Supplementary data for Dalton Transactions This journal is (c) The Royal Society of Chemistry 2007 data_global _journal_name_full 'Dalton Trans.' _journal_coden_cambridge 0222 _publ_contact_author ;Prof. Myoung Soo Lah Chemistry and Applied Chemistry Hanyang University 1271 Sa-1-dong Ansan Kyunggi-do 426-791 SOUTH KOREA ; _publ_contact_author_email MSLAH@HANYANG.AC.KR _publ_contact_author_name 'Prof. Myoung Soo Lah' loop_ _publ_author_name 'Myoung Soo Lah' 'Rohith P. John ' 'Ghyung Hwa Kim.' 'Kyungjin Lee. ' ; Dohyun Moon ; 'Mira Park. ' data_structure1 _database_code_depnum_ccdc_archive 'CCDC 644811' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C150 H169 Ga6 N12 O33.50' _chemical_formula_weight 3094.29 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' Ga Ga 0.2307 1.6083 '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 16.918(3) _cell_length_b 27.325(6) _cell_length_c 16.928(3) _cell_angle_alpha 90.00 _cell_angle_beta 107.05(3) _cell_angle_gamma 90.00 _cell_volume 7482(3) _cell_formula_units_Z 2 _cell_measurement_temperature 99(2) _cell_measurement_reflns_used 41821 _cell_measurement_theta_min 1.47 _cell_measurement_theta_max 30.44 _exptl_crystal_description block _exptl_crystal_colour colorless _exptl_crystal_size_max 0.20 _exptl_crystal_size_mid 0.20 _exptl_crystal_size_min 0.10 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.374 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 3214 _exptl_absorpt_coefficient_mu 1.143 _exptl_absorpt_correction_type empirical _exptl_absorpt_correction_T_min 0.8037 _exptl_absorpt_correction_T_max 0.8943 _exptl_absorpt_process_details HKL2000-Scalepack _exptl_special_details ; ? ; _diffrn_ambient_temperature 99(2) _diffrn_radiation_wavelength 0.70000 _diffrn_radiation_type synchrotron _diffrn_radiation_source 'Fixed gap multiple wiggler beamline' _diffrn_radiation_monochromator 'Pt coated Si double crystal' _diffrn_measurement_device_type 'CCD area detector' _diffrn_measurement_method 'phi scans' _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 41821 _diffrn_reflns_av_R_equivalents 0.0511 _diffrn_reflns_av_sigmaI/netI 0.0599 _diffrn_reflns_limit_h_min 0 _diffrn_reflns_limit_h_max 24 _diffrn_reflns_limit_k_min -39 _diffrn_reflns_limit_k_max 39 _diffrn_reflns_limit_l_min -24 _diffrn_reflns_limit_l_max 23 _diffrn_reflns_theta_min 1.47 _diffrn_reflns_theta_max 30.44 _reflns_number_total 23484 _reflns_number_gt 15096 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'PAL ADSC Quantum-210' _computing_cell_refinement HKL2000 _computing_data_reduction HKL2000 _computing_structure_solution 'Bruker SHELXTL' _computing_structure_refinement 'Bruker SHELXTL' _computing_molecular_graphics ORTEP3 _computing_publication_material WinGX _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^)+(0.1157P)^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 SHELXL _refine_ls_extinction_coef 0.0077(4) _refine_ls_extinction_expression Fc^*^=kFc[1+0.001xFc^2^\l^3^/sin(2\q)]^-1/4^ _refine_ls_number_reflns 23484 _refine_ls_number_parameters 959 _refine_ls_number_restraints 3 _refine_ls_R_factor_all 0.0905 _refine_ls_R_factor_gt 0.0589 _refine_ls_wR_factor_ref 0.1924 _refine_ls_wR_factor_gt 0.1717 _refine_ls_goodness_of_fit_ref 1.024 _refine_ls_restrained_S_all 1.025 _refine_ls_shift/su_max 0.001 _refine_ls_shift/su_mean 0.000 loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_occupancy _atom_site_symmetry_multiplicity _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group Ga1 Ga 0.968347(17) -0.008780(10) 0.77262(2) 0.04178(9) Uani 1 1 d . . . O1A O 0.94382(12) -0.06839(7) 0.81802(13) 0.0497(5) Uani 1 1 d . . . O2A O 0.72272(11) -0.02642(7) 0.62739(13) 0.0474(4) Uani 1 1 d . A . O3A O 0.97203(11) 0.05382(7) 0.71341(13) 0.0460(4) Uani 1 1 d . A . O4A O 0.92664(14) 0.02911(8) 0.85653(15) 0.0555(5) Uani 1 1 d . . . H4OA H 0.872(3) 0.0288(15) 0.836(3) 0.083 Uiso 1 1 d . . . N1A N 0.85825(13) -0.00941(8) 0.68914(15) 0.0425(5) Uani 1 1 d . . . N2A N 0.84369(13) 0.03034(8) 0.63381(16) 0.0448(5) Uani 1 1 d . A . C1A C 0.87077(17) -0.09183(10) 0.80229(19) 0.0464(6) Uani 1 1 d . A . C2A C 0.79879(17) -0.07927(10) 0.73575(19) 0.0451(6) Uani 1 1 d . . . C3A C 0.72971(18) -0.11015(10) 0.7190(2) 0.0497(6) Uani 1 1 d . A . H3A H 0.6827 -0.1023 0.6741 0.060 Uiso 1 1 calc R . . C4A C 0.72699(19) -0.15186(10) 0.7655(2) 0.0520(7) Uani 1 1 d . . . C5A C 0.6580(2) -0.18417(11) 0.7464(2) 0.0601(8) Uani 1 1 d . A . H5A H 0.6120 -0.1779 0.6995 0.072 Uiso 1 1 calc R . . C6A C 0.6573(2) -0.22375(12) 0.7945(3) 0.0662(9) Uani 1 1 d . . . H6A H 0.6115 -0.2455 0.7801 0.079 Uiso 1 1 calc R A . C7A C 0.7238(2) -0.23297(12) 0.8658(3) 0.0691(10) Uani 1 1 d . A . H7A H 0.7212 -0.2600 0.9003 0.083 Uiso 1 1 calc R . . C8A C 0.7924(2) -0.20322(11) 0.8857(2) 0.0611(8) Uani 1 1 d . . . H8A H 0.8374 -0.2102 0.9331 0.073 Uiso 1 1 calc R A . C9A C 0.79601(19) -0.16209(10) 0.8355(2) 0.0521(7) Uani 1 1 d . A . C10A C 0.86568(19) -0.13102(10) 0.8511(2) 0.0505(6) Uani 1 1 d . . . H10A H 0.9115 -0.1377 0.8980 0.061 Uiso 1 1 calc R A . C11A C 0.79221(16) -0.03640(10) 0.68170(19) 0.0444(6) Uani 1 1 d . A . C12A C 0.90723(17) 0.06128(10) 0.65264(19) 0.0457(6) Uani 1 1 d . . . C13A C 0.89868(17) 0.10532(10) 0.60331(19) 0.0472(6) Uani 1 1 d . A . H13A H 0.8522 0.1084 0.5558 0.057 Uiso 1 1 calc R . . C14A C 0.95364(17) 0.14175(10) 0.6221(2) 0.0471(6) Uani 1 1 d . . . H14A H 1.0014 0.1369 0.6678 0.056 Uiso 1 1 calc R A . C15A C 0.94678(17) 0.18862(10) 0.5784(2) 0.0474(6) Uani 1 1 d . A . C16A C 0.99709(19) 0.22743(10) 0.6176(2) 0.0533(7) Uani 1 1 d . . . H16A H 1.0369 0.2223 0.6697 0.064 Uiso 1 1 calc R A . C17A C 0.9893(2) 0.27343(11) 0.5810(3) 0.0646(9) Uani 1 1 d . A . H17A H 1.0222 0.2998 0.6092 0.078 Uiso 1 1 calc R . . C18A C 0.9346(2) 0.28087(13) 0.5049(3) 0.0703(10) Uani 1 1 d . . . H18A H 0.9296 0.3124 0.4802 0.084 Uiso 1 1 calc R A . C19A C 0.8858(2) 0.24229(13) 0.4632(2) 0.0648(9) Uani 1 1 d . A . H19A H 0.8485 0.2473 0.4097 0.078 Uiso 1 1 calc R . . C20A C 0.89195(18) 0.19666(11) 0.5003(2) 0.0538(7) Uani 1 1 d . . . H20A H 0.8584 0.1705 0.4720 0.065 Uiso 1 1 calc R A . C21A C 0.9605(4) 0.0762(2) 0.8928(5) 0.0603(17) Uani 0.50 1 d P A 1 H21A H 0.9395 0.1030 0.8527 0.072 Uiso 0.50 1 calc PR A 1 H21B H 1.0216 0.0758 0.9070 0.072 Uiso 0.50 1 calc PR A 1 C22A C 0.9337(5) 0.0848(3) 0.9712(4) 0.152(3) Uani 0.50 1 d P A 1 C211 C 0.9547(9) 0.0341(5) 0.9406(6) 0.129(5) Uani 0.50 1 d P A 2 H21C H 1.0155 0.0296 0.9590 0.155 Uiso 0.50 1 calc PR A 2 H21D H 0.9300 0.0081 0.9665 0.155 Uiso 0.50 1 calc PR A 2 C221 C 0.9337(5) 0.0848(3) 0.9712(4) 0.152(3) Uani 0.50 1 d P A 2 Ga2 Ga 0.733951(17) 0.019838(11) 0.54413(2) 0.04325(9) Uani 1 1 d . . . O1B O 0.68550(13) 0.07769(8) 0.57368(14) 0.0521(5) Uani 1 1 d . A . O2B O 0.72994(11) 0.10971(7) 0.34278(12) 0.0445(4) Uani 1 1 d . A . O3B O 0.78492(12) -0.03322(7) 0.49324(13) 0.0457(4) Uani 1 1 d . A . O4B O 0.62012(13) -0.00210(9) 0.47102(15) 0.0523(5) Uani 1 1 d . A . H4OB H 0.613(3) 0.0019(17) 0.428(3) 0.078 Uiso 1 1 d . . . N1B N 0.75197(13) 0.05469(8) 0.44791(14) 0.0413(5) Uani 1 1 d . A . N2B N 0.79053(13) 0.02683(8) 0.40052(15) 0.0425(5) Uani 1 1 d . . . C1B C 0.65161(16) 0.11523(10) 0.5251(2) 0.0477(6) Uani 1 1 d . . . C2B C 0.66843(15) 0.12677(10) 0.44898(19) 0.0458(6) Uani 1 1 d . A . C3B C 0.63227(17) 0.16749(10) 0.4045(2) 0.0516(7) Uani 1 1 d . . . H3B H 0.6440 0.1745 0.3542 0.062 Uiso 1 1 calc R A . C4B C 0.57929(18) 0.19890(10) 0.4300(2) 0.0558(8) Uani 1 1 d . A . C5B C 0.5411(2) 0.24042(11) 0.3845(3) 0.0640(9) Uani 1 1 d . . . H5B H 0.5509 0.2474 0.3331 0.077 Uiso 1 1 calc R A . C6B C 0.4914(2) 0.27036(12) 0.4117(3) 0.0735(11) Uani 1 1 d . A . H6B H 0.4668 0.2980 0.3800 0.088 Uiso 1 1 calc R . . C7B C 0.4764(2) 0.26043(12) 0.4867(3) 0.0735(11) Uani 1 1 d . . . H7B H 0.4418 0.2818 0.5060 0.088 Uiso 1 1 calc R A . C8B C 0.5103(2) 0.22061(12) 0.5329(3) 0.0691(10) Uani 1 1 d . A . H8B H 0.4986 0.2144 0.5835 0.083 Uiso 1 1 calc R . . C9B C 0.56363(18) 0.18806(11) 0.5056(2) 0.0575(8) Uani 1 1 d . . . C10B C 0.59926(18) 0.14664(11) 0.5506(2) 0.0549(7) Uani 1 1 d . A . H10B H 0.5871 0.1397 0.6008 0.066 Uiso 1 1 calc R . . C11B C 0.71997(15) 0.09613(9) 0.41140(18) 0.0432(6) Uani 1 1 d . . . C12B C 0.80114(17) -0.01917(10) 0.4275(2) 0.0461(6) Uani 1 1 d . A . C13B C 0.82404(19) -0.05449(11) 0.3717(2) 0.0528(7) Uani 1 1 d . . . H13B H 0.8523 -0.0431 0.3343 0.063 Uiso 1 1 calc R A . C14B C 0.80598(18) -0.10207(11) 0.3727(2) 0.0541(7) Uani 1 1 d . A . H14B H 0.7885 -0.1133 0.4180 0.065 Uiso 1 1 calc R . . C15B C 0.81047(18) -0.13852(11) 0.3106(2) 0.0523(7) Uani 1 1 d . . . C16B C 0.7813(2) -0.18564(11) 0.3156(2) 0.0620(8) Uani 1 1 d . A . H16B H 0.7635 -0.1945 0.3619 0.074 Uiso 1 1 calc R . . C17B C 0.7778(2) -0.22016(13) 0.2540(3) 0.0710(10) Uani 1 1 d . . . H17B H 0.7573 -0.2521 0.2583 0.085 Uiso 1 1 calc R A . C18B C 0.8039(2) -0.20801(13) 0.1870(3) 0.0664(9) Uani 1 1 d . A . H18B H 0.7999 -0.2312 0.1442 0.080 Uiso 1 1 calc R . . C19B C 0.8362(2) -0.16153(12) 0.1817(2) 0.0629(8) Uani 1 1 d . . . H19B H 0.8556 -0.1532 0.1361 0.075 Uiso 1 1 calc R A . C20B C 0.8400(2) -0.12732(11) 0.2440(2) 0.0576(8) Uani 1 1 d . A . H20B H 0.8630 -0.0959 0.2410 0.069 Uiso 1 1 calc R . . C21B C 0.5714(2) -0.04364(16) 0.4845(3) 0.0790(12) Uani 1 1 d . . . H21E H 0.5728 -0.0446 0.5433 0.095 Uiso 1 1 calc R A . H21F H 0.5131 -0.0392 0.4509 0.095 Uiso 1 1 calc R . . C22B C 0.6021(3) -0.08993(16) 0.4625(4) 0.114(2) Uani 1 1 d . A . H22A H 0.5899 -0.0920 0.4023 0.171 Uiso 1 1 calc R . . H22B H 0.5752 -0.1171 0.4823 0.171 Uiso 1 1 calc R . . H22C H 0.6620 -0.0918 0.4882 0.171 Uiso 1 1 calc R . . Ga3 Ga 0.797494(17) 0.065650(10) 0.299731(19) 0.04168(9) Uani 1 1 d . A . O1C O 0.70666(11) 0.03136(7) 0.22787(13) 0.0491(5) Uani 1 1 d . . . O2C O 0.92166(11) -0.00463(7) 0.15363(13) 0.0444(4) Uani 1 1 d . . . O3C O 0.90198(11) 0.09682(7) 0.36111(12) 0.0442(4) Uani 1 1 d . . . O4C O 0.79043(13) 0.11916(8) 0.21003(14) 0.0540(5) Uani 1 1 d . . . H4OC H 0.830(3) 0.1228(15) 0.186(3) 0.081 Uiso 1 1 d . . . N1C N 0.87645(13) 0.02884(8) 0.25580(15) 0.0423(5) Uani 1 1 d . . . N2C N 0.95945(13) 0.04344(8) 0.28999(15) 0.0424(5) Uani 1 1 d . . . C1C C 0.70566(16) 0.00169(9) 0.16485(18) 0.0424(6) Uani 1 1 d . A . C2C C 0.77833(16) -0.01175(9) 0.14185(18) 0.0410(5) Uani 1 1 d . . . C3C C 0.77019(16) -0.04330(9) 0.07627(18) 0.0440(6) Uani 1 1 d . A . H3C H 0.8185 -0.0525 0.0621 0.053 Uiso 1 1 calc R . . C4C C 0.69371(17) -0.06236(9) 0.02952(19) 0.0455(6) Uani 1 1 d . . . C5C C 0.68571(18) -0.09490(10) -0.0383(2) 0.0520(7) Uani 1 1 d . A . H5C H 0.7338 -0.1058 -0.0512 0.062 Uiso 1 1 calc R . . C6C C 0.60958(19) -0.11047(11) -0.0846(2) 0.0554(7) Uani 1 1 d . . . H6C H 0.6046 -0.1317 -0.1303 0.067 Uiso 1 1 calc R A . C7C C 0.53815(18) -0.09477(11) -0.0644(2) 0.0534(7) Uani 1 1 d . A . H7C H 0.4853 -0.1056 -0.0971 0.064 Uiso 1 1 calc R . . C8C C 0.54337(17) -0.06443(10) 0.0009(2) 0.0476(6) Uani 1 1 d . . . H8C H 0.4945 -0.0545 0.0132 0.057 Uiso 1 1 calc R A . C9C C 0.62141(16) -0.04758(9) 0.05050(18) 0.0435(6) Uani 1 1 d . A . C10C C 0.63019(16) -0.01619(9) 0.11808(18) 0.0439(6) Uani 1 1 d . . . H10C H 0.5820 -0.0068 0.1323 0.053 Uiso 1 1 calc R A . C11C C 0.86226(15) 0.00493(9) 0.18489(18) 0.0407(5) Uani 1 1 d . A . C12C C 0.96563(16) 0.07956(10) 0.34383(18) 0.0429(6) Uani 1 1 d . A . C13C C 1.04578(17) 0.10205(10) 0.37815(18) 0.0456(6) Uani 1 1 d . . . H13C H 1.0942 0.0857 0.3747 0.055 Uiso 1 1 calc R A . C14C C 1.05190(19) 0.14581(10) 0.4147(2) 0.0524(7) Uani 1 1 d . A . H14C H 1.0031 0.1579 0.4248 0.063 Uiso 1 1 calc R . . C15C C 1.1252(2) 0.17746(12) 0.4411(2) 0.0577(8) Uani 1 1 d . . . C16C C 1.1133(3) 0.22579(13) 0.4616(3) 0.0763(11) Uani 1 1 d . A . H16C H 1.0594 0.2365 0.4602 0.092 Uiso 1 1 calc R . . C17C C 1.1786(3) 0.25841(15) 0.4839(3) 0.0866(13) Uani 1 1 d . . . H17C H 1.1701 0.2910 0.4991 0.104 Uiso 1 1 calc R A . C18C C 1.2560(3) 0.24319(15) 0.4838(3) 0.0830(12) Uani 1 1 d . A . H18C H 1.3010 0.2656 0.4986 0.100 Uiso 1 1 calc R . . C19C C 1.2692(2) 0.19622(15) 0.4626(3) 0.0719(10) Uani 1 1 d . . . H19C H 1.3230 0.1860 0.4631 0.086 Uiso 1 1 calc R A . C20C C 1.2035(2) 0.16358(13) 0.4405(2) 0.0628(8) Uani 1 1 d . A . H20C H 1.2125 0.1312 0.4247 0.075 Uiso 1 1 calc R . . C21C C 0.7176(2) 0.13692(14) 0.1513(3) 0.0754(11) Uani 1 1 d . A . H21G H 0.7210 0.1730 0.1480 0.091 Uiso 1 1 calc R . . H21H H 0.6692 0.1290 0.1706 0.091 Uiso 1 1 calc R . . C22C C 0.7048(4) 0.11565(15) 0.0670(3) 0.1055(18) Uani 1 1 d . . . H22D H 0.7476 0.1280 0.0437 0.158 Uiso 1 1 calc R A . H22E H 0.6502 0.1252 0.0312 0.158 Uiso 1 1 calc R . . H22F H 0.7083 0.0799 0.0710 0.158 Uiso 1 1 calc R . . O1S O 0.76969(17) 0.03454(11) 0.8286(2) 0.0611(8) Uani 0.75 1 d P B 1 H1S H 0.7428 0.0538 0.7918 0.092 Uiso 0.75 1 calc PR B 1 C11S C 0.7154(3) 0.00459(17) 0.8538(3) 0.0619(11) Uani 0.75 1 d P B 1 H11E H 0.7478 -0.0172 0.8983 0.074 Uiso 0.75 1 calc PR B 1 H11F H 0.6857 -0.0164 0.8067 0.074 Uiso 0.75 1 calc PR B 1 C12S C 0.6557(3) 0.03029(18) 0.8831(4) 0.0725(14) Uani 0.75 1 d P B 1 H12G H 0.6832 0.0566 0.9204 0.109 Uiso 0.75 1 calc PR B 1 H12H H 0.6298 0.0075 0.9129 0.109 Uiso 0.75 1 calc PR B 1 H12I H 0.6132 0.0443 0.8361 0.109 Uiso 0.75 1 calc PR B 1 O2S O 0.92909(15) 0.14067(9) 0.16913(17) 0.0668(6) Uani 1 1 d . . . H2S H 0.9607 0.1202 0.1571 0.100 Uiso 1 1 calc R . . C21S C 0.9751(2) 0.18473(12) 0.2012(2) 0.0650(9) Uani 1 1 d . . . H21I H 0.9970 0.1995 0.1585 0.078 Uiso 1 1 calc R . . H21J H 1.0225 0.1766 0.2498 0.078 Uiso 1 1 calc R . . C22S C 0.9190(3) 0.22024(15) 0.2256(3) 0.0904(13) Uani 1 1 d . . . H22G H 0.8689 0.2249 0.1792 0.136 Uiso 1 1 calc R . . H22H H 0.9475 0.2517 0.2402 0.136 Uiso 1 1 calc R . . H22I H 0.9039 0.2074 0.2732 0.136 Uiso 1 1 calc R . . O3S O 0.4624(3) 0.8665(3) 0.2661(4) 0.198(3) Uani 1 1 d D . . H3S H 0.4155 0.8534 0.2503 0.298 Uiso 1 1 calc R . . C31S C 0.4966(6) 0.8686(5) 0.1996(7) 0.283(8) Uani 1 1 d D . . H31A H 0.4706 0.8424 0.1600 0.340 Uiso 1 1 calc R . . H31B H 0.4805 0.9002 0.1709 0.340 Uiso 1 1 calc R . . C32S C 0.5806(5) 0.8639(3) 0.2174(6) 0.176(4) Uani 1 1 d D . . H32A H 0.6070 0.8954 0.2369 0.264 Uiso 1 1 calc R . . H32B H 0.5946 0.8540 0.1675 0.264 Uiso 1 1 calc R . . H32C H 0.6004 0.8391 0.2605 0.264 Uiso 1 1 calc R . . O4S O 0.7034(2) 0.10771(11) 0.7301(2) 0.0619(8) Uani 0.75 1 d P C 1 H4S H 0.7024 0.0943 0.6852 0.093 Uiso 0.75 1 calc PR C 1 C41S C 0.7596(4) 0.15067(18) 0.7442(3) 0.0728(13) Uani 0.75 1 d P C 1 H41A H 0.8169 0.1397 0.7504 0.087 Uiso 0.75 1 calc PR C 1 H41B H 0.7427 0.1730 0.6961 0.087 Uiso 0.75 1 calc PR C 1 C42S C 0.7566(4) 0.1761(2) 0.8172(3) 0.0786(15) Uani 0.75 1 d P C 1 H42A H 0.7016 0.1906 0.8082 0.118 Uiso 0.75 1 calc PR C 1 H42B H 0.7984 0.2020 0.8299 0.118 Uiso 0.75 1 calc PR C 1 H42C H 0.7675 0.1531 0.8636 0.118 Uiso 0.75 1 calc PR C 1 O51S O 0.59399(14) 0.00944(11) 0.31102(16) 0.0716(9) Uani 0.810(6) 1 d P D 1 H51S H 0.6280 0.0052 0.2841 0.107 Uiso 0.810(6) 1 calc PR D 1 C511 C 0.5320(4) 0.0511(3) 0.2698(4) 0.102(2) Uani 0.810(6) 1 d P D 1 H51A H 0.5644 0.0797 0.2611 0.122 Uiso 0.810(6) 1 calc PR D 1 H51B H 0.4985 0.0396 0.2147 0.122 Uiso 0.810(6) 1 calc PR D 1 C521 C 0.4826(4) 0.0653(2) 0.3099(4) 0.122(2) Uani 0.810(6) 1 d P D 1 O52S O 0.59399(14) 0.00944(11) 0.31102(16) 0.0716(9) Uani 0.19 1 d P D 2 H52S H 0.6028 -0.0168 0.3381 0.107 Uiso 0.190(6) 1 calc PR D 2 C512 C 0.5108(6) 0.0162(4) 0.2784(6) 0.020(2) Uiso 0.190(6) 1 d P D 2 H51C H 0.4810 -0.0115 0.2943 0.024 Uiso 0.190(6) 1 calc PR D 2 H51D H 0.4964 0.0169 0.2173 0.024 Uiso 0.190(6) 1 calc PR D 2 C522 C 0.4826(4) 0.0653(2) 0.3099(4) 0.122(2) Uani 0.19 1 d P D 2 O1W O 0.6514(12) 0.0594(7) 0.7211(12) 0.134(6) Uiso 0.25 1 d P 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 Ga1 0.03080(15) 0.03545(15) 0.05702(19) -0.00682(12) 0.00964(12) -0.00195(10) O1A 0.0386(10) 0.0461(10) 0.0623(12) 0.0017(9) 0.0114(9) -0.0053(8) O2A 0.0333(9) 0.0476(10) 0.0599(12) -0.0027(9) 0.0112(8) -0.0063(8) O3A 0.0329(9) 0.0375(9) 0.0619(12) -0.0035(8) 0.0050(8) -0.0057(7) O4A 0.0409(11) 0.0571(12) 0.0679(14) -0.0208(11) 0.0149(10) -0.0047(9) N1A 0.0316(10) 0.0361(10) 0.0563(13) -0.0042(9) 0.0077(9) -0.0041(8) N2A 0.0313(10) 0.0393(11) 0.0597(14) -0.0017(10) 0.0071(9) -0.0031(9) C1A 0.0363(13) 0.0419(13) 0.0626(17) -0.0063(12) 0.0172(12) -0.0019(11) C2A 0.0393(13) 0.0376(12) 0.0601(16) -0.0088(12) 0.0171(12) -0.0042(10) C3A 0.0408(14) 0.0422(14) 0.0695(18) -0.0101(13) 0.0216(13) -0.0058(11) C4A 0.0497(16) 0.0382(13) 0.076(2) -0.0108(13) 0.0306(15) -0.0048(12) C5A 0.0562(18) 0.0452(15) 0.089(2) -0.0153(16) 0.0370(17) -0.0105(13) C6A 0.067(2) 0.0428(15) 0.100(3) -0.0119(17) 0.042(2) -0.0141(15) C7A 0.079(2) 0.0413(15) 0.104(3) -0.0052(17) 