . ? C181 C182 C183 C184 -4(5) . . . . ? C182 C183 C184 C185 8(6) . . . . ? C182 C183 C184 Br18 177(2) . . . . ? C183 C184 C185 C186 -14(6) . . . . ? Br18 C184 C185 C186 177(2) . . . . ? C184 C185 C186 C181 14(5) . . . . ? C182 C181 C186 C185 -12(5) . . . . ? C18 C181 C186 C185 -179(3) . . . . ? O11 Fe1 O21 C21 161(3) . . . . ? O33 Fe1 O21 C21 50(5) . . . . ? O23 Fe1 O21 C21 -23(3) . . . . ? O13 Fe1 O21 C21 -110(3) . . . . ? O31 Fe1 O21 C21 70(3) . . . . ? Fe1 O21 C21 C22 13(5) . . . . ? Fe1 O21 C21 C211 -174.9(19) . . . . ? C22 C21 C211 C212 11(6) . . . . ? O21 C21 C211 C212 -162(3) . . . . ? C22 C21 C211 C216 -162(4) . . . . ? O21 C21 C211 C216 25(4) . . . . ? C216 C211 C212 C213 -14(6) . . . . ? C21 C211 C212 C213 174(4) . . . . ? C211 C212 C213 C214 12(6) . . . . ? C212 C213 C214 C215 -9(7) . . . . ? C212 C213 C214 Br21 180(3) . . . . ? C213 C214 C215 C216 7(9) . . . . ? Br21 C214 C215 C216 178(3) . . . . ? C212 C211 C216 C215 10(5) . . . . ? C21 C211 C216 C215 -177(4) . . . . ? C214 C215 C216 C211 -7(7) . . . . ? O21 C21 C22 C23 -2(6) . . . . ? C211 C21 C22 C23 -174(3) . . . . ? C21 C22 C23 O23 14(6) . . . . ? C21 C22 C23 C24 175(3) . . . . ? C22 C23 O23 Fe1 -36(5) . . . . ? C24 C23 O23 Fe1 163(2) . . . . ? O11 Fe1 O23 C23 128(13) . . . . ? O33 Fe1 O23 C23 -133(3) . . . . ? O21 Fe1 O23 C23 35(3) . . . . ? O13 Fe1 O23 C23 128(3) . . . . ? O31 Fe1 O23 C23 -48(3) . . . . ? O23 C23 C24 O24 -175(3) . . . . ? C22 C23 C24 O24 24(4) . . . . ? O23 C23 C24 C25 69(4) . . . . ? C22 C23 C24 C25 -92(4) . . . . ? C23 C24 O24 C29 -137(3) . . . . ? C25 C24 O24 C29 -14(4) . . . . ? C24 O24 C29 C29B -128(3) . . . . ? C24 O24 C29 O25 -8(4) . . . . ? C24 O24 C29 C29A 109(4) . . . . ? O24 C29 O25 C25 28(3) . . . . ? C29B C29 O25 C25 152(3) . . . . ? C29A C29 O25 C25 -89(3) . . . . ? C29 O25 C25 C26 -156(3) . . . . ? C29 O25 C25 C24 -36(3) . . . . ? O24 C24 C25 O25 30(3) . . . . ? C23 C24 C25 O25 153(3) . . . . ? O24 C24 C25 C26 143(3) . . . . ? C23 C24 C25 C26 -94(4) . . . . ? O25 C25 C26 O26 -162(3) . . . . ? C24 C25 C26 O26 87(4) . . . . ? O25 C25 C26 C27 26(4) . . . . ? C24 C25 C26 C27 -85(4) . . . . ? C27 C26 O26 Fe2 8(5) . . . . ? C25 C26 O26 Fe2 -165(2) . . . . ? O16 Fe2 O26 C26 168(3) . . . . ? O28 Fe2 O26 C26 -19(3) . . . . ? O36 Fe2 O26 C26 73(3) . . . . ? O38 Fe2 O26 C26 105(9) . . . . ? O18 Fe2 O26 C26 -105(3) . . . . ? O26 C26 C27 C28 13(5) . . . . ? C25 C26 C27 C28 -175(3) . . . . ? C26 C27 C28 O28 -12(6) . . . . ? C26 C27 C28 C281 170(3) . . . . ? C27 C28 O28 Fe2 -9(6) . . . . ? C281 C28 O28 Fe2 169(2) . . . . ? O16 Fe2 O28 C28 78(9) . . . . ? O36 Fe2 O28 C28 -67(3) . . . . ? O26 Fe2 O28 C28 21(3) . . . . ? O38 Fe2 O28 C28 -154(3) . . . . ? O18 Fe2 O28 C28 119(4) . . . . ? O28 C28 C281 C282 -172(4) . . . . ? C27 C28 C281 C282 6(6) . . . . ? O28 C28 C281 C286 32(5) . . . . ? C27 C28 C281 C286 -150(4) . . . . ? C286 C281 C282 C283 -22(7) . . . . ? C28 C281 C282 C283 -177(3) . . . . ? C281 C282 C283 C284 14(6) . . . . ? C286 C285 C284 C283 12(8) . . . . ? C286 C285 C284 Br28 -170(3) . . . . ? C282 C283 C284 C285 -9(7) . . . . ? C282 C283 C284 Br28 173(3) . . . . ? C282 C281 C286 C285 22(6) . . . . ? C28 C281 C286 C285 179(4) . . . . ? C284 C285 C286 C281 -17(7) . . . . ? O11 Fe1 O31 C31 114(3) . . . . ? O33 Fe1 O31 C31 22(2) . . . . ? O21 Fe1 O31 C31 -154(3) . . . . ? O23 Fe1 O31 C31 -66(3) . . . . ? O13 Fe1 O31 C31 -157(12) . . . . ? Fe1 O31 C31 C32 -15(5) . . . . ? Fe1 O31 C31 C311 148(2) . . . . ? C32 C31 C311 C316 -158(5) . . . . ? O31 C31 C311 C316 41(5) . . . . ? C32 C31 C311 C312 -14(6) . . . . ? O31 C31 C311 C312 -175(3) . . . . ? C316 C311 C312 C313 -30(6) . . . . ? C31 C311 C312 C313 -177(4) . . . . ? C311 C312 C313 C314 6(6) . . . . ? C312 C313 C314 C315 10(7) . . . . ? C312 C313 C314 Br31 -177(3) . . . . ? C313 C314 C315 C316 -4(8) . . . . ? Br31 C314 C315 C316 -177(4) . . . . ? C312 C311 C316 C315 36(7) . . . . ? C31 C311 C316 C315 -179(5) . . . . ? C314 C315 C316 C311 -21(8) . . . . ? O31 C31 C32 C33 -9(6) . . . . ? C311 C31 C32 C33 -168(3) . . . . ? C31 C32 C33 O33 17(6) . . . . ? C31 C32 C33 C34 -169(4) . . . . ? C34 C33 O33 Fe1 -173.0(18) . . . . ? C32 C33 O33 Fe1 1(4) . . . . ? O11 Fe1 O33 C33 -107(2) . . . . ? O21 Fe1 O33 C33 4(5) . . . . ? O23 Fe1 O33 C33 77(2) . . . . ? O13 Fe1 O33 C33 164(2) . . . . ? O31 Fe1 O33 C33 -16(2) . . . . ? O33 C33 C34 O34 -162(2) . . . . ? C32 C33 C34 O34 24(4) . . . . ? O33 C33 C34 C35 84(3) . . . . ? C32 C33 C34 C35 -90(4) . . . . ? C33 C34 O34 C39 -153(3) . . . . ? C35 C34 O34 C39 -32(4) . . . . ? C34 O34 C39 C39A 120(4) . . . . ? C34 O34 C39 C39B -93(4) . . . . ? C34 O34 C39 O35 12(4) . . . . ? C39A C39 O35 C35 -98(4) . . . . ? O34 C39 O35 C35 13(4) . . . . ? C39B C39 O35 C35 130(3) . . . . ? C39 O35 C35 C36 -160(3) . . . . ? C39 O35 C35 C34 -31(3) . . . . ? C33 C34 C35 C36 -86(4) . . . . ? O34 C34 C35 C36 153(3) . . . . ? C33 C34 C35 O35 157(3) . . . . ? O34 C34 C35 O35 35(3) . . . . ? O35 C35 C36 O36 -147(3) . . . . ? C34 C35 C36 O36 98(4) . . . . ? O35 C35 C36 C37 51(5) . . . . ? C34 C35 C36 C37 -64(5) . . . . ? C37 C36 O36 Fe2 -13(5) . . . . ? C35 C36 O36 Fe2 -175.1(19) . . . . ? O16 Fe2 O36 C36 83(3) . . . . ? O28 Fe2 O36 C36 -102(3) . . . . ? O26 Fe2 O36 C36 173(3) . . . . ? O38 Fe2 O36 C36 -4(3) . . . . ? O18 Fe2 O36 C36 -28(9) . . . . ? O36 C36 C37 C38 23(6) . . . . ? C35 C36 C37 C38 -178(3) . . . . ? C36 C37 C38 O38 -10(7) . . . . ? C36 C37 C38 C381 178(3) . . . . ? C37 C38 O38 Fe2 -12(6) . . . . ? C381 C38 O38 Fe2 160(2) . . . . ? O16 Fe2 O38 C38 -79(3) . . . . ? O28 Fe2 O38 C38 107(3) . . . . ? O36 Fe2 O38 C38 16(3) . . . . ? O26 Fe2 O38 C38 -17(11) . . . . ? O18 Fe2 O38 C38 -167(3) . . . . ? O38 C38 C381 C386 -39(4) . . . . ? C37 C38 C381 C386 134(4) . . . . ? O38 C38 C381 C382 148(3) . . . . ? C37 C38 C381 C382 -39(5) . . . . ? C386 C381 C382 C383 12(5) . . . . ? C38 C381 C382 C383 -176(3) . . . . ? C381 C382 C383 C384 -7(4) . . . . ? C382 C383 C384 C385 5(6) . . . . ? C382 C383 C384 Br38 -180(2) . . . . ? C383 C384 C385 C386 -4(6) . . . . ? Br38 C384 C385 C386 -180(2) . . . . ? C382 C381 C386 C385 -12(5) . . . . ? C38 C381 C386 C385 176(3) . . . . ? C384 C385 C386 C381 7(5) . . . . ? _diffrn_measured_fraction_theta_max 0.675 _diffrn_reflns_theta_full 26.30 _diffrn_measured_fraction_theta_full 0.675 _refine_diff_density_max 0.978 _refine_diff_density_min -0.848 _refine_diff_density_rms 0.137 data_fro2483 _database_code_CSD 215038 _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C69 H56 Br6 Ga2 O19' _chemical_formula_weight 1808.04 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' O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Ga Ga 0.2307 1.6083 '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' _symmetry_cell_setting orthorhombic _symmetry_space_group_name_H-M P212121 loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x+1/2, -y, z+1/2' '-x, y+1/2, -z+1/2' 'x+1/2, -y+1/2, -z' _cell_length_a 13.526(1) _cell_length_b 18.122(1) _cell_length_c 34.335(1) _cell_angle_alpha 90.00 _cell_angle_beta 90.00 _cell_angle_gamma 90.00 _cell_volume 8416.1(8) _cell_formula_units_Z 4 _cell_measurement_temperature 198(2) _cell_measurement_reflns_used ? _cell_measurement_theta_min ? _cell_measurement_theta_max ? _exptl_crystal_description needle _exptl_crystal_colour 'light yellow' _exptl_crystal_size_max 0.35 _exptl_crystal_size_mid 0.06 _exptl_crystal_size_min 0.03 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.427 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 3576 _exptl_absorpt_coefficient_mu 3.548 _exptl_absorpt_correction_type empirical _exptl_absorpt_correction_T_min 0.3698 _exptl_absorpt_correction_T_max 0.9010 _exptl_absorpt_process_details 'SORTAV (Blessing, 1995 & 1997)' _exptl_special_details ; ? ; _diffrn_ambient_temperature 198(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'rotating anode Nonius FR591' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'Nonius KappaCCD' _diffrn_measurement_method '\w and \f scans' _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 26673 _diffrn_reflns_av_R_equivalents 0.0820 _diffrn_reflns_av_sigmaI/netI 0.1067 _diffrn_reflns_limit_h_min -10 _diffrn_reflns_limit_h_max 14 _diffrn_reflns_limit_k_min -16 _diffrn_reflns_limit_k_max 19 _diffrn_reflns_limit_l_min -29 _diffrn_reflns_limit_l_max 36 _diffrn_reflns_theta_min 1.62 _diffrn_reflns_theta_max 22.50 _reflns_number_total 10986 _reflns_number_gt 8213 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'Collect (Nonius B.V., 1998)' _computing_cell_refinement 'Collect (Nonius B.V., 1998)' _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 'SCHAKAL (Keller, 1997)' _computing_publication_material 'SHELXL-97 (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. Hydrogen atoms at the water molecule could not be located. Remaining electron density indicates that two additional n-hexane molecules are present, which can not be located in a chemically meaningful way, therefor it was not used in the final refinement. ; _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^)+(0.1146P)^2^+14.7849P] 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 'refined as riding atoms' _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_abs_structure_details 'Flack H D (1983), Acta Cryst. A39, 876-881' _refine_ls_abs_structure_Flack 0.013(16) _refine_ls_number_reflns 10986 _refine_ls_number_parameters 871 _refine_ls_number_restraints 6 _refine_ls_R_factor_all 0.1023 _refine_ls_R_factor_gt 0.0694 _refine_ls_wR_factor_ref 0.2033 _refine_ls_wR_factor_gt 0.1845 _refine_ls_goodness_of_fit_ref 1.072 _refine_ls_restrained_S_all 1.072 _refine_ls_shift/su_max 0.000 _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 Ga1 Ga 0.94944(9) 1.02978(8) -0.01522(4) 0.0259(4) Uani 1 1 d . . . Ga2 Ga 0.74955(10) 0.94724(8) 0.11546(4) 0.0244(3) Uani 1 1 d . . . Br11 Br 1.34718(14) 0.79207(12) -0.16848(6) 0.0757(6) Uani 1 1 d . . . C12 C 1.2730(11) 0.8336(9) -0.1276(5) 0.049(4) Uani 1 1 d . . . C13 C 1.2183(10) 0.8970(10) -0.1338(4) 0.050(4) Uani 1 1 d . . . H13 H 1.2186 0.9208 -0.1585 0.061 Uiso 1 1 calc R . . C14 C 1.1629(9) 0.9251(8) -0.1030(4) 0.035(3) Uani 1 1 d . . . H14 H 1.1242 0.9682 -0.1069 0.042 Uiso 1 1 calc R . . C15 C 1.1631(8) 0.8912(7) -0.0669(4) 0.027(3) Uani 1 1 d U . . C16 C 1.2185(9) 0.8271(8) -0.0605(4) 0.032(3) Uani 1 1 d . . . H16 H 1.2185 0.8037 -0.0357 0.039 Uiso 1 1 calc R . . C17 C 1.2740(9) 0.7984(9) -0.0913(5) 0.042(4) Uani 1 1 d . . . H17 H 1.3123 0.7550 -0.0877 0.051 Uiso 1 1 calc R . . C18 C 1.0990(9) 