# Electronic Supplementary Material (ESI) for CrystEngComm # This journal is © The Royal Society of Chemistry 2014 ####################################################################### # # Cambridge Crystallographic Data Centre # CCDC # ####################################################################### # # This CIF contains data from an original supplementary publication # deposited with the CCDC, and may include chemical, crystal, # experimental, refinement, atomic coordinates, # anisotropic displacement parameters and molecular geometry data, # as required by the journal to which it was submitted. # # This CIF is provided on the understanding that it is used for bona # fide research purposes only. It may contain copyright material # of the CCDC or of third parties, and may not be copied or further # disseminated in any form, whether machine-readable or not, # except for the purpose of generating routine backup copies # on your local computer system. # # For further information on the CCDC, data deposition and # data retrieval see: # www.ccdc.cam.ac.uk # # Bona fide researchers may freely download Mercury and enCIFer # from this site to visualise CIF-encoded structures and # to carry out CIF format checking respectively. # data_(BrIO3)_EtOAc_[12-009] #TrackingRef 'Bromo_JFG_v09.cif' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety '2(C39 H21 Br3 N6 O6), C4 H8 O2' _chemical_formula_sum 'C82 H50 Br6 N12 O14' _chemical_formula_weight 1906.74 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' N N 0.0061 0.0033 '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' Br Br -0.2901 2.4595 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting Monoclinic _symmetry_space_group_name_H-M 'P 21/n' _symmetry_space_group_name_Hall '-P 2yn' loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x+1/2, y+1/2, -z+1/2' '-x, -y, -z' 'x-1/2, -y-1/2, z-1/2' _cell_length_a 10.9440(3) _cell_length_b 65.6499(13) _cell_length_c 11.2294(3) _cell_angle_alpha 90.00 _cell_angle_beta 110.447(3) _cell_angle_gamma 90.00 _cell_volume 7559.7(3) _cell_formula_units_Z 4 _cell_measurement_temperature 294(2) _cell_measurement_reflns_used 5859 _cell_measurement_theta_min 2.14 _cell_measurement_theta_max 26.95 _exptl_crystal_description Plate _exptl_crystal_colour Colourless _exptl_crystal_size_max 0.52 _exptl_crystal_size_mid 0.29 _exptl_crystal_size_min 0.08 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.675 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 3792 _exptl_absorpt_coefficient_mu 3.263 _exptl_absorpt_correction_type Analytical _exptl_absorpt_correction_T_min 0.2817 _exptl_absorpt_correction_T_max 0.7803 _exptl_absorpt_process_details '(ABSFAC, Clark and Reid, 1998)' _exptl_special_details ; ? ; _diffrn_ambient_temperature 294(1) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'Enhance (Mo) X-ray Source' _diffrn_radiation_monochromator graphite _diffrn_measurement_device 'Xcalibur, Sapphire3, Gemini Ultra' _diffrn_measurement_method '\w scans' _diffrn_standards_number 5670 _diffrn_standards_interval_time 60 _diffrn_standards_decay_% 1 _diffrn_reflns_number 32690 _diffrn_reflns_av_R_equivalents 0.0505 _diffrn_reflns_av_sigmaI/netI 0.0746 _diffrn_reflns_limit_h_min -13 _diffrn_reflns_limit_h_max 13 _diffrn_reflns_limit_k_min -83 _diffrn_reflns_limit_k_max 78 _diffrn_reflns_limit_l_min -14 _diffrn_reflns_limit_l_max 14 _diffrn_reflns_theta_min 2.15 _diffrn_reflns_theta_max 27.01 _diffrn_measured_fraction_theta_max 0.959 _diffrn_reflns_theta_full 26.00 _diffrn_measured_fraction_theta_full 1.000 _reflns_number_total 15826 _reflns_number_gt 10079 _reflns_threshold_expression I>2\s(I) _computing_data_collection ; CrysAlisPro, Agilent Technologies, Version 1.171.34.49 (release 20-01-2011 CrysAlis171 .NET) (compiled Jan 20 2011,15:58:25) ; _computing_cell_refinement ; CrysAlisPro, Agilent Technologies, Version 1.171.34.49 (release 20-01-2011 CrysAlis171 .NET) (compiled Jan 20 2011,15:58:25) ; _computing_data_reduction ; CrysAlisPro, Agilent Technologies, Version 1.171.34.49 (release 20-01-2011 CrysAlis171 .NET) (compiled Jan 20 2011,15:58:25) ; _computing_structure_solution 'SHELXS97 (Sheldrick, 2008)' _computing_structure_refinement 'SHELXL97 (Sheldrick, 2008) and SORTX (McArdle, 1995)' _computing_molecular_graphics 'PLATON (Spek, 2009)' _computing_publication_material SHELXL97 _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 'w=1/[\s^2^(Fo^2^)+(0.039P)^2^+11.5267P] 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 constr _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 15826 _refine_ls_number_parameters 1047 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.1237 _refine_ls_R_factor_gt 0.0747 _refine_ls_wR_factor_ref 0.1587 _refine_ls_wR_factor_gt 0.1398 _refine_ls_goodness_of_fit_ref 1.096 _refine_ls_restrained_S_all 1.096 _refine_ls_shift/su_max 0.000 _refine_ls_shift/su_mean 0.000 _refine_diff_density_max 0.685 _refine_diff_density_min -0.830 _refine_diff_density_rms 0.072 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 Br1A Br 0.77067(8) 0.006443(11) -0.40027(8) 0.0829(2) Uani 1 1 d . A -1 Br2A Br 1.1163(5) 0.09729(7) 0.5403(5) 0.0727(7) Uani 0.58 1 d P B -1 Br2C Br 1.0935(8) 0.09939(14) 0.5594(9) 0.121(3) Uani 0.42 1 d P B -2 Br3A Br 0.88790(11) -0.033485(12) -0.06065(10) 0.1012(3) Uani 1 1 d . . . O1A O 0.7691(4) 0.11021(7) -0.1001(4) 0.0675(12) Uani 1 1 d . . . C1A C 0.7531(6) 0.09259(9) -0.0847(5) 0.0458(13) Uani 1 1 d . . . N1A N 0.6437(4) 0.08150(7) -0.1656(4) 0.0432(10) Uani 1 1 d . . . O2A O 0.4502(5) 0.08407(8) -0.3293(4) 0.0818(15) Uani 1 1 d . . . C2A C 0.5216(6) 0.09075(9) -0.2286(5) 0.0525(15) Uani 1 1 d . . . O3A O 0.5418(4) 0.14426(6) 0.2090(4) 0.0562(10) Uani 1 1 d . . . C3A C 0.5188(5) 0.12781(8) 0.1603(5) 0.0410(12) Uani 1 1 d . . . N2A N 0.5433(4) 0.10954(6) 0.2372(4) 0.0384(10) Uani 1 1 d . . . O4A O 0.3277(4) 0.10416(6) 0.1779(4) 0.0524(10) Uani 1 1 d . . . C4A C 0.4365(5) 0.09805(8) 0.2326(5) 0.0407(12) Uani 1 1 d . . . O5A O 0.5773(4) 0.00915(6) 0.2522(4) 0.0585(10) Uani 1 1 d . . . C5A C 0.6124(5) 0.02692(8) 0.2586(5) 0.0432(12) Uani 1 1 d . . . N3A N 0.7120(4) 0.03238(6) 0.2118(4) 0.0385(9) Uani 1 1 d . . . O6A O 0.8340(4) 0.04955(6) 0.3923(4) 0.0554(10) Uani 1 1 d . . . C6A C 0.8080(5) 0.04682(8) 0.2803(5) 0.0396(12) Uani 1 1 d . . . C11 C 0.8690(5) 0.05876(7) 0.2033(5) 0.0369(11) Uani 1 1 d . . . C12 C 0.7913(5) 0.06658(7) 0.0866(4) 0.0369(11) Uani 1 1 d . . . H12 H 0.7056 0.0622 0.0492 0.044 Uiso 1 1 calc R . . C13 C 0.8416(5) 0.08105(7) 0.0255(5) 0.0396(12) Uani 1 1 d . . . C14 C 0.9708(5) 0.08655(8) 0.0787(5) 0.0472(13) Uani 1 1 d . . . H14 H 1.0049 0.0963 0.0388 0.057 Uiso 1 1 calc R . . C15 C 1.0498(5) 0.07776(9) 0.1902(6) 0.0510(14) Uani 1 1 d . . . H15 H 1.1384 0.0808 0.2222 0.061 Uiso 1 1 calc R . . C16 C 0.9978(5) 0.06454(9) 0.2542(5) 0.0479(13) Uani 1 1 d . . . H16 H 1.0501 0.0594 0.3327 0.057 Uiso 1 1 calc R . . C11A C 0.6723(6) 0.06304(8) -0.2170(5) 0.0443(13) Uani 1 1 d . A . N12A N 0.7743(5) 0.06369(7) -0.2535(5) 0.0541(12) Uani 1 1 d . . . C13A C 0.8015(7) 0.04654(10) -0.3051(6) 0.0622(17) Uani 1 1 d . A . H13A H 0.8736 0.0464 -0.3307 0.075 Uiso 1 1 calc R . . C14A C 0.7283(6) 0.02938(9) -0.3213(5) 0.0546(15) Uani 1 1 d . . . C15A C 0.6251(6) 0.02881(9) -0.2806(5) 0.0563(15) Uani 1 1 d . A . H15A H 0.5755 0.0170 -0.2890 0.068 Uiso 1 1 calc R . . C16A C 0.5958(6) 0.04612(10) -0.2266(5) 0.0543(15) Uani 1 1 d . . . H16A H 0.5261 0.0463 -0.1974 0.065 Uiso 1 1 calc R A . C21 C 0.4802(5) 0.10768(8) -0.1645(5) 0.0432(12) Uani 1 1 d . . . C22 C 0.5157(5) 0.10884(8) -0.0325(5) 0.0408(12) Uani 1 1 d . . . H22 H 0.5696 0.0990 0.0192 0.049 Uiso 1 1 calc R . . C23 C 0.4697(5) 0.12482(7) 0.0205(5) 0.0397(12) Uani 1 1 d . . . C24 C 0.3871(6) 0.13901(8) -0.0570(6) 0.0535(15) Uani 1 1 d . . . H24 H 0.3564 0.1497 -0.0209 0.064 Uiso 1 1 calc R . . C25 C 0.3496(6) 0.13764(9) -0.1861(6) 0.0576(15) Uani 1 1 d . . . H25 H 0.2920 0.1472 -0.2370 0.069 Uiso 1 1 calc R . . C26 C 0.3958(5) 0.12238(9) -0.2408(5) 0.0497(14) Uani 1 1 d . . . H26 H 0.3715 0.1217 -0.3288 0.060 Uiso 1 1 calc R . . C21A C 0.6741(5) 0.10672(8) 0.3213(5) 0.0405(12) Uani 1 1 d . B . N22A N 0.7610(4) 0.11103(7) 0.2668(4) 0.0464(11) Uani 1 1 d . . . C23A C 0.8865(6) 0.10881(9) 0.3373(6) 0.0587(16) Uani 1 1 d . B . H23A H 0.9488 0.1125 0.3024 0.070 Uiso 1 1 calc R . . C24A C 0.9275(6) 0.10136(10) 0.4578(6) 0.0611(17) Uani 1 1 d . . . C25A C 0.8374(7) 0.09759(10) 0.5140(6) 0.0646(18) Uani 1 1 d . B . H25A H 0.8640 0.0931 0.5979 0.077 Uiso 1 1 calc R . . C26A C 0.7069(6) 0.10043(9) 0.4456(5) 0.0557(15) Uani 1 1 d . . . H26A H 0.6435 0.0982 0.4819 0.067 Uiso 1 1 calc R B . C31 C 0.4615(5) 0.07724(8) 0.2921(4) 0.0384(11) Uani 1 1 d . . . C32 C 0.5341(5) 0.06280(8) 0.2557(5) 0.0387(12) Uani 1 1 d . . . H32 H 0.5758 0.0664 0.1995 0.046 Uiso 1 1 calc R . . C33 C 0.5453(5) 0.04307(8) 0.3021(5) 0.0405(12) Uani 1 1 d . . . C34 C 0.4835(5) 0.03801(9) 0.3864(5) 0.0496(14) Uani 1 1 d . . . H34 H 0.4884 0.0248 0.4170 0.060 Uiso 1 1 calc R . . C35 C 0.4144(6) 0.05256(10) 0.4252(5) 0.0588(16) Uani 1 1 d . . . H35 H 0.3754 0.0491 0.4838 0.071 Uiso 1 1 calc R . . C36 C 0.4021(5) 0.07197(9) 0.3793(5) 0.0470(13) Uani 1 1 d . . . H36 H 0.3547 0.0816 0.4059 0.056 Uiso 1 1 calc R . . C31A C 0.7515(5) 0.01745(7) 0.1400(5) 0.0412(12) Uani 1 1 d . . . N32A N 0.8733(5) 0.01124(7) 0.1886(5) 0.0540(12) Uani 1 1 d . . . C33A C 0.9125(7) -0.00310(10) 0.1258(7) 0.0666(18) Uani 1 1 d . . . H33A H 0.9993 -0.0072 0.1570 0.080 Uiso 1 1 calc R . . C34A C 0.8302(7) -0.01193(8) 0.0176(6) 0.0575(16) Uani 1 1 d . . . C35A C 0.7050(7) -0.00515(10) -0.0327(6) 0.0641(17) Uani 1 1 d . . . H35A H 0.6479 -0.0108 -0.1073 0.077 Uiso 1 1 calc R . . C36A C 0.6642(6) 0.01002(10) 0.0273(6) 0.0582(15) Uani 1 1 d . . . H36A H 0.5801 0.0152 -0.0067 0.070 Uiso 1 1 calc R . . Br1B Br 0.85606(8) 0.202218(12) -0.17027(7) 0.0757(2) Uani 1 1 d . C -1 Br2B Br 0.1157(2) 0.23004(4) 0.6301(3) 0.0793(6) Uani 0.58 1 d P D -1 Br2D Br 0.1385(7) 0.23520(10) 0.5989(6) 0.196(4) Uani 0.42 1 d P D -2 Br3B Br 0.58026(8) 0.245980(12) -0.26219(7) 0.0785(2) Uani 1 1 d . . . O1B O 0.8538(4) 0.20077(7) 0.5130(4) 0.0633(11) Uani 1 1 d . . . C1B C 0.7792(5) 0.19963(8) 0.4049(5) 0.0427(12) Uani 1 1 d . . . N1B N 0.7915(4) 0.18333(7) 0.3263(4) 0.0432(10) Uani 1 1 d . . . O2B O 0.9257(4) 0.15586(7) 0.3484(4) 0.0680(12) Uani 1 1 d . . . C2B C 0.8534(5) 0.16515(9) 0.3868(5) 0.0483(13) Uani 1 1 d . . . O3B O 0.5302(4) 0.16531(7) 0.7147(3) 0.0622(11) Uani 1 1 d . . . C3B C 0.5354(6) 0.16084(8) 0.6126(5) 0.0435(13) Uani 1 1 d . . . N2B N 0.4249(4) 0.16411(6) 0.5001(4) 0.0436(10) Uani 1 1 d . . . O4B O 0.4156(4) 0.13068(6) 0.4436(4) 0.0582(10) Uani 1 1 d . . . C4B C 0.3743(5) 0.14797(9) 0.4163(5) 0.0439(13) Uani 1 1 d . . . O5B O 0.1866(4) 0.17961(6) -0.1169(3) 0.0548(10) Uani 1 1 d . . . C5B C 0.2280(5) 0.18400(8) -0.0050(5) 0.0400(12) Uani 1 1 d . . . N3B N 0.3167(4) 0.20010(6) 0.0397(4) 0.0373(9) Uani 1 1 d . . . O6B O 0.2129(4) 0.21586(6) 0.1601(4) 0.0595(11) Uani 1 1 d . . . C6B C 0.3132(5) 0.21268(8) 0.1427(5) 0.0412(12) Uani 1 1 d . . . C41 C 0.4412(5) 0.22005(7) 0.2299(4) 0.0365(11) Uani 1 1 d . . . C42 C 0.5515(5) 0.20795(7) 0.2577(5) 0.0380(11) Uani 1 1 d . . . H42 H 0.5491 0.1961 0.2118 0.046 Uiso 1 1 calc R . . C43 C 0.6669(5) 0.21367(8) 0.3553(5) 0.0392(12) Uani 1 1 d . . . C44 C 0.6703(6) 0.23193(8) 0.4181(5) 0.0455(13) Uani 1 1 d . . . H44 H 0.7461 0.2359 0.4831 0.055 Uiso 1 1 calc R . . C45 C 0.5625(6) 0.24425(8) 0.3850(5) 0.0517(14) Uani 1 1 d . . . H45 H 0.5673 0.2567 0.4259 0.062 Uiso 1 1 calc R . . C46 C 0.4477(6) 0.23863(8) 0.2929(5) 0.0450(13) Uani 1 1 d . . . H46 H 0.3749 0.2471 0.2725 0.054 Uiso 1 1 calc R . . C11B C 0.7969(5) 0.18778(8) 0.2036(5) 0.0437(12) Uani 1 1 d . C . N12B N 0.8470(6) 0.20548(8) 0.1921(5) 0.0640(14) Uani 1 1 d . . . C13B C 0.8596(7) 0.20967(10) 0.0798(7) 0.0693(19) Uani 1 1 d . C . H13B H 0.8928 0.2223 0.0685 0.083 Uiso 1 1 calc R . . C14B C 0.8255(6) 0.19610(9) -0.0178(5) 0.0520(14) Uani 1 1 d . . . C15B C 0.7699(6) 0.17790(9) -0.0056(6) 0.0552(15) Uani 1 1 d . C . H15B H 0.7438 0.1686 -0.0725 0.066 Uiso 1 1 calc R . . C16B C 0.7537(6) 0.17364(9) 0.1070(5) 0.0508(14) Uani 1 1 d . . . H16B H 0.7146 0.1616 0.1182 0.061 Uiso 1 1 calc R C . C51 C 0.8163(5) 0.15776(8) 0.4951(5) 0.0461(13) Uani 1 1 d . . . C52 C 0.6905(5) 0.16080(8) 0.4958(5) 0.0409(12) Uani 1 1 d . . . H52 H 0.6284 0.1673 0.4276 0.049 Uiso 1 1 calc R . . C53 C 0.6578(5) 0.15419(8) 0.5980(5) 0.0418(12) Uani 1 1 d . . . C54 C 0.7502(6) 0.14422(9) 0.6973(5) 0.0558(16) Uani 1 1 d . . . H54 H 0.7293 0.1399 0.7668 0.067 Uiso 1 1 calc R . . C55 C 0.8726(7) 0.14058(10) 0.6946(6) 0.0655(18) Uani 1 1 d . . . H55 H 0.9330 0.1334 0.7605 0.079 Uiso 1 1 calc R . . C56 C 0.9065(6) 0.14758(9) 0.5934(6) 0.0558(15) Uani 1 1 d . . . H56 H 0.9901 0.1454 0.5925 0.067 Uiso 1 1 calc R . . C21B C 0.3399(6) 0.18033(8) 0.5104(5) 0.0476(13) Uani 1 1 d . D . N22B N 0.2402(5) 0.17529(9) 0.5492(5) 0.0706(15) Uani 1 1 d . . . C23B C 0.1722(7) 0.19076(12) 0.5754(7) 0.072(2) Uani 1 1 d . D . H24B H 0.1022 0.1879 0.6015 0.087 Uiso 1 1 calc R . . C24B C 0.2044(7) 0.21048(11) 0.5641(6) 0.0689(19) Uani 1 1 d . . . C25B C 0.3015(9) 0.21516(10) 0.5192(6) 0.078(2) Uani 1 1 d . D . H25B H 0.3196 0.2286 0.5058 0.094 Uiso 1 1 calc R . . C26B C 0.3732(7) 0.19932(9) 0.4938(5) 0.0557(15) Uani 1 1 d . . . H26B H 0.4424 0.2019 0.4661 0.067 Uiso 1 1 calc R D . C61 C 0.2710(5) 0.15293(8) 0.2923(5) 0.0391(12) Uani 1 1 d . . . C62 C 0.2910(5) 0.16805(8) 0.2143(5) 0.0398(12) Uani 1 1 d . . . H62 H 0.3645 0.1763 0.2435 0.048 Uiso 1 1 calc R . . C63 C 0.2009(5) 0.17078(7) 0.0925(5) 0.0376(11) Uani 1 1 d . . . C64 C 0.0880(5) 0.15900(9) 0.0518(5) 0.0474(13) Uani 1 1 d . . . H64 H 0.0268 0.1609 -0.0291 0.057 Uiso 1 1 calc R . . C65 C 0.0671(6) 0.14462(9) 0.1304(6) 0.0572(15) Uani 1 1 d . . . H65 H -0.0099 0.1371 0.1043 0.069 Uiso 1 1 calc R . . C66 C 0.1603(6) 0.14117(9) 0.2486(6) 0.0508(14) Uani 1 1 d . . . H66 H 0.1479 0.1308 0.2993 0.061 Uiso 1 1 calc R . . C31B C 0.3739(5) 0.20938(8) -0.0422(4) 0.0381(11) Uani 1 1 d . . . N32B N 0.3616(4) 0.22939(7) -0.0484(4) 0.0452(11) Uani 1 1 d . . . C33B C 0.4206(6) 0.23962(9) -0.1166(5) 0.0538(14) Uani 1 1 d . . . H33B H 0.4122 0.2537 -0.1229 0.065 Uiso 1 1 calc R . . C34B C 0.4930(5) 0.22987(9) -0.1774(5) 0.0487(14) Uani 1 1 d . . . C35B C 0.5030(5) 0.20904(9) -0.1732(5) 0.0495(14) Uani 1 1 d . . . H35B H 0.5499 0.2022 -0.2158 0.059 Uiso 1 1 calc R . . C36B C 0.4417(5) 0.19860(8) -0.1042(5) 0.0440(12) Uani 1 1 d . . . H36B H 0.4459 0.1845 -0.0993 0.053 Uiso 1 1 calc R . . C1S C 0.1995(10) 0.07936(15) -0.0931(9) 0.112(3) Uani 1 1 d . . . H1S1 H 0.1064 0.0778 -0.1258 0.168 Uiso 1 1 calc R . . H1S2 H 0.2226 0.0921 -0.1221 0.168 Uiso 1 1 calc R . . H1S3 H 0.2298 0.0793 -0.0019 0.168 Uiso 1 1 calc R . . C2S C 0.2605(12) 0.06241(16) -0.1383(9) 0.106(3) Uani 1 1 d . . . O1S O 0.3777(7) 0.05696(13) -0.0902(6) 0.122(3) Uani 1 1 d . . . O2S O 0.1832(6) 0.05283(8) -0.2349(5) 0.0887(15) Uani 1 1 d . . . C3S C 0.2345(8) 0.03773(12) -0.2984(7) 0.081(2) Uani 1 1 d . . . H3S1 H 0.2740 0.0267 -0.2405 0.097 Uiso 1 1 calc R . . H3S2 H 0.3009 0.0438 -0.3262 0.097 Uiso 1 1 calc R . . C4S C 0.1284(10) 0.02998(16) -0.4074(8) 0.114(3) Uani 1 1 d . . . H4S1 H 0.0826 0.0412 -0.4587 0.171 Uiso 1 1 calc R . . H4S2 H 0.0695 0.0223 -0.3785 0.171 Uiso 1 1 calc R . . H4S3 H 0.1630 0.0213 -0.4569 0.171 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 Br1A 0.0929(6) 0.0610(4) 0.0911(5) -0.0242(4) 0.0275(4) 0.0167(4) Br2A 0.0380(16) 0.0820(15) 0.0781(11) -0.0129(11) -0.0046(10) 0.0043(13) Br2C 0.047(3) 0.123(3) 0.150(6) -0.032(3) -0.018(3) 0.0264(18) Br3A 0.1502(9) 0.0602(5) 0.1287(7) -0.0199(5) 0.0934(7) 0.0037(5) O1A 0.072(3) 0.047(3) 0.084(3) 0.020(2) 0.028(2) -0.002(2) C1A 0.051(3) 0.043(3) 0.052(3) 0.004(3) 0.030(3) 0.002(3) N1A 0.055(3) 0.041(2) 0.036(2) 0.0024(19) 0.019(2) 0.009(2) O2A 0.098(4) 0.084(3) 0.042(2) -0.016(2) -0.002(2) 0.035(3) C2A 0.066(4) 0.057(4) 0.032(3) 0.002(3) 0.015(3) 0.009(3) O3A 0.073(3) 0.033(2) 0.060(2) -0.0152(18) 0.020(2) 0.0024(19) C3A 0.039(3) 0.032(3) 0.052(3) -0.003(2) 0.017(2) 0.005(2) N2A 0.040(2) 0.036(2) 0.039(2) -0.0067(18) 0.014(2) -0.001(2) O4A 0.039(2) 0.054(2) 0.063(2) -0.0032(19) 0.0155(19) 0.0106(19) C4A 0.039(3) 0.048(3) 0.039(3) -0.013(2) 0.017(2) -0.001(3) O5A 0.069(3) 0.036(2) 0.078(3) 0.0012(19) 0.035(2) -0.009(2) C5A 0.043(3) 0.043(3) 0.039(3) 0.005(2) 0.008(2) 0.000(3) N3A 0.039(2) 0.032(2) 0.045(2) 0.0012(18) 0.016(2) 0.0004(19) O6A 0.055(2) 0.065(3) 0.041(2) 0.0030(19) 0.0113(19) -0.007(2) C6A 0.040(3) 0.033(3) 0.046(3) 0.004(2) 0.014(2) 0.004(2) C11 0.035(3) 0.034(3) 0.041(3) -0.005(2) 0.012(2) 0.000(2) C12 0.041(3) 0.032(3) 0.039(3) -0.005(2) 0.016(2) -0.002(2) C13 0.050(3) 0.027(3) 0.047(3) -0.005(2) 0.023(3) -0.002(2) C14 0.046(3) 0.043(3) 0.060(3) -0.006(3) 0.028(3) -0.007(3) C15 0.031(3) 0.050(3) 0.070(4) -0.008(3) 0.016(3) -0.010(3) C16 0.039(3) 0.048(3) 0.053(3) -0.002(3) 0.011(3) 0.002(3) C11A 0.060(4) 0.043(3) 0.034(3) 0.003(2) 0.022(3) 0.012(3) N12A 0.069(3) 0.043(3) 0.064(3) -0.010(2) 0.041(3) -0.005(2) C13A 0.075(4) 0.062(4) 0.067(4) -0.004(3) 0.046(4) 0.008(4) C14A 0.068(4) 0.040(3) 0.052(3) -0.001(3) 0.015(3) 0.009(3) C15A 0.062(4) 0.054(4) 0.054(3) -0.007(3) 0.021(3) -0.007(3) C16A 0.052(4) 0.063(4) 0.052(3) 0.002(3) 0.023(3) -0.001(3) C21 0.045(3) 0.042(3) 0.042(3) 0.003(2) 0.015(2) 0.003(2) C22 0.049(3) 0.031(3) 0.040(3) 0.006(2) 0.012(2) 0.008(2) C23 0.043(3) 0.027(3) 0.048(3) -0.001(2) 0.016(2) 0.002(2) C24 0.065(4) 0.039(3) 0.061(4) 0.003(3) 0.027(3) 0.015(3) C25 0.059(4) 0.050(4) 0.060(4) 0.015(3) 0.016(3) 0.020(3) C26 0.051(3) 0.050(3) 0.043(3) 0.009(3) 0.010(3) 0.003(3) C21A 0.048(3) 0.032(3) 0.040(3) -0.008(2) 0.014(3) -0.005(2) N22A 0.043(3) 0.046(3) 0.051(3) -0.004(2) 0.018(2) 0.001(2) C23A 0.047(4) 0.054(4) 0.073(4) -0.012(3) 0.018(3) 0.002(3) C24A 0.048(4) 0.050(4) 0.068(4) -0.009(3) -0.002(3) -0.004(3) C25A 0.076(5) 0.051(4) 0.045(3) 0.000(3) -0.007(3) -0.015(3) C26A 0.060(4) 0.059(4) 0.043(3) -0.006(3) 0.011(3) -0.023(3) C31 0.031(3) 0.049(3) 0.034(3) -0.005(2) 0.009(2) -0.001(2) C32 0.033(3) 0.047(3) 0.038(3) -0.002(2) 0.016(2) -0.009(2) C33 0.040(3) 0.042(3) 0.042(3) 0.000(2) 0.017(2) -0.006(2) C34 0.052(3) 0.047(3) 0.047(3) 0.003(3) 0.014(3) -0.004(3) C35 0.062(4) 0.078(5) 0.048(3) 0.005(3) 0.033(3) -0.006(3) C36 0.044(3) 0.060(4) 0.039(3) -0.003(3) 0.017(2) 0.003(3) C31A 0.048(3) 0.028(3) 0.050(3) 0.003(2) 0.020(3) 0.000(2) N32A 0.051(3) 0.046(3) 0.062(3) 0.001(2) 0.017(2) 0.003(2) C33A 0.063(4) 0.059(4) 0.082(5) 0.000(4) 0.030(4) 0.016(3) C34A 0.078(5) 0.033(3) 0.072(4) -0.009(3) 0.040(4) -0.004(3) C35A 0.080(5) 0.058(4) 0.051(3) -0.016(3) 0.019(3) -0.016(4) C36A 0.058(4) 0.059(4) 0.055(4) -0.003(3) 0.016(3) 0.000(3) Br1B 0.0904(5) 0.0805(5) 0.0725(4) 0.0155(4) 0.0488(4) 0.0103(4) Br2B 0.0593(8) 0.0720(11) 0.0837(13) -0.0362(10) -0.0038(8) 0.0257(8) Br2D 0.247(6) 0.166(5) 0.140(4) -0.027(3) 0.021(3) 0.142(5) Br3B 0.0773(5) 0.0787(5) 0.0932(5) 0.0313(4) 0.0467(4) 0.0005(4) O1B 0.050(2) 0.061(3) 0.064(3) -0.016(2) 0.003(2) -0.001(2) C1B 0.036(3) 0.037(3) 0.054(3) -0.005(2) 0.015(3) -0.010(2) N1B 0.043(3) 0.039(2) 0.050(3) -0.005(2) 0.020(2) -0.001(2) O2B 0.068(3) 0.060(3) 0.091(3) 0.014(2) 0.047(3) 0.024(2) C2B 0.038(3) 0.050(3) 0.058(3) -0.001(3) 0.019(3) 0.004(3) O3B 0.079(3) 0.074(3) 0.039(2) -0.0041(19) 0.027(2) 0.004(2) C3B 0.059(4) 0.036(3) 0.037(3) 0.002(2) 0.018(3) -0.003(3) N2B 0.053(3) 0.039(2) 0.042(2) -0.0061(19) 0.021(2) -0.003(2) O4B 0.079(3) 0.035(2) 0.054(2) 0.0037(18) 0.014(2) -0.002(2) C4B 0.053(3) 0.045(3) 0.041(3) -0.002(2) 0.025(3) -0.006(3) O5B 0.054(2) 0.065(3) 0.040(2) -0.0046(19) 0.0100(18) -0.006(2) C5B 0.033(3) 0.047(3) 0.038(3) 0.001(2) 0.009(2) 0.007(2) N3B 0.041(2) 0.033(2) 0.040(2) 0.0023(18) 0.0174(19) 0.0044(19) O6B 0.047(2) 0.063(3) 0.075(3) -0.018(2) 0.029(2) 0.002(2) C6B 0.046(3) 0.037(3) 0.044(3) -0.001(2) 0.021(3) 0.007(2) C41 0.045(3) 0.029(3) 0.038(3) 0.000(2) 0.019(2) 0.002(2) C42 0.049(3) 0.028(2) 0.041(3) -0.003(2) 0.021(2) -0.003(2) C43 0.041(3) 0.039(3) 0.042(3) -0.002(2) 0.020(2) -0.003(2) C44 0.050(3) 0.038(3) 0.050(3) -0.009(2) 0.019(3) -0.012(3) C45 0.066(4) 0.034(3) 0.059(3) -0.012(3) 0.028(3) -0.006(3) C46 0.053(3) 0.034(3) 0.054(3) -0.005(2) 0.025(3) 0.001(3) C11B 0.038(3) 0.042(3) 0.056(3) 0.000(3) 0.022(3) 0.001(2) N12B 0.081(4) 0.053(3) 0.072(3) -0.010(3) 0.044(3) -0.017(3) C13B 0.090(5) 0.050(4) 0.083(5) 0.000(3) 0.049(4) -0.018(4) C14B 0.055(4) 0.055(4) 0.053(3) 0.005(3) 0.029(3) 0.008(3) C15B 0.059(4) 0.054(4) 0.052(3) -0.008(3) 0.019(3) -0.004(3) C16B 0.051(3) 0.044(3) 0.061(4) -0.003(3) 0.023(3) -0.009(3) C51 0.047(3) 0.044(3) 0.042(3) -0.006(2) 0.009(3) 0.001(3) C52 0.044(3) 0.040(3) 0.038(3) -0.002(2) 0.012(2) 0.001(2) C53 0.053(3) 0.032(3) 0.038(3) -0.002(2) 0.013(2) -0.002(2) C54 0.077(5) 0.050(4) 0.038(3) 0.001(3) 0.018(3) 0.014(3) C55 0.083(5) 0.053(4) 0.049(4) 0.005(3) 0.009(3) 0.024(4) C56 0.051(4) 0.049(3) 0.059(4) -0.003(3) 0.008(3) 0.011(3) C21B 0.061(4) 0.039(3) 0.043(3) -0.006(2) 0.018(3) -0.001(3) N22B 0.063(3) 0.076(4) 0.078(4) -0.017(3) 0.032(3) -0.007(3) C23B 0.051(4) 0.083(5) 0.089(5) -0.023(4) 0.031(4) 0.004(4) C24B 0.068(4) 0.059(5) 0.066(4) -0.014(3) 0.005(4) 0.021(4) C25B 0.117(7) 0.042(4) 0.064(4) 0.006(3) 0.018(4) 0.003(4) C26B 0.078(4) 0.046(3) 0.049(3) 0.005(3) 0.030(3) -0.003(3) C61 0.045(3) 0.035(3) 0.042(3) -0.003(2) 0.021(2) 0.002(2) C62 0.036(3) 0.041(3) 0.044(3) -0.005(2) 0.016(2) -0.006(2) C63 0.036(3) 0.034(3) 0.043(3) -0.004(2) 0.014(2) 0.004(2) C64 0.039(3) 0.049(3) 0.049(3) -0.005(3) 0.009(3) -0.002(3) C65 0.042(3) 0.057(4) 0.069(4) 0.001(3) 0.014(3) -0.012(3) C66 0.051(3) 0.046(3) 0.063(4) 0.008(3) 0.029(3) -0.006(3) C31B 0.041(3) 0.035(3) 0.036(3) 0.003(2) 0.010(2) 0.008(2) N32B 0.051(3) 0.037(2) 0.049(3) 0.006(2) 0.018(2) 0.009(2) C33B 0.065(4) 0.038(3) 0.060(4) 0.007(3) 0.024(3) 0.005(3) C34B 0.044(3) 0.051(3) 0.052(3) 0.015(3) 0.019(3) -0.005(3) C35B 0.050(3) 0.059(4) 0.044(3) 0.003(3) 0.022(3) 0.013(3) C36B 0.052(3) 0.033(3) 0.049(3) -0.001(2) 0.020(3) 0.004(2) C1S 0.134(8) 0.114(7) 0.113(7) -0.056(6) 0.073(6) -0.041(6) C2S 0.137(9) 0.121(8) 0.083(6) -0.026(6) 0.066(7) -0.042(7) O1S 0.087(4) 0.191(8) 0.099(5) -0.026(4) 0.047(4) -0.020(5) O2S 0.113(4) 0.080(4) 0.081(3) -0.011(3) 0.044(3) -0.003(3) C3S 0.088(5) 0.089(6) 0.080(5) -0.016(4) 0.046(5) 0.003(4) C4S 0.118(8) 0.132(9) 0.089(6) -0.030(6) 0.032(6) 0.024(7) _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 Br1A C14A 1.886(6) . ? Br2A C24A 1.965(8) . ? Br2C C24A 1.781(10) . ? Br3A C34A 1.887(6) . ? O1A C1A 1.192(7) . ? C1A N1A 1.424(7) . ? C1A C13 1.486(8) . ? N1A C2A 1.412(7) . ? N1A C11A 1.424(7) . ? O2A C2A 1.210(7) . ? C2A C21 1.479(8) . ? O3A C3A 1.197(6) . ? C3A N2A 1.447(7) . ? C3A C23 1.484(7) . ? N2A C4A 1.376(7) . ? N2A C21A 1.425(7) . ? O4A C4A 1.202(6) . ? C4A C31 1.504(8) . ? O5A C5A 1.223(6) . ? C5A N3A 1.412(7) . ? C5A C33 1.467(8) . ? N3A C6A 1.425(7) . ? N3A C31A 1.428(6) . ? O6A C6A 1.201(6) . ? C6A C11 1.487(7) . ? C11 C16 1.376(7) . ? C11 C12 1.388(7) . ? C12 C13 1.392(7) . ? C12 H12 0.9300 . ? C13 C14 1.378(7) . ? C14 C15 1.376(8) . ? C14 H14 0.9300 . ? C15 C16 1.371(8) . ? C15 H15 0.9300 . ? C16 H16 0.9300 . ? C11A N12A 1.317(7) . ? C11A C16A 1.372(8) . ? N12A C13A 1.346(7) . ? C13A C14A 1.357(9) . ? C13A H13A 0.9300 . ? C14A C15A 1.359(9) . ? C15A C16A 1.377(8) . ? C15A H15A 0.9300 . ? C16A H16A 0.9300 . ? C21 C22 1.397(7) . ? C21 C26 1.402(8) . ? C22 C23 1.385(7) . ? C22 H22 0.9300 . ? C23 C24 1.376(7) . ? C24 C25 1.364(8) . ? C24 H24 0.9300 . ? C25 C26 1.362(8) . ? C25 H25 0.9300 . ? C26 H26 0.9300 . ? C21A N22A 1.329(7) . ? C21A C26A 1.378(8) . ? N22A C23A 1.332(7) . ? C23A C24A 1.359(9) . ? C23A H23A 0.9300 . ? C24A C25A 1.367(10) . ? C25A C26A 1.378(9) . ? C25A H25A 0.9300 . ? C26A H26A 0.9300 . ? C31 C32 1.387(7) . ? C31 C36 1.395(7) . ? C32 C33 1.386(7) . ? C32 H32 0.9300 . ? C33 C34 1.382(7) . ? C34 C35 1.380(8) . ? C34 H34 0.9300 . ? C35 C36 1.363(9) . ? C35 H35 0.9300 . ? C36 H36 0.9300 . ? C31A N32A 1.316(7) . ? C31A C36A 1.382(8) . ? N32A C33A 1.334(8) . ? C33A C34A 1.365(9) . ? C33A H33A 0.9300 . ? C34A C35A 1.361(9) . ? C35A C36A 1.362(9) . ? C35A H35A 0.9300 . ? C36A H36A 0.9300 . ? Br1B C14B 1.898(5) . ? Br2B C24B 1.909(7) . ? Br2D C24B 1.872(9) . ? Br3B C34B 1.890(5) . ? O1B C1B 1.206(6) . ? C1B N1B 1.423(7) . ? C1B C43 1.480(8) . ? N1B C2B 1.422(7) . ? N1B C11B 1.429(7) . ? O2B C2B 1.193(6) . ? C2B C51 1.491(8) . ? O3B C3B 1.204(6) . ? C3B N2B 1.427(7) . ? C3B C53 1.471(8) . ? N2B C4B 1.396(7) . ? N2B C21B 1.445(7) . ? O4B C4B 1.221(7) . ? C4B C61 1.491(8) . ? O5B C5B 1.212(6) . ? C5B N3B 1.404(7) . ? C5B C63 1.505(7) . ? N3B C31B 1.419(6) . ? N3B C6B 1.433(6) . ? O6B C6B 1.199(6) . ? C6B C41 1.482(7) . ? C41 C42 1.387(7) . ? C41 C46 1.399(7) . ? C42 C43 1.404(7) . ? C42 H42 0.9300 . ? C43 C44 1.384(7) . ? C44 C45 1.371(8) . ? C44 H44 0.9300 . ? C45 C46 1.370(8) . ? C45 H45 0.9300 . ? C46 H46 0.9300 . ? C11B N12B 1.311(7) . ? C11B C16B 1.380(8) . ? N12B C13B 1.344(8) . ? C13B C14B 1.359(9) . ? C13B H13B 0.9300 . ? C14B C15B 1.369(8) . ? C15B C16B 1.367(8) . ? C15B H15B 0.9300 . ? C16B H16B 0.9300 . ? C51 C56 1.370(8) . ? C51 C52 1.395(8) . ? C52 C53 1.386(7) . ? C52 H52 0.9300 . ? C53 C54 1.381(8) . ? C54 C55 1.372(9) . ? C54 H54 0.9300 . ? C55 C56 1.390(9) . ? C55 H55 0.9300 . ? C56 H56 0.9300 . ? C21B C26B 1.330(8) . ? C21B N22B 1.349(8) . ? N22B C23B 1.351(9) . ? C23B C24B 1.359(10) . ? C23B H24B 0.9300 . ? C24B C25B 1.362(11) . ? C25B C26B 1.390(10) . ? C25B H25B 0.9300 . ? C26B H26B 0.9300 . ? C61 C66 1.375(8) . ? C61 C62 1.391(7) . ? C62 C63 1.390(7) . ? C62 H62 0.9300 . ? C63 C64 1.392(7) . ? C64 C65 1.365(8) . ? C64 H64 0.9300 . ? C65 C66 1.381(8) . ? C65 H65 0.9300 . ? C66 H66 0.9300 . ? C31B N32B 1.320(6) . ? C31B C36B 1.377(7) . ? N32B C33B 1.342(7) . ? C33B C34B 1.371(8) . ? C33B H33B 0.9300 . ? C34B C35B 1.371(8) . ? C35B C36B 1.373(8) . ? C35B H35B 0.9300 . ? C36B H36B 0.9300 . ? C1S C2S 1.476(13) . ? C1S H1S1 0.9600 . ? C1S H1S2 0.9600 . ? C1S H1S3 0.9600 . ? C2S O1S 1.257(12) . ? C2S O2S 1.284(10) . ? O2S C3S 1.444(8) . ? C3S C4S 1.453(11) . ? C3S H3S1 0.9700 . ? C3S H3S2 0.9700 . ? C4S H4S1 0.9600 . ? C4S H4S2 0.9600 . ? C4S H4S3 0.9600 . ? 