# Supplementary Material (ESI) for Chemical Communications # This journal is © The Royal Society of Chemistry 2003 data_global _publ_contact_author_name 'Noel Lugan' # #------------------------------------------------------------------------- #2 Person making the deposition # _publ_contact_author 'Noel Lugan' _publ_contact_author_email lugan@lcc-toulouse.fr #------------------------------------------------------------------------- #3 Publication details # loop_ _publ_author_name 'Yannick Ortin' 'Alix Sournia-Saquet' 'Noel Lugan' 'Rene Mathieu' _journal_coden_Cambridge 0182 _journal_name_full Chem.Commun. _journal_volume ? _journal_page_first ? _journal_page_last ? _journal_year ? # #------------------------------------------------------------------------- #------------------------------------------------------------------------- #SUBMISSION INFORMATION # data_nl220101 _database_code_CSD 201834 _audit_creation_date 2003-02-10T15:35:42-00:00 _audit_creation_method 'WinGX routine CIF_UPDATE' #-------------------------------------------------------------------------- # CHEMICAL INFORMATION #-------------------------------------------------------------------------- _chemical_name_systematic ; ? ; _chemical_formula_sum '1.5(C46 H34 Mn2 O4)' _chemical_formula_weight 1140.92 #-------------------------------------------------------------------------- # UNIT CELL INFORMATION #-------------------------------------------------------------------------- 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' _symmetry_cell_setting monoclinic _symmetry_space_group_name_H-M P21/n _cell_length_a 10.8160(13) _cell_length_b 18.3310(18) _cell_length_c 28.208(4) _cell_angle_alpha 90 _cell_angle_beta 100.244(15) _cell_angle_gamma 90 _cell_volume 5503.6(11) _cell_formula_units_Z 4 _cell_measurement_temperature 160(2) #-------------------------------------------------------------------------- # CRYSTAL INFORMATION #-------------------------------------------------------------------------- _exptl_crystal_colour red _exptl_crystal_description needle _exptl_crystal_size_min 0.62 _exptl_crystal_size_mid 0.12 _exptl_crystal_size_max 0.12 _exptl_crystal_size_rad ? _exptl_crystal_density_diffrn 1.377 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 2352 _exptl_special_details ; The asymmetric unit contains 1 complete molecule in a general position and 1/2 molecule lying about an inversion centre. ; #-------------------------------------------------------------------------- # ABSORPTION CORRECTION #-------------------------------------------------------------------------- _exptl_absorpt_coefficient_mu 0.733 #-------------------------------------------------------------------------- # DATA COLLECTION #-------------------------------------------------------------------------- _diffrn_ambient_temperature 293(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_monochromator graphite _diffrn_reflns_av_R_equivalents 0.0635 _diffrn_reflns_av_unetI/netI 0.0486 _diffrn_reflns_number 32196 _diffrn_reflns_limit_h_min -12 _diffrn_reflns_limit_h_max 12 _diffrn_reflns_limit_k_min -20 _diffrn_reflns_limit_k_max 20 _diffrn_reflns_limit_l_min -30 _diffrn_reflns_limit_l_max 31 _diffrn_reflns_theta_min 1.84 _diffrn_reflns_theta_max 23.26 _diffrn_reflns_theta_full 23.26 _diffrn_measured_fraction_theta_full 1 _diffrn_measured_fraction_theta_max 1 _reflns_number_total 7903 _reflns_number_gt 6056 _reflns_threshold_expression >2sigma(I) #-------------------------------------------------------------------------- # COMPUTER PROGRAMS USED #-------------------------------------------------------------------------- _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' #-------------------------------------------------------------------------- # REFINEMENT INFORMATION #-------------------------------------------------------------------------- _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^)+(0.0426P)^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 7903 _refine_ls_number_parameters 706 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0449 _refine_ls_R_factor_gt 0.0301 _refine_ls_wR_factor_ref 0.0731 _refine_ls_wR_factor_gt 0.0689 _refine_ls_goodness_of_fit_ref 0.92 _refine_ls_restrained_S_all 0.92 _refine_ls_shift/su_max 0.001 _refine_ls_shift/su_mean 0 _refine_diff_density_max 0.409 _refine_diff_density_min -0.307 _refine_diff_density_rms 0.051 #-------------------------------------------------------------------------- # ATOMIC TYPES, COORDINATES AND THERMAL PARAMETERS #-------------------------------------------------------------------------- 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 0 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' O O 0.0106 0.006 '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' 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 Mn1A Mn 0.66247(3) -0.016722(19) 0.126224(11) 0.02339(10) Uani 1 1 d . . . O1A O 0.92851(18) 0.01694(12) 0.13009(9) 0.0651(6) Uani 1 1 d . . . O2A O 0.59317(17) 0.12486(10) 0.08018(6) 0.0424(5) Uani 1 1 d . . . C1A C 0.8234(3) 0.00298(15) 0.12772(9) 0.0358(6) Uani 1 1 d . . . C2A C 0.6223(2) 0.06929(14) 0.09832(8) 0.0277(6) Uani 1 1 d . . . C5A C 0.6783(2) -0.09214(13) 0.07244(7) 0.0240(5) Uani 1 1 d . . . C6A C 0.5927(2) -0.05080(13) 0.05281(7) 0.0243(5) Uani 1 1 d . . . C7A C 0.4899(2) -0.02016(13) 0.01892(7) 0.0267(5) Uani 1 1 d . . . C11A C 0.5428(2) 0.00912(15) 0.17771(8) 0.0368(6) Uani 1 1 d . . . C12A C 0.6654(3) -0.00646(16) 0.20164(8) 0.0396(7) Uani 1 1 d . . . H12A H 0.7182 0.0258 0.2211 0.048 Uiso 1 1 calc R . . C13A C 0.6953(3) -0.07905(16) 0.19129(8) 0.0407(7) Uani 1 1 d . . . H13A H 0.7705 -0.1031 0.2026 0.049 Uiso 1 1 calc R . . C14A C 0.5908(3) -0.10812(16) 0.16076(8) 0.0396(7) Uani 1 1 d . . . H14A H 0.5843 -0.1552 0.1482 0.047 Uiso 1 1 calc R . . C15A C 0.4978(2) -0.05435(16) 0.15231(8) 0.0360(7) Uani 1 1 d . . . H15A H 0.4192 -0.0597 0.133 0.043 Uiso 1 1 calc R . . C16A C 0.4720(3) 0.07810(19) 0.18158(11) 0.0633(9) Uani 1 1 d . . . H16A H 0.43 0.0752 0.2088 