Supplementary Material (ESI) for Dalton Transactions This journal is © The Royal Society of Chemistry 2009 data_global _journal_name_full 'Dalton Trans.' _journal_coden_Cambridge 0222 _publ_contact_author_name 'Yongge Wei' _publ_contact_author_email YONGGEWEI@MAIL.TSINGHUA.EDU.CN _publ_section_title ; Convenient Syntheses and Structural Characterizations of Mono-substituted Alkylimido Hexamolybdates: [Mo6O18(NR)]2- (R = Me, Et, n-Pr, i-Pr, n-Bu, t-Bu, Cy, Hex, Ode) ; _publ_contact_author_address ; Department of Chemistry Tsinghua University Beijing 100084 P. R. China ; loop_ _publ_author_name 'Yongge Wei.' 'Jian Hao.' 'Qiang Li.' 'Longsheng Wang.' 'Panchao Yin.' ; Gu Yuan ; 'Yulin Zhu.' 'Li Zhu.' # Attachment 'LQ8-Dalton.CIF' data_compound-2 _database_code_depnum_ccdc_archive 'CCDC 688713' _database_code_CSD ? _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C34 H77 Mo6 N3 O18' _chemical_formula_weight 1391.63 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' Mo Mo -1.6832 0.6857 '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 2(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 12.542(4) _cell_length_b 22.590(7) _cell_length_c 18.807(6) _cell_angle_alpha 90.00 _cell_angle_beta 104.422(6) _cell_angle_gamma 90.00 _cell_volume 5160(3) _cell_formula_units_Z 4 _cell_measurement_temperature 296(2) __cell_measurement_reflns_used 1499 _cell_measurement_theta_min 2.24 _cell_measurement_theta_max 16.18 _exptl_crystal_description rod _exptl_crystal_colour yellow _exptl_crystal_size_max 0.30 _exptl_crystal_size_mid 0.10 _exptl_crystal_size_min 0.05 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.791 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 2792 _exptl_absorpt_coefficient_mu 1.479 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.6653 _exptl_absorpt_correction_T_max 0.9297 _exptl_absorpt_process_details ? _exptl_special_details ; ? ; _diffrn_ambient_temperature 296(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 'CCD area detector' _diffrn_measurement_method 'phi and omega scans' _diffrn_detector_area_resol_mean ? _diffrn_reflns_number 24640 _diffrn_reflns_av_R_equivalents 0.0730 _diffrn_reflns_av_sigmaI/netI 0.1340 _diffrn_reflns_limit_h_min -15 _diffrn_reflns_limit_h_max 15 _diffrn_reflns_limit_k_min -27 _diffrn_reflns_limit_k_max 27 _diffrn_reflns_limit_l_min -17 _diffrn_reflns_limit_l_max 23 _diffrn_reflns_theta_min 1.44 _diffrn_reflns_theta_max 26.00 _reflns_number_total 10130 _reflns_number_gt 4909 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'Bruker SMART' _computing_cell_refinement 'Bruker SMART' _computing_data_reduction 'Bruker SAINT' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _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^)+(0.0583P)^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_extinction_coef ? _refine_ls_number_reflns 10130 _refine_ls_number_parameters 451 _refine_ls_number_restraints 427 _refine_ls_R_factor_all 0.0899 _refine_ls_R_factor_gt 0.0605 _refine_ls_wR_factor_ref 0.1557 _refine_ls_wR_factor_gt 0.1516 _refine_ls_goodness_of_fit_ref 1.012 _refine_ls_restrained_S_all 1.048 _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 Mo1 Mo 0.33298(7) 0.66702(3) 0.29843(4) 0.0709(2) Uani 1 1 d U . . Mo2 Mo 0.44793(6) 0.65486(4) 0.16169(4) 0.0769(2) Uani 1 1 d U . . Mo3 Mo 0.34656(8) 0.52081(3) 0.12978(4) 0.0741(2) Uani 1 1 d . . . Mo4 Mo 0.23158(6) 0.53436(3) 0.26840(4) 0.05977(19) Uani 1 1 d . . . Mo5 Mo 0.49659(6) 0.55554(3) 0.29360(4) 0.0631(2) Uani 1 1 d . . . Mo6 Mo 0.18234(6) 0.63283(3) 0.13524(4) 0.05679(18) Uani 1 1 d . . . O1 O 0.3359(4) 0.5947(2) 0.2158(2) 0.0482(10) Uani 1 1 d . . . O2 O 0.5298(4) 0.6999(2) 0.1285(2) 0.0566(9) Uani 1 1 d U . . O3 O 0.3709(4) 0.4725(2) 0.0680(2) 0.0566(9) Uani 1 1 d . . . O4 O 0.1511(6) 0.4920(3) 0.3055(4) 0.099(2) Uani 1 1 d . . . O5 O 0.6081(6) 0.5291(4) 0.3534(3) 0.095(2) Uani 1 1 d . . . O6 O 0.0701(5) 0.6615(3) 0.0778(4) 0.093(2) Uani 1 1 d . . . O9 O 0.1259(5) 0.5762(3) 0.1935(3) 0.0779(17) Uani 1 1 d . . . O11 O 0.3775(4) 0.5142(2) 0.3223(3) 0.0600(13) Uani 1 1 d . . . O15 O 0.2571(5) 0.4868(2) 0.1889(3) 0.0684(14) Uani 1 1 d . . . O18 O 0.2453(5) 0.6040(3) 0.3231(3) 0.0814(18) Uani 1 1 d . . . O7 O 0.4598(5) 0.6213(3) 0.3468(3) 0.0773(16) Uani 1 1 d . . . O8 O 0.4711(5) 0.5053(3) 0.2105(3) 0.0758(17) Uani 1 1 d . . . O10 O 0.5517(5) 0.6130(3) 0.2365(4) 0.0895(19) Uani 1 1 d . . . O12 O 0.3011(4) 0.6730(2) 0.1085(3) 0.0553(11) Uani 1 1 d . . . O13 O 0.2106(5) 0.6842(2) 0.2186(3) 0.0713(15) Uani 1 1 d . . . O14 O 0.2216(5) 0.5664(2) 0.0819(3) 0.0655(14) Uani 1 1 d . . . O16 O 0.4310(6) 0.5845(3) 0.1054(3) 0.091(2) Uani 1 1 d . . . O17 O 0.4221(5) 0.7023(2) 0.2421(3) 0.0806(18) Uani 1 1 d . . . N2 N 0.1665(8) 0.8451(4) 0.0710(5) 0.1083(15) Uani 1 1 d U . . N3 N 0.1823(10) 0.4742(6) -0.1559(6) 0.1330(19) Uani 1 1 d U . . C3 C 0.0809(7) 0.8936(3) 0.0398(5) 0.071(2) Uani 1 1 d DU . . H3A H 0.0978 0.9275 0.0724 0.086 Uiso 1 1 calc R . . H3B H 0.0925 0.9058 -0.0071 0.086 Uiso 1 1 calc R . . C4 C -0.0380(7) 0.8808(3) 0.0286(4) 0.0656(18) Uani 1 1 d DU . . H4A H -0.0600 0.8507 -0.0090 0.079 Uiso 1 1 calc R . . H4B H -0.0517 0.8657 0.0738 0.079 Uiso 1 1 calc R . . C5 C -0.1041(9) 0.9349(4) 0.0060(6) 0.100(3) Uani 1 1 d DU . . H5A H -0.0714 0.9672 0.0382 0.120 Uiso 1 1 calc R . . H5B H -0.1008 0.9454 -0.0434 0.120 Uiso 1 1 calc R . . C6 C -0.2200(10) 0.9291(6) 0.0076(7) 0.136(5) Uani 1 1 d DU . . H6A H -0.2585 0.9652 -0.0096 0.204 Uiso 1 1 calc R . . H6B H -0.2245 0.9215 0.0570 0.204 Uiso 1 1 calc R . . H6C H -0.2530 0.8969 -0.0235 0.204 Uiso 1 1 calc R . . C7 C 0.1503(12) 0.8188(4) 0.1398(6) 0.1112(19) Uani 1 1 d DU . . H7A H 0.2124 0.7928 0.1594 0.133 Uiso 1 1 calc R . . H7B H 0.0852 0.7940 0.1269 0.133 Uiso 1 1 calc R . . C8 C 0.1381(11) 0.8591(4) 0.2009(6) 0.1112(19) Uani 1 1 d DU . . H8A H 0.2082 0.8785 0.2207 0.133 Uiso 1 1 calc R . . H8B H 0.0852 0.8897 0.1800 0.133 Uiso 1 1 calc R . . C9 C 0.1037(9) 0.8320(4) 0.2607(6) 0.1112(19) Uani 1 1 d DU . . H9A H 0.0966 0.8630 0.2949 0.133 Uiso 1 1 calc R . . H9B H 0.1622 0.8059 0.2861 0.133 Uiso 1 1 calc RD . . C10 C -0.0031(9) 0.7967(4) 0.2425(6) 0.1112(19) Uani 1 1 d DU . . H10A H -0.0143 0.7789 0.2864 0.167 Uiso 1 1 calc RD . . H10B H 0.0012 0.7662 0.2077 0.167 Uiso 1 1 calc R . . H10C H -0.0635 0.8226 0.2218 0.167 Uiso 1 1 calc R . . C11 C 0.2739(9) 0.8712(5) 0.0901(7) 0.1083(15) Uani 1 1 d DU . . H11A H 0.2737 0.9017 0.1263 0.130 Uiso 1 1 calc R . . H11B H 0.2851 0.8909 0.0466 0.130 Uiso 1 1 calc R . . C12 C 0.3710(8) 0.8327(5) 0.1193(7) 0.1083(15) Uani 1 1 d DU . . H12A H 0.3695 0.8173 0.1672 0.130 Uiso 1 1 calc R . . H12B H 0.3712 0.7996 0.0864 0.130 Uiso 1 1 calc R . . C13 C 0.4679(8) 0.8692(5) 0.1247(7) 0.1083(15) Uani 1 1 d DU . . H13A H 0.4649 0.9010 0.1588 0.130 Uiso 1 1 calc R . . H13B H 0.4613 0.8873 0.0770 0.130 Uiso 1 1 calc R . . C14 C 0.5791(8) 0.8424(5) 0.1476(7) 0.1083(15) Uani 1 1 d DU . . H14A H 0.6327 0.8699 0.1388 0.163 Uiso 1 1 calc R . . H14B H 0.5811 0.8069 0.1198 0.163 Uiso 1 1 calc R . . H14C H 0.5954 0.8329 0.1989 0.163 Uiso 1 1 calc R . . C15 C 0.1537(8) 0.7983(3) 0.0140(5) 0.079(2) Uani 1 1 d DU . . H15A H 0.0766 0.7871 0.0010 0.094 Uiso 1 1 calc R . . H15B H 0.1944 0.7641 0.0376 0.094 Uiso 1 1 calc R . . C16 C 0.1861(8) 0.8076(4) -0.0561(5) 0.082(2) Uani 1 1 d DU . . H16A H 0.1473 0.8419 -0.0807 0.098 Uiso 1 1 calc R . . H16B H 0.2643 0.8162 -0.0450 0.098 Uiso 1 1 calc R . . C17 C 0.1630(11) 0.7568(5) -0.1066(5) 0.117(4) Uani 1 1 d DU . . H17A H 0.0839 0.7509 -0.1208 0.140 Uiso 1 1 calc R . . H17B H 0.1950 0.7218 -0.0796 0.140 Uiso 1 1 calc R . . C18 C 0.2032(11) 0.7600(6) -0.1757(6) 0.128(5) Uani 1 1 d DU . . H18A H 0.1816 0.7248 -0.2042 0.192 Uiso 1 1 calc R . . H18B H 0.2820 0.7633 -0.1630 0.192 Uiso 1 1 calc R . . H18C H 0.1715 0.7940 -0.2038 0.192 Uiso 1 1 calc R . . C19 C 0.1155(9) 0.4979(5) -0.1064(5) 0.089(2) Uani 1 1 d DU . . H19A H 0.0641 0.4671 -0.1012 0.107 Uiso 1 1 calc R . . H19B H 0.1653 0.5035 -0.0584 0.107 Uiso 1 1 calc R . . C20 C 0.0511(7) 0.5537(4) -0.1250(5) 0.090(3) Uani 1 1 d DU . . H20A H 0.1023 0.5862 -0.1225 0.108 Uiso 1 1 calc R . . H20B H 0.0077 0.5509 -0.1754 0.108 Uiso 1 1 calc R . . C21 C -0.0213(7) 0.5676(5) -0.0794(6) 0.105(3) Uani 1 1 d DU . . H21A H 0.0211 0.5697 -0.0287 0.126 Uiso 1 1 calc R . . H21B H -0.0748 0.5360 -0.0830 0.126 Uiso 1 1 calc R . . C22 C -0.0815(12) 0.6256(5) -0.1001(8) 0.135(5) Uani 1 1 d DU . . H22A H -0.1263 0.6337 -0.0667 0.203 Uiso 1 1 calc R . . H22B H -0.1273 0.6229 -0.1492 0.203 Uiso 1 1 calc R . . H22C H -0.0290 0.6569 -0.0976 0.203 Uiso 1 1 calc R . . C23 C 0.2508(12) 0.4218(6) -0.1215(10) 0.144(3) Uani 1 1 d DU . . H23A H 0.3015 0.4115 -0.1510 0.173 Uiso 1 1 calc R . . H23B H 0.2940 0.4328 -0.0730 0.173 Uiso 1 1 calc R . . C24 C 0.1831(12) 0.3695(6) -0.1152(10) 0.144(3) Uani 1 1 d DU . . H24A H 0.1460 0.3555 -0.1638 0.173 Uiso 1 1 calc R . . H24B H 0.1274 0.3803 -0.0898 0.173 Uiso 1 1 calc R . . C25 C 0.2543(12) 0.3214(6) -0.0738(9) 0.144(3) Uani 1 1 d DU . . H25A H 0.3194 0.3156 -0.0921 0.173 Uiso 1 1 calc R . . H25B H 0.2769 0.3304 -0.0218 0.173 Uiso 1 1 calc R . . C26 C 0.1817(12) 0.2680(6) -0.0878(9) 0.144(3) Uani 1 1 d DU . . H26A H 0.2200 0.2348 -0.0613 0.217 Uiso 1 1 calc R . . H26B H 0.1624 0.2592 -0.1394 0.217 Uiso 1 1 calc R . . H26C H 0.1160 0.2755 -0.0718 0.217 Uiso 1 1 calc R . . C27 C 0.1146(11) 0.4581(8) -0.2260(6) 0.1330(19) Uani 1 1 d DU . . H27A H 0.0717 0.4928 -0.2458 0.160 Uiso 1 1 calc R . . H27B H 0.0630 0.4285 -0.2177 0.160 Uiso 1 1 calc R . . C28 C 0.1644(10) 0.4347(7) -0.2852(6) 0.1330(19) Uani 1 1 d DU . . H28A H 0.2233 0.4074 -0.2635 0.160 Uiso 1 1 calc R . . H28B H 0.1964 0.4673 -0.3063 0.160 Uiso 1 1 calc R . . C29 C 0.0810(11) 0.4027(6) -0.3467(6) 0.1330(19) Uani 1 1 d DU . . H29A H 0.1146 0.3699 -0.3662 0.160 Uiso 1 1 calc R . . H29B H 0.0185 0.3884 -0.3299 0.160 Uiso 1 1 calc R . . C30 C 0.0483(11) 0.4513(6) -0.4021(6) 0.1330(19) Uani 1 1 d DU . . H30A H -0.0028 0.4362 -0.4450 0.199 Uiso 1 1 calc R . . H30B H 0.1125 0.4661 -0.4154 0.199 Uiso 1 1 calc R . . H30C H 0.0144 0.4828 -0.3814 0.199 Uiso 1 1 calc R . . C31 C 0.2599(9) 0.5251(7) -0.1633(6) 0.122(4) Uani 1 1 d DU . . H31A H 0.3029 0.5120 -0.1967 0.146 Uiso 1 1 calc R . . H31B H 0.2144 0.5577 -0.1872 0.146 Uiso 1 1 calc R . . C32 C 0.3385(9) 0.5496(5) -0.0971(6) 0.110(3) Uani 1 1 d DU . . H32A H 0.3950 0.5206 -0.0771 0.132 Uiso 1 1 calc R . . H32B H 0.2999 0.5589 -0.0597 0.132 Uiso 1 1 calc R . . C33 C 0.3907(9) 0.6052(5) -0.1182(6) 0.114(4) Uani 1 1 d DU . . H33A H 0.4414 0.5932 -0.1470 0.137 Uiso 1 1 calc R . . H33B H 0.3330 0.6281 -0.1504 0.137 Uiso 1 1 calc R . . C34 C 0.4518(14) 0.6459(7) -0.0591(7) 0.158(6) Uani 1 1 d DU . . H34A H 0.4811 0.6785 -0.0810 0.236 Uiso 1 1 calc R . . H34B H 0.5110 0.6247 -0.0270 0.236 Uiso 1 1 calc R . . H34C H 0.4025 0.6605 -0.0315 0.236 Uiso 1 1 calc R . . N1 N 0.3020(10) 0.7124(5) 0.3629(6) 0.124(2) Uani 1 1 d U . . C1 C 0.2711(10) 0.7513(7) 0.4179(6) 0.124(2) Uani 1 1 d DU . . H1A H 0.2671 0.7922 0.4016 0.149 Uiso 1 1 calc RD . . H1B H 0.3252 0.7485 0.4647 0.149 Uiso 1 1 calc R . . C2 C 0.1589(9) 0.7304(6) 0.4255(6) 0.124(2) Uani 1 1 d DU . . H2A H 0.1360 0.7545 0.4611 0.186 Uiso 1 1 calc R . . H2B H 0.1640 0.6899 0.4413 0.186 Uiso 1 1 calc RD . . H2C H 0.1061 0.7337 0.3790 0.186 Uiso 1 1 calc RD . . 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 Mo1 0.0909(6) 0.0497(4) 0.0674(4) -0.0103(3) 0.0108(4) 0.0018(4) Mo2 0.0600(4) 0.0789(5) 0.0919(5) 0.0297(5) 0.0190(4) -0.0034(4) Mo3 0.0974(6) 0.0610(4) 0.0597(4) -0.0050(3) 0.0117(4) 0.0168(4) Mo4 0.0560(4) 0.0464(3) 0.0757(4) 0.0145(3) 0.0141(3) -0.0009(3) Mo5 0.0526(4) 0.0664(4) 0.0660(4) 0.0138(3) 0.0069(3) 0.0019(3) Mo6 0.0543(4) 0.0462(3) 0.0636(3) 0.0094(3) 0.0026(3) -0.0005(3) O1 0.052(3) 0.045(2) 0.049(2) -0.003(2) 0.016(2) 0.008(2) O2 0.065(2) 0.063(2) 0.0324(12) -0.0024(15) -0.0063(12) 0.0101(18) O3 0.065(2) 0.063(2) 0.0324(12) -0.0024(15) -0.0063(12) 0.0101(18) O4 0.077(4) 0.098(5) 0.121(5) 0.067(4) 0.025(4) 0.005(4) O5 0.074(4) 0.119(6) 0.089(4) 0.017(4) 0.013(3) -0.005(4) O6 0.056(4) 0.096(5) 0.116(5) 0.008(4) 0.002(3) 0.011(4) O9 0.051(3) 0.077(4) 0.097(4) 0.030(3) 0.002(3) -0.012(3) O11 0.055(3) 0.044(2) 0.070(3) -0.006(2) -0.005(2) 0.008(2) O15 0.071(4) 0.051(3) 0.075(3) 0.004(3) 0.003(3) 0.009(3) O18 0.090(4) 0.090(4) 0.065(3) 0.015(3) 0.021(3) 0.034(4) O7 0.069(4) 0.060(3) 0.089(4) 0.003(3) -0.005(3) 0.000(3) O8 0.077(4) 0.082(4) 0.082(3) 0.023(3) 0.046(3) 0.027(3) O10 0.073(4) 0.094(5) 0.098(4) 0.046(4) 0.015(3) 0.012(4) O12 0.059(3) 0.042(2) 0.063(3) 0.003(2) 0.012(2) -0.006(2) O13 0.084(4) 0.043(2) 0.081(3) 0.005(3) 0.009(3) 0.012(3) O14 0.084(4) 0.056(3) 0.053(2) 0.013(2) 0.010(2) 0.007(3) O16 0.086(4) 0.117(6) 0.075(3) 0.021(4) 0.029(3) 0.018(4) O17 0.087(5) 0.050(3) 0.095(4) 0.012(3) 0.004(3) -0.014(3) N2 0.103(3) 0.084(3) 0.121(3) 0.001(3) -0.005(3) 0.003(2) N3 0.110(4) 0.170(5) 0.117(4) -0.021(4) 0.025(3) 0.007(4) C3 0.090(5) 0.042(3) 0.069(4) -0.005(4) -0.004(4) 0.015(4) C4 0.094(5) 0.036(3) 0.068(4) -0.002(4) 0.022(4) -0.006(3) C5 0.132(8) 0.075(6) 0.083(5) 0.001(5) 0.006(6) 0.045(6) C6 0.140(9) 0.150(12) 0.120(9) -0.005(10) 0.035(8) 0.055(10) C7 0.152(6) 0.056(3) 0.119(4) -0.008(3) 0.022(4) -0.001(3) C8 0.152(6) 0.056(3) 0.119(4) -0.008(3) 0.022(4) -0.001(3) C9 0.152(6) 0.056(3) 0.119(4) -0.008(3) 0.022(4) -0.001(3) C10 0.152(6) 0.056(3) 0.119(4) -0.008(3) 0.022(4) -0.001(3) C11 0.103(3) 0.084(3) 0.121(3) 0.001(3) -0.005(3) 0.003(2) C12 0.103(3) 0.084(3) 0.121(3) 0.001(3) -0.005(3) 0.003(2) C13 0.103(3) 0.084(3) 0.121(3) 0.001(3) -0.005(3) 0.003(2) C14 0.103(3) 0.084(3) 0.121(3) 0.001(3) -0.005(3) 0.003(2) C15 0.083(6) 0.033(3) 0.108(5) -0.002(4) 0.001(5) 0.003(4) C16 0.079(6) 0.071(5) 0.086(4) 0.027(4) 0.002(4) 0.000(5) C17 0.133(11) 0.109(9) 0.096(6) -0.016(6) 0.006(6) -0.009(8) C18 0.131(11) 0.125(10) 0.119(8) -0.022(8) 0.016(7) 0.055(9) C19 0.092(6) 0.097(6) 0.076(5) 0.011(5) 0.016(4) -0.018(5) C20 0.055(5) 0.070(5) 0.122(7) 0.016(5) -0.022(4) -0.020(4) C21 0.035(4) 0.133(8) 0.137(8) 0.012(8) 0.002(4) -0.016(5) C22 0.136(12) 0.120(9) 0.162(12) -0.023(9) 0.058(10) -0.011(7) C23 0.107(5) 0.134(5) 0.190(7) -0.029(5) 0.034(5) -0.009(4) C24 0.107(5) 0.134(5) 0.190(7) -0.029(5) 0.034(5) -0.009(4) C25 0.107(5) 0.134(5) 0.190(7) -0.029(5) 0.034(5) -0.009(4) C26 0.107(5) 0.134(5) 0.190(7) -0.029(5) 0.034(5) -0.009(4) C27 0.110(4) 0.170(5) 0.117(4) -0.021(4) 0.025(3) 0.007(4) C28 0.110(4) 0.170(5) 0.117(4) -0.021(4) 0.025(3) 0.007(4) C29 0.110(4) 0.170(5) 0.117(4) -0.021(4) 0.025(3) 0.007(4) C30 0.110(4) 0.170(5) 0.117(4) -0.021(4) 0.025(3) 0.007(4) C31 0.074(7) 0.177(9) 0.115(7) -0.001(8) 0.024(5) -0.007(6) C32 0.081(7) 0.142(9) 0.116(7) 0.008(7) 0.044(5) 0.002(6) C33 0.073(6) 0.150(10) 0.135(8) 0.013(8) 0.052(6) 0.000(6) C34 0.189(17) 0.172(14) 0.119(9) 0.016(9) 0.051(10) -0.033(12) N1 0.119(6) 0.152(6) 0.101(4) 0.004(4) 0.026(4) 0.018(5) C1 0.119(6) 0.152(6) 0.101(4) 0.004(4) 0.026(4) 0.018(5) C2 0.119(6) 0.152(6) 0.101(4) 0.004(4) 0.026(4) 0.018(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 Mo1 N1 1.705(11) . ? Mo1 O17 1.896(7) . ? Mo1 O13 1.901(6) . ? Mo1 O7 1.925(6) . ? Mo1 O18 1.925(7) . ? Mo1 O1 2.260(4) . ? Mo2 O2 1.672(6) . ? Mo2 O16 1.891(8) . ? Mo2 O12 1.909(5) . ? Mo2 O10 1.912(6) . ? Mo2 O17 1.946(7) . ? Mo2 O1 2.359(5) . ? Mo3 O3 1.677(5) . ? Mo3 O14 1.903(5) . ? Mo3 O16 1.910(8) . ? Mo3 O8 1.920(6) . ? Mo3 O15 1.925(6) . ? Mo3 O1 2.352(4) . ? Mo4 O4 1.664(6) . ? Mo4 O18 1.864(7) . ? Mo4 O11 1.913(5) . ? Mo4 O9 1.925(6) . ? Mo4 O15 1.931(6) . ? Mo4 O1 2.279(5) . ? Mo5 O5 1.671(7) . ? Mo5 O8 1.892(6) . ? Mo5 O7 1.910(6) . ? Mo5 O10 1.920(6) . ? Mo5 O11 1.948(6) . ? Mo5 O1 2.349(4) . ? Mo6 O6 1.677(6) . ? Mo6 O13 1.911(6) . ? Mo6 O12 1.916(5) . ? Mo6 O9 1.929(6) . ? Mo6 O14 1.936(6) . ? Mo6 O1 2.301(4) . ? N2 C11 1.433(14) . ? N2 C7 1.484(15) . ? N2 C15 1.485(12) . ? N2 C3 1.544(11) . ? N3 C27 1.426(15) . ? N3 C19 1.498(15) . ? N3 C23 1.511(18) . ? N3 C31 1.535(16) . ? C3 C4 1.481(10) . ? C3 H3A 0.9700 . ? C3 H3B 0.9700 . ? C4 C5 1.479(9) . ? C4 H4A 0.9700 . ? C4 H4B 0.9700 . ? C5 C6 1.468(12) . ? C5 H5A 0.9700 . ? C5 H5B 0.9700 . ? C6 H6A 0.9600 . ? C6 H6B 0.9600 . ? C6 H6C 0.9600 . ? C7 C8 1.503(11) . ? C7 H7A 0.9700 . ? C7 H7B 0.9700 . ? C8 C9 1.439(11) . ? C8 H8A 0.9700 . ? C8 H8B 0.9700 . ? C9 C10 1.522(8) . ? C9 H9A 0.9700 . ? C9 H9B 0.9700 . ? C10 H10A 0.9600 . ? C10 H10B 0.9600 . ? C10 H10C 0.9600 . ? C11 C12 1.486(11) . ? C11 H11A 0.9700 . ? C11 H11B 0.9700 . ? C12 C13 1.451(12) . ? C12 H12A 0.9700 . ? C12 H12B 0.9700 . ? C13 C14 1.482(8) . ? C13 H13A 0.9700 . ? C13 H13B 0.9700 . ? C14 H14A 0.9600 . ? C14 H14B 0.9600 . ? C14 H14C 0.9600 . ? C15 C16 1.489(10) . ? C15 H15A 0.9700 . ? C15 H15B 0.9700 . ? C16 C17 1.472(11) . ? C16 H16A 0.9700 . ? C16 H16B 0.9700 . ? C17 C18 1.508(8) . ? C17 H17A 0.9700 . ? C17 H17B 0.9700 . ? C18 H18A 0.9600 . ? C18 H18B 0.9600 . ? C18 H18C 0.9600 . ? C19 C20 1.490(11) . ? C19 H19A 0.9700 . ? C19 H19B 0.9700 . ? C20 C21 1.431(11) . ? C20 H20A 0.9700 . ? C20 H20B 0.9700 . ? C21 C22 1.513(8) . ? C21 H21A 0.9700 . ? C21 H21B 0.9700 . ? C22 H22A 0.9600 . ? C22 H22B 0.9600 . ? C22 H22C 0.9600 . ? C23 C24 1.477(12) . ? C23 H23A 0.9700 . ? C23 H23B 0.9700 . ? C24 C25 1.497(13) . ? C24 H24A 0.9700 . ? C24 H24B 0.9700 . ? C25 C26 1.495(12) . ? C25 H25A 0.9700 . ? C25 H25B 0.9700 . ? C26 H26A 0.9600 . ? C26 H26B 0.9600 . ? C26 H26C 0.9600 . ? C27 C28 1.502(12) . ? C27 H27A 0.9700 . ? C27 H27B 0.9700 . ? C28 C29 1.532(12) . ? C28 H28A 0.9700 . ? C28 H28B 0.9700 . ? C29 C30 1.499(8) . ? C29 H29A 0.9700 . ? C29 H29B 0.9700 . ? C30 H30A 0.9600 . ? C30 H30B 0.9600 . ? C30 H30C 0.9600 . ? C31 C32 1.489(11) . ? C31 H31A 0.9700 . ? C31 H31B 0.9700 . ? C32 C33 1.514(11) . ? C32 H32A 0.9700 . ? C32 H32B 0.9700 . ? C33 C34 1.497(8) . ? C33 H33A 0.9700 . ? C33 H33B 0.9700 . ? C34 H34A 0.9600 . ? C34 H34B 0.9600 . ? C34 H34C 0.9600 . ? N1 C1 1.481(15) . ? C1 C2 1.524(9) . ? C1 H1A 0.9700 . ? C1 H1B 0.9700 . ? C2 H2A 0.9600 . ? C2 H2B 0.9600 . ? C2 H2C 0.9600 . ? 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 N1 Mo1 O17 114.5(4) . . ? N1 Mo1 O13 99.0(4) . . ? O17 Mo1 O13 86.9(3) . . ? N1 Mo1 O7 107.1(4) . . ? O17 Mo1 O7 87.5(3) . . ? O13 Mo1 O7 153.2(2) . . ? N1 Mo1 O18 91.6(5) . . ? O17 Mo1 O18 153.8(2) . . ? O13 Mo1 O18 86.8(3) . . ? O7 Mo1 O18 86.8(3) . . ? N1 Mo1 O1 165.6(4) . . ? O17 Mo1 O1 78.9(2) . . ? O13 Mo1 O1 75.7(2) . . ? O7 Mo1 O1 77.5(2) . . ? O18 Mo1 O1 74.9(2) . . ? O2 Mo2 O16 107.2(3) . . ? O2 Mo2 O12 106.0(2) . . ? O16 Mo2 O12 85.9(3) . . ? O2 Mo2 O10 101.9(3) . . ? O16 Mo2 O10 87.5(3) . . ? O12 Mo2 O10 152.0(3) . . ? O2 Mo2 O17 101.1(2) . . ? O16 Mo2 O17 151.7(3) . . ? O12 Mo2 O17 87.9(2) . . ? O10 Mo2 O17 85.1(3) . . ? O2 Mo2 O1 176.25(18) . . ? O16 Mo2 O1 76.3(2) . . ? O12 Mo2 O1 75.49(19) . . ? O10 Mo2 O1 76.5(2) . . ? O17 Mo2 O1 75.5(2) . . ? O3 Mo3 O14 107.2(2) . . ? O3 Mo3 O16 96.7(3) . . ? O14 Mo3 O16 85.4(3) . . ? O3 Mo3 O8 100.2(2) . . ? O14 Mo3 O8 152.2(2) . . ? O16 Mo3 O8 86.4(3) . . ? O3 Mo3 O15 111.9(2) . . ? O14 Mo3 O15 87.6(2) . . ? O16 Mo3 O15 151.3(3) . . ? O8 Mo3 O15 87.0(2) . . ? O3 Mo3 O1 172.0(2) . . ? O14 Mo3 O1 76.13(19) . . ? O16 Mo3 O1 76.1(2) . . ? O8 Mo3 O1 76.1(2) . . ? O15 Mo3 O1 75.2(2) . . ? O4 Mo4 O18 103.6(4) . . ? O4 Mo4 O11 104.0(3) . . ? O18 Mo4 O11 87.9(2) . . ? O4 Mo4 O9 102.1(3) . . ? O18 Mo4 O9 86.7(3) . . ? O11 Mo4 O9 153.9(3) . . ? O4 Mo4 O15 103.9(3) . . ? O18 Mo4 O15 152.4(3) . . ? O11 Mo4 O15 87.5(2) . . ? O9 Mo4 O15 85.6(3) . . ? O4 Mo4 O1 177.7(3) . . ? O18 Mo4 O1 75.6(2) . . ? O11 Mo4 O1 78.2(2) . . ? O9 Mo4 O1 75.7(2) . . ? O15 Mo4 O1 76.9(2) . . ? O5 Mo5 O8 106.4(3) . . ? O5 Mo5 O7 101.3(3) . . ? O8 Mo5 O7 152.3(2) . . ? O5 Mo5 O10 105.1(3) . . ? O8 Mo5 O10 87.3(3) . . ? O7 Mo5 O10 86.3(3) . . ? O5 Mo5 O11 102.3(3) . . ? O8 Mo5 O11 87.6(2) . . ? O7 Mo5 O11 85.7(2) . . ? O10 Mo5 O11 152.5(2) . . ? O5 Mo5 O1 176.4(3) . . ? O8 Mo5 O1 76.7(2) . . ? O7 Mo5 O1 75.60(19) . . ? O10 Mo5 O1 76.7(2) . . ? O11 Mo5 O1 75.82(18) . . ? O6 Mo6 O13 104.4(3) . . ? O6 Mo6 O12 103.3(3) . . ? O13 Mo6 O12 86.0(2) . . ? O6 Mo6 O9 104.7(3) . . ? O13 Mo6 O9 87.5(3) . . ? O12 Mo6 O9 152.0(2) . . ? O6 Mo6 O14 104.3(3) . . ? O13 Mo6 O14 151.2(2) . . ? O12 Mo6 O14 85.2(2) . . ? O9 Mo6 O14 87.5(3) . . ? O6 Mo6 O1 178.9(3) . . ? O13 Mo6 O1 74.52(19) . . ? O12 Mo6 O1 76.82(18) . . ? O9 Mo6 O1 75.1(2) . . ? O14 Mo6 O1 76.82(18) . . ? Mo1 O1 Mo4 91.42(15) . . ? Mo1 O1 Mo6 91.63(16) . . ? Mo4 O1 Mo6 91.87(17) . . ? Mo1 O1 Mo5 90.15(15) . . ? Mo4 O1 Mo5 90.02(15) . . ? Mo6 O1 Mo5 177.4(2) . . ? Mo1 O1 Mo3 177.6(2) . . ? Mo4 O1 Mo3 90.60(17) . . ? Mo6 O1 Mo3 89.65(14) . . ? Mo5 O1 Mo3 88.50(15) . . ? Mo1 O1 Mo2 89.67(17) . . ? Mo4 O1 Mo2 178.2(2) . . ? Mo6 O1 Mo2 89.51(15) . . ? Mo5 O1 Mo2 88.57(16) . . ? Mo3 O1 Mo2 88.27(14) . . ? Mo4 O9 Mo6 117.2(3) . . ? Mo4 O11 Mo5 115.9(3) . . ? Mo3 O15 Mo4 117.3(3) . . ? Mo4 O18 Mo1 118.1(3) . . ? Mo5 O7 Mo1 116.7(3) . . ? Mo5 O8 Mo3 118.8(3) . . ? Mo2 O10 Mo5 118.2(3) . . ? Mo2 O12 Mo6 118.2(2) . . ? Mo1 O13 Mo6 118.2(3) . . ? Mo3 O14 Mo6 117.4(3) . . ? Mo2 O16 Mo3 119.4(3) . . ? Mo1 O17 Mo2 116.0(3) . . ? C11 N2 C7 105.7(10) . . ? C11 N2 C15 113.6(10) . . ? C7 N2 C15 109.3(8) . . ? C11 N2 C3 108.9(8) . . ? C7 N2 C3 112.5(10) . . ? C15 N2 C3 107.0(7) . . ? C27 N3 C19 111.7(10) . . ? C27 N3 C23 109.9(14) . . ? C19 N3 C23 111.1(11) . . ? C27 N3 C31 110.7(12) . . ? C19 N3 C31 104.7(11) . . ? C23 N3 C31 108.7(11) . . ? C4 C3 N2 119.8(7) . . ? C4 C3 H3A 107.4 . . ? N2 C3 H3A 107.4 . . ? C4 C3 H3B 107.4 . . ? N2 C3 H3B 107.4 . . ? H3A C3 H3B 106.9 . . ? C5 C4 C3 110.7(7) . . ? C5 C4 H4A 109.5 . . ? C3 C4 H4A 109.5 . . ? C5 C4 H4B 109.5 . . ? C3 C4 H4B 109.5 . . ? H4A C4 H4B 108.1 . . ? C6 C5 C4 114.0(10) . . ? C6 C5 H5A 108.7 . . ? C4 C5 H5A 108.7 . . ? C6 C5 H5B 108.7 . . ? C4 C5 H5B 108.7 . . ? H5A C5 H5B 107.6 . . ? C5 C6 H6A 109.5 . . ? C5 C6 H6B 109.5 . . ? H6A C6 H6B 109.5 . . ? C5 C6 H6C 109.5 . . ? H6A C6 H6C 109.5 . . ? H6B C6 H6C 109.5 . . ? N2 C7 C8 119.0(8) . . ? N2 C7 H7A 107.6 . . ? C8 C7 H7A 107.6 . . ? N2 C7 H7B 107.6 . . ? C8 C7 H7B 107.6 . . ? H7A C7 H7B 107.0 . . ? C9 C8 C7 116.5(8) . . ? C9 C8 H8A 108.2 . . ? C7 C8 H8A 108.2 . . ? C9 C8 H8B 108.2 . . ? C7 C8 H8B 108.2 . . ? H8A C8 H8B 107.3 . . ? C8 C9 C10 117.7(10) . . ? C8 C9 H9A 107.9 . . ? C10 C9 H9A 107.9 . . ? C8 C9 H9B 107.9 . . ? C10 C9 H9B 107.9 . . ? H9A C9 H9B 107.2 . . ? C9 C10 H10A 109.5 . . ? C9 C10 H10B 109.5 . . ? H10A C10 H10B 109.5 . . ? C9 C10 H10C 109.5 . . ? H10A C10 H10C 109.5 . . ? H10B C10 H10C 109.5 . . ? N2 C11 C12 119.0(9) . . ? N2 C11 H11A 107.6 . . ? C12 C11 H11A 107.6 . . ? N2 C11 H11B 107.6 . . ? C12 C11 H11B 107.6 . . ? H11A C11 H11B 107.0 . . ? C13 C12 C11 106.7(9) . . ? C13 C12 H12A 110.4 . . ? C11 C12 H12A 110.4 . . ? C13 C12 H12B 110.4 . . ? C11 C12 H12B 110.4 . . ? H12A C12 H12B 108.6 . . ? C12 C13 C14 119.9(9) . . ? C12 C13 H13A 107.3 . . ? C14 C13 H13A 107.3 . . ? C12 C13 H13B 107.3 . . ? C14 C13 H13B 107.3 . . ? H13A C13 H13B 106.9 . . ? C13 C14 H14A 109.5 . . ? C13 C14 H14B 109.5 . . ? H14A C14 H14B 109.5 . . ? C13 C14 H14C 109.5 . . ? H14A C14 H14C 109.5 . . ? H14B C14 H14C 109.5 . . ? N2 C15 C16 122.3(8) . . ? N2 C15 H15A 106.8 . . ? C16 C15 H15A 106.8 . . ? N2 C15 H15B 106.8 . . ? C16 C15 H15B 106.8 . . ? H15A C15 H15B 106.6 . . ? C17 C16 C15 114.1(8) . . ? C17 C16 H16A 108.7 . . ? C15 C16 H16A 108.7 . . ? C17 C16 H16B 108.7 . . ? C15 C16 H16B 108.7 . . ? H16A C16 H16B 107.6 . . ? C16 C17 C18 117.6(10) . . ? C16 C17 H17A 107.9 . . ? C18 C17 H17A 107.9 . . ? C16 C17 H17B 107.9 . . ? C18 C17 H17B 107.9 . . ? H17A C17 H17B 107.2 . . ? C17 C18 H18A 109.5 . . ? C17 C18 H18B 109.5 . . ? H18A C18 H18B 109.5 . . ? C17 C18 H18C 109.5 . . ? H18A C18 H18C 109.5 . . ? H18B C18 H18C 109.5 . . ? C20 C19 N3 120.7(10) . . ? C20 C19 H19A 107.2 . . ? N3 C19 H19A 107.2 . . ? C20 C19 H19B 107.2 . . ? N3 C19 H19B 107.2 . . ? H19A C19 H19B 106.8 . . ? C21 C20 C19 115.6(9) . . ? C21 C20 H20A 108.4 . . ? C19 C20 H20A 108.4 . . ? C21 C20 H20B 108.4 . . ? C19 C20 H20B 108.4 . . ? H20A C20 H20B 107.4 . . ? C20 C21 C22 112.7(10) . . ? C20 C21 H21A 109.1 . . ? C22 C21 H21A 109.1 . . ? C20 C21 H21B 109.1 . . ? C22 C21 H21B 109.1 . . ? H21A C21 H21B 107.8 . . ? C21 C22 H22A 109.5 . . ? C21 C22 H22B 109.5 . . ? H22A C22 H22B 109.5 . . ? C21 C22 H22C 109.5 . . ? H22A C22 H22C 109.5 . . ? H22B C22 H22C 109.5 . . ? C24 C23 N3 112.6(12) . . ? C24 C23 H23A 109.1 . . ? N3 C23 H23A 109.1 . . ? C24 C23 H23B 109.1 . . ? N3 C23 H23B 109.1 . . ? H23A C23 H23B 107.8 . . ? C23 C24 C25 110.0(12) . . ? C23 C24 H24A 109.7 . . ? C25 C24 H24A 109.7 . . ? C23 C24 H24B 109.7 . . ? C25 C24 H24B 109.7 . . ? H24A C24 H24B 108.2 . . ? C26 C25 C24 103.6(11) . . ? C26 C25 H25A 111.0 . . ? C24 C25 H25A 111.0 . . ? C26 C25 H25B 111.0 . . ? C24 C25 H25B 111.0 . . ? H25A C25 H25B 109.0 . . ? C25 C26 H26A 109.5 . . ? C25 C26 H26B 109.5 . . ? H26A C26 H26B 109.5 . . ? C25 C26 H26C 109.5 . . ? H26A C26 H26C 109.5 . . ? H26B C26 H26C 109.5 . . ? N3 C27 C28 120.9(12) . . ? N3 C27 H27A 107.1 . . ? C28 C27 H27A 107.1 . . ? N3 C27 H27B 107.1 . . ? C28 C27 H27B 107.1 . . ? H27A C27 H27B 106.8 . . ? C27 C28 C29 113.2(11) . . ? C27 C28 H28A 108.9 . . ? C29 C28 H28A 108.9 . . ? C27 C28 H28B 108.9 . . ? C29 C28 H28B 108.9 . . ? H28A C28 H28B 107.8 . . ? C30 C29 C28 101.3(10) . . ? C30 C29 H29A 111.5 . . ? C28 C29 H29A 111.5 . . ? C30 C29 H29B 111.5 . . ? C28 C29 H29B 111.5 . . ? H29A C29 H29B 109.3 . . ? C29 C30 H30A 109.5 . . ? C29 C30 H30B 109.5 . . ? H30A C30 H30B 109.5 . . ? C29 C30 H30C 109.5 . . ? H30A C30 H30C 109.5 . . ? H30B C30 H30C 109.5 . . ? C32 C31 N3 120.4(11) . . ? C32 C31 H31A 107.2 . . ? N3 C31 H31A 107.2 . . ? C32 C31 H31B 107.2 . . ? N3 C31 H31B 107.2 . . ? H31A C31 H31B 106.9 . . ? C31 C32 C33 109.2(10) . . ? C31 C32 H32A 109.8 . . ? C33 C32 H32A 109.8 . . ? C31 C32 H32B 109.8 . . ? C33 C32 H32B 109.8 . . ? H32A C32 H32B 108.3 . . ? C34 C33 C32 119.3(10) . . ? C34 C33 H33A 107.5 . . ? C32 C33 H33A 107.5 . . ? C34 C33 H33B 107.5 . . ? C32 C33 H33B 107.5 . . ? H33A C33 H33B 107.0 . . ? 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 . . ? C1 N1 Mo1 178.1(10) . . ? N1 C1 C2 106.8(11) . . ? N1 C1 H1A 110.4 . . ? C2 C1 H1A 110.4 . . ? N1 C1 H1B 110.4 . . ? C2 C1 H1B 110.4 . . ? H1A C1 H1B 108.6 . . ? C1 C2 H2A 109.5 . . ? C1 C2 H2B 109.5 . . ? H2A C2 H2B 109.5 . . ? C1 C2 H2C 109.5 . . ? H2A C2 H2C 109.5 . . ? H2B C2 H2C 109.5 . . ? _diffrn_measured_fraction_theta_max 0.999 _diffrn_reflns_theta_full 26.00 _diffrn_measured_fraction_theta_full 0.999 _refine_diff_density_max 1.219 _refine_diff_density_min -1.731 _refine_diff_density_rms 0.130 #===END data_compound-3 _database_code_depnum_ccdc_archive 'CCDC 688714' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C35 H79 Mo6 N3 O18' _chemical_formula_weight 1405.65 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' Mo Mo -1.6832 0.6857 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting orthorhombic _symmetry_space_group_name_H-M Pbca loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x+1/2, -y, z+1/2' '-x, y+1/2, -z+1/2' 'x+1/2, -y+1/2, -z' '-x, -y, -z' 'x-1/2, y, -z-1/2' 'x, -y-1/2, z-1/2' '-x-1/2, y-1/2, z' _cell_length_a 16.616(3) _cell_length_b 20.009(4) _cell_length_c 31.640(6) _cell_angle_alpha 90.00 _cell_angle_beta 90.00 _cell_angle_gamma 90.00 _cell_volume 10520(4) _cell_formula_units_Z 8 _cell_measurement_temperature 293(2) _cell_measurement_reflns_used 43668 _cell_measurement_theta_min 3.03 _cell_measurement_theta_max 27.54 _exptl_crystal_description block _exptl_crystal_colour orange _exptl_crystal_size_max 0.80 _exptl_crystal_size_mid 0.25 _exptl_crystal_size_min 0.20 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.775 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 5648 _exptl_absorpt_coefficient_mu 1.452 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.3896 _exptl_absorpt_correction_T_max 0.7600 _exptl_absorpt_process_details ? _exptl_special_details ; ? ; _diffrn_ambient_temperature 293(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 'Rigaku RAXIS-RAPID' _diffrn_measurement_method Oscillation _diffrn_detector_area_resol_mean '100x100 micron' _diffrn_reflns_number 49206 _diffrn_reflns_av_R_equivalents 0.0269 _diffrn_reflns_av_sigmaI/netI 0.0256 _diffrn_reflns_limit_h_min -20 _diffrn_reflns_limit_h_max 20 _diffrn_reflns_limit_k_min -24 _diffrn_reflns_limit_k_max 20 _diffrn_reflns_limit_l_min -39 _diffrn_reflns_limit_l_max 33 _diffrn_reflns_theta_min 3.03 _diffrn_reflns_theta_max 26.00 _reflns_number_total 10187 _reflns_number_gt 8371 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'Rigaku RAPID AUTO Ver2.30' _computing_cell_refinement 'Rigaku RAPID AUTO Ver2.30' _computing_data_reduction 'Rigaku RAPID AUTO Ver2.30' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _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^)+(0.0536P)^2^+16.5455P] 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 10187 _refine_ls_number_parameters 580 _refine_ls_number_restraints 434 _refine_ls_R_factor_all 0.0509 _refine_ls_R_factor_gt 0.0404 _refine_ls_wR_factor_ref 0.1101 _refine_ls_wR_factor_gt 0.1043 _refine_ls_goodness_of_fit_ref 1.028 _refine_ls_restrained_S_all 1.051 _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 Mo1 Mo 1.01971(2) 0.31002(2) 0.168661(16) 0.05997(13) Uani 1 1 d . A . Mo2 Mo 0.86701(2) 0.403896(19) 0.191660(13) 0.05019(11) Uani 1 1 d . . . Mo3 Mo 0.93988(2) 0.40063(2) 0.095119(14) 0.05620(12) Uani 1 1 d . . . Mo4 Mo 0.84908(2) 0.240366(19) 0.190461(13) 0.05186(11) Uani 1 1 d . . . Mo5 Mo 0.92113(3) 0.23591(2) 0.093928(14) 0.05708(12) Uani 1 1 d . . . Mo6 Mo 0.76551(2) 0.33087(2) 0.115568(13) 0.05164(11) Uani 1 1 d . . . O1 O 0.89550(14) 0.32008(13) 0.14280(9) 0.0409(6) Uani 1 1 d . . . O2 O 0.8461(2) 0.46316(18) 0.22784(11) 0.0745(10) Uani 1 1 d . . . O3 O 0.9710(2) 0.45938(19) 0.06083(13) 0.0810(11) Uani 1 1 d . . . O4 O 0.8161(2) 0.18191(17) 0.22445(13) 0.0775(11) Uani 1 1 d . . . O5 O 0.9377(3) 0.1768(2) 0.05716(14) 0.0919(13) Uani 1 1 d . . . O6 O 0.6712(2) 0.3382(2) 0.09703(14) 0.0798(11) Uani 1 1 d . . . O7 O 1.03469(18) 0.37750(17) 0.12497(12) 0.0653(9) Uani 1 1 d . . . O8 O 1.01872(18) 0.24352(17) 0.12301(12) 0.0647(9) Uani 1 1 d . . . O9 O 0.96118(19) 0.24516(16) 0.20207(11) 0.0600(8) Uani 1 1 d . . . O10 O 0.97514(19) 0.37951(17) 0.20467(11) 0.0615(8) Uani 1 1 d . . . O11 O 0.8365(2) 0.32231(16) 0.22080(10) 0.0585(8) Uani 1 1 d . . . O12 O 0.76875(16) 0.39540(15) 0.16088(10) 0.0519(7) Uani 1 1 d . . . O13 O 0.90902(18) 0.45221(14) 0.14396(10) 0.0548(7) Uani 1 1 d . . . O14 O 0.82567(19) 0.39436(16) 0.08378(10) 0.0596(8) Uani 1 1 d . . . O15 O 0.9501(2) 0.31846(17) 0.06449(11) 0.0650(9) Uani 1 1 d . . . O16 O 0.75439(17) 0.26494(15) 0.15915(11) 0.0577(8) Uani 1 1 d . . . O17 O 0.87812(18) 0.18764(14) 0.14068(11) 0.0557(8) Uani 1 1 d . . . O18 O 0.8108(2) 0.26259(17) 0.08162(11) 0.0637(9) Uani 1 1 d . . . N1 N 1.1147(3) 0.3031(3) 0.18843(18) 0.0844(15) Uani 1 1 d . . . N2 N 0.5694(3) 0.4869(2) 0.19819(15) 0.0702(12) Uani 1 1 d . . . N3 N 0.8856(3) 0.6644(3) 0.03133(14) 0.0766(13) Uani 1 1 d . . . C11 C 0.4840(3) 0.5133(3) 0.1998(2) 0.0800(16) Uani 1 1 d DU . . H11A H 0.4527 0.4908 0.1782 0.096 Uiso 1 1 calc R . . H11B H 0.4609 0.5016 0.2270 0.096 Uiso 1 1 calc R . . C12 C 0.4755(4) 0.5874(3) 0.1936(3) 0.130(3) Uani 1 1 d DU . . H12A H 0.5065 0.6012 0.1692 0.156 Uiso 1 1 calc R . . H12B H 0.4967 0.6106 0.2181 0.156 Uiso 1 1 calc R . . C13 C 0.3831(5) 0.6075(5) 0.1870(4) 0.200(6) Uani 1 1 d DU . . H13A H 0.3774 0.6416 0.1654 0.240 Uiso 1 1 calc R . . H13B H 0.3509 0.5689 0.1793 0.240 Uiso 1 1 calc R . . C14 C 0.3623(9) 0.6311(10) 0.2256(6) 0.308(10) Uani 1 1 d DU . . H14A H 0.3064 0.6431 0.2256 0.462 Uiso 1 1 calc R . . H14B H 0.3942 0.6698 0.2321 0.462 Uiso 1 1 calc R . . H14C H 0.3717 0.5972 0.2465 0.462 Uiso 1 1 calc R . . C21 C 0.6090(4) 0.5044(3) 0.15620(19) 0.0823(16) Uani 1 1 d DU . . H21A H 0.6161 0.5525 0.1553 0.099 Uiso 1 1 calc R . . H21B H 0.6623 0.4846 0.1561 0.099 Uiso 1 1 calc R . . C22 C 0.5677(4) 0.4839(4) 0.1167(2) 0.102(2) Uani 1 1 d DU . . H22A H 0.5147 0.5041 0.1153 0.123 Uiso 1 1 calc R . . H22B H 0.5613 0.4357 0.1161 0.123 Uiso 1 1 calc R . . C23 C 0.6191(5) 0.5070(4) 0.0785(2) 0.114(3) Uani 1 1 d DU . . H23A H 0.6282 0.5548 0.0805 0.136 Uiso 1 1 calc R . . H23B H 0.6710 0.4849 0.0794 0.136 Uiso 1 1 calc R . . C24 C 0.5812(7) 0.4924(7) 0.0395(3) 0.171(5) Uani 1 1 d DU . . H24A H 0.6145 0.5076 0.0166 0.256 Uiso 1 1 calc R . . H24B H 0.5300 0.5147 0.0382 0.256 Uiso 1 1 calc R . . H24C H 0.5732 0.4450 0.0371 0.256 Uiso 1 1 calc R . . C31 C 0.5735(4) 0.4099(3) 0.20587(19) 0.0783(15) Uani 1 1 d DU . . H31A H 0.6250 0.3942 0.1955 0.094 Uiso 1 1 calc R . . H31B H 0.5729 0.4024 0.2362 0.094 Uiso 1 1 calc R . . C32 C 0.5107(4) 0.3679(3) 0.1871(2) 0.0912(18) Uani 1 1 d DU . . H32A H 0.5078 0.3758 0.1569 0.109 Uiso 1 1 calc R . . H32B H 0.4589 0.3787 0.1994 0.109 Uiso 1 1 calc R . . C33 C 0.5320(5) 0.2937(3) 0.1958(2) 0.103(2) Uani 1 1 d DU . . H33A H 0.5813 0.2826 0.1810 0.123 Uiso 1 1 calc R . . H33B H 0.5417 0.2879 0.2259 0.123 Uiso 1 1 calc R . . C34 C 0.4689(6) 0.2480(4) 0.1827(3) 0.132(3) Uani 1 1 d DU . . H34A H 0.4835 0.2032 0.1904 0.198 Uiso 1 1 calc R . . H34B H 0.4622 0.2507 0.1526 0.198 Uiso 1 1 calc R . . H34C H 0.4194 0.2599 0.1963 0.198 Uiso 1 1 calc R . . C41 C 0.6205(4) 0.5190(3) 0.23193(19) 0.0805(16) Uani 1 1 d DU . . H41A H 0.6723 0.4967 0.2322 0.097 Uiso 1 1 calc R . . H41B H 0.6298 0.5651 0.2239 0.097 Uiso 1 1 calc R . . C42 C 0.5877(4) 0.5183(4) 0.2760(2) 0.0943(19) Uani 1 1 d DU . . H42A H 0.5806 0.4725 0.2853 0.113 Uiso 1 1 calc R . . H42B H 0.5356 0.5402 0.2765 0.113 Uiso 1 1 calc R . . C43 C 0.6451(5) 0.5543(4) 0.3057(2) 0.113(2) Uani 1 1 d DU . . H43A H 0.6970 0.5321 0.3050 0.136 Uiso 1 1 calc R . . H43B H 0.6526 0.5998 0.2959 0.136 Uiso 1 1 calc R . . C44 C 0.6158(6) 0.5554(5) 0.3485(3) 0.138(3) Uani 1 1 d DU . . H44A H 0.6540 0.5779 0.3662 0.207 Uiso 1 1 calc R . . H44B H 0.6086 0.5104 0.3583 0.207 Uiso 1 1 calc R . . H44C H 0.5652 0.5785 0.3494 0.207 Uiso 1 1 calc R . . C51 C 0.9730(3) 0.6850(4) 0.03119(19) 0.0883(18) Uani 1 1 d DU . . H51A H 1.0028 0.6537 0.0486 0.106 Uiso 1 1 calc R . . H51B H 0.9933 0.6809 0.0026 0.106 Uiso 1 1 calc R . . C52 C 0.9907(4) 0.7546(4) 0.0466(2) 0.098(2) Uani 1 1 d DU . . H52A H 0.9681 0.7607 0.0746 0.117 Uiso 1 1 calc R . . H52B H 0.9661 0.7870 0.0278 0.117 Uiso 1 1 calc R . . C53 C 1.0812(4) 0.7659(5) 0.0481(2) 0.121(3) Uani 1 1 d DU . . H53A H 1.1046 0.7367 0.0692 0.145 Uiso 1 1 calc R . . H53B H 1.1043 0.7541 0.0209 0.145 Uiso 1 1 calc R . . C54 C 1.1021(6) 0.8348(6) 0.0579(4) 0.170(4) Uani 1 1 d DU . . H54A H 1.1596 0.8392 0.0592 0.256 Uiso 1 1 calc R . . H54B H 1.0793 0.8468 0.0848 0.256 Uiso 1 1 calc R . . H54C H 1.0812 0.8638 0.0364 0.256 Uiso 1 1 calc R . . C61 C 0.8336(3) 0.7170(3) 0.01010(18) 0.0800(16) Uani 1 1 d DU . . H61A H 0.7777 0.7037 0.0125 0.096 Uiso 1 1 calc R . . H61B H 0.8400 0.7589 0.0252 0.096 Uiso 1 1 calc R . . C62 C 0.8525(4) 0.7287(4) -0.0359(2) 0.102(2) Uani 1 1 d DU . . H62A H 0.8374 0.6896 -0.0521 0.122 Uiso 1 1 calc R . . H62B H 0.9099 0.7356 -0.0392 0.122 Uiso 1 1 calc R . . C63 C 0.8074(5) 0.7895(5) -0.0527(3) 0.149(4) Uani 1 1 d DU . . H63A H 0.8016 0.7850 -0.0830 0.179 Uiso 1 1 calc R . . H63B H 0.7537 0.7899 -0.0405 0.179 Uiso 1 1 calc R . . C64 C 0.8434(9) 0.8482(6) -0.0442(6) 0.249(9) Uani 1 1 d DU . . H64A H 0.8092 0.8842 -0.0531 0.374 Uiso 1 1 calc R . . H64B H 0.8937 0.8506 -0.0590 0.374 Uiso 1 1 calc R . . H64C H 0.8530 0.8517 -0.0143 0.374 Uiso 1 1 calc R . . C71 C 0.8812(4) 0.5971(4) 0.0078(2) 0.098(2) Uani 1 1 d DU . . H71A H 0.8999 0.6042 -0.0209 0.118 Uiso 1 1 calc R . . H71B H 0.9186 0.5665 0.0213 0.118 Uiso 1 1 calc R . . C72 C 0.8004(5) 0.5637(5) 0.0058(4) 0.155(4) Uani 1 1 d DU . . H72A H 0.7588 0.5972 0.0018 0.186 Uiso 1 1 calc R . . H72B H 0.7898 0.5408 0.0322 0.186 Uiso 1 1 calc R . . C73 C 0.7980(7) 0.5118(5) -0.0321(5) 0.204(6) Uani 1 1 d DU . . H73A H 0.7427 0.4976 -0.0361 0.244 Uiso 1 1 calc R . . H73B H 0.8148 0.5346 -0.0577 0.244 Uiso 1 1 calc R . . C74 C 0.8447(8) 0.4563(6) -0.0271(4) 0.201(5) Uani 1 1 d DU . . H74A H 0.8405 0.4287 -0.0518 0.302 Uiso 1 1 calc R . . H74B H 0.8268 0.4317 -0.0028 0.302 Uiso 1 1 calc R . . H74C H 0.8998 0.4695 -0.0232 0.302 Uiso 1 1 calc R . . C81 C 0.8550(4) 0.6607(3) 0.07646(19) 0.093(2) Uani 1 1 d DU . . H81A H 0.8536 0.7055 0.0880 0.112 Uiso 1 1 calc R . . H81B H 0.8001 0.6441 0.0760 0.112 Uiso 1 1 calc R . . C82 C 0.9039(5) 0.6168(4) 0.1058(2) 0.113(3) Uani 1 1 d DU . . H82A H 0.9590 0.6328 0.1065 0.136 Uiso 1 1 calc R . . H82B H 0.9044 0.5715 0.0950 0.136 Uiso 1 1 calc R . . C83 C 0.8687(5) 0.6166(4) 0.1522(2) 0.105(2) Uani 1 1 d DU . . H83A H 0.9040 0.5922 0.1711 0.126 Uiso 1 1 calc R . . H83B H 0.8630 0.6620 0.1626 0.126 Uiso 1 1 calc R . . C84 C 0.7941(4) 0.5857(4) 0.1496(3) 0.108(2) Uani 1 1 d DU . . H84A H 0.7697 0.5846 0.1772 0.163 Uiso 1 1 calc R . . H84B H 0.8007 0.5409 0.1394 0.163 Uiso 1 1 calc R . . H84C H 0.7601 0.6102 0.1306 0.163 Uiso 1 1 calc R . . C1 C 1.1964(4) 0.2997(4) 0.2049(3) 0.116(3) Uani 0.50 1 d PDU A 1 H1A H 1.2017 0.3320 0.2276 0.139 Uiso 0.50 1 calc PR A 1 H1B H 1.2048 0.2557 0.2169 0.139 Uiso 0.50 1 calc PR A 1 C2 C 1.2587(9) 0.3121(11) 0.1744(7) 0.142(6) Uani 0.50 1 d PDU A 1 H2A H 1.2479 0.2891 0.1480 0.170 Uiso 0.50 1 calc PR A 1 H2B H 1.3109 0.2984 0.1850 0.170 Uiso 0.50 1 calc PR A 1 C3 C 1.255(2) 0.3872(13) 0.1688(10) 0.171(11) Uani 0.50 1 d PDU A 1 H3A H 1.2878 0.4002 0.1454 0.256 Uiso 0.50 1 calc PR A 1 H3B H 1.2733 0.4087 0.1941 0.256 Uiso 0.50 1 calc PR A 1 H3C H 1.1999 0.4002 0.1634 0.256 Uiso 0.50 1 calc PR A 1 C1A C 1.1964(4) 0.2997(4) 0.2049(3) 0.116(3) Uani 0.50 1 d PU A 2 H1A1 H 1.2229 0.2600 0.1941 0.139 Uiso 0.50 1 calc PR A 2 H1A2 H 1.1950 0.2969 0.2355 0.139 Uiso 0.50 1 calc PR A 2 C2A C 1.2419(8) 0.3599(9) 0.1919(5) 0.100(4) Uani 0.50 1 d PDU A 2 H2A1 H 1.2960 0.3558 0.2031 0.120 Uiso 0.50 1 calc PR A 2 H2A2 H 1.2173 0.3982 0.2056 0.120 Uiso 0.50 1 calc PR A 2 C3A C 1.2489(15) 0.3757(16) 0.1455(6) 0.140(8) Uani 0.50 1 d PDU A 2 H3A1 H 1.2738 0.4186 0.1420 0.209 Uiso 0.50 1 calc PR A 2 H3A2 H 1.1962 0.3764 0.1330 0.209 Uiso 0.50 1 calc PR A 2 H3A3 H 1.2810 0.3421 0.1319 0.209 Uiso 0.50 1 calc PR 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 Mo1 0.03502(19) 0.0621(3) 0.0828(3) 0.0009(2) -0.01057(18) 0.00341(16) Mo2 0.0518(2) 0.0447(2) 0.0540(2) -0.01107(18) -0.00233(16) 0.00128(15) Mo3 0.0554(2) 0.0505(2) 0.0627(3) 0.00794(19) 0.01290(18) -0.00028(17) Mo4 0.0532(2) 0.0444(2) 0.0579(2) 0.00587(18) 0.00421(16) -0.00065(15) Mo5 0.0618(2) 0.0500(2) 0.0595(3) -0.0120(2) 0.00849(18) 0.00734(17) Mo6 0.03883(19) 0.0533(2) 0.0628(2) -0.00504(19) -0.01124(16) 0.00166(15) O1 0.0327(13) 0.0399(14) 0.0502(16) -0.0020(12) -0.0013(11) 0.0001(10) O2 0.098(3) 0.059(2) 0.067(2) -0.0207(18) 0.0013(19) 0.0085(18) O3 0.088(3) 0.069(2) 0.086(3) 0.023(2) 0.028(2) -0.0023(19) O4 0.088(3) 0.058(2) 0.086(3) 0.0181(19) 0.015(2) -0.0044(18) O5 0.120(4) 0.072(3) 0.084(3) -0.030(2) 0.015(2) 0.019(2) O6 0.0481(19) 0.081(2) 0.110(3) -0.006(2) -0.0299(19) 0.0047(17) O7 0.0398(16) 0.066(2) 0.090(2) 0.0092(19) 0.0061(15) -0.0051(14) O8 0.0459(17) 0.062(2) 0.086(2) -0.0032(18) 0.0112(15) 0.0129(14) O9 0.0526(17) 0.0570(18) 0.070(2) 0.0068(17) -0.0113(15) 0.0061(14) O10 0.0553(18) 0.0601(19) 0.069(2) -0.0101(17) -0.0194(15) -0.0035(14) O11 0.068(2) 0.0565(19) 0.0513(18) -0.0022(15) 0.0089(15) 0.0014(15) O12 0.0395(15) 0.0499(16) 0.0664(19) -0.0065(15) 0.0028(13) 0.0078(12) O13 0.0545(17) 0.0390(15) 0.071(2) 0.0000(15) -0.0003(15) -0.0015(12) O14 0.0600(19) 0.0603(19) 0.0583(18) 0.0057(16) -0.0032(15) 0.0074(15) O15 0.073(2) 0.069(2) 0.0534(18) -0.0007(17) 0.0204(16) 0.0091(16) O16 0.0420(15) 0.0542(18) 0.077(2) 0.0029(16) 0.0018(14) -0.0076(13) O17 0.0571(18) 0.0397(15) 0.070(2) -0.0059(15) 0.0002(15) 0.0011(12) O18 0.066(2) 0.063(2) 0.063(2) -0.0169(17) -0.0156(16) 0.0030(15) N1 0.044(2) 0.083(3) 0.125(4) 0.008(3) -0.017(2) 0.003(2) N2 0.075(3) 0.052(2) 0.083(3) 0.013(2) 0.026(2) 0.002(2) N3 0.072(3) 0.095(3) 0.062(3) 0.006(3) 0.024(2) 0.027(2) C11 0.073(3) 0.068(3) 0.098(4) 0.004(3) 0.027(3) -0.010(3) C12 0.081(4) 0.065(4) 0.245(10) 0.001(5) 0.048(5) 0.006(3) C13 0.108(6) 0.096(6) 0.398(18) 0.061(8) 0.143(8) 0.039(5) C14 0.161(13) 0.30(2) 0.47(2) -0.06(2) 0.121(16) 0.016(13) C21 0.081(4) 0.072(3) 0.095(4) 0.028(3) 0.034(3) 0.015(3) C22 0.107(5) 0.105(5) 0.095(4) 0.031(4) 0.025(4) 0.008(4) C23 0.131(6) 0.117(6) 0.094(4) 0.044(5) 0.032(4) 0.022(5) C24 0.187(10) 0.236(13) 0.090(5) 0.027(7) 0.024(6) -0.016(9) C31 0.093(4) 0.070(3) 0.071(3) 0.013(3) 0.017(3) -0.008(3) C32 0.102(5) 0.081(4) 0.091(4) 0.015(4) 0.010(3) -0.004(3) C33 0.138(6) 0.061(3) 0.110(5) 0.012(4) 0.048(4) 0.003(3) C34 0.195(10) 0.075(4) 0.127(7) -0.013(5) 0.017(6) -0.009(5) C41 0.073(3) 0.065(3) 0.104(4) 0.008(3) 0.019(3) -0.012(3) C42 0.086(4) 0.088(4) 0.108(4) -0.008(4) 0.021(3) -0.025(3) C43 0.115(6) 0.108(6) 0.116(5) 0.002(5) -0.003(4) -0.038(4) C44 0.154(8) 0.147(8) 0.113(5) 0.008(6) -0.012(6) -0.024(6) C51 0.067(3) 0.133(5) 0.065(3) -0.003(4) 0.010(3) 0.037(3) C52 0.071(3) 0.144(6) 0.079(4) -0.009(4) 0.006(3) 0.019(4) C53 0.076(4) 0.199(8) 0.087(5) -0.008(6) -0.013(4) 0.009(5) C54 0.118(8) 0.230(11) 0.164(10) -0.025(9) -0.014(7) -0.039(7) C61 0.053(3) 0.099(4) 0.088(4) 0.010(3) 0.011(3) 0.018(3) C62 0.080(4) 0.139(6) 0.086(4) 0.027(4) -0.001(3) 0.008(4) C63 0.100(6) 0.189(9) 0.159(8) 0.092(8) -0.009(6) 0.005(6) C64 0.187(13) 0.132(7) 0.43(3) 0.029(13) 0.047(14) 0.050(8) C71 0.094(4) 0.107(5) 0.094(5) 0.000(4) 0.028(4) 0.024(4) C72 0.108(6) 0.128(7) 0.231(11) -0.005(7) 0.053(7) -0.010(5) C73 0.128(8) 0.123(8) 0.360(17) -0.079(10) 0.030(10) -0.016(6) C74 0.200(14) 0.175(11) 0.229(14) -0.041(10) -0.014(11) 0.002(9) C81 0.110(5) 0.092(4) 0.078(4) 0.018(3) 0.043(3) 0.035(4) C82 0.129(6) 0.110(6) 0.101(5) 0.029(5) 0.029(4) 0.027(5) C83 0.117(5) 0.084(5) 0.113(5) 0.018(4) 0.014(4) 0.010(4) C84 0.099(5) 0.098(5) 0.128(6) 0.012(5) 0.012(4) 0.031(4) C1 0.046(3) 0.136(6) 0.167(7) 0.020(5) -0.035(4) 0.002(3) C2 0.067(8) 0.191(13) 0.168(14) -0.040(12) -0.002(8) 0.036(10) C3 0.127(18) 0.190(15) 0.19(3) 0.02(2) -0.01(2) -0.047(15) C1A 0.046(3) 0.136(6) 0.167(7) 0.020(5) -0.035(4) 0.002(3) C2A 0.049(6) 0.143(12) 0.108(9) 0.025(9) -0.018(6) -0.014(7) C3A 0.073(10) 0.25(2) 0.100(11) -0.001(13) -0.001(10) -0.029(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 Mo1 N1 1.704(4) . ? Mo1 O9 1.936(3) . ? Mo1 O10 1.944(3) . ? Mo1 O7 1.948(3) . ? Mo1 O8 1.964(4) . ? Mo1 O1 2.229(2) . ? Mo2 O2 1.685(3) . ? Mo2 O10 1.907(3) . ? Mo2 O12 1.909(3) . ? Mo2 O13 1.923(3) . ? Mo2 O11 1.942(3) . ? Mo2 O1 2.329(3) . ? Mo3 O3 1.681(3) . ? Mo3 O7 1.894(3) . ? Mo3 O15 1.916(3) . ? Mo3 O13 1.928(3) . ? Mo3 O14 1.935(3) . ? Mo3 O1 2.328(3) . ? Mo4 O4 1.681(3) . ? Mo4 O9 1.901(3) . ? Mo4 O11 1.912(3) . ? Mo4 O16 1.923(3) . ? Mo4 O17 1.956(3) . ? Mo4 O1 2.327(3) . ? Mo5 O5 1.682(4) . ? Mo5 O8 1.871(3) . ? Mo5 O17 1.906(3) . ? Mo5 O18 1.948(3) . ? Mo5 O15 1.956(3) . ? Mo5 O1 2.326(3) . ? Mo6 O6 1.680(3) . ? Mo6 O18 1.894(3) . ? Mo6 O14 1.904(3) . ? Mo6 O16 1.917(3) . ? Mo6 O12 1.930(3) . ? Mo6 O1 2.335(2) . ? N1 C1 1.455(7) . ? N2 C41 1.508(7) . ? N2 C11 1.514(7) . ? N2 C21 1.524(7) . ? N2 C31 1.561(7) . ? N3 C51 1.510(8) . ? N3 C81 1.518(7) . ? N3 C61 1.518(7) . ? N3 C71 1.540(8) . ? C11 C12 1.502(7) . ? C12 C13 1.600(9) . ? C13 C14 1.356(13) . ? C21 C22 1.485(8) . ? C22 C23 1.550(8) . ? C23 C24 1.416(9) . ? C31 C32 1.465(8) . ? C32 C33 1.551(8) . ? C33 C34 1.452(9) . ? C41 C42 1.497(7) . ? C42 C43 1.518(8) . ? C43 C44 1.440(9) . ? C51 C52 1.504(8) . ? C52 C53 1.521(8) . ? C53 C54 1.455(10) . ? C61 C62 1.506(7) . ? C62 C63 1.523(9) . ? C63 C64 1.346(11) . ? C71 C72 1.501(9) . ? C72 C73 1.586(11) . ? C73 C74 1.364(11) . ? C81 C82 1.514(8) . ? C82 C83 1.579(8) . ? C83 C84 1.388(8) . ? C1 C2 1.437(16) . ? C2 C3 1.51(2) . ? C2A C3A 1.506(19) . ? 