Supplementary Material (ESI) for Chemical Communications This journal is © The Royal Society of Chemistry 2002 data_global #=============================================================================== _audit_creation_date 31-08-00 _journal_coden_Cambridge 182 loop_ _publ_author_name 'Djukic, Jean-Pierre' 'de Cian, Andre' 'Fischer, Jean' 'Heinz Dotz, Karl' 'Pfeffer, Michel' # 1. SUBMISSION DETAILS _publ_contact_author_name # ; Jean-Pierre Djukic ; _publ_contact_author_address # ; LSMI- UMR 7513 CNRS Université Louis Pasteur 4, rue Blaise Pascal STRASBOURG 67070 FRANCE ; _publ_contact_author_phone '+33(0)390241523' _publ_contact_author_fax '+33(0)390245001' _publ_contact_author_email djukic@chimie.u-strasbg.fr _publ_requested_journal 'Chem. Commun.' _publ_section_title ; Expression of the prohelicity of biscyclomanganated 2,3-diphenylquinoxaline through reaction with diaryldiazoalkane ; _publ_contact_letter ; Please consider this CIF submission forthe publication of a new paper in Chemical Communications. ; _publ_requested_category FM #=============================================================================== # 3. TITLE AND AUTHOR LIST # The loop structure below should contain the names and addresses of all # authors, in the required order of publication. Repeat as necessary. # 4. TEXT _publ_section_abstract ; ? ; _publ_section_comment ; ? ; _publ_section_exptl_prep ; ? ; _publ_section_exptl_refinement ; ? ; _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. ; _publ_section_figure_captions ; ? ; _publ_section_acknowledgements ; ? ; #=============================================================================== # If more than one structure is reported, sections 5-10 should be filled in # per structure. For each data set, replace the ? in the data_? line below # by a unique identifier. data_1c _database_code_CSD 176859 #=============================================================================== # 5. CHEMICAL DATA _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_formula_moiety 'C52 H32 Mn2 N2 O6' _chemical_formula_structural ? _chemical_formula_analytical ? _chemical_formula_sum 'C52 H32 Mn2 N2 O6' _chemical_formula_weight 890.72 _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 21/n' _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 15.6887(7) _cell_length_b 16.7698(9) _cell_length_c 15.9857(7) _cell_angle_alpha 90 _cell_angle_beta 93.588(5) _cell_angle_gamma 90 _cell_volume 4197.5(3) _cell_formula_units_Z 4 _cell_measurement_temperature 294 _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 blue' _exptl_crystal_size_max 0.20 _exptl_crystal_size_mid 0.14 _exptl_crystal_size_min 0.10 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.41 _exptl_crystal_density_method 'none' _exptl_crystal_F_000 1824 _exptl_absorpt_coefficient_mu 0.657 _exptl_absorpt_correction_type none _exptl_absorpt_correction_T_min ? _exptl_absorpt_correction_T_max ? #=============================================================================== # 7. EXPERIMENTAL DATA _diffrn_special_details ; ? ; _diffrn_ambient_temperature 294 _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 ; 16708 reflections were collected using program Collect ("Collect" Data collection software, Nonius B.V., 1998) The conditions were as follow : crystal to detector distance = 35. mm. Scan angle = 2.0 deg 1 scans of 40 sec per frame. Data collection was divided into 1 set(s) with the following starting angles and number of frames : Set 1 Theta = 5.90 Omega = 0.00 Kappa = 0.00 99 frames Friedel pairs were averaged. Internal R = 0.06 ; _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% 0 _diffrn_reflns_number 16708 _diffrn_reflns_av_R_equivalents 0.060 _diffrn_reflns_av_sigmaI/netI 0.333 _diffrn_reflns_limit_h_min -20 _diffrn_reflns_limit_h_max 20 _diffrn_reflns_limit_k_min -21 _diffrn_reflns_limit_k_max 20 _diffrn_reflns_limit_l_min -20 _diffrn_reflns_limit_l_max 20 _diffrn_reflns_theta_min 2.5 _diffrn_reflns_theta_max 27.51 _reflns_number_total 9786 _reflns_number_gt 3947 _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 3947 _refine_ls_number_parameters 559 _refine_ls_number_restraints 0 _refine_ls_number_constraints 0 _refine_ls_R_factor_all 0.139 _refine_ls_R_factor_gt 0.035 _refine_ls_wR_factor_all 0.283 _refine_ls_wR_factor_ref 0.040 _refine_ls_goodness_of_fit_all 8.409 _refine_ls_goodness_of_fit_ref 1.040 _refine_ls_shift/su_max 0.003 _refine_ls_shift/esd_mean 0.000 _refine_diff_density_max 0.289 _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 0.28683(3) 0.18729(3) 0.32886(3) 0.0374(3) Uani ? ? Mn MN2 0.65448(3) 0.09686(3) 0.16454(3) 0.0341(3) Uani ? ? Mn C1 0.1903(1) 0.1668(2) 0.3794(1) 0.049(2) Uani ? ? C O1 0.1292(1) 0.1580(2) 0.4147(1) 0.079(2) Uani ? ? O C2 0.3379(2) 0.1985(3) 0.4334(2) 0.065(3) Uani ? ? C O2 0.3647(1) 0.2033(3) 0.5009(1) 0.107(3) Uani ? ? O C3 0.2466(2) 0.2863(2) 0.3194(2) 0.053(2) Uani ? ? C O3 0.2163(1) 0.3491(1) 0.3172(1) 0.080(2) Uani ? ? O C4 0.2419(2) 0.1370(2) 0.2097(2) 0.032(2) Uani ? ? C C5 0.1476(2) 0.1345(2) 0.1805(2) 0.037(2) Uani ? ? C C6 0.0912(2) 0.1963(2) 0.1926(2) 0.049(2) Uani ? ? C C7 0.0068(2) 0.1927(3) 0.1606(2) 0.061(3) Uani ? ? C C8 -0.0229(2) 0.1280(3) 0.1170(2) 0.062(3) Uani ? ? C C9 0.0312(2) 0.0656(2) 0.1044(2) 0.065(3) Uani ? ? C C10 0.1163(2) 0.0694(2) 0.1343(2) 0.055(2) Uani ? ? C C11 0.2912(1) 0.1610(2) 0.1347(1) 0.031(2) Uani ? ? C C12 0.3345(1) 0.1059(2) 0.0891(1) 0.043(2) Uani ? ? C C13 0.3776(2) 0.1286(2) 0.0198(2) 0.053(2) Uani ? ? C C14 0.3761(2) 0.2064(2) -0.0054(2) 0.058(2) Uani ? ? C C15 0.3315(1) 0.2614(2) 0.0371(1) 0.054(2) Uani ? ? C C16 0.2892(1) 0.2391(2) 0.1062(1) 0.045(2) Uani ? ? C C17 0.2736(2) 0.0719(2) 0.2634(2) 0.031(2) Uani ? ? C C18 0.2176(2) 0.0143(2) 0.2980(2) 0.038(2) Uani ? ? C C19 0.2450(2) -0.0428(2) 0.3527(2) 0.046(2) Uani ? ? C C20 0.3306(2) -0.0482(2) 0.3800(2) 0.047(2) Uani ? ? C C21 0.3870(2) 0.0056(2) 0.3527(2) 0.040(2) Uani ? ? C C22 0.3607(2) 0.0669(2) 0.2963(2) 0.031(2) Uani ? ? C C23 0.4257(1) 0.1231(2) 0.2662(1) 0.028(2) Uani ? ? C N1 0.4017(1) 0.1983(1) 0.2745(1) 0.030(1) Uani ? ? N C24 0.4530(1) 0.2579(2) 0.2472(1) 0.034(2) Uani ? ? C C25 0.5267(1) 0.2383(2) 0.2055(1) 0.033(2) Uani ? ? C C26 0.5746(2) 0.2996(2) 0.1715(2) 0.052(2) Uani ? ? C C27 0.5545(2) 0.3766(2) 0.1860(2) 0.062(2) Uani ? ? C C28 0.4860(1) 0.3960(2) 0.2332(1) 0.058(2) Uani ? ? C C29 0.4348(1) 0.3383(2) 0.2621(2) 0.046(2) Uani ? ? C C30 0.7370(2) 0.0308(2) 0.1338(2) 0.047(2) Uani ? ? C O4 0.7907(1) -0.0089(2) 0.1104(1) 0.076(2) Uani ? ? O C31 0.6099(2) 0.0932(2) 0.0569(2) 0.051(2) Uani ? ? C O5 0.5879(1) 0.0910(2) -0.0129(1) 0.081(2) Uani ? ? O C32 0.7260(2) 0.1760(2) 0.1471(2) 0.044(2) Uani ? ? C O6 0.7747(1) 0.2255(2) 0.1350(1) 0.067(2) Uani ? ? O C33 0.6853(2) 0.0837(2) 0.2971(2) 0.032(2) Uani ? ? C C34 0.6501(1) 0.1492(2) 0.3509(1) 0.034(2) Uani ? ? C C35 0.5910(1) 0.1334(2) 0.4098(1) 0.043(2) Uani ? ? C C36 0.5642(2) 0.1934(3) 0.4618(2) 0.059(2) Uani ? ? C C37 0.5964(2) 0.2688(2) 0.4560(2) 0.072(3) Uani ? ? C C38 0.6553(1) 0.2857(2) 0.3993(1) 0.067(3) Uani ? ? C C39 0.6828(1) 0.2259(2) 0.3479(1) 0.051(2) Uani ? ? C C40 0.7750(2) 0.0672(2) 