# Electronic Supplementary Material (ESI) for Dalton Transactions # This journal is © The Royal Society of Chemistry 2011 data_global _journal_name_full 'Dalton Trans.' _journal_coden_cambridge 0222 _journal_year ? _journal_volume ? _journal_page_first ? _publ_contact_author_email skkar_cu@yahoo.co.in _publ_contact_author_name 'Susanta Kar' _publ_author_name 'Susanta Kar' data_sksr37a _database_code_depnum_ccdc_archive 'CCDC 796250' #TrackingRef 'Rev. complex1.cif' _alert_response ; Alert C PLat 041, 044, 068, Calculated and Reported Values for formula, denisty, molecular mass and F000 value. Response A water molecule was present as the solvent molecule which was removed using SQUEEZE. Thus two hydrogen atoms and one oxygen atom of water molecule were added to the chemical formula to adjust the density, molecular mass and F000 value. Results in the chemical_formula_moiety C72 H72 Mn5 N30 O6, 4(Cl O4), (H2 O). ; _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety 'C72 H72 Mn5 N30 O6, 4(Cl O4), (H2 O)' _chemical_formula_sum 'C72 H74 Cl4 Mn5 N30 O23' _chemical_formula_weight 2144.10 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' Mn Mn 0.3368 0.7283 '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 Triclinic _symmetry_space_group_name_H-M P-1 _symmetry_space_group_name_Hall '-P 1' loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, -y, -z' _cell_length_a 13.832(6) _cell_length_b 14.491(6) _cell_length_c 25.245(11) _cell_angle_alpha 89.257(6) _cell_angle_beta 88.790(6) _cell_angle_gamma 61.571(5) _cell_volume 4449(3) _cell_formula_units_Z 2 _cell_measurement_temperature 150(2) _cell_measurement_reflns_used 57068 _cell_measurement_theta_min 0.8 _cell_measurement_theta_max 30.8 _exptl_crystal_description Rectangular _exptl_crystal_colour White _exptl_crystal_size_max 0.15 _exptl_crystal_size_mid 0.14 _exptl_crystal_size_min 0.12 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.608 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 2194 _exptl_absorpt_coefficient_mu 0.899 _exptl_absorpt_correction_type Empirical _exptl_absorpt_correction_T_min 0.9094 _exptl_absorpt_correction_T_max 0.9265 _exptl_absorpt_process_details SADABS _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 50768 _diffrn_reflns_av_R_equivalents 0.0259 _diffrn_reflns_av_sigmaI/netI 0.0457 _diffrn_reflns_limit_h_min -19 _diffrn_reflns_limit_h_max 19 _diffrn_reflns_limit_k_min -20 _diffrn_reflns_limit_k_max 20 _diffrn_reflns_limit_l_min -35 _diffrn_reflns_limit_l_max 35 _diffrn_reflns_theta_min 0.81 _diffrn_reflns_theta_max 30.75 _reflns_number_total 27211 _reflns_number_gt 21031 _reflns_threshold_expression >2\s(I) _computing_data_collection 'Bruker SMART' _computing_cell_refinement 'Bruker SMART' _computing_data_reduction 'Bruker SAINT' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'Ortep-3 for Windows (Farrugia, 1997)' _computing_publication_material 'WINGX V1.80.05' _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^ > 2\s(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^)+(0.0897P)^2^+3.6459P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment constr _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 27211 _refine_ls_number_parameters 1211 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0689 _refine_ls_R_factor_gt 0.0587 _refine_ls_wR_factor_ref 0.1675 _refine_ls_wR_factor_gt 0.1611 _refine_ls_goodness_of_fit_ref 1.100 _refine_ls_restrained_S_all 1.100 _refine_ls_shift/su_max 0.002 _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 Mn5 Mn 0.54077(5) 0.81685(5) 0.85255(2) 0.02283(12) Uani 1 1 d . . . Mn3 Mn 0.76873(5) 0.48203(5) 0.75042(2) 0.02181(11) Uani 1 1 d . . . Mn2 Mn 0.48023(5) 0.72288(5) 0.71701(2) 0.02275(12) Uani 1 1 d . . . Mn1 Mn 0.65342(5) 0.83767(5) 0.65097(2) 0.02292(12) Uani 1 1 d . . . Mn4 Mn 0.82054(5) 0.72144(5) 0.78129(2) 0.02195(11) Uani 1 1 d . . . Cl3 Cl 0.28282(10) 0.44141(9) 0.74673(5) 0.0384(2) Uani 1 1 d . . . Cl4 Cl 1.01633(11) 0.97886(10) 0.75262(6) 0.0467(3) Uani 1 1 d . . . Cl1 Cl 1.27018(11) 0.78585(13) 0.51767(5) 0.0474(3) Uani 1 1 d . . . Cl2 Cl 0.98229(10) 0.74035(11) 0.98220(4) 0.0423(3) Uani 1 1 d . . . O4 O 0.8271(2) 0.5954(2) 0.73062(10) 0.0218(5) Uani 1 1 d . . . N17 N 0.8523(3) 0.4440(3) 0.67252(13) 0.0234(6) Uani 1 1 d . . . O5 O 0.7102(2) 0.7025(2) 0.83765(10) 0.0243(5) Uani 1 1 d . . . O3 O 0.5966(2) 0.5936(2) 0.76806(10) 0.0237(5) Uani 1 1 d . . . N12 N 0.7201(3) 0.4403(3) 0.82660(13) 0.0244(6) Uani 1 1 d . . . O6 O 0.4763(2) 0.8402(2) 0.77258(11) 0.0260(5) Uani 1 1 d . . . O1 O 0.6968(2) 0.8475(2) 0.73253(10) 0.0230(5) Uani 1 1 d . . . N26 N 0.5902(3) 0.9043(3) 0.91410(14) 0.0288(7) Uani 1 1 d . . . C39 C 0.6946(4) 0.2209(4) 0.6523(2) 0.0401(11) Uani 1 1 d . . . H39 H 0.6830 0.1728 0.6331 0.048 Uiso 1 1 calc R . . O2 O 0.6042(2) 0.7172(2) 0.66128(10) 0.0253(5) Uani 1 1 d . . . N19 N 0.9457(3) 0.6953(3) 0.71955(14) 0.0263(7) Uani 1 1 d . . . N14 N 0.3776(3) 0.6920(3) 0.77467(14) 0.0283(7) Uani 1 1 d . . . C46 C 1.0490(3) 0.6086(4) 0.64900(16) 0.0281(8) Uani 1 1 d . . . H46 H 1.0780 0.5615 0.6210 0.034 Uiso 1 1 calc R . . N16 N 0.7285(3) 0.3651(3) 0.70868(14) 0.0297(7) Uani 1 1 d . . . N13 N 0.6090(3) 0.4854(3) 0.83968(13) 0.0249(6) Uani 1 1 d . . . N15 N 0.2710(3) 0.7317(3) 0.78831(15) 0.0315(8) Uani 1 1 d . . . H15N H 0.2183 0.7804 0.7708 0.038 Uiso 1 1 calc R . . N25 N 1.0357(3) 0.5403(3) 0.84897(15) 0.0314(7) Uani 1 1 d . . . H25N H 1.0881 0.5378 0.8290 0.038 Uiso 1 1 calc R . . N27 N 0.4575(3) 0.9847(3) 0.83439(14) 0.0264(7) Uani 1 1 d . . . C65 C 0.5409(3) 1.0091(4) 0.90801(18) 0.0314(9) Uani 1 1 d . . . C33 C 0.4326(3) 0.6183(3) 0.81135(15) 0.0236(7) Uani 1 1 d . . . C9 C 0.7218(3) 0.9568(3) 0.79316(15) 0.0249(7) Uani 1 1 d . . . O8 O 1.2297(6) 0.7138(6) 0.50836(19) 0.098(2) Uani 1 1 d . . . N18 N 0.9169(3) 0.4902(3) 0.65836(13) 0.0245(6) Uani 1 1 d . . . C71 C 0.2138(3) 1.0210(4) 0.65232(18) 0.0321(9) Uani 1 1 d . . . C3 C 0.3387(4) 1.0614(5) 0.5289(2) 0.0480(13) Uani 1 1 d . . . H3 H 0.2808 1.1049 0.5072 0.058 Uiso 1 1 calc R . . C26 C 1.1157(4) 0.2561(4) 0.8031(2) 0.0449(12) Uani 1 1 d . . . H26 H 1.1866 0.2337 0.7899 0.054 Uiso 1 1 calc R . . C18 C 0.8195(3) 0.7101(4) 0.56224(16) 0.0316(9) Uani 1 1 d . . . C38 C 0.6490(5) 0.2506(4) 0.7021(2) 0.0410(11) Uani 1 1 d . . . H38 H 0.6071 0.2225 0.7175 0.049 Uiso 1 1 calc R . . C47 C 1.0780(3) 0.6816(4) 0.66342(17) 0.0294(8) Uani 1 1 d . . . N1 N 0.5117(3) 0.9320(3) 0.59281(14) 0.0292(7) Uani 1 1 d . . . C41 C 0.7743(3) 0.3347(3) 0.65964(16) 0.0268(8) Uani 1 1 d . . . N2 N 0.5639(3) 1.0014(3) 0.67639(14) 0.0263(7) Uani 1 1 d . . . N24 N 0.9280(3) 0.6003(3) 0.83815(14) 0.0279(7) Uani 1 1 d . . . O17 O 0.9752(5) 0.8392(5) 0.9924(2) 0.0758(15) Uani 1 1 d . . . N20 N 1.0134(3) 0.7338(3) 0.70538(15) 0.0286(7) Uani 1 1 d . . . H20N H 1.0155 0.7853 0.7210 0.034 Uiso 1 1 calc R . . N11 N 0.9235(3) 0.3680(3) 0.79432(14) 0.0303(7) Uani 1 1 d . . . N22 N 0.5892(3) 0.6876(3) 0.91044(13) 0.0291(7) Uani 1 1 d . . . N5 N 0.8294(3) 0.9033(3) 0.85869(14) 0.0286(7) Uani 1 1 d . . . H5N H 0.8760 0.8624 0.8814 0.034 Uiso 1 1 calc R . . C20 C 0.6287(3) 0.6547(3) 0.62075(15) 0.0250(7) Uani 1 1 d . . . C21 C 0.5706(3) 0.5933(3) 0.61728(15) 0.0268(8) Uani 1 1 d . . . C2 C 0.3985(4) 0.9579(5) 0.51770(19) 0.0410(11) Uani 1 1 d . . . H2 H 0.3820 0.9293 0.4887 0.049 Uiso 1 1 calc R . . N21 N 0.3854(3) 0.8287(3) 0.89427(14) 0.0305(7) Uani 1 1 d . . . C62 C 0.6789(5) 0.9193(5) 0.99173(19) 0.0440(12) Uani 1 1 d . . . H62 H 0.7268 0.8868 1.0195 0.053 Uiso 1 1 calc R . . C35 C 0.2558(3) 0.6870(4) 0.83234(17) 0.0314(9) Uani 1 1 d . . . O19 O 0.3684(6) 0.3766(5) 0.7797(3) 0.114(3) Uani 1 1 d . . . O16 O 0.9162(4) 0.7201(5) 1.01951(17) 0.0679(13) Uani 1 1 d . . . N6 N 0.7955(3) 0.8570(3) 0.61420(15) 0.0303(7) Uani 1 1 d . . . C25 C 1.0265(4) 0.3319(4) 0.77711(19) 0.0389(10) Uani 1 1 d . . . H25 H 1.0389 0.3595 0.7458 0.047 Uiso 1 1 calc R . . N9 N 0.4997(3) 0.6055(3) 0.65702(14) 0.0284(7) Uani 1 1 d . . . N8 N 0.7003(3) 0.6444(3) 0.58263(13) 0.0283(7) Uani 1 1 d . . . C58 C 0.9497(4) 0.5078(4) 0.91405(18) 0.0347(9) Uani 1 1 d . . . H58 H 0.9335 0.4814 0.9448 0.042 Uiso 1 1 calc R . . C27 C 1.0982(4) 0.2138(4) 0.8492(2) 0.0460(12) Uani 1 1 d . . . H27 H 1.1572 0.1614 0.8671 0.055 Uiso 1 1 calc R . . N10 N 0.4556(3) 0.5434(3) 0.64506(15) 0.0334(8) Uani 1 1 d . . . H10N H 0.4077 0.5363 0.6645 0.040 Uiso 1 1 calc R . . N23 N 0.7012(3) 0.6199(3) 0.91599(14) 0.0298(7) Uani 1 1 d . . . C11 C 0.7856(4) 1.0081(4) 0.85930(18) 0.0336(9) Uani 1 1 d . . . C63 C 0.6273(4) 1.0262(5) 0.9857(2) 0.0465(13) Uani 1 1 d . . . H63 H 0.6383 1.0677 1.0101 0.056 Uiso 1 1 calc R . . O13 O 1.1179(4) 0.9064(4) 0.7274(2) 0.0740(15) Uani 1 1 d . . . N29 N 0.3548(3) 0.8761(3) 0.68573(13) 0.0259(7) Uani 1 1 d . . . N4 N 0.7921(3) 0.8695(3) 0.81863(13) 0.0255(7) Uani 1 1 d . . . C68 C 0.4049(3) 0.9375(3) 0.76297(16) 0.0241(7) Uani 1 1 d . . . C49 C 0.2831(4) 0.8996(5) 0.88475(19) 0.0398(11) Uani 1 1 d . . . H49 H 0.2700 0.9451 0.8563 0.048 Uiso 1 1 calc R . . N30 N 0.2804(3) 0.9160(3) 0.64688(14) 0.0293(7) Uani 1 1 d . . . H30N H 0.2756 0.8793 0.6216 0.035 Uiso 1 1 calc R . . C57 C 0.8754(3) 0.5792(3) 0.87802(15) 0.0270(8) Uani 1 1 d . . . C44 C 0.8993(3) 0.5647(3) 0.69190(14) 0.0215(7) Uani 1 1 d . . . C5 C 0.4511(3) 1.0359(4) 0.60377(17) 0.0298(8) Uani 1 1 d . . . C40 C 0.7582(4) 0.2634(4) 0.63088(18) 0.0353(9) Uani 1 1 d . . . H40 H 0.7897 0.2437 0.5972 0.042 Uiso 1 1 calc R . . C64 C 0.5590(4) 1.0722(4) 0.9434(2) 0.0423(11) Uani 1 1 d . . . H64 H 0.5253 1.1445 0.9386 0.051 Uiso 1 1 calc R . . C29 C 0.9058(4) 0.3282(3) 0.84050(16) 0.0288(8) Uani 1 1 d . . . C32 C 0.5535(3) 0.5622(3) 0.80600(14) 0.0220(7) Uani 1 1 d . . . C69 C 0.3353(3) 0.9584(3) 0.71600(16) 0.0252(7) Uani 1 1 d . . . C17 C 0.8498(3) 0.7919(4) 0.57364(16) 0.0302(9) Uani 1 1 d . . . C34 C 0.3596(4) 0.6112(4) 0.84800(17) 0.0304(9) Uani 1 1 d . . . H34 H 0.3767 0.5656 0.8767 0.036 Uiso 1 1 calc R . . C30 C 0.7899(4) 0.3739(3) 0.85873(16) 0.0274(8) Uani 1 1 d . . . C28 C 0.9922(4) 0.2498(4) 0.8685(2) 0.0403(11) Uani 1 1 d . . . H28 H 0.9787 0.2222 0.8995 0.048 Uiso 1 1 calc R . . C51 C 0.2133(5) 0.8394(6) 0.9569(2) 0.0515(15) Uani 1 1 d . . . H51 H 0.1555 0.8436 0.9780 0.062 Uiso 1 1 calc R . . N7 N 0.7393(3) 0.7148(3) 0.59127(13) 0.0287(7) Uani 1 1 d . . . C6 C 0.4821(3) 1.0725(3) 0.65165(18) 0.0305(8) Uani 1 1 d . . . C8 C 0.6693(3) 0.9434(3) 0.74597(15) 0.0226(7) Uani 1 1 d . . . C61 C 0.6574(4) 0.8605(4) 0.95473(17) 0.0359(10) Uani 1 1 d . . . H61 H 0.6914 0.7880 0.9586 0.043 Uiso 1 1 calc R . . O7 O 1.3349(6) 0.7887(6) 0.4744(2) 0.103(3) Uani 1 1 d . . . C12 C 0.8174(5) 1.0622(5) 0.8994(2) 0.0485(13) Uani 1 1 d . . . H12A H 0.8519 1.0155 0.9285 0.073 Uiso 1 1 calc R . . H12B H 0.7531 1.1233 0.9120 0.073 Uiso 1 1 calc R . . H12C H 0.8680 1.0829 0.8836 0.073 Uiso 1 1 calc R . . C16 C 0.9301(4) 0.8044(5) 0.5438(2) 0.0426(12) Uani 1 1 d . . . H16 H 0.9680 0.7589 0.5161 0.051 Uiso 1 1 calc R . . C31 C 0.7604(4) 0.3468(4) 0.91212(18) 0.0408(11) Uani 1 1 d . . . H31A H 0.6821 0.3747 0.9150 0.061 Uiso 1 1 calc R . . H31B H 0.7845 0.3765 0.9393 0.061 Uiso 1 1 calc R . . H31C H 0.7956 0.2719 0.9162 0.061 Uiso 1 1 calc R . . C45 C 0.9656(3) 0.6190(3) 0.68533(15) 0.0229(7) Uani 1 1 d . . . O18 O 0.9437(3) 0.7403(3) 0.92988(14) 0.0474(9) Uani 1 1 d . . . O15 O 1.0940(4) 0.6596(5) 0.98540(18) 0.0771(16) Uani 1 1 d . . . O22 O 0.2288(5) 0.3830(4) 0.7294(2) 0.0789(15) Uani 1 1 d . . . N3 N 0.6000(3) 1.0289(3) 0.72148(14) 0.0293(7) Uani 1 1 d . . . C67 C 0.4157(5) 1.1669(4) 0.8484(3) 0.0530(15) Uani 1 1 d . . . H67A H 0.4704 1.1897 0.8467 0.079 Uiso 1 1 calc R . . H67B H 0.3617 1.2059 0.8752 0.079 Uiso 1 1 calc R . . H67C H 0.3808 1.1783 0.8147 0.079 Uiso 1 1 calc R . . C1 C 0.4853(4) 0.8949(4) 0.55072(17) 0.0351(9) Uani 1 1 d . . . H1 H 0.5265 0.8239 0.5429 0.042 Uiso 1 1 calc R . . C42 C 0.8404(3) 0.3830(3) 0.63962(15) 0.0258(7) Uani 1 1 d . . . C48 C 1.1620(4) 0.7092(5) 0.6411(2) 0.0417(11) Uani 1 1 d . . . H48A H 1.2106 0.7055 0.6687 0.063 Uiso 1 1 calc R . . H48B H 1.1258 0.7791 0.6269 0.063 Uiso 1 1 calc R . . H48C H 1.2036 0.6607 0.6135 0.063 Uiso 1 1 calc R . . C53 C 0.4042(4) 0.7598(4) 0.93485(17) 0.0343(10) Uani 1 1 d . . . C59 C 1.0522(4) 0.4851(4) 0.89413(18) 0.0340(9) Uani 1 1 d . . . C72 C 0.1217(4) 1.0831(5) 0.6153(2) 0.0467(12) Uani 1 1 d . . . H72A H 0.0541 1.0902 0.6303 0.070 Uiso 1 1 calc R . . H72B H 0.1364 1.0476 0.5819 0.070 Uiso 1 1 calc R . . H72C H 0.1156 1.1514 0.6101 0.070 Uiso 1 1 calc R . . O20 O 0.2000(4) 0.5339(4) 0.7711(2) 0.0686(13) Uani 1 1 d . . . C10 C 0.7155(4) 1.0458(4) 0.81748(18) 0.0324(9) Uani 1 1 d . . . H10 H 0.6728 1.1155 0.8074 0.039 Uiso 1 1 calc R . . C19 C 0.8770(5) 0.6301(5) 0.5205(2) 0.0511(14) Uani 1 1 d . . . H19A H 0.9548 0.5958 0.5264 0.077 Uiso 1 1 calc R . . H19B H 0.8622 0.6636 0.4863 0.077 Uiso 1 1 calc R . . H19C H 0.8513 0.5791 0.5217 0.077 Uiso 1 1 calc R . . C36 C 0.1427(4) 0.7186(5) 0.8533(2) 0.0453(12) Uani 1 1 d . . . H36A H 0.1072 0.7916 0.8626 0.068 Uiso 1 1 calc R . . H36B H 0.1470 0.6774 0.8841 0.068 Uiso 1 1 calc R . . H36C H 0.1010 0.7073 0.8267 0.068 Uiso 1 1 calc R . . C23 C 0.4968(4) 0.4932(4) 0.59821(18) 0.0348(9) Uani 1 1 d . . . O14 O 0.9498(5) 0.9287(5) 0.7559(3) 0.103(2) Uani 1 1 d . . . C43 C 0.8897(4) 0.3621(4) 0.58460(16) 0.0335(9) Uani 1 1 d . . . H43A H 0.9184 0.4094 0.5766 0.050 Uiso 1 1 calc R . . H43B H 0.8341 0.3724 0.5596 0.050 Uiso 1 1 calc R . . H43C H 0.9480 0.2911 0.5824 0.050 Uiso 1 1 calc R . . C66 C 0.4688(3) 1.0531(3) 0.86175(18) 0.0302(8) Uani 1 1 d . . . C52 C 0.3193(5) 0.7636(5) 0.9668(2) 0.0474(13) Uani 1 1 d . . . H52 H 0.3339 0.7158 0.9944 0.057 Uiso 1 1 calc R . . C60 C 1.1669(4) 0.4173(5) 0.9141(3) 0.0526(14) Uani 1 1 d . . . H60A H 1.1723 0.3537 0.9289 0.079 Uiso 1 1 calc R . . H60B H 1.1826 0.4545 0.9409 0.079 Uiso 1 1 calc R . . H60C H 1.2189 0.4006 0.8853 0.079 Uiso 1 1 calc R . . C4 C 0.3635(4) 1.1024(4) 0.5721(2) 0.0415(11) Uani 1 1 d . . . H4 H 0.3225 1.1733 0.5801 0.050 Uiso 1 1 calc R . . C55 C 0.5560(6) 0.6023(5) 0.9884(3) 0.0628(18) Uani 1 1 d . . . H55A H 0.6344 0.5592 0.9871 0.094 Uiso 1 1 calc R . . H55B H 0.5214 0.5590 0.9846 0.094 Uiso 1 1 calc R . . H55C H 0.5344 0.6380 1.0218 0.094 Uiso 1 1 calc R . . O9 O 1.3302(4) 0.7587(4) 0.56595(19) 0.0703(14) Uani 1 1 d . . . C24 C 0.4550(5) 0.4241(5) 0.5761(2) 0.0537(14) Uani 1 1 d . . . H24A H 0.4614 0.3727 0.6022 0.081 Uiso 1 1 calc R . . H24B H 0.4975 0.3893 0.5451 0.081 Uiso 1 1 calc R . . H24C H 0.3792 0.4658 0.5669 0.081 Uiso 1 1 calc R . . C70 C 0.2484(3) 1.0505(4) 0.69593(19) 0.0337(9) Uani 1 1 d . . . H70 H 0.2202 1.1179 0.7096 0.040 Uiso 1 1 calc R . . C56 C 0.7538(3) 0.6376(3) 0.87707(15) 0.0236(7) Uani 1 1 d . . . C15 C 0.9518(4) 0.8857(5) 0.5565(2) 0.0497(14) Uani 1 1 d . . . H15 H 1.0023 0.8969 0.5363 0.060 Uiso 1 1 calc R . . O11 O 0.9659(5) 1.0693(5) 0.7207(3) 0.111(3) Uani 1 1 d . . . N28 N 0.3879(3) 1.0195(3) 0.79100(14) 0.0276(7) Uani 1 1 d . . . C7 C 0.4167(4) 1.1841(4) 0.6691(2) 0.0482(13) Uani 1 1 d . . . H7A H 0.4364 1.1909 0.7045 0.072 Uiso 1 1 calc R . . H7B H 0.3397 1.2046 0.6683 0.072 Uiso 1 1 calc R . . H7C H 0.4319 1.2285 0.6456 0.072 Uiso 1 1 calc R . . C14 C 0.8995(4) 0.9485(5) 0.5981(3) 0.0513(14) Uani 1 1 d . . . H14 H 0.9155 1.0015 0.6077 0.062 Uiso 1 1 calc R . . O10 O 1.1816(5) 0.8880(6) 0.5249(3) 0.108(2) Uani 1 1 d . . . C54 C 0.5211(4) 0.6818(4) 0.94407(17) 0.0348(10) Uani 1 1 d . . . C13 C 0.8206(4) 0.9322(4) 0.6265(2) 0.0431(11) Uani 1 1 d . . . H13 H 0.7844 0.9756 0.6551 0.052 Uiso 1 1 calc R . . C22 C 0.5717(4) 0.5229(4) 0.57973(17) 0.0335(9) Uani 1 1 d . . . H22 H 0.6142 0.5009 0.5488 0.040 Uiso 1 1 calc R . . O21 O 0.3227(6) 0.4688(6) 0.7021(3) 0.117(3) Uani 1 1 d . . . O12 O 1.0356(7) 1.0024(7) 0.8035(2) 0.110(2) Uani 1 1 d . . . C37 C 0.6675(4) 0.3238(5) 0.72865(19) 0.0407(11) Uani 1 1 d . . . H37 H 0.6357 0.3452 0.7621 0.049 Uiso 1 1 calc R . . C50 C 0.1931(4) 0.9095(6) 0.9155(2) 0.0524(15) Uani 1 1 d . . . H50 H 0.1220 0.9615 0.9083 0.063 Uiso 1 1 calc R . . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 Mn5 0.0244(3) 0.0239(3) 0.0228(3) -0.0042(2) 0.0022(2) -0.0137(2) Mn3 0.0226(3) 0.0235(3) 0.0199(2) -0.0014(2) 0.00110(19) -0.0114(2) Mn2 0.0236(3) 0.0217(3) 0.0221(3) -0.0024(2) 0.0020(2) -0.0102(2) Mn1 0.0204(3) 0.0238(3) 0.0228(3) 0.0003(2) 0.00021(19) -0.0091(2) Mn4 0.0232(3) 0.0193(3) 0.0217(2) -0.0008(2) 0.00058(19) -0.0088(2) Cl3 0.0360(5) 0.0324(5) 0.0430(5) -0.0023(5) -0.0002(4) -0.0131(5) Cl4 0.0393(6) 0.0455(7) 0.0597(7) -0.0041(6) 0.0076(5) -0.0241(6) Cl1 0.0534(7) 0.0725(10) 0.0320(5) -0.0062(5) 0.0029(5) -0.0427(7) Cl2 0.0371(5) 0.0593(8) 0.0313(5) 0.0052(5) -0.0039(4) -0.0236(6) O4 0.0229(12) 0.0214(13) 0.0223(12) -0.0029(10) 0.0032(9) -0.0117(11) N17 0.0218(14) 0.0232(16) 0.0249(15) -0.0040(12) 0.0008(11) -0.0104(13) O5 0.0263(13) 0.0239(14) 0.0223(12) 0.0021(10) -0.0010(10) -0.0116(11) O3 0.0245(13) 0.0258(14) 0.0226(12) 0.0015(10) 0.0031(10) -0.0135(11) N12 0.0280(16) 0.0226(16) 0.0231(15) -0.0010(12) -0.0005(12) -0.0124(14) O6 0.0254(13) 0.0257(14) 0.0251(13) -0.0045(11) 0.0010(10) -0.0106(12) O1 0.0227(12) 0.0208(13) 0.0242(12) 0.0004(10) -0.0031(10) -0.0093(11) N26 0.0289(17) 0.0315(19) 0.0286(17) -0.0116(14) 0.0062(13) -0.0166(15) C39 0.053(3) 0.036(3) 0.040(2) -0.005(2) -0.007(2) -0.028(2) O2 0.0293(14) 0.0268(15) 0.0212(12) -0.0040(11) 0.0033(10) -0.0146(12) N19 0.0221(14) 0.0252(17) 0.0318(17) -0.0015(13) 0.0030(12) -0.0117(13) N14 0.0217(15) 0.0313(19) 0.0330(17) -0.0033(14) 0.0042(12) -0.0135(14) C46 0.0229(17) 0.034(2) 0.0263(18) 0.0010(16) 0.0025(14) -0.0132(17) N16 0.0380(19) 0.0304(19) 0.0264(16) -0.0040(14) 0.0026(14) -0.0210(16) N13 0.0285(16) 0.0258(17) 0.0232(15) -0.0021(13) 0.0019(12) -0.0152(14) N15 0.0220(15) 0.032(2) 0.0412(19) -0.0079(16) 0.0070(13) -0.0134(15) N25 0.0250(16) 0.0253(18) 0.0369(18) -0.0008(14) -0.0050(13) -0.0061(14) N27 0.0229(15) 0.0271(18) 0.0318(17) -0.0083(13) 0.0034(12) -0.0139(14) C65 0.0247(18) 0.034(2) 0.040(2) -0.0163(18) 0.0077(16) -0.0182(17) C33 0.0283(18) 0.025(2) 0.0217(16) -0.0055(14) 0.0043(13) -0.0165(16) C9 0.0231(17) 0.026(2) 0.0273(18) -0.0005(15) 0.0005(13) -0.0128(15) O8 0.172(6) 0.155(6) 0.051(3) -0.018(3) 0.011(3) -0.144(6) N18 0.0242(15) 0.0258(17) 0.0237(15) -0.0040(12) 0.0046(11) -0.0122(14) C71 0.0240(18) 0.028(2) 0.038(2) 0.0026(17) -0.0020(15) -0.0070(16) C3 0.042(3) 0.058(4) 0.044(3) 0.022(3) -0.020(2) -0.024(3) C26 0.032(2) 0.044(3) 0.044(3) -0.008(2) -0.0058(19) -0.007(2) C18 0.0236(18) 0.035(2) 0.0258(18) 0.0055(16) 0.0025(14) -0.0057(17) C38 0.054(3) 0.043(3) 0.040(2) -0.001(2) -0.002(2) -0.035(3) C47 0.0209(17) 0.035(2) 0.0310(19) 0.0069(16) -0.0011(14) -0.0129(17) N1 0.0291(16) 0.033(2) 0.0258(16) 0.0045(14) -0.0048(13) -0.0151(15) C41 0.0247(17) 0.024(2) 0.0289(19) -0.0006(15) -0.0036(14) -0.0088(15) N2 0.0215(14) 0.0258(17) 0.0306(16) 0.0023(13) -0.0038(12) -0.0104(13) N24 0.0241(15) 0.0270(18) 0.0279(16) 0.0005(13) -0.0036(12) -0.0083(14) O17 0.084(4) 0.083(4) 0.083(3) -0.023(3) 0.005(3) -0.058(3) N20 0.0255(16) 0.0249(18) 0.0387(18) 0.0043(14) -0.0025(13) -0.0147(14) N11 0.0279(17) 0.0289(19) 0.0305(17) -0.0004(14) -0.0051(13) -0.0105(15) N22 0.0396(19) 0.0324(19) 0.0230(15) -0.0044(13) 0.0035(13) -0.0236(16) N5 0.0308(17) 0.0306(19) 0.0273(16) -0.0035(14) -0.0042(13) -0.0168(15) C20 0.0236(17) 0.0228(19) 0.0216(16) -0.0023(14) -0.0004(13) -0.0052(15) C21 0.0283(18) 0.0230(19) 0.0208(17) 0.0002(14) -0.0037(14) -0.0055(16) C2 0.040(2) 0.058(3) 0.031(2) 0.009(2) -0.0103(18) -0.028(2) N21 0.0298(17) 0.037(2) 0.0309(17) -0.0116(15) 0.0075(13) -0.0205(16) C62 0.052(3) 0.061(4) 0.031(2) -0.013(2) -0.001(2) -0.036(3) C35 0.0278(19) 0.038(2) 0.035(2) -0.0125(18) 0.0090(16) -0.0219(18) O19 0.144(6) 0.056(3) 0.131(5) 0.036(3) -0.103(5) -0.035(4) O16 0.071(3) 0.085(4) 0.050(2) 0.019(2) 0.009(2) -0.039(3) N6 0.0229(15) 0.0308(19) 0.0363(18) 0.0064(15) -0.0003(13) -0.0122(15) C25 0.029(2) 0.047(3) 0.032(2) -0.001(2) 0.0009(17) -0.011(2) N9 0.0308(17) 0.0276(18) 0.0298(17) -0.0016(13) -0.0036(13) -0.0160(15) N8 0.0280(16) 0.0263(18) 0.0243(15) -0.0027(13) 0.0022(12) -0.0079(14) C58 0.039(2) 0.028(2) 0.035(2) 0.0072(17) -0.0109(17) -0.0140(19) C27 0.040(3) 0.034(3) 0.045(3) -0.001(2) -0.016(2) -0.003(2) N10 0.0377(19) 0.032(2) 0.0359(19) -0.0033(15) -0.0039(15) -0.0207(17) N23 0.0371(18) 0.0287(19) 0.0246(16) -0.0011(13) 0.0026(13) -0.0167(16) C11 0.035(2) 0.039(3) 0.033(2) -0.0091(18) 0.0012(16) -0.023(2) C63 0.043(3) 0.048(3) 0.050(3) -0.029(2) 0.004(2) -0.023(2) O13 0.043(2) 0.067(3) 0.089(3) 0.020(3) 0.018(2) -0.009(2) N29 0.0248(15) 0.0270(18) 0.0224(15) -0.0002(13) -0.0024(12) -0.0094(14) N4 0.0284(16) 0.0283(18) 0.0251(15) -0.0016(13) -0.0017(12) -0.0178(14) C68 0.0180(15) 0.0248(19) 0.0297(18) -0.0022(15) 0.0027(13) -0.0104(15) C49 0.034(2) 0.053(3) 0.039(2) -0.013(2) 0.0060(18) -0.026(2) N30 0.0257(16) 0.034(2) 0.0261(16) -0.0027(14) -0.0033(12) -0.0122(15) C57 0.034(2) 0.0199(19) 0.0249(18) -0.0005(14) -0.0076(15) -0.0107(16) C44 0.0197(15) 0.0224(18) 0.0211(16) 0.0015(13) -0.0027(12) -0.0088(14) C5 0.0257(18) 0.030(2) 0.0320(19) 0.0129(16) -0.0067(15) -0.0114(17) C40 0.048(3) 0.031(2) 0.031(2) -0.0072(17) 0.0009(18) -0.021(2) C64 0.041(2) 0.034(3) 0.055(3) -0.020(2) 0.004(2) -0.021(2) C29 0.034(2) 0.025(2) 0.0252(18) 0.0003(15) -0.0068(15) -0.0129(17) C32 0.0301(18) 0.0225(18) 0.0185(15) -0.0040(13) 0.0030(13) -0.0166(15) C69 0.0222(16) 0.0241(19) 0.0298(18) -0.0008(15) 0.0004(14) -0.0112(15) C17 0.0195(16) 0.038(2) 0.0272(18) 0.0115(16) -0.0006(14) -0.0086(16) C34 0.034(2) 0.032(2) 0.031(2) -0.0078(16) 0.0111(16) -0.0205(18) C30 0.038(2) 0.026(2) 0.0246(18) 0.0005(15) -0.0037(15) -0.0204(18) C28 0.044(3) 0.032(3) 0.040(2) 0.0051(19) -0.015(2) -0.013(2) C51 0.051(3) 0.078(4) 0.046(3) -0.024(3) 0.024(2) -0.047(3) N7 0.0238(15) 0.034(2) 0.0242(15) 0.0017(14) 0.0027(12) -0.0106(15) C6 0.0241(18) 0.025(2) 0.039(2) 0.0051(16) -0.0037(15) -0.0085(16) C8 0.0215(16) 0.0196(18) 0.0266(17) 0.0002(13) 0.0009(13) -0.0097(14) C61 0.040(2) 0.043(3) 0.028(2) -0.0122(18) -0.0007(17) -0.022(2) O7 0.157(6) 0.167(7) 0.055(3) -0.049(3) 0.052(3) -0.135(6) C12 0.059(3) 0.053(3) 0.047(3) -0.013(2) -0.006(2) -0.038(3) C16 0.0242(19) 0.053(3) 0.042(2) 0.015(2) 0.0046(17) -0.012(2) C31 0.050(3) 0.042(3) 0.031(2) 0.0123(19) -0.0058(19) -0.022(2) C45 0.0185(15) 0.0230(19) 0.0249(17) 0.0007(14) -0.0005(12) -0.0081(14) O18 0.050(2) 0.048(2) 0.0374(18) 0.0079(16) -0.0134(15) -0.0176(18) O15 0.039(2) 0.107(4) 0.056(3) 0.005(3) -0.0196(19) -0.010(2) O22 0.085(4) 0.063(3) 0.100(4) -0.024(3) 0.000(3) -0.044(3) N3 0.0276(16) 0.0259(18) 0.0336(17) -0.0019(14) -0.0053(13) -0.0119(14) C67 0.047(3) 0.027(3) 0.084(4) -0.009(3) -0.020(3) -0.015(2) C1 0.039(2) 0.040(3) 0.031(2) 0.0053(18) -0.0056(17) -0.022(2) C42 0.0279(18) 0.0221(19) 0.0240(17) -0.0021(14) -0.0008(14) -0.0091(15) C48 0.037(2) 0.045(3) 0.052(3) 0.005(2) 0.006(2) -0.027(2) C53 0.044(2) 0.038(2) 0.032(2) -0.0131(18) 0.0124(18) -0.029(2) C59 0.034(2) 0.025(2) 0.038(2) -0.0011(17) -0.0060(17) -0.0102(18) C72 0.036(2) 0.046(3) 0.047(3) 0.007(2) -0.013(2) -0.010(2) O20 0.073(3) 0.054(3) 0.075(3) -0.025(2) 0.026(2) -0.028(2) C10 0.032(2) 0.023(2) 0.040(2) -0.0044(17) -0.0022(17) -0.0113(17) C19 0.046(3) 0.055(3) 0.043(3) -0.008(2) 0.021(2) -0.018(3) C36 0.036(2) 0.057(3) 0.051(3) -0.018(2) 0.020(2) -0.030(3) C23 0.043(2) 0.028(2) 0.033(2) -0.0050(17) -0.0079(17) -0.017(2) O14 0.091(4) 0.102(5) 0.154(6) -0.070(4) 0.076(4) -0.078(4) C43 0.038(2) 0.040(3) 0.0246(19) -0.0087(17) 0.0044(16) -0.020(2) C66 0.0258(18) 0.026(2) 0.039(2) -0.0103(17) 0.0020(15) -0.0119(16) C52 0.058(3) 0.060(4) 0.043(3) -0.015(2) 0.020(2) -0.044(3) C60 0.038(3) 0.044(3) 0.063(4) 0.015(3) -0.013(2) -0.009(2) C4 0.033(2) 0.038(3) 0.048(3) 0.015(2) -0.015(2) -0.012(2) C55 0.076(4) 0.050(4) 0.057(3) 0.017(3) 0.022(3) -0.027(3) O9 0.084(3) 0.075(4) 0.062(3) 0.000(2) -0.024(2) -0.046(3) C24 0.068(4) 0.048(3) 0.057(3) -0.014(3) -0.007(3) -0.037(3) C70 0.0256(19) 0.026(2) 0.043(2) -0.0012(18) -0.0036(16) -0.0073(17) C56 0.0303(18) 0.0185(18) 0.0215(16) -0.0001(13) -0.0040(13) -0.0111(15) C15 0.032(2) 0.055(3) 0.066(3) 0.021(3) 0.000(2) -0.024(2) O11 0.077(4) 0.082(5) 0.133(6) 0.044(4) 0.014(4) -0.008(3) N28 0.0241(15) 0.0217(17) 0.0360(18) -0.0035(14) -0.0011(13) -0.0098(14) C7 0.038(2) 0.025(2) 0.067(3) 0.001(2) -0.020(2) -0.003(2) C14 0.037(3) 0.049(3) 0.076(4) 0.010(3) 0.005(2) -0.027(3) O10 0.048(3) 0.091(5) 0.177(7) 0.011(5) 0.008(4) -0.027(3) C54 0.047(3) 0.035(2) 0.033(2) -0.0074(17) 0.0142(18) -0.028(2) C13 0.034(2) 0.040(3) 0.058(3) 0.005(2) 0.002(2) -0.020(2) C22 0.038(2) 0.032(2) 0.0286(19) -0.0046(17) -0.0022(16) -0.0150(19) O21 0.092(4) 0.110(6) 0.133(6) 0.039(5) 0.041(4) -0.038(4) O12 0.136(6) 0.147(7) 0.077(4) -0.039(4) 0.006(4) -0.091(6) C37 0.052(3) 0.052(3) 0.032(2) -0.008(2) 0.0032(19) -0.036(3) C50 0.034(2) 0.075(4) 0.056(3) -0.028(3) 0.017(2) -0.032(3) _geom_special_details ; All s.u.'s (except the s.u. in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell s.u.'s are taken into account individually in the estimation of s.u.'s in distances, angles and torsion angles; correlations between s.u.'s in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell s.u.'s is used for estimating s.u.'s 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 Mn5 O5 2.159(3) . ? Mn5 O6 2.181(3) . ? Mn5 N27 2.186(4) . ? Mn5 N22 2.206(4) . ? Mn5 N21 2.306(3) . ? Mn5 N26 2.325(3) . ? Mn3 O3 2.188(3) . ? Mn3 N12 2.195(3) . ? Mn3 O4 2.197(3) . ? Mn3 N17 2.198(3) . ? Mn3 N11 2.286(4) . ? Mn3 N16 2.293(4) . ? Mn2 O2 2.167(3) . ? Mn2 O6 2.198(3) . ? Mn2 N14 2.198(3) . ? Mn2 N9 2.207(4) . ? Mn2 N29 2.215(4) . ? Mn2 O3 2.217(3) . ? Mn1 O2 2.166(3) . ? Mn1 O1 2.182(3) . ? Mn1 N2 2.187(4) . ? Mn1 N7 2.198(4) . ? Mn1 N6 2.289(4) . ? Mn1 N1 2.320(4) . ? Mn4 O5 2.174(3) . ? Mn4 O1 2.199(3) . ? Mn4 N19 2.202(3) . ? Mn4 N4 2.209(4) . ? Mn4 O4 2.209(3) . ? Mn4 N24 2.212(4) . ? Cl3 O21 1.378(6) . ? Cl3 O19 1.392(5) . ? Cl3 O20 1.419(5) . ? Cl3 O22 1.447(5) . ? Cl4 O12 1.395(6) . ? Cl4 O11 1.407(6) . ? Cl4 O14 1.419(5) . ? Cl4 O13 1.435(5) . ? Cl1 O7 1.410(5) . ? Cl1 O10 1.413(7) . ? Cl1 O8 1.424(5) . ? Cl1 O9 1.431(5) . ? Cl2 O17 1.414(5) . ? Cl2 O16 1.421(4) . ? Cl2 O15 1.429(5) . ? Cl2 O18 1.435(4) . ? O4 C44 1.303(4) . ? N17 C42 1.289(5) . ? N17 N18 1.388(4) . ? O5 C56 1.304(5) . ? O3 C32 1.305(4) . ? N12 C30 1.282(6) . ? N12 N13 1.388(5) . ? O6 C68 1.303(5) . ? O1 C8 1.303(5) . ? N26 C61 1.335(6) . ? N26 C65 1.345(6) . ? C39 C38 1.371(7) . ? C39 C40 1.391(7) . ? C39 H39 0.9300 . ? O2 C20 1.303(5) . ? N19 C45 1.331(5) . ? N19 N20 1.339(5) . ? N14 N15 1.342(5) . ? N14 C33 1.344(6) . ? C46 C47 1.353(6) . ? C46 C45 1.411(5) . ? C46 H46 0.9300 . ? N16 C37 1.334(6) . ? N16 C41 1.358(5) . ? N13 C32 1.319(5) . ? N15 C35 1.342(6) . ? N15 H15N 0.8600 . ? N25 C59 1.344(6) . ? N25 N24 1.352(5) . ? N25 H25N 0.8600 . ? N27 C66 1.286(5) . ? N27 N28 1.396(5) . ? C65 C64 1.395(6) . ? C65 C66 1.480(6) . ? C33 C34 1.394(5) . ? C33 C32 1.475(5) . ? C9 N4 1.339(6) . ? C9 C10 1.399(6) . ? C9 C8 1.470(5) . ? N18 C44 1.306(5) . ? C71 N30 1.359(6) . ? C71 C70 1.362(6) . ? C71 C72 1.497(6) . ? C3 C2 1.355(9) . ? C3 C4 1.373(8) . ? C3 H3 0.9300 . ? C26 C25 1.373(7) . ? C26 C27 1.378(8) . ? C26 H26 0.9300 . ? C18 N7 1.291(5) . ? C18 C17 1.465(7) . ? C18 C19 1.486(7) . ? C38 C37 1.387(6) . ? C38 H38 0.9300 . ? C47 N20 1.353(6) . ? C47 C48 1.497(6) . ? N1 C1 1.330(6) . ? N1 C5 1.359(6) . ? C41 C40 1.375(6) . ? C41 C42 1.470(6) . ? N2 C6 1.279(5) . ? N2 N3 1.388(5) . ? N24 C57 1.346(5) . ? N20 H20N 0.8600 . ? N11 C25 1.328(6) . ? N11 C29 1.362(6) . ? N22 C54 1.286(5) . ? N22 N23 1.394(5) . ? N5 C11 1.340(6) . ? N5 N4 1.343(4) . ? N5 H5N 0.8600 . ? C20 N8 1.323(5) . ? C20 C21 1.460(6) . ? C21 N9 1.341(5) . ? C21 C22 1.396(6) . ? C2 C1 1.396(7) . ? C2 H2 0.9300 . ? N21 C49 1.318(6) . ? N21 C53 1.361(6) . ? C62 C63 1.370(9) . ? C62 C61 1.400(6) . ? C62 H62 0.9300 . ? C35 C34 1.392(7) . ? C35 C36 1.492(6) . ? N6 C13 1.334(6) . ? N6 C17 1.349(6) . ? C25 H25 0.9300 . ? N9 N10 1.346(5) . ? N8 N7 1.384(5) . ? C58 C59 1.379(7) . ? C58 C57 1.399(6) . ? C58 H58 0.9300 . ? C27 C28 1.381(8) . ? C27 H27 0.9300 . ? N10 C23 1.361(6) . ? N10 H10N 0.8600 . ? N23 C56 1.304(5) . ? C11 C10 1.371(6) . ? C11 C12 1.484(6) . ? C63 C64 1.379(8) . ? C63 H63 0.9300 . ? N29 C69 1.338(5) . ? N29 N30 1.348(5) . ? C68 N28 1.310(5) . ? C68 C69 1.478(5) . ? C49 C50 1.402(6) . ? C49 H49 0.9300 . ? N30 H30N 0.8600 . ? C57 C56 1.481(6) . ? C44 C45 1.471(5) . ? C5 C4 1.395(6) . ? C5 C6 1.476(6) . ? C40 H40 0.9300 . ? C64 H64 0.9300 . ? C29 C28 1.393(6) . ? C29 C30 1.478(6) . ? C69 C70 1.401(6) . ? C17 C16 1.410(6) . ? C34 H34 0.9300 . ? C30 C31 1.501(6) . ? C28 H28 0.9300 . ? C51 C52 1.376(9) . ? C51 C50 1.384(9) . ? C51 H51 0.9300 . ? C6 C7 1.495(7) . ? C8 N3 1.307(5) . ? C61 H61 0.9300 . ? C12 H12A 0.9600 . ? C12 H12B 0.9600 . ? C12 H12C 0.9600 . ? C16 C15 1.390(9) . ? C16 H16 0.9300 . ? C31 H31A 0.9600 . ? C31 H31B 0.9600 . ? C31 H31C 0.9600 . ? C67 C66 1.487(7) . ? C67 H67A 0.9600 . ? C67 H67B 0.9600 . ? C67 H67C 0.9600 . ? C1 H1 0.9300 . ? C42 C43 1.503(6) . ? C48 H48A 0.9600 . ? C48 H48B 0.9600 . ? C48 H48C 0.9600 . ? C53 C52 1.390(6) . ? C53 C54 1.489(7) . ? C59 C60 1.508(7) . ? C72 H72A 0.9600 . ? C72 H72B 0.9600 . ? C72 H72C 0.9600 . ? C10 H10 0.9300 . ? C19 H19A 0.9600 . ? C19 H19B 0.9600 . ? C19 H19C 0.9600 . ? C36 H36A 0.9600 . ? C36 H36B 0.9600 . ? C36 H36C 0.9600 . ? C23 C22 1.370(7) . ? C23 C24 1.492(6) . ? C43 H43A 0.9600 . ? C43 H43B 0.9600 . ? C43 H43C 0.9600 . ? C52 H52 0.9300 . ? C60 H60A 0.9600 . ? C60 H60B 0.9600 . ? C60 H60C 0.9600 . ? C4 H4 0.9300 . ? C55 C54 1.508(7) . ? C55 H55A 0.9600 . ? C55 H55B 0.9600 . ? C55 H55C 0.9600 . ? C24 H24A 0.9600 . ? C24 H24B 0.9600 . ? C24 H24C 0.9600 . ? C70 H70 0.9300 . ? C15 C14 1.348(9) . ? C15 H15 0.9300 . ? C7 H7A 0.9600 . ? C7 H7B 0.9600 . ? C7 H7C 0.9600 . ? C14 C13 1.404(7) . ? C14 H14 0.9300 . ? C13 H13 0.9300 . ? C22 H22 0.9300 . ? C37 H37 0.9300 . ? C50 H50 0.9300 . ? 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 O5 Mn5 O6 100.55(11) . . ? O5 Mn5 N27 128.69(11) . . ? O6 Mn5 N27 71.05(12) . . ? O5 Mn5 N22 71.01(12) . . ? O6 Mn5 N22 132.95(12) . . ? N27 Mn5 N22 150.04(13) . . ? O5 Mn5 N21 139.50(13) . . ? O6 Mn5 N21 95.67(12) . . ? N27 Mn5 N21 91.65(14) . . ? N22 Mn5 N21 70.77(14) . . ? O5 Mn5 N26 92.01(12) . . ? O6 Mn5 N26 139.07(13) . . ? N27 Mn5 N26 70.74(13) . . ? N22 Mn5 N26 87.98(14) . . ? N21 Mn5 N26 99.54(12) . . ? O3 Mn3 N12 70.77(12) . . ? O3 Mn3 O4 98.34(10) . . ? N12 Mn3 O4 131.14(11) . . ? O3 Mn3 N17 127.64(11) . . ? N12 Mn3 N17 153.16(12) . . ? O4 Mn3 N17 70.41(11) . . ? O3 Mn3 N11 139.00(12) . . ? N12 Mn3 N11 71.11(13) . . ? O4 Mn3 N11 95.40(13) . . ? N17 Mn3 N11 93.35(13) . . ? O3 Mn3 N16 94.27(13) . . ? N12 Mn3 N16 89.61(13) . . ? O4 Mn3 N16 139.24(12) . . ? N17 Mn3 N16 71.21(12) . . ? N11 Mn3 N16 100.00(13) . . ? O2 Mn2 O6 99.64(11) . . ? O2 Mn2 N14 167.67(13) . . ? O6 Mn2 N14 87.58(12) . . ? O2 Mn2 N9 74.19(12) . . ? O6 Mn2 N9 173.78(12) . . ? N14 Mn2 N9 98.35(14) . . ? O2 Mn2 N29 92.18(12) . . ? O6 Mn2 N29 74.86(12) . . ? N14 Mn2 N29 99.38(14) . . ? N9 Mn2 N29 105.80(13) . . ? O2 Mn2 O3 95.49(11) . . ? O6 Mn2 O3 90.87(11) . . ? N14 Mn2 O3 74.29(12) . . ? N9 Mn2 O3 88.96(13) . . ? N29 Mn2 O3 164.78(12) . . ? O2 Mn1 O1 98.99(10) . . ? O2 Mn1 N2 127.66(12) . . ? O1 Mn1 N2 71.32(12) . . ? O2 Mn1 N7 70.96(12) . . ? O1 Mn1 N7 130.09(12) . . ? N2 Mn1 N7 152.82(13) . . ? O2 Mn1 N6 139.06(13) . . ? O1 Mn1 N6 94.58(12) . . ? N2 Mn1 N6 93.27(14) . . ? N7 Mn1 N6 70.77(14) . . ? O2 Mn1 N1 92.27(12) . . ? O1 Mn1 N1 138.94(12) . . ? N2 Mn1 N1 70.60(13) . . ? N7 Mn1 N1 90.92(13) . . ? N6 Mn1 N1 102.32(13) . . ? O5 Mn4 O1 98.64(11) . . ? O5 Mn4 N19 164.23(12) . . ? O1 Mn4 N19 89.30(12) . . ? O5 Mn4 N4 91.92(12) . . ? O1 Mn4 N4 74.41(12) . . ? N19 Mn4 N4 103.36(13) . . ? O5 Mn4 O4 91.51(10) . . ? O1 Mn4 O4 93.61(10) . . ? N19 Mn4 O4 74.33(11) . . ? N4 Mn4 O4 167.90(12) . . ? O5 Mn4 N24 74.36(12) . . ? O1 Mn4 N24 172.64(12) . . ? N19 Mn4 N24 98.04(13) . . ? N4 Mn4 N24 103.18(14) . . ? O4 Mn4 N24 88.92(12) . . ? O21 Cl3 O19 110.8(5) . . ? O21 Cl3 O20 109.0(4) . . ? O19 Cl3 O20 115.0(4) . . ? O21 Cl3 O22 107.4(5) . . ? O19 Cl3 O22 108.0(4) . . ? O20 Cl3 O22 106.3(3) . . ? O12 Cl4 O11 111.7(5) . . ? O12 Cl4 O14 109.6(4) . . ? O11 Cl4 O14 110.1(5) . . ? O12 Cl4 O13 110.2(4) . . ? O11 Cl4 O13 108.2(3) . . ? O14 Cl4 O13 106.8(3) . . ? O7 Cl1 O10 108.1(5) . . ? O7 Cl1 O8 111.0(3) . . ? O10 Cl1 O8 110.1(4) . . ? O7 Cl1 O9 111.7(4) . . ? O10 Cl1 O9 106.3(4) . . ? O8 Cl1 O9 109.5(3) . . ? O17 Cl2 O16 110.0(3) . . ? O17 Cl2 O15 110.0(4) . . ? O16 Cl2 O15 109.7(3) . . ? O17 Cl2 O18 109.4(3) . . ? O16 Cl2 O18 108.9(3) . . ? O15 Cl2 O18 108.7(3) . . ? C44 O4 Mn3 113.2(2) . . ? C44 O4 Mn4 116.1(2) . . ? Mn3 O4 Mn4 127.55(12) . . ? C42 N17 N18 119.7(3) . . ? C42 N17 Mn3 122.0(3) . . ? N18 N17 Mn3 118.2(2) . . ? C56 O5 Mn5 113.0(2) . . ? C56 O5 Mn4 117.8(2) . . ? Mn5 O5 Mn4 125.20(13) . . ? C32 O3 Mn3 113.4(3) . . ? C32 O3 Mn2 116.6(2) . . ? Mn3 O3 Mn2 127.57(12) . . ? C30 N12 N13 