Supplementary Material (ESI) for Dalton Transactions This journal is © The Royal Society of Chemistry 2006 data_global _journal_name_full 'Dalton Trans.' _journal_coden_Cambridge 0222 _audit_creation_date 29-07-02 _publ_contact_author_name 'Jean Pierre Djukic' _publ_contact_author_address ;UMR 7513 CNRS Universite Louis Pasteur 4, rue Blaise Pascal F 67000 Strasbourg FRANCE ; _publ_contact_author_email djukic@chimie.u-strasbg.fr _publ_contact_author_phone 33(0)390241523 _publ_contact_author_fax 33(0)390245001 loop_ _publ_author_name _publ_author_address J.P.Djukic ;UMR 7513 CNRS Universite Louis Pasteur 4, rue Blaise Pascal F 67000 Strasbourg FRANCE ; C.Michon ;UMR 7513 CNRS Universite Louis Pasteur 4, rue Blaise Pascal F 67000 Strasbourg FRANCE ; M.Pfeffer ;UMR 7513 CNRS Universite Louis Pasteur 4, rue Blaise Pascal F 67000 Strasbourg FRANCE ; 'A.De Cian' ;UMR 7513 CNRS Universite Louis Pasteur 4, rue Blaise Pascal F 67000 Strasbourg FRANCE ; 'N.Kyritsakas Gruber' ;UMR 7513 CNRS Universite Louis Pasteur 4, rue Blaise Pascal F 67000 Strasbourg FRANCE ; _publ_section_title ; New metallo-organic triple-deckers based on quinoxaline, pyrazine and pyrimidine cores. ; _publ_section_references ; Burla, M.C., Camalli, M., Cascarano, G.,Giacovazzo, C., Polidori, G., Spagna, R. &Viterbo, D. (1989). SIR. J. Appl. Cryst. 22, 389-393. OpenMoleN, Interactive Intelligent Structure solution (1997) Nonius B.V., Delft, The Netherlands. KappaCCD Operation Manual (1997), Nonius B.V., Delft, The Nederlands. Otwinowski, Z. & Minor, W. (1997), Methods in Enzymology, 276, 307-326. Walker, N. & Stuart, D. (1983). Acta Cryst., A39, 158-166. ; data_1c _database_code_depnum_ccdc_archive 'CCDC 284341' #=============================================================================== # 5. CHEMICAL DATA _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_formula_moiety 'C55 H48 Mn2 N2 O6' _chemical_formula_structural ? _chemical_formula_analytical ? _chemical_formula_sum 'C55 H48 Mn2 N2 O6' _chemical_formula_weight 942.88 _chemical_melting_point ? _chemical_compound_source ? loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source C ? 0.002 0.002 International_Tables_Vol_IV_Table_2.3.1 H ? 0.000 0.000 International_Tables_Vol_IV_Table_2.3.1 Mn ? 0.295 0.729 International_Tables_Vol_IV_Table_2.3.1 N ? 0.004 0.003 International_Tables_Vol_IV_Table_2.3.1 O ? 0.008 0.006 International_Tables_Vol_IV_Table_2.3.1 #=============================================================================== # 6. CRYSTAL DATA _symmetry_cell_setting monoclinic _symmetry_space_group_name_H-M 'P 1 21/n 1' _symmetry_space_group_name_Hall '-P 2yn' loop_ _symmetry_equiv_pos_as_xyz x,y,z 1/2-x,1/2+y,1/2-z -x,-y,-z 1/2+x,1/2-y,1/2+z _cell_length_a 10.4636(1) _cell_length_b 28.2835(3) _cell_length_c 15.5722(2) _cell_angle_alpha 90 _cell_angle_beta 100.253(5) _cell_angle_gamma 90 _cell_volume 4534.96(11) _cell_formula_units_Z 4 _cell_measurement_temperature 173 _cell_measurement_reflns_used 12451 _cell_measurement_theta_min 1.4 _cell_measurement_theta_max 29.1 _cell_special_details ; Cell parameters refined using Scalepack part of DENZO Z. Otwinowski, W. Minor, 1997 ; _exptl_crystal_description prism _exptl_crystal_colour yellow _exptl_crystal_size_max 0.10 _exptl_crystal_size_mid 0.08 _exptl_crystal_size_min 0.08 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.38 _exptl_crystal_density_method none _exptl_crystal_F_000 1960 _exptl_absorpt_coefficient_mu 0.612 _exptl_absorpt_correction_type refdelf_(Walker_&_Stuart,_1983) _exptl_absorpt_correction_T_min 0.9414 _exptl_absorpt_correction_T_max 1.0000 #=============================================================================== # 7. EXPERIMENTAL DATA _diffrn_special_details ; ? ; _diffrn_ambient_temperature 173 _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type Mo-K\a _diffrn_source xray_tube _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type KappaCCD _diffrn_measurement_method '\p scans' _diffrn_measurement_details ; 12451 reflections were collected using program Collect ("Collect" Data collection software, Nonius B.V., 1998) The conditions were as follow : crystal to detector distance = 36. mm. Scan angle = 1.1 deg 1 scans of 40 sec per frame. Data collection was divided into 2 set(s) with the following starting angles and number of frames : Set 1 Theta = 7.80 Omega = 0.00 Kappa = 0.00 332 frames Set 2 Theta = -7.20 Kappa = -144.00 Phi = 0.00 33 frames Friedel pairs were averaged. Internal R = 0.04 ; _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% 0 _diffrn_reflns_number 12451 _diffrn_reflns_av_R_equivalents 0.040 _diffrn_reflns_av_sigmaI/netI 0.333 _diffrn_reflns_limit_h_min 0 _diffrn_reflns_limit_h_max 14 _diffrn_reflns_limit_k_min 0 _diffrn_reflns_limit_k_max 38 _diffrn_reflns_limit_l_min -21 _diffrn_reflns_limit_l_max 20 _diffrn_reflns_theta_min 2.5 _diffrn_reflns_theta_max 29.13 _reflns_number_total 12451 _reflns_number_gt 6562 _reflns_threshold_expression >3.0\s(I) _computing_structure_solution Direct_methods_(SIR,_Burla_et_al.,_1989) _computing_structure_refinement LSFM_OpenMoleN_(_1997) _computing_molecular_graphics ? _computing_publication_material CIFGEN_IN_OpenMoleN_(_1997) #=============================================================================== # 8. REFINEMENT DATA _refine_ls_structure_factor_coef F _refine_ls_matrix_type full _refine_ls_weighting_scheme sigma _refine_ls_hydrogen_treatment noref _refine_ls_extinction_method none _refine_ls_extinction_expression ? _refine_ls_extinction_coef ? _refine_ls_abs_structure_Flack ? _refine_ls_number_reflns 6562 _refine_ls_number_parameters 586 _refine_ls_number_restraints 0 _refine_ls_number_constraints 0 _refine_ls_R_factor_all 0.102 _refine_ls_R_factor_gt 0.040 _refine_ls_wR_factor_all 0.243 _refine_ls_wR_factor_ref 0.058 _refine_ls_goodness_of_fit_all 1.364 _refine_ls_goodness_of_fit_ref 1.052 _refine_ls_shift/su_max 0.006 _refine_ls_shift/esd_mean 0.000 _refine_diff_density_max 0.448 _refine_diff_density_min -0.118 #=============================================================================== # 9. ATOMIC COORDINATES AND THERMAL PARAMETERS loop_ _atom_site_label _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_calc_flag _atom_site_calc_attached_atom _atom_site_type_symbol MN1 0.73790(4) 0.18657(1) 0.52237(2) 0.0241(2) Uani ? ? Mn MN2 0.38654(3) 0.08715(1) 0.78153(2) 0.0204(2) Uani ? ? Mn C1 0.8200(3) 0.2255(1) 0.6083(2) 0.036(1) Uani ? ? C O1 0.8804(2) 0.25190(8) 0.6556(1) 0.057(1) Uani ? ? O C2 0.8945(3) 0.1882(1) 0.4888(1) 0.031(1) Uani ? ? C O2 0.9984(2) 0.19165(8) 0.4765(1) 0.046(1) Uani ? ? O C3 0.6824(3) 0.2330(1) 0.4467(2) 0.034(1) Uani ? ? C O3 0.6515(2) 0.26304(8) 0.3973(1) 0.050(1) Uani ? ? O C4 0.3481(2) 0.0363(1) 0.8418(2) 0.026(1) Uani ? ? C O4 0.3141(2) 0.00256(7) 0.8727(1) 0.038(1) Uani ? ? O C5 0.2530(3) 0.1167(1) 0.8162(2) 0.028(1) Uani ? ? C O5 0.1642(2) 0.13275(8) 0.8397(1) 0.047(1) Uani ? ? O C6 0.2931(2) 0.05589(9) 0.6892(2) 0.024(1) Uani ? ? C O6 0.2324(2) 0.03330(7) 0.6352(1) 0.032(1) Uani ? ? O N1 0.5865(2) 0.17740(7) 0.5873(1) 0.023(1) Uani ? ? N C7 0.4767(2) 0.19916(9) 0.6033(2) 0.026(1) Uani ? ? C C8 0.4389(3) 0.2433(1) 0.5654(2) 0.044(2) Uani ? ? C C9 0.3232(3) 0.2625(1) 0.5772(2) 0.059(2) Uani ? ? C C10 0.2428(3) 0.2396(1) 0.6275(2) 0.052(2) Uani ? ? C C11 0.2789(3) 0.1974(1) 0.6665(2) 0.034(1) Uani ? ? C C12 0.3982(2) 0.17659(9) 0.6570(2) 0.024(1) Uani ? ? C N2 0.4416(2) 0.13588(7) 0.6991(1) 0.020(1) Uani ? ? N C13 0.5524(2) 0.11669(9) 0.6876(1) 0.019(1) Uani ? ? C C14 0.6224(2) 0.13637(9) 0.6262(2) 0.019(1) Uani ? ? C C15 0.7401(2) 0.11703(9) 0.5971(2) 0.020(1) Uani ? ? C C16 0.8431(2) 0.1011(1) 0.6617(2) 0.026(1) Uani ? ? C C17 0.9459(2) 0.0770(1) 0.6425(2) 0.032(1) Uani ? ? C C18 0.9474(2) 0.0660(1) 0.5544(2) 0.033(1) Uani ? ? C C19 0.8527(2) 0.0815(1) 0.4890(2) 0.027(1) Uani ? ? C C20 0.7426(2) 0.10880(9) 0.5043(1) 0.022(1) Uani ? ? C C21 0.6453(2) 0.12972(9) 0.4357(1) 0.023(1) Uani ? ? C C22 0.5064(2) 0.1191(1) 0.4430(1) 0.022(1) Uani ? ? C C23 0.4726(2) 0.0731(1) 0.4639(2) 0.026(1) Uani ? ? C C24 0.3442(3) 0.0612(1) 0.4682(2) 0.034(1) Uani ? ? C C25 0.2479(3) 0.0947(1) 0.4515(2) 0.036(2) Uani ? ? C C26 0.2787(3) 0.1407(1) 0.4308(2) 0.036(2) Uani ? ? C C27 0.4064(3) 0.1521(1) 0.4262(2) 0.029(1) Uani ? ? C C28 0.6620(3) 0.1268(1) 0.3369(2) 0.027(1) Uani ? ? C C29 0.5565(3) 0.1568(1) 0.2787(2) 0.035(2) Uani ? ? C C30 0.6421(3) 0.0756(1) 0.3029(2) 0.035(2) Uani ? ? C C31 0.7918(3) 0.1456(1) 0.3169(2) 0.033(1) Uani ? ? C C32 0.5847(2) 0.07392(9) 0.7422(1) 0.020(1) Uani ? ? C C33 0.6222(2) 0.0325(1) 0.7018(2) 0.023(1) Uani ? ? C C34 0.6668(2) -0.0068(1) 0.7480(2) 0.026(1) Uani ? ? C C35 0.6778(2) -0.00568(9) 0.8391(2) 0.027(1) Uani ? ? C C36 0.6412(2) 0.0325(1) 0.8808(2) 0.024(1) Uani ? ? C C37 0.5924(2) 0.07545(9) 0.8372(1) 0.019(1) Uani ? ? C C38 0.5460(2) 0.11660(9) 0.8790(1) 0.021(1) Uani ? ? C C39 0.6042(2) 0.1629(1) 0.8537(1) 0.024(1) Uani ? ? C C40 0.7364(3) 0.1647(1) 0.8509(2) 0.029(1) Uani ? ? C C41 0.7968(3) 0.2062(1) 0.8306(2) 0.037(2) Uani ? ? C C42 0.7250(3) 0.2468(1) 0.8136(2) 0.041(2) Uani ? ? C C43 0.5934(3) 0.2465(1) 0.8172(2) 0.034(2) Uani ? ? C C44 0.5341(3) 0.2051(1) 0.8381(2) 0.029(1) Uani ? ? C C45 0.5405(2) 0.1171(1) 0.9797(1) 0.025(1) Uani ? ? C C46 0.4601(3) 0.0775(1) 1.0115(2) 0.029(1) Uani ? ? C C47 0.4774(3) 0.1634(1) 1.0044(2) 0.034(1) Uani ? ? C C48 0.6772(3) 0.1147(1) 1.0341(2) 0.032(1) Uani ? ? C C49 0.9703(3) -0.0712(1) 0.8297(2) 0.053(2) Uani ? ? C C50 0.9004(4) -0.1117(2) 0.8063(2) 0.069(2) Uani ? ? C C51 0.8632(5) -0.1416(2) 0.8684(3) 0.080(3) Uani ? ? C C52 0.8946(4) -0.1303(2) 0.9551(2) 0.078(2) Uani ? ? C C53 0.9624(3) -0.0897(2) 0.9799(2) 0.067(2) Uani ? ? C C54 1.0008(3) -0.0605(1) 0.9184(3) 0.063(2) Uani ? ? C C55 1.0095(4) -0.0388(2) 0.7622(3) 0.083(3) Uani ? ? C H1 0.4928 0.2595 0.5321 0.0561 Uiso calc C8 H H2 0.2966 0.2920 0.5508 0.0754 Uiso calc C9 H H3 0.1627 0.2537 0.6344 0.0642 Uiso calc C10 H H4 0.2239 0.1819 0.7001 0.0435 Uiso calc C11 H H5 0.8400 0.1075 0.7212 0.0347 Uiso calc C16 H H6 1.0154 0.0678 0.6872 0.0433 Uiso calc C17 H H7 1.0163 0.0474 0.5403 0.0430 Uiso calc C18 H H8 0.8594 0.0739 0.4306 0.0344 Uiso calc C19 H H9 0.5382 0.0495 0.4754 0.0343 Uiso calc C23 H H10 0.3234 0.0298 0.4827 0.0449 Uiso calc C24 H H11 0.1606 0.0865 0.4541 0.0502 Uiso calc C25 H H12 0.2127 0.1641 0.4198 0.0481 Uiso calc C26 H H13 0.4262 0.1835 0.4112 0.0375 Uiso calc C27 H H14 0.5677 0.1547 0.2196 0.0500 Uiso calc C29 H H15 0.4729 0.1452 0.2837 0.0500 Uiso calc C29 H H16 0.5642 0.1889 0.2970 0.0500 Uiso calc C29 H H17 0.6525 0.0745 0.2436 0.0461 Uiso calc C30 H H18 0.7045 0.0556 0.3367 0.0461 Uiso calc C30 H H19 0.5572 0.0653 0.3076 0.0461 Uiso calc C30 H H20 0.7928 0.1424 0.2563 0.0434 Uiso calc C31 H H21 0.8010 0.1780 0.3328 0.0434 Uiso calc C31 H H22 0.8615 0.1281 0.3492 0.0434 Uiso calc C31 H H23 0.6161 0.0322 0.6402 0.0297 Uiso calc C33 H H24 0.6899 -0.0343 0.7193 0.0343 Uiso calc C34 H H25 0.7119 -0.0325 0.8723 0.0357 Uiso calc C35 H H26 0.6480 0.0310 0.9424 0.0312 Uiso calc C36 H H27 0.7870 0.1368 0.8630 0.0385 Uiso calc C40 H H28 0.8870 0.2063 0.8286 0.0496 Uiso calc C41 H H29 0.7654 0.2751 0.7993 0.0582 Uiso calc C42 H H30 0.5438 0.2746 0.8055 0.0498 Uiso calc C43 H H31 0.4445 0.2054 0.8417 0.0389 Uiso calc C44 H H32 0.4626 0.0808 1.0725 0.0385 Uiso calc C46 H H33 0.3727 0.0796 0.9818 0.0385 Uiso calc C46 H H34 0.4951 0.0477 0.9998 0.0385 Uiso calc C46 H H35 0.4747 0.1632 1.0651 0.0451 Uiso calc C47 H H36 0.5271 0.1896 0.9912 0.0451 Uiso calc C47 H H37 0.3916 0.1657 0.9722 0.0451 Uiso calc C47 H H38 0.6718 0.1150 1.0943 0.0443 Uiso calc C48 H H39 0.7185 0.0864 1.0207 0.0443 Uiso calc C48 H H40 0.7261 0.1412 1.0210 0.0443 Uiso calc C48 H H41 1.0487 -0.0327 0.9367 0.0857 Uiso calc C54 H H42 0.9832 -0.0816 1.0399 0.0901 Uiso calc C53 H H43 0.8693 -0.1505 0.9978 0.0983 Uiso calc C52 H H44 0.8162 -0.1697 0.8508 0.1056 Uiso calc C51 H H45 0.8769 -0.1195 0.7463 0.0885 Uiso calc C50 H H46 0.9809 -0.0517 0.7057 0.1111 Uiso calc C55 H H47 0.9711 -0.0086 0.7659 0.1111 Uiso calc C55 H H48 1.1014 -0.0357 0.7723 0.1111 Uiso calc C55 H loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_12 _atom_site_aniso_U_13 _atom_site_aniso_U_23 _atom_site_aniso_type_symbol MN1 0.0271(2) 0.0229(2) 0.0225(2) -0.0023(2) 0.0083(1) 0.0019(2) Mn MN2 0.0198(2) 0.0210(2) 0.0204(2) 0.0002(2) 0.0053(1) 0.0007(2) Mn C1 0.042(1) 0.035(2) 0.031(1) -0.012(1) 0.014(1) 0.002(1) C O1 0.074(1) 0.059(1) 0.043(1) -0.037(1) 0.019(1) -0.021(1) O C2 0.038(1) 0.033(2) 0.023(1) -0.005(1) 0.008(1) 0.002(1) C O2 0.032(1) 0.067(2) 0.047(1) -0.013(1) 0.0166(8) -0.004(1) O C3 0.038(1) 0.029(2) 0.035(1) -0.004(1) 0.017(1) -0.001(1) C O3 0.070(1) 0.036(1) 0.050(1) 0.006(1) 0.012(1) 0.019(1) O C4 0.023(1) 0.031(1) 0.025(1) -0.002(1) 0.003(1) -0.002(1) C O4 0.046(1) 0.034(1) 0.036(1) -0.0115(9) 0.0069(8) 0.0080(9) O C5 0.035(1) 0.027(1) 0.025(1) -0.002(1) 0.010(1) 0.001(1) C O5 0.043(1) 0.048(1) 0.051(1) 0.014(1) 0.0247(8) -0.000(1) O C6 0.018(1) 