Supplementary Material (ESI) for Dalton Transactions This journal is © The Royal Society of Chemistry 2002 data_global _journal_coden_Cambridge 186 _publ_requested_journal 'Dalton Transactions' loop_ _publ_author_name 'Gao, En-Qing' 'Jiang, Zong-Hui' 'Liao, Dai-Zheng' 'Tang, Jin-Kui' 'Wang, Li-Ya' 'Yan, Shi-Ping' 'Zhang, Lei' _publ_contact_author_name 'Dr Dai-Zheng Liao' _publ_contact_author_address ; Department of Chemistry Nankai University Tianjin 300071 CHINA ; _publ_contact_author_email 'COORD@NANKAI.EDU.CN' _publ_section_title ; Heterobinuclear copper(II)-manganese(II) complexes behaving three-dimensional supramolecular network via both macrocyclic oxamidobridge and hydrogen bonds ; data_001022d _database_code_CSD 171324 _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C34 H41 Cl2 Cu Mn N11 O11' _chemical_formula_weight 969.21 loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source 'Cu' 'Cu' 0.3201 1.2651 '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' 'O' 'O' 0.0106 0.0060 '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' 'C' 'C' 0.0033 0.0016 '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' 'H' 'H' 0.0000 0.0000 '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 loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, -y, -z' _cell_length_a 9.7676(11) _cell_length_b 15.3391(18) _cell_length_c 16.1155(19) _cell_angle_alpha 113.477(2) _cell_angle_beta 97.085(2) _cell_angle_gamma 98.055(3) _cell_volume 2149.7(4) _cell_formula_units_Z 2 _cell_measurement_temperature 293(2) _cell_measurement_reflns_used ? _cell_measurement_theta_min ? _cell_measurement_theta_max ? _exptl_crystal_description ? _exptl_crystal_colour ? _exptl_crystal_size_max 0.30 _exptl_crystal_size_mid 0.25 _exptl_crystal_size_min 0.20 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.464 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 953 _exptl_absorpt_coefficient_mu 0.980 _exptl_absorpt_correction_type none _exptl_absorpt_correction_T_min 0.7576 _exptl_absorpt_correction_T_max 0.8281 _exptl_absorpt_process_details ? _exptl_special_details ; ? ; _diffrn_ambient_temperature 293(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 8779 _diffrn_reflns_av_R_equivalents 0.0358 _diffrn_reflns_av_sigmaI/netI 0.1053 _diffrn_reflns_limit_h_min -11 _diffrn_reflns_limit_h_max 11 _diffrn_reflns_limit_k_min -18 _diffrn_reflns_limit_k_max 9 _diffrn_reflns_limit_l_min -19 _diffrn_reflns_limit_l_max 19 _diffrn_reflns_theta_min 2.15 _diffrn_reflns_theta_max 25.03 _reflns_number_total 7386 _reflns_number_gt 3679 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'Bruker SMART' _computing_cell_refinement 'Bruker SMART' _computing_data_reduction 'Bruker SHELXTL' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'Bruker SHELXTL' _computing_publication_material 'Bruker SHELXTL' _refine_special_details ; Refinement of F^2^ against ALL reflections. The weighted R-factor wR and goodness of fit S are based on F^2^, conventional R-factors R are based on F, with F set to zero for negative F^2^. The threshold expression of F^2^ > 2sigma(F^2^) is used only for calculating R-factors(gt) etc. and is not relevant to the choice of reflections for refinement. R-factors based on F^2^ are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger. ; _refine_ls_structure_factor_coef Fsqd _refine_ls_matrix_type full _refine_ls_weighting_scheme calc _refine_ls_weighting_details 'calc w=1/[\s^2^(Fo^2^)+(0.0800P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment mixed _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 7386 _refine_ls_number_parameters 569 _refine_ls_number_restraints 33 _refine_ls_R_factor_all 0.1530 _refine_ls_R_factor_gt 0.0676 _refine_ls_wR_factor_ref 0.1770 _refine_ls_wR_factor_gt 0.1435 _refine_ls_goodness_of_fit_ref 0.988 _refine_ls_restrained_S_all 0.997 _refine_ls_shift/su_max 0.246 _refine_ls_shift/su_mean 0.008 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 1.07188(9) 0.75333(6) 0.27111(5) 0.0633(3) Uani 1 1 d . . . Mn1 Mn 0.96752(9) 0.73412(6) -0.07877(6) 0.0431(3) Uani 1 1 d . . . O1 O 0.9141(4) 0.6623(3) 0.0038(3) 0.0533(10) Uani 1 1 d . . . O2 O 1.1035(4) 0.8303(3) 0.0650(3) 0.0496(10) Uani 1 1 d . . . N1 N 1.1560(5) 0.8232(3) 0.2060(3) 0.0562(13) Uani 1 1 d . . . N2 N 0.9502(5) 0.6731(4) 0.1518(4) 0.0622(15) Uani 1 1 d . . . N3 N 0.9691(7) 0.6938(5) 0.3417(4) 0.0831(18) Uani 1 1 d . . . N4 N 1.2239(7) 0.8144(5) 0.3834(4) 0.089(2) Uani 1 1 d . . . N5 N 0.9601(5) 0.7776(4) -0.2186(3) 0.0523(12) Uani 1 1 d . . . N6 N 1.1630(5) 0.7156(3) -0.1273(3) 0.0498(12) Uani 1 1 d . . . N7 