# Electronic Supplementary Material (ESI) for Dalton Transactions # This journal is © The Royal Society of Chemistry 2011 data_global _journal_name_full 'Dalton Trans.' _journal_coden_cambridge 0222 _journal_year ? _journal_volume ? _journal_page_first ? loop_ _publ_author_name _publ_author_address 'Muhammad Usman Anwar' ; Department of Chemistry Memorial University of Newfoundland St. Johns, NL, A1B 3X7, Canada ; 'Louise N. Dawe' ; Department of chemistry Memorial University of Newfoundland St. Johns, NL, A1B 3X7, Canada ; 'Laurence K. Thompson' ; Department of Chemistry Memorial University of Newfoundland St. Johns, NL, A1B 3X7, Canada ; _publ_contact_author_address ; Department of chemistry Memorial University of Newfoundland St. Johns, NL, A1B 3X7, Canada ; _publ_contact_author_email lk.thompson@mun.ca _publ_contact_author_fax 1-709-864-3702 _publ_contact_author_phone 1-709-864-8750 #TrackingRef 'MUA1097 CIF.cif' _publ_contact_author_name 'Prof. Laurence K. Thompson' _publ_section_title ; Approaching Polymetallic 'Assemblies of Assemblies' using ligands with multiple functionality -- novel Mn10M2 (M = Alkali metal) chains with 'ionophoric' end cavities. ; data_MUA1097 _database_code_depnum_ccdc_archive 'CCDC 814529' _publ_section_abstract ; Please see full paper. ; # start Validation Reply Form _vrf_PLAT602_MUA1097 ; PROBLEM: VERY LARGE Solvent Accessible VOID(S) in Structure ! RESPONSE: This situation was examined using Platon's SQUEEZE procedure. The following was reported: _platon_squeeze_void_nr _platon_squeeze_void_average_x _platon_squeeze_void_average_y _platon_squeeze_void_average_z _platon_squeeze_void_volume _platon_squeeze_void_count_electrons _platon_squeeze_void_content 1 0.500 0.000 0.000 748 165 ' ' 2 0.500 0.500 0.500 749 164 ' ' Residual electron density was not found in these regions by examination of difference maps, and given the acceptable refinement that was achieved without the use of SQUEEZE, the solvent accessible voids were left untreated in this reported structure. ; # end Validation Reply Form _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety '6(C11 H10 N3 O4) Cs2 Mn10 O2 4(C2 H O2) 4(C H3 O) 2(C2 H4 O) 2(H2 O)' _chemical_formula_sum 'C80 H96 Cs2 Mn10 N18 O42' _chemical_formula_weight 2796.92 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' Cs Cs -0.3680 2.1192 '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' 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' _symmetry_cell_setting monoclinic _symmetry_space_group_name_H-M 'P 1 21/c 1' _symmetry_space_group_name_Hall '-P 2ybc' _symmetry_Int_Tables_number 14 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 21.111(12) _cell_length_b 17.0489(10) _cell_length_c 17.7810(10) _cell_angle_alpha 90.00 _cell_angle_beta 92.586(7) _cell_angle_gamma 90.00 _cell_volume 6393(4) _cell_formula_units_Z 2 _cell_measurement_temperature 163(2) _cell_measurement_reflns_used 18683 _cell_measurement_theta_min 1.9 _cell_measurement_theta_max 29.6 _exptl_crystal_description Prism _exptl_crystal_colour 'Dark Red' _exptl_crystal_size_max 0.22 _exptl_crystal_size_mid 0.20 _exptl_crystal_size_min 0.07 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.453 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 2796 _exptl_absorpt_coefficient_mu 1.591 _exptl_absorpt_correction_type Numerical _exptl_absorpt_correction_T_max 0.941 _exptl_absorpt_correction_T_min 0.799 _exptl_absorpt_process_details '(T. Higashi, 2000)' _exptl_special_details ; ? ; _diffrn_ambient_temperature 163(2) _diffrn_radiation_wavelength 0.71075 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator 'graphite - Rigaku SHINE' _diffrn_measurement_device_type 'Rigaku Saturn' _diffrn_measurement_method \w _diffrn_detector_area_resol_mean 14.63 _diffrn_reflns_number 75464 _diffrn_reflns_av_R_equivalents 0.0610 _diffrn_reflns_av_sigmaI/netI 0.0384 _diffrn_reflns_limit_h_min -26 _diffrn_reflns_limit_h_max 26 _diffrn_reflns_limit_k_min -21 _diffrn_reflns_limit_k_max 21 _diffrn_reflns_limit_l_min -20 _diffrn_reflns_limit_l_max 22 _diffrn_reflns_theta_min 2.50 _diffrn_reflns_theta_max 26.50 _reflns_number_total 13253 _reflns_number_gt 11864 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'CrystalClear (Rigaku/MSC Inc., 2005)' _computing_cell_refinement 'CrystalClear (Rigaku/MSC Inc., 2005)' _computing_data_reduction 'CrystalClear (Rigaku/MSC Inc., 2005)' _computing_structure_solution 'SHELXS-97 (Acta Cryst.2008, A64, 112-122)' _computing_structure_refinement 'SHELXL-97 (Acta Cryst.2008, A64, 112-122)' _computing_molecular_graphics 'CrystalStructure3.7.0(Rigaku/MSC Inc.,2005)' _computing_publication_material 'CrystalStructure3.7.0(Rigaku/MSC Inc.,2005)' _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^)+(0.1603P)^2^+30.9791P] 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_extinction_coef ? _refine_ls_number_reflns 13253 _refine_ls_number_parameters 703 _refine_ls_number_restraints 12 _refine_ls_R_factor_all 0.1010 _refine_ls_R_factor_gt 0.0940 _refine_ls_wR_factor_ref 0.2867 _refine_ls_wR_factor_gt 0.2794 _refine_ls_goodness_of_fit_ref 1.103 _refine_ls_restrained_S_all 1.104 _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 Cs1 Cs 0.33614(3) 0.50033(3) 1.04814(3) 0.0564(2) Uani 1 1 d . . . Mn1 Mn 0.06110(5) 0.47839(6) 0.54348(6) 0.0380(3) Uani 1 1 d . . . Mn2 Mn 0.15099(5) 0.49058(6) 0.72430(6) 0.0344(2) Uani 1 1 d . . . Mn3 Mn 0.22678(5) 0.38493(6) 0.89273(6) 0.0358(3) Uani 1 1 d . . . Mn4 Mn 0.18184(5) 0.57083(6) 0.92402(6) 0.0380(3) Uani 1 1 d . . . Mn5 Mn 0.30167(5) 0.54878(6) 0.83565(6) 0.0387(3) Uani 1 1 d . . . O1 O 0.0835(2) 0.3852(3) 0.5977(3) 0.0433(11) Uani 1 1 d . . . O2 O 0.1814(2) 0.3907(3) 0.7924(3) 0.0407(11) Uani 1 1 d . . . O3 O 0.2682(2) 0.3563(3) 0.9871(3) 0.0424(11) Uani 1 1 d . . . O4 O 0.2991(3) 0.3575(3) 1.1322(3) 0.0495(12) Uani 1 1 d . . . O5 O 0.0305(2) 0.5496(3) 0.6339(3) 0.0437(11) Uani 1 1 d . . . O6 O 0.1308(2) 0.5557(3) 0.8274(3) 0.0364(10) Uani 1 1 d . . . O7 O 0.2236(3) 0.6094(3) 1.0165(3) 0.0484(12) Uani 1 1 d . . . O8 O 0.2954(4) 0.6350(6) 1.1382(5) 0.112(3) Uani 1 1 d U . . O9 O 0.1439(2) 0.5212(3) 0.5410(3) 0.0449(11) Uani 1 1 d . . . O10 O 0.2447(2) 0.5337(3) 0.7349(3) 0.0401(10) Uani 1 1 d . . . O11 O 0.3757(3) 0.5798(5) 0.9077(3) 0.0687(18) Uani 1 1 d . . . O12 O 0.4594(3) 0.5840(5) 1.0198(4) 0.083(2) Uani 1 1 d . . . O13 O 0.2438(2) 0.4929(3) 0.9004(3) 0.0408(11) Uani 1 1 d . . . O14 O 0.1359(3) 0.3809(3) 0.9419(4) 0.0539(14) Uani 1 1 d . . . O15 O 0.1198(3) 0.5009(3) 0.9844(4) 0.0578(16) Uani 1 1 d . . . O16 O 0.2488(2) 0.6391(3) 0.8588(3) 0.0422(11) Uani 1 1 d . . . O17 O 0.3574(4) 0.4680(5) 0.8058(5) 0.084(2) Uani 1 1 d . . . O18 O 0.3133(4) 0.3561(6) 0.8314(5) 0.090(2) Uani 1 1 d . . . O19 O -0.0272(2) 0.4443(3) 0.5280(3) 0.0417(11) Uani 1 1 d . . . O20 O 0.0785(3) 0.4009(3) 0.4361(3) 0.0505(13) Uani 1 1 d . . . O21 O 0.0916(9) 0.5258(14) 0.2220(12) 0.133(9) Uani 0.58(2) 1 d P A 1 O22 O 0.0113(9) 0.5983(13) 0.1885(12) 0.098(9) Uani 0.42(2) 1 d P A 2 N1 N 0.1156(3) 0.3860(3) 0.6646(3) 0.0375(12) Uani 1 1 d . . . N2 N 0.1809(3) 0.2560(3) 0.7981(3) 0.0400(12) Uani 1 1 d . . . N3 N 0.2099(3) 0.2723(3) 0.8697(3) 0.0389(12) Uani 1 1 d . . . N4 N 0.0631(2) 0.5542(3) 0.7008(3) 0.0365(12) Uani 1 1 d . . . N5 N 0.0729(3) 0.6599(4) 0.8684(3) 0.0443(13) Uani 1 1 d . . . N6 N 0.1169(3) 0.6545(3) 0.9298(3) 0.0398(12) Uani 1 1 d . . . N7 N 0.1790(3) 0.5266(3) 0.6072(3) 0.0386(12) Uani 1 1 d . . . N8 N 0.3209(3) 0.6090(5) 0.6800(4) 0.0595(19) Uani 1 1 d . . . N9 N 0.3484(3) 0.6098(5) 0.7545(4) 0.0593(19) Uani 1 1 d . . . C1 C 0.1204(4) 0.2434(4) 0.6484(4) 0.0428(15) Uani 1 1 d . . . H1A H 0.0759 0.2415 0.6306 0.051 Uiso 1 1 calc R . . H1B H 0.1297 0.1989 0.6820 0.051 Uiso 1 1 calc R . . H1C H 0.1476 0.2408 0.6053 0.051 Uiso 1 1 calc R . . C2 C 0.1328(3) 0.3183(4) 