Supplementary Material (ESI) for Dalton Transactions This journal is (c) The Royal Society of Chemistry 2001 data_global _journal_coden_Cambridge 186 _publ_requested_journal 'Dalton Transactions' loop_ _publ_author_name 'Maubert, Beatrice M.' 'McKee, Vickie' 'Nelson, Jane' 'Pal, Ibolya' 'Town, Raewyn' _publ_contact_author_name 'Prof Jane Nelson' _publ_contact_author_address ; Prof Jane Nelson School of Chemistry Queens University Belfast BT9 5AG UNITED KINGDOM ; data_'r3bmcr_Complex_1' _database_code_CSD 159484 _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C36 H73.50 Cl4 Cr N8 O27' _chemical_formula_weight 1244.33 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' 'Cr' 'Cr' 0.3209 0.6236 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting Monoclinic _symmetry_space_group_name_H-M P2(1)/n 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 14.321(3) _cell_length_b 14.050(3) _cell_length_c 27.431(5) _cell_angle_alpha 90.00 _cell_angle_beta 90.372(4) _cell_angle_gamma 90.00 _cell_volume 5519.5(17) _cell_formula_units_Z 4 _cell_measurement_temperature 150(2) _cell_measurement_reflns_used ? _cell_measurement_theta_min ? _cell_measurement_theta_max ? _exptl_crystal_description plate _exptl_crystal_colour yellow _exptl_crystal_size_max 0.16 _exptl_crystal_size_mid 0.06 _exptl_crystal_size_min 0.02 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.497 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 2614 _exptl_absorpt_coefficient_mu 0.492 _exptl_absorpt_correction_type none _exptl_absorpt_correction_T_min ? _exptl_absorpt_correction_T_max ? _exptl_absorpt_process_details ? _exptl_special_details ; ? ; _diffrn_ambient_temperature 150(2) _diffrn_radiation_wavelength 0.69230 _diffrn_radiation_type Synchrotron _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'CCD area detector' _diffrn_measurement_method 'phi and omega scans' _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 29246 _diffrn_reflns_av_R_equivalents 0.0785 _diffrn_reflns_av_sigmaI/netI 0.0971 _diffrn_reflns_limit_h_min -17 _diffrn_reflns_limit_h_max 13 _diffrn_reflns_limit_k_min -17 _diffrn_reflns_limit_k_max 16 _diffrn_reflns_limit_l_min -33 _diffrn_reflns_limit_l_max 33 _diffrn_reflns_theta_min 1.98 _diffrn_reflns_theta_max 25.00 _reflns_number_total 10467 _reflns_number_gt 5751 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'Bruker SMART' _computing_cell_refinement 'local programs' _computing_data_reduction 'Bruker SHELXTL' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'Bruker SHELXTL' _computing_publication_material 'Bruker SHELXTL' _refine_special_details ; Refinement of F^2^ against ALL reflections. The weighted R-factor wR and goodness of fit S are based on F^2^, conventional R-factors R are based on F, with F set to zero for negative F^2^. The threshold expression of F^2^ > 2sigma(F^2^) is used only for calculating R-factors(gt) etc. and is not relevant to the choice of reflections for refinement. R-factors based on F^2^ are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger. ; _refine_ls_structure_factor_coef Fsqd _refine_ls_matrix_type full _refine_ls_weighting_scheme calc _refine_ls_weighting_details 'calc w=1/[\s^2^(Fo^2^)+(0.2000P)^2^+0.0000P] 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 10467 _refine_ls_number_parameters 901 _refine_ls_number_restraints 1052 _refine_ls_R_factor_all 0.2048 _refine_ls_R_factor_gt 0.1412 _refine_ls_wR_factor_ref 0.4034 _refine_ls_wR_factor_gt 0.3779 _refine_ls_goodness_of_fit_ref 1.333 _refine_ls_restrained_S_all 1.382 _refine_ls_shift/su_max 0.243 _refine_ls_shift/su_mean 0.041 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 N1 N 0.3015(5) -0.3083(5) -0.1936(3) 0.0546(19) Uani 1 1 d . B . C1A C 0.2866(6) -0.2903(8) -0.2452(4) 0.070(3) Uani 1 1 d . . . H1A1 H 0.2241 -0.2617 -0.2502 0.050 Uiso 1 1 calc R . . H1A2 H 0.2883 -0.3514 -0.2632 0.050 Uiso 1 1 calc R . . C2A C 0.3616(6) -0.2230(8) -0.2655(4) 0.072(3) Uani 1 1 d . . . H2A1 H 0.3433 -0.2019 -0.2987 0.050 Uiso 1 1 calc R . . H2A2 H 0.3668 -0.1660 -0.2445 0.050 Uiso 1 1 calc R . . N3A N 0.4542(4) -0.2732(5) -0.2674(2) 0.0494(18) Uani 1 1 d . . . H3A1N H 0.4676 -0.2994 -0.2375 0.050 Uiso 1 1 calc R . . H3A2N H 0.4515 -0.3216 -0.2900 0.050 Uiso 1 1 calc R . . C3A C 0.5278(6) -0.2057(6) -0.2809(4) 0.055(2) Uani 1 1 d . . . H3A3 H 0.5382 -0.1608 -0.2536 0.050 Uiso 1 1 calc R . . H3A4 H 0.5069 -0.1684 -0.3095 0.050 Uiso 1 1 calc R . . C4A C 0.6187(6) -0.2548(6) -0.2927(3) 0.044(2) Uani 1 1 d . . . C5A C 0.6290(6) -0.3118(6) -0.3331(3) 0.053(2) Uani 1 1 d . . . H5A H 0.5768 -0.3241 -0.3537 0.050 Uiso 1 1 calc R . . C6A C 0.7162(7) -0.3518(6) -0.3440(3) 0.058(2) Uani 1 1 d . . . H6A H 0.7222 -0.3932 -0.3712 0.050 Uiso 1 1 calc R . . C7A C 0.7912(6) -0.3319(6) -0.3162(3) 0.048(2) Uani 1 1 d . . . H7A H 0.8505 -0.3572 -0.3244 0.050 Uiso 1 1 calc R . . C8A C 0.7823(5) -0.2758(6) -0.2763(3) 0.0436(19) Uani 1 1 d . . . C9A C 0.6965(5) -0.2366(5) -0.2639(3) 0.0393(18) Uani 1 1 d . . . H9A H 0.6912 -0.1975 -0.2357 0.050 Uiso 1 1 calc R . . C10A C 0.8679(6) -0.2507(7) -0.2458(3) 0.056(2) Uani 1 1 d . . . H10A H 0.9246 -0.2653 -0.2649 0.050 Uiso 1 1 calc R . . H10B H 0.8677 -0.1814 -0.2393 0.050 Uiso 1 1 calc R . . N4A N 0.8728(4) -0.3025(5) -0.1986(2) 0.0414(15) Uani 1 1 d . . . H4A1 H 0.8227 -0.2857 -0.1796 0.050 Uiso 1 1 calc R . . H4A2 H 0.8697 -0.3670 -0.2042 0.050 Uiso 1 1 calc R . . C11A C 0.9604(6) -0.2799(7) -0.1724(3) 0.057(2) Uani 1 1 d . . . H11A H 0.9556 -0.2157 -0.1578 0.050 Uiso 1 1 calc R . . H11B H 1.0128 -0.2793 -0.1958 0.050 Uiso 1 1 calc R . . C12A C 0.9799(5) -0.3523(6) -0.1328(3) 0.049(2) Uani 1 1 d . . . H12A H 0.9851 -0.4162 -0.1477 0.050 Uiso 1 1 calc R . . H12B H 1.0405 -0.3372 -0.1170 0.050 Uiso 1 1 calc R . . N2 N 0.9060(4) -0.3538(5) -0.0954(2) 0.0481(17) Uani 1 1 d . . . C1C C 0.2697(9) -0.2298(9) -0.1623(5) 0.097(4) Uani 1 1 d . . . H1C1 H 0.2846 -0.1687 -0.1785 0.050 Uiso 1 1 calc R A 1 H1C2 H 0.2009 -0.2336 -0.1593 0.050 Uiso 1 1 calc R A 1 C2C C 0.3102(11) -0.2288(11) -0.1135(5) 0.113(5) Uani 0.50 1 d P B 1 H2C1 H 0.3266 -0.2950 -0.1046 0.050 Uiso 0.50 1 calc PR B 1 H2C2 H 0.2616 -0.2073 -0.0905 0.050 Uiso 0.50 1 calc PR B 1 N3C N 0.4054(17) -0.161(2) -0.1047(8) 0.064(5) Uani 0.50 1 d PU B 1 H3C1 H 0.4505 -0.1777 -0.1269 0.050 Uiso 0.50 1 calc PR B 1 H3C2 H 0.3902 -0.0980 -0.1101 0.050 Uiso 0.50 1 calc PR B 1 C3C C 0.445(2) -0.172(3) -0.0517(11) 0.086(6) Uani 0.50 1 d PU B 1 H3C3 H 0.3984 -0.1514 -0.0277 0.050 Uiso 0.50 1 calc PR B 1 H3C4 H 0.4602 -0.2401 -0.0453 0.050 Uiso 0.50 1 calc PR B 1 C4C C 0.5349(9) -0.1113(11) -0.0464(6) 0.061(4) Uani 0.50 1 d PGU B 1 C5C C 0.5460(12) -0.0177(12) -0.0617(7) 0.084(5) Uani 0.50 1 d PGU B 1 H5C H 0.4985 0.0123 -0.0805 0.050 Uiso 0.50 1 calc PR B 1 C6C C 0.6268(13) 0.0320(9) -0.0494(6) 0.070(5) Uani 0.50 1 d PGU B 1 H6C H 0.6344 0.0960 -0.0599 0.050 Uiso 0.50 1 calc PR B 1 C7C C 0.6963(10) -0.0119(10) -0.0220(6) 0.068(5) Uani 0.50 1 d PGU B 1 H7C H 0.7515 0.0220 -0.0136 0.050 Uiso 0.50 1 calc PR B 1 C8C C 0.6852(9) -0.1056(11) -0.0067(6) 0.064(5) Uani 0.50 1 d PGU B 1 C9C C 0.6044(10) -0.1553(9) -0.0190(6) 0.059(4) Uani 0.50 1 d PGU B 1 H9C H 0.5968 -0.2193 -0.0086 0.050 Uiso 0.50 1 calc PR B 1 C10C C 0.7592(16) -0.1521(18) 0.0297(9) 0.065(5) Uani 0.50 1 d PU B 1 H10C H 0.7786 -0.1045 0.0544 0.050 Uiso 0.50 1 calc PR B 1 H10D H 0.7301 -0.2064 0.0469 0.050 Uiso 0.50 1 calc PR B 1 N4C N 0.8459(16) -0.1873(18) 0.0015(8) 0.065(5) Uani 0.50 1 d PU B 1 H4C1 H 0.8725 -0.1365 -0.0144 0.050 Uiso 0.50 1 calc PR B 1 H4C2 H 0.8892 -0.2103 0.0234 0.050 Uiso 0.50 1 calc PR B 1 C11C C 0.8254(19) -0.258(2) -0.0321(8) 0.056(5) Uani 0.50 1 d PU B 1 H11C H 0.7729 -0.2375 -0.0534 0.050 Uiso 0.50 1 calc PR B 1 H11D H 0.8076 -0.3172 -0.0153 0.050 Uiso 0.50 1 calc PR B 1 C12C C 0.9151(7) -0.2736(9) -0.0630(4) 0.072(3) Uani 0.50 1 d PU B 1 H12C H 0.9279 -0.2156 -0.0824 0.050 Uiso 0.50 1 calc PR B 1 H12D H 0.9689 -0.2841 -0.0408 0.050 Uiso 0.50 1 calc PR B 1 C2C' C 0.3102(11) -0.2288(11) -0.1135(5) 0.113(5) Uani 0.50 1 d PU B 2 H2C3 H 0.2661 -0.2024 -0.0894 0.050 Uiso 0.50 1 calc PR B 2 H2C4 H 0.3297 -0.2933 -0.1031 0.050 Uiso 0.50 1 calc PR B 2 N3C' N 0.385(2) -0.171(3) -0.1196(11) 0.095(7) Uani 0.50 1 d PU B 2 H3C5 H 0.3683 -0.1141 -0.1339 0.050 Uiso 0.50 1 calc PR B 2 H3C6 H 0.4311 -0.1997 -0.1374 0.050 Uiso 0.50 1 calc PR B 2 C3C' C 0.413(3) -0.158(3) -0.0650(15) 0.109(8) Uani 0.50 1 d PU B 2 H3C7 H 0.3608 -0.1291 -0.0471 0.050 Uiso 0.50 1 calc PR B 2 H3C8 H 0.4258 -0.2215 -0.0505 0.050 Uiso 0.50 1 calc PR B 2 C4C' C 0.4957(13) -0.0989(14) -0.0588(8) 0.090(6) Uani 0.50 1 d PGU B 2 C5C' C 0.5035(12) -0.0054(15) -0.0748(7) 0.092(6) Uani 0.50 1 d PGU B 2 H5C' H 0.4532 0.0236 -0.0920 0.050 Uiso 0.50 1 calc PR B 2 C6C' C 0.5847(13) 0.0458(12) -0.0655(7) 0.076(5) Uani 0.50 1 d PGU B 2 H6C' H 0.5900 0.1097 -0.0765 0.050 Uiso 0.50 1 calc PR B 2 C7C' C 0.6583(10) 0.0034(14) -0.0404(7) 0.081(6) Uani 0.50 1 d PGU B 2 H7C' H 0.7139 0.0384 -0.0341 0.050 Uiso 0.50 1 calc PR B 2 C8C' C 0.6506(12) -0.0901(14) -0.0244(7) 0.083(5) Uani 0.50 1 d PGU B 2 C9C' C 0.5693(15) -0.1413(12) -0.0336(7) 0.095(6) Uani 0.50 1 d PGU B 2 H9C' H 0.5640 -0.2052 -0.0227 0.050 Uiso 0.50 1 calc PR B 2 C10' C 0.729(2) -0.133(2) 0.0088(10) 0.088(6) Uani 0.50 1 d PU B 2 H10'E H 0.7408 -0.0872 0.0356 0.050 Uiso 0.50 1 calc PR B 2 H10'F H 0.7037 -0.1917 0.0238 0.050 Uiso 0.50 1 calc PR B 2 N4C' N 0.8255(17) -0.158(2) -0.0159(8) 0.076(5) Uani 0.50 1 d PU B 2 H4C3 H 0.8477 -0.1055 -0.0322 0.050 Uiso 0.50 1 calc PR B 2 H4C4 H 0.8684 -0.1741 0.0078 0.050 Uiso 0.50 1 calc PR B 2 C11' C 0.814(2) -0.238(2) -0.0503(7) 0.058(6) Uani 0.50 1 d PU B 2 H11'E H 0.7811 -0.2164 -0.0801 0.050 Uiso 0.50 1 calc PR B 2 H11'F H 0.7775 -0.2896 -0.0351 0.050 Uiso 0.50 1 calc PR B 2 C12' C 0.9151(7) -0.2736(9) -0.0630(4) 0.072(3) Uani 0.50 1 d P B 2 H12'E H 0.9509 -0.2221 -0.0789 0.050 Uiso 0.50 1 calc PR B 2 H12'F H 0.9487 -0.2927 -0.0329 0.050 Uiso 0.50 1 calc PR B 2 C1B C 0.2451(6) -0.3957(8) -0.1796(3) 0.067(3) Uani 1 1 d . . . H1B1 H 0.2379 -0.3964 -0.1437 0.050 Uiso 1 1 calc R B . H1B2 H 0.1819 -0.3902 -0.1942 0.050 Uiso 1 1 calc R . . C2B C 0.2845(6) -0.4836(8) -0.1943(4) 0.063(3) Uani 1 1 d . B . H2B1 H 0.2996 -0.4802 -0.2294 0.050 Uiso 1 1 calc R . . H2B2 H 0.2376 -0.5346 -0.1899 0.050 Uiso 1 1 calc R . . N3B N 0.3710(4) -0.5092(5) -0.1663(3) 