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 N1 Mo1 O9 102.2(2) . . ? N1 Mo1 O10 101.3(2) . . ? O9 Mo1 O10 88.17(15) . . ? N1 Mo1 O7 101.4(2) . . ? O9 Mo1 O7 156.37(13) . . ? O10 Mo1 O7 88.21(15) . . ? N1 Mo1 O8 102.9(2) . . ? O9 Mo1 O8 86.75(14) . . ? O10 Mo1 O8 155.83(12) . . ? O7 Mo1 O8 87.06(16) . . ? N1 Mo1 O1 179.47(19) . . ? O9 Mo1 O1 78.22(11) . . ? O10 Mo1 O1 78.33(11) . . ? O7 Mo1 O1 78.18(11) . . ? O8 Mo1 O1 77.50(11) . . ? O2 Mo2 O10 103.19(17) . . ? O2 Mo2 O12 103.45(16) . . ? O10 Mo2 O12 153.30(13) . . ? O2 Mo2 O13 104.74(16) . . ? O10 Mo2 O13 87.48(14) . . ? O12 Mo2 O13 87.42(13) . . ? O2 Mo2 O11 102.42(16) . . ? O10 Mo2 O11 85.90(15) . . ? O12 Mo2 O11 86.78(14) . . ? O13 Mo2 O11 152.84(13) . . ? O2 Mo2 O1 178.70(15) . . ? O10 Mo2 O1 76.55(11) . . ? O12 Mo2 O1 76.77(10) . . ? O13 Mo2 O1 76.55(11) . . ? O11 Mo2 O1 76.29(11) . . ? O3 Mo3 O7 103.69(18) . . ? O3 Mo3 O15 104.26(17) . . ? O7 Mo3 O15 88.21(16) . . ? O3 Mo3 O13 102.99(17) . . ? O7 Mo3 O13 87.27(14) . . ? O15 Mo3 O13 152.68(13) . . ? O3 Mo3 O14 103.15(18) . . ? O7 Mo3 O14 153.14(14) . . ? O15 Mo3 O14 86.43(15) . . ? O13 Mo3 O14 85.55(13) . . ? O3 Mo3 O1 179.33(15) . . ? O7 Mo3 O1 76.77(12) . . ? O15 Mo3 O1 76.22(12) . . ? O13 Mo3 O1 76.52(11) . . ? O14 Mo3 O1 76.39(11) . . ? O4 Mo4 O9 103.36(18) . . ? O4 Mo4 O11 103.88(17) . . ? O9 Mo4 O11 88.10(15) . . ? O4 Mo4 O16 103.93(17) . . ? O9 Mo4 O16 152.66(14) . . ? O11 Mo4 O16 87.13(14) . . ? O4 Mo4 O17 102.73(17) . . ? O9 Mo4 O17 86.62(14) . . ? O11 Mo4 O17 153.38(13) . . ? O16 Mo4 O17 85.69(14) . . ? O4 Mo4 O1 179.18(16) . . ? O9 Mo4 O1 76.45(12) . . ? O11 Mo4 O1 76.92(12) . . ? O16 Mo4 O1 76.24(11) . . ? O17 Mo4 O1 76.47(11) . . ? O5 Mo5 O8 104.8(2) . . ? O5 Mo5 O17 104.00(18) . . ? O8 Mo5 O17 89.12(15) . . ? O5 Mo5 O18 102.05(19) . . ? O8 Mo5 O18 153.06(14) . . ? O17 Mo5 O18 86.63(14) . . ? O5 Mo5 O15 102.95(19) . . ? O8 Mo5 O15 87.26(16) . . ? O17 Mo5 O15 152.83(13) . . ? O18 Mo5 O15 84.55(15) . . ? O5 Mo5 O1 177.77(18) . . ? O8 Mo5 O1 76.87(12) . . ? O17 Mo5 O1 77.42(11) . . ? O18 Mo5 O1 76.24(11) . . ? O15 Mo5 O1 75.53(12) . . ? O6 Mo6 O18 103.64(17) . . ? O6 Mo6 O14 104.32(18) . . ? O18 Mo6 O14 88.45(15) . . ? O6 Mo6 O16 102.78(18) . . ? O18 Mo6 O16 87.13(15) . . ? O14 Mo6 O16 152.83(13) . . ? O6 Mo6 O12 103.12(16) . . ? O18 Mo6 O12 153.21(13) . . ? O14 Mo6 O12 86.07(14) . . ? O16 Mo6 O12 85.91(14) . . ? O6 Mo6 O1 178.74(17) . . ? O18 Mo6 O1 76.98(12) . . ? O14 Mo6 O1 76.76(11) . . ? O16 Mo6 O1 76.13(11) . . ? O12 Mo6 O1 76.23(10) . . ? Mo1 O1 Mo5 90.52(9) . . ? Mo1 O1 Mo4 90.41(9) . . ? Mo5 O1 Mo4 89.73(9) . . ? Mo1 O1 Mo3 90.41(9) . . ? Mo5 O1 Mo3 90.71(10) . . ? Mo4 O1 Mo3 179.07(12) . . ? Mo1 O1 Mo2 90.55(9) . . ? Mo5 O1 Mo2 178.82(12) . . ? Mo4 O1 Mo2 89.78(10) . . ? Mo3 O1 Mo2 89.77(9) . . ? Mo1 O1 Mo6 179.82(16) . . ? Mo5 O1 Mo6 89.48(9) . . ? Mo4 O1 Mo6 89.76(9) . . ? Mo3 O1 Mo6 89.42(9) . . ? Mo2 O1 Mo6 89.45(9) . . ? Mo3 O7 Mo1 114.64(15) . . ? Mo5 O8 Mo1 115.10(15) . . ? Mo4 O9 Mo1 114.87(16) . . ? Mo2 O10 Mo1 114.55(15) . . ? Mo4 O11 Mo2 116.99(16) . . ? Mo2 O12 Mo6 117.54(14) . . ? Mo2 O13 Mo3 117.16(14) . . ? Mo6 O14 Mo3 117.40(16) . . ? Mo3 O15 Mo5 117.51(16) . . ? Mo6 O16 Mo4 117.87(15) . . ? Mo5 O17 Mo4 116.37(14) . . ? Mo6 O18 Mo5 117.29(16) . . ? C1 N1 Mo1 177.9(5) . . ? C41 N2 C11 110.8(4) . . ? C41 N2 C21 106.0(4) . . ? C11 N2 C21 110.7(4) . . ? C41 N2 C31 106.6(4) . . ? C11 N2 C31 112.4(4) . . ? C21 N2 C31 110.1(4) . . ? C51 N3 C81 109.8(5) . . ? C51 N3 C61 110.9(5) . . ? C81 N3 C61 105.1(4) . . ? C51 N3 C71 106.4(4) . . ? C81 N3 C71 113.3(5) . . ? C61 N3 C71 111.4(5) . . ? C12 C11 N2 115.4(5) . . ? C11 C12 C13 110.8(6) . . ? C14 C13 C12 102.3(11) . . ? C22 C21 N2 118.1(5) . . ? C21 C22 C23 108.6(6) . . ? C24 C23 C22 111.9(7) . . ? C32 C31 N2 118.1(5) . . ? C31 C32 C33 108.3(6) . . ? C34 C33 C32 112.8(7) . . ? C42 C41 N2 116.8(5) . . ? C41 C42 C43 110.1(5) . . ? C44 C43 C42 112.1(6) . . ? C52 C51 N3 116.1(5) . . ? C51 C52 C53 109.9(6) . . ? C54 C53 C52 112.5(7) . . ? C62 C61 N3 114.7(5) . . ? C61 C62 C63 111.0(6) . . ? C64 C63 C62 114.1(9) . . ? C72 C71 N3 116.9(6) . . ? C71 C72 C73 110.3(7) . . ? C74 C73 C72 115.6(12) . . ? C82 C81 N3 115.2(5) . . ? C81 C82 C83 111.8(6) . . ? C84 C83 C82 106.1(7) . . ? C2 C1 N1 115.1(10) . . ? C1 C2 C3 102.5(17) . . ? _diffrn_measured_fraction_theta_max 0.984 _diffrn_reflns_theta_full 26.00 _diffrn_measured_fraction_theta_full 0.984 _refine_diff_density_max 1.168 _refine_diff_density_min -0.971 _refine_diff_density_rms 0.083 #===END data_compound-4 _database_code_depnum_ccdc_archive 'CCDC 688715' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C35 H79 Mo6 N3 O18' _chemical_formula_weight 1405.65 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' Mo Mo -1.6832 0.6857 '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 12.470(3) _cell_length_b 19.020(4) _cell_length_c 23.237(5) _cell_angle_alpha 93.59(3) _cell_angle_beta 102.64(3) _cell_angle_gamma 91.85(3) _cell_volume 5361.4(19) _cell_formula_units_Z 4 _cell_measurement_temperature 296(2) _cell_measurement_reflns_used 7079 _cell_measurement_theta_min 2.40 _cell_measurement_theta_max 29.48 _exptl_crystal_description block _exptl_crystal_colour orange _exptl_crystal_size_max 0.46 _exptl_crystal_size_mid 0.22 _exptl_crystal_size_min 0.17 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.741 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 2824 _exptl_absorpt_coefficient_mu 1.425 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.5602 _exptl_absorpt_correction_T_max 0.7937 _exptl_absorpt_process_details ? _exptl_special_details ; ? ; _diffrn_ambient_temperature 296(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 'CCD area detector' _diffrn_measurement_method 'phi and omega scans' _diffrn_detector_area_resol_mean ? _diffrn_reflns_number 30104 _diffrn_reflns_av_R_equivalents 0.0257 _diffrn_reflns_av_sigmaI/netI 0.0438 _diffrn_reflns_limit_h_min -14 _diffrn_reflns_limit_h_max 14 _diffrn_reflns_limit_k_min -17 _diffrn_reflns_limit_k_max 22 _diffrn_reflns_limit_l_min -27 _diffrn_reflns_limit_l_max 21 _diffrn_reflns_theta_min 2.27 _diffrn_reflns_theta_max 25.00 _reflns_number_total 18653 _reflns_number_gt 13688 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'Bruker SMART' _computing_cell_refinement 'Bruker SMART' _computing_data_reduction 'Bruker SAINT' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _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^)+(0.0510P)^2^+18.9364P] 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 18653 _refine_ls_number_parameters 1034 _refine_ls_number_restraints 71 _refine_ls_R_factor_all 0.0760 _refine_ls_R_factor_gt 0.0581 _refine_ls_wR_factor_ref 0.1551 _refine_ls_wR_factor_gt 0.1440 _refine_ls_goodness_of_fit_ref 1.087 _refine_ls_restrained_S_all 1.089 _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 Mo1 Mo 0.69706(6) -0.31511(4) 0.34443(3) 0.06723(19) Uani 1 1 d . . . Mo2 Mo 0.80412(6) -0.15598(4) 0.37625(3) 0.06808(19) Uani 1 1 d . . . Mo3 Mo 0.53634(5) -0.18650(4) 0.35121(3) 0.06242(18) Uani 1 1 d . . . Mo4 Mo 0.83849(6) -0.27212(4) 0.47704(3) 0.0720(2) Uani 1 1 d . . . Mo5 Mo 0.57012(5) -0.30147(3) 0.45235(3) 0.05816(17) Uani 1 1 d . . . Mo6 Mo 0.67781(6) -0.14105(4) 0.48614(3) 0.06524(19) Uani 1 1 d . . . Mo7 Mo 0.59756(7) 0.36410(5) 0.05355(3) 0.0827(2) Uani 1 1 d . . . Mo8 Mo 0.65540(5) 0.20018(4) 0.06250(3) 0.06661(19) Uani 1 1 d . . . Mo9 Mo 0.50397(5) 0.18863(4) 0.16108(3) 0.06547(19) Uani 1 1 d . . . Mo10 Mo 0.44586(5) 0.35529(4) 0.15013(3) 0.06694(19) Uani 1 1 d . . . Mo11 Mo 0.70348(5) 0.31078(4) 0.18181(3) 0.06524(19) Uani 1 1 d . . . Mo12 Mo 0.39800(5) 0.24563(5) 0.03130(3) 0.0794(2) Uani 1 1 d . . . O1 O 0.6871(3) -0.2301(2) 0.41335(19) 0.0531(11) Uani 1 1 d . . . O2 O 0.8890(5) -0.1018(4) 0.3500(3) 0.097(2) Uani 1 1 d . . . O3 O 0.4288(5) -0.1550(4) 0.3054(3) 0.0888(18) Uani 1 1 d . . . O4 O 0.9478(5) -0.3005(4) 0.5236(3) 0.105(2) Uani 1 1 d . . . O5 O 0.4852(5) -0.3555(3) 0.4790(2) 0.0771(15) Uani 1 1 d . . . O6 O 0.6719(6) -0.0766(3) 0.5379(3) 0.0943(19) Uani 1 1 d . . . O7 O 0.4705(4) -0.2543(3) 0.3931(2) 0.0639(13) Uani 1 1 d . . . O8 O 0.5818(4) -0.2164(3) 0.5017(2) 0.0627(12) Uani 1 1 d . . . O9 O 0.7131(4) -0.3204(3) 0.4971(2) 0.0660(13) Uani 1 1 d . . . O10 O 0.6000(4) -0.3593(3) 0.3886(2) 0.0672(13) Uani 1 1 d . . . O11 O 0.6602(4) -0.1357(3) 0.3328(2) 0.0649(13) Uani 1 1 d . . . O12 O 0.5573(4) -0.1239(3) 0.4210(2) 0.0689(14) Uani 1 1 d . . . O13 O 0.5731(4) -0.2645(3) 0.3050(2) 0.0656(13) Uani 1 1 d . . . O14 O 0.7983(4) -0.1921(3) 0.5226(2) 0.0715(14) Uani 1 1 d . . . O15 O 0.7716(5) -0.0992(3) 0.4414(2) 0.0722(14) Uani 1 1 d . . . O16 O 0.9029(4) -0.2027(3) 0.4360(2) 0.0759(15) Uani 1 1 d . . . O17 O 0.7928(4) -0.2395(3) 0.3272(2) 0.0724(14) Uani 1 1 d . . . O18 O 0.8193(4) -0.3344(3) 0.4097(2) 0.0757(15) Uani 1 1 d . . . O19 O 0.5511(3) 0.2792(3) 0.10560(18) 0.0568(12) Uani 1 1 d . . . O20 O 0.7302(4) 0.1431(3) 0.0306(3) 0.0863(18) Uani 1 1 d . . . O21 O 0.4697(5) 0.1232(3) 0.2000(3) 0.0922(18) Uani 1 1 d . . . O22 O 0.3696(5) 0.4094(4) 0.1835(2) 0.0877(18) Uani 1 1 d . . . O23 O 0.8163(5) 0.3310(4) 0.2356(3) 0.0909(18) Uani 1 1 d . . . O24 O 0.2856(5) 0.2209(4) -0.0217(3) 0.109(3) Uani 1 1 d . . . O25 O 0.7156(4) 0.3742(3) 0.1238(3) 0.0814(16) Uani 1 1 d . . . O26 O 0.6729(5) 0.2848(3) 0.0261(2) 0.0831(17) Uani 1 1 d . . . O27 O 0.5046(5) 0.4121(3) 0.1002(2) 0.0791(16) Uani 1 1 d . . . O28 O 0.4618(5) 0.3230(4) 0.0019(2) 0.0893(19) Uani 1 1 d . . . O29 O 0.5083(4) 0.1885(3) 0.0107(2) 0.0756(16) Uani 1 1 d . . . O30 O 0.5946(4) 0.1431(3) 0.1149(2) 0.0696(14) Uani 1 1 d . . . O31 O 0.3421(4) 0.3149(3) 0.0825(2) 0.0745(15) Uani 1 1 d . . . O32 O 0.7573(4) 0.2392(3) 0.1308(2) 0.0682(14) Uani 1 1 d . . . O33 O 0.6368(4) 0.2307(3) 0.2094(2) 0.0649(13) Uani 1 1 d . . . O34 O 0.4311(4) 0.2692(3) 0.1867(2) 0.0651(13) Uani 1 1 d . . . O35 O 0.3886(4) 0.1817(3) 0.0914(2) 0.0727(15) Uani 1 1 d . . . O36 O 0.5918(4) 0.3657(3) 0.2037(2) 0.0686(14) Uani 1 1 d . . . N1 N 0.7037(7) -0.3818(4) 0.2924(3) 0.093(2) Uani 1 1 d U . . N2 N 0.6303(8) 0.4300(5) 0.0140(4) 0.120(3) Uani 1 1 d U . . N3 N 0.4456(5) 0.4417(3) 0.3626(2) 0.0610(15) Uani 1 1 d . . . N4 N 0.9342(7) -0.2245(7) 0.8756(4) 0.1246(18) Uani 1 1 d . . . N5 N 0.6109(8) -0.0927(5) 0.1610(4) 0.1179(17) Uani 1 1 d . . . N6 N 0.7685(6) 0.1343(4) 0.5276(4) 0.091(2) Uani 1 1 d . . . C1 C 0.7069(7) -0.4444(5) 0.2506(4) 0.093 Uani 1 1 d DU . . H1 H 0.6672 -0.4831 0.2642 0.111 Uiso 1 1 calc R . . C2 C 0.8190(7) -0.4651(5) 0.2575(4) 0.093 Uani 1 1 d DU . . H2A H 0.8454 -0.4792 0.2969 0.139 Uiso 1 1 calc R . . H2B H 0.8643 -0.4261 0.2508 0.139 Uiso 1 1 calc R . . H2C H 0.8221 -0.5039 0.2295 0.139 Uiso 1 1 calc R . . C3 C 0.6414(8) -0.4299(5) 0.1932(4) 0.093 Uani 1 1 d DU . . H3A H 0.5674 -0.4216 0.1964 0.139 Uiso 1 1 calc R . . H3B H 0.6412 -0.4695 0.1655 0.139 Uiso 1 1 calc R . . H3C H 0.6724 -0.3888 0.1797 0.139 Uiso 1 1 calc R . . C4 C 0.6620(10) 0.4895(6) -0.0189(5) 0.134 Uani 1 1 d DU . . H4 H 0.5931 0.5077 -0.0404 0.161 Uiso 1 1 calc R . . C5 C 0.7121(10) 0.5447(6) 0.0270(5) 0.134 Uani 1 1 d DU . . H5A H 0.6643 0.5527 0.0538 0.201 Uiso 1 1 calc R . . H5B H 0.7230 0.5876 0.0089 0.201 Uiso 1 1 calc R . . H5C H 0.7817 0.5301 0.0483 0.201 Uiso 1 1 calc R . . C6 C 0.7198(10) 0.4640(6) -0.0630(5) 0.134 Uani 1 1 d DU . . H6A H 0.6686 0.4392 -0.0954 0.201 Uiso 1 1 calc R . . H6B H 0.7748 0.4326 -0.0458 0.201 Uiso 1 1 calc R . . H6C H 0.7545 0.5031 -0.0772 0.201 Uiso 1 1 calc R . . C7 C 0.9827(8) 0.0635(7) 0.4427(5) 0.110(4) Uani 1 1 d . . . H7A H 1.0447 0.0721 0.4761 0.132 Uiso 1 1 calc R . . H7B H 0.9605 0.0139 0.4406 0.132 Uiso 1 1 calc R . . C8 C 1.0202(9) 0.0777(7) 0.3885(5) 0.124(4) Uani 1 1 d . . . H8A H 1.0781 0.0471 0.3842 0.186 Uiso 1 1 calc R . . H8B H 1.0471 0.1259 0.3910 0.186 Uiso 1 1 calc R . . H8C H 0.9598 0.0694 0.3549 0.186 Uiso 1 1 calc R . . C9 C 0.8256(12) 0.2057(7) 0.5385(7) 0.152(5) Uani 1 1 d D . . H9A H 0.8405 0.2201 0.5016 0.182 Uiso 1 1 calc R . . H9B H 0.8958 0.2026 0.5660 0.182 Uiso 1 1 calc R . . C10 C 0.7623(12) 0.2614(8) 0.5627(8) 0.164(6) Uani 1 1 d D . . H10A H 0.7577 0.2514 0.6026 0.197 Uiso 1 1 calc R . . H10B H 0.6880 0.2600 0.5387 0.197 Uiso 1 1 calc R . . C11 C 0.8155(13) 0.3353(7) 0.5639(8) 0.163(7) Uani 1 1 d D . . H11A H 0.8375 0.3411 0.5269 0.195 Uiso 1 1 calc R . . H11B H 0.7625 0.3704 0.5682 0.195 Uiso 1 1 calc R . . C12 C 0.9150(14) 0.3465(10) 0.6146(8) 0.223(10) Uani 1 1 d D . . H12A H 0.9480 0.3927 0.6144 0.334 Uiso 1 1 calc R . . H12B H 0.9674 0.3117 0.6103 0.334 Uiso 1 1 calc R . . H12C H 0.8929 0.3420 0.6513 0.334 Uiso 1 1 calc R . . C13 C 0.4247(7) 0.4936(4) 0.3139(3) 0.069(2) Uani 1 1 d . . . H13A H 0.4955 0.5102 0.3079 0.082 Uiso 1 1 calc R . . H13B H 0.3864 0.4677 0.2776 0.082 Uiso 1 1 calc R . . C14 C 0.3601(7) 0.5572(4) 0.3235(4) 0.072(2) Uani 1 1 d . . . H14A H 0.3965 0.5841 0.3598 0.087 Uiso 1 1 calc R . . H14B H 0.2871 0.5421 0.3273 0.087 Uiso 1 1 calc R . . C15 C 0.3513(7) 0.6032(5) 0.2715(4) 0.081(2) Uani 1 1 d . . . H15A H 0.4236 0.6239 0.2720 0.097 Uiso 1 1 calc R . . H15B H 0.3279 0.5736 0.2350 0.097 Uiso 1 1 calc R . . C16 C 0.2750(9) 0.6596(6) 0.2716(6) 0.119(4) Uani 1 1 d . . . H16A H 0.2723 0.6856 0.2373 0.179 Uiso 1 1 calc R . . H16B H 0.2994 0.6905 0.3066 0.179 Uiso 1 1 calc R . . H16C H 0.2030 0.6396 0.2710 0.179 Uiso 1 1 calc R . . C17 C 0.3441(6) 0.4278(5) 0.3868(4) 0.073(2) Uani 1 1 d . . . H17A H 0.3628 0.3961 0.4183 0.088 Uiso 1 1 calc R . . H17B H 0.3251 0.4720 0.4044 0.088 Uiso 1 1 calc R . . C18 C 0.2445(8) 0.3970(6) 0.3435(4) 0.092(3) Uani 1 1 d . . . H18A H 0.2560 0.3485 0.3316 0.111 Uiso 1 1 calc R . . H18B H 0.2308 0.4236 0.3085 0.111 Uiso 1 1 calc R . . C19 C 0.1451(8) 0.3999(8) 0.3732(5) 0.128(5) Uani 1 1 d D . . H19A H 0.1638 0.3775 0.4102 0.153 Uiso 1 1 calc R . . H19B H 0.1324 0.4490 0.3825 0.153 Uiso 1 1 calc R . . C20 C 0.0404(10) 0.3655(10) 0.3369(6) 0.187(8) Uani 1 1 d D . . H20A H -0.0160 0.3683 0.3591 0.281 Uiso 1 1 calc R . . H20B H 0.0518 0.3169 0.3272 0.281 Uiso 1 1 calc R . . H20C H 0.0184 0.3891 0.3012 0.281 Uiso 1 1 calc R . . C21 C 0.4800(7) 0.3750(4) 0.3354(3) 0.071(2) Uani 1 1 d . . . H21A H 0.5442 0.3861 0.3199 0.085 Uiso 1 1 calc R . . H21B H 0.4214 0.3579 0.3023 0.085 Uiso 1 1 calc R . . C22 C 0.5067(8) 0.3166(4) 0.3762(4) 0.081(2) Uani 1 1 d . . . H22A H 0.4392 0.2963 0.3838 0.097 Uiso 1 1 calc R . . H22B H 0.5523 0.3356 0.4136 0.097 Uiso 1 1 calc R . . C23 C 0.5670(10) 0.2595(5) 0.3493(4) 0.100(3) Uani 1 1 d . . . H23A H 0.5581 0.2161 0.3680 0.120 Uiso 1 1 calc R . . H23B H 0.5321 0.2512 0.3077 0.120 Uiso 1 1 calc R . . C24 C 0.6874(10) 0.2752(6) 0.3547(4) 0.108(4) Uani 1 1 d . . . H24A H 0.7185 0.2363 0.3368 0.162 Uiso 1 1 calc R . . H24B H 0.7235 0.2824 0.3957 0.162 Uiso 1 1 calc R . . H24C H 0.6975 0.3170 0.3350 0.162 Uiso 1 1 calc R . . C25 C 0.5334(6) 0.4728(4) 0.4148(3) 0.0653(19) Uani 1 1 d . . . H25A H 0.5314 0.4453 0.4484 0.078 Uiso 1 1 calc R . . H25B H 0.5141 0.5203 0.4249 0.078 Uiso 1 1 calc R . . C26 C 0.6513(7) 0.4763(4) 0.4064(4) 0.072(2) Uani 1 1 d . . . H26A H 0.6698 0.4301 0.3923 0.086 Uiso 1 1 calc R . . H26B H 0.6575 0.5091 0.3769 0.086 Uiso 1 1 calc R . . C27 C 0.7299(8) 0.4993(5) 0.4627(5) 0.092(3) Uani 1 1 d . . . H27A H 0.7205 0.4679 0.4928 0.111 Uiso 1 1 calc R . . H27B H 0.7134 0.5463 0.4757 0.111 Uiso 1 1 calc R . . C28 C 0.8498(8) 0.4996(7) 0.4566(6) 0.125(4) Uani 1 1 d . . . H28A H 0.8977 0.5127 0.4943 0.188 Uiso 1 1 calc R . . H28B H 0.8608 0.5328 0.4288 0.188 Uiso 1 1 calc R . . H28C H 0.8662 0.4533 0.4429 0.188 Uiso 1 1 calc R . . C29 C 0.9876(7) -0.2889(5) 0.8546(4) 0.082(3) Uani 1 1 d . . . H29A H 1.0068 -0.2797 0.8174 0.099 Uiso 1 1 calc R . . H29B H 1.0556 -0.2951 0.8830 0.099 Uiso 1 1 calc R . . C30 C 0.9209(8) -0.3551(6) 0.8461(5) 0.104(3) Uani 1 1 d . . . H30A H 0.8587 -0.3521 0.8131 0.125 Uiso 1 1 calc R . . H30B H 0.8925 -0.3613 0.8811 0.125 Uiso 1 1 calc R . . C31 C 0.9830(10) -0.4176(7) 0.8344(6) 0.118(4) Uani 1 1 d . . . H31A H 1.0448 -0.4204 0.8677 0.141 Uiso 1 1 calc R . . H31B H 1.0128 -0.4103 0.7999 0.141 Uiso 1 1 calc R . . C32 C 0.9186(12) -0.4880(7) 0.8242(7) 0.156(6) Uani 1 1 d . . . H32A H 0.9650 -0.5245 0.8151 0.234 Uiso 1 1 calc R . . H32B H 0.8563 -0.4861 0.7917 0.234 Uiso 1 1 calc R . . H32C H 0.8936 -0.4980 0.8592 0.234 Uiso 1 1 calc R . . C33 C 1.0135(6) -0.1601(5) 0.8791(4) 0.079(2) Uani 1 1 d . . . H33A H 1.0811 -0.1681 0.9072 0.095 Uiso 1 1 calc R . . H33B H 1.0315 -0.1571 0.8407 0.095 Uiso 1 1 calc R . . C34 C 0.9732(7) -0.0902(5) 0.8965(4) 0.089(3) Uani 1 1 d . . . H34A H 0.9064 -0.0809 0.8683 0.107 Uiso 1 1 calc R . . H34B H 0.9554 -0.0922 0.9350 0.107 Uiso 1 1 calc R . . C35 C 1.0552(8) -0.0323(6) 0.8989(5) 0.103(3) Uani 1 1 d . . . H35A H 1.0722 -0.0305 0.8603 0.123 Uiso 1 1 calc R . . H35B H 1.1222 -0.0425 0.9266 0.123 Uiso 1 1 calc R . . C36 C 1.0195(10) 0.0382(6) 0.9169(5) 0.117(4) Uani 1 1 d . . . H36A H 1.0762 0.0734 0.9166 0.175 Uiso 1 1 calc R . . H36B H 1.0061 0.0377 0.9561 0.175 Uiso 1 1 calc R . . H36C H 0.9532 0.0489 0.8898 0.175 Uiso 1 1 calc R . . C37 C 0.9085(9) -0.2333(8) 0.9368(5) 0.1246(18) Uani 1 1 d U . . H37A H 0.8717 -0.1921 0.9479 0.150 Uiso 1 1 calc R . . H37B H 0.8581 -0.2739 0.9339 0.150 Uiso 1 1 calc R . . C38 C 1.0088(9) -0.2427(8) 0.9849(5) 0.1246(18) Uani 1 1 d U . . H38A H 1.0518 -0.2795 0.9718 0.150 Uiso 1 1 calc R . . H38B H 1.0541 -0.1993 0.9925 0.150 Uiso 1 1 calc R . . C39 C 0.9787(8) -0.2610(8) 1.0389(4) 0.1246(18) Uani 1 1 d DU . . H39A H 0.9187 -0.2965 1.0287 0.150 Uiso 1 1 calc R . . H39B H 0.9507 -0.2195 1.0560 0.150 Uiso 1 1 calc R . . C40 C 1.0674(8) -0.2882(7) 1.0855(4) 0.1246(18) Uani 1 1 d DU . . H40A H 1.0440 -0.2875 1.1222 0.187 Uiso 1 1 calc R . . H40B H 1.1332 -0.2588 1.0903 0.187 Uiso 1 1 calc R . . H40C H 1.0817 -0.3356 1.0737 0.187 Uiso 1 1 calc R . . C41 C 0.8257(6) -0.2130(5) 0.8329(4) 0.081(2) Uani 1 1 d . . . H41A H 0.7919 -0.1729 0.8484 0.097 Uiso 1 1 calc R . . H41B H 0.7767 -0.2541 0.8310 0.097 Uiso 1 1 calc R . . C42 C 0.8381(7) -0.1999(6) 0.7706(4) 0.095(3) Uani 1 1 d . . . H42A H 0.8868 -0.1587 0.7724 0.114 Uiso 1 1 calc R . . H42B H 0.8719 -0.2400 0.7551 0.114 Uiso 1 1 calc R . . C43 C 0.7329(9) -0.1891(7) 0.7302(5) 0.111(4) Uani 1 1 d . . . H43A H 0.6982 -0.1499 0.7462 0.133 Uiso 1 1 calc R . . H43B H 0.6849 -0.2309 0.7277 0.133 Uiso 1 1 calc R . . C44 C 0.7451(10) -0.1743(7) 0.6682(5) 0.121(4) Uani 1 1 d . . . H44A H 0.6737 -0.1697 0.6433 0.181 Uiso 1 1 calc R . . H44B H 0.7808 -0.2125 0.6523 0.181 Uiso 1 1 calc R . . H44C H 0.7885 -0.1312 0.6700 0.181 Uiso 1 1 calc R . . C45 C 0.6442(7) -0.0368(5) 0.2120(3) 0.073(2) Uani 1 1 d . . . H45A H 0.6709 -0.0601 0.2480 0.087 Uiso 1 1 calc R . . H45B H 0.5791 -0.0124 0.2167 0.087 Uiso 1 1 calc R . . C46 C 0.7319(7) 0.0178(5) 0.2056(4) 0.078(2) Uani 1 1 d . . . H46A H 0.7985 -0.0057 0.2026 0.094 Uiso 1 1 calc R . . H46B H 0.7067 0.0409 0.1693 0.094 Uiso 1 1 calc R . . C47 C 0.7578(7) 0.0728(5) 0.2570(4) 0.082(2) Uani 1 1 d . . . H47A H 0.6914 0.0968 0.2596 0.098 Uiso 1 1 calc R . . H47B H 0.7819 0.0496 0.2933 0.098 Uiso 1 1 calc R . . C48 C 0.8453(8) 0.1262(5) 0.2513(4) 0.090(3) Uani 1 1 d . . . H48A H 0.8592 0.1598 0.2850 0.135 Uiso 1 1 calc R . . H48B H 0.8211 0.1502 0.2159 0.135 Uiso 1 1 calc R . . H48C H 0.9116 0.1029 0.2494 0.135 Uiso 1 1 calc R . . C49 C 0.5530(7) -0.0607(5) 0.1050(3) 0.076(2) Uani 1 1 d . . . H49A H 0.5996 -0.0219 0.0978 0.092 Uiso 1 1 calc R . . H49B H 0.5461 -0.0960 0.0722 0.092 Uiso 1 1 calc R . . C50 C 0.4407(7) -0.0338(6) 0.1047(4) 0.090(3) Uani 1 1 d . . . H50A H 0.4448 -0.0020 0.1395 0.108 Uiso 1 1 calc R . . H50B H 0.3904 -0.0732 0.1066 0.108 Uiso 1 1 calc R . . C51 C 0.3962(7) 0.0046(6) 0.0499(4) 0.095(3) Uani 1 1 d . . . H51A H 0.4434 0.0462 0.0499 0.113 Uiso 1 1 calc R . . H51B H 0.3986 -0.0259 0.0152 0.113 Uiso 1 1 calc R . . C52 C 0.2815(8) 0.0264(7) 0.0459(6) 0.129(4) Uani 1 1 d . . . H52A H 0.2566 0.0487 0.0097 0.193 Uiso 1 1 calc R . . H52B H 0.2792 0.0588 0.0789 0.193 Uiso 1 1 calc R . . H52C H 0.2344 -0.0145 0.0464 0.193 Uiso 1 1 calc R . . C53 C 0.7124(8) -0.1274(5) 0.1472(4) 0.085(3) Uani 1 1 d . . . H53A H 0.6880 -0.1635 0.1152 0.102 Uiso 1 1 calc R . . H53B H 0.7564 -0.0921 0.1332 0.102 Uiso 1 1 calc R . . C54 C 0.7846(9) -0.1605(6) 0.1980(4) 0.105(3) Uani 1 1 d . . . H54A H 0.8143 -0.1246 0.2294 0.126 Uiso 1 1 calc R . . H54B H 0.7415 -0.1950 0.2135 0.126 Uiso 1 1 calc R . . C55 C 0.8764(12) -0.1955(8) 0.1774(5) 0.144(5) Uani 1 1 d . . . H55A H 0.9188 -0.1603 0.1621 0.173 Uiso 1 1 calc R . . H55B H 0.8455 -0.2302 0.1452 0.173 Uiso 1 1 calc R . . C56 C 0.9548(13) -0.2324(10) 0.2265(7) 0.195(9) Uani 1 1 d . . . H56A H 1.0164 -0.2488 0.2118 0.292 Uiso 1 1 calc R . . H56B H 0.9160 -0.2717 0.2379 0.292 Uiso 1 1 calc R . . H56C H 0.9805 -0.1995 0.2601 0.292 Uiso 1 1 calc R . . C57 C 0.5357(10) -0.1461(6) 0.1805(4) 0.1179(17) Uani 1 1 d D . . H57A H 0.5746 -0.1637 0.2173 0.142 Uiso 1 1 calc R . . H57B H 0.4723 -0.1224 0.1885 0.142 Uiso 1 1 calc R . . C58 C 0.4963(10) -0.2076(6) 0.1366(4) 0.1179(17) Uani 1 1 d D . . H58A H 0.5595 -0.2317 0.1288 0.142 Uiso 1 1 calc R . . H58B H 0.4573 -0.1903 0.0998 0.142 Uiso 1 1 calc R . . C59 C 0.4216(9) -0.2595(6) 0.1573(5) 0.1179(17) Uani 1 1 d D . . H59A H 0.4483 -0.2681 0.1986 0.142 Uiso 1 1 calc R . . H59B H 0.4118 -0.3039 0.1335 0.142 Uiso 1 1 calc R . . C60 C 0.3164(9) -0.2191(6) 0.1477(4) 0.1179(17) Uani 1 1 d D . . H60A H 0.2616 -0.2444 0.1626 0.177 Uiso 1 1 calc R . . H60B H 0.2900 -0.2141 0.1062 0.177 Uiso 1 1 calc R . . H60C H 0.3313 -0.1732 0.1683 0.177 Uiso 1 1 calc R . . C61 C 0.7342(10) 0.1039(7) 0.5787(6) 0.121(4) Uani 1 1 d . . . H61A H 0.6704 0.1285 0.5852 0.145 Uiso 1 1 calc R . . H61B H 0.7099 0.0551 0.5668 0.145 Uiso 1 1 calc R . . C62 C 0.8116(11) 0.1048(8) 0.6350(5) 0.126(4) Uani 1 1 d . . . H62A H 0.8180 0.1523 0.6537 0.152 Uiso 1 1 calc R . . H62B H 0.8832 0.0938 0.6278 0.152 Uiso 1 1 calc R . . C63 C 0.7832(13) 0.0555(9) 0.6767(7) 0.155(6) Uani 1 1 d . . . H63A H 0.7768 0.0083 0.6574 0.186 Uiso 1 1 calc R . . H63B H 0.7109 0.0664 0.6828 0.186 Uiso 1 1 calc R . . C64 C 0.8596(18) 0.0532(11) 0.7373(7) 0.217(9) Uani 1 1 d . . . H64A H 0.8316 0.0183 0.7589 0.326 Uiso 1 1 calc R . . H64B H 0.8638 0.0986 0.7585 0.326 Uiso 1 1 calc R . . H64C H 0.9317 0.0414 0.7326 0.326 Uiso 1 1 calc R . . C65 C 0.6664(9) 0.1331(6) 0.4781(6) 0.119(4) Uani 1 1 d . . . H65A H 0.6122 0.1605 0.4925 0.143 Uiso 1 1 calc R . . H65B H 0.6856 0.1575 0.4461 0.143 Uiso 1 1 calc R . . C66 C 0.6144(10) 0.0664(8) 0.4537(7) 0.145(5) Uani 1 1 d . . . H66A H 0.6710 0.0366 0.4445 0.174 Uiso 1 1 calc R . . H66B H 0.5857 0.0450 0.4843 0.174 Uiso 1 1 calc R . . C67 C 0.5298(12) 0.0646(10) 0.4035(7) 0.183(8) Uani 1 1 d D . . H67A H 0.5014 0.1115 0.4021 0.220 Uiso 1 1 calc R . . H67B H 0.4718 0.0334 0.4107 0.220 Uiso 1 1 calc R . . C68 C 0.5432(18) 0.0440(11) 0.3435(7) 0.226(11) Uani 1 1 d D . . H68A H 0.4881 0.0652 0.3151 0.339 Uiso 1 1 calc R . . H68B H 0.5352 -0.0064 0.3367 0.339 Uiso 1 1 calc R . . H68C H 0.6149 0.0598 0.3395 0.339 Uiso 1 1 calc R . . C69 C 0.8554(8) 0.0899(6) 0.5092(5) 0.103(3) Uani 1 1 d . . . H69A H 0.9205 0.0942 0.5411 0.123 Uiso 1 1 calc R . . H69B H 0.8288 0.0410 0.5049 0.123 Uiso 1 1 calc R . . C70 C 0.8889(9) 0.1062(7) 0.4546(5) 0.114(4) Uani 1 1 d . . . H70A H 0.9106 0.1559 0.4571 0.137 Uiso 1 1 calc R . . H70B H 0.8262 0.0974 0.4216 0.137 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 Mo1 0.0758(4) 0.0696(4) 0.0631(4) -0.0065(3) 0.0328(3) 0.0079(3) Mo2 0.0655(4) 0.0820(5) 0.0621(4) 0.0111(3) 0.0258(3) -0.0099(3) Mo3 0.0598(4) 0.0802(5) 0.0528(4) 0.0169(3) 0.0194(3) 0.0139(3) Mo4 0.0604(4) 0.0889(5) 0.0689(4) 0.0182(4) 0.0141(3) 0.0140(4) Mo5 0.0648(4) 0.0599(4) 0.0561(4) 0.0094(3) 0.0258(3) 0.0004(3) Mo6 0.0877(5) 0.0588(4) 0.0536(4) -0.0004(3) 0.0264(3) 0.0020(3) Mo7 0.0846(5) 0.1086(6) 0.0710(5) 0.0359(4) 0.0407(4) 0.0262(4) Mo8 0.0455(3) 0.0971(5) 0.0603(4) 0.0015(3) 0.0182(3) 0.0125(3) Mo9 0.0524(4) 0.0868(5) 0.0594(4) 0.0083(3) 0.0178(3) -0.0060(3) Mo10 0.0587(4) 0.0947(5) 0.0524(4) 0.0034(3) 0.0218(3) 0.0146(3) Mo11 0.0462(3) 0.0879(5) 0.0598(4) 0.0063(3) 0.0089(3) -0.0053(3) Mo12 0.0475(4) 0.1423(7) 0.0455(4) -0.0083(4) 0.0058(3) 0.0217(4) O1 0.049(2) 0.062(3) 0.052(3) 0.011(2) 0.017(2) 0.005(2) O2 0.091(4) 0.114(5) 0.092(4) 0.016(4) 0.037(4) -0.031(4) O3 0.072(4) 0.126(5) 0.073(4) 0.034(3) 0.016(3) 0.026(3) O4 0.076(4) 0.141(6) 0.098(5) 0.040(4) 0.012(3) 0.029(4) O5 0.084(4) 0.082(4) 0.071(3) 0.019(3) 0.028(3) -0.015(3) O6 0.146(6) 0.073(4) 0.069(4) -0.007(3) 0.039(4) 0.002(4) O7 0.052(3) 0.081(3) 0.064(3) 0.021(3) 0.020(2) 0.004(2) O8 0.080(3) 0.063(3) 0.053(3) 0.005(2) 0.033(2) 0.004(3) O9 0.070(3) 0.068(3) 0.063(3) 0.018(2) 0.016(2) 0.012(3) O10 0.081(3) 0.057(3) 0.068(3) -0.004(2) 0.029(3) -0.004(3) O11 0.072(3) 0.073(3) 0.054(3) 0.016(2) 0.020(2) 0.001(3) O12 0.081(3) 0.066(3) 0.067(3) 0.011(3) 0.029(3) 0.022(3) O13 0.073(3) 0.077(3) 0.049(3) 0.002(2) 0.018(2) -0.001(3) O14 0.079(4) 0.082(4) 0.051(3) 0.004(3) 0.011(2) -0.004(3) O15 0.090(4) 0.066(3) 0.062(3) 0.000(2) 0.024(3) -0.012(3) O16 0.053(3) 0.098(4) 0.078(4) 0.014(3) 0.016(3) -0.005(3) O17 0.073(3) 0.088(4) 0.066(3) 0.005(3) 0.038(3) 0.001(3) O18 0.074(3) 0.076(4) 0.084(4) 0.008(3) 0.029(3) 0.022(3) O19 0.043(2) 0.084(3) 0.046(2) 0.011(2) 0.014(2) 0.008(2) O20 0.060(3) 0.111(5) 0.090(4) -0.013(3) 0.025(3) 0.018(3) O21 0.085(4) 0.100(5) 0.101(4) 0.026(4) 0.036(3) -0.008(3) O22 0.081(4) 0.116(5) 0.072(4) -0.007(3) 0.031(3) 0.026(3) O23 0.064(3) 0.115(5) 0.084(4) -0.002(4) 0.001(3) -0.013(3) O24 0.061(3) 0.194(8) 0.061(3) -0.029(4) -0.003(3) 0.028(4) O25 0.070(3) 0.096(4) 0.088(4) 0.028(3) 0.033(3) 0.000(3) O26 0.074(3) 0.118(5) 0.074(4) 0.023(3) 0.045(3) 0.027(3) O27 0.083(4) 0.095(4) 0.069(3) 0.026(3) 0.030(3) 0.024(3) O28 0.082(4) 0.143(6) 0.050(3) 0.025(3) 0.019(3) 0.040(4) O29 0.053(3) 0.119(5) 0.053(3) -0.014(3) 0.011(2) 0.019(3) O30 0.059(3) 0.086(4) 0.067(3) 0.008(3) 0.019(2) 0.006(3) O31 0.053(3) 0.121(5) 0.051(3) 0.000(3) 0.013(2) 0.021(3) O32 0.043(3) 0.098(4) 0.066(3) 0.012(3) 0.015(2) 0.007(3) O33 0.053(3) 0.088(4) 0.052(3) 0.015(2) 0.005(2) -0.001(2) O34 0.054(3) 0.095(4) 0.051(3) 0.001(3) 0.025(2) -0.001(3) O35 0.044(3) 0.104(4) 0.068(3) -0.009(3) 0.012(2) -0.008(3) O36 0.057(3) 0.089(4) 0.056(3) -0.002(3) 0.009(2) -0.005(3) N1 0.123(6) 0.087(5) 0.076(4) -0.017(4) 0.046(4) 0.014(4) N2 0.130(7) 0.153(6) 0.112(6) 0.082(5) 0.072(5) 0.062(5) N3 0.066(4) 0.068(4) 0.053(3) 0.008(3) 0.021(3) 0.001(3) N4 0.085(3) 0.207(6) 0.089(3) 0.021(4) 0.028(2) 0.018(3) N5 0.142(4) 0.139(5) 0.077(3) 0.000(3) 0.040(3) -0.031(3) N6 0.067(5) 0.070(5) 0.136(7) 0.008(5) 0.023(5) -0.006(4) C1 0.112 0.099 0.075 -0.017 0.042 0.018 C2 0.112 0.099 0.075 -0.017 0.042 0.018 C3 0.112 0.099 0.075 -0.017 0.042 0.018 C4 0.157 0.165 0.124 0.095 0.092 0.082 C5 0.157 0.165 0.124 0.095 0.092 0.082 C6 0.157 0.165 0.124 0.095 0.092 0.082 C7 0.079(7) 0.143(10) 0.102(8) 0.021(7) 0.007(6) -0.013(7) C8 0.095(8) 0.183(13) 0.090(7) 0.035(8) 0.011(6) -0.022(8) C9 0.123(11) 0.141(13) 0.197(15) 0.009(11) 0.047(10) 0.009(9) C10 0.146(13) 0.163(15) 0.207(17) 0.010(12) 0.086(12) 0.030(11) C11 0.135(12) 0.106(11) 0.26(2) -0.027(12) 0.080(13) -0.003(9) C12 0.165(17) 0.21(2) 0.31(3) -0.087(19) 0.134(19) -0.001(15) C13 0.076(5) 0.080(5) 0.052(4) 0.018(4) 0.017(4) 0.000(4) C14 0.070(5) 0.080(6) 0.066(5) 0.015(4) 0.013(4) -0.008(4) C15 0.074(5) 0.085(6) 0.086(6) 0.031(5) 0.015(4) -0.001(5) C16 0.108(8) 0.122(9) 0.134(10) 0.053(8) 0.025(7) 0.019(7) C17 0.071(5) 0.085(6) 0.070(5) 0.021(4) 0.026(4) -0.001(4) C18 0.090(7) 0.097(7) 0.091(7) 0.018(5) 0.022(5) -0.013(5) C19 0.080(7) 0.198(13) 0.104(8) 0.037(8) 0.015(6) -0.043(8) C20 0.117(11) 0.29(2) 0.147(13) 0.038(14) 0.018(10) -0.023(13) C21 0.085(6) 0.065(5) 0.061(5) 0.000(4) 0.017(4) -0.001(4) C22 0.113(7) 0.067(5) 0.064(5) 0.010(4) 0.025(5) 0.003(5) C23 0.131(9) 0.084(7) 0.079(6) 0.002(5) 0.008(6) 0.015(6) C24 0.127(9) 0.120(9) 0.076(6) 0.000(6) 0.018(6) 0.042(7) C25 0.078(5) 0.062(5) 0.056(4) 0.007(3) 0.016(4) -0.002(4) C26 0.078(5) 0.064(5) 0.076(5) 0.006(4) 0.024(4) 0.005(4) C27 0.087(6) 0.076(6) 0.107(7) 0.006(5) 0.003(5) 0.016(5) C28 0.072(7) 0.130(10) 0.165(12) 0.009(8) 0.007(7) 0.008(6) C29 0.055(5) 0.117(8) 0.078(6) 0.002(5) 0.025(4) 0.002(5) C30 0.078(6) 0.118(9) 0.121(8) -0.010(7) 0.040(6) -0.014(6) C31 0.099(8) 0.122(10) 0.136(10) 0.003(8) 0.038(7) -0.012(7) C32 0.156(13) 0.110(10) 0.217(16) 0.032(10) 0.069(12) -0.008(9) C33 0.049(4) 0.108(7) 0.081(6) -0.001(5) 0.021(4) -0.010(4) C34 0.069(5) 0.111(8) 0.090(6) 0.002(5) 0.026(5) 0.001(5) C35 0.088(7) 0.108(8) 0.114(8) -0.015(6) 0.035(6) -0.010(6) C36 0.119(9) 0.118(9) 0.119(9) 0.018(7) 0.037(7) 0.002(7) C37 0.085(3) 0.207(6) 0.089(3) 0.021(4) 0.028(2) 0.018(3) C38 0.085(3) 0.207(6) 0.089(3) 0.021(4) 0.028(2) 0.018(3) C39 0.085(3) 0.207(6) 0.089(3) 0.021(4) 0.028(2) 0.018(3) C40 0.085(3) 0.207(6) 0.089(3) 0.021(4) 0.028(2) 0.018(3) C41 0.046(4) 0.117(7) 0.079(6) 0.008(5) 0.012(4) 0.001(4) C42 0.071(6) 0.136(9) 0.078(6) 0.005(6) 0.020(5) 0.000(6) C43 0.094(7) 0.149(10) 0.097(7) 0.035(7) 0.032(6) 0.010(7) C44 0.114(9) 0.150(11) 0.104(8) 0.055(8) 0.026(7) 0.005(8) C45 0.077(5) 0.098(6) 0.048(4) 0.003(4) 0.024(4) 0.000(5) C46 0.079(5) 0.099(7) 0.062(5) 0.009(4) 0.025(4) 0.005(5) C47 0.079(6) 0.109(7) 0.057(5) 0.005(5) 0.015(4) 0.007(5) C48 0.082(6) 0.105(7) 0.081(6) 0.015(5) 0.009(5) -0.005(5) C49 0.078(5) 0.109(7) 0.044(4) 0.004(4) 0.017(4) 0.007(5) C50 0.074(6) 0.130(8) 0.066(5) -0.011(5) 0.023(4) -0.007(5) C51 0.069(6) 0.120(8) 0.085(6) -0.016(6) 0.005(5) -0.004(5) C52 0.068(6) 0.135(10) 0.166(12) -0.028(9) -0.003(7) 0.007(6) C53 0.105(7) 0.105(7) 0.055(5) 0.009(4) 0.038(5) 0.015(5) C54 0.124(9) 0.127(9) 0.072(6) 0.017(6) 0.033(6) 0.029(7) C55 0.160(12) 0.199(14) 0.099(8) 0.054(9) 0.060(8) 0.081(11) C56 0.186(15) 0.28(2) 0.159(13) 0.106(14) 0.089(12) 0.145(16) C57 0.142(4) 0.139(5) 0.077(3) 0.000(3) 0.040(3) -0.031(3) C58 0.142(4) 0.139(5) 0.077(3) 0.000(3) 0.040(3) -0.031(3) C59 0.142(4) 0.139(5) 0.077(3) 0.000(3) 0.040(3) -0.031(3) C60 0.142(4) 0.139(5) 0.077(3) 0.000(3) 0.040(3) -0.031(3) C61 0.100(8) 0.107(9) 0.159(12) -0.001(8) 0.040(9) 0.010(7) C62 0.127(10) 0.157(12) 0.090(8) 0.004(8) 0.016(8) 0.008(9) C63 0.151(13) 0.178(15) 0.148(13) 0.016(11) 0.052(11) 0.052(11) C64 0.25(2) 0.27(2) 0.125(13) 0.035(14) 0.022(14) 0.045(19) C65 0.087(7) 0.098(8) 0.168(12) 0.007(8) 0.018(8) 0.013(6) C66 0.085(8) 0.138(12) 0.202(15) -0.016(11) 0.014(9) 0.026(8) C67 0.118(11) 0.211(18) 0.197(17) -0.040(14) -0.011(12) 0.069(11) C68 0.34(3) 0.24(2) 0.124(12) 0.027(13) 0.076(15) 0.17(2) C69 0.061(5) 0.114(8) 0.135(9) 0.027(7) 0.023(6) 0.007(5) C70 0.074(6) 0.146(10) 0.121(9) 0.037(8) 0.015(6) -0.008(7) _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 Mo1 N1 1.713(7) . ? Mo1 O13 1.934(5) . ? Mo1 O10 1.952(5) . ? Mo1 O17 1.955(5) . ? Mo1 O18 1.963(6) . ? Mo1 O1 2.230(5) . ? Mo2 O2 1.687(6) . ? Mo2 O17 1.879(5) . ? Mo2 O11 1.921(5) . ? Mo2 O16 1.927(6) . ? Mo2 O15 1.928(5) . ? Mo2 O1 2.330(4) . ? Mo3 O3 1.673(5) . ? Mo3 O13 1.905(5) . ? Mo3 O12 1.917(5) . ? Mo3 O7 1.928(5) . ? Mo3 O11 1.935(5) . ? Mo3 O1 2.317(4) . ? Mo4 O4 1.673(6) . ? Mo4 O18 1.869(6) . ? Mo4 O16 1.929(5) . ? Mo4 O14 1.940(5) . ? Mo4 O9 1.945(5) . ? Mo4 O1 2.328(4) . ? Mo5 O5 1.690(5) . ? Mo5 O10 1.900(5) . ? Mo5 O8 1.907(5) . ? Mo5 O9 1.915(5) . ? Mo5 O7 1.930(5) . ? Mo5 O1 2.323(4) . ? Mo6 O6 1.678(6) . ? Mo6 O14 1.887(6) . ? Mo6 O15 1.912(5) . ? Mo6 O12 1.937(5) . ? Mo6 O8 1.940(5) . ? Mo6 O1 2.341(5) . ? Mo7 N2 1.691(8) . ? Mo7 O25 1.939(6) . ? Mo7 O26 1.949(6) . ? Mo7 O28 1.955(6) . ? Mo7 O27 1.961(5) . ? Mo7 O19 2.212(5) . ? Mo8 O20 1.693(5) . ? Mo8 O26 1.893(6) . ? Mo8 O32 1.895(5) . ? Mo8 O30 1.937(5) . ? Mo8 O29 1.959(5) . ? Mo8 O19 2.337(4) . ? Mo9 O21 1.681(6) . ? Mo9 O33 1.906(5) . ? Mo9 O35 1.910(5) . ? Mo9 O30 1.912(5) . ? Mo9 O34 1.934(5) . ? Mo9 O19 2.350(5) . ? Mo10 O22 1.688(5) . ? Mo10 O27 1.879(5) . ? Mo10 O31 1.906(5) . ? Mo10 O34 1.914(5) . ? Mo10 O36 1.964(5) . ? Mo10 O19 2.327(4) . ? Mo11 O23 1.681(5) . ? Mo11 O25 1.892(5) . ? Mo11 O36 1.904(5) . ? Mo11 O33 1.922(5) . ? Mo11 O32 1.979(5) . ? Mo11 O19 2.330(4) . ? Mo12 O24 1.683(6) . ? Mo12 O28 1.885(7) . ? Mo12 O29 1.902(5) . ? Mo12 O35 1.929(6) . ? Mo12 O31 1.965(5) . ? Mo12 O19 2.318(4) . ? N1 C1 1.497(10) . ? N2 C4 1.493(13) . ? N3 C21 1.499(9) . ? N3 C17 1.515(9) . ? N3 C25 1.519(9) . ? N3 C13 1.533(9) . ? N4 C29 1.517(13) . ? N4 C41 1.524(11) . ? N4 C33 1.536(13) . ? N4 C37 1.543(13) . ? N5 C57 1.516(13) . ? N5 C49 1.517(12) . ? N5 C45 1.520(11) . ? N5 C53 1.531(13) . ? N6 C61 1.489(14) . ? N6 C9 1.495(15) . ? N6 C69 1.513(12) . ? N6 C65 1.516(13) . ? C1 C2 1.443(10) . ? C1 C3 1.452(10) . ? C1 H1 0.9800 . ? C2 H2A 0.9600 . ? C2 H2B 0.9600 . ? C2 H2C 0.9600 . ? C3 H3A 0.9600 . ? C3 H3B 0.9600 . ? C3 H3C 0.9600 . ? C4 C6 1.448(10) . ? C4 C5 1.469(13) . ? C4 H4 0.9800 . ? C5 H5A 0.9600 . ? C5 H5B 0.9600 . ? C5 H5C 0.9600 . ? C6 H6A 0.9600 . ? C6 H6B 0.9600 . ? C6 H6C 0.9600 . ? C7 C8 1.474(14) . ? C7 C70 1.510(15) . ? C7 H7A 0.9700 . ? C7 H7B 0.9700 . ? C8 H8A 0.9600 . ? C8 H8B 0.9600 . ? C8 H8C 0.9600 . ? C9 C10 1.495(8) . ? C9 H9A 0.9700 . ? C9 H9B 0.9700 . ? C10 C11 1.532(15) . ? C10 H10A 0.9700 . ? C10 H10B 0.9700 . ? C11 C12 1.511(9) . ? C11 H11A 0.9700 . ? C11 H11B 0.9700 . ? C12 H12A 0.9600 . ? C12 H12B 0.9600 . ? C12 H12C 0.9600 . ? C13 C14 1.506(11) . ? C13 H13A 0.9700 . ? C13 H13B 0.9700 . ? C14 C15 1.524(11) . ? C14 H14A 0.9700 . ? C14 H14B 0.9700 . ? C15 C16 1.456(13) . ? C15 H15A 0.9700 . ? C15 H15B 0.9700 . ? C16 H16A 0.9600 . ? C16 H16B 0.9600 . ? C16 H16C 0.9600 . ? C17 C18 1.494(12) . ? C17 H17A 0.9700 . ? C17 H17B 0.9700 . ? C18 C19 1.546(14) . ? C18 H18A 0.9700 . ? C18 H18B 0.9700 . ? C19 C20 1.496(9) . ? C19 H19A 0.9700 . ? C19 H19B 0.9700 . ? C20 H20A 0.9600 . ? C20 H20B 0.9600 . ? C20 H20C 0.9600 . ? C21 C22 1.505(11) . ? C21 H21A 0.9700 . ? C21 H21B 0.9700 . ? C22 C23 1.520(13) . ? C22 H22A 0.9700 . ? C22 H22B 0.9700 . ? C23 C24 1.499(14) . ? C23 H23A 0.9700 . ? C23 H23B 0.9700 . ? C24 H24A 0.9600 . ? C24 H24B 0.9600 . ? C24 H24C 0.9600 . ? C25 C26 1.525(11) . ? C25 H25A 0.9700 . ? C25 H25B 0.9700 . ? C26 C27 1.484(12) . ? C26 H26A 0.9700 . ? C26 H26B 0.9700 . ? C27 C28 1.533(14) . ? C27 H27A 0.9700 . ? C27 H27B 0.9700 . ? C28 H28A 0.9600 . ? C28 H28B 0.9600 . ? C28 H28C 0.9600 . ? C29 C30 1.465(13) . ? C29 H29A 0.9700 . ? C29 H29B 0.9700 . ? C30 C31 1.482(15) . ? C30 H30A 0.9700 . ? C30 H30B 0.9700 . ? C31 C32 1.517(16) . ? C31 H31A 0.9700 . ? C31 H31B 0.9700 . ? C32 H32A 0.9600 . ? C32 H32B 0.9600 . ? C32 H32C 0.9600 . ? C33 C34 1.499(12) . ? C33 H33A 0.9700 . ? C33 H33B 0.9700 . ? C34 C35 1.468(13) . ? C34 H34A 0.9700 . ? C34 H34B 0.9700 . ? C35 C36 1.491(14) . ? C35 H35A 0.9700 . ? C35 H35B 0.9700 . ? C36 H36A 0.9600 . ? C36 H36B 0.9600 . ? C36 H36C 0.9600 . ? C37 C38 1.507(14) . ? C37 H37A 0.9700 . ? C37 H37B 0.9700 . ? C38 C39 1.446(13) . ? C38 H38A 0.9700 . ? C38 H38B 0.9700 . ? C39 C40 1.498(8) . ? C39 H39A 0.9700 . ? C39 H39B 0.9700 . ? C40 H40A 0.9600 . ? C40 H40B 0.9600 . ? C40 H40C 0.9600 . ? C41 C42 1.525(12) . ? C41 H41A 0.9700 . ? C41 H41B 0.9700 . ? C42 C43 1.465(13) . ? C42 H42A 0.9700 . ? C42 H42B 0.9700 . ? C43 C44 1.523(13) . ? C43 H43A 0.9700 . ? C43 H43B 0.9700 . ? C44 H44A 0.9600 . ? C44 H44B 0.9600 . ? C44 H44C 0.9600 . ? C45 C46 1.522(11) . ? C45 H45A 0.9700 . ? C45 H45B 0.9700 . ? C46 C47 1.510(11) . ? C46 H46A 0.9700 . ? C46 H46B 0.9700 . ? C47 C48 1.500(12) . ? C47 H47A 0.9700 . ? C47 H47B 0.9700 . ? C48 H48A 0.9600 . ? C48 H48B 0.9600 . ? C48 H48C 0.9600 . ? C49 C50 1.505(12) . ? C49 H49A 0.9700 . ? C49 H49B 0.9700 . ? C50 C51 1.516(13) . ? C50 H50A 0.9700 . ? C50 H50B 0.9700 . ? C51 C52 1.488(13) . ? C51 H51A 0.9700 . ? C51 H51B 0.9700 . ? C52 H52A 0.9600 . ? C52 H52B 0.9600 . ? C52 H52C 0.9600 . ? C53 C54 1.504(12) . ? C53 H53A 0.9700 . ? C53 H53B 0.9700 . ? C54 C55 1.494(14) . ? C54 H54A 0.9700 . ? C54 H54B 0.9700 . ? C55 C56 1.551(16) . ? C55 H55A 0.9700 . ? C55 H55B 0.9700 . ? C56 H56A 0.9600 . ? C56 H56B 0.9600 . ? C56 H56C 0.9600 . ? C57 C58 1.498(12) . ? C57 H57A 0.9700 . ? C57 H57B 0.9700 . ? C58 C59 1.507(12) . ? C58 H58A 0.9700 . ? C58 H58B 0.9700 . ? C59 C60 1.523(8) . ? C59 H59A 0.9700 . ? C59 H59B 0.9700 . ? C60 H60A 0.9600 . ? C60 H60B 0.9600 . ? C60 H60C 0.9600 . ? C61 C62 1.445(15) . ? C61 H61A 0.9700 . ? C61 H61B 0.9700 . ? C62 C63 1.479(18) . ? C62 H62A 0.9700 . ? C62 H62B 0.9700 . ? C63 C64 1.52(2) . ? C63 H63A 0.9700 . ? C63 H63B 0.9700 . ? C64 H64A 0.9600 . ? C64 H64B 0.9600 . ? C64 H64C 0.9600 . ? C65 C66 1.431(16) . ? C65 H65A 0.9700 . ? C65 H65B 0.9700 . ? C66 C67 1.388(17) . ? C66 H66A 0.9700 . ? C66 H66B 0.9700 . ? C67 C68 1.472(9) . ? C67 H67A 0.9700 . ? C67 H67B 0.9700 . ? C68 H68A 0.9600 . ? C68 H68B 0.9600 . ? C68 H68C 0.9600 . ? C69 C70 1.466(14) . ? C69 H69A 0.9700 . ? C69 H69B 0.9700 . ? C70 H70A 0.9700 . ? C70 H70B 0.9700 . ? 