N 1.3129(6) 0.7132(4) -0.2193(4) 0.0653(15) Uani 1 1 d . . . H7A H 1.3473 0.7185 -0.2640 0.078 Uiso 1 1 calc R . . N8 N 0.8299(5) 0.6118(3) -0.2015(3) 0.0453(11) Uani 1 1 d . . . N9 N 0.6823(5) 0.5541(4) -0.3366(3) 0.0615(14) Uani 1 1 d . . . H9A H 0.6399 0.5520 -0.3876 0.074 Uiso 1 1 calc R . . N10 N 0.8572(5) 0.8531(3) -0.0588(3) 0.0464(12) Uani 1 1 d . . . N11 N 0.8188(5) 0.9840(3) -0.0775(3) 0.0538(13) Uani 1 1 d . . . H11A H 0.8201 1.0268 -0.0994 0.065 Uiso 1 1 calc R . . C1 C 0.9744(6) 0.7018(4) 0.0896(4) 0.0473(14) Uani 1 1 d . . . C2 C 1.0859(6) 0.7934(4) 0.1220(4) 0.0437(14) Uani 1 1 d . . . C3 C 1.2636(7) 0.9128(5) 0.2456(5) 0.072(2) Uani 1 1 d . . . H3A H 1.2181 0.9680 0.2646 0.086 Uiso 1 1 calc R . . H3B H 1.3155 0.9156 0.1988 0.086 Uiso 1 1 calc R . . C4 C 1.3662(9) 0.9196(6) 0.3284(6) 0.096(3) Uani 1 1 d . . . H4A H 1.4185 0.8682 0.3068 0.115 Uiso 1 1 calc R . . H4B H 1.4336 0.9809 0.3525 0.115 Uiso 1 1 calc R . . C5 C 1.3038(9) 0.9127(6) 0.4062(5) 0.095(3) Uani 1 1 d . . . H5A H 1.3790 0.9315 0.4592 0.114 Uiso 1 1 calc R . . H5B H 1.2415 0.9582 0.4233 0.114 Uiso 1 1 calc R . . C6 C 1.1629(10) 0.8062(8) 0.4599(5) 0.108(3) Uani 1 1 d . . . H6A H 1.2372 0.8144 0.5099 0.130 Uiso 1 1 calc R . . H6B H 1.1083 0.8558 0.4833 0.130 Uiso 1 1 calc R . . C7 C 1.0726(10) 0.7098(7) 0.4236(6) 0.104(3) Uani 1 1 d . . . H7B H 1.0237 0.7039 0.4706 0.125 Uiso 1 1 calc R . . H7C H 1.1298 0.6609 0.4072 0.125 Uiso 1 1 calc R . . C8 C 0.8845(10) 0.5932(7) 0.2867(6) 0.098(3) Uani 1 1 d . . . H8A H 0.9482 0.5496 0.2650 0.117 Uiso 1 1 calc R . . H8B H 0.8342 0.5732 0.3265 0.117 Uiso 1 1 calc R . . C9 C 0.7832(9) 0.5833(6) 0.2076(6) 0.092(3) Uani 1 1 d . . . H9B H 0.7336 0.6364 0.2277 0.110 Uiso 1 1 calc R . . H9C H 0.7142 0.5234 0.1877 0.110 Uiso 1 1 calc R . . C10 C 0.8429(8) 0.5827(5) 0.1249(5) 0.080(2) Uani 1 1 d . . . H10A H 0.8858 0.5267 0.1002 0.097 Uiso 1 1 calc R . . H10B H 0.7673 0.5776 0.0770 0.097 Uiso 1 1 calc R . . C11 C 1.0817(7) 0.7504(5) -0.2611(4) 0.0635(18) Uani 1 1 d . . . H11B H 1.1282 0.8038 -0.2722 0.076 Uiso 1 1 calc R . . H11C H 1.0488 0.6946 -0.3202 0.076 Uiso 1 1 calc R . . C12 C 1.1846(6) 0.7267(4) -0.2017(4) 0.0521(15) Uani 1 1 d . . . C13 C 1.2847(6) 0.6918(4) -0.0958(4) 0.0506(15) Uani 1 1 d . . . C14 C 1.3205(6) 0.6713(5) -0.0205(4) 0.0614(17) Uani 1 1 d . . . H14A H 1.2588 0.6735 0.0195 0.074 Uiso 1 1 calc R . . C15 C 1.4508(7) 0.6474(5) -0.0064(5) 0.073(2) Uani 1 1 d . . . H15A H 1.4763 0.6325 0.0432 0.087 Uiso 1 1 calc R . . C16 C 1.5412(7) 0.6455(5) -0.0645(6) 0.078(2) Uani 1 1 d . . . H16A H 1.6276 0.6290 -0.0537 0.094 Uiso 1 1 calc R . . C17 C 1.5101(7) 0.6667(5) -0.1372(6) 0.077(2) Uani 1 1 d . . . H17A H 1.5744 0.6661 -0.1753 0.092 Uiso 1 1 calc R . . C18 C 1.3790(7) 0.6895(4) -0.1540(5) 0.0582(16) Uani 1 1 d . . . C19 C 0.8250(7) 0.7215(4) -0.2807(4) 0.0569(16) Uani 1 1 d . . . H19A H 0.8331 0.7086 -0.3438 0.068 Uiso 1 1 calc R . . H19B H 0.7527 0.7593 -0.2649 0.068 Uiso 1 1 calc R . . C20 C 0.7824(6) 0.6265(4) -0.2738(4) 0.0516(15) Uani 1 1 d . . . C21 C 0.7516(7) 0.5180(4) -0.2210(4) 0.0536(16) Uani 1 1 d . . . C22 C 0.7567(7) 0.4628(5) -0.1704(4) 0.0603(17) Uani 1 1 d . . . H22A H 0.8205 0.4843 -0.1150 0.072 Uiso 1 1 calc R . . C23 C 0.6626(8) 0.3750(5) -0.2063(5) 0.0687(19) Uani 1 1 d . . . H23A H 0.6637 0.3364 -0.1740 0.082 Uiso 1 1 calc R . . C24 C 0.5670(8) 0.3420(5) -0.2879(6) 0.081(2) Uani 1 1 d . . . H24A H 0.5033 0.2833 -0.3080 0.097 Uiso 1 1 calc R . . C25 C 0.5638(8) 0.3938(5) -0.3402(5) 0.075(2) Uani 1 1 d . . . H25A H 0.5014 0.3705 -0.3965 0.090 Uiso 1 1 calc R . . C26 C 0.6588(7) 0.4833(5) -0.3052(4) 0.0595(17) Uani 1 1 d . . . C27 C 0.9600(6) 0.8822(4) -0.1812(4) 0.0522(15) Uani 1 1 d . . . H27A H 1.0559 0.9197 -0.1574 0.063 Uiso 1 1 calc R . . H27B H 0.9171 0.8983 -0.2293 0.063 Uiso 1 1 calc R . . C28 C 0.8795(6) 0.9049(4) -0.1070(4) 0.0453(14) Uani 1 1 d . . . C29 C 0.7788(6) 0.9005(4) 0.0051(4) 0.0476(14) Uani 1 1 d . . . C30 C 0.7323(7) 0.8799(5) 0.0741(5) 0.0611(17) Uani 1 1 d . . . H30A H 0.7518 0.8267 0.0837 0.073 Uiso 1 1 calc R . . C31 C 0.6564(7) 0.9409(5) 0.1281(5) 0.073(2) Uani 1 1 d . . . H31A H 0.6244 0.9283 0.1750 0.088 Uiso 1 1 calc R . . C32 C 0.6256(7) 1.0209(6) 0.1147(6) 0.082(2) Uani 1 1 d . . . H32A H 0.5707 1.0589 0.1512 0.098 Uiso 1 1 calc R . . C33 C 0.6750(7) 1.0451(5) 0.0482(5) 0.0631(17) Uani 1 1 d . . . H33A H 0.6568 1.0991 0.0395 0.076 Uiso 1 1 calc R . . C34 C 0.7543(6) 0.9830(4) -0.0055(4) 0.0528(15) Uani 1 1 d . . . Cl1 Cl 0.4984(4) 0.7943(3) 0.6272(3) 0.0708(10) Uani 0.50 1 d PD . . O11 O 0.5063(15) 0.8115(10) 0.5490(7) 