0.025(1) 0.029(1) 0.005(1) 0.0091(9) 0.007(1) C O6 0.0292(9) 0.037(1) 0.031(1) -0.0002(9) -0.0051(8) -0.0055(9) O N1 0.026(1) 0.020(1) 0.023(1) 0.0013(9) 0.0055(8) -0.0014(9) N C7 0.033(1) 0.022(1) 0.023(1) 0.005(1) 0.009(1) -0.000(1) C C8 0.059(2) 0.030(2) 0.048(2) 0.015(1) 0.029(1) 0.013(1) C C9 0.078(2) 0.041(2) 0.064(2) 0.035(2) 0.036(1) 0.025(2) C C10 0.052(2) 0.052(2) 0.051(2) 0.028(1) 0.027(1) 0.020(2) C C11 0.033(1) 0.036(2) 0.034(1) 0.010(1) 0.012(1) 0.006(1) C C12 0.031(1) 0.022(1) 0.020(1) 0.005(1) 0.005(1) 0.000(1) C N2 0.021(1) 0.023(1) 0.0182(9) -0.0010(9) 0.0018(8) -0.0008(9) N C13 0.022(1) 0.021(1) 0.015(1) -0.000(1) 0.001(1) -0.002(1) C C14 0.022(1) 0.018(1) 0.018(1) -0.002(1) 0.0022(9) -0.001(1) C C15 0.020(1) 0.020(1) 0.021(1) -0.002(1) 0.005(1) 0.002(1) C C16 0.025(1) 0.037(2) 0.019(1) -0.000(1) 0.004(1) 0.004(1) C C17 0.022(1) 0.047(2) 0.032(1) 0.007(1) 0.006(1) 0.012(1) C C18 0.024(1) 0.040(2) 0.037(1) 0.010(1) 0.012(1) 0.008(1) C C19 0.027(1) 0.030(2) 0.024(1) 0.005(1) 0.009(1) 0.004(1) C C20 0.023(1) 0.021(1) 0.021(1) -0.001(1) 0.0077(9) 0.000(1) C C21 0.025(1) 0.023(1) 0.021(1) 0.003(1) 0.006(1) 0.001(1) C C22 0.026(1) 0.028(1) 0.015(1) 0.003(1) -0.001(1) 0.000(1) C C23 0.027(1) 0.031(1) 0.021(1) -0.002(1) 0.002(1) -0.002(1) C C24 0.038(1) 0.039(2) 0.028(1) -0.011(1) 0.008(1) -0.003(1) C C25 0.025(1) 0.059(2) 0.032(1) -0.008(1) 0.007(1) 0.002(1) C C26 0.027(1) 0.052(2) 0.032(1) 0.009(1) 0.007(1) 0.004(1) C C27 0.030(1) 0.034(2) 0.024(1) 0.004(1) 0.005(1) 0.003(1) C C28 0.032(1) 0.034(2) 0.019(1) 0.002(1) 0.005(1) 0.002(1) C C29 0.042(2) 0.053(2) 0.020(1) 0.007(1) 0.005(1) 0.006(1) C C30 0.040(2) 0.039(2) 0.028(1) -0.002(1) 0.009(1) -0.005(1) C C31 0.040(1) 0.043(2) 0.020(1) -0.001(1) 0.013(1) -0.000(1) C C32 0.019(1) 0.022(1) 0.020(1) -0.001(1) 0.0072(9) 0.001(1) C C33 0.022(1) 0.026(1) 0.021(1) 0.001(1) 0.004(1) -0.000(1) C C34 0.026(1) 0.021(1) 0.034(1) 0.002(1) 0.009(1) -0.001(1) C C35 0.024(1) 0.025(1) 0.034(1) 0.004(1) 0.006(1) 0.007(1) C C36 0.023(1) 0.029(1) 0.021(1) 0.001(1) 0.006(1) 0.008(1) C C37 0.016(1) 0.023(1) 0.020(1) -0.002(1) 0.0016(9) 0.001(1) C C38 0.019(1) 0.023(1) 0.021(1) -0.002(1) 0.004(1) -0.000(1) C C39 0.032(1) 0.025(1) 0.016(1) -0.005(1) 0.005(1) -0.001(1) C C40 0.036(1) 0.033(2) 0.021(1) -0.009(1) 0.005(1) -0.006(1) C C41 0.042(2) 0.045(2) 0.028(1) -0.020(1) 0.007(1) -0.007(1) C C42 0.076(2) 0.033(2) 0.028(1) -0.026(2) 0.015(1) -0.008(1) C C43 0.069(2) 0.024(1) 0.025(1) -0.008(1) 0.013(1) -0.004(1) C C44 0.041(1) 0.026(1) 0.023(1) -0.004(1) 0.008(1) -0.003(1) C C45 0.027(1) 0.028(1) 0.020(1) -0.003(1) 0.004(1) -0.002(1) C C46 0.033(1) 0.038(2) 0.020(1) -0.004(1) 0.008(1) 0.001(1) C C47 0.047(2) 0.035(2) 0.024(1) 0.002(1) 0.014(1) -0.004(1) C C48 0.041(2) 0.040(2) 0.020(1) -0.009(1) 0.003(1) -0.003(1) C C49 0.035(2) 0.065(2) 0.064(2) 0.019(2) 0.016(1) 0.018(2) C C50 0.079(2) 0.069(3) 0.060(2) 0.004(2) 0.022(2) 0.005(2) C C51 0.114(3) 0.058(3) 0.078(2) 0.001(3) 0.033(2) 0.002(2) C C52 0.087(2) 0.078(3) 0.071(2) 0.021(2) 0.039(2) 0.023(2) C C53 0.056(2) 0.098(3) 0.055(2) 0.027(2) 0.014(2) 0.009(2) C C54 0.043(2) 0.074(3) 0.078(2) 0.013(2) 0.003(2) 0.003(2) C C55 0.052(2) 0.101(3) 0.108(3) 0.012(2) 0.025(2) 0.038(3) C # 10. MOLECULAR GEOMETRY loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_1 _geom_bond_site_symmetry_2 _geom_bond_publ_flag MN1 C1 1.826(3) . . ? MN1 C2 1.807(3) . . ? MN1 C3 1.791(3) . . ? MN1 N1 2.042(2) . . ? MN1 C15 2.283(3) . . ? MN1 C20 2.219(3) . . ? MN1 C21 2.208(3) . . ? MN2 C4 1.802(3) . . ? MN2 C5 1.792(3) . . ? MN2 C6 1.818(3) . . ? MN2 N2 2.035(2) . . ? MN2 C32 2.294(2) . . ? MN2 C37 2.200(2) . . ? MN2 C38 2.209(3) . . ? C1 O1 1.154(4) . . ? C2 O2 1.141(3) . . ? C3 O3 1.153(3) . . ? C4 O4 1.153(3) . . ? C5 O5 1.151(3) . . ? C6 O6 1.152(3) . . ? N1 C7 1.365(3) . . ? N1 C14 1.332(3) . . ? C7 C8 1.406(4) . . ? C7 C12 1.423(4) . . ? C8 C9 1.369(4) . . ? C9 C10 1.405(5) . . ? C10 C11 1.364(4) . . ? C11 C12 1.411(4) . . ? C12 N2 1.363(3) . . ? N2 C13 1.321(3) . . ? C13 C14 1.418(3) . . ? C13 C32 1.483(4) . . ? C14 C15 1.490(4) . . ? C15 C16 1.412(4) . . ? C15 C20 1.468(4) . . ? C16 C17 1.349(4) . . ? C17 C18 1.410(4) . . ? C18 C19 1.360(4) . . ? C19 C20 1.441(4) . . ? C20 C21 1.462(4) . . ? C21 C22 1.509(4) . . ? C21 C28 1.582(4) . . ? C22 C23 1.401(4) . . ? C22 C27 1.392(4) . . ? C23 C24 1.399(4) . . ? C24 C25 1.375(5) . . ? C25 C26 1.390(5) . . ? C26 C27 1.390(4) . . ? C28 C29 1.551(4) . . ? C28 C30 1.541(4) . . ? C28 C31 1.542(4) . . ? C32 C33 1.418(4) . . ? C32 C37 1.467(3) . . ? C33 C34 1.361(4) . . ? C34 C35 1.403(4) . . ? C35 C36 1.351(4) . . ? C36 C37 1.439(4) . . ? C37 C38 1.459(4) . . ? C38 C39 1.526(4) . . ? C38 C45 1.579(4) . . ? C39 C40 1.393(4) . . ? C39 C44 1.398(4) . . ? C40 C41 1.395(4) . . ? C41 C42 1.372(5) . . ? C42 C43 1.388(5) . . ? C43 C44 1.390(4) . . ? C45 C46 1.534(4) . . ? C45 C47 1.546(4) . . ? C45 C48 1.528(4) . . ? C49 C50 1.373(6) . . ? C49 C54 1.395(6) . . ? C49 C55 1.505(5) . . ? C50 C51 1.391(6) . . ? C51 C52 1.369(6) . . ? C52 C53 1.367(6) . . ? C53 C54 1.378(6) . . ? loop_ _geom_contact_atom_site_label_1 _geom_contact_atom_site_label_2 _geom_contact_distance _geom_contact_site_symmetry_1 _geom_contact_site_symmetry_2 _geom_contact_publ_flag ? ? ? ? ? ? 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_2 _geom_angle_site_symmetry_3 _geom_angle_publ_flag C1 MN1 C2 82.2(1) . . . ? C1 MN1 C3 95.4(1) . . . ? C1 MN1 N1 91.1(1) . . . ? C1 MN1 C15 100.7(1) . . . ? C1 MN1 C20 132.3(1) . . . ? C1 MN1 C21 170.1(1) . . . ? C2 MN1 C3 89.7(1) . . . ? C2 MN1 N1 165.9(1) . . . ? C2 MN1 C15 104.0(1) . . . ? C2 MN1 C20 87.0(1) . . . ? C2 MN1 C21 99.4(1) . . . ? C3 MN1 N1 103.3(1) . . . ? C3 MN1 C15 160.0(1) . . . ? C3 MN1 C20 130.9(1) . . . ? C3 MN1 C21 94.4(1) . . . ? N1 MN1 C15 64.94(9) . . . ? N1 MN1 C20 88.47(9) . . . ? N1 MN1 C21 85.16(9) . . . ? C15 MN1 C20 38.02(9) . . . ? C15 MN1 C21 69.37(9) . . . ? C20 MN1 C21 38.6(1) . . . ? C4 MN2 C5 87.6(1) . . . ? C4 MN2 C6 83.4(1) . . . ? C4 MN2 N2 169.6(1) . . . ? C4 MN2 C32 107.7(1) . . . ? C4 MN2 C37 88.2(1) . . . ? C4 MN2 C38 98.9(1) . . . ? C5 MN2 C6 97.3(1) . . . ? C5 MN2 N2 101.4(1) . . . ? C5 MN2 C32 161.2(1) . . . ? C5 MN2 C37 135.5(1) . . . ? C5 MN2 C38 98.7(1) . . . ? C6 MN2 N2 90.2(1) . . . ? C6 MN2 C32 95.4(1) . . . ? C6 MN2 C37 126.2(1) . . . ? C6 MN2 C38 164.0(1) . . . ? N2 MN2 C32 64.63(9) . . . ? N2 MN2 C37 89.02(9) . . . ? N2 MN2 C38 85.07(9) . . . ? C32 MN2 C37 38.04(9) . . . ? C32 MN2 C38 68.73(9) . . . ? C37 MN2 C38 38.64(9) . . . ? C7 N1 C14 119.2(2) . . . ? N1 C7 C8 120.5(3) . . . ? N1 C7 C12 119.8(2) . . . ? C8 C7 C12 119.7(3) . . . ? C7 C8 C9 119.1(3) . . . ? C8 C9 C10 121.6(3) . . . ? C9 C10 C11 120.4(3) . . . ? C10 C11 C12 119.9(3) . . . ? C7 C12 C11 119.3(3) . . . ? C7 C12 N2 119.0(2) . . . ? C11 C12 N2 121.7(2) . . . ? C12 N2 C13 120.5(2) . . . ? N2 C13 C14 120.1(2) . . . ? N2 C13 C32 111.9(2) . . . ? C14 C13 C32 128.0(2) . . . ? N1 C14 C13 120.7(2) . . . ? N1 C14 C15 111.3(2) . . . ? C13 C14 C15 128.0(2) . . . ? C14 C15 C16 117.9(2) . . . ? C14 C15 C20 121.2(2) . . . ? C16 C15 C20 120.4(2) . . . ? C15 C16 C17 122.7(3) . . . ? C16 C17 C18 118.3(3) . . . ? C17 C18 C19 121.6(3) . . . ? C18 C19 C20 123.1(2) . . . ? C15 C20 C19 113.7(2) . . . ? C15 C20 C21 121.5(2) . . . ? C19 C20 C21 124.7(2) . . . ? C20 C21 C22 114.8(2) . . . ? C20 C21 C28 120.4(2) . . . ? C22 C21 C28 109.7(2) . . . ? C21 C22 C23 119.2(2) . . . ? C21 C22 C27 123.6(3) . . . ? C23 C22 C27 117.1(3) . . . ? C22 C23 C24 121.2(3) . . . ? C23 C24 C25 120.2(3) . . . ? C24 C25 C26 119.8(3) . . . ? C25 C26 C27 119.7(3) . . . ? C22 C27 C26 122.0(3) . . . ? C21 C28 C29 110.5(2) . . . ? C21 C28 C30 110.6(2) . . . ? C21 C28 C31 115.6(2) . . . ? C29 C28 C30 105.9(2) . . . ? C29 C28 C31 104.7(2) . . . ? C30 C28 C31 109.0(2) . . . ? C13 C32 C33 118.2(2) . . . ? C13 C32 C37 121.3(2) . . . ? C33 C32 C37 120.1(2) . . . ? C32 C33 C34 122.4(2) . . . ? C33 C34 C35 118.4(3) . . . ? C34 C35 C36 121.6(3) . . . ? C35 C36 C37 123.7(2) . . . ? C32 C37 C36 113.7(2) . . . ? C32 C37 C38 120.7(2) . . . ? C36 C37 C38 125.5(2) . . . ? C37 C38 C39 112.9(2) . . . ? C37 C38 C45 121.6(2) . . . ? C39 C38 C45 109.6(2) . . . ? C38 C39 C40 118.9(3) . . . ? C38 C39 C44 123.8(2) . . . ? C40 C39 C44 117.2(3) . . . ? C39 C40 C41 122.0(3) . . . ? C40 C41 C42 119.6(3) . . . ? C41 C42 C43 120.1(3) . . . ? C42 C43 C44 120.1(3) . . . ? C39 C44 C43 121.1(3) . . . ? C38 C45 C46 115.7(2) . . . ? C38 C45 C47 110.3(2) . . . ? C38 C45 C48 110.7(2) . . . ? C46 C45 C47 104.7(2) . . . ? C46 C45 C48 107.6(2) . . . ? C47 C45 C48 107.4(2) . . . ? C50 C49 C54 117.4(4) . . . ? C50 C49 C55 121.5(4) . . . ? C54 C49 C55 121.1(4) . . . ? C49 C50 C51 121.6(4) . . . ? C50 C51 C52 119.8(5) . . . ? C51 C52 C53 119.7(4) . . . ? C52 C53 C54 120.5(4) . . . ? C49 C54 C53 121.0(4) . . . ? _diffrn_measured_fraction_theta_max 0.996 _diffrn_reflns_theta_full 29.13 _diffrn_measured_fraction_theta_full 0.996 data_2c _database_code_depnum_ccdc_archive 'CCDC 284342' #=============================================================================== # 5. CHEMICAL DATA _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_formula_moiety 'C45 H40 Cl2 Mn2 N2 O6' _chemical_formula_structural ? _chemical_formula_analytical ? _chemical_formula_sum 'C45 H40 Cl2 Mn2 N2 O6' _chemical_formula_weight 885.61 _chemical_melting_point ? _chemical_compound_source ? loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source C ? 0.002 0.002 International_Tables_Vol_IV_Table_2.3.1 H ? 0.000 0.000 International_Tables_Vol_IV_Table_2.3.1 Cl ? 0.132 0.159 International_Tables_Vol_IV_Table_2.3.1 Mn ? 0.295 0.729 International_Tables_Vol_IV_Table_2.3.1 N ? 0.004 0.003 International_Tables_Vol_IV_Table_2.3.1 O ? 0.008 0.006 International_Tables_Vol_IV_Table_2.3.1 #=============================================================================== # 6. CRYSTAL DATA _symmetry_cell_setting monoclinic _symmetry_space_group_name_H-M 'P 1 21/c 1' _symmetry_space_group_name_Hall '-P 2ybc' loop_ _symmetry_equiv_pos_as_xyz x,y,z -x,1/2+y,1/2-z -x,-y,-z +x,1/2-y,1/2+z _cell_length_a 18.8855(3) _cell_length_b 13.7903(4) _cell_length_c 15.9732(5) _cell_angle_alpha 90 _cell_angle_beta 101.257(5) _cell_angle_gamma 90 _cell_volume 4080.0(2) _cell_formula_units_Z 4 _cell_measurement_temperature 173 _cell_measurement_reflns_used ? _cell_measurement_theta_min ? _cell_measurement_theta_max ? _cell_special_details ; Cell parameters refined using Scalepack part of DENZO Z. Otwinowski, W. Minor, 1997 ; _exptl_crystal_description prism _exptl_crystal_colour 'dark red' _exptl_crystal_size_max 0.10 _exptl_crystal_size_mid 0.08 _exptl_crystal_size_min 0.06 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.44 _exptl_crystal_density_method none _exptl_crystal_F_000 1824 _exptl_absorpt_coefficient_mu 0.801 _exptl_absorpt_correction_type refdelf_(Walker_&_Stuart,_1983) _exptl_absorpt_correction_T_min 0.921 _exptl_absorpt_correction_T_max 0.951 #=============================================================================== # 7. EXPERIMENTAL DATA _diffrn_special_details ; ? ; _diffrn_ambient_temperature 173 _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type Mo-K\a _diffrn_source xray_tube _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type KappaCCD _diffrn_measurement_method '\p scans' _diffrn_measurement_details ; 20231 reflections were collected using program Collect ("Collect" Data collection software, Nonius B.V., 1998) The conditions were as follow : crystal to detector distance = 36. mm. Scan angle = 1.2 deg 1 scans of 200 sec per frame. Data collection was divided into 2 set(s) with the following starting angles and number of frames : Set 1 Theta = 8.81 Omega = 0.00 Kappa = 0.00 151 frames Set 2 Theta = -8.06 Kappa = -154.88 Phi = 0.00 32 frames Friedel pairs were averaged. Internal R = 0.04 ; _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% 0 _diffrn_reflns_number 20231 _diffrn_reflns_av_R_equivalents 0.040 _diffrn_reflns_av_sigmaI/netI 0.333 _diffrn_reflns_limit_h_min -22 _diffrn_reflns_limit_h_max 22 _diffrn_reflns_limit_k_min -17 _diffrn_reflns_limit_k_max 19 _diffrn_reflns_limit_l_min -26 _diffrn_reflns_limit_l_max 26 _diffrn_reflns_theta_min 2.5 _diffrn_reflns_theta_max 29.97 _reflns_number_total 12280 _reflns_number_gt 3693 _reflns_threshold_expression >3.0\s(I) _computing_structure_solution Direct_methods_(SIR,_Burla_et_al.,_1989) _computing_structure_refinement LSFM_OpenMoleN_(_1997) _computing_molecular_graphics ? _computing_publication_material CIFGEN_IN_OpenMoleN_(_1997) #=============================================================================== # 8. REFINEMENT DATA _refine_ls_structure_factor_coef F _refine_ls_matrix_type full _refine_ls_weighting_scheme sigma _refine_ls_hydrogen_treatment noref _refine_ls_extinction_method none _refine_ls_extinction_expression ? _refine_ls_extinction_coef ? _refine_ls_abs_structure_Flack ? _refine_ls_number_reflns 3693 _refine_ls_number_parameters 514 _refine_ls_number_restraints 0 _refine_ls_number_constraints 0 _refine_ls_R_factor_all 0.112 _refine_ls_R_factor_gt 0.087 _refine_ls_wR_factor_all 0.198 _refine_ls_wR_factor_ref 0.099 _refine_ls_goodness_of_fit_all 1.898 _refine_ls_goodness_of_fit_ref 1.590 _refine_ls_shift/su_max 0.000 _refine_ls_shift/esd_mean 0.010 _refine_diff_density_max 0.925 _refine_diff_density_min -0.805 #=============================================================================== # 9. ATOMIC COORDINATES AND THERMAL PARAMETERS loop_ _atom_site_label _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_calc_flag _atom_site_calc_attached_atom _atom_site_type_symbol MN1 0.52578(6) 0.3425(1) 0.66348(7) 0.0144(6) Uani ? ? Mn C1 0.5610(4) 0.2434(7) 0.7316(5) 0.025(5) Uani ? ? C O1 0.5900(3) 0.1848(5) 0.7779(4) 0.034(4) Uani ? ? O C2 0.6189(5) 0.3893(7) 0.6979(5) 0.024(5) Uani ? ? C O2 0.6760(3) 0.4133(5) 0.7228(4) 0.041(4) Uani ? ? O C3 0.4882(4) 0.3970(6) 0.7478(6) 0.017(4) Uani ? ? C O3 0.4668(3) 0.4292(5) 0.8042(4) 0.042(4) Uani ? ? O C4 0.4825(4) 0.2372(6) 0.5602(5) 0.015(4) Uani ? ? C C5 0.5054(4) 0.1372(6) 0.5654(5) 0.020(5) Uani ? ? C C6 0.5621(5) 0.1033(7) 0.5347(6) 0.026(5) Uani ? ? C C7 0.6044(4) 0.1656(7) 0.4945(5) 0.027(5) Uani ? ? C C8 0.5882(4) 0.2611(7) 0.4894(6) 0.022(5) Uani ? ? C C9 0.5287(4) 0.2998(6) 0.5209(5) 0.013(4) Uani ? ? C C10 0.4239(4) 0.2766(6) 0.5984(5) 0.013(4) Uani ? ? C C11 0.3760(4) 0.2072(6) 0.6439(5) 0.022(4) Uani ? ? C C12 0.4185(5) 0.1506(7) 0.7208(5) 0.030(5) Uani ? ? C C13 0.3341(4) 0.1358(6) 0.5804(6) 0.026(5) Uani ? ? C C14 0.3209(4) 0.2636(7) 0.6820(5) 0.032(5) Uani ? ? C C15 0.3755(4) 0.3466(6) 0.5419(5) 0.013(4) Uani ? ? C C16 0.3544(4) 0.3271(7) 0.4534(5) 0.019(5) Uani ? ? C C17 0.3079(4) 0.3900(8) 0.3998(6) 0.024(5) Uani ? ? C C18 0.2822(4) 0.4718(7) 0.4321(6) 0.023(5) Uani ? ? C C19 0.3008(4) 0.4920(6) 0.5168(6) 0.021(5) Uani ? ? C C20 0.3471(4) 0.4311(6) 0.5711(5) 0.017(4) Uani ? ? C C21 0.5120(4) 0.4044(6) 0.5050(5) 0.011(4) Uani ? ? C N1 0.5031(3) 0.4514(5) 0.5755(4) 0.013(3) Uani ? ? N C22 0.5092(4) 0.4517(6) 0.4274(5) 0.012(4) Uani ? ? C MN2 0.04698(6) 0.3461(1) 0.16352(8) 0.0143(6) Uani ? ? Mn C23 0.0967(4) 0.2576(7) 0.2356(6) 0.022(5) Uani ? ? C O4 0.1330(4) 0.2082(5) 0.2829(4) 0.041(4) Uani ? ? O C24 0.1284(4) 0.4184(6) 0.1995(5) 0.020(5) Uani ? ? C O5 0.1805(3) 0.4581(5) 0.2262(4) 0.035(4) Uani ? ? O C25 0.0002(5) 0.3781(7) 0.2467(6) 0.022(4) Uani ? ? C O6 -0.0302(3) 0.3960(5) 0.3005(4) 0.045(4) Uani ? ? O C26 0.0274(4) 0.2357(6) 0.0605(5) 0.020(5) Uani ? ? C C27 0.0670(4) 0.1466(6) 0.0705(5) 0.014(4) Uani ? ? C C28 0.1288(4) 0.1345(6) 0.0412(5) 0.022(5) Uani ? ? C C29 0.1577(4) 0.2079(7) -0.0008(6) 0.032(5) Uani ? ? C C30 0.1239(4) 0.2961(6) -0.0104(5) 0.022(5) Uani ? ? C C31 0.0610(4) 0.3138(6) 0.0216(5) 0.018(4) Uani ? ? C C32 -0.0399(4) 0.2544(6) 0.0926(5) 0.015(4) Uani ? ? C C33 -0.0763(4) 0.1702(6) 0.1363(5) 0.019(4) Uani ? ? C C34 -0.0322(5) 0.1295(7) 0.2190(6) 0.028(5) Uani ? ? C C35 -0.0995(4) 0.0866(7) 0.0719(6) 0.033(5) Uani ? ? C C36 -0.1474(5) 0.2048(7) 0.1616(6) 0.030(5) Uani ? ? C C37 -0.0979(4) 0.3085(6) 0.0308(5) 0.013(4) Uani ? ? C C38 -0.1160(4) 0.2800(6) -0.0546(5) 0.023(4) Uani ? ? C C39 -0.1739(5) 0.3227(8) -0.1102(5) 0.029(6) Uani ? ? C C40 -0.2131(4) 0.3937(8) -0.0827(6) 0.025(5) Uani ? ? C C41 -0.1965(4) 0.4244(7) -0.0022(6) 0.024(5) Uani ? ? C C42 -0.1394(4) 0.3830(6) 0.0560(5) 0.018(4) Uani ? ? C C43 0.0277(4) 0.4092(6) 0.0049(5) 0.014(4) Uani ? ? C N2 0.0105(3) 0.4496(5) 0.0758(4) 0.011(3) Uani ? ? N C44 0.0178(4) 0.4619(6) -0.0701(5) 0.012(4) Uani ? ? C C45 0.2846(7) -0.049(1) 0.2934(9) 0.13(1) Uani ? ? C CL1 0.2157(3) -0.0693(5) 0.2126(3) 0.157(4) Uani ? ? Cl CL2 0.2809(2) 0.0632(3) 0.3461(2) 0.105(3) Uani ? ? Cl H1 0.4788 0.0924 0.5923 0.0264 Uiso calc C5 H H2 0.5738 0.0363 0.5402 0.0363 Uiso calc C6 H H3 0.6435 0.1409 0.4715 0.0341 Uiso calc C7 H H4 0.6175 0.3036 0.4639 0.0303 Uiso calc C8 H H5 0.3863 0.1109 0.7445 0.0385 Uiso calc C12 H H6 0.4538 0.1110 0.7026 0.0385 Uiso calc C12 H H7 0.4417 0.1950 0.7629 0.0385 Uiso calc C12 H H8 0.3058 0.0950 0.6088 0.0368 Uiso calc C13 H H9 0.3034 0.1704 0.5363 0.0368 Uiso calc C13 H H10 0.3669 0.0974 0.5566 0.0368 Uiso calc C13 H H11 0.2932 0.2198 0.7086 0.0395 Uiso calc C14 H H12 0.3451 0.3081 0.7232 0.0395 Uiso calc C14 H H13 0.2897 0.2980 0.6380 0.0395 Uiso calc C14 H H14 0.3720 0.2707 0.4301 0.0287 Uiso calc C16 H H15 0.2941 0.3758 0.3407 0.0398 Uiso calc C17 H H16 0.2513 0.5147 0.3952 0.0361 Uiso calc C18 H H17 0.2820 0.5482 0.5391 0.0355 Uiso calc C19 H H18 0.3600 0.4472 0.6299 0.0217 Uiso calc C20 H H19 0.5155 0.4180 0.3776 0.0156 Uiso calc C22 H H20 0.0492 0.0941 0.0987 0.0238 Uiso calc C27 H H21 0.1531 0.0740 0.0497 0.0296 Uiso calc C28 H H22 0.2004 0.1972 -0.0227 0.0415 Uiso calc C29 H H23 0.1435 0.3466 -0.0394 0.0282 Uiso calc C30 H H24 -0.0588 0.0796 0.2398 0.0371 Uiso calc C34 H H25 0.0119 0.1037 0.2084 0.0371 Uiso calc C34 H H26 -0.0221 0.1798 0.2602 0.0371 Uiso calc C34 H H27 -0.1681 0.1528 0.1876 0.0429 Uiso calc C36 H H28 -0.1374 0.2573 0.2006 0.0429 Uiso calc C36 H H29 -0.1803 0.2254 0.1120 0.0429 Uiso calc C36 H H30 -0.1213 0.0364 0.0988 0.0416 Uiso calc C35 H H31 -0.1331 0.1104 0.0242 0.0416 Uiso calc C35 H H32 -0.0583 0.0617 0.0532 0.0416 Uiso calc C35 H H33 -0.1287 0.4059 0.1132 0.0231 Uiso calc C42 H H34 -0.2239 0.4752 0.0160 0.0348 Uiso calc C41 H H35 -0.2527 0.4218 -0.1209 0.0390 Uiso calc C40 H H36 -0.1859 0.3017 -0.1679 0.0427 Uiso calc C39 H H37 -0.0885 0.2309 -0.0751 0.0274 Uiso calc C38 H H38 0.0315 0.4340 -0.1189 0.0166 Uiso calc C44 H H39 0.3280 -0.0508 0.2716 0.1578 Uiso calc C45 H H40 0.2854 -0.0996 0.3340 0.1578 Uiso calc C45 H loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_12 _atom_site_aniso_U_13 _atom_site_aniso_U_23 _atom_site_aniso_type_symbol MN1 0.0161(6) 0.0144(6) 0.0129(6) 0.0001(6) 0.0017(5) 0.0018(7) Mn C1 0.032(5) 0.020(5) 0.025(5) -0.005(4) 0.012(4) -0.003(5) C O1 0.035(3) 0.035(4) 0.031(4) 0.009(3) -0.004(3) 0.013(4) O C2 0.035(5) 0.026(5) 0.016(5) -0.001(4) 0.001(4) 0.012(5) C O2 0.030(3) 0.063(5) 0.036(4) -0.016(3) -0.008(3) 0.014(4) O C3 0.020(4) 0.009(4) 0.028(5) -0.002(4) 0.004(4) 0.006(4) C O3 0.058(4) 0.041(4) 0.031(3) -0.007(3) 0.020(3) -0.014(4) O C4 0.015(4) 0.015(4) 0.015(4) 0.000(3) 0.003(3) 0.000(4) C C5 0.024(4) 0.014(5) 0.024(5) 0.000(4) 0.008(3) 0.004(4) C C6 0.030(5) 0.016(5) 0.036(6) 0.007(4) 0.003(4) -0.000(5) C C7 0.022(4) 0.024(5) 0.036(5) 0.006(4) 0.013(4) -0.005(5) C C8 0.018(4) 0.024(5) 0.027(5) -0.008(4) 0.001(4) 0.003(5) C C9 0.013(4) 0.013(4) 0.013(4) 0.000(3) 0.002(3) 0.000(4) C C10 0.013(4) 0.013(4) 0.013(4) 0.000(3) 0.003(3) 0.000(4) C C11 0.018(4) 0.022(5) 0.026(5) -0.004(4) 0.008(3) 0.017(4) C C12 0.035(5) 0.026(5) 0.031(5) -0.008(4) 0.013(4) 0.005(5) C C13 0.017(4) 0.023(5) 0.048(6) -0.009(4) 0.012(4) 0.007(5) C C14 0.031(4) 0.026(5) 0.043(5) -0.000(4) 0.028(3) 0.011(5) C C15 0.015(4) 0.017(4) 0.009(4) -0.006(4) -0.001(3) 0.000(4) C C16 0.008(4) 0.029(5) 0.031(5) -0.007(4) 0.008(3) -0.003(5) C C17 0.011(4) 0.058(7) 0.021(5) -0.000(5) -0.000(4) 0.003(5) C C18 0.010(4) 0.045(6) 0.027(5) 0.001(4) 0.000(4) 0.017(5) C C19 0.017(4) 0.013(4) 0.022(4) -0.006(3) 0.009(3) -0.000(4) C C20 0.017(4) 0.013(4) 0.022(4) -0.006(3) 0.009(3) -0.000(4) C C21 0.011(4) 0.011(4) 0.011(4) 0.000(3) 0.002(3) 0.000(4) C N1 0.010(3) 0.019(4) 0.013(3) -0.002(3) 0.003(3) -0.002(3) N C22 0.012(4) 0.012(4) 0.012(4) 0.000(3) 0.002(3) 0.000(4) C MN2 0.0176(6) 0.0121(6) 0.0138(6) 0.0011(6) 0.0003(5) 0.0007(7) Mn C23 0.021(4) 0.022(5) 0.022(5) 0.001(4) -0.002(4) -0.002(5) C O4 0.049(4) 0.037(4) 0.039(4) 0.014(4) -0.011(4) 0.011(4) O C24 0.017(4) 0.024(5) 0.020(5) 0.005(4) -0.000(4) 0.003(5) C O5 0.030(3) 0.040(4) 0.036(4) -0.008(3) -0.008(3) 0.006(4) O C25 0.031(4) 0.020(5) 0.018(4) -0.002(4) 0.001(4) -0.001(5) C O6 0.060(4) 0.045(4) 0.033(3) -0.009(3) 0.029(3) -0.011(4) O C26 0.029(5) 0.019(5) 0.015(4) 0.006(4) 0.003(4) -0.002(4) C C27 0.022(4) 0.005(4) 0.027(5) -0.002(4) 0.001(4) 0.001(4) C C28 0.020(4) 0.020(5) 0.027(5) -0.001(4) 0.003(4) -0.006(5) C C29 0.023(4) 0.031(5) 0.047(5) 0.004(4) 0.019(4) -0.013(5) C C30 0.030(4) 0.016(5) 0.021(4) 0.003(4) 0.010(4) -0.004(4) C C31 0.018(4) 0.014(4) 0.023(5) -0.005(4) 0.001(4) 0.000(4) C C32 0.022(4) 0.010(4) 0.017(4) -0.003(3) 0.009(3) -0.002(4) C C33 0.020(4) 0.015(5) 0.022(4) -0.003(3) 0.010(3) -0.003(4) C C34 0.041(5) 0.021(5) 0.025(5) -0.010(4) 0.008(4) -0.001(5) C C35 0.031(5) 0.025(5) 0.044(6) -0.006(4) 0.018(4) -0.004(5) C C36 0.052(5) 0.014(5) 0.038(5) -0.014(4) 0.022(4) -0.004(5) C C37 0.013(4) 0.013(4) 0.013(4) 0.000(3) 0.002(3) 0.000(4) C C38 0.021(4) 0.023(5) 0.024(4) -0.006(4) 0.015(3) -0.005(4) C C39 0.028(5) 0.052(7) 0.017(5) 0.005(5) -0.000(4) 0.001(5) C C40 0.014(4) 0.051(6) 0.023(5) -0.002(5) -0.002(4) 0.010(6) C C41 0.012(4) 0.032(5) 0.037(5) 0.008(4) 0.008(4) 0.009(5) C C42 0.013(4) 0.023(5) 0.022(4) -0.004(4) 0.012(3) -0.004(4) C C43 0.009(4) 0.017(4) 0.016(4) -0.010(3) -0.001(3) -0.002(4) C N2 0.011(3) 0.014(4) 0.008(3) -0.001(3) -0.001(3) 0.002(3) N C44 0.007(4) 0.019(4) 0.012(4) 0.001(3) 0.001(3) -0.009(4) C C45 0.110(9) 0.15(1) 0.117(9) 0.084(9) 0.065(7) 0.08(1) C CL1 0.184(4) 0.222(5) 0.094(3) -0.094(4) -0.019(3) 0.065(4) Cl CL2 0.126(2) 0.086(3) 0.108(2) 0.011(2) 0.061(2) 0.036(2) Cl # 10. MOLECULAR GEOMETRY loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_1 _geom_bond_site_symmetry_2 _geom_bond_publ_flag MN1 C1 1.79(1) . . ? MN1 C2 1.85(1) . . ? MN1 C3 1.80(1) . . ? MN1 C10 2.197(9) . . ? MN1 N1 2.045(8) . . ? C1 O1 1.16(1) . . ? C2 O2 1.12(1) . . ? C3 O3 1.15(1) . . ? C4 C5 1.44(1) . . ? C4 C9 1.45(1) . . ? C4 C10 1.47(1) . . ? C5 C6 1.35(1) . . ? C6 C7 1.41(1) . . ? C7 C8 1.35(1) . . ? C8 C9 1.42(1) . . ? C9 C21 1.49(1) . . ? C10 C11 1.59(1) . . ? C10 C15 1.50(1) . . ? C11 C12 1.54(1) . . ? C11 C13 1.52(1) . . ? C11 C14 1.52(1) . . ? C15 C16 1.42(1) . . ? C15 C20 1.40(1) . . ? C16 C17 1.40(1) . . ? C17 C18 1.37(1) . . ? C18 C19 1.36(1) . . ? C19 C20 1.39(1) . . ? C21 N1 1.34(1) . . ? C21 C22 1.39(1) . . ? N1 C22 1.35(1) . 3_666 ? MN2 C23 1.81(1) . . ? MN2 C24 1.83(1) . . ? MN2 C25 1.79(1) . . ? MN2 C26 2.22(1) . . ? MN2 C32 2.202(9) . . ? MN2 N2 2.024(7) . . ? C23 O4 1.14(1) . . ? C24 O5 1.13(1) . . ? C25 O6 1.15(1) . . ? C26 C27 1.43(1) . . ? C26 C31 1.45(1) . . ? C26 C32 1.48(1) . . ? C27 C28 1.35(1) . . ? C28 C29 1.39(1) . . ? C29 C30 1.37(1) . . ? C30 C31 1.40(1) . . ? C31 C43 1.46(1) . . ? C32 C33 1.58(1) . . ? C32 C37 1.52(1) . . ? C33 C34 1.52(1) . . ? C33 C35 1.55(1) . . ? C33 C36 1.55(1) . . ? C37 C38 1.40(1) . . ? C37 C42 1.40(1) . . ? C38 C39 1.40(1) . . ? C39 C40 1.35(1) . . ? C40 C41 1.33(1) . . ? C41 C42 1.40(1) . . ? C43 N2 1.36(1) . . ? C43 C44 1.38(1) . . ? N2 C44 1.33(1) . 3_565 ? C45 CL1 1.67(2) . . ? C45 CL2 1.77(2) . . ? loop_ _geom_contact_atom_site_label_1 _geom_contact_atom_site_label_2 _geom_contact_distance _geom_contact_site_symmetry_1 _geom_contact_site_symmetry_2 _geom_contact_publ_flag ? ? ? ? ? ? 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_2 _geom_angle_site_symmetry_3 _geom_angle_publ_flag C1 MN1 C2 82.4(4) . . . ? C1 MN1 C3 91.0(4) . . . ? C1 MN1 C10 99.1(4) . . . ? C1 MN1 N1 168.8(3) . . . ? C2 MN1 C3 97.0(4) . . . ? C2 MN1 C10 167.7(4) . . . ? C2 MN1 N1 90.4(4) . . . ? C3 MN1 C10 95.2(4) . . . ? C3 MN1 N1 98.4(4) . . . ? C10 MN1 N1 86.1(3) . . . ? MN1 C1 O1 173.1(9) . . . ? MN1 C2 O2 175.5(9) . . . ? MN1 C3 O3 176.7(9) . . . ? C5 C4 C9 113.2(8) . . . ? C5 C4 C10 124.8(8) . . . ? C9 C4 C10 121.6(8) . . . ? C4 C5 C6 124.2(8) . . . ? C5 C6 C7 121.0(9) . . . ? C6 C7 C8 118.7(8) . . . ? C7 C8 C9 122.0(8) . . . ? C4 C9 C8 120.8(8) . . . ? C4 C9 C21 121.6(8) . . . ? C8 C9 C21 117.4(8) . . . ? MN1 C10 C4 71.8(5) . . . ? MN1 C10 C11 123.9(6) . . . ? MN1 C10 C15 113.1(6) . . . ? C4 C10 C11 120.7(8) . . . ? C4 C10 C15 114.0(7) . . . ? C11 C10 C15 109.1(7) . . . ? C10 C11 C12 114.5(7) . . . ? C10 C11 C13 110.8(7) . . . ? C10 C11 C14 111.8(7) . . . ? C12 C11 C13 109.0(8) . . . ? C12 C11 C14 103.3(7) . . . ? C13 C11 C14 106.9(8) . . . ? C10 C15 C16 119.7(8) . . . ? C10 C15 C20 124.2(8) . . . ? C16 C15 C20 116.1(9) . . . ? C15 C16 C17 120.7(9) . . . ? C16 C17 C18 120.5(9) . . . ? C17 C18 C19 120(1) . . . ? C18 C19 C20 120.4(9) . . . ? C15 C20 C19 122.1(9) . . . ? C9 C21 N1 112.6(8) . . . ? C9 C21 C22 125.2(8) . . . ? N1 C21 C22 122.1(8) . . . ? MN1 N1 C21 100.3(6) . . . ? MN1 N1 C22 139.4(7) . . 3_666 ? C21 N1 C22 119.9(8) . . 3_666 ? C21 C22 N1 118.0(8) . . 