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 N1 Mo1 O13 102.2(3) . . ? N1 Mo1 O10 101.0(3) . . ? O13 Mo1 O10 88.3(2) . . ? N1 Mo1 O17 103.8(3) . . ? O13 Mo1 O17 87.7(2) . . ? O10 Mo1 O17 155.2(2) . . ? N1 Mo1 O18 102.2(3) . . ? O13 Mo1 O18 155.6(2) . . ? O10 Mo1 O18 86.9(2) . . ? O17 Mo1 O18 86.7(2) . . ? N1 Mo1 O1 178.7(3) . . ? O13 Mo1 O1 78.26(18) . . ? O10 Mo1 O1 77.72(18) . . ? O17 Mo1 O1 77.47(19) . . ? O18 Mo1 O1 77.39(19) . . ? O2 Mo2 O17 104.1(3) . . ? O2 Mo2 O11 103.7(3) . . ? O17 Mo2 O11 87.6(2) . . ? O2 Mo2 O16 103.4(3) . . ? O17 Mo2 O16 87.8(3) . . ? O11 Mo2 O16 152.9(2) . . ? O2 Mo2 O15 102.9(3) . . ? O17 Mo2 O15 153.0(2) . . ? O11 Mo2 O15 86.6(2) . . ? O16 Mo2 O15 85.5(2) . . ? O2 Mo2 O1 179.5(3) . . ? O17 Mo2 O1 76.40(19) . . ? O11 Mo2 O1 76.45(18) . . ? O16 Mo2 O1 76.50(18) . . ? O15 Mo2 O1 76.57(19) . . ? O3 Mo3 O13 102.7(3) . . ? O3 Mo3 O12 103.8(3) . . ? O13 Mo3 O12 153.5(2) . . ? O3 Mo3 O7 103.9(3) . . ? O13 Mo3 O7 87.1(2) . . ? O12 Mo3 O7 87.4(2) . . ? O3 Mo3 O11 102.6(3) . . ? O13 Mo3 O11 86.5(2) . . ? O12 Mo3 O11 86.9(2) . . ? O7 Mo3 O11 153.4(2) . . ? O3 Mo3 O1 178.9(2) . . ? O13 Mo3 O1 76.65(19) . . ? O12 Mo3 O1 76.88(19) . . ? O7 Mo3 O1 76.90(18) . . ? O11 Mo3 O1 76.52(18) . . ? O4 Mo4 O18 104.5(3) . . ? O4 Mo4 O16 102.9(3) . . ? O18 Mo4 O16 89.0(2) . . ? O4 Mo4 O14 102.4(3) . . ? O18 Mo4 O14 153.1(2) . . ? O16 Mo4 O14 85.5(2) . . ? O4 Mo4 O9 104.4(3) . . ? O18 Mo4 O9 88.5(2) . . ? O16 Mo4 O9 152.3(2) . . ? O14 Mo4 O9 84.3(2) . . ? O4 Mo4 O1 178.7(3) . . ? O18 Mo4 O1 76.7(2) . . ? O16 Mo4 O1 76.52(19) . . ? O14 Mo4 O1 76.37(19) . . ? O9 Mo4 O1 76.07(18) . . ? O5 Mo5 O10 101.7(3) . . ? O5 Mo5 O8 104.2(2) . . ? O10 Mo5 O8 154.1(2) . . ? O5 Mo5 O9 103.4(2) . . ? O10 Mo5 O9 88.1(2) . . ? O8 Mo5 O9 86.5(2) . . ? O5 Mo5 O7 103.2(2) . . ? O10 Mo5 O7 86.4(2) . . ? O8 Mo5 O7 87.2(2) . . ? O9 Mo5 O7 153.4(2) . . ? O5 Mo5 O1 178.1(2) . . ? O10 Mo5 O1 76.40(19) . . ? O8 Mo5 O1 77.70(18) . . ? O9 Mo5 O1 76.74(18) . . ? O7 Mo5 O1 76.72(18) . . ? O6 Mo6 O14 103.1(3) . . ? O6 Mo6 O15 102.8(3) . . ? O14 Mo6 O15 88.1(2) . . ? O6 Mo6 O12 104.0(3) . . ? O14 Mo6 O12 152.9(2) . . ? O15 Mo6 O12 86.2(2) . . ? O6 Mo6 O8 104.0(3) . . ? O14 Mo6 O8 87.9(2) . . ? O15 Mo6 O8 153.1(2) . . ? O12 Mo6 O8 85.3(2) . . ? O6 Mo6 O1 179.4(3) . . ? O14 Mo6 O1 77.00(19) . . ? O15 Mo6 O1 76.58(19) . . ? O12 Mo6 O1 75.92(18) . . ? O8 Mo6 O1 76.64(17) . . ? N2 Mo7 O25 102.1(4) . . ? N2 Mo7 O26 102.8(3) . . ? O25 Mo7 O26 87.7(3) . . ? N2 Mo7 O28 101.7(4) . . ? O25 Mo7 O28 156.2(2) . . ? O26 Mo7 O28 87.6(3) . . ? N2 Mo7 O27 101.4(3) . . ? O25 Mo7 O27 87.6(2) . . ? O26 Mo7 O27 155.9(2) . . ? O28 Mo7 O27 87.2(2) . . ? N2 Mo7 O19 178.6(3) . . ? O25 Mo7 O19 78.5(2) . . ? O26 Mo7 O19 78.5(2) . . ? O28 Mo7 O19 77.7(2) . . ? O27 Mo7 O19 77.4(2) . . ? O20 Mo8 O26 103.3(3) . . ? O20 Mo8 O32 103.5(2) . . ? O26 Mo8 O32 88.4(3) . . ? O20 Mo8 O30 103.4(3) . . ? O26 Mo8 O30 153.3(2) . . ? O32 Mo8 O30 86.9(2) . . ? O20 Mo8 O29 103.6(2) . . ? O26 Mo8 O29 87.1(3) . . ? O32 Mo8 O29 152.8(2) . . ? O30 Mo8 O29 85.1(2) . . ? O20 Mo8 O19 179.5(2) . . ? O26 Mo8 O19 76.45(19) . . ? O32 Mo8 O19 76.96(18) . . ? O30 Mo8 O19 76.85(19) . . ? O29 Mo8 O19 75.91(18) . . ? O21 Mo9 O33 104.3(3) . . ? O21 Mo9 O35 103.1(3) . . ? O33 Mo9 O35 152.6(2) . . ? O21 Mo9 O30 102.6(3) . . ? O33 Mo9 O30 86.6(2) . . ? O35 Mo9 O30 87.6(2) . . ? O21 Mo9 O34 104.3(3) . . ? O33 Mo9 O34 86.9(2) . . ? O35 Mo9 O34 86.4(2) . . ? O30 Mo9 O34 153.2(2) . . ? O21 Mo9 O19 179.3(3) . . ? O33 Mo9 O19 76.25(18) . . ? O35 Mo9 O19 76.3(2) . . ? O30 Mo9 O19 77.0(2) . . ? O34 Mo9 O19 76.17(18) . . ? O22 Mo10 O27 105.0(3) . . ? O22 Mo10 O31 103.1(3) . . ? O27 Mo10 O31 88.7(3) . . ? O22 Mo10 O34 101.8(3) . . ? O27 Mo10 O34 153.1(2) . . ? O31 Mo10 O34 87.7(2) . . ? O22 Mo10 O36 103.2(3) . . ? O27 Mo10 O36 86.5(2) . . ? O31 Mo10 O36 153.7(2) . . ? O34 Mo10 O36 85.0(2) . . ? O22 Mo10 O19 178.9(3) . . ? O27 Mo10 O19 76.1(2) . . ? O31 Mo10 O19 77.26(18) . . ? O34 Mo10 O19 77.10(18) . . ? O36 Mo10 O19 76.44(19) . . ? O23 Mo11 O25 103.7(3) . . ? O23 Mo11 O36 104.8(3) . . ? O25 Mo11 O36 89.5(2) . . ? O23 Mo11 O33 103.2(3) . . ? O25 Mo11 O33 152.7(2) . . ? O36 Mo11 O33 87.7(2) . . ? O23 Mo11 O32 102.1(3) . . ? O25 Mo11 O32 86.2(2) . . ? O36 Mo11 O32 153.1(2) . . ? O33 Mo11 O32 84.2(2) . . ? O23 Mo11 O19 177.7(3) . . ? O25 Mo11 O19 76.4(2) . . ? O36 Mo11 O19 77.48(18) . . ? O33 Mo11 O19 76.47(18) . . ? O32 Mo11 O19 75.64(18) . . ? O24 Mo12 O28 104.5(3) . . ? O24 Mo12 O29 103.2(3) . . ? O28 Mo12 O29 88.9(3) . . ? O24 Mo12 O35 102.3(3) . . ? O28 Mo12 O35 153.1(2) . . ? O29 Mo12 O35 87.4(2) . . ? O24 Mo12 O31 103.0(3) . . ? O28 Mo12 O31 86.8(3) . . ? O29 Mo12 O31 153.7(2) . . ? O35 Mo12 O31 84.9(2) . . ? O24 Mo12 O19 178.9(3) . . ? O28 Mo12 O19 76.4(2) . . ? O29 Mo12 O19 77.42(19) . . ? O35 Mo12 O19 76.76(18) . . ? O31 Mo12 O19 76.37(18) . . ? Mo1 O1 Mo3 90.51(16) . . ? Mo1 O1 Mo5 90.97(17) . . ? Mo3 O1 Mo5 89.94(15) . . ? Mo1 O1 Mo4 90.54(16) . . ? Mo3 O1 Mo4 178.9(2) . . ? Mo5 O1 Mo4 90.13(15) . . ? Mo1 O1 Mo2 90.63(15) . . ? Mo3 O1 Mo2 90.06(15) . . ? Mo5 O1 Mo2 178.4(2) . . ? Mo4 O1 Mo2 89.84(15) . . ? Mo1 O1 Mo6 179.6(2) . . ? Mo3 O1 Mo6 89.91(15) . . ? Mo5 O1 Mo6 89.08(14) . . ? Mo4 O1 Mo6 89.04(15) . . ? Mo2 O1 Mo6 89.31(16) . . ? Mo3 O7 Mo5 116.4(2) . . ? Mo5 O8 Mo6 116.5(2) . . ? Mo5 O9 Mo4 117.0(2) . . ? Mo5 O10 Mo1 114.9(2) . . ? Mo2 O11 Mo3 117.0(2) . . ? Mo3 O12 Mo6 117.3(2) . . ? Mo3 O13 Mo1 114.6(2) . . ? Mo6 O14 Mo4 117.6(2) . . ? Mo6 O15 Mo2 117.5(3) . . ? Mo2 O16 Mo4 117.1(2) . . ? Mo2 O17 Mo1 115.5(2) . . ? Mo4 O18 Mo1 115.3(3) . . ? Mo7 O19 Mo12 91.10(16) . . ? Mo7 O19 Mo10 91.22(18) . . ? Mo12 O19 Mo10 90.10(15) . . ? Mo7 O19 Mo11 90.42(17) . . ? Mo12 O19 Mo11 178.5(2) . . ? Mo10 O19 Mo11 89.77(16) . . ? Mo7 O19 Mo8 90.48(15) . . ? Mo12 O19 Mo8 89.87(16) . . ? Mo10 O19 Mo8 178.3(2) . . ? Mo11 O19 Mo8 90.21(15) . . ? Mo7 O19 Mo9 179.3(2) . . ? Mo12 O19 Mo9 89.36(16) . . ? Mo10 O19 Mo9 89.32(14) . . ? Mo11 O19 Mo9 89.12(15) . . ? Mo8 O19 Mo9 88.98(17) . . ? Mo11 O25 Mo7 114.7(3) . . ? Mo8 O26 Mo7 114.6(2) . . ? Mo10 O27 Mo7 115.3(3) . . ? Mo12 O28 Mo7 114.8(3) . . ? Mo12 O29 Mo8 116.8(3) . . ? Mo9 O30 Mo8 117.2(3) . . ? Mo10 O31 Mo12 116.3(2) . . ? Mo8 O32 Mo11 117.2(2) . . ? Mo9 O33 Mo11 118.1(2) . . ? Mo10 O34 Mo9 117.4(2) . . ? Mo9 O35 Mo12 117.5(3) . . ? Mo11 O36 Mo10 116.3(2) . . ? C1 N1 Mo1 175.0(7) . . ? C4 N2 Mo7 177.8(10) . . ? C21 N3 C17 110.8(6) . . ? C21 N3 C25 112.0(6) . . ? C17 N3 C25 105.8(5) . . ? C21 N3 C13 106.5(5) . . ? C17 N3 C13 111.8(6) . . ? C25 N3 C13 110.0(6) . . ? C29 N4 C41 110.6(8) . . ? C29 N4 C33 108.3(7) . . ? C41 N4 C33 109.7(9) . . ? C29 N4 C37 111.4(10) . . ? C41 N4 C37 107.2(7) . . ? C33 N4 C37 109.7(9) . . ? C57 N5 C49 111.2(9) . . ? C57 N5 C45 106.1(7) . . ? C49 N5 C45 111.1(8) . . ? C57 N5 C53 111.0(9) . . ? C49 N5 C53 106.8(7) . . ? C45 N5 C53 110.6(8) . . ? C61 N6 C9 117.0(10) . . ? C61 N6 C69 109.5(8) . . ? C9 N6 C69 101.6(8) . . ? C61 N6 C65 106.7(9) . . ? C9 N6 C65 111.3(10) . . ? C69 N6 C65 110.7(9) . . ? C2 C1 C3 121.2(8) . . ? C2 C1 N1 109.1(8) . . ? C3 C1 N1 107.6(7) . . ? C2 C1 H1 106.0 . . ? C3 C1 H1 106.0 . . ? N1 C1 H1 106.0 . . ? C1 C2 H2A 109.5 . . ? C1 C2 H2B 109.5 . . ? H2A C2 H2B 109.5 . . ? C1 C2 H2C 109.5 . . ? H2A C2 H2C 109.5 . . ? H2B C2 H2C 109.5 . . ? C1 C3 H3A 109.5 . . ? C1 C3 H3B 109.5 . . ? H3A C3 H3B 109.5 . . ? C1 C3 H3C 109.5 . . ? H3A C3 H3C 109.5 . . ? H3B C3 H3C 109.5 . . ? C6 C4 C5 121.0(11) . . ? C6 C4 N2 110.5(9) . . ? C5 C4 N2 105.2(9) . . ? C6 C4 H4 106.4 . . ? C5 C4 H4 106.4 . . ? N2 C4 H4 106.4 . . ? C4 C5 H5A 109.5 . . ? C4 C5 H5B 109.5 . . ? H5A C5 H5B 109.5 . . ? C4 C5 H5C 109.5 . . ? H5A C5 H5C 109.5 . . ? H5B C5 H5C 109.5 . . ? C4 C6 H6A 109.5 . . ? C4 C6 H6B 109.5 . . ? H6A C6 H6B 109.5 . . ? C4 C6 H6C 109.5 . . ? H6A C6 H6C 109.5 . . ? H6B C6 H6C 109.5 . . ? C8 C7 C70 115.8(10) . . ? C8 C7 H7A 108.3 . . ? C70 C7 H7A 108.3 . . ? C8 C7 H7B 108.3 . . ? C70 C7 H7B 108.3 . . ? H7A C7 H7B 107.4 . . ? C7 C8 H8A 109.5 . . ? C7 C8 H8B 109.5 . . ? H8A C8 H8B 109.5 . . ? C7 C8 H8C 109.5 . . ? H8A C8 H8C 109.5 . . ? H8B C8 H8C 109.5 . . ? N6 C9 C10 114.3(11) . . ? N6 C9 H9A 108.7 . . ? C10 C9 H9A 108.7 . . ? N6 C9 H9B 108.7 . . ? C10 C9 H9B 108.7 . . ? H9A C9 H9B 107.6 . . ? C9 C10 C11 112.1(11) . . ? C9 C10 H10A 109.2 . . ? C11 C10 H10A 109.2 . . ? C9 C10 H10B 109.2 . . ? C11 C10 H10B 109.2 . . ? H10A C10 H10B 107.9 . . ? C12 C11 C10 110.5(14) . . ? C12 C11 H11A 109.5 . . ? C10 C11 H11A 109.5 . . ? C12 C11 H11B 109.5 . . ? C10 C11 H11B 109.5 . . ? H11A C11 H11B 108.1 . . ? C11 C12 H12A 109.5 . . ? C11 C12 H12B 109.5 . . ? H12A C12 H12B 109.5 . . ? C11 C12 H12C 109.5 . . ? H12A C12 H12C 109.5 . . ? H12B C12 H12C 109.5 . . ? C14 C13 N3 117.7(6) . . ? C14 C13 H13A 107.9 . . ? N3 C13 H13A 107.9 . . ? C14 C13 H13B 107.9 . . ? N3 C13 H13B 107.9 . . ? H13A C13 H13B 107.2 . . ? C13 C14 C15 109.8(7) . . ? C13 C14 H14A 109.7 . . ? C15 C14 H14A 109.7 . . ? C13 C14 H14B 109.7 . . ? C15 C14 H14B 109.7 . . ? H14A C14 H14B 108.2 . . ? C16 C15 C14 113.9(8) . . ? C16 C15 H15A 108.8 . . ? C14 C15 H15A 108.8 . . ? C16 C15 H15B 108.8 . . ? C14 C15 H15B 108.8 . . ? H15A C15 H15B 107.7 . . ? 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 N3 116.3(7) . . ? C18 C17 H17A 108.2 . . ? N3 C17 H17A 108.2 . . ? C18 C17 H17B 108.2 . . ? N3 C17 H17B 108.2 . . ? H17A C17 H17B 107.4 . . ? C17 C18 C19 108.5(8) . . ? C17 C18 H18A 110.0 . . ? C19 C18 H18A 110.0 . . ? C17 C18 H18B 110.0 . . ? C19 C18 H18B 110.0 . . ? H18A C18 H18B 108.4 . . ? C20 C19 C18 115.0(11) . . ? C20 C19 H19A 108.5 . . ? C18 C19 H19A 108.5 . . ? C20 C19 H19B 108.5 . . ? C18 C19 H19B 108.5 . . ? H19A C19 H19B 107.5 . . ? C19 C20 H20A 109.5 . . ? C19 C20 H20B 109.5 . . ? H20A C20 H20B 109.5 . . ? C19 C20 H20C 109.5 . . ? H20A C20 H20C 109.5 . . ? H20B C20 H20C 109.5 . . ? N3 C21 C22 115.5(6) . . ? N3 C21 H21A 108.4 . . ? C22 C21 H21A 108.4 . . ? N3 C21 H21B 108.4 . . ? C22 C21 H21B 108.4 . . ? H21A C21 H21B 107.5 . . ? C21 C22 C23 110.9(7) . . ? C21 C22 H22A 109.5 . . ? C23 C22 H22A 109.5 . . ? C21 C22 H22B 109.5 . . ? C23 C22 H22B 109.5 . . ? H22A C22 H22B 108.1 . . ? C24 C23 C22 115.4(9) . . ? C24 C23 H23A 108.4 . . ? C22 C23 H23A 108.4 . . ? C24 C23 H23B 108.4 . . ? C22 C23 H23B 108.4 . . ? H23A C23 H23B 107.5 . . ? C23 C24 H24A 109.5 . . ? C23 C24 H24B 109.5 . . ? H24A C24 H24B 109.5 . . ? C23 C24 H24C 109.5 . . ? H24A C24 H24C 109.5 . . ? H24B C24 H24C 109.5 . . ? N3 C25 C26 116.8(6) . . ? N3 C25 H25A 108.1 . . ? C26 C25 H25A 108.1 . . ? N3 C25 H25B 108.1 . . ? C26 C25 H25B 108.1 . . ? H25A C25 H25B 107.3 . . ? C27 C26 C25 111.1(7) . . ? C27 C26 H26A 109.4 . . ? C25 C26 H26A 109.4 . . ? C27 C26 H26B 109.4 . . ? C25 C26 H26B 109.4 . . ? H26A C26 H26B 108.0 . . ? C26 C27 C28 112.4(9) . . ? C26 C27 H27A 109.1 . . ? C28 C27 H27A 109.1 . . ? C26 C27 H27B 109.1 . . ? C28 C27 H27B 109.1 . . ? H27A C27 H27B 107.9 . . ? C27 C28 H28A 109.5 . . ? C27 C28 H28B 109.5 . . ? H28A C28 H28B 109.5 . . ? C27 C28 H28C 109.5 . . ? H28A C28 H28C 109.5 . . ? H28B C28 H28C 109.5 . . ? C30 C29 N4 115.8(8) . . ? C30 C29 H29A 108.3 . . ? N4 C29 H29A 108.3 . . ? C30 C29 H29B 108.3 . . ? N4 C29 H29B 108.3 . . ? H29A C29 H29B 107.4 . . ? C29 C30 C31 113.2(8) . . ? C29 C30 H30A 108.9 . . ? C31 C30 H30A 108.9 . . ? C29 C30 H30B 108.9 . . ? C31 C30 H30B 108.9 . . ? H30A C30 H30B 107.7 . . ? C30 C31 C32 116.1(10) . . ? C30 C31 H31A 108.3 . . ? C32 C31 H31A 108.3 . . ? C30 C31 H31B 108.3 . . ? C32 C31 H31B 108.3 . . ? H31A C31 H31B 107.4 . . ? C31 C32 H32A 109.5 . . ? C31 C32 H32B 109.5 . . ? H32A C32 H32B 109.5 . . ? C31 C32 H32C 109.5 . . ? H32A C32 H32C 109.5 . . ? H32B C32 H32C 109.5 . . ? C34 C33 N4 116.5(7) . . ? C34 C33 H33A 108.2 . . ? N4 C33 H33A 108.2 . . ? C34 C33 H33B 108.2 . . ? N4 C33 H33B 108.2 . . ? H33A C33 H33B 107.3 . . ? C35 C34 C33 112.2(8) . . ? C35 C34 H34A 109.2 . . ? C33 C34 H34A 109.2 . . ? C35 C34 H34B 109.2 . . ? C33 C34 H34B 109.2 . . ? H34A C34 H34B 107.9 . . ? C34 C35 C36 114.2(9) . . ? C34 C35 H35A 108.7 . . ? C36 C35 H35A 108.7 . . ? C34 C35 H35B 108.7 . . ? C36 C35 H35B 108.7 . . ? H35A C35 H35B 107.6 . . ? C35 C36 H36A 109.5 . . ? C35 C36 H36B 109.5 . . ? H36A C36 H36B 109.5 . . ? C35 C36 H36C 109.5 . . ? H36A C36 H36C 109.5 . . ? H36B C36 H36C 109.5 . . ? C38 C37 N4 113.8(8) . . ? C38 C37 H37A 108.8 . . ? N4 C37 H37A 108.8 . . ? C38 C37 H37B 108.8 . . ? N4 C37 H37B 108.8 . . ? H37A C37 H37B 107.7 . . ? C39 C38 C37 111.4(9) . . ? C39 C38 H38A 109.4 . . ? C37 C38 H38A 109.4 . . ? C39 C38 H38B 109.4 . . ? C37 C38 H38B 109.4 . . ? H38A C38 H38B 108.0 . . ? C38 C39 C40 116.9(9) . . ? C38 C39 H39A 108.1 . . ? C40 C39 H39A 108.1 . . ? C38 C39 H39B 108.1 . . ? C40 C39 H39B 108.1 . . ? H39A C39 H39B 107.3 . . ? C39 C40 H40A 109.5 . . ? C39 C40 H40B 109.5 . . ? H40A C40 H40B 109.5 . . ? C39 C40 H40C 109.5 . . ? H40A C40 H40C 109.5 . . ? H40B C40 H40C 109.5 . . ? N4 C41 C42 113.7(7) . . ? N4 C41 H41A 108.8 . . ? C42 C41 H41A 108.8 . . ? N4 C41 H41B 108.8 . . ? C42 C41 H41B 108.8 . . ? H41A C41 H41B 107.7 . . ? C43 C42 C41 112.9(8) . . ? C43 C42 H42A 109.0 . . ? C41 C42 H42A 109.0 . . ? C43 C42 H42B 109.0 . . ? C41 C42 H42B 109.0 . . ? H42A C42 H42B 107.8 . . ? C42 C43 C44 113.1(9) . . ? C42 C43 H43A 109.0 . . ? C44 C43 H43A 109.0 . . ? C42 C43 H43B 109.0 . . ? C44 C43 H43B 109.0 . . ? H43A C43 H43B 107.8 . . ? C43 C44 H44A 109.5 . . ? C43 C44 H44B 109.5 . . ? H44A C44 H44B 109.5 . . ? C43 C44 H44C 109.5 . . ? H44A C44 H44C 109.5 . . ? H44B C44 H44C 109.5 . . ? N5 C45 C46 115.4(6) . . ? N5 C45 H45A 108.4 . . ? C46 C45 H45A 108.4 . . ? N5 C45 H45B 108.4 . . ? C46 C45 H45B 108.4 . . ? H45A C45 H45B 107.5 . . ? C47 C46 C45 112.2(7) . . ? C47 C46 H46A 109.2 . . ? C45 C46 H46A 109.2 . . ? C47 C46 H46B 109.2 . . ? C45 C46 H46B 109.2 . . ? H46A C46 H46B 107.9 . . ? C48 C47 C46 112.5(7) . . ? C48 C47 H47A 109.1 . . ? C46 C47 H47A 109.1 . . ? C48 C47 H47B 109.1 . . ? C46 C47 H47B 109.1 . . ? H47A C47 H47B 107.8 . . ? C47 C48 H48A 109.5 . . ? C47 C48 H48B 109.5 . . ? H48A C48 H48B 109.5 . . ? C47 C48 H48C 109.5 . . ? H48A C48 H48C 109.5 . . ? H48B C48 H48C 109.5 . . ? C50 C49 N5 116.3(7) . . ? C50 C49 H49A 108.2 . . ? N5 C49 H49A 108.2 . . ? C50 C49 H49B 108.2 . . ? N5 C49 H49B 108.2 . . ? H49A C49 H49B 107.4 . . ? C49 C50 C51 111.9(7) . . ? C49 C50 H50A 109.2 . . ? C51 C50 H50A 109.2 . . ? C49 C50 H50B 109.2 . . ? C51 C50 H50B 109.2 . . ? H50A C50 H50B 107.9 . . ? C52 C51 C50 113.0(9) . . ? C52 C51 H51A 109.0 . . ? C50 C51 H51A 109.0 . . ? C52 C51 H51B 109.0 . . ? C50 C51 H51B 109.0 . . ? H51A C51 H51B 107.8 . . ? C51 C52 H52A 109.5 . . ? C51 C52 H52B 109.5 . . ? H52A C52 H52B 109.5 . . ? C51 C52 H52C 109.5 . . ? H52A C52 H52C 109.5 . . ? H52B C52 H52C 109.5 . . ? C54 C53 N5 115.6(7) . . ? C54 C53 H53A 108.4 . . ? N5 C53 H53A 108.4 . . ? C54 C53 H53B 108.4 . . ? N5 C53 H53B 108.4 . . ? H53A C53 H53B 107.4 . . ? C55 C54 C53 109.7(8) . . ? C55 C54 H54A 109.7 . . ? C53 C54 H54A 109.7 . . ? C55 C54 H54B 109.7 . . ? C53 C54 H54B 109.7 . . ? H54A C54 H54B 108.2 . . ? C54 C55 C56 113.7(10) . . ? C54 C55 H55A 108.8 . . ? C56 C55 H55A 108.8 . . ? C54 C55 H55B 108.8 . . ? C56 C55 H55B 108.8 . . ? H55A C55 H55B 107.7 . . ? C55 C56 H56A 109.5 . . ? C55 C56 H56B 109.5 . . ? H56A C56 H56B 109.5 . . ? C55 C56 H56C 109.5 . . ? H56A C56 H56C 109.5 . . ? H56B C56 H56C 109.5 . . ? C58 C57 N5 114.5(8) . . ? C58 C57 H57A 108.6 . . ? N5 C57 H57A 108.6 . . ? C58 C57 H57B 108.6 . . ? N5 C57 H57B 108.6 . . ? H57A C57 H57B 107.6 . . ? C57 C58 C59 113.1(8) . . ? C57 C58 H58A 109.0 . . ? C59 C58 H58A 109.0 . . ? C57 C58 H58B 109.0 . . ? C59 C58 H58B 109.0 . . ? H58A C58 H58B 107.8 . . ? C58 C59 C60 99.9(9) . . ? C58 C59 H59A 111.8 . . ? C60 C59 H59A 111.8 . . ? C58 C59 H59B 111.8 . . ? C60 C59 H59B 111.8 . . ? H59A C59 H59B 109.5 . . ? C59 C60 H60A 109.5 . . ? C59 C60 H60B 109.5 . . ? H60A C60 H60B 109.5 . . ? C59 C60 H60C 109.5 . . ? H60A C60 H60C 109.5 . . ? H60B C60 H60C 109.5 . . ? C62 C61 N6 119.7(11) . . ? C62 C61 H61A 107.4 . . ? N6 C61 H61A 107.4 . . ? C62 C61 H61B 107.4 . . ? N6 C61 H61B 107.4 . . ? H61A C61 H61B 106.9 . . ? C61 C62 C63 115.2(13) . . ? C61 C62 H62A 108.5 . . ? C63 C62 H62A 108.5 . . ? C61 C62 H62B 108.5 . . ? C63 C62 H62B 108.5 . . ? H62A C62 H62B 107.5 . . ? C62 C63 C64 118.9(16) . . ? C62 C63 H63A 107.6 . . ? C64 C63 H63A 107.6 . . ? C62 C63 H63B 107.6 . . ? C64 C63 H63B 107.6 . . ? H63A C63 H63B 107.0 . . ? C63 C64 H64A 109.5 . . ? C63 C64 H64B 109.5 . . ? H64A C64 H64B 109.5 . . ? C63 C64 H64C 109.5 . . ? H64A C64 H64C 109.5 . . ? H64B C64 H64C 109.5 . . ? C66 C65 N6 118.7(10) . . ? C66 C65 H65A 107.6 . . ? N6 C65 H65A 107.6 . . ? C66 C65 H65B 107.6 . . ? N6 C65 H65B 107.6 . . ? H65A C65 H65B 107.1 . . ? C67 C66 C65 118.7(15) . . ? C67 C66 H66A 107.6 . . ? C65 C66 H66A 107.6 . . ? C67 C66 H66B 107.6 . . ? C65 C66 H66B 107.6 . . ? H66A C66 H66B 107.1 . . ? C66 C67 C68 123.9(15) . . ? C66 C67 H67A 106.4 . . ? C68 C67 H67A 106.4 . . ? C66 C67 H67B 106.4 . . ? C68 C67 H67B 106.4 . . ? H67A C67 H67B 106.4 . . ? C67 C68 H68A 109.5 . . ? C67 C68 H68B 109.5 . . ? H68A C68 H68B 109.5 . . ? C67 C68 H68C 109.5 . . ? H68A C68 H68C 109.5 . . ? H68B C68 H68C 109.5 . . ? C70 C69 N6 117.3(9) . . ? C70 C69 H69A 108.0 . . ? N6 C69 H69A 108.0 . . ? C70 C69 H69B 108.0 . . ? N6 C69 H69B 108.0 . . ? H69A C69 H69B 107.2 . . ? C69 C70 C7 113.4(10) . . ? C69 C70 H70A 108.9 . . ? C7 C70 H70A 108.9 . . ? C69 C70 H70B 108.9 . . ? C7 C70 H70B 108.9 . . ? H70A C70 H70B 107.7 . . ? _diffrn_measured_fraction_theta_max 0.988 _diffrn_reflns_theta_full 25.00 _diffrn_measured_fraction_theta_full 0.988 _refine_diff_density_max 1.748 _refine_diff_density_min -2.082 _refine_diff_density_rms 0.120 #===END data_compound-5 _database_code_depnum_ccdc_archive 'CCDC 688716' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C36 H81 Mo6 N3 O18' _chemical_formula_weight 1419.68 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' Mo Mo -1.6832 0.6857 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting orthorhombic _symmetry_space_group_name_H-M Pbca loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x+1/2, -y, z+1/2' '-x, y+1/2, -z+1/2' 'x+1/2, -y+1/2, -z' '-x, -y, -z' 'x-1/2, y, -z-1/2' 'x, -y-1/2, z-1/2' '-x-1/2, y-1/2, z' _cell_length_a 16.8504(8) _cell_length_b 20.0036(10) _cell_length_c 31.6503(15) _cell_angle_alpha 90.00 _cell_angle_beta 90.00 _cell_angle_gamma 90.00 _cell_volume 10668.3(9) _cell_formula_units_Z 8 _cell_measurement_temperature 296(2) _cell_measurement_reflns_used 8234 _cell_measurement_theta_min 2.14 _cell_measurement_theta_max 28.64 _exptl_crystal_description block _exptl_crystal_colour orange _exptl_crystal_size_max 0.30 _exptl_crystal_size_mid 0.20 _exptl_crystal_size_min 0.20 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.768 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 5712 _exptl_absorpt_coefficient_mu 1.433 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.6731 _exptl_absorpt_correction_T_max 0.7626 _exptl_absorpt_process_details ? _exptl_special_details ; ? ; _diffrn_ambient_temperature 296(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 'CCD area detector' _diffrn_measurement_method 'phi and omega scans' _diffrn_detector_area_resol_mean ? _diffrn_reflns_number 48987 _diffrn_reflns_av_R_equivalents 0.0327 _diffrn_reflns_av_sigmaI/netI 0.0247 _diffrn_reflns_limit_h_min -20 _diffrn_reflns_limit_h_max 19 _diffrn_reflns_limit_k_min -23 _diffrn_reflns_limit_k_max 9 _diffrn_reflns_limit_l_min -37 _diffrn_reflns_limit_l_max 37 _diffrn_reflns_theta_min 2.04 _diffrn_reflns_theta_max 25.00 _reflns_number_total 9378 _reflns_number_gt 7120 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'Bruker SMART' _computing_cell_refinement 'Bruker SMART' _computing_data_reduction 'Bruker SAINT' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _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^)+(0.0449P)^2^+46.6940P] 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 9378 _refine_ls_number_parameters 590 _refine_ls_number_restraints 153 _refine_ls_R_factor_all 0.0736 _refine_ls_R_factor_gt 0.0509 _refine_ls_wR_factor_ref 0.1351 _refine_ls_wR_factor_gt 0.1175 _refine_ls_goodness_of_fit_ref 1.127 _refine_ls_restrained_S_all 1.140 _refine_ls_shift/su_max 0.003 _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 Mo1 Mo 0.51581(4) 0.18930(3) 0.17127(2) 0.0608(2) Uani 1 1 d . A . Mo2 Mo 0.36474(4) 0.09495(3) 0.19277(2) 0.05133(17) Uani 1 1 d . . . Mo3 Mo 0.26662(4) 0.16773(3) 0.11565(2) 0.05366(18) Uani 1 1 d . . . Mo4 Mo 0.42077(4) 0.26305(3) 0.09546(2) 0.05849(19) Uani 1 1 d . . . Mo5 Mo 0.34624(4) 0.25843(3) 0.19136(2) 0.05156(17) Uani 1 1 d . . . Mo6 Mo 0.44000(4) 0.09849(3) 0.09690(2) 0.05901(19) Uani 1 1 d . . . O1 O 0.3942(2) 0.1792(2) 0.14431(13) 0.0432(10) Uani 1 1 d . . . O2 O 0.3430(4) 0.0350(3) 0.22860(17) 0.0750(16) Uani 1 1 d . . . O3 O 0.1740(3) 0.1600(3) 0.0963(2) 0.0803(17) Uani 1 1 d . . . O4 O 0.4391(4) 0.3221(3) 0.0590(2) 0.091(2) Uani 1 1 d . . . O5 O 0.3124(4) 0.3165(3) 0.22527(19) 0.0767(16) Uani 1 1 d . . . O6 O 0.4716(4) 0.0400(3) 0.06242(19) 0.0821(17) Uani 1 1 d . . . O7 O 0.5164(3) 0.2557(3) 0.12576(18) 0.0654(14) Uani 1 1 d . . . O8 O 0.4565(3) 0.2541(2) 0.20416(16) 0.0600(13) Uani 1 1 d . . . O9 O 0.5327(3) 0.1217(3) 0.12722(18) 0.0672(14) Uani 1 1 d . . . O10 O 0.4715(3) 0.1195(2) 0.20645(16) 0.0609(13) Uani 1 1 d . . . O11 O 0.3333(3) 0.1765(2) 0.22166(15) 0.0575(12) Uani 1 1 d . . . O12 O 0.2687(3) 0.1028(2) 0.16122(15) 0.0539(12) Uani 1 1 d . . . O13 O 0.4079(3) 0.0466(2) 0.14560(15) 0.0561(12) Uani 1 1 d . . . O14 O 0.3266(3) 0.1048(2) 0.08430(16) 0.0618(13) Uani 1 1 d . . . O15 O 0.4503(3) 0.1812(3) 0.06597(16) 0.0672(14) Uani 1 1 d . . . O16 O 0.3764(3) 0.3113(2) 0.14198(16) 0.0581(12) Uani 1 1 d . . . O17 O 0.3120(3) 0.2366(3) 0.08200(16) 0.0658(14) Uani 1 1 d . . . O18 O 0.2538(3) 0.2337(2) 0.15957(16) 0.0582(12) Uani 1 1 d . . . N1 N 0.6098(4) 0.1971(4) 0.1919(3) 0.082(2) Uani 1 1 d . . . N2 N 0.4274(4) 0.5113(3) 0.1995(2) 0.0649(17) Uani 1 1 d . . . N3 N 0.6134(4) 0.1664(4) -0.0301(2) 0.081(2) Uani 1 1 d . . . C5 C 0.4241(5) 0.5875(4) 0.2065(3) 0.073(2) Uani 1 1 d D . . H5A H 0.3730 0.6030 0.1963 0.088 Uiso 1 1 calc R . . H5B H 0.4252 0.5954 0.2367 0.088 Uiso 1 1 calc R . . C6 C 0.4855(6) 0.6298(4) 0.1872(3) 0.086(3) Uani 1 1 d D . . H6A H 0.4885 0.6208 0.1571 0.103 Uiso 1 1 calc R . . H6B H 0.5367 0.6196 0.1996 0.103 Uiso 1 1 calc R . . C7 C 0.4655(6) 0.7046(4) 0.1945(3) 0.095(3) Uani 1 1 d D . . H7A H 0.4175 0.7156 0.1790 0.114 Uiso 1 1 calc R . . H7B H 0.4552 0.7118 0.2243 0.114 Uiso 1 1 calc R . . C8 C 0.5291(8) 0.7489(5) 0.1809(4) 0.124(4) Uani 1 1 d D . . H8A H 0.5141 0.7944 0.1862 0.186 Uiso 1 1 calc R . . H8B H 0.5386 0.7428 0.1513 0.186 Uiso 1 1 calc R . . H8C H 0.5766 0.7386 0.1964 0.186 Uiso 1 1 calc R . . C9 C 0.3877(5) 0.4937(4) 0.1575(3) 0.073(2) Uani 1 1 d . . . H9A H 0.3809 0.4456 0.1566 0.088 Uiso 1 1 calc R . . H9B H 0.3350 0.5133 0.1576 0.088 Uiso 1 1 calc R . . C10 C 0.4281(6) 0.5146(6) 0.1172(3) 0.096(3) Uani 1 1 d . . . H10A H 0.4813 0.4962 0.1163 0.116 Uiso 1 1 calc R . . H10B H 0.4323 0.5630 0.1163 0.116 Uiso 1 1 calc R . . C11 C 0.3809(7) 0.4900(6) 0.0791(3) 0.109(4) Uani 1 1 d . . . H11A H 0.3753 0.4419 0.0810 0.131 Uiso 1 1 calc R . . H11B H 0.3282 0.5094 0.0800 0.131 Uiso 1 1 calc R . . C12 C 0.4173(10) 0.5066(8) 0.0391(4) 0.164(6) Uani 1 1 d . . . H12A H 0.3852 0.4896 0.0165 0.246 Uiso 1 1 calc R . . H12B H 0.4692 0.4870 0.0377 0.246 Uiso 1 1 calc R . . H12C H 0.4216 0.5543 0.0366 0.246 Uiso 1 1 calc R . . C13 C 0.5120(5) 0.4852(4) 0.2007(3) 0.074(2) Uani 1 1 d DU . . H13A H 0.5421 0.5071 0.1786 0.089 Uiso 1 1 calc R . . H13B H 0.5356 0.4979 0.2275 0.089 Uiso 1 1 calc R . . C14 C 0.5204(6) 0.4105(4) 0.1955(4) 0.120(4) Uani 1 1 d DU . . H14A H 0.4888 0.3959 0.1715 0.144 Uiso 1 1 calc R . . H14B H 0.5005 0.3882 0.2205 0.144 Uiso 1 1 calc R . . C15 C 0.6099(6) 0.3903(6) 0.1881(6) 0.189(8) Uani 1 1 d DU . . H15A H 0.6147 0.3516 0.1698 0.227 Uiso 1 1 calc R . . H15B H 0.6407 0.4270 0.1766 0.227 Uiso 1 1 calc R . . C16 C 0.6327(11) 0.3751(11) 0.2310(6) 0.267(11) Uani 1 1 d DU . . H16A H 0.6879 0.3633 0.2317 0.400 Uiso 1 1 calc R . . H16B H 0.6015 0.3383 0.2412 0.400 Uiso 1 1 calc R . . H16C H 0.6238 0.4135 0.2485 0.400 Uiso 1 1 calc R . . C17 C 0.3768(5) 0.4794(4) 0.2329(3) 0.076(2) Uani 1 1 d . . . H17A H 0.3683 0.4330 0.2252 0.091 Uiso 1 1 calc R . . H17B H 0.3254 0.5012 0.2328 0.091 Uiso 1 1 calc R . . C18 C 0.4088(6) 0.4812(5) 0.2775(3) 0.091(3) Uani 1 1 d . . . H18A H 0.4620 0.4626 0.2780 0.109 Uiso 1 1 calc R . . H18B H 0.4117 0.5271 0.2872 0.109 Uiso 1 1 calc R . . C19 C 0.3567(7) 0.4421(6) 0.3062(3) 0.108(4) Uani 1 1 d . . . H19A H 0.3537 0.3964 0.2961 0.129 Uiso 1 1 calc R . . H19B H 0.3036 0.4607 0.3053 0.129 Uiso 1 1 calc R . . C20 C 0.3848(8) 0.4416(7) 0.3512(4) 0.135(5) Uani 1 1 d . . . H20A H 0.3486 0.4161 0.3682 0.203 Uiso 1 1 calc R . . H20B H 0.3872 0.4866 0.3616 0.203 Uiso 1 1 calc R . . H20C H 0.4366 0.4218 0.3526 0.203 Uiso 1 1 calc R . . C21 C 0.5277(6) 0.1875(6) -0.0302(3) 0.092(3) Uani 1 1 d . . . H21A H 0.4983 0.1559 -0.0474 0.111 Uiso 1 1 calc R . . H21B H 0.5077 0.1838 -0.0015 0.111 Uiso 1 1 calc R . . C22 C 0.5097(6) 0.2560(7) -0.0457(4) 0.107(4) Uani 1 1 d . . . H22A H 0.5307 0.2616 -0.0740 0.129 Uiso 1 1 calc R . . H22B H 0.5346 0.2888 -0.0275 0.129 Uiso 1 1 calc R . . C23 C 0.4207(7) 0.2663(9) -0.0460(4) 0.134(5) Uani 1 1 d . . . H23A H 0.3971 0.2380 -0.0675 0.160 Uiso 1 1 calc R . . H23B H 0.3990 0.2532 -0.0188 0.160 Uiso 1 1 calc R . . C24 C 0.4001(9) 0.3363(10) -0.0545(5) 0.182(8) Uani 1 1 d . . . H24A H 0.3434 0.3412 -0.0545 0.273 Uiso 1 1 calc R . . H24B H 0.4207 0.3492 -0.0816 0.273 Uiso 1 1 calc R . . H24C H 0.4226 0.3644 -0.0330 0.273 Uiso 1 1 calc R . . C25 C 0.6647(5) 0.2175(5) -0.0086(3) 0.082(3) Uani 1 1 d DU . . H25A H 0.7196 0.2031 -0.0106 0.099 Uiso 1 1 calc R . . H25B H 0.6602 0.2593 -0.0239 0.099 Uiso 1 1 calc R . . C26 C 0.6460(6) 0.2305(6) 0.0370(3) 0.115(4) Uani 1 1 d DU . . H26A H 0.6575 0.1907 0.0533 0.138 Uiso 1 1 calc R . . H26B H 0.5897 0.2398 0.0398 0.138 Uiso 1 1 calc R . . C27 C 0.6928(8) 0.2888(8) 0.0550(5) 0.160(6) Uani 1 1 d DU . . H27A H 0.6967 0.2840 0.0854 0.192 Uiso 1 1 calc R . . H27B H 0.7461 0.2882 0.0435 0.192 Uiso 1 1 calc R . . C28 C 0.6561(12) 0.3507(8) 0.0452(8) 0.253(12) Uani 1 1 d DU . . H28A H 0.6890 0.3867 0.0550 0.379 Uiso 1 1 calc R . . H28B H 0.6053 0.3530 0.0588 0.379 Uiso 1 1 calc R . . H28C H 0.6494 0.3543 0.0152 0.379 Uiso 1 1 calc R . . C29 C 0.6448(6) 0.1622(5) -0.0750(3) 0.091(3) Uani 1 1 d . . . H29A H 0.6469 0.2070 -0.0868 0.109 Uiso 1 1 calc R . . H29B H 0.6986 0.1450 -0.0743 0.109 Uiso 1 1 calc R . . C30 C 0.5957(8) 0.1186(6) -0.1039(3) 0.114(4) Uani 1 1 d . . . H30A H 0.5415 0.1348 -0.1043 0.137 Uiso 1 1 calc R . . H30B H 0.5952 0.0733 -0.0930 0.137 Uiso 1 1 calc R . . C31 C 0.6307(7) 0.1184(6) -0.1515(4) 0.106(4) Uani 1 1 d . . . H31A H 0.5960 0.0936 -0.1703 0.127 Uiso 1 1 calc R . . H31B H 0.6359 0.1637 -0.1621 0.127 Uiso 1 1 calc R . . C32 C 0.7031(7) 0.0884(5) -0.1488(4) 0.103(3) Uani 1 1 d . . . H32A H 0.7273 0.0875 -0.1762 0.154 Uiso 1 1 calc R . . H32B H 0.6967 0.0435 -0.1387 0.154 Uiso 1 1 calc R . . H32C H 0.7362 0.1130 -0.1296 0.154 Uiso 1 1 calc R . . C33 C 0.6180(6) 0.0984(5) -0.0074(3) 0.099(3) Uani 1 1 d DU . . H33A H 0.5986 0.1045 0.0212 0.119 Uiso 1 1 calc R . . H33B H 0.5817 0.0681 -0.0215 0.119 Uiso 1 1 calc R . . C34 C 0.6968(8) 0.0652(7) -0.0049(5) 0.145(5) Uani 1 1 d DU . . H34A H 0.7372 0.0987 0.0004 0.175 Uiso 1 1 calc R . . H34B H 0.7085 0.0443 -0.0318 0.175 Uiso 1 1 calc R . . C35 C 0.7003(10) 0.0116(8) 0.0303(6) 0.192(7) Uani 1 1 d DU . . H35A H 0.7549 -0.0031 0.0330 0.231 Uiso 1 1 calc R . . H35B H 0.6856 0.0327 0.0568 0.231 Uiso 1 1 calc R . . C36 C 0.6533(11) -0.0442(8) 0.0251(6) 0.189(7) Uani 1 1 d DU . . H36A H 0.6580 -0.0724 0.0495 0.283 Uiso 1 1 calc R . . H36B H 0.6701 -0.0682 0.0004 0.283 Uiso 1 1 calc R . . H36C H 0.5990 -0.0307 0.0218 0.283 Uiso 1 1 calc R . . C1A C 0.6890(6) 0.2019(6) 0.2084(5) 0.118(4) Uani 0.50 1 d PDU A 1 H1A1 H 0.6880 0.1977 0.2389 0.141 Uiso 0.50 1 calc PR A 1 H1A2 H 0.7116 0.2451 0.2013 0.141 Uiso 0.50 1 calc PR A 1 C2A C 0.7395(11) 0.1462(13) 0.1894(6) 0.116(7) Uani 0.50 1 d PDU A 1 H2A1 H 0.7939 0.1577 0.1963 0.140 Uiso 0.50 1 calc PR A 1 H2A2 H 0.7271 0.1066 0.2058 0.140 Uiso 0.50 1 calc PR A 1 C3A C 0.7414(12) 0.1243(14) 0.1458(6) 0.113(7) Uani 0.50 1 d PDU A 1 H3A1 H 0.7545 0.1624 0.1282 0.136 Uiso 0.50 1 calc PR A 1 H3A2 H 0.6886 0.1096 0.1379 0.136 Uiso 0.50 1 calc PR A 1 C4A C 0.7993(17) 0.0686(14) 0.1361(9) 0.140(6) Uani 0.50 1 d PDU A 1 H4A1 H 0.7977 0.0586 0.1064 0.211 Uiso 0.50 1 calc PR A 1 H4A2 H 0.7849 0.0294 0.1519 0.211 Uiso 0.50 1 calc PR A 1 H4A3 H 0.8519 0.0823 0.1439 0.211 Uiso 0.50 1 calc PR A 1 C1B C 0.6890(6) 0.2019(6) 0.2084(5) 0.118(4) Uani 0.50 1 d PDU A 2 H1B1 H 0.7025 0.1597 0.2217 0.141 Uiso 0.50 1 calc PR A 2 H1B2 H 0.6898 0.2361 0.2302 0.141 Uiso 0.50 1 calc PR A 2 C2B C 0.7492(14) 0.2175(13) 0.1776(8) 0.132(7) Uani 0.50 1 d PDU A 2 H2B1 H 0.7988 0.2254 0.1923 0.159 Uiso 0.50 1 calc PR A 2 H2B2 H 0.7346 0.2588 0.1636 0.159 Uiso 0.50 1 calc PR A 2 C3B C 0.7625(19) 0.1655(15) 0.1451(8) 0.152(10) Uani 0.50 1 d PDU A 2 H3B1 H 0.8076 0.1772 0.1275 0.183 Uiso 0.50 1 calc PR A 2 H3B2 H 0.7160 0.1611 0.1272 0.183 Uiso 0.50 1 calc PR A 2 C4B C 0.7784(19) 0.1007(14) 0.1685(9) 0.140(6) Uani 0.50 1 d PDU A 2 H4B1 H 0.7846 0.0650 0.1485 0.211 Uiso 0.50 1 calc PR A 2 H4B2 H 0.7346 0.0910 0.1869 0.211 Uiso 0.50 1 calc PR A 2 H4B3 H 0.8260 0.1050 0.1849 0.211 Uiso 0.50 1 calc PR 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 Mo1 0.0362(3) 0.0611(4) 0.0851(5) -0.0011(4) -0.0086(3) -0.0026(3) Mo2 0.0527(4) 0.0434(3) 0.0578(4) 0.0103(3) -0.0003(3) -0.0012(3) Mo3 0.0428(3) 0.0530(4) 0.0652(4) 0.0034(3) -0.0108(3) -0.0025(3) Mo4 0.0650(4) 0.0484(4) 0.0621(4) 0.0106(3) 0.0109(3) -0.0067(3) Mo5 0.0513(4) 0.0435(3) 0.0599(4) -0.0052(3) 0.0046(3) 0.0007(3) Mo6 0.0613(4) 0.0493(4) 0.0664(4) -0.0081(3) 0.0149(3) 0.0011(3) O1 0.037(2) 0.040(2) 0.052(2) 0.002(2) 0.0041(19) -0.0019(18) O2 0.096(4) 0.057(3) 0.072(3) 0.022(3) 0.005(3) -0.005(3) O3 0.055(3) 0.080(4) 0.106(4) 0.001(3) -0.030(3) -0.009(3) O4 0.119(5) 0.067(4) 0.087(4) 0.024(3) 0.020(4) -0.014(4) O5 0.083(4) 0.056(3) 0.092(4) -0.019(3) 0.017(3) 0.006(3) O6 0.090(4) 0.067(4) 0.089(4) -0.021(3) 0.026(3) 0.003(3) O7 0.047(3) 0.061(3) 0.089(4) 0.000(3) 0.010(3) -0.016(2) O8 0.054(3) 0.055(3) 0.071(3) -0.006(3) -0.011(2) -0.007(2) O9 0.041(3) 0.063(3) 0.098(4) -0.010(3) 0.007(3) 0.005(2) O10 0.054(3) 0.057(3) 0.072(3) 0.007(3) -0.016(2) 0.003(2) O11 0.065(3) 0.053(3) 0.055(3) 0.005(2) 0.006(2) -0.002(2) O12 0.041(3) 0.048(3) 0.073(3) 0.004(2) -0.002(2) -0.011(2) O13 0.055(3) 0.041(2) 0.072(3) -0.004(2) 0.001(2) 0.003(2) O14 0.063(3) 0.060(3) 0.063(3) -0.009(3) -0.005(2) -0.008(3) O15 0.079(4) 0.066(3) 0.057(3) -0.001(3) 0.019(3) -0.008(3) O16 0.058(3) 0.043(3) 0.074(3) 0.006(2) 0.001(3) 0.001(2) O17 0.066(3) 0.064(3) 0.067(3) 0.018(3) -0.017(3) -0.005(3) O18 0.044(3) 0.051(3) 0.079(3) -0.003(3) 0.000(2) 0.006(2) N1 0.042(4) 0.075(5) 0.129(6) -0.006(4) -0.021(4) 0.003(3) N2 0.067(4) 0.049(4) 0.079(4) -0.010(3) -0.021(3) 0.001(3) N3 0.073(5) 0.106(6) 0.063(4) 0.001(4) 0.017(4) -0.027(4) C5 0.079(6) 0.062(5) 0.078(6) -0.007(4) -0.009(5) -0.006(4) C6 0.100(7) 0.077(6) 0.081(6) -0.017(5) 0.001(5) -0.004(6) C7 0.116(8) 0.053(5) 0.115(8) -0.001(5) -0.045(7) -0.001(5) C8 0.167(12) 0.073(7) 0.131(10) 0.017(7) -0.019(9) -0.013(8) C9 0.071(5) 0.062(5) 0.087(6) -0.017(5) -0.018(5) 0.009(4) C10 0.097(7) 0.103(8) 0.090(7) -0.028(6) -0.023(6) 0.009(6) C11 0.137(10) 0.110(8) 0.081(7) -0.029(6) -0.030(7) 0.023(7) C12 0.216(17) 0.202(16) 0.074(8) -0.024(9) -0.011(9) -0.024(14) C13 0.059(5) 0.062(5) 0.101(6) -0.003(5) -0.018(4) -0.009(4) C14 0.090(7) 0.064(5) 0.205(12) -0.010(7) -0.033(7) 0.007(5) C15 0.093(7) 0.084(8) 0.39(2) -0.043(11) -0.127(11) 0.033(6) C16 0.184(19) 0.21(2) 0.41(3) -0.02(2) -0.13(2) 0.054(16) C17 0.072(6) 0.059(5) 0.095(6) -0.005(5) -0.015(5) -0.015(4) C18 0.086(7) 0.096(7) 0.091(7) 0.010(6) -0.019(5) -0.018(6) C19 0.108(9) 0.109(9) 0.105(8) 0.000(7) 0.006(7) -0.031(7) C20 0.160(13) 0.155(12) 0.091(9) 0.013(8) 0.008(8) -0.007(10) C21 0.069(6) 0.140(10) 0.068(6) 0.008(6) 0.010(5) -0.030(6) C22 0.074(7) 0.147(11) 0.101(8) -0.002(8) 0.003(6) -0.013(7) C23 0.090(9) 0.200(16) 0.111(10) 0.011(10) -0.022(7) 0.009(10) C24 0.119(12) 0.28(2) 0.149(14) -0.002(15) -0.030(10) 0.035(14) C25 0.057(5) 0.111(7) 0.079(5) -0.006(5) 0.010(4) -0.016(5) C26 0.087(7) 0.167(10) 0.091(6) -0.030(7) 0.001(6) -0.006(7) C27 0.110(10) 0.209(14) 0.161(12) -0.099(11) -0.010(9) 0.001(9) C28 0.20(2) 0.158(11) 0.40(3) -0.013(19) 0.05(2) -0.042(13) C29 0.100(7) 0.089(7) 0.083(6) -0.018(5) 0.035(5) -0.037(6) C30 0.129(10) 0.120(9) 0.093(8) -0.007(7) 0.034(7) -0.032(8) C31 0.091(8) 0.084(7) 0.143(10) -0.014(7) 0.003(7) -0.007(6) C32 0.106(9) 0.093(7) 0.109(8) -0.006(6) 0.009(7) -0.030(7) C33 0.101(7) 0.110(8) 0.086(7) 0.006(6) 0.020(6) -0.029(6) C34 0.131(9) 0.139(10) 0.167(12) 0.011(8) 0.028(10) 0.014(8) C35 0.171(15) 0.139(13) 0.267(19) 0.057(12) -0.012(14) 0.004(10) C36 0.21(2) 0.164(14) 0.192(16) 0.033(13) -0.010(14) -0.011(12) C1A 0.049(5) 0.124(9) 0.179(11) -0.004(8) -0.030(6) -0.010(5) C2A 0.036(9) 0.21(2) 0.101(11) 0.008(12) -0.009(9) 0.023(11) C3A 0.052(11) 0.19(2) 0.096(11) 0.030(13) -0.011(10) -0.004(12) C4A 0.131(16) 0.175(16) 0.115(15) 0.005(12) 0.003(13) 0.009(12) C1B 0.049(5) 0.124(9) 0.179(11) -0.004(8) -0.030(6) -0.010(5) C2B 0.089(14) 0.162(16) 0.146(18) 0.038(14) -0.029(11) -0.005(15) C3B 0.12(2) 0.19(2) 0.15(2) 0.025(13) -0.004(16) -0.02(2) C4B 0.131(16) 0.175(16) 0.115(15) 0.005(12) 0.003(13) 0.009(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 Mo1 N1 1.721(6) . ? Mo1 O10 1.936(5) . ? Mo1 O8 1.940(5) . ? Mo1 O7 1.960(5) . ? Mo1 O9 1.962(5) . ? Mo1 O1 2.228(4) . ? Mo2 O2 1.691(5) . ? Mo2 O12 1.909(5) . ? Mo2 O10 1.914(5) . ? Mo2 O13 1.922(5) . ? Mo2 O11 1.944(5) . ? Mo2 O1 2.332(4) . ? Mo3 O3 1.684(5) . ? Mo3 O14 1.896(5) . ? Mo3 O17 1.902(5) . ? Mo3 O18 1.929(5) . ? Mo3 O12 1.941(5) . ? Mo3 O1 2.345(4) . ? Mo4 O4 1.680(5) . ? Mo4 O7 1.881(5) . ? Mo4 O16 1.913(5) . ? Mo4 O15 1.950(5) . ? Mo4 O17 1.954(5) . ? Mo4 O1 2.325(4) . ? Mo5 O5 1.681(5) . ? Mo5 O8 1.903(5) . ? Mo5 O11 1.911(5) . ? Mo5 O18 1.920(5) . ? Mo5 O16 1.954(5) . ? Mo5 O1 2.321(4) . ? Mo6 O6 1.686(5) . ? Mo6 O9 1.891(5) . ? Mo6 O15 1.930(5) . ? Mo6 O13 1.935(5) . ? Mo6 O14 1.956(5) . ? Mo6 O1 2.335(4) . ? N1 C1A 1.436(11) . ? N2 C17 1.501(10) . ? N2 C13 1.518(10) . ? N2 C9 1.529(10) . ? N2 C5 1.542(9) . ? N3 C25 1.502(11) . ? N3 C21 1.505(12) . ? N3 C29 1.520(10) . ? N3 C33 1.538(12) . ? C5 C6 1.471(10) . ? C6 C7 1.550(10) . ? C7 C8 1.455(12) . ? C9 C10 1.506(13) . ? C10 C11 1.526(12) . ? C11 C12 1.444(16) . ? C13 C14 1.509(10) . ? C14 C15 1.579(11) . ? C15 C16 1.441(13) . ? C17 C18 1.512(12) . ? C18 C19 1.487(13) . ? C19 C20 1.499(14) . ? C21 C22 1.487(15) . ? C22 C23 1.514(15) . ? C23 C24 1.47(2) . ? C25 C26 1.500(10) . ? C26 C27 1.517(12) . ? C27 C28 1.418(12) . ? C29 C30 1.509(14) . ? C30 C31 1.618(15) . ? C31 C32 1.362(14) . ? C33 C34 1.487(12) . ? C34 C35 1.547(13) . ? C35 C36 1.377(14) . ? C1A C2A 1.52(2) . ? C2A C3A 1.45(2) . ? C3A C4A 1.51(3) . ? C2B C3B 1.48(3) . ? C3B C4B 1.52(3) . ? 