# Supplementary Material (ESI) for New Journal of Chemistry # This journal is © The Royal Society of Chemistry and # The Centre National de la Recherche Scientifique, 2002 data_global _journal_coden_Cambridge 440 _publ_requested_journal 'New Journal of Chemistry' loop_ _publ_author_name 'Redshaw, Carl' 'Elsegood, Mark R. J.' 'Gibson, Vernon C.' _publ_contact_author_name 'Dr Carl Redshaw' _publ_contact_author_address ; School of Chemical Sciences University of East Anglia Norwich NR4 7TJ UNITED KINGDOM ; _publ_contact_author_email 'CARL.REDSHAW@UEA.AC.UK' _publ_section_title ; A novel ligand family on bulky metallocalix[4] and [8]arene substituents ; data_1 _database_code_CSD 173184 _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C70 H78 Mo N6 O4' _chemical_formula_weight 1163.32 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 P2(1)/n loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x+1/2, y+1/2, -z+1/2' '-x, -y, -z' 'x-1/2, -y-1/2, z-1/2' _cell_length_a 14.142(2) _cell_length_b 21.946(3) _cell_length_c 20.008(3) _cell_angle_alpha 90.00 _cell_angle_beta 90.146(3) _cell_angle_gamma 90.00 _cell_volume 6209.5(16) _cell_formula_units_Z 4 _cell_measurement_temperature 160(2) _cell_measurement_reflns_used 2784 _cell_measurement_theta_min 2.68 _cell_measurement_theta_max 21.58 _exptl_crystal_description needle _exptl_crystal_colour yellow _exptl_crystal_size_max 0.08 _exptl_crystal_size_mid 0.02 _exptl_crystal_size_min 0.01 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.244 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 2456 _exptl_absorpt_coefficient_mu 0.264 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.979 _exptl_absorpt_correction_T_max 0.997 _exptl_absorpt_process_details ? _exptl_special_details ; ? ; _diffrn_ambient_temperature 160(2) _diffrn_radiation_wavelength 0.6923 _diffrn_radiation_type synchrotron _diffrn_radiation_source 'Daresbury SRS station 9.8' _diffrn_radiation_monochromator 'silicon 111' _diffrn_measurement_device_type 'Bruker SMART 1K CCD diffractometer' _diffrn_measurement_method '\w rotation with narrow frames' _diffrn_detector_area_resol_mean ? _diffrn_standards_number 0 _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% 11 _diffrn_reflns_number 29388 _diffrn_reflns_av_R_equivalents 0.1887 _diffrn_reflns_av_sigmaI/netI 0.2545 _diffrn_reflns_limit_h_min -10 _diffrn_reflns_limit_h_max 16 _diffrn_reflns_limit_k_min -25 _diffrn_reflns_limit_k_max 25 _diffrn_reflns_limit_l_min -22 _diffrn_reflns_limit_l_max 23 _diffrn_reflns_theta_min 2.59 _diffrn_reflns_theta_max 24.00 _reflns_number_total 10529 _reflns_number_gt 5448 _reflns_threshold_expression I>2\s(I) _computing_data_collection 'Bruker SMART' _computing_cell_refinement 'Bruker SAINT' _computing_data_reduction 'Bruker SAINT' _computing_structure_solution 'Bruker SHELXTL' _computing_structure_refinement 'Bruker SHELXTL' _computing_molecular_graphics 'Bruker SHELXTL' _computing_publication_material 'Bruker SHELXTL and local programs' _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^)+(0.1015P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary heavy _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 10529 _refine_ls_number_parameters 746 _refine_ls_number_restraints 1264 _refine_ls_R_factor_all 0.1929 _refine_ls_R_factor_gt 0.0926 _refine_ls_wR_factor_ref 0.2341 _refine_ls_wR_factor_gt 0.1885 _refine_ls_goodness_of_fit_ref 0.989 _refine_ls_restrained_S_all 0.949 _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 0.86977(8) 0.82715(3) 0.98488(5) 0.0131(2) Uani 1 1 d U . . O1 O 0.9640(5) 0.8717(3) 0.9352(4) 0.0139(10) Uani 1 1 d U . . O2 O 0.7722(5) 0.8701(3) 0.9354(4) 0.0149(10) Uani 1 1 d U . . O3 O 0.7732(5) 0.7703(3) 1.0142(5) 0.0157(10) Uani 1 1 d U . . O4 O 0.9658(5) 0.7708(3) 1.0146(5) 0.0155(10) Uani 1 1 d U . . C1 C 1.0015(8) 0.8606(5) 0.8727(5) 0.0118(14) Uani 1 1 d U . . C2 C 1.0798(7) 0.8235(5) 0.8665(5) 0.0135(13) Uani 1 1 d U . . C3 C 1.1160(9) 0.8135(4) 0.8027(4) 0.0154(17) Uani 1 1 d U . . H3 H 1.1686 0.7870 0.7980 0.018 Uiso 1 1 calc R . . C4 C 1.0785(8) 0.8405(5) 0.7457(5) 0.0202(17) Uani 1 1 d U . . C5 C 0.9983(8) 0.8760(5) 0.7555(6) 0.0186(18) Uani 1 1 d U . . H5 H 0.9689 0.8933 0.7172 0.022 Uiso 1 1 calc R . . C6 C 0.9583(8) 0.8879(5) 0.8176(5) 0.0137(14) Uani 1 1 d U . . C7 C 1.1201(11) 0.8313(5) 0.6773(5) 0.0310(19) Uani 1 1 d U . . C8 C 1.1722(12) 0.8921(7) 0.6581(7) 0.062(4) Uani 1 1 d U . . H8A H 1.1262 0.9255 0.6564 0.094 Uiso 1 1 calc R . . H8B H 1.2021 0.8875 0.6143 0.094 Uiso 1 1 calc R . . H8C H 1.2206 0.9012 0.6918 0.094 Uiso 1 1 calc R . . C9 C 1.0452(11) 0.8226(8) 0.6244(7) 0.065(4) Uani 1 1 d U . . H9A H 1.0023 0.7899 0.6379 0.098 Uiso 1 1 calc R . . H9B H 1.0753 0.8119 0.5819 0.098 Uiso 1 1 calc R . . H9C H 1.0094 0.8605 0.6189 0.098 Uiso 1 1 calc R . . C10 C 