# 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_volume ? _journal_page_first ? _journal_year ? _publ_contact_author_name 'Dr Ashutosh Ghosh' _publ_contact_author_email 'ghosh 59@yahoo.com' _publ_section_title ; Synthesis of the first heterometalic star-shaped oxido-bridged MnCu3 complex and its conversion into trinuclear species modulated by pseudohalides (N3-, NCS- and NCO-): Structural analysis and magnetic properties ; loop_ _publ_author_name S.Biswas S.Naiya C.J.Gomez-Garcia A.Ghosh # Attachment '- 1-4.cif' data_1 _database_code_depnum_ccdc_archive 'CCDC 833841' #TrackingRef '- 1-4.cif' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety 'C57 H64 Cu3 Mn N6 O8 2(ClO4)' _chemical_formula_sum 'C57 H64 Cl2 Cu3 Mn N6 O16' _chemical_formula_weight 1405.60 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' Cu Cu 0.3201 1.2651 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting Triclinic _symmetry_space_group_name_H-M 'P -1' _symmetry_space_group_name_Hall '-P 1' loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, -y, -z' _cell_length_a 12.478(5) _cell_length_b 15.326(5) _cell_length_c 18.404(5) _cell_angle_alpha 68.759(5) _cell_angle_beta 77.929(5) _cell_angle_gamma 69.453(5) _cell_volume 3058.2(18) _cell_formula_units_Z 2 _cell_measurement_temperature 150(2) _cell_measurement_reflns_used 20557 _cell_measurement_theta_min 1.2 _cell_measurement_theta_max 32.3 _exptl_crystal_description rectangular _exptl_crystal_colour green _exptl_crystal_size_max 0.24 _exptl_crystal_size_mid 0.22 _exptl_crystal_size_min 0.12 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.526 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1444 _exptl_absorpt_coefficient_mu 1.390 _exptl_absorpt_correction_type empirical _exptl_absorpt_correction_T_min 0.7315 _exptl_absorpt_correction_T_max 0.8510 _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 56746 _diffrn_reflns_av_R_equivalents 0.0303 _diffrn_reflns_av_sigmaI/netI 0.0421 _diffrn_reflns_limit_h_min -18 _diffrn_reflns_limit_h_max 18 _diffrn_reflns_limit_k_min -22 _diffrn_reflns_limit_k_max 22 _diffrn_reflns_limit_l_min -25 _diffrn_reflns_limit_l_max 26 _diffrn_reflns_theta_min 1.19 _diffrn_reflns_theta_max 32.30 _reflns_number_total 20557 _reflns_number_gt 13908 _reflns_threshold_expression >2sigma(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 V1.80.03' _refine_special_details ; Refinement of F^2^ against ALL reflections. The weighted R-factor wR and goodness of fit S are based on F^2^, conventional R-factors R are based on F, with F set to zero for negative F^2^. The threshold expression of F^2^ > 2sigma(F^2^) is used only for calculating R-factors(gt) etc. and is not relevant to the choice of reflections for refinement. R-factors based on F^2^ are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger. ; _refine_ls_structure_factor_coef Fsqd _refine_ls_matrix_type full _refine_ls_weighting_scheme calc _refine_ls_weighting_details 'calc w=1/[\s^2^(Fo^2^)+(0.1204P)^2^+1.3566P] 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 20557 _refine_ls_number_parameters 766 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0884 _refine_ls_R_factor_gt 0.0585 _refine_ls_wR_factor_ref 0.1995 _refine_ls_wR_factor_gt 0.1755 _refine_ls_goodness_of_fit_ref 1.018 _refine_ls_restrained_S_all 1.018 _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 C1 C 0.8229(3) 0.2206(2) 0.94333(17) 0.0401(6) Uani 1 1 d . . . C2 C 0.7982(3) 0.3052(3) 0.9637(2) 0.0509(7) Uani 1 1 d . . . H2 H 0.8219 0.3579 0.9288 0.061 Uiso 1 1 calc R . . C3 C 0.7397(5) 0.3123(4) 1.0340(2) 0.0731(12) Uani 1 1 d . . . H3 H 0.7229 0.3699 1.0462 0.088 Uiso 1 1 calc R . . C4 C 0.7057(6) 0.2339(4) 1.0870(3) 0.0922(17) Uani 1 1 d . . . H4 H 0.6637 0.2396 1.1340 0.111 Uiso 1 1 calc R . . C5 C 0.7332(4) 0.1485(4) 1.0707(2) 0.0741(12) Uani 1 1 d . . . H5 H 0.7102 0.0963 1.1073 0.089 Uiso 1 1 calc R . . C6 C 0.7956(3) 0.1370(3) 1.00002(18) 0.0490(7) Uani 1 1 d . . . C7 C 0.8375(3) 0.0397(2) 0.9900(2) 0.0515(8) Uani 1 1 d . . . C8 C 0.8419(5) -0.0490(3) 1.0630(2) 0.0769(13) Uani 1 1 d . . . H8A H 0.8707 -0.1078 1.0484 0.115 Uiso 1 1 calc R . . H8B H 0.7660 -0.0440 1.0893 0.115 Uiso 1 1 calc R . . H8C H 0.8916 -0.0512 1.0974 0.115 Uiso 1 1 calc R . . C9 C 0.9274(4) -0.0711(2) 0.9157(2) 0.0619(10) Uani 1 1 d . . . H9A H 0.8679 -0.0996 0.9183 0.074 Uiso 1 1 calc R . . H9B H 0.9733 -0.1122 0.9592 0.074 Uiso 1 1 calc R . . C10 C 1.0021(4) -0.0686(3) 0.8402(3) 0.0620(9) Uani 1 1 d . . . H10A H 1.0448 -0.0228 0.8305 0.074 Uiso 1 1 calc R . . H10B H 1.0573 -0.1331 0.8459 0.074 Uiso 1 1 calc R . . C11 C 0.9391(4) -0.0398(3) 0.7704(3) 0.0674(11) Uani 1 1 d . . . H11A H 0.9945 -0.0444 0.7253 0.081 Uiso 1 1 calc R . . H11B H 0.8970 -0.0858 0.7795 0.081 Uiso 1 1 calc R . . C12 C 0.8047(4) 0.0949(3) 0.6907(2) 0.0562(8) Uani 1 1 d . . . C13 C 0.8258(6) 0.0340(4) 0.6373(3) 0.103(2) Uani 1 1 d . . . H13A H 0.8821 -0.0282 0.6573 0.154 Uiso 1 1 calc R . . H13B H 0.8533 0.0680 0.5857 0.154 Uiso 1 1 calc R . . H13C H 0.7553 0.0235 0.6349 0.154 Uiso 1 1 calc R . . C14 C 0.7205(3) 0.1931(3) 0.6691(2) 0.0554(8) Uani 1 1 d . . . C15 C 0.6345(5) 0.2143(4) 0.6201(3) 0.0868(15) Uani 1 1 d . . . H15 H 0.6315 0.1648 0.6035 0.104 Uiso 1 1 calc R . . C16 C 0.5570(5) 0.3040(5) 0.5969(3) 0.0938(17) Uani 1 1 d . . . H16 H 0.5030 0.3156 0.5639 0.113 Uiso 1 1 calc R . . C17 C 0.5574(4) 0.3776(4) 0.6217(2) 0.0698(11) Uani 1 1 d . . . H17 H 0.5043 0.4395 0.6052 0.084 Uiso 1 1 calc R . . C18 C 0.6369(3) 0.3599(3) 0.67119(18) 0.0479(7) Uani 1 1 d . . . H18 H 0.6345 0.4096 0.6897 0.058 Uiso 1 1 calc R . . C19 C 0.7207(3) 0.2695(2) 0.69409(17) 0.0417(6) Uani 1 1 d . . . C20 C 0.6275(3) 0.4878(3) 0.79964(19) 0.0455(7) Uani 1 1 d . . . C21 C 0.5834(3) 0.4126(3) 0.8432(2) 0.0563(8) Uani 1 1 d . . . H21 H 0.6332 0.3489 0.8581 0.068 Uiso 1 1 calc R . . C22 C 0.4667(4) 0.4281(4) 0.8659(3) 0.0776(14) Uani 1 1 d . . . H22 H 0.4389 0.3762 0.8975 0.093 Uiso 1 1 calc R . . C23 C 0.3917(4) 0.5235(5) 0.8403(4) 0.0875(17) Uani 1 1 d . . . H23 H 0.3132 0.5354 0.8549 0.105 Uiso 1 1 calc R . . C24 C 0.4333(3) 0.5982(4) 0.7945(4) 0.0849(17) Uani 1 1 d . . . H24 H 0.3818 0.6605 0.7763 0.102 Uiso 1 1 calc R . . C25 C 0.5531(3) 0.5851(3) 0.7730(2) 0.0577(9) Uani 1 1 d . . . C26 C 0.5926(3) 0.6690(3) 0.7222(3) 0.0656(11) Uani 1 1 d . . . C27 C 0.5072(5) 0.7557(4) 0.6712(5) 0.112(2) Uani 1 1 d . . . H27A H 0.5434 0.8054 0.6411 0.168 Uiso 1 1 calc R . . H27B H 0.4423 0.7821 0.7038 0.168 Uiso 1 1 calc R . . H27C H 0.4819 0.7344 0.6365 0.168 Uiso 1 1 calc R . . C28 C 0.7290(4) 0.7565(3) 0.6620(3) 0.0709(12) Uani 1 1 d . . . H28A H 0.7157 0.7645 0.6096 0.085 Uiso 1 1 calc R . . H28B H 0.6797 0.8146 0.6753 0.085 Uiso 1 1 calc R . . C29 C 0.8507(4) 0.7488(3) 0.6625(2) 0.0656(10) Uani 1 1 d . . . H29A H 0.8660 0.8071 0.6241 0.079 Uiso 1 1 calc R . . H29B H 0.8994 0.6929 0.6460 0.079 Uiso 1 1 calc R . . C30 C 0.8840(4) 0.7376(2) 0.7396(3) 0.0617(9) Uani 1 1 d . . . H30A H 0.9510 0.7596 0.7312 0.074 Uiso 1 1 calc R . . H30B H 0.8217 0.7781 0.7656 0.074 Uiso 1 1 calc R . . C31 C 0.9836(3) 0.6006(2) 0.84133(19) 0.0428(6) Uani 1 1 d . . . C32 C 1.0253(4) 0.6713(3) 0.8592(3) 0.0645(10) Uani 1 1 d . . . H32A H 0.9866 0.7374 0.8297 0.097 Uiso 1 1 calc R . . H32B H 1.1067 0.6578 0.8452 0.097 Uiso 1 1 calc R . . H32C H 1.0092 0.6637 0.9141 0.097 Uiso 1 1 calc R . . C33 C 1.0332(2) 0.4951(2) 0.88126(16) 0.0374(5) Uani 1 1 d . . . C34 C 1.1126(3) 0.4642(3) 0.93782(19) 0.0486(7) Uani 1 1 d . . . H34 H 1.1242 0.5114 0.9534 0.058 Uiso 1 1 calc R . . C35 C 1.1719(3) 0.3682(3) 0.9698(2) 0.0552(8) Uani 1 1 d . . . H35 H 1.2238 0.3509 1.0060 0.066 Uiso 1 1 calc R . . C36 C 1.1552(3) 0.2963(3) 0.94881(18) 0.0489(7) Uani 1 1 d . . . H36 H 1.1965 0.2307 0.9701 0.059 Uiso 1 1 calc R . . C37 C 1.0767(3) 0.3227(2) 0.89584(17) 0.0419(6) Uani 1 1 d . . . H37 H 1.0646 0.2738 0.8829 0.050 Uiso 1 1 calc R . . C38 C 1.0149(2) 0.4208(2) 0.86113(15) 0.0346(5) Uani 1 1 d . . . C39 C 0.8836(2) 0.5309(2) 0.59065(16) 0.0381(6) Uani 1 1 d . . . C40 C 0.7687(3) 0.5447(3) 0.5844(2) 0.0541(8) Uani 1 1 d . . . H40 H 0.7319 0.5013 0.6209 0.065 Uiso 1 1 calc R . . C41 C 0.7084(3) 0.6205(3) 0.5260(2) 0.0644(10) Uani 1 1 d . . . H41 H 0.6314 0.6287 0.5241 0.077 Uiso 1 1 calc R . . C42 C 0.7617(4) 0.6838(3) 0.4706(2) 0.0672(11) Uani 1 1 d . . . H42 H 0.7218 0.7342 0.4302 0.081 Uiso 1 1 calc R . . C43 C 0.8745(3) 0.6722(2) 0.47531(19) 0.0534(8) Uani 1 1 d . . . H43 H 0.9096 0.7160 0.4378 0.064 Uiso 1 1 calc R . . C44 C 0.9396(3) 0.5961(2) 0.53511(15) 0.0386(6) Uani 1 1 d . . . C45 C 1.0571(3) 0.5945(2) 0.53876(16) 0.0395(6) Uani 1 1 d . . . C46 C 1.1041(4) 0.6708(3) 0.4745(2) 0.0629(10) Uani 1 1 d . . . H46A H 1.1808 0.6621 0.4835 0.094 Uiso 1 1 calc R . . H46B H 1.0560 0.7353 0.4746 0.094 Uiso 1 1 calc R . . H46C H 1.1052 0.6633 0.4247 0.094 Uiso 1 1 calc R . . C47 C 1.2241(3) 0.5464(3) 0.6067(2) 0.0514(8) Uani 1 1 d . . . H47A H 1.2271 0.6120 0.5758 0.062 Uiso 1 1 calc R . . H47B H 1.2904 0.4995 0.5893 0.062 Uiso 1 1 calc R . . C48 C 1.2255(3) 0.5306(3) 0.6927(2) 0.0526(8) Uani 1 1 d . . . H48A H 1.2687 0.5697 0.6974 0.063 Uiso 1 1 calc R . . H48B H 1.1473 0.5539 0.7148 0.063 Uiso 1 1 calc R . . C49 C 1.2774(3) 0.4247(3) 0.73977(19) 0.0470(7) Uani 1 1 d . . . H49A H 1.3604 0.4069 0.7288 0.056 Uiso 1 1 calc R . . H49B H 1.2595 0.4177 0.7951 0.056 Uiso 1 1 calc R . . C50 C 1.2869(2) 0.2644(2) 0.74962(17) 0.0424(6) Uani 1 1 d . . . C51 C 1.3862(3) 0.2268(3) 0.7989(2) 0.0630(10) Uani 1 1 d . . . H51A H 1.4008 0.2812 0.8049 0.094 Uiso 1 1 calc R . . H51B H 1.4535 0.1908 0.7738 0.094 Uiso 1 1 calc R . . H51C H 1.3674 0.1844 0.8495 0.094 Uiso 1 1 calc R . . C52 C 1.2510(3) 0.1913(2) 0.73390(17) 0.0431(6) Uani 1 1 d . . . C53 C 1.3340(3) 0.1034(3) 0.7292(2) 0.0613(10) Uani 1 1 d . . . H53 H 1.4094 0.0915 0.7379 0.074 Uiso 1 1 calc R . . C54 C 1.3062(4) 0.0354(3) 0.7121(3) 0.0769(13) Uani 1 1 d . . . H54 H 1.3626 -0.0223 0.7089 0.092 Uiso 1 1 calc R . . C55 C 1.1945(5) 0.0517(3) 0.6995(3) 0.0709(12) Uani 1 1 d . . . H55 H 1.1762 0.0056 0.6866 0.085 Uiso 1 1 calc R . . C56 C 1.1089(3) 0.1373(2) 0.7062(2) 0.0512(7) Uani 1 1 d . . . H56 H 1.0333 0.1471 0.6993 0.061 Uiso 1 1 calc R . . C57 C 1.1367(2) 0.2075(2) 0.72308(15) 0.0375(5) Uani 1 1 d . . . N1 N 0.8741(2) 0.02784(19) 0.92210(16) 0.0470(6) Uani 1 1 d . . . N2 N 0.8577(3) 0.0611(2) 0.75267(18) 0.0518(6) Uani 1 1 d . . . N3 N 0.6970(3) 0.6691(2) 0.71798(19) 0.0536(7) Uani 1 1 d . . . N4 N 0.9103(2) 0.63361(18) 0.78994(17) 0.0453(6) Uani 1 1 d . . . N5 N 1.1171(2) 0.53315(17) 0.59612(14) 0.0384(5) Uani 1 1 d . . . N6 N 1.2351(2) 0.35686(18) 0.72225(14) 0.0385(5) Uani 1 1 d . . . O1 O 0.87185(19) 0.22088(14) 0.87142(11) 0.0403(4) Uani 1 1 d . . . O2 O 0.79967(19) 0.25814(15) 0.73874(12) 0.0421(4) Uani 1 1 d . . . O3 O 0.74109(17) 0.46909(15) 0.77926(13) 0.0430(5) Uani 1 1 d . . . O4 O 0.94352(18) 0.43938(14) 0.80936(13) 0.0404(4) Uani 1 1 d . . . O5 O 0.93236(17) 0.45620(16) 0.65015(12) 0.0434(5) Uani 1 1 d . . . O6 O 1.05439(16) 0.29032(13) 0.72659(12) 0.0383(4) Uani 1 1 d . . . O7 O 0.1940(5) 0.7960(5) 0.6960(3) 0.159(3) Uani 1 1 d . . . O8 O 0.2827(5) 0.7629(5) 0.5840(4) 0.153(2) Uani 1 1 d . . . O9 O 0.1894(13) 0.9118(5) 0.5843(5) 0.287(7) Uani 1 1 d . . . O10 O 0.0953(7) 0.8102(9) 0.6001(5) 0.236(5) Uani 1 1 d . . . O11 O 0.5633(12) 0.8366(14) 0.8365(12) 0.396(11) Uani 1 1 d . . . O12 O 0.6357(15) 0.9744(12) 0.7876(17) 0.58(2) Uani 1 1 d . . . O13 O 0.6989(7) 0.8384(8) 0.8814(5) 0.230(5) Uani 1 1 d . . . O14 O 0.5220(12) 0.9266(12) 0.8970(11) 0.382(10) Uani 1 1 d . . . O15 O 0.6955(5) 0.5799(5) 0.9082(3) 0.144(2) Uani 1 1 d . . . O16 O 0.6388(3) 0.1488(4) 0.8676(3) 0.1114(14) Uani 1 1 d . . . Cl1 Cl 0.18771(11) 0.82115(9) 0.61745(8) 0.0758(3) Uani 1 1 d . . . Cl2 Cl 0.6043(2) 0.8914(2) 0.8580(3) 0.1877(14) Uani 1 1 d . . . Mn1 Mn 0.87938(3) 0.34596(3) 0.76555(2) 0.03214(10) Uani 1 1 d . . . Cu1 Cu 0.84078(3) 0.13719(2) 0.82444(2) 0.03966(10) Uani 1 1 d . . . Cu2 Cu 0.81965(3) 0.55909(2) 0.77685(2) 0.04030(10) Uani 1 1 d . . . Cu3 Cu 1.08950(3) 0.41264(2) 0.670580(19) 0.03370(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 C1 0.0466(15) 0.0449(15) 0.0362(13) -0.0092(11) -0.0101(11) -0.0226(12) C2 0.064(2) 0.0550(18) 0.0441(16) -0.0174(14) -0.0047(14) -0.0283(16) C3 0.104(3) 0.077(3) 0.053(2) -0.034(2) 0.010(2) -0.041(3) C4 0.132(5) 0.096(4) 0.057(2) -0.036(2) 0.031(3) -0.055(3) C5 0.097(3) 0.080(3) 0.045(2) -0.0102(19) 0.008(2) -0.046(3) C6 0.0614(19) 0.0538(18) 0.0374(15) -0.0055(12) -0.0076(13) -0.0315(15) C7 0.069(2) 0.0450(16) 0.0451(17) 0.0031(13) -0.0178(15) -0.0338(15) C8 0.121(4) 0.056(2) 0.055(2) 0.0038(17) -0.016(2) -0.046(2) C9 0.082(3) 0.0333(15) 0.071(2) -0.0020(15) -0.025(2) -0.0231(16) C10 0.067(2) 0.0341(15) 0.086(3) -0.0163(16) -0.015(2) -0.0158(15) C11 0.092(3) 0.0387(17) 0.083(3) -0.0275(17) -0.019(2) -0.0185(18) C12 0.078(2) 0.0511(18) 0.058(2) -0.0242(15) -0.0155(17) -0.0285(17) C13 0.162(6) 0.078(3) 0.092(4) -0.049(3) -0.047(4) -0.020(3) C14 0.068(2) 0.069(2) 0.0479(18) -0.0203(16) -0.0122(15) -0.0362(18) C15 0.104(4) 0.104(4) 0.083(3) -0.033(3) -0.047(3) -0.042(3) C16 0.082(3) 0.131(5) 0.086(3) -0.037(3) -0.046(3) -0.029(3) C17 0.055(2) 0.088(3) 0.060(2) -0.010(2) -0.0190(17) -0.019(2) C18 0.0437(15) 0.0584(19) 0.0395(15) -0.0091(13) -0.0055(12) -0.0184(13) C19 0.0458(15) 0.0515(16) 0.0347(13) -0.0092(11) -0.0068(11) -0.0255(13) C20 0.0375(14) 0.0600(18) 0.0516(17) -0.0335(15) -0.0040(12) -0.0131(13) C21 0.0454(17) 0.080(2) 0.058(2) -0.0316(18) 0.0003(14) -0.0289(17) C22 0.057(2) 0.132(4) 0.081(3) -0.063(3) 0.018(2) -0.057(3) C23 0.046(2) 0.132(5) 0.127(4) -0.096(4) 0.016(2) -0.034(3) C24 0.0434(19) 0.109(4) 0.130(4) -0.089(4) -0.018(2) 0.003(2) C25 0.0394(15) 0.068(2) 0.080(3) -0.052(2) -0.0105(15) -0.0015(14) C26 0.058(2) 0.052(2) 0.094(3) -0.040(2) -0.031(2) 0.0056(16) C27 0.081(3) 0.071(3) 0.168(6) -0.019(4) -0.062(4) 0.004(3) C28 0.099(3) 0.0350(16) 0.076(3) -0.0112(16) -0.032(2) -0.0093(18) C29 0.097(3) 0.0383(17) 0.064(2) -0.0133(15) -0.008(2) -0.0252(18) C30 0.077(2) 0.0350(16) 0.081(3) -0.0202(16) -0.015(2) -0.0207(16) C31 0.0485(15) 0.0434(15) 0.0501(16) -0.0265(13) 0.0071(13) -0.0243(12) C32 0.079(3) 0.056(2) 0.083(3) -0.0324(19) -0.010(2) -0.0372(19) C33 0.0429(14) 0.0436(14) 0.0364(13) -0.0197(11) 0.0025(10) -0.0220(11) C34 0.0555(17) 0.067(2) 0.0423(16) -0.0269(14) -0.0003(13) -0.0338(16) C35 0.064(2) 0.069(2) 0.0428(17) -0.0127(15) -0.0143(15) -0.0315(17) C36 0.0580(18) 0.0497(17) 0.0381(15) -0.0028(12) -0.0124(13) -0.0223(14) C37 0.0521(16) 0.0378(14) 0.0416(15) -0.0091(11) -0.0120(12) -0.0195(12) C38 0.0363(12) 0.0397(13) 0.0335(12) -0.0137(10) -0.0011(10) -0.0173(10) C39 0.0406(13) 0.0406(14) 0.0309(12) -0.0087(10) -0.0070(10) -0.0103(11) C40 0.0431(16) 0.071(2) 0.0421(16) -0.0052(15) -0.0128(13) -0.0180(15) C41 0.0496(18) 0.082(3) 0.0512(19) -0.0067(18) -0.0219(15) -0.0126(17) C42 0.070(2) 0.067(2) 0.0441(18) -0.0029(16) -0.0236(17) -0.0012(18) C43 0.067(2) 