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 N1 Mo1 O10 101.7(3) . . ? N1 Mo1 O8 102.2(3) . . ? O10 Mo1 O8 88.6(2) . . ? N1 Mo1 O7 102.3(3) . . ? O10 Mo1 O7 156.1(2) . . ? O8 Mo1 O7 86.8(2) . . ? N1 Mo1 O9 101.4(3) . . ? O10 Mo1 O9 88.2(2) . . ? O8 Mo1 O9 156.4(2) . . ? O7 Mo1 O9 86.8(2) . . ? N1 Mo1 O1 179.8(3) . . ? O10 Mo1 O1 78.46(17) . . ? O8 Mo1 O1 78.02(17) . . ? O7 Mo1 O1 77.59(17) . . ? O9 Mo1 O1 78.38(18) . . ? O2 Mo2 O12 103.1(2) . . ? O2 Mo2 O10 103.5(3) . . ? O12 Mo2 O10 153.4(2) . . ? O2 Mo2 O13 104.2(2) . . ? O12 Mo2 O13 87.5(2) . . ? O10 Mo2 O13 87.1(2) . . ? O2 Mo2 O11 102.8(2) . . ? O12 Mo2 O11 86.9(2) . . ? O10 Mo2 O11 86.3(2) . . ? O13 Mo2 O11 153.0(2) . . ? O2 Mo2 O1 178.9(2) . . ? O12 Mo2 O1 77.10(17) . . ? O10 Mo2 O1 76.32(18) . . ? O13 Mo2 O1 76.79(17) . . ? O11 Mo2 O1 76.18(17) . . ? O3 Mo3 O14 104.1(3) . . ? O3 Mo3 O17 103.7(3) . . ? O14 Mo3 O17 88.5(2) . . ? O3 Mo3 O18 102.8(3) . . ? O14 Mo3 O18 153.1(2) . . ? O17 Mo3 O18 87.3(2) . . ? O3 Mo3 O12 103.0(2) . . ? O14 Mo3 O12 86.3(2) . . ? O17 Mo3 O12 153.3(2) . . ? O18 Mo3 O12 85.7(2) . . ? O3 Mo3 O1 178.5(3) . . ? O14 Mo3 O1 77.18(18) . . ? O17 Mo3 O1 77.12(18) . . ? O18 Mo3 O1 75.97(17) . . ? O12 Mo3 O1 76.19(16) . . ? O4 Mo4 O7 104.3(3) . . ? O4 Mo4 O16 104.2(3) . . ? O7 Mo4 O16 89.0(2) . . ? O4 Mo4 O15 102.5(3) . . ? O7 Mo4 O15 87.7(2) . . ? O16 Mo4 O15 153.2(2) . . ? O4 Mo4 O17 102.3(3) . . ? O7 Mo4 O17 153.3(2) . . ? O16 Mo4 O17 86.4(2) . . ? O15 Mo4 O17 84.7(2) . . ? O4 Mo4 O1 178.3(3) . . ? O7 Mo4 O1 76.68(18) . . ? O16 Mo4 O1 77.13(17) . . ? O15 Mo4 O1 76.18(18) . . ? O17 Mo4 O1 76.65(18) . . ? O5 Mo5 O8 103.1(3) . . ? O5 Mo5 O11 103.5(2) . . ? O8 Mo5 O11 88.0(2) . . ? O5 Mo5 O18 103.7(3) . . ? O8 Mo5 O18 153.2(2) . . ? O11 Mo5 O18 87.1(2) . . ? O5 Mo5 O16 103.0(2) . . ? O8 Mo5 O16 86.6(2) . . ? O11 Mo5 O16 153.5(2) . . ? O18 Mo5 O16 86.0(2) . . ? O5 Mo5 O1 179.3(2) . . ? O8 Mo5 O1 76.44(18) . . ? O11 Mo5 O1 77.06(18) . . ? O18 Mo5 O1 76.74(17) . . ? O16 Mo5 O1 76.48(17) . . ? O6 Mo6 O9 103.8(3) . . ? O6 Mo6 O15 103.7(3) . . ? O9 Mo6 O15 88.4(2) . . ? O6 Mo6 O13 103.4(2) . . ? O9 Mo6 O13 87.6(2) . . ? O15 Mo6 O13 152.7(2) . . ? O6 Mo6 O14 102.8(3) . . ? O9 Mo6 O14 153.4(2) . . ? O15 Mo6 O14 86.0(2) . . ? O13 Mo6 O14 85.7(2) . . ? O6 Mo6 O1 179.1(3) . . ? O9 Mo6 O1 77.10(18) . . ? O15 Mo6 O1 76.32(18) . . ? O13 Mo6 O1 76.49(17) . . ? O14 Mo6 O1 76.35(18) . . ? Mo1 O1 Mo5 90.71(15) . . ? Mo1 O1 Mo4 90.69(15) . . ? Mo5 O1 Mo4 90.03(14) . . ? Mo1 O1 Mo2 90.56(15) . . ? Mo5 O1 Mo2 89.85(14) . . ? Mo4 O1 Mo2 178.7(2) . . ? Mo1 O1 Mo6 90.30(15) . . ? Mo5 O1 Mo6 178.9(2) . . ? Mo4 O1 Mo6 90.45(14) . . ? Mo2 O1 Mo6 89.65(14) . . ? Mo1 O1 Mo3 179.5(2) . . ? Mo5 O1 Mo3 89.73(14) . . ? Mo4 O1 Mo3 89.39(15) . . ? Mo2 O1 Mo3 89.35(14) . . ? Mo6 O1 Mo3 89.25(14) . . ? Mo4 O7 Mo1 115.0(2) . . ? Mo5 O8 Mo1 114.8(2) . . ? Mo6 O9 Mo1 114.2(2) . . ? Mo2 O10 Mo1 114.7(2) . . ? Mo5 O11 Mo2 116.9(2) . . ? Mo2 O12 Mo3 117.3(2) . . ? Mo2 O13 Mo6 117.1(2) . . ? Mo3 O14 Mo6 117.2(2) . . ? Mo6 O15 Mo4 117.0(2) . . ? Mo4 O16 Mo5 116.3(2) . . ? Mo3 O17 Mo4 116.8(2) . . ? Mo5 O18 Mo3 117.6(2) . . ? C1A N1 Mo1 178.4(8) . . ? C17 N2 C13 111.7(6) . . ? C17 N2 C9 105.4(6) . . ? C13 N2 C9 110.7(6) . . ? C17 N2 C5 107.4(6) . . ? C13 N2 C5 111.7(6) . . ? C9 N2 C5 109.6(6) . . ? C25 N3 C21 111.2(8) . . ? C25 N3 C29 105.1(6) . . ? C21 N3 C29 110.3(7) . . ? C25 N3 C33 111.2(8) . . ? C21 N3 C33 107.3(7) . . ? C29 N3 C33 111.8(8) . . ? C6 C5 N2 119.0(7) . . ? C5 C6 C7 109.9(8) . . ? C8 C7 C6 112.5(9) . . ? C10 C9 N2 118.3(7) . . ? C9 C10 C11 110.2(9) . . ? C12 C11 C10 113.4(11) . . ? C14 C13 N2 115.2(7) . . ? C13 C14 C15 111.1(8) . . ? C16 C15 C14 99.8(12) . . ? N2 C17 C18 116.4(7) . . ? C19 C18 C17 110.3(8) . . ? C18 C19 C20 113.3(10) . . ? C22 C21 N3 117.1(8) . . ? C21 C22 C23 109.3(11) . . ? C24 C23 C22 111.5(14) . . ? C26 C25 N3 115.6(7) . . ? C25 C26 C27 112.6(10) . . ? C28 C27 C26 111.2(13) . . ? C30 C29 N3 114.0(7) . . ? C29 C30 C31 111.4(9) . . ? C32 C31 C30 105.6(11) . . ? C34 C33 N3 117.7(9) . . ? C33 C34 C35 112.5(11) . . ? C36 C35 C34 116.9(15) . . ? N1 C1A C2A 109.0(11) . . ? C3A C2A C1A 127.5(17) . . ? C2A C3A C4A 115.5(18) . . ? C2B C3B C4B 107(2) . . ? _diffrn_measured_fraction_theta_max 0.999 _diffrn_reflns_theta_full 25.00 _diffrn_measured_fraction_theta_full 0.999 _refine_diff_density_max 1.099 _refine_diff_density_min -0.766 _refine_diff_density_rms 0.105 #===END data_compound-6 _database_code_depnum_ccdc_archive 'CCDC 688717' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C37.50 H84 Mo6 N3 O18.50' _chemical_formula_weight 1448.72 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' Mo Mo -1.6832 0.6857 '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 2(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 17.3661(7) _cell_length_b 16.8920(7) _cell_length_c 19.8925(8) _cell_angle_alpha 90.00 _cell_angle_beta 105.4010(10) _cell_angle_gamma 90.00 _cell_volume 5625.9(4) _cell_formula_units_Z 4 _cell_measurement_temperature 296(2) _cell_measurement_reflns_used 9632 _cell_measurement_theta_min 2.41 _cell_measurement_theta_max 27.44 _exptl_crystal_description tabular _exptl_crystal_colour yellow _exptl_crystal_size_max 0.30 _exptl_crystal_size_mid 0.15 _exptl_crystal_size_min 0.05 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.710 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 2920 _exptl_absorpt_coefficient_mu 1.361 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.6856 _exptl_absorpt_correction_T_max 0.9351 _exptl_absorpt_process_details ? _exptl_special_details ; ? ; _diffrn_ambient_temperature 296(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 'CCD area detector' _diffrn_measurement_method 'phi and omega scans' _diffrn_detector_area_resol_mean ? _diffrn_reflns_number 31391 _diffrn_reflns_av_R_equivalents 0.0447 _diffrn_reflns_av_sigmaI/netI 0.0496 _diffrn_reflns_limit_h_min -15 _diffrn_reflns_limit_h_max 20 _diffrn_reflns_limit_k_min -19 _diffrn_reflns_limit_k_max 20 _diffrn_reflns_limit_l_min -23 _diffrn_reflns_limit_l_max 22 _diffrn_reflns_theta_min 2.12 _diffrn_reflns_theta_max 25.00 _reflns_number_total 9899 _reflns_number_gt 6601 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'Bruker SMART' _computing_cell_refinement 'Bruker SMART' _computing_data_reduction 'Bruker SAINT' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _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^)+(0.0895P)^2^+0.9718P] 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 9899 _refine_ls_number_parameters 575 _refine_ls_number_restraints 33 _refine_ls_R_factor_all 0.0922 _refine_ls_R_factor_gt 0.0595 _refine_ls_wR_factor_ref 0.1608 _refine_ls_wR_factor_gt 0.1431 _refine_ls_goodness_of_fit_ref 1.015 _refine_ls_restrained_S_all 1.017 _refine_ls_shift/su_max 0.003 _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 Mo6 Mo -0.02863(4) -0.16837(4) -0.35693(3) 0.05072(18) Uani 1 1 d . . . Mo2 Mo -0.13023(4) -0.28618(4) -0.28023(4) 0.0618(2) Uani 1 1 d . . . Mo4 Mo 0.11768(4) -0.29903(4) -0.32703(4) 0.0645(2) Uani 1 1 d . . . Mo3 Mo 0.05217(4) -0.23159(4) -0.19789(3) 0.0649(2) Uani 1 1 d . . . Mo5 Mo 0.01547(4) -0.41578(4) -0.25027(4) 0.0667(2) Uani 1 1 d . . . Mo1 Mo -0.06300(4) -0.35051(4) -0.40663(4) 0.0676(2) Uani 1 1 d . . . O1 O -0.0076(2) -0.2928(2) -0.3044(2) 0.0434(10) Uani 1 1 d . . . O2 O -0.2195(3) -0.2787(3) -0.2626(4) 0.0907(19) Uani 1 1 d . . . O3 O 0.0951(4) -0.1879(4) -0.1213(3) 0.102(2) Uani 1 1 d . . . O4 O 0.2084(3) -0.3082(3) -0.3415(4) 0.093(2) Uani 1 1 d . . . O5 O 0.0286(4) -0.5039(3) -0.2101(4) 0.099(2) Uani 1 1 d . . . O6 O -0.0400(3) -0.0778(3) -0.3949(3) 0.0704(14) Uani 1 1 d . . . O7 O -0.0669(3) -0.2378(3) -0.4322(2) 0.0616(13) Uani 1 1 d . . . O8 O -0.0379(3) -0.4415(3) -0.3440(3) 0.0728(15) Uani 1 1 d . . . O9 O -0.1551(3) -0.3313(3) -0.3704(3) 0.0686(14) Uani 1 1 d . . . O10 O 0.0500(3) -0.3495(3) -0.4046(3) 0.0738(15) Uani 1 1 d . . . O11 O -0.0921(3) -0.3849(3) -0.2423(3) 0.0668(14) Uani 1 1 d . . . O12 O -0.1225(3) -0.1848(3) -0.3281(3) 0.0610(13) Uani 1 1 d . . . O13 O -0.0577(4) -0.2348(3) -0.2009(3) 0.0770(16) Uani 1 1 d . . . O14 O 0.0254(3) -0.1450(2) -0.2610(2) 0.0586(12) Uani 1 1 d . . . O15 O 0.0544(3) -0.3433(3) -0.1753(3) 0.0721(15) Uani 1 1 d . . . O16 O 0.1410(3) -0.2531(3) -0.2362(3) 0.0673(14) Uani 1 1 d . . . O17 O 0.0794(3) -0.1987(3) -0.3633(3) 0.0579(12) Uani 1 1 d . . . O18 O 0.1108(3) -0.3997(3) -0.2771(3) 0.0734(15) Uani 1 1 d . . . N1 N -0.1053(5) -0.3933(5) -0.4862(4) 0.092(2) Uani 1 1 d . . . N2 N 0.1655(4) 0.0673(4) -0.3724(3) 0.0641(16) Uani 1 1 d . . . N3 N -0.2349(4) -0.0580(4) -0.1762(4) 0.083(2) Uani 1 1 d . . . C1 C -0.1389(7) -0.4309(7) -0.5521(5) 0.103(3) Uani 1 1 d . . . C2 C -0.2127(8) -0.3812(9) -0.5983(7) 0.182(8) Uani 1 1 d . . . H2A H -0.1948 -0.3293 -0.6070 0.274 Uiso 1 1 calc R . . H2B H -0.2532 -0.3766 -0.5737 0.274 Uiso 1 1 calc R . . H2C H -0.2344 -0.4078 -0.6418 0.274 Uiso 1 1 calc R . . C3 C -0.1698(7) -0.5084(6) -0.5422(6) 0.117(4) Uani 1 1 d . . . H3A H -0.2093 -0.5033 -0.5166 0.176 Uiso 1 1 calc R . . H3B H -0.1270 -0.5414 -0.5166 0.176 Uiso 1 1 calc R . . H3C H -0.1937 -0.5319 -0.5868 0.176 Uiso 1 1 calc R . . C4 C -0.0784(6) -0.4310(7) -0.5930(6) 0.116(4) Uani 1 1 d . . . H4A H -0.0616 -0.3777 -0.5980 0.174 Uiso 1 1 calc R . . H4B H -0.1015 -0.4533 -0.6383 0.174 Uiso 1 1 calc R . . H4C H -0.0332 -0.4622 -0.5691 0.174 Uiso 1 1 calc R . . C5 C 0.1856(5) -0.0185(5) -0.3794(5) 0.076(2) Uani 1 1 d . . . H5A H 0.1451 -0.0508 -0.3673 0.092 Uiso 1 1 calc R . . H5B H 0.1831 -0.0289 -0.4279 0.092 Uiso 1 1 calc R . . C6 C 0.2654(7) -0.0437(6) -0.3357(7) 0.117(4) Uani 1 1 d D . . H6A H 0.2680 -0.0345 -0.2869 0.140 Uiso 1 1 calc R . . H6B H 0.3063 -0.0116 -0.3474 0.140 Uiso 1 1 calc R . . C7 C 0.2816(7) -0.1288(6) -0.3458(9) 0.157(6) Uani 1 1 d D . . H7A H 0.2348 -0.1589 -0.3435 0.188 Uiso 1 1 calc R . . H7B H 0.2879 -0.1351 -0.3925 0.188 Uiso 1 1 calc R . . C8 C 0.3506(9) -0.1642(8) -0.2972(10) 0.185(8) Uani 1 1 d . . . H8A H 0.3553 -0.2185 -0.3098 0.277 Uiso 1 1 calc R . . H8B H 0.3442 -0.1615 -0.2508 0.277 Uiso 1 1 calc R . . H8C H 0.3979 -0.1359 -0.2991 0.277 Uiso 1 1 calc R . . C9 C 0.2233(5) 0.1231(5) -0.3946(4) 0.068(2) Uani 1 1 d . . . H9A H 0.2051 0.1770 -0.3919 0.082 Uiso 1 1 calc R . . H9B H 0.2753 0.1182 -0.3614 0.082 Uiso 1 1 calc R . . C10 C 0.2328(5) 0.1092(5) -0.4670(4) 0.075(2) Uani 1 1 d . . . H10A H 0.1811 0.1128 -0.5008 0.090 Uiso 1 1 calc R . . H10B H 0.2539 0.0565 -0.4698 0.090 Uiso 1 1 calc R . . C11 C 0.2889(6) 0.1699(6) -0.4842(5) 0.089(3) Uani 1 1 d . . . H11A H 0.2655 0.2221 -0.4841 0.106 Uiso 1 1 calc R . . H11B H 0.3387 0.1690 -0.4478 0.106 Uiso 1 1 calc R . . C12 C 0.3064(6) 0.1572(6) -0.5525(6) 0.103(3) Uani 1 1 d . . . H12A H 0.3416 0.1980 -0.5601 0.155 Uiso 1 1 calc R . . H12B H 0.2575 0.1588 -0.5890 0.155 Uiso 1 1 calc R . . H12C H 0.3314 0.1065 -0.5526 0.155 Uiso 1 1 calc R . . C13 C 0.1699(5) 0.0876(5) -0.2965(4) 0.069(2) Uani 1 1 d . . . H13A H 0.2242 0.0784 -0.2687 0.083 Uiso 1 1 calc R . . H13B H 0.1591 0.1437 -0.2939 0.083 Uiso 1 1 calc R . . C14 C 0.1142(5) 0.0425(5) -0.2641(4) 0.075(2) Uani 1 1 d . . . H14A H 0.0597 0.0499 -0.2920 0.090 Uiso 1 1 calc R . . H14B H 0.1265 -0.0135 -0.2638 0.090 Uiso 1 1 calc R . . C15 C 0.1213(6) 0.0696(6) -0.1915(5) 0.085(3) Uani 1 1 d . . . H15A H 0.1099 0.1259 -0.1925 0.102 Uiso 1 1 calc R . . H15B H 0.1761 0.0622 -0.1644 0.102 Uiso 1 1 calc R . . C16 C 0.0670(7) 0.0279(6) -0.1548(6) 0.113(4) Uani 1 1 d . . . H16A H 0.0753 0.0491 -0.1086 0.169 Uiso 1 1 calc R . . H16B H 0.0788 -0.0277 -0.1519 0.169 Uiso 1 1 calc R . . H16C H 0.0123 0.0358 -0.1804 0.169 Uiso 1 1 calc R . . C17 C 0.0802(4) 0.0791(5) -0.4190(4) 0.072(2) Uani 1 1 d . . . H17A H 0.0806 0.0681 -0.4667 0.086 Uiso 1 1 calc R . . H17B H 0.0460 0.0399 -0.4058 0.086 Uiso 1 1 calc R . . C18 C 0.0434(5) 0.1583(6) -0.4172(5) 0.081(2) Uani 1 1 d . . . H18A H 0.0721 0.1977 -0.4366 0.097 Uiso 1 1 calc R . . H18B H 0.0467 0.1729 -0.3693 0.097 Uiso 1 1 calc R . . C19 C -0.0444(6) 0.1557(7) -0.4597(5) 0.100(3) Uani 1 1 d . . . H19A H -0.0466 0.1411 -0.5073 0.119 Uiso 1 1 calc R . . H19B H -0.0716 0.1148 -0.4407 0.119 Uiso 1 1 calc R . . C20 C -0.0883(7) 0.2326(8) -0.4606(7) 0.133(5) Uani 1 1 d . . . H20A H -0.1427 0.2264 -0.4876 0.200 Uiso 1 1 calc R . . H20B H -0.0630 0.2731 -0.4809 0.200 Uiso 1 1 calc R . . H20C H -0.0873 0.2472 -0.4137 0.200 Uiso 1 1 calc R . . C21 C -0.2007(5) -0.0459(6) -0.2377(5) 0.090(3) Uani 1 1 d U . . H21A H -0.2040 -0.0956 -0.2628 0.108 Uiso 1 1 calc R . . H21B H -0.1445 -0.0327 -0.2203 0.108 Uiso 1 1 calc R . . C22 C -0.2412(7) 0.0180(7) -0.2886(6) 0.121(4) Uani 1 1 d U . . H22A H -0.2949 0.0015 -0.3127 0.145 Uiso 1 1 calc R . . H22B H -0.2446 0.0666 -0.2635 0.145 Uiso 1 1 calc R . . C23 C -0.1931(9) 0.0320(9) -0.3406(8) 0.164(4) Uani 1 1 d DU . . H23A H -0.1401 0.0497 -0.3156 0.196 Uiso 1 1 calc R . . H23B H -0.1873 -0.0179 -0.3629 0.196 Uiso 1 1 calc R . . C24 C -0.2277(9) 0.0900(9) -0.3947(8) 0.164(4) Uani 1 1 d DU . . H24A H -0.1953 0.0936 -0.4269 0.245 Uiso 1 1 calc R . . H24B H -0.2298 0.1408 -0.3737 0.245 Uiso 1 1 calc R . . H24C H -0.2807 0.0738 -0.4192 0.245 Uiso 1 1 calc R . . C25 C -0.2257(6) 0.0156(5) -0.1319(5) 0.090(3) Uani 1 1 d . . . H25A H -0.2572 0.0576 -0.1593 0.108 Uiso 1 1 calc R . . H25B H -0.2475 0.0052 -0.0926 0.108 Uiso 1 1 calc R . . C26 C -0.1410(7) 0.0445(7) -0.1043(6) 0.114(4) Uani 1 1 d . . . H26A H -0.1082 0.0018 -0.0795 0.137 Uiso 1 1 calc R . . H26B H -0.1202 0.0596 -0.1431 0.137 Uiso 1 1 calc R . . C27 C -0.1362(8) 0.1122(8) -0.0575(7) 0.132(4) Uani 1 1 d . . . H27A H -0.1688 0.1546 -0.0832 0.158 Uiso 1 1 calc R . . H27B H -0.1594 0.0968 -0.0201 0.158 Uiso 1 1 calc R . . C28 C -0.0562(10) 0.1435(10) -0.0263(8) 0.165(6) Uani 1 1 d . . . H28A H -0.0596 0.1876 0.0032 0.248 Uiso 1 1 calc R . . H28B H -0.0328 0.1605 -0.0625 0.248 Uiso 1 1 calc R . . H28C H -0.0236 0.1029 0.0010 0.248 Uiso 1 1 calc R . . C29 C -0.1900(6) -0.1281(6) -0.1372(6) 0.095(3) Uani 1 1 d . . . H29A H -0.1333 -0.1184 -0.1296 0.115 Uiso 1 1 calc R . . H29B H -0.2033 -0.1744 -0.1668 0.115 Uiso 1 1 calc R . . C30 C -0.2055(9) -0.1470(7) -0.0675(7) 0.128(4) Uani 1 1 d . . . H30A H -0.1891 -0.1029 -0.0357 0.154 Uiso 1 1 calc R . . H30B H -0.2620 -0.1563 -0.0735 0.154 Uiso 1 1 calc R . . C31 C -0.1588(10) -0.2197(10) -0.0384(8) 0.158(6) Uani 1 1 d D . . H31A H -0.1803 -0.2652 -0.0671 0.190 Uiso 1 1 calc R . . H31B H -0.1035 -0.2131 -0.0389 0.190 Uiso 1 1 calc R . . C32 C -0.1633(12) -0.2331(14) 0.0332(10) 0.237(9) Uani 1 1 d D . . H32A H -0.1326 -0.2791 0.0519 0.356 Uiso 1 1 calc R . . H32B H -0.2180 -0.2411 0.0334 0.356 Uiso 1 1 calc R . . H32C H -0.1423 -0.1879 0.0614 0.356 Uiso 1 1 calc R . . C33 C -0.3244(6) -0.0750(6) -0.1995(6) 0.099(3) Uani 1 1 d . . . H33A H -0.3441 -0.0787 -0.1583 0.119 Uiso 1 1 calc R . . H33B H -0.3508 -0.0303 -0.2266 0.119 Uiso 1 1 calc R . . C34 C -0.3477(7) -0.1473(8) -0.2409(8) 0.146(5) Uani 1 1 d D . . H34A H -0.3394 -0.1379 -0.2866 0.175 Uiso 1 1 calc R . . H34B H -0.3110 -0.1889 -0.2192 0.175 Uiso 1 1 calc R . . C35 C -0.4288(9) -0.1780(9) -0.2515(11) 0.184(7) Uani 1 1 d D . . H35A H -0.4659 -0.1382 -0.2763 0.221 Uiso 1 1 calc R . . H35B H -0.4388 -0.1847 -0.2061 0.221 Uiso 1 1 calc R . . C36 C -0.4477(10) -0.2531(10) -0.2896(12) 0.221(9) Uani 1 1 d . . . H36A H -0.5015 -0.2684 -0.2916 0.332 Uiso 1 1 calc R . . H36B H -0.4115 -0.2935 -0.2661 0.332 Uiso 1 1 calc R . . H36C H -0.4424 -0.2466 -0.3361 0.332 Uiso 1 1 calc R . . C38 C 0.4781(14) -0.0301(13) -0.4788(11) 0.415(16) Uiso 0.50 1 d PD . . O19 O 0.447(2) -0.075(2) -0.447(2) 0.415(16) Uiso 0.50 1 d PD . . C37 C 0.522(2) 0.0440(16) -0.4463(10) 0.415(16) Uiso 1 1 d D . 1 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 Mo6 0.0491(4) 0.0441(4) 0.0548(4) 0.0024(3) 0.0065(3) 0.0020(3) Mo2 0.0535(4) 0.0500(4) 0.0894(5) -0.0039(3) 0.0319(4) 0.0027(3) Mo4 0.0434(4) 0.0531(4) 0.0984(6) 0.0008(4) 0.0216(4) 0.0015(3) Mo3 0.0813(5) 0.0526(4) 0.0507(4) -0.0045(3) -0.0003(3) -0.0074(3) Mo5 0.0596(5) 0.0385(4) 0.1010(6) 0.0073(3) 0.0197(4) 0.0008(3) Mo1 0.0665(5) 0.0646(5) 0.0695(5) -0.0308(4) 0.0145(4) -0.0123(3) O1 0.038(2) 0.036(2) 0.055(3) -0.0061(19) 0.010(2) -0.0007(17) O2 0.071(4) 0.077(4) 0.141(6) 0.002(4) 0.057(4) 0.012(3) O3 0.139(6) 0.087(5) 0.058(4) -0.013(3) -0.009(4) -0.013(4) O4 0.063(4) 0.076(4) 0.147(6) 0.008(4) 0.043(4) 0.004(3) O5 0.096(5) 0.054(4) 0.149(6) 0.028(4) 0.036(4) 0.008(3) O6 0.067(3) 0.059(3) 0.079(4) 0.015(3) 0.008(3) 0.002(2) O7 0.055(3) 0.074(4) 0.048(3) -0.009(2) 0.000(2) -0.008(2) O8 0.071(4) 0.048(3) 0.106(4) -0.028(3) 0.034(3) -0.011(2) O9 0.045(3) 0.066(3) 0.089(4) -0.015(3) 0.008(3) -0.016(2) O10 0.075(4) 0.066(3) 0.090(4) -0.019(3) 0.039(3) -0.003(3) O11 0.066(3) 0.048(3) 0.094(4) 0.010(3) 0.035(3) 0.000(2) O12 0.052(3) 0.049(3) 0.082(4) 0.001(2) 0.016(3) 0.013(2) O13 0.136(5) 0.047(3) 0.054(3) -0.006(2) 0.036(3) 0.012(3) O14 0.077(3) 0.035(2) 0.056(3) -0.004(2) 0.004(2) -0.004(2) O15 0.085(4) 0.056(3) 0.066(3) 0.015(3) 0.003(3) -0.003(3) O16 0.046(3) 0.054(3) 0.090(4) 0.009(3) -0.002(3) -0.005(2) O17 0.049(3) 0.051(3) 0.072(3) 0.009(2) 0.014(2) 0.000(2) O18 0.053(3) 0.048(3) 0.118(5) 0.008(3) 0.020(3) 0.008(2) N1 0.094(6) 0.094(6) 0.087(5) -0.044(4) 0.022(4) -0.021(4) N2 0.053(4) 0.064(4) 0.068(4) -0.008(3) 0.003(3) -0.009(3) N3 0.079(5) 0.059(4) 0.116(6) -0.010(4) 0.033(5) 0.020(4) C1 0.119(9) 0.112(9) 0.079(7) -0.051(6) 0.028(6) -0.015(7) C2 0.150(12) 0.190(15) 0.156(13) -0.076(11) -0.049(10) 0.114(11) C3 0.155(11) 0.068(7) 0.129(9) -0.043(6) 0.037(8) -0.032(6) C4 0.099(8) 0.132(10) 0.121(9) -0.058(8) 0.035(7) -0.002(7) C5 0.069(6) 0.063(5) 0.098(7) -0.008(5) 0.023(5) -0.012(4) C6 0.103(9) 0.070(7) 0.164(11) -0.003(7) 0.013(8) 0.001(6) C7 0.099(10) 0.072(8) 0.281(19) -0.027(10) 0.018(11) 0.002(6) C8 0.135(13) 0.078(9) 0.31(2) -0.009(11) 0.011(13) 0.013(8) C9 0.056(5) 0.063(5) 0.083(6) -0.004(4) 0.013(4) -0.012(4) C10 0.061(5) 0.086(6) 0.073(6) -0.003(5) 0.007(4) -0.012(4) C11 0.094(7) 0.085(7) 0.085(7) 0.006(5) 0.019(5) -0.013(5) C12 0.092(8) 0.110(9) 0.107(8) 0.010(7) 0.024(6) -0.009(6) C13 0.071(6) 0.064(5) 0.060(5) -0.003(4) -0.003(4) -0.004(4) C14 0.085(6) 0.067(5) 0.071(6) -0.004(4) 0.017(5) -0.011(4) C15 0.095(7) 0.080(6) 0.076(6) 0.002(5) 0.016(5) -0.008(5) C16 0.143(10) 0.097(8) 0.110(8) -0.017(7) 0.053(8) -0.020(7) C17 0.052(5) 0.093(7) 0.062(5) -0.001(4) 0.002(4) -0.013(4) C18 0.060(6) 0.097(7) 0.076(6) 0.010(5) 0.002(4) 0.007(5) C19 0.074(7) 0.152(10) 0.077(6) 0.017(6) 0.026(5) -0.003(6) C20 0.093(9) 0.165(13) 0.141(11) 0.042(9) 0.029(7) 0.049(8) C21 0.075(6) 0.096(7) 0.108(7) -0.009(5) 0.041(5) 0.029(5) C22 0.134(9) 0.099(8) 0.141(9) 0.017(6) 0.056(7) 0.028(6) C23 0.166(9) 0.163(10) 0.183(10) 0.050(7) 0.083(8) 0.034(7) C24 0.166(9) 0.163(10) 0.183(10) 0.050(7) 0.083(8) 0.034(7) C25 0.100(8) 0.067(6) 0.114(8) -0.016(5) 0.047(6) 0.002(5) C26 0.129(10) 0.091(8) 0.131(10) -0.025(7) 0.050(8) -0.002(7) C27 0.107(10) 0.135(11) 0.156(12) -0.045(9) 0.040(9) -0.012(8) C28 0.173(16) 0.180(15) 0.150(13) -0.031(11) 0.057(12) 0.001(12) C29 0.082(7) 0.073(6) 0.131(9) -0.010(6) 0.028(6) 0.009(5) C30 0.162(12) 0.092(9) 0.129(11) 0.003(8) 0.037(9) 0.019(8) C31 0.170(15) 0.162(15) 0.136(13) 0.032(11) 0.030(11) -0.026(11) C32 0.22(2) 0.30(3) 0.171(19) 0.032(19) 0.021(16) -0.012(18) C33 0.077(7) 0.089(7) 0.138(9) -0.025(6) 0.043(6) 0.015(5) C34 0.090(9) 0.131(11) 0.222(16) -0.071(11) 0.050(9) -0.005(7) C35 0.151(15) 0.113(11) 0.31(2) -0.047(13) 0.101(15) -0.014(10) C36 0.146(14) 0.137(14) 0.37(3) -0.110(16) 0.046(15) -0.032(10) _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 Mo6 O6 1.694(5) . ? Mo6 O7 1.879(5) . ? Mo6 O12 1.887(5) . ? Mo6 O14 1.931(5) . ? Mo6 O17 1.981(5) . ? Mo6 O1 2.332(4) . ? Mo2 O2 1.683(5) . ? Mo2 O11 1.877(5) . ? Mo2 O9 1.890(5) . ? Mo2 O13 1.943(6) . ? Mo2 O12 1.981(5) . ? Mo2 O1 2.307(4) . ? Mo4 O4 1.682(5) . ? Mo4 O10 1.879(6) . ? Mo4 O17 1.892(5) . ? Mo4 O16 1.908(5) . ? Mo4 O18 1.989(5) . ? Mo4 O1 2.338(4) . ? Mo3 O3 1.679(6) . ? Mo3 O13 1.894(6) . ? Mo3 O14 1.903(5) . ? Mo3 O16 1.928(5) . ? Mo3 O15 1.937(5) . ? Mo3 O1 2.338(4) . ? Mo5 O5 1.677(6) . ? Mo5 O18 1.890(5) . ? Mo5 O8 1.899(6) . ? Mo5 O15 1.910(5) . ? Mo5 O11 1.986(5) . ? Mo5 O1 2.326(4) . ? Mo1 N1 1.718(7) . ? Mo1 O9 1.949(5) . ? Mo1 O10 1.952(5) . ? Mo1 O8 1.953(6) . ? Mo1 O7 1.967(5) . ? Mo1 O1 2.230(4) . ? N1 C1 1.433(11) . ? N2 C5 1.506(9) . ? N2 C9 1.524(9) . ? N2 C13 1.529(9) . ? N2 C17 1.538(9) . ? N3 C21 1.508(11) . ? N3 C25 1.509(10) . ? N3 C29 1.513(11) . ? N3 C33 1.526(11) . ? C1 C3 1.449(14) . ? C1 C4 1.489(13) . ? C1 C2 1.603(15) . ? C2 H2A 0.9600 . ? C2 H2B 0.9600 . ? C2 H2C 0.9600 . ? C3 H3A 0.9600 . ? C3 H3B 0.9600 . ? C3 H3C 0.9600 . ? C4 H4A 0.9600 . ? C4 H4B 0.9600 . ? C4 H4C 0.9600 . ? C5 C6 1.489(12) . ? C5 H5A 0.9700 . ? C5 H5B 0.9700 . ? C6 C7 1.490(11) . ? C6 H6A 0.9700 . ? C6 H6B 0.9700 . ? C7 C8 1.453(18) . ? C7 H7A 0.9700 . ? C7 H7B 0.9700 . ? C8 H8A 0.9600 . ? C8 H8B 0.9600 . ? C8 H8C 0.9600 . ? C9 C10 1.511(11) . ? C9 H9A 0.9700 . ? C9 H9B 0.9700 . ? C10 C11 1.514(11) . ? C10 H10A 0.9700 . ? C10 H10B 0.9700 . ? C11 C12 1.485(13) . ? C11 H11A 0.9700 . ? C11 H11B 0.9700 . ? C12 H12A 0.9600 . ? C12 H12B 0.9600 . ? C12 H12C 0.9600 . ? C13 C14 1.504(10) . ? C13 H13A 0.9700 . ? C13 H13B 0.9700 . ? C14 C15 1.488(11) . ? C14 H14A 0.9700 . ? C14 H14B 0.9700 . ? C15 C16 1.512(12) . ? C15 H15A 0.9700 . ? C15 H15B 0.9700 . ? C16 H16A 0.9600 . ? C16 H16B 0.9600 . ? C16 H16C 0.9600 . ? C17 C18 1.486(11) . ? C17 H17A 0.9700 . ? C17 H17B 0.9700 . ? C18 C19 1.535(12) . ? C18 H18A 0.9700 . ? C18 H18B 0.9700 . ? C19 C20 1.503(14) . ? C19 H19A 0.9700 . ? C19 H19B 0.9700 . ? C20 H20A 0.9600 . ? C20 H20B 0.9600 . ? C20 H20C 0.9600 . ? C21 C22 1.519(13) . ? C21 H21A 0.9700 . ? C21 H21B 0.9700 . ? C22 C23 1.511(14) . ? C22 H22A 0.9700 . ? C22 H22B 0.9700 . ? C23 C24 1.462(13) . ? C23 H23A 0.9700 . ? C23 H23B 0.9700 . ? C24 H24A 0.9600 . ? C24 H24B 0.9600 . ? C24 H24C 0.9600 . ? C25 C26 1.507(14) . ? C25 H25A 0.9700 . ? C25 H25B 0.9700 . ? C26 C27 1.464(14) . ? C26 H26A 0.9700 . ? C26 H26B 0.9700 . ? C27 C28 1.462(17) . ? C27 H27A 0.9700 . ? C27 H27B 0.9700 . ? C28 H28A 0.9600 . ? C28 H28B 0.9600 . ? C28 H28C 0.9600 . ? C29 C30 1.514(15) . ? C29 H29A 0.9700 . ? C29 H29B 0.9700 . ? C30 C31 1.499(17) . ? C30 H30A 0.9700 . ? C30 H30B 0.9700 . ? C31 C32 1.466(15) . ? C31 H31A 0.9700 . ? C31 H31B 0.9700 . ? C32 H32A 0.9600 . ? C32 H32B 0.9600 . ? C32 H32C 0.9600 . ? C33 C34 1.469(14) . ? C33 H33A 0.9700 . ? C33 H33B 0.9700 . ? C34 C35 1.463(13) . ? C34 H34A 0.9700 . ? C34 H34B 0.9700 . ? C35 C36 1.470(18) . ? C35 H35A 0.9700 . ? C35 H35B 0.9700 . ? C36 H36A 0.9600 . ? C36 H36B 0.9600 . ? C36 H36C 0.9600 . ? C38 O19 1.210(10) . ? C38 C37 1.507(13) 3_654 ? C38 C37 1.518(9) . ? C37 C38 1.507(13) 3_654 ? 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 O6 Mo6 O7 103.5(2) . . ? O6 Mo6 O12 105.1(2) . . ? O7 Mo6 O12 90.0(2) . . ? O6 Mo6 O14 103.0(2) . . ? O7 Mo6 O14 153.1(2) . . ? O12 Mo6 O14 87.8(2) . . ? O6 Mo6 O17 101.8(2) . . ? O7 Mo6 O17 85.9(2) . . ? O12 Mo6 O17 152.95(19) . . ? O14 Mo6 O17 84.0(2) . . ? O6 Mo6 O1 177.7(2) . . ? O7 Mo6 O1 76.98(19) . . ? O12 Mo6 O1 77.06(17) . . ? O14 Mo6 O1 76.37(16) . . ? O17 Mo6 O1 75.95(16) . . ? O2 Mo2 O11 103.3(3) . . ? O2 Mo2 O9 103.7(3) . . ? O11 Mo2 O9 89.5(2) . . ? O2 Mo2 O13 103.4(3) . . ? O11 Mo2 O13 89.3(2) . . ? O9 Mo2 O13 152.4(2) . . ? O2 Mo2 O12 102.6(2) . . ? O11 Mo2 O12 154.07(19) . . ? O9 Mo2 O12 85.4(2) . . ? O13 Mo2 O12 83.8(2) . . ? O2 Mo2 O1 178.4(2) . . ? O11 Mo2 O1 78.13(17) . . ? O9 Mo2 O1 76.94(18) . . ? O13 Mo2 O1 75.86(19) . . ? O12 Mo2 O1 75.96(16) . . ? O4 Mo4 O10 103.1(3) . . ? O4 Mo4 O17 105.5(3) . . ? O10 Mo4 O17 90.8(2) . . ? O4 Mo4 O16 103.1(3) . . ? O10 Mo4 O16 153.1(2) . . ? O17 Mo4 O16 87.8(2) . . ? O4 Mo4 O18 100.9(3) . . ? O10 Mo4 O18 85.1(2) . . ? O17 Mo4 O18 153.5(2) . . ? O16 Mo4 O18 84.3(2) . . ? O4 Mo4 O1 177.1(2) . . ? O10 Mo4 O1 76.56(18) . . ? O17 Mo4 O1 77.40(17) . . ? O16 Mo4 O1 76.92(18) . . ? O18 Mo4 O1 76.15(17) . . ? O3 Mo3 O13 104.0(3) . . ? O3 Mo3 O14 103.5(3) . . ? O13 Mo3 O14 86.2(2) . . ? O3 Mo3 O16 103.5(3) . . ? O13 Mo3 O16 152.5(2) . . ? O14 Mo3 O16 88.0(2) . . ? O3 Mo3 O15 103.9(3) . . ? O13 Mo3 O15 86.4(2) . . ? O14 Mo3 O15 152.6(2) . . ? O16 Mo3 O15 86.5(2) . . ? O3 Mo3 O1 179.8(3) . . ? O13 Mo3 O1 75.98(18) . . ? O14 Mo3 O1 76.74(17) . . ? O16 Mo3 O1 76.56(18) . . ? O15 Mo3 O1 75.92(19) . . ? O5 Mo5 O18 104.1(3) . . ? O5 Mo5 O8 103.6(3) . . ? O18 Mo5 O8 89.5(2) . . ? O5 Mo5 O15 102.8(3) . . ? O18 Mo5 O15 88.5(2) . . ? O8 Mo5 O15 153.2(2) . . ? O5 Mo5 O11 101.9(3) . . ? O18 Mo5 O11 153.9(2) . . ? O8 Mo5 O11 85.0(2) . . ? O15 Mo5 O11 85.1(2) . . ? O5 Mo5 O1 177.6(2) . . ? O18 Mo5 O1 78.29(18) . . ? O8 Mo5 O1 76.73(19) . . ? O15 Mo5 O1 76.71(18) . . ? O11 Mo5 O1 75.66(16) . . ? N1 Mo1 O9 102.7(3) . . ? N1 Mo1 O10 101.7(3) . . ? O9 Mo1 O10 155.6(2) . . ? N1 Mo1 O8 103.0(3) . . ? O9 Mo1 O8 87.8(2) . . ? O10 Mo1 O8 86.6(2) . . ? N1 Mo1 O7 101.1(3) . . ? O9 Mo1 O7 87.7(2) . . ? O10 Mo1 O7 87.8(2) . . ? O8 Mo1 O7 155.9(2) . . ? N1 Mo1 O1 178.8(3) . . ? O9 Mo1 O1 77.73(18) . . ? O10 Mo1 O1 77.88(19) . . ? O8 Mo1 O1 78.07(18) . . ? O7 Mo1 O1 77.83(17) . . ? Mo1 O1 Mo2 90.72(14) . . ? Mo1 O1 Mo5 90.62(14) . . ? Mo2 O1 Mo5 90.10(14) . . ? Mo1 O1 Mo6 90.41(15) . . ? Mo2 O1 Mo6 90.38(14) . . ? Mo5 O1 Mo6 178.9(2) . . ? Mo1 O1 Mo3 179.1(2) . . ? Mo2 O1 Mo3 90.13(14) . . ? Mo5 O1 Mo3 89.71(15) . . ? Mo6 O1 Mo3 89.25(13) . . ? Mo1 O1 Mo4 90.15(14) . . ? Mo2 O1 Mo4 179.1(2) . . ? Mo5 O1 Mo4 89.65(14) . . ? Mo6 O1 Mo4 89.86(14) . . ? Mo3 O1 Mo4 89.00(14) . . ? Mo6 O7 Mo1 114.7(2) . . ? Mo5 O8 Mo1 114.5(2) . . ? Mo2 O9 Mo1 114.5(2) . . ? Mo4 O10 Mo1 115.3(2) . . ? Mo2 O11 Mo5 116.1(2) . . ? Mo6 O12 Mo2 116.6(2) . . ? Mo3 O13 Mo2 117.9(2) . . ? Mo3 O14 Mo6 117.6(2) . . ? Mo5 O15 Mo3 117.5(3) . . ? Mo4 O16 Mo3 117.4(2) . . ? Mo4 O17 Mo6 116.8(2) . . ? Mo5 O18 Mo4 115.9(2) . . ? C1 N1 Mo1 178.3(8) . . ? C5 N2 C9 112.4(6) . . ? C5 N2 C13 110.8(6) . . ? C9 N2 C13 106.4(6) . . ? C5 N2 C17 106.1(6) . . ? C9 N2 C17 110.4(6) . . ? C13 N2 C17 110.7(6) . . ? C21 N3 C25 111.0(7) . . ? C21 N3 C29 105.2(7) . . ? C25 N3 C29 112.6(8) . . ? C21 N3 C33 111.7(8) . . ? C25 N3 C33 105.9(6) . . ? C29 N3 C33 110.7(7) . . ? N1 C1 C3 110.6(9) . . ? N1 C1 C4 109.0(9) . . ? C3 C1 C4 114.4(9) . . ? N1 C1 C2 111.2(9) . . ? C3 C1 C2 106.4(11) . . ? C4 C1 C2 105.1(11) . . ? C1 C2 H2A 109.5 . . ? C1 C2 H2B 109.5 . . ? H2A C2 H2B 109.5 . . ? C1 C2 H2C 109.5 . . ? H2A C2 H2C 109.5 . . ? H2B C2 H2C 109.5 . . ? C1 C3 H3A 109.5 . . ? C1 C3 H3B 109.5 . . ? H3A C3 H3B 109.5 . . ? C1 C3 H3C 109.5 . . ? H3A C3 H3C 109.5 . . ? H3B C3 H3C 109.5 . . ? C1 C4 H4A 109.5 . . ? C1 C4 H4B 109.5 . . ? H4A C4 H4B 109.5 . . ? C1 C4 H4C 109.5 . . ? H4A C4 H4C 109.5 . . ? H4B C4 H4C 109.5 . . ? C6 C5 N2 115.0(7) . . ? C6 C5 H5A 108.5 . . ? N2 C5 H5A 108.5 . . ? C6 C5 H5B 108.5 . . ? N2 C5 H5B 108.5 . . ? H5A C5 H5B 107.5 . . ? C5 C6 C7 112.2(9) . . ? C5 C6 H6A 109.2 . . ? C7 C6 H6A 109.2 . . ? C5 C6 H6B 109.2 . . ? C7 C6 H6B 109.2 . . ? H6A C6 H6B 107.9 . . ? C8 C7 C6 117.4(12) . . ? C8 C7 H7A 108.0 . . ? C6 C7 H7A 108.0 . . ? C8 C7 H7B 108.0 . . ? C6 C7 H7B 108.0 . . ? H7A C7 H7B 107.2 . . ? C7 C8 H8A 109.5 . . ? C7 C8 H8B 109.5 . . ? H8A C8 H8B 109.5 . . ? C7 C8 H8C 109.5 . . ? H8A C8 H8C 109.5 . . ? H8B C8 H8C 109.5 . . ? C10 C9 N2 115.4(6) . . ? C10 C9 H9A 108.4 . . ? N2 C9 H9A 108.4 . . ? C10 C9 H9B 108.4 . . ? N2 C9 H9B 108.4 . . ? H9A C9 H9B 107.5 . . ? C9 C10 C11 110.5(7) . . ? C9 C10 H10A 109.5 . . ? C11 C10 H10A 109.5 . . ? C9 C10 H10B 109.5 . . ? C11 C10 H10B 109.5 . . ? H10A C10 H10B 108.1 . . ? C12 C11 C10 114.1(8) . . ? C12 C11 H11A 108.7 . . ? C10 C11 H11A 108.7 . . ? C12 C11 H11B 108.7 . . ? C10 C11 H11B 108.7 . . ? H11A C11 H11B 107.6 . . ? C11 C12 H12A 109.5 . . ? C11 C12 H12B 109.5 . . ? H12A C12 H12B 109.5 . . ? C11 C12 H12C 109.5 . . ? H12A C12 H12C 109.5 . . ? H12B C12 H12C 109.5 . . ? C14 C13 N2 116.1(6) . . ? C14 C13 H13A 108.3 . . ? N2 C13 H13A 108.3 . . ? C14 C13 H13B 108.3 . . ? N2 C13 H13B 108.3 . . ? H13A C13 H13B 107.4 . . ? C15 C14 C13 111.3(7) . . ? C15 C14 H14A 109.4 . . ? C13 C14 H14A 109.4 . . ? C15 C14 H14B 109.4 . . ? C13 C14 H14B 109.4 . . ? H14A C14 H14B 108.0 . . ? C14 C15 C16 115.2(8) . . ? C14 C15 H15A 108.5 . . ? C16 C15 H15A 108.5 . . ? C14 C15 H15B 108.5 . . ? C16 C15 H15B 108.5 . . ? H15A C15 H15B 107.5 . . ? 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 N2 116.9(7) . . ? C18 C17 H17A 108.1 . . ? N2 C17 H17A 108.1 . . ? C18 C17 H17B 108.1 . . ? N2 C17 H17B 108.1 . . ? H17A C17 H17B 107.3 . . ? C17 C18 C19 109.4(8) . . ? C17 C18 H18A 109.8 . . ? C19 C18 H18A 109.8 . . ? C17 C18 H18B 109.8 . . ? C19 C18 H18B 109.8 . . ? H18A C18 H18B 108.2 . . ? C20 C19 C18 114.2(10) . . ? C20 C19 H19A 108.7 . . ? C18 C19 H19A 108.7 . . ? C20 C19 H19B 108.7 . . ? C18 C19 H19B 108.7 . . ? H19A C19 H19B 107.6 . . ? C19 C20 H20A 109.5 . . ? C19 C20 H20B 109.5 . . ? H20A C20 H20B 109.5 . . ? C19 C20 H20C 109.5 . . ? H20A C20 H20C 109.5 . . ? H20B C20 H20C 109.5 . . ? N3 C21 C22 115.1(7) . . ? N3 C21 H21A 108.5 . . ? C22 C21 H21A 108.5 . . ? N3 C21 H21B 108.5 . . ? C22 C21 H21B 108.5 . . ? H21A C21 H21B 107.5 . . ? C23 C22 C21 109.0(9) . . ? C23 C22 H22A 109.9 . . ? C21 C22 H22A 109.9 . . ? C23 C22 H22B 109.9 . . ? C21 C22 H22B 109.9 . . ? H22A C22 H22B 108.3 . . ? C24 C23 C22 114.6(12) . . ? C24 C23 H23A 108.6 . . ? C22 C23 H23A 108.6 . . ? C24 C23 H23B 108.6 . . ? C22 C23 H23B 108.6 . . ? H23A C23 H23B 107.6 . . ? C23 C24 H24A 109.5 . . ? C23 C24 H24B 109.5 . . ? H24A C24 H24B 109.5 . . ? C23 C24 H24C 109.5 . . ? H24A C24 H24C 109.5 . . ? H24B C24 H24C 109.5 . . ? C26 C25 N3 115.0(8) . . ? C26 C25 H25A 108.5 . . ? N3 C25 H25A 108.5 . . ? C26 C25 H25B 108.5 . . ? N3 C25 H25B 108.5 . . ? H25A C25 H25B 107.5 . . ? C27 C26 C25 111.7(9) . . ? C27 C26 H26A 109.3 . . ? C25 C26 H26A 109.3 . . ? C27 C26 H26B 109.3 . . ? C25 C26 H26B 109.3 . . ? H26A C26 H26B 107.9 . . ? C28 C27 C26 116.1(11) . . ? C28 C27 H27A 108.3 . . ? C26 C27 H27A 108.3 . . ? C28 C27 H27B 108.3 . . ? C26 C27 H27B 108.3 . . ? H27A C27 H27B 107.4 . . ? C27 C28 H28A 109.5 . . ? C27 C28 H28B 109.5 . . ? H28A C28 H28B 109.5 . . ? C27 C28 H28C 109.5 . . ? H28A C28 H28C 109.5 . . ? H28B C28 H28C 109.5 . . ? N3 C29 C30 116.3(8) . . ? N3 C29 H29A 108.2 . . ? C30 C29 H29A 108.2 . . ? N3 C29 H29B 108.2 . . ? C30 C29 H29B 108.2 . . ? H29A C29 H29B 107.4 . . ? C31 C30 C29 108.5(11) . . ? C31 C30 H30A 110.0 . . ? C29 C30 H30A 110.0 . . ? C31 C30 H30B 110.0 . . ? C29 C30 H30B 110.0 . . ? H30A C30 H30B 108.4 . . ? C32 C31 C30 109.8(16) . . ? C32 C31 H31A 109.7 . . ? C30 C31 H31A 109.7 . . ? C32 C31 H31B 109.7 . . ? C30 C31 H31B 109.7 . . ? H31A C31 H31B 108.2 . . ? C31 C32 H32A 109.5 . . ? C31 C32 H32B 109.5 . . ? H32A C32 H32B 109.5 . . ? C31 C32 H32C 109.5 . . ? H32A C32 H32C 109.5 . . ? H32B C32 H32C 109.5 . . ? C34 C33 N3 115.6(7) . . ? C34 C33 H33A 108.4 . . ? N3 C33 H33A 108.4 . . ? C34 C33 H33B 108.4 . . ? N3 C33 H33B 108.4 . . ? H33A C33 H33B 107.4 . . ? C35 C34 C33 119.1(11) . . ? C35 C34 H34A 107.5 . . ? C33 C34 H34A 107.5 . . ? C35 C34 H34B 107.5 . . ? C33 C34 H34B 107.5 . . ? H34A C34 H34B 107.0 . . ? C34 C35 C36 117.0(12) . . ? C34 C35 H35A 108.1 . . ? C36 C35 H35A 108.1 . . ? C34 C35 H35B 108.1 . . ? C36 C35 H35B 108.1 . . ? H35A C35 H35B 107.3 . . ? C35 C36 H36A 109.5 . . ? C35 C36 H36B 109.5 . . ? H36A C36 H36B 109.5 . . ? C35 C36 H36C 109.5 . . ? H36A C36 H36C 109.5 . . ? H36B C36 H36C 109.5 . . ? O19 C38 C37 122.5(11) . 3_654 ? O19 C38 C37 122.8(13) . . ? C37 C38 C37 114.7(14) 3_654 . ? _diffrn_measured_fraction_theta_max 0.998 _diffrn_reflns_theta_full 25.00 _diffrn_measured_fraction_theta_full 0.998 _refine_diff_density_max 1.669 _refine_diff_density_min -0.590 _refine_diff_density_rms 0.117 #===END data_compound-7I _database_code_depnum_ccdc_archive 'CCDC 688718' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C38 H83 Mo6 N3 O18' _chemical_formula_weight 1445.71 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' Mo Mo -1.6832 0.6857 '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 12.5288(4) _cell_length_b 19.4569(6) _cell_length_c 23.1302(7) _cell_angle_alpha 93.7700(10) _cell_angle_beta 103.1410(10) _cell_angle_gamma 91.4990(10) _cell_volume 5474.0(3) _cell_formula_units_Z 4 _cell_measurement_temperature 296(2) _cell_measurement_reflns_used 5741 _cell_measurement_theta_min 2.72 _cell_measurement_theta_max 27.51 _exptl_crystal_description block _exptl_crystal_colour orange _exptl_crystal_size_max 0.46 _exptl_crystal_size_mid 0.22 _exptl_crystal_size_min 0.17 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.754 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 2912 _exptl_absorpt_coefficient_mu 1.398 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.5656 _exptl_absorpt_correction_T_max 0.7970 _exptl_absorpt_process_details ? _exptl_special_details ; ? ; _diffrn_ambient_temperature 296(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 'CCD area detector' _diffrn_measurement_method 'phi and omega scans' _diffrn_detector_area_resol_mean ? _diffrn_reflns_number 44067 _diffrn_reflns_av_R_equivalents 0.0302 _diffrn_reflns_av_sigmaI/netI 0.0394 _diffrn_reflns_limit_h_min -14 _diffrn_reflns_limit_h_max 14 _diffrn_reflns_limit_k_min -20 _diffrn_reflns_limit_k_max 23 _diffrn_reflns_limit_l_min -27 _diffrn_reflns_limit_l_max 27 _diffrn_reflns_theta_min 1.81 _diffrn_reflns_theta_max 25.00 _reflns_number_total 18581 _reflns_number_gt 12438 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'Bruker SMART' _computing_cell_refinement 'Bruker SMART' _computing_data_reduction 'Bruker SAINT' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _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^)+(0.0434P)^2^+21.3101P] 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 18581 _refine_ls_number_parameters 1141 _refine_ls_number_restraints 108 _refine_ls_R_factor_all 0.0891 _refine_ls_R_factor_gt 0.0561 _refine_ls_wR_factor_ref 0.1489 _refine_ls_wR_factor_gt 0.1260 _refine_ls_goodness_of_fit_ref 1.140 _refine_ls_restrained_S_all 1.418 _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 Mo1 Mo 0.57209(7) 0.35309(4) 0.04606(4) 0.0496(2) Uani 1 1 d . . . Mo2 Mo 0.64611(6) 0.19583(4) 0.06138(4) 0.0462(2) Uani 1 1 d D . . Mo3 Mo 0.50422(6) 0.18586(4) 0.16437(4) 0.0480(2) Uani 1 1 d . . . Mo4 Mo 0.43188(6) 0.34628(4) 0.14772(3) 0.0452(2) Uani 1 1 d . . . Mo5 Mo 0.69320(6) 0.31038(5) 0.17738(4) 0.0504(2) Uani 1 1 d . . . Mo6 Mo 0.38451(6) 0.23214(4) 0.03185(3) 0.0462(2) Uani 1 1 d . . . Mo7 Mo 0.56035(9) -0.30159(5) 0.45052(4) 0.0667(3) Uani 1 1 d . . . Mo8 Mo 0.52847(8) -0.18817(6) 0.34933(4) 0.0676(3) Uani 1 1 d . . . Mo9 Mo 0.66795(9) -0.14507(5) 0.48591(4) 0.0688(3) Uani 1 1 d . . . Mo10 Mo 0.79486(9) -0.16015(8) 0.37610(5) 0.0895(4) Uani 1 1 d . . . Mo11 Mo 0.68479(12) -0.31620(7) 0.34261(5) 0.0951(4) Uani 1 1 d . . . Mo12 Mo 0.82761(10) -0.27507(8) 0.47665(5) 0.0924(4) Uani 1 1 d D . . O1 O 0.5390(4) 0.2714(3) 0.1038(2) 0.0380(12) Uani 1 1 d . . . O2 O 0.7214(5) 0.1404(4) 0.0302(3) 0.0640(18) Uani 1 1 d . . . O3 O 0.4776(6) 0.1239(4) 0.2071(3) 0.0685(19) Uani 1 1 d . . . O4 O 0.3561(5) 0.3997(4) 0.1808(3) 0.0622(18) Uani 1 1 d . . . O5 O 0.8076(5) 0.3340(4) 0.2292(3) 0.072(2) Uani 1 1 d . . . O6 O 0.2701(5) 0.2031(4) -0.0190(3) 0.0627(18) Uani 1 1 d . . . O7 O 0.6971(5) 0.3683(3) 0.1158(3) 0.0570(16) Uani 1 1 d . . . O8 O 0.6515(5) 0.2757(3) 0.0197(3) 0.0532(16) Uani 1 1 d . . . O9 O 0.4839(5) 0.4011(3) 0.0943(3) 0.0528(15) Uani 1 1 d . . . O10 O 0.4375(5) 0.3083(3) -0.0021(3) 0.0521(15) Uani 1 1 d . . . O11 O 0.4960(5) 0.1781(3) 0.0110(3) 0.0484(14) Uani 1 1 d . . . O12 O 0.5907(5) 0.1403(3) 0.1161(3) 0.0495(14) Uani 1 1 d . . . O13 O 0.3276(4) 0.3024(3) 0.0823(3) 0.0496(15) Uani 1 1 d . . . O14 O 0.7480(5) 0.2380(3) 0.1270(3) 0.0523(15) Uani 1 1 d . . . O15 O 0.6356(5) 0.2313(3) 0.2097(3) 0.0542(16) Uani 1 1 d . . . O16 O 0.4276(5) 0.2641(3) 0.1886(3) 0.0495(15) Uani 1 1 d . . . O17 O 0.3829(5) 0.1743(3) 0.0955(3) 0.0486(14) Uani 1 1 d . . . O18 O 0.5814(5) 0.3619(3) 0.1999(3) 0.0528(15) Uani 1 1 d . . . O19 O 0.6775(5) -0.2311(4) 0.4123(3) 0.0592(17) Uani 1 1 d . . . O20 O 0.4760(7) -0.3542(4) 0.4770(3) 0.086(2) Uani 1 1 d . . . O21 O 0.4203(7) -0.1579(5) 0.3030(4) 0.096(3) Uani 1 1 d . . . O22 O 0.6606(9) -0.0823(5) 0.5376(4) 0.105(3) Uani 1 1 d . . . O23 O 0.8798(8) -0.1070(7) 0.3511(4) 0.130(4) Uani 1 1 d . . . O24 O 0.9360(8) -0.3043(7) 0.5234(5) 0.133(4) Uani 1 1 d . . . O25 O 0.4629(6) -0.2544(4) 0.3914(3) 0.071(2) Uani 1 1 d . . . O26 O 0.5742(6) -0.2194(4) 0.5010(3) 0.0640(18) Uani 1 1 d . . . O27 O 0.7043(7) -0.3224(4) 0.4957(3) 0.079(2) Uani 1 1 d . . . O28 O 0.5899(8) -0.3585(4) 0.3868(4) 0.087(2) Uani 1 1 d . . . O29 O 0.6512(6) -0.1383(4) 0.3321(3) 0.077(2) Uani 1 1 d . . . O30 O 0.5468(6) -0.1280(4) 0.4205(3) 0.073(2) Uani 1 1 d . . . O31 O 0.5641(7) -0.2653(5) 0.3029(3) 0.089(3) Uani 1 1 d . . . O32 O 0.7886(7) -0.1965(4) 0.5220(3) 0.081(2) Uani 1 1 d . . . O33 O 0.7611(7) -0.1034(5) 0.4418(3) 0.085(2) Uani 1 1 d . . . O34 O 0.8922(6) -0.2074(6) 0.4351(4) 0.103(3) Uani 1 1 d . . . O35 O 0.7789(8) -0.2442(6) 0.3257(4) 0.113(4) Uani 1 1 d . . . O36 O 0.8088(8) -0.3354(5) 0.4079(4) 0.109(3) Uani 1 1 d . . . N3 N 0.4417(8) 0.4405(5) 0.3615(4) 0.068(2) Uani 1 1 d . . . N4 N 0.9429(6) -0.2191(5) 0.8764(4) 0.061(2) Uani 1 1 d . . . N5 N 0.6127(7) -0.0882(4) 0.1623(3) 0.058(2) Uani 1 1 d . . . N6 N 0.7724(10) 0.1303(6) 0.5351(7) 0.109(4) Uani 1 1 d U . . N1 N 0.5967(7) 0.4164(4) 0.0028(3) 0.056(2) Uani 1 1 d D . . C1 C 0.6224(8) 0.4724(5) -0.0328(4) 0.060(3) Uani 1 1 d D . . H1 H 0.5543 0.4947 -0.0497 0.072 Uiso 1 1 calc R . . C2 C 0.6990(10) 0.5246(6) 0.0079(5) 0.077(3) Uani 1 1 d D . . H2A H 0.7071 0.5651 -0.0133 0.092 Uiso 1 1 calc R . . H2B H 0.6682 0.5385 0.0415 0.092 Uiso 1 1 calc R . . C3 C 0.8092(10) 0.4956(7) 0.0299(6) 0.091(4) Uani 1 1 d D . . H3A H 0.8589 0.5317 0.0529 0.109 Uiso 1 1 calc R . . H3B H 0.8024 0.4596 0.0561 0.109 Uiso 1 1 calc R . . C4 C 0.8562(11) 0.4667(9) -0.0193(8) 0.110(5) Uani 1 1 d D . . H4A H 0.9245 0.4455 -0.0026 0.132 Uiso 1 1 calc R . . H4B H 0.8728 0.5039 -0.0422 0.132 Uiso 1 1 calc R . . C5 C 0.7802(11) 0.4138(8) -0.0604(7) 0.104(5) Uani 1 1 d D . . H5A H 0.8118 0.3998 -0.0937 0.125 Uiso 1 1 calc R . . H5B H 0.7716 0.3734 -0.0392 0.125 Uiso 1 1 calc R . . C6 C 0.6698(10) 0.4433(7) -0.0831(5) 0.084(4) Uani 1 1 d D . . H6A H 0.6199 0.4074 -0.1063 0.100 Uiso 1 1 calc R . . H6B H 0.6772 0.4794 -0.1091 0.100 Uiso 1 1 calc R . . N2 N 0.6862(12) -0.3845(7) 0.2899(5) 0.136(5) Uani 1 1 d DU . . C7 C 0.6827(17) -0.4471(9) 0.2487(7) 0.162(6) Uani 1 1 d DU . . H7 H 0.6361 -0.4823 0.2605 0.195 Uiso 1 1 calc R . . C8 C 0.794(2) -0.4727(11) 0.2584(10) 0.181(8) Uani 1 1 d DU . . H8A H 0.7940 -0.5153 0.2341 0.218 Uiso 1 1 calc R . . H8B H 0.8209 -0.4815 0.2998 0.218 Uiso 1 1 calc R . . C9 C 0.8636(19) -0.4183(16) 0.2411(12) 0.212(9) Uani 1 1 d DU . . H9A H 0.8729 -0.3789 0.2701 0.254 Uiso 1 1 calc R . . H9B H 0.9355 -0.4358 0.2415 0.254 Uiso 1 1 calc R . . C10 C 0.815(2) -0.3960(17) 0.1818(14) 0.232(11) Uani 1 1 d DU . . H10A H 0.8226 -0.4329 0.1528 0.278 Uiso 1 1 calc R . . H10B H 0.8598 -0.3568 0.1754 0.278 Uiso 1 1 calc R . . C11 