0.0513(18) Uani 1 1 d . . . H3B1 H 0.4175 -0.4670 -0.1744 0.050 Uiso 1 1 calc R B . H3B2 H 0.3594 -0.5020 -0.1335 0.050 Uiso 1 1 calc R . . C3B C 0.4055(7) -0.6070(7) -0.1747(4) 0.067(3) Uani 1 1 d . B . H3B3 H 0.3528 -0.6524 -0.1721 0.050 Uiso 1 1 calc R . . H3B4 H 0.4308 -0.6117 -0.2082 0.050 Uiso 1 1 calc R . . C4B C 0.4782(7) -0.6329(7) -0.1396(4) 0.069(3) Uani 1 1 d . . . C5B C 0.4547(18) -0.702(2) -0.1095(10) 0.078(7) Uani 0.50 1 d PU B 1 H5B H 0.3950 -0.7313 -0.1106 0.050 Uiso 0.50 1 calc PR B 1 C6B C 0.5232(15) -0.7287(19) -0.0758(9) 0.075(5) Uani 0.50 1 d PU B 1 H6B H 0.5063 -0.7701 -0.0499 0.050 Uiso 0.50 1 calc PR B 1 C7B C 0.6109(16) -0.6990(18) -0.0785(8) 0.064(5) Uani 0.50 1 d PU B 1 H7B H 0.6559 -0.7227 -0.0560 0.050 Uiso 0.50 1 calc PR B 1 C5B' C 0.4509(15) -0.6544(18) -0.0871(8) 0.063(6) Uani 0.50 1 d PU B 2 H5B' H 0.3866 -0.6605 -0.0793 0.050 Uiso 0.50 1 calc PR B 2 C6B' C 0.5187(12) -0.6657(17) -0.0498(8) 0.065(5) Uani 0.50 1 d PU B 2 H6B' H 0.4995 -0.6838 -0.0180 0.050 Uiso 0.50 1 calc PR B 2 C7B' C 0.6106(13) -0.6509(16) -0.0586(7) 0.051(5) Uani 0.50 1 d PU B 2 C8B C 0.6381(6) -0.6341(6) -0.1136(4) 0.059(2) Uani 1 1 d . . . C9B C 0.5721(6) -0.6121(6) -0.1469(3) 0.050(2) Uani 1 1 d . B . H9B H 0.5901 -0.5814 -0.1762 0.050 Uiso 1 1 calc R . . C10B C 0.7392(6) -0.6115(6) -0.1204(3) 0.052(2) Uani 1 1 d . B . H10E H 0.7763 -0.6652 -0.1071 0.050 Uiso 1 1 calc R . . H10F H 0.7514 -0.6084 -0.1558 0.050 Uiso 1 1 calc R . . N4B N 0.7736(4) -0.5248(5) -0.0984(2) 0.0440(16) Uani 1 1 d . . . H4B1 H 0.7462 -0.5167 -0.0685 0.050 Uiso 1 1 calc R B . H4B2 H 0.7569 -0.4739 -0.1177 0.050 Uiso 1 1 calc R . . C11B C 0.8782(6) -0.5258(7) -0.0921(3) 0.053(2) Uani 1 1 d . B . H11E H 0.8959 -0.5827 -0.0729 0.050 Uiso 1 1 calc R . . H11F H 0.9073 -0.5318 -0.1246 0.050 Uiso 1 1 calc R . . C12B C 0.9157(6) -0.4409(7) -0.0678(3) 0.053(2) Uani 1 1 d . B . H12E H 0.8835 -0.4329 -0.0362 0.050 Uiso 1 1 calc R . . H12F H 0.9827 -0.4514 -0.0607 0.050 Uiso 1 1 calc R . . Cr Cr 0.57367(9) -0.34091(10) -0.14900(5) 0.0486(5) Uani 1 1 d . . . O1 O 0.5213(4) -0.3984(4) -0.1939(2) 0.0569(16) Uani 1 1 d U . . O2 O 0.6799(5) -0.3654(5) -0.1488(2) 0.0674(18) Uani 1 1 d U . . O3 O 0.5272(5) -0.3724(5) -0.0967(2) 0.080(2) Uani 1 1 d U . . O4 O 0.5519(5) -0.2276(5) -0.1592(3) 0.078(2) Uani 1 1 d U . . Cl1 Cl 0.86429(18) 0.6331(3) 0.09646(9) 0.0782(9) Uani 1 1 d D . . O11 O 0.9047(5) 0.5710(6) 0.1316(3) 0.092(2) Uani 1 1 d DU . . O12 O 0.7785(6) 0.6496(13) 0.1071(5) 0.217(9) Uani 1 1 d DU . . O13 O 0.9134(14) 0.7144(10) 0.1058(8) 0.302(14) Uani 1 1 d DU . . O14 O 0.8902(14) 0.6175(17) 0.0509(3) 0.268(11) Uani 1 1 d DU . . Cl2 Cl 0.9399(2) 0.0216(2) 0.16950(13) 0.0698(9) Uani 0.80 1 d PD C 1 O21 O 1.0375(6) 0.0246(8) 0.1626(5) 0.111(4) Uani 0.80 1 d PDU C 1 O22 O 0.9127(7) 0.0735(8) 0.1282(3) 0.139(4) Uani 0.80 1 d PDU C 1 O23 O 0.9093(12) 0.0798(11) 0.2044(5) 0.171(6) Uani 0.80 1 d PDU C 1 O24 O 0.9102(10) -0.0673(8) 0.1716(8) 0.166(7) Uani 0.80 1 d PDU C 1 Cl2' Cl 0.8805(8) -0.0008(8) 0.1474(4) 0.049(2) Uiso 0.20 1 d PD D 2 O21' O 0.7870(13) 0.001(2) 0.1317(14) 0.095 Uiso 0.20 1 d PD D 2 O22' O 0.9127(7) 0.0735(8) 0.1282(3) 0.139(4) Uani 0.20 1 d PDU D 2 O23' O 0.884(4) -0.002(4) 0.1958(6) 0.26(6) Uiso 0.20 1 d PD D 2 O24' O 0.917(3) -0.0867(15) 0.1336(14) 0.083(13) Uiso 0.20 1 d PD D 2 Cl3 Cl 0.4375(3) 0.0499(3) -0.21108(14) 0.1035(13) Uani 0.50 1 d PD E 1 O31 O 0.4670(8) 0.0484(10) -0.2593(3) 0.151(4) Uani 0.50 1 d PDU E 1 O32 O 0.3645(16) -0.008(2) -0.2089(7) 0.165(16) Uani 0.50 1 d PDU E 1 O33 O 0.4257(16) 0.1340(16) -0.1928(13) 0.22(2) Uani 0.50 1 d PDU E 1 O34 O 0.5115(14) 0.0078(18) -0.1865(11) 0.23(3) Uani 0.50 1 d PDU E 1 Cl3' Cl 0.4375(3) 0.0499(3) -0.21108(14) 0.1035(13) Uani 0.50 1 d PD F 2 O31' O 0.4670(8) 0.0484(10) -0.2593(3) 0.151(4) Uani 0.50 1 d PDU F 2 O32' O 0.3465(10) 0.040(3) -0.2117(12) 0.30(3) Uani 0.50 1 d PDU F 2 O33' O 0.469(2) 0.120(2) -0.1840(10) 0.21(2) Uani 0.50 1 d PDU F 2 O34' O 0.489(3) -0.0268(18) -0.1940(8) 0.25(3) Uani 0.50 1 d PDU F 2 Cl4 Cl 0.8286(5) 0.2632(8) 0.0062(3) 0.093(2) Uani 0.50 1 d PD G 1 O41 O 0.761(2) 0.202(2) -0.0094(13) 0.26(3) Uani 0.50 1 d PDU G 1 O42 O 0.8592(14) 0.233(3) 0.0488(6) 0.25(3) Uani 0.50 1 d PDU G 1 O43 O 0.8005(19) 0.3550(13) 0.0096(9) 0.26(2) Uani 0.50 1 d PDU G 1 O44 O 0.9002(17) 0.2710(17) -0.0276(10) 0.189(14) Uani 0.50 1 d PDU G 1 Cl4' Cl 0.8623(4) 0.1945(6) -0.0015(2) 0.0786(17) Uani 0.50 1 d PD H 2 O41' O 0.841(2) 0.1202(17) 0.0299(9) 0.213(17) Uani 0.50 1 d PDU H 2 O42' O 0.875(2) 0.266(2) 0.0298(12) 0.29(3) Uani 0.50 1 d PDU H 2 O43' O 0.9362(12) 0.1778(19) -0.0281(8) 0.155(11) Uani 0.50 1 d PDU H 2 O44' O 0.789(2) 0.2122(18) -0.0323(11) 0.20(2) Uani 0.50 1 d PDU H 2 O1W O 0.6540(5) -0.5030(5) -0.2467(2) 0.0684(18) Uani 1 1 d U . . O2W O 0.8348(5) -0.4893(5) -0.2185(3) 0.077(2) Uani 1 1 d U . . O3W O 0.6658(5) -0.4314(7) -0.0265(3) 0.096(3) Uani 1 1 d U . . O4W O 0.3653(7) -0.4637(9) -0.0628(4) 0.131(4) Uani 1 1 d U . . O5W O 1.0910(11) 0.0282(11) 0.0647(5) 0.086(5) Uani 0.50 1 d PU . . O6W O 0.7421(15) -0.1476(16) -0.1490(8) 0.100(7) Uani 0.50 1 d PU . . O7W O 0.7105(11) 0.0049(12) 0.1060(5) 0.083(5) Uani 0.50 1 d PU . . O8W O 0.6381(12) -0.0673(11) -0.1764(5) 0.095(5) Uani 0.50 1 d PU . . O9W O 1.0264(19) 0.1360(13) -0.0537(7) 0.132(8) Uani 0.50 1 d PU . . O10W O 0.809(2) -0.110(2) -0.1521(9) 0.158(12) Uani 0.50 1 d PU . . 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 N1 0.036(4) 0.070(5) 0.057(4) 0.016(4) 0.017(3) 0.018(3) C1A 0.030(5) 0.101(8) 0.080(7) 0.046(6) 0.016(4) 0.020(5) C2A 0.046(5) 0.083(7) 0.087(7) 0.021(6) 0.012(5) 0.014(5) N3A 0.038(4) 0.060(4) 0.050(4) 0.018(3) 0.008(3) 0.013(3) C3A 0.039(5) 0.055(5) 0.072(6) 0.023(5) 0.013(4) -0.001(4) C4A 0.044(5) 0.039(4) 0.050(5) 0.007(4) 0.023(4) -0.003(4) C5A 0.055(5) 0.045(5) 0.059(5) 0.015(4) 0.006(4) -0.014(4) C6A 0.072(7) 0.049(5) 0.054(5) 0.000(4) 0.027(5) -0.014(5) C7A 0.038(5) 0.056(5) 0.050(5) 0.013(4) 0.023(4) 0.004(4) C8A 0.038(4) 0.045(5) 0.048(5) 0.019(4) 0.017(4) -0.002(3) C9A 0.045(5) 0.034(4) 0.039(4) 0.012(3) 0.016(4) 0.004(3) C10A 0.041(5) 0.052(5) 0.074(6) 0.011(5) 0.010(4) -0.006(4) N4A 0.029(3) 0.043(4) 0.052(4) 0.010(3) 0.008(3) -0.002(3) C11A 0.045(5) 0.058(6) 0.068(6) 0.002(5) 0.002(4) -0.012(4) C12A 0.025(4) 0.065(6) 0.056(5) -0.010(4) 0.001(3) -0.010(4) N2 0.026(3) 0.068(5) 0.051(4) -0.011(4) 0.001(3) -0.002(3) C1C 0.071(8) 0.092(9) 0.128(11) 0.012(8) 0.040(8) 0.033(7) C2C 0.137(11) 0.111(10) 0.091(9) -0.042(8) 0.057(8) -0.026(8) N3C 0.081(11) 0.080(11) 0.032(9) -0.017(8) 0.009(7) 0.037(9) C3C 0.088(12) 0.130(14) 0.040(11) -0.008(12) -0.003(10) 0.022(11) C4C 0.066(10) 0.096(10) 0.020(9) -0.006(8) 0.010(7) 0.042(8) C5C 0.108(14) 0.094(10) 0.050(12) -0.015(10) -0.009(11) 0.042(10) C6C 0.098(15) 0.078(11) 0.035(11) -0.002(9) 0.006(10) 0.043(9) C7C 0.082(12) 0.075(10) 0.047(12) -0.006(9) 0.015(8) 0.032(8) C8C 0.067(10) 0.093(11) 0.032(11) 0.011(9) 0.012(8) 0.027(8) C9C 0.054(9) 0.088(11) 0.036(10) -0.002(8) 0.024(7) 0.026(7) C10C 0.064(10) 0.080(12) 0.051(12) -0.002(9) 0.006(7) 0.026(9) N4C 0.064(10) 0.084(13) 0.048(11) -0.001(8) -0.007(8) 0.021(8) C11C 0.040(10) 0.093(14) 0.034(13) -0.006(9) -0.002(9) 0.010(9) C12C 0.045(5) 0.101(8) 0.071(6) -0.024(6) 0.011(5) -0.011(5) C2C' 0.137(11) 0.111(10) 0.091(9) -0.042(8) 0.057(8) -0.026(8) N3C' 0.103(15) 0.083(13) 0.100(17) -0.055(13) 0.009(12) -0.007(10) C3C' 0.117(14) 0.126(15) 0.083(15) -0.028(15) 0.034(11) -0.010(13) C4C' 0.107(13) 0.109(12) 0.053(13) -0.045(10) 0.029(10) -0.006(10) C5C' 0.092(14) 0.115(12) 0.069(14) -0.039(11) 0.014(11) 0.004(11) C6C' 0.076(13) 0.107(13) 0.045(12) -0.023(10) 0.021(10) 0.005(9) C7C' 0.077(13) 0.101(12) 0.064(15) -0.001(11) 0.037(10) 0.019(11) C8C' 0.086(10) 0.104(11) 0.060(13) -0.010(10) 0.054(9) 0.024(9) C9C' 0.116(14) 0.098(13) 0.071(16) -0.029(11) 0.043(11) 0.008(11) C10' 0.113(13) 0.100(14) 0.051(15) -0.002(10) 0.046(9) 0.026(12) N4C' 0.075(10) 0.103(15) 0.050(12) -0.022(10) 0.008(9) -0.003(10) C11' 0.050(11) 0.109(15) 0.015(11) -0.025(10) 0.010(10) -0.018(11) C12' 0.045(5) 0.101(8) 0.071(6) -0.024(6) 0.011(5) -0.011(5) C1B 0.030(5) 0.115(9) 0.054(5) 0.028(6) 0.010(4) -0.002(5) C2B 0.029(4) 0.093(8) 0.066(6) 0.030(6) -0.012(4) -0.014(5) N3B 0.032(4) 0.065(5) 0.057(4) 0.013(4) 0.002(3) -0.018(3) C3B 0.058(6) 0.061(6) 0.083(7) 0.012(5) -0.010(5) -0.012(5) C4B 0.053(6) 0.053(6) 0.101(8) 0.036(6) -0.006(5) -0.007(5) C5B 0.053(10) 0.088(18) 0.091(17) 0.010(13) 0.005(10) -0.016(12) C6B 0.060(9) 0.096(14) 0.071(12) 0.037(11) 0.023(9) -0.006(10) C7B 0.057(8) 0.091(16) 0.045(12) 0.019(10) 0.007(9) -0.004(11) C5B' 0.040(8) 0.090(15) 0.060(12) 0.040(11) 0.009(8) -0.023(11) C6B' 0.040(7) 0.101(14) 0.053(10) 0.042(10) 0.011(7) -0.002(10) C7B' 0.040(7) 0.071(14) 0.043(11) 0.011(9) 0.015(8) -0.007(9) C8B 0.044(5) 0.050(5) 0.083(7) 0.022(5) 0.013(5) -0.006(4) C9B 0.053(5) 0.039(5) 0.057(5) 0.007(4) 0.007(4) -0.006(4) C10B 0.049(5) 0.046(5) 0.061(5) 0.005(4) 0.020(4) 0.008(4) N4B 0.036(4) 0.057(4) 0.039(3) 0.011(3) 0.019(3) 0.009(3) C11B 0.039(5) 0.070(6) 0.049(5) 0.006(4) 0.017(4) 0.008(4) C12B 0.037(5) 0.080(7) 0.043(5) -0.001(5) -0.002(4) 0.005(4) Cr 0.0463(8) 0.0497(9) 0.0500(8) 0.0097(6) 0.0124(6) -0.0007(6) O1 0.035(3) 0.070(4) 0.065(4) 0.007(3) 0.004(3) -0.001(3) O2 0.064(4) 0.080(5) 0.057(4) 0.012(3) -0.010(3) -0.015(3) O3 0.077(5) 0.092(5) 0.070(4) 0.020(4) 0.023(4) -0.009(4) O4 0.092(5) 0.060(4) 0.082(5) 0.005(4) 0.039(4) 0.003(4) Cl1 0.0479(14) 0.139(3) 0.0476(13) 0.0189(15) 0.0080(10) 0.0063(15) O11 0.078(5) 0.096(6) 0.103(6) 0.003(5) 0.009(4) 0.007(4) O12 0.060(6) 0.39(2) 0.196(13) 0.168(15) 0.001(7) 0.018(9) O13 0.26(2) 0.202(17) 0.44(3) 0.21(2) -0.07(2) -0.107(16) O14 0.31(2) 0.44(3) 0.055(7) -0.015(11) 0.021(9) 0.08(2) Cl2 0.075(2) 0.062(2) 0.073(2) 0.0156(16) 0.0135(17) 0.0070(17) O21 0.065(7) 0.118(9) 0.152(10) 0.001(8) 0.016(7) 0.007(6) O22 0.140(9) 0.172(11) 0.106(7) 0.029(7) 0.006(6) 0.080(8) O23 0.160(15) 0.177(17) 0.178(15) 0.010(13) 0.052(12) -0.015(12) O24 0.113(11) 0.101(11) 0.28(2) 0.063(14) 0.007(13) -0.019(9) O22' 0.140(9) 0.172(11) 0.106(7) 0.029(7) 0.006(6) 0.080(8) Cl3 0.098(3) 0.120(3) 0.092(2) 0.032(2) -0.039(2) -0.056(2) O31 0.132(9) 0.202(13) 0.118(9) 0.024(8) 0.002(7) 0.001(8) O32 0.21(3) 0.20(3) 0.088(14) -0.026(16) 0.055(17) -0.18(2) O33 0.043(14) 0.23(4) 0.40(6) -0.13(3) -0.03(2) -0.028(16) O34 0.22(3) 0.17(3) 