0.3344(2) 0.034(2) Uani ? ? C C41 0.7857(2) 0.0304(2) 0.4129(2) 0.045(2) Uani ? ? C C42 0.8644(2) 0.0262(2) 0.4565(2) 0.048(2) Uani ? ? C C43 0.9342(2) 0.0602(2) 0.4238(2) 0.049(2) Uani ? ? C C44 0.9265(2) 0.0952(2) 0.3469(2) 0.050(2) Uani ? ? C C45 0.8481(2) 0.0982(2) 0.3024(2) 0.044(2) Uani ? ? C C46 0.6321(1) 0.0156(2) 0.2706(1) 0.033(2) Uani ? ? C C47 0.6643(2) -0.0642(2) 0.2701(2) 0.041(2) Uani ? ? C C48 0.6181(2) -0.1265(2) 0.2380(2) 0.047(2) Uani ? ? C C49 0.5356(1) -0.1160(2) 0.2025(1) 0.045(2) Uani ? ? C C50 0.5009(1) -0.0421(2) 0.1999(1) 0.038(2) Uani ? ? C C51 0.5469(1) 0.0249(2) 0.2322(1) 0.031(2) Uani ? ? C C52 0.5048(1) 0.1041(2) 0.2339(1) 0.026(2) Uani ? ? C N2 0.5522(1) 0.1602(1) 0.2016(1) 0.031(1) Uani ? ? N H1 0.1105 0.2420 0.2234 0.0663 Uiso calc C6 H H2 -0.0305 0.2361 0.1693 0.0878 Uiso calc C7 H H3 -0.0807 0.1259 0.0955 0.0925 Uiso calc C8 H H4 0.0106 0.0195 0.0751 0.0866 Uiso calc C9 H H5 0.1537 0.0267 0.1229 0.0725 Uiso calc C10 H H6 0.3348 0.0515 0.1055 0.0556 Uiso calc C12 H H7 0.4080 0.0901 -0.0101 0.0705 Uiso calc C13 H H8 0.4062 0.2222 -0.0525 0.0771 Uiso calc C14 H H9 0.3295 0.3153 0.0188 0.0718 Uiso calc C15 H H10 0.2581 0.2779 0.1350 0.0585 Uiso calc C16 H H11 0.1584 0.0166 0.2815 0.0504 Uiso calc C18 H H12 0.2052 -0.0797 0.3729 0.0603 Uiso calc C19 H H13 0.3495 -0.0894 0.4175 0.0616 Uiso calc C20 H H14 0.4454 0.0021 0.3720 0.0529 Uiso calc C21 H H15 0.6210 0.2870 0.1383 0.0716 Uiso calc C26 H H16 0.5877 0.4179 0.1637 0.0942 Uiso calc C27 H H17 0.4749 0.4504 0.2454 0.0900 Uiso calc C28 H H18 0.3868 0.3524 0.2924 0.0671 Uiso calc C29 H H19 0.5687 0.0811 0.4146 0.0587 Uiso calc C35 H H20 0.5234 0.1821 0.5017 0.0842 Uiso calc C36 H H21 0.5776 0.3097 0.4916 0.0949 Uiso calc C37 H H22 0.6774 0.3382 0.3952 0.0897 Uiso calc C38 H H23 0.7251 0.2376 0.3096 0.0665 Uiso calc C39 H H24 0.7375 0.0076 0.4369 0.0593 Uiso calc C41 H H25 0.8701 -0.0003 0.5091 0.0633 Uiso calc C42 H H26 0.9879 0.0595 0.4547 0.0669 Uiso calc C43 H H27 0.9753 0.1176 0.3236 0.0684 Uiso calc C44 H H28 0.8443 0.1222 0.2485 0.0589 Uiso calc C45 H H29 0.7206 -0.0739 0.2933 0.0547 Uiso calc C47 H H30 0.6424 -0.1784 0.2397 0.0646 Uiso calc C48 H H31 0.5038 -0.1603 0.1804 0.0593 Uiso calc C49 H H32 0.4445 -0.0350 0.1759 0.0496 Uiso calc C50 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 0.0307(3) 0.0401(3) 0.0427(3) -0.0011(3) 0.0073(2) -0.0049(3) Mn MN2 0.0298(3) 0.0378(3) 0.0352(3) 0.0020(2) 0.0048(2) 0.0003(3) Mn C1 0.048(2) 0.052(2) 0.047(2) -0.003(2) 0.007(2) -0.005(2) C O1 0.054(1) 0.106(2) 0.085(2) -0.016(2) 0.037(1) -0.001(2) O C2 0.042(2) 0.125(3) 0.051(2) -0.002(3) 0.009(2) -0.037(2) C O2 0.066(2) 0.329(5) 0.057(2) 0.007(3) -0.005(2) -0.078(3) O C3 0.041(2) 0.048(2) 0.074(2) -0.002(2) 0.018(2) -0.008(2) C O3 0.076(2) 0.050(2) 0.136(2) 0.019(1) 0.039(2) 0.002(2) O C4 0.028(2) 0.033(2) 0.037(2) -0.002(2) 0.004(1) 0.005(2) C C5 0.029(2) 0.046(2) 0.039(2) -0.002(2) -0.001(2) 0.007(2) C C6 0.034(2) 0.068(2) 0.050(2) 0.004(2) 0.002(2) 0.002(2) C C7 0.035(2) 0.105(3) 0.063(3) 0.018(2) 0.006(2) 0.007(3) C C8 0.035(2) 0.122(4) 0.056(2) -0.014(2) -0.002(2) 0.018(3) C C9 0.054(2) 0.085(3) 0.058(2) -0.030(2) -0.012(2) 0.006(2) C C10 0.048(2) 0.057(2) 0.061(2) -0.005(2) -0.005(2) 0.006(2) C C11 0.025(2) 0.035(2) 0.035(2) 0.001(2) -0.005(2) 0.001(2) C C12 0.045(2) 0.040(2) 0.043(2) 0.006(2) -0.001(2) 0.002(2) C C13 0.056(2) 0.069(2) 0.039(2) 0.010(2) 0.010(2) -0.004(2) C C14 0.066(2) 0.073(3) 0.041(2) -0.006(2) 0.017(2) 0.009(2) C C15 0.071(2) 0.045(2) 0.051(2) -0.008(2) 0.009(2) 0.013(2) C C16 0.048(2) 0.039(2) 0.048(2) 0.002(2) 0.007(2) 0.004(2) C C17 0.029(2) 0.031(2) 0.033(2) -0.003(2) 0.003(1) -0.004(2) C C18 0.030(2) 0.040(2) 0.046(2) -0.008(2) 0.001(2) -0.000(2) C C19 0.054(2) 0.041(2) 0.046(2) -0.007(2) 0.012(2) 0.009(2) C C20 0.054(2) 0.048(2) 0.040(2) 0.003(2) -0.002(2) 0.014(2) C C21 0.039(2) 0.043(2) 0.040(2) -0.001(2) -0.004(2) 0.010(2) C C22 0.029(2) 0.032(2) 0.032(2) -0.001(1) 0.003(1) -0.001(2) C C23 0.028(2) 0.030(2) 0.026(2) 0.001(2) -0.005(1) 0.000(2) C N1 0.023(1) 0.034(1) 0.035(1) -0.001(1) -0.002(1) -0.004(1) N C24 0.026(2) 0.032(2) 0.049(2) -0.002(2) -0.004(2) 0.001(2) C C25 0.026(2) 0.032(2) 0.044(2) 0.002(2) -0.001(2) 0.005(2) C C26 0.039(2) 0.040(2) 0.088(3) 0.003(2) 0.020(2) 0.021(2) C C27 0.048(2) 0.038(2) 0.134(3) 0.006(2) 0.023(2) 0.032(2) C C28 0.046(2) 0.032(2) 0.130(4) 0.008(2) 0.015(2) -0.002(2) C C29 0.034(2) 0.032(2) 0.090(3) -0.000(2) 0.016(2) -0.002(2) C C30 0.043(2) 0.051(2) 0.048(2) -0.002(2) 0.007(2) -0.005(2) C O4 0.061(2) 0.072(2) 0.100(2) 0.021(1) 0.027(1) -0.018(2) O C31 0.045(2) 0.069(2) 0.043(2) 0.004(2) 0.006(2) -0.003(2) C O5 0.089(2) 0.142(3) 0.042(2) 0.017(2) -0.005(1) -0.009(2) O C32 0.033(2) 0.054(2) 0.047(2) 0.006(2) 0.012(1) 0.007(2) C O6 0.046(1) 0.066(2) 0.096(2) -0.011(1) 0.017(1) 0.018(2) O C33 0.029(2) 0.035(2) 0.033(2) 0.004(2) 0.002(1) 0.003(2) C C34 0.029(2) 0.039(2) 0.035(2) 0.005(2) -0.007(2) 0.000(2) C C35 0.034(2) 0.062(2) 0.038(2) 0.005(2) -0.005(2) -0.003(2) C C36 0.048(2) 0.104(3) 0.042(2) 0.019(2) -0.001(2) -0.025(2) C C37 0.074(3) 0.079(3) 0.063(3) 0.029(2) -0.017(2) -0.036(2) C C38 0.087(3) 0.051(2) 0.067(3) 0.003(2) -0.014(2) -0.018(2) C C39 0.056(2) 0.045(2) 0.051(2) -0.002(2) -0.004(2) -0.006(2) C C40 0.031(2) 0.032(2) 0.039(2) 0.003(2) 0.000(2) -0.001(2) C C41 0.032(2) 0.056(2) 0.049(2) 0.008(2) 0.005(2) 0.004(2) C C42 0.041(2) 0.062(2) 0.043(2) 0.015(2) -0.001(2) 0.006(2) C C43 0.033(2) 0.058(2) 0.061(2) 0.007(2) -0.014(2) 0.001(2) C C44 0.031(2) 0.060(2) 0.067(2) -0.002(2) -0.002(2) 0.010(2) C C45 0.030(2) 0.054(2) 0.051(2) -0.001(2) -0.003(2) 0.009(2) C C46 0.030(2) 0.035(2) 0.035(2) 0.003(2) 0.003(1) 0.002(2) C C47 0.034(2) 0.039(2) 0.053(2) 0.009(2) 0.000(2) 0.005(2) C C48 0.052(2) 0.030(2) 0.067(2) 0.004(2) 0.006(2) 0.002(2) C C49 0.046(2) 0.035(2) 0.056(2) -0.002(2) 0.002(2) -0.005(2) C C50 0.031(2) 0.039(2) 0.044(2) -0.001(2) -0.000(2) -0.001(2) C C51 0.029(2) 0.029(2) 0.035(2) 0.001(1) 0.003(1) 0.001(2) C C52 0.024(2) 0.031(2) 0.025(2) 0.001(2) -0.003(1) 0.001(2) C N2 0.028(1) 0.034(1) 0.031(1) 0.002(1) -0.001(1) 0.005(1) N # 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 1.795(4) . . ? MN1 C2 1.818(5) . . ? MN1 C3 1.780(4) . . ? MN1 C4 2.161(4) . . ? MN1 C17 2.203(3) . . ? MN1 N1 2.057(3) . . ? MN2 C30 1.797(4) . . ? MN2 C31 1.819(5) . . ? MN2 C32 1.772(4) . . ? MN2 C33 2.154(4) . . ? MN2 C46 2.220(3) . . ? MN2 N2 2.043(3) . . ? C1 O1 1.151(4) . . ? C2 O2 1.135(5) . . ? C3 O3 1.154(4) . . ? C4 C5 1.523(5) . . ? C4 C11 1.521(5) . . ? C4 C17 1.457(5) . . ? C5 C6 1.385(5) . . ? C5 C10 1.391(5) . . ? C6 C7 1.390(6) . . ? C7 C8 1.356(7) . . ? C8 C9 1.370(7) . . ? C9 C10 1.390(6) . . ? C11 C12 1.382(5) . . ? C11 C16 1.387(5) . . ? C12 C13 1.385(5) . . ? C13 C14 1.365(6) . . ? C14 C15 1.365(5) . . ? C15 C16 1.376(5) . . ? C17 C18 1.439(4) . . ? C17 C22 1.437(5) . . ? C18 C19 1.348(5) . . ? C19 C20 1.389(6) . . ? C20 C21 1.356(5) . . ? C21 C22 1.412(5) . . ? C22 C23 1.491(4) . . ? C23 N1 1.325(4) . . ? C23 C52 1.410(4) . . ? N1 C24 1.371(4) . . ? C24 C25 1.408(4) . . ? C24 C29 1.403(5) . . ? C25 C26 1.404(5) . . ? C25 N2 1.372(4) . . ? C26 