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 O1A C1A N1A 122.5(5) . . ? O1A C1A C13 122.0(5) . . ? N1A C1A C13 115.4(4) . . ? C2A N1A C11A 117.8(4) . . ? C2A N1A C1A 122.5(5) . . ? C11A N1A C1A 116.0(4) . . ? O2A C2A N1A 120.1(5) . . ? O2A C2A C21 121.3(5) . . ? N1A C2A C21 118.5(5) . . ? O3A C3A N2A 120.6(5) . . ? O3A C3A C23 122.9(5) . . ? N2A C3A C23 116.4(4) . . ? C4A N2A C21A 126.7(4) . . ? C4A N2A C3A 117.0(4) . . ? C21A N2A C3A 115.9(4) . . ? O4A C4A N2A 120.8(5) . . ? O4A C4A C31 121.6(5) . . ? N2A C4A C31 117.5(5) . . ? O5A C5A N3A 119.2(5) . . ? O5A C5A C33 121.7(5) . . ? N3A C5A C33 118.8(5) . . ? C5A N3A C6A 119.2(4) . . ? C5A N3A C31A 117.5(4) . . ? C6A N3A C31A 116.7(4) . . ? O6A C6A N3A 121.7(5) . . ? O6A C6A C11 122.7(5) . . ? N3A C6A C11 115.6(4) . . ? C16 C11 C12 119.4(5) . . ? C16 C11 C6A 120.4(5) . . ? C12 C11 C6A 119.5(4) . . ? C11 C12 C13 120.0(5) . . ? C11 C12 H12 120.0 . . ? C13 C12 H12 120.0 . . ? C14 C13 C12 119.2(5) . . ? C14 C13 C1A 119.9(5) . . ? C12 C13 C1A 120.3(5) . . ? C15 C14 C13 120.5(5) . . ? C15 C14 H14 119.7 . . ? C13 C14 H14 119.7 . . ? C16 C15 C14 119.9(5) . . ? C16 C15 H15 120.0 . . ? C14 C15 H15 120.0 . . ? C15 C16 C11 120.6(5) . . ? C15 C16 H16 119.7 . . ? C11 C16 H16 119.7 . . ? N12A C11A C16A 124.2(5) . . ? N12A C11A N1A 115.4(5) . . ? C16A C11A N1A 120.5(5) . . ? C11A N12A C13A 116.5(5) . . ? N12A C13A C14A 122.9(6) . . ? N12A C13A H13A 118.5 . . ? C14A C13A H13A 118.5 . . ? C13A C14A C15A 119.9(5) . . ? C13A C14A Br1A 119.7(5) . . ? C15A C14A Br1A 120.4(5) . . ? C14A C15A C16A 118.3(6) . . ? C14A C15A H15A 120.9 . . ? C16A C15A H15A 120.9 . . ? C11A C16A C15A 118.2(5) . . ? C11A C16A H16A 120.9 . . ? C15A C16A H16A 120.9 . . ? C22 C21 C26 119.3(5) . . ? C22 C21 C2A 122.6(5) . . ? C26 C21 C2A 118.0(5) . . ? C23 C22 C21 119.3(5) . . ? C23 C22 H22 120.3 . . ? C21 C22 H22 120.3 . . ? C24 C23 C22 119.8(5) . . ? C24 C23 C3A 119.7(5) . . ? C22 C23 C3A 120.2(4) . . ? C25 C24 C23 121.0(5) . . ? C25 C24 H24 119.5 . . ? C23 C24 H24 119.5 . . ? C26 C25 C24 120.4(5) . . ? C26 C25 H25 119.8 . . ? C24 C25 H25 119.8 . . ? C25 C26 C21 120.0(5) . . ? C25 C26 H26 120.0 . . ? C21 C26 H26 120.0 . . ? N22A C21A C26A 123.7(5) . . ? N22A C21A N2A 112.5(4) . . ? C26A C21A N2A 123.8(5) . . ? C21A N22A C23A 117.3(5) . . ? N22A C23A C24A 123.0(6) . . ? N22A C23A H23A 118.5 . . ? C24A C23A H23A 118.5 . . ? C23A C24A C25A 119.0(6) . . ? C23A C24A Br2C 124.9(6) . . ? C25A C24A Br2C 115.5(6) . . ? C23A C24A Br2A 116.5(5) . . ? C25A C24A Br2A 124.5(5) . . ? C24A C25A C26A 119.5(6) . . ? C24A C25A H25A 120.2 . . ? C26A C25A H25A 120.2 . . ? C25A C26A C21A 117.2(6) . . ? C25A C26A H26A 121.4 . . ? C21A C26A H26A 121.4 . . ? C32 C31 C36 119.5(5) . . ? C32 C31 C4A 121.6(4) . . ? C36 C31 C4A 118.7(4) . . ? C33 C32 C31 120.8(4) . . ? C33 C32 H32 119.6 . . ? C31 C32 H32 119.6 . . ? C34 C33 C32 118.8(5) . . ? C34 C33 C5A 118.5(5) . . ? C32 C33 C5A 122.6(4) . . ? C35 C34 C33 120.2(5) . . ? C35 C34 H34 119.9 . . ? C33 C34 H34 119.9 . . ? C36 C35 C34 121.3(5) . . ? C36 C35 H35 119.3 . . ? C34 C35 H35 119.3 . . ? C35 C36 C31 119.2(5) . . ? C35 C36 H36 120.4 . . ? C31 C36 H36 120.4 . . ? N32A C31A C36A 123.1(5) . . ? N32A C31A N3A 116.2(5) . . ? C36A C31A N3A 120.7(5) . . ? C31A N32A C33A 117.8(5) . . ? N32A C33A C34A 122.5(6) . . ? N32A C33A H33A 118.8 . . ? C34A C33A H33A 118.8 . . ? C35A C34A C33A 119.1(5) . . ? C35A C34A Br3A 120.3(5) . . ? C33A C34A Br3A 120.6(5) . . ? C34A C35A C36A 119.3(6) . . ? C34A C35A H35A 120.3 . . ? C36A C35A H35A 120.3 . . ? C35A C36A C31A 118.1(6) . . ? C35A C36A H36A 121.0 . . ? C31A C36A H36A 121.0 . . ? O1B C1B N1B 119.6(5) . . ? O1B C1B C43 121.4(5) . . ? N1B C1B C43 118.8(5) . . ? C2B N1B C1B 117.8(4) . . ? C2B N1B C11B 117.4(4) . . ? C1B N1B C11B 119.2(4) . . ? O2B C2B N1B 121.4(5) . . ? O2B C2B C51 122.2(5) . . ? N1B C2B C51 116.3(5) . . ? O3B C3B N2B 119.9(5) . . ? O3B C3B C53 121.7(5) . . ? N2B C3B C53 118.0(4) . . ? C4B N2B C3B 119.8(4) . . ? C4B N2B C21B 119.9(5) . . ? C3B N2B C21B 114.2(4) . . ? O4B C4B N2B 120.7(5) . . ? O4B C4B C61 122.1(5) . . ? N2B C4B C61 117.2(5) . . ? O5B C5B N3B 120.7(5) . . ? O5B C5B C63 121.3(5) . . ? N3B C5B C63 117.5(4) . . ? C5B N3B C31B 119.9(4) . . ? C5B N3B C6B 120.9(4) . . ? C31B N3B C6B 114.7(4) . . ? O6B C6B N3B 121.0(5) . . ? O6B C6B C41 122.9(5) . . ? N3B C6B C41 115.9(4) . . ? C42 C41 C46 119.9(5) . . ? C42 C41 C6B 120.6(4) . . ? C46 C41 C6B 119.2(5) . . ? C41 C42 C43 119.8(4) . . ? C41 C42 H42 120.1 . . ? C43 C42 H42 120.1 . . ? C44 C43 C42 119.1(5) . . ? C44 C43 C1B 118.5(5) . . ? C42 C43 C1B 121.9(5) . . ? C45 C44 C43 120.4(5) . . ? C45 C44 H44 119.8 . . ? C43 C44 H44 119.8 . . ? C46 C45 C44 121.4(5) . . ? C46 C45 H45 119.3 . . ? C44 C45 H45 119.3 . . ? C45 C46 C41 119.2(5) . . ? C45 C46 H46 120.4 . . ? C41 C46 H46 120.4 . . ? N12B C11B C16B 124.0(5) . . ? N12B C11B N1B 115.9(5) . . ? C16B C11B N1B 120.1(5) . . ? C11B N12B C13B 117.2(5) . . ? N12B C13B C14B 122.2(6) . . ? N12B C13B H13B 118.9 . . ? C14B C13B H13B 118.9 . . ? C13B C14B C15B 119.8(5) . . ? C13B C14B Br1B 120.2(5) . . ? C15B C14B Br1B 119.9(4) . . ? C16B C15B C14B 118.5(5) . . ? C16B C15B H15B 120.7 . . ? C14B C15B H15B 120.7 . . ? C15B C16B C11B 118.1(5) . . ? C15B C16B H16B 121.0 . . ? C11B C16B H16B 121.0 . . ? C56 C51 C52 120.0(5) . . ? C56 C51 C2B 119.5(5) . . ? C52 C51 C2B 120.6(5) . . ? C53 C52 C51 120.1(5) . . ? C53 C52 H52 120.0 . . ? C51 C52 H52 120.0 . . ? C54 C53 C52 119.3(5) . . ? C54 C53 C3B 119.3(5) . . ? C52 C53 C3B 120.5(5) . . ? C55 C54 C53 120.7(5) . . ? C55 C54 H54 119.7 . . ? C53 C54 H54 119.7 . . ? C54 C55 C56 120.2(6) . . ? C54 C55 H55 119.9 . . ? C56 C55 H55 119.9 . . ? C51 C56 C55 119.8(6) . . ? C51 C56 H56 120.1 . . ? C55 C56 H56 120.1 . . ? C26B C21B N22B 124.5(6) . . ? C26B C21B N2B 117.7(5) . . ? N22B C21B N2B 117.4(5) . . ? C21B N22B C23B 117.1(6) . . ? N22B C23B C24B 121.0(7) . . ? N22B C23B H24B 119.5 . . ? C24B C23B H24B 119.5 . . ? C23B C24B C25B 120.7(6) . . ? C23B C24B Br2D 132.5(7) . . ? C25B C24B Br2D 106.8(6) . . ? C23B C24B Br2B 114.9(6) . . ? C25B C24B Br2B 124.1(6) . . ? C24B C25B C26B 118.4(6) . . ? C24B C25B H25B 120.8 . . ? C26B C25B H25B 120.8 . . ? C21B C26B C25B 118.1(6) . . ? C21B C26B H26B 121.0 . . ? C25B C26B H26B 121.0 . . ? C66 C61 C62 119.2(5) . . ? C66 C61 C4B 119.8(5) . . ? C62 C61 C4B 120.7(5) . . ? C63 C62 C61 119.9(5) . . ? C63 C62 H62 120.0 . . ? C61 C62 H62 120.0 . . ? C62 C63 C64 119.6(5) . . ? C62 C63 C5B 122.5(4) . . ? C64 C63 C5B 117.3(5) . . ? C65 C64 C63 120.1(5) . . ? C65 C64 H64 119.9 . . ? C63 C64 H64 119.9 . . ? C64 C65 C66 120.0(5) . . ? C64 C65 H65 120.0 . . ? C66 C65 H65 120.0 . . ? C61 C66 C65 120.9(5) . . ? C61 C66 H66 119.5 . . ? C65 C66 H66 119.5 . . ? N32B C31B C36B 123.3(5) . . ? N32B C31B N3B 113.6(4) . . ? C36B C31B N3B 123.0(5) . . ? C31B N32B C33B 117.8(5) . . ? N32B C33B C34B 121.8(5) . . ? N32B C33B H33B 119.1 . . ? C34B C33B H33B 119.1 . . ? C33B C34B C35B 120.1(5) . . ? C33B C34B Br3B 118.1(4) . . ? C35B C34B Br3B 121.8(4) . . ? C34B C35B C36B 117.9(5) . . ? C34B C35B H35B 121.0 . . ? C36B C35B H35B 121.0 . . ? C35B C36B C31B 119.0(5) . . ? C35B C36B H36B 120.5 . . ? C31B C36B H36B 120.5 . . ? C2S C1S H1S1 109.5 . . ? C2S C1S H1S2 109.5 . . ? H1S1 C1S H1S2 109.5 . . ? C2S C1S H1S3 109.5 . . ? H1S1 C1S H1S3 109.5 . . ? H1S2 C1S H1S3 109.5 . . ? O1S C2S O2S 119.7(9) . . ? O1S C2S C1S 125.7(9) . . ? O2S C2S C1S 114.7(10) . . ? C2S O2S C3S 120.0(8) . . ? O2S C3S C4S 108.8(7) . . ? O2S C3S H3S1 109.9 . . ? C4S C3S H3S1 109.9 . . ? O2S C3S H3S2 109.9 . . ? C4S C3S H3S2 109.9 . . ? H3S1 C3S H3S2 108.3 . . ? C3S C4S H4S1 109.5 . . ? C3S C4S H4S2 109.5 . . ? H4S1 C4S H4S2 109.5 . . ? C3S C4S H4S3 109.5 . . ? H4S1 C4S H4S3 109.5 . . ? H4S2 C4S H4S3 109.5 . . ? 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 O1A C1A N1A C2A -29.8(8) . . . . ? C13 C1A N1A C2A 146.2(5) . . . . ? O1A C1A N1A C11A 128.1(5) . . . . ? C13 C1A N1A C11A -55.8(6) . . . . ? C11A N1A C2A O2A -6.9(8) . . . . ? C1A N1A C2A O2A 150.7(6) . . . . ? C11A N1A C2A C21 168.9(5) . . . . ? C1A N1A C2A C21 -33.5(7) . . . . ? O3A C3A N2A C4A 114.7(6) . . . . ? C23 C3A N2A C4A -67.6(6) . . . . ? O3A C3A N2A C21A -58.1(6) . . . . ? C23 C3A N2A C21A 119.6(5) . . . . ? C21A N2A C4A O4A 164.1(5) . . . . ? C3A N2A C4A O4A -7.9(7) . . . . ? C21A N2A C4A C31 -19.1(7) . . . . ? C3A N2A C4A C31 168.9(4) . . . . ? O5A C5A N3A C6A -140.3(5) . . . . ? C33 C5A N3A C6A 45.6(6) . . . . ? O5A C5A N3A C31A 10.2(7) . . . . ? C33 C5A N3A C31A -163.9(4) . . . . ? C5A N3A C6A O6A 24.5(7) . . . . ? C31A N3A C6A O6A -126.2(5) . . . . ? C5A N3A C6A C11 -153.0(4) . . . . ? C31A N3A C6A C11 56.3(6) . . . . ? O6A C6A C11 C16 36.6(8) . . . . ? N3A C6A C11 C16 -145.9(5) . . . . ? O6A C6A C11 C12 -134.1(5) . . . . ? N3A C6A C11 C12 43.4(6) . . . . ? C16 C11 C12 C13 -3.7(7) . . . . ? C6A C11 C12 C13 167.1(4) . . . . ? C11 C12 C13 C14 3.8(7) . . . . ? C11 C12 C13 C1A -167.4(4) . . . . ? O1A C1A C13 C14 -30.0(8) . . . . ? N1A C1A C13 C14 154.0(5) . . . . ? O1A C1A C13 C12 141.1(5) . . . . ? N1A C1A C13 C12 -35.0(6) . . . . ? C12 C13 C14 C15 0.5(8) . . . . ? C1A C13 C14 C15 171.7(5) . . . . ? C13 C14 C15 C16 -4.8(8) . . . . ? C14 C15 C16 C11 4.9(9) . . . . ? C12 C11 C16 C15 -0.6(8) . . . . ? C6A C11 C16 C15 -171.3(5) . . . . ? C2A N1A C11A N12A 118.9(6) . . . . ? C1A N1A C11A N12A -40.1(6) . . . . ? C2A N1A C11A C16A -60.8(7) . . . . ? C1A N1A C11A C16A 140.2(5) . . . . ? C16A C11A N12A C13A 1.1(9) . . . . ? N1A C11A N12A C13A -178.6(5) . . . . ? C11A N12A C13A C14A 0.9(9) . . . . ? N12A C13A C14A C15A -2.4(10) . . . . ? N12A C13A C14A Br1A 177.7(5) . . . . ? C13A C14A C15A C16A 1.8(9) . . . . ? Br1A C14A C15A C16A -178.3(4) . . . . ? N12A C11A C16A C15A -1.7(9) . . . . ? N1A C11A C16A C15A 178.0(5) . . . . ? C14A C15A C16A C11A 0.1(9) . . . . ? O2A C2A C21 C22 143.8(6) . . . . ? N1A C2A C21 C22 -32.0(8) . . . . ? O2A C2A C21 C26 -32.4(9) . . . . ? N1A C2A C21 C26 151.8(5) . . . . ? C26 C21 C22 C23 -1.8(8) . . . . ? C2A C21 C22 C23 -177.9(5) . . . . ? C21 C22 C23 C24 1.7(8) . . . . ? C21 C22 C23 C3A -172.4(5) . . . . ? O3A C3A C23 C24 -34.0(8) . . . . ? N2A C3A C23 C24 148.3(5) . . . . ? O3A C3A C23 C22 140.1(6) . . . . ? N2A C3A C23 C22 -37.5(7) . . . . ? C22 C23 C24 C25 -0.1(9) . . . . ? C3A C23 C24 C25 174.1(6) . . . . ? C23 C24 C25 C26 -1.5(10) . . . . ? C24 C25 C26 C21 1.5(9) . . . . ? C22 C21 C26 C25 0.2(8) . . . . ? C2A C21 C26 C25 176.5(6) . . . . ? C4A N2A C21A N22A 144.7(5) . . . . ? C3A N2A C21A N22A -43.3(6) . . . . ? C4A N2A C21A C26A -35.9(7) . . . . ? C3A N2A C21A C26A 136.1(5) . . . . ? C26A C21A N22A C23A 0.9(8) . . . . ? N2A C21A N22A C23A -179.8(5) . . . . ? C21A N22A C23A C24A 3.8(8) . . . . ? N22A C23A C24A C25A -5.9(10) . . . . ? N22A C23A C24A Br2C -176.3(6) . . . . ? N22A C23A C24A Br2A 175.3(5) . . . . ? C23A C24A C25A C26A 3.2(9) . . . . ? Br2C C24A C25A C26A 174.5(6) . . . . ? Br2A C24A C25A C26A -178.1(5) . . . . ? C24A C25A C26A C21A 1.0(9) . . . . ? N22A C21A C26A C25A -3.2(8) . . . . ? N2A C21A C26A C25A 177.5(5) . . . . ? O4A C4A C31 C32 120.7(5) . . . . ? N2A C4A C31 C32 -56.1(6) . . . . ? O4A C4A C31 C36 -54.7(7) . . . . ? N2A C4A C31 C36 128.6(5) . . . . ? C36 C31 C32 C33 1.8(7) . . . . ? C4A C31 C32 C33 -173.5(5) . . . . ? C31 C32 C33 C34 -0.5(8) . . . . ? C31 C32 C33 C5A 175.1(5) . . . . ? O5A C5A C33 C34 28.4(8) . . . . ? N3A C5A C33 C34 -157.7(5) . . . . ? O5A C5A C33 C32 -147.1(5) . . . . ? N3A C5A C33 C32 26.8(7) . . . . ? C32 C33 C34 C35 -1.4(8) . . . . ? C5A C33 C34 C35 -177.1(5) . . . . ? C33 C34 C35 C36 1.9(9) . . . . ? C34 C35 C36 C31 -0.5(9) . . . . ? C32 C31 C36 C35 -1.4(8) . . . . ? C4A C31 C36 C35 174.1(5) . . . . ? C5A N3A C31A N32A -117.3(5) . . . . ? C6A N3A C31A N32A 33.9(6) . . . . ? C5A N3A C31A C36A 61.8(6) . . . . ? C6A N3A C31A C36A -147.0(5) . . . . ? C36A C31A N32A C33A -0.8(8) . . . . ? N3A C31A N32A C33A 178.3(5) . . . . ? C31A N32A C33A C34A -2.7(9) . . . . ? N32A C33A C34A C35A 3.8(10) . . . . ? N32A C33A C34A Br3A -175.5(5) . . . . ? C33A C34A C35A C36A -1.2(10) . . . . ? Br3A C34A C35A C36A 178.1(5) . . . . ? C34A C35A C36A C31A -2.1(9) . . . . ? N32A C31A C36A C35A 3.3(9) . . . . ? N3A C31A C36A C35A -175.8(5) . . . . ? O1B C1B N1B C2B 24.2(7) . . . . ? C43 C1B N1B C2B -150.0(5) . . . . ? O1B C1B N1B C11B -128.8(5) . . . . ? C43 C1B N1B C11B 57.0(6) . . . . ? C1B N1B C2B O2B -140.7(6) . . . . ? C11B N1B C2B O2B 12.8(8) . . . . ? C1B N1B C2B C51 43.0(7) . . . . ? C11B N1B C2B C51 -163.5(5) . . . . ? O3B C3B N2B C4B -125.7(5) . . . . ? C53 C3B N2B C4B 61.1(6) . . . . ? O3B C3B N2B C21B 26.7(7) . . . . ? C53 C3B N2B C21B -146.5(5) . . . . ? C3B N2B C4B O4B 6.8(7) . . . . ? C21B N2B C4B O4B -144.0(5) . . . . ? C3B N2B C4B C61 -171.7(4) . . . . ? C21B N2B C4B C61 37.5(6) . . . . ? O5B C5B N3B C31B -9.6(7) . . . . ? C63 C5B N3B C31B 162.4(4) . . . . ? O5B C5B N3B C6B 145.2(5) . . . . ? C63 C5B N3B C6B -42.8(6) . . . . ? C5B N3B C6B O6B -30.5(7) . . . . ? C31B N3B C6B O6B 125.6(5) . . . . ? C5B N3B C6B C41 145.1(4) . . . . ? C31B N3B C6B C41 -58.8(6) . . . . ? O6B C6B C41 C42 141.0(5) . . . . ? N3B C6B C41 C42 -34.6(6) . . . . ? O6B C6B C41 C46 -33.4(8) . . . . ? N3B C6B C41 C46 151.0(4) . . . . ? C46 C41 C42 C43 4.6(7) . . . . ? C6B C41 C42 C43 -169.8(4) . . . . ? C41 C42 C43 C44 -3.3(7) . . . . ? C41 C42 C43 C1B 168.5(4) . . . . ? O1B C1B C43 C44 20.5(7) . . . . ? N1B C1B C43 C44 -165.4(4) . . . . ? O1B C1B C43 C42 -151.3(5) . . . . ? N1B C1B C43 C42 22.8(7) . . . . ? C42 C43 C44 C45 -0.2(7) . . . . ? C1B C43 C44 C45 -172.2(5) . . . . ? C43 C44 C45 C46 2.4(8) . . . . ? C44 C45 C46 C41 -1.1(8) . . . . ? C42 C41 C46 C45 -2.4(7) . . . . ? C6B C41 C46 C45 172.0(5) . . . . ? C2B N1B C11B N12B -123.8(6) . . . . ? C1B N1B C11B N12B 29.3(7) . . . . ? C2B N1B C11B C16B 54.7(7) . . . . ? C1B N1B C11B C16B -152.2(5) . . . . ? C16B C11B N12B C13B -1.8(9) . . . . ? N1B C11B N12B C13B 176.6(6) . . . . ? C11B N12B C13B C14B -1.7(10) . . . . ? N12B C13B C14B C15B 3.5(11) . . . . ? N12B C13B C14B Br1B -175.9(5) . . . . ? C13B C14B C15B C16B -1.9(9) . . . . ? Br1B C14B C15B C16B 177.6(5) . . . . ? C14B C15B C16B C11B -1.4(9) . . . . ? N12B C11B C16B C15B 3.4(9) . . . . ? N1B C11B C16B C15B -175.0(5) . . . . ? O2B C2B C51 C56 35.4(8) . . . . ? N1B C2B C51 C56 -148.4(5) . . . . ? O2B C2B C51 C52 -143.5(6) . . . . ? N1B C2B C51 C52 32.7(7) . . . . ? C56 C51 C52 C53 2.3(8) . . . . ? C2B C51 C52 C53 -178.8(5) . . . . ? C51 C52 C53 C54 -1.4(8) . . . . ? C51 C52 C53 C3B 167.6(5) . . . . ? O3B C3B C53 C54 29.4(8) . . . . ? N2B C3B C53 C54 -157.5(5) . . . . ? O3B C3B C53 C52 -139.5(5) . . . . ? N2B C3B C53 C52 33.6(7) . . . . ? C52 C53 C54 C55 -1.0(8) . . . . ? C3B C53 C54 C55 -170.1(5) . . . . ? C53 C54 C55 C56 2.4(10) . . . . ? C52 C51 C56 C55 -1.0(9) . . . . ? C2B C51 C56 C55 -179.8(5) . . . . ? C54 C55 C56 C51 -1.4(9) . . . . ? C4B N2B C21B C26B -125.8(6) . . . . ? C3B N2B C21B C26B 81.9(6) . . . . ? C4B N2B C21B N22B 60.9(7) . . . . ? C3B N2B C21B N22B -91.4(6) . . . . ? C26B C21B N22B C23B -1.6(9) . . . . ? N2B C21B N22B C23B 171.2(5) . . . . ? C21B N22B C23B C24B -0.6(10) . . . . ? N22B C23B C24B C25B 3.7(11) . . . . ? N22B C23B C24B Br2D -176.7(6) . . . . ? N22B C23B C24B Br2B -170.6(5) . . . . ? C23B C24B C25B C26B -4.6(11) . . . . ? Br2D C24B C25B C26B 175.8(5) . . . . ? Br2B C24B C25B C26B 169.2(5) . . . . ? N22B C21B C26B C25B 0.7(9) . . . . ? N2B C21B C26B C25B -172.1(5) . . . . ? C24B C25B C26B C21B 2.4(10) . . . . ? O4B C4B C61 C66 47.9(7) . . . . ? N2B C4B C61 C66 -133.6(5) . . . . ? O4B C4B C61 C62 -125.6(6) . . . . ? N2B C4B C61 C62 52.8(6) . . . . ? C66 C61 C62 C63 -1.5(7) . . . . ? C4B C61 C62 C63 172.0(4) . . . . ? C61 C62 C63 C64 3.1(7) . . . . ? C61 C62 C63 C5B -168.3(5) . . . . ? O5B C5B C63 C62 144.9(5) . . . . ? N3B C5B C63 C62 -27.0(7) . . . . ? O5B C5B C63 C64 -26.7(7) . . . . ? N3B C5B C63 C64 161.4(4) . . . . ? C62 C63 C64 C65 -1.1(8) . . . . ? C5B C63 C64 C65 170.8(5) . . . . ? C63 C64 C65 C66 -2.5(9) . . . . ? C62 C61 C66 C65 -2.1(8) . . . . ? C4B C61 C66 C65 -175.8(5) . . . . ? C64 C65 C66 C61 4.2(9) . . . . ? C5B N3B C31B N32B 127.7(5) . . . . ? C6B N3B C31B N32B -28.6(6) . . . . ? C5B N3B C31B C36B -55.5(7) . . . . ? C6B N3B C31B C36B 148.2(5) . . . . ? C36B C31B N32B C33B -1.3(8) . . . . ? N3B C31B N32B C33B 175.5(5) . . . . ? C31B N32B C33B C34B -0.7(8) . . . . ? N32B C33B C34B C35B 2.2(9) . . . . ? N32B C33B C34B Br3B -176.2(4) . . . . ? C33B C34B C35B C36B -1.7(9) . . . . ? Br3B C34B C35B C36B 176.8(4) . . . . ? C34B C35B C36B C31B -0.3(8) . . . . ? N32B C31B C36B C35B 1.9(8) . . . . ? N3B C31B C36B C35B -174.6(5) . . . . ? O1S C2S O2S C3S -8.4(13) . . . . ? C1S C2S O2S C3S 171.9(7) . . . . ? C2S O2S C3S C4S -177.2(8) . . . . ? _iucr_refine_instructions_details ; TITL 12-009 is BrIO3:0.5(EtOAc) in P21/n [Z'=2] @ 40kV30mA - 0.80\%A CELL 0.71073 10.9440 65.6499 11.2294 90.000 110.447 90.000 ZERR 8 0.0003 0.0013 0.0003 0.000 0.003 0.000 LATT 1 SYMM 1/2-X,1/2+Y,1/2-Z SFAC C H N O BR UNIT 328 200 48 56 24 MERG 3 FMAP 2 L.S. 8 3 LIST 4 ACTA 52 CONF BOND $H FREE BR2A BR2C FREE BR2B BR2D EQIV $1 1-X,-Y,-1-Z EQIV $2 1-X,-Y,-Z EQIV $3 X,Y,-1+Z EQIV $4 X,Y,1+Z EQIV $5 1/2+X,1/2-Y,-1/2+Z EQIV $6 -1/2+X,1/2-Y,1/2+Z HTAB HTAB C1S O4A HTAB C4S BR1A_$1 HTAB C15A O5A_$2 HTAB C16A O1S HTAB C35A O5A_$2 HTAB C35B O3B_$3 HTAB C54 O1A_$4 RTAB BR3B O6B_$5 RTAB BR2D C33B_$6 RTAB XX BR1A BR2A RTAB XX BR1A BR3A RTAB XX BR2A BR3A RTAB XX BR1B BR2B RTAB XX BR1B BR3B RTAB XX BR2B BR3B RTAB XX BR1A BR2C RTAB XX BR2C BR3A RTAB XX BR1B BR2D RTAB XX BR2D BR3B RTAB OO O1A O2A RTAB OO O3A O4A RTAB OO O5A O6A RTAB OO O1A O6A RTAB OO O2A O3A RTAB OO O4A O5A RTAB NN N1A N2A RTAB NN N1A N3A RTAB NN N2A N3A RTAB NN N12A N22A RTAB NN N12A N32A RTAB NN N22A N32A RTAB OO O1B O2B RTAB OO O3B O4B RTAB OO O5B O6B RTAB OO O1B O6B RTAB OO O2B O3B RTAB OO O4B O5B RTAB NN N1B N2B RTAB NN N1B N3B RTAB NN N2B N3B RTAB NN N12B N22B RTAB NN N12B N32B RTAB NN N22B N32B RTAB XNNX BR1A N1A N2A BR2A RTAB XNNX BR1A N1A N3A BR3A RTAB XNNX BR2A N2A N3A BR3A RTAB XNNX BR1B N1B N2B BR2B RTAB XNNX BR1B N1B N3B BR3B RTAB XNNX BR2B N2B N3B BR3B RTAB OCCO O1A C1A C2A O2A RTAB OCCO O3A C3A C4A O4A RTAB OCCO O5A C5A C6A O6A RTAB OCCO O1B C1B C2B O2B RTAB OCCO O3B C3B C4B O4B RTAB OCCO O5B C5B C6B O6B RTAB OCCO O1A C1A C6A O6A RTAB OCCO O2A C2A C3A O3A RTAB OCCO O4A C5A C6A O6A RTAB OCCO O1B C1B C6B O6B RTAB OCCO O2B C2B C3B O3B RTAB OCCO O4B C5B C6B O6B SIZE 0.08 0.29 0.52 TEMP 21 PLAN 15 MPLA 3 C1A C2A C11A N1A N2A N3A MPLA 3 C3A C4A C21A N2A N1A N3A MPLA 3 C5A C6A C31A N3A N1A N2A MPLA 3 C1B C2B C11B N1B N2B N3B MPLA 3 C3B C4B C21B N2B N1B N3B MPLA 3 C5B C6B C31B N3B N1B N2B MPLA 6 C11 C12 C13 C14 C15 C16 MPLA 7 C11A N12A C13A C14A C15A C16A BR2A BR2C MPLA 6 C21 C22 C23 C24 C25 C26 MPLA 7 C21A N22A C23A C24A C25A C26A BR2A BR2C MPLA 6 C31 C32 C33 C34 C35 C36 MPLA 7 C31A N32A C33A C34A C35A C36A BR2A BR2C MPLA 6 C41 C42 C43 C44 C45 C46 MPLA 7 C11B N12B C13B C14B C15B C16B BR2B BR2D MPLA 6 C51 C52 C53 C54 C55 C56 MPLA 7 C21B N22B C23B C24B C25B C26B BR2B BR2D MPLA 6 C61 C62 C63 C64 C65 C66 MPLA 7 C31B N32B C33B C34B C35B C36B BR2B BR2D WGHT 0.039000 11.526700 FVAR 1.58088 MOLE 1 PART -1 BR1A 5 0.770665 0.006443 -0.400271 11.00000 0.09292 0.06100 = 0.09114 -0.02422 0.02750 0.01674 BR2A 5 1.116303 0.097293 0.540298 10.58000 0.03801 0.08205 = 0.07813 -0.01293 -0.00462 0.00429 PART -2 BR2C 5 1.093549 0.099394 0.559420 10.42000 0.04659 0.12330 = 0.15034 -0.03158 -0.01821 0.02644 PART 0 BR3A 5 0.887901 -0.033485 -0.060649 11.00000 0.15025 0.06023 = 0.12869 -0.01991 0.09342 0.00374 O1A 4 0.769141 0.110213 -0.100113 11.00000 0.07219 0.04678 = 0.08404 0.01952 0.02787 -0.00186 C1A 1 0.753127 0.092590 -0.084748 11.00000 0.05140 0.04349 = 0.05179 0.00359 0.02973 0.00181 N1A 3 0.643722 0.081503 -0.165613 11.00000 0.05495 0.04105 = 0.03575 0.00241 0.01868 0.00943 O2A 4 0.450227 0.084072 -0.329302 11.00000 0.09824 0.08414 = 0.04185 -0.01629 -0.00212 0.03460 C2A 1 0.521605 0.090746 -0.228611 11.00000 0.06643 0.05720 = 0.03189 0.00220 0.01483 0.00904 O3A 4 0.541756 0.144260 0.208979 11.00000 0.07285 0.03331 = 0.06007 -0.01521 0.02027 0.00239 C3A 1 0.518841 0.127805 0.160296 11.00000 0.03931 0.03248 = 0.05222 -0.00330 0.01709 0.00500 N2A 3 0.543255 0.109544 0.237243 11.00000 0.03987 0.03606 = 0.03924 -0.00672 0.01380 -0.00059 O4A 4 0.327728 0.104161 0.177921 11.00000 0.03902 0.05353 = 0.06291 -0.00321 0.01554 0.01064 C4A 1 0.436546 0.098051 0.232584 11.00000 0.03858 0.04785 = 0.03856 -0.01273 0.01711 -0.00143 O5A 4 0.577279 0.009151 0.252150 11.00000 0.06932 0.03584 = 0.07787 0.00119 0.03512 -0.00948 C5A 1 0.612398 0.026925 0.258600 11.00000 0.04291 0.04282 = 0.03889 0.00491 0.00808 0.00025 N3A 3 0.712026 0.032382 0.211783 11.00000 0.03873 0.03244 = 0.04503 0.00119 0.01563 0.00041 O6A 4 0.833983 0.049554 0.392263 11.00000 0.05524 0.06542 = 0.04115 0.00302 0.01132 -0.00706 C6A 1 0.808042 0.046820 0.280343 11.00000 0.03977 0.03257 = 0.04574 0.00374 0.01391 0.00429 C11 1 0.869050 0.058757 0.203289 11.00000 0.03507 0.03361 = 0.04107 -0.00481 0.01214 0.00020 C12 1 0.791313 0.066580 0.086613 11.00000 0.04092 0.03213 = 0.03931 -0.00513 0.01596 -0.00208 AFIX 43 H12 2 0.705626 0.062158 0.049198 11.00000 -1.20000 AFIX 0 C13 1 0.841562 0.081047 0.025546 11.00000 0.05008 0.02712 = 0.04664 -0.00503 0.02339 -0.00210 C14 1 0.970822 0.086553 0.078657 11.00000 0.04642 0.04260 = 0.05991 -0.00605 0.02761 -0.00693 AFIX 43 H14 2 1.004937 0.096289 0.038806 11.00000 -1.20000 AFIX 0 C15 1 1.049837 0.077760 0.190208 11.00000 0.03086 0.05048 = 0.07022 -0.00820 0.01575 -0.01039 AFIX 43 H15 2 1.138421 0.080781 0.222154 11.00000 -1.20000 AFIX 0 C16 1 0.997828 0.064542 0.254192 11.00000 0.03856 0.04818 = 0.05267 -0.00195 0.01057 0.00234 AFIX 43 H16 2 1.050052 0.059434 0.332742 11.00000 -1.20000 AFIX 0 C11A 1 0.672293 0.063035 -0.217023 11.00000 0.05969 0.04344 = 0.03426 0.00273 0.02209 0.01185 N12A 3 0.774261 0.063686 -0.253519 11.00000 0.06933 0.04317 = 0.06366 -0.00968 0.04072 -0.00459 C13A 1 0.801489 0.046540 -0.305069 11.00000 0.07512 0.06172 = 0.06684 -0.00443 0.04611 0.00838 AFIX 43 H13A 2 0.873649 0.046447 -0.330664 11.00000 -1.20000 AFIX 0 C14A 1 0.728301 0.029381 -0.321349 11.00000 0.06813 0.03972 = 0.05150 -0.00099 0.01545 0.00910 C15A 1 0.625084 0.028810 -0.280635 11.00000 0.06197 0.05367 = 0.05394 -0.00676 0.02091 -0.00678 AFIX 43 H15A 2 0.575496 0.017038 -0.289041 11.00000 -1.20000 AFIX 0 C16A 1 0.595817 0.046116 -0.226605 11.00000 0.05169 0.06333 = 0.05153 0.00167 0.02253 -0.00095 AFIX 43 H16A 2 0.526091 0.046327 -0.197400 11.00000 -1.20000 AFIX 0 C21 1 0.480185 0.107680 -0.164547 11.00000 0.04519 0.04230 = 0.04220 0.00308 0.01542 0.00339 C22 1 0.515656 0.108844 -0.032522 11.00000 0.04889 0.03122 = 0.03955 0.00615 0.01197 0.00804 AFIX 43 H22 2 0.569614 0.098990 0.019203 11.00000 -1.20000 AFIX 0 C23 1 0.469656 0.124816 0.020516 11.00000 0.04330 0.02722 = 0.04832 -0.00052 0.01575 0.00244 C24 1 0.387078 0.139006 -0.057025 11.00000 0.06454 0.03913 = 0.06078 0.00331 0.02688 0.01496 AFIX 43 H24 2 0.356361 0.149691 -0.020901 11.00000 -1.20000 AFIX 0 C25 1 0.349557 0.137644 -0.186094 11.00000 0.05900 0.05033 = 0.05992 0.01537 0.01627 0.01970 AFIX 43 H25 2 0.292033 0.147194 -0.237022 11.00000 -1.20000 AFIX 0 C26 1 0.395832 0.122384 -0.240812 11.00000 0.05073 0.05036 = 0.04290 0.00931 0.01006 0.00341 AFIX 43 H26 2 0.371463 0.121719 -0.328786 11.00000 -1.20000 AFIX 0 C21A 1 0.674067 0.106723 0.321265 11.00000 0.04849 0.03217 = 0.04002 -0.00817 0.01437 -0.00457 N22A 3 0.760989 0.111025 0.266763 11.00000 0.04318 0.04571 = 0.05116 -0.00356 0.01760 0.00107 C23A 1 0.886472 0.108807 0.337263 11.00000 0.04704 0.05378 = 0.07326 -0.01222 0.01830 0.00190 AFIX 43 H23A 2 0.948846 0.112524 0.302443 11.00000 -1.20000 AFIX 0 C24A 1 0.927506 0.101360 0.457754 11.00000 0.04832 0.04952 = 0.06762 -0.00867 -0.00207 -0.00369 C25A 1 0.837415 0.097590 0.514026 11.00000 0.07558 0.05081 = 0.04471 0.00005 -0.00735 -0.01480 AFIX 43 H25A 2 0.864017 0.093139 0.597861 11.00000 -1.20000 AFIX 0 C26A 1 0.706879 0.100431 0.445642 11.00000 0.06037 0.05864 = 0.04283 -0.00639 0.01143 -0.02324 AFIX 43 H26A 2 0.643548 0.098197 0.481904 11.00000 -1.20000 AFIX 0 C31 1 0.461506 0.077239 0.292112 11.00000 0.03073 0.04903 = 0.03391 -0.00528 0.00950 -0.00126 C32 1 0.534128 0.062800 0.255720 11.00000 0.03304 0.04747 = 0.03831 -0.00207 0.01594 -0.00931 AFIX 43 H32 2 0.575830 0.066407 0.199464 11.00000 -1.20000 AFIX 0 C33 1 0.545320 0.043066 0.302139 11.00000 0.03983 0.04218 = 0.04157 -0.00039 0.01675 -0.00592 C34 1 0.483464 0.038015 0.386361 11.00000 0.05239 0.04699 = 0.04699 0.00335 0.01436 -0.00384 AFIX 43 H34 2 0.488407 0.024764 0.416981 11.00000 -1.20000 AFIX 0 C35 1 0.414404 0.052564 0.425169 11.00000 0.06154 0.07771 = 0.04790 0.00549 0.03276 -0.00625 AFIX 43 H35 2 0.375429 0.049059 0.483818 11.00000 -1.20000 AFIX 0 C36 1 0.402135 0.071968 0.379310 11.00000 0.04385 0.06049 = 0.03880 -0.00304 0.01703 0.00268 AFIX 43 H36 2 0.354713 0.081585 0.405861 11.00000 -1.20000 AFIX 0 C31A 1 0.751530 0.017450 0.140040 11.00000 0.04787 0.02794 = 0.05008 0.00315 0.01997 0.00036 N32A 3 0.873318 0.011237 0.188641 11.00000 0.05119 0.04606 = 0.06247 0.00062 0.01693 0.00258 C33A 1 0.912535 -0.003096 0.125844 11.00000 0.06292 0.05898 = 0.08194 0.00017 0.03021 0.01640 AFIX 43 H33A 2 0.999275 -0.007222 0.157014 11.00000 -1.20000 AFIX 0 C34A 1 0.830156 -0.011933 0.017563 11.00000 0.07803 0.03327 = 0.07194 -0.00873 0.03951 -0.00401 C35A 1 0.704998 -0.005153 -0.032743 11.00000 0.08028 0.05818 = 0.05100 -0.01626 0.01927 -0.01569 AFIX 43 H35A 2 0.647901 -0.010821 -0.107339 11.00000 -1.20000 AFIX 0 C36A 1 0.664226 0.010017 0.027276 11.00000 0.05797 0.05933 = 0.05454 -0.00261 0.01624 0.00035 AFIX 43 H36A 2 0.580072 0.015220 -0.006657 11.00000 -1.20000 AFIX 0 MOLE 2 PART -1 BR1B 5 0.856060 0.202218 -0.170274 11.00000 0.09040 0.08050 = 0.07249 0.01551 0.04885 0.01034 BR2B 5 0.115716 0.230044 0.630148 10.58000 0.05925 0.07199 = 0.08366 -0.03617 -0.00381 0.02575 PART -2 BR2D 5 0.138479 0.235202 0.598882 10.42000 0.24707 0.16585 = 0.13953 -0.02652 0.02121 0.14243 PART 0 BR3B 5 0.580260 0.245980 -0.262193 11.00000 0.07728 0.07867 = 0.09316 0.03128 0.04668 0.00049 O1B 4 0.853782 0.200766 0.513033 11.00000 0.05031 0.06131 = 0.06439 -0.01566 0.00273 -0.00150 C1B 1 0.779172 0.199630 0.404869 11.00000 0.03595 0.03738 = 0.05401 -0.00479 0.01461 -0.00960 N1B 3 0.791525 0.183326 0.326301 11.00000 0.04288 0.03946 = 0.05036 -0.00491 0.02030 -0.00071 O2B 4 0.925651 0.155857 0.348364 11.00000 0.06813 0.05959 = 0.09113 0.01400 0.04656 0.02372 C2B 1 0.853388 0.165153 0.386832 11.00000 0.03809 0.04984 = 0.05831 -0.00141 0.01866 0.00421 O3B 4 0.530206 0.165312 0.714714 11.00000 0.07868 0.07383 = 0.03878 -0.00409 0.02653 0.00408 C3B 1 0.535414 0.160845 0.612580 11.00000 0.05878 0.03636 = 0.03672 0.00169 0.01826 -0.00251 N2B 3 0.424888 0.164108 0.500077 11.00000 0.05341 0.03913 = 0.04151 -0.00614 0.02076 -0.00348 O4B 4 0.415612 0.130684 0.443618 11.00000 0.07887 0.03452 = 0.05373 0.00370 0.01378 -0.00160 C4B 1 0.374257 0.147972 0.416312 11.00000 0.05336 0.04456 = 0.04057 -0.00161 0.02497 -0.00601 O5B 4 0.186609 0.179607 -0.116887 11.00000 0.05425 0.06534 = 0.03961 -0.00457 0.01000 -0.00626 C5B 1 0.228017 0.183995 -0.004972 11.00000 0.03316 0.04654 = 0.03757 0.00147 0.00885 0.00687 N3B 3 0.316656 0.200102 0.039728 11.00000 0.04140 0.03329 = 0.03990 0.00226 0.01742 0.00439 O6B 4 0.212923 0.215856 0.160141 11.00000 0.04672 0.06281 = 0.07523 -0.01787 0.02930 0.00245 C6B 1 0.313231 0.212685 0.142746 11.00000 0.04622 0.03730 = 0.04394 -0.00052 0.02050 0.00677 C41 1 0.441171 0.220053 0.229920 11.00000 0.04547 0.02906 = 0.03847 0.00020 0.01921 0.00158 C42 1 0.551525 0.207946 0.257701 11.00000 0.04936 0.02809 = 0.04105 -0.00272 0.02144 -0.00300 AFIX 43 H42 2 0.549066 0.196069 0.211773 11.00000 -1.20000 AFIX 0 C43 1 0.666936 0.213671 0.355348 11.00000 0.04129 0.03887 = 0.04176 -0.00225 0.02000 -0.00347 C44 1 0.670289 0.231931 0.418079 11.00000 0.04980 0.03848 = 0.04980 -0.00932 0.01949 -0.01186 AFIX 43 H44 2 0.746138 0.235859 0.483068 11.00000 -1.20000 AFIX 0 C45 1 0.562468 0.244252 0.384954 11.00000 0.06630 0.03441 = 0.05940 -0.01169 0.02836 -0.00632 AFIX 43 H45 2 0.567350 0.256703 0.425873 11.00000 -1.20000 AFIX 0 C46 1 0.447685 0.238626 0.292889 11.00000 0.05255 0.03384 = 0.05380 -0.00531 0.02525 0.00132 AFIX 43 H46 2 0.374943 0.247053 0.272486 11.00000 -1.20000 AFIX 0 C11B 1 0.796861 0.187784 0.203648 11.00000 0.03846 0.04169 = 0.05574 -0.00024 0.02250 0.00057 N12B 3 0.846987 0.205484 0.192097 11.00000 0.08105 0.05288 = 0.07181 -0.00982 0.04402 -0.01688 C13B 1 0.859592 0.209666 0.079798 11.00000 0.08968 0.05022 = 0.08274 -0.00045 0.04876 -0.01832 AFIX 43 H13B 2 0.892754 0.222271 0.068477 11.00000 -1.20000 AFIX 0 C14B 1 0.825520 0.196100 -0.017813 11.00000 0.05541 0.05487 = 0.05348 0.00530 0.02878 0.00809 C15B 1 0.769933 0.177903 -0.005624 11.00000 0.05904 0.05410 = 0.05238 -0.00849 0.01942 -0.00381 AFIX 43 H15B 2 0.743835 0.168648 -0.072507 11.00000 -1.20000 AFIX 0 C16B 1 0.753651 0.173640 0.107022 11.00000 0.05095 0.04358 = 0.06067 -0.00273 0.02292 -0.00912 AFIX 43 H16B 2 0.714596 0.161562 0.118237 11.00000 -1.20000 AFIX 0 C51 1 0.816343 0.157756 0.495090 11.00000 0.04662 0.04426 = 0.04227 -0.00605 0.00917 0.00052 C52 1 0.690459 0.160800 0.495782 11.00000 0.04367 0.03965 = 0.03756 -0.00193 0.01171 0.00077 AFIX 43 H52 2 0.628388 0.167269 0.427578 11.00000 -1.20000 AFIX 0 C53 1 0.657786 0.154191 0.598044 11.00000 0.05314 0.03214 = 0.03768 -0.00152 0.01286 -0.00163 C54 1 0.750206 0.144223 0.697340 11.00000 0.07727 0.05011 = 0.03837 0.00070 0.01802 0.01357 AFIX 43 H54 2 0.729265 0.139936 0.766795 11.00000 -1.20000 AFIX 0 C55 1 0.872593 0.140580 0.694555 11.00000 0.08292 0.05309 = 0.04943 0.00457 0.00930 0.02399 AFIX 43 H55 2 0.933045 0.133414 0.760479 11.00000 -1.20000 AFIX 0 C56 1 0.906472 0.147575 0.593432 11.00000 0.05072 0.04887 = 0.05897 -0.00263 0.00792 0.01072 AFIX 43 H56 2 0.990063 0.145353 0.592511 11.00000 -1.20000 AFIX 0 C21B 1 0.339907 0.180333 0.510431 11.00000 0.06127 0.03869 = 0.04274 -0.00648 0.01793 -0.00104 N22B 3 0.240238 0.175289 0.549169 11.00000 0.06308 0.07575 = 0.07840 -0.01680 0.03165 -0.00704 C23B 1 0.172165 0.190761 0.575381 11.00000 0.05070 0.08296 = 0.08898 -0.02341 0.03121 0.00366 AFIX 43 H24B 2 0.102235 0.187873 0.601530 11.00000 -1.20000 AFIX 0 C24B 1 0.204382 0.210476 0.564095 11.00000 0.06752 0.05871 = 0.06572 -0.01439 0.00477 0.02101 C25B 1 0.301548 0.215161 0.519187 11.00000 0.11677 0.04186 = 0.06446 0.00633 0.01796 0.00251 AFIX 43 H25B 2 0.319567 0.228637 0.505787 11.00000 -1.20000 AFIX 0 C26B 1 0.373176 0.199317 0.493846 11.00000 0.07815 0.04602 = 0.04893 0.00455 0.02985 -0.00343 AFIX 43 H26B 2 0.442377 0.201924 0.466089 11.00000 -1.20000 AFIX 0 C61 1 0.271049 0.152934 0.292312 11.00000 0.04501 0.03506 = 0.04161 -0.00289 0.02079 0.00187 C62 1 0.290988 0.168047 0.214252 11.00000 0.03621 0.04094 = 0.04375 -0.00468 0.01593 -0.00643 AFIX 43 H62 2 0.364485 0.176315 0.243484 11.00000 -1.20000 AFIX 0 C63 1 0.200900 0.170777 0.092467 11.00000 0.03649 0.03373 = 0.04270 -0.00365 0.01397 0.00387 C64 1 0.088030 0.159002 0.051773 11.00000 0.03862 0.04879 = 0.04935 -0.00524 0.00858 -0.00157 AFIX 43 H64 2 0.026769 0.160936 -0.029097 11.00000 -1.20000 AFIX 0 C65 1 0.067099 0.144620 0.130371 11.00000 0.04164 0.05698 = 0.06905 0.00122 0.01439 -0.01154 AFIX 43 H65 2 -0.009927 0.137142 0.104284 11.00000 -1.20000 AFIX 0 C66 1 0.160253 0.141172 0.248597 11.00000 0.05081 0.04624 = 0.06267 0.00768 0.02904 -0.00590 AFIX 43 H66 2 0.147891 0.130752 0.299349 11.00000 -1.20000 AFIX 0 C31B 1 0.373926 0.209384 -0.042245 11.00000 0.04071 0.03514 = 0.03574 0.00273 0.01008 0.00803 N32B 3 0.361613 0.229395 -0.048376 11.00000 0.05054 0.03714 = 0.04856 0.00595 0.01801 0.00862 C33B 1 0.420636 0.239622 -0.116630 11.00000 0.06471 0.03782 = 0.06042 0.00717 0.02382 0.00501 AFIX 43 H33B 2 0.412245 0.253716 -0.122856 11.00000 -1.20000 AFIX 0 C34B 1 0.492971 0.229870 -0.177443 11.00000 0.04436 0.05114 = 0.05230 0.01521 0.01901 -0.00465 C35B 1 0.503001 0.209039 -0.173212 11.00000 0.04981 0.05912 = 0.04418 0.00295 0.02226 0.01250 AFIX 43 H35B 2 0.549878 0.202199 -0.215796 11.00000 -1.20000 AFIX 0 C36B 1 0.441697 0.198598 -0.104169 11.00000 0.05199 0.03316 = 0.04863 -0.00131 0.01981 0.00430 AFIX 43 H36B 2 0.445882 0.184459 -0.099301 11.00000 -1.20000 AFIX 0 MOLE 3 C1S 1 0.199488 0.079360 -0.093061 11.00000 0.13416 0.11354 = 0.11306 -0.05642 0.07316 -0.04085 AFIX 137 H1S1 2 0.106427 0.077780 -0.125849 11.00000 -1.50000 H1S2 2 0.222571 0.092052 -0.122068 11.00000 -1.50000 H1S3 2 0.229790 0.079274 -0.001858 11.00000 -1.50000 AFIX 0 C2S 1 0.260475 0.062415 -0.138263 11.00000 0.13680 0.12056 = 0.08311 -0.02626 0.06631 -0.04225 O1S 4 0.377676 0.056965 -0.090233 11.00000 0.08723 0.19092 = 0.09886 -0.02580 0.04699 -0.01973 O2S 4 0.183244 0.052825 -0.234902 11.00000 0.11322 0.08007 = 0.08087 -0.01142 0.04390 -0.00289 C3S 1 0.234533 0.037726 -0.298429 11.00000 0.08757 0.08886 = 0.08023 -0.01648 0.04566 0.00348 AFIX 23 H3S1 2 0.274027 0.026670 -0.240450 11.00000 -1.20000 H3S2 2 0.300892 0.043786 -0.326179 11.00000 -1.20000 AFIX 0 C4S 1 0.128406 0.029980 -0.407386 11.00000 0.11760 0.13183 = 0.08900 -0.03049 0.03162 0.02403 AFIX 137 H4S1 2 0.082605 0.041177 -0.458669 11.00000 -1.50000 H4S2 2 