0.31(5) 0.16(3) -0.17(3) -0.15(3) Cl3' 0.098(3) 0.120(3) 0.092(2) 0.032(2) -0.039(2) -0.056(2) O31' 0.132(9) 0.202(13) 0.118(9) 0.024(8) 0.002(7) 0.001(8) O32' 0.10(2) 0.43(6) 0.35(5) 0.19(5) -0.15(3) -0.09(3) O33' 0.14(3) 0.22(4) 0.28(4) -0.14(3) 0.12(3) -0.11(2) O34' 0.53(7) 0.14(2) 0.081(16) -0.058(17) -0.08(3) 0.10(4) Cl4 0.057(4) 0.138(7) 0.085(5) 0.034(5) -0.016(4) -0.003(5) O41 0.16(3) 0.32(5) 0.30(4) 0.18(4) -0.17(3) -0.16(3) O42 0.036(11) 0.63(7) 0.071(13) 0.13(3) -0.028(11) -0.07(2) O43 0.17(3) 0.50(6) 0.12(2) 0.04(3) 0.08(2) -0.14(4) O44 0.19(3) 0.14(2) 0.23(3) 0.14(2) 0.12(2) 0.029(19) Cl4' 0.045(3) 0.116(5) 0.076(4) -0.018(4) -0.008(3) -0.018(3) O41' 0.28(4) 0.24(4) 0.12(2) 0.02(2) 0.03(2) 0.09(3) O42' 0.11(3) 0.54(7) 0.23(4) -0.25(5) 0.08(3) -0.05(4) O43' 0.112(17) 0.20(3) 0.15(2) -0.112(19) 0.032(15) -0.041(17) O44' 0.33(5) 0.103(18) 0.17(3) -0.04(2) -0.12(3) 0.05(3) O1W 0.075(5) 0.060(4) 0.071(4) 0.008(3) 0.004(3) -0.012(3) O2W 0.081(5) 0.052(4) 0.099(5) 0.014(4) -0.013(4) -0.009(3) O3W 0.072(5) 0.136(7) 0.081(5) -0.002(5) 0.015(4) -0.012(5) O4W 0.116(7) 0.173(10) 0.104(7) 0.047(7) -0.012(6) -0.062(7) O5W 0.093(11) 0.080(10) 0.086(10) -0.023(8) 0.038(8) -0.022(8) O6W 0.098(15) 0.113(15) 0.089(13) -0.028(10) 0.008(11) -0.025(12) O7W 0.086(10) 0.106(12) 0.058(8) -0.016(8) -0.010(7) 0.048(9) O8W 0.118(13) 0.089(11) 0.078(10) -0.019(8) 0.048(9) -0.048(10) O9W 0.21(2) 0.088(13) 0.094(13) -0.016(10) -0.023(14) -0.061(14) O10W 0.20(3) 0.17(2) 0.103(15) -0.081(17) -0.053(18) 0.13(2) _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 N1 C1A 1.451(12) . ? N1 C1C 1.473(14) . ? N1 C1B 1.521(12) . ? C1A C2A 1.538(13) . ? C2A N3A 1.503(11) . ? N3A C3A 1.466(10) . ? C3A C4A 1.511(11) . ? C4A C5A 1.377(12) . ? C4A C9A 1.385(12) . ? C5A C6A 1.402(13) . ? C6A C7A 1.343(13) . ? C7A C8A 1.355(12) . ? C8A C9A 1.391(11) . ? C8A C10A 1.521(12) . ? C10A N4A 1.488(11) . ? N4A C11A 1.474(11) . ? C11A C12A 1.513(12) . ? C12A N2 1.480(10) . ? N2 C12C 1.441(12) . ? N2 C12B 1.444(11) . ? C1C C2C 1.455(19) . ? C2C N3C 1.68(3) . ? N3C C3C 1.57(3) . ? C3C C4C 1.55(4) . ? C4C C5C 1.3900 . ? C4C C9C 1.3900 . ? C5C C6C 1.3900 . ? C6C C7C 1.3900 . ? C7C C8C 1.3900 . ? C8C C9C 1.3900 . ? C8C C10C 1.59(2) . ? C10C N4C 1.55(3) . ? N4C C11C 1.38(4) . ? C11C C12C 1.56(3) . ? N3C' C3C' 1.56(4) . ? C3C' C4C' 1.45(4) . ? C4C' C5C' 1.3900 . ? C4C' C9C' 1.3900 . ? C5C' C6C' 1.3900 . ? C6C' C7C' 1.3900 . ? C7C' C8C' 1.3900 . ? C8C' C9C' 1.3900 . ? C8C' C10' 1.56(3) . ? C10' N4C' 1.59(3) . ? N4C' C11' 1.47(3) . ? C1B C2B 1.416(14) . ? C2B N3B 1.498(10) . ? N3B C3B 1.479(12) . ? C3B C4B 1.461(13) . ? C4B C5B 1.32(3) . ? C4B C9B 1.392(13) . ? C4B C5B' 1.52(2) . ? C5B C6B 1.39(3) . ? C6B C7B 1.33(3) . ? C7B C8B 1.38(2) . ? C5B' C6B' 1.42(3) . ? C6B' C7B' 1.36(3) . ? C7B' C8B 1.58(2) . ? C8B C9B 1.346(13) . ? C8B C10B 1.495(12) . ? C10B N4B 1.445(11) . ? N4B C11B 1.506(10) . ? C11B C12B 1.468(13) . ? Cr O2 1.560(7) . ? Cr O3 1.645(6) . ? Cr O1 1.648(6) . ? Cr O4 1.646(7) . ? Cl1 O12 1.285(9) . ? Cl1 O14 1.325(9) . ? Cl1 O13 1.365(12) . ? Cl1 O11 1.420(8) . ? Cl2 O24 1.321(10) . ? Cl2 O23 1.335(12) . ? Cl2 O22 1.402(8) . ? Cl2 O21 1.412(9) . ? Cl2' O23' 1.327(15) . ? Cl2' O24' 1.369(15) . ? Cl2' O21' 1.403(15) . ? O21' O7W 1.30(2) . ? Cl3 O33 1.294(14) . ? Cl3 O32 1.324(11) . ? Cl3 O34 1.385(13) . ? Cl3 O31 1.392(8) . ? Cl4 O42 1.315(13) . ? Cl4 O43 1.354(15) . ? Cl4 O41 1.357(13) . ? Cl4 O44 1.391(13) . ? Cl4' O43' 1.312(13) . ? Cl4' O42' 1.338(14) . ? Cl4' O44' 1.364(14) . ? Cl4' O41' 1.386(14) . ? O43' O9W 1.59(3) . ? O6W O10W 1.10(4) . ? 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 C1A N1 C1C 113.3(8) . . ? C1A N1 C1B 108.2(8) . . ? C1C N1 C1B 106.9(8) . . ? N1 C1A C2A 111.2(9) . . ? N3A C2A C1A 110.0(8) . . ? C3A N3A C2A 110.0(7) . . ? N3A C3A C4A 112.4(7) . . ? C5A C4A C9A 118.5(7) . . ? C5A C4A C3A 122.3(9) . . ? C9A C4A C3A 119.0(8) . . ? C4A C5A C6A 120.3(9) . . ? C7A C6A C5A 120.3(9) . . ? C6A C7A C8A 120.1(8) . . ? C7A C8A C9A 121.0(8) . . ? C7A C8A C10A 119.9(7) . . ? C9A C8A C10A 119.0(8) . . ? C4A C9A C8A 119.7(8) . . ? N4A C10A C8A 113.5(6) . . ? C11A N4A C10A 110.7(6) . . ? N4A C11A C12A 110.9(7) . . ? N2 C12A C11A 112.3(7) . . ? C12C N2 C12B 109.4(7) . . ? C12C N2 C12A 110.7(7) . . ? C12B N2 C12A 108.0(7) . . ? C2C C1C N1 114.9(10) . . ? C1C C2C N3C 117.1(13) . . ? C3C N3C C2C 111(2) . . ? C4C C3C N3C 109(2) . . ? C5C C4C C9C 120.0 . . ? C5C C4C C3C 126.4(15) . . ? C9C C4C C3C 113.2(15) . . ? C4C C5C C6C 120.0 . . ? C5C C6C C7C 120.0 . . ? C8C C7C C6C 120.0 . . ? C7C C8C C9C 120.0 . . ? C7C C8C C10C 120.0(13) . . ? C9C C8C C10C 119.6(13) . . ? C8C C9C C4C 120.0 . . ? N4C C10C C8C 110.5(17) . . ? C11C N4C C10C 113(2) . . ? N4C C11C C12C 107(2) . . ? N2 C12C C11C 112.1(14) . . ? C4C' C3C' N3C' 113(3) . . ? C5C' C4C' C9C' 120.0 . . ? C5C' C4C' C3C' 125(2) . . ? C9C' C4C' C3C' 115(2) . . ? C6C' C5C' C4C' 120.0 . . ? C5C' C6C' C7C' 120.0 . . ? C8C' C7C' C6C' 120.0 . . ? C9C' C8C' C7C' 120.0 . . ? C9C' C8C' C10' 120.2(17) . . ? C7C' C8C' C10' 119.4(17) . . ? C8C' C9C' C4C' 120.0 . . ? N4C' C10' C8C' 117.5(19) . . ? C11' N4C' C10' 110(2) . . ? C2B C1B N1 114.8(7) . . ? C1B C2B N3B 113.2(8) . . ? C3B N3B C2B 114.7(7) . . ? C4B C3B N3B 111.4(8) . . ? C5B C4B C9B 119.7(14) . . ? C5B C4B C3B 114.4(14) . . ? C9B C4B C3B 122.5(9) . . ? C5B C4B C5B' 36.3(12) . . ? C9B C4B C5B' 115.6(11) . . ? C3B C4B C5B' 119.1(11) . . ? C4B C5B C6B 116(2) . . ? C7B C6B C5B 123(2) . . ? C6B C7B C8B 121(2) . . ? C6B' C5B' C4B 121.8(16) . . ? C7B' C6B' C5B' 121.0(17) . . ? C6B' C7B' C8B 116.3(16) . . ? C9B C8B C7B 115.1(12) . . ? C9B C8B C10B 122.9(8) . . ? C7B C8B C10B 120.2(12) . . ? C9B C8B C7B' 120.2(10) . . ? C7B C8B C7B' 33.3(10) . . ? C10B C8B C7B' 113.5(10) . . ? C8B C9B C4B 121.9(8) . . ? N4B C10B C8B 117.1(7) . . ? C10B N4B C11B 112.1(6) . . ? C12B C11B N4B 113.9(7) . . ? N2 C12B C11B 114.7(7) . . ? O2 Cr O3 109.8(4) . . ? O2 Cr O1 109.4(3) . . ? O3 Cr O1 109.5(3) . . ? O2 Cr O4 113.4(4) . . ? O3 Cr O4 109.3(4) . . ? O1 Cr O4 105.2(4) . . ? O12 Cl1 O14 121.2(11) . . ? O12 Cl1 O13 107.4(13) . . ? O14 Cl1 O13 99.7(12) . . ? O12 Cl1 O11 110.0(6) . . ? O14 Cl1 O11 115.0(9) . . ? O13 Cl1 O11 100.3(8) . . ? O24 Cl2 O23 116.2(11) . . ? O24 Cl2 O22 116.0(10) . . ? O23 Cl2 O22 99.8(9) . . ? O24 Cl2 O21 110.7(8) . . ? O23 Cl2 O21 114.1(9) . . ? O22 Cl2 O21 98.4(7) . . ? O23' Cl2' O24' 105(2) . . ? O23' Cl2' O21' 110(2) . . ? O24' Cl2' O21' 107.3(18) . . ? O7W O21' Cl2' 165(3) . . ? O33 Cl3 O32 115.7(16) . . ? O33 Cl3 O34 107.7(16) . . ? O32 Cl3 O34 108.6(15) . . ? O33 Cl3 O31 115.0(18) . . ? O32 Cl3 O31 106.2(9) . . ? O34 Cl3 O31 102.7(15) . . ? O42 Cl4 O43 109.9(19) . . ? O42 Cl4 O41 108.0(16) . . ? O43 Cl4 O41 114.5(18) . . ? O42 Cl4 O44 112.0(14) . . ? O43 Cl4 O44 101.0(12) . . ? O41 Cl4 O44 111.4(19) . . ? O43' Cl4' O42' 112.6(15) . . ? O43' Cl4' O44' 107.9(16) . . ? O42' Cl4' O44' 111.1(19) . . ? O43' Cl4' O41' 113.0(16) . . ? O42' Cl4' O41' 101.5(17) . . ? O44' Cl4' O41' 110.7(18) . . ? Cl4' O43' O9W 167(3) . . ? 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 N3A H3A1N O1 0.92 1.99 2.841(9) 153.8 . N3A H3A2N O24 0.92 1.97 2.864(16) 162.9 4 N4A H4A2 O2W 0.92 1.83 2.734(9) 166.7 . N4A H4A1 O6W 0.92 2.41 3.18(2) 141.4 . N4A H4A1 O10W 0.92 2.60 3.14(2) 118.1 . N3C H3C1 O4 0.92 1.84 2.75(3) 166.7 . N3C H3C2 O7W 0.92 1.95 2.75(3) 143.9 3_655 N4C H4C2 O14 0.92 2.54 3.12(3) 122.0 1_545 N4C H4C1 O5W 0.92 2.12 3.02(3) 166.0 3_755 N3C' H3C6 O4 0.92 1.88 2.75(4) 158.3 . N3C' H3C5 O7W 0.92 2.05 2.73(4) 129.3 3_655 N4C' H4C3 O5W 0.92 1.66 2.56(3) 165.8 3_755 N4C' H4C4 O9W 0.92 2.03 2.86(3) 150.2 3_755 N3B H3B1 O1 0.92 1.85 2.766(8) 171.1 . N3B H3B2 O4W 0.92 2.02 2.912(13) 164.2 . N4B H4B2 O2 0.92 2.06 2.950(9) 161.4 . N4B H4B1 O3W 0.92 2.03 2.835(10) 145.9 . _diffrn_measured_fraction_theta_max 0.995 _diffrn_reflns_theta_full 25.00 _diffrn_measured_fraction_theta_full 0.995 _refine_diff_density_max 1.067 _refine_diff_density_min -1.035 _refine_diff_density_rms 0.131 data_'jnse_Complex_2' _database_code_CSD 159485 _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C36 H77 Cl4 N8 O28.50 Se' _chemical_formula_weight 1298.82 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' 'Se' 'Se' -0.0929 2.2259 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting Monoclinic _symmetry_space_group_name_H-M P2(1)/n 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 14.4758(10) _cell_length_b 13.9235(9) _cell_length_c 27.5511(18) _cell_angle_alpha 90.00 _cell_angle_beta 90.3820(10) _cell_angle_gamma 90.00 _cell_volume 5552.9(6) _cell_formula_units_Z 4 _cell_measurement_temperature 150(2) _cell_measurement_reflns_used 7653 _cell_measurement_theta_min 2.16 _cell_measurement_theta_max 26.22 _exptl_crystal_description 'irregular block' _exptl_crystal_colour colourless _exptl_crystal_size_max 0.36 _exptl_crystal_size_mid 0.30 _exptl_crystal_size_min 0.22 _exptl_crystal_density_meas not_measured _exptl_crystal_density_diffrn 1.554 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 2716 _exptl_absorpt_coefficient_mu 0.963 _exptl_absorpt_correction_type empirical _exptl_absorpt_correction_T_min 0.548718 _exptl_absorpt_correction_T_max 0.928075 _exptl_absorpt_process_details ? _exptl_special_details ; ? ; _diffrn_ambient_temperature 150(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'CCD area detector' _diffrn_measurement_method 'phi and omega scans' _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 53095 _diffrn_reflns_av_R_equivalents 0.0586 _diffrn_reflns_av_sigmaI/netI 0.0443 _diffrn_reflns_limit_h_min -17 _diffrn_reflns_limit_h_max 17 _diffrn_reflns_limit_k_min -16 _diffrn_reflns_limit_k_max 16 _diffrn_reflns_limit_l_min -32 _diffrn_reflns_limit_l_max 32 _diffrn_reflns_theta_min 1.58 _diffrn_reflns_theta_max 25.00 _reflns_number_total 9787 _reflns_number_gt 7054 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'Bruker SMART' _computing_cell_refinement 'Bruker SMART' _computing_data_reduction 'Bruker SHELXTL' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'Bruker SHELXTL' _computing_publication_material 'Bruker SHELXTL' _refine_special_details ; Refinement of F^2^ against ALL reflections. The weighted R-factor wR and goodness of fit S are based on F^2^, conventional R-factors R are based on F, with F set to zero for negative F^2^. The threshold expression of F^2^ > 2sigma(F^2^) is