0.9235(7) -0.0363(4) 0.031(3) Uani 1 1 d . . . O19 O 1.0243(6) 0.9595(5) -0.0467(2) 0.031(2) Uani 1 1 d . . . C20 C 1.1235(9) 0.9119(8) 0.0043(4) 0.031(3) Uani 1 1 d . . . H20 H 1.1813 0.8845 0.0105 0.037 Uiso 1 1 calc R . . C21 C 1.0655(10) 0.9393(8) 0.0348(4) 0.032(3) Uani 1 1 d . . . O22 O 0.9877(6) 0.9766(5) 0.0319(2) 0.029(2) Uani 1 1 d . . . C23 C 1.0959(9) 0.9229(8) 0.0771(4) 0.034(4) Uani 1 1 d . . . H23 H 1.0884 0.9685 0.0933 0.040 Uiso 1 1 calc R . . O24 O 1.1958(6) 0.8949(5) 0.0806(3) 0.033(2) Uani 1 1 d . . . C25 C 1.1959(10) 0.8243(9) 0.1021(4) 0.046(4) Uani 1 1 d . . . C26 C 1.2080(12) 0.7621(9) 0.0734(5) 0.059(5) Uani 1 1 d . . . H26A H 1.1545 0.7641 0.0542 0.089 Uiso 1 1 calc R . . H26B H 1.2054 0.7148 0.0872 0.089 Uiso 1 1 calc R . . H26C H 1.2718 0.7669 0.0601 0.089 Uiso 1 1 calc R . . C27 C 1.2748(10) 0.8273(9) 0.1326(4) 0.048(4) Uani 1 1 d . . . H27A H 1.3399 0.8284 0.1201 0.072 Uiso 1 1 calc R . . H27B H 1.2700 0.7836 0.1494 0.072 Uiso 1 1 calc R . . H27C H 1.2662 0.8719 0.1484 0.072 Uiso 1 1 calc R . . O28 O 1.1005(6) 0.8223(5) 0.1201(3) 0.041(2) Uani 1 1 d . . . C29 C 1.0327(9) 0.8574(7) 0.0955(4) 0.032(3) Uani 1 1 d . . . H29 H 1.0081 0.8231 0.0749 0.038 Uiso 1 1 calc R . . C30 C 0.9461(9) 0.8899(7) 0.1194(4) 0.031(3) Uani 1 1 d . . . O31 O 0.8670(6) 0.8938(5) 0.0988(2) 0.026(2) Uani 1 1 d . . . C32 C 0.9579(9) 0.9103(8) 0.1570(3) 0.032(3) Uani 1 1 d . . . H32 H 1.0225 0.9099 0.1678 0.039 Uiso 1 1 calc R . . C33 C 0.8793(10) 0.9316(8) 0.1804(3) 0.032(3) Uani 1 1 d . . . O34 O 0.7901(6) 0.9384(5) 0.1693(2) 0.028(2) Uani 1 1 d . . . C35 C 0.8961(10) 0.9525(8) 0.2214(4) 0.036(3) Uani 1 1 d . . . C36 C 0.8177(11) 0.9747(12) 0.2428(5) 0.072(6) Uani 1 1 d . . . H36 H 0.7541 0.9771 0.2312 0.086 Uiso 1 1 calc R . . C37 C 0.8297(14) 0.9947(13) 0.2829(5) 0.091(8) Uani 1 1 d . . . H37 H 0.7731 1.0043 0.2985 0.109 Uiso 1 1 calc R . . C38 C 0.9213(13) 1.0001(9) 0.2988(4) 0.051(4) Uani 1 1 d . . . C39 C 0.9981(14) 0.9837(19) 0.2779(5) 0.138(13) Uani 1 1 d . . . H39 H 1.0622 0.9877 0.2891 0.165 Uiso 1 1 calc R . . C40 C 0.9881(11) 0.9599(15) 0.2387(5) 0.104(9) Uani 1 1 d . . . H40 H 1.0458 0.9488 0.2241 0.125 Uiso 1 1 calc R . . Br41 Br 0.93625(14) 1.03112(12) 0.35078(4) 0.0701(6) Uani 1 1 d . . . Br51 Br 0.8031(2) 1.22324(14) -0.24283(6) 0.1030(9) Uani 1 1 d . . . C52 C 0.8136(16) 1.1796(10) -0.1926(5) 0.064(5) Uani 1 1 d . . . C53 C 0.9008(14) 1.1611(8) -0.1773(4) 0.051(4) Uani 1 1 d . . . H53 H 0.9597 1.1704 -0.1915 0.062 Uiso 1 1 calc R . . C54 C 0.9061(11) 1.1284(8) -0.1410(4) 0.044(4) Uani 1 1 d . . . H54 H 0.9685 1.1137 -0.1310 0.053 Uiso 1 1 calc R . . C55 C 0.8205(9) 1.1168(8) -0.1188(4) 0.032(3) Uani 1 1 d . . . C56 C 0.7307(12) 1.1379(9) -0.1346(4) 0.058(5) Uani 1 1 d . . . H56 H 0.6716 1.1300 -0.1203 0.069 Uiso 1 1 calc R . . C57 C 0.7257(13) 1.1711(9) -0.1718(5) 0.061(5) Uani 1 1 d . . . H57 H 0.6644 1.1871 -0.1824 0.073 Uiso 1 1 calc R . . C58 C 0.8269(10) 1.0752(8) -0.0813(4) 0.030(3) Uani 1 1 d . . . O59 O 0.9118(6) 1.0781(5) -0.0646(2) 0.032(2) Uani 1 1 d . . . C60 C 0.7444(9) 1.0382(7) -0.0679(4) 0.031(3) Uani 1 1 d . . . H60 H 0.6813 1.0482 -0.0788 0.037 Uiso 1 1 calc R . . C61 C 0.7538(9) 0.9853(7) -0.0379(3) 0.026(3) Uani 1 1 d . . . O62 O 0.8300(6) 0.9697(5) -0.0181(2) 0.026(2) Uani 1 1 d . . . C63 C 0.6625(9) 0.9379(8) -0.0266(3) 0.029(3) Uani 1 1 d . . . H63 H 0.6833 0.8858 -0.0216 0.035 Uiso 1 1 calc R . . O64 O 0.5903(6) 0.9400(5) -0.0579(2) 0.030(2) Uani 1 1 d . . . C65 C 0.4975(9) 0.9234(7) -0.0390(3) 0.026(3) Uani 1 1 d . . . C66 C 0.4840(10) 0.8400(7) -0.0360(4) 0.040(4) Uani 1 1 d . . . H66A H 0.4864 0.8182 -0.0622 0.060 Uiso 1 1 calc R . . H66B H 0.4198 0.8292 -0.0241 0.060 Uiso 1 1 calc R . . H66C H 0.5369 0.8191 -0.0200 0.060 Uiso 1 1 calc R . . C67 C 0.4172(9) 0.9602(8) -0.0617(4) 0.038(4) Uani 1 1 d . . . H67A H 0.4327 1.0127 -0.0647 0.057 Uiso 1 1 calc R . . H67B H 0.3543 0.9549 -0.0477 0.057 Uiso 1 1 calc R . . H67C H 0.4118 0.9372 -0.0874 0.057 Uiso 1 1 calc R . . O68 O 0.5042(5) 0.9563(5) -0.0016(2) 0.033(2) Uani 1 1 d . . . C69 C 0.6051(8) 0.9677(7) 0.0084(3) 0.025(3) Uani 1 1 d . . . H69 H 0.6172 1.0221 0.0103 0.029 Uiso 1 1 calc R . . C70 C 0.6354(9) 0.9329(7) 0.0461(3) 0.028(3) Uani 1 1 d . . . O71 O 0.7143(5) 0.9590(5) 0.0604(2) 0.028(2) Uani 1 1 d . . . C72 C 0.5739(9) 0.8752(7) 0.0628(3) 0.029(3) Uani 1 1 d . . . H72 H 0.5138 0.8626 0.0501 0.035 Uiso 1 1 calc R . . C73 C 0.6002(9) 0.8373(7) 0.0973(4) 0.025(3) Uani 1 1 d . . . O74 O 0.6741(6) 0.8543(5) 0.1186(2) 0.029(2) Uani 1 1 d . . . C75 C 0.5398(8) 0.7765(6) 0.1106(3) 0.022(3) Uani 1 1 d . . . C76 C 0.5427(9) 0.7580(7) 0.1483(4) 0.032(3) Uani 1 1 d . . . H76 H 0.5821 0.7862 0.1657 0.038 Uiso 1 1 calc R . . C77 C 0.4895(11) 0.6986(9) 0.1624(5) 0.051(4) Uani 1 1 d . . . H77 H 0.4893 0.6878 0.1895 0.062 Uiso 1 1 calc R . . C78 C 0.4369(10) 0.6554(8) 0.1371(5) 0.049(4) Uani 1 1 d . . . C79 C 0.4330(10) 0.6745(8) 0.0977(4) 0.039(4) Uani 1 1 d . . . H79 H 0.3957 0.6460 0.0797 0.047 Uiso 1 1 calc R . . C80 C 0.4840(9) 0.7353(7) 0.0858(4) 0.032(3) Uani 1 1 d . . . H80 H 0.4805 0.7495 0.0592 0.038 Uiso 1 1 calc R . . Br81 Br 0.3695(2) 0.56990(13) 0.15410(7) 0.1033(9) Uani 1 1 d . . . Br91 Br 1.53555(10) 1.19128(9) 0.03560(5) 0.0489(4) Uani 1 1 d . . . C92 C 1.3960(9) 1.1770(8) 0.0296(4) 0.036(4) Uani 1 1 d . . . C93 C 1.3315(9) 1.2342(7) 0.0377(4) 0.034(3) Uani 1 1 d . . . H93 H 1.3555 1.2808 0.0462 0.041 Uiso 1 1 calc R . . C94 C 1.2318(10) 1.2220(8) 0.0332(4) 0.036(3) Uani 1 1 d . . . H94 H 1.1861 1.2602 0.0391 0.043 Uiso 1 1 calc R . . C95 C 1.1966(9) 1.1531(7) 0.0197(4) 0.029(3) Uani 1 1 d . . . C96 C 1.2636(10) 1.0978(8) 0.0121(4) 0.039(4) Uani 1 1 d . . . H96 H 1.2410 1.0512 0.0031 0.047 Uiso 1 1 calc R . . C97 C 1.3644(9) 1.1099(9) 0.0175(4) 0.043(4) Uani 1 1 d . . . H97 H 1.4105 1.0715 0.0126 0.052 Uiso 1 1 calc R . . C98 C 1.0900(8) 1.1342(7) 0.0144(4) 0.029(3) Uani 1 1 d . . . O99 O 1.0696(5) 1.0882(5) -0.0119(2) 0.0240(19) Uani 1 1 d . . . C100 C 1.0185(9) 1.1686(7) 0.0379(4) 0.032(3) Uani 1 1 d . . . H100 H 1.0400 1.2053 0.0558 0.038 Uiso 1 1 calc R . . C101 C 0.9186(9) 1.1522(7) 0.0366(4) 0.025(3) Uani 1 1 d . . . O102 O 0.8786(6) 1.1026(5) 0.0155(2) 0.026(2) Uani 1 1 d . . . C103 C 0.8469(9) 1.1960(8) 0.0621(4) 0.033(3) Uani 1 1 d . . . H103 H 0.7793 1.1945 0.0503 0.039 Uiso 1 1 calc R . . O104 O 0.8773(6) 1.2697(5) 0.0664(3) 0.038(2) Uani 1 1 d . . . C105 C 0.8432(11) 1.2960(8) 0.1024(4) 0.044(4) Uani 1 1 d . . . C106 C 0.9304(13) 1.3295(10) 0.1213(5) 0.073(6) Uani 1 1 d . . . H10A H 0.9114 1.3494 0.1467 0.109 Uiso 1 1 calc R . . H10B H 0.9560 1.3694 0.1048 0.109 Uiso 1 1 calc R . . H10C H 0.9817 1.2918 0.1247 0.109 Uiso 1 1 calc R . . C107 C 0.7503(14) 1.3461(11) 0.0959(5) 0.084(7) Uani 1 1 d . . . H10D H 0.6965 1.3164 0.0850 0.126 Uiso 1 1 calc R . . H10E H 0.7670 1.3860 0.0779 0.126 Uiso 1 1 calc R . . H10F H 0.7294 1.3671 0.1209 0.126 Uiso 1 1 calc R . . O108 O 0.8095(6) 1.2348(5) 0.1237(3) 0.035(2) Uani 1 1 d . . . C109 C 0.8417(9) 1.1695(8) 0.1044(4) 0.035(3) Uani 1 1 d . . . H109 H 0.9102 1.1577 0.1135 0.042 Uiso 1 1 calc R . . C110 C 0.7750(9) 1.1035(8) 0.1131(4) 0.029(3) Uani 1 1 d . . . O111 O 0.8184(6) 1.0421(5) 0.1122(2) 0.026(2) Uani 1 1 d . . . C112 C 0.6738(9) 1.1189(7) 0.1173(4) 0.032(3) Uani 1 1 d . . . H112 H 0.6518 1.1684 0.1146 0.039 Uiso 1 1 calc R . . C113 C 0.6046(8) 1.0637(7) 0.1253(4) 0.027(3) Uani 1 1 d . . . O114 O 0.6273(6) 0.9961(5) 0.1303(2) 0.029(2) Uani 1 1 d . . . C115 C 0.4959(9) 1.0803(8) 0.1269(4) 0.033(3) Uani 1 1 d . . . C116 C 0.4592(10) 1.1509(8) 0.1341(4) 0.044(4) Uani 1 1 d . . . H116 H 0.5029 1.1910 0.1387 0.053 Uiso 1 1 calc R . . C117 C 0.3594(10) 1.1614(9) 0.1343(5) 0.049(4) Uani 1 1 d . . . H117 H 0.3333 1.2092 0.1392 0.059 Uiso 1 1 calc R . . C118 C 0.2952(9) 1.1022(8) 0.1275(4) 0.037(4) Uani 1 1 d . . . C119 C 0.3313(9) 1.0353(8) 0.1197(5) 0.046(4) Uani 1 1 d . . . H119 H 0.2869 0.9958 0.1148 0.056 Uiso 1 1 calc R . . C120 C 0.4303(9) 1.0228(8) 0.1185(4) 0.043(4) Uani 1 1 d . . . H120 H 0.4549 0.9752 0.1120 0.052 Uiso 1 1 calc R . . Br12 Br 0.15626(10) 1.12061(10) 0.12941(6) 0.0606(5) Uani 1 1 d . . . O1 O 0.8499(8) 0.8263(6) 0.0186(3) 0.056(3) Uani 1 1 d . . . 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 Ga1 0.0195(7) 0.0277(8) 0.0304(8) -0.0008(7) -0.0023(6) -0.0010(6) Ga2 0.0200(7) 0.0267(8) 0.0264(7) 0.0016(6) -0.0031(6) -0.0009(6) Br11 0.0700(12) 0.0948(16) 0.0624(11) -0.0342(11) 0.0205(10) 0.0136(11) C12 0.038(9) 0.056(11) 0.054(10) -0.032(9) -0.012(8) -0.004(8) C13 0.039(9) 0.074(13) 0.038(9) -0.013(9) 0.003(7) 0.014(9) C14 0.019(7) 0.045(9) 0.041(9) -0.001(7) -0.003(6) 0.009(7) C15 0.014(5) 0.035(7) 0.033(6) -0.007(6) -0.008(5) -0.011(5) C16 0.025(7) 0.044(9) 0.028(7) -0.012(7) -0.004(6) 0.000(7) C17 0.018(7) 0.046(10) 0.063(11) -0.014(8) 0.003(7) -0.005(7) C18 0.025(8) 0.028(8) 0.041(9) -0.001(7) -0.004(7) -0.012(7) O19 0.028(5) 0.029(6) 0.036(5) -0.004(4) -0.006(4) -0.001(4) C20 0.022(7) 0.038(9) 0.034(8) -0.002(7) 0.004(6) 0.002(6) C21 0.032(8) 0.033(8) 0.030(7) 0.013(7) -0.001(7) -0.014(7) O22 0.013(4) 0.035(6) 0.039(5) -0.002(4) -0.004(4) 0.000(4) C23 0.017(7) 0.045(9) 0.038(8) -0.014(7) -0.020(6) 0.008(6) O24 0.021(5) 0.041(6) 0.039(5) 0.005(5) -0.015(4) 0.000(4) C25 0.036(9) 0.066(12) 0.036(9) -0.006(8) -0.008(7) 0.011(8) C26 0.047(10) 0.052(11) 0.078(12) -0.018(10) -0.020(9) 0.018(8) C27 0.038(9) 0.059(11) 0.046(9) -0.002(8) -0.024(7) 0.006(8) O28 0.028(5) 0.044(6) 0.051(6) 0.010(5) 0.011(5) 0.007(5) C29 0.027(7) 0.032(8) 0.035(8) 0.016(6) 0.000(6) 0.013(7) C30 0.022(7) 0.029(8) 0.040(8) 0.006(7) -0.003(7) 0.009(6) O31 0.020(5) 0.034(5) 0.024(5) -0.003(4) -0.008(4) 0.006(4) C32 0.015(6) 0.055(9) 0.027(8) -0.016(7) -0.004(6) 0.001(7) C33 0.035(8) 0.042(9) 0.021(7) 0.014(6) -0.011(6) -0.004(7) O34 0.025(5) 0.034(5) 0.025(4) 0.007(4) -0.008(4) -0.001(4) C35 0.035(8) 0.037(9) 0.036(8) -0.001(7) -0.003(7) 0.002(7) C36 0.034(9) 0.128(18) 0.053(11) -0.035(12) -0.014(8) 0.016(10) C37 0.048(11) 0.16(2) 0.067(13) -0.045(14) -0.014(10) 0.012(13) C38 0.063(11) 0.061(11) 0.030(8) 0.009(8) 0.001(8) -0.005(9) C39 0.038(11) 0.33(4) 0.047(12) -0.028(18) -0.017(10) -0.003(17) C40 0.025(9) 0.23(3) 0.055(12) -0.045(16) -0.018(8) 0.028(13) Br41 0.0853(13) 0.0923(15) 0.0327(8) -0.0104(9) -0.0078(9) -0.0141(12) Br51 0.148(2) 0.1101(19) 0.0509(12) 0.0438(12) -0.0129(12) -0.0193(16) C52 0.098(15) 0.050(12) 0.045(10) 0.008(9) 0.015(11) -0.014(11) C53 0.073(12) 0.032(9) 0.048(11) 0.008(8) 0.016(9) 0.001(9) C54 0.047(9) 0.035(9) 