C27 1.352(5) . . ? C27 C28 1.390(6) . . ? C28 C29 1.357(5) . . ? C30 O4 1.153(4) . . ? C31 O5 1.146(5) . . ? C32 O6 1.152(4) . . ? C33 C34 1.520(5) . . ? C33 C40 1.520(5) . . ? C33 C46 1.462(5) . . ? C34 C35 1.387(5) . . ? C34 C39 1.388(5) . . ? C35 C36 1.388(5) . . ? C36 C37 1.366(7) . . ? C37 C38 1.365(7) . . ? C38 C39 1.382(5) . . ? C40 C41 1.398(5) . . ? C40 C45 1.388(5) . . ? C41 C42 1.382(5) . . ? C42 C43 1.367(5) . . ? C43 C44 1.360(6) . . ? C44 C45 1.381(5) . . ? C46 C47 1.431(5) . . ? C46 C51 1.444(5) . . ? C47 C48 1.356(5) . . ? C48 C49 1.391(5) . . ? C49 C50 1.353(5) . . ? C50 C51 1.413(5) . . ? C51 C52 1.485(4) . . ? C52 N2 1.325(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 86.7(2) . . . ? C1 MN1 C3 85.0(2) . . . ? C1 MN1 C4 94.8(2) . . . ? C1 MN1 C17 89.3(1) . . . ? C1 MN1 N1 173.7(2) . . . ? C2 MN1 C3 96.6(2) . . . ? C2 MN1 C4 162.2(2) . . . ? C2 MN1 C17 123.4(2) . . . ? C2 MN1 N1 91.8(2) . . . ? C3 MN1 C4 101.3(2) . . . ? C3 MN1 C17 139.2(2) . . . ? C3 MN1 N1 101.3(1) . . . ? C4 MN1 C17 39.0(1) . . . ? C4 MN1 N1 84.8(1) . . . ? C17 MN1 N1 86.4(1) . . . ? C30 MN2 C31 87.8(2) . . . ? C30 MN2 C32 86.8(2) . . . ? C30 MN2 C33 94.9(2) . . . ? C30 MN2 C46 88.9(1) . . . ? C30 MN2 N2 173.2(1) . . . ? C31 MN2 C32 94.9(2) . . . ? C31 MN2 C33 167.6(2) . . . ? C31 MN2 C46 129.2(2) . . . ? C31 MN2 N2 91.7(2) . . . ? C32 MN2 C33 97.3(2) . . . ? C32 MN2 C46 135.4(2) . . . ? C32 MN2 N2 99.9(1) . . . ? C33 MN2 C46 39.0(1) . . . ? C33 MN2 N2 84.2(1) . . . ? C46 MN2 N2 86.2(1) . . . ? MN1 C1 O1 175.6(4) . . . ? MN1 C2 O2 175.1(4) . . . ? MN1 C3 O3 175.2(4) . . . ? MN1 C4 C5 122.5(2) . . . ? MN1 C4 C11 115.9(2) . . . ? MN1 C4 C17 72.1(2) . . . ? C5 C4 C11 107.4(3) . . . ? C5 C4 C17 116.7(3) . . . ? C11 C4 C17 119.3(3) . . . ? C4 C5 C6 123.6(4) . . . ? C4 C5 C10 119.3(3) . . . ? C6 C5 C10 117.0(4) . . . ? C5 C6 C7 121.2(4) . . . ? C6 C7 C8 120.9(4) . . . ? C7 C8 C9 119.3(4) . . . ? C8 C9 C10 120.4(4) . . . ? C5 C10 C9 121.2(4) . . . ? C4 C11 C12 122.1(3) . . . ? C4 C11 C16 120.4(3) . . . ? C12 C11 C16 117.3(3) . . . ? C11 C12 C13 121.3(3) . . . ? C12 C13 C14 119.9(4) . . . ? C13 C14 C15 120.0(4) . . . ? C14 C15 C16 120.2(4) . . . ? C11 C16 C15 121.3(3) . . . ? MN1 C17 C4 68.9(2) . . . ? MN1 C17 C18 116.6(2) . . . ? MN1 C17 C22 79.5(2) . . . ? C4 C17 C18 122.4(3) . . . ? C4 C17 C22 122.8(3) . . . ? C18 C17 C22 114.1(3) . . . ? C17 C18 C19 123.3(3) . . . ? C18 C19 C20 120.9(3) . . . ? C19 C20 C21 119.6(4) . . . ? C20 C21 C22 121.3(4) . . . ? C17 C22 C21 120.7(3) . . . ? C17 C22 C23 119.9(3) . . . ? C21 C22 C23 119.2(3) . . . ? C22 C23 N1 111.4(3) . . . ? C22 C23 C52 127.6(3) . . . ? N1 C23 C52 121.0(3) . . . ? MN1 N1 C23 102.7(2) . . . ? MN1 N1 C24 138.3(2) . . . ? C23 N1 C24 119.0(3) . . . ? N1 C24 C25 119.8(3) . . . ? N1 C24 C29 121.1(3) . . . ? C25 C24 C29 119.1(3) . . . ? C24 C25 C26 119.3(3) . . . ? C24 C25 N2 119.6(3) . . . ? C26 C25 N2 121.0(3) . . . ? C25 C26 C27 119.7(3) . . . ? C26 C27 C28 121.0(4) . . . ? C27 C28 C29 120.7(4) . . . ? C24 C29 C28 119.8(3) . . . ? MN2 C30 O4 176.2(4) . . . ? MN2 C31 O5 174.8(4) . . . ? MN2 C32 O6 177.5(3) . . . ? MN2 C33 C34 114.6(2) . . . ? MN2 C33 C40 123.4(2) . . . ? MN2 C33 C46 72.9(2) . . . ? C34 C33 C40 105.6(3) . . . ? C34 C33 C46 120.5(3) . . . ? C40 C33 C46 118.0(3) . . . ? C33 C34 C35 121.9(3) . . . ? C33 C34 C39 120.1(3) . . . ? C35 C34 C39 117.7(3) . . . ? C34 C35 C36 120.6(4) . . . ? C35 C36 C37 120.2(4) . . . ? C36 C37 C38 120.4(4) . . . ? C37 C38 C39 119.6(4) . . . ? C34 C39 C38 121.5(4) . . . ? C33 C40 C41 119.4(3) . . . ? C33 C40 C45 123.6(3) . . . ? C41 C40 C45 116.1(4) . . . ? C40 C41 C42 122.0(3) . . . ? C41 C42 C43 119.8(4) . . . ? C42 C43 C44 119.8(4) . . . ? C43 C44 C45 120.5(4) . . . ? C40 C45 C44 121.7(4) . . . ? MN2 C46 C33 68.1(2) . . . ? MN2 C46 C47 119.8(2) . . . ? MN2 C46 C51 78.2(2) . . . ? C33 C46 C47 122.4(3) . . . ? C33 C46 C51 122.4(3) . . . ? C47 C46 C51 114.6(3) . . . ? C46 C47 C48 122.8(4) . . . ? C47 C48 C49 121.3(3) . . . ? C48 C49 C50 119.4(4) . . . ? C49 C50 C51 121.4(4) . . . ? C46 C51 C50 120.5(3) . . . ? C46 C51 C52 119.3(3) . . . ? C50 C51 C52 120.0(3) . . . ? C23 C52 C51 127.8(3) . . . ? C23 C52 N2 120.7(3) . . . ? C51 C52 N2 111.6(3) . . . ? MN2 N2 C25 138.3(2) . . . ? MN2 N2 C52 102.3(2) . . . ? C25 N2 C52 119.2(3) . . . ? #-----------------END #=============================================================================== # If more than one structure is reported, sections 5-10 should be filled in # per structure. For each data set, replace the ? in the data_? line below # by a unique identifier. data_1d _database_code_CSD 176860 #=============================================================================== # 5. CHEMICAL DATA _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_formula_moiety 'C53 H30 Cl2 Mn2 N2 O6' _chemical_formula_structural ? _chemical_formula_analytical ? _chemical_formula_sum 'C53 H30 Cl2 Mn2 N2 O6' _chemical_formula_weight 971.62 _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 orthorhombic _symmetry_space_group_name_H-M 'P b c a' _symmetry_space_group_name_Hall '-P 2ac 2ab' loop_ _symmetry_equiv_pos_as_xyz 'x,y,z' 1/2-x,-y,1/2+z -x,1/2+y,1/2-z 1/2+x,1/2-y,-z -x,-y,-z 1/2+x,+y,1/2-z +x,1/2-y,1/2+z 1/2-x,1/2+y,+z _cell_length_a 14.8379(2) _cell_length_b 35.4532(3) _cell_length_c 16.3323(5) _cell_angle_alpha 90 _cell_angle_beta 90 _cell_angle_gamma 90 _cell_volume 8591.6(3) _cell_formula_units_Z 8 _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 'yellow' _exptl_crystal_size_max 0.16 _exptl_crystal_size_mid 0.13 _exptl_crystal_size_min 0.10 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.50 _exptl_crystal_density_method 'none' _exptl_crystal_F_000 3952 _exptl_absorpt_coefficient_mu 0.769 _exptl_absorpt_correction_type refdelf_(Walker_&_Stuart,_1983) _exptl_absorpt_correction_T_min 0.8063 _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 ; 19157 reflections were collected using program Collect ("Collect" Data collection software, Nonius B.V., 1998) The conditions were as follow : crystal to detector distance = 43. mm. Scan angle = 2.0 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 = 0.00 224 frames Set 2 Theta = -8.80 Kappa = -150.00 Phi = 0.00 41 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 19157 _diffrn_reflns_av_R_equivalents 0.040 _diffrn_reflns_av_sigmaI/netI 0.333 _diffrn_reflns_limit_h_min -19 _diffrn_reflns_limit_h_max 19 _diffrn_reflns_limit_k_min -21 _diffrn_reflns_limit_k_max 21 _diffrn_reflns_limit_l_min -45 _diffrn_reflns_limit_l_max 45 _diffrn_reflns_theta_min 2.5 _diffrn_reflns_theta_max 27.48 _reflns_number_total 10687 _reflns_number_gt 3614 _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 3614 _refine_ls_number_parameters 586 _refine_ls_number_restraints 0 _refine_ls_number_constraints 0 _refine_ls_R_factor_all 0.158 _refine_ls_R_factor_gt 0.051 _refine_ls_wR_factor_all 0.321 _refine_ls_wR_factor_ref 0.082 _refine_ls_goodness_of_fit_all 15.033 _refine_ls_goodness_of_fit_ref 1.415 _refine_ls_shift/su_max 0.017 _refine_ls_shift/esd_mean 0.001 _refine_diff_density_max 0.589 _refine_diff_density_min -0.203 #=============================================================================== # 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 1.13242(8) 0.10226(3) 0.49421(7) 0.0201(5) Uani ? ? Mn MN2 0.55251(8) 0.08461(3) 0.51944(7) 0.0196(5) Uani ? ? Mn C1 1.2370(5) 0.1006(2) 0.4352(4) 0.024(4) Uani ? ? C O1 1.3022(4) 0.0986(1) 0.3987(3) 0.037(3) Uani ? ? O C2 1.1858(6) 0.1238(2) 0.5789(5) 0.039(5) Uani ? ? C O2 1.2194(5) 0.1378(2) 0.6358(3) 0.071(4) Uani ? ? O C3 1.1507(5) 0.0571(2) 0.5371(5) 0.026(4) Uani ? ? C O3 1.1626(4) 0.0277(1) 0.5676(4) 0.044(4) Uani ? ? O C4 0.5151(5) 0.1112(2) 0.4302(5) 0.023(4) Uani ? ? C O4 0.4960(4) 0.1284(1) 0.3741(3) 0.037(3) Uani ? ? O C5 0.5484(5) 0.0436(2) 0.4580(4) 0.026(4) Uani ? ? C O5 0.5476(4) 0.0163(1) 0.4184(3) 0.037(3) Uani ? ? O C6 0.4409(5) 0.0758(2) 0.5549(5) 0.027(4) Uani ? ? C O6 0.3686(4) 0.0697(1) 0.5773(3) 0.039(3) Uani ? ? O C7 1.0329(5) 0.1478(2) 0.4913(4) 0.018(4) Uani ? ? C C8 1.0448(5) 0.1829(2) 0.5346(4) 0.024(4) Uani ? ? C C9 1.0870(6) 0.2112(2) 0.4955(5) 0.031(4) Uani ? ? C C10 1.1204(6) 0.2072(2) 0.4142(5) 0.033(5) Uani ? ? C C11 1.1139(5) 0.1750(2) 0.3731(5) 0.031(4) Uani ? ? C C12 1.0697(5) 0.1447(2) 0.4108(4) 0.017(4) Uani ? ? C C13 1.0515(5) 0.1070(2) 0.3813(4) 0.021(4) Uani ? ? C C14 0.9991(5) 0.0885(2) 0.4432(4) 0.019(4) Uani ? ? C C15 0.9912(5) 0.1118(2) 0.5138(4) 0.018(4) Uani ? ? C C16 1.0682(5) 0.0895(2) 0.3055(4) 0.024(4) Uani ? ? C C17 1.0359(6) 0.0543(2) 0.2927(5) 0.031(4) Uani ? ? C C18 0.9840(6) 0.0355(2) 0.3530(5) 0.031(5) Uani ? ? C C19 0.9657(5) 0.0507(2) 0.4266(4) 0.023(4) Uani ? ? C C20 0.9341(5) 0.1039(2) 0.5860(4) 0.020(4) Uani ? ? C C21 0.9433(5) 0.0687(2) 0.6265(4) 0.024(4) Uani ? ? C C22 0.8922(5) 0.0590(2) 0.6941(4) 0.026(4) Uani ? ? C C23 0.8305(5) 0.0847(2) 0.7260(4) 0.024(4) Uani ? ? C C24 0.8199(5) 0.1191(2) 0.6884(4) 0.021(4) Uani ? ? C C25 0.8680(5) 0.1291(2) 0.6168(4) 0.021(4) Uani ? ? C C26 0.8484(5) 0.1671(2) 0.5805(5) 0.019(4) Uani ? ? C N1 0.8608(4) 0.1950(1) 0.6342(3) 0.025(3) Uani ? ? N C27 0.8533(5) 0.2310(2) 0.6048(5) 0.026(4) Uani ? ? C C28 0.8326(5) 0.2375(2) 0.5220(5) 0.023(4) Uani ? ? C N2 0.8148(4) 0.2078(1) 0.4698(4) 0.023(3) Uani ? ? N C29 0.8214(5) 0.1735(2) 0.4979(4) 0.017(4) Uani ? ? C C30 0.8695(6) 0.2620(2) 0.6580(5) 0.034(5) Uani ? ? C C31 0.8691(6) 0.2974(2) 0.6296(5) 0.044(5) Uani ? ? C C32 0.8503(6) 0.3037(2) 0.5474(6) 0.032(5) Uani ? ? C C33 0.8321(6) 0.2744(2) 0.4930(5) 0.034(5) Uani ? ? C C34 0.8039(5) 0.1437(2) 0.4353(4) 0.018(4) Uani ? ? C C35 0.8498(5) 0.1478(2) 0.3608(4) 0.021(4) Uani ? ? C C36 0.8422(5) 0.1228(2) 0.2993(4) 0.024(4) Uani ? ? C C37 0.7876(6) 0.0923(2) 0.3078(4) 0.025(4) Uani ? ? C C38 0.7390(5) 0.0879(2) 0.3788(4) 0.025(4) Uani ? ? C C39 0.7449(5) 0.1123(2) 0.4447(4) 0.015(4) Uani ? ? C C40 0.6272(5) 0.0740(2) 0.6325(4) 0.024(4) Uani ? ? C C41 0.6145(6) 0.0438(2) 0.6883(5) 0.031(5) Uani ? ? C C42 0.6589(6) 0.0103(2) 0.6746(5) 0.032(5) Uani ? ? C C43 0.7170(6) 0.0065(2) 0.6072(5) 0.030(5) Uani ? ? C C44 0.7311(5) 0.0355(2) 0.5519(5) 0.026(4) Uani ? ? C C45 0.6868(5) 0.0704(2) 0.5645(4) 0.018(4) Uani ? ? C C46 0.6881(5) 0.1058(2) 0.5183(4) 0.014(4) Uani ? ? C C47 0.6345(5) 0.1326(2) 0.5642(4) 0.019(4) Uani ? ? C C48 0.5943(5) 0.1128(2) 0.6332(4) 0.019(4) Uani ? ? C C49 0.6099(5) 0.1708(2) 0.5501(5) 0.026(4) Uani ? ? C C50 0.5540(6) 0.1887(2) 0.6038(5) 0.031(5) Uani ? ? C C51 0.5173(6) 0.1698(2) 0.6719(5) 0.035(5) Uani ? ? C C52 0.5357(5) 0.1336(2) 0.6872(4) 0.028(5) Uani ? ? C C53 0.6998(6) 0.2283(2) 0.3042(5) 0.046(5) Uani ? ? C CL1 0.6855(2) 0.27600(6) 0.2841(2) 0.083(2) Uani ? ? Cl CL2 0.6010(2) 0.20618(8) 0.3354(2) 0.075(2) Uani ? ? Cl H1 1.0234 0.1859 0.5891 0.0317 Uiso calc C8 H H2 1.0949 0.2346 0.5229 0.0428 Uiso calc C9 H H3 1.1482 0.2282 0.3885 0.0451 Uiso calc C10 H H4 1.1385 0.1725 0.3196 0.0419 Uiso calc C11 H H5 1.1015 0.1022 0.2641 0.0330 Uiso calc C16 H H6 1.0483 0.0420 0.2423 0.0412 Uiso calc C17 H H7 0.9611 0.0111 0.3409 0.0403 Uiso calc C18 H H8 0.9320 0.0372 0.4665 0.0301 Uiso calc C19 H H9 0.9863 0.0512 0.6064 0.0316 Uiso calc C21 H H10 0.8992 0.0349 0.7186 0.0334 Uiso calc C22 H H11 0.7961 0.0785 0.7732 0.0338 Uiso calc C23 H H12 0.7789 0.1368 0.7113 0.0275 Uiso calc C24 H H13 0.8807 0.2575 0.7144 0.0448 Uiso calc C30 H H14 0.8815 0.3179 0.6651 0.0575 Uiso calc C31 H H15 0.8498 0.3289 0.5276 0.0614 Uiso calc C32 H H16 0.8196 0.2796 0.4371 0.0465 Uiso calc C33 H H17 0.8878 0.1691 0.3536 0.0285 Uiso calc C35 H H18 0.8750 0.1265 0.2500 0.0325 Uiso calc C36 H H19 0.7831 0.0742 0.2651 0.0341 Uiso calc C37 H H20 0.6993 0.0670 0.3829 0.0331 Uiso calc C38 H H21 0.5759 0.0467 0.7343 0.0408 Uiso calc C41 H H22 0.6503 -0.0104 0.7109 0.0425 Uiso calc C42 H H23 0.7477 -0.0167 0.5992 0.0427 Uiso calc C43 H H24 0.7698 0.0320 0.5062 0.0364 Uiso calc C44 H H25 0.6324 0.1838 0.5035 0.0339 Uiso calc C49 H H26 0.5394 0.2145 0.5951 0.0448 Uiso calc C50 H H27 0.4785 0.1832 0.7080 0.0463 Uiso calc C51 H H28 0.5101 0.1215 0.7337 0.0401 Uiso calc C52 H H29 0.7435 0.2256 0.3464 0.0603 Uiso calc C53 H H30 0.7209 0.2163 0.2559 0.0603 Uiso calc C53 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 0.0197(6) 0.0200(5) 0.0207(6) 0.0022(5) 0.0008(6) 0.0009(5) Mn MN2 0.0177(6) 0.0222(5) 0.0192(5) -0.0020(5) -0.0004(6) -0.0004(5) Mn C1 0.032(5) 0.015(3) 0.027(4) -0.000(4) -0.005(4) 0.006(3) C O1 0.024(3) 0.056(3) 0.036(3) -0.001(3) 0.012(3) -0.001(3) O C2 0.033(5) 0.044(4) 0.040(5) 0.021(4) -0.017(5) -0.003(4) C O2 0.095(5) 0.069(4) 0.054(4) 0.038(4) -0.048(4) -0.027(3) O C3 0.021(5) 0.023(4) 0.038(5) -0.001(4) 0.002(4) -0.004(3) C O3 0.031(4) 0.044(3) 0.063(4) 0.003(3) 0.005(4) 0.016(3) O C4 0.015(4) 0.021(3) 0.037(4) -0.008(3) 0.004(4) -0.012(3) C O4 0.043(4) 0.047(3) 0.025(3) 0.003(3) -0.012(3) 0.014(3) O C5 0.026(5) 0.024(4) 0.027(4) -0.007(4) 0.002(4) 0.005(3) C O5 0.048(4) 0.028(3) 0.038(3) -0.008(3) -0.000(3) -0.009(2) O C6 0.018(5) 0.043(4) 0.026(4) -0.007(4) -0.008(4) -0.002(4) C O6 0.024(3) 0.079(4) 0.032(3) -0.009(3) 0.000(3) -0.008(3) O C7 0.018(4) 0.011(3) 0.029(4) 0.006(3) -0.002(4) 0.007(3) C C8 0.019(4) 0.033(4) 0.021(4) 0.006(4) -0.000(4) -0.003(3) C C9 0.030(5) 0.019(3) 0.050(5) -0.004(4) -0.005(5) 0.004(4) C C10 0.032(5) 0.022(4) 0.050(5) -0.005(4) 0.007(5) 0.015(4) C C11 0.021(5) 0.042(4) 0.033(5) -0.005(4) 0.010(4) 0.013(4) C C12 0.019(4) 0.012(3) 0.024(4) 0.000(3) 0.004(4) 0.003(3) C C13 0.018(4) 0.025(4) 0.020(4) 0.012(3) 0.002(4) 0.007(3) C C14 0.020(4) 0.021(3) 0.016(4) 0.004(4) -0.001(4) 0.002(3) C C15 0.020(4) 0.022(3) 0.014(4) -0.001(3) 0.001(4) 0.002(3) C C16 0.029(5) 0.031(4) 0.016(4) 0.007(4) -0.001(4) -0.002(3) C C17 0.042(6) 0.030(4) 0.023(4) 0.012(4) 0.007(4) -0.003(3) C C18 0.030(5) 0.031(4) 0.031(5) 0.005(4) -0.011(5) -0.011(4) C C19 0.021(5) 0.025(4) 0.024(4) 0.001(4) -0.001(4) 0.001(3) C C20 0.018(4) 0.020(3) 0.022(4) 0.001(3) -0.003(4) 0.001(3) C C21 0.022(5) 0.033(4) 0.019(4) -0.001(4) -0.002(4) -0.002(3) C C22 0.029(5) 0.023(4) 0.025(4) -0.001(4) -0.004(4) 0.006(3) C C23 0.017(4) 0.043(4) 0.018(4) -0.006(4) -0.003(4) -0.000(4) C C24 0.018(4) 0.029(4) 0.017(4) 0.003(4) -0.003(4) -0.009(3) C C25 0.020(4) 0.025(3) 0.020(4) -0.005(4) -0.003(4) -0.005(3) C C26 0.009(4) 0.029(4) 