1.1934(11) 0.7816(7) 0.6737(7) 0.053(4) Uani 1 1 d U . . H10A H 1.2416 0.7884 0.7082 0.079 Uiso 1 1 calc R . . H10B H 1.2232 0.7819 0.6296 0.079 Uiso 1 1 calc R . . H10C H 1.1630 0.7420 0.6811 0.079 Uiso 1 1 calc R . . C11 C 0.8694(10) 0.9243(4) 0.8251(5) 0.0177(12) Uani 1 1 d U . . H11A H 0.8687 0.9573 0.7914 0.021 Uiso 1 1 calc R . . H11B H 0.8686 0.9434 0.8699 0.021 Uiso 1 1 calc R . . C12 C 0.7375(8) 0.8589(5) 0.8745(5) 0.0129(14) Uani 1 1 d U . . C13 C 0.7804(8) 0.8849(5) 0.8164(5) 0.0150(14) Uani 1 1 d U . . C14 C 0.7413(8) 0.8732(5) 0.7550(6) 0.0186(17) Uani 1 1 d U . . H14 H 0.7685 0.8922 0.7169 0.022 Uiso 1 1 calc R . . C15 C 0.6624(8) 0.8344(5) 0.7454(5) 0.0221(17) Uani 1 1 d U . . C16 C 0.6233(10) 0.8091(4) 0.8036(4) 0.0177(17) Uani 1 1 d U . . H16 H 0.5704 0.7828 0.7988 0.021 Uiso 1 1 calc R . . C17 C 0.6566(7) 0.8201(5) 0.8669(5) 0.0153(13) Uani 1 1 d U . . C18 C 0.6222(12) 0.8240(5) 0.6756(5) 0.0317(19) Uani 1 1 d U . . C19 C 0.5872(11) 0.8842(7) 0.6454(7) 0.056(4) Uani 1 1 d U . . H19A H 0.5681 0.8776 0.5989 0.084 Uiso 1 1 calc R . . H19B H 0.6381 0.9145 0.6471 0.084 Uiso 1 1 calc R . . H19C H 0.5329 0.8991 0.6711 0.084 Uiso 1 1 calc R . . C20 C 0.6973(12) 0.7994(8) 0.6298(7) 0.061(4) Uani 1 1 d U . . H20A H 0.7213 0.7608 0.6477 0.091 Uiso 1 1 calc R . . H20B H 0.7493 0.8288 0.6267 0.091 Uiso 1 1 calc R . . H20C H 0.6703 0.7926 0.5853 0.091 Uiso 1 1 calc R . . C21 C 0.5394(11) 0.7806(6) 0.6749(7) 0.045(3) Uani 1 1 d U . . H21A H 0.5209 0.7721 0.6286 0.067 Uiso 1 1 calc R . . H21B H 0.4860 0.7990 0.6987 0.067 Uiso 1 1 calc R . . H21C H 0.5575 0.7425 0.6970 0.067 Uiso 1 1 calc R . . C22 C 0.6148(8) 0.7898(4) 0.9276(5) 0.0156(14) Uani 1 1 d U . . H22A H 0.5455 0.7862 0.9214 0.019 Uiso 1 1 calc R . . H22B H 0.6262 0.8159 0.9672 0.019 Uiso 1 1 calc R . . C23 C 0.7370(8) 0.7194(5) 0.9823(6) 0.0143(15) Uani 1 1 d U . . C24 C 0.6556(7) 0.7272(5) 0.9407(5) 0.0151(16) Uani 1 1 d U . . C25 C 0.6199(9) 0.6737(5) 0.9125(4) 0.0185(17) Uani 1 1 d U . . H25 H 0.5658 0.6774 0.8845 0.022 Uiso 1 1 calc R . . C26 C 0.6558(8) 0.6163(5) 0.9215(5) 0.0239(18) Uani 1 1 d U . . C27 C 0.7352(8) 0.6125(5) 0.9612(5) 0.0195(18) Uani 1 1 d U . . H27 H 0.7622 0.5734 0.9683 0.023 Uiso 1 1 calc R . . C28 C 0.7784(7) 0.6623(5) 0.9917(5) 0.0163(15) Uani 1 1 d U . . C29 C 0.6081(10) 0.5610(5) 0.8906(6) 0.036(2) Uani 1 1 d U . . C30 C 0.6508(12) 0.5012(6) 0.9121(8) 0.063(4) Uani 1 1 d U . . H30A H 0.7185 0.5011 0.9018 0.095 Uiso 1 1 calc R . . H30B H 0.6197 0.4678 0.8881 0.095 Uiso 1 1 calc R . . H30C H 0.6419 0.4959 0.9603 0.095 Uiso 1 1 calc R . . C31 C 0.6040(11) 0.5659(6) 0.8163(6) 0.050(3) Uani 1 1 d U . . H31A H 0.6679 0.5619 0.7980 0.075 Uiso 1 1 calc R . . H31B H 0.5776 0.6055 0.8037 0.075 Uiso 1 1 calc R . . H31C H 0.5637 0.5333 0.7985 0.075 Uiso 1 1 calc R . . C32 C 0.5046(10) 0.5582(7) 0.9133(8) 0.050(3) Uani 1 1 d U . . H32A H 0.4714 0.5263 0.8882 0.075 Uiso 1 1 calc R . . H32B H 0.4741 0.5976 0.9049 0.075 Uiso 1 1 calc R . . H32C H 0.5021 0.5489 0.9611 0.075 Uiso 1 1 calc R . . C33 C 0.8704(9) 0.6569(4) 1.0314(4) 0.0188(13) Uani 1 1 d U . . H33A H 0.8712 0.6885 1.0668 0.023 Uiso 1 1 calc R . . H33B H 0.8722 0.6166 1.0537 0.023 Uiso 1 1 calc R . . C34 C 1.0022(8) 0.7212(5) 0.9799(6) 0.0129(15) Uani 1 1 d U . . C35 C 0.9568(7) 0.6638(5) 0.9893(5) 0.0150(15) Uani 1 1 d U . . C36 C 0.9936(9) 0.6141(5) 0.9543(6) 0.0215(19) Uani 1 1 d U . . H36 H 0.9640 0.5754 0.9585 0.026 Uiso 1 1 calc R . . C37 C 1.0723(9) 0.6197(5) 0.9137(6) 0.0265(19) Uani 1 1 d U . . C38 C 1.1179(10) 0.6778(5) 0.9062(5) 0.0215(18) Uani 1 1 d U . . H38 H 1.1730 0.6819 0.8794 0.026 Uiso 1 1 calc R . . C39 C 1.0799(8) 0.7273(5) 0.9387(5) 0.0147(15) Uani 1 1 d U . . C40 C 1.1203(12) 0.5650(5) 0.8770(6) 0.044(2) Uani 1 1 d U . . C41 C 1.0617(13) 0.5061(6) 0.8881(9) 0.079(4) Uani 1 1 d U . . H41A H 1.0903 0.4724 0.8631 0.118 Uiso 1 1 calc R . . H41B H 0.9968 0.5126 0.8724 0.118 Uiso 1 1 calc R . . H41C H 1.0610 0.4960 0.9358 0.118 Uiso 1 1 calc R . . C42 C 1.2175(12) 0.5556(8) 0.9048(9) 0.067(4) Uani 1 1 d U . . H42A H 1.2556 0.5922 0.8971 0.101 Uiso 1 1 calc R . . H42B H 1.2472 0.5207 0.8826 0.101 Uiso 1 1 calc R . . H42C H 1.2134 0.5477 0.9529 0.101 Uiso 1 1 calc R . . C43 C 1.1151(14) 0.5758(6) 0.8025(6) 0.059(4) Uani 1 1 d U . . H43A H 1.1515 0.6123 0.7911 0.089 Uiso 1 1 calc R . . H43B H 1.0489 0.5816 0.7891 0.089 Uiso 1 1 calc R . . H43C H 1.1413 0.5405 0.7789 0.089 Uiso 1 1 calc R . . C44 C 1.1239(10) 0.7902(4) 0.9265(5) 0.0162(13) Uani 1 1 d U . . H44A H 1.1926 0.7853 0.9188 0.019 Uiso 1 1 calc R . . H44B H 1.1157 0.8155 0.9671 0.019 Uiso 1 1 calc R . . N1 N 0.8684(8) 0.8718(3) 1.0566(4) 0.0199(10) Uani 1 1 d U . . C45 C 0.8675(11) 0.8992(4) 1.1176(5) 0.0232(16) Uani 1 1 d U . . C46 C 0.8638(11) 0.8644(5) 1.1751(5) 0.0316(19) Uani 1 1 d U . . H46 H 0.8625 0.8212 1.1717 