0.095 Uiso 1 1 calc R . . H16B H 0.4111 0.085 0.1527 0.095 Uiso 1 1 calc R . . H16C H 0.5294 0.1185 0.1857 0.095 Uiso 1 1 calc R . . C21A C 0.7464(2) -0.15960(13) 0.06912(8) 0.0282(6) Uani 1 1 d . . . C22A C 0.7025(3) -0.20895(14) 0.03266(9) 0.0367(6) Uani 1 1 d . . . H22A H 0.6332 -0.1972 0.0093 0.044 Uiso 1 1 calc R . . C23A C 0.7620(3) -0.27598(16) 0.03096(11) 0.0518(8) Uani 1 1 d . . . H23A H 0.7311 -0.3093 0.0069 0.062 Uiso 1 1 calc R . . C24A C 0.8664(3) -0.29320(17) 0.06463(12) 0.0546(8) Uani 1 1 d . . . H24A H 0.9055 -0.3382 0.0635 0.066 Uiso 1 1 calc R . . C25A C 0.9121(3) -0.24413(17) 0.09952(11) 0.0510(8) Uani 1 1 d . . . H25A H 0.9841 -0.2553 0.1217 0.061 Uiso 1 1 calc R . . C26A C 0.8531(2) -0.17802(15) 0.10246(9) 0.0387(7) Uani 1 1 d . . . H26A H 0.8848 -0.1454 0.1269 0.046 Uiso 1 1 calc R . . C31A C 0.3621(2) -0.03266(14) 0.03077(7) 0.0279(6) Uani 1 1 d . . . C32A C 0.2815(3) 0.02426(16) 0.03612(9) 0.0417(7) Uani 1 1 d . . . H32A H 0.3044 0.0719 0.0304 0.05 Uiso 1 1 calc R . . C33A C 0.1668(3) 0.0105(2) 0.04995(10) 0.0577(9) Uani 1 1 d . . . H33A H 0.113 0.0489 0.0535 0.069 Uiso 1 1 calc R . . C34A C 0.1330(3) -0.0600(2) 0.05832(10) 0.0554(9) Uani 1 1 d . . . H34A H 0.0558 -0.0692 0.0673 0.067 Uiso 1 1 calc R . . C35A C 0.2118(3) -0.11656(18) 0.05347(8) 0.0440(7) Uani 1 1 d . . . H35A H 0.1887 -0.1641 0.0594 0.053 Uiso 1 1 calc R . . C36A C 0.3255(2) -0.10300(15) 0.03988(8) 0.0339(6) Uani 1 1 d . . . H36A H 0.3789 -0.1418 0.0367 0.041 Uiso 1 1 calc R . . Mn1B Mn 0.09812(3) 0.08163(2) 0.430043(11) 0.02566(10) Uani 1 1 d . . . Mn2B Mn 0.26729(3) -0.19398(2) 0.263547(11) 0.02215(10) Uani 1 1 d . . . O1B O -0.16225(19) 0.04296(13) 0.43554(6) 0.0524(5) Uani 1 1 d . . . O2B O 0.1702(2) -0.06887(11) 0.45737(6) 0.0601(6) Uani 1 1 d . . . O3B O -0.00648(18) -0.20289(14) 0.23703(7) 0.0617(6) Uani 1 1 d . . . O4B O 0.27954(19) -0.35168(11) 0.28058(7) 0.0497(5) Uani 1 1 d . . . C1B C -0.0597(3) 0.05884(14) 0.43353(8) 0.0334(6) Uani 1 1 d . . . C2B C 0.1401(3) -0.01002(16) 0.44658(8) 0.0373(7) Uani 1 1 d . . . C3B C 0.1011(3) -0.19965(16) 0.24992(8) 0.0378(7) Uani 1 1 d . . . C4B C 0.2731(2) -0.28940(15) 0.27396(8) 0.0311(6) Uani 1 1 d . . . C5B C 0.0340(2) 0.08731(13) 0.35601(7) 0.0225(5) Uani 1 1 d . . . C6B C 0.1162(2) 0.03891(13) 0.36083(7) 0.0229(5) Uani 1 1 d . . . C7B C 0.1997(2) -0.01666(13) 0.34845(7) 0.0208(5) Uani 1 1 d . . . C8B C 0.1612(2) -0.08665(13) 0.34008(7) 0.0204(5) Uani 1 1 d . . . C9B C 0.2458(2) -0.14345(13) 0.32994(7) 0.0211(5) Uani 1 1 d . . . C10B C 0.3262(2) -0.19211(13) 0.33857(7) 0.0215(5) Uani 1 1 d . . . C11B C 0.2714(2) 0.11696(15) 0.47465(8) 0.0387(6) Uani 1 1 d . . . C12B C 0.1685(3) 0.13315(17) 0.49695(10) 0.0493(8) Uani 1 1 d . . . H12C H 0.1548 0.1148 0.5263 0.059 Uiso 1 1 calc R . . C13B C 0.0900(3) 0.18176(17) 0.46718(12) 0.0565(9) Uani 1 1 d . . . H13B H 0.0156 0.2017 0.4736 0.068 Uiso 1 1 calc R . . C14B C 0.1429(3) 0.19523(16) 0.42620(11) 0.0502(8) Uani 1 1 d . . . H14B H 0.1098 0.2251 0.4004 0.06 Uiso 1 1 calc R . . C15B C 0.2549(2) 0.15541(15) 0.43117(9) 0.0394(7) Uani 1 1 d . . . H15B H 0.3094 0.1546 0.4091 0.047 Uiso 1 1 calc R . . C16B C 0.3829(3) 0.0704(2) 0.49449(12) 0.0658(10) Uani 1 1 d . . . H16D H 0.4177 0.05 0.4684 0.099 Uiso 1 1 calc R . . H16E H 0.3571 0.0316 0.5134 0.099 Uiso 1 1 calc R . . H16F H 0.4453 0.0996 0.5143 0.099 Uiso 1 1 calc R . . C21B C -0.0577(2) 0.12750(12) 0.32252(7) 0.0214(5) Uani 1 1 d . . . C22B C -0.0626(2) 0.11779(13) 0.27306(8) 0.0277(5) Uani 1 1 d . . . H22B H -0.0065 0.0861 0.2622 0.033 Uiso 1 1 calc R . . C23B C -0.1503(2) 0.15495(14) 0.24011(8) 0.0335(6) Uani 1 1 d . . . H23B H -0.1532 0.1478 0.2073 0.04 Uiso 1 1 calc R . . C24B C -0.2333(2) 0.20254(15) 0.25566(9) 0.0369(6) Uani 1 1 d . . . H24B H -0.2914 0.2279 0.2334 0.044 Uiso 1 1 calc R . . C25B C -0.2299(2) 0.21238(14) 0.30411(9) 0.0348(6) Uani 1 1 d . . . H25B H -0.2865 0.2441 0.3146 0.042 Uiso 1 1 calc R . . C26B C -0.1429(2) 0.17546(13) 0.33754(8) 0.0259(5) Uani 1 1 d . . . H26B H -0.1413 0.1827 0.3703 0.031 Uiso 1 1 calc R . . C31B C 0.3308(2) 0.00829(13) 0.34848(7) 0.0221(5) Uani 1 1 d . . . C32B C 0.4345(2) -0.02793(13) 0.37391(8) 0.0259(5) Uani 1 1 d . . . H32B H 0.4229 -0.0686 0.3923 0.031 Uiso 1 1 calc R . . C33B C 0.5545(2) -0.00406(15) 0.37210(9) 0.0358(6) Uani 1 1 d . . . H33B H 0.6232 -0.0289 0.3892 0.043 Uiso 1 1 calc R . . C34B C 0.5736(2) 0.05628(16) 0.34515(10) 0.0421(7) Uani 1 1 d . . . H34B H 0.6547 0.0715 0.3435 0.05 Uiso 1 1 calc R . . C35B C 0.4713(3) 0.09404(15) 0.32069(9) 0.0392(7) Uani 1 1 d . . . H35B H 0.4835 0.1352 0.3028 0.047 Uiso 1 1 calc R . . C36B C 0.3510(2) 0.07082(14) 0.32282(8) 0.0304(6) Uani 1 1 d . . . H36B H 0.2825 0.0972 0.3069 0.036 Uiso 1 1 calc R . . C41B C 0.0312(2) -0.11108(12) 0.34224(7) 0.0212(5) Uani 1 1 d . . . C42B C 0.0121(2) -0.17241(14) 0.36916(8) 0.0315(6) Uani 1 1 d . . . H42B H 0.0809 -0.1994 0.3841 0.038 Uiso 1 1 calc R . . C43B C -0.1072(2) -0.19392(16) 0.37407(9) 0.0405(7) Uani 1 1 d . . . H43B H -0.1181 -0.2342 0.393 0.049 Uiso 1 1 calc R . . C44B C -0.2102(2) -0.15570(15) 0.35098(9) 0.0394(7) Uani 1 1 d . . . H44B H -0.2907 -0.1699 0.3545 0.047 Uiso 1 1 calc R . . C45B C -0.1937(2) -0.09637(15) 0.32269(9) 0.0347(6) Uani 1 1 d . . . H45B H -0.2631 -0.0711 0.3066 0.042 Uiso 1 1 calc R . . C46B C -0.0742(2) -0.07445(13) 0.31827(8) 0.0270(5) Uani 1 1 d . . . H46B H -0.064 -0.0346 0.299 0.032 Uiso 1 1 calc R . . C51B C 0.4177(2) -0.23134(13) 0.37326(7) 0.0240(5) Uani 1 1 d . . . C52B C 0.5128(2) -0.27166(13) 0.35910(8) 0.0291(6) Uani 1 1 d . . . H52B H 0.5164 -0.2757 0.3265 0.035 Uiso 1 1 calc R . . C53B C 0.6023(2) -0.30585(16) 0.39254(9) 0.0405(7) Uani 1 1 d . . . H53B H 0.6664 -0.3322 0.3825 0.049 Uiso 1 1 calc R . . C54B C 0.5972(3) -0.30115(19) 0.44033(10) 0.0578(9) Uani 1 1 d . . . H54B H 0.6578 -0.3242 0.4629 0.069 Uiso 1 1 calc R . . C55B C 0.5029(3) -0.2625(2) 0.45505(10) 0.0705(11) Uani 1 1 d . . . H55B H 0.4991 -0.2598 0.4877 0.085 Uiso 1 1 calc R . . C56B C 0.4130(3) -0.22726(17) 0.42180(8) 0.0472(8) Uani 1 1 d . . . H56B H 0.3494 -0.2009 0.4322 0.057 Uiso 1 1 calc R . . C61B C 0.2693(2) -0.10509(14) 0.21310(8) 0.0326(6) Uani 1 1 d . . . C62B C 0.3751(2) -0.09846(15) 0.24965(8) 0.0353(6) Uani 1 1 d . . . H62B H 0.3927 -0.0588 0.2703 0.042 Uiso 1 1 calc R . . C63B C 0.4494(2) -0.16020(17) 0.25025(9) 0.0419(7) Uani 1 1 d . . . H63B H 0.5242 -0.1691 0.2714 0.05 Uiso 1 1 calc R . . C64B C 0.3929(3) -0.20623(16) 0.21407(10) 0.0449(7) Uani 1 1 d . . . H64B H 0.4235 -0.2513 0.2064 0.054 Uiso 1 1 calc R . . C65B C 0.2820(3) -0.17348(16) 0.19090(8) 0.0414(7) Uani 1 1 d . . . H65B H 0.2259 -0.1931 0.1653 0.05 Uiso 1 1 calc R . . C66B C 0.1700(3) -0.0483(2) 0.19910(14) 0.0752(11) Uani 1 1 d . . . H66A H 0.1571 -0.0221 0.2273 0.113 Uiso 1 1 calc R . . H66B H 0.0929 -0.0715 0.1845 0.113 Uiso 1 1 calc R . . H66C H 0.1962 -0.0151 0.1765 0.113 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 Mn1A 0.02564(19) 0.0231(2) 0.02057(17) 0.00025(14) 0.00181(14) -0.00265(16) O1A 0.0246(11) 0.0595(16) 0.1066(18) 0.0187(13) -0.0007(11) -0.0044(10) O2A 0.0492(11) 0.0237(11) 0.0507(11) 0.0023(9) -0.0008(9) 0.0014(9) C1A 0.0352(17) 0.0277(16) 0.0418(14) 0.0070(11) -0.0005(12) 0.0014(12) C2A 0.0255(13) 0.0256(16) 0.0311(12) -0.0067(11) 0.0024(10) -0.0029(11) C5A 0.0280(13) 0.0228(14) 0.0216(11) 0.0022(10) 0.0054(10) -0.0024(11) C6A 0.0301(13) 0.0240(14) 0.0191(11) -0.0007(10) 0.0049(10) -0.0047(12) C7A 0.0341(13) 0.0239(13) 0.0201(10) -0.0030(9) -0.0003(10) 0.0002(11) C11A 0.0456(16) 0.0418(17) 0.0257(12) -0.0018(12) 0.0134(12) 0.0017(14) C12A 0.0484(17) 0.0482(19) 0.0207(12) -0.0057(11) 0.0016(11) -0.0123(14) C13A 0.0500(17) 0.0459(19) 0.0263(13) 0.0100(12) 0.0066(12) 0.0028(15) C14A 0.0612(18) 0.0337(17) 0.0274(13) 0.0014(11) 0.0177(13) -0.0122(15) C15A 0.0330(15) 0.057(2) 0.0210(12) -0.0008(12) 0.0113(11) -0.0108(14) C16A 0.075(2) 0.067(2) 0.0553(18) -0.0058(16) 0.0304(17) 0.0177(19) C21A 0.0337(14) 0.0233(14) 0.0306(12) 0.0054(10) 0.0142(11) -0.0016(11) C22A 0.0454(16) 0.0286(16) 0.0398(14) -0.0028(12) 0.0181(12) -0.0060(13) C23A 0.074(2) 0.0314(18) 0.0612(18) -0.0130(14) 0.0424(18) -0.0104(16) C24A 0.064(2) 0.0332(19) 0.076(2) 0.0129(17) 0.0397(18) 0.0179(16) C25A 0.0517(18) 0.044(2) 0.0607(18) 0.0152(16) 0.0195(15) 0.0187(16) C26A 0.0415(16) 0.0344(17) 0.0418(14) 0.0082(12) 0.0122(13) 0.0100(13) C31A 0.0280(13) 0.0379(16) 0.0171(11) 0.0004(10) 0.0020(9) -0.0043(12) C32A 0.0466(17) 0.0438(19) 0.0381(14) 0.0120(13) 0.0167(13) 0.0050(14) C33A 0.0484(19) 0.074(3) 0.0571(18) 0.0125(17) 0.0257(15) 0.0203(18) C34A 0.0401(18) 0.086(3) 0.0430(16) 0.0066(16) 0.0139(14) -0.0158(18) C35A 0.0499(18) 0.054(2) 0.0280(13) -0.0010(13) 0.0071(12) -0.0190(16) C36A 0.0337(14) 0.0384(17) 0.0276(12) -0.0053(11) 0.0002(11) -0.0067(13) Mn1B 0.0287(2) 0.0234(2) 0.02363(18) -0.00281(15) 0.00120(14) 0.00354(16) Mn2B 0.02211(19) 0.0250(2) 0.01921(17) -0.00230(14) 0.00348(14) -0.00046(16) O1B 0.0396(12) 0.0770(16) 0.0435(11) -0.0003(10) 0.0152(9) -0.0142(11) O2B 0.1105(18) 0.0330(13) 0.0315(10) 0.0074(9) -0.0019(11) 0.0229(12) O3B 0.0244(11) 0.099(2) 0.0576(12) -0.0273(12) -0.0029(9) -0.0109(11) O4B 0.0738(14) 0.0260(13) 0.0500(11) -0.0067(9) 0.0134(10) -0.0112(11) C1B 0.0437(17) 0.0343(16) 0.0220(12) 0.0003(10) 0.0056(11) 0.0025(13) C2B 0.0549(17) 0.0385(19) 0.0161(11) -0.0002(11) -0.0002(11) 0.0090(14) C3B 0.0380(17) 0.0465(18) 0.0287(13) -0.0133(12) 0.0053(12) -0.0030(13) C4B 0.0365(14) 0.0315(18) 0.0267(12) -0.0096(11) 0.0098(11) -0.0069(12) C5B 0.0235(12) 0.0199(13) 0.0249(11) -0.0004(10) 0.0060(9) -0.0014(11) C6B 0.0245(13) 0.0219(14) 0.0223(11) 0.0008(9) 0.0038(9) -0.0019(11) C7B 0.0231(12) 0.0217(14) 0.0170(10) 0.0023(9) 0.0020(9) 0.0043(10) C8B 0.0226(12) 0.0238(14) 0.0149(10) 0.0011(9) 0.0036(9) 0.0048(10) C9B 0.0246(12) 0.0205(13) 0.0184(10) -0.0028(9) 0.0043(9) -0.0036(11) C10B 0.0246(12) 0.0206(13) 0.0202(11) -0.0009(9) 0.0065(9) -0.0004(11) C11B 0.0378(15) 0.0398(17) 0.0329(13) -0.0104(12) -0.0089(12) -0.0022(13) C12B 0.0587(19) 0.053(2) 0.0360(14) -0.0224(14) 0.0076(14) -0.0084(17) C13B 0.0397(17) 0.042(2) 0.086(2) -0.0371(17) 0.0063(17) 0.0043(15) C14B 0.0545(19) 0.0239(17) 0.0633(19) -0.0058(13) -0.0142(16) -0.0047(15) C15B 0.0392(16) 0.0360(17) 0.0400(14) -0.0079(12) -0.0013(12) -0.0114(13) C16B 0.0503(19) 0.071(3) 0.064(2) -0.0057(17) -0.0243(16) 0.0093(18) C21B 0.0227(12) 0.0151(13) 0.0264(11) 0.0023(9) 0.0048(9) -0.0028(10) C22B 0.0317(13) 0.0230(14) 0.0297(12) 0.0021(10) 0.0092(10) 0.0001(11) C23B 0.0397(15) 0.0355(16) 0.0241(12) 0.0079(11) 0.0023(11) -0.0098(13) C24B 0.0330(14) 0.0305(16) 0.0424(15) 0.0138(12) -0.0059(12) -0.0007(13) C25B 0.0286(14) 0.0292(16) 0.0457(15) 0.0043(12) 0.0038(11) 0.0070(12) C26B 0.0245(12) 0.0236(14) 0.0295(12) 0.0021(10) 0.0043(10) 0.0025(11) C31B 0.0260(12) 0.0214(14) 0.0184(10) -0.0050(9) 0.0025(9) -0.0002(10) C32B 0.0267(13) 0.0246(14) 0.0249(11) -0.0026(10) 0.0004(10) -0.0013(11) C33B 0.0248(13) 0.0406(18) 0.0395(14) -0.0077(12) -0.0007(11) -0.0001(12) C34B 0.0293(15) 0.049(2) 0.0491(16) -0.0115(14) 0.0114(13) -0.0163(14) C35B 0.0492(17) 0.0335(17) 0.0375(14) -0.0016(12) 0.0149(13) -0.0144(14) C36B 0.0335(14) 0.0289(15) 0.0282(12) 0.0013(10) 0.0041(10) -0.0017(12) C41B 0.0226(12) 0.0193(13) 0.0220(11) -0.0033(9) 0.0050(9) 0.0013(10) C42B 0.0314(14) 0.0281(15) 0.0346(13) 0.0058(11) 0.0050(11) 0.0042(12) C43B 0.0421(16) 0.0343(17) 0.0478(15) 0.0084(13) 0.0149(13) -0.0093(14) C44B 0.0283(14) 0.0434(18) 0.0483(15) -0.0039(13) 0.0115(12) -0.0080(13) C45B 0.0238(13) 0.0376(17) 0.0411(14) -0.0030(12) 0.0016(11) 0.0017(12) C46B 0.0280(13) 0.0233(14) 0.0297(12) 0.0006(10) 0.0046(10) -0.0021(11) C51B 0.0278(13) 0.0195(13) 0.0239(11) 0.0018(10) 0.0023(10) 0.0016(11) C52B 0.0321(14) 0.0292(15) 0.0269(12) 0.0043(10) 0.0075(10) 0.0080(12) C53B 0.0385(15) 0.0399(18) 0.0431(15) 0.0090(13) 0.0076(12) 0.0171(14) C54B 0.060(2) 0.070(2) 0.0392(16) 0.0146(15) -0.0006(14) 0.0352(18) C55B 0.085(2) 0.100(3) 0.0250(14) 0.0128(16) 0.0056(15) 0.047(2) C56B 0.0562(18) 0.061(2) 0.0247(13) 0.0032(13) 0.0085(12) 0.0279(16) C61B 0.0353(14) 