0.054(2) -0.0094(16) C8A 0.066(2) 0.0461(15) 0.080(2) -0.0031(15) 0.0342(18) 0.0015(14) C9A 0.0520(16) 0.0390(13) 0.074(2) -0.0069(13) 0.0321(15) -0.0026(12) C10A 0.0452(15) 0.0434(14) 0.0652(18) -0.0036(13) 0.0200(13) 0.0010(12) C11A 0.0346(12) 0.0386(12) 0.0608(16) -0.0084(12) 0.0154(11) -0.0041(10) C12A 0.0339(12) 0.0375(12) 0.0637(17) -0.0053(12) 0.0112(12) -0.0043(10) C13A 0.0348(13) 0.0410(13) 0.0622(17) 0.0008(12) 0.0084(12) -0.0019(10) C14A 0.0359(13) 0.0395(13) 0.0631(17) -0.0022(12) 0.0103(12) 0.0003(10) C15A 0.0399(14) 0.0369(12) 0.0658(18) -0.0017(12) 0.0162(12) 0.0020(11) C16A 0.0515(16) 0.0388(13) 0.0695(19) -0.0033(13) 0.0175(14) -0.0031(12) C17A 0.074(2) 0.0361(14) 0.086(2) -0.0030(15) 0.0253(19) -0.0014(14) C18A 0.078(2) 0.0460(17) 0.089(3) 0.0137(17) 0.027(2) 0.0097(16) C19A 0.067(2) 0.0539(18) 0.072(2) 0.0072(16) 0.0177(17) 0.0161(16) C20A 0.0437(15) 0.0462(15) 0.070(2) -0.0021(14) 0.0139(14) 0.0070(12) C21A 0.052(3) 0.047(3) 0.086(5) -0.022(3) 0.026(3) -0.004(3) C22A 0.196(7) 0.135(6) 0.113(5) -0.066(4) 0.025(5) 0.019(5) C211 0.167(11) 0.141(10) 0.071(6) 0.009(6) 0.025(7) 0.099(9) C221 0.196(7) 0.135(6) 0.113(5) -0.066(4) 0.025(5) 0.019(5) Ga2 0.02998(15) 0.04104(16) 0.05728(19) -0.00543(13) 0.01053(12) -0.00217(11) O1B 0.0433(11) 0.0516(11) 0.0626(13) -0.0116(10) 0.0176(9) 0.0024(9) O2B 0.0377(9) 0.0364(9) 0.0579(11) -0.0039(8) 0.0118(8) 0.0078(7) O3B 0.0399(10) 0.0377(9) 0.0599(12) -0.0019(8) 0.0154(9) 0.0005(8) O4B 0.0343(10) 0.0578(12) 0.0620(13) -0.0054(11) 0.0098(9) -0.0068(9) N1B 0.0314(10) 0.0384(10) 0.0537(13) -0.0045(9) 0.0115(9) 0.0037(8) N2B 0.0356(11) 0.0344(10) 0.0582(13) -0.0052(9) 0.0148(10) 0.0041(8) C1B 0.0337(13) 0.0408(13) 0.0678(18) -0.0114(13) 0.0136(12) -0.0020(10) C2B 0.0291(12) 0.0399(13) 0.0661(17) -0.0092(12) 0.0106(11) 0.0030(10) C3B 0.0381(14) 0.0402(13) 0.076(2) -0.0088(13) 0.0166(13) 0.0021(11) C4B 0.0372(14) 0.0397(13) 0.092(2) -0.0083(14) 0.0209(15) 0.0005(11) C5B 0.0491(17) 0.0424(15) 0.102(3) 0.0014(16) 0.0250(17) 0.0096(13) C6B 0.056(2) 0.0454(16) 0.122(3) 0.0004(19) 0.032(2) 0.0098(15) C7B 0.0533(19) 0.0484(17) 0.124(3) -0.015(2) 0.034(2) 0.0086(15) C8B 0.0510(18) 0.0518(17) 0.113(3) -0.0175(19) 0.0368(19) 0.0003(14) C9B 0.0398(14) 0.0389(13) 0.095(2) -0.0157(15) 0.0218(15) -0.0007(11) C10B 0.0412(15) 0.0481(15) 0.079(2) -0.0166(15) 0.0237(14) -0.0058(12) C11B 0.0307(12) 0.0337(11) 0.0616(17) -0.0075(11) 0.0080(11) 0.0006(9) C12B 0.0350(13) 0.0377(12) 0.0643(17) -0.0013(12) 0.0126(12) 0.0036(10) C13B 0.0453(15) 0.0406(13) 0.075(2) -0.0007(14) 0.0213(14) 0.0051(12) C14B 0.0451(15) 0.0417(14) 0.072(2) -0.0020(14) 0.0121(14) 0.0009(12) C15B 0.0429(15) 0.0389(13) 0.074(2) -0.0043(13) 0.0158(14) -0.0013(11) C16B 0.0570(18) 0.0446(15) 0.086(2) -0.0115(16) 0.0236(17) -0.0065(14) C17B 0.059(2) 0.0468(17) 0.106(3) -0.0130(19) 0.022(2) -0.0102(15) C18B 0.0514(18) 0.0545(18) 0.091(3) -0.0213(18) 0.0170(17) -0.0018(15) C19B 0.0591(19) 0.0520(17) 0.078(2) -0.0051(16) 0.0213(17) 0.0078(15) C20B 0.0562(18) 0.0378(14) 0.075(2) -0.0022(14) 0.0139(16) 0.0047(12) C21B 0.0464(19) 0.080(3) 0.101(3) 0.006(2) 0.0067(19) -0.0220(18) C22B 0.063(3) 0.064(3) 0.198(6) -0.006(3) 0.013(3) -0.016(2) Ga3 0.03336(15) 0.03493(15) 0.05473(18) -0.00711(12) 0.00976(12) 0.00104(10) O1C 0.0339(9) 0.0490(11) 0.0628(12) -0.0186(9) 0.0118(8) -0.0032(8) O2C 0.0330(9) 0.0426(9) 0.0557(11) -0.0101(8) 0.0100(8) -0.0017(7) O3C 0.0334(9) 0.0385(9) 0.0577(11) -0.0099(8) 0.0087(8) -0.0002(7) O4C 0.0447(11) 0.0537(12) 0.0600(13) 0.0072(10) 0.0101(9) 0.0074(9) N1C 0.0309(10) 0.0370(10) 0.0580(13) -0.0079(9) 0.0114(9) -0.0003(8) N2C 0.0317(10) 0.0358(10) 0.0568(13) -0.0077(9) 0.0083(9) -0.0019(8) C1C 0.0362(13) 0.0323(11) 0.0558(15) -0.0053(11) 0.0093(11) 0.0010(9) C2C 0.0324(12) 0.0330(11) 0.0535(15) -0.0038(10) 0.0061(10) 0.0001(9) C3C 0.0365(13) 0.0361(12) 0.0573(16) -0.0060(11) 0.0103(11) 0.0023(10) C4C 0.0361(13) 0.0345(12) 0.0628(17) -0.0068(11) 0.0095(12) -0.0007(10) C5C 0.0444(15) 0.0415(13) 0.0667(19) -0.0118(13) 0.0110(13) 0.0013(12) C6C 0.0475(16) 0.0456(15) 0.0672(19) -0.0173(14) 0.0075(14) -0.0056(12) C7C 0.0422(15) 0.0435(14) 0.0666(19) -0.0083(13) 0.0034(13) -0.0052(12) C8C 0.0362(13) 0.0367(12) 0.0647(18) -0.0044(12) 0.0066(12) -0.0019(10) C9C 0.0367(13) 0.0311(11) 0.0592(16) -0.0026(11) 0.0087(11) -0.0003(9) C10C 0.0339(12) 0.0363(12) 0.0591(16) -0.0036(11) 0.0099(11) 0.0010(10) C11C 0.0330(12) 0.0313(11) 0.0551(15) -0.0043(10) 0.0087(11) 0.0007(9) C12C 0.0355(13) 0.0368(12) 0.0544(15) -0.0044(11) 0.0102(11) -0.0005(10) C13C 0.0350(13) 0.0410(13) 0.0575(16) -0.0086(12) 0.0085(11) -0.0032(10) C14C 0.0454(15) 0.0419(14) 0.0707(19) -0.0083(13) 0.0185(14) -0.0043(12) C15C 0.0516(17) 0.0499(16) 0.075(2) -0.0165(15) 0.0238(15) -0.0119(13) C16C 0.068(2) 0.0492(18) 0.113(3) -0.021(2) 0.030(2) -0.0099(16) C17C 0.082(3) 0.053(2) 0.124(4) -0.021(2) 0.028(3) -0.0170(19) C18C 0.076(3) 0.073(2) 0.101(3) -0.024(2) 0.028(2) -0.036(2) C19C 0.057(2) 0.070(2) 0.093(3) -0.020(2) 0.0289(19) -0.0224(17) C20C 0.0557(18) 0.0609(19) 0.076(2) -0.0226(17) 0.0252(16) -0.0166(15) C21C 0.068(2) 0.061(2) 0.084(3) 0.0122(19) -0.0004(19) 0.0087(18) C22C 0.155(5) 0.054(2) 0.076(3) -0.001(2) -0.015(3) 0.000(3) O1S 0.0393(14) 0.0587(17) 0.089(2) 0.0209(16) 0.0248(14) 0.0019(13) C11S 0.052(2) 0.061(2) 0.079(3) 0.004(2) 0.028(2) -0.005(2) C12S 0.071(3) 0.058(3) 0.104(4) 0.004(3) 0.048(3) 0.010(2) O2S 0.0670(15) 0.0529(13) 0.0863(17) 0.0040(12) 0.0315(13) 0.0103(11) C21S 0.068(2) 0.0499(17) 0.083(2) 0.0026(17) 0.0303(18) 0.0036(16) C22S 0.091(3) 0.059(2) 0.126(4) -0.017(2) 0.039(3) 0.010(2) O3S 0.142(5) 0.311(9) 0.161(5) 0.014(5) 0.073(4) 0.027(5) C31S 0.226(11) 0.415(19) 0.273(13) 0.174(13) 0.175(11) 0.221(13) C32S 0.169(7) 0.139(6) 0.245(10) 0.080(6) 0.099(7) 0.047(5) O4S 0.076(2) 0.0489(16) 0.0634(19) -0.0001(14) 0.0244(16) 0.0047(15) C41S 0.098(4) 0.054(3) 0.066(3) 0.001(2) 0.024(3) -0.008(3) C42S 0.086(4) 0.073(3) 0.079(3) -0.019(3) 0.027(3) -0.004(3) O51S 0.0310(11) 0.115(2) 0.0659(16) -0.0118(14) 0.0092(10) 0.0018(12) C511 0.059(3) 0.155(7) 0.077(4) 0.010(4) -0.002(3) 0.020(4) C521 0.099(4) 0.119(4) 0.117(4) -0.024(3) -0.014(3) 0.059(3) O52S 0.0310(11) 0.115(2) 0.0659(16) -0.0118(14) 0.0092(10) 0.0018(12) C522 0.099(4) 0.119(4) 0.117(4) -0.024(3) -0.014(3) 0.059(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 Ga1 O1A 1.898(2) . ? Ga1 O2C 1.948(2) 3_756 ? Ga1 N1A 1.981(2) . ? Ga1 O3A 1.993(2) . ? Ga1 O4A 2.043(2) . ? Ga1 N2C 2.067(2) 3_756 ? O1A C1A 1.347(3) . ? O2A C11A 1.291(3) . ? O2A Ga2 1.944(2) . ? O3A C12A 1.281(3) . ? O4A C211 1.369(10) . ? O4A C21A 1.469(6) . ? N1A C11A 1.314(3) . ? N1A N2A 1.408(3) . ? N2A C12A 1.331(3) . ? N2A Ga2 2.045(2) . ? C1A C10A 1.371(4) . ? C1A C2A 1.437(4) . ? C2A C3A 1.401(4) . ? C2A C11A 1.470(4) . ? C3A C4A 1.393(4) . ? C4A C5A 1.423(4) . ? C4A C9A 1.427(5) . ? C5A C6A 1.356(5) . ? C6A C7A 1.410(6) . ? C7A C8A 1.375(5) . ? C8A C9A 1.421(4) . ? C9A C10A 1.413(4) . ? C12A C13A 1.448(4) . ? C13A C14A 1.335(4) . ? C14A C15A 1.467(4) . ? C15A C20A 1.392(4) . ? C15A C16A 1.399(4) . ? C16A C17A 1.390(4) . ? C17A C18A 1.363(5) . ? C18A C19A 1.396(5) . ? C19A C20A 1.386(5) . ? C21A C22A 1.540(10) . ? Ga2 O1B 1.913(2) . ? Ga2 N1B 1.986(2) . ? Ga2 O3B 2.0059(19) . ? Ga2 O4B 2.050(2) . ? O1B C1B 1.335(4) . ? O2B C11B 1.277(4) . ? O2B Ga3 1.9429(18) . ? O3B C12B 1.280(4) . ? O4B C21B 1.460(4) . ? N1B C11B 1.327(3) . ? N1B N2B 1.398(3) . ? N2B C12B 1.331(3) . ? N2B Ga3 2.042(2) . ? C1B C10B 1.390(4) . ? C1B C2B 1.434(4) . ? C2B C3B 1.381(4) . ? C2B C11B 1.480(4) . ? C3B C4B 1.397(4) . ? C4B C9B 1.412(5) . ? C4B C5B 1.416(5) . ? C5B C6B 1.348(5) . ? C6B C7B 1.391(6) . ? C7B C8B 1.365(6) . ? C8B C9B 1.436(4) . ? C9B C10B 1.398(5) . ? C12B C13B 1.479(4) . ? C13B C14B 1.337(4) . ? C14B C15B 1.467(4) . ? C15B C16B 1.390(4) . ? C15B C20B 1.394(5) . ? C16B C17B 1.394(5) . ? C17B C18B 1.373(6) . ? C18B C19B 1.396(5) . ? C19B C20B 1.397(5) . ? C21B C22B 1.457(6) . ? Ga3 O1C 1.903(2) . ? Ga3 O3C 1.9629(18) . ? Ga3 N1C 1.983(2) . ? Ga3 O4C 2.086(2) . ? O1C C1C 1.336(3) . ? O2C C11C 1.292(3) . ? O2C Ga1 1.948(2) 3_756 ? O3C C12C 1.285(3) . ? O4C C21C 1.422(4) . ? N1C C11C 1.325(3) . ? N1C N2C 1.410(3) . ? N2C C12C 1.327(3) . ? N2C Ga1 2.067(2) 3_756 ? C1C C10C 1.380(4) . ? C1C C2C 1.442(4) . ? C2C C3C 1.380(4) . ? C2C C11C 1.466(3) . ? C3C C4C 1.404(4) . ? C4C C5C 1.426(4) . ? C4C C9C 1.428(4) . ? C5C C6C 1.365(4) . ? C6C C7C 1.416(4) . ? C7C C8C 1.364(4) . ? C8C C9C 1.418(4) . ? C9C C10C 1.402(4) . ? C12C C13C 1.446(4) . ? C13C C14C 1.336(4) . ? C14C C15C 1.469(4) . ? C15C C20C 1.381(5) . ? C15C C16C 1.395(5) . ? C16C C17C 1.384(5) . ? C17C C18C 1.375(6) . ? C18C C19C 1.368(6) . ? C19C C20C 1.388(4) . ? C21C C22C 1.497(6) . ? O1S C11S 1.388(5) . ? C11S C12S 1.434(6) . ? O2S C21S 1.450(4) . ? C21S C22S 1.497(5) . ? O3S C31S 1.410(9) . ? C31S C32S 1.370(10) . ? O4S C41S 1.485(6) . ? C41S C42S 1.432(7) . ? O51S C511 1.565(7) . ? C511 C521 1.282(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 O1A Ga1 O2C 100.55(9) . 