0.120(4) Uiso 0.50 1 d PD . . O12 O 0.3716(14) 0.8228(13) 0.6496(14) 0.195(7) Uiso 0.50 1 d PD . . O13 O 0.4767(13) 0.7084(7) 0.6368(9) 0.114(4) Uiso 0.50 1 d PD . . O14 O 0.5905(11) 0.8599(8) 0.7083(7) 0.117(4) Uiso 0.50 1 d PD . . Cl2 Cl 0.7318(11) 0.8110(5) 0.5245(5) 0.129(3) Uani 0.35 1 d PD . . O21 O 0.614(3) 0.821(2) 0.568(2) 0.233(15) Uiso 0.35 1 d PD . . O22 O 0.749(2) 0.7141(9) 0.4932(15) 0.148(7) Uiso 0.35 1 d PD . . O23 O 0.8492(16) 0.8678(13) 0.5944(11) 0.136(7) Uiso 0.35 1 d PD . . O24 O 0.745(3) 0.830(2) 0.4473(14) 0.193(10) Uiso 0.35 1 d PD . . Cl3 Cl 0.8020(16) 0.8957(11) 0.3510(11) 0.085(5) Uani 0.15 1 d PD . . O31 O 0.747(5) 0.979(2) 0.365(4) 0.183 Uiso 0.15 1 d PD . . O32 O 0.9449(17) 0.8935(18) 0.3473(17) 0.046(7) Uiso 0.15 1 d PD . . O33 O 0.732(5) 0.831(3) 0.2602(19) 0.22(3) Uiso 0.15 1 d PD . . O34 O 0.754(6) 0.849(4) 0.404(3) 0.194 Uiso 0.15 1 d PD . . Cl4 Cl 0.0723(10) 0.5054(7) 0.5070(7) 0.177(6) Uani 0.50 1 d PD . . O41 O 0.122(2) 0.4209(9) 0.4924(11) 0.166(7) Uani 0.50 1 d PD . . O42 O 0.160(2) 0.5965(10) 0.5397(12) 0.191(8) Uani 0.50 1 d PD . . O43 O 0.0057(14) 0.4832(7) 0.4189(7) 0.223(5) Uani 1 1 d D . . O3 O 0.3833(17) 0.5048(9) 0.5335(8) 0.138(5) Uani 0.50 1 d P . . O4 O 0.8789(18) 0.9459(15) 0.3509(10) 0.147(7) Uani 0.50 1 d P . . 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 0.0810(6) 0.0626(5) 0.0453(5) 0.0284(4) 0.0005(4) 0.0055(4) Mn1 0.0443(5) 0.0460(5) 0.0396(5) 0.0188(4) 0.0057(4) 0.0114(4) O1 0.056(2) 0.056(2) 0.042(2) 0.024(2) -0.006(2) -0.004(2) O2 0.058(3) 0.047(2) 0.042(2) 0.0215(19) 0.0044(19) 0.002(2) N1 0.059(3) 0.050(3) 0.049(3) 0.021(3) -0.006(3) -0.007(3) N2 0.068(4) 0.057(3) 0.055(3) 0.032(3) -0.006(3) -0.015(3) N3 0.106(5) 0.092(5) 0.063(4) 0.048(4) 0.016(4) 0.012(4) N4 0.111(5) 0.093(5) 0.057(4) 0.045(3) -0.016(3) -0.006(4) N5 0.053(3) 0.059(3) 0.046(3) 0.024(3) 0.004(2) 0.012(3) N6 0.047(3) 0.053(3) 0.046(3) 0.017(2) 0.009(2) 0.013(2) N7 0.067(4) 0.076(4) 0.069(4) 0.036(3) 0.035(3) 0.027(3) N8 0.045(3) 0.051(3) 0.039(3) 0.017(2) 0.005(2) 0.014(2) N9 0.071(4) 0.057(3) 0.043(3) 0.017(3) -0.011(3) 0.003(3) N10 0.047(3) 0.044(3) 0.049(3) 0.022(2) 0.007(2) 0.007(2) N11 0.052(3) 0.043(3) 0.062(3) 0.025(3) -0.005(3) 0.004(3) C1 0.052(4) 0.044(3) 0.050(4) 0.024(3) 0.012(3) 0.009(3) C2 0.044(3) 0.037(3) 0.042(3) 0.010(3) 0.002(3) 0.008(3) C3 0.080(5) 0.056(4) 0.060(4) 0.021(3) -0.018(4) -0.009(4) C4 0.104(6) 0.069(5) 0.082(6) 0.028(4) -0.043(5) -0.019(5) C5 0.125(7) 0.082(6) 0.051(4) 0.022(4) -0.026(5) -0.004(5) C6 0.133(8) 0.132(8) 0.051(5) 0.041(5) 0.002(5) 0.007(7) C7 0.122(7) 0.134(8) 0.087(6) 0.085(6) 0.008(5) 0.012(7) C8 0.126(7) 0.104(7) 0.083(6) 0.068(5) 0.014(5) 0.004(6) C9 0.101(6) 0.091(6) 0.084(6) 0.047(5) 0.023(5) -0.011(5) C10 0.087(5) 0.078(5) 0.067(5) 0.038(4) 0.001(4) -0.022(4) C11 0.062(4) 0.082(5) 0.052(4) 0.029(4) 0.021(3) 0.020(4) C12 0.052(4) 0.048(4) 0.055(4) 0.017(3) 0.017(3) 0.013(3) C13 0.043(4) 0.049(4) 0.056(4) 0.018(3) 0.008(3) 0.011(3) C14 0.053(4) 0.075(5) 0.052(4) 0.020(4) 0.010(3) 0.021(4) C15 0.057(4) 0.084(5) 0.076(5) 0.032(4) 0.001(4) 0.026(4) C16 0.044(4) 0.091(6) 0.096(6) 0.033(5) 0.008(4) 0.031(4) C17 0.057(5) 0.086(5) 0.100(6) 0.039(5) 0.036(4) 0.035(4) C18 0.055(4) 0.053(4) 0.067(4) 0.020(3) 0.020(4) 0.019(3) C19 0.069(4) 0.054(4) 0.046(4) 0.023(3) 0.003(3) 0.016(3) C20 0.054(4) 0.052(4) 0.046(4) 0.017(3) 0.007(3) 0.016(3) C21 0.062(4) 0.051(4) 0.043(3) 0.017(3) 0.004(3) 0.014(3) C22 0.072(5) 0.056(4) 0.049(4) 0.018(3) 0.010(3) 0.018(4) C23 0.085(5) 0.051(4) 0.072(5) 0.029(4) 0.014(4) 0.013(4) C24 0.083(5) 0.050(4) 0.101(6) 0.026(4) 0.008(5) 0.016(4) C25 0.077(5) 0.054(4) 0.066(4) 0.006(4) -0.011(4) 0.012(4) C26 0.064(4) 0.048(4) 0.058(4) 0.017(3) -0.001(3) 0.018(4) C27 0.049(4) 0.050(4) 0.056(4) 0.025(3) 0.004(3) 0.004(3) C28 0.041(3) 0.039(3) 0.051(3) 0.016(3) 0.003(3) 0.009(3) C29 0.048(4) 0.041(3) 0.046(3) 0.013(3) 0.002(3) 0.006(3) C30 0.066(4) 0.056(4) 0.066(4) 0.028(3) 0.020(4) 0.013(4) C31 0.076(5) 0.070(5) 0.072(5) 0.021(4) 0.029(4) 0.023(4) C32 0.062(5) 0.074(5) 0.086(6) 0.009(4) 0.021(4) 0.015(4) C33 0.053(4) 0.053(4) 0.068(4) 0.013(4) 0.003(4) 0.012(3) C34 0.049(4) 0.047(4) 0.053(4) 0.015(3) 0.002(3) 0.007(3) Cl1 0.057(2) 0.082(2) 0.078(2) 0.049(2) -0.0073(17) 0.0025(19) Cl2 0.202(8) 0.079(4) 0.079(4) 0.023(4) -0.008(5) 0.000(5) Cl3 0.101(12) 0.088(10) 0.092(11) 0.044(9) 0.056(10) 0.052(9) Cl4 0.367(17) 0.069(3) 0.090(5) 0.032(3) 0.059(10) 0.023(9) O41 0.28(2) 0.091(10) 0.132(12) 0.037(9) 0.080(13) 0.038(12) O42 0.29(2) 0.126(14) 0.155(15) 0.083(12) 0.023(15) 0.001(15) O43 0.324(14) 0.151(8) 