0.069469 0.022295 -0.378528 11.00000 -1.50000 H4S3 2 0.163033 0.021349 -0.456940 11.00000 -1.50000 HKLF 4 REM 12-009 is BrIO3:0.5(EtOAc) in P21/n [Z'=2] @ 40kV30mA - 0.80\%A REM R1 = 0.0747 for 10079 Fo > 4sig(Fo) and 0.1237 for all 15826 data REM 1047 parameters refined using 0 restraints END WGHT 0.0390 11.5172 REM Highest difference peak 0.685, deepest hole -0.830, 1-sigma level 0.072 Q1 1 0.9682 -0.0298 0.0191 11.00000 0.05 0.68 Q2 1 0.1576 0.0665 -0.2138 11.00000 0.05 0.59 Q3 1 0.7802 0.0025 -0.3234 11.00000 0.05 0.55 Q4 1 0.5422 0.2343 -0.3386 11.00000 0.05 0.51 Q5 1 0.1163 0.0985 -0.1351 11.00000 0.05 0.48 Q6 1 0.8024 -0.0259 -0.1038 11.00000 0.05 0.43 Q7 1 0.7644 -0.0050 -0.4344 11.00000 0.05 0.38 Q8 1 0.1161 0.2436 0.4607 11.00000 0.05 0.36 Q9 1 0.2627 0.2458 0.5802 11.00000 0.05 0.36 Q10 1 0.7679 0.2105 -0.2080 11.00000 0.05 0.36 Q11 1 0.8448 0.0141 -0.4023 11.00000 0.05 0.34 Q12 1 0.1887 0.1601 0.5342 11.00000 0.05 0.34 Q13 1 0.3059 0.0508 -0.1814 11.00000 0.05 0.33 Q14 1 0.0276 0.2151 0.5948 11.00000 0.05 0.33 Q15 1 0.6591 0.0718 -0.1730 11.00000 0.05 0.31 ; loop_ _geom_hbond_atom_site_label_D _geom_hbond_atom_site_label_H _geom_hbond_atom_site_label_A _geom_hbond_distance_DH _geom_hbond_distance_HA _geom_hbond_distance_DA _geom_hbond_angle_DHA _geom_hbond_site_symmetry_A _geom_hbond_publ_flag # # Hydrogen bonding scheme # ======== ======= ====== # # D H A D-H H...A D...A D-H...A symm publ # - - - --- ----- ----- ------- ---- ---- C15A H15A O5A 0.93 2.53 3.422(7) 161 3_655 yes C16A H16A O1S 0.93 2.44 3.333(9) 162 . yes C35A H35A O5A 0.93 2.44 3.219(8) 142 3_655 yes C35B H35B O3B 0.93 2.53 3.190(7) 128 1_554 yes C54 H54 O1A 0.93 2.40 3.142(7) 136 1_556 yes C1S H1S3 O4A 0.96 2.53 3.301(9) 138 . yes C4S H4S3 Br1A 0.96 2.69 3.643(8) 172 3_654 yes _database_code_depnum_ccdc_archive 'CCDC 930689' ####################################################################### # # Cambridge Crystallographic Data Centre # CCDC # ####################################################################### # # This CIF contains data from an original supplementary publication # deposited with the CCDC, and may include chemical, crystal, # experimental, refinement, atomic coordinates, # anisotropic displacement parameters and molecular geometry data, # as required by the journal to which it was submitted. # # This CIF is provided on the understanding that it is used for bona # fide research purposes only. It may contain copyright material # of the CCDC or of third parties, and may not be copied or further # disseminated in any form, whether machine-readable or not, # except for the purpose of generating routine backup copies # on your local computer system. # # For further information on the CCDC, data deposition and # data retrieval see: # www.ccdc.cam.ac.uk # # Bona fide researchers may freely download Mercury and enCIFer # from this site to visualise CIF-encoded structures and # to carry out CIF format checking respectively. # data_(BrIO)4_CHCl3_[12-005] #TrackingRef 'Bromo_JFG_v09.cif' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety 'C52 H28 Br4 N8 O8, 0.2(C4 H4 Cl12)' _chemical_formula_sum 'C52.80 H28.80 Br4 Cl2.40 N8 O8' _chemical_formula_weight 1307.96 loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source C C 0.0181 0.0091 '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' N N 0.0311 0.0180 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' O O 0.0492 0.0322 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Cl Cl 0.3639 0.7018 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Br Br -0.6763 1.2805 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting Orthorhombic _symmetry_space_group_name_H-M 'P c c n' _symmetry_space_group_name_Hall '-P 2ab 2ac' loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x+1/2, -y+1/2, z' '-x, y+1/2, -z+1/2' 'x+1/2, -y, -z+1/2' '-x, -y, -z' 'x-1/2, y-1/2, -z' 'x, -y-1/2, z-1/2' '-x-1/2, y, z-1/2' _cell_length_a 14.0441(4) _cell_length_b 19.1432(3) _cell_length_c 19.1482(4) _cell_angle_alpha 90.00 _cell_angle_beta 90.00 _cell_angle_gamma 90.00 _cell_volume 5148.0(2) _cell_formula_units_Z 4 _cell_measurement_temperature 294(2) _cell_measurement_reflns_used 10083 _cell_measurement_theta_min 3.14 _cell_measurement_theta_max 63.11 _exptl_crystal_description Needle _exptl_crystal_colour Colourless _exptl_crystal_size_max 0.35 _exptl_crystal_size_mid 0.13 _exptl_crystal_size_min 0.09 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.688 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 2585.6 _exptl_absorpt_coefficient_mu 5.498 _exptl_absorpt_correction_type Analytical _exptl_absorpt_correction_T_min 0.2492 _exptl_absorpt_correction_T_max 0.6375 _exptl_absorpt_process_details '(ABSFAC, Clark and Reid, 1998)' _exptl_special_details ; [12-005] One of the pyridinyl rings at C21A/C21B is 50:50% disordered as it cannot have both of the aromatic C-H atoms oriented towards one another with 100% occupancy and a H...H separation of 1.88 Angstroms. ; _diffrn_ambient_temperature 294(1) _diffrn_radiation_wavelength 1.54184 _diffrn_radiation_type CuK\a _diffrn_radiation_source 'Enhance (Cu) X-ray Source' _diffrn_radiation_monochromator graphite _diffrn_measurement_device 'Xcalibur, Sapphire3, Gemini Ultra' _diffrn_measurement_method '\w scans' _diffrn_standards_number 10083 _diffrn_standards_interval_time 60 _diffrn_standards_decay_% 1 _diffrn_reflns_number 30530 _diffrn_reflns_av_R_equivalents 0.0389 _diffrn_reflns_av_sigmaI/netI 0.0192 _diffrn_reflns_limit_h_min -15 _diffrn_reflns_limit_h_max 16 _diffrn_reflns_limit_k_min -20 _diffrn_reflns_limit_k_max 22 _diffrn_reflns_limit_l_min -19 _diffrn_reflns_limit_l_max 22 _diffrn_reflns_theta_min 3.90 _diffrn_reflns_theta_max 63.20 _diffrn_measured_fraction_theta_max 0.997 _diffrn_reflns_theta_full 63.20 _diffrn_measured_fraction_theta_full 0.997 _reflns_number_total 4178 _reflns_number_gt 3574 _reflns_threshold_expression I>2\s(I) _computing_data_collection ; CrysAlisPro, Agilent Technologies, Version 1.171.34.49 (release 20-01-2011 CrysAlis171 .NET) (compiled Jan 20 2011,15:58:25) ; _computing_cell_refinement ; CrysAlisPro, Agilent Technologies, Version 1.171.34.49 (release 20-01-2011 CrysAlis171 .NET) (compiled Jan 20 2011,15:58:25) ; _computing_data_reduction ; CrysAlisPro, Agilent Technologies, Version 1.171.34.49 (release 20-01-2011 CrysAlis171 .NET) (compiled Jan 20 2011,15:58:25) ; _computing_structure_solution 'SHELXS97 (Sheldrick, 2008)' _computing_structure_refinement 'SHELXL97 (Sheldrick, 2008) and SORTX (McArdle, 1995)' _computing_molecular_graphics 'PLATON (Spek, 2009)' _computing_publication_material SHELXL97 _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 'w=1/[\s^2^(Fo^2^)+(0.0576P)^2^+6.0P] 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 none _refine_ls_extinction_coef ? _refine_ls_number_reflns 4178 _refine_ls_number_parameters 457 _refine_ls_number_restraints 170 _refine_ls_R_factor_all 0.0516 _refine_ls_R_factor_gt 0.0440 _refine_ls_wR_factor_ref 0.1224 _refine_ls_wR_factor_gt 0.1154 _refine_ls_goodness_of_fit_ref 1.042 _refine_ls_restrained_S_all 1.057 _refine_ls_shift/su_max 0.001 _refine_ls_shift/su_mean 0.000 _refine_diff_density_max 0.967 _refine_diff_density_min -0.658 _refine_diff_density_rms 0.055 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 Br14 Br 0.64128(5) 0.36238(4) -0.28747(4) 0.1197(3) Uani 1 1 d . . . Br24 Br 0.11821(5) 0.52279(2) 0.11735(3) 0.0845(2) Uani 1 1 d . . . O1 O 0.1780(2) 0.4114(2) -0.28689(16) 0.0945(11) Uani 1 1 d . . . C1 C 0.1684(3) 0.3951(2) -0.2266(2) 0.0594(9) Uani 1 1 d . A . N1 N 0.2459(2) 0.40499(14) -0.17875(15) 0.0552(7) Uani 1 1 d . . . O2 O 0.1530(2) 0.47766(15) -0.11514(18) 0.0817(9) Uani 1 1 d . . . C2 C 0.2272(3) 0.44594(17) -0.11950(19) 0.0572(9) Uani 1 1 d . . . O3 O 0.0430(3) 0.19249(15) 0.10342(15) 0.0988(13) Uani 1 1 d . . . C3 C 0.0585(3) 0.18304(18) 0.04279(19) 0.0606(10) Uani 1 1 d . A . N2 N 0.0481(2) 0.23970(13) -0.00570(15) 0.0522(7) Uani 1 1 d . . . O4 O -0.0475(2) 0.17432(13) -0.07446(16) 0.0736(8) Uani 1 1 d . . . C4 C -0.0037(3) 0.22839(17) -0.06672(19) 0.0548(9) Uani 1 1 d . A . C11 C -0.0014(3) 0.28220(17) -0.12306(17) 0.0507(8) Uani 1 1 d . . . C12 C 0.0799(3) 0.31911(16) -0.14068(17) 0.0483(8) Uani 1 1 d . A . H12 H 0.1339 0.3160 -0.1127 0.058 Uiso 1 1 calc R . . C13 C 0.0809(3) 0.36073(17) -0.20010(17) 0.0501(8) Uani 1 1 d . . . C14 C -0.0013(3) 0.36657(18) -0.24020(18) 0.0561(9) Uani 1 1 d . A . H14 H -0.0010 0.3945 -0.2800 0.067 Uiso 1 1 calc R . . C15 C -0.0824(3) 0.3318(2) -0.2219(2) 0.0612(9) Uani 1 1 d . . . H15 H -0.1376 0.3373 -0.2482 0.073 Uiso 1 1 calc R A . C16 C -0.0822(3) 0.28846(19) -0.1641(2) 0.0586(9) Uani 1 1 d . A . H16 H -0.1367 0.2633 -0.1526 0.070 Uiso 1 1 calc R . . C11A C 0.3400(3) 0.39624(18) -0.20584(18) 0.0528(8) Uani 1 1 d . . . N12A N 0.4042(3) 0.44730(17) -0.19582(19) 0.0714(9) Uani 1 1 d . . . C13A C 0.4931(3) 0.4363(2) -0.2201(2) 0.0747(12) Uani 1 1 d . . . H13A H 0.5396 0.4702 -0.2131 0.090 Uiso 1 1 calc R . . C14A C 0.5163(3) 0.3760(2) -0.2549(2) 0.0678(11) Uani 1 1 d . . . C15A C 0.4479(4) 0.3261(2) -0.2660(2) 0.0727(12) Uani 1 1 d . . . H15A H 0.4621 0.2861 -0.2916 0.087 Uiso 1 1 calc R . . C16A C 0.3595(3) 0.33556(19) -0.2395(2) 0.0584(9) Uani 1 1 d . . . H16A H 0.3131 0.3012 -0.2442 0.070 Uiso 1 1 calc R . . C21 C 0.2020(3) 0.05494(16) -0.06253(18) 0.0520(8) Uani 1 1 d . . . C22 C 0.1550(3) 0.11587(16) -0.04317(18) 0.0507(8) Uani 1 1 d . A . H22 H 0.1626 0.1562 -0.0696 0.061 Uiso 1 1 calc R . . C23 C 0.0974(3) 0.11673(17) 0.01490(19) 0.0528(9) Uani 1 1 d . . . C24 C 0.0827(3) 0.05543(18) 0.0531(2) 0.0619(10) Uani 1 1 d . A . H24 H 0.0429 0.0558 0.0919 0.074 Uiso 1 1 calc R . . C25 C 0.1270(3) -0.00534(19) 0.0330(2) 0.0696(12) Uani 1 1 d . . . H25 H 0.1160 -0.0463 0.0578 0.084 Uiso 1 1 calc R A . C26 C 0.1872(3) -0.00594(18) -0.0230(2) 0.0658(11) Uani 1 1 d . A . H26 H 0.2186 -0.0470 -0.0351 0.079 Uiso 1 1 calc R . . C21A C 0.0737(14) 0.3086(8) 0.0270(10) 0.031(3) Uani 0.50 1 d PDU A -1 N22A N -0.0013(12) 0.3570(12) 0.0254(12) 0.041(3) Uani 0.50 1 d PDU A -1 C23A C 0.0182(15) 0.4234(10) 0.0543(12) 0.044(4) Uani 0.50 1 d PDU A -1 H23A H -0.0283 0.4580 0.0541 0.052 Uiso 0.50 1 calc PR A -1 C24A C 0.1055(18) 0.4362(17) 0.0826(16) 0.039(4) Uani 0.50 1 d PDU A -1 C25A C 0.1759(15) 0.3866(12) 0.0811(12) 0.040(3) Uani 0.50 1 d PDU A -1 H25A H 0.2352 0.3970 0.1000 0.048 Uiso 0.50 1 calc PR A -1 C26A C 0.1609(18) 0.3223(17) 0.0527(17) 0.044(4) Uani 0.50 1 d PDU A -1 H26A H 0.2092 0.2891 0.0510 0.053 Uiso 0.50 1 calc PR A -1 C21B C 0.0526(17) 0.3077(13) 0.0190(12) 0.048(5) Uani 0.50 1 d PDU A -2 N22B N 0.1409(15) 0.3194(15) 0.0465(14) 0.052(5) Uani 0.50 1 d PDU A -2 C23B C 0.1559(17) 0.3819(17) 0.0754(16) 0.060(5) Uani 0.50 1 d PDU A -2 H23B H 0.2140 0.3917 0.0965 0.072 Uiso 0.50 1 calc PR A -2 C24B C 0.085(2) 0.4320(19) 0.0739(18) 0.045(5) Uani 0.50 1 d PDU A -2 C25B C -0.0009(17) 0.4127(13) 0.0472(14) 0.055(5) Uani 0.50 1 d PDU A -2 H25B H -0.0498 0.4454 0.0484 0.066 Uiso 0.50 1 calc PR A -2 C26B C -0.0205(19) 0.3498(17) 0.0192(17) 0.055(5) Uani 0.50 1 d PDU A -2 H26B H -0.0800 0.3376 0.0018 0.066 Uiso 0.50 1 calc PR A -2 Cl1S Cl 0.832(2) 0.2008(15) 0.1064(12) 0.109(8) Uani 0.20 1 d PDU B -1 Cl2S Cl 0.718(2) 0.3132(10) 0.0406(14) 0.256(13) Uani 0.20 1 d PDU B -1 Cl3S Cl 0.7455(13) 0.2158(9) -0.0338(7) 0.114(6) Uani 0.20 1 d PDU B -1 C1S C 0.742(2) 0.2288(13) 0.0538(12) 0.14(2) Uani 0.20 1 d PDU B -1 H1S H 0.685(3) 0.207(2) 0.070(2) 0.170 Uiso 0.20 1 d PD C -1 Cl1T Cl 0.8157(18) 0.2032(14) 0.0960(12) 0.088(5) Uani 0.20 1 d PDU D -2 Cl2T Cl 0.6873(18) 0.3100(9) 0.0788(11) 0.099(6) Uani 0.20 1 d PDU D -2 Cl3T Cl 0.742(2) 0.1887(9) -0.0277(9) 0.116(5) Uani 0.20 1 d PDU D -2 C1T C 0.7159(18) 0.2311(12) 0.0473(11) 0.070(8) Uani 0.20 1 d PDU D -2 H1T H 0.667(3) 0.2003(18) 0.068(2) 0.085 Uiso 0.20 1 d PD E -2 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 Br14 0.0897(4) 0.1385(6) 0.1309(6) 0.0487(5) 0.0419(4) 0.0404(4) Br24 0.1242(5) 0.0480(3) 0.0813(3) -0.0224(2) 0.0080(3) -0.0039(2) O1 0.083(2) 0.141(3) 0.0599(19) 0.040(2) -0.0008(15) -0.006(2) C1 0.070(2) 0.056(2) 0.053(2) 0.0119(17) -0.0007(18) 0.0093(18) N1 0.0656(18) 0.0459(15) 0.0542(17) 0.0081(13) 0.0043(15) 0.0054(14) O2 0.083(2) 0.0602(17) 0.102(2) -0.0146(16) -0.0031(17) 0.0273(15) C2 0.072(2) 0.0351(16) 0.064(2) 0.0023(15) 0.0056(18) 0.0062(17) O3 0.192(4) 0.0511(16) 0.0529(17) 0.0042(13) 0.026(2) 0.009(2) C3 0.094(3) 0.0412(18) 0.047(2) 0.0034(15) 0.0080(19) -0.0011(18) N2 0.078(2) 0.0311(14) 0.0473(15) 0.0008(12) 0.0051(14) -0.0011(13) O4 0.094(2) 0.0455(15) 0.0812(19) 0.0044(13) -0.0120(16) -0.0169(14) C4 0.070(2) 0.0398(18) 0.054(2) -0.0002(15) 0.0031(18) -0.0001(16) C11 0.069(2) 0.0366(16) 0.0461(18) -0.0058(14) 0.0032(16) 0.0045(15) C12 0.060(2) 0.0388(16) 0.0463(18) -0.0016(14) -0.0021(15) 0.0076(15) C13 0.067(2) 0.0409(17) 0.0429(18) 0.0003(14) 0.0003(16) 0.0096(15) C14 0.077(3) 0.0492(19) 0.0423(19) 0.0007(15) -0.0025(17) 0.0079(18) C15 0.069(2) 0.061(2) 0.054(2) -0.0047(18) -0.0093(18) 0.0068(19) C16 0.065(2) 0.053(2) 0.058(2) -0.0076(17) 0.0001(18) -0.0021(17) C11A 0.068(2) 0.0424(18) 0.0476(19) 0.0087(15) 0.0025(17) 0.0049(16) N12A 0.083(2) 0.0515(19) 0.080(2) 0.0015(16) 0.0127(19) -0.0045(17) C13A 0.074(3) 0.062(2) 0.088(3) 0.009(2) 0.008(2) -0.009(2) C14A 0.070(3) 0.071(3) 0.062(2) 0.020(2) 0.012(2) 0.018(2) C15A 0.099(3) 0.051(2) 0.068(3) -0.0001(19) -0.010(2) 0.017(2) C16A 0.069(2) 0.0429(18) 0.063(2) 0.0016(16) -0.0082(19) 0.0058(17) C21 0.067(2) 0.0333(16) 0.055(2) 0.0005(14) -0.0114(17) 0.0002(15) C22 0.075(2) 0.0322(15) 0.0453(18) 0.0064(13) -0.0065(17) 0.0005(15) C23 0.073(2) 0.0340(16) 0.051(2) 0.0048(14) -0.0069(17) -0.0049(15) C24 0.090(3) 0.0426(19) 0.053(2) 0.0108(16) -0.0033(19) -0.0100(18) C25 0.103(3) 0.0342(18) 0.071(3) 0.0159(17) -0.006(2) -0.0097(19) C26 0.091(3) 0.0307(16) 0.076(3) 0.0035(17) -0.016(2) 0.0034(17) C21A 0.041(8) 0.013(4) 0.037(6) -0.007(3) -0.002(6) 0.003(4) N22A 0.033(6) 0.038(7) 0.052(5) -0.008(4) -0.010(4) 0.000(5) C23A 0.047(8) 0.025(5) 0.060(8) -0.009(5) 0.002(7) 0.003(6) C24A 0.051(9) 0.034(5) 0.032(6) -0.011(4) -0.005(6) -0.004(6) C25A 0.044(7) 0.035(5) 0.042(6) -0.003(4) -0.006(5) -0.004(5) C26A 0.040(7) 0.035(6) 0.057(7) 0.001(5) -0.006(6) 0.005(5) C21B 0.049(8) 0.060(8) 0.035(6) 0.009(4) -0.009(5) -0.009(5) N22B 0.054(10) 0.043(6) 0.058(7) -0.004(4) -0.005(7) 0.002(7) C23B 0.048(9) 0.066(9) 0.065(9) -0.005(6) -0.010(6) -0.009(6) C24B 0.048(9) 0.041(7) 0.045(10) -0.007(6) -0.005(7) -0.004(7) C25B 0.054(8) 0.051(8) 0.059(6) -0.008(6) -0.016(5) -0.013(6) C26B 0.056(10) 0.049(7) 0.061(8) -0.008(5) -0.005(7) -0.010(6) Cl1S 0.112(10) 0.130(14) 0.086(9) 0.028(10) -0.036(6) 0.007(9) Cl2S 0.28(2) 0.151(13) 0.33(3) 0.047(19) -0.09(2) -0.017(15) Cl3S 0.080(5) 0.198(19) 0.063(4) 0.025(6) 0.002(4) 0.002(15) C1S 0.16(4) 0.11(3) 0.16(3) -0.05(2) 0.01(3) 0.03(3) Cl1T 0.092(8) 0.104(12) 0.069(10) -0.047(9) -0.002(8) 0.001(7) Cl2T 0.111(11) 0.074(6) 0.111(15) 0.055(8) -0.039(10) -0.014(6) Cl3T 0.102(7) 0.119(8) 0.125(9) 0.045(6) -0.007(7) 0.007(6) C1T 0.037(9) 0.093(18) 0.081(17) -0.011(15) 0.000(10) -0.009(11) _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 Br14 C14A 1.881(4) . ? Br24 C24A 1.79(3) . ? Br24 C24B 1.98(3) . ? O1 C1 1.203(5) . ? C1 N1 1.436(5) . ? C1 C13 1.484(6) . ? N1 C2 1.404(5) . ? N1 C11A 1.430(5) . ? O2 C2 1.209(5) . ? C2 C21 1.476(5) 2 ? O3 C3 1.195(5) . ? C3 N2 1.435(4) . ? C3 C23 1.481(5) . ? N2 C21B 1.39(3) . ? N2 C4 1.393(5) . ? N2 C21A 1.503(16) . ? O4 C4 1.214(4) . ? C4 C11 1.492(5) . ? C11 C16 1.385(5) . ? C11 C12 1.385(5) . ? C12 C13 1.389(5) . ? C12 H12 0.9300 . ? C13 C14 1.391(5) . ? C14 C15 1.365(6) . ? C14 H14 0.9300 . ? C15 C16 1.384(5) . ? C15 H15 0.9300 . ? C16 H16 0.9300 . ? C11A N12A 1.343(5) . ? C11A C16A 1.356(5) . ? N12A C13A 1.349(6) . ? C13A C14A 1.372(6) . ? C13A H13A 0.9300 . ? C14A C15A 1.372(7) . ? C15A C16A 1.353(6) . ? C15A H15A 0.9300 . ? C16A H16A 0.9300 . ? C21 C22 1.390(5) . ? C21 C26 1.405(5) . ? C21 C2 1.476(5) 2 ? C22 C23 1.375(5) . ? C22 H22 0.9300 . ? C23 C24 1.398(5) . ? C24 C25 1.374(6) . ? C24 H24 0.9300 . ? C25 C26 1.365(6) . ? C25 H25 0.9300 . ? C26 H26 0.9300 . ? C21A C26A 1.35(3) . ? C21A N22A 1.40(2) . ? N22A C23A 1.41(2) . ? C23A C24A 1.36(2) . ? C23A H23A 0.9300 . ? C24A C25A 1.37(4) . ? C25A C26A 1.36(4) . ? C25A H25A 0.9300 . ? C26A H26A 0.9300 . ? C21B C26B 1.31(3) . ? C21B N22B 1.36(2) . ? N22B C23B 1.34(4) . ? C23B C24B 1.38(4) . ? C23B H23B 0.9300 . ? C24B C25B 1.37(2) . ? C25B C26B 1.35(3) . ? C25B H25B 0.9300 . ? C26B H26B 0.9300 . ? Cl1S C1S 1.707(18) . ? Cl2S C1S 1.668(19) . ? Cl2S Cl3S 2.38(3) . ? Cl3S C1S 1.696(19) . ? C1S H1S 0.96(2) . ? C1S H1T 1.21(5) . ? Cl1T C1T 1.766(19) . ? Cl2T C1T 1.675(17) . ? Cl3T C1T 1.691(17) . ? C1T H1S 0.77(4) . ? C1T H1T 0.988(19) . ? 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 O1 C1 N1 119.5(4) . . ? O1 C1 C13 122.4(4) . . ? N1 C1 C13 117.9(3) . . ? C2 N1 C11A 122.1(3) . . ? C2 N1 C1 116.6(3) . . ? C11A N1 C1 117.0(3) . . ? O2 C2 N1 119.8(4) . . ? O2 C2 C21 122.4(3) . 2 ? N1 C2 C21 117.7(3) . 2 ? O3 C3 N2 119.7(3) . . ? O3 C3 C23 123.2(3) . . ? N2 C3 C23 116.9(3) . . ? C21B N2 C4 117.1(10) . . ? C21B N2 C3 119.0(10) . . ? C4 N2 C3 118.6(3) . . ? C4 N2 C21A 127.6(8) . . ? C3 N2 C21A 111.6(8) . . ? O4 C4 N2 120.0(3) . . ? O4 C4 C11 120.8(3) . . ? N2 C4 C11 119.2(3) . . ? C16 C11 C12 119.6(3) . . ? C16 C11 C4 116.9(3) . . ? C12 C11 C4 123.1(3) . . ? C11 C12 C13 120.0(3) . . ? C11 C12 H12 120.0 . . ? C13 C12 H12 120.0 . . ? C12 C13 C14 119.4(3) . . ? C12 C13 C1 122.9(3) . . ? C14 C13 C1 117.6(3) . . ? C15 C14 C13 120.8(3) . . ? C15 C14 H14 119.6 . . ? C13 C14 H14 119.6 . . ? C14 C15 C16 119.7(4) . . ? C14 C15 H15 120.1 . . ? C16 C15 H15 120.1 . . ? C15 C16 C11 120.5(4) . . ? C15 C16 H16 119.8 . . ? C11 C16 H16 119.8 . . ? N12A C11A C16A 123.8(4) . . ? N12A C11A N1 118.9(3) . . ? C16A C11A N1 117.3(3) . . ? C11A N12A C13A 117.3(4) . . ? N12A C13A C14A 121.2(4) . . ? N12A C13A H13A 119.4 . . ? C14A C13A H13A 119.4 . . ? C13A C14A C15A 119.7(4) . . ? C13A C14A Br14 120.0(4) . . ? C15A C14A Br14 120.3(3) . . ? C16A C15A C14A 119.4(4) . . ? C16A C15A H15A 120.3 . . ? C14A C15A H15A 120.3 . . ? C15A C16A C11A 118.6(4) . . ? C15A C16A H16A 120.7 . . ? C11A C16A H16A 120.7 . . ? C22 C21 C26 118.8(4) . . ? C22 C21 C2 121.8(3) . 2 ? C26 C21 C2 119.3(3) . 2 ? C23 C22 C21 120.3(3) . . ? C23 C22 H22 119.8 . . ? C21 C22 H22 119.8 . . ? C22 C23 C24 120.0(3) . . ? C22 C23 C3 121.2(3) . . ? C24 C23 C3 118.5(3) . . ? C25 C24 C23 119.8(4) . . ? C25 C24 H24 120.1 . . ? C23 C24 H24 120.1 . . ? C26 C25 C24 120.5(3) . . ? C26 C25 H25 119.8 . . ? C24 C25 H25 119.8 . . ? C25 C26 C21 120.5(4) . . ? C25 C26 H26 119.7 . . ? C21 C26 H26 119.7 . . ? C26A C21A N22A 124.2(18) . . ? C26A C21A N2 122.7(19) . . ? N22A C21A N2 113.0(15) . . ? C21A N22A C23A 116.1(15) . . ? C24A C23A N22A 119.5(19) . . ? C24A C23A H23A 120.3 . . ? N22A C23A H23A 120.3 . . ? C23A C24A C25A 121(2) . . ? C23A C24A Br24 114(2) . . ? C25A C24A Br24 125.2(17) . . ? C26A C25A C24A 122(2) . . ? C26A C25A H25A 119.2 . . ? C24A C25A H25A 119.2 . . ? C21A C26A C25A 118(2) . . ? C21A C26A H26A 121.2 . . ? C25A C26A H26A 121.2 . . ? C26B C21B N22B 128(2) . . ? C26B C21B N2 123(2) . . ? N22B C21B N2 109(2) . . ? C23B N22B C21B 117(2) . . ? N22B C23B C24B 120(2) . . ? N22B C23B H23B 120.0 . . ? C24B C23B H23B 120.0 . . ? C25B C24B C23B 117(3) . . ? C25B C24B Br24 127(2) . . ? C23B C24B Br24 115.7(18) . . ? C26B C25B C24B 125(3) . . ? C26B C25B H25B 117.5 . . ? C24B C25B H25B 117.5 . . ? C21B C26B C25B 113(2) . . ? C21B C26B H26B 123.5 . . ? C25B C26B H26B 123.5 . . ? Cl2S C1S Cl3S 89.8(16) . . ? Cl2S C1S Cl1S 122.6(19) . . ? Cl3S C1S Cl1S 120.9(18) . . ? Cl2S C1S H1S 108(3) . . ? Cl3S C1S H1S 106(3) . . ? Cl1S C1S H1S 107(2) . . ? Cl2S C1S H1T 108(3) . . ? Cl3S C1S H1T 101(3) . . ? Cl1S C1S H1T 112(3) . . ? Cl2T C1T Cl3T 142.2(18) . . ? Cl2T C1T Cl1T 105.9(15) . . ? Cl3T C1T Cl1T 97.5(15) . . ? Cl2T C1T H1S 102(4) . . ? Cl3T C1T H1S 108(4) . . ? Cl1T C1T H1S 89(4) . . ? Cl2T C1T H1T 103(2) . . ? Cl3T C1T H1T 102(2) . . ? Cl1T C1T H1T 99(3) . . ? 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 O1 C1 N1 C2 123.6(4) . . . . ? C13 C1 N1 C2 -60.2(4) . . . . ? O1 C1 N1 C11A -33.6(5) . . . . ? C13 C1 N1 C11A 142.6(3) . . . . ? C11A N1 C2 O2 147.0(4) . . . . ? C1 N1 C2 O2 -9.0(5) . . . . ? C11A N1 C2 C21 -36.5(4) . . . 2 ? C1 N1 C2 C21 167.5(3) . . . 2 ? O3 C3 N2 C21B 21.9(13) . . . . ? C23 C3 N2 C21B -152.4(12) . . . . ? O3 C3 N2 C4 -131.6(5) . . . . ? C23 C3 N2 C4 54.1(5) . . . . ? O3 C3 N2 C21A 33.0(10) . . . . ? C23 C3 N2 C21A -141.3(8) . . . . ? C21B N2 C4 O4 -145.8(11) . . . . ? C3 N2 C4 O4 8.1(5) . . . . ? C21A N2 C4 O4 -153.7(10) . . . . ? C21B N2 C4 C11 36.4(12) . . . . ? C3 N2 C4 C11 -169.6(3) . . . . ? C21A N2 C4 C11 28.6(10) . . . . ? O4 C4 C11 C16 33.1(5) . . . . ? N2 C4 C11 C16 -149.2(3) . . . . ? O4 C4 C11 C12 -139.2(4) . . . . ? N2 C4 C11 C12 38.5(5) . . . . ? C16 C11 C12 C13 -1.6(5) . . . . ? C4 C11 C12 C13 170.5(3) . . . . ? C11 C12 C13 C14 2.0(5) . . . . ? C11 C12 C13 C1 -172.7(3) . . . . ? O1 C1 C13 C12 155.4(4) . . . . ? N1 C1 C13 C12 -20.7(5) . . . . ? O1 C1 C13 C14 -19.4(6) . . . . ? N1 C1 C13 C14 164.4(3) . . . . ? C12 C13 C14 C15 -0.1(5) . . . . ? C1 C13 C14 C15 174.9(3) . . . . ? C13 C14 C15 C16 -2.1(6) . . . . ? C14 C15 C16 C11 2.6(6) . . . . ? C12 C11 C16 C15 -0.7(5) . . . . ? C4 C11 C16 C15 -173.2(3) . . . . ? C2 N1 C11A N12A -28.3(5) . . . . ? C1 N1 C11A N12A 127.6(4) . . . . ? C2 N1 C11A C16A 150.7(3) . . . . ? C1 N1 C11A C16A -53.4(4) . . . . ? C16A C11A N12A C13A -1.0(6) . . . . ? N1 C11A N12A C13A 177.9(3) . . . . ? C11A N12A C13A C14A 1.4(6) . . . . ? N12A C13A C14A C15A 0.7(7) . . . . ? N12A C13A C14A Br14 -179.6(3) . . . . ? C13A C14A C15A C16A -3.2(6) . . . . ? Br14 C14A C15A C16A 177.1(3) . . . . ? C14A C15A C16A C11A 3.6(6) . . . . ? N12A C11A C16A C15A -1.6(6) . . . . ? N1 C11A C16A C15A 179.6(3) . . . . ? C26 C21 C22 C23 1.9(5) . . . . ? C2 C21 C22 C23 -172.8(3) 2 . . . ? C21 C22 C23 C24 -2.7(6) . . . . ? C21 C22 C23 C3 170.5(4) . . . . ? O3 C3 C23 C22 -148.6(5) . . . . ? N2 C3 C23 C22 25.5(6) . . . . ? O3 C3 C23 C24 24.7(7) . . . . ? N2 C3 C23 C24 -161.1(4) . . . . ? C22 C23 C24 C25 1.0(6) . . . . ? C3 C23 C24 C25 -172.4(4) . . . . ? C23 C24 C25 C26 1.5(7) . . . . ? C24 C25 C26 C21 -2.3(7) . . . . ? C22 C21 C26 C25 0.6(6) . . . . ? C2 C21 C26 C25 175.5(4) 2 . . . ? C21B N2 C21A C26A -171(9) . . . . ? C4 N2 C21A C26A -136.3(18) . . . . ? C3 N2 C21A C26A 61(2) . . . . ? C21B N2 C21A N22A 7(7) . . . . ? C4 N2 C21A N22A 41.5(17) . . . . ? C3 N2 C21A N22A -121.4(13) . . . . ? C26A C21A N22A C23A -1(3) . . . . ? N2 C21A N22A C23A -179.1(17) . . . . ? C21A N22A C23A C24A -1(3) . . . . ? N22A C23A C24A C25A 2(4) . . . . ? N22A C23A C24A Br24 -179.7(18) . . . . ? C24B Br24 C24A C23A -6(12) . . . . ? C24B Br24 C24A C25A 172(17) . . . . ? C23A C24A C25A C26A -1(4) . . . . ? Br24 C24A C25A C26A -179(2) . . . . ? N22A C21A C26A C25A 3(3) . . . . ? N2 C21A C26A C25A 180(2) . . . . ? C24A C25A C26A C21A -1(3) . . . . ? C4 N2 C21B C26B 41(3) . . . . ? C3 N2 C21B C26B -113(2) . . . . ? C21A N2 C21B C26B -169(9) . . . . ? C4 N2 C21B N22B -143.2(14) . . . . ? C3 N2 C21B N22B 62.9(18) . . . . ? C21A N2 C21B N22B 6(7) . . . . ? C26B C21B N22B C23B -2(3) . . . . ? N2 C21B N22B C23B -177(2) . . . . ? C21B N22B C23B C24B -3(3) . . . . ? N22B C23B C24B C25B 5(4) . . . . ? N22B C23B C24B Br24 -179(2) . . . . ? C24A Br24 C24B C25B 170(17) . . . . ? C24A Br24 C24B C23B -5(12) . . . . ? C23B C24B C25B C26B -4(5) . . . . ? Br24 C24B C25B C26B -179(3) . . . . ? N22B C21B C26B C25B 4(4) . . . . ? N2 C21B C26B C25B 178(2) . . . . ? C24B C25B C26B C21B -1(4) . . . . ? Cl3S Cl2S C1S Cl1S 127(3) . . . . ? Cl2S Cl3S C1S Cl1S -129(3) . . . . ? _iucr_refine_instructions_details ; TITL 12-005 is BrIO4:CHCl3 in Pccn @ 40kV30mA to 0.88\%A [12-004] CELL 1.54184 14.0441 19.1432 19.1482 90.000 90.000 90.000 ZERR 4 0.0004 0.0003 0.0004 0.000 0.000 0.000 LATT 1 SYMM 1/2-X,1/2-Y,Z SYMM -X,1/2+Y,1/2-Z SYMM 1/2+X,-Y,1/2-Z SFAC C H N O CL BR UNIT 211.2 115.2 32 32 9.6 16 MERG 3 FMAP 2 L.S. 10 3 LIST 4 ACTA 127 CONF BOND $H DELU 0.015 C21A N22A C23A C24A C25A C26A ISOR 0.015 C21A N22A C23A C24A C25A C26A FLAT 0.200 C21A N22A C23A C24A C25A C26A DELU 0.015 C21B N22B C23B C24B C25B C26B ISOR 0.015 C21B N22B C23B C24B C25B C26B FLAT 0.200 C21B N22B C23B C24B C25B C26B ISOR 0.030 CL1S CL2S CL3S C1S CL1T CL2T CL3T C1T EQIV $1 -X,1-Y,-Z EQIV $2 1/2-X,Y,1/2+Z EQIV $3 1/2-X,1/2-Y,Z HTAB HTAB C22 N2 HTAB C23A O2_$1 HTAB C23B O1_$2 HTAB C23A O2_$1 HTAB C26A N22B_$3 RTAB XX BR14 BR24 RTAB XX BR14 BR14_$3 RTAB XX BR24 BR24_$3 RTAB XX BR14 BR24_$3 RTAB XX BR14_$3 BR24 RTAB XX BR14_$3 BR24_$3 RTAB OO O1 O2 RTAB OO O3 O4 RTAB OO O1 O4 RTAB OO O2 O3 RTAB NN N1 N2 RTAB NN N1 N1_$3 RTAB NN N2 N2_$3 RTAB NN N1 N2_$3 RTAB NN N1_$3 N2 RTAB NN N1_$3 N2_$3 RTAB NN N12A N22A RTAB NC N22B N22B_$3 RTAB NC C26A C26A_$3 RTAB NC N22B C26A_$3 RTAB NC C26A_$3 N22B RTAB NC C16A C16A_$3 RTAB OCCO O1 C1 C2 O2 RTAB OCCO O3 C3 C4 O4 RTAB OCCO O1 C1 C4 O4 RTAB OCCO O2 C2 C3_$3 O3_$3 RTAB CCNC C13 C1 N1 C2 RTAB CCNC C23 C3 N2 C4 RTAB CNCC C1 N1 C2 C21 RTAB CNCC C3 N2 C4 C11 RTAB OCNC O1 C1 N1 C2 RTAB OCNC O3 C3 N2 C4 RTAB CNCO C1 N1 C2 O2 RTAB CNCO C3 N2 C4 O4 RTAB CNCN C1 N1 C11A N12A RTAB CNCN C3 N2 C21A N22A SIZE 0.09 0.13 0.35 TEMP 21 PLAN 10 MPLA 3 C1 C2 C11A N1 MPLA 3 C3 C4 C21A N2 MPLA 6 C11 C12 C13 C14 C15 C16 MPLA 6 O1 O2 C1 C2 N1 MPLA 6 C21 C22 C23 C24 C25 C26 MPLA 6 C11A N12A C13A C14A C15A C16A BR14 MPLA 5 O1 N1 C1 C11 C21A MPLA 6 C21A N22A C23A C24A C25A C26A BR24 MPLA 6 C21B N22B C23B C24B C25B C26B BR24 MPLA 5 O3 O4 C3 C4 N2 MPLA 6 C21A N22A C23A C24A C25A C26A MPLA 6 C11 C12 C13 C14 C15 C16 BR14 BR24 MPLA 6 C21 C22 C23 C24 C25 C26 BR14 BR24 WGHT 0.057600 6.000000 FVAR 1.96185 MOLE 1 BR14 6 0.641277 0.362384 -0.287473 11.00000 0.08973 0.13851 = 0.13095 0.04872 0.04192 0.04037 BR24 6 0.118208 0.522790 0.117355 11.00000 0.12424 0.04795 = 0.08130 -0.02242 0.00804 -0.00390 O1 4 0.177990 0.411430 -0.286894 11.00000 0.08273 0.14081 = 0.05992 0.04046 -0.00078 -0.00580 C1 1 0.168368 0.395118 -0.226623 11.00000 0.07009 0.05560 = 0.05256 0.01194 -0.00072 0.00929 N1 3 0.245887 0.404986 -0.178752 11.00000 0.06564 0.04586 = 0.05422 0.00812 0.00428 0.00539 O2 4 0.153026 0.477657 -0.115138 11.00000 0.08273 0.06018 = 0.10211 -0.01458 -0.00305 0.02728 C2 1 0.227197 0.445940 -0.119503 11.00000 0.07237 0.03513 = 0.06416 0.00228 0.00562 0.00619 O3 4 0.043009 0.192490 0.103419 11.00000 0.19248 0.05105 = 0.05293 0.00422 0.02606 0.00879 C3 1 0.058527 0.183036 0.042787 11.00000 0.09367 0.04118 = 0.04681 0.00343 0.00795 -0.00113 N2 3 0.048092 0.239697 -0.005697 11.00000 0.07820 0.03105 = 0.04730 0.00077 0.00511 -0.00108 O4 4 -0.047524 0.174318 -0.074465 11.00000 0.09413 0.04552 = 0.08119 0.00441 -0.01203 -0.01691 C4 1 -0.003687 0.228394 -0.066717 11.00000 0.07027 0.03979 = 0.05427 -0.00024 0.00308 -0.00006 C11 1 -0.001415 0.282202 -0.123064 11.00000 0.06948 0.03661 = 0.04607 -0.00580 0.00316 0.00452 C12 1 0.079922 0.319106 -0.140683 11.00000 0.05997 0.03878 = 0.04626 -0.00164 -0.00209 0.00756 AFIX 43 H12 2 0.133918 0.316019 -0.112737 11.00000 -1.20000 AFIX 0 C13 1 0.080854 0.360735 -0.200101 11.00000 0.06659 0.04091 = 0.04288 0.00032 0.00025 0.00957 C14 1 -0.001312 0.366569 -0.240200 11.00000 0.07668 0.04921 = 0.04231 0.00068 -0.00248 0.00790 AFIX 43 H14 2 -0.000989 0.394471 -0.279958 11.00000 -1.20000 AFIX 0 C15 1 -0.082440 0.331825 -0.221897 11.00000 0.06870 0.06093 = 0.05390 -0.00467 -0.00934 0.00679 AFIX 43 H15 2 -0.137635 0.337268 -0.248175 11.00000 -1.20000 AFIX 0 C16 1 -0.082194 0.288456 -0.164052 11.00000 0.06517 0.05273 = 0.05805 -0.00764 0.00006 -0.00208 AFIX 43 H16 2 -0.136690 0.263331 -0.152632 11.00000 -1.20000 AFIX 0 C11A 1 0.340019 0.396242 -0.205844 11.00000 0.06828 0.04244 = 0.04765 0.00868 0.00246 0.00489 N12A 3 0.404192 0.447302 -0.195822 11.00000 0.08266 0.05148 = 0.08016 0.00150 0.01265 -0.00445 C13A 1 0.493108 0.436315 -0.220085 11.00000 0.07378 0.06191 = 0.08845 0.00933 0.00808 -0.00867 AFIX 43 H13A 2 0.539550 0.470228 -0.213075 11.00000 -1.20000 AFIX 0 C14A 1 0.516301 0.376046 -0.254907 11.00000 0.07028 0.07122 = 0.06202 0.02028 0.01211 0.01783 C15A 1 0.447852 0.326109 -0.266043 11.00000 0.09923 0.05109 = 0.06772 -0.00015 -0.01045 0.01729 AFIX 43 H15A 2 0.462061 0.286141 -0.291611 11.00000 -1.20000 AFIX 0 C16A 1 0.359502 0.335556 -0.239484 11.00000 0.06875 0.04288 = 0.06349 0.00160 -0.00822 0.00584 AFIX 43 H16A 2 0.313148 0.301184 -0.244194 11.00000 -1.20000 AFIX 0 PART 0 C21 1 0.202002 0.054941 -0.062531 11.00000 0.06743 0.03335 = 0.05525 0.00048 -0.01137 0.00019 C22 1 0.155016 0.115867 -0.043166 11.00000 0.07458 0.03222 = 0.04526 0.00640 -0.00649 0.00048 AFIX 43 H22 2 0.162589 0.156235 -0.069612 11.00000 -1.20000 AFIX 0 C23 1 0.097399 0.116731 0.014903 11.00000 0.07339 0.03404 = 0.05095 0.00483 -0.00690 -0.00488 C24 1 0.082664 0.055433 0.053052 11.00000 0.09006 0.04264 = 0.05312 0.01084 -0.00330 -0.00999 AFIX 43 H24 2 0.042936 0.055764 0.091907 11.00000 -1.20000 AFIX 0 C25 1 0.127034 -0.005341 0.033003 11.00000 0.10334 0.03424 = 0.07130 0.01595 -0.00562 -0.00974 AFIX 43 H25 2 0.116004 -0.046344 0.057764 11.00000 -1.20000 AFIX 0 C26 1 0.187151 -0.005939 -0.022975 11.00000 0.09090 0.03073 = 0.07586 0.00350 -0.01554 0.00338 AFIX 43 H26 2 0.218557 -0.046967 -0.035054 11.00000 -1.20000 AFIX 0 PART -1 C21A 1 0.073659 0.308551 0.027013 10.50000 0.04126 0.01304 = 0.03739 -0.00713 -0.00190 0.00280 N22A 3 -0.001283 0.356974 0.025383 10.50000 0.03333 0.03845 = 0.05161 -0.00791 -0.00997 -0.00031 C23A 1 0.018165 0.423354 0.054341 10.50000 0.04661 0.02465 = 0.05981 -0.00851 0.00240 0.00270 AFIX 43 H23A 2 -0.028271 0.457987 0.054145 10.50000 -1.20000 AFIX 0 C24A 1 0.105544 0.436224 0.082571 10.50000 0.05094 0.03351 = 0.03190 -0.01101 -0.00460 -0.00400 C25A 1 0.175869 0.386553 0.081143 10.50000 0.04372 0.03537 = 0.04200 -0.00348 -0.00579 -0.00434 AFIX 43 H25A 2 0.235183 0.396994 0.100048 10.50000 -1.20000 AFIX 0 C26A 1 0.160871 0.322261 0.052674 10.50000 0.03994 0.03525 = 0.05732 0.00150 -0.00618 0.00515 AFIX 43 H26A 2 0.209159 0.289057 0.051037 10.50000 -1.20000 AFIX 0 PART -2 C21B 1 0.052607 0.307738 0.019020 10.50000 0.04855 0.06046 = 0.03536 0.00890 -0.00936 -0.00858 N22B 3 0.140866 0.319382 0.046475 10.50000 0.05410 0.04326 = 0.05760 -0.00394 -0.00515 0.00183 C23B 1 0.155945 0.381923 0.075382 10.50000 0.04837 0.06593 = 0.06543 -0.00453 -0.00963 -0.00896 AFIX 43 H23B 2 0.214045 0.391690 0.096541 10.50000 -1.20000 AFIX 0 C24B 1 0.085402 0.432009 0.073861 10.50000 0.04848 0.04139 = 0.04540 -0.00708 -0.00540 -0.00402 C25B 1 -0.000926 0.412673 0.047172 10.50000 0.05422 0.05107 = 0.05923 -0.00756 -0.01580 -0.01293 AFIX 43 H25B 2 -0.049803 0.445426 0.048441 10.50000 -1.20000 AFIX 0 C26B 1 -0.020515 0.349824 0.019202 10.50000 0.05580 0.04874 = 0.06140 -0.00802 -0.00521 -0.01037 AFIX 43 H26B 2 -0.080049 0.337617 0.001785 10.50000 -1.20000 AFIX 0 MOLE 2 PART -1 CL1S 5 0.832104 0.200776 0.106360 10.20000 0.11189 0.13007 = 0.08605 0.02756 -0.03582 0.00675 CL2S 5 0.718441 0.313193 0.040568 10.20000 0.28384 0.15132 = 0.33416 0.04712 -0.08605 -0.01749 CL3S 5 0.745472 0.215832 -0.033757 10.20000 0.07982 0.19811 = 0.06280 0.02456 0.00162 0.00154 C1S 1 0.741575 0.228753 0.053824 10.20000 0.15686 0.10980 = 0.15772 -0.04974 0.01210 0.02850 H1S 2 0.684534 0.206768 0.069875 10.20000 -1.20000 PART -2 CL1T 5 0.815737 0.203231 0.096043 10.20000 0.09153 0.10425 = 0.06934 -0.04701 -0.00172 0.00069 CL2T 5 0.687295 0.309989 0.078765 10.20000 0.11145 0.07420 = 0.11088 0.05513 -0.03873 -0.01441 CL3T 5 0.742109 0.188713 -0.027699 10.20000 0.10204 0.11946 = 0.12500 0.04532 -0.00685 0.00669 C1T 1 0.715907 0.231096 0.047346 10.20000 0.03715 0.09318 = 0.08106 -0.01087 -0.00009 -0.00867 H1T 2 0.667165 0.200268 0.068156 10.20000 -1.20000 PART 0 DFIX 1.75 0.02 C1S CL1S C1S CL2S C1S CL3S DFIX 0.98 0.02 C1S H1S DFIX 2.15 0.03 H1S CL1S H1S CL2S H1S CL3S DFIX 1.75 0.02 C1T CL1T C1T CL2T C1T CL3T DFIX 0.98 0.02 C1T H1T DFIX 2.15 0.03 H1T CL1T H1T CL2T H1T CL3T DFIX 2.85 0.05 CL1S CL2S CL1S CL3S CL2S CL3S DFIX 2.85 0.05 CL1T CL2T CL1T CL3T CL2T CL3T HKLF 4 REM 12-005 is BrIO4:CHCl3 in Pccn @ 40kV30mA to 0.88\%A [12-004] REM R1 = 0.0440 for 3574 Fo > 4sig(Fo) and 0.0516 for all 4178 data REM 457 parameters refined using 170 restraints END WGHT 0.0576 6.0617 REM Highest difference peak 0.967, deepest hole -0.658, 1-sigma level 0.055 Q1 1 0.6626 0.3782 -0.2380 11.00000 0.05 0.97 Q2 1 0.1162 0.5304 0.0675 11.00000 0.05 0.37 Q3 1 0.1802 0.5180 0.1310 11.00000 0.05 0.35 Q4 1 0.7500 0.2500 0.0103 10.50000 0.05 0.29 Q5 1 0.1984 0.3618 -0.2907 11.00000 0.05 0.27 Q6 1 0.0824 0.5185 0.1711 11.00000 0.05 0.25 Q7 1 0.3472 0.3596 -0.2331 11.00000 0.05 0.22 Q8 1 0.5814 0.3597 -0.2892 11.00000 0.05 0.22 Q9 1 0.3744 0.3440 -0.2584 11.00000 0.05 0.21 Q10 1 0.6794 0.2550 0.0440 11.00000 0.05 0.20 ; loop_ _geom_hbond_atom_site_label_D _geom_hbond_atom_site_label_H _geom_hbond_atom_site_label_A _geom_hbond_distance_DH _geom_hbond_distance_HA _geom_hbond_distance_DA _geom_hbond_angle_DHA _geom_hbond_site_symmetry_A _geom_hbond_publ_flag # # Hydrogen bonding scheme # ======== ======= ====== # # D H A D-H H...A D...A D-H...A symm publ # - - - --- ----- ----- ------- ---- ---- C22 H22 N2 0.93 2.58 2.896(4) 101 . yes C23A H23A O2 0.93 2.44 3.275(19) 150 5_565 yes C23A H23A O2 0.93 2.44 3.275(19) 150 5_565 yes _database_code_depnum_ccdc_archive 'CCDC 930690' ####################################################################### # # Cambridge Crystallographic Data Centre # CCDC # ####################################################################### # # This CIF contains data from an original supplementary publication # deposited with the CCDC, and may include chemical, crystal, # experimental, refinement, atomic coordinates, # anisotropic displacement parameters and molecular geometry data, # as required by the journal to which it was submitted. # # This CIF is provided on the understanding that it is used for bona # fide research purposes only. It may contain copyright material # of the CCDC or of third parties, and may not be copied or further # disseminated in any form, whether machine-readable or not, # except for the purpose of generating routine backup copies # on your local computer system. # # For further information on the CCDC, data deposition and # data retrieval see: # www.ccdc.cam.ac.uk # # Bona fide researchers may freely download Mercury and enCIFer # from this site to visualise CIF-encoded structures and # to carry out CIF format checking respectively. # data_A_[11-124] #TrackingRef 'Bromo_JFG_v09.cif' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common 11-124_(26BrIO)3_2CHCl3 _chemical_melting_point ? _chemical_formula_moiety 'C36 H18 Br3 N9 O6, 2(C H Cl3)' _chemical_formula_sum 'C38 H20 Br3 Cl6 N9 O6' _chemical_formula_weight 1151.06 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' N N 0.0061 0.0033 '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' Cl Cl 0.1484 0.1585 '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 Triclinic _symmetry_space_group_name_H-M 'P -1' _symmetry_space_group_name_Hall '-P 1' loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, -y, -z' _cell_length_a 12.8150(6) _cell_length_b 13.6159(5) _cell_length_c 25.7452(11) _cell_angle_alpha 84.442(3) _cell_angle_beta 87.666(4) _cell_angle_gamma 80.070(4) _cell_volume 4402.8(3) _cell_formula_units_Z 4 _cell_measurement_temperature 294(2) _cell_measurement_reflns_used 5231 _cell_measurement_theta_min 2.10 _cell_measurement_theta_max 27.7 _exptl_crystal_description Plate _exptl_crystal_colour Colourless _exptl_crystal_size_max 0.34 _exptl_crystal_size_mid 0.17 _exptl_crystal_size_min 0.04 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.737 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 2264 _exptl_absorpt_coefficient_mu 3.170 _exptl_absorpt_correction_type Analytical _exptl_absorpt_correction_T_min 0.4121 _exptl_absorpt_correction_T_max 0.8837 _exptl_absorpt_process_details '(ABSFAC, Clark and Reid, 1998)' _exptl_special_details ; [11-124] C-Br...O=C short contacts Distance X...O 3.036(4) Br1A...O4A_$1 2.955(4) Br1B...O4B_$2 Angle C--X...O 150.9(2) C14A--Br1A...O4A_$1 171.9(3) C14B--Br1B...O4B_$2 Angle X...O=C 97.0(4) Br1A...(O4A--C4A)_$1 113.2(4) Br1B...(O4B--C4B)_$2 The symmetry codes $1 and $2 are detailed in the 11-124.res file in the '_iucr_refine_instructions_details' section below. #================================================================= Analysis of Short Non-Hydrogen Inter-Molecular Contacts For Inter- Molecular Clusters and/or Networks #================================================================= Contact-Nr Atom I[ ARU ] Atom J[ ARU ] d(I-J) Del #------------------------------------------------------------------ 1 Br(1A)[ 1555.01] ... O(4A) [ 1545.01] = 3.036 -0.33 2 O(1A) [ 1555.01] ... C(3S) [ 1555.05] = 3.004 -0.22 3 O(4A) [ 1555.01] ... Br(1A)[ 1565.01] = 3.036 -0.33 4 O(6A) [ 1555.01] ... Cl(2C)[ 1455.05] = 3.004 -0.27 5 C(33A)[ 1555.01] ... Cl(1C)[ 2655.05] = 3.246 -0.20 6 Br(1B)[ 1555.02] ... O(4B) [ 1565.02] = 2.955 -0.41 7 O(4B) [ 1555.02] ... Br(1B)[ 1545.02] = 2.955 -0.42 8 Cl(1C)[ 1555.05] ... C(33A)[ 2655.01] = 3.246 -0.20 9 Cl(2C)[ 1555.05] ... O(6A) [ 1655.01] = 3.004 -0.27 10 C(3S) [ 1555.05] ... O(1A) [ 1555.01] = 3.004 -0.22 ; _diffrn_ambient_temperature 294(1) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'Enhance (Mo) X-ray Source' _diffrn_radiation_monochromator graphite _diffrn_measurement_device 'Xcalibur, Sapphire3, Gemini Ultra' _diffrn_measurement_method '\w scans' _diffrn_standards_number 5231 _diffrn_standards_interval_time 60 _diffrn_standards_decay_% 1 _diffrn_reflns_number 38013 _diffrn_reflns_av_R_equivalents 0.0579 _diffrn_reflns_av_sigmaI/netI 0.1303 _diffrn_reflns_limit_h_min -16 _diffrn_reflns_limit_h_max 16 _diffrn_reflns_limit_k_min -17 _diffrn_reflns_limit_k_max 15 _diffrn_reflns_limit_l_min -29 _diffrn_reflns_limit_l_max 33 _diffrn_reflns_theta_min 2.10 _diffrn_reflns_theta_max 27.77 _diffrn_measured_fraction_theta_max 0.913 _diffrn_reflns_theta_full 26.00 _diffrn_measured_fraction_theta_full 0.999 _reflns_number_total 18957 _reflns_number_gt 8469 _reflns_threshold_expression I>2\s(I) _computing_data_collection ; CrysAlisPro, Agilent Technologies, Version 1.171.34.49 (release 20-01-2011 CrysAlis171 .NET) (compiled Jan 20 2011,15:58:25) ; _computing_cell_refinement ; CrysAlisPro, Agilent Technologies, Version 1.171.34.49 (release 20-01-2011 CrysAlis171 .NET) (compiled Jan 20 2011,15:58:25) ; _computing_data_reduction ; CrysAlisPro, Agilent Technologies, Version 1.171.34.49 (release 20-01-2011 CrysAlis171 .NET) (compiled Jan 20 2011,15:58:25) ; _computing_structure_solution 'SHELXS97 (Sheldrick, 2008)' _computing_structure_refinement 'SHELXL97 (Sheldrick, 2008) and SORTX (McArdle, 1995)' _computing_molecular_graphics 'PLATON (Spek, 2009)' _computing_publication_material SHELXL97 _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 'w=1/[\s^2^(Fo^2^)+(0.0601P)^2^+2.4788P] 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 constr _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 18957 _refine_ls_number_parameters 1153 _refine_ls_number_restraints 30 _refine_ls_R_factor_all 0.1883 _refine_ls_R_factor_gt 0.0793 _refine_ls_wR_factor_ref 0.1931 _refine_ls_wR_factor_gt 0.1463 _refine_ls_goodness_of_fit_ref 1.012 _refine_ls_restrained_S_all 1.012 _refine_ls_shift/su_max 0.001 _refine_ls_shift/su_mean 0.000 _refine_diff_density_max 1.263 _refine_diff_density_min -1.190 _refine_diff_density_rms 0.085 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 Br1A Br 0.29221(8) -0.32192(6) 0.18503(4) 0.0769(3) Uani 1 1 d . . . Br2A Br 0.14753(10) 0.47279(9) -0.08992(4) 0.1089(4) Uani 1 1 d . . . Br3A Br 0.02246(9) -0.26518(5) 0.10818(4) 0.0837(3) Uani 1 1 d . . . O1A O 0.5768(4) 0.0880(4) 0.07633(19) 0.0588(14) Uani 1 1 d . . . C1A C 0.4891(6) 0.0800(4) 0.0913(3) 0.0369(16) Uani 1 1 d . . . N1A N 0.4683(4) 0.0519(3) 0.1454(2) 0.0401(14) Uani 1 1 d . . . O2A O 0.5577(5) 0.0240(4) 0.2218(2) 0.0724(17) Uani 1 1 d . . . C2A C 0.5315(6) 0.0792(5) 0.1833(3) 0.0482(19) Uani 1 1 d . . . O3A O 0.4775(4) 0.5138(4) 0.0974(2) 0.0689(16) Uani 1 1 d . . . C3A C 0.4478(6) 0.4420(5) 0.1186(3) 0.0448(18) Uani 1 1 d . . . N2A N 0.3349(4) 0.4335(4) 0.1179(2) 0.0382(13) Uani 1 1 d . . . O4A O 0.3270(4) 0.4514(3) 0.20416(18) 0.0486(12) Uani 1 1 d . . . C4A C 0.2814(6) 0.4360(4) 0.1658(3) 0.0396(17) Uani 1 1 d . . . O5A O -0.0632(4) 0.1808(3) 0.1750(2) 0.0567(14) Uani 1 1 d . . . C5A C 0.0101(5) 0.2127(5) 0.1527(3) 0.0386(16) Uani 1 1 d . . . N3A N 0.0726(4) 0.1577(4) 0.1148(2) 0.0361(13) Uani 1 1 d . . . O6A O 0.0537(4) 0.2857(3) 0.04853(18) 0.0513(13) Uani 1 1 d . . . C6A C 0.1051(6) 0.2083(5) 0.0670(3) 0.0420(17) Uani 1 1 d . . . C11 C 0.2100(6) 0.1656(4) 0.0449(3) 0.0383(16) Uani 1 1 d . . . C12 C 0.2934(6) 0.1264(4) 0.0779(2) 0.0369(16) Uani 1 1 d . . . H12 H 0.2810 0.1149 0.1136 0.044 Uiso 1 1 calc R . . C13 C 0.3955(6) 0.1046(4) 0.0568(3) 0.0383(16) Uani 1 1 d . . . C14 C 0.4124(6) 0.1166(4) 0.0035(3) 0.0435(17) Uani 1 1 d . . . H14 H 0.4807 0.1026 -0.0107 0.052 Uiso 1 1 calc R . . C15 C 0.3277(7) 0.1494(5) -0.0287(3) 0.053(2) Uani 1 1 d . . . H15 H 0.3388 0.1529 -0.0647 0.064 Uiso 1 1 calc R . . C16 C 0.2282(6) 0.1767(5) -0.0089(3) 0.0467(18) Uani 1 1 d . . . H16 H 0.1727 0.2027 -0.0311 0.056 Uiso 1 1 calc R . . C11A C 0.4246(5) -0.0375(4) 0.1557(3) 0.0397(17) Uani 1 1 d . . . N12A N 0.4441(5) -0.1002(4) 0.1196(2) 0.0477(15) Uani 1 1 d . . . C13A C 0.4026(6) -0.1840(5) 0.1284(3) 0.053(2) Uani 1 1 d . . . H13A H 0.4135 -0.2308 0.1039 0.064 Uiso 1 1 calc R . . C14A C 0.3446(6) -0.2020(4) 0.1728(3) 0.0480(19) Uani 1 1 d . . . C15A C 0.3288(6) -0.1307(5) 0.2082(3) 0.0466(18) Uani 1 1 d . . . H15A H 0.2906 -0.1425 0.2390 0.056 Uiso 1 1 calc R . . N16A N 0.3666(5) -0.0457(4) 0.1995(2) 0.0461(15) Uani 1 1 d . . . C21 C 0.5598(6) 0.1805(5) 0.1745(3) 0.0433(17) Uani 1 1 d . . . C22 C 0.4904(5) 0.2618(4) 0.1512(2) 0.0378(16) Uani 1 1 d . . . H22 H 0.4256 0.2523 0.1395 0.045 Uiso 1 1 calc R . . C23 C 0.5172(5) 0.3558(5) 0.1455(3) 0.0380(16) Uani 1 1 d . . . C24 C 0.6144(6) 0.3702(6) 0.1627(3) 0.060(2) Uani 1 1 d . . . H24 H 0.6341 0.4332 0.1581 0.071 Uiso 1 1 calc R . . C25 C 0.6814(7) 0.2897(6) 0.1867(4) 0.077(3) Uani 1 1 d . . . H25 H 0.7455 0.2991 0.1994 0.093 Uiso 1 1 calc R . . C26 C 0.6546(6) 0.1970(6) 0.1919(3) 0.062(2) Uani 1 1 d . . . H26 H 0.7014 0.1435 0.2076 0.074 Uiso 1 1 calc R . . C21A C 0.2877(6) 0.4459(5) 0.0688(3) 0.0397(16) Uani 1 1 d . . . N22A N 0.1922(5) 0.4992(4) 0.0640(2) 0.0512(16) Uani 1 1 d . . . C23A C 0.1515(6) 0.5049(6) 0.0169(3) 0.063(2) Uani 1 1 d . . . H23A H 0.0828 0.5390 0.0116 0.076 Uiso 1 1 calc R . . C24A C 0.2066(8) 0.4630(6) -0.0236(3) 0.059(2) Uani 1 1 d . . . C25A C 0.3062(8) 0.4118(5) -0.0153(3) 0.068(2) Uani 1 1 d . . . H25A H 0.3451 0.3834 -0.0430 0.081 Uiso 1 1 calc R . . N26A N 0.3505(5) 0.4009(4) 0.0324(2) 0.0566(17) Uani 1 1 d . . . C31 C 0.1705(5) 0.4173(4) 0.1698(2) 0.0321(15) Uani 1 1 d . . . C32 C 0.1432(5) 0.3300(4) 0.1549(2) 0.0383(16) Uani 1 1 d . . . H32 H 0.1936 0.2856 0.1381 0.046 Uiso 1 1 calc R . . C33 C 0.0426(5) 0.3078(4) 0.1646(2) 0.0357(16) Uani 1 1 d . . . C34 C -0.0297(6) 0.3759(5) 0.1896(2) 0.0437(17) Uani 1 1 d . . . H34 H -0.0972 0.3615 0.1975 0.052 Uiso 1 1 calc R . . C35 C -0.0055(6) 0.4638(5) 0.2031(3) 0.0455(18) Uani 1 1 d . . . H35 H -0.0568 0.5094 0.2187 0.055 Uiso 1 1 calc R . . C36 C 0.0940(6) 0.4841(4) 0.1935(2) 0.0405(17) Uani 1 1 d . . . H36 H 0.1108 0.5435 0.2030 0.049 Uiso 1 1 calc R . . C31A C 0.0621(5) 0.0554(5) 0.1137(3) 0.0401(16) Uani 1 1 d . . . N32A N 0.0374(4) 0.0304(4) 0.0682(2) 0.0432(14) Uani 1 1 d . . . C33A C 0.0267(6) -0.0650(5) 0.0669(3) 0.0502(19) Uani 1 1 d . . . H33A H 0.0121 -0.0876 0.0355 0.060 Uiso 1 1 calc R . . C34A C 0.0370(5) -0.1302(5) 0.1112(3) 0.0457(18) Uani 1 1 d . . . C35A C 0.0635(6) -0.0967(5) 0.1564(3) 0.0507(19) Uani 1 1 d . . . H35A H 0.0726 -0.1407 0.1865 0.061 Uiso 1 1 calc R . . N36A N 0.0769(5) -0.0009(4) 0.1584(2) 0.0494(15) Uani 1 1 d . . . Br1B Br 0.85673(9) 1.20197(5) 0.30584(3) 0.0786(3) Uani 1 1 d . . . Br2B Br 0.62825(8) 0.47625(7) 0.58508(3) 0.0762(3) Uani 1 1 d . . . Br3B Br 0.57379(10) 1.24615(6) 0.38886(4) 0.1007(4) Uani 1 1 d . . . O1B O 1.0805(4) 0.6829(4) 0.42866(19) 0.0592(14) Uani 1 1 d . . . C1B C 1.0006(6) 0.7303(5) 0.4114(3) 0.0409(17) Uani 1 1 d . . . N1B N 0.9959(4) 0.7681(4) 0.3577(2) 0.0431(14) Uani 1 1 d . . . O2B O 1.1192(5) 0.7636(4) 0.2906(3) 0.094(2) Uani 1 1 d . . . C2B C 1.0702(6) 0.7174(5) 0.3225(3) 0.053(2) Uani 1 1 d . . . O3B O 0.9517(4) 0.3180(3) 0.39633(18) 0.0513(13) Uani 1 1 d . . . C3B C 0.9308(5) 0.3997(4) 0.3735(2) 0.0362(16) Uani 1 1 d . . . N2B N 0.8206(4) 0.4523(3) 0.37337(19) 0.0341(12) Uani 1 1 d . . . O4B O 0.8129(4) 0.4228(3) 0.28902(16) 0.0438(12) Uani 1 1 d . . . C4B C 0.7688(5) 0.4619(4) 0.3259(2) 0.0333(15) Uani 1 1 d . . . O5B O 0.4488(4) 0.8454(3) 0.32570(19) 0.0587(14) Uani 1 1 d . . . C5B C 0.5150(5) 0.7845(5) 0.3468(3) 0.0393(16) Uani 1 1 d . . . N3B N 0.5818(4) 0.8109(3) 0.38478(19) 0.0369(13) Uani 1 1 d . . . O6B O 0.5493(4) 0.6927(3) 0.45013(17) 0.0497(12) Uani 1 1 d . . . C6B C 0.6074(5) 0.7496(5) 0.4319(2) 0.0358(16) Uani 1 1 d . . . C41 C 0.7104(6) 0.7534(4) 0.4543(2) 0.0361(16) Uani 1 1 d . . . C42 C 0.7992(6) 0.7592(4) 0.4226(2) 0.0376(16) Uani 1 1 d . . . H42 H 0.7917 0.7729 0.3867 0.045 Uiso 1 1 calc R . . C43 C 0.8996(6) 0.7447(4) 0.4436(3) 0.0393(17) Uani 1 1 d . . . C44 C 0.9087(6) 0.7310(5) 0.4969(3) 0.0458(18) Uani 1 1 d . . . H44 H 0.9756 0.7210 0.5113 0.055 Uiso 1 1 calc R . . C45 C 0.8213(7) 0.7320(5) 0.5291(3) 0.057(2) Uani 1 1 d . . . H45 H 0.8283 0.7277 0.5651 0.068 Uiso 1 1 calc R . . C46 C 0.7214(6) 0.7394(5) 0.5079(3) 0.0482(19) Uani 1 1 d . . . H46 H 0.6624 0.7349 0.5297 0.058 Uiso 1 1 calc R . . C11B C 0.9599(6) 0.8724(4) 0.3453(3) 0.0458(18) Uani 1 1 d . . . N12B N 0.9702(5) 0.9293(4) 0.3825(2) 0.0549(17) Uani 1 1 d . . . C13B C 0.9370(7) 1.0274(5) 0.3700(3) 0.064(2) Uani 1 1 d . . . H13B H 0.9398 1.0715 0.3952 0.076 Uiso 1 1 calc R . . C14B C 0.8996(6) 1.0652(5) 0.3225(3) 0.055(2) Uani 1 1 d . . . C15B C 0.8978(8) 0.9986(5) 0.2862(3) 0.086(3) Uani 1 1 d . . . H15B H 0.8762 1.0225 0.2526 0.103 Uiso 1 1 calc R . . N16B N 0.9263(7) 0.9003(4) 0.2977(3) 0.086(3) Uani 1 1 d . . . C51 C 1.0807(6) 0.6071(4) 0.3265(3) 0.0406(17) Uani 1 1 d . . . C52 C 0.9974(5) 0.5579(4) 0.3448(2) 0.0351(15) Uani 1 1 d . . . H52 H 0.9326 0.5946 0.3545 0.042 Uiso 1 1 calc R . . C53 C 1.0115(5) 0.4549(4) 0.3483(2) 0.0332(15) Uani 1 1 d . . . C54 C 1.1077(6) 0.4003(5) 0.3335(2) 0.0416(17) Uani 1 1 d . . . H54 H 1.1171 0.3308 0.3360 0.050 Uiso 1 1 calc R . . C55 C 1.1899(6) 0.4492(5) 0.3147(3) 0.0493(19) Uani 1 1 d . . . H55 H 1.2544 0.4125 0.3046 0.059 Uiso 1 1 calc R . . C56 C 1.1757(6) 0.5521(5) 0.3111(3) 0.0445(17) Uani 1 1 d . . . H56 H 1.2306 0.5848 0.2982 0.053 Uiso 1 1 calc R . . C21B C 0.7711(5) 0.4578(4) 0.4239(2) 0.0329(15) Uani 1 1 d . . . N22B N 0.8310(4) 0.4852(4) 0.4585(2) 0.0412(14) Uani 1 1 d . . . C23B C 0.7872(6) 0.4889(4) 0.5066(2) 0.0394(17) Uani 1 1 d . . . H23B H 0.8251 0.5072 0.5331 0.047 Uiso 1 1 calc R . . C24B C 0.6873(6) 0.4662(5) 0.5178(2) 0.0421(17) Uani 1 1 d . . . C25B C 0.6361(6) 0.4370(5) 0.4789(3) 0.0434(17) Uani 1 1 d . . . H25B H 0.5695 0.4198 0.4862 0.052 Uiso 1 1 calc R . . N26B N 0.6764(4) 0.4315(3) 0.4302(2) 0.0372(13) Uani 1 1 d . . . C61 C 0.6606(5) 0.5244(4) 0.3226(2) 0.0331(15) Uani 1 1 d . . . C62 C 0.6381(5) 0.6180(4) 0.3420(2) 0.0342(15) Uani 1 1 d . . . H62 H 0.6884 0.6396 0.3611 0.041 Uiso 1 1 calc R . . C63 C 0.5413(5) 0.6789(4) 0.3328(2) 0.0359(16) Uani 1 1 d . . . C64 C 0.4657(5) 0.6440(5) 0.3054(3) 0.0432(17) Uani 1 1 d . . . H64 H 0.3999 0.6838 0.2996 0.052 Uiso 1 1 calc R . . C65 C 0.4881(6) 0.5502(5) 0.2867(3) 0.0474(18) Uani 1 1 d . . . H65 H 0.4371 0.5268 0.2689 0.057 Uiso 1 1 calc R . . C66 C 0.5849(6) 0.4927(5) 0.2946(2) 0.0418(17) Uani 1 1 d . . . H66 H 0.6005 0.4310 0.2808 0.050 Uiso 1 1 calc R . . C31B C 0.5849(5) 0.9151(5) 0.3856(3) 0.0425(17) Uani 1 1 d . . . N32B N 0.5580(5) 0.9517(4) 0.4314(2) 0.0513(16) Uani 1 1 d . . . C33B C 0.5592(6) 1.0496(5) 0.4322(3) 0.059(2) Uani 1 1 d . . . H33B H 0.5450 1.0793 0.4634 0.071 Uiso 1 1 calc R . . C34B C 0.5814(7) 1.1069(5) 0.3874(3) 0.059(2) Uani 1 1 d . . . C35B C 0.6073(6) 1.0609(5) 0.3431(3) 0.061(2) Uani 1 1 d . . . H35B H 0.6215 1.0995 0.3126 0.073 Uiso 1 1 calc R . . N36B N 0.6134(5) 0.9623(4) 0.3415(2) 0.0534(16) Uani 1 1 d . . . Cl1A Cl 0.7743(3) -0.1149(2) 0.17289(13) 0.1293(11) Uani 1 1 d . . . Cl2A Cl 0.8251(3) -0.2825(2) 0.25023(13) 0.1275(11) Uani 1 1 d . . . Cl3A Cl 0.6340(3) -0.2545(3) 0.19758(15) 0.1596(15) Uani 1 1 d . . . C1S C 0.7227(8) -0.1925(7) 0.2230(4) 0.095(3) Uani 1 1 d . . . H1S H 0.6875 -0.1518 0.2501 0.114 Uiso 1 1 calc R . . Cl1B Cl 0.8293(3) 0.18957(17) 0.47556(10) 0.1040(9) Uani 1 1 d . . . Cl2B Cl 0.8260(3) -0.01158(18) 0.51606(13) 0.1487(14) Uani 1 1 d . . . Cl3B Cl 0.7024(4) 0.1503(3) 0.5635(2) 0.225(3) Uani 1 1 d . . . C2S C 0.8165(7) 0.1109(6) 0.5309(3) 0.075(3) Uani 1 1 d . . . H2S H 0.8753 0.1137 0.5536 0.090 Uiso 1 1 calc R . . Cl1C Cl 0.7390(2) 0.12468(19) -0.01454(11) 0.1033(9) Uani 1 1 d . . . Cl2C Cl 0.8270(3) 0.2571(2) 0.04455(14) 0.1368(12) Uani 1 1 d . . . Cl3C Cl 0.6274(2) 0.3230(2) -0.00271(14) 0.1261(11) Uani 1 1 d . . . C3S C 0.7168(8) 0.2253(7) 0.0236(4) 0.095(3) Uani 1 1 d . . . H3S H 0.6812 0.2005 0.0554 0.114 Uiso 1 1 calc R . . Cl1D Cl 0.3390(4) 0.2042(3) 0.26468(19) 0.1141(16) Uani 0.75 1 d P A -1 Cl2D Cl 0.1726(4) 0.0927(5) 0.2702(2) 0.154(2) Uani 0.75 1 d P A -1 Cl3D Cl 0.2899(9) 0.1023(8) 0.3605(3) 0.146(4) Uani 0.75 1 d P A -1 C4S C 0.2939(19) 0.0954(17) 0.2918(5) 0.057(4) Uani 0.75 1 d P A -1 H4S H 0.3434 0.0359 0.2827 0.068 Uiso 0.75 1 calc PR A -1 Cl4D Cl 0.2565(18) 0.1802(11) 0.2498(6) 0.145(6) Uani 0.25 1 d PU B -2 Cl5D Cl 0.1900(11) 0.0235(13) 0.3078(6) 0.129(5) Uani 0.25 1 d PU B -2 Cl6D Cl 0.324(2) 0.132(2) 0.3538(11) 0.150(11) Uani 0.25 1 d PU B -2 C5S C 0.302(6) 0.092(6) 0.309(2) 0.070(13) Uani 0.25 1 d PU B -2 H5S H 0.3668 0.0470 0.2992 0.084 Uiso 0.25 1 calc PR B -2 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 Br1A 0.1105(8) 0.0496(5) 0.0779(6) -0.0018(4) -0.0032(6) -0.0358(5) Br2A 0.1499(11) 0.1328(9) 0.0573(6) 0.0109(6) -0.0427(7) -0.0625(8) Br3A 0.1200(9) 0.0404(4) 0.0959(7) -0.0053(4) -0.0270(6) -0.0228(5) O1A 0.042(3) 0.078(4) 0.058(3) -0.010(3) 0.008(3) -0.015(3) C1A 0.040(5) 0.032(3) 0.037(4) -0.004(3) 0.009(4) -0.003(3) N1A 0.045(4) 0.036(3) 0.040(3) -0.004(3) -0.003(3) -0.006(3) O2A 0.099(5) 0.055(3) 0.065(4) 0.013(3) -0.038(3) -0.018(3) C2A 0.052(5) 0.041(4) 0.050(5) -0.005(4) -0.004(4) -0.003(4) O3A 0.055(4) 0.060(3) 0.092(4) 0.025(3) -0.009(3) -0.029(3) C3A 0.042(5) 0.046(4) 0.048(5) -0.004(3) 0.007(4) -0.017(4) N2A 0.031(4) 0.045(3) 0.039(3) 0.000(3) -0.003(3) -0.007(3) O4A 0.049(3) 0.060(3) 0.045(3) -0.015(2) -0.004(2) -0.024(2) C4A 0.042(5) 0.023(3) 0.053(5) -0.002(3) -0.002(4) -0.003(3) O5A 0.045(3) 0.062(3) 0.070(4) -0.019(3) 0.020(3) -0.027(3) C5A 0.031(4) 0.044(4) 0.041(4) -0.005(3) -0.003(3) -0.007(3) N3A 0.030(3) 0.041(3) 0.039(3) -0.007(3) 0.001(3) -0.011(2) O6A 0.049(3) 0.050(3) 0.051(3) 0.002(2) -0.001(3) -0.001(2) C6A 0.049(5) 0.038(4) 0.043(4) -0.008(3) -0.012(4) -0.014(4) C11 0.044(5) 0.033(3) 0.039(4) -0.007(3) 0.004(3) -0.010(3) C12 0.050(5) 0.033(3) 0.028(4) 0.004(3) -0.001(3) -0.009(3) C13 0.042(5) 0.033(3) 0.042(4) -0.008(3) 0.003(4) -0.008(3) C14 0.047(5) 0.041(4) 0.042(4) -0.007(3) 0.006(4) -0.005(3) C15 0.073(6) 0.060(5) 0.025(4) -0.004(3) 0.005(4) -0.009(4) C16 0.047(5) 0.056(4) 0.037(4) -0.006(3) -0.005(4) -0.007(4) C11A 0.047(5) 0.026(3) 0.046(4) -0.008(3) -0.002(4) -0.004(3) N12A 0.064(4) 0.041(3) 0.037(3) -0.003(3) 0.007(3) -0.012(3) C13A 0.075(6) 0.042(4) 0.041(5) -0.006(3) -0.002(4) -0.006(4) C14A 0.063(6) 0.034(4) 0.048(5) 0.001(3) -0.009(4) -0.009(3) C15A 0.058(5) 0.040(4) 0.040(4) -0.004(3) 0.006(4) -0.006(4) N16A 0.052(4) 0.040(3) 0.046(4) -0.005(3) 0.010(3) -0.008(3) C21 0.045(5) 0.043(4) 0.043(4) -0.002(3) -0.015(4) -0.009(3) C22 0.029(4) 0.046(4) 0.041(4) -0.007(3) -0.008(3) -0.009(3) C23 0.030(4) 0.040(4) 0.045(4) -0.007(3) -0.001(3) -0.006(3) C24 0.046(5) 0.054(5) 0.084(6) -0.002(4) -0.008(5) -0.026(4) C25 0.045(6) 0.080(6) 0.109(8) 0.013(5) -0.038(5) -0.019(5) C26 0.035(5) 0.066(5) 0.084(6) 0.008(4) -0.022(4) -0.011(4) C21A 0.041(5) 0.042(4) 0.039(4) -0.001(3) -0.001(4) -0.015(3) N22A 0.044(4) 0.062(4) 0.046(4) 0.003(3) -0.008(3) -0.005(3) C23A 0.044(5) 0.091(6) 0.054(5) 0.013(5) -0.003(4) -0.021(4) C24A 0.076(7) 0.061(5) 0.045(5) 0.006(4) -0.024(5) -0.029(5) C25A 0.104(8) 0.053(5) 0.048(5) -0.011(4) 0.004(5) -0.015(5) N26A 0.067(5) 0.059(4) 0.043(4) -0.007(3) -0.001(4) -0.007(3) C31 0.032(4) 0.038(3) 0.028(3) -0.001(3) 0.000(3) -0.011(3) C32 0.037(4) 0.037(4) 0.043(4) -0.010(3) 0.003(3) -0.009(3) C33 0.036(4) 0.035(3) 0.037(4) -0.005(3) -0.005(3) -0.007(3) C34 0.038(5) 0.055(4) 0.040(4) -0.006(3) 0.003(3) -0.011(4) C35 0.048(5) 0.042(4) 0.046(4) -0.010(3) -0.003(4) -0.003(3) C36 0.044(5) 0.034(3) 0.044(4) -0.005(3) -0.005(4) -0.008(3) C31A 0.041(5) 0.040(4) 0.042(4) -0.003(3) -0.005(3) -0.012(3) N32A 0.046(4) 0.041(3) 0.046(4) -0.006(3) -0.008(3) -0.015(3) C33A 0.060(5) 0.045(4) 0.050(5) -0.006(4) -0.013(4) -0.017(4) C34A 0.040(5) 0.038(4) 0.062(5) -0.006(4) -0.012(4) -0.011(3) C35A 0.065(6) 0.039(4) 0.049(5) -0.001(3) -0.008(4) -0.011(4) N36A 0.063(5) 0.046(3) 0.042(4) -0.005(3) -0.010(3) -0.015(3) Br1B 0.1324(9) 0.0356(4) 0.0633(6) -0.0027(4) -0.0136(6) 0.0003(5) Br2B 0.0762(7) 0.1182(7) 0.0345(5) -0.0114(5) 0.0069(4) -0.0170(5) Br3B 0.1604(11) 0.0387(5) 0.1069(8) -0.0111(5) 0.0009(7) -0.0261(5) O1B 0.049(3) 0.067(3) 0.058(3) -0.011(3) -0.018(3) 0.008(3) C1B 0.046(5) 0.033(4) 0.046(4) -0.008(3) -0.015(4) -0.009(3) N1B 0.048(4) 0.031(3) 0.048(4) -0.003(3) -0.002(3) -0.003(3) O2B 0.115(6) 0.054(3) 0.109(5) 0.003(3) 0.061(4) -0.025(3) C2B 0.055(5) 0.042(4) 0.060(5) -0.002(4) 0.007(4) -0.009(4) O3B 0.054(3) 0.037(3) 0.058(3) 0.007(2) 0.000(3) -0.001(2) C3B 0.046(5) 0.034(3) 0.029(4) -0.005(3) -0.012(3) -0.003(3) N2B 0.035(3) 0.035(3) 0.030(3) -0.001(2) 0.001(3) -0.004(2) O4B 0.053(3) 0.043(3) 0.035(3) -0.016(2) 0.006(2) -0.002(2) C4B 0.042(4) 0.024(3) 0.037(4) -0.002(3) -0.003(3) -0.014(3) O5B 0.060(4) 0.041(3) 0.072(4) -0.008(2) -0.033(3) 0.010(3) C5B 0.035(4) 0.039(4) 0.042(4) -0.005(3) -0.003(3) -0.003(3) N3B 0.052(4) 0.028(3) 0.031(3) -0.005(2) -0.011(3) -0.002(2) O6B 0.049(3) 0.056(3) 0.044(3) -0.002(2) 0.002(2) -0.012(3) C6B 0.034(4) 0.040(4) 0.032(4) -0.009(3) 0.002(3) -0.001(3) C41 0.048(5) 0.032(3) 0.031(4) -0.008(3) -0.003(3) -0.010(3) C42 0.055(5) 0.028(3) 0.029(4) -0.001(3) -0.010(4) -0.006(3) C43 0.050(5) 0.029(3) 0.039(4) 0.001(3) -0.014(4) -0.007(3) C44 0.052(5) 0.050(4) 0.037(4) -0.001(3) -0.006(4) -0.015(4) C45 0.087(7) 0.057(5) 0.028(4) 0.003(3) -0.019(4) -0.017(4) C46 0.056(5) 0.047(4) 0.039(4) 0.000(3) 0.003(4) -0.004(4) C11B 0.054(5) 0.029(3) 0.054(5) -0.007(3) -0.005(4) -0.005(3) N12B 0.083(5) 0.033(3) 0.050(4) -0.004(3) -0.017(3) -0.011(3) C13B 0.103(7) 0.040(4) 0.049(5) -0.015(4) -0.006(5) -0.008(4) C14B 0.078(6) 0.035(4) 0.052(5) -0.006(4) -0.007(4) -0.006(4) C15B 0.164(10) 0.038(4) 0.054(5) 0.001(4) -0.043(6) -0.005(5) N16B 0.162(8) 0.040(4) 0.056(5) -0.008(3) -0.037(5) -0.009(4) C51 0.044(5) 0.038(4) 0.042(4) -0.006(3) -0.001(3) -0.009(3) C52 0.030(4) 0.037(3) 0.037(4) -0.007(3) -0.001(3) 0.002(3) C53 0.034(4) 0.037(3) 0.025(3) -0.004(3) -0.002(3) 0.004(3) C54 0.048(5) 0.037(4) 0.039(4) -0.007(3) -0.004(4) -0.003(3) C55 0.036(5) 0.059(5) 0.045(4) -0.004(4) 0.002(4) 0.013(4) C56 0.040(5) 0.044(4) 0.048(4) -0.002(3) 0.003(4) -0.008(3) C21B 0.037(4) 0.027(3) 0.034(4) 0.005(3) 0.001(3) -0.008(3) N22B 0.044(4) 0.042(3) 0.041(4) -0.010(3) -0.010(3) -0.012(3) C23B 0.048(5) 0.042(4) 0.029(4) -0.008(3) -0.008(3) -0.004(3) C24B 0.053(5) 0.045(4) 0.028(4) -0.001(3) -0.006(4) -0.006(4) C25B 0.042(5) 0.048(4) 0.039(4) 0.001(3) 0.007(4) -0.010(3) N26B 0.037(4) 0.038(3) 0.037(3) -0.002(2) -0.001(3) -0.009(3) C61 0.035(4) 0.037(3) 0.027(3) -0.001(3) -0.002(3) -0.006(3) C62 0.043(4) 0.032(3) 0.027(3) 0.000(3) -0.007(3) -0.005(3) C63 0.044(5) 0.037(3) 0.029(4) -0.005(3) -0.009(3) -0.009(3) C64 0.033(4) 0.047(4) 0.047(4) -0.001(3) -0.016(3) 0.001(3) C65 0.046(5) 0.053(4) 0.049(5) -0.015(4) -0.012(4) -0.014(4) C66 0.046(5) 0.044(4) 0.037(4) -0.009(3) -0.004(3) -0.009(4) C31B 0.043(5) 0.039(4) 0.045(4) 0.003(3) -0.010(4) -0.006(3) N32B 0.071(5) 0.038(3) 0.042(4) -0.005(3) -0.005(3) -0.002(3) C33B 0.089(7) 0.040(4) 0.048(5) -0.013(4) -0.012(4) -0.004(4) C34B 0.083(6) 0.032(4) 0.065(6) -0.004(4) -0.014(5) -0.018(4) C35B 0.083(7) 0.047(4) 0.051(5) 0.006(4) 0.003(4) -0.014(4) N36B 0.078(5) 0.037(3) 0.046(4) -0.005(3) -0.002(3) -0.013(3) Cl1A 0.134(3) 0.116(2) 0.127(3) 0.0193(19) 0.033(2) -0.0170(19) Cl2A 0.113(3) 0.125(2) 0.146(3) 0.026(2) -0.058(2) -0.0347(19) Cl3A 0.118(3) 0.213(4) 0.153(3) 0.047(3) -0.054(2) -0.068(3) C1S 0.119(9) 0.082(6) 0.081(7) 0.024(5) -0.005(6) -0.027(6) Cl1B 0.159(3) 0.0721(15) 0.0804(18) 0.0036(13) 0.0034(17) -0.0258(16) Cl2B 0.264(5) 0.0643(16) 0.121(3) -0.0114(16) 0.034(3) -0.044(2) Cl3B 0.224(5) 0.179(4) 0.271(6) -0.057(3) 0.180(5) -0.051(3) C2S 0.089(7) 0.066(5) 0.072(6) -0.004(5) -0.005(5) -0.023(5) Cl1C 0.089(2) 0.1070(19) 0.116(2) -0.0347(16) 0.0270(16) -0.0153(15) Cl2C 0.115(3) 0.124(2) 0.176(3) 0.002(2) -0.072(2) -0.025(2) Cl3C 0.102(2) 0.0951(18) 0.181(3) -0.0258(19) -0.060(2) 0.0042(17) C3S 0.074(7) 0.088(7) 0.129(9) -0.027(6) -0.003(6) -0.021(6) Cl1D 0.138(4) 0.078(2) 0.119(4) -0.002(2) 0.047(3) -0.013(3) Cl2D 0.092(4) 0.215(6) 0.163(5) -0.031(4) -0.015(4) -0.035(4) Cl3D 0.216(10) 0.156(6) 0.055(3) -0.004(3) 0.019(4) -0.013(5) C4S 0.067(10) 0.076(9) 0.025(7) -0.021(8) -0.009(7) 0.003(7) Cl4D 0.219(18) 0.094(9) 0.102(10) 0.008(7) 0.000(11) 0.014(11) Cl5D 0.082(9) 0.174(12) 0.140(12) -0.030(9) 0.017(8) -0.044(9) Cl6D 0.128(15) 0.18(2) 0.143(19) -0.080(15) -0.065(14) 0.023(14) C5S 0.06(2) 0.08(2) 0.06(2) -0.030(18) 0.02(2) 0.016(16) _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 Br1A C14A 1.865(6) . ? Br2A C24A 1.879(7) . ? Br3A C34A 1.888(6) . ? O1A C1A 1.193(7) . ? C1A N1A 1.435(8) . ? C1A C13 1.494(9) . ? N1A C2A 1.409(8) . ? N1A C11A 1.423(7) . ? O2A C2A 1.207(8) . ? C2A C21 1.480(9) . ? O3A C3A 1.185(7) . ? C3A N2A 1.472(8) . ? C3A C23 1.477(9) . ? N2A C4A 1.386(8) . ? N2A C21A 1.408(8) . ? O4A C4A 1.220(7) . ? C4A C31 1.485(9) . ? O5A C5A 1.204(7) . ? C5A N3A 1.424(8) . ? C5A C33 1.488(8) . ? N3A C31A 1.426(7) . ? N3A C6A 1.434(8) . ? O6A C6A 1.208(7) . ? C6A C11 1.483(9) . ? C11 C12 1.392(9) . ? C11 C16 1.394(9) . ? C12 C13 1.391(9) . ? C12 H12 0.9300 . ? C13 C14 1.378(8) . ? C14 C15 1.378(9) . ? C14 H14 0.9300 . ? C15 C16 1.358(9) . ? C15 H15 0.9300 . ? C16 H16 0.9300 . ? C11A N12A 1.309(7) . ? C11A N16A 1.332(8) . ? N12A C13A 1.336(8) . ? C13A C14A 1.363(9) . ? C13A H13A 0.9300 . ? C14A C15A 1.380(9) . ? C15A N16A 1.326(8) . ? C15A H15A 0.9300 . ? C21 C26 1.373(9) . ? C21 C22 1.396(8) . ? C22 C23 1.373(8) . ? C22 H22 0.9300 . ? C23 C24 1.390(9) . ? C24 C25 1.382(10) . ? C24 H24 0.9300 . ? C25 C26 1.358(10) . ? C25 H25 0.9300 . ? C26 H26 0.9300 . ? C21A N22A 1.313(8) . ? C21A N26A 1.333(8) . ? N22A C23A 1.331(9) . ? C23A C24A 1.352(11) . ? C23A H23A 0.9300 . ? C24A C25A 1.360(11) . ? C25A N26A 1.358(9) . ? C25A H25A 0.9300 . ? C31 C36 1.383(8) . ? C31 C32 1.386(8) . ? C32 C33 1.382(8) . ? C32 H32 0.9300 . ? C33 C34 1.379(8) . ? C34 C35 1.366(8) . ? C34 H34 0.9300 . ? C35 C36 1.358(9) . ? C35 H35 0.9300 . ? C36 H36 0.9300 . ? C31A N32A 1.318(8) . ? C31A N36A 1.320(8) . ? N32A C33A 1.332(7) . ? C33A C34A 1.371(9) . ? C33A H33A 0.9300 . ? C34A C35A 1.368(9) . ? C35A N36A 1.351(7) . ? C35A H35A 0.9300 . ? Br1B C14B 1.862(6) . ? Br2B C24B 1.869(7) . ? Br3B C34B 1.885(6) . ? O1B C1B 1.190(7) . ? C1B N1B 1.429(8) . ? C1B C43 1.502(9) . ? N1B C11B 1.424(7) . ? N1B C2B 1.424(8) . ? O2B C2B 1.208(8) . ? C2B C51 1.478(8) . ? O3B C3B 1.199(6) . ? C3B N2B 1.469(8) . ? C3B C53 1.474(9) . ? N2B C4B 1.399(7) . ? N2B C21B 1.426(7) . ? O4B C4B 1.206(7) . ? C4B C61 1.497(8) . ? O5B C5B 1.188(7) . ? C5B N3B 1.435(8) . ? C5B C63 1.495(8) . ? N3B C6B 1.421(7) . ? N3B C31B 1.429(7) . ? O6B C6B 1.214(7) . ? C6B C41 1.472(9) . ? C41 C42 1.382(9) . ? C41 C46 1.385(8) . ? C42 C43 1.392(9) . ? C42 H42 0.9300 . ? C43 C44 1.375(8) . ? C44 C45 1.365(10) . ? C44 H44 0.9300 . ? C45 C46 1.397(10) . ? C45 H45 0.9300 . ? C46 H46 0.9300 . ? C11B N12B 1.313(8) . ? C11B N16B 1.316(8) . ? N12B C13B 1.343(8) . ? C13B C14B 1.354(9) . ? C13B H13B 0.9300 . ? C14B C15B 1.367(9) . ? C15B N16B 1.332(8) . ? C15B H15B 0.9300 . ? C51 C56 1.380(9) . ? C51 C52 1.398(8) . ? C52 C53 1.377(7) . ? C52 H52 0.9300 . ? C53 C54 1.385(8) . ? C54 C55 1.387(9) . ? C54 H54 0.9300 . ? C55 C56 1.376(8) . ? C55 H55 0.9300 . ? C56 H56 0.9300 . ? C21B N22B 1.320(7) . ? C21B N26B 1.323(8) . ? N22B C23B 1.341(8) . ? C23B C24B 1.381(9) . ? C23B H23B 0.9300 . ? C24B C25B 1.346(9) . ? C25B N26B 1.340(8) . ? C25B H25B 0.9300 . ? C61 C66 1.383(8) . ? C61 C62 1.392(8) . ? C62 C63 1.383(8) . ? C62 H62 0.9300 . ? C63 C64 1.393(8) . ? C64 C65 1.388(8) . ? C64 H64 0.9300 . ? C65 C66 1.359(9) . ? C65 H65 0.9300 . ? C66 H66 0.9300 . ? C31B N36B 1.320(8) . ? C31B N32B 1.334(8) . ? N32B C33B 1.338(8) . ? C33B C34B 1.378(10) . ? C33B H33B 0.9300 . ? C34B C35B 1.356(10) . ? C35B N36B 1.335(8) . ? C35B H35B 0.9300 . ? Cl1A C1S 1.768(9) . ? Cl2A C1S 1.752(10) . ? Cl3A C1S 1.712(10) . ? C1S H1S 0.9800 . ? Cl1B C2S 1.717(8) . ? Cl2B C2S 1.730(8) . ? Cl3B C2S 1.688(9) . ? C2S H2S 0.9800 . ? Cl1C C3S 1.740(9) . ? Cl2C C3S 1.671(9) . ? Cl3C C3S 1.704(10) . ? C3S H3S 0.9800 . ? Cl1D C4S 1.75(2) . ? Cl2D C4S 1.68(2) . ? Cl3D C4S 1.778(16) . ? C4S H4S 0.9800 . ? Cl4D C5S 1.91(6) . ? Cl5D C5S 1.85(8) . ? Cl6D C5S 1.37(6) . ? C5S H5S 0.9800 . ? 