used only for calculating R-factors(gt) etc. and is not relevant to the choice of reflections for refinement. R-factors based on F^2^ are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger. ; _refine_ls_structure_factor_coef Fsqd _refine_ls_matrix_type full _refine_ls_weighting_scheme calc _refine_ls_weighting_details 'calc w=1/[\s^2^(Fo^2^)+(0.1441P)^2^+7.8372P] 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 9787 _refine_ls_number_parameters 907 _refine_ls_number_restraints 418 _refine_ls_R_factor_all 0.0983 _refine_ls_R_factor_gt 0.0742 _refine_ls_wR_factor_ref 0.2303 _refine_ls_wR_factor_gt 0.2071 _refine_ls_goodness_of_fit_ref 1.057 _refine_ls_restrained_S_all 1.109 _refine_ls_shift/su_max 1.195 _refine_ls_shift/su_mean 0.034 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 N2 N 0.0976(3) -0.8502(4) 0.40570(18) 0.0430(11) Uani 1 1 d U D . C12A C 0.0901(4) -0.9404(5) 0.4326(2) 0.0483(14) Uani 1 1 d U . . H12A H 0.0242 -0.9525 0.4398 0.058 Uiso 1 1 calc R . . H12B H 0.1233 -0.9336 0.4640 0.058 Uiso 1 1 calc R . . C11A C 0.1281(4) -1.0250(4) 0.4061(2) 0.0458(14) Uani 1 1 d U . . H11A H 0.1006 -1.0273 0.3731 0.055 Uiso 1 1 calc R . . H11B H 0.1102 -1.0845 0.4233 0.055 Uiso 1 1 calc R . . N4A N 0.2319(3) -1.0215(3) 0.40200(17) 0.0376(10) Uani 1 1 d U . . H4A1 H 0.2485 -0.9696 0.3833 0.045 Uiso 1 1 calc R . . H4A2 H 0.2575 -1.0136 0.4324 0.045 Uiso 1 1 calc R . . C10A C 0.2684(4) -1.1111(4) 0.3797(2) 0.0495(15) Uani 1 1 d U . . H10A H 0.2591 -1.1080 0.3441 0.059 Uiso 1 1 calc R . . H10B H 0.2328 -1.1666 0.3920 0.059 Uiso 1 1 calc R . . C8A C 0.3688(4) -1.1268(4) 0.3904(2) 0.0440(13) Uani 1 1 d U . . C7A C 0.3951(5) -1.1557(5) 0.4371(3) 0.064(2) Uani 1 1 d U . . H7A H 0.3497 -1.1650 0.4614 0.077 Uiso 1 1 calc R . . C6A C 0.4870(5) -1.1706(6) 0.4479(3) 0.078(3) Uani 1 1 d U . . H6A H 0.5048 -1.1879 0.4800 0.093 Uiso 1 1 calc R . . C5A C 0.5541(5) -1.1606(5) 0.4124(3) 0.065(2) Uani 1 1 d U . . H5A H 0.6169 -1.1743 0.4198 0.078 Uiso 1 1 calc R . . C4A C 0.5293(4) -1.1308(4) 0.3662(2) 0.0430(13) Uani 1 1 d U . . C9A C 0.4359(4) -1.1139(4) 0.3560(2) 0.0420(13) Uani 1 1 d U . . H9A H 0.4184 -1.0930 0.3244 0.050 Uiso 1 1 calc R . . C3A C 0.6011(5) -1.1101(4) 0.3292(2) 0.0547(16) Uani 1 1 d U . . H3A1 H 0.5746 -1.1169 0.2962 0.066 Uiso 1 1 calc R . . H3A2 H 0.6528 -1.1562 0.3326 0.066 Uiso 1 1 calc R . . N3A N 0.6357(3) -1.0089(3) 0.33681(17) 0.0422(11) Uani 1 1 d U . . H3A1N H 0.5894 -0.9665 0.3288 0.051 Uiso 1 1 calc R . . H3A2N H 0.6498 -1.0004 0.3691 0.051 Uiso 1 1 calc R . . C2A C 0.7195(4) -0.9864(5) 0.3072(3) 0.0617(17) Uani 1 1 d U . . H2A1 H 0.7668 -1.0367 0.3125 0.074 Uiso 1 1 calc R . . H2A2 H 0.7026 -0.9864 0.2723 0.074 Uiso 1 1 calc R . . C1A C 0.7584(4) -0.8915(6) 0.3206(3) 0.0625(18) Uani 1 1 d U . . H1A1 H 0.8203 -0.8856 0.3059 0.075 Uiso 1 1 calc R A 1 H1A2 H 0.7666 -0.8895 0.3563 0.075 Uiso 1 1 calc R A 1 C12B C 0.0254(4) -0.8462(4) 0.3681(2) 0.0439(13) Uani 1 1 d U . . H12C H -0.0341 -0.8296 0.3834 0.053 Uiso 1 1 calc R . . H12D H 0.0188 -0.9105 0.3531 0.053 Uiso 1 1 calc R . . C11B C 0.0460(4) -0.7739(4) 0.3289(2) 0.0534(16) Uani 1 1 d U . . H11C H 0.0526 -0.7094 0.3436 0.064 Uiso 1 1 calc R . . H11D H -0.0062 -0.7717 0.3056 0.064 Uiso 1 1 calc R . . N4B N 0.1335(3) -0.7990(3) 0.30226(16) 0.0373(10) Uani 1 1 d U . . H4B1 H 0.1840 -0.7832 0.3211 0.045 Uiso 1 1 calc R . . H4B2 H 0.1352 -0.8641 0.2965 0.045 Uiso 1 1 calc R . . C10B C 0.1374(4) -0.7454(4) 0.2548(2) 0.0419(13) Uani 1 1 d U . . H10C H 0.0806 -0.7593 0.2359 0.050 Uiso 1 1 calc R . . H10D H 0.1387 -0.6756 0.2616 0.050 Uiso 1 1 calc R . . C8B C 0.2194(4) -0.7711(3) 0.22500(19) 0.0348(11) Uani 1 1 d U . . C7B C 0.2103(4) -0.8279(4) 0.1840(2) 0.0394(12) Uani 1 1 d U . . H7B H 0.1518 -0.8543 0.1757 0.047 Uiso 1 1 calc R . . C6B C 0.2859(4) -0.8464(4) 0.1551(2) 0.0436(13) Uani 1 1 d U . . H6B H 0.2789 -0.8856 0.1271 0.052 Uiso 1 1 calc R . . C5B C 0.3711(4) -0.8087(4) 0.1663(2) 0.0387(12) Uani 1 1 d U . . H5B H 0.4224 -0.8209 0.1459 0.046 Uiso 1 1 calc R . . C4B C 0.3819(3) -0.7525(3) 0.20776(19) 0.0327(11) Uani 1 1 d U . . C9B C 0.3056(4) -0.7343(3) 0.23703(18) 0.0327(11) Uani 1 1 d U . . H9B H 0.3127 -0.6963 0.2655 0.039 Uiso 1 1 calc R . . C3B C 0.4728(4) -0.7041(4) 0.2195(2) 0.0414(13) Uani 1 1 d U . . H3BC H 0.4929 -0.6664 0.1910 0.050 Uiso 1 1 calc R . . H3BD H 0.4638 -0.6589 0.2468 0.050 Uiso 1 1 calc R . . N3B N 0.5472(3) -0.7741(3) 0.23285(17) 0.0420(11) Uani 1 1 d U . . H3B1 H 0.5474 -0.8240 0.2110 0.050 Uiso 1 1 calc R . . H3B2 H 0.5358 -0.7990 0.2632 0.050 Uiso 1 1 calc R . . C2B C 0.6396(4) -0.7251(6) 0.2329(3) 0.073(2) Uani 1 1 d U . . H2C H 0.6363 -0.6656 0.2524 0.088 Uiso 1 1 calc R . . H2D H 0.6561 -0.7073 0.1992 0.088 Uiso 1 1 calc R . . C1B C 0.7139(4) -0.7914(6) 0.2540(3) 0.073(2) Uani 1 1 d U . . H1C1 H 0.7116 -0.8540 0.2370 0.087 Uiso 1 1 calc R B 1 H1D2 H 0.7755 -0.7627 0.2483 0.087 Uiso 1 1 calc R B 1 C12C C 0.0868(4) -0.7694(6) 0.4391(3) 0.068(2) Uani 1 1 d U . . H12E H 0.0397 -0.7856 0.4637 0.082 Uiso 1 1 calc R C 1 H12F H 0.0649 -0.7124 0.4209 0.082 Uiso 1 1 calc R C 1 C11C C 0.1765(7) -0.7464(8) 0.4640(5) 0.0980(4) Uani 0.50 1 d PU D 1 H11E H 0.1942 -0.7995 0.4861 0.118 Uiso 0.50 1 calc PR D 1 H11F H 0.2259 -0.7386 0.4396 0.118 Uiso 0.50 1 calc PR D 1 N4C N 0.1663(7) -0.6612(8) 0.4905(5) 0.076(3) Uani 0.50 1 d PU D 1 H4C1 H 0.1183 -0.6691 0.5119 0.092 Uiso 0.50 1 calc PR D 1 H4C2 H 0.1499 -0.6130 0.4693 0.092 Uiso 0.50 1 calc PR D 1 C10C C 0.2498(10) -0.6296(10) 0.5185(6) 0.064(3) Uani 0.50 1 d PU D 1 H10E H 0.2309 -0.5835 0.5439 0.077 Uiso 0.50 1 calc PR D 1 H10F H 0.2779 -0.6860 0.5348 0.077 Uiso 0.50 1 calc PR D 1 C8C C 0.3185(6) -0.5844(6) 0.4872(4) 0.064(3) Uani 0.50 1 d PGU D 1 C7C C 0.3128(8) -0.4902(6) 0.4708(4) 0.093(5) Uani 0.50 1 d PGU D 1 H7C H 0.2595 -0.4528 0.4775 0.112 Uiso 0.50 1 calc PR D 1 C6C C 0.3850(10) -0.4506(5) 0.4445(4) 0.115(7) Uani 0.50 1 d PGU D 1 H6C H 0.3811 -0.3862 0.4333 0.138 Uiso 0.50 1 calc PR D 1 C5C C 0.4630(8) -0.5052(5) 0.4346(3) 0.093(5) Uani 0.50 1 d PGU D 1 H5C H 0.5124 -0.4782 0.4166 0.111 Uiso 0.50 1 calc PR D 1 C4C C 0.4688(6) -0.5995(5) 0.4510(2) 0.053(3) Uani 0.50 1 d PGU D 1 C9C C 0.3965(6) -0.6390(4) 0.4773(3) 0.045(2) Uani 0.50 1 d PGU D 1 H9C H 0.4005 -0.7034 0.4885 0.054 Uiso 0.50 1 calc PR D 1 C3C C 0.5524(6) -0.6432(7) 0.4436(3) 0.062(3) Uani 0.50 1 d PGU D 1 H3CE H 0.5481 -0.7089 0.4571 0.075 Uiso 0.50 1 calc PR D 1 H3CF H 0.5989 -0.6083 0.4633 0.075 Uiso 0.50 1 calc PR D 1 N3C N 0.5902(10) -0.6521(10) 0.3938(4) 0.055(3) Uani 0.50 1 d PU D 1 H3C1 H 0.6041 -0.5916 0.3825 0.066 Uiso 0.50 1 calc PR D 1 H3C2 H 0.5449 -0.6770 0.3738 0.066 Uiso 0.50 1 calc PR D 1 C2C C 0.6760(15) -0.7147(16) 0.3896(6) 0.070(4) Uani 0.50 1 d PU D 1 H2C1 H 0.7227 -0.6926 0.4135 0.084 Uiso 0.50 1 calc PR D 1 H2C2 H 0.6595 -0.7818 0.3978 0.084 Uiso 0.50 1 calc PR D 1 C1C C 0.7178(14) -0.7124(18) 0.3394(8) 0.070(4) Uani 0.50 1 d PU D 1 H1E H 0.7851 -0.7019 0.3431 0.084 Uiso 0.50 1 calc PR D 1 H1F H 0.6922 -0.6561 0.3220 0.084 Uiso 0.50 1 calc PR D 1 N1 N 0.7020(3) -0.8070(4) 0.3055(2) 0.0587(14) Uani 0.50 1 d PU D 1 C11' C 0.1755(13) -0.7460(15) 0.4658(10) 0.103(6) Uani 0.50 1 d PU D 2 H11G H 0.1573 -0.7186 0.4975 0.123 Uiso 0.50 1 calc PR D 2 H11H H 0.2059 -0.8081 0.4728 0.123 Uiso 0.50 1 calc PR D 2 N4C' N 0.2338(10) -0.6946(11) 0.4502(5) 0.077(3) Uani 0.50 1 d PU D 2 H4C5 H 0.2049 -0.6439 0.4350 0.092 Uiso 0.50 1 calc PR D 2 H4C6 H 0.2652 -0.7281 0.4267 0.092 Uiso 0.50 1 calc PR D 2 C10' C 0.3083(15) -0.6515(17) 0.4870(8) 0.109(6) Uani 0.50 1 d PU D 2 H107 H 0.2761 -0.6156 0.5129 0.131 Uiso 0.50 1 calc PR D 2 H108 H 0.3429 -0.7048 0.5024 0.131 Uiso 0.50 1 calc PR D 2 C8C' C 0.3720(7) -0.5886(7) 0.4631(4) 0.070(4) Uani 0.50 1 d PGU D 2 C7C' C 0.3501(5) -0.4936(7) 0.4527(4) 0.043(3) Uani 0.50 1 d PGU D 2 H7C' H 0.2909 -0.4690 0.4608 0.052 Uiso 0.50 1 calc PR D 2 C6C' C 0.4147(6) -0.4346(6) 0.4305(4) 0.047(3) Uani 0.50 1 d PGU D 2 H6C' H 0.3997 -0.3696 0.4234 0.056 Uiso 0.50 1 calc PR D 2 C5C' C 0.5012(6) -0.4705(8) 0.4187(4) 0.057(3) Uani 0.50 1 d PGU D 2 H5C' H 0.5454 -0.4302 0.4035 0.069 Uiso 0.50 1 calc PR D 2 C4C' C 0.5232(6) -0.5656(8) 0.4291(4) 0.080(4) Uani 0.50 1 d PGU D 2 C9C' C 0.4586(8) -0.6246(6) 0.4513(5) 0.085(5) Uani 0.50 1 d PGU D 2 H9C' H 0.4736 -0.6895 0.4584 0.102 Uiso 0.50 1 calc PR D 2 C3C' C 0.6186(15) -0.601(2) 0.4183(9) 0.132(7) Uani 0.50 1 d PU D 2 H3CG H 0.6611 -0.5454 0.4186 0.159 Uiso 0.50 1 calc PR D 2 H3CH H 0.6381 -0.6444 0.4450 0.159 Uiso 0.50 1 calc PR D 2 N3C' N 0.6297(9) -0.6508(11) 0.3735(6) 0.066(4) Uani 0.50 1 d PU D 2 H3C3 H 0.6307 -0.6067 0.3486 0.080 Uiso 0.50 1 calc PR D 2 H3C4 H 0.5795 -0.6902 0.3686 0.080 Uiso 0.50 1 calc PR D 2 C2' C 0.7145(12) -0.7093(15) 0.3715(11) 0.076(6) Uani 0.50 1 d PU D 2 H2G H 0.7634 -0.6757 0.3902 0.091 Uiso 0.50 1 calc PR D 2 H2H H 0.7024 -0.7711 0.3880 0.091 Uiso 0.50 1 calc PR D 2 C1' C 0.7501(10) -0.7300(14) 0.3234(8) 0.066(4) Uani 0.50 1 d PU D 2 H1'1 H 0.7418 -0.6736 0.3019 0.080 Uiso 0.50 1 calc PR D 2 H1'2 H 0.8169 -0.7452 0.3253 0.080 Uiso 0.50 1 calc PR D 2 N1' N 0.7020(3) -0.8070(4) 0.3055(2) 0.0587(14) Uani 0.50 1 d PU D 2 Se Se 0.42836(3) -0.83728(3) 0.354239(18) 0.0311(2) Uani 1 1 d . . . O1 O 0.4801(3) -0.8980(3) 0.31071(13) 0.0399(9) Uani 1 1 d . . . O2 O 0.3180(3) -0.8585(3) 0.35277(15) 0.0484(10) Uani 1 1 d . . . O3 O 0.4732(3) -0.8665(3) 0.40687(13) 0.0451(9) Uani 1 1 d . . . O4 O 0.4500(3) -0.7241(3) 0.34303(15) 0.0515(11) Uani 1 1 d . . . Cl1 Cl 0.87084(11) -1.13162(15) 0.40425(6) 0.0613(7) Uani 0.524(7) 1 d PD E 1 O11 O 0.9144(6) -1.0749(6) 0.3678(3) 0.037(2) Uani 0.524(7) 1 d PD E 1 O12 O 0.9199(11) -1.1118(15) 0.4453(4) 0.171(11) Uani 0.524(7) 1 d PD E 1 O13 O 0.7826(8) -1.0957(17) 0.4108(7) 0.146(9) Uani 0.524(7) 1 d PD E 1 O14 O 0.8689(18) -1.2207(8) 0.3886(6) 0.169(12) Uani 0.524(7) 1 d PD E 1 Cl1' Cl 0.87084(11) -1.13162(15) 0.40425(6) 0.0613(7) Uani 0.48 1 d PD E 2 O11' O 0.878(2) -1.1571(17) 0.4530(4) 0.217(16) Uani 0.476(7) 1 d PDU E 2 O12' O 0.8860(18) -1.0461(11) 0.3869(12) 0.30(2) Uani 0.476(7) 1 d PDU E 2 O13' O 0.7825(8) -1.1646(14) 0.3868(6) 0.099(6) Uani 0.476(7) 1 d PDU E 2 O14' O 0.9304(11) -1.2036(14) 0.3881(8) 0.135(8) Uani 0.476(7) 1 d PDU E 2 Cl2 Cl 0.9439(3) -0.52465(17) 0.32872(9) 0.0417(9) Uani 0.634(9) 1 d PD . . O21 O 0.9167(4) -0.5778(4) 0.36985(19) 0.0761(15) Uani 1 1 d D . . O22 O 