0.176(10) 0.052(8) 0.048(10) 0.047(8) O3 0.215(14) 0.111(10) 0.071(7) 0.035(7) -0.019(8) 0.033(10) O4 0.120(12) 0.25(2) 0.105(11) 0.105(13) 0.022(10) 0.053(14) _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 N2 1.941(5) . ? Cu1 N1 1.946(5) . ? Cu1 N4 1.988(6) . ? Cu1 N3 1.997(6) . ? Mn1 O1 2.106(4) . ? Mn1 N6 2.163(5) . ? Mn1 N10 2.183(5) . ? Mn1 N8 2.217(5) . ? Mn1 O2 2.297(4) . ? O1 C1 1.288(6) . ? O2 C2 1.272(6) . ? N1 C2 1.305(7) . ? N1 C3 1.460(7) . ? N2 C1 1.278(7) . ? N2 C10 1.486(8) . ? N3 C7 1.473(9) . ? N3 C8 1.490(10) . ? N4 C5 1.475(9) . ? N4 C6 1.476(9) . ? N5 C19 1.467(7) . ? N5 C11 1.471(7) . ? N5 C27 1.472(7) . ? N6 C12 1.314(7) . ? N6 C13 1.387(7) . ? N7 C12 1.344(7) . ? N7 C18 1.363(8) . ? N8 C20 1.315(7) . ? N8 C21 1.424(7) . ? N9 C20 1.331(7) . ? N9 C26 1.372(8) . ? N10 C28 1.329(7) . ? N10 C29 1.390(7) . ? N11 C28 1.365(7) . ? N11 C34 1.391(8) . ? C1 C2 1.510(8) . ? C3 C4 1.526(9) . ? C4 C5 1.493(11) . ? C6 C7 1.457(11) . ? C8 C9 1.455(10) . ? C9 C10 1.517(9) . ? C11 C12 1.484(9) . ? C13 C14 1.387(8) . ? C13 C18 1.388(8) . ? C14 C15 1.390(9) . ? C15 C16 1.360(10) . ? C16 C17 1.347(10) . ? C17 C18 1.397(9) . ? C19 C20 1.510(8) . ? C21 C26 1.390(8) . ? C21 C22 1.391(8) . ? C22 C23 1.377(8) . ? C23 C24 1.376(10) . ? C24 C25 1.370(10) . ? C25 C26 1.400(9) . ? C27 C28 1.464(8) . ? C29 C30 1.381(8) . ? C29 C34 1.391(8) . ? C30 C31 1.373(9) . ? C31 C32 1.395(10) . ? C32 C33 1.383(10) . ? C33 C34 1.403(9) . ? Cl1 O13 1.378(8) . ? Cl1 O14 1.392(8) . ? Cl1 O11 1.394(8) . ? Cl1 O12 1.411(9) . ? Cl1 O21 1.67(2) . ? O11 O21 1.04(3) . ? Cl2 O23 1.401(9) . ? Cl2 O24 1.402(10) . ? Cl2 O22 1.410(9) . ? Cl2 O21 1.414(10) . ? O24 O34 0.86(3) . ? Cl3 O4 0.998(18) . ? Cl3 O31 1.400(10) . ? Cl3 O34 1.403(10) . ? Cl3 O32 1.408(10) . ? Cl3 O33 1.415(10) . ? O31 O4 1.46(4) . ? O32 O4 1.09(2) . ? Cl4 O43 1.372(9) . ? Cl4 Cl4 1.38(2) 2_566 ? Cl4 O41 1.388(9) . ? Cl4 O42 1.388(9) . ? Cl4 O43 1.460(14) 2_566 ? O43 Cl4 1.460(14) 2_566 ? 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 N2 Cu1 N1 84.1(2) . . ? N2 Cu1 N4 167.2(3) . . ? N1 Cu1 N4 95.6(2) . . ? N2 Cu1 N3 96.1(2) . . ? N1 Cu1 N3 172.6(2) . . ? N4 Cu1 N3 85.9(3) . . ? O1 Mn1 N6 116.14(17) . . ? O1 Mn1 N10 111.46(17) . . ? N6 Mn1 N10 128.38(17) . . ? O1 Mn1 N8 89.87(16) . . ? N6 Mn1 N8 96.10(17) . . ? N10 Mn1 N8 102.92(17) . . ? O1 Mn1 O2 75.09(14) . . ? N6 Mn1 O2 86.92(16) . . ? N10 Mn1 O2 86.91(16) . . ? N8 Mn1 O2 164.35(15) . . ? C1 O1 Mn1 118.2(3) . . ? C2 O2 Mn1 111.8(3) . . ? C2 N1 C3 119.1(5) . . ? C2 N1 Cu1 112.2(4) . . ? C3 N1 Cu1 127.4(4) . . ? C1 N2 C10 118.5(5) . . ? C1 N2 Cu1 113.1(4) . . ? C10 N2 Cu1 128.3(4) . . ? C7 N3 C8 117.0(6) . . ? C7 N3 Cu1 106.1(5) . . ? C8 N3 Cu1 115.7(4) . . ? C5 N4 C6 113.7(6) . . ? C5 N4 Cu1 117.5(4) . . ? C6 N4 Cu1 107.3(5) . . ? C19 N5 C11 112.4(5) . . ? C19 N5 C27 110.1(5) . . ? C11 N5 C27 114.6(5) . . ? C12 N6 C13 105.4(5) . . ? C12 N6 Mn1 121.3(4) . . ? C13 N6 Mn1 133.3(4) . . ? C12 N7 C18 108.3(5) . . ? C20 N8 C21 103.6(5) . . ? C20 N8 Mn1 119.3(4) . . ? C21 N8 Mn1 136.0(4) . . ? C20 N9 C26 107.6(5) . . ? C28 N10 C29 106.7(5) . . ? C28 N10 Mn1 118.4(4) . . ? C29 N10 Mn1 134.2(4) . . ? C28 N11 C34 107.7(5) . . ? N2 C1 O1 127.6(5) . . ? N2 C1 C2 115.4(5) . . ? O1 C1 C2 116.9(5) . . ? O2 C2 N1 128.0(5) . . ? O2 C2 C1 117.7(5) . . ? N1 C2 C1 114.3(5) . . ? N1 C3 C4 111.9(5) . . ? C5 C4 C3 116.7(7) . . ? N4 C5 C4 113.1(6) . . ? C7 C6 N4 107.3(7) . . ? C6 C7 N3 110.1(7) . . ? C9 C8 N3 113.8(7) . . ? C8 C9 C10 116.3(7) . . ? N2 C10 C9 110.4(6) . . ? N5 C11 C12 111.9(5) . . ? N6 C12 N7 111.9(6) . . ? N6 C12 C11 125.3(5) . . ? N7 C12 C11 122.9(6) . . ? C14 C13 C18 119.9(6) . . ? C14 C13 N6 130.8(6) . . ? C18 C13 N6 109.3(6) . . ? C13 C14 C15 118.4(6) . . ? C16 C15 C14 120.5(7) . . ? C17 C16 C15 122.3(7) . . ? C16 C17 C18 118.5(7) . . ? N7 C18 C13 105.1(5) . . ? N7 C18 C17 134.5(7) . . ? C13 C18 C17 120.4(7) . . ? N5 C19 C20 111.1(5) . . ? N8 C20 N9 114.2(5) . . ? N8 C20 C19 123.2(5) . . ? N9 C20 C19 122.3(5) . . ? C26 C21 C22 120.8(6) . . ? C26 C21 N8 108.8(5) . . ? C22 C21 N8 130.4(5) . . ? C23 C22 C21 116.8(6) . . ? C24 C23 C22 122.6(7) . . ? C25 C24 C23 121.4(7) . . ? C24 C25 C26 116.9(7) . . ? N9 C26 C21 105.7(5) . . ? N9 C26 C25 132.8(6) . . ? C21 C26 C25 121.4(6) . . ? C28 C27 N5 108.1(5) . . ? N10 C28 N11 110.9(5) . . ? N10 C28 C27 125.3(5) . . ? N11 C28 C27 123.8(5) . . ? C30 C29 N10 130.5(5) . . ? C30 C29 C34 120.3(6) . . ? N10 C29 C34 109.1(5) . . ? C31 C30 C29 117.7(6) . . ? C30 C31 C32 122.1(7) . . ? C33 C32 C31 121.4(7) . . ? C32 C33 C34 115.9(6) . . ? N11 C34 C29 105.6(5) . . ? N11 C34 