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 O1A C1A N1A 120.2(6) . . ? O1A C1A C13 123.0(6) . . ? N1A C1A C13 116.7(6) . . ? C2A N1A C11A 119.1(5) . . ? C2A N1A C1A 119.0(6) . . ? C11A N1A C1A 115.1(5) . . ? O2A C2A N1A 121.4(6) . . ? O2A C2A C21 122.0(7) . . ? N1A C2A C21 116.5(6) . . ? O3A C3A N2A 119.8(6) . . ? O3A C3A C23 124.7(7) . . ? N2A C3A C23 115.5(5) . . ? C4A N2A C21A 125.8(6) . . ? C4A N2A C3A 115.7(5) . . ? C21A N2A C3A 116.9(5) . . ? O4A C4A N2A 119.5(6) . . ? O4A C4A C31 121.1(6) . . ? N2A C4A C31 119.4(6) . . ? O5A C5A N3A 120.5(6) . . ? O5A C5A C33 122.5(6) . . ? N3A C5A C33 116.9(6) . . ? C5A N3A C31A 117.1(5) . . ? C5A N3A C6A 120.3(5) . . ? C31A N3A C6A 116.9(5) . . ? O6A C6A N3A 121.4(6) . . ? O6A C6A C11 122.4(6) . . ? N3A C6A C11 115.9(6) . . ? C12 C11 C16 119.9(6) . . ? C12 C11 C6A 120.2(6) . . ? C16 C11 C6A 119.3(6) . . ? C13 C12 C11 119.2(6) . . ? C13 C12 H12 120.4 . . ? C11 C12 H12 120.4 . . ? C14 C13 C12 120.1(6) . . ? C14 C13 C1A 118.8(6) . . ? C12 C13 C1A 120.7(6) . . ? C15 C14 C13 119.7(7) . . ? C15 C14 H14 120.2 . . ? C13 C14 H14 120.2 . . ? C16 C15 C14 121.3(7) . . ? C16 C15 H15 119.3 . . ? C14 C15 H15 119.3 . . ? C15 C16 C11 119.5(7) . . ? C15 C16 H16 120.2 . . ? C11 C16 H16 120.2 . . ? N12A C11A N16A 128.1(6) . . ? N12A C11A N1A 115.2(6) . . ? N16A C11A N1A 116.6(5) . . ? C11A N12A C13A 116.0(6) . . ? N12A C13A C14A 121.0(6) . . ? N12A C13A H13A 119.5 . . ? C14A C13A H13A 119.5 . . ? C13A C14A C15A 118.2(6) . . ? C13A C14A Br1A 119.9(5) . . ? C15A C14A Br1A 121.9(6) . . ? N16A C15A C14A 121.7(7) . . ? N16A C15A H15A 119.1 . . ? C14A C15A H15A 119.1 . . ? C15A N16A C11A 114.9(5) . . ? C26 C21 C22 118.4(6) . . ? C26 C21 C2A 119.5(6) . . ? C22 C21 C2A 122.0(6) . . ? C23 C22 C21 120.6(6) . . ? C23 C22 H22 119.7 . . ? C21 C22 H22 119.7 . . ? C22 C23 C24 119.9(6) . . ? C22 C23 C3A 121.6(6) . . ? C24 C23 C3A 118.3(6) . . ? C25 C24 C23 119.0(7) . . ? C25 C24 H24 120.5 . . ? C23 C24 H24 120.5 . . ? C26 C25 C24 120.7(7) . . ? C26 C25 H25 119.7 . . ? C24 C25 H25 119.7 . . ? C25 C26 C21 121.4(7) . . ? C25 C26 H26 119.3 . . ? C21 C26 H26 119.3 . . ? N22A C21A N26A 128.9(7) . . ? N22A C21A N2A 118.5(6) . . ? N26A C21A N2A 112.6(6) . . ? C21A N22A C23A 115.0(7) . . ? N22A C23A C24A 122.2(8) . . ? N22A C23A H23A 118.9 . . ? C24A C23A H23A 118.9 . . ? C23A C24A C25A 118.4(7) . . ? C23A C24A Br2A 121.4(7) . . ? C25A C24A Br2A 120.2(7) . . ? N26A C25A C24A 121.8(7) . . ? N26A C25A H25A 119.1 . . ? C24A C25A H25A 119.1 . . ? C21A N26A C25A 113.5(7) . . ? C36 C31 C32 118.8(6) . . ? C36 C31 C4A 119.1(6) . . ? C32 C31 C4A 121.8(6) . . ? C33 C32 C31 121.3(6) . . ? C33 C32 H32 119.4 . . ? C31 C32 H32 119.4 . . ? C34 C33 C32 117.4(6) . . ? C34 C33 C5A 118.5(6) . . ? C32 C33 C5A 124.0(6) . . ? C35 C34 C33 122.2(7) . . ? C35 C34 H34 118.9 . . ? C33 C34 H34 118.9 . . ? C36 C35 C34 119.5(6) . . ? C36 C35 H35 120.2 . . ? C34 C35 H35 120.2 . . ? C35 C36 C31 120.7(6) . . ? C35 C36 H36 119.7 . . ? C31 C36 H36 119.7 . . ? N32A C31A N36A 128.9(6) . . ? N32A C31A N3A 115.2(6) . . ? N36A C31A N3A 115.9(6) . . ? C31A N32A C33A 115.6(6) . . ? N32A C33A C34A 121.1(6) . . ? N32A C33A H33A 119.4 . . ? C34A C33A H33A 119.4 . . ? C35A C34A C33A 118.5(6) . . ? C35A C34A Br3A 121.2(5) . . ? C33A C34A Br3A 120.2(5) . . ? N36A C35A C34A 121.4(6) . . ? N36A C35A H35A 119.3 . . ? C34A C35A H35A 119.3 . . ? C31A N36A C35A 114.5(6) . . ? O1B C1B N1B 120.4(7) . . ? O1B C1B C43 121.6(7) . . ? N1B C1B C43 117.7(6) . . ? C11B N1B C2B 117.7(5) . . ? C11B N1B C1B 118.2(5) . . ? C2B N1B C1B 117.2(6) . . ? O2B C2B N1B 120.8(6) . . ? O2B C2B C51 122.9(7) . . ? N1B C2B C51 116.3(6) . . ? O3B C3B N2B 119.4(6) . . ? O3B C3B C53 123.4(6) . . ? N2B C3B C53 117.0(5) . . ? C4B N2B C21B 126.2(6) . . ? C4B N2B C3B 116.2(5) . . ? C21B N2B C3B 114.3(5) . . ? O4B C4B N2B 119.8(6) . . ? O4B C4B C61 122.4(6) . . ? N2B C4B C61 117.8(5) . . ? O5B C5B N3B 121.2(6) . . ? O5B C5B C63 123.2(6) . . ? N3B C5B C63 115.4(5) . . ? C6B N3B C31B 116.5(5) . . ? C6B N3B C5B 122.1(5) . . ? C31B N3B C5B 116.5(5) . . ? O6B C6B N3B 120.5(6) . . ? O6B C6B C41 122.9(6) . . ? N3B C6B C41 116.5(6) . . ? C42 C41 C46 119.2(6) . . ? C42 C41 C6B 121.0(6) . . ? C46 C41 C6B 119.4(6) . . ? C41 C42 C43 120.9(6) . . ? C41 C42 H42 119.5 . . ? C43 C42 H42 119.5 . . ? C44 C43 C42 118.8(7) . . ? C44 C43 C1B 117.0(6) . . ? C42 C43 C1B 123.7(6) . . ? C45 C44 C43 121.1(7) . . ? C45 C44 H44 119.4 . . ? C43 C44 H44 119.4 . . ? C44 C45 C46 119.9(7) . . ? C44 C45 H45 120.1 . . ? C46 C45 H45 120.1 . . ? C41 C46 C45 119.8(7) . . ? C41 C46 H46 120.1 . . ? C45 C46 H46 120.1 . . ? N12B C11B N16B 128.1(6) . . ? N12B C11B N1B 115.2(6) . . ? N16B C11B N1B 116.7(6) . . ? C11B N12B C13B 114.3(6) . . ? N12B C13B C14B 123.0(6) . . ? N12B C13B H13B 118.5 . . ? C14B C13B H13B 118.5 . . ? C13B C14B C15B 117.0(6) . . ? C13B C14B Br1B 122.0(5) . . ? C15B C14B Br1B 120.9(6) . . ? N16B C15B C14B 121.7(7) . . ? N16B C15B H15B 119.1 . . ? C14B C15B H15B 119.1 . . ? C11B N16B C15B 115.7(6) . . ? C56 C51 C52 119.6(6) . . ? C56 C51 C2B 118.4(6) . . ? C52 C51 C2B 122.0(6) . . ? C53 C52 C51 119.8(6) . . ? C53 C52 H52 120.1 . . ? C51 C52 H52 120.1 . . ? C52 C53 C54 120.1(6) . . ? C52 C53 C3B 121.4(6) . . ? C54 C53 C3B 118.1(5) . . ? C53 C54 C55 120.1(6) . . ? C53 C54 H54 119.9 . . ? C55 C54 H54 119.9 . . ? C56 C55 C54 119.7(6) . . ? C56 C55 H55 120.1 . . ? C54 C55 H55 120.1 . . ? C55 C56 C51 120.6(6) . . ? C55 C56 H56 119.7 . . ? C51 C56 H56 119.7 . . ? N22B C21B N26B 129.4(6) . . ? N22B C21B N2B 113.2(6) . . ? N26B C21B N2B 117.3(6) . . ? C21B N22B C23B 114.4(6) . . ? N22B C23B C24B 121.6(6) . . ? N22B C23B H23B 119.2 . . ? C24B C23B H23B 119.2 . . ? C25B C24B C23B 117.6(6) . . ? C25B C24B Br2B 122.5(6) . . ? C23B C24B Br2B 119.9(5) . . ? N26B C25B C24B 123.1(7) . . ? N26B C25B H25B 118.4 . . ? C24B C25B H25B 118.4 . . ? C21B N26B C25B 113.8(6) . . ? C66 C61 C62 119.3(6) . . ? C66 C61 C4B 118.5(5) . . ? C62 C61 C4B 121.8(6) . . ? C63 C62 C61 120.3(6) . . ? C63 C62 H62 119.9 . . ? C61 C62 H62 119.9 . . ? C62 C63 C64 119.1(6) . . ? C62 C63 C5B 123.8(6) . . ? C64 C63 C5B 116.9(6) . . ? C65 C64 C63 120.4(6) . . ? C65 C64 H64 119.8 . . ? C63 C64 H64 119.8 . . ? C66 C65 C64 119.8(6) . . ? C66 C65 H65 120.1 . . ? C64 C65 H65 120.1 . . ? C65 C66 C61 121.1(6) . . ? C65 C66 H66 119.4 . . ? C61 C66 H66 119.4 . . ? N36B C31B N32B 128.7(6) . . ? N36B C31B N3B 116.5(6) . . ? N32B C31B N3B 114.9(6) . . ? C31B N32B C33B 115.2(6) . . ? N32B C33B C34B 120.6(7) . . ? N32B C33B H33B 119.7 . . ? C34B C33B H33B 119.7 . . ? C35B C34B C33B 118.5(6) . . ? C35B C34B Br3B 121.9(6) . . ? C33B C34B Br3B 119.6(6) . . ? N36B C35B C34B 122.6(7) . . ? N36B C35B H35B 118.7 . . ? C34B C35B H35B 118.7 . . ? C31B N36B C35B 114.1(6) . . ? Cl3A C1S Cl2A 107.7(5) . . ? Cl3A C1S Cl1A 109.7(5) . . ? Cl2A C1S Cl1A 110.0(6) . . ? Cl3A C1S H1S 109.8 . . ? Cl2A C1S H1S 109.8 . . ? Cl1A C1S H1S 109.8 . . ? Cl3B C2S Cl1B 110.5(5) . . ? Cl3B C2S Cl2B 111.9(5) . . ? Cl1B C2S Cl2B 111.0(5) . . ? Cl3B C2S H2S 107.7 . . ? Cl1B C2S H2S 107.7 . . ? Cl2B C2S H2S 107.7 . . ? Cl2C C3S Cl3C 114.8(5) . . ? Cl2C C3S Cl1C 114.3(6) . . ? Cl3C C3S Cl1C 112.8(6) . . ? Cl2C C3S H3S 104.5 . . ? Cl3C C3S H3S 104.5 . . ? Cl1C C3S H3S 104.5 . . ? Cl2D C4S Cl1D 110.1(10) . . ? Cl2D C4S Cl3D 110.7(14) . . ? Cl1D C4S Cl3D 105.6(10) . . ? Cl2D C4S H4S 110.1 . . ? Cl1D C4S H4S 110.1 . . ? Cl3D C4S H4S 110.1 . . ? Cl6D C5S Cl5D 121(5) . . ? Cl6D C5S Cl4D 119(5) . . ? Cl5D C5S Cl4D 93(3) . . ? Cl6D C5S H5S 107.6 . . ? Cl5D C5S H5S 107.6 . . ? Cl4D C5S H5S 107.6 . . ? 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 O1A C1A N1A C2A 30.0(8) . . . . ? C13 C1A N1A C2A -146.0(6) . . . . ? O1A C1A N1A C11A -120.8(7) . . . . ? C13 C1A N1A C11A 63.2(7) . . . . ? C11A N1A C2A O2A 7.2(10) . . . . ? C1A N1A C2A O2A -142.4(7) . . . . ? C11A N1A C2A C21 -170.1(6) . . . . ? C1A N1A C2A C21 40.2(8) . . . . ? O3A C3A N2A C4A -113.3(7) . . . . ? C23 C3A N2A C4A 68.2(7) . . . . ? O3A C3A N2A C21A 53.1(9) . . . . ? C23 C3A N2A C21A -125.4(6) . . . . ? C21A N2A C4A O4A -160.3(6) . . . . ? C3A N2A C4A O4A 4.7(8) . . . . ? C21A N2A C4A C31 21.4(8) . . . . ? C3A N2A C4A C31 -173.6(5) . . . . ? O5A C5A N3A C31A -14.9(9) . . . . ? C33 C5A N3A C31A 162.6(5) . . . . ? O5A C5A N3A C6A 137.7(7) . . . . ? C33 C5A N3A C6A -44.8(8) . . . . ? C5A N3A C6A O6A -27.1(9) . . . . ? C31A N3A C6A O6A 125.6(6) . . . . ? C5A N3A C6A C11 146.7(6) . . . . ? C31A N3A C6A C11 -60.6(7) . . . . ? O6A C6A C11 C12 136.7(6) . . . . ? N3A C6A C11 C12 -37.0(8) . . . . ? O6A C6A C11 C16 -35.0(9) . . . . ? N3A C6A C11 C16 151.2(6) . . . . ? C16 C11 C12 C13 4.0(9) . . . . ? C6A C11 C12 C13 -167.7(5) . . . . ? C11 C12 C13 C14 -3.6(9) . . . . ? C11 C12 C13 C1A 169.0(5) . . . . ? O1A C1A C13 C14 14.2(9) . . . . ? N1A C1A C13 C14 -169.9(5) . . . . ? O1A C1A C13 C12 -158.5(6) . . . . ? N1A C1A C13 C12 17.4(8) . . . . ? C12 C13 C14 C15 -0.6(9) . . . . ? C1A C13 C14 C15 -173.3(6) . . . . ? C13 C14 C15 C16 4.5(10) . . . . ? C14 C15 C16 C11 -4.1(10) . . . . ? C12 C11 C16 C15 -0.2(9) . . . . ? C6A C11 C16 C15 171.6(6) . . . . ? C2A N1A C11A N12A -127.0(7) . . . . ? C1A N1A C11A N12A 23.8(8) . . . . ? C2A N1A C11A N16A 55.1(8) . . . . ? C1A N1A C11A N16A -154.1(6) . . . . ? N16A C11A N12A C13A -1.7(11) . . . . ? N1A C11A N12A C13A -179.3(6) . . . . ? C11A N12A C13A C14A -0.6(10) . . . . ? N12A C13A C14A C15A 0.7(11) . . . . ? N12A C13A C14A Br1A -177.7(5) . . . . ? C13A C14A C15A N16A 1.3(11) . . . . ? Br1A C14A C15A N16A 179.7(5) . . . . ? C14A C15A N16A C11A -3.2(10) . . . . ? N12A C11A N16A C15A 3.5(10) . . . . ? N1A C11A N16A C15A -178.9(6) . . . . ? O2A C2A C21 C26 33.8(11) . . . . ? N1A C2A C21 C26 -148.9(7) . . . . ? O2A C2A C21 C22 -142.8(7) . . . . ? N1A C2A C21 C22 34.5(10) . . . . ? C26 C21 C22 C23 0.6(10) . . . . ? C2A C21 C22 C23 177.2(6) . . . . ? C21 C22 C23 C24 0.5(10) . . . . ? C21 C22 C23 C3A 176.7(6) . . . . ? O3A C3A C23 C22 -154.1(7) . . . . ? N2A C3A C23 C22 24.4(9) . . . . ? O3A C3A C23 C24 22.2(11) . . . . ? N2A C3A C23 C24 -159.3(6) . . . . ? C22 C23 C24 C25 -1.9(11) . . . . ? C3A C23 C24 C25 -178.3(7) . . . . ? C23 C24 C25 C26 2.3(13) . . . . ? C24 C25 C26 C21 -1.2(14) . . . . ? C22 C21 C26 C25 -0.2(12) . . . . ? C2A C21 C26 C25 -177.0(8) . . . . ? C4A N2A C21A N22A 27.1(9) . . . . ? C3A N2A C21A N22A -137.8(6) . . . . ? C4A N2A C21A N26A -153.9(6) . . . . ? C3A N2A C21A N26A 41.2(8) . . . . ? N26A C21A N22A C23A 3.2(11) . . . . ? N2A C21A N22A C23A -178.0(6) . . . . ? C21A N22A C23A C24A -3.0(11) . . . . ? N22A C23A C24A C25A 1.2(12) . . . . ? N22A C23A C24A Br2A -179.7(5) . . . . ? C23A C24A C25A N26A 0.9(12) . . . . ? Br2A C24A C25A N26A -178.3(5) . . . . ? N22A C21A N26A C25A -1.3(10) . . . . ? N2A C21A N26A C25A 179.8(6) . . . . ? C24A C25A N26A C21A -0.9(11) . . . . ? O4A C4A C31 C36 52.1(8) . . . . ? N2A C4A C31 C36 -129.6(6) . . . . ? O4A C4A C31 C32 -121.7(7) . . . . ? N2A C4A C31 C32 56.6(8) . . . . ? C36 C31 C32 C33 -1.8(9) . . . . ? C4A C31 C32 C33 172.1(6) . . . . ? C31 C32 C33 C34 0.1(9) . . . . ? C31 C32 C33 C5A -175.9(6) . . . . ? O5A C5A C33 C34 -19.8(10) . . . . ? N3A C5A C33 C34 162.7(6) . . . . ? O5A C5A C33 C32 156.2(7) . . . . ? N3A C5A C33 C32 -21.3(9) . . . . ? C32 C33 C34 C35 2.0(10) . . . . ? C5A C33 C34 C35 178.3(6) . . . . ? C33 C34 C35 C36 -2.4(10) . . . . ? C34 C35 C36 C31 0.7(10) . . . . ? C32 C31 C36 C35 1.4(9) . . . . ? C4A C31 C36 C35 -172.7(6) . . . . ? C5A N3A C31A N32A 125.0(6) . . . . ? C6A N3A C31A N32A -28.6(8) . . . . ? C5A N3A C31A N36A -54.0(8) . . . . ? C6A N3A C31A N36A 152.4(6) . . . . ? N36A C31A N32A C33A -0.7(11) . . . . ? N3A C31A N32A C33A -179.6(6) . . . . ? C31A N32A C33A C34A 2.6(10) . . . . ? N32A C33A C34A C35A -3.1(11) . . . . ? N32A C33A C34A Br3A -179.6(5) . . . . ? C33A C34A C35A N36A 1.7(11) . . . . ? Br3A C34A C35A N36A 178.2(5) . . . . ? N32A C31A N36A C35A -0.6(11) . . . . ? N3A C31A N36A C35A 178.3(6) . . . . ? C34A C35A N36A C31A 0.1(10) . . . . ? O1B C1B N1B C11B -126.3(7) . . . . ? C43 C1B N1B C11B 59.0(8) . . . . ? O1B C1B N1B C2B 24.0(9) . . . . ? C43 C1B N1B C2B -150.7(6) . . . . ? C11B N1B C2B O2B 16.9(11) . . . . ? C1B N1B C2B O2B -133.5(8) . . . . ? C11B N1B C2B C51 -161.5(6) . . . . ? C1B N1B C2B C51 48.0(9) . . . . ? O3B C3B N2B C4B -109.3(6) . . . . ? C53 C3B N2B C4B 75.1(6) . . . . ? O3B C3B N2B C21B 51.5(7) . . . . ? C53 C3B N2B C21B -124.1(6) . . . . ? C21B N2B C4B O4B -153.9(5) . . . . ? C3B N2B C4B O4B 4.2(8) . . . . ? C21B N2B C4B C61 28.2(8) . . . . ? C3B N2B C4B C61 -173.6(5) . . . . ? O5B C5B N3B C6B 137.7(7) . . . . ? C63 C5B N3B C6B -47.5(8) . . . . ? O5B C5B N3B C31B -16.4(10) . . . . ? C63 C5B N3B C31B 158.5(6) . . . . ? C31B N3B C6B O6B 129.5(6) . . . . ? C5B N3B C6B O6B -24.5(9) . . . . ? C31B N3B C6B C41 -55.2(7) . . . . ? C5B N3B C6B C41 150.7(6) . . . . ? O6B C6B C41 C42 136.2(6) . . . . ? N3B C6B C41 C42 -38.9(8) . . . . ? O6B C6B C41 C46 -36.2(9) . . . . ? N3B C6B C41 C46 148.7(5) . . . . ? C46 C41 C42 C43 4.2(9) . . . . ? C6B C41 C42 C43 -168.3(5) . . . . ? C41 C42 C43 C44 -4.3(8) . . . . ? C41 C42 C43 C1B 167.9(5) . . . . ? O1B C1B C43 C44 20.9(9) . . . . ? N1B C1B C43 C44 -164.4(5) . . . . ? O1B C1B C43 C42 -151.3(6) . . . . ? N1B C1B C43 C42 23.3(8) . . . . ? C42 C43 C44 C45 -0.3(9) . . . . ? C1B C43 C44 C45 -173.0(6) . . . . ? C43 C44 C45 C46 4.9(10) . . . . ? C42 C41 C46 C45 0.4(9) . . . . ? C6B C41 C46 C45 173.0(6) . . . . ? C44 C45 C46 C41 -4.9(10) . . . . ? C2B N1B C11B N12B -126.8(7) . . . . ? C1B N1B C11B N12B 23.3(9) . . . . ? C2B N1B C11B N16B 49.6(9) . . . . ? C1B N1B C11B N16B -160.3(7) . . . . ? N16B C11B N12B C13B 3.4(12) . . . . ? N1B C11B N12B C13B 179.3(6) . . . . ? C11B N12B C13B C14B -2.3(12) . . . . ? N12B C13B C14B C15B -0.9(13) . . . . ? N12B C13B C14B Br1B -178.7(6) . . . . ? C13B C14B C15B N16B 3.4(14) . . . . ? Br1B C14B C15B N16B -178.8(7) . . . . ? N12B C11B N16B C15B -1.1(14) . . . . ? N1B C11B N16B C15B -176.9(7) . . . . ? C14B C15B N16B C11B -2.5(14) . . . . ? O2B C2B C51 C56 28.2(11) . . . . ? N1B C2B C51 C56 -153.4(6) . . . . ? O2B C2B C51 C52 -150.9(8) . . . . ? N1B C2B C51 C52 27.5(10) . . . . ? C56 C51 C52 C53 1.5(9) . . . . ? C2B C51 C52 C53 -179.4(6) . . . . ? C51 C52 C53 C54 -0.6(9) . . . . ? C51 C52 C53 C3B 172.1(6) . . . . ? O3B C3B C53 C52 -148.7(6) . . . . ? N2B C3B C53 C52 26.8(8) . . . . ? O3B C3B C53 C54 24.1(9) . . . . ? N2B C3B C53 C54 -160.5(5) . . . . ? C52 C53 C54 C55 -0.3(9) . . . . ? C3B C53 C54 C55 -173.2(6) . . . . ? C53 C54 C55 C56 0.2(10) . . . . ? C54 C55 C56 C51 0.7(10) . . . . ? C52 C51 C56 C55 -1.6(10) . . . . ? C2B C51 C56 C55 179.3(6) . . . . ? C4B N2B C21B N22B -155.1(5) . . . . ? C3B N2B C21B N22B 46.4(7) . . . . ? C4B N2B C21B N26B 27.7(8) . . . . ? C3B N2B C21B N26B -130.8(6) . . . . ? N26B C21B N22B C23B -1.9(9) . . . . ? N2B C21B N22B C23B -178.7(5) . . . . ? C21B N22B C23B C24B -0.4(8) . . . . ? N22B C23B C24B C25B 2.0(9) . . . . ? N22B C23B C24B Br2B -178.2(4) . . . . ? C23B C24B C25B N26B -1.7(10) . . . . ? Br2B C24B C25B N26B 178.5(4) . . . . ? N22B C21B N26B C25B 2.2(9) . . . . ? N2B C21B N26B C25B 178.9(5) . . . . ? C24B C25B N26B C21B -0.3(9) . . . . ? O4B C4B C61 C66 40.7(9) . . . . ? N2B C4B C61 C66 -141.6(6) . . . . ? O4B C4B C61 C62 -132.2(6) . . . . ? N2B C4B C61 C62 45.6(8) . . . . ? C66 C61 C62 C63 -0.5(9) . . . . ? C4B C61 C62 C63 172.3(6) . . . . ? C61 C62 C63 C64 1.9(9) . . . . ? C61 C62 C63 C5B -172.8(6) . . . . ? O5B C5B C63 C62 155.8(7) . . . . ? N3B C5B C63 C62 -18.9(9) . . . . ? O5B C5B C63 C64 -19.0(10) . . . . ? N3B C5B C63 C64 166.2(6) . . . . ? C62 C63 C64 C65 -1.2(10) . . . . ? C5B C63 C64 C65 173.9(6) . . . . ? C63 C64 C65 C66 -1.0(10) . . . . ? C64 C65 C66 C61 2.4(10) . . . . ? C62 C61 C66 C65 -1.7(10) . . . . ? C4B C61 C66 C65 -174.7(6) . . . . ? C6B N3B C31B N36B 147.6(6) . . . . ? C5B N3B C31B N36B -56.9(8) . . . . ? C6B N3B C31B N32B -32.6(8) . . . . ? C5B N3B C31B N32B 122.9(6) . . . . ? N36B C31B N32B C33B 0.7(11) . . . . ? N3B C31B N32B C33B -179.1(6) . . . . ? C31B N32B C33B C34B 3.4(11) . . . . ? N32B C33B C34B C35B -3.4(12) . . . . ? N32B C33B C34B Br3B 176.0(6) . . . . ? C33B C34B C35B N36B -0.8(13) . . . . ? Br3B C34B C35B N36B 179.7(6) . . . . ? N32B C31B N36B C35B -4.6(11) . . . . ? N3B C31B N36B C35B 175.2(6) . . . . ? C34B C35B N36B C31B 4.5(11) . . . . ? _iucr_refine_instructions_details ; TITL 11-124 is 2,6_BrIO3:2CHCl3 in P-1 at 40kV30mA to 0.80\%A CELL 0.71073 12.8150 13.6159 25.7452 84.442 87.666 80.070 ZERR 4 0.0006 0.0005 0.0011 0.003 0.004 0.004 LATT 1 SFAC C H N O CL BR UNIT 152 80 36 24 24 12 MERG 3 FMAP 2 L.S. 10 3 LIST 4 ACTA 54 CONF DELU 0.03 CL4D CL5D CL6D C5S ISOR 0.03 CL4D CL5D CL6D C5S BOND $H HTAB EQIV $1 X,Y-1,Z EQIV $2 X,1+Y,Z EQIV $3 2-X,1-Y,1-Z HTAB C3S O1A HTAB C4S N16A HTAB C12 N1A HTAB C22 N2A HTAB C52 N2B HTAB C62 N3B HTAB C44 O3B_$3 HTAB C2S N12B_$3 RTAB XO BR1A O4A_$1 RTAB XO BR1B O4B_$2 RTAB XOC BR1A O4A_$1 C4A_$1 RTAB XOC BR1B O4B_$2 C4B_$2 RTAB CXO C14A BR1A O4A_$1 RTAB CXO C14B BR1B O4B_$2 RTAB XX BR1A BR2A RTAB XX BR1A BR3A RTAB XX BR2A BR3A RTAB XX BR1B BR2B RTAB XX BR1B BR3B RTAB XX BR2B BR3B RTAB OO O2A O5A RTAB OO O1A O2A RTAB OO O3A O4A RTAB OO O5A O6A RTAB OO O1A O3A RTAB OO O2A O4A RTAB OO O1A O5A RTAB NN N1A N2A RTAB NN N1A N3A RTAB NN N2A N3A RTAB NN N12A N22A RTAB NN N12A N32A RTAB NN N22A N32A RTAB OCCO O1A C1A C6A O6A RTAB OCCO O2A C2A C3A O3A RTAB OCCO O4A C4A C5A O5A RTAB OCCO O1A C1A C2A O2A RTAB OCCO O3A C3A C4A O4A RTAB OCCO O5A C5A C6A O6A RTAB CCNC C13A C1A N1A C2A RTAB CCNC C23A C3A N2A C4A RTAB CCNC C33A C5A N3A C6A RTAB CNCC C1A N1A C2A C21 RTAB CNCC C3A N2A C4A C31 RTAB CNCC C5A N3A C6A C11 RTAB OCNC O1A C1A N1A C2A RTAB OCNC O3A C3A N2A C4A RTAB OCNC O5A C5A N3A C6A RTAB CNCO C1A N1A C2A O2A RTAB CNCO C3A N2A C4A O4A RTAB CNCO C5A N3A C6A O6A RTAB CNCN C1A N1A C11A N12A RTAB CNCN C3A N2A C21A N22A RTAB CNCN C5A N3A C31A N32A RTAB OO O2B O5B RTAB OO O1B O2B RTAB OO O3B O4B RTAB OO O5B O6B RTAB OO O1B O3B RTAB OO O2B O4B RTAB OO O1B O5B RTAB NN N1B N2B RTAB NN N1B N3B RTAB NN N2B N3B RTAB NN N12B N22B RTAB NN N12B N32B RTAB NN N22B N32B RTAB OCCO O1B C1B C6B O6B RTAB OCCO O2B C2B C3B O3B RTAB OCCO O4B C4B C5B O5B RTAB OCCO O1B C1B C2B O2B RTAB OCCO O3B C3B C4B O4B RTAB OCCO O5B C5B C6B O6B RTAB CCNC C13B C1B N1B C2B RTAB CCNC C23B C3B N2B C4B RTAB CCNC C33B C5B N3B C6B RTAB CNCC C1B N1B C2B C21 RTAB CNCC C3B N2B C4B C31 RTAB CNCC C5B N3B C6B C11 RTAB OCNC O1B C1B N1B C2B RTAB OCNC O3B C3B N2B C4B RTAB OCNC O5B C5B N3B C6B RTAB CNCO C1B N1B C2B O2B RTAB CNCO C3B N2B C4B O4B RTAB CNCO C5B N3B C6B O6B RTAB CNCN C1B N1B C11B N12B RTAB CNCN C3B N2B C21B N22B RTAB CNCN C5B N3B C31B N32B SIZE 0.04 0.17 0.34 TEMP 21 PLAN 10 MPLA 3 C1A C2A C11A N1A N2A N3A MPLA 3 C3A C4A C21A N2A N1A N3A MPLA 3 C5A C6A C31A N3A N1A N2A MPLA 6 C11 C12 C13 C14 C15 C16 C1A O1A C6A O6A MPLA 6 C21 C22 C23 C24 C25 C26 C2A O2A C3A O3A MPLA 6 C31 C32 C33 C34 C35 C36 C4A O4A C5A O5A MPLA 6 C11 C12 C13 C14 C15 C16 MPLA 6 C31 C32 C33 C34 C35 C36 MPLA 3 C1A C2A N1A O1A O2A C11 C11A C21 MPLA 6 C11A N12A C13A C14A C15A N16A MPLA 6 C11 C12 C13 C14 C15 C16 MPLA 6 C21 C22 C23 C24 C25 C26 MPLA 3 C3A C4A N2A O3A O4A C21 C21A C31 MPLA 6 C21A N22A C23A C24A C25A N26A MPLA 6 C21 C22 C23 C24 C25 C26 MPLA 6 C31 C32 C33 C34 C35 C36 MPLA 3 C5A C6A N3A O5A O6A C31 C31A MPLA 6 C31A N32A C33A C34A C35A N36A MPLA 6 C31 C32 C33 C34 C35 C36 MPLA 3 C1B C2B C11B N1B N2B N3B MPLA 3 C3B C4B C21B N2B N1B N3B MPLA 3 C5B C6B C31B N3B N1B N2B MPLA 6 C11 C12 C13 C14 C15 C16 C1B O1B C6B O6B MPLA 6 C21 C22 C23 C24 C25 C26 C2B O2B C3B O3B MPLA 6 C31 C32 C33 C34 C35 C36 C4B O4B C5B O5B MPLA 6 C11 C12 C13 C14 C15 C16 MPLA 6 C31 C32 C33 C34 C35 C36 MPLA 3 C1B C2B N1B O1B O2B C11 C11B C21 MPLA 6 C11B N12B C13B C14B C15B N16B MPLA 6 C11 C12 C13 C14 C15 C16 MPLA 6 C21 C22 C23 C24 C25 C26 MPLA 3 C3B C4B N2B O3B O4B C21 C21B C31 MPLA 6 C21B N22B C23B C24B C25B N26B MPLA 6 C21 C22 C23 C24 C25 C26 MPLA 6 C31 C32 C33 C34 C35 C36 MPLA 3 C5B C6B N3B O5B O6B C31 C31B MPLA 6 C31B N32B C33B C34B C35B N36B MPLA 6 C31 C32 C33 C34 C35 C36 WGHT 0.060100 2.478800 FVAR 1.71853 MOLE 1 BR1A 6 0.292212 -0.321916 0.185030 11.00000 0.11047 0.04961 = 0.07790 -0.00181 -0.00316 -0.03584 BR2A 6 0.147534 0.472786 -0.089921 11.00000 0.14989 0.13283 = 0.05733 0.01085 -0.04271 -0.06255 BR3A 6 0.022461 -0.265176 0.108182 11.00000 0.12004 0.04041 = 0.09589 -0.00532 -0.02700 -0.02281 O1A 4 0.576816 0.088031 0.076330 11.00000 0.04203 0.07824 = 0.05807 -0.01045 0.00800 -0.01510 C1A 1 0.489063 0.079956 0.091295 11.00000 0.04020 0.03185 = 0.03700 -0.00435 0.00856 -0.00303 N1A 3 0.468278 0.051856 0.145404 11.00000 0.04505 0.03577 = 0.03978 -0.00421 -0.00287 -0.00647 O2A 4 0.557685 0.024047 0.221827 11.00000 0.09873 0.05471 = 0.06493 0.01284 -0.03815 -0.01777 C2A 1 0.531520 0.079231 0.183295 11.00000 0.05178 0.04117 = 0.05030 -0.00531 -0.00374 -0.00298 O3A 4 0.477461 0.513783 0.097441 11.00000 0.05539 0.06037 = 0.09212 0.02508 -0.00927 -0.02927 C3A 1 0.447843 0.441966 0.118606 11.00000 0.04250 0.04634 = 0.04836 -0.00425 0.00692 -0.01750 N2A 3 0.334909 0.433488 0.117942 11.00000 0.03072 0.04480 = 0.03864 0.00046 -0.00316 -0.00726 O4A 4 0.327008 0.451380 0.204165 11.00000 0.04868 0.05990 = 0.04461 -0.01515 -0.00361 -0.02389 C4A 1 0.281420 0.436031 0.165806 11.00000 0.04152 0.02323 = 0.05293 -0.00172 -0.00214 -0.00350 O5A 4 -0.063203 0.180809 0.175032 11.00000 0.04522 0.06226 = 0.06975 -0.01898 0.02026 -0.02726 C5A 1 0.010073 0.212750 0.152744 11.00000 0.03082 0.04432 = 0.04139 -0.00482 -0.00293 -0.00728 N3A 3 0.072645 0.157729 0.114814 11.00000 0.03012 0.04136 = 0.03884 -0.00700 0.00085 -0.01055 O6A 4 0.053662 0.285692 0.048528 11.00000 0.04901 0.04959 = 0.05131 0.00212 -0.00051 -0.00066 C6A 1 0.105052 0.208281 0.066956 11.00000 0.04884 0.03788 = 0.04343 -0.00835 -0.01227 -0.01407 C11 1 0.209983 0.165600 0.044934 11.00000 0.04413 0.03302 = 0.03927 -0.00669 0.00403 -0.00969 C12 1 0.293408 0.126388 0.077887 11.00000 0.04999 0.03273 = 0.02752 0.00449 -0.00103 -0.00933 AFIX 43 H12 2 0.281048 0.114901 0.113625 11.00000 -1.20000 AFIX 0 C13 1 0.395456 0.104586 0.056758 11.00000 0.04166 0.03285 = 0.04176 -0.00797 0.00316 -0.00827 C14 1 0.412425 0.116582 0.003478 11.00000 0.04669 0.04107 = 0.04179 -0.00673 0.00613 -0.00459 AFIX 43 H14 2 0.480708 0.102606 -0.010685 11.00000 -1.20000 AFIX 0 C15 1 0.327671 0.149397 -0.028699 11.00000 0.07324 0.05992 = 0.02469 -0.00387 0.00516 -0.00896 AFIX 43 H15 2 0.338830 0.152891 -0.064703 11.00000 -1.20000 AFIX 0 C16 1 0.228221 0.176721 -0.008881 11.00000 0.04750 0.05561 = 0.03706 -0.00565 -0.00536 -0.00702 AFIX 43 H16 2 0.172668 0.202673 -0.031056 11.00000 -1.20000 AFIX 0 C11A 1 0.424583 -0.037487 0.155689 11.00000 0.04660 0.02646 = 0.04628 -0.00824 -0.00175 -0.00430 N12A 3 0.444057 -0.100182 0.119637 11.00000 0.06446 0.04128 = 0.03743 -0.00282 0.00737 -0.01176 C13A 1 0.402618 -0.183991 0.128407 11.00000 0.07488 0.04210 = 0.04131 -0.00616 -0.00247 -0.00558 AFIX 43 H13A 2 0.413503 -0.230770 0.103854 11.00000 -1.20000 AFIX 0 C14A 1 0.344618 -0.201981 0.172804 11.00000 0.06254 0.03367 = 0.04792 0.00051 -0.00866 -0.00941 C15A 1 0.328771 -0.130658 0.208239 11.00000 0.05807 0.03985 = 0.04046 -0.00363 0.00558 -0.00622 AFIX 43 H15A 2 0.290579 -0.142517 0.239031 11.00000 -1.20000 AFIX 0 N16A 3 0.366568 -0.045698 0.199529 11.00000 0.05181 0.03963 = 0.04645 -0.00488 0.00952 -0.00830 C21 1 0.559794 0.180495 0.174465 11.00000 0.04538 0.04292 = 0.04326 -0.00233 -0.01547 -0.00949 C22 1 0.490438 0.261827 0.151217 11.00000 0.02928 0.04571 = 0.04064 -0.00704 -0.00839 -0.00918 AFIX 43 H22 2 0.425556 0.252293 0.139474 11.00000 -1.20000 AFIX 0 C23 1 0.517199 0.355773 0.145544 11.00000 0.02961 0.04031 = 0.04459 -0.00693 -0.00058 -0.00562 C24 1 0.614403 0.370248 0.162701 11.00000 0.04588 0.05422 = 0.08421 -0.00161 -0.00841 -0.02575 AFIX 43 H24 2 0.634061 0.433213 0.158092 11.00000 -1.20000 AFIX 0 C25 1 0.681378 0.289698 0.186703 11.00000 0.04500 0.08013 = 0.10897 0.01318 -0.03789 -0.01948 AFIX 43 H25 2 0.745477 0.299092 0.199439 11.00000 -1.20000 AFIX 0 C26 1 0.654570 0.196964 0.191886 11.00000 0.03475 0.06598 = 0.08368 0.00766 -0.02155 -0.01088 AFIX 43 H26 2 0.701382 0.143498 0.207563 11.00000 -1.20000 AFIX 0 C21A 1 0.287657 0.445925 0.068769 11.00000 0.04082 0.04213 = 0.03851 -0.00064 -0.00105 -0.01532 N22A 3 0.192243 0.499155 0.064020 11.00000 0.04374 0.06183 = 0.04557 0.00347 -0.00839 -0.00514 C23A 1 0.151505 0.504925 0.016860 11.00000 0.04409 0.09123 = 0.05429 0.01282 -0.00257 -0.02069 AFIX 43 H23A 2 0.082819 0.538967 0.011583 11.00000 -1.20000 AFIX 0 C24A 1 0.206604 0.462974 -0.023621 11.00000 0.07588 0.06089 = 0.04496 0.00633 -0.02403 -0.02875 C25A 1 0.306224 0.411761 -0.015263 11.00000 0.10355 0.05326 = 0.04818 -0.01104 0.00424 -0.01499 AFIX 43 H25A 2 0.345139 0.383399 -0.042978 11.00000 -1.20000 AFIX 0 N26A 3 0.350462 0.400886 0.032440 11.00000 0.06690 0.05916 = 0.04305 -0.00709 -0.00083 -0.00727 C31 1 0.170453 0.417262 0.169820 11.00000 0.03207 0.03759 = 0.02784 -0.00083 0.00010 -0.01092 C32 1 0.143206 0.330023 0.154917 11.00000 0.03720 0.03677 = 0.04263 -0.00970 0.00267 -0.00867 AFIX 43 H32 2 0.193621 0.285581 0.138069 11.00000 -1.20000 AFIX 0 C33 1 0.042574 0.307822 0.164612 11.00000 0.03592 0.03471 = 0.03744 -0.00494 -0.00546 -0.00693 C34 1 -0.029706 0.375899 0.189582 11.00000 0.03786 0.05459 = 0.03987 -0.00643 0.00291 -0.01102 AFIX 43 H34 2 -0.097222 0.361505 0.197493 11.00000 -1.20000 AFIX 0 C35 1 -0.005506 0.463772 0.203095 11.00000 0.04811 0.04170 = 0.04640 -0.00976 -0.00284 -0.00339 AFIX 43 H35 2 -0.056767 0.509355 0.218725 11.00000 -1.20000 AFIX 0 C36 1 0.093954 0.484083 0.193539 11.00000 0.04431 0.03374 = 0.04440 -0.00526 -0.00533 -0.00773 AFIX 43 H36 2 0.110801 0.543544 0.203043 11.00000 -1.20000 AFIX 0 C31A 1 0.062137 0.055411 0.113738 11.00000 0.04113 0.03973 = 0.04165 -0.00311 -0.00526 -0.01214 N32A 3 0.037376 0.030391 0.068197 11.00000 0.04616 0.04082 = 0.04633 -0.00613 -0.00751 -0.01519 C33A 1 0.026741 -0.064967 0.066948 11.00000 0.06020 0.04484 = 0.04996 -0.00647 -0.01265 -0.01717 AFIX 43 H33A 2 0.012108 -0.087646 0.035543 11.00000 -1.20000 AFIX 0 C34A 1 0.037011 -0.130243 0.111196 11.00000 0.04046 0.03765 = 0.06181 -0.00611 -0.01211 -0.01127 C35A 1 0.063545 -0.096675 0.156444 11.00000 0.06538 0.03917 = 0.04854 -0.00093 -0.00830 -0.01145 AFIX 43 H35A 2 0.072591 -0.140746 0.186480 11.00000 -1.20000 AFIX 0 N36A 3 0.076888 -0.000860 0.158422 11.00000 0.06314 0.04645 = 0.04159 -0.00506 -0.01035 -0.01475 MOLE 2 BR1B 6 0.856728 1.201972 0.305842 11.00000 0.13244 0.03555 = 0.06326 -0.00272 -0.01363 0.00029 BR2B 6 0.628254 0.476248 0.585076 11.00000 0.07617 0.11824 = 0.03452 -0.01138 0.00689 -0.01701 BR3B 6 0.573786 1.246150 0.388858 11.00000 0.16042 0.03870 = 0.10695 -0.01112 0.00092 -0.02610 O1B 4 1.080519 0.682939 0.428660 11.00000 0.04894 0.06659 = 0.05795 -0.01068 -0.01788 0.00847 C1B 1 1.000587 0.730329 0.411402 11.00000 0.04578 0.03343 = 0.04646 -0.00814 -0.01534 -0.00887 N1B 3 0.995892 0.768102 0.357661 11.00000 0.04826 0.03147 = 0.04811 -0.00293 -0.00158 -0.00293 O2B 4 1.119243 0.763587 0.290581 11.00000 0.11522 0.05410 = 0.10909 0.00321 0.06116 -0.02504 C2B 1 1.070164 0.717360 0.322467 11.00000 0.05501 0.04153 = 0.06043 -0.00207 0.00726 -0.00892 O3B 4 0.951685 0.318022 0.396327 11.00000 0.05413 0.03732 = 0.05777 0.00740 -0.00044 -0.00106 C3B 1 0.930820 0.399728 0.373527 11.00000 0.04611 0.03355 = 