118.8(3) . . ? C30 N12 Mn3 122.6(3) . . ? N13 N12 Mn3 118.5(2) . . ? C68 O6 Mn5 112.7(2) . . ? C68 O6 Mn2 116.3(2) . . ? Mn5 O6 Mn2 128.77(15) . . ? C8 O1 Mn1 112.0(2) . . ? C8 O1 Mn4 116.8(2) . . ? Mn1 O1 Mn4 127.79(13) . . ? C61 N26 C65 119.1(4) . . ? C61 N26 Mn5 126.2(3) . . ? C65 N26 Mn5 114.7(3) . . ? C38 C39 C40 119.4(4) . . ? C38 C39 H39 120.3 . . ? C40 C39 H39 120.3 . . ? C20 O2 Mn1 113.7(2) . . ? C20 O2 Mn2 117.7(2) . . ? Mn1 O2 Mn2 125.54(13) . . ? C45 N19 N20 106.0(3) . . ? C45 N19 Mn4 115.6(3) . . ? N20 N19 Mn4 138.4(3) . . ? N15 N14 C33 105.4(3) . . ? N15 N14 Mn2 138.7(3) . . ? C33 N14 Mn2 115.6(3) . . ? C47 C46 C45 105.5(4) . . ? C47 C46 H46 127.3 . . ? C45 C46 H46 127.3 . . ? C37 N16 C41 118.5(4) . . ? C37 N16 Mn3 126.1(3) . . ? C41 N16 Mn3 115.4(3) . . ? C32 N13 N12 108.9(3) . . ? N14 N15 C35 112.4(4) . . ? N14 N15 H15N 123.8 . . ? C35 N15 H15N 123.8 . . ? C59 N25 N24 112.9(4) . . ? C59 N25 H25N 123.6 . . ? N24 N25 H25N 123.6 . . ? C66 N27 N28 118.3(4) . . ? C66 N27 Mn5 123.5(3) . . ? N28 N27 Mn5 118.3(2) . . ? N26 C65 C64 121.0(4) . . ? N26 C65 C66 116.7(4) . . ? C64 C65 C66 122.2(5) . . ? N14 C33 C34 110.5(4) . . ? N14 C33 C32 116.8(3) . . ? C34 C33 C32 132.7(4) . . ? N4 C9 C10 110.6(4) . . ? N4 C9 C8 117.1(4) . . ? C10 C9 C8 132.3(4) . . ? C44 N18 N17 109.5(3) . . ? N30 C71 C70 106.4(4) . . ? N30 C71 C72 122.6(4) . . ? C70 C71 C72 131.0(5) . . ? C2 C3 C4 120.1(5) . . ? C2 C3 H3 120.0 . . ? C4 C3 H3 120.0 . . ? C25 C26 C27 118.8(5) . . ? C25 C26 H26 120.6 . . ? C27 C26 H26 120.6 . . ? N7 C18 C17 114.1(4) . . ? N7 C18 C19 123.9(5) . . ? C17 C18 C19 122.0(4) . . ? C39 C38 C37 117.9(4) . . ? C39 C38 H38 121.0 . . ? C37 C38 H38 121.0 . . ? N20 C47 C46 107.3(3) . . ? N20 C47 C48 121.1(4) . . ? C46 C47 C48 131.6(4) . . ? C1 N1 C5 118.1(4) . . ? C1 N1 Mn1 126.9(3) . . ? C5 N1 Mn1 115.0(3) . . ? N16 C41 C40 121.1(4) . . ? N16 C41 C42 116.1(4) . . ? C40 C41 C42 122.8(4) . . ? C6 N2 N3 118.8(4) . . ? C6 N2 Mn1 123.7(3) . . ? N3 N2 Mn1 117.5(3) . . ? C57 N24 N25 104.1(3) . . ? C57 N24 Mn4 115.3(3) . . ? N25 N24 Mn4 140.4(3) . . ? N19 N20 C47 111.4(4) . . ? N19 N20 H20N 124.3 . . ? C47 N20 H20N 124.3 . . ? C25 N11 C29 118.1(4) . . ? C25 N11 Mn3 126.2(3) . . ? C29 N11 Mn3 115.5(3) . . ? C54 N22 N23 118.8(4) . . ? C54 N22 Mn5 122.9(3) . . ? N23 N22 Mn5 117.4(2) . . ? C11 N5 N4 112.4(4) . . ? C11 N5 H5N 123.8 . . ? N4 N5 H5N 123.8 . . ? O2 C20 N8 125.0(4) . . ? O2 C20 C21 116.7(3) . . ? N8 C20 C21 118.2(4) . . ? N9 C21 C22 110.8(4) . . ? N9 C21 C20 116.2(3) . . ? C22 C21 C20 133.0(4) . . ? C3 C2 C1 118.6(5) . . ? C3 C2 H2 120.7 . . ? C1 C2 H2 120.7 . . ? C49 N21 C53 118.5(4) . . ? C49 N21 Mn5 126.1(3) . . ? C53 N21 Mn5 115.3(3) . . ? C63 C62 C61 117.9(5) . . ? C63 C62 H62 121.1 . . ? C61 C62 H62 121.1 . . ? N15 C35 C34 106.4(3) . . ? N15 C35 C36 120.6(5) . . ? C34 C35 C36 132.9(5) . . ? C13 N6 C17 119.0(4) . . ? C13 N6 Mn1 125.2(3) . . ? C17 N6 Mn1 115.5(3) . . ? N11 C25 C26 123.4(5) . . ? N11 C25 H25 118.3 . . ? C26 C25 H25 118.3 . . ? C21 N9 N10 105.6(3) . . ? C21 N9 Mn2 115.1(3) . . ? N10 N9 Mn2 139.1(3) . . ? C20 N8 N7 108.9(3) . . ? C59 C58 C57 105.0(4) . . ? C59 C58 H58 127.5 . . ? C57 C58 H58 127.5 . . ? C26 C27 C28 119.4(5) . . ? C26 C27 H27 120.3 . . ? C28 C27 H27 120.3 . . ? N9 N10 C23 111.1(4) . . ? N9 N10 H10N 124.4 . . ? C23 N10 H10N 124.4 . . ? C56 N23 N22 108.3(3) . . ? N5 C11 C10 106.9(4) . . ? N5 C11 C12 121.5(5) . . ? C10 C11 C12 131.5(5) . . ? C62 C63 C64 119.9(4) . . ? C62 C63 H63 120.0 . . ? C64 C63 H63 120.0 . . ? C69 N29 N30 104.8(3) . . ? C69 N29 Mn2 114.5(3) . . ? N30 N29 Mn2 140.3(3) . . ? C9 N4 N5 104.9(3) . . ? C9 N4 Mn4 114.9(3) . . ? N5 N4 Mn4 140.0(3) . . ? O6 C68 N28 126.5(4) . . ? O6 C68 C69 117.3(3) . . ? N28 C68 C69 116.2(4) . . ? N21 C49 C50 123.1(5) . . ? N21 C49 H49 118.4 . . ? C50 C49 H49 118.4 . . ? N29 N30 C71 112.2(4) . . ? N29 N30 H30N 123.9 . . ? C71 N30 H30N 123.9 . . ? N24 C57 C58 111.3(4) . . ? N24 C57 C56 115.8(3) . . ? C58 C57 C56 132.8(4) . . ? O4 C44 N18 125.3(3) . . ? O4 C44 C45 117.2(3) . . ? N18 C44 C45 117.5(3) . . ? N1 C5 C4 121.3(4) . . ? N1 C5 C6 115.9(4) . . ? C4 C5 C6 122.7(4) . . ? C41 C40 C39 119.7(4) . . ? C41 C40 H40 120.2 . . ? C39 C40 H40 120.2 . . ? C63 C64 C65 119.3(5) . . ? C63 C64 H64 120.3 . . ? C65 C64 H64 120.3 . . ? N11 C29 C28 121.6(4) . . ? N11 C29 C30 115.7(4) . . ? C28 C29 C30 122.7(4) . . ? O3 C32 N13 125.4(4) . . ? O3 C32 C33 116.6(3) . . ? N13 C32 C33 118.0(3) . . ? N29 C69 C70 110.7(4) . . ? N29 C69 C68 116.9(4) . . ? C70 C69 C68 132.3(4) . . ? N6 C17 C16 120.7(5) . . ? N6 C17 C18 116.6(3) . . ? C16 C17 C18 122.6(4) . . ? C35 C34 C33 105.2(4) . . ? C35 C34 H34 127.4 . . ? C33 C34 H34 127.4 . . ? N12 C30 C29 114.6(4) . . ? N12 C30 C31 124.2(4) . . ? C29 C30 C31 121.1(4) . . ? C27 C28 C29 118.7(5) . . ? C27 C28 H28 120.6 . . ? C29 C28 H28 120.6 . . ? C52 C51 C50 119.9(4) . . ? C52 C51 H51 120.1 . . ? C50 C51 H51 120.1 . . ? C18 N7 N8 119.4(4) . . ? C18 N7 Mn1 122.6(3) . . ? N8 N7 Mn1 117.8(2) . . ? N2 C6 C5 114.8(4) . . ? N2 C6 C7 124.9(4) . . ? C5 C6 C7 120.3(4) . . ? O1 C8 N3 126.4(4) . . ? O1 C8 C9 116.7(3) . . ? N3 C8 C9 116.9(3) . . ? N26 C61 C62 122.8(5) . . ? N26 C61 H61 118.6 . . ? C62 C61 H61 118.6 . . ? C11 C12 H12A 109.5 . . ? C11 C12 H12B 109.5 . . ? H12A C12 H12B 109.5 . . ? C11 C12 H12C 109.5 . . ? H12A C12 H12C 109.5 . . ? H12B C12 H12C 109.5 . . ? C15 C16 C17 118.9(5) . . ? C15 C16 H16 120.6 . . ? C17 C16 H16 120.6 . . ? C30 C31 H31A 109.5 . . ? C30 C31 H31B 109.5 . . ? H31A C31 H31B 109.5 . . ? C30 C31 H31C 109.5 . . ? H31A C31 H31C 109.5 . . ? H31B C31 H31C 109.5 . . ? N19 C45 C46 109.8(3) . . ? N19 C45 C44 116.7(3) . . ? C46 C45 C44 133.5(4) . . ? C8 N3 N2 109.0(3) . . ? C66 C67 H67A 109.5 . . ? C66 C67 H67B 109.5 . . ? H67A C67 H67B 109.5 . . ? C66 C67 H67C 109.5 . . ? H67A C67 H67C 109.5 . . ? H67B C67 H67C 109.5 . . ? N1 C1 C2 123.0(5) . . ? N1 C1 H1 118.5 . . ? C2 C1 H1 118.5 . . ? N17 C42 C41 115.1(4) . . ? N17 C42 C43 123.2(4) . . ? C41 C42 C43 121.7(4) . . ? C47 C48 H48A 109.5 . . ? C47 C48 H48B 109.5 . . ? H48A C48 H48B 109.5 . . ? C47 C48 H48C 109.5 . . ? H48A C48 H48C 109.5 . . ? H48B C48 H48C 109.5 . . ? N21 C53 C52 122.0(5) . . ? N21 C53 C54 116.3(4) . . ? C52 C53 C54 121.7(5) . . ? N25 C59 C58 106.6(4) . . ? N25 C59 C60 120.7(4) . . ? C58 C59 C60 132.7(5) . . ? C71 C72 H72A 109.5 . . ? C71 C72 H72B 109.5 . . ? H72A C72 H72B 109.5 . . ? C71 C72 H72C 109.5 . . ? H72A C72 H72C 109.5 . . ? H72B C72 H72C 109.5 . . ? C11 C10 C9 105.1(4) . . ? C11 C10 H10 127.4 . . ? C9 C10 H10 127.4 . . ? C18 C19 H19A 109.5 . . ? C18 C19 H19B 109.5 . . ? H19A C19 H19B 109.5 . . ? C18 C19 H19C 109.5 . . ? H19A C19 H19C 109.5 . . ? H19B C19 H19C 109.5 . . ? C35 C36 H36A 109.5 . . ? C35 C36 H36B 109.5 . . ? H36A C36 H36B 109.5 . . ? C35 C36 H36C 109.5 . . ? H36A C36 H36C 109.5 . . ? H36B C36 H36C 109.5 . . ? N10 C23 C22 107.2(4) . . ? N10 C23 C24 120.0(5) . . ? C22 C23 C24 132.7(5) . . ? C42 C43 H43A 109.5 . . ? C42 C43 H43B 109.5 . . ? H43A C43 H43B 109.5 . . ? C42 C43 H43C 109.5 . . ? H43A C43 H43C 109.5 . . ? H43B C43 H43C 109.5 . . ? N27 C66 C65 114.2(4) . . ? N27 C66 C67 123.7(4) . . ? C65 C66 C67 122.1(4) . . ? C51 C52 C53 118.7(5) . . ? C51 C52 H52 120.6 . . ? C53 C52 H52 120.6 . . ? C59 C60 H60A 109.5 . . ? C59 C60 H60B 109.5 . . ? H60A C60 H60B 109.5 . . ? C59 C60 H60C 109.5 . . ? H60A C60 H60C 109.5 . . ? H60B C60 H60C 109.5 . . ? C3 C4 C5 119.0(5) . . ? C3 C4 H4 120.5 . . ? C5 C4 H4 120.5 . . ? C54 C55 H55A 109.5 . . ? C54 C55 H55B 109.5 . . ? H55A C55 H55B 109.5 . . ? C54 C55 H55C 109.5 . . ? H55A C55 H55C 109.5 . . ? H55B C55 H55C 109.5 . . ? C23 C24 H24A 109.5 . . ? C23 C24 H24B 109.5 . . ? H24A C24 H24B 109.5 . . ? C23 C24 H24C 109.5 . . ? H24A C24 H24C 109.5 . . ? H24B C24 H24C 109.5 . . ? C71 C70 C69 105.8(4) . . ? C71 C70 H70 127.1 . . ? C69 C70 H70 127.1 . . ? O5 C56 N23 126.6(4) . . ? O5 C56 C57 116.6(3) . . ? N23 C56 C57 116.8(4) . . ? C14 C15 C16 120.0(5) . . ? C14 C15 H15 120.0 . . ? C16 C15 H15 120.0 . . ? C68 N28 N27 108.2(3) . . ? C6 C7 H7A 109.5 . . ? C6 C7 H7B 109.5 . . ? H7A C7 H7B 109.5 . . ? C6 C7 H7C 109.5 . . ? H7A C7 H7C 109.5 . . ? H7B C7 H7C 109.5 . . ? C15 C14 C13 118.6(5) . . ? C15 C14 H14 120.7 . . ? C13 C14 H14 120.7 . . ? N22 C54 C53 113.9(4) . . ? N22 C54 C55 123.3(5) . . ? C53 C54 C55 122.8(4) . . ? N6 C13 C14 122.7(5) . . ? N6 C13 H13 118.6 . . ? C14 C13 H13 118.6 . . ? C23 C22 C21 105.2(4) . . ? C23 C22 H22 127.4 . . ? C21 C22 H22 127.4 . . ? N16 C37 C38 123.4(4) . . ? N16 C37 H37 118.3 . . ? C38 C37 H37 118.3 . . ? C51 C50 C49 117.8(6) . . ? C51 C50 H50 121.1 . . ? C49 C50 H50 121.1 . . ? _diffrn_measured_fraction_theta_max 0.982 _diffrn_reflns_theta_full 30.75 _diffrn_measured_fraction_theta_full 0.982 _refine_diff_density_max 0.795 _refine_diff_density_min -0.957 _refine_diff_density_rms 0.093 # Details about the Squeezed Material loop_ _platon_squeeze_void_nr _platon_squeeze_void_average_x _platon_squeeze_void_average_y _platon_squeeze_void_average_z _platon_squeeze_void_volume _platon_squeeze_void_count_electrons _platon_squeeze_void_content 1 0.204 0.336 0.604 46 15 ' ' 2 0.165 0.558 0.537 7 1 ' ' 3 0.483 0.672 0.125 30 12 ' ' 4 0.517 0.328 0.875 30 12 ' ' 5 0.796 0.664 0.396 46 15 ' ' 6 0.834 0.442 0.463 7 1 ' ' _platon_squeeze_details ; SQUEEZE was used to remove the contributions of a water solvent molecule. ; # Attachment 'Rev. complex2.cif' data_sksr39m _database_code_depnum_ccdc_archive 'CCDC 796251' #TrackingRef 'Rev. complex2.cif' _alert_response ; Alert C CHEMW03, DENSD01, PLat 041, 043, 046, 068, Calculated and Reported Values for formula, denisty, molecular mass and F000 value. Response Four water molecule was present as the solvent molecule which was removed using SQUEEZE. Thus eight hydrogen atoms and four oxygen atoms of water molecules were added to the chemical formula to adjust the density, molecular mass and F000 value. Results in the chemical_formula_moiety C72 H72 Mn5 N30 O6, 4(Cl O4), 4(H2 O). ; _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety 'C66 H66 Mn5 N36 O6, 4(Cl O4), 4(H2 O)' _chemical_formula_sum 'C66 H74 Cl4 Mn5 N36 O26' _chemical_formula_weight 2204.14 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' Mn Mn 0.3368 0.7283 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting Monoclinic _symmetry_space_group_name_H-M 'C 2/c' _symmetry_space_group_name_Hall '-C 2yc' loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, y, -z+1/2' 'x+1/2, y+1/2, z' '-x+1/2, y+1/2, -z+1/2' '-x, -y, -z' 'x, -y, z-1/2' '-x+1/2, -y+1/2, -z' 'x+1/2, -y+1/2, z-1/2' _cell_length_a 34.1672(11) _cell_length_b 19.6474(7) _cell_length_c 29.3633(9) _cell_angle_alpha 90.00 _cell_angle_beta 111.754(2) _cell_angle_gamma 90.00 _cell_volume 18307.7(10) _cell_formula_units_Z 8 _cell_measurement_temperature 150(2) _cell_measurement_reflns_used 171710 _cell_measurement_theta_min 1.3 _cell_measurement_theta_max 26.4 _exptl_crystal_description Rectangular _exptl_crystal_colour White _exptl_crystal_size_max 0.14 _exptl_crystal_size_mid 0.12 _exptl_crystal_size_min 0.11 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.556 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 8760 _exptl_absorpt_coefficient_mu 0.875 _exptl_absorpt_correction_type Empirical _exptl_absorpt_correction_T_min 0.8872 _exptl_absorpt_correction_T_max 0.9098 _exptl_absorpt_process_details SADABS _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 171710 _diffrn_reflns_av_R_equivalents 0.0799 _diffrn_reflns_av_sigmaI/netI 0.0566 _diffrn_reflns_limit_h_min -42 _diffrn_reflns_limit_h_max 42 _diffrn_reflns_limit_k_min -24 _diffrn_reflns_limit_k_max 24 _diffrn_reflns_limit_l_min -36 _diffrn_reflns_limit_l_max 36 _diffrn_reflns_theta_min 1.28 _diffrn_reflns_theta_max 26.37 _reflns_number_total 18403 _reflns_number_gt 11889 _reflns_threshold_expression >2\s(I) _computing_data_collection 'Bruker SMART' _computing_cell_refinement 'Bruker SMART' _computing_data_reduction 'Bruker SAINT' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'Ortep-3 for Windows (Farrugia, 1997)' _computing_publication_material 'WINGX V1.80.05' _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^ > 2\s(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^)+(0.1203P)^2^+43.9263P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment constr _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 18403 _refine_ls_number_parameters 1204 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.1062 _refine_ls_R_factor_gt 0.0718 _refine_ls_wR_factor_ref 0.2153 _refine_ls_wR_factor_gt 0.1981 _refine_ls_goodness_of_fit_ref 1.060 _refine_ls_restrained_S_all 1.060 _refine_ls_shift/su_max 0.003 _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 0.30692(2) 0.34574(4) 0.31134(3) 0.0321(2) Uani 1 1 d . . . Mn2 Mn 0.39172(2) 0.24429(4) 0.42215(3) 0.02888(19) Uani 1 1 d . . . Mn4 Mn 0.32927(2) 0.23364(4) 0.21337(3) 0.02786(18) Uani 1 1 d . . . Mn5 Mn 0.43846(2) 0.27737(4) 0.31989(3) 0.02890(19) Uani 1 1 d . . . Mn3 Mn 0.33372(2) 0.10697(4) 0.32029(3) 0.0327(2) Uani 1 1 d . . . Cl1 Cl 0.29600(5) 0.17632(9) 0.01289(6) 0.0566(4) Uani 1 1 d . . . Cl3 Cl 0.15125(8) -0.14547(12) -0.08890(9) 0.0848(7) Uani 1 1 d . . . Cl4 Cl -0.04580(7) -0.15575(11) -0.09229(8) 0.0806(6) Uani 1 1 d . . . O2 O 0.38881(10) 0.15453(18) 0.37690(12) 0.0319(8) Uani 1 1 d . . . O5 O 0.41399(10) 0.30789(17) 0.37657(11) 0.0303(8) Uani 1 1 d . . . Cl2 Cl 0.05036(9) -0.42534(17) -0.08974(13) 0.1161(10) Uani 1 1 d . . . O6 O 0.33274(10) 0.32531(17) 0.25425(12) 0.0299(7) Uani 1 1 d . . . O4 O 0.39342(10) 0.21179(17) 0.26347(11) 0.0300(7) Uani 1 1 d . . . O1 O 0.32847(10) 0.27047(17) 0.37172(12) 0.0316(8) Uani 1 1 d . . . O3 O 0.30359(10) 0.17730(18) 0.25874(12) 0.0322(8) Uani 1 1 d . . . N23 N 0.35082(14) 0.1506(2) 0.17857(15) 0.0355(10) Uani 1 1 d . . . N17 N 0.26153(14) 0.2216(2) 0.16663(15) 0.0384(11) Uani 1 1 d . . . N18 N 0.23290(14) 0.2379(2) 0.12284(16) 0.0416(11) Uani 1 1 d . . . H18N H 0.2389 0.2566 0.0998 0.050 Uiso 1 1 calc R . . N35 N 0.33365(14) 0.3155(2) 0.16328(15) 0.0335(10) Uani 1 1 d . . . N27 N 0.44334(13) 0.3858(2) 0.32827(14) 0.0324(10) Uani 1 1 d . . . N25 N 0.44691(14) 0.3309(2) 0.24969(15) 0.0359(10) Uani 1 1 d . . . N13 N 0.31963(16) 0.0629(2) 0.38919(16) 0.0438(12) Uani 1 1 d . . . N7 N 0.31941(17) 0.0217(2) 0.25382(17) 0.0462(12) Uani 1 1 d . . . N4 N 0.25768(14) 0.2671(2) 0.36218(17) 0.0374(10) Uani 1 1 d . . . N33 N 0.33462(14) 0.4379(2) 0.29700(14) 0.0342(10) Uani 1 1 d . . . N28 N 0.44275(14) 0.4135(2) 0.37225(14) 0.0334(10) Uani 1 1 d . . . N15 N 0.26783(14) 0.1126(2) 0.30739(16) 0.0393(11) Uani 1 1 d . . . N11 N 0.45111(13) 0.1869(2) 0.46114(14) 0.0356(10) Uani 1 1 d . . . N6 N 0.35041(16) 0.1853(3) 0.50287(17) 0.0455(12) Uani 1 1 d . . . H6N H 0.3731 0.1724 0.5261 0.055 Uiso 1 1 calc R . . N19 N 0.50388(13) 0.2608(3) 0.39282(16) 0.0392(11) Uani 1 1 d . . . N3 N 0.25242(13) 0.3010(2) 0.31844(15) 0.0369(10) Uani 1 1 d . . . N1 N 0.24074(15) 0.3669(3) 0.23747(17) 0.0439(12) Uani 1 1 d . . . N9 N 0.38770(14) 0.0456(2) 0.32924(15) 0.0369(10) Uani 1 1 d . . . N26 N 0.45764(16) 0.4956(2) 0.30811(18) 0.0477(12) Uani 1 1 d . . . H26A H 0.4578 0.5121 0.3353 0.057 Uiso 1 1 calc R . . H26B H 0.4621 0.5217 0.2870 0.057 Uiso 1 1 calc R . . N24 N 0.33717(15) 0.1124(2) 0.13788(16) 0.0411(11) Uani 1 1 d . . . H24N H 0.3136 0.1191 0.1140 0.049 Uiso 1 1 calc R . . N5 N 0.34972(14) 0.2119(2) 0.46042(15) 0.0355(10) Uani 1 1 d . . . N31 N 0.32294(14) 0.4258(2) 0.37924(15) 0.0381(11) Uani 1 1 d . . . O10 O 0.26909(16) 0.1766(3) -0.03648(17) 0.0721(14) Uani 1 1 d . . . N10 N 0.42360(14) 0.0559(2) 0.37249(15) 0.0380(10) Uani 1 1 d . . . N21 N 0.46908(13) 0.1820(2) 0.31668(16) 0.0352(10) Uani 1 1 d . . . N34 N 0.34210(13) 0.4423(2) 0.25318(14) 0.0322(10) Uani 1 1 d . . . N2 N 0.18243(15) 0.2694(3) 0.2952(2) 0.0590(15) Uani 1 1 d . . . H2A H 0.1871 0.2490 0.3226 0.071 Uiso 1 1 calc R . . H2B H 0.1574 0.2700 0.2731 0.071 Uiso 1 1 calc R . . N30 N 0.41628(15) 0.3714(3) 0.50744(16) 0.0416(11) Uani 1 1 d . . . H30N H 0.4090 0.3526 0.5295 0.050 Uiso 1 1 calc R . . N32 N 0.36510(16) 0.5451(2) 0.31603(19) 0.0491(13) Uani 1 1 d . . . H32A H 0.3692 0.5476 0.2889 0.059 Uiso 1 1 calc R . . H32B H 0.3727 0.5781 0.3367 0.059 Uiso 1 1 calc R . . N36 N 0.33076(14) 0.3268(2) 0.11716(15) 0.0353(10) Uani 1 1 d . . . H36N H 0.3278 0.2949 0.0961 0.042 Uiso 1 1 calc R . . N22 N 0.44921(13) 0.1379(2) 0.27742(16) 0.0369(10) Uani 1 1 d . . . N12 N 0.48721(15) 0.1910(3) 0.50155(17) 0.0473(12) Uani 1 1 d . . . H12N H 0.4938 0.2245 0.5219 0.057 Uiso 1 1 calc R . . N16 N 0.24084(14) 0.1394(2) 0.26339(16) 0.0386(11) Uani 1 1 d . . . N29 N 0.41294(15) 0.3411(2) 0.46490(15) 0.0375(10) Uani 1 1 d . . . N14 N 0.20824(16) 0.0955(3) 0.3275(2) 0.0543(14) Uani 1 1 d . . . H14A H 0.1916 0.1115 0.2999 0.065 Uiso 1 1 calc R . . H14B H 0.1982 0.0815 0.3488 0.065 Uiso 1 1 calc R . . O9 O 0.33278(17) 0.1373(3) 0.0200(2) 0.0868(17) Uani 1 1 d . . . C19 C 0.45474(15) 0.1296(3) 0.43975(19) 0.0344(12) Uani 1 1 d . . . C63 C 0.33814(16) 0.3773(3) 0.18375(18) 0.0316(11) Uani 1 1 d . . . C49 C 0.44856(15) 0.3995(3) 0.25205(18) 0.0325(11) Uani 1 1 d . . . O8 O 0.27444(17) 0.1466(4) 0.0413(2) 0.102(2) Uani 1 1 d . . . C50 C 0.45039(16) 0.4291(3) 0.29858(19) 0.0330(11) Uani 1 1 d . . . C56 C 0.3157(2) 0.4181(3) 0.4205(2) 0.0519(16) Uani 1 1 d . . . H56 H 0.3068 0.3758 0.4270 0.062 Uiso 1 1 calc R . . C45 C 0.44270(17) 0.3010(3) 0.2075(2) 0.0417(13) Uani 1 1 d . . . H45 H 0.4415 0.2537 0.2058 0.050 Uiso 1 1 calc R . . C48 C 0.44672(18) 0.4393(3) 0.2122(2) 0.0436(14) Uani 1 1 d . . . H48 H 0.4481 0.4865 0.2145 0.052 Uiso 1 1 calc R . . C52 C 0.42716(17) 0.3873(3) 0.44214(18) 0.0348(12) Uani 1 1 d . . . C5 C 0.20632(18) 0.3360(3) 0.2399(2) 0.0415(13) Uani 1 1 d . . . C38 C 0.52489(17) 0.2034(3) 0.3906(2) 0.0431(14) Uani 1 1 d . . . C6 C 0.21386(17) 0.2998(3) 0.2869(2) 0.0391(13) Uani 1 1 d . . . N8 N 0.42546(19) -0.0429(3) 0.3122(2) 0.0613(15) Uani 1 1 d . . . H8A H 0.4473 -0.0353 0.3382 0.074 Uiso 1 1 calc R . . H8B H 0.4257 -0.0754 0.2927 0.074 Uiso 1 1 calc R . . N20 N 0.51592(16) 0.0929(3) 0.3526(2) 0.0636(16) Uani 1 1 d . . . H20A H 0.5034 0.0651 0.3290 0.076 Uiso 1 1 calc R . . H20B H 0.5377 0.0798 0.3770 0.076 Uiso 1 1 calc R . . C18 C 0.42041(16) 0.1125(3) 0.39254(18) 0.0312(11) Uani 1 1 d . . . C61 C 0.34712(17) 0.4904(3) 0.32596(19) 0.0389(13) Uani 1 1 d . . . C60 C 0.3381(2) 0.4855(3) 0.37115(18) 0.0410(14) Uani 1 1 d . . . C62 C 0.33873(15) 0.3819(3) 0.23438(17) 0.0310(11) Uani 1 1 d . . . C9 C 0.28413(19) 0.2050(3) 0.4615(2) 0.0470(15) Uani 1 1 d . . . H9 H 0.2550 0.2083 0.4518 0.056 Uiso 1 1 calc R . . C28 C 0.25006(18) 0.0924(3) 0.3376(2) 0.0411(13) Uani 1 1 d . . . O7 O 0.30978(19) 0.2442(3) 0.0287(2) 0.0831(17) Uani 1 1 d . . . C30 C 0.23951(16) 0.1949(3) 0.19157(18) 0.0342(12) Uani 1 1 d . . . C20 C 0.49213(18) 0.0959(3) 0.4663(2) 0.0473(15) Uani 1 1 d . . . H20 H 0.5016 0.0549 0.4583 0.057 Uiso 1 1 calc R . . C47 C 0.44280(19) 0.4064(4) 0.1686(2) 0.0488(15) Uani 1 1 d . . . H47 H 0.4421 0.4316 0.1416 0.059 Uiso 1 1 calc R . . C42 C 0.39793(19) 0.0688(3) 0.1820(2) 0.0421(13) Uani 1 1 d . . . H42 H 0.4219 0.0417 0.1935 0.051 Uiso 1 1 calc R . . C41 C 0.38833(17) 0.1247(3) 0.20552(19) 0.0339(11) Uani 1 1 d . . . C7 C 0.29717(16) 0.2556(3) 0.38636(18) 0.0328(11) Uani 1 1 d . . . C23 C 0.3481(2) 0.0357(4) 0.4297(2) 0.0549(17) Uani 1 1 d . . . H23 H 0.3764 0.0377 0.4339 0.066 Uiso 1 1 calc R . . C12 C 0.2845(2) 0.0152(3) 0.2140(2) 0.0557(17) Uani 1 1 d . . . H12 H 0.2606 0.0393 0.2122 0.067 Uiso 1 1 calc R . . C17 C 0.3911(2) -0.0044(3) 0.3021(2) 0.0475(15) Uani 1 1 d . . . C53 C 0.4396(2) 0.4457(3) 0.4698(2) 0.0461(14) Uani 1 1 d . . . H53 H 0.4508 0.4849 0.4615 0.055 Uiso 1 1 calc R . . C39 C 0.50160(17) 0.1558(3) 0.3513(2) 0.0437(14) Uani 1 1 d . . . C37 C 0.5659(2) 0.1906(4) 0.4225(2) 0.0630(19) Uani 1 1 d . . . H37 H 0.5797 0.1508 0.4201 0.076 Uiso 1 1 calc R . . C8 C 0.30887(16) 0.2237(3) 0.43434(19) 0.0343(11) Uani 1 1 d . . . C64 C 0.33790(17) 0.4275(3) 0.14998(18) 0.0361(12) Uani 1 1 d . . . H64 H 0.3405 0.4742 0.1552 0.043 Uiso 1 1 calc R . . C32 C 0.19377(17) 0.2218(3) 0.1190(2) 0.0457(14) Uani 1 1 d . . . C4 C 0.16744(19) 0.3379(3) 0.2023(2) 0.0534(16) Uani 1 1 d . . . H4 H 0.1441 0.3175 0.2057 0.064 Uiso 1 1 calc R . . C27 C 0.27950(19) 0.0605(3) 0.3834(2) 0.0433(14) Uani 1 1 d . . . O16 O 0.1165(3) -0.1697(4) -0.0821(3) 0.121(3) Uani 1 1 d . . . O17 O 0.1638(3) -0.1964(4) -0.1153(3) 0.138(3) Uani 1 1 d . . . C46 C 0.43995(19) 0.3374(4) 0.1656(2) 0.0513(16) Uani 1 1 d . . . H46 H 0.4363 0.3150 0.1364 0.062 Uiso 1 1 calc R . . C10 C 0.3120(2) 0.1809(3) 0.5053(2) 0.0495(15) Uani 1 1 d . . . C65 C 0.33300(18) 0.3930(3) 0.10721(19) 0.0395(13) Uani 1 1 d . . . C16 C 0.3533(2) -0.0146(3) 0.2568(2) 0.0497(16) Uani 1 1 d . . . C51 C 0.42756(16) 0.3689(3) 0.39314(18) 0.0319(11) Uani 1 1 d . . . C26 C 0.2652(2) 0.0313(3) 0.4172(2) 0.0534(16) Uani 1 1 d . . . H26 H 0.2367 0.0307 0.4122 0.064 Uiso 1 1 calc R . . C54 C 0.4323(2) 0.4343(3) 0.5112(2) 0.0514(16) Uani 1 1 d . . . C2 C 0.1985(2) 0.4010(4) 0.1552(2) 0.0543(17) Uani 1 1 d . . . H2 H 0.1967 0.4224 0.1262 0.065 Uiso 1 1 calc R . . C34 C 0.52312(18) 0.3059(4) 0.4285(2) 0.0474(15) Uani 1 1 d . . . H34 H 0.5086 0.3449 0.4310 0.057 Uiso 1 1 calc R . . C31 C 0.19652(17) 0.1941(3) 0.1622(2) 0.0450(14) Uani 1 1 d . . . H31 H 0.1745 0.1780 0.1707 0.054 Uiso 1 1 calc R . . C24 C 0.3371(3) 0.0051(4) 0.4654(2) 0.068(2) Uani 1 1 d . . . H24 H 0.3574 -0.0138 0.4932 0.082 Uiso 1 1 calc R . . C29 C 0.26271(15) 0.1694(3) 0.24158(17) 0.0311(11) Uani 1 1 d . . . C33 C 0.1567(2) 0.2351(4) 0.0715(3) 0.070(2) Uani 1 1 d . . . H33A H 0.1494 0.2825 0.0695 0.105 Uiso 1 1 calc R . . H33B H 0.1330 0.2083 0.0709 0.105 Uiso 1 1 calc R . . H33C H 0.1642 0.2229 0.0442 0.105 Uiso 1 1 calc R . . C66 C 0.3306(2) 0.4174(4) 0.0584(2) 0.0586(18) Uani 1 1 d . . . H66A H 0.3556 0.4041 0.0532 0.088 Uiso 1 1 calc R . . H66B H 0.3282 0.4661 0.0571 0.088 Uiso 1 1 calc R . . H66C H 0.3064 0.3978 0.0334 0.088 Uiso 1 1 calc R . . C43 C 0.36424(19) 0.0625(3) 0.1384(2) 0.0440(14) Uani 1 1 d . . . C57 C 0.3206(3) 0.4688(4) 0.4532(2) 0.070(2) Uani 1 1 d . . . H57 H 0.3145 0.4614 0.4812 0.084 Uiso 1 1 calc R . . C21 C 0.51147(18) 0.1349(3) 0.5054(2) 0.0509(16) Uani 1 1 d . . . C14 C 0.3169(3) -0.0640(4) 0.1784(2) 0.070(2) Uani 1 1 d . . . H14 H 0.3159 -0.0939 0.1535 0.084 Uiso 1 1 calc R . . C13 C 0.2827(3) -0.0266(4) 0.1745(2) 0.065(2) Uani 1 1 d . . . H13 H 0.2585 -0.0285 0.1462 0.078 Uiso 1 1 calc R . . C40 C 0.41199(15) 0.1599(2) 0.25247(18) 0.0292(11) Uani 1 1 d . . . C1 C 0.2365(2) 0.3989(4) 0.1956(2) 0.0530(16) Uani 1 1 d . . . H1 H 0.2599 0.4205 0.1932 0.064 Uiso 1 1 calc R . . C15 C 0.3531(3) -0.0577(4) 0.2193(2) 0.0631(19) Uani 1 1 d . . . H15 H 0.3771 -0.0821 0.2218 0.076 Uiso 1 1 calc R . . C25 C 0.2948(3) 0.0033(4) 0.4584(2) 0.067(2) Uani 1 1 d . . . H25 H 0.2864 -0.0170 0.4818 0.080 Uiso 1 1 calc R . . C22 C 0.5533(2) 0.1279(4) 0.5472(3) 0.074(2) Uani 1 1 d . . . H22A H 0.5533 0.0872 0.5653 0.111 Uiso 1 1 calc R . . H22B H 0.5578 0.1666 0.5684 0.111 Uiso 1 1 calc R . . H22C H 0.5754 0.1255 0.5344 0.111 Uiso 1 1 calc R . . C11 C 0.3047(3) 0.1519(4) 0.5483(3) 0.072(2) Uani 1 1 d . . . H11A H 0.3298 0.1295 0.5695 0.108 Uiso 1 1 calc R . . H11B H 0.2820 0.1197 0.5372 0.108 Uiso 1 1 calc R . . H11C H 0.2975 0.1879 0.5660 0.108 Uiso 1 1 calc R . . C3 C 0.1642(2) 0.3707(4) 0.1596(2) 0.063(2) Uani 1 1 d . . . H3 H 0.1384 0.3723 0.1335 0.076 Uiso 1 1 calc R . . C55 C 0.4395(3) 0.4786(4) 0.5558(2) 0.077(2) Uani 1 1 d . . . H55A H 0.4195 0.4667 0.5705 0.116 Uiso 1 1 calc R . . H55B H 0.4360 0.5256 0.5462 0.116 Uiso 1 1 calc R . . H55C H 0.4676 0.4715 0.5792 0.116 Uiso 1 1 calc R . . C36 C 0.5853(2) 0.2385(4) 0.4576(3) 0.066(2) Uani 1 1 d . . . H36 H 0.6131 0.2319 0.4788 0.079 Uiso 1 1 calc R . . C59 C 0.3443(3) 0.5402(4) 0.4031(2) 0.074(2) Uani 1 1 d . . . H59 H 0.3547 0.5811 0.3964 0.089 Uiso 1 1 calc R . . C44 C 0.3556(3) 0.0128(4) 0.0979(2) 0.068(2) Uani 1 1 d . . . H44A H 0.3307 -0.0127 0.0945 0.103 Uiso 1 1 calc R . . H44B H 0.3791 -0.0177 0.1051 0.103 Uiso 1 1 calc R . . H44C H 0.3514 0.0366 0.0679 0.103 Uiso 1 1 calc R . . C35 C 0.5641(2) 0.2961(4) 0.4616(2) 0.064(2) Uani 1 1 d . . . H35 H 0.5769 0.3279 0.4861 0.077 Uiso 1 1 calc R . . O11 O 0.0624(3) -0.4867(5) -0.0631(3) 0.154(4) Uani 1 1 d . . . O14 O 0.0755(3) -0.3726(6) -0.0741(5) 0.219(6) Uani 1 1 d . . . O19 O -0.0311(3) -0.1072(6) -0.1172(4) 0.197(5) Uani 1 1 d . . . C58 C 0.3351(4) 0.5334(4) 0.4446(3) 0.099(4) Uani 1 1 d . . . H58 H 0.3382 0.5696 0.4660 0.119 Uiso 1 1 calc R . . O21 O -0.0845(3) -0.1731(8) -0.1213(4) 0.227(7) Uani 1 1 d . . . O12 O 0.0537(7) -0.4309(11) -0.1364(6) 0.327(11) Uani 1 1 d . . . O20 O -0.0174(3) -0.2022(5) -0.0764(5) 0.213(6) Uani 1 1 d . . . O22 O -0.0481(8) -0.1274(7) -0.0507(6) 0.308(11) Uani 1 1 d . . . O15 O 0.1822(3) -0.1404(8) -0.0382(5) 0.240(8) Uani 1 1 d . . . O13 O 0.0077(3) -0.4180(8) -0.1041(5) 0.236(7) Uani 1 1 d . . . O18 O 0.1500(6) -0.0879(4) -0.1091(5) 0.266(9) 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 0.0388(4) 0.0326(4) 0.0250(4) 0.0018(3) 0.0119(3) 0.0023(3) Mn2 0.0311(4) 0.0288(4) 0.0250(4) 0.0006(3) 0.0085(3) 0.0009(3) Mn4 0.0306(4) 0.0280(4) 0.0226(4) 0.0006(3) 0.0071(3) -0.0021(3) Mn5 0.0309(4) 0.0305(4) 0.0241(4) -0.0036(3) 0.0089(3) -0.0015(3) Mn3 0.0343(4) 0.0355(4) 0.0236(4) 0.0025(3) 0.0054(3) -0.0056(3) Cl1 0.0537(9) 0.0627(10) 0.0478(9) -0.0003(7) 0.0123(7) -0.0028(8) Cl3 0.0987(15) 0.0774(14) 0.1116(18) -0.0338(13) 0.0777(15) -0.0242(12) Cl4 0.0858(14) 0.0769(14) 0.0842(14) 0.0405(11) 0.0376(12) 0.0206(11) O2 0.0286(17) 0.0345(19) 0.0276(17) -0.0006(14) 0.0044(14) 0.0030(15) O5 0.0337(18) 0.0304(19) 0.0270(17) -0.0067(14) 0.0116(15) -0.0039(15) Cl2 0.0926(18) 0.117(2) 0.152(3) -0.055(2) 0.0612(18) -0.0292(17) O6 0.0373(18) 0.0263(18) 0.0283(17) 0.0010(14) 0.0145(15) -0.0051(15) O4 0.0328(17) 0.0297(18) 0.0265(17) -0.0042(14) 0.0097(14) -0.0003(15) O1 0.0317(17) 0.034(2) 0.0311(18) 0.0039(14) 0.0141(15) 0.0030(15) O3 0.0261(17) 0.039(2) 0.0267(17) -0.0006(15) 0.0042(14) -0.0026(15) N23 0.041(2) 0.037(2) 0.027(2) -0.0081(18) 0.0116(19) -0.006(2) N17 0.035(2) 0.042(3) 0.027(2) 0.0082(19) -0.0013(18) -0.008(2) N18 0.037(2) 0.044(3) 0.032(2) 0.009(2) -0.0020(19) -0.003(2) N35 0.040(2) 0.034(2) 0.027(2) -0.0009(18) 0.0131(19) -0.0023(19) N27 0.036(2) 0.038(2) 0.026(2) -0.0057(18) 0.0143(18) -0.0069(19) N25 0.036(2) 0.041(3) 0.032(2) -0.0031(19) 0.0134(19) -0.004(2) N13 0.061(3) 0.044(3) 0.027(2) -0.002(2) 0.017(2) -0.020(2) N7 0.061(3) 0.035(3) 0.037(3) 0.000(2) 0.012(2) -0.013(2) N4 0.036(2) 0.037(3) 0.042(3) 0.007(2) 0.017(2) 0.003(2) N33 0.047(2) 0.030(2) 0.024(2) -0.0005(17) 0.0108(19) 0.001(2) N28 0.043(2) 0.034(2) 0.025(2) -0.0034(17) 0.0139(19) -0.003(2) N15 0.036(2) 0.049(3) 0.031(2) 0.000(2) 0.0103(19) -0.014(2) N11 0.030(2) 0.044(3) 0.023(2) 0.0040(18) -0.0016(17) -0.002(2) N6 0.058(3) 0.047(3) 0.034(2) 0.016(2) 0.020(2) 0.018(2) N19 0.031(2) 0.054(3) 0.030(2) 0.001(2) 0.0083(18) 0.001(2) N3 0.033(2) 0.041(3) 0.033(2) 0.0059(19) 0.0080(19) 0.008(2) N1 0.043(3) 0.048(3) 0.037(3) 0.005(2) 0.012(2) 0.015(2) N9 0.047(3) 0.029(2) 0.033(2) -0.0063(18) 0.013(2) -0.001(2) N26 0.068(3) 0.034(3) 0.046(3) 0.002(2) 0.026(3) -0.008(2) N24 0.049(3) 0.037(3) 0.030(2) -0.0081(19) 0.006(2) -0.011(2) N5 0.042(2) 0.036(2) 0.028(2) 0.0115(18) 0.0127(19) 0.007(2) N31 0.049(3) 0.037(3) 0.027(2) -0.0014(18) 0.012(2) 0.005(2) O10 0.071(3) 0.090(4) 0.045(3) 0.004(2) 0.010(2) -0.006(3) N10 0.040(2) 0.036(3) 0.033(2) -0.0041(19) 0.008(2) 0.001(2) N21 0.029(2) 0.040(3) 0.037(2) -0.0048(19) 0.0125(19) 0.0014(19) N34 0.041(2) 0.033(2) 0.023(2) -0.0047(17) 0.0113(18) 0.0028(19) N2 0.033(2) 0.052(3) 0.077(4) 0.017(3) 0.004(3) -0.002(2) N30 0.053(3) 0.048(3) 0.028(2) -0.008(2) 0.021(2) -0.004(2) N32 0.063(3) 0.031(3) 0.053(3) -0.009(2) 0.021(3) -0.007(2) N36 0.046(3) 0.037(2) 0.025(2) -0.0034(18) 0.0153(19) -0.006(2) N22 0.036(2) 0.036(2) 0.038(2) -0.0095(19) 0.012(2) -0.002(2) N12 0.041(3) 0.049(3) 0.037(3) -0.002(2) -0.003(2) -0.005(2) N16 0.035(2) 0.047(3) 0.033(2) 0.002(2) 0.0116(19) -0.006(2) N29 0.048(3) 0.041(3) 0.027(2) -0.0006(19) 0.018(2) 0.000(2) N14 0.052(3) 0.056(3) 0.063(3) 0.012(3) 0.032(3) -0.008(3) O9 0.070(3) 0.057(3) 0.131(5) 0.000(3) 0.035(3) 0.005(3) C19 0.030(2) 0.033(3) 0.038(3) 0.001(2) 0.009(2) 0.001(2) C63 0.035(3) 0.033(3) 0.026(2) -0.001(2) 0.011(2) 0.003(2) C49 0.025(2) 0.041(3) 0.032(3) 0.003(2) 0.011(2) -0.004(2) O8 0.061(3) 0.171(7) 0.066(3) 0.050(4) 0.016(3) -0.009(4) C50 0.034(3) 0.028(3) 0.037(3) 0.002(2) 0.013(2) -0.003(2) C56 0.074(4) 0.045(4) 0.037(3) -0.003(3) 0.020(3) 0.010(3) C45 0.044(3) 0.048(3) 0.039(3) -0.006(3) 0.022(3) -0.004(3) C48 0.053(3) 0.046(3) 0.037(3) 0.008(2) 0.022(3) 0.001(3) C52 0.042(3) 0.035(3) 0.027(3) -0.005(2) 0.012(2) 0.001(2) C5 0.042(3) 0.035(3) 0.038(3) -0.004(2) 0.005(2) 0.009(2) C38 0.032(3) 0.055(4) 0.037(3) 0.001(3) 0.007(2) -0.002(3) C6 0.038(3) 0.037(3) 0.037(3) -0.001(2) 0.008(2) 0.008(2) N8 0.070(4) 0.044(3) 0.072(4) -0.013(3) 0.028(3) 0.004(3) N20 0.042(3) 0.053(3) 0.083(4) -0.013(3) 0.009(3) 0.010(3) C18 0.033(3) 0.028(3) 0.032(3) 0.003(2) 0.012(2) 0.001(2) C61 0.040(3) 0.037(3) 0.035(3) 0.000(2) 0.009(2) 0.009(2) C60 0.065(4) 0.028(3) 0.024(3) -0.001(2) 0.009(2) 0.014(3) C62 0.032(2) 0.035(3) 0.025(2) 0.005(2) 0.010(2) 0.000(2) C9 0.049(3) 0.037(3) 0.064(4) 0.017(3) 0.032(3) 0.007(3) C28 0.049(3) 0.037(3) 0.044(3) -0.007(2) 0.026(3) -0.017(3) O7 0.101(4) 0.070(4) 0.073(4) -0.027(3) 0.025(3) -0.005(3) C30 0.034(3) 0.031(3) 0.032(3) -0.001(2) 0.006(2) -0.004(2) C20 0.043(3) 0.046(3) 0.041(3) 0.004(3) 0.002(3) 0.009(3) C47 0.053(3) 0.064(4) 0.036(3) 0.015(3) 0.024(3) 0.006(3) C42 0.051(3) 0.038(3) 0.041(3) -0.013(2) 0.022(3) -0.010(3) C41 0.046(3) 0.023(3) 0.036(3) -0.003(2) 0.019(2) -0.004(2) C7 0.038(3) 0.030(3) 0.030(3) 0.003(2) 0.012(2) 0.003(2) C23 0.059(4) 0.067(4) 0.035(3) 0.007(3) 0.014(3) -0.022(3) C12 0.071(4) 0.049(4) 0.038(3) -0.006(3) 0.008(3) -0.018(3) C17 0.065(4) 0.034(3) 0.045(3) -0.003(3) 0.023(3) -0.008(3) C53 0.068(4) 0.032(3) 0.041(3) -0.005(2) 0.024(3) -0.007(3) C39 0.029(3) 0.045(3) 0.052(3) 0.006(3) 0.009(2) 0.006(2) C37 0.043(3) 0.077(5) 0.056(4) 0.005(4) 0.004(3) 0.015(3) C8 0.039(3) 0.028(3) 0.036(3) 0.005(2) 0.015(2) 0.001(2) C64 0.045(3) 0.029(3) 0.031(3) 0.005(2) 0.011(2) 0.001(2) C32 0.036(3) 0.043(3) 0.047(3) 0.007(3) 0.001(3) 0.003(3) C4 0.039(3) 0.058(4) 0.048(4) 0.002(3) -0.002(3) 0.001(3) C27 0.059(4) 0.042(3) 0.034(3) -0.009(2) 0.023(3) -0.023(3) O16 0.145(6) 0.114(6) 0.160(7) 0.000(5) 0.122(6) -0.003(5) O17 0.207(9) 0.095(5) 0.185(8) -0.045(5) 0.156(7) -0.017(5) C46 0.042(3) 0.078(5) 0.036(3) -0.009(3) 0.018(3) -0.007(3) C10 0.065(4) 0.039(3) 0.060(4) 0.014(3) 0.041(3) 0.015(3) C65 0.048(3) 0.039(3) 0.035(3) 0.005(2) 0.020(2) -0.007(3) C16 0.077(4) 0.038(3) 0.037(3) -0.009(2) 0.026(3) -0.018(3) C51 0.033(3) 0.029(3) 0.029(3) -0.007(2) 0.006(2) 0.000(2) C26 0.068(4) 0.059(4) 0.041(3) -0.002(3) 0.029(3) -0.019(3) C54 0.071(4) 0.045(4) 0.038(3) -0.014(3) 0.020(3) -0.003(3) C2 0.058(4) 0.066(4) 0.033(3) 0.009(3) 0.011(3) 0.017(3) C34 0.038(3) 0.067(4) 0.039(3) -0.013(3) 0.016(3) -0.004(3) C31 0.034(3) 0.056(4) 0.039(3) -0.001(3) 0.006(2) -0.003(3) C24 0.086(5) 0.076(5) 0.031(3) 0.015(3) 0.009(3) -0.028(4) C29 0.032(2) 0.034(3) 0.024(2) -0.003(2) 0.006(2) -0.002(2) C33 0.048(4) 0.089(6) 0.052(4) 0.019(4) -0.006(3) -0.003(4) C66 0.083(5) 0.063(4) 0.029(3) 0.008(3) 0.020(3) -0.005(4) C43 0.056(3) 0.039(3) 0.042(3) -0.010(2) 0.024(3) -0.014(3) C57 0.128(7) 0.050(4) 0.042(4) -0.001(3) 0.043(4) 0.013(4) C21 0.039(3) 0.058(4) 0.042(3) 0.009(3) -0.001(3) 0.010(3) C14 0.114(7) 0.057(5) 0.041(4) -0.017(3) 0.032(4) -0.041(5) C13 0.097(6) 0.050(4) 0.039(4) -0.006(3) 0.016(4) -0.031(4) C40 0.032(2) 0.027(3) 0.030(3) -0.005(2) 0.013(2) -0.002(2) C1 0.046(3) 0.072(5) 0.035(3) 0.010(3) 0.007(3) 0.018(3) C15 0.089(5) 0.054(4) 0.054(4) -0.020(3) 0.035(4) -0.018(4) C25 0.087(5) 0.076(5) 0.040(4) 0.010(3) 0.027(4) -0.021(4) C22 0.043(4) 0.094(6) 0.057(4) -0.001(4) -0.013(3) 0.016(4) C11 0.101(6) 0.064(5) 0.066(5) 0.033(4) 0.049(5) 0.023(4) C3 0.062(4) 0.059(4) 0.037(3) -0.006(3) -0.017(3) 0.013(4) C55 0.130(7) 0.064(5) 0.046(4) -0.028(3) 0.042(4) -0.019(5) C36 0.040(3) 0.089(6) 0.050(4) -0.009(4) -0.007(3) 0.008(4) C59 0.138(8) 0.044(4) 0.047(4) -0.002(3) 0.042(5) 0.000(4) C44 0.108(6) 0.046(4) 0.052(4) -0.018(3) 0.030(4) -0.009(4) C35 0.041(3) 0.099(6) 0.039(3) -0.017(4) -0.001(3) 0.003(4) O11 0.136(7) 0.134(7) 0.166(8) 0.068(6) 0.026(6) -0.019(6) O14 0.109(6) 0.178(10) 0.289(14) -0.109(10) -0.020(8) -0.058(7) O19 0.142(7) 0.220(11) 0.226(10) 0.167(9) 0.065(7) 0.002(7) C58 0.215(12) 0.055(5) 0.040(4) -0.016(3) 0.061(6) -0.004(6) O21 0.089(6) 0.364(18) 0.189(10) 0.134(12) 0.007(6) -0.050(8) O12 0.45(3) 0.38(2) 0.279(17) -0.016(16) 0.29(2) 0.09(2) O20 0.107(6) 0.170(9) 0.309(14) 0.165(10) 0.017(7) 0.052(6) O22 0.61(3) 0.159(11) 0.329(19) -0.054(12) 0.38(2) -0.063(15) O15 0.118(7) 0.350(19) 0.213(12) -0.158(13) 0.017(8) -0.016(9) O13 0.073(5) 0.339(18) 