0.051(10) 0.015(8) -0.008(8) 0.007(8) C55 0.026(7) 0.040(9) 0.029(7) 0.006(7) -0.007(6) 0.001(6) C56 0.062(11) 0.065(12) 0.047(10) 0.015(9) -0.017(9) -0.015(9) C57 0.071(12) 0.056(11) 0.055(11) 0.019(9) -0.036(10) -0.022(9) C58 0.035(9) 0.036(9) 0.020(7) -0.003(6) -0.005(6) 0.007(7) O59 0.027(5) 0.030(6) 0.038(5) 0.002(4) 0.006(4) -0.004(4) C60 0.022(7) 0.029(8) 0.041(8) 0.001(7) 0.008(6) 0.002(7) C61 0.016(6) 0.035(8) 0.026(7) -0.009(6) 0.005(6) 0.002(6) O62 0.020(4) 0.027(5) 0.030(5) 0.002(4) -0.006(4) 0.001(4) C63 0.026(7) 0.036(8) 0.026(7) -0.012(6) -0.004(6) -0.014(6) O64 0.024(5) 0.048(6) 0.018(4) 0.003(4) -0.011(4) -0.006(4) C65 0.020(7) 0.039(9) 0.020(7) -0.003(6) 0.002(6) -0.004(6) C66 0.037(8) 0.033(9) 0.050(9) -0.004(7) -0.001(7) -0.005(7) C67 0.032(7) 0.048(10) 0.035(8) 0.006(7) -0.001(6) -0.014(7) O68 0.010(4) 0.054(7) 0.034(5) -0.004(5) -0.001(4) 0.004(4) C69 0.021(7) 0.028(8) 0.025(7) 0.002(6) 0.008(6) -0.004(6) C70 0.025(7) 0.034(8) 0.024(7) 0.001(6) -0.007(6) 0.008(6) O71 0.016(4) 0.042(6) 0.025(4) 0.010(4) -0.004(4) -0.005(4) C72 0.023(7) 0.040(9) 0.025(7) -0.011(7) 0.002(6) -0.007(6) C73 0.014(7) 0.025(8) 0.037(8) -0.003(6) -0.004(6) 0.010(6) O74 0.025(5) 0.024(5) 0.037(5) 0.005(4) -0.002(4) 0.001(4) C75 0.019(6) 0.020(7) 0.028(7) -0.006(6) 0.007(6) -0.009(6) C76 0.026(7) 0.030(8) 0.039(8) -0.003(7) 0.003(6) -0.008(7) C77 0.044(9) 0.053(11) 0.057(10) -0.009(9) 0.012(8) 0.008(9) C78 0.032(9) 0.033(9) 0.083(13) 0.002(9) 0.021(9) -0.017(7) C79 0.028(8) 0.036(9) 0.052(10) -0.008(8) 0.011(7) 0.008(7) C80 0.029(8) 0.020(8) 0.046(8) 0.012(7) 0.012(7) 0.002(6) Br81 0.136(2) 0.0703(15) 0.1035(18) 0.0088(13) 0.0278(15) -0.0661(15) Br91 0.0214(7) 0.0626(11) 0.0625(10) 0.0154(9) -0.0064(7) -0.0101(7) C92 0.024(7) 0.044(10) 0.039(8) 0.000(7) -0.006(6) -0.010(7) C93 0.023(7) 0.024(8) 0.055(9) -0.010(7) -0.010(7) 0.002(6) C94 0.031(8) 0.034(9) 0.044(8) -0.010(7) 0.011(7) 0.000(7) C95 0.017(7) 0.034(9) 0.034(8) 0.000(7) -0.001(6) -0.001(6) C96 0.038(9) 0.037(9) 0.043(8) -0.011(7) -0.001(7) -0.010(7) C97 0.014(7) 0.055(11) 0.060(10) 0.000(9) 0.004(7) 0.006(7) C98 0.016(7) 0.030(8) 0.040(8) 0.013(7) 0.002(6) -0.001(6) O99 0.016(4) 0.030(5) 0.026(5) -0.010(4) 0.002(4) -0.003(4) C100 0.037(9) 0.023(8) 0.035(8) -0.011(6) 0.005(7) 0.001(6) C101 0.018(7) 0.016(7) 0.042(8) 0.011(7) 0.012(6) 0.004(6) O102 0.020(4) 0.027(5) 0.032(5) 0.004(4) -0.002(4) 0.000(4) C103 0.022(7) 0.045(10) 0.031(8) -0.005(7) -0.001(6) 0.002(7) O104 0.038(5) 0.021(5) 0.053(6) -0.007(5) 0.021(5) -0.004(4) C105 0.054(10) 0.026(9) 0.053(10) -0.015(8) 0.016(8) -0.013(8) C106 0.085(13) 0.058(12) 0.076(13) 0.003(10) 0.007(11) -0.041(10) C107 0.091(15) 0.099(16) 0.063(12) -0.014(11) 0.025(11) 0.057(14) O108 0.037(5) 0.027(6) 0.042(6) -0.012(5) 0.013(4) -0.009(4) C109 0.013(7) 0.046(9) 0.047(9) -0.010(7) 0.003(6) 0.006(6) C110 0.030(8) 0.032(9) 0.024(7) -0.009(6) 0.007(6) -0.015(7) O111 0.022(4) 0.021(5) 0.035(5) -0.005(4) 0.001(4) -0.002(4) C112 0.024(7) 0.030(8) 0.043(8) -0.006(7) 0.000(6) 0.002(6) C113 0.020(7) 0.022(8) 0.038(8) -0.003(6) -0.009(6) -0.008(6) O114 0.022(5) 0.028(6) 0.036(5) 0.001(4) 0.007(4) 0.004(4) C115 0.028(7) 0.048(10) 0.024(7) 0.012(7) -0.008(6) 0.002(7) C116 0.037(8) 0.030(9) 0.065(10) -0.017(8) -0.006(8) 0.005(7) C117 0.033(9) 0.044(10) 0.071(11) -0.019(9) 0.004(8) 0.018(8) C118 0.017(7) 0.045(10) 0.050(9) -0.011(8) 0.000(7) 0.005(7) C119 0.017(7) 0.041(10) 0.081(11) -0.025(9) -0.008(7) -0.010(7) C120 0.028(8) 0.041(9) 0.060(10) -0.009(8) 0.002(7) -0.002(7) Br12 0.0229(8) 0.0723(13) 0.0867(13) -0.0068(10) 0.0001(8) 0.0074(8) O1 0.067(7) 0.041(7) 0.059(7) -0.007(6) -0.008(6) 0.000(6) _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 Ga1 O102 1.943(8) . ? Ga1 O99 1.943(8) . ? Ga1 O19 1.954(9) . ? Ga1 O22 1.953(8) . ? Ga1 O62 1.950(8) . ? Ga1 O59 1.975(9) . ? Ga2 O34 1.936(8) . ? Ga2 O31 1.947(8) . ? Ga2 O114 1.943(8) . ? Ga2 O71 1.962(8) . ? Ga2 O111 1.959(8) . ? Ga2 O74 1.971(8) . ? Br11 C12 1.881(15) . ? C12 C13 1.38(2) . ? C12 C17 1.40(2) . ? C13 C14 1.392(18) . ? C14 C15 1.384(18) . ? C15 C16 1.400(18) . ? C15 C18 1.484(18) . ? C16 C17 1.398(18) . ? C18 O19 1.256(15) . ? C18 C20 1.448(18) . ? C20 C21 1.398(18) . ? C21 O22 1.254(15) . ? C21 C23 1.540(18) . ? C23 O24 1.449(14) . ? C23 C29 1.594(19) . ? O24 C25 1.477(18) . ? C25 O28 1.431(16) . ? C25 C26 1.51(2) . ? C25 C27 1.497(18) . ? O28 C29 1.399(15) . ? C29 C30 1.546(18) . ? C30 O31 1.285(14) . ? C30 C32 1.352(18) . ? C32 C33 1.387(18) . ? C33 O34 1.271(14) . ? C33 C35 1.476(18) . ? C35 C36 1.35(2) . ? C35 C40 1.39(2) . ? C36 C37 1.43(2) . ? C37 C38 1.36(2) . ? C38 C39 1.30(2) . ? C38 Br41 1.882(15) . ? C39 C40 1.42(3) . ? Br51 C52 1.902(17) . ? C52 C53 1.33(2) . ? C52 C57 1.39(2) . ? C53 C54 1.38(2) . ? C54 C55 1.403(19) . ? C55 C56 1.38(2) . ? C55 C58 1.495(18) . ? C56 C57 1.41(2) . ? C58 O59 1.284(14) . ? C58 C60 1.382(18) . ? C60 C61 1.411(17) . ? C61 O62 1.266(14) . ? C61 C63 1.555(17) . ? C63 O64 1.452(14) . ? C63 C69 1.531(16) . ? O64 C65 1.445(14) . ? C65 O68 1.418(14) . ? C65 C67 1.493(18) . ? C65 C66 1.526(18) . ? O68 C69 1.424(14) . ? C69 C70 1.496(17) . ? C70 O71 1.267(14) . ? C70 C72 1.454(18) . ? C72 C73 1.416(18) . ? C73 O74 1.277(14) . ? C73 C75 1.446(17) . ? C75 C76 1.339(17) . ? C75 