0.026(4) 0.000(3) 0.005(4) 0.002(3) C N1 0.028(4) 0.027(3) 0.021(3) -0.003(3) -0.001(4) -0.006(3) N C27 0.019(5) 0.023(4) 0.039(5) 0.001(4) 0.010(4) 0.001(3) C C28 0.019(4) 0.016(3) 0.040(5) -0.002(3) 0.004(4) -0.003(3) C N2 0.022(4) 0.019(3) 0.031(4) 0.000(3) -0.002(3) 0.006(3) N C29 0.008(4) 0.024(3) 0.024(4) 0.003(3) 0.003(4) -0.001(3) C C30 0.035(5) 0.027(4) 0.041(5) -0.007(4) 0.009(5) -0.018(4) C C31 0.045(6) 0.036(4) 0.051(5) 0.001(5) 0.001(6) -0.014(4) C C32 0.031(5) 0.011(4) 0.100(7) -0.002(4) 0.015(6) -0.005(4) C C33 0.032(5) 0.024(4) 0.051(5) 0.002(4) 0.003(5) 0.004(4) C C34 0.019(4) 0.014(3) 0.023(4) 0.000(3) -0.007(4) 0.003(3) C C35 0.030(5) 0.021(3) 0.015(4) -0.001(4) 0.003(4) 0.010(3) C C36 0.027(5) 0.033(4) 0.015(4) -0.004(4) 0.002(4) 0.008(3) C C37 0.036(5) 0.028(4) 0.015(4) 0.008(4) 0.000(4) -0.003(3) C C38 0.027(5) 0.020(4) 0.030(4) -0.003(4) -0.002(4) -0.007(3) C C39 0.013(4) 0.020(3) 0.013(3) 0.004(3) 0.002(4) 0.000(3) C C40 0.021(4) 0.029(4) 0.023(4) -0.002(4) -0.001(4) 0.002(3) C C41 0.028(5) 0.040(4) 0.026(4) -0.004(4) 0.007(4) 0.008(4) C C42 0.035(5) 0.026(4) 0.037(5) -0.002(4) 0.001(5) 0.004(4) C C43 0.039(5) 0.017(4) 0.042(5) 0.010(4) 0.007(5) -0.001(4) C C44 0.016(4) 0.039(4) 0.029(4) 0.003(4) -0.001(4) -0.009(4) C C45 0.010(4) 0.026(4) 0.024(4) -0.002(3) -0.000(4) -0.006(3) C C46 0.015(4) 0.009(3) 0.020(4) -0.005(3) -0.004(4) -0.002(3) C C47 0.011(4) 0.031(4) 0.020(4) 0.001(4) -0.002(4) -0.003(3) C C48 0.022(4) 0.015(3) 0.019(4) -0.001(3) 0.003(4) -0.000(3) C C49 0.021(5) 0.030(4) 0.027(4) -0.000(4) -0.001(4) 0.003(4) C C50 0.034(5) 0.017(4) 0.052(5) -0.000(4) 0.012(5) 0.005(4) C C51 0.026(5) 0.034(4) 0.047(5) 0.005(4) 0.005(5) -0.009(4) C C52 0.016(5) 0.050(5) 0.026(4) -0.007(4) 0.011(4) -0.001(4) C C53 0.046(6) 0.057(5) 0.035(5) -0.017(5) -0.001(5) 0.005(4) C CL1 0.130(3) 0.062(1) 0.071(2) 0.030(2) 0.028(2) 0.018(1) Cl CL2 0.074(2) 0.128(2) 0.044(2) -0.048(2) 0.015(2) -0.011(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 1.83(1) . . ? MN1 C2 1.77(1) . . ? MN1 C3 1.768(9) . . ? MN1 C7 2.190(7) . . ? MN1 C15 2.147(8) . . ? MN2 C4 1.821(9) . . ? MN2 C5 1.768(8) . . ? MN2 C6 1.781(9) . . ? MN2 C40 2.185(8) . . ? MN2 C45 2.183(8) . . ? MN2 C46 2.148(8) . . ? MN2 C48 2.199(7) . . ? C1 O1 1.139(9) . . ? C2 O2 1.17(1) . . ? C3 O3 1.169(9) . . ? C4 O4 1.138(9) . . ? C5 O5 1.163(9) . . ? C6 O6 1.15(1) . . ? C7 C8 1.44(1) . . ? C7 C12 1.43(1) . . ? C7 C15 1.47(1) . . ? C8 C9 1.34(1) . . ? C9 C10 1.42(1) . . ? C10 C11 1.33(1) . . ? C11 C12 1.40(1) . . ? C12 C13 1.45(1) . . ? C13 C14 1.43(1) . . ? C13 C16 1.41(1) . . ? C14 C15 1.42(1) . . ? C14 C19 1.46(1) . . ? C15 C20 1.48(1) . . ? C16 C17 1.35(1) . . ? C17 C18 1.42(1) . . ? C18 C19 1.35(1) . . ? C20 C21 1.42(1) . . ? C20 C25 1.42(1) . . ? C21 C22 1.38(1) . . ? C22 C23 1.39(1) . . ? C23 C24 1.38(1) . . ? C24 C25 1.41(1) . . ? C25 C26 1.50(1) . . ? C26 N1 1.334(9) . . ? C26 C29 1.42(1) . . ? N1 C27 1.370(9) . . ? C27 C28 1.41(1) . . ? C27 C30 1.42(1) . . ? C28 N2 1.38(1) . . ? C28 C33 1.39(1) . . ? N2 C29 1.307(9) . . ? C29 C34 1.49(1) . . ? C30 C31 1.34(1) . . ? C31 C32 1.39(1) . . ? C32 C33 1.39(1) . . ? C34 C35 1.40(1) . . ? C34 C39 1.42(1) . . ? C35 C36 1.34(1) . . ? C36 C37 1.36(1) . . ? C37 C38 1.37(1) . . ? C38 C39 1.38(1) . . ? C39 C46 1.49(1) . . ? C40 C41 1.42(1) . . ? C40 C45 1.43(1) . . ? C40 C48 1.46(1) . . ? C41 C42 1.38(1) . . ? C42 C43 1.41(1) . . ? C43 C44 1.38(1) . . ? C44 C45 1.42(1) . . ? C45 C46 1.47(1) . . ? C46 C47 1.45(1) . . ? C47 C48 1.46(1) . . ? C47 C49 1.42(1) . . ? C48 C52 1.44(1) . . ? C49 C50 1.36(1) . . ? C50 C51 1.41(1) . . ? C51 C52 1.34(1) . . ? C53 CL1 1.736(9) . . ? C53 CL2 1.74(1) . . ? 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 92.7(4) . . . ? C1 MN1 C3 92.9(4) . . . ? C1 MN1 C7 125.8(3) . . . ? C1 MN1 C15 155.8(3) . . . ? C2 MN1 C3 90.7(4) . . . ? C2 MN1 C7 90.0(3) . . . ? C2 MN1 C15 104.6(4) . . . ? C3 MN1 C7 141.3(3) . . . ? C3 MN1 C15 103.5(3) . . . ? C7 MN1 C15 39.5(3) . . . ? C4 MN2 C5 87.7(3) . . . ? C4 MN2 C6 93.9(4) . . . ? C4 MN2 C40 156.8(3) . . . ? C4 MN2 C45 131.9(3) . . . ? C4 MN2 C46 95.6(3) . . . ? C4 MN2 C48 121.8(3) . . . ? C5 MN2 C6 90.4(4) . . . ? C5 MN2 C40 110.8(3) . . . ? C5 MN2 C45 91.9(3) . . . ? C5 MN2 C46 108.4(3) . . . ? C5 MN2 C48 149.7(3) . . . ? C6 MN2 C40 99.6(3) . . . ? C6 MN2 C45 134.3(3) . . . ? C6 MN2 C46 159.2(3) . . . ? C6 MN2 C48 93.9(3) . . . ? C40 MN2 C45 38.1(3) . . . ? C40 MN2 C46 65.9(3) . . . ? C40 MN2 C48 38.9(3) . . . ? C45 MN2 C46 39.6(3) . . . ? C45 MN2 C48 64.1(3) . . . ? C46 MN2 C48 65.4(3) . . . ? MN1 C1 O1 178.3(7) . . . ? MN1 C2 O2 178(1) . . . ? MN1 C3 O3 178.1(8) . . . ? MN2 C4 O4 176.6(7) . . . ? MN2 C5 O5 178.4(8) . . . ? MN2 C6 O6 179.3(8) . . . ? MN1 C7 C8 122.9(6) . . . ? MN1 C7 C12 72.8(4) . . . ? MN1 C7 C15 68.7(4) . . . ? C8 C7 C12 118.2(7) . . . ? C8 C7 C15 132.8(7) . . . ? C12 C7 C15 108.9(6) . . . ? C7 C8 C9 117.8(7) . . . ? C8 C9 C10 122.0(8) . . . ? C9 C10 C11 122.2(7) . . . ? C10 C11 C12 118.0(8) . . . ? C7 C12 C11 121.6(7) . . . ? C7 C12 C13 107.9(6) . . . ? C11 C12 C13 130.5(8) . . . ? C12 C13 C14 106.8(7) . . . ? C12 C13 C16 131.9(7) . . . ? C14 C13 C16 121.0(7) . . . ? C13 C14 C15 110.5(6) . . . ? C13 C14 C19 118.3(7) . . . ? C15 C14 C19 131.1(7) . . . ? MN1 C15 C7 71.8(4) . . . ? MN1 C15 C14 73.0(5) . . . ? MN1 C15 C20 130.4(5) . . . ? C7 C15 C14 105.5(6) . . . ? C7 C15 C20 127.4(6) . . . ? C14 C15 C20 125.7(7) . . . ? C13 C16 C17 118.7(8) . . . ? C16 C17 C18 121.3(7) . . . ? C17 C18 C19 122.8(7) . . . ? C14 C19 C18 117.8(8) . . . ? C15 C20 C21 118.9(7) . . . ? C15 C20 C25 124.0(6) . . . ? C21 C20 C25 117.0(7) . . . ? C20 C21 C22 122.6(7) . . . ? C21 C22 C23 119.7(7) . . . ? C22 C23 C24 119.2(7) . . . ? C23 C24 C25 122.2(7) . . . ? C20 C25 C24 119.0(7) . . . ? C20 C25 C26 123.9(7) . . . ? C24 C25 C26 117.0(7) . . . ? C25 C26 N1 112.2(7) . . . ? C25 C26 C29 124.8(7) . . . ? N1 C26 C29 122.9(7) . . . ? C26 N1 C27 116.8(7) . . . ? N1 C27 C28 120.3(7) . . . ? N1 C27 C30 119.6(8) . . . ? C28 C27 C30 120.0(7) . . . ? C27 C28 N2 120.9(7) . . . ? C27 C28 C33 118.7(7) . . . ? N2 C28 C33 120.4(8) . . . ? C28 N2 C29 118.7(7) . . . ? C26 C29 N2 120.1(7) . . . ? C26 C29 C34 125.8(7) . . . ? N2 C29 C34 114.0(7) . . . ? C27 C30 C31 120.8(9) . . . ? C30 C31 C32 119.2(8) . . . ? C31 C32 C33 122.3(8) . . . ? C28 C33 C32 119.0(9) . . . ? C29 C34 C35 115.7(6) . . . ? C29 C34 C39 125.9(7) . . . ? C35 C34 C39 118.3(7) . . . ? C34 C35 C36 122.6(7) . . . ? C35 C36 C37 119.9(7) . . . ? C36 C37 C38 119.2(7) . . . ? C37 C38 C39 123.6(7) . . . ? C34 C39 C38 116.3(7) . . . ? C34 C39 C46 123.7(6) . . . ? C38 C39 C46 119.9(7) . . . ? MN2 C40 C41 127.2(6) . . . ? MN2 C40 C45 70.8(4) . . . ? MN2 C40 C48 71.1(4) . . . ? C41 C40 C45 121.0(7) . . . ? C41 C40 C48 131.4(8) . . . ? C45 C40 C48 107.5(6) . . . ? C40 C41 C42 119.0(8) . . . ? C41 C42 C43 120.1(7) . . . ? C42 C43 C44 122.3(7) . . . ? C43 C44 C45 119.0(8) . . . ? MN2 C45 C40 71.1(5) . . . ? MN2 C45 C44 125.2(6) . . . ? MN2 C45 C46 68.9(4) . . . ? C40 C45 C44 118.7(7) . . . ? C40 C45 C46 109.3(6) . . . ? C44 C45 C46 131.9(7) . . . ? MN2 C46 C39 126.3(5) . . . ? MN2 C46 C45 71.5(4) . . . ? MN2 