0.02905 -0.00528 -0.01239 -0.00311 N2B 3 0.820598 0.452345 0.373373 11.00000 0.03529 0.03543 = 0.03029 -0.00129 0.00117 -0.00388 O4B 4 0.812912 0.422805 0.289020 11.00000 0.05331 0.04300 = 0.03460 -0.01569 0.00622 -0.00200 C4B 1 0.768785 0.461911 0.325907 11.00000 0.04179 0.02441 = 0.03663 -0.00196 -0.00334 -0.01383 O5B 4 0.448773 0.845405 0.325697 11.00000 0.06033 0.04077 = 0.07157 -0.00804 -0.03330 0.00992 C5B 1 0.515016 0.784495 0.346813 11.00000 0.03530 0.03939 = 0.04231 -0.00540 -0.00251 -0.00275 N3B 3 0.581834 0.810899 0.384784 11.00000 0.05197 0.02761 = 0.03050 -0.00502 -0.01072 -0.00152 O6B 4 0.549307 0.692704 0.450127 11.00000 0.04886 0.05618 = 0.04441 -0.00226 0.00175 -0.01214 C6B 1 0.607434 0.749577 0.431932 11.00000 0.03447 0.03951 = 0.03224 -0.00885 0.00193 -0.00055 C41 1 0.710419 0.753415 0.454260 11.00000 0.04769 0.03217 = 0.03063 -0.00849 -0.00306 -0.00958 C42 1 0.799186 0.759188 0.422564 11.00000 0.05532 0.02780 = 0.02938 -0.00062 -0.00956 -0.00570 AFIX 43 H42 2 0.791713 0.772942 0.386687 11.00000 -1.20000 AFIX 0 C43 1 0.899641 0.744705 0.443580 11.00000 0.05032 0.02899 = 0.03879 0.00098 -0.01412 -0.00681 C44 1 0.908733 0.731032 0.496930 11.00000 0.05247 0.04982 = 0.03700 -0.00050 -0.00596 -0.01465 AFIX 43 H44 2 0.975555 0.720969 0.511322 11.00000 -1.20000 AFIX 0 C45 1 0.821334 0.731980 0.529115 11.00000 0.08658 0.05732 = 0.02796 0.00345 -0.01935 -0.01734 AFIX 43 H45 2 0.828305 0.727706 0.565116 11.00000 -1.20000 AFIX 0 C46 1 0.721374 0.739383 0.507876 11.00000 0.05605 0.04698 = 0.03855 0.00037 0.00282 -0.00373 AFIX 43 H46 2 0.662389 0.734901 0.529678 11.00000 -1.20000 AFIX 0 C11B 1 0.959938 0.872351 0.345345 11.00000 0.05401 0.02912 = 0.05439 -0.00740 -0.00456 -0.00468 N12B 3 0.970190 0.929258 0.382536 11.00000 0.08305 0.03290 = 0.05047 -0.00360 -0.01709 -0.01142 C13B 1 0.936956 1.027423 0.370032 11.00000 0.10252 0.04043 = 0.04939 -0.01452 -0.00572 -0.00850 AFIX 43 H13B 2 0.939759 1.071484 0.395178 11.00000 -1.20000 AFIX 0 C14B 1 0.899561 1.065189 0.322502 11.00000 0.07848 0.03523 = 0.05185 -0.00602 -0.00664 -0.00647 C15B 1 0.897835 0.998587 0.286202 11.00000 0.16357 0.03823 = 0.05382 0.00075 -0.04328 -0.00548 AFIX 43 H15B 2 0.876189 1.022504 0.252607 11.00000 -1.20000 AFIX 0 N16B 3 0.926343 0.900347 0.297691 11.00000 0.16159 0.03959 = 0.05624 -0.00763 -0.03719 -0.00920 C51 1 1.080696 0.607120 0.326546 11.00000 0.04379 0.03767 = 0.04156 -0.00623 -0.00072 -0.00890 C52 1 0.997371 0.557884 0.344771 11.00000 0.03003 0.03651 = 0.03680 -0.00733 -0.00066 0.00193 AFIX 43 H52 2 0.932607 0.594575 0.354461 11.00000 -1.20000 AFIX 0 C53 1 1.011490 0.454898 0.348330 11.00000 0.03424 0.03692 = 0.02493 -0.00391 -0.00155 0.00426 C54 1 1.107655 0.400315 0.333456 11.00000 0.04775 0.03741 = 0.03925 -0.00683 -0.00424 -0.00347 AFIX 43 H54 2 1.117117 0.330759 0.336047 11.00000 -1.20000 AFIX 0 C55 1 1.189880 0.449178 0.314702 11.00000 0.03614 0.05903 = 0.04495 -0.00412 0.00230 0.01275 AFIX 43 H55 2 1.254354 0.412528 0.304591 11.00000 -1.20000 AFIX 0 C56 1 1.175678 0.552061 0.311118 11.00000 0.04017 0.04441 = 0.04831 -0.00209 0.00312 -0.00776 AFIX 43 H56 2 1.230572 0.584809 0.298184 11.00000 -1.20000 AFIX 0 C21B 1 0.771148 0.457848 0.423861 11.00000 0.03724 0.02680 = 0.03390 0.00509 0.00054 -0.00796 N22B 3 0.831012 0.485218 0.458503 11.00000 0.04352 0.04237 = 0.04128 -0.00965 -0.00969 -0.01198 C23B 1 0.787234 0.488925 0.506632 11.00000 0.04824 0.04152 = 0.02855 -0.00797 -0.00788 -0.00386 AFIX 43 H23B 2 0.825089 0.507229 0.533142 11.00000 -1.20000 AFIX 0 C24B 1 0.687274 0.466217 0.517793 11.00000 0.05265 0.04487 = 0.02792 -0.00097 -0.00629 -0.00607 C25B 1 0.636055 0.437001 0.478900 11.00000 0.04224 0.04849 = 0.03866 0.00130 0.00670 -0.00973 AFIX 43 H25B 2 0.569482 0.419815 0.486157 11.00000 -1.20000 AFIX 0 N26B 3 0.676440 0.431507 0.430231 11.00000 0.03693 0.03814 = 0.03728 -0.00198 -0.00142 -0.00928 C61 1 0.660632 0.524422 0.322625 11.00000 0.03502 0.03697 = 0.02685 -0.00122 -0.00233 -0.00563 C62 1 0.638132 0.617980 0.341969 11.00000 0.04302 0.03220 = 0.02697 0.00014 -0.00656 -0.00522 AFIX 43 H62 2 0.688413 0.639635 0.361124 11.00000 -1.20000 AFIX 0 C63 1 0.541303 0.678866 0.332818 11.00000 0.04393 0.03673 = 0.02885 -0.00467 -0.00885 -0.00931 C64 1 0.465710 0.643993 0.305401 11.00000 0.03340 0.04736 = 0.04664 -0.00135 -0.01587 0.00132 AFIX 43 H64 2 0.399871 0.683799 0.299585 11.00000 -1.20000 AFIX 0 C65 1 0.488107 0.550197 0.286722 11.00000 0.04589 0.05293 = 0.04854 -0.01526 -0.01227 -0.01401 AFIX 43 H65 2 0.437062 0.526769 0.268902 11.00000 -1.20000 AFIX 0 C66 1 0.584893 0.492703 0.294564 11.00000 0.04647 0.04382 = 0.03697 -0.00907 -0.00432 -0.00908 AFIX 43 H66 2 0.600457 0.430990 0.280829 11.00000 -1.20000 AFIX 0 C31B 1 0.584930 0.915138 0.385592 11.00000 0.04279 0.03879 = 0.04475 0.00256 -0.00961 -0.00552 N32B 3 0.558017 0.951732 0.431387 11.00000 0.07120 0.03807 = 0.04249 -0.00489 -0.00485 -0.00177 C33B 1 0.559240 1.049613 0.432232 11.00000 0.08910 0.04032 = 0.04778 -0.01293 -0.01203 -0.00428 AFIX 43 H33B 2 0.545015 1.079251 0.463388 11.00000 -1.20000 AFIX 0 C34B 1 0.581383 1.106926 0.387361 11.00000 0.08299 0.03166 = 0.06512 -0.00387 -0.01408 -0.01797 C35B 1 0.607335 1.060876 0.343095 11.00000 0.08332 0.04684 = 0.05061 0.00643 0.00348 -0.01440 AFIX 43 H35B 2 0.621457 1.099474 0.312647 11.00000 -1.20000 AFIX 0 N36B 3 0.613428 0.962339 0.341464 11.00000 0.07823 0.03697 = 0.04629 -0.00515 -0.00246 -0.01270 MOLE 3 CL1A 5 0.774269 -0.114856 0.172891 11.00000 0.13431 0.11617 = 0.12691 0.01933 0.03300 -0.01699 CL2A 5 0.825072 -0.282453 0.250230 11.00000 0.11325 0.12512 = 0.14610 0.02613 -0.05849 -0.03466 CL3A 5 0.634018 -0.254471 0.197583 11.00000 0.11832 0.21300 = 0.15325 0.04731 -0.05389 -0.06800 C1S 1 0.722685 -0.192461 0.223006 11.00000 0.11923 0.08204 = 0.08085 0.02449 -0.00528 -0.02657 AFIX 13 H1S 2 0.687525 -0.151752 0.250111 11.00000 -1.20000 AFIX 0 MOLE 4 CL1B 5 0.829295 0.189567 0.475560 11.00000 0.15919 0.07214 = 0.08036 0.00356 0.00337 -0.02582 CL2B 5 0.826012 -0.011579 0.516058 11.00000 0.26437 0.06428 = 0.12056 -0.01139 0.03363 -0.04419 CL3B 5 0.702422 0.150294 0.563534 11.00000 0.22398 0.17859 = 0.27079 -0.05703 0.18044 -0.05062 C2S 1 0.816532 0.110910 0.530882 11.00000 0.08947 0.06590 = 0.07189 -0.00361 -0.00465 -0.02275 AFIX 13 H2S 2 0.875272 0.113747 0.553598 11.00000 -1.20000 AFIX 0 MOLE 5 CL1C 5 0.739012 0.124677 -0.014537 11.00000 0.08861 0.10698 = 0.11635 -0.03475 0.02700 -0.01533 CL2C 5 0.826990 0.257109 0.044547 11.00000 0.11489 0.12422 = 0.17553 0.00207 -0.07184 -0.02462 CL3C 5 0.627375 0.323023 -0.002712 11.00000 0.10221 0.09505 = 0.18093 -0.02578 -0.05983 0.00420 C3S 1 0.716754 0.225347 0.023579 11.00000 0.07376 0.08780 = 0.12858 -0.02723 -0.00299 -0.02135 AFIX 13 H3S 2 0.681241 0.200501 0.055366 11.00000 -1.20000 AFIX 0 MOLE 6 PART -1 CL1D 5 0.339026 0.204225 0.264684 10.75000 0.13809 0.07815 = 0.11879 -0.00235 0.04694 -0.01341 CL2D 5 0.172623 0.092707 0.270184 10.75000 0.09185 0.21471 = 0.16331 -0.03115 -0.01486 -0.03489 CL3D 5 0.289870 0.102296 0.360499 10.75000 0.21643 0.15601 = 0.05487 -0.00442 0.01851 -0.01331 C4S 1 0.293905 0.095428 0.291816 10.75000 0.06671 0.07648 = 0.02503 -0.02078 -0.00850 0.00264 AFIX 13 H4S 2 0.343353 0.035918 0.282728 10.75000 -1.20000 AFIX 0 PART -2 CL4D 5 0.256507 0.180154 0.249797 10.25000 0.21925 0.09430 = 0.10188 0.00777 -0.00041 0.01405 CL5D 5 0.189988 0.023513 0.307811 10.25000 0.08206 0.17393 = 0.14032 -0.03012 0.01712 -0.04371 CL6D 5 0.323676 0.131577 0.353824 10.25000 0.12804 0.17890 = 0.14314 -0.08034 -0.06541 0.02288 C5S 1 0.302486 0.091751 0.309499 10.25000 0.06000 0.08341 = 0.05990 -0.03016 0.01572 0.01616 AFIX 13 H5S 2 0.366762 0.046955 0.299245 10.25000 -1.20000 PART 0 HKLF 4 REM 11-124 is 2,6_BrIO3:2CHCl3 in P-1 at 40kV30mA to 0.80\%A REM R1 = 0.0793 for 8469 Fo > 4sig(Fo) and 0.1883 for all 18957 data REM 1153 parameters refined using 30 restraints END WGHT 0.0601 2.4787 REM Highest difference peak 1.263, deepest hole -1.190, 1-sigma level 0.085 Q1 1 0.2135 0.4085 -0.1003 11.00000 0.05 1.26 Q2 1 0.7826 0.2066 0.0755 11.00000 0.05 1.05 Q3 1 0.2545 -0.3112 0.1490 11.00000 0.05 0.63 Q4 1 0.6841 0.1790 0.5426 11.00000 0.05 0.57 Q5 1 0.6824 0.0916 0.5440 11.00000 0.05 0.54 Q6 1 0.7847 0.1277 0.5791 11.00000 0.05 0.52 Q7 1 0.7094 -0.3182 0.1760 11.00000 0.05 0.49 Q8 1 0.7386 0.1816 0.4786 11.00000 0.05 0.47 Q9 1 0.8759 -0.2674 0.2129 11.00000 0.05 0.43 Q10 1 0.6018 1.2428 0.3916 11.00000 0.05 0.42 ; loop_ _geom_hbond_atom_site_label_D _geom_hbond_atom_site_label_H _geom_hbond_atom_site_label_A _geom_hbond_distance_DH _geom_hbond_distance_HA _geom_hbond_distance_DA _geom_hbond_angle_DHA _geom_hbond_site_symmetry_A _geom_hbond_publ_flag # # Hydrogen bonding scheme # ======== ======= ====== # # D H A D-H H...A D...A D-H...A symm publ # - - - --- ----- ----- ------- ---- ---- C3S H3S O1A 0.98 2.22 3.004(11) 136 . yes C4S H4S N16A 0.98 2.49 3.208(19) 130 . yes C12 H12 N1A 0.93 2.54 2.875(9) 101 . yes C22 H22 N2A 0.93 2.56 2.883(8) 101 . yes C52 H52 N2B 0.93 2.60 2.919(8) 101 . yes C62 H62 N3B 0.93 2.60 2.912(7) 100 . yes C44 H44 O3B 0.93 2.56 3.291(8) 135 2_766 yes C2S H2S N12B 0.98 2.58 3.533(11) 165 2_766 yes _database_code_depnum_ccdc_archive 'CCDC 930691' ####################################################################### # # Cambridge Crystallographic Data Centre # CCDC # ####################################################################### # # This CIF contains data from an original supplementary publication # deposited with the CCDC, and may include chemical, crystal, # experimental, refinement, atomic coordinates, # anisotropic displacement parameters and molecular geometry data, # as required by the journal to which it was submitted. # # This CIF is provided on the understanding that it is used for bona # fide research purposes only. It may contain copyright material # of the CCDC or of third parties, and may not be copied or further # disseminated in any form, whether machine-readable or not, # except for the purpose of generating routine backup copies # on your local computer system. # # For further information on the CCDC, data deposition and # data retrieval see: # www.ccdc.cam.ac.uk # # Bona fide researchers may freely download Mercury and enCIFer # from this site to visualise CIF-encoded structures and # to carry out CIF format checking respectively. # data_B_[11-125] #TrackingRef 'Bromo_JFG_v09.cif' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common (26BrIO)3_CH2Cl2_[11-125] _chemical_melting_point ? _chemical_formula_moiety 'C36 H18 Br3 N9 O6, 2(C H2 Cl2)' _chemical_formula_sum 'C38 H22 Br3 Cl4 N9 O6' _chemical_formula_weight 1082.18 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' N N 0.0061 0.0033 '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' Cl Cl 0.1484 0.1585 '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 Triclinic _symmetry_space_group_name_H-M 'P -1' _symmetry_space_group_name_Hall '-P 1' loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, -y, -z' _cell_length_a 12.2390(5) _cell_length_b 13.6149(5) _cell_length_c 13.6447(5) _cell_angle_alpha 100.749(3) _cell_angle_beta 99.990(3) _cell_angle_gamma 95.463(3) _cell_volume 2180.69(14) _cell_formula_units_Z 2 _cell_measurement_temperature 294(2) _cell_measurement_reflns_used 4213 _cell_measurement_theta_min 2.06 _cell_measurement_theta_max 27.75 _exptl_crystal_description Block _exptl_crystal_colour Colourless _exptl_crystal_size_max 0.49 _exptl_crystal_size_mid 0.38 _exptl_crystal_size_min 0.15 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.648 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1068 _exptl_absorpt_coefficient_mu 3.076 _exptl_absorpt_correction_type Analytical _exptl_absorpt_correction_T_min 0.3141 _exptl_absorpt_correction_T_max 0.6555 _exptl_absorpt_process_details '(ABSFAC, Clark and Reid, 1998)' _exptl_special_details ; [11-125] C--Br...O=C Short contacts Distance X...O 2.982(3) Br14...O4_$3 Angle C--X...O 149.4(1) C14--Br14...O4_$3 Angle X...O=C 111.7(3) Br14...(O4--C4)_$3 The symmetry code $3 is detailed in the 11-125.res file below in the '_iucr_refine_instructions_details' section. ; _diffrn_ambient_temperature 294(1) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'Enhance (Mo) X-ray Source' _diffrn_radiation_monochromator graphite _diffrn_measurement_device 'Xcalibur, Sapphire3, Gemini Ultra' _diffrn_measurement_method '\w scans' _diffrn_standards_number 4213 _diffrn_standards_interval_time 60 _diffrn_standards_decay_% 1 _diffrn_reflns_number 16290 _diffrn_reflns_av_R_equivalents 0.0238 _diffrn_reflns_av_sigmaI/netI 0.0513 _diffrn_reflns_limit_h_min -14 _diffrn_reflns_limit_h_max 15 _diffrn_reflns_limit_k_min -17 _diffrn_reflns_limit_k_max 17 _diffrn_reflns_limit_l_min -17 _diffrn_reflns_limit_l_max 17 _diffrn_reflns_theta_min 2.07 _diffrn_reflns_theta_max 27.85 _diffrn_measured_fraction_theta_max 0.906 _diffrn_reflns_theta_full 26.00 _diffrn_measured_fraction_theta_full 0.999 _reflns_number_total 9391 _reflns_number_gt 5817 _reflns_threshold_expression I>2\s(I) _computing_data_collection ; CrysAlisPro, Agilent Technologies, Version 1.171.34.49 (release 20-01-2011 CrysAlis171 .NET) (compiled Jan 20 2011,15:58:25) ; _computing_cell_refinement ; CrysAlisPro, Agilent Technologies, Version 1.171.34.49 (release 20-01-2011 CrysAlis171 .NET) (compiled Jan 20 2011,15:58:25) ; _computing_data_reduction ; CrysAlisPro, Agilent Technologies, Version 1.171.34.49 (release 20-01-2011 CrysAlis171 .NET) (compiled Jan 20 2011,15:58:25) ; _computing_structure_solution 'SHELXS97 (Sheldrick, 2008)' _computing_structure_refinement 'SHELXL97 (Sheldrick, 2008) and SORTX (McArdle, 1995)' _computing_molecular_graphics 'PLATON (Spek, 2009)' _computing_publication_material SHELXL97 _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 'w=1/[\s^2^(Fo^2^)+(0.0777P)^2^+4.2375P] 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 constr _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 9391 _refine_ls_number_parameters 568 _refine_ls_number_restraints 47 _refine_ls_R_factor_all 0.1119 _refine_ls_R_factor_gt 0.0667 _refine_ls_wR_factor_ref 0.1867 _refine_ls_wR_factor_gt 0.1607 _refine_ls_goodness_of_fit_ref 1.013 _refine_ls_restrained_S_all 1.030 _refine_ls_shift/su_max 0.001 _refine_ls_shift/su_mean 0.000 _refine_diff_density_max 1.449 _refine_diff_density_min -1.295 _refine_diff_density_rms 0.083 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 Br14 Br 0.27480(7) 0.12895(5) 0.25571(4) 0.0729(2) Uani 1 1 d . . . Br24 Br 0.17378(7) 0.66974(5) 1.02941(7) 0.0896(3) Uani 1 1 d . . . Br34 Br 0.02104(10) 0.29465(7) 0.22350(5) 0.1091(4) Uani 1 1 d . . . O1 O 0.5710(3) 0.3428(3) 0.8007(3) 0.0624(11) Uani 1 1 d . . . C1 C 0.4802(4) 0.3139(4) 0.7479(4) 0.0441(12) Uani 1 1 d . . . N1 N 0.4509(3) 0.2108(3) 0.6985(3) 0.0443(10) Uani 1 1 d . . . O2 O 0.5376(5) 0.0689(4) 0.6823(3) 0.0933(17) Uani 1 1 d . . . C2 C 0.5070(5) 0.1353(5) 0.7375(4) 0.0538(14) Uani 1 1 d . . . O3 O 0.4318(3) 0.2951(3) 1.1581(3) 0.0499(9) Uani 1 1 d . . . C3 C 0.3989(4) 0.2510(3) 1.0723(3) 0.0351(10) Uani 1 1 d . . . N2 N 0.2847(3) 0.2568(3) 1.0207(3) 0.0328(8) Uani 1 1 d . . . O4 O 0.2397(3) 0.0957(2) 1.0296(2) 0.0417(8) Uani 1 1 d . . . C4 C 0.2105(4) 0.1691(3) 0.9989(3) 0.0312(9) Uani 1 1 d . . . O5 O -0.1189(3) 0.1576(4) 0.6103(3) 0.0780(15) Uani 1 1 d . . . C5 C -0.0419(4) 0.2013(4) 0.6754(4) 0.0474(13) Uani 1 1 d . . . N3 N 0.0364(3) 0.2742(3) 0.6551(3) 0.0411(10) Uani 1 1 d . . . O6 O 0.0258(3) 0.4023(3) 0.7875(3) 0.0573(10) Uani 1 1 d . . . C6 C 0.0794(4) 0.3661(4) 0.7281(4) 0.0423(12) Uani 1 1 d . . . C11 C 0.1968(4) 0.4062(4) 0.7301(3) 0.0394(11) Uani 1 1 d . . . C12 C 0.2771(4) 0.3415(4) 0.7193(3) 0.0383(11) Uani 1 1 d . . . H12 H 0.2555 0.2723 0.6986 0.046 Uiso 1 1 calc R . . C13 C 0.3900(4) 0.3802(4) 0.7393(3) 0.0436(12) Uani 1 1 d . . . C14 C 0.4203(5) 0.4840(4) 0.7638(4) 0.0537(14) Uani 1 1 d . . . H14 H 0.4955 0.5106 0.7764 0.064 Uiso 1 1 calc R . . C15 C 0.3398(5) 0.5482(4) 0.7698(5) 0.0598(16) Uani 1 1 d . . . H15 H 0.3606 0.6176 0.7830 0.072 Uiso 1 1 calc R . . C16 C 0.2289(5) 0.5096(4) 0.7562(4) 0.0522(13) Uani 1 1 d . . . H16 H 0.1753 0.5530 0.7646 0.063 Uiso 1 1 calc R . . C11A C 0.4074(4) 0.1908(4) 0.5919(4) 0.0461(12) Uani 1 1 d . . . N12A N 0.4397(5) 0.2598(4) 0.5438(3) 0.0646(14) Uani 1 1 d . . . C13A C 0.3982(6) 0.2408(5) 0.4440(4) 0.0671(17) Uani 1 1 d . . . H13A H 0.4173 0.2875 0.4059 0.081 Uiso 1 1 calc R . . C14A C 0.3280(5) 0.1543(4) 0.3963(4) 0.0523(14) Uani 1 1 d . . . C15A C 0.3008(5) 0.0878(4) 0.4539(4) 0.0603(16) Uani 1 1 d . . . H15A H 0.2543 0.0281 0.4226 0.072 Uiso 1 1 calc R . . N16A N 0.3390(4) 0.1059(3) 0.5540(3) 0.0565(12) Uani 1 1 d . . . C21 C 0.5192(4) 0.1406(4) 0.8485(4) 0.0417(11) Uani 1 1 d . . . C22 C 0.4500(4) 0.1890(4) 0.9057(3) 0.0384(11) Uani 1 1 d . . . H22 H 0.3922 0.2190 0.8745 0.046 Uiso 1 1 calc R . . C23 C 0.4666(4) 0.1929(3) 1.0098(3) 0.0339(10) Uani 1 1 d . . . C24 C 0.5516(4) 0.1470(4) 1.0562(4) 0.0437(12) Uani 1 1 d . . . H24 H 0.5639 0.1511 1.1262 0.052 Uiso 1 1 calc R . . C25 C 0.6176(4) 0.0956(4) 0.9988(4) 0.0504(13) Uani 1 1 d . . . H25 H 0.6737 0.0634 1.0296 0.060 Uiso 1 1 calc R . . C26 C 0.6010(4) 0.0914(4) 0.8955(4) 0.0488(13) Uani 1 1 d . . . H26 H 0.6451 0.0553 0.8568 0.059 Uiso 1 1 calc R . . C21A C 0.2562(4) 0.3555(3) 1.0242(3) 0.0339(10) Uani 1 1 d . . . N22A N 0.1600(3) 0.3739(3) 1.0501(3) 0.0428(10) Uani 1 1 d . . . C23A C 0.1372(5) 0.4680(4) 1.0516(4) 0.0506(13) Uani 1 1 d . . . H23A H 0.0702 0.4855 1.0685 0.061 Uiso 1 1 calc R . . C24A C 0.2086(5) 0.5386(4) 1.0293(4) 0.0493(13) Uani 1 1 d . . . C25A C 0.3087(5) 0.5125(4) 1.0075(4) 0.0512(14) Uani 1 1 d . . . H25A H 0.3602 0.5612 0.9952 0.061 Uiso 1 1 calc R . . N26A N 0.3336(4) 0.4187(3) 1.0034(3) 0.0431(10) Uani 1 1 d . . . C31 C 0.0984(4) 0.1646(3) 0.9343(3) 0.0308(9) Uani 1 1 d . . . C32 C 0.0835(4) 0.1955(3) 0.8426(3) 0.0343(10) Uani 1 1 d . . . H32 H 0.1439 0.2283 0.8232 0.041 Uiso 1 1 calc R . . C33 C -0.0214(4) 0.1778(3) 0.7791(3) 0.0355(10) Uani 1 1 d . . . C34 C -0.1113(4) 0.1308(4) 0.8099(4) 0.0413(11) Uani 1 1 d . . . H34 H -0.1819 0.1193 0.7682 0.050 Uiso 1 1 calc R . . C35 C -0.0965(4) 0.1010(4) 0.9015(4) 0.0424(12) Uani 1 1 d . . . H35 H -0.1572 0.0695 0.9215 0.051 Uiso 1 1 calc R . . C36 C 0.0078(4) 0.1173(3) 0.9639(4) 0.0367(10) Uani 1 1 d . . . H36 H 0.0173 0.0967 1.0258 0.044 Uiso 1 1 calc R . . C31A C 0.0362(4) 0.2789(4) 0.5516(4) 0.0442(12) Uani 1 1 d . . . N32A N 0.0282(4) 0.3683(3) 0.5290(3) 0.0545(12) Uani 1 1 d . . . C33A C 0.0270(6) 0.3725(5) 0.4326(4) 0.0633(16) Uani 1 1 d . . . H33A H 0.0240 0.4342 0.4131 0.076 Uiso 1 1 calc R . . C34A C 0.0300(5) 0.2883(5) 0.3610(4) 0.0616(16) Uani 1 1 d . . . C35A C 0.0395(5) 0.1996(5) 0.3927(4) 0.0611(15) Uani 1 1 d . . . H35A H 0.0419 0.1416 0.3452 0.073 Uiso 1 1 calc R . . N36A N 0.0456(4) 0.1936(4) 0.4900(3) 0.0553(12) Uani 1 1 d . . . Cl1S Cl -0.2250(4) 0.0299(3) 0.2574(3) 0.1741(14) Uani 1 1 d . . . Cl2S Cl -0.2865(4) 0.2140(3) 0.3516(3) 0.2006(18) Uani 1 1 d . . . C1S C -0.2642(10) 0.0953(7) 0.3633(7) 0.126(4) Uani 1 1 d . . . H1S1 H -0.3322 0.0595 0.3739 0.151 Uiso 1 1 calc R . . H1S2 H -0.2061 0.0986 0.4225 0.151 Uiso 1 1 calc R . . Cl3S Cl 0.6732(6) 0.4778(5) 0.4896(4) 0.215(3) Uani 0.80 1 d PU A -1 Cl4S Cl 0.7379(12) 0.5037(12) 0.6837(9) 0.378(7) Uani 0.80 1 d PU A -1 C2S C 0.714(3) 0.400(2) 0.584(2) 0.253(11) Uani 0.80 1 d PU A -1 H2S1 H 0.6531 0.3500 0.5872 0.303 Uiso 0.80 1 calc PR A -1 H2S2 H 0.7802 0.3688 0.5750 0.303 Uiso 0.80 1 calc PR A -1 Cl5S Cl 0.7060(11) 0.5439(8) 0.6956(8) 0.082(3) Uani 0.20 1 d PDU B -2 Cl6S Cl 0.7850(10) 0.4097(12) 0.6611(12) 0.113(4) Uani 0.20 1 d PDU B -2 C3S C 0.6638(18) 0.4422(17) 0.5959(16) 0.041(4) Uani 0.20 1 d PDU B -2 H3S1 H 0.6674 0.4555 0.5291 0.050 Uiso 0.20 1 calc PR B -2 H3S2 H 0.5950 0.4010 0.5968 0.050 Uiso 0.20 1 calc PR B -2 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 Br14 0.1191(6) 0.0628(4) 0.0318(3) 0.0086(3) 0.0044(3) 0.0085(4) Br24 0.1102(6) 0.0373(3) 0.1094(6) 0.0120(3) -0.0143(5) 0.0223(3) Br34 0.1838(10) 0.1191(7) 0.0416(4) 0.0344(4) 0.0323(5) 0.0511(7) O1 0.042(2) 0.073(3) 0.061(2) 0.007(2) -0.0065(19) -0.0069(19) C1 0.042(3) 0.054(3) 0.033(2) 0.008(2) 0.007(2) -0.007(2) N1 0.045(2) 0.054(3) 0.029(2) 0.0045(18) 0.0022(17) 0.002(2) O2 0.117(4) 0.117(4) 0.050(3) -0.001(3) 0.014(3) 0.075(3) C2 0.046(3) 0.070(4) 0.043(3) 0.003(3) 0.008(2) 0.018(3) O3 0.048(2) 0.056(2) 0.0383(19) -0.0005(16) -0.0024(16) 0.0071(17) C3 0.030(2) 0.036(2) 0.037(2) 0.010(2) 0.0001(19) -0.0001(19) N2 0.032(2) 0.0303(19) 0.0349(19) 0.0076(15) 0.0019(15) 0.0032(15) O4 0.046(2) 0.0369(18) 0.0437(18) 0.0181(15) 0.0016(15) 0.0042(15) C4 0.037(2) 0.032(2) 0.025(2) 0.0071(18) 0.0077(18) 0.0032(19) O5 0.061(3) 0.114(4) 0.044(2) 0.026(2) -0.0148(19) -0.039(3) C5 0.042(3) 0.060(3) 0.036(3) 0.016(2) -0.005(2) -0.006(2) N3 0.041(2) 0.049(2) 0.031(2) 0.0153(18) -0.0029(17) -0.0052(19) O6 0.058(2) 0.056(2) 0.062(2) 0.012(2) 0.020(2) 0.0114(19) C6 0.046(3) 0.044(3) 0.037(3) 0.016(2) 0.001(2) 0.006(2) C11 0.045(3) 0.041(3) 0.030(2) 0.011(2) 0.001(2) -0.001(2) C12 0.042(3) 0.037(2) 0.030(2) 0.0079(19) 0.002(2) -0.011(2) C13 0.049(3) 0.046(3) 0.030(2) 0.006(2) -0.001(2) -0.005(2) C14 0.051(3) 0.052(3) 0.049(3) 0.006(3) 0.002(3) -0.013(3) C15 0.067(4) 0.039(3) 0.064(4) 0.009(3) -0.004(3) -0.010(3) C16 0.061(4) 0.042(3) 0.048(3) 0.009(2) -0.001(3) 0.002(3) C11A 0.048(3) 0.053(3) 0.034(2) 0.006(2) 0.006(2) 0.001(2) N12A 0.083(4) 0.064(3) 0.038(2) 0.006(2) 0.012(2) -0.022(3) C13A 0.094(5) 0.063(4) 0.041(3) 0.014(3) 0.015(3) -0.013(3) C14A 0.073(4) 0.050(3) 0.032(3) 0.006(2) 0.009(2) 0.005(3) C15A 0.089(4) 0.045(3) 0.036(3) 0.005(2) -0.003(3) -0.009(3) N16A 0.077(3) 0.048(3) 0.038(2) 0.010(2) 0.001(2) -0.008(2) C21 0.028(2) 0.049(3) 0.045(3) 0.004(2) 0.004(2) 0.008(2) C22 0.031(2) 0.044(3) 0.038(2) 0.008(2) -0.001(2) 0.009(2) C23 0.026(2) 0.035(2) 0.040(2) 0.0090(19) 0.0020(19) 0.0003(18) C24 0.036(3) 0.054(3) 0.042(3) 0.018(2) 0.002(2) 0.005(2) C25 0.036(3) 0.058(3) 0.059(3) 0.020(3) 0.001(2) 0.018(2) C26 0.034(3) 0.052(3) 0.060(3) 0.005(3) 0.008(2) 0.014(2) C21A 0.037(3) 0.033(2) 0.028(2) 0.0038(18) 0.0010(19) 0.004(2) N22A 0.040(2) 0.040(2) 0.047(2) 0.0064(18) 0.0044(19) 0.0069(18) C23A 0.047(3) 0.045(3) 0.055(3) 0.004(2) -0.001(2) 0.017(2) C24A 0.065(4) 0.031(3) 0.044(3) 0.003(2) -0.009(3) 0.013(3) C25A 0.071(4) 0.032(3) 0.046(3) 0.010(2) 0.004(3) -0.008(3) N26A 0.052(3) 0.034(2) 0.043(2) 0.0074(18) 0.0108(19) 0.0003(19) C31 0.034(2) 0.025(2) 0.033(2) 0.0060(17) 0.0046(18) 0.0029(18) C32 0.033(2) 0.035(2) 0.031(2) 0.0078(18) 0.0036(18) -0.0076(19) C33 0.034(2) 0.035(2) 0.034(2) 0.0087(19) -0.0007(19) -0.0048(19) C34 0.033(3) 0.041(3) 0.046(3) 0.011(2) -0.001(2) -0.004(2) C35 0.033(3) 0.042(3) 0.053(3) 0.019(2) 0.006(2) -0.006(2) C36 0.040(3) 0.032(2) 0.041(2) 0.014(2) 0.010(2) 0.003(2) C31A 0.039(3) 0.055(3) 0.036(3) 0.015(2) 0.000(2) -0.006(2) N32A 0.073(3) 0.054(3) 0.038(2) 0.018(2) 0.007(2) 0.006(2) C33A 0.090(5) 0.064(4) 0.041(3) 0.027(3) 0.007(3) 0.012(3) C34A 0.072(4) 0.082(4) 0.037(3) 0.025(3) 0.012(3) 0.012(3) C35A 0.080(4) 0.063(4) 0.042(3) 0.010(3) 0.015(3) 0.011(3) N36A 0.071(3) 0.055(3) 0.043(2) 0.016(2) 0.012(2) 0.007(2) Cl1S 0.203(4) 0.175(3) 0.115(2) -0.006(2) 0.017(2) -0.023(3) Cl2S 0.269(5) 0.130(3) 0.193(4) 0.068(3) -0.013(3) 0.018(3) C1S 0.184(10) 0.091(6) 0.082(6) 0.030(5) -0.012(6) -0.037(6) Cl3S 0.291(6) 0.237(6) 0.120(3) 0.086(3) 0.024(4) -0.023(5) Cl4S 0.414(14) 0.465(15) 0.227(8) 0.046(10) 0.104(9) -0.099(12) C2S 0.28(2) 0.254(17) 0.209(16) 0.062(12) 0.009(15) -0.017(15) Cl5S 0.107(6) 0.075(5) 0.048(4) -0.010(4) 0.016(4) -0.024(4) Cl6S 0.088(6) 0.136(7) 0.124(8) 0.049(6) 0.006(5) 0.037(6) C3S 0.044(8) 0.047(8) 0.030(7) 0.010(6) 0.011(6) -0.020(7) _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 Br14 C14A 1.871(5) . ? Br24 C24A 1.874(5) . ? Br34 C34A 1.879(5) . ? O1 C1 1.200(6) . ? C1 N1 1.422(6) . ? C1 C13 1.494(8) . ? N1 C2 1.421(7) . ? N1 C11A 1.425(6) . ? O2 C2 1.198(7) . ? C2 C21 1.484(7) . ? O3 C3 1.192(5) . ? C3 N2 1.468(6) . ? C3 C23 1.470(7) . ? N2 C4 1.381(6) . ? N2 C21A 1.414(6) . ? O4 C4 1.215(5) . ? C4 C31 1.485(6) . ? O5 C5 1.199(6) . ? C5 N3 1.411(6) . ? C5 C33 1.493(6) . ? N3 C31A 1.424(6) . ? N3 C6 1.436(6) . ? O6 C6 1.195(6) . ? C6 C11 1.481(7) . ? C11 C16 1.387(7) . ? C11 C12 1.390(7) . ? C12 C13 1.392(7) . ? C12 H12 0.9300 . ? C13 C14 1.389(7) . ? C14 C15 1.380(8) . ? C14 H14 0.9300 . ? C15 C16 1.376(8) . ? C15 H15 0.9300 . ? C16 H16 0.9300 . ? C11A N12A 1.311(7) . ? C11A N16A 1.321(7) . ? N12A C13A 1.336(7) . ? C13A C14A 1.369(8) . ? C13A H13A 0.9300 . ? C14A C15A 1.359(8) . ? C15A N16A 1.332(7) . ? C15A H15A 0.9300 . ? C21 C22 1.380(7) . ? C21 C26 1.387(7) . ? C22 C23 1.390(6) . ? C22 H22 0.9300 . ? C23 C24 1.385(6) . ? C24 C25 1.371(7) . ? C24 H24 0.9300 . ? C25 C26 1.379(8) . ? C25 H25 0.9300 . ? C26 H26 0.9300 . ? C21A N22A 1.320(6) . ? C21A N26A 1.322(6) . ? N22A C23A 1.335(6) . ? C23A C24A 1.349(8) . ? C23A H23A 0.9300 . ? C24A C25A 1.374(8) . ? C25A N26A 1.334(6) . ? C25A H25A 0.9300 . ? C31 C32 1.381(6) . ? C31 C36 1.387(6) . ? C32 C33 1.391(6) . ? C32 H32 0.9300 . ? C33 C34 1.386(6) . ? C34 C35 1.373(7) . ? C34 H34 0.9300 . ? C35 C36 1.379(7) . ? C35 H35 0.9300 . ? C36 H36 0.9300 . ? C31A N32A 1.318(7) . ? C31A N36A 1.329(7) . ? N32A C33A 1.325(7) . ? C33A C34A 1.368(9) . ? C33A H33A 0.9300 . ? C34A C35A 1.366(8) . ? C35A N36A 1.335(7) . ? C35A H35A 0.9300 . ? Cl1S C1S 1.718(11) . ? Cl2S C1S 1.697(10) . ? C1S H1S1 0.9700 . ? C1S H1S2 0.9700 . ? Cl3S C2S 1.84(3) . ? Cl4S C2S 1.73(3) . ? C2S H2S1 0.9700 . ? C2S H2S2 0.9700 . ? Cl5S C3S 1.72(2) . ? Cl5S Cl6S 2.16(2) . ? Cl6S C3S 1.73(2) . ? C3S H3S1 0.9700 . ? C3S H3S2 0.9700 . ? 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 O1 C1 N1 120.4(5) . . ? O1 C1 C13 122.4(5) . . ? N1 C1 C13 116.9(4) . . ? C2 N1 C1 120.2(4) . . ? C2 N1 C11A 117.1(4) . . ? C1 N1 C11A 116.6(4) . . ? O2 C2 N1 121.2(5) . . ? O2 C2 C21 122.4(5) . . ? N1 C2 C21 116.3(5) . . ? O3 C3 N2 119.7(4) . . ? O3 C3 C23 124.7(4) . . ? N2 C3 C23 115.5(4) . . ? C4 N2 C21A 126.1(4) . . ? C4 N2 C3 116.3(4) . . ? C21A N2 C3 115.2(3) . . ? O4 C4 N2 119.3(4) . . ? O4 C4 C31 121.1(4) . . ? N2 C4 C31 119.6(4) . . ? O5 C5 N3 120.9(4) . . ? O5 C5 C33 121.8(5) . . ? N3 C5 C33 117.3(4) . . ? C5 N3 C31A 118.1(4) . . ? C5 N3 C6 121.0(4) . . ? C31A N3 C6 115.6(4) . . ? O6 C6 N3 121.3(5) . . ? O6 C6 C11 123.2(5) . . ? N3 C6 C11 115.3(5) . . ? C16 C11 C12 119.9(5) . . ? C16 C11 C6 119.0(5) . . ? C12 C11 C6 120.6(4) . . ? C11 C12 C13 120.0(4) . . ? C11 C12 H12 120.0 . . ? C13 C12 H12 120.0 . . ? C14 C13 C12 119.2(5) . . ? C14 C13 C1 118.5(5) . . ? C12 C13 C1 121.9(4) . . ? C15 C14 C13 120.5(5) . . ? C15 C14 H14 119.7 . . ? C13 C14 H14 119.7 . . ? C16 C15 C14 120.1(5) . . ? C16 C15 H15 119.9 . . ? C14 C15 H15 119.9 . . ? C15 C16 C11 120.1(5) . . ? C15 C16 H16 120.0 . . ? C11 C16 H16 120.0 . . ? N12A C11A N16A 128.1(5) . . ? N12A C11A N1 115.6(5) . . ? N16A C11A N1 116.3(4) . . ? C11A N12A C13A 115.3(5) . . ? N12A C13A C14A 121.6(5) . . ? N12A C13A H13A 119.2 . . ? C14A C13A H13A 119.2 . . ? C15A C14A C13A 118.0(5) . . ? C15A C14A Br14 121.8(4) . . ? C13A C14A Br14 120.2(4) . . ? N16A C15A C14A 121.7(5) . . ? N16A C15A H15A 119.1 . . ? C14A C15A H15A 119.1 . . ? C11A N16A C15A 115.3(5) . . ? C22 C21 C26 119.0(5) . . ? C22 C21 C2 122.6(4) . . ? C26 C21 C2 118.3(5) . . ? C21 C22 C23 120.1(4) . . ? C21 C22 H22 120.0 . . ? C23 C22 H22 120.0 . . ? C24 C23 C22 120.1(4) . . ? C24 C23 C3 119.4(4) . . ? C22 C23 C3 120.3(4) . . ? C25 C24 C23 119.8(5) . . ? C25 C24 H24 120.1 . . ? C23 C24 H24 120.1 . . ? C24 C25 C26 120.1(5) . . ? C24 C25 H25 119.9 . . ? C26 C25 H25 119.9 . . ? C25 C26 C21 120.8(5) . . ? C25 C26 H26 119.6 . . ? C21 C26 H26 119.6 . . ? N22A C21A N26A 128.5(4) . . ? N22A C21A N2 117.5(4) . . ? N26A C21A N2 113.9(4) . . ? C21A N22A C23A 114.9(4) . . ? N22A C23A C24A 121.9(5) . . ? N22A C23A H23A 119.0 . . ? C24A C23A H23A 119.0 . . ? C23A C24A C25A 118.3(5) . . ? C23A C24A Br24 121.3(4) . . ? C25A C24A Br24 120.4(4) . . ? N26A C25A C24A 121.5(5) . . ? N26A C25A H25A 119.2 . . ? C24A C25A H25A 119.2 . . ? C21A N26A C25A 114.7(4) . . ? C32 C31 C36 119.8(4) . . ? C32 C31 C4 122.7(4) . . ? C36 C31 C4 117.2(4) . . ? C31 C32 C33 120.3(4) . . ? C31 C32 H32 119.9 . . ? C33 C32 H32 119.9 . . ? C34 C33 C32 119.3(4) . . ? C34 C33 C5 117.3(4) . . ? C32 C33 C5 123.2(4) . . ? C35 C34 C33 120.3(4) . . ? C35 C34 H34 119.8 . . ? C33 C34 H34 119.8 . . ? C34 C35 C36 120.5(4) . . ? C34 C35 H35 119.8 . . ? C36 C35 H35 119.8 . . ? C35 C36 C31 119.9(4) . . ? C35 C36 H36 120.1 . . ? C31 C36 H36 120.1 . . ? N32A C31A N36A 127.8(5) . . ? N32A C31A N3 115.7(5) . . ? N36A C31A N3 116.4(5) . . ? C31A N32A C33A 115.7(5) . . ? N32A C33A C34A 121.7(5) . . ? N32A C33A H33A 119.2 . . ? C34A C33A H33A 119.2 . . ? C35A C34A C33A 117.8(5) . . ? C35A C34A Br34 121.1(5) . . ? C33A C34A Br34 121.0(5) . . ? N36A C35A C34A 121.9(6) . . ? N36A C35A H35A 119.0 . . ? C34A C35A H35A 119.0 . . ? C31A N36A C35A 114.8(5) . . ? Cl2S C1S Cl1S 111.7(5) . . ? Cl2S C1S H1S1 109.3 . . ? Cl1S C1S H1S1 109.3 . . ? Cl2S C1S H1S2 109.3 . . ? Cl1S C1S H1S2 109.3 . . ? H1S1 C1S H1S2 107.9 . . ? Cl4S C2S Cl3S 92.0(15) . . ? Cl4S C2S H2S1 113.3 . . ? Cl3S C2S H2S1 113.3 . . ? Cl4S C2S H2S2 113.3 . . ? Cl3S C2S H2S2 113.3 . . ? H2S1 C2S H2S2 110.6 . . ? C3S Cl5S Cl6S 51.5(8) . . ? C3S Cl6S Cl5S 50.9(8) . . ? Cl5S C3S Cl6S 77.5(11) . . ? Cl5S C3S H3S1 115.6 . . ? Cl6S C3S H3S1 115.6 . . ? Cl5S C3S H3S2 115.6 . . ? Cl6S C3S H3S2 115.6 . . ? H3S1 C3S H3S2 112.6 . . ? 