0.0354(16) 0.0286(12) 0.0119(11) 0.0095(11) 0.0076(12) C62B 0.0497(16) 0.0354(17) 0.0229(12) 0.0006(11) 0.0117(11) -0.0154(14) C63B 0.0256(14) 0.062(2) 0.0396(15) 0.0228(14) 0.0098(12) -0.0014(14) C64B 0.0613(19) 0.0341(17) 0.0492(16) 0.0118(14) 0.0366(15) 0.0151(15) C65B 0.0571(18) 0.0489(19) 0.0176(12) -0.0045(11) 0.0050(12) -0.0145(15) C66B 0.062(2) 0.072(3) 0.094(3) 0.044(2) 0.0196(19) 0.031(2) #-------------------------------------------------------------------------- # MOLECULAR GEOMETRY #-------------------------------------------------------------------------- _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 Mn1A C1A 1.770(3) . ? Mn1A C2A 1.781(3) . ? Mn1A C5A 2.082(2) . ? Mn1A C12A 2.130(2) . ? Mn1A C13A 2.137(2) . ? Mn1A C14A 2.151(3) . ? Mn1A C15A 2.157(2) . ? Mn1A C11A 2.163(2) . ? Mn1A C6A 2.166(2) . ? O1A C1A 1.156(3) . ? O2A C2A 1.158(3) . ? C5A C6A 1.247(3) . ? C5A C21A 1.451(3) . ? C6A C7A 1.445(3) . ? C7A C7A 1.348(5) 3_655 ? C7A C31A 1.496(3) . ? C11A C12A 1.406(4) . ? C11A C15A 1.407(4) . ? C11A C16A 1.492(4) . ? C12A C13A 1.412(4) . ? C13A C14A 1.399(4) . ? C14A C15A 1.398(4) . ? C21A C22A 1.389(3) . ? C21A C26A 1.395(3) . ? C22A C23A 1.392(4) . ? C23A C24A 1.377(4) . ? C24A C25A 1.360(4) . ? C25A C26A 1.379(4) . ? C31A C32A 1.385(4) . ? C31A C36A 1.386(4) . ? C32A C33A 1.388(4) . ? C33A C34A 1.376(5) . ? C34A C35A 1.365(4) . ? C35A C36A 1.374(4) . ? Mn1B C1B 1.777(3) . ? Mn1B C2B 1.781(3) . ? Mn1B C5B 2.083(2) . ? Mn1B C13B 2.123(3) . ? Mn1B C12B 2.126(3) . ? Mn1B C6B 2.144(2) . ? Mn1B C14B 2.145(3) . ? Mn1B C11B 2.163(2) . ? Mn1B C15B 2.165(3) . ? Mn2B C4B 1.773(3) . ? Mn2B C3B 1.773(3) . ? Mn2B C10B 2.099(2) . ? Mn2B C65B 2.117(2) . ? Mn2B C64B 2.126(2) . ? Mn2B C9B 2.139(2) . ? Mn2B C63B 2.160(2) . ? Mn2B C61B 2.166(2) . ? Mn2B C62B 2.178(2) . ? O1B C1B 1.158(3) . ? O2B C2B 1.152(3) . ? O3B C3B 1.157(3) . ? O4B C4B 1.157(3) . ? C5B C6B 1.246(3) . ? C5B C21B 1.444(3) . ? C6B C7B 1.445(3) . ? C7B C8B 1.357(3) . ? C7B C31B 1.490(3) . ? C8B C9B 1.448(3) . ? C8B C41B 1.487(3) . ? C9B C10B 1.239(3) . ? C10B C51B 1.453(3) . ? C11B C15B 1.398(4) . ? C11B C12B 1.404(4) . ? C11B C16B 1.503(4) . ? C12B C13B 1.402(4) . ? C13B C14B 1.400(4) . ? C14B C15B 1.399(4) . ? C21B C26B 1.393(3) . ? C21B C22B 1.398(3) . ? C22B C23B 1.383(3) . ? C23B C24B 1.378(4) . ? C24B C25B 1.373(4) . ? C25B C26B 1.385(3) . ? C31B C32B 1.388(3) . ? C31B C36B 1.393(3) . ? C32B C33B 1.379(3) . ? C33B C34B 1.378(4) . ? C34B C35B 1.381(4) . ? C35B C36B 1.381(4) . ? C41B C46B 1.390(3) . ? C41B C42B 1.393(3) . ? C42B C43B 1.379(3) . ? C43B C44B 1.378(4) . ? C44B C45B 1.379(4) . ? C45B C46B 1.380(3) . ? C51B C56B 1.381(3) . ? C51B C52B 1.382(3) . ? C52B C53B 1.377(3) . ? C53B C54B 1.362(4) . ? C54B C55B 1.366(4) . ? C55B C56B 1.385(4) . ? C61B C62B 1.402(3) . ? C61B C65B 1.419(4) . ? C61B C66B 1.498(4) . ? C62B C63B 1.386(4) . ? C63B C64B 1.380(4) . ? C64B C65B 1.396(4) . ? 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 C1A Mn1A C2A 89.52(11) . . ? C1A Mn1A C5A 86.84(11) . . ? C2A Mn1A C5A 108.12(10) . . ? C1A Mn1A C12A 96.79(11) . . ? C2A Mn1A C12A 108.80(11) . . ? C5A Mn1A C12A 142.92(10) . . ? C1A Mn1A C13A 94.36(11) . . ? C2A Mn1A C13A 147.45(11) . . ? C5A Mn1A C13A 104.36(10) . . ? C12A Mn1A C13A 38.65(10) . . ? C1A Mn1A C14A 125.45(11) . . ? C2A Mn1A C14A 144.14(11) . . ? C5A Mn1A C14A 84.02(9) . . ? C12A Mn1A C14A 63.83(10) . . ? C13A Mn1A C14A 38.08(10) . . ? C1A Mn1A C15A 157.60(10) . . ? C2A Mn1A C15A 106.40(11) . . ? C5A Mn1A C15A 102.47(9) . . ? C12A Mn1A C15A 63.53(10) . . ? C13A Mn1A C15A 63.74(10) . . ? C14A Mn1A C15A 37.87(10) . . ? C1A Mn1A C11A 129.98(11) . . ? C2A Mn1A C11A 88.54(10) . . ? C5A Mn1A C11A 140.47(10) . . ? C12A Mn1A C11A 38.24(10) . . ? C13A Mn1A C11A 64.44(10) . . ? C14A Mn1A C11A 63.86(11) . . ? C15A Mn1A C11A 38.01(10) . . ? C1A Mn1A C6A 104.80(10) . . ? C2A Mn1A C6A 79.44(10) . . ? C5A Mn1A C6A 34.08(9) . . ? C12A Mn1A C6A 157.06(10) . . ? C13A Mn1A C6A 130.03(10) . . ? C14A Mn1A C6A 96.66(9) . . ? C15A Mn1A C6A 93.75(9) . . ? C11A Mn1A C6A 123.82(9) . . ? O1A C1A Mn1A 177.8(3) . . ? O2A C2A Mn1A 178.4(2) . . ? C6A C5A C21A 146.5(2) . . ? C6A C5A Mn1A 76.66(15) . . ? C21A C5A Mn1A 136.18(16) . . ? C5A C6A C7A 162.4(2) . . ? C5A C6A Mn1A 69.26(14) . . ? C7A C6A Mn1A 128.08(17) . . ? C7A C7A C6A 121.5(3) 3_655 . ? C7A C7A C31A 123.2(3) 3_655 . ? C6A C7A C31A 115.17(19) . . ? C12A C11A C15A 106.7(2) . . ? C12A C11A C16A 126.1(3) . . ? C15A C11A C16A 127.1(3) . . ? C12A C11A Mn1A 69.61(14) . . ? C15A C11A Mn1A 70.77(13) . . ? C16A C11A Mn1A 127.66(19) . . ? C11A C12A C13A 108.9(2) . . ? C11A C12A Mn1A 72.15(13) . . ? C13A C12A Mn1A 70.95(14) . . ? C14A C13A C12A 107.2(2) . . ? C14A C13A Mn1A 71.48(14) . . ? C12A C13A Mn1A 70.40(14) . . ? C15A C14A C13A 108.3(2) . . ? C15A C14A Mn1A 71.32(15) . . ? C13A C14A Mn1A 70.44(15) . . ? C14A C15A C11A 108.9(2) . . ? C14A C15A Mn1A 70.81(14) . . ? C11A C15A Mn1A 71.22(14) . . ? C22A C21A C26A 118.3(2) . . ? C22A C21A C5A 119.5(2) . . ? C26A C21A C5A 122.1(2) . . ? C21A C22A C23A 120.1(3) . . ? C24A C23A C22A 120.4(3) . . ? C25A C24A C23A 119.7(3) . . ? C24A C25A C26A 120.8(3) . . ? C25A C26A C21A 120.6(3) . . ? C32A C31A C36A 118.3(2) . . ? C32A C31A C7A 122.2(2) . . ? C36A C31A C7A 119.3(2) . . ? C31A C32A C33A 120.3(3) . . ? C34A C33A C32A 119.8(3) . . ? C35A C34A C33A 120.4(3) . . ? C34A C35A C36A 119.8(3) . . ? C35A C36A C31A 121.3(3) . . ? C1B Mn1B C2B 88.08(12) . . ? C1B Mn1B C5B 85.15(9) . . ? C2B Mn1B C5B 109.50(10) . . ? C1B Mn1B C13B 92.96(12) . . ? C2B Mn1B C13B 135.84(12) . . ? C5B Mn1B C13B 114.58(12) . . ? C1B Mn1B C12B 104.54(11) . . ? C2B Mn1B C12B 98.75(12) . . ? C5B Mn1B C12B 150.51(11) . . ? C13B Mn1B C12B 38.53(12) . . ? C1B Mn1B C6B 102.04(10) . . ? C2B Mn1B C6B 80.43(9) . . ? C5B Mn1B C6B 34.26(8) . . ? C13B Mn1B C6B 141.57(12) . . ? C12B Mn1B C6B 153.37(10) . . ? C1B Mn1B C14B 117.32(12) . . ? C2B Mn1B C14B 151.60(12) . . ? C5B Mn1B C14B 86.49(10) . . ? C13B Mn1B C14B 38.29(12) . . ? C12B Mn1B C14B 64.23(12) . . ? C6B Mn1B C14B 