# Supplementary Material (ESI) for Chemical Communications # This journal is (c) The Royal Society of Chemistry 2010 data_global _journal_coden_Cambridge 182 _publ_requested_journal 'Chemical Communications' loop_ _publ_author_name 'Stewart, Mason' 'Moore, Curtis' 'Ditri, Treffly' 'Labios, Liezel' 'Rheingold, Arnold' 'Figueroa, Joshua S.' _publ_contact_author_name 'Joshua S. Figueroa' _publ_contact_author_address ; 500 Gilman Drive Mail Code 0358 San Diego. California United States 92093 ; _publ_contact_author_email jsfig@ucsd.edu # Attachment 'cif-full.cif' data_JFig236 _database_code_depnum_ccdc_archive 'CCDC 785481' #TrackingRef 'cif-full.cif' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common BrMn(CO)2(CNArMes2)3 _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C79 H80 Br Mn N3 O2.50' _chemical_formula_weight 1246.31 loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source C C 0.0181 0.0091 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' N N 0.0311 0.0180 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' O O 0.0492 0.0322 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Mn Mn -0.5299 2.8052 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Br Br -0.6763 1.2805 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting Monoclinic _symmetry_space_group_name_H-M P2(1)/n loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x+1/2, y+1/2, -z+1/2' '-x, -y, -z' 'x-1/2, -y-1/2, z-1/2' _cell_length_a 17.8362(9) _cell_length_b 15.7440(8) _cell_length_c 24.2053(11) _cell_angle_alpha 90.00 _cell_angle_beta 103.907(3) _cell_angle_gamma 90.00 _cell_volume 6597.9(6) _cell_formula_units_Z 4 _cell_measurement_temperature 100(2) _cell_measurement_reflns_used 9868 _cell_measurement_theta_min 3.40 _cell_measurement_theta_max 64.12 _exptl_crystal_description Block _exptl_crystal_colour Yellow _exptl_crystal_size_max 0.25 _exptl_crystal_size_mid 0.16 _exptl_crystal_size_min 0.11 _exptl_crystal_density_meas 'not measured' _exptl_crystal_density_diffrn 1.255 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 2620 _exptl_absorpt_coefficient_mu 2.718 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.5498 _exptl_absorpt_correction_T_max 0.7542 _exptl_absorpt_process_details SADABS _exptl_special_details ; ? ; _diffrn_ambient_temperature 100(2) _diffrn_radiation_wavelength 1.54178 _diffrn_radiation_type CuK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'Bruker APEX-II CCD' _diffrn_measurement_method '\f and \w scans' _diffrn_reflns_number 75319 _diffrn_reflns_av_R_equivalents 0.0984 _diffrn_reflns_av_sigmaI/netI 0.0519 _diffrn_reflns_limit_h_min -20 _diffrn_reflns_limit_h_max 20 _diffrn_reflns_limit_k_min -18 _diffrn_reflns_limit_k_max 17 _diffrn_reflns_limit_l_min -27 _diffrn_reflns_limit_l_max 28 _diffrn_reflns_theta_min 2.78 _diffrn_reflns_theta_max 64.28 _reflns_number_total 10551 _reflns_number_gt 7479 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'Bruker APEX2' _computing_cell_refinement 'Bruker SAINT' _computing_data_reduction 'Bruker SAINT' _computing_structure_solution 'SHELXS-97 (Sheldrick, 2008)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 2008)' _computing_molecular_graphics 'Bruker SHELXTL' _computing_publication_material 'Bruker SHELXTL' _refine_special_details ; Refinement of F^2^ against ALL reflections. The weighted R-factor wR and goodness of fit S are based on F^2^, conventional R-factors R are based on F, with F set to zero for negative F^2^. The threshold expression of F^2^ > 2sigma(F^2^) is used only for calculating R-factors(gt) etc. and is not relevant to the choice of reflections for refinement. R-factors based on F^2^ are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger. ; _refine_ls_structure_factor_coef Fsqd _refine_ls_matrix_type full _refine_ls_weighting_scheme calc _refine_ls_weighting_details 'calc w=1/[\s^2^(Fo^2^)+(0.0397P)^2^+6.6067P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment constr _refine_ls_extinction_method none _refine_ls_number_reflns 10551 _refine_ls_number_parameters 823 _refine_ls_number_restraints 4 _refine_ls_R_factor_all 0.0770 _refine_ls_R_factor_gt 0.0418 _refine_ls_wR_factor_ref 0.1061 _refine_ls_wR_factor_gt 0.0902 _refine_ls_goodness_of_fit_ref 1.026 _refine_ls_restrained_S_all 1.038 _refine_ls_shift/su_max 0.002 _refine_ls_shift/su_mean 0.000 loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_occupancy _atom_site_symmetry_multiplicity _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group Br1 Br 0.86059(2) 1.04254(3) 0.811279(15) 0.03337(14) Uani 0.8944(13) 1 d P A 1 Br1B Br 0.9122(5) 0.8584(5) 0.7457(3) 0.03337(14) Uani 0.1056(13) 1 d P A 2 Mn2 Mn 0.94661(3) 1.00617(3) 0.745928(19) 0.01996(13) Uani 1 1 d . . . O1 O 0.9042(2) 0.8207(3) 0.74704(15) 0.0561(13) Uani 1 1 d . A 1 O2 O 0.98089(15) 1.19116(18) 0.74515(10) 0.0462(7) Uani 1 1 d . . . N1 N 0.80892(14) 1.03449(15) 0.64454(10) 0.0209(5) Uani 1 1 d . . . N2 N 1.05126(14) 0.96834(16) 0.66835(10) 0.0228(6) Uani 1 1 d . . . N3 N 1.06728(14) 0.97495(15) 0.85785(10) 0.0214(6) Uani 1 1 d . . . C1 C 0.86122(17) 1.02389(18) 0.68335(13) 0.0203(7) Uani 1 1 d . A . C2 C 1.01075(17) 0.98344(18) 0.69877(12) 0.0198(7) Uani 1 1 d . A . C3 C 1.02383(17) 0.98805(19) 0.81382(13) 0.0219(7) Uani 1 1 d . A . C4 C 0.9197(3) 0.8946(4) 0.7463(2) 0.0442(17) Uani 1 1 d . A 1 C5 C 0.96840(16) 1.1259(2) 0.74717(12) 0.0220(7) Uani 1 1 d . A . C6 C 0.74565(16) 1.0421(2) 0.59818(12) 0.0224(7) Uani 1 1 d . A . C7 C 0.71566(17) 1.1234(2) 0.58242(12) 0.0226(7) Uani 1 1 d . . . C8 C 0.65328(18) 1.1287(2) 0.53525(12) 0.0274(7) Uani 1 1 d . A . H8 H 0.6316 1.1826 0.5231 0.033 Uiso 1 1 calc R . . C9 C 0.62246(18) 1.0568(2) 0.50597(13) 0.0308(8) Uani 1 1 d . . . H9 H 0.5803 1.0619 0.4736 0.037 Uiso 1 1 calc R A . C10 C 0.65215(18) 0.9774(2) 0.52314(13) 0.0284(8) Uani 1 1 d . A . H10 H 0.6294 0.9285 0.5028 0.034 Uiso 1 1 calc R . . C11 C 0.71496(17) 0.96792(19) 0.56984(12) 0.0225(7) Uani 1 1 d . . . C12 C 0.74434(17) 0.88190(19) 0.58998(12) 0.0227(7) Uani 1 1 d . A . C13 C 0.81493(17) 0.8516(2) 0.58264(12) 0.0246(7) Uani 1 1 d . . . C14 C 0.83831(18) 0.7700(2) 0.60094(13) 0.0264(7) Uani 1 1 d . A . H14 H 0.8860 0.7494 0.5954 0.032 Uiso 1 1 calc R . . C15 C 0.79478(18) 0.7178(2) 0.62686(13) 0.0264(7) Uani 1 1 d . . . C16 C 0.72555(18) 0.7497(2) 0.63482(13) 0.0288(8) Uani 1 1 d . A . H16 H 0.6948 0.7150 0.6528 0.035 Uiso 1 1 calc R . . C17 C 0.70005(17) 0.8307(2) 0.61727(13) 0.0252(7) Uani 1 1 d . . . C18 C 0.74809(17) 1.20070(19) 0.61518(12) 0.0229(7) Uani 1 1 d . A . C19 C 0.74067(17) 1.21246(19) 0.67114(12) 0.0241(7) Uani 1 1 d . . . C20 C 0.77162(19) 1.2853(2) 0.70043(13) 0.0301(8) Uani 1 1 d . A . H20 H 0.7662 1.2935 0.7382 0.036 Uiso 1 1 calc R . . C21 C 0.80987(19) 1.3459(2) 0.67656(14) 0.0313(8) Uani 1 1 d . . . C22 C 0.81584(19) 1.3337(2) 0.62084(14) 0.0318(8) Uani 1 1 d . A . H22 H 0.8413 1.3754 0.6036 0.038 Uiso 1 1 calc R . . C23 C 0.78563(18) 1.2624(2) 0.58986(13) 0.0265(7) Uani 1 1 d . . . C24 C 0.70034(18) 1.1497(2) 0.70099(13) 0.0291(8) Uani 1 1 d . A . H24C H 0.6657 1.1801 0.7200 0.044 Uiso 1 1 calc R . . H24B H 0.7388 1.1181 0.7293 0.044 Uiso 1 1 calc R . . H24A H 0.6703 1.1100 0.6731 0.044 Uiso 1 1 calc R . . C25 C 0.8449(2) 1.4227(2) 0.70985(17) 0.0454(10) Uani 1 1 d . A . H25B H 0.8672 1.4598 0.6855 0.068 Uiso 1 1 calc R . . H25C H 0.8855 1.4048 0.7427 0.068 Uiso 1 1 calc R . . H25A H 0.8048 1.4537 0.7231 0.068 Uiso 1 1 calc R . . C26 C 0.7954(2) 1.2513(2) 0.52999(13) 0.0334(8) Uani 1 1 d . A . H26B H 0.8204 1.1966 0.5269 0.050 Uiso 1 1 calc R . . H26C H 0.8275 1.2974 0.5211 0.050 Uiso 1 1 calc R . . H26A H 0.7447 1.2526 0.5031 0.050 Uiso 1 1 calc R . . C27 C 0.62592(19) 0.8633(2) 0.62917(16) 0.0380(9) Uani 1 1 d . A . H27C H 0.6354 0.9184 0.6484 0.057 Uiso 1 1 calc R . . H27B H 0.6073 0.8228 0.6536 0.057 Uiso 1 1 calc R . . H27A H 0.5870 0.8699 0.5932 0.057 Uiso 1 1 calc R . . C28 C 0.8231(2) 0.6306(2) 0.64700(15) 0.0351(8) Uani 1 1 d . A . H28B H 0.7828 0.6006 0.6607 0.053 Uiso 1 1 calc R . . H28C H 0.8696 0.6355 0.6780 0.053 Uiso 1 1 calc R . . H28A H 0.8351 0.5988 0.6154 0.053 Uiso 1 1 calc R . . C29 C 0.86759(19) 0.9039(2) 0.55640(14) 0.0346(8) Uani 1 1 d . A . H29A H 0.8802 0.8722 0.5250 0.052 Uiso 1 1 calc R . . H29C H 0.9152 0.9165 0.5852 0.052 Uiso 1 1 calc R . . H29B H 0.8418 0.9572 0.5419 0.052 Uiso 1 1 calc R . . C30 C 1.10559(16) 0.9557(2) 0.63635(12) 0.0218(7) Uani 1 1 d . A . C31 C 1.13108(17) 0.8731(2) 0.62965(12) 0.0241(7) Uani 1 1 d . . . C32 C 1.18415(18) 0.8633(2) 0.59650(13) 0.0293(8) Uani 1 1 d . A . H32 H 1.2016 0.8079 0.5901 0.035 Uiso 1 1 calc R . . C33 C 1.21213(19) 0.9325(2) 0.57257(14) 0.0311(8) Uani 1 1 d . . . H33 H 1.2487 0.9245 0.5502 0.037 Uiso 1 1 calc R A . C34 C 1.18703(18) 1.0134(2) 0.58113(13) 0.0286(8) Uani 1 1 d . A . H34 H 1.2073 1.0606 0.5650 0.034 Uiso 1 1 calc R . . C35 C 1.13278(17) 1.0271(2) 0.61285(12) 0.0234(7) Uani 1 1 d . . . C36 C 1.10475(17) 0.7987(2) 0.65818(13) 0.0248(7) Uani 1 1 d . A . C37 C 1.12190(18) 0.7949(2) 0.71816(13) 0.0278(7) Uani 1 1 d . . . C38 C 1.09605(19) 0.7251(2) 0.74364(15) 0.0352(8) Uani 1 1 d . A . H38 H 1.1059 0.7233 0.7840 0.042 Uiso 1 1 calc R . . C39 C 1.0567(2) 0.6586(2) 0.71258(15) 0.0380(9) Uani 1 1 d . . . C40 C 1.04188(19) 0.6628(2) 0.65380(15) 0.0339(8) Uani 1 1 d . A . H40 H 1.0155 0.6170 0.6319 0.041 Uiso 1 1 calc R . . C41 C 1.06439(18) 0.7317(2) 0.62591(13) 0.0278(7) Uani 1 1 d . . . C42 C 1.10707(18) 1.11415(19) 0.62293(13) 0.0248(7) Uani 1 1 d . A . C43 C 1.03761(18) 1.1470(2) 0.59024(13) 0.0270(7) Uani 1 1 d . . . C44 C 1.0172(2) 1.2293(2) 0.59981(14) 0.0343(8) Uani 1 1 d . A . H44 H 0.9703 1.2517 0.5772 0.041 Uiso 1 1 calc R . . C45 C 1.0625(2) 1.2805(2) 0.64106(16) 0.0391(9) Uani 1 1 d . . . C46 C 1.1303(2) 1.2462(2) 0.67379(15) 0.0387(9) Uani 1 1 d . A . H46 H 1.1620 1.2802 0.7026 0.046 Uiso 1 1 calc R . . C47 C 1.15351(19) 1.1636(2) 0.66591(14) 0.0328(8) Uani 1 1 d . . . C48 C 1.1699(2) 0.8612(2) 0.75542(14) 0.0359(8) Uani 1 1 d . A . H48B H 1.2062 0.8863 0.7355 0.054 Uiso 1 1 calc R . . H48C H 1.1986 0.8348 0.7909 0.054 Uiso 1 1 calc R . . H48A H 1.1360 0.9056 0.7642 0.054 Uiso 1 1 calc R . . C49 C 1.0306(2) 0.5833(3) 0.74180(18) 0.0558(11) Uani 1 1 d . A . H49A H 1.0110 0.5389 0.7137 0.084 Uiso 1 1 calc R . . H49B H 0.9895 0.6011 0.7599 0.084 Uiso 1 1 calc R . . H49C H 1.0743 0.5612 0.7708 0.084 Uiso 1 1 calc R . . C50 C 1.0432(2) 0.7324(2) 0.56190(14) 0.0380(9) Uani 1 1 d . A . H50A H 1.0056 0.6873 0.5479 0.057 Uiso 1 1 calc R . . H50C H 1.0896 0.7229 0.5478 0.057 Uiso 1 1 calc R . . H50B H 1.0205 0.7875 0.5483 0.057 Uiso 1 1 calc R . . C51 C 0.9855(2) 1.0928(2) 0.54605(14) 0.0355(8) Uani 1 1 d . A . H51A H 0.9749 1.0393 0.5634 0.053 Uiso 1 1 calc R . . H51C H 1.0107 1.0808 0.5151 0.053 Uiso 1 1 calc R . . H51B H 0.9368 1.1229 0.5308 0.053 Uiso 1 1 calc R . . C52 C 1.0376(3) 1.3692(2) 0.6519(2) 0.0634(13) Uani 1 1 d . A . H52C H 1.0832 1.4035 0.6689 0.095 Uiso 1 1 calc R . . H52B H 1.0033 1.3669 0.6780 0.095 Uiso 1 1 calc R . . H52A H 1.0101 1.3950 0.6158 0.095 Uiso 1 1 calc R . . C53 C 1.2261(2) 1.1274(3) 0.70337(16) 0.0469(10) Uani 1 1 d . A . H53A H 1.2133 1.0773 0.7233 0.070 Uiso 1 1 calc R . . H53C H 1.2508 1.1702 0.7312 0.070 Uiso 1 1 calc R . . H53B H 1.2616 1.1110 0.6799 0.070 Uiso 1 1 calc R . . C54 C 1.10712(16) 0.97553(19) 0.91500(12) 0.0215(7) Uani 1 1 d . A . C55 C 1.13596(16) 1.0534(2) 0.93882(12) 0.0231(7) Uani 1 1 d . . . C56 C 1.17023(18) 1.0553(2) 0.99685(13) 0.0296(8) Uani 1 1 d . A . H56 H 1.1899 1.1074 1.0143 0.036 Uiso 1 1 calc R . . C57 C 1.17608(18) 0.9824(2) 1.02948(13) 0.0317(8) Uani 1 1 d . . . H57 H 1.1985 0.9850 1.0692 0.038 Uiso 1 1 calc R A . C58 C 1.14953(17) 0.9062(2) 1.00463(13) 0.0276(7) Uani 1 1 d . A . H58 H 1.1551 0.8564 1.0274 0.033 Uiso 1 1 calc R . . C59 C 1.11446(16) 0.9004(2) 0.94652(12) 0.0224(7) Uani 1 1 d . . . C60 C 1.08515(17) 0.81601(19) 0.92227(12) 0.0219(7) Uani 1 1 d . A . C61 C 1.13839(18) 0.7516(2) 0.91896(13) 0.0274(7) Uani 1 1 d . . . C62 C 1.11139(19) 0.6701(2) 0.90392(13) 0.0304(8) Uani 1 1 d . A . H62 H 1.1474 0.6266 0.9016 0.036 Uiso 1 1 calc R . . C63 C 1.03338(19) 0.6502(2) 0.89224(13) 0.0270(7) Uani 1 1 d . . . C64 C 0.98195(18) 0.7158(2) 0.89356(12) 0.0261(7) Uani 1 1 d . A . H64 H 0.9282 0.7036 0.8841 0.031 Uiso 1 1 calc R . . C65 C 1.00572(17) 0.7984(2) 0.90806(12) 0.0232(7) Uani 1 1 d . . . C66 C 1.12962(17) 1.1328(2) 0.90426(12) 0.0242(7) Uani 1 1 d . A . C67 C 1.18302(17) 1.1487(2) 0.87133(13) 0.0267(7) Uani 1 1 d . . . C68 C 1.17853(19) 1.2244(2) 0.84191(14) 0.0314(8) Uani 1 1 d . A . H68 H 1.2146 1.2350 0.8195 0.038 Uiso 1 1 calc R . . C69 C 1.12363(19) 1.2854(2) 0.84387(14) 0.0315(8) Uani 1 1 d . . . C70 C 1.07099(19) 1.2679(2) 0.87601(13) 0.0302(8) Uani 1 1 d . A . H70 H 1.0330 1.3093 0.8780 0.036 Uiso 1 1 calc R . . C71 C 1.07170(17) 1.1922(2) 0.90546(13) 0.0269(7) Uani 1 1 d . . . C72 C 1.2458(2) 1.0854(2) 0.86942(16) 0.0408(9) Uani 1 1 d . A . H72C H 1.2750 1.0727 0.9083 0.061 Uiso 1 1 calc R . . H72B H 1.2806 1.1094 0.8477 0.061 Uiso 1 1 calc R . . H72A H 1.2226 1.0331 0.8510 0.061 Uiso 1 1 calc R . . C73 C 1.1203(2) 1.3685(2) 0.81267(17) 0.0452(10) Uani 1 1 d . A . H73A H 1.0683 1.3767 0.7883 0.068 Uiso 1 1 calc R . . H73B H 1.1579 1.3680 0.7891 0.068 Uiso 1 1 calc R . . H73C H 1.1324 1.4151 0.8402 0.068 Uiso 1 1 calc R . . C74 C 1.0099(2) 1.1746(2) 0.93681(15) 0.0384(9) Uani 1 1 d . A . H74C H 1.0338 1.1538 0.9751 0.058 Uiso 1 1 calc R . . H74A H 0.9742 1.1316 0.9161 0.058 Uiso 1 1 calc R . . H74B H 0.9814 1.2271 0.9395 0.058 Uiso 1 1 calc R . . C75 C 0.94599(18) 0.8651(2) 0.90905(14) 0.0287(8) Uani 1 1 d . A . H75C H 0.9666 0.9062 0.9393 0.043 Uiso 1 1 calc R . . H75B H 0.8997 0.8383 0.9163 0.043 Uiso 1 1 calc R . . H75A H 0.9326 0.8944 0.8723 0.043 Uiso 1 1 calc R . . C76 C 1.0055(2) 0.5601(2) 0.88119(15) 0.0369(8) Uani 1 1 d . A . H76B H 1.0489 0.5235 0.8786 0.055 Uiso 1 1 calc R . . H76A H 0.9658 0.5576 0.8453 0.055 Uiso 1 1 calc R . . H76C H 0.9835 0.5407 0.9124 0.055 Uiso 1 1 calc R . . C77 C 1.22416(18) 0.7691(2) 0.93219(16) 0.0377(9) Uani 1 1 d . A . H77B H 1.2333 0.8239 0.9157 0.057 Uiso 1 1 calc R . . H77A H 1.2500 0.7240 0.9159 0.057 Uiso 1 1 calc R . . H77C H 1.2448 0.7709 0.9735 0.057 Uiso 1 1 calc R . . O1S O 1.5000 1.0000 1.0000 0.0905(17) Uani 1 2 d SD . . C1S C 1.3740(6) 0.9737(8) 1.0048(4) 0.058(3) Uani 0.50 1 d PD B 1 H1SA H 1.3283 0.9460 0.9811 0.087 Uiso 0.50 1 calc PR B 1 H1SB H 1.3615 1.0327 1.0120 0.087 Uiso 0.50 1 calc PR B 1 H1SC H 1.3903 0.9434 1.0411 0.087 Uiso 0.50 1 calc PR B 1 C1SB C 1.3702(6) 0.9291(7) 0.9813(5) 0.062(3) Uani 0.50 1 d PD C 2 H1SD H 1.3574 0.9451 0.9409 0.092 Uiso 0.50 1 calc PR C 2 H1SE H 1.3236 0.9318 0.9959 0.092 Uiso 0.50 1 calc PR C 2 H1SF H 1.3909 0.8712 0.9854 0.092 Uiso 0.50 1 calc PR C 2 C2S C 1.4376(5) 0.9723(5) 0.9749(4) 0.0430(19) Uani 0.50 1 d PD B 1 H2SA H 1.4451 0.9127 0.9643 0.052 Uiso 0.50 1 calc PR B 1 H2SB H 1.4204 1.0047 0.9391 0.052 Uiso 0.50 1 calc PR B 1 C2SB C 1.4294(5) 0.9893(5) 1.0142(4) 0.048(2) Uani 0.50 1 d PD C 2 H2SC H 1.4048 1.0459 1.0121 0.057 Uiso 0.50 1 calc PR C 2 H2SD H 1.4408 0.9713 1.0545 0.057 Uiso 0.50 1 calc PR C 2 loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 Br1 0.0305(2) 0.0431(3) 0.0276(2) 0.00351(18) 0.00902(16) 0.01176(19) Br1B 0.0305(2) 0.0431(3) 0.0276(2) 0.00351(18) 0.00902(16) 0.01176(19) Mn2 0.0173(2) 0.0241(3) 0.0180(2) 0.0011(2) 0.00306(19) 0.0023(2) O1 0.068(2) 0.038(2) 0.058(2) 0.0047(18) 0.0065(15) -0.0094(19) O2 0.0468(16) 0.0440(17) 0.0424(15) -0.0053(13) 0.0002(12) 0.0017(14) N1 0.0199(13) 0.0202(14) 0.0219(13) 0.0004(11) 0.0034(12) 0.0007(11) N2 0.0241(14) 0.0208(14) 0.0245(13) 0.0019(11) 0.0078(12) 0.0028(12) N3 0.0198(13) 0.0237(15) 0.0211(14) 0.0003(11) 0.0061(12) -0.0010(11) C1 0.0238(17) 0.0161(17) 0.0254(16) -0.0016(13) 0.0147(15) -0.0016(13) C2 0.0192(15) 0.0168(17) 0.0206(15) 0.0028(12) -0.0009(14) -0.0011(13) C3 0.0211(16) 0.0187(17) 0.0279(17) -0.0009(13) 0.0098(15) -0.0013(13) C4 0.045(3) 0.048(3) 0.039(2) 0.008(3) 0.0083(18) 0.003(3) C5 0.0132(15) 0.032(2) 0.0159(15) 0.0104(14) -0.0055(12) -0.0104(15) C6 0.0199(15) 0.0287(18) 0.0178(15) 0.0034(14) 0.0028(13) 0.0022(14) C7 0.0209(16) 0.0268(18) 0.0209(15) 0.0026(13) 0.0068(13) 0.0045(14) C8 0.0259(17) 0.0316(19) 0.0238(16) 0.0051(14) 0.0043(14) 0.0106(15) C9 0.0249(17) 0.043(2) 0.0217(16) 0.0014(15) 0.0009(14) 0.0049(16) C10 0.0261(17) 0.034(2) 0.0234(16) -0.0013(14) 0.0017(14) -0.0010(15) C11 0.0210(16) 0.0258(18) 0.0216(15) 0.0005(13) 0.0068(13) -0.0003(14) C12 0.0246(17) 0.0223(17) 0.0200(15) -0.0045(13) 0.0030(13) -0.0028(14) C13 0.0262(17) 0.0242(18) 0.0232(16) -0.0007(14) 0.0055(13) -0.0040(14) C14 0.0245(17) 0.0269(19) 0.0293(17) -0.0015(14) 0.0090(14) 0.0014(15) C15 0.0276(17) 0.0224(18) 0.0280(17) -0.0048(14) 0.0044(14) -0.0029(15) C16 0.0264(18) 0.0290(19) 0.0324(18) -0.0013(15) 0.0101(15) -0.0070(15) C17 0.0221(16) 0.0237(18) 0.0294(17) -0.0033(14) 0.0055(14) -0.0036(14) C18 0.0212(16) 0.0213(17) 0.0257(16) 0.0030(14) 0.0046(13) 0.0081(14) C19 0.0227(16) 0.0231(18) 0.0253(16) 0.0028(14) 0.0035(13) 0.0092(14) C20 0.0343(19) 0.0281(19) 0.0269(17) -0.0019(15) 0.0052(15) 0.0080(16) C21 0.0316(19) 0.0236(18) 0.0357(19) -0.0005(15) 0.0020(15) 0.0057(15) C22 0.0355(19) 0.0219(18) 0.040(2) 0.0086(15) 0.0126(16) 0.0064(16) C23 0.0277(17) 0.0234(18) 0.0278(17) 0.0055(14) 0.0058(14) 0.0084(15) C24 0.0287(18) 0.033(2) 0.0259(17) 0.0013(14) 0.0065(14) 0.0030(15) C25 0.056(3) 0.028(2) 0.051(2) -0.0061(17) 0.011(2) -0.0018(18) C26 0.042(2) 0.0287(19) 0.0325(18) 0.0083(15) 0.0147(16) 0.0049(16) C27 0.0312(19) 0.035(2) 0.053(2) 0.0020(17) 0.0199(17) -0.0001(16) C28 0.038(2) 0.0265(19) 0.042(2) 0.0005(16) 0.0116(17) 0.0001(16) C29 0.0312(19) 0.036(2) 0.040(2) 0.0098(16) 0.0145(16) 0.0044(16) C30 0.0184(15) 0.0279(18) 0.0205(15) 0.0000(14) 0.0074(13) -0.0001(14) C31 0.0236(17) 0.0265(19) 0.0232(16) 0.0025(14) 0.0076(13) 0.0016(14) C32 0.0290(18) 0.0296(19) 0.0318(18) 0.0003(15) 0.0124(15) 0.0046(15) C33 0.0261(18) 0.039(2) 0.0329(18) -0.0001(16) 0.0152(15) 0.0003(16) C34 0.0273(17) 0.032(2) 0.0293(17) 0.0019(15) 0.0110(14) -0.0034(15) C35 0.0222(16) 0.0280(19) 0.0205(15) 0.0004(13) 0.0059(13) -0.0042(14) C36 0.0237(17) 0.0249(18) 0.0284(17) 0.0057(14) 0.0111(14) 0.0085(14) C37 0.0228(17) 0.0312(19) 0.0307(18) 0.0076(15) 0.0088(14) 0.0100(15) C38 0.034(2) 0.040(2) 0.0323(18) 0.0142(17) 0.0099(16) 0.0100(17) C39 0.034(2) 0.038(2) 0.043(2) 0.0168(18) 0.0126(17) 0.0075(17) C40 0.0336(19) 0.0272(19) 0.041(2) 0.0045(16) 0.0103(16) 0.0030(16) C41 0.0253(17) 0.0274(19) 0.0330(18) 0.0048(15) 0.0117(15) 0.0059(15) C42 0.0268(17) 0.0218(18) 0.0290(17) 0.0006(14) 0.0130(14) -0.0039(14) C43 0.0296(18) 0.0225(18) 0.0291(17) 0.0036(14) 0.0072(14) -0.0012(15) C44 0.035(2) 0.028(2) 0.0374(19) 0.0040(16) 0.0042(16) 0.0031(16) C45 0.041(2) 0.025(2) 0.050(2) -0.0033(17) 0.0088(18) 0.0015(17) C46 0.037(2) 0.031(2) 0.046(2) -0.0106(17) 0.0067(17) -0.0082(17) C47 0.0273(18) 0.032(2) 0.039(2) -0.0039(16) 0.0083(15) -0.0030(16) C48 0.036(2) 0.040(2) 0.0301(18) 0.0044(16) 0.0047(16) 0.0099(17) C49 0.061(3) 0.048(3) 0.057(3) 0.024(2) 0.011(2) -0.005(2) C50 0.043(2) 0.038(2) 0.0357(19) -0.0017(16) 0.0146(17) -0.0031(18) C51 0.038(2) 0.029(2) 0.0349(19) 0.0017(16) -0.0003(16) 0.0001(16) C52 0.071(3) 0.031(2) 0.078(3) -0.015(2) -0.001(2) 0.009(2) C53 0.033(2) 0.050(2) 0.051(2) -0.0145(19) -0.0034(18) 0.0009(18) C54 0.0162(15) 0.0300(19) 0.0173(15) 0.0020(13) 0.0022(12) -0.0003(13) C55 0.0156(15) 0.0292(19) 0.0244(16) -0.0001(14) 0.0045(13) -0.0020(14) C56 0.0270(17) 0.035(2) 0.0252(17) -0.0061(15) 0.0024(14) -0.0044(15) C57 0.0297(18) 0.044(2) 0.0181(16) -0.0005(15) 0.0002(14) -0.0014(16) C58 0.0229(17) 0.034(2) 0.0243(16) 0.0053(15) 0.0024(14) 0.0002(15) C59 0.0172(15) 0.0277(18) 0.0218(15) 0.0002(14) 0.0038(13) 0.0000(14) C60 0.0224(16) 0.0259(18) 0.0178(15) 0.0045(13) 0.0057(13) 0.0009(14) C61 0.0248(17) 0.031(2) 0.0262(17) 0.0076(14) 0.0058(14) 0.0003(15) C62 0.0302(19) 0.030(2) 0.0330(18) 0.0077(15) 0.0116(15) 0.0103(16) C63 0.0327(18) 0.0259(18) 0.0232(16) 0.0042(14) 0.0082(14) -0.0021(15) C64 0.0254(17) 0.0305(19) 0.0230(16) 0.0042(14) 0.0069(14) -0.0033(15) C65 0.0227(16) 0.0280(19) 0.0193(15) 0.0049(13) 0.0054(13) -0.0002(14) C66 0.0217(16) 0.0265(18) 0.0226(16) -0.0024(13) 0.0014(13) -0.0046(14) C67 0.0228(17) 0.0272(19) 0.0304(17) -0.0019(14) 0.0068(14) -0.0023(14) C68 0.0297(18) 0.031(2) 0.0356(19) -0.0011(16) 0.0127(15) -0.0043(16) C69 0.0323(19) 0.0272(19) 0.0336(18) 0.0006(15) 0.0052(15) -0.0036(16) C70 0.0284(18) 0.0281(19) 0.0334(18) -0.0030(15) 0.0062(15) 0.0029(15) C71 0.0226(17) 0.0306(19) 0.0266(17) -0.0036(15) 0.0044(14) -0.0040(15) C72 0.035(2) 0.039(2) 0.053(2) 0.0059(18) 0.0208(18) 0.0046(17) C73 0.049(2) 0.033(2) 0.056(2) 0.0107(18) 0.019(2) 0.0054(18) C74 0.0304(19) 0.047(2) 0.041(2) 0.0068(17) 0.0138(16) 0.0057(17) C75 0.0246(17) 0.0296(19) 0.0330(18) 0.0034(15) 0.0090(14) 0.0014(15) C76 0.041(2) 0.030(2) 0.040(2) 0.0021(16) 0.0125(17) -0.0010(17) C77 0.0234(18) 0.041(2) 0.047(2) 0.0049(17) 0.0060(16) 0.0034(16) O1S 0.038(3) 0.151(5) 0.085(3) 0.053(3) 0.021(3) 0.017(3) C1S 0.035(6) 0.086(9) 0.053(6) -0.002(5) 0.009(5) -0.012(6) C1SB 0.033(5) 0.065(8) 0.082(8) -0.001(6) 0.005(6) 0.003(5) C2S 0.043(6) 0.037(5) 0.049(5) 0.003(4) 0.011(4) 0.003(4) C2SB 0.042(6) 0.053(6) 0.049(6) 0.000(4) 0.014(5) 0.007(5) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag Br1 Mn2 2.5200(6) . ? Br1B Mn2 2.405(9) . ? Mn2 C4 1.821(6) . ? Mn2 C2 1.835(3) . ? Mn2 C1 1.893(3) . ? Mn2 C3 1.895(3) . ? Mn2 C5 1.924(4) . ? O1 C4 1.197(7) . ? O2 C5 1.055(4) . ? N1 C1 1.166(4) . ? N1 C6 1.392(4) . ? N2 C2 1.173(4) . ? N2 C30 1.393(4) . ? N3 C3 1.176(4) . ? N3 C54 1.395(4) . ? C6 C11 1.398(4) . ? C6 C7 1.404(4) . ? C7 C8 1.392(4) . ? C7 C18 1.491(4) . ? C8 C9 1.377(5) . ? C8 H8 0.9500 . ? C9 C10 1.383(5) . ? C9 H9 0.9500 . ? C10 C11 1.395(4) . ? C10 H10 0.9500 . ? C11 C12 1.491(4) . ? C12 C13 1.397(4) . ? C12 C17 1.401(4) . ? C13 C14 1.390(4) . ? C13 C29 1.500(4) . ? C14 C15 1.381(4) . ? C14 H14 0.9500 . ? C15 C16 1.388(4) . ? C15 C28 1.503(4) . ? C16 C17 1.386(4) . ? C16 H16 0.9500 . ? C17 C27 1.509(4) . ? C18 C23 1.401(4) . ? C18 C19 1.405(4) . ? C19 C20 1.391(4) . ? C19 C24 1.505(4) . ? C20 C21 1.378(5) . ? C20 H20 0.9500 . ? C21 C22 1.392(5) . ? C21 C25 1.504(5) . ? C22 C23 1.386(5) . ? C22 H22 0.9500 . ? C23 C26 1.511(4) . ? C24 H24C 0.9800 . ? C24 H24B 0.9800 . ? C24 H24A 0.9800 . ? C25 H25B 0.9800 . ? C25 H25C 0.9800 . ? C25 H25A 0.9800 . ? C26 H26B 0.9800 . ? C26 H26C 0.9800 . ? C26 H26A 0.9800 . ? C27 H27C 0.9800 . ? C27 H27B 0.9800 . ? C27 H27A 0.9800 . ? C28 H28B 0.9800 . ? C28 H28C 0.9800 . ? C28 H28A 0.9800 . ? C29 H29A 0.9800 . ? C29 H29C 0.9800 . ? C29 H29B 0.9800 . ? C30 C35 1.398(4) . ? C30 C31 1.400(4) . ? C31 C32 1.389(4) . ? C31 C36 1.492(4) . ? C32 C33 1.383(5) . ? C32 H32 0.9500 . ? C33 C34 1.382(5) . ? C33 H33 0.9500 . ? C34 C35 1.389(4) . ? C34 H34 0.9500 . ? C35 C42 1.484(4) . ? C36 C41 1.404(4) . ? C36 C37 1.411(4) . ? C37 C38 1.392(5) . ? C37 C48 1.504(5) . ? C38 C39 1.379(5) . ? C38 H38 0.9500 . ? C39 C40 1.385(5) . ? C39 C49 1.509(5) . ? C40 C41 1.387(5) . ? C40 H40 0.9500 . ? C41 C50 1.504(4) . ? C42 C43 1.399(4) . ? C42 C47 1.400(4) . ? C43 C44 1.381(5) . ? C43 C51 1.503(4) . ? C44 C45 1.382(5) . ? C44 H44 0.9500 . ? C45 C46 1.386(5) . ? C45 C52 1.508(5) . ? C46 C47 1.391(5) . ? C46 H46 0.9500 . ? C47 C53 1.503(5) . ? C48 H48B 0.9800 . ? C48 H48C 0.9800 . ? C48 H48A 0.9800 . ? C49 H49A 0.9800 . ? C49 H49B 0.9800 . ? C49 H49C 0.9800 . ? C50 H50A 0.9800 . ? C50 H50C 0.9800 . ? C50 H50B 0.9800 . ? C51 H51A 0.9800 . ? C51 H51C 0.9800 . ? C51 H51B 0.9800 . ? C52 H52C 0.9800 . ? C52 H52B 0.9800 . ? C52 H52A 0.9800 . ? C53 H53A 0.9800 . ? C53 H53C 0.9800 . ? C53 H53B 0.9800 . ? C54 C59 1.396(4) . ? C54 C55 1.399(4) . ? C55 C56 1.391(4) . ? C55 C66 1.493(4) . ? C56 C57 1.383(5) . ? C56 H56 0.9500 . ? C57 C58 1.374(5) . ? C57 H57 0.9500 . ? C58 C59 1.398(4) . ? C58 H58 0.9500 . ? C59 C60 1.496(4) . ? C60 C65 1.403(4) . ? C60 C61 1.404(4) . ? C61 C62 1.389(5) . ? C61 C77 1.511(4) . ? C62 C63 1.387(4) . ? C62 H62 0.9500 . ? C63 C64 1.387(4) . ? C63 C76 1.505(5) . ? C64 C65 1.387(4) . ? C64 H64 0.9500 . ? C65 C75 1.500(4) . ? C66 C71 1.399(4) . ? C66 C67 1.404(4) . ? C67 C68 1.382(5) . ? C67 C72 1.508(5) . ? C68 C69 1.379(5) . ? C68 H68 0.9500 . ? C69 C70 1.383(5) . ? C69 C73 1.506(5) . ? C70 C71 1.388(4) . ? C70 H70 0.9500 . ? C71 C74 1.507(4) . ? C72 H72C 0.9800 . ? C72 H72B 0.9800 . ? C72 H72A 0.9800 . ? C73 H73A 0.9800 . ? C73 H73B 0.9800 . ? C73 H73C 0.9800 . ? C74 H74C 0.9800 . ? C74 H74A 0.9800 . ? C74 H74B 0.9800 . ? C75 H75C 0.9800 . ? C75 H75B 0.9800 . ? C75 H75A 0.9800 . ? C76 H76B 0.9800 . ? C76 H76A 0.9800 . ? C76 H76C 0.9800 . ? C77 H77B 0.9800 . ? C77 H77A 0.9800 . ? C77 H77C 0.9800 . ? O1S C2S 1.213(8) 3_877 ? O1S C2S 1.213(8) . ? O1S C2SB 1.392(10) 3_877 ? O1S C2SB 1.392(10) . ? C1S C2S 1.485(11) . ? C1S H1SA 0.9800 . ? C1S H1SB 0.9800 . ? C1S H1SC 0.9800 . ? C1SB C2SB 1.497(11) . ? C1SB H1SD 0.9800 . ? C1SB H1SE 0.9800 . ? C1SB H1SF 0.9800 . ? C2S H2SA 0.9900 . ? C2S H2SB 0.9900 . ? C2SB H2SC 0.9900 . ? C2SB H2SD 0.9900 . ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag C4 Mn2 C2 91.1(2) . . ? C4 Mn2 C1 89.05(19) . . ? C2 Mn2 C1 91.89(12) . . ? C4 Mn2 C3 89.33(19) . . ? C2 Mn2 C3 94.48(12) . . ? C1 Mn2 C3 173.45(12) . . ? C4 Mn2 C5 175.9(2) . . ? C2 Mn2 C5 92.70(13) . . ? C1 Mn2 C5 89.36(12) . . ? C3 Mn2 C5 91.84(12) . . ? C4 Mn2 Br1B 0.7(3) . . ? C2 Mn2 Br1B 90.4(2) . . ? C1 Mn2 Br1B 89.1(2) . . ? C3 Mn2 Br1B 89.3(2) . . ? C5 Mn2 Br1B 176.6(2) . . ? C4 Mn2 Br1 90.89(18) . . ? C2 Mn2 Br1 177.98(9) . . ? C1 Mn2 Br1 88.55(8) . . ? C3 Mn2 Br1 85.13(9) . . ? C5 Mn2 Br1 85.33(9) . . ? Br1B Mn2 Br1 91.60(18) . . ? C1 N1 C6 176.7(3) . . ? C2 N2 C30 173.6(3) . . ? C3 N3 C54 164.9(3) . . ? N1 C1 Mn2 179.5(3) . . ? N2 C2 Mn2 179.4(3) . . ? N3 C3 Mn2 174.9(3) . . ? O1 C4 Mn2 178.1(4) . . ? O2 C5 Mn2 176.3(3) . . ? N1 C6 C11 118.0(3) . . ? N1 C6 C7 118.7(3) . . ? C11 C6 C7 123.3(3) . . ? C8 C7 C6 117.0(3) . . ? C8 C7 C18 121.3(3) . . ? C6 C7 C18 121.7(3) . . ? C9 C8 C7 121.0(3) . . ? C9 C8 H8 119.5 . . ? C7 C8 H8 119.5 . . ? C8 C9 C10 120.8(3) . . ? C8 C9 H9 119.6 . . ? C10 C9 H9 119.6 . . ? C9 C10 C11 121.0(3) . . ? C9 C10 H10 119.5 . . ? C11 C10 H10 119.5 . . ? C10 C11 C6 116.9(3) . . ? C10 C11 C12 120.8(3) . . ? C6 C11 C12 122.2(3) . . ? C13 C12 C17 119.4(3) . . ? C13 C12 C11 121.7(3) . . ? C17 C12 C11 118.9(3) . . ? C14 C13 C12 119.0(3) . . ? C14 C13 C29 118.2(3) . . ? C12 C13 C29 122.8(3) . . ? C15 C14 C13 122.5(3) . . ? C15 C14 H14 118.8 . . ? C13 C14 H14 118.8 . . ? C14 C15 C16 117.6(3) . . ? C14 C15 C28 120.6(3) . . ? C16 C15 C28 121.7(3) . . ? C17 C16 C15 121.8(3) . . ? C17 C16 H16 119.1 . . ? C15 C16 H16 119.1 . . ? C16 C17 C12 119.6(3) . . ? C16 C17 C27 119.5(3) . . ? C12 C17 C27 120.9(3) . . ? C23 C18 C19 119.7(3) . . ? C23 C18 C7 119.9(3) . . ? C19 C18 C7 120.4(3) . . ? C20 C19 C18 118.8(3) . . ? C20 C19 C24 118.3(3) . . ? C18 C19 C24 122.9(3) . . ? C21 C20 C19 122.2(3) . . ? C21 C20 H20 118.9 . . ? C19 C20 H20 118.9 . . ? C20 C21 C22 118.2(3) . . ? C20 C21 C25 121.1(3) . . ? C22 C21 C25 120.7(3) . . ? C23 C22 C21 121.7(3) . . ? C23 C22 H22 119.2 . . ? C21 C22 H22 119.2 . . ? C22 C23 C18 119.3(3) . . ? C22 C23 C26 119.5(3) . . ? C18 C23 C26 121.1(3) . . ? C19 C24 H24C 109.5 . . ? C19 C24 H24B 109.5 . . ? H24C C24 H24B 109.5 . . ? C19 C24 H24A 109.5 . . ? H24C C24 H24A 109.5 . . ? H24B C24 H24A 109.5 . . ? C21 C25 H25B 109.5 . . ? C21 C25 H25C 109.5 . . ? H25B C25 H25C 109.5 . . ? C21 C25 H25A 109.5 . . ? H25B C25 H25A 109.5 . . ? H25C C25 H25A 109.5 . . ? C23 C26 H26B 109.5 . . ? C23 C26 H26C 109.5 . . ? H26B C26 H26C 109.5 . . ? C23 C26 H26A 109.5 . . ? H26B C26 H26A 109.5 . . ? H26C C26 H26A 109.5 . . ? C17 C27 H27C 109.5 . . ? C17 C27 H27B 109.5 . . ? H27C C27 H27B 109.5 . . ? C17 C27 H27A 109.5 . . ? H27C C27 H27A 109.5 . . ? H27B C27 H27A 109.5 . . ? C15 C28 H28B 109.5 . . ? C15 C28 H28C 109.5 . . ? H28B C28 H28C 109.5 . . ? C15 C28 H28A 109.5 . . ? H28B C28 H28A 109.5 . . ? H28C C28 H28A 109.5 . . ? C13 C29 H29A 109.5 . . ? C13 C29 H29C 109.5 . . ? H29A C29 H29C 109.5 . . ? C13 C29 H29B 109.5 . . ? H29A C29 H29B 109.5 . . ? H29C C29 H29B 109.5 . . ? N2 C30 C35 117.9(3) . . ? N2 C30 C31 119.1(3) . . ? C35 C30 C31 123.1(3) . . ? C32 C31 C30 117.1(3) . . ? C32 C31 C36 120.9(3) . . ? C30 C31 C36 121.9(3) . . ? C33 C32 C31 121.2(3) . . ? C33 C32 H32 119.4 . . ? C31 C32 H32 119.4 . . ? C34 C33 C32 120.1(3) . . ? C34 C33 H33 120.0 . . ? C32 C33 H33 120.0 . . ? C33 C34 C35 121.3(3) . . ? C33 C34 H34 119.4 . . ? C35 C34 H34 119.4 . . ? C34 C35 C30 117.2(3) . . ? C34 C35 C42 121.2(3) . . ? C30 C35 C42 121.6(3) . . ? C41 C36 C37 119.7(3) . . ? C41 C36 C31 120.6(3) . . ? C37 C36 C31 119.7(3) . . ? C38 C37 C36 118.4(3) . . ? C38 C37 C48 118.9(3) . . ? C36 C37 C48 122.6(3) . . ? C39 C38 C37 122.5(3) . . ? C39 C38 H38 118.7 . . ? C37 C38 H38 118.7 . . ? C38 C39 C40 118.0(3) . . ? C38 C39 C49 121.0(3) . . ? C40 C39 C49 121.0(4) . . ? C39 C40 C41 122.1(3) . . ? C39 C40 H40 119.0 . . ? C41 C40 H40 119.0 . . ? C40 C41 C36 119.1(3) . . ? C40 C41 C50 118.4(3) . . ? C36 C41 C50 122.4(3) . . ? C43 C42 C47 120.0(3) . . ? C43 C42 C35 121.0(3) . . ? C47 C42 C35 119.0(3) . . ? C44 C43 C42 119.1(3) . . ? C44 C43 C51 120.6(3) . . ? C42 C43 C51 120.3(3) . . ? C43 C44 C45 122.4(3) . . ? C43 C44 H44 118.8 . . ? C45 C44 H44 118.8 . . ? C44 C45 C46 117.7(3) . . ? C44 C45 C52 121.3(3) . . ? C46 C45 C52 121.0(3) . . ? C45 C46 C47 122.2(3) . . ? C45 C46 H46 118.9 . . ? C47 C46 H46 118.9 . . ? C46 C47 C42 118.6(3) . . ? C46 C47 C53 120.9(3) . . ? C42 C47 C53 120.4(3) . . ? C37 C48 H48B 109.5 . . ? C37 C48 H48C 109.5 . . ? H48B C48 H48C 109.5 . . ? C37 C48 H48A 109.5 . . ? H48B C48 H48A 109.5 . . ? H48C C48 H48A 109.5 . . ? C39 C49 H49A 109.5 . . ? C39 C49 H49B 109.5 . . ? H49A C49 H49B 109.5 . . ? C39 C49 H49C 109.5 . . ? H49A C49 H49C 109.5 . . ? H49B C49 H49C 109.5 . . ? C41 C50 H50A 109.5 . . ? C41 C50 H50C 109.5 . . ? H50A C50 H50C 109.5 . . ? C41 C50 H50B 109.5 . . ? H50A C50 H50B 109.5 . . ? H50C C50 H50B 109.5 . . ? C43 C51 H51A 109.5 . . ? C43 C51 H51C 109.5 . . ? H51A C51 H51C 109.5 . . ? C43 C51 H51B 109.5 . . ? H51A C51 H51B 109.5 . . ? H51C C51 H51B 109.5 . . ? C45 C52 H52C 109.5 . . ? C45 C52 H52B 109.5 . . ? H52C C52 H52B 109.5 . . ? C45 C52 H52A 109.5 . . ? H52C C52 H52A 109.5 . . ? H52B C52 H52A 109.5 . . ? C47 C53 H53A 109.5 . . ? C47 C53 H53C 109.5 . . ? H53A C53 H53C 109.5 . . ? C47 C53 H53B 109.5 . . ? H53A C53 H53B 109.5 . . ? H53C C53 H53B 109.5 . . ? N3 C54 C59 119.7(3) . . ? N3 C54 C55 117.6(3) . . ? C59 C54 C55 122.7(3) . . ? C56 C55 C54 117.6(3) . . ? C56 C55 C66 120.2(3) . . ? C54 C55 C66 122.1(3) . . ? C57 C56 C55 120.9(3) . . ? C57 C56 H56 119.5 . . ? C55 C56 H56 119.5 . . ? C58 C57 C56 120.2(3) . . ? C58 C57 H57 119.9 . . ? C56 C57 H57 119.9 . . ? C57 C58 C59 121.4(3) . . ? C57 C58 H58 119.3 . . ? C59 C58 H58 119.3 . . ? C54 C59 C58 117.1(3) . . ? C54 C59 C60 124.1(3) . . ? C58 C59 C60 118.8(3) . . ? C65 C60 C61 120.0(3) . . ? C65 C60 C59 120.6(3) . . ? C61 C60 C59 119.1(3) . . ? C62 C61 C60 119.1(3) . . ? C62 C61 C77 119.6(3) . . ? C60 C61 C77 121.4(3) . . ? C63 C62 C61 122.0(3) . . ? C63 C62 H62 119.0 . . ? C61 C62 H62 119.0 . . ? C64 C63 C62 117.6(3) . . ? C64 C63 C76 120.9(3) . . ? C62 C63 C76 121.5(3) . . ? C65 C64 C63 122.7(3) . . ? C65 C64 H64 118.6 . . ? C63 C64 H64 118.6 . . ? C64 C65 C60 118.5(3) . . ? C64 C65 C75 119.1(3) . . ? C60 C65 C75 122.5(3) . . ? C71 C66 C67 119.9(3) . . ? C71 C66 C55 120.3(3) . . ? C67 C66 C55 119.8(3) . . ? C68 C67 C66 118.9(3) . . ? C68 C67 C72 120.4(3) . . ? C66 C67 C72 120.7(3) . . ? C69 C68 C67 122.4(3) . . ? C69 C68 H68 118.8 . . ? C67 C68 H68 118.8 . . ? C68 C69 C70 117.7(3) . . ? C68 C69 C73 122.0(3) . . ? C70 C69 C73 120.3(3) . . ? C69 C70 C71 122.4(3) . . ? C69 C70 H70 118.8 . . ? C71 C70 H70 118.8 . . ? C70 C71 C66 118.6(3) . . ? C70 C71 C74 119.9(3) . . ? C66 C71 C74 121.4(3) . . ? C67 C72 H72C 109.5 . . ? C67 C72 H72B 109.5 . . ? H72C C72 H72B 109.5 . . ? C67 C72 H72A 109.5 . . ? H72C C72 H72A 109.5 . . ? H72B C72 H72A 109.5 . . ? C69 C73 H73A 109.5 . . ? C69 C73 H73B 109.5 . . ? H73A C73 H73B 109.5 . . ? C69 C73 H73C 109.5 . . ? H73A C73 H73C 109.5 . . ? H73B C73 H73C 109.5 . . ? C71 C74 H74C 109.5 . . ? C71 C74 H74A 109.5 . . ? H74C C74 H74A 109.5 . . ? C71 C74 H74B 109.5 . . ? H74C C74 H74B 109.5 . . ? H74A C74 H74B 109.5 . . ? C65 C75 H75C 109.5 . . ? C65 C75 H75B 109.5 . . ? H75C C75 H75B 109.5 . . ? C65 C75 H75A 109.5 . . ? H75C C75 H75A 109.5 . . ? H75B C75 H75A 109.5 . . ? C63 C76 H76B 109.5 . . ? C63 C76 H76A 109.5 . . ? H76B C76 H76A 109.5 . . ? C63 C76 H76C 109.5 . . ? H76B C76 H76C 109.5 . . ? H76A C76 H76C 109.5 . . ? C61 C77 H77B 109.5 . . ? C61 C77 H77A 109.5 . . ? H77B C77 H77A 109.5 . . ? C61 C77 H77C 109.5 . . ? H77B C77 H77C 109.5 . . ? H77A C77 H77C 109.5 . . ? C2S O1S C2S 179.996(3) 3_877 . ? C2S O1S C2SB 46.0(5) 3_877 3_877 ? C2S O1S C2SB 134.0(5) . 