0.6903(4) 0.0347(13) Uani 1 1 d . . . C3 C 0.1668(3) 0.3211(4) 0.7634(4) 0.0381(14) Uani 1 1 d . . . C4 C 0.2202(4) 0.2126(4) 0.9136(4) 0.0437(16) Uani 1 1 d . . . H4 H 0.2099 0.1620 0.8941 0.052 Uiso 1 1 calc R . . C5 C 0.2461(3) 0.2173(4) 0.9896(4) 0.0423(15) Uani 1 1 d . . . C6 C 0.2468(4) 0.1473(4) 1.0319(4) 0.0477(17) Uani 1 1 d . . . H6 H 0.2328 0.0997 1.0090 0.057 Uiso 1 1 calc R . . C7 C 0.2676(4) 0.1478(5) 1.1057(5) 0.0518(19) Uani 1 1 d . . . H7 H 0.2704 0.1001 1.1332 0.062 Uiso 1 1 calc R . . C8 C 0.2844(3) 0.2176(5) 1.1403(4) 0.0452(16) Uani 1 1 d . . . H8 H 0.2965 0.2180 1.1924 0.054 Uiso 1 1 calc R . . C9 C 0.2839(3) 0.2862(4) 1.1008(4) 0.0405(15) Uani 1 1 d . . . C10 C 0.2657(3) 0.2894(4) 1.0226(4) 0.0374(14) Uani 1 1 d . . . C11 C 0.3117(5) 0.3583(6) 1.2123(5) 0.063(2) Uani 1 1 d . . . H11A H 0.3475 0.3235 1.2253 0.076 Uiso 1 1 calc R . . H11B H 0.2741 0.3402 1.2376 0.076 Uiso 1 1 calc R . . H11C H 0.3221 0.4118 1.2288 0.076 Uiso 1 1 calc R . . C12 C -0.0102(4) 0.6593(6) 0.7340(5) 0.063(2) Uani 1 1 d . . . H12A H -0.0030 0.6911 0.6893 0.076 Uiso 1 1 calc R . . H12B H -0.0143 0.6938 0.7776 0.076 Uiso 1 1 calc R . . H12C H -0.0492 0.6288 0.7258 0.076 Uiso 1 1 calc R . . C13 C 0.0446(3) 0.6048(4) 0.7482(4) 0.0403(15) Uani 1 1 d . . . C14 C 0.0839(3) 0.6067(4) 0.8194(4) 0.0392(14) Uani 1 1 d . . . C15 C 0.1087(4) 0.7027(4) 0.9848(4) 0.0484(17) Uani 1 1 d . . . H15 H 0.0732 0.7369 0.9803 0.058 Uiso 1 1 calc R . . C16 C 0.1485(4) 0.7088(4) 1.0514(4) 0.0464(16) Uani 1 1 d . . . C17 C 0.1318(4) 0.7652(5) 1.1056(5) 0.058(2) Uani 1 1 d . . . H17 H 0.0948 0.7962 1.0968 0.070 Uiso 1 1 calc R . . C18 C 0.1685(5) 0.7755(6) 1.1710(6) 0.068(2) Uani 1 1 d . . . H18 H 0.1559 0.8117 1.2082 0.082 Uiso 1 1 calc R . . C19 C 0.2236(5) 0.7328(6) 1.1819(5) 0.068(3) Uani 1 1 d . . . H19 H 0.2497 0.7410 1.2262 0.082 Uiso 1 1 calc R . . C20 C 0.2416(5) 0.6784(7) 1.1292(6) 0.075(3) Uani 1 1 d U . . C21 C 0.2040(4) 0.6641(4) 1.0628(4) 0.0471(17) Uani 1 1 d . . . C22 C 0.3371(9) 0.6496(12) 1.2047(10) 0.157(7) Uani 1 1 d U . . H22A H 0.3137 0.6403 1.2502 0.188 Uiso 1 1 calc R . . H22B H 0.3518 0.7041 1.2042 0.188 Uiso 1 1 calc R . . H22C H 0.3736 0.6142 1.2042 0.188 Uiso 1 1 calc R . . C23 C 0.2547(4) 0.6020(7) 0.5334(5) 0.068(3) Uani 1 1 d . . . H23A H 0.2918 0.5738 0.5161 0.081 Uiso 1 1 calc R . . H23B H 0.2662 0.6567 0.5440 0.081 Uiso 1 1 calc R . . H23C H 0.2206 0.6003 0.4942 0.081 Uiso 1 1 calc R . . C24 C 0.2325(3) 0.5641(5) 0.6038(4) 0.0444(16) Uani 1 1 d . . . C25 C 0.2679(3) 0.5685(5) 0.6776(4) 0.0423(15) Uani 1 1 d . . . C26 C 0.4017(4) 0.6473(8) 0.7611(5) 0.074(3) Uani 1 1 d . . . H26 H 0.4151 0.6740 0.7177 0.089 Uiso 1 1 calc R . . C27 C 0.4425(4) 0.6524(8) 0.8275(6) 0.078(3) Uani 1 1 d . . . C28 C 0.5004(5) 0.6920(10) 0.8204(6) 0.104(5) Uani 1 1 d . . . H28 H 0.5104 0.7140 0.7733 0.125 Uiso 1 1 calc R . . C29 C 0.5429(5) 0.6991(9) 0.8816(7) 0.093(4) Uani 1 1 d . . . H29 H 0.5806 0.7288 0.8771 0.112 Uiso 1 1 calc R . . C30 C 0.5310(4) 0.6632(8) 0.9491(7) 0.081(3) Uani 1 1 d . . . H30 H 0.5611 0.6669 0.9903 0.098 Uiso 1 1 calc R . . C31 C 0.4756(4) 0.6223(7) 0.9570(5) 0.067(3) Uani 1 1 d . . . C32 C 0.4285(4) 0.6185(6) 0.8960(6) 0.064(2) Uani 1 1 d . . . C33 C 0.5061(6) 0.5898(9) 1.0817(7) 0.101(4) Uani 1 1 d . . . H33A H 0.5123 0.6450 1.0955 0.121 Uiso 1 1 calc R . . H33B H 0.5464 0.5675 1.0665 0.121 Uiso 1 1 calc R . . H33C H 0.4913 0.5607 1.1251 0.121 Uiso 1 1 calc R . . C34 C 0.1069(4) 0.4295(4) 0.9796(5) 0.0473(17) Uani 1 1 d . . . C35 C 0.0491(5) 0.4018(6) 1.0221(7) 0.074(3) Uani 1 1 d . . . H35A H 0.0400 0.3468 1.0096 0.089 Uiso 1 1 calc R . . H35B H 0.0122 0.4342 1.0073 0.089 Uiso 1 1 calc R . . H35C H 0.0582 0.4067 1.0764 0.089 Uiso 1 1 calc R . . C36 C 0.2728(4) 0.7108(5) 0.8813(6) 0.061(2) Uani 1 1 d . . . H36A H 0.2833 0.7097 0.9355 0.073 Uiso 1 1 calc R . . H36B H 0.2410 0.7516 0.8703 0.073 Uiso 1 1 calc R . . H36C H 0.3111 