3_756 ? O1A Ga1 N1A 90.57(9) . . ? O2C Ga1 N1A 168.76(9) 3_756 . ? O1A Ga1 O3A 169.43(8) . . ? O2C Ga1 O3A 89.77(8) 3_756 . ? N1A Ga1 O3A 79.05(8) . . ? O1A Ga1 O4A 89.56(10) . . ? O2C Ga1 O4A 85.35(9) 3_756 . ? N1A Ga1 O4A 93.23(10) . . ? O3A Ga1 O4A 89.02(9) . . ? O1A Ga1 N2C 92.68(9) . 3_756 ? O2C Ga1 N2C 79.49(8) 3_756 3_756 ? N1A Ga1 N2C 101.75(9) . 3_756 ? O3A Ga1 N2C 91.43(9) . 3_756 ? O4A Ga1 N2C 164.83(9) . 3_756 ? C1A O1A Ga1 128.66(19) . . ? C11A O2A Ga2 113.04(17) . . ? C12A O3A Ga1 113.27(16) . . ? C211 O4A C21A 60.2(7) . . ? C211 O4A Ga1 133.5(4) . . ? C21A O4A Ga1 124.2(3) . . ? C11A N1A N2A 113.0(2) . . ? C11A N1A Ga1 132.0(2) . . ? N2A N1A Ga1 114.36(15) . . ? C12A N2A N1A 111.1(2) . . ? C12A N2A Ga2 139.5(2) . . ? N1A N2A Ga2 109.23(15) . . ? O1A C1A C10A 117.9(3) . . ? O1A C1A C2A 124.0(3) . . ? C10A C1A C2A 118.1(3) . . ? C3A C2A C1A 118.6(3) . . ? C3A C2A C11A 116.6(3) . . ? C1A C2A C11A 124.8(2) . . ? C4A C3A C2A 122.8(3) . . ? C3A C4A C5A 122.7(3) . . ? C3A C4A C9A 118.4(3) . . ? C5A C4A C9A 118.9(3) . . ? C6A C5A C4A 120.7(4) . . ? C5A C6A C7A 120.7(3) . . ? C8A C7A C6A 120.6(3) . . ? C7A C8A C9A 120.1(4) . . ? C10A C9A C8A 122.9(3) . . ? C10A C9A C4A 118.2(3) . . ? C8A C9A C4A 118.9(3) . . ? C1A C10A C9A 123.6(3) . . ? O2A C11A N1A 121.4(3) . . ? O2A C11A C2A 119.9(2) . . ? N1A C11A C2A 118.7(3) . . ? O3A C12A N2A 122.2(3) . . ? O3A C12A C13A 120.9(2) . . ? N2A C12A C13A 116.9(3) . . ? C14A C13A C12A 122.5(3) . . ? C13A C14A C15A 125.7(3) . . ? C20A C15A C16A 118.3(3) . . ? C20A C15A C14A 123.3(3) . . ? C16A C15A C14A 118.4(3) . . ? C17A C16A C15A 120.6(3) . . ? C18A C17A C16A 120.4(3) . . ? C17A C18A C19A 120.1(3) . . ? C20A C19A C18A 119.8(3) . . ? C19A C20A C15A 120.8(3) . . ? O4A C21A C22A 108.4(6) . . ? O1B Ga2 O2A 101.96(9) . . ? O1B Ga2 N1B 89.93(9) . . ? O2A Ga2 N1B 167.90(9) . . ? O1B Ga2 O3B 168.66(9) . . ? O2A Ga2 O3B 89.26(8) . . ? N1B Ga2 O3B 78.79(9) . . ? O1B Ga2 N2A 93.17(9) . . ? O2A Ga2 N2A 79.25(9) . . ? N1B Ga2 N2A 102.55(10) . . ? O3B Ga2 N2A 90.52(9) . . ? O1B Ga2 O4B 90.05(9) . . ? O2A Ga2 O4B 88.47(9) . . ? N1B Ga2 O4B 89.31(10) . . ? O3B Ga2 O4B 88.59(9) . . ? N2A Ga2 O4B 167.70(10) . . ? C1B O1B Ga2 127.85(19) . . ? C11B O2B Ga3 114.23(16) . . ? C12B O3B Ga2 112.65(17) . . ? C21B O4B Ga2 127.4(2) . . ? C11B N1B N2B 113.1(2) . . ? C11B N1B Ga2 130.64(19) . . ? N2B N1B Ga2 114.78(17) . . ? C12B N2B N1B 110.8(2) . . ? C12B N2B Ga3 137.9(2) . . ? N1B N2B Ga3 110.33(16) . . ? O1B C1B C10B 118.8(3) . . ? O1B C1B C2B 124.1(2) . . ? C10B C1B C2B 117.1(3) . . ? C3B C2B C1B 119.6(3) . . ? C3B C2B C11B 116.4(3) . . ? C1B C2B C11B 124.0(3) . . ? C2B C3B C4B 123.3(3) . . ? C3B C4B C9B 117.3(3) . . ? C3B C4B C5B 123.8(3) . . ? C9B C4B C5B 119.0(3) . . ? C6B C5B C4B 122.0(4) . . ? C5B C6B C7B 119.5(4) . . ? C8B C7B C6B 121.3(3) . . ? C7B C8B C9B 120.5(4) . . ? C10B C9B C4B 119.9(3) . . ? C10B C9B C8B 122.5(4) . . ? C4B C9B C8B 117.6(3) . . ? C1B C10B C9B 122.9(3) . . ? O2B C11B N1B 121.8(2) . . ? O2B C11B C2B 118.6(2) . . ? N1B C11B C2B 119.6(3) . . ? O3B C12B N2B 122.7(3) . . ? O3B C12B C13B 121.5(3) . . ? N2B C12B C13B 115.5(3) . . ? C14B C13B C12B 121.5(3) . . ? C13B C14B C15B 126.3(3) . . ? C16B C15B C20B 118.0(3) . . ? C16B C15B C14B 119.4(3) . . ? C20B C15B C14B 122.5(3) . . ? C15B C16B C17B 121.3(4) . . ? C18B C17B C16B 120.0(3) . . ? C17B C18B C19B 120.0(3) . . ? C18B C19B C20B 119.5(4) . . ? C15B C20B C19B 121.1(3) . . ? C22B C21B O4B 112.0(4) . . ? O1C Ga3 O2B 95.24(8) . . ? O1C Ga3 O3C 170.04(8) . . ? O2B Ga3 O3C 94.02(8) . . ? O1C Ga3 N1C 90.98(9) . . ? O2B Ga3 N1C 171.91(9) . . ? O3C Ga3 N1C 79.48(8) . . ? O1C Ga3 N2B 92.56(10) . . ? O2B Ga3 N2B 79.87(8) . . ? O3C Ga3 N2B 92.68(9) . . ? N1C Ga3 N2B 105.08(9) . . ? O1C Ga3 O4C 90.95(10) . . ? O2B Ga3 O4C 85.66(9) . . ? O3C Ga3 O4C 86.08(9) . . ? N1C Ga3 O4C 89.06(9) . . ? N2B Ga3 O4C 165.36(9) . . ? C1C O1C Ga3 128.89(17) . . ? C11C O2C Ga1 114.27(17) . 3_756 ? C12C O3C Ga3 113.88(16) . . ? C21C O4C Ga3 126.9(2) . . ? C11C N1C N2C 113.9(2) . . ? C11C N1C Ga3 128.81(18) . . ? N2C N1C Ga3 113.69(16) . . ? C12C N2C N1C 111.1(2) . . ? C12C N2C Ga1 138.93(18) . 3_756 ? N1C N2C Ga1 109.08(15) . 3_756 ? O1C C1C C10C 117.8(2) . . ? O1C C1C C2C 123.9(2) . . ? C10C C1C C2C 118.3(2) . . ? C3C C2C C1C 119.0(2) . . ? C3C C2C C11C 116.6(2) . . ? C1C C2C C11C 124.4(2) . . ? C2C C3C C4C 122.9(3) . . ? C3C C4C C5C 122.6(3) . . ? C3C C4C C9C 118.0(2) . . ? C5C C4C C9C 119.4(2) . . ? C6C C5C C4C 120.5(3) . . ? C5C C6C C7C 119.6(3) . . ? C8C C7C C6C 121.6(3) . . ? C7C C8C C9C 120.3(3) . . ? C10C C9C C8C 122.6(3) . . ? C10C C9C C4C 118.8(2) . . ? C8C C9C C4C 118.5(3) . . ? C1C C10C C9C 122.9(3) . . ? O2C C11C N1C 121.0(2) . . ? O2C C11C C2C 119.3(2) . . ? N1C C11C C2C 119.7(2) . . ? O3C C12C N2C 121.8(2) . . ? O3C C12C C13C 120.1(2) . . ? N2C C12C C13C 117.9(2) . . ? C14C C13C C12C 120.2(3) . . ? C13C C14C C15C 127.7(3) . . ? C20C C15C C16C 118.1(3) . . ? C20C C15C C14C 124.2(3) . . ? C16C C15C C14C 117.6(3) . . ? C17C C16C C15C 121.0(4) . . ? C18C C17C C16C 119.4(4) . . ? C19C C18C C17C 120.8(3) . . ? C18C C19C C20C 119.7(4) . . ? C15C C20C C19C 121.0(3) . . ? O4C C21C C22C 112.7(4) . . ? O1S C11S C12S 114.5(4) . . ? O2S C21S C22S 109.1(3) . . ? C32S C31S O3S 117.5(9) . . ? C42S C41S O4S 109.8(4) . . ? C521 C511 O51S 116.1(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 O4A H4OA O1S 0.89(4) 1.70(4) 2.561(4) 161(4) . O4B H4OB O51S 0.71(4) 1.92(4) 2.632(4) 177(5) . O4B H4OB O52S 0.71(4) 1.92(4) 2.632(4) 177(5) . O4C H4OC O2S 0.89(4) 1.84(4) 2.698(3) 161(4) . O1S H1S O4S 0.84 1.82 2.634(4) 164.2 . O2S H2S O1A 0.84 2.09 2.880(3) 155.5 3_756 O4S H4S O1B 0.84 1.88 2.703(4) 166.2 . O51S H51S O1C 0.84 1.98 2.747(3) 151.0 . O52S H52S O4B 0.84 2.22 2.632(4) 110.4 . _diffrn_measured_fraction_theta_max 0.988 _diffrn_reflns_theta_full 30.44 _diffrn_measured_fraction_theta_full 0.988 _refine_diff_density_max 1.114 _refine_diff_density_min -0.935 _refine_diff_density_rms 0.108 #===END data_structure2 _database_code_depnum_ccdc_archive 'CCDC 644812' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C368 H344 Mn16 N32 O72 S16' _chemical_formula_weight 7758.75 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' Mn Mn 0.3368 0.7283 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting Tetragonal _symmetry_space_group_name_H-M P4/n loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x+1/2, -y+1/2, z' '-y+1/2, x, z' 'y, -x+1/2, z' '-x, -y, -z' 'x-1/2, y-1/2, -z' 'y-1/2, -x, -z' '-y, x-1/2, -z' _cell_length_a 39.134(6) _cell_length_b 39.134(6) _cell_length_c 14.553(3) _cell_angle_alpha 90.00 _cell_angle_beta 90.00 _cell_angle_gamma 90.00 _cell_volume 22288(6) _cell_formula_units_Z 2 _cell_measurement_temperature 103(2) _cell_measurement_reflns_used 35175 _cell_measurement_theta_min 1.56 _cell_measurement_theta_max 30.42 _exptl_crystal_description Needle _exptl_crystal_colour 'Dark brown' _exptl_crystal_size_max 0.20 _exptl_crystal_size_mid 0.10 _exptl_crystal_size_min 0.10 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.110 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 7680 _exptl_absorpt_coefficient_mu 0.555 _exptl_absorpt_correction_type Empirical _exptl_absorpt_correction_T_min 0.8934 _exptl_absorpt_correction_T_max 0.9446 _exptl_absorpt_process_details HKL2000-Scalepack _exptl_special_details ; ? ; _diffrn_ambient_temperature 103(2) _diffrn_radiation_wavelength 0.70000 _diffrn_radiation_type synchrotron _diffrn_radiation_source 'Fixed gap multiple wiggler beamline' _diffrn_radiation_monochromator 'Pt coated Si double crystal' _diffrn_measurement_device_type 'CCD area detector' _diffrn_measurement_method 'phi