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 O1 C1 N1 C2 23.4(7) . . . . ? C13 C1 N1 C2 -150.7(5) . . . . ? O1 C1 N1 C11A -128.5(5) . . . . ? C13 C1 N1 C11A 57.5(6) . . . . ? C1 N1 C2 O2 -135.9(6) . . . . ? C11A N1 C2 O2 15.7(8) . . . . ? C1 N1 C2 C21 47.4(7) . . . . ? C11A N1 C2 C21 -161.0(5) . . . . ? O3 C3 N2 C4 -111.7(5) . . . . ? C23 C3 N2 C4 71.1(5) . . . . ? O3 C3 N2 C21A 51.9(6) . . . . ? C23 C3 N2 C21A -125.3(4) . . . . ? C21A N2 C4 O4 -155.9(4) . . . . ? C3 N2 C4 O4 5.7(6) . . . . ? C21A N2 C4 C31 26.9(6) . . . . ? C3 N2 C4 C31 -171.5(4) . . . . ? O5 C5 N3 C31A -13.4(8) . . . . ? C33 C5 N3 C31A 163.7(5) . . . . ? O5 C5 N3 C6 139.8(6) . . . . ? C33 C5 N3 C6 -43.1(7) . . . . ? C5 N3 C6 O6 -28.1(7) . . . . ? C31A N3 C6 O6 125.7(5) . . . . ? C5 N3 C6 C11 146.6(4) . . . . ? C31A N3 C6 C11 -59.6(6) . . . . ? O6 C6 C11 C16 -36.6(7) . . . . ? N3 C6 C11 C16 148.9(4) . . . . ? O6 C6 C11 C12 135.0(5) . . . . ? N3 C6 C11 C12 -39.6(6) . . . . ? C16 C11 C12 C13 3.1(7) . . . . ? C6 C11 C12 C13 -168.5(4) . . . . ? C11 C12 C13 C14 -4.0(7) . . . . ? C11 C12 C13 C1 168.3(4) . . . . ? O1 C1 C13 C14 21.9(7) . . . . ? N1 C1 C13 C14 -164.3(4) . . . . ? O1 C1 C13 C12 -150.5(5) . . . . ? N1 C1 C13 C12 23.4(7) . . . . ? C12 C13 C14 C15 1.0(8) . . . . ? C1 C13 C14 C15 -171.6(5) . . . . ? C13 C14 C15 C16 3.1(9) . . . . ? C14 C15 C16 C11 -4.1(8) . . . . ? C12 C11 C16 C15 1.0(8) . . . . ? C6 C11 C16 C15 172.7(5) . . . . ? C2 N1 C11A N12A -125.8(6) . . . . ? C1 N1 C11A N12A 26.9(7) . . . . ? C2 N1 C11A N16A 54.7(7) . . . . ? C1 N1 C11A N16A -152.6(5) . . . . ? N16A C11A N12A C13A -0.3(10) . . . . ? N1 C11A N12A C13A -179.7(5) . . . . ? C11A N12A C13A C14A -0.9(10) . . . . ? N12A C13A C14A C15A 0.5(10) . . . . ? N12A C13A C14A Br14 -178.3(5) . . . . ? C13A C14A C15A N16A 1.1(10) . . . . ? Br14 C14A C15A N16A 179.8(5) . . . . ? N12A C11A N16A C15A 1.7(9) . . . . ? N1 C11A N16A C15A -178.9(5) . . . . ? C14A C15A N16A C11A -2.0(9) . . . . ? O2 C2 C21 C22 -154.2(6) . . . . ? N1 C2 C21 C22 22.5(8) . . . . ? O2 C2 C21 C26 23.3(9) . . . . ? N1 C2 C21 C26 -160.0(5) . . . . ? C26 C21 C22 C23 3.6(7) . . . . ? C2 C21 C22 C23 -178.9(5) . . . . ? C21 C22 C23 C24 -0.9(7) . . . . ? C21 C22 C23 C3 175.2(4) . . . . ? O3 C3 C23 C24 30.1(7) . . . . ? N2 C3 C23 C24 -152.8(4) . . . . ? O3 C3 C23 C22 -146.1(5) . . . . ? N2 C3 C23 C22 31.0(6) . . . . ? C22 C23 C24 C25 -1.6(7) . . . . ? C3 C23 C24 C25 -177.8(4) . . . . ? C23 C24 C25 C26 1.4(8) . . . . ? C24 C25 C26 C21 1.3(8) . . . . ? C22 C21 C26 C25 -3.8(8) . . . . ? C2 C21 C26 C25 178.6(5) . . . . ? C4 N2 C21A N22A 29.4(6) . . . . ? C3 N2 C21A N22A -132.3(4) . . . . ? C4 N2 C21A N26A -152.5(4) . . . . ? C3 N2 C21A N26A 45.8(5) . . . . ? N26A C21A N22A C23A 2.6(7) . . . . ? N2 C21A N22A C23A -179.6(4) . . . . ? C21A N22A C23A C24A -0.7(7) . . . . ? N22A C23A C24A C25A -1.9(8) . . . . ? N22A C23A C24A Br24 178.8(4) . . . . ? C23A C24A C25A N26A 3.1(8) . . . . ? Br24 C24A C25A N26A -177.6(4) . . . . ? N22A C21A N26A C25A -1.5(7) . . . . ? N2 C21A N26A C25A -179.3(4) . . . . ? C24A C25A N26A C21A -1.5(7) . . . . ? O4 C4 C31 C32 -128.3(5) . . . . ? N2 C4 C31 C32 48.8(6) . . . . ? O4 C4 C31 C36 44.8(6) . . . . ? N2 C4 C31 C36 -138.0(4) . . . . ? C36 C31 C32 C33 -1.2(7) . . . . ? C4 C31 C32 C33 171.8(4) . . . . ? C31 C32 C33 C34 1.4(7) . . . . ? C31 C32 C33 C5 -174.8(5) . . . . ? O5 C5 C33 C34 -21.5(8) . . . . ? N3 C5 C33 C34 161.4(5) . . . . ? O5 C5 C33 C32 154.7(6) . . . . ? N3 C5 C33 C32 -22.4(8) . . . . ? C32 C33 C34 C35 -0.7(7) . . . . ? C5 C33 C34 C35 175.6(5) . . . . ? C33 C34 C35 C36 -0.1(8) . . . . ? C34 C35 C36 C31 0.2(7) . . . . ? C32 C31 C36 C35 0.4(7) . . . . ? C4 C31 C36 C35 -173.0(4) . . . . ? C5 N3 C31A N32A 126.7(5) . . . . ? C6 N3 C31A N32A -27.9(6) . . . . ? C5 N3 C31A N36A -54.2(7) . . . . ? C6 N3 C31A N36A 151.2(5) . . . . ? N36A C31A N32A C33A 1.6(9) . . . . ? N3 C31A N32A C33A -179.4(5) . . . . ? C31A N32A C33A C34A 2.1(9) . . . . ? N32A C33A C34A C35A -2.9(10) . . . . ? N32A C33A C34A Br34 176.9(5) . . . . ? C33A C34A C35A N36A 0.1(10) . . . . ? Br34 C34A C35A N36A -179.8(5) . . . . ? N32A C31A N36A C35A -4.2(8) . . . . ? N3 C31A N36A C35A 176.8(5) . . . . ? C34A C35A N36A C31A 3.1(9) . . . . ? _iucr_refine_instructions_details ; TITL 11-125 is 2,6-BrIO3:2CH2Cl2 in P-1 at 40kV30mA to 0.80\%A CELL 0.71073 12.2390 13.6149 13.6447 100.749 99.990 95.463 ZERR 2 0.0005 0.0005 0.0005 0.003 0.003 0.003 LATT 1 SFAC C H N O CL BR UNIT 76 44 18 12 8 6 MERG 3 FMAP 2 L.S. 8 3 LIST 4 ACTA 52 CONF DELU 0.020 CL3S CL4S C2S ISOR 0.020 CL3S CL4S C2S DELU 0.010 CL5S CL6S C3S ISOR 0.010 CL5S CL6S C3S BIND CL1S C1S BIND CL2S C1S BIND CL3S C2S BIND CL4S C2S BIND CL5S C3S BIND CL6S C3S BOND $H HTAB EQIV $1 -X,-Y,1-Z EQIV $2 1-X,-Y,2-Z EQIV $3 X,Y,Z-1 HTAB C1S O5 HTAB C1S N16A_$1 HTAB C12 N1 HTAB C22 N2 HTAB C25 O4_$2 RTAB XO BR14 O4_$3 RTAB CXO C14 BR14 O4_$3 RTAB XOC BR14 O4_$3 C4_$3 RTAB XX BR14 BR24 RTAB XX BR14 BR34 RTAB XX BR24 BR34 RTAB OO O1 O2 RTAB OO O3 O4 RTAB OO O5 O6 RTAB OO O1 O3 RTAB OO O2 O4 RTAB OO O1 O5 RTAB OO O2 O5 RTAB OO O1 O6 RTAB OO O2 O6 RTAB NN N1 N2 RTAB NN N1 N3 RTAB NN N2 N3 RTAB NN N12A N22A RTAB NN N12A N32A RTAB NN N22A N32A RTAB OCCO O1 C1 C6 O6 RTAB OCCO O2 C2 C3 O3 RTAB OCCO O4 C4 C5 O5 RTAB OCCO O1 C1 C2 O2 RTAB OCCO O3 C3 C4 O4 RTAB OCCO O5 C5 C6 O6 RTAB CCNC C13 C1 N1 C2 RTAB CCNC C23 C3 N2 C4 RTAB CCNC C33 C5 N3 C6 RTAB CNCC C1 N1 C2 C21 RTAB CNCC C3 N2 C4 C31 RTAB CNCC C5 N3 C6 C11 RTAB OCNC O1 C1 N1 C2 RTAB OCNC O3 C3 N2 C4 RTAB OCNC O5 C5 N3 C6 RTAB CNCO C1 N1 C2 O2 RTAB CNCO C3 N2 C4 O4 RTAB CNCO C5 N3 C6 O6 RTAB CNCN C1 N1 C11A N12A RTAB CNCN C3 N2 C21A N22A RTAB CNCN C5 N3 C31A N32A SIZE 0.15 0.38 0.49 TEMP 21 PLAN 10 MPLA 3 C1 C2 C11A N1 N2 N3 MPLA 3 C3 C4 C21A N2 N1 N3 MPLA 3 C5 C6 C31A N3 N1 N2 MPLA 6 C11 C12 C13 C14 C15 C16 C1 O1 C6 O6 BR14 BR24 BR34 MPLA 6 C21 C22 C23 C24 C25 C26 C2 O2 C3 O3 BR14 BR24 BR34 MPLA 6 C31 C32 C33 C34 C35 C36 C4 O4 C5 O5 BR14 BR24 BR34 MPLA 6 C11 C12 C13 C14 C15 C16 MPLA 6 C31 C32 C33 C34 C35 C36 MPLA 3 C1 C2 N1 O1 O2 C11 C11A C21 MPLA 6 C11A N12A C13A C14A C15A N16A BR14 BR24 BR34 MPLA 6 C11 C12 C13 C14 C15 C16 MPLA 6 C21 C22 C23 C24 C25 C26 MPLA 3 C3 C4 N2 O3 O4 C21 C21A C31 MPLA 6 C21A N22A C23A C24A C25A N26A BR14 BR24 BR34 MPLA 6 C21 C22 C23 C24 C25 C26 MPLA 6 C31 C32 C33 C34 C35 C36 MPLA 3 C5 C6 N3 O5 O6 C31 C31A C11 MPLA 6 C31A N32A C33A C34A C35A N36A BR14 BR24 BR34 MPLA 6 C31 C32 C33 C34 C35 C36 WGHT 0.077700 4.237500 FVAR 3.81087 MOLE 1 BR14 6 0.274799 0.128950 0.255708 11.00000 0.11911 0.06282 = 0.03180 0.00859 0.00444 0.00853 BR24 6 0.173779 0.669740 1.029406 11.00000 0.11025 0.03731 = 0.10943 0.01204 -0.01425 0.02234 BR34 6 0.021035 0.294650 0.223504 11.00000 0.18379 0.11909 = 0.04159 0.03440 0.03229 0.05111 O1 4 0.571002 0.342850 0.800724 11.00000 0.04178 0.07314 = 0.06059 0.00699 -0.00654 -0.00686 C1 1 0.480243 0.313886 0.747942 11.00000 0.04213 0.05360 = 0.03322 0.00768 0.00652 -0.00689 N1 3 0.450909 0.210766 0.698485 11.00000 0.04483 0.05424 = 0.02938 0.00446 0.00216 0.00167 O2 4 0.537639 0.068903 0.682281 11.00000 0.11703 0.11684 = 0.04979 -0.00140 0.01370 0.07536 C2 1 0.506963 0.135341 0.737472 11.00000 0.04577 0.07034 = 0.04348 0.00314 0.00766 0.01819 O3 4 0.431754 0.295093 1.158090 11.00000 0.04770 0.05575 = 0.03825 -0.00054 -0.00244 0.00707 C3 1 0.398870 0.251013 1.072339 11.00000 0.02998 0.03573 = 0.03720 0.00957 0.00012 -0.00008 N2 3 0.284703 0.256823 1.020723 11.00000 0.03178 0.03026 = 0.03487 0.00756 0.00192 0.00323 O4 4 0.239671 0.095668 1.029589 11.00000 0.04559 0.03693 = 0.04370 0.01813 0.00160 0.00420 C4 1 0.210500 0.169101 0.998856 11.00000 0.03723 0.03214 = 0.02487 0.00705 0.00767 0.00315 O5 4 -0.118921 0.157581 0.610338 11.00000 0.06074 0.11442 = 0.04352 0.02635 -0.01481 -0.03941 C5 1 -0.041876 0.201324 0.675421 11.00000 0.04153 0.06001 = 0.03619 0.01638 -0.00479 -0.00598 N3 3 0.036357 0.274184 0.655069 11.00000 0.04057 0.04891 = 0.03088 0.01535 -0.00294 -0.00518 O6 4 0.025793 0.402299 0.787509 11.00000 0.05789 0.05565 = 0.06208 0.01232 0.01961 0.01142 C6 1 0.079403 0.366059 0.728103 11.00000 0.04598 0.04429 = 0.03699 0.01637 0.00051 0.00598 C11 1 0.196784 0.406194 0.730109 11.00000 0.04473 0.04081 = 0.03043 0.01084 0.00135 -0.00145 C12 1 0.277141 0.341479 0.719285 11.00000 0.04218 0.03729 = 0.03039 0.00788 0.00157 -0.01087 AFIX 43 H12 2 0.255481 0.272276 0.698634 11.00000 -1.20000 AFIX 0 C13 1 0.389994 0.380196 0.739338 11.00000 0.04883 0.04617 = 0.02953 0.00630 -0.00115 -0.00504 C14 1 0.420314 0.484030 0.763848 11.00000 0.05125 0.05200 = 0.04916 0.00601 0.00204 -0.01315 AFIX 43 H14 2 0.495467 0.510561 0.776359 11.00000 -1.20000 AFIX 0 C15 1 0.339800 0.548172 0.769789 11.00000 0.06683 0.03861 = 0.06395 0.00931 -0.00419 -0.00965 AFIX 43 H15 2 0.360569 0.617579 0.782990 11.00000 -1.20000 AFIX 0 C16 1 0.228856 0.509640 0.756220 11.00000 0.06053 0.04208 = 0.04822 0.00854 -0.00123 0.00192 AFIX 43 H16 2 0.175345 0.553005 0.764567 11.00000 -1.20000 AFIX 0 C11A 1 0.407378 0.190772 0.591886 11.00000 0.04781 0.05344 = 0.03398 0.00564 0.00615 0.00109 N12A 3 0.439727 0.259767 0.543778 11.00000 0.08350 0.06380 = 0.03832 0.00587 0.01194 -0.02178 C13A 1 0.398152 0.240803 0.443954 11.00000 0.09440 0.06295 = 0.04138 0.01427 0.01509 -0.01286 AFIX 43 H13A 2 0.417296 0.287461 0.405903 11.00000 -1.20000 AFIX 0 C14A 1 0.328037 0.154323 0.396335 11.00000 0.07336 0.04996 = 0.03157 0.00580 0.00949 0.00452 C15A 1 0.300816 0.087826 0.453885 11.00000 0.08881 0.04496 = 0.03643 0.00464 -0.00258 -0.00911 AFIX 43 H15A 2 0.254282 0.028147 0.422609 11.00000 -1.20000 AFIX 0 N16A 3 0.339045 0.105875 0.553956 11.00000 0.07701 0.04803 = 0.03792 0.01008 0.00077 -0.00782 C21 1 0.519246 0.140555 0.848510 11.00000 0.02841 0.04910 = 0.04468 0.00415 0.00367 0.00768 C22 1 0.450006 0.188991 0.905657 11.00000 0.03081 0.04392 = 0.03836 0.00830 -0.00142 0.00928 AFIX 43 H22 2 0.392191 0.219046 0.874462 11.00000 -1.20000 AFIX 0 C23 1 0.466577 0.192904 1.009773 11.00000 0.02555 0.03455 = 0.03988 0.00897 0.00199 0.00031 C24 1 0.551600 0.147039 1.056236 11.00000 0.03569 0.05415 = 0.04232 0.01837 0.00176 0.00469 AFIX 43 H24 2 0.563890 0.151119 1.126162 11.00000 -1.20000 AFIX 0 C25 1 0.617622 0.095582 0.998812 11.00000 0.03629 0.05849 = 0.05855 0.01980 0.00094 0.01759 AFIX 43 H25 2 0.673698 0.063439 1.029613 11.00000 -1.20000 AFIX 0 C26 1 0.600995 0.091421 0.895464 11.00000 0.03359 0.05154 = 0.06004 0.00515 0.00799 0.01440 AFIX 43 H26 2 0.645107 0.055250 0.856797 11.00000 -1.20000 AFIX 0 C21A 1 0.256247 0.355471 1.024249 11.00000 0.03715 0.03306 = 0.02850 0.00385 0.00102 0.00435 N22A 3 0.159966 0.373863 1.050126 11.00000 0.03962 0.04012 = 0.04657 0.00643 0.00444 0.00691 C23A 1 0.137183 0.468030 1.051596 11.00000 0.04684 0.04506 = 0.05525 0.00358 -0.00125 0.01741 AFIX 43 H23A 2 0.070155 0.485491 1.068485 11.00000 -1.20000 AFIX 0 C24A 1 0.208555 0.538611 1.029297 11.00000 0.06485 0.03127 = 0.04425 0.00305 -0.00851 0.01281 C25A 1 0.308658 0.512454 1.007456 11.00000 0.07109 0.03178 = 0.04574 0.00992 0.00379 -0.00824 AFIX 43 H25A 2 0.360202 0.561217 0.995207 11.00000 -1.20000 AFIX 0 N26A 3 0.333628 0.418695 1.003414 11.00000 0.05221 0.03373 = 0.04271 0.00736 0.01083 0.00030 C31 1 0.098404 0.164560 0.934279 11.00000 0.03426 0.02467 = 0.03268 0.00605 0.00458 0.00291 C32 1 0.083519 0.195502 0.842577 11.00000 0.03306 0.03544 = 0.03122 0.00778 0.00365 -0.00760 AFIX 43 H32 2 0.143915 0.228307 0.823191 11.00000 -1.20000 AFIX 0 C33 1 -0.021411 0.177800 0.779124 11.00000 0.03385 0.03531 = 0.03353 0.00873 -0.00072 -0.00477 C34 1 -0.111259 0.130764 0.809863 11.00000 0.03257 0.04141 = 0.04567 0.01078 -0.00071 -0.00406 AFIX 43 H34 2 -0.181874 0.119346 0.768236 11.00000 -1.20000 AFIX 0 C35 1 -0.096485 0.100963 0.901459 11.00000 0.03278 0.04235 = 0.05267 0.01936 0.00622 -0.00633 AFIX 43 H35 2 -0.157220 0.069513 0.921548 11.00000 -1.20000 AFIX 0 C36 1 0.007782 0.117325 0.963914 11.00000 0.04019 0.03238 = 0.04080 0.01432 0.01033 0.00303 AFIX 43 H36 2 0.017313 0.096731 1.025770 11.00000 -1.20000 AFIX 0 C31A 1 0.036171 0.278940 0.551637 11.00000 0.03874 0.05518 = 0.03558 0.01467 0.00020 -0.00637 N32A 3 0.028177 0.368296 0.529043 11.00000 0.07285 0.05385 = 0.03823 0.01777 0.00719 0.00634 C33A 1 0.026959 0.372481 0.432601 11.00000 0.09004 0.06352 = 0.04095 0.02667 0.00724 0.01172 AFIX 43 H33A 2 0.023951 0.434221 0.413080 11.00000 -1.20000 AFIX 0 C34A 1 0.030012 0.288315 0.361020 11.00000 0.07206 0.08173 = 0.03687 0.02505 0.01236 0.01161 C35A 1 0.039533 0.199567 0.392741 11.00000 0.07991 0.06307 = 0.04163 0.01037 0.01500 0.01061 AFIX 43 H35A 2 0.041854 0.141595 0.345152 11.00000 -1.20000 AFIX 0 N36A 3 0.045604 0.193582 0.490013 11.00000 0.07090 0.05502 = 0.04264 0.01625 0.01230 0.00668 MOLE 2 CL1S 5 -0.225014 0.029926 0.257416 11.00000 0.20280 0.17515 = 0.11530 -0.00599 0.01695 -0.02293 CL2S 5 -0.286524 0.213988 0.351550 11.00000 0.26945 0.12980 = 0.19269 0.06758 -0.01340 0.01769 C1S 1 -0.264229 0.095271 0.363335 11.00000 0.18358 0.09145 = 0.08218 0.02981 -0.01225 -0.03693 AFIX 23 H1S1 2 -0.332193 0.059470 0.373902 11.00000 -1.20000 H1S2 2 -0.206109 0.098588 0.422506 11.00000 -1.20000 AFIX 0 MOLE 3 PART -1 CL3S 5 0.673200 0.477800 0.489593 10.80000 0.29061 0.23691 = 0.11966 0.08620 0.02424 -0.02310 CL4S 5 0.737859 0.503711 0.683658 10.80000 0.41447 0.46494 = 0.22735 0.04625 0.10428 -0.09875 C2S 1 0.713566 0.399984 0.583723 10.80000 0.27642 0.25450 = 0.20855 0.06183 0.00890 -0.01651 AFIX 23 H2S1 2 0.653134 0.349998 0.587209 10.80000 -1.20000 H2S2 2 0.780250 0.368850 0.574958 10.80000 -1.20000 AFIX 0 PART -2 CL5S 5 0.706048 0.543942 0.695589 10.20000 0.10726 0.07454 = 0.04838 -0.00958 0.01561 -0.02436 CL6S 5 0.785026 0.409725 0.661088 10.20000 0.08844 0.13559 = 0.12417 0.04923 0.00608 0.03697 C3S 1 0.663813 0.442242 0.595901 10.20000 0.04385 0.04688 = 0.03001 0.00996 0.01065 -0.02001 AFIX 23 H3S1 2 0.667441 0.455549 0.529054 10.20000 -1.20000 H3S2 2 0.594953 0.401040 0.596754 10.20000 -1.20000 DFIX 1.70 0.03 CL5S C3S CL6S C3S HKLF 4 REM 11-125 is 2,6-BrIO3:2CH2Cl2 in P-1 at 40kV30mA to 0.80\%A REM R1 = 0.0667 for 5817 Fo > 4sig(Fo) and 0.1119 for all 9391 data REM 568 parameters refined using 47 restraints END WGHT 0.0777 4.2372 REM Highest difference peak 1.449, deepest hole -1.295, 1-sigma level 0.083 Q1 1 0.2411 0.6807 0.9931 11.00000 0.05 1.45 Q2 1 -0.3855 0.1578 0.3449 11.00000 0.05 0.77 Q3 1 -0.0007 0.2231 0.2205 11.00000 0.05 0.70 Q4 1 0.6747 0.5359 0.5523 11.00000 0.05 0.57 Q5 1 0.7492 0.3321 0.6160 11.00000 0.05 0.57 Q6 1 0.0913 0.3286 0.2632 11.00000 0.05 0.55 Q7 1 0.7406 0.4349 0.4966 11.00000 0.05 0.53 Q8 1 0.7570 0.4089 0.5134 11.00000 0.05 0.51 Q9 1 0.1399 0.6593 1.0173 11.00000 0.05 0.49 Q10 1 0.0091 0.3043 0.2034 11.00000 0.05 0.44 ; loop_ _geom_hbond_atom_site_label_D _geom_hbond_atom_site_label_H _geom_hbond_atom_site_label_A _geom_hbond_distance_DH _geom_hbond_distance_HA _geom_hbond_distance_DA _geom_hbond_angle_DHA _geom_hbond_site_symmetry_A _geom_hbond_publ_flag # # Hydrogen bonding scheme # ======== ======= ====== # # D H A D-H H...A D...A D-H...A symm publ # - - - --- ----- ----- ------- ---- ---- C1S H1S2 O5 0.97 2.54 3.436(10) 153 . yes C1S H1S1 N16A 0.97 2.62 3.263(9) 124 2_556 yes C12 H12 N1 0.93 2.61 2.918(7) 100 . yes C22 H22 N2 0.93 2.58 2.886(6) 100 . yes C25 H25 O4 0.93 2.56 3.272(6) 134 2_657 yes _database_code_depnum_ccdc_archive 'CCDC 930692' ####################################################################### # # Cambridge Crystallographic Data Centre # CCDC # ####################################################################### # # This CIF contains data from an original supplementary publication # deposited with the CCDC, and may include chemical, crystal, # experimental, refinement, atomic coordinates, # anisotropic displacement parameters and molecular geometry data, # as required by the journal to which it was submitted. # # This CIF is provided on the understanding that it is used for bona # fide research purposes only. It may contain copyright material # of the CCDC or of third parties, and may not be copied or further # disseminated in any form, whether machine-readable or not, # except for the purpose of generating routine backup copies # on your local computer system. # # For further information on the CCDC, data deposition and # data retrieval see: # www.ccdc.cam.ac.uk # # Bona fide researchers may freely download Mercury and enCIFer # from this site to visualise CIF-encoded structures and # to carry out CIF format checking respectively. # data_(26BrIO)4_2CHCl3_[11-128] #TrackingRef 'Bromo_JFG_v09.cif' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety '2(C48 H24 Br4 N12 O8), 3.8(C H Cl3), H2 O' _chemical_formula_sum 'C99.80 H53.80 Br8 Cl11.40 N24 O17' _chemical_formula_weight 2904.40 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' N N 0.0061 0.0033 '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' Cl Cl 0.1484 0.1585 '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 Monoclinic _symmetry_space_group_name_H-M 'P 21/n' _symmetry_space_group_name_Hall '-P 2yn' loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x+1/2, y+1/2, -z+1/2' '-x, -y, -z' 'x-1/2, -y-1/2, z-1/2' _cell_length_a 10.5779(3) _cell_length_b 13.2805(3) _cell_length_c 40.7855(13) _cell_angle_alpha 90.00 _cell_angle_beta 95.936(2) _cell_angle_gamma 90.00 _cell_volume 5698.8(3) _cell_formula_units_Z 2 _cell_measurement_temperature 294(2) _cell_measurement_reflns_used 5712 _cell_measurement_theta_min 2.15 _cell_measurement_theta_max 27.13 _exptl_crystal_description Block _exptl_crystal_colour Colourless _exptl_crystal_size_max 0.39 _exptl_crystal_size_mid 0.35 _exptl_crystal_size_min 0.22 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.693 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 2860.8 _exptl_absorpt_coefficient_mu 3.156 _exptl_absorpt_correction_type Analytical _exptl_absorpt_correction_T_min 0.3724 _exptl_absorpt_correction_T_max 0.5435 _exptl_absorpt_process_details '(ABSFAC, Clark and Reid, 1998)' _exptl_special_details ; ? ; _diffrn_ambient_temperature 294(1) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'Enhance (Mo) X-ray Source' _diffrn_radiation_monochromator graphite _diffrn_measurement_device 'Xcalibur, Sapphire3, Gemini Ultra' _diffrn_measurement_method '\w scans' _diffrn_standards_number 5712 _diffrn_standards_interval_time 60 _diffrn_standards_decay_% 1 _diffrn_reflns_number 41540 _diffrn_reflns_av_R_equivalents 0.0456 _diffrn_reflns_av_sigmaI/netI 0.0480 _diffrn_reflns_limit_h_min -13 _diffrn_reflns_limit_h_max 13 _diffrn_reflns_limit_k_min -16 _diffrn_reflns_limit_k_max 16 _diffrn_reflns_limit_l_min -47 _diffrn_reflns_limit_l_max 52 _diffrn_reflns_theta_min 2.15 _diffrn_reflns_theta_max 27.14 _diffrn_measured_fraction_theta_max 0.967 _diffrn_reflns_theta_full 26.00 _diffrn_measured_fraction_theta_full 0.999 _reflns_number_total 12192 _reflns_number_gt 7949 _reflns_threshold_expression I>2\s(I) _computing_data_collection ; CrysAlisPro, Agilent Technologies, Version 1.171.34.49 (release 20-01-2011 CrysAlis171 .NET) (compiled Jan 20 2011,15:58:25) ; _computing_cell_refinement ; CrysAlisPro, Agilent Technologies, Version 1.171.34.49 (release 20-01-2011 CrysAlis171 .NET) (compiled Jan 20 2011,15:58:25) ; _computing_data_reduction ; CrysAlisPro, Agilent Technologies, Version 1.171.34.49 (release 20-01-2011 CrysAlis171 .NET) (compiled Jan 20 2011,15:58:25) ; _computing_structure_solution 'SHELXS97 (Sheldrick, 2008)' _computing_structure_refinement 'SHELXL97 (Sheldrick, 2008) and SORTX (McArdle, 1995)' _computing_molecular_graphics 'PLATON (Spek, 2009)' _computing_publication_material SHELXL97 _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 'w=1/[\s^2^(Fo^2^)+(0.0845P)^2^+14.96P] 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 constr _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 12192 _refine_ls_number_parameters 754 _refine_ls_number_restraints 39 _refine_ls_R_factor_all 0.1177 _refine_ls_R_factor_gt 0.0763 _refine_ls_wR_factor_ref 0.2053 _refine_ls_wR_factor_gt 0.1820 _refine_ls_goodness_of_fit_ref 1.032 _refine_ls_restrained_S_all 1.040 _refine_ls_shift/su_max 0.001 _refine_ls_shift/su_mean 0.000 _refine_diff_density_max 1.159 _refine_diff_density_min -1.224 _refine_diff_density_rms 0.087 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 Br14 Br 0.30604(11) 0.51523(7) 0.00600(3) 0.1063(4) Uani 1 1 d . . . Br24 Br -0.03196(9) 1.23862(5) 0.076724(18) 0.0758(3) Uani 1 1 d . . . Br34 Br 0.58592(8) 0.82649(7) 0.267698(18) 0.0806(3) Uani 1 1 d . . . Br44 Br -0.47756(9) 0.50005(8) 0.17745(3) 0.1168(4) Uani 1 1 d . . . O1 O 0.2267(6) 0.3967(4) 0.15359(12) 0.0902(18) Uani 1 1 d . . . C1 C 0.1540(6) 0.4633(4) 0.15776(14) 0.0487(14) Uani 1 1 d . . . N1 N 0.0641(4) 0.4944(3) 0.12981(10) 0.0404(10) Uani 1 1 d . . . O2 O -0.0915(4) 0.4245(4) 0.15577(11) 0.0677(13) Uani 1 1 d . . . C2 C -0.0634(5) 0.4742(4) 0.13287(14) 0.0440(12) Uani 1 1 d . . . O3 O -0.3231(4) 0.8181(3) 0.05777(13) 0.0642(12) Uani 1 1 d . . . C3 C -0.2338(5) 0.7633(4) 0.06262(14) 0.0418(12) Uani 1 1 d . . . N2 N -0.1095(4) 0.8003(3) 0.05884(10) 0.0367(9) Uani 1 1 d . . . O4 O -0.0682(4) 0.6753(3) 0.02351(10) 0.0561(10) Uani 1 1 d . . . C4 C -0.0288(5) 0.7447(4) 0.04040(12) 0.0367(11) Uani 1 1 d . . . O5 O 0.4733(4) 0.7924(4) 0.11698(11) 0.0757(15) Uani 1 1 d . . . C5 C 0.3721(5) 0.8318(5) 0.11022(14) 0.0483(13) Uani 1 1 d . . . N3 N 0.3139(4) 0.8850(4) 0.13481(11) 0.0432(10) Uani 1 1 d . . . O6 O 0.2528(5) 1.0201(3) 0.10206(11) 0.0627(11) Uani 1 1 d . . . C6 C 0.2456(5) 0.9745(4) 0.12746(14) 0.0446(13) Uani 1 1 d . . . O7 O -0.1982(4) 0.9242(3) 0.20720(15) 0.0781(16) Uani 1 1 d . . . C7 C -0.0967(5) 0.8990(4) 0.20016(14) 0.0449(13) Uani 1 1 d . . . N4 N -0.0596(4) 0.7948(3) 0.20257(11) 0.0407(10) Uani 1 1 d . . . O8 O 0.1115(4) 0.8347(3) 0.23781(11) 0.0635(12) Uani 1 1 d . . . C8 C 0.0556(5) 0.7706(4) 0.22142(12) 0.0403(12) Uani 1 1 d . . . C11 C 0.1052(5) 0.6679(4) 0.21899(12) 0.0367(11) Uani 1 1 d . . . C12 C 0.0946(5) 0.6135(4) 0.18997(12) 0.0355(11) Uani 1 1 d . . . H12 H 0.0479 0.6398 0.1713 0.043 Uiso 1 1 calc R . . C13 C 0.1527(5) 0.5204(4) 0.18830(13) 0.0402(12) Uani 1 1 d . . . C14 C 0.2200(5) 0.4804(4) 0.21659(15) 0.0487(14) Uani 1 1 d . . . H14 H 0.2581 0.4174 0.2159 0.058 Uiso 1 1 calc R . . C15 C 0.2301(6) 0.5345(5) 0.24557(14) 0.0542(15) Uani 1 1 d . . . H15 H 0.2748 0.5077 0.2644 0.065 Uiso 1 1 calc R . . C16 C 0.1745(5) 0.6274(5) 0.24677(14) 0.0498(14) Uani 1 1 d . . . H16 H 0.1831 0.6639 0.2663 0.060 Uiso 1 1 calc R . . C11A C 0.1163(5) 0.5021(4) 0.09934(13) 0.0384(11) Uani 1 1 d . . . N12A N 0.2220(5) 0.5565(4) 0.10052(13) 0.0526(12) Uani 1 1 d . . . C14A C 0.2245(7) 0.5119(4) 0.04486(17) 0.0582(16) Uani 1 1 d . . . C15A C 0.1125(7) 0.4620(5) 0.04580(16) 0.0588(16) Uani 1 1 d . . . H15A H 0.0739 0.4322 0.0267 0.071 Uiso 1 1 calc R . . C13A C 0.2766(6) 0.5588(5) 0.07234(19) 0.0638(18) Uani 1 1 d . . . H13A H 0.3526 0.5937 0.0717 0.077 Uiso 1 1 calc R . . N16A N 0.0568(5) 0.4549(3) 0.07377(11) 0.0472(11) Uani 1 1 d . . . C21 C -0.1606(5) 0.5202(4) 0.10851(13) 0.0393(11) Uani 1 1 d . . . C22 C -0.1447(5) 0.6145(4) 0.09494(12) 0.0360(11) Uani 1 1 d . . . H22 H -0.0680 0.6484 0.0995 0.043 Uiso 1 1 calc R . . C23 C -0.2425(5) 0.6581(4) 0.07473(12) 0.0377(11) Uani 1 1 d . . . C24 C -0.3555(5) 0.6068(5) 0.06714(15) 0.0494(14) Uani 1 1 d . . . H24 H -0.4214 0.6361 0.0536 0.059 Uiso 1 1 calc R . . C25 C -0.3695(6) 0.5122(5) 0.07978(17) 0.0587(16) Uani 1 1 d . . . H25 H -0.4445 0.4768 0.0742 0.070 Uiso 1 1 calc R . . C26 C -0.2740(6) 0.4690(5) 0.10057(16) 0.0528(15) Uani 1 1 d . . . H26 H -0.2855 0.4054 0.1093 0.063 Uiso 1 1 calc R . . C21A C -0.0912(4) 0.9062(4) 0.06292(12) 0.0342(10) Uani 1 1 d . . . N22A N -0.1171(5) 0.9429(4) 0.09154(12) 0.0474(11) Uani 1 1 d . . . C23A C -0.1019(6) 1.0417(5) 0.09481(14) 0.0518(14) Uani 1 1 d . . . H23A H -0.1216 1.0727 0.1141 0.062 Uiso 1 1 calc R . . C24A C -0.0582(6) 1.0992(4) 0.07053(15) 0.0497(14) Uani 1 1 d . . . C25A C -0.0319(6) 1.0535(4) 0.04252(14) 0.0513(14) Uani 1 1 d . . . H25A H 0.0002 1.0917 0.0261 0.062 Uiso 1 1 calc R . . N26A N -0.0510(5) 0.9543(3) 0.03759(11) 0.0443(10) Uani 1 1 d . . . C31 C 0.1075(5) 0.7744(4) 0.04410(12) 0.0356(11) Uani 1 1 d . . . C32 C 0.1682(5) 0.8022(4) 0.07446(13) 0.0370(11) Uani 1 1 d . . . H32 H 0.1222 0.8090 0.0926 0.044 Uiso 1 1 calc R . . C33 C 0.2984(5) 0.8200(4) 0.07760(13) 0.0391(11) Uani 1 1 d . . . C34 C 0.3644(5) 0.8148(5) 0.05002(15) 0.0509(14) Uani 1 1 d . . . H34 H 0.4511 0.8285 0.0520 0.061 Uiso 1 1 calc R . . C35 C 0.3033(6) 0.7894(5) 0.01985(15) 0.0538(15) Uani 1 1 d . . . H35 H 0.3480 0.7879 0.0014 0.065 Uiso 1 1 calc R . . C36 C 0.1753(5) 0.7662(4) 0.01687(14) 0.0456(13) Uani 1 1 d . . . H36 H 0.1348 0.7451 -0.0033 0.055 Uiso 1 1 calc R . . C31A C 0.3730(5) 0.8713(4) 0.16790(13) 0.0409(12) Uani 1 1 d . . . N32A N 0.3600(5) 0.7822(4) 0.18073(13) 0.0548(12) Uani 1 1 d . . . C33A C 0.4230(6) 0.7690(5) 0.21065(16) 0.0563(15) Uani 1 1 d . . . H33A H 0.4177 0.7071 0.2211 0.068 Uiso 1 1 calc R . . C34A C 0.4951(5) 0.8437(5) 0.22636(13) 0.0474(13) Uani 1 1 d . . . C35A C 0.4967(6) 0.9341(5) 0.21046(15) 0.0546(15) Uani 1 1 d . . . H35A H 0.5430 0.9868 0.2208 0.066 Uiso 1 1 calc R . . N36A N 0.4350(5) 0.9499(4) 0.18098(12) 0.0523(12) Uani 1 1 d . . . C41 C 0.1582(5) 1.0071(4) 0.15163(13) 0.0393(11) Uani 1 1 d . . . C42 C 0.0861(5) 0.9367(4) 0.16686(12) 0.0362(11) Uani 1 1 d . . . H42 H 0.0997 0.8683 0.1640 0.043 Uiso 1 1 calc R . . C43 C -0.0061(5) 0.9690(4) 0.18634(13) 0.0389(11) Uani 1 1 d . . . C44 C -0.0219(6) 1.0722(4) 0.19125(15) 0.0504(14) Uani 1 1 d . . . H44 H -0.0825 1.0945 0.2045 0.061 Uiso 1 1 calc R . . C45 C 0.0513(6) 1.1413(4) 0.17661(16) 0.0558(15) Uani 1 1 d . . . H45 H 0.0412 1.2097 0.1803 0.067 Uiso 1 1 calc R . . C46 C 0.1390(6) 1.1090(4) 0.15657(15) 0.0493(14) Uani 1 1 d . . . H46 H 0.1863 1.1560 0.1461 0.059 Uiso 1 1 calc R . . C41A C -0.1598(5) 0.7231(4) 0.19720(14) 0.0405(12) Uani 1 1 d . . . N42A N -0.2299(5) 0.7321(4) 0.16876(13) 0.0544(12) Uani 1 1 d . . . C43A C -0.3248(6) 0.6644(5) 0.16356(18) 0.0625(17) Uani 1 1 d . . . H43A H -0.3786 0.6674 0.1440 0.075 Uiso 1 1 calc R . . C44A C -0.3438(6) 0.5927(5) 0.18579(19) 0.0600(17) Uani 1 1 d . . . C45A C -0.2646(6) 0.5903(5) 0.2146(2) 0.0666(18) Uani 1 1 d . . . H45A H -0.2768 0.5412 0.2302 0.080 Uiso 1 1 calc R . . N46A N -0.1703(5) 0.6567(4) 0.22087(13) 0.0535(12) Uani 1 1 d . . . Cl1S Cl 0.6066(3) 0.1859(2) 0.20405(8) 0.1179(10) Uani 0.90 1 d P . . Cl2S Cl 0.4487(3) 0.2411(3) 0.14488(12) 0.1416(14) Uani 0.90 1 d P . . Cl3S Cl 0.7176(3) 0.2220(3) 0.14704(10) 0.1358(14) Uani 0.90 1 d P . . C1S C 0.5820(10) 0.1733(7) 0.1615(2) 0.086(3) Uani 0.90 1 d P . . H1S H 0.5726 0.1020 0.1555 0.103 Uiso 0.90 1 calc PR . . Cl1T Cl 0.4224(10) 1.2651(4) 0.0424(2) 0.223(4) Uani 0.70 1 d P A -1 Cl2T Cl 0.5428(6) 1.0747(6) 0.0582(2) 0.190(3) Uani 0.70 1 d P A -1 Cl3T Cl 0.3040(8) 1.0908(6) 0.02024(14) 0.195(3) Uani 0.70 1 d P A -1 C1T C 0.4092(10) 1.1439(7) 0.0534(2) 0.107(5) Uani 0.70 1 d P A -1 H1T H 0.3677 1.1407 0.0738 0.129 Uiso 0.70 1 calc PR A -1 Cl4T Cl 0.5477(10) 1.2372(7) 0.0609(2) 0.206(8) Uani 0.30 1 d PRDU A -2 Cl5T Cl 0.4429(10) 1.0734(7) 0.0245(2) 0.270(10) Uani 0.30 1 d PRDU A -2 Cl6T Cl 0.2886(10) 1.2140(7) 0.0320(2) 0.324(12) Uani 0.30 1 d PRDU A -2 C2T C 0.4080(10) 1.1436(7) 0.0534(2) 0.23(2) Uani 0.30 1 d PRDU A -2 H2T H 0.3843 1.1088 0.0731 0.272 Uiso 0.30 1 calc PR A -2 O1W O -0.355(2) 0.997(3) 0.1335(6) 0.259(13) Uani 0.50 1 d PU B 1 H1W H -0.2851 0.9692 0.1225 0.388 Uiso 0.50 1 d P C 1 H2W H -0.3082 0.9648 0.1525 0.388 Uiso 0.50 1 d P D 1 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 Br14 0.1567(9) 0.0748(5) 0.1028(7) -0.0200(5) 0.0878(7) -0.0150(6) Br24 0.1223(7) 0.0391(3) 0.0648(4) -0.0062(3) 0.0046(4) -0.0065(4) Br34 0.0882(5) 0.1006(6) 0.0491(4) 0.0244(4) -0.0113(3) -0.0106(4) Br44 0.0701(5) 0.0948(7) 0.1882(12) -0.0351(7) 0.0259(6) -0.0444(5) O1 0.115(4) 0.087(4) 0.064(3) -0.012(3) -0.012(3) 0.065(3) C1 0.056(3) 0.044(3) 0.044(3) 0.006(2) 0.000(3) 0.017(3) N1 0.044(2) 0.041(2) 0.035(2) 0.0008(18) -0.0006(18) 0.005(2) O2 0.068(3) 0.080(3) 0.054(3) 0.030(2) 0.000(2) -0.019(2) C2 0.049(3) 0.041(3) 0.041(3) 0.000(2) 0.001(2) -0.004(2) O3 0.034(2) 0.054(3) 0.104(4) 0.021(2) 0.008(2) 0.0083(19) C3 0.032(3) 0.045(3) 0.049(3) 0.004(2) 0.006(2) 0.002(2) N2 0.030(2) 0.037(2) 0.044(2) 0.0045(18) 0.0033(17) -0.0001(17) O4 0.053(2) 0.061(3) 0.055(2) -0.020(2) 0.0109(19) -0.013(2) C4 0.040(3) 0.038(3) 0.032(3) 0.003(2) 0.004(2) -0.001(2) O5 0.044(2) 0.121(4) 0.061(3) -0.006(3) -0.001(2) 0.034(3) C5 0.031(3) 0.063(4) 0.051(3) -0.005(3) 0.006(2) 0.003(3) N3 0.034(2) 0.053(3) 0.042(2) -0.001(2) -0.0005(18) 0.004(2) O6 0.081(3) 0.054(3) 0.056(3) 0.011(2) 0.020(2) 0.002(2) C6 0.039(3) 0.042(3) 0.052(3) 0.005(3) 0.002(2) -0.003(2) O7 0.057(3) 0.049(3) 0.136(5) -0.001(3) 0.049(3) 0.006(2) C7 0.041(3) 0.037(3) 0.057(3) -0.003(2) 0.011(3) -0.001(2) N4 0.039(2) 0.035(2) 0.048(3) -0.0018(19) 0.0048(19) -0.0034(19) O8 0.078(3) 0.047(2) 0.059(3) -0.009(2) -0.021(2) -0.010(2) C8 0.044(3) 0.043(3) 0.033(3) -0.003(2) 0.000(2) -0.007(2) C11 0.033(3) 0.040(3) 0.037(3) 0.003(2) 0.000(2) -0.009(2) C12 0.033(2) 0.039(3) 0.034(3) 0.006(2) -0.001(2) 0.000(2) C13 0.038(3) 0.038(3) 0.045(3) 0.007(2) 0.004(2) 0.005(2) C14 0.043(3) 0.046(3) 0.055(4) 0.017(3) -0.005(3) 0.007(2) C15 0.058(4) 0.059(4) 0.041(3) 0.012(3) -0.016(3) 0.006(3) C16 0.051(3) 0.056(3) 0.040(3) -0.001(3) -0.007(2) -0.005(3) C11A 0.039(3) 0.031(2) 0.045(3) -0.002(2) 0.003(2) 0.008(2) N12A 0.046(3) 0.052(3) 0.060(3) -0.014(2) 0.006(2) -0.004(2) C14A 0.075(4) 0.037(3) 0.068(4) -0.009(3) 0.034(3) 0.002(3) C15A 0.078(4) 0.051(3) 0.050(4) -0.010(3) 0.018(3) -0.005(3) C13A 0.056(4) 0.051(4) 0.091(5) -0.016(3) 0.036(4) -0.008(3) N16A 0.055(3) 0.043(3) 0.044(3) -0.008(2) 0.004(2) -0.008(2) C21 0.040(3) 0.039(3) 0.039(3) 0.001(2) 0.007(2) -0.008(2) C22 0.030(2) 0.039(3) 0.040(3) -0.001(2) 0.005(2) -0.003(2) C23 0.032(3) 0.044(3) 0.038(3) -0.002(2) 0.011(2) -0.002(2) C24 0.031(3) 0.056(4) 0.060(4) 0.001(3) 