C33 131.8(6) . . ? C29 C34 C33 122.5(6) . . ? O13 Cl1 O14 104.3(8) . . ? O13 Cl1 O11 130.6(8) . . ? O14 Cl1 O11 116.3(8) . . ? O13 Cl1 O12 98.2(9) . . ? O14 Cl1 O12 98.7(10) . . ? O11 Cl1 O12 102.0(10) . . ? O13 Cl1 O21 123.5(12) . . ? O14 Cl1 O21 88.3(14) . . ? O11 Cl1 O21 38.2(12) . . ? O12 Cl1 O21 134.6(14) . . ? O21 O11 Cl1 85.5(18) . . ? O23 Cl2 O24 108.0(15) . . ? O23 Cl2 O22 106.5(13) . . ? O24 Cl2 O22 101.9(15) . . ? O23 Cl2 O21 105.4(17) . . ? O24 Cl2 O21 124.9(19) . . ? O22 Cl2 O21 109.0(16) . . ? O11 O21 Cl2 137(3) . . ? O11 O21 Cl1 56.3(10) . . ? Cl2 O21 Cl1 156(3) . . ? O34 O24 Cl2 173(6) . . ? O4 Cl3 O31 73(2) . . ? O4 Cl3 O34 143(3) . . ? O31 Cl3 O34 112(3) . . ? O4 Cl3 O32 50.2(14) . . ? O31 Cl3 O32 123(2) . . ? O34 Cl3 O32 111(2) . . ? O4 Cl3 O33 111(3) . . ? O31 Cl3 O33 102(3) . . ? O34 Cl3 O33 103(3) . . ? O32 Cl3 O33 103(2) . . ? Cl3 O31 O4 40.8(10) . . ? O4 O32 Cl3 44.9(10) . . ? O24 O34 Cl3 164(7) . . ? O43 Cl4 Cl4 64.1(9) . 2_566 ? O43 Cl4 O41 100.0(11) . . ? Cl4 Cl4 O41 115.4(13) 2_566 . ? O43 Cl4 O42 107.0(11) . . ? Cl4 Cl4 O42 120.9(15) 2_566 . ? O41 Cl4 O42 123.6(14) . . ? O43 Cl4 O43 121.9(10) . 2_566 ? Cl4 Cl4 O43 57.7(6) 2_566 2_566 ? O41 Cl4 O43 103.9(10) . 2_566 ? O42 Cl4 O43 102.1(11) . 2_566 ? Cl4 O43 Cl4 58.1(10) . 2_566 ? Cl3 O4 O32 84.9(18) . . ? Cl3 O4 O31 66.4(17) . . ? O32 O4 O31 151(2) . . ? _diffrn_measured_fraction_theta_max 0.972 _diffrn_reflns_theta_full 25.03 _diffrn_measured_fraction_theta_full 0.972 _refine_diff_density_max 0.739 _refine_diff_density_min -0.302 _refine_diff_density_rms 0.077 data_1 _database_code_CSD 171325 _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_formula_moiety ? _chemical_formula_sum 'C34 H37 Cl2 Cu Mn N8 O11.50' _chemical_formula_weight 931.10 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' '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 Monoclinic _symmetry_space_group_name_H-M C2/c 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 31.133(6) _cell_length_b 16.989(3) _cell_length_c 14.827(3) _cell_angle_alpha 90.00 _cell_angle_beta 97.25(3) _cell_angle_gamma 90.00 _cell_volume 7780(3) _cell_formula_units_Z 8 _cell_measurement_temperature 293(2) _cell_measurement_reflns_used 4249 _cell_measurement_theta_min 1.32 _cell_measurement_theta_max 25.03 _exptl_crystal_description 'Prism' _exptl_crystal_colour 'Red' _exptl_crystal_size_max .42 _exptl_crystal_size_mid .42 _exptl_crystal_size_min .24 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.590 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 3816 _exptl_absorpt_coefficient_mu 1.080 _exptl_absorpt_correction_type empirical _exptl_absorpt_process_details 'SADABS (Sheldrick, 1996)' _exptl_absorpt_correction_T_min 0.5662 _exptl_absorpt_correction_T_max 0.8309 _exptl_special_details ; ? ; _diffrn_ambient_temperature 293(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 none _diffrn_standards_interval_count none _diffrn_standards_interval_time none _diffrn_standards_decay_% none _diffrn_reflns_number 11743 _diffrn_reflns_av_R_equivalents 0.0409 _diffrn_reflns_av_sigmaI/netI 0.0559 _diffrn_reflns_limit_h_min -35 _diffrn_reflns_limit_h_max 36 _diffrn_reflns_limit_k_min -17 _diffrn_reflns_limit_k_max 20 _diffrn_reflns_limit_l_min -8 _diffrn_reflns_limit_l_max 17 _diffrn_reflns_theta_min 1.89 _diffrn_reflns_theta_max 25.02 _reflns_number_total 6716 _reflns_number_gt 4515 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'Siemens SMART' _computing_cell_refinement 'Siemens SMART & SAINT' _computing_data_reduction 'Siemens XPREP' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'Siemens SHELXTL' _computing_publication_material 'Siemens SHELXTL' _refine_special_details ; Refinement of F^2^ against ALL reflections. The weighted R-factor wR and goodness of fit S are based on F^2^, conventional R-factors R are based on F, with F set to zero for negative F^2^. The threshold expression of F^2^ > 2sigma(F^2^) is used only for calculating R-factors(gt) etc. and is not relevant to the choice of reflections for refinement. R-factors based on F^2^ are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger. ; _refine_ls_structure_factor_coef Fsqd _refine_ls_matrix_type full _refine_ls_weighting_scheme 'calc w=1/[\s^2^(Fo^2^)+(0.0384P)^2^+56.8006P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment mixed _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 6716 _refine_ls_number_parameters 532 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.1171 _refine_ls_R_factor_gt 0.0709 _refine_ls_wR_factor_ref 0.1690 _refine_ls_wR_factor_gt 0.1389 _refine_ls_goodness_of_fit_ref 1.123 _refine_ls_restrained_S_all 1.123 _refine_ls_shift/su_max 0.028 _refine_ls_shift/su_mean 0.002 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_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group Cu1 Cu 0.37071(2) 0.11453(5) 0.36756(5) 0.0509(2) Uani 1 d . . . Mn1 Mn 0.38639(3) 0.32227(6) 0.09614(7) 0.0506(3) Uani 1 d . . . N1 N 0.40040(16) 0.1220(3) 0.2608(3) 0.0471(12) Uani 1 d . . . N2 N 0.35067(16) 0.2208(3) 0.3338(3) 0.0495(13) Uani 1 d . . . N3 N 0.3305(2) 0.1003(4) 0.4616(4) 0.0704(17) Uani 1 d . . . N4 N 0.3978(2) 0.0133(4) 0.4137(4) 0.0710(17) Uani 1 d . . . N5 N 0.31656(17) 0.3343(3) 0.0314(4) 0.0526(13) Uani 1 d . . . N6 N 0.38528(16) 0.2927(3) -0.0524(3) 0.0505(13) Uani 1 d . . . N7 N 0.45912(17) 0.3449(4) 0.1163(4) 0.0564(14) Uani 1 d . . . N8 N 0.3960(2) 0.4547(3) 0.1008(4) 0.0628(15) Uani 1 d . . . O1 O 0.39999(15) 0.2024(3) 0.1349(3) 0.0565(12) Uani 1 d . . . O2 O 0.36137(14) 0.3143(3) 0.2256(3) 0.0544(11) Uani 1 d . . . C1 C 0.4260(2) 0.0604(4) 0.2235(5) 0.065(2) Uani 1 d . . . H1A H 0.4477 0.0844 0.1918 0.080 Uiso 1 d R . . H1B H 0.4072 0.0301 0.1804 0.080 Uiso 1 d R . . C2 C 0.39050(18) 0.1851(4) 0.2129(4) 0.0452(15) Uani 1 d . . . C3 C 0.36506(18) 0.2462(4) 0.2608(4) 0.0433(14) Uani 1 d . . . C4 C 0.3279(2) 0.2748(5) 0.3872(5) 0.067(2) Uani 1 d . . . H4A H 0.3112 0.3107 0.3469 0.080 Uiso 1 d R . . H4B H 0.3490 0.3048 0.4257 0.080 Uiso 1 d R . . C5 C 0.2998(3) 0.2352(6) 0.4465(6) 0.093(3) Uani 1 d . . . H5A H 0.2760 0.2136 0.4067 0.080 Uiso 1 d R . . H5B H 0.2881 0.2741 0.4835 0.080 Uiso 1 d R . . C6 C 0.3175(3) 0.1699(6) 0.5054(6) 0.096(3) Uani 1 d . . . H6A H 0.3425 0.1902 0.5428 0.080 Uiso 1 d R . . H6B H 0.2967 0.1555 0.5450 0.080 Uiso 1 d R . . C7 C 0.3456(3) 0.0341(6) 0.5189(6) 0.088(3) Uani 1 d . . . H7A H 0.3216 0.0101 0.5432 0.080 Uiso 1 d R . . H7B H 0.3655 0.0532 0.5690 0.080 Uiso 1 d R . . C8 C 0.3682(3) -0.0251(5) 0.4683(6) 0.078(2) Uani 1 d . . . H8A H 0.3841 -0.0612 0.5097 0.080 Uiso 1 d R . . H8B H 0.3470 -0.0545 0.4294 0.080 Uiso 1 d R . . C9 C 0.4169(3) -0.0364(5) 0.3500(6) 0.077(2) Uani 1 d . . . H9A H 0.3942 -0.0600 0.3089 0.080 Uiso 1 d R . . H9B H 0.4325 -0.0780 0.3834 0.080 Uiso 1 d R . . C10 C 0.4462(3) 0.0048(5) 0.2938(6) 0.087(3) Uani 1 d . . . H10A H 0.4658 0.0355 0.3348 0.080 Uiso 1 d R . . H10B H 0.4631 -0.0333 0.2658 0.080 Uiso 1 d R . . C11 C 0.2827(2) 0.3529(4) 0.0737(5) 0.0592(18) Uani 1 d . . . H11A H 0.2875 0.3612 0.1382 0.080 Uiso 1 d R . . C12 C 0.2406(2) 0.3600(4) 0.0293(6) 0.0642(19) Uani 1 d . . . H12A H 0.2172 0.3747 0.0622 0.080 Uiso 1 d R . . C13 C 0.2331(2) 0.3465(4) -0.0620(6) 0.068(2) Uani 1 d . . . H13A H 0.2043 0.3500 -0.0939 0.080 Uiso 1 d R . . C14 C 0.2679(2) 0.3261(4) -0.1095(5) 0.0573(17) Uani 1 d . . . C15 C 0.2628(2) 0.3076(5) -0.2039(5) 0.072(2) Uani 1 d . . . H15A H 0.2346 0.3121 -0.2382 0.080 Uiso 1 d R . . C16 C 0.2963(3) 0.2841(5) -0.2442(6) 0.080(2) Uani 1 d . . . H16A H 0.2917 0.2708 -0.3077 0.080 Uiso 1 d R . . C17 C 0.3392(2) 0.2772(4) -0.1962(5) 0.0602(18) Uani 1 d . . . C18 C 0.3753(2) 0.2510(5) -0.2347(5) 0.069(2) Uani 1 d . . . H18A H 0.3719 0.2349 -0.2973 0.080 Uiso 1 d R . . C19 C 0.4149(2) 0.2473(4) -0.1841(5) 0.0643(19) Uani 1 d . . . H19A H 0.4399 0.2299 -0.2106 0.080 Uiso 1 d R . . C20 C 0.4181(2) 0.2690(4) -0.0931(5) 0.0594(18) Uani 1 d . . . H20A H 0.4461 0.2674 -0.0575 0.080 Uiso 1 d R . . C21 C 0.3095(2) 0.3207(4) -0.0597(4) 0.0492(15) Uani 1 d . . . C22 C 0.34564(19) 0.2972(4) -0.1040(4) 0.0465(15) Uani 1 d . . . C31 C 0.4896(2) 0.2909(5) 0.1237(5) 0.073(2) Uani 1 d . . . H31A H 0.4809 0.2367 0.1223 0.080 Uiso 1 d R . . C32 C 0.5336(3) 0.3089(7) 0.1332(6) 0.088(3) Uani 1 d . . . H32A H 0.5549 0.2677 0.1391 0.080 Uiso 1 d R . . C33 C 0.5460(3) 0.3856(7) 0.1356(6) 0.090(3) Uani 1 d . . . H33A H 0.5762 0.3990 0.1416 0.080 Uiso 1 d R . . C34 C 0.5151(3) 0.4453(6) 0.1282(5) 0.073(2) Uani 1 d . . . C35 C 0.5246(3) 0.5270(7) 0.1301(6) 0.096(3) Uani 1 d . . . H35A H 0.5544 0.5433 0.1391 0.080 Uiso 1 d R . . C36 C 0.4942(3) 0.5809(6) 0.1214(6) 0.092(3) Uani 1 d . . . H36A H 0.5020 0.6355 0.1203 0.080 Uiso 1 d R . . C37 C 0.4493(3) 0.5596(5) 0.1115(5) 0.074(2) Uani 1 d . . . C38 C 0.4158(4) 0.6137(5) 0.1026(7) 0.097(3) Uani 1 d . . . H38A H 0.4222 0.6690 0.1037 0.080 Uiso 1 d R . . C39 C 0.3740(4) 0.5888(6) 0.0941(7) 0.104(3) Uani 1 d . . . H39A H 0.3505 0.6258 0.0861 0.080 Uiso 1 d R . . C40 C 0.3654(3) 0.5088(5) 0.0933(7) 0.090(3) Uani 1 d . . . H40A H 0.3358 0.4913 0.0876 0.080 Uiso 1 d R . . C41 C 0.4381(2) 0.4801(5) 0.1098(5) 0.0616(19) Uani 1 d . . . C42 C 0.4711(2) 