scans' _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 125699 _diffrn_reflns_av_R_equivalents 0.0687 _diffrn_reflns_av_sigmaI/netI 0.1000 _diffrn_reflns_limit_h_min -56 _diffrn_reflns_limit_h_max 56 _diffrn_reflns_limit_k_min -56 _diffrn_reflns_limit_k_max 56 _diffrn_reflns_limit_l_min -21 _diffrn_reflns_limit_l_max 0 _diffrn_reflns_theta_min 1.56 _diffrn_reflns_theta_max 30.42 _reflns_number_total 35175 _reflns_number_gt 10456 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'PAL ADSC Quantum-210' _computing_cell_refinement HKL2000 _computing_data_reduction HKL2000 _computing_structure_solution 'Bruker SHELXTL' _computing_structure_refinement 'Bruker SHELXTL' _computing_molecular_graphics ORTEP3 _computing_publication_material WinGX _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^)+(0.1375P)^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 ridden _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 35175 _refine_ls_number_parameters 1168 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.1877 _refine_ls_R_factor_gt 0.0742 _refine_ls_wR_factor_ref 0.2451 _refine_ls_wR_factor_gt 0.2042 _refine_ls_goodness_of_fit_ref 0.800 _refine_ls_restrained_S_all 0.800 _refine_ls_shift/su_max 0.001 _refine_ls_shift/su_mean 0.000 loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_occupancy _atom_site_symmetry_multiplicity _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group Mn1 Mn 0.219284(14) 0.499329(14) 0.04292(5) 0.07644(19) Uani 1 1 d . . . O1A O 0.21621(7) 0.54274(7) -0.0120(2) 0.0871(8) Uani 1 1 d . . . O2A O 0.14245(7) 0.54300(6) 0.2038(2) 0.0789(7) Uani 1 1 d . . . O3A O 0.21536(6) 0.45667(6) 0.10940(18) 0.0728(7) Uani 1 1 d . . . O4A O 0.18263(6) 0.47658(7) -0.0556(2) 0.0869(8) Uani 1 1 d . . . N1A N 0.18346(8) 0.51107(8) 0.1287(2) 0.0777(9) Uani 1 1 d . . . N2A N 0.17051(8) 0.48323(7) 0.1784(2) 0.0783(9) Uani 1 1 d . . . C1A C 0.20546(11) 0.57119(11) 0.0283(3) 0.0870(12) Uani 1 1 d . . . C2A C 0.18118(11) 0.57201(10) 0.1054(3) 0.0860(12) Uani 1 1 d . . . C3A C 0.17096(11) 0.60263(10) 0.1416(4) 0.0915(13) Uani 1 1 d . . . H3A H 0.1548 0.6026 0.1904 0.110 Uiso 1 1 calc R . . C4A C 0.17334(14) 0.66543(12) 0.1507(5) 0.127(2) Uani 1 1 d . . . H4A H 0.1587 0.6659 0.2028 0.152 Uiso 1 1 calc R . . C5A C 0.1858(2) 0.69542(14) 0.1118(6) 0.160(3) Uani 1 1 d . . . H5A H 0.1782 0.7167 0.1355 0.192 Uiso 1 1 calc R . . C6A C 0.20899(18) 0.69529(16) 0.0393(7) 0.160(3) Uani 1 1 d . . . H6A H 0.2181 0.7162 0.0171 0.192 Uiso 1 1 calc R . . C7A C 0.21849(15) 0.66542(13) 0.0006(5) 0.134(2) Uani 1 1 d . . . H7A H 0.2337 0.6658 -0.0503 0.160 Uiso 1 1 calc R . . C8A C 0.21700(11) 0.60248(12) -0.0039(4) 0.1000(14) Uani 1 1 d . . . H8A H 0.2328 0.6028 -0.0535 0.120 Uiso 1 1 calc R . . C9A C 0.20634(13) 0.63331(12) 0.0338(5) 0.1091(17) Uani 1 1 d . . . C10A C 0.18331(13) 0.63398(11) 0.1096(4) 0.1042(16) Uani 1 1 d . . . C11A C 0.16723(10) 0.54066(9) 0.1483(3) 0.0769(11) Uani 1 1 d . . . C12A C 0.18961(9) 0.45591(10) 0.1636(3) 0.0720(10) Uani 1 1 d . . . C13A C 0.18189(9) 0.42523(9) 0.2152(3) 0.0724(10) Uani 1 1 d . . . H13A H 0.1620 0.4252 0.2525 0.087 Uiso 1 1 calc R . . C14A C 0.20074(9) 0.39716(9) 0.2138(3) 0.0742(10) Uani 1 1 d . . . H14A H 0.2197 0.3970 0.1731 0.089 Uiso 1 1 calc R . . C15A C 0.19526(9) 0.36624(9) 0.2691(3) 0.0740(10) Uani 1 1 d . . . C16A C 0.21951(9) 0.33976(9) 0.2635(3) 0.0811(11) Uani 1 1 d . . . H16A H 0.2385 0.3416 0.2233 0.097 Uiso 1 1 calc R . . C17A C 0.21522(10) 0.31103(9) 0.3176(3) 0.0893(13) Uani 1 1 d . . . H17A H 0.2321 0.2935 0.3167 0.107 Uiso 1 1 calc R . . C18A C 0.18695(10) 0.30746(10) 0.3726(3) 0.0876(12) Uani 1 1 d . . . H18A H 0.1838 0.2871 0.4072 0.105 Uiso 1 1 calc R . . C19A C 0.16344(10) 0.33301(10) 0.3777(3) 0.0811(11) Uani 1 1 d . . . H19A H 0.1444 0.3309 0.4176 0.097 Uiso 1 1 calc R . . C20A C 0.16735(9) 0.36139(9) 0.3256(3) 0.0726(10) Uani 1 1 d . . . H20A H 0.1503 0.3786 0.3281 0.087 Uiso 1 1 calc R . . C21A C 0.15498(12) 0.49366(12) -0.1047(4) 0.1002(14) Uani 1 1 d . . . C22A C 0.12613(15) 0.5000(2) -0.0480(5) 0.168(3) Uani 1 1 d . . . Mn2 Mn 0.126123(15) 0.501708(14) 0.26616(5) 0.07587(18) Uani 1 1 d . . . O1B O 0.15444(7) 0.50751(7) 0.3665(2) 0.0841(8) Uani 1 1 d . . . O2B O 0.10128(6) 0.41414(6) 0.41315(17) 0.0716(6) Uani 1 1 d . A . O3B O 0.09473(6) 0.48962(6) 0.17023(18) 0.0766(7) Uani 1 1 d . A . N1B N 0.10868(7) 0.45903(7) 0.3154(2) 0.0704(8) Uani 1 1 d . . . N2B N 0.08308(7) 0.44323(8) 0.2612(2) 0.0720(8) Uani 1 1 d . . . C1B C 0.16083(10) 0.48674(10) 0.4368(3) 0.0763(10) Uani 1 1 d . . . C2B C 0.14417(8) 0.45445(9) 0.4520(3) 0.0692(9) Uani 1 1 d . . . C3B C 0.15266(9) 0.43549(10) 0.5265(3) 0.0709(9) Uani 1 1 d . . . H3B H 0.1417 0.4140 0.5348 0.085 Uiso 1 1 calc R A . C4B C 0.18389(10) 0.42743(11) 0.6726(3) 0.0841(11) Uani 1 1 d . . . H4B H 0.1726 0.4063 0.6837 0.101 Uiso 1 1 calc R A . C5B C 0.20709(11) 0.43966(15) 0.7351(3) 0.0985(14) Uani 1 1 d . . . H5B H 0.2124 0.4265 0.7882 0.118 Uiso 1 1 calc R . . C6B C 0.22306(12) 0.47131(13) 0.7215(4) 0.0982(14) Uani 1 1 d . . . H6B H 0.2384 0.4799 0.7667 0.118 Uiso 1 1 calc R A . C7B C 0.21698(11) 0.48957(13) 0.6457(3) 0.0977(14) Uani 1 1 d . . . H7B H 0.2286 0.5106 0.6368 0.117 Uiso 1 1 calc R . . C8B C 0.18543(10) 0.49712(10) 0.4998(3) 0.0811(11) Uani 1 1 d . . . H8B H 0.1973 0.5179 0.4891 0.097 Uiso 1 1 calc R . . C9B C 0.19340(10) 0.47812(11) 0.5783(3) 0.0837(11) Uani 1 1 d . . . C10B C 0.17679(9) 0.44592(11) 0.5923(3) 0.0758(10) Uani 1 1 d . . . C11B C 0.11612(9) 0.44222(10) 0.3901(3) 0.0712(10) Uani 1 1 d . . . C12B C 0.07748(9) 0.46146(10) 0.1881(3) 0.0740(10) Uani 1 1 d . A . C13B C 0.05162(9) 0.45055(10) 0.1218(3) 0.0735(10) Uani 1 1 d . . . H13B H 0.0396 0.4299 0.1332 0.088 Uiso 1 1 calc R A . C14B C 0.04415(9) 0.46786(9) 0.0475(3) 0.0730(10) Uani 1 1 d . . . H14B H 0.0579 0.4874 0.0355 0.088 Uiso 1 1 calc R . . C15B C 0.01677(10) 0.46065(9) -0.0204(3) 0.0741(10) Uani 1 1 d . . . C16B C 0.01881(11) 0.47370(10) -0.1072(3) 0.0808(11) Uani 1 1 d . . . H16B H 0.0378 0.4873 -0.1247 0.097 Uiso 1 1 calc R . . C17B C -0.00755(13) 0.46680(11) -0.1705(3) 0.0932(13) Uani 1 1 d . . . H17B H -0.0063 0.4755 -0.2314 0.112 Uiso 1 1 calc R A . C18B C -0.03475(12) 0.44771(12) -0.1442(4) 0.0973(14) Uani 1 1 d . . . H18B H -0.0526 0.4433 -0.1869 0.117 Uiso 1 1 calc R . . C19B C -0.03703(11) 0.43438(11) -0.0556(3) 0.0882(12) Uani 1 1 d . . . H19B H -0.0563 0.4212 -0.0376 0.106 Uiso 1 1 calc R A . C20B C -0.01132(10) 0.44061(10) 0.0041(3) 0.0811(11) Uani 1 1 d . . . H20B H -0.0124 0.4311 0.0641 0.097 Uiso 1 1 calc R . . S1B S 0.08928(6) 0.56403(6) 0.38061(18) 0.0923(6) Uani 0.50 1 d P A 1 O41B O 0.08703(8) 0.53503(8) 0.3283(2) 0.0985(9) Uani 0.50 1 d P A 1 C211 C 0.10299(13) 0.55409(12) 0.4948(3) 0.1020(14) Uani 0.50 1 d P A 1 C221 C 0.04286(14) 0.57064(17) 0.4161(4) 0.135(2) Uani 0.50 1 d P A 1 S2B S 0.07339(6) 0.53454(5) 0.41631(18) 0.0884(6) Uani 0.50 1 d P A 2 O42B O 0.08703(8) 0.53503(8) 0.3283(2) 0.0985(9) Uani 0.50 1 d P A 2 C212 C 0.10299(13) 0.55409(12) 0.4948(3) 0.1020(14) Uani 0.50 1 d P A 2 C222 C 0.04286(14) 0.57064(17) 0.4161(4) 0.135(2) Uani 0.50 1 d P A 2 Mn3 Mn 0.060998(13) 0.399453(14) 0.34142(4) 0.06994(17) Uani 1 1 d . A . O1C O 0.03113(6) 0.42983(6) 0.39745(18) 0.0773(7) Uani 1 1 d . . . O2C O -0.02646(6) 0.38241(6) 0.18552(19) 0.0756(7) Uani 1 1 d . A . O3C O 0.08520(6) 0.36466(6) 0.27297(18) 0.0739(7) Uani 1 1 d . . . O4C O 0.05013(6) 0.36018(6) 0.44736(19) 0.0786(7) Uani 1 1 d . . . N1C N 0.02428(7) 0.38315(7) 0.2620(2) 0.0704(8) Uani 1 1 d . . . N2C N 0.03325(7) 0.35511(7) 0.2064(2) 0.0687(8) Uani 1 1 d . A . C1C C 0.00379(9) 0.44398(9) 0.3590(3) 0.0700(10) Uani 1 1 d . A . C2C C -0.01675(8) 0.42743(9) 0.2915(3) 0.0685(9) Uani 1 1 d . . . C3C C -0.04800(9) 0.44180(9) 0.2654(3) 0.0732(10) Uani 1 1 d . A . H3C H -0.0619 0.4302 0.2220 0.088 Uiso 1 1 calc R . . C4C C -0.09119(11) 0.48698(12) 0.2788(3) 0.0971(14) Uani 1 1 d . A . H4C H -0.1058 0.4753 0.2371 0.117 Uiso 1 1 calc R . . C5C C -0.10130(13) 0.51714(13) 0.3158(3) 0.1055(16) Uani 1 1 d . . . H5C H -0.1231 0.5262 0.3006 0.127 Uiso 1 1 calc R . . C6C C -0.08000(13) 0.53488(12) 0.3757(3) 0.0987(14) Uani 1 1 d . . . H6C H -0.0876 0.5557 0.4023 0.118 Uiso 1 1 calc R . . C7C C -0.04864(11) 0.52287(11) 0.3967(3) 0.0929(13) Uani 1 1 d . . . H7C H -0.0339 0.5362 0.4341 0.111 Uiso 1 1 calc R . . C8C C -0.00595(10) 