3_877 ? C2S O1S C2SB 134.0(5) 3_877 . ? C2S O1S C2SB 46.0(5) . . ? C2SB O1S C2SB 179.997(3) 3_877 . ? C2SB C1SB H1SD 109.5 . . ? C2SB C1SB H1SE 109.5 . . ? H1SD C1SB H1SE 109.5 . . ? C2SB C1SB H1SF 109.5 . . ? H1SD C1SB H1SF 109.5 . . ? H1SE C1SB H1SF 109.5 . . ? O1S C2S C1S 117.8(9) . . ? O1S C2S H2SA 107.9 . . ? C1S C2S H2SA 107.9 . . ? O1S C2S H2SB 107.9 . . ? C1S C2S H2SB 107.9 . . ? H2SA C2S H2SB 107.2 . . ? O1S C2SB C1SB 120.7(8) . . ? O1S C2SB H2SC 107.2 . . ? C1SB C2SB H2SC 107.2 . . ? O1S C2SB H2SD 107.2 . . ? C1SB C2SB H2SD 107.2 . . ? H2SC C2SB H2SD 106.8 . . ? _diffrn_measured_fraction_theta_max 0.957 _diffrn_reflns_theta_full 64.28 _diffrn_measured_fraction_theta_full 0.957 _refine_diff_density_max 0.611 _refine_diff_density_min -0.376 _refine_diff_density_rms 0.057 #===END data_JFig293 _database_code_depnum_ccdc_archive 'CCDC 785482' #TrackingRef 'cif-full.cif' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common '[K(DME)(18-c-6)][Mn(CO)2(CNArMes2)3]' _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C105 H139 K Mn N3 O16' _chemical_formula_weight 1793.23 loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' K K 0.2009 0.2494 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Mn Mn 0.3368 0.7283 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting Triclinic _symmetry_space_group_name_H-M P-1 loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, -y, -z' _cell_length_a 12.881(5) _cell_length_b 15.819(5) _cell_length_c 24.700(5) _cell_angle_alpha 96.168(5) _cell_angle_beta 96.275(5) _cell_angle_gamma 98.166(5) _cell_volume 4913(3) _cell_formula_units_Z 2 _cell_measurement_temperature 100(2) _cell_measurement_reflns_used 9942 _cell_measurement_theta_min 2.25 _cell_measurement_theta_max 25.33 _exptl_crystal_description Block _exptl_crystal_colour Red _exptl_crystal_size_max 0.21 _exptl_crystal_size_mid 0.13 _exptl_crystal_size_min 0.09 _exptl_crystal_density_meas 'not measured' _exptl_crystal_density_diffrn 1.212 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1924 _exptl_absorpt_coefficient_mu 0.242 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.9510 _exptl_absorpt_correction_T_max 0.9786 _exptl_absorpt_process_details SADABS _exptl_special_details ; ? ; _diffrn_ambient_temperature 100(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'Bruker APEX CCD' _diffrn_measurement_method '\f and \w scans' _diffrn_reflns_number 61207 _diffrn_reflns_av_R_equivalents 0.0318 _diffrn_reflns_av_sigmaI/netI 0.0380 _diffrn_reflns_limit_h_min -15 _diffrn_reflns_limit_h_max 15 _diffrn_reflns_limit_k_min -19 _diffrn_reflns_limit_k_max 19 _diffrn_reflns_limit_l_min -29 _diffrn_reflns_limit_l_max 29 _diffrn_reflns_theta_min 0.84 _diffrn_reflns_theta_max 25.34 _reflns_number_total 17902 _reflns_number_gt 14377 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'Bruker APEX2' _computing_cell_refinement 'Bruker SAINT' _computing_data_reduction 'Bruker SAINT' _computing_structure_solution 'SHELXS-97 (Sheldrick, 2008)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 2008)' _computing_molecular_graphics 'Bruker SHELXTL' _computing_publication_material 'Bruker SHELXTL' _refine_special_details ; Refinement of F^2^ against ALL reflections. The weighted R-factor wR and goodness of fit S are based on F^2^, conventional R-factors R are based on F, with F set to zero for negative F^2^. The threshold expression of F^2^ > 2sigma(F^2^) is used only for calculating R-factors(gt) etc. and is not relevant to the choice of reflections for refinement. R-factors based on F^2^ are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger. ; _refine_ls_structure_factor_coef Fsqd _refine_ls_matrix_type full _refine_ls_weighting_scheme calc _refine_ls_weighting_details 'calc w=1/[\s^2^(Fo^2^)+(0.0365P)^2^+3.8105P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment constr _refine_ls_extinction_method none _refine_ls_number_reflns 17902 _refine_ls_number_parameters 1204 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0595 _refine_ls_R_factor_gt 0.0436 _refine_ls_wR_factor_ref 0.1066 _refine_ls_wR_factor_gt 0.0976 _refine_ls_goodness_of_fit_ref 1.050 _refine_ls_restrained_S_all 1.050 _refine_ls_shift/su_max 0.001 _refine_ls_shift/su_mean 0.000 loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_occupancy _atom_site_symmetry_multiplicity _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group Mn1 Mn 0.68652(2) 0.731372(18) 0.237752(12) 0.01577(8) Uani 1 1 d . . . C1 C 0.64661(16) 0.79003(12) 0.18044(8) 0.0175(4) Uani 1 1 d . . . C2 C 0.82475(16) 0.73394(11) 0.26610(8) 0.0171(4) Uani 1 1 d . . . C3 C 0.60650(16) 0.65991(12) 0.27704(8) 0.0184(4) Uani 1 1 d . . . C4 C 0.66984(16) 0.82187(13) 0.28677(8) 0.0190(4) Uani 1 1 d . . . C5 C 0.69242(16) 0.64099(13) 0.18593(9) 0.0203(5) Uani 1 1 d . . . C7 C 0.55707(16) 0.85463(12) 0.10193(8) 0.0185(4) Uani 1 1 d . . . C8 C 0.49762(16) 0.91985(12) 0.11681(8) 0.0190(4) Uani 1 1 d . . . C9 C 0.43236(18) 0.94807(13) 0.07572(9) 0.0251(5) Uani 1 1 d . . . H9 H 0.3915 0.9915 0.0855 0.030 Uiso 1 1 calc R . . C10 C 0.42584(19) 0.91426(14) 0.02109(9) 0.0297(5) Uani 1 1 d . . . H10 H 0.3808 0.9340 -0.0063 0.036 Uiso 1 1 calc R . . C11 C 0.48580(19) 0.85142(13) 0.00714(9) 0.0271(5) Uani 1 1 d . . . H11 H 0.4818 0.8285 -0.0303 0.033 Uiso 1 1 calc R . . C12 C 0.55203(17) 0.82057(12) 0.04636(8) 0.0205(4) Uani 1 1 d . . . C13 C 0.45479(16) 0.91225(13) 0.21320(9) 0.0211(4) Uani 1 1 d . . . C14 C 0.46221(17) 0.94927(14) 0.26714(9) 0.0255(5) Uani 1 1 d . . . H14 H 0.4283 0.9176 0.2926 0.031 Uiso 1 1 calc R . . C15 C 0.51751(18) 1.03109(14) 0.28522(9) 0.0268(5) Uani 1 1 d . . . C16 C 0.56072(17) 1.07782(13) 0.24654(9) 0.0245(5) Uani 1 1 d . . . H16 H 0.5955 1.1351 0.2578 0.029 Uiso 1 1 calc R . . C17 C 0.55485(16) 1.04367(13) 0.19176(9) 0.0208(4) Uani 1 1 d . . . C18 C 0.50336(16) 0.95889(12) 0.17495(8) 0.0187(4) Uani 1 1 d . . . C19 C 0.61464(17) 0.75278(13) 0.02761(8) 0.0213(5) Uani 1 1 d . . . C20 C 0.69598(18) 0.77230(14) -0.00447(9) 0.0261(5) Uani 1 1 d . . . C21 C 0.74793(19) 0.70722(15) -0.02516(9) 0.0304(5) Uani 1 1 d . . . H21 H 0.8029 0.7209 -0.0469 0.037 Uiso 1 1 calc R . . C22 C 0.72182(19) 0.62245(15) -0.01497(9) 0.0314(6) Uani 1 1 d . . . C23 C 0.64202(19) 0.60444(14) 0.01712(9) 0.0290(5) Uani 1 1 d . . . H23 H 0.6238 0.5470 0.0247 0.035 Uiso 1 1 calc R . . C24 C 0.58732(18) 0.66752(13) 0.03875(9) 0.0238(5) Uani 1 1 d . . . C25 C 0.7285(2) 0.86316(15) -0.01790(10) 0.0378(6) Uani 1 1 d . . . H25A H 0.7270 0.9046 0.0144 0.057 Uiso 1 1 calc R . . H25B H 0.6793 0.8746 -0.0484 0.057 Uiso 1 1 calc R . . H25C H 0.8002 0.8689 -0.0283 0.057 Uiso 1 1 calc R . . C26 C 0.7798(2) 0.55327(17) -0.03828(11) 0.0445(7) Uani 1 1 d . . . H26A H 0.7835 0.5574 -0.0773 0.067 Uiso 1 1 calc R . . H26B H 0.7420 0.4966 -0.0339 0.067 Uiso 1 1 calc R . . H26C H 0.8515 0.5609 -0.0187 0.067 Uiso 1 1 calc R . . C27 C 0.49823(18) 0.64311(13) 0.07134(9) 0.0277(5) Uani 1 1 d . . . H27A H 0.4397 0.6739 0.0610 0.042 Uiso 1 1 calc R . . H27B H 0.5230 0.6585 0.1106 0.042 Uiso 1 1 calc R . . H27C H 0.4739 0.5809 0.0637 0.042 Uiso 1 1 calc R . . C28 C 0.39446(18) 0.82244(13) 0.19618(9) 0.0262(5) Uani 1 1 d . . . H28A H 0.3537 0.8198 0.1600 0.039 Uiso 1 1 calc R . . H28B H 0.3463 0.8081 0.2231 0.039 Uiso 1 1 calc R . . H28C H 0.4443 0.7812 0.1944 0.039 Uiso 1 1 calc R . . C29 C 0.5347(2) 1.06573(18) 0.34527(10) 0.0424(7) Uani 1 1 d . . . H29A H 0.5596 1.1279 0.3495 0.064 Uiso 1 1 calc R . . H29B H 0.5878 1.0372 0.3645 0.064 Uiso 1 1 calc R . . H29C H 0.4680 1.0547 0.3608 0.064 Uiso 1 1 calc R . . C30 C 0.60512(19) 1.09768(14) 0.15203(10) 0.0296(5) Uani 1 1 d . . . H30A H 0.6492 1.1493 0.1724 0.044 Uiso 1 1 calc R . . H30B H 0.5498 1.1146 0.1268 0.044 Uiso 1 1 calc R . . H30C H 0.6491 1.0642 0.1310 0.044 Uiso 1 1 calc R . . C31 C 0.98898(16) 0.70288(12) 0.32036(8) 0.0185(4) Uani 1 1 d . . . C32 C 1.03482(16) 0.63223(12) 0.30038(8) 0.0189(4) Uani 1 1 d . . . C33 C 1.11172(17) 0.60346(13) 0.33496(9) 0.0236(5) Uani 1 1 d . . . H33 H 1.1438 0.5562 0.3216 0.028 Uiso 1 1 calc R . . C34 C 1.14220(18) 0.64248(14) 0.38843(9) 0.0276(5) Uani 1 1 d . . . H34 H 1.1937 0.6215 0.4117 0.033 Uiso 1 1 calc R . . C35 C 1.09697(17) 0.71222(13) 0.40751(9) 0.0257(5) Uani 1 1 d . . . H35 H 1.1174 0.7384 0.4443 0.031 Uiso 1 1 calc R . . C36 C 1.02226(16) 0.74513(12) 0.37418(9) 0.0206(4) Uani 1 1 d . . . C37 C 1.00479(16) 0.58832(12) 0.24276(8) 0.0186(4) Uani 1 1 d . . . C38 C 0.90972(16) 0.53003(12) 0.22840(9) 0.0191(4) Uani 1 1 d . . . C39 C 0.88759(17) 0.48711(13) 0.17514(9) 0.0227(5) Uani 1 1 d . . . H39 H 0.8234 0.4481 0.1652 0.027 Uiso 1 1 calc R . . C40 C 0.95634(18) 0.49954(13) 0.13630(9) 0.0246(5) Uani 1 1 d . . . C41 C 1.04917(18) 0.55806(13) 0.15127(9) 0.0237(5) Uani 1 1 d . . . H41 H 1.0970 0.5672 0.1250 0.028 Uiso 1 1 calc R . . C42 C 1.07362(17) 0.60339(12) 0.20352(9) 0.0212(5) Uani 1 1 d . . . C43 C 0.98133(17) 0.82424(13) 0.39512(8) 0.0213(5) Uani 1 1 d . . . C44 C 1.05117(18) 0.90321(13) 0.40580(9) 0.0246(5) Uani 1 1 d . . . C45 C 1.01215(19) 0.97699(14) 0.42518(9) 0.0285(5) Uani 1 1 d . . . H45 H 1.0594 1.0299 0.4333 0.034 Uiso 1 1 calc R . . C46 C 0.9070(2) 0.97617(14) 0.43299(9) 0.0289(5) Uani 1 1 d . . . C47 C 0.84043(19) 0.89719(15) 0.42371(9) 0.0286(5) Uani 1 1 d . . . H47 H 0.7687 0.8951 0.4300 0.034 Uiso 1 1 calc R . . C48 C 0.87592(18) 0.82124(13) 0.40553(8) 0.0234(5) Uani 1 1 d . . . C49 C 0.83220(17) 0.51409(13) 0.26903(9) 0.0229(5) Uani 1 1 d . . . H49A H 0.8706 0.5083 0.3046 0.034 Uiso 1 1 calc R . . H49B H 0.7828 0.4610 0.2558 0.034 Uiso 1 1 calc R . . H49C H 0.7928 0.5625 0.2731 0.034 Uiso 1 1 calc R . . C50 C 0.9316(2) 0.45145(17) 0.07892(10) 0.0391(6) Uani 1 1 d . . . H50A H 0.9599 0.4882 0.0527 0.059 Uiso 1 1 calc R . . H50B H 0.8549 0.4361 0.0695 0.059 Uiso 1 1 calc R . . H50C H 0.9641 0.3990 0.0774 0.059 Uiso 1 1 calc R . . C51 C 1.17082(18) 0.67118(14) 0.21642(10) 0.0285(5) Uani 1 1 d . . . H51A H 1.2190 0.6553 0.2458 0.043 Uiso 1 1 calc R . . H51B H 1.1501 0.7268 0.2283 0.043 Uiso 1 1 calc R . . H51C H 1.2064 0.6755 0.1835 0.043 Uiso 1 1 calc R . . C52 C 1.16576(18) 0.90926(14) 0.39681(10) 0.0312(5) Uani 1 1 d . . . H52A H 1.1716 0.8727 0.3630 0.047 Uiso 1 1 calc R . . H52B H 1.2059 0.8899 0.4279 0.047 Uiso 1 1 calc R . . H52C H 1.1943 0.9691 0.3937 0.047 Uiso 1 1 calc R . . C53 C 0.8656(2) 1.05839(16) 0.44914(11) 0.0404(6) Uani 1 1 d . . . H53A H 0.8006 1.0453 0.4659 0.061 Uiso 1 1 calc R . . H53B H 0.8504 1.0868 0.4164 0.061 Uiso 1 1 calc R . . H53C H 0.9188 1.0966 0.4755 0.061 Uiso 1 1 calc R . . C54 C 0.80023(18) 0.73768(14) 0.39811(9) 0.0273(5) Uani 1 1 d . . . H54A H 0.8400 0.6900 0.4026 0.041 Uiso 1 1 calc R . . H54B H 0.7605 0.7290 0.3613 0.041 Uiso 1 1 calc R . . H54C H 0.7510 0.7398 0.4256 0.041 Uiso 1 1 calc R . . C55 C 0.48802(16) 0.56132(12) 0.32767(8) 0.0187(4) Uani 1 1 d . . . C56 C 0.45482(16) 0.58709(13) 0.37846(8) 0.0200(4) Uani 1 1 d . . . C57 C 0.38109(17) 0.53021(13) 0.39906(9) 0.0234(5) Uani 1 1 d . . . H57 H 0.3589 0.5467 0.4335 0.028 Uiso 1 1 calc R . . C58 C 0.33895(18) 0.44995(14) 0.37069(9) 0.0265(5) Uani 1 1 d . . . H58 H 0.2874 0.4126 0.3851 0.032 Uiso 1 1 calc R . . C59 C 0.37306(17) 0.42528(13) 0.32115(9) 0.0247(5) Uani 1 1 d . . . H59 H 0.3447 0.3702 0.3018 0.030 Uiso 1 1 calc R . . C60 C 0.44777(16) 0.47883(13) 0.29878(8) 0.0206(4) Uani 1 1 d . . . C61 C 0.48572(16) 0.44803(12) 0.24629(8) 0.0199(4) Uani 1 1 d . . . C62 C 0.55300(16) 0.38569(12) 0.24605(9) 0.0222(5) Uani 1 1 d . . . C63 C 0.58710(17) 0.35614(13) 0.19683(9) 0.0242(5) Uani 1 1 d . . . H63 H 0.6338 0.3147 0.1970 0.029 Uiso 1 1 calc R . . C64 C 0.55492(17) 0.38535(13) 0.14756(9) 0.0242(5) Uani 1 1 d . . . C65 C 0.48635(17) 0.44563(13) 0.14863(9) 0.0233(5) Uani 1 1 d . . . H65 H 0.4617 0.4649 0.1151 0.028 Uiso 1 1 calc R . . C66 C 0.45248(16) 0.47882(12) 0.19687(9) 0.0209(5) Uani 1 1 d . . . C67 C 0.49697(16) 0.67301(13) 0.41093(8) 0.0204(4) Uani 1 1 d . . . C68 C 0.46701(17) 0.74857(13) 0.39323(9) 0.0241(5) Uani 1 1 d . . . C69 C 0.50331(19) 0.82703(14) 0.42539(10) 0.0300(5) Uani 1 1 d . . . H69 H 0.4837 0.8781 0.4130 0.036 Uiso 1 1 calc R . . C70 C 0.56740(19) 0.83292(14) 0.47501(10) 0.0307(5) Uani 1 1 d . . . C71 C 0.59618(18) 0.75801(15) 0.49209(9) 0.0286(5) Uani 1 1 d . . . H71 H 0.6399 0.7611 0.5260 0.034 Uiso 1 1 calc R . . C72 C 0.56271(17) 0.67823(14) 0.46080(9) 0.0238(5) Uani 1 1 d . . . C73 C 0.59094(19) 0.35164(15) 0.29813(10) 0.0319(5) Uani 1 1 d . . . H73A H 0.6151 0.3998 0.3273 0.048 Uiso 1 1 calc R . . H73B H 0.6496 0.3200 0.2918 0.048 Uiso 1 1 calc R . . H73C H 0.5328 0.3129 0.3092 0.048 Uiso 1 1 calc R . . C74 C 0.5958(2) 0.35595(16) 0.09519(9) 0.0339(6) Uani 1 1 d . . . H74A H 0.5370 0.3419 0.0654 0.051 Uiso 1 1 calc R . . H74B H 0.6291 0.3047 0.0998 0.051 Uiso 1 1 calc R . . H74C H 0.6481 0.4020 0.0862 0.051 Uiso 1 1 calc R . . C75 C 0.38253(18) 0.54720(13) 0.19594(9) 0.0246(5) Uani 1 1 d . . . H75A H 0.3306 0.5374 0.2217 0.037 Uiso 1 1 calc R . . H75B H 0.3457 0.5448 0.1588 0.037 Uiso 1 1 calc R . . H75C H 0.4257 0.6039 0.2067 0.037 Uiso 1 1 calc R . . C76 C 0.39547(19) 0.74542(15) 0.34018(10) 0.0312(5) Uani 1 1 d . . . H76A H 0.3445 0.6920 0.3343 0.047 Uiso 1 1 calc R . . H76B H 0.4380 0.7473 0.3096 0.047 Uiso 1 1 calc R . . H76C H 0.3574 0.7949 0.3421 0.047 Uiso 1 1 calc R . . C77 C 0.6044(2) 0.91864(16) 0.51027(11) 0.0459(7) Uani 1 1 d . . . H77A H 0.6676 0.9147 0.5352 0.069 Uiso 1 1 calc R . . H77B H 0.5483 0.9332 0.5317 0.069 Uiso 1 1 calc R . . H77C H 0.6212 0.9634 0.4867 0.069 Uiso 1 1 calc R . . C78 C 0.5995(2) 0.59943(15) 0.48140(10) 0.0331(6) Uani 1 1 d . . . H78A H 0.6071 0.5582 0.4501 0.050 Uiso 1 1 calc R . . H78B H 0.5474 0.5728 0.5031 0.050 Uiso 1 1 calc R . . H78C H 0.6678 0.6163 0.5044 0.050 Uiso 1 1 calc R . . C79 C 0.10588(18) 0.37920(13) 0.23615(10) 0.0279(5) Uani 1 1 d . . . H79A H 0.0540 0.3787 0.2034 0.033 Uiso 1 1 calc R . . H79B H 0.1521 0.4359 0.2426 0.033 Uiso 1 1 calc R . . C80 C 0.04930(18) 0.36587(13) 0.28471(9) 0.0261(5) Uani 1 1 d . . . H80A H 0.1005 0.3616 0.3169 0.031 Uiso 1 1 calc R . . H80B H 0.0121 0.4152 0.2937 0.031 Uiso 1 1 calc R . . C81 C -0.09242(18) 0.27737(14) 0.31352(10) 0.0283(5) Uani 1 1 d . . . H81A H -0.1341 0.3253 0.3167 0.034 Uiso 1 1 calc R . . H81B H -0.0496 0.2774 0.3494 0.034 Uiso 1 1 calc R . . C82 C -0.16481(18) 0.19367(14) 0.29826(10) 0.0287(5) Uani 1 1 d . . . H82A H -0.2163 0.1869 0.3250 0.034 Uiso 1 1 calc R . . H82B H -0.2045 0.1925 0.2615 0.034 Uiso 1 1 calc R . . C83 C -0.16849(18) 0.04316(14) 0.28080(10) 0.0291(5) Uani 1 1 d . . . H83A H -0.2023 0.0409 0.2426 0.035 Uiso 1 1 calc R . . H83B H -0.2249 0.0340 0.3047 0.035 Uiso 1 1 calc R . . C84 C -0.10019(18) -0.02552(14) 0.28429(10) 0.0286(5) Uani 1 1 d . . . H84A H -0.0647 -0.0222 0.3223 0.034 Uiso 1 1 calc R . . H84B H -0.1440 -0.0830 0.2744 0.034 Uiso 1 1 calc R . . C85 C 0.0482(2) -0.07392(15) 0.24997(11) 0.0371(6) Uani 1 1 d . . . H85A H 0.0084 -0.1327 0.2482 0.045 Uiso 1 1 calc R . . H85B H 0.0959 -0.0610 0.2851 0.045 Uiso 1 1 calc R . . C86 C 0.1114(2) -0.06896(14) 0.20294(11) 0.0368(6) Uani 1 1 d . . . H86A H 0.1583 -0.1135 0.2029 0.044 Uiso 1 1 calc R . . H86B H 0.0636 -0.0796 0.1679 0.044 Uiso 1 1 calc R . . C87 C 0.23439(18) 0.02180(14) 0.16393(10) 0.0283(5) Uani 1 1 d . . . H87A H 0.1873 0.0150 0.1288 0.034 Uiso 1 1 calc R . . H87B H 0.2797 -0.0238 0.1623 0.034 Uiso 1 1 calc R . . C88 C 0.30156(17) 0.10843(14) 0.17281(10) 0.0269(5) Uani 1 1 d . . . H88A H 0.3442 0.1173 0.2094 0.032 Uiso 1 1 calc R . . H88B H 0.3504 0.1127 0.1446 0.032 Uiso 1 1 calc R . . C89 C 0.29295(18) 0.25712(13) 0.17467(10) 0.0281(5) Uani 1 1 d . . . H89A H 0.3316 0.2642 0.1425 0.034 Uiso 1 1 calc R . . H89B H 0.3451 0.2671 0.2081 0.034 Uiso 1 1 calc R . . C90 C 0.21736(18) 0.31999(13) 0.17831(9) 0.0277(5) Uani 1 1 d . . . H90A H 0.2555 0.3792 0.1794 0.033 Uiso 1 1 calc R . . H90B H 0.1632 0.3081 0.1457 0.033 Uiso 1 1 calc R . . C91 C 1.1146(2) 0.26354(17) 0.87591(11) 0.0396(6) Uani 1 1 d . . . H91A H 1.1391 0.2312 0.8450 0.059 Uiso 0.727(9) 1 calc PR A 1 H91B H 1.1691 0.2722 0.9078 0.059 Uiso 0.727(9) 1 calc PR A 1 H91C H 1.1008 0.3195 0.8659 0.059 Uiso 0.727(9) 1 calc PR A 1 H91D H 1.1363 0.2289 0.8461 0.059 Uiso 0.273(9) 1 d PR A 2 H91E H 1.1755 0.2889 0.9014 0.059 Uiso 0.273(9) 1 d PR A 2 H91F H 1.0804 0.3082 0.8619 0.059 Uiso 0.273(9) 1 d PR A 2 C92 C 0.9797(2) 0.25774(17) 0.93297(11) 0.0428(7) Uani 1 1 d . . . H92A H 0.9584 0.3129 0.9241 0.051 Uiso 1 1 calc R A 1 H92B H 1.0323 0.2695 0.9663 0.051 Uiso 1 1 calc R A 1 C94 C 0.7547(2) 0.2825(2) 0.96887(12) 0.0505(7) Uani 1 1 d . . . H94A H 0.7755 0.3079 0.9364 0.076 Uiso 0.727(9) 1 calc PR A 1 H94B H 0.7542 0.3284 0.9988 0.076 Uiso 0.727(9) 1 calc PR A 1 H94C H 0.6839 0.2485 0.9599 0.076 Uiso 0.727(9) 1 calc PR A 1 H94D H 0.7310 0.2596 0.9313 0.076 Uiso 0.273(9) 1 d PR A 2 H94E H 0.7318 0.3372 0.9766 0.076 Uiso 0.273(9) 1 d PR A 2 H94F H 0.7256 0.2435 0.9925 0.076 Uiso 0.273(9) 1 d PR A 2 C95 C 0.3053(2) 0.17039(19) 0.32165(12) 0.0507(7) Uani 1 1 d . . . H95A H 0.3825 0.1857 0.3275 0.076 Uiso 1 1 calc R . . H95B H 0.2760 0.2016 0.2929 0.076 Uiso 1 1 calc R . . H95C H 0.2861 0.1083 0.3104 0.076 Uiso 1 1 calc R . . C96 C 0.1530(2) 0.17832(16) 0.36335(11) 0.0382(6) Uani 1 1 d . . . H96A H 0.1272 0.1159 0.3539 0.046 Uiso 1 1 calc R . . H96B H 0.1269 0.2082 0.3326 0.046 Uiso 1 1 calc R . . C97 C 0.1126(2) 0.21083(15) 0.41446(10) 0.0375(6) Uani 1 1 d . . . H97A H 0.0359 0.1896 0.4121 0.045 Uiso 1 1 calc R . . H97B H 0.1492 0.1894 0.4464 0.045 Uiso 1 1 calc R . . C98 C 0.0831(3) 0.3362(2) 0.46600(11) 0.0576(9) Uani 1 1 d . . . H98A H 0.1030 0.3989 0.4717 0.086 Uiso 1 1 calc R . . H98B H 0.1075 0.3123 0.4993 0.086 Uiso 1 1 calc R . . H98C H 0.0061 0.3214 0.4580 0.086 Uiso 1 1 calc R . . C99 C -0.1360(2) 0.24345(17) 0.12893(12) 0.0414(6) Uani 1 1 d . . . H99A H -0.1366 0.2913 0.1575 0.062 Uiso 1 1 calc R . . H99B H -0.1861 0.1936 0.1349 0.062 Uiso 1 1 calc R . . H99C H -0.1565 0.2608 0.0929 0.062 Uiso 1 1 calc R . . C100 C -0.0175(2) 0.16352(17) 0.08517(11) 0.0409(6) Uani 1 1 d . . . H10A H 0.0564 0.1523 0.0897 0.049 Uiso 1 1 calc R . . H10B H -0.0280 0.1918 0.0516 0.049 Uiso 1 1 calc R . . C101 C -0.0906(2) 0.07879(16) 0.07735(10) 0.0399(6) Uani 1 1 d . . . H10C H -0.1642 0.0878 0.0669 0.048 Uiso 1 1 calc R . . H10D H -0.0705 0.0395 0.0477 0.048 Uiso 1 1 calc R . . C102 C -0.1518(2) -0.03809(15) 0.12343(11) 0.0411(7) Uani 1 1 d . . . H10E H -0.1473 -0.0593 0.1593 0.062 Uiso 1 1 calc R . . H10F H -0.1306 -0.0801 0.0963 0.062 Uiso 1 1 calc R . . H10G H -0.2247 -0.0300 0.1122 0.062 Uiso 1 1 calc R . . C103 C 0.9497(2) 0.50810(17) 0.42765(11) 0.0428(7) Uani 1 1 d . . . H10H H 1.0159 0.5259 0.4524 0.064 Uiso 1 1 calc R B 1 H10I H 0.9217 0.5592 0.4171 0.064 Uiso 1 1 calc R B 1 H10J H 0.9632 0.4730 0.3947 0.064 Uiso 1 1 calc R B 1 C104 C 0.7788(2) 0.43291(18) 0.42118(11) 0.0424(6) Uani 1 1 d . . . H10K H 0.7919 0.4053 0.3852 0.051 Uiso 1 1 calc R C 1 H10L H 0.7450 0.4840 0.4148 0.051 Uiso 1 1 calc R C 1 C105 C 0.7059(2) 0.37134(17) 0.44633(11) 0.0397(6) Uani 1 1 d . F . H10M H 0.7028 0.3944 0.4849 0.048 Uiso 1 1 calc R D 1 H10N H 0.6339 0.3644 0.4262 0.048 Uiso 1 1 calc R D 1 C106 C 0.6746(2) 0.23282(19) 0.47189(14) 0.0525(8) Uani 1 1 d . . . H10O H 0.7000 0.1772 0.4700 0.079 Uiso 1 1 calc R E 1 H10P H 0.6017 0.2249 0.4538 0.079 Uiso 1 1 calc R E 1 H10Q H 0.6771 0.2565 0.5104 0.079 Uiso 1 1 calc R E 1 C93A C 0.8798(3) 0.1928(3) 0.94269(16) 0.0301(9) Uani 0.727(9) 1 d P A 1 H93A H 0.8295 0.1797 0.9085 0.036 Uiso 0.727(9) 1 calc PR A 1 H93B H 0.9025 0.1382 0.9518 0.036 Uiso 0.727(9) 1 calc PR A 1 C93B C 0.8860(9) 0.2415(12) 0.9354(5) 0.048(4) Uani 0.273(9) 1 d P A 2 H93C H 0.8681 0.1802 0.9406 0.057 Uiso 0.273(9) 1 calc PR A 2 H93D H 0.8469 0.2500 0.9001 0.057 Uiso 0.273(9) 1 calc PR A 2 K1 K 0.04473(4) 0.14446(3) 0.21896(2) 0.02393(11) Uani 1 1 d . . . N1 N 0.62511(14) 0.82705(10) 0.14150(7) 0.0191(4) Uani 1 1 d . . . N2 N 0.91397(13) 0.73377(10) 0.28586(7) 0.0177(4) Uani 1 1 d . . . N3 N 0.56218(14) 0.61518(10) 0.30609(7) 0.0208(4) Uani 1 1 d . . . O1 O 0.65932(12) 0.87844(9) 0.31855(6) 0.0266(3) Uani 1 1 d . . . O2 O 0.69592(12) 0.58506(9) 0.15229(6) 0.0273(4) Uani 1 1 d . . . O3 O 0.23417(11) 0.17218(9) 0.16928(6) 0.0250(3) Uani 1 1 d . . . O4 O 0.16787(12) 0.31273(9) 0.22687(6) 0.0240(3) Uani 1 1 d . . . O5 O -0.02514(12) 0.28827(9) 0.27203(6) 0.0253(3) Uani 1 1 d . . . O6 O -0.10451(12) 0.12530(9) 0.29791(6) 0.0262(3) Uani 1 1 d . . . O7 O -0.02307(12) -0.01342(9) 0.24731(6) 0.0263(3) Uani 1 1 d . . . O8 O 0.17317(12) 0.01427(9) 0.20806(6) 0.0273(3) Uani 1 1 d . . . O11 O 0.26370(15) 0.19304(12) 0.37131(8) 0.0465(5) Uani 1 1 d . . . O12 O 0.13049(15) 0.30150(10) 0.42137(7) 0.0401(4) Uani 1 1 d . . . O15 O -0.03245(13) 0.22112(10) 0.13109(7) 0.0360(4) Uani 1 1 d . . . O16 O -0.08299(14) 0.04231(10) 0.12706(7) 0.0384(4) Uani 1 1 d . . . O9A O 0.87497(16) 0.45900(14) 0.45476(9) 0.0379(7) Uani 0.898(5) 1 d P F 1 O10A O 0.74064(17) 0.29108(14) 0.44475(13) 0.0461(8) Uani 0.898(5) 1 d P F 1 O13A O 1.0227(8) 0.2179(6) 0.8887(3) 0.0420(16) Uani 0.727(9) 1 d P A 1 O14A O 0.8289(2) 0.2277(2) 0.98571(9) 0.0314(9) Uani 0.727(9) 1 d P A 1 O9B O 0.8719(14) 0.4202(11) 0.4177(9) 0.037(6) Uani 0.102(5) 1 d P F 2 O10B O 0.7396(14) 0.3205(13) 0.4833(8) 0.040(6) Uani 0.102(5) 1 d P F 2 O13B O 1.038(2) 0.2073(17) 0.9049(10) 0.061(7) Uani 0.273(9) 1 d P A 2 O14B O 0.8543(6) 0.2917(10) 0.9771(4) 0.065(5) Uani 0.273(9) 1 d P A 2 loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 Mn1 0.01477(16) 0.01503(14) 0.01728(16) 0.00354(12) 0.00067(12) 0.00142(12) C1 0.0169(10) 0.0155(9) 0.0194(10) -0.0020(8) 0.0043(8) 0.0020(8) C2 0.0235(12) 0.0105(9) 0.0168(10) 0.0007(7) 0.0044(8) 0.0005(8) C3 0.0175(11) 0.0173(9) 0.0187(10) -0.0016(8) -0.0023(8) 0.0028(8) C4 0.0156(10) 0.0211(10) 0.0215(11) 0.0085(9) 0.0015(8) 0.0028(8) C5 0.0162(11) 0.0229(10) 0.0224(11) 0.0096(9) -0.0008(8) 0.0027(8) C7 0.0193(11) 0.0156(9) 0.0198(10) 0.0049(8) 0.0003(8) -0.0001(8) C8 0.0190(11) 0.0172(9) 0.0202(11) 0.0040(8) 0.0005(8) 0.0007(8) C9 0.0275(12) 0.0224(10) 0.0266(12) 0.0041(9) 0.0012(9) 0.0094(9) C10 0.0374(14) 0.0285(11) 0.0238(12) 0.0057(9) -0.0061(10) 0.0128(10) C11 0.0371(14) 0.0250(11) 0.0183(11) 0.0015(9) -0.0039(10) 0.0081(10) C12 0.0256(12) 0.0168(9) 0.0184(10) 0.0023(8) 0.0007(9) 0.0028(9) C13 0.0173(11) 0.0233(10) 0.0243(11) 0.0053(9) 0.0019(9) 0.0070(9) C14 0.0237(12) 0.0339(12) 0.0229(11) 0.0096(9) 0.0067(9) 0.0106(10) C15 0.0246(12) 0.0336(12) 0.0230(12) -0.0003(9) 0.0003(9) 0.0122(10) C16 0.0202(11) 0.0225(10) 0.0292(12) -0.0040(9) -0.0007(9) 0.0066(9) C17 0.0156(11) 0.0217(10) 0.0255(11) 0.0026(9) 0.0022(9) 0.0054(8) C18 0.0150(10) 0.0201(10) 0.0217(11) 0.0035(8) 0.0001(8) 0.0068(8) C19 0.0273(12) 0.0212(10) 0.0141(10) -0.0007(8) -0.0039(9) 0.0065(9) C20 0.0323(13) 0.0280(11) 0.0172(11) 0.0007(9) 0.0009(9) 0.0053(10) C21 0.0334(14) 0.0374(13) 0.0208(11) -0.0003(10) 0.0018(10) 0.0106(11) C22 0.0344(14) 0.0349(13) 0.0237(12) -0.0039(10) -0.0057(10) 0.0142(11) C23 0.0382(14) 0.0191(10) 0.0269(12) -0.0012(9) -0.0094(10) 0.0082(10) C24 0.0286(12) 0.0205(10) 0.0198(11) 0.0004(8) -0.0058(9) 0.0037(9) C25 0.0515(17) 0.0322(13) 0.0307(13) 0.0063(10) 0.0126(12) 0.0030(12) C26 0.0527(18) 0.0440(15) 0.0391(15) -0.0054(12) 0.0002(13) 0.0272(14) C27 0.0276(13) 0.0200(10) 0.0338(13) 0.0047(9) -0.0037(10) 0.0024(9) C28 0.0226(12) 0.0251(11) 0.0315(12) 0.0093(9) 0.0043(9) 0.0004(9) C29 0.0504(17) 0.0496(15) 0.0272(13) -0.0041(11) 0.0011(12) 0.0175(13) C30 0.0297(13) 0.0227(11) 0.0348(13) 0.0028(10) 0.0058(10) -0.0017(10) C31 0.0149(10) 0.0174(9) 0.0225(11) 0.0052(8) 0.0001(8) 0.0005(8) C32 0.0150(10) 0.0158(9) 0.0245(11) 0.0024(8) 0.0009(8) -0.0011(8) C33 0.0212(11) 0.0186(10) 0.0305(12) 0.0013(9) -0.0011(9) 0.0059(9) C34 0.0244(12) 0.0262(11) 0.0309(12) 0.0043(9) -0.0070(10) 0.0075(9) C35 0.0249(12) 0.0261(11) 0.0240(11) 0.0006(9) -0.0041(9) 0.0042(9) C36 0.0179(11) 0.0185(10) 0.0245(11) 0.0029(8) 0.0007(9) 0.0014(8) C37 0.0195(11) 0.0134(9) 0.0230(11) 0.0019(8) -0.0009(8) 0.0059(8) C38 0.0183(11) 0.0133(9) 0.0262(11) 0.0034(8) 0.0002(9) 0.0052(8) C39 0.0205(11) 0.0170(10) 0.0285(12) 0.0014(9) -0.0039(9) 0.0025(8) C40 0.0281(12) 0.0223(10) 0.0233(11) 0.0014(9) -0.0004(9) 0.0078(9) C41 0.0257(12) 0.0227(10) 0.0254(11) 0.0060(9) 0.0068(9) 0.0078(9) C42 0.0199(11) 0.0168(9) 0.0277(12) 0.0041(8) 0.0011(9) 0.0060(8) C43 0.0239(12) 0.0222(10) 0.0174(10) 0.0000(8) -0.0020(9) 0.0070(9) C44 0.0269(12) 0.0235(11) 0.0214(11) -0.0012(9) -0.0024(9) 0.0046(9) C45 0.0371(14) 0.0211(11) 0.0250(12) -0.0022(9) -0.0011(10) 0.0040(10) C46 0.0405(14) 0.0284(11) 0.0199(11) 0.0010(9) 0.0032(10) 0.0141(11) C47 0.0306(13) 0.0368(13) 0.0206(11) 0.0015(10) 0.0041(9) 0.0134(11) C48 0.0269(12) 0.0271(11) 0.0163(10) 0.0013(8) 0.0005(9) 0.0073(9) C49 0.0207(11) 0.0183(10) 0.0278(12) 0.0025(9) -0.0002(9) -0.0002(9) C50 0.0435(16) 0.0439(14) 0.0260(13) -0.0054(11) 0.0025(11) 0.0021(12) C51 0.0232(12) 0.0230(11) 0.0391(14) 0.0026(10) 0.0068(10) 0.0017(9) C52 0.0292(13) 0.0244(11) 0.0367(14) -0.0010(10) -0.0012(10) 0.0004(10) C53 0.0554(18) 0.0330(13) 0.0374(15) 0.0020(11) 0.0110(13) 0.0201(12) C54 0.0241(12) 0.0327(12) 0.0253(12) 0.0050(9) 0.0044(9) 0.0033(10) C55 0.0153(10) 0.0196(10) 0.0209(10) 0.0068(8) 0.0016(8) -0.0004(8) C56 0.0172(11) 0.0221(10) 0.0207(11) 0.0057(8) 0.0011(8) 0.0017(8) C57 0.0227(12) 0.0281(11) 0.0200(11) 0.0063(9) 0.0038(9) 0.0019(9) C58 0.0219(12) 0.0285(11) 0.0271(12) 0.0078(9) 0.0030(9) -0.0059(9) C59 0.0238(12) 0.0231(11) 0.0241(11) 0.0032(9) -0.0008(9) -0.0040(9) C60 0.0198(11) 0.0195(10) 0.0211(11) 0.0044(8) -0.0005(8) -0.0004(8) C61 0.0192(11) 0.0149(9) 0.0222(11) 0.0004(8) 0.0001(8) -0.0057(8) C62 0.0185(11) 0.0173(10) 0.0279(12) 0.0027(9) -0.0027(9) -0.0028(8) C63 0.0196(11) 0.0176(10) 0.0330(12) -0.0024(9) -0.0016(9) 0.0025(9) C64 0.0199(11) 0.0216(10) 0.0262(12) -0.0049(9) -0.0010(9) -0.0042(9) C65 0.0236(12) 0.0220(10) 0.0211(11) 0.0019(8) -0.0030(9) -0.0029(9) C66 0.0178(11) 0.0162(9) 0.0259(11) 0.0017(8) -0.0007(9) -0.0036(8) C67 0.0203(11) 0.0243(10) 0.0170(10) 0.0028(8) 0.0075(8) 0.0002(9) C68 0.0236(12) 0.0264(11) 0.0230(11) 0.0056(9) 0.0066(9) 0.0020(9) C69 0.0354(14) 0.0224(11) 0.0343(13) 0.0050(10) 0.0124(11) 0.0048(10) C70 0.0325(13) 0.0286(12) 0.0292(13) -0.0042(10) 0.0128(10) -0.0029(10) C71 0.0270(12) 0.0371(13) 0.0189(11) -0.0016(9) 0.0027(9) -0.0012(10) C72 0.0225(12) 0.0284(11) 0.0203(11) 0.0028(9) 0.0058(9) 0.0013(9) C73 0.0302(13) 0.0324(12) 0.0329(13) 0.0083(10) -0.0024(10) 0.0062(10) C74 0.0357(14) 0.0353(13) 0.0281(13) -0.0078(10) 0.0022(11) 0.0068(11) C75 0.0262(12) 0.0215(10) 0.0257(12) 0.0037(9) 0.0014(9) 0.0033(9) C76 0.0336(14) 0.0285(12) 0.0330(13) 0.0110(10) 0.0020(10) 0.0064(10) C77 0.0533(18) 0.0362(14) 0.0433(16) -0.0124(12) 0.0138(13) -0.0029(13) C78 0.0326(14) 0.0357(13) 0.0295(13) 0.0069(10) -0.0040(10) 0.0040(11) C79 0.0279(13) 0.0174(10) 0.0378(13) 0.0039(9) 0.0019(10) 0.0029(9) C80 0.0271(12) 0.0164(10) 0.0333(13) 0.0004(9) 0.0014(10) 0.0029(9) C81 0.0264(12) 0.0265(11) 0.0332(13) 0.0014(10) 0.0070(10) 0.0077(10) C82 0.0221(12) 0.0271(11) 0.0374(13) 0.0031(10) 0.0049(10) 0.0054(10) C83 0.0229(12) 0.0254(11) 0.0371(13) 0.0033(10) 0.0053(10) -0.0034(9) C84 0.0268(12) 0.0233(11) 0.0361(13) 0.0085(10) 0.0076(10) -0.0012(9) C85 0.0343(14) 0.0260(12) 0.0569(17) 0.0158(11) 0.0144(12) 0.0102(11) C86 0.0378(15) 0.0196(11) 0.0569(17) 0.0078(11) 0.0160(12) 0.0077(10) C87 0.0266(12) 0.0282(11) 0.0330(13) 0.0044(10) 0.0080(10) 0.0102(10) C88 0.0202(12) 0.0314(12) 0.0313(12) 0.0038(10) 0.0061(9) 0.0096(10) C89 0.0213(12) 0.0257(11) 0.0351(13) 0.0011(10) 0.0061(10) -0.0034(9) C90 0.0270(12) 0.0212(11) 0.0331(13) 0.0038(9) 0.0056(10) -0.0041(9) C91 0.0353(15) 0.0423(14) 0.0419(15) 0.0088(12) 0.0082(12) 0.0025(12) C92 0.055(2) 0.0423(15) 0.0366(15) 0.0051(12) 0.0108(13) 0.0215(14) C94 0.0369(17) 0.0643(19) 0.0476(17) -0.0090(14) 0.0013(13) 0.0136(14) C95 0.0482(18) 0.0538(17) 0.0508(18) -0.0001(14) 0.0117(14) 0.0117(14) C96 0.0350(15) 0.0352(13) 0.0416(15) 0.0012(11) -0.0059(12) 0.0072(11) C97 0.0427(16) 0.0325(13) 0.0369(14) 0.0063(11) 0.0015(12) 0.0058(11) C98 0.082(2) 0.0633(19) 0.0332(16) 0.0005(14) 0.0038(15) 0.0372(18) C99 0.0318(14) 0.0412(14) 0.0505(17) 0.0083(12) 0.0034(12) 0.0023(12) C100 0.0411(16) 0.0448(15) 0.0377(15) 0.0118(12) 0.0080(12) 0.0028(12) C101 0.0474(16) 0.0404(14) 0.0292(13) 0.0022(11) 0.0001(12) 0.0032(12) C102 0.0468(17) 0.0293(12) 0.0409(15) 0.0021(11) -0.0066(12) -0.0046(12) C103 0.0499(17) 0.0382(14) 0.0404(15) 0.0139(12) 0.0021(13) 0.0033(13) C104 0.0412(17) 0.0515(16) 0.0369(15) 0.0055(12) 0.0034(12) 0.0167(13) C105 0.0367(15) 0.0551(16) 0.0302(14) 0.0008(12) 0.0061(11) 0.0187(13) C106 0.0370(16) 0.0487(17) 0.070(2) 0.0066(15) 0.0106(15) -0.0017(13) C93A 0.028(2) 0.029(2) 0.034(2) 0.0014(17) 0.0078(15) 0.0039(18) C93B 0.029(6) 0.064(10) 0.046(7) -0.016(7) 0.004(5) 0.012(7) K1 0.0230(2) 0.0186(2) 0.0306(3) 0.00359(18) 0.0053(2) 0.00263(18) N1 0.0221(9) 0.0174(8) 0.0176(9) 0.0014(7) -0.0001(7) 0.0052(7) N2 0.0152(9) 0.0163(8) 0.0209(9) 0.0005(7) -0.0005(7) 0.0032(7) N3 0.0228(10) 0.0181(8) 0.0200(9) 0.0011(7) 0.0041(7) -0.0026(7) O1 0.0296(9) 0.0235(8) 0.0270(8) 0.0000(7) 0.0032(7) 0.0078(7) O2 0.0299(9) 0.0228(8) 0.0273(8) -0.0039(7) 0.0005(7) 0.0055(7) O3 0.0194(8) 0.0209(7) 0.0335(9) 0.0013(6) 0.0031(7) 0.0010(6) O4 0.0241(8) 0.0179(7) 0.0298(8) 0.0020(6) 0.0029(6) 0.0039(6) O5 0.0242(8) 0.0227(7) 0.0277(8) -0.0006(6) 0.0040(6) 0.0011(6) O6 0.0223(8) 0.0204(7) 0.0350(9) 0.0027(6) 0.0032(7) 0.0006(6) O7 0.0239(8) 0.0219(7) 0.0354(9) 0.0095(7) 0.0068(7) 0.0046(6) O8 0.0242(8) 0.0235(7) 0.0357(9) 0.0051(7) 0.0089(7) 0.0040(6) O11 0.0405(11) 0.0560(11) 0.0404(11) -0.0027(9) -0.0023(9) 0.0112(9) O12 0.0518(12) 0.0316(9) 0.0365(10) -0.0012(8) 0.0045(8) 0.0101(8) O15 0.0333(10) 0.0338(9) 0.0401(10) 0.0085(8) 0.0009(8) 0.0023(8) O16 0.0443(11) 0.0315(9) 0.0337(10) 0.0055(7) -0.0066(8) -0.0057(8) O9A 0.0444(13) 0.0404(12) 0.0264(13) 0.0049(10) -0.0005(9) 0.0011(9) O10A 0.0369(12) 0.0398(12) 0.063(2) -0.0005(12) 0.0196(12) 0.0078(10) O13A 0.039(2) 0.040(4) 0.043(3) -0.012(2) 0.023(2) -0.009(2) O14A 0.0263(14) 0.044(2) 0.0259(13) 0.0048(11) 0.0035(10) 0.0105(13) O9B 0.046(12) 0.023(9) 0.044(14) 0.001(9) 0.028(9) -0.005(8) O10B 0.036(10) 0.053(12) 0.023(11) 0.014(9) -0.010(8) -0.015(9) O13B 0.079(15) 0.032(5) 0.088(16) 0.014(9) 0.069(12) 0.012(7) O14B 0.031(5) 0.107(12) 0.048(5) -0.024(6) 0.000(4) 0.009(5) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag Mn1 C4 1.826(2) . ? Mn1 C5 1.830(2) . ? Mn1 C2 1.834(2) . ? Mn1 C1 1.841(2) . ? Mn1 C3 1.845(2) . ? C1 N1 1.206(3) . ? C2 N2 1.199(3) . ? C3 N3 1.194(3) . ? C4 O1 1.159(2) . ? C5 O2 1.156(2) . ? C7 N1 1.388(2) . ? C7 C12 1.411(3) . ? C7 C8 1.411(3) . ? C8 C9 1.398(3) . ? C8 C18 1.491(3) . ? C9 C10 1.386(3) . ? C9 H9 0.9500 . ? C10 C11 1.381(3) . ? C10 H10 0.9500 . ? C11 C12 1.394(3) . ? C11 H11 0.9500 . ? C12 C19 1.495(3) . ? C13 C14 1.384(3) . ? C13 C18 1.406(3) . ? C13 C28 1.512(3) . ? C14 C15 1.388(3) . ? C14 H14 0.9500 . ? C15 C16 1.386(3) . ? C15 C29 1.506(3) . ? C16 C17 1.392(3) . ? C16 H16 0.9500 . ? C17 C18 1.406(3) . ? C17 C30 1.508(3) . ? C19 C20 1.401(3) . ? C19 C24 1.409(3) . ? C20 C21 1.388(3) . ? C20 C25 1.521(3) . ? C21 C22 1.392(3) . ? C21 H21 0.9500 . ? C22 C23 1.382(4) . ? C22 C26 1.509(3) . ? C23 C24 1.395(3) . ? C23 H23 0.9500 . ? C24 C27 1.502(3) . ? C25 H25A 0.9800 . ? C25 H25B 0.9800 . ? C25 H25C 0.9800 . ? C26 H26A 0.9800 . ? C26 H26B 0.9800 . ? C26 H26C 0.9800 . ? C27 H27A 0.9800 . ? C27 H27B 0.9800 . ? C27 H27C 0.9800 . ? C28 H28A 0.9800 . ? C28 H28B 0.9800 . ? C28 H28C 0.9800 . ? C29 H29A 0.9800 . ? C29 H29B 0.9800 . ? C29 H29C 0.9800 . ? C30 H30A 0.9800 . ? C30 H30B 0.9800 . ? C30 H30C 0.9800 . ? C31 N2 1.394(2) . ? C31 C32 1.405(3) . ? C31 C36 1.415(3) . ? C32 C33 1.395(3) . ? C32 C37 1.499(3) . ? C33 C34 1.386(3) . ? C33 H33 0.9500 . ? C34 C35 1.382(3) . ? C34 H34 0.9500 . ? C35 C36 1.391(3) . ? C35 H35 0.9500 . ? C36 C43 1.490(3) . ? C37 C42 1.400(3) . ? C37 C38 1.410(3) . ? C38 C39 1.394(3) . ? C38 C49 1.507(3) . ? C39 C40 1.386(3) . ? C39 H39 0.9500 . ? C40 C41 1.392(3) . ? C40 C50 1.513(3) . ? C41 C42 1.388(3) . ? C41 H41 0.9500 . ? C42 C51 1.509(3) . ? C43 C48 1.404(3) . ? C43 C44 1.413(3) . ? C44 C45 1.394(3) . ? C44 C52 1.508(3) . ? C45 C46 1.388(3) . ? C45 H45 0.9500 . ? C46 C47 1.393(3) . ? C46 C53 1.506(3) . ? C47 C48 1.393(3) . ? C47 H47 0.9500 . ? C48 C54 1.508(3) . ? C49 H49A 0.9800 . ? C49 H49B 0.9800 . ? C49 H49C 0.9800 . ? C50 H50A 0.9800 . ? C50 H50B 0.9800 . ? C50 H50C 0.9800 . ? C51 H51A 0.9800 . ? C51 H51B 0.9800 . ? C51 H51C 0.9800 . ? C52 H52A 0.9800 . ? C52 H52B 0.9800 . ? C52 H52C 0.9800 . ? C53 H53A 0.9800 . ? C53 H53B 0.9800 . ? C53 H53C 0.9800 . ? C54 H54A 0.9800 . ? C54 H54B 0.9800 . ? C54 H54C 0.9800 . ? C55 N3 1.378(3) . ? C55 C56 1.407(3) . ? C55 C60 1.417(3) . ? C56 C57 1.390(3) . ? C56 C67 1.499(3) . ? C57 C58 1.388(3) . ? C57 H57 0.9500 . ? C58 C59 1.381(3) . ? C58 H58 0.9500 . ? C59 C60 1.391(3) . ? C59 H59 0.9500 . ? C60 C61 1.493(3) . ? C61 C62 1.402(3) . ? C61 C66 1.408(3) . ? C62 C63 1.394(3) . ? C62 C73 1.507(3) . ? C63 C64 1.390(3) . ? C63 H63 0.9500 . ? C64 C65 1.389(3) . ? C64 C74 1.502(3) . ? C65 C66 1.389(3) . ? C65 H65 0.9500 . ? C66 C75 1.503(3) . ? C67 C72 1.404(3) . ? C67 C68 1.405(3) . ? C68 C69 1.390(3) . ? C68 C76 1.509(3) . ? C69 C70 1.387(3) . ? C69 H69 0.9500 . ? C70 C71 1.385(3) . ? C70 C77 1.515(3) . ? C71 C72 1.392(3) . ? C71 H71 0.9500 . ? C72 C78 1.513(3) . ? C73 H73A 0.9800 . ? C73 H73B 0.9800 . ? C73 H73C 0.9800 . ? C74 H74A 0.9800 . ? C74 H74B 0.9800 . ? C74 H74C 0.9800 . ? C75 H75A 0.9800 . ? C75 H75B 0.9800 . ? C75 H75C 0.9800 . ? C76 H76A 0.9800 . ? C76 H76B 0.9800 . ? C76 H76C 0.9800 . ? C77 H77A 0.9800 . ? C77 H77B 0.9800 . ? C77 H77C 0.9800 . ? C78 H78A 0.9800 . ? C78 H78B 0.9800 . ? C78 H78C 0.9800 . ? C79 O4 1.422(3) . ? C79 C80 1.489(3) . ? C79 H79A 0.9900 . ? C79 H79B 0.9900 . ? C80 O5 1.429(2) . ? C80 H80A 0.9900 . ? C80 H80B 0.9900 . ? C81 O5 1.422(3) . ? C81 C82 1.493(3) . ? C81 H81A 0.9900 . ? C81 H81B 0.9900 . ? C82 O6 1.418(3) . ? C82 H82A 0.9900 . ? C82 H82B 0.9900 . ? C83 O6 1.431(2) . ? C83 C84 1.496(3) . ? C83 H83A 0.9900 . ? C83 H83B 0.9900 . ? C84 O7 1.428(3) . ? C84 H84A 0.9900 . ? C84 H84B 0.9900 . ? C85 O7 1.419(3) . ? C85 C86 1.492(4) . ? C85 H85A 0.9900 . ? C85 H85B 0.9900 . ? C86 O8 1.424(3) . ? C86 H86A 0.9900 . ? C86 H86B 0.9900 . ? C87 O8 1.419(3) . ? C87 C88 1.494(3) . ? C87 H87A 0.9900 . ? C87 H87B 0.9900 . ? C88 O3 1.424(3) . ? C88 H88A 0.9900 . ? C88 H88B 0.9900 . ? C89 O3 1.431(2) . ? C89 C90 1.490(3) . ? C89 H89A 0.9900 . ? C89 H89B 0.9900 . ? C90 O4 1.426(3) . ? C90 H90A 0.9900 . ? C90 H90B 0.9900 . ? C91 O13A 1.383(10) . ? C91 O13B 1.52(3) . ? C91 H91A 0.9800 . ? C91 H91B 0.9800 . ? C91 H91C 0.9800 . ? C91 H91D 0.9600 . ? C91 H91E 0.9600 . ? C91 H91F 0.9600 . ? C92 C93B 1.207(12) . ? C92 O13B 1.36(3) . ? C92 O13A 1.407(11) . ? C92 C93A 1.586(5) . ? C92 H92A 0.9900 . ? C92 H92B 0.9900 . ? C94 O14B 1.261(8) . ? C94 O14A 1.436(4) . ? C94 H94A 0.9800 . ? C94 H94B 0.9800 . ? C94 H94C 0.9800 . ? C94 H94D 0.9600 . ? C94 H94E 0.9600 . ? C94 H94F 0.9600 . ? C95 O11 1.423(3) . ? C95 H95A 0.9800 . ? C95 H95B 0.9800 . ? C95 H95C 0.9800 . ? C96 O11 1.400(3) . ? C96 C97 1.487(4) . ? C96 H96A 0.9900 . ? C96 H96B 0.9900 . ? C97 O12 1.409(3) . ? C97 H97A 0.9900 . ? C97 H97B 0.9900 . ? C98 O12 1.414(3) . ? C98 H98A 0.9800 . ? C98 H98B 0.9800 . ? C98 H98C 0.9800 . ? C99 O15 1.424(3) . ? C99 H99A 0.9800 . ? C99 H99B 0.9800 . ? C99 H99C 0.9800 . ? C100 O15 1.424(3) . ? C100 C101 1.505(4) . ? C100 H10A 0.9900 . ? C100 H10B 0.9900 . ? C101 O16 1.411(3) . ? C101 H10C 0.9900 . ? C101 H10D 0.9900 . ? C102 O16 1.432(3) . ? C102 H10E 0.9800 . ? C102 H10F 0.9800 . ? C102 H10G 0.9800 . ? C103 O9A 1.421(3) . ? C103 O9B 1.573(16) . ? C103 H10H 0.9800 . ? C103 H10I 0.9800 . ? C103 H10J 0.9800 . ? C104 O9B 1.255(18) . ? C104 O9A 1.396(3) . ? C104 C105 1.488(4) . ? C104 H10K 0.9900 . ? C104 H10L 0.9900 . ? C105 O10B 1.356(16) . ? C105 O10A 1.403(3) . ? C105 H10M 0.9900 . ? C105 H10N 0.9900 . ? C106 O10A 1.434(4) . ? C106 O10B 1.496(18) . ? C106 H10O 0.9800 . ? C106 H10P 0.9800 . ? C106 H10Q 0.9800 . ? C93A O14A 1.412(5) . ? C93A H93A 0.9900 . ? C93A H93B 0.9900 . ? C93B O14B 1.368(14) . ? C93B H93C 0.9900 . ? C93B H93D 0.9900 . ? K1 O7 2.7169(16) . ? K1 O5 2.8110(17) . ? K1 O8 2.8279(17) . ? K1 O3 2.8493(18) . ? K1 O4 2.8741(16) . ? K1 O6 2.8933(18) . ? O14A H94F 1.4126 . ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag C4 Mn1 C5 175.34(9) . . ? C4 Mn1 C2 92.91(9) . . ? C5 Mn1 C2 91.74(9) . . ? C4 Mn1 C1 90.18(9) . . ? C5 Mn1 C1 86.90(9) . . ? C2 Mn1 C1 123.22(9) . . ? C4 Mn1 C3 88.13(9) . . ? C5 Mn1 C3 91.02(9) . . ? C2 Mn1 C3 106.11(9) . . ? C1 Mn1 C3 130.65(9) . . ? N1 C1 Mn1 176.34(19) . . ? N2 C2 Mn1 177.78(18) . . ? N3 C3 Mn1 174.14(17) . . ? O1 C4 Mn1 178.88(17) . . ? O2 C5 Mn1 178.49(17) . . ? N1 C7 C12 119.68(18) . . ? N1 C7 C8 120.10(18) . . ? C12 C7 C8 120.12(18) . . ? C9 C8 C7 118.68(19) . . ? C9 C8 C18 119.83(19) . . ? C7 C8 C18 121.49(17) . . ? C10 C9 C8 121.6(2) . . ? C10 C9 H9 119.2 . . ? C8 C9 H9 119.2 . . ? C11 C10 C9 118.92(19) . . ? C11 C10 H10 120.5 . . ? C9 C10 H10 120.5 . . ? C10 C11 C12 122.0(2) . . ? C10 C11 H11 119.0 . . ? C12 C11 H11 119.0 . . ? C11 C12 C7 118.63(19) . . ? C11 C12 C19 118.46(18) . . ? C7 C12 C19 122.91(17) . . ? C14 C13 C18 119.43(19) . . ? C14 C13 C28 119.6(2) . . ? C18 C13 C28 120.92(19) . . ? C13 C14 C15 122.2(2) . . ? C13 C14 H14 118.9 . . ? C15 C14 H14 118.9 . . ? C16 C15 C14 117.7(2) . . ? C16 C15 C29 121.3(2) . . ? C14 C15 C29 120.9(2) . . ? C15 C16 C17 122.2(2) . . ? C15 C16 H16 118.9 . . ? C17 C16 H16 118.9 . . ? C16 C17 C18 119.0(2) . . ? C16 C17 C30 119.42(19) . . ? C18 C17 C30 121.53(19) . . ? C13 C18 C17 119.28(19) . . ? C13 C18 C8 120.35(18) . . ? C17 C18 C8 120.34(19) . . ? C20 C19 C24 119.5(2) . . ? C20 C19 C12 120.14(19) . . ? C24 C19 C12 120.2(2) . . ? C21 C20 C19 119.5(2) . . ? C21 C20 C25 118.8(2) . . ? C19 C20 C25 121.7(2) . . ? C20 C21 C22 121.9(2) . . ? C20 C21 H21 119.0 . . ? C22 C21 H21 119.0 . . ? C23 C22 C21 117.8(2) . . ? C23 C22 C26 121.7(2) . . ? C21 C22 C26 120.5(3) . . ? C22 C23 C24 122.4(2) . . ? C22 C23 H23 118.8 . . ? C24 C23 H23 118.8 . . ? C23 C24 C19 118.8(2) . . ? C23 C24 C27 119.82(19) . . ? C19 C24 C27 121.3(2) . . ? C20 C25 H25A 109.5 . . ? C20 C25 H25B 109.5 . . ? H25A C25 H25B 109.5 . . ? C20 C25 H25C 109.5 . . ? H25A C25 H25C 109.5 . . ? H25B C25 H25C 109.5 . . ? C22 C26 H26A 109.5 . . ? C22 C26 H26B 109.5 . . ? H26A C26 H26B 109.5 . . ? C22 C26 H26C 109.5 . . ? H26A C26 H26C 109.5 . . ? H26B C26 H26C 109.5 . . ? C24 C27 H27A 109.5 . . ? C24 C27 H27B 109.5 . . ? H27A C27 H27B 109.5 . . ? C24 C27 H27C 109.5 . . ? H27A C27 H27C 109.5 . . ? H27B C27 H27C 109.5 . . ? C13 C28 H28A 109.5 . . ? C13 C28 H28B 109.5 . . ? H28A C28 H28B 109.5 . . ? C13 C28 H28C 109.5 . . ? H28A C28 H28C 109.5 . . ? H28B C28 H28C 109.5 . . ? C15 C29 H29A 109.5 . . ? C15 C29 H29B 109.5 . . ? H29A C29 H29B 109.5 . . ? C15 C29 H29C 109.5 . . ? H29A C29 H29C 109.5 . . ? H29B C29 H29C 109.5 . . ? C17 C30 H30A 109.5 . . ? C17 C30 H30B 109.5 . . ? H30A C30 H30B 109.5 . . ? C17 C30 H30C 109.5 . . ? H30A C30 H30C 109.5 . . ? H30B C30 H30C 109.5 . . ? N2 C31 C32 119.49(18) . . ? N2 C31 C36 120.04(18) . . ? C32 C31 C36 120.40(18) . . ? C33 C32 C31 118.80(19) . . ? C33 C32 C37 119.38(18) . . ? C31 C32 C37 121.81(17) . . ? C34 C33 C32 121.3(2) . . ? C34 C33 H33 119.4 . . ? C32 C33 H33 119.4 . . ? C35 C34 C33 119.38(19) . . ? C35 C34 H34 120.3 . . ? C33 C34 H34 120.3 . . ? C34 C35 C36 121.7(2) . . ? C34 C35 H35 119.2 . . ? C36 C35 H35 119.2 . . ? C35 C36 C31 118.40(19) . . ? C35 C36 C43 119.86(18) . . ? C31 C36 C43 121.73(18) . . ? C42 C37 C38 119.98(19) . . ? C42 C37 C32 119.46(18) . . ? C38 C37 C32 120.53(19) . . ? C39 C38 C37 118.7(2) . . ? C39 C38 C49 119.85(18) . . ? C37 C38 C49 121.50(18) . . ? C40 C39 C38 122.0(2) . . ? C40 C39 H39 119.0 . . ? C38 C39 H39 119.0 . . ? C39 C40 C41 118.3(2) . . ? C39 C40 C50 121.3(2) . . ? C41 C40 C50 120.5(2) . . ? C42 C41 C40 121.7(2) . . ? C42 C41 H41 119.1 . . ? C40 C41 H41 119.1 . . ? C41 C42 C37 119.32(19) . . ? C41 C42 C51 119.7(2) . . ? C37 C42 C51 120.90(19) . . ? C48 C43 C44 119.8(2) . . ? C48 C43 C36 121.29(19) . . ? C44 C43 C36 118.9(2) . . ? C45 C44 C43 118.6(2) . . ? C45 C44 C52 119.7(2) . . ? C43 C44 C52 121.7(2) . . ? C46 C45 C44 122.5(2) . . ? C46 C45 H45 118.7 . . ? C44 C45 H45 118.7 . . ? C45 C46 C47 117.8(2) . . ? C45 C46 C53 121.0(2) . . ? C47 C46 C53 121.2(2) . . ? C46 C47 C48 122.0(2) . . ? C46 C47 H47 119.0 . . ? C48 C47 H47 119.0 . . ? C47 C48 C43 119.3(2) . . ? C47 C48 C54 119.0(2) . . ? C43 C48 C54 121.72(19) . . ? C38 C49 H49A 109.5 . . ? C38 C49 H49B 109.5 . . ? H49A C49 H49B 109.5 . . ? C38 C49 H49C 109.5 . . ? H49A C49 H49C 109.5 . . ? H49B C49 H49C 109.5 . . ? C40 C50 H50A 109.5 . . ? C40 C50 H50B 109.5 . . ? H50A C50 H50B 109.5 . . ? C40 C50 H50C 109.5 . . ? H50A C50 H50C 109.5 . . ? H50B C50 H50C 109.5 . . ? C42 C51 H51A 109.5 . . ? C42 C51 H51B 109.5 . . ? H51A C51 H51B 109.5 . . ? C42 C51 H51C 109.5 . . ? H51A C51 H51C 109.5 . . ? H51B C51 H51C 109.5 . . ? C44 C52 H52A 109.5 . . ? C44 C52 H52B 109.5 . . ? H52A C52 H52B 109.5 . . ? C44 C52 H52C 109.5 . . ? H52A C52 H52C 109.5 . . ? H52B C52 H52C 109.5 . . ? C46 C53 H53A 109.5 . . ? C46 C53 H53B 109.5 . . ? H53A C53 H53B 109.5 . . ? C46 C53 H53C 109.5 . . ? H53A C53 H53C 109.5 . . ? H53B C53 H53C 109.5 . . ? C48 C54 H54A 109.5 . . ? C48 C54 H54B 109.5 . . ? H54A C54 H54B 109.5 . . ? C48 C54 H54C 109.5 . . ? H54A C54 H54C 109.5 . . ? H54B C54 H54C 109.5 . . ? N3 C55 C56 120.38(17) . . ? N3 C55 C60 119.16(19) . . ? C56 C55 C60 120.44(19) . . ? C57 C56 C55 118.43(18) . . ? C57 C56 C67 119.36(19) . . ? C55 C56 C67 122.21(18) . . ? C58 C57 C56 121.9(2) . . ? C58 C57 H57 119.0 . . ? C56 C57 H57 119.0 . . ? C59 C58 C57 119.0(2) . . ? C59 C58 H58 120.5 . . ? C57 C58 H58 120.5 . . ? C58 C59 C60 121.81(19) . . ? C58 C59 H59 119.1 . . ? C60 C59 H59 119.1 . . ? C59 C60 C55 118.4(2) . . ? C59 C60 C61 119.97(18) . . ? C55 C60 C61 121.59(18) . . ? C62 C61 C66 119.7(2) . . ? C62 C61 C60 119.35(18) . . ? C66 C61 C60 120.95(19) . . ? C63 C62 C61 119.23(19) . . ? C63 C62 C73 119.5(2) . . ? C61 C62 C73 121.3(2) . . ? C64 C63 C62 122.0(2) . . ? C64 C63 H63 119.0 . . ? C62 C63 H63 119.0 . . ? C65 C64 C63 117.7(2) . . ? C65 C64 C74 120.7(2) . . ? C63 C64 C74 121.6(2) . . ? C64 C65 C66 122.44(19) . . ? C64 C65 H65 118.8 . . ? C66 C65 H65 118.8 . . ? C65 C66 C61 118.91(19) . . ? C65 C66 C75 120.08(18) . . ? C61 C66 C75 121.01(19) . . ? C72 C67 C68 