0.4214(5) 0.1192(4) 0.0605(19) Uani 1 d . . . Cl1 Cl 0.27505(8) -0.02301(14) 0.23992(15) 0.0823(6) Uani 1 d . . . O11 O 0.2510(3) 0.0010(5) 0.3103(6) 0.171(4) Uani 1 d . . . O12 O 0.3077(2) 0.0340(4) 0.2367(5) 0.123(2) Uani 1 d . . . O13 O 0.2487(3) -0.0212(5) 0.1570(5) 0.144(3) Uani 1 d . . . O14 O 0.2926(3) -0.0964(4) 0.2589(6) 0.164(4) Uani 1 d . . . Cl2 Cl 0.45930(6) 0.15627(12) -0.43249(14) 0.0694(5) Uani 1 d . . . O21 O 0.4258(2) 0.1851(4) -0.4946(6) 0.136(3) Uani 1 d . . . O22 O 0.4935(5) 0.1488(10) -0.4922(11) 0.129(5) Uani 0.50 d P . . O22' O 0.4306(6) 0.1476(13) -0.3606(11) 0.163(7) Uani 0.50 d P . . O23 O 0.4823(3) 0.2097(6) -0.3835(8) 0.193(5) Uani 1 d . . . O24 O 0.4618(3) 0.0771(5) -0.4228(7) 0.174(4) Uani 1 d . . . O4 O 0.3526(3) 0.4775(6) 0.3169(7) 0.179(4) Uani 1 d . . . O5 O 0.2328(5) 0.0738(10) 0.4616(12) 0.141(6) Uani 0.50 d P . . 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 0.0470(5) 0.0612(5) 0.0445(4) 0.0045(4) 0.0053(3) 0.0003(4) Mn1 0.0461(6) 0.0574(6) 0.0467(6) 0.0052(5) -0.0004(4) 0.0013(5) N1 0.047(3) 0.051(3) 0.042(3) -0.002(3) 0.004(2) 0.001(3) N2 0.044(3) 0.063(4) 0.042(3) 0.000(3) 0.004(2) 0.007(3) N3 0.064(4) 0.087(5) 0.064(4) 0.021(4) 0.023(3) 0.005(3) N4 0.083(4) 0.064(4) 0.068(4) 0.020(3) 0.014(3) 0.005(3) N5 0.046(3) 0.059(4) 0.052(3) 0.006(3) 0.001(3) -0.001(3) N6 0.043(3) 0.060(3) 0.047(3) 0.004(3) 0.001(2) 0.000(3) N7 0.048(3) 0.073(4) 0.047(3) 0.003(3) -0.001(2) 0.004(3) N8 0.068(4) 0.054(4) 0.065(4) 0.002(3) 0.001(3) 0.001(3) O1 0.072(3) 0.057(3) 0.043(3) 0.005(2) 0.015(2) 0.010(2) O2 0.059(3) 0.053(3) 0.050(3) 0.005(2) 0.003(2) 0.013(2) C1 0.081(5) 0.057(4) 0.059(4) -0.002(4) 0.019(4) 0.015(4) C2 0.037(3) 0.056(4) 0.041(4) 0.000(3) -0.002(3) 0.002(3) C3 0.037(3) 0.056(4) 0.035(3) -0.004(3) -0.004(3) 0.000(3) C4 0.066(5) 0.087(6) 0.048(4) -0.007(4) 0.010(3) 0.015(4) C5 0.086(6) 0.125(8) 0.074(6) 0.004(6) 0.034(5) 0.031(6) C6 0.082(6) 0.146(9) 0.064(5) 0.017(6) 0.026(5) 0.034(6) C7 0.089(6) 0.110(7) 0.068(5) 0.026(5) 0.026(5) 0.003(5) C8 0.073(5) 0.081(6) 0.078(6) 0.026(5) -0.002(4) -0.016(5) C9 0.082(6) 0.058(5) 0.089(6) 0.005(4) 0.007(5) 0.002(4) C10 0.098(7) 0.074(6) 0.092(6) 0.007(5) 0.025(5) 0.030(5) C11 0.049(4) 0.064(4) 0.064(4) 0.005(4) 0.004(3) 0.001(3) C12 0.047(4) 0.065(5) 0.081(5) 0.002(4) 0.008(4) 0.010(3) C13 0.048(4) 0.065(5) 0.090(6) -0.004(4) 0.000(4) 0.005(4) C14 0.056(4) 0.047(4) 0.066(5) 0.002(3) -0.005(3) 0.001(3) C15 0.054(4) 0.080(5) 0.073(5) -0.011(4) -0.022(4) 0.018(4) C16 0.076(6) 0.093(6) 0.065(5) -0.019(5) -0.020(4) 0.019(5) C17 0.063(4) 0.064(5) 0.050(4) 0.000(4) -0.006(3) 0.006(4) C18 0.075(5) 0.080(5) 0.049(4) -0.004(4) 0.000(4) 0.009(4) C19 0.059(5) 0.071(5) 0.061(5) 0.001(4) 0.005(4) 0.006(4) C20 0.046(4) 0.075(5) 0.057(4) 0.001(4) 0.006(3) -0.001(4) C21 0.046(4) 0.044(4) 0.055(4) 0.006(3) -0.004(3) 0.004(3) C22 0.041(3) 0.046(4) 0.050(4) 0.005(3) -0.006(3) -0.003(3) C31 0.060(5) 0.093(6) 0.062(5) 0.001(4) -0.007(4) 0.018(4) C32 0.051(5) 0.133(9) 0.076(6) -0.003(6) -0.006(4) 0.022(5) C33 0.051(5) 0.146(9) 0.071(6) -0.011(6) -0.003(4) -0.007(6) C34 0.065(5) 0.107(7) 0.045(4) -0.004(4) 0.003(4) -0.015(5) C35 0.067(6) 0.135(10) 0.087(7) -0.003(6) 0.009(5) -0.036(6) C36 0.084(7) 0.104(8) 0.088(6) 0.001(6) 0.006(5) -0.050(6) C37 0.089(6) 0.068(5) 0.067(5) 0.000(4) 0.013(4) -0.012(5) C38 0.129(9) 0.056(5) 0.106(7) 0.006(5) 0.016(6) -0.029(6) C39 0.106(8) 0.070(6) 0.135(9) 0.008(6) 0.006(7) 0.004(6) C40 0.070(6) 0.066(6) 0.131(8) 0.006(5) 0.003(5) 0.003(5) C41 0.062(5) 0.069(5) 0.051(4) 0.003(4) -0.004(3) -0.020(4) C42 0.055(4) 0.086(6) 0.038(4) 0.001(4) -0.003(3) -0.010(4) Cl1 0.0911(15) 0.0853(16) 0.0698(14) 0.0073(12) 0.0076(12) -0.0041(13) O11 0.218(10) 0.164(8) 0.153(8) 0.036(6) 0.110(7) 0.046(7) O12 0.103(5) 0.121(6) 0.141(6) 0.014(5) -0.003(4) -0.032(4) O13 0.127(6) 0.176(8) 0.116(6) 0.000(5) -0.031(5) -0.034(6) O14 0.249(11) 0.075(5) 0.165(8) 0.015(5) 0.019(7) 0.038(6) Cl2 0.0663(12) 0.0639(13) 0.0729(13) -0.0005(10) -0.0106(10) -0.0043(10) O21 0.105(5) 0.123(6) 0.163(7) 0.048(5) -0.057(5) -0.021(4) O22 0.124(12) 0.145(13) 0.125(12) 0.023(10) 0.038(10) 0.050(10) O22' 0.155(15) 0.23(2) 0.114(12) -0.020(13) 0.073(11) -0.039(15) O23 0.152(8) 0.154(8) 0.248(12) -0.060(8) -0.072(8) -0.025(7) O24 0.186(9) 0.105(6) 0.204(10) 0.028(6) -0.076(8) 0.006(6) O4 0.129(7) 0.201(10) 0.202(10) 0.010(8) -0.003(7) 0.011(7) O5 0.095(10) 0.140(13) 0.180(16) -0.019(11) -0.016(10) -0.025(9) _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 N1 1.935(5) . ? Cu1 N2 1.955(5) . ? Cu1 N4 1.997(6) . ? Cu1 N3 2.002(6) . ? Mn1 O1 2.143(4) . ? Mn1 