0.47608(10) 0.3886(3) 0.0829(11) Uani 1 1 d . . . H8C H 0.0092 0.4886 0.4269 0.099 Uiso 1 1 calc R A . C9C C -0.03731(10) 0.49084(9) 0.3642(3) 0.0758(10) Uani 1 1 d . A . C10C C -0.05920(10) 0.47282(10) 0.3017(3) 0.0838(11) Uani 1 1 d . . . C11C C -0.00628(9) 0.39574(9) 0.2449(3) 0.0681(9) Uani 1 1 d . A . C12C C 0.06566(9) 0.34812(9) 0.2156(3) 0.0704(10) Uani 1 1 d . A . C13C C 0.07982(9) 0.32179(9) 0.1581(3) 0.0719(10) Uani 1 1 d . . . H13C H 0.0648 0.3086 0.1213 0.086 Uiso 1 1 calc R A . C14C C 0.11342(9) 0.31517(9) 0.1545(3) 0.0700(9) Uani 1 1 d . A . H14C H 0.1277 0.3271 0.1964 0.084 Uiso 1 1 calc R . . C15C C 0.13007(9) 0.29097(8) 0.0910(3) 0.0676(9) Uani 1 1 d . . . C16C C 0.16563(9) 0.29100(9) 0.0850(3) 0.0768(11) Uani 1 1 d . A . H16C H 0.1785 0.3054 0.1246 0.092 Uiso 1 1 calc R . . C17C C 0.18277(10) 0.27011(10) 0.0214(3) 0.0854(12) Uani 1 1 d . . . C18C C 0.16307(10) 0.24785(10) -0.0324(3) 0.0891(13) Uani 1 1 d . A . H18C H 0.1741 0.2333 -0.0753 0.107 Uiso 1 1 calc R . . C19C C 0.12842(10) 0.24673(10) -0.0246(3) 0.0873(12) Uani 1 1 d . . . H19C H 0.1157 0.2311 -0.0609 0.105 Uiso 1 1 calc R A . C20C C 0.11182(9) 0.26803(9) 0.0354(3) 0.0747(10) Uani 1 1 d . A . H20C H 0.0876 0.2673 0.0394 0.090 Uiso 1 1 calc R . . C21C C 0.01701(18) 0.35604(17) 0.4877(6) 0.154(4) Uani 0.716(19) 1 d P A 1 C22C C 0.0083(4) 0.3316(5) 0.5466(16) 0.255(12) Uani 0.716(19) 1 d P A 1 C23C C 0.01701(18) 0.35604(17) 0.4877(6) 0.154(4) Uani 0.28 1 d P A 2 C24C C -0.0044(5) 0.3322(7) 0.4575(19) 0.125(10) Uani 0.284(19) 1 d P A 2 Mn4 Mn -0.012160(14) 0.340479(14) 0.11828(5) 0.07427(18) Uani 1 1 d . . . S1D S -0.09501(4) 0.34383(5) 0.10547(14) 0.1417(6) Uani 1 1 d . . . O1D O 0.00543(7) 0.36166(6) 0.0166(2) 0.0889(8) Uani 1 1 d . A . O2D O 0.01756(6) 0.25583(7) -0.03572(19) 0.0822(7) Uani 1 1 d . A . O3D O -0.02978(6) 0.31170(6) 0.21372(19) 0.0798(7) Uani 1 1 d . A . O4D O -0.06320(7) 0.34099(8) 0.0529(2) 0.1055(10) Uani 1 1 d . A . N1D N -0.00044(7) 0.29595(7) 0.0665(2) 0.0689(8) Uani 1 1 d . A . N2D N -0.01291(8) 0.26808(8) 0.1180(2) 0.0768(9) Uani 1 1 d . . . C1D C 0.02361(10) 0.35008(11) -0.0552(3) 0.0800(11) Uani 1 1 d . . . C2D C 0.03702(10) 0.37230(10) -0.1178(3) 0.0812(11) Uani 1 1 d . A . H2D H 0.0335 0.3961 -0.1088 0.097 Uiso 1 1 calc R . . C3D C 0.06892(13) 0.38479(13) -0.2602(4) 0.1060(15) Uani 1 1 d . A . H3D H 0.0648 0.4086 -0.2544 0.127 Uiso 1 1 calc R . . C4D C 0.08814(14) 0.37209(14) -0.3338(4) 0.1164(17) Uani 1 1 d . . . H4D H 0.0975 0.3878 -0.3767 0.140 Uiso 1 1 calc R . . C5D C 0.09410(13) 0.33761(13) -0.3466(4) 0.1112(16) Uani 1 1 d . . . H5D H 0.1067 0.3298 -0.3983 0.133 Uiso 1 1 calc R . . C6D C 0.08185(11) 0.31520(13) -0.2848(4) 0.0971(13) Uani 1 1 d . . . H6D H 0.0861 0.2915 -0.2932 0.116 Uiso 1 1 calc R . . C7D C 0.04864(10) 0.30349(11) -0.1433(3) 0.0813(11) Uani 1 1 d . . . H7D H 0.0529 0.2798 -0.1512 0.098 Uiso 1 1 calc R A . C8D C 0.02905(10) 0.31366(9) -0.0695(3) 0.0746(10) Uani 1 1 d . A . C9D C 0.06255(10) 0.32624(10) -0.2068(3) 0.0810(11) Uani 1 1 d . A . C10D C 0.05578(11) 0.36177(11) -0.1949(3) 0.0879(12) Uani 1 1 d . . . C11D C 0.01479(9) 0.28747(10) -0.0107(3) 0.0707(10) Uani 1 1 d . . . C12D C -0.02757(9) 0.27839(10) 0.1925(3) 0.0765(10) Uani 1 1 d . A . C13D C -0.04228(10) 0.25406(11) 0.2569(3) 0.0785(11) Uani 1 1 d . . . H13D H -0.0414 0.2305 0.2411 0.094 Uiso 1 1 calc R A . C14D C -0.05657(12) 0.26234(12) 0.3348(3) 0.0926(12) Uani 1 1 d . A . H14D H -0.0556 0.2858 0.3511 0.111 Uiso 1 1 calc R . . C15D C -0.07337(13) 0.24054(13) 0.3978(4) 0.1030(15) Uani 1 1 d . . . C16D C -0.08216(11) 0.20633(13) 0.3787(4) 0.0979(14) Uani 1 1 d . A . H16D H -0.0760 0.1973 0.3204 0.117 Uiso 1 1 calc R . . C17D C -0.09880(15) 0.18557(16) 0.4384(5) 0.1228(18) Uani 1 1 d . . . H17D H -0.1043 0.1627 0.4222 0.147 Uiso 1 1 calc R A . C18D C -0.1076(2) 0.1988(2) 0.5243(6) 0.174(3) Uani 1 1 d . A . H18D H -0.1202 0.1849 0.5661 0.208 Uiso 1 1 calc R . . C19D C -0.0985(3) 0.2317(2) 0.5501(6) 0.225(5) Uani 1 1 d . . . H19D H -0.1043 0.2404 0.6090 0.270 Uiso 1 1 calc R A . C20D C -0.0806(2) 0.25141(17) 0.4875(5) 0.168(3) Uani 1 1 d . A . H20D H -0.0729 0.2734 0.5062 0.202 Uiso 1 1 calc R . . C21D C -0.11645(17) 0.3796(2) 0.0586(6) 0.197(4) Uani 1 1 d . A . H21C H -0.1134 0.3994 0.0992 0.295 Uiso 1 1 calc R . . H21D H -0.1409 0.3745 0.0527 0.295 Uiso 1 1 calc R . . H21E H -0.1070 0.3849 -0.0022 0.295 Uiso 1 1 calc R . . C22D C -0.1219(2) 0.3108(2) 0.0577(8) 0.240(5) Uani 1 1 d . A . H22D H -0.1188 0.3099 -0.0091 0.360 Uiso 1 1 calc R . . H22E H -0.1459 0.3158 0.0718 0.360 Uiso 1 1 calc R . . H22F H -0.1156 0.2887 0.0844 0.360 Uiso 1 1 calc R . . S1S S 0.08545(3) 0.27249(3) 0.37897(9) 0.0889(3) Uani 1 1 d . . . O1S O 0.08493(7) 0.30156(6) 0.4474(2) 0.0889(8) Uani 1 1 d . . . C1S C 0.08947(14) 0.23549(10) 0.4495(3) 0.1047(15) Uani 1 1 d . . . H1S1 H 0.1133 0.2329 0.4690 0.157 Uiso 1 1 calc R . . H1S2 H 0.0825 0.2152 0.4146 0.157 Uiso 1 1 calc R . . H1S3 H 0.0748 0.2379 0.5038 0.157 Uiso 1 1 calc R . . C2S C 0.04239(12) 0.26650(13) 0.3415(4) 0.1104(16) Uani 1 1 d . . . H2S1 H 0.0271 0.2663 0.3949 0.166 Uiso 1 1 calc R . . H2S2 H 0.0405 0.2447 0.3088 0.166 Uiso 1 1 calc R . . H2S3 H 0.0359 0.2852 0.3002 0.166 Uiso 1 1 calc R . . S21S S 0.84435(4) 0.61770(4) 0.01411(12) 0.0961(6) Uani 0.815(3) 1 d P B 1 S22S S 0.86796(17) 0.60077(15) 0.0689(5) 0.095(3) Uani 0.185(3) 1 d P B 2 O2S O 0.82857(7) 0.59041(7) 0.0727(2) 0.0998(9) Uani 1 1 d . . . C3S C 0.86072(15) 0.64817(13) 0.0967(4) 0.1172(17) Uani 1 1 d . . . C4S C 0.88274(14) 0.59897(16) -0.0310(4) 0.1300(19) Uani 1 1 d . . . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 Mn1 0.0635(3) 0.0648(3) 0.1010(5) 0.0087(3) -0.0160(3) -0.0006(3) O1A 0.0787(17) 0.0684(16) 0.114(2) 0.0142(15) -0.0174(16) -0.0017(14) O2A 0.0681(16) 0.0645(15) 0.104(2) 0.0020(14) -0.0064(15) 0.0035(13) O3A 0.0624(14) 0.0592(13) 0.0969(19) 0.0054(13) -0.0109(14) 0.0028(11) O4A 0.0683(15) 0.0854(17) 0.107(2) 0.0067(15) -0.0236(14) 0.0030(14) N1A 0.0636(18) 0.0610(18) 0.108(3) 0.0079(17) -0.0188(17) 0.0010(15) N2A 0.0670(18) 0.0542(17) 0.114(3) 0.0110(17) -0.0133(17) 0.0036(15) C1A 0.074(3) 0.072(3) 0.116(4) 0.016(3) -0.029(3) -0.005(2) C2A 0.077(3) 0.062(2) 0.119(4) 0.011(2) -0.033(3) -0.003(2) C3A 0.074(2) 0.062(2) 0.138(4) 0.000(2) -0.015(2) 0.006(2) C4A 0.115(4) 0.067(3) 0.198(6) -0.001(3) -0.023(4) 0.014(3) C5A 0.165(6) 0.062(3) 0.252(9) 0.019(4) 0.010(6) -0.008(4) C6A 0.124(5) 0.080(4) 0.275(10) 0.037(5) 0.004(6) -0.019(4) C7A 0.121(4) 0.076(3) 0.205(6) 0.028(4) 0.006(4) -0.006(3) C8A 0.077(3) 0.090(3) 0.133(4) 0.028(3) -0.021(3) -0.008(2) C9A 0.088(3) 0.066(3) 0.173(5) 0.017(3) -0.033(3) -0.003(2) C10A 0.089(3) 0.060(2) 0.164(5) 0.019(3) -0.019(3) 0.003(2) C11A 0.066(2) 0.061(2) 0.103(3) 0.007(2) -0.035(2) -0.0042(19) C12A 0.058(2) 0.069(2) 0.089(3) 0.000(2) -0.014(2) 0.0040(18) C13A 0.060(2) 0.062(2) 0.095(3) 0.003(2) -0.0072(19) -0.0032(17) C14A 0.0543(19) 0.061(2) 0.107(3) 0.001(2) -0.0110(19) 0.0017(17) C15A 0.060(2) 0.060(2) 0.102(3) 0.004(2) -0.007(2) 0.0023(17) C16A 0.059(2) 0.054(2) 0.130(4) 0.004(2) 0.005(2) 0.0030(17) C17A 0.062(2) 0.055(2) 0.151(4) 0.014(2) 0.001(2) 0.0012(18) C18A 0.060(2) 0.060(2) 0.142(4) 0.016(2) -0.007(2) -0.0022(18) C19A 0.060(2) 0.066(2) 0.117(3) 0.005(2) 0.005(2) -0.0033(19) C20A 0.0539(19) 0.065(2) 0.099(3) 0.003(2) -0.0054(19) 0.0048(17) C21A 0.076(3) 0.105(3) 0.119(4) 0.006(3) -0.028(3) 0.015(2) C22A 0.087(4) 0.288(9) 0.131(5) 0.059(5) -0.004(3) 0.064(5) Mn2 0.0692(3) 0.0637(3) 0.0948(4) -0.0013(3) -0.0185(3) 0.0033(3) O1B 0.0794(17) 0.0700(15) 0.103(2) 0.0034(15) -0.0321(15) -0.0063(13) O2B 0.0567(13) 0.0679(15) 0.0901(18) -0.0045(13) -0.0073(12) 0.0032(12) O3B 0.0678(15) 0.0698(15) 0.0922(19) -0.0010(13) -0.0178(13) 0.0050(13) N1B 0.0640(17) 0.0647(17) 0.082(2) -0.0040(16) -0.0169(16) 0.0042(14) N2B 0.0633(18) 0.0667(18) 0.086(2) -0.0045(17) -0.0161(16) 0.0032(15) C1B 0.065(2) 0.075(2) 0.089(3) -0.004(2) -0.008(2) -0.0005(19) C2B 0.0532(18) 0.070(2) 0.084(3) -0.006(2) -0.0104(18) 0.0058(17) C3B 0.058(2) 0.070(2) 0.085(3) -0.001(2) -0.0034(19) 0.0040(17) C4B 0.068(2) 0.092(3) 0.093(3) 0.000(2) -0.006(2) 0.008(2) C5B 0.077(3) 0.130(4) 0.088(3) 0.000(3) -0.014(2) 0.019(3) C6B 0.081(3) 0.105(3) 0.108(4) -0.003(3) -0.034(3) 0.008(3) C7B 0.081(3) 0.098(3) 0.114(4) -0.008(3) -0.033(3) 0.012(2) C8B 0.072(2) 0.071(2) 