0.7222 0.8541 0.073 Uiso 1 1 calc R . . C37 C 0.3560(4) 0.3898(6) 0.8058(5) 0.057(2) Uani 1 1 d . . . C38 C 0.4076(5) 0.3580(9) 0.7650(6) 0.083(3) Uani 1 1 d . . . H38A H 0.4082 0.3007 0.7703 0.100 Uiso 1 1 calc R . . H38B H 0.4478 0.3797 0.7853 0.100 Uiso 1 1 calc R . . H38C H 0.4018 0.3718 0.7116 0.100 Uiso 1 1 calc R . . C39 C -0.0617(4) 0.4052(5) 0.5833(5) 0.056(2) Uani 1 1 d . . . H39A H -0.0646 0.4389 0.6276 0.068 Uiso 1 1 calc R . . H39B H -0.0399 0.3563 0.5977 0.068 Uiso 1 1 calc R . . H39C H -0.1044 0.3931 0.5627 0.068 Uiso 1 1 calc R . . C40 C 0.0720(4) 0.3147(6) 0.4480(5) 0.061(2) Uani 1 1 d . . . H40A H 0.1006 0.2981 0.4899 0.073 Uiso 1 1 calc R . . H40B H 0.0829 0.2868 0.4021 0.073 Uiso 1 1 calc R . . H40C H 0.0281 0.3025 0.4596 0.073 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 Cs1 0.0678(4) 0.0436(3) 0.0560(4) 0.0034(2) -0.0170(3) -0.0047(2) Mn1 0.0341(5) 0.0358(5) 0.0428(6) -0.0002(4) -0.0110(4) 0.0019(4) Mn2 0.0341(5) 0.0289(5) 0.0394(6) -0.0001(4) -0.0066(4) 0.0004(4) Mn3 0.0406(5) 0.0288(5) 0.0374(5) 0.0017(4) -0.0060(4) 0.0007(4) Mn4 0.0439(6) 0.0318(5) 0.0380(5) -0.0020(4) -0.0018(4) -0.0025(4) Mn5 0.0323(5) 0.0429(6) 0.0404(6) 0.0016(4) -0.0056(4) 0.0006(4) O1 0.046(3) 0.039(3) 0.044(3) -0.002(2) -0.017(2) 0.001(2) O2 0.052(3) 0.026(2) 0.044(3) 0.0034(18) -0.010(2) -0.0018(19) O3 0.053(3) 0.034(2) 0.040(3) 0.0041(19) -0.008(2) -0.002(2) O4 0.060(3) 0.047(3) 0.040(3) 0.001(2) -0.009(2) -0.003(2) O5 0.036(2) 0.052(3) 0.042(3) -0.003(2) -0.013(2) 0.007(2) O6 0.036(2) 0.035(2) 0.037(2) -0.0012(18) -0.0051(18) 0.0009(18) O7 0.054(3) 0.047(3) 0.044(3) -0.010(2) -0.001(2) 0.007(2) O8 0.098(6) 0.141(7) 0.092(5) -0.071(5) -0.048(4) 0.060(5) O9 0.037(2) 0.057(3) 0.040(3) 0.002(2) -0.009(2) -0.003(2) O10 0.030(2) 0.046(3) 0.043(3) -0.003(2) -0.0064(19) -0.0041(19) O11 0.042(3) 0.110(6) 0.053(3) 0.011(3) -0.010(3) -0.007(3) O12 0.063(4) 0.118(6) 0.065(4) 0.008(4) -0.024(3) 0.001(4) O13 0.045(3) 0.034(2) 0.042(3) 0.0038(19) -0.008(2) -0.0035(19) O14 0.045(3) 0.038(3) 0.078(4) -0.005(3) 0.006(3) 0.000(2) O15 0.078(4) 0.034(3) 0.064(4) 0.003(2) 0.028(3) 0.001(2) O16 0.038(2) 0.036(2) 0.053(3) -0.003(2) -0.001(2) -0.0025(19) O17 0.067(4) 0.062(4) 0.123(7) 0.002(4) -0.001(4) 0.001(3) O18 0.077(5) 0.105(6) 0.090(5) -0.005(5) 0.028(4) -0.010(5) O19 0.037(2) 0.042(3) 0.045(3) 0.003(2) -0.009(2) 0.001(2) O20 0.046(3) 0.056(3) 0.048(3) -0.007(2) -0.009(2) 0.007(2) O21 0.112(14) 0.163(18) 0.130(16) 0.021(13) 0.075(12) 0.035(13) O22 0.076(12) 0.112(17) 0.105(16) 0.062(13) -0.016(10) -0.024(11) N1 0.039(3) 0.033(3) 0.040(3) -0.001(2) -0.009(2) -0.002(2) N2 0.049(3) 0.034(3) 0.036(3) -0.005(2) -0.005(2) 0.002(2) N3 0.045(3) 0.032(3) 0.039(3) 0.002(2) -0.008(2) 0.005(2) N4 0.028(2) 0.040(3) 0.041(3) -0.002(2) -0.007(2) -0.002(2) N5 0.047(3) 0.042(3) 0.044(3) 0.000(3) -0.006(3) 0.004(3) N6 0.045(3) 0.035(3) 0.040(3) -0.001(2) 0.001(2) -0.002(2) N7 0.031(3) 0.040(3) 0.045(3) -0.001(2) -0.009(2) 0.002(2) N8 0.038(3) 0.096(6) 0.043(3) 0.006(4) -0.006(3) -0.022(3) N9 0.035(3) 0.100(6) 0.043(4) -0.005(4) -0.003(3) -0.014(3) C1 0.048(4) 0.038(4) 0.041(4) -0.003(3) -0.006(3) -0.002(3) C2 0.037(3) 0.026(3) 0.041(3) -0.003(2) 0.000(3) 0.000(2) C3 0.045(4) 0.028(3) 0.041(3) 0.001(3) -0.001(3) 0.000(3) C4 0.060(4) 0.030(3) 0.041(4) 0.000(3) -0.001(3) -0.003(3) C5 0.047(4) 0.035(3) 0.045(4) 0.001(3) -0.005(3) 0.002(3) C6 0.053(4) 0.037(4) 0.052(4) 0.008(3) -0.009(3) 0.001(3) C7 0.055(4) 0.047(4) 0.052(4) 0.015(3) -0.012(4) 0.000(3) C8 0.042(4) 0.050(4) 0.042(4) 0.010(3) -0.008(3) 0.001(3) C9 0.033(3) 0.043(4) 0.045(4) 0.004(3) -0.004(3) -0.003(3) C10 0.035(3) 0.034(3) 0.043(4) 0.004(3) -0.005(3) 0.003(3) C11 0.086(7) 0.058(5) 0.044(4) -0.003(4) -0.006(4) -0.003(5) C12 0.060(5) 0.070(6) 0.059(5) -0.010(4) -0.009(4) 0.026(4) C13 0.036(3) 0.042(4) 0.042(4) 0.000(3) -0.004(3) 0.004(3) C14 0.035(3) 0.041(4) 0.042(4) -0.003(3) 0.001(3) -0.003(3) C15 