C 0.700(3) -0.3764(14) 0.1681(11) 0.220(11) Uani 1 1 d DU . . H11A H 0.6751 -0.3707 0.1259 0.264 Uiso 1 1 calc R . . H11B H 0.6927 -0.3330 0.1898 0.264 Uiso 1 1 calc R . . C12 C 0.6312(18) -0.4327(14) 0.1862(9) 0.194(8) Uani 1 1 d DU . . H12A H 0.5569 -0.4181 0.1834 0.233 Uiso 1 1 calc R . . H12B H 0.6283 -0.4741 0.1600 0.233 Uiso 1 1 calc R . . C13 C 0.4186(10) 0.4917(6) 0.3118(5) 0.075(3) Uani 1 1 d D . . H13A H 0.4888 0.5077 0.3056 0.090 Uiso 1 1 calc R . . H13B H 0.3805 0.4658 0.2753 0.090 Uiso 1 1 calc R . . C14 C 0.3558(11) 0.5523(6) 0.3195(5) 0.082(3) Uani 1 1 d D . . H14A H 0.3922 0.5795 0.3556 0.098 Uiso 1 1 calc R . . H14B H 0.2834 0.5379 0.3236 0.098 Uiso 1 1 calc R . . C15 C 0.3450(12) 0.5962(7) 0.2669(6) 0.095(4) Uani 1 1 d D . . H15A H 0.4170 0.6155 0.2667 0.114 Uiso 1 1 calc R . . H15B H 0.3204 0.5665 0.2306 0.114 Uiso 1 1 calc R . . C16 C 0.2695(14) 0.6528(9) 0.2658(7) 0.125(6) Uani 1 1 d D . . H16A H 0.2686 0.6779 0.2313 0.187 Uiso 1 1 calc R . . H16B H 0.2936 0.6831 0.3010 0.187 Uiso 1 1 calc R . . H16C H 0.1970 0.6343 0.2642 0.187 Uiso 1 1 calc R . . C17 C 0.3421(10) 0.4271(7) 0.3863(5) 0.079(3) Uani 1 1 d . . . H17A H 0.3226 0.4703 0.4037 0.094 Uiso 1 1 calc R . . H17B H 0.3619 0.3964 0.4181 0.094 Uiso 1 1 calc R . . C18 C 0.2412(12) 0.3955(8) 0.3413(6) 0.097(4) Uani 1 1 d . . . H18A H 0.2542 0.3483 0.3295 0.116 Uiso 1 1 calc R . . H18B H 0.2274 0.4213 0.3061 0.116 Uiso 1 1 calc R . . C19 C 0.1409(15) 0.3971(14) 0.3691(8) 0.159(9) Uani 1 1 d . . . H19A H 0.1612 0.3765 0.4069 0.191 Uiso 1 1 calc R . . H19B H 0.1275 0.4451 0.3779 0.191 Uiso 1 1 calc R . . C20 C 0.0421(19) 0.3655(19) 0.3380(11) 0.230(15) Uani 1 1 d . . . H20A H -0.0112 0.3698 0.3619 0.345 Uiso 1 1 calc R . . H20B H 0.0524 0.3176 0.3290 0.345 Uiso 1 1 calc R . . H20C H 0.0166 0.3874 0.3017 0.345 Uiso 1 1 calc R . . C21 C 0.4781(11) 0.3750(6) 0.3348(5) 0.075(3) Uani 1 1 d . . . H21A H 0.5415 0.3860 0.3191 0.090 Uiso 1 1 calc R . . H21B H 0.4199 0.3570 0.3017 0.090 Uiso 1 1 calc R . . C22 C 0.5077(13) 0.3187(7) 0.3777(5) 0.091(4) Uani 1 1 d . . . H22A H 0.4413 0.2993 0.3862 0.109 Uiso 1 1 calc R . . H22B H 0.5537 0.3386 0.4149 0.109 Uiso 1 1 calc R . . C23 C 0.5683(18) 0.2613(8) 0.3519(7) 0.121(6) Uani 1 1 d . . . H23A H 0.5329 0.2511 0.3103 0.146 Uiso 1 1 calc R . . H23B H 0.5620 0.2200 0.3724 0.146 Uiso 1 1 calc R . . C24 C 0.6910(18) 0.2794(11) 0.3571(7) 0.138(7) Uani 1 1 d . . . H24A H 0.7236 0.2416 0.3396 0.207 Uiso 1 1 calc R . . H24B H 0.7274 0.2878 0.3983 0.207 Uiso 1 1 calc R . . H24C H 0.6981 0.3199 0.3365 0.207 Uiso 1 1 calc R . . C25 C 0.5307(10) 0.4719(6) 0.4143(4) 0.069(3) Uani 1 1 d . . . H25A H 0.5091 0.5176 0.4254 0.082 Uiso 1 1 calc R . . H25B H 0.5321 0.4442 0.4478 0.082 Uiso 1 1 calc R . . C26 C 0.6445(10) 0.4783(7) 0.4053(5) 0.079(3) Uani 1 1 d . . . H26A H 0.6476 0.5123 0.3768 0.095 Uiso 1 1 calc R . . H26B H 0.6643 0.4345 0.3891 0.095 Uiso 1 1 calc R . . C27 C 0.7261(12) 0.4998(8) 0.4634(6) 0.097(4) Uani 1 1 d . . . H27A H 0.7186 0.4677 0.4927 0.117 Uiso 1 1 calc R . . H27B H 0.7090 0.5451 0.4779 0.117 Uiso 1 1 calc R . . C28 C 0.8452(13) 0.5018(11) 0.4567(9) 0.136(6) Uani 1 1 d . . . H28A H 0.8935 0.5150 0.4946 0.205 Uiso 1 1 calc R . . H28B H 0.8538 0.5346 0.4287 0.205 Uiso 1 1 calc R . . H28C H 0.8628 0.4569 0.4426 0.205 Uiso 1 1 calc R . . C29 C 0.9959(8) -0.2822(6) 0.8564(5) 0.064(3) Uani 1 1 d . . . H29A H 1.0137 -0.2744 0.8186 0.077 Uiso 1 1 calc R . . H29B H 1.0645 -0.2874 0.8850 0.077 Uiso 1 1 calc R . . C30 C 0.9290(10) -0.3486(7) 0.8493(7) 0.090(4) Uani 1 1 d . . . H30A H 0.9058 -0.3549 0.8859 0.108 Uiso 1 1 calc R . . H30B H 0.8637 -0.3455 0.8178 0.108 Uiso 1 1 calc R . . C31 C 0.9894(11) -0.4100(7) 0.8348(7) 0.095(4) Uani 1 1 d . . . H31A H 1.0540 -0.4133 0.8667 0.114 Uiso 1 1 calc R . . H31B H 1.0142 -0.4028 0.7988 0.114 Uiso 1 1 calc R . . C32 C 0.9240(13) -0.4773(8) 0.8260(8) 0.114(5) Uani 1 1 d . . . H32A H 0.9688 -0.5140 0.8170 0.171 Uiso 1 1 calc R . . H32B H 0.8609 -0.4753 0.7937 0.171 Uiso 1 1 calc R . . H32C H 0.9007 -0.4857 0.8618 0.171 Uiso 1 1 calc R . . C33 C 1.0207(8) -0.1579(6) 0.8786(5) 0.066(3) Uani 1 1 d . . . H33A H 1.0893 -0.1659 0.9062 0.079 Uiso 1 1 calc R . . H33B H 1.0359 -0.1553 0.8395 0.079 Uiso 1 1 calc R . . C34 C 0.9806(10) -0.0896(6) 0.8970(6) 0.077(3) Uani 1 1 d . . . H34A H 0.9668 -0.0915 0.9364 0.092 Uiso 1 1 calc R . . H34B H 0.9117 -0.0814 0.8698 0.092 Uiso 1 1 calc R . . C35 C 1.0607(11) -0.0300(7) 0.8976(6) 0.091(4) Uani 1 1 d . . . H35A H 1.1302 -0.0390 0.9240 0.109 Uiso 1 1 calc R . . H35B H 1.0732 -0.0277 0.8579 0.109 Uiso 1 1 calc R . . C36 C 1.0241(12) 0.0382(7) 0.9171(7) 0.099(4) Uani 1 1 d . . . H36A H 1.0794 0.0732 0.9169 0.149 Uiso 1 1 calc R . . H36B H 1.0125 0.0367 0.9566 0.149 Uiso 1 1 calc R . . H36C H 0.9569 0.0485 0.8903 0.149 Uiso 1 1 calc R . . C37 C 0.9205(8) -0.2283(7) 0.9373(5) 0.068(3) Uani 1 1 d . . . H37A H 0.8699 -0.2677 0.9339 0.082 Uiso 1 1 calc R . . H37B H 0.8841 -0.1880 0.9489 0.082 Uiso 1 1 calc R . . C38 C 1.0213(10) -0.2387(9) 0.9870(6) 0.097(4) Uani 1 1 d . . . H38A H 1.0600 -0.2779 0.9753 0.116 Uiso 1 1 calc R . . H38B H 1.0705 -0.1983 0.9926 0.116 Uiso 1 1 calc R . . C39 C 0.9912(11) -0.2508(9) 1.0443(6) 0.097(4) Uani 1 1 d . . . H39A H 1.0574 -0.2471 1.0758 0.116 Uiso 1 1 calc R . . H39B H 0.9441 -0.2145 1.0529 0.116 Uiso 1 1 calc R . . C40 C 0.9355(14) -0.3170(9) 1.0456(7) 0.112(5) Uani 1 1 d . . . H40A H 0.9178 -0.3201 1.0836 0.168 Uiso 1 1 calc R . . H40B H 0.9827 -0.3534 1.0391 0.168 Uiso 1 1 calc R . . H40C H 0.8693 -0.3212 1.0148 0.168 Uiso 1 1 calc R . . C41 C 0.8337(7) -0.2092(6) 0.8338(4) 0.062(3) Uani 1 1 d . . . H41A H 0.8000 -0.1696 0.8489 0.075 Uiso 1 1 calc R . . H41B H 0.7858 -0.2493 0.8332 0.075 Uiso 1 1 calc R . . C42 C 0.8409(9) -0.1984(7) 0.7703(5) 0.077(3) Uani 1 1 d . . . H42A H 0.8878 -0.1578 0.7706 0.093 Uiso 1 1 calc R . . H42B H 0.8750 -0.2376 0.7550 0.093 Uiso 1 1 calc R . . C43 C 0.7331(11) -0.1897(8) 0.7297(5) 0.091(4) Uani 1 1 d . . . H43A H 0.6978 -0.1514 0.7456 0.109 Uiso 1 1 calc R . . H43B H 0.6871 -0.2309 0.7283 0.109 Uiso 1 1 calc R . . C44 C 0.7409(12) -0.1766(8) 0.6673(6) 0.100(4) Uani 1 1 d . . . H44A H 0.6686 -0.1722 0.6430 0.150 Uiso 1 1 calc R . . H44B H 0.7751 -0.2144 0.6510 0.150 Uiso 1 1 calc R . . H44C H 0.7839 -0.1348 0.6680 0.150 Uiso 1 1 calc R . . C45 C 0.6455(8) -0.0334(5) 0.2142(4) 0.058(2) Uani 1 1 d . . . H45A H 0.5802 -0.0101 0.2189 0.070 Uiso 1 1 calc R . . H45B H 0.6729 -0.0565 0.2502 0.070 Uiso 1 1 calc R . . C46 C 0.7302(9) 0.0199(6) 0.2088(4) 0.062(3) Uani 1 1 d . . . H46A H 0.7045 0.0428 0.1725 0.074 Uiso 1 1 calc R . . H46B H 0.7972 -0.0026 0.2058 0.074 Uiso 1 1 calc R . . C47 C 0.7552(9) 0.0733(6) 0.2612(5) 0.068(3) Uani 1 1 d . . . H47A H 0.7816 0.0505 0.2975 0.082 Uiso 1 1 calc R . . H47B H 0.6882 0.0956 0.2644 0.082 Uiso 1 1 calc R . . C48 C 0.8411(10) 0.1281(7) 0.2552(6) 0.082(3) Uani 1 1 d . . . H48A H 0.8540 0.1611 0.2890 0.123 Uiso 1 1 calc R . . H48B H 0.8150 0.1511 0.2195 0.123 Uiso 1 1 calc R . . H48C H 0.9083 0.1064 0.2532 0.123 Uiso 1 1 calc R . . C49 C 0.5533(8) -0.0550(5) 0.1062(4) 0.055(2) Uani 1 1 d . . . H49A H 0.5986 -0.0160 0.1004 0.066 Uiso 1 1 calc R . . H49B H 0.5480 -0.0882 0.0724 0.066 Uiso 1 1 calc R . . C50 C 0.4398(9) -0.0303(6) 0.1056(5) 0.072(3) Uani 1 1 d . . . H50A H 0.4428 0.0010 0.1404 0.087 Uiso 1 1 calc R . . H50B H 0.3913 -0.0694 0.1075 0.087 Uiso 1 1 calc R . . C51 C 0.3940(9) 0.0063(6) 0.0498(5) 0.073(3) Uani 1 1 d . . . H51A H 0.4386 0.0478 0.0496 0.088 Uiso 1 1 calc R . . H51B H 0.3969 -0.0235 0.0149 0.088 Uiso 1 1 calc R . . C52 C 0.2767(10) 0.0251(8) 0.0471(7) 0.106(5) Uani 1 1 d . . . H52A H 0.2490 0.0478 0.0114 0.159 Uiso 1 1 calc R . . H52B H 0.2741 0.0555 0.0811 0.159 Uiso 1 1 calc R . . H52C H 0.2325 -0.0160 0.0470 0.159 Uiso 1 1 calc R . . C53 C 0.7141(10) -0.1209(6) 0.1485(4) 0.069(3) Uani 1 1 d . . . H53A H 0.6906 -0.1556 0.1157 0.083 Uiso 1 1 calc R . . H53B H 0.7574 -0.0856 0.1352 0.083 Uiso 1 1 calc R . . C54 C 0.7872(10) -0.1539(6) 0.1997(5) 0.075(3) Uani 1 1 d . . . H54A H 0.8119 -0.1198 0.2330 0.091 Uiso 1 1 calc R . . H54B H 0.7460 -0.1904 0.2127 0.091 Uiso 1 1 calc R . . C55 C 0.8844(12) -0.1830(9) 0.1805(6) 0.103(5) Uani 1 1 d . . . H55A H 0.9234 -0.1463 0.1664 0.123 Uiso 1 1 calc R . . H55B H 0.8586 -0.2172 0.1475 0.123 Uiso 1 1 calc R . . C56 C 0.9632(12) -0.2159(9) 0.2292(7) 0.117(5) Uani 1 1 d . . . H56A H 1.0243 -0.2322 0.2143 0.175 Uiso 1 1 calc R . . H56B H 0.9264 -0.2540 0.2420 0.175 Uiso 1 1 calc R . . H56C H 0.9891 -0.1826 0.2622 0.175 Uiso 1 1 calc R . . C57 C 0.5388(10) -0.1416(6) 0.1803(4) 0.070(3) Uani 1 1 d . . . H57A H 0.5781 -0.1597 0.2168 0.084 Uiso 1 1 calc R . . H57B H 0.4753 -0.1190 0.1886 0.084 Uiso 1 1 calc R . . C58 C 0.4995(14) -0.2012(7) 0.1344(6) 0.100(5) Uani 1 1 d . . . H58A H 0.5603 -0.2303 0.1320 0.120 Uiso 1 1 calc R . . H58B H 0.4726 -0.1837 0.0956 0.120 Uiso 1 1 calc R . . C59 C 0.4078(18) -0.2438(8) 0.1511(6) 0.124(7) Uani 1 1 d . . . H59A H 0.3975 -0.2875 0.1274 0.149 Uiso 1 1 calc R . . H59B H 0.4311 -0.2535 0.1925 0.149 Uiso 1 1 calc R . . C60 C 0.2999(17) -0.2101(13) 0.1422(10) 0.174(10) Uani 1 1 d . . . H60A H 0.2473 -0.2399 0.1538 0.261 Uiso 1 1 calc R . . H60B H 0.2747 -0.2015 0.1011 0.261 Uiso 1 1 calc R . . H60C H 0.3084 -0.1672 0.1662 0.261 Uiso 1 1 calc R . . C61 C 0.7391(18) 0.0961(12) 0.5829(11) 0.149(7) Uani 1 1 d . . . H61A H 0.6754 0.1190 0.5905 0.179 Uiso 1 1 calc R . . H61B H 0.7147 0.0494 0.5674 0.179 Uiso 1 1 calc R . . C62 C 0.8122(18) 0.0917(13) 0.6379(10) 0.146(7) Uani 1 1 d . . . H62A H 0.8235 0.1378 0.6575 0.175 Uiso 1 1 calc R . . H62B H 0.8820 0.0787 0.6299 0.175 Uiso 1 1 calc R . . C63 C 0.786(2) 0.0446(15) 0.6815(13) 0.185(10) Uani 1 1 d . . . H63A H 0.7130 0.0557 0.6856 0.221 Uiso 1 1 calc R . . H63B H 0.7790 -0.0013 0.6614 0.221 Uiso 1 1 calc R . . C64 C 0.847(3) 0.0372(18) 0.7400(12) 0.238(15) Uani 1 1 d . . . H64A H 0.8132 0.0018 0.7575 0.357 Uiso 1 1 calc R . . H64B H 0.8503 0.0801 0.7635 0.357 Uiso 1 1 calc R . . H64C H 0.9206 0.0248 0.7387 0.357 Uiso 1 1 calc R . . C65 C 0.6726(14) 0.1315(11) 0.4842(10) 0.162(8) Uani 1 1 d DU . . H65A H 0.6161 0.1544 0.4997 0.195 Uiso 1 1 calc R . . H65B H 0.6918 0.1604 0.4552 0.195 Uiso 1 1 calc R . . C66 C 0.6248(16) 0.0689(13) 0.4532(10) 0.187(8) Uani 1 1 d DU . . H66A H 0.5880 0.0448 0.4790 0.225 Uiso 1 1 calc R . . H66B H 0.6835 0.0404 0.4459 0.225 Uiso 1 1 calc R . . C67 C 0.5472(16) 0.0739(13) 0.3971(10) 0.187(8) Uani 1 1 d DU . . H67A H 0.4791 0.0847 0.4082 0.225 Uiso 1 1 calc R . . H67B H 0.5710 0.1157 0.3820 0.225 Uiso 1 1 calc R . . C68 C 0.515(2) 0.0278(13) 0.3462(9) 0.198(11) Uani 1 1 d DU . . H68A H 0.4571 0.0470 0.3179 0.297 Uiso 1 1 calc R . . H68B H 0.4891 -0.0152 0.3573 0.297 Uiso 1 1 calc R . . H68C H 0.5764 0.0201 0.3286 0.297 Uiso 1 1 calc R . . C69 C 0.8632(14) 0.0945(14) 0.5138(12) 0.176(10) Uani 1 1 d . . . H69A H 0.8474 0.0457 0.5154 0.212 Uiso 1 1 calc R . . H69B H 0.9288 0.1060 0.5447 0.212 Uiso 1 1 calc R . . C70 C 0.8985(18) 0.1005(11) 0.4551(8) 0.209(15) Uani 1 1 d . . . H70A H 0.8376 0.0833 0.4231 0.250 Uiso 1 1 calc RD . . H70B H 0.9098 0.1492 0.4504 0.250 Uiso 1 1 calc R . . C71 C 0.9878(15) 0.0688(15) 0.4471(10) 0.173(10) Uani 1 1 d . . . H71A H 0.9736 0.0194 0.4463 0.207 Uiso 1 1 calc R . . H71B H 1.0475 0.0816 0.4813 0.207 Uiso 1 1 calc R . . C72 C 1.0244(16) 0.0832(14) 0.3935(8) 0.166(9) Uani 1 1 d . . . H72A H 1.0821 0.0532 0.3890 0.249 Uiso 1 1 calc R . . H72B H 1.0512 0.1303 0.3967 0.249 Uiso 1 1 calc R . . H72C H 0.9640 0.0755 0.3595 0.249 Uiso 1 1 calc R . . C73 C 0.8325(11) 0.2003(7) 0.5600(7) 0.107 Uani 1 1 d DU . . H73A H 0.8851 0.1920 0.5964 0.129 Uiso 1 1 calc R . . H73B H 0.8744 0.2137 0.5318 0.129 Uiso 1 1 calc RD . . C74 C 0.7752(11) 0.2567(7) 0.5727(8) 0.107 Uani 1 1 d DU . . H74A H 0.7638 0.2541 0.6126 0.129 Uiso 1 1 calc R . . H74B H 0.7035 0.2532 0.5455 0.129 Uiso 1 1 calc R . . C75 C 0.8270(11) 0.3267(7) 0.5689(7) 0.107 Uani 1 1 d DU . . H75A H 0.8466 0.3258 0.5306 0.129 Uiso 1 1 calc R . . H75B H 0.7698 0.3596 0.5675 0.129 Uiso 1 1 calc R . . C76 C 0.9201(11) 0.3550(8) 0.6119(7) 0.107 Uani 1 1 d DU . . H76A H 0.9362 0.4012 0.6031 0.161 Uiso 1 1 calc R . . H76B H 0.9820 0.3273 0.6108 0.161 Uiso 1 1 calc R . . H76C H 0.9050 0.3557 0.6508 0.161 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 Mo1 0.0510(5) 0.0515(5) 0.0526(5) 0.0153(4) 0.0215(4) 0.0031(4) Mo2 0.0365(4) 0.0504(5) 0.0538(5) 0.0009(4) 0.0151(3) 0.0045(3) Mo3 0.0467(4) 0.0509(5) 0.0486(5) 0.0129(4) 0.0135(4) -0.0024(4) Mo4 0.0441(4) 0.0499(5) 0.0443(4) -0.0003(3) 0.0164(3) 0.0031(3) Mo5 0.0374(4) 0.0608(5) 0.0489(5) 0.0008(4) 0.0035(3) -0.0069(4) Mo6 0.0352(4) 0.0602(5) 0.0410(4) -0.0026(4) 0.0062(3) 0.0005(3) Mo7 0.0871(7) 0.0646(6) 0.0520(5) 0.0085(4) 0.0225(5) 0.0009(5) Mo8 0.0674(6) 0.0888(7) 0.0472(5) 0.0193(5) 0.0104(4) 0.0063(5) Mo9 0.0885(7) 0.0689(6) 0.0487(5) 0.0012(4) 0.0170(5) -0.0035(5) Mo10 0.0691(7) 0.1437(11) 0.0608(6) 0.0337(7) 0.0199(5) -0.0103(7) Mo11 0.1233(10) 0.1081(10) 0.0651(7) -0.0058(6) 0.0458(7) 0.0276(8) Mo12 0.0771(7) 0.1320(11) 0.0741(7) 0.0348(7) 0.0189(6) 0.0348(7) O1 0.032(3) 0.043(3) 0.040(3) 0.008(2) 0.011(2) 0.001(2) O2 0.050(4) 0.065(4) 0.079(5) -0.007(4) 0.022(3) 0.009(3) O3 0.075(5) 0.066(5) 0.071(5) 0.026(4) 0.024(4) -0.005(4) O4 0.058(4) 0.069(5) 0.061(4) -0.010(3) 0.022(3) 0.007(3) O5 0.048(4) 0.090(5) 0.068(5) -0.006(4) -0.004(3) -0.012(4) O6 0.044(4) 0.082(5) 0.056(4) -0.011(3) 0.004(3) -0.002(3) O7 0.046(4) 0.057(4) 0.070(4) 0.008(3) 0.019(3) -0.013(3) O8 0.050(4) 0.058(4) 0.059(4) 0.006(3) 0.027(3) 0.004(3) O9 0.059(4) 0.048(4) 0.057(4) 0.009(3) 0.022(3) 0.007(3) O10 0.050(4) 0.063(4) 0.044(3) 0.014(3) 0.010(3) 0.004(3) O11 0.043(3) 0.053(4) 0.048(3) -0.005(3) 0.012(3) -0.001(3) O12 0.041(3) 0.047(4) 0.059(4) 0.005(3) 0.009(3) 0.000(3) O13 0.033(3) 0.063(4) 0.053(4) 0.000(3) 0.012(3) 0.004(3) O14 0.035(3) 0.061(4) 0.059(4) 0.007(3) 0.006(3) 0.002(3) O15 0.047(4) 0.070(4) 0.043(3) 0.013(3) 0.002(3) 0.001(3) O16 0.051(4) 0.059(4) 0.041(3) 0.005(3) 0.018(3) -0.003(3) O17 0.039(3) 0.055(4) 0.051(4) 0.002(3) 0.011(3) -0.006(3) O18 0.047(4) 0.063(4) 0.045(3) -0.008(3) 0.007(3) -0.007(3) O19 0.063(4) 0.075(5) 0.042(3) 0.006(3) 0.017(3) 0.008(3) O20 0.108(6) 0.084(6) 0.070(5) 0.017(4) 0.027(5) -0.016(5) O21 0.086(6) 0.126(8) 0.070(5) 0.034(5) 0.000(4) 0.004(5) O22 0.159(9) 0.080(6) 0.076(6) -0.004(5) 0.031(6) -0.001(6) O23 0.102(7) 0.204(12) 0.092(7) 0.046(7) 0.033(6) -0.035(7) O24 0.092(7) 0.197(12) 0.122(8) 0.076(8) 0.025(6) 0.057(7) O25 0.068(5) 0.084(5) 0.060(4) 0.007(4) 0.016(4) -0.007(4) O26 0.081(5) 0.072(5) 0.044(4) 0.007(3) 0.024(3) 0.002(4) O27 0.104(6) 0.078(5) 0.060(4) 0.019(4) 0.022(4) 0.028(5) O28 0.121(7) 0.074(5) 0.071(5) -0.002(4) 0.034(5) 0.010(5) O29 0.082(5) 0.099(6) 0.051(4) 0.029(4) 0.012(4) -0.002(4) O30 0.081(5) 0.074(5) 0.066(5) 0.020(4) 0.018(4) 0.021(4) O31 0.113(7) 0.105(7) 0.047(4) -0.003(4) 0.019(4) 0.002(5) O32 0.083(5) 0.100(6) 0.053(4) 0.023(4) -0.002(4) -0.009(5) O33 0.091(6) 0.093(6) 0.066(5) 0.018(4) 0.005(4) -0.023(5) O34 0.058(5) 0.170(10) 0.087(6) 0.040(6) 0.020(4) 0.008(5) O35 0.099(7) 0.185(11) 0.059(5) -0.016(6) 0.026(5) 0.043(7) O36 0.120(8) 0.126(8) 0.102(7) 0.029(6) 0.055(6) 0.060(6) N3 0.088(6) 0.075(6) 0.042(5) 0.006(4) 0.014(4) -0.006(5) N4 0.037(4) 0.084(6) 0.063(5) -0.001(4) 0.019(4) -0.010(4) N5 0.078(6) 0.063(5) 0.034(4) 0.003(4) 0.018(4) -0.002(4) N6 0.088(8) 0.090(7) 0.149(11) 0.028(7) 0.025(7) -0.007(6) N1 0.064(5) 0.053(5) 0.057(5) 0.015(4) 0.022(4) 0.003(4) C1 0.068(7) 0.050(6) 0.069(7) 0.024(5) 0.024(5) 0.003(5) C2 0.095(9) 0.053(7) 0.081(8) 0.005(6) 0.019(7) -0.006(6) C3 0.080(9) 0.078(9) 0.107(10) 0.020(8) 0.002(8) -0.008(7) C4 0.063(8) 0.115(12) 0.156(15) 0.013(11) 0.031(9) -0.003(8) C5 0.091(10) 0.101(11) 0.140(13) 0.005(10) 0.070(10) 0.004(9) C6 0.098(10) 0.084(9) 0.077(8) 0.013(7) 0.038(7) -0.011(7) N2 0.181(13) 0.147(12) 0.098(8) -0.023(8) 0.078(9) 0.021(10) C7 0.222(16) 0.169(15) 0.123(11) -0.022(10) 0.106(12) 0.010(13) C8 0.27(2) 0.135(16) 0.160(15) 0.014(12) 0.093(14) 0.069(14) C9 0.211(17) 0.24(2) 0.20(2) 0.006(19) 0.096(18) 0.023(17) C10 0.29(2) 0.21(2) 0.21(2) 0.040(18) 0.10(2) -0.07(2) C11 0.36(3) 0.17(2) 0.130(15) 0.021(13) 0.06(2) 0.05(2) C12 0.203(17) 0.24(2) 0.131(12) -0.063(14) 0.037(13) 0.008(16) C13 0.095(9) 0.079(8) 0.051(6) 0.014(6) 0.015(6) -0.008(7) C14 0.103(9) 0.069(8) 0.073(8) 0.018(6) 0.015(7) 0.003(7) C15 0.101(10) 0.098(10) 0.090(9) 0.039(8) 0.023(8) -0.006(8) C16 0.144(15) 0.121(14) 0.108(12) 0.043(10) 0.015(11) 0.020(12) C17 0.083(8) 0.091(9) 0.064(7) 0.015(6) 0.019(6) -0.007(7) C18 0.101(10) 0.101(11) 0.082(9) 0.018(8) 0.008(8) -0.019(8) C19 0.097(13) 0.26(3) 0.116(14) 0.060(15) 0.008(11) -0.058(15) C20 0.131(19) 0.39(5) 0.16(2) 0.06(2) 0.006(16) -0.05(2) C21 0.111(9) 0.063(7) 0.047(6) -0.007(5) 0.015(6) -0.002(6) C22 0.131(12) 0.080(9) 0.065(8) 0.016(6) 0.023(8) 0.011(8) C23 0.183(19) 0.092(11) 0.078(10) -0.006(8) 0.008(11) 0.030(12) C24 0.175(19) 0.153(17) 0.085(11) 0.007(10) 0.022(12) 0.068(15) C25 0.090(8) 0.065(7) 0.048(6) 0.004(5) 0.010(6) -0.006(6) C26 0.092(9) 0.075(8) 0.068(7) 0.003(6) 0.015(7) -0.004(7) C27 0.110(11) 0.084(9) 0.092(10) 0.006(7) 0.008(8) 0.016(8) C28 0.084(11) 0.156(17) 0.158(17) 0.010(13) 0.004(11) -0.002(11) C29 0.045(5) 0.080(8) 0.069(7) 0.001(6) 0.020(5) -0.005(5) C30 0.066(8) 0.096(10) 0.113(11) -0.002(8) 0.036(7) -0.016(7) C31 0.079(9) 0.086(10) 0.123(12) 0.012(8) 0.029(8) -0.002(7) C32 0.115(12) 0.086(10) 0.143(14) -0.005(9) 0.040(11) -0.009(9) C33 0.041(5) 0.091(8) 0.067(7) 0.001(6) 0.018(5) -0.015(5) C34 0.068(7) 0.080(8) 0.085(8) -0.003(6) 0.027(6) -0.010(6) C35 0.081(9) 0.098(10) 0.099(10) 0.013(8) 0.030(8) -0.008(7) C36 0.113(11) 0.085(10) 0.103(11) 0.014(8) 0.031(9) -0.002(8) C37 0.047(6) 0.097(9) 0.064(7) 0.004(6) 0.025(5) -0.011(5) C38 0.058(7) 0.156(14) 0.075(8) 0.014(8) 0.013(6) -0.016(8) C39 0.078(9) 0.121(13) 0.090(10) 0.028(9) 0.013(7) 0.009(8) C40 0.120(12) 0.108(12) 0.112(12) 0.014(9) 0.030(10) 0.017(10) C41 0.037(5) 0.083(8) 0.064(6) 0.002(5) 0.010(5) -0.006(5) C42 0.059(7) 0.112(10) 0.059(7) -0.001(6) 0.013(5) -0.005(6) C43 0.082(9) 0.121(11) 0.074(8) 0.027(8) 0.022(7) -0.009(8) C44 0.113(11) 0.118(12) 0.073(8) 0.031(8) 0.021(8) -0.008(9) C45 0.065(6) 0.066(7) 0.046(5) -0.001(5) 0.018(5) -0.002(5) C46 0.068(7) 0.069(7) 0.049(6) 0.010(5) 0.014(5) 0.008(5) C47 0.065(7) 0.075(8) 0.061(7) 0.001(5) 0.010(5) -0.008(6) C48 0.072(8) 0.082(8) 0.085(9) 0.006(7) 0.005(6) -0.011(6) C49 0.076(7) 0.055(6) 0.033(5) 0.001(4) 0.011(4) -0.007(5) C50 0.068(7) 0.081(8) 0.070(7) 0.007(6) 0.021(6) -0.003(6) C51 0.066(7) 0.072(7) 0.075(8) 0.005(6) 0.000(6) -0.006(6) C52 0.070(8) 0.088(10) 0.139(13) -0.004(9) -0.015(8) -0.004(7) C53 0.094(8) 0.071(7) 0.048(6) 0.006(5) 0.027(6) 0.018(6) C54 0.105(9) 0.069(7) 0.057(6) 0.014(5) 0.023(6) 0.022(7) C55 0.114(11) 0.123(12) 0.082(9) 0.023(8) 0.036(8) 0.038(10) C56 0.095(11) 0.138(14) 0.121(13) 0.027(11) 0.024(9) 0.029(10) C57 0.090(8) 0.079(8) 0.043(6) 0.004(5) 0.019(5) -0.017(6) C58 0.152(13) 0.078(9) 0.063(8) 0.005(6) 0.016(8) -0.030(9) C59 0.191(19) 0.097(11) 0.071(9) 0.013(8) 0.007(11) -0.064(12) C60 0.116(15) 0.22(3) 0.167(19) 0.071(18) -0.006(14) -0.086(17) C61 0.140(17) 0.131(17) 0.18(2) 0.014(15) 0.048(17) -0.003(13) C62 0.131(16) 0.17(2) 0.116(16) -0.020(15) 0.007(13) -0.009(15) C63 0.22(3) 0.19(3) 0.15(2) 0.01(2) 0.06(2) 0.02(2) C64 0.27(3) 0.30(4) 0.13(2) 0.01(2) 0.01(2) -0.04(3) C65 0.081(11) 0.185(18) 0.21(2) -0.005(15) 0.011(10) 0.033(11) C66 0.102(11) 0.223(18) 0.211(18) -0.041(14) -0.005(9) 0.042(11) C67 0.102(11) 0.223(18) 0.211(18) -0.041(14) -0.005(9) 0.042(11) C68 0.26(3) 0.21(3) 0.125(15) 0.000(13) 0.057(15) 0.05(2) C69 0.060(10) 0.23(3) 0.23(3) 0.03(2) 0.014(13) 0.033(13) C70 0.098(15) 0.35(4) 0.18(2) 0.15(3) -0.002(15) -0.04(2) C71 0.060(10) 0.28(3) 0.17(2) 0.07(2) 0.007(12) -0.026(14) C72 0.116(14) 0.27(3) 0.110(14) 0.057(16) 0.010(11) -0.051(16) C73 0.086 0.092 0.144 0.026 0.024 -0.004 C74 0.086 0.092 0.144 0.026 0.024 -0.004 C75 0.086 0.092 0.144 0.026 0.024 -0.004 C76 0.086 0.092 0.144 0.026 0.024 -0.004 _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 Mo1 N1 1.702(7) . ? Mo1 O10 1.946(6) . ? Mo1 O9 1.954(6) . ? Mo1 O8 1.965(6) . ? Mo1 O7 1.976(7) . ? Mo1 O1 2.231(5) . ? Mo2 O2 1.683(6) . ? Mo2 O14 1.873(6) . ? Mo2 O8 1.889(6) . ? Mo2 O12 1.948(6) . ? Mo2 O11 1.983(6) . ? Mo2 O1 2.332(5) . ? Mo3 O3 1.681(6) . ? Mo3 O15 1.899(6) . ? Mo3 O12 1.917(6) . ? Mo3 O17 1.931(6) . ? Mo3 O16 1.940(6) . ? Mo3 O1 2.339(5) . ? Mo4 O4 1.687(6) . ? Mo4 O9 1.894(6) . ? Mo4 O13 1.897(6) . ? Mo4 O16 1.917(6) . ? Mo4 O18 1.988(6) . ? Mo4 O1 2.342(5) . ? Mo5 O5 1.678(6) . ? Mo5 O7 1.883(6) . ? Mo5 O18 1.891(6) . ? Mo5 O15 1.946(6) . ? Mo5 O14 2.001(6) . ? Mo5 O1 2.337(5) . ? Mo6 O6 1.691(6) . ? Mo6 O10 1.895(6) . ? Mo6 O11 1.899(6) . ? Mo6 O17 1.916(6) . ? Mo6 O13 1.990(6) . ? Mo6 O1 2.322(5) . ? Mo7 O20 1.692(8) . ? Mo7 O28 1.895(8) . ? Mo7 O26 1.898(7) . ? Mo7 O25 1.915(7) . ? Mo7 O27 1.935(8) . ? Mo7 O19 2.338(7) . ? Mo8 O21 1.673(8) . ? Mo8 O31 1.908(8) . ? Mo8 O30 1.921(8) . ? Mo8 O29 1.928(8) . ? Mo8 O25 1.938(7) . ? Mo8 O19 2.304(7) . ? Mo9 O22 1.671(9) . ? Mo9 O32 1.897(8) . ? Mo9 O33 1.913(8) . ? Mo9 O30 1.937(7) . ? Mo9 O26 1.938(7) . ? Mo9 O19 2.333(7) . ? Mo10 O23 1.684(9) . ? Mo10 O34 1.913(9) . ? Mo10 O35 1.923(11) . ? Mo10 O29 1.929(8) . ? Mo10 O33 1.951(9) . ? Mo10 O19 2.317(7) . ? Mo11 N2 1.748(10) . ? Mo11 O31 1.918(9) . ? Mo11 O35 1.924(12) . ? Mo11 O28 1.936(9) . ? Mo11 O36 1.968(10) . ? Mo11 O19 2.252(7) . ? Mo12 O24 1.670(9) . ? Mo12 O36 1.878(10) . ? Mo12 O27 1.928(9) . ? Mo12 O32 1.934(9) . ? Mo12 O34 1.943(9) . ? Mo12 O19 2.338(7) . ? N3 C21 1.506(14) . ? N3 C17 1.511(14) . ? N3 C25 1.536(13) . ? N3 C13 1.553(13) . ? N4 C29 1.508(13) . ? N4 C33 1.509(13) . ? N4 C37 1.518(12) . ? N4 C41 1.518(12) . ? N5 C57 1.514(13) . ? N5 C53 1.523(13) . ? N5 C45 1.526(12) . ? N5 C49 1.532(12) . ? N6 C61 1.46(2) . ? N6 C69 1.51(2) . ? N6 C65 1.51(2) . ? N6 C73 1.549(18) . ? N1 C1 1.479(10) . ? C1 C2 1.500(14) . ? C1 C6 1.508(14) . ? C1 H1 0.9800 . ? C2 C3 1.497(15) . ? C2 H2A 0.9700 . ? C2 H2B 0.9700 . ? C3 C4 1.483(18) . ? C3 H3A 0.9700 . ? C3 H3B 0.9700 . ? C4 C5 1.508(19) . ? C4 H4A 0.9700 . ? C4 H4B 0.9700 . ? C5 C6 1.506(17) . ? C5 H5A 0.9700 . ? C5 H5B 0.9700 . ? C6 H6A 0.9700 . ? C6 H6B 0.9700 . ? N2 C7 1.487(11) . ? C7 C8 1.46(2) . ? C7 C12 1.49(2) . ? C7 H7 0.9800 . ? C8 C9 1.49(2) . ? C8 H8A 0.9700 . ? C8 H8B 0.9700 . ? C9 C10 1.47(2) . ? C9 H9A 0.9700 . ? C9 H9B 0.9700 . ? C10 C11 1.48(2) . ? C10 H10A 0.9700 . ? C10 H10B 0.9700 . ? C11 C12 1.51(2) . ? C11 H11A 0.9700 . ? C11 H11B 0.9700 . ? C12 H12A 0.9700 . ? C12 H12B 0.9700 . ? C13 C14 1.459(14) . ? C13 H13A 0.9700 . ? C13 H13B 0.9700 . ? C14 C15 1.514(14) . ? C14 H14A 0.9700 . ? C14 H14B 0.9700 . ? C15 C16 1.468(16) . ? C15 H15A 0.9700 . ? C15 H15B 0.9700 . ? C16 H16A 0.9600 . ? C16 H16B 0.9600 . ? C16 H16C 0.9600 . ? C17 C18 1.529(17) . ? C17 H17A 0.9700 . ? C17 H17B 0.9700 . ? C18 C19 1.53(2) . ? C18 H18A 0.9700 . ? C18 H18B 0.9700 . ? C19 C20 1.39(3) . ? C19 H19A 0.9700 . ? C19 H19B 0.9700 . ? C20 H20A 0.9600 . ? C20 H20B 0.9600 . ? C20 H20C 0.9600 . ? C21 C22 1.522(16) . ? C21 H21A 0.9700 . ? C21 H21B 0.9700 . ? C22 C23 1.53(2) . ? C22 H22A 0.9700 . ? C22 H22B 0.9700 . ? C23 C24 1.54(2) . ? C23 H23A 0.9700 . ? C23 H23B 0.9700 . ? C24 H24A 0.9600 . ? C24 H24B 0.9600 . ? C24 H24C 0.9600 . ? C25 C26 1.490(16) . ? C25 H25A 0.9700 . ? C25 H25B 0.9700 . ? C26 C27 1.517(17) . ? C26 H26A 0.9700 . ? C26 H26B 0.9700 . ? C27 C28 1.53(2) . ? C27 H27A 0.9700 . ? C27 H27B 0.9700 . ? C28 H28A 0.9600 . ? C28 H28B 0.9600 . ? C28 H28C 0.9600 . ? C29 C30 1.501(16) . ? C29 H29A 0.9700 . ? C29 H29B 0.9700 . ? C30 C31 1.489(18) . ? C30 H30A 0.9700 . ? C30 H30B 0.9700 . ? C31 C32 1.505(19) . ? C31 H31A 0.9700 . ? C31 H31B 0.9700 . ? C32 H32A 0.9600 . ? C32 H32B 0.9600 . ? C32 H32C 0.9600 . ? C33 C34 1.503(16) . ? C33 H33A 0.9700 . ? C33 H33B 0.9700 . ? C34 C35 1.510(17) . ? C34 H34A 0.9700 . ? C34 H34B 0.9700 . ? C35 C36 1.490(19) . ? C35 H35A 0.9700 . ? C35 H35B 0.9700 . ? C36 H36A 0.9600 . ? C36 H36B 0.9600 . ? C36 H36C 0.9600 . ? C37 C38 1.531(16) . ? C37 H37A 0.9700 . ? C37 H37B 0.9700 . ? C38 C39 1.490(17) . ? C38 H38A 0.9700 . ? C38 H38B 0.9700 . ? C39 C40 1.45(2) . ? C39 H39A 0.9700 . ? C39 H39B 0.9700 . ? C40 H40A 0.9600 . ? C40 H40B 0.9600 . ? C40 H40C 0.9600 . ? C41 C42 1.520(14) . ? C41 H41A 0.9700 . ? C41 H41B 0.9700 . ? C42 C43 1.480(16) . ? C42 H42A 0.9700 . ? C42 H42B 0.9700 . ? C43 C44 1.506(16) . ? C43 H43A 0.9700 . ? C43 H43B 0.9700 . ? C44 H44A 0.9600 . ? C44 H44B 0.9600 . ? C44 H44C 0.9600 . ? C45 C46 1.496(14) . ? C45 H45A 0.9700 . ? C45 H45B 0.9700 . ? C46 C47 1.514(14) . ? C46 H46A 0.9700 . ? C46 H46B 0.9700 . ? C47 C48 1.530(15) . ? C47 H47A 0.9700 . ? C47 H47B 0.9700 . ? C48 H48A 0.9600 . ? C48 H48B 0.9600 . ? C48 H48C 0.9600 . ? C49 C50 1.511(14) . ? C49 H49A 0.9700 . ? C49 H49B 0.9700 . ? C50 C51 1.520(15) . ? C50 H50A 0.9700 . ? C50 H50B 0.9700 . ? C51 C52 1.512(16) . ? C51 H51A 0.9700 . ? C51 H51B 0.9700 . ? C52 H52A 0.9600 . ? C52 H52B 0.9600 . ? C52 H52C 0.9600 . ? C53 C54 1.514(14) . ? C53 H53A 0.9700 . ? C53 H53B 0.9700 . ? C54 C55 1.501(16) . ? C54 H54A 0.9700 . ? C54 H54B 0.9700 . ? C55 C56 1.508(18) . ? C55 H55A 0.9700 . ? C55 H55B 0.9700 . ? C56 H56A 0.9600 . ? C56 H56B 0.9600 . ? C56 H56C 0.9600 . ? C57 C58 1.511(16) . ? C57 H57A 0.9700 . ? C57 H57B 0.9700 . ? C58 C59 1.53(2) . ? C58 H58A 0.9700 . ? C58 H58B 0.9700 . ? C59 C60 1.50(3) . ? C59 H59A 0.9700 . ? C59 H59B 0.9700 . ? C60 H60A 0.9600 . ? C60 H60B 0.9600 . ? C60 H60C 0.9600 . ? C61 C62 1.40(3) . ? C61 H61A 0.9700 . ? C61 H61B 0.9700 . ? C62 C63 1.49(3) . ? C62 H62A 0.9700 . ? C62 H62B 0.9700 . ? C63 C64 1.42(3) . ? C63 H63A 0.9700 . ? C63 H63B 0.9700 . ? C64 H64A 0.9600 . ? C64 H64B 0.9600 . ? C64 H64C 0.9600 . ? C65 C66 1.418(19) . ? C65 H65A 0.9700 . ? C65 H65B 0.9700 . ? C66 C67 1.444(19) . ? C66 H66A 0.9700 . ? C66 H66B 0.9700 . ? C67 C68 1.407(15) . ? C67 H67A 0.9700 . ? C67 H67B 0.9700 . ? C68 H68A 0.9600 . ? C68 H68B 0.9600 . ? C68 H68C 0.9600 . ? C69 C70 1.53(3) . ? C69 H69A 0.9700 . ? C69 H69B 0.9700 . ? C70 C71 1.34(3) . ? C70 H70A 0.9700 . ? C70 H70B 0.9700 . ? C71 C72 1.46(2) . ? C71 H71A 0.9700 . ? C71 H71B 0.9700 . ? C72 H72A 0.9600 . ? C72 H72B 0.9600 . ? C72 H72C 0.9600 . ? C73 C74 1.376(13) . ? C73 H73A 0.9700 . ? C73 H73B 0.9700 . ? C74 C75 1.510(15) . ? C74 H74A 0.9700 . ? C74 H74B 0.9700 . ? C75 C76 1.421(13) . ? C75 H75A 0.9700 . ? C75 H75B 0.9700 . ? C76 H76A 0.9600 . ? C76 H76B 0.9600 . ? C76 H76C 0.9600 . ? 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 N1 Mo1 O10 102.0(3) . . ? N1 Mo1 O9 101.1(3) . . ? O10 Mo1 O9 88.5(3) . . ? N1 Mo1 O8 102.8(3) . . ? O10 Mo1 O8 87.9(3) . . ? O9 Mo1 O8 156.1(3) . . ? N1 Mo1 O7 101.7(3) . . ? O10 Mo1 O7 156.2(2) . . ? O9 Mo1 O7 87.0(3) . . ? O8 Mo1 O7 86.9(3) . . ? N1 Mo1 O1 179.0(3) . . ? O10 Mo1 O1 78.2(2) . . ? O9 Mo1 O1 78.0(2) . . ? O8 Mo1 O1 78.1(2) . . ? O7 Mo1 O1 78.0(2) . . ? O2 Mo2 O14 103.4(3) . . ? O2 Mo2 O8 103.3(3) . . ? O14 Mo2 O8 90.0(3) . . ? O2 Mo2 O12 103.1(3) . . ? O14 Mo2 O12 88.2(3) . . ? O8 Mo2 O12 153.2(2) . . ? O2 Mo2 O11 103.2(3) . . ? O14 Mo2 O11 153.2(2) . . ? O8 Mo2 O11 86.4(3) . . ? O12 Mo2 O11 83.3(2) . . ? O2 Mo2 O1 179.0(3) . . ? O14 Mo2 O1 77.5(2) . . ? O8 Mo2 O1 77.1(2) . . ? O12 Mo2 O1 76.5(2) . . ? O11 Mo2 O1 75.8(2) . . ? O3 Mo3 O15 104.2(3) . . ? O3 Mo3 O12 103.1(3) . . ? O15 Mo3 O12 88.0(3) . . ? O3 Mo3 O17 103.1(3) . . ? O15 Mo3 O17 152.7(3) . . ? O12 Mo3 O17 86.9(2) . . ? O3 Mo3 O16 103.7(3) . . ? O15 Mo3 O16 87.0(3) . . ? O12 Mo3 O16 153.2(2) . . ? O17 Mo3 O16 85.5(3) . . ? O3 Mo3 O1 179.1(3) . . ? O15 Mo3 O1 76.7(2) . . ? O12 Mo3 O1 76.9(2) . . ? O17 Mo3 O1 76.1(2) . . ? O16 Mo3 O1 76.4(2) . . ? O4 Mo4 O9 104.5(3) . . ? O4 Mo4 O13 103.4(3) . . ? O9 Mo4 O13 89.2(3) . . ? O4 Mo4 O16 102.4(3) . . ? O9 Mo4 O16 152.8(2) . . ? O13 Mo4 O16 88.3(3) . . ? O4 Mo4 O18 102.8(3) . . ? O9 Mo4 O18 85.7(3) . . ? O13 Mo4 O18 153.7(2) . . ? O16 Mo4 O18 84.7(3) . . ? O4 Mo4 O1 178.7(3) . . ? O9 Mo4 O1 76.4(2) . . ? O13 Mo4 O1 77.5(2) . . ? O16 Mo4 O1 76.7(2) . . ? O18 Mo4 O1 76.3(2) . . ? O5 Mo5 O7 103.9(3) . . ? O5 Mo5 O18 105.1(3) . . ? O7 Mo5 O18 90.7(3) . . ? O5 Mo5 O15 102.9(3) . . ? O7 Mo5 O15 152.7(3) . . ? O18 Mo5 O15 87.7(3) . . ? O5 Mo5 O14 101.6(3) . . ? O7 Mo5 O14 85.8(3) . . ? O18 Mo5 O14 153.1(2) . . ? O15 Mo5 O14 83.4(3) . . ? O5 Mo5 O1 176.5(3) . . ? O7 Mo5 O1 77.1(2) . . ? O18 Mo5 O1 78.2(2) . . ? O15 Mo5 O1 75.8(2) . . ? O14 Mo5 O1 75.1(2) . . ? O6 Mo6 O10 104.3(3) . . ? O6 Mo6 O11 103.3(3) . . ? O10 Mo6 O11 89.6(3) . . ? O6 Mo6 O17 101.9(3) . . ? O10 Mo6 O17 153.4(3) . . ? O11 Mo6 O17 88.7(3) . . ? O6 Mo6 O13 102.8(3) . . ? O10 Mo6 O13 85.6(3) . . ? O11 Mo6 O13 153.8(2) . . ? O17 Mo6 O13 84.4(3) . . ? O6 Mo6 O1 178.3(3) . . ? O10 Mo6 O1 77.0(2) . . ? O11 Mo6 O1 77.6(2) . . ? O17 Mo6 O1 76.8(2) . . ? O13 Mo6 O1 76.2(2) . . ? O20 Mo7 O28 101.5(4) . . ? O20 Mo7 O26 104.2(4) . . ? O28 Mo7 O26 154.3(3) . . ? O20 Mo7 O25 104.0(4) . . ? O28 Mo7 O25 86.9(3) . . ? O26 Mo7 O25 87.5(3) . . ? O20 Mo7 O27 102.8(4) . . ? O28 Mo7 O27 87.1(4) . . ? O26 Mo7 O27 86.7(3) . . ? O25 Mo7 O27 153.2(3) . . ? O20 Mo7 O19 178.6(3) . . ? O28 Mo7 O19 77.1(3) . . ? O26 Mo7 O19 77.2(3) . . ? O25 Mo7 O19 76.1(3) . . ? O27 Mo7 O19 77.0(3) . . ? O21 Mo8 O31 102.4(4) . . ? O21 Mo8 O30 103.8(4) . . ? O31 Mo8 O30 153.8(3) . . ? O21 Mo8 O29 103.2(4) . . ? O31 Mo8 O29 87.7(4) . . ? O30 Mo8 O29 87.6(3) . . ? O21 Mo8 O25 103.4(4) . . ? O31 Mo8 O25 86.7(3) . . ? O30 Mo8 O25 86.0(3) . . ? O29 Mo8 O25 153.4(3) . . ? O21 Mo8 O19 179.2(4) . . ? O31 Mo8 O19 76.9(3) . . ? O30 Mo8 O19 77.0(3) . . ? O29 Mo8 O19 76.8(3) . . ? O25 Mo8 O19 76.6(3) . . ? O22 Mo9 O32 104.5(4) . . ? O22 Mo9 O33 102.5(4) . . ? O32 Mo9 O33 88.2(4) . . ? O22 Mo9 O30 103.2(4) . . ? O32 Mo9 O30 152.2(3) . . ? O33 Mo9 O30 86.6(3) . . ? O22 Mo9 O26 104.2(4) . . ? O32 Mo9 O26 86.9(3) . . ? O33 Mo9 O26 153.3(3) . . ? O30 Mo9 O26 85.6(3) . . ? O22 Mo9 O19 178.8(4) . . ? O32 Mo9 O19 76.3(3) . . ? O33 Mo9 O19 76.7(3) . . ? O30 Mo9 O19 75.9(3) . . ? O26 Mo9 O19 76.6(3) . . ? O23 Mo10 O34 103.4(5) . . ? O23 Mo10 O35 106.2(5) . . ? O34 Mo10 O35 87.2(5) . . ? O23 Mo10 O29 103.5(4) . . ? O34 Mo10 O29 153.1(3) . . ? O35 Mo10 O29 87.3(4) . . ? O23 Mo10 O33 102.1(5) . . ? O34 Mo10 O33 86.9(4) . . ? O35 Mo10 O33 151.6(4) . . ? O29 Mo10 O33 85.5(3) . . ? O23 Mo10 O19 178.6(5) . . ? O34 Mo10 O19 76.6(3) . . ? O35 Mo10 O19 75.2(4) . . ? O29 Mo10 O19 76.5(3) . . ? O33 Mo10 O19 76.4(3) . . ? N2 Mo11 O31 102.0(6) . . ? N2 Mo11 O35 105.8(5) . . ? O31 Mo11 O35 86.7(4) . . ? N2 Mo11 O28 98.9(5) . . ? O31 Mo11 O28 89.6(4) . . ? O35 Mo11 O28 155.2(3) . . ? N2 Mo11 O36 102.4(6) . . ? O31 Mo11 O36 155.6(4) . . ? O35 Mo11 O36 86.1(4) . . ? O28 Mo11 O36 87.3(4) . . ? N2 Mo11 O19 177.4(5) . . ? O31 Mo11 O19 78.0(3) . . ? O35 Mo11 O19 76.8(3) . . ? O28 Mo11 O19 78.4(3) . . ? O36 Mo11 O19 77.7(3) . . ? O24 Mo12 O36 104.1(5) . . ? O24 Mo12 O27 103.7(5) . . ? O36 Mo12 O27 88.5(4) . . ? O24 Mo12 O32 103.1(5) . . ? O36 Mo12 O32 152.8(4) . . ? O27 Mo12 O32 85.4(3) . . ? O24 Mo12 O34 103.5(5) . . ? O36 Mo12 O34 88.0(4) . . ? O27 Mo12 O34 152.7(3) . . ? O32 Mo12 O34 85.5(4) . . ? O24 Mo12 O19 178.4(6) . . ? O36 Mo12 O19 77.3(3) . . ? O27 Mo12 O19 77.2(3) . . ? O32 Mo12 O19 75.6(3) . . ? O34 Mo12 O19 75.6(3) . . ? Mo1 O1 Mo6 90.33(19) . . ? Mo1 O1 Mo2 90.41(18) . . ? Mo6 O1 Mo2 90.24(19) . . ? Mo1 O1 Mo5 90.45(19) . . ? Mo6 O1 Mo5 179.1(3) . . ? Mo2 O1 Mo5 90.20(17) . . ? Mo1 O1 Mo3 179.9(3) . . ? Mo6 O1 Mo3 89.67(18) . . ? Mo2 O1 Mo3 89.65(19) . . ? Mo5 O1 Mo3 89.55(18) . . ? Mo1 O1 Mo4 90.43(19) . . ? Mo6 O1 Mo4 90.10(17) . . ? Mo2 O1 Mo4 179.1(3) . . ? Mo5 O1 Mo4 89.45(19) . . ? Mo3 O1 Mo4 89.51(17) . . ? Mo5 O7 Mo1 114.4(3) . . ? Mo2 O8 Mo1 114.3(3) . . ? Mo4 O9 Mo1 115.1(3) . . ? Mo6 O10 Mo1 114.4(3) . . ? Mo6 O11 Mo2 116.3(3) . . ? Mo3 O12 Mo2 116.9(3) . . ? Mo4 O13 Mo6 116.2(3) . . ? Mo2 O14 Mo5 117.2(3) . . ? Mo3 O15 Mo5 117.9(3) . . ? Mo4 O16 Mo3 117.4(3) . . ? Mo6 O17 Mo3 117.4(3) . . ? Mo5 O18 Mo4 116.1(3) . . ? Mo11 O19 Mo8 90.2(2) . . ? Mo11 O19 Mo10 91.5(2) . . ? Mo8 O19 Mo10 90.3(2) . . ? Mo11 O19 Mo9 178.4(3) . . ? Mo8 O19 Mo9 90.3(2) . . ? Mo10 O19 Mo9 90.1(3) . . ? Mo11 O19 Mo12 90.0(2) . . ? Mo8 O19 Mo12 179.4(3) . . ? Mo10 O19 Mo12 90.2(2) . . ? Mo9 O19 Mo12 89.6(2) . . ? Mo11 O19 Mo7 89.5(3) . . ? Mo8 O19 Mo7 90.2(2) . . ? Mo10 O19 Mo7 178.9(3) . . ? Mo9 O19 Mo7 89.0(2) . . ? Mo12 O19 Mo7 89.3(2) . . ? Mo7 O25 Mo8 117.1(4) . . ? Mo7 O26 Mo9 117.2(3) . . ? Mo12 O27 Mo7 116.5(4) . . ? Mo7 O28 Mo11 115.0(4) . . ? Mo8 O29 Mo10 116.4(3) . . ? Mo8 O30 Mo9 116.8(4) . . ? Mo8 O31 Mo11 115.0(4) . . ? Mo9 O32 Mo12 118.5(4) . . ? Mo9 O33 Mo10 116.8(4) . . ? Mo10 O34 Mo12 117.5(4) . . ? Mo10 O35 Mo11 116.5(4) . . ? Mo12 O36 Mo11 115.0(4) . . ? C21 N3 C17 111.3(9) . . ? C21 N3 C25 111.2(9) . . ? C17 N3 C25 105.6(8) . . ? C21 N3 C13 107.2(8) . . ? C17 N3 C13 111.9(9) . . ? C25 N3 C13 109.7(9) . . ? C29 N4 C33 107.7(7) . . ? C29 N4 C37 109.3(9) . . ? C33 N4 C37 111.0(8) . . ? C29 N4 C41 110.6(8) . . ? C33 N4 C41 110.6(8) . . ? C37 N4 C41 107.6(7) . . ? C57 N5 C53 110.8(8) . . ? C57 N5 C45 107.3(7) . . ? C53 N5 C45 110.4(8) . . ? C57 N5 C49 111.1(8) . . ? C53 N5 C49 107.4(7) . . ? C45 N5 C49 109.9(8) . . ? C61 N6 C69 112.6(16) . . ? C61 N6 C65 107.5(16) . . ? C69 N6 C65 109.8(15) . . ? C61 N6 C73 109.7(15) . . ? C69 N6 C73 99.9(13) . . ? C65 N6 C73 117.3(13) . . ? C1 N1 Mo1 177.5(8) . . ? N1 C1 C2 108.5(8) . . ? N1 C1 C6 110.2(8) . . ? C2 C1 C6 112.4(9) . . ? N1 C1 H1 108.5 . . ? C2 C1 H1 108.5 . . ? C6 C1 H1 108.5 . . ? C3 C2 C1 110.9(10) . . ? C3 C2 H2A 109.5 . . ? C1 C2 H2A 109.5 . . ? C3 C2 H2B 109.5 . . ? C1 C2 H2B 109.5 . . ? H2A C2 H2B 108.0 . . ? C4 C3 C2 112.4(11) . . ? C4 C3 H3A 109.1 . . ? C2 C3 H3A 109.1 . . ? C4 C3 H3B 109.1 . . ? C2 C3 H3B 109.1 . . ? H3A C3 H3B 107.9 . . ? C3 C4 C5 112.9(11) . . ? C3 C4 H4A 109.0 . . ? C5 C4 H4A 109.0 . . ? C3 C4 H4B 109.0 . . ? C5 C4 H4B 109.0 . . ? H4A C4 H4B 107.8 . . ? C6 C5 C4 110.4(12) . . ? C6 C5 H5A 109.6 . . ? C4 C5 H5A 109.6 . . ? C6 C5 H5B 109.6 . . ? C4 C5 H5B 109.6 . . ? H5A C5 H5B 108.1 . . ? C5 C6 C1 111.5(10) . . ? C5 C6 H6A 109.3 . . ? C1 C6 H6A 109.3 . . ? C5 C6 H6B 109.3 . . ? C1 C6 H6B 109.3 . . ? H6A C6 H6B 108.0 . . ? C7 N2 Mo11 174.3(12) . . ? C8 C7 N2 107.9(15) . . ? C8 C7 C12 115.4(15) . . ? N2 C7 C12 110.9(15) . . ? C8 C7 H7 107.4 . . ? N2 C7 H7 107.4 . . ? C12 C7 H7 107.4 . . ? C7 C8 C9 106.7(17) . . ? C7 C8 H8A 110.4 . . ? C9 C8 H8A 110.4 . . ? C7 C8 H8B 110.4 . . ? C9 C8 H8B 110.4 . . ? H8A C8 H8B 108.6 . . ? C10 C9 C8 112(2) . . ? C10 C9 H9A 109.2 . . ? C8 C9 H9A 109.2 . . ? C10 C9 H9B 109.2 . . ? C8 C9 H9B 109.2 . . ? H9A C9 H9B 107.9 . . ? C9 C10 C11 119(2) . . ? C9 C10 H10A 107.6 . . ? C11 C10 H10A 107.6 . . ? C9 C10 H10B 107.6 . . ? C11 C10 H10B 107.6 . . ? H10A C10 H10B 107.0 . . ? C10 C11 C12 108(2) . . ? C10 C11 H11A 110.0 . . ? C12 C11 H11A 110.0 . . ? C10 C11 H11B 110.0 . . ? C12 C11 H11B 110.0 . . ? H11A C11 H11B 108.4 . . ? C7 C12 C11 108.1(17) . . ? C7 C12 H12A 110.1 . . ? C11 C12 H12A 110.1 . . ? C7 C12 H12B 110.1 . . ? C11 C12 H12B 110.1 . . ? H12A C12 H12B 108.4 . . ? C14 C13 N3 119.4(9) . . ? C14 C13 H13A 107.5 . . ? N3 C13 H13A 107.5 . . ? C14 C13 H13B 107.5 . . ? N3 C13 H13B 107.5 . . ? H13A C13 H13B 107.0 . . ? C13 C14 C15 111.0(10) . . ? C13 C14 H14A 109.4 . . ? C15 C14 H14A 109.4 . . ? C13 C14 H14B 109.4 . . ? C15 C14 H14B 109.4 . . ? H14A C14 H14B 108.0 . . ? C16 C15 C14 115.3(11) . . ? C16 C15 H15A 108.4 . . ? C14 C15 H15A 108.4 . . ? C16 C15 H15B 108.4 . . ? C14 C15 H15B 108.4 . . ? H15A C15 H15B 107.5 . . ? 