0.100(3) 0.002(2) -0.025(2) 0.0019(19) C9B 0.067(2) 0.083(3) 0.101(3) -0.013(2) -0.014(2) 0.006(2) C10B 0.057(2) 0.086(3) 0.084(3) -0.004(2) -0.0036(19) 0.021(2) C11B 0.061(2) 0.069(2) 0.083(3) -0.008(2) -0.0023(19) 0.0056(18) C12B 0.061(2) 0.061(2) 0.100(3) -0.005(2) -0.006(2) 0.0093(18) C13B 0.062(2) 0.063(2) 0.095(3) -0.008(2) -0.012(2) 0.0032(17) C14B 0.068(2) 0.062(2) 0.089(3) -0.005(2) -0.008(2) 0.0059(18) C15B 0.073(2) 0.062(2) 0.088(3) -0.007(2) -0.012(2) 0.0160(19) C16B 0.079(3) 0.077(2) 0.087(3) -0.008(2) -0.005(2) 0.016(2) C17B 0.106(3) 0.077(3) 0.097(3) 0.001(2) -0.020(3) 0.018(3) C18B 0.085(3) 0.080(3) 0.127(4) -0.012(3) -0.028(3) 0.013(2) C19B 0.082(3) 0.085(3) 0.097(3) -0.003(2) -0.025(2) 0.007(2) C20B 0.076(3) 0.075(2) 0.092(3) -0.004(2) -0.016(2) 0.013(2) S1B 0.0808(14) 0.0823(14) 0.1137(18) 0.0029(13) 0.0018(12) 0.0046(11) O41B 0.094(2) 0.095(2) 0.106(2) -0.0302(18) -0.0235(18) 0.0280(16) C211 0.111(3) 0.095(3) 0.100(3) -0.013(3) -0.020(3) -0.002(3) C221 0.106(4) 0.162(5) 0.137(4) -0.042(4) -0.004(3) 0.058(4) S2B 0.1056(16) 0.0650(12) 0.0945(17) -0.0035(11) -0.0061(13) -0.0083(11) O42B 0.094(2) 0.095(2) 0.106(2) -0.0302(18) -0.0235(18) 0.0280(16) C212 0.111(3) 0.095(3) 0.100(3) -0.013(3) -0.020(3) -0.002(3) C222 0.106(4) 0.162(5) 0.137(4) -0.042(4) -0.004(3) 0.058(4) Mn3 0.0552(3) 0.0642(3) 0.0904(4) -0.0104(3) -0.0067(3) 0.0054(2) O1C 0.0590(14) 0.0731(15) 0.0999(19) -0.0169(14) -0.0113(13) 0.0074(12) O2C 0.0555(13) 0.0679(15) 0.103(2) -0.0118(14) -0.0069(13) 0.0093(12) O3C 0.0525(13) 0.0758(15) 0.0936(18) -0.0138(14) -0.0037(13) 0.0076(12) O4C 0.0604(14) 0.0714(15) 0.104(2) -0.0021(14) 0.0054(13) 0.0058(12) N1C 0.0485(15) 0.0638(17) 0.099(2) -0.0093(16) -0.0019(15) 0.0059(13) N2C 0.0557(16) 0.0576(16) 0.093(2) -0.0156(15) 0.0005(15) 0.0068(13) C1C 0.063(2) 0.058(2) 0.090(3) -0.0077(18) -0.0027(19) 0.0085(17) C2C 0.0545(19) 0.061(2) 0.090(3) -0.0071(19) 0.0008(18) 0.0072(16) C3C 0.060(2) 0.072(2) 0.088(3) -0.012(2) -0.0056(19) 0.0140(18) C4C 0.078(3) 0.107(3) 0.106(3) -0.011(3) -0.012(2) 0.038(3) C5C 0.100(3) 0.116(4) 0.101(4) -0.024(3) -0.015(3) 0.051(3) C6C 0.108(3) 0.085(3) 0.104(3) -0.001(3) 0.007(3) 0.042(3) C7C 0.086(3) 0.073(3) 0.120(4) -0.012(2) -0.004(3) 0.014(2) C8C 0.075(2) 0.070(2) 0.103(3) -0.024(2) -0.013(2) 0.007(2) C9C 0.074(2) 0.056(2) 0.097(3) -0.0084(19) -0.006(2) 0.0120(18) C10C 0.071(2) 0.078(2) 0.103(3) -0.005(2) 0.002(2) 0.018(2) C11C 0.057(2) 0.060(2) 0.088(3) -0.0077(18) -0.0056(18) 0.0039(17) C12C 0.0531(19) 0.064(2) 0.094(3) -0.002(2) -0.0040(19) 0.0006(17) C13C 0.060(2) 0.061(2) 0.095(3) -0.0134(19) 0.0002(19) 0.0065(17) C14C 0.0534(19) 0.062(2) 0.095(3) -0.0027(19) -0.0020(18) 0.0023(16) C15C 0.0562(19) 0.0534(18) 0.093(3) -0.0026(18) 0.0091(18) -0.0005(16) C16C 0.056(2) 0.055(2) 0.119(3) -0.003(2) -0.007(2) -0.0008(17) C17C 0.075(2) 0.061(2) 0.121(3) -0.004(2) 0.010(2) 0.006(2) C18C 0.072(2) 0.062(2) 0.133(4) -0.020(2) 0.013(2) 0.0084(19) C19C 0.076(3) 0.062(2) 0.125(4) -0.022(2) -0.002(2) 0.002(2) C20C 0.058(2) 0.063(2) 0.104(3) 0.000(2) -0.001(2) 0.0012(17) C21C 0.114(6) 0.116(5) 0.232(9) 0.065(5) 0.089(6) 0.038(4) C22C 0.167(12) 0.265(16) 0.33(3) 0.163(17) 0.148(15) 0.084(11) C23C 0.114(6) 0.116(5) 0.232(9) 0.065(5) 0.089(6) 0.038(4) C24C 0.076(11) 0.17(2) 0.128(19) 0.003(16) 0.039(12) -0.047(13) Mn4 0.0617(3) 0.0627(3) 0.0984(5) -0.0158(3) -0.0063(3) 0.0038(3) S1D 0.0770(8) 0.1576(14) 0.1905(17) -0.0189(13) -0.0138(9) 0.0022(9) O1D 0.0989(19) 0.0604(15) 0.107(2) -0.0179(14) -0.0085(17) 0.0137(14) O2D 0.0746(16) 0.0731(16) 0.099(2) -0.0200(14) -0.0085(14) 0.0059(13) O3D 0.0674(15) 0.0660(15) 0.106(2) -0.0172(14) 0.0039(14) 0.0054(12) O4D 0.0664(17) 0.113(2) 0.137(3) -0.029(2) -0.0124(17) 0.0098(16) N1D 0.0634(17) 0.0593(17) 0.084(2) -0.0082(16) -0.0056(16) -0.0020(14) N2D 0.0617(17) 0.073(2) 0.096(2) -0.0154(18) -0.0002(17) -0.0018(15) C1D 0.072(2) 0.077(3) 0.091(3) -0.018(2) -0.014(2) 0.006(2) C2D 0.081(3) 0.062(2) 0.100(3) -0.002(2) -0.008(2) 0.002(2) C3D 0.110(4) 0.082(3) 0.127(4) -0.004(3) 0.015(3) 0.005(3) C4D 0.122(4) 0.105(4) 0.122(4) 0.010(3) 0.026(3) 0.002(3) C5D 0.112(4) 0.084(3) 0.138(4) -0.007(3) 0.038(3) 0.008(3) C6D 0.085(3) 0.094(3) 0.112(4) -0.019(3) 0.006(3) -0.003(3) C7D 0.067(2) 0.078(3) 0.099(3) -0.020(2) -0.006(2) -0.005(2) C8D 0.073(2) 0.064(2) 0.087(3) -0.012(2) -0.004(2) -0.0016(19) C9D 0.077(2) 0.074(2) 0.092(3) -0.011(2) 0.004(2) -0.002(2) C10D 0.075(3) 0.085(3) 0.104(3) 0.000(3) 0.007(2) 0.000(2) C11D 0.061(2) 0.067(2) 0.084(3) -0.013(2) -0.0117(19) -0.0010(18) C12D 0.059(2) 0.071(2) 0.100(3) -0.007(2) -0.011(2) -0.0019(19) C13D 0.068(2) 0.075(2) 0.093(3) -0.012(2) 0.006(2) 0.0018(19) C14D 0.094(3) 0.078(3) 0.106(4) -0.007(3) 0.002(3) 0.004(2) C15D 0.112(4) 0.085(3) 0.112(4) -0.002(3) 0.020(3) 0.018(3) C16D 0.076(3) 0.097(3) 0.122(4) -0.005(3) 0.009(3) 0.002(2) C17D 0.120(4) 0.118(4) 0.130(5) 0.013(4) 0.024(4) 0.003(3) C18D 0.210(8) 0.154(7) 0.156(7) 0.018(5) 0.068(6) -0.037(6) C19D 0.374(15) 0.113(5) 0.187(8) -0.010(5) 0.135(9) -0.025(7) C20D 0.237(8) 0.112(5) 0.156(6) -0.014(5) 0.077(6) 0.000(5) C21D 0.117(5) 0.226(8) 0.247(9) 0.008(7) -0.018(5) 0.082(6) C22D 0.141(6) 0.170(7) 0.410(16) -0.058(9) 0.006(8) -0.063(6) S1S 0.0783(6) 0.0713(6) 0.1171(9) -0.0011(6) 0.0100(6) 0.0054(5) O1S 0.0703(16) 0.0651(15) 0.131(2) -0.0113(16) 0.0006(15) 0.0036(13) C1S 0.134(4) 0.065(2) 0.115(4) 0.000(2) 0.016(3) 0.001(3) C2S 0.094(3) 0.096(3) 0.141(4) -0.023(3) -0.017(3) -0.003(3) S21S 0.0926(10) 0.0755(9) 0.1202(13) 0.0070(8) -0.0220(9) -0.0045(7) S22S 0.088(4) 0.066(3) 0.131(6) 0.010(3) -0.034(4) -0.007(3) O2S 0.0789(18) 0.0833(19) 0.137(3) -0.0003(18) -0.0018(18) -0.0053(15) C3S 0.143(4) 0.088(3) 0.120(4) -0.001(3) -0.028(3) -0.023(3) C4S 0.101(4) 0.152(5) 0.137(5) 0.027(4) 0.024(3) 0.011(4) _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 Mn1 O1A 1.881(3) . ? Mn1 N1A 1.933(3) . ? Mn1 O3A 1.936(2) . ? Mn1 O2D 1.947(3) 4 ? Mn1 O4A 2.215(3) . ? Mn1 N2D 2.264(3) 4 ? O1A C1A 1.327(5) . ? O2A C11A 1.265(5) . ? O2A Mn2 1.961(3) . ? O3A C12A 1.280(4) . ? O4A C21A 1.459(5) . ? N1A C11A 1.351(5) . ? N1A N2A 1.402(4) . ? N2A C12A 1.322(5) . ? N2A Mn2 2.274(3) . ? C1A C8A 1.387(6) . ? C1A C2A 1.470(6) . ? C2A C3A 1.369(6) . ? C2A C11A 1.481(6) . ? C3A C10A 1.398(6) . ? C4A C5A 1.392(8) . ? C4A C10A 1.423(7) . ? C5A C6A 1.391(10) . ? C6A C7A 1.350(9) . ? C7A C9A 1.428(7) . ? C8A C9A 1.389(7) . ? C9A C10A 1.425(7) . ? C12A C13A 1.448(5) . ? C13A C14A 1.323(5) . ? C14A C15A 1.468(5) . ? C15A C20A 1.381(5) . ? C15A C16A 1.407(5) . ? C16A C17A 1.382(5) . ? C17A C18A 1.373(6) . ? C18A C19A 1.361(5) . ? C19A C20A 1.353(5) . ? C21A C22A 1.420(7) . ? Mn2 O1B 1.847(3) . ? Mn2 O3B 1.919(2) . ? Mn2 N1B 1.941(3) . ? Mn2 O41B 2.204(3) . ? O1B C1B 1.330(5) . ? O2B C11B 1.287(4) . ? O2B Mn3 1.976(2) . ? O3B C12B 1.318(4) . ? N1B C11B 1.304(5) . ? N1B N2B 1.418(4) . ? N2B C12B 1.299(5) . ? N2B Mn3 2.246(3) . ? C1B C8B 1.390(5) . ? C1B C2B 1.439(5) . ? C2B C3B 1.356(5) . ? C2B C11B 1.498(5) . ? C3B C10B 1.405(5) . ? C4B C5B 1.372(6) . ? C4B C10B 1.402(6) . ? C5B C6B 1.402(7) . ? C6B C7B 1.336(6) . ? C7B C9B 1.420(6) . ? C8B C9B 1.399(6) . ? C9B C10B 1.432(6) . ? C12B C13B 1.462(5) . ? C13B C14B 1.310(5) . ? C14B C15B 1.484(5) . ? C15B C16B 1.364(6) . ? C15B C20B 1.397(5) . ? C16B C17B 1.410(6) . ? C17B C18B 1.356(6) . ? C18B C19B 1.394(6) . ? C19B C20B 1.352(5) . ? S1B O41B 1.369(4) . ? S1B C211 1.788(6) . ? S1B C221 1.907(6) . ? Mn3 O1C 1.856(2) . ? Mn3 O3C 1.935(2) . ? Mn3 N1C 1.951(3) . ? Mn3 O4C 2.218(3) . ? O1C C1C 1.328(4) . ? O2C C11C 1.282(4) . ? O2C Mn4 1.991(2) . ? O3C C12C 1.305(4) . ? O4C C21C 1.432(6) . ? N1C C11C 1.317(4) . ? N1C N2C 1.408(4) . ? N2C C12C 1.304(4) . ? N2C Mn4 2.265(3) . ? C1C C8C 1.381(5) . ? C1C C2C 1.425(5) . ? C2C C3C 1.399(5) . ? C2C C11C 1.472(5) . ? C3C C10C 1.395(5) . ? C4C C5C 1.356(6) . ? C4C C10C 1.409(5) . ? C5C C6C 1.393(7) . ? C6C C7C 1.349(6) . ? C7C C9C 1.411(5) . ? C8C C9C 1.402(5) . ? C9C C10C 1.435(6) . ? C12C C13C 1.438(5) . ? C13C C14C 1.341(5) . ? C14C C15C 1.475(5) . ? C15C C16C 1.394(5) . ? C15C C20C 1.404(5) . ? C16C C17C 1.405(6) . ? C17C C18C 1.403(6) . ? C18C C19C 1.361(5) . ? C19C C20C 1.371(5) . ? C21C C22C 1.327(13) . ? Mn4 O1D 1.831(3) . ? Mn4 O3D 1.916(3) . ? Mn4 N1D 1.953(3) . ? Mn4 O4D 2.213(3) . ? S1D O4D 1.466(3) . ? S1D C21D 1.770(7) . ? S1D C22D 1.807(7) . ? O1D C1D 1.342(5) . ? O2D C11D 1.295(4) . ? O2D Mn1 1.947(3) 3 ? O3D C12D 1.342(4) . ? N1D C11D 1.315(5) . ? N1D N2D 1.410(4) . ? N2D C12D 1.291(5) . ? N2D Mn1 2.264(3) 3 ? C1D C2D 1.365(6) . ? C1D C8D 1.456(5) . ? C2D C10D 1.402(6) . ? C3D C4D 1.400(7) . ? C3D C10D 1.407(6) . ? C4D C5D 1.382(7) . ? C5D C6D 1.344(6) . ? C6D C9D 1.430(6) . ? C7D C8D 1.378(5) . ? C7D C9D 1.394(6) . ? C8D C11D 1.447(5) . ? C9D C10D 1.426(6) . ? C12D C13D 1.454(6) . ? C13D C14D 1.305(6) . ? C14D C15D 1.414(7) . ? C15D C20D 1.403(8) . ? C15D C16D 1.410(7) . ? C16D C17D 1.356(7) . ? C17D C18D 1.397(9) . ? C18D C19D 1.390(10) . ? C19D C20D 1.383(9) . ? S1S O1S 1.513(3) . ? S1S C1S 1.782(4) . ? S1S C2S 1.787(5) . ? S21S O2S 1.500(3) . ? S21S C4S 1.796(6) . ? S21S C3S 1.810(5) . ? S22S C4S 1.567(9) . ? S22S O2S 1.595(7) . ? S22S C3S 1.920(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 O1A Mn1 N1A 90.75(13) . . ? O1A Mn1 O3A 170.43(12) . . ? N1A Mn1 O3A 79.90(12) . . ? O1A Mn1 O2D 95.96(12) . 