0.9125(5) -0.4258(5) 0.3377(4) 0.176(5) Uani 1 1 d D . . O23 O 0.9165(6) -0.5653(9) 0.2884(3) 0.176(5) Uani 1 1 d D . . O24 O 1.0410(4) -0.5213(5) 0.3337(3) 0.064(2) Uani 0.634(9) 1 d PD . . Cl2' Cl 0.8913(6) -0.5056(5) 0.3412(3) 0.063(2) Uani 0.366(9) 1 d P K . O24' O 0.7923(11) -0.5055(12) 0.3463(10) 0.135(10) Uani 0.366(9) 1 d P . . Cl3 Cl -0.17737(16) -0.76223(19) 0.49415(9) 0.0571(9) Uani 0.672(5) 1 d PD F 1 O31 O -0.2068(10) -0.8555(8) 0.4886(5) 0.138(5) Uani 0.672(5) 1 d PD F 1 O32 O -0.2604(9) -0.7153(12) 0.5020(7) 0.217(12) Uani 0.672(5) 1 d PD F 1 O33 O -0.1161(9) -0.7644(9) 0.5333(4) 0.152(6) Uani 0.672(5) 1 d PD F 1 O34 O -0.1319(4) -0.7307(7) 0.4557(2) 0.152(4) Uani 0.672(5) 1 d PD F 1 Cl3' Cl -0.1379(3) -0.6818(3) 0.49611(18) 0.0483(16) Uani 0.328(5) 1 d PD F 2 O31' O -0.1616(10) -0.5923(8) 0.4756(5) 0.064(4) Uani 0.328(5) 1 d PD F 2 O32' O -0.2077(13) -0.7121(9) 0.5278(6) 0.078(7) Uani 0.328(5) 1 d PD F 2 O33' O -0.0552(9) -0.6701(11) 0.5253(6) 0.078(5) Uani 0.328(5) 1 d PD F 2 O34' O -0.1319(4) -0.7307(7) 0.4557(2) 0.152(4) Uani 0.33 1 d PD F 2 Cl4 Cl 0.55995(15) -0.44420(17) 0.28750(8) 0.0852(7) Uani 1 1 d D . . O41 O 0.5533(9) -0.3638(7) 0.3094(4) 0.204(6) Uani 1 1 d D . . O42 O 0.5335(5) -0.4362(8) 0.2385(2) 0.147(4) Uani 1 1 d D . . O43 O 0.4842(8) -0.5057(7) 0.3066(4) 0.190(5) Uani 1 1 d D . . O44 O 0.6367(7) -0.4982(8) 0.2893(3) 0.189(5) Uani 1 1 d D . . O1W O 0.3471(3) -1.0017(3) 0.25491(14) 0.0467(10) Uani 1 1 d . . . O2W O 0.3361(3) -0.9245(4) 0.47504(15) 0.0582(12) Uani 1 1 d . . . O3W O 0.6355(3) -0.9544(4) 0.43779(16) 0.0636(13) Uani 1 1 d . . . O4W O 0.1670(3) -0.9897(3) 0.28101(18) 0.0608(12) Uani 1 1 d . . . O5W O 0.0239(6) -0.6331(6) 0.5576(3) 0.055(2) Uani 0.50 1 d P G 1 O6WA O 0.0717(14) -0.5372(14) 0.4420(7) 0.082(5) Uiso 0.33 1 d P H 1 O6WB O 0.1347(10) -0.5313(10) 0.4278(5) 0.053(3) Uiso 0.33 1 d P I 2 O6WC O 0.0855(10) -0.5067(10) 0.4240(5) 0.046(3) Uiso 0.33 1 d P J 3 O7W O 0.7110(8) -0.4879(8) 0.3945(5) 0.094(4) Uani 0.50 1 d P K 3 O8W O -0.1338(13) -0.5122(13) 0.4729(6) 0.140(6) Uani 0.50 1 d P L 3 O9W O 0.2670(7) -0.6383(6) 0.3507(3) 0.055(2) Uani 0.50 1 d P M 3 O10W O 0.3587(9) -0.5635(9) 0.3239(5) 0.096(4) Uani 0.50 1 d P N 1 O11W O 0.1748(9) -0.5859(9) 0.3406(4) 0.094(4) Uani 0.50 1 d P O 1 O12W O -0.2075(10) -0.9319(13) 0.4795(6) 0.120(5) Uani 0.50 1 d P P 3 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 N2 0.026(2) 0.057(3) 0.047(3) -0.002(2) 0.0052(19) -0.004(2) C12A 0.031(3) 0.080(4) 0.035(3) 0.009(3) 0.000(2) -0.013(3) C11A 0.034(3) 0.052(3) 0.052(3) 0.017(3) -0.017(2) -0.016(2) N4A 0.033(2) 0.037(2) 0.043(3) 0.0086(19) -0.0138(19) -0.0106(18) C10A 0.050(3) 0.036(3) 0.062(4) 0.005(3) -0.022(3) -0.008(2) C8A 0.048(3) 0.029(3) 0.055(3) 0.007(2) -0.016(3) -0.004(2) C7A 0.042(3) 0.086(5) 0.065(4) 0.044(4) -0.006(3) -0.002(3) C6A 0.051(4) 0.116(7) 0.067(5) 0.063(5) -0.005(3) 0.002(4) C5A 0.042(3) 0.081(5) 0.073(4) 0.041(4) -0.003(3) 0.006(3) C4A 0.053(3) 0.032(3) 0.045(3) 0.005(2) -0.005(3) 0.006(2) C9A 0.065(3) 0.024(2) 0.037(3) -0.002(2) -0.013(3) 0.005(2) C3A 0.078(4) 0.041(3) 0.044(3) 0.003(3) 0.013(3) 0.018(3) N3A 0.039(2) 0.050(3) 0.037(3) 0.012(2) 0.006(2) 0.012(2) C2A 0.047(4) 0.081(4) 0.057(4) 0.033(4) 0.017(3) 0.018(3) C1A 0.030(3) 0.096(4) 0.061(4) 0.041(4) -0.010(3) -0.001(3) C12B 0.035(3) 0.058(4) 0.039(3) 0.004(2) 0.007(2) 0.002(3) C11B 0.053(4) 0.045(3) 0.062(4) 0.012(3) 0.017(3) 0.019(3) N4B 0.037(2) 0.035(2) 0.040(3) 0.0081(19) 0.0021(19) 0.0083(19) C10B 0.046(3) 0.033(3) 0.047(3) 0.014(2) 0.001(2) 0.009(2) C8B 0.037(3) 0.027(2) 0.040(3) 0.011(2) -0.003(2) 0.005(2) C7B 0.037(3) 0.036(3) 0.045(3) 0.004(2) -0.015(2) -0.002(2) C6B 0.052(3) 0.038(3) 0.041(3) -0.005(2) -0.013(3) 0.003(2) C5B 0.040(3) 0.034(3) 0.043(3) -0.001(2) -0.003(2) 0.010(2) C4B 0.035(3) 0.026(2) 0.037(3) 0.008(2) -0.008(2) 0.000(2) C9B 0.045(3) 0.025(2) 0.029(3) 0.003(2) -0.007(2) 0.001(2) C3B 0.037(3) 0.037(3) 0.050(3) 0.011(2) -0.009(2) -0.004(2) N3B 0.032(2) 0.051(3) 0.043(3) 0.019(2) -0.011(2) -0.007(2) C2B 0.034(3) 0.096(6) 0.089(5) 0.056(5) -0.023(3) -0.023(3) C1B 0.032(3) 0.108(6) 0.077(4) 0.056(4) -0.011(3) -0.012(3) C12C 0.032(3) 0.082(5) 0.089(5) -0.038(4) -0.010(3) 0.009(3) C11C 0.0457(7) 0.0713(8) 0.1765(5) -0.057(4) -0.035(6) 0.002(7) N4C 0.037(4) 0.096(6) 0.095(7) -0.080(5) -0.052(5) 0.050(4) C10C 0.057(7) 0.066(8) 0.069(9) -0.055(6) -0.041(5) 0.034(5) C8C 0.087(7) 0.032(6) 0.071(10) -0.024(6) -0.055(6) 0.012(5) C7C 0.159(15) 0.040(6) 0.079(13) -0.041(6) -0.086(9) 0.040(8) C6C 0.24(2) 0.025(7) 0.077(15) 0.007(8) -0.087(13) -0.012(8) C5C 0.207(17) 0.041(7) 0.029(8) 0.010(6) -0.036(10) -0.037(8) C4C 0.094(8) 0.044(6) 0.022(7) 0.006(5) -0.027(6) -0.024(6) C9C 0.057(6) 0.030(5) 0.048(8) -0.010(5) -0.035(5) -0.008(5) C3C 0.090(8) 0.077(9) 0.019(5) 0.010(5) -0.017(5) -0.042(6) N3C 0.078(8) 0.063(7) 0.023(5) 0.002(5) -0.014(5) -0.051(6) C2C 0.071(11) 0.094(12) 0.044(7) 0.024(6) -0.020(7) -0.042(8) C1C 0.039(10) 0.094(9) 0.076(9) 0.019(7) -0.009(8) -0.040(8) N1 0.040(3) 0.068(3) 0.067(3) 0.029(3) -0.026(2) -0.022(2) C11' 0.044(8) 0.074(11) 0.190(19) -0.037(11) -0.035(10) -0.007(8) N4C' 0.076(8) 0.080(8) 0.075(8) -0.010(7) -0.004(7) -0.009(6) C10' 0.107(11) 0.121(13) 0.098(13) 0.048(11) -0.072(9) -0.049(10) C8C' 0.083(8) 0.059(7) 0.067(10) 0.003(7) -0.049(7) -0.015(6) C7C' 0.031(5) 0.069(7) 0.029(7) -0.020(6) -0.003(5) 0.001(5) C6C' 0.050(6) 0.064(8) 0.027(7) 0.000(6) -0.005(5) -0.003(5) C5C' 0.049(6) 0.086(8) 0.036(7) -0.018(7) 0.000(5) -0.005(6) C4C' 0.074(7) 0.085(9) 0.078(10) -0.042(8) -0.048(6) 0.031(6) C9C' 0.090(9) 0.060(8) 0.105(15) -0.016(8) -0.077(8) 0.015(6) C3C' 0.088(9) 0.184(17) 0.124(15) -0.090(13) -0.047(9) 0.068(10) N3C' 0.038(7) 0.070(9) 0.091(11) -0.034(8) -0.023(6) 0.001(6) C2' 0.038(9) 0.064(10) 0.127(14) -0.036(11) -0.026(10) 0.006(8) C1' 0.016(7) 0.065(7) 0.117(11) 0.000(8) -0.010(6) -0.002(6) N1' 0.040(3) 0.068(3) 0.067(3) 0.029(3) -0.026(2) -0.022(2) Se 0.0320(3) 0.0310(3) 0.0302(3) 0.0026(2) -0.0038(2) -0.0013(2) O1 0.041(2) 0.042(2) 0.037(2) 0.0021(16) -0.0044(16) 0.0037(16) O2 0.030(2) 0.064(3) 0.051(2) 0.017(2) 0.0005(17) -0.0007(18) O3 0.050(2) 0.054(2) 0.031(2) 0.0088(17) -0.0089(17) 0.0015(19) O4 0.073(3) 0.032(2) 0.049(2) 0.0041(17) -0.025(2) -0.0073(19) Cl1 0.0446(10) 0.0914(16) 0.0479(10) 0.0084(9) -0.0046(7) 0.0148(9) O11 0.031(4) 0.049(5) 0.031(4) -0.004(3) 0.006(3) -0.002(4) O12 0.168(15) 0.30(3) 0.043(7) 0.054(10) -0.023(8) -0.175(18) O13 0.048(7) 0.26(2) 0.134(15) 0.113(15) 0.037(8) 0.065(11) O14 0.27(3) 0.103(12) 0.133(14) 0.062(11) -0.085(18) -0.100(17) Cl1' 0.0446(10) 0.0914(16) 0.0479(10) 0.0084(9) -0.0046(7) 0.0148(9) O11' 0.39(4) 0.24(2) 0.024(7) 0.028(11) 0.008(14) 0.22(3) O12' 0.26(3) 0.043(10) 0.59(6) 0.10(2) -0.29(4) -0.047(14) O13' 0.037(7) 0.153(17) 0.108(13) 0.022(10) 0.012(7) 0.009(8) O14' 0.077(11) 0.152(18) 0.175(19) -0.032(15) -0.012(11) 0.053(11) Cl2 0.041(2) 0.0399(13) 0.0444(14) 0.0067(10) -0.0019(12) 0.0015(11) O21 0.090(4) 0.068(3) 0.070(3) 0.014(3) -0.002(3) -0.018(3) O22 0.098(5) 0.066(5) 0.365(15) 0.081(7) 0.060(7) 0.021(4) O23 0.113(6) 0.339(15) 0.076(5) -0.011(7) -0.029(4) 0.031(8) O24 0.051(4) 0.067(5) 0.073(5) 0.005(4) -0.003(4) -0.012(4) Cl2' 0.056(5) 0.058(3) 0.075(4) 0.007(3) -0.024(3) -0.019(3) O24' 0.051(9) 0.068(10) 0.28(3) 0.022(14) -0.060(14) -0.011(8) Cl3 0.0414(13) 0.0675(18) 0.0623(16) 0.0137(12) 0.0001(11) -0.0060(11) O31 0.164(12) 0.091(8) 0.157(12) -0.042(8) -0.057(9) 0.005(8) O32 0.088(9) 0.245(19) 0.32(2) 0.209(19) 0.084(12) 0.067(11) O33 0.189(13) 0.140(10) 0.125(9) 0.089(8) -0.101(9) -0.094(10) O34 0.062(4) 0.323(13) 0.070(5) 0.037(6) 0.018(3) -0.029(6) Cl3' 0.031(2) 0.054(3) 0.060(3) -0.014(2) 0.0011(19) 0.0093(19) O31' 0.080(10) 0.041(8) 0.071(10) 0.005(7) 0.010(8) 0.010(7) O32' 0.116(16) 0.037(8) 0.083(13) -0.033(8) 0.088(13) -0.012(9) O33' 0.057(9) 0.074(11) 0.102(13) -0.032(9) -0.021(9) 0.026(8) O34' 0.062(4) 0.323(13) 0.070(5) 0.037(6) 0.018(3) -0.029(6) Cl4 0.0824(14) 0.0986(16) 0.0751(13) 0.0360(12) 0.0355(11) 0.0520(12) O41 0.251(13) 0.147(8) 0.212(11) -0.080(8) -0.060(9) 0.120(9) O42 0.100(5) 0.249(11) 0.092(5) 0.043(6) 0.015(4) 0.044(6) O43 0.255(13) 0.135(8) 0.182(9) 0.040(7) 0.112(9) 0.019(8) O44 0.223(10) 0.234(10) 0.110(6) 0.013(6) -0.007(6) 0.181(9) O1W 0.058(2) 0.036(2) 0.045(2) -0.0026(17) -0.0109(19) 0.0016(18) O2W 0.044(2) 0.093(3) 0.038(2) 0.003(2) -0.0070(18) 0.013(2) O3W 0.066(3) 0.081(3) 0.044(3) 0.006(2) -0.010(2) 0.018(2) O4W 0.074(3) 0.033(2) 0.075(3) 0.013(2) 0.014(2) 0.006(2) O5W 0.043(5) 0.044(5) 0.077(6) 0.013(4) 0.007(4) 0.007(4) O7W 0.085(8) 0.079(7) 0.116(9) 0.047(7) -0.063(7) -0.055(6) O8W 0.169(17) 0.119(13) 0.134(14) -0.001(11) 0.037(12) -0.028(11) O9W 0.090(7) 0.039(4) 0.036(4) -0.018(4) -0.019(4) 0.021(4) O10W 0.119(10) 0.078(8) 0.091(8) -0.014(6) -0.041(7) 0.017(7) O11W 0.113(10) 0.092(9) 0.078(8) -0.016(6) 0.008(7) -0.019(7) O12W 0.095(10) 0.128(13) 0.135(13) 0.014(11) -0.033(9) 0.000(10) _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 N2 C12C 1.461(8) . ? N2 C12A 1.463(8) . ? N2 C12B 1.469(7) . ? C12A C11A 1.493(9) . ? C11A N4A 1.507(7) . ? N4A C10A 1.489(8) . ? C10A C8A 1.498(8) . ? C8A C9A 1.374(8) . ? C8A C7A 1.399(9) . ? C7A C6A 1.377(9) . ? C6A C5A 1.390(10) . ? C5A C4A 1.384(9) . ? C4A C9A 1.398(8) . ? C4A C3A 1.488(9) . ? C3A N3A 1.510(8) . ? N3A C2A 1.499(7) . ? C2A C1A 1.482(11) . ? C1A N1 1.490(9) . ? C12B C11B 1.506(8) . ? C11B N4B 1.509(7) . ? N4B C10B 1.506(7) . ? C10B C8B 1.492(8) . ? C8B C7B 1.384(8) . ? C8B C9B 1.387(7) . ? C7B C6B 1.382(8) . ? C6B C5B 1.374(8) . ? C5B C4B 1.392(7) . ? C4B C9B 1.395(7) . ? C4B C3B 1.512(7) . ? C3B N3B 1.496(7) . ? N3B C2B 1.501(7) . ? C2B C1B 1.530(9) . ? C1B N1 1.448(9) . ? C12C C11' 1.511(18) . ? N4C C10C 1.495(14) . ? C10C C8C 1.46(2) . ? C8C C7C 1.3900 . ? C8C C9C 1.3900 . ? C7C C6C 1.3900 . ? C6C C5C 1.3900 . ? C5C C4C 1.3900 . ? C4C C3C 1.3723 . ? C4C C9C 1.3900 . ? C3C N3C 1.486(15) . ? N3C C2C 1.52(3) . ? C2C C1C 1.51(3) . ? C1C N1 1.63(3) . ? C11' N4C' 1.19(3) . ? N4C' C10' 1.59(2) . ? C10' C8C' 1.43(2) . ? C8C' C7C' 1.3900 . ? C8C' C9C' 1.3900 . ? C7C' C6C' 1.3900 . ? C6C' C5C' 1.3900 . ? C5C' C4C' 1.3900 . ? C4C' C9C' 1.3900 . ? C4C' C3C' 1.499(19) . ? C3C' N3C' 1.43(2) . ? N3C' C2' 1.47(2) . ? C2' C1' 1.45(3) . ? Se O2 1.625(4) . ? Se O4 1.637(4) . ? Se O3 1.636(4) . ? Se O1 1.651(4) . ? Cl1 O14 1.313(12) . ? Cl1 O12 1.360(10) . ? Cl1 O13 1.385(10) . ? Cl1 O11 1.428(7) . ? Cl2 O23 1.306(8) . ? Cl2 O21 1.412(5) . ? Cl2 O24 1.412(7) . ? Cl2 O22 1.471(7) . ? O21 Cl2' 1.328(7) . ? O22 Cl2' 1.157(8) . ? O23 Cl2' 1.716(12) . ? Cl2' O24' 1.44(2) . ? O24' O7W 1.80(3) . ? Cl3 O34 1.326(6) . ? Cl3 O32 1.385(10) . ? Cl3 O31 1.375(10) . ? Cl3 O33 1.392(8) . ? Cl3' O32' 1.404(11) . ? Cl3' O31' 1.410(11) . ? Cl3' O33' 1.448(11) . ? Cl4 O41 1.275(8) . ? Cl4 O44 1.341(6) . ? Cl4 O42 1.406(7) . ? Cl4 O43 1.490(9) . ? 