0.0446(16) 0.0366(15) -0.0022(12) -0.0115(14) -0.0106(14) C44 0.0486(15) 0.0352(13) 0.0288(12) -0.0094(10) -0.0047(11) -0.0090(11) C45 0.0515(15) 0.0358(13) 0.0314(12) -0.0108(10) 0.0039(11) -0.0178(11) C46 0.081(3) 0.060(2) 0.0450(18) -0.0013(15) 0.0015(17) -0.0376(19) C47 0.0482(16) 0.0561(18) 0.0535(18) -0.0062(14) -0.0026(14) -0.0327(14) C48 0.0583(19) 0.0533(18) 0.059(2) -0.0208(15) -0.0079(15) -0.0279(15) C49 0.0453(15) 0.0601(19) 0.0457(16) -0.0180(14) -0.0072(12) -0.0247(14) C50 0.0334(13) 0.0514(16) 0.0373(14) -0.0087(12) -0.0064(10) -0.0104(11) C51 0.0498(18) 0.067(2) 0.066(2) -0.0054(18) -0.0282(17) -0.0136(16) C52 0.0437(14) 0.0388(14) 0.0387(14) -0.0062(11) -0.0065(11) -0.0074(11) C53 0.0526(19) 0.0452(18) 0.066(2) -0.0083(16) -0.0069(16) 0.0004(14) C54 0.085(3) 0.0419(19) 0.088(3) -0.0243(19) -0.004(2) 0.0014(19) C55 0.101(3) 0.0414(18) 0.071(3) -0.0253(17) 0.004(2) -0.022(2) C56 0.069(2) 0.0388(15) 0.0492(17) -0.0125(13) -0.0037(15) -0.0229(14) C57 0.0445(14) 0.0323(12) 0.0302(12) -0.0040(9) -0.0046(10) -0.0105(10) N1 0.0594(15) 0.0363(12) 0.0486(14) -0.0021(10) -0.0155(12) -0.0241(11) N2 0.0671(17) 0.0419(14) 0.0595(17) -0.0188(12) -0.0112(14) -0.0260(12) N3 0.0587(16) 0.0380(13) 0.0683(18) -0.0247(13) -0.0163(14) -0.0053(11) N4 0.0518(14) 0.0338(12) 0.0584(15) -0.0221(11) -0.0012(12) -0.0166(10) N5 0.0410(12) 0.0370(11) 0.0388(12) -0.0096(9) -0.0016(9) -0.0173(9) N6 0.0364(11) 0.0440(12) 0.0377(12) -0.0114(9) -0.0050(9) -0.0159(9) O1 0.0568(12) 0.0358(10) 0.0351(10) -0.0084(7) -0.0078(8) -0.0231(9) O2 0.0536(12) 0.0357(10) 0.0453(11) -0.0082(8) -0.0192(9) -0.0195(8) O3 0.0351(9) 0.0391(10) 0.0592(13) -0.0212(9) -0.0028(9) -0.0114(8) O4 0.0466(10) 0.0314(9) 0.0513(11) -0.0169(8) -0.0144(9) -0.0116(8) O5 0.0364(9) 0.0481(11) 0.0373(10) 0.0030(8) -0.0088(8) -0.0168(8) O6 0.0372(9) 0.0304(9) 0.0471(11) -0.0113(8) -0.0027(8) -0.0117(7) O7 0.145(5) 0.202(6) 0.087(3) -0.037(4) -0.012(3) -0.010(4) O8 0.128(4) 0.204(6) 0.154(5) -0.108(5) 0.025(4) -0.051(4) O9 0.57(2) 0.110(5) 0.207(8) -0.036(5) -0.050(11) -0.143(9) O10 0.146(6) 0.378(14) 0.235(9) -0.088(9) -0.043(6) -0.133(7) O11 0.289(15) 0.54(3) 0.56(3) -0.31(2) 0.097(16) -0.293(18) O12 0.326(19) 0.278(16) 0.96(5) 0.19(2) -0.20(3) -0.209(15) O13 0.145(6) 0.300(11) 0.189(7) -0.064(7) -0.059(5) 0.013(7) O14 0.273(12) 0.48(2) 0.57(2) -0.44(2) 0.224(14) -0.192(13) O15 0.167(5) 0.218(6) 0.110(3) -0.074(4) -0.015(3) -0.108(5) O16 0.081(2) 0.125(3) 0.119(3) -0.007(3) -0.045(2) -0.033(2) Cl1 0.0817(7) 0.0688(6) 0.0852(7) -0.0295(5) -0.0148(6) -0.0231(5) Cl2 0.0807(11) 0.172(2) 0.332(5) -0.135(3) -0.0370(19) 0.0033(14) Mn1 0.03391(19) 0.02822(18) 0.0377(2) -0.01008(14) -0.00544(15) -0.01260(14) Cu1 0.0547(2) 0.03109(17) 0.04021(19) -0.00769(13) -0.01300(15) -0.02007(14) Cu2 0.04279(19) 0.03080(17) 0.0527(2) -0.01727(14) -0.00997(15) -0.01012(13) Cu3 0.03334(16) 0.03218(16) 0.03581(17) -0.00663(12) -0.00543(12) -0.01316(12) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag C1 O1 1.336(4) . ? C1 C2 1.393(5) . ? C1 C6 1.426(4) . ? C2 C3 1.368(5) . ? C3 C4 1.383(7) . ? C4 C5 1.359(7) . ? C5 C6 1.406(6) . ? C6 C7 1.464(5) . ? C7 N1 1.292(5) . ? C7 C8 1.521(5) . ? C9 N1 1.465(5) . ? C9 C10 1.498(6) . ? C10 C11 1.492(6) . ? C11 N2 1.483(5) . ? C12 N2 1.286(5) . ? C12 C14 1.469(6) . ? C12 C13 1.514(6) . ? C14 C19 1.406(5) . ? C14 C15 1.419(5) . ? C15 C16 1.349(8) . ? C16 C17 1.363(8) . ? C17 C18 1.378(5) . ? C18 C19 1.391(5) . ? C19 O2 1.339(3) . ? C20 O3 1.342(4) . ? C20 C21 1.365(5) . ? C20 C25 1.419(5) . ? C21 C22 1.388(5) . ? C22 C23 1.400(8) . ? C23 C24 1.352(9) . ? C24 C25 1.425(6) . ? C25 C26 1.467(7) . ? C26 N3 1.289(5) . ? C26 C27 1.518(6) . ? C28 C29 1.483(7) . ? C28 N3 1.490(5) . ? C29 C30 1.496(6) . ? C30 N4 1.482(4) . ? C31 N4 1.295(4) . ? C31 C33 1.472(4) . ? C31 C32 1.509(4) . ? C33 C38 1.417(4) . ? C33 C34 1.426(4) . ? C34 C35 1.360(5) . ? C35 C36 1.382(5) . ? C36 C37 1.382(4) . ? C37 C38 1.400(4) . ? C38 O4 1.328(3) . ? C39 O5 1.327(3) . ? C39 C40 1.397(4) . ? C39 C44 1.408(4) . ? C40 C41 1.375(5) . ? C41 C42 1.370(6) . ? C42 C43 1.373(6) . ? C43 C44 1.418(4) . ? C44 C45 1.473(4) . ? C45 N5 1.294(4) . ? C45 C46 1.516(4) . ? C47 N5 1.479(4) . ? C47 C48 1.516(5) . ? C48 C49 1.511(5) . ? C49 N6 1.471(4) . ? C50 N6 1.286(4) . ? C50 C52 1.477(5) . ? C50 C51 1.510(4) . ? C52 C53 1.401(5) . ? C52 C57 1.404(4) . ? C53 C54 1.357(7) . ? C54 C55 1.381(7) . ? C55 C56 1.398(5) . ? C56 C57 1.387(5) . ? C57 O6 1.337(3) . ? N1 Cu1 1.963(3) . ? N2 Cu1 1.994(3) . ? N3 Cu2 1.979(3) . ? N4 Cu2 1.965(3) . ? N5 Cu3 1.955(2) . ? N6 Cu3 1.995(2) . ? O1 Cu1 1.958(2) . ? O1 Mn1 2.196(2) . ? O2 Cu1 1.934(2) . ? O2 Mn1 2.161(2) . ? O3 Cu2 1.937(2) . ? O3 Mn1 2.116(2) . ? O4 Cu2 1.927(2) . ? O4 Mn1 2.292(2) . ? O5 Cu3 1.908(2) . ? O5 Mn1 2.324(2) . ? O6 Cu3 1.938(2) . ? O6 Mn1 2.119(2) . ? O7 Cl1 1.367(5) . ? O8 Cl1 1.390(6) . ? O9 Cl1 1.306(7) . ? O10 Cl1 1.337(7) . ? O11 Cl2 1.323(13) . ? O12 Cl2 1.546(16) . ? O13 Cl2 1.235(7) . ? O14 Cl2 1.202(9) . ? Mn1 Cu3 3.1054(11) . ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag O1 C1 C2 118.5(3) . . ? O1 C1 C6 122.6(3) . . ? C2 C1 C6 118.9(3) . . ? C3 C2 C1 121.3(3) . . ? C2 C3 C4 119.9(4) . . ? C5 C4 C3 120.4(4) . . ? C4 C5 C6 121.7(4) . . ? C5 C6 C1 117.5(3) . . ? C5 C6 C7 119.5(3) . . ? C1 C6 C7 122.8(3) . . ? N1 C7 C6 122.0(3) . . ? N1 C7 C8 120.2(3) . . ? C6 C7 C8 117.8(3) . . ? N1 C9 C10 110.9(3) . . ? C11 C10 C9 114.9(4) . . ? N2 C11 C10 113.2(3) . . ? N2 C12 C14 121.9(3) . . ? N2 C12 C13 121.0(4) . . ? C14 C12 C13 117.1(4) . . ? C19 C14 C15 117.1(4) . . ? C19 C14 C12 123.1(3) . . ? C15 C14 C12 119.9(4) . . ? C16 C15 C14 122.2(4) . . ? C15 C16 C17 120.4(4) . . ? C16 C17 C18 119.6(4) . . ? C17 C18 C19 121.5(4) . . ? O2 C19 C18 118.9(3) . . ? O2 C19 C14 122.0(3) . . ? C18 C19 C14 119.0(3) . . ? O3 C20 C21 119.9(3) . . ? O3 C20 C25 119.8(3) . . ? C21 C20 C25 120.2(3) . . ? C20 C21 C22 122.1(4) . . ? C21 C22 C23 118.6(5) . . ? C24 C23 C22 120.0(4) . . ? C23 C24 C25 122.5(5) . . ? C20 C25 C24 116.4(4) . . ? C20 C25 C26 123.7(3) . . ? C24 C25 C26 119.8(4) . . ? N3 C26 C25 122.1(3) . . ? N3 C26 C27 120.2(5) . . ? C25 C26 C27 117.7(4) . . ? C29 C28 N3 112.9(3) . . ? C28 C29 C30 115.2(4) . . ? N4 C30 C29 110.4(3) . . ? N4 C31 C33 122.5(3) . . ? N4 C31 C32 119.8(3) . . ? C33 C31 C32 117.6(3) . . ? C38 C33 C34 117.2(3) . . ? C38 C33 C31 123.2(3) . . ? C34 C33 C31 119.4(3) . . ? C35 C34 C33 122.3(3) . . ? C34 C35 C36 120.2(3) . . ? C37 C36 C35 119.4(3) . . ? C36 C37 C38 121.9(3) . . ? O4 C38 C37 117.7(2) . . ? O4 C38 C33 123.4(2) . . ? C37 C38 C33 118.9(3) . . ? O5 C39 C40 116.6(3) . . ? O5 C39 C44 124.4(3) . . ? C40 C39 C44 119.0(3) . . ? C41 C40 C39 122.0(3) . . ? C42 C41 C40 119.9(3) . . ? C41 C42 C43 119.4(3) . . ? C42 C43 C44 122.7(3) . . ? C39 C44 C43 117.0(3) . . ? C39 C44 C45 124.3(2) . . ? C43 C44 C45 118.5(3) . . ? N5 C45 C44 121.7(2) . . ? N5 C45 C46 120.7(3) . . ? C44 C45 C46 117.5(3) . . ? N5 C47 C48 108.5(3) . . ? C49 C48 C47 113.8(3) . . ? N6 C49 C48 112.6(2) . . ? N6 C50 C52 121.0(3) . . ? N6 C50 C51 121.4(3) . . ? C52 C50 C51 117.6(3) . . ? C53 C52 C57 119.1(3) . . ? C53 C52 C50 118.8(3) . . ? C57 C52 C50 122.1(3) . . ? C54 C53 C52 121.1(4) . . ? C53 C54 C55 120.1(4) . . ? C54 C55 C56 120.2(4) . . ? C57 C56 C55 119.9(4) . . ? O6 C57 C56 119.1(3) . . ? O6 C57 C52 121.4(3) . . ? C56 C57 C52 119.4(3) . . ? C7 N1 C9 120.2(3) . . ? C7 N1 Cu1 121.9(2) . . ? C9 N1 Cu1 117.3(2) . . ? C12 N2 C11 117.8(3) . . ? C12 N2 Cu1 124.1(2) . . ? C11 