4 ? N1A Mn1 O2D 173.27(12) . 4 ? O3A Mn1 O2D 93.41(11) . 4 ? O1A Mn1 O4A 92.67(11) . . ? N1A Mn1 O4A 92.52(12) . . ? O3A Mn1 O4A 85.73(11) . . ? O2D Mn1 O4A 87.64(11) 4 . ? O1A Mn1 N2D 92.69(11) . 4 ? N1A Mn1 N2D 104.13(13) . 4 ? O3A Mn1 N2D 91.62(11) . 4 ? O2D Mn1 N2D 75.16(12) 4 4 ? O4A Mn1 N2D 162.43(12) . 4 ? C1A O1A Mn1 126.2(3) . . ? C11A O2A Mn2 119.1(2) . . ? C12A O3A Mn1 113.0(2) . . ? C21A O4A Mn1 127.8(3) . . ? C11A N1A N2A 112.8(3) . . ? C11A N1A Mn1 133.0(3) . . ? N2A N1A Mn1 114.2(2) . . ? C12A N2A N1A 109.9(3) . . ? C12A N2A Mn2 141.3(3) . . ? N1A N2A Mn2 108.6(2) . . ? O1A C1A C8A 119.2(5) . . ? O1A C1A C2A 124.1(4) . . ? C8A C1A C2A 116.7(4) . . ? C3A C2A C1A 120.1(4) . . ? C3A C2A C11A 117.1(5) . . ? C1A C2A C11A 122.8(4) . . ? C2A C3A C10A 122.6(5) . . ? C5A C4A C10A 117.5(6) . . ? C6A C5A C4A 122.3(6) . . ? C7A C6A C5A 120.0(6) . . ? C6A C7A C9A 121.9(7) . . ? C1A C8A C9A 122.4(5) . . ? C8A C9A C10A 120.8(5) . . ? C8A C9A C7A 122.0(6) . . ? C10A C9A C7A 117.2(5) . . ? C3A C10A C4A 121.6(6) . . ? C3A C10A C9A 117.4(5) . . ? C4A C10A C9A 121.0(5) . . ? O2A C11A N1A 123.9(4) . . ? O2A C11A C2A 119.5(4) . . ? N1A C11A C2A 116.6(4) . . ? O3A C12A N2A 121.8(4) . . ? O3A C12A C13A 120.2(3) . . ? N2A C12A C13A 117.9(4) . . ? C14A C13A C12A 124.4(4) . . ? C13A C14A C15A 126.5(4) . . ? C20A C15A C16A 117.8(3) . . ? C20A C15A C14A 123.7(3) . . ? C16A C15A C14A 118.5(4) . . ? C17A C16A C15A 119.0(4) . . ? C18A C17A C16A 120.8(4) . . ? C19A C18A C17A 120.1(4) . . ? C20A C19A C18A 119.7(4) . . ? C19A C20A C15A 122.4(3) . . ? C22A C21A O4A 112.7(4) . . ? O1B Mn2 O3B 171.72(12) . . ? O1B Mn2 N1B 91.42(13) . . ? O3B Mn2 N1B 80.30(12) . . ? O1B Mn2 O2A 93.98(12) . . ? O3B Mn2 O2A 94.29(11) . . ? N1B Mn2 O2A 174.04(13) . . ? O1B Mn2 O41B 91.11(12) . . ? O3B Mn2 O41B 89.99(11) . . ? N1B Mn2 O41B 96.51(13) . . ? O2A Mn2 O41B 85.91(13) . . ? O1B Mn2 N2A 91.43(13) . . ? O3B Mn2 N2A 90.11(12) . . ? N1B Mn2 N2A 101.68(12) . . ? O2A Mn2 N2A 75.70(11) . . ? O41B Mn2 N2A 161.56(12) . . ? C1B O1B Mn2 130.2(2) . . ? C11B O2B Mn3 118.1(2) . . ? C12B O3B Mn2 113.0(2) . . ? C11B N1B N2B 113.7(3) . . ? C11B N1B Mn2 131.6(3) . . ? N2B N1B Mn2 114.7(2) . . ? C12B N2B N1B 109.6(3) . . ? C12B N2B Mn3 141.2(3) . . ? N1B N2B Mn3 108.4(2) . . ? O1B C1B C8B 117.3(4) . . ? O1B C1B C2B 124.7(3) . . ? C8B C1B C2B 118.0(4) . . ? C3B C2B C1B 119.5(3) . . ? C3B C2B C11B 119.1(3) . . ? C1B C2B C11B 121.4(4) . . ? C2B C3B C10B 123.4(4) . . ? C5B C4B C10B 120.3(4) . . ? C4B C5B C6B 120.6(5) . . ? C7B C6B C5B 120.7(4) . . ? C6B C7B C9B 121.2(5) . . ? C1B C8B C9B 122.5(4) . . ? C8B C9B C7B 122.8(4) . . ? C8B C9B C10B 118.9(4) . . ? C7B C9B C10B 118.3(4) . . ? C4B C10B C3B 123.4(4) . . ? C4B C10B C9B 118.8(4) . . ? C3B C10B C9B 117.6(4) . . ? O2B C11B N1B 123.2(3) . . ? O2B C11B C2B 116.5(4) . . ? N1B C11B C2B 120.2(4) . . ? N2B C12B O3B 122.3(3) . . ? N2B C12B C13B 119.8(4) . . ? O3B C12B C13B 117.9(4) . . ? C14B C13B C12B 123.3(4) . . ? C13B C14B C15B 127.8(4) . . ? C16B C15B C20B 119.5(4) . . ? C16B C15B C14B 120.2(4) . . ? C20B C15B C14B 120.3(4) . . ? C15B C16B C17B 119.4(4) . . ? C18B C17B C16B 119.7(5) . . ? C17B C18B C19B 121.2(4) . . ? C20B C19B C18B 118.6(5) . . ? C19B C20B C15B 121.5(4) . . ? O41B S1B C211 110.8(2) . . ? O41B S1B C221 101.6(3) . . ? C211 S1B C221 93.6(3) . . ? S1B O41B Mn2 132.3(2) . . ? O1C Mn3 O3C 170.17(10) . . ? O1C Mn3 N1C 90.34(11) . . ? O3C Mn3 N1C 79.95(11) . . ? O1C Mn3 O2B 94.83(10) . . ? O3C Mn3 O2B 94.93(10) . . ? N1C Mn3 O2B 174.51(11) . . ? O1C Mn3 O4C 91.01(11) . . ? O3C Mn3 O4C 87.94(10) . . ? N1C Mn3 O4C 92.53(11) . . ? O2B Mn3 O4C 89.27(10) . . ? O1C Mn3 N2B 88.98(12) . . ? O3C Mn3 N2B 94.63(11) . . ? N1C Mn3 N2B 102.98(12) . . ? O2B Mn3 N2B 75.28(11) . . ? O4C Mn3 N2B 164.49(10) . . ? C1C O1C Mn3 126.1(2) . . ? C11C O2C Mn4 119.6(2) . . ? C12C O3C Mn3 113.1(2) . . ? C21C O4C Mn3 122.5(3) . . ? C11C N1C N2C 114.2(3) . . ? C11C N1C Mn3 131.2(2) . . ? N2C N1C Mn3 114.32(19) . . ? C12C N2C N1C 110.3(3) . . ? C12C N2C Mn4 140.2(3) . . ? N1C N2C Mn4 109.08(19) . . ? O1C C1C C8C 118.1(3) . . ? O1C C1C C2C 123.7(3) . . ? C8C C1C C2C 118.2(3) . . ? C3C C2C C1C 119.9(3) . . ? C3C C2C C11C 117.2(3) . . ? C1C C2C C11C 122.9(3) . . ? C10C C3C C2C 121.4(4) . . ? C5C C4C C10C 120.5(5) . . ? C4C C5C C6C 120.5(4) . . ? C7C C6C C5C 120.8(4) . . ? C6C C7C C9C 121.3(4) . . ? C1C C8C C9C 122.5(4) . . ? C8C C9C C7C 123.8(4) . . ? C8C C9C C10C 118.7(3) . . ? C7C C9C C10C 117.5(4) . . ? C3C C10C C4C 122.1(4) . . ? C3C C10C C9C 118.7(3) . . ? C4C C10C C9C 119.2(4) . . ? O2C C11C N1C 122.3(3) . . ? O2C C11C C2C 118.8(3) . . ? N1C C11C C2C 118.8(3) . . ? N2C C12C O3C 122.1(3) . . ? N2C C12C C13C 117.7(3) . . ? O3C C12C C13C 120.1(3) . . ? C14C C13C C12C 122.6(4) . . ? C13C C14C C15C 125.6(4) . . ? C16C C15C C20C 118.2(3) . . ? C16C C15C C14C 118.7(3) . . ? C20C C15C C14C 123.1(3) . . ? C15C C16C C17C 121.1(4) . . ? C18C C17C C16C 117.8(4) . . ? C19C C18C C17C 121.4(4) . . ? C18C C19C C20C 120.4(4) . . ? C19C C20C C15C 121.0(3) . . ? C22C C21C O4C 125.3(7) . . ? O1D Mn4 O3D 170.85(11) . . ? O1D Mn4 N1D 90.22(13) . . ? O3D Mn4 N1D 80.77(12) . . ? O1D Mn4 O2C 97.46(11) . . ? O3D Mn4 O2C 91.55(11) . . ? N1D Mn4 O2C 172.31(13) . . ? O1D Mn4 O4D 89.27(13) . . ? O3D Mn4 O4D 89.56(12) . . ? N1D Mn4 O4D 93.09(12) . . ? O2C Mn4 O4D 87.16(11) . . ? O1D Mn4 N2C 92.76(12) . . ? O3D Mn4 N2C 91.19(11) . . ? N1D Mn4 N2C 105.05(11) . . ? O2C Mn4 N2C 74.57(10) . . ? O4D Mn4 N2C 161.73(11) . . ? O4D S1D C21D 105.1(3) . . ? O4D S1D C22D 103.8(3) . . ? C21D S1D C22D 98.2(5) . . ? C1D O1D Mn4 132.5(3) . . ? C11D O2D Mn1 120.6(3) . 3 ? C12D O3D Mn4 112.4(3) . . ? S1D O4D Mn4 122.9(2) . . ? C11D N1D N2D 114.6(3) . . ? C11D N1D Mn4 131.4(3) . . ? N2D N1D Mn4 113.8(2) . . ? C12D N2D N1D 111.0(3) . . ? C12D N2D Mn1 140.7(3) . 3 ? N1D N2D Mn1 108.3(2) . 3 ? O1D C1D C2D 120.5(4) . . ? O1D C1D C8D 121.3(4) . . ? C2D C1D C8D 118.2(4) . . ? C1D C2D C10D 123.2(4) . . ? C4D C3D C10D 119.1(5) . . ? C5D C4D C3D 122.7(5) . . ? C6D C5D C4D 119.1(5) . . ? C5D C6D C9D 121.5(5) . . ? C8D C7D C9D 123.3(4) . . ? C7D C8D C11D 118.1(4) . . ? C7D C8D C1D 118.4(4) . . ? C11D C8D C1D 123.5(4) . . ? C7D C9D C10D 118.0(4) . . ? C7D C9D C6D 122.7(4) . . ? C10D C9D C6D 119.3(4) . . ? C2D C10D C3D 122.9(4) . . ? C2D C10D C9D 118.8(4) . . ? C3D C10D C9D 118.3(4) . . ? O2D C11D N1D 121.3(4) . . ? O2D C11D C8D 118.6(4) . . ? N1D C11D C8D 120.1(3) . . ? N2D C12D O3D 121.7(4) . . ? N2D C12D C13D 120.8(4) . . ? O3D C12D C13D 117.6(4) . . ? C14D C13D C12D 124.5(4) . . ? C13D C14D C15D 127.8(4) . . ? C20D C15D C16D 115.0(5) . . ? C20D C15D C14D 121.0(5) . . ? C16D C15D C14D 124.0(5) . . ? C17D C16D C15D 124.1(5) . . ? C16D C17D C18D 118.1(6) . . ? C19D C18D C17D 121.4(7) . . ? C20D C19D C18D 118.0(7) . . ? C19D C20D C15D 123.1(7) . . ? O1S S1S C1S 103.5(2) . . ? O1S S1S C2S 106.7(2) . . ? C1S S1S C2S 98.8(3) . . ? O2S S21S C4S 105.2(2) . . ? O2S S21S C3S 103.7(2) . . ? C4S S21S C3S 102.5(3) . . ? C4S S22S O2S 112.2(5) . . ? C4S S22S C3S 107.0(5) . . ? O2S S22S C3S 95.5(4) . . ? S21S O2S S22S 53.2(3) . . ? S21S C3S S22S 43.6(2) . . ? S22S C4S S21S 48.2(3) . . ? _diffrn_measured_fraction_theta_max 0.995 _diffrn_reflns_theta_full 30.42 _diffrn_measured_fraction_theta_full 0.995 _refine_diff_density_max 0.607 _refine_diff_density_min -0.569 _refine_diff_density_rms 0.082 #===END