119.37(19) . . ? C72 C67 C56 120.11(18) . . ? C68 C67 C56 120.44(18) . . ? C69 C68 C67 119.3(2) . . ? C69 C68 C76 119.8(2) . . ? C67 C68 C76 120.90(19) . . ? C70 C69 C68 121.9(2) . . ? C70 C69 H69 119.1 . . ? C68 C69 H69 119.1 . . ? C71 C70 C69 118.3(2) . . ? C71 C70 C77 120.4(2) . . ? C69 C70 C77 121.3(2) . . ? C70 C71 C72 121.7(2) . . ? C70 C71 H71 119.1 . . ? C72 C71 H71 119.1 . . ? C71 C72 C67 119.4(2) . . ? C71 C72 C78 118.76(19) . . ? C67 C72 C78 121.79(19) . . ? C62 C73 H73A 109.5 . . ? C62 C73 H73B 109.5 . . ? H73A C73 H73B 109.5 . . ? C62 C73 H73C 109.5 . . ? H73A C73 H73C 109.5 . . ? H73B C73 H73C 109.5 . . ? C64 C74 H74A 109.5 . . ? C64 C74 H74B 109.5 . . ? H74A C74 H74B 109.5 . . ? C64 C74 H74C 109.5 . . ? H74A C74 H74C 109.5 . . ? H74B C74 H74C 109.5 . . ? C66 C75 H75A 109.5 . . ? C66 C75 H75B 109.5 . . ? H75A C75 H75B 109.5 . . ? C66 C75 H75C 109.5 . . ? H75A C75 H75C 109.5 . . ? H75B C75 H75C 109.5 . . ? C68 C76 H76A 109.5 . . ? C68 C76 H76B 109.5 . . ? H76A C76 H76B 109.5 . . ? C68 C76 H76C 109.5 . . ? H76A C76 H76C 109.5 . . ? H76B C76 H76C 109.5 . . ? C70 C77 H77A 109.5 . . ? C70 C77 H77B 109.5 . . ? H77A C77 H77B 109.5 . . ? C70 C77 H77C 109.5 . . ? H77A C77 H77C 109.5 . . ? H77B C77 H77C 109.5 . . ? C72 C78 H78A 109.5 . . ? C72 C78 H78B 109.5 . . ? H78A C78 H78B 109.5 . . ? C72 C78 H78C 109.5 . . ? H78A C78 H78C 109.5 . . ? H78B C78 H78C 109.5 . . ? O4 C79 C80 109.68(17) . . ? O4 C79 H79A 109.7 . . ? C80 C79 H79A 109.7 . . ? O4 C79 H79B 109.7 . . ? C80 C79 H79B 109.7 . . ? H79A C79 H79B 108.2 . . ? O5 C80 C79 108.59(17) . . ? O5 C80 H80A 110.0 . . ? C79 C80 H80A 110.0 . . ? O5 C80 H80B 110.0 . . ? C79 C80 H80B 110.0 . . ? H80A C80 H80B 108.4 . . ? O5 C81 C82 108.45(19) . . ? O5 C81 H81A 110.0 . . ? C82 C81 H81A 110.0 . . ? O5 C81 H81B 110.0 . . ? C82 C81 H81B 110.0 . . ? H81A C81 H81B 108.4 . . ? O6 C82 C81 109.30(18) . . ? O6 C82 H82A 109.8 . . ? C81 C82 H82A 109.8 . . ? O6 C82 H82B 109.8 . . ? C81 C82 H82B 109.8 . . ? H82A C82 H82B 108.3 . . ? O6 C83 C84 108.99(18) . . ? O6 C83 H83A 109.9 . . ? C84 C83 H83A 109.9 . . ? O6 C83 H83B 109.9 . . ? C84 C83 H83B 109.9 . . ? H83A C83 H83B 108.3 . . ? O7 C84 C83 108.75(18) . . ? O7 C84 H84A 109.9 . . ? C83 C84 H84A 109.9 . . ? O7 C84 H84B 109.9 . . ? C83 C84 H84B 109.9 . . ? H84A C84 H84B 108.3 . . ? O7 C85 C86 108.96(19) . . ? O7 C85 H85A 109.9 . . ? C86 C85 H85A 109.9 . . ? O7 C85 H85B 109.9 . . ? C86 C85 H85B 109.9 . . ? H85A C85 H85B 108.3 . . ? O8 C86 C85 109.1(2) . . ? O8 C86 H86A 109.9 . . ? C85 C86 H86A 109.9 . . ? O8 C86 H86B 109.9 . . ? C85 C86 H86B 109.9 . . ? H86A C86 H86B 108.3 . . ? O8 C87 C88 108.72(19) . . ? O8 C87 H87A 109.9 . . ? C88 C87 H87A 109.9 . . ? O8 C87 H87B 109.9 . . ? C88 C87 H87B 109.9 . . ? H87A C87 H87B 108.3 . . ? O3 C88 C87 108.49(18) . . ? O3 C88 H88A 110.0 . . ? C87 C88 H88A 110.0 . . ? O3 C88 H88B 110.0 . . ? C87 C88 H88B 110.0 . . ? H88A C88 H88B 108.4 . . ? O3 C89 C90 108.30(18) . . ? O3 C89 H89A 110.0 . . ? C90 C89 H89A 110.0 . . ? O3 C89 H89B 110.0 . . ? C90 C89 H89B 110.0 . . ? H89A C89 H89B 108.4 . . ? O4 C90 C89 109.10(18) . . ? O4 C90 H90A 109.9 . . ? C89 C90 H90A 109.9 . . ? O4 C90 H90B 109.9 . . ? C89 C90 H90B 109.9 . . ? H90A C90 H90B 108.3 . . ? O13A C91 O13B 18.4(11) . . ? O13A C91 H91A 109.5 . . ? O13B C91 H91A 112.7 . . ? O13A C91 H91B 109.5 . . ? O13B C91 H91B 91.8 . . ? H91A C91 H91B 109.5 . . ? O13A C91 H91C 109.5 . . ? O13B C91 H91C 122.1 . . ? H91A C91 H91C 109.5 . . ? H91B C91 H91C 109.5 . . ? O13A C91 H91D 106.4 . . ? O13B C91 H91D 109.4 . . ? H91A C91 H91D 3.3 . . ? H91B C91 H91D 109.9 . . ? H91C C91 H91D 112.1 . . ? O13A C91 H91E 126.0 . . ? O13B C91 H91E 109.4 . . ? H91A C91 H91E 107.9 . . ? H91B C91 H91E 19.3 . . ? H91C C91 H91E 92.7 . . ? H91D C91 H91E 109.5 . . ? O13A C91 H91F 94.5 . . ? O13B C91 H91F 109.6 . . ? H91A C91 H91F 107.7 . . ? H91B C91 H91F 124.8 . . ? H91C C91 H91F 17.6 . . ? H91D C91 H91F 109.5 . . ? H91E C91 H91F 109.5 . . ? C93B C92 O13B 126.0(15) . . ? C93B C92 O13A 119.3(7) . . ? O13B C92 O13A 20.0(11) . . ? C93B C92 C93A 29.8(9) . . ? O13B C92 C93A 104.1(12) . . ? O13A C92 C93A 106.5(4) . . ? C93B C92 H92A 80.7 . . ? O13B C92 H92A 128.1 . . ? O13A C92 H92A 110.4 . . ? C93A C92 H92A 110.4 . . ? C93B C92 H92B 122.1 . . ? O13B C92 H92B 93.5 . . ? O13A C92 H92B 110.4 . . ? C93A C92 H92B 110.4 . . ? H92A C92 H92B 108.6 . . ? O14B C94 O14A 46.1(7) . . ? O14B C94 H94A 77.5 . . ? O14A C94 H94A 109.5 . . ? O14B C94 H94B 90.7 . . ? O14A C94 H94B 109.5 . . ? H94A C94 H94B 109.5 . . ? O14B C94 H94C 153.8 . . ? O14A C94 H94C 109.5 . . ? H94A C94 H94C 109.5 . . ? H94B C94 H94C 109.5 . . ? O14B C94 H94D 109.4 . . ? O14A C94 H94D 103.1 . . ? H94A C94 H94D 53.7 . . ? H94B C94 H94D 147.1 . . ? H94C C94 H94D 61.7 . . ? O14B C94 H94E 109.7 . . ? O14A C94 H94E 145.3 . . ? H94A C94 H94E 81.7 . . ? H94B C94 H94E 37.8 . . ? H94C C94 H94E 96.4 . . ? H94D C94 H94E 109.5 . . ? O14B C94 H94F 109.3 . . ? O14A C94 H94F 69.0 . . ? H94A C94 H94F 162.9 . . ? H94B C94 H94F 86.5 . . ? H94C C94 H94F 57.6 . . ? H94D C94 H94F 109.5 . . ? H94E C94 H94F 109.5 . . ? O11 C95 H95A 109.5 . . ? O11 C95 H95B 109.5 . . ? H95A C95 H95B 109.5 . . ? O11 C95 H95C 109.5 . . ? H95A C95 H95C 109.5 . . ? H95B C95 H95C 109.5 . . ? O11 C96 C97 109.3(2) . . ? O11 C96 H96A 109.8 . . ? C97 C96 H96A 109.8 . . ? O11 C96 H96B 109.8 . . ? C97 C96 H96B 109.8 . . ? H96A C96 H96B 108.3 . . ? O12 C97 C96 109.4(2) . . ? O12 C97 H97A 109.8 . . ? C96 C97 H97A 109.8 . . ? O12 C97 H97B 109.8 . . ? C96 C97 H97B 109.8 . . ? H97A C97 H97B 108.2 . . ? O12 C98 H98A 109.5 . . ? O12 C98 H98B 109.5 . . ? H98A C98 H98B 109.5 . . ? O12 C98 H98C 109.5 . . ? H98A C98 H98C 109.5 . . ? H98B C98 H98C 109.5 . . ? O15 C99 H99A 109.5 . . ? O15 C99 H99B 109.5 . . ? H99A C99 H99B 109.5 . . ? O15 C99 H99C 109.5 . . ? H99A C99 H99C 109.5 . . ? H99B C99 H99C 109.5 . . ? O15 C100 C101 114.2(2) . . ? O15 C100 H10A 108.7 . . ? C101 C100 H10A 108.7 . . ? O15 C100 H10B 108.7 . . ? C101 C100 H10B 108.7 . . ? H10A C100 H10B 107.6 . . ? O16 C101 C100 108.6(2) . . ? O16 C101 H10C 110.0 . . ? C100 C101 H10C 110.0 . . ? O16 C101 H10D 110.0 . . ? C100 C101 H10D 110.0 . . ? H10C C101 H10D 108.3 . . ? O16 C102 H10E 109.5 . . ? O16 C102 H10F 109.5 . . ? H10E C102 H10F 109.5 . . ? O16 C102 H10G 109.5 . . ? H10E C102 H10G 109.5 . . ? H10F C102 H10G 109.5 . . ? O9A C103 O9B 40.3(7) . . ? O9A C103 H10H 109.5 . . ? O9B C103 H10H 130.4 . . ? O9A C103 H10I 109.5 . . ? O9B C103 H10I 117.4 . . ? H10H C103 H10I 109.5 . . ? O9A C103 H10J 109.5 . . ? O9B C103 H10J 69.8 . . ? H10H C103 H10J 109.5 . . ? H10I C103 H10J 109.5 . . ? O9B C104 O9A 45.8(9) . . ? O9B C104 C105 119.9(8) . . ? O9A C104 C105 111.5(2) . . ? O9B C104 H10K 64.1 . . ? O9A C104 H10K 109.3 . . ? C105 C104 H10K 109.3 . . ? O9B C104 H10L 130.1 . . ? O9A C104 H10L 109.3 . . ? C105 C104 H10L 109.3 . . ? H10K C104 H10L 108.0 . . ? O10B C105 O10A 43.2(10) . . ? O10B C105 C104 123.4(8) . . ? O10A C105 C104 110.5(2) . . ? O10B C105 H10M 66.4 . . ? O10A C105 H10M 109.5 . . ? C104 C105 H10M 109.5 . . ? O10B C105 H10N 125.7 . . ? O10A C105 H10N 109.5 . . ? C104 C105 H10N 109.5 . . ? H10M C105 H10N 108.1 . . ? O10A C106 O10B 40.5(8) . . ? O10A C106 H10O 109.5 . . ? O10B C106 H10O 127.5 . . ? O10A C106 H10P 109.5 . . ? O10B C106 H10P 120.5 . . ? H10O C106 H10P 109.5 . . ? O10A C106 H10Q 109.5 . . ? O10B C106 H10Q 69.1 . . ? H10O C106 H10Q 109.5 . . ? H10P C106 H10Q 109.5 . . ? O14A C93A C92 111.1(3) . . ? O14A C93A H93A 109.4 . . ? C92 C93A H93A 109.4 . . ? O14A C93A H93B 109.4 . . ? C92 C93A H93B 109.4 . . ? H93A C93A H93B 108.0 . . ? C92 C93B O14B 112.6(10) . . ? C92 C93B H93C 109.1 . . ? O14B C93B H93C 109.1 . . ? C92 C93B H93D 109.1 . . ? O14B C93B H93D 109.1 . . ? H93C C93B H93D 107.8 . . ? O7 K1 O5 118.46(5) . . ? O7 K1 O8 60.59(5) . . ? O5 K1 O8 155.47(5) . . ? O7 K1 O3 119.67(5) . . ? O5 K1 O3 118.09(5) . . ? O8 K1 O3 59.33(5) . . ? O7 K1 O4 158.28(5) . . ? O5 K1 O4 59.66(5) . . ? O8 K1 O4 111.21(5) . . ? O3 K1 O4 58.50(4) . . ? O7 K1 O6 59.74(4) . . ? O5 K1 O6 58.80(4) . . ? O8 K1 O6 115.78(5) . . ? O3 K1 O6 163.43(4) . . ? O4 K1 O6 115.11(5) . . ? C1 N1 C7 154.7(2) . . ? C2 N2 C31 151.98(19) . . ? C3 N3 C55 163.74(19) . . ? C88 O3 C89 111.94(16) . . ? C88 O3 K1 116.65(12) . . ? C89 O3 K1 119.34(13) . . ? C79 O4 C90 111.20(16) . . ? C79 O4 K1 112.01(12) . . ? C90 O4 K1 109.24(11) . . ? C81 O5 C80 111.79(16) . . ? C81 O5 K1 119.83(12) . . ? C80 O5 K1 117.12(13) . . ? C82 O6 C83 112.31(17) . . ? C82 O6 K1 109.73(13) . . ? C83 O6 K1 105.53(13) . . ? C85 O7 C84 112.30(17) . . ? C85 O7 K1 118.96(13) . . ? C84 O7 K1 121.58(12) . . ? C87 O8 C86 110.92(18) . . ? C87 O8 K1 112.54(12) . . ? C86 O8 K1 110.96(13) . . ? C96 O11 C95 111.0(2) . . ? C97 O12 C98 111.9(2) . . ? C99 O15 C100 114.03(19) . . ? C101 O16 C102 112.23(18) . . ? C104 O9A C103 111.5(2) . . ? C105 O10A C106 111.0(2) . . ? C91 O13A C92 114.9(6) . . ? C93A O14A C94 114.1(3) . . ? C93A O14A H94F 136.4 . . ? C94 O14A H94F 39.4 . . ? C104 O9B C103 110.4(12) . . ? C105 O10B C106 110.0(11) . . ? C92 O13B C91 109.3(17) . . ? C94 O14B C93B 107.0(8) . . ? _diffrn_measured_fraction_theta_max 0.996 _diffrn_reflns_theta_full 25.00 _diffrn_measured_fraction_theta_full 0.997 _refine_diff_density_max 0.725 _refine_diff_density_min -0.341 _refine_diff_density_rms 0.049 #===END data_jfig267 _database_code_depnum_ccdc_archive 'CCDC 785483' #TrackingRef 'cif-full.cif' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common BrMn(CO)3(CNArDipp2)2 _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C65 H74 Br Mn N2 O3' _chemical_formula_weight 1066.11 loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Mn Mn 0.3368 0.7283 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Br Br -0.2901 2.4595 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting Monoclinic _symmetry_space_group_name_H-M C2/c loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, y, -z+1/2' 'x+1/2, y+1/2, z' '-x+1/2, y+1/2, -z+1/2' '-x, -y, -z' 'x, -y, z-1/2' '-x+1/2, -y+1/2, -z' 'x+1/2, -y+1/2, z-1/2' _cell_length_a 23.9872(18) _cell_length_b 23.8244(18) _cell_length_c 21.3103(16) _cell_angle_alpha 90.00 _cell_angle_beta 108.9770(10) _cell_angle_gamma 90.00 _cell_volume 11516.5(15) _cell_formula_units_Z 8 _cell_measurement_temperature 100(2) _cell_measurement_reflns_used 6001 _cell_measurement_theta_min 2.65 _cell_measurement_theta_max 24.26 _exptl_crystal_description Block _exptl_crystal_colour Yellow _exptl_crystal_size_max 0.27 _exptl_crystal_size_mid 0.16 _exptl_crystal_size_min 0.11 _exptl_crystal_density_meas 'not measured' _exptl_crystal_density_diffrn 1.230 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 4496 _exptl_absorpt_coefficient_mu 0.969 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.7799 _exptl_absorpt_correction_T_max 0.9009 _exptl_absorpt_process_details SADABS _exptl_special_details ; ? ; _diffrn_ambient_temperature 100(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'Bruker APEX-II CCD' _diffrn_measurement_method '\f and \w scans' _diffrn_reflns_number 40670 _diffrn_reflns_av_R_equivalents 0.0729 _diffrn_reflns_av_sigmaI/netI 0.0793 _diffrn_reflns_limit_h_min -28 _diffrn_reflns_limit_h_max 27 _diffrn_reflns_limit_k_min -28 _diffrn_reflns_limit_k_max 28 _diffrn_reflns_limit_l_min -25 _diffrn_reflns_limit_l_max 25 _diffrn_reflns_theta_min 1.24 _diffrn_reflns_theta_max 25.37 _reflns_number_total 10536 _reflns_number_gt 6722 _reflns_threshold_expression >2\s(I) _computing_data_collection 'Bruker APEX2' _computing_cell_refinement 'Bruker SAINT' _computing_data_reduction 'Bruker SAINT' _computing_structure_solution 'SHELXS-97 (Sheldrick, 2008)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 2008)' _computing_molecular_graphics 'Bruker SHELXTL' _computing_publication_material 'Bruker SHELXTL' _refine_special_details ; Refinement of F^2^ against ALL reflections. The weighted R-factor wR and goodness of fit S are based on F^2^, conventional R-factors R are based on F, with F set to zero for negative F^2^. The threshold expression of F^2^ > 2\s(F^2^) is used only for calculating R-factors(gt) etc. and is not relevant to the choice of reflections for refinement. R-factors based on F^2^ are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger. ; _refine_ls_structure_factor_coef Fsqd _refine_ls_matrix_type full _refine_ls_weighting_scheme calc _refine_ls_weighting_details 'calc w=1/[\s^2^(Fo^2^)+(0.0594P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment constr _refine_ls_extinction_method none _refine_ls_number_reflns 10536 _refine_ls_number_parameters 699 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0934 _refine_ls_R_factor_gt 0.0471 _refine_ls_wR_factor_ref 0.1292 _refine_ls_wR_factor_gt 0.1077 _refine_ls_goodness_of_fit_ref 1.032 _refine_ls_restrained_S_all 1.032 _refine_ls_shift/su_max 0.001 _refine_ls_shift/su_mean 0.000 loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_occupancy _atom_site_symmetry_multiplicity _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group Mn1 Mn 0.5000 0.43801(2) 0.2500 0.02680(18) Uani 1 2 d S . . Mn2 Mn 0.0000 0.43305(3) 0.2500 0.02548(18) Uani 1 2 d S . . Br1 Br 0.4636(2) 0.4388(3) 0.3383(2) 0.0204(7) Uani 0.25 1 d P . . Br2 Br 0.02358(13) 0.50082(11) 0.33616(12) 0.0211(5) Uani 0.35 1 d P . . Br1B Br 0.4078(2) 0.4386(2) 0.1657(2) 0.0208(8) Uani 0.25 1 d P . . Br2B Br 0.0220(4) 0.3722(3) 0.3404(3) 0.0201(12) Uani 0.15 1 d P . . O1 O 0.37874(17) 0.4375(2) 0.1444(3) 0.0326(12) Uani 0.75 1 d P . . O2 O 0.03141(18) 0.34877(14) 0.3613(2) 0.0302(10) Uani 0.85 1 d P . . O1B O 0.44617(18) 0.4422(2) 0.3610(2) 0.0291(10) Uani 0.75 1 d P . . O2B O 0.0232(2) 0.52367(19) 0.3578(2) 0.0298(12) Uani 0.65 1 d P . . N1 N 0.5000 0.30870(12) 0.2500 0.0176(7) Uani 1 2 d S . . N2 N 0.5000 0.56706(12) 0.2500 0.0154(7) Uani 1 2 d S . . N3 N 0.12970(10) 0.43291(9) 0.25547(10) 0.0168(5) Uani 1 1 d . . . C1O C 0.4249(7) 0.4371(9) 0.1845(7) 0.033(4) Uani 0.75 1 d P . . C2O C 0.0192(7) 0.3811(6) 0.3188(5) 0.029(3) Uani 0.85 1 d P . . C1OB C 0.4663(9) 0.4385(10) 0.3194(8) 0.037(5) Uani 0.75 1 d P . . C2OB C 0.0134(8) 0.4910(7) 0.3162(7) 0.039(5) Uani 0.65 1 d P . . C1 C 0.5000 0.35751(17) 0.2500 0.0191(9) Uani 1 2 d S . . C2 C 0.5000 0.51822(17) 0.2500 0.0192(9) Uani 1 2 d S . . C3 C 0.08076(13) 0.43348(11) 0.25341(13) 0.0205(6) Uani 1 1 d . . . C4 C 0.5000 0.24958(15) 0.2500 0.0183(9) Uani 1 2 d S . . C5 C 0.47048(12) 0.22145(10) 0.19066(13) 0.0179(6) Uani 1 1 d . . . C6 C 0.47089(13) 0.16323(11) 0.19214(14) 0.0222(7) Uani 1 1 d . . . H6 H 0.4509 0.1428 0.1530 0.027 Uiso 1 1 calc R . . C7 C 0.5000 0.13445(16) 0.2500 0.0236(10) Uani 1 2 d S . . H7 H 0.5000 0.0946 0.2500 0.028 Uiso 1 2 calc SR . . C8 C 0.43988(12) 0.25355(11) 0.12878(13) 0.0194(6) Uani 1 1 d . . . C9 C 0.47134(13) 0.26757(11) 0.08536(14) 0.0233(7) Uani 1 1 d . . . C10 C 0.44270(14) 0.29991(12) 0.02988(15) 0.0313(8) Uani 1 1 d . . . H10 H 0.4631 0.3102 0.0002 0.038 Uiso 1 1 calc R . . C11 C 0.38523(15) 0.31723(13) 0.01726(15) 0.0337(8) Uani 1 1 d . . . H11 H 0.3668 0.3401 -0.0203 0.040 Uiso 1 1 calc R . . C12 C 0.35439(14) 0.30149(12) 0.05881(15) 0.0293(7) Uani 1 1 d . . . H12 H 0.3145 0.3129 0.0490 0.035 Uiso 1 1 calc R . . C13 C 0.38083(13) 0.26918(11) 0.11486(14) 0.0226(7) Uani 1 1 d . . . C14 C 0.29472(17) 0.21324(15) 0.12155(19) 0.0551(11) Uani 1 1 d . . . H14A H 0.2724 0.2021 0.1507 0.083 Uiso 1 1 calc R . . H14B H 0.3106 0.1797 0.1068 0.083 Uiso 1 1 calc R . . H14C H 0.2686 0.2332 0.0829 0.083 Uiso 1 1 calc R . . C15 C 0.34511(13) 0.25153(12) 0.15913(15) 0.0284(7) Uani 1 1 d . . . H15 H 0.3718 0.2297 0.1972 0.034 Uiso 1 1 calc R . . C16 C 0.32260(16) 0.30179(14) 0.18736(17) 0.0439(9) Uani 1 1 d . . . H16A H 0.3002 0.2888 0.2158 0.066 Uiso 1 1 calc R . . H16B H 0.2969 0.3244 0.1510 0.066 Uiso 1 1 calc R . . H16C H 0.3560 0.3246 0.2136 0.066 Uiso 1 1 calc R . . C17 C 0.57717(14) 0.29833(14) 0.12408(16) 0.0414(9) Uani 1 1 d . . . H17C H 0.6178 0.2853 0.1329 0.062 Uiso 1 1 calc R . . H17A H 0.5727 0.3132 0.1650 0.062 Uiso 1 1 calc R . . H17B H 0.5683 0.3279 0.0903 0.062 Uiso 1 1 calc R . . C18 C 0.53494(13) 0.24959(12) 0.09924(15) 0.0304(7) Uani 1 1 d . . . H18 H 0.5442 0.2208 0.1353 0.036 Uiso 1 1 calc R . . C19 C 0.54493(16) 0.22239(15) 0.03894(18) 0.0503(10) Uani 1 1 d . . . H19C H 0.5863 0.2111 0.0503 0.075 Uiso 1 1 calc R . . H19B H 0.5353 0.2493 0.0022 0.075 Uiso 1 1 calc R . . H19A H 0.5196 0.1893 0.0256 0.075 Uiso 1 1 calc R . . C20 C 0.5000 0.62615(15) 0.2500 0.0158(9) Uani 1 2 d S . . C21 C 0.50295(11) 0.65416(11) 0.19353(12) 0.0168(6) Uani 1 1 d . . . C22 C 0.50311(12) 0.71239(11) 0.19495(13) 0.0204(6) Uani 1 1 d . . . H22 H 0.5054 0.7328 0.1576 0.024 Uiso 1 1 calc R . . C23 C 0.5000 0.74087(16) 0.2500 0.0244(10) Uani 1 2 d S . . H23 H 0.5000 0.7807 0.2500 0.029 Uiso 1 2 calc SR . . C24 C 0.50685(12) 0.62293(10) 0.13410(13) 0.0167(6) Uani 1 1 d . . . C25 C 0.45533(13) 0.61391(11) 0.07965(13) 0.0208(7) Uani 1 1 d . . . C26 C 0.46123(13) 0.58597(11) 0.02468(14) 0.0244(7) Uani 1 1 d . . . H26 H 0.4272 0.5795 -0.0128 0.029 Uiso 1 1 calc R . . C27 C 0.51540(14) 0.56750(11) 0.02352(14) 0.0264(7) Uani 1 1 d . . . H27 H 0.5184 0.5485 -0.0145 0.032 Uiso 1 1 calc R . . C28 C 0.56512(13) 0.57657(11) 0.07748(14) 0.0234(7) Uani 1 1 d . . . H28 H 0.6022 0.5636 0.0762 0.028 Uiso 1 1 calc R . . C29 C 0.56217(12) 0.60425(11) 0.13358(13) 0.0184(6) Uani 1 1 d . . . C30 C 0.36576(15) 0.58789(15) 0.11007(17) 0.0477(10) Uani 1 1 d . . . H30B H 0.3276 0.6017 0.1111 0.071 Uiso 1 1 calc R . . H30C H 0.3908 0.5786 0.1552 0.071 Uiso 1 1 calc R . . H30A H 0.3597 0.5543 0.0822 0.071 Uiso 1 1 calc R . . C31 C 0.39572(13) 0.63338(12) 0.08151(14) 0.0258(7) Uani 1 1 d . . . H31 H 0.4027 0.6664 0.1121 0.031 Uiso 1 1 calc R . . C32 C 0.35364(14) 0.65226(14) 0.01425(15) 0.0401(9) Uani 1 1 d . . . H32B H 0.3163 0.6646 0.0193 0.060 Uiso 1 1 calc R . . H32A H 0.3462 0.6209 -0.0171 0.060 Uiso 1 1 calc R . . H32C H 0.3714 0.6835 -0.0026 0.060 Uiso 1 1 calc R . . C33 C 0.65000(13) 0.55980(12) 0.21873(15) 0.0318(8) Uani 1 1 d . . . H33C H 0.6856 0.5681 0.2561 0.048 Uiso 1 1 calc R . . H33B H 0.6610 0.5406 0.1838 0.048 Uiso 1 1 calc R . . H33A H 0.6238 0.5356 0.2338 0.048 Uiso 1 1 calc R . . C34 C 0.61827(12) 0.61444(11) 0.19142(13) 0.0215(7) Uani 1 1 d . . . H34 H 0.6069 0.6328 0.2277 0.026 Uiso 1 1 calc R . . C35 C 0.65943(13) 0.65469(13) 0.17135(15) 0.0334(8) Uani 1 1 d . . . H35C H 0.6951 0.6610 0.2094 0.050 Uiso 1 1 calc R . . H35B H 0.6392 0.6905 0.1570 0.050 Uiso 1 1 calc R . . H35A H 0.6703 0.6382 0.1348 0.050 Uiso 1 1 calc R . . C36 C 0.18885(11) 0.43081(10) 0.25714(13) 0.0167(6) Uani 1 1 d . . . C37 C 0.23169(12) 0.41306(11) 0.31613(13) 0.0167(6) Uani 1 1 d . . . C38 C 0.28908(12) 0.40995(11) 0.31603(14) 0.0206(7) Uani 1 1 d . . . H38 H 0.3192 0.3979 0.3550 0.025 Uiso 1 1 calc R . . C39 C 0.30360(12) 0.42404(11) 0.26030(13) 0.0205(7) Uani 1 1 d . . . H39 H 0.3434 0.4211 0.2613 0.025 Uiso 1 1 calc R . . C40 C 0.26091(12) 0.44238(11) 0.20325(13) 0.0204(6) Uani 1 1 d . . . H40 H 0.2717 0.4524 0.1656 0.024 Uiso 1 1 calc R . . C41 C 0.20225(12) 0.44628(11) 0.20049(13) 0.0182(6) Uani 1 1 d . . . C42 C 0.15621(12) 0.46693(11) 0.13908(13) 0.0189(6) Uani 1 1 d . . . C43 C 0.13186(12) 0.42988(12) 0.08564(14) 0.0252(7) Uani 1 1 d . . . C44 C 0.09041(13) 0.45126(13) 0.02842(14) 0.0293(7) Uani 1 1 d . . . H44 H 0.0733 0.4270 -0.0082 0.035 Uiso 1 1 calc R . . C45 C 0.07387(13) 0.50694(13) 0.02405(14) 0.0294(7) Uani 1 1 d . . . H45 H 0.0457 0.5207 -0.0155 0.035 Uiso 1 1 calc R . . C46 C 0.09782(12) 0.54254(13) 0.07640(14) 0.0260(7) Uani 1 1 d . . . H46 H 0.0859 0.5808 0.0728 0.031 Uiso 1 1 calc R . . C47 C 0.13933(12) 0.52362(12) 0.13475(13) 0.0204(6) Uani 1 1 d . . . C48 C 0.21532(12) 0.39854(11) 0.37619(13) 0.0193(6) Uani 1 1 d . . . C49 C 0.21244(12) 0.44124(12) 0.42058(13) 0.0229(7) Uani 1 1 d . . . C50 C 0.19525(14) 0.42717(12) 0.47507(14) 0.0299(7) Uani 1 1 d . . . H50 H 0.1931 0.4555 0.5055 0.036 Uiso 1 1 calc R . . C51 C 0.18136(13) 0.37223(13) 0.48515(15) 0.0322(8) Uani 1 1 d . . . H51 H 0.1692 0.3632 0.5221 0.039 Uiso 1 1 calc R . . C52 C 0.18516(13) 0.33083(13) 0.44193(14) 0.0283(7) Uani 1 1 d . . . H52 H 0.1761 0.2932 0.4499 0.034 Uiso 1 1 calc R . . C53 C 0.20203(12) 0.34257(11) 0.38667(13) 0.0213(7) Uani 1 1 d . . . C54 C 0.11926(15) 0.58663(14) 0.22012(17) 0.0409(9) Uani 1 1 d . . . H54C H 0.1374 0.6130 0.2563 0.061 Uiso 1 1 calc R . . H54A H 0.1025 0.5549 0.2372 0.061 Uiso 1 1 calc R . . H54B H 0.0879 0.6057 0.1853 0.061 Uiso 1 1 calc R . . C55 C 0.16590(13) 0.56522(11) 0.19136(14) 0.0244(7) Uani 1 1 d . . . H55 H 0.1967 0.5449 0.2274 0.029 Uiso 1 1 calc R . . C56 C 0.19538(14) 0.61475(12) 0.17005(15) 0.0349(8) Uani 1 1 d . . . H56C H 0.2117 0.6401 0.2078 0.052 Uiso 1 1 calc R . . H56B H 0.1662 0.6350 0.1341 0.052 Uiso 1 1 calc R . . H56A H 0.2272 0.6011 0.1545 0.052 Uiso 1 1 calc R . . C57 C 0.10407(19) 0.33339(15) 0.1109(2) 0.0612(11) Uani 1 1 d . . . H57A H 0.1158 0.2938 0.1146 0.092 Uiso 1 1 calc R . . H57B H 0.0650 0.3374 0.0775 0.092 Uiso 1 1 calc R . . H57C H 0.1027 0.3467 0.1539 0.092 Uiso 1 1 calc R . . C58 C 0.14846(14) 0.36786(12) 0.09045(15) 0.0317(8) Uani 1 1 d . . . H58 H 0.1873 0.3641 0.1264 0.038 Uiso 1 1 calc R . . C59 C 0.15590(19) 0.34432(15) 0.02733(18) 0.0580(11) Uani 1 1 d . . . H59A H 0.1671 0.3047 0.0340 0.087 Uiso 1 1 calc R . . H59C H 0.1867 0.3653 0.0166 0.087 Uiso 1 1 calc R . . H59B H 0.1186 0.3478 -0.0092 0.087 Uiso 1 1 calc R . . C60 C 0.17785(18) 0.54102(15) 0.4043(3) 0.0823(16) Uani 1 1 d . . . H60A H 0.1429 0.5281 0.3685 0.123 Uiso 1 1 calc R . . H60C H 0.1884 0.5789 0.3941 0.123 Uiso 1 1 calc R . . H60B H 0.1693 0.5417 0.4462 0.123 Uiso 1 1 calc R . . C61 C 0.22804(14) 0.50192(12) 0.41034(15) 0.0306(8) Uani 1 1 d . . . H61 H 0.2367 0.5035 0.3675 0.037 Uiso 1 1 calc R . . C62 C 0.2819(2) 0.52216(19) 0.4638(3) 0.105(2) Uani 1 1 d . . . H62A H 0.3148 0.4965 0.4676 0.157 Uiso 1 1 calc R . . H62B H 0.2741 0.5233 0.5062 0.157 Uiso 1 1 calc R . . H62C H 0.2921 0.5599 0.4528 0.157 Uiso 1 1 calc R . . C63 C 0.14363(15) 0.27315(14) 0.30280(17) 0.0423(9) Uani 1 1 d . . . H63A H 0.1466 0.2433 0.2724 0.063 Uiso 1 1 calc R . . H63C H 0.1187 0.3035 0.2775 0.063 Uiso 1 1 calc R . . H63B H 0.1261 0.2580 0.3349 0.063 Uiso 1 1 calc R . . C64 C 0.20500(13) 0.29601(12) 0.33962(15) 0.0277(7) Uani 1 1 d . . . H64 H 0.2213 0.3122 0.3060 0.033 Uiso 1 1 calc R . . C65 C 0.24626(15) 0.24850(13) 0.37593(17) 0.0450(9) Uani 1 1 d . . . H65A H 0.2475 0.2193 0.3440 0.068 Uiso 1 1 calc R . . H65B H 0.2316 0.2323 0.4098 0.068 Uiso 1 1 calc R . . H65C H 0.2860 0.2635 0.3971 0.068 Uiso 1 1 calc R . . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 Mn1 0.0406(4) 0.0127(3) 0.0245(4) 0.000 0.0069(3) 0.000 Mn2 0.0133(3) 0.0365(4) 0.0270(4) 0.000 0.0071(3) 0.000 Br1 0.0179(13) 0.0218(10) 0.023(2) -0.0017(17) 0.0080(13) 0.0035(9) Br2 0.0218(12) 0.0201(9) 0.0200(15) 0.0017(8) 0.0048(11) 0.0016(8) Br1B 0.018(2) 0.0208(9) 0.025(3) -0.0002(18) 0.0082(19) -0.002(2) Br2B 0.0199(18) 0.010(3) 0.030(4) 0.005(2) 0.009(3) 0.0032(19) O1 0.025(3) 0.038(2) 0.031(3) -0.0008(19) 0.004(2) -0.004(3) O2 0.034(2) 0.021(2) 0.033(2) 0.0047(16) 0.0079(17) 0.0053(18) O1B 0.030(3) 0.0325(19) 0.026(3) -0.0023(17) 0.0111(17) 0.0058(18) O2B 0.039(2) 0.026(3) 0.023(3) -0.004(2) 0.009(2) 0.005(2) N1 0.0210(19) 0.0129(18) 0.0216(19) 0.000 0.0106(15) 0.000 N2 0.0212(18) 0.0130(18) 0.0106(16) 0.000 0.0032(14) 0.000 N3 0.0143(13) 0.0201(12) 0.0164(12) -0.0024(10) 0.0054(10) -0.0007(10) C1O 0.045(10) 0.022(3) 0.039(9) 0.002(6) 0.023(7) 0.003(6) C2O 0.020(3) 0.022(5) 0.047(8) -0.003(4) 0.014(6) -0.004(3) C1OB 0.032(5) 0.024(3) 0.045(11) -0.007(7) 0.000(6) -0.001(3) C2OB 0.012(6) 0.069(10) 0.029(9) 0.020(6) -0.002(6) 0.009(5) C1 0.020(2) 0.024(2) 0.013(2) 0.000 0.0054(18) 0.000 C2 0.019(2) 0.023(2) 0.015(2) 0.000 0.0057(18) 0.000 C3 0.0195(17) 0.0227(15) 0.0174(15) 0.0021(12) 0.0033(13) 0.0001(13) C4 0.020(2) 0.014(2) 0.025(2) 0.000 0.0117(19) 0.000 C5 0.0200(16) 0.0143(14) 0.0235(16) 0.0013(12) 0.0126(13) -0.0005(12) C6 0.0275(17) 0.0176(15) 0.0249(17) -0.0080(12) 0.0133(14) -0.0049(13) C7 0.030(3) 0.016(2) 0.029(3) 0.000 0.015(2) 0.000 C8 0.0272(17) 0.0123(14) 0.0199(16) -0.0027(11) 0.0094(14) -0.0013(12) C9 0.0265(17) 0.0196(15) 0.0265(17) -0.0012(13) 0.0125(14) -0.0018(13) C10 0.038(2) 0.0312(18) 0.0302(19) 0.0071(14) 0.0183(16) 0.0006(15) C11 0.042(2) 0.0332(18) 0.0251(18) 0.0099(14) 0.0095(16) 0.0053(16) C12 0.0263(18) 0.0274(17) 0.0317(19) 0.0003(14) 0.0061(15) 0.0055(14) C13 0.0248(17) 0.0157(14) 0.0266(17) -0.0017(12) 0.0075(14) -0.0015(13) C14 0.063(3) 0.044(2) 0.072(3) -0.0144(19) 0.041(2) -0.025(2) C15 0.0263(18) 0.0272(17) 0.0348(19) 0.0035(14) 0.0141(15) 0.0016(14) C16 0.049(2) 0.040(2) 0.055(2) -0.0016(17) 0.033(2) 0.0024(17) C17 0.031(2) 0.052(2) 0.044(2) -0.0066(17) 0.0157(17) -0.0012(17) C18 0.0315(19) 0.0301(17) 0.0359(19) 0.0070(14) 0.0198(16) 0.0029(15) C19 0.038(2) 0.054(2) 0.065(3) -0.0212(19) 0.026(2) -0.0022(18) C20 0.015(2) 0.0137(19) 0.015(2) 0.000 -0.0013(17) 0.000 C21 0.0126(15) 0.0185(14) 0.0157(15) -0.0004(11) -0.0004(12) 0.0018(12) C22 0.0199(16) 0.0186(15) 0.0196(16) 0.0023(12) 0.0024(13) -0.0033(12) C23 0.028(3) 0.014(2) 0.025(2) 0.000 0.001(2) 0.000 C24 0.0221(16) 0.0124(13) 0.0159(15) 0.0052(11) 0.0065(13) -0.0028(12) C25 0.0255(17) 0.0168(15) 0.0178(15) 0.0016(12) 0.0038(13) -0.0030(13) C26 0.0249(18) 0.0231(16) 0.0204(16) -0.0003(12) 0.0007(14) -0.0018(13) C27 0.039(2) 0.0230(16) 0.0205(16) -0.0023(13) 0.0143(15) 0.0004(14) C28 0.0254(17) 0.0219(16) 0.0244(17) 0.0017(12) 0.0104(14) 0.0014(13) C29 0.0242(16) 0.0133(14) 0.0181(15) 0.0036(11) 0.0074(13) 0.0017(12) C30 0.031(2) 0.069(3) 0.044(2) 0.0229(19) 0.0145(18) 0.0051(18) C31 0.0241(17) 0.0298(17) 0.0211(16) -0.0039(13) 0.0040(14) 0.0010(13) C32 0.0262(19) 0.054(2) 0.039(2) 0.0173(17) 0.0093(16) 0.0074(17) C33 0.0248(17) 0.0304(17) 0.0355(19) 0.0070(14) 0.0035(15) 0.0045(14) C34 0.0175(16) 0.0234(16) 0.0237(16) 0.0017(12) 0.0069(13) 0.0000(12) C35 0.0292(19) 0.0351(18) 0.0303(19) 0.0041(14) 0.0022(15) -0.0071(15) C36 0.0135(15) 0.0184(14) 0.0188(15) -0.0026(12) 0.0061(12) -0.0007(12) C37 0.0155(15) 0.0165(14) 0.0180(15) -0.0039(11) 0.0050(13) -0.0032(12) C38 0.0158(16) 0.0213(15) 0.0219(16) -0.0037(12) 0.0020(13) 0.0005(12) C39 0.0138(15) 0.0238(16) 0.0264(17) -0.0035(12) 0.0098(14) -0.0002(12) C40 0.0192(16) 0.0222(15) 0.0224(16) -0.0017(12) 0.0106(13) -0.0018(13) C41 0.0176(15) 0.0201(15) 0.0165(15) -0.0044(11) 0.0052(13) -0.0033(12) C42 0.0147(15) 0.0266(16) 0.0183(16) -0.0008(12) 0.0092(13) -0.0004(12) C43 0.0208(16) 0.0338(18) 0.0220(16) -0.0031(13) 0.0083(14) -0.0022(14) C44 0.0239(17) 0.042(2) 0.0212(17) -0.0075(14) 0.0057(14) -0.0021(15) C45 0.0196(17) 0.046(2) 0.0210(17) 0.0043(15) 0.0039(14) 0.0032(15) C46 0.0193(17) 0.0324(17) 0.0289(18) 0.0060(14) 0.0114(15) 0.0044(14) C47 0.0151(15) 0.0281(16) 0.0204(16) 0.0032(12) 0.0093(13) -0.0006(13) C48 0.0126(15) 0.0263(16) 0.0171(15) 0.0016(12) 0.0022(12) 0.0021(12) C49 0.0216(16) 0.0267(16) 0.0217(16) -0.0028(13) 0.0090(13) 0.0013(13) C50 0.0368(19) 0.0322(18) 0.0236(17) -0.0048(14) 0.0137(15) -0.0015(15) C51 0.033(2) 0.045(2) 0.0237(18) 0.0058(15) 0.0157(15) -0.0003(16) C52 0.0265(18) 0.0305(17) 0.0281(18) 0.0063(14) 0.0094(15) -0.0037(14) C53 0.0160(16) 0.0246(16) 0.0217(16) 0.0009(12) 0.0038(13) 0.0012(13) C54 0.040(2) 0.0373(19) 0.048(2) -0.0149(16) 0.0187(18) -0.0062(16) C55 0.0234(16) 0.0229(15) 0.0260(16) 0.0003(13) 0.0068(14) 0.0000(13) C56 0.0324(19) 0.0339(19) 0.0348(19) 0.0066(15) 0.0058(16) -0.0055(15) C57 0.079(3) 0.038(2) 0.075(3) 0.000(2) 0.037(3) 0.001(2) C58 0.0331(19) 0.0315(18) 0.0279(18) -0.0077(14) 0.0065(15) 0.0023(15) C59 0.084(3) 0.047(2) 0.052(2) -0.0059(19) 0.035(2) 0.014(2) C60 0.061(3) 0.026(2) 0.168(5) 0.007(3) 0.049(3) 0.008(2) C61 0.046(2) 0.0246(16) 0.0288(18) -0.0048(14) 0.0224(16) -0.0028(15) C62 0.071(3) 0.067(3) 0.130(4) 0.040(3) -0.031(3) -0.042(3) C63 0.041(2) 0.0344(19) 0.046(2) -0.0123(16) 0.0070(18) -0.0074(17) C64 0.0330(19) 0.0224(16) 0.0298(18) -0.0019(13) 0.0130(15) -0.0053(14) C65 0.041(2) 0.037(2) 0.056(2) -0.0117(17) 0.0141(19) 0.0068(17) _geom_special_details ; All s.u.'s (except the s.u. in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell s.u.'s are taken into account individually in the estimation of s.u.'s in distances, angles and torsion angles; correlations between s.u.'s in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell s.u.'s is used for estimating s.u.'s involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag Mn1 C1O 1.886(12) 2_655 ? Mn1 C1O 1.886(12) . ? Mn1 C1OB 1.902(14) . ? Mn1 C1OB 1.902(14) 2_655 ? Mn1 C2 1.911(4) . ? Mn1 C1 1.918(4) . ? Mn1 Br1 2.319(5) . ? Mn1 Br1 2.319(5) 2_655 ? Mn1 Br1B 2.352(4) . ? Mn1 Br1B 2.352(4) 2_655 ? Mn2 C2O 1.858(9) 2 ? Mn2 C2O 1.858(9) . ? Mn2 C3 1.915(3) 2 ? Mn2 C3 1.915(3) . ? Mn2 C2OB 1.925(13) . ? Mn2 C2OB 1.925(13) 2 ? Mn2 Br2B 2.330(6) . ? Mn2 Br2B 2.330(6) 2 ? Mn2 Br2 2.371(3) . ? Mn2 Br2 2.371(3) 2 ? Br1 O1B 0.739(5) . ? Br2 O2B 0.715(4) . ? Br1B O1 0.698(4) . ? Br2B O2 0.704(5) . ? O1 C1O 1.158(13) . ? O2 C2O 1.153(10) . ? O1B C1OB 1.144(16) . ? O2B C2OB 1.145(13) . ? N1 C1 1.163(4) . ? N1 C4 1.409(5) . ? N2 C2 1.164(4) . ? N2 C20 1.408(4) . ? N3 C3 1.161(3) . ? N3 C36 1.408(3) . ? C4 C5 1.403(3) . ? C4 C5 1.403(3) 2_655 ? C5 C6 1.387(4) . ? C5 C8 1.494(4) . ? C6 C7 1.385(3) . ? C6 H6 0.9500 . ? C7 C6 1.385(3) 2_655 ? C7 H7 0.9500 . ? C8 C13 1.400(4) . ? C8 C9 1.411(4) . ? C9 C10 1.391(4) . ? C9 C18 1.518(4) . ? C10 C11 1.379(4) . ? C10 H10 0.9500 . ? C11 C12 1.378(4) . ? C11 H11 0.9500 . ? C12 C13 1.389(4) . ? C12 H12 0.9500 . ? C13 C15 1.525(4) . ? C14 C15 1.518(4) . ? C14 H14A 0.9800 . ? C14 H14B 0.9800 . ? C14 H14C 0.9800 . ? C15 C16 1.516(4) . ? C15 H15 1.0000 . ? C16 H16A 0.9800 . ? C16 H16B 0.9800 . ? C16 H16C 0.9800 . ? C17 C18 1.519(4) . ? C17 H17C 0.9800 . ? C17 H17A 0.9800 . ? C17 H17B 0.9800 . ? C18 C19 1.526(4) . ? C18 H18 1.0000 . ? C19 H19C 0.9800 . ? C19 H19B 0.9800 . ? C19 H19A 0.9800 . ? C20 C21 1.398(3) 2_655 ? C20 C21 1.398(3) . ? C21 C22 1.388(3) . ? C21 C24 1.498(4) . ? C22 C23 1.378(3) . ? C22 H22 0.9500 . ? C23 C22 1.378(3) 2_655 ? C23 H23 0.9500 . ? C24 C29 1.403(4) . ? C24 C25 1.410(4) . ? C25 C26 1.394(4) . ? C25 C31 1.516(4) . ? C26 C27 1.380(4) . ? C26 H26 0.9500 . ? C27 C28 1.378(4) . ? C27 H27 0.9500 . ? C28 C29 1.387(4) . ? C28 H28 0.9500 . ? C29 C34 1.520(4) . ? C30 C31 1.532(4) . ? C30 H30B 0.9800 . ? C30 H30C 0.9800 . ? C30 H30A 0.9800 . ? C31 C32 1.528(4) . ? C31 H31 1.0000 . ? C32 H32B 0.9800 . ? C32 H32A 0.9800 . ? C32 H32C 0.9800 . ? C33 C34 1.525(4) . ? C33 H33C 0.9800 . ? C33 H33B 0.9800 . ? C33 H33A 0.9800 . ? C34 C35 1.534(4) . ? C34 H34 1.0000 . ? C35 H35C 0.9800 . ? C35 H35B 0.9800 . ? C35 H35A 0.9800 . ? C36 C41 1.396(4) . ? C36 C37 1.405(4) . ? C37 C38 1.379(4) . ? C37 C48 1.496(4) . ? C38 C39 1.383(4) . ? C38 H38 0.9500 . ? C39 C40 1.381(4) . ? C39 H39 0.9500 . ? C40 C41 1.392(4) . ? C40 H40 0.9500 . ? C41 C42 1.495(4) . ? C42 C47 1.404(4) . ? C42 C43 1.409(4) . ? C43 C44 1.395(4) . ? C43 C58 1.525(4) . ? C44 C45 1.379(4) . ? C44 H44 0.9500 . ? C45 C46 1.370(4) . ? C45 H45 0.9500 . ? C46 C47 1.391(4) . ? C46 H46 0.9500 . ? C47 C55 1.531(4) . ? C48 C53 1.406(4) . ? C48 C49 1.406(4) . ? C49 C50 1.394(4) . ? C49 C61 1.527(4) . ? C50 C51 1.385(4) . ? C50 H50 0.9500 . ? C51 C52 1.373(4) . ? C51 H51 0.9500 . ? C52 C53 1.393(4) . ? C52 H52 0.9500 . ? C53 C64 1.512(4) . ? C54 C55 1.527(4) . ? C54 H54C 0.9800 . ? C54 H54A 0.9800 . ? C54 H54B 0.9800 . ? C55 C56 1.519(4) . ? C55 H55 1.0000 . ? C56 H56C 0.9800 . ? C56 H56B 0.9800 . ? C56 H56A 0.9800 . ? C57 C58 1.517(5) . ? C57 H57A 0.9800 . ? C57 H57B 0.9800 . ? C57 H57C 0.9800 . ? C58 C59 1.520(4) . ? C58 H58 1.0000 . ? C59 H59A 0.9800 . ? C59 H59C 0.9800 . ? C59 H59B 0.9800 . ? C60 C61 1.494(5) . ? C60 H60A 0.9800 . ? C60 H60C 0.9800 . ? C60 H60B 0.9800 . ? C61 C62 1.498(5) . ? C61 H61 1.0000 . ? C62 H62A 0.9800 . ? C62 H62B 0.9800 . ? C62 H62C 0.9800 . ? C63 C64 1.526(4) . ? C63 H63A 0.9800 . ? C63 H63C 0.9800 . ? C63 H63B 0.9800 . ? C64 C65 1.537(4) . ? C64 H64 1.0000 . ? C65 H65A 0.9800 . ? C65 H65B 0.9800 . ? C65 H65C 0.9800 . ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag C1O Mn1 C1O 178.6(13) 2_655 . ? C1O Mn1 C1OB 88.3(9) 2_655 . ? C1O Mn1 C1OB 91.7(9) . . ? C1O Mn1 C1OB 91.7(9) 2_655 2_655 ? C1O Mn1 C1OB 88.3(9) . 2_655 ? C1OB Mn1 C1OB 179.3(14) . 2_655 ? C1O Mn1 C2 90.7(7) 2_655 . ? C1O Mn1 C2 90.7(7) . . ? C1OB Mn1 C2 89.6(7) . . ? C1OB Mn1 C2 89.6(7) 2_655 . ? C1O Mn1 C1 89.3(7) 2_655 . ? C1O Mn1 C1 89.3(7) . . ? C1OB Mn1 C1 90.4(7) . . ? C1OB Mn1 C1 90.4(7) 2_655 . ? C2 Mn1 C1 180.000(1) . . ? C1O Mn1 Br1 85.5(6) 2_655 . ? C1O Mn1 Br1 94.5(6) . . ? C1OB Mn1 Br1 2.8(8) . . ? C1OB Mn1 Br1 177.1(7) 2_655 . ? C2 Mn1 Br1 89.55(15) . . ? C1 Mn1 Br1 90.45(15) . . ? C1O Mn1 Br1 94.5(6) 2_655 2_655 ? C1O Mn1 Br1 85.5(6) . 2_655 ? C1OB Mn1 Br1 177.1(7) . 2_655 ? C1OB Mn1 Br1 2.8(8) 2_655 2_655 ? C2 Mn1 Br1 89.55(15) . 2_655 ? C1 Mn1 Br1 90.45(15) . 2_655 ? Br1 Mn1 Br1 179.1(3) . 2_655 ? C1O Mn1 Br1B 178.1(7) 2_655 . ? C1O Mn1 Br1B 2.1(7) . . ? C1OB Mn1 Br1B 93.6(6) . . ? C1OB Mn1 Br1B 86.4(6) 2_655 . ? C2 Mn1 Br1B 89.66(13) . . ? C1 Mn1 Br1B 90.34(13) . . ? Br1 Mn1 Br1B 96.42(18) . . ? Br1 Mn1 Br1B 83.58(18) 2_655 . ? C1O Mn1 Br1B 2.1(7) 2_655 2_655 ? C1O Mn1 Br1B 178.1(7) . 2_655 ? C1OB Mn1 Br1B 86.4(6) . 2_655 ? C1OB Mn1 Br1B 93.6(6) 2_655 2_655 ? C2 Mn1 Br1B 89.66(13) . 2_655 ? C1 Mn1 Br1B 90.34(13) . 2_655 ? Br1 Mn1 Br1B 83.58(18) . 2_655 ? Br1 Mn1 Br1B 96.42(18) 2_655 2_655 ? Br1B Mn1 Br1B 179.3(3) . 2_655 ? C2O Mn2 C2O 96.5(9) 2 . ? C2O Mn2 C3 89.2(5) 2 2 ? C2O Mn2 C3 91.2(5) . 2 ? C2O Mn2 C3 91.2(5) 2 . ? C2O Mn2 C3 89.2(5) . . ? C3 Mn2 C3 179.39(17) 2 . ? C2O Mn2 C2OB 174.5(7) 2 . ? C2O Mn2 C2OB 87.7(7) . . ? C3 Mn2 C2OB 87.1(6) 2 . ? C3 Mn2 C2OB 92.4(6) . . ? C2O Mn2 C2OB 87.7(7) 2 2 ? C2O Mn2 C2OB 174.5(7) . 2 ? C3 Mn2 C2OB 92.4(6) 2 2 ? C3 Mn2 C2OB 87.1(6) . 2 ? C2OB Mn2 C2OB 88.3(10) . 2 ? C2O Mn2 Br2B 99.7(3) 2 . ? C2O Mn2 Br2B 3.7(6) . . ? C3 Mn2 Br2B 89.4(2) 2 . ? C3 Mn2 Br2B 91.0(2) . . ? C2OB Mn2 Br2B 84.4(5) . . ? C2OB Mn2 Br2B 172.4(5) 2 . ? C2O Mn2 Br2B 3.7(6) 2 2 ? C2O Mn2 Br2B 99.7(3) . 2 ? C3 Mn2 Br2B 91.0(2) 2 2 ? C3 Mn2 Br2B 89.4(2) . 2 ? C2OB Mn2 Br2B 172.4(5) . 2 ? C2OB Mn2 Br2B 84.4(5) 2 2 ? Br2B Mn2 Br2B 103.0(4) . 2 ? C2O Mn2 Br2 178.8(5) 2 . ? C2O Mn2 Br2 84.7(5) . . ? C3 Mn2 Br2 90.54(11) 2 . ? C3 Mn2 Br2 89.05(11) . . ? C2OB Mn2 Br2 4.5(6) . . ? C2OB Mn2 Br2 91.1(5) 2 . ? Br2B Mn2 Br2 81.44(19) . . ? Br2B Mn2 Br2 175.3(2) 2 . ? C2O Mn2 Br2 84.7(5) 2 2 ? C2O Mn2 Br2 178.8(5) . 2 ? C3 Mn2 Br2 89.05(11) 2 2 ? C3 Mn2 Br2 90.54(11) . 2 ? C2OB Mn2 Br2 91.1(5) . 2 ? C2OB Mn2 Br2 4.5(6) 2 2 ? Br2B Mn2 Br2 175.3(2) . 2 ? Br2B Mn2 Br2 81.44(19) 2 2 ? Br2 Mn2 Br2 94.17(12) . 2 ? O1B Br1 Mn1 167.0(5) . . ? O2B Br2 Mn2 165.3(5) . . ? O1 Br1B Mn1 171.3(5) . . ? O2 Br2B Mn2 163.1(8) . . ? Br1B O1 C1O 6.9(13) . . ? Br2B O2 C2O 12.7(12) . . ? Br1 O1B C1OB 9.1(13) . . ? Br2 O2B C2OB 13.2(10) . . ? C1 N1 C4 180.000(1) . . ? C2 N2 C20 180.000(1) . . ? C3 N3 C36 178.5(3) . . ? O1 C1O Mn1 179(2) . . ? O2 C2O Mn2 179.5(15) . . ? O1B C1OB Mn1 176(2) . . ? O2B C2OB Mn2 176.6(15) . . ? N1 C1 Mn1 180.000(1) . . ? N2 C2 Mn1 180.000(1) . . ? N3 C3 Mn2 179.0(3) . . ? C5 C4 C5 122.9(3) . 