0.038 Uiso 1 1 calc R . . C47 C 0.8619(11) 0.8911(5) 1.2365(5) 0.036(2) Uani 1 1 d U . . H47 H 0.8613 0.8669 1.2758 0.043 Uiso 1 1 calc R . . C48 C 0.8609(12) 0.9550(5) 1.2408(6) 0.042(2) Uani 1 1 d U . . H48 H 0.8568 0.9740 1.2833 0.050 Uiso 1 1 calc R . . C49 C 0.8660(12) 0.9908(5) 1.1831(5) 0.036(2) Uani 1 1 d U . . H49 H 0.8689 1.0340 1.1867 0.043 Uiso 1 1 calc R . . C50 C 0.8666(11) 0.9640(5) 1.1222(5) 0.0309(16) Uani 1 1 d U . . C51 C 0.8773(11) 1.0028(5) 1.0595(5) 0.0338(19) Uani 1 1 d U . . H51A H 0.9305 0.9867 1.0327 0.041 Uiso 1 1 calc R . . H51B H 0.8935 1.0450 1.0728 0.041 Uiso 1 1 calc R . . C52 C 0.7881(9) 1.0042(5) 1.0159(7) 0.037(2) Uani 1 1 d U . . H52A H 0.7739 0.9622 1.0006 0.045 Uiso 1 1 calc R . . H52B H 0.7343 1.0182 1.0433 0.045 Uiso 1 1 calc R . . C53 C 0.7968(10) 1.0450(6) 0.9556(6) 0.0380(19) Uani 1 1 d U . . C54 C 0.8742(12) 1.0821(5) 0.9427(6) 0.039(2) Uani 1 1 d U . . H54 H 0.9254 1.0813 0.9735 0.046 Uiso 1 1 calc R . . C55 C 0.8815(12) 1.1195(6) 0.8886(6) 0.046(2) Uani 1 1 d U . . H55 H 0.9353 1.1449 0.8829 0.055 Uiso 1 1 calc R . . C56 C 0.8100(11) 1.1196(7) 0.8429(8) 0.055(3) Uani 1 1 d U . . H56 H 0.8154 1.1451 0.8048 0.066 Uiso 1 1 calc R . . C57 C 0.7279(11) 1.0835(6) 0.8500(8) 0.053(2) Uani 1 1 d U . . H57 H 0.6777 1.0850 0.8184 0.064 Uiso 1 1 calc R . . C58 C 0.7245(10) 1.0446(6) 0.9068(7) 0.043(2) Uani 1 1 d U . . N2 N 0.6390(10) 1.0085(5) 0.9191(5) 0.049(2) Uani 1 1 d U . . C59 C 0.6010(10) 0.9871(6) 0.8660(8) 0.058(3) Uani 1 1 d U . . H59 H 0.6269 0.9954 0.8232 0.070 Uiso 1 1 calc R . . C60 C 0.5168(12) 0.9498(7) 0.8734(9) 0.065(3) Uani 1 1 d U . . C61 C 0.4796(12) 0.9301(7) 0.9354(10) 0.069(3) Uani 1 1 d U . . H61 H 0.5097 0.9409 0.9762 0.083 Uiso 1 1 calc R . . C62 C 0.3994(12) 0.8951(7) 0.9352(10) 0.078(3) Uani 1 1 d U . . H62 H 0.3769 0.8773 0.9754 0.093 Uiso 1 1 calc R . . C63 C 0.3511(14) 0.8859(8) 0.8746(10) 0.086(3) Uani 1 1 d U . . H63 H 0.2910 0.8665 0.8738 0.103 Uiso 1 1 calc R . . C64 C 0.3930(14) 0.9058(8) 0.8164(11) 0.085(3) Uani 1 1 d U . . H64 H 0.3630 0.8958 0.7753 0.103 Uiso 1 1 calc R . . N3 N 0.4726(10) 0.9378(6) 0.8139(8) 0.077(3) Uani 1 1 d U . . N4 N 0.8692(7) 0.7663(3) 0.8898(3) 0.0125(13) Uani 1 1 d U . . C65 C 0.8720(11) 0.7388(5) 0.8430(5) 0.026(2) Uani 1 1 d U . . C66 C 0.8749(15) 0.7021(7) 0.7824(6) 0.079(5) Uani 1 1 d U . . H66A H 0.9407 0.6971 0.7681 0.119 Uiso 1 1 calc R . . H66B H 0.8388 