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 C12C N2 C12A 109.4(5) . . ? C12C N2 C12B 109.7(5) . . ? C12A N2 C12B 109.6(4) . . ? N2 C12A C11A 113.6(5) . . ? C12A C11A N4A 112.5(4) . . ? C10A N4A C11A 111.1(4) . . ? N4A C10A C8A 112.9(4) . . ? C9A C8A C7A 118.9(6) . . ? C9A C8A C10A 122.4(5) . . ? C7A C8A C10A 118.7(6) . . ? C6A C7A C8A 119.9(6) . . ? C7A C6A C5A 120.8(6) . . ? C4A C5A C6A 119.9(6) . . ? C5A C4A C9A 118.7(6) . . ? C5A C4A C3A 120.6(6) . . ? C9A C4A C3A 120.6(5) . . ? C8A C9A C4A 121.7(5) . . ? C4A C3A N3A 108.6(5) . . ? C2A N3A C3A 112.9(5) . . ? C1A C2A N3A 111.0(6) . . ? C2A C1A N1 115.4(5) . . ? N2 C12B C11B 112.8(5) . . ? C12B C11B N4B 111.4(4) . . ? C10B N4B C11B 110.1(4) . . ? C8B C10B N4B 113.2(4) . . ? C7B C8B C9B 119.1(5) . . ? C7B C8B C10B 121.0(5) . . ? C9B C8B C10B 119.8(5) . . ? C6B C7B C8B 120.4(5) . . ? C5B C6B C7B 120.8(5) . . ? C6B C5B C4B 119.7(5) . . ? C5B C4B C9B 119.5(5) . . ? C5B C4B C3B 121.2(5) . . ? C9B C4B C3B 119.1(5) . . ? C8B C9B C4B 120.6(5) . . ? N3B C3B C4B 112.8(4) . . ? C3B N3B C2B 110.1(5) . . ? N3B C2B C1B 110.5(5) . . ? N1 C1B C2B 112.1(7) . . ? N2 C12C C11' 112.2(9) . . ? C8C C10C N4C 112.0(12) . . ? C7C C8C C9C 120.0 . . ? C7C C8C C10C 123.9(7) . . ? C9C C8C C10C 115.9(7) . . ? C8C C7C C6C 120.0 . . ? C7C C6C C5C 120.0 . . ? C6C C5C C4C 120.0 . . ? C3C C4C C9C 124.7 . . ? C3C C4C C5C 115.0 . . ? C9C C4C C5C 120.0 . . ? C4C C9C C8C 120.0 . . ? C4C C3C N3C 120.3(8) . . ? C3C N3C C2C 115.0(10) . . ? C1C C2C N3C 112.8(15) . . ? C2C C1C N1 116.8(14) . . ? C1B N1 C1A 108.8(6) . . ? C1B N1 C1C 115.1(9) . . ? C1A N1 C1C 113.9(9) . . ? N4C' C11' C12C 124(2) . . ? C11' N4C' C10' 118.4(18) . . ? C8C' C10' N4C' 111.9(14) . . ? C7C' C8C' C9C' 120.0 . . ? C7C' C8C' C10' 121.9(13) . . ? C9C' C8C' C10' 118.1(13) . . ? C8C' C7C' C6C' 120.0 . . ? C7C' C6C' C5C' 120.0 . . ? C6C' C5C' C4C' 120.0 . . ? C9C' C4C' C5C' 120.0 . . ? C9C' C4C' C3C' 121.0(15) . . ? C5C' C4C' C3C' 118.9(14) . . ? C4C' C9C' C8C' 120.0 . . ? N3C' C3C' C4C' 116.2(15) . . ? C3C' N3C' C2' 113.5(16) . . ? C1' C2' N3C' 116(2) . . ? O2 Se O4 111.1(2) . . ? O2 Se O3 111.2(2) . . ? O4 Se O3 109.4(2) . . ? O2 Se O1 109.8(2) . . ? O4 Se O1 105.6(2) . . ? O3 Se O1 109.68(19) . . ? O14 Cl1 O12 118.4(12) . . ? O14 Cl1 O13 111.4(13) . . ? O12 Cl1 O13 107.2(13) . . ? O14 Cl1 O11 107.4(9) . . ? O12 Cl1 O11 104.0(6) . . ? O13 Cl1 O11 107.7(7) . . ? O23 Cl2 O21 111.8(6) . . ? O23 Cl2 O24 113.2(6) . . ? O21 Cl2 O24 102.8(4) . . ? O23 Cl2 O22 117.1(7) . . ? O21 Cl2 O22 105.5(5) . . ? O24 Cl2 O22 105.2(5) . . ? Cl2' O21 Cl2 37.2(4) . . ? Cl2' O22 Cl2 36.6(5) . . ? Cl2 O23 Cl2' 30.1(3) . . ? O22 Cl2' O21 134.7(7) . . ? O22 Cl2' O24' 105.7(10) . . ? O21 Cl2' O24' 102.3(10) . . ? O22 Cl2' O23 109.7(9) . . ? O21 Cl2' O23 94.5(7) . . ? O24' Cl2' O23 107.5(11) . . ? Cl2' O24' O7W 136.8(17) . . ? O34 Cl3 O32 113.9(7) . . ? O34 Cl3 O31 112.2(8) . . ? O32 Cl3 O31 101.2(10) . . ? O34 Cl3 O33 108.0(6) . . ? O32 Cl3 O33 116.0(11) . . ? O31 Cl3 O33 105.2(7) . . ? O32' Cl3' O31' 110.0(10) . . ? O32' Cl3' O33' 106.5(12) . . ? O31' Cl3' O33' 108.7(9) . . ? O41 Cl4 O44 122.6(7) . . ? O41 Cl4 O42 111.3(7) . . ? O44 Cl4 O42 107.5(5) . . ? O41 Cl4 O43 106.2(8) . . ? O44 Cl4 O43 106.0(7) . . ? O42 Cl4 O43 100.9(6) . . ? 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 N4A H4A1 O2 0.92 2.03 2.927(6) 164.2 . N4A H4A2 O2W 0.92 2.05 2.848(6) 144.4 . N3A H3A1N O1 0.92 1.91 2.820(6) 169.9 . N3A H3A2N O3W 0.92 2.01 2.884(6) 158.4 . N4B H4B2 O4W 0.92 1.86 2.762(6) 166.7 . N4B H4B1 O2 0.92 2.37 3.116(6) 138.4 . N4B H4B1 O9W 0.92 2.48 3.239(10) 139.5 . N3B H3B1 O22 0.92 2.04 2.932(9) 163.5 2_645 N3B H3B2 O1 0.92 2.07 2.924(6) 154.0 . N4C H4C1 O5W 0.92 1.93 2.805(15) 157.8 . N4C H4C2 O6WA 0.92 1.71 2.57(2) 153.6 . N4C H4C2 O6WB 0.92 1.63 2.54(2) 171.4 . N4C' H4C5 O6WB 0.92 1.88 2.76(2) 159.2 . N3C H3C1 O7W 0.92 2.14 2.879(14) 136.5 . N3C H3C2 O4 0.92 1.74 2.653(12) 172.3 . N3C' H3C4 O4 0.92 2.05 2.913(13) 154.8 . N4C' H4C6 O9W 0.92 2.44 2.894(17) 110.9 . _diffrn_measured_fraction_theta_max 1.000 _diffrn_reflns_theta_full 25.00 _diffrn_measured_fraction_theta_full 1.000 _refine_diff_density_max 1.206 _refine_diff_density_min -0.984 _refine_diff_density_rms 0.109 data_global _journal_coden_Cambridge 186 _publ_requested_journal 'Dalton Transactions' loop_ _publ_author_name 'Maubert, Beatrice M.' 'McKee, Vickie' 'Nelson, Jane' 'Pal, Ibolya' 'Town, Raewyn' _publ_contact_author_name 'Prof Jane Nelson' _publ_contact_author_address ; Prof Jane Nelson School of Chemistry Queens University Belfast BT9 5AG UNITED KINGDOM ; _publ_contact_author_email 'JANE.NELSON@QUB.AC.UK' data_'complex 3' _database_code_CSD 161207 _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C36 H82 Cl4 N8 O30 S2' _chemical_formula_weight 1313.02 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' 'S' 'S' 0.1246 0.1234 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'Cl' 'Cl' 0.1484 0.1585 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting Monoclinic _symmetry_space_group_name_H-M P2(1)/n 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 14.6926(4) _cell_length_b 13.7829(4) _cell_length_c 28.5979(2) _cell_angle_alpha 90.00 _cell_angle_beta 91.1400(10) _cell_angle_gamma 90.00 _cell_volume 5790.1(2) _cell_formula_units_Z 4 _cell_measurement_temperature 150(2) _cell_measurement_reflns_used ? _cell_measurement_theta_min ? _cell_measurement_theta_max ? _exptl_crystal_description block _exptl_crystal_colour colourless _exptl_crystal_size_max 0.20 _exptl_crystal_size_mid 0.12 _exptl_crystal_size_min 0.10 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.506 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 2776 _exptl_absorpt_coefficient_mu 0.371 _exptl_absorpt_correction_type none _exptl_absorpt_correction_T_min ? _exptl_absorpt_correction_T_max ? _exptl_absorpt_process_details ? _exptl_special_details ; ? ; _diffrn_ambient_temperature 150(2) _diffrn_radiation_wavelength 0.69410 _diffrn_radiation_type Synchrotron _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'CCD area detector' _diffrn_measurement_method 'phi and omega scans' _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 30687 _diffrn_reflns_av_R_equivalents 0.0557 _diffrn_reflns_av_sigmaI/netI 0.0638 _diffrn_reflns_limit_h_min -16 _diffrn_reflns_limit_h_max 17 _diffrn_reflns_limit_k_min -16 _diffrn_reflns_limit_k_max 8 _diffrn_reflns_limit_l_min -34 _diffrn_reflns_limit_l_max 32 _diffrn_reflns_theta_min 1.98 _diffrn_reflns_theta_max 25.00 _reflns_number_total 10904 _reflns_number_gt 8029 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'Bruker SMART' _computing_cell_refinement 'Bruker SMART' _computing_data_reduction 'Bruker SHELXTL' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'Bruker SHELXTL' _computing_publication_material 'Bruker SHELXTL' _refine_special_details ; Refinement of F^2^ against ALL reflections. The weighted R-factor wR and goodness of fit S are based on F^2^, conventional R-factors R are based on F, with F set to zero for negative F^2^. The threshold expression of F^2^ > 2sigma(F^2^) is used only for calculating R-factors(gt) etc. and is not relevant to the choice of reflections for refinement. R-factors based on F^2^ are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger. ; _refine_ls_structure_factor_coef Fsqd _refine_ls_matrix_type full _refine_ls_weighting_scheme calc _refine_ls_weighting_details 'calc w=1/[\s^2^(Fo^2^)+(0.1410P)^2^+0.0000P] 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 10904 _refine_ls_number_parameters 784 _refine_ls_number_restraints 118 _refine_ls_R_factor_all 0.0881 _refine_ls_R_factor_gt 0.0699 _refine_ls_wR_factor_ref 0.2081 _refine_ls_wR_factor_gt 0.2006 _refine_ls_goodness_of_fit_ref 1.071 _refine_ls_restrained_S_all 1.112 _refine_ls_shift/su_max 0.148 _refine_ls_shift/su_mean 0.006 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 N1 N -0.20150(19) 0.2795(2) 0.19968(11) 0.0253(6) Uani 1 1 d . . . C1A C -0.2415(3) 0.1946(3) 0.17550(15) 0.0343(9) Uani 1 1 d . . . H1A1 H -0.3086 0.1969 0.1781 0.041 Uiso 1 1 calc R . . H1A2 H -0.2198 0.1347 0.1912 0.041 Uiso 1 1 calc R . . C2A C -0.2173(3) 0.1903(3) 0.12454(15) 0.0407(10) Uani 1 1 d . . . H2A1 H -0.2668 0.1572 0.1068 0.049 Uiso 1 1 calc R . . H2A2 H -0.2122 0.2572 0.1122 0.049 Uiso 1 1 calc R . . N3A N -0.1301(2) 0.1379(3) 0.11704(12) 0.0346(8) Uani 1 1 d . . . H3A1 H -0.0848 0.1664 0.1349 0.042 Uiso 1 1 calc R . . H3A2 H -0.1361 0.0747 0.1268 0.042 Uiso 1 1 calc R . . C3A C -0.1033(3) 0.1387(4) 0.06717(16) 0.0483(12) Uani 1 1 d . . . H3A3 H -0.1011 0.2067 0.0561 0.058 Uiso 1 1 calc R . . H3A4 H -0.1503 0.1043 0.0482 0.058 Uiso 1 1 calc R . . C4A C -0.0125(3) 0.0919(3) 0.05953(13) 0.0372(10) Uani 1 1 d . . . C5A C 0.0007(3) -0.0080(3) 0.06473(14) 0.0385(10) Uani 1 1 d . . . H5A H -0.0486 -0.0479 0.0738 0.046 Uiso 1 1 calc R . . C6A C 0.0835(3) -0.0486(3) 0.05693(14) 0.0395(10) Uani 1 1 d . . . H6A H 0.0922 -0.1162 0.0617 0.047 Uiso 1 1 calc R . . C7A C 0.1557(3) 0.0086(3) 0.04201(14) 0.0356(9) Uani 1 1 d . . . H7A H 0.2131 -0.0200 0.0359 0.043 Uiso 1 1 calc R . . C8A C 0.1432(3) 0.1074(3) 0.03613(13) 0.0354(9) Uani 1 1 d . . . C9A C 0.0598(3) 0.1489(3) 0.04574(13) 0.0370(10) Uani 1 1 d . . . H9A H 0.0520 0.2171 0.0428 0.044 Uiso 1 1 calc R . . C10A C 0.2189(3) 0.1700(4) 0.01746(15) 0.0437(11) Uani 1 1 d . . . H10A H 0.2520 0.1330 -0.0065 0.052 Uiso 1 1 calc R . . H10B H 0.1919 0.2279 0.0021 0.052 Uiso 1 1 calc R . . N4A N 0.2847(2) 0.2020(3) 0.05473(10) 0.0317(7) Uani 1 1 d . . . H4A1 H 0.2553 0.2415 0.0755 0.038 Uiso 1 1 calc R . . H4A2 H 0.3060 0.1486 0.0709 0.038 Uiso 1 1 calc R . . C11A C 0.3620(3) 0.2548(3) 0.03491(14) 0.0411(10) Uani 1 1 d . . . H11A H 0.3397 0.3156 0.0202 0.049 Uiso 1 1 calc R . . H11B H 0.3897 0.2147 0.0102 0.049 Uiso 1 1 calc R . . C12A C 0.4344(3) 0.2793(3) 0.07209(15) 0.0376(9) Uani 1 1 d . . . H12A