0.277(14) -0.049(13) 0.042(7) -0.045(8) O18 0.60(3) 0.061(5) 0.315(15) 0.007(7) 0.377(19) -0.007(9) _geom_special_details ; All s.u.'s (except the s.u. in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell s.u.'s are taken into account individually in the estimation of s.u.'s in distances, angles and torsion angles; correlations between s.u.'s in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell s.u.'s is used for estimating s.u.'s 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 N3 2.138(5) . ? Mn1 N33 2.155(4) . ? Mn1 O6 2.201(3) . ? Mn1 O1 2.215(3) . ? Mn1 N31 2.437(4) . ? Mn1 N1 2.521(4) . ? Mn2 O5 2.165(3) . ? Mn2 O1 2.181(3) . ? Mn2 O2 2.188(3) . ? Mn2 N5 2.218(5) . ? Mn2 N11 2.231(4) . ? Mn2 N29 2.247(5) . ? Mn4 O6 2.143(3) . ? Mn4 O3 2.153(4) . ? Mn4 O4 2.182(3) . ? Mn4 N23 2.192(4) . ? Mn4 N35 2.222(4) . ? Mn4 N17 2.223(4) . ? Mn5 N27 2.145(4) . ? Mn5 N21 2.165(4) . ? Mn5 O5 2.205(3) . ? Mn5 O4 2.210(3) . ? Mn5 N25 2.425(4) . ? Mn5 N19 2.478(4) . ? Mn3 N9 2.136(5) . ? Mn3 N15 2.143(5) . ? Mn3 O3 2.204(3) . ? Mn3 O2 2.205(3) . ? Mn3 N13 2.408(4) . ? Mn3 N7 2.479(5) . ? Cl1 O10 1.399(5) . ? Cl1 O9 1.420(6) . ? Cl1 O8 1.427(6) . ? Cl1 O7 1.434(6) . ? Cl3 O18 1.270(9) . ? Cl3 O16 1.362(7) . ? Cl3 O17 1.425(6) . ? Cl3 O15 1.476(11) . ? Cl4 O20 1.288(8) . ? Cl4 O21 1.325(9) . ? Cl4 O22 1.371(12) . ? Cl4 O19 1.403(7) . ? O2 C18 1.301(6) . ? O5 C51 1.312(6) . ? Cl2 O14 1.316(9) . ? Cl2 O13 1.365(9) . ? Cl2 O11 1.413(8) . ? Cl2 O12 1.420(13) . ? O6 C62 1.307(6) . ? O4 C40 1.304(6) . ? O1 C7 1.324(6) . ? O3 C29 1.307(6) . ? N23 C41 1.333(7) . ? N23 N24 1.340(6) . ? N17 N18 1.335(6) . ? N17 C30 1.336(7) . ? N18 C32 1.338(7) . ? N18 H18N 0.8600 . ? N35 C63 1.338(7) . ? N35 N36 1.339(6) . ? N27 C50 1.303(7) . ? N27 N28 1.408(6) . ? N25 C45 1.330(7) . ? N25 C49 1.350(7) . ? N13 C27 1.318(8) . ? N13 C23 1.337(8) . ? N7 C12 1.331(8) . ? N7 C16 1.336(9) . ? N4 C7 1.290(7) . ? N4 N3 1.398(6) . ? N33 C61 1.304(7) . ? N33 N34 1.404(6) . ? N28 C51 1.285(7) . ? N15 C28 1.308(7) . ? N15 N16 1.383(6) . ? N11 C19 1.318(7) . ? N11 N12 1.360(6) . ? N6 N5 1.344(6) . ? N6 C10 1.344(8) . ? N6 H6N 0.8600 . ? N19 C34 1.343(7) . ? N19 C38 1.350(8) . ? N3 C6 1.300(7) . ? N1 C1 1.340(8) . ? N1 C5 1.348(8) . ? N9 C17 1.297(7) . ? N9 N10 1.416(6) . ? N26 C50 1.339(7) . ? N26 H26A 0.8600 . ? N26 H26B 0.8600 . ? N24 C43 1.345(8) . ? N24 H24N 0.8600 . ? N5 C8 1.340(7) . ? N31 C56 1.331(8) . ? N31 C60 1.338(7) . ? N10 C18 1.281(7) . ? N21 C39 1.301(7) . ? N21 N22 1.400(6) . ? N34 C62 1.295(7) . ? N2 C6 1.328(8) . ? N2 H2A 0.8600 . ? N2 H2B 0.8600 . ? N30 C54 1.339(8) . ? N30 N29 1.350(6) . ? N30 H30N 0.8600 . ? N32 C61 1.323(7) . ? N32 H32A 0.8600 . ? N32 H32B 0.8600 . ? N36 C65 1.342(7) . ? N36 H36N 0.8600 . ? N22 C40 1.284(6) . ? N12 C21 1.359(8) . ? N12 H12N 0.8600 . ? N16 C29 1.292(7) . ? N29 C52 1.321(7) . ? N14 C28 1.349(8) . ? N14 H14A 0.8600 . ? N14 H14B 0.8600 . ? C19 C20 1.392(7) . ? C19 C18 1.485(7) . ? C63 C64 1.396(7) . ? C63 C62 1.482(7) . ? C49 C48 1.390(7) . ? C49 C50 1.465(7) . ? C56 C57 1.351(9) . ? C56 H56 0.9300 . ? C45 C46 1.395(9) . ? C45 H45 0.9300 . ? C48 C47 1.395(8) . ? C48 H48 0.9300 . ? C52 C53 1.378(7) . ? C52 C51 1.488(7) . ? C5 C4 1.377(8) . ? C5 C6 1.489(8) . ? C38 C37 1.390(8) . ? C38 C39 1.470(8) . ? N8 C17 1.334(8) . ? N8 H8A 0.8600 . ? N8 H8B 0.8600 . ? N20 C39 1.326(8) . ? N20 H20A 0.8600 . ? N20 H20B 0.8600 . ? C61 C60 1.473(8) . ? C60 C59 1.389(8) . ? C9 C10 1.370(9) . ? C9 C8 1.409(8) . ? C9 H9 0.9300 . ? C28 C27 1.486(8) . ? C30 C31 1.401(7) . ? C30 C29 1.474(7) . ? C20 C21 1.335(9) . ? C20 H20 0.9300 . ? C47 C46 1.359(9) . ? C47 H47 0.9300 . ? C42 C43 1.374(8) . ? C42 C41 1.399(7) . ? C42 H42 0.9300 . ? C41 C40 1.485(7) . ? C7 C8 1.457(7) . ? C23 C24 1.375(9) . ? C23 H23 0.9300 . ? C12 C13 1.404(9) . ? C12 H12 0.9300 . ? C17 C16 1.486(9) . ? C53 C54 1.347(9) . ? C53 H53 0.9300 . ? C37 C36 1.372(10) . ? C37 H37 0.9300 . ? C64 C65 1.381(8) . ? C64 H64 0.9300 . ? C32 C31 1.352(8) . ? C32 C33 1.520(8) . ? C4 C3 1.379(10) . ? C4 H4 0.9300 . ? C27 C26 1.384(8) . ? C46 H46 0.9300 . ? C10 C11 1.488(9) . ? C65 C66 1.484(8) . ? C16 C15 1.387(9) . ? C26 C25 1.372(10) . ? C26 H26 0.9300 . ? C54 C55 1.516(8) . ? C2 C3 1.363(10) . ? C2 C1 1.396(8) . ? C2 H2 0.9300 . ? C34 C35 1.392(8) . ? C34 H34 0.9300 . ? C31 H31 0.9300 . ? C24 C25 1.383(11) . ? C24 H24 0.9300 . ? C33 H33A 0.9600 . ? C33 H33B 0.9600 . ? C33 H33C 0.9600 . ? C66 H66A 0.9600 . ? C66 H66B 0.9600 . ? C66 H66C 0.9600 . ? C43 C44 1.481(8) . ? C57 C58 1.419(11) . ? C57 H57 0.9300 . ? C21 C22 1.504(8) . ? C14 C13 1.348(12) . ? C14 C15 1.373(10) . ? C14 H14 0.9300 . ? C13 H13 0.9300 . ? C1 H1 0.9300 . ? C15 H15 0.9300 . ? C25 H25 0.9300 . ? C22 H22A 0.9600 . ? C22 H22B 0.9600 . ? C22 H22C 0.9600 . ? C11 H11A 0.9600 . ? C11 H11B 0.9600 . ? C11 H11C 0.9600 . ? C3 H3 0.9300 . ? C55 H55A 0.9600 . ? C55 H55B 0.9600 . ? C55 H55C 0.9600 . ? C36 C35 1.372(10) . ? C36 H36 0.9300 . ? C59 C58 1.374(11) . ? C59 H59 0.9300 . ? C44 H44A 0.9600 . ? C44 H44B 0.9600 . ? C44 H44C 0.9600 . ? C35 H35 0.9300 . ? C58 H58 0.9300 . ? 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 N3 Mn1 N33 145.67(17) . . ? N3 Mn1 O6 127.48(15) . . ? N33 Mn1 O6 71.06(14) . . ? N3 Mn1 O1 71.97(14) . . ? N33 Mn1 O1 132.65(14) . . ? O6 Mn1 O1 112.32(13) . . ? N3 Mn1 N31 97.21(17) . . ? N33 Mn1 N31 68.65(16) . . ? O6 Mn1 N31 135.13(15) . . ? O1 Mn1 N31 82.47(14) . . ? N3 Mn1 N1 67.42(16) . . ? N33 Mn1 N1 90.68(16) . . ? O6 Mn1 N1 81.93(14) . . ? O1 Mn1 N1 136.48(15) . . ? N31 Mn1 N1 117.06(15) . . ? O5 Mn2 O1 86.04(13) . . ? O5 Mn2 O2 92.13(13) . . ? O1 Mn2 O2 88.12(13) . . ? O5 Mn2 N5 156.94(15) . . ? O1 Mn2 N5 75.37(14) . . ? O2 Mn2 N5 100.62(15) . . ? O5 Mn2 N11 98.49(15) . . ? O1 Mn2 N11 162.12(15) . . ? O2 Mn2 N11 74.48(14) . . ? N5 Mn2 N11 103.38(16) . . ? O5 Mn2 N29 75.05(14) . . ? O1 Mn2 N29 102.29(15) . . ? O2 Mn2 N29 162.67(15) . . ? N5 Mn2 N29 95.45(17) . . ? N11 Mn2 N29 95.59(16) . . ? O6 Mn4 O3 92.07(13) . . ? O6 Mn4 O4 87.39(13) . . ? O3 Mn4 O4 91.11(13) . . ? O6 Mn4 N23 158.13(15) . . ? O3 Mn4 N23 100.97(15) . . ? O4 Mn4 N23 74.98(14) . . ? O6 Mn4 N35 76.06(14) . . ? O3 Mn4 N35 157.62(15) . . ? O4 Mn4 N35 106.94(14) . . ? N23 Mn4 N35 96.51(17) . . ? O6 Mn4 N17 105.32(16) . . ? O3 Mn4 N17 75.96(14) . . ? O4 Mn4 N17 161.97(15) . . ? N23 Mn4 N17 94.91(17) . . ? N35 Mn4 N17 88.78(16) . . ? N27 Mn5 N21 147.86(16) . . ? N27 Mn5 O5 71.22(14) . . ? N21 Mn5 O5 126.36(15) . . ? N27 Mn5 O4 131.93(14) . . ? N21 Mn5 O4 71.11(14) . . ? O5 Mn5 O4 111.77(12) . . ? N27 Mn5 N25 68.77(15) . . ? N21 Mn5 N25 97.28(16) . . ? O5 Mn5 N25 136.20(14) . . ? O4 Mn5 N25 83.39(14) . . ? N27 Mn5 N19 91.42(16) . . ? N21 Mn5 N19 68.17(16) . . ? O5 Mn5 N19 81.75(14) . . ? O4 Mn5 N19 136.53(15) . . ? N25 Mn5 N19 115.99(15) . . ? N9 Mn3 N15 148.58(18) . . ? N9 Mn3 O3 125.04(16) . . ? N15 Mn3 O3 71.46(15) . . ? N9 Mn3 O2 71.91(14) . . ? N15 Mn3 O2 131.21(16) . . ? O3 Mn3 O2 111.18(13) . . ? N9 Mn3 N13 97.26(18) . . ? N15 Mn3 N13 69.07(17) . . ? O3 Mn3 N13 137.43(16) . . ? O2 Mn3 N13 84.23(14) . . ? N9 Mn3 N7 67.98(17) . . ? N15 Mn3 N7 90.45(18) . . ? O3 Mn3 N7 83.24(14) . . ? O2 Mn3 N7 138.09(16) . . ? N13 Mn3 N7 112.09(16) . . ? O10 Cl1 O9 111.2(4) . . ? O10 Cl1 O8 108.9(3) . . ? O9 Cl1 O8 108.3(4) . . ? O10 Cl1 O7 110.0(4) . . ? O9 Cl1 O7 106.7(4) . . ? O8 Cl1 O7 111.8(4) . . ? O18 Cl3 O16 120.0(9) . . ? O18 Cl3 O17 109.7(6) . . ? O16 Cl3 O17 106.8(5) . . ? O18 Cl3 O15 107.4(10) . . ? O16 Cl3 O15 102.2(7) . . ? O17 Cl3 O15 110.4(7) . . ? O20 Cl4 O21 119.3(9) . . ? O20 Cl4 O22 104.4(11) . . ? O21 Cl4 O22 107.7(11) . . ? O20 Cl4 O19 107.7(7) . . ? O21 Cl4 O19 107.8(6) . . ? O22 Cl4 O19 109.7(8) . . ? C18 O2 Mn2 116.9(3) . . ? C18 O2 Mn3 111.2(3) . . ? Mn2 O2 Mn3 129.31(16) . . ? C51 O5 Mn2 117.1(3) . . ? C51 O5 Mn5 110.4(3) . . ? Mn2 O5 Mn5 128.92(16) . . ? O14 Cl2 O13 120.6(9) . . ? O14 Cl2 O11 117.4(7) . . ? O13 Cl2 O11 108.7(8) . . ? O14 Cl2 O12 96.9(11) . . ? O13 Cl2 O12 99.7(11) . . ? O11 Cl2 O12 111.0(9) . . ? C62 O6 Mn4 116.8(3) . . ? C62 O6 Mn1 111.0(3) . . ? Mn4 O6 Mn1 128.69(16) . . ? C40 O4 Mn4 116.5(3) . . ? C40 O4 Mn5 112.0(3) . . ? Mn4 O4 Mn5 129.58(16) . . ? C7 O1 Mn2 116.4(3) . . ? C7 O1 Mn1 109.7(3) . . ? Mn2 O1 Mn1 130.76(16) . . ? C29 O3 Mn4 116.4(3) . . ? C29 O3 Mn3 110.4(3) . . ? Mn4 O3 Mn3 131.01(16) . . ? C41 N23 N24 104.8(4) . . ? C41 N23 Mn4 115.0(3) . . ? N24 N23 Mn4 140.0(4) . . ? N18 N17 C30 105.2(4) . . ? N18 N17 Mn4 142.5(4) . . ? C30 N17 Mn4 111.9(3) . . ? N17 N18 C32 112.2(5) . . ? N17 N18 H18N 123.9 . . ? C32 N18 H18N 123.9 . . ? C63 N35 N36 104.9(4) . . ? C63 N35 Mn4 112.6(3) . . ? N36 N35 Mn4 142.3(3) . . ? C50 N27 N28 115.5(4) . . ? C50 N27 Mn5 126.7(3) . . ? N28 N27 Mn5 117.5(3) . . ? C45 N25 C49 118.5(5) . . ? C45 N25 Mn5 126.5(4) . . ? C49 N25 Mn5 113.9(3) . . ? C27 N13 C23 118.6(5) . . ? C27 N13 Mn3 115.2(4) . . ? C23 N13 Mn3 125.9(4) . . ? C12 N7 C16 118.5(6) . . ? C12 N7 Mn3 127.4(5) . . ? C16 N7 Mn3 113.4(4) . . ? C7 N4 N3 109.9(4) . . ? C61 N33 N34 115.0(4) . . ? C61 N33 Mn1 126.8(4) . . ? N34 N33 Mn1 118.2(3) . . ? C51 N28 N27 108.7(4) . . ? C28 N15 N16 115.6(5) . . ? C28 N15 Mn3 125.9(4) . . ? N16 N15 Mn3 118.5(3) . . ? C19 N11 N12 104.5(4) . . ? C19 N11 Mn2 114.6(3) . . ? N12 N11 Mn2 140.9(4) . . ? N5 N6 C10 113.1(5) . . ? N5 N6 H6N 123.4 . . ? C10 N6 H6N 123.4 . . ? C34 N19 C38 118.2(5) . . ? C34 N19 Mn5 127.7(4) . . ? C38 N19 Mn5 113.2(3) . . ? C6 N3 N4 113.4(5) . . ? C6 N3 Mn1 128.9(4) . . ? N4 N3 Mn1 117.7(3) . . ? C1 N1 C5 117.4(5) . . ? C1 N1 Mn1 128.6(4) . . ? C5 N1 Mn1 113.7(3) . . ? C17 N9 N10 114.4(5) . . ? C17 N9 Mn3 128.5(4) . . ? N10 N9 Mn3 116.8(3) . . ? C50 N26 H26A 120.0 . . ? C50 N26 H26B 120.0 . . ? H26A N26 H26B 120.0 . . ? N23 N24 C43 112.8(4) . . ? N23 N24 H24N 123.6 . . ? C43 N24 H24N 123.6 . . ? C8 N5 N6 104.7(4) . . ? C8 N5 Mn2 113.2(3) . . ? N6 N5 Mn2 142.1(4) . . ? C56 N31 C60 118.4(5) . . ? C56 N31 Mn1 127.6(4) . . ? C60 N31 Mn1 113.9(3) . . ? C18 N10 N9 110.1(4) . . ? C39 N21 N22 114.3(5) . . ? C39 N21 Mn5 126.5(4) . . ? N22 N21 Mn5 118.4(3) . . ? C62 N34 N33 108.5(4) . . ? C6 N2 H2A 120.0 . . ? C6 N2 H2B 120.0 . . ? H2A N2 H2B 120.0 . . ? C54 N30 N29 112.0(5) . . ? C54 N30 H30N 124.0 . . ? N29 N30 H30N 124.0 . . ? C61 N32 H32A 120.0 . . ? C61 N32 H32B 120.0 . . ? H32A N32 H32B 120.0 . . ? N35 N36 C65 113.1(4) . . ? N35 N36 H36N 123.5 . . ? C65 N36 H36N 123.5 . . ? C40 N22 N21 109.8(4) . . ? C21 N12 N11 110.7(5) . . ? C21 N12 H12N 124.7 . . ? N11 N12 H12N 124.7 . . ? C29 N16 N15 109.2(4) . . ? C52 N29 N30 104.2(4) . . ? C52 N29 Mn2 113.7(3) . . ? N30 N29 Mn2 142.2(4) . . ? C28 N14 H14A 120.0 . . ? C28 N14 H14B 120.0 . . ? H14A N14 H14B 120.0 . . ? N11 C19 C20 111.7(5) . . ? N11 C19 C18 117.2(4) . . ? C20 C19 C18 131.1(5) . . ? N35 C63 C64 110.6(4) . . ? N35 C63 C62 117.6(5) . . ? C64 C63 C62 131.6(5) . . ? N25 C49 C48 122.1(5) . . ? N25 C49 C50 115.6(4) . . ? C48 C49 C50 122.3(5) . . ? N27 C50 N26 124.2(5) . . ? N27 C50 C49 114.2(4) . . ? N26 C50 C49 121.5(5) . . ? N31 C56 C57 123.3(7) . . ? N31 C56 H56 118.4 . . ? C57 C56 H56 118.4 . . ? N25 C45 C46 122.9(6) . . ? N25 C45 H45 118.5 . . ? C46 C45 H45 118.5 . . ? C49 C48 C47 118.0(6) . . ? C49 C48 H48 121.0 . . ? C47 C48 H48 121.0 . . ? N29 C52 C53 111.4(5) . . ? N29 C52 C51 117.4(5) . . ? C53 C52 C51 131.2(5) . . ? N1 C5 C4 123.2(6) . . ? N1 C5 C6 114.2(5) . . ? C4 C5 C6 122.6(6) . . ? N19 C38 C37 122.7(6) . . ? N19 C38 C39 115.2(5) . . ? C37 C38 C39 122.1(6) . . ? N3 C6 N2 123.6(5) . . ? N3 C6 C5 115.7(5) . . ? N2 C6 C5 120.8(5) . . ? C17 N8 H8A 120.0 . . ? C17 N8 H8B 120.0 . . ? H8A N8 H8B 120.0 . . ? C39 N20 H20A 120.0 . . ? C39 N20 H20B 120.0 . . ? H20A N20 H20B 120.0 . . ? N10 C18 O2 126.1(5) . . ? N10 C18 C19 117.0(4) . . ? O2 C18 C19 116.8(4) . . ? N33 C61 N32 124.4(5) . . ? N33 C61 C60 114.1(5) . . ? N32 C61 C60 121.4(5) . . ? N31 C60 C59 122.1(6) . . ? N31 C60 C61 116.1(5) . . ? C59 C60 C61 121.8(6) . . ? N34 C62 O6 126.4(5) . . ? N34 C62 C63 116.7(4) . . ? O6 C62 C63 116.7(4) . . ? C10 C9 C8 105.5(5) . . ? C10 C9 H9 127.2 . . ? C8 C9 H9 127.2 . . ? N15 C28 N14 123.9(6) . . ? N15 C28 C27 114.3(5) . . ? N14 C28 C27 121.6(5) . . ? N17 C30 C31 110.0(5) . . ? N17 C30 C29 118.4(4) . . ? C31 C30 C29 131.5(5) . . ? C21 C20 C19 105.5(5) . . ? C21 C20 H20 127.2 . . ? C19 C20 H20 127.2 . . ? C46 C47 C48 120.2(6) . . ? C46 C47 H47 119.9 . . ? C48 C47 H47 119.9 . . ? C43 C42 C41 105.2(5) . . ? C43 C42 H42 127.4 . . ? C41 C42 H42 127.4 . . ? N23 C41 C42 110.9(5) . . ? N23 C41 C40 116.5(4) . . ? C42 C41 C40 132.6(5) . . ? N4 C7 O1 126.1(5) . . ? N4 C7 C8 117.6(5) . . ? O1 C7 C8 116.3(4) . . ? N13 C23 C24 122.7(7) . . ? N13 C23 H23 118.7 . . ? C24 C23 H23 118.7 . . ? N7 C12 C13 122.3(7) . . ? N7 C12 H12 118.9 . . ? C13 C12 H12 118.9 . . ? N9 C17 N8 124.5(6) . . ? N9 C17 C16 114.0(6) . . ? N8 C17 C16 121.5(6) . . ? C54 C53 C52 105.8(5) . . ? C54 C53 H53 127.1 . . ? C52 C53 H53 127.1 . . ? N21 C39 N20 126.2(6) . . ? N21 C39 C38 114.8(5) . . ? N20 C39 C38 119.0(5) . . ? C36 C37 C38 117.9(7) . . ? C36 C37 H37 121.0 . . ? C38 C37 H37 121.0 . . ? N5 C8 C9 110.4(5) . . ? N5 C8 C7 118.8(5) . . ? C9 C8 C7 130.7(5) . . ? C65 C64 C63 105.5(5) . . ? C65 C64 H64 127.3 . . ? C63 C64 H64 127.3 . . ? N18 C32 C31 107.3(5) . . ? N18 C32 C33 120.3(6) . . ? C31 C32 C33 132.4(6) . . ? C5 C4 C3 118.0(6) . . ? C5 C4 H4 121.0 . . ? C3 C4 H4 121.0 . . ? N13 C27 C26 123.3(6) . . ? N13 C27 C28 115.2(5) . . ? C26 C27 C28 121.5(6) . . ? C47 C46 C45 118.3(6) . . ? C47 C46 H46 120.9 . . ? C45 C46 H46 120.9 . . ? N6 C10 C9 106.3(5) . . ? N6 C10 C11 123.0(6) . . ? C9 C10 C11 130.7(6) . . ? N36 C65 C64 105.9(5) . . ? N36 C65 C66 122.4(5) . . ? C64 C65 C66 131.6(5) . . ? N7 C16 C15 121.6(6) . . ? N7 C16 C17 115.5(5) . . ? C15 C16 C17 122.8(7) . . ? N28 C51 O5 126.6(5) . . ? N28 C51 C52 116.5(4) . . ? O5 C51 C52 116.8(5) . . ? C25 C26 C27 117.2(7) . . ? C25 C26 H26 121.4 . . ? C27 C26 H26 121.4 . . ? N30 C54 C53 106.6(5) . . ? N30 C54 C55 122.0(6) . . ? C53 C54 C55 131.3(6) . . ? C3 C2 C1 117.9(6) . . ? C3 C2 H2 121.0 . . ? C1 C2 H2 121.0 . . ? N19 C34 C35 122.0(6) . . ? N19 C34 H34 119.0 . . ? C35 C34 H34 119.0 . . ? C32 C31 C30 105.4(5) . . ? C32 C31 H31 127.3 . . ? C30 C31 H31 127.3 . . ? C23 C24 C25 117.5(6) . . ? C23 C24 H24 121.2 . . ? C25 C24 H24 121.2 . . ? N16 C29 O3 126.5(4) . . ? N16 C29 C30 116.9(4) . . ? O3 C29 C30 116.6(5) . . ? C32 C33 H33A 109.5 . . ? C32 C33 H33B 109.5 . . ? H33A C33 H33B 109.5 . . ? C32 C33 H33C 109.5 . . ? H33A C33 H33C 109.5 . . ? H33B C33 H33C 109.5 . . ? C65 C66 H66A 109.5 . . ? C65 C66 H66B 109.5 . . ? H66A C66 H66B 109.5 . . ? C65 C66 H66C 109.5 . . ? H66A C66 H66C 109.5 . . ? H66B C66 H66C 109.5 . . ? N24 C43 C42 106.3(5) . . ? N24 C43 C44 122.7(6) . . ? C42 C43 C44 131.1(6) . . ? C56 C57 C58 119.3(7) . . ? C56 C57 H57 120.3 . . ? C58 C57 H57 120.3 . . ? C20 C21 N12 107.5(5) . . ? C20 C21 C22 131.9(6) . . ? N12 C21 C22 120.5(6) . . ? C13 C14 C15 119.8(7) . . ? C13 C14 H14 120.1 . . ? C15 C14 H14 120.1 . . ? C14 C13 C12 118.5(7) . . ? C14 C13 H13 120.8 . . ? C12 C13 H13 120.8 . . ? N22 C40 O4 126.2(4) . . ? N22 C40 C41 117.2(4) . . ? O4 C40 C41 116.5(4) . . ? N1 C1 C2 122.9(7) . . ? N1 C1 H1 118.6 . . ? C2 C1 H1 118.6 . . ? C14 C15 C16 119.2(8) . . ? C14 C15 H15 120.4 . . ? C16 C15 H15 120.4 . . ? C26 C25 C24 120.7(6) . . ? C26 C25 H25 119.7 . . ? C24 C25 H25 119.7 . . ? C21 C22 H22A 109.5 . . ? C21 C22 H22B 109.5 . . ? H22A C22 H22B 109.5 . . ? C21 C22 H22C 109.5 . . ? H22A C22 H22C 109.5 . . ? H22B C22 H22C 109.5 . . ? C10 C11 H11A 109.5 . . ? C10 C11 H11B 109.5 . . ? H11A C11 H11B 109.5 . . ? C10 C11 H11C 109.5 . . ? H11A C11 H11C 109.5 . . ? H11B C11 H11C 109.5 . . ? C2 C3 C4 120.6(6) . . ? C2 C3 H3 119.7 . . ? C4 C3 H3 119.7 . . ? C54 C55 H55A 109.5 . . ? C54 C55 H55B 109.5 . . ? H55A C55 H55B 109.5 . . ? C54 C55 H55C 109.5 . . ? H55A C55 H55C 109.5 . . ? H55B C55 H55C 109.5 . . ? C37 C36 C35 120.4(6) . . ? C37 C36 H36 119.8 . . ? C35 C36 H36 119.8 . . ? C58 C59 C60 119.7(7) . . ? C58 C59 H59 120.2 . . ? C60 C59 H59 120.2 . . ? C43 C44 H44A 109.5 . . ? C43 C44 H44B 109.5 . . ? H44A C44 H44B 109.5 . . ? C43 C44 H44C 109.5 . . ? H44A C44 H44C 109.5 . . ? H44B C44 H44C 109.5 . . ? C36 C35 C34 118.7(6) . . ? C36 C35 H35 120.6 . . ? C34 C35 H35 120.6 . . ? C59 C58 C57 117.1(7) . . ? C59 C58 H58 121.4 . . ? C57 C58 H58 121.4 . . ? _diffrn_measured_fraction_theta_max 0.982 _diffrn_reflns_theta_full 26.37 _diffrn_measured_fraction_theta_full 0.982 _refine_diff_density_max 1.860 _refine_diff_density_min -0.874 _refine_diff_density_rms 0.105 # Details about the