0.7224 0.7470 0.119 Uiso 1 1 calc R . . H66C H 0.8473 0.6619 0.7913 0.119 Uiso 1 1 calc R . . N5 N 0.3676(17) 0.7261(8) 0.8618(8) 0.120(5) Uani 1 1 d DU . . C67 C 0.368(2) 0.7233(11) 0.9203(10) 0.119(6) Uani 1 1 d DU . . C68 C 0.366(2) 0.7288(11) 0.9934(9) 0.151(7) Uani 1 1 d DU . . H68A H 0.4115 0.7005 1.0133 0.227 Uiso 1 1 calc R . . H68B H 0.3021 0.7189 1.0094 0.227 Uiso 1 1 calc R . . H68C H 0.3817 0.7706 1.0063 0.227 Uiso 1 1 calc R . . N6 N 0.5273(15) 1.1614(9) 0.8727(15) 0.170(8) Uani 1 1 d DU . . C69 C 0.4576(17) 1.1333(11) 0.8800(17) 0.143(7) Uani 1 1 d DU . . C70 C 0.3739(16) 1.0991(9) 0.9014(12) 0.131(7) Uani 1 1 d DU . . H70A H 0.3364 1.0876 0.8621 0.196 Uiso 1 1 calc R . . H70B H 0.3355 1.1246 0.9310 0.196 Uiso 1 1 calc R . . H70C H 0.3938 1.0623 0.9253 0.196 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 0.0204(4) 0.0057(3) 0.0133(3) -0.0042(4) -0.0006(5) -0.0015(6) O1 0.020(2) 0.004(3) 0.0171(19) -0.0044(19) 0.0001(17) -0.0022(18) O2 0.020(2) 0.002(3) 0.022(2) -0.0017(19) -0.0019(17) -0.0026(17) O3 0.022(2) 0.0121(19) 0.013(3) 0.002(2) -0.001(2) -0.0029(17) O4 0.022(2) 0.0111(19) 0.014(3) -0.001(2) -0.003(2) -0.0009(16) C1 0.017(3) 0.003(4) 0.016(2) -0.004(2) -0.0010(17) -0.004(2) C2 0.014(2) 0.009(2) 0.0175(17) -0.0016(17) 0.0003(17) -0.0035(17) C3 0.021(4) 0.004(4) 0.021(2) 0.000(3) 0.007(3) -0.005(3) C4 0.030(4) 0.011(4) 0.0194(18) 0.002(3) 0.007(3) -0.004(3) C5 0.027(4) 0.010(5) 0.019(2) 0.005(4) 0.003(3) -0.005(3) C6 0.019(2) 0.003(4) 0.019(2) 0.000(3) -0.002(3) -0.005(2) C7 0.044(5) 0.029(4) 0.020(2) -0.001(4) 0.010(3) 0.000(4) C8 0.102(11) 0.043(5) 0.042(7) 0.000(6) 0.050(7) -0.018(6) C9 0.064(7) 0.106(11) 0.025(4) -0.018(8) -0.002(5) 0.009(7) C10 0.069(8) 0.057(7) 0.032(7) 0.005(6) 0.027(6) 0.026(6) C11 0.026(3) 0.002(4) 0.025(3) 0.003(2) -0.001(2) 0.0001(16) C12 0.013(3) 0.004(4) 0.022(2) -0.004(2) 0.0000(16) 0.006(2) C13 0.019(2) 0.003(4) 0.023(2) 0.001(3) -0.002(3) 0.005(2) C14 0.027(4) 0.006(4) 0.023(2) -0.002(3) -0.003(3) 0.007(3) C15 0.032(4) 0.013(4) 0.0218(18) -0.003(3) -0.008(3) 0.003(3) C16 0.024(4) 0.006(4) 0.023(2) -0.004(3) -0.007(3) 0.005(3) C17 0.015(2) 0.010(2) 0.0211(17) -0.0036(17) -0.0026(17) 0.0025(17) C18 0.047(5) 0.025(4) 0.023(2) -0.002(3) -0.013(3) -0.001(3) C19 0.077(10) 0.038(5) 0.054(7) 0.018(6) -0.039(7) -0.006(5) C20 0.073(7) 0.074(9) 0.035(5) -0.030(7) 0.002(6) -0.003(6) C21 0.067(7) 0.039(7) 