H 0.4487 0.2200 0.0904 0.045 Uiso 1 1 calc R . . H12B H 0.4907 0.2998 0.0564 0.045 Uiso 1 1 calc R . . N2 N 0.4067(2) 0.3561(2) 0.10423(10) 0.0259(7) Uani 1 1 d . . . C1B C -0.2594(2) 0.3643(3) 0.18963(14) 0.0304(8) Uani 1 1 d . . . H1B1 H -0.3156 0.3589 0.2080 0.037 Uiso 1 1 calc R . . H1B2 H -0.2773 0.3635 0.1561 0.037 Uiso 1 1 calc R . . C2B C -0.2136(3) 0.4609(3) 0.20092(14) 0.0317(8) Uani 1 1 d . . . H2B1 H -0.2602 0.5128 0.2010 0.038 Uiso 1 1 calc R . . H2B2 H -0.1855 0.4577 0.2326 0.038 Uiso 1 1 calc R . . N3B N -0.1423(2) 0.4860(2) 0.16656(11) 0.0268(7) Uani 1 1 d . . . H3B1 H -0.0956 0.4418 0.1690 0.032 Uiso 1 1 calc R . . H3B2 H -0.1668 0.4820 0.1368 0.032 Uiso 1 1 calc R . . C3B C -0.1053(3) 0.5855(3) 0.17441(15) 0.0400(10) Uani 1 1 d . . . H3B3 H -0.0746 0.5884 0.2055 0.048 Uiso 1 1 calc R . . H3B4 H -0.1561 0.6327 0.1742 0.048 Uiso 1 1 calc R . . C4B C -0.0383(3) 0.6130(3) 0.13711(13) 0.0307(8) Uani 1 1 d . . . C5B C -0.0696(3) 0.6573(3) 0.09668(15) 0.0387(10) Uani 1 1 d . . . H5B H -0.1327 0.6702 0.0923 0.046 Uiso 1 1 calc R . . C6B C -0.0087(3) 0.6829(3) 0.06236(16) 0.0454(11) Uani 1 1 d . . . H6B H -0.0307 0.7116 0.0341 0.055 Uiso 1 1 calc R . . C7B C 0.0843(3) 0.6669(3) 0.06877(14) 0.0387(10) Uani 1 1 d . . . H7B H 0.1256 0.6854 0.0452 0.046 Uiso 1 1 calc R . . C8B C 0.1168(3) 0.6235(3) 0.11005(14) 0.0323(9) Uani 1 1 d . . . C9B C 0.0541(3) 0.5972(3) 0.14374(13) 0.0316(9) Uani 1 1 d . . . H9B H 0.0753 0.5678 0.1719 0.038 Uiso 1 1 calc R . . C10B C 0.2170(3) 0.6148(3) 0.11898(16) 0.0391(10) Uani 1 1 d . . . H10C H 0.2286 0.6139 0.1532 0.047 Uiso 1 1 calc R . . H10D H 0.2472 0.6731 0.1063 0.047 Uiso 1 1 calc R . . N4B N 0.2599(2) 0.5265(2) 0.09808(11) 0.0282(7) Uani 1 1 d . . . H4B1 H 0.2455 0.5233 0.0667 0.034 Uiso 1 1 calc R . . H4B2 H 0.2379 0.4716 0.1122 0.034 Uiso 1 1 calc R . . C11B C 0.3615(3) 0.5313(3) 0.10485(14) 0.0327(9) Uani 1 1 d . . . H11C H 0.3767 0.5274 0.1387 0.039 Uiso 1 1 calc R . . H11D H 0.3836 0.5945 0.0932 0.039 Uiso 1 1 calc R . . C12B C 0.4100(3) 0.4507(3) 0.07969(14) 0.0338(9) Uani 1 1 d . . . H12C H 0.3822 0.4431 0.0481 0.041 Uiso 1 1 calc R . . H12D H 0.4744 0.4694 0.0758 0.041 Uiso 1 1 calc R . . C1C C -0.2006(2) 0.2602(3) 0.25022(13) 0.0283(8) Uani 1 1 d . . . H1C1 H -0.2585 0.2286 0.2587 0.034 Uiso 1 1 calc R . . H1C2 H -0.1962 0.3224 0.2674 0.034 Uiso 1 1 calc R . . C2C C -0.1220(2) 0.1956(3) 0.26506(14) 0.0306(8) Uani 1 1 d . . . H2C1 H -0.1368 0.1632 0.2949 0.037 Uiso 1 1 calc R . . H2C2 H -0.1138 0.1446 0.2411 0.037 Uiso 1 1 calc R . . N3C N -0.03481(19) 0.2504(2) 0.27139(11) 0.0251(6) Uani 1 1 d . . . H3C1 H -0.0407 0.2947 0.2952 0.030 Uiso 1 1 calc R . . H3C2 H -0.0227 0.2839 0.2444 0.030 Uiso 1 1 calc R . . C3C C 0.0431(2) 0.1834(3) 0.28278(14) 0.0276(8) Uani 1 1 d . . . H3C3 H 0.0524 0.1396 0.2559 0.033 Uiso 1 1 calc R . . H3C4 H 0.0269 0.1428 0.3099 0.033 Uiso 1 1 calc R . . C4C C 0.1307(2) 0.2355(2) 0.29384(12) 0.0244(7) Uani 1 1 d . . . C5C C 0.1399(3) 0.2958(3) 0.33270(13) 0.0285(8) Uani 1 1 d . . . H5C H 0.0890 0.3075 0.3518 0.034 Uiso 1 1 calc R . . C6C C 0.2230(3) 0.3389(3) 0.34376(13) 0.0296(8) Uani 1 1 d . . . H6C H 0.2282 0.3818 0.3697 0.036 Uiso 1 1 calc R . . C7C C 0.2989(3) 0.3193(2) 0.31678(13) 0.0280(8) Uani 1 1 d . . . H7C H 0.3561 0.3472 0.3250 0.034 Uiso 1 1 calc R . . C8C C 0.2914(2) 0.2594(2) 0.27818(12) 0.0232(7) Uani 1 1 d . . . C9C C 0.2067(2) 0.2192(2) 0.26625(12) 0.0229(7) Uani 1 1 d . . . H9C H 0.2007 0.1802 0.2390 0.028 Uiso 1 1 calc R . . C10C C 0.3734(2) 0.2360(3) 0.25000(13) 0.0260(8) Uani 1 1 d . . . H10E H 0.3747 0.1655 0.2436 0.031 Uiso 1 1 calc R . . H10F H 0.4290 0.2527 0.2684 0.031 Uiso 1 1 calc R . . N4C N 0.37384(18) 0.2902(2) 0.20446(10) 0.0229(6) Uani 1 1 d . . . H4C1 H 0.3272 0.2677 0.1855 0.027 Uiso 1 1 calc R . . H4C2 H 0.3635 0.3550 0.2101 0.027 Uiso 1 1 calc R . . C11C C 0.4618(2) 0.2794(3) 0.17964(13) 0.0284(8) Uani 1 1 d . . . H11E H 0.4632 0.2156 0.1638 0.034 Uiso 1 1 calc R . . H11F H 0.5129 0.2814 0.2027 0.034 Uiso 1 1 calc R . . C12C C 0.4739(2) 0.3596(3) 0.14372(13) 0.0289(8) Uani 1 1 d . . . H12E H 0.4688 0.4232 0.1596 0.035 Uiso 1 1 calc R . . H12F H 0.5360 0.3551 0.1310 0.035 Uiso 1 1 calc R . . S1 S 0.04051(6) 0.31213(6) 0.15680(3) 0.0240(2) Uani 1 1 d . . . S2 S 0.17134(6) 0.32621(7) 0.14088(3) 0.0266(2) Uani 1 1 d . . . O1 O -0.02019(18) 0.3396(2) 0.11757(10) 0.0371(7) Uani 1 1 d . . . O3 O 0.02012(17) 0.37484(18) 0.19746(9) 0.0287(6) Uani 1 1 d . . . O4 O 0.02253(17) 0.21051(18) 0.16993(9) 0.0282(6) Uani 1 1 d . . . Cl1 Cl 0.55226(6) 1.00993(7) 0.17131(3) 0.0321(2) Uani 1 1 d D . . O11 O 0.5955(3) 0.9167(3) 0.16985(15) 0.0644(11) Uani 1 1 d D . . O12 O 0.5731(3) 1.0601(3) 0.21360(12) 0.0694(11) Uani 1 1 d D . . O13 O 0.4548(2) 0.9940(2) 0.16856(13) 0.0509(8) Uani 1 1 d D . . O14 O 0.5778(2) 1.0676(2) 0.13249(11) 0.0479(8) Uani 1 1 d D . . Cl2 Cl 0.92383(6) 0.91740(7) 0.20662(3) 0.0311(2) Uani 1 1 d . . . O21 O 0.9729(3) 0.9390(4) 0.16589(12) 0.0761(13) Uani 1 1 d . . . O22 O 0.9106(2) 0.8151(2) 0.21014(13) 0.0538(9) Uani 1 1 d . . . O23 O 0.9741(2) 0.9490(3) 0.24737(11) 0.0518(9) Uani 1 1 d . . . O24 O 0.8372(3) 0.9635(3) 0.20522(15) 0.0635(10) Uani 1 1 d . . . Cl3 Cl 0.32748(9) 0.73538(11) 0.00335(5) 0.0636(4) Uani 0.60 1 d PD A 1 O31 O 0.3592(4) 0.7830(5) -0.03582(19) 0.118(2) Uani 0.60 1 d PD A 1 O32 O 0.2822(6) 0.6447(6) 0.0036(3) 0.088(2) Uani 0.60 1 d PDU A 1 O33 O 0.4117(6) 0.7248(7) 0.0301(3) 0.101(3) Uani 0.60 1 d PDU A 1 O34 O 0.2689(8) 0.8041(7) 0.0279(4) 0.123(4) Uani 0.60 1 d PDU A 1 Cl3' Cl 0.32748(9) 0.73538(11) 0.00335(5) 0.0636(4) Uani 0.40 1 d PD B 2 O31' O 0.3592(4) 0.7830(5) -0.03582(19) 0.118(2) Uani 0.40 1 d PD B 2 O32' O 0.2358(5) 0.7110(8) -0.0175(3) 0.062(2) Uani 0.40 1 d PD B 2 O33' O 0.3731(9) 0.6394(8) 0.0020(5) 0.096(4) Uani 0.40 1 d PD B 2 O34' O 0.3252(15) 0.7731(12) 0.0461(3) 0.132(7) Uani 0.40 1 d PD B 2 Cl4 Cl -0.13338(10) 0.15265(12) 0.39986(5) 0.0671(4) Uani 0.60 1 d PD C 1 O41 O -0.0546(6) 0.1886(9) 0.3799(3) 0.069(3) Uani 0.60 1 d PD C 1 O42 O -0.1197(5) 0.0835(7) 0.4390(3) 0.065(2) Uani 0.60 1 d PD C 1 O43 O -0.1922(7) 0.1065(8) 0.3657(2) 0.093(3) Uani 0.60 1 d PD C 1 O44 O -0.1873(5) 0.2331(6) 0.4185(3) 0.080(2) Uani 0.60 1 d PD C 1 Cl4' Cl -0.13338(10) 0.15265(12) 0.39986(5) 0.0671(4) Uani 0.40 1 d PD D 2 O41' O -0.1179(11) 0.0625(8) 0.3731(4) 0.099(4) Uani 0.40 1 d PD D 2 O43' O -0.2065(10) 0.2055(19) 0.3838(11) 0.39(3) Uani 0.40 1 d PD D 2 O44' O -0.0578(16) 0.2151(17) 0.3860(9) 0.173(15) Uani 0.40 1 d PD D 2 O42' O -0.107(2) 0.1198(14) 0.4455(4) 0.179(14) Uani 0.40 1 d PD D 2 O1W O 0.33017(18) 0.48054(19) 0.22471(10) 0.0330(6) Uani 1 1 d . . . O2W O 0.15055(18) 0.48792(19) 0.24347(10) 0.0331(6) Uani 1 1 d . . . O3W O 0.13702(19) 0.05658(19) 0.17653(10) 0.0365(7) Uani 1 1 d . . . O4W O 0.3063(2) 0.1223(2) 0.14944(12) 0.0489(8) Uani 1 1 d . . . O5W O -0.2213(3) -0.0433(3) 0.10003(13) 0.0631(10) Uani 1 1 d . . . O6W O 0.0165(3) 0.4325(3) 0.03777(11) 0.0604(10) Uani 1 1 d . . . O7W O 0.1956(3) 0.4358(3) 0.01616(12) 0.0653(10) Uani 1 1 d . . . O8W O 0.2218(3) 0.5418(3) -0.07374(13) 0.0781(13) Uani 1 1 d . . . O9W O 0.3880(3) 0.0317(3) 0.06289(16) 0.0857(14) Uani 1 1 d . . . O10W O 0.5147(4) 0.8757(3) 0.06646(18) 0.0899(14) Uani 1 1 d . . . O11W O -0.3660(3) 0.0060(4) 0.03240(16) 0.0829(13) Uani 1 1 d . . . H1WA H 0.2739 0.4832 0.2309 0.050 Uiso 1 1 d . . . H1WB H 0.3598 0.4991 0.2489 0.050 Uiso 1 1 d . . . H2WA H 0.1189 0.4460 0.2287 0.050 Uiso 1 1 d . . . H2WB H 0.1254 0.4862 0.2700 0.050 Uiso 1 1 d . . . H3WA H 0.1024 0.1052 0.1716 0.050 Uiso 1 1 d . . . H3WB H 0.0975 0.0138 0.1694 0.050 Uiso 1 1 d . . . H4WA H 0.3390 0.0736 0.1568 0.050 Uiso 1 1 d . . . H4WB H 0.2534 0.1012 0.1555 0.050 Uiso 1 1 d . . . H5WA H -0.2628 -0.0283 0.0805 0.050 Uiso 1 1 d . . . H5WB H -0.2512 -0.0618 0.1237 0.050 Uiso 1 1 d . . . H6WA H 0.0052 0.4030 0.0631 0.050 Uiso 1 1 d . . . H6WB H 0.0726 0.4336 0.0311 0.050 Uiso 0.50 1 d P . . H6WC H 0.0066 0.4722 0.0156 0.050 Uiso 0.50 1 d P . . H7WA H 0.1395 0.4352 0.0228 0.050 Uiso 0.50 1 d P . . H7WB H 0.2222 0.4648 -0.0059 0.050 Uiso 1 1 d . . . H7WC H 0.2122 0.3764 0.0162 0.050 Uiso 0.50 1 d P . . H8WA H 0.2405 0.5138 -0.0488 0.050 Uiso 1 1 d . . . H8WB H 0.2471 0.4995 -0.0909 0.050 Uiso 1 1 d . . . H9WA H 0.3936 0.0185 0.0340 0.050 Uiso 1 1 d . . . H9WB H 0.4177 -0.0131 0.0767 0.050 Uiso 1 1 d . . . H1WC H 0.5277 0.8248 0.0820 0.050 Uiso 1 1 d . . . H1WD H 0.4643 0.8471 0.0610 0.050 Uiso 1 1 d . . . H1WE H -0.4046 -0.0357 0.0413 0.050 Uiso 1 1 d . . . H1WF H -0.3746 0.0664 0.0281 0.050 Uiso 1 1 d . . . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 N1 0.0158(14) 0.0242(15) 0.0355(17) -0.0028(13) -0.0040(12) 0.0009(12) C1A 0.0256(19) 0.028(2) 0.049(2) -0.0096(18) -0.0035(17) -0.0064(16) C2A 0.032(2) 0.040(2) 0.050(3) -0.012(2) -0.0153(18) 0.0032(19) N3A 0.0292(17) 0.0400(19) 0.0344(18) -0.0102(15) -0.0078(13) -0.0035(15) C3A 0.045(3) 0.062(3) 0.038(2) -0.013(2) -0.0119(19) 0.012(2) C4A 0.044(2) 0.047(2) 0.0208(19) -0.0084(17) -0.0084(16) -0.002(2) C5A 0.041(2) 0.046(2) 0.029(2) -0.0048(18) -0.0003(17) -0.013(2) C6A 0.053(3) 0.032(2) 0.033(2) -0.0088(18) -0.0064(18) -0.004(2) C7A 0.039(2) 0.039(2) 0.029(2) -0.0067(17) -0.0047(16) -0.0008(19) C8A 0.047(2) 0.039(2) 0.0201(18) -0.0003(16) -0.0094(16) -0.0108(19) C9A 0.049(3) 0.036(2) 0.0250(19) -0.0027(17) -0.0109(17) 0.003(2) C10A 0.051(3) 0.049(3) 0.030(2) 0.0031(19) -0.0099(19) -0.016(2) N4A 0.0370(18) 0.0360(18) 0.0220(15) -0.0035(14) -0.0033(13) 0.0030(15) C11A 0.051(3) 0.044(2) 0.029(2) -0.0030(18) 0.0049(18) -0.009(2) C12A 0.031(2) 0.042(2) 0.040(2) -0.0036(19) 0.0072(17) -0.0031(19) N2 0.0228(15) 0.0301(16) 0.0245(15) -0.0020(13) -0.0019(12) -0.0021(13) C1B 0.0235(18) 0.031(2) 0.037(2) -0.0003(16) -0.0039(15) 0.0064(16) C2B 0.030(2) 0.029(2) 0.037(2) 0.0012(17) 0.0038(16) 0.0067(16) N3B 0.0266(16) 0.0207(15) 0.0328(17) -0.0025(13) -0.0022(13) 0.0067(13) C3B 0.056(3) 0.023(2) 0.041(2) -0.0042(17) 0.010(2) -0.0081(19) C4B 0.041(2) 0.0204(17) 0.031(2) -0.0020(15) -0.0009(16) -0.0014(16) C5B 0.037(2) 0.039(2) 0.040(2) 0.0035(19) -0.0028(18) 0.0042(19) C6B 0.051(3) 0.046(3) 0.039(2) 0.019(2) -0.005(2) 0.012(2) C7B 0.048(3) 0.036(2) 0.033(2) 0.0088(18) 0.0055(18) -0.002(2) C8B 0.038(2) 0.0187(17) 0.040(2) -0.0075(16) -0.0095(17) 0.0003(16) C9B 0.051(2) 0.0190(17) 0.0243(18) -0.0004(14) -0.0094(17) -0.0027(17) C10B 0.039(2) 