O2 2.165(4) . ? Mn1 N6 2.254(5) . ? Mn1 N8 2.269(6) . ? Mn1 N5 2.273(5) . ? Mn1 N7 2.279(6) . ? N1 C2 1.301(8) . ? N1 C1 1.466(8) . ? N2 C3 1.296(8) . ? N2 C4 1.453(8) . ? N3 C6 1.433(11) . ? N3 C7 1.450(10) . ? N4 C9 1.450(10) . ? N4 C8 1.457(9) . ? N5 C11 1.331(8) . ? N5 C21 1.360(8) . ? N6 C20 1.316(8) . ? N6 C22 1.370(7) . ? N7 C31 1.316(9) . ? N7 C42 1.351(9) . ? N8 C40 1.321(9) . ? N8 C41 1.369(9) . ? O1 C2 1.265(7) . ? O2 C3 1.267(7) . ? C1 C10 1.486(10) . ? C2 C3 1.534(8) . ? C4 C5 1.479(11) . ? C5 C6 1.475(11) . ? C7 C8 1.485(11) . ? C9 C10 1.486(11) . ? C11 C12 1.395(9) . ? C12 C13 1.364(10) . ? C13 C14 1.408(10) . ? C14 C21 1.410(9) . ? C14 C15 1.424(10) . ? C15 C16 1.326(11) . ? C16 C17 1.438(10) . ? C17 C18 1.396(10) . ? C17 C22 1.398(9) . ? C18 C19 1.362(10) . ? C19 C20 1.390(9) . ? C21 C22 1.430(9) . ? C31 C32 1.393(11) . ? C32 C33 1.359(12) . ? C33 C34 1.392(12) . ? C34 C35 1.418(13) . ? C34 C42 1.418(10) . ? C35 C36 1.312(13) . ? C36 C37 1.433(12) . ? C37 C41 1.394(10) . ? C37 C38 1.384(12) . ? C38 C39 1.359(13) . ? C39 C40 1.386(12) . ? C41 C42 1.427(10) . ? Cl1 O14 1.376(7) . ? Cl1 O13 1.389(7) . ? Cl1 O12 1.409(7) . ? Cl1 O11 1.419(8) . ? Cl2 O23 1.317(8) . ? Cl2 O24 1.354(8) . ? Cl2 O21 1.390(6) . ? Cl2 O22 1.474(14) . ? Cl2 O22' 1.483(14) . ? 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 N1 Cu1 N2 84.2(2) . . ? N1 Cu1 N4 96.4(2) . . ? N2 Cu1 N4 171.9(2) . . ? N1 Cu1 N3 169.3(2) . . ? N2 Cu1 N3 94.8(2) . . ? N4 Cu1 N3 86.0(3) . . ? O1 Mn1 O2 77.50(16) . . ? O1 Mn1 N6 91.62(18) . . ? O2 Mn1 N6 152.75(18) . . ? O1 Mn1 N8 155.9(2) . . ? O2 Mn1 N8 95.5(2) . . ? N6 Mn1 N8 103.7(2) . . ? O1 Mn1 N5 110.18(19) . . ? O2 Mn1 N5 87.04(18) . . ? N6 Mn1 N5 73.22(19) . . ? N8 Mn1 N5 92.3(2) . . ? O1 Mn1 N7 88.1(2) . . ? O2 Mn1 N7 110.92(18) . . ? N6 Mn1 N7 93.34(19) . . ? N8 Mn1 N7 72.7(2) . . ? N5 Mn1 N7 157.2(2) . . ? C2 N1 C1 119.0(5) . . ? C2 N1 Cu1 113.3(4) . . ? C1 N1 Cu1 126.9(4) . . ? C3 N2 C4 119.3(6) . . ? C3 N2 Cu1 112.9(4) . . ? C4 N2 Cu1 127.2(4) . . ? C6 N3 C7 117.6(7) . . ? C6 N3 Cu1 116.9(5) . . ? C7 N3 Cu1 108.5(5) . . ? C9 N4 C8 116.2(6) . . ? C9 N4 Cu1 117.9(5) . . ? C8 N4 Cu1 107.9(5) . . ? C11 N5 C21 118.0(6) . . ? C11 N5 Mn1 126.5(5) . . ? C21 N5 Mn1 115.5(4) . . ? C20 N6 C22 117.3(6) . . ? C20 N6 Mn1 126.9(4) . . ? C22 N6 Mn1 115.8(4) . . ? C31 N7 C42 118.3(7) . . ? C31 N7 Mn1 126.0(5) . . ? C42 N7 Mn1 115.7(5) . . ? C40 N8 C41 117.4(7) . . ? C40 N8 Mn1 126.6(5) . . ? C41 N8 Mn1 116.0(5) . . ? C2 O1 Mn1 113.9(4) . . ? C3 O2 Mn1 113.5(4) . . ? N1 C1 C10 113.0(6) . . ? O1 C2 N1 128.7(6) . . ? O1 C2 C3 117.4(6) . . ? N1 C2 C3 113.9(5) . . ? O2 C3 N2 128.7(6) . . ? O2 C3 C2 116.9(5) . . ? N2 C3 C2 114.4(6) . . ? N2 C4 C5 113.8(7) . . ? C6 C5 C4 119.2(7) . . ? N3 C6 C5 117.3(7) . . ? N3 C7 C8 111.6(7) . . ? N4 C8 C7 110.5(7) . . ? N4 C9 C10 115.0(7) . . ? C9 C10 C1 117.2(7) . . ? N5 C11 C12 123.4(7) . . ? C13 C12 C11 119.2(7) . . ? C12 C13 C14 119.4(7) . . ? C13 C14 C21 117.9(7) . . ? C13 C14 C15 123.3(7) . . ? C21 C14 C15 118.8(7) . . ? C16 C15 C14 120.9(7) . . ? C15 C16 C17 122.3(7) . . ? C18 C17 C22 117.0(6) . . ? C18 C17 C16 124.7(7) . . ? C22 C17 C16 118.3(7) . . ? C19 C18 C17 120.6(7) . . ? C18 C19 C20 118.1(7) . . ? N6 C20 C19 124.2(6) . . ? N5 C21 C14 122.1(6) . . ? N5 C21 C22 117.7(5) . . ? C14 C21 C22 120.1(6) . . ? N6 C22 C17 122.7(6) . . ? N6 C22 C21 117.7(6) . . ? C17 C22 C21 119.5(6) . . ? N7 C31 C32 123.1(9) . . ? C33 C32 C31 119.1(9) . . ? C32 C33 C34 120.3(8) . . ? C33 C34 C35 124.8(9) . . ? C33 C34 C42 116.7(8) . . ? C35 C34 C42 118.6(9) . . ? C36 C35 C34 122.4(9) . . ? C35 C36 C37 121.1(9) . . ? C41 C37 C38 117.3(8) . . ? C41 C37 C36 119.0(9) . . ? C38 C37 C36 123.7(9) . . ? C39 C38 C37 120.2(9) . . ? C38 C39 C40 119.3(10) . . ? N8 C40 C39 123.0(9) . . ? N8 C41 C37 122.8(8) . . ? N8 C41 C42 117.2(6) . . ? C37 C41 C42 120.0(7) . . ? N7 C42 C34 122.6(8) . . ? N7 C42 C41 118.4(6) . . ? C34 C42 C41 119.0(8) . . ? O14 Cl1 O13 112.1(6) . . ? O14 Cl1 O12 111.2(6) . . ? O13 Cl1 O12 107.6(5) . . ? O14 Cl1 O11 110.0(6) . . ? O13 Cl1 O11 109.6(6) . . ? O12 Cl1 O11 106.1(6) . . ? O23 Cl2 O24 127.3(6) . . ? O23 Cl2 O21 115.6(6) . . ? O24 Cl2 O21 116.7(5) . . ? O23 Cl2 O22 90.4(9) . . ? O24 Cl2 O22 86.6(8) . . ? O21 Cl2 O22 99.8(7) . . ? O23 Cl2 O22' 90.4(9) . . ? O24 Cl2 O22' 81.8(9) . . ? O21 Cl2 O22' 92.4(9) . . ? O22 Cl2 O22' 166.0(10) . . ? _diffrn_measured_fraction_theta_max 0.993 _diffrn_reflns_theta_full 25.02 _diffrn_measured_fraction_theta_full 0.993 _refine_diff_density_max 0.428 _refine_diff_density_min -0.408 _refine_diff_density_rms 0.076 #===END