2_655 ? C5 C4 N1 118.54(17) . . ? C5 C4 N1 118.54(17) 2_655 . ? C6 C5 C4 117.4(3) . . ? C6 C5 C8 122.0(2) . . ? C4 C5 C8 120.7(2) . . ? C7 C6 C5 120.9(3) . . ? C7 C6 H6 119.6 . . ? C5 C6 H6 119.6 . . ? C6 C7 C6 120.7(4) 2_655 . ? C6 C7 H7 119.7 2_655 . ? C6 C7 H7 119.7 . . ? C13 C8 C9 121.2(2) . . ? C13 C8 C5 119.7(2) . . ? C9 C8 C5 119.1(2) . . ? C10 C9 C8 117.8(3) . . ? C10 C9 C18 120.6(3) . . ? C8 C9 C18 121.5(2) . . ? C11 C10 C9 121.2(3) . . ? C11 C10 H10 119.4 . . ? C9 C10 H10 119.4 . . ? C12 C11 C10 120.3(3) . . ? C12 C11 H11 119.8 . . ? C10 C11 H11 119.8 . . ? C11 C12 C13 120.9(3) . . ? C11 C12 H12 119.6 . . ? C13 C12 H12 119.6 . . ? C12 C13 C8 118.5(3) . . ? C12 C13 C15 119.6(3) . . ? C8 C13 C15 121.9(2) . . ? C15 C14 H14A 109.5 . . ? C15 C14 H14B 109.5 . . ? H14A C14 H14B 109.5 . . ? C15 C14 H14C 109.5 . . ? H14A C14 H14C 109.5 . . ? H14B C14 H14C 109.5 . . ? C16 C15 C14 111.0(3) . . ? C16 C15 C13 111.8(2) . . ? C14 C15 C13 110.5(3) . . ? C16 C15 H15 107.8 . . ? C14 C15 H15 107.8 . . ? C13 C15 H15 107.8 . . ? C15 C16 H16A 109.5 . . ? C15 C16 H16B 109.5 . . ? H16A C16 H16B 109.5 . . ? C15 C16 H16C 109.5 . . ? H16A C16 H16C 109.5 . . ? H16B C16 H16C 109.5 . . ? C18 C17 H17C 109.5 . . ? C18 C17 H17A 109.5 . . ? H17C C17 H17A 109.5 . . ? C18 C17 H17B 109.5 . . ? H17C C17 H17B 109.5 . . ? H17A C17 H17B 109.5 . . ? C9 C18 C17 111.5(2) . . ? C9 C18 C19 112.3(3) . . ? C17 C18 C19 110.4(3) . . ? C9 C18 H18 107.5 . . ? C17 C18 H18 107.5 . . ? C19 C18 H18 107.5 . . ? C18 C19 H19C 109.5 . . ? C18 C19 H19B 109.5 . . ? H19C C19 H19B 109.5 . . ? C18 C19 H19A 109.5 . . ? H19C C19 H19A 109.5 . . ? H19B C19 H19A 109.5 . . ? C21 C20 C21 123.0(3) 2_655 . ? C21 C20 N2 118.51(17) 2_655 . ? C21 C20 N2 118.51(17) . . ? C22 C21 C20 117.3(3) . . ? C22 C21 C24 121.0(2) . . ? C20 C21 C24 121.7(2) . . ? C23 C22 C21 120.7(3) . . ? C23 C22 H22 119.7 . . ? C21 C22 H22 119.7 . . ? C22 C23 C22 121.0(4) 2_655 . ? C22 C23 H23 119.5 2_655 . ? C22 C23 H23 119.5 . . ? C29 C24 C25 121.6(2) . . ? C29 C24 C21 118.9(2) . . ? C25 C24 C21 119.5(2) . . ? C26 C25 C24 117.6(3) . . ? C26 C25 C31 121.5(2) . . ? C24 C25 C31 120.9(2) . . ? C27 C26 C25 121.4(3) . . ? C27 C26 H26 119.3 . . ? C25 C26 H26 119.3 . . ? C28 C27 C26 120.0(3) . . ? C28 C27 H27 120.0 . . ? C26 C27 H27 120.0 . . ? C27 C28 C29 121.4(3) . . ? C27 C28 H28 119.3 . . ? C29 C28 H28 119.3 . . ? C28 C29 C24 118.1(3) . . ? C28 C29 C34 119.7(3) . . ? C24 C29 C34 122.2(2) . . ? C31 C30 H30B 109.5 . . ? C31 C30 H30C 109.5 . . ? H30B C30 H30C 109.5 . . ? C31 C30 H30A 109.5 . . ? H30B C30 H30A 109.5 . . ? H30C C30 H30A 109.5 . . ? C25 C31 C32 114.0(2) . . ? C25 C31 C30 111.2(2) . . ? C32 C31 C30 109.2(3) . . ? C25 C31 H31 107.4 . . ? C32 C31 H31 107.4 . . ? C30 C31 H31 107.4 . . ? C31 C32 H32B 109.5 . . ? C31 C32 H32A 109.5 . . ? H32B C32 H32A 109.5 . . ? C31 C32 H32C 109.5 . . ? H32B C32 H32C 109.5 . . ? H32A C32 H32C 109.5 . . ? C34 C33 H33C 109.5 . . ? C34 C33 H33B 109.5 . . ? H33C C33 H33B 109.5 . . ? C34 C33 H33A 109.5 . . ? H33C C33 H33A 109.5 . . ? H33B C33 H33A 109.5 . . ? C29 C34 C33 111.9(2) . . ? C29 C34 C35 110.7(2) . . ? C33 C34 C35 110.7(2) . . ? C29 C34 H34 107.8 . . ? C33 C34 H34 107.8 . . ? C35 C34 H34 107.8 . . ? C34 C35 H35C 109.5 . . ? C34 C35 H35B 109.5 . . ? H35C C35 H35B 109.5 . . ? C34 C35 H35A 109.5 . . ? H35C C35 H35A 109.5 . . ? H35B C35 H35A 109.5 . . ? C41 C36 C37 123.1(2) . . ? C41 C36 N3 118.8(2) . . ? C37 C36 N3 118.1(2) . . ? C38 C37 C36 117.0(2) . . ? C38 C37 C48 121.9(2) . . ? C36 C37 C48 121.1(2) . . ? C37 C38 C39 121.2(3) . . ? C37 C38 H38 119.4 . . ? C39 C38 H38 119.4 . . ? C40 C39 C38 120.7(3) . . ? C40 C39 H39 119.6 . . ? C38 C39 H39 119.6 . . ? C39 C40 C41 120.5(3) . . ? C39 C40 H40 119.7 . . ? C41 C40 H40 119.7 . . ? C40 C41 C36 117.4(2) . . ? C40 C41 C42 120.5(2) . . ? C36 C41 C42 122.1(2) . . ? C47 C42 C43 121.0(3) . . ? C47 C42 C41 119.3(2) . . ? C43 C42 C41 119.7(2) . . ? C44 C43 C42 117.9(3) . . ? C44 C43 C58 120.6(3) . . ? C42 C43 C58 121.5(3) . . ? C45 C44 C43 121.2(3) . . ? C45 C44 H44 119.4 . . ? C43 C44 H44 119.4 . . ? C46 C45 C44 120.3(3) . . ? C46 C45 H45 119.8 . . ? C44 C45 H45 119.8 . . ? C45 C46 C47 121.1(3) . . ? C45 C46 H46 119.5 . . ? C47 C46 H46 119.5 . . ? C46 C47 C42 118.5(3) . . ? C46 C47 C55 119.2(3) . . ? C42 C47 C55 122.2(2) . . ? C53 C48 C49 121.1(3) . . ? C53 C48 C37 119.4(2) . . ? C49 C48 C37 119.5(2) . . ? C50 C49 C48 118.6(3) . . ? C50 C49 C61 120.0(2) . . ? C48 C49 C61 121.4(2) . . ? C51 C50 C49 120.5(3) . . ? C51 C50 H50 119.7 . . ? C49 C50 H50 119.7 . . ? C52 C51 C50 120.2(3) . . ? C52 C51 H51 119.9 . . ? C50 C51 H51 119.9 . . ? C51 C52 C53 121.6(3) . . ? C51 C52 H52 119.2 . . ? C53 C52 H52 119.2 . . ? C52 C53 C48 117.9(3) . . ? C52 C53 C64 120.2(3) . . ? C48 C53 C64 121.9(2) . . ? C55 C54 H54C 109.5 . . ? C55 C54 H54A 109.5 . . ? H54C C54 H54A 109.5 . . ? C55 C54 H54B 109.5 . . ? H54C C54 H54B 109.5 . . ? H54A C54 H54B 109.5 . . ? C56 C55 C54 109.5(2) . . ? C56 C55 C47 112.5(2) . . ? C54 C55 C47 111.2(2) . . ? C56 C55 H55 107.9 . . ? C54 C55 H55 107.9 . . ? C47 C55 H55 107.9 . . ? C55 C56 H56C 109.5 . . ? C55 C56 H56B 109.5 . . ? H56C C56 H56B 109.5 . . ? C55 C56 H56A 109.5 . . ? H56C C56 H56A 109.5 . . ? H56B C56 H56A 109.5 . . ? C58 C57 H57A 109.5 . . ? C58 C57 H57B 109.5 . . ? H57A C57 H57B 109.5 . . ? C58 C57 H57C 109.5 . . ? H57A C57 H57C 109.5 . . ? H57B C57 H57C 109.5 . . ? C57 C58 C59 110.5(3) . . ? C57 C58 C43 110.6(3) . . ? C59 C58 C43 113.6(3) . . ? C57 C58 H58 107.3 . . ? C59 C58 H58 107.3 . . ? C43 C58 H58 107.3 . . ? C58 C59 H59A 109.5 . . ? C58 C59 H59C 109.5 . . ? H59A C59 H59C 109.5 . . ? C58 C59 H59B 109.5 . . ? H59A C59 H59B 109.5 . . ? H59C C59 H59B 109.5 . . ? C61 C60 H60A 109.5 . . ? C61 C60 H60C 109.5 . . ? H60A C60 H60C 109.5 . . ? C61 C60 H60B 109.5 . . ? H60A C60 H60B 109.5 . . ? H60C C60 H60B 109.5 . . ? C60 C61 C62 109.7(3) . . ? C60 C61 C49 112.0(3) . . ? C62 C61 C49 112.8(3) . . ? C60 C61 H61 107.4 . . ? C62 C61 H61 107.4 . . ? C49 C61 H61 107.4 . . ? C61 C62 H62A 109.5 . . ? C61 C62 H62B 109.5 . . ? H62A C62 H62B 109.5 . . ? C61 C62 H62C 109.5 . . ? H62A C62 H62C 109.5 . . ? H62B C62 H62C 109.5 . . ? C64 C63 H63A 109.5 . . ? C64 C63 H63C 109.5 . . ? H63A C63 H63C 109.5 . . ? C64 C63 H63B 109.5 . . ? H63A C63 H63B 109.5 . . ? H63C C63 H63B 109.5 . . ? C53 C64 C63 110.9(3) . . ? C53 C64 C65 111.6(2) . . ? C63 C64 C65 110.6(3) . . ? C53 C64 H64 107.9 . . ? C63 C64 H64 107.9 . . ? C65 C64 H64 107.9 . . ? C64 C65 H65A 109.5 . . ? C64 C65 H65B 109.5 . . ? H65A C65 H65B 109.5 . . ? C64 C65 H65C 109.5 . . ? H65A C65 H65C 109.5 . . ? H65B C65 H65C 109.5 . . ? _diffrn_measured_fraction_theta_max 0.997 _diffrn_reflns_theta_full 25.00 _diffrn_measured_fraction_theta_full 0.998 _refine_diff_density_max 0.327 _refine_diff_density_min -0.588 _refine_diff_density_rms 0.085 #===END data_jfig326 _database_code_depnum_ccdc_archive 'CCDC 785484' #TrackingRef 'cif-full.cif' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common '[Na(NCMe)2][Mn(CO)3(CNDipp2)2]' _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C76 H88 Mn N4 Na O3' _chemical_formula_weight 1183.43 loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Na Na 0.0362 0.0249 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Mn Mn 0.3368 0.7283 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting Monoclinic _symmetry_space_group_name_H-M Cm loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' 'x, -y, z' 'x+1/2, y+1/2, z' 'x+1/2, -y+1/2, z' _cell_length_a 16.0055(11) _cell_length_b 24.3120(17) _cell_length_c 11.5994(8) _cell_angle_alpha 90.00 _cell_angle_beta 128.7135(7) _cell_angle_gamma 90.00 _cell_volume 3521.9(4) _cell_formula_units_Z 2 _cell_measurement_temperature 100(2) _cell_measurement_reflns_used 4578 _cell_measurement_theta_min 2.25 _cell_measurement_theta_max 24.20 _exptl_crystal_description Block _exptl_crystal_colour Red _exptl_crystal_size_max 0.28 _exptl_crystal_size_mid 0.22 _exptl_crystal_size_min 0.16 _exptl_crystal_density_meas 'not measured' _exptl_crystal_density_diffrn 1.116 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1264 _exptl_absorpt_coefficient_mu 0.241 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.9356 _exptl_absorpt_correction_T_max 0.9625 _exptl_absorpt_process_details SADABS _exptl_special_details ; ? ; _diffrn_ambient_temperature 100(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'Bruker APEX CCD' _diffrn_measurement_method '\f and \w scans' _diffrn_reflns_number 23856 _diffrn_reflns_av_R_equivalents 0.0389 _diffrn_reflns_av_sigmaI/netI 0.0503 _diffrn_reflns_limit_h_min -20 _diffrn_reflns_limit_h_max 21 _diffrn_reflns_limit_k_min -31 _diffrn_reflns_limit_k_max 30 _diffrn_reflns_limit_l_min -15 _diffrn_reflns_limit_l_max 14 _diffrn_reflns_theta_min 1.83 _diffrn_reflns_theta_max 28.23 _reflns_number_total 8014 _reflns_number_gt 6589 _reflns_threshold_expression >2\s(I) _computing_data_collection 'Bruker APEX2' _computing_cell_refinement 'Bruker SAINT' _computing_data_reduction 'Bruker SAINT' _computing_structure_solution 'SHELXS-97 (Sheldrick, 2008)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 2008)' _computing_molecular_graphics 'Bruker SHELXTL' _computing_publication_material 'Bruker SHELXTL' _refine_special_details ; Refinement of F^2^ against ALL reflections. The weighted R-factor wR and goodness of fit S are based on F^2^, conventional R-factors R are based on F, with F set to zero for negative F^2^. The threshold expression of F^2^ > 2\s(F^2^) is used only for calculating R-factors(gt) etc. and is not relevant to the choice of reflections for refinement. R-factors based on F^2^ are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger. ; _refine_ls_structure_factor_coef Fsqd _refine_ls_matrix_type full _refine_ls_weighting_scheme calc _refine_ls_weighting_details 'calc w=1/[\s^2^(Fo^2^)+(0.0781P)^2^+0.0171P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment constr _refine_ls_extinction_method SHELXL _refine_ls_extinction_coef 0.0001(3) _refine_ls_extinction_expression Fc^*^=kFc[1+0.001xFc^2^\l^3^/sin(2\q)]^-1/4^ _refine_ls_abs_structure_details 'Flack H D (1983), Acta Cryst. A39, 876-881' _refine_ls_abs_structure_Flack 0.092(17) _refine_ls_number_reflns 8014 _refine_ls_number_parameters 425 _refine_ls_number_restraints 44 _refine_ls_R_factor_all 0.0651 _refine_ls_R_factor_gt 0.0492 _refine_ls_wR_factor_ref 0.1317 _refine_ls_wR_factor_gt 0.1216 _refine_ls_goodness_of_fit_ref 1.031 _refine_ls_restrained_S_all 1.031 _refine_ls_shift/su_max 0.000 _refine_ls_shift/su_mean 0.000 loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_occupancy _atom_site_symmetry_multiplicity _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group Mn1 Mn 0.91189(4) 0.5000 0.58039(6) 0.03038(17) Uani 1 2 d S . . Na1 Na 0.6357(2) 0.5000 0.1578(3) 0.0695(6) Uani 1 2 d S . . O1 O 1.0463(3) 0.5000 0.9091(4) 0.0620(10) Uani 1 2 d S . . O2 O 1.0217(5) 0.5000 0.4486(7) 0.0964(17) Uani 1 2 d S . . O3 O 0.6756(3) 0.5000 0.3893(4) 0.0642(10) Uani 1 2 d S . . N1 N 0.92933(17) 0.37551(7) 0.5925(3) 0.0217(4) Uani 1 1 d . . . C1 C 0.9189(2) 0.42368(8) 0.5851(4) 0.0244(5) Uani 1 1 d . . . C2 C 0.9936(4) 0.5000 0.7794(5) 0.0420(10) Uani 1 2 d S . . C3 C 0.9767(5) 0.5000 0.4972(7) 0.0578(15) Uani 1 2 d S . . C4 C 0.7699(4) 0.5000 0.4665(5) 0.0416(10) Uani 1 2 d S . . C5 C 0.93083(19) 0.31866(8) 0.5887(3) 0.0173(4) Uani 1 1 d . . . C6 C 1.01976(18) 0.29009(9) 0.7084(3) 0.0185(5) Uani 1 1 d . . . C7 C 1.0182(2) 0.23298(10) 0.7021(3) 0.0226(5) Uani 1 1 d . . . H7 H 1.0775 0.2127 0.7819 0.027 Uiso 1 1 calc R . . C8 C 0.9309(2) 0.20500(9) 0.5805(3) 0.0247(5) Uani 1 1 d . . . H8 H 0.9307 0.1659 0.5784 0.030 Uiso 1 1 calc R . . C9 C 0.84468(19) 0.23392(10) 0.4632(3) 0.0220(5) Uani 1 1 d . . . H9 H 0.7860 0.2145 0.3800 0.026 Uiso 1 1 calc R . . C10 C 0.84252(18) 0.29125(9) 0.4652(3) 0.0179(5) Uani 1 1 d . . . C11 C 1.11296(18) 0.32114(9) 0.8383(3) 0.0183(5) Uani 1 1 d . . . C12 C 1.11152(19) 0.33571(10) 0.9543(3) 0.0225(5) Uani 1 1 d . . . C13 C 1.1991(2) 0.36394(11) 1.0754(3) 0.0276(6) Uani 1 1 d . . . H13 H 1.1986 0.3748 1.1537 0.033 Uiso 1 1 calc R . . C14 C 1.2869(2) 0.37627(12) 1.0828(3) 0.0288(6) Uani 1 1 d . . . H14 H 1.3471 0.3944 1.1673 0.035 Uiso 1 1 calc R . . C15 C 1.2869(2) 0.36221(10) 0.9674(3) 0.0257(5) Uani 1 1 d . . . H15 H 1.3472 0.3712 0.9732 0.031 Uiso 1 1 calc R . . C16 C 1.20029(19) 0.33507(10) 0.8426(3) 0.0211(5) Uani 1 1 d . . . C17 C 1.2025(2) 0.32165(11) 0.7166(3) 0.0251(5) Uani 1 1 d . . . H17 H 1.1333 0.3032 0.6370 0.030 Uiso 1 1 calc R . . C18 C 1.2931(2) 0.28180(12) 0.7661(3) 0.0363(7) Uani 1 1 d . . . H18C H 1.3618 0.2982 0.8475 0.054 Uiso 1 1 calc R . . H18B H 1.2932 0.2743 0.6832 0.054 Uiso 1 1 calc R . . H18A H 1.2826 0.2474 0.7995 0.054 Uiso 1 1 calc R . . C19 C 1.2119(3) 0.37347(13) 0.6508(4) 0.0409(7) Uani 1 1 d . . . H19A H 1.1537 0.3989 0.6198 0.061 Uiso 1 1 calc R . . H19B H 1.2072 0.3635 0.5650 0.061 Uiso 1 1 calc R . . H19C H 1.2809 0.3913 0.7252 0.061 Uiso 1 1 calc R . . C20 C 1.01849(19) 0.32082(11) 0.9516(3) 0.0233(5) Uani 1 1 d . . . H20 H 0.9680 0.2978 0.8617 0.028 Uiso 1 1 calc R . . C21 C 1.0554(2) 0.28613(12) 1.0853(3) 0.0341(7) Uani 1 1 d . . . H21B H 1.0993 0.2555 1.0954 0.051 Uiso 1 1 calc R . . H21A H 0.9928 0.2716 1.0721 0.051 Uiso 1 1 calc R . . H21C H 1.0977 0.3089 1.1745 0.051 Uiso 1 1 calc R . . C22 C 0.9570(2) 0.37127(13) 0.9387(4) 0.0368(7) Uani 1 1 d . . . H22C H 1.0054 0.3959 1.0225 0.055 Uiso 1 1 calc R . . H22A H 0.8984 0.3599 0.9391 0.055 Uiso 1 1 calc R . . H22B H 0.9275 0.3906 0.8462 0.055 Uiso 1 1 calc R . . C23 C 0.75205(18) 0.32378(9) 0.3369(3) 0.0177(5) Uani 1 1 d . . . C24 C 0.66686(19) 0.34098(10) 0.3339(3) 0.0201(5) Uani 1 1 d . . . C25 C 0.5831(2) 0.37035(10) 0.2114(3) 0.0250(5) Uani 1 1 d . . . H25 H 0.5257 0.3829 0.2087 0.030 Uiso 1 1 calc R . . C26 C 0.5821(2) 0.38149(11) 0.0934(3) 0.0246(5) Uani 1 1 d . . . H26 H 0.5231 0.4003 0.0091 0.030 Uiso 1 1 calc R . . C27 C 0.6674(2) 0.36516(10) 0.0987(3) 0.0251(5) Uani 1 1 d . . . H27 H 0.6670 0.3735 0.0184 0.030 Uiso 1 1 calc R . . C28 C 0.75354(19) 0.33666(10) 0.2203(3) 0.0201(5) Uani 1 1 d . . . C29 C 0.6628(2) 0.32707(11) 0.4585(3) 0.0253(5) Uani 1 1 d . . . H29 H 0.7323 0.3091 0.5392 0.030 Uiso 1 1 calc R . . C30 C 0.5737(2) 0.28612(12) 0.4063(3) 0.0348(6) Uani 1 1 d . . . H30B H 0.5051 0.3016 0.3220 0.052 Uiso 1 1 calc R . . H30C H 0.5710 0.2786 0.4870 0.052 Uiso 1 1 calc R . . H30A H 0.5876 0.2518 0.3765 0.052 Uiso 1 1 calc R . . C31 C 0.6511(3) 0.37866(14) 0.5234(3) 0.0417(8) Uani 1 1 d . . . H31C H 0.7117 0.4033 0.5619 0.063 Uiso 1 1 calc R . . H31A H 0.6497 0.3680 0.6037 0.063 Uiso 1 1 calc R . . H31B H 0.5842 0.3976 0.4460 0.063 Uiso 1 1 calc R . . C32 C 0.8475(2) 0.31957(11) 0.2246(3) 0.0256(6) Uani 1 1 d . . . H32 H 0.8957 0.2954 0.3127 0.031 Uiso 1 1 calc R . . C33 C 0.8088(2) 0.28668(13) 0.0873(4) 0.0398(8) Uani 1 1 d . . . H33A H 0.7646 0.2558 0.0755 0.060 Uiso 1 1 calc R . . H33C H 0.8707 0.2725 0.0981 0.060 Uiso 1 1 calc R . . H33B H 0.7663 0.3105 0.0002 0.060 Uiso 1 1 calc R . . C34 C 0.9118(3) 0.36981(13) 0.2426(4) 0.0441(8) Uani 1 1 d . . . H34A H 0.8679 0.3928 0.1539 0.066 Uiso 1 1 calc R . . H34C H 0.9761 0.3578 0.2565 0.066 Uiso 1 1 calc R . . H34B H 0.9329 0.3911 0.3289 0.066 Uiso 1 1 calc R . . N1S N 0.4414(4) 0.5000 0.0064(7) 0.0859(19) Uani 1 2 d S . . N2S N 0.7041(5) 0.5000 0.0179(7) 0.0792(15) Uani 1 2 d S . . C1S C 0.3509(5) 0.5000 -0.0543(8) 0.0753(19) Uani 1 2 d S . . C2S C 0.2332(5) 0.5000 -0.1365(9) 0.085(2) Uani 1 2 d S . . H2SC H 0.1983 0.5220 -0.2266 0.128 Uiso 0.50 1 calc PR . . H2SB H 0.2175 0.5158 -0.0742 0.128 Uiso 0.50 1 calc PR . . H2SA H 0.2063 0.4622 -0.1628 0.128 Uiso 0.50 1 calc PR . . C3S C 0.7546(6) 0.5000 -0.0214(10) 0.085(2) Uani 1 2 d S . . C4S C 0.8151(8) 0.5000 -0.0802(16) 0.154(5) Uani 1 2 d S . . H4SC H 0.8005 0.5342 -0.1347 0.231 Uiso 0.50 1 calc PR . . H4SA H 0.7926 0.4685 -0.1465 0.231 Uiso 0.50 1 calc PR . . H4SB H 0.8920 0.4973 0.0021 0.231 Uiso 0.50 1 calc PR . . C5S C 0.3320(13) 0.5000 0.5348(16) 0.167(5) Uani 1 2 d SU . . H5S H 0.3036 0.5000 0.5862 0.201 Uiso 1 2 calc SR . . C6S C 0.4341(18) 0.5000 0.605(2) 0.232(8) Uani 1 2 d SU . . H6S H 0.4793 0.5000 0.7096 0.278 Uiso 1 2 calc SR . . C7S C 0.4858(14) 0.5000 0.537(2) 0.198(6) Uani 1 2 d SU . . H7S H 0.5615 0.5000 0.5943 0.238 Uiso 1 2 calc SR . . C8S C 0.4174(9) 0.5000 0.3847(12) 0.122(3) Uani 1 2 d SU . . H8S H 0.4463 0.5000 0.3338 0.146 Uiso 1 2 calc SR . . C9S C 0.3080(6) 0.5000 0.3053(8) 0.0786(18) Uani 1 2 d SU . . H9S H 0.2628 0.5000 0.2004 0.094 Uiso 1 2 calc SR . . C10S C 0.2626(9) 0.5000 0.3745(10) 0.107(2) Uani 1 2 d SU . . C11S C 0.1454(9) 0.5000 0.2868(10) 0.137(4) Uani 1 2 d SU . . H11B H 0.1119 0.4904 0.1842 0.205 Uiso 0.50 1 calc PR . . H11C H 0.1215 0.5366 0.2901 0.205 Uiso 0.50 1 calc PR . . H11A H 0.1249 0.4730 0.3277 0.205 Uiso 0.50 1 calc PR . . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 Mn1 0.0381(4) 0.0148(2) 0.0368(3) 0.000 0.0227(3) 0.000 Na1 0.0779(16) 0.0453(12) 0.0867(16) 0.000 0.0522(14) 0.000 O1 0.081(3) 0.0295(16) 0.0426(19) 0.000 0.0228(19) 0.000 O2 0.173(5) 0.035(2) 0.189(5) 0.000 0.166(5) 0.000 O3 0.047(2) 0.0304(17) 0.072(3) 0.000 0.016(2) 0.000 N1 0.0179(10) 0.0180(8) 0.0193(9) 0.0003(10) 0.0068(8) -0.0013(8) C1 0.0231(12) 0.0226(10) 0.0251(10) 0.0034(14) 0.0139(10) 0.0007(12) C2 0.052(3) 0.0210(19) 0.039(3) 0.000 0.021(2) 0.000 C3 0.099(4) 0.020(2) 0.101(4) 0.000 0.085(4) 0.000 C4 0.032(2) 0.0211(18) 0.042(2) 0.000 0.009(2) 0.000 C5 0.0172(11) 0.0143(9) 0.0220(10) 0.0002(11) 0.0130(9) 0.0000(9) C6 0.0144(11) 0.0210(12) 0.0182(12) 0.0020(9) 0.0093(10) 0.0011(9) C7 0.0171(12) 0.0204(12) 0.0245(13) 0.0024(10) 0.0102(11) 0.0027(9) C8 0.0258(13) 0.0152(10) 0.0303(12) 0.0002(11) 0.0160(11) 0.0014(10) C9 0.0185(12) 0.0206(12) 0.0221(13) -0.0052(10) 0.0103(11) -0.0041(9) C10 0.0166(12) 0.0182(11) 0.0190(12) 0.0010(9) 0.0111(10) 0.0003(9) C11 0.0138(11) 0.0177(11) 0.0185(13) 0.0012(9) 0.0077(10) 0.0024(9) C12 0.0160(12) 0.0230(12) 0.0228(13) 0.0039(10) 0.0094(11) 0.0048(10) C13 0.0214(13) 0.0391(15) 0.0202(13) -0.0060(12) 0.0119(12) -0.0013(11) C14 0.0162(12) 0.0343(15) 0.0244(14) -0.0081(11) 0.0072(11) -0.0046(10) C15 0.0163(12) 0.0276(13) 0.0278(13) -0.0018(11) 0.0112(11) -0.0025(10) C16 0.0161(12) 0.0196(12) 0.0219(13) 0.0016(9) 0.0091(11) 0.0012(9) C17 0.0208(13) 0.0332(14) 0.0213(14) -0.0030(10) 0.0131(12) -0.0029(10) C18 0.0336(16) 0.0397(16) 0.0426(18) -0.0030(13) 0.0273(15) 0.0034(13) C19 0.0522(19) 0.0403(17) 0.0395(18) 0.0055(14) 0.0332(17) 0.0011(15) C20 0.0145(12) 0.0330(14) 0.0208(13) 0.0002(10) 0.0102(11) 0.0001(10) C21 0.0237(14) 0.0449(17) 0.0338(16) 0.0150(13) 0.0180(13) 0.0100(12) C22 0.0291(15) 0.0440(17) 0.0430(18) 0.0096(14) 0.0254(15) 0.0114(13) C23 0.0135(12) 0.0163(11) 0.0174(13) -0.0007(9) 0.0068(10) -0.0017(9) C24 0.0159(12) 0.0216(12) 0.0197(13) -0.0009(10) 0.0097(11) -0.0018(9) C25 0.0168(12) 0.0267(13) 0.0277(13) -0.0004(11) 0.0120(11) 0.0018(10) C26 0.0158(12) 0.0276(13) 0.0192(13) 0.0037(10) 0.0055(11) 0.0017(10) C27 0.0242(13) 0.0256(13) 0.0221(13) 0.0031(11) 0.0128(12) 0.0000(10) C28 0.0172(12) 0.0212(12) 0.0194(13) -0.0020(10) 0.0102(11) -0.0023(9) C29 0.0209(13) 0.0317(13) 0.0246(14) 0.0040(11) 0.0149(12) 0.0021(11) C30 0.0337(16) 0.0394(16) 0.0328(15) 0.0042(13) 0.0215(14) -0.0065(13) C31 0.054(2) 0.0411(17) 0.0420(19) -0.0051(14) 0.0362(18) -0.0010(15) C32 0.0195(13) 0.0325(14) 0.0227(14) 0.0020(11) 0.0121(12) 0.0027(10) C33 0.0286(15) 0.0517(19) 0.047(2) -0.0199(15) 0.0276(15) -0.0104(13) C34 0.0351(17) 0.0468(19) 0.062(2) -0.0233(16) 0.0359(17) -0.0181(14) N1S 0.045(3) 0.035(2) 0.117(5) 0.000 0.021(3) 0.000 N2S 0.073(3) 0.051(3) 0.119(5) 0.000 0.063(4) 0.000 C1S 0.051(4) 0.023(2) 0.101(5) 0.000 0.023(4) 0.000 C2S 0.053(4) 0.033(3) 0.112(5) 0.000 0.023(4) 0.000 C3S 0.088(5) 0.045(3) 0.150(7) 0.000 0.088(5) 0.000 C4S 0.153(9) 0.061(5) 0.331(16) 0.000 0.192(12) 0.000 C5S 0.186(9) 0.193(9) 0.134(7) 0.000 0.106(6) 0.000 C6S 0.223(11) 0.265(12) 0.210(11) 0.000 0.137(9) 0.000 C7S 0.186(9) 0.209(10) 0.190(10) 0.000 0.113(8) 0.000 C8S 0.116(6) 0.107(6) 0.125(6) 0.000 0.067(5) 0.000 C9S 0.082(4) 0.069(4) 0.072(4) 0.000 0.042(4) 0.000 C10S 0.126(6) 0.117(5) 0.084(5) 0.000 0.069(5) 0.000 C11S 0.123(9) 0.212(12) 0.085(6) 0.000 0.070(6) 0.000 _geom_special_details ; All s.u.'s (except the s.u. in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell s.u.'s are taken into account individually in the estimation of s.u.'s in distances, angles and torsion angles; correlations between s.u.'s in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell s.u.'s is used for estimating s.u.'s involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag Mn1 C4 1.776(4) . ? Mn1 C3 1.805(5) . ? Mn1 C2 1.806(4) . ? Mn1 C1 1.858(2) 2_565 ? Mn1 C1 1.858(2) . ? Na1 O3 2.340(5) . ? Na1 N1S 2.434(6) . ? Na1 N2S 2.461(7) . ? Na1 C4 2.795(5) . ? Na1 C26 2.965(3) . ? Na1 C26 2.965(3) 2_565 ? O1 C2 1.179(5) . ? O2 C3 1.160(5) . ? O3 C4 1.179(5) . ? N1 C1 1.178(3) . ? N1 C5 1.383(3) . ? C5 C10 1.400(3) . ? C5 C6 1.401(3) . ? C6 C7 1.390(3) . ? C6 C11 1.501(3) . ? C7 C8 1.393(4) . ? C8 C9 1.379(4) . ? C9 C10 1.395(3) . ? C10 C23 1.497(3) . ? C11 C12 1.405(3) . ? C11 C16 1.408(3) . ? C12 C13 1.395(4) . ? C12 C20 1.514(3) . ? C13 C14 1.385(4) . ? C14 C15 1.382(4) . ? C15 C16 1.394(4) . ? C16 C17 1.519(3) . ? C17 C18 1.527(4) . ? C17 C19 1.529(4) . ? C20 C22 1.520(4) . ? C20 C21 1.523(4) . ? C23 C28 1.403(3) . ? C23 C24 1.405(3) . ? C24 C25 1.394(4) . ? C24 C29 1.524(3) . ? C25 C26 1.385(4) . ? C26 C27 1.385(4) . ? C27 C28 1.392(4) . ? C28 C32 1.530(3) . ? C29 C30 1.521(4) . ? C29 C31 1.534(4) . ? C32 C33 1.525(4) . ? C32 C34 1.526(4) . ? N1S C1S 1.149(7) . ? N2S C3S 1.149(8) . ? C1S C2S 1.486(9) . ? C3S C4S 1.493(12) . ? C5S C6S 1.29(2) . ? C5S C10S 1.451(16) . ? C6S C7S 1.45(2) . ? C7S C8S 1.382(17) . ? C8S C9S 1.377(11) . ? C9S C10S 1.380(11) . ? C10S C11S 1.472(13) . ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag C4 Mn1 C3 119.9(3) . . ? C4 Mn1 C2 121.2(2) . . ? C3 Mn1 C2 119.0(3) . . ? C4 Mn1 C1 92.73(9) . 2_565 ? C3 Mn1 C1 88.37(9) . 2_565 ? C2 Mn1 C1 88.85(10) . 2_565 ? C4 Mn1 C1 92.73(9) . . ? C3 Mn1 C1 88.37(9) . . ? C2 Mn1 C1 88.85(10) . . ? C1 Mn1 C1 174.51(17) 2_565 . ? O3 Na1 N1S 97.8(2) . . ? O3 Na1 N2S 147.4(2) . . ? N1S Na1 N2S 114.8(2) . . ? O3 Na1 C4 24.55(13) . . ? N1S Na1 C4 122.4(2) . . ? N2S Na1 C4 122.85(19) . . ? O3 Na1 C26 96.74(7) . . ? N1S Na1 C26 77.32(7) . . ? N2S Na1 C26 90.68(7) . . ? C4 Na1 C26 101.07(7) . . ? O3 Na1 C26 96.74(7) . 2_565 ? N1S Na1 C26 77.32(7) . 2_565 ? N2S Na1 C26 90.68(8) . 2_565 ? C4 Na1 C26 101.07(7) . 2_565 ? C26 Na1 C26 152.63(14) . 2_565 ? C4 O3 Na1 99.9(4) . . ? C1 N1 C5 174.2(3) . . ? N1 C1 Mn1 176.3(2) . . ? O1 C2 Mn1 179.5(5) . . ? O2 C3 Mn1 177.6(6) . . ? O3 C4 Mn1 179.2(5) . . ? O3 C4 Na1 55.6(3) . . ? Mn1 C4 Na1 123.6(2) . . ? N1 C5 C10 118.8(2) . . ? N1 C5 C6 119.4(2) . . ? C10 C5 C6 121.83(18) . . ? C7 C6 C5 118.0(2) . . ? C7 C6 C11 121.9(2) . . ? C5 C6 C11 120.1(2) . . ? C6 C7 C8 121.0(2) . . ? C9 C8 C7 120.1(2) . . ? C8 C9 C10 120.9(2) . . ? C9 C10 C5 118.2(2) . . ? C9 C10 C23 122.0(2) . . ? C5 C10 C23 119.68(19) . . ? C12 C11 C16 121.0(2) . . ? C12 C11 C6 119.1(2) . . ? C16 C11 C6 119.8(2) . . ? C13 C12 C11 118.7(2) . . ? C13 C12 C20 119.6(2) . . ? C11 C12 C20 121.7(2) . . ? C14 C13 C12 120.7(2) . . ? C15 C14 C13 120.1(2) . . ? C14 C15 C16 121.3(2) . . ? C15 C16 C11 118.1(2) . . ? C15 C16 C17 119.6(2) . . ? C11 C16 C17 122.3(2) . . ? C16 C17 C18 111.3(2) . . ? C16 C17 C19 111.9(2) . . ? C18 C17 C19 110.1(2) . . ? C12 C20 C22 112.1(2) . . ? C12 C20 C21 111.2(2) . . ? C22 C20 C21 111.2(2) . . ? C28 C23 C24 120.7(2) . . ? C28 C23 C10 119.2(2) . . ? C24 C23 C10 120.2(2) . . ? C25 C24 C23 118.6(2) . . ? C25 C24 C29 119.7(2) . . ? C23 C24 C29 121.7(2) . . ? C26 C25 C24 121.1(2) . . ? C27 C26 C25 119.9(2) . . ? C27 C26 Na1 98.37(16) . . ? C25 C26 Na1 96.81(17) . . ? C26 C27 C28 120.8(2) . . ? C27 C28 C23 119.0(2) . . ? C27 C28 C32 119.9(2) . . ? C23 C28 C32 121.1(2) . . ? C30 C29 C24 110.7(2) . . ? C30 C29 C31 111.0(2) . . ? C24 C29 C31 112.0(2) . . ? C33 C32 C34 111.2(2) . . ? C33 C32 C28 111.1(2) . . ? C34 C32 C28 110.6(2) . . ? C1S N1S Na1 174.3(7) . . ? C3S N2S Na1 167.1(6) . . ? N1S C1S C2S 178.6(9) . . ? N2S C3S C4S 177.1(10) . . ? C6S C5S C10S 117.3(15) . . ? C5S C6S C7S 125.8(19) . . ? C8S C7S C6S 115.4(17) . . ? C9S C8S C7S 120.9(13) . . ? C8S C9S C10S 121.5(9) . . ? C9S C10S C5S 119.0(10) . . ? C9S C10S C11S 120.3(8) . . ? C5S C10S C11S 120.6(10) . . ? _diffrn_measured_fraction_theta_max 0.952 _diffrn_reflns_theta_full 25.00 _diffrn_measured_fraction_theta_full 0.999 _refine_diff_density_max 0.839 _refine_diff_density_min -0.352 _refine_diff_density_rms 0.053 #===END data_jfig365 _database_code_depnum_ccdc_archive 'CCDC 785485' #TrackingRef 'cif-full.cif' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common HMn(CO)3(CNArDipp2) _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C65 H75 Mn N2 O3' _chemical_formula_weight 987.21 loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Mn Mn 0.3368 0.7283 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting Monoclinic _symmetry_space_group_name_H-M C2/c loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, y, -z+1/2' 'x+1/2, y+1/2, z' '-x+1/2, y+1/2, -z+1/2' '-x, -y, -z' 'x, -y, z-1/2' '-x+1/2, -y+1/2, -z' 'x+1/2, -y+1/2, z-1/2' _cell_length_a 23.733(6) _cell_length_b 23.631(6) _cell_length_c 21.360(5) _cell_angle_alpha 90.00 _cell_angle_beta 108.669(4) _cell_angle_gamma 90.00 _cell_volume 11349(5) _cell_formula_units_Z 8 _cell_measurement_temperature 100(2) _cell_measurement_reflns_used 6326 _cell_measurement_theta_min 2.24 _cell_measurement_theta_max 22.00 _exptl_crystal_description Block _exptl_crystal_colour red _exptl_crystal_size_max 0.22 _exptl_crystal_size_mid 0.16 _exptl_crystal_size_min 0.08 _exptl_crystal_density_meas 'not measured' _exptl_crystal_density_diffrn 1.156 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 4224 _exptl_absorpt_coefficient_mu 0.279 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.9413 _exptl_absorpt_correction_T_max 0.9781 _exptl_absorpt_process_details TWINABS _exptl_special_details ; ? ; _diffrn_ambient_temperature 100(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'Bruker APEX-II CCD' _diffrn_measurement_method '\f and \w scans' _diffrn_reflns_number 10317 _diffrn_reflns_av_R_equivalents 0.0669 _diffrn_reflns_av_sigmaI/netI 0.1049 _diffrn_reflns_limit_h_min -28 _diffrn_reflns_limit_h_max 26 _diffrn_reflns_limit_k_min 0 _diffrn_reflns_limit_k_max 28 _diffrn_reflns_limit_l_min 0 _diffrn_reflns_limit_l_max 25 _diffrn_reflns_theta_min 1.25 _diffrn_reflns_theta_max 25.00 _reflns_number_total 10317 _reflns_number_gt 7001 _reflns_threshold_expression >2\s(I) _computing_data_collection 'Bruker APEX2' _computing_cell_refinement 'Bruker SAINT' _computing_data_reduction 'Bruker SAINT' _computing_structure_solution 'SHELXS-97 (Sheldrick, 2008)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 2008)' _computing_molecular_graphics 'Bruker SHELXTL' _computing_publication_material 'Bruker SHELXTL' _refine_special_details ; Refinement of F^2^ against ALL reflections. The weighted R-factor wR and goodness of fit S are based on F^2^, conventional R-factors R are based on F, with F set to zero for negative F^2^. The threshold expression of F^2^ > 2\s(F^2^) is used only for calculating R-factors(gt) etc. and is not relevant to the choice of reflections for refinement. R-factors based on F^2^ are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger. ; _refine_ls_structure_factor_coef Fsqd _refine_ls_matrix_type full _refine_ls_weighting_scheme calc _refine_ls_weighting_details 'calc w=1/[\s^2^(Fo^2^)+(0.1086P)^2^+52.5121P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment constr _refine_ls_extinction_method SHELXL _refine_ls_extinction_coef 0.00028(11) _refine_ls_extinction_expression Fc^*^=kFc[1+0.001xFc^2^\l^3^/sin(2\q)]^-1/4^ _refine_ls_number_reflns 10318 _refine_ls_number_parameters 689 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.1438 _refine_ls_R_factor_gt 0.0953 _refine_ls_wR_factor_ref 0.2470 _refine_ls_wR_factor_gt 0.2181 _refine_ls_goodness_of_fit_ref 1.022 _refine_ls_restrained_S_all 1.022 _refine_ls_shift/su_max 0.000 _refine_ls_shift/su_mean 0.000 loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_occupancy _atom_site_symmetry_multiplicity _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group Mn1 Mn -0.00375(19) 0.43326(8) 0.23534(8) 0.0189(6) Uani 0.50 1 d P . . Mn2 Mn 0.4980(4) 0.43591(8) 0.23778(15) 0.0201(9) Uani 0.50 1 d P . . O1 O -0.0327(3) 0.3514(4) 0.1339(4) 0.066(2) Uani 0.75 1 d P . . O2 O 0.0244(3) 0.5232(4) 0.3599(3) 0.063(2) Uani 0.75 1 d P . . O3 O 0.4429(4) 0.4407(4) 0.3628(4) 0.064(2) Uani 0.75 1 d P . . O4 O 0.6152(4) 0.4344(3) 0.3608(3) 0.055(2) Uani 0.75 1 d P . . N1 N 0.1300(2) 0.4325(2) 0.2530(3) 0.0226(10) Uani 1 1 d . . . N2 N 0.5000 0.5649(3) 0.2500 0.0228(15) Uani 1 2 d S . . N3 N 0.5000 0.3056(3) 0.2500 0.0218(15) Uani 1 2 d S . . C1 C -0.0205(4) 0.3815(4) 0.1772(5) 0.034(2) Uani 0.75 1 d P . . C2 C 0.0167(4) 0.4870(4) 0.3204(5) 0.037(2) Uani 0.75 1 d P . . C3 C 0.0810(3) 0.4325(3) 0.2524(4) 0.0404(16) Uani 1 1 d . . . C4 C 0.1891(2) 0.4300(2) 0.2550(3) 0.0185(11) Uani 1 1 d . . . C5 C 0.2327(3) 0.4140(2) 0.3141(3) 0.0195(12) Uani 1 1 d . . . C6 C 0.2911(3) 0.4118(3) 0.3141(3) 0.0244(14) Uani 1 1 d . . . H6 H 0.3216 0.4015 0.3535 0.029 Uiso 1 1 calc R . . C7 C 0.3060(3) 0.4240(2) 0.2586(3) 0.0249(14) Uani 1 1 d . . . H7 H 0.3461 0.4208 0.2595 0.030 Uiso 1 1 calc R . . C8 C 0.2626(3) 0.4411(3) 0.2016(3) 0.0239(13) Uani 1 1 d . . . H8 H 0.2736 0.4501 0.1637 0.029 Uiso 1 1 calc R . . C9 C 0.2024(2) 0.4457(2) 0.1980(3) 0.0177(12) Uani 1 1 d . . . C10 C 0.2153(3) 0.3992(3) 0.3738(3) 0.0252(14) Uani 1 1 d . . . C11 C 0.2029(3) 0.3437(3) 0.3852(3) 0.0230(13) Uani 1 1 d . . . C12 C 0.1855(3) 0.3316(3) 0.4405(3) 0.0354(16) Uani 1 1 d . . . H12 H 0.1767 0.2938 0.4490 0.042 Uiso 1 1 calc R . . C13 C 0.1810(3) 0.3744(3) 0.4827(3) 0.0374(16) Uani 1 1 d . . . H13 H 0.1692 0.3657 0.5201 0.045 Uiso 1 1 calc R . . C14 C 0.1934(3) 0.4292(3) 0.4711(4) 0.0419(18) Uani 1 1 d . . . H14 H 0.1899 0.4579 0.5008 0.050 Uiso 1 1 calc R . . C15 C 0.2109(3) 0.4439(3) 0.4172(3) 0.0341(16) Uani 1 1 d . . . C16 C 0.2073(3) 0.2958(3) 0.3392(3) 0.0349(16) Uani 1 1 d . . . H16 H 0.2243 0.3117 0.3056 0.042 Uiso 1 1 calc R . . C17 C 0.2489(4) 0.2486(3) 0.3768(4) 0.053(2) Uani 1 1 d . . . H17B H 0.2327 0.2319 0.4095 0.080 Uiso 1 1 calc R . . H17C H 0.2883 0.2644 0.3994 0.080 Uiso 1 1 calc R . . H17A H 0.2521 0.2193 0.3456 0.080 Uiso 1 1 calc R . . C18 C 0.1453(4) 0.2720(3) 0.3025(4) 0.056(2) Uani 1 1 d . . . H18A H 0.1491 0.2402 0.2746 0.084 Uiso 1 1 calc R . . H18B H 0.1208 0.3016 0.2748 0.084 Uiso 1 1 calc R . . H18C H 0.1266 0.2588 0.3346 0.084 Uiso 1 1 calc R . . C19 C 0.2245(4) 0.5049(3) 0.4054(4) 0.050(2) Uani 1 1 d . . . H19 H 0.2377 0.5056 0.3654 0.060 Uiso 1 1 calc R . . C20 C 0.2750(5) 0.5289(4) 0.4629(6) 0.084(3) Uani 1 1 d . . . H20B H 0.2640 0.5272 0.5034 0.125 Uiso 1 1 calc R . . H20C H 0.2823 0.5683 0.4535 0.125 Uiso 1 1 calc R . . H20A H 0.3111 0.5065 0.4688 0.125 Uiso 1 1 calc R . . C21 C 0.1692(5) 0.5408(4) 0.3906(5) 0.067(3) Uani 1 1 d . . . H21A H 0.1376 0.5243 0.3536 0.100 Uiso 1 1 calc R . . H21C H 0.1779 0.5792 0.3789 0.100 Uiso 1 1 calc R . . H21B H 0.1562 0.5424 0.4297 0.100 Uiso 1 1 calc R . . C22 C 0.1564(3) 0.4652(3) 0.1365(3) 0.0224(13) Uani 1 1 d . . . C23 C 0.1399(3) 0.5227(3) 0.1325(3) 0.0251(14) Uani 1 1 d . . . C24 C 0.0977(3) 0.5414(3) 0.0740(3) 0.0296(14) Uani 1 1 d . . . H24 H 0.0852 0.5798 0.0704 0.036 Uiso 1 1 calc R . . C25 C 0.0742(3) 0.5057(3) 0.0223(3) 0.0356(16) Uani 1 1 d . . . H25 H 0.0468 0.5195 -0.0176 0.043 Uiso 1 1 calc R . . C26 C 0.0905(3) 0.4488(3) 0.0280(4) 0.0456(19) Uani 1 1 d . . . H26 H 0.0727 0.4240 -0.0079 0.055 Uiso 1 1 calc R . . C27 C 0.1317(3) 0.4273(3) 0.0844(3) 0.0320(15) Uani 1 1 d . . . C28 C 0.1658(3) 0.5644(3) 0.1883(3) 0.0316(15) Uani 1 1 d . . . H28 H 0.1960 0.5441 0.2251 0.038 Uiso 1 1 calc R . . C29 C 0.1175(3) 0.5865(3) 0.2144(4) 0.0439(19) Uani 1 1 d . . . H29B H 0.0875 0.6068 0.1791 0.066 Uiso 1 1 calc R . . H29C H 0.1351 0.6123 0.2514 0.066 Uiso 1 1 calc R . . H29A H 0.0987 0.5547 0.2295 0.066 Uiso 1 1 calc R . . C30 C 0.1962(3) 0.6138(3) 0.1669(4) 0.0434(18) Uani 1 1 d . . . H30A H 0.2253 0.5994 0.1471 0.065 Uiso 1 1 calc R . . H30C H 0.2165 0.6371 0.2055 0.065 Uiso 1 1 calc R . . H30B H 0.1664 0.6366 0.1344 0.065 Uiso 1 1 calc R . . C31 C 0.1491(3) 0.3662(3) 0.0902(4) 0.047(2) Uani 1 1 d . . . H31 H 0.1873 0.3625 0.1273 0.056 Uiso 1 1 calc R . . C32 C 0.1589(4) 0.3424(4) 0.0275(4) 0.063(2) Uani 1 1 d . . . H32B H 0.1220 0.3458 -0.0098 0.095 Uiso 1 1 calc R . . H32A H 0.1703 0.3024 0.0344 0.095 Uiso 1 1 calc R . . H32C H 0.1905 0.3637 0.0179 0.095 Uiso 1 1 calc R . . C33 C 0.1023(6) 0.3310(3) 0.1072(5) 0.078(3) Uani 1 1 d . . . H33B H 0.0644 0.3337 0.0713 0.117 Uiso 1 1 calc R . . H33C H 0.0972 0.3452 0.1482 0.117 Uiso 1 1 calc R . . H33A H 0.1151 0.2914 0.1132 0.117 Uiso 1 1 calc R . . C34 C 0.4656(4) 0.4381(4) 0.3210(6) 0.045(2) Uani 0.75 1 d P . . C35 C 0.5715(4) 0.4360(3) 0.3197(4) 0.0236(18) Uani 0.75 1 d P . . C36 C 0.5000 0.5155(4) 0.2500 0.0253(19) Uani 1 2 d S . . C37 C 0.5000 0.3553(4) 0.2500 0.0244(19) Uani 1 2 d S . . C38 C 0.5000 0.6246(3) 0.2500 0.0191(17) Uani 1 2 d S . . C39 C 0.4984(2) 0.6524(3) 0.3068(3) 0.0222(13) Uani 1 1 d . . . C40 C 0.4981(3) 0.7116(3) 0.3054(3) 0.0241(14) Uani 1 1 d . . . H40 H 0.4965 0.7321 0.3430 0.029 Uiso 1 1 calc R . . C41 C 0.5000 0.7403(4) 0.2500 0.032(2) Uani 1 2 d S . . H41 H 0.5000 0.7805 0.2500 0.038 Uiso 1 2 calc SR . . C42 C 0.4948(3) 0.6220(2) 0.3658(3) 0.0222(13) Uani 1 1 d . . . C43 C 0.4390(3) 0.6033(3) 0.3687(3) 0.0270(14) Uani 1 1 d . . . C44 C 0.4353(3) 0.5768(2) 0.4239(3) 0.0309(15) Uani 1 1 d . . . H44 H 0.3977 0.5650 0.4260 0.037 Uiso 1 1 calc R . . C45 C 0.4862(3) 0.5671(3) 0.4771(3) 0.0348(16) Uani 1 1 d . . . H45 H 0.4834 0.5482 0.5153 0.042 Uiso 1 1 calc R . . C46 C 0.5410(3) 0.5847(3) 0.4746(3) 0.0327(15) Uani 1 1 d . . . H46 H 0.5757 0.5779 0.5113 0.039 Uiso 1 1 calc R . . C47 C 0.5463(3) 0.6125(2) 0.4186(3) 0.0253(13) Uani 1 1 d . . . C48 C 0.3827(3) 0.6135(3) 0.3119(3) 0.0292(15) Uani 1 1 d . . . H48 H 0.3944 0.6326 0.2761 0.035 Uiso 1 1 calc R . . C49 C 0.3390(3) 0.6526(3) 0.3301(4) 0.0426(18) Uani 1 1 d . . . H49A H 0.3044 0.6593 0.2910 0.064 Uiso 1 1 calc R . . H49C H 0.3586 0.6887 0.3464 0.064 Uiso 1 1 calc R . . H49B H 0.3261 0.6348 0.3647 0.064 Uiso 1 1 calc R . . C50 C 0.3515(3) 0.5579(3) 0.2833(4) 0.0411(17) Uani 1 1 d . . . H50C H 0.3784 0.5345 0.2677 0.062 Uiso 1 1 calc R . . H50B H 0.3155 0.5663 0.2462 0.062 Uiso 1 1 calc R . . H50A H 0.3406 0.5374 0.3176 0.062 Uiso 1 1 calc R . . C51 C 0.6075(3) 0.6300(3) 0.4157(3) 0.0364(17) Uani 1 1 d . . . H51 H 0.6008 0.6610 0.3821 0.044 Uiso 1 1 calc R . . C52 C 0.6480(3) 0.6539(4) 0.4807(4) 0.050(2) Uani 1 1 d . . . H52C H 0.6856 0.6661 0.4752 0.075 Uiso 1 1 calc R . . H52A H 0.6559 0.6246 0.5149 0.075 Uiso 1 1 calc R . . H52B H 0.6286 0.6862 0.4939 0.075 Uiso 1 1 calc R . . C53 C 0.6373(4) 0.5837(4) 0.3931(4) 0.066(3) Uani 1 1 d . . . H53C H 0.6771 0.5959 0.3944 0.100 Uiso 1 1 calc R . . H53A H 0.6141 0.5733 0.3477 0.100 Uiso 1 1 calc R . . H53B H 0.6406 0.5508 0.4221 0.100 Uiso 1 1 calc R . . C54 C 0.5000 0.2470(3) 0.2500 0.0231(19) Uani 1 2 d S . . C55 C 0.5299(3) 0.2188(2) 0.3082(3) 0.0203(13) Uani 1 1 d . . . C56 C 0.5289(3) 0.1603(3) 0.3075(3) 0.0284(14) Uani 1 1 d . . . H56 H 0.5481 0.1399 0.3469 0.034 Uiso 1 1 calc R . . C57 C 0.5000 0.1314(3) 0.2500 0.030(2) Uani 1 2 d S . . H57 H 0.5000 0.0912 0.2500 0.037 Uiso 1 2 calc SR . . C58 C 0.5613(3) 0.2514(3) 0.3706(3) 0.0256(14) Uani 1 1 d . . . C59 C 0.5294(3) 0.2683(3) 0.4135(3) 0.0343(16) Uani 1 1 d . . . C60 C 0.5575(3) 0.3003(3) 0.4686(3) 0.0372(16) Uani 1 1 d . . . H60 H 0.5364 0.3119 0.4975 0.045 Uiso 1 1 calc R . . C61 C 0.6165(3) 0.3155(3) 0.4819(3) 0.0360(16) Uani 1 1 d . . . H61 H 0.6355 0.3379 0.5197 0.043 Uiso 1 1 calc R . . C62 C 0.6481(3) 0.2984(3) 0.4406(3) 0.0339(16) Uani 1 1 d . . . H62 H 0.6887 0.3089 0.4510 0.041 Uiso 1 1 calc R . . C63 C 0.6211(3) 0.2659(3) 0.3838(3) 0.0270(14) Uani 1 1 d . . . C64 C 0.4645(3) 0.2512(3) 0.3999(4) 0.0411(18) Uani 1 1 d . . . H64 H 0.4539 0.2248 0.3612 0.049 Uiso 1 1 calc R . . C65 C 0.4243(3) 0.3032(4) 0.3795(4) 0.052(2) Uani 1 1 d . . . H65C H 0.4338 0.3302 0.4162 0.078 Uiso 1 1 calc R . . H65A H 0.3826 0.2915 0.3682 0.078 Uiso 1 1 calc R . . H65B H 0.4309 0.3210 0.3410 0.078 Uiso 1 1 calc R . . C66 C 0.4532(4) 0.2206(4) 0.4558(5) 0.061(2) Uani 1 1 d . . . H66B H 0.4758 0.1852 0.4642 0.092 Uiso 1 1 calc R . . H66A H 0.4106 0.2123 0.4444 0.092 Uiso 1 1 calc R . . H66C H 0.4657 0.2444 0.4955 0.092 Uiso 1 1 calc R . . C67 C 0.6567(3) 0.2475(3) 0.3406(4) 0.0380(17) Uani 1 1 d . . . H67 H 0.6306 0.2234 0.3043 0.046 Uiso 1 1 calc R . . C68 C 0.6765(4) 0.2991(4) 0.3088(4) 0.055(2) Uani 1 1 d . . . H68C H 0.6967 0.3263 0.3434 0.083 Uiso 1 1 calc R . . H68A H 0.6415 0.3171 0.2776 0.083 Uiso 1 1 calc R . . H68B H 0.7037 0.2868 0.2854 0.083 Uiso 1 1 calc R . . C69 C 0.7101(4) 0.2122(3) 0.3794(4) 0.055(2) Uani 1 1 d . . . H69B H 0.7294 0.1962 0.3491 0.083 Uiso 1 1 calc R . . H69A H 0.6969 0.1815 0.4022 0.083 Uiso 1 1 calc R . . H69C H 0.7385 0.2362 0.4120 0.083 Uiso 1 1 calc R . . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 Mn1 0.0150(13) 0.0206(7) 0.0204(19) -0.0004(7) 0.005(2) 0.0019(9) Mn2 0.0251(13) 0.0126(7) 0.024(3) -0.0004(8) 0.009(3) 0.0007(11) O1 0.028(4) 0.126(8) 0.040(4) -0.003(5) 0.005(3) 0.001(5) O2 0.041(4) 0.111(7) 0.035(4) -0.001(4) 0.009(3) 0.004(5) O3 0.075(6) 0.060(5) 0.052(5) -0.005(4) 0.016(4) 0.006(4) O4 0.096(6) 0.023(4) 0.024(3) -0.002(3) -0.012(4) 0.002(4) N1 0.017(3) 0.017(2) 0.031(3) -0.002(2) 0.003(2) -0.003(2) N2 0.026(4) 0.018(4) 0.026(4) 0.000 0.010(3) 0.000 N3 0.018(4) 0.005(3) 0.039(4) 0.000 0.005(3) 0.000 C1 0.011(4) 0.046(6) 0.048(6) 0.010(5) 0.011(4) 0.007(4) C2 0.024(5) 0.043(6) 0.046(6) 0.026(5) 0.014(4) 0.014(4) C3 0.034(4) 0.024(3) 0.060(5) 0.010(3) 0.011(4) 0.012(3) C4 0.010(3) 0.016(3) 0.030(3) 0.001(3) 0.007(2) -0.002(2) C5 0.023(3) 0.016(3) 0.018(3) -0.002(2) 0.004(2) -0.001(2) C6 0.017(3) 0.027(3) 0.026(3) 0.000(3) 0.002(3) -0.001(3) C7 0.015(3) 0.022(3) 0.037(4) -0.005(3) 0.007(3) 0.001(2) C8 0.026(3) 0.019(3) 0.030(3) 0.002(3) 0.015(3) 0.003(3) C9 0.020(3) 0.012(3) 0.023(3) -0.005(2) 0.008(2) -0.001(2) C10 0.022(3) 0.029(4) 0.026(3) 0.005(3) 0.009(3) 0.000(3) C11 0.019(3) 0.024(3) 0.024(3) 0.001(3) 0.003(3) 0.001(3) C12 0.031(4) 0.038(4) 0.038(4) 0.012(3) 0.012(3) -0.001(3) C13 0.040(4) 0.047(4) 0.033(4) 0.004(3) 0.022(3) 0.006(3) C14 0.048(4) 0.044(4) 0.043(4) -0.006(4) 0.027(4) 0.002(4) C15 0.046(4) 0.021(3) 0.042(4) 0.000(3) 0.023(3) 0.002(3) C16 0.042(4) 0.020(3) 0.045(4) 0.004(3) 0.017(3) -0.010(3) C17 0.056(5) 0.042(5) 0.064(5) 0.002(4) 0.024(4) 0.025(4) C18 0.055(5) 0.039(4) 0.066(5) -0.016(4) 0.009(4) -0.007(4) C19 0.092(7) 0.025(4) 0.051(5) -0.006(3) 0.048(5) -0.006(4) C20 0.070(7) 0.056(6) 0.128(9) -0.005(6) 0.037(7) -0.028(5) C21 0.091(8) 0.037(5) 0.065(6) -0.007(4) 0.016(5) -0.002(5) C22 0.023(3) 0.025(3) 0.020(3) 0.003(3) 0.008(3) 0.006(3) C23 0.019(3) 0.029(3) 0.030(3) 0.015(3) 0.012(3) 0.005(3) C24 0.024(3) 0.038(4) 0.027(3) 0.001(3) 0.009(3) 0.004(3) C25 0.026(4) 0.056(5) 0.022(3) 0.008(3) 0.004(3) 0.006(3) C26 0.041(5) 0.060(5) 0.035(4) -0.007(4) 0.011(3) -0.005(4) C27 0.028(4) 0.035(4) 0.029(3) -0.008(3) 0.004(3) 0.001(3) C28 0.034(4) 0.025(3) 0.035(4) 0.001(3) 0.010(3) 0.005(3) C29 0.050(5) 0.032(4) 0.060(5) -0.004(4) 0.031(4) -0.002(3) C30 0.040(4) 0.040(4) 0.047(4) 0.010(4) 0.009(3) -0.010(4) C31 0.044(5) 0.039(4) 0.043(4) -0.016(4) -0.007(4) 0.005(4) C32 0.071(6) 0.047(5) 0.073(6) -0.015(5) 0.025(5) 0.010(5) C33 0.129(9) 0.030(5) 0.081(7) -0.009(4) 0.042(7) -0.002(6) C34 0.035(6) 0.031(5) 0.057(7) -0.001(5) -0.003(5) 0.005(5) C35 0.039(5) 0.008(4) 0.027(5) 0.002(3) 0.016(4) 0.004(4) C36 0.021(5) 0.021(5) 0.036(5) 0.000 0.012(4) 0.000 C37 0.005(4) 0.029(5) 0.035(5) 0.000 0.000(4) 0.000 C38 0.020(4) 0.007(4) 0.035(5) 0.000 0.015(4) 0.000 C39 0.014(3) 0.025(3) 0.024(3) -0.003(3) 0.002(2) -0.002(3) C40 0.025(3) 0.021(3) 0.024(3) -0.005(3) 0.004(3) 0.000(3) C41 0.035(6) 0.020(5) 0.040(5) 0.000 0.013(5) 0.000 C42 0.029(3) 0.015(3) 0.024(3) -0.007(2) 0.009(3) -0.003(3) C43 0.032(4) 0.021(3) 0.032(3) -0.012(3) 0.016(3) -0.005(3) C44 0.035(4) 0.020(3) 0.044(4) -0.006(3) 0.022(3) -0.008(3) C45 0.055(5) 0.027(4) 0.028(3) 0.002(3) 0.021(3) 0.000(3) C46 0.037(4) 0.029(4) 0.029(3) 0.003(3) 0.007(3) 0.004(3) C47 0.027(3) 0.019(3) 0.031(3) 0.002(3) 0.012(3) -0.005(3) C48 0.024(4) 0.028(3) 0.040(4) -0.005(3) 0.017(3) -0.005(3) C49 0.034(4) 0.043(4) 0.051(4) -0.010(4) 0.013(3) 0.009(3) C50 0.032(4) 0.042(4) 0.052(4) -0.015(4) 0.019(3) -0.006(3) C51 0.024(4) 0.050(5) 0.032(4) 0.013(3) 0.005(3) -0.004(3) C52 0.033(4) 0.065(6) 0.050(5) -0.013(4) 0.009(4) -0.008(4) C53 0.030(5) 0.111(8) 0.058(5) -0.032(5) 0.014(4) -0.013(5) C54 0.027(5) 0.012(4) 0.037(5) 0.000 0.020(4) 0.000 C55 0.022(3) 0.014(3) 0.031(3) 0.003(2) 0.017(3) 0.004(2) C56 0.034(4) 0.025(3) 0.033(3) 0.004(3) 0.020(3) 0.006(3) C57 0.055(6) 0.012(4) 0.034(5) 0.000 0.028(5) 0.000 C58 0.031(4) 0.016(3) 0.030(3) 0.002(3) 0.009(3) 0.002(3) C59 0.031(4) 0.030(4) 0.044(4) -0.007(3) 0.014(3) 0.001(3) C60 0.039(4) 0.035(4) 0.035(4) -0.005(3) 0.008(3) 0.003(3) C61 0.043(4) 0.033(4) 0.025(3) -0.005(3) 0.000(3) -0.002(3) C62 0.027(4) 0.032(4) 0.034(4) 0.008(3) -0.002(3) -0.005(3) C63 0.029(4) 0.020(3) 0.028(3) 0.006(3) 0.004(3) -0.005(3) C64 0.021(4) 0.058(5) 0.046(4) -0.020(4) 0.013(3) -0.003(3) C65 0.035(4) 0.081(6) 0.044(4) 0.013(4) 0.018(4) 0.015(4) C66 0.042(5) 0.061(6) 0.086(6) -0.007(5) 0.028(5) -0.017(4) C67 0.028(4) 0.040(4) 0.047(4) 0.003(3) 0.015(3) -0.002(3) C68 0.055(5) 0.063(6) 0.060(5) 0.017(4) 0.038(4) 0.000(4) C69 0.060(6) 0.041(5) 0.073(6) -0.003(4) 0.034(5) 0.015(4) _geom_special_details ; All s.u.'s (except the s.u. in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell s.u.'s are taken into account individually in the estimation of s.u.'s in distances, angles and torsion angles; correlations between s.u.'s in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell s.u.'s is used for estimating s.u.'s involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag Mn1 Mn1 0.594(3) 2 ? Mn1 C1 1.697(11) . ? Mn1 C2 1.701(12) 2 ? Mn1 C3 1.925(8) . ? Mn1 C3 1.933(8) 2 ? Mn1 C2 2.142(12) . ? Mn1 C1 2.151(11) 2 ? Mn2 Mn2 0.500(6) 2_655 ? Mn2 C35 1.713(11) 2_655 ? Mn2 C34 1.737(13) 2_655 ? Mn2 C36 1.898(9) . ? Mn2 C37 1.920(9) . ? Mn2 C35 2.037(11) . ? Mn2 C34 2.151(13) . ? O1 C1 1.129(11) . ? O2 C2 1.174(12) . ? O3 C34 1.183(13) . ? O4 C35 1.124(10) . ? N1 C3 1.159(8) . ? N1 C4 1.392(7) . ? N2 C36 1.166(10) . ? N2 C38 1.412(10) . ? N3 C37 1.174(10) . ? N3 C54 1.386(10) . ? C1 Mn1 2.151(11) 2 ? C2 Mn1 1.701(12) 2 ? C3 Mn1 1.933(8) 2 ? C4 C9 1.402(8) . ? C4 C5 1.404(8) . ? C5 C6 1.389(8) . ? C5 C10 1.502(8) . ? C6 C7 1.371(8) . ? C6 H6 0.9500 . ? C7 C8 1.381(8) . ? C7 H7 0.9500 . ? C8 C9 1.410(8) . ? C8 H8 0.9500 . ? C9 C22 1.487(8) . ? C10 C11 1.382(9) . ? C10 C15 1.432(9) . ? C11 C12 1.400(9) . ? C11 C16 1.524(9) . ? C12 C13 1.381(10) . ? C12 H12 0.9500 . ? C13 C14 1.367(10) . ? C13 H13 0.9500 . ? C14 C15 1.388(9) . ? C14 H14 0.9500 . ? C15 C19 1.515(9) . ? C16 C17 1.535(10) . ? C16 C18 1.536(10) . ? C16 H16 1.0000 . ? C17 H17B 0.9800 . ? C17 H17C 0.9800 . ? C17 H17A 0.9800 . ? C18 H18A 0.9800 . ? C18 H18B 0.9800 . ? C18 H18C 0.9800 . ? C19 C21 1.510(12) . ? C19 C20 1.525(13) . ? C19 H19 1.0000 . ? C20 H20B 0.9800 . ? C20 H20C 0.9800 . ? C20 H20A 0.9800 . ? C21 H21A 0.9800 . ? C21 H21C 0.9800 . ? C21 H21B 0.9800 . ? C22 C27 1.402(9) . ? C22 C23 1.408(8) . ? C23 C24 1.399(8) . ? C23 C28 1.517(9) . ? C24 C25 1.359(9) . ? C24 H24 0.9500 . ? C25 C26 1.395(10) . ? C25 H25 0.9500 . ? C26 C27 1.382(10) . ? C26 H26 0.9500 . ? C27 C31 1.495(10) . ? C28 C30 1.518(9) . ? C28 C29 1.518(9) . ? C28 H28 1.0000 . ? C29 H29B 0.9800 . ? C29 H29C 0.9800 . ? C29 H29A 0.9800 . ? C30 H30A 0.9800 . ? C30 H30C 0.9800 . ? C30 H30B 0.9800 . ? C31 C33 1.524(13) . ? C31 C32 1.537(11) . ? C31 H31 1.0000 . ? C32 H32B 0.9800 . ? C32 H32A 0.9800 . ? C32 H32C 0.9800 . ? C33 H33B 0.9800 . ? C33 H33C 0.9800 . ? C33 H33A 0.9800 . ? C34 Mn2 1.737(13) 2_655 ? C35 Mn2 1.713(11) 2_655 ? C36 Mn2 1.898(9) 2_655 ? C37 Mn2 1.920(9) 2_655 ? C38 C39 1.391(7) . ? C38 C39 1.391(7) 2_655 ? C39 C40 1.397(8) . ? C39 C42 1.477(8) . ? C40 C41 1.378(7) . ? C40 H40 0.9500 . ? C41 C40 1.378(7) 2_655 ? C41 H41 0.9500 . ? C42 C47 1.391(8) . ? C42 C43 1.418(9) . ? C43 C44 1.361(9) . ? C43 C48 1.508(9) . ? C44 C45 1.388(10) . ? C44 H44 0.9500 . ? C45 C46 1.385(10) . ? C45 H45 0.9500 . ? C46 C47 1.404(9) . ? C46 H46 0.9500 . ? C47 C51 1.531(9) . ? C48 C49 1.529(9) . ? C48 C50 1.536(9) . ? C48 H48 1.0000 . ? C49 H49A 0.9800 . ? C49 H49C 0.9800 . ? C49 H49B 0.9800 . ? C50 H50C 0.9800 . ? C50 H50B 0.9800 . ? C50 H50A 0.9800 . ? C51 C53 1.467(11) . ? C51 C52 1.522(10) . ? C51 H51 1.0000 . ? C52 H52C 0.9800 . ? C52 H52A 0.9800 . ? C52 H52B 0.9800 . ? C53 H53C 0.9800 . ? C53 H53A 0.9800 . ? C53 H53B 0.9800 . ? C54 C55 1.388(7) 2_655 ? C54 C55 1.388(7) . ? C55 C56 1.384(8) . ? C55 C58 1.514(9) . ? C56 C57 1.382(8) . ? C56 H56 0.9500 . ? C57 C56 1.382(8) 2_655 ? C57 H57 0.9500 . ? C58 C63 1.398(9) . ? C58 C59 1.420(9) . ? C59 C60 1.379(9) . ? C59 C64 1.527(9) . ? C60 C61 1.383(10) . ? C60 H60 0.9500 . ? C61 C62 1.389(10) . ? C61 H61 0.9500 . ? C62 C63 1.407(9) . ? C62 H62 0.9500 . ? C63 C67 1.500(9) . ? C64 C66 1.492(11) . ? C64 C65 1.529(11) . ? C64 H64 1.0000 . ? C65 H65C 0.9800 . ? C65 H65A 0.9800 . ? C65 H65B 0.9800 . ? C66 H66B 0.9800 . ? C66 H66A 0.9800 . ? C66 H66C 0.9800 . ? C67 C69 1.524(10) . ? C67 C68 1.540(10) . ? C67 H67 1.0000 . ? C68 H68C 0.9800 . ? C68 H68A 0.9800 . ? C68 H68B 0.9800 . ? C69 H69B 0.9800 . ? C69 H69A 0.9800 . ? C69 H69C 0.9800 . ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag Mn1 Mn1 C1 133.9(3) 2 . ? Mn1 Mn1 C2 131.7(3) 2 2 ? C1 Mn1 C2 94.5(4) . 2 ? Mn1 Mn1 C3 81.9(9) 2 . ? C1 Mn1 C3 96.7(4) . . ? C2 Mn1 C3 94.8(4) 2 . ? Mn1 Mn1 C3 80.4(9) 2 2 ? C1 Mn1 C3 94.7(4) . 2 ? C2 Mn1 C3 97.8(4) 2 2 ? C3 Mn1 C3 162.26(12) . 2 ? Mn1 Mn1 C2 36.4(2) 2 . ? C1 Mn1 C2 170.0(4) . . ? C2 Mn1 C2 95.3(5) 2 . ? C3 Mn1 C2 84.6(4) . . ? C3 Mn1 C2 81.8(3) 2 . ? Mn1 Mn1 C1 34.7(2) 2 2 ? C1 Mn1 C1 99.3(5) . 2 ? C2 Mn1 C1 166.1(4) 2 2 ? C3 Mn1 C1 81.8(3) . 2 ? C3 Mn1 C1 83.0(3) 2 2 ? C2 Mn1 C1 71.1(3) . 2 ? Mn2 Mn2 C35 124(2) 2_655 2_655 ? Mn2 Mn2 C34 142(2) 2_655 2_655 ? C35 Mn2 C34 94.0(4) 2_655 2_655 ? Mn2 Mn2 C36 82.43(9) 2_655 . ? C35 Mn2 C36 94.2(3) 2_655 . ? C34 Mn2 C36 94.3(4) 2_655 . ? Mn2 Mn2 C37 82.53(9) 2_655 . ? C35 Mn2 C37 94.3(3) 2_655 . ? C34 Mn2 C37 97.5(4) 2_655 . ? C36 Mn2 C37 164.96(18) . . ? Mn2 Mn2 C35 43.9(18) 2_655 . ? C35 Mn2 C35 168.3(4) 2_655 . ? C34 Mn2 C35 97.7(5) 2_655 . ? C36 Mn2 C35 84.5(3) . . ? C37 Mn2 C35 84.7(3) . . ? Mn2 Mn2 C34 30.1(17) 2_655 . ? C35 Mn2 C34 94.3(5) 2_655 . ? C34 Mn2 C34 171.2(5) 2_655 . ? C36 Mn2 C34 82.1(3) . . ? C37 Mn2 C34 84.9(3) . . ? C35 Mn2 C34 74.0(3) . . ? C3 N1 C4 177.3(7) . . ? C36 N2 C38 180.000(2) . . ? C37 N3 C54 180.000(2) . . ? O1 C1 Mn1 173.0(9) . . ? O1 C1 Mn1 175.6(9) . 2 ? Mn1 C1 Mn1 11.48(11) . 2 ? O2 C2 Mn1 177.7(9) . 2 ? O2 C2 Mn1 169.4(8) . . ? Mn1 C2 Mn1 11.95(11) 2 . ? N1 C3 Mn1 170.3(7) . . ? N1 C3 Mn1 172.0(7) . 2 ? Mn1 C3 Mn1 17.70(11) . 2 ? N1 C4 C9 117.8(5) . . ? N1 C4 C5 118.9(5) . . ? C9 C4 C5 123.2(5) . . ? C6 C5 C4 117.2(5) . . ? C6 C5 C10 122.5(5) . . ? C4 C5 C10 120.3(5) . . ? C7 C6 C5 121.8(6) . . ? C7 C6 H6 119.1 . . ? C5 C6 H6 119.1 . . ? C6 C7 C8 119.9(5) . . ? C6 C7 H7 120.0 . . ? C8 C7 H7 120.0 . . ? C7 C8 C9 121.8(5) . . ? C7 C8 H8 119.1 . . ? C9 C8 H8 119.1 . . ? C4 C9 C8 115.9(5) . . ? C4 C9 C22 123.0(5) . . ? C8 C9 C22 121.1(5) . . ? C11 C10 C15 121.6(5) . . ? C11 C10 C5 120.1(5) . . ? C15 C10 C5 118.3(5) . . ? C10 C11 C12 118.5(6) . . ? C10 C11 C16 121.9(5) . . ? C12 C11 C16 119.5(6) . . ? C13 C12 C11 120.5(6) . . ? C13 C12 H12 119.8 . . ? C11 C12 H12 119.8 . . ? C14 C13 C12 120.6(6) . . ? C14 C13 H13 119.7 . . ? C12 C13 H13 119.7 . . ? C13 C14 C15 121.7(6) . . ? C13 C14 H14 119.1 . . ? C15 C14 H14 119.1 . . ? C14 C15 C10 117.0(6) . . ? C14 C15 C19 120.9(6) . . ? C10 C15 C19 122.1(6) . . ? C11 C16 C17 111.5(6) . . ? C11 C16 C18 110.4(6) . . ? C17 C16 C18 110.5(6) . . ? C11 C16 H16 108.1 . . ? C17 C16 H16 108.1 . . ? C18 C16 H16 108.1 . . ? C16 C17 H17B 109.5 . . ? C16 C17 H17C 109.5 . . ? H17B C17 H17C 109.5 . . ? C16 C17 H17A 109.5 . . ? H17B C17 H17A 109.5 . . ? H17C C17 H17A 109.5 . . ? C16 C18 H18A 109.5 . . ? C16 C18 H18B 109.5 . . ? H18A C18 H18B 109.5 . . ? C16 C18 H18C 109.5 . . ? H18A C18 H18C 109.5 . . ? H18B C18 H18C 109.5 . . ? C21 C19 C15 110.7(7) . . ? C21 C19 C20 111.5(7) . . ? C15 C19 C20 111.9(7) . . ? C21 C19 H19 107.5 . . ? C15 C19 H19 107.5 . . ? C20 C19 H19 107.5 . . ? C19 C20 H20B 109.5 . . ? C19 C20 H20C 109.5 . . ? H20B C20 H20C 109.5 . . ? C19 C20 H20A 109.5 . . ? H20B C20 H20A 109.5 . . ? H20C C20 H20A 109.5 . . ? C19 C21 H21A 109.5 . . ? C19 C21 H21C 109.5 . . ? H21A C21 H21C 109.5 . . ? C19 C21 H21B 109.5 . . ? H21A C21 H21B 109.5 . . ? H21C C21 H21B 109.5 . . ? C27 C22 C23 122.1(6) . . ? C27 C22 C9 120.3(5) . . ? C23 C22 C9 117.6(5) . . ? C24 C23 C22 117.6(6) . . ? C24 C23 C28 119.4(6) . . ? C22 C23 C28 123.0(5) . . ? C25 C24 C23 121.3(6) . . ? C25 C24 H24 119.3 . . ? C23 C24 H24 119.3 . . ? C24 C25 C26 119.8(6) . . ? C24 C25 H25 120.1 . . ? C26 C25 H25 120.1 . . ? C27 C26 C25 122.0(7) . . ? C27 C26 H26 119.0 . . ? C25 C26 H26 119.0 . . ? C26 C27 C22 117.1(6) . . ? C26 C27 C31 121.8(6) . . ? C22 C27 C31 121.2(6) . . ? C23 C28 C30 112.0(5) . . ? C23 C28 C29 110.4(6) . . ? C30 C28 C29 109.5(6) . . ? C23 C28 H28 108.3 . . ? C30 C28 H28 108.3 . . ? C29 C28 H28 108.3 . . ? C28 C29 H29B 109.5 . . ? C28 C29 H29C 109.5 . . ? H29B C29 H29C 109.5 . . ? C28 C29 H29A 109.5 . . ? H29B C29 H29A 109.5 . . ? H29C C29 H29A 109.5 . . ? C28 C30 H30A 109.5 . . ? C28 C30 H30C 109.5 . . ? H30A C30 H30C 109.5 . . ? C28 C30 H30B 109.5 . . ? H30A C30 H30B 109.5 . . ? H30C C30 H30B 109.5 . . ? C27 C31 C33 110.1(7) . . ? C27 C31 C32 113.4(7) . . ? C33 C31 C32 109.4(7) . . ? C27 C31 H31 107.9 . . ? C33 C31 H31 107.9 . . ? C32 C31 H31 107.9 . . ? C31 C32 H32B 109.5 . . ? C31 C32 H32A 109.5 . . ? H32B C32 H32A 109.5 . . ? C31 C32 H32C 109.5 . . ? H32B C32 H32C 109.5 . . ? H32A C32 H32C 109.5 . . ? C31 C33 H33B 109.5 . . ? C31 C33 H33C 109.5 . . ? H33B C33 H33C 109.5 . . ? C31 C33 H33A 109.5 . . ? H33B C33 H33A 109.5 . . ? H33C C33 H33A 109.5 . . ? O3 C34 Mn2 177.2(10) . 2_655 ? O3 C34 Mn2 173.9(9) . . ? Mn2 C34 Mn2 8.3(4) 2_655 . ? O4 C35 Mn2 174.6(8) . 2_655 ? O4 C35 Mn2 173.1(7) . . ? Mn2 C35 Mn2 11.7(4) 2_655 . ? N2 C36 Mn2 172.43(9) . . ? N2 C36 Mn2 172.43(9) . 2_655 ? Mn2 C36 Mn2 15.13(19) . 2_655 ? N3 C37 Mn2 172.53(9) . 2_655 ? N3 C37 Mn2 172.53(9) . . ? Mn2 C37 Mn2 14.95(18) 2_655 . ? C39 C38 C39 123.6(7) . 2_655 ? C39 C38 N2 118.2(4) . . ? C39 C38 N2 118.2(4) 2_655 . ? C38 C39 C40 117.1(5) . . ? C38 C39 C42 122.6(5) . . ? C40 C39 C42 120.3(5) . . ? C41 C40 C39 120.7(6) . . ? C41 C40 H40 119.7 . . ? C39 C40 H40 119.7 . . ? C40 C41 C40 120.9(8) 2_655 . ? C40 C41 H41 119.5 2_655 . ? C40 C41 H41 119.5 . . ? C47 C42 C43 120.3(5) . . ? C47 C42 C39 119.7(5) . . ? C43 C42 C39 120.0(5) . . ? C44 C43 C42 120.1(6) . . ? C44 C43 C48 119.0(6) . . ? C42 C43 C48 120.9(5) . . ? C43 C44 C45 120.4(6) . . ? C43 C44 H44 119.8 . . ? C45 C44 H44 119.8 . . ? C46 C45 C44 120.0(6) . . ? C46 C45 H45 120.0 . . ? C44 C45 H45 120.0 . . ? C45 C46 C47 121.0(6) . . ? C45 C46 H46 119.5 . . ? C47 C46 H46 119.5 . . ? C42 C47 C46 118.2(6) . . ? C42 C47 C51 121.4(5) . . ? C46 C47 C51 120.4(6) . . ? C43 C48 C49 112.9(5) . . ? C43 C48 C50 111.9(5) . . ? C49 C48 C50 109.7(5) . . ? C43 C48 H48 107.3 . . ? C49 C48 H48 107.3 . . ? C50 C48 H48 107.3 . . ? C48 C49 H49A 109.5 . . ? C48 C49 H49C 109.5 . . ? H49A C49 H49C 109.5 . . ? C48 C49 H49B 109.5 . . ? H49A C49 H49B 109.5 . . ? H49C C49 H49B 109.5 . . ? C48 C50 H50C 109.5 . . ? C48 C50 H50B 109.5 . . ? H50C C50 H50B 109.5 . . ? C48 C50 H50A 109.5 . . ? H50C C50 H50A 109.5 . . ? H50B C50 H50A 109.5 . . ? C53 C51 C52 110.2(6) . . ? C53 C51 C47 112.1(6) . . ? C52 C51 C47 113.1(6) . . ? C53 C51 H51 107.0 . . ? C52 C51 H51 107.0 . . ? C47 C51 H51 107.0 . . ? C51 C52 H52C 109.5 . . ? C51 C52 H52A 109.5 . . ? H52C C52 H52A 109.5 . . ? C51 C52 H52B 109.5 . . ? H52C C52 H52B 109.5 . . ? H52A C52 H52B 109.5 . . ? C51 C53 H53C 109.5 . . ? C51 C53 H53A 109.5 . . ? H53C C53 H53A 109.5 . . ? C51 C53 H53B 109.5 . . ? H53C C53 H53B 109.5 . . ? H53A C53 H53B 109.5 . . ? N3 C54 C55 118.7(4) . 2_655 ? N3 C54 C55 118.7(4) . . ? C55 C54 C55 122.7(7) 2_655 . ? C54 C55 C56 117.9(6) . . ? C54 C55 C58 120.8(5) . . ? C56 C55 C58 121.3(5) . . ? C57 C56 C55 120.4(6) . . ? C57 C56 H56 119.8 . . ? C55 C56 H56 119.8 . . ? C56 C57 C56 120.7(8) . 2_655 ? C56 C57 H57 119.7 . . ? C56 C57 H57 119.7 2_655 . ? C63 C58 C59 121.3(6) . . ? C63 C58 C55 118.9(5) . . ? C59 C58 C55 119.8(5) . . ? C60 C59 C58 119.5(6) . . ? C60 C59 C64 119.4(6) . . ? C58 C59 C64 121.1(6) . . ? C59 C60 C61 119.9(6) . . ? C59 C60 H60 120.0 . . ? C61 C60 H60 120.0 . . ? C60 C61 C62 120.8(6) . . ? C60 C61 H61 119.6 . . ? C62 C61 H61 119.6 . . ? C61 C62 C63 121.2(6) . . ? C61 C62 H62 119.4 . . ? C63 C62 H62 119.4 . . ? C58 C63 C62 117.4(6) . . ? C58 C63 C67 122.7(6) . . ? C62 C63 C67 119.9(6) . . ? C66 C64 C59 113.9(6) . . ? C66 C64 C65 111.2(6) . . ? C59 C64 C65 109.9(6) . . ? C66 C64 H64 107.2 . . ? C59 C64 H64 107.2 . . ? C65 C64 H64 107.2 . . ? C64 C65 H65C 109.5 . . ? C64 C65 H65A 109.5 . . ? H65C C65 H65A 109.5 . . ? C64 C65 H65B 109.5 . . ? H65C C65 H65B 109.5 . . ? H65A C65 H65B 109.5 . . ? C64 C66 H66B 109.5 . . ? C64 C66 H66A 109.5 . . ? H66B C66 H66A 109.5 . . ? C64 C66 H66C 109.5 . . ? H66B C66 H66C 109.5 . . ? H66A C66 H66C 109.5 . . ? C63 C67 C69 111.0(6) . . ? C63 C67 C68 110.6(6) . . ? C69 C67 C68 110.8(6) . . ? C63 C67 H67 108.1 . . ? C69 C67 H67 108.1 . . ? C68 C67 H67 108.1 . . ? C67 C68 H68C 109.5 . . ? C67 C68 H68A 109.5 . . ? H68C C68 H68A 109.5 . . ? C67 C68 H68B 109.5 . . ? H68C C68 H68B 109.5 . . ? H68A C68 H68B 109.5 . . ? C67 C69 H69B 109.5 . . ? C67 C69 H69A 109.5 . . ? H69B C69 H69A 109.5 . . ? C67 C69 H69C 109.5 . . ? H69B C69 H69C 109.5 . . ? H69A C69 H69C 109.5 . . ? _diffrn_measured_fraction_theta_max 0.998 _diffrn_reflns_theta_full 25.00 _diffrn_measured_fraction_theta_full 0.998 _refine_diff_density_max 0.801 _refine_diff_density_min -0.460 _refine_diff_density_rms 0.075 #===END data_JFig339 _database_code_depnum_ccdc_archive 'CCDC 785486' #TrackingRef 'cif-full.cif' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common H3CMn(CO)3(CNArDipp2)2 _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C132 H154 Mn2 N4 O6' _chemical_formula_weight 2002.47 loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Mn Mn 0.3368 0.7283 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting Triclinic _symmetry_space_group_name_H-M P-1 loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, -y, -z' _cell_length_a 16.737(6) _cell_length_b 18.896(8) _cell_length_c 20.570(8) _cell_angle_alpha 114.849(5) _cell_angle_beta 90.031(5) _cell_angle_gamma 90.131(5) _cell_volume 5903(4) _cell_formula_units_Z 2 _cell_measurement_temperature 100(2) _cell_measurement_reflns_used 9960 _cell_measurement_theta_min 2.38 _cell_measurement_theta_max 25.53 _exptl_crystal_description Block _exptl_crystal_colour Yellow _exptl_crystal_size_max 0.27 _exptl_crystal_size_mid 0.21 _exptl_crystal_size_min 0.13 _exptl_crystal_density_meas 'not measured' _exptl_crystal_density_diffrn 1.127 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 2144 _exptl_absorpt_coefficient_mu 0.269 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.9310 _exptl_absorpt_correction_T_max 0.9659 _exptl_absorpt_process_details SADABS _exptl_special_details ; ? ; _diffrn_ambient_temperature 100(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'Bruker APEX CCD' _diffrn_measurement_method '\f and \w scans' _diffrn_reflns_number 60904 _diffrn_reflns_av_R_equivalents 0.0469 _diffrn_reflns_av_sigmaI/netI 0.0610 _diffrn_reflns_limit_h_min -12 _diffrn_reflns_limit_h_max 20 _diffrn_reflns_limit_k_min -23 _diffrn_reflns_limit_k_max 23 _diffrn_reflns_limit_l_min -25 _diffrn_reflns_limit_l_max 24 _diffrn_reflns_theta_min 1.09 _diffrn_reflns_theta_max 25.77 _reflns_number_total 21907 _reflns_number_gt 15555 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'Bruker APEX2' _computing_cell_refinement 'Bruker SAINT' _computing_data_reduction 'Bruker SAINT' _computing_structure_solution 'SHELXS-97 (Sheldrick, 2008)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 2008)' _computing_molecular_graphics 'Bruker SHELXTL' _computing_publication_material 'Bruker SHELXTL' _refine_special_details ; Refinement of F^2^ against ALL reflections. The weighted R-factor wR and goodness of fit S are based on F^2^, conventional R-factors R are based on F, with F set to zero for negative F^2^. The threshold expression of F^2^ > 2sigma(F^2^) is used only for calculating R-factors(gt) etc. and is not relevant to the choice of reflections for refinement. R-factors based on F^2^ are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger. ; _refine_ls_structure_factor_coef Fsqd _refine_ls_matrix_type full _refine_ls_weighting_scheme calc _refine_ls_weighting_details 'calc w=1/[\s^2^(Fo^2^)+(0.0613P)^2^+0.8136P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment constr _refine_ls_extinction_method none _refine_ls_number_reflns 21907 _refine_ls_number_parameters 1373 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0737 _refine_ls_R_factor_gt 0.0488 _refine_ls_wR_factor_ref 0.1297 _refine_ls_wR_factor_gt 0.1200 _refine_ls_goodness_of_fit_ref 1.038 _refine_ls_restrained_S_all 1.038 _refine_ls_shift/su_max 0.001 _refine_ls_shift/su_mean 0.000 loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_occupancy _atom_site_symmetry_multiplicity _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group Mn1 Mn 0.436883(19) 0.76011(2) 0.236934(19) 0.02317(9) Uani 1 1 d . . . O1 O 0.35395(12) 0.81194(13) 0.37793(11) 0.0547(6) Uani 1 1 d . . . O2 O 0.35587(11) 0.60953(11) 0.15432(11) 0.0477(5) Uani 1 1 d . . . O3 O 0.54033(12) 0.75130(14) 0.11562(13) 0.0634(7) Uani 1 1 d . . . N1 N 0.31621(10) 0.85002(10) 0.18848(9) 0.0191(4) Uani 1 1 d . . . N2 N 0.56573(10) 0.68001(10) 0.28773(10) 0.0212(4) Uani 1 1 d . . . C1 C 0.36164(12) 0.81647(13) 0.20781(12) 0.0215(5) Uani 1 1 d . . . C2 C 0.51644(13) 0.71058(13) 0.26824(12) 0.0229(5) Uani 1 1 d . . . C3 C 0.49865(15) 0.86941(15) 0.30108(15) 0.0387(7) Uani 1 1 d . . . H3A H 0.5205 0.8672 0.3444 0.058 Uiso 1 1 calc R . . H3B H 0.4609 0.9128 0.3146 0.058 Uiso 1 1 calc R . . H3C H 0.5423 0.8773 0.2730 0.058 Uiso 1 1 calc R . . C4 C 0.38308(15) 0.78893(15) 0.32306(15) 0.0341(6) Uani 1 1 d . . . C5 C 0.38622(14) 0.66687(16) 0.18575(15) 0.0328(6) Uani 1 1 d . . . C6 C 0.50096(15) 0.75323(16) 0.16149(15) 0.0355(6) Uani 1 1 d . . . C7 C 0.25819(12) 0.88423(12) 0.16143(11) 0.0182(5) Uani 1 1 d . . . C8 C 0.19171(12) 0.91943(12) 0.20393(11) 0.0182(4) Uani 1 1 d . . . C9 C 0.13363(12) 0.95079(13) 0.17478(12) 0.0217(5) Uani 1 1 d . . . H9 H 0.0878 0.9752 0.2023 0.026 Uiso 1 1 calc R . . C10 C 0.14205(12) 0.94675(13) 0.10633(12) 0.0201(5) Uani 1 1 d . . . H10A H 0.1016 0.9676 0.0870 0.024 Uiso 1 1 calc R . . C11 C 0.20923(12) 0.91238(12) 0.06565(12) 0.0186(5) Uani 1 1 d . . . H11A H 0.2143 0.9104 0.0189 0.022 Uiso 1 1 calc R . . C12 C 0.26929(11) 0.88081(12) 0.09233(11) 0.0165(4) Uani 1 1 d . . . C13 C 0.18402(12) 0.92404(13) 0.27849(12) 0.0205(5) Uani 1 1 d . . . C14 C 0.20401(12) 0.99374(13) 0.33745(12) 0.0226(5) Uani 1 1 d . . . C15 C 0.19699(13) 0.99639(14) 0.40612(12) 0.0261(5) Uani 1 1 d . . . H15A H 0.2101 1.0430 0.4467 0.031 Uiso 1 1 calc R . . C16 C 0.17118(13) 0.93184(15) 0.41566(13) 0.0304(6) Uani 1 1 d . . . H16A H 0.1671 0.9344 0.4627 0.037 Uiso 1 1 calc R . . C17 C 0.15143(13) 0.86419(15) 0.35785(13) 0.0284(5) Uani 1 1 d . . . H17A H 0.1335 0.8205 0.3654 0.034 Uiso 1 1 calc R . . C18 C 0.15729(12) 0.85838(13) 0.28805(12) 0.0232(5) Uani 1 1 d . . . C19 C 0.23444(13) 1.06434(13) 0.32722(13) 0.0263(5) Uani 1 1 d . . . H19A H 0.2071 1.0647 0.2841 0.032 Uiso 1 1 calc R . . C20 C 0.21699(15) 1.14278(15) 0.39090(14) 0.0365(6) Uani 1 1 d . . . H20D H 0.1603 1.1452 0.4036 0.055 Uiso 1 1 calc R . . H20F H 0.2298 1.1856 0.3776 0.055 Uiso 1 1 calc R . . H20E H 0.2497 1.1475 0.4321 0.055 Uiso 1 1 calc R . . C21 C 0.32459(13) 1.05643(15) 0.31190(13) 0.0313(6) Uani 1 1 d . . . H21E H 0.3529 1.0553 0.3531 0.047 Uiso 1 1 calc R . . H21F H 0.3434 1.1009 0.3034 0.047 Uiso 1 1 calc R . . H21D H 0.3349 1.0080 0.2694 0.047 Uiso 1 1 calc R . . C22 C 0.13072(14) 0.78409(14) 0.22591(13) 0.0296(5) Uani 1 1 d . . . H22A H 0.1495 0.7864 0.1807 0.035 Uiso 1 1 calc R . . C23 C 0.03929(15) 0.77878(16) 0.22304(16) 0.0435(7) Uani 1 1 d . . . H23D H 0.0228 0.7312 0.1819 0.065 Uiso 1 1 calc R . . H23F H 0.0174 0.8244 0.2182 0.065 Uiso 1 1 calc R . . H23E H 0.0192 0.7773 0.2672 0.065 Uiso 1 1 calc R . . C24 C 0.16582(16) 0.71049(15) 0.22850(16) 0.0421(7) Uani 1 1 d . . . H24E H 0.1443 0.7042 0.2700 0.063 Uiso 1 1 calc R . . H24F H 0.2241 0.7153 0.2325 0.063 Uiso 1 1 calc R . . H24D H 0.1515 0.6649 0.1846 0.063 Uiso 1 1 calc R . . C25 C 0.34292(12) 0.84489(12) 0.04904(11) 0.0175(4) Uani 1 1 d . . . C26 C 0.41442(12) 0.88853(13) 0.06258(12) 0.0201(5) Uani 1 1 d . . . C27 C 0.48092(12) 0.85393(13) 0.02040(12) 0.0237(5) Uani 1 1 d . . . H27A H 0.5293 0.8827 0.0285 0.028 Uiso 1 1 calc R . . C28 C 0.47807(13) 0.77925(14) -0.03248(13) 0.0268(5) Uani 1 1 d . . . H28A H 0.5244 0.7567 -0.0601 0.032 Uiso 1 1 calc R . . C29 C 0.40781(13) 0.73683(14) -0.04554(12) 0.0247(5) Uani 1 1 d . . . H29A H 0.4063 0.6852 -0.0822 0.030 Uiso 1 1 calc R . . C30 C 0.33922(12) 0.76871(13) -0.00561(12) 0.0205(5) Uani 1 1 d . . . C31 C 0.42131(12) 0.97099(13) 0.12159(12) 0.0216(5) Uani 1 1 d . . . H31A H 0.3678 0.9865 0.1447 0.026 Uiso 1 1 calc R . . C32 C 0.44553(15) 1.02979(14) 0.09203(13) 0.0304(6) Uani 1 1 d . . . H32E H 0.4989 1.0169 0.0707 0.046 Uiso 1 1 calc R . . H32F H 0.4462 1.0824 0.1310 0.046 Uiso 1 1 calc R . . H32D H 0.4070 1.0278 0.0554 0.046 Uiso 1 1 calc R . . C33 C 0.48094(13) 0.97369(14) 0.17883(13) 0.0281(5) Uani 1 1 d . . . H33D H 0.4645 0.9366 0.1983 0.042 Uiso 1 1 calc R . . H33F H 0.4825 1.0265 0.2175 0.042 Uiso 1 1 calc R . . H33E H 0.5342 0.9597 0.1575 0.042 Uiso 1 1 calc R . . C34 C 0.26278(13) 0.72024(13) -0.01907(12) 0.0237(5) Uani 1 1 d . . . H34A H 0.2167 0.7572 -0.0046 0.028 Uiso 1 1 calc R . . C35 C 0.25092(15) 0.66450(14) -0.09762(13) 0.0329(6) Uani 1 1 d . . . H35E H 0.2913 0.6233 -0.1117 0.049 Uiso 1 1 calc R . . H35F H 0.2563 0.6933 -0.1274 0.049 Uiso 1 1 calc R . . H35D H 0.1975 0.6411 -0.1042 0.049 Uiso 1 1 calc R . . C36 C 0.26169(15) 0.67578(14) 0.02851(13) 0.0326(6) Uani 1 1 d . . . H36D H 0.2116 0.6464 0.0209 0.049 Uiso 1 1 calc R . . H36F H 0.2658 0.7129 0.0789 0.049 Uiso 1 1 calc R . . H36E H 0.3069 0.6397 0.0161 0.049 Uiso 1 1 calc R . . C37 C 0.62032(12) 0.63778(13) 0.30934(12) 0.0213(5) Uani 1 1 d . . . C38 C 0.65876(12) 0.67625(13) 0.37544(12) 0.0206(5) Uani 1 1 d . . . C39 C 0.71243(13) 0.63300(13) 0.39621(13) 0.0252(5) Uani 1 1 d . . . H39A H 0.7399 0.6575 0.4406 0.030 Uiso 1 1 calc R . . C40 C 0.72633(14) 0.55454(14) 0.35288(13) 0.0310(6) Uani 1 1 d . . . H40A H 0.7620 0.5256 0.3683 0.037 Uiso 1 1 calc R . . C41 C 0.68805(15) 0.51869(15) 0.28726(14) 0.0332(6) Uani 1 1 d . . . H41A H 0.6985 0.4653 0.2578 0.040 Uiso 1 1 calc R . . C42 C 0.63443(14) 0.55945(14) 0.26359(13) 0.0280(5) Uani 1 1 d . . . C43 C 0.64317(12) 0.76088(13) 0.41903(12) 0.0219(5) Uani 1 1 d . . . C44 C 0.68474(13) 0.81633(13) 0.40305(13) 0.0247(5) Uani 1 1 d . . . C45 C 0.66781(14) 0.89483(14) 0.44274(14) 0.0328(6) Uani 1 1 d . . . H45A H 0.6961 0.9331 0.4332 0.039 Uiso 1 1 calc R . . C46 C 0.60998(15) 0.91828(15) 0.49633(14) 0.0357(6) Uani 1 1 d . . . H46A H 0.5988 0.9722 0.5227 0.043 Uiso 1 1 calc R . . C47 C 0.56903(14) 0.86349(14) 0.51113(13) 0.0313(6) Uani 1 1 d . . . H47A H 0.5295 0.8801 0.5476 0.038 Uiso 1 1 calc R . . C48 C 0.58457(13) 0.78436(13) 0.47364(12) 0.0245(5) Uani 1 1 d . . . C49 C 0.74890(13) 0.79153(15) 0.34553(14) 0.0323(6) Uani 1 1 d . . . H49A H 0.7362 0.7372 0.3101 0.039 Uiso 1 1 calc R . . C50 C 0.83049(14) 0.78968(17) 0.37931(17) 0.0437(7) Uani 1 1 d . . . H50F H 0.8431 0.8417 0.4163 0.066 Uiso 1 1 calc R . . H50E H 0.8718 0.7738 0.3422 0.066 Uiso 1 1 calc R . . H50D H 0.8285 0.7524 0.4010 0.066 Uiso 1 1 calc R . . C51 C 0.75258(18) 0.8428(2) 0.30489(19) 0.0572(9) Uani 1 1 d . . . H51D H 0.6997 0.8448 0.2853 0.086 Uiso 1 1 calc R . . H51E H 0.7911 0.8210 0.2656 0.086 Uiso 1 1 calc R . . H51F H 0.7693 0.8956 0.3376 0.086 Uiso 1 1 calc R . . C52 C 0.54202(13) 0.72462(14) 0.49267(13) 0.0285(5) Uani 1 1 d . . . H52A H 0.5458 0.6731 0.4502 0.034 Uiso 1 1 calc R . . C53 C 0.58451(16) 0.71678(18) 0.55513(16) 0.0449(7) Uani 1 1 d . . . H53F H 0.5818 0.7665 0.5977 0.067 Uiso 1 1 calc R . . H53E H 0.6406 0.7029 0.5426 0.067 Uiso 1 1 calc R . . H53D H 0.5584 0.6759 0.5651 0.067 Uiso 1 1 calc R . . C54 C 0.45339(15) 0.74240(18) 0.50906(17) 0.0474(7) Uani 1 1 d . . . H54D H 0.4278 0.6990 0.5154 0.071 Uiso 1 1 calc R . . H54E H 0.4278 0.7493 0.4692 0.071 Uiso 1 1 calc R . . H54F H 0.4477 0.7903 0.5531 0.071 Uiso 1 1 calc R . . C55 C 0.59433(16) 0.52228(14) 0.19193(13) 0.0338(6) Uani 1 1 d . . . C56 C 0.6275(2) 0.53294(15) 0.13314(15) 0.0477(8) Uani 1 1 d . A . C57 C 0.5894(3) 0.49578(19) 0.06743(16) 0.0608(10) Uani 1 1 d . . . H57A H 0.6110 0.5011 0.0270 0.073 Uiso 1 1 calc R . . C58 C 0.5221(2) 0.4520(2) 0.05877(17) 0.0659(11) Uani 1 1 d . . . H58A H 0.4979 0.4271 0.0128 0.079 Uiso 1 1 calc R . . C59 C 0.48877(18) 0.44374(17) 0.11696(16) 0.0516(8) Uani 1 1 d . . . H59A H 0.4410 0.4143 0.1109 0.062 Uiso 1 1 calc R . . C60 C 0.52481(16) 0.47834(15) 0.18449(14) 0.0384(7) Uani 1 1 d . . . C61 C 0.7016(3) 0.58237(17) 0.14108(16) 0.0668(11) Uani 1 1 d . . . H61C H 0.6977 0.6287 0.1883 0.080 Uiso 0.494(6) 1 calc PR A 2 H61B H 0.7226 0.5910 0.1894 0.080 Uiso 0.506(6) 1 d PR A 1 C62 C 0.7795(3) 0.5378(3) 0.0852(3) 0.0336(15) Uani 0.506(6) 1 d P A 1 H62D H 0.7903 0.4875 0.0865 0.050 Uiso 0.506(6) 1 calc PR A 1 H62F H 0.8271 0.5709 0.1008 0.050 Uiso 0.506(6) 1 calc PR A 1 H62E H 0.7657 0.5294 0.0362 0.050 Uiso 0.506(6) 1 calc PR A 1 C62A C 0.7634(3) 0.5465(4) 0.1424(4) 0.048(2) Uani 0.494(6) 1 d P A 2 H62H H 0.7604 0.5309 0.1821 0.072 Uiso 0.494(6) 1 calc PR A 2 H62I H 0.8099 0.5805 0.1490 0.072 Uiso 0.494(6) 1 calc PR A 2 H62G H 0.7685 0.5000 0.0970 0.072 Uiso 0.494(6) 1 calc PR A 2 C63 C 0.7005(3) 0.6609(3) 0.1439(3) 0.0366(16) Uani 0.506(6) 1 d P A 1 H63E H 0.6820 0.6585 0.0978 0.055 Uiso 0.506(6) 1 calc PR A 1 H63F H 0.7545 0.6831 0.1538 0.055 Uiso 0.506(6) 1 calc PR A 1 H63D H 0.6642 0.6938 0.1819 0.055 Uiso 0.506(6) 1 calc PR A 1 C63A C 0.6858(4) 0.6124(4) 0.0793(4) 0.053(2) Uani 0.494(6) 1 d P A 2 H63H H 0.6983 0.5705 0.0324 0.079 Uiso 0.494(6) 1 calc PR A 2 H63I H 0.7200 0.6576 0.0878 0.079 Uiso 0.494(6) 1 calc PR A 2 H63G H 0.6296 0.6273 0.0804 0.079 Uiso 0.494(6) 1 calc PR A 2 C64 C 0.48748(15) 0.46941(15) 0.24833(15) 0.0379(6) Uani 1 1 d . . . H64A H 0.5309 0.4767 0.2840 0.045 Uiso 1 1 calc R . . C65 C 0.44955(19) 0.38953(16) 0.22949(18) 0.0570(9) Uani 1 1 d . . . H65E H 0.4330 0.3856 0.2735 0.086 Uiso 1 1 calc R . . H65F H 0.4885 0.3486 0.2040 0.086 Uiso 1 1 calc R . . H65D H 0.4028 0.3832 0.1988 0.086 Uiso 1 1 calc R . . C66 C 0.42450(16) 0.53303(16) 0.28472(18) 0.0471(8) Uani 1 1 d . . . H66D H 0.3806 0.5267 0.2512 0.071 Uiso 1 1 calc R . . H66F H 0.4490 0.5845 0.2988 0.071 Uiso 1 1 calc R . . H66E H 0.4038 0.5284 0.3273 0.071 Uiso 1 1 calc R . . Mn1' Mn 0.063106(19) 0.76010(2) 0.736919(19) 0.02333(9) Uani 1 1 d . . . O1' O -0.04047(12) 0.75150(14) 0.61590(13) 0.0632(6) Uani 1 1 d . . . O2' O 0.14386(11) 0.60968(11) 0.65434(11) 0.0481(5) Uani 1 1 d . . . O3' O 0.14603(12) 0.81168(13) 0.87792(11) 0.0548(6) Uani 1 1 d . . . N1' N 0.18390(10) 0.85011(10) 0.68852(9) 0.0187(4) Uani 1 1 d . . . N2' N -0.06563(10) 0.67980(10) 0.78772(10) 0.0219(4) Uani 1 1 d . . . C0AA C -0.1861(4) 0.6130(4) 0.5796(4) 0.0433(18) Uani 0.476(6) 1 d P B 2 H0AB H -0.1315 0.6333 0.5841 0.065 Uiso 0.476(6) 1 calc PR B 2 H0AC H -0.2241 0.6545 0.5851 0.065 Uiso 0.476(6) 1 calc PR B 2 H0AA H -0.1931 0.5696 0.5323 0.065 Uiso 0.476(6) 1 calc PR B 2 C1' C 0.13829(12) 0.81645(13) 0.70794(12) 0.0209(5) Uani 1 1 d . . . C2' C -0.01644(13) 0.71046(13) 0.76819(12) 0.0232(5) Uani 1 1 d . . . C3' C 0.00118(15) 0.86907(15) 0.80084(15) 0.0381(7) Uani 1 1 d . . . H3'A H -0.0434 0.8759 0.7731 0.057 Uiso 1 1 calc R . . H3'C H 0.0385 0.9129 0.8134 0.057 Uiso 1 1 calc R . . H3'B H -0.0194 0.8673 0.8447 0.057 Uiso 1 1 calc R . . C4' C -0.00075(15) 0.75326(16) 0.66121(15) 0.0351(6) Uani 1 1 d . . . C5' C 0.11374(14) 0.66705(16) 0.68561(15) 0.0323(6) Uani 1 1 d . . . C6 C -0.2640(3) 0.5464(4) 0.6422(4) 0.0441(19) Uani 0.476(6) 1 d P B 2 H6A H -0.2689 0.4998 0.5970 0.066 Uiso 0.476(6) 1 calc PR B 2 H6C H -0.3105 0.5801 0.6484 0.066 Uiso 0.476(6) 1 calc PR B 2 H6B H -0.2613 0.5310 0.6821 0.066 Uiso 0.476(6) 1 calc PR B 2 C6' C 0.11683(14) 0.78878(15) 0.82302(15) 0.0339(6) Uani 1 1 d . . . C7' C 0.24189(11) 0.88405(12) 0.66118(11) 0.0167(4) Uani 1 1 d . . . C8' C 0.23058(12) 0.88071(12) 0.59243(11) 0.0170(4) Uani 1 1 d . . . C9' C 0.29088(12) 0.91239(12) 0.56566(12) 0.0185(5) Uani 1 1 d . . . H9' H 0.2858 0.9103 0.5189 0.022 Uiso 1 1 calc R . . C10' C 0.35799(12) 0.94686(12) 0.60646(12) 0.0197(5) Uani 1 1 d . . . H10 H 0.3985 0.9679 0.5873 0.024 Uiso 1 1 calc R . . C11' C 0.36628(12) 0.95082(13) 0.67490(12) 0.0204(5) Uani 1 1 d . . . H11 H 0.4121 0.9753 0.7025 0.024 Uiso 1 1 calc R . . C12' C 0.30841(12) 0.91941(12) 0.70395(11) 0.0188(5) Uani 1 1 d . . . C13' C 0.15744(12) 0.84497(12) 0.54933(11) 0.0168(4) Uani 1 1 d . . . C14' C 0.08560(12) 0.88828(12) 0.56235(11) 0.0185(5) Uani 1 1 d . . . C15' C 0.01887(12) 0.85388(13) 0.52033(12) 0.0236(5) Uani 1 1 d . . . H15 H -0.0295 0.8825 0.5283 0.028 Uiso 1 1 calc R . . C16' C 0.02186(13) 0.77925(14) 0.46753(13) 0.0265(5) Uani 1 1 d . . . H16 H -0.0244 0.7565 0.4398 0.032 Uiso 1 1 calc R . . C17' C 0.09255(13) 0.73668(13) 0.45447(12) 0.0246(5) Uani 1 1 d . . . H17 H 0.0939 0.6850 0.4179 0.030 Uiso 1 1 calc R . . C18' C 0.16090(12) 0.76870(13) 0.49423(12) 0.0201(5) Uani 1 1 d . . . C19' C 0.07886(12) 0.97062(13) 0.62129(12) 0.0218(5) Uani 1 1 d . . . H19 H 0.1326 0.9864 0.6443 0.026 Uiso 1 1 calc R . . C20' C 0.05386(15) 1.02976(14) 0.59204(13) 0.0310(6) Uani 1 1 d . . . H20B H 0.0921 1.0284 0.5555 0.046 Uiso 1 1 calc R . . H20C H 0.0531 1.0822 0.6312 0.046 Uiso 1 1 calc R . . H20A H 0.0004 1.0165 0.5708 0.046 Uiso 1 1 calc R . . C21' C 0.01935(13) 0.97387(14) 0.67924(13) 0.0274(5) Uani 1 1 d . . . H21A H -0.0341 0.9599 0.6582 0.041 Uiso 1 1 calc R . . H21C H 0.0184 1.0268 0.7177 0.041 Uiso 1 1 calc R . . H21B H 0.0358 0.9370 0.6988 0.041 Uiso 1 1 calc R . . C22' C 0.23733(13) 0.72031(13) 0.48119(12) 0.0237(5) Uani 1 1 d . . . H22 H 0.2835 0.7574 0.4959 0.028 Uiso 1 1 calc R . . C23' C 0.24935(15) 0.66438(14) 0.40248(13) 0.0327(6) Uani 1 1 d . . . H23B H 0.3025 0.6409 0.3963 0.049 Uiso 1 1 calc R . . H23C H 0.2446 0.6932 0.3726 0.049 Uiso 1 1 calc R . . H23A H 0.2086 0.6233 0.3881 0.049 Uiso 1 1 calc R . . C24' C 0.23835(14) 0.67575(15) 0.52833(14) 0.0325(6) Uani 1 1 d . . . H24A H 0.1927 0.6399 0.5161 0.049 Uiso 1 1 calc R . . H24C H 0.2349 0.7128 0.5788 0.049 Uiso 1 1 calc R . . H24B H 0.2881 0.6460 0.5203 0.049 Uiso 1 1 calc R . . C25' C 0.31588(12) 0.92418(13) 0.77842(12) 0.0203(5) Uani 1 1 d . . . C26' C 0.29629(12) 0.99405(13) 0.83765(12) 0.0222(5) Uani 1 1 d . . . C27' C 0.30296(13) 0.99627(15) 0.90598(12) 0.0274(5) Uani 1 1 d . . . H27 H 0.2896 1.0427 0.9465 0.033 Uiso 1 1 calc R . . C28' C 0.32877(13) 0.93194(15) 0.91571(13) 0.0298(6) Uani 1 1 d . . . H28 H 0.3328 0.9346 0.9628 0.036 Uiso 1 1 calc R . . C29' C 0.34862(13) 0.86393(15) 0.85771(13) 0.0284(5) Uani 1 1 d . . . H29 H 0.3664 0.8203 0.8653 0.034 Uiso 1 1 calc R . . C30' C 0.34297(13) 0.85832(14) 0.78783(12) 0.0245(5) Uani 1 1 d . . . C31' C 0.26550(13) 1.06451(13) 0.82731(13) 0.0265(5) Uani 1 1 d . . . H31 H 0.2928 1.0651 0.7843 0.032 Uiso 1 1 calc R . . C32' C 0.28329(15) 1.14271(15) 0.89111(14) 0.0371(6) Uani 1 1 d . . . H32A H 0.2514 1.1467 0.9325 0.056 Uiso 1 1 calc R . . H32C H 0.2696 1.1857 0.8783 0.056 Uiso 1 1 calc R . . H32B H 0.3402 1.1456 0.9032 0.056 Uiso 1 1 calc R . . C33' C 0.17537(14) 1.05629(14) 0.81175(13) 0.0308(6) Uani 1 1 d . . . H33A H 0.1649 1.0077 0.7693 0.046 Uiso 1 1 calc R . . H33C H 0.1567 1.1006 0.8030 0.046 Uiso 1 1 calc R . . H33B H 0.1470 1.0553 0.8530 0.046 Uiso 1 1 calc R . . C34' C 0.36937(14) 0.78368(14) 0.72567(13) 0.0294(5) Uani 1 1 d . . . H34 H 0.3506 0.7858 0.6804 0.035 Uiso 1 1 calc R . . C35' C 0.46079(15) 0.77874(17) 0.72286(17) 0.0455(7) Uani 1 1 d . . . H35C H 0.4810 0.7782 0.7674 0.068 Uiso 1 1 calc R . . H35B H 0.4827 0.8240 0.7173 0.068 Uiso 1 1 calc R . . H35A H 0.4771 0.7308 0.6821 0.068 Uiso 1 1 calc R . . C36' C 0.33414(16) 0.71057(15) 0.72829(16) 0.0414(7) Uani 1 1 d . . . H36A H 0.3476 0.6651 0.6841 0.062 Uiso 1 1 calc R . . H36B H 0.2759 0.7157 0.7329 0.062 Uiso 1 1 calc R . . H36C H 0.3562 0.7039 0.7695 0.062 Uiso 1 1 calc R . . C37' C -0.12029(12) 0.63759(13) 0.80915(12) 0.0218(5) Uani 1 1 d . . . C38' C -0.15891(12) 0.67648(13) 0.87553(12) 0.0213(5) Uani 1 1 d . . . C39' C -0.21244(13) 0.63279(14) 0.89621(13) 0.0258(5) Uani 1 1 d . . . H39 H -0.2398 0.6571 0.9406 0.031 Uiso 1 1 calc R . . C40' C -0.22612(14) 0.55472(15) 0.85295(13) 0.0316(6) Uani 1 1 d . . . H40 H -0.2618 0.5257 0.8684 0.038 Uiso 1 1 calc R . . C41' C -0.18810(15) 0.51851(14) 0.78712(14) 0.0337(6) Uani 1 1 d . . . H41 H -0.1987 0.4651 0.7577 0.040 Uiso 1 1 calc R . . C42' C -0.13435(14) 0.55962(14) 0.76360(13) 0.0278(5) Uani 1 1 d . . . C43' C -0.14307(12) 0.76108(13) 0.91905(12) 0.0224(5) Uani 1 1 d . . . C44' C -0.18501(13) 0.81626(14) 0.90324(13) 0.0256(5) Uani 1 1 d . . . C45' C -0.16758(14) 0.89479(14) 0.94310(14) 0.0326(6) Uani 1 1 d . . . H45 H -0.1958 0.9329 0.9335 0.039 Uiso 1 1 calc R . . C46' C -0.10991(15) 0.91858(15) 0.99641(14) 0.0353(6) Uani 1 1 d . . . H46 H -0.0986 0.9725 1.0228 0.042 Uiso 1 1 calc R . . C47' C -0.06898(14) 0.86361(14) 1.01103(13) 0.0314(6) Uani 1 1 d . . . H47 H -0.0293 0.8802 1.0474 0.038 Uiso 1 1 calc R . . C48' C -0.08479(12) 0.78413(13) 0.97339(12) 0.0241(5) Uani 1 1 d . . . C49' C -0.24914(14) 0.79165(15) 0.84577(14) 0.0321(6) Uani 1 1 d . . . H49 H -0.2368 0.7372 0.8105 0.039 Uiso 1 1 calc R . . C50' C -0.33060(14) 0.78994(17) 0.87955(17) 0.0444(7) Uani 1 1 d . . . H50C H -0.3423 0.8418 0.9172 0.067 Uiso 1 1 calc R . . H50B H -0.3291 0.7519 0.9004 0.067 Uiso 1 1 calc R . . H50A H -0.3722 0.7751 0.8426 0.067 Uiso 1 1 calc R . . C51' C -0.25288(17) 0.8428(2) 0.80455(19) 0.0566(9) Uani 1 1 d . . . H51C H -0.2694 0.8956 0.8370 0.085 Uiso 1 1 calc R . . H51A H -0.2916 0.8207 0.7653 0.085 Uiso 1 1 calc R . . H51B H -0.2000 0.8448 0.7849 0.085 Uiso 1 1 calc R . . C52' C -0.04178(13) 0.72447(15) 0.99255(14) 0.0298(6) Uani 1 1 d . . . H52 H -0.0458 0.6729 0.9502 0.036 Uiso 1 1 calc R . . C53' C -0.08436(16) 0.71665(18) 1.05515(16) 0.0451(7) Uani 1 1 d . . . H53C H -0.0835 0.7670 1.0971 0.068 Uiso 1 1 calc R . . H53B H -0.0570 0.6776 1.0667 0.068 Uiso 1 1 calc R . . H53A H -0.1398 0.7004 1.0417 0.068 Uiso 1 1 calc R . . C54' C 0.04663(15) 0.74217(18) 1.00899(18) 0.0484(8) Uani 1 1 d . . . H54A H 0.0720 0.7503 0.9697 0.073 Uiso 1 1 calc R . . H54B H 0.0722 0.6982 1.0142 0.073 Uiso 1 1 calc R . . H54C H 0.0526 0.7894 1.0536 0.073 Uiso 1 1 calc R . . C55' C -0.09438(16) 0.52213(14) 0.69188(13) 0.0333(6) Uani 1 1 d . . . C56' C -0.1274(2) 0.53291(15) 0.63335(15) 0.0467(8) Uani 1 1 d . B . C57' C -0.0902(3) 0.49567(18) 0.56690(16) 0.0609(10) Uani 1 1 d . . . H57 H -0.1123 0.5005 0.5264 0.073 Uiso 1 1 calc R . . C58' C -0.0223(2) 0.4522(2) 0.55877(16) 0.0645(11) Uani 1 1 d . . . H58 H 0.0019 0.4276 0.5129 0.077 Uiso 1 1 calc R . . C59' C 0.01135(18) 0.44380(16) 0.61652(16) 0.0512(9) Uani 1 1 d . . . H59 H 0.0591 0.4145 0.6102 0.061 Uiso 1 1 calc R . . C60' C -0.02466(16) 0.47834(15) 0.68469(14) 0.0379(7) Uani 1 1 d . . . C61' C -0.2021(3) 0.58249(17) 0.64128(16) 0.0663(11) Uani 1 1 d . . . H61 H -0.2230 0.5912 0.6896 0.080 Uiso 0.524(6) 1 calc PR B 1 H61A H -0.1982 0.6288 0.6886 0.080 Uiso 0.476(6) 1 d PR B 2 C62' C -0.2800(3) 0.5377(3) 0.5854(3) 0.0389(15) Uani 0.524(6) 1 d P B 1 H62A H -0.2670 0.5311 0.5367 0.058 Uiso 0.524(6) 1 calc PR B 1 H62C H -0.3280 0.5698 0.6020 0.058 Uiso 0.524(6) 1 calc PR B 1 H62B H -0.2896 0.4865 0.5854 0.058 Uiso 0.524(6) 1 calc PR B 1 C63' C -0.2008(3) 0.6612(3) 0.6436(3) 0.0394(15) Uani 0.524(6) 1 d P B 1 H63C H -0.1637 0.6941 0.6810 0.059 Uiso 0.524(6) 1 calc PR B 1 H63B H -0.2545 0.6836 0.6541 0.059 Uiso 0.524(6) 1 calc PR B 1 H63A H -0.1832 0.6584 0.5971 0.059 Uiso 0.524(6) 1 calc PR B 1 C64' C 0.01274(15) 0.46924(15) 0.74812(14) 0.0374(6) Uani 1 1 d . . . H64 H -0.0306 0.4764 0.7837 0.045 Uiso 1 1 calc R . . C65' C 0.0502(2) 0.38934(17) 0.72928(18) 0.0588(9) Uani 1 1 d . . . H65A H 0.0114 0.3484 0.7028 0.088 Uiso 1 1 calc R . . H65C H 0.0657 0.3849 0.7734 0.088 Uiso 1 1 calc R . . H65B H 0.0976 0.3835 0.6995 0.088 Uiso 1 1 calc R . . C66' C 0.07548(16) 0.53271(16) 0.78471(17) 0.0470(7) Uani 1 1 d . . . H66A H 0.1199 0.5261 0.7517 0.071 Uiso 1 1 calc R . . H66C H 0.0954 0.5286 0.8278 0.071 Uiso 1 1 calc R . . H66B H 0.0513 0.5841 0.7981 0.071 Uiso 1 1 calc R . . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 Mn1 0.02474(18) 0.0248(2) 0.0243(2) 0.01445(16) -0.00474(15) 0.00192(14) O1 0.0611(13) 0.0774(16) 0.0365(12) 0.0345(12) 0.0116(10) 0.0226(11) O2 0.0506(11) 0.0295(11) 0.0612(14) 0.0172(10) -0.0233(10) -0.0017(9) O3 0.0518(13) 0.0989(19) 0.0667(16) 0.0612(15) 0.0219(12) 0.0317(12) N1 0.0217(9) 0.0216(10) 0.0167(10) 0.0106(8) 0.0003(8) 0.0012(7) N2 0.0255(9) 0.0181(10) 0.0209(10) 0.0092(8) -0.0024(8) 0.0018(8) C1 0.0235(11) 0.0250(13) 0.0171(12) 0.0101(10) 0.0024(9) -0.0013(9) C2 0.0280(12) 0.0214(12) 0.0195(12) 0.0090(10) -0.0013(10) -0.0020(9) C3 0.0353(14) 0.0453(17) 0.0507(18) 0.0351(15) -0.0153(13) 0.0009(11) C4 0.0348(14) 0.0404(16) 0.0357(16) 0.0245(13) -0.0048(12) 0.0078(11) C5 0.0277(13) 0.0411(17) 0.0403(16) 0.0276(14) -0.0036(11) 0.0080(11) C6 0.0319(13) 0.0458(17) 0.0409(17) 0.0301(14) 0.0010(12) 0.0104(11) C7 0.0201(10) 0.0190(12) 0.0188(12) 0.0112(10) -0.0039(9) -0.0005(8) C8 0.0220(11) 0.0189(11) 0.0152(11) 0.0087(9) -0.0013(9) -0.0012(8) C9 0.0205(11) 0.0245(12) 0.0214(12) 0.0109(10) 0.0040(9) 0.0032(9) C10 0.0203(11) 0.0242(12) 0.0195(12) 0.0128(10) -0.0039(9) -0.0001(9) C11 0.0232(11) 0.0201(12) 0.0151(11) 0.0101(9) -0.0009(9) -0.0025(8) C12 0.0204(10) 0.0162(11) 0.0146(11) 0.0079(9) -0.0006(9) -0.0017(8) C13 0.0194(11) 0.0297(13) 0.0161(12) 0.0132(10) 0.0007(9) 0.0050(9) C14 0.0199(11) 0.0311(13) 0.0197(12) 0.0137(11) -0.0008(9) 0.0037(9) C15 0.0250(12) 0.0378(14) 0.0166(12) 0.0124(11) -0.0012(9) 0.0056(10) C16 0.0262(12) 0.0511(17) 0.0211(13) 0.0221(13) 0.0046(10) 0.0092(11) C17 0.0272(12) 0.0386(15) 0.0290(14) 0.0236(12) 0.0043(10) 0.0042(10) C18 0.0225(11) 0.0295(13) 0.0241(13) 0.0175(11) 0.0033(9) 0.0049(9) C19 0.0318(12) 0.0294(14) 0.0192(12) 0.0117(11) -0.0038(10) -0.0011(10) C20 0.0387(14) 0.0328(15) 0.0342(16) 0.0102(12) 0.0009(12) 0.0016(11) C21 0.0359(13) 0.0332(15) 0.0230(13) 0.0101(11) 0.0018(11) -0.0050(11) C22 0.0392(13) 0.0293(14) 0.0257(14) 0.0168(11) 0.0030(11) -0.0016(10) C23 0.0409(15) 0.0385(17) 0.0485(18) 0.0157(14) -0.0119(13) -0.0032(12) C24 0.0434(15) 0.0341(16) 0.0499(18) 0.0187(14) 0.0016(13) 0.0052(12) C25 0.0197(10) 0.0215(12) 0.0157(11) 0.0121(10) -0.0001(9) 0.0019(8) C26 0.0214(11) 0.0262(13) 0.0172(12) 0.0137(10) -0.0018(9) 0.0017(9) C27 0.0193(11) 0.0304(14) 0.0259(13) 0.0162(11) -0.0005(9) -0.0004(9) C28 0.0243(11) 0.0329(14) 0.0260(13) 0.0150(11) 0.0070(10) 0.0071(10) C29 0.0274(12) 0.0248(13) 0.0203(12) 0.0080(10) 0.0027(10) 0.0058(9) C30 0.0236(11) 0.0249(12) 0.0172(12) 0.0130(10) -0.0017(9) 0.0012(9) C31 0.0204(11) 0.0250(12) 0.0195(12) 0.0095(10) -0.0020(9) -0.0012(9) C32 0.0436(14) 0.0254(13) 0.0244(13) 0.0125(11) -0.0047(11) -0.0044(11) C33 0.0293(12) 0.0331(14) 0.0220(13) 0.0117(11) -0.0034(10) -0.0040(10) C34 0.0239(11) 0.0205(12) 0.0239(13) 0.0068(10) 0.0010(10) -0.0001(9) C35 0.0398(14) 0.0281(14) 0.0273(14) 0.0081(11) -0.0041(11) -0.0049(11) C36 0.0391(14) 0.0321(14) 0.0282(14) 0.0144(12) -0.0010(11) -0.0086(11) C37 0.0249(11) 0.0214(12) 0.0231(13) 0.0146(10) 0.0001(9) 0.0046(9) C38 0.0210(11) 0.0229(12) 0.0223(12) 0.0136(10) 0.0033(9) 0.0026(9) C39 0.0257(11) 0.0302(14) 0.0242(13) 0.0158(11) -0.0011(10) 0.0034(9) C40 0.0367(13) 0.0332(14) 0.0299(14) 0.0199(12) -0.0007(11) 0.0127(11) C41 0.0480(15) 0.0258(14) 0.0272(14) 0.0124(11) 0.0016(12) 0.0142(11) C42 0.0368(13) 0.0268(13) 0.0228(13) 0.0126(11) 0.0026(10) 0.0079(10) C43 0.0210(11) 0.0239(12) 0.0231(12) 0.0122(10) -0.0055(9) 0.0006(9) C44 0.0242(11) 0.0276(13) 0.0294(14) 0.0190(11) -0.0107(10) -0.0032(9) C45 0.0380(14) 0.0286(14) 0.0385(16) 0.0207(12) -0.0168(12) -0.0057(11) C46 0.0472(15) 0.0232(14) 0.0313(15) 0.0063(12) -0.0155(12) 0.0062(11) C47 0.0308(13) 0.0324(15) 0.0260(14) 0.0075(12) -0.0026(11) 0.0080(10) C48 0.0231(11) 0.0293(13) 0.0212(13) 0.0107(11) -0.0044(10) 0.0039(9) C49 0.0304(13) 0.0371(15) 0.0390(16) 0.0254(13) -0.0016(11) -0.0055(10) C50 0.0296(13) 0.0492(18) 0.063(2) 0.0336(16) -0.0003(13) 0.0013(12) C51 0.0477(17) 0.082(2) 0.071(2) 0.061(2) 0.0107(16) 0.0063(16) C52 0.0270(12) 0.0322(14) 0.0271(14) 0.0133(11) 0.0023(10) 0.0024(10) C53 0.0441(16) 0.061(2) 0.0428(18) 0.0349(16) 0.0018(13) -0.0013(13) C54 0.0315(14) 0.058(2) 0.059(2) 0.0311(17) 0.0063(14) 0.0023(13) C55 0.0537(16) 0.0211(13) 0.0240(14) 0.0070(11) -0.0073(12) 0.0149(11) C56 0.096(2) 0.0234(15) 0.0242(15) 0.0104(12) 0.0016(15) 0.0244(15) C57 0.115(3) 0.0430(19) 0.0239(17) 0.0129(15) -0.0061(18) 0.036(2) C58 0.099(3) 0.055(2) 0.0263(18) -0.0011(16) -0.0228(18) 0.044(2) C59 0.0560(18) 0.0426(18) 0.0369(18) -0.0024(14) -0.0174(15) 0.0265(14) C60 0.0482(16) 0.0310(15) 0.0279(15) 0.0045(12) -0.0095(12) 0.0207(12) C61 0.150(4) 0.0260(17) 0.0242(16) 0.0107(13) 0.0135(19) -0.014(2) C62 0.031(3) 0.031(3) 0.039(4) 0.015(3) 0.006(2) 0.006(2) C62A 0.039(3) 0.041(4) 0.073(6) 0.033(4) -0.008(3) -0.008(3) C63 0.040(3) 0.030(3) 0.044(4) 0.019(3) 0.007(3) 0.006(2) C63A 0.049(4) 0.072(5) 0.056(5) 0.045(4) 0.006(3) 0.002(3) C64 0.0343(14) 0.0350(15) 0.0357(16) 0.0063(13) -0.0081(12) 0.0074(11) C65 0.076(2) 0.0281(16) 0.057(2) 0.0083(15) -0.0146(17) 0.0076(14) C66 0.0412(15) 0.0303(16) 0.064(2) 0.0138(15) 0.0095(14) 0.0034(12) Mn1' 0.02440(18) 0.0250(2) 0.0249(2) 0.01475(16) 0.00466(15) -0.00075(14) O1' 0.0485(12) 0.0989(19) 0.0677(16) 0.0603(15) -0.0210(12) -0.0278(12) O2' 0.0506(11) 0.0303(11) 0.0609(14) 0.0166(10) 0.0241(10) 0.0022(9) O3' 0.0604(13) 0.0750(16) 0.0391(13) 0.0340(12) -0.0115(11) -0.0187(11) N1' 0.0229(9) 0.0205(10) 0.0154(10) 0.0102(8) -0.0012(7) -0.0020(7) N2' 0.0286(10) 0.0182(10) 0.0187(10) 0.0075(8) 0.0009(8) -0.0023(8) C0AA 0.047(3) 0.051(4) 0.046(4) 0.035(4) -0.005(3) -0.002(3) C1' 0.0240(11) 0.0228(12) 0.0163(12) 0.0086(10) -0.0013(9) 0.0023(9) C2' 0.0278(12) 0.0205(12) 0.0230(13) 0.0108(10) 0.0028(10) 0.0015(9) C3' 0.0391(14) 0.0405(16) 0.0491(18) 0.0328(14) 0.0183(13) 0.0044(11) C4' 0.0308(13) 0.0466(17) 0.0401(16) 0.0303(14) 0.0016(12) -0.0081(11) C5' 0.0269(12) 0.0376(16) 0.0423(16) 0.0266(14) 0.0059(12) -0.0037(11) C6 0.035(3) 0.039(4) 0.065(5) 0.028(4) 0.006(3) 0.005(3) C6' 0.0315(13) 0.0391(16) 0.0387(17) 0.0238(13) 0.0042(12) -0.0071(11) C7' 0.0186(10) 0.0175(11) 0.0165(11) 0.0097(9) 0.0027(9) 0.0013(8) C8' 0.0219(10) 0.0151(11) 0.0142(11) 0.0062(9) 0.0000(9) 0.0033(8) C9' 0.0222(11) 0.0205(12) 0.0160(11) 0.0107(10) 0.0005(9) 0.0026(8) C10' 0.0208(11) 0.0226(12) 0.0193(12) 0.0122(10) 0.0036(9) 0.0003(9) C11' 0.0189(10) 0.0247(12) 0.0199(12) 0.0117(10) -0.0007(9) -0.0002(9) C12' 0.0241(11) 0.0191(11) 0.0150(11) 0.0090(9) 0.0016(9) 0.0028(8) C13' 0.0214(10) 0.0209(12) 0.0134(11) 0.0124(9) -0.0012(9) -0.0024(8) C14' 0.0228(11) 0.0218(12) 0.0144(11) 0.0113(10) 0.0008(9) -0.0003(9) C15' 0.0197(11) 0.0303(13) 0.0253(13) 0.0161(11) -0.0016(9) 0.0003(9) C16' 0.0236(11) 0.0324(14) 0.0258(13) 0.0145(11) -0.0076(10) -0.0070(10) C17' 0.0301(12) 0.0231(13) 0.0196(12) 0.0079(10) -0.0036(10) -0.0039(9) C18' 0.0247(11) 0.0229(12) 0.0162(12) 0.0117(10) -0.0007(9) -0.0010(9) C19' 0.0215(11) 0.0254(13) 0.0194(12) 0.0101(10) 0.0011(9) 0.0024(9) C20' 0.0437(14) 0.0254(13) 0.0262(14) 0.0130(11) 0.0057(11) 0.0055(11) C21' 0.0272(12) 0.0339(14) 0.0224(13) 0.0131(11) 0.0048(10) 0.0051(10) C22' 0.0252(11) 0.0215(12) 0.0234(13) 0.0084(10) -0.0015(10) 0.0012(9) C23' 0.0390(14) 0.0294(14) 0.0265(14) 0.0086(11) 0.0027(11) 0.0053(11) C24' 0.0368(13) 0.0336(15) 0.0296(14) 0.0157(12) 0.0013(11) 0.0116(11) C25' 0.0194(10) 0.0289(13) 0.0162(12) 0.0130(10) -0.0018(9) -0.0039(9) C26' 0.0209(11) 0.0298(13) 0.0175(12) 0.0115(10) 0.0003(9) -0.0019(9) C27' 0.0272(12) 0.0376(15) 0.0161(12) 0.0102(11) 0.0024(10) -0.0035(10) C28' 0.0289(12) 0.0482(16) 0.0201(13) 0.0221(12) -0.0065(10) -0.0083(11) C29' 0.0286(12) 0.0376(15) 0.0289(14) 0.0237(12) -0.0033(10) -0.0012(10) C30' 0.0251(11) 0.0309(14) 0.0228(13) 0.0166(11) -0.0046(10) -0.0034(9) C31' 0.0318(12) 0.0290(14) 0.0200(13) 0.0114(11) 0.0026(10) 0.0028(10) C32' 0.0415(14) 0.0330(15) 0.0360(16) 0.0137(13) -0.0012(12) 0.0012(11) C33' 0.0390(14) 0.0294(14) 0.0212(13) 0.0078(11) -0.0028(11) 0.0054(11) C34' 0.0374(13) 0.0309(14) 0.0253(14) 0.0170(11) -0.0026(11) 0.0034(10) C35' 0.0432(16) 0.0409(17) 0.0512(19) 0.0181(15) 0.0132(14) 0.0056(12) C36' 0.0445(15) 0.0318(15) 0.0483(18) 0.0171(14) -0.0022(13) -0.0015(12) C37' 0.0251(11) 0.0206(12) 0.0245(13) 0.0142(10) -0.0003(10) -0.0037(9) C38' 0.0211(11) 0.0245(12) 0.0229(12) 0.0147(10) -0.0040(9) -0.0019(9) C39' 0.0272(12) 0.0302(14) 0.0224(13) 0.0135(11) 0.0009(10) -0.0036(10) C40' 0.0353(13) 0.0349(15) 0.0292(14) 0.0180(12) -0.0010(11) -0.0130(11) C41' 0.0519(15) 0.0229(13) 0.0259(14) 0.0100(11) -0.0024(12) -0.0142(11) C42' 0.0365(13) 0.0252(13) 0.0246(13) 0.0133(11) -0.0010(10) -0.0058(10) C43' 0.0225(11) 0.0251(13) 0.0219(12) 0.0121(10) 0.0068(9) -0.0003(9) C44' 0.0251(11) 0.0294(14) 0.0284(14) 0.0181(11) 0.0099(10) 0.0048(9) C45' 0.0390(14) 0.0273(14) 0.0378(16) 0.0200(12) 0.0168(12) 0.0088(11) C46' 0.0471(15) 0.0231(14) 0.0311(15) 0.0068(12) 0.0152(12) -0.0048(11) C47' 0.0304(13) 0.0337(15) 0.0256(14) 0.0080(12) 0.0031(11) -0.0062(10) C48' 0.0219(11) 0.0288(13) 0.0219(13) 0.0110(11) 0.0045(9) -0.0002(9) C49' 0.0305(13) 0.0387(15) 0.0366(15) 0.0251(13) 0.0004(11) 0.0071(11) C50' 0.0290(13) 0.0496(18) 0.065(2) 0.0348(16) -0.0001(13) 0.0017(12) C51' 0.0465(17) 0.081(2) 0.072(2) 0.061(2) -0.0070(16) -0.0018(15) C52' 0.0253(12) 0.0364(15) 0.0289(14) 0.0148(12) -0.0026(10) -0.0016(10) C53' 0.0457(16) 0.062(2) 0.0418(17) 0.0359(16) -0.0015(13) 0.0019(14) C54' 0.0315(14) 0.063(2) 0.062(2) 0.0365(17) -0.0069(14) -0.0004(13) C55' 0.0551(16) 0.0203(13) 0.0207(13) 0.0049(11) 0.0044(12) -0.0144(11) C56' 0.091(2) 0.0242(15) 0.0257(15) 0.0118(12) -0.0034(15) -0.0195(14) C57' 0.117(3) 0.0392(19) 0.0230(16) 0.0101(14) 0.0032(18) -0.035(2) C58' 0.099(3) 0.054(2) 0.0221(17) -0.0011(15) 0.0174(18) -0.044(2) C59' 0.0572(18) 0.0372(17) 0.0405(19) -0.0020(14) 0.0187(15) -0.0243(14) C60' 0.0479(16) 0.0291(15) 0.0264(14) 0.0016(12) 0.0096(12) -0.0202(12) C61' 0.148(4) 0.0268(17) 0.0241(16) 0.0110(14) -0.0162(19) 0.012(2) C62' 0.035(3) 0.042(3) 0.041(4) 0.019(3) -0.005(2) -0.005(2) C63' 0.044(3) 0.032(3) 0.042(4) 0.015(3) -0.009(3) -0.003(2) C64' 0.0343(14) 0.0347(15) 0.0347(16) 0.0063(13) 0.0089(12) -0.0047(11) C65' 0.078(2) 0.0297(17) 0.059(2) 0.0094(15) 0.0144(18) -0.0079(15) C66' 0.0430(16) 0.0310(16) 0.060(2) 0.0118(15) -0.0081(14) -0.0019(12) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag Mn1 C5 1.834(3) . ? Mn1 C6 1.846(3) . ? Mn1 C4 1.854(3) . ? Mn1 C2 1.891(2) . ? Mn1 C1 1.903(2) . ? Mn1 C3 2.185(3) . ? O1 C4 1.136(3) . ? O2 C5 1.122(3) . ? O3 C6 1.139(3) . ? N1 C1 1.163(3) . ? N1 C7 1.405(3) . ? N2 C2 1.171(3) . ? N2 C37 1.404(3) . ? C3 H3A 0.9800 . ? C3 H3B 0.9800 . ? C3 H3C 0.9800 . ? C7 C8 1.400(3) . ? C7 C12 1.408(3) . ? C8 C9 1.399(3) . ? C8 C13 1.505(3) . ? C9 C10 1.385(3) . ? C9 H9 0.9500 . ? C10 C11 1.391(3) . ? C10 H10A 0.9500 . ? C11 C12 1.395(3) . ? C11 H11A 0.9500 . ? C12 C25 1.506(3) . ? C13 C14 1.404(3) . ? C13 C18 1.407(3) . ? C14 C15 1.397(3) . ? C14 C19 1.522(3) . ? C15 C16 1.383(3) . ? C15 H15A 0.9500 . ? C16 C17 1.370(3) . ? C16 H16A 0.9500 . ? C17 C18 1.397(3) . ? C17 H17A 0.9500 . ? C18 C22 1.514(3) . ? C19 C21 1.536(3) . ? C19 C20 1.539(3) . ? C19 H19A 1.0000 . ? C20 H20D 0.9800 . ? C20 H20F 0.9800 . ? C20 H20E 0.9800 . ? C21 H21E 0.9800 . ? C21 H21F 0.9800 . ? C21 H21D 0.9800 . ? C22 C24 1.532(3) . ? C22 C23 1.533(3) . ? C22 H22A 1.0000 . ? C23 H23D 0.9800 . ? C23 H23F 0.9800 . ? C23 H23E 0.9800 . ? C24 H24E 0.9800 . ? C24 H24F 0.9800 . ? C24 H24D 0.9800 . ? C25 C30 1.407(3) . ? C25 C26 1.411(3) . ? C26 C27 1.395(3) . ? C26 C31 1.524(3) . ? C27 C28 1.374(3) . ? C27 H27A 0.9500 . ? C28 C29 1.383(3) . ? C28 H28A 0.9500 . ? C29 C30 1.394(3) . ? C29 H29A 0.9500 . ? C30 C34 1.528(3) . ? C31 C33 1.528(3) . ? C31 C32 1.528(3) . ? C31 H31A 1.0000 . ? C32 H32E 0.9800 . ? C32 H32F 0.9800 . ? C32 H32D 0.9800 . ? C33 H33D 0.9800 . ? C33 H33F 0.9800 . ? C33 H33E 0.9800 . ? C34 C35 1.526(3) . ? C34 C36 1.535(3) . ? C34 H34A 1.0000 . ? C35 H35E 0.9800 . ? C35 H35F 0.9800 . ? C35 H35D 0.9800 . ? C36 H36D 0.9800 . ? C36 H36F 0.9800 . ? C36 H36E 0.9800 . ? C37 C38 1.399(3) . ? C37 C42 1.401(3) . ? C38 C39 1.398(3) . ? C38 C43 1.492(3) . ? C39 C40 1.392(3) . ? C39 H39A 0.9500 . ? C40 C41 1.386(4) . ? C40 H40A 0.9500 . ? C41 C42 1.398(3) . ? C41 H41A 0.9500 . ? C42 C55 1.498(3) . ? C43 C44 1.406(3) . ? C43 C48 1.416(3) . ? C44 C45 1.390(3) . ? C44 C49 1.520(3) . ? C45 C46 1.393(4) . ? C45 H45A 0.9500 . ? C46 C47 1.377(4) . ? C46 H46A 0.9500 . ? C47 C48 1.390(3) . ? C47 H47A 0.9500 . ? C48 C52 1.517(3) . ? C49 C51 1.524(4) . ? C49 C50 1.539(3) . ? C49 H49A 1.0000 . ? C50 H50F 0.9800 . ? C50 H50E 0.9800 . ? C50 H50D 0.9800 . ? C51 H51D 0.9800 . ? C51 H51E 0.9800 . ? C51 H51F 0.9800 . ? C52 C53 1.529(4) . ? C52 C54 1.528(3) . ? C52 H52A 1.0000 . ? C53 H53F 0.9800 . ? C53 H53E 0.9800 . ? C53 H53D 0.9800 . ? C54 H54D 0.9800 . ? C54 H54E 0.9800 . ? C54 H54F 0.9800 . ? C55 C60 1.398(4) . ? C55 C56 1.420(4) . ? C56 C57 1.388(4) . ? C56 C61 1.517(5) . ? C57 C58 1.363(5) . ? C57 H57A 0.9500 . ? C58 C59 1.387(5) . ? C58 H58A 0.9500 . ? C59 C60 1.398(4) . ? C59 H59A 0.9500 . ? C60 C64 1.526(4) . ? C61 C62A 1.243(6) . ? C61 C63 1.461(6) . ? C61 C63A 1.616(7) . ? C61 C62 1.710(6) . ? C61 H61C 1.0000 . ? C61 H61B 1.0000 . ? C62 H62D 0.9800 . ? C62 H62F 0.9800 . ? C62 H62E 0.9800 . ? C62A H61B 1.1939 . ? C62A H62H 0.9800 . ? C62A H62I 0.9800 . ? C62A H62G 0.9800 . ? C63 H63E 0.9800 . ? C63 H63F 0.9800 . ? C63 H63D 0.9800 . ? C63A H63H 0.9800 . ? C63A H63I 0.9800 . ? C63A H63G 0.9800 . ? C64 C65 1.528(4) . ? C64 C66 1.539(3) . ? C64 H64A 1.0000 . ? C65 H65E 0.9800 . ? C65 H65F 0.9800 . ? C65 H65D 0.9800 . ? C66 H66D 0.9800 . ? C66 H66F 0.9800 . ? C66 H66E 0.9800 . ? Mn1' C5' 1.836(3) . ? Mn1' C4' 1.847(3) . ? Mn1' C6' 1.852(3) . ? Mn1' C2' 1.889(2) . ? Mn1' C1' 1.898(2) . ? Mn1' C3' 2.186(3) . ? O1' C4' 1.134(3) . ? O2' C5' 1.122(3) . ? O3' C6' 1.135(3) . ? N1' C1' 1.165(3) . ? N1' C7' 1.404(2) . ? N2' C2' 1.170(3) . ? N2' C37' 1.400(3) . ? C0AA C61' 1.621(6) . ? C0AA H0AB 0.9800 . ? C0AA H0AC 0.9800 . ? C0AA H0AA 0.9800 . ? C3' H3'A 0.9800 . ? C3' H3'C 0.9800 . ? C3' H3'B 0.9800 . ? C6 C61' 1.244(6) . ? C6 H6A 0.9800 . ? C6 H6C 0.9800 . ? C6 H6B 0.9800 . ? C7' C12' 1.401(3) . ? C7' C8' 1.402(3) . ? C8' C9' 1.398(3) . ? C8' C13' 1.494(3) . ? C9' C10' 1.388(3) . ? C9' H9' 0.9500 . ? C10' C11' 1.385(3) . ? C10' H10 0.9500 . ? C11' C12' 1.394(3) . ? C11' H11 0.9500 . ? C12' C25' 1.501(3) . ? C13' C18' 1.412(3) . ? C13' C14' 1.417(3) . ? C14' C15' 1.393(3) . ? C14' C19' 1.523(3) . ? C15' C16' 1.373(3) . ? C15' H15 0.9500 . ? C16' C17' 1.394(3) . ? C16' H16 0.9500 . ? C17' C18' 1.387(3) . ? C17' H17 0.9500 . ? C18' C22' 1.531(3) . ? C19' C20' 1.534(3) . ? C19' C21' 1.535(3) . ? C19' H19 1.0000 . ? C20' H20B 0.9800 . ? C20' H20C 0.9800 . ? C20' H20A 0.9800 . ? C21' H21A 0.9800 . ? C21' H21C 0.9800 . ? C21' H21B 0.9800 . ? C22' C24' 1.528(3) . ? C22' C23' 1.530(3) . ? C22' H22 1.0000 . ? C23' H23B 0.9800 . ? C23' H23C 0.9800 . ? C23' H23A 0.9800 . ? C24' H24A 0.9800 . ? C24' H24C 0.9800 . ? C24' H24B 0.9800 . ? C25' C26' 1.409(3) . ? C25' C30' 1.413(3) . ? C26' C27' 1.393(3) . ? C26' C31' 1.525(3) . ? C27' C28' 1.382(3) . ? C27' H27 0.9500 . ? C28' C29' 1.378(3) . ? C28' H28 0.9500 . ? C29' C30' 1.399(3) . ? C29' H29 0.9500 . ? C30' C34' 1.519(3) . ? C31' C33' 1.536(3) . ? C31' C32' 1.537(3) . ? C31' H31 1.0000 . ? C32' H32A 0.9800 . ? C32' H32C 0.9800 . ? C32' H32B 0.9800 . ? C33' H33A 0.9800 . ? C33' H33C 0.9800 . ? C33' H33B 0.9800 . ? C34' C36' 1.523(3) . ? C34' C35' 1.533(3) . ? C34' H34 1.0000 . ? C35' H35C 0.9800 . ? C35' H35B 0.9800 . ? C35' H35A 0.9800 . ? C36' H36A 0.9800 . ? C36' H36B 0.9800 . ? C36' H36C 0.9800 . ? C37' C42' 1.393(3) . ? C37' C38' 1.408(3) . ? C38' C39' 1.399(3) . ? C38' C43' 1.491(3) . ? C39' C40' 1.384(3) . ? C39' H39 0.9500 . ? C40' C41' 1.389(3) . ? C40' H40 0.9500 . ? C41' C42' 1.400(3) . ? C41' H41 0.9500 . ? C42' C55' 1.500(3) . ? C43' C44' 1.405(3) . ? C43' C48' 1.406(3) . ? C44' C45' 1.391(3) . ? C44' C49' 1.517(3) . ? C45' C46' 1.385(4) . ? C45' H45 0.9500 . ? C46' C47' 1.380(4) . ? C46' H46 0.9500 . ? C47' C48' 1.395(3) . ? C47' H47 0.9500 . ? C48' C52' 1.524(3) . ? C49' C51' 1.532(4) . ? C49' C50' 1.537(3) . ? C49' H49 1.0000 . ? C50' H50C 0.9800 . ? C50' H50B 0.9800 . ? C50' H50A 0.9800 . ? C51' H51C 0.9800 . ? C51' H51A 0.9800 . ? C51' H51B 0.9800 . ? C52' C54' 1.522(3) . ? C52' C53' 1.532(3) . ? C52' H52 1.0000 . ? C53' H53C 0.9800 . ? C53' H53B 0.9800 . ? C53' H53A 0.9800 . ? C54' H54A 0.9800 . ? C54' H54B 0.9800 . ? C54' H54C 0.9800 . ? C55' C60' 1.404(4) . ? C55' C56' 1.415(4) . ? C56' C57' 1.395(4) . ? C56' C61' 1.531(5) . ? C57' C58' 1.373(5) . ? C57' H57 0.9500 . ? C58' C59' 1.382(5) . ? C58' H58 0.9500 . ? C59' C60' 1.410(4) . ? C59' H59 0.9500 . ? C60' C64' 1.520(4) . ? C61' C63' 1.468(6) . ? C61' C62' 1.707(6) . ? C61' H61 1.0000 . ? C61' H61A 1.0000 . ? C62' H62A 0.9800 . ? C62' H62C 0.9800 . ? C62' H62B 0.9800 . ? C63' H61A 1.3075 . ? C63' H63C 0.9800 . ? C63' H63B 0.9800 . ? C63' H63A 0.9800 . ? C64' C65' 1.528(4) . ? C64' C66' 1.531(3) . ? C64' H64 1.0000 . ? C65' H65A 0.9800 . ? C65' H65C 0.9800 . ? C65' H65B 0.9800 . ? C66' H66A 0.9800 . ? C66' H66C 0.9800 . ? C66' H66B 0.9800 . ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag C5 Mn1 C6 94.22(12) . . ? C5 Mn1 C4 98.63(12) . . ? C6 Mn1 C4 167.10(12) . . ? C5 Mn1 C2 91.50(10) . . ? C6 Mn1 C2 90.35(10) . . ? C4 Mn1 C2 90.37(10) . . ? C5 Mn1 C1 92.53(10) . . ? C6 Mn1 C1 88.39(10) . . ? C4 Mn1 C1 89.97(10) . . ? C2 Mn1 C1 175.86(9) . . ? C5 Mn1 C3 177.69(10) . . ? C6 Mn1 C3 87.06(12) . . ? C4 Mn1 C3 80.13(11) . . ? C2 Mn1 C3 86.56(10) . . ? C1 Mn1 C3 89.43(10) . . ? C1 N1 C7 175.0(2) . . ? C2 N2 C37 175.0(2) . . ? N1 C1 Mn1 178.5(2) . . ? N2 C2 Mn1 179.9(3) . . ? Mn1 C3 H3A 109.5 . . ? Mn1 C3 H3B 109.5 . . ? H3A C3 H3B 109.5 . . ? Mn1 C3 H3C 109.5 . . ? H3A C3 H3C 109.5 . . ? H3B C3 H3C 109.5 . . ? O1 C4 Mn1 174.4(3) . . ? O2 C5 Mn1 179.4(3) . . ? O3 C6 Mn1 178.0(2) . . ? C8 C7 N1 118.71(19) . . ? C8 C7 C12 122.96(19) . . ? N1 C7 C12 118.32(18) . . ? C9 C8 C7 117.51(19) . . ? C9 C8 C13 121.57(19) . . ? C7 C8 C13 120.91(19) . . ? C10 C9 C8 120.8(2) . . ? C10 C9 H9 119.6 . . ? C8 C9 H9 119.6 . . ? C9 C10 C11 120.5(2) . . ? C9 C10 H10A 119.8 . . ? C11 C10 H10A 119.8 . . ? C10 C11 C12 121.1(2) . . ? C10 C11 H11A 119.5 . . ? C12 C11 H11A 119.5 . . ? C11 C12 C7 117.12(19) . . ? C11 C12 C25 121.31(19) . . ? C7 C12 C25 121.57(18) . . ? C14 C13 C18 121.0(2) . . ? C14 C13 C8 119.43(19) . . ? C18 C13 C8 119.5(2) . . ? C15 C14 C13 118.4(2) . . ? C15 C14 C19 120.5(2) . . ? C13 C14 C19 121.2(2) . . ? C16 C15 C14 120.7(2) . . ? C16 C15 H15A 119.6 . . ? C14 C15 H15A 119.6 . . ? C17 C16 C15 120.5(2) . . ? C17 C16 H16A 119.7 . . ? C15 C16 H16A 119.7 . . ? C16 C17 C18 121.1(2) . . ? C16 C17 H17A 119.4 . . ? C18 C17 H17A 119.4 . . ? C17 C18 C13 118.2(2) . . ? C17 C18 C22 119.5(2) . . ? C13 C18 C22 122.2(2) . . ? C14 C19 C21 109.87(19) . . ? C14 C19 C20 113.9(2) . . ? C21 C19 C20 109.86(19) . . ? C14 C19 H19A 107.7 . . ? C21 C19 H19A 107.7 . . ? C20 C19 H19A 107.7 . . ? C19 C20 H20D 109.5 . . ? C19 C20 H20F 109.5 . . ? H20D C20 H20F 109.5 . . ? C19 C20 H20E 109.5 . . ? H20D C20 H20E 109.5 . . ? H20F C20 H20E 109.5 . . ? C19 C21 H21E 109.5 . . ? C19 C21 H21F 109.5 . . ? H21E C21 H21F 109.5 . . ? C19 C21 H21D 109.5 . . ? H21E C21 H21D 109.5 . . ? H21F C21 H21D 109.5 . . ? C18 C22 C24 113.1(2) . . ? C18 C22 C23 110.2(2) . . ? C24 C22 C23 109.9(2) . . ? C18 C22 H22A 107.8 . . ? C24 C22 H22A 107.8 . . ? C23 C22 H22A 107.8 . . ? C22 C23 H23D 109.5 . . ? C22 C23 H23F 109.5 . . ? H23D C23 H23F 109.5 . . ? C22 C23 H23E 109.5 . . ? H23D C23 H23E 109.5 . . ? H23F C23 H23E 109.5 . . ? C22 C24 H24E 109.5 . . ? C22 C24 H24F 109.5 . . ? H24E C24 H24F 109.5 . . ? C22 C24 H24D 109.5 . . ? H24E C24 H24D 109.5 . . ? H24F C24 H24D 109.5 . . ? C30 C25 C26 120.62(19) . . ? C30 C25 C12 119.62(17) . . ? C26 C25 C12 119.75(19) . . ? C27 C26 C25 118.1(2) . . ? C27 C26 C31 119.47(18) . . ? C25 C26 C31 122.40(18) . . ? C28 C27 C26 121.6(2) . . ? C28 C27 H27A 119.2 . . ? C26 C27 H27A 119.2 . . ? C27 C28 C29 120.0(2) . . ? C27 C28 H28A 120.0 . . ? C29 C28 H28A 120.0 . . ? C28 C29 C30 120.9(2) . . ? C28 C29 H29A 119.5 . . ? C30 C29 H29A 119.5 . . ? C29 C30 C25 118.72(19) . . ? C29 C30 C34 120.3(2) . . ? C25 C30 C34 120.90(18) . . ? C26 C31 C33 110.69(18) . . ? C26 C31 C32 111.92(19) . . ? C33 C31 C32 109.89(18) . . ? C26 C31 H31A 108.1 . . ? C33 C31 H31A 108.1 . . ? C32 C31 H31A 108.1 . . ? C31 C32 H32E 109.5 . . ? C31 C32 H32F 109.5 . . ? H32E C32 H32F 109.5 . . ? C31 C32 H32D 109.5 . . ? H32E C32 H32D 109.5 . . ? H32F C32 H32D 109.5 . . ? C31 C33 H33D 109.5 . . ? C31 C33 H33F 109.5 . . ? H33D C33 H33F 109.5 . . ? C31 C33 H33E 109.5 . . ? H33D C33 H33E 109.5 . . ? H33F C33 H33E 109.5 . . ? C35 C34 C30 113.16(18) . . ? C35 C34 C36 110.78(19) . . ? C30 C34 C36 109.92(18) . . ? C35 C34 H34A 107.6 . . ? C30 C34 H34A 107.6 . . ? C36 C34 H34A 107.6 . . ? C34 C35 H35E 109.5 . . ? C34 C35 H35F 109.5 . . ? H35E C35 H35F 109.5 . . ? C34 C35 H35D 109.5 . . ? H35E C35 H35D 109.5 . . ? H35F C35 H35D 109.5 . . ? C34 C36 H36D 109.5 . . ? C34 C36 H36F 109.5 . . ? H36D C36 H36F 109.5 . . ? C34 C36 H36E 109.5 . . ? H36D C36 H36E 109.5 . . ? H36F C36 H36E 109.5 . . ? C38 C37 C42 123.0(2) . . ? C38 C37 N2 118.31(19) . . ? C42 C37 N2 118.7(2) . . ? C37 C38 C39 117.4(2) . . ? C37 C38 C43 119.38(19) . . ? C39 C38 C43 123.2(2) . . ? C40 C39 C38 121.1(2) . . ? C40 C39 H39A 119.5 . . ? C38 C39 H39A 119.5 . . ? C41 C40 C39 119.9(2) . . ? C41 C40 H40A 120.0 . . ? C39 C40 H40A 120.0 . . ? C40 C41 C42 121.4(2) . . ? C40 C41 H41A 119.3 . . ? C42 C41 H41A 119.3 . . ? C41 C42 C37 117.2(2) . . ? C41 C42 C55 122.1(2) . . ? C37 C42 C55 120.7(2) . . ? C44 C43 C48 120.8(2) . . ? C44 C43 C38 119.2(2) . . ? C48 C43 C38 119.95(19) . . ? C45 C44 C43 118.5(2) . . ? C45 C44 C49 120.5(2) . . ? C43 C44 C49 121.0(2) . . ? C44 C45 C46 121.0(2) . . ? C44 C45 H45A 119.5 . . ? C46 C45 H45A 119.5 . . ? C47 C46 C45 120.1(2) . . ? C47 C46 H46A 120.0 . . ? C45 C46 H46A 120.0 . . ? C46 C47 C48 121.1(2) . . ? C46 C47 H47A 119.4 . . ? C48 C47 H47A 119.4 . . ? C47 C48 C43 118.5(2) . . ? C47 C48 C52 120.8(2) . . ? C43 C48 C52 120.7(2) . . ? C44 C49 C51 113.3(2) . . ? C44 C49 C50 109.5(2) . . ? C51 C49 C50 110.7(2) . . ? C44 C49 H49A 107.7 . . ? C51 C49 H49A 107.7 . . ? C50 C49 H49A 107.7 . . ? C49 C50 H50F 109.5 . . ? C49 C50 H50E 109.5 . . ? H50F C50 H50E 109.5 . . ? C49 C50 H50D 109.5 . . ? H50F C50 H50D 109.5 . . ? H50E C50 H50D 109.5 . . ? C49 C51 H51D 109.5 . . ? C49 C51 H51E 109.5 . . ? H51D C51 H51E 109.5 . . ? C49 C51 H51F 109.5 . . ? H51D C51 H51F 109.5 . . ? H51E C51 H51F 109.5 . . ? C48 C52 C53 110.2(2) . . ? C48 C52 C54 113.1(2) . . ? C53 C52 C54 110.9(2) . . ? C48 C52 H52A 107.5 . . ? C53 C52 H52A 107.5 . . ? C54 C52 H52A 107.5 . . ? C52 C53 H53F 109.5 . . ? C52 C53 H53E 109.5 . . ? H53F C53 H53E 109.5 . . ? C52 C53 H53D 109.5 . . ? H53F C53 H53D 109.5 . . ? H53E C53 H53D 109.5 . . ? C52 C54 H54D 109.5 . . ? C52 C54 H54E 109.5 . . ? H54D C54 H54E 109.5 . . ? C52 C54 H54F 109.5 . . ? H54D C54 H54F 109.5 . . ? H54E C54 H54F 109.5 . . ? C60 C55 C56 121.5(3) . . ? C60 C55 C42 119.3(2) . . ? C56 C55 C42 119.2(2) . . ? C57 C56 C55 117.1(3) . . ? C57 C56 C61 121.0(3) . . ? C55 C56 C61 121.9(3) . . ? C58 C57 C56 122.4(3) . . ? C58 C57 H57A 118.8 . . ? C56 C57 H57A 118.8 . . ? C57 C58 C59 120.1(3) . . ? C57 C58 H58A 120.0 . . ? C59 C58 H58A 120.0 . . ? C58 C59 C60 120.6(3) . . ? C58 C59 H59A 119.7 . . ? C60 C59 H59A 119.7 . . ? C59 C60 C55 118.3(3) . . ? C59 C60 C64 120.3(3) . . ? C55 C60 C64 121.4(2) . . ? C62A C61 C63 124.4(5) . . ? C62A C61 C56 111.4(4) . . ? C63 C61 C56 124.1(4) . . ? C62A C61 C63A 121.8(5) . . ? C63 C61 C63A 48.8(3) . . ? C56 C61 C63A 100.7(4) . . ? C62A C61 C62 42.2(4) . . ? C63 C61 C62 104.1(3) . . ? C56 C61 C62 116.3(3) . . ? C63A C61 C62 80.4(3) . . ? C62A C61 H61C 107.4 . . ? C63 C61 H61C 60.0 . . ? C56 C61 H61C 107.4 . . ? C63A C61 H61C 107.4 . . ? C62 C61 H61C 133.4 . . ? C62A C61 H61B 63.2 . . ? C63 C61 H61B 103.2 . . ? C56 C61 H61B 103.2 . . ? C63A C61 H61B 150.9 . . ? C62 C61 H61B 103.2 . . ? H61C C61 H61B 49.4 . . ? C61 C62 H62D 109.5 . . ? C61 C62 H62F 109.5 . . ? C61 C62 H62E 109.5 . . ? C61 C62A H61B 48.4 . . ? C61 C62A H62H 109.5 . . ? C61 C62A H62I 109.5 . . ? H62H C62A H62I 109.5 . . ? C61 C62A H62G 109.5 . . ? H62H C62A H62G 109.5 . . ? H62I C62A H62G 109.5 . . ? C61 C63 H63E 109.5 . . ? C61 C63 H63F 109.5 . . ? C61 C63 H63D 109.5 . . ? C61 C63A H63H 109.5 . . ? C61 C63A H63I 109.5 . . ? H63H C63A H63I 109.5 . . ? C61 C63A H63G 109.5 . . ? H63H C63A H63G 109.5 . . ? H63I C63A H63G 109.5 . . ? C60 C64 C65 113.9(2) . . ? C60 C64 C66 110.7(2) . . ? C65 C64 C66 109.0(2) . . ? C60 C64 H64A 107.6 . . ? C65 C64 H64A 107.6 . . ? C66 C64 H64A 107.6 . . ? C64 C65 H65E 109.5 . . ? C64 C65 H65F 109.5 . . ? H65E C65 H65F 109.5 . . ? C64 C65 H65D 109.5 . . ? H65E C65 H65D 109.5 . . ? H65F C65 H65D 109.5 . . ? C64 C66 H66D 109.5 . . ? C64 C66 H66F 109.5 . . ? H66D C66 H66F 109.5 . . ? C64 C66 H66E 109.5 . . ? H66D C66 H66E 109.5 . . ? H66F C66 H66E 109.5 . . ? C5' Mn1' C4' 94.17(12) . . ? C5' Mn1' C6' 98.61(12) . . ? C4' Mn1' C6' 167.17(12) . . ? C5' Mn1' C2' 91.71(10) . . ? C4' Mn1' C2' 90.66(10) . . ? C6' Mn1' C2' 90.16(10) . . ? C5' Mn1' C1' 92.31(10) . . ? C4' Mn1' C1' 88.14(10) . . ? C6' Mn1' C1' 90.14(10) . . ? C2' Mn1' C1' 175.88(9) . . ? C5' Mn1' C3' 177.81(10) . . ? C4' Mn1' C3' 86.92(12) . . ? C6' Mn1' C3' 80.36(11) . . ? C2' Mn1' C3' 86.37(10) . . ? C1' Mn1' C3' 89.62(9) . . ? C1' N1' C7' 174.8(2) . . ? C2' N2' C37' 175.2(2) . . ? C61' C0AA H0AB 109.5 . . ? C61' C0AA H0AC 109.5 . . ? H0AB C0AA H0AC 109.5 . . ? C61' C0AA H0AA 109.5 . . ? H0AB C0AA H0AA 109.5 . . ? H0AC C0AA H0AA 109.5 . . ? N1' C1' Mn1' 178.4(2) . . ? N2' C2' Mn1' 179.8(3) . . ? Mn1' C3' H3'A 109.5 . . ? Mn1' C3' H3'C 109.5 . . ? H3'A C3' H3'C 109.5 . . ? Mn1' C3' H3'B 109.5 . . ? H3'A C3' H3'B 109.5 . . ? H3'C C3' H3'B 109.5 . . ? O1' C4' Mn1' 177.8(3) . . ? O2' C5' Mn1' 179.1(2) . . ? C61' C6 H6A 109.5 . . ? C61' C6 H6C 109.5 . . ? H6A C6 H6C 109.5 . . ? C61' C6 H6B 109.5 . . ? H6A C6 H6B 109.5 . . ? H6C C6 H6B 109.5 . . ? O3' C6' Mn1' 174.4(3) . . ? C12' C7' C8' 123.21(18) . . ? C12' C7' N1' 118.29(18) . . ? C8' C7' N1' 118.50(18) . . ? C9' C8' C7' 117.08(19) . . ? C9' C8' C13' 121.18(19) . . ? C7' C8' C13' 121.74(18) . . ? C10' C9' C8' 120.9(2) . . ? C10' C9' H9' 119.5 . . ? C8' C9' H9' 119.5 . . ? C11' C10' C9' 120.41(19) . . ? C11' C10' H10 119.8 . . ? C9' C10' H10 119.8 . . ? C10' C11' C12' 121.0(2) . . ? C10' C11' H11 119.5 . . ? C12' C11' H11 119.5 . . ? C11' C12' C7' 117.26(19) . . ? C11' C12' C25' 121.75(19) . . ? C7' C12' C25' 120.98(18) . . ? C18' C13' C14' 120.18(18) . . ? C18' C13' C8' 119.66(18) . . ? C14' C13' C8' 120.13(19) . . ? C15' C14' C13' 118.8(2) . . ? C15' C14' C19' 119.12(18) . . ? C13' C14' C19' 122.11(18) . . ? C16' C15' C14' 121.1(2) . . ? C16' C15' H15 119.5 . . ? C14' C15' H15 119.5 . . ? C15' C16' C17' 120.3(2) . . ? C15' C16' H16 119.9 . . ? C17' C16' H16 119.9 . . ? C18' C17' C16' 120.9(2) . . ? C18' C17' H17 119.6 . . ? C16' C17' H17 119.6 . . ? C17' C18' C13' 118.85(19) . . ? C17' C18' C22' 120.4(2) . . ? C13' C18' C22' 120.70(18) . . ? C14' C19' C20' 112.20(19) . . ? C14' C19' C21' 111.23(18) . . ? C20' C19' C21' 109.18(18) . . ? C14' C19' H19 108.0 . . ? C20' C19' H19 108.0 . . ? C21' C19' H19 108.0 . . ? C19' C20' H20B 109.5 . . ? C19' C20' H20C 109.5 . . ? H20B C20' H20C 109.5 . . ? C19' C20' H20A 109.5 . . ? H20B C20' H20A 109.5 . . ? H20C C20' H20A 109.5 . . ? C19' C21' H21A 109.5 . . ? C19' C21' H21C 109.5 . . ? H21A C21' H21C 109.5 . . ? C19' C21' H21B 109.5 . . ? H21A C21' H21B 109.5 . . ? H21C C21' H21B 109.5 . . ? C24' C22' C23' 110.49(19) . . ? C24' C22' C18' 110.29(18) . . ? C23' C22' C18' 113.16(19) . . ? C24' C22' H22 107.6 . . ? C23' C22' H22 107.6 . . ? C18' C22' H22 107.6 . . ? C22' C23' H23B 109.5 . . ? C22' C23' H23C 109.5 . . ? H23B C23' H23C 109.5 . . ? C22' C23' H23A 109.5 . . ? H23B C23' H23A 109.5 . . ? H23C C23' H23A 109.5 . . ? C22' C24' H24A 109.5 . . ? C22' C24' H24C 109.5 . . ? H24A C24' H24C 109.5 . . ? C22' C24' H24B 109.5 . . ? H24A C24' H24B 109.5 . . ? H24C C24' H24B 109.5 . . ? C26' C25' C30' 121.1(2) . . ? C26' C25' C12' 119.70(19) . . ? C30' C25' C12' 119.2(2) . . ? C27' C26' C25' 118.3(2) . . ? C27' C26' C31' 120.7(2) . . ? C25' C26' C31' 121.0(2) . . ? C28' C27' C26' 121.0(2) . . ? C28' C27' H27 119.5 . . ? C26' C27' H27 119.5 . . ? C29' C28' C27' 120.5(2) . . ? C29' C28' H28 119.7 . . ? C27' C28' H28 119.7 . . ? C28' C29' C30' 120.9(2) . . ? C28' C29' H29 119.5 . . ? C30' C29' H29 119.5 . . ? C29' C30' C25' 118.1(2) . . ? C29' C30' C34' 119.2(2) . . ? C25' C30' C34' 122.6(2) . . ? C26' C31' C33' 110.18(18) . . ? C26' C31' C32' 113.5(2) . . ? C33' C31' C32' 110.02(19) . . ? C26' C31' H31 107.6 . . ? C33' C31' H31 107.6 . . ? C32' C31' H31 107.6 . . ? C31' C32' H32A 109.5 . . ? C31' C32' H32C 109.5 . . ? H32A C32' H32C 109.5 . . ? C31' C32' H32B 109.5 . . ? H32A C32' H32B 109.5 . . ? H32C C32' H32B 109.5 . . ? C31' C33' H33A 109.5 . . ? C31' C33' H33C 109.5 . . ? H33A C33' H33C 109.5 . . ? C31' C33' H33B 109.5 . . ? H33A C33' H33B 109.5 . . ? H33C C33' H33B 109.5 . . ? C30' C34' C36' 113.1(2) . . ? C30' C34' C35' 110.2(2) . . ? C36' C34' C35' 110.1(2) . . ? C30' C34' H34 107.7 . . ? C36' C34' H34 107.7 . . ? C35' C34' H34 107.7 . . ? C34' C35' H35C 109.5 . . ? C34' C35' H35B 109.5 . . ? H35C C35' H35B 109.5 . . ? C34' C35' H35A 109.5 . . ? H35C C35' H35A 109.5 . . ? H35B C35' H35A 109.5 . . ? C34' C36' H36A 109.5 . . ? C34' C36' H36B 109.5 . . ? H36A C36' H36B 109.5 . . ? C34' C36' H36C 109.5 . . ? H36A C36' H36C 109.5 . . ? H36B C36' H36C 109.5 . . ? C42' C37' N2' 118.6(2) . . ? C42' C37' C38' 123.30(19) . . ? N2' C37' C38' 118.15(19) . . ? C39' C38' C37' 117.1(2) . . ? C39' C38' C43' 123.4(2) . . ? C37' C38' C43' 119.52(18) . . ? C40' C39' C38' 120.9(2) . . ? C40' C39' H39 119.5 . . ? C38' C39' H39 119.5 . . ? C39' C40' C41' 120.5(2) . . ? C39' C40' H40 119.8 . . ? C41' C40' H40 119.8 . . ? C40' C41' C42' 120.9(2) . . ? C40' C41' H41 119.5 . . ? C42' C41' H41 119.5 . . ? C37' C42' C41' 117.2(2) . . ? C37' C42' C55' 121.05(19) . . ? C41' C42' C55' 121.7(2) . . ? C44' C43' C48' 121.3(2) . . ? C44' C43' C38' 119.1(2) . . ? C48' C43' C38' 119.6(2) . . ? C45' C44' C43' 118.1(2) . . ? C45' C44' C49' 120.5(2) . . ? C43' C44' C49' 121.4(2) . . ? C46' C45' C44' 121.4(2) . . ? C46' C45' H45 119.3 . . ? C44' C45' H45 119.3 . . ? C47' C46' C45' 119.7(2) . . ? C47' C46' H46 120.2 . . ? C45' C46' H46 120.2 . . ? C46' C47' C48' 121.3(2) . . ? C46' C47' H47 119.4 . . ? C48' C47' H47 119.4 . . ? C47' C48' C43' 118.2(2) . . ? C47' C48' C52' 120.6(2) . . ? C43' C48' C52' 121.2(2) . . ? C44' C49' C51' 113.8(2) . . ? C44' C49' C50' 109.4(2) . . ? C51' C49' C50' 110.6(2) . . ? C44' C49' H49 107.6 . . ? C51' C49' H49 107.6 . . ? C50' C49' H49 107.6 . . ? C49' C50' H50C 109.5 . . ? C49' C50' H50B 109.5 . . ? H50C C50' H50B 109.5 . . ? C49' C50' H50A 109.5 . . ? H50C C50' H50A 109.5 . . ? H50B C50' H50A 109.5 . . ? C49' C51' H51C 109.5 . . ? C49' C51' H51A 109.5 . . ? H51C C51' H51A 109.5 . . ? C49' C51' H51B 109.5 . . ? H51C C51' H51B 109.5 . . ? H51A C51' H51B 109.5 . . ? C54' C52' C48' 113.6(2) . . ? C54' C52' C53' 110.8(2) . . ? C48' C52' C53' 109.9(2) . . ? C54' C52' H52 107.4 . . ? C48' C52' H52 107.4 . . ? C53' C52' H52 107.4 . . ? C52' C53' H53C 109.5 . . ? C52' C53' H53B 109.5 . . ? H53C C53' H53B 109.5 . . ? C52' C53' H53A 109.5 . . ? H53C C53' H53A 109.5 . . ? H53B C53' H53A 109.5 . . ? C52' C54' H54A 109.5 . . ? C52' C54' H54B 109.5 . . ? H54A C54' H54B 109.5 . . ? C52' C54' H54C 109.5 . . ? H54A C54' H54C 109.5 . . ? H54B C54' H54C 109.5 . . ? C60' C55' C56' 121.7(2) . . ? C60' C55' C42' 119.3(2) . . ? C56' C55' C42' 119.0(2) . . ? C57' C56' C55' 117.7(3) . . ? C57' C56' C61' 120.3(3) . . ? C55' C56' C61' 122.0(3) . . ? C58' C57' C56' 121.4(3) . . ? C58' C57' H57 119.3 . . ? C56' C57' H57 119.3 . . ? C57' C58' C59' 120.8(3) . . ? C57' C58' H58 119.6 . . ? C59' C58' H58 119.6 . . ? C58' C59' C60' 120.5(3) . . ? C58' C59' H59 119.7 . . ? C60' C59' H59 119.7 . . ? C55' C60' C59' 117.9(3) . . ? C55' C60' C64' 121.8(2) . . ? C59' C60' C64' 120.3(3) . . ? C6 C61' C63' 124.4(5) . . ? C6 C61' C56' 111.5(4) . . ? C63' C61' C56' 124.0(4) . . ? C6 C61' C0AA 121.8(5) . . ? C63' C61' C0AA 48.3(3) . . ? C56' C61' C0AA 100.7(3) . . ? C6 C61' C62' 42.0(4) . . ? C63' C61' C62' 103.9(3) . . ? C56' C61' C62' 116.3(3) . . ? C0AA C61' C62' 80.6(3) . . ? C6 C61' H61 63.6 . . ? C63' C61' H61 103.3 . . ? C56' C61' H61 103.3 . . ? C0AA C61' H61 150.6 . . ? C62' C61' H61 103.3 . . ? C6 C61' H61A 107.4 . . ? C63' C61' H61A 60.5 . . ? C56' C61' H61A 107.3 . . ? C0AA C61' H61A 107.3 . . ? C62' C61' H61A 133.4 . . ? H61 C61' H61A 49.0 . . ? C61' C62' H62A 109.5 . . ? C61' C62' H62C 109.5 . . ? C61' C62' H62B 109.5 . . ? C61' C63' H61A 41.7 . . ? C61' C63' H63C 109.5 . . ? H61A C63' H63C 75.7 . . ? C61' C63' H63B 109.5 . . ? H61A C63' H63B 99.3 . . ? C61' C63' H63A 109.5 . . ? H61A C63' H63A 146.1 . . ? C60' C64' C65' 114.1(2) . . ? C60' C64' C66' 110.8(2) . . ? C65' C64' C66' 109.2(2) . . ? C60' C64' H64 107.5 . . ? C65' C64' H64 107.5 . . ? C66' C64' H64 107.5 . . ? C64' C65' H65A 109.5 . . ? C64' C65' H65C 109.5 . . ? H65A C65' H65C 109.5 . . ? C64' C65' H65B 109.5 . . ? H65A C65' H65B 109.5 . . ? H65C C65' H65B 109.5 . . ? C64' C66' H66A 109.5 . . ? C64' C66' H66C 109.5 . . ? H66A C66' H66C 109.5 . . ? C64' C66' H66B 109.5 . . ? H66A C66' H66B 109.5 . . ? H66C C66' H66B 109.5 . . ? _diffrn_measured_fraction_theta_max 0.968 _diffrn_reflns_theta_full 25.00 _diffrn_measured_fraction_theta_full 0.987 _refine_diff_density_max 0.514 _refine_diff_density_min -0.433 _refine_diff_density_rms 0.051 #===END data_JFig370 _database_code_depnum_ccdc_archive 'CCDC 785487' #TrackingRef 'cif-full.cif' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common (Cl2(CH3)Si)Mn(CO)3(CNArDipp2)2 _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C66 H77 Cl2 Mn N2 O3 Si' _chemical_formula_weight 1100.23 loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Si Si 0.0817 0.0704 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Cl Cl 0.1484 0.1585 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Mn Mn 0.3368 0.7283 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting Triclinic _symmetry_space_group_name_H-M P-1 loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, -y, -z' _cell_length_a 10.625(3) _cell_length_b 23.786(7) _cell_length_c 25.576(8) _cell_angle_alpha 78.096(4) _cell_angle_beta 78.251(4) _cell_angle_gamma 84.842(4) _cell_volume 6185(3) _cell_formula_units_Z 4 _cell_measurement_temperature 100(2) _cell_measurement_reflns_used 3651 _cell_measurement_theta_min 2.17 _cell_measurement_theta_max 22.59 _exptl_crystal_description Block _exptl_crystal_colour Yellow _exptl_crystal_size_max 0.18 _exptl_crystal_size_mid 0.13 _exptl_crystal_size_min 0.08 _exptl_crystal_density_meas 'not measured' _exptl_crystal_density_diffrn 1.182 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 2336 _exptl_absorpt_coefficient_mu 0.364 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.9374 _exptl_absorpt_correction_T_max 0.9715 _exptl_absorpt_process_details TWINABS _exptl_special_details ; ? ; _diffrn_ambient_temperature 100(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'Bruker APEX CCD' _diffrn_measurement_method '\f and \w scans' _diffrn_reflns_number 22216 _diffrn_reflns_av_R_equivalents 0.0000 _diffrn_reflns_av_sigmaI/netI 0.1606 _diffrn_reflns_limit_h_min -12 _diffrn_reflns_limit_h_max 12 _diffrn_reflns_limit_k_min -27 _diffrn_reflns_limit_k_max 28 _diffrn_reflns_limit_l_min 0 _diffrn_reflns_limit_l_max 30 _diffrn_reflns_theta_min 1.96 _diffrn_reflns_theta_max 25.41 _reflns_number_total 22216 _reflns_number_gt 11854 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'Bruker APEX2' _computing_cell_refinement 'Bruker SAINT' _computing_data_reduction 'Bruker SAINT' _computing_structure_solution 'SHELXS-97 (Sheldrick, 2008)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 2008)' _computing_molecular_graphics 'Bruker SHELXTL' _computing_publication_material 'Bruker SHELXTL' _refine_special_details ; Refinement of F^2^ against ALL reflections. The weighted R-factor wR and goodness of fit S are based on F^2^, conventional R-factors R are based on F, with F set to zero for negative F^2^. The threshold expression of F^2^ > 2sigma(F^2^) is used only for calculating R-factors(gt) etc. and is not relevant to the choice of reflections for refinement. R-factors based on F^2^ are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger. ; _refine_ls_structure_factor_coef Fsqd _refine_ls_matrix_type full _refine_ls_weighting_scheme calc _refine_ls_weighting_details 'calc w=1/[\s^2^(Fo^2^)+(0.0758P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment constr _refine_ls_extinction_method SHELXL _refine_ls_extinction_coef 0.00008(13) _refine_ls_extinction_expression Fc^*^=kFc[1+0.001xFc^2^\l^3^/sin(2\q)]^-1/4^ _refine_ls_number_reflns 22216 _refine_ls_number_parameters 1386 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.1622 _refine_ls_R_factor_gt 0.0818 _refine_ls_wR_factor_ref 0.1942 _refine_ls_wR_factor_gt 0.1627 _refine_ls_goodness_of_fit_ref 1.013 _refine_ls_restrained_S_all 1.013 _refine_ls_shift/su_max 0.001 _refine_ls_shift/su_mean 0.000 loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_occupancy _atom_site_symmetry_multiplicity _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group Mn1 Mn 0.80114(7) 0.29269(3) 0.75589(3) 0.0230(2) Uani 1 1 d . . . Cl1 Cl 1.13997(12) 0.28909(6) 0.76975(6) 0.0368(4) Uani 1 1 d . . . Cl2 Cl 1.03576(13) 0.16487(6) 0.77202(6) 0.0406(4) Uani 1 1 d . . . Si1 Si 1.01094(13) 0.25220(6) 0.73654(6) 0.0254(4) Uani 1 1 d . . . O1 O 0.7941(3) 0.29576(16) 0.63942(16) 0.0362(10) Uani 1 1 d . . . O2 O 0.5344(4) 0.34467(17) 0.77811(18) 0.0500(12) Uani 1 1 d . . . O3 O 