0.026(2) 0.051(3) -0.0152(18) -0.0112(19) -0.0011(18) N4B 0.0285(16) 0.0251(16) 0.0306(17) 0.0022(13) -0.0058(13) -0.0069(13) C11B 0.030(2) 0.028(2) 0.039(2) 0.0042(17) -0.0103(16) -0.0088(16) C12B 0.0256(19) 0.040(2) 0.035(2) 0.0098(18) -0.0004(16) -0.0062(17) C1C 0.0206(17) 0.0296(19) 0.034(2) 0.0010(16) -0.0010(14) 0.0018(15) C2C 0.0257(19) 0.0257(19) 0.040(2) 0.0052(16) -0.0044(16) -0.0025(16) N3C 0.0229(15) 0.0225(15) 0.0300(16) 0.0020(12) 0.0008(12) 0.0018(13) C3C 0.0241(18) 0.0198(17) 0.039(2) 0.0069(15) -0.0026(15) 0.0037(15) C4C 0.0264(18) 0.0179(16) 0.0287(18) 0.0060(14) -0.0050(14) 0.0026(14) C5C 0.033(2) 0.0192(17) 0.033(2) 0.0013(15) -0.0013(15) 0.0085(16) C6C 0.042(2) 0.0173(17) 0.0299(19) -0.0003(15) -0.0036(16) 0.0015(16) C7C 0.033(2) 0.0170(17) 0.034(2) 0.0042(15) -0.0092(16) -0.0051(15) C8C 0.0252(17) 0.0150(15) 0.0292(18) 0.0052(14) -0.0052(14) -0.0009(14) C9C 0.0256(18) 0.0157(16) 0.0273(18) 0.0047(14) -0.0061(14) -0.0012(14) C10C 0.0222(17) 0.0203(17) 0.035(2) 0.0065(15) -0.0065(15) -0.0003(14) N4C 0.0172(14) 0.0210(14) 0.0303(16) 0.0011(12) -0.0041(11) 0.0028(12) C11C 0.0188(17) 0.033(2) 0.033(2) -0.0032(16) -0.0006(14) 0.0023(15) C12C 0.0159(17) 0.036(2) 0.034(2) 0.0016(17) -0.0009(14) -0.0020(16) S1 0.0235(4) 0.0187(4) 0.0296(5) 0.0002(3) -0.0043(3) 0.0021(3) S2 0.0256(5) 0.0229(4) 0.0314(5) 0.0012(4) -0.0006(4) -0.0008(4) O1 0.0327(15) 0.0413(16) 0.0367(15) 0.0052(13) -0.0116(12) 0.0054(13) O3 0.0285(13) 0.0222(13) 0.0355(14) -0.0057(11) 0.0031(11) 0.0002(11) O4 0.0267(13) 0.0174(12) 0.0402(15) 0.0005(11) -0.0034(11) 0.0000(10) Cl1 0.0286(5) 0.0280(5) 0.0394(5) 0.0065(4) -0.0036(4) -0.0008(4) O11 0.058(2) 0.0421(19) 0.094(3) 0.026(2) 0.016(2) 0.0195(17) O12 0.083(3) 0.080(3) 0.044(2) -0.0034(19) -0.0128(18) -0.022(2) O13 0.0298(16) 0.0505(19) 0.072(2) 0.0041(17) -0.0016(15) -0.0032(14) O14 0.056(2) 0.0390(17) 0.0486(18) 0.0127(14) -0.0003(15) -0.0100(15) Cl2 0.0294(5) 0.0288(5) 0.0350(5) 0.0040(4) -0.0030(4) -0.0037(4) O21 0.067(2) 0.121(4) 0.0393(19) 0.009(2) 0.0020(17) -0.049(3) O22 0.052(2) 0.0308(17) 0.078(2) -0.0028(16) -0.0056(17) -0.0037(15) O23 0.061(2) 0.054(2) 0.0398(17) 0.0028(15) -0.0137(15) -0.0132(17) O24 0.052(2) 0.058(2) 0.081(3) 0.002(2) -0.0119(18) 0.0209(18) Cl3 0.0470(7) 0.0729(9) 0.0711(9) 0.0240(7) 0.0036(6) 0.0022(7) O31 0.108(4) 0.146(5) 0.100(4) 0.057(4) 0.030(3) 0.033(4) O32 0.081(5) 0.091(6) 0.092(5) -0.007(5) 0.000(4) -0.029(5) O33 0.081(5) 0.108(7) 0.113(6) 0.044(6) -0.035(5) -0.022(5) O34 0.126(8) 0.077(6) 0.169(10) 0.004(7) 0.079(7) 0.030(6) Cl3' 0.0470(7) 0.0729(9) 0.0711(9) 0.0240(7) 0.0036(6) 0.0022(7) O31' 0.108(4) 0.146(5) 0.100(4) 0.057(4) 0.030(3) 0.033(4) O32' 0.045(5) 0.077(7) 0.065(6) 0.016(5) -0.003(4) 0.004(5) O33' 0.099(10) 0.071(8) 0.117(10) 0.021(7) -0.009(8) 0.024(7) O34' 0.24(2) 0.120(13) 0.035(6) -0.056(8) -0.014(9) -0.024(13) Cl4 0.0620(9) 0.0836(10) 0.0559(8) -0.0138(7) 0.0075(6) -0.0163(8) O41 0.056(4) 0.096(7) 0.055(4) -0.035(5) 0.018(3) -0.050(4) O42 0.058(4) 0.073(6) 0.063(6) -0.013(4) 0.003(3) 0.019(4) O43 0.117(7) 0.132(8) 0.030(3) -0.017(4) 0.006(4) -0.087(6) O44 0.063(5) 0.102(6) 0.075(5) -0.008(4) 0.002(4) 0.026(4) Cl4' 0.0620(9) 0.0836(10) 0.0559(8) -0.0138(7) 0.0075(6) -0.0163(8) O41' 0.125(12) 0.086(9) 0.084(9) 0.001(7) -0.034(8) -0.015(9) O43' 0.026(9) 0.54(6) 0.60(7) -0.32(6) 0.03(2) -0.008(18) O44' 0.21(3) 0.134(18) 0.18(2) -0.103(16) 0.077(18) -0.096(16) O42' 0.40(4) 0.115(17) 0.024(7) -0.025(8) 0.022(11) 0.038(18) O1W 0.0292(14) 0.0216(13) 0.0483(17) -0.0001(12) -0.0007(12) 0.0005(11) O2W 0.0329(15) 0.0287(14) 0.0376(15) -0.0037(12) -0.0024(11) -0.0040(12) O3W 0.0345(15) 0.0213(13) 0.0532(18) -0.0006(12) -0.0115(13) 0.0019(12) O4W 0.0364(17) 0.0409(18) 0.069(2) 0.0073(16) -0.0049(15) -0.0023(14) O5W 0.056(2) 0.068(3) 0.064(2) 0.0036(19) -0.0073(18) -0.0046(19) O6W 0.071(2) 0.072(2) 0.0379(18) 0.0167(17) -0.0044(16) -0.011(2) O7W 0.065(2) 0.083(3) 0.048(2) -0.0004(19) -0.0016(17) -0.018(2) O8W 0.123(4) 0.064(3) 0.047(2) -0.0005(19) -0.020(2) 0.004(3) O9W 0.097(3) 0.080(3) 0.079(3) -0.021(2) -0.018(2) 0.034(3) O10W 0.096(3) 0.074(3) 0.100(3) 0.017(3) -0.011(3) 0.015(3) O11W 0.089(3) 0.089(3) 0.071(3) -0.006(2) 0.007(2) -0.012(3) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag N1 C1C 1.470(5) . ? N1 C1B 1.470(5) . ? N1 C1A 1.475(5) . ? C1A C2A 1.508(6) . ? C2A N3A 1.490(5) . ? N3A C3A 1.487(6) . ? C3A C4A 1.502(6) . ? C4A C9A 1.384(6) . ? C4A C5A 1.398(6) . ? C5A C6A 1.362(6) . ? C6A C7A 1.396(6) . ? C7A C8A 1.384(6) . ? C8A C9A 1.386(6) . ? C8A C10A 1.512(6) . ? C10A N4A 1.491(5) . ? N4A C11A 1.473(5) . ? C11A C12A 1.526(6) . ? C12A N2 1.465(5) . ? N2 C12B 1.481(5) . ? N2 C12C 1.486(4) . ? C1B C2B 1.524(5) . ? C2B N3B 1.491(5) . ? N3B C3B 1.490(5) . ? C3B C4B 1.514(6) . ? C4B C5B 1.378(6) . ? C4B C9B 1.385(6) . ? C5B C6B 1.387(6) . ? C6B C7B 1.393(6) . ? C7B C8B 1.399(6) . ? C8B C9B 1.394(6) . ? C8B C10B 1.493(6) . ? C10B N4B 1.500(5) . ? N4B C11B 1.502(5) . ? C11B C12B 1.510(6) . ? C1C C2C 1.512(5) . ? C2C N3C 1.494(5) . ? N3C C3C 1.501(4) . ? C3C C4C 1.503(5) . ? C4C C5C 1.392(5) . ? C4C C9C 1.398(5) . ? C5C C6C 1.389(5) . ? C6C C7C 1.395(6) . ? C7C C8C 1.381(5) . ? C8C C9C 1.399(5) . ? C8C C10C 1.497(5) . ? C10C N4C 1.502(4) . ? N4C C11C 1.495(4) . ? C11C C12C 1.522(5) . ? S1 O1 1.469(3) . ? S1 O4 1.475(3) . ? S1 O3 1.484(3) . ? S1 S2 1.9937(13) . ? Cl1 O12 1.421(4) . ? Cl1 O14 1.421(3) . ? Cl1 O11 1.435(3) . ? Cl1 O13 1.449(3) . ? Cl2 O21 1.413(4) . ? Cl2 O24 1.422(4) . ? Cl2 O22 1.427(3) . ? Cl2 O23 1.435(3) . ? Cl3 O31 1.387(5) . ? Cl3 O32 1.416(7) . ? Cl3 O33 1.449(7) . ? Cl3 O34 1.468(8) . ? Cl4 O41 1.392(7) . ? Cl4 O43 1.439(6) . ? Cl4 O44 1.469(7) . ? Cl4 O42 1.482(8) . ? 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 C1C N1 C1B 109.3(3) . . ? C1C N1 C1A 108.2(3) . . ? C1B N1 C1A 108.4(3) . . ? N1 C1A C2A 112.6(3) . . ? N3A C2A C1A 112.2(3) . . ? C3A N3A C2A 112.3(3) . . ? N3A C3A C4A 112.9(3) . . ? C9A C4A C5A 118.9(4) . . ? C9A C4A C3A 119.1(4) . . ? C5A C4A C3A 122.0(4) . . ? C6A C5A C4A 120.7(4) . . ? C5A C6A C7A 120.3(4) . . ? C8A C7A C6A 119.6(4) . . ? C7A C8A C9A 119.9(4) . . ? C7A C8A C10A 120.5(4) . . ? C9A C8A C10A 119.6(4) . . ? C4A C9A C8A 120.6(4) . . ? N4A C10A C8A 112.8(3) . . ? C11A N4A C10A 111.4(3) . . ? N4A C11A C12A 111.9(3) . . ? N2 C12A C11A 113.5(3) . . ? C12A N2 C12B 109.1(3) . . ? C12A N2 C12C 108.2(3) . . ? C12B N2 C12C 107.7(3) . . ? N1 C1B C2B 113.7(3) . . ? N3B C2B C1B 112.1(3) . . ? C3B N3B C2B 111.9(3) . . ? N3B C3B C4B 111.4(3) . . ? C5B C4B C9B 119.6(4) . . ? C5B C4B C3B 119.4(4) . . ? C9B C4B C3B 120.9(4) . . ? C4B C5B C6B 119.8(4) . . ? C5B C6B C7B 120.8(4) . . ? C6B C7B C8B 119.8(4) . . ? C9B C8B C7B 118.4(4) . . ? C9B C8B C10B 121.6(4) . . ? C7B C8B C10B 119.8(4) . . ? C4B C9B C8B 121.6(4) . . ? C8B C10B N4B 114.7(3) . . ? C10B N4B C11B 109.7(3) . . ? N4B C11B C12B 112.5(3) . . ? N2 C12B C11B 113.7(3) . . ? N1 C1C C2C 112.0(3) . . ? N3C C2C C1C 112.6(3) . . ? C2C N3C C3C 111.3(3) . . ? N3C C3C C4C 113.4(3) . . ? C5C C4C C9C 118.7(3) . . ? C5C C4C C3C 121.6(3) . . ? C9C C4C C3C 119.7(3) . . ? C6C C5C C4C 120.6(4) . . ? C5C C6C C7C 120.0(3) . . ? C8C C7C C6C 120.4(3) . . ? C7C C8C C9C 119.2(3) . . ? C7C C8C C10C 120.4(3) . . ? C9C C8C C10C 120.4(3) . . ? C4C C9C C8C 121.1(3) . . ? C8C C10C N4C 112.1(3) . . ? C11C N4C C10C 112.4(3) . . ? N4C C11C C12C 111.2(3) . . ? N2 C12C C11C 113.9(3) . . ? O1 S1 O4 109.25(16) . . ? O1 S1 O3 108.64(16) . . ? O4 S1 O3 108.27(15) . . ? O1 S1 S2 111.96(13) . . ? O4 S1 S2 109.20(11) . . ? O3 S1 S2 109.44(11) . . ? O12 Cl1 O14 109.7(2) . . ? O12 Cl1 O11 111.9(3) . . ? O14 Cl1 O11 110.7(2) . . ? O12 Cl1 O13 108.4(2) . . ? O14 Cl1 O13 108.5(2) . . ? O11 Cl1 O13 107.5(2) . . ? O21 Cl2 O24 110.7(3) . . ? O21 Cl2 O22 109.8(3) . . ? O24 Cl2 O22 108.7(2) . . ? O21 Cl2 O23 110.0(2) . . ? O24 Cl2 O23 109.4(2) . . ? O22 Cl2 O23 108.2(2) . . ? O31 Cl3 O32 125.9(5) . . ? O31 Cl3 O33 100.2(4) . . ? O32 Cl3 O33 107.8(5) . . ? O31 Cl3 O34 106.9(5) . . ? O32 Cl3 O34 106.7(6) . . ? O33 Cl3 O34 108.4(7) . . ? O41 Cl4 O43 111.8(5) . . ? O41 Cl4 O44 109.8(7) . . ? O43 Cl4 O44 105.0(6) . . ? O41 Cl4 O42 116.0(6) . . ? O43 Cl4 O42 107.4(5) . . ? O44 Cl4 O42 106.1(4) . . ? 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 N3A H3A2 O5W 0.92 2.18 2.871(5) 131.0 . N3A H3A1 O4 0.92 1.95 2.861(4) 171.4 . N3A H3A1 O1 0.92 2.62 3.214(5) 123.0 . N4A H4A2 O9W 0.92 2.03 2.802(5) 140.9 . N4A H4A2 O4W 0.92 2.28 2.934(5) 128.1 . N4A H4A1 S2 0.92 2.54 3.455(3) 170.8 . N3B H3B1 O3 0.92 2.09 2.957(4) 157.5 . N3B H3B1 O1 0.92 2.33 3.059(4) 135.8 . N3B H3B2 O8W 0.92 1.99 2.904(5) 173.8 3_565 N4B H4B1 O7W 0.92 2.01 2.803(5) 143.6 . N4B H4B1 O32 0.92 2.53 3.178(9) 128.1 . N4B H4B2 S2 0.92 2.38 3.298(3) 173.6 . N3C H3C1 O11 0.92 2.12 2.989(5) 156.5 2_545 N3C H3C2 O3 0.92 1.95 2.852(4) 166.1 . N3C H3C2 O4 0.92 2.46 3.087(4) 125.4 . N4C H4C1 O4W 0.92 2.27 2.959(4) 131.1 . N4C H4C1 S2 0.92 2.72 3.491(3) 141.9 . N4C H4C2 O1W 0.92 1.85 2.764(4) 173.2 . O1W H1WA O2W 0.85 1.86 2.705(4) 179.1 . O1W H1WB O3W 0.85 2.27 3.042(4) 150.5 2 O1W H1WB O23 0.85 2.54 3.001(4) 115.3 2_645 O2W H2WA O3 0.85 1.95 2.781(4) 164.6 . O2W H2WB O13 0.85 2.14 2.981(4) 171.1 2_545 O3W H3WA O4 0.85 1.87 2.712(4) 171.8 . O3W H3WB O21 0.85 2.10 2.917(5) 160.5 1_445 O4W H4WA O13 0.85 2.05 2.853(4) 158.1 1_545 O4W H4WB O3W 0.85 1.93 2.772(4) 173.5 . O5W H5WA O11W 0.85 2.08 2.925(6) 179.0 . O5W H5WB O24 0.85 2.67 3.114(5) 113.9 1_445 O6W H6WA O1 0.85 1.83 2.681(4) 179.5 . O6W H6WB O7W 0.85 1.86 2.715(6) 179.7 . O6W H6WC O6W 0.85 2.04 2.886(7) 179.7 3_565 O7W H7WA O6W 0.85 1.87 2.715(6) 179.3 . O7W H7WB O8W 0.85 2.21 2.989(6) 152.2 . O7W H7WB O32 0.85 2.64 3.172(8) 121.6 . O8W H8WA O7W 0.85 2.26 2.989(6) 144.1 . O8W H8WB O43 0.85 2.13 2.977(8) 178.9 4_665 O9W H9WA O11W 0.85 1.96 2.787(6) 162.4 3 O9W H9WB O10W 0.85 2.12 2.845(6) 143.4 1_545 O10W H1WC O44' 0.85 1.82 2.67(2) 178.4 2 O10W H1WC O41 0.85 2.20 3.052(12) 176.6 2 O10W H1WD O33 0.85 2.05 2.764(11) 141.4 . O10W H1WD O34' 0.85 2.32 3.166(19) 178.5 . O11W H1WE O10W 0.85 1.86 2.705(7) 174.6 1_445 O11W H1WF O31 0.85 2.10 2.911(8) 159.5 3_565 O11W H1WF O31' 0.85 2.10 2.911(8) 159.5 3_565 _diffrn_measured_fraction_theta_max 0.996 _diffrn_reflns_theta_full 25.00 _diffrn_measured_fraction_theta_full 0.996 _refine_diff_density_max 0.895 _refine_diff_density_min -0.934 _refine_diff_density_rms 0.092