N2 Cu1 118.1(2) . . ? C26 N3 C28 117.6(3) . . ? C26 N3 Cu2 124.8(3) . . ? C28 N3 Cu2 117.5(3) . . ? C31 N4 C30 119.2(3) . . ? C31 N4 Cu2 125.2(2) . . ? C30 N4 Cu2 115.4(2) . . ? C45 N5 C47 120.2(3) . . ? C45 N5 Cu3 126.9(2) . . ? C47 N5 Cu3 112.76(19) . . ? C50 N6 C49 117.5(3) . . ? C50 N6 Cu3 124.2(2) . . ? C49 N6 Cu3 117.79(19) . . ? C1 O1 Cu1 118.20(17) . . ? C1 O1 Mn1 129.31(18) . . ? Cu1 O1 Mn1 98.94(9) . . ? C19 O2 Cu1 117.93(18) . . ? C19 O2 Mn1 139.50(19) . . ? Cu1 O2 Mn1 100.93(9) . . ? C20 O3 Cu2 120.65(19) . . ? C20 O3 Mn1 135.9(2) . . ? Cu2 O3 Mn1 102.36(9) . . ? C38 O4 Cu2 124.95(17) . . ? C38 O4 Mn1 135.28(17) . . ? Cu2 O4 Mn1 96.64(8) . . ? C39 O5 Cu3 126.74(18) . . ? C39 O5 Mn1 139.09(18) . . ? Cu3 O5 Mn1 93.91(8) . . ? C57 O6 Cu3 117.11(17) . . ? C57 O6 Mn1 142.82(18) . . ? Cu3 O6 Mn1 99.78(8) . . ? O9 Cl1 O10 110.3(8) . . ? O9 Cl1 O7 108.7(5) . . ? O10 Cl1 O7 113.6(5) . . ? O9 Cl1 O8 107.2(7) . . ? O10 Cl1 O8 106.2(6) . . ? O7 Cl1 O8 110.7(4) . . ? O14 Cl2 O13 125.7(12) . . ? O14 Cl2 O11 100.6(9) . . ? O13 Cl2 O11 106.0(10) . . ? O14 Cl2 O12 109.4(13) . . ? O13 Cl2 O12 102.7(8) . . ? O11 Cl2 O12 112.5(14) . . ? O3 Mn1 O6 147.67(8) . . ? O3 Mn1 O2 104.26(9) . . ? O6 Mn1 O2 102.33(9) . . ? O3 Mn1 O1 107.74(9) . . ? O6 Mn1 O1 97.52(8) . . ? O2 Mn1 O1 72.55(8) . . ? O3 Mn1 O4 70.48(8) . . ? O6 Mn1 O4 84.88(8) . . ? O2 Mn1 O4 171.52(9) . . ? O1 Mn1 O4 102.32(8) . . ? O3 Mn1 O5 84.98(9) . . ? O6 Mn1 O5 68.92(7) . . ? O2 Mn1 O5 109.52(8) . . ? O1 Mn1 O5 166.44(8) . . ? O4 Mn1 O5 77.09(8) . . ? O3 Mn1 Cu3 110.04(6) . . ? O6 Mn1 Cu3 37.96(5) . . ? O2 Mn1 Cu3 126.09(7) . . ? O1 Mn1 Cu3 129.86(6) . . ? O4 Mn1 Cu3 62.39(6) . . ? O5 Mn1 Cu3 37.80(5) . . ? O2 Cu1 O1 82.97(9) . . ? O2 Cu1 N1 170.88(11) . . ? O1 Cu1 N1 89.17(10) . . ? O2 Cu1 N2 89.82(11) . . ? O1 Cu1 N2 159.89(11) . . ? N1 Cu1 N2 99.10(12) . . ? O4 Cu2 O3 82.49(9) . . ? O4 Cu2 N4 90.07(10) . . ? O3 Cu2 N4 170.54(11) . . ? O4 Cu2 N3 163.80(11) . . ? O3 Cu2 N3 89.02(11) . . ? N4 Cu2 N3 99.57(12) . . ? O5 Cu3 O6 81.85(9) . . ? O5 Cu3 N5 92.55(9) . . ? O6 Cu3 N5 168.71(10) . . ? O5 Cu3 N6 164.28(10) . . ? O6 Cu3 N6 89.08(9) . . ? N5 Cu3 N6 98.45(10) . . ? O5 Cu3 Mn1 48.29(6) . . ? O6 Cu3 Mn1 42.26(6) . . ? N5 Cu3 Mn1 137.20(7) . . ? N6 Cu3 Mn1 117.33(7) . . ? _diffrn_measured_fraction_theta_max 0.945 _diffrn_reflns_theta_full 32.30 _diffrn_measured_fraction_theta_full 0.945 _refine_diff_density_max 1.585 _refine_diff_density_min -1.018 _refine_diff_density_rms 0.116 data_2 _database_code_depnum_ccdc_archive 'CCDC 833842' #TrackingRef '- 1-4.cif' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety 'C38 H40 Cu2 Mn N10 O4' _chemical_formula_sum 'C38 H40 Cu2 Mn N10 O4' _chemical_formula_weight 882.84 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' Cu Cu 0.3201 1.2651 '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 22.7481(6) _cell_length_b 10.0972(3) _cell_length_c 17.6258(5) _cell_angle_alpha 90.00 _cell_angle_beta 97.2420(10) _cell_angle_gamma 90.00 _cell_volume 4016.2(2) _cell_formula_units_Z 4 _cell_measurement_temperature 150(2) _cell_measurement_reflns_used 9007 _cell_measurement_theta_min 1.8 _cell_measurement_theta_max 35.3 _exptl_crystal_description RECTANGULAR _exptl_crystal_colour Green _exptl_crystal_size_max 0.30 _exptl_crystal_size_mid 0.08 _exptl_crystal_size_min 0.08 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.46 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 2034 _exptl_absorpt_coefficient_mu 1.411 _exptl_absorpt_correction_type EMPIRICAL _exptl_absorpt_correction_T_min 0.5737 _exptl_absorpt_correction_T_max 0.8510 _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 39682 _diffrn_reflns_av_R_equivalents 0.0284 _diffrn_reflns_av_sigmaI/netI 0.0301 _diffrn_reflns_limit_h_min -36 _diffrn_reflns_limit_h_max 36 _diffrn_reflns_limit_k_min -15 _diffrn_reflns_limit_k_max 16 _diffrn_reflns_limit_l_min -28 _diffrn_reflns_limit_l_max 25 _diffrn_reflns_theta_min 1.80 _diffrn_reflns_theta_max 35.35 _reflns_number_total 9007 _reflns_number_gt 5696 _reflns_threshold_expression >2sigma(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 V1.80.03' _refine_special_details ; Refinement of F^2^ against ALL reflections. The weighted R-factor wR and goodness of fit S are based on F^2^, conventional R-factors R are based on F, with F set to zero for negative F^2^. The threshold expression of F^2^ > 2sigma(F^2^) is used only for calculating R-factors(gt) etc. and is not relevant to the choice of reflections for refinement. R-factors based on F^2^ are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger. ; _refine_ls_structure_factor_coef Fsqd _refine_ls_matrix_type full _refine_ls_weighting_scheme calc _refine_ls_weighting_details 'calc w=1/[\s^2^(Fo^2^)+(0.1267P)^2^+1.1389P] 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 8948 _refine_ls_number_parameters 249 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0854 _refine_ls_R_factor_gt 0.0532 _refine_ls_wR_factor_ref 0.2098 _refine_ls_wR_factor_gt 0.1874 _refine_ls_goodness_of_fit_ref 1.053 _refine_ls_restrained_S_all 1.053 _refine_ls_shift/su_max 0.087 _refine_ls_shift/su_mean 0.010 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 Cu1 Cu 0.934843(11) 0.02119(3) 0.682509(16) 0.03872(11) Uani 1 1 d . . . Mn1 Mn 1.0000 -0.23921(5) 0.7500 0.04558(14) Uani 1 2 d S . . O1 O 1.01476(8) -0.03195(18) 0.67922(10) 0.0451(4) Uani 1 1 d . . . N5 N 1.11473(18) -0.4419(5) 0.6255(3) 0.1088(14) Uani 1 1 d . . . O2 O 0.91878(8) -0.16498(17) 0.69669(11) 0.0484(4) Uani 1 1 d . . . N1 N 0.95260(10) 0.1937(2) 0.64065(14) 0.0497(5) Uani 1 1 d . . . N2 N 0.85500(10) 0.0628(2) 0.70652(15) 0.0525(5) Uani 1 1 d . . . C1 C 1.04451(11) -0.0019(2) 0.62189(13) 0.0416(5) Uani 1 1 d . . . N4 N 1.07259(14) -0.4074(3) 0.64965(18) 0.0671(7) Uani 1 1 d . . . C7 C 0.98817(14) 0.2109(3) 0.58896(15) 0.0529(6) Uani 1 1 d . . . N3 N 1.02802(15) -0.3771(3) 0.67217(19) 0.0732(8) Uani 1 1 d . . . C6 C 1.03133(11) 0.1105(3) 0.57389(13) 0.0480(6) Uani 1 1 d . . . C15 C 0.76247(14) -0.2039(4) 0.62379(19) 0.0678(9) Uani 1 1 d . . . H15 H 0.7266 -0.1594 0.6221 0.081 Uiso 1 1 calc R . . C10 C 0.90025(16) 0.2802(3) 0.7436(2) 0.0688(9) Uani 1 1 d . . . H10A H 0.9336 0.2405 0.7754 0.083 Uiso 1 1 calc R . . H10B H 0.8919 0.3645 0.7665 0.083 Uiso 1 1 calc R . . C14 C 0.81408(11) -0.1470(3) 0.66242(15) 0.0505(6) Uani 1 1 d . . . C5 C 1.06626(15) 0.1282(4) 0.51374(16) 0.0654(9) Uani 1 1 d . . . H5 H 1.0579 0.1990 0.4804 0.079 Uiso 1 1 calc R . . C19 C 0.86796(11) -0.2171(2) 0.66448(14) 0.0454(5) Uani 1 1 d . . . C2 C 1.09230(12) -0.0838(3) 0.61045(17) 0.0550(6) Uani 1 1 d . . . H2 H 1.1019 -0.1544 0.6435 0.066 Uiso 1 1 calc R . . C3 C 1.12556(15) -0.0621(5) 0.5512(2) 0.0729(10) Uani 1 1 d . . . H3 H 1.1567 -0.1184 0.5437 0.087 Uiso 1 1 calc R . . C11 C 0.84741(17) 0.1920(4) 0.7440(3) 0.0794(11) Uani 1 1 d . . . H11A H 0.8404 0.1767 0.7964 0.095 Uiso 1 1 calc R . . H11B H 0.8128 0.2363 0.7178 0.095 Uiso 1 1 calc R . . C4 C 1.11161(18) 0.0458(5) 0.50268(19) 0.0804(12) Uani 1 1 d . . . H4 H 1.1335 0.0614 0.4625 0.096 Uiso 1 1 calc R . . C18 C 0.86852(16) -0.3427(3) 0.6323(2) 0.0651(8) Uani 1 1 d . . . H18 H 0.9034 -0.3917 0.6365 0.078 Uiso 1 1 calc R . . C16 C 0.76454(19) -0.3261(4) 0.5881(2) 0.0827(12) Uani 1 1 d . . . H16 H 0.7306 -0.3611 0.5604 0.099 Uiso 1 1 calc R . . C17 C 0.8164(2) -0.3945(4) 0.5938(2) 0.0824(11) Uani 1 1 d . . . H17 H 0.8171 -0.4778 0.5714 0.099 Uiso 1 1 calc R . . C13 C 0.81108(13) -0.0181(4) 