C80 1.359(17) . ? C76 C77 1.38(2) . ? C77 C78 1.37(2) . ? C78 C79 1.40(2) . ? C78 Br81 1.891(14) . ? C79 C80 1.363(19) . ? Br91 C92 1.916(13) . ? C92 C97 1.36(2) . ? C92 C93 1.383(18) . ? C93 C94 1.376(18) . ? C94 C95 1.414(19) . ? C95 C96 1.375(18) . ? C95 C98 1.493(17) . ? C96 C97 1.393(18) . ? C98 O99 1.261(15) . ? C98 C100 1.407(17) . ? C100 C101 1.384(17) . ? C101 O102 1.274(15) . ? C101 C103 1.529(17) . ? C103 O104 1.405(16) . ? C103 C109 1.532(18) . ? O104 C105 1.404(16) . ? C105 O108 1.403(16) . ? C105 C106 1.48(2) . ? C105 C107 1.57(2) . ? O108 C109 1.423(15) . ? C109 C110 1.529(18) . ? C110 O111 1.257(15) . ? C110 C112 1.404(17) . ? C112 C113 1.399(17) . ? C113 O114 1.274(14) . ? C113 C115 1.502(17) . ? C115 C116 1.395(19) . ? C115 C120 1.398(19) . ? C116 C117 1.363(19) . ? C117 C118 1.40(2) . ? C118 C119 1.334(19) . ? C118 Br12 1.909(12) . ? C119 C120 1.360(18) . ? 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 O102 Ga1 O99 90.6(3) . . ? O102 Ga1 O19 177.7(4) . . ? O99 Ga1 O19 87.3(3) . . ? O102 Ga1 O22 91.0(3) . . ? O99 Ga1 O22 90.0(3) . . ? O19 Ga1 O22 90.0(4) . . ? O102 Ga1 O62 89.9(3) . . ? O99 Ga1 O62 179.0(4) . . ? O19 Ga1 O62 92.2(3) . . ? O22 Ga1 O62 89.2(3) . . ? O102 Ga1 O59 92.1(3) . . ? O99 Ga1 O59 91.4(3) . . ? O19 Ga1 O59 87.0(4) . . ? O22 Ga1 O59 176.6(4) . . ? O62 Ga1 O59 89.4(3) . . ? O34 Ga2 O31 90.5(3) . . ? O34 Ga2 O114 91.6(3) . . ? O31 Ga2 O114 176.4(4) . . ? O34 Ga2 O71 177.2(3) . . ? O31 Ga2 O71 88.2(3) . . ? O114 Ga2 O71 89.8(3) . . ? O34 Ga2 O111 89.6(3) . . ? O31 Ga2 O111 91.8(3) . . ? O114 Ga2 O111 91.1(3) . . ? O71 Ga2 O111 88.0(3) . . ? O34 Ga2 O74 91.3(3) . . ? O31 Ga2 O74 90.8(3) . . ? O114 Ga2 O74 86.2(3) . . ? O71 Ga2 O74 91.1(4) . . ? O111 Ga2 O74 177.2(3) . . ? C13 C12 C17 121.4(14) . . ? C13 C12 Br11 120.2(13) . . ? C17 C12 Br11 118.5(12) . . ? C12 C13 C14 118.3(15) . . ? C15 C14 C13 121.1(14) . . ? C14 C15 C16 120.8(12) . . ? C14 C15 C18 117.4(12) . . ? C16 C15 C18 121.8(12) . . ? C15 C16 C17 118.4(13) . . ? C12 C17 C16 120.0(14) . . ? O19 C18 C20 122.3(12) . . ? O19 C18 C15 118.2(12) . . ? C20 C18 C15 119.5(12) . . ? C18 O19 Ga1 126.7(8) . . ? C21 C20 C18 122.7(12) . . ? O22 C21 C20 127.1(12) . . ? O22 C21 C23 113.7(11) . . ? C20 C21 C23 119.2(12) . . ? C21 O22 Ga1 123.6(8) . . ? O24 C23 C21 113.3(11) . . ? O24 C23 C29 101.9(10) . . ? C21 C23 C29 112.0(10) . . ? C23 O24 C25 110.3(10) . . ? O28 C25 O24 103.7(11) . . ? O28 C25 C26 111.2(13) . . ? O24 C25 C26 108.7(12) . . ? O28 C25 C27 110.0(12) . . ? O24 C25 C27 108.6(12) . . ? C26 C25 C27 114.1(13) . . ? C29 O28 C25 108.6(10) . . ? O28 C29 C30 110.5(10) . . ? O28 C29 C23 103.1(10) . . ? C30 C29 C23 109.5(10) . . ? O31 C30 C32 127.5(12) . . ? O31 C30 C29 111.1(11) . . ? C32 C30 C29 121.4(11) . . ? C30 O31 Ga2 123.0(8) . . ? C30 C32 C33 122.6(12) . . ? O34 C33 C32 125.6(11) . . ? O34 C33 C35 114.0(12) . . ? C32 C33 C35 120.4(11) . . ? C33 O34 Ga2 124.2(8) . . ? C36 C35 C40 116.3(14) . . ? C36 C35 C33 118.3(12) . . ? C40 C35 C33 125.0(13) . . ? C35 C36 C37 120.6(15) . . ? C38 C37 C36 120.5(17) . . ? C39 C38 C37 119.5(16) . . ? C39 C38 Br41 120.4(13) . . ? C37 C38 Br41 120.0(13) . . ? C38 C39 C40 121.1(16) . . ? C35 C40 C39 121.5(16) . . ? C53 C52 C57 121.7(16) . . ? C53 C52 Br51 121.8(14) . . ? C57 C52 Br51 116.5(15) . . ? C52 C53 C54 120.6(16) . . ? C53 C54 C55 120.8(14) . . ? C56 C55 C54 117.9(13) . . ? C56 C55 C58 121.9(12) . . ? C54 C55 C58 119.8(11) . . ? C55 C56 C57 120.9(16) . . ? C52 C57 C56 118.0(16) . . ? O59 C58 C60 126.4(12) . . ? O59 C58 C55 114.6(12) . . ? C60 C58 C55 119.0(12) . . ? C58 O59 Ga1 126.6(8) . . ? C58 C60 C61 120.0(12) . . ? O62 C61 C60 128.1(11) . . ? O62 C61 C63 113.0(11) . . ? C60 C61 C63 119.0(11) . . ? C61 O62 Ga1 125.2(8) . . ? O64 C63 C69 103.4(9) . . ? O64 C63 C61 109.6(10) . . ? C69 C63 C61 113.7(10) . . ? C65 O64 C63 104.2(8) . . ? O68 C65 O64 105.3(9) . . ? O68 C65 C67 109.3(11) . . ? O64 C65 C67 107.8(10) . . ? O68 C65 C66 111.3(10) . . ? O64 C65 C66 109.9(11) . . ? C67 C65 C66 112.9(11) . . ? C69 O68 C65 110.0(8) . . ? O68 C69 C70 114.2(10) . . ? O68 C69 C63 104.1(9) . . ? C70 C69 C63 113.0(10) . . ? O71 C70 C72 126.7(11) . . ? O71 C70 C69 114.1(11) . . ? C72 C70 C69 119.2(11) . . ? C70 O71 Ga2 122.6(8) . . ? C73 C72 C70 122.4(11) . . ? O74 C73 C72 124.0(12) . . ? O74 C73 C75 116.5(11) . . ? C72 C73 C75 119.5(11) . . ? C73 O74 Ga2 125.5(8) . . ? C76 C75 C80 119.0(12) . . ? C76 C75 C73 118.6(11) . . ? C80 C75 C73 122.3(11) . . ? C75 C76 C77 121.2(13) . . ? C78 C77 C76 119.5(15) . . ? C77 C78 C79 119.5(14) . . ? C77 C78 Br81 121.5(13) . . ? C79 C78 Br81 119.0(12) . . ? C80 C79 C78 118.1(14) . . ? C75 C80 C79 122.5(13) . . ? C97 C92 C93 122.4(12) . . ? C97 C92 Br91 117.7(11) . . ? C93 C92 Br91 119.9(10) . . ? C94 C93 C92 118.3(12) . . ? C93 C94 C95 120.6(12) . . ? C96 C95 C94 118.9(11) . . ? C96 C95 C98 116.5(12) . . ? C94 C95 C98 124.5(12) . . ? C95 C96 C97 120.3(13) . . ? C92 C97 C96 119.4(14) . . ? O99 C98 C100 123.7(11) . . ? O99 C98 C95 116.8(11) . . ? C100 C98 C95 119.5(12) . . ? C98 O99 Ga1 125.8(7) . . ? C101 C100 C98 123.9(12) . . ? O102 C101 C100 125.8(11) . . ? O102 C101 C103 115.0(10) . . ? C100 C101 C103 119.3(12) . . ? C101 O102 Ga1 125.3(7) . . ? O104 C103 C101 111.6(10) . . ? O104 C103 C109 