104.51(11) . . ? C1B Mn1B C11B 141.24(10) . . ? C2B Mn1B C11B 88.62(11) . . ? C5B Mn1B C11B 131.92(10) . . ? C13B Mn1B C11B 63.98(11) . . ? C12B Mn1B C11B 38.21(10) . . ? C6B Mn1B C11B 115.41(9) . . ? C14B Mn1B C11B 63.79(11) . . ? C1B Mn1B C15B 154.65(12) . . ? C2B Mn1B C15B 115.03(12) . . ? C5B Mn1B C15B 95.96(9) . . ? C13B Mn1B C15B 63.47(12) . . ? C12B Mn1B C15B 63.49(11) . . ? C6B Mn1B C15B 92.49(9) . . ? C14B Mn1B C15B 37.89(11) . . ? C11B Mn1B C15B 37.70(10) . . ? C4B Mn2B C3B 89.01(13) . . ? C4B Mn2B C10B 81.59(10) . . ? C3B Mn2B C10B 109.49(10) . . ? C4B Mn2B C65B 109.20(11) . . ? C3B Mn2B C65B 92.77(11) . . ? C10B Mn2B C65B 155.70(10) . . ? C4B Mn2B C64B 89.80(11) . . ? C3B Mn2B C64B 126.38(11) . . ? C10B Mn2B C64B 123.29(10) . . ? C65B Mn2B C64B 38.41(11) . . ? C4B Mn2B C9B 106.77(9) . . ? C3B Mn2B C9B 87.21(10) . . ? C10B Mn2B C9B 33.99(8) . . ? C65B Mn2B C9B 144.03(10) . . ? C64B Mn2B C9B 143.35(11) . . ? C4B Mn2B C63B 107.76(11) . . ? C3B Mn2B C63B 154.11(11) . . ? C10B Mn2B C63B 92.74(9) . . ? C65B Mn2B C63B 63.46(10) . . ? C64B Mn2B C63B 37.56(11) . . ? C9B Mn2B C63B 105.80(10) . . ? C4B Mn2B C61B 147.86(10) . . ? C3B Mn2B C61B 91.73(11) . . ? C10B Mn2B C61B 127.83(9) . . ? C65B Mn2B C61B 38.67(10) . . ? C64B Mn2B C61B 64.26(10) . . ? C9B Mn2B C61B 105.36(9) . . ? C63B Mn2B C61B 63.52(10) . . ? C4B Mn2B C62B 144.96(11) . . ? C3B Mn2B C62B 124.25(12) . . ? C10B Mn2B C62B 95.29(9) . . ? C65B Mn2B C62B 63.14(10) . . ? C64B Mn2B C62B 62.71(11) . . ? C9B Mn2B C62B 87.39(9) . . ? C63B Mn2B C62B 37.27(10) . . ? C61B Mn2B C62B 37.67(9) . . ? O1B C1B Mn1B 179.0(3) . . ? O2B C2B Mn1B 178.4(3) . . ? O3B C3B Mn2B 174.3(2) . . ? O4B C4B Mn2B 178.5(2) . . ? C6B C5B C21B 145.9(2) . . ? C6B C5B Mn1B 75.59(14) . . ? C21B C5B Mn1B 138.50(16) . . ? C5B C6B C7B 160.1(2) . . ? C5B C6B Mn1B 70.16(14) . . ? C7B C6B Mn1B 129.77(15) . . ? C8B C7B C6B 121.5(2) . . ? C8B C7B C31B 123.6(2) . . ? C6B C7B C31B 114.8(2) . . ? C7B C8B C9B 122.0(2) . . ? C7B C8B C41B 122.7(2) . . ? C9B C8B C41B 115.3(2) . . ? C10B C9B C8B 157.6(2) . . ? C10B C9B Mn2B 71.26(13) . . ? C8B C9B Mn2B 130.95(15) . . ? C9B C10B C51B 149.2(2) . . ? C9B C10B Mn2B 74.75(13) . . ? C51B C10B Mn2B 135.99(16) . . ? C15B C11B C12B 107.4(3) . . ? C15B C11B C16B 125.6(3) . . ? C12B C11B C16B 127.0(3) . . ? C15B C11B Mn1B 71.23(14) . . ? C12B C11B Mn1B 69.51(15) . . ? C16B C11B Mn1B 127.0(2) . . ? C13B C12B C11B 108.0(3) . . ? C13B C12B Mn1B 70.60(15) . . ? C11B C12B Mn1B 72.29(14) . . ? C14B C13B C12B 108.3(3) . . ? C14B C13B Mn1B 71.72(16) . . ? C12B C13B Mn1B 70.87(16) . . ? C15B C14B C13B 107.4(3) . . ? C15B C14B Mn1B 71.81(16) . . ? C13B C14B Mn1B 69.99(17) . . ? C11B C15B C14B 108.9(3) . . ? C11B C15B Mn1B 71.06(15) . . ? C14B C15B Mn1B 70.30(16) . . ? C26B C21B C22B 118.3(2) . . ? C26B C21B C5B 122.51(19) . . ? C22B C21B C5B 119.2(2) . . ? C23B C22B C21B 120.5(2) . . ? C24B C23B C22B 120.4(2) . . ? C25B C24B C23B 119.8(2) . . ? C24B C25B C26B 120.5(2) . . ? C25B C26B C21B 120.5(2) . . ? C32B C31B C36B 118.4(2) . . ? C32B C31B C7B 122.3(2) . . ? C36B C31B C7B 119.3(2) . . ? C33B C32B C31B 120.5(2) . . ? C34B C33B C32B 120.6(2) . . ? C33B C34B C35B 119.5(2) . . ? C34B C35B C36B 120.1(2) . . ? C35B C36B C31B 120.8(2) . . ? C46B C41B C42B 117.8(2) . . ? C46B C41B C8B 122.3(2) . . ? C42B C41B C8B 119.9(2) . . ? C43B C42B C41B 121.2(2) . . ? C44B C43B C42B 119.9(2) . . ? C43B C44B C45B 119.8(2) . . ? C44B C45B C46B 120.1(2) . . ? C45B C46B C41B 121.0(2) . . ? C56B C51B C52B 118.4(2) . . ? C56B C51B C10B 120.0(2) . . ? C52B C51B C10B 121.54(19) . . ? C53B C52B C51B 120.9(2) . . ? C54B C53B C52B 120.1(2) . . ? C53B C54B C55B 119.8(3) . . ? C54B C55B C56B 120.6(3) . . ? C51B C56B C55B 120.0(3) . . ? C62B C61B C65B 105.7(2) . . ? C62B C61B C66B 125.9(3) . . ? C65B C61B C66B 128.2(3) . . ? C62B C61B Mn2B 71.61(14) . . ? C65B C61B Mn2B 68.80(14) . . ? C66B C61B Mn2B 127.24(19) . . ? C63B C62B C61B 109.5(2) . . ? C63B C62B Mn2B 70.67(15) . . ? C61B C62B Mn2B 70.71(14) . . ? C64B C63B C62B 108.1(2) . . ? C64B C63B Mn2B 69.88(15) . . ? C62B C63B Mn2B 72.06(14) . . ? C63B C64B C65B 108.3(2) . . ? C63B C64B Mn2B 72.56(14) . . ? C65B C64B Mn2B 70.46(14) . . ? C64B C65B C61B 108.4(2) . . ? C64B C65B Mn2B 71.13(14) . . ? C61B C65B Mn2B 72.53(13) . . ? # CIF produced by WinGX routine CIF_UPDATE # Created on 2001-09-17 at 14:30:18 # Using CIFtbx version 2.6.2 16 Jun 1998 # Dictionary name : cif_core.dic # Dictionary vers : 2.2 # Request file : C:\Progra~1\wingx\files\archive.dat # CIF files read : nn3 data_nn3 _database_code_CSD 201835 _audit_creation_date 2001-09-17T14:30:18-00:00 _audit_creation_method 'WinGX routine CIF_UPDATE' #-------------------------------------------------------------------------- # CHEMICAL INFORMATION # #-------------------------------------------------------------------------- _chemical_name_systematic ; ? ; _chemical_formula_sum 'C48 H38 Mn2 O4' _chemical_formula_weight 788.66 #-------------------------------------------------------------------------- # UNIT CELL INFORMATION # #-------------------------------------------------------------------------- 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' _symmetry_cell_setting monoclinic _symmetry_space_group_name_H-M 'P 21/n' _cell_length_a 11.3732(16) _cell_length_b 18.282(3) _cell_length_c 19.260(5) _cell_angle_alpha 90 _cell_angle_beta 106.65(2) _cell_angle_gamma 90 _cell_volume 3836.8(12) _cell_formula_units_Z 4 _cell_measurement_temperature 293(2) #-------------------------------------------------------------------------- # CRYSTAL INFORMATION # #------------------------------------------------------------------------- _exptl_crystal_colour red _exptl_crystal_description needle _exptl_crystal_size_min ? _exptl_crystal_size_mid ? _exptl_crystal_size_max ? _exptl_crystal_size_rad ? _exptl_crystal_density_diffrn 1.365 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1632 _exptl_special_details ; ? ; #-------------------------------------------------------------------------- # ABSORPTION CORRECTION # #-------------------------------------------------------------------------- _exptl_absorpt_coefficient_mu 0.703 #-------------------------------------------------------------------------- # DATA COLLECTION # #-------------------------------------------------------------------------- _diffrn_ambient_temperature 293(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_monochromator graphite _diffrn_reflns_av_unetI/netI 0.051 _diffrn_reflns_number 28664 _diffrn_reflns_limit_h_min -13 _diffrn_reflns_limit_h_max 12 _diffrn_reflns_limit_k_min -22 _diffrn_reflns_limit_k_max 21 _diffrn_reflns_limit_l_min -23 _diffrn_reflns_limit_l_max 23 _diffrn_reflns_theta_min 2.18 _diffrn_reflns_theta_max 26.09 _diffrn_reflns_theta_full 26.09 _diffrn_measured_fraction_theta_full 0.975 _diffrn_measured_fraction_theta_max 0.975 _reflns_number_total 7405 _reflns_number_gt 5276 _reflns_threshold_expression >2sigma(I) #-------------------------------------------------------------------------- # COMPUTER PROGRAMS USED #-------------------------------------------------------------------------- _computing_structure_solution 'SIR-92 (Giacovazzo, 1993)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'Ortep-3 for Windows (Farrugia, 1997)' _computing_publication_material 'WinGX (Farrugia, 1999)' #-------------------------------------------------------------------------- # REFINEMENT INFORMATION #-------------------------------------------------------------------------- _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^)+(0.0635P)^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 7405 _refine_ls_number_parameters 491 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0717 _refine_ls_R_factor_gt 0.0447 _refine_ls_wR_factor_ref 0.1067 _refine_ls_wR_factor_gt 0.096 _refine_ls_goodness_of_fit_ref 0.998 _refine_ls_restrained_S_all 0.998 _refine_ls_shift/su_max 0.008 _refine_ls_shift/su_mean 0.001 _refine_diff_density_max 0.384 _refine_diff_density_min -0.467 _refine_diff_density_rms 0.06 #-------------------------------------------------------------------------- # ATOMIC TYPES, COORDINATES AND THERMAL PARAMETERS # #-------------------------------------------------------------------------- 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 0 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' O O 0.0106 0.006 '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' 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 0.79909(3) 0.12513(2) 0.70477(2) 0.02781(11) Uani 1 1 d . . . Mn2 Mn 0.92767(3) 0.34561(2) 0.418584(19) 0.02636(11) Uani 1 1 d . . . O1 O 0.5653(2) 0.18360(15) 0.71506(13) 0.0624(7) Uani 1 1 d . . . O2 O 0.6776(2) 0.09360(13) 0.55182(11) 0.0523(5) Uani 1 1 d . . . O3 O 1.1685(2) 0.30678(16) 0.40492(13) 0.0628(7) Uani 1 1 d . . . O4 O 1.0580(2) 0.37012(11) 0.57131(11) 0.0492(5) Uani 1 1 d . . . C1 C 0.6595(3) 0.16246(17) 0.71107(15) 0.0397(7) Uani 1 1 d . . . C2 C 0.7254(2) 0.10715(15) 0.61192(15) 0.0361(6) Uani 1 1 d . . . C3 C 1.0711(3) 0.31948(16) 0.40930(14) 0.0367(6) Uani 1 1 d . . . C4 C 1.0060(3) 0.35959(13) 0.51143(15) 0.0339(6) Uani 1 1 d . . . C5 C 0.8719(2) 0.23104(14) 0.71873(13) 0.0291(5) Uani 1 1 d . . . C6 C 0.8826(2) 0.21175(14) 0.65887(13) 0.0305(5) Uani 1 1 d . . . C7 C 0.9099(2) 0.21460(14) 0.59054(13) 0.0287(5) Uani 1 1 d . . . C8 C 0.8326(2) 0.24803(13) 0.53239(13) 0.0273(5) Uani 1 1 d . . . C9 C 0.8608(2) 0.25063(13) 0.46458(13) 0.0278(5) Uani 1 1 d . . . C10 C 0.8750(2) 0.23516(13) 0.40428(13) 0.0281(5) Uani 1 1 d . . . C11 C 0.8834(3) 0.01773(14) 0.71124(15) 0.0359(6) Uani 1 1 d . . . C12 C 0.7933(3) 0.01903(16) 0.74947(15) 0.0411(7) Uani 1 1 d . . . H12 H 0.7224 -0.0093 0.739 0.049 Uiso 1 1 calc R . . C13 C 0.8303(3) 0.07074(16) 0.80606(15) 0.0420(7) Uani 1 1 d . . . H13 H 0.7883 0.0819 0.8396 0.05 Uiso 1 1 calc R . . C14 C 0.9409(3) 0.10229(16) 0.80299(14) 0.0376(6) Uani 1 1 d . . . H14 H 0.9849 0.1382 0.8339 0.045 Uiso 1 1 calc R . . C15 C 0.9737(2) 0.06980(15) 0.74463(14) 0.0355(6) Uani 1 1 d . . . H15 H 1.0434 0.0809 0.7305 0.043 Uiso 1 1 calc R . . C16 C 0.8869(3) -0.03071(18) 0.64970(18) 0.0495(8) Uani 1 1 d . . . H16A H 0.9436 -0.0112 0.626 0.074 Uiso 1 1 calc R . . H16B H 0.8066 -0.0333 0.6158 0.074 Uiso 1 1 calc R . . H16C H 0.9128 -0.0788 0.6677 0.074 Uiso 1 1 calc R . . C21 C 0.8925(2) 0.28637(14) 0.77440(13) 0.0294(5) Uani 1 1 d . . . C22 C 0.9759(3) 0.34309(15) 0.77612(15) 0.0376(6) Uani 1 1 d . . . H22 H 1.018 0.3449 0.7413 0.045 Uiso 1 1 calc R . . C23 C 0.9961(3) 0.39614(16) 0.82877(17) 0.0432(7) Uani 1 1 d . . . H23 H 1.0516 0.4336 0.829 0.052 Uiso 1 1 calc R . . C24 C 0.9352(3) 0.39474(16) 0.88139(16) 0.0417(7) Uani 1 1 d . . . H24 H 0.9495 0.4308 0.9169 0.05 Uiso 1 1 calc R . . C25 C 0.8529(3) 0.33909(16) 0.88053(15) 0.0425(7) Uani 1 1 d . . . H25 H 0.8115 0.3375 0.9157 0.051 Uiso 1 1 calc R . . C26 C 0.8316(3) 0.28565(15) 0.82743(14) 0.0357(6) Uani 1 1 d . . . H26 H 0.7754 0.2486 0.8273 0.043 Uiso 1 1 calc R . . C31 C 1.0242(2) 0.17710(14) 0.58683(13) 0.0298(5) Uani 1 1 d . . . C32 C 1.0214(3) 0.11702(17) 0.54360(15) 0.0420(7) Uani 1 1 d . . . H32 H 0.9462 0.0984 0.5163 0.05 Uiso 1 1 calc R . . C33 C 1.1294(3) 0.08361(18) 0.54014(16) 0.0466(7) Uani 1 1 d . . . H33 H 1.1252 0.0421 0.5116 0.056 Uiso 1 1 calc R . . C34 C 1.2431(3) 0.11095(16) 0.57841(15) 0.0394(6) Uani 1 1 d . . . C35 C 1.2449(3) 0.17142(17) 0.62203(16) 0.0418(7) Uani 1 1 d . . . H35 H 1.32 0.1907 0.6484 0.05 Uiso 1 1 calc R . . C36 C 1.1384(3) 0.20370(15) 0.62736(15) 0.0378(6) Uani 1 1 d . . . H36 H 1.1425 0.2434 0.6581 0.045 Uiso 1 1 calc R . . C37 C 1.3604(3) 0.0765(2) 0.5735(2) 0.0595(9) Uani 1 1 d . . . H37A H 1.4074 0.112 0.556 0.089 Uiso 1 1 calc R . . H37B H 1.3417 0.0358 0.5407 0.089 Uiso 1 1 calc R . . H37C H 1.407 0.0599 0.6206 0.089 Uiso 1 1 calc R . . C41 C 0.7215(2) 0.28960(14) 0.53635(13) 0.0292(5) Uani 1 1 d . . . C42 C 0.6073(2) 0.27552(16) 0.48863(15) 0.0358(6) Uani 1 1 d . . . H42 H 0.5986 0.2381 0.4549 0.043 Uiso 1 1 calc R . . C43 C 0.5061(3) 0.31622(18) 0.49042(16) 0.0424(7) Uani 1 1 d . . . H43 