3_666 ? C23 MN2 C24 82.4(4) . . . ? C23 MN2 C25 87.9(4) . . . ? C23 MN2 C26 90.0(4) . . . ? C23 MN2 C32 100.5(4) . . . ? C23 MN2 N2 168.5(3) . . . ? C24 MN2 C25 98.0(4) . . . ? C24 MN2 C26 128.0(4) . . . ? C24 MN2 C32 166.2(4) . . . ? C24 MN2 N2 89.1(4) . . . ? C25 MN2 C26 133.2(4) . . . ? C25 MN2 C32 95.6(4) . . . ? C25 MN2 N2 101.0(4) . . . ? C26 MN2 C32 39.2(3) . . . ? C26 MN2 N2 89.2(3) . . . ? C32 MN2 N2 86.0(3) . . . ? MN2 C23 O4 173.6(9) . . . ? MN2 C24 O5 175.0(9) . . . ? MN2 C25 O6 178.2(9) . . . ? MN2 C26 C27 119.9(7) . . . ? MN2 C26 C31 77.6(6) . . . ? MN2 C26 C32 69.8(5) . . . ? C27 C26 C31 115.0(8) . . . ? C27 C26 C32 125.1(8) . . . ? C31 C26 C32 119.7(8) . . . ? C26 C27 C28 122.5(8) . . . ? C27 C28 C29 121.8(9) . . . ? C28 C29 C30 118.9(8) . . . ? C29 C30 C31 121.6(9) . . . ? C26 C31 C30 120.0(9) . . . ? C26 C31 C43 122.6(8) . . . ? C30 C31 C43 117.0(8) . . . ? MN2 C32 C26 71.0(5) . . . ? MN2 C32 C33 122.7(6) . . . ? MN2 C32 C37 115.0(6) . . . ? C26 C32 C33 120.1(8) . . . ? C26 C32 C37 114.8(7) . . . ? C33 C32 C37 109.1(7) . . . ? C32 C33 C34 116.2(8) . . . ? C32 C33 C35 110.2(7) . . . ? C32 C33 C36 111.3(7) . . . ? C34 C33 C35 109.7(8) . . . ? C34 C33 C36 104.0(7) . . . ? C35 C33 C36 104.7(7) . . . ? C32 C37 C38 120.2(8) . . . ? C32 C37 C42 123.2(8) . . . ? C38 C37 C42 116.4(9) . . . ? C37 C38 C39 120.9(9) . . . ? C38 C39 C40 120.6(9) . . . ? C39 C40 C41 120(1) . . . ? C40 C41 C42 121.2(9) . . . ? C37 C42 C41 120.7(9) . . . ? C31 C43 N2 112.4(9) . . . ? C31 C43 C44 127.8(9) . . . ? N2 C43 C44 119.5(8) . . . ? MN2 N2 C43 100.6(6) . . . ? MN2 N2 C44 140.7(7) . . 3_565 ? C43 N2 C44 118.6(8) . . 3_565 ? C43 C44 N2 121.9(8) . . 3_565 ? CL1 C45 CL2 114.6(9) . . . ? _diffrn_measured_fraction_theta_max 0.996 _diffrn_reflns_theta_full 29.97 _diffrn_measured_fraction_theta_full 0.996 data_3c _database_code_depnum_ccdc_archive 'CCDC 284343' #=============================================================================== # 5. CHEMICAL DATA _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_formula_moiety 'C34 H24 Mn2 N2 O7' _chemical_formula_structural ? _chemical_formula_analytical ? _chemical_formula_sum 'C34 H24 Mn2 N2 O7' _chemical_formula_weight 682.46 _chemical_melting_point ? _chemical_compound_source ? loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source C ? 0.002 0.002 International_Tables_Vol_IV_Table_2.3.1 H ? 0.000 0.000 International_Tables_Vol_IV_Table_2.3.1 Mn ? 0.295 0.729 International_Tables_Vol_IV_Table_2.3.1 N ? 0.004 0.003 International_Tables_Vol_IV_Table_2.3.1 O ? 0.008 0.006 International_Tables_Vol_IV_Table_2.3.1 #=============================================================================== # 6. CRYSTAL DATA _symmetry_cell_setting monoclinic _symmetry_space_group_name_H-M 'P 1 21/c 1' _symmetry_space_group_name_Hall '-P 2ybc' loop_ _symmetry_equiv_pos_as_xyz x,y,z -x,1/2+y,1/2-z -x,-y,-z +x,1/2-y,1/2+z _cell_length_a 16.7067(3) _cell_length_b 11.9869(2) _cell_length_c 16.2192(3) _cell_angle_alpha 90 _cell_angle_beta 112.429(5) _cell_angle_gamma 90 _cell_volume 3002.38(14) _cell_formula_units_Z 4 _cell_measurement_temperature 173 _cell_measurement_reflns_used 16229 _cell_measurement_theta_min 1.4 _cell_measurement_theta_max 30.1 _cell_special_details ; Cell parameters refined using Scalepack part of DENZO Z. Otwinowski, W. Minor, 1997 ; _exptl_crystal_description prism _exptl_crystal_colour red _exptl_crystal_size_max 0.22 _exptl_crystal_size_mid 0.20 _exptl_crystal_size_min 0.18 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.51 _exptl_crystal_density_method none _exptl_crystal_F_000 1392 _exptl_absorpt_coefficient_mu 0.894 _exptl_absorpt_correction_type refdelf_(Walker_&_Stuart,_1983) _exptl_absorpt_correction_T_min 0.8840 _exptl_absorpt_correction_T_max 1.0000 #=============================================================================== # 7. EXPERIMENTAL DATA _diffrn_special_details ; ? ; _diffrn_ambient_temperature 173 _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type Mo-K\a _diffrn_source xray_tube _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type KappaCCD _diffrn_measurement_method '\p scans' _diffrn_measurement_details ; 16229 reflections were collected using program Collect ("Collect" Data collection software, Nonius B.V., 1998) The conditions were as follow : crystal to detector distance = 36. mm. Scan angle = 2.0 deg 1 scans of 40 sec per frame. Data collection was divided into 2 set(s) with the following starting angles and number of frames : Set 1 Theta = 8.80 Omega = 0.00 Kappa = 0.00 90 frames Set 2 Theta = -8.50 Kappa = -60.00 Phi = 0.00 43 frames Friedel pairs were averaged. Internal R = 0.04 ; _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% 0 _diffrn_reflns_number 16229 _diffrn_reflns_av_R_equivalents 0.040 _diffrn_reflns_av_sigmaI/netI 0.333 _diffrn_reflns_limit_h_min -22 _diffrn_reflns_limit_h_max 22 _diffrn_reflns_limit_k_min -16 _diffrn_reflns_limit_k_max 14 _diffrn_reflns_limit_l_min -23 _diffrn_reflns_limit_l_max 23 _diffrn_reflns_theta_min 2.5 _diffrn_reflns_theta_max 30.06 _reflns_number_total 9177 _reflns_number_gt 4068 _reflns_threshold_expression >3.0\s(I) _computing_structure_solution Direct_methods_(SIR,_Burla_et_al.,_1989) _computing_structure_refinement LSFM_OpenMoleN_(_1997) _computing_molecular_graphics ? _computing_publication_material CIFGEN_IN_OpenMoleN_(_1997) #=============================================================================== # 8. REFINEMENT DATA _refine_ls_structure_factor_coef F _refine_ls_matrix_type full _refine_ls_weighting_scheme sigma _refine_ls_hydrogen_treatment noref _refine_ls_extinction_method none _refine_ls_extinction_expression ? _refine_ls_extinction_coef ? _refine_ls_abs_structure_Flack ? _refine_ls_number_reflns 4068 _refine_ls_number_parameters 406 _refine_ls_number_restraints 0 _refine_ls_number_constraints 0 _refine_ls_R_factor_all 0.099 _refine_ls_R_factor_gt 0.033 _refine_ls_wR_factor_all 0.178 _refine_ls_wR_factor_ref 0.041 _refine_ls_goodness_of_fit_all 1.350 _refine_ls_goodness_of_fit_ref 1.034 _refine_ls_shift/su_max 0.002 _refine_ls_shift/esd_mean 0.000 _refine_diff_density_max 0.262 _refine_diff_density_min -0.126 #=============================================================================== # 9. ATOMIC COORDINATES AND THERMAL PARAMETERS loop_ _atom_site_label _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_calc_flag _atom_site_calc_attached_atom _atom_site_type_symbol MN1 0.64711(2) 0.19652(3) 0.15536(3) 0.0232(2) Uani ? ? Mn MN2 0.77790(2) -0.29469(3) 0.19424(3) 0.0249(2) Uani ? ? Mn C1 0.6988(1) 0.1843(2) 0.0748(2) 0.029(1) Uani ? ? C O1 0.7312(1) 0.1826(2) 0.0237(1) 0.052(1) Uani ? ? O C2 0.7483(1) 0.2488(2) 0.2435(2) 0.030(1) Uani ? ? C O2 0.8088(1) 0.2854(1) 0.2976(1) 0.039(1) Uani ? ? O C3 0.6163(1) 0.3386(2) 0.1229(2) 0.031(1) Uani ? ? C O3 0.5950(1) 0.4292(1) 0.1030(1) 0.040(1) Uani ? ? O C4 0.5401(2) 0.1463(2) 0.0778(2) 0.029(1) Uani ? ? C O4 0.4741(1) 0.1144(2) 0.0314(1) 0.041(1) Uani ? ? O C5 0.5953(1) 0.2032(2) 0.2511(2) 0.022(1) Uani ? ? C C6 0.5571(1) 0.2935(2) 0.2775(2) 0.026(1) Uani ? ? C C7 0.5255(1) 0.2831(2) 0.3447(2) 0.029(1) Uani ? ? C C8 0.5291(1) 0.1826(2) 0.3875(2) 0.029(1) Uani ? ? C C9 0.5677(1) 0.0919(2) 0.3651(2) 0.028(1) Uani ? ? C C10 0.6011(1) 0.1028(2) 0.2984(2) 0.021(1) Uani ? ? C C11 0.6438(1) 0.0109(2) 0.2725(2) 0.021(1) Uani ? ? C N1 0.6719(1) 0.0359(2) 0.2056(1) 0.021(1) Uani ? ? N C12 0.7123(1) -0.0449(2) 0.1792(2) 0.024(1) Uani ? ? C N2 0.7288(1) -0.1465(2) 0.2145(1) 0.021(1) Uani ? ? N C13 0.7025(1) -0.1719(2) 0.2811(2) 0.021(1) Uani ? ? C C14 0.6582(1) -0.0954(2) 0.3112(2) 0.024(1) Uani ? ? C C15 0.7230(1) -0.2882(2) 0.3120(2) 0.024(1) Uani ? ? C C16 0.6567(1) -0.3479(2) 0.3274(2) 0.030(1) Uani ? ? C C17 0.6702(2) -0.4525(2) 0.3622(2) 0.036(1) Uani ? ? C C18 0.7510(2) -0.5028(2) 0.3819(2) 0.034(1) Uani ? ? C C19 0.8161(1) -0.4476(2) 0.3693(2) 0.031(1) Uani ? ? C C20 0.8087(1) -0.3350(2) 0.3376(2) 0.024(1) Uani ? ? C C21 0.8793(1) -0.2702(2) 0.3282(2) 0.026(1) Uani ? ? C C22 0.8843(1) -0.1517(2) 0.3627(2) 0.024(1) Uani ? ? C C23 0.8695(2) -0.1312(2) 0.4403(2) 0.029(1) Uani ? ? C C24 0.8716(2) -0.0239(2) 0.4735(2) 0.038(2) Uani ? ? C C25 0.8882(2) 0.0655(2) 0.4291(2) 0.035(1) Uani ? ? C C26 0.9059(2) 0.0472(2) 0.3542(2) 0.031(1) Uani ? ? C C27 0.9036(1) -0.0593(2) 0.3208(2) 0.028(1) Uani ? ? C C28 0.9735(1) -0.3221(2) 0.3591(2) 0.032(1) Uani ? ? C C29 1.0096(2) -0.3419(2) 0.4607(2) 0.038(2) Uani ? ? C C30 0.9815(2) -0.4300(2) 0.3118(2) 0.046(2) Uani ? ? C C31 1.0363(2) -0.2397(2) 0.3411(2) 0.042(2) Uani ? ? C C32 0.6847(1) -0.3141(2) 0.0913(2) 0.031(1) Uani ? ? C O5 0.6311(1) -0.3302(2) 0.0214(1) 0.042(1) Uani ? ? O C33 0.8001(1) -0.4380(2) 0.1758(2) 0.032(1) Uani ? ? C O6 0.8060(1) -0.5294(1) 0.1566(1) 0.041(1) Uani ? ? O C34 0.8476(2) -0.2408(2) 0.1441(2) 0.034(1) Uani ? ? C O7 0.8928(1) -0.2026(2) 0.1122(1) 0.063(1) Uani ? ? O H1 0.5527 0.3634 0.2486 0.0357 Uiso calc C6 H H2 0.5009 0.3463 0.3616 0.0385 Uiso calc C7 H H3 0.5054 0.1758 0.4320 0.0378 Uiso calc C8 H H4 0.5715 0.0226 0.3947 0.0355 Uiso calc C9 H H5 0.7305 -0.0283 0.1318 0.0301 Uiso calc C12 H H6 0.6381 -0.1143 0.3569 0.0298 Uiso calc C14 H H7 0.6017 -0.3140 0.3131 0.0379 Uiso calc C16 H H8 0.6255 -0.4910 0.3731 0.0451 Uiso calc C17 H H9 0.7602 -0.5769 0.4044 0.0447 Uiso calc C18 H H10 0.8695 -0.4855 0.3823 0.0392 Uiso calc C19 H H11 0.8577 -0.1922 0.4713 0.0392 Uiso calc C23 H H12 0.8616 -0.0122 0.5267 0.0508 Uiso calc C24 H H13 0.8875 0.1393 0.4501 0.0492 Uiso calc C25 H H14 0.9198 0.1085 0.3250 0.0419 Uiso calc C26 H H15 0.9154 -0.0700 0.2685 0.0361 Uiso calc C27 H H16 1.0400 -0.4542 0.3349 0.0572 Uiso calc C30 H H17 0.9459 -0.4861 0.3216 0.0572 Uiso calc C30 H H18 0.9634 -0.4164 0.2496 0.0572 Uiso calc C30 H H19 1.0661 -0.3730 0.4792 0.0529 Uiso calc C29 H H20 1.0123 -0.2729 0.4905 0.0529 Uiso calc C29 H H21 0.9728 -0.3919 0.4751 0.0529 Uiso calc C29 H H22 1.0923 -0.2722 0.3601 0.0539 Uiso calc C31 H H23 1.0160 -0.2239 0.2791 0.0539 Uiso calc C31 H H24 1.0391 -0.1726 0.3732 0.0539 Uiso calc C31 H loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_12 _atom_site_aniso_U_13 _atom_site_aniso_U_23 _atom_site_aniso_type_symbol MN1 0.0285(2) 0.0181(2) 0.0243(2) 0.0026(2) 0.0113(1) 0.0026(2) Mn MN2 0.0332(2) 0.0182(2) 0.0257(2) 0.0022(2) 0.0164(1) -0.0005(2) Mn C1 0.029(1) 0.025(1) 0.033(1) 0.003(1) 0.011(1) -0.000(1) C O1 0.0507(9) 0.062(1) 0.044(1) 0.007(1) 0.0303(7) -0.000(1) O C2 0.036(1) 0.019(1) 0.037(1) 0.008(1) 0.019(1) 0.005(1) C O2 0.0398(9) 0.030(1) 0.048(1) -0.0006(9) 0.0049(9) -0.004(1) O C3 0.034(1) 0.028(1) 0.031(1) 0.002(1) 0.017(1) 0.001(1) C O3 0.056(1) 0.0233(9) 0.050(1) 0.0093(9) 0.0218(8) 0.007(1) O C4 0.042(1) 0.022(1) 0.028(1) 0.006(1) 0.017(1) 0.005(1) C O4 0.0365(9) 0.044(1) 0.042(1) -0.003(1) 0.0062(8) -0.000(1) O C5 0.021(1) 0.023(1) 0.022(1) 0.001(1) 0.0057(9) -0.002(1) C C6 0.028(1) 0.022(1) 0.028(1) 0.003(1) 0.006(1) 0.000(1) C C7 0.028(1) 0.033(1) 0.028(1) 0.007(1) 0.010(1) -0.006(1) C C8 0.031(1) 0.036(2) 0.022(1) 0.003(1) 0.0122(9) -0.002(1) C C9 0.031(1) 0.026(1) 0.026(1) 0.002(1) 0.0122(9) 0.001(1) C C10 0.021(1) 0.022(1) 0.021(1) 0.001(1) 0.0075(9) -0.002(1) C C11 0.019(1) 0.022(1) 0.020(1) -0.000(1) 0.0058(9) -0.000(1) C N1 0.0230(8) 0.018(1) 0.021(1) 0.0020(9) 0.0086(7) -0.0010(9) N C12 0.028(1) 0.023(1) 0.021(1) 0.000(1) 0.0119(9) 0.002(1) C N2 0.0280(9) 0.018(1) 0.019(1) 0.0042(9) 0.0103(7) 0.0028(9) N C13 0.019(1) 0.021(1) 0.023(1) -0.002(1) 0.0061(9) -0.000(1) C C14 0.025(1) 0.023(1) 0.024(1) -0.002(1) 0.0135(8) 0.001(1) C C15 0.028(1) 0.019(1) 0.025(1) 0.002(1) 0.0114(9) 0.003(1) C C16 0.030(1) 0.025(1) 0.036(1) 0.002(1) 0.017(1) 0.004(1) C C17 0.041(1) 0.023(1) 0.047(2) -0.003(1) 0.026(1) 0.003(1) C C18 0.050(1) 0.018(1) 0.043(2) 0.003(1) 0.027(1) 0.006(1) C C19 0.038(1) 0.023(1) 0.034(1) 0.010(1) 0.018(1) 0.009(1) C C20 0.031(1) 0.021(1) 0.022(1) 0.003(1) 0.0127(9) 0.003(1) C C21 0.029(1) 0.024(1) 0.025(1) 0.003(1) 0.0135(9) 0.001(1) C C22 0.023(1) 0.024(1) 0.023(1) 0.004(1) 0.0082(9) -0.000(1) C C23 0.033(1) 0.032(1) 0.024(1) 0.003(1) 0.009(1) 0.003(1) C C24 0.045(1) 0.045(2) 0.028(2) 0.002(1) 0.014(1) -0.011(1) C C25 0.041(1) 0.028(1) 0.039(2) -0.001(1) 0.009(1) -0.011(1) C C26 0.035(1) 0.025(1) 0.034(2) -0.002(1) 0.011(1) -0.002(1) C C27 0.029(1) 0.028(1) 0.028(1) -0.001(1) 0.013(1) -0.001(1) C C28 0.030(1) 0.028(1) 0.038(2) 0.007(1) 0.016(1) 0.001(1) C C29 0.033(1) 0.038(2) 0.045(2) 0.010(1) 0.007(1) 0.006(2) C C30 0.042(1) 0.039(2) 0.059(2) 0.014(1) 0.028(1) 0.000(2) C C31 0.030(1) 0.044(2) 0.055(2) 0.008(1) 0.021(1) 0.002(2) C C32 0.040(1) 0.025(1) 0.029(1) 0.002(1) 0.0195(9) 0.001(1) C O5 0.048(1) 0.043(1) 0.036(1) 0.000(1) 0.0130(8) -0.002(1) O C33 0.035(1) 0.026(1) 0.036(1) 0.001(1) 0.021(1) 0.002(1) C O6 0.059(1) 0.0228(9) 0.052(1) 0.0032(9) 0.0295(8) -0.0061(9) O C34 0.045(1) 0.030(1) 0.029(1) -0.004(1) 0.019(1) -0.012(1) C O7 0.078(1) 0.059(1) 0.055(1) -0.030(1) 0.0489(8) -0.020(1) O # 10. MOLECULAR GEOMETRY loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_1 _geom_bond_site_symmetry_2 _geom_bond_publ_flag MN1 C1 1.826(3) . . ? MN1 C2 1.858(3) . . ? MN1 C3 1.799(3) . . ? MN1 C4 1.851(3) . . ? MN1 C5 2.047(3) . . ? MN1 N1 2.070(2) . . ? MN2 C32 1.811(3) . . ? MN2 C33 1.806(3) . . ? MN2 C34 1.777(3) . . ? C1 O1 1.150(3) . . ? C2 O2 1.143(3) . . ? C3 O3 1.150(3) . . ? C4 O4 1.138(3) . . ? C5 C6 1.405(4) . . ? C5 C10 1.411(3) . . ? C6 C7 1.387(4) . . ? C7 C8 1.380(4) . . ? C8 C9 1.381(4) . . ? C9 C10 1.399(4) . . ? C10 C11 1.459(3) . . ? C11 N1 1.370(3) . . ? C11 C14 1.400(3) . . ? N1 C12 1.340(3) . . ? C12 N2 1.329(3) . . ? N2 C13 1.348(3) . . ? C13 C14 1.379(3) . . ? C13 C15 1.477(3) . . ? C15 C16 1.418(4) . . ? C15 C20 1.444(3) . . ? C16 C17 1.358(4) . . ? C17 C18 1.399(4) . . ? C18 C19 1.353(4) . . ? C19 C20 1.434(3) . . ? C20 C21 1.467(4) . . ? C21 C22 1.518(4) . . ? C21 C28 1.586(4) . . ? C22 C23 1.393(4) . . ? C22 C27 1.400(4) . . ? C23 C24 1.390(4) . . ? C24 C25 1.377(4) . . ? C25 C26 1.371(4) . . ? C26 C27 1.382(4) . . ? C28 C29 1.542(4) . . ? C28 C30 1.535(4) . . ? C28 C31 1.547(4) . . ? C32 O5 1.163(3) . . ? C33 O6 1.154(3) . . ? C34 O7 1.160(3) . . ? loop_ _geom_contact_atom_site_label_1 _geom_contact_atom_site_label_2 _geom_contact_distance _geom_contact_site_symmetry_1 _geom_contact_site_symmetry_2 _geom_contact_publ_flag ? ? ? ? ? ? 