102.2(10) . . ? C101 C103 C109 114.2(11) . . ? C105 O104 C103 108.6(10) . . ? O104 C105 O108 107.2(10) . . ? O104 C105 C106 105.3(12) . . ? O108 C105 C106 110.8(13) . . ? O104 C105 C107 109.6(13) . . ? O108 C105 C107 105.7(12) . . ? C106 C105 C107 117.8(14) . . ? C105 O108 C109 108.5(10) . . ? O108 C109 C110 112.3(10) . . ? O108 C109 C103 101.2(11) . . ? C110 C109 C103 117.2(11) . . ? O111 C110 C112 129.4(12) . . ? O111 C110 C109 114.3(10) . . ? C112 C110 C109 116.0(12) . . ? C110 O111 Ga2 123.5(7) . . ? C110 C112 C113 122.0(12) . . ? O114 C113 C112 123.5(11) . . ? O114 C113 C115 115.1(11) . . ? C112 C113 C115 121.3(12) . . ? C113 O114 Ga2 127.5(8) . . ? C116 C115 C120 119.7(12) . . ? C116 C115 C113 122.6(13) . . ? C120 C115 C113 117.6(13) . . ? C117 C116 C115 118.8(14) . . ? C116 C117 C118 120.4(13) . . ? C119 C118 C117 120.2(12) . . ? C119 C118 Br12 121.7(10) . . ? C117 C118 Br12 118.1(10) . . ? C118 C119 C120 121.3(13) . . ? C119 C120 C115 119.6(14) . . ? 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 C17 C12 C13 C14 -1(2) . . . . ? Br11 C12 C13 C14 178.7(10) . . . . ? C12 C13 C14 C15 1(2) . . . . ? C13 C14 C15 C16 -1(2) . . . . ? C13 C14 C15 C18 -177.9(12) . . . . ? C14 C15 C16 C17 0.2(18) . . . . ? C18 C15 C16 C17 177.4(11) . . . . ? C13 C12 C17 C16 0(2) . . . . ? Br11 C12 C17 C16 -179.0(9) . . . . ? C15 C16 C17 C12 -0.1(18) . . . . ? C14 C15 C18 O19 25.6(17) . . . . ? C16 C15 C18 O19 -151.7(11) . . . . ? C14 C15 C18 C20 -155.1(12) . . . . ? C16 C15 C18 C20 27.7(17) . . . . ? C20 C18 O19 Ga1 19.1(17) . . . . ? C15 C18 O19 Ga1 -161.6(8) . . . . ? O102 Ga1 O19 C18 86(9) . . . . ? O99 Ga1 O19 C18 61.9(10) . . . . ? O22 Ga1 O19 C18 -28.1(10) . . . . ? O62 Ga1 O19 C18 -117.3(10) . . . . ? O59 Ga1 O19 C18 153.4(10) . . . . ? O19 C18 C20 C21 1(2) . . . . ? C15 C18 C20 C21 -178.7(12) . . . . ? C18 C20 C21 O22 0(2) . . . . ? C18 C20 C21 C23 178.7(12) . . . . ? C20 C21 O22 Ga1 -18.8(18) . . . . ? C23 C21 O22 Ga1 162.0(8) . . . . ? O102 Ga1 O22 C21 -150.9(10) . . . . ? O99 Ga1 O22 C21 -60.3(10) . . . . ? O19 Ga1 O22 C21 27.0(10) . . . . ? O62 Ga1 O22 C21 119.2(10) . . . . ? O59 Ga1 O22 C21 53(6) . . . . ? O22 C21 C23 O24 -166.9(10) . . . . ? C20 C21 C23 O24 13.9(17) . . . . ? O22 C21 C23 C29 78.5(14) . . . . ? C20 C21 C23 C29 -100.7(13) . . . . ? C21 C23 O24 C25 -125.6(12) . . . . ? C29 C23 O24 C25 -5.1(12) . . . . ? C23 O24 C25 O28 -15.5(13) . . . . ? C23 O24 C25 C26 102.9(12) . . . . ? C23 O24 C25 C27 -132.4(11) . . . . ? O24 C25 O28 C29 33.0(13) . . . . ? C26 C25 O28 C29 -83.6(14) . . . . ? C27 C25 O28 C29 149.0(13) . . . . ? C25 O28 C29 C30 -152.9(11) . . . . ? C25 O28 C29 C23 -36.0(13) . . . . ? O24 C23 C29 O28 24.4(12) . . . . ? C21 C23 C29 O28 145.8(11) . . . . ? O24 C23 C29 C30 142.1(10) . . . . ? C21 C23 C29 C30 -96.6(13) . . . . ? O28 C29 C30 O31 -152.7(11) . . . . ? C23 C29 C30 O31 94.4(12) . . . . ? O28 C29 C30 C32 27.2(17) . . . . ? C23 C29 C30 C32 -85.7(14) . . . . ? C32 C30 O31 Ga2 11.2(19) . . . . ? C29 C30 O31 Ga2 -168.9(7) . . . . ? O34 Ga2 O31 C30 -23.1(10) . . . . ? O114 Ga2 O31 C30 -149(5) . . . . ? O71 Ga2 O31 C30 154.5(10) . . . . ? O111 Ga2 O31 C30 66.5(10) . . . . ? O74 Ga2 O31 C30 -114.4(9) . . . . ? O31 C30 C32 C33 7(2) . . . . ? C29 C30 C32 C33 -172.4(12) . . . . ? C30 C32 C33 O34 -4(2) . . . . ? C30 C32 C33 C35 179.3(13) . . . . ? C32 C33 O34 Ga2 -17.9(19) . . . . ? C35 C33 O34 Ga2 159.0(9) . . . . ? O31 Ga2 O34 C33 26.5(10) . . . . ? O114 Ga2 O34 C33 -156.5(10) . . . . ? O71 Ga2 O34 C33 -36(8) . . . . ? O111 Ga2 O34 C33 -65.3(10) . . . . ? O74 Ga2 O34 C33 117.3(10) . . . . ? O34 C33 C35 C36 1(2) . . . . ? C32 C33 C35 C36 178.3(16) . . . . ? O34 C33 C35 C40 -170.5(18) . . . . ? C32 C33 C35 C40 7(3) . . . . ? C40 C35 C36 C37 -8(3) . . . . ? C33 C35 C36 C37 179.2(18) . . . . ? C35 C36 C37 C38 8(4) . . . . ? C36 C37 C38 C39 -3(4) . . . . ? C36 C37 C38 Br41 176.9(17) . . . . ? C37 C38 C39 C40 0(4) . . . . ? Br41 C38 C39 C40 180(2) . . . . ? C36 C35 C40 C39 5(4) . . . . ? C33 C35 C40 C39 177(2) . . . . ? C38 C39 C40 C35 -1(5) . . . . ? C57 C52 C53 C54 4(3) . . . . ? Br51 C52 C53 C54 -179.0(12) . . . . ? C52 C53 C54 C55 -3(2) . . . . ? C53 C54 C55 C56 1(2) . . . . ? C53 C54 C55 C58 174.4(13) . . . . ? C54 C55 C56 C57 -1(2) . . . . ? C58 C55 C56 C57 -174.0(14) . . . . ? C53 C52 C57 C56 -4(3) . . . . ? Br51 C52 C57 C56 179.2(12) . . . . ? C55 C56 C57 C52 2(2) . . . . ? C56 C55 C58 O59 -160.6(14) . . . . ? C54 C55 C58 O59 26.3(18) . . . . ? C56 C55 C58 C60 19(2) . . . . ? C54 C55 C58 C60 -153.7(13) . . . . ? C60 C58 O59 Ga1 0.7(19) . . . . ? C55 C58 O59 Ga1 -179.3(8) . . . . ? O102 Ga1 O59 C58 -76.1(10) . . . . ? O99 Ga1 O59 C58 -166.8(10) . . . . ? O19 Ga1 O59 C58 105.9(10) . . . . ? O22 Ga1 O59 C58 80(6) . . . . ? O62 Ga1 O59 C58 13.7(10) . . . . ? O59 C58 C60 C61 -15(2) . . . . ? C55 C58 C60 C61 165.4(12) . . . . ? C58 C60 C61 O62 6(2) . . . . ? C58 C60 C61 C63 -172.9(11) . . . . ? C60 C61 O62 Ga1 14.9(17) . . . . ? C63 C61 O62 Ga1 -165.9(7) . . . . ? O102 Ga1 O62 C61 71.3(9) . . . . ? O99 Ga1 O62 C61 -166(59) . . . . ? O19 Ga1 O62 C61 -107.8(9) . . . . ? O22 Ga1 O62 C61 162.3(9) . . . . ? O59 Ga1 O62 C61 -20.8(9) . . . . ? O62 C61 C63 O64 -160.8(10) . . . . ? C60 C61 C63 O64 18.5(15) . . . . ? O62 C61 C63 C69 84.1(14) . . . . ? C60 