0.052(4) 0.038(4) 0.055(4) -0.010(3) 0.001(3) 0.000(3) C16 0.054(4) 0.038(4) 0.047(4) -0.007(3) 0.004(3) 0.001(3) C17 0.059(5) 0.052(5) 0.063(5) -0.021(4) -0.001(4) 0.004(4) C18 0.071(6) 0.057(5) 0.075(6) -0.025(5) 0.000(5) 0.004(4) C19 0.072(6) 0.074(6) 0.057(5) -0.030(5) -0.013(4) 0.012(5) C20 0.072(6) 0.085(7) 0.066(5) -0.036(5) -0.020(5) 0.022(5) C21 0.059(4) 0.038(4) 0.043(4) -0.006(3) 0.002(3) -0.004(3) C22 0.141(12) 0.179(14) 0.144(12) -0.092(11) -0.063(10) 0.063(11) C23 0.049(5) 0.107(8) 0.046(4) 0.008(5) -0.003(4) -0.025(5) C24 0.037(3) 0.054(4) 0.042(4) 0.000(3) -0.004(3) -0.003(3) C25 0.037(3) 0.051(4) 0.038(4) -0.006(3) -0.004(3) -0.004(3) C26 0.040(4) 0.137(10) 0.047(5) 0.002(5) 0.001(4) -0.037(5) C27 0.043(4) 0.134(10) 0.058(5) -0.008(6) 0.001(4) -0.032(6) C28 0.060(6) 0.190(16) 0.062(6) -0.010(8) -0.003(5) -0.052(8) C29 0.047(5) 0.149(12) 0.083(8) -0.017(8) -0.002(5) -0.039(7) C30 0.041(5) 0.119(10) 0.083(7) -0.015(7) -0.017(5) -0.007(5) C31 0.050(5) 0.099(8) 0.050(5) -0.007(5) -0.008(4) 0.001(5) C32 0.035(4) 0.089(7) 0.068(6) -0.005(5) -0.007(4) -0.007(4) C33 0.100(9) 0.127(11) 0.072(7) -0.004(7) -0.047(7) 0.004(8) C34 0.049(4) 0.037(4) 0.056(4) 0.010(3) 0.004(3) 0.002(3) C35 0.070(6) 0.046(5) 0.110(8) 0.016(5) 0.036(6) 0.005(4) C36 0.062(5) 0.033(4) 0.088(6) -0.008(4) 0.011(5) -0.008(3) C37 0.051(4) 0.079(6) 0.041(4) -0.010(4) -0.010(3) -0.013(4) C38 0.045(5) 0.130(11) 0.074(7) -0.009(7) -0.002(5) -0.008(6) C39 0.043(4) 0.056(5) 0.068(5) 0.017(4) -0.010(4) -0.008(3) C40 0.061(5) 0.066(5) 0.054(5) -0.012(4) -0.013(4) 0.013(4) _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 Cs1 O8 2.949(7) . ? Cs1 O4 2.981(6) . ? Cs1 O11 2.992(6) . ? Cs1 O3 3.021(5) . ? Cs1 O12 3.030(8) . ? Cs1 O7 3.048(5) . ? Cs1 O13 3.203(5) . ? Mn1 O9 1.896(5) . ? Mn1 O1 1.907(5) . ? Mn1 O19 1.945(5) 3_566 ? Mn1 O19 1.961(5) . ? Mn1 O5 2.138(5) . ? Mn1 O20 2.364(5) . ? Mn1 Mn1 3.038(2) 3_566 ? Mn2 O10 2.112(5) . ? Mn2 O2 2.169(5) . ? Mn2 N4 2.174(5) . ? Mn2 N1 2.190(5) . ? Mn2 O6 2.201(5) . ? Mn2 N7 2.274(6) . ? Mn3 O13 1.879(5) . ? Mn3 O3 1.920(5) . ? Mn3 O2 1.990(5) . ? Mn3 N3 1.992(6) . ? Mn3 O14 2.146(6) . ? Mn3 O18 2.225(8) . ? Mn4 O13 1.924(5) . ? Mn4 O7 1.945(5) . ? Mn4 N6 1.985(6) . ? Mn4 O6 2.002(5) . ? Mn4 O15 2.102(6) . ? Mn4 O16 2.202(5) . ? Mn4 Mn5 3.061(2) . ? Mn5 O17 1.902(8) . ? Mn5 O16 1.956(5) . ? Mn5 O13 1.963(5) . ? Mn5 O11 2.045(6) . ? Mn5 N9 2.064(7) . ? Mn5 O10 2.127(5) . ? O1 N1 1.342(7) . ? O2 C3 1.324(8) . ? O3 C10 1.306(8) . ? O4 C9 1.369(9) . ? O4 C11 1.437(9) . ? O5 N4 1.348(7) . ? O6 C14 1.321(8) . ? O7 C21 1.324(9) . ? O8 C20 1.359(12) . ? O8 C22 1.462(15) . ? O9 N7 1.367(7) . ? O10 C25 1.294(9) . ? O11 C32 1.321(11) . ? O12 C31 1.351(13) . ? O12 C33 1.448(11) . ? O14 C34 1.243(10) . ? O15 C34 1.250(9) . ? O16 C36 1.375(9) . ? O17 C37 1.334(12) . ? O18 C37 1.177(12) . ? O19 C39 1.415(10) . ? O19 Mn1 1.945(5) 3_566 ? O20 C40 1.492(11) . ? N1 C2 1.287(8) . ? N2 C3 1.299(9) . ? N2 N3 1.414(8) . ? N3 C4 1.296(9) . ? N4 C13 1.280(9) . ? N5 C14 1.286(9) . ? N5 N6 1.405(8) . ? N6 C15 1.294(9) . ? N7 C24 1.300(9) . ? N8 C25 1.314(10) . ? N8 N9 1.423(9) . ? N9 C26 1.296(11) . ? C1 C2 1.495(9) . ? C1 H1A 0.9800 . ? C1 H1B 0.9800 . ? C1 H1C 0.9800 . ? C2 C3 1.457(9) . ? C4 C5 1.436(10) . ? C4 H4 0.9500 . ? C5 C6 1.411(10) . ? C5 C10 1.415(10) . ? C6 C7 1.364(11) . ? C6 H6 0.9500 . ? C7 C8 1.379(12) . ? C7 H7 0.9500 . ? C8 C9 1.364(10) . ? C8 H8 0.9500 . ? C9 C10 1.427(10) . ? C11 H11A 0.9800 . ? C11 H11B 0.9800 . ? C11 H11C 0.9800 . ? C12 C13 1.497(10) . ? C12 H12A 0.9800 . ? C12 H12B 0.9800 . ? C12 H12C 0.9800 . ? C13 C14 1.482(10) . ? C15 C16 1.426(11) . ? C15 H15 0.9500 . ? C16 C21 1.404(11) . ? C16 C17 1.417(11) . ? C17 C18 1.379(13) . ? C17 H17 0.9500 . ? C18 C19 1.379(14) . ? C18 H18 0.9500 . ? C19 C20 1.384(12) . ? C19 H19 0.9500 . ? C20 C21 1.414(12) . ? C22 H22A 0.9800 . ? C22 H22B 0.9800 . ? C22 H22C 0.9800 . ? C23 C24 1.504(11) . ? C23 H23A 0.9800 . ? C23 H23B 0.9800 . ? C23 H23C 0.9800 . ? C24 C25 1.482(10) . ? C26 C27 1.431(12) . ? C26 H26 0.9500 . ? C27 C32 1.391(14) . ? C27 C28 1.407(14) . ? C28 C29 1.384(15) . ? C28 H28 0.9500 . ? C29 C30 1.381(17) . ? C29 H29 0.9500 . ? C30 C31 1.374(15) . ? C30 H30 0.9500 . ? C31 C32 1.439(12) . ? C33 H33A 0.9800 . ? C33 H33B 0.9800 . ? C33 H33C 0.9800 . ? C34 C35 1.537(12) . ? C35 H35A 0.9800 . ? C35 H35B 0.9800 . ? C35 H35C 0.9800 . ? C36 H36A 0.9800 . ? C36 H36B 0.9800 . ? C36 H36C 0.9800 . ? C37 C38 1.442(14) . ? C38 H38A 0.9800 . ? C38 H38B 0.9800 . ? C38 H38C 0.9800 . ? C39 H39A 0.9800 . ? C39 H39B 0.9800 . ? C39 H39C 0.9800 . ? C40 H40A 0.9800 . ? C40 H40B 0.9800 . ? C40 H40C 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 O8 Cs1 O4 105.9(3) . . ? O8 Cs1 O11 101.5(3) . . ? O4 Cs1 O11 151.40(19) . . ? O8 Cs1 O3 133.0(2) . . ? O4 Cs1 O3 52.04(13) . . ? O11 Cs1 O3 102.37(17) . . ? O8 Cs1 O12 89.8(3) . . ? O4 Cs1 O12 135.66(18) . . ? O11 Cs1 O12 51.24(17) . . ? O3 Cs1 O12 136.10(19) . . ? O8 Cs1 O7 51.83(17) . . ? O4 Cs1 O7 111.76(16) . . ? O11 Cs1 O7 79.29(17) . . ? O3 Cs1 O7 94.34(14) . . ? O12 Cs1 O7 110.49(19) . . ? O8 Cs1 O13 107.14(17) . . ? O4 Cs1 O13 102.43(13) . . ? O11 Cs1 O13 61.04(15) . . ? O3 Cs1 O13 53.95(12) . . ? O12 Cs1 O13 112.19(16) . . ? O7 Cs1 O13 55.40(13) . . ? O8 Cs1 C22 20.9(3) . . ? O4 Cs1 C22 100.0(4) . . ? O11 Cs1 C22 108.5(4) . . ? O3 Cs1 C22 143.2(4) . . ? O12 Cs1 C22 80.2(4) . . ? O7 Cs1 C22 72.7(3) . . ? O13 Cs1 C22 127.9(3) . . ? O8 Cs1 C11 91.5(3) . . ? O4 Cs1 C11 19.52(17) . . ? O11 Cs1 C11 166.1(2) . . ? O3 Cs1 C11 71.53(16) . . ? O12 Cs1 C11 124.6(2) . . ? O7 Cs1 C11 113.2(2) . . ? O13 Cs1 C11 120.02(17) . . ? C22 Cs1 C11 82.0(4) . . ? O8 Cs1 Mn5 108.35(19) . . ? O4 Cs1 Mn5 128.08(10) . . ? O11 Cs1 Mn5 31.07(12) . . ? O3 Cs1 Mn5 76.09(9) . . ? O12 Cs1 Mn5 82.14(13) . . ? O7 Cs1 Mn5 65.32(10) . . ? O13 Cs1 Mn5 30.05(9) . . ? C22 Cs1 Mn5 124.5(3) . . ? C11 Cs1 Mn5 147.41(14) . . ? O8 Cs1 C10 131.3(3) . . ? O4 Cs1 C10 36.85(14) . . ? O11 Cs1 C10 116.01(18) . . ? O3 Cs1 C10 15.99(13) . . ? O12 Cs1 C10 137.6(2) . . ? O7 Cs1 C10 104.49(14) . . ? O13 Cs1 C10 69.76(13) . . ? C22 Cs1 C10 134.1(4) . . ? C11 Cs1 C10 56.34(17) . . ? Mn5 Cs1 C10 91.66(10) . . ? O8 Cs1 C33 84.3(3) . . ? O4 Cs1 C33 120.1(2) . . ? O11 Cs1 C33 70.3(2) . . ? O3 Cs1 C33 142.0(3) . . ? O12 Cs1 C33 19.1(2) . . ? O7 Cs1 C33 119.4(3) . . ? O13 Cs1 C33 131.3(2) . . ? C22 Cs1 C33 69.6(4) . . ? C11 Cs1 C33 106.4(2) . . ? Mn5 Cs1 C33 101.21(19) . . ? C10 Cs1 C33 135.8(2) . . ? O9 Mn1 O1 97.2(2) . . ? O9 Mn1 O19 92.1(2) . 3_566 ? O1 Mn1 O19 166.0(2) . 3_566 ? O9 Mn1 O19 169.3(2) . . ? O1 Mn1 O19 92.1(2) . . ? O19 Mn1 O19 77.9(2) 3_566 . ? O9 Mn1 O5 96.3(2) . . ? O1 Mn1 O5 99.7(2) . . ? O19 Mn1 O5 89.6(2) 3_566 . ? O19 Mn1 O5 87.5(2) . . ? O9 Mn1 O20 91.1(2) . . ? O1 Mn1 O20 84.2(2) . . ? O19 Mn1 O20 85.2(2) 3_566 . ? O19 Mn1 O20 84.4(2) . . ? O5 Mn1 O20 171.16(18) . . ? O9 Mn1 Mn1 131.09(17) . 3_566 ? O1 Mn1 Mn1 130.14(16) . 3_566 ? O19 Mn1 Mn1 39.13(14) 3_566 3_566 ? O19 Mn1 Mn1 38.74(14) . 3_566 ? O5 Mn1 Mn1 88.11(13) . 3_566 ? O20 Mn1 Mn1 83.34(13) . 3_566 ? O10 Mn2 O2 88.32(19) . . ? O10 Mn2 N4 129.2(2) . . ? O2 Mn2 N4 136.7(2) . . ? O10 Mn2 N1 128.7(2) . . ? O2 Mn2 N1 73.56(19) . . ? N4 Mn2 N1 92.5(2) . . ? O10 Mn2 O6 88.02(18) . . ? O2 Mn2 O6 89.68(18) . . ? N4 Mn2 O6 73.33(19) . . ? N1 Mn2 O6 137.7(2) . . ? O10 Mn2 N7 72.92(19) . . ? O2 Mn2 N7 129.8(2) . . ? N4 Mn2 N7 86.8(2) . . ? N1 Mn2 N7 82.7(2) . . ? O6 Mn2 N7 134.0(2) . . ? O13 Mn3 O3 96.2(2) . . ? O13 Mn3 O2 95.7(2) . . ? O3 Mn3 O2 168.1(2) . . ? O13 Mn3 N3 172.3(2) . . ? O3 Mn3 N3 90.3(2) . . ? O2 Mn3 N3 77.8(2) . . ? O13 Mn3 O14 100.0(2) . . ? O3 Mn3 O14 90.9(2) . . ? O2 Mn3 O14 87.9(2) . . ? N3 Mn3 O14 84.1(2) . . ? O13 Mn3 O18 95.4(3) . . ? O3 Mn3 O18 91.2(3) . . ? O2 Mn3 O18 86.8(3) . . ? N3 Mn3 O18 80.2(3) . . ? O14 Mn3 O18 