0.8463(4) 0.27560(17) 0.86991(16) 0.0450(11) Uani 1 1 d . . . N1 N 0.9206(4) 0.41024(18) 0.72991(16) 0.0196(9) Uani 1 1 d . . . N2 N 0.7193(4) 0.16956(18) 0.77570(15) 0.0195(9) Uani 1 1 d . . . C1 C 0.8762(4) 0.3653(2) 0.73950(19) 0.0211(12) Uani 1 1 d . . . C2 C 0.7484(5) 0.2171(2) 0.7694(2) 0.0229(12) Uani 1 1 d . . . C3 C 0.7974(5) 0.2956(2) 0.6835(2) 0.0245(12) Uani 1 1 d . . . C4 C 0.6378(5) 0.3239(2) 0.7700(2) 0.0292(13) Uani 1 1 d . . . C5 C 0.8278(5) 0.2827(2) 0.8267(3) 0.0341(14) Uani 1 1 d . . . C6 C 0.9622(4) 0.4667(2) 0.7133(2) 0.0190(11) Uani 1 1 d . . . C7 C 1.0032(4) 0.4883(2) 0.65793(19) 0.0172(11) Uani 1 1 d . . . C8 C 1.0378(4) 0.5456(2) 0.6414(2) 0.0207(11) Uani 1 1 d . . . H8 H 1.0625 0.5614 0.6038 0.025 Uiso 1 1 calc R . . C9 C 1.0359(4) 0.5793(2) 0.6798(2) 0.0227(12) Uani 1 1 d . . . H9 H 1.0609 0.6179 0.6686 0.027 Uiso 1 1 calc R . . C10 C 0.9977(4) 0.5566(2) 0.7345(2) 0.0210(12) Uani 1 1 d . . . H10 H 0.9966 0.5802 0.7603 0.025 Uiso 1 1 calc R . . C11 C 0.9607(4) 0.5000(2) 0.75279(19) 0.0181(11) Uani 1 1 d . . . C12 C 1.0091(4) 0.4507(2) 0.61684(19) 0.0214(12) Uani 1 1 d . . . C13 C 0.8987(4) 0.4444(2) 0.59733(19) 0.0220(12) Uani 1 1 d . . . C14 C 0.9097(5) 0.4083(2) 0.5598(2) 0.0290(13) Uani 1 1 d . . . H14 H 0.8354 0.4024 0.5467 0.035 Uiso 1 1 calc R . . C15 C 1.0253(5) 0.3811(2) 0.5412(2) 0.0281(13) Uani 1 1 d . . . H15 H 1.0301 0.3568 0.5156 0.034 Uiso 1 1 calc R . . C16 C 1.1339(5) 0.3892(2) 0.5600(2) 0.0285(13) Uani 1 1 d . . . H16 H 1.2133 0.3705 0.5469 0.034 Uiso 1 1 calc R . . C17 C 1.1292(4) 0.4244(2) 0.59784(19) 0.0201(11) Uani 1 1 d . . . C18 C 0.7725(4) 0.4767(2) 0.6138(2) 0.0261(13) Uani 1 1 d . . . H18 H 0.7863 0.5018 0.6389 0.031 Uiso 1 1 calc R . . C19 C 0.7315(6) 0.5158(2) 0.5642(2) 0.0414(15) Uani 1 1 d . . . H19A H 0.7096 0.4921 0.5404 0.062 Uiso 1 1 calc R . . H19C H 0.8023 0.5400 0.5442 0.062 Uiso 1 1 calc R . . H19B H 0.6562 0.5402 0.5760 0.062 Uiso 1 1 calc R . . C20 C 0.6656(5) 0.4372(2) 0.6439(2) 0.0391(15) Uani 1 1 d . . . H20B H 0.5864 0.4603 0.6537 0.059 Uiso 1 1 calc R . . H20C H 0.6904 0.4142 0.6770 0.059 Uiso 1 1 calc R . . H20A H 0.6511 0.4116 0.6204 0.059 Uiso 1 1 calc R . . C21 C 1.2519(4) 0.4337(2) 0.6165(2) 0.0273(13) Uani 1 1 d . . . H21 H 1.2280 0.4580 0.6449 0.033 Uiso 1 1 calc R . . C22 C 1.3449(5) 0.4664(2) 0.5692(2) 0.0291(13) Uani 1 1 d . . . H22A H 1.3731 0.4427 0.5415 0.044 Uiso 1 1 calc R . . H22C H 1.4198 0.4755 0.5823 0.044 Uiso 1 1 calc R . . H22B H 1.3018 0.5022 0.5534 0.044 Uiso 1 1 calc R . . C23 C 1.3156(5) 0.3776(2) 0.6418(2) 0.0381(15) Uani 1 1 d . . . H23B H 1.2564 0.3586 0.6739 0.057 Uiso 1 1 calc R . . H23C H 1.3945 0.3857 0.6526 0.057 Uiso 1 1 calc R . . H23A H 1.3371 0.3522 0.6152 0.057 Uiso 1 1 calc R . . C24 C 0.9197(4) 0.4783(2) 0.8125(2) 0.0213(12) Uani 1 1 d . . . C25 C 0.7948(5) 0.4921(2) 0.8378(2) 0.0278(13) Uani 1 1 d . . . C26 C 0.7616(6) 0.4769(2) 0.8944(2) 0.0371(15) Uani 1 1 d . . . H26 H 0.6766 0.4853 0.9122 0.045 Uiso 1 1 calc R . . C27 C 0.8509(6) 0.4497(2) 0.9245(2) 0.0396(15) Uani 1 1 d . . . H27 H 0.8283 0.4409 0.9631 0.048 Uiso 1 1 calc R . . C28 C 0.9722(5) 0.4354(2) 0.8990(2) 0.0321(14) Uani 1 1 d . . . H28 H 1.0321 0.4160 0.9204 0.038 Uiso 1 1 calc R . . C29 C 1.0104(5) 0.4481(2) 0.8427(2) 0.0254(12) Uani 1 1 d . . . C30 C 0.6939(5) 0.5211(2) 0.8052(2) 0.0321(14) Uani 1 1 d . . . H30 H 0.7387 0.5326 0.7665 0.039 Uiso 1 1 calc R . . C31 C 0.6308(6) 0.5751(3) 0.8236(3) 0.0577(19) Uani 1 1 d . . . H31A H 0.5631 0.5904 0.8029 0.087 Uiso 1 1 calc R . . H31C H 0.6954 0.6039 0.8174 0.087 Uiso 1 1 calc R . . H31B H 0.5930 0.5660 0.8625 0.087 Uiso 1 1 calc R . . C32 C 0.5923(7) 0.4784(3) 0.8063(4) 0.082(3) Uani 1 1 d . . . H32A H 0.6330 0.4475 0.7876 0.122 Uiso 1 1 calc R . . H32B H 0.5241 0.4986 0.7879 0.122 Uiso 1 1 calc R . . H32C H 0.5553 0.4620 0.8442 0.122 Uiso 1 1 calc R . . C33 C 1.1457(5) 0.4314(2) 0.8150(2) 0.0301(13) Uani 1 1 d . . . H33 H 1.1384 0.4204 0.7801 0.036 Uiso 1 1 calc R . . C34 C 1.2348(5) 0.4806(3) 0.8009(2) 0.0398(15) Uani 1 1 d . . . H34A H 1.1953 0.5142 0.7797 0.060 Uiso 1 1 calc R . . H34B H 1.3169 0.4693 0.7794 0.060 Uiso 1 1 calc R . . H34C H 1.2499 0.4903 0.8344 0.060 Uiso 1 1 calc R . . C35 C 1.2044(6) 0.3791(3) 0.8494(2) 0.0459(17) Uani 1 1 d . . . H35C H 1.2243 0.3900 0.8816 0.069 Uiso 1 1 calc R . . H35B H 1.2836 0.3652 0.8277 0.069 Uiso 1 1 calc R . . H35A H 1.1429 0.3485 0.8608 0.069 Uiso 1 1 calc R . . C36 C 0.6849(4) 0.1129(2) 0.7842(2) 0.0208(12) Uani 1 1 d . . . C37 C 0.6854(4) 0.0882(2) 0.73860(19) 0.0182(11) Uani 1 1 d . . . C38 C 0.6433(5) 0.0331(2) 0.7488(2) 0.0284(13) Uani 1 1 d . . . H38 H 0.6436 0.0151 0.7189 0.034 Uiso 1 1 calc R . . C39 C 0.6008(4) 0.0029(2) 0.8007(2) 0.0262(12) Uani 1 1 d . . . H39 H 0.5702 -0.0346 0.8060 0.031 Uiso 1 1 calc R . . C40 C 0.6031(4) 0.0280(2) 0.8456(2) 0.0263(12) Uani 1 1 d . . . H40 H 0.5766 0.0068 0.8814 0.032 Uiso 1 1 calc R . . C41 C 0.6438(4) 0.0834(2) 0.8381(2) 0.0206(12) Uani 1 1 d . . . C42 C 0.7230(5) 0.1217(2) 0.6815(2) 0.0226(12) Uani 1 1 d . . . C43 C 0.6309(5) 0.1604(2) 0.6591(2) 0.0270(13) Uani 1 1 d . . . C44 C 0.6622(5) 0.1874(2) 0.6050(2) 0.0328(14) Uani 1 1 d . . . H44 H 0.6008 0.2133 0.5892 0.039 Uiso 1 1 calc R . . C45 C 0.7818(6) 0.1770(3) 0.5737(2) 0.0394(15) Uani 1 1 d . . . H45 H 0.8017 0.1959 0.5367 0.047 Uiso 1 1 calc R . . C46 C 0.8712(5) 0.1398(2) 0.5960(2) 0.0346(14) Uani 1 1 d . . . H46 H 0.9534 0.1339 0.5744 0.041 Uiso 1 1 calc R . . C47 C 0.8434(5) 0.1103(2) 0.6502(2) 0.0262(13) Uani 1 1 d . . . C48 C 0.4993(5) 0.1721(2) 0.6922(2) 0.0328(14) Uani 1 1 d . . . H48 H 0.5064 0.1616 0.7314 0.039 Uiso 1 1 calc R . . C49 C 0.4017(5) 0.1331(3) 0.6833(3) 0.0479(17) Uani 1 1 d . . . H49A H 0.3932 0.1419 0.6450 0.072 Uiso 1 1 calc R . . H49C H 0.3180 0.1397 0.7063 0.072 Uiso 1 1 calc R . . H49B H 0.4314 0.0928 0.6930 0.072 Uiso 1 1 calc R . . C50 C 0.4539(5) 0.2353(2) 0.6812(3) 0.0464(17) Uani 1 1 d . . . H50A H 0.4282 0.2450 0.6456 0.070 Uiso 1 1 calc R . . H50C H 0.5240 0.2593 0.6814 0.070 Uiso 1 1 calc R . . H50B H 0.3802 0.2423 0.7095 0.070 Uiso 1 1 calc R . . C51 C 0.9427(5) 0.0679(2) 0.6730(2) 0.0305(13) Uani 1 1 d . . . H51 H 0.9187 0.0614 0.7136 0.037 Uiso 1 1 calc R . . C52 C 0.9391(5) 0.0097(2) 0.6559(3) 0.0404(15) Uani 1 1 d . . . H52B H 0.8531 -0.0053 0.6695 0.061 Uiso 1 1 calc R . . H52C H 1.0030 -0.0176 0.6712 0.061 Uiso 1 1 calc R . . H52A H 0.9589 0.0150 0.6161 0.061 Uiso 1 1 calc R . . C53 C 1.0792(5) 0.0881(2) 0.6568(2) 0.0387(15) Uani 1 1 d . . . H53A H 1.1086 0.0911 0.6175 0.058 Uiso 1 1 calc R . . H53C H 1.1361 0.0604 0.6762 0.058 Uiso 1 1 calc R . . H53B H 1.0811 0.1258 0.6663 0.058 Uiso 1 1 calc R . . C54 C 0.6411(4) 0.1128(2) 0.88493(19) 0.0198(11) Uani 1 1 d . . . C55 C 0.5338(4) 0.1493(2) 0.8998(2) 0.0241(12) Uani 1 1 d . . . C56 C 0.5336(5) 0.1773(2) 0.9428(2) 0.0304(13) Uani 1 1 d . . . H56 H 0.4622 0.2022 0.9535 0.036 Uiso 1 1 calc R . . C57 C 0.6345(5) 0.1693(2) 0.9697(2) 0.0320(13) Uani 1 1 d . . . H57 H 0.6326 0.1888 0.9987 0.038 Uiso 1 1 calc R . . C58 C 0.7384(5) 0.1335(2) 0.9550(2) 0.0290(13) Uani 1 1 d . . . H58 H 0.8080 0.1288 0.9740 0.035 Uiso 1 1 calc R . . C59 C 0.7442(4) 0.1038(2) 0.9128(2) 0.0220(12) Uani 1 1 d . . . C60 C 0.4186(5) 0.1575(3) 0.8715(2) 0.0360(15) Uani 1 1 d . . . H60 H 0.4450 0.1428 0.8368 0.043 Uiso 1 1 calc R . . C61 C 0.3092(6) 0.1226(3) 0.9066(3) 0.068(2) Uani 1 1 d . . . H61C H 0.2789 0.1374 0.9402 0.102 Uiso 1 1 calc R . . H61B H 0.3394 0.0822 0.9155 0.102 Uiso 1 1 calc R . . H61A H 0.2384 0.1254 0.8867 0.102 Uiso 1 1 calc R . . C62 C 0.3728(7) 0.2194(3) 0.8577(4) 0.092(3) Uani 1 1 d . . . H62A H 0.3064 0.2227 0.8355 0.138 Uiso 1 1 calc R . . H62B H 0.4453 0.2424 0.8373 0.138 Uiso 1 1 calc R . . H62C H 0.3367 0.2336 0.8913 0.138 Uiso 1 1 calc R . . C63 C 0.8568(5) 0.0622(2) 0.8996(2) 0.0267(13) Uani 1 1 d . . . H63 H 0.8649 0.0586 0.8607 0.032 Uiso 1 1 calc R . . C64 C 0.8306(5) 0.0028(2) 0.9353(2) 0.0391(15) Uani 1 1 d . . . H64C H 0.8237 0.0051 0.9735 0.059 Uiso 1 1 calc R . . H64B H 0.9013 -0.0246 0.9250 0.059 Uiso 1 1 calc R . . H64A H 0.7498 -0.0102 0.9301 0.059 Uiso 1 1 calc R . . C65 C 0.9847(5) 0.0810(2) 0.9064(2) 0.0364(14) Uani 1 1 d . . . H65A H 1.0000 0.1198 0.8851 0.055 Uiso 1 1 calc R . . H65B H 1.0542 0.0543 0.8935 0.055 Uiso 1 1 calc R . . H65C H 0.9823 0.0809 0.9449 0.055 Uiso 1 1 calc R . . C66 C 1.0891(5) 0.2540(2) 0.6642(2) 0.0332(14) Uani 1 1 d . . . H66A H 1.0356 0.2351 0.6467 0.050 Uiso 1 1 calc R . . H66C H 1.1740 0.2338 0.6626 0.050 Uiso 1 1 calc R . . H66B H 1.0989 0.2941 0.6453 0.050 Uiso 1 1 calc R . . Mn1' Mn 0.29796(7) 0.76136(3) 0.74730(3) 0.0234(2) Uani 1 1 d . . . Cl1' Cl 0.10640(13) 0.75211(7) 0.64220(6) 0.0440(4) Uani 1 1 d . . . Cl2' Cl -0.04536(13) 0.72900(7) 0.76664(7) 0.0465(4) Uani 1 1 d . . . Si1' Si 0.10277(13) 0.77787(7) 0.71619(6) 0.0280(4) Uani 1 1 d . . . O1' O 0.2919(3) 0.88853(17) 0.73616(15) 0.0374(10) Uani 1 1 d . . . O2' O 0.5434(4) 0.73889(17) 0.78947(16) 0.0418(10) Uani 1 1 d . . . O3' O 0.2515(4) 0.63839(18) 0.75262(16) 0.0460(11) Uani 1 1 d . . . N1' N 0.4304(3) 0.77851(16) 0.62762(17) 0.0174(9) Uani 1 1 d . . . N2' N 0.1532(3) 0.75885(16) 0.86396(17) 0.0180(9) Uani 1 1 d . . . C1' C 0.3813(4) 0.7700(2) 0.6739(2) 0.0218(12) Uani 1 1 d . . . C2' C 0.2042(5) 0.7586(2) 0.8191(2) 0.0227(12) Uani 1 1 d . . . C3' C 0.2952(5) 0.8390(3) 0.7406(2) 0.0271(13) Uani 1 1 d . . . C4' C 0.4485(5) 0.7477(2) 0.7725(2) 0.0261(12) Uani 1 1 d . . . C5' C 0.2728(5) 0.6852(3) 0.7507(2) 0.0283(13) Uani 1 1 d . . . C6' C 0.1013(4) 0.7634(2) 0.91825(19) 0.0198(11) Uani 1 1 d . . . C7' C 0.0416(4) 0.8158(2) 0.92908(19) 0.0178(11) Uani 1 1 d . . . C8' C -0.0064(4) 0.8184(2) 0.9831(2) 0.0237(12) Uani 1 1 d . . . H8' H -0.0471 0.8533 0.9921 0.028 Uiso 1 1 calc R . . C9' C 0.0035(5) 0.7714(2) 1.0244(2) 0.0252(12) Uani 1 1 d . . . H9' H -0.0303 0.7742 1.0612 0.030 Uiso 1 1 calc R . . C10' C 0.0625(4) 0.7206(2) 1.0121(2) 0.0261(12) Uani 1 1 d . . . H10A H 0.0686 0.6886 1.0408 0.031 Uiso 1 1 calc R . . C11' C 0.1129(4) 0.7147(2) 0.95918(19) 0.0193(11) Uani 1 1 d . . . C12' C 0.0345(4) 0.8674(2) 0.88477(18) 0.0173(11) Uani 1 1 d . . . C13' C 0.1346(4) 0.9055(2) 0.86982(19) 0.0195(11) Uani 1 1 d . . . C14' C 0.1257(5) 0.9542(2) 0.8293(2) 0.0264(12) Uani 1 1 d . . . H14A H 0.1932 0.9802 0.8184 0.032 Uiso 1 1 calc R . . C15' C 0.0188(5) 0.9644(2) 0.8052(2) 0.0258(12) Uani 1 1 d . . . H15A H 0.0136 0.9976 0.7777 0.031 Uiso 1 1 calc R . . C16' C -0.0804(5) 0.9274(2) 0.8203(2) 0.0261(13) Uani 1 1 d . . . H16A H -0.1537 0.9357 0.8035 0.031 Uiso 1 1 calc R . . C17' C -0.0741(4) 0.8779(2) 0.8600(2) 0.0226(12) Uani 1 1 d . . . C18' C -0.1858(4) 0.8386(2) 0.8776(2) 0.0236(12) Uani 1 1 d . . . H18A H -0.1507 0.7993 0.8921 0.028 Uiso 1 1 calc R . . C19' C -0.2853(5) 0.8575(3) 0.9236(2) 0.0372(15) Uani 1 1 d . . . H19E H -0.3216 0.8960 0.9106 0.056 Uiso 1 1 calc R . . H19F H -0.2441 0.8583 0.9543 0.056 Uiso 1 1 calc R . . H19D H -0.3543 0.8303 0.9352 0.056 Uiso 1 1 calc R . . C20' C -0.2538(5) 0.8334(3) 0.8314(2) 0.0362(15) Uani 1 1 d . . . H20F H -0.2951 0.8707 0.8182 0.054 Uiso 1 1 calc R . . H20E H -0.3192 0.8047 0.8450 0.054 Uiso 1 1 calc R . . H20D H -0.1906 0.8216 0.8016 0.054 Uiso 1 1 calc R . . C21' C 0.2520(4) 0.8957(2) 0.8968(2) 0.0238(12) Uani 1 1 d . . . H21A H 0.2304 0.8665 0.9311 0.029 Uiso 1 1 calc R . . C22' C 0.2862(5) 0.9505(2) 0.9125(2) 0.0325(14) Uani 1 1 d . . . H22E H 0.3583 0.9416 0.9319 0.049 Uiso 1 1 calc R . . H22F H 0.2115 0.9652 0.9361 0.049 Uiso 1 1 calc R . . H22D H 0.3107 0.9796 0.8796 0.049 Uiso 1 1 calc R . . C23' C 0.3688(5) 0.8713(2) 0.8612(2) 0.0364(15) Uani 1 1 d . . . H23D H 0.3494 0.8339 0.8550 0.055 Uiso 1 1 calc R . . H23F H 0.4427 0.8663 0.8796 0.055 Uiso 1 1 calc R . . H23E H 0.3893 0.8979 0.8262 0.055 Uiso 1 1 calc R . . C24' C 0.1796(5) 0.6593(2) 0.9470(2) 0.0241(12) Uani 1 1 d . . . C25' C 0.1125(5) 0.6208(2) 0.9288(2) 0.0286(13) Uani 1 1 d . . . C26' C 0.1740(5) 0.5684(2) 0.9213(2) 0.0375(15) Uani 1 1 d . . . H26A H 0.1293 0.5412 0.9106 0.045 Uiso 1 1 calc R . . C27' C 0.2986(5) 0.5547(2) 0.9290(2) 0.0376(15) Uani 1 1 d . . . H27A H 0.3397 0.5190 0.9226 0.045 Uiso 1 1 calc R . . C28' C 0.3634(5) 0.5931(2) 0.9461(2) 0.0354(14) Uani 1 1 d . . . H28A H 0.4485 0.5832 0.9523 0.042 Uiso 1 1 calc R . . C29' C 0.3059(5) 0.6463(2) 0.9545(2) 0.0290(13) Uani 1 1 d . . . C30' C -0.0256(5) 0.6346(3) 0.9203(2) 0.0335(14) Uani 1 1 d . . . H30A H -0.0381 0.6774 0.9106 0.040 Uiso 1 1 calc R . . C31' C -0.1207(5) 0.6141(3) 0.9718(2) 0.0518(18) Uani 1 1 d . . . H31E H -0.2085 0.6230 0.9650 0.078 Uiso 1 1 calc R . . H31F H -0.1079 0.6336 1.0004 0.078 Uiso 1 1 calc R . . H31D H -0.1074 0.5725 0.9834 0.078 Uiso 1 1 calc R . . C32' C -0.0518(6) 0.6096(3) 0.8731(2) 0.0489(17) Uani 1 1 d . . . H32E H 0.0156 0.6204 0.8410 0.073 Uiso 1 1 calc R . . H32F H -0.1357 0.6247 0.8647 0.073 Uiso 1 1 calc R . . H32D H -0.0520 0.5675 0.8835 0.073 Uiso 1 1 calc R . . C33' C 0.3801(5) 0.6864(2) 0.9745(2) 0.0376(15) Uani 1 1 d . . . H33A H 0.3241 0.7221 0.9777 0.045 Uiso 1 1 calc R . . C34' C 0.4109(7) 0.6615(3) 1.0305(3) 0.0564(19) Uani 1 1 d . . . H34E H 0.3308 0.6520 1.0565 0.085 Uiso 1 1 calc R . . H34F H 0.4547 0.6898 1.0423 0.085 Uiso 1 1 calc R . . H34D H 0.4669 0.6266 1.0287 0.085 Uiso 1 1 calc R . . C35' C 0.5032(6) 0.7043(3) 0.9342(3) 0.060(2) Uani 1 1 d . . . H35E H 0.5603 0.6702 0.9299 0.090 Uiso 1 1 calc R . . H35F H 0.5465 0.7313 0.9479 0.090 Uiso 1 1 calc R . . H35D H 0.4819 0.7228 0.8989 0.090 Uiso 1 1 calc R . . C36' C 0.5019(4) 0.7883(2) 0.57452(19) 0.0192(11) Uani 1 1 d . . . C37' C 0.5284(4) 0.8453(2) 0.54917(19) 0.0179(11) Uani 1 1 d . . . C38' C 0.6048(5) 0.8540(2) 0.4974(2) 0.0262(12) Uani 1 1 d . . . H38A H 0.6249 0.8918 0.4786 0.031 Uiso 1 1 calc R . . C39' C 0.6517(5) 0.8071(2) 0.4730(2) 0.0284(13) Uani 1 1 d . . . H39A H 0.7041 0.8134 0.4377 0.034 Uiso 1 1 calc R . . C40' C 0.6234(4) 0.7515(2) 0.4994(2) 0.0222(12) Uani 1 1 d . . . H40A H 0.6567 0.7203 0.4819 0.027 Uiso 1 1 calc R . . C41' C 0.5476(4) 0.7407(2) 0.55079(19) 0.0174(11) Uani 1 1 d . . . C42' C 0.4788(4) 0.8941(2) 0.5774(2) 0.0211(11) Uani 1 1 d . . . C43' C 0.5418(5) 0.9062(2) 0.6168(2) 0.0270(13) Uani 1 1 d . . . C44' C 0.4966(5) 0.9530(2) 0.6408(2) 0.0341(14) Uani 1 1 d . . . H44A H 0.5385 0.9620 0.6673 0.041 Uiso 1 1 calc R . . C45' C 0.3917(5) 0.9870(2) 0.6268(2) 0.0377(15) Uani 1 1 d . . . H45A H 0.3631 1.0194 0.6431 0.045 Uiso 1 1 calc R . . C46' C 0.3283(5) 0.9742(2) 0.5894(2) 0.0367(15) Uani 1 1 d . . . H46A H 0.2549 0.9973 0.5808 0.044 Uiso 1 1 calc R . . C47' C 0.3701(5) 0.9278(2) 0.5639(2) 0.0290(13) Uani 1 1 d . . . C48' C 0.6578(5) 0.8684(2) 0.6323(2) 0.0324(14) Uani 1 1 d . . . H48A H 0.6470 0.8288 0.6268 0.039 Uiso 1 1 calc R . . C49' C 0.7830(5) 0.8893(3) 0.5960(2) 0.0422(16) Uani 1 1 d . . . H49D H 0.7765 0.8929 0.5578 0.063 Uiso 1 1 calc R . . H49E H 0.8538 0.8616 0.6042 0.063 Uiso 1 1 calc R . . H49F H 0.7998 0.9268 0.6026 0.063 Uiso 1 1 calc R . . C50' C 0.6658(5) 0.8639(3) 0.6923(2) 0.0432(16) Uani 1 1 d . . . H50F H 0.6900 0.9008 0.6976 0.065 Uiso 1 1 calc R . . H50D H 0.7306 0.8338 0.7023 0.065 Uiso 1 1 calc R . . H50E H 0.5818 0.8543 0.7152 0.065 Uiso 1 1 calc R . . C51' C 0.2982(5) 0.9143(2) 0.5226(2) 0.0289(13) Uani 1 1 d . . . H51A H 0.3367 0.8773 0.5122 0.035 Uiso 1 1 calc R . . C52' C 0.3161(9) 0.9607(4) 0.4715(3) 0.113(4) Uani 1 1 d . . . H52D H 0.2802 0.9486 0.4434 0.169 Uiso 1 1 calc R . . H52E H 0.4081 0.9667 0.4584 0.169 Uiso 1 1 calc R . . H52F H 0.2717 0.9966 0.4798 0.169 Uiso 1 1 calc R . . C53' C 0.1570(5) 0.9065(3) 0.5453(3) 0.064(2) Uani 1 1 d . . . H53F H 0.1177 0.9415 0.5577 0.096 Uiso 1 1 calc R . . H53E H 0.1469 0.8739 0.5760 0.096 Uiso 1 1 calc R . . H53D H 0.1147 0.8991 0.5169 0.096 Uiso 1 1 calc R . . C54' C 0.5138(4) 0.6823(2) 0.5825(2) 0.0221(12) Uani 1 1 d . . . C55' C 0.4117(4) 0.6553(2) 0.5727(2) 0.0231(12) Uani 1 1 d . . . C56' C 0.3731(5) 0.6043(2) 0.6076(2) 0.0311(14) Uani 1 1 d . . . H56A H 0.3019 0.5859 0.6026 0.037 Uiso 1 1 calc R . . C57' C 0.4364(5) 0.5800(2) 0.6493(2) 0.0370(14) Uani 1 1 d . . . H57A H 0.4081 0.5452 0.6728 0.044 Uiso 1 1 calc R . . C58' C 0.5397(5) 0.6054(2) 0.6573(2) 0.0332(14) Uani 1 1 d . . . H58A H 0.5835 0.5877 0.6858 0.040 Uiso 1 1 calc R . . C59' C 0.5813(5) 0.6571(2) 0.6240(2) 0.0256(12) Uani 1 1 d . . . C60' C 0.3441(4) 0.6807(2) 0.5250(2) 0.0271(13) Uani 1 1 d . . . H60A H 0.3534 0.7233 0.5165 0.033 Uiso 1 1 calc R . . C61' C 0.4108(5) 0.6567(3) 0.4748(2) 0.0364(15) Uani 1 1 d . . . H61D H 0.4096 0.6146 0.4831 0.055 Uiso 1 1 calc R . . H61F H 0.5001 0.6682 0.4643 0.055 Uiso 1 1 calc R . . H61E H 0.3655 0.6718 0.4447 0.055 Uiso 1 1 calc R . . C62' C 0.2014(5) 0.6701(3) 0.5365(2) 0.0369(15) Uani 1 1 d . . . H62E H 0.1619 0.6925 0.5068 0.055 Uiso 1 1 calc R . . H62F H 0.1602 0.6818 0.5708 0.055 Uiso 1 1 calc R . . H62D H 0.1900 0.6290 0.5394 0.055 Uiso 1 1 calc R . . C63' C 0.6987(5) 0.6841(2) 0.6315(2) 0.0322(14) Uani 1 1 d . . . H63A H 0.6824 0.7268 0.6229 0.039 Uiso 1 1 calc R . . C64' C 0.8178(5) 0.6692(3) 0.5908(2) 0.0393(15) Uani 1 1 d . . . H64E H 0.8365 0.6275 0.5979 0.059 Uiso 1 1 calc R . . H64F H 0.8916 0.6888 0.5948 0.059 Uiso 1 1 calc R . . H64D H 0.8015 0.6817 0.5537 0.059 Uiso 1 1 calc R . . C65' C 0.7273(5) 0.6690(3) 0.6892(2) 0.0462(17) Uani 1 1 d . . . H65E H 0.6487 0.6752 0.7154 0.069 Uiso 1 1 calc R . . H65F H 0.7937 0.6936 0.6922 0.069 Uiso 1 1 calc R . . H65D H 0.7579 0.6286 0.6969 0.069 Uiso 1 1 calc R . . C66' C 0.0323(5) 0.8525(2) 0.7046(2) 0.0334(14) Uani 1 1 d . . . H66E H 0.0934 0.8773 0.6778 0.050 Uiso 1 1 calc R . . H66F H 0.0138 0.8665 0.7390 0.050 Uiso 1 1 calc R . . H66D H -0.0477 0.8531 0.6910 0.050 Uiso 1 1 calc R . . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 Mn1 0.0282(4) 0.0189(5) 0.0235(5) -0.0058(4) -0.0050(4) -0.0049(3) Cl1 0.0328(7) 0.0419(9) 0.0398(9) -0.0116(7) -0.0121(7) -0.0033(6) Cl2 0.0418(8) 0.0280(9) 0.0471(10) -0.0002(7) -0.0068(7) 0.0044(6) Si1 0.0288(8) 0.0233(9) 0.0248(9) -0.0049(7) -0.0057(7) -0.0024(6) O1 0.049(2) 0.032(3) 0.030(2) -0.0042(19) -0.012(2) -0.0081(18) O2 0.034(2) 0.032(3) 0.079(4) -0.012(2) 0.000(2) 0.001(2) O3 0.068(3) 0.049(3) 0.021(2) -0.004(2) -0.014(2) -0.017(2) N1 0.022(2) 0.017(3) 0.020(2) -0.0012(19) -0.0052(18) -0.0038(19) N2 0.025(2) 0.023(3) 0.012(2) -0.004(2) -0.0070(18) -0.0023(19) C1 0.020(3) 0.027(3) 0.016(3) -0.003(2) -0.004(2) -0.003(2) C2 0.031(3) 0.018(3) 0.022(3) -0.005(2) -0.008(2) -0.001(2) C3 0.027(3) 0.017(3) 0.031(3) -0.006(3) -0.007(3) -0.003(2) C4 0.031(3) 0.023(3) 0.033(4) -0.007(3) 0.002(3) -0.012(3) C5 0.033(3) 0.031(4) 0.044(4) -0.018(3) -0.010(3) -0.005(3) C6 0.015(2) 0.017(3) 0.025(3) -0.004(2) -0.003(2) -0.001(2) C7 0.019(2) 0.021(3) 0.014(3) -0.003(2) -0.008(2) -0.003(2) C8 0.026(3) 0.018(3) 0.018(3) 0.000(2) -0.004(2) -0.007(2) C9 0.023(3) 0.017(3) 0.027(3) -0.001(2) -0.005(2) -0.004(2) C10 0.022(3) 0.018(3) 0.026(3) -0.010(2) -0.004(2) -0.003(2) C11 0.016(2) 0.022(3) 0.017(3) -0.004(2) -0.003(2) -0.002(2) C12 0.029(3) 0.017(3) 0.017(3) 0.000(2) -0.006(2) -0.004(2) C13 0.022(3) 0.024(3) 0.018(3) -0.001(2) -0.002(2) -0.002(2) C14 0.038(3) 0.030(3) 0.024(3) -0.007(3) -0.013(3) -0.009(3) C15 0.034(3) 0.033(3) 0.018(3) -0.013(3) 0.000(2) -0.002(3) C16 0.027(3) 0.023(3) 0.036(4) -0.008(3) -0.004(3) -0.001(2) C17 0.025(3) 0.024(3) 0.012(3) 0.000(2) -0.005(2) -0.005(2) C18 0.027(3) 0.031(3) 0.025(3) -0.011(3) -0.009(2) 0.000(2) C19 0.052(4) 0.036(4) 0.031(4) -0.001(3) -0.006(3) 0.007(3) C20 0.026(3) 0.036(4) 0.047(4) 0.003(3) -0.002(3) 0.002(3) C21 0.025(3) 0.036(4) 0.025(3) -0.013(3) -0.009(2) 0.006(2) C22 0.028(3) 0.025(3) 0.033(3) 0.000(3) -0.012(3) -0.001(2) C23 0.031(3) 0.043(4) 0.039(4) 0.001(3) -0.013(3) -0.003(3) C24 0.022(3) 0.023(3) 0.023(3) -0.014(2) -0.001(2) -0.006(2) C25 0.028(3) 0.030(3) 0.030(3) -0.016(3) -0.002(2) -0.008(2) C26 0.045(3) 0.034(4) 0.029(4) -0.010(3) 0.007(3) -0.012(3) C27 0.065(4) 0.028(4) 0.022(3) -0.001(3) 0.001(3) -0.012(3) C28 0.055(4) 0.022(3) 0.022(3) -0.003(3) -0.018(3) 0.001(3) C29 0.038(3) 0.020(3) 0.022(3) -0.008(2) -0.008(3) -0.005(2) C30 0.020(3) 0.044(4) 0.033(4) -0.016(3) 0.003(2) -0.006(2) C31 0.061(4) 0.066(5) 0.048(4) -0.022(4) -0.013(4) 0.024(4) C32 0.058(4) 0.062(5) 0.141(8) -0.022(5) -0.053(5) -0.007(4) C33 0.039(3) 0.029(3) 0.027(3) -0.009(3) -0.014(3) 0.000(3) C34 0.028(3) 0.048(4) 0.048(4) -0.016(3) -0.009(3) -0.005(3) C35 0.060(4) 0.044(4) 0.037(4) -0.010(3) -0.020(3) 0.013(3) C36 0.016(2) 0.018(3) 0.029(3) -0.007(2) -0.006(2) 0.001(2) C37 0.019(2) 0.018(3) 0.019(3) -0.003(2) -0.006(2) 0.000(2) C38 0.038(3) 0.024(3) 0.030(3) -0.013(3) -0.017(3) 0.001(2) C39 0.027(3) 0.019(3) 0.033(3) -0.002(3) -0.008(3) -0.006(2) C40 0.028(3) 0.022(3) 0.028(3) -0.002(3) -0.007(2) -0.002(2) C41 0.017(2) 0.023(3) 0.021(3) -0.003(2) -0.005(2) -0.001(2) C42 0.030(3) 0.021(3) 0.020(3) -0.007(2) -0.009(2) 0.003(2) C43 0.032(3) 0.028(3) 0.024(3) -0.008(3) -0.011(3) 0.002(2) C44 0.044(3) 0.030(4) 0.029(4) -0.010(3) -0.019(3) 0.008(3) C45 0.058(4) 0.038(4) 0.022(3) -0.004(3) -0.010(3) 0.001(3) C46 0.044(3) 0.031(4) 0.026(3) -0.011(3) -0.002(3) 0.009(3) C47 0.037(3) 0.020(3) 0.025(3) -0.008(3) -0.014(3) 0.005(2) C48 0.034(3) 0.031(4) 0.038(4) -0.008(3) -0.019(3) 0.001(3) C49 0.037(3) 0.054(5) 0.058(5) -0.016(4) -0.017(3) -0.004(3) C50 0.034(3) 0.034(4) 0.070(5) -0.014(3) -0.011(3) 0.012(3) C51 0.028(3) 0.031(4) 0.033(3) -0.012(3) -0.003(3) 0.004(2) C52 0.044(3) 0.024(4) 0.053(4) -0.008(3) -0.012(3) 0.008(3) C53 0.042(3) 0.037(4) 0.040(4) -0.016(3) -0.013(3) 0.013(3) C54 0.028(3) 0.012(3) 0.018(3) 0.003(2) -0.002(2) -0.011(2) C55 0.022(3) 0.031(3) 0.016(3) 0.000(2) 0.000(2) -0.003(2) C56 0.035(3) 0.031(4) 0.024(3) -0.006(3) -0.006(3) 0.005(3) C57 0.050(3) 0.025(3) 0.022(3) -0.010(3) -0.005(3) 0.002(3) C58 0.035(3) 0.027(3) 0.026(3) -0.004(3) -0.010(3) -0.005(3) C59 0.025(3) 0.022(3) 0.018(3) -0.002(2) -0.002(2) -0.008(2) C60 0.033(3) 0.044(4) 0.031(4) -0.012(3) -0.007(3) 0.010(3) C61 0.051(4) 0.077(6) 0.083(6) -0.007(5) -0.028(4) -0.028(4) C62 0.074(5) 0.053(6) 0.147(9) 0.029(5) -0.068(6) -0.002(4) C63 0.034(3) 0.026(3) 0.023(3) -0.005(3) -0.012(2) 0.003(2) C64 0.049(4) 0.034(4) 0.038(4) -0.013(3) -0.014(3) 0.011(3) C65 0.035(3) 0.042(4) 0.037(4) -0.012(3) -0.011(3) -0.003(3) C66 0.033(3) 0.030(4) 0.038(4) -0.011(3) -0.009(3) 0.004(3) Mn1' 0.0306(4) 0.0219(5) 0.0174(4) -0.0060(4) -0.0014(3) -0.0016(3) Cl1' 0.0455(8) 0.0585(11) 0.0390(9) -0.0287(8) -0.0154(7) 0.0011(7) Cl2' 0.0351(8) 0.0477(11) 0.0548(11) -0.0060(8) -0.0033(7) -0.0136(7) Si1' 0.0297(8) 0.0328(10) 0.0244(9) -0.0118(7) -0.0052(7) -0.0020(7) O1' 0.049(2) 0.032(3) 0.030(2) -0.008(2) -0.0006(19) -0.005(2) O2' 0.037(2) 0.053(3) 0.036(3) -0.012(2) -0.011(2) 0.007(2) O3' 0.065(3) 0.025(3) 0.044(3) -0.009(2) 0.005(2) -0.010(2) N1' 0.022(2) 0.016(2) 0.015(3) -0.0023(19) -0.0052(19) 0.0010(17) N2' 0.020(2) 0.016(2) 0.018(3) -0.0015(19) -0.0042(19) -0.0055(17) C1' 0.026(3) 0.013(3) 0.029(3) -0.008(2) -0.008(3) 0.001(2) C2' 0.031(3) 0.016(3) 0.019(3) 0.002(2) -0.004(2) -0.002(2) C3' 0.032(3) 0.031(4) 0.020(3) -0.013(3) 0.000(2) -0.006(3) C4' 0.034(3) 0.027(3) 0.015(3) -0.004(2) 0.003(2) -0.003(2) C5' 0.038(3) 0.029(4) 0.016(3) -0.004(3) 0.001(2) 0.000(3) C6' 0.023(3) 0.021(3) 0.017(3) -0.005(2) -0.003(2) -0.009(2) C7' 0.020(2) 0.017(3) 0.017(3) 0.001(2) -0.007(2) -0.006(2) C8' 0.025(3) 0.026(3) 0.021(3) -0.009(3) -0.003(2) -0.002(2) C9' 0.032(3) 0.031(3) 0.014(3) -0.004(3) -0.004(2) -0.007(2) C10' 0.031(3) 0.027(3) 0.021(3) -0.005(3) -0.006(2) -0.004(2) C11' 0.025(3) 0.022(3) 0.012(3) 0.000(2) -0.006(2) -0.005(2) C12' 0.028(3) 0.012(3) 0.011(3) -0.002(2) -0.002(2) 0.000(2) C13' 0.027(3) 0.018(3) 0.013(3) -0.003(2) -0.002(2) -0.003(2) C14' 0.026(3) 0.026(3) 0.025(3) -0.003(3) 0.001(2) -0.004(2) C15' 0.037(3) 0.023(3) 0.018(3) -0.003(2) -0.010(2) 0.006(2) C16' 0.031(3) 0.026(3) 0.027(3) -0.012(3) -0.012(2) 0.004(2) C17' 0.028(3) 0.024(3) 0.019(3) -0.008(2) -0.007(2) 0.002(2) C18' 0.026(3) 0.021(3) 0.025(3) 0.000(2) -0.010(2) -0.004(2) C19' 0.031(3) 0.050(4) 0.030(4) -0.010(3) 0.004(3) -0.018(3) C20' 0.027(3) 0.053(4) 0.034(4) -0.018(3) -0.008(3) -0.007(3) C21' 0.026(3) 0.017(3) 0.029(3) 0.000(2) -0.011(2) -0.006(2) C22' 0.037(3) 0.030(3) 0.035(4) -0.010(3) -0.011(3) -0.009(3) C23' 0.028(3) 0.036(4) 0.051(4) -0.018(3) -0.012(3) -0.001(3) C24' 0.037(3) 0.015(3) 0.021(3) -0.001(2) -0.007(2) -0.005(2) C25' 0.038(3) 0.028(3) 0.019(3) -0.003(3) -0.006(2) -0.001(3) C26' 0.053(4) 0.031(4) 0.030(4) -0.008(3) -0.005(3) -0.014(3) C27' 0.050(4) 0.029(4) 0.030(4) -0.011(3) 0.003(3) 0.005(3) C28' 0.034(3) 0.035(4) 0.033(4) -0.008(3) 0.006(3) -0.002(3) C29' 0.035(3) 0.022(3) 0.026(3) 0.001(3) -0.004(3) 0.000(2) C30' 0.045(3) 0.035(4) 0.025(3) -0.008(3) -0.008(3) -0.011(3) C31' 0.042(4) 0.075(5) 0.039(4) -0.007(4) -0.017(3) 0.001(3) C32' 0.068(4) 0.044(4) 0.044(4) -0.009(3) -0.023(3) -0.019(3) C33' 0.030(3) 0.033(4) 0.053(4) -0.017(3) -0.005(3) -0.001(3) C34' 0.077(5) 0.054(5) 0.047(4) -0.012(4) -0.021(4) -0.023(4) C35' 0.058(4) 0.066(5) 0.049(5) 0.005(4) -0.004(4) -0.029(4) C36' 0.019(2) 0.030(3) 0.010(3) -0.004(2) -0.006(2) -0.002(2) C37' 0.023(3) 0.016(3) 0.014(3) 0.004(2) -0.006(2) -0.006(2) C38' 0.031(3) 0.024(3) 0.021(3) 0.000(2) -0.003(2) -0.005(2) C39' 0.027(3) 0.036(4) 0.020(3) -0.006(3) -0.001(2) -0.001(2) C40' 0.026(3) 0.016(3) 0.024(3) -0.003(2) -0.005(2) 0.000(2) C41' 0.020(2) 0.019(3) 0.015(3) -0.005(2) -0.005(2) -0.005(2) C42' 0.022(3) 0.019(3) 0.020(3) -0.001(2) 0.002(2) -0.006(2) C43' 0.032(3) 0.020(3) 0.029(3) -0.004(3) -0.005(3) -0.008(2) C44' 0.051(4) 0.021(3) 0.035(4) -0.007(3) -0.012(3) -0.011(3) C45' 0.045(3) 0.025(4) 0.042(4) -0.013(3) 0.003(3) -0.003(3) C46' 0.038(3) 0.019(3) 0.053(4) -0.009(3) -0.009(3) 0.006(3) C47' 0.032(3) 0.023(3) 0.031(3) -0.004(3) -0.007(3) 0.000(2) C48' 0.034(3) 0.030(3) 0.040(4) -0.014(3) -0.014(3) -0.008(3) C49' 0.035(3) 0.057(4) 0.040(4) -0.018(3) -0.012(3) -0.002(3) C50' 0.044(3) 0.055(4) 0.033(4) -0.001(3) -0.013(3) -0.015(3) C51' 0.028(3) 0.028(3) 0.030(3) -0.001(3) -0.007(2) 0.001(2) C52' 0.144(8) 0.140(9) 0.057(6) 0.064(6) -0.070(6) -0.098(7) C53' 0.041(4) 0.104(6) 0.061(5) -0.047(5) -0.003(3) -0.020(4) C54' 0.021(3) 0.022(3) 0.025(3) -0.010(2) -0.004(2) 0.003(2) C55' 0.025(3) 0.013(3) 0.029(3) -0.005(2) 0.003(2) 0.000(2) C56' 0.029(3) 0.026(4) 0.040(4) -0.015(3) -0.004(3) 0.000(2) C57' 0.045(3) 0.019(3) 0.037(4) 0.000(3) 0.008(3) 0.003(3) C58' 0.042(3) 0.024(4) 0.031(4) -0.003(3) -0.009(3) 0.009(3) C59' 0.029(3) 0.022(3) 0.029(3) -0.014(3) -0.004(2) 0.005(2) C60' 0.029(3) 0.026(3) 0.030(3) -0.012(3) -0.003(2) -0.007(2) C61' 0.034(3) 0.049(4) 0.029(3) -0.016(3) -0.002(3) -0.006(3) C62' 0.031(3) 0.051(4) 0.035(4) -0.018(3) -0.008(3) -0.008(3) C63' 0.038(3) 0.026(3) 0.036(4) -0.009(3) -0.015(3) 0.007(3) C64' 0.028(3) 0.047(4) 0.047(4) -0.015(3) -0.010(3) 0.000(3) C65' 0.046(4) 0.058(5) 0.040(4) -0.020(3) -0.020(3) 0.020(3) C66' 0.032(3) 0.036(4) 0.034(4) -0.008(3) -0.010(3) -0.002(3) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag Mn1 C4 1.821(6) . ? Mn1 C3 1.847(6) . ? Mn1 C5 1.853(6) . ? Mn1 C2 1.875(5) . ? Mn1 C1 1.900(5) . ? Mn1 Si1 2.3458(17) . ? Cl1 Si1 2.0903(19) . ? Cl2 Si1 2.105(2) . ? Si1 C66 1.860(5) . ? O1 C3 1.134(6) . ? O2 C4 1.160(6) . ? O3 C5 1.138(6) . ? N1 C1 1.165(6) . ? N1 C6 1.404(6) . ? N2 C2 1.169(6) . ? N2 C36 1.390(6) . ? C6 C7 1.397(6) . ? C6 C11 1.404(6) . ? C7 C8 1.400(6) . ? C7 C12 1.502(6) . ? C8 C9 1.387(6) . ? C8 H8 0.9500 . ? C9 C10 1.381(7) . ? C9 H9 0.9500 . ? C10 C11 1.394(7) . ? C10 H10 0.9500 . ? C11 C24 1.494(7) . ? C12 C13 1.396(6) . ? C12 C17 1.409(6) . ? C13 C14 1.395(7) . ? C13 C18 1.512(6) . ? C14 C15 1.379(7) . ? C14 H14 0.9500 . ? C15 C16 1.380(6) . ? C15 H15 0.9500 . ? C16 C17 1.395(7) . ? C16 H16 0.9500 . ? C17 C21 1.525(6) . ? C18 C20 1.518(7) . ? C18 C19 1.527(7) . ? C18 H18 1.0000 . ? C19 H19A 0.9800 . ? C19 H19C 0.9800 . ? C19 H19B 0.9800 . ? C20 H20B 0.9800 . ? C20 H20C 0.9800 . ? C20 H20A 0.9800 . ? C21 C22 1.520(7) . ? C21 C23 1.523(7) . ? C21 H21 1.0000 . ? C22 H22A 0.9800 . ? C22 H22C 0.9800 . ? C22 H22B 0.9800 . ? C23 H23B 0.9800 . ? C23 H23C 0.9800 . ? C23 H23A 0.9800 . ? C24 C25 1.396(7) . ? C24 C29 1.411(7) . ? C25 C26 1.394(7) . ? C25 C30 1.522(7) . ? C26 C27 1.376(8) . ? C26 H26 0.9500 . ? C27 C28 1.368(8) . ? C27 H27 0.9500 . ? C28 C29 1.391(7) . ? C28 H28 0.9500 . ? C29 C33 1.525(7) . ? C30 C31 1.512(7) . ? C30 C32 1.539(8) . ? C30 H30 1.0000 . ? C31 H31A 0.9800 . ? C31 H31C 0.9800 . ? C31 H31B 0.9800 . ? C32 H32A 0.9800 . ? C32 H32B 0.9800 . ? C32 H32C 0.9800 . ? C33 C34 1.511(7) . ? C33 C35 1.531(7) . ? C33 H33 1.0000 . ? C34 H34A 0.9800 . ? C34 H34B 0.9800 . ? C34 H34C 0.9800 . ? C35 H35C 0.9800 . ? C35 H35B 0.9800 . ? C35 H35A 0.9800 . ? C36 C37 1.409(6) . ? C36 C41 1.413(7) . ? C37 C38 1.380(7) . ? C37 C42 1.506(7) . ? C38 C39 1.379(7) . ? C38 H38 0.9500 . ? C39 C40 1.404(7) . ? C39 H39 0.9500 . ? C40 C41 1.388(7) . ? C40 H40 0.9500 . ? C41 C54 1.501(6) . ? C42 C47 1.399(7) . ? C42 C43 1.407(7) . ? C43 C44 1.386(7) . ? C43 C48 1.515(7) . ? C44 C45 1.389(8) . ? C44 H44 0.9500 . ? C45 C46 1.367(7) . ? C45 H45 0.9500 . ? C46 C47 1.404(7) . ? C46 H46 0.9500 . ? C47 C51 1.513(7) . ? C48 C50 1.524(7) . ? C48 C49 1.531(7) . ? C48 H48 1.0000 . ? C49 H49A 0.9800 . ? C49 H49C 0.9800 . ? C49 H49B 0.9800 . ? C50 H50A 0.9800 . ? C50 H50C 0.9800 . ? C50 H50B 0.9800 . ? C51 C53 1.518(7) . ? C51 C52 1.541(7) . ? C51 H51 1.0000 . ? C52 H52B 0.9800 . ? C52 H52C 0.9800 . ? C52 H52A 0.9800 . ? C53 H53A 0.9800 . ? C53 H53C 0.9800 . ? C53 H53B 0.9800 . ? C54 C59 1.403(6) . ? C54 C55 1.407(7) . ? C55 C56 1.397(7) . ? C55 C60 1.523(7) . ? C56 C57 1.367(7) . ? C56 H56 0.9500 . ? C57 C58 1.371(7) . ? C57 H57 0.9500 . ? C58 C59 1.397(7) . ? C58 H58 0.9500 . ? C59 C63 1.511(7) . ? C60 C62 1.502(8) . ? C60 C61 1.513(8) . ? C60 H60 1.0000 . ? C61 H61C 0.9800 . ? C61 H61B 0.9800 . ? C61 H61A 0.9800 . ? C62 H62A 0.9800 . ? C62 H62B 0.9800 . ? C62 H62C 0.9800 . ? C63 C65 1.521(7) . ? C63 C64 1.530(7) . ? C63 H63 1.0000 . ? C64 H64C 0.9800 . ? C64 H64B 0.9800 . ? C64 H64A 0.9800 . ? C65 H65A 0.9800 . ? C65 H65B 0.9800 . ? C65 H65C 0.9800 . ? C66 H66A 0.9800 . ? C66 H66C 0.9800 . ? C66 H66B 0.9800 . ? Mn1' C3' 1.818(6) . ? Mn1' C4' 1.822(5) . ? Mn1' C5' 1.837(6) . ? Mn1' C1' 1.883(6) . ? Mn1' C2' 1.893(5) . ? Mn1' Si1' 2.3421(17) . ? Cl1' Si1' 2.098(2) . ? Cl2' Si1' 2.092(2) . ? Si1' C66' 1.853(5) . ? O1' C3' 1.158(6) . ? O2' C4' 1.162(6) . ? O3' C5' 1.145(6) . ? N1' C1' 1.177(6) . ? N1' C36' 1.399(6) . ? N2' C2' 1.167(6) . ? N2' C6' 1.408(6) . ? C6' C7' 1.402(6) . ? C6' C11' 1.407(7) . ? C7' C8' 1.385(6) . ? C7' C12' 1.496(7) . ? C8' C9' 1.384(7) . ? C8' H8' 0.9500 . ? C9' C10' 1.377(7) . ? C9' H9' 0.9500 . ? C10' C11' 1.381(7) . ? C10' H10A 0.9500 . ? C11' C24' 1.498(7) . ? C12' C13' 1.401(6) . ? C12' C17' 1.405(6) . ? C13' C14' 1.396(7) . ? C13' C21' 1.523(6) . ? C14' C15' 1.380(6) . ? C14' H14A 0.9500 . ? C15' C16' 1.376(7) . ? C15' H15A 0.9500 . ? C16' C17' 1.394(7) . ? C16' H16A 0.9500 . ? C17' C18' 1.515(7) . ? C18' C19' 1.526(7) . ? C18' C20' 1.535(6) . ? C18' H18A 1.0000 . ? C19' H19E 0.9800 . ? C19' H19F 0.9800 . ? C19' H19D 0.9800 . ? C20' H20F 0.9800 . ? C20' H20E 0.9800 . ? C20' H20D 0.9800 . ? C21' C23' 1.528(7) . ? C21' C22' 1.534(6) . ? C21' H21A 1.0000 . ? C22' H22E 0.9800 . ? C22' H22F 0.9800 . ? C22' H22D 0.9800 . ? C23' H23D 0.9800 . ? C23' H23F 0.9800 . ? C23' H23E 0.9800 . ? C24' C29' 1.392(7) . ? C24' C25' 1.412(7) . ? C25' C26' 1.386(7) . ? C25' C30' 1.523(7) . ? C26' C27' 1.378(8) . ? C26' H26A 0.9500 . ? C27' C28' 1.378(7) . ? C27' H27A 0.9500 . ? C28' C29' 1.391(7) . ? C28' H28A 0.9500 . ? C29' C33' 1.516(7) . ? C30' C31' 1.508(8) . ? C30' C32' 1.533(7) . ? C30' H30A 1.0000 . ? C31' H31E 0.9800 . ? C31' H31F 0.9800 . ? C31' H31D 0.9800 . ? C32' H32E 0.9800 . ? C32' H32F 0.9800 . ? C32' H32D 0.9800 . ? C33' C34' 1.523(8) . ? C33' C35' 1.523(8) . ? C33' H33A 1.0000 . ? C34' H34E 0.9800 . ? C34' H34F 0.9800 . ? C34' H34D 0.9800 . ? C35' H35E 0.9800 . ? C35' H35F 0.9800 . ? C35' H35D 0.9800 . ? C36' C41' 1.396(6) . ? C36' C37' 1.403(7) . ? C37' C38' 1.392(7) . ? C37' C42' 1.493(6) . ? C38' C39' 1.391(7) . ? C38' H38A 0.9500 . ? C39' C40' 1.384(7) . ? C39' H39A 0.9500 . ? C40' C41' 1.381(7) . ? C40' H40A 0.9500 . ? C41' C54' 1.491(7) . ? C42' C43' 1.406(6) . ? C42' C47' 1.407(7) . ? C43' C44' 1.383(7) . ? C43' C48' 1.528(7) . ? C44' C45' 1.381(7) . ? C44' H44A 0.9500 . ? C45' C46' 1.370(7) . ? C45' H45A 0.9500 . ? C46' C47' 1.389(7) . ? C46' H46A 0.9500 . ? C47' C51' 1.522(7) . ? C48' C49' 1.518(7) . ? C48' C50' 1.535(7) . ? C48' H48A 1.0000 . ? C49' H49D 0.9800 . ? C49' H49E 0.9800 . ? C49' H49F 0.9800 . ? C50' H50F 0.9800 . ? C50' H50D 0.9800 . ? C50' H50E 0.9800 . ? C51' C53' 1.507(7) . ? C51' C52' 1.516(8) . ? C51' H51A 1.0000 . ? C52' H52D 0.9800 . ? C52' H52E 0.9800 . ? C52' H52F 0.9800 . ? C53' H53F 0.9800 . ? C53' H53E 0.9800 . ? C53' H53D 0.9800 . ? C54' C55' 1.396(6) . ? C54' C59' 1.403(7) . ? C55' C56' 1.390(7) . ? C55' C60' 1.531(7) . ? C56' C57' 1.375(7) . ? C56' H56A 0.9500 . ? C57' C58' 1.369(7) . ? C57' H57A 0.9500 . ? C58' C59' 1.395(7) . ? C58' H58A 0.9500 . ? C59' C63' 1.517(7) . ? C60' C62' 1.518(7) . ? C60' C61' 1.531(7) . ? C60' H60A 1.0000 . ? C61' H61D 0.9800 . ? C61' H61F 0.9800 . ? C61' H61E 0.9800 . ? C62' H62E 0.9800 . ? C62' H62F 0.9800 . ? C62' H62D 0.9800 . ? C63' C65' 1.530(7) . ? C63' C64' 1.532(7) . ? C63' H63A 1.0000 . ? C64' H64E 0.9800 . ? C64' H64F 0.9800 . ? C64' H64D 0.9800 . ? C65' H65E 0.9800 . ? C65' H65F 0.9800 . ? C65' H65D 0.9800 . ? C66' H66E 0.9800 . ? C66' H66F 0.9800 . ? C66' H66D 0.9800 . ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag C4 Mn1 C3 93.3(2) . . ? C4 Mn1 C5 95.4(2) . . ? C3 Mn1 C5 171.2(2) . . ? C4 Mn1 C2 94.1(2) . . ? C3 Mn1 C2 87.3(2) . . ? C5 Mn1 C2 90.3(2) . . ? C4 Mn1 C1 93.2(2) . . ? C3 Mn1 C1 91.6(2) . . ? C5 Mn1 C1 89.7(2) . . ? C2 Mn1 C1 172.7(2) . . ? C4 Mn1 Si1 179.21(17) . . ? C3 Mn1 Si1 85.99(15) . . ? C5 Mn1 Si1 85.38(17) . . ? C2 Mn1 Si1 85.71(15) . . ? C1 Mn1 Si1 86.99(15) . . ? C66 Si1 Cl1 105.27(18) . . ? C66 Si1 Cl2 102.51(18) . . ? Cl1 Si1 Cl2 100.83(8) . . ? C66 Si1 Mn1 118.80(17) . . ? Cl1 Si1 Mn1 112.00(8) . . ? Cl2 Si1 Mn1 115.39(8) . . ? C1 N1 C6 172.1(4) . . ? C2 N2 C36 179.0(5) . . ? N1 C1 Mn1 179.0(5) . . ? N2 C2 Mn1 177.0(5) . . ? O1 C3 Mn1 178.0(5) . . ? O2 C4 Mn1 178.6(6) . . ? O3 C5 Mn1 178.4(5) . . ? C7 C6 C11 121.6(4) . . ? C7 C6 N1 119.1(4) . . ? C11 C6 N1 119.3(4) . . ? C6 C7 C8 118.9(4) . . ? C6 C7 C12 120.4(4) . . ? C8 C7 C12 120.7(4) . . ? C9 C8 C7 120.1(5) . . ? C9 C8 H8 119.9 . . ? C7 C8 H8 119.9 . . ? C10 C9 C8 119.9(5) . . ? C10 C9 H9 120.0 . . ? C8 C9 H9 120.0 . . ? C9 C10 C11 121.9(4) . . ? C9 C10 H10 119.0 . . ? C11 C10 H10 119.0 . . ? C10 C11 C6 117.4(5) . . ? C10 C11 C24 119.2(4) . . ? C6 C11 C24 123.4(4) . . ? C13 C12 C17 122.1(4) . . ? C13 C12 C7 120.0(4) . . ? C17 C12 C7 117.9(4) . . ? C14 C13 C12 117.4(4) . . ? C14 C13 C18 120.3(4) . . ? C12 C13 C18 122.3(4) . . ? C15 C14 C13 121.8(4) . . ? C15 C14 H14 119.1 . . ? C13 C14 H14 119.1 . . ? C14 C15 C16 119.7(5) . . ? C14 C15 H15 120.1 . . ? C16 C15 H15 120.1 . . ? C15 C16 C17 121.3(5) . . ? C15 C16 H16 119.4 . . ? C17 C16 H16 119.4 . . ? C16 C17 C12 117.6(4) . . ? C16 C17 C21 119.8(4) . . ? C12 C17 C21 122.5(4) . . ? C13 C18 C20 112.9(4) . . ? C13 C18 C19 110.5(4) . . ? C20 C18 C19 110.1(4) . . ? C13 C18 H18 107.7 . . ? C20 C18 H18 107.7 . . ? C19 C18 H18 107.7 . . ? C18 C19 H19A 109.5 . . ? C18 C19 H19C 109.5 . . ? H19A C19 H19C 109.5 . . ? C18 C19 H19B 109.5 . . ? H19A C19 H19B 109.5 . . ? H19C C19 H19B 109.5 . . ? C18 C20 H20B 109.5 . . ? C18 C20 H20C 109.5 . . ? H20B C20 H20C 109.5 . . ? C18 C20 H20A 109.5 . . ? H20B C20 H20A 109.5 . . ? H20C C20 H20A 109.5 . . ? C22 C21 C23 110.8(4) . . ? C22 C21 C17 109.9(4) . . ? C23 C21 C17 112.6(4) . . ? C22 C21 H21 107.8 . . ? C23 C21 H21 107.8 . . ? C17 C21 H21 107.8 . . ? C21 C22 H22A 109.5 . . ? C21 C22 H22C 109.5 . . ? H22A C22 H22C 109.5 . . ? C21 C22 H22B 109.5 . . ? H22A C22 H22B 109.5 . . ? H22C C22 H22B 109.5 . . ? C21 C23 H23B 109.5 . . ? C21 C23 H23C 109.5 . . ? H23B C23 H23C 109.5 . . ? C21 C23 H23A 109.5 . . ? H23B C23 H23A 109.5 . . ? H23C C23 H23A 109.5 . . ? C25 C24 C29 121.3(5) . . ? C25 C24 C11 119.0(4) . . ? C29 C24 C11 119.5(4) . . ? C26 C25 C24 118.7(5) . . ? C26 C25 C30 119.7(5) . . ? C24 C25 C30 121.6(5) . . ? C27 C26 C25 120.6(5) . . ? C27 C26 H26 119.7 . . ? C25 C26 H26 119.7 . . ? C28 C27 C26 120.1(5) . . ? C28 C27 H27 119.9 . . ? C26 C27 H27 119.9 . . ? C27 C28 C29 122.1(5) . . ? C27 C28 H28 119.0 . . ? C29 C28 H28 119.0 . . ? C28 C29 C24 117.2(5) . . ? C28 C29 C33 121.3(5) . . ? C24 C29 C33 121.5(4) . . ? C31 C30 C25 113.2(4) . . ? C31 C30 C32 110.9(5) . . ? C25 C30 C32 110.5(5) . . ? C31 C30 H30 107.4 . . ? C25 C30 H30 107.4 . . ? C32 C30 H30 107.4 . . ? C30 C31 H31A 109.5 . . ? C30 C31 H31C 109.5 . . ? H31A C31 H31C 109.5 . . ? C30 C31 H31B 109.5 . . ? H31A C31 H31B 109.5 . . ? H31C C31 H31B 109.5 . . ? C30 C32 H32A 109.5 . . ? C30 C32 H32B 109.5 . . ? H32A C32 H32B 109.5 . . ? C30 C32 H32C 109.5 . . ? H32A C32 H32C 109.5 . . ? H32B C32 H32C 109.5 . . ? C34 C33 C29 112.6(4) . . ? C34 C33 C35 110.1(4) . . ? C29 C33 C35 111.7(5) . . ? C34 C33 H33 107.4 . . ? C29 C33 H33 107.4 . . ? C35 C33 H33 107.4 . . ? C33 C34 H34A 109.5 . . ? C33 C34 H34B 109.5 . . ? H34A C34 H34B 109.5 . . ? C33 C34 H34C 109.5 . . ? H34A C34 H34C 109.5 . . ? H34B C34 H34C 109.5 . . ? C33 C35 H35C 109.5 . . ? C33 C35 H35B 109.5 . . ? H35C C35 H35B 109.5 . . ? C33 C35 H35A 109.5 . . ? H35C C35 H35A 109.5 . . ? H35B C35 H35A 109.5 . . ? N2 C36 C37 118.8(4) . . ? N2 C36 C41 118.7(4) . . ? C37 C36 C41 122.4(5) . . ? C38 C37 C36 116.8(5) . . ? C38 C37 C42 121.7(4) . . ? C36 C37 C42 121.4(4) . . ? C39 C38 C37 122.8(5) . . ? C39 C38 H38 118.6 . . ? C37 C38 H38 118.6 . . ? C38 C39 C40 119.4(5) . . ? C38 C39 H39 120.3 . . ? C40 C39 H39 120.3 . . ? C41 C40 C39 120.6(5) . . ? C41 C40 H40 119.7 . . ? C39 C40 H40 119.7 . . ? C40 C41 C36 117.8(4) . . ? C40 C41 C54 122.2(5) . . ? C36 C41 C54 119.9(4) . . ? C47 C42 C43 121.2(5) . . ? C47 C42 C37 120.0(4) . . ? C43 C42 C37 118.6(4) . . ? C44 C43 C42 118.4(5) . . ? C44 C43 C48 119.8(5) . . ? C42 C43 C48 121.8(5) . . ? C43 C44 C45 120.9(5) . . ? C43 C44 H44 119.5 . . ? C45 C44 H44 119.5 . . ? C46 C45 C44 120.2(5) . . ? C46 C45 H45 119.9 . . ? C44 C45 H45 119.9 . . ? C45 C46 C47 121.1(5) . . ? C45 C46 H46 119.4 . . ? C47 C46 H46 119.4 . . ? C42 C47 C46 118.1(5) . . ? C42 C47 C51 122.1(5) . . ? C46 C47 C51 119.8(5) . . ? C43 C48 C50 112.9(5) . . ? C43 C48 C49 110.2(4) . . ? C50 C48 C49 111.7(4) . . ? C43 C48 H48 107.2 . . ? C50 C48 H48 107.2 . . ? C49 C48 H48 107.2 . . ? C48 C49 H49A 109.5 . . ? C48 C49 H49C 109.5 . . ? H49A C49 H49C 109.5 . . ? C48 C49 H49B 109.5 . . ? H49A C49 H49B 109.5 . . ? H49C C49 H49B 109.5 . . ? C48 C50 H50A 109.5 . . ? C48 C50 H50C 109.5 . . ? H50A C50 H50C 109.5 . . ? C48 C50 H50B 109.5 . . ? H50A C50 H50B 109.5 . . ? H50C C50 H50B 109.5 . . ? C47 C51 C53 114.3(5) . . ? C47 C51 C52 110.1(4) . . ? C53 C51 C52 109.3(4) . . ? C47 C51 H51 107.6 . . ? C53 C51 H51 107.6 . . ? C52 C51 H51 107.6 . . ? C51 C52 H52B 109.5 . . ? C51 C52 H52C 109.5 . . ? H52B C52 H52C 109.5 . . ? C51 C52 H52A 109.5 . . ? H52B C52 H52A 109.5 . . ? H52C C52 H52A 109.5 . . ? C51 C53 H53A 109.5 . . ? C51 C53 H53C 109.5 . . ? H53A C53 H53C 109.5 . . ? C51 C53 H53B 109.5 . . ? H53A C53 H53B 109.5 . . ? H53C C53 H53B 109.5 . . ? C59 C54 C55 121.4(4) . . ? C59 C54 C41 120.0(4) . . ? C55 C54 C41 118.6(4) . . ? C56 C55 C54 118.1(4) . . ? C56 C55 C60 120.0(4) . . ? C54 C55 C60 121.9(4) . . ? C57 C56 C55 120.9(5) . . ? C57 C56 H56 119.5 . . ? C55 C56 H56 119.5 . . ? C56 C57 C58 120.6(5) . . ? C56 C57 H57 119.7 . . ? C58 C57 H57 119.7 . . ? C57 C58 C59 121.4(5) . . ? C57 C58 H58 119.3 . . ? C59 C58 H58 119.3 . . ? C58 C59 C54 117.6(4) . . ? C58 C59 C63 120.1(4) . . ? C54 C59 C63 122.3(4) . . ? C62 C60 C61 109.7(5) . . ? C62 C60 C55 113.0(5) . . ? C61 C60 C55 110.1(5) . . ? C62 C60 H60 108.0 . . ? C61 C60 H60 108.0 . . ? C55 C60 H60 108.0 . . ? C60 C61 H61C 109.5 . . ? C60 C61 H61B 109.5 . . ? H61C C61 H61B 109.5 . . ? C60 C61 H61A 109.5 . . ? H61C C61 H61A 109.5 . . ? H61B C61 H61A 109.5 . . ? C60 C62 H62A 109.5 . . ? C60 C62 H62B 109.5 . . ? H62A C62 H62B 109.5 . . ? C60 C62 H62C 109.5 . . ? H62A C62 H62C 109.5 . . ? H62B C62 H62C 109.5 . . ? C59 C63 C65 114.0(4) . . ? C59 C63 C64 109.7(4) . . ? C65 C63 C64 109.0(4) . . ? C59 C63 H63 108.0 . . ? C65 C63 H63 108.0 . . ? C64 C63 H63 108.0 . . ? C63 C64 H64C 109.5 . . ? C63 C64 H64B 109.5 . . ? H64C C64 H64B 109.5 . . ? C63 C64 H64A 109.5 . . ? H64C C64 H64A 109.5 . . ? H64B C64 H64A 109.5 . . ? C63 C65 H65A 109.5 . . ? C63 C65 H65B 109.5 . . ? H65A C65 H65B 109.5 . . ? C63 C65 H65C 109.5 . . ? H65A C65 H65C 109.5 . . ? H65B C65 H65C 109.5 . . ? Si1 C66 H66A 109.5 . . ? Si1 C66 H66C 109.5 . . ? H66A C66 H66C 109.5 . . ? Si1 C66 H66B 109.5 . . ? H66A C66 H66B 109.5 . . ? H66C C66 H66B 109.5 . . ? C3' Mn1' C4' 95.0(2) . . ? C3' Mn1' C5' 169.9(2) . . ? C4' Mn1' C5' 95.0(2) . . ? C3' Mn1' C1' 88.7(2) . . ? C4' Mn1' C1' 93.3(2) . . ? C5' Mn1' C1' 91.6(2) . . ? C3' Mn1' C2' 87.4(2) . . ? C4' Mn1' C2' 90.5(2) . . ? C5' Mn1' C2' 91.6(2) . . ? C1' Mn1' C2' 174.7(2) . . ? C3' Mn1' Si1' 85.49(16) . . ? C4' Mn1' Si1' 179.04(18) . . ? C5' Mn1' Si1' 84.48(17) . . ? C1' Mn1' Si1' 87.49(14) . . ? C2' Mn1' Si1' 88.67(15) . . ? C66' Si1' Cl2' 104.91(19) . . ? C66' Si1' Cl1' 103.05(18) . . ? Cl2' Si1' Cl1' 100.50(9) . . ? C66' Si1' Mn1' 118.33(17) . . ? Cl2' Si1' Mn1' 113.42(8) . . ? Cl1' Si1' Mn1' 114.54(8) . . ? C1' N1' C36' 173.6(4) . . ? C2' N2' C6' 173.9(4) . . ? N1' C1' Mn1' 176.2(4) . . ? N2' C2' Mn1' 175.3(4) . . ? O1' C3' Mn1' 179.0(5) . . ? O2' C4' Mn1' 178.9(5) . . ? O3' C5' Mn1' 176.9(5) . . ? C7' C6' C11' 123.2(4) . . ? C7' C6' N2' 118.9(4) . . ? C11' C6' N2' 117.9(4) . . ? C8' C7' C6' 116.8(5) . . ? C8' C7' C12' 121.3(4) . . ? C6' C7' C12' 121.8(4) . . ? C9' C8' C7' 121.6(5) . . ? C9' C8' H8' 119.2 . . ? C7' C8' H8' 119.2 . . ? C10' C9' C8' 119.8(5) . . ? C10' C9' H9' 120.1 . . ? C8' C9' H9' 120.1 . . ? C9' C10' C11' 122.0(5) . . ? C9' C10' H10A 119.0 . . ? C11' C10' H10A 119.0 . . ? C10' C11' C6' 116.6(5) . . ? C10' C11' C24' 120.8(5) . . ? C6' C11' C24' 122.5(4) . . ? C13' C12' C17' 121.0(4) . . ? C13' C12' C7' 119.3(4) . . ? C17' C12' C7' 119.7(4) . . ? C14' C13' C12' 118.9(4) . . ? C14' C13' C21' 119.0(4) . . ? C12' C13' C21' 122.0(4) . . ? C15' C14' C13' 119.8(5) . . ? C15' C14' H14A 120.1 . . ? C13' C14' H14A 120.1 . . ? C16' C15' C14' 121.4(5) . . ? C16' C15' H15A 119.3 . . ? C14' C15' H15A 119.3 . . ? C15' C16' C17' 120.4(5) . . ? C15' C16' H16A 119.8 . . ? C17' C16' H16A 119.8 . . ? C16' C17' C12' 118.5(5) . . ? C16' C17' C18' 120.0(4) . . ? C12' C17' C18' 121.5(5) . . ? C17' C18' C19' 111.3(4) . . ? C17' C18' C20' 114.1(4) . . ? C19' C18' C20' 108.8(4) . . ? C17' C18' H18A 107.4 . . ? C19' C18' H18A 107.4 . . ? C20' C18' H18A 107.4 . . ? C18' C19' H19E 109.5 . . ? C18' C19' H19F 109.5 . . ? H19E C19' H19F 109.5 . . ? C18' C19' H19D 109.5 . . ? H19E C19' H19D 109.5 . . ? H19F C19' H19D 109.5 . . ? C18' C20' H20F 109.5 . . ? C18' C20' H20E 109.5 . . ? H20F C20' H20E 109.5 . . ? C18' C20' H20D 109.5 . . ? H20F C20' H20D 109.5 . . ? H20E C20' H20D 109.5 . . ? C13' C21' C23' 111.9(4) . . ? C13' C21' C22' 112.3(4) . . ? C23' C21' C22' 110.1(4) . . ? C13' C21' H21A 107.4 . . ? C23' C21' H21A 107.4 . . ? C22' C21' H21A 107.4 . . ? C21' C22' H22E 109.5 . . ? C21' C22' H22F 109.5 . . ? H22E C22' H22F 109.5 . . ? C21' C22' H22D 109.5 . . ? H22E C22' H22D 109.5 . . ? H22F C22' H22D 109.5 . . ? C21' C23' H23D 109.5 . . ? C21' C23' H23F 109.5 . . ? H23D C23' H23F 109.5 . . ? C21' C23' H23E 109.5 . . ? H23D C23' H23E 109.5 . . ? H23F C23' H23E 109.5 . . ? C29' C24' C25' 121.1(5) . . ? C29' C24' C11' 119.7(4) . . ? C25' C24' C11' 119.3(4) . . ? C26' C25' C24' 117.8(5) . . ? C26' C25' C30' 120.5(5) . . ? C24' C25' C30' 121.7(5) . . ? C27' C26' C25' 121.7(5) . . ? C27' C26' H26A 119.2 . . ? C25' C26' H26A 119.2 . . ? C28' C27' C26' 119.8(5) . . ? C28' C27' H27A 120.1 . . ? C26' C27' H27A 120.1 . . ? C27' C28' C29' 120.9(5) . . ? C27' C28' H28A 119.5 . . ? C29' C28' H28A 119.5 . . ? C28' C29' C24' 118.7(5) . . ? C28' C29' C33' 118.9(5) . . ? C24' C29' C33' 122.3(5) . . ? C31' C30' C25' 111.3(4) . . ? C31' C30' C32' 110.8(5) . . ? C25' C30' C32' 111.7(5) . . ? C31' C30' H30A 107.6 . . ? C25' C30' H30A 107.6 . . ? C32' C30' H30A 107.6 . . ? C30' C31' H31E 109.5 . . ? C30' C31' H31F 109.5 . . ? H31E C31' H31F 109.5 . . ? C30' C31' H31D 109.5 . . ? H31E C31' H31D 109.5 . . ? H31F C31' H31D 109.5 . . ? C30' C32' H32E 109.5 . . ? C30' C32' H32F 109.5 . . ? H32E C32' H32F 109.5 . . ? C30' C32' H32D 109.5 . . ? H32E C32' H32D 109.5 . . ? H32F C32' H32D 109.5 . . ? C29' C33' C34' 112.7(5) . . ? C29' C33' C35' 112.0(5) . . ? C34' C33' C35' 110.0(5) . . ? C29' C33' H33A 107.3 . . ? C34' C33' H33A 107.3 . . ? C35' C33' H33A 107.3 . . ? C33' C34' H34E 109.5 . . ? C33' C34' H34F 109.5 . . ? H34E C34' H34F 109.5 . . ? C33' C34' H34D 109.5 . . ? H34E C34' H34D 109.5 . . ? H34F C34' H34D 109.5 . . ? C33' C35' H35E 109.5 . . ? C33' C35' H35F 109.5 . . ? H35E C35' H35F 109.5 . . ? C33' C35' H35D 109.5 . . ? H35E C35' H35D 109.5 . . ? H35F C35' H35D 109.5 . . ? C41' C36' N1' 118.2(4) . . ? C41' C36' C37' 123.9(5) . . ? N1' C36' C37' 117.9(4) . . ? C38' C37' C36' 117.1(4) . . ? C38' C37' C42' 121.8(4) . . ? C36' C37' C42' 121.1(4) . . ? C39' C38' C37' 120.0(5) . . ? C39' C38' H38A 120.0 . . ? C37' C38' H38A 120.0 . . ? C40' C39' C38' 121.1(5) . . ? C40' C39' H39A 119.4 . . ? C38' C39' H39A 119.4 . . ? C41' C40' C39' 121.1(5) . . ? C41' C40' H40A 119.4 . . ? C39' C40' H40A 119.4 . . ? C40' C41' C36' 116.8(5) . . ? C40' C41' C54' 124.7(4) . . ? C36' C41' C54' 118.5(4) . . ? C43' C42' C47' 120.7(5) . . ? C43' C42' C37' 119.7(4) . . ? C47' C42' C37' 119.5(4) . . ? C44' C43' C42' 118.4(5) . . ? C44' C43' C48' 121.3(4) . . ? C42' C43' C48' 120.4(4) . . ? C45' C44' C43' 121.1(5) . . ? C45' C44' H44A 119.5 . . ? C43' C44' H44A 119.5 . . ? C46' C45' C44' 120.4(5) . . ? C46' C45' H45A 119.8 . . ? C44' C45' H45A 119.8 . . ? C45' C46' C47' 120.9(5) . . ? C45' C46' H46A 119.6 . . ? C47' C46' H46A 119.6 . . ? C46' C47' C42' 118.5(5) . . ? C46' C47' C51' 120.0(5) . . ? C42' C47' C51' 121.5(4) . . ? C49' C48' C43' 111.8(5) . . ? C49' C48' C50' 109.9(4) . . ? C43' C48' C50' 112.2(4) . . ? C49' C48' H48A 107.6 . . ? C43' C48' H48A 107.6 . . ? C50' C48' H48A 107.6 . . ? C48' C49' H49D 109.5 . . ? C48' C49' H49E 109.5 . . ? H49D C49' H49E 109.5 . . ? C48' C49' H49F 109.5 . . ? H49D C49' H49F 109.5 . . ? H49E C49' H49F 109.5 . . ? C48' C50' H50F 109.5 . . ? C48' C50' H50D 109.5 . . ? H50F C50' H50D 109.5 . . ? C48' C50' H50E 109.5 . . ? H50F C50' H50E 109.5 . . ? H50D C50' H50E 109.5 . . ? C53' C51' C52' 110.4(6) . . ? C53' C51' C47' 112.6(5) . . ? C52' C51' C47' 110.5(5) . . ? C53' C51' H51A 107.7 . . ? C52' C51' H51A 107.7 . . ? C47' C51' H51A 107.7 . . ? C51' C52' H52D 109.5 . . ? C51' C52' H52E 109.5 . . ? H52D C52' H52E 109.5 . . ? C51' C52' H52F 109.5 . . ? H52D C52' H52F 109.5 . . ? H52E C52' H52F 109.5 . . ? C51' C53' H53F 109.5 . . ? C51' C53' H53E 109.5 . . ? H53F C53' H53E 109.5 . . ? C51' C53' H53D 109.5 . . ? H53F C53' H53D 109.5 . . ? H53E C53' H53D 109.5 . . ? C55' C54' C59' 121.5(5) . . ? C55' C54' C41' 119.8(4) . . ? C59' C54' C41' 118.6(4) . . ? C56' C55' C54' 117.9(5) . . ? C56' C55' C60' 120.6(4) . . ? C54' C55' C60' 121.5(5) . . ? C57' C56' C55' 121.1(5) . . ? C57' C56' H56A 119.5 . . ? C55' C56' H56A 119.5 . . ? C58' C57' C56' 120.6(6) . . ? C58' C57' H57A 119.7 . . ? C56' C57' H57A 119.7 . . ? C57' C58' C59' 120.7(5) . . ? C57' C58' H58A 119.6 . . ? C59' C58' H58A 119.6 . . ? C58' C59' C54' 118.1(5) . . ? C58' C59' C63' 120.7(5) . . ? C54' C59' C63' 121.2(5) . . ? C62' C60' C61' 109.4(4) . . ? C62' C60' C55' 114.0(5) . . ? C61' C60' C55' 109.5(4) . . ? C62' C60' H60A 107.9 . . ? C61' C60' H60A 107.9 . . ? C55' C60' H60A 107.9 . . ? C60' C61' H61D 109.5 . . ? C60' C61' H61F 109.5 . . ? H61D C61' H61F 109.5 . . ? C60' C61' H61E 109.5 . . ? H61D C61' H61E 109.5 . . ? H61F C61' H61E 109.5 . . ? C60' C62' H62E 109.5 . . ? C60' C62' H62F 109.5 . . ? H62E C62' H62F 109.5 . . ? C60' C62' H62D 109.5 . . ? H62E C62' H62D 109.5 . . ? H62F C62' H62D 109.5 . . ? C59' C63' C65' 114.9(5) . . ? C59' C63' C64' 110.5(4) . . ? C65' C63' C64' 109.7(4) . . ? C59' C63' H63A 107.1 . . ? C65' C63' H63A 107.1 . . ? C64' C63' H63A 107.1 . . ? C63' C64' H64E 109.5 . . ? C63' C64' H64F 109.5 . . ? H64E C64' H64F 109.5 . . ? C63' C64' H64D 109.5 . . ? H64E C64' H64D 109.5 . . ? H64F C64' H64D 109.5 . . ? C63' C65' H65E 109.5 . . ? C63' C65' H65F 109.5 . . ? H65E C65' H65F 109.5 . . ? C63' C65' H65D 109.5 . . ? H65E C65' H65D 109.5 . . ? H65F C65' H65D 109.5 . . ? Si1' C66' H66E 109.5 . . ? Si1' C66' H66F 109.5 . . ? H66E C66' H66F 109.5 . . ? Si1' C66' H66D 109.5 . . ? H66E C66' H66D 109.5 . . ? H66F C66' H66D 109.5 . . ? _diffrn_measured_fraction_theta_max 0.975 _diffrn_reflns_theta_full 25.00 _diffrn_measured_fraction_theta_full 0.989 _refine_diff_density_max 1.074 _refine_diff_density_min -0.752 _refine_diff_density_rms 0.094 #===END data_JFig368 _database_code_depnum_ccdc_archive 'CCDC 785488' #TrackingRef 'cif-full.cif' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ClSnMn(CO)3(CNArDipp2)2 _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C67 H79 Cl Mn N2 O3.50 Sn' _chemical_formula_weight 1177.40 loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Cl Cl 0.1484 0.1585 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Mn Mn 0.3368 0.7283 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Sn Sn -0.6537 1.4246 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting Monoclinic _symmetry_space_group_name_H-M P2(1)/c loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, y+1/2, -z+1/2' '-x, -y, -z' 'x, -y-1/2, z-1/2' _cell_length_a 19.479(5) _cell_length_b 16.599(5) _cell_length_c 20.104(5) _cell_angle_alpha 90.000(5) _cell_angle_beta 113.546(5) _cell_angle_gamma 90.000(5) _cell_volume 5959(3) _cell_formula_units_Z 4 _cell_measurement_temperature 100(2) _cell_measurement_reflns_used 8928 _cell_measurement_theta_min 2.43 _cell_measurement_theta_max 25.73 _exptl_crystal_description Block _exptl_crystal_colour Green _exptl_crystal_size_max 0.26 _exptl_crystal_size_mid 0.14 _exptl_crystal_size_min 0.05 _exptl_crystal_density_meas 'not measured' _exptl_crystal_density_diffrn 1.312 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 2460 _exptl_absorpt_coefficient_mu 0.724 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.8342 _exptl_absorpt_correction_T_max 0.9647 _exptl_absorpt_process_details SADABS _exptl_special_details ; ? ; _diffrn_ambient_temperature 100(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'Bruker APEX CCD' _diffrn_measurement_method '\f and \w scans' _diffrn_reflns_number 71933 _diffrn_reflns_av_R_equivalents 0.0464 _diffrn_reflns_av_sigmaI/netI 0.0309 _diffrn_reflns_limit_h_min -23 _diffrn_reflns_limit_h_max 23 _diffrn_reflns_limit_k_min -20 _diffrn_reflns_limit_k_max 20 _diffrn_reflns_limit_l_min -24 _diffrn_reflns_limit_l_max 24 _diffrn_reflns_theta_min 1.14 _diffrn_reflns_theta_max 25.80 _reflns_number_total 11292 _reflns_number_gt 9455 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'Bruker APEX2' _computing_cell_refinement 'Bruker SAINT' _computing_data_reduction 'Bruker SAINT' _computing_structure_solution 'SHELXS-97 (Sheldrick, 2008)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 2008)' _computing_molecular_graphics 'Bruker SHELXTL' _computing_publication_material 'Bruker SHELXTL' _refine_special_details ; Refinement of F^2^ against ALL reflections. The weighted R-factor wR and goodness of fit S are based on F^2^, conventional R-factors R are based on F, with F set to zero for negative F^2^. The threshold expression of F^2^ > 2sigma(F^2^) is used only for calculating R-factors(gt) etc. and is not relevant to the choice of reflections for refinement. R-factors based on F^2^ are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger. ; _refine_ls_structure_factor_coef Fsqd _refine_ls_matrix_type full _refine_ls_weighting_scheme calc _refine_ls_weighting_details 'calc w=1/[\s^2^(Fo^2^)+(0.0759P)^2^+17.6156P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment constr _refine_ls_extinction_method none _refine_ls_number_reflns 11292 _refine_ls_number_parameters 763 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0603 _refine_ls_R_factor_gt 0.0487 _refine_ls_wR_factor_ref 0.1467 _refine_ls_wR_factor_gt 0.1363 _refine_ls_goodness_of_fit_ref 1.033 _refine_ls_restrained_S_all 1.033 _refine_ls_shift/su_max 0.001 _refine_ls_shift/su_mean 0.000 loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_occupancy _atom_site_symmetry_multiplicity _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group Sn1 Sn 0.137312(15) 0.963318(16) -0.285428(15) 0.02677(10) Uani 1 1 d . . . Mn1 Mn 0.25079(3) 1.06445(3) -0.23379(3) 0.01885(13) Uani 1 1 d . . . Cl1 Cl 0.04340(6) 1.04566(6) -0.37401(6) 0.0382(3) Uani 1 1 d . . . O1 O 0.2753(2) 0.9767(2) -0.09695(18) 0.0493(9) Uani 1 1 d . . . O2 O 0.38976(17) 1.1625(2) -0.1695(2) 0.0512(10) Uani 1 1 d . . . O3 O 0.19420(18) 1.13694(18) -0.38088(18) 0.0388(7) Uani 1 1 d . . . N1 N 0.15008(15) 1.18085(16) -0.19490(15) 0.0146(6) Uani 1 1 d . . . N2 N 0.33050(16) 0.93087(17) -0.28002(16) 0.0174(6) Uani 1 1 d . . . C1 C 0.29968(19) 0.9823(2) -0.26229(19) 0.0190(7) Uani 1 1 d . . . C2 C 0.18777(19) 1.1370(2) -0.21100(19) 0.0180(7) Uani 1 1 d . . . C3 C 0.2664(2) 1.0108(2) -0.1492(2) 0.0296(9) Uani 1 1 d . . . C4 C 0.3368(2) 1.1255(2) -0.1935(3) 0.0329(9) Uani 1 1 d . . . C5 C 0.21646(19) 1.1107(2) -0.3267(2) 0.0201(7) Uani 1 1 d . . . C6 C 0.36868(19) 0.8731(2) -0.30180(19) 0.0176(7) Uani 1 1 d . . . C7 C 0.32939(19) 0.8305(2) -0.36606(19) 0.0181(7) Uani 1 1 d . . . C8 C 0.3685(2) 0.7733(2) -0.3873(2) 0.0231(8) Uani 1 1 d . . . H8 H 0.3435 0.7439 -0.4309 0.028 Uiso 1 1 calc R . . C9 C 0.4434(2) 0.7584(2) -0.3460(2) 0.0253(8) Uani 1 1 d . . . H9 H 0.4693 0.7192 -0.3616 0.030 Uiso 1 1 calc R . . C10 C 0.4810(2) 0.8004(2) -0.2819(2) 0.0238(8) Uani 1 1 d . . . H10 H 0.5324 0.7893 -0.2538 0.029 Uiso 1 1 calc R . . C11 C 0.4441(2) 0.8586(2) -0.2584(2) 0.0200(7) Uani 1 1 d . . . C12 C 0.24787(19) 0.8464(2) -0.40606(19) 0.0188(7) Uani 1 1 d . . . C13 C 0.1972(2) 0.8033(2) -0.3857(2) 0.0232(8) Uani 1 1 d . A . C14 C 0.1214(2) 0.8233(2) -0.4186(2) 0.0285(8) Uani 1 1 d . . . H14 H 0.0863 0.7954 -0.4052 0.034 Uiso 1 1 calc R . . C15 C 0.0971(2) 0.8827(3) -0.4698(2) 0.0336(9) Uani 1 1 d . . . H15 H 0.0454 0.8962 -0.4911 0.040 Uiso 1 1 calc R . . C16 C 0.1467(2) 0.9233(3) -0.4910(2) 0.0309(9) Uani 1 1 d . . . H16 H 0.1285 0.9635 -0.5276 0.037 Uiso 1 1 calc R . . C17 C 0.2232(2) 0.9064(2) -0.4597(2) 0.0234(8) Uani 1 1 d . . . C18 C 0.2234(2) 0.7343(2) -0.3316(2) 0.0301(9) Uani 1 1 d . . . H18B H 0.2773 0.7244 -0.3217 0.036 Uiso 0.43(2) 1 calc PR A 2 H18 H 0.2763 0.7420 -0.2998 0.036 Uiso 0.57(2) 1 d PR A 1 C19 C 0.2146(7) 0.6587(5) -0.3755(6) 0.040(3) Uani 0.57(2) 1 d P A 1 H19A H 0.2290 0.6120 -0.3429 0.060 Uiso 0.57(2) 1 calc PR A 1 H19C H 0.2467 0.6617 -0.4025 0.060 Uiso 0.57(2) 1 calc PR A 1 H19B H 0.1622 0.6530 -0.4096 0.060 Uiso 0.57(2) 1 calc PR A 1 C19B C 0.1820(12) 0.6559(8) -0.3606(11) 0.062(5) Uani 0.43(2) 1 d P A 2 H19D H 0.2026 0.6135 -0.3240 0.093 Uiso 0.43(2) 1 calc PR A 2 H19F H 0.1881 0.6405 -0.4050 0.093 Uiso 0.43(2) 1 calc PR A 2 H19E H 0.1287 0.6631 -0.3714 0.093 Uiso 0.43(2) 1 calc PR A 2 C20 C 0.1768(8) 0.7257(7) -0.2857(7) 0.049(3) Uani 0.57(2) 1 d P A 1 H20B H 0.1235 0.7224 -0.3177 0.073 Uiso 0.57(2) 1 calc PR A 1 H20C H 0.1853 0.7725 -0.2537 0.073 Uiso 0.57(2) 1 calc PR A 1 H20A H 0.1917 0.6765 -0.2563 0.073 Uiso 0.57(2) 1 calc PR A 1 C20B C 0.2197(8) 0.7534(8) -0.2586(7) 0.033(4) Uani 0.43(2) 1 d P A 2 H20E H 0.1683 0.7680 -0.2664 0.050 Uiso 0.43(2) 1 calc PR A 2 H20F H 0.2533 0.7984 -0.2356 0.050 Uiso 0.43(2) 1 calc PR A 2 H20D H 0.2352 0.7059 -0.2271 0.050 Uiso 0.43(2) 1 calc PR A 2 C21 C 0.2777(2) 0.9481(2) -0.4851(2) 0.0269(8) Uani 1 1 d . . . H21 H 0.3288 0.9434 -0.4454 0.032 Uiso 1 1 calc R . . C22 C 0.2791(3) 0.9057(3) -0.5515(3) 0.0440(11) Uani 1 1 d . . . H22A H 0.2933 0.8492 -0.5397 0.066 Uiso 1 1 calc R . . H22C H 0.3157 0.9321 -0.5665 0.066 Uiso 1 1 calc R . . H22B H 0.2294 0.9084 -0.5912 0.066 Uiso 1 1 calc R . . C23 C 0.2612(3) 1.0377(3) -0.5012(3) 0.0472(13) Uani 1 1 d . . . H23B H 0.2119 1.0441 -0.5410 0.071 Uiso 1 1 calc R . . H23C H 0.2995 1.0615 -0.5151 0.071 Uiso 1 1 calc R . . H23A H 0.2616 1.0648 -0.4578 0.071 Uiso 1 1 calc R . . C24 C 0.4827(2) 0.9031(2) -0.1883(2) 0.0236(8) Uani 1 1 d . . . C25 C 0.5264(2) 0.9710(2) -0.1869(2) 0.0276(8) Uani 1 1 d . . . C26 C 0.5621(2) 1.0107(3) -0.1203(3) 0.0388(11) Uani 1 1 d . . . H26 H 0.5915 1.0572 -0.1178 0.047 Uiso 1 1 calc R . . C27 C 0.5554(3) 0.9839(3) -0.0591(3) 0.0447(13) Uani 1 1 d . . . H27 H 0.5808 1.0114 -0.0145 0.054 Uiso 1 1 calc R . . C28 C 0.5124(3) 0.9173(3) -0.0611(2) 0.0452(13) Uani 1 1 d . . . H28 H 0.5088 0.8994 -0.0178 0.054 Uiso 1 1 calc R . . C29 C 0.4740(2) 0.8759(3) -0.1259(2) 0.0319(9) Uani 1 1 d . B . C30 C 0.5329(2) 1.0020(2) -0.2548(2) 0.0311(9) Uani 1 1 d . . . H30 H 0.5272 0.9547 -0.2874 0.037 Uiso 1 1 calc R . . C31 C 0.6084(3) 1.0413(3) -0.2409(3) 0.0440(12) Uani 1 1 d . . . H31B H 0.6125 1.0923 -0.2151 0.066 Uiso 1 1 calc R . . H31C H 0.6122 1.0515 -0.2873 0.066 Uiso 1 1 calc R . . H31A H 0.6489 1.0051 -0.2115 0.066 Uiso 1 1 calc R . . C32 C 0.4695(2) 1.0611(3) -0.2953(3) 0.0425(11) Uani 1 1 d . . . H32A H 0.4211 1.0339 -0.3089 0.064 Uiso 1 1 calc R . . H32C H 0.4748 1.0802 -0.3392 0.064 Uiso 1 1 calc R . . H32B H 0.4720 1.1071 -0.2638 0.064 Uiso 1 1 calc R . . C33 C 0.4266(2) 0.8039(3) -0.1279(2) 0.0403(11) Uani 1 1 d . . . H33B H 0.4148 0.7833 -0.1780 0.048 Uiso 0.275(14) 1 calc PR B 2 H33 H 0.3850 0.8019 -0.1757 0.048 Uiso 0.725(14) 1 d PR B 1 C34 C 0.4689(4) 0.7300(4) -0.1177(6) 0.0369(18) Uani 0.725(14) 1 d P B 1 H34B H 0.5100 0.7300 -0.0695 0.055 Uiso 0.725(14) 1 calc PR B 1 H34C H 0.4893 0.7259 -0.1549 0.055 Uiso 0.725(14) 1 calc PR B 1 H34A H 0.4359 0.6839 -0.1219 0.055 Uiso 0.725(14) 1 calc PR B 1 C34B C 0.4702(10) 0.7244(10) -0.0783(14) 0.033(5) Uani 0.275(14) 1 d P B 2 H34E H 0.4858 0.7369 -0.0267 0.049 Uiso 0.275(14) 1 calc PR B 2 H34F H 0.5143 0.7113 -0.0881 0.049 Uiso 0.275(14) 1 calc PR B 2 H34D H 0.4360 0.6782 -0.0910 0.049 Uiso 0.275(14) 1 calc PR B 2 C35 C 0.3927(5) 0.8139(4) -0.0692(4) 0.043(2) Uani 0.725(14) 1 d P B 1 H35A H 0.3529 0.7740 -0.0779 0.065 Uiso 0.725(14) 1 calc PR B 1 H35C H 0.3719 0.8682 -0.0724 0.065 Uiso 0.725(14) 1 calc PR B 1 H35B H 0.4322 0.8057 -0.0207 0.065 Uiso 0.725(14) 1 calc PR B 1 C35B C 0.3500(9) 0.8045(9) -0.1266(12) 0.036(6) Uani 0.275(14) 1 d P B 2 H35D H 0.3332 0.7490 -0.1258 0.054 Uiso 0.275(14) 1 calc PR B 2 H35F H 0.3148 0.8320 -0.1700 0.054 Uiso 0.275(14) 1 calc PR B 2 H35E H 0.3519 0.8330 -0.0832 0.054 Uiso 0.275(14) 1 calc PR B 2 C36 C 0.11740(17) 1.23810(19) -0.16589(18) 0.0139(6) Uani 1 1 d . . . C37 C 0.08029(17) 1.30419(19) -0.20878(18) 0.0145(6) Uani 1 1 d . . . C38 C 0.05341(18) 1.3632(2) -0.17596(19) 0.0177(7) Uani 1 1 d . . . H38 H 0.0288 1.4091 -0.2033 0.021 Uiso 1 1 calc R . . C39 C 0.06173(19) 1.3565(2) -0.10470(19) 0.0181(7) Uani 1 1 d . . . H39 H 0.0437 1.3980 -0.0833 0.022 Uiso 1 1 calc R . . C40 C 0.09640(18) 1.2892(2) -0.06430(18) 0.0164(7) Uani 1 1 d . . . H40 H 0.1013 1.2846 -0.0155 0.020 Uiso 1 1 calc R . . C41 C 0.12415(17) 1.22821(19) -0.09430(18) 0.0138(6) Uani 1 1 d . . . C42 C 0.07029(19) 1.31149(19) -0.28614(19) 0.0174(7) Uani 1 1 d . . . C43 C 0.0004(2) 1.2940(2) -0.34186(19) 0.0189(7) Uani 1 1 d . . . C44 C -0.0064(2) 1.2986(2) -0.4137(2) 0.0234(8) Uani 1 1 d . . . H44 H -0.0531 1.2867 -0.4522 0.028 Uiso 1 1 calc R . . C45 C 0.0533(2) 1.3200(2) -0.4293(2) 0.0276(8) Uani 1 1 d . . . H45 H 0.0479 1.3215 -0.4784 0.033 Uiso 1 1 calc R . . C46 C 0.1214(2) 1.3395(2) -0.3747(2) 0.0278(9) Uani 1 1 d . . . H46 H 0.1618 1.3558 -0.3866 0.033 Uiso 1 1 calc R . . C47 C 0.1312(2) 1.3352(2) -0.3020(2) 0.0208(7) Uani 1 1 d . . . C48 C -0.0666(2) 1.2685(2) -0.3261(2) 0.0212(7) Uani 1 1 d . . . H48 H -0.0628 1.2967 -0.2808 0.025 Uiso 1 1 calc R . . C49 C -0.0635(2) 1.1778(2) -0.3112(2) 0.0316(9) Uani 1 1 d . . . H49C H -0.0700 1.1483 -0.3556 0.047 Uiso 1 1 calc R . . H49B H -0.1037 1.1630 -0.2959 0.047 Uiso 1 1 calc R . . H49A H -0.0150 1.1640 -0.2728 0.047 Uiso 1 1 calc R . . C50 C -0.1423(2) 1.2903(3) -0.3858(2) 0.0318(9) Uani 1 1 d . . . H50B H -0.1506 1.2579 -0.4291 0.048 Uiso 1 1 calc R . . H50C H -0.1427 1.3476 -0.3977 0.048 Uiso 1 1 calc R . . H50A H -0.1822 1.2794 -0.3690 0.048 Uiso 1 1 calc R . . C51 C 0.2046(2) 1.3613(2) -0.2427(2) 0.0253(8) Uani 1 1 d . . . H51 H 0.2077 1.3365 -0.1963 0.030 Uiso 1 1 calc R . . C52 C 0.2730(2) 1.3334(3) -0.2558(3) 0.0374(10) Uani 1 1 d . . . H52A H 0.2682 1.2759 -0.2678 0.056 Uiso 1 1 calc R . . H52B H 0.3183 1.3424 -0.2119 0.056 Uiso 1 1 calc R . . H52C H 0.2762 1.3641 -0.2961 0.056 Uiso 1 1 calc R . . C53 C 0.2061(2) 1.4527(3) -0.2335(3) 0.0376(10) Uani 1 1 d . . . H53C H 0.2013 1.4787 -0.2789 0.056 Uiso 1 1 calc R . . H53B H 0.2536 1.4687 -0.1946 0.056 Uiso 1 1 calc R . . H53A H 0.1645 1.4694 -0.2210 0.056 Uiso 1 1 calc R . . C54 C 0.15950(18) 1.15529(19) -0.05030(18) 0.0149(6) Uani 1 1 d . . . C55 C 0.23283(19) 1.1603(2) 0.00313(19) 0.0181(7) Uani 1 1 d . . . C56 C 0.2642(2) 1.0930(2) 0.0448(2) 0.0225(7) Uani 1 1 d . . . H56 H 0.3141 1.0953 0.0804 0.027 Uiso 1 1 calc R . . C57 C 0.2237(2) 1.0226(2) 0.0353(2) 0.0273(8) Uani 1 1 d . . . H57 H 0.2459 0.9771 0.0646 0.033 Uiso 1 1 calc R . . C58 C 0.1510(2) 1.0178(2) -0.0167(2) 0.0249(8) Uani 1 1 d . . . H58 H 0.1236 0.9691 -0.0225 0.030 Uiso 1 1 calc R . . C59 C 0.11779(19) 1.0838(2) -0.06061(18) 0.0174(7) Uani 1 1 d . . . C60 C 0.27908(19) 1.2372(2) 0.01302(19) 0.0210(7) Uani 1 1 d . . . H60 H 0.2435 1.2837 -0.0014 0.025 Uiso 1 1 calc R . . C61 C 0.3199(2) 1.2361(3) -0.0377(2) 0.0289(9) Uani 1 1 d . . . H61A H 0.3552 1.1909 -0.0250 0.043 Uiso 1 1 calc R . . H61C H 0.3473 1.2867 -0.0329 0.043 Uiso 1 1 calc R . . H61B H 0.2834 1.2299 -0.0879 0.043 Uiso 1 1 calc R . . C62 C 0.3345(2) 1.2514(3) 0.0914(2) 0.0303(9) Uani 1 1 d . . . H62B H 0.3081 1.2480 0.1238 0.045 Uiso 1 1 calc R . . H62C H 0.3570 1.3050 0.0955 0.045 Uiso 1 1 calc R . . H62A H 0.3739 1.2104 0.1052 0.045 Uiso 1 1 calc R . . C63 C 0.0390(2) 1.0761(2) -0.1187(2) 0.0212(7) Uani 1 1 d . . . H63 H 0.0214 1.1310 -0.1387 0.025 Uiso 1 1 calc R . . C64 C 0.0393(2) 1.0226(2) -0.1808(2) 0.0276(8) Uani 1 1 d . . . H64A H 0.0554 0.9681 -0.1624 0.041 Uiso 1 1 calc R . . H64C H 0.0738 1.0451 -0.2003 0.041 Uiso 1 1 calc R . . H64B H -0.0113 1.0205 -0.2192 0.041 Uiso 1 1 calc R . . C65 C -0.0171(2) 1.0415(3) -0.0905(2) 0.0365(10) Uani 1 1 d . . . H65B H -0.0672 1.0410 -0.1299 0.055 Uiso 1 1 calc R . . H65C H -0.0176 1.0750 -0.0506 0.055 Uiso 1 1 calc R . . H65A H -0.0025 0.9864 -0.0731 0.055 Uiso 1 1 calc R . . O1S O 0.5159(6) 1.4862(7) 0.0112(7) 0.055(3) Uani 0.50 1 d P . . C1S C 0.4398(6) 1.4006(7) -0.0857(7) 0.044(2) Uani 0.50 1 d P C 1 H1SA H 0.4155 1.3854 -0.0533 0.066 Uiso 0.50 1 calc PR C 1 H1SB H 0.4524 1.3519 -0.1061 0.066 Uiso 0.50 1 calc PR C 1 H1SC H 0.4057 1.4342 -0.1252 0.066 Uiso 0.50 1 calc PR C 1 C1SB C 0.4843(8) 1.3744(8) -0.0647(6) 0.055(3) Uani 0.50 1 d P D 2 H1SF H 0.5046 1.4002 -0.0969 0.082 Uiso 0.50 1 calc PR D 2 H1SD H 0.4424 1.3394 -0.0933 0.082 Uiso 0.50 1 calc PR D 2 H1SE H 0.5236 1.3421 -0.0283 0.082 Uiso 0.50 1 calc PR D 2 C2S C 0.5103(6) 1.4471(7) -0.0437(7) 0.054(3) Uani 0.50 1 d P C 1 H2S1 H 0.5524 1.4083 -0.0286 0.065 Uiso 0.50 1 calc PR C 1 H2S2 H 0.5182 1.4853 -0.0778 0.065 Uiso 0.50 1 calc PR C 1 C2SB C 0.4578(7) 1.4372(8) -0.0278(8) 0.066(3) Uani 0.50 1 d P D 2 H2S3 H 0.4174 1.4693 -0.0643 0.079 Uiso 0.50 1 calc PR D 2 H2S4 H 0.4374 1.4114 0.0049 0.079 Uiso 0.50 1 calc PR D 2 loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 Sn1 0.02516(16) 0.02168(16) 0.03378(18) -0.00307(10) 0.01210(12) -0.00020(10) Mn1 0.0188(3) 0.0135(3) 0.0257(3) -0.0037(2) 0.0104(2) 0.0034(2) Cl1 0.0290(5) 0.0338(6) 0.0432(6) -0.0025(4) 0.0055(5) 0.0031(4) O1 0.064(2) 0.051(2) 0.0355(19) 0.0107(16) 0.0229(17) 0.0284(17) O2 0.0245(16) 0.0428(19) 0.082(3) -0.0298(18) 0.0168(16) -0.0095(14) O3 0.0479(18) 0.0321(16) 0.046(2) 0.0059(14) 0.0290(16) 0.0066(14) N1 0.0169(13) 0.0102(13) 0.0182(14) 0.0016(11) 0.0085(12) 0.0017(11) N2 0.0191(14) 0.0125(14) 0.0200(15) -0.0025(11) 0.0073(12) 0.0028(11) C1 0.0176(16) 0.0167(17) 0.0202(18) 0.0010(13) 0.0048(14) -0.0027(13) C2 0.0210(17) 0.0131(16) 0.0190(17) 0.0016(13) 0.0070(14) -0.0029(13) C3 0.029(2) 0.027(2) 0.032(2) -0.0060(17) 0.0112(17) 0.0131(16) C4 0.028(2) 0.025(2) 0.049(3) -0.0116(18) 0.0184(19) 0.0070(17) C5 0.0200(17) 0.0162(17) 0.028(2) -0.0065(15) 0.0136(15) 0.0070(13) C6 0.0186(16) 0.0134(16) 0.0234(18) -0.0003(13) 0.0110(14) 0.0021(13) C7 0.0211(17) 0.0120(16) 0.0244(18) -0.0013(13) 0.0124(15) -0.0003(13) C8 0.0285(19) 0.0170(17) 0.028(2) -0.0060(14) 0.0153(16) 0.0000(14) C9 0.0263(19) 0.0190(18) 0.035(2) -0.0042(15) 0.0164(17) 0.0067(15) C10 0.0216(18) 0.0227(19) 0.028(2) 0.0002(15) 0.0112(16) 0.0060(14) C11 0.0210(17) 0.0160(16) 0.0236(19) 0.0020(14) 0.0096(15) 0.0027(13) C12 0.0215(17) 0.0141(16) 0.0222(18) -0.0083(13) 0.0103(15) -0.0012(13) C13 0.0264(19) 0.0199(18) 0.0266(19) -0.0088(15) 0.0140(16) -0.0048(15) C14 0.0240(19) 0.030(2) 0.036(2) -0.0085(17) 0.0158(17) -0.0035(16) C15 0.0211(19) 0.045(3) 0.034(2) -0.0063(19) 0.0105(17) 0.0060(17) C16 0.031(2) 0.031(2) 0.027(2) 0.0017(16) 0.0077(17) 0.0114(17) C17 0.0274(19) 0.0196(18) 0.0246(19) -0.0055(14) 0.0119(16) 0.0011(14) C18 0.033(2) 0.0201(19) 0.045(2) 0.0023(17) 0.0238(19) -0.0011(16) C19 0.050(6) 0.016(4) 0.061(6) -0.004(4) 0.030(5) -0.005(4) C19B 0.079(12) 0.019(6) 0.087(12) 0.001(6) 0.033(10) -0.010(7) C20 0.063(8) 0.040(5) 0.059(7) 0.010(5) 0.040(6) 0.001(5) C20B 0.033(7) 0.034(6) 0.036(6) 0.017(5) 0.017(5) 0.003(5) C21 0.033(2) 0.0202(19) 0.031(2) 0.0027(15) 0.0160(17) 0.0006(15) C22 0.058(3) 0.038(3) 0.050(3) -0.006(2) 0.036(3) -0.007(2) C23 0.069(3) 0.020(2) 0.069(4) 0.003(2) 0.044(3) 0.003(2) C24 0.0185(17) 0.0248(19) 0.0233(19) -0.0032(15) 0.0038(15) 0.0095(14) C25 0.0246(19) 0.0215(19) 0.031(2) -0.0070(15) 0.0056(16) 0.0092(15) C26 0.028(2) 0.033(2) 0.043(3) -0.017(2) -0.0003(19) 0.0105(18) C27 0.037(2) 0.057(3) 0.028(2) -0.018(2) 0.0004(19) 0.021(2) C28 0.037(2) 0.072(4) 0.025(2) -0.005(2) 0.0104(19) 0.030(2) C29 0.0245(19) 0.043(2) 0.029(2) 0.0028(18) 0.0113(17) 0.0153(18) C30 0.030(2) 0.0196(19) 0.039(2) -0.0018(17) 0.0096(18) -0.0011(16) C31 0.031(2) 0.036(3) 0.064(3) -0.003(2) 0.017(2) 0.0002(19) C32 0.028(2) 0.033(2) 0.057(3) 0.016(2) 0.006(2) -0.0029(18) C33 0.028(2) 0.063(3) 0.032(2) 0.011(2) 0.0146(19) 0.008(2) C34 0.043(4) 0.027(3) 0.045(5) -0.002(3) 0.023(4) 0.003(3) C34B 0.023(8) 0.029(9) 0.040(12) 0.007(8) 0.005(8) 0.006(6) C35 0.062(5) 0.036(4) 0.049(5) 0.005(3) 0.040(4) 0.009(3) C35B 0.035(9) 0.019(7) 0.064(15) 0.010(7) 0.030(10) 0.002(6) C36 0.0133(15) 0.0100(15) 0.0197(17) -0.0011(12) 0.0081(13) 0.0011(12) C37 0.0133(15) 0.0125(16) 0.0185(17) 0.0018(12) 0.0072(13) 0.0004(12) C38 0.0177(16) 0.0125(16) 0.0230(18) 0.0034(13) 0.0083(14) 0.0037(13) C39 0.0202(17) 0.0135(16) 0.0233(18) -0.0015(13) 0.0114(14) 0.0025(13) C40 0.0203(16) 0.0136(16) 0.0168(16) -0.0006(13) 0.0090(14) -0.0017(13) C41 0.0141(15) 0.0096(15) 0.0175(16) 0.0013(12) 0.0060(13) -0.0006(12) C42 0.0236(17) 0.0116(16) 0.0207(18) 0.0035(13) 0.0127(14) 0.0074(13) C43 0.0260(18) 0.0116(16) 0.0208(18) 0.0012(13) 0.0110(15) 0.0068(13) C44 0.031(2) 0.0186(18) 0.0207(18) -0.0017(14) 0.0101(16) 0.0050(15) C45 0.041(2) 0.0230(19) 0.0227(19) 0.0058(15) 0.0167(17) 0.0119(17) C46 0.039(2) 0.0233(19) 0.034(2) 0.0097(16) 0.0271(19) 0.0099(16) C47 0.0254(18) 0.0152(17) 0.0271(19) 0.0043(14) 0.0159(16) 0.0059(14) C48 0.0224(18) 0.0184(18) 0.0225(18) -0.0001(14) 0.0085(15) -0.0013(14) C49 0.032(2) 0.024(2) 0.039(2) 0.0064(17) 0.0133(18) -0.0006(16) C50 0.025(2) 0.034(2) 0.032(2) 0.0067(17) 0.0068(17) -0.0010(17) C51 0.0240(18) 0.0239(19) 0.032(2) 0.0085(16) 0.0157(16) 0.0016(15) C52 0.025(2) 0.033(2) 0.062(3) 0.006(2) 0.025(2) 0.0051(17) C53 0.030(2) 0.031(2) 0.050(3) -0.0052(19) 0.014(2) 0.0012(17) C54 0.0188(16) 0.0109(15) 0.0175(17) 0.0017(12) 0.0100(14) 0.0025(12) C55 0.0210(17) 0.0151(17) 0.0205(18) 0.0011(13) 0.0106(14) 0.0027(13) C56 0.0235(18) 0.0215(18) 0.0215(18) 0.0034(14) 0.0080(15) 0.0067(14) C57 0.036(2) 0.0191(18) 0.028(2) 0.0096(15) 0.0138(17) 0.0121(16) C58 0.039(2) 0.0124(16) 0.028(2) 0.0020(14) 0.0182(18) 0.0006(15) C59 0.0229(17) 0.0134(16) 0.0193(17) -0.0016(13) 0.0120(14) 0.0006(13) C60 0.0170(16) 0.0191(18) 0.0228(19) 0.0003(14) 0.0037(14) 0.0005(13) C61 0.0260(19) 0.034(2) 0.027(2) 0.0028(16) 0.0117(16) -0.0079(16) C62 0.026(2) 0.033(2) 0.027(2) -0.0036(17) 0.0067(17) -0.0047(17) C63 0.0259(18) 0.0154(17) 0.0237(19) -0.0030(14) 0.0116(15) -0.0046(14) C64 0.041(2) 0.0191(18) 0.025(2) -0.0058(15) 0.0152(18) -0.0038(16) C65 0.033(2) 0.049(3) 0.031(2) -0.0115(19) 0.0174(19) -0.022(2) O1S 0.061(9) 0.046(8) 0.065(8) -0.015(5) 0.034(7) -0.011(5) C1S 0.037(6) 0.039(6) 0.062(7) -0.010(5) 0.027(5) -0.002(5) C1SB 0.056(7) 0.066(8) 0.045(6) -0.004(6) 0.023(6) -0.006(6) C2S 0.045(6) 0.063(7) 0.059(7) -0.008(6) 0.024(5) -0.006(5) C2SB 0.050(7) 0.058(8) 0.095(10) 0.017(7) 0.035(7) 0.013(6) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag Sn1 Cl1 2.4048(12) . ? Sn1 Mn1 2.6359(8) . ? Mn1 C3 1.834(5) . ? Mn1 C4 1.845(4) . ? Mn1 C1 1.879(4) . ? Mn1 C5 1.879(4) . ? Mn1 C2 1.902(4) . ? O1 C3 1.145(5) . ? O2 C4 1.130(5) . ? O3 C5 1.089(5) . ? N1 C2 1.167(4) . ? N1 C36 1.395(4) . ? N2 C1 1.178(5) . ? N2 C6 1.388(4) . ? C6 C11 1.398(5) . ? C6 C7 1.401(5) . ? C7 C8 1.388(5) . ? C7 C12 1.489(5) . ? C8 C9 1.382(5) . ? C9 C10 1.389(5) . ? C10 C11 1.395(5) . ? C11 C24 1.501(5) . ? C12 C17 1.404(5) . ? C12 C13 1.405(5) . ? C13 C14 1.396(5) . ? C13 C18 1.520(6) . ? C14 C15 1.366(6) . ? C15 C16 1.378(6) . ? C16 C17 1.395(5) . ? C17 C21 1.516(5) . ? C18 C19 1.504(10) . ? C18 C19B 1.518(15) . ? C18 C20B 1.531(12) . ? C18 C20 1.540(10) . ? C21 C22 1.520(6) . ? C21 C23 1.528(6) . ? C24 C25 1.405(6) . ? C24 C29 1.406(6) . ? C25 C26 1.403(6) . ? C25 C30 1.510(6) . ? C26 C27 1.363(7) . ? C27 C28 1.377(8) . ? C28 C29 1.396(6) . ? C29 C33 1.502(7) . ? C30 C31 1.530(6) . ? C30 C32 1.532(6) . ? C33 C34 1.445(8) . ? C33 C35B 1.503(15) . ? C33 C35 1.574(7) . ? C33 C34B 1.667(18) . ? C36 C41 1.402(5) . ? C36 C37 1.404(4) . ? C37 C38 1.395(5) . ? C37 C42 1.493(5) . ? C38 C39 1.380(5) . ? C39 C40 1.389(5) . ? C40 C41 1.393(5) . ? C41 C54 1.495(4) . ? C42 C47 1.403(5) . ? C42 C43 1.405(5) . ? C43 C44 1.399(5) . ? C43 C48 1.521(5) . ? C44 C45 1.366(6) . ? C45 C46 1.380(6) . ? C46 C47 1.398(5) . ? C47 C51 1.513(5) . ? C48 C50 1.528(5) . ? C48 C49 1.531(5) . ? C51 C53 1.528(6) . ? C51 C52 1.529(5) . ? C54 C59 1.405(5) . ? C54 C55 1.405(5) . ? C55 C56 1.384(5) . ? C55 C60 1.528(5) . ? C56 C57 1.378(6) . ? C57 C58 1.386(6) . ? C58 C59 1.394(5) . ? C59 C63 1.518(5) . ? C60 C61 1.524(5) . ? C60 C62 1.532(5) . ? C63 C65 1.528(5) . ? C63 C64 1.533(5) . ? O1S O1S 0.759(15) 3_685 ? O1S C2S 1.247(18) . ? O1S C2SB 1.359(19) . ? O1S C2SB 1.361(19) 3_685 ? O1S C2S 1.477(17) 3_685 ? C1S C2S 1.506(15) . ? C1SB C2SB 1.487(18) . ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag Cl1 Sn1 Mn1 101.53(4) . . ? C3 Mn1 C4 94.2(2) . . ? C3 Mn1 C1 90.77(16) . . ? C4 Mn1 C1 92.92(16) . . ? C3 Mn1 C5 169.08(17) . . ? C4 Mn1 C5 96.44(19) . . ? C1 Mn1 C5 90.91(15) . . ? C3 Mn1 C2 88.19(15) . . ? C4 Mn1 C2 96.10(16) . . ? C1 Mn1 C2 170.97(15) . . ? C5 Mn1 C2 88.47(14) . . ? C3 Mn1 Sn1 81.86(14) . . ? C4 Mn1 Sn1 173.73(13) . . ? C1 Mn1 Sn1 82.25(11) . . ? C5 Mn1 Sn1 87.67(11) . . ? C2 Mn1 Sn1 88.73(10) . . ? C2 N1 C36 169.5(3) . . ? C1 N2 C6 177.3(3) . . ? N2 C1 Mn1 179.8(4) . . ? N1 C2 Mn1 178.0(3) . . ? O1 C3 Mn1 179.0(4) . . ? O2 C4 Mn1 179.0(4) . . ? O3 C5 Mn1 177.6(3) . . ? N2 C6 C11 119.0(3) . . ? N2 C6 C7 118.4(3) . . ? C11 C6 C7 122.7(3) . . ? C8 C7 C6 117.6(3) . . ? C8 C7 C12 123.6(3) . . ? C6 C7 C12 118.7(3) . . ? C9 C8 C7 121.0(3) . . ? C8 C9 C10 120.5(3) . . ? C9 C10 C11 120.6(3) . . ? C10 C11 C6 117.6(3) . . ? C10 C11 C24 121.8(3) . . ? C6 C11 C24 120.6(3) . . ? C17 C12 C13 121.3(3) . . ? C17 C12 C7 120.3(3) . . ? C13 C12 C7 118.3(3) . . ? C14 C13 C12 118.2(4) . . ? C14 C13 C18 120.5(3) . . ? C12 C13 C18 121.2(3) . . ? C15 C14 C13 120.8(4) . . ? C14 C15 C16 120.7(4) . . ? C15 C16 C17 121.1(4) . . ? C16 C17 C12 117.8(4) . . ? C16 C17 C21 121.4(4) . . ? C12 C17 C21 120.8(3) . . ? C19 C18 C19B 30.9(7) . . ? C19 C18 C13 106.4(5) . . ? C19B C18 C13 113.4(7) . . ? C19 C18 C20B 134.2(6) . . ? C19B C18 C20B 108.9(9) . . ? C13 C18 C20B 113.5(5) . . ? C19 C18 C20 108.5(6) . . ? C19B C18 C20 78.5(9) . . ? C13 C18 C20 112.9(5) . . ? C20B C18 C20 34.8(5) . . ? C17 C21 C22 110.2(3) . . ? C17 C21 C23 113.5(3) . . ? C22 C21 C23 110.0(4) . . ? C25 C24 C29 121.8(4) . . ? C25 C24 C11 119.0(3) . . ? C29 C24 C11 119.1(4) . . ? C26 C25 C24 117.5(4) . . ? C26 C25 C30 120.9(4) . . ? C24 C25 C30 121.6(3) . . ? C27 C26 C25 121.2(5) . . ? C26 C27 C28 120.8(4) . . ? C27 C28 C29 121.0(5) . . ? C28 C29 C24 117.6(4) . . ? C28 C29 C33 120.8(4) . . ? C24 C29 C33 121.6(4) . . ? C25 C30 C31 113.7(4) . . ? C25 C30 C32 111.0(4) . . ? C31 C30 C32 109.6(3) . . ? C34 C33 C29 111.3(4) . . ? C34 C33 C35B 121.1(7) . . ? C29 C33 C35B 126.7(7) . . ? C34 C33 C35 111.7(5) . . ? C29 C33 C35 109.4(5) . . ? C35B C33 C35 43.1(8) . . ? C34 C33 C34B 28.2(7) . . ? C29 C33 C34B 117.0(7) . . ? C35B C33 C34B 105.5(10) . . ? C35 C33 C34B 84.3(9) . . ? N1 C36 C41 118.6(3) . . ? N1 C36 C37 119.0(3) . . ? C41 C36 C37 122.4(3) . . ? C38 C37 C36 117.2(3) . . ? C38 C37 C42 121.2(3) . . ? C36 C37 C42 121.6(3) . . ? C39 C38 C37 121.6(3) . . ? C38 C39 C40 120.0(3) . . ? C39 C40 C41 120.9(3) . . ? C40 C41 C36 117.8(3) . . ? C40 C41 C54 119.9(3) . . ? C36 C41 C54 122.3(3) . . ? C47 C42 C43 121.0(3) . . ? C47 C42 C37 119.3(3) . . ? C43 C42 C37 119.7(3) . . ? C44 C43 C42 118.3(3) . . ? C44 C43 C48 119.7(3) . . ? C42 C43 C48 122.0(3) . . ? C45 C44 C43 120.9(4) . . ? C44 C45 C46 120.9(3) . . ? C45 C46 C47 120.4(4) . . ? C46 C47 C42 118.5(3) . . ? C46 C47 C51 120.1(3) . . ? C42 C47 C51 121.3(3) . . ? C43 C48 C50 114.1(3) . . ? C43 C48 C49 110.2(3) . . ? C50 C48 C49 109.6(3) . . ? C47 C51 C53 110.3(3) . . ? C47 C51 C52 113.1(3) . . ? C53 C51 C52 110.2(3) . . ? C59 C54 C55 120.9(3) . . ? C59 C54 C41 119.6(3) . . ? C55 C54 C41 119.4(3) . . ? C56 C55 C54 118.8(3) . . ? C56 C55 C60 120.1(3) . . ? C54 C55 C60 121.0(3) . . ? C57 C56 C55 120.7(3) . . ? C56 C57 C58 120.6(3) . . ? C57 C58 C59 120.5(3) . . ? C58 C59 C54 118.4(3) . . ? C58 C59 C63 119.4(3) . . ? C54 C59 C63 122.2(3) . . ? C61 C60 C55 109.9(3) . . ? C61 C60 C62 110.4(3) . . ? C55 C60 C62 113.5(3) . . ? C59 C63 C65 113.6(3) . . ? C59 C63 C64 110.1(3) . . ? C65 C63 C64 108.6(3) . . ? O1S O1S C2S 92(2) 3_685 . ? O1S O1S C2SB 74(2) 3_685 . ? C2S O1S C2SB 54.5(9) . . ? O1S O1S C2SB 73.7(19) 3_685 3_685 ? C2S O1S C2SB 126.5(13) . 3_685 ? C2SB O1S C2SB 147.6(7) . 3_685 ? O1S O1S C2S 57.6(18) 3_685 3_685 ? C2S O1S C2S 149.1(8) . 3_685 ? C2SB O1S C2S 110.3(10) . 3_685 ? C2SB O1S C2S 49.8(8) 3_685 3_685 ? O1S C2S C1S 120.1(11) . . ? O1S C2SB C1SB 109.4(10) . . ? _diffrn_measured_fraction_theta_max 0.984 _diffrn_reflns_theta_full 25.00 _diffrn_measured_fraction_theta_full 0.991 _refine_diff_density_max 1.400 _refine_diff_density_min -1.493 _refine_diff_density_rms 0.103 #===END