H 0.43 0.3051 0.4584 0.051 Uiso 1 1 calc R . . C44 C 0.5155(3) 0.37349(17) 0.53909(16) 0.0425(7) Uani 1 1 d . . . C45 C 0.6287(3) 0.38716(17) 0.58684(16) 0.0458(7) Uani 1 1 d . . . H45 H 0.6371 0.4247 0.6205 0.055 Uiso 1 1 calc R . . C46 C 0.7306(3) 0.34608(15) 0.58572(15) 0.0381(6) Uani 1 1 d . . . H46 H 0.8062 0.3566 0.6186 0.046 Uiso 1 1 calc R . . C47 C 0.4052(3) 0.4203(2) 0.5394(2) 0.0630(10) Uani 1 1 d . . . H47A H 0.4249 0.4501 0.5822 0.095 Uiso 1 1 calc R . . H47B H 0.3369 0.3892 0.5389 0.095 Uiso 1 1 calc R . . H47C H 0.3841 0.451 0.4973 0.095 Uiso 1 1 calc R . . C51 C 0.8606(2) 0.18282(14) 0.34583(13) 0.0304(5) Uani 1 1 d . . . C52 C 0.8968(3) 0.19852(15) 0.28465(14) 0.0402(7) Uani 1 1 d . . . H52 H 0.9343 0.243 0.2812 0.048 Uiso 1 1 calc R . . C53 C 0.8774(3) 0.14831(17) 0.22834(15) 0.0476(8) Uani 1 1 d . . . H53 H 0.9012 0.1596 0.1872 0.057 Uiso 1 1 calc R . . C54 C 0.8233(3) 0.08192(17) 0.23311(16) 0.0479(8) Uani 1 1 d . . . H54 H 0.8097 0.0486 0.1952 0.057 Uiso 1 1 calc R . . C55 C 0.7894(3) 0.06507(17) 0.29432(17) 0.0470(7) Uani 1 1 d . . . H55 H 0.7541 0.0199 0.298 0.056 Uiso 1 1 calc R . . C56 C 0.8075(3) 0.11492(15) 0.35032(15) 0.0380(6) Uani 1 1 d . . . H56 H 0.784 0.1031 0.3914 0.046 Uiso 1 1 calc R . . C61 C 0.9214(3) 0.44628(14) 0.36050(16) 0.0392(6) Uani 1 1 d . . . C62 C 0.8581(3) 0.39123(16) 0.31196(15) 0.0453(8) Uani 1 1 d . . . H62 H 0.8789 0.3744 0.2715 0.054 Uiso 1 1 calc R . . C63 C 0.7594(3) 0.36659(16) 0.33510(17) 0.0468(8) Uani 1 1 d . . . H63 H 0.704 0.3303 0.3129 0.056 Uiso 1 1 calc R . . C64 C 0.7577(3) 0.40585(16) 0.39779(16) 0.0411(7) Uani 1 1 d . . . H64 H 0.7014 0.4004 0.4241 0.049 Uiso 1 1 calc R . . C65 C 0.8579(3) 0.45503(14) 0.41314(15) 0.0361(6) Uani 1 1 d . . . H65 H 0.8787 0.4878 0.4517 0.043 Uiso 1 1 calc R . . C66 C 1.0288(4) 0.48931(18) 0.3531(2) 0.0612(10) Uani 1 1 d . . . H66A H 1.0006 0.5343 0.3282 0.092 Uiso 1 1 calc R . . H66B H 1.0721 0.4615 0.326 0.092 Uiso 1 1 calc R . . H66C H 1.0827 0.4998 0.4004 0.092 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 0.0220(2) 0.0344(2) 0.0285(2) -0.00269(16) 0.00974(15) -0.00226(16) Mn2 0.0249(2) 0.0267(2) 0.0293(2) 0.00092(15) 0.01052(15) 0.00316(15) O1 0.0284(12) 0.0930(18) 0.0696(15) -0.0200(13) 0.0200(10) 0.0072(12) O2 0.0538(13) 0.0591(14) 0.0357(11) -0.0122(10) -0.0002(10) -0.0046(11) O3 0.0339(12) 0.0961(19) 0.0661(15) -0.0057(14) 0.0266(11) 0.0096(12) O4 0.0611(14) 0.0401(11) 0.0373(11) -0.0058(9) -0.0007(10) -0.0050(10) C1 0.0305(15) 0.0525(17) 0.0370(15) -0.0061(12) 0.0112(12) -0.0074(13) C2 0.0284(14) 0.0368(15) 0.0445(16) -0.0034(12) 0.0127(12) -0.0004(11) C3 0.0360(16) 0.0417(15) 0.0354(14) 0.0023(12) 0.0147(12) 0.0038(12) C4 0.0349(15) 0.0259(14) 0.0419(16) -0.0006(11) 0.0128(12) 0.0008(11) C5 0.0268(13) 0.0322(13) 0.0306(13) -0.0003(10) 0.0119(11) -0.0010(10) C6 0.0274(13) 0.0355(14) 0.0304(13) 0.0001(10) 0.0111(10) -0.0018(11) C7 0.0277(13) 0.0330(13) 0.0279(13) -0.0042(10) 0.0118(10) -0.0051(11) C8 0.0284(13) 0.0302(13) 0.0261(12) -0.0019(10) 0.0125(10) -0.0034(10) C9 0.0260(13) 0.0291(13) 0.0297(13) 0.0003(10) 0.0103(10) 0.0005(10) C10 0.0262(13) 0.0307(13) 0.0282(13) -0.0003(10) 0.0091(10) 0.0016(10) C11 0.0341(15) 0.0307(14) 0.0405(15) -0.0034(11) 0.0066(12) 0.0009(11) C12 0.0419(17) 0.0379(16) 0.0446(16) 0.0053(12) 0.0139(13) -0.0075(13) C13 0.0492(18) 0.0455(17) 0.0345(15) 0.0055(12) 0.0168(13) 0.0004(14) C14 0.0381(16) 0.0401(15) 0.0311(14) 0.0009(11) 0.0042(11) 0.0032(12) C15 0.0258(13) 0.0388(14) 0.0390(15) -0.0010(11) 0.0048(11) 0.0037(11) C16 0.0432(18) 0.0452(17) 0.0581(19) -0.0134(14) 0.0115(15) 0.0033(14) C21 0.0308(14) 0.0301(13) 0.0292(13) 0.0009(10) 0.0115(11) 0.0014(11) C22 0.0335(15) 0.0410(15) 0.0420(15) -0.0027(12) 0.0167(12) 0.0001(12) C23 0.0353(16) 0.0391(16) 0.0551(18) -0.0089(13) 0.0129(13) -0.0071(13) C24 0.0423(17) 0.0381(15) 0.0436(16) -0.0109(12) 0.0106(13) 0.0032(13) C25 0.0519(18) 0.0414(16) 0.0392(15) -0.0042(12) 0.0213(13) 0.0046(14) C26 0.0394(16) 0.0368(15) 0.0353(14) -0.0035(11) 0.0179(12) -0.0047(12) C31 0.0303(14) 0.0340(13) 0.0281(13) 0.0008(10) 0.0132(10) 0.0011(11) C32 0.0351(15) 0.0499(17) 0.0404(15) -0.0105(13) 0.0099(12) 0.0041(13) C33 0.0510(19) 0.0492(18) 0.0402(16) -0.0120(13) 0.0141(14) 0.0074(14) C34 0.0350(15) 0.0519(18) 0.0334(14) 0.0068(12) 0.0129(12) 0.0107(13) C35 0.0290(15) 0.0494(18) 0.0434(16) 0.0000(13) 0.0045(12) 0.0017(12) C36 0.0348(16) 0.0377(15) 0.0397(15) -0.0044(12) 0.0087(12) 0.0000(12) C37 0.048(2) 0.069(2) 0.063(2) 0.0017(17) 0.0175(16) 0.0229(17) C41 0.0273(13) 0.0346(13) 0.0284(13) 0.0002(10) 0.0125(10) -0.0002(11) C42 0.0307(15) 0.0432(16) 0.0354(14) -0.0063(11) 0.0121(11) -0.0007(12) C43 0.0295(15) 0.0563(18) 0.0419(16) 0.0024(13) 0.0111(12) 0.0041(13) C44 0.0428(17) 0.0484(17) 0.0406(15) 0.0036(13) 0.0186(13) 0.0123(14) C45 0.0500(18) 0.0482(18) 0.0405(16) -0.0070(13) 0.0151(14) 0.0140(15) C46 0.0373(15) 0.0399(15) 0.0369(14) -0.0065(12) 0.0103(12) 0.0021(13) C47 0.056(2) 0.073(2) 0.065(2) 0.0049(18) 0.0239(17) 0.0294(19) C51 0.0318(14) 0.0299(13) 0.0296(13) -0.0027(10) 0.0086(10) 0.0049(11) C52 0.0583(19) 0.0347(15) 0.0319(14) -0.0005(11) 0.0200(13) 0.0054(13) C53 0.070(2) 0.0459(17) 0.0297(14) -0.0044(12) 0.0188(14) 0.0131(16) C54 0.0519(19) 0.0468(18) 0.0412(16) -0.0189(14) 0.0072(14) 0.0072(14) C55 0.0423(17) 0.0419(16) 0.0577(19) -0.0176(14) 0.0157(14) -0.0072(14) C56 0.0337(15) 0.0430(16) 0.0393(15) -0.0072(12) 0.0135(12) -0.0058(12) C61 0.0490(17) 0.0287(14) 0.0461(16) 0.0112(12) 0.0233(13) 0.0088(12) C62 0.064(2) 0.0408(17) 0.0300(14) 0.0059(12) 0.0116(14) 0.0184(15) C63 0.0399(17) 0.0373(16) 0.0509(18) 0.0033(13) -0.0068(14) 0.0083(13) C64 0.0324(15) 0.0415(15) 0.0512(17) 0.0089(13) 0.0146(13) 0.0126(13) C65 0.0418(16) 0.0285(13) 0.0406(15) 0.0022(11) 0.0157(12) 0.0092(12) C66 0.075(3) 0.0431(18) 0.085(3) 0.0166(17) 0.054(2) 0.0047(17) #-------------------------------------------------------------------------- # MOLECULAR GEOMETRY #-------------------------------------------------------------------------- _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 