164.2(3) . . ? O13 Mn3 Cs1 51.02(15) . . ? O3 Mn3 Cs1 45.67(14) . . ? O2 Mn3 Cs1 145.92(13) . . ? N3 Mn3 Cs1 134.65(16) . . ? O14 Mn3 Cs1 103.36(17) . . ? O18 Mn3 Cs1 89.2(2) . . ? O13 Mn4 O7 97.5(2) . . ? O13 Mn4 N6 170.3(2) . . ? O7 Mn4 N6 90.1(2) . . ? O13 Mn4 O6 93.9(2) . . ? O7 Mn4 O6 167.1(2) . . ? N6 Mn4 O6 77.9(2) . . ? O13 Mn4 O15 99.5(2) . . ? O7 Mn4 O15 91.7(3) . . ? N6 Mn4 O15 86.2(2) . . ? O6 Mn4 O15 92.4(2) . . ? O13 Mn4 O16 77.9(2) . . ? O7 Mn4 O16 89.4(2) . . ? N6 Mn4 O16 96.2(2) . . ? O6 Mn4 O16 87.10(19) . . ? O15 Mn4 O16 177.3(2) . . ? O13 Mn4 Mn5 38.50(15) . . ? O7 Mn4 Mn5 96.97(17) . . ? N6 Mn4 Mn5 134.73(18) . . ? O6 Mn4 Mn5 88.20(14) . . ? O15 Mn4 Mn5 137.80(16) . . ? O16 Mn4 Mn5 39.58(13) . . ? O13 Mn4 Cs1 51.23(15) . . ? O7 Mn4 Cs1 46.67(16) . . ? N6 Mn4 Cs1 136.75(17) . . ? O6 Mn4 Cs1 145.13(14) . . ? O15 Mn4 Cs1 93.3(2) . . ? O16 Mn4 Cs1 85.64(14) . . ? Mn5 Mn4 Cs1 65.08(4) . . ? O17 Mn5 O16 173.9(3) . . ? O17 Mn5 O13 102.8(3) . . ? O16 Mn5 O13 83.3(2) . . ? O17 Mn5 O11 84.1(3) . . ? O16 Mn5 O11 95.3(3) . . ? O13 Mn5 O11 103.7(2) . . ? O17 Mn5 N9 81.3(4) . . ? O16 Mn5 N9 92.6(3) . . ? O13 Mn5 N9 169.7(2) . . ? O11 Mn5 N9 86.1(3) . . ? O17 Mn5 O10 90.6(3) . . ? O16 Mn5 O10 88.1(2) . . ? O13 Mn5 O10 95.3(2) . . ? O11 Mn5 O10 161.0(2) . . ? N9 Mn5 O10 75.1(2) . . ? O17 Mn5 Mn4 140.2(3) . . ? O16 Mn5 Mn4 45.83(15) . . ? O13 Mn5 Mn4 37.60(15) . . ? O11 Mn5 Mn4 105.79(19) . . ? N9 Mn5 Mn4 136.8(2) . . ? O10 Mn5 Mn4 89.91(14) . . ? O17 Mn5 Cs1 91.5(3) . . ? O16 Mn5 Cs1 92.66(16) . . ? O13 Mn5 Cs1 54.80(15) . . ? O11 Mn5 Cs1 49.02(19) . . ? N9 Mn5 Cs1 135.14(18) . . ? O10 Mn5 Cs1 149.64(14) . . ? Mn4 Mn5 Cs1 69.60(4) . . ? N1 O1 Mn1 122.9(4) . . ? C3 O2 Mn3 113.5(4) . . ? C3 O2 Mn2 115.4(4) . . ? Mn3 O2 Mn2 131.1(2) . . ? C10 O3 Mn3 128.2(4) . . ? C10 O3 Cs1 124.4(4) . . ? Mn3 O3 Cs1 107.30(19) . . ? C9 O4 C11 116.3(6) . . ? C9 O4 Cs1 125.6(4) . . ? C11 O4 Cs1 116.6(5) . . ? N4 O5 Mn1 122.5(4) . . ? C14 O6 Mn4 112.3(4) . . ? C14 O6 Mn2 114.5(4) . . ? Mn4 O6 Mn2 131.5(2) . . ? C21 O7 Mn4 128.4(5) . . ? C21 O7 Cs1 125.3(5) . . ? Mn4 O7 Cs1 105.7(2) . . ? C20 O8 C22 118.2(9) . . ? C20 O8 Cs1 128.4(5) . . ? C22 O8 Cs1 113.1(8) . . ? N7 O9 Mn1 118.1(4) . . ? C25 O10 Mn2 118.3(4) . . ? C25 O10 Mn5 112.9(4) . . ? Mn2 O10 Mn5 127.5(2) . . ? C32 O11 Mn5 131.0(6) . . ? C32 O11 Cs1 128.9(5) . . ? Mn5 O11 Cs1 99.9(2) . . ? C31 O12 C33 114.0(9) . . ? C31 O12 Cs1 128.1(5) . . ? C33 O12 Cs1 117.8(8) . . ? Mn3 O13 Mn4 124.3(3) . . ? Mn3 O13 Mn5 123.7(3) . . ? Mn4 O13 Mn5 103.9(2) . . ? Mn3 O13 Cs1 101.84(19) . . ? Mn4 O13 Cs1 100.8(2) . . ? Mn5 O13 Cs1 95.15(18) . . ? C34 O14 Mn3 132.0(5) . . ? C34 O15 Mn4 131.1(5) . . ? C36 O16 Mn5 123.7(5) . . ? C36 O16 Mn4 123.6(5) . . ? Mn5 O16 Mn4 94.6(2) . . ? C37 O17 Mn5 135.2(7) . . ? C37 O18 Mn3 137.8(8) . . ? C39 O19 Mn1 126.0(5) . 3_566 ? C39 O19 Mn1 123.9(4) . . ? Mn1 O19 Mn1 102.1(2) 3_566 . ? C40 O20 Mn1 114.7(5) . . ? C2 N1 O1 115.4(5) . . ? C2 N1 Mn2 118.2(4) . . ? O1 N1 Mn2 125.8(4) . . ? C3 N2 N3 109.9(5) . . ? C4 N3 N2 116.2(6) . . ? C4 N3 Mn3 127.6(5) . . ? N2 N3 Mn3 116.2(4) . . ? C13 N4 O5 117.6(5) . . ? C13 N4 Mn2 119.5(4) . . ? O5 N4 Mn2 122.5(4) . . ? C14 N5 N6 110.3(6) . . ? C15 N6 N5 116.1(6) . . ? C15 N6 Mn4 127.7(5) . . ? N5 N6 Mn4 116.2(4) . . ? C24 N7 O9 115.6(6) . . ? C24 N7 Mn2 115.9(5) . . ? O9 N7 Mn2 128.1(4) . . ? C25 N8 N9 110.2(6) . . ? C26 N9 N8 113.9(7) . . ? C26 N9 Mn5 128.7(6) . . ? N8 N9 Mn5 117.3(5) . . ? C2 C1 H1A 109.5 . . ? C2 C1 H1B 109.5 . . ? H1A C1 H1B 109.5 . . ? C2 C1 H1C 109.5 . . ? H1A C1 H1C 109.5 . . ? H1B C1 H1C 109.5 . . ? N1 C2 C3 114.0(6) . . ? N1 C2 C1 123.3(6) . . ? C3 C2 C1 122.7(6) . . ? N2 C3 O2 122.4(6) . . ? N2 C3 C2 119.3(6) . . ? O2 C3 C2 118.3(6) . . ? N3 C4 C5 124.6(6) . . ? N3 C4 H4 117.7 . . ? C5 C4 H4 117.7 . . ? C6 C5 C10 121.1(7) . . ? C6 C5 C4 116.7(7) . . ? C10 C5 C4 122.1(6) . . ? C7 C6 C5 120.2(7) . . ? C7 C6 H6 