0.6998(2) 0.0628(8) Uani 1 1 d . . . C9 C 0.91782(18) 0.3054(3) 0.6652(2) 0.0727(9) Uani 1 1 d . . . H9A H 0.8825 0.3176 0.6289 0.087 Uiso 1 1 calc R . . H9B H 0.9411 0.3859 0.6662 0.087 Uiso 1 1 calc R . . C8 C 0.9880(2) 0.3398(4) 0.5450(2) 0.0868(12) Uani 1 1 d . . . H8A H 0.9577 0.3970 0.5599 0.130 Uiso 1 1 calc R . . H8B H 0.9801 0.3220 0.4911 0.130 Uiso 1 1 calc R . . H8C H 1.0259 0.3821 0.5560 0.130 Uiso 1 1 calc R . . C12 C 0.7533(2) 0.0146(6) 0.7311(4) 0.119(2) Uani 1 1 d . . . H12A H 0.7560 0.1013 0.7537 0.179 Uiso 1 1 calc R . . H12B H 0.7463 -0.0496 0.7692 0.179 Uiso 1 1 calc R . . H12C H 0.7211 0.0127 0.6902 0.179 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 Cu1 0.03712(16) 0.02998(15) 0.04883(19) 0.00020(9) 0.00454(11) 0.00104(9) Mn1 0.0486(3) 0.0335(2) 0.0519(3) 0.000 -0.0048(2) 0.000 O1 0.0450(9) 0.0477(9) 0.0450(9) 0.0138(7) 0.0148(7) 0.0082(7) N5 0.078(2) 0.108(3) 0.142(4) 0.012(3) 0.017(2) 0.032(2) O2 0.0447(8) 0.0350(8) 0.0617(10) 0.0012(7) -0.0080(7) -0.0059(7) N1 0.0552(11) 0.0299(9) 0.0599(12) 0.0041(8) -0.0090(10) -0.0005(8) N2 0.0435(10) 0.0521(12) 0.0619(13) -0.0084(10) 0.0066(9) 0.0066(9) C1 0.0424(11) 0.0469(11) 0.0358(10) 0.0009(8) 0.0064(8) -0.0096(9) N4 0.0720(17) 0.0475(13) 0.0775(17) -0.0023(12) -0.0069(14) 0.0067(12) C7 0.0683(16) 0.0387(11) 0.0462(13) 0.0108(10) -0.0140(11) -0.0160(11) N3 0.0783(18) 0.0560(15) 0.0849(19) -0.0265(14) 0.0086(15) -0.0013(13) C6 0.0540(13) 0.0539(13) 0.0341(10) 0.0042(9) -0.0020(9) -0.0236(11) C15 0.0464(14) 0.088(2) 0.0671(18) 0.0161(17) -0.0012(12) -0.0209(15) C10 0.0682(19) 0.0479(15) 0.086(2) -0.0196(15) -0.0055(16) 0.0155(13) C14 0.0458(12) 0.0589(15) 0.0470(12) 0.0060(11) 0.0066(10) -0.0150(11) C5 0.0691(18) 0.083(2) 0.0439(13) 0.0111(14) 0.0071(12) -0.0318(17) C19 0.0504(12) 0.0428(11) 0.0412(11) 0.0064(9) -0.0017(9) -0.0151(9) C2 0.0471(13) 0.0663(17) 0.0540(14) -0.0046(12) 0.0160(11) -0.0051(12) C3 0.0550(16) 0.103(3) 0.0654(19) -0.0201(19) 0.0254(14) -0.0172(17) C11 0.067(2) 0.069(2) 0.105(3) -0.030(2) 0.0166(19) 0.0156(16) C4 0.074(2) 0.128(3) 0.0429(14) -0.0030(18) 0.0195(14) -0.045(2) C18 0.0700(18) 0.0397(13) 0.081(2) 0.0021(13) -0.0077(15) -0.0128(12) C16 0.077(2) 0.088(3) 0.076(2) 0.0087(19) -0.0185(18) -0.043(2) C17 0.096(3) 0.0547(18) 0.089(2) -0.0063(17) -0.018(2) -0.0283(19) C13 0.0423(14) 0.081(2) 0.0663(18) -0.0075(15) 0.0120(13) -0.0015(13) C9 0.079(2) 0.0369(13) 0.096(2) 0.0023(14) -0.0090(18) 0.0151(14) C8 0.125(3) 0.0518(17) 0.079(2) 0.0286(17) -0.007(2) -0.0164(19) C12 0.060(2) 0.137(5) 0.171(6) -0.050(4) 0.057(3) -0.014(2) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag Cu1 O1 1.9033(18) . ? Cu1 O2 1.9372(17) . ? Cu1 N1 1.954(2) . ? Cu1 N2 1.962(2) . ? Mn1 O2 2.1026(18) 2_756 ? Mn1 O2 2.1026(18) . ? Mn1 N3 2.109(3) 2_756 ? Mn1 N3 2.109(3) . ? Mn1 O1 2.4808(17) . ? Mn1 O1 2.4808(17) 2_756 ? O1 C1 1.320(3) . ? N5 N4 1.150(5) . ? O2 C19 1.330(3) . ? N1 C7 1.304(4) . ? N1 C9 1.474(4) . ? N2 C13 1.284(4) . ? N2 C11 1.482(4) . ? C1 C2 1.400(4) . ? C1 C6 1.425(4) . ? N4 N3 1.175(4) . ? C7 C6 1.459(5) . ? C7 C8 1.514(4) . ? C6 C5 1.414(4) . ? C15 C16 1.388(6) . ? C15 C14 1.404(4) . ? C15 H15 0.9300 . ? C10 C11 1.497(5) . ? C10 C9 1.507(6) . ? C10 H10A 0.9700 . ? C10 H10B 0.9700 . ? C14 C19 1.412(4) . ? C14 C13 1.464(5) . ? C5 C4 1.358(6) . ? C5 H5 0.9300 . ? C19 C18 1.390(4) . ? C2 C3 1.383(4) . ? C2 H2 0.9300 . ? C3 C4 1.396(7) . ? C3 H3 0.9300 . ? C11 H11A 0.9700 . ? C11 H11B 0.9700 . ? C4 H4 0.9300 . ? C18 C17 1.391(5) . ? C18 H18 0.9300 . ? C16 C17 1.361(7) . ? C16 H16 0.9300 . ? C17 H17 0.9300 . ? C13 C12 1.525(5) . ? C9 H9A 0.9700 . ? C9 H9B 0.9700 . ? C8 H8A 0.9600 . ? C8 H8B 0.9600 . ? C8 H8C 0.9600 . ? C12 H12A 0.9600 . ? C12 H12B 0.9600 . ? C12 H12C 0.9600 . ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag O1 Cu1 O2 85.80(8) . . ? O1 Cu1 N1 89.78(9) . . ? O2 Cu1 N1 164.85(9) . . ? O1 Cu1 N2 168.76(9) . . ? O2 Cu1 N2 89.16(10) . . ? N1 Cu1 N2 97.55(10) . . ? O2 Mn1 O2 138.23(9) 2_756 . ? O2 Mn1 N3 105.38(11) 2_756 2_756 ? O2 Mn1 N3 101.86(10) . 2_756 ? O2 Mn1 N3 101.86(10) 2_756 . ? O2 Mn1 N3 105.38(11) . . ? N3 Mn1 N3 97.35(19) 2_756 . ? O2 Mn1 O1 75.94(7) 2_756 . ? O2 Mn1 O1 68.99(7) . . ? N3 Mn1 O1 162.81(10) 2_756 . ? N3 Mn1 O1 99.14(10) . . ? O2 Mn1 O1 68.99(7) 2_756 2_756 ? O2 Mn1 O1 75.94(7) . 2_756 ? N3 Mn1 O1 99.14(10) 2_756 2_756 ? N3 Mn1 O1 162.81(10) . 2_756 ? O1 Mn1 O1 64.96(9) . 2_756 ? C1 O1 Cu1 122.83(16) . . ? C1 O1 Mn1 133.91(16) . . ? Cu1 O1 Mn1 91.84(7) . . ? C19 O2 Cu1 119.79(16) . . ? C19 O2 Mn1 135.80(16) . . ? Cu1 O2 Mn1 103.54(8) . . ? C7 N1 C9 120.4(3) . . ? C7 N1 Cu1 123.97(19) . . ? C9 N1 Cu1 115.3(2) . . ? C13 N2 C11 117.9(3) . . ? C13 N2 Cu1 125.1(2) . . ? C11 N2 Cu1 116.6(2) . . ? O1 C1 C2 117.2(2) . . ? O1 C1 C6 123.2(2) . . ? C2 C1 C6 119.6(2) . . ? N5 N4 N3 176.6(4) . . ? N1 C7 C6 121.7(2) . . ? N1 C7 C8 120.7(3) . . ? C6 C7 C8 117.6(3) . . ? N4 N3 Mn1 137.4(3) . . ? C5 C6 C1 116.7(3) . . ? C5 C6 C7 120.2(3) . . ? C1 C6 C7 122.8(2) . . ? C16 C15 C14 120.7(3) . . ? C16 C15 H15 119.7 . . ? C14 C15 H15 119.7 . . ? C11 C10 C9 114.2(3) . . ? C11 C10 H10A 108.7 . . ? C9 C10 H10A 108.7 . . ? C11 C10 H10B 108.7 . . ? C9 C10 H10B 108.7 . . ? H10A C10 H10B 107.6 . . ? C15 C14 C19 118.5(3) . . ? C15 C14 C13 119.9(3) . . ? C19 C14 C13 121.6(2) . . ? C4 C5 C6 122.6(3) . . ? C4 C5 H5 118.7 . . ? C6 C5 H5 118.7 . . ? O2 C19 C18 118.9(3) . . ? O2 C19 C14 121.1(2) . . ? C18 C19 C14 120.0(2) . . ? C3 C2 C1 121.6(3) . . ? C3 C2 H2 119.2 . . ? C1 C2 H2 119.2 . . ? C2 C3 C4 118.8(4) . . ? C2 C3 H3 120.6 . . ? C4 C3 H3 120.6 . . ? N2 C11 C10 112.5(3) . . ? N2 C11 H11A 109.1 . . ? C10 C11 H11A 109.1 . . ? N2 C11 H11B 109.1 . . ? C10 C11 H11B 109.1 . . ? H11A C11 H11B 107.8 . . ? C5 C4 C3 120.5(3) . . ? C5 C4 H4 119.7 . . ? C3 C4 H4 119.7 . . ? C17 C18 C19 119.4(3) . . ? C17 C18 H18 120.3 . . ? C19 C18 H18 120.3 . . ? C17 C16 C15 119.8(3) . . ? C17 C16 H16 120.1 . . ? C15 C16 H16 120.1 . . ? C16 C17 C18 121.5(4) . . ? C16 C17 H17 119.2 . . ? C18 C17 H17 119.2 . . ? N2 C13 C14 121.8(3) . . ? N2 C13 C12 121.7(4) . . ? C14 C13 C12 116.5(3) . . ? N1 C9 C10 110.8(3) . . ? N1 C9 H9A 109.5 . . ? C10 C9 H9A 109.5 . . ? N1 C9 H9B 109.5 . . ? C10 C9 H9B 109.5 . . ? H9A C9 H9B 108.1 . . ? C7 C8 H8A 109.5 . . ? C7 C8 H8B 109.5 . . ? H8A C8 H8B 109.5 . . ? C7 C8 H8C 109.5 . . ? H8A C8 H8C 109.5 . . ? H8B C8 H8C 109.5 . . ? C13 C12 H12A 109.5 . . ? C13 C12 H12B 109.4 . . ? H12A C12 H12B 109.5 . . ? C13 C12 H12C 109.5 . . ? H12A C12 H12C 109.5 . . ? H12B C12 H12C 109.5 . . ? _diffrn_measured_fraction_theta_max 0.986 _diffrn_reflns_theta_full 35.35 _diffrn_measured_fraction_theta_full 0.986 _refine_diff_density_max 1.633 _refine_diff_density_min -0.340 _refine_diff_density_rms 0.134 data_3 _database_code_depnum_ccdc_archive 'CCDC 833843' #TrackingRef '- 1-4.cif' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety 'C40 H40 Cu2 Mn N6 O6' _chemical_formula_sum 'C40 H40 Cu2 Mn N6 O6' _chemical_formula_weight 882.82 loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Mn Mn 0.3368 0.7283 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Cu Cu 0.3201 1.2651 '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 21.1530(7) _cell_length_b 9.9031(3) _cell_length_c 18.0054(6) _cell_angle_alpha 90.00 _cell_angle_beta 91.8330(10) _cell_angle_gamma 90.00 _cell_volume 3769.8(2) _cell_formula_units_Z 4 _cell_measurement_temperature 150(2) _cell_measurement_reflns_used 6121 _cell_measurement_theta_min 1.93 _cell_measurement_theta_max 