C1 1.764(3) . ? Mn1 C2 1.775(3) . ? Mn1 C5 2.093(3) . ? Mn1 C13 2.127(3) . ? Mn1 C12 2.131(3) . ? Mn1 C14 2.146(3) . ? Mn1 C6 2.162(3) . ? Mn1 C15 2.164(3) . ? Mn1 C11 2.173(3) . ? Mn2 C3 1.758(3) . ? Mn2 C4 1.773(3) . ? Mn2 C10 2.102(3) . ? Mn2 C65 2.143(3) . ? Mn2 C61 2.144(3) . ? Mn2 C62 2.147(3) . ? Mn2 C63 2.152(3) . ? Mn2 C64 2.160(3) . ? Mn2 C9 2.183(3) . ? O1 C1 1.162(4) . ? O2 C2 1.156(3) . ? O3 C3 1.158(3) . ? O4 C4 1.152(3) . ? C5 C6 1.244(4) . ? C5 C21 1.444(4) . ? C6 C7 1.437(3) . ? C7 C8 1.355(4) . ? C7 C31 1.490(4) . ? C8 C9 1.432(3) . ? C8 C41 1.496(4) . ? C9 C10 1.250(3) . ? C10 C51 1.450(3) . ? C11 C15 1.413(4) . ? C11 C12 1.423(4) . ? C11 C16 1.489(4) . ? C12 C13 1.413(4) . ? C13 C14 1.401(4) . ? C14 C15 1.413(4) . ? C21 C26 1.389(4) . ? C21 C22 1.399(4) . ? C22 C23 1.374(4) . ? C23 C24 1.382(4) . ? C24 C25 1.380(4) . ? C25 C26 1.385(4) . ? C31 C32 1.373(4) . ? C31 C36 1.397(4) . ? C32 C33 1.390(4) . ? C33 C34 1.385(4) . ? C34 C35 1.385(4) . ? C34 C37 1.502(4) . ? C35 C36 1.377(4) . ? C41 C42 1.384(4) . ? C41 C46 1.387(4) . ? C42 C43 1.379(4) . ? C43 C44 1.389(4) . ? C44 C45 1.374(4) . ? C44 C47 1.519(4) . ? C45 C46 1.387(4) . ? C51 C52 1.385(4) . ? C51 C56 1.394(4) . ? C52 C53 1.389(4) . ? C53 C54 1.376(5) . ? C54 C55 1.376(5) . ? C55 C56 1.382(4) . ? C61 C65 1.412(4) . ? C61 C62 1.421(4) . ? C61 C66 1.493(4) . ? C62 C63 1.396(5) . ? C63 C64 1.409(4) . ? C64 C65 1.415(4) . ? 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 C1 Mn1 C2 88.08(13) . . ? C1 Mn1 C5 87.94(12) . . ? C2 Mn1 C5 110.86(11) . . ? C1 Mn1 C13 92.00(13) . . ? C2 Mn1 C13 138.09(12) . . ? C5 Mn1 C13 111.03(11) . . ? C1 Mn1 C12 101.07(13) . . ? C2 Mn1 C12 100.27(12) . . ? C5 Mn1 C12 147.91(11) . . ? C13 Mn1 C12 38.76(11) . . ? C1 Mn1 C14 118.60(12) . . ? C2 Mn1 C14 150.55(12) . . ? C5 Mn1 C14 84.08(11) . . ? C13 Mn1 C14 38.27(11) . . ? C12 Mn1 C14 64.48(11) . . ? C1 Mn1 C6 104.73(12) . . ? C2 Mn1 C6 81.92(11) . . ? C5 Mn1 C6 33.97(10) . . ? C13 Mn1 C6 137.75(11) . . ? C12 Mn1 C6 154.18(11) . . ? C14 Mn1 C6 101.28(11) . . ? C1 Mn1 C15 155.38(12) . . ? C2 Mn1 C15 113.03(11) . . ? C5 Mn1 C15 95.60(10) . . ? C13 Mn1 C15 63.97(11) . . ? C12 Mn1 C15 64.06(11) . . ? C14 Mn1 C15 38.26(10) . . ? C6 Mn1 C15 91.23(11) . . ? C1 Mn1 C11 137.45(13) . . ? C2 Mn1 C11 87.91(11) . . ? C5 Mn1 C11 132.60(10) . . ? C13 Mn1 C11 64.53(11) . . ? C12 Mn1 C11 38.59(11) . . ? C14 Mn1 C11 64.27(10) . . ? C6 Mn1 C11 116.56(10) . . ? C15 Mn1 C11 38.03(10) . . ? C3 Mn2 C4 85.93(13) . . ? C3 Mn2 C10 87.90(12) . . ? C4 Mn2 C10 108.22(11) . . ? C3 Mn2 C65 126.16(12) . . ? C4 Mn2 C65 89.24(11) . . ? C10 Mn2 C65 143.40(11) . . ? C3 Mn2 C61 94.20(12) . . ? C4 Mn2 C61 109.54(12) . . ? C10 Mn2 C61 142.24(11) . . ? C65 Mn2 C61 38.46(10) . . ? C3 Mn2 C62 96.14(13) . . ? C4 Mn2 C62 148.20(12) . . ? C10 Mn2 C62 103.57(11) . . ? C65 Mn2 C62 63.95(11) . . ? C61 Mn2 C62 38.69(12) . . ? C3 Mn2 C63 128.69(13) . . ? C4 Mn2 C63 144.10(13) . . ? C10 Mn2 C63 85.08(11) . . ? C65 Mn2 C63 63.88(11) . . ? C61 Mn2 C63 64.39(12) . . ? C62 Mn2 C63 37.89(13) . . ? C3 Mn2 C64 158.00(12) . . ? C4 Mn2 C64 106.13(12) . . ? C10 Mn2 C64 105.03(11) . . ? C65 Mn2 C64 38.39(11) . . ? C61 Mn2 C64 64.63(11) . . ? C62 Mn2 C64 63.86(12) . . ? C63 Mn2 C64 38.15(12) . . ? C3 Mn2 C9 105.45(11) . . ? C4 Mn2 C9 80.68(11) . . ? C10 Mn2 C9 33.86(9) . . ? C65 Mn2 C9 126.54(10) . . ? C61 Mn2 C9 158.63(11) . . ? C62 Mn2 C9 128.42(11) . . ? C63 Mn2 C9 96.11(11) . . ? C64 Mn2 C9 94.80(11) . . ? O1 C1 Mn1 176.7(3) . . ? O2 C2 Mn1 178.3(3) . . ? O3 C3 Mn2 175.5(3) . . ? O4 C4 Mn2 178.4(2) . . ? C6 C5 C21 148.1(3) . . ? C6 C5 Mn1 76.04(17) . . ? C21 C5 Mn1 135.87(18) . . ? C5 C6 C7 160.4(3) . . ? C5 C6 Mn1 69.99(16) . . ? C7 C6 Mn1 129.54(18) . . ? C8 C7 C6 120.9(2) . . ? C8 C7 C31 122.4(2) . . ? C6 C7 C31 116.6(2) . . ? C7 C8 C9 120.5(2) . . ? C7 C8 C41 123.0(2) . . ? C9 C8 C41 116.3(2) . . ? C10 C9 C8 164.2(3) . . ? C10 C9 Mn2 69.53(16) . . ? C8 C9 Mn2 126.27(18) . . ? C9 C10 C51 148.7(3) . . ? C9 C10 Mn2 76.62(16) . . ? C51 C10 Mn2 134.45(18) . . ? C15 C11 C12 106.9(2) . . ? C15 C11 C16 125.5(3) . . ? C12 C11 C16 127.6(3) . . ? C15 C11 Mn1 70.66(15) . . ? C12 C11 Mn1 69.11(16) . . ? C16 C11 Mn1 127.1(2) . . ? C13 C12 C11 108.1(3) . . ? C13 C12 Mn1 70.47(16) . . ? C11 C12 Mn1 72.31(16) . . ? C14 C13 C12 108.4(3) . . ? C14 C13 Mn1 71.62(16) . . ? C12 C13 Mn1 70.77(16) . . ? C13 C14 C15 107.8(3) . . ? C13 C14 Mn1 70.12(16) . . ? C15 C14 Mn1 71.56(15) . . ? C14 C15 C11 108.8(3) . . ? C14 C15 Mn1 70.18(15) . . ? C11 C15 Mn1 71.31(15) . . ? C26 C21 C22 117.9(2) . . ? C26 C21 C5 122.0(2) . . ? C22 C21 C5 120.1(2) . . ? C23 C22 C21 120.6(3) . . ? C22 C23 C24 121.0(3) . . ? C25 C24 C23 119.1(3) . . ? C24 C25 C26 120.3(3) . . ? C25 C26 C21 121.2(3) . . ? C32 C31 C36 118.3(3) . . ? C32 C31 C7 121.9(2) . . ? C36 C31 C7 119.8(2) . . ? C31 C32 C33 120.9(3) . . ? C34 C33 C32 121.2(3) . . ? C35 C34 C33 117.4(3) . . ? C35 C34 C37 120.9(3) . . ? C33 C34 C37 121.7(3) . . ? C36 C35 C34 121.8(3) . . ? C35 C36 C31 120.4(3) . . ? C42 C41 C46 117.7(2) . . ? C42 C41 C8 121.2(2) . . ? C46 C41 C8 121.0(2) . . ? C43 C42 C41 120.9(3) . . ? C42 C43 C44 121.4(3) . . ? C45 C44 C43 117.7(3) . . ? C45 C44 C47 120.8(3) . . ? C43 C44 C47 121.6(3) . . ? C44 C45 C46 121.2(3) . . ? C45 C46 C41 121.0(3) . . ? C52 C51 C56 118.5(2) . . ? C52 C51 C10 121.9(2) . . ? C56 C51 C10 119.6(2) . . ? C51 C52 C53 120.5(3) . . ? C54 C53 C52 120.3(3) . . ? C53 C54 C55 119.7(3) . . ? C54 C55 C56 120.4(3) . . ? C55 C56 C51 120.6(3) . . ? C65 C61 C62 106.6(3) . . ? C65 C61 C66 127.5(3) . . ? C62 C61 C66 125.8(3) . . ? C65 C61 Mn2 70.73(15) . . ? C62 C61 Mn2 70.74(15) . . ? C66 C61 Mn2 126.6(2) . . ? C63 C62 C61 108.7(3) . . ? C63 C62 Mn2 71.28(17) . . ? C61 C62 Mn2 70.57(16) . . ? C62 C63 C64 108.6(3) . . ? C62 C63 Mn2 70.84(17) . . ? C64 C63 Mn2 71.21(16) . . ? C63 C64 C65 107.2(3) . . ? C63 C64 Mn2 70.64(16) . . ? C65 C64 Mn2 70.18(15) . . ? C61 C65 C64 108.9(3) . . ? C61 C65 Mn2 70.81(15) . . ? C64 C65 Mn2 71.44(15) . . ?