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 . . ? N3 C17 C18 115.3(10) . . ? N3 C17 H17A 108.5 . . ? C18 C17 H17A 108.5 . . ? N3 C17 H17B 108.5 . . ? C18 C17 H17B 108.5 . . ? H17A C17 H17B 107.5 . . ? C17 C18 C19 109.9(12) . . ? C17 C18 H18A 109.7 . . ? C19 C18 H18A 109.7 . . ? C17 C18 H18B 109.7 . . ? C19 C18 H18B 109.7 . . ? H18A C18 H18B 108.2 . . ? C20 C19 C18 120(2) . . ? C20 C19 H19A 107.4 . . ? C18 C19 H19A 107.4 . . ? C20 C19 H19B 107.4 . . ? C18 C19 H19B 107.4 . . ? H19A C19 H19B 106.9 . . ? C19 C20 H20A 109.5 . . ? C19 C20 H20B 109.5 . . ? H20A C20 H20B 109.5 . . ? C19 C20 H20C 109.5 . . ? H20A C20 H20C 109.5 . . ? H20B C20 H20C 109.5 . . ? N3 C21 C22 114.9(9) . . ? N3 C21 H21A 108.5 . . ? C22 C21 H21A 108.5 . . ? N3 C21 H21B 108.5 . . ? C22 C21 H21B 108.5 . . ? H21A C21 H21B 107.5 . . ? C21 C22 C23 111.5(11) . . ? C21 C22 H22A 109.3 . . ? C23 C22 H22A 109.3 . . ? C21 C22 H22B 109.3 . . ? C23 C22 H22B 109.3 . . ? H22A C22 H22B 108.0 . . ? C22 C23 C24 113.8(14) . . ? C22 C23 H23A 108.8 . . ? C24 C23 H23A 108.8 . . ? C22 C23 H23B 108.8 . . ? C24 C23 H23B 108.8 . . ? H23A C23 H23B 107.7 . . ? C23 C24 H24A 109.5 . . ? C23 C24 H24B 109.5 . . ? H24A C24 H24B 109.5 . . ? C23 C24 H24C 109.5 . . ? H24A C24 H24C 109.5 . . ? H24B C24 H24C 109.5 . . ? C26 C25 N3 117.1(9) . . ? C26 C25 H25A 108.0 . . ? N3 C25 H25A 108.0 . . ? C26 C25 H25B 108.0 . . ? N3 C25 H25B 108.0 . . ? H25A C25 H25B 107.3 . . ? C25 C26 C27 111.2(10) . . ? C25 C26 H26A 109.4 . . ? C27 C26 H26A 109.4 . . ? C25 C26 H26B 109.4 . . ? C27 C26 H26B 109.4 . . ? H26A C26 H26B 108.0 . . ? C26 C27 C28 112.7(13) . . ? C26 C27 H27A 109.1 . . ? C28 C27 H27A 109.1 . . ? C26 C27 H27B 109.1 . . ? C28 C27 H27B 109.1 . . ? H27A C27 H27B 107.8 . . ? C27 C28 H28A 109.5 . . ? C27 C28 H28B 109.5 . . ? H28A C28 H28B 109.5 . . ? C27 C28 H28C 109.5 . . ? H28A C28 H28C 109.5 . . ? H28B C28 H28C 109.5 . . ? C30 C29 N4 115.8(8) . . ? C30 C29 H29A 108.3 . . ? N4 C29 H29A 108.3 . . ? C30 C29 H29B 108.3 . . ? N4 C29 H29B 108.3 . . ? H29A C29 H29B 107.4 . . ? C31 C30 C29 113.3(10) . . ? C31 C30 H30A 108.9 . . ? C29 C30 H30A 108.9 . . ? C31 C30 H30B 108.9 . . ? C29 C30 H30B 108.9 . . ? H30A C30 H30B 107.7 . . ? C30 C31 C32 114.9(11) . . ? C30 C31 H31A 108.6 . . ? C32 C31 H31A 108.6 . . ? C30 C31 H31B 108.6 . . ? C32 C31 H31B 108.6 . . ? H31A C31 H31B 107.5 . . ? C31 C32 H32A 109.5 . . ? C31 C32 H32B 109.5 . . ? H32A C32 H32B 109.5 . . ? C31 C32 H32C 109.5 . . ? H32A C32 H32C 109.5 . . ? H32B C32 H32C 109.5 . . ? C34 C33 N4 115.4(8) . . ? C34 C33 H33A 108.4 . . ? N4 C33 H33A 108.4 . . ? C34 C33 H33B 108.4 . . ? N4 C33 H33B 108.4 . . ? H33A C33 H33B 107.5 . . ? C33 C34 C35 113.3(10) . . ? C33 C34 H34A 108.9 . . ? C35 C34 H34A 108.9 . . ? C33 C34 H34B 108.9 . . ? C35 C34 H34B 108.9 . . ? H34A C34 H34B 107.7 . . ? C36 C35 C34 114.3(11) . . ? C36 C35 H35A 108.7 . . ? C34 C35 H35A 108.7 . . ? C36 C35 H35B 108.7 . . ? C34 C35 H35B 108.7 . . ? H35A C35 H35B 107.6 . . ? C35 C36 H36A 109.5 . . ? C35 C36 H36B 109.5 . . ? H36A C36 H36B 109.5 . . ? C35 C36 H36C 109.5 . . ? H36A C36 H36C 109.5 . . ? H36B C36 H36C 109.5 . . ? N4 C37 C38 115.7(8) . . ? N4 C37 H37A 108.4 . . ? C38 C37 H37A 108.4 . . ? N4 C37 H37B 108.4 . . ? C38 C37 H37B 108.4 . . ? H37A C37 H37B 107.4 . . ? C39 C38 C37 112.0(10) . . ? C39 C38 H38A 109.2 . . ? C37 C38 H38A 109.2 . . ? C39 C38 H38B 109.2 . . ? C37 C38 H38B 109.2 . . ? H38A C38 H38B 107.9 . . ? C40 C39 C38 114.9(14) . . ? C40 C39 H39A 108.5 . . ? C38 C39 H39A 108.5 . . ? C40 C39 H39B 108.5 . . ? C38 C39 H39B 108.5 . . ? H39A C39 H39B 107.5 . . ? C39 C40 H40A 109.5 . . ? C39 C40 H40B 109.5 . . ? H40A C40 H40B 109.5 . . ? C39 C40 H40C 109.5 . . ? H40A C40 H40C 109.5 . . ? H40B C40 H40C 109.5 . . ? N4 C41 C42 114.8(8) . . ? N4 C41 H41A 108.6 . . ? C42 C41 H41A 108.6 . . ? N4 C41 H41B 108.6 . . ? C42 C41 H41B 108.6 . . ? H41A C41 H41B 107.6 . . ? C43 C42 C41 113.5(9) . . ? C43 C42 H42A 108.9 . . ? C41 C42 H42A 108.9 . . ? C43 C42 H42B 108.9 . . ? C41 C42 H42B 108.9 . . ? H42A C42 H42B 107.7 . . ? C42 C43 C44 113.4(11) . . ? C42 C43 H43A 108.9 . . ? C44 C43 H43A 108.9 . . ? C42 C43 H43B 108.9 . . ? C44 C43 H43B 108.9 . . ? H43A C43 H43B 107.7 . . ? C43 C44 H44A 109.5 . . ? C43 C44 H44B 109.5 . . ? H44A C44 H44B 109.5 . . ? C43 C44 H44C 109.5 . . ? H44A C44 H44C 109.5 . . ? H44B C44 H44C 109.5 . . ? C46 C45 N5 116.0(8) . . ? C46 C45 H45A 108.3 . . ? N5 C45 H45A 108.3 . . ? C46 C45 H45B 108.3 . . ? N5 C45 H45B 108.3 . . ? H45A C45 H45B 107.4 . . ? C45 C46 C47 112.4(8) . . ? C45 C46 H46A 109.1 . . ? C47 C46 H46A 109.1 . . ? C45 C46 H46B 109.1 . . ? C47 C46 H46B 109.1 . . ? H46A C46 H46B 107.8 . . ? C46 C47 C48 112.2(9) . . ? C46 C47 H47A 109.2 . . ? C48 C47 H47A 109.2 . . ? C46 C47 H47B 109.2 . . ? C48 C47 H47B 109.2 . . ? H47A C47 H47B 107.9 . . ? C47 C48 H48A 109.5 . . ? C47 C48 H48B 109.5 . . ? H48A C48 H48B 109.5 . . ? C47 C48 H48C 109.5 . . ? H48A C48 H48C 109.5 . . ? H48B C48 H48C 109.5 . . ? C50 C49 N5 116.7(8) . . ? C50 C49 H49A 108.1 . . ? N5 C49 H49A 108.1 . . ? C50 C49 H49B 108.1 . . ? N5 C49 H49B 108.1 . . ? H49A C49 H49B 107.3 . . ? C49 C50 C51 111.3(9) . . ? C49 C50 H50A 109.4 . . ? C51 C50 H50A 109.4 . . ? C49 C50 H50B 109.4 . . ? C51 C50 H50B 109.4 . . ? H50A C50 H50B 108.0 . . ? C52 C51 C50 110.7(11) . . ? C52 C51 H51A 109.5 . . ? C50 C51 H51A 109.5 . . ? C52 C51 H51B 109.5 . . ? C50 C51 H51B 109.5 . . ? H51A C51 H51B 108.1 . . ? C51 C52 H52A 109.5 . . ? C51 C52 H52B 109.5 . . ? H52A C52 H52B 109.5 . . ? C51 C52 H52C 109.5 . . ? H52A C52 H52C 109.5 . . ? H52B C52 H52C 109.5 . . ? C54 C53 N5 115.5(8) . . ? C54 C53 H53A 108.4 . . ? N5 C53 H53A 108.4 . . ? C54 C53 H53B 108.4 . . ? N5 C53 H53B 108.4 . . ? H53A C53 H53B 107.5 . . ? C55 C54 C53 110.0(9) . . ? C55 C54 H54A 109.7 . . ? C53 C54 H54A 109.7 . . ? C55 C54 H54B 109.7 . . ? C53 C54 H54B 109.7 . . ? H54A C54 H54B 108.2 . . ? C54 C55 C56 113.8(11) . . ? C54 C55 H55A 108.8 . . ? C56 C55 H55A 108.8 . . ? C54 C55 H55B 108.8 . . ? C56 C55 H55B 108.8 . . ? H55A C55 H55B 107.7 . . ? C55 C56 H56A 109.5 . . ? C55 C56 H56B 109.5 . . ? H56A C56 H56B 109.5 . . ? C55 C56 H56C 109.5 . . ? H56A C56 H56C 109.5 . . ? H56B C56 H56C 109.5 . . ? C58 C57 N5 114.8(9) . . ? C58 C57 H57A 108.6 . . ? N5 C57 H57A 108.6 . . ? C58 C57 H57B 108.6 . . ? N5 C57 H57B 108.6 . . ? H57A C57 H57B 107.5 . . ? C57 C58 C59 110.4(11) . . ? C57 C58 H58A 109.6 . . ? C59 C58 H58A 109.6 . . ? C57 C58 H58B 109.6 . . ? C59 C58 H58B 109.6 . . ? H58A C58 H58B 108.1 . . ? C60 C59 C58 114.8(14) . . ? C60 C59 H59A 108.6 . . ? C58 C59 H59A 108.6 . . ? C60 C59 H59B 108.6 . . ? C58 C59 H59B 108.6 . . ? H59A C59 H59B 107.6 . . ? C59 C60 H60A 109.5 . . ? C59 C60 H60B 109.5 . . ? H60A C60 H60B 109.5 . . ? C59 C60 H60C 109.5 . . ? H60A C60 H60C 109.5 . . ? H60B C60 H60C 109.5 . . ? C62 C61 N6 121(2) . . ? C62 C61 H61A 107.1 . . ? N6 C61 H61A 107.1 . . ? C62 C61 H61B 107.1 . . ? N6 C61 H61B 107.1 . . ? H61A C61 H61B 106.8 . . ? C61 C62 C63 120(2) . . ? C61 C62 H62A 107.3 . . ? C63 C62 H62A 107.3 . . ? C61 C62 H62B 107.3 . . ? C63 C62 H62B 107.3 . . ? H62A C62 H62B 106.9 . . ? C64 C63 C62 127(3) . . ? C64 C63 H63A 105.5 . . ? C62 C63 H63A 105.5 . . ? C64 C63 H63B 105.5 . . ? C62 C63 H63B 105.5 . . ? H63A C63 H63B 106.1 . . ? C63 C64 H64A 109.5 . . ? C63 C64 H64B 109.5 . . ? H64A C64 H64B 109.5 . . ? C63 C64 H64C 109.5 . . ? H64A C64 H64C 109.5 . . ? H64B C64 H64C 109.5 . . ? C66 C65 N6 120.0(17) . . ? C66 C65 H65A 107.3 . . ? N6 C65 H65A 107.3 . . ? C66 C65 H65B 107.3 . . ? N6 C65 H65B 107.3 . . ? H65A C65 H65B 106.9 . . ? C65 C66 C67 117(2) . . ? C65 C66 H66A 108.0 . . ? C67 C66 H66A 108.0 . . ? C65 C66 H66B 108.0 . . ? C67 C66 H66B 108.0 . . ? H66A C66 H66B 107.3 . . ? C68 C67 C66 132(2) . . ? C68 C67 H67A 104.2 . . ? C66 C67 H67A 104.2 . . ? C68 C67 H67B 104.2 . . ? C66 C67 H67B 104.2 . . ? H67A C67 H67B 105.5 . . ? C67 C68 H68A 109.5 . . ? C67 C68 H68B 109.5 . . ? H68A C68 H68B 109.5 . . ? C67 C68 H68C 109.5 . . ? H68A C68 H68C 109.5 . . ? H68B C68 H68C 109.5 . . ? N6 C69 C70 129(2) . . ? N6 C69 H69A 105.2 . . ? C70 C69 H69A 105.2 . . ? N6 C69 H69B 105.2 . . ? C70 C69 H69B 105.2 . . ? H69A C69 H69B 105.9 . . ? C71 C70 C69 119(2) . . ? C71 C70 H70A 107.6 . . ? C69 C70 H70A 107.6 . . ? C71 C70 H70B 107.6 . . ? C69 C70 H70B 107.6 . . ? H70A C70 H70B 107.0 . . ? C70 C71 C72 116(2) . . ? C70 C71 H71A 108.3 . . ? C72 C71 H71A 108.3 . . ? C70 C71 H71B 108.3 . . ? C72 C71 H71B 108.3 . . ? H71A C71 H71B 107.4 . . ? C71 C72 H72A 109.5 . . ? C71 C72 H72B 109.5 . . ? H72A C72 H72B 109.5 . . ? C71 C72 H72C 109.5 . . ? H72A C72 H72C 109.5 . . ? H72B C72 H72C 109.5 . . ? C74 C73 N6 121.1(12) . . ? C74 C73 H73A 107.0 . . ? N6 C73 H73A 107.0 . . ? C74 C73 H73B 107.0 . . ? N6 C73 H73B 107.0 . . ? H73A C73 H73B 106.8 . . ? C73 C74 C75 116.6(12) . . ? C73 C74 H74A 108.1 . . ? C75 C74 H74A 108.1 . . ? C73 C74 H74B 108.1 . . ? C75 C74 H74B 108.1 . . ? H74A C74 H74B 107.3 . . ? C76 C75 C74 122.7(13) . . ? C76 C75 H75A 106.6 . . ? C74 C75 H75A 106.6 . . ? C76 C75 H75B 106.6 . . ? C74 C75 H75B 106.6 . . ? H75A C75 H75B 106.6 . . ? C75 C76 H76A 109.5 . . ? C75 C76 H76B 109.5 . . ? H76A C76 H76B 109.5 . . ? C75 C76 H76C 109.5 . . ? H76A C76 H76C 109.5 . . ? H76B C76 H76C 109.5 . . ? _diffrn_measured_fraction_theta_max 0.965 _diffrn_reflns_theta_full 25.00 _diffrn_measured_fraction_theta_full 0.965 _refine_diff_density_max 2.677 _refine_diff_density_min -1.960 _refine_diff_density_rms 0.112 #===END data_compound-7II _database_code_depnum_ccdc_archive 'CCDC 688719' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C76 H166 Mo12 N6 O36' _chemical_formula_weight 2891.43 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' Mo Mo -1.6832 0.6857 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting Monoclinic _symmetry_space_group_name_Hall '-P 2ybc' _symmetry_space_group_name_H-M 'P 21/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 30.461(6) _cell_length_b 16.390(3) _cell_length_c 22.807(5) _cell_angle_alpha 90.00 _cell_angle_beta 96.97(3) _cell_angle_gamma 90.00 _cell_volume 11303(4) _cell_formula_units_Z 4 _cell_measurement_temperature 293(2) _cell_measurement_reflns_used 64905 _cell_measurement_theta_min 3.03 _cell_measurement_theta_max 27.52 _exptl_crystal_description yellow _exptl_crystal_colour plate _exptl_crystal_size_max 0.80 _exptl_crystal_size_mid 0.80 _exptl_crystal_size_min 0.10 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.699 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 5824 _exptl_absorpt_coefficient_mu 1.354 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.4105 _exptl_absorpt_correction_T_max 0.8765 _exptl_absorpt_process_details ? _exptl_special_details ; ? ; _diffrn_ambient_temperature 293(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 'Rigaku RAXIS-RAPID' _diffrn_measurement_method Oscillation _diffrn_detector_area_resol_mean '100x100 micron' _diffrn_reflns_number 83142 _diffrn_reflns_av_R_equivalents 0.0504 _diffrn_reflns_av_sigmaI/netI 0.0509 _diffrn_reflns_limit_h_min -36 _diffrn_reflns_limit_h_max 35 _diffrn_reflns_limit_k_min 0 _diffrn_reflns_limit_k_max 19 _diffrn_reflns_limit_l_min 0 _diffrn_reflns_limit_l_max 27 _diffrn_reflns_theta_min 3.00 _diffrn_reflns_theta_max 25.00 _reflns_number_total 19635 _reflns_number_gt 15144 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'Rigaku RAPID AUTO Ver2.30' _computing_cell_refinement 'Rigaku RAPID AUTO Ver2.30' _computing_data_reduction 'Rigaku RAPID AUTO Ver2.30' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _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^)+(0.0280P)^2^+48.4956P] 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 19624 _refine_ls_number_parameters 1089 _refine_ls_number_restraints 705 _refine_ls_R_factor_all 0.0820 _refine_ls_R_factor_gt 0.0684 _refine_ls_wR_factor_ref 0.1557 _refine_ls_wR_factor_gt 0.1491 _refine_ls_goodness_of_fit_ref 1.095 _refine_ls_restrained_S_all 1.118 _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 Mo1 Mo 0.08630(2) 0.32319(4) 0.44504(3) 0.06124(17) Uani 1 1 d . . . Mo2 Mo 0.07720(2) 0.12880(4) 0.47177(3) 0.06444(18) Uani 1 1 d D . . Mo3 Mo 0.17370(2) 0.20398(4) 0.46060(3) 0.07011(19) Uani 1 1 d . . . Mo4 Mo 0.03760(2) 0.19884(4) 0.34353(3) 0.06803(18) Uani 1 1 d . . . Mo5 Mo 0.13543(3) 0.27523(4) 0.32917(3) 0.0759(2) Uani 1 1 d . . . Mo6 Mo 0.12564(3) 0.08054(4) 0.35802(3) 0.0741(2) Uani 1 1 d . . . Mo7 Mo 0.35934(3) 0.70092(5) 0.17466(4) 0.0950(3) Uani 1 1 d . . . Mo8 Mo 0.40728(3) 0.90673(6) 0.05774(4) 0.1069(3) Uani 1 1 d . . . Mo9 Mo 0.44454(3) 0.82459(6) 0.18532(4) 0.1058(3) Uani 1 1 d . . . Mo10 Mo 0.42232(4) 0.70888(6) 0.06972(5) 0.1114(3) Uani 1 1 d . . . Mo11 Mo 0.32273(4) 0.78461(7) 0.04709(6) 0.1339(5) Uani 1 1 d . . . Mo12 Mo 0.34572(5) 0.89762(7) 0.16318(6) 0.1333(4) Uani 1 1 d D A . O1 O -0.0108(2) 0.1943(4) 0.2995(3) 0.0981(19) Uani 1 1 d . . . O2 O 0.1417(2) -0.0058(4) 0.3264(3) 0.106(2) Uani 1 1 d . . . O3 O 0.22293(19) 0.2080(4) 0.5024(3) 0.0979(19) Uani 1 1 d . . . O4 O 0.07120(19) 0.4121(3) 0.4738(2) 0.0806(15) Uani 1 1 d . . . O5 O 0.17714(17) 0.1068(3) 0.4144(2) 0.0765(14) Uani 1 1 d . . . O7 O 0.1572(3) 0.3287(4) 0.2771(3) 0.114(2) Uani 1 1 d . . . O8 O 0.07523(19) 0.2561(3) 0.2965(2) 0.0806(15) Uani 1 1 d . . . O9 O 0.10551(14) 0.2011(2) 0.40286(17) 0.0525(10) Uani 1 1 d . . . O11 O 0.14377(16) 0.3037(3) 0.4831(2) 0.0679(12) Uani 1 1 d . . . O12 O 0.1472(2) 0.1637(3) 0.3105(2) 0.0881(17) Uani 1 1 d . . . O13 O 0.03499(16) 0.2972(3) 0.38796(19) 0.0665(12) Uani 1 1 d . . . O14 O 0.18342(18) 0.2640(3) 0.3906(3) 0.0823(15) Uani 1 1 d . . . O15 O 0.11339(19) 0.3578(3) 0.3775(2) 0.0756(14) Uani 1 1 d . . . O16 O 0.13737(16) 0.1471(3) 0.5083(2) 0.0701(13) Uani 1 1 d . . . O17 O 0.02692(16) 0.1391(3) 0.4108(2) 0.0714(13) Uani 1 1 d . . . O18 O 0.06513(16) 0.2417(3) 0.49405(19) 0.0667(12) Uani 1 1 d . . . O6 O 0.09922(17) 0.0431(3) 0.4241(2) 0.0708(13) Uani 1 1 d . . . O10 O 0.06791(18) 0.1011(3) 0.3194(2) 0.0773(14) Uani 1 1 d . . . O21 O 0.4030(3) 0.8958(4) 0.2109(3) 0.128(2) Uani 1 1 d . . . O22 O 0.3150(2) 0.7056(4) 0.1076(4) 0.125(3) Uani 1 1 d . . . O23 O 0.3945(2) 0.6458(3) 0.1247(3) 0.110(2) Uani 1 1 d . . . O24 O 0.4123(2) 0.7370(4) 0.2180(3) 0.105(2) Uani 1 1 d . . . O25 O 0.38304(17) 0.8042(3) 0.1164(2) 0.0736(14) Uani 1 1 d . . . O27 O 0.4525(2) 0.9037(4) 0.1246(3) 0.115(2) Uani 1 1 d . . . O28 O 0.3326(3) 0.7952(5) 0.2024(4) 0.149(3) Uani 1 1 d . . . O29 O 0.4342(3) 0.8117(5) 0.0318(3) 0.129(3) Uani 1 1 d . . . O30 O 0.4641(2) 0.7464(4) 0.1334(3) 0.116(2) Uani 1 1 d . . . O31 O 0.2786(4) 0.7703(7) -0.0024(6) 0.231(6) Uani 1 1 d . . . O32 O 0.4514(4) 0.6425(7) 0.0349(5) 0.221(6) Uani 1 1 d . . . O33 O 0.4242(3) 0.9798(5) 0.0138(4) 0.173(4) Uani 1 1 d . . . O34 O 0.3047(3) 0.8647(5) 0.1051(6) 0.172(4) Uani 1 1 d . . . O35 O 0.4887(3) 0.8388(6) 0.2354(4) 0.172(4) Uani 1 1 d . . . O36 O 0.3419(3) 0.6267(5) 0.2164(4) 0.154(3) Uani 1 1 d . . . O26 O 0.3719(3) 0.9638(4) 0.1070(3) 0.125(2) Uani 1 1 d . . . O20 O 0.3635(3) 0.7129(4) 0.0240(3) 0.138(3) Uani 1 1 d . . . O19 O 0.3542(3) 0.8698(4) 0.0129(3) 0.128(3) Uani 1 1 d . . . N3 N 0.0141(2) 0.0676(4) 0.1407(3) 0.0775(18) Uani 1 1 d . . . N4 N 0.2763(3) 0.4348(5) 0.4555(4) 0.107(3) Uani 1 1 d . . . N5 N 0.2221(4) -0.0570(6) 0.5569(5) 0.133(3) Uani 1 1 d . . . N6 N 0.4805(4) 0.6266(8) 0.3602(5) 0.159(3) Uani 1 1 d . . . N1 N 0.0551(2) 0.0722(4) 0.5241(2) 0.0773(18) Uani 1 1 d D . . C1 C 0.0352(3) 0.0218(5) 0.5670(3) 0.079(2) Uani 1 1 d D . . H1A H 0.0201 -0.0244 0.5461 0.095 Uiso 1 1 calc R . . C2 C 0.0712(3) -0.0109(6) 0.6116(4) 0.098(3) Uani 1 1 d D . . H2A H 0.0586 -0.0501 0.6368 0.117 Uiso 1 1 calc R . . H2B H 0.0928 -0.0393 0.5913 0.117 Uiso 1 1 calc R . . C3 C 0.0935(4) 0.0549(8) 0.6489(5) 0.122(4) Uani 1 1 d D . . H3A H 0.1087 0.0912 0.6244 0.147 Uiso 1 1 calc R . . H3B H 0.1154 0.0311 0.6784 0.147 Uiso 1 1 calc R . . C4 C 0.0604(5) 0.1025(8) 0.6789(5) 0.142(5) Uani 1 1 d D . . H4A H 0.0754 0.1462 0.7020 0.170 Uiso 1 1 calc R . . H4B H 0.0470 0.0669 0.7057 0.170 Uiso 1 1 calc R . . C5 C 0.0248(4) 0.1381(6) 0.6347(5) 0.124(4) Uani 1 1 d D . . H5A H 0.0377 0.1782 0.6106 0.149 Uiso 1 1 calc R . . H5B H 0.0030 0.1655 0.6554 0.149 Uiso 1 1 calc R . . C6 C 0.0019(3) 0.0707(6) 0.5946(5) 0.103(3) Uani 1 1 d D . . H6A H -0.0147 0.0351 0.6178 0.124 Uiso 1 1 calc R . . H6B H -0.0187 0.0954 0.5639 0.124 Uiso 1 1 calc R . . N2 N 0.3151(5) 0.9664(7) 0.1977(7) 0.232(7) Uani 1 1 d DU . . C7 C 0.2919(8) 1.0196(13) 0.2370(10) 0.299(9) Uani 1 1 d DU A 1 H7A H 0.3032 1.0750 0.2325 0.358 Uiso 1 1 calc R A 1 C8 C 0.2996(8) 1.0003(18) 0.3019(10) 0.328(10) Uani 1 1 d DU A 1 H8A H 0.3288 0.9759 0.3099 0.393 Uiso 1 1 calc R A 1 H8B H 0.3006 1.0517 0.3232 0.393 Uiso 1 1 calc R A 1 C9 C 0.2687(11) 0.947(2) 0.3274(11) 0.376(13) Uani 1 1 d DU A 1 H9A H 0.2505 0.9802 0.3502 0.451 Uiso 1 1 calc R A 1 H9B H 0.2853 0.9095 0.3543 0.451 Uiso 1 1 calc R A 1 C10 C 0.2398(11) 0.9005(17) 0.2835(14) 0.355(13) Uani 1 1 d DU A 1 H10A H 0.2559 0.8521 0.2740 0.426 Uiso 1 1 calc R A 1 H10B H 0.2146 0.8822 0.3022 0.426 Uiso 1 1 calc R A 1 C11 C 0.2228(9) 0.940(2) 0.2278(13) 0.360(12) Uani 1 1 d DU A 1 H11A H 0.1911 0.9475 0.2268 0.432 Uiso 1 1 calc R A 1 H11B H 0.2276 0.9040 0.1953 0.432 Uiso 1 1 calc R A 1 C12 C 0.2444(8) 1.0229(17) 0.2185(12) 0.346(11) Uani 1 1 d DU A 1 H12A H 0.2391 1.0379 0.1771 0.415 Uiso 1 1 calc R A 1 H12B H 0.2312 1.0644 0.2412 0.415 Uiso 1 1 calc R A 1 C111 C 0.0286(3) -0.0201(5) 0.1494(4) 0.089(3) Uani 1 1 d D . . H11F H 0.0036 -0.0547 0.1354 0.107 Uiso 1 1 calc R . . H11G H 0.0515 -0.0305 0.1243 0.107 Uiso 1 1 calc R . . C112 C 0.0455(4) -0.0460(6) 0.2106(4) 0.117(4) Uani 1 1 d D . . H11H H 0.0678 -0.0076 0.2276 0.141 Uiso 1 1 calc R . . H11I H 0.0215 -0.0460 0.2349 0.141 Uiso 1 1 calc R . . C113 C 0.0651(5) -0.1290(6) 0.2102(6) 0.171(6) Uani 1 1 d D . . H11J H 0.0441 -0.1655 0.1880 0.205 Uiso 1 1 calc R . . H11K H 0.0915 -0.1271 0.1903 0.205 Uiso 1 1 calc R . . C114 C 0.0767(6) -0.1617(8) 0.2704(7) 0.204(8) Uani 1 1 d D . . H11C H 0.0909 -0.2137 0.2683 0.307 Uiso 1 1 calc R . . H11D H 0.0503 -0.1680 0.2891 0.307 Uiso 1 1 calc R . . H11E H 0.0964 -0.1246 0.2930 0.307 Uiso 1 1 calc R . . C121 C 0.0527(3) 0.1253(5) 0.1601(3) 0.083(2) Uani 1 1 d D . . H12F H 0.0424 0.1807 0.1521 0.100 Uiso 1 1 calc R . . H12G H 0.0598 0.1202 0.2025 0.100 Uiso 1 1 calc R . . C122 C 0.0943(3) 0.1142(6) 0.1327(4) 0.102(3) Uani 1 1 d D . . H12H H 0.0876 0.1151 0.0900 0.123 Uiso 1 1 calc R . . H12I H 0.1071 0.0614 0.1440 0.123 Uiso 1 1 calc R . . C123 C 0.1273(3) 0.1797(7) 0.1516(5) 0.120(4) Uani 1 1 d D . . H12J H 0.1153 0.2314 0.1363 0.143 Uiso 1 1 calc R . . H12K H 0.1306 0.1831 0.1943 0.143 Uiso 1 1 calc R . . C124 C 0.1709(4) 0.1694(9) 0.1329(6) 0.160(6) Uani 1 1 d D . . H12C H 0.1898 0.2133 0.1483 0.239 Uiso 1 1 calc R . . H12D H 0.1685 0.1697 0.0905 0.239 Uiso 1 1 calc R . . H12E H 0.1833 0.1184 0.1475 0.239 Uiso 1 1 calc R . . C131 C -0.0022(3) 0.0786(5) 0.0756(3) 0.083(2) Uani 1 1 d D . . H13D H 0.0220 0.0654 0.0533 0.100 Uiso 1 1 calc R . . H13E H -0.0254 0.0388 0.0650 0.100 Uiso 1 1 calc R . . C132 C -0.0196(3) 0.1603(6) 0.0560(4) 0.094(3) Uani 1 1 d D . . H13F H 0.0044 0.1996 0.0602 0.113 Uiso 1 1 calc R . . H13G H -0.0414 0.1777 0.0810 0.113 Uiso 1 1 calc R . . C133 C -0.0405(3) 0.1590(7) -0.0075(4) 0.111(3) Uani 1 1 d D . . H13H H -0.0188 0.1402 -0.0321 0.133 Uiso 1 1 calc R . . H13I H -0.0646 0.1199 -0.0112 0.133 Uiso 1 1 calc R . . C134 C -0.0580(4) 0.2395(8) -0.0302(5) 0.143(5) Uani 1 1 d D . . H13A H -0.0704 0.2341 -0.0707 0.215 Uiso 1 1 calc R . . H13B H -0.0344 0.2786 -0.0272 0.215 Uiso 1 1 calc R . . H13C H -0.0805 0.2577 -0.0072 0.215 Uiso 1 1 calc R . . C141 C -0.0220(3) 0.0887(5) 0.1790(3) 0.080(2) Uani 1 1 d D . . H14D H -0.0109 0.0769 0.2198 0.096 Uiso 1 1 calc R . . H14E H -0.0274 0.1469 0.1761 0.096 Uiso 1 1 calc R . . C142 C -0.0649(3) 0.0458(6) 0.1647(4) 0.095(3) Uani 1 1 d D . . H14F H -0.0606 -0.0125 0.1701 0.114 Uiso 1 1 calc R . . H14G H -0.0763 0.0555 0.1237 0.114 Uiso 1 1 calc R . . C143 C -0.0978(3) 0.0763(6) 0.2045(4) 0.105(3) Uani 1 1 d D . . H14H H -0.0866 0.0637 0.2451 0.126 Uiso 1 1 calc R . . H14I H -0.1000 0.1352 0.2010 0.126 Uiso 1 1 calc R . . C144 C -0.1422(3) 0.0411(7) 0.1912(5) 0.123(4) Uani 1 1 d D . . H14A H -0.1612 0.0631 0.2178 0.184 Uiso 1 1 calc R . . H14B H -0.1405 -0.0171 0.1958 0.184 Uiso 1 1 calc R . . H14C H -0.1538 0.0542 0.1513 0.184 Uiso 1 1 calc R . . C211 C 0.2296(3) 0.4500(7) 0.4696(5) 0.118(4) Uani 1 1 d D . . H21D H 0.2106 0.4575 0.4326 0.141 Uiso 1 1 calc R . . H21E H 0.2195 0.4014 0.4882 0.141 Uiso 1 1 calc R . . C212 C 0.2230(4) 0.5211(7) 0.5085(6) 0.135(4) Uani 1 1 d D . . H21F H 0.2334 0.5704 0.4910 0.162 Uiso 1 1 calc R . . H21G H 0.2404 0.5133 0.5466 0.162 Uiso 1 1 calc R . . C213 C 0.1752(4) 0.5311(9) 0.5168(7) 0.153(5) Uani 1 1 d D . . H21H H 0.1584 0.5419 0.4787 0.183 Uiso 1 1 calc R . . H21I H 0.1645 0.4800 0.5313 0.183 Uiso 1 1 calc R . . C214 C 0.1666(6) 0.5961(10) 0.5574(8) 0.214(8) Uani 1 1 d D . . H21A H 0.1353 0.6001 0.5592 0.321 Uiso 1 1 calc R . . H21B H 0.1773 0.6469 0.5438 0.321 Uiso 1 1 calc R . . H21C H 0.1814 0.5841 0.5960 0.321 Uiso 1 1 calc R . . C221 C 0.2936(4) 0.5100(7) 0.4247(5) 0.121(4) Uani 1 1 d D . . H22D H 0.2976 0.5539 0.4534 0.146 Uiso 1 1 calc R . . H22E H 0.3226 0.4967 0.4139 0.146 Uiso 1 1 calc R . . C222 C 0.2664(4) 0.5412(9) 0.3717(6) 0.155(5) Uani 1 1 d D . . H22F H 0.2380 0.5594 0.3820 0.186 Uiso 1 1 calc R . . H22G H 0.2611 0.4980 0.3427 0.186 Uiso 1 1 calc R . . C223 C 0.2899(5) 0.6121(13) 0.3455(8) 0.213(9) Uani 1 1 d D . . H22H H 0.3015 0.6482 0.3773 0.256 Uiso 1 1 calc R . . H22I H 0.3148 0.5907 0.3276 0.256 Uiso 1 1 calc R . . C224 C 0.2626(7) 0.6589(14) 0.3020(11) 0.328(17) Uani 1 1 d D . . H22A H 0.2798 0.7019 0.2876 0.491 Uiso 1 1 calc R . . H22B H 0.2383 0.6820 0.3195 0.491 Uiso 1 1 calc R . . H22C H 0.2514 0.6240 0.2697 0.491 Uiso 1 1 calc R . . C231 C 0.2735(3) 0.3597(7) 0.4164(6) 0.126(4) Uani 1 1 d D . . H23D H 0.2633 0.3147 0.4388 0.152 Uiso 1 1 calc R . . H23E H 0.2510 0.3696 0.3832 0.152 Uiso 1 1 calc R . . C232 C 0.3150(4) 0.3331(9) 0.3924(8) 0.184(7) Uani 1 1 d D . . H23F H 0.3384 0.3248 0.4246 0.221 Uiso 1 1 calc R . . H23G H 0.3244 0.3751 0.3667 0.221 Uiso 1 1 calc R . . C233 C 0.3061(5) 0.2532(11) 0.3576(9) 0.241(10) Uani 1 1 d D . . H23H H 0.2963 0.2113 0.3831 0.289 Uiso 1 1 calc R . . H23I H 0.2831 0.2616 0.3249 0.289 Uiso 1 1 calc R . . C234 C 0.3479(5) 0.2277(12) 0.3352(10) 0.272 Uani 1 1 d D . . H23A H 0.3440 0.1749 0.3171 0.408 Uiso 1 1 calc R . . H23B H 0.3713 0.2252 0.3674 0.408 Uiso 1 1 calc R . . H23C H 0.3555 0.2665 0.3065 0.408 Uiso 1 1 calc R . . C241 C 0.3084(4) 0.4209(7) 0.5104(5) 0.124(4) Uani 1 1 d D . . H24D H 0.3376 0.4122 0.4987 0.149 Uiso 1 1 calc R . . H24E H 0.3097 0.4701 0.5342 0.149 Uiso 1 1 calc R . . C242 C 0.2976(5) 0.3505(9) 0.5481(7) 0.184(7) Uani 1 1 d D . . H24F H 0.2710 0.3622 0.5658 0.221 Uiso 1 1 calc R . . H24G H 0.2925 0.3019 0.5239 0.221 Uiso 1 1 calc R . . C243 C 0.3354(6) 0.3365(10) 0.5954(8) 0.200(8) Uani 1 1 d D . . H24H H 0.3623 0.3286 0.5773 0.240 Uiso 1 1 calc R . . H24I H 0.3394 0.3844 0.6204 0.240 Uiso 1 1 calc R . . C244 C 0.3281(8) 0.2655(13) 0.6316(10) 0.299(14) Uani 1 1 d D . . H24A H 0.3533 0.2576 0.6606 0.449 Uiso 1 1 calc R . . H24B H 0.3240 0.2180 0.6069 0.449 Uiso 1 1 calc R . . H24C H 0.3023 0.2741 0.6510 0.449 Uiso 1 1 calc R . . C311 C 0.2122(5) 0.0216(7) 0.5888(6) 0.149(5) Uani 1 1 d D . . H31D H 0.2117 0.0663 0.5608 0.179 Uiso 1 1 calc R . . H31E H 0.1829 0.0172 0.6008 0.179 Uiso 1 1 calc R . . C312 C 0.2437(5) 0.0426(10) 0.6415(7) 0.177(6) Uani 1 1 d D . . H31F H 0.2730 0.0522 0.6301 0.213 Uiso 1 1 calc R . . H31G H 0.2457 -0.0020 0.6697 0.213 Uiso 1 1 calc R . . C313 C 0.2271(6) 0.1187(13) 0.6691(8) 0.227(10) Uani 1 1 d D . . H31H H 0.2257 0.1627 0.6405 0.272 Uiso 1 1 calc R . . H31I H 0.1973 0.1088 0.6783 0.272 Uiso 1 1 calc R . . C314 C 0.2546(7) 0.1443(14) 0.7228(8) 0.266(11) Uani 1 1 d D . . H31A H 0.2424 0.1927 0.7381 0.399 Uiso 1 1 calc R . . H31B H 0.2841 0.1554 0.7139 0.399 Uiso 1 1 calc R . . H31C H 0.2556 0.1016 0.7518 0.399 Uiso 1 1 calc R . . C321 C 0.2232(4) -0.1301(8) 0.5987(6) 0.147(5) Uani 1 1 d D . . H32D H 0.2304 -0.1784 0.5773 0.177 Uiso 1 1 calc R . . H32E H 0.2468 -0.1217 0.6306 0.177 Uiso 1 1 calc R . . C322 C 0.1809(5) -0.1464(9) 0.6253(7) 0.177(6) Uani 1 1 d D . . H32F H 0.1569 -0.1586 0.5946 0.213 Uiso 1 1 calc R . . H32G H 0.1728 -0.0993 0.6474 0.213 Uiso 1 1 calc R . . C323 C 0.1908(4) -0.2201(9) 0.6664(7) 0.179 Uani 1 1 d D . . H32H H 0.2012 -0.2656 0.6445 0.215 Uiso 1 1 calc R . . H32I H 0.2136 -0.2063 0.6983 0.215 Uiso 1 1 calc R . . C324 C 0.1499(4) -0.2423(9) 0.6901(7) 0.178 Uani 1 1 d D . . H32A H 0.1550 -0.2900 0.7145 0.267 Uiso 1 1 calc R . . H32B H 0.1272 -0.2535 0.6582 0.267 Uiso 1 1 calc R . . H32C H 0.1408 -0.1980 0.7134 0.267 Uiso 1 1 calc R . . C331 C 0.1858(5) -0.0675(8) 0.5035(6) 0.154(5) Uani 1 1 d D . . H33D H 0.1570 -0.0674 0.5177 0.185 Uiso 1 1 calc R . . H33E H 0.1868 -0.0210 0.4773 0.185 Uiso 1 1 calc R . . C332 C 0.1902(6) -0.1429(11) 0.4693(8) 0.215(10) Uani 1 1 d D . . H33F H 0.2155 -0.1373 0.4476 0.258 Uiso 1 1 calc R . . H33G H 0.1963 -0.1879 0.4967 0.258 Uiso 1 1 calc R . . C333 C 0.1511(6) -0.1635(10) 0.4274(8) 0.211(8) Uani 1 1 d D . . H33H H 0.1255 -0.1657 0.4487 0.254 Uiso 1 1 calc R . . H33I H 0.1462 -0.1202 0.3984 0.254 Uiso 1 1 calc R . . C334 C 0.1546(7) -0.2410(10) 0.3964(8) 0.240(10) Uani 1 1 d D . . H33A H 0.1271 -0.2525 0.3727 0.360 Uiso 1 1 calc R . . H33B H 0.1613 -0.2839 0.4248 0.360 Uiso 1 1 calc R . . H33C H 0.1778 -0.2373 0.3715 0.360 Uiso 1 1 calc R . . C341 C 0.2667(5) -0.0541(9) 0.5360(7) 0.174(6) Uani 1 1 d D . . H34D H 0.2884 -0.0511 0.5708 0.208 Uiso 1 1 calc R . . H34E H 0.2712 -0.1057 0.5169 0.208 Uiso 1 1 calc R . . C342 C 0.2773(4) 0.0118(9) 0.4950(8) 0.196(7) Uani 1 1 d D . . H34F H 0.2668 0.0642 0.5074 0.235 Uiso 1 1 calc R . . H34G H 0.2639 0.0007 0.4551 0.235 Uiso 1 1 calc R . . C343 C 0.3297(5) 0.0116(9) 0.4985(7) 0.190 Uani 1 1 d D . . H34H H 0.3461 0.0296 0.5353 0.228 Uiso 1 1 d R . . H34I H 0.3422 -0.0375 0.4836 0.228 Uiso 1 1 d R . . C344 C 0.3359(5) 0.0775(9) 0.4559(7) 0.191 Uani 1 1 d D . . H34A H 0.3665 0.0804 0.4500 0.286 Uiso 1 1 calc R . . H34B H 0.3269 0.1286 0.4711 0.286 Uiso 1 1 calc R . . H34C H 0.3184 0.0662 0.4189 0.286 Uiso 1 1 calc R . . C411 C 0.5058(5) 0.6506(9) 0.3072(7) 0.165(5) Uani 1 1 d DU . . H41D H 0.4853 0.6511 0.2712 0.199 Uiso 1 1 calc R . . H41E H 0.5177 0.7053 0.3135 0.199 Uiso 1 1 calc R . . C412 C 0.5419(5) 0.5943(10) 0.3002(8) 0.208(6) Uani 1 1 d DU . . H41F H 0.5293 0.5425 0.2862 0.249 Uiso 1 1 calc R . . H41G H 0.5584 0.5850 0.3387 0.249 Uiso 1 1 calc R . . C413 C 0.5743(5) 0.6228(10) 0.2576(7) 0.198 Uani 1 1 d DU . . H41H H 0.5810 0.6804 0.2632 0.238 Uiso 1 1 calc R . . H41I H 0.6017 0.5922 0.2642 0.238 Uiso 1 1 calc R . . C414 C 0.5520(6) 0.6078(12) 0.1982(7) 0.233 Uani 1 1 d DU . . H41A H 0.5702 0.6270 0.1696 0.349 Uiso 1 1 calc R . . H41B H 0.5242 0.6362 0.1932 0.349 Uiso 1 1 calc R . . H41C H 0.5469 0.5503 0.1928 0.349 Uiso 1 1 calc R . . C421 C 0.4613(4) 0.5405(8) 0.3521(6) 0.145(4) Uani 1 1 d DU . . H42D H 0.4854 0.5017 0.3589 0.174 Uiso 1 1 calc R . . H42E H 0.4419 0.5313 0.3823 0.174 Uiso 1 1 calc R . . C422 C 0.4363(5) 0.5231(9) 0.2941(7) 0.202(8) Uani 1 1 d DU . . H42F H 0.4562 0.5222 0.2639 0.242 Uiso 1 1 calc R . . H42G H 0.4143 0.5652 0.2840 0.242 Uiso 1 1 calc R . . C423 C 0.4139(5) 0.4404(10) 0.2974(8) 0.212(4) Uani 1 1 d DU . . H42H H 0.4357 0.3989 0.3101 0.254 Uiso 1 1 calc R . . H42I H 0.3924 0.4424 0.3255 0.254 Uiso 1 1 calc R . . C424 C 0.3915(5) 0.4207(8) 0.2376(7) 0.185 Uani 1 1 d DU . . H42A H 0.3767 0.3692 0.2386 0.277 Uiso 1 1 calc R . . H42B H 0.4131 0.4178 0.2103 0.277 Uiso 1 1 calc R . . H42C H 0.3704 0.4626 0.2252 0.277 Uiso 1 1 calc R . . C431 C 0.5036(5) 0.6223(9) 0.4204(7) 0.186(7) Uani 1 1 d DU . . H43D H 0.4823 0.6024 0.4453 0.223 Uiso 1 1 calc R . . H43E H 0.5260 0.5803 0.4201 0.223 Uiso 1 1 calc R . . C432 C 0.5254(5) 0.6928(10) 0.4509(8) 0.228(10) Uani 1 1 d DU . . H43F H 0.5034 0.7345 0.4550 0.274 Uiso 1 1 calc R . . H43G H 0.5466 0.7152 0.4266 0.274 Uiso 1 1 calc R . . C433 C 0.5496(5) 0.6732(9) 0.5122(7) 0.211(8) Uani 1 1 d DU . . H43H H 0.5295 0.6449 0.5351 0.253 Uiso 1 1 calc R . . H43I H 0.5742 0.6370 0.5079 0.253 Uiso 1 1 calc R . . C434 C 0.5662(5) 0.7470(10) 0.5440(8) 0.232 Uani 1 1 d DU . . H43A H 0.5787 0.7326 0.5833 0.349 Uiso 1 1 calc R . . H43B H 0.5422 0.7846 0.5458 0.349 Uiso 1 1 calc R . . H43C H 0.5885 0.7719 0.5236 0.349 Uiso 1 1 calc R . . C441 C 0.4500(5) 0.6930(8) 0.3527(6) 0.159(3) Uani 1 1 d DU . . H44D H 0.4359 0.6895 0.3122 0.191 Uiso 1 1 calc R . . H44E H 0.4678 0.7422 0.3550 0.191 Uiso 1 1 calc R . . C442 C 0.4150(6) 0.7083(11) 0.3880(8) 0.250 Uani 1 1 d DU . . H44F H 0.4281 0.7179 0.4284 0.300 Uiso 1 1 calc R . . H44G H 0.3970 0.6595 0.3880 0.300 Uiso 1 1 calc R . . C443 C 0.3854(6) 0.7794(11) 0.3684(8) 0.248 Uani 1 1 d DU . . H44H H 0.3755 0.7722 0.3267 0.297 Uiso 1 1 calc R . . H44I H 0.3594 0.7755 0.3890 0.297 Uiso 1 1 calc R . . C444 C 0.4023(6) 0.8624(11) 0.3764(8) 0.250 Uani 1 1 d DU . . H44A H 0.3791 0.9005 0.3641 0.375 Uiso 1 1 calc R . . H44B H 0.4262 0.8701 0.3531 0.375 Uiso 1 1 calc R . . H44C H 0.4128 0.8712 0.4173 0.375 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 Mo1 0.0804(4) 0.0531(3) 0.0501(3) -0.0034(3) 0.0072(3) 0.0012(3) Mo2 0.0769(4) 0.0631(4) 0.0525(3) 0.0099(3) 0.0043(3) -0.0170(3) Mo3 0.0635(4) 0.0634(4) 0.0799(5) 0.0083(3) -0.0052(3) -0.0080(3) Mo4 0.0802(4) 0.0687(4) 0.0513(4) -0.0037(3) -0.0082(3) 0.0044(3) Mo5 0.1044(6) 0.0668(4) 0.0613(4) 0.0117(3) 0.0294(4) -0.0008(4) Mo6 0.0943(5) 0.0552(4) 0.0727(4) -0.0048(3) 0.0090(4) 0.0090(3) Mo7 0.1041(6) 0.0805(5) 0.1027(6) 0.0234(4) 0.0212(5) -0.0117(4) Mo8 0.1220(7) 0.0884(6) 0.1057(7) 0.0355(5) -0.0046(5) -0.0319(5) Mo9 0.1166(7) 0.0925(6) 0.0992(6) 0.0153(5) -0.0240(5) -0.0262(5) Mo10 0.1438(9) 0.0858(6) 0.1115(7) -0.0070(5) 0.0431(6) 0.0112(6) Mo11 0.1219(8) 0.1073(8) 0.1547(10) 0.0450(7) -0.0559(7) -0.0409(6) Mo12 0.1561(11) 0.0882(7) 0.1649(11) -0.0006(7) 0.0573(9) 0.0300(7) O1 0.106(4) 0.104(4) 0.074(4) -0.014(3) -0.032(3) 0.014(4) O2 0.144(6) 0.071(4) 0.106(5) -0.022(3) 0.025(4) 0.023(4) O3 0.072(4) 0.093(4) 0.120(5) 0.005(4) -0.023(3) -0.010(3) O4 0.112(4) 0.059(3) 0.072(3) -0.014(2) 0.014(3) 0.008(3) O5 0.076(3) 0.063(3) 0.090(4) 0.004(3) 0.007(3) 0.007(3) O7 0.164(6) 0.102(5) 0.085(4) 0.027(3) 0.056(4) -0.004(4) O8 0.115(4) 0.075(3) 0.048(3) 0.005(2) -0.004(3) 0.012(3) O9 0.068(3) 0.047(2) 0.041(2) 0.0003(18) 0.0047(19) -0.003(2) O11 0.078(3) 0.056(3) 0.067(3) -0.002(2) -0.001(2) -0.013(2) O12 0.123(5) 0.070(3) 0.080(4) -0.003(3) 0.042(3) 0.012(3) O13 0.082(3) 0.066(3) 0.050(3) 0.002(2) 0.000(2) 0.013(2) O14 0.077(3) 0.072(3) 0.104(4) 0.004(3) 0.033(3) -0.013(3) O15 0.114(4) 0.050(3) 0.065(3) 0.011(2) 0.021(3) -0.002(3) O16 0.075(3) 0.070(3) 0.061(3) 0.013(2) -0.011(2) -0.010(2) O17 0.071(3) 0.072(3) 0.070(3) -0.003(2) 0.003(2) -0.014(3) O18 0.083(3) 0.073(3) 0.045(2) -0.004(2) 0.013(2) -0.008(3) O6 0.092(4) 0.051(3) 0.068(3) 0.000(2) 0.003(3) -0.005(2) O10 0.097(4) 0.069(3) 0.064(3) -0.014(2) 0.001(3) 0.006(3) O21 0.157(7) 0.103(5) 0.120(6) -0.017(4) 0.001(5) -0.011(5) O22 0.092(5) 0.107(5) 0.168(7) 0.029(5) -0.012(4) -0.037(4) O23 0.134(6) 0.061(4) 0.131(6) 0.003(3) 0.007(4) -0.001(4) O24 0.146(6) 0.084(4) 0.083(4) 0.020(3) 0.010(4) -0.009(4) O25 0.078(3) 0.061(3) 0.081(3) 0.008(2) 0.002(3) -0.009(2) O27 0.116(5) 0.102(5) 0.122(5) 0.018(4) -0.007(4) -0.048(4) O28 0.168(8) 0.133(6) 0.167(8) 0.017(5) 0.099(6) 0.014(6) O29 0.148(7) 0.148(7) 0.100(5) 0.023(4) 0.048(5) -0.023(5) O30 0.077(4) 0.123(5) 0.151(6) 0.013(5) 0.023(4) 0.004(4) O31 0.191(10) 0.195(10) 0.266(13) 0.084(9) -0.141(9) -0.082(8) O32 0.294(14) 0.157(9) 0.241(12) -0.052(8) 0.152(11) 0.025(9) O33 0.230(10) 0.135(7) 0.154(7) 0.076(6) 0.018(7) -0.063(7) O34 0.154(8) 0.082(5) 0.298(13) 0.006(7) 0.100(9) 0.019(5) O35 0.178(8) 0.153(7) 0.162(8) 0.029(6) -0.074(6) -0.064(6) O36 0.186(8) 0.131(6) 0.154(7) 0.059(6) 0.051(6) -0.030(6) O26 0.159(7) 0.064(4) 0.150(6) 0.017(4) 0.013(5) 0.005(4) O20 0.217(9) 0.104(5) 0.081(5) 0.005(4) -0.034(5) -0.056(6) O19 0.147(6) 0.108(5) 0.117(5) 0.047(4) -0.033(5) -0.029(5) N3 0.107(5) 0.071(4) 0.057(4) -0.016(3) 0.018(3) -0.017(4) N4 0.081(5) 0.113(6) 0.125(7) -0.015(5) 0.005(5) -0.032(5) N5 0.139(9) 0.103(7) 0.156(9) 0.032(6) 0.014(7) 0.046(6) N6 0.180(8) 0.154(8) 0.132(7) 0.007(6) -0.032(5) 0.064(6) N1 0.104(5) 0.078(4) 0.049(3) 0.008(3) 0.005(3) -0.024(4) C1 0.101(6) 0.064(5) 0.076(5) 0.006(4) 0.026(5) -0.028(4) C2 0.113(7) 0.101(7) 0.078(6) 0.033(5) 0.007(5) -0.003(6) C3 0.127(9) 0.152(11) 0.083(7) 0.030(7) -0.006(6) -0.036(8) C4 0.194(14) 0.161(12) 0.069(7) -0.029(7) 0.007(8) -0.056(11) C5 0.175(12) 0.091(7) 0.115(9) -0.008(7) 0.055(9) -0.004(8) C6 0.099(7) 0.100(7) 0.114(8) 0.020(6) 0.025(6) -0.015(6) N2 0.317(16) 0.131(9) 0.275(15) -0.010(10) 0.141(13) 0.088(10) C7 0.314(17) 0.33(2) 0.282(17) -0.023(16) 0.163(17) 0.109(16) C8 0.33(2) 0.42(3) 0.253(15) -0.055(19) 0.121(16) -0.002(19) C9 0.38(3) 0.46(3) 0.29(2) 0.05(2) 0.04(2) -0.06(2) C10 0.40(3) 0.39(3) 0.28(3) 0.06(2) 0.02(2) -0.02(2) C11 0.34(2) 0.45(3) 0.29(2) 0.08(2) 0.05(2) 0.05(2) C12 0.322(19) 0.37(3) 0.37(2) 0.10(2) 0.125(17) 0.17(2) C111 0.115(7) 0.072(5) 0.081(6) -0.025(4) 0.014(5) -0.013(5) C112 0.179(11) 0.080(7) 0.091(7) 0.004(5) 0.009(7) -0.014(7) C113 0.238(17) 0.081(8) 0.172(14) 0.013(8) -0.064(12) -0.017(9) C114 0.26(2) 0.118(11) 0.219(19) 0.034(12) -0.047(15) -0.047(12) C121 0.123(7) 0.071(5) 0.056(5) -0.011(4) 0.008(4) -0.022(5) C122 0.115(8) 0.121(8) 0.071(6) -0.006(5) 0.012(5) -0.027(6) C123 0.114(9) 0.146(10) 0.097(8) -0.017(7) 0.003(6) -0.038(8) C124 0.145(12) 0.212(16) 0.115(10) 0.009(10) -0.011(8) -0.059(11) C131 0.098(6) 0.102(7) 0.052(4) -0.018(4) 0.016(4) -0.022(5) C132 0.104(7) 0.105(7) 0.076(6) 0.003(5) 0.019(5) -0.014(6) C133 0.095(7) 0.164(11) 0.072(6) 0.004(6) 0.005(5) -0.023(7) C134 0.124(10) 0.192(14) 0.114(9) 0.050(9) 0.011(7) 0.009(9) C141 0.110(7) 0.072(5) 0.064(5) -0.015(4) 0.030(4) -0.012(5) C142 0.113(7) 0.092(6) 0.084(6) -0.013(5) 0.032(5) -0.017(6) C143 0.117(8) 0.096(7) 0.106(7) -0.008(6) 0.035(6) -0.006(6) C144 0.124(9) 0.117(9) 0.133(9) -0.006(7) 0.035(7) 0.009(7) C211 0.092(7) 0.123(9) 0.136(9) -0.020(7) 0.010(6) -0.037(6) C212 0.129(10) 0.123(10) 0.149(11) -0.033(8) 0.008(8) -0.030(8) C213 0.120(10) 0.149(12) 0.191(14) -0.054(11) 0.027(9) -0.006(9) C214 0.199(18) 0.196(18) 0.24(2) -0.018(16) 0.017(15) 0.027(14) C221 0.095(7) 0.117(9) 0.152(11) -0.013(8) 0.011(7) -0.033(7) C222 0.128(11) 0.169(14) 0.172(14) 0.011(11) 0.032(10) -0.026(10) C223 0.172(16) 0.28(3) 0.193(17) 0.117(16) 0.039(13) -0.016(16) C224 0.36(4) 0.21(2) 0.46(5) 0.07(3) 0.23(4) -0.02(2) C231 0.104(8) 0.118(9) 0.155(11) -0.037(8) 0.005(7) -0.033(7) C232 0.115(11) 0.197(16) 0.246(19) -0.078(14) 0.048(11) -0.016(10) C233 0.212(18) 0.213(19) 0.32(3) -0.136(18) 0.120(18) 0.004(15) C234 0.223 0.270 0.341 -0.166 0.107 0.024 C241 0.105(8) 0.120(9) 0.138(10) -0.015(8) -0.017(7) -0.032(7) C242 0.171(14) 0.155(13) 0.210(17) 0.023(12) -0.042(12) -0.069(11) C243 0.200(17) 0.159(15) 0.221(19) 0.039(13) -0.050(14) -0.042(13) C244 0.30(3) 0.22(2) 0.35(3) 0.11(2) -0.08(2) -0.05(2) C311 0.185(14) 0.113(10) 0.144(11) 0.005(8) -0.001(10) 0.048(9) C312 0.199(17) 0.164(15) 0.153(14) 0.009(11) -0.037(12) 0.005(13) C313 0.169(17) 0.30(3) 0.20(2) -0.093(19) -0.004(14) -0.022(17) C314 0.22(2) 0.34(3) 0.23(2) 0.01(2) 0.005(18) -0.04(2) C321 0.163(13) 0.117(10) 0.162(12) 0.033(9) 0.021(10) 0.029(9) C322 0.167(14) 0.176(15) 0.197(16) 0.041(12) 0.056(12) 0.027(11) C323 0.155 0.187 0.205 0.037 0.058 0.005 C324 0.156 0.183 0.205 0.037 0.058 0.005 C331 0.154(12) 0.145(12) 0.150(12) 0.002(9) -0.032(9) 0.047(9) C332 0.26(2) 0.201(18) 0.168(16) -0.061(14) -0.043(14) 0.106(17) C333 0.31(3) 0.134(14) 0.20(2) -0.010(13) 0.048(18) -0.002(16) C334 0.38(3) 0.141(15) 0.183(18) -0.004(13) -0.014(18) 0.004(17) C341 0.142(12) 0.148(12) 0.240(18) 0.057(12) 0.059(12) 0.054(10) C342 0.169(14) 0.153(13) 0.26(2) 0.096(14) 0.000(13) 0.012(11) C343 0.183 0.159 0.234 0.088 0.052 0.028 C344 0.184 0.160 0.234 0.088 0.052 0.028 C411 0.176(13) 0.120(11) 0.192(15) 0.020(10) -0.011(10) -0.005(9) C412 0.146(13) 0.164(15) 0.314(12) 0.030(15) 0.031(12) -0.016(9) C413 0.153 0.148 0.291 0.026 0.011 -0.010 C414 0.162 0.241 0.291 0.026 0.011 -0.010 C421 0.147(12) 0.127(10) 0.169(12) 0.020(8) 0.047(8) 0.014(8) C422 0.153(14) 0.179(14) 0.262(19) -0.022(13) -0.020(12) -0.016(10) C423 0.149 0.209(13) 0.272 -0.007 0.005 -0.018 C424 0.144 0.133 0.272 -0.007 0.005 -0.018 C431 0.179(15) 0.168(14) 0.195(15) -0.004(11) -0.044(11) 0.072(11) C432 0.134(13) 0.26(2) 0.271(18) -0.083(15) -0.063(13) 0.062(13) C433 0.161(14) 0.170(13) 0.280(18) -0.072(13) -0.058(13) 0.054(11) C434 0.184 0.200 0.286 -0.094 -0.084 0.065 C441 0.180(8) 0.154(8) 0.132(7) 0.007(6) -0.032(5) 0.064(6) C442 0.229 0.320 0.189 -0.002 -0.021 0.140 C443 0.225 0.317 0.189 -0.002 -0.021 0.140 C444 0.229 0.320 0.189 -0.002 -0.021 0.140 _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 Mo1 O4 1.685(5) . ? Mo1 O11 1.885(5) . ? Mo1 O18 1.903(5) . ? Mo1 O15 1.919(5) . ? Mo1 O13 1.956(5) . ? Mo1 O9 2.326(4) . ? Mo2 N1 1.712(5) . ? Mo2 O16 1.943(5) . ? Mo2 O6 1.945(5) . ? Mo2 O17 1.946(5) . ? Mo2 O18 1.966(5) . ? Mo2 O9 2.224(4) . ? Mo3 O3 1.678(5) . ? Mo3 O16 1.890(5) . ? Mo3 O5 1.920(5) . ? Mo3 O14 1.928(5) . ? Mo3 O11 1.970(5) . ? Mo3 O9 2.321(4) . ? Mo4 O1 1.681(5) . ? Mo4 O17 1.883(5) . ? Mo4 O8 1.909(6) . ? Mo4 O13 1.910(5) . ? Mo4 O10 1.961(5) . ? Mo4 O9 2.331(4) . ? Mo5 O7 1.675(5) . ? Mo5 O14 1.907(6) . ? Mo5 O15 1.918(5) . ? Mo5 O8 1.919(6) . ? Mo5 O12 1.921(5) . ? Mo5 O9 2.346(4) . ? Mo6 O2 1.688(5) . ? Mo6 O6 1.894(5) . ? Mo6 O10 1.899(5) . ? Mo6 O12 1.907(5) . ? Mo6 O5 1.952(5) . ? Mo6 O9 2.340(4) . ? Mo7 O36 1.671(7) . ? Mo7 O24 1.883(7) . ? Mo7 O23 1.887(7) . ? Mo7 O28 1.891(8) . ? Mo7 O22 1.915(7) . ? Mo7 O25 2.321(5) . ? Mo8 O33 1.682(6) . ? Mo8 O29 1.888(8) . ? Mo8 O26 1.895(8) . ? Mo8 O19 1.904(7) . ? Mo8 O27 1.928(7) . ? Mo8 O25 2.323(5) . ? Mo9 O35 1.671(7) . ? Mo9 O21 1.865(8) . ? Mo9 O30 1.889(8) . ? Mo9 O27 1.934(6) . ? Mo9 O24 1.938(6) . ? Mo9 O25 2.319(5) . ? Mo10 O32 1.665(9) . ? Mo10 O23 1.901(7) . ? Mo10 O30 1.912(8) . ? Mo10 O29 1.947(7) . ? Mo10 O20 1.963(9) . ? Mo10 O25 2.306(5) . ? Mo11 O31 1.664(8) . ? Mo11 O20 1.831(10) . ? Mo11 O19 1.913(7) . ? Mo11 O22 1.928(7) . ? Mo11 O34 1.987(10) . ? Mo11 O25 2.296(5) . ? Mo12 N2 1.714(9) . ? Mo12 O34 1.790(12) . ? Mo12 O26 1.925(7) . ? Mo12 O21 1.942(8) . ? Mo12 O28 1.966(8) . ? Mo12 O25 2.251(5) . ? N3 C111 1.509(10) . ? N3 C131 1.518(9) . ? N3 C141 1.525(9) . ? N3 C121 1.530(9) . ? N4 C241 1.511(12) . ? N4 C231 1.516(12) . ? N4 C211 1.518(12) . ? N4 C221 1.542(13) . ? N5 C341 1.495(14) . ? N5 C311 1.526(14) . ? N5 C321 1.528(13) . ? N5 C331 1.553(14) . ? N6 C441 1.428(14) . ? N6 C431 1.467(16) . ? N6 C421 1.530(16) . ? N6 C411 1.561(17) . ? N1 C1 1.468(8) . ? C1 C6 1.490(11) . ? C1 C2 1.501(11) . ? C2 C3 1.486(13) . ? C3 C4 1.506(15) . ? C4 C5 1.506(15) . ? C5 C6 1.546(13) . ? N2 C7 1.488(10) . ? C7 C12 1.459(19) . ? C7 C8 1.506(18) . ? C8 C9 1.454(19) . ? C9 C10 1.47(2) . ? C10 C11 1.46(2) . ? C11 C12 1.54(2) . ? C111 C112 1.492(9) . ? C112 C113 1.486(11) . ? C113 C114 1.477(12) . ? C121 C122 1.492(9) . ? C122 C123 1.496(10) . ? C123 C124 1.455(11) . ? C131 C132 1.490(9) . ? C132 C133 1.510(9) . ? C133 C134 1.491(11) . ? C141 C142 1.485(9) . ? C142 C143 1.516(9) . ? C143 C144 1.468(10) . ? C211 C212 1.492(10) . ? C212 C213 1.501(11) . ? C213 C214 1.457(10) . ? C221 C222 1.472(11) . ? C222 C223 1.523(12) . ? C223 C224 1.438(14) . ? C231 C232 1.503(11) . ? C232 C233 1.537(12) . ? C233 C234 1.491(9) . ? C241 C242 1.498(11) . ? C242 C243 1.497(12) . ? C243 C244 1.460(11) . ? C311 C312 1.486(11) . ? C312 C313 1.512(13) . ? C313 C314 1.460(13) . ? C321 C322 1.511(11) . ? C322 C323 1.536(12) . ? C323 C324 1.463(10) . ? C331 C332 1.476(12) . ? C332 C333 1.473(13) . ? C333 C334 1.463(12) . ? C341 C342 1.490(11) . ? C342 C343 1.586(12) . ? C343 C344 1.481(10) . ? C411 C412 1.458(12) . ? C412 C413 1.540(12) . ? C413 C414 1.461(11) . ? C421 C422 1.473(12) . ? C422 C423 1.525(12) . ? C423 C424 1.484(12) . ? C431 C432 1.466(11) . ? C432 C433 1.532(13) . ? C433 C434 1.468(10) . ? C441 C442 1.432(11) . ? C442 C443 1.510(12) . ? C443 C444 1.457(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 O4 Mo1 O11 104.4(2) . . ? O4 Mo1 O18 104.5(2) . . ? O11 Mo1 O18 88.4(2) . . ? O4 Mo1 O15 102.7(2) . . ? O11 Mo1 O15 87.4(2) . . ? O18 Mo1 O15 152.6(2) . . ? O4 Mo1 O13 102.4(2) . . ? O11 Mo1 O13 153.2(2) . . ? O18 Mo1 O13 86.4(2) . . ? O15 Mo1 O13 85.3(2) . . ? O4 Mo1 O9 178.2(2) . . ? O11 Mo1 O9 77.22(18) . . ? O18 Mo1 O9 76.09(17) . . ? O15 Mo1 O9 76.61(17) . . ? O13 Mo1 O9 75.99(17) . . ? N1 Mo2 O16 102.4(3) . . ? N1 Mo2 O6 101.0(3) . . ? O16 Mo2 O6 88.9(2) . . ? N1 Mo2 O17 101.7(3) . . ? O16 Mo2 O17 155.9(2) . . ? O6 Mo2 O17 87.6(2) . . ? N1 Mo2 O18 103.2(3) . . ? O16 Mo2 O18 86.6(2) . . ? O6 Mo2 O18 155.83(19) . . ? O17 Mo2 O18 87.0(2) . . ? N1 Mo2 O9 179.2(2) . . ? O16 Mo2 O9 78.15(18) . . ? O6 Mo2 O9 78.44(18) . . ? O17 Mo2 O9 77.79(18) . . ? O18 Mo2 O9 77.39(17) . . ? O3 Mo3 O16 103.7(3) . . ? O3 Mo3 O5 103.9(3) . . ? O16 Mo3 O5 88.9(2) . . ? O3 Mo3 O14 103.5(3) . . ? O16 Mo3 O14 152.6(2) . . ? O5 Mo3 O14 86.8(2) . . ? O3 Mo3 O11 103.2(3) . . ? O16 Mo3 O11 86.4(2) . . ? O5 Mo3 O11 152.8(2) . . ? O14 Mo3 O11 85.1(2) . . ? O3 Mo3 O9 178.9(2) . . ? O16 Mo3 O9 76.74(17) . . ? O5 Mo3 O9 77.07(18) . . ? O14 Mo3 O9 75.96(19) . . ? O11 Mo3 O9 75.78(17) . . ? O1 Mo4 O17 103.8(3) . . ? O1 Mo4 O8 103.2(3) . . ? O17 Mo4 O8 152.8(2) . . ? O1 Mo4 O13 105.3(3) . . ? O17 Mo4 O13 89.1(2) . . ? O8 Mo4 O13 87.1(2) . . ? O1 Mo4 O10 101.8(3) . . ? O17 Mo4 O10 86.4(2) . . ? O8 Mo4 O10 84.8(2) . . ? O13 Mo4 O10 152.8(2) . . ? O1 Mo4 O9 178.0(2) . . ? O17 Mo4 O9 76.33(18) . . ? O8 Mo4 O9 76.54(18) . . ? O13 Mo4 O9 76.70(17) . . ? O10 Mo4 O9 76.16(18) . . ? O7 Mo5 O14 