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_2 _geom_angle_site_symmetry_3 _geom_angle_publ_flag C1 MN1 C2 92.2(1) . . . ? C1 MN1 C3 91.6(1) . . . ? C1 MN1 C4 94.9(1) . . . ? C1 MN1 C5 176.2(1) . . . ? C1 MN1 N1 97.4(1) . . . ? C2 MN1 C3 88.9(1) . . . ? C2 MN1 C4 172.9(1) . . . ? C2 MN1 C5 85.8(1) . . . ? C2 MN1 N1 91.4(1) . . . ? C3 MN1 C4 90.8(1) . . . ? C3 MN1 C5 91.6(1) . . . ? C3 MN1 N1 171.0(1) . . . ? C4 MN1 C5 87.2(1) . . . ? C4 MN1 N1 87.8(1) . . . ? C5 MN1 N1 79.5(1) . . . ? C32 MN2 C33 83.3(1) . . . ? C32 MN2 C34 96.2(1) . . . ? C33 MN2 C34 93.3(1) . . . ? C6 C5 C10 115.8(3) . . . ? C5 C6 C7 121.7(3) . . . ? C6 C7 C8 121.0(3) . . . ? C7 C8 C9 119.4(3) . . . ? C8 C9 C10 119.6(3) . . . ? C5 C10 C9 122.4(2) . . . ? C5 C10 C11 115.2(2) . . . ? C9 C10 C11 122.4(2) . . . ? C10 C11 N1 114.6(2) . . . ? C10 C11 C14 125.2(3) . . . ? N1 C11 C14 120.1(2) . . . ? C11 N1 C12 117.4(2) . . . ? N1 C12 N2 124.9(3) . . . ? C12 N2 C13 118.4(2) . . . ? N2 C13 C14 121.1(2) . . . ? N2 C13 C15 112.4(2) . . . ? C14 C13 C15 126.5(3) . . . ? C11 C14 C13 118.0(3) . . . ? C13 C15 C16 116.1(2) . . . ? C13 C15 C20 122.7(2) . . . ? C16 C15 C20 120.6(2) . . . ? C15 C16 C17 121.5(2) . . . ? C16 C17 C18 119.0(3) . . . ? C17 C18 C19 121.0(2) . . . ? C18 C19 C20 123.4(2) . . . ? C15 C20 C19 114.1(2) . . . ? C15 C20 C21 120.9(2) . . . ? C19 C20 C21 125.0(2) . . . ? C20 C21 C22 113.0(2) . . . ? C20 C21 C28 120.0(2) . . . ? C22 C21 C28 110.0(2) . . . ? C21 C22 C23 119.7(3) . . . ? C21 C22 C27 123.5(3) . . . ? C23 C22 C27 116.8(3) . . . ? C22 C23 C24 121.8(3) . . . ? C23 C24 C25 119.9(3) . . . ? C24 C25 C26 119.5(3) . . . ? C25 C26 C27 120.8(3) . . . ? C22 C27 C26 121.1(3) . . . ? C21 C28 C29 109.5(2) . . . ? C21 C28 C30 115.9(2) . . . ? C21 C28 C31 110.7(2) . . . ? C29 C28 C30 109.4(2) . . . ? C29 C28 C31 106.4(2) . . . ? C30 C28 C31 104.4(2) . . . ? MN2 C32 O5 172.8(3) . . . ? MN2 C33 O6 172.8(3) . . . ? MN2 C34 O7 178.0(3) . . . ? _diffrn_measured_fraction_theta_max 0.996 _diffrn_reflns_theta_full 30.06 _diffrn_measured_fraction_theta_full 0.996 data_3e _database_code_depnum_ccdc_archive 'CCDC 284344' #=============================================================================== # 5. CHEMICAL DATA _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_formula_moiety 'C41 H39 Mn N2 O3' _chemical_formula_structural ? _chemical_formula_analytical ? _chemical_formula_sum 'C41 H39 Mn N2 O3' _chemical_formula_weight 662.72 _chemical_melting_point ? _chemical_compound_source ? loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source C ? 0.002 0.002 International_Tables_Vol_IV_Table_2.3.1 H ? 0.000 0.000 International_Tables_Vol_IV_Table_2.3.1 Mn ? 0.295 0.729 International_Tables_Vol_IV_Table_2.3.1 N ? 0.004 0.003 International_Tables_Vol_IV_Table_2.3.1 O ? 0.008 0.006 International_Tables_Vol_IV_Table_2.3.1 #=============================================================================== # 6. CRYSTAL DATA _symmetry_cell_setting monoclinic _symmetry_space_group_name_H-M 'P 1 21/c 1' _symmetry_space_group_name_Hall '-P 2ybc' loop_ _symmetry_equiv_pos_as_xyz x,y,z -x,1/2+y,1/2-z -x,-y,-z +x,1/2-y,1/2+z _cell_length_a 12.5455(3) _cell_length_b 16.0358(4) _cell_length_c 17.4291(5) _cell_angle_alpha 90 _cell_angle_beta 95.923(5) _cell_angle_gamma 90 _cell_volume 3487.6(2) _cell_formula_units_Z 4 _cell_measurement_temperature 173 _cell_measurement_reflns_used 9646 _cell_measurement_theta_min 1.4 _cell_measurement_theta_max 29.1 _cell_special_details ; Cell parameters refined using Scalepack part of DENZO Z. Otwinowski, W. Minor, 1997 ; _exptl_crystal_description prism _exptl_crystal_colour orange _exptl_crystal_size_max 0.12 _exptl_crystal_size_mid 0.10 _exptl_crystal_size_min 0.08 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.26 _exptl_crystal_density_method none _exptl_crystal_F_000 1392 _exptl_absorpt_coefficient_mu 0.419 _exptl_absorpt_correction_type refdelf_(Walker_&_Stuart,_1983) _exptl_absorpt_correction_T_min 0.9317 _exptl_absorpt_correction_T_max 1.0000 #=============================================================================== # 7. EXPERIMENTAL DATA _diffrn_special_details ; ? ; _diffrn_ambient_temperature 173 _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type Mo-K\a _diffrn_source xray_tube _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type KappaCCD _diffrn_measurement_method '\p scans' _diffrn_measurement_details ; 9646 reflections were collected using program Collect ("Collect" Data collection software, Nonius B.V., 1998) The conditions were as follow : crystal to detector distance = 36. mm. Scan angle = 1.8 deg 1 scans of 70 sec per frame. Data collection was divided into 2 set(s) with the following starting angles and number of frames : Set 1 Theta = 7.80 Omega = 0.00 Kappa = 0.00 101 frames Set 2 Theta = -7.50 Kappa = 127.00 Phi = 0.00 12 frames Friedel pairs were averaged. Internal R = 0.05 ; _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% 0 _diffrn_reflns_number 9646 _diffrn_reflns_av_R_equivalents 0.050 _diffrn_reflns_av_sigmaI/netI 0.333 _diffrn_reflns_limit_h_min 0 _diffrn_reflns_limit_h_max 17 _diffrn_reflns_limit_k_min 0 _diffrn_reflns_limit_k_max 21 _diffrn_reflns_limit_l_min -23 _diffrn_reflns_limit_l_max 23 _diffrn_reflns_theta_min 2.5 _diffrn_reflns_theta_max 29.09 _reflns_number_total 9646 _reflns_number_gt 5225 _reflns_threshold_expression >3.0\s(I) _computing_structure_solution Direct_methods_(SIR,_Burla_et_al.,_1989) _computing_structure_refinement LSFM_OpenMoleN_(_1997) _computing_molecular_graphics ? _computing_publication_material CIFGEN_IN_OpenMoleN_(_1997) #=============================================================================== # 8. REFINEMENT DATA _refine_ls_structure_factor_coef F _refine_ls_matrix_type full _refine_ls_weighting_scheme sigma _refine_ls_hydrogen_treatment noref _refine_ls_extinction_method none _refine_ls_extinction_expression ? _refine_ls_extinction_coef ? _refine_ls_abs_structure_Flack ? _refine_ls_number_reflns 5225 _refine_ls_number_parameters 424 _refine_ls_number_restraints 4 _refine_ls_number_constraints 0 _refine_ls_R_factor_all 0.083 _refine_ls_R_factor_gt 0.043 _refine_ls_wR_factor_all 0.170 _refine_ls_wR_factor_ref 0.064 _refine_ls_goodness_of_fit_all 1.355 _refine_ls_goodness_of_fit_ref 1.149 _refine_ls_shift/su_max 0.002 _refine_ls_shift/esd_mean 0.000 _refine_diff_density_max 0.304 _refine_diff_density_min -0.235 #=============================================================================== # 9. ATOMIC COORDINATES AND THERMAL PARAMETERS loop_ _atom_site_label _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_calc_flag _atom_site_calc_attached_atom _atom_site_type_symbol MN 0.52354(3) 0.25084(2) 0.18369(2) 0.0243(2) Uani ? ? Mn C1 0.5874(2) 0.3456(1) 0.1521(1) 0.030(1) Uani ? ? C O1 0.6250(1) 0.4047(1) 0.1300(1) 0.045(1) Uani ? ? O C2 0.4304(2) 0.2695(2) 0.1000(2) 0.036(1) Uani ? ? C O2 0.3771(2) 0.2881(1) 0.0446(1) 0.056(1) Uani ? ? O C3 0.4367(2) 0.2961(2) 0.2464(1) 0.036(1) Uani ? ? C O3 0.3808(2) 0.3236(1) 0.2888(1) 0.063(1) Uani ? ? O N1 0.6493(1) 0.2350(1) 0.2647(1) 0.0249(9) Uani ? ? N C4 0.6894(2) 0.2671(1) 0.3316(1) 0.029(1) Uani ? ? C N2 0.7875(2) 0.2527(1) 0.3664(1) 0.030(1) Uani ? ? N C5 0.8489(2) 0.1997(1) 0.3298(1) 0.026(1) Uani ? ? C C6 0.8113(2) 0.1615(1) 0.2608(1) 0.026(1) Uani ? ? C C7 0.7096(2) 0.1807(1) 0.2291(1) 0.023(1) Uani ? ? C C8 0.6538(2) 0.1546(1) 0.1538(1) 0.023(1) Uani ? ? C C9 0.7156(2) 0.1573(1) 0.0897(1) 0.029(1) Uani ? ? C C10 0.6743(2) 0.1335(2) 0.0183(1) 0.034(1) Uani ? ? C C11 0.5683(2) 0.1048(2) 0.0081(1) 0.033(1) Uani ? ? C C12 0.5072(2) 0.0986(2) 0.0683(1) 0.030(1) Uani ? ? C C13 0.5456(2) 0.1219(1) 0.1459(1) 0.023(1) Uani ? ? C C14 0.4807(2) 0.1209(1) 0.2113(1) 0.025(1) Uani ? ? C C15 0.5395(2) 0.0874(1) 0.2856(1) 0.027(1) Uani ? ? C C16 0.5275(2) 0.1222(2) 0.3583(1) 0.037(1) Uani ? ? C C17 0.5779(3) 0.0882(2) 0.4246(1) 0.049(2) Uani ? ? C C18 0.6433(3) 0.0192(2) 0.4214(2) 0.056(2) Uani ? ? C C19 0.6576(2) -0.0157(2) 0.3511(2) 0.045(2) Uani ? ? C C20 0.6055(2) 0.0180(2) 0.2840(1) 0.032(1) Uani ? ? C C21 0.3612(2) 0.0879(2) 0.2009(1) 0.031(1) Uani ? ? C C22 0.3599(2) -0.0059(2) 0.1825(1) 0.039(1) Uani ? ? C C23 0.3077(2) 0.0977(2) 0.2763(2) 0.043(1) Uani ? ? C C24 0.2846(2) 0.1337(2) 0.1404(2) 0.040(1) Uani ? ? C C25 0.9601(2) 0.1832(2) 0.3659(1) 0.028(1) Uani ? ? C C26 0.9847(2) 0.1015(2) 0.3885(1) 0.035(1) Uani ? ? C C27 1.0864(2) 0.0815(2) 0.4224(2) 0.041(1) Uani ? ? C C28 1.1632(2) 0.1424(2) 0.4317(2) 0.040(1) Uani ? ? C C29 1.1402(2) 0.2235(2) 0.4073(1) 0.035(1) Uani ? ? C C30 1.0386(2) 0.2466(1) 0.3744(1) 0.028(1) Uani ? ? C C31 1.0078(2) 0.3335(1) 0.3417(1) 0.029(1) Uani ? ? C C32 0.9967(2) 0.3295(2) 0.2535(1) 0.032(1) Uani ? ? C C33 0.9048(2) 0.3587(2) 0.2103(1) 0.037(1) Uani ? ? C C34 0.8917(2) 0.3530(2) 0.1308(2) 0.045(2) Uani ? ? C C35 0.9716(3) 0.3183(2) 0.0918(2) 0.052(2) Uani ? ? C C36 1.0634(3) 0.2896(2) 0.1336(2) 0.060(2) Uani ? ? C C37 1.0760(2) 0.2945(2) 0.2133(2) 0.047(2) Uani ? ? C C38 1.0705(2) 0.4118(2) 0.3758(1) 0.036(1) Uani ? ? C C39 1.0785(2) 0.4087(2) 0.4639(2) 0.048(2) Uani ? ? C C40 1.1827(2) 0.4237(2) 0.3494(2) 0.053(2) Uani ? ? C C41 1.0048(2) 0.4890(2) 0.3494(2) 0.046(2) Uani ? ? C H01 0.9258 0.3481 0.3532 0.0532 Uiso ? ? H H1 0.6446 0.3035 0.3570 0.0381 Uiso calc C4 H H2 0.8546 0.1233 0.2363 0.0336 Uiso calc C6 H H3 0.7876 0.1763 0.0974 0.0375 Uiso calc C9 H H4 0.7162 0.1362 -0.0240 0.0453 Uiso calc C10 H H5 0.5381 0.0892 -0.0421 0.0448 Uiso calc C11 H H6 0.4361 0.0780 0.0585 0.0396 Uiso calc C12 H H7 0.4837 0.1702 0.3615 0.0506 Uiso calc C16 H H8 0.5678 0.1123 0.4731 0.0706 Uiso calc C17 H H9 0.6781 -0.0040 0.4675 0.0772 Uiso calc C18 H H10 0.7031 -0.0627 0.3484 0.0614 Uiso calc C19 H H11 0.6152 -0.0070 0.2359 0.0419 Uiso calc C20 H H12 0.2880 -0.0254 0.1764 0.0505 Uiso calc C22 H H13 0.3920 -0.0152 0.1362 0.0505 Uiso calc C22 H H14 0.3990 -0.0352 0.2236 0.0505 Uiso calc C22 H H15 0.2362 0.0776 0.2688 0.0556 Uiso calc C23 H H16 0.3469 0.0667 0.3163 0.0556 Uiso calc C23 H H17 0.3072 0.1550 0.2904 0.0556 Uiso calc C23 H H18 0.2153 0.1095 0.1385 0.0554 Uiso calc C24 H H19 0.2807 0.1909 0.1541 0.0554 Uiso calc C24 H H20 0.3105 0.1291 0.0912 0.0554 Uiso calc C24 H H21 0.9316 0.0593 0.3806 0.0469 Uiso calc C26 H H22 1.1026 0.0261 0.4390 0.0545 Uiso calc C27 H H23 1.2329 0.1291 0.4550 0.0536 Uiso calc C28 H H24 1.1954 0.2643 0.4132 0.0463 Uiso calc C29 H H25 0.8495 0.3832 0.2362 0.0485 Uiso calc C33 H H26 0.8277 0.3729 0.1029 0.0597 Uiso calc C34 H H27 0.9632 0.3144 0.0372 0.0728 Uiso calc C35 H H28 1.1189 0.2661 0.1074 0.0829 Uiso calc C36 H H29 1.1396 0.2737 0.2410 0.0631 Uiso calc C37 H H30 1.1164 0.4562 0.4846 0.0632 Uiso calc C39 H H31 1.0085 0.4084 0.4802 0.0632 Uiso calc C39 H H32 1.1154 0.3595 0.4816 0.0632 Uiso calc C39 H H33 1.2147 0.4724 0.3727 0.0708 Uiso calc C40 H H34 1.2259 0.3766 0.3643 0.0708 Uiso calc C40 H H35 1.1769 0.4295 0.2949 0.0708 Uiso calc C40 H H36 1.0409 0.5377 0.3693 0.0604 Uiso calc C41 H H37 0.9965 0.4913 0.2946 0.0604 Uiso calc C41 H H38 0.9363 0.4859 0.3679 0.0604 Uiso calc C41 H loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_12 _atom_site_aniso_U_13 _atom_site_aniso_U_23 _atom_site_aniso_type_symbol MN 0.0251(2) 0.0218(2) 0.0261(2) 0.0038(1) -0.0018(1) -0.0016(2) Mn C1 0.035(1) 0.030(1) 0.026(1) 0.004(1) -0.001(1) -0.005(1) C O1 0.057(1) 0.034(1) 0.047(1) -0.0072(9) 0.0091(9) 0.0026(9) O C2 0.038(1) 0.026(1) 0.045(1) 0.002(1) -0.004(1) -0.000(1) C O2 0.060(1) 0.053(1) 0.056(1) 0.001(1) -0.027(1) 0.012(1) O C3 0.033(1) 0.029(1) 0.048(1) 0.005(1) 0.004(1) 0.005(1) C O3 0.066(1) 0.047(1) 0.080(1) 0.018(1) 0.0391(9) -0.001(1) O N1 0.0254(9) 0.024(1) 0.0257(9) 0.0012(8) 0.0001(8) -0.0042(8) N C4 0.028(1) 0.031(1) 0.029(1) 0.003(1) 0.002(1) -0.007(1) C N2 0.0280(9) 0.035(1) 0.026(1) 0.0026(9) -0.0022(8) -0.0059(9) N C5 0.027(1) 0.027(1) 0.023(1) 0.000(1) -0.0002(9) 0.002(1) C C6 0.027(1) 0.024(1) 0.026(1) 0.003(1) 0.0011(9) -0.003(1) C C7 0.027(1) 0.020(1) 0.023(1) 0.002(1) 0.0028(9) -0.0003(9) C C8 0.029(1) 0.019(1) 0.023(1) 0.004(1) -0.0006(9) -0.0010(9) C C9 0.029(1) 0.032(1) 0.026(1) 0.001(1) 0.003(1) -0.000(1) C C10 0.042(1) 0.040(1) 0.023(1) -0.002(1) 0.008(1) -0.002(1) C C11 0.046(1) 0.034(1) 0.022(1) -0.003(1) 