C46 C47 73.2(4) . . . ? C39 C46 C45 123.7(6) . . . ? C39 C46 C47 129.0(6) . . . ? C45 C46 C47 106.8(6) . . . ? C46 C47 C48 108.0(6) . . . ? C46 C47 C49 133.0(7) . . . ? C48 C47 C49 118.7(7) . . . ? MN2 C48 C40 70.1(4) . . . ? MN2 C48 C47 71.4(4) . . . ? MN2 C48 C52 125.4(6) . . . ? C40 C48 C47 108.1(7) . . . ? C40 C48 C52 133.5(7) . . . ? C47 C48 C52 118.3(7) . . . ? C47 C49 C50 119.7(7) . . . ? C49 C50 C51 121.5(7) . . . ? C50 C51 C52 121.8(8) . . . ? C48 C52 C51 120.0(7) . . . ? CL1 C53 CL2 113.1(6) . . . ? #-----------------END #=============================================================================== # If more than one structure is reported, sections 5-10 should be filled in # per structure. For each data set, replace the ? in the data_? line below # by a unique identifier. data_1e _database_code_CSD 176861 #=============================================================================== # 5. CHEMICAL DATA _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_formula_moiety 'C55 H39 Ag B F4 Mn2 N2 O9' _chemical_formula_structural ? _chemical_formula_analytical ? _chemical_formula_sum 'C55 H39 Ag B F4 Mn2 N2 O9' _chemical_formula_weight 1176.48 _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 Ag ? -1.085 1.101 International_Tables_Vol_IV_Table_2.3.1 B ? 0.000 0.001 International_Tables_Vol_IV_Table_2.3.1 F ? 0.014 0.010 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 orthorhombic _symmetry_space_group_name_H-M 'P 21 21 21' _symmetry_space_group_name_Hall ' P 2ac 2ab' loop_ _symmetry_equiv_pos_as_xyz 'x,y,z' 1/2-x,-y,1/2+z -x,1/2+y,1/2-z 1/2+x,1/2-y,-z _cell_length_a 13.6186(5) _cell_length_b 15.1375(7) _cell_length_c 25.032(1) _cell_angle_alpha 90 _cell_angle_beta 90 _cell_angle_gamma 90 _cell_volume 5160.5(4) _cell_formula_units_Z 4 _cell_measurement_temperature 173 _cell_measurement_reflns_used 11811 _cell_measurement_theta_min 1.4 _cell_measurement_theta_max 27.5 _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 0.12 _exptl_crystal_size_mid 0.10 _exptl_crystal_size_min 0.08 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.51 _exptl_crystal_density_method 'none' _exptl_crystal_F_000 2372 _exptl_absorpt_coefficient_mu 0.930 _exptl_absorpt_correction_type refdelf_(Walker_&_Stuart,_1983) _exptl_absorpt_correction_T_min 0.8920 _exptl_absorpt_correction_T_max 0.928 #=============================================================================== # 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 ; 11811 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 = 0.4 deg 1 scans of 90 sec per frame. Data collection was divided into 2 set(s) with the following starting angles and number of frames : Set 1 Theta = 6.30 Omega = 0.00 Kappa = 0.00 598 frames Set 2 Theta = -6.30 Kappa = 139.00 Phi = 0.00 153 frames Friedel pairs were not averaged. Internal R = 0.07 ; _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% 0 _diffrn_reflns_number 11811 _diffrn_reflns_av_R_equivalents 0.070 _diffrn_reflns_av_sigmaI/netI 0.333 _diffrn_reflns_limit_h_min -17 _diffrn_reflns_limit_h_max 17 _diffrn_reflns_limit_k_min -19 _diffrn_reflns_limit_k_max 19 _diffrn_reflns_limit_l_min -32 _diffrn_reflns_limit_l_max 32 _diffrn_reflns_theta_min 2.5 _diffrn_reflns_theta_max 27.48 _reflns_number_total 6521 _reflns_number_gt 3656 _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 0.03(5) _refine_ls_number_reflns 3656 _refine_ls_number_parameters 634 _refine_ls_number_restraints 0 _refine_ls_number_constraints 0 _refine_ls_abs_structure_details 'Flack H D (1983), Acta Cryst. A39, 876-881' _refine_ls_R_factor_all 0.113 _refine_ls_R_factor_gt 0.058 _refine_ls_wR_factor_all 0.897 _refine_ls_wR_factor_ref 0.080 _refine_ls_goodness_of_fit_all 22.454 _refine_ls_goodness_of_fit_ref 1.513 _refine_ls_shift/su_max 0.010 _refine_ls_shift/esd_mean 0.002 _refine_diff_density_max 0.959 _refine_diff_density_min -0.213 #=============================================================================== # 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 AG 0.84699(6) 0.29846(6) 0.45854(3) 0.0347(4) 1.000 Uani ? ? Ag MN1 0.7833(1) -0.1075(1) 0.51419(6) 0.0357(8) 1.000 Uani ? ? Mn MN2 0.4117(1) 0.1737(1) 0.29627(6) 0.0353(8) 1.000 Uani ? ? Mn C1 0.8275(9) -0.1896(8) 0.4711(5) 0.051(7) 1.000 Uani ? ? C O1 0.8518(7) -0.2439(7) 0.4402(3) 0.087(6) 1.000 Uani ? ? O C2 0.8963(8) -0.0483(7) 0.5111(4) 0.037(6) 1.000 Uani ? ? C O2 0.9692(6) -0.0091(6) 0.5080(3) 0.058(5) 1.000 Uani ? ? O C3 0.827(1) -0.1716(9) 0.5724(4) 0.057(7) 1.000 Uani ? ? C O3 0.8545(6) -0.2095(6) 0.6076(3) 0.065(5) 1.000 Uani ? ? O C4 0.2957(9) 0.1952(8) 0.3277(4) 0.045(6) 1.000 Uani ? ? C O4 0.7228(6) 0.2913(6) 0.6500(3) 0.062(5) 1.000 Uani ? ? O C5 0.3819(8) 0.2382(9) 0.2410(4) 0.046(6) 1.000 Uani ? ? C O5 0.8634(8) 0.2141(6) 0.7967(3) 0.078(6) 1.000 Uani ? ? O C6 0.3592(8) 0.0799(8) 0.2662(4) 0.043(6) 1.000 Uani ? ? C O6 0.8237(7) 0.4836(6) 0.7527(3) 0.073(6) 1.000 Uani ? ? O C7 0.7275(7) 0.0492(7) 0.4310(4) 0.033(5) 1.000 Uani ? ? C C8 0.7840(7) 0.0126(8) 0.3881(4) 0.037(6) 1.000 Uani ? ? C C9 0.8126(9) 0.0588(9) 0.3445(4) 0.049(7) 1.000 Uani ? ? C C10 0.7894(8) 0.1476(8) 0.3410(4) 0.046(6) 1.000 Uani ? ? C C11 0.7360(7) 0.1871(7) 0.3815(4) 0.031(5) 1.000 Uani ? ? C C12 0.7024(7) 0.1410(7) 0.4265(3) 0.027(5) 1.000 Uani ? ? C C13 0.6477(7) 0.1913(7) 0.4646(3) 0.034(5) 1.000 Uani ? ? C N1 0.6927(6) 0.2639(6) 0.4830(3) 0.031(4) 1.000 Uani ? ? N C14 0.6458(6) 0.3168(7) 0.5193(4) 0.025(5) 1.000 Uani ? ? C C15 0.6916(8) 0.3939(8) 0.5392(4) 0.046(6) 1.000 Uani ? ? C C16 0.6472(8) 0.4462(7) 0.5763(4) 0.036(6) 1.000 Uani ? ? C C17 0.5534(8) 0.4220(8) 0.5949(4) 0.042(6) 1.000 Uani ? ? C C18 0.5092(8) 0.3493(8) 0.5785(4) 0.039(6) 1.000 Uani ? ? C C19 0.5511(7) 0.2940(6) 0.5381(3) 0.027(5) 1.000 Uani ? ? C N2 1.0063(5) 0.2765(6) 0.4832(3) 0.029(4) 1.000 Uani ? ? N C20 0.5494(7) 0.1721(7) 0.4814(3) 0.026(5) 1.000 Uani ? ? C C21 0.4918(6) 0.0945(7) 0.4639(4) 0.027(5) 1.000 Uani ? ? C C22 0.4593(7) 0.0390(7) 0.5048(4) 0.028(5) 1.000 Uani ? ? C C23 0.4051(8) -0.0384(7) 0.4930(4) 0.042(6) 1.000 Uani ? ? C C24 0.3828(8) -0.0571(7) 0.4412(5) 0.040(6) 1.000 Uani ? ? C C25 0.4106(8) -0.0003(7) 0.4008(4) 0.037(6) 1.000 Uani ? ? C C26 0.4660(7) 0.0767(7) 0.4117(4) 0.027(5) 1.000 Uani ? ? C O7 0.8428(9) 0.3850(7) 0.3819(3) 0.094(7) 1.000 Uani ? ? O C27 0.910(2) 0.374(1) 0.3332(7) 0.14(2) 1.000 Uani ? ? C C28 0.6961(7) -0.0098(7) 0.4743(4) 0.030(5) 1.000 Uani ? ? C C29 0.6492(7) -0.0944(7) 0.4667(3) 0.035(5) 1.000 Uani ? ? C C30 0.6232(8) -0.1418(8) 0.4193(4) 0.042(6) 1.000 Uani ? ? C C31 0.5817(9) -0.2212(9) 0.4236(4) 0.053(7) 1.000 Uani ? ? C C32 1.060(1) 0.7598(9) 0.5259(5) 0.062(8) 1.000 Uani ? ? C C33 0.5806(9) -0.2155(8) 0.5193(4) 0.054(7) 1.000 Uani ? ? C C34 0.6249(7) -0.1320(7) 0.5160(4) 0.038(6) 1.000 Uani ? ? C C35 0.6493(8) -0.0653(8) 0.5576(4) 0.040(6) 1.000 Uani ? ? C C36 0.6334(9) -0.0668(9) 0.6136(4) 0.051(7) 1.000 Uani ? ? C C37 0.659(1) 0.0045(9) 0.6407(4) 0.053(7) 1.000 Uani ? ? C C38 0.705(1) 0.0787(9) 0.6188(4) 0.052(7) 1.000 Uani ? ? C C39 0.7238(8) 0.0832(7) 0.5632(4) 0.041(6) 1.000 Uani ? ? C C40 0.6916(7) 0.0083(7) 0.5309(4) 0.030(5) 1.000 Uani ? ? C C41 