103.7(3) . . ? O7 Mo5 O15 103.6(3) . . ? O14 Mo5 O15 86.3(2) . . ? O7 Mo5 O8 104.6(3) . . ? O14 Mo5 O8 151.7(2) . . ? O15 Mo5 O8 87.4(2) . . ? O7 Mo5 O12 103.9(3) . . ? O14 Mo5 O12 85.6(3) . . ? O15 Mo5 O12 152.5(2) . . ? O8 Mo5 O12 87.3(3) . . ? O7 Mo5 O9 179.4(3) . . ? O14 Mo5 O9 75.71(18) . . ? O15 Mo5 O9 76.12(17) . . ? O8 Mo5 O9 75.97(18) . . ? O12 Mo5 O9 76.42(18) . . ? O2 Mo6 O6 104.0(3) . . ? O2 Mo6 O10 104.6(3) . . ? O6 Mo6 O10 88.1(2) . . ? O2 Mo6 O12 102.6(3) . . ? O6 Mo6 O12 153.2(2) . . ? O10 Mo6 O12 88.4(3) . . ? O2 Mo6 O5 102.4(3) . . ? O6 Mo6 O5 86.1(2) . . ? O10 Mo6 O5 153.1(2) . . ? O12 Mo6 O5 85.0(2) . . ? O2 Mo6 O9 178.3(3) . . ? O6 Mo6 O9 76.51(17) . . ? O10 Mo6 O9 77.04(18) . . ? O12 Mo6 O9 76.82(18) . . ? O5 Mo6 O9 76.03(18) . . ? O36 Mo7 O24 104.0(4) . . ? O36 Mo7 O23 103.8(4) . . ? O24 Mo7 O23 87.4(3) . . ? O36 Mo7 O28 103.0(4) . . ? O24 Mo7 O28 86.8(4) . . ? O23 Mo7 O28 153.2(3) . . ? O36 Mo7 O22 104.0(4) . . ? O24 Mo7 O22 152.0(3) . . ? O23 Mo7 O22 86.2(3) . . ? O28 Mo7 O22 86.8(4) . . ? O36 Mo7 O25 179.6(4) . . ? O24 Mo7 O25 76.4(2) . . ? O23 Mo7 O25 76.4(2) . . ? O28 Mo7 O25 76.8(3) . . ? O22 Mo7 O25 75.6(2) . . ? O33 Mo8 O29 103.0(4) . . ? O33 Mo8 O26 103.8(4) . . ? O29 Mo8 O26 153.2(3) . . ? O33 Mo8 O19 101.9(4) . . ? O29 Mo8 O19 86.7(4) . . ? O26 Mo8 O19 88.2(4) . . ? O33 Mo8 O27 104.4(4) . . ? O29 Mo8 O27 86.1(3) . . ? O26 Mo8 O27 87.0(3) . . ? O19 Mo8 O27 153.6(3) . . ? O33 Mo8 O25 178.6(4) . . ? O29 Mo8 O25 76.3(2) . . ? O26 Mo8 O25 76.9(2) . . ? O19 Mo8 O25 76.8(2) . . ? O27 Mo8 O25 76.8(2) . . ? O35 Mo9 O21 102.6(5) . . ? O35 Mo9 O30 103.6(5) . . ? O21 Mo9 O30 153.8(3) . . ? O35 Mo9 O27 103.6(4) . . ? O21 Mo9 O27 87.3(3) . . ? O30 Mo9 O27 86.0(3) . . ? O35 Mo9 O24 104.1(4) . . ? O21 Mo9 O24 87.1(3) . . ? O30 Mo9 O24 87.2(3) . . ? O27 Mo9 O24 152.3(3) . . ? O35 Mo9 O25 179.6(4) . . ? O21 Mo9 O25 77.3(3) . . ? O30 Mo9 O25 76.5(2) . . ? O27 Mo9 O25 76.8(2) . . ? O24 Mo9 O25 75.5(2) . . ? O32 Mo10 O23 105.4(4) . . ? O32 Mo10 O30 103.3(5) . . ? O23 Mo10 O30 89.0(3) . . ? O32 Mo10 O29 102.4(5) . . ? O23 Mo10 O29 152.2(3) . . ? O30 Mo10 O29 85.2(3) . . ? O32 Mo10 O20 105.9(6) . . ? O23 Mo10 O20 85.3(3) . . ? O30 Mo10 O20 150.8(3) . . ? O29 Mo10 O20 86.6(3) . . ? O32 Mo10 O25 178.1(4) . . ? O23 Mo10 O25 76.5(2) . . ? O30 Mo10 O25 76.4(2) . . ? O29 Mo10 O25 75.7(3) . . ? O20 Mo10 O25 74.4(3) . . ? O31 Mo11 O20 103.5(6) . . ? O31 Mo11 O19 103.3(4) . . ? O20 Mo11 O19 87.7(4) . . ? O31 Mo11 O22 103.4(4) . . ? O20 Mo11 O22 85.5(3) . . ? O19 Mo11 O22 153.3(3) . . ? O31 Mo11 O34 106.2(6) . . ? O20 Mo11 O34 150.0(4) . . ? O19 Mo11 O34 88.9(4) . . ? O22 Mo11 O34 84.3(4) . . ? O31 Mo11 O25 179.2(5) . . ? O20 Mo11 O25 77.0(2) . . ? O19 Mo11 O25 77.3(2) . . ? O22 Mo11 O25 76.0(2) . . ? O34 Mo11 O25 73.3(4) . . ? N2 Mo12 O34 99.7(7) . . ? N2 Mo12 O26 103.1(5) . . ? O34 Mo12 O26 89.1(4) . . ? N2 Mo12 O21 104.8(7) . . ? O34 Mo12 O21 155.4(3) . . ? O26 Mo12 O21 88.0(3) . . ? N2 Mo12 O28 101.6(5) . . ? O34 Mo12 O28 85.3(4) . . ? O26 Mo12 O28 155.2(3) . . ? O21 Mo12 O28 87.1(4) . . ? N2 Mo12 O25 177.4(6) . . ? O34 Mo12 O25 78.0(3) . . ? O26 Mo12 O25 78.1(2) . . ? O21 Mo12 O25 77.5(3) . . ? O28 Mo12 O25 77.1(2) . . ? Mo3 O5 Mo6 116.8(2) . . ? Mo4 O8 Mo5 118.2(2) . . ? Mo2 O9 Mo3 90.40(14) . . ? Mo2 O9 Mo1 91.57(15) . . ? Mo3 O9 Mo1 90.03(14) . . ? Mo2 O9 Mo4 90.51(15) . . ? Mo3 O9 Mo4 179.1(2) . . ? Mo1 O9 Mo4 90.20(15) . . ? Mo2 O9 Mo6 90.21(14) . . ? Mo3 O9 Mo6 90.07(15) . . ? Mo1 O9 Mo6 178.2(2) . . ? Mo4 O9 Mo6 89.66(14) . . ? Mo2 O9 Mo5 179.0(2) . . ? Mo3 O9 Mo5 89.84(15) . . ? Mo1 O9 Mo5 89.41(14) . . ? Mo4 O9 Mo5 89.24(14) . . ? Mo6 O9 Mo5 88.80(14) . . ? Mo1 O11 Mo3 117.0(2) . . ? Mo6 O12 Mo5 117.9(3) . . ? Mo4 O13 Mo1 117.1(2) . . ? Mo5 O14 Mo3 118.5(3) . . ? Mo5 O15 Mo1 117.9(2) . . ? Mo3 O16 Mo2 114.6(2) . . ? Mo4 O17 Mo2 115.4(2) . . ? Mo1 O18 Mo2 114.9(2) . . ? Mo6 O6 Mo2 114.8(2) . . ? Mo6 O10 Mo4 117.1(2) . . ? Mo9 O21 Mo12 115.6(4) . . ? Mo7 O22 Mo11 117.6(3) . . ? Mo7 O23 Mo10 118.0(3) . . ? Mo7 O24 Mo9 118.2(3) . . ? Mo12 O25 Mo11 90.78(19) . . ? Mo12 O25 Mo10 179.0(3) . . ? Mo11 O25 Mo10 90.22(19) . . ? Mo12 O25 Mo9 89.64(19) . . ? Mo11 O25 Mo9 179.2(3) . . ? Mo10 O25 Mo9 89.36(18) . . ? Mo12 O25 Mo7 90.84(19) . . ? Mo11 O25 Mo7 90.77(17) . . ? Mo10 O25 Mo7 89.13(17) . . ? Mo9 O25 Mo7 89.92(18) . . ? Mo12 O25 Mo8 89.73(17) . . ? Mo11 O25 Mo8 89.34(18) . . ? Mo10 O25 Mo8 90.31(19) . . ? Mo9 O25 Mo8 89.96(17) . . ? Mo7 O25 Mo8 179.4(3) . . ? Mo8 O27 Mo9 116.4(3) . . ? Mo7 O28 Mo12 115.2(3) . . ? Mo8 O29 Mo10 117.7(3) . . ? Mo9 O30 Mo10 117.6(3) . . ? Mo12 O34 Mo11 117.9(4) . . ? Mo8 O26 Mo12 115.3(3) . . ? Mo11 O20 Mo10 118.4(3) . . ? Mo8 O19 Mo11 116.6(3) . . ? C111 N3 C131 107.3(6) . . ? C111 N3 C141 111.1(6) . . ? C131 N3 C141 111.1(7) . . ? C111 N3 C121 110.5(7) . . ? C131 N3 C121 111.0(6) . . ? C141 N3 C121 106.0(5) . . ? C241 N4 C231 110.5(9) . . ? C241 N4 C211 112.2(9) . . ? C231 N4 C211 105.7(7) . . ? C241 N4 C221 106.0(8) . . ? C231 N4 C221 112.3(9) . . ? C211 N4 C221 110.2(9) . . ? C341 N5 C311 111.3(12) . . ? C341 N5 C321 105.8(9) . . ? C311 N5 C321 110.8(10) . . ? C341 N5 C331 110.0(11) . . ? C311 N5 C331 107.7(9) . . ? C321 N5 C331 111.3(11) . . ? C441 N6 C431 112.3(12) . . ? C441 N6 C421 117.1(13) . . ? C431 N6 C421 101.6(11) . . ? C441 N6 C411 95.2(11) . . ? C431 N6 C411 120.7(14) . . ? C421 N6 C411 110.9(11) . . ? C1 N1 Mo2 177.8(6) . . ? N1 C1 C6 109.7(7) . . ? N1 C1 C2 109.1(7) . . ? C6 C1 C2 112.6(8) . . ? C3 C2 C1 112.0(8) . . ? C2 C3 C4 110.5(9) . . ? C3 C4 C5 111.4(9) . . ? C4 C5 C6 110.9(9) . . ? C1 C6 C5 110.6(8) . . ? C7 N2 Mo12 170.4(15) . . ? C12 C7 N2 112.0(18) . . ? C12 C7 C8 108.8(16) . . ? N2 C7 C8 116.2(18) . . ? C9 C8 C7 119(2) . . ? C8 C9 C10 114(2) . . ? C11 C10 C9 119(2) . . ? C10 C11 C12 113(2) . . ? C7 C12 C11 110.7(19) . . ? C112 C111 N3 117.1(7) . . ? C113 C112 C111 110.3(8) . . ? C114 C113 C112 112.1(11) . . ? C122 C121 N3 117.7(6) . . ? C121 C122 C123 111.5(8) . . ? C124 C123 C122 115.9(10) . . ? C132 C131 N3 117.6(6) . . ? C131 C132 C133 111.7(8) . . ? C134 C133 C132 114.3(9) . . ? C142 C141 N3 116.4(6) . . ? C141 C142 C143 109.8(7) . . ? C144 C143 C142 113.9(8) . . ? C212 C211 N4 116.8(8) . . ? C211 C212 C213 111.2(9) . . ? C214 C213 C212 114.3(11) . . ? C222 C221 N4 117.5(9) . . ? C221 C222 C223 110.0(11) . . ? C224 C223 C222 114.7(14) . . ? C232 C231 N4 117.4(9) . . ? C231 C232 C233 109.4(10) . . ? C234 C233 C232 108.2(12) . . ? C242 C241 N4 115.3(9) . . ? C243 C242 C241 109.2(11) . . ? C244 C243 C242 111.9(13) . . ? C312 C311 N5 115.9(11) . . ? C311 C312 C313 108.2(12) . . ? C314 C313 C312 113.5(15) . . ? C322 C321 N5 115.7(10) . . ? C321 C322 C323 105.7(10) . . ? C324 C323 C322 108.0(11) . . ? C332 C331 N5 113.8(11) . . ? C333 C332 C331 114.5(13) . . ? C334 C333 C332 114.3(15) . . ? C342 C341 N5 119.9(11) . . ? C341 C342 C343 105.1(10) . . ? C344 C343 C342 100.0(10) . . ? C412 C411 N6 112.0(12) . . ? C411 C412 C413 115.2(13) . . ? C414 C413 C412 105.8(12) . . ? C422 C421 N6 115.7(11) . . ? C421 C422 C423 108.2(13) . . ? C424 C423 C422 107.8(12) . . ? C432 C431 N6 123.0(14) . . ? C431 C432 C433 114.0(14) . . ? C434 C433 C432 112.1(13) . . ? N6 C441 C442 125.6(13) . . ? C441 C442 C443 115.3(14) . . ? C444 C443 C442 119.6(15) . . ? _diffrn_measured_fraction_theta_max 0.984 _diffrn_reflns_theta_full 25.00 _diffrn_measured_fraction_theta_full 0.984 _refine_diff_density_max 1.490 _refine_diff_density_min -1.360 _refine_diff_density_rms 0.108 # SQUEEZE RESULTS (APPEND TO CIF) loop_ _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 1 0.500 0.000 0.500 237.0 4.4 2 0.500 0.500 0.000 237.1 3.9 _platon_squeeze_details ; ? ; #===END data_compound-8 _database_code_depnum_ccdc_archive 'CCDC 688720' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C76 H170 Mo12 N6 O36' _chemical_formula_weight 2895.46 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' Mo Mo -1.6832 0.6857 '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 17.486(4) _cell_length_b 17.636(4) _cell_length_c 20.083(4) _cell_angle_alpha 87.21(3) _cell_angle_beta 66.99(3) _cell_angle_gamma 88.72(3) _cell_volume 5694(2) _cell_formula_units_Z 2 _cell_measurement_temperature 296(2) _cell_measurement_reflns_used 42125 _cell_measurement_theta_min 3.01 _cell_measurement_theta_max 27.0 _exptl_crystal_description block _exptl_crystal_colour organge _exptl_crystal_size_max 0.50 _exptl_crystal_size_mid 0.40 _exptl_crystal_size_min 0.30 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.689 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 2920 _exptl_absorpt_coefficient_mu 1.344 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.5530 _exptl_absorpt_correction_T_max 0.6886 _exptl_absorpt_process_details ? _exptl_special_details ; ? ; _diffrn_ambient_temperature 296(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 'Rigaku RAXIS-RAPID' _diffrn_measurement_method Oscillation _diffrn_detector_area_resol_mean '100x100 micron' _diffrn_reflns_number 42626 _diffrn_reflns_av_R_equivalents 0.0226 _diffrn_reflns_av_sigmaI/netI 0.0287 _diffrn_reflns_limit_h_min -20 _diffrn_reflns_limit_h_max 20 _diffrn_reflns_limit_k_min -20 _diffrn_reflns_limit_k_max 20 _diffrn_reflns_limit_l_min -23 _diffrn_reflns_limit_l_max 23 _diffrn_reflns_theta_min 3.01 _diffrn_reflns_theta_max 25.00 _reflns_number_total 19000 _reflns_number_gt 15220 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'Rigaku RAPID AUTO Ver2.30' _computing_cell_refinement 'Rigaku RAPID AUTO Ver2.30' _computing_data_reduction 'Rigaku RAPID AUTO Ver2.30' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _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^)+(0.0570P)^2^+4.5255P] 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 19000 _refine_ls_number_parameters 1273 _refine_ls_number_restraints 1175 _refine_ls_R_factor_all 0.0487 _refine_ls_R_factor_gt 0.0378 _refine_ls_wR_factor_ref 0.1077 _refine_ls_wR_factor_gt 0.1021 _refine_ls_goodness_of_fit_ref 1.056 _refine_ls_restrained_S_all 1.103 _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 Mo1A Mo 0.69597(3) 0.15331(2) 0.12861(2) 0.05943(12) Uani 1 1 d . B . Mo1 Mo 0.08987(3) 0.62844(3) 0.39062(2) 0.05713(11) Uani 1 1 d . A . Mo2A Mo 0.84990(2) 0.13254(2) 0.18052(2) 0.05260(11) Uani 1 1 d . . . Mo2 Mo 0.28979(3) 0.61889(3) 0.33852(3) 0.06214(13) Uani 1 1 d . . . Mo3A Mo 0.71023(3) -0.00256(2) 0.21518(2) 0.05352(11) Uani 1 1 d . . . Mo3 Mo 0.18941(3) 0.49321(2) 0.28779(2) 0.05104(11) Uani 1 1 d . . . Mo4A Mo 0.70013(3) 0.25528(2) 0.25714(3) 0.05386(11) Uani 1 1 d . . . Mo4 Mo 0.20361(3) 0.75745(2) 0.27571(3) 0.05869(12) Uani 1 1 d . . . Mo5 Mo 0.10262(3) 0.63159(2) 0.22529(2) 0.05137(11) Uani 1 1 d . . . Mo5A Mo 0.56070(3) 0.12043(2) 0.29252(3) 0.05879(12) Uani 1 1 d . . . Mo6A Mo 0.71503(3) 0.09807(2) 0.34682(2) 0.05431(11) Uani 1 1 d . . . Mo6 Mo 0.30644(3) 0.62176(3) 0.16929(3) 0.06158(12) Uani 1 1 d . . . O1 O 0.19503(17) 0.62490(15) 0.28325(15) 0.0441(6) Uani 1 1 d . . . O1A O 0.70533(17) 0.12688(14) 0.23472(15) 0.0426(6) Uani 1 1 d . . . O2A O 0.9544(2) 0.1341(2) 0.1408(2) 0.0733(10) Uani 1 1 d . . . O2 O 0.3589(3) 0.6130(2) 0.3778(3) 0.0968(14) Uani 1 1 d . . . O3 O 0.1840(2) 0.39805(18) 0.2909(2) 0.0726(10) Uani 1 1 d . . . O3A O 0.7110(3) -0.09646(18) 0.2048(2) 0.0744(10) Uani 1 1 d . . . O4A O 0.6989(2) 0.34890(18) 0.2707(2) 0.0754(11) Uani 1 1 d . . . O4 O 0.2116(3) 0.85232(19) 0.2685(3) 0.0858(12) Uani 1 1 d . . . O5 O 0.0365(2) 0.6376(2) 0.1826(2) 0.0743(10) Uani 1 1 d . . . O5A O 0.4568(2) 0.1169(2) 0.3354(3) 0.0848(12) Uani 1 1 d . . . O6A O 0.7202(3) 0.0803(2) 0.42819(19) 0.0772(11) Uani 1 1 d . . . O6 O 0.3863(3) 0.6178(3) 0.0884(2) 0.0990(14) Uani 1 1 d . . . O7 O 0.1845(2) 0.6220(2) 0.41796(18) 0.0676(9) Uani 1 1 d . . . O7A O 0.8157(2) 0.14866(19) 0.10150(17) 0.0608(8) Uani 1 1 d . . . O8A O 0.6985(2) 0.04154(18) 0.13275(19) 0.0638(9) Uani 1 1 d . . . O8 O 0.1010(2) 0.52023(17) 0.37452(18) 0.0589(8) Uani 1 1 d . . . O9 O 0.1154(2) 0.73597(18) 0.36517(18) 0.0610(8) Uani 1 1 d . . . O9A O 0.6962(2) 0.25357(17) 0.16364(19) 0.0609(8) Uani 1 1 d . . . O10 O 0.03227(19) 0.63483(18) 0.32339(18) 0.0575(8) Uani 1 1 d . . . O10A O 0.5784(2) 0.1452(2) 0.1954(2) 0.0669(9) Uani 1 1 d . . . O11A O 0.8244(2) 0.02480(17) 0.17624(17) 0.0564(8) Uani 1 1 d . . . O11 O 0.2648(2) 0.51239(18) 0.3323(2) 0.0649(9) Uani 1 1 d . . . O12A O 0.81995(19) 0.23411(17) 0.20630(18) 0.0559(8) Uani 1 1 d . . . O12 O 0.2787(2) 0.72603(19) 0.3233(2) 0.0673(9) Uani 1 1 d . . . O13 O 0.1160(2) 0.52468(17) 0.23866(18) 0.0559(8) Uani 1 1 d . . . O13A O 0.5912(2) 0.01811(17) 0.26805(19) 0.0614(8) Uani 1 1 d . . . O14 O 0.1298(2) 0.73757(17) 0.22920(18) 0.0581(8) Uani 1 1 d . . . O14A O 0.5865(2) 0.22783(18) 0.2983(2) 0.0629(9) Uani 1 1 d . . . O15A O 0.8293(2) 0.10778(18) 0.27987(18) 0.0587(8) Uani 1 1 d . . . O15 O 0.3599(2) 0.6149(2) 0.2375(2) 0.0706(10) Uani 1 1 d . . . O16A O 0.7151(2) 0.00122(17) 0.31054(17) 0.0597(8) Uani 1 1 d . . . O16 O 0.2787(2) 0.51659(18) 0.19655(19) 0.0641(9) Uani 1 1 d . . . O17A O 0.7130(2) 0.20836(18) 0.33950(18) 0.0589(8) Uani 1 1 d . . . O17 O 0.2926(2) 0.72709(19) 0.18800(19) 0.0652(9) Uani 1 1 d . . . O18 O 0.2115(2) 0.62860(19) 0.14567(17) 0.0635(9) Uani 1 1 d . . . O18A O 0.5985(2) 0.1035(2) 0.37085(18) 0.0640(9) Uani 1 1 d . . . N1 N 0.0072(3) 0.6339(3) 0.4717(2) 0.0719(12) Uani 1 1 d DU . . N1A N 0.6871(3) 0.1759(3) 0.0481(3) 0.0785(13) Uani 1 1 d DU . . N2 N 0.4586(4) 0.8344(3) 0.3827(3) 0.1015(10) Uani 1 1 d DU . . N3 N 0.4792(3) 0.5789(3) 0.8238(3) 0.0944(15) Uani 1 1 d U . . N4 N 0.0826(3) 0.6137(2) 0.6980(3) 0.0753(12) Uani 1 1 d U . . N5 N 0.0346(3) 0.8927(2) 0.1337(2) 0.0671(11) Uani 1 1 d U . . C1 C -0.0646(12) 0.6451(11) 0.5372(8) 0.088(7) Uani 0.50 1 d PDU A 1 H1A H -0.0528 0.6259 0.5783 0.105 Uiso 0.50 1 calc PR A 1 H1B H -0.1108 0.6164 0.5362 0.105 Uiso 0.50 1 calc PR A 1 C2 C -0.0884(9) 0.7262(7) 0.5464(7) 0.088(3) Uani 0.50 1 d PDU A 1 H2A H -0.0414 0.7555 0.5450 0.106 Uiso 0.50 1 calc PR A 1 H2B H -0.1334 0.7322 0.5931 0.106 Uiso 0.50 1 calc PR A 1 C3 C -0.1157(15) 0.7559(10) 0.4863(12) 0.155(6) Uani 0.50 1 d PDU A 1 H3A H -0.1718 0.7383 0.4977 0.186 Uiso 0.50 1 calc PR A 1 H3B H -0.0800 0.7334 0.4415 0.186 Uiso 0.50 1 calc PR A 1 C4 C -0.1144(18) 0.8429(11) 0.473(2) 0.229(8) Uani 0.50 1 d PDU A 1 H4A H -0.1420 0.8527 0.4400 0.275 Uiso 0.50 1 calc PR A 1 H4B H -0.1507 0.8631 0.5189 0.275 Uiso 0.50 1 calc PR A 1 C5 C -0.0370(15) 0.8941(12) 0.4448(17) 0.229 Uani 0.50 1 d PDU A 1 H5A H -0.0092 0.8932 0.3925 0.275 Uiso 0.50 1 calc PR A 1 H5B H 0.0020 0.8785 0.4664 0.275 Uiso 0.50 1 calc PR A 1 C6 C -0.0737(17) 0.9746(12) 0.4691(15) 0.229 Uani 0.50 1 d PDU A 1 H6A H -0.0355 1.0024 0.4823 0.229 Uiso 0.50 1 calc PR A 1 H6B H -0.1257 0.9694 0.5099 0.229 Uiso 0.50 1 calc PR A 1 H6C H -0.0824 1.0015 0.4299 0.229 Uiso 0.50 1 calc PR A 1 C1' C -0.0661(9) 0.6441(9) 0.5362(7) 0.074(5) Uani 0.50 1 d PDU A 2 H1'1 H -0.0501 0.6601 0.5745 0.089 Uiso 0.50 1 calc PR A 2 H1'2 H -0.0950 0.5961 0.5519 0.089 Uiso 0.50 1 calc PR A 2 C2' C -0.1221(10) 0.7011(9) 0.5234(12) 0.125(5) Uani 0.50 1 d PDU A 2 H2'1 H -0.1718 0.7050 0.5672 0.151 Uiso 0.50 1 calc PR A 2 H2'2 H -0.1384 0.6845 0.4856 0.151 Uiso 0.50 1 calc PR A 2 C3' C -0.0815(14) 0.7794(10) 0.5012(18) 0.171(8) Uani 0.50 1 d PDU A 2 H3'1 H -0.0507 0.7867 0.5314 0.205 Uiso 0.50 1 calc PR A 2 H3'2 H -0.0408 0.7760 0.4521 0.205 Uiso 0.50 1 calc PR A 2 C4' C -0.1293(19) 0.8508(13) 0.503(2) 0.235(12) Uani 0.50 1 d PDU A 2 H4'1 H -0.1790 0.8382 0.4954 0.282 Uiso 0.50 1 calc PR A 2 H4'2 H -0.1470 0.8703 0.5509 0.282 Uiso 0.50 1 calc PR A 2 C5' C -0.0856(17) 0.9124(15) 0.449(2) 0.271(12) Uani 0.50 1 d PDU A 2 H5'1 H -0.0416 0.8903 0.4087 0.325 Uiso 0.50 1 calc PR A 2 H5'2 H -0.0601 0.9459 0.4717 0.325 Uiso 0.50 1 calc PR A 2 C6' C -0.142(2) 0.959(2) 0.4218(18) 0.32(2) Uani 0.50 1 d PDU A 2 H6'1 H -0.1086 0.9848 0.3768 0.316 Uiso 0.50 1 calc PR A 2 H6'2 H -0.1716 0.9954 0.4567 0.316 Uiso 0.50 1 calc PR A 2 H6'3 H -0.1803 0.9260 0.4143 0.316 Uiso 0.50 1 calc PR A 2 C1A C 0.664(2) 0.1963(12) -0.0126(13) 0.124(7) Uani 0.50 1 d PDU B 1 H1A1 H 0.6073 0.2152 0.0063 0.149 Uiso 0.50 1 calc PR B 1 H1A2 H 0.6994 0.2374 -0.0411 0.149 Uiso 0.50 1 calc PR B 1 C2A C 0.6697(19) 0.1350(14) -0.0600(12) 0.176(7) Uani 0.50 1 d PDU B 1 H2A1 H 0.7275 0.1201 -0.0832 0.211 Uiso 0.50 1 calc PR B 1 H2A2 H 0.6520 0.1542 -0.0978 0.211 Uiso 0.50 1 calc PR B 1 C3A C 0.619(2) 0.0641(13) -0.0234(14) 0.216(9) Uani 0.50 1 d PDU B 1 H3A1 H 0.5609 0.0789 0.0017 0.259 Uiso 0.50 1 calc PR B 1 H3A2 H 0.6382 0.0428 0.0126 0.259 Uiso 0.50 1 calc PR B 1 C4A C 0.623(4) 0.0026(17) -0.077(2) 0.277(11) Uani 0.50 1 d PDU B 1 H4A1 H 0.5914 0.0236 -0.1033 0.333 Uiso 0.50 1 calc PR B 1 H4A2 H 0.6809 0.0040 -0.1109 0.333 Uiso 0.50 1 calc PR B 1 C5A C 0.603(4) -0.0784(17) -0.0669(19) 0.333(15) Uani 0.50 1 d PDU B 1 H5A1 H 0.5434 -0.0844 -0.0397 0.333 Uiso 0.50 1 calc PR B 1 H5A2 H 0.6313 -0.1038 -0.0393 0.333 Uiso 0.50 1 calc PR B 1 C6A C 0.628(3) -0.115(2) -0.141(2) 0.314(19) Uani 0.50 1 d PDU B 1 H6A1 H 0.6410 -0.1680 -0.1355 0.314 Uiso 0.50 1 calc PR B 1 H6A2 H 0.6757 -0.0900 -0.1756 0.314 Uiso 0.50 1 calc PR B 1 H6A3 H 0.5827 -0.1114 -0.1563 0.314 Uiso 0.50 1 calc PR B 1 C1A' C 0.6782(17) 0.1995(11) -0.0190(11) 0.094(5) Uani 0.50 1 d PDU B 2 H1A3 H 0.7315 0.1963 -0.0592 0.112 Uiso 0.50 1 calc PR B 2 H1A4 H 0.6594 0.2519 -0.0165 0.112 Uiso 0.50 1 calc PR B 2 C2A' C 0.6174(12) 0.1504(11) -0.0310(13) 0.142(6) Uani 0.50 1 d PDU B 2 H2A3 H 0.5952 0.1762 -0.0633 0.170 Uiso 0.50 1 calc PR B 2 H2A4 H 0.5718 0.1377 0.0145 0.170 Uiso 0.50 1 calc PR B 2 C3A' C 0.6658(18) 0.0765(14) -0.0657(17) 0.220(9) Uani 0.50 1 d PDU B 2 H3A3 H 0.7212 0.0918 -0.0984 0.264 Uiso 0.50 1 calc PR B 2 H3A4 H 0.6719 0.0451 -0.0270 0.264 Uiso 0.50 1 calc PR B 2 C4A' C 0.631(3) 0.0258(17) -0.107(2) 0.285(13) Uani 0.50 1 d PDU B 2 H4A3 H 0.5713 0.0294 -0.0842 0.343 Uiso 0.50 1 calc PR B 2 H4A4 H 0.6471 0.0495 -0.1554 0.343 Uiso 0.50 1 calc PR B 2 C5A' C 0.652(2) -0.0567(18) -0.118(2) 0.302(13) Uani 0.50 1 d PDU B 2 H5A3 H 0.6649 -0.0778 -0.0779 0.362 Uiso 0.50 1 calc PR B 2 H5A4 H 0.6997 -0.0629 -0.1623 0.362 Uiso 0.50 1 calc PR B 2 C6A' C 0.577(3) -0.099(3) -0.121(3) 0.36(2) Uani 0.50 1 d PDU B 2 H6A4 H 0.5913 -0.1519 -0.1293 0.362 Uiso 0.50 1 calc PR B 2 H6A5 H 0.5627 -0.0773 -0.1589 0.362 Uiso 0.50 1 calc PR B 2 H6A6 H 0.5302 -0.0956 -0.0752 0.362 Uiso 0.50 1 calc PR B 2 C111 C 0.4947(5) 0.8866(5) 0.4243(5) 0.051(2) Uani 0.50 1 d PDU C 1 H11D H 0.4962 0.9386 0.4056 0.061 Uiso 0.50 1 calc PR C 1 H11E H 0.4580 0.8851 0.4751 0.061 Uiso 0.50 1 calc PR C 1 C112 C 0.5813(7) 0.8630(9) 0.4172(6) 0.075(3) Uani 0.50 1 d PDU C 1 H11F H 0.5838 0.8080 0.4198 0.090 Uiso 0.50 1 calc PR C 1 H11G H 0.6204 0.8800 0.3697 0.090 Uiso 0.50 1 calc PR C 1 C113 C 0.6081(13) 0.8914(7) 0.4709(12) 0.108(5) Uani 0.50 1 d PDU C 1 H11H H 0.5635 0.9148 0.5103 0.129 Uiso 0.50 1 calc PR C 1 H11I H 0.6549 0.9257 0.4502 0.129 Uiso 0.50 1 calc PR C 1 C114 C 0.6326(6) 0.8129(6) 0.4926(6) 0.077 Uani 0.50 1 d PDU C 1 H11A H 0.6576 0.8183 0.5269 0.115 Uiso 0.50 1 calc PR C 1 H11B H 0.6715 0.7895 0.4504 0.115 Uiso 0.50 1 calc PR C 1 H11C H 0.5839 0.7818 0.5140 0.115 Uiso 0.50 1 calc PR C 1 C121 C 0.4555(10) 0.7521(7) 0.4160(6) 0.1015(10) Uani 0.50 1 d PDU C 1 H12D H 0.4300 0.7191 0.3933 0.122 Uiso 0.50 1 calc PR C 1 H12E H 0.5119 0.7343 0.4044 0.122 Uiso 0.50 1 calc PR C 1 C122 C 0.4071(7) 0.7445(6) 0.4993(6) 0.071(3) Uani 0.50 1 d PDU C 1 H12F H 0.4280 0.7811 0.5226 0.085 Uiso 0.50 1 calc PR C 1 H12G H 0.3486 0.7552 0.5113 0.085 Uiso 0.50 1 calc PR C 1 C123 C 0.4172(8) 0.6662(6) 0.5261(7) 0.082(3) Uani 0.50 1 d PDU C 1 H12H H 0.4124 0.6304 0.4928 0.099 Uiso 0.50 1 calc PR C 1 H12I H 0.3719 0.6563 0.5726 0.099 Uiso 0.50 1 calc PR C 1 C124 C 0.4976(9) 0.6517(9) 0.5347(9) 0.116(5) Uani 0.50 1 d PDU C 1 H12A H 0.4959 0.6027 0.5584 0.174 Uiso 0.50 1 calc PR C 1 H12B H 0.5062 0.6901 0.5633 0.174 Uiso 0.50 1 calc PR C 1 H12C H 0.5424 0.6528 0.4879 0.174 Uiso 0.50 1 calc PR C 1 C131 C 0.3712(6) 0.8603(6) 0.3962(7) 0.0830(17) Uani 0.50 1 d PDU C 1 H13D H 0.3406 0.8660 0.4477 0.100 Uiso 0.50 1 calc PR C 1 H13E H 0.3435 0.8219 0.3808 0.100 Uiso 0.50 1 calc PR C 1 C132 C 0.3699(7) 0.9351(6) 0.3560(8) 0.0830(17) Uani 0.50 1 d PDU C 1 H13F H 0.3962 0.9743 0.3718 0.100 Uiso 0.50 1 calc PR C 1 H13G H 0.4001 0.9301 0.3044 0.100 Uiso 0.50 1 calc PR C 1 C133 C 0.2806(7) 0.9558(6) 0.3720(8) 0.0830(17) Uani 0.50 1 d PDU C 1 H13H H 0.2501 0.9613 0.4235 0.100 Uiso 0.50 1 calc PR C 1 H13I H 0.2541 0.9171 0.3558 0.100 Uiso 0.50 1 calc PR C 1 C134 C 0.2836(8) 1.0312(6) 0.3304(7) 0.0830(17) Uani 0.50 1 d PDU C 1 H13A H 0.2285 1.0519 0.3448 0.125 Uiso 0.50 1 calc PR C 1 H13B H 0.3059 1.0230 0.2794 0.125 Uiso 0.50 1 calc PR C 1 H13C H 0.3184 1.0661 0.3408 0.125 Uiso 0.50 1 calc PR C 1 C141 C 0.5190(8) 0.8346(9) 0.3041(5) 0.097(2) Uani 0.50 1 d PDU C 1 H14D H 0.5720 0.8139 0.3013 0.116 Uiso 0.50 1 calc PR C 1 H14E H 0.5280 0.8864 0.2841 0.116 Uiso 0.50 1 calc PR C 1 C142 C 0.4852(9) 0.7873(9) 0.2596(6) 0.097(2) Uani 0.50 1 d PDU C 1 H14F H 0.4888 0.7344 0.2738 0.116 Uiso 0.50 1 calc PR C 1 H14G H 0.4266 0.7993 0.2748 0.116 Uiso 0.50 1 calc PR C 1 C143 C 0.5201(10) 0.7928(8) 0.1832(6) 0.097(2) Uani 0.50 1 d PDU C 1 H14H H 0.4814 0.7679 0.1676 0.116 Uiso 0.50 1 calc PR C 1 H14I H 0.5698 0.7615 0.1682 0.116 Uiso 0.50 1 calc PR C 1 C144 C 0.5434(9) 0.8633(7) 0.1398(6) 0.097(2) Uani 0.50 1 d PDU C 1 H14A H 0.5831 0.8528 0.0923 0.145 Uiso 0.50 1 calc PR C 1 H14B H 0.5675 0.8970 0.1623 0.145 Uiso 0.50 1 calc PR C 1 H14C H 0.4949 0.8866 0.1363 0.145 Uiso 0.50 1 calc PR C 1 C211 C 0.4806(5) 0.5057(4) 0.7859(5) 0.122(3) Uani 1 1 d U . . H21D H 0.4599 0.4649 0.8225 0.146 Uiso 1 1 calc R . . H21E H 0.5380 0.4937 0.7561 0.146 Uiso 1 1 calc R . . C212 C 0.4302(7) 0.5067(6) 0.7381(6) 0.155(4) Uani 1 1 d U . . H21F H 0.3745 0.5253 0.7652 0.186 Uiso 1 1 calc R . . H21G H 0.4561 0.5410 0.6963 0.186 Uiso 1 1 calc R . . C213 C 0.4254(8) 0.4280(8) 0.7131(9) 0.212(6) Uani 1 1 d U . . H21H H 0.4811 0.4086 0.6875 0.254 Uiso 1 1 calc R . . H21I H 0.3976 0.3942 0.7548 0.254 Uiso 1 1 calc R . . C214 C 0.3805(10) 0.4294(10) 0.6656(10) 0.296(11) Uani 1 1 d U . . H21A H 0.3800 0.3793 0.6490 0.296 Uiso 1 1 calc R . . H21B H 0.4073 0.4637 0.6248 0.296 Uiso 1 1 calc R . . H21C H 0.3245 0.4460 0.6917 0.296 Uiso 1 1 calc R . . C221 C 0.5142(5) 0.6454(4) 0.7695(4) 0.108(2) Uani 1 1 d U . . H22D H 0.4775 0.6557 0.7443 0.130 Uiso 1 1 calc R . . H22E H 0.5143 0.6900 0.7959 0.130 Uiso 1 1 calc R . . C222 C 0.5999(6) 0.6331(5) 0.7149(5) 0.146(4) Uani 1 1 d U . . H22F H 0.5997 0.5905 0.6862 0.176 Uiso 1 1 calc R . . H22G H 0.6365 0.6203 0.7397 0.176 Uiso 1 1 calc R . . C223 C 0.6332(7) 0.7022(6) 0.6652(7) 0.168(5) Uani 1 1 d U . . H22H H 0.6776 0.6880 0.6205 0.202 Uiso 1 1 calc R . . H22I H 0.5894 0.7269 0.6537 0.202 Uiso 1 1 calc R . . C224 C 0.6643(9) 0.7527(7) 0.7042(8) 0.211(6) Uani 1 1 d U . . H22A H 0.6859 0.7979 0.6748 0.316 Uiso 1 1 calc R . . H22B H 0.7076 0.7275 0.7150 0.316 Uiso 1 1 calc R . . H22C H 0.6198 0.7659 0.7485 0.316 Uiso 1 1 calc R . . C231 C 0.5317(5) 0.5642(4) 0.8676(4) 0.109(2) Uani 1 1 d U . . H23D H 0.5083 0.5215 0.9013 0.131 Uiso 1 1 calc R . . H23E H 0.5870 0.5494 0.8349 0.131 Uiso 1 1 calc R . . C232 C 0.5401(5) 0.6296(5) 0.9099(4) 0.116(2) Uani 1 1 d U . . H23F H 0.4858 0.6440 0.9446 0.139 Uiso 1 1 calc R . . H23G H 0.5637 0.6731 0.8773 0.139 Uiso 1 1 calc R . . C233 C 0.5958(6) 0.6058(7) 0.9491(6) 0.155(4) Uani 1 1 d U . . H23H H 0.5728 0.5608 0.9795 0.186 Uiso 1 1 calc R . . H23I H 0.6501 0.5925 0.9136 0.186 Uiso 1 1 calc R . . C234 C 0.6059(8) 0.6644(8) 0.9939(7) 0.199(5) Uani 1 1 d U . . H23A H 0.6416 0.6458 1.0172 0.298 Uiso 1 1 calc R . . H23B H 0.5526 0.6771 1.0299 0.298 Uiso 1 1 calc R . . H23C H 0.6301 0.7087 0.9640 0.298 Uiso 1 1 calc R . . C241 C 0.3909(4) 0.6003(4) 0.8723(4) 0.0931(19) Uani 1 1 d U . . H24D H 0.3930 0.6469 0.8953 0.112 Uiso 1 1 calc R . . H24E H 0.3602 0.6114 0.8418 0.112 Uiso 1 1 calc R . . C242 C 0.3425(5) 0.5425(4) 0.9305(4) 0.106(2) Uani 1 1 d U . . H24F H 0.3701 0.5337 0.9638 0.127 Uiso 1 1 calc R . . H24G H 0.3415 0.4949 0.9087 0.127 Uiso 1 1 calc R . . C243 C 0.2542(4) 0.5689(5) 0.9721(4) 0.101(2) Uani 1 1 d U . . H24H H 0.2557 0.6143 0.9971 0.121 Uiso 1 1 calc R . . H24I H 0.2289 0.5825 0.9379 0.121 Uiso 1 1 calc R . . C244 C 0.2025(5) 0.5122(5) 1.0248(5) 0.118(3) Uani 1 1 d U . . H24A H 0.1482 0.5331 1.0503 0.177 Uiso 1 1 calc R . . H24B H 0.2274 0.4980 1.0587 0.177 Uiso 1 1 calc R . . H24C H 0.1980 0.4683 1.0003 0.177 Uiso 1 1 calc R . . C311 C 0.1289(4) 0.6847(3) 0.6580(4) 0.0867(17) Uani 1 1 d U . . H31D H 0.1223 0.7226 0.6933 0.104 Uiso 1 1 calc R . . H31E H 0.1876 0.6724 0.6358 0.104 Uiso 1 1 calc R . . C312 C 0.1024(5) 0.7193(4) 0.6005(4) 0.107(2) Uani 1 1 d U . . H31F H 0.1121 0.6831 0.5632 0.128 Uiso 1 1 calc R . . H31G H 0.0433 0.7301 0.6216 0.128 Uiso 1 1 calc R . . C313 C 0.1482(6) 0.7904(5) 0.5672(5) 0.130(3) Uani 1 1 d U . . H31H H 0.1409 0.8246 0.6057 0.156 Uiso 1 1 calc R . . H31I H 0.2070 0.7782 0.5451 0.156 Uiso 1 1 calc R . . C314 C 0.1254(7) 0.8304(6) 0.5136(5) 0.161(4) Uani 1 1 d U . . H31A H 0.1600 0.8744 0.4951 0.241 Uiso 1 1 calc R . . H31B H 0.0683 0.8460 0.5353 0.241 Uiso 1 1 calc R . . H31C H 0.1327 0.7977 0.4748 0.241 Uiso 1 1 calc R . . C321 C 0.0880(4) 0.5526(3) 0.6454(4) 0.0824(16) Uani 1 1 d U . . H32D H 0.0555 0.5093 0.6727 0.099 Uiso 1 1 calc R . . H32E H 0.0626 0.5721 0.6129 0.099 Uiso 1 1 calc R . . C322 C 0.1738(5) 0.5255(4) 0.6008(4) 0.105(2) Uani 1 1 d U . . H32F H 0.2072 0.5685 0.5740 0.126 Uiso 1 1 calc R . . H32G H 0.1990 0.5041 0.6329 0.126 Uiso 1 1 calc R . . C323 C 0.1752(5) 0.4684(4) 0.5498(4) 0.111(2) Uani 1 1 d U . . H32H H 0.1518 0.4904 0.5167 0.133 Uiso 1 1 calc R . . H32I H 0.1402 0.4262 0.5765 0.133 Uiso 1 1 calc R . . C324 C 0.2612(6) 0.4389(5) 0.5067(5) 0.139(3) Uani 1 1 d U . . H32A H 0.2583 0.4023 0.4739 0.208 Uiso 1 1 calc R . . H32B H 0.2840 0.4154 0.5390 0.208 Uiso 1 1 calc R . . H32C H 0.2960 0.4803 0.4796 0.208 Uiso 1 1 calc R . . C331 C 0.1229(4) 0.5867(4) 0.7495(4) 0.0865(17) Uani 1 1 d U . . H33D H 0.1812 0.5766 0.7213 0.104 Uiso 1 1 calc R . . H33E H 0.1202 0.6277 0.7809 0.104 Uiso 1 1 calc R . . C332 C 0.0862(6) 0.5177(5) 0.7959(5) 0.124(3) Uani 1 1 d U . . H33F H 0.0817 0.4775 0.7663 0.149 Uiso 1 1 calc R . . H33G H 0.0310 0.5290 0.8310 0.149 Uiso 1 1 calc R . . C333 C 0.1439(7) 0.4921(5) 0.8353(5) 0.147(4) Uani 1 1 d DU . . H33H H 0.2000 0.4874 0.7992 0.177 Uiso 1 1 calc R . . H33I H 0.1443 0.5320 0.8668 0.177 Uiso 1 1 calc R . . C334 C 0.1220(10) 0.4205(7) 0.8787(8) 0.237(8) Uani 1 1 d DU . . H33A H 0.1613 0.4100 0.9006 0.355 Uiso 1 1 calc R . . H33B H 0.1231 0.3800 0.8481 0.355 Uiso 1 1 calc R . . H33C H 0.0673 0.4246 0.9159 0.355 Uiso 1 1 calc R . . C341 C -0.0087(4) 0.6316(3) 0.7389(4) 0.0846(17) Uani 1 1 d U . . H34D H -0.0317 0.6494 0.7041 0.101 Uiso 1 1 calc R . . H34E H -0.0370 0.5849 0.7619 0.101 Uiso 1 1 calc R . . C342 C -0.0277(5) 0.6894(5) 0.7955(5) 0.122(3) Uani 1 1 d U . . H34F H -0.0030 0.7377 0.7734 0.146 Uiso 1 1 calc R . . H34G H -0.0050 0.6731 0.8309 0.146 Uiso 1 1 calc R . . C343 C -0.1219(6) 0.6976(7) 0.8322(7) 0.175(5) Uani 1 1 d DU . . H34H H -0.1432 0.7174 0.7969 0.210 Uiso 1 1 calc R . . H34I H -0.1462 0.6479 0.8495 0.210 Uiso 1 1 calc R . . C344 C -0.1478(9) 0.7483(10) 0.8934(8) 0.301(11) Uani 1 1 d DU . . H34A H -0.2074 0.7502 0.9157 0.301 Uiso 1 1 calc R . . H34B H -0.1267 0.7984 0.8762 0.301 Uiso 1 1 calc R . . H34C H -0.1263 0.7294 0.9283 0.301 Uiso 1 1 calc R . . C411 C -0.0574(4) 0.8763(3) 0.1753(3) 0.0756(15) Uani 1 1 d U . . H41D H -0.0841 0.9215 0.2001 0.091 Uiso 1 1 calc R . . H41E H -0.0818 0.8661 0.1408 0.091 Uiso 1 1 calc R . . C412 C -0.0763(4) 0.8106(4) 0.2300(4) 0.0885(18) Uani 1 1 d U . . H41F H -0.0468 0.7660 0.2061 0.106 Uiso 1 1 calc R . . H41G H -0.0559 0.8222 0.2668 0.106 Uiso 1 1 calc R . . C413 C -0.1665(5) 0.7932(5) 0.2654(5) 0.123(3) Uani 1 1 d U . . H41H H -0.1873 0.7842 0.2282 0.148 Uiso 1 1 calc R . . H41I H -0.1955 0.8372 0.2911 0.148 Uiso 1 1 calc R . . C414 C -0.1867(6) 0.7255(5) 0.3177(5) 0.145(3) Uani 1 1 d U . . H41A H -0.2458 0.7182 0.3391 0.217 Uiso 1 1 calc R . . H41B H -0.1668 0.7338 0.3550 0.217 Uiso 1 1 calc R . . H41C H -0.1604 0.6811 0.2925 0.217 Uiso 1 1 calc R . . C421 C 0.0739(4) 0.9137(3) 0.1853(3) 0.0776(16) Uani 1 1 d U . . H42D H 0.0674 0.8714 0.2199 0.093 Uiso 1 1 calc R . . H42E H 0.1330 0.9210 0.1580 0.093 Uiso 1 1 calc R . . C422 C 0.0387(5) 0.9838(4) 0.2263(4) 0.098(2) Uani 1 1 d U . . H42F H -0.0157 0.9723 0.2634 0.118 Uiso 1 1 calc R . . H42G H 0.0316 1.0228 0.1934 0.118 Uiso 1 1 calc R . . C423 C 0.0932(6) 1.0143(5) 0.2615(5) 0.131(3) Uani 1 1 d U . . H42H H 0.1488 1.0222 0.2249 0.157 Uiso 1 1 calc R . . H42I H 0.0969 0.9768 0.2971 0.157 Uiso 1 1 calc R . . C424 C 0.0610(8) 1.0882(5) 0.2982(6) 0.176(5) Uani 1 1 d U . . H42A H 0.0977 1.1050 0.3196 0.264 Uiso 1 1 calc R . . H42B H 0.0065 1.0804 0.3351 0.264 Uiso 1 1 calc R . . H42C H 0.0584 1.1259 0.2630 0.264 Uiso 1 1 calc R . . C431 C 0.0425(4) 0.9582(3) 0.0785(3) 0.0754(15) Uani 1 1 d U . . H43D H 0.0289 0.9393 0.0400 0.090 Uiso 1 1 calc R . . H43E H 0.0016 0.9967 0.1021 0.090 Uiso 1 1 calc R . . C432 C 0.1266(4) 0.9952(3) 0.0452(4) 0.0858(17) Uani 1 1 d U . . H43F H 0.1675 0.9579 0.0188 0.103 Uiso 1 1 calc R . . H43G H 0.1419 1.0125 0.0834 0.103 Uiso 1 1 calc R . . C433 C 0.1286(5) 1.0618(4) -0.0057(4) 0.096(2) Uani 1 1 d U . . H43H H 0.1254 1.0430 -0.0491 0.115 Uiso 1 1 calc R . . H43I H 0.0803 1.0936 0.0173 0.115 Uiso 1 1 calc R . . C434 C 0.2043(6) 1.1081(4) -0.0262(4) 0.123(3) Uani 1 1 d U . . H43A H 0.2024 1.1496 -0.0583 0.185 Uiso 1 1 calc R . . H43B H 0.2524 1.0773 -0.0501 0.185 Uiso 1 1 calc R . . H43C H 0.2074 1.1276 0.0165 0.185 Uiso 1 1 calc R . . C441 C 0.0805(4) 0.8232(3) 0.0938(3) 0.0697(14) Uani 1 1 d U . . H44D H 0.1362 0.8385 0.0616 0.084 Uiso 1 1 calc R . . H44E H 0.0859 0.7862 0.1292 0.084 Uiso 1 1 calc R . . C442 C 0.0401(4) 0.7847(3) 0.0500(3) 0.0753(15) Uani 1 1 d U . . H44F H 0.0353 0.8206 0.0136 0.090 Uiso 1 1 calc R . . H44G H -0.0153 0.7683 0.0816 0.090 Uiso 1 1 calc R . . C443 C 0.0914(4) 0.7168(3) 0.0135(3) 0.0828(17) Uani 1 1 d U . . H44H H 0.1478 0.7330 -0.0156 0.099 Uiso 1 1 calc R . . H44I H 0.0935 0.6799 0.0502 0.099 Uiso 1 1 calc R . . C444 C 0.0554(6) 0.6799(4) -0.0343(4) 0.114(3) Uani 1 1 d U . . H44A H 0.0893 0.6373 -0.0566 0.171 Uiso 1 1 calc R . . H44B H 0.0541 0.7161 -0.0711 0.171 Uiso 1 1 calc R . . H44C H 0.0000 0.6630 -0.0055 0.171 Uiso 1 1 calc R . . C511 C 0.4111(8) 0.9100(7) 0.3819(9) 0.1015(10) Uani 0.50 1 d PDU C 2 H51A H 0.3961 0.9308 0.4292 0.122 Uiso 0.50 1 calc PR C 2 H51B H 0.4511 0.9447 0.3475 0.122 Uiso 0.50 1 calc PR C 2 C512 C 0.3377(9) 0.9147(8) 0.3658(9) 0.1015(10) Uani 0.50 1 d PD C 2 H51C H 0.3536 0.9056 0.3149 0.122 Uiso 0.50 1 calc PR C 2 H51D H 0.3003 0.8742 0.3933 0.122 Uiso 0.50 1 calc PR C 2 C513 C 0.2933(9) 0.9849(8) 0.3810(9) 0.1015(10) Uani 0.50 1 d PD C 2 H51E H 0.3348 1.0247 0.3662 0.122 Uiso 0.50 1 calc PR C 2 H51F H 0.2656 0.9860 0.4332 0.122 Uiso 0.50 1 calc PR C 2 C514 C 0.2300(9) 1.0085(8) 0.3510(8) 0.1015(10) Uani 0.50 1 d PD C 2 H51G H 0.2127 1.0597 0.3634 0.152 Uiso 0.50 1 calc PR C 2 H51H H 0.1829 0.9754 0.3711 0.152 Uiso 0.50 1 calc PR C 2 H51I H 0.2539 1.0054 0.2993 0.152 Uiso 0.50 1 calc PR C 2 C521 C 0.4752(10) 0.7983(8) 0.3093(6) 0.1015(10) Uani 0.50 1 d PD C 2 H52A H 0.5070 0.7523 0.3083 0.122 Uiso 0.50 1 calc PR C 2 H52B H 0.4217 0.7826 0.3108 0.122 Uiso 0.50 1 calc PR C 2 C522 C 0.5165(10) 0.8384(8) 0.2405(6) 0.1015(10) Uani 0.50 1 d PD C 2 H52C H 0.4745 0.8675 0.2300 0.122 Uiso 0.50 1 calc PR C 2 H52D H 0.5538 0.8748 0.2468 0.122 Uiso 0.50 1 calc PR C 2 C523 C 0.5638(9) 0.7974(9) 0.1770(7) 0.1015(10) Uani 0.50 1 d PD C 2 H52E H 0.5748 0.7471 0.1931 0.122 Uiso 0.50 1 calc PR C 2 H52F H 0.6170 0.8225 0.1532 0.122 Uiso 0.50 1 calc PR C 2 C524 C 0.5294(9) 0.7882(8) 0.1229(7) 0.1015(10) Uani 0.50 1 d PD C 2 H52G H 0.5667 0.7583 0.0849 0.152 Uiso 0.50 1 calc PR C 2 H52H H 0.5220 0.8372 0.1031 0.152 Uiso 0.50 1 calc PR C 2 H52I H 0.4766 0.7631 0.1448 0.152 Uiso 0.50 1 calc PR C 2 C531 C 0.4041(9) 0.7835(7) 0.4413(7) 0.1015(10) Uani 0.50 1 d PD C 2 H53A H 0.3745 0.8144 0.4823 0.122 Uiso 0.50 1 calc PR C 2 H53B H 0.3629 0.7641 0.4253 0.122 Uiso 0.50 1 calc PR C 2 C532 C 0.4380(10) 0.7198(8) 0.4675(9) 0.1015(10) Uani 0.50 1 d PD C 2 H53C H 0.4761 0.7390 0.4870 0.122 Uiso 0.50 1 calc PR C 2 H53D H 0.4706 0.6903 0.4263 0.122 Uiso 0.50 1 calc PR C 2 C533 C 0.3802(10) 0.6678(9) 0.5227(10) 0.1015(10) Uani 0.50 1 d PD C 2 H53E H 0.3512 0.6947 0.5667 0.122 Uiso 0.50 1 calc PR C 2 H53F H 0.3393 0.6500 0.5057 0.122 Uiso 0.50 1 calc PR C 2 C534 C 0.4251(9) 0.6030(7) 0.5383(8) 0.1015(10) Uani 0.50 1 d PD C 2 H53G H 0.4072 0.5949 0.5898 0.152 Uiso 0.50 1 calc PR C 2 H53H H 0.4836 0.6131 0.5174 0.152 Uiso 0.50 1 calc PR C 2 H53I H 0.4138 0.5585 0.5180 0.152 Uiso 0.50 1 calc PR C 2 C541 C 0.5349(9) 0.8586(9) 0.3876(7) 0.099(3) Uani 0.50 1 d PD C 2 H54A H 0.5741 0.8181 0.3663 0.119 Uiso 0.50 1 calc PR C 2 H54B H 0.5530 0.9016 0.3532 0.119 Uiso 0.50 1 calc PR C 2 C542 C 0.5530(11) 0.8790(11) 0.4444(8) 0.099(3) Uani 0.50 1 d PD C 2 H54C H 0.5580 0.8289 0.4644 0.119 Uiso 0.50 1 calc PR C 2 H54D H 0.4983 0.8962 0.4761 0.119 Uiso 0.50 1 calc PR C 2 C543 C 0.6007(13) 0.9193(10) 0.4719(13) 0.099(3) Uani 0.50 1 d PD C 2 H54E H 0.5632 0.9314 0.5204 0.119 Uiso 0.50 1 calc PR C 2 H54F H 0.6129 0.9671 0.4439 0.119 Uiso 0.50 1 calc PR C 2 C544 C 0.6799(8) 0.8962(8) 0.4786(7) 0.099(3) Uani 0.50 1 d PD C 2 H54G H 0.6933 0.9318 0.5070 0.148 Uiso 0.50 1 calc PR C 2 H54H H 0.7237 0.8953 0.4313 0.148 Uiso 0.50 1 calc PR C 2 H54I H 0.6737 0.8465 0.5018 0.148 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 Mo1A 0.0741(3) 0.0567(3) 0.0532(3) 0.00515(19) -0.0319(2) 0.0028(2) Mo1 0.0564(3) 0.0630(3) 0.0445(2) -0.00281(18) -0.0119(2) 0.00684(19) Mo2A 0.0424(2) 0.0516(2) 0.0550(3) 0.00036(18) -0.0101(2) 0.00572(17) Mo2 0.0604(3) 0.0615(3) 0.0792(3) -0.0031(2) -0.0432(3) 0.0007(2) Mo3A 0.0647(3) 0.0393(2) 0.0561(3) -0.00381(17) -0.0230(2) 0.00307(17) Mo3 0.0529(2) 0.0397(2) 0.0607(3) 0.00092(17) -0.0227(2) 0.00112(16) Mo4A 0.0525(2) 0.0383(2) 0.0701(3) -0.00550(18) -0.0231(2) 0.00477(16) Mo4 0.0670(3) 0.0402(2) 0.0732(3) -0.00144(19) -0.0321(3) -0.00210(18) Mo5 0.0557(2) 0.0508(2) 0.0544(2) 0.00415(17) -0.0295(2) -0.00106(17) Mo5A 0.0425(2) 0.0566(3) 0.0715(3) -0.0033(2) -0.0159(2) -0.00074(18) Mo6A 0.0624(3) 0.0559(2) 0.0440(2) -0.00036(17) -0.0204(2) 0.00022(19) Mo6 0.0507(2) 0.0637(3) 0.0550(3) 0.0010(2) -0.0043(2) -0.00187(19) O1 0.0422(16) 0.0425(16) 0.0453(17) 0.0010(12) -0.0151(15) -0.0001(12) O1A 0.0438(16) 0.0400(15) 0.0419(16) -0.0026(12) -0.0145(14) 0.0040(12) O2A 0.0449(19) 0.078(2) 0.081(3) -0.001(2) -0.008(2) 0.0096(16) O2 0.095(3) 0.099(3) 0.137(4) -0.001(3) -0.089(3) -0.002(2) O3 0.086(3) 0.0423(18) 0.093(3) -0.0015(17) -0.039(2) 0.0029(17) O3A 0.099(3) 0.0428(18) 0.082(3) -0.0075(17) -0.035(2) 0.0055(18) O4A 0.073(2) 0.0413(18) 0.111(3) -0.0116(19) -0.034(2) 0.0058(16) O4 0.108(3) 0.044(2) 0.118(3) 0.000(2) -0.057(3) -0.0079(19) O5 0.084(3) 0.076(2) 0.086(3) 0.0085(19) -0.058(2) -0.0072(19) O5A 0.047(2) 0.089(3) 0.109(3) -0.004(2) -0.021(2) -0.0055(18) O6A 0.098(3) 0.087(3) 0.052(2) 0.0018(18) -0.035(2) -0.002(2) O6 0.073(3) 0.112(4) 0.073(3) -0.003(2) 0.013(2) -0.004(2) O7 0.082(3) 0.077(2) 0.052(2) -0.0036(17) -0.037(2) 0.0065(19) O7A 0.066(2) 0.062(2) 0.0463(19) 0.0068(15) -0.0147(18) 0.0022(16) O8A 0.081(2) 0.0543(19) 0.062(2) -0.0064(16) -0.034(2) 0.0012(17) O8 0.063(2) 0.0500(18) 0.057(2) 0.0098(15) -0.0176(18) -0.0033(15) O9 0.066(2) 0.0547(19) 0.059(2) -0.0126(15) -0.0206(19) 0.0103(16) O9A 0.071(2) 0.0439(17) 0.071(2) 0.0076(15) -0.033(2) 0.0054(15) O10 0.0454(17) 0.065(2) 0.058(2) 0.0019(15) -0.0166(17) 0.0020(14) O10A 0.058(2) 0.068(2) 0.084(3) 0.0006(18) -0.038(2) 0.0023(16) O11A 0.059(2) 0.0490(18) 0.055(2) -0.0053(14) -0.0151(17) 0.0144(14) O11 0.064(2) 0.0553(19) 0.085(3) 0.0009(17) -0.040(2) 0.0095(16) O12A 0.0506(18) 0.0469(17) 0.068(2) -0.0013(15) -0.0203(18) -0.0020(14) O12 0.072(2) 0.056(2) 0.089(3) -0.0086(18) -0.048(2) -0.0054(16) O13 0.060(2) 0.0490(18) 0.061(2) -0.0026(15) -0.0266(18) -0.0070(14) O13A 0.062(2) 0.0493(18) 0.072(2) 0.0047(16) -0.0256(19) -0.0113(15) O14 0.066(2) 0.0486(18) 0.065(2) 0.0074(15) -0.0330(19) 0.0012(15) O14A 0.0492(19) 0.0543(19) 0.079(2) -0.0148(17) -0.0178(19) 0.0108(15) O15A 0.0535(19) 0.064(2) 0.063(2) -0.0005(16) -0.0276(18) 0.0080(15) O15 0.0427(18) 0.074(2) 0.090(3) -0.002(2) -0.021(2) 0.0029(16) O16A 0.078(2) 0.0478(18) 0.0503(19) 0.0058(14) -0.0230(19) 0.0014(16) O16 0.058(2) 0.0534(19) 0.064(2) -0.0099(16) -0.0049(18) 0.0082(15) O17A 0.064(2) 0.0568(19) 0.056(2) -0.0116(15) -0.0223(18) 0.0041(15) O17 0.065(2) 0.055(2) 0.067(2) 0.0114(16) -0.0176(19) -0.0148(16) O18 0.073(2) 0.069(2) 0.0432(19) -0.0018(15) -0.0171(18) -0.0066(17) O18A 0.057(2) 0.069(2) 0.054(2) -0.0038(16) -0.0073(18) -0.0022(16) N1 0.070(3) 0.087(3) 0.047(2) -0.002(2) -0.009(2) 0.009(2) N1A 0.103(4) 0.077(3) 0.069(3) 0.010(2) -0.049(3) -0.001(3) N2 0.110(3) 0.095(2) 0.092(2) -0.0095(18) -0.030(2) -0.0154(18) N3 0.090(3) 0.085(3) 0.098(4) 0.004(3) -0.030(3) 0.046(3) N4 0.076(3) 0.064(3) 0.099(4) -0.011(2) -0.047(3) -0.016(2) N5 0.078(3) 0.065(3) 0.061(3) -0.0047(19) -0.032(2) 0.028(2) C1 0.076(11) 0.096(10) 0.058(11) 0.014(10) 0.006(8) 0.024(10) C2 0.076(8) 0.091(8) 0.085(8) -0.012(6) -0.017(7) 0.002(6) C3 0.124(13) 0.181(9) 0.153(13) 0.019(12) -0.052(11) 0.078(8) C4 0.197(13) 0.190(9) 0.246(19) 0.061(13) -0.040(15) 0.078(9) C5 0.197 0.190 0.246 0.061 -0.040 0.078 C6 0.197 0.190 0.246 0.061 -0.040 0.078 C1' 0.063(9) 0.094(9) 0.052(10) -0.016(9) -0.004(7) -0.018(8) C2' 0.076(9) 0.142(10) 0.136(13) -0.014(10) -0.017(9) 0.017(7) C3' 0.128(15) 0.136(10) 0.207(17) 0.024(13) -0.025(13) 0.026(9) C4' 0.191(19) 0.166(13) 0.26(2) 0.032(15) -0.001(18) 0.064(13) C5' 0.199(18) 0.173(15) 0.33(2) 0.071(15) 0.009(17) 0.088(14) C6' 0.27(4) 0.40(4) 0.23(3) 0.12(3) -0.06(3) 0.06(3) C1A 0.167(17) 0.145(12) 0.077(10) 0.016(9) -0.070(11) 0.014(13) C2A 0.239(18) 0.203(14) 0.113(13) 0.002(10) -0.097(14) -0.048(14) C3A 0.26(2) 0.229(15) 0.207(19) 0.014(12) -0.144(16) -0.093(15) C4A 0.32(2) 0.266(17) 0.25(2) -0.045(16) -0.109(19) -0.104(18) C5A 0.39(3) 0.265(19) 0.30(3) -0.07(2) -0.06(3) -0.09(2) C6A 0.33(4) 0.28(3) 0.29(3) -0.07(2) -0.07(3) -0.13(3) C1A' 0.099(10) 0.128(11) 0.084(10) 0.024(9) -0.071(9) -0.003(8) C2A' 0.146(13) 0.189(12) 0.128(13) 0.047(10) -0.097(11) -0.065(10) C3A' 0.267(19) 0.190(14) 0.186(19) -0.011(14) -0.065(15) -0.096(14) C4A' 0.33(2) 0.279(19) 0.24(2) -0.052(18) -0.10(2) -0.101(19) C5A' 0.36(2) 0.276(19) 0.23(2) -0.09(2) -0.06(2) -0.12(2) C6A' 0.39(4) 0.37(3) 0.32(3) -0.19(3) -0.11(3) -0.11(3) C111 0.047(5) 0.056(5) 0.028(5) -0.008(4) 0.011(4) -0.010(4) C112 0.065(7) 0.084(8) 