0.000(1) -0.004(1) C C12 0.033(1) 0.031(1) 0.027(1) -0.001(1) -0.002(1) -0.003(1) C C13 0.030(1) 0.018(1) 0.022(1) 0.002(1) 0.0004(9) -0.0010(9) C C14 0.030(1) 0.022(1) 0.025(1) 0.002(1) 0.001(1) -0.003(1) C C15 0.031(1) 0.026(1) 0.025(1) -0.002(1) 0.003(1) 0.003(1) C C16 0.053(1) 0.038(1) 0.026(1) 0.005(1) 0.005(1) 0.001(1) C C17 0.078(2) 0.058(2) 0.026(1) -0.004(2) 0.001(1) 0.007(1) C C18 0.075(2) 0.056(2) 0.042(2) -0.005(2) -0.018(2) 0.021(1) C C19 0.050(2) 0.035(1) 0.054(2) 0.004(1) -0.009(1) 0.015(1) C C20 0.033(1) 0.026(1) 0.037(1) 0.000(1) 0.002(1) 0.004(1) C C21 0.027(1) 0.032(1) 0.034(1) -0.005(1) 0.005(1) -0.003(1) C C22 0.040(1) 0.037(1) 0.040(1) -0.010(1) 0.009(1) -0.004(1) C C23 0.035(1) 0.046(2) 0.050(1) -0.004(1) 0.016(1) -0.005(1) C C24 0.025(1) 0.046(2) 0.056(2) -0.004(1) -0.004(1) 0.000(1) C C25 0.029(1) 0.035(1) 0.020(1) 0.004(1) -0.0010(9) -0.004(1) C C26 0.040(1) 0.028(1) 0.038(1) 0.003(1) -0.007(1) -0.002(1) C C27 0.046(1) 0.036(1) 0.040(1) 0.013(1) -0.010(1) -0.000(1) C C28 0.037(1) 0.047(2) 0.037(1) 0.014(1) -0.009(1) -0.006(1) C C29 0.027(1) 0.042(1) 0.037(1) 0.001(1) -0.003(1) -0.006(1) C C30 0.026(1) 0.034(1) 0.024(1) 0.006(1) 0.0008(9) -0.005(1) C C31 0.025(1) 0.031(1) 0.032(1) 0.003(1) 0.004(1) -0.002(1) C C32 0.033(1) 0.030(1) 0.034(1) 0.002(1) 0.004(1) 0.003(1) C C33 0.034(1) 0.039(1) 0.039(1) 0.003(1) 0.005(1) 0.006(1) C C34 0.047(2) 0.048(2) 0.041(1) 0.003(1) -0.002(1) 0.015(1) C C35 0.072(2) 0.065(2) 0.030(1) 0.012(2) 0.001(1) 0.009(1) C C36 0.072(2) 0.086(2) 0.034(1) 0.037(2) 0.013(1) 0.005(2) C C37 0.047(1) 0.061(2) 0.037(1) 0.024(1) 0.002(1) 0.004(1) C C38 0.032(1) 0.035(1) 0.041(1) 0.004(1) 0.008(1) -0.007(1) C C39 0.049(2) 0.048(2) 0.048(2) 0.006(1) -0.001(1) -0.017(1) C C40 0.038(1) 0.047(2) 0.080(2) -0.009(1) 0.018(1) -0.013(2) C C41 0.050(2) 0.037(1) 0.053(2) -0.001(1) 0.009(1) -0.004(1) C # 10. MOLECULAR GEOMETRY loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_1 _geom_bond_site_symmetry_2 _geom_bond_publ_flag MN C1 1.829(3) . . ? MN C2 1.798(3) . . ? MN C3 1.777(3) . . ? MN N1 2.021(2) . . ? MN C13 2.196(2) . . ? MN C14 2.217(2) . . ? C1 O1 1.143(3) . . ? C2 O2 1.156(3) . . ? C3 O3 1.157(3) . . ? N1 C4 1.326(3) . . ? N1 C7 1.346(3) . . ? C4 N2 1.334(3) . . ? N2 C5 1.350(3) . . ? C5 C6 1.388(3) . . ? C5 C25 1.494(3) . . ? C6 C7 1.371(3) . . ? C7 C8 1.483(3) . . ? C8 C9 1.424(3) . . ? C8 C13 1.447(3) . . ? C9 C10 1.353(3) . . ? C10 C11 1.401(4) . . ? C11 C12 1.366(3) . . ? C12 C13 1.437(3) . . ? C13 C14 1.468(3) . . ? C14 C15 1.522(3) . . ? C14 C21 1.582(3) . . ? C15 C16 1.406(3) . . ? C15 C20 1.389(4) . . ? C16 C17 1.371(4) . . ? C17 C18 1.382(5) . . ? C18 C19 1.376(5) . . ? C19 C20 1.388(4) . . ? C21 C22 1.539(4) . . ? C21 C23 1.545(4) . . ? C21 C24 1.538(4) . . ? C25 C26 1.394(4) . . ? C25 C30 1.412(3) . . ? C26 C27 1.387(4) . . ? C27 C28 1.370(4) . . ? C28 C29 1.388(4) . . ? C29 C30 1.394(3) . . ? C30 C31 1.540(3) . . ? C31 C32 1.530(4) . . ? C31 C38 1.565(4) . . ? C32 C33 1.392(4) . . ? C32 C37 1.392(4) . . ? C33 C34 1.381(4) . . ? C34 C35 1.385(4) . . ? C35 C36 1.377(4) . . ? C36 C37 1.383(4) . . ? C38 C39 1.529(4) . . ? C38 C40 1.538(4) . . ? C38 C41 1.530(4) . . ? loop_ _geom_contact_atom_site_label_1 _geom_contact_atom_site_label_2 _geom_contact_distance _geom_contact_site_symmetry_1 _geom_contact_site_symmetry_2 _geom_contact_publ_flag ? ? ? ? ? ? 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_2 _geom_angle_site_symmetry_3 _geom_angle_publ_flag C1 MN C2 83.4(1) . . . ? C1 MN C3 99.3(1) . . . ? C1 MN N1 88.9(1) . . . ? C1 MN C13 128.2(1) . . . ? C1 MN C14 165.8(1) . . . ? C2 MN C3 92.4(1) . . . ? C2 MN N1 169.4(1) . . . ? C2 MN C13 90.3(1) . . . ? C2 MN C14 100.4(1) . . . ? C3 MN N1 96.1(1) . . . ? C3 MN C13 132.4(1) . . . ? C3 MN C14 94.2(1) . . . ? N1 MN C13 88.72(8) . . . ? N1 MN C14 85.40(8) . . . ? C13 MN C14 38.85(8) . . . ? MN C1 O1 177.7(2) . . . ? MN C2 O2 173.1(3) . . . ? MN C3 O3 177.9(2) . . . ? MN N1 C4 139.8(2) . . . ? MN N1 C7 101.3(1) . . . ? C4 N1 C7 118.4(2) . . . ? N1 C4 N2 125.5(2) . . . ? C4 N2 C5 116.0(2) . . . ? N2 C5 C6 121.8(2) . . . ? N2 C5 C25 117.8(2) . . . ? C6 C5 C25 120.4(2) . . . ? C5 C6 C7 118.0(2) . . . ? N1 C7 C6 120.2(2) . . . ? N1 C7 C8 110.7(2) . . . ? C6 C7 C8 128.9(2) . . . ? C7 C8 C9 116.1(2) . . . ? C7 C8 C13 122.6(2) . . . ? C9 C8 C13 121.1(2) . . . ? C8 C9 C10 121.7(2) . . . ? C9 C10 C11 118.6(2) . . . ? C10 C11 C12 121.7(2) . . . ? C11 C12 C13 123.0(2) . . . ? MN C13 C8 77.1(1) . . . ? MN C13 C12 119.1(2) . . . ? MN C13 C14 71.4(1) . . . ? C8 C13 C12 113.8(2) . . . ? C8 C13 C14 121.3(2) . . . ? C12 C13 C14 124.6(2) . . . ? MN C14 C13 69.8(1) . . . ? MN C14 C15 114.1(2) . . . ? MN C14 C21 122.5(2) . . . ? C13 C14 C15 113.9(2) . . . ? C13 C14 C21 120.7(2) . . . ? C15 C14 C21 110.5(2) . . . ? C14 C15 C16 122.7(2) . . . ? C14 C15 C20 120.2(2) . . . ? C16 C15 C20 117.1(2) . . . ? C15 C16 C17 121.2(3) . . . ? C16 C17 C18 120.5(3) . . . ? C17 C18 C19 119.6(3) . . . ? C18 C19 C20 119.8(3) . . . ? C15 C20 C19 121.7(3) . . . ? C14 C21 C22 109.9(2) . . . ? C14 C21 C23 111.0(2) . . . ? C14 C21 C24 115.9(2) . . . ? C22 C21 C23 106.3(2) . . . ? C22 C21 C24 109.4(2) . . . ? C23 C21 C24 103.9(2) . . . ? C5 C25 C26 117.1(2) . . . ? C5 C25 C30 121.9(2) . . . ? C26 C25 C30 121.0(2) . . . ? C25 C26 C27 120.3(2) . . . ? C26 C27 C28 119.4(3) . . . ? C27 C28 C29 120.7(2) . . . ? C28 C29 C30 121.8(2) . . . ? C25 C30 C29 116.7(2) . . . ? C25 C30 C31 117.9(2) . . . ? C29 C30 C31 125.2(2) . . . ? C30 C31 C32 109.1(2) . . . ? C30 C31 C38 119.2(2) . . . ? C32 C31 C38 113.9(2) . . . ? C31 C32 C33 120.9(2) . . . ? C31 C32 C37 121.8(2) . . . ? C33 C32 C37 117.3(2) . . . ? C32 C33 C34 121.8(3) . . . ? C33 C34 C35 120.1(3) . . . ? C34 C35 C36 118.9(3) . . . ? C35 C36 C37 121.0(3) . . . ? C32 C37 C36 121.0(3) . . . ? C31 C38 C39 109.5(2) . . . ? C31 C38 C40 115.1(2) . . . ? C31 C38 C41 107.5(2) . . . ? C39 C38 C40 109.7(2) . . . ? C39 C38 C41 107.8(2) . . . ? C40 C38 C41 106.9(2) . . . ? _diffrn_measured_fraction_theta_max 0.996 _diffrn_reflns_theta_full 29.09 _diffrn_measured_fraction_theta_full 0.996 data_4e _database_code_depnum_ccdc_archive 'CCDC 284345' #=============================================================================== # 5. CHEMICAL DATA _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_formula_moiety 'C38 H34 Mn2 N2 O6' _chemical_formula_structural ? _chemical_formula_analytical ? _chemical_formula_sum 'C38 H34 Mn2 N2 O6' _chemical_formula_weight 724.58 _chemical_melting_point ? _chemical_compound_source ? loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source C ? 0.002 0.002 International_Tables_Vol_IV_Table_2.3.1 H ? 0.000 0.000 International_Tables_Vol_IV_Table_2.3.1 Mn ? 0.295 0.729 International_Tables_Vol_IV_Table_2.3.1 N ? 0.004 0.003 International_Tables_Vol_IV_Table_2.3.1 O ? 0.008 0.006 International_Tables_Vol_IV_Table_2.3.1 #=============================================================================== # 6. CRYSTAL DATA _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 9.5308(2) _cell_length_b 12.9309(3) _cell_length_c 15.1767(6) _cell_angle_alpha 70.543(5) _cell_angle_beta 80.913(5) _cell_angle_gamma 69.573(5) _cell_volume 1650.86(8) _cell_formula_units_Z 2 _cell_measurement_temperature 173 _cell_measurement_reflns_used ? _cell_measurement_theta_min ? _cell_measurement_theta_max ? _cell_special_details ; Cell parameters refined using Scalepack part of DENZO Z. Otwinowski, W. Minor, 1997 ; _exptl_crystal_description prism _exptl_crystal_colour orange _exptl_crystal_size_max 0.12 _exptl_crystal_size_mid 0.10 _exptl_crystal_size_min 0.06 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.46 _exptl_crystal_density_method none _exptl_crystal_F_000 748 _exptl_absorpt_coefficient_mu 0.816 _exptl_absorpt_correction_type refdelf_(Walker_&_Stuart,_1983) _exptl_absorpt_correction_T_min 0.9445 _exptl_absorpt_correction_T_max 1.0000 #=============================================================================== # 7. EXPERIMENTAL DATA _diffrn_special_details ; ? ; _diffrn_ambient_temperature 173 _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type Mo-K\a _diffrn_source xray_tube _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type KappaCCD _diffrn_measurement_method '\p scans' _diffrn_measurement_details ; 12849 reflections were collected using program Collect ("Collect" Data collection software, Nonius B.V., 1998) The conditions were as follow : crystal to detector distance = 36. mm. Scan angle = 1.0 deg 1 scans of 40 sec per frame. Data collection was divided into 2 set(s) with the following starting angles and number of frames : Set 1 Theta = 8.80 Omega = 0.00 Kappa = 0.00 91 frames Set 2 Theta = -8.80 Kappa = 134.00 Phi = 0.00 25 frames Friedel pairs were averaged. Internal R = 0.03 ; _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% 0 _diffrn_reflns_number 12849 _diffrn_reflns_av_R_equivalents 0.030 _diffrn_reflns_av_sigmaI/netI 0.333 _diffrn_reflns_limit_h_min -13 _diffrn_reflns_limit_h_max 13 _diffrn_reflns_limit_k_min -18 _diffrn_reflns_limit_k_max 12 _diffrn_reflns_limit_l_min -21 _diffrn_reflns_limit_l_max 19 _diffrn_reflns_theta_min 2.5 _diffrn_reflns_theta_max 30.02 _reflns_number_total 9474 _reflns_number_gt 5753 _reflns_threshold_expression >3.0\s(I) _computing_structure_solution Direct_methods_(SIR,_Burla_et_al.,_1989) _computing_structure_refinement LSFM_OpenMoleN_(_1997) _computing_molecular_graphics ? _computing_publication_material CIFGEN_IN_OpenMoleN_(_1997) #=============================================================================== # 8. REFINEMENT DATA _refine_ls_structure_factor_coef F _refine_ls_matrix_type full _refine_ls_weighting_scheme sigma _refine_ls_hydrogen_treatment noref _refine_ls_extinction_method none _refine_ls_extinction_expression ? _refine_ls_extinction_coef ? _refine_ls_abs_structure_Flack ? _refine_ls_number_reflns 5753 _refine_ls_number_parameters 433 _refine_ls_number_restraints 0 _refine_ls_number_constraints 0 _refine_ls_R_factor_all 0.082 _refine_ls_R_factor_gt 0.038 _refine_ls_wR_factor_all 0.108 _refine_ls_wR_factor_ref 0.055 _refine_ls_goodness_of_fit_all 1.080 _refine_ls_goodness_of_fit_ref 1.011 _refine_ls_shift/su_max 0.003 _refine_ls_shift/esd_mean 0.001 _refine_diff_density_max 0.502 _refine_diff_density_min -0.412 #=============================================================================== # 9. ATOMIC COORDINATES AND THERMAL PARAMETERS loop_ _atom_site_label _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_calc_flag _atom_site_calc_attached_atom _atom_site_type_symbol MN1 0.03285(3) 0.03919(3) 0.75858(2) 0.0207(1) Uani ? ? Mn MN2 -0.17655(4) 0.48099(3) 0.84643(2) 0.0246(1) Uani ? ? Mn C1 0.0045(2) -0.0963(2) 0.8202(2) 0.027(1) Uani ? ? C O1 -0.0127(2) -0.1857(1) 0.8552(1) 0.0395(8) Uani ? ? O C2 -0.0935(2) 0.0642(2) 0.6713(2) 0.029(1) Uani ? ? C O2 -0.1850(2) 0.0851(2) 0.6214(1) 0.0426(9) Uani ? ? O C3 -0.1315(2) 0.1308(2) 0.8069(2) 0.028(1) Uani ? ? C O3 -0.2401(2) 0.1838(2) 0.8373(1) 0.041(1) Uani ? ? O C4 -0.1812(3) 0.5310(2) 0.9452(2) 0.031(1) Uani ? ? C O4 -0.1829(2) 0.5594(2) 1.0094(1) 0.048(1) Uani ? ? O C5 -0.0813(3) 0.3337(2) 0.9090(2) 0.035(1) Uani ? ? C O5 -0.0238(3) 0.2378(2) 0.9476(2) 0.050(1) Uani ? ? O C6 -0.3605(3) 0.4682(2) 0.8847(2) 0.036(1) Uani ? ? C O6 -0.4781(2) 0.4624(2) 0.9093(2) 0.061(1) Uani ? ? O C7 0.2501(2) -0.0515(2) 0.6981(1) 0.0203(8) Uani ? ? C C8 0.2057(2) 0.0726(2) 0.6473(1) 0.0197(8) Uani ? ? C C9 0.1625(2) 0.1198(2) 0.5516(2) 0.0251(9) Uani ? ? C C10 0.1171(3) 0.2350(2) 0.5067(2) 0.027(1) Uani ? ? C C11 0.1158(3) 0.3154(2) 0.5503(2) 0.025(1) Uani ? ? C C12 0.1567(2) 0.2800(2) 0.6410(2) 0.0220(9) Uani ? ? C C13 0.1916(2) 0.1588(2) 0.6932(1) 0.0192(8) Uani ? ? C C14 0.2303(2) 0.1215(2) 0.7928(1) 0.0209(9) Uani ? ? C N1 0.1610(2) 0.0467(1) 0.8482(1) 0.0204(8) Uani ? ? N C15 0.1885(3) 0.0035(2) 0.9392(2) 0.025(1) Uani ? ? C C16 0.2821(3) 0.0381(2) 0.9755(2) 0.029(1) Uani ? ? C C17 0.3446(3) 0.1173(2) 0.9139(2) 0.036(1) Uani ? ? C N2 0.3209(2) 0.1597(2) 0.8221(1) 0.0287(8) Uani ? ? N C18 0.3819(2) -0.0942(2) 0.7601(1) 0.0205(8) Uani ? ? C C19 0.5052(2) -0.0551(2) 0.7273(2) 0.0253(9) Uani ? ? C C20 0.6298(2) -0.0956(2) 0.7806(2) 0.031(1) Uani ? ? C C21 0.6351(2) -0.1768(2) 0.8673(2) 0.031(1) Uani ? ? C C22 0.5153(2) -0.2177(2) 0.9008(2) 0.026(1) Uani ? ? C C23 0.3898(2) -0.1764(2) 0.8483(2) 0.0229(9) Uani ? ? C C24 0.2661(2) -0.1428(2) 0.6462(2) 0.0269(9) Uani ? ? C C25 0.1235(3) -0.1326(2) 0.6045(2) 0.036(1) Uani ? ? C C26 0.3135(3) -0.2678(2) 0.7131(2) 0.036(1) Uani ? ? C C27 0.3928(3) -0.1388(2) 0.5690(2) 0.037(1) Uani ? ? C C28 0.1690(2) 0.3686(2) 0.6805(2) 0.0229(9) Uani ? ? C C29 0.0426(2) 0.4347(2) 0.7147(2) 0.0229(9) Uani ? ? C C30 -0.1082(2) 0.4263(2) 0.7155(2) 0.028(1) Uani ? ? C C31 -0.2343(2) 0.5245(2) 0.7048(2) 0.026(1) Uani ? ? C C32 -0.2313(3) 0.6238(2) 0.7239(2) 0.028(1) Uani ? ? C C33 -0.0962(3) 0.6176(2) 0.7557(2) 0.028(1) Uani ? ? C C34 0.0278(2) 0.5192(2) 0.7638(2) 0.030(1) Uani ? ? C C35 0.3215(2) 0.3938(2) 