31.32 _exptl_crystal_description rectangular _exptl_crystal_colour green _exptl_crystal_size_max 0.30 _exptl_crystal_size_mid 0.08 _exptl_crystal_size_min 0.08 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.555 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1912 _exptl_absorpt_coefficient_mu 1.504 _exptl_absorpt_correction_type EMPIRICAL _exptl_absorpt_correction_T_min 0.6105 _exptl_absorpt_correction_T_max 0.8678 _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 32118 _diffrn_reflns_av_R_equivalents 0.0725 _diffrn_reflns_av_sigmaI/netI 0.0693 _diffrn_reflns_limit_h_min -30 _diffrn_reflns_limit_h_max 30 _diffrn_reflns_limit_k_min -13 _diffrn_reflns_limit_k_max 14 _diffrn_reflns_limit_l_min -26 _diffrn_reflns_limit_l_max 23 _diffrn_reflns_theta_min 1.93 _diffrn_reflns_theta_max 31.32 _reflns_number_total 6121 _reflns_number_gt 3256 _reflns_threshold_expression >2sigma(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 V1.80.03' _refine_special_details ; Refinement of F^2^ against ALL reflections. The weighted R-factor wR and goodness of fit S are based on F^2^, conventional R-factors R are based on F, with F set to zero for negative F^2^. The threshold expression of F^2^ > 2sigma(F^2^) is used only for calculating R-factors(gt) etc. and is not relevant to the choice of reflections for refinement. R-factors based on F^2^ are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger. ; _refine_ls_structure_factor_coef Fsqd _refine_ls_matrix_type full _refine_ls_weighting_scheme calc _refine_ls_weighting_details 'calc w=1/[\s^2^(Fo^2^)+(0.0922P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment constr _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 6121 _refine_ls_number_parameters 249 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.1135 _refine_ls_R_factor_gt 0.0512 _refine_ls_wR_factor_ref 0.1578 _refine_ls_wR_factor_gt 0.1285 _refine_ls_goodness_of_fit_ref 0.899 _refine_ls_restrained_S_all 0.899 _refine_ls_shift/su_max 0.000 _refine_ls_shift/su_mean 0.000 loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_occupancy _atom_site_symmetry_multiplicity _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group Cu1 Cu 0.054695(16) -0.01597(4) 0.18343(2) 0.03918(14) Uani 1 1 d . . . Mn1 Mn 0.0000 -0.29079(6) 0.2500 0.04306(19) Uani 1 2 d S . . O2 O 0.07760(10) -0.2049(2) 0.19225(12) 0.0449(5) Uani 1 1 d . . . O1 O -0.03142(9) -0.0724(2) 0.18544(11) 0.0466(5) Uani 1 1 d . . . N3 N -0.04240(16) -0.4210(3) 0.17332(19) 0.0662(8) Uani 1 1 d . . . N2 N 0.02680(12) 0.1495(3) 0.13228(15) 0.0451(6) Uani 1 1 d . . . C7 C 0.19134(15) -0.0373(3) 0.19120(18) 0.0449(7) Uani 1 1 d . . . C20 C -0.08153(19) -0.4645(4) 0.1354(3) 0.0691(11) Uani 1 1 d . . . C1 C 0.12905(14) -0.2501(3) 0.15991(16) 0.0401(6) Uani 1 1 d . . . N1 N 0.14280(12) 0.0393(3) 0.20077(15) 0.0429(6) Uani 1 1 d . . . C6 C 0.18484(14) -0.1721(3) 0.15690(16) 0.0416(7) Uani 1 1 d . . . C14 C -0.06152(14) 0.0380(3) 0.06990(16) 0.0427(7) Uani 1 1 d . . . C8 C 0.25671(18) 0.0101(4) 0.2136(3) 0.0730(13) Uani 1 1 d . . . H8A H 0.2543 0.0986 0.2351 0.109 Uiso 1 1 calc R . . H8B H 0.2824 0.0133 0.1707 0.109 Uiso 1 1 calc R . . H8C H 0.2752 -0.0513 0.2494 0.109 Uiso 1 1 calc R . . C2 C 0.12768(17) -0.3774(3) 0.12704(19) 0.0506(8) Uani 1 1 d . . . H2 H 0.0918 -0.4308 0.1308 0.061 Uiso 1 1 calc R . . C18 C -0.12228(15) -0.1474(3) 0.12069(18) 0.0486(8) Uani 1 1 d . . . H18 H -0.1305 -0.2054 0.1598 0.058 Uiso 1 1 calc R . . C15 C -0.10320(17) 0.0329(4) 0.00750(19) 0.0541(9) Uani 1 1 d . . . H15 H -0.0978 0.0947 -0.0307 0.065 Uiso 1 1 calc R . . O3 O -0.12240(19) -0.5119(5) 0.0959(3) 0.1313(17) Uani 1 1 d . . . C17 C -0.16136(17) -0.1489(4) 0.0577(2) 0.0577(9) Uani 1 1 d . . . H17 H -0.1945 -0.2103 0.0536 0.069 Uiso 1 1 calc R . . C19 C -0.07037(14) -0.0596(3) 0.12629(16) 0.0401(7) Uani 1 1 d . . . C12 C -0.01531(15) 0.1496(3) 0.07829(18) 0.0467(8) Uani 1 1 d . . . C16 C -0.15099(18) -0.0586(4) 0.0006(2) 0.0624(10) Uani 1 1 d . . . H16 H -0.1766 -0.0605 -0.0423 0.075 Uiso 1 1 calc R . . C5 C 0.23584(17) -0.2237(4) 0.1175(2) 0.0567(9) Uani 1 1 d . . . H5 H 0.2726 -0.1728 0.1146 0.068 Uiso 1 1 calc R . . C10 C 0.09358(17) 0.2614(4) 0.2257(2) 0.0603(10) Uani 1 1 d . . . H10A H 0.0626 0.2240 0.2584 0.072 Uiso 1 1 calc R . . H10B H 0.1036 0.3518 0.2431 0.072 Uiso 1 1 calc R . . C13 C -0.0202(2) 0.2637(4) 0.0235(2) 0.0739(12) Uani 1 1 d . . . H13A H 0.0120 0.3293 0.0350 0.111 Uiso 1 1 calc R . . H13B H -0.0611 0.3052 0.0261 0.111 Uiso 1 1 calc R . . H13C H -0.0147 0.2294 -0.0258 0.111 Uiso 1 1 calc R . . C3 C 0.1784(2) -0.4255(4) 0.0891(2) 0.0674(11) Uani 1 1 d . . . H3 H 0.1765 -0.5106 0.0672 0.081 Uiso 1 1 calc R . . C11 C 0.06451(18) 0.2712(3) 0.1494(2) 0.0598(9) Uani 1 1 d . . . H11A H 0.0376 0.3504 0.1459 0.072 Uiso 1 1 calc R . . H11B H 0.0975 0.2807 0.1135 0.072 Uiso 1 1 calc R . . C9 C 0.15285(17) 0.1764(4) 0.2319(2) 0.0605(9) Uani 1 1 d . . . H9A H 0.1864 0.2207 0.2056 0.073 Uiso 1 1 calc R . . H9B H 0.1663 0.1690 0.2837 0.073 Uiso 1 1 calc R . . C4 C 0.2327(2) -0.3463(4) 0.0836(2) 0.0688(11) Uani 1 1 d . . . H4 H 0.2666 -0.3774 0.0567 0.083 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 Cu1 0.0362(2) 0.0313(2) 0.0499(2) 0.00030(15) -0.00129(16) 0.00018(14) Mn1 0.0424(4) 0.0307(3) 0.0561(4) 0.000 0.0026(3) 0.000 O2 0.0428(11) 0.0327(11) 0.0595(13) -0.0003(9) 0.0078(10) 0.0012(9) O1 0.0413(12) 0.0542(14) 0.0438(12) 0.0091(10) -0.0070(9) -0.0055(10) N3 0.068(2) 0.0483(18) 0.081(2) -0.0124(16) -0.0108(17) -0.0024(16) N2 0.0449(14) 0.0333(14) 0.0573(16) 0.0013(11) 0.0062(12) 0.0015(11) C7 0.0400(16) 0.0444(18) 0.0502(18) 0.0024(14) -0.0021(13) -0.0016(14) C20 0.057(2) 0.066(3) 0.085(3) -0.024(2) 0.008(2) -0.001(2) C1 0.0427(16) 0.0376(16) 0.0397(16) 0.0036(12) -0.0034(12) 0.0067(13) N1 0.0428(14) 0.0338(14) 0.0517(15) -0.0023(11) -0.0040(11) -0.0020(11) C6 0.0379(15) 0.0417(17) 0.0448(17) 0.0048(13) -0.0037(12) 0.0075(13) C14 0.0430(17) 0.0457(18) 0.0397(16) 0.0006(13) 0.0047(13) 0.0134(13) C8 0.0412(19) 0.069(3) 0.107(4) -0.013(2) -0.017(2) -0.0022(18) C2 0.059(2) 0.0345(17) 0.058(2) -0.0045(14) -0.0012(16) 0.0046(15) C18 0.0438(17) 0.0484(19) 0.0530(19) 0.0031(15) -0.0076(14) 0.0017(15) C15 0.059(2) 0.063(2) 0.0401(18) 0.0024(15) 0.0033(15) 0.0191(18) O3 0.078(2) 0.171(4) 0.144(4) -0.085(3) -0.017(2) -0.019(2) C17 0.0501(19) 0.059(2) 0.063(2) -0.0086(18) -0.0109(16) 0.0061(17) C19 0.0388(15) 0.0433(17) 0.0378(16) -0.0006(12) -0.0045(12) 0.0090(13) C12 0.0513(18) 0.0406(17) 0.0490(18) 0.0086(14) 0.0125(15) 0.0155(14) C16 0.060(2) 0.081(3) 0.045(2) -0.0053(19) -0.0145(16) 0.009(2) C5 0.0504(19) 0.054(2) 0.066(2) 0.0065(17) 0.0100(16) 0.0129(16) C10 0.056(2) 0.0416(19) 0.084(3) -0.0198(18) 0.0101(19) -0.0054(16) C13 0.089(3) 0.059(2) 0.073(3) 0.023(2) 0.003(2) 0.006(2) C3 0.084(3) 0.048(2) 0.070(3) -0.0104(18) 0.010(2) 0.021(2) C11 0.061(2) 0.0330(18) 0.085(3) 0.0053(17) 0.0077(19) 0.0045(16) C9 0.055(2) 0.046(2) 0.080(3) -0.0151(18) -0.0075(18) -0.0048(17) C4 0.070(3) 0.066(3) 0.073(3) 0.000(2) 0.022(2) 0.018(2) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag Cu1 O1 1.907(2) . ? Cu1 O2 1.938(2) . ? Cu1 N1 1.958(3) . ? Cu1 N2 1.961(3) . ? Mn1 N3 2.072(3) . ? Mn1 N3 2.072(3) 2 ? Mn1 O2 2.147(2) . ? Mn1 O2 2.147(2) 2 ? O2 C1 1.329(4) . ? O1 C19 1.332(3) . ? N3 C20 1.140(5) . ? N2 C12 1.297(4) . ? N2 C11 1.473(4) . ? C7 N1 1.292(4) . ? C7 C6 1.476(4) . ? C7 C8 1.504(5) . ? C20 O3 1.198(5) . ? C1 C2 1.392(4) . ? C1 C6 1.413(4) . ? N1 C9 1.481(4) . ? C6 C5 1.406(4) . ? C14 C15 1.407(5) . ? C14 C19 1.419(4) . ? C14 C12 1.480(5) . ? C8 H8A 0.9600 . ? C8 H8B 0.9600 . ? C8 H8C 0.9600 . ? C2 C3 1.375(5) . ? C2 H2 0.9300 . ? C18 C17 1.382(5) . ? C18 C19 1.402(4) . ? C18 H18 0.9300 . ? C15 C16 1.360(5) . ? C15 H15 0.9300 . ? C17 C16 1.385(6) . ? C17 H17 0.9300 . ? C12 C13 1.501(5) . ? C16 H16 0.9300 . ? C5 C4 1.360(5) . ? C5 H5 0.9300 . ? C10 C11 1.490(5) . ? C10 C9 1.511(5) . ? C10 H10A 0.9700 . ? C10 H10B 0.9700 . ? C13 H13A 0.9600 . ? C13 H13B 0.9600 . ? C13 H13C 0.9600 . ? C3 C4 1.398(6) . ? C3 H3 0.9300 . ? C11 H11A 0.9700 . ? C11 H11B 0.9700 . ? C9 H9A 0.9700 . ? C9 H9B 0.9700 . ? C4 H4 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 O1 Cu1 O2 87.23(9) . . ? O1 Cu1 N1 169.72(10) . . ? O2 Cu1 N1 91.30(10) . . ? O1 Cu1 N2 88.89(10) . . ? O2 Cu1 N2 156.31(10) . . ? N1 Cu1 N2 96.43(11) . . ? N3 Mn1 N3 103.04(19) . 