0.049(7) -0.010(6) 0.009(6) -0.006(5) C113 0.113(11) 0.112(10) 0.102(11) 0.041(11) -0.048(10) -0.055(10) C114 0.049 0.106 0.071 -0.025 -0.016 -0.015 C121 0.110(3) 0.095(2) 0.092(2) -0.0095(18) -0.030(2) -0.0154(18) C122 0.067(7) 0.066(6) 0.057(6) -0.014(4) 0.003(5) -0.005(5) C123 0.104(9) 0.067(6) 0.066(7) 0.003(5) -0.021(8) -0.018(7) C124 0.122(12) 0.110(11) 0.122(13) -0.001(10) -0.053(11) 0.006(9) C131 0.076(3) 0.080(4) 0.104(5) -0.001(3) -0.047(4) -0.024(3) C132 0.076(3) 0.080(4) 0.104(5) -0.001(3) -0.047(4) -0.024(3) C133 0.076(3) 0.080(4) 0.104(5) -0.001(3) -0.047(4) -0.024(3) C134 0.076(3) 0.080(4) 0.104(5) -0.001(3) -0.047(4) -0.024(3) C141 0.104(5) 0.123(6) 0.060(3) -0.009(3) -0.025(4) -0.046(4) C142 0.104(5) 0.123(6) 0.060(3) -0.009(3) -0.025(4) -0.046(4) C143 0.104(5) 0.123(6) 0.060(3) -0.009(3) -0.025(4) -0.046(4) C144 0.104(5) 0.123(6) 0.060(3) -0.009(3) -0.025(4) -0.046(4) C211 0.123(6) 0.103(5) 0.129(7) -0.027(4) -0.039(5) 0.068(4) C212 0.166(9) 0.161(8) 0.151(8) -0.057(7) -0.076(7) 0.077(7) C213 0.148(10) 0.213(11) 0.278(16) -0.142(11) -0.075(9) 0.068(9) C214 0.217(16) 0.37(2) 0.34(2) -0.217(19) -0.132(15) 0.074(15) C221 0.111(5) 0.104(5) 0.091(5) 0.009(4) -0.023(4) 0.057(4) C222 0.120(6) 0.130(7) 0.134(8) 0.025(5) 0.004(5) 0.049(5) C223 0.148(9) 0.130(8) 0.159(11) 0.020(6) 0.007(7) 0.044(6) C224 0.221(15) 0.145(10) 0.234(16) 0.038(10) -0.059(12) 0.011(9) C231 0.087(5) 0.116(6) 0.115(6) 0.024(4) -0.035(4) 0.037(4) C232 0.090(5) 0.147(7) 0.097(6) 0.021(4) -0.025(4) 0.016(5) C233 0.125(7) 0.220(12) 0.129(8) 0.012(7) -0.063(6) 0.018(7) C234 0.159(10) 0.261(16) 0.192(13) -0.003(10) -0.086(10) -0.018(10) C241 0.089(4) 0.095(4) 0.090(4) -0.005(3) -0.031(3) 0.048(3) C242 0.103(5) 0.101(5) 0.106(5) -0.001(4) -0.035(4) 0.039(4) C243 0.086(4) 0.126(6) 0.093(5) -0.031(4) -0.036(4) 0.021(4) C244 0.102(5) 0.128(7) 0.117(6) -0.031(5) -0.032(5) -0.004(5) C311 0.083(4) 0.074(4) 0.111(5) -0.004(3) -0.044(4) -0.025(3) C312 0.117(6) 0.092(5) 0.126(6) 0.011(4) -0.063(5) -0.030(4) C313 0.119(6) 0.126(7) 0.155(8) 0.039(5) -0.066(6) -0.048(5) C314 0.202(11) 0.170(9) 0.120(8) 0.044(6) -0.074(8) -0.090(8) C321 0.094(4) 0.072(4) 0.090(4) -0.009(3) -0.044(4) -0.021(3) C322 0.102(5) 0.100(5) 0.115(6) -0.028(4) -0.041(5) -0.008(4) C323 0.134(6) 0.096(5) 0.106(6) -0.017(4) -0.049(5) 0.000(4) C324 0.152(8) 0.132(7) 0.110(7) -0.029(5) -0.024(6) 0.009(6) C331 0.089(4) 0.084(4) 0.100(5) -0.011(3) -0.050(4) -0.016(3) C332 0.149(7) 0.115(6) 0.133(7) 0.024(5) -0.083(6) -0.042(5) C333 0.213(10) 0.135(7) 0.136(8) 0.020(5) -0.114(8) -0.044(7) C334 0.337(19) 0.213(13) 0.244(15) 0.099(11) -0.210(15) -0.114(13) C341 0.077(3) 0.076(4) 0.103(5) -0.009(3) -0.037(3) -0.019(3) C342 0.108(5) 0.113(6) 0.145(7) -0.043(5) -0.047(5) 0.002(5) C343 0.113(6) 0.182(10) 0.222(12) -0.109(9) -0.046(7) 0.017(7) C344 0.193(13) 0.33(2) 0.32(2) -0.203(17) -0.013(13) 0.019(13) C411 0.072(3) 0.078(4) 0.072(4) -0.004(3) -0.025(3) 0.028(3) C412 0.082(4) 0.098(5) 0.074(4) 0.009(3) -0.022(3) 0.031(3) C413 0.090(5) 0.135(7) 0.119(7) 0.034(5) -0.018(5) 0.013(4) C414 0.140(8) 0.131(7) 0.132(8) 0.030(6) -0.022(7) -0.021(6) C421 0.092(4) 0.079(4) 0.068(4) -0.010(3) -0.039(3) 0.028(3) C422 0.129(6) 0.095(5) 0.081(4) -0.027(3) -0.051(4) 0.047(4) C423 0.163(8) 0.121(6) 0.138(7) -0.060(5) -0.086(7) 0.046(6) C424 0.280(14) 0.109(7) 0.166(10) -0.057(6) -0.113(10) 0.044(8) C431 0.097(4) 0.063(3) 0.073(4) 0.000(2) -0.041(3) 0.025(3) C432 0.105(5) 0.077(4) 0.078(4) -0.002(3) -0.041(4) 0.017(3) C433 0.134(6) 0.074(4) 0.066(4) -0.003(3) -0.026(4) 0.023(4) C434 0.171(8) 0.099(6) 0.093(6) -0.003(4) -0.043(6) -0.023(5) C441 0.079(4) 0.061(3) 0.068(3) -0.006(2) -0.028(3) 0.028(3) C442 0.082(4) 0.077(4) 0.063(4) -0.004(3) -0.025(3) 0.011(3) C443 0.115(5) 0.062(3) 0.056(3) 0.004(2) -0.018(3) 0.004(3) C444 0.158(8) 0.094(5) 0.080(5) -0.008(4) -0.034(5) -0.020(5) C511 0.110(3) 0.095(2) 0.092(2) -0.0095(18) -0.030(2) -0.0154(18) C512 0.110(3) 0.095(2) 0.092(2) -0.0095(18) -0.030(2) -0.0154(18) C513 0.110(3) 0.095(2) 0.092(2) -0.0095(18) -0.030(2) -0.0154(18) C514 0.110(3) 0.095(2) 0.092(2) -0.0095(18) -0.030(2) -0.0154(18) C521 0.110(3) 0.095(2) 0.092(2) -0.0095(18) -0.030(2) -0.0154(18) C522 0.110(3) 0.095(2) 0.092(2) -0.0095(18) -0.030(2) -0.0154(18) C523 0.110(3) 0.095(2) 0.092(2) -0.0095(18) -0.030(2) -0.0154(18) C524 0.110(3) 0.095(2) 0.092(2) -0.0095(18) -0.030(2) -0.0154(18) C531 0.110(3) 0.095(2) 0.092(2) -0.0095(18) -0.030(2) -0.0154(18) C532 0.110(3) 0.095(2) 0.092(2) -0.0095(18) -0.030(2) -0.0154(18) C533 0.110(3) 0.095(2) 0.092(2) -0.0095(18) -0.030(2) -0.0154(18) C534 0.110(3) 0.095(2) 0.092(2) -0.0095(18) -0.030(2) -0.0154(18) C541 0.110(6) 0.117(6) 0.079(5) 0.020(4) -0.048(5) -0.052(5) C542 0.110(6) 0.117(6) 0.079(5) 0.020(4) -0.048(5) -0.052(5) C543 0.110(6) 0.117(6) 0.079(5) 0.020(4) -0.048(5) -0.052(5) C544 0.110(6) 0.117(6) 0.079(5) 0.020(4) -0.048(5) -0.052(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 Mo1A N1A 1.711(4) . ? Mo1A O9A 1.935(3) . ? Mo1A O7A 1.947(3) . ? Mo1A O8A 1.969(3) . ? Mo1A O10A 1.971(4) . ? Mo1A O1A 2.227(3) . ? Mo1 N1 1.709(4) . ? Mo1 O7 1.936(3) . ? Mo1 O8 1.944(3) . ? Mo1 O9 1.955(3) . ? Mo1 O10 1.973(3) . ? Mo1 O1 2.223(3) . ? Mo2A O2A 1.685(3) . ? Mo2A O12A 1.894(3) . ? Mo2A O7A 1.910(3) . ? Mo2A O15A 1.914(3) . ? Mo2A O11A 1.975(3) . ? Mo2A O1A 2.331(3) . ? Mo2 O2 1.682(3) . ? Mo2 O7 1.909(4) . ? Mo2 O12 1.917(3) . ? Mo2 O15 1.921(4) . ? Mo2 O11 1.959(3) . ? Mo2 O1 2.325(3) . ? Mo3A O3A 1.678(3) . ? Mo3A O8A 1.876(3) . ? Mo3A O11A 1.902(3) . ? Mo3A O16A 1.954(3) . ? Mo3A O13A 1.966(4) . ? Mo3A O1A 2.329(3) . ? Mo3 O3 1.680(3) . ? Mo3 O8 1.896(4) . ? Mo3 O11 1.904(3) . ? Mo3 O16 1.919(4) . ? Mo3 O13 1.957(3) . ? Mo3 O1 2.323(3) . ? Mo4A O4A 1.685(3) . ? Mo4A O14A 1.893(3) . ? Mo4A O17A 1.903(3) . ? Mo4A O9A 1.907(3) . ? Mo4A O12A 1.975(3) . ? Mo4A O1A 2.323(3) . ? Mo4 O4 1.677(3) . ? Mo4 O9 1.883(4) . ? Mo4 O14 1.912(3) . ? Mo4 O17 1.930(4) . ? Mo4 O12 1.960(3) . ? Mo4 O1 2.340(3) . ? Mo5 O5 1.687(3) . ? Mo5 O10 1.874(3) . ? Mo5 O13 1.914(3) . ? Mo5 O18 1.951(4) . ? Mo5 O14 1.951(3) . ? Mo5 O1 2.330(3) . ? Mo5A O5A 1.680(4) . ? Mo5A O10A 1.883(4) . ? Mo5A O13A 1.903(3) . ? Mo5A O18A 1.939(4) . ? Mo5A O14A 1.976(3) . ? Mo5A O1A 2.337(3) . ? Mo6A O6A 1.685(3) . ? Mo6A O16A 1.889(3) . ? Mo6A O18A 1.903(3) . ? Mo6A O15A 1.930(3) . ? Mo6A O17A 1.944(3) . ? Mo6A O1A 2.354(3) . ? Mo6 O6 1.681(4) . ? Mo6 O18 1.897(3) . ? Mo6 O17 1.904(3) . ? Mo6 O16 1.926(3) . ? Mo6 O15 1.936(4) . ? Mo6 O1 2.357(3) . ? N1 C1' 1.436(8) . ? N1 C1 1.438(6) . ? N1A C1A 1.454(8) . ? N1A C1A' 1.456(8) . ? N2 C541 1.451(11) . ? N2 C531 1.468(11) . ? N2 C131 1.508(10) . ? N2 C141 1.518(10) . ? N2 C521 1.554(11) . ? N2 C511 1.558(11) . ? N2 C121 1.562(11) . ? N2 C111 1.566(9) . ? N3 C231 1.511(8) . ? N3 C241 1.520(8) . ? N3 C221 1.524(9) . ? N3 C211 1.526(9) . ? N4 C341 1.516(8) . ? N4 C331 1.518(7) . ? N4 C311 1.519(7) . ? N4 C321 1.521(7) . ? N5 C421 1.513(7) . ? N5 C411 1.522(7) . ? N5 C441 1.530(6) . ? N5 C431 1.531(6) . ? C1 C2 1.481(16) . ? C1 H1A 0.9700 . ? C1 H1B 0.9700 . ? C2 C3 1.529(9) . ? C2 H2A 0.9700 . ? C2 H2B 0.9700 . ? C3 C4 1.544(9) . ? C3 H3A 0.9700 . ? C3 H3B 0.9700 . ? C4 C5 1.541(10) . ? C4 H4A 0.9700 . ? C4 H4B 0.9700 . ? C5 C6 1.565(10) . ? C5 H5A 0.9700 . ? C5 H5B 0.9700 . ? C6 H6A 0.9600 . ? C6 H6B 0.9600 . ? C6 H6C 0.9600 . ? C1' C2' 1.470(16) . ? C1' H1'1 0.9700 . ? C1' H1'2 0.9700 . ? C2' C3' 1.531(15) . ? C2' H2'1 0.9700 . ? C2' H2'2 0.9700 . ? C3' C4' 1.490(17) . ? C3' H3'1 0.9700 . ? C3' H3'2 0.9700 . ? C4' C5' 1.482(18) . ? C4' H4'1 0.9700 . ? C4' H4'2 0.9700 . ? C5' C6' 1.51(2) . ? C5' H5'1 0.9700 . ? C5' H5'2 0.9700 . ? C6' H6'1 0.9600 . ? C6' H6'2 0.9600 . ? C6' H6'3 0.9600 . ? C1A C2A 1.452(17) . ? C1A H1A1 0.9700 . ? C1A H1A2 0.9700 . ? C2A C3A 1.533(17) . ? C2A H2A1 0.9700 . ? C2A H2A2 0.9700 . ? C3A C4A 1.540(18) . ? C3A H3A1 0.9700 . ? C3A H3A2 0.9700 . ? C4A C5A 1.466(19) . ? C4A H4A1 0.9700 . ? C4A H4A2 0.9700 . ? C5A C6A 1.54(2) . ? C5A H5A1 0.9700 . ? C5A H5A2 0.9700 . ? C6A H6A1 0.9600 . ? C6A H6A2 0.9600 . ? C6A H6A3 0.9600 . ? C1A' C2A' 1.483(17) . ? C1A' H1A3 0.9700 . ? C1A' H1A4 0.9700 . ? C2A' C3A' 1.574(17) . ? C2A' H2A3 0.9700 . ? C2A' H2A4 0.9700 . ? C3A' C4A' 1.534(18) . ? C3A' H3A3 0.9700 . ? C3A' H3A4 0.9700 . ? C4A' C5A' 1.494(19) . ? C4A' H4A3 0.9700 . ? C4A' H4A4 0.9700 . ? C5A' C6A' 1.54(2) . ? C5A' H5A3 0.9700 . ? C5A' H5A4 0.9700 . ? C6A' H6A4 0.9600 . ? C6A' H6A5 0.9600 . ? C6A' H6A6 0.9600 . ? C111 C112 1.516(11) . ? C111 H11D 0.9700 . ? C111 H11E 0.9700 . ? C112 C113 1.446(13) . ? C112 H11F 0.9700 . ? C112 H11G 0.9700 . ? C113 C114 1.532(8) . ? C113 H11H 0.9700 . ? C113 H11I 0.9700 . ? C114 H11A 0.9600 . ? C114 H11B 0.9600 . ? C114 H11C 0.9600 . ? C121 C122 1.552(12) . ? C121 H12D 0.9700 . ? C121 H12E 0.9700 . ? C122 C123 1.491(11) . ? C122 H12F 0.9700 . ? C122 H12G 0.9700 . ? C123 C124 1.498(8) . ? C123 H12H 0.9700 . ? C123 H12I 0.9700 . ? C124 H12A 0.9600 . ? C124 H12B 0.9600 . ? C124 H12C 0.9600 . ? C131 C132 1.517(12) . ? C131 H13D 0.9700 . ? C131 H13E 0.9700 . ? C132 C133 1.506(12) . ? C132 H13F 0.9700 . ? C132 H13G 0.9700 . ? C133 C134 1.526(12) . ? C133 H13H 0.9700 . ? C133 H13I 0.9700 . ? C134 H13A 0.9600 . ? C134 H13B 0.9600 . ? C134 H13C 0.9600 . ? C141 C142 1.534(11) . ? C141 H14D 0.9700 . ? C141 H14E 0.9700 . ? C142 C143 1.412(12) . ? C142 H14F 0.9700 . ? C142 H14G 0.9700 . ? C143 C144 1.452(12) . ? C143 H14H 0.9700 . ? C143 H14I 0.9700 . ? C144 H14A 0.9600 . ? C144 H14B 0.9600 . ? C144 H14C 0.9600 . ? C211 C212 1.536(11) . ? C211 H21D 0.9700 . ? C211 H21E 0.9700 . ? C212 C213 1.514(13) . ? C212 H21F 0.9700 . ? C212 H21G 0.9700 . ? C213 C214 1.451(17) . ? C213 H21H 0.9700 . ? C213 H21I 0.9700 . ? C214 H21A 0.9600 . ? C214 H21B 0.9600 . ? C214 H21C 0.9600 . ? C221 C222 1.490(10) . ? C221 H22D 0.9700 . ? C221 H22E 0.9700 . ? C222 C223 1.510(13) . ? C222 H22F 0.9700 . ? C222 H22G 0.9700 . ? C223 C224 1.457(16) . ? C223 H22H 0.9700 . ? C223 H22I 0.9700 . ? C224 H22A 0.9600 . ? C224 H22B 0.9600 . ? C224 H22C 0.9600 . ? C231 C232 1.507(11) . ? C231 H23D 0.9700 . ? C231 H23E 0.9700 . ? C232 C233 1.515(11) . ? C232 H23F 0.9700 . ? C232 H23G 0.9700 . ? C233 C234 1.459(14) . ? C233 H23H 0.9700 . ? C233 H23I 0.9700 . ? C234 H23A 0.9600 . ? C234 H23B 0.9600 . ? C234 H23C 0.9600 . ? C241 C242 1.508(10) . ? C241 H24D 0.9700 . ? C241 H24E 0.9700 . ? C242 C243 1.515(9) . ? C242 H24F 0.9700 . ? C242 H24G 0.9700 . ? C243 C244 1.459(10) . ? C243 H24H 0.9700 . ? C243 H24I 0.9700 . ? C244 H24A 0.9600 . ? C244 H24B 0.9600 . ? C244 H24C 0.9600 . ? C311 C312 1.503(9) . ? C311 H31D 0.9700 . ? C311 H31E 0.9700 . ? C312 C313 1.486(9) . ? C312 H31F 0.9700 . ? C312 H31G 0.9700 . ? C313 C314 1.436(11) . ? C313 H31H 0.9700 . ? C313 H31I 0.9700 . ? C314 H31A 0.9600 . ? C314 H31B 0.9600 . ? C314 H31C 0.9600 . ? C321 C322 1.497(9) . ? C321 H32D 0.9700 . ? C321 H32E 0.9700 . ? C322 C323 1.465(9) . ? C322 H32F 0.9700 . ? C322 H32G 0.9700 . ? C323 C324 1.508(11) . ? C323 H32H 0.9700 . ? C323 H32I 0.9700 . ? C324 H32A 0.9600 . ? C324 H32B 0.9600 . ? C324 H32C 0.9600 . ? C331 C332 1.488(9) . ? C331 H33D 0.9700 . ? C331 H33E 0.9700 . ? C332 C333 1.554(11) . ? C332 H33F 0.9700 . ? C332 H33G 0.9700 . ? C333 C334 1.469(8) . ? C333 H33H 0.9700 . ? C333 H33I 0.9700 . ? C334 H33A 0.9600 . ? C334 H33B 0.9600 . ? C334 H33C 0.9600 . ? C341 C342 1.498(9) . ? C341 H34D 0.9700 . ? C341 H34E 0.9700 . ? C342 C343 1.526(11) . ? C342 H34F 0.9700 . ? C342 H34G 0.9700 . ? C343 C344 1.473(9) . ? C343 H34H 0.9700 . ? C343 H34I 0.9700 . ? C344 H34A 0.9600 . ? C344 H34B 0.9600 . ? C344 H34C 0.9600 . ? C411 C412 1.506(8) . ? C411 H41D 0.9700 . ? C411 H41E 0.9700 . ? C412 C413 1.487(9) . ? C412 H41F 0.9700 . ? C412 H41G 0.9700 . ? C413 C414 1.504(10) . ? C413 H41H 0.9700 . ? C413 H41I 0.9700 . ? C414 H41A 0.9600 . ? C414 H41B 0.9600 . ? C414 H41C 0.9600 . ? C421 C422 1.503(8) . ? C421 H42D 0.9700 . ? C421 H42E 0.9700 . ? C422 C423 1.511(10) . ? C422 H42F 0.9700 . ? C422 H42G 0.9700 . ? C423 C424 1.514(10) . ? C423 H42H 0.9700 . ? C423 H42I 0.9700 . ? C424 H42A 0.9600 . ? C424 H42B 0.9600 . ? C424 H42C 0.9600 . ? C431 C432 1.507(9) . ? C431 H43D 0.9700 . ? C431 H43E 0.9700 . ? C432 C433 1.509(8) . ? C432 H43F 0.9700 . ? C432 H43G 0.9700 . ? C433 C434 1.477(10) . ? C433 H43H 0.9700 . ? C433 H43I 0.9700 . ? C434 H43A 0.9600 . ? C434 H43B 0.9600 . ? C434 H43C 0.9600 . ? C441 C442 1.516(8) . ? C441 H44D 0.9700 . ? C441 H44E 0.9700 . ? C442 C443 1.517(8) . ? C442 H44F 0.9700 . ? C442 H44G 0.9700 . ? C443 C444 1.514(9) . ? C443 H44H 0.9700 . ? C443 H44I 0.9700 . ? C444 H44A 0.9600 . ? C444 H44B 0.9600 . ? C444 H44C 0.9600 . ? C511 C512 1.440(12) . ? C511 H51A 0.9700 . ? C511 H51B 0.9700 . ? C512 C513 1.427(12) . ? C512 H51C 0.9700 . ? C512 H51D 0.9700 . ? C513 C514 1.495(8) . ? C513 H51E 0.9700 . ? C513 H51F 0.9700 . ? C514 H51G 0.9600 . ? C514 H51H 0.9600 . ? C514 H51I 0.9600 . ? C521 C522 1.442(13) . ? C521 H52A 0.9700 . ? C521 H52B 0.9700 . ? C522 C523 1.440(12) . ? C522 H52C 0.9700 . ? C522 H52D 0.9700 . ? C523 C524 1.450(13) . ? C523 H52E 0.9700 . ? C523 H52F 0.9700 . ? C524 H52G 0.9600 . ? C524 H52H 0.9600 . ? C524 H52I 0.9600 . ? C531 C532 1.432(13) . ? C531 H53A 0.9700 . ? C531 H53B 0.9700 . ? C532 C533 1.468(13) . ? C532 H53C 0.9700 . ? C532 H53D 0.9700 . ? C533 C534 1.462(13) . ? C533 H53E 0.9700 . ? C533 H53F 0.9700 . ? C534 H53G 0.9600 . ? C534 H53H 0.9600 . ? C534 H53I 0.9600 . ? C541 C542 1.364(12) . ? C541 H54A 0.9700 . ? C541 H54B 0.9700 . ? C542 C543 1.388(12) . ? C542 H54C 0.9700 . ? C542 H54D 0.9700 . ? C543 C544 1.488(14) . ? C543 H54E 0.9700 . ? C543 H54F 0.9700 . ? C544 H54G 0.9600 . ? C544 H54H 0.9600 . ? C544 H54I 0.9600 . ? 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 N1A Mo1A O9A 100.65(19) . . ? N1A Mo1A O7A 103.0(2) . . ? O9A Mo1A O7A 88.65(15) . . ? N1A Mo1A O8A 103.63(19) . . ? O9A Mo1A O8A 155.71(13) . . ? O7A Mo1A O8A 86.62(15) . . ? N1A Mo1A O10A 101.4(2) . . ? O9A Mo1A O10A 87.79(15) . . ? O7A Mo1A O10A 155.51(14) . . ? O8A Mo1A O10A 86.74(15) . . ? N1A Mo1A O1A 178.37(19) . . ? O9A Mo1A O1A 77.97(12) . . ? O7A Mo1A O1A 77.87(12) . . ? O8A Mo1A O1A 77.74(12) . . ? O10A Mo1A O1A 77.69(12) . . ? N1 Mo1 O7 103.38(19) . . ? N1 Mo1 O8 103.5(2) . . ? O7 Mo1 O8 88.91(15) . . ? N1 Mo1 O9 100.92(19) . . ? O7 Mo1 O9 88.01(15) . . ? O8 Mo1 O9 155.41(14) . . ? N1 Mo1 O10 100.46(18) . . ? O7 Mo1 O10 156.12(15) . . ? O8 Mo1 O10 86.75(14) . . ? O9 Mo1 O10 86.26(14) . . ? N1 Mo1 O1 177.67(17) . . ? O7 Mo1 O1 78.35(13) . . ? O8 Mo1 O1 77.99(13) . . ? O9 Mo1 O1 77.50(13) . . ? O10 Mo1 O1 77.77(12) . . ? O2A Mo2A O12A 104.19(16) . . ? O2A Mo2A O7A 103.83(18) . . ? O12A Mo2A O7A 89.27(14) . . ? O2A Mo2A O15A 102.94(17) . . ? O12A Mo2A O15A 88.23(14) . . ? O7A Mo2A O15A 152.91(14) . . ? O2A Mo2A O11A 102.61(16) . . ? O12A Mo2A O11A 153.18(13) . . ? O7A Mo2A O11A 85.02(14) . . ? O15A Mo2A O11A 85.14(14) . . ? O2A Mo2A O1A 178.44(15) . . ? O12A Mo2A O1A 77.36(12) . . ? O7A Mo2A O1A 75.98(13) . . ? O15A Mo2A O1A 77.15(12) . . ? O11A Mo2A O1A 75.84(12) . . ? O2 Mo2 O7 104.2(2) . . ? O2 Mo2 O12 103.47(18) . . ? O7 Mo2 O12 87.78(16) . . ? O2 Mo2 O15 102.3(2) . . ? O7 Mo2 O15 153.42(14) . . ? O12 Mo2 O15 88.08(17) . . ? O2 Mo2 O11 103.10(17) . . ? O7 Mo2 O11 86.17(16) . . ? O12 Mo2 O11 153.43(13) . . ? O15 Mo2 O11 85.90(16) . . ? O2 Mo2 O1 178.95(18) . . ? O7 Mo2 O1 76.32(12) . . ? O12 Mo2 O1 77.45(12) . . ? O15 Mo2 O1 77.15(12) . . ? O11 Mo2 O1 75.99(11) . . ? O3A Mo3A O8A 104.82(17) . . ? O3A Mo3A O11A 104.35(17) . . ? O8A Mo3A O11A 90.08(15) . . ? O3A Mo3A O16A 101.66(16) . . ? O8A Mo3A O16A 153.31(13) . . ? O11A Mo3A O16A 86.63(15) . . ? O3A Mo3A O13A 102.09(17) . . ? O8A Mo3A O13A 87.09(15) . . ? O11A Mo3A O13A 153.25(13) . . ? O16A Mo3A O13A 84.10(15) . . ? O3A Mo3A O1A 177.56(16) . . ? O8A Mo3A O1A 76.95(12) . . ? O11A Mo3A O1A 77.22(12) . . ? O16A Mo3A O1A 76.49(11) . . ? O13A Mo3A O1A 76.22(12) . . ? O3 Mo3 O8 103.25(17) . . ? O3 Mo3 O11 103.77(16) . . ? O8 Mo3 O11 88.58(15) . . ? O3 Mo3 O16 103.58(18) . . ? O8 Mo3 O16 153.06(13) . . ? O11 Mo3 O16 87.30(16) . . ? O3 Mo3 O13 102.94(15) . . ? O8 Mo3 O13 86.23(14) . . ? O11 Mo3 O13 153.28(13) . . ? O16 Mo3 O13 85.59(15) . . ? O3 Mo3 O1 179.13(14) . . ? O8 Mo3 O1 76.43(12) . . ? O11 Mo3 O1 77.06(12) . . ? O16 Mo3 O1 76.70(12) . . ? O13 Mo3 O1 76.24(11) . . ? O4A Mo4A O14A 103.83(16) . . ? O4A Mo4A O17A 104.08(17) . . ? O14A Mo4A O17A 88.89(16) . . ? O4A Mo4A O9A 102.67(17) . . ? O14A Mo4A O9A 88.71(16) . . ? O17A Mo4A O9A 152.93(13) . . ? O4A Mo4A O12A 102.46(16) . . ? O14A Mo4A O12A 153.71(13) . . ? O17A Mo4A O12A 85.01(14) . . ? O9A Mo4A O12A 85.30(15) . . ? O4A Mo4A O1A 178.12(17) . . ? O14A Mo4A O1A 77.63(12) . . ? O17A Mo4A O1A 77.04(12) . . ? O9A Mo4A O1A 76.11(11) . . ? O12A Mo4A O1A 76.07(11) . . ? O4 Mo4 O9 105.3(2) . . ? O4 Mo4 O14 103.22(17) . . ? O9 Mo4 O14 88.21(15) . . ? O4 Mo4 O17 102.4(2) . . ? O9 Mo4 O17 152.31(14) . . ? O14 Mo4 O17 86.86(15) . . ? O4 Mo4 O12 103.63(17) . . ? O9 Mo4 O12 87.05(16) . . ? O14 Mo4 O12 153.03(13) . . ? O17 Mo4 O12 85.13(16) . . ? O4 Mo4 O1 178.72(19) . . ? O9 Mo4 O1 75.98(12) . . ? O14 Mo4 O1 76.79(11) . . ? O17 Mo4 O1 76.37(12) . . ? O12 Mo4 O1 76.31(12) . . ? O5 Mo5 O10 103.44(18) . . ? O5 Mo5 O13 103.82(16) . . ? O10 Mo5 O13 89.10(15) . . ? O5 Mo5 O18 103.21(18) . . ? O10 Mo5 O18 153.28(13) . . ? O13 Mo5 O18 86.38(15) . . ? O5 Mo5 O14 102.98(15) . . ? O10 Mo5 O14 87.90(15) . . ? O13 Mo5 O14 153.00(12) . . ? O18 Mo5 O14 84.35(15) . . ? O5 Mo5 O1 179.16(15) . . ? O10 Mo5 O1 77.02(12) . . ? O13 Mo5 O1 76.86(11) . . ? O18 Mo5 O1 76.31(12) . . ? O14 Mo5 O1 76.32(11) . . ? O5A Mo5A O10A 104.12(19) . . ? O5A Mo5A O13A 103.66(18) . . ? O10A Mo5A O13A 89.63(15) . . ? O5A Mo5A O18A 102.95(19) . . ? O10A Mo5A O18A 152.68(14) . . ? O13A Mo5A O18A 87.56(15) . . ? O5A Mo5A O14A 103.35(17) . . ? O10A Mo5A O14A 86.12(16) . . ? O13A Mo5A O14A 152.88(13) . . ? O18A Mo5A O14A 84.13(15) . . ? O5A Mo5A O1A 178.84(17) . . ? O10A Mo5A O1A 76.64(12) . . ? O13A Mo5A O1A 77.18(12) . . ? O18A Mo5A O1A 76.24(12) . . ? O14A Mo5A O1A 75.77(12) . . ? O6A Mo6A O16A 104.70(17) . . ? O6A Mo6A O18A 102.50(18) . . ? O16A Mo6A O18A 88.45(15) . . ? O6A Mo6A O15A 104.64(17) . . ? O16A Mo6A O15A 87.67(15) . . ? O18A Mo6A O15A 152.68(14) . . ? O6A Mo6A O17A 102.71(17) . . ? O16A Mo6A O17A 152.59(13) . . ? O18A Mo6A O17A 86.03(15) . . ? O15A Mo6A O17A 85.08(15) . . ? O6A Mo6A O1A 178.00(16) . . ? O16A Mo6A O1A 77.05(11) . . ? O18A Mo6A O1A 76.48(13) . . ? O15A Mo6A O1A 76.30(12) . . ? O17A Mo6A O1A 75.55(12) . . ? O6 Mo6 O18 103.9(2) . . ? O6 Mo6 O17 104.7(2) . . ? O18 Mo6 O17 87.82(15) . . ? O6 Mo6 O16 103.2(2) . . ? O18 Mo6 O16 87.32(15) . . ? O17 Mo6 O16 152.05(15) . . ? O6 Mo6 O15 103.4(2) . . ? O18 Mo6 O15 152.69(15) . . ? O17 Mo6 O15 86.35(15) . . ? O16 Mo6 O15 85.46(16) . . ? O6 Mo6 O1 178.87(18) . . ? O18 Mo6 O1 76.60(12) . . ? O17 Mo6 O1 76.37(13) . . ? O16 Mo6 O1 75.73(12) . . ? O15 Mo6 O1 76.09(13) . . ? Mo1 O1 Mo3 90.71(10) . . ? Mo1 O1 Mo2 90.69(10) . . ? Mo3 O1 Mo2 90.12(9) . . ? Mo1 O1 Mo5 90.60(10) . . ? Mo3 O1 Mo5 90.19(9) . . ? Mo2 O1 Mo5 178.67(14) . . ? Mo1 O1 Mo4 90.80(11) . . ? Mo3 O1 Mo4 178.50(15) . . ? Mo2 O1 Mo4 89.86(9) . . ? Mo5 O1 Mo4 89.79(9) . . ? Mo1 O1 Mo6 179.73(15) . . ? Mo3 O1 Mo6 89.55(10) . . ? Mo2 O1 Mo6 89.39(9) . . ? Mo5 O1 Mo6 89.31(10) . . ? Mo4 O1 Mo6 88.95(10) . . ? Mo1A O1A Mo4A 90.85(10) . . ? Mo1A O1A Mo3A 90.56(10) . . ? Mo4A O1A Mo3A 178.58(13) . . ? Mo1A O1A Mo2A 91.03(10) . . ? Mo4A O1A Mo2A 90.00(10) . . ? Mo3A O1A Mo2A 90.19(10) . . ? Mo1A O1A Mo5A 90.76(10) . . ? Mo4A O1A Mo5A 89.93(10) . . ? Mo3A O1A Mo5A 89.82(10) . . ? Mo2A O1A Mo5A 178.22(13) . . ? Mo1A O1A Mo6A 179.61(14) . . ? Mo4A O1A Mo6A 89.54(9) . . ? Mo3A O1A Mo6A 89.06(9) . . ? Mo2A O1A Mo6A 89.06(9) . . ? Mo5A O1A Mo6A 89.16(10) . . ? Mo2 O7 Mo1 114.63(16) . . ? Mo2A O7A Mo1A 114.97(17) . . ? Mo3A O8A Mo1A 114.69(16) . . ? Mo3 O8 Mo1 114.81(16) . . ? Mo4 O9 Mo1 115.72(16) . . ? Mo4A O9A Mo1A 115.04(15) . . ? Mo5 O10 Mo1 114.58(15) . . ? Mo5A O10A Mo1A 114.89(15) . . ? Mo3A O11A Mo2A 116.74(15) . . ? Mo3 O11 Mo2 116.82(15) . . ? Mo2A O12A Mo4A 116.54(15) . . ? Mo2 O12 Mo4 116.37(15) . . ? Mo5 O13 Mo3 116.70(15) . . ? Mo5A O13A Mo3A 116.74(16) . . ? Mo4 O14 Mo5 117.08(15) . . ? Mo4A O14A Mo5A 116.65(16) . . ? Mo2A O15A Mo6A 117.49(15) . . ? Mo2 O15 Mo6 117.32(16) . . ? Mo6A O16A Mo3A 117.38(15) . . ? Mo3 O16 Mo6 118.02(17) . . ? Mo4A O17A Mo6A 117.77(16) . . ? Mo6 O17 Mo4 118.24(17) . . ? Mo6 O18 Mo5 117.77(16) . . ? Mo6A O18A Mo5A 117.96(18) . . ? C1' N1 C1 2(2) . . ? C1' N1 Mo1 174.1(8) . . ? C1 N1 Mo1 174.6(7) . . ? C1A N1A C1A' 9(2) . . ? C1A N1A Mo1A 169.8(16) . . ? C1A' N1A Mo1A 176.7(10) . . ? C541 N2 C531 117.4(9) . . ? C541 N2 C131 142.2(9) . . ? C531 N2 C131 74.3(7) . . ? C541 N2 C141 78.2(8) . . ? C531 N2 C141 141.5(9) . . ? C131 N2 C141 116.2(9) . . ? C541 N2 C521 111.8(9) . . ? C531 N2 C521 108.4(8) . . ? C131 N2 C521 95.8(9) . . ? C141 N2 C521 37.2(6) . . ? C541 N2 C511 103.9(9) . . ? C531 N2 C511 108.8(9) . . ? C131 N2 C511 41.6(6) . . ? C141 N2 C511 100.0(10) . . ? C521 N2 C511 105.9(9) . . ? C541 N2 C121 98.0(9) . . ? C531 N2 C121 38.8(7) . . ? C131 N2 C121 108.8(8) . . ? C141 N2 C121 107.9(9) . . ? C521 N2 C121 87.5(8) . . ? C511 N2 C121 147.4(9) . . ? C541 N2 C111 36.3(7) . . ? C531 N2 C111 102.2(8) . . ? C131 N2 C111 108.4(7) . . ? C141 N2 C111 108.2(6) . . ? C521 N2 C111 145.1(8) . . ? C511 N2 C111 79.0(7) . . ? C121 N2 C111 107.0(7) . . ? C231 N3 C241 111.0(5) . . ? C231 N3 C221 110.2(6) . . ? C241 N3 C221 106.8(4) . . ? C231 N3 C211 106.4(5) . . ? C241 N3 C211 111.0(6) . . ? C221 N3 C211 111.6(6) . . ? C341 N4 C331 111.1(5) . . ? C341 N4 C311 110.2(5) . . ? C331 N4 C311 106.5(4) . . ? C341 N4 C321 107.4(4) . . ? C331 N4 C321 110.6(5) . . ? C311 N4 C321 111.0(5) . . ? C421 N5 C411 110.2(4) . . ? C421 N5 C441 107.8(4) . . ? C411 N5 C441 111.1(4) . . ? C421 N5 C431 110.5(4) . . ? C411 N5 C431 108.0(4) . . ? C441 N5 C431 109.2(4) . . ? N1 C1 C2 111.9(12) . . ? N1 C1 H1A 109.2 . . ? C2 C1 H1A 109.2 . . ? N1 C1 H1B 109.2 . . ? C2 C1 H1B 109.2 . . ? H1A C1 H1B 107.9 . . ? C1 C2 C3 110.4(14) . . ? C1 C2 H2A 109.6 . . ? C3 C2 H2A 109.6 . . ? C1 C2 H2B 109.6 . . ? C3 C2 H2B 109.6 . . ? H2A C2 H2B 108.1 . . ? C2 C3 C4 116.1(17) . . ? C2 C3 H3A 108.3 . . ? C4 C3 H3A 108.3 . . ? C2 C3 H3B 108.3 . . ? C4 C3 H3B 108.3 . . ? H3A C3 H3B 107.4 . . ? C5 C4 C3 126.5(19) . . ? C5 C4 H4A 105.7 . . ? C3 C4 H4A 105.7 . . ? C5 C4 H4B 105.7 . . ? C3 C4 H4B 105.7 . . ? H4A C4 H4B 106.1 . . ? C4 C5 C6 103.1(17) . . ? C4 C5 H5A 111.1 . . ? C6 C5 H5A 111.1 . . ? C4 C5 H5B 111.1 . . ? C6 C5 H5B 111.1 . . ? H5A C5 H5B 109.1 . . ? C5 C6 H6A 109.5 . . ? C5 C6 H6B 109.5 . . ? H6A C6 H6B 109.5 . . ? C5 C6 H6C 109.5 . . ? H6A C6 H6C 109.5 . . ? H6B C6 H6C 109.5 . . ? N1 C1' C2' 111.2(13) . . ? N1 C1' H1'1 109.4 . . ? C2' C1' H1'1 109.4 . . ? N1 C1' H1'2 109.4 . . ? C2' C1' H1'2 109.4 . . ? H1'1 C1' H1'2 108.0 . . ? C1' C2' C3' 112.3(15) . . ? C1' C2' H2'1 109.1 . . ? C3' C2' H2'1 109.1 . . ? C1' C2' H2'2 109.1 . . ? C3' C2' H2'2 109.1 . . ? H2'1 C2' H2'2 107.9 . . ? C4' C3' C2' 123.4(19) . . ? C4' C3' H3'1 106.5 . . ? C2' C3' H3'1 106.5 . . ? C4' C3' H3'2 106.5 . . ? C2' C3' H3'2 106.5 . . ? H3'1 C3' H3'2 106.5 . . ? C5' C4' C3' 117(2) . . ? C5' C4' H4'1 108.1 . . ? C3' C4' H4'1 108.1 . . ? C5' C4' H4'2 108.1 . . ? C3' C4' H4'2 108.1 . . ? H4'1 C4' H4'2 107.3 . . ? C4' C5' C6' 114(2) . . ? C4' C5' H5'1 108.8 . . ? C6' C5' H5'1 108.8 . . ? C4' C5' H5'2 108.8 . . ? C6' C5' H5'2 108.8 . . ? H5'1 C5' H5'2 107.7 . . ? C5' C6' H6'1 109.5 . . ? C5' C6' H6'2 109.5 . . ? H6'1 C6' H6'2 109.5 . . ? C5' C6' H6'3 109.5 . . ? H6'1 C6' H6'3 109.5 . . ? H6'2 C6' H6'3 109.5 . . ? C2A C1A N1A 115.0(19) . . ? C2A C1A H1A1 108.5 . . ? N1A C1A H1A1 108.5 . . ? C2A C1A H1A2 108.5 . . ? N1A C1A H1A2 108.5 . . ? H1A1 C1A H1A2 107.5 . . ? C1A C2A C3A 116(2) . . ? C1A C2A H2A1 108.4 . . ? C3A C2A H2A1 108.4 . . ? C1A C2A H2A2 108.4 . . ? C3A C2A H2A2 108.4 . . ? H2A1 C2A H2A2 107.5 . . ? C2A C3A C4A 113(2) . . ? C2A C3A H3A1 108.9 . . ? C4A C3A H3A1 108.9 . . ? C2A C3A H3A2 108.9 . . ? C4A C3A H3A2 108.9 . . ? H3A1 C3A H3A2 107.7 . . ? C5A C4A C3A 133(3) . . ? C5A C4A H4A1 104.0 . . ? C3A C4A H4A1 104.0 . . ? C5A C4A H4A2 104.0 . . ? C3A C4A H4A2 104.0 . . ? H4A1 C4A H4A2 105.5 . . ? C4A C5A C6A 111(2) . . ? C4A C5A H5A1 109.4 . . ? C6A C5A H5A1 109.4 . . ? C4A C5A H5A2 109.4 . . ? C6A C5A H5A2 109.4 . . ? H5A1 C5A H5A2 108.0 . . ? C5A C6A H6A1 109.5 . . ? C5A C6A H6A2 109.5 . . ? H6A1 C6A H6A2 109.5 . . ? C5A C6A H6A3 109.5 . . ? H6A1 C6A H6A3 109.5 . . ? H6A2 C6A H6A3 109.5 . . ? N1A C1A' C2A' 110.3(14) . . ? N1A C1A' H1A3 109.6 . . ? C2A' C1A' H1A3 109.6 . . ? N1A C1A' H1A4 109.6 . . ? C2A' C1A' H1A4 109.6 . . ? H1A3 C1A' H1A4 108.1 . . ? C1A' C2A' C3A' 106.6(17) . . ? C1A' C2A' H2A3 110.4 . . ? C3A' C2A' H2A3 110.4 . . ? C1A' C2A' H2A4 110.4 . . ? C3A' C2A' H2A4 110.4 . . ? H2A3 C2A' H2A4 108.6 . . ? C4A' C3A' C2A' 120(2) . . ? C4A' C3A' H3A3 107.3 . . ? C2A' C3A' H3A3 107.3 . . ? C4A' C3A' H3A4 107.3 . . ? C2A' C3A' H3A4 107.3 . . ? H3A3 C3A' H3A4 106.9 . . ? C5A' C4A' C3A' 124(3) . . ? C5A' C4A' H4A3 106.4 . . ? C3A' C4A' H4A3 106.4 . . ? C5A' C4A' H4A4 106.4 . . ? C3A' C4A' H4A4 106.4 . . ? H4A3 C4A' H4A4 106.5 . . ? C4A' C5A' C6A' 110(2) . . ? C4A' C5A' H5A3 109.6 . . ? C6A' C5A' H5A3 109.6 . . ? C4A' C5A' H5A4 109.6 . . ? C6A' C5A' H5A4 109.6 . . ? H5A3 C5A' H5A4 108.2 . . ? C5A' C6A' H6A4 109.5 . . ? C5A' C6A' H6A5 109.5 . . ? H6A4 C6A' H6A5 109.5 . . ? C5A' C6A' H6A6 109.5 . . ? H6A4 C6A' H6A6 109.5 . . ? H6A5 C6A' H6A6 109.5 . . ? C112 C111 N2 112.7(8) . . ? C112 C111 H11D 109.1 . . ? N2 C111 H11D 109.1 . . ? C112 C111 H11E 109.1 . . ? N2 C111 H11E 109.1 . . ? H11D C111 H11E 107.8 . . ? C113 C112 C111 115.7(11) . . ? C113 C112 H11F 108.4 . . ? C111 C112 H11F 108.4 . . ? C113 C112 H11G 108.4 . . ? C111 C112 H11G 108.4 . . ? H11F C112 H11G 107.4 . . ? C112 C113 C114 94.3(10) . . ? C112 C113 H11H 112.9 . . ? C114 C113 H11H 112.9 . . ? C112 C113 H11I 112.9 . . ? C114 C113 H11I 112.9 . . ? H11H C113 H11I 110.3 . . ? C113 C114 H11A 109.5 . . ? C113 C114 H11B 109.5 . . ? H11A C114 H11B 109.5 . . ? C113 C114 H11C 109.5 . . ? H11A C114 H11C 109.5 . . ? H11B C114 H11C 109.5 . . ? C122 C121 N2 114.5(9) . . ? C122 C121 H12D 108.6 . . ? N2 C121 H12D 108.6 . . ? C122 C121 H12E 108.6 . . ? N2 C121 H12E 108.6 . . ? H12D C121 H12E 107.6 . . ? C123 C122 C121 109.8(10) . . ? C123 C122 H12F 109.7 . . ? C121 C122 H12F 109.7 . . ? C123 C122 H12G 109.7 . . ? C121 C122 H12G 109.7 . . ? H12F C122 H12G 108.2 . . ? C122 C123 C124 114.9(10) . . ? C122 C123 H12H 108.5 . . ? C124 C123 H12H 108.5 . . ? C122 C123 H12I 108.5 . . ? C124 C123 H12I 108.5 . . ? H12H C123 H12I 107.5 . . ? C123 C124 H12A 109.5 . . ? C123 C124 H12B 109.5 . . ? H12A C124 H12B 109.5 . . ? C123 C124 H12C 109.5 . . ? H12A C124 H12C 109.5 . . ? H12B C124 H12C 109.5 . . ? N2 C131 C132 111.8(8) . . ? N2 C131 H13D 109.2 . . ? C132 C131 H13D 109.2 . . ? N2 C131 H13E 109.2 . . ? C132 C131 H13E 109.2 . . ? H13D C131 H13E 107.9 . . ? C133 C132 C131 108.1(9) . . ? C133 C132 H13F 110.1 . . ? C131 C132 H13F 110.1 . . ? C133 C132 H13G 110.1 . . ? C131 C132 H13G 110.1 . . ? H13F C132 H13G 108.4 . . ? C132 C133 C134 105.5(9) . . ? C132 C133 H13H 110.6 . . ? C134 C133 H13H 110.6 . . ? C132 C133 H13I 110.6 . . ? C134 C133 H13I 110.6 . . ? H13H C133 H13I 108.8 . . ? C133 C134 H13A 109.5 . . ? C133 C134 H13B 109.5 . . ? H13A C134 H13B 109.5 . . ? C133 C134 H13C 109.5 . . ? H13A C134 H13C 109.5 . . ? H13B C134 H13C 109.5 . . ? N2 C141 C142 110.8(9) . . ? N2 C141 H14D 109.5 . . ? C142 C141 H14D 109.5 . . ? N2 C141 H14E 109.5 . . ? C142 C141 H14E 109.5 . . ? H14D C141 H14E 108.1 . . ? C143 C142 C141 121.1(10) . . ? C143 C142 H14F 107.1 . . ? C141 C142 H14F 107.1 . . ? C143 C142 H14G 107.1 . . ? C141 C142 H14G 107.1 . . ? H14F C142 H14G 106.8 . . ? C142 C143 C144 124.9(12) . . ? C142 C143 H14H 106.1 . . ? C144 C143 H14H 106.1 . . ? C142 C143 H14I 106.1 . . ? C144 C143 H14I 106.1 . . ? H14H C143 H14I 106.3 . . ? C143 C144 H14A 109.5 . . ? C143 C144 H14B 109.5 . . ? H14A C144 H14B 109.5 . . ? C143 C144 H14C 109.5 . . ? H14A C144 H14C 109.5 . . ? H14B C144 H14C 109.5 . . ? N3 C211 C212 115.9(6) . . ? N3 C211 H21D 108.3 . . ? C212 C211 H21D 108.3 . . ? N3 C211 H21E 108.3 . . ? C212 C211 H21E 108.3 . . ? H21D C211 H21E 107.4 . . ? C213 C212 C211 110.8(9) . . ? C213 C212 H21F 109.5 . . ? C211 C212 H21F 109.5 . . ? C213 C212 H21G 109.5 . . ? C211 C212 H21G 109.5 . . ? H21F C212 H21G 108.1 . . ? C214 C213 C212 110.9(13) . . ? C214 C213 H21H 109.5 . . ? C212 C213 H21H 109.5 . . ? C214 C213 H21I 109.5 . . ? C212 C213 H21I 109.5 . . ? H21H C213 H21I 108.0 . . ? C213 C214 H21A 109.5 . . ? C213 C214 H21B 109.5 . . ? H21A C214 H21B 109.5 . . ? C213 C214 H21C 109.5 . . ? H21A C214 H21C 109.5 . . ? H21B C214 H21C 109.5 . . ? C222 C221 N3 114.5(5) . . ? C222 C221 H22D 108.6 . . ? N3 C221 H22D 108.6 . . ? C222 C221 H22E 108.6 . . ? N3 C221 H22E 108.6 . . ? H22D C221 H22E 107.6 . . ? C221 C222 C223 112.2(7) . . ? C221 C222 H22F 109.2 . . ? C223 C222 H22F 109.2 . . ? C221 C222 H22G 109.2 . . ? C223 C222 H22G 109.2 . . ? H22F C222 H22G 107.9 . . ? C224 C223 C222 106.3(12) . . ? C224 C223 H22H 110.5 . . ? C222 C223 H22H 110.5 . . ? C224 C223 H22I 110.5 . . ? C222 C223 H22I 110.5 . . ? H22H C223 H22I 108.7 . . ? C223 C224 H22A 109.5 . . ? C223 C224 H22B 109.5 . . ? H22A C224 H22B 109.5 . . ? C223 C224 H22C 109.5 . . ? H22A C224 H22C 109.5 . . ? H22B C224 H22C 109.5 . . ? C232 C231 N3 116.0(6) . . ? C232 C231 H23D 108.3 . . ? N3 C231 H23D 108.3 . . ? C232 C231 H23E 108.3 . . ? N3 C231 H23E 108.3 . . ? H23D C231 H23E 107.4 . . ? C231 C232 C233 109.1(8) . . ? C231 C232 H23F 109.9 . . ? C233 C232 H23F 109.9 . . ? C231 C232 H23G 109.9 . . ? C233 C232 H23G 109.9 . . ? H23F C232 H23G 108.3 . . ? C234 C233 C232 113.6(10) . . ? C234 C233 H23H 108.8 . . ? C232 C233 H23H 108.8 . . ? C234 C233 H23I 108.8 . . ? C232 C233 H23I 108.8 . . ? H23H C233 H23I 107.7 . . ? C233 C234 H23A 109.5 . . ? C233 C234 H23B 109.5 . . ? H23A C234 H23B 109.5 . . ? C233 C234 H23C 109.5 . . ? H23A C234 H23C 109.5 . . ? H23B C234 H23C 109.5 . . ? C242 C241 N3 116.8(5) . . ? C242 C241 H24D 108.1 . . ? N3 C241 H24D 108.1 . . ? C242 C241 H24E 108.1 . . ? N3 C241 H24E 108.1 . . ? H24D C241 H24E 107.3 . . ? C241 C242 C243 111.5(6) . . ? C241 C242 H24F 109.3 . . ? C243 C242 H24F 109.3 . . ? C241 C242 H24G 109.3 . . ? C243 C242 H24G 109.3 . . ? H24F C242 H24G 108.0 . . ? C244 C243 C242 113.7(7) . . ? C244 C243 H24H 108.8 . . ? C242 C243 H24H 108.8 . . ? C244 C243 H24I 108.8 . . ? C242 C243 H24I 108.8 . . ? H24H C243 H24I 107.7 . . ? C243 C244 H24A 109.5 . . ? C243 C244 H24B 109.5 . . ? H24A C244 H24B 109.5 . . ? C243 C244 H24C 109.5 . . ? H24A C244 H24C 109.5 . . ? H24B C244 H24C 109.5 . . ? C312 C311 N4 116.0(5) . . ? C312 C311 H31D 108.3 . . ? N4 C311 H31D 108.3 . . ? C312 C311 H31E 108.3 . . ? N4 C311 H31E 108.3 . . ? H31D C311 H31E 107.4 . . ? C313 C312 C311 111.9(6) . . ? C313 C312 H31F 109.2 . . ? C311 C312 H31F 109.2 . . ? C313 C312 H31G 109.2 . . ? C311 C312 H31G 109.2 . . ? H31F C312 H31G 107.9 . . ? C314 C313 C312 116.9(7) . . ? C314 C313 H31H 108.1 . . ? C312 C313 H31H 108.1 . . ? C314 C313 H31I 108.1 . . ? C312 C313 H31I 108.1 . . ? H31H C313 H31I 107.3 . . ? C313 C314 H31A 109.5 . . ? C313 C314 H31B 109.5 . . ? H31A C314 H31B 109.5 . . ? C313 C314 H31C 109.5 . . ? H31A C314 H31C 109.5 . . ? H31B C314 H31C 109.5 . . ? C322 C321 N4 115.6(5) . . ? C322 C321 H32D 108.4 . . ? N4 C321 H32D 108.4 . . ? C322 C321 H32E 108.4 . . ? N4 C321 H32E 108.4 . . ? H32D C321 H32E 107.4 . . ? C323 C322 C321 113.0(6) . . ? C323 C322 H32F 109.0 . . ? C321 C322 H32F 109.0 . . ? C323 C322 H32G 109.0 . . ? C321 C322 H32G 109.0 . . ? H32F C322 H32G 107.8 . . ? C322 C323 C324 113.2(7) . . ? C322 C323 H32H 108.9 . . ? C324 C323 H32H 108.9 . . ? C322 C323 H32I 108.9 . . ? C324 C323 H32I 108.9 . . ? H32H C323 H32I 107.8 . . ? C323 C324 H32A 109.5 . . ? C323 C324 H32B 109.5 . . ? H32A C324 H32B 109.5 . . ? C323 C324 H32C 109.5 . . ? H32A C324 H32C 109.5 . . ? H32B C324 H32C 109.5 . . ? C332 C331 N4 116.0(5) . . ? C332 C331 H33D 108.3 . . ? N4 C331 H33D 108.3 . . ? C332 C331 H33E 108.3 . . ? N4 C331 H33E 108.3 . . ? H33D C331 H33E 107.4 . . ? C331 C332 C333 108.0(6) . . ? C331 C332 H33F 110.1 . . ? C333 C332 H33F 110.1 . . ? C331 C332 H33G 110.1 . . ? C333 C332 H33G 110.1 . . ? H33F C332 H33G 108.4 . . ? C334 C333 C332 116.2(8) . . ? C334 C333 H33H 108.2 . . ? C332 C333 H33H 108.2 . . ? C334 C333 H33I 108.2 . . ? C332 C333 H33I 108.2 . . ? H33H C333 H33I 107.4 . . ? C333 C334 H33A 109.5 . . ? C333 C334 H33B 109.5 . . ? H33A C334 H33B 109.5 . . ? C333 C334 H33C 109.5 . . ? H33A C334 H33C 109.5 . . ? H33B C334 H33C 109.5 . . ? C342 C341 N4 115.8(5) . . ? C342 C341 H34D 108.3 . . ? N4 C341 H34D 108.3 . . ? C342 C341 H34E 108.3 . . ? N4 C341 H34E 108.3 . . ? H34D C341 H34E 107.4 . . ? C341 C342 C343 108.2(6) . . ? C341 C342 H34F 110.1 . . ? C343 C342 H34F 110.1 . . ? C341 C342 H34G 110.1 . . ? C343 C342 H34G 110.1 . . ? H34F C342 H34G 108.4 . . ? C344 C343 C342 112.7(9) . . ? C344 C343 H34H 109.1 . . ? C342 C343 H34H 109.1 . . ? C344 C343 H34I 109.1 . . ? C342 C343 H34I 109.1 . . ? H34H C343 H34I 107.8 . . ? C343 C344 H34A 109.5 . . ? C343 C344 H34B 109.5 . . ? H34A C344 H34B 109.5 . . ? C343 C344 H34C 109.5 . . ? H34A C344 H34C 109.5 . . ? H34B C344 H34C 109.5 . . ? C412 C411 N5 114.9(4) . . ? C412 C411 H41D 108.5 . . ? N5 C411 H41D 108.5 . . ? C412 C411 H41E 108.5 . . ? N5 C411 H41E 108.5 . . ? H41D C411 H41E 107.5 . . ? C413 C412 C411 113.1(5) . . ? C413 C412 H41F 109.0 . . ? C411 C412 H41F 109.0 . . ? C413 C412 H41G 109.0 . . ? C411 C412 H41G 109.0 . . ? H41F C412 H41G 107.8 . . ? C412 C413 C414 114.1(7) . . ? C412 C413 H41H 108.7 . . ? C414 C413 H41H 108.7 . . ? C412 C413 H41I 108.7 . . ? C414 C413 H41I 108.7 . . ? H41H C413 H41I 107.6 . . ? C413 C414 H41A 109.5 . . ? C413 C414 H41B 109.5 . . ? H41A C414 H41B 109.5 . . ? C413 C414 H41C 109.5 . . ? H41A C414 H41C 109.5 . . ? H41B C414 H41C 109.5 . . ? C422 C421 N5 114.7(4) . . ? C422 C421 H42D 108.6 . . ? N5 C421 H42D 108.6 . . ? C422 C421 H42E 108.6 . . ? N5 C421 H42E 108.6 . . ? H42D C421 H42E 107.6 . . ? C421 C422 C423 112.8(6) . . ? C421 C422 H42F 109.0 . . ? C423 C422 H42F 109.0 . . ? C421 C422 H42G 109.0 . . ? C423 C422 H42G 109.0 . . ? H42F C422 H42G 107.8 . . ? C422 C423 C424 112.8(7) . . ? C422 C423 H42H 109.0 . . ? C424 C423 H42H 109.0 . . ? C422 C423 H42I 109.0 . . ? C424 C423 H42I 109.0 . . ? H42H C423 H42I 107.8 . . ? C423 C424 H42A 109.5 . . ? C423 C424 H42B 109.5 . . ? H42A C424 H42B 109.5 . . ? C423 C424 H42C 109.5 . . ? H42A C424 H42C 109.5 . . ? H42B C424 H42C 109.5 . . ? C432 C431 N5 115.5(5) . . ? C432 C431 H43D 108.4 . . ? N5 C431 H43D 108.4 . . ? C432 C431 H43E 108.4 . . ? N5 C431 H43E 108.4 . . ? H43D C431 H43E 107.5 . . ? C431 C432 C433 112.6(5) . . ? C431 C432 H43F 109.1 . . ? C433 C432 H43F 109.1 . . ? C431 C432 H43G 109.1 . . ? C433 C432 H43G 109.1 . . ? H43F C432 H43G 107.8 . . ? C434 C433 C432 112.8(7) . . ? C434 C433 H43H 109.0 . . ? C432 C433 H43H 109.0 . . ? C434 C433 H43I 109.0 . . ? C432 C433 H43I 109.0 . . ? H43H C433 H43I 107.8 . . ? C433 C434 H43A 109.5 . . ? C433 C434 H43B 109.5 . . ? H43A C434 H43B 109.5 . . ? C433 C434 H43C 109.5 . . ? H43A C434 H43C 109.5 . . ? H43B C434 H43C 109.5 . . ? C442 C441 N5 115.5(4) . . ? C442 C441 H44D 108.4 . . ? N5 C441 H44D 108.4 . . ? C442 C441 H44E 108.4 . . ? N5 C441 H44E 108.4 . . ? H44D C441 H44E 107.5 . . ? C441 C442 C443 110.3(5) . . ? C441 C442 H44F 109.6 . . ? C443 C442 H44F 109.6 . . ? C441 C442 H44G 109.6 . . ? C443 C442 H44G 109.6 . . ? H44F C442 H44G 108.1 . . ? C444 C443 C442 111.6(6) . . ? C444 C443 H44H 109.3 . . ? C442 C443 H44H 109.3 . . ? C444 C443 H44I 109.3 . . ? C442 C443 H44I 109.3 . . ? H44H C443 H44I 108.0 . . ? C443 C444 H44A 109.5 . . ? C443 C444 H44B 109.5 . . ? H44A C444 H44B 109.5 . . ? C443 C444 H44C 109.5 . . ? H44A C444 H44C 109.5 . . ? H44B C444 H44C 109.5 . . ? C512 C511 N2 123.4(10) . . ? C512 C511 H51A 106.5 . . ? N2 C511 H51A 106.5 . . ? C512 C511 H51B 106.5 . . ? N2 C511 H51B 106.5 . . ? H51A C511 H51B 106.5 . . ? C513 C512 C511 115.6(11) . . ? C513 C512 H51C 108.4 . . ? C511 C512 H51C 108.4 . . ? C513 C512 H51D 108.4 . . ? C511 C512 H51D 108.4 . . ? H51C C512 H51D 107.4 . . ? C512 C513 C514 123.3(12) . . ? C512 C513 H51E 106.5 . . ? C514 C513 H51E 106.5 . . ? C512 C513 H51F 106.5 . . ? C514 C513 H51F 106.5 . . ? H51E C513 H51F 106.5 . . ? C513 C514 H51G 109.5 . . ? C513 C514 H51H 109.5 . . ? H51G C514 H51H 109.5 . . ? C513 C514 H51I 109.5 . . ? H51G C514 H51I 109.5 . . ? H51H C514 H51I 109.5 . . ? C522 C521 N2 122.7(11) . . ? C522 C521 H52A 106.7 . . ? N2 C521 H52A 106.7 . . ? C522 C521 H52B 106.7 . . ? N2 C521 H52B 106.7 . . ? H52A C521 H52B 106.6 . . ? C523 C522 C521 120.3(12) . . ? C523 C522 H52C 107.3 . . ? C521 C522 H52C 107.3 . . ? C523 C522 H52D 107.3 . . ? C521 C522 H52D 107.3 . . ? H52C C522 H52D 106.9 . . ? C522 C523 C524 119.0(13) . . ? C522 C523 H52E 107.6 . . ? C524 C523 H52E 107.6 . . ? C522 C523 H52F 107.6 . . ? C524 C523 H52F 107.6 . . ? H52E C523 H52F 107.0 . . ? C523 C524 H52G 109.5 . . ? C523 C524 H52H 109.5 . . ? H52G C524 H52H 109.5 . . ? C523 C524 H52I 109.5 . . ? H52G C524 H52I 109.5 . . ? H52H C524 H52I 109.5 . . ? C532 C531 N2 120.4(12) . . ? C532 C531 H53A 107.2 . . ? N2 C531 H53A 107.2 . . ? C532 C531 H53B 107.2 . . ? N2 C531 H53B 107.2 . . ? H53A C531 H53B 106.9 . . ? C531 C532 C533 118.2(13) . . ? C531 C532 H53C 107.8 . . ? C533 C532 H53C 107.8 . . ? C531 C532 H53D 107.8 . . ? C533 C532 H53D 107.8 . . ? H53C C532 H53D 107.1 . . ? C534 C533 C532 110.6(13) . . ? C534 C533 H53E 109.5 . . ? C532 C533 H53E 109.5 . . ? C534 C533 H53F 109.5 . . ? C532 C533 H53F 109.5 . . ? H53E C533 H53F 108.1 . . ? C533 C534 H53G 109.5 . . ? C533 C534 H53H 109.5 . . ? H53G C534 H53H 109.5 . . ? C533 C534 H53I 109.5 . . ? H53G C534 H53I 109.5 . . ? H53H C534 H53I 109.5 . . ? C542 C541 N2 132.4(14) . . ? C542 C541 H54A 104.1 . . ? N2 C541 H54A 104.1 . . ? C542 C541 H54B 104.1 . . ? N2 C541 H54B 104.1 . . ? H54A C541 H54B 105.5 . . ? C541 C542 C543 150.6(18) . . ? C541 C542 H54C 99.0 . . ? C543 C542 H54C 99.0 . . ? C541 C542 H54D 99.0 . . ? C543 C542 H54D 99.0 . . ? H54C C542 H54D 103.9 . . ? C542 C543 C544 128.6(16) . . ? C542 C543 H54E 105.1 . . ? C544 C543 H54E 105.1 . . ? C542 C543 H54F 105.1 . . ? C544 C543 H54F 105.1 . . ? H54E C543 H54F 105.9 . . ? C543 C544 H54G 109.5 . . ? C543 C544 H54H 109.5 . . ? H54G C544 H54H 109.5 . . ? C543 C544 H54I 109.5 . . ? H54G C544 H54I 109.5 . . ? H54H C544 H54I 109.5 . . ? _diffrn_measured_fraction_theta_max 0.949 _diffrn_reflns_theta_full 25.00 _diffrn_measured_fraction_theta_full 0.949 _refine_diff_density_max 1.508 _refine_diff_density_min -1.341 _refine_diff_density_rms 0.076 #===END