Squeezed Material loop_ _platon_squeeze_void_nr _platon_squeeze_void_average_x _platon_squeeze_void_average_y _platon_squeeze_void_average_z _platon_squeeze_void_volume _platon_squeeze_void_count_electrons _platon_squeeze_void_content 1 0.500 0.745 0.250 396 163 ' ' 2 1.000 0.245 0.250 396 163 ' ' 3 0.138 0.181 0.221 5 1 ' ' 4 0.638 0.681 0.221 5 1 ' ' 5 0.362 0.681 0.279 4 1 ' ' 6 0.862 0.181 0.279 4 1 ' ' 7 0.500 0.255 0.750 397 164 ' ' 8 1.000 0.755 0.750 397 164 ' ' 9 0.138 0.819 0.721 5 1 ' ' 10 0.638 0.319 0.721 5 1 ' ' 11 0.362 0.319 0.779 4 1 ' ' 12 0.862 0.819 0.779 4 1 ' ' _platon_squeeze_details ; SQUEEZE was used to remove the contributions of four disordered solvent water molecule. ; # Attachment 'Rev. complex3.cif' data_cha _database_code_depnum_ccdc_archive 'CCDC 796252' #TrackingRef 'Rev. complex3.cif' _alert_response ; Alert C CHEMW03, PLat 041, 043, 044, 068, Calculated and Reported Values for formula, denisty, molecular mass and F000 value. Response Three water molecule was present as the solvent molecule which was removed using SQUEEZE. Thus six hydrogen atoms and three oxygen atoms of water molecules were added to the chemical formula to adjust the density, molecular mass and F000 value. Results in the chemical_formula_moiety C72 H72 Mn5 N30 O6, 4(Cl O4), 3(H2 O). ; _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety 'C90 H78 Mn5 N48 O6, 4(Cl O4), 3(H2 O)' _chemical_formula_sum 'C90 H84 Cl4 Mn5 N48 O25' _chemical_formula_weight 2654.77 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' Mn Mn 0.3368 0.7283 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting Monoclinic _symmetry_space_group_name_H-M 'P 21/c' _symmetry_space_group_name_Hall '-P 2ybc' loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, y+1/2, -z+1/2' '-x, -y, -z' 'x, -y-1/2, z-1/2' _cell_length_a 15.011(2) _cell_length_b 28.447(4) _cell_length_c 26.921(3) _cell_angle_alpha 90.00 _cell_angle_beta 107.93(1) _cell_angle_gamma 90.00 _cell_volume 10937(3) _cell_formula_units_Z 4 _cell_measurement_temperature 150(2) _cell_measurement_reflns_used 71466 _cell_measurement_theta_min 1.1 _cell_measurement_theta_max 25.5 _exptl_crystal_description Rectangular _exptl_crystal_colour White _exptl_crystal_size_max 0.16 _exptl_crystal_size_mid 0.15 _exptl_crystal_size_min 0.13 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.614 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 5365 _exptl_absorpt_coefficient_mu 0.752 _exptl_absorpt_correction_type Empirical _exptl_absorpt_correction_T_min 0.8668 _exptl_absorpt_correction_T_max 0.8898 _exptl_absorpt_process_details SADABS _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 'omega scans' _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 71466 _diffrn_reflns_av_R_equivalents 0.0810 _diffrn_reflns_av_sigmaI/netI 0.0433 _diffrn_reflns_limit_h_min -18 _diffrn_reflns_limit_h_max 18 _diffrn_reflns_limit_k_min -34 _diffrn_reflns_limit_k_max 34 _diffrn_reflns_limit_l_min -32 _diffrn_reflns_limit_l_max 32 _diffrn_reflns_theta_min 1.07 _diffrn_reflns_theta_max 25.48 _reflns_number_total 20109 _reflns_number_gt 13202 _reflns_threshold_expression >2\s(I) _computing_data_collection 'Bruker SMART' _computing_cell_refinement 'Bruker SMART' _computing_data_reduction 'Bruker SAINT' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'Ortep-3 for Windows (Farrugia, 1997)' _computing_publication_material 'WINGX V1.80.05' _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^ > 2\s(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^)+(0.0825P)^2^+57.0932P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment constr _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 20109 _refine_ls_number_parameters 1528 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0790 _refine_ls_R_factor_gt 0.0665 _refine_ls_wR_factor_ref 0.1819 _refine_ls_wR_factor_gt 0.1726 _refine_ls_goodness_of_fit_ref 1.127 _refine_ls_restrained_S_all 1.127 _refine_ls_shift/su_max 0.004 _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 0.18750(9) 0.22974(5) 0.29575(5) 0.0283(4) Uani 1 1 d . . . Mn2 Mn 0.45742(8) 0.19217(4) 0.34781(5) 0.0276(4) Uani 1 1 d . . . Mn3 Mn 0.33067(9) 0.07912(5) 0.36370(5) 0.0337(4) Uani 1 1 d . . . Mn4 Mn 0.13080(9) 0.10166(5) 0.23493(5) 0.0316(4) Uani 1 1 d . . . Mn5 Mn 0.34651(9) 0.14808(5) 0.19819(5) 0.0355(4) Uani 1 1 d . . . Cl2 Cl 0.0214(2) 0.33503(12) 0.03361(11) 0.0654(9) Uani 1 1 d . . . Cl1 Cl -0.0735(2) 0.34858(11) 0.39869(15) 0.0773(10) Uani 1 1 d . . . Cl3 Cl 0.3527(2) 0.43326(11) 0.24775(16) 0.0789(10) Uani 1 1 d . . . O4 O 0.2026(4) 0.1518(2) 0.1984(2) 0.0325(15) Uani 1 1 d . . . O1 O 0.3330(4) 0.2285(2) 0.2961(2) 0.0307(14) Uani 1 1 d . . . O5 O 0.1397(4) 0.15633(19) 0.2932(2) 0.0290(14) Uani 1 1 d . . . O6 O 0.4376(4) 0.1438(2) 0.2799(2) 0.0355(15) Uani 1 1 d . . . O2 O 0.3630(4) 0.15295(19) 0.3775(2) 0.0269(14) Uani 1 1 d . . . O3 O 0.2633(4) 0.0722(2) 0.2808(2) 0.0328(15) Uani 1 1 d . . . N23 N 0.1286(6) 0.0254(3) 0.1369(3) 0.0358(19) Uani 1 1 d . . . N12 N 0.2656(6) 0.1033(3) 0.4202(3) 0.039(2) Uani 1 1 d . . . N31 N -0.0802(5) 0.1497(3) 0.1620(3) 0.0330(19) Uani 1 1 d . . . N4 N 0.2014(5) 0.2770(2) 0.2362(3) 0.0286(18) Uani 1 1 d . . . N6 N 0.5160(6) 0.2456(3) 0.3038(3) 0.0337(19) Uani 1 1 d . . . N7 N 0.5982(5) 0.2610(3) 0.2995(3) 0.0320(19) Uani 1 1 d . . . N47 N 0.6547(5) 0.1312(3) 0.4135(3) 0.0334(19) Uani 1 1 d . . . N37 N 0.0845(5) 0.1770(3) 0.3612(3) 0.0311(18) Uani 1 1 d . . . N35 N 0.1117(5) 0.2382(3) 0.4392(3) 0.044(2) Uani 1 1 d . . . H35A H 0.0872 0.2115 0.4421 0.053 Uiso 1 1 calc R . . H35B H 0.1191 0.2590 0.4633 0.053 Uiso 1 1 calc R . . N14 N 0.4330(5) 0.2382(3) 0.4138(3) 0.040(2) Uani 1 1 d . . . O16 O -0.0204(5) 0.3516(3) -0.0173(3) 0.068(2) Uani 1 1 d . . . N39 N 0.0017(6) 0.0338(3) 0.2931(3) 0.043(2) Uani 1 1 d . . . N29 N 0.1807(5) 0.2090(3) 0.1336(3) 0.0312(18) Uani 1 1 d . . . N20 N 0.4092(6) 0.0299(2) 0.3346(3) 0.042(2) Uani 1 1 d . . . N30 N 0.0151(5) 0.1446(2) 0.1788(3) 0.0317(19) Uani 1 1 d . . . N1 N 0.0384(5) 0.2585(3) 0.2431(3) 0.040(2) Uani 1 1 d . . . N33 N 0.2144(5) 0.2970(3) 0.3511(3) 0.0292(18) Uani 1 1 d . . . N28 N 0.2795(6) 0.2054(3) 0.1484(3) 0.040(2) Uani 1 1 d . . . N41 N 0.3012(6) 0.1027(3) 0.1180(3) 0.041(2) Uani 1 1 d . . . N44 N 0.4408(5) 0.0897(3) 0.2036(3) 0.040(2) Uani 1 1 d . . . N45 N 0.5150(5) 0.0837(3) 0.2493(3) 0.046(2) Uani 1 1 d . . . N5 N 0.2905(5) 0.2886(2) 0.2350(3) 0.0290(18) Uani 1 1 d . . . N36 N 0.1307(5) 0.2193(3) 0.3588(3) 0.0289(18) Uani 1 1 d . . . N46 N 0.5780(5) 0.1415(3) 0.3712(3) 0.0333(19) Uani 1 1 d . . . N27 N 0.2773(6) 0.2708(3) 0.0967(3) 0.066(3) Uani 1 1 d . . . H27A H 0.2178 0.2746 0.0895 0.079 Uiso 1 1 calc R . . H27B H 0.3095 0.2897 0.0841 0.079 Uiso 1 1 calc R . . N25 N 0.4562(6) 0.1955(3) 0.1747(4) 0.056(2) Uani 1 1 d . . . C52 C 0.0487(6) 0.1770(3) 0.1529(3) 0.023(2) Uani 1 1 d . . . N15 N 0.4591(5) 0.2791(3) 0.4403(3) 0.039(2) Uani 1 1 d . . . N24 N 0.0266(6) 0.0794(3) 0.0849(3) 0.047(2) Uani 1 1 d . . . N13 N 0.2877(5) 0.1479(3) 0.4405(3) 0.040(2) Uani 1 1 d . . . N2 N -0.1232(7) 0.3041(4) 0.1852(4) 0.064(3) Uani 1 1 d . . . N22 N 0.1637(6) 0.0450(2) 0.1847(3) 0.0364(19) Uani 1 1 d . . . N21 N 0.3716(6) 0.0132(3) 0.2830(3) 0.046(2) Uani 1 1 d . . . C67 C 0.0430(6) 0.1041(3) 0.3237(4) 0.030(2) Uani 1 1 d . . . C86 C 0.6673(7) 0.1526(3) 0.4612(4) 0.036(2) Uani 1 1 d . . . C11 C 0.6820(7) 0.2416(3) 0.3278(4) 0.038(3) Uani 1 1 d . . . C56 C -0.1356(7) 0.1232(4) 0.1827(3) 0.036(2) Uani 1 1 d . . . C65 C 0.1379(6) 0.2474(3) 0.3978(4) 0.031(2) Uani 1 1 d . . . C64 C 0.1803(6) 0.2929(3) 0.3925(3) 0.036(3) Uani 1 1 d . . . C76 C 0.2289(7) 0.1097(3) 0.0737(4) 0.040(3) Uani 1 1 d . . . H76 H 0.1840 0.1320 0.0746 0.048 Uiso 1 1 calc R . . C3 C -0.0378(8) 0.3149(4) 0.1794(4) 0.050(3) Uani 1 1 d . . . H3 H -0.0340 0.3379 0.1557 0.060 Uiso 1 1 calc R . . C69 C -0.0369(6) 0.0411(4) 0.3322(5) 0.046(3) Uani 1 1 d . . . N3 N 0.1463(5) 0.3352(3) 0.1725(3) 0.047(2) Uani 1 1 d . . . H3A H 0.2015 0.3418 0.1713 0.057 Uiso 1 1 calc R . . H3B H 0.0985 0.3501 0.1529 0.057 Uiso 1 1 calc R . . C7 C 0.4477(7) 0.2704(3) 0.2703(3) 0.033(2) Uani 1 1 d . . . N42 N 0.2808(8) 0.0530(3) 0.0269(3) 0.065(3) Uani 1 1 d . . . N38 N 0.0510(5) 0.0725(3) 0.2880(3) 0.038(2) Uani 1 1 d . . . C79 C 0.3671(7) 0.0688(3) 0.1170(4) 0.041(3) Uani 1 1 d . . . N34 N 0.2261(6) 0.3718(3) 0.4202(3) 0.057(2) Uani 1 1 d . . . C66 C 0.0916(6) 0.1488(3) 0.3263(3) 0.024(2) Uani 1 1 d . . . C77 C 0.2178(7) 0.0867(4) 0.0289(4) 0.047(3) Uani 1 1 d . . . H77 H 0.1677 0.0937 -0.0005 0.056 Uiso 1 1 calc R . . C6 C 0.3518(6) 0.2613(3) 0.2675(3) 0.027(2) Uani 1 1 d . . . C54 C -0.1040(7) 0.1853(3) 0.1260(3) 0.037(2) Uani 1 1 d . . . O14 O 0.3366(6) 0.4815(3) 0.2385(4) 0.097(3) Uani 1 1 d . . . N9 N 0.2398(6) 0.0186(3) 0.3837(3) 0.056(3) Uani 1 1 d . . . C5 C 0.1349(7) 0.3022(3) 0.2045(4) 0.032(2) Uani 1 1 d . . . N17 N 0.4654(5) 0.0573(3) 0.4305(3) 0.038(2) Uani 1 1 d . . . C26 C 0.5199(7) 0.3090(4) 0.4266(5) 0.051(3) Uani 1 1 d . . . C51 C 0.1498(6) 0.1802(3) 0.1623(3) 0.032(2) Uani 1 1 d . . . C71 C 0.0035(8) -0.0071(4) 0.2663(4) 0.051(3) Uani 1 1 d . . . C78 C 0.3581(8) 0.0446(4) 0.0717(4) 0.054(3) Uani 1 1 d . . . H78 H 0.4031 0.0225 0.0705 0.065 Uiso 1 1 calc R . . C41 C 0.0401(8) 0.0358(4) 0.1054(4) 0.045(3) Uani 1 1 d . . . C22 C 0.3724(6) 0.2164(4) 0.4355(4) 0.037(2) Uani 1 1 d . . . C45 C -0.0624(10) 0.0899(5) 0.0543(4) 0.070(4) Uani 1 1 d . . . H45 H -0.0732 0.1195 0.0391 0.084 Uiso 1 1 calc R . . N18 N 0.6323(7) 0.0272(4) 0.5027(4) 0.068(3) Uani 1 1 d . . . C82 C 0.5797(6) 0.1112(3) 0.3326(4) 0.033(2) Uani 1 1 d . . . C83 C 0.6577(7) 0.0820(4) 0.3510(4) 0.046(3) Uani 1 1 d . . . H83 H 0.6750 0.0582 0.3322 0.056 Uiso 1 1 calc R . . O7 O -0.0053(5) 0.3849(3) 0.4137(4) 0.097(3) Uani 1 1 d . . . C53 C -0.0230(7) 0.2018(3) 0.1204(3) 0.035(2) Uani 1 1 d . . . H53 H -0.0175 0.2259 0.0982 0.042 Uiso 1 1 calc R . . C35 C 0.4864(8) 0.0105(4) 0.3623(4) 0.054(3) Uani 1 1 d . . . C68 C -0.0110(6) 0.0848(4) 0.3509(4) 0.044(3) Uani 1 1 d . . . H68 H -0.0273 0.0993 0.3779 0.053 Uiso 1 1 calc R . . N11 N 0.1697(6) 0.0947(4) 0.4711(4) 0.078(3) Uani 1 1 d . . . H11A H 0.1809 0.1227 0.4837 0.094 Uiso 1 1 calc R . . H11B H 0.1323 0.0766 0.4808 0.094 Uiso 1 1 calc R . . C81 C 0.5069(7) 0.1131(4) 0.2851(4) 0.042(3) Uani 1 1 d . . . N16 N 0.6064(8) 0.3136(4) 0.4638(4) 0.081(3) Uani 1 1 d . . . N48 N 0.5866(6) 0.1681(3) 0.4693(3) 0.050(2) Uani 1 1 d . . . C87 C 0.7529(7) 0.1567(4) 0.5001(4) 0.049(3) Uani 1 1 d . . . H87 H 0.8076 0.1464 0.4943 0.059 Uiso 1 1 calc R . . O8 O -0.0921(6) 0.3296(3) 0.4442(4) 0.092(3) Uani 1 1 d . . . O9 O -0.0384(7) 0.3124(3) 0.3728(4) 0.111(3) Uani 1 1 d . . . C8C C 0.4884(7) 0.3023(3) 0.2457(4) 0.044(3) Uani 1 1 d . . . H8C H 0.4570 0.3243 0.2211 0.052 Uiso 1 1 calc R . . C31 C 0.4918(7) 0.0730(3) 0.4797(4) 0.044(3) Uani 1 1 d . . . H31 H 0.4536 0.0943 0.4898 0.053 Uiso 1 1 calc R . . C61 C 0.2546(7) 0.3383(4) 0.3457(4) 0.041(3) Uani 1 1 d . . . H61 H 0.2787 0.3419 0.3180 0.049 Uiso 1 1 calc R . . C36 C 0.2975(7) 0.0372(3) 0.2601(4) 0.037(2) Uani 1 1 d . . . O12 O 0.4472(7) 0.4252(3) 0.2509(4) 0.121(4) Uani 1 1 d . . . C2 C -0.1254(8) 0.2703(4) 0.2204(4) 0.062(3) Uani 1 1 d . . . H2 H -0.1823 0.2619 0.2249 0.074 Uiso 1 1 calc R . . C39 C 0.1889(8) -0.0061(3) 0.1293(4) 0.043(3) Uani 1 1 d . . . C4 C 0.0415(6) 0.2924(3) 0.2080(3) 0.031(2) Uani 1 1 d . . . C38 C 0.2625(7) -0.0079(4) 0.1731(4) 0.049(3) Uani 1 1 d . . . H38 H 0.3142 -0.0275 0.1789 0.059 Uiso 1 1 calc R . . C9 C 0.5826(7) 0.2960(3) 0.2635(4) 0.038(2) Uani 1 1 d . . . C24 C 0.4180(8) 0.2825(4) 0.4786(4) 0.048(3) Uani 1 1 d . . . O17 O 0.1173(6) 0.3285(5) 0.0416(3) 0.138(5) Uani 1 1 d . . . C21 C 0.3375(6) 0.1701(4) 0.4169(3) 0.033(2) Uani 1 1 d . . . C23 C 0.3646(7) 0.2436(4) 0.4752(4) 0.042(3) Uani 1 1 d . . . H23 H 0.3283 0.2366 0.4967 0.050 Uiso 1 1 calc R . . O15 O 0.0032(6) 0.3656(3) 0.0701(3) 0.100(3) Uani 1 1 d . . . C34 C 0.5227(7) 0.0256(3) 0.4164(4) 0.044(3) Uani 1 1 d . . . C27 C 0.4973(7) 0.3297(4) 0.3804(4) 0.045(3) Uani 1 1 d . . . H27 H 0.4379 0.3254 0.3568 0.054 Uiso 1 1 calc R . . C13 C 0.8002(10) 0.2262(4) 0.4081(5) 0.069(3) Uani 1 1 d . . . H13 H 0.8229 0.2286 0.4443 0.083 Uiso 1 1 calc R . . C63 C 0.1846(7) 0.3302(4) 0.4256(4) 0.053(3) Uani 1 1 d . . . H63 H 0.1583 0.3271 0.4525 0.064 Uiso 1 1 calc R . . N40 N 0.0824(7) -0.0186(3) 0.2537(4) 0.062(3) Uani 1 1 d . . . O10 O -0.1556(7) 0.3658(3) 0.3625(4) 0.114(4) Uani 1 1 d . . . N26 N 0.5735(8) 0.2491(5) 0.1360(4) 0.094(4) Uani 1 1 d . . . C1 C -0.0463(8) 0.2488(4) 0.2488(4) 0.061(3) Uani 1 1 d . . . H1 H -0.0498 0.2265 0.2733 0.073 Uiso 1 1 calc R . . C12 C 0.7127(8) 0.2437(4) 0.3808(5) 0.063(3) Uani 1 1 d . . . H12 H 0.6750 0.2570 0.3988 0.075 Uiso 1 1 calc R . . N8 N 0.7360(7) 0.2216(3) 0.3008(3) 0.063(3) Uani 1 1 d . . . C50 C 0.3194(8) 0.2355(4) 0.1275(4) 0.047(3) Uani 1 1 d . . . C85 C 0.7898(7) 0.0719(4) 0.4401(4) 0.061(3) Uani 1 1 d . . . H85A H 0.7803 0.0385 0.4409 0.091 Uiso 1 1 calc R . . H85B H 0.7989 0.0847 0.4743 0.091 Uiso 1 1 calc R . . H85C H 0.8441 0.0781 0.4295 0.091 Uiso 1 1 calc R . . C37 C 0.2480(7) 0.0238(3) 0.2070(4) 0.034(2) Uani 1 1 d . . . C40 C 0.1683(8) -0.0323(4) 0.0776(4) 0.060(3) Uani 1 1 d . . . H40A H 0.1497 -0.0102 0.0493 0.090 Uiso 1 1 calc R . . H40B H 0.1188 -0.0545 0.0746 0.090 Uiso 1 1 calc R . . H40C H 0.2236 -0.0486 0.0764 0.090 Uiso 1 1 calc R . . C59 C -0.2564(7) 0.0764(5) 0.2230(4) 0.059(3) Uani 1 1 d . . . H59 H -0.2986 0.0612 0.2366 0.071 Uiso 1 1 calc R . . N19 N 0.5317(7) -0.0226(3) 0.3450(4) 0.082(3) Uani 1 1 d . . . H19A H 0.5099 -0.0326 0.3135 0.098 Uiso 1 1 calc R . . H19B H 0.5829 -0.0341 0.3655 0.098 Uiso 1 1 calc R . . C57 C -0.1550(13) 0.0774(6) 0.1716(6) 0.117(6) Uani 1 1 d . . . H57 H -0.1277 0.0623 0.1493 0.140 Uiso 1 1 calc R . . C33 C 0.6035(8) 0.0112(4) 0.4524(4) 0.059(3) Uani 1 1 d . . . H33 H 0.6408 -0.0105 0.4422 0.071 Uiso 1 1 calc R . . C14 C 0.8526(7) 0.2053(4) 0.3809(6) 0.066(4) Uani 1 1 d . . . H14 H 0.9106 0.1924 0.3987 0.080 Uiso 1 1 calc R . . C88 C 0.7560(8) 0.1760(3) 0.5466(4) 0.052(3) Uani 1 1 d . . . H88 H 0.8132 0.1789 0.5727 0.062 Uiso 1 1 calc R . . C42 C -0.0317(9) 0.0034(4) 0.0958(4) 0.059(3) Uani 1 1 d . . . H42 H -0.0207 -0.0266 0.1100 0.071 Uiso 1 1 calc R . . C84 C 0.7045(7) 0.0945(3) 0.4017(4) 0.044(3) Uani 1 1 d . . . C20 C 0.2109(7) 0.0792(5) 0.4360(4) 0.048(3) Uani 1 1 d . . . C32 C 0.5744(9) 0.0585(4) 0.5159(5) 0.064(3) Uani 1 1 d . . . H32 H 0.5906 0.0702 0.5498 0.077 Uiso 1 1 calc R . . C80 C 0.4402(6) 0.0621(4) 0.1667(4) 0.042(3) Uani 1 1 d . . . C46 C 0.5493(8) 0.1869(4) 0.1894(4) 0.063(3) Uani 1 1 d . . . H46 H 0.5735 0.1627 0.2128 0.076 Uiso 1 1 calc R . . C25 C 0.4344(8) 0.3261(4) 0.5127(4) 0.065(3) Uani 1 1 d . . . H25A H 0.3777 0.3342 0.5201 0.097 Uiso 1 1 calc R . . H25B H 0.4528 0.3517 0.4948 0.097 Uiso 1 1 calc R . . H25C H 0.4830 0.3200 0.5448 0.097 Uiso 1 1 calc R . . C43 C -0.1206(9) 0.0164(5) 0.0645(5) 0.071(4) Uani 1 1 d . . . H43 H -0.1695 -0.0052 0.0572 0.085 Uiso 1 1 calc R . . C89 C 0.6762(7) 0.1911(4) 0.5558(4) 0.048(3) Uani 1 1 d . . . H89 H 0.6785 0.2040 0.5879 0.057 Uiso 1 1 calc R . . C10 C 0.6598(7) 0.3228(4) 0.2513(4) 0.064(3) Uani 1 1 d . . . H10A H 0.6888 0.3031 0.2317 0.096 Uiso 1 1 calc R . . H10B H 0.7058 0.3321 0.2833 0.096 Uiso 1 1 calc R . . H10C H 0.6343 0.3502 0.2311 0.096 Uiso 1 1 calc R . . C75 C 0.0811(12) -0.0596(6) 0.2279(5) 0.087(4) Uani 1 1 d . . . H75 H 0.1344 -0.0665 0.2186 0.104 Uiso 1 1 calc R . . C90 C 0.5929(7) 0.1871(4) 0.5169(4) 0.051(3) Uani 1 1 d . . . H90 H 0.5386 0.1975 0.5231 0.061 Uiso 1 1 calc R . . C30 C 0.6709(10) 0.3429(6) 0.4499(7) 0.099(5) Uani 1 1 d . . . H30 H 0.7297 0.3482 0.4737 0.119 Uiso 1 1 calc R . . C62 C 0.2612(7) 0.3746(4) 0.3786(4) 0.054(3) Uani 1 1 d . . . H62 H 0.2902 0.4022 0.3733 0.065 Uiso 1 1 calc R . . C44 C -0.1356(9) 0.0599(5) 0.0449(4) 0.063(3) Uani 1 1 d . . . H44 H -0.1953 0.0693 0.0252 0.076 Uiso 1 1 calc R . . C58 C -0.2135(12) 0.0522(5) 0.1919(6) 0.111(6) Uani 1 1 d . . . H58 H -0.2240 0.0203 0.1852 0.134 Uiso 1 1 calc R . . C15 C 0.8212(9) 0.2033(4) 0.3286(6) 0.070(3) Uani 1 1 d . . . H15 H 0.8580 0.1890 0.3108 0.083 Uiso 1 1 calc R . . N32 N -0.1765(8) 0.1455(4) 0.2144(4) 0.088(3) Uani 1 1 d . . . C72 C -0.0730(9) -0.0380(5) 0.2519(5) 0.080(4) Uani 1 1 d . . . H72 H -0.1289 -0.0309 0.2583 0.097 Uiso 1 1 calc R . . C47 C 0.6082(9) 0.2125(6) 0.1710(5) 0.082(4) Uani 1 1 d . . . H47 H 0.6719 0.2056 0.1817 0.099 Uiso 1 1 calc R . . C70 C -0.0933(8) 0.0058(4) 0.3507(5) 0.071(3) Uani 1 1 d . . . H70A H -0.0586 -0.0229 0.3594 0.107 Uiso 1 1 calc R . . H70B H -0.1510 0.0000 0.3236 0.107 Uiso 1 1 calc R . . H70C H -0.1065 0.0178 0.3811 0.107 Uiso 1 1 calc R . . C28 C 0.5591(13) 0.3566(5) 0.3676(6) 0.088(4) Uani 1 1 d . . . H28 H 0.5426 0.3710 0.3350 0.105 Uiso 1 1 calc R . . C55 C -0.2034(7) 0.1980(4) 0.1005(4) 0.061(3) Uani 1 1 d . . . H55A H -0.2076 0.2202 0.0731 0.092 Uiso 1 1 calc R . . H55B H -0.2287 0.2117 0.1259 0.092 Uiso 1 1 calc R . . H55C H -0.2384 0.1703 0.0862 0.092 Uiso 1 1 calc R . . C74 C 0.0123(16) -0.0911(6) 0.2144(6) 0.107(6) Uani 1 1 d . . . H74 H 0.0160 -0.1189 0.1971 0.128 Uiso 1 1 calc R . . C49 C 0.4211(8) 0.2314(5) 0.1408(4) 0.055(3) Uani 1 1 d . . . O11 O 0.3367(13) 0.4190(5) 0.2916(7) 0.217(8) Uani 1 1 d . . . C60 C -0.2364(10) 0.1215(5) 0.2331(6) 0.102(5) Uani 1 1 d . . . H60 H -0.2654 0.1373 0.2542 0.123 Uiso 1 1 calc R . . C16 C 0.2305(9) -0.0259(5) 0.3665(5) 0.077(4) Uani 1 1 d . . . H16 H 0.2622 -0.0347 0.3433 0.092 Uiso 1 1 calc R . . O13 O 0.3017(11) 0.4075(4) 0.2046(6) 0.206(8) Uani 1 1 d . . . C48 C 0.4793(10) 0.2570(5) 0.1217(4) 0.088(4) Uani 1 1 d . . . H48 H 0.4541 0.2810 0.0980 0.106 Uiso 1 1 calc R . . C29 C 0.6477(13) 0.3634(5) 0.4022(8) 0.098(5) Uani 1 1 d . . . H29 H 0.6910 0.3819 0.3928 0.117 Uiso 1 1 calc R . . O18 O -0.0238(11) 0.2908(4) 0.0379(5) 0.175(6) Uani 1 1 d . . . C19 C 0.1951(7) 0.0318(5) 0.4185(5) 0.057(4) Uani 1 1 d . . . N10 N 0.1346(9) -0.0463(7) 0.4153(8) 0.131(8) Uani 1 1 d . . . C18 C 0.1436(10) 0.0002(6) 0.4336(6) 0.101(5) Uani 1 1 d . . . H18 H 0.1125 0.0092 0.4571 0.121 Uiso 1 1 calc R . . C73 C -0.0617(16) -0.0789(5) 0.2279(6) 0.113(6) Uani 1 1 d . . . H73 H -0.1111 -0.1002 0.2204 0.136 Uiso 1 1 calc R . . Cl4 Cl 0.5813(6) -0.1279(2) 0.4081(3) 0.174(2) Uani 1 1 d . . . C17 C 0.1782(14) -0.0584(6) 0.3807(8) 0.125(7) Uani 1 1 d . . . H17 H 0.1725 -0.0886 0.3668 0.150 Uiso 1 1 calc R . . O21 O 0.6350(9) -0.1513(5) 0.4470(4) 0.147(5) Uani 1 1 d . . . O20 O 0.6105(19) -0.1380(12) 0.3629(9) 0.372(17) Uani 1 1 d . . . O22 O 0.4861(18) -0.1405(12) 0.4066(16) 0.45(2) Uani 1 1 d . . . O19 O 0.6079(19) -0.0812(6) 0.4255(10) 0.350(16) Uani 1 1 d . . . N43 N 0.5021(6) 0.0266(3) 0.1704(3) 0.066(3) Uani 1 1 d . . . H43A H 0.5455 0.0216 0.1993 0.079 Uiso 1 1 calc R . . H43B H 0.4979 0.0090 0.1438 0.079 Uiso 1 1 calc R . . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 Mn1 0.0236(8) 0.0381(9) 0.0232(8) -0.0010(6) 0.0072(6) -0.0040(6) Mn2 0.0230(8) 0.0367(9) 0.0251(8) 0.0002(6) 0.0103(6) -0.0028(6) Mn3 0.0319(9) 0.0358(9) 0.0276(8) 0.0043(7) 0.0009(7) -0.0047(7) Mn4 0.0324(9) 0.0354(9) 0.0231(8) -0.0014(6) 0.0029(6) -0.0004(7) Mn5 0.0247(8) 0.0516(10) 0.0294(8) -0.0075(7) 0.0070(7) 0.0006(7) Cl2 0.059(2) 0.094(2) 0.048(2) 0.0252(18) 0.0246(15) 0.0351(17) Cl1 0.053(2) 0.061(2) 0.116(3) 0.009(2) 0.025(2) 0.0106(18) Cl3 0.063(2) 0.042(2) 0.129(3) 0.008(2) 0.025(2) -0.0061(17) O4 0.025(4) 0.045(4) 0.028(4) -0.009(3) 0.009(3) -0.005(3) O1 0.029(4) 0.041(4) 0.025(3) 0.010(3) 0.013(3) -0.002(3) O5 0.030(3) 0.036(4) 0.023(3) -0.005(3) 0.010(3) -0.004(3) O6 0.030(4) 0.044(4) 0.032(4) -0.007(3) 0.009(3) 0.000(3) O2 0.025(3) 0.037(4) 0.021(3) -0.006(3) 0.010(3) -0.013(3) O3 0.025(3) 0.037(4) 0.031(4) 0.002(3) 0.000(3) 0.000(3) N23 0.039(6) 0.037(5) 0.023(5) -0.010(4) -0.003(5) 0.007(5) N12 0.036(5) 0.043(6) 0.038(5) 0.014(5) 0.011(4) -0.008(5) N31 0.024(5) 0.053(6) 0.027(5) 0.006(4) 0.015(4) 0.000(4) N4 0.025(5) 0.033(5) 0.029(5) -0.006(4) 0.009(4) 0.003(4) N6 0.030(5) 0.039(5) 0.043(5) -0.002(4) 0.028(5) -0.009(4) N7 0.019(5) 0.048(5) 0.026(5) 0.013(4) 0.004(4) 0.008(4) N47 0.029(5) 0.044(5) 0.025(5) -0.013(4) 0.005(4) 0.007(4) N37 0.032(5) 0.040(5) 0.022(5) -0.005(4) 0.009(4) -0.002(4) N35 0.051(5) 0.062(6) 0.027(5) -0.010(4) 0.022(4) -0.011(4) N14 0.029(5) 0.051(6) 0.037(5) -0.014(5) 0.005(4) 0.004(4) O16 0.062(5) 0.097(6) 0.041(5) 0.030(4) 0.011(4) -0.010(4) N39 0.051(6) 0.025(6) 0.050(6) -0.006(5) 0.011(5) -0.011(5) N29 0.035(6) 0.040(5) 0.021(4) 0.007(4) 0.012(4) 0.005(4) N20 0.044(6) 0.030(5) 0.041(6) 0.002(4) -0.003(5) 0.007(4) N30 0.037(6) 0.035(5) 0.022(4) -0.003(4) 0.007(4) 0.000(4) N1 0.035(6) 0.045(5) 0.037(5) -0.004(4) 0.007(4) 0.003(4) N33 0.025(4) 0.037(5) 0.031(5) -0.006(4) 0.015(4) -0.001(4) N28 0.042(6) 0.060(6) 0.019(4) 0.002(4) 0.012(4) 0.005(5) N41 0.043(5) 0.040(5) 0.041(6) -0.006(4) 0.014(5) -0.003(4) N44 0.033(5) 0.064(6) 0.022(5) -0.028(5) 0.008(5) -0.002(4) N45 0.026(5) 0.074(6) 0.031(5) -0.024(5) -0.003(5) 0.005(4) N5 0.022(5) 0.038(5) 0.028(5) -0.002(4) 0.008(4) 0.004(4) N36 0.028(4) 0.030(5) 0.030(5) -0.011(4) 0.011(4) -0.017(4) N46 0.017(5) 0.046(5) 0.030(5) -0.002(4) -0.005(4) -0.002(4) N27 0.065(6) 0.091(7) 0.047(6) 0.018(6) 0.024(5) -0.039(6) N25 0.036(7) 0.081(7) 0.060(6) -0.029(6) 0.028(5) -0.016(5) C52 0.022(6) 0.023(5) 0.020(5) 0.000(4) -0.002(5) 0.003(5) N15 0.023(5) 0.056(6) 0.038(5) -0.013(5) 0.012(4) -0.016(4) N24 0.053(7) 0.055(7) 0.024(5) -0.004(4) 0.001(5) 0.010(5) N13 0.025(5) 0.068(7) 0.031(5) 0.014(5) 0.015(4) -0.005(4) N2 0.053(7) 0.080(7) 0.063(7) 0.005(6) 0.022(5) 0.017(5) N22 0.043(6) 0.037(5) 0.023(5) -0.006(4) 0.000(4) 0.002(4) N21 0.046(6) 0.053(6) 0.029(5) -0.008(4) -0.002(4) 0.007(5) C67 0.039(6) 0.018(6) 0.022(6) -0.002(5) -0.007(5) -0.008(5) C86 0.031(7) 0.038(6) 0.038(7) 0.006(5) 0.010(6) 0.005(5) C11 0.052(8) 0.036(6) 0.032(7) -0.001(5) 0.023(7) -0.011(6) C56 0.034(6) 0.053(8) 0.024(6) -0.003(5) 0.011(5) -0.002(6) C65 0.027(6) 0.039(7) 0.029(6) -0.012(6) 0.011(5) -0.017(5) C64 0.025(5) 0.055(8) 0.023(6) -0.024(6) 0.003(5) 0.006(5) C76 0.038(7) 0.054(7) 0.024(6) -0.001(6) 0.003(6) -0.011(5) C3 0.039(7) 0.059(7) 0.048(7) -0.011(6) 0.006(6) -0.001(6) C69 0.026(6) 0.035(8) 0.070(8) 0.012(6) 0.003(6) -0.011(5) N3 0.036(5) 0.046(5) 0.052(5) 0.040(5) 0.003(4) -0.002(4) C7 0.032(7) 0.048(6) 0.021(5) 0.013(5) 0.014(5) 0.010(6) N42 0.099(8) 0.068(7) 0.020(5) -0.003(5) 0.006(6) -0.025(6) N38 0.028(5) 0.029(5) 0.044(5) 0.015(5) -0.008(4) -0.018(4) C79 0.057(7) 0.046(7) 0.028(7) -0.021(5) 0.026(6) -0.003(6) N34 0.051(6) 0.073(7) 0.056(6) -0.028(5) 0.031(5) -0.007(5) C66 0.033(6) 0.024(6) 0.014(5) -0.009(5) 0.005(5) 0.000(5) C77 0.048(7) 0.040(7) 0.046(8) -0.009(6) 0.005(5) -0.001(6) C6 0.026(7) 0.039(6) 0.016(5) -0.005(5) 0.010(5) 0.006(5) C54 0.037(7) 0.051(7) 0.028(6) 0.016(5) 0.015(5) 0.017(6) O14 0.105(7) 0.044(6) 0.151(8) 0.001(5) 0.051(6) 0.004(5) N9 0.049(6) 0.058(8) 0.040(6) 0.022(5) -0.018(5) -0.026(5) C5 0.024(7) 0.038(6) 0.030(6) -0.005(5) 0.002(5) 0.000(5) N17 0.034(5) 0.045(5) 0.023(5) 0.006(4) -0.009(4) -0.005(4) C26 0.032(8) 0.064(8) 0.046(8) -0.020(7) -0.005(7) 0.002(6) C51 0.029(7) 0.041(6) 0.014(5) -0.004(5) -0.010(5) 0.011(5) C71 0.041(8) 0.050(8) 0.048(7) 0.012(6) -0.005(6) -0.019(7) C78 0.069(8) 0.065(8) 0.032(7) -0.004(6) 0.023(6) 0.002(6) C41 0.046(8) 0.053(8) 0.033(6) -0.019(6) 0.008(6) -0.002(7) C22 0.026(6) 0.061(8) 0.027(6) -0.005(6) 0.015(5) 0.004(5) C45 0.069(10) 0.098(10) 0.038(7) -0.012(7) 0.011(7) 0.019(9) N18 0.080(7) 0.069(7) 0.042(7) 0.007(5) -0.004(6) -0.007(6) C82 0.024(6) 0.043(6) 0.031(7) -0.015(5) 0.006(6) 0.010(5) C83 0.036(7) 0.055(7) 0.045(7) -0.025(6) 0.008(6) 0.000(6) O7 0.059(5) 0.064(6) 0.166(9) 0.012(6) 0.033(6) -0.022(5) C53 0.048(7) 0.038(6) 0.026(6) 0.016(5) 0.020(6) 0.009(6) C35 0.049(8) 0.059(8) 0.044(8) 0.003(6) -0.002(7) 0.018(7) C68 0.032(6) 0.058(9) 0.046(6) 0.022(6) 0.016(5) 0.001(6) N11 0.037(6) 0.118(9) 0.088(8) 0.052(7) 0.031(6) 0.019(6) C81 0.038(7) 0.050(7) 0.031(7) -0.010(6) -0.001(6) -0.012(6) N16 0.072(8) 0.074(7) 0.096(8) -0.022(6) 0.023(8) -0.014(6) N48 0.042(6) 0.059(6) 0.047(6) -0.012(5) 0.011(4) -0.004(5) C87 0.038(7) 0.066(8) 0.036(7) -0.013(6) 0.000(6) 0.017(5) O8 0.073(6) 0.102(7) 0.095(7) 0.005(6) 0.017(5) -0.025(5) O9 0.105(7) 0.065(6) 0.180(10) -0.005(6) 0.070(7) 0.008(5) C8C 0.038(8) 0.054(7) 0.039(6) 0.016(5) 0.013(6) 0.008(6) C31 0.034(7) 0.047(7) 0.041(7) 0.018(6) -0.004(6) -0.001(5) C61 0.046(7) 0.043(7) 0.033(6) -0.013(6) 0.010(5) -0.002(6) C36 0.033(7) 0.035(6) 0.037(7) -0.002(6) 0.002(6) 0.005(6) O12 0.102(8) 0.084(7) 0.172(10) 0.046(7) 0.037(7) 0.031(6) C2 0.031(8) 0.094(9) 0.062(8) 0.006(7) 0.017(6) -0.002(7) C39 0.062(8) 0.035(7) 0.028(7) -0.004(5) 0.010(7) -0.008(6) C4 0.029(7) 0.040(6) 0.018(5) 0.008(5) 0.000(5) 0.009(5) C38 0.044(7) 0.051(7) 0.042(7) -0.001(6) -0.002(7) -0.005(5) C9 0.033(7) 0.045(7) 0.038(6) 0.015(5) 0.013(5) 0.003(5) C24 0.057(7) 0.053(8) 0.042(7) -0.009(6) 0.028(6) 0.004(6) O17 0.061(6) 0.288(15) 0.071(6) 0.034(7) 0.029(5) 0.093(8) C21 0.022(5) 0.055(8) 0.018(6) -0.001(5) 0.003(5) 0.001(5) C23 0.041(6) 0.063(8) 0.026(6) -0.010(6) 0.018(5) -0.012(6) O15 0.120(8) 0.135(8) 0.048(5) -0.011(5) 0.028(5) 0.044(6) C34 0.036(7) 0.033(6) 0.055(8) 0.008(6) 0.001(7) 0.011(5) C27 0.037(7) 0.056(7) 0.036(8) -0.004(6) 0.003(6) -0.009(6) C13 0.073(10) 0.075(9) 0.061(8) 0.005(7) 0.020(8) -0.010(7) C63 0.053(7) 0.068(8) 0.049(7) -0.012(7) 0.030(6) -0.018(6) N40 0.069(8) 0.048(7) 0.061(6) 0.016(5) 0.007(5) 0.002(5) O10 0.093(7) 0.104(7) 0.099(7) 0.017(6) -0.039(6) -0.041(6) N26 0.061(9) 0.164(12) 0.069(8) -0.009(8) 0.037(6) -0.029(8) C1 0.030(7) 0.081(9) 0.075(8) 0.021(7) 0.020(7) 0.013(7) C12 0.059(9) 0.072(8) 0.061(9) 0.009(6) 0.023(7) 0.039(7) N8 0.059(7) 0.080(7) 0.057(6) 0.010(5) 0.026(6) 0.017(6) C50 0.052(9) 0.079(9) 0.008(6) 0.009(6) 0.006(6) -0.011(7) C85 0.058(8) 0.064(8) 0.054(7) -0.003(6) 0.007(6) 0.025(6) C37 0.051(8) 0.024(6) 0.023(6) -0.009(5) 0.006(6) -0.002(5) C40 0.069(8) 0.058(7) 0.046(7) -0.006(6) 0.007(6) -0.004(6) C59 0.038(7) 0.081(11) 0.053(8) 0.013(7) 0.006(6) -0.008(7) N19 0.071(7) 0.074(7) 0.071(7) -0.013(6) -0.021(6) 0.045(6) C57 0.195(18) 0.087(12) 0.109(12) -0.035(10) 0.105(13) -0.048(12) C33 0.054(8) 0.056(7) 0.052(8) 0.001(6) -0.006(7) 0.017(6) C14 0.015(6) 0.107(10) 0.071(10) 0.032(8) 0.003(7) 0.001(6) C88 0.049(8) 0.059(7) 0.038(7) -0.015(6) -0.002(5) 0.015(6) C42 0.072(9) 0.056(8) 0.040(7) -0.018(6) 0.006(7) -0.010(8) C84 0.042(6) 0.037(6) 0.045(7) -0.010(5) 0.003(6) 0.006(6) C20 0.025(6) 0.068(10) 0.054(8) 0.036(7) 0.016(6) -0.007(7) C32 0.077(10) 0.052(8) 0.057(8) -0.003(6) 0.011(8) -0.013(7) C80 0.025(6) 0.052(7) 0.038(7) -0.005(6) -0.006(5) 0.011(5) C46 0.040(8) 0.099(9) 0.060(8) -0.013(7) 0.028(7) -0.015(7) C25 0.068(8) 0.068(8) 0.059(7) -0.035(7) 0.019(6) -0.001(6) C43 0.064(10) 0.089(12) 0.049(8) -0.024(8) 0.001(7) -0.010(8) C89 0.045(7) 0.067(7) 0.029(6) -0.021(5) 0.007(6) 0.002(6) C10 0.046(7) 0.065(8) 0.087(9) 0.022(7) 0.027(6) -0.004(6) C75 0.139(14) 0.064(10) 0.051(8) 0.001(8) 0.019(8) -0.009(10) C90 0.041(7) 0.069(8) 0.042(7) -0.018(6) 0.012(6) 0.009(6) C30 0.075(10) 0.124(13) 0.109(14) -0.052(11) 0.043(10) -0.047(10) C62 0.037(7) 0.071(8) 0.062(8) -0.013(7) 0.026(6) -0.010(6) C44 0.057(9) 0.085(10) 0.033(7) -0.023(7) -0.008(6) 0.030(9) C58 0.159(15) 0.083(11) 0.103(12) -0.016(10) 0.056(12) -0.076(11) C15 0.052(9) 0.078(9) 0.078(11) 0.011(7) 0.020(8) 0.021(7) N32 0.089(8) 0.087(8) 0.110(9) -0.025(7) 0.064(7) -0.048(7) C72 0.066(9) 0.079(11) 0.085(9) 0.016(8) 0.007(7) -0.019(8) C47 0.052(9) 0.143(13) 0.065(9) 0.005(9) 0.036(8) -0.003(9) C70 0.065(8) 0.053(8) 0.102(10) 0.023(7) 0.036(7) -0.009(6) C28 0.111(13) 0.068(10) 0.095(11) -0.025(8) 0.048(12) -0.007(9) C55 0.035(7) 0.086(9) 0.055(7) 0.028(6) 0.004(6) 0.013(6) C74 0.171(19) 0.061(12) 0.077(11) -0.031(8) 0.022(12) -0.005(13) C49 0.043(9) 0.089(9) 0.034(7) 0.007(7) 0.011(6) -0.010(7) O11 0.32(2) 0.176(13) 0.246(17) 0.062(12) 0.214(17) -0.024(13) C60 0.108(12) 0.071(11) 0.171(15) -0.011(10) 0.105(12) -0.033(9) C16 0.074(9) 0.045(9) 0.079(9) 0.016(7) -0.025(7) -0.037(7) O13 0.257(16) 0.067(7) 0.201(13) 0.016(8) -0.064(12) -0.074(9) C48 0.059(10) 0.156(13) 0.051(8) 0.020(8) 0.020(7) -0.032(9) C29 0.113(15) 0.085(11) 0.124(14) -0.025(11) 0.079(13) -0.046(10) O18 0.304(18) 0.107(9) 0.177(12) 0.067(8) 0.167(13) 0.047(10) C19 0.019(6) 0.083(11) 0.062(9) 0.061(8) 0.003(6) -0.016(7) N10 0.057(9) 0.135(17) 0.165(16) 0.106(14) -0.017(9) -0.030(9) C18 0.073(10) 0.083(12) 0.128(13) 0.055(11) 0.003(9) 0.001(9) C73 0.18(2) 0.032(10) 0.100(13) -0.016(9) -0.003(12) -0.037(11) Cl4 0.224(8) 0.137(5) 0.155(5) 0.005(4) 0.049(5) 0.004(5) C17 0.108(16) 0.076(12) 0.135(17) 0.036(12) -0.045(12) -0.043(13) O21 0.170(12) 0.164(11) 0.093(8) 0.023(8) 0.018(8) 0.068(9) O20 0.37(3) 0.58(5) 0.23(2) -0.10(3) 0.19(2) 0.06(3) O22 0.20(2) 0.48(4) 0.73(7) -0.06(4) 0.22(3) -0.11(3) O19 0.47(4) 0.096(12) 0.36(3) -0.065(15) -0.05(2) -0.030(16) N43 0.060(6) 0.081(7) 0.042(5) -0.017(5) -0.004(5) 0.014(6) _geom_special_details ; All s.u.'s (except the s.u. in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell s.u.'s are taken into account individually in the estimation of s.u.'s in distances, angles and torsion angles; correlations between s.u.'s in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell s.u.'s is used for estimating s.u.'s 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 N36 2.142(7) . ? Mn1 N4 2.149(7) . ? Mn1 O1 2.181(5) . ? Mn1 O5 2.202(5) . ? Mn1 N33 2.382(7) . ? Mn1 N1 2.395(7) . ? Mn2 O2 2.142(5) . ? Mn2 O1 2.212(5) . ? Mn2 O6 2.235(6) . ? Mn2 N46 2.248(7) . ? Mn2 N6 2.263(7) . ? Mn2 N14 2.325(7) . ? Mn3 N20 2.129(8) . ? Mn3 O3 2.158(5) . ? Mn3 N12 2.158(8) . ? Mn3 O2 2.162(5) . ? Mn3 N17 2.339(7) . ? Mn3 N9 2.360(9) . ? Mn4 O3 2.161(5) . ? Mn4 O5 2.184(5) . ? Mn4 O4 2.194(6) . ? Mn4 N22 2.255(7) . ? Mn4 N30 2.275(7) . ? Mn4 N38 2.284(7) . ? Mn5 N28 2.153(8) . ? Mn5 N44 2.159(8) . ? Mn5 O4 2.164(5) . ? Mn5 O6 2.206(6) . ? Mn5 N25 2.361(8) . ? Mn5 N41 2.425(7) . ? Cl2 O15 1.401(8) . ? Cl2 O17 1.401(8) . ? Cl2 O16 1.401(7) . ? Cl2 O18 1.450(13) . ? Cl1 O10 1.403(9) . ? Cl1 O7 1.424(8) . ? Cl1 O9 1.433(9) . ? Cl1 O8 1.443(9) . ? Cl3 O11 1.339(12) . ? Cl3 O13 1.387(12) . ? Cl3 O14 1.402(8) . ? Cl3 O12 1.413(10) . ? O4 C51 1.324(10) . ? O1 C6 1.295(10) . ? O5 C66 1.326(10) . ? O6 C81 1.331(11) . ? O2 C21 1.326(10) . ? O3 C36 1.319(10) . ? N23 C39 1.333(12) . ? N23 N22 1.349(9) . ? N23 C41 1.371(12) . ? N12 C20 1.240(12) . ? N12 N13 1.381(10) . ? N31 C56 1.363(11) . ? N31 N30 1.369(9) . ? N31 C54 1.370(11) . ? N4 C5 1.309(11) . ? N4 N5 1.388(9) . ? N6 C7 1.341(11) . ? N6 N7 1.348(9) . ? N7 C9 1.358(11) . ? N7 C11 1.371(12) . ? N47 C84 1.376(11) . ? N47 N46 1.377(9) . ? N47 C86 1.382(11) . ? N37 C66 1.263(10) . ? N37 N36 1.402(9) . ? N35 C65 1.317(10) . ? N35 H35A 0.8600 . ? N35 H35B 0.8600 . ? N14 N15 1.359(10) . ? N14 C22 1.370(11) . ? N39 N38 1.357(10) . ? N39 C69 1.365(12) . ? N39 C71 1.375(13) . ? N29 C51 1.305(11) . ? N29 N28 1.417(10) . ? N20 C35 1.292(12) . ? N20 N21 1.411(10) . ? N30 C52 1.344(10) . ? N1 C1 1.355(12) . ? N1 C4 1.360(11) . ? N33 C61 1.350(11) . ? N33 C64 1.368(11) . ? N28 C50 1.272(12) . ? N41 C76 1.358(11) . ? N41 C79 1.388(11) . ? N44 C80 1.263(11) . ? N44 N45 1.393(10) . ? N45 C81 1.309(12) . ? N5 C6 1.311(10) . ? N36 C65 1.297(10) . ? N46 C82 1.357(10) . ? N27 C50 1.330(13) . ? N27 H27A 0.8600 . ? N27 H27B 0.8600 . ? N25 C46 1.352(13) . ? N25 C49 1.363(13) . ? C52 C53 1.358(11) . ? C52 C51 1.461(12) . ? N15 C24 1.359(11) . ? N15 C26 1.378(13) . ? N24 C41 1.345(12) . ? N24 C45 1.369(14) . ? N13 C21 1.285(11) . ? N2 C2 1.358(13) . ? N2 C3 1.372(13) . ? N22 C37 1.364(11) . ? N21 C36 1.289(11) . ? C67 N38 1.349(11) . ? C67 C68 1.363(12) . ? C67 C66 1.457(12) . ? C86 N48 1.368(11) . ? C86 C87 1.390(13) . ? C11 C12 1.361(13) . ? C11 N8 1.366(12) . ? C56 C57 1.349(16) . ? C56 N32 1.353(13) . ? C65 C64 1.467(13) . ? C64 C63 1.375(13) . ? C76 C77 1.337(12) . ? C76 H76 0.9300 . ? C3 C4 1.362(13) . ? C3 H3 0.9300 . ? C69 C68 1.354(13) . ? C69 C70 1.494(14) . ? N3 C5 1.322(11) . ? N3 H3A 0.8600 . ? N3 H3B 0.8600 . ? C7 C8C 1.371(12) . ? C7 C6 1.442(12) . ? N42 C77 1.360(13) . ? N42 C78 1.413(13) . ? C79 C78 1.371(13) . ? C79 C80 1.458(13) . ? N34 C63 1.365(13) . ? N34 C62 1.378(12) . ? C77 H77 0.9300 . ? C54 C53 1.354(12) . ? C54 C55 1.483(13) . ? N9 C16 1.340(14) . ? N9 C19 1.360(14) . ? C5 C4 1.460(12) . ? N17 C31 1.336(11) . ? N17 C34 1.378(12) . ? C26 C27 1.321(13) . ? C26 N16 1.381(13) . ? C71 N40 1.368(13) . ? C71 C72 1.402(15) . ? C78 H78 0.9300 . ? C41 C42 1.381(14) . ? C22 C23 1.352(12) . ? C22 C21 1.451(13) . ? C45 C44 1.353(16) . ? C45 H45 0.9300 . ? N18 C32 1.365(14) . ? N18 C33 1.369(13) . ? C82 C83 1.397(12) . ? C82 C81 1.404(13) . ? C83 C84 1.376(12) . ? C83 H83 0.9300 . ? C53 H53 0.9300 . ? C35 N19 1.328(13) . ? C35 C34 1.454(14) . ? C68 H68 0.9300 . ? N11 C20 1.351(13) . ? N11 H11A 0.8600 . ? N11 H11B 0.8600 . ? N16 C30 1.412(17) . ? N48 C90 1.368(12) . ? C87 C88 1.354(13) . ? C87 H87 0.9300 . ? C8C C9 1.357(12) . ? C8C H8C 0.9300 . ? C31 C32 1.384(14) . ? C31 H31 0.9300 . ? C61 C62 1.344(13) . ? C61 H61 0.9300 . ? C36 C37 1.444(13) . ? C2 C1 1.345(14) . ? C2 H2 0.9300 . ? C39 C38 1.345(13) . ? C39 C40 1.524(13) . ? C38 C37 1.347(13) . ? C38 H38 0.9300 . ? C9 C10 1.507(13) . ? C24 C23 1.353(13) . ? C24 C25 1.518(14) . ? C23 H23 0.9300 . ? C34 C33 1.362(13) . ? C27 C28 1.327(16) . ? C27 H27 0.9300 . ? C13 C14 1.365(15) . ? C13 C12 1.385(15) . ? C13 H13 0.9300 . ? C63 H63 0.9300 . ? N40 C75 1.353(16) . ? N26 C48 1.366(15) . ? N26 C47 1.394(16) . ? C1 H1 0.9300 . ? C12 H12 0.9300 . ? N8 C15 1.371(13) . ? C50 C49 1.460(14) . ? C85 C84 1.520(13) . ? C85 H85A 0.9600 . ? C85 H85B 0.9600 . ? C85 H85C 0.9600 . ? C40 H40A 0.9600 . ? C40 H40B 0.9600 . ? C40 H40C 0.9600 . ? C59 C60 1.327(16) . ? C59 C58 1.384(18) . ? C59 H59 0.9300 . ? N19 H19A 0.8600 . ? N19 H19B 0.8600 . ? C57 C58 1.371(18) . ? C57 H57 0.9300 . ? C33 H33 0.9300 . ? C14 C15 1.340(15) . ? C14 H14 0.9300 . ? C88 C89 1.365(13) . ? C88 H88 0.9300 . ? C42 C43 1.391(15) . ? C42 H42 0.9300 . ? C20 C19 1.427(16) . ? C32 H32 0.9300 . ? C80 N43 1.354(12) . ? C46 C47 1.351(15) . ? C46 H46 0.9300 . ? C25 H25A 0.9600 . ? C25 H25B 0.9600 . ? C25 H25C 0.9600 . ? C43 C44 1.337(16) . ? C43 H43 0.9300 . ? C89 C90 1.365(13) . ? C89 H89 0.9300 . ? C10 H10A 0.9600 . ? C10 H10B 0.9600 . ? C10 H10C 0.9600 . ? C75 C74 1.33(2) . ? C75 H75 0.9300 . ? C90 H90 0.9300 . ? C30 C29 1.355(19) . ? C30 H30 0.9300 . ? C62 H62 0.9300 . ? C44 H44 0.9300 . ? C58 H58 0.9300 . ? C15 H15 0.9300 . ? N32 C60 1.344(14) . ? C72 C73 1.37(2) . ? C72 H72 0.9300 . ? C47 H47 0.9300 . ? C70 H70A 0.9600 . ? C70 H70B 0.9600 . ? C70 H70C 0.9600 . ? C28 C29 1.382(19) . ? C28 H28 0.9300 . ? C55 H55A 0.9600 . ? C55 H55B 0.9600 . ? C55 H55C 0.9600 . ? C74 C73 1.32(2) . ? C74 H74 0.9300 . ? C49 C48 1.354(15) . ? C60 H60 0.9300 . ? C16 C17 1.34(2) . ? C16 H16 0.9300 . ? C48 H48 0.9300 . ? C29 H29 0.9300 . ? C19 C18 1.330(18) . ? N10 C17 1.34(2) . ? N10 C18 1.40(2) . ? C18 H18 0.9300 . ? C73 H73 0.9300 . ? Cl4 O21 1.292(11) . ? Cl4 O19 1.425(15) . ? Cl4 O20 1.444(17) . ? Cl4 O22 1.46(2) . ? C17 H17 0.9300 . ? N43 H43A 0.8600 . ? N43 H43B 0.8600 . ? 