C61 C63 C69 -96.6(13) . . . . ? C69 C63 O64 C65 -34.5(12) . . . . ? C61 C63 O64 C65 -156.1(10) . . . . ? C63 O64 C65 O68 34.9(12) . . . . ? C63 O64 C65 C67 151.5(11) . . . . ? C63 O64 C65 C66 -85.0(12) . . . . ? O64 C65 O68 C69 -21.2(13) . . . . ? C67 C65 O68 C69 -136.8(11) . . . . ? C66 C65 O68 C69 97.8(12) . . . . ? C65 O68 C69 C70 -124.3(11) . . . . ? C65 O68 C69 C63 -0.5(13) . . . . ? O64 C63 C69 O68 21.7(12) . . . . ? C61 C63 C69 O68 140.5(11) . . . . ? O64 C63 C69 C70 146.2(11) . . . . ? C61 C63 C69 C70 -95.0(14) . . . . ? O68 C69 C70 O71 -161.4(10) . . . . ? C63 C69 C70 O71 79.8(14) . . . . ? O68 C69 C70 C72 17.7(16) . . . . ? C63 C69 C70 C72 -101.2(12) . . . . ? C72 C70 O71 Ga2 -18.4(17) . . . . ? C69 C70 O71 Ga2 160.6(8) . . . . ? O34 Ga2 O71 C70 -179(100) . . . . ? O31 Ga2 O71 C70 118.7(10) . . . . ? O114 Ga2 O71 C70 -58.3(10) . . . . ? O111 Ga2 O71 C70 -149.4(10) . . . . ? O74 Ga2 O71 C70 27.9(10) . . . . ? O71 C70 C72 C73 -4(2) . . . . ? C69 C70 C72 C73 176.9(11) . . . . ? C70 C72 C73 O74 6.8(19) . . . . ? C70 C72 C73 C75 -175.0(11) . . . . ? C72 C73 O74 Ga2 13.9(17) . . . . ? C75 C73 O74 Ga2 -164.3(8) . . . . ? O34 Ga2 O74 C73 154.7(9) . . . . ? O31 Ga2 O74 C73 -114.8(9) . . . . ? O114 Ga2 O74 C73 63.1(10) . . . . ? O71 Ga2 O74 C73 -26.6(10) . . . . ? O111 Ga2 O74 C73 46(8) . . . . ? O74 C73 C75 C76 21.4(17) . . . . ? C72 C73 C75 C76 -156.9(12) . . . . ? O74 C73 C75 C80 -155.3(12) . . . . ? C72 C73 C75 C80 26.3(17) . . . . ? C80 C75 C76 C77 -1(2) . . . . ? C73 C75 C76 C77 -177.5(12) . . . . ? C75 C76 C77 C78 4(2) . . . . ? C76 C77 C78 C79 -4(2) . . . . ? C76 C77 C78 Br81 176.0(11) . . . . ? C77 C78 C79 C80 1(2) . . . . ? Br81 C78 C79 C80 -178.4(10) . . . . ? C76 C75 C80 C79 -1.9(19) . . . . ? C73 C75 C80 C79 174.8(12) . . . . ? C78 C79 C80 C75 1(2) . . . . ? C97 C92 C93 C94 0(2) . . . . ? Br91 C92 C93 C94 -179.9(10) . . . . ? C92 C93 C94 C95 -1(2) . . . . ? C93 C94 C95 C96 1(2) . . . . ? C93 C94 C95 C98 179.1(13) . . . . ? C94 C95 C96 C97 0(2) . . . . ? C98 C95 C96 C97 -178.0(13) . . . . ? C93 C92 C97 C96 1(2) . . . . ? Br91 C92 C97 C96 -178.8(11) . . . . ? C95 C96 C97 C92 -1(2) . . . . ? C96 C95 C98 O99 -32.3(17) . . . . ? C94 C95 C98 O99 150.0(13) . . . . ? C96 C95 C98 C100 148.7(13) . . . . ? C94 C95 C98 C100 -28.9(19) . . . . ? C100 C98 O99 Ga1 -22.0(17) . . . . ? C95 C98 O99 Ga1 159.0(8) . . . . ? O102 Ga1 O99 C98 24.6(10) . . . . ? O19 Ga1 O99 C98 -156.3(10) . . . . ? O22 Ga1 O99 C98 -66.4(10) . . . . ? O62 Ga1 O99 C98 -98(21) . . . . ? O59 Ga1 O99 C98 116.7(10) . . . . ? O99 C98 C100 C101 5(2) . . . . ? C95 C98 C100 C101 -176.6(12) . . . . ? C98 C100 C101 O102 3(2) . . . . ? C98 C100 C101 C103 -176.8(12) . . . . ? C100 C101 O102 Ga1 8.2(18) . . . . ? C103 C101 O102 Ga1 -172.1(8) . . . . ? O99 Ga1 O102 C101 -17.5(9) . . . . ? O19 Ga1 O102 C101 -42(9) . . . . ? O22 Ga1 O102 C101 72.5(9) . . . . ? O62 Ga1 O102 C101 161.7(9) . . . . ? O59 Ga1 O102 C101 -108.9(9) . . . . ? O102 C101 C103 O104 -145.8(11) . . . . ? C100 C101 C103 O104 33.9(16) . . . . ? O102 C101 C103 C109 98.9(13) . . . . ? C100 C101 C103 C109 -81.4(15) . . . . ? C101 C103 O104 C105 -151.2(11) . . . . ? C109 C103 O104 C105 -28.8(13) . . . . ? C103 O104 C105 O108 11.8(15) . . . . ? C103 O104 C105 C106 129.9(13) . . . . ? C103 O104 C105 C107 -102.5(14) . . . . ? O104 C105 O108 C109 12.2(14) . . . . ? C106 C105 O108 C109 -102.2(14) . . . . ? C107 C105 O108 C109 129.1(12) . . . . ? C105 O108 C109 C110 -154.4(12) . . . . ? C105 O108 C109 C103 -28.7(13) . . . . ? O104 C103 C109 O108 34.5(11) . . . . ? C101 C103 C109 O108 155.1(10) . . . . ? O104 C103 C109 C110 157.0(10) . . . . ? C101 C103 C109 C110 -82.4(14) . . . . ? O108 C109 C110 O111 -150.4(11) . . . . ? C103 C109 C110 O111 93.1(14) . . . . ? O108 C109 C110 C112 35.3(16) . . . . ? C103 C109 C110 C112 -81.2(14) . . . . ? C112 C110 O111 Ga2 1.5(19) . . . . ? C109 C110 O111 Ga2 -171.8(8) . . . . ? O34 Ga2 O111 C110 -102.9(9) . . . . ? O31 Ga2 O111 C110 166.6(9) . . . . ? O114 Ga2 O111 C110 -11.3(10) . . . . ? O71 Ga2 O111 C110 78.5(9) . . . . ? O74 Ga2 O111 C110 6(8) . . . . ? O111 C110 C112 C113 7(2) . . . . ? C109 C110 C112 C113 -179.9(12) . . . . ? C110 C112 C113 O114 2(2) . . . . ? C110 C112 C113 C115 -175.6(12) . . . . ? C112 C113 O114 Ga2 -17.3(18) . . . . ? C115 C113 O114 Ga2 160.0(8) . . . . ? O34 Ga2 O114 C113 109.0(10) . . . . ? O31 Ga2 O114 C113 -125(6) . . . . ? O71 Ga2 O114 C113 -68.6(10) . . . . ? O111 Ga2 O114 C113 19.4(10) . . . . ? O74 Ga2 O114 C113 -159.8(10) . . . . ? O114 C113 C115 C116 159.7(13) . . . . ? C112 C113 C115 C116 -23(2) . . . . ? O114 C113 C115 C120 -24.0(17) . . . . ? C112 C113 C115 C120 153.3(13) . . . . ? C120 C115 C116 C117 3(2) . . . . ? C113 C115 C116 C117 178.9(13) . . . . ? C115 C116 C117 C118 0(2) . . . . ? C116 C117 C118 C119 -2(2) . . . . ? C116 C117 C118 Br12 178.7(12) . . . . ? C117 C118 C119 C120 1(2) . . . . ? Br12 C118 C119 C120 -179.9(12) . . . . ? C118 C119 C120 C115 2(2) . . . . ? C116 C115 C120 C119 -4(2) . . . . ? C113 C115 C120 C119 179.8(13) . . . . ? _diffrn_measured_fraction_theta_max 0.999 _diffrn_reflns_theta_full 22.50 _diffrn_measured_fraction_theta_full 0.999 _refine_diff_density_max 1.277 _refine_diff_density_min -0.561 _refine_diff_density_rms 0.200