0.4936(7) 0.1309(7) 0.3667(4) 0.029(5) 1.000 Uani ? ? C C42 0.4984(8) 0.2275(7) 0.3643(4) 0.037(6) 1.000 Uani ? ? C C43 0.4631(8) 0.2946(7) 0.3969(4) 0.038(6) 1.000 Uani ? ? C C44 0.478(1) 0.3802(8) 0.3856(4) 0.050(7) 1.000 Uani ? ? C C45 0.5291(9) 0.4072(9) 0.3391(5) 0.061(8) 1.000 Uani ? ? C C46 0.560(1) 0.3448(9) 0.3004(4) 0.056(7) 1.000 Uani ? ? C C47 0.5439(7) 0.2513(8) 0.3122(4) 0.038(6) 1.000 Uani ? ? C C48 0.5697(9) 0.1734(7) 0.2823(4) 0.043(6) 1.000 Uani ? ? C C49 0.6191(8) 0.1612(9) 0.2364(4) 0.050(7) 1.000 Uani ? ? C C50 0.641(1) 0.078(1) 0.2207(4) 0.062(8) 1.000 Uani ? ? C C51 0.617(1) 0.0026(9) 0.2521(4) 0.058(7) 1.000 Uani ? ? C C52 0.5678(8) 0.0118(8) 0.2998(4) 0.042(6) 1.000 Uani ? ? C C53 0.5437(7) 0.0993(8) 0.3168(4) 0.037(6) 1.000 Uani ? ? C C54 0.931(2) -0.380(2) 0.2690(9) 0.18(1) 1.000 Uiso ? ? C O8 0.869(2) -0.332(1) 0.3134(7) 0.211(8) 1.000 Uiso ? ? O C55 0.297(2) 0.071(2) 0.1012(9) 0.17(1) 1.000 Uiso ? ? C O9 0.191(1) 0.053(1) 0.1221(6) 0.154(5) 1.000 Uiso ? ? O B1 0.324(2) 0.154(2) 0.8209(8) 0.111(7) 1.000 Uiso ? ? B F1 0.338(3) 0.242(2) 0.820(1) 0.20(1) 0.500 Uiso ? ? F F2 0.391(1) 0.0834(9) 0.8104(5) 0.153(4) 1.000 Uiso ? ? F F3 0.217(2) 0.139(2) 0.8197(8) 0.131(7) 0.500 Uiso ? ? F F4 0.328(2) 0.167(1) 0.8739(7) 0.111(6) 0.500 Uiso ? ? F F1a 0.320(2) 0.201(1) 0.7796(7) 0.110(6) 0.500 Uiso ? ? F F3A 0.265(2) 0.121(2) 0.8510(7) 0.123(7) 0.500 Uiso ? ? F F4a 0.404(2) 0.221(2) 0.8490(9) 0.151(9) 0.500 Uiso ? ? F H1 0.8025 -0.0478 0.3904 0.0507 1.000 Uiso calc C8 H H2 0.8482 0.0307 0.3167 0.0654 1.000 Uiso calc C9 H H3 0.8100 0.1812 0.3110 0.0606 1.000 Uiso calc C10 H H4 0.7214 0.2483 0.3787 0.0444 1.000 Uiso calc C11 H H5 0.7548 0.4097 0.5263 0.0603 1.000 Uiso calc C15 H H6 0.6787 0.4978 0.5892 0.0506 1.000 Uiso calc C16 H H7 0.5211 0.4589 0.6201 0.0560 1.000 Uiso calc C17 H H8 0.4480 0.3332 0.5938 0.0525 1.000 Uiso calc C18 H H9 0.4737 0.0533 0.5409 0.0425 1.000 Uiso calc C22 H H10 0.3846 -0.0768 0.5209 0.0555 1.000 Uiso calc C23 H H11 0.3480 -0.1097 0.4327 0.0603 1.000 Uiso calc C24 H H12 0.3921 -0.0131 0.3650 0.0484 1.000 Uiso calc C25 H H13 0.6354 -0.1169 0.3851 0.0555 1.000 Uiso calc C30 H H14 0.5661 -0.2529 0.3920 0.0728 1.000 Uiso calc C31 H H15 0.5309 -0.3168 0.4759 0.0805 1.000 Uiso calc ? H H16 0.5655 -0.2405 0.5531 0.0711 1.000 Uiso calc C33 H H17 0.6056 -0.1168 0.6308 0.0687 1.000 Uiso calc C36 H H18 0.6457 0.0052 0.6780 0.0740 1.000 Uiso calc C37 H H19 0.7229 0.1265 0.6413 0.0780 1.000 Uiso calc C38 H H20 0.7561 0.1326 0.5477 0.0535 1.000 Uiso calc C39 H H21 0.4274 0.2795 0.4282 0.0501 1.000 Uiso calc C43 H H22 0.4538 0.4239 0.4094 0.0664 1.000 Uiso calc C44 H H23 0.5425 0.4681 0.3337 0.0870 1.000 Uiso calc C45 H H24 0.5908 0.3630 0.2681 0.0725 1.000 Uiso calc C46 H H25 0.6383 0.2103 0.2153 0.0679 1.000 Uiso calc C49 H H26 0.6737 0.0693 0.1876 0.0875 1.000 Uiso calc C50 H H27 0.6358 -0.0546 0.2400 0.0790 1.000 Uiso calc C51 H H28 0.5504 -0.0382 0.3207 0.0578 1.000 Uiso calc C52 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 AG 0.0195(3) 0.0449(4) 0.0478(4) -0.0001(4) -0.0006(4) 0.0004(4) Ag MN1 0.0287(8) 0.0365(9) 0.0432(8) 0.0045(9) -0.0049(8) -0.0031(8) Mn MN2 0.0302(8) 0.0420(9) 0.0347(7) -0.0001(9) -0.0050(7) -0.0017(8) Mn C1 0.042(7) 0.042(7) 0.075(7) 0.011(6) -0.007(6) -0.004(6) C O1 0.090(6) 0.094(6) 0.078(5) 0.050(6) -0.036(5) -0.044(5) O C2 0.031(5) 0.032(6) 0.053(6) 0.006(5) -0.007(5) -0.003(5) C O2 0.046(5) 0.059(5) 0.071(5) -0.007(5) 0.002(4) -0.001(5) O C3 0.063(8) 0.055(8) 0.053(6) 0.005(8) 0.002(6) -0.003(6) C O3 0.068(5) 0.085(6) 0.048(4) 0.031(6) -0.009(4) 0.025(4) O C4 0.046(6) 0.040(7) 0.048(5) 0.001(7) -0.017(5) 0.006(6) C O4 0.041(4) 0.072(6) 0.080(5) 0.001(5) -0.015(4) -0.004(5) O C5 0.032(6) 0.068(8) 0.044(6) -0.005(6) 0.000(5) -0.014(6) C O5 0.116(8) 0.071(6) 0.058(4) -0.001(7) 0.017(5) 0.041(4) O C6 0.029(5) 0.063(8) 0.045(5) 0.016(6) -0.006(5) -0.010(6) C O6 0.055(5) 0.076(6) 0.093(6) -0.015(5) 0.014(5) -0.043(5) O C7 0.025(5) 0.047(7) 0.029(5) -0.005(6) -0.002(5) -0.000(5) C C8 0.023(5) 0.057(7) 0.037(5) 0.010(6) 0.006(5) -0.000(6) C C9 0.035(6) 0.064(8) 0.052(6) -0.008(7) 0.003(5) -0.015(6) C C10 0.037(6) 0.060(8) 0.043(6) -0.008(7) 0.003(5) -0.000(6) C C11 0.016(4) 0.043(7) 0.043(5) -0.007(5) -0.002(4) -0.003(6) C C12 0.016(4) 0.047(7) 0.025(5) 0.001(5) -0.005(4) 0.002(5) C C13 0.032(5) 0.032(6) 0.038(5) -0.003(6) -0.005(5) 0.006(5) C N1 0.021(4) 0.034(5) 0.044(4) 0.001(4) 0.001(4) 0.001(4) N C14 0.009(4) 0.040(6) 0.045(5) 0.004(5) -0.001(4) -0.001(5) C C15 0.037(6) 0.047(7) 0.055(6) -0.006(6) 0.002(6) -0.004(6) C C16 0.027(5) 0.029(6) 0.061(6) 0.006(6) -0.007(6) -0.005(5) C C17 0.032(6) 0.056(7) 0.041(5) 0.013(6) 0.007(5) 0.000(6) C C18 0.028(5) 0.045(7) 0.048(6) 0.002(6) -0.007(5) -0.007(6) C C19 0.019(4) 0.025(5) 0.039(5) -0.002(5) -0.004(4) 0.000(5) C N2 0.020(4) 0.051(6) 0.024(4) -0.007(4) -0.002(3) -0.004(4) N C20 0.022(5) 0.036(6) 0.023(4) 0.002(5) -0.002(4) 0.003(5) C C21 0.015(4) 0.038(6) 0.033(5) 0.001(5) 0.011(4) 0.002(5) C C22 0.012(4) 0.037(6) 0.049(6) -0.003(5) -0.001(5) 0.006(5) C C23 0.047(6) 0.036(6) 0.045(6) -0.004(6) -0.005(6) 0.015(5) C C24 0.031(6) 0.024(6) 0.084(7) 0.005(5) -0.013(6) -0.005(6) C C25 0.032(6) 0.042(6) 0.038(5) -0.004(6) -0.003(5) 0.002(5) C C26 0.016(4) 0.033(6) 0.039(5) 0.008(5) 0.005(4) -0.004(5) C O7 0.113(8) 0.111(7) 0.066(5) -0.042(8) -0.018(6) 0.039(5) O C27 0.21(2) 0.09(1) 0.15(1) -0.01(2) 0.09(1) -0.03(1) C C28 0.016(4) 0.041(6) 0.042(5) 0.009(5) -0.009(4) -0.004(5) C C29 0.032(5) 0.045(6) 0.030(5) 0.024(6) 0.002(5) -0.002(5) C C30 0.037(6) 0.037(7) 0.054(6) -0.005(6) -0.005(5) -0.001(6) C C31 0.035(6) 0.08(1) 0.050(6) -0.003(8) 0.002(6) 0.001(7) C C32 0.059(8) 0.058(8) 0.068(7) 0.022(8) 0.009(7) -0.000(7) C C33 0.051(7) 0.052(8) 0.061(6) -0.003(7) -0.003(6) 0.014(6) C C34 0.026(5) 0.037(6) 0.058(6) -0.001(5) -0.003(5) 0.017(6) C C35 0.028(5) 0.049(7) 0.047(5) 0.009(6) -0.007(5) -0.005(5) C C36 0.055(7) 0.068(8) 0.036(5) 0.008(7) 0.003(6) 0.006(6) C C37 0.078(9) 0.063(8) 0.030(5) 0.001(9) 0.005(6) 0.002(6) C C38 0.080(9) 0.077(9) 0.023(5) 0.017(9) -0.000(6) -0.006(6) C C39 0.036(6) 0.039(6) 0.048(6) 0.010(6) -0.009(5) -0.005(5) C C40 0.023(5) 0.034(6) 0.035(5) 0.010(5) 0.005(4) 0.006(5) C C41 0.019(5) 0.023(6) 0.058(6) -0.001(5) -0.005(5) -0.005(5) C C42 0.042(6) 0.027(6) 0.046(6) -0.004(6) -0.017(5) 0.000(5) C C43 0.041(6) 0.038(6) 0.037(5) 0.009(6) -0.004(5) -0.005(6) C C44 0.065(8) 0.046(7) 0.042(6) 0.002(7) -0.007(6) -0.001(6) C C45 0.051(7) 0.040(8) 0.110(9) 0.003(7) -0.043(7) -0.007(8) C C46 0.050(7) 0.060(8) 0.057(6) 0.002(7) 0.004(6) 0.013(7) C C47 0.021(5) 0.054(7) 0.046(6) -0.002(6) -0.005(5) 0.007(6) C C48 0.040(6) 0.042(7) 0.046(6) -0.004(6) -0.006(5) 0.012(6) C C49 0.042(6) 0.073(9) 0.041(6) -0.011(7) 0.011(5) -0.002(6) C C50 0.048(7) 0.11(1) 0.047(6) -0.004(9) 0.009(6) 0.000(8) C C51 0.061(8) 0.083(9) 0.039(6) 0.023(8) 0.006(6) -0.025(7) C C52 0.026(5) 0.043(6) 0.065(6) 0.014(6) -0.009(6) 0.006(6) C C53 0.025(5) 0.054(7) 0.038(5) 0.007(6) -0.003(5) -0.004(6) 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 AG N1 2.251(9) . . ? AG N2 2.281(9) . . ? AG O7 2.32(1) . . ? MN1 C1 1.75(1) . . ? MN1 C2 1.78(1) . . ? MN1 C3 1.85(2) . . ? MN1 C28 2.14(1) . . ? MN1 C29 2.19(1) . . ? MN1 C34 2.19(1) . . ? MN1 C35 2.22(1) . . ? MN1 C40 2.19(1) . . ? MN2 C4 1.79(1) . . ? MN2 C5 1.74(2) . . ? MN2 C6 1.76(2) . . ? MN2 C41 2.19(1) . . ? MN2 C42 2.23(1) . . ? MN2 C47 2.19(1) . . ? MN2 C48 2.18(1) . . ? MN2 C53 2.18(1) . . ? C1 O1 1.18(2) . . ? C2 O2 1.16(1) . . ? C3 O3 1.12(2) . . ? C4 O4 1.16(2) . 