0.6610(2) 0.030(1) Uani ? ? C C36 0.4427(3) 0.3037(2) 0.6217(2) 0.043(1) Uani ? ? C C37 0.3851(3) 0.3987(2) 0.7464(2) 0.037(1) Uani ? ? C C38 0.2940(3) 0.5121(2) 0.5845(2) 0.042(1) Uani ? ? C H1 0.1660 0.0681 0.5186 0.0322 Uiso calc C9 H H2 0.0856 0.2618 0.4444 0.0373 Uiso calc C10 H H3 0.0862 0.3955 0.5166 0.0365 Uiso calc C11 H H4 0.1432 -0.0514 0.9791 0.0353 Uiso calc C15 H H5 0.3025 0.0086 1.0400 0.0400 Uiso calc C16 H H6 0.4081 0.1434 0.9377 0.0447 Uiso calc C17 H H7 0.5038 0.0001 0.6674 0.0332 Uiso calc C19 H H8 0.7120 -0.0671 0.7571 0.0403 Uiso calc C20 H H9 0.7205 -0.2043 0.9037 0.0409 Uiso calc C21 H H10 0.5187 -0.2745 0.9601 0.0355 Uiso calc C22 H H11 0.3075 -0.2045 0.8727 0.0298 Uiso calc C23 H H12 0.1453 -0.1912 0.5750 0.0439 Uiso calc C25 H H13 0.0483 -0.1417 0.6529 0.0439 Uiso calc C25 H H14 0.0887 -0.0587 0.5596 0.0439 Uiso calc C25 H H15 0.3222 -0.3204 0.6799 0.0471 Uiso calc C26 H H16 0.4074 -0.2844 0.7377 0.0471 Uiso calc C26 H H17 0.2402 -0.2752 0.7630 0.0471 Uiso calc C26 H H18 0.4022 -0.1937 0.5379 0.0461 Uiso calc C27 H H19 0.3695 -0.0635 0.5253 0.0461 Uiso calc C27 H H20 0.4846 -0.1566 0.5965 0.0461 Uiso calc C27 H H21 -0.1194 0.3536 0.7234 0.0346 Uiso calc C30 H H22 -0.3238 0.5249 0.6844 0.0364 Uiso calc C31 H H23 -0.3164 0.6915 0.7158 0.0400 Uiso calc C32 H H24 -0.0902 0.6810 0.7717 0.0379 Uiso calc C33 H H25 0.1058 0.5058 0.8022 0.0372 Uiso calc C34 H H26 0.5339 0.3213 0.6105 0.0552 Uiso calc C36 H H27 0.4573 0.2290 0.6655 0.0552 Uiso calc C36 H H28 0.4118 0.3050 0.5646 0.0552 Uiso calc C36 H H29 0.4775 0.4144 0.7283 0.0481 Uiso calc C37 H H30 0.3159 0.4582 0.7695 0.0481 Uiso calc C37 H H31 0.4012 0.3265 0.7940 0.0481 Uiso calc C37 H H32 0.3841 0.5314 0.5701 0.0544 Uiso calc C38 H H33 0.2624 0.5078 0.5298 0.0544 Uiso calc C38 H H34 0.2184 0.5698 0.6065 0.0544 Uiso calc C38 H loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_12 _atom_site_aniso_U_13 _atom_site_aniso_U_23 _atom_site_aniso_type_symbol MN1 0.0202(1) 0.0251(1) 0.0176(1) -0.0071(1) -0.0026(1) -0.0037(1) Mn MN2 0.0286(2) 0.0230(1) 0.0228(2) -0.0040(1) -0.0001(1) -0.0076(1) Mn C1 0.0237(9) 0.035(1) 0.022(1) -0.0097(7) -0.0027(8) -0.0073(8) C O1 0.0403(7) 0.0389(8) 0.0394(9) -0.0228(5) -0.0064(7) -0.0013(7) O C2 0.0245(9) 0.041(1) 0.024(1) -0.0117(8) -0.0007(8) -0.0044(9) C O2 0.0332(8) 0.073(1) 0.0319(9) -0.0159(7) -0.0125(6) -0.0069(8) O C3 0.028(1) 0.030(1) 0.026(1) -0.0084(8) -0.0025(9) -0.0011(9) C O3 0.0339(9) 0.045(1) 0.047(1) -0.0013(8) 0.0072(8) -0.0106(9) O C4 0.027(1) 0.033(1) 0.034(1) -0.0004(9) -0.0025(9) -0.0131(9) C O4 0.048(1) 0.057(1) 0.0396(9) -0.0015(8) -0.0080(8) -0.0280(7) O C5 0.055(1) 0.035(1) 0.022(1) -0.003(1) -0.001(1) -0.010(1) C O5 0.097(2) 0.033(1) 0.038(1) 0.014(1) -0.011(1) -0.0049(9) O C6 0.045(1) 0.041(1) 0.025(1) -0.0181(8) 0.0013(9) -0.0109(9) C O6 0.0504(9) 0.090(1) 0.049(1) -0.0410(7) 0.0144(8) -0.0253(9) O C7 0.0221(8) 0.0193(8) 0.0195(9) -0.0070(6) -0.0014(7) -0.0074(7) C C8 0.0188(8) 0.0228(8) 0.0179(9) -0.0073(6) 0.0012(7) -0.0074(7) C C9 0.033(1) 0.0262(9) 0.0183(9) -0.0111(7) -0.0003(8) -0.0096(7) C C10 0.037(1) 0.031(1) 0.017(1) -0.0108(8) -0.0047(8) -0.0042(8) C C11 0.035(1) 0.0184(9) 0.025(1) -0.0046(8) -0.0028(9) -0.0026(8) C C12 0.0227(9) 0.0218(8) 0.0216(9) -0.0058(6) 0.0022(7) -0.0091(7) C C13 0.0191(8) 0.0186(8) 0.0198(9) -0.0047(6) 0.0005(7) -0.0063(7) C C14 0.0236(9) 0.0191(8) 0.0203(9) -0.0024(6) -0.0024(7) -0.0098(7) C N1 0.0227(8) 0.0209(7) 0.0179(8) -0.0033(6) -0.0011(6) -0.0060(6) N C15 0.031(1) 0.025(1) 0.020(1) -0.0028(8) -0.0009(8) -0.0071(8) C C16 0.041(1) 0.029(1) 0.020(1) -0.0034(8) -0.0093(8) -0.0092(8) C C17 0.040(1) 0.035(1) 0.032(1) -0.0088(8) -0.0134(8) -0.0142(8) C N2 0.0342(8) 0.0263(7) 0.0264(9) -0.0091(6) -0.0066(7) -0.0108(6) N C18 0.0217(8) 0.0164(7) 0.0243(9) -0.0045(6) -0.0011(7) -0.0100(7) C C19 0.0250(9) 0.0221(8) 0.029(1) -0.0072(7) 0.0007(8) -0.0087(8) C C20 0.0220(9) 0.0309(9) 0.043(1) -0.0084(7) -0.0018(9) -0.0150(9) C C21 0.026(1) 0.032(1) 0.037(1) -0.0038(7) -0.0102(8) -0.0135(8) C C22 0.029(1) 0.0219(9) 0.027(1) -0.0018(7) -0.0079(8) -0.0070(8) C C23 0.0259(9) 0.0194(8) 0.024(1) -0.0075(6) -0.0031(7) -0.0057(7) C C24 0.032(1) 0.0229(8) 0.026(1) -0.0077(7) -0.0056(8) -0.0103(7) C C25 0.046(1) 0.0322(9) 0.032(1) -0.0165(7) -0.0092(9) -0.0124(8) C C26 0.049(1) 0.0233(9) 0.042(1) -0.0092(7) -0.0135(9) -0.0148(8) C C27 0.041(1) 0.036(1) 0.034(1) -0.0067(8) 0.0003(9) -0.0234(8) C C28 0.0276(9) 0.0202(8) 0.022(1) -0.0074(6) 0.0014(8) -0.0089(7) C C29 0.0259(9) 0.0198(8) 0.023(1) -0.0059(7) -0.0010(8) -0.0061(7) C C30 0.031(1) 0.0272(9) 0.025(1) -0.0124(7) 0.0015(8) -0.0102(8) C C31 0.026(1) 0.033(1) 0.021(1) -0.0083(8) -0.0009(8) -0.0050(9) C C32 0.031(1) 0.022(1) 0.031(1) -0.0008(8) -0.0006(9) -0.0059(9) C C33 0.036(1) 0.0203(9) 0.031(1) -0.0085(7) 0.0044(9) -0.0108(8) C C34 0.028(1) 0.0290(9) 0.032(1) -0.0075(7) -0.0004(8) -0.0154(8) C C35 0.028(1) 0.0262(9) 0.036(1) -0.0106(7) 0.0054(9) -0.0140(8) C C36 0.033(1) 0.040(1) 0.061(2) -0.0153(8) 0.016(1) -0.029(1) C C37 0.031(1) 0.031(1) 0.054(1) -0.0096(8) -0.004(1) -0.0184(9) C C38 0.043(1) 0.038(1) 0.045(1) -0.0208(8) 0.009(1) -0.011(1) C # 10. MOLECULAR GEOMETRY loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_1 _geom_bond_site_symmetry_2 _geom_bond_publ_flag MN1 C1 1.782(3) . . ? MN1 C2 1.805(3) . . ? MN1 C3 1.821(3) . . ? MN1 C7 2.219(2) . . ? MN1 C8 2.210(2) . . ? MN1 N1 2.012(2) . . ? MN2 C4 1.809(3) . . ? MN2 C5 1.792(3) . . ? MN2 C6 1.804(3) . . ? MN2 C30 2.253(3) . . ? MN2 C31 2.143(3) . . ? MN2 C32 2.118(3) . . ? MN2 C33 2.143(2) . . ? MN2 C34 2.258(3) . . ? C1 O1 1.158(3) . . ? C2 O2 1.146(3) . . ? C3 O3 1.148(3) . . ? C4 O4 1.147(3) . . ? C5 O5 1.151(3) . . ? C6 O6 1.145(3) . . ? C7 C8 1.468(3) . . ? C7 C18 1.520(3) . . ? C7 C24 1.579(3) . . ? C8 C9 1.440(3) . . ? C8 C13 1.459(3) . . ? C9 C10 1.356(4) . . ? C10 C11 1.402(4) . . ? C11 C12 1.372(3) . . ? C12 C13 1.444(3) . . ? C12 C28 1.503(3) . . ? C13 C14 1.490(3) . . ? C14 N1 1.344(3) . . ? C14 N2 1.323(3) . . ? N1 C15 1.337(3) . . ? C15 C16 1.377(4) . . ? C16 C17 1.374(4) . . ? C17 N2 1.341(3) . . ? C18 C19 1.394(3) . . ? C18 C23 1.398(3) . . ? C19 C20 1.388(3) . . ? C20 C21 1.379(4) . . ? C21 C22 1.379(4) . . ? C22 C23 1.387(3) . . ? C24 C25 1.535(3) . . ? C24 C26 1.546(4) . . ? C24 C27 1.546(4) . . ? C28 C29 1.353(3) . . ? C28 C35 1.561(3) . . ? C29 C30 1.477(3) . . ? C29 C34 1.473(4) . . ? C30 C31 1.394(4) . . ? C31 C32 1.418(4) . . ? C32 C33 1.413(4) . . ? C33 C34 1.387(4) . . ? C35 C36 1.534(4) . . ? C35 C37 1.543(4) . . ? C35 C38 1.546(4) . . ? loop_ _geom_contact_atom_site_label_1 _geom_contact_atom_site_label_2 _geom_contact_distance _geom_contact_site_symmetry_1 _geom_contact_site_symmetry_2 _geom_contact_publ_flag ? ? ? ? ? ? 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_2 _geom_angle_site_symmetry_3 _geom_angle_publ_flag C1 MN1 C2 90.4(1) . . . ? C1 MN1 C3 97.8(1) . . . ? C1 MN1 C7 90.0(1) . . . ? C1 MN1 C8 127.4(1) . . . ? C1 MN1 N1 100.1(1) . . . ? C2 MN1 C3 83.6(1) . . . ? C2 MN1 C7 101.1(1) . . . ? C2 MN1 C8 90.0(1) . . . ? C2 MN1 N1 168.3(1) . . . ? C3 MN1 C7 170.9(1) . . . ? C3 MN1 C8 134.4(1) . . . ? C3 MN1 N1 89.7(1) . . . ? C7 MN1 C8 38.71(8) . . . ? C7 MN1 N1 84.29(8) . . . ? C8 MN1 N1 87.84(8) . . . ? C4 MN2 C5 92.7(1) . . . ? C4 MN2 C6 88.8(1) . . . ? C4 MN2 C30 164.1(1) . . . ? C4 MN2 C31 147.4(1) . . . ? C4 MN2 C32 109.9(1) . . . ? C4 MN2 C33 90.5(1) . . . ? C4 MN2 C34 100.9(1) . . . ? C5 MN2 C6 93.8(1) . . . ? C5 MN2 C30 86.5(1) . . . ? C5 MN2 C31 119.9(1) . . . ? C5 MN2 C32 153.8(1) . . . ? C5 MN2 C33 132.1(1) . . . ? C5 MN2 C34 96.2(1) . . . ? C6 MN2 C30 107.2(1) . . . ? C6 MN2 C31 88.8(1) . . . ? C6 MN2 C32 99.7(1) . . . ? C6 MN2 C33 134.1(1) . . . ? C6 MN2 C34 165.8(1) . . . ? C30 MN2 C31 36.9(1) . . . ? C30 MN2 C32 68.0(1) . . . ? C30 MN2 C33 78.41(9) . . . ? C30 MN2 C34 63.48(9) . . . ? C31 MN2 C32 38.9(1) . . . ? C31 MN2 C33 68.6(1) . . . ? C31 MN2 C34 77.48(9) . . . ? C32 MN2 C33 38.7(1) . . . ? C32 MN2 C34 67.3(1) . . . ? C33 MN2 C34 36.6(1) . . . ? C8 C7 C18 114.6(2) . . . ? C8 C7 C24 120.5(2) . . . ? C18 C7 C24 109.6(2) . . . ? C7 C8 C9 123.5(2) . . . ? C7 C8 C13 121.7(2) . . . ? C9 C8 C13 114.7(2) . . . ? C8 C9 C10 122.7(2) . . . ? C9 C10 C11 121.3(2) . . . ? C10 C11 C12 120.9(2) . . . ? C11 C12 C13 118.7(2) . . . ? C11 C12 C28 118.4(2) . . . ? C13 C12 C28 122.9(2) . . . ? C8 C13 C12 121.1(2) . . . ? C8 C13 C14 120.1(2) . . . ? C12 C13 C14 118.5(2) . . . ? C13 C14 N1 112.0(2) . . . ? C13 C14 N2 123.2(2) . . . ? N1 C14 N2 124.8(2) . . . ? C14 N1 C15 118.6(2) . . . ? N1 C15 C16 120.4(2) . . . ? C15 C16 C17 116.9(2) . . . ? C16 C17 N2 123.5(2) . . . ? C14 N2 C17 115.8(2) . . . ? C7 C18 C19 119.7(2) . . . ? C7 C18 C23 122.9(2) . . . ? C19 C18 C23 117.3(2) . . . ? C18 C19 C20 121.2(2) . . . ? C19 C20 C21 120.5(2) . . . ? C20 C21 C22 119.4(2) . . . ? C21 C22 C23 120.3(2) . . . ? C18 C23 C22 121.4(2) . . . ? C7 C24 C25 116.3(2) . . . ? C7 C24 C26 111.5(2) . . . ? C7 C24 C27 109.6(2) . . . ? C25 C24 C26 103.7(2) . . . ? C25 C24 C27 109.5(2) . . . ? C26 C24 C27 105.6(2) . . . ? C12 C28 C29 118.4(2) . . . ? C12 C28 C35 116.5(2) . . . ? C29 C28 C35 124.0(2) . . . ? C28 C29 C30 124.4(2) . . . ? C28 C29 C34 128.4(2) . . . ? C30 C29 C34 107.1(2) . . . ? C29 C30 C31 120.4(2) . . . ? C30 C31 C32 121.1(2) . . . ? C31 C32 C33 117.0(2) . . . ? C32 C33 C34 120.2(2) . . . ? C29 C34 C33 122.2(2) . . . ? C28 C35 C36 111.4(2) . . . ? C28 C35 C37 115.1(2) . . . ? C28 C35 C38 106.3(2) . . . ? C36 C35 C37 107.3(2) . . . ? C36 C35 C38 107.4(2) . . . ? C37 C35 C38 109.0(2) . . . ? _diffrn_measured_fraction_theta_max 0.996 _diffrn_reflns_theta_full 30.02 _diffrn_measured_fraction_theta_full 0.996 data_4d _database_code_depnum_ccdc_archive 'CCDC 284346' #=============================================================================== # 5. CHEMICAL DATA _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_formula_moiety 'C72 H76 Cl2 Mn2 N8 O7' _chemical_formula_structural ? _chemical_formula_analytical ? _chemical_formula_sum 'C72 H76 Cl2 Mn2 N8 O7' _chemical_formula_weight 1346.24 _chemical_melting_point ? _chemical_compound_source ? loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source C ? 0.002 0.002 International_Tables_Vol_IV_Table_2.3.1 H ? 0.000 0.000 International_Tables_Vol_IV_Table_2.3.1 Cl ? 0.132 0.159 International_Tables_Vol_IV_Table_2.3.1 Mn ? 0.295 0.729 International_Tables_Vol_IV_Table_2.3.1 N ? 0.004 0.003 International_Tables_Vol_IV_Table_2.3.1 O ? 0.008 0.006 International_Tables_Vol_IV_Table_2.3.1 #=============================================================================== # 6. CRYSTAL DATA _symmetry_cell_setting monoclinic _symmetry_space_group_name_H-M 'P 1 21/n 1' _symmetry_space_group_name_Hall '-P 2yn' loop_ _symmetry_equiv_pos_as_xyz x,y,z 1/2-x,1/2+y,1/2-z -x,-y,-z 1/2+x,1/2-y,1/2+z _cell_length_a 12.0775(2) _cell_length_b 11.8548(2) _cell_length_c 26.0230(5) _cell_angle_alpha 90 _cell_angle_beta 97.232(5) _cell_angle_gamma 90 _cell_volume 3696.2(1) _cell_formula_units_Z 2 _cell_measurement_temperature 173 _cell_measurement_reflns_used 18493 _cell_measurement_theta_min 1.4 _cell_measurement_theta_max 30.0 _cell_special_details ; Cell parameters refined using Scalepack part of DENZO Z. Otwinowski, W. Minor, 1997 ; _exptl_crystal_description prism _exptl_crystal_colour orange _exptl_crystal_size_max 0.20 _exptl_crystal_size_mid 0.06 _exptl_crystal_size_min 0.06 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.21 _exptl_crystal_density_method none _exptl_crystal_F_000 1408 _exptl_absorpt_coefficient_mu 0.468 _exptl_absorpt_correction_type refdelf_(Walker_&_Stuart,_1983) _exptl_absorpt_correction_T_min 0.910 _exptl_absorpt_correction_T_max 0.971 #=============================================================================== # 7. EXPERIMENTAL DATA _diffrn_special_details ; ? ; _diffrn_ambient_temperature 173 _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type Mo-K\a _diffrn_source xray_tube _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type KappaCCD _diffrn_measurement_method '\p scans' _diffrn_measurement_details ; 18493 reflections were collected using program Collect ("Collect" Data collection software, Nonius B.V., 1998) The conditions were as follow : crystal to detector distance = 36. mm. Scan angle = 1.1 deg 1 scans of 50 sec per frame. Data collection was divided into 2 set(s) with the following starting angles and number of frames : Set 1 Theta = 8.80 Omega = 0.00 Kappa = 0.00 165 frames Set 2 Theta = -8.50 Kappa = 109.00 Phi = 0.00 46 frames Friedel pairs were averaged. Internal R = 0.04 ; _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% 0 _diffrn_reflns_number 18493 _diffrn_reflns_av_R_equivalents 0.040 _diffrn_reflns_av_sigmaI/netI 0.333 _diffrn_reflns_limit_h_min -16 _diffrn_reflns_limit_h_max 16 _diffrn_reflns_limit_k_min -13 _diffrn_reflns_limit_k_max 16 _diffrn_reflns_limit_l_min -36 _diffrn_reflns_limit_l_max 36 _diffrn_reflns_theta_min 2.5 _diffrn_reflns_theta_max 30.02 _reflns_number_total 11258 _reflns_number_gt 4648 _reflns_threshold_expression >3.0\s(I) _computing_structure_solution Direct_methods_(SIR,_Burla_et_al.,_1989) _computing_structure_refinement LSFM_OpenMoleN_(_1997) _computing_molecular_graphics ? _computing_publication_material CIFGEN_IN_OpenMoleN_(_1997) #=============================================================================== # 8. REFINEMENT DATA _refine_ls_structure_factor_coef F _refine_ls_matrix_type full _refine_ls_weighting_scheme sigma _refine_ls_hydrogen_treatment noref _refine_ls_extinction_method none _refine_ls_extinction_expression ? _refine_ls_extinction_coef ? _refine_ls_abs_structure_Flack ? _refine_ls_number_reflns 4648 _refine_ls_number_parameters 423 _refine_ls_number_restraints 4 _refine_ls_number_constraints 0 _refine_ls_R_factor_all 0.116 _refine_ls_R_factor_gt 0.061 _refine_ls_wR_factor_all 0.234 _refine_ls_wR_factor_ref 0.087 _refine_ls_goodness_of_fit_all 1.586 _refine_ls_goodness_of_fit_ref 1.090 _refine_ls_shift/su_max 0.013 _refine_ls_shift/esd_mean 0.002 _refine_diff_density_max 1.138 _refine_diff_density_min -0.866 #=============================================================================== # 9. ATOMIC COORDINATES AND THERMAL PARAMETERS loop_ _atom_site_label _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_occupancy _atom_site_thermal_displace_type _atom_site_calc_flag _atom_site_calc_attached_atom _atom_site_type_symbol MN 1.00125(6) 0.23340(6) 0.29547(3) 0.0185(3) 1.000 Uani ? ? Mn C1 1.1394(5) 0.2208(5) 0.3300(2) 0.028(3) 1.000 Uani ? ? C O1 1.2242(3) 0.2189(4) 0.3559(2) 0.039(2) 1.000 Uani ? ? O C2 1.0406(5) 0.3636(4) 0.2675(2) 0.027(3) 1.000 Uani ? ? C O2 1.0689(4) 0.4451(3) 0.2496(2) 0.042(2) 1.000 Uani ? ? O C3 0.9658(5) 0.2867(5) 0.3566(2) 0.030(3) 1.000 Uani ? ? C O3 0.9460(4) 0.3193(4) 0.3960(2) 0.051(3) 1.000 Uani ? ? O C4 1.0179(4) 0.1283(4) 0.2259(2) 0.020(2) 1.000 Uani ? ? C C5 0.9149(4) 0.1225(4) 0.1863(2) 0.020(2) 1.000 Uani ? ? C C6 0.8657(5) 0.2169(5) 0.1605(2) 0.030(3) 1.000 Uani ? ? C C7 0.7742(5) 0.2060(6) 0.1226(2) 0.040(3) 1.000 Uani ? ? C C8 0.7302(5) 0.1005(7) 0.1096(3) 0.041(4) 1.000 Uani ? ? C C9 0.7771(5) 0.0066(6) 0.1348(2) 0.037(3) 1.000 Uani ? ? C C10 0.8689(5) 0.0181(5) 0.1725(2) 0.027(3) 1.000 Uani ? ? C C11 1.1270(4) 0.1313(5) 0.1980(2) 0.027(3) 1.000 Uani ? ? C C12 1.2351(5) 0.1620(5) 0.2330(2) 0.032(3) 1.000 Uani ? ? C C13 1.1154(5) 0.2221(5) 0.1548(2) 0.038(3) 1.000 Uani ? ? C C14 1.1416(5) 0.0178(5) 0.1704(2) 0.036(3) 1.000 Uani ? ? C C15 1.0132(4) 0.0544(4) 0.2707(2) 0.017(2) 1.000 Uani ? ? C C16 0.9169(4) 0.0623(4) 0.3001(2) 0.016(2) 1.000 Uani ? ? C C17 0.9162(4) 0.0007(4) 0.3473(2) 0.019(2) 1.000 Uani ? ? C C18 1.0033(4) -0.0696(4) 0.3653(2) 0.023(3) 1.000 Uani ? ? C C19 1.0929(4) -0.0797(4) 0.3364(2) 0.023(3) 1.000 Uani ? ? C C20 1.0993(4) -0.0209(4) 0.2920(2) 0.021(2) 1.000 Uani ? ? C C21 0.8142(4) 0.1250(4) 0.2790(2) 0.018(2) 1.000 Uani ? ? C N1 0.8366(3) 0.2333(3) 0.2693(2) 0.017(2) 1.000 Uani ? ? N C22 0.7524(5) 0.3019(4) 0.2517(2) 0.023(2) 1.000 Uani ? ? C C23 0.6450(4) 0.2602(4) 0.2438(2) 0.023(2) 1.000 Uani ? ? C C24 0.6287(4) 0.1484(4) 0.2554(2) 0.023(3) 1.000 Uani ? ? C N2 0.7132(3) 0.0790(3) 0.2734(2) 0.020(2) 1.000 Uani ? ? N N3 0.8261(4) 0.0172(4) 0.3744(2) 0.026(2) 1.000 Uani ? ? N N4 0.8283(4) -0.0278(4) 0.4235(2) 0.024(2) 1.000 Uani ? ? N C25 0.7442(5) -0.0055(4) 0.4473(2) 0.025(3) 1.000 Uani ? ? C C26 0.6504(4) 0.0675(5) 0.4233(2) 0.025(3) 1.000 Uani ? ? C C27 0.6593(5) 0.1842(5) 0.4274(3) 0.038(3) 1.000 Uani ? ? C C28 0.5781(5) 0.2532(5) 0.4026(3) 0.046(4) 1.000 Uani ? ? C C29 0.4874(5) 0.2081(6) 0.3722(3) 0.046(4) 1.000 Uani ? ? C C30 0.4768(5) 0.0923(6) 0.3674(2) 0.035(3) 1.000 Uani ? ? C C31 0.5585(5) 0.0225(5) 0.3929(2) 0.031(3) 1.000 Uani ? ? C C32 0.7421(5) -0.0541(5) 0.5014(2) 0.033(3) 1.000 Uani ? ? C C33 0.8491(6) -0.1197(7) 0.5188(3) 0.060(4) 1.000 Uani ? ? C C34 0.6408(6) -0.1323(6) 0.5005(3) 0.050(4) 1.000 Uani ? ? C C35 0.7300(6) 0.0411(7) 0.5388(3) 0.047(4) 1.000 Uani ? ? C C36 0.386(2) 0.051(1) 0.0606(6) 0.08(1) 0.500 Uani ? ? C CL1 0.4211(5) 0.1486(6) 0.0208(3) 0.133(4) 0.500 Uani ? ? Cl CL2 0.4358(4) 0.1044(6) 0.1253(2) 0.101(3) 0.500 Uani ? ? Cl O4 0.041(1) -0.043(1) -0.0089(5) 0.090(4) 0.500 Uiso ? ? O C37 0.147(1) -0.038(1) 0.0174(7) 0.067(5) 0.500 Uiso ? ? C H01 0.7619 0.0523 0.3575 0.0466 1.000 Uiso ? ? H H1 0.8953 0.2897 0.1690 0.0390 1.000 Uiso calc C6 H H2 0.7418 0.2712 0.1055 0.0530 1.000 Uiso calc C7 H H3 0.6682 0.0929 0.0835 0.0592 1.000 Uiso calc C8 H H4 0.7468 -0.0661 0.1264 0.0492 1.000 Uiso calc C9 H H5 0.9009 -0.0475 0.1893 0.0344 1.000 Uiso calc C10 H H6 1.2959 0.1618 0.2131 0.0433 1.000 Uiso calc C12 H H7 1.2278 0.2349 0.2473 0.0433 1.000 Uiso calc C12 H H8 1.2484 0.1083 0.2602 0.0433 1.000 Uiso calc C12 H H9 1.1812 0.2232 0.1383 0.0486 1.000 Uiso calc C13 H H10 1.0530 0.2048 0.1300 0.0486 1.000 Uiso calc C13 H H11 1.1048 0.2940 0.1695 0.0486 1.000 Uiso calc C13 H H12 1.2072 0.0205 0.1538 0.0463 1.000 Uiso calc C14 H H13 1.1478 -0.0414 0.1952 0.0463 1.000 Uiso calc C14 H H14 1.0786 0.0047 0.1454 0.0463 1.000 Uiso calc C14 H H15 1.0026 -0.1104 0.3967 0.0308 1.000 Uiso calc C18 H H16 1.1519 -0.1299 0.3483 0.0316 1.000 Uiso calc C19 H H17 1.1632 -0.0303 0.2746 0.0288 1.000 Uiso calc C20 H H18 0.7665 0.3788 0.2447 0.0308 1.000 Uiso calc C22 H H19 0.5841 0.3071 0.2308 0.0312 1.000 Uiso calc C23 H H20 0.5549 0.1190 0.2505 0.0321 1.000 Uiso calc C24 H H21 0.7224 0.2166 0.4475 0.0514 1.000 Uiso calc C27 H H22 0.5847 0.3327 0.4065 0.0635 1.000 Uiso calc C28 H H23 0.4323 0.2563 0.3546 0.0626 1.000 Uiso calc C29 H H24 0.4141 0.0606 0.3467 0.0527 1.000 Uiso calc C30 H H25 0.5512 -0.0570 0.3895 0.0407 1.000 Uiso calc C31 H H26 0.8462 -0.1493 0.5525 0.0831 1.000 Uiso calc C33 H H27 0.8563 -0.1799 0.4953 0.0831 1.000 Uiso calc C33 H H28 0.9115 -0.0707 0.5193 0.0831 1.000 Uiso calc C33 H H29 0.6387 -0.1632 0.5341 0.0649 1.000 Uiso calc C34 H H30 0.5744 -0.0906 0.4905 0.0649 1.000 Uiso calc C34 H H31 0.6464 -0.1917 0.4765 0.0649 1.000 Uiso calc C34 H H32 0.7286 0.0112 0.5726 0.0663 1.000 Uiso calc C35 H H33 0.7913 0.0914 0.5390 0.0663 1.000 Uiso calc C35 H H34 0.6624 0.0805 0.5284 0.0663 1.000 Uiso calc C35 H loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_12 _atom_site_aniso_U_13 _atom_site_aniso_U_23 _atom_site_aniso_type_symbol MN 0.0141(3) 0.0160(3) 0.0281(4) -0.0005(4) 0.0006(3) -0.0011(4) Mn C1 0.028(3) 0.031(3) 0.027(3) 0.000(3) 0.004(2) -0.000(2) C O1 0.019(2) 0.070(3) 0.045(3) 0.002(2) -0.008(2) 0.001(2) O C2 0.022(3) 0.021(2) 0.045(3) -0.001(2) 0.004(3) -0.004(2) C O2 0.044(3) 0.023(2) 0.074(3) -0.009(2) 0.011(2) 0.010(2) O C3 0.023(3) 0.029(3) 0.039(3) 0.005(2) -0.006(3) -0.009(3) C O3 0.048(3) 0.068(3) 0.040(2) 0.013(2) 0.003(2) -0.021(2) O C4 0.018(2) 0.017(2) 0.024(3) -0.000(2) 0.005(2) 0.001(2) C C5 0.018(2) 0.023(2) 0.021(2) 0.002(2) 0.008(2) 0.001(2) C C6 0.034(3) 0.030(3) 0.028(3) 0.005(3) 0.008(2) 0.005(2) C C7 0.041(3) 0.051(4) 0.029(3) 0.021(3) 0.002(3) 0.007(3) C C8 0.029(3) 0.074(4) 0.031(3) 0.011(3) -0.005(3) -0.009(3) C C9 0.027(3) 0.049(3) 0.038(3) -0.006(3) 0.005(3) -0.013(3) C C10 0.025(3) 0.028(3) 0.027(3) -0.000(2) 0.006(2) -0.002(2) C C11 0.020(3) 0.029(3) 0.034(3) 0.001(2) 0.011(2) -0.000(2) C C12 0.018(3) 0.039(3) 0.045(3) -0.003(3) 0.013(2) -0.000(3) C C13 0.032(3) 0.043(3) 0.040(3) -0.004(3) 0.018(2) 0.011(3) C C14 0.028(3) 0.040(3) 0.041(3) -0.001(3) 0.015(3) -0.004(3) C C15 0.014(2) 0.014(2) 0.024(3) 0.001(2) 0.001(2) -0.002(2) C C16 0.015(2) 0.013(2) 0.023(2) -0.000(2) 0.002(2) 0.002(2) C C17 0.015(2) 0.018(2) 0.025(3) -0.001(2) 0.003(2) 0.000(2) C C18 0.022(3) 0.023(2) 0.025(3) 0.003(2) 0.001(2) 0.006(2) C C19 0.019(3) 0.021(2) 0.032(3) 0.007(2) -0.001(2) 0.002(2) C C20 0.014(2) 0.021(2) 0.032(3) 0.003(2) 0.003(2) -0.002(2) C C21 0.017(2) 0.014(2) 0.022(3) 0.003(2) 0.004(2) -0.000(2) C N1 0.013(2) 0.015(2) 0.024(2) 0.001(2) 0.001(2) -0.001(2) N C22 0.024(3) 0.015(2) 0.031(3) 0.001(2) 0.001(2) 0.002(2) C C23 0.020(2) 0.021(2) 0.030(3) 0.007(2) 0.001(2) 0.003(2) C C24 0.015(2) 0.021(2) 0.037(3) 0.002(2) 0.001(2) -0.000(2) C N2 0.015(2) 0.017(2) 0.029(2) -0.000(2) 0.002(2) 0.000(2) N N3 0.021(2) 0.033(2) 0.024(2) 0.010(2) 0.005(2) 0.010(2) N N4 0.023(2) 0.030(2) 0.019(2) 0.003(2) 0.001(2) 0.006(2) N C25 0.022(3) 0.026(3) 0.026(3) -0.001(2) 0.004(2) -0.000(2) C C26 0.020(3) 0.032(3) 0.025(3) 0.003(2) 0.008(2) 0.002(2) C C27 0.028(3) 0.034(3) 0.056(4) -0.005(3) 0.005(3) 0.000(3) C C28 0.036(3) 0.034(3) 0.079(5) 0.007(3) 0.018(3) 0.014(3) C C29 0.028(3) 0.058(4) 0.061(4) 0.016(3) 0.015(3) 0.026(3) C C30 0.019(3) 0.067(4) 0.035(3) 0.006(3) 0.001(3) 0.003(3) C C31 0.029(3) 0.037(3) 0.029(3) 0.003(3) 0.007(2) -0.003(3) C C32 0.029(3) 0.048(3) 0.027(3) 0.005(3) 0.008(2) 0.006(3) C C33 0.057(4) 0.097(5) 0.040(4) 0.031(4) 0.013(3) 0.037(4) C C34 0.063(4) 0.052(4) 0.040(4) -0.002(4) 0.023(3) 0.011(3) C C35 0.050(4) 0.077(5) 0.026(3) -0.004(4) 0.006(3) 0.000(4) C C36 0.11(1) 0.059(9) 0.06(1) 0.027(9) 0.036(9) 0.016(8) C CL1 0.100(4) 0.173(5) 0.137(4) 0.058(4) 0.031(3) 0.077(4) Cl CL2 0.072(3) 0.143(5) 0.101(3) 0.005(3) 0.047(2) -0.019(3) Cl # 10. MOLECULAR GEOMETRY loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_1 _geom_bond_site_symmetry_2 _geom_bond_publ_flag MN C1 1.799(6) . . ? MN C2 1.795(6) . . ? MN C3 1.812(7) . . ? MN C4 2.228(5) . . ? MN C15 2.227(5) . . ? MN C16 2.279(5) . . ? MN N1 2.019(4) . . ? C1 O1 1.154(7) . . ? C2 O2 1.144(7) . . ? C3 O3 1.150(7) . . ? C4 C5 1.514(7) . . ? C4 C11 1.582(7) . . ? C4 C15 1.465(7) . . ? C5 C6 1.398(7) . . ? C5 C10 1.385(8) . . ? C6 C7 1.393(9) . . ? C7 C8 1.38(1) . . ? C8 C9 1.38(1) . . ? C9 C10 1.392(8) . . ? C11 C12 1.539(8) . . ? C11 C13 1.551(8) . . ? C11 C14 1.544(8) . . ? C15 C16 1.472(7) . . ? C15 C20 1.429(7) . . ? C16 C17 1.432(7) . . ? C16 C21 1.490(7) . . ? C17 C18 1.377(7) . . ? C17 N3 1.383(7) . . ? C18 C19 1.399(8) . . ? C19 C20 1.358(8) . . ? C21 N1 1.343(6) . . ? C21 N2 1.327(6) . . ? N1 C22 1.337(7) . . ? C22 C23 1.379(8) . . ? C23 C24 1.380(7) . . ? C24 N2 1.348(7) . . ? N3 N4 1.381(6) . . ? N4 C25 1.283(7) . . ? C25 C26 1.498(8) . . ? C25 C32 1.523(8) . . ? C26 C27 1.390(8) . . ? C26 C31 1.385(8) . . ? C27 C28 1.374(9) . . ? C28 C29 1.38(1) . . ? C29 C30 1.38(1) . . ? C30 C31 1.391(9) . . ? C32 C33 1.527(9) . . ? C32 C34 1.53(1) . . ? C32 C35 1.51(1) . . ? C36 CL1 1.64(2) . . ? C36 CL2 1.83(2) . . ? O4 O4 1.52(3) . 3_555 ? O4 C37 1.38(2) . . ? loop_ _geom_contact_atom_site_label_1 _geom_contact_atom_site_label_2 _geom_contact_distance _geom_contact_site_symmetry_1 _geom_contact_site_symmetry_2 _geom_contact_publ_flag ? ? ? ? ? ? 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_2 _geom_angle_site_symmetry_3 _geom_angle_publ_flag C1 MN C2 89.8(3) . . . ? C1 MN C3 84.2(3) . . . ? C1 MN C4 100.7(2) . . . ? C1 MN C15 88.6(2) . . . ? C1 MN C16 107.0(2) . . . ? C1 MN N1 168.7(2) . . . ? C2 MN C3 99.2(3) . . . ? C2 MN C4 95.5(2) . . . ? C2 MN C15 132.2(2) . . . ? C2 MN C16 158.2(2) . . . ? C2 MN N1 99.4(2) . . . ? C3 MN C4 164.6(2) . . . ? C3 MN C15 128.1(2) . . . ? C3 MN C16 96.2(2) . . . ? C3 MN N1 88.0(2) . . . ? C4 MN C15 38.4(2) . . . ? C4 MN C16 68.4(2) . . . ? C4 MN N1 85.0(2) . . . ? C15 MN C16 38.1(2) . . . ? C15 MN N1 90.0(2) . . . ? C16 MN N1 65.8(2) . . . ? C5 C4 C11 110.4(4) . . . ? C5 C4 C15 113.8(4) . . . ? C11 C4 C15 119.8(4) . . . ? C4 C5 C6 123.6(5) . . . ? C4 C5 C10 119.0(5) . . . ? C6 C5 C10 117.3(5) . . . ? C5 C6 C7 121.2(6) . . . ? C6 C7 C8 120.1(6) . . . ? C7 C8 C9 119.6(6) . . . ? C8 C9 C10 120.0(6) . . . ? C5 C10 C9 121.9(6) . . . ? C4 C11 C12 115.3(5) . . . ? C4 C11 C13 110.1(5) . . . ? C4 C11 C14 110.1(4) . . . ? C12 C11 C13 104.9(5) . . . ? C12 C11 C14 110.1(5) . . . ? C13 C11 C14 105.8(5) . . . ? C4 C15 C16 119.2(4) . . . ? C4 C15 C20 125.7(5) . . . ? C16 C15 C20 115.0(5) . . . ? C15 C16 C17 120.2(4) . . . ? C15 C16 C21 121.1(4) . . . ? C17 C16 C21 118.4(4) . . . ? C16 C17 C18 120.9(5) . . . ? C16 C17 N3 117.2(4) . . . ? C18 C17 N3 121.9(5) . . . ? C17 C18 C19 118.6(5) . . . ? C18 C19 C20 122.9(5) . . . ? C15 C20 C19 122.3(5) . . . ? C16 C21 N1 111.5(4) . . . ? C16 C21 N2 123.2(4) . . . ? N1 C21 N2 125.2(5) . . . ? C21 N1 C22 118.9(4) . . . ? N1 C22 C23 119.6(5) . . . ? C22 C23 C24 118.0(5) . . . ? C23 C24 N2 122.6(5) . . . ? C21 N2 C24 115.7(4) . . . ? C17 N3 N4 119.5(4) . . . ? N3 N4 C25 116.3(4) . . . ? N4 C25 C26 121.4(5) . . . ? N4 C25 C32 118.3(5) . . . ? C26 C25 C32 120.3(5) . . . ? C25 C26 C27 119.7(6) . . . ? C25 C26 C31 121.7(5) . . . ? C27 C26 C31 118.4(6) . . . ? C26 C27 C28 120.8(6) . . . ? C27 C28 C29 120.5(6) . . . ? C28 C29 C30 119.7(6) . . . ? C29 C30 C31 119.7(6) . . . ? C26 C31 C30 120.8(6) . . . ? C25 C32 C33 110.8(5) . . . ? C25 C32 C34 108.8(5) . . . ? C25 C32 C35 109.1(5) . . . ? C33 C32 C34 109.9(6) . . . ? C33 C32 C35 109.6(6) . . . ? C34 C32 C35 108.6(5) . . . ? CL1 C36 CL2 105(1) . . . ? O4 O4 C37 114(1) 3_555 . . ? _diffrn_measured_fraction_theta_max 0.996 _diffrn_reflns_theta_full 30.02 _diffrn_measured_fraction_theta_full 0.996 #END