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 N36 Mn1 N4 146.2(3) . . ? N36 Mn1 O1 129.5(2) . . ? N4 Mn1 O1 71.7(3) . . ? N36 Mn1 O5 71.8(2) . . ? N4 Mn1 O5 132.4(2) . . ? O1 Mn1 O5 107.5(2) . . ? N36 Mn1 N33 69.3(3) . . ? N4 Mn1 N33 85.9(2) . . ? O1 Mn1 N33 91.9(2) . . ? O5 Mn1 N33 140.5(2) . . ? N36 Mn1 N1 89.4(3) . . ? N4 Mn1 N1 68.4(3) . . ? O1 Mn1 N1 139.5(3) . . ? O5 Mn1 N1 94.0(2) . . ? N33 Mn1 N1 92.5(2) . . ? O2 Mn2 O1 87.2(2) . . ? O2 Mn2 O6 92.7(2) . . ? O1 Mn2 O6 84.2(2) . . ? O2 Mn2 N46 97.4(2) . . ? O1 Mn2 N46 158.1(2) . . ? O6 Mn2 N46 74.2(2) . . ? O2 Mn2 N6 162.3(3) . . ? O1 Mn2 N6 75.3(3) . . ? O6 Mn2 N6 87.7(2) . . ? N46 Mn2 N6 99.7(3) . . ? O2 Mn2 N14 74.3(3) . . ? O1 Mn2 N14 85.2(2) . . ? O6 Mn2 N14 163.7(3) . . ? N46 Mn2 N14 116.7(3) . . ? N6 Mn2 N14 101.5(3) . . ? N20 Mn3 O3 72.3(3) . . ? N20 Mn3 N12 153.0(3) . . ? O3 Mn3 N12 126.1(3) . . ? N20 Mn3 O2 125.6(3) . . ? O3 Mn3 O2 106.0(2) . . ? N12 Mn3 O2 72.3(3) . . ? N20 Mn3 N17 70.3(3) . . ? O3 Mn3 N17 142.2(3) . . ? N12 Mn3 N17 90.8(3) . . ? O2 Mn3 N17 91.7(2) . . ? N20 Mn3 N9 91.6(4) . . ? O3 Mn3 N9 92.8(3) . . ? N12 Mn3 N9 69.7(4) . . ? O2 Mn3 N9 141.7(3) . . ? N17 Mn3 N9 93.2(3) . . ? O3 Mn4 O5 91.4(2) . . ? O3 Mn4 O4 90.9(2) . . ? O5 Mn4 O4 86.0(2) . . ? O3 Mn4 N22 74.5(3) . . ? O5 Mn4 N22 164.6(3) . . ? O4 Mn4 N22 88.1(2) . . ? O3 Mn4 N30 165.4(3) . . ? O5 Mn4 N30 87.7(2) . . ? O4 Mn4 N30 74.6(3) . . ? N22 Mn4 N30 104.4(3) . . ? O3 Mn4 N38 94.0(2) . . ? O5 Mn4 N38 74.7(3) . . ? O4 Mn4 N38 160.2(3) . . ? N22 Mn4 N38 111.7(3) . . ? N30 Mn4 N38 99.8(3) . . ? N28 Mn5 N44 142.7(3) . . ? N28 Mn5 O4 71.9(3) . . ? N44 Mn5 O4 132.2(3) . . ? N28 Mn5 O6 133.6(3) . . ? N44 Mn5 O6 72.4(3) . . ? O4 Mn5 O6 108.2(2) . . ? N28 Mn5 N25 68.3(4) . . ? N44 Mn5 N25 87.8(3) . . ? O4 Mn5 N25 138.8(3) . . ? O6 Mn5 N25 91.7(3) . . ? N28 Mn5 N41 84.2(3) . . ? N44 Mn5 N41 69.4(3) . . ? O4 Mn5 N41 91.2(2) . . ? O6 Mn5 N41 140.8(3) . . ? N25 Mn5 N41 95.4(3) . . ? O15 Cl2 O17 112.8(6) . . ? O15 Cl2 O16 110.5(5) . . ? O17 Cl2 O16 109.0(5) . . ? O15 Cl2 O18 106.6(6) . . ? O17 Cl2 O18 110.9(8) . . ? O16 Cl2 O18 106.9(7) . . ? O10 Cl1 O7 110.2(5) . . ? O10 Cl1 O9 106.8(7) . . ? O7 Cl1 O9 108.6(6) . . ? O10 Cl1 O8 111.3(6) . . ? O7 Cl1 O8 110.0(6) . . ? O9 Cl1 O8 109.9(6) . . ? O11 Cl3 O13 112.0(10) . . ? O11 Cl3 O14 112.6(8) . . ? O13 Cl3 O14 110.3(7) . . ? O11 Cl3 O12 110.4(9) . . ? O13 Cl3 O12 104.5(9) . . ? O14 Cl3 O12 106.5(5) . . ? C51 O4 Mn5 113.6(5) . . ? C51 O4 Mn4 117.4(6) . . ? Mn5 O4 Mn4 126.8(3) . . ? C6 O1 Mn1 112.7(5) . . ? C6 O1 Mn2 114.5(5) . . ? Mn1 O1 Mn2 131.3(3) . . ? C66 O5 Mn4 116.3(5) . . ? C66 O5 Mn1 111.8(5) . . ? Mn4 O5 Mn1 130.1(3) . . ? C81 O6 Mn5 111.5(5) . . ? C81 O6 Mn2 114.5(5) . . ? Mn5 O6 Mn2 131.8(3) . . ? C21 O2 Mn2 119.6(5) . . ? C21 O2 Mn3 112.9(5) . . ? Mn2 O2 Mn3 125.5(3) . . ? C36 O3 Mn3 112.7(5) . . ? C36 O3 Mn4 117.5(5) . . ? Mn3 O3 Mn4 127.7(3) . . ? C39 N23 N22 109.9(7) . . ? C39 N23 C41 128.6(8) . . ? N22 N23 C41 121.3(8) . . ? C20 N12 N13 118.4(9) . . ? C20 N12 Mn3 123.9(8) . . ? N13 N12 Mn3 117.7(6) . . ? C56 N31 N30 120.8(8) . . ? C56 N31 C54 129.7(8) . . ? N30 N31 C54 109.4(7) . . ? C5 N4 N5 113.6(7) . . ? C5 N4 Mn1 126.8(6) . . ? N5 N4 Mn1 118.8(5) . . ? C7 N6 N7 107.4(7) . . ? C7 N6 Mn2 111.5(6) . . ? N7 N6 Mn2 141.0(6) . . ? N6 N7 C9 109.9(7) . . ? N6 N7 C11 121.9(8) . . ? C9 N7 C11 128.2(8) . . ? C84 N47 N46 110.3(7) . . ? C84 N47 C86 128.3(8) . . ? N46 N47 C86 120.9(7) . . ? C66 N37 N36 110.8(7) . . ? C65 N35 H35A 120.0 . . ? C65 N35 H35B 120.0 . . ? H35A N35 H35B 120.0 . . ? N15 N14 C22 106.6(7) . . ? N15 N14 Mn2 142.7(6) . . ? C22 N14 Mn2 110.7(6) . . ? N38 N39 C69 109.3(8) . . ? N38 N39 C71 122.3(9) . . ? C69 N39 C71 128.0(9) . . ? C51 N29 N28 108.7(7) . . ? C35 N20 N21 116.1(8) . . ? C35 N20 Mn3 124.6(7) . . ? N21 N20 Mn3 119.1(6) . . ? C52 N30 N31 106.0(6) . . ? C52 N30 Mn4 112.4(6) . . ? N31 N30 Mn4 141.6(6) . . ? C1 N1 C4 117.2(8) . . ? C1 N1 Mn1 127.0(7) . . ? C4 N1 Mn1 115.3(6) . . ? C61 N33 C64 117.0(7) . . ? C61 N33 Mn1 128.9(6) . . ? C64 N33 Mn1 114.1(6) . . ? C50 N28 N29 115.0(8) . . ? C50 N28 Mn5 126.3(7) . . ? N29 N28 Mn5 118.5(6) . . ? C76 N41 C79 117.8(8) . . ? C76 N41 Mn5 129.3(7) . . ? C79 N41 Mn5 112.4(6) . . ? C80 N44 N45 115.4(8) . . ? C80 N44 Mn5 125.4(6) . . ? N45 N44 Mn5 118.9(5) . . ? C81 N45 N44 110.0(8) . . ? C6 N5 N4 109.0(7) . . ? C65 N36 N37 114.3(7) . . ? C65 N36 Mn1 127.0(6) . . ? N37 N36 Mn1 118.6(5) . . ? C82 N46 N47 106.9(7) . . ? C82 N46 Mn2 113.3(5) . . ? N47 N46 Mn2 139.8(6) . . ? C50 N27 H27A 120.0 . . ? C50 N27 H27B 120.0 . . ? H27A N27 H27B 120.0 . . ? C46 N25 C49 118.9(9) . . ? C46 N25 Mn5 124.2(9) . . ? C49 N25 Mn5 116.7(7) . . ? N30 C52 C53 109.9(8) . . ? N30 C52 C51 119.2(8) . . ? C53 C52 C51 130.9(9) . . ? N14 N15 C24 109.5(8) . . ? N14 N15 C26 119.8(8) . . ? C24 N15 C26 130.8(9) . . ? C41 N24 C45 116.4(10) . . ? C21 N13 N12 111.2(8) . . ? C2 N2 C3 117.5(9) . . ? N23 N22 C37 105.9(7) . . ? N23 N22 Mn4 140.6(6) . . ? C37 N22 Mn4 113.3(6) . . ? C36 N21 N20 108.4(7) . . ? N38 C67 C68 108.3(8) . . ? N38 C67 C66 117.5(9) . . ? C68 C67 C66 134.2(10) . . ? N48 C86 N47 114.5(8) . . ? N48 C86 C87 120.8(9) . . ? N47 C86 C87 124.6(9) . . ? C12 C11 N8 120.8(10) . . ? C12 C11 N7 121.4(9) . . ? N8 C11 N7 117.8(9) . . ? C57 C56 N32 118.9(10) . . ? C57 C56 N31 124.1(10) . . ? N32 C56 N31 116.9(9) . . ? N36 C65 N35 126.2(8) . . ? N36 C65 C64 113.3(8) . . ? N35 C65 C64 120.5(9) . . ? N33 C64 C63 120.5(9) . . ? N33 C64 C65 115.9(8) . . ? C63 C64 C65 123.6(9) . . ? C77 C76 N41 124.4(10) . . ? C77 C76 H76 117.8 . . ? N41 C76 H76 117.8 . . ? C4 C3 N2 121.1(10) . . ? C4 C3 H3 119.5 . . ? N2 C3 H3 119.5 . . ? C68 C69 N39 106.5(8) . . ? C68 C69 C70 128.3(12) . . ? N39 C69 C70 125.1(11) . . ? C5 N3 H3A 120.0 . . ? C5 N3 H3B 120.0 . . ? H3A N3 H3B 120.0 . . ? N6 C7 C8C 108.1(8) . . ? N6 C7 C6 119.0(8) . . ? C8C C7 C6 132.9(9) . . ? C77 N42 C78 119.0(8) . . ? C67 N38 N39 107.3(7) . . ? C67 N38 Mn4 112.6(6) . . ? N39 N38 Mn4 139.9(7) . . ? C78 C79 N41 119.5(9) . . ? C78 C79 C80 126.1(10) . . ? N41 C79 C80 114.4(8) . . ? C63 N34 C62 116.0(9) . . ? N37 C66 O5 125.8(8) . . ? N37 C66 C67 115.7(9) . . ? O5 C66 C67 118.4(8) . . ? C76 C77 N42 119.0(9) . . ? C76 C77 H77 120.5 . . ? N42 C77 H77 120.5 . . ? O1 C6 N5 126.0(8) . . ? O1 C6 C7 119.7(8) . . ? N5 C6 C7 114.4(9) . . ? C53 C54 N31 106.7(8) . . ? C53 C54 C55 132.4(9) . . ? N31 C54 C55 120.9(9) . . ? C16 N9 C19 118.5(11) . . ? C16 N9 Mn3 128.0(10) . . ? C19 N9 Mn3 113.5(8) . . ? N4 C5 N3 126.1(8) . . ? N4 C5 C4 114.1(8) . . ? N3 C5 C4 119.8(9) . . ? C31 N17 C34 118.2(8) . . ? C31 N17 Mn3 126.6(7) . . ? C34 N17 Mn3 115.2(6) . . ? C27 C26 N15 121.9(10) . . ? C27 C26 N16 123.5(11) . . ? N15 C26 N16 114.6(11) . . ? N29 C51 O4 125.1(8) . . ? N29 C51 C52 118.4(8) . . ? O4 C51 C52 116.4(9) . . ? N40 C71 N39 119.4(9) . . ? N40 C71 C72 118.6(12) . . ? N39 C71 C72 121.9(12) . . ? C79 C78 N42 120.2(10) . . ? C79 C78 H78 119.9 . . ? N42 C78 H78 119.9 . . ? N24 C41 N23 116.6(9) . . ? N24 C41 C42 121.9(10) . . ? N23 C41 C42 121.6(11) . . ? C23 C22 N14 108.1(9) . . ? C23 C22 C21 133.1(10) . . ? N14 C22 C21 118.6(9) . . ? C44 C45 N24 124.1(12) . . ? C44 C45 H45 118.0 . . ? N24 C45 H45 118.0 . . ? C32 N18 C33 116.3(9) . . ? N46 C82 C83 108.4(8) . . ? N46 C82 C81 118.8(8) . . ? C83 C82 C81 132.7(9) . . ? C84 C83 C82 108.4(8) . . ? C84 C83 H83 125.8 . . ? C82 C83 H83 125.8 . . ? C54 C53 C52 108.0(8) . . ? C54 C53 H53 126.0 . . ? C52 C53 H53 126.0 . . ? N20 C35 N19 124.5(10) . . ? N20 C35 C34 116.4(10) . . ? N19 C35 C34 119.1(10) . . ? C69 C68 C67 108.7(9) . . ? C69 C68 H68 125.7 . . ? C67 C68 H68 125.7 . . ? C20 N11 H11A 120.0 . . ? C20 N11 H11B 120.0 . . ? H11A N11 H11B 120.0 . . ? N45 C81 O6 126.0(8) . . ? N45 C81 C82 115.0(9) . . ? O6 C81 C82 119.0(9) . . ? C26 N16 C30 115.6(12) . . ? C86 N48 C90 117.8(8) . . ? C88 C87 C86 119.4(9) . . ? C88 C87 H87 120.3 . . ? C86 C87 H87 120.3 . . ? C9 C8C C7 108.3(8) . . ? C9 C8C H8C 125.9 . . ? C7 C8C H8C 125.9 . . ? N17 C31 C32 121.9(10) . . ? N17 C31 H31 119.1 . . ? C32 C31 H31 119.1 . . ? C62 C61 N33 122.9(9) . . ? C62 C61 H61 118.6 . . ? N33 C61 H61 118.6 . . ? N21 C36 O3 126.1(8) . . ? N21 C36 C37 116.0(9) . . ? O3 C36 C37 117.9(9) . . ? C1 C2 N2 120.8(10) . . ? C1 C2 H2 119.6 . . ? N2 C2 H2 119.6 . . ? N23 C39 C38 107.7(8) . . ? N23 C39 C40 120.9(9) . . ? C38 C39 C40 131.4(11) . . ? N1 C4 C3 120.9(9) . . ? N1 C4 C5 114.7(8) . . ? C3 C4 C5 124.3(9) . . ? C39 C38 C37 107.9(9) . . ? C39 C38 H38 126.0 . . ? C37 C38 H38 126.0 . . ? C8C C9 N7 106.3(8) . . ? C8C C9 C10 130.1(9) . . ? N7 C9 C10 123.5(9) . . ? C23 C24 N15 106.8(8) . . ? C23 C24 C25 133.8(10) . . ? N15 C24 C25 119.3(10) . . ? N13 C21 O2 124.8(9) . . ? N13 C21 C22 118.5(9) . . ? O2 C21 C22 116.6(8) . . ? C22 C23 C24 109.1(8) . . ? C22 C23 H23 125.5 . . ? C24 C23 H23 125.5 . . ? C33 C34 N17 119.7(9) . . ? C33 C34 C35 126.9(10) . . ? N17 C34 C35 113.4(9) . . ? C26 C27 C28 120.3(11) . . ? C26 C27 H27 119.9 . . ? C28 C27 H27 119.9 . . ? C14 C13 C12 118.8(11) . . ? C14 C13 H13 120.6 . . ? C12 C13 H13 120.6 . . ? N34 C63 C64 122.2(9) . . ? N34 C63 H63 118.9 . . ? C64 C63 H63 118.9 . . ? C75 N40 C71 117.1(11) . . ? C48 N26 C47 116.9(11) . . ? C2 C1 N1 122.5(10) . . ? C2 C1 H1 118.7 . . ? N1 C1 H1 118.7 . . ? C11 C12 C13 120.0(10) . . ? C11 C12 H12 120.0 . . ? C13 C12 H12 120.0 . . ? C11 N8 C15 118.3(9) . . ? N28 C50 N27 125.8(10) . . ? N28 C50 C49 115.9(10) . . ? N27 C50 C49 118.3(11) . . ? C84 C85 H85A 109.5 . . ? C84 C85 H85B 109.5 . . ? H85A C85 H85B 109.5 . . ? C84 C85 H85C 109.5 . . ? H85A C85 H85C 109.5 . . ? H85B C85 H85C 109.5 . . ? C38 C37 N22 108.5(8) . . ? C38 C37 C36 134.9(10) . . ? N22 C37 C36 116.4(9) . . ? C39 C40 H40A 109.5 . . ? C39 C40 H40B 109.5 . . ? H40A C40 H40B 109.5 . . ? C39 C40 H40C 109.5 . . ? H40A C40 H40C 109.5 . . ? H40B C40 H40C 109.5 . . ? C60 C59 C58 119.2(11) . . ? C60 C59 H59 120.4 . . ? C58 C59 H59 120.4 . . ? C35 N19 H19A 120.0 . . ? C35 N19 H19B 120.0 . . ? H19A N19 H19B 120.0 . . ? C56 C57 C58 122.5(13) . . ? C56 C57 H57 118.8 . . ? C58 C57 H57 118.8 . . ? C34 C33 N18 123.1(10) . . ? C34 C33 H33 118.5 . . ? N18 C33 H33 118.5 . . ? C15 C14 C13 120.5(11) . . ? C15 C14 H14 119.8 . . ? C13 C14 H14 119.8 . . ? C87 C88 C89 120.8(9) . . ? C87 C88 H88 119.6 . . ? C89 C88 H88 119.6 . . ? C41 C42 C43 119.0(11) . . ? C41 C42 H42 120.5 . . ? C43 C42 H42 120.5 . . ? C83 C84 N47 106.0(8) . . ? C83 C84 C85 129.2(9) . . ? N47 C84 C85 124.6(9) . . ? N12 C20 N11 123.6(12) . . ? N12 C20 C19 117.9(11) . . ? N11 C20 C19 118.3(11) . . ? N18 C32 C31 121.0(10) . . ? N18 C32 H32 119.5 . . ? C31 C32 H32 119.5 . . ? N44 C80 N43 124.5(8) . . ? N44 C80 C79 117.4(9) . . ? N43 C80 C79 118.1(9) . . ? C47 C46 N25 122.0(12) . . ? C47 C46 H46 119.0 . . ? N25 C46 H46 119.0 . . ? C24 C25 H25A 109.5 . . ? C24 C25 H25B 109.5 . . ? H25A C25 H25B 109.5 . . ? C24 C25 H25C 109.5 . . ? H25A C25 H25C 109.5 . . ? H25B C25 H25C 109.5 . . ? C44 C43 C42 119.9(12) . . ? C44 C43 H43 120.1 . . ? C42 C43 H43 120.1 . . ? C88 C89 C90 118.9(9) . . ? C88 C89 H89 120.6 . . ? C90 C89 H89 120.6 . . ? C9 C10 H10A 109.5 . . ? C9 C10 H10B 109.5 . . ? H10A C10 H10B 109.5 . . ? C9 C10 H10C 109.5 . . ? H10A C10 H10C 109.5 . . ? H10B C10 H10C 109.5 . . ? C74 C75 N40 127.5(16) . . ? C74 C75 H75 116.3 . . ? N40 C75 H75 116.3 . . ? C89 C90 N48 122.3(9) . . ? C89 C90 H90 118.9 . . ? N48 C90 H90 118.9 . . ? C29 C30 N16 120.5(13) . . ? C29 C30 H30 119.8 . . ? N16 C30 H30 119.8 . . ? C61 C62 N34 121.4(10) . . ? C61 C62 H62 119.3 . . ? N34 C62 H62 119.3 . . ? C43 C44 C45 118.9(11) . . ? C43 C44 H44 120.6 . . ? C45 C44 H44 120.6 . . ? C57 C58 C59 117.1(13) . . ? C57 C58 H58 121.4 . . ? C59 C58 H58 121.4 . . ? C14 C15 N8 121.7(11) . . ? C14 C15 H15 119.2 . . ? N8 C15 H15 119.2 . . ? C60 N32 C56 119.1(11) . . ? C73 C72 C71 117.0(14) . . ? C73 C72 H72 121.5 . . ? C71 C72 H72 121.5 . . ? C46 C47 N26 120.0(12) . . ? C46 C47 H47 120.0 . . ? N26 C47 H47 120.0 . . ? C69 C70 H70A 109.5 . . ? C69 C70 H70B 109.5 . . ? H70A C70 H70B 109.5 . . ? C69 C70 H70C 109.5 . . ? H70A C70 H70C 109.5 . . ? H70B C70 H70C 109.5 . . ? C27 C28 C29 120.6(14) . . ? C27 C28 H28 119.7 . . ? C29 C28 H28 119.7 . . ? C54 C55 H55A 109.5 . . ? C54 C55 H55B 109.5 . . ? H55A C55 H55B 109.5 . . ? C54 C55 H55C 109.5 . . ? H55A C55 H55C 109.5 . . ? H55B C55 H55C 109.5 . . ? C73 C74 C75 113.3(16) . . ? C73 C74 H74 123.3 . . ? C75 C74 H74 123.3 . . ? C48 C49 N25 119.7(11) . . ? C48 C49 C50 127.7(12) . . ? N25 C49 C50 112.6(10) . . ? C59 C60 N32 123.2(12) . . ? C59 C60 H60 118.4 . . ? N32 C60 H60 118.4 . . ? N9 C16 C17 124.0(16) . . ? N9 C16 H16 118.0 . . ? C17 C16 H16 118.0 . . ? C49 C48 N26 122.6(13) . . ? C49 C48 H48 118.7 . . ? N26 C48 H48 118.7 . . ? C30 C29 C28 119.5(13) . . ? C30 C29 H29 120.3 . . ? C28 C29 H29 120.3 . . ? C18 C19 N9 118.8(15) . . ? C18 C19 C20 126.2(15) . . ? N9 C19 C20 114.9(9) . . ? C17 N10 C18 118.2(15) . . ? C19 C18 N10 122.0(16) . . ? C19 C18 H18 119.0 . . ? N10 C18 H18 119.0 . . ? C74 C73 C72 126.3(17) . . ? C74 C73 H73 116.8 . . ? C72 C73 H73 116.8 . . ? O21 Cl4 O19 99.9(12) . . ? O21 Cl4 O20 107.8(14) . . ? O19 Cl4 O20 109.6(19) . . ? O21 Cl4 O22 104.9(18) . . ? O19 Cl4 O22 114.2(19) . . ? O20 Cl4 O22 118(2) . . ? N10 C17 C16 118.4(19) . . ? N10 C17 H17 120.8 . . ? C16 C17 H17 120.8 . . ? C80 N43 H43A 120.0 . . ? C80 N43 H43B 120.0 . . ? H43A N43 H43B 120.0 . . ? _diffrn_measured_fraction_theta_max 0.990 _diffrn_reflns_theta_full 25.48 _diffrn_measured_fraction_theta_full 0.990 _refine_diff_density_max 0.498 _refine_diff_density_min -0.832 _refine_diff_density_rms 0.089 # Details about the Squeezed Material loop_ _platon_squeeze_void_nr _platon_squeeze_void_average_x _platon_squeeze_void_average_y _platon_squeeze_void_average_z _platon_squeeze_void_volume _platon_squeeze_void_count_electrons _platon_squeeze_void_content 1 0.500 0.000 0.000 253 79 ' ' 2 0.048 0.463 0.029 29 10 ' ' 3 -0.055 0.542 -0.033 25 9 ' ' 4 0.072 0.200 0.024 14 8 ' ' 5 0.708 0.424 0.227 7 1 ' ' 6 0.292 0.924 0.273 7 1 ' ' 7 0.500 0.500 0.500 253 79 ' ' 8 0.952 0.963 0.471 28 9 ' ' 9 0.928 0.700 0.476 14 8 ' ' 10 1.055 0.042 0.533 27 9 ' ' 11 0.072 0.300 0.524 14 8 ' ' 12 0.708 0.076 0.727 7 1 ' ' 13 0.292 0.576 0.773 7 1 ' ' 14 0.928 0.800 0.976 14 8 ' ' _platon_squeeze_details ; SQUEEZE was used to remove the contributions of three solvent water molecule. ;