0.000(2) -0.005(2) C25 0.042(3) 0.056(4) 0.078(4) -0.001(3) 0.003(3) -0.019(3) C26 0.050(3) 0.044(3) 0.065(4) 0.008(3) 0.008(3) -0.009(3) C21A 0.026(2) 0.036(3) 0.039(3) 0.002(2) 0.002(2) 0.002(2) N22A 0.051(3) 0.044(3) 0.048(3) 0.000(2) 0.012(2) 0.002(2) C23A 0.068(4) 0.049(3) 0.040(3) -0.004(3) 0.012(3) 0.009(3) C24A 0.059(4) 0.036(3) 0.053(3) 0.000(2) 0.000(3) 0.002(3) C25A 0.072(4) 0.036(3) 0.047(3) 0.006(2) 0.010(3) 0.001(3) N26A 0.058(3) 0.038(2) 0.037(2) 0.0047(19) 0.009(2) 0.004(2) C31 0.033(2) 0.038(3) 0.037(3) 0.003(2) 0.006(2) 0.006(2) C32 0.032(3) 0.041(3) 0.040(3) 0.002(2) 0.009(2) 0.006(2) C33 0.031(3) 0.045(3) 0.041(3) -0.001(2) 0.004(2) 0.007(2) C34 0.035(3) 0.065(4) 0.055(4) 0.000(3) 0.015(3) 0.003(3) C35 0.049(3) 0.070(4) 0.045(3) 0.001(3) 0.020(3) 0.002(3) C36 0.049(3) 0.051(3) 0.038(3) -0.002(2) 0.010(2) 0.005(3) C31A 0.030(3) 0.047(3) 0.046(3) 0.000(2) 0.007(2) 0.001(2) N32A 0.054(3) 0.051(3) 0.059(3) 0.004(2) 0.001(2) -0.009(2) C33A 0.058(4) 0.054(4) 0.058(4) 0.015(3) 0.010(3) 0.000(3) C34A 0.045(3) 0.059(4) 0.038(3) 0.005(3) 0.005(2) 0.003(3) C35A 0.053(3) 0.053(3) 0.056(4) 0.002(3) -0.008(3) -0.009(3) N36A 0.054(3) 0.051(3) 0.049(3) 0.006(2) -0.008(2) -0.006(2) C41 0.038(3) 0.038(3) 0.041(3) 0.000(2) -0.002(2) 0.002(2) C42 0.037(3) 0.031(2) 0.040(3) -0.003(2) 0.003(2) 0.003(2) C43 0.037(3) 0.033(3) 0.048(3) -0.001(2) 0.004(2) 0.001(2) C44 0.051(3) 0.041(3) 0.060(4) -0.007(3) 0.012(3) 0.007(3) C45 0.068(4) 0.031(3) 0.071(4) -0.008(3) 0.020(3) 0.002(3) C46 0.051(3) 0.040(3) 0.057(4) 0.003(3) 0.007(3) -0.009(3) C41A 0.033(3) 0.036(3) 0.053(3) -0.002(2) 0.007(2) -0.001(2) N42A 0.045(3) 0.058(3) 0.059(3) 0.006(2) -0.006(2) -0.002(2) C43A 0.039(3) 0.071(4) 0.076(5) -0.011(4) -0.006(3) -0.003(3) C44A 0.040(3) 0.049(4) 0.092(5) -0.013(3) 0.015(3) -0.011(3) C45A 0.060(4) 0.050(4) 0.093(5) 0.013(3) 0.022(4) -0.005(3) N46A 0.048(3) 0.056(3) 0.057(3) 0.010(2) 0.009(2) -0.009(2) Cl1S 0.149(3) 0.106(2) 0.102(2) -0.0222(16) 0.0293(18) -0.0343(19) Cl2S 0.0630(15) 0.120(2) 0.235(4) -0.027(3) -0.0203(19) -0.0006(15) Cl3S 0.0841(18) 0.141(3) 0.190(3) 0.080(3) 0.052(2) 0.0239(18) C1S 0.114(7) 0.056(5) 0.091(6) 0.002(4) 0.025(5) -0.020(5) Cl1T 0.318(11) 0.088(3) 0.277(10) 0.022(4) 0.105(8) -0.012(5) Cl2T 0.120(4) 0.202(6) 0.245(8) 0.040(6) 0.007(4) 0.007(4) Cl3T 0.262(8) 0.205(6) 0.105(4) 0.014(4) -0.045(4) 0.006(6) C1T 0.137(13) 0.108(11) 0.084(10) 0.037(8) 0.046(9) 0.008(10) Cl4T 0.254(15) 0.266(18) 0.111(9) -0.051(10) 0.085(10) -0.097(14) Cl5T 0.33(2) 0.214(16) 0.29(2) -0.018(15) 0.125(19) -0.107(16) Cl6T 0.32(2) 0.26(2) 0.39(3) 0.10(2) -0.014(19) -0.036(17) C2T 0.23(3) 0.23(3) 0.22(3) 0.00(2) 0.03(3) -0.04(2) O1W 0.177(16) 0.41(3) 0.207(19) 0.024(19) 0.102(15) -0.130(18) _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 Br14 C14A 1.881(6) . ? Br24 C24A 1.886(6) . ? Br34 C34A 1.866(5) . ? Br44 C44A 1.879(6) . ? O1 C1 1.195(7) . ? C1 C13 1.459(8) . ? C1 N1 1.466(7) . ? N1 C2 1.393(7) . ? N1 C11A 1.415(7) . ? O2 C2 1.206(7) . ? C2 C21 1.485(8) . ? O3 C3 1.193(6) . ? C3 N2 1.427(7) . ? C3 C23 1.487(8) . ? N2 C4 1.404(7) . ? N2 C21A 1.427(6) . ? O4 C4 1.199(6) . ? C4 C31 1.487(7) . ? O5 C5 1.198(7) . ? C5 N3 1.418(7) . ? C5 C33 1.479(8) . ? N3 C6 1.407(7) . ? N3 C31A 1.439(7) . ? O6 C6 1.210(7) . ? C6 C41 1.484(8) . ? O7 C7 1.188(7) . ? C7 N4 1.439(7) . ? C7 C43 1.487(8) . ? N4 C8 1.409(7) . ? N4 C41A 1.425(7) . ? O8 C8 1.199(6) . ? C8 C11 1.469(8) . ? C11 C12 1.381(7) . ? C11 C16 1.392(7) . ? C12 C13 1.387(7) . ? C12 H12 0.9300 . ? C13 C14 1.397(7) . ? C14 C15 1.377(9) . ? C14 H14 0.9300 . ? C15 C16 1.371(9) . ? C15 H15 0.9300 . ? C16 H16 0.9300 . ? C11A N16A 1.319(7) . ? C11A N12A 1.328(7) . ? N12A C13A 1.339(8) . ? C14A C13A 1.349(10) . ? C14A C15A 1.362(9) . ? C15A N16A 1.340(8) . ? C15A H15A 0.9300 . ? C13A H13A 0.9300 . ? C21 C22 1.386(7) . ? C21 C26 1.388(8) . ? C22 C23 1.382(7) . ? C22 H22 0.9300 . ? C23 C24 1.383(7) . ? C24 C25 1.372(9) . ? C24 H24 0.9300 . ? C25 C26 1.374(9) . ? C25 H25 0.9300 . ? C26 H26 0.9300 . ? C21A N22A 1.319(7) . ? C21A N26A 1.322(7) . ? N22A C23A 1.327(8) . ? C23A C24A 1.368(8) . ? C23A H23A 0.9300 . ? C24A C25A 1.347(8) . ? C25A N26A 1.345(7) . ? C25A H25A 0.9300 . ? C31 C32 1.385(7) . ? C31 C36 1.388(7) . ? C32 C33 1.391(7) . ? C32 H32 0.9300 . ? C33 C34 1.386(8) . ? C34 C35 1.371(9) . ? C34 H34 0.9300 . ? C35 C36 1.382(8) . ? C35 H35 0.9300 . ? C36 H36 0.9300 . ? C31A N32A 1.306(7) . ? C31A N36A 1.316(7) . ? N32A C33A 1.340(8) . ? C33A C34A 1.369(9) . ? C33A H33A 0.9300 . ? C34A C35A 1.366(8) . ? C35A N36A 1.324(7) . ? C35A H35A 0.9300 . ? C41 C46 1.387(8) . ? C41 C42 1.392(7) . ? C42 C43 1.387(7) . ? C42 H42 0.9300 . ? C43 C44 1.398(7) . ? C44 C45 1.375(9) . ? C44 H44 0.9300 . ? C45 C46 1.367(8) . ? C45 H45 0.9300 . ? C46 H46 0.9300 . ? C41A N42A 1.316(7) . ? C41A N46A 1.320(7) . ? N42A C43A 1.348(8) . ? C43A C44A 1.344(10) . ? C43A H43A 0.9300 . ? C44A C45A 1.371(10) . ? C45A N46A 1.336(8) . ? C45A H45A 0.9300 . ? Cl1S C1S 1.738(10) . ? Cl2S C1S 1.749(11) . ? Cl3S C1S 1.731(10) . ? C1S H1S 0.9800 . ? Cl1T C1T 1.681(11) . ? Cl2T C1T 1.680(12) . ? Cl3T C1T 1.804(11) . ? C1T H1T 0.9800 . ? Cl4T C2T 1.9312 . ? Cl5T C2T 1.5752 . ? Cl6T C2T 1.7312 . ? C2T H2T 0.9800 . ? O1W H1W 0.98(3) . ? O1W H2W 0.97(3) . ? 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 O1 C1 C13 124.6(5) . . ? O1 C1 N1 118.2(5) . . ? C13 C1 N1 117.0(4) . . ? C2 N1 C11A 124.2(4) . . ? C2 N1 C1 115.6(4) . . ? C11A N1 C1 115.0(4) . . ? O2 C2 N1 119.6(5) . . ? O2 C2 C21 122.3(5) . . ? N1 C2 C21 118.1(5) . . ? O3 C3 N2 119.6(5) . . ? O3 C3 C23 123.6(5) . . ? N2 C3 C23 116.7(4) . . ? C4 N2 C21A 119.9(4) . . ? C4 N2 C3 119.7(4) . . ? C21A N2 C3 116.2(4) . . ? O4 C4 N2 121.1(5) . . ? O4 C4 C31 122.5(5) . . ? N2 C4 C31 116.3(4) . . ? O5 C5 N3 119.8(5) . . ? O5 C5 C33 122.4(5) . . ? N3 C5 C33 117.5(4) . . ? C6 N3 C5 121.4(5) . . ? C6 N3 C31A 118.0(4) . . ? C5 N3 C31A 115.0(4) . . ? O6 C6 N3 121.9(5) . . ? O6 C6 C41 121.4(5) . . ? N3 C6 C41 116.5(5) . . ? O7 C7 N4 120.1(5) . . ? O7 C7 C43 123.4(5) . . ? N4 C7 C43 116.4(4) . . ? C8 N4 C41A 121.2(4) . . ? C8 N4 C7 118.1(4) . . ? C41A N4 C7 116.1(4) . . ? O8 C8 N4 119.4(5) . . ? O8 C8 C11 122.5(5) . . ? N4 C8 C11 118.0(4) . . ? C12 C11 C16 119.0(5) . . ? C12 C11 C8 123.0(4) . . ? C16 C11 C8 117.7(5) . . ? C11 C12 C13 120.7(5) . . ? C11 C12 H12 119.6 . . ? C13 C12 H12 119.6 . . ? C12 C13 C14 119.3(5) . . ? C12 C13 C1 123.3(5) . . ? C14 C13 C1 117.3(5) . . ? C15 C14 C13 119.9(5) . . ? C15 C14 H14 120.0 . . ? C13 C14 H14 120.0 . . ? C16 C15 C14 120.3(5) . . ? C16 C15 H15 119.8 . . ? C14 C15 H15 119.8 . . ? C15 C16 C11 120.7(5) . . ? C15 C16 H16 119.7 . . ? C11 C16 H16 119.7 . . ? N16A C11A N12A 128.2(5) . . ? N16A C11A N1 117.5(5) . . ? N12A C11A N1 114.3(5) . . ? C11A N12A C13A 114.7(5) . . ? C13A C14A C15A 118.9(6) . . ? C13A C14A Br14 120.4(5) . . ? C15A C14A Br14 120.7(5) . . ? N16A C15A C14A 121.2(6) . . ? N16A C15A H15A 119.4 . . ? C14A C15A H15A 119.4 . . ? N12A C13A C14A 121.8(6) . . ? N12A C13A H13A 119.1 . . ? C14A C13A H13A 119.1 . . ? C11A N16A C15A 115.1(5) . . ? C22 C21 C26 119.1(5) . . ? C22 C21 C2 122.3(5) . . ? C26 C21 C2 118.5(5) . . ? C23 C22 C21 120.2(5) . . ? C23 C22 H22 119.9 . . ? C21 C22 H22 119.9 . . ? C22 C23 C24 120.2(5) . . ? C22 C23 C3 121.6(5) . . ? C24 C23 C3 118.1(5) . . ? C25 C24 C23 119.5(5) . . ? C25 C24 H24 120.3 . . ? C23 C24 H24 120.3 . . ? C24 C25 C26 120.8(5) . . ? C24 C25 H25 119.6 . . ? C26 C25 H25 119.6 . . ? C25 C26 C21 120.2(5) . . ? C25 C26 H26 119.9 . . ? C21 C26 H26 119.9 . . ? N22A C21A N26A 128.7(5) . . ? N22A C21A N2 115.4(4) . . ? N26A C21A N2 115.8(4) . . ? C21A N22A C23A 114.9(5) . . ? N22A C23A C24A 121.7(5) . . ? N22A C23A H23A 119.2 . . ? C24A C23A H23A 119.2 . . ? C25A C24A C23A 118.5(5) . . ? C25A C24A Br24 121.0(5) . . ? C23A C24A Br24 120.5(5) . . ? N26A C25A C24A 121.8(5) . . ? N26A C25A H25A 119.1 . . ? C24A C25A H25A 119.1 . . ? C21A N26A C25A 114.3(5) . . ? C32 C31 C36 120.4(5) . . ? C32 C31 C4 121.1(4) . . ? C36 C31 C4 118.3(5) . . ? C31 C32 C33 119.4(5) . . ? C31 C32 H32 120.3 . . ? C33 C32 H32 120.3 . . ? C34 C33 C32 119.6(5) . . ? C34 C33 C5 118.2(5) . . ? C32 C33 C5 121.7(5) . . ? C35 C34 C33 120.7(5) . . ? C35 C34 H34 119.7 . . ? C33 C34 H34 119.7 . . ? C34 C35 C36 120.0(5) . . ? C34 C35 H35 120.0 . . ? C36 C35 H35 120.0 . . ? C35 C36 C31 119.7(5) . . ? C35 C36 H36 120.2 . . ? C31 C36 H36 120.2 . . ? N32A C31A N36A 128.7(5) . . ? N32A C31A N3 115.9(5) . . ? N36A C31A N3 115.4(5) . . ? C31A N32A C33A 114.8(5) . . ? N32A C33A C34A 122.1(6) . . ? N32A C33A H33A 118.9 . . ? C34A C33A H33A 118.9 . . ? C35A C34A C33A 116.6(5) . . ? C35A C34A Br34 120.4(5) . . ? C33A C34A Br34 123.0(5) . . ? N36A C35A C34A 122.8(6) . . ? N36A C35A H35A 118.6 . . ? C34A C35A H35A 118.6 . . ? C31A N36A C35A 114.9(5) . . ? C46 C41 C42 119.7(5) . . ? C46 C41 C6 119.5(5) . . ? C42 C41 C6 120.5(5) . . ? C43 C42 C41 119.9(5) . . ? C43 C42 H42 120.1 . . ? C41 C42 H42 120.1 . . ? C42 C43 C44 119.1(5) . . ? C42 C43 C7 122.9(5) . . ? C44 C43 C7 117.9(5) . . ? C45 C44 C43 120.7(5) . . ? C45 C44 H44 119.6 . . ? C43 C44 H44 119.6 . . ? C46 C45 C44 119.9(5) . . ? C46 C45 H45 120.1 . . ? C44 C45 H45 120.1 . . ? C45 C46 C41 120.7(5) . . ? C45 C46 H46 119.6 . . ? C41 C46 H46 119.6 . . ? N42A C41A N46A 128.5(5) . . ? N42A C41A N4 114.6(5) . . ? N46A C41A N4 116.8(5) . . ? C41A N42A C43A 114.8(5) . . ? C44A C43A N42A 121.8(6) . . ? C44A C43A H43A 119.1 . . ? N42A C43A H43A 119.1 . . ? C43A C44A C45A 118.3(6) . . ? C43A C44A Br44 120.3(6) . . ? C45A C44A Br44 121.5(5) . . ? N46A C45A C44A 121.8(6) . . ? N46A C45A H45A 119.1 . . ? C44A C45A H45A 119.1 . . ? C41A N46A C45A 114.7(5) . . ? Cl3S C1S Cl1S 105.1(6) . . ? Cl3S C1S Cl2S 109.8(5) . . ? Cl1S C1S Cl2S 111.6(6) . . ? Cl3S C1S H1S 110.1 . . ? Cl1S C1S H1S 110.1 . . ? Cl2S C1S H1S 110.1 . . ? Cl2T C1T Cl1T 117.6(6) . . ? Cl2T C1T Cl3T 108.7(7) . . ? Cl1T C1T Cl3T 103.7(6) . . ? Cl2T C1T H1T 108.8 . . ? Cl1T C1T H1T 108.8 . . ? Cl3T C1T H1T 108.8 . . ? Cl5T C2T Cl6T 99.1 . . ? Cl5T C2T Cl4T 105.3 . . ? Cl6T C2T Cl4T 103.8 . . ? Cl5T C2T H2T 115.6 . . ? Cl6T C2T H2T 115.6 . . ? Cl4T C2T H2T 115.6 . . ? H1W O1W H2W 81(2) . . ? 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 O1 C1 N1 C2 112.9(7) . . . . ? C13 C1 N1 C2 -70.5(7) . . . . ? O1 C1 N1 C11A -42.8(8) . . . . ? C13 C1 N1 C11A 133.8(5) . . . . ? C11A N1 C2 O2 145.5(6) . . . . ? C1 N1 C2 O2 -7.6(8) . . . . ? C11A N1 C2 C21 -37.9(7) . . . . ? C1 N1 C2 C21 168.9(5) . . . . ? O3 C3 N2 C4 -131.6(6) . . . . ? C23 C3 N2 C4 52.2(6) . . . . ? O3 C3 N2 C21A 25.2(7) . . . . ? C23 C3 N2 C21A -150.9(5) . . . . ? C21A N2 C4 O4 -144.2(5) . . . . ? C3 N2 C4 O4 11.8(7) . . . . ? C21A N2 C4 C31 38.1(6) . . . . ? C3 N2 C4 C31 -165.9(4) . . . . ? O5 C5 N3 C6 142.3(6) . . . . ? C33 C5 N3 C6 -43.0(7) . . . . ? O5 C5 N3 C31A -10.8(8) . . . . ? C33 C5 N3 C31A 163.9(5) . . . . ? C5 N3 C6 O6 -14.1(8) . . . . ? C31A N3 C6 O6 138.2(6) . . . . ? C5 N3 C6 C41 162.5(5) . . . . ? C31A N3 C6 C41 -45.2(6) . . . . ? O7 C7 N4 C8 -126.0(6) . . . . ? C43 C7 N4 C8 58.3(7) . . . . ? O7 C7 N4 C41A 30.3(8) . . . . ? C43 C7 N4 C41A -145.4(5) . . . . ? C41A N4 C8 O8 -146.5(5) . . . . ? C7 N4 C8 O8 8.5(8) . . . . ? C41A N4 C8 C11 36.0(7) . . . . ? C7 N4 C8 C11 -168.9(5) . . . . ? O8 C8 C11 C12 -140.7(6) . . . . ? N4 C8 C11 C12 36.7(7) . . . . ? O8 C8 C11 C16 34.1(8) . . . . ? N4 C8 C11 C16 -148.5(5) . . . . ? C16 C11 C12 C13 -0.5(7) . . . . ? C8 C11 C12 C13 174.3(5) . . . . ? C11 C12 C13 C14 1.5(8) . . . . ? C11 C12 C13 C1 -174.7(5) . . . . ? O1 C1 C13 C12 160.9(7) . . . . ? N1 C1 C13 C12 -15.4(8) . . . . ? O1 C1 C13 C14 -15.3(9) . . . . ? N1 C1 C13 C14 168.4(5) . . . . ? C12 C13 C14 C15 -1.2(8) . . . . ? C1 C13 C14 C15 175.2(6) . . . . ? C13 C14 C15 C16 -0.2(9) . . . . ? C14 C15 C16 C11 1.2(9) . . . . ? C12 C11 C16 C15 -0.9(8) . . . . ? C8 C11 C16 C15 -175.9(5) . . . . ? C2 N1 C11A N16A -24.5(7) . . . . ? C1 N1 C11A N16A 128.8(5) . . . . ? C2 N1 C11A N12A 156.1(5) . . . . ? C1 N1 C11A N12A -50.6(6) . . . . ? N16A C11A N12A C13A -3.5(9) . . . . ? N1 C11A N12A C13A 175.8(5) . . . . ? C13A C14A C15A N16A -3.1(10) . . . . ? Br14 C14A C15A N16A 176.6(5) . . . . ? C11A N12A C13A C14A 2.2(9) . . . . ? C15A C14A C13A N12A 0.8(10) . . . . ? Br14 C14A C13A N12A -178.9(5) . . . . ? N12A C11A N16A C15A 1.4(8) . . . . ? N1 C11A N16A C15A -177.9(5) . . . . ? C14A C15A N16A C11A 2.0(9) . . . . ? O2 C2 C21 C22 142.6(6) . . . . ? N1 C2 C21 C22 -33.9(8) . . . . ? O2 C2 C21 C26 -33.7(8) . . . . ? N1 C2 C21 C26 149.9(5) . . . . ? C26 C21 C22 C23 2.3(8) . . . . ? C2 C21 C22 C23 -174.0(5) . . . . ? C21 C22 C23 C24 -1.9(8) . . . . ? C21 C22 C23 C3 173.5(5) . . . . ? O3 C3 C23 C22 -147.2(6) . . . . ? N2 C3 C23 C22 28.8(7) . . . . ? O3 C3 C23 C24 28.3(8) . . . . ? N2 C3 C23 C24 -155.7(5) . . . . ? C22 C23 C24 C25 -0.1(9) . . . . ? C3 C23 C24 C25 -175.7(5) . . . . ? C23 C24 C25 C26 1.7(10) . . . . ? C24 C25 C26 C21 -1.4(10) . . . . ? C22 C21 C26 C25 -0.6(9) . . . . ? C2 C21 C26 C25 175.8(6) . . . . ? C4 N2 C21A N22A -145.8(5) . . . . ? C3 N2 C21A N22A 57.4(6) . . . . ? C4 N2 C21A N26A 34.4(6) . . . . ? C3 N2 C21A N26A -122.4(5) . . . . ? N26A C21A N22A C23A 1.0(8) . . . . ? N2 C21A N22A C23A -178.8(5) . . . . ? C21A N22A C23A C24A -2.3(9) . . . . ? N22A C23A C24A C25A 1.0(10) . . . . ? N22A C23A C24A Br24 -177.7(5) . . . . ? C23A C24A C25A N26A 1.9(9) . . . . ? Br24 C24A C25A N26A -179.5(5) . . . . ? N22A C21A N26A C25A 1.6(8) . . . . ? N2 C21A N26A C25A -178.6(5) . . . . ? C24A C25A N26A C21A -3.0(8) . . . . ? O4 C4 C31 C32 -138.7(5) . . . . ? N2 C4 C31 C32 39.0(7) . . . . ? O4 C4 C31 C36 36.5(7) . . . . ? N2 C4 C31 C36 -145.9(5) . . . . ? C36 C31 C32 C33 -1.3(8) . . . . ? C4 C31 C32 C33 173.8(5) . . . . ? C31 C32 C33 C34 3.3(8) . . . . ? C31 C32 C33 C5 -168.8(5) . . . . ? O5 C5 C33 C34 -36.0(9) . . . . ? N3 C5 C33 C34 149.5(5) . . . . ? O5 C5 C33 C32 136.2(6) . . . . ? N3 C5 C33 C32 -38.4(8) . . . . ? C32 C33 C34 C35 -1.8(9) . . . . ? C5 C33 C34 C35 170.5(6) . . . . ? C33 C34 C35 C36 -1.8(10) . . . . ? C34 C35 C36 C31 3.8(9) . . . . ? C32 C31 C36 C35 -2.3(8) . . . . ? C4 C31 C36 C35 -177.5(5) . . . . ? C6 N3 C31A N32A 136.1(5) . . . . ? C5 N3 C31A N32A -69.9(6) . . . . ? C6 N3 C31A N36A -45.1(6) . . . . ? C5 N3 C31A N36A 108.9(6) . . . . ? N36A C31A N32A C33A -3.0(9) . . . . ? N3 C31A N32A C33A 175.6(5) . . . . ? C31A N32A C33A C34A 0.1(9) . . . . ? N32A C33A C34A C35A 1.9(9) . . . . ? N32A C33A C34A Br34 -178.9(5) . . . . ? C33A C34A C35A N36A -1.6(10) . . . . ? Br34 C34A C35A N36A 179.3(5) . . . . ? N32A C31A N36A C35A 3.3(9) . . . . ? N3 C31A N36A C35A -175.3(5) . . . . ? C34A C35A N36A C31A -0.8(9) . . . . ? O6 C6 C41 C46 -36.4(8) . . . . ? N3 C6 C41 C46 147.0(5) . . . . ? O6 C6 C41 C42 137.2(6) . . . . ? N3 C6 C41 C42 -39.4(7) . . . . ? C46 C41 C42 C43 1.2(8) . . . . ? C6 C41 C42 C43 -172.3(5) . . . . ? C41 C42 C43 C44 -2.2(8) . . . . ? C41 C42 C43 C7 172.6(5) . . . . ? O7 C7 C43 C42 -154.5(6) . . . . ? N4 C7 C43 C42 21.1(8) . . . . ? O7 C7 C43 C44 20.4(9) . . . . ? N4 C7 C43 C44 -164.0(5) . . . . ? C42 C43 C44 C45 1.0(9) . . . . ? C7 C43 C44 C45 -174.1(6) . . . . ? C43 C44 C45 C46 1.2(10) . . . . ? C44 C45 C46 C41 -2.1(10) . . . . ? C42 C41 C46 C45 0.9(9) . . . . ? C6 C41 C46 C45 174.6(6) . . . . ? C8 N4 C41A N42A -148.4(5) . . . . ? C7 N4 C41A N42A 56.1(7) . . . . ? C8 N4 C41A N46A 31.3(7) . . . . ? C7 N4 C41A N46A -124.2(5) . . . . ? N46A C41A N42A C43A 0.3(9) . . . . ? N4 C41A N42A C43A 180.0(5) . . . . ? C41A N42A C43A C44A -0.9(9) . . . . ? N42A C43A C44A C45A 0.8(10) . . . . ? N42A C43A C44A Br44 179.9(5) . . . . ? C43A C44A C45A N46A -0.1(10) . . . . ? Br44 C44A C45A N46A -179.2(5) . . . . ? N42A C41A N46A C45A 0.4(9) . . . . ? N4 C41A N46A C45A -179.3(5) . . . . ? C44A C45A N46A C41A -0.5(9) . . . . ? _iucr_refine_instructions_details ; TITL 11-128 is 2,6_BrIO4:2CHCl3 Mo = 40kV30mA to 0.80\%A [Relabel] CELL 0.71073 10.5779 13.2805 40.7855 90.000 95.936 90.000 ZERR 4 0.0003 0.0003 0.0013 0.000 0.002 0.000 LATT 1 SYMM 1/2-X,1/2+Y,1/2-Z SFAC C H N O CL BR UNIT 199.6 107.6 48 34 22.8 16 MERG 3 FMAP 2 L.S. 10 3 LIST 4 ACTA 52 CONF BOND $H DELU 0.03 CL4T CL5T CL6T C2T O1W ISOR 0.03 CL4T CL5T CL6T C2T O1W EQIV $1 X-1,Y,Z EQIV $2 1/2-X,-1/2+Y,1/2-Z EQIV $3 -X,1-Y,-Z EQIV $4 X,1+Y,Z EQIV $5 1+X,Y,Z HTAB HTAB C12 N1 HTAB C42 N4 HTAB C43A O5_$1 HTAB C14 O8_$2 HTAB C15 O8_$2 HTAB C15A O4_$3 HTAB C35A CL1S_$4 HTAB C34 O3_$5 RTAB XX BR14 BR24 RTAB XX BR14 BR34 RTAB XX BR14 BR44 RTAB XX BR24 BR34 RTAB XX BR24 BR44 RTAB XX BR34 BR44 RTAB XN BR34 N16A_$4 RTAB OO O1 O2 RTAB OO O3 O4 RTAB OO O5 O6 RTAB OO O7 O8 RTAB OO O1 O8 RTAB OO O2 O3 RTAB OO O4 O5 RTAB OO O6 O7 RTAB NN N1 N2 RTAB NN N1 N3 RTAB NN N1 N4 RTAB NN N2 N3 RTAB NN N2 N4 RTAB NN N3 N4 RTAB NN N12A N32A RTAB NN N22A N42A RTAB OCCO O1 C1 C2 O2 RTAB OCCO O3 C3 C4 O4 RTAB OCCO O5 C5 C6 O6 RTAB OCCO O7 C7 C8 O8 RTAB OCCO O1 C1 C8 O8 RTAB OCCO O2 C2 C3 O3 RTAB OCCO O4 C4 C5 O5 RTAB OCCO O6 C6 C7 O7 RTAB CCNC C13 C1 N1 C2 RTAB CCNC C23 C3 N2 C4 RTAB CCNC C33 C5 N3 C6 RTAB CCNC C43 C7 N4 C8 RTAB CNCC C1 N1 C2 C21 RTAB CNCC C3 N2 C4 C31 RTAB CNCC C5 N3 C6 C41 RTAB CNCC C7 N4 C8 C11 RTAB OCNC O1 C1 N1 C2 RTAB OCNC O3 C3 N2 C4 RTAB OCNC O5 C5 N3 C6 RTAB OCNC O7 C7 N4 C8 RTAB CNCO C1 N1 C2 O2 RTAB CNCO C3 N2 C4 O4 RTAB CNCO C5 N3 C6 O6 RTAB CNCO C7 N4 C8 O8 RTAB CNCN C1 N1 C11A N12A RTAB CNCN C3 N2 C21A N22A RTAB CNCN C5 N3 C31A N32A RTAB CNCN C7 N4 C41A N42A SIZE 0.22 0.35 0.39 TEMP 21 PLAN 15 MPLA 3 C1 C2 C11A N1 MPLA 3 C3 C4 C21A N2 MPLA 3 C5 C6 C31A N3 MPLA 3 C7 C8 C41A N4 MPLA 6 C11 C12 C13 C14 C15 C16 C1 O1 C8 O8 BR14 BR24 BR34 BR44 MPLA 6 C21 C22 C23 C24 C25 C26 C2 O2 C3 O3 BR14 BR24 BR34 BR44 MPLA 6 C31 C32 C33 C34 C35 C36 C4 O4 C5 O5 BR14 BR24 BR34 BR44 MPLA 6 C41 C42 C43 C44 C45 C46 C6 O6 C7 O7 BR14 BR24 BR34 BR44 MPLA 6 C11 C12 C13 C14 C15 C16 C1 O1 C8 O8 BR14 BR24 BR34 BR44 WGHT 0.084500 14.950000 FVAR 2.17235 MOLE 1 BR14 6 0.306037 0.515234 0.006004 11.00000 0.15671 0.07482 = 0.10280 -0.02002 0.08780 -0.01500 BR24 6 -0.031960 1.238617 0.076724 11.00000 0.12233 0.03912 = 0.06478 -0.00621 0.00464 -0.00651 BR34 6 0.585918 0.826491 0.267698 11.00000 0.08824 0.10064 = 0.04908 0.02443 -0.01127 -0.01059 BR44 6 -0.477556 0.500049 0.177453 11.00000 0.07011 0.09482 = 0.18821 -0.03512 0.02588 -0.04436 O1 4 0.226674 0.396706 0.153589 11.00000 0.11453 0.08736 = 0.06415 -0.01165 -0.01209 0.06476 C1 1 0.153983 0.463282 0.157756 11.00000 0.05621 0.04445 = 0.04444 0.00556 -0.00016 0.01676 N1 3 0.064063 0.494362 0.129809 11.00000 0.04437 0.04125 = 0.03452 0.00084 -0.00056 0.00524 O2 4 -0.091502 0.424500 0.155774 11.00000 0.06763 0.08010 = 0.05420 0.03029 -0.00003 -0.01876 C2 1 -0.063375 0.474171 0.132869 11.00000 0.04949 0.04081 = 0.04108 -0.00014 0.00140 -0.00427 O3 4 -0.323090 0.818124 0.057767 11.00000 0.03405 0.05448 = 0.10424 0.02124 0.00777 0.00831 C3 1 -0.233819 0.763297 0.062624 11.00000 0.03174 0.04544 = 0.04856 0.00433 0.00554 0.00183 N2 3 -0.109509 0.800287 0.058837 11.00000 0.02956 0.03663 = 0.04394 0.00447 0.00330 -0.00010 O4 4 -0.068247 0.675294 0.023508 11.00000 0.05315 0.06142 = 0.05469 -0.01951 0.01086 -0.01323 C4 1 -0.028821 0.744709 0.040396 11.00000 0.03994 0.03828 = 0.03185 0.00342 0.00401 -0.00113 O5 4 0.473313 0.792403 0.116984 11.00000 0.04389 0.12110 = 0.06095 -0.00597 -0.00052 0.03419 C5 1 0.372088 0.831818 0.110217 11.00000 0.03121 0.06312 = 0.05099 -0.00476 0.00620 0.00321 N3 3 0.313879 0.884968 0.134809 11.00000 0.03371 0.05297 = 0.04187 -0.00105 -0.00054 0.00445 O6 4 0.252760 1.020100 0.102058 11.00000 0.08064 0.05431 = 0.05580 0.01057 0.02030 0.00165 C6 1 0.245557 0.974458 0.127465 11.00000 0.03888 0.04222 = 0.05229 0.00539 0.00232 -0.00336 O7 4 -0.198234 0.924197 0.207205 11.00000 0.05746 0.04918 = 0.13589 -0.00132 0.04908 0.00606 C7 1 -0.096675 0.899013 0.200158 11.00000 0.04145 0.03749 = 0.05682 -0.00333 0.01063 -0.00136 N4 3 -0.059613 0.794834 0.202570 11.00000 0.03915 0.03482 = 0.04819 -0.00176 0.00484 -0.00342 O8 4 0.111507 0.834682 0.237811 11.00000 0.07791 0.04721 = 0.05943 -0.00936 -0.02092 -0.01038 C8 1 0.055605 0.770645 0.221415 11.00000 0.04399 0.04318 = 0.03302 -0.00253 0.00018 -0.00725 C11 1 0.105202 0.667868 0.218995 11.00000 0.03257 0.03987 = 0.03708 0.00347 0.00040 -0.00924 C12 1 0.094584 0.613542 0.189968 11.00000 0.03266 0.03860 = 0.03436 0.00632 -0.00148 0.00047 AFIX 43 H12 2 0.047941 0.639759 0.171331 11.00000 -1.20000 AFIX 0 C13 1 0.152673 0.520356 0.188298 11.00000 0.03751 0.03752 = 0.04546 0.00691 0.00352 0.00481 C14 1 0.220038 0.480424 0.216590 11.00000 0.04290 0.04642 = 0.05463 0.01657 -0.00511 0.00662 AFIX 43 H14 2 0.258069 0.417437 0.215865 11.00000 -1.20000 AFIX 0 C15 1 0.230075 0.534458 0.245570 11.00000 0.05766 0.05921 = 0.04136 0.01198 -0.01597 0.00639 AFIX 43 H15 2 0.274784 0.507733 0.264410 11.00000 -1.20000 AFIX 0 C16 1 0.174484 0.627423 0.246772 11.00000 0.05131 0.05604 = 0.03957 -0.00085 -0.00712 -0.00535 AFIX 43 H16 2 0.183144 0.663856 0.266348 11.00000 -1.20000 AFIX 0 C11A 1 0.116322 0.502100 0.099342 11.00000 0.03898 0.03084 = 0.04522 -0.00156 0.00349 0.00838 N12A 3 0.222022 0.556538 0.100520 11.00000 0.04591 0.05206 = 0.06009 -0.01355 0.00638 -0.00370 C14A 1 0.224530 0.511949 0.044857 11.00000 0.07457 0.03739 = 0.06807 -0.00910 0.03366 0.00218 C15A 1 0.112494 0.461982 0.045800 11.00000 0.07807 0.05099 = 0.04959 -0.01015 0.01760 -0.00475 AFIX 43 H15A 2 0.073940 0.432221 0.026680 11.00000 -1.20000 AFIX 0 C13A 1 0.276643 0.558827 0.072343 11.00000 0.05613 0.05057 = 0.09064 -0.01631 0.03569 -0.00818 AFIX 43 H13A 2 0.352596 0.593691 0.071700 11.00000 -1.20000 AFIX 0 N16A 3 0.056784 0.454910 0.073774 11.00000 0.05486 0.04285 = 0.04384 -0.00816 0.00426 -0.00840 C21 1 -0.160566 0.520163 0.108509 11.00000 0.04014 0.03921 = 0.03938 0.00091 0.00735 -0.00811 C22 1 -0.144694 0.614467 0.094943 11.00000 0.02972 0.03888 = 0.03957 -0.00143 0.00503 -0.00331 AFIX 43 H22 2 -0.067993 0.648448 0.099455 11.00000 -1.20000 AFIX 0 C23 1 -0.242542 0.658133 0.074728 11.00000 0.03169 0.04448 = 0.03839 -0.00178 0.01064 -0.00246 C24 1 -0.355483 0.606771 0.067135 11.00000 0.03060 0.05631 = 0.06036 0.00144 0.00022 -0.00463 AFIX 43 H24 2 -0.421425 0.636116 0.053565 11.00000 -1.20000 AFIX 0 C25 1 -0.369479 0.512158 0.079784 11.00000 0.04162 0.05588 = 0.07786 -0.00112 0.00333 -0.01851 AFIX 43 H25 2 -0.444497 0.476762 0.074221 11.00000 -1.20000 AFIX 0 C26 1 -0.274039 0.469037 0.100571 11.00000 0.04993 0.04351 = 0.06545 0.00817 0.00831 -0.00860 AFIX 43 H26 2 -0.285523 0.405443 0.109339 11.00000 -1.20000 AFIX 0 C21A 1 -0.091197 0.906163 0.062923 11.00000 0.02647 0.03637 = 0.03944 0.00202 0.00169 0.00161 N22A 3 -0.117058 0.942898 0.091536 11.00000 0.05135 0.04390 = 0.04840 -0.00010 0.01232 0.00195 C23A 1 -0.101936 1.041687 0.094805 11.00000 0.06818 0.04880 = 0.03967 -0.00369 0.01179 0.00882 AFIX 43 H23A 2 -0.121599 1.072662 0.114089 11.00000 -1.20000 AFIX 0 C24A 1 -0.058156 1.099157 0.070534 11.00000 0.05909 0.03567 = 0.05313 -0.00023 -0.00019 0.00231 C25A 1 -0.031921 1.053516 0.042519 11.00000 0.07175 0.03632 = 0.04663 0.00568 0.01018 0.00143 AFIX 43 H25A 2 0.000223 1.091651 0.026148 11.00000 -1.20000 AFIX 0 N26A 3 -0.050968 0.954285 0.037592 11.00000 0.05849 0.03827 = 0.03696 0.00472 0.00880 0.00357 C31 1 0.107468 0.774386 0.044104 11.00000 0.03283 0.03761 = 0.03682 0.00250 0.00574 0.00623 C32 1 0.168166 0.802241 0.074462 11.00000 0.03176 0.04078 = 0.03958 0.00190 0.00856 0.00608 AFIX 43 H32 2 0.122232 0.808982 0.092587 11.00000 -1.20000 AFIX 0 C33 1 0.298414 0.820046 0.077605 11.00000 0.03135 0.04499 = 0.04114 -0.00085 0.00446 0.00665 C34 1 0.364403 0.814751 0.050020 11.00000 0.03467 0.06476 = 0.05525 0.00030 0.01459 0.00345 AFIX 43 H34 2 0.451061 0.828513 0.051987 11.00000 -1.20000 AFIX 0 C35 1 0.303262 0.789431 0.019851 11.00000 0.04941 0.06977 = 0.04535 0.00102 0.02001 0.00225 AFIX 43 H35 2 0.347980 0.787912 0.001387 11.00000 -1.20000 AFIX 0 C36 1 0.175287 0.766179 0.016869 11.00000 0.04944 0.05091 = 0.03770 -0.00211 0.01022 0.00521 AFIX 43 H36 2 0.134798 0.745130 -0.003293 11.00000 -1.20000 AFIX 0 C31A 1 0.372982 0.871266 0.167905 11.00000 0.03035 0.04712 = 0.04583 0.00046 0.00731 0.00099 N32A 3 0.359987 0.782197 0.180726 11.00000 0.05392 0.05065 = 0.05887 0.00380 0.00058 -0.00881 C33A 1 0.423040 0.768970 0.210647 11.00000 0.05836 0.05359 = 0.05790 0.01532 0.01040 0.00040 AFIX 43 H33A 2 0.417695 0.707055 0.221067 11.00000 -1.20000 AFIX 0 C34A 1 0.495065 0.843676 0.226364 11.00000 0.04504 0.05922 = 0.03804 0.00521 0.00500 0.00299 C35A 1 0.496682 0.934086 0.210463 11.00000 0.05270 0.05279 = 0.05557 0.00233 -0.00815 -0.00860 AFIX 43 H35A 2 0.543048 0.986795 0.220779 11.00000 -1.20000 AFIX 0 N36A 3 0.435024 0.949881 0.180976 11.00000 0.05442 0.05091 = 0.04863 0.00557 -0.00810 -0.00557 C41 1 0.158177 1.007072 0.151633 11.00000 0.03751 0.03793 = 0.04122 0.00020 -0.00222 0.00179 C42 1 0.086094 0.936748 0.166862 11.00000 0.03734 0.03077 = 0.04034 -0.00256 0.00267 0.00253 AFIX 43 H42 2 0.099682 0.868273 0.163982 11.00000 -1.20000 AFIX 0 C43 1 -0.006064 0.968967 0.186344 11.00000 0.03668 0.03257 = 0.04755 -0.00089 0.00440 0.00054 C44 1 -0.021870 1.072230 0.191246 11.00000 0.05139 0.04117 = 0.06005 -0.00665 0.01201 0.00741 AFIX 43 H44 2 -0.082526 1.094467 0.204542 11.00000 -1.20000 AFIX 0 C45 1 0.051323 1.141251 0.176615 11.00000 0.06762 0.03122 = 0.07136 -0.00814 0.01992 0.00243 AFIX 43 H45 2 0.041180 1.209720 0.180349 11.00000 -1.20000 AFIX 0 C46 1 0.139001 1.109028 0.156574 11.00000 0.05126 0.03980 = 0.05704 0.00297 0.00673 -0.00910 AFIX 43 H46 2 0.186327 1.155989 0.146136 11.00000 -1.20000 AFIX 0 C41A 1 -0.159769 0.723081 0.197202 11.00000 0.03287 0.03616 = 0.05305 -0.00180 0.00673 -0.00139 N42A 3 -0.229884 0.732128 0.168756 11.00000 0.04480 0.05754 = 0.05851 0.00597 -0.00557 -0.00227 C43A 1 -0.324775 0.664406 0.163558 11.00000 0.03856 0.07078 = 0.07567 -0.01122 -0.00641 -0.00331 AFIX 43 H43A 2 -0.378563 0.667361 0.144046 11.00000 -1.20000 AFIX 0 C44A 1 -0.343813 0.592722 0.185794 11.00000 0.04022 0.04915 = 0.09220 -0.01298 0.01479 -0.01103 C45A 1 -0.264581 0.590340 0.214593 11.00000 0.06002 0.05001 = 0.09260 0.01313 0.02208 -0.00507 AFIX 43 H45A 2 -0.276818 0.541167 0.230190 11.00000 -1.20000 AFIX 0 N46A 3 -0.170280 0.656709 0.220870 11.00000 0.04778 0.05609 = 0.05721 0.00986 0.00887 -0.00888 MOLE 2 CL1S 5 0.606633 0.185916 0.204051 10.90000 0.14936 0.10602 = 0.10171 -0.02216 0.02929 -0.03432 CL2S 5 0.448698 0.241066 0.144884 10.90000 0.06297 0.11982 = 0.23463 -0.02654 -0.02034 -0.00063 CL3S 5 0.717616 0.221999 0.147041 10.90000 0.08405 0.14147 = 0.18974 0.07955 0.05163 0.02390 C1S 1 0.582032 0.173258 0.161468 10.90000 0.11363 0.05624 = 0.09079 0.00163 0.02470 -0.02001 AFIX 13 H1S 2 0.572567 0.101989 0.155482 10.90000 -1.20000 AFIX 0 MOLE 3 PART -1 CL1T 5 0.422386 1.265134 0.042407 10.70000 0.31800 0.08849 = 0.27663 0.02207 0.10478 -0.01236 CL2T 5 0.542843 1.074694 0.058212 10.70000 0.11997 0.20244 = 0.24499 0.04009 0.00688 0.00723 CL3T 5 0.303962 1.090798 0.020238 10.70000 0.26211 0.20471 = 0.10493 0.01413 -0.04503 0.00561 C1T 1 0.409239 1.143858 0.053388 10.70000 0.13682 0.10823 = 0.08447 0.03737 0.04597 0.00770 AFIX 13 H1T 2 0.367721 1.140743 0.073760 10.70000 -1.20000 PART -2 CL4T 5 0.547666 1.237226 0.060862 10.30000 0.25387 0.26645 = 0.11104 -0.05150 0.08515 -0.09747 CL5T 5 0.442939 1.073428 0.024550 10.30000 0.32829 0.21436 = 0.28820 -0.01777 0.12482 -0.10727 CL6T 5 0.288639 1.213950 0.032050 10.30000 0.31518 0.25520 = 0.39032 0.09752 -0.01402 -0.03588 C2T 1 0.407952 1.143607 0.053412 10.30000 0.22502 0.23260 = 0.22435 0.00144 0.02909 -0.03958 AFIX 13 H2T 2 0.384263 1.108777 0.073059 10.30000 -1.20000 AFIX 0 PART 1 MOLE 4 O1W 4 -0.355171 0.996957 0.133487 10.50000 0.17671 0.40914 = 0.20737 0.02438 0.10184 -0.13042 H1W 2 9.714931 10.969212 10.122461 10.50000 -1.50000 H2W 2 9.691792 10.964828 10.152460 10.50000 -1.50000 PART 0 DFIX 1.70 0.030 CL4T C2T CL5T C2T CL6T C2T HKLF 4 REM 11-128 is 2,6_BrIO4:2CHCl3 in P21/n with Mo 40kV30mA to 0.80\%A REM R1 = 0.0763 for 7949 Fo > 4sig(Fo) and 0.1177 for all 12192 data REM 754 parameters refined using 39 restraints END WGHT 0.0845 14.9598 REM Highest difference peak 1.159, deepest hole -1.224, 1-sigma level 0.087 Q1 1 -0.4761 0.5117 0.2032 11.00000 0.05 1.16 Q2 1 0.4961 0.2238 0.1926 11.00000 0.05 1.14 Q3 1 0.2267 0.5314 -0.0045 11.00000 0.05 1.13 Q4 1 0.3443 1.2857 0.0890 11.00000 0.05 0.70 Q5 1 0.3413 0.5421 0.0129 11.00000 0.05 0.68 Q6 1 0.5074 0.7841 0.2675 11.00000 0.05 0.65 Q7 1 -0.3206 0.9539 0.1353 11.00000 0.05 0.60 Q8 1 0.3231 0.5019 0.0128 11.00000 0.05 0.59 Q9 1 0.6146 0.0779 0.1373 11.00000 0.05 0.59 Q10 1 0.3189 1.2587 0.0700 11.00000 0.05 0.58 Q11 1 0.3405 1.2755 0.0652 11.00000 0.05 0.57 Q12 1 0.5306 1.0587 0.0414 11.00000 0.05 0.51 Q13 1 0.5725 1.1450 0.0609 11.00000 0.05 0.51 Q14 1 0.4710 0.1778 0.1446 11.00000 0.05 0.50 Q15 1 0.3784 1.1470 0.0133 11.00000 0.05 0.48 ; loop_ _geom_hbond_atom_site_label_D _geom_hbond_atom_site_label_H _geom_hbond_atom_site_label_A _geom_hbond_distance_DH _geom_hbond_distance_HA _geom_hbond_distance_DA _geom_hbond_angle_DHA _geom_hbond_site_symmetry_A _geom_hbond_publ_flag # # Hydrogen bonding scheme # ======== ======= ====== # # D H A D-H H...A D...A D-H...A symm publ # - - - --- ----- ----- ------- ---- ---- C12 H12 N1 0.93 2.59 2.910(7) 101 . yes C42 H42 N4 0.93 2.61 2.918(7) 100 . yes C43A H43A O5 0.93 2.46 3.197(8) 136 1_455 yes C14 H14 O8 0.93 2.48 3.114(6) 126 2_545 yes C15 H15 O8 0.93 2.60 3.174(7) 120 2_545 yes C15A H15A O4 0.93 2.49 3.356(7) 155 3_565 yes C35A H35A Cl1S 0.93 2.83 3.559(7) 136 1_565 yes C34 H34 O3 0.93 2.38 3.288(7) 165 1_655 yes #======================================================================= # END of the FIVE structure CIF file #======================================================================= #===END _database_code_depnum_ccdc_archive 'CCDC 930693'