119.9 . . ? C5 C6 H6 119.9 . . ? C6 C7 C8 120.0(7) . . ? C6 C7 H7 120.0 . . ? C8 C7 H7 120.0 . . ? C9 C8 C7 120.9(7) . . ? C9 C8 H8 119.5 . . ? C7 C8 H8 119.5 . . ? C8 C9 O4 123.7(7) . . ? C8 C9 C10 122.0(7) . . ? O4 C9 C10 114.3(6) . . ? O3 C10 C5 125.1(6) . . ? O3 C10 C9 119.3(6) . . ? C5 C10 C9 115.6(6) . . ? C5 C10 Cs1 161.6(5) . . ? C9 C10 Cs1 80.6(4) . . ? O4 C11 H11A 109.5 . . ? Cs1 C11 H11A 115.5 . . ? O4 C11 H11B 109.5 . . ? Cs1 C11 H11B 133.3 . . ? H11A C11 H11B 109.5 . . ? O4 C11 H11C 109.5 . . ? Cs1 C11 H11C 66.7 . . ? H11A C11 H11C 109.5 . . ? H11B C11 H11C 109.5 . . ? C13 C12 H12A 109.5 . . ? C13 C12 H12B 109.5 . . ? H12A C12 H12B 109.5 . . ? C13 C12 H12C 109.5 . . ? H12A C12 H12C 109.5 . . ? H12B C12 H12C 109.5 . . ? N4 C13 C14 113.7(6) . . ? N4 C13 C12 124.3(7) . . ? C14 C13 C12 122.0(7) . . ? N5 C14 O6 123.4(6) . . ? N5 C14 C13 118.8(6) . . ? O6 C14 C13 117.8(6) . . ? N6 C15 C16 125.5(7) . . ? N6 C15 H15 117.3 . . ? C16 C15 H15 117.3 . . ? C21 C16 C17 120.2(7) . . ? C21 C16 C15 122.5(7) . . ? C17 C16 C15 117.3(7) . . ? C18 C17 C16 120.8(8) . . ? C18 C17 H17 119.6 . . ? C16 C17 H17 119.6 . . ? C17 C18 C19 119.3(8) . . ? C17 C18 H18 120.4 . . ? C19 C18 H18 120.4 . . ? C18 C19 C20 121.0(9) . . ? C18 C19 H19 119.5 . . ? C20 C19 H19 119.5 . . ? O8 C20 C19 122.6(8) . . ? O8 C20 C21 116.1(8) . . ? C19 C20 C21 121.3(9) . . ? O7 C21 C16 125.2(7) . . ? O7 C21 C20 117.4(8) . . ? C16 C21 C20 117.4(7) . . ? O8 C22 Cs1 46.0(6) . . ? O8 C22 H22A 109.5 . . ? Cs1 C22 H22A 121.0 . . ? O8 C22 H22B 109.5 . . ? Cs1 C22 H22B 128.6 . . ? H22A C22 H22B 109.5 . . ? O8 C22 H22C 109.5 . . ? Cs1 C22 H22C 63.6 . . ? H22A C22 H22C 109.5 . . ? H22B C22 H22C 109.5 . . ? C24 C23 H23A 109.5 . . ? C24 C23 H23B 109.5 . . ? H23A C23 H23B 109.5 . . ? C24 C23 H23C 109.5 . . ? H23A C23 H23C 109.5 . . ? H23B C23 H23C 109.5 . . ? N7 C24 C25 112.8(6) . . ? N7 C24 C23 123.6(7) . . ? C25 C24 C23 123.5(7) . . ? O10 C25 N8 124.6(6) . . ? O10 C25 C24 118.7(6) . . ? N8 C25 C24 116.7(7) . . ? N9 C26 C27 126.3(9) . . ? N9 C26 H26 116.8 . . ? C27 C26 H26 116.8 . . ? C32 C27 C28 119.8(9) . . ? C32 C27 C26 123.6(8) . . ? C28 C27 C26 116.6(9) . . ? C29 C28 C27 120.5(11) . . ? C29 C28 H28 119.7 . . ? C27 C28 H28 119.7 . . ? C30 C29 C28 120.4(10) . . ? C30 C29 H29 119.8 . . ? C28 C29 H29 119.8 . . ? C31 C30 C29 120.2(9) . . ? C31 C30 H30 119.9 . . ? C29 C30 H30 119.9 . . ? O12 C31 C30 125.3(9) . . ? O12 C31 C32 114.2(9) . . ? C30 C31 C32 120.6(10) . . ? O11 C32 C27 124.0(8) . . ? O11 C32 C31 117.6(9) . . ? C27 C32 C31 118.3(8) . . ? O12 C33 H33A 109.5 . . ? Cs1 C33 H33A 121.5 . . ? O12 C33 H33B 109.5 . . ? Cs1 C33 H33B 127.4 . . ? H33A C33 H33B 109.5 . . ? O12 C33 H33C 109.5 . . ? Cs1 C33 H33C 66.4 . . ? H33A C33 H33C 109.5 . . ? H33B C33 H33C 109.5 . . ? O14 C34 O15 125.0(7) . . ? O14 C34 C35 118.8(7) . . ? O15 C34 C35 116.2(7) . . ? C34 C35 H35A 109.5 . . ? C34 C35 H35B 109.5 . . ? H35A C35 H35B 109.5 . . ? C34 C35 H35C 109.5 . . ? H35A C35 H35C 109.5 . . ? H35B C35 H35C 109.5 . . ? O16 C36 H36A 109.5 . . ? O16 C36 H36B 109.5 . . ? H36A C36 H36B 109.5 . . ? O16 C36 H36C 109.5 . . ? H36A C36 H36C 109.5 . . ? H36B C36 H36C 109.5 . . ? O18 C37 O17 120.4(10) . . ? O18 C37 C38 128.2(11) . . ? O17 C37 C38 111.1(10) . . ? C37 C38 H38A 109.5 . . ? C37 C38 H38B 109.5 . . ? H38A C38 H38B 109.5 . . ? C37 C38 H38C 109.5 . . ? H38A C38 H38C 109.5 . . ? H38B C38 H38C 109.5 . . ? O19 C39 H39A 109.5 . . ? O19 C39 H39B 109.5 . . ? H39A C39 H39B 109.5 . . ? O19 C39 H39C 109.5 . . ? H39A C39 H39C 109.5 . . ? H39B C39 H39C 109.5 . . ? O20 C40 H40A 109.5 . . ? O20 C40 H40B 109.5 . . ? H40A C40 H40B 109.5 . . ? O20 C40 H40C 109.5 . . ? H40A C40 H40C 109.5 . . ? H40B C40 H40C 109.5 . . ? _diffrn_measured_fraction_theta_max 0.999 _diffrn_reflns_theta_full 26.50 _diffrn_measured_fraction_theta_full 0.999 _refine_diff_density_max 3.985 _refine_diff_density_min -2.427 _refine_diff_density_rms 0.186