2 ? N3 Mn1 O2 104.19(11) . . ? N3 Mn1 O2 104.35(11) 2 . ? N3 Mn1 O2 104.35(11) . 2 ? N3 Mn1 O2 104.19(11) 2 2 ? O2 Mn1 O2 133.32(11) . 2 ? C1 O2 Cu1 119.71(19) . . ? C1 O2 Mn1 136.78(19) . . ? Cu1 O2 Mn1 103.25(9) . . ? C19 O1 Cu1 121.60(19) . . ? C20 N3 Mn1 157.5(3) . . ? C12 N2 C11 120.7(3) . . ? C12 N2 Cu1 122.8(2) . . ? C11 N2 Cu1 115.6(2) . . ? N1 C7 C6 121.5(3) . . ? N1 C7 C8 120.6(3) . . ? C6 C7 C8 117.9(3) . . ? N3 C20 O3 179.1(6) . . ? O2 C1 C2 119.0(3) . . ? O2 C1 C6 122.0(3) . . ? C2 C1 C6 119.0(3) . . ? C7 N1 C9 118.9(3) . . ? C7 N1 Cu1 124.8(2) . . ? C9 N1 Cu1 116.2(2) . . ? C5 C6 C1 118.4(3) . . ? C5 C6 C7 118.5(3) . . ? C1 C6 C7 123.1(3) . . ? C15 C14 C19 117.0(3) . . ? C15 C14 C12 120.2(3) . . ? C19 C14 C12 122.5(3) . . ? C7 C8 H8A 109.5 . . ? C7 C8 H8B 109.5 . . ? H8A C8 H8B 109.5 . . ? C7 C8 H8C 109.5 . . ? H8A C8 H8C 109.5 . . ? H8B C8 H8C 109.5 . . ? C3 C2 C1 121.3(3) . . ? C3 C2 H2 119.4 . . ? C1 C2 H2 119.4 . . ? C17 C18 C19 120.8(3) . . ? C17 C18 H18 119.6 . . ? C19 C18 H18 119.6 . . ? C16 C15 C14 122.8(3) . . ? C16 C15 H15 118.6 . . ? C14 C15 H15 118.6 . . ? C18 C17 C16 119.9(4) . . ? C18 C17 H17 120.1 . . ? C16 C17 H17 120.1 . . ? O1 C19 C18 117.5(3) . . ? O1 C19 C14 123.0(3) . . ? C18 C19 C14 119.5(3) . . ? N2 C12 C14 120.7(3) . . ? N2 C12 C13 121.7(3) . . ? C14 C12 C13 117.6(3) . . ? C15 C16 C17 119.8(3) . . ? C15 C16 H16 120.1 . . ? C17 C16 H16 120.1 . . ? C4 C5 C6 121.6(4) . . ? C4 C5 H5 119.2 . . ? C6 C5 H5 119.2 . . ? C11 C10 C9 114.9(3) . . ? C11 C10 H10A 108.5 . . ? C9 C10 H10A 108.5 . . ? C11 C10 H10B 108.5 . . ? C9 C10 H10B 108.5 . . ? H10A C10 H10B 107.5 . . ? C12 C13 H13A 109.5 . . ? C12 C13 H13B 109.5 . . ? H13A C13 H13B 109.5 . . ? C12 C13 H13C 109.5 . . ? H13A C13 H13C 109.5 . . ? H13B C13 H13C 109.5 . . ? C2 C3 C4 119.8(4) . . ? C2 C3 H3 120.1 . . ? C4 C3 H3 120.1 . . ? N2 C11 C10 110.2(3) . . ? N2 C11 H11A 109.6 . . ? C10 C11 H11A 109.6 . . ? N2 C11 H11B 109.6 . . ? C10 C11 H11B 109.6 . . ? H11A C11 H11B 108.1 . . ? N1 C9 C10 112.0(3) . . ? N1 C9 H9A 109.2 . . ? C10 C9 H9A 109.2 . . ? N1 C9 H9B 109.2 . . ? C10 C9 H9B 109.2 . . ? H9A C9 H9B 107.9 . . ? C5 C4 C3 119.8(3) . . ? C5 C4 H4 120.1 . . ? C3 C4 H4 120.1 . . ? _diffrn_measured_fraction_theta_max 0.992 _diffrn_reflns_theta_full 31.32 _diffrn_measured_fraction_theta_full 0.992 _refine_diff_density_max 0.362 _refine_diff_density_min -1.087 _refine_diff_density_rms 0.082 data_4 _database_code_depnum_ccdc_archive 'CCDC 833844' #TrackingRef '- 1-4.cif' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety 'C40 H40 Cu2 Mn N6 O4 S2' _chemical_formula_sum 'C40 H40 Cu2 Mn N6 O4 S2' _chemical_formula_weight 914.92 loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' S S 0.1246 0.1234 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Mn Mn 0.3368 0.7283 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Cu Cu 0.3201 1.2651 '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 23.540(5) _cell_length_b 10.194(5) _cell_length_c 17.215(5) _cell_angle_alpha 90.000 _cell_angle_beta 95.494(5) _cell_angle_gamma 90.000 _cell_volume 4112(3) _cell_formula_units_Z 4 _cell_measurement_temperature 150(2) _cell_measurement_reflns_used 4969 _cell_measurement_theta_min 1.7 _cell_measurement_theta_max 28.2 _exptl_crystal_description rectanglular _exptl_crystal_colour green _exptl_crystal_size_max 0.12 _exptl_crystal_size_mid 0.08 _exptl_crystal_size_min 0.04 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.478 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1876 _exptl_absorpt_coefficient_mu 1.476 _exptl_absorpt_correction_type empirical _exptl_absorpt_correction_T_min 0.8427 _exptl_absorpt_correction_T_max 0.9433 _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 26506 _diffrn_reflns_av_R_equivalents 0.0292 _diffrn_reflns_av_sigmaI/netI 0.0242 _diffrn_reflns_limit_h_min -29 _diffrn_reflns_limit_h_max 26 _diffrn_reflns_limit_k_min -13 _diffrn_reflns_limit_k_max 13 _diffrn_reflns_limit_l_min -22 _diffrn_reflns_limit_l_max 22 _diffrn_reflns_theta_min 1.74 _diffrn_reflns_theta_max 28.21 _reflns_number_total 4969 _reflns_number_gt 3617 _reflns_threshold_expression >2sigma(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 V1.80.03' _refine_special_details ; Refinement of F^2^ against ALL reflections. The weighted R-factor wR and goodness of fit S are based on F^2^, conventional R-factors R are based on F, with F set to zero for negative F^2^. The threshold expression of F^2^ > 2sigma(F^2^) is used only for calculating R-factors(gt) etc. and is not relevant to the choice of reflections for refinement. R-factors based on F^2^ are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger. ; _refine_ls_structure_factor_coef Fsqd _refine_ls_matrix_type full _refine_ls_weighting_scheme calc _refine_ls_weighting_details 'calc w=1/[\s^2^(Fo^2^)+(0.1165P)^2^+2.7295P] 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 4969 _refine_ls_number_parameters 249 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0674 _refine_ls_R_factor_gt 0.0486 _refine_ls_wR_factor_ref 0.1904 _refine_ls_wR_factor_gt 0.1748 _refine_ls_goodness_of_fit_ref 1.090 _refine_ls_restrained_S_all 1.090 _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 Cu1 Cu 0.438663(19) -0.00109(3) 0.17801(3) 0.05181(19) Uani 1 1 d . . . Mn1 Mn 0.5000 0.25269(6) 0.2500 0.0430(2) Uani 1 2 d S . . S1 S 0.62553(6) 0.49310(14) 0.09839(9) 0.0897(4) Uani 1 1 d . . . O2 O 0.42391(10) 0.1828(2) 0.19063(14) 0.0503(5) Uani 1 1 d . . . O1 O 0.51591(11) 0.0537(3) 0.17660(15) 0.0597(6) Uani 1 1 d . . . N1 N 0.36116(16) -0.0435(3) 0.20519(19) 0.0634(8) Uani 1 1 d . . . C6 C 0.32263(15) 0.1668(4) 0.16360(19) 0.0525(8) Uani 1 1 d . . . N3 N 0.53912(15) 0.3882(3) 0.17764(19) 0.0632(8) Uani 1 1 d . . . N2 N 0.45651(18) -0.1707(3) 0.1341(2) 0.0750(11) Uani 1 1 d . . . C1 C 0.37443(14) 0.2353(3) 0.16190(17) 0.0435(7) Uani 1 1 d . . . C20 C 0.57586(16) 0.4315(4) 0.1455(2) 0.0550(8) Uani 1 1 d . . . C14 C 0.5379(2) -0.0921(4) 0.0731(2) 0.0690(12) Uani 1 1 d . . . C2 C 0.37424(17) 0.3598(3) 0.1288(2) 0.0578(8) Uani 1 1 d . . . H2 H 0.4078 0.4082 0.1308 0.069 Uiso 1 1 calc R . . C5 C 0.27263(17) 0.2263(5) 0.1265(2) 0.0684(11) Uani 1 1 d . . . H5 H 0.2379 0.1831 0.1273 0.082 Uiso 1 1 calc R . . C3 C 0.3244(2) 0.4114(4) 0.0929(2) 0.0723(12) Uani 1 1 d . . . H3 H 0.3249 0.4941 0.0702 0.087 Uiso 1 1 calc R . . C15 C 0.5761(3) -0.1157(6) 0.0178(3) 0.098(2) Uani 1 1 d . . . H15 H 0.5695 -0.1868 -0.0157 0.118 Uiso 1 1 calc R . . C19 C 0.54908(18) 0.0200(4) 0.1223(2) 0.0566(9) Uani 1 1 d . . . C12 C 0.4935(2) -0.1868(4) 0.0832(3) 0.0797(15) Uani 