4_456 ? C5 O5 1.21(2) . 4_456 ? C6 O6 1.18(2) . 4_456 ? C7 C8 1.43(2) . . ? C7 C12 1.44(2) . . ? C7 C28 1.47(2) . . ? C8 C9 1.35(2) . . ? C9 C10 1.38(2) . . ? C10 C11 1.38(2) . . ? C11 C12 1.40(2) . . ? C12 C13 1.43(2) . . ? C13 N1 1.34(1) . . ? C13 C20 1.43(2) . . ? N1 C14 1.37(1) . . ? C14 C15 1.41(2) . . ? C14 C19 1.41(1) . . ? C15 C16 1.36(2) . . ? C16 C17 1.41(2) . . ? C17 C18 1.32(2) . . ? C18 C19 1.43(2) . . ? C19 N2 1.34(1) . 4_456 ? N2 C20 1.32(1) . 4_556 ? C20 C21 1.48(2) . . ? C21 C22 1.40(2) . . ? C21 C26 1.38(2) . . ? C22 C23 1.42(2) . . ? C23 C24 1.36(2) . . ? C24 C25 1.38(2) . . ? C25 C26 1.42(2) . . ? C26 C41 1.44(2) . . ? O7 C27 1.54(3) . . ? C28 C29 1.44(2) . . ? C28 C40 1.45(2) . . ? C29 C30 1.43(2) . . ? C29 C34 1.40(2) . . ? C30 C31 1.33(2) . . ? C31 C32 1.43(2) . 4_456 ? C32 C33 1.34(2) . 4_556 ? C33 C34 1.40(2) . . ? C34 C35 1.49(2) . . ? C35 C36 1.42(2) . . ? C35 C40 1.42(2) . . ? C36 C37 1.32(2) . . ? C37 C38 1.39(2) . . ? C38 C39 1.42(2) . . ? C39 C40 1.46(2) . . ? C41 C42 1.47(2) . . ? C41 C53 1.50(2) . . ? C42 C43 1.39(2) . . ? C42 C47 1.49(2) . . ? C43 C44 1.34(2) . . ? C44 C45 1.41(2) . . ? C45 C46 1.42(2) . . ? C46 C47 1.46(2) . . ? C47 C48 1.44(2) . . ? C48 C49 1.34(2) . . ? C48 C53 1.46(2) . . ? C49 C50 1.36(2) . . ? C50 C51 1.42(2) . . ? C51 C52 1.38(2) . . ? C52 C53 1.43(2) . . ? C54 O8 1.57(4) . . ? C55 O9 1.56(4) . . ? B1 F1 1.34(5) . . ? B1 F2 1.43(3) . . ? B1 F3 1.47(4) . . ? B1 F4 1.34(4) . . ? B1 F1a 1.25(4) . . ? B1 F3A 1.21(4) . . ? B1 F4a 1.64(5) . . ? F1 F4 1.76(5) . . ? F1 F1a 1.22(4) . . ? F1 F4a 1.18(5) . . ? F3 F1a 1.96(4) . . ? F3 F3A 1.06(3) . . ? F4 F3A 1.24(3) . . ? F4 F4a 1.46(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 N1 AG N2 141.3(3) . . . ? N1 AG O7 109.4(4) . . . ? N2 AG O7 109.2(4) . . . ? C1 MN1 C2 91.9(6) . . . ? C1 MN1 C3 90.2(6) . . . ? C1 MN1 C28 113.1(5) . . . ? C1 MN1 C29 90.9(5) . . . ? C1 MN1 C34 103.4(6) . . . ? C1 MN1 C35 142.0(6) . . . ? C1 MN1 C40 151.7(5) . . . ? C2 MN1 C3 91.1(6) . . . ? C2 MN1 C28 96.4(5) . . . ? C2 MN1 C29 130.6(5) . . . ? C2 MN1 C34 159.5(5) . . . ? C2 MN1 C35 125.9(5) . . . ? C2 MN1 C40 95.6(5) . . . ? C3 MN1 C28 155.2(5) . . . ? C3 MN1 C29 138.2(6) . . . ? C3 MN1 C34 102.3(6) . . . ? C3 MN1 C35 91.8(6) . . . ? C3 MN1 C40 116.9(5) . . . ? C28 MN1 C29 38.9(4) . . . ? C28 MN1 C34 65.2(5) . . . ? C28 MN1 C35 64.8(5) . . . ? C28 MN1 C40 38.9(4) . . . ? C29 MN1 C34 37.3(4) . . . ? C29 MN1 C35 63.5(4) . . . ? C29 MN1 C40 63.6(4) . . . ? C34 MN1 C35 39.4(5) . . . ? C34 MN1 C40 64.5(5) . . . ? C35 MN1 C40 37.6(5) . . . ? C4 MN2 C5 92.3(6) . . . ? C4 MN2 C6 88.6(6) . . . ? C4 MN2 C41 98.6(5) . . . ? C4 MN2 C42 93.8(5) . . . ? C4 MN2 C47 123.2(6) . . . ? C4 MN2 C48 160.0(5) . . . ? C4 MN2 C53 135.7(5) . . . ? C5 MN2 C6 91.0(6) . . . ? C5 MN2 C41 157.9(5) . . . ? C5 MN2 C42 121.8(6) . . . ? C5 MN2 C47 92.1(5) . . . ? C5 MN2 C48 96.0(5) . . . ? C5 MN2 C53 132.0(5) . . . ? C6 MN2 C41 108.2(5) . . . ? C6 MN2 C42 146.9(5) . . . ? C6 MN2 C47 147.8(6) . . . ? C6 MN2 C48 109.3(6) . . . ? C6 MN2 C53 91.1(5) . . . ? C41 MN2 C42 38.8(5) . . . ? C41 MN2 C47 65.9(5) . . . ? C41 MN2 C48 68.0(4) . . . ? C41 MN2 C53 40.2(4) . . . ? C42 MN2 C47 39.4(5) . . . ? C42 MN2 C48 66.4(5) . . . ? C42 MN2 C53 64.7(5) . . . ? C47 MN2 C48 38.5(5) . . . ? C47 MN2 C53 63.7(5) . . . ? C48 MN2 C53 39.1(5) . . . ? C8 C7 C12 116(1) . . . ? C8 C7 C28 118(1) . . . ? C12 C7 C28 125(1) . . . ? C7 C8 C9 123(1) . . . ? C8 C9 C10 119(1) . . . ? C9 C10 C11 119(1) . . . ? C10 C11 C12 123(1) . . . ? C7 C12 C11 117(1) . . . ? C7 C12 C13 125(1) . . . ? C11 C12 C13 116(1) . . . ? C12 C13 N1 115(1) . . . ? C12 C13 C20 125(1) . . . ? N1 C13 C20 119(1) . . . ? C13 N1 C14 119(1) . . . ? N1 C14 C15 120(1) . . . ? N1 C14 C19 120(1) . . . ? C15 C14 C19 119(1) . . . ? C14 C15 C16 121(1) . . . ? C15 C16 C17 118(1) . . . ? C16 C17 C18 121(1) . . . ? C17 C18 C19 121(1) . . . ? C14 C19 C18 117(1) . . . ? C14 C19 N2 118(1) . . 4_456 ? C18 C19 N2 124(1) . . 4_456 ? C19 N2 C20 122.4(9) 4_556 . 4_556 ? C13 C20 N2 119(1) . . 4_456 ? C13 C20 C21 124(1) . . . ? N2 C20 C21 115.6(9) 4_456 . . ? C20 C21 C22 115(1) . . . ? C20 C21 C26 124(1) . . . ? C22 C21 C26 119(1) . . . ? C21 C22 C23 120(1) . . . ? C22 C23 C24 119(1) . . . ? C23 C24 C25 120(1) . . . ? C24 C25 C26 121(1) . . . ? C21 C26 C25 118(1) . . . ? C21 C26 C41 124(1) . . . ? C25 C26 C41 117(1) . . . ? C7 C28 C29 124(1) . . . ? C7 C28 C40 128(1) . . . ? C29 C28 C40 106(1) . . . ? C28 C29 C30 131(1) . . . ? C28 C29 C34 110(1) . . . ? C30 C29 C34 117(1) . . . ? C29 C30 C31 119(1) . . . ? C30 C31 C32 121(1) . . 4_456 ? C31 C32 C33 119(1) 4_556 . 4_556 ? C32 C33 C34 119(1) 4_456 . . ? C29 C34 C33 121(1) . . . ? C29 C34 C35 106(1) . . . ? C33 C34 C35 131(1) . . . ? C34 C35 C36 130(1) . . . ? C34 C35 C40 107(1) . . . ? C36 C35 C40 122(1) . . . ? C35 C36 C37 117(1) . . . ? C36 C37 C38 124(1) . . . ? C37 C38 C39 120(1) . . . ? C38 C39 C40 116(1) . . . ? C28 C40 C35 109(1) . . . ? C28 C40 C39 132(1) . . . ? C35 C40 C39 118(1) . . . ? C26 C41 C42 127(1) . . . ? C26 C41 C53 125(1) . . . ? C42 C41 C53 105(1) . . . ? C41 C42 C43 133(1) . . . ? C41 C42 C47 107(1) . . . ? C43 C42 C47 118(1) . . . ? C42 C43 C44 121(1) . . . ? C43 C44 C45 121(1) . . . ? C44 C45 C46 121(1) . . . ? C45 C46 C47 117(1) . . . ? C42 C47 C46 118(1) . . . ? C42 C47 C48 111(1) . . . ? C46 C47 C48 130(1) . . . ? C47 C48 C49 132(1) . . . ? C47 C48 C53 105(1) . . . ? C49 C48 C53 121(1) . . . ? C48 C49 C50 119(1) . . . ? C49 C50 C51 122(1) . . . ? C50 C51 C52 120(1) . . . ? C51 C52 C53 117(1) . . . ? C41 C53 C48 110(1) . . . ? C41 C53 C52 130(1) . . . ? C48 C53 C52 118(1) . . . ? F1 B1 F2 130(3) . . . ? F1 B1 F3 107(3) . . . ? F1 B1 F4 81(3) . . . ? F1 B1 F1a 56(2) . . . ? F1 B1 F3A 120(4) . . . ? F1 B1 F4a 45(2) . . . ? F2 B1 F3 120(2) . . . ? F2 B1 F4 105(2) . . . ? F2 B1 F1a 107(2) . . . ? F2 B1 F3A 103(2) . . . ? F2 B1 F4a 96(2) . . . ? F3 B1 F4 94(2) . . . ? F3 B1 F1a 91(2) . . . ? F3 B1 F3A 45(1) . . . ? F3 B1 F4a 139(2) . . . ? F4 B1 F1a 137(3) . . . ? F4 B1 F3A 57(2) . . . ? F4 B1 F4a 57(1) . . . ? F1a B1 F3A 136(3) . . . ? F1a B1 F4a 91(2) . . . ? F3A B1 F4a 115(2) . . . ? B1 F1 F4 49(2) . . . ? B1 F1 F1a 58(2) . . . ? B1 F1 F4a 81(3) . . . ? F4 F1 F1a 107(3) . . . ? F4 F1 F4a 55(2) . . . ? F1a F1 F4a 122(4) . . . ? B1 F3 F1a 39(1) . . . ? B1 F3 F3A 53(2) . . . ? F1a F3 F3A 93(2) . . . ? B1 F4 F1 48(1) . . . ? B1 F4 F3A 55(1) . . . ? B1 F4 F4a 71(2) . . . ? F1 F4 F3A 93(2) . . . ? F1 F4 F4a 41(1) . . . ? F3A F4 F4a 127(2) . . . ? B1 F1a F1 65(2) . . . ? B1 F1a F3 48(1) . . . ? F1 F1a F3 87(2) . . . ? B1 F3A F3 81(2) . . . ? B1 F3A F4 66(2) . . . ? F3 F3A F4 129(3) . . . ? B1 F4a F1 53(2) . . . ? B1 F4a F4 50(1) . . . ? F1 F4a F4 82(3) . . . ? #-----------------END