1 1 d . . . C7 C 0.31915(18) 0.0385(5) 0.2009(2) 0.0641(10) Uani 1 1 d . . . C18 C 0.59717(19) 0.0964(5) 0.1142(2) 0.0686(11) Uani 1 1 d . . . H18 H 0.6047 0.1674 0.1475 0.082 Uiso 1 1 calc R . . C4 C 0.2738(2) 0.3429(5) 0.0902(3) 0.0780(13) Uani 1 1 d . . . H4 H 0.2408 0.3769 0.0636 0.094 Uiso 1 1 calc R . . C11 C 0.4194(3) -0.2799(4) 0.1563(4) 0.111(2) Uani 1 1 d . . . H11A H 0.3853 -0.2836 0.1199 0.133 Uiso 1 1 calc R . . H11B H 0.4395 -0.3625 0.1533 0.133 Uiso 1 1 calc R . . C17 C 0.6337(2) 0.0709(6) 0.0591(3) 0.0901(16) Uani 1 1 d . . . H17 H 0.6649 0.1249 0.0537 0.108 Uiso 1 1 calc R . . C10 C 0.4029(3) -0.2612(5) 0.2365(4) 0.106(2) Uani 1 1 d . . . H10A H 0.4357 -0.2277 0.2689 0.127 Uiso 1 1 calc R . . H10B H 0.3936 -0.3462 0.2571 0.127 Uiso 1 1 calc R . . C13 C 0.4920(3) -0.3085(6) 0.0317(4) 0.131(3) Uani 1 1 d . . . H13A H 0.4610 -0.3640 0.0435 0.196 Uiso 1 1 calc R . . H13B H 0.5273 -0.3555 0.0414 0.196 Uiso 1 1 calc R . . H13C H 0.4867 -0.2829 -0.0221 0.196 Uiso 1 1 calc R . . C8 C 0.2632(2) 0.0065(6) 0.2355(4) 0.100(2) Uani 1 1 d . . . H8A H 0.2657 -0.0795 0.2583 0.150 Uiso 1 1 calc R . . H8B H 0.2322 0.0090 0.1950 0.150 Uiso 1 1 calc R . . H8C H 0.2567 0.0699 0.2749 0.150 Uiso 1 1 calc R . . C9 C 0.3535(2) -0.1704(5) 0.2439(3) 0.0984(19) Uani 1 1 d . . . H9A H 0.3187 -0.2115 0.2209 0.118 Uiso 1 1 calc R . . H9B H 0.3495 -0.1554 0.2988 0.118 Uiso 1 1 calc R . . C16 C 0.6228(3) -0.0393(8) 0.0105(3) 0.111(2) Uani 1 1 d . . . H16 H 0.6475 -0.0599 -0.0266 0.134 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 Cu1 0.0576(3) 0.0326(2) 0.0628(3) -0.00172(15) -0.0066(2) -0.00467(15) Mn1 0.0417(4) 0.0348(3) 0.0520(4) 0.000 0.0016(3) 0.000 S1 0.0696(8) 0.1067(11) 0.0955(9) 0.0044(7) 0.0221(7) -0.0255(6) O2 0.0472(12) 0.0363(11) 0.0655(14) 0.0005(10) -0.0046(10) -0.0016(9) O1 0.0557(15) 0.0579(15) 0.0661(15) -0.0254(12) 0.0088(12) -0.0040(12) N1 0.073(2) 0.0525(17) 0.0624(18) 0.0093(14) -0.0043(15) -0.0252(17) C6 0.0496(19) 0.064(2) 0.0450(16) -0.0053(14) 0.0078(14) -0.0013(15) N3 0.074(2) 0.0548(17) 0.0616(18) 0.0032(14) 0.0120(16) -0.0085(16) N2 0.095(3) 0.0357(15) 0.085(2) -0.0104(15) -0.038(2) 0.0066(16) C1 0.0469(17) 0.0451(16) 0.0385(14) -0.0018(11) 0.0049(12) 0.0037(13) C20 0.057(2) 0.0518(18) 0.0541(18) -0.0011(15) -0.0030(16) -0.0033(16) C14 0.087(3) 0.069(3) 0.0451(18) -0.0158(16) -0.0194(18) 0.041(2) C2 0.065(2) 0.0458(18) 0.063(2) 0.0012(15) 0.0099(17) 0.0081(16) C5 0.047(2) 0.096(3) 0.063(2) -0.018(2) 0.0042(17) 0.009(2) C3 0.087(3) 0.062(2) 0.067(2) 0.0060(18) 0.005(2) 0.028(2) C15 0.120(5) 0.111(4) 0.060(3) -0.029(3) -0.011(3) 0.063(4) C19 0.066(2) 0.0561(19) 0.0465(18) -0.0073(14) -0.0016(16) 0.0242(17) C12 0.105(4) 0.051(2) 0.072(3) -0.0227(19) -0.047(3) 0.031(2) C7 0.058(2) 0.076(3) 0.058(2) 0.0071(19) 0.0006(17) -0.022(2) C18 0.068(3) 0.077(3) 0.062(2) -0.0055(19) 0.0122(18) 0.026(2) C4 0.069(3) 0.093(3) 0.071(3) -0.005(2) -0.003(2) 0.034(3) C11 0.121(5) 0.040(2) 0.158(6) -0.010(3) -0.052(4) -0.014(2) C17 0.084(3) 0.119(4) 0.070(3) 0.010(3) 0.025(2) 0.037(3) C10 0.129(5) 0.057(3) 0.119(5) 0.032(3) -0.050(4) -0.034(3) C13 0.170(6) 0.081(4) 0.127(5) -0.066(4) -0.060(4) 0.047(4) C8 0.073(4) 0.123(5) 0.106(4) 0.025(3) 0.027(3) -0.027(3) C9 0.106(4) 0.076(3) 0.106(4) 0.041(3) -0.023(3) -0.041(3) C16 0.120(5) 0.162(6) 0.053(3) -0.012(3) 0.017(3) 0.082(5) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag Cu1 O1 1.904(3) . ? Cu1 O2 1.922(2) . ? Cu1 N2 1.949(4) . ? Cu1 N1 1.974(4) . ? Mn1 O2 2.100(2) . ? Mn1 O2 2.100(2) 2_655 ? Mn1 N3 2.128(3) 2_655 ? Mn1 N3 2.128(3) . ? Mn1 O1 2.438(3) . ? Mn1 O1 2.438(3) 2_655 ? S1 C20 1.613(4) . ? O2 C1 1.333(4) . ? O1 C19 1.320(5) . ? N1 C7 1.291(6) . ? N1 C9 1.475(5) . ? C6 C1 1.408(5) . ? C6 C5 1.421(5) . ? C6 C7 1.463(6) . ? N3 C20 1.158(5) . ? N2 C12 1.304(7) . ? N2 C11 1.488(7) . ? C1 C2 1.392(5) . ? C14 C15 1.391(7) . ? C14 C19 1.432(5) . ? C14 C12 1.446(8) . ? C2 C3 1.376(6) . ? C2 H2 0.9300 . ? C5 C4 1.344(7) . ? C5 H5 0.9300 . ? C3 C4 1.379(7) . ? C3 H3 0.9300 . ? C15 C16 1.362(10) . ? C15 H15 0.9300 . ? C19 C18 1.392(6) . ? C12 C13 1.523(6) . ? C7 C8 1.532(6) . ? C18 C17 1.364(6) . ? C18 H18 0.9300 . ? C4 H4 0.9300 . ? C11 C10 1.482(10) . ? C11 H11A 0.9700 . ? C11 H11B 0.9700 . ? C17 C16 1.409(9) . ? C17 H17 0.9300 . ? C10 C9 1.501(9) . ? C10 H10A 0.9700 . ? C10 H10B 0.9700 . ? C13 H13A 0.9600 . ? C13 H13B 0.9600 . ? C13 H13C 0.9600 . ? C8 H8A 0.9600 . ? C8 H8B 0.9600 . ? C8 H8C 0.9600 . ? C9 H9A 0.9700 . ? C9 H9B 0.9700 . ? C16 H16 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 O1 Cu1 O2 84.19(11) . . ? O1 Cu1 N2 90.78(15) . . ? O2 Cu1 N2 163.12(14) . . ? O1 Cu1 N1 166.48(12) . . ? O2 Cu1 N1 90.31(13) . . ? N2 Cu1 N1 97.82(17) . . ? O2 Mn1 O2 140.32(13) . 2_655 ? O2 Mn1 N3 96.23(12) . 2_655 ? O2 Mn1 N3 109.40(12) 2_655 2_655 ? O2 Mn1 N3 109.40(12) . . ? O2 Mn1 N3 96.23(12) 2_655 . ? N3 Mn1 N3 99.04(19) 2_655 . ? O2 Mn1 O1 68.38(9) . . ? O2 Mn1 O1 78.68(9) 2_655 . ? N3 Mn1 O1 160.09(12) 2_655 . ? N3 Mn1 O1 98.06(11) . . ? O2 Mn1 O1 78.68(9) . 2_655 ? O2 Mn1 O1 68.38(9) 2_655 2_655 ? N3 Mn1 O1 98.06(11) 2_655 2_655 ? N3 Mn1 O1 160.09(12) . 2_655 ? O1 Mn1 O1 67.35(14) . 2_655 ? C1 O2 Cu1 120.69(19) . . ? C1 O2 Mn1 135.9(2) . . ? Cu1 O2 Mn1 103.35(10) . . ? C19 O1 Cu1 124.3(2) . . ? C19 O1 Mn1 135.6(3) . . ? Cu1 O1 Mn1 92.47(10) . . ? C7 N1 C9 117.9(4) . . ? C7 N1 Cu1 124.4(3) . . ? C9 N1 Cu1 117.1(3) . . ? C1 C6 C5 117.4(4) . . ? C1 C6 C7 122.5(3) . . ? C5 C6 C7 120.1(4) . . ? C20 N3 Mn1 155.8(3) . . ? C12 N2 C11 121.7(4) . . ? C12 N2 Cu1 123.7(3) . . ? C11 N2 Cu1 114.2(4) . . ? O2 C1 C2 119.1(3) . . ? O2 C1 C6 121.4(3) . . ? C2 C1 C6 119.5(3) . . ? N3 C20 S1 178.1(4) . . ? C15 C14 C19 116.7(5) . . ? C15 C14 C12 119.3(4) . . ? C19 C14 C12 123.7(4) . . ? C3 C2 C1 120.1(4) . . ? C3 C2 H2 119.9 . . ? C1 C2 H2 119.9 . . ? C4 C5 C6 122.3(4) . . ? C4 C5 H5 118.8 . . ? C6 C5 H5 118.8 . . ? C2 C3 C4 121.2(4) . . ? C2 C3 H3 119.4 . . ? C4 C3 H3 119.4 . . ? C16 C15 C14 122.9(5) . . ? C16 C15 H15 118.6 . . ? C14 C15 H15 118.6 . . ? O1 C19 C18 117.9(3) . . ? O1 C19 C14 122.7(4) . . ? C18 C19 C14 119.5(4) . . ? N2 C12 C14 122.3(3) . . ? N2 C12 C13 120.9(6) . . ? C14 C12 C13 116.8(6) . . ? N1 C7 C6 121.9(4) . . ? N1 C7 C8 121.5(4) . . ? C6 C7 C8 116.6(4) . . ? C17 C18 C19 122.4(5) . . ? C17 C18 H18 118.8 . . ? C19 C18 H18 118.8 . . ? C5 C4 C3 119.2(4) . . ? C5 C4 H4 120.4 . . ? C3 C4 H4 120.4 . . ? C10 C11 N2 110.8(4) . . ? C10 C11 H11A 109.5 . . ? N2 C11 H11A 109.5 . . ? C10 C11 H11B 109.5 . . ? N2 C11 H11B 109.5 . . ? H11A C11 H11B 108.1 . . ? C18 C17 C16 118.2(6) . . ? C18 C17 H17 120.9 . . ? C16 C17 H17 120.9 . . ? C11 C10 C9 115.6(5) . . ? C11 C10 H10A 108.4 . . ? C9 C10 H10A 108.4 . . ? C11 C10 H10B 108.4 . . ? C9 C10 H10B 108.4 . . ? H10A C10 H10B 107.4 . . ? C12 C13 H13A 109.5 . . ? C12 C13 H13B 109.5 . . ? H13A C13 H13B 109.5 . . ? C12 C13 H13C 109.5 . . ? H13A C13 H13C 109.5 . . ? H13B C13 H13C 109.5 . . ? C7 C8 H8A 109.5 . . ? C7 C8 H8B 109.5 . . ? H8A C8 H8B 109.5 . . ? C7 C8 H8C 109.5 . . ? H8A C8 H8C 109.5 . . ? H8B C8 H8C 109.5 . . ? N1 C9 C10 111.9(5) . . ? N1 C9 H9A 109.2 . . ? C10 C9 H9A 109.2 . . ? N1 C9 H9B 109.2 . . ? C10 C9 H9B 109.2 . . ? H9A C9 H9B 107.9 . . ? C15 C16 C17 120.3(5) . . ? C15 C16 H16 119.8 . . ? C17 C16 H16 119.8 . . ? _diffrn_measured_fraction_theta_max 0.979 _diffrn_reflns_theta_full 28.21 _diffrn_measured_fraction_theta_full 0.979 _refine_diff_density_max 1.285 _refine_diff_density_min -0.630 _refine_diff_density_rms 0.091