0.028(7) -0.004(6) -0.021(5) -0.019(6) C22 0.008(4) 0.016(2) 0.023(2) -0.007(3) 0.002(3) 0.002(2) C23 0.018(3) 0.0102(19) 0.015(4) 0.004(3) 0.001(3) -0.0036(16) C24 0.015(4) 0.0141(19) 0.017(4) -0.002(2) 0.003(3) -0.001(2) C25 0.021(4) 0.013(2) 0.021(4) 0.004(3) -0.001(3) -0.008(3) C26 0.031(4) 0.014(2) 0.027(4) -0.002(3) -0.001(3) -0.003(3) C27 0.027(4) 0.010(2) 0.021(5) 0.002(3) 0.005(3) 0.000(3) C28 0.021(2) 0.010(2) 0.018(4) 0.007(3) 0.005(3) -0.003(3) C29 0.042(4) 0.013(2) 0.053(4) 0.000(4) -0.011(4) -0.008(4) C30 0.074(9) 0.013(2) 0.102(9) -0.002(5) -0.020(9) 0.003(6) C31 0.071(10) 0.029(7) 0.050(4) -0.026(4) -0.011(5) 0.001(7) C32 0.043(5) 0.029(8) 0.077(8) 0.001(7) -0.007(6) -0.018(4) C33 0.025(3) 0.012(3) 0.019(4) 0.012(2) 0.001(2) -0.001(2) C34 0.015(3) 0.0089(19) 0.015(4) 0.001(3) -0.004(3) -0.0012(15) C35 0.020(2) 0.009(2) 0.016(4) 0.004(3) -0.002(3) -0.001(3) C36 0.027(5) 0.006(3) 0.032(5) 0.005(3) 0.001(3) 0.004(3) C37 0.039(5) 0.008(2) 0.032(4) 0.001(3) 0.010(3) 0.005(3) C38 0.032(5) 0.012(3) 0.021(4) 0.004(3) 0.006(3) 0.003(3) C39 0.017(4) 0.011(2) 0.017(4) -0.001(2) -0.003(3) -0.003(2) C40 0.062(5) 0.014(3) 0.055(4) -0.003(4) 0.022(4) 0.013(4) C41 0.112(9) 0.014(4) 0.110(10) -0.023(6) 0.063(9) -0.003(6) C42 0.073(6) 0.046(9) 0.082(9) -0.005(8) 0.012(7) 0.042(5) C43 0.093(10) 0.035(7) 0.049(4) -0.020(4) 0.018(6) 0.015(8) C44 0.012(3) 0.014(2) 0.022(2) 0.000(3) -0.006(3) -0.006(3) N1 0.027(4) 0.016(3) 0.0172(14) -0.0102(17) 0.0016(16) -0.002(2) C45 0.036(4) 0.015(2) 0.0184(14) -0.0113(13) -0.001(5) -0.008(5) C46 0.049(5) 0.028(3) 0.0186(17) -0.006(2) 0.003(6) -0.004(6) C47 0.054(6) 0.034(3) 0.0187(15) -0.008(3) -0.003(6) 0.002(6) C48 0.056(6) 0.035(4) 0.034(3) -0.017(3) -0.003(6) -0.002(6) C49 0.050(5) 0.018(3) 0.039(3) -0.0202(19) 0.004(6) -0.004(6) C50 0.043(5) 0.015(2) 0.035(2) -0.0156(14) 0.007(4) -0.011(5) C51 0.053(5) 0.008(3) 0.040(3) -0.012(3) 0.000(4) -0.008(5) C52 0.051(5) 0.016(5) 0.045(4) -0.013(3) 0.001(4) -0.005(4) C53 0.049(4) 0.020(5) 0.045(4) -0.011(3) 0.000(3) 0.000(4) C54 0.048(5) 0.023(5) 0.045(5) -0.006(3) 0.001(4) 0.001(4) C55 0.054(6) 0.030(5) 0.055(6) 0.003(4) 0.002(5) 0.005(5) C56 0.064(6) 0.040(6) 0.060(6) 0.010(5) -0.006(5) 0.005(5) C57 0.062(6) 0.038(6) 0.059(5) -0.001(4) -0.011(4) 0.006(4) C58 0.047(4) 0.027(5) 0.054(5) -0.009(3) -0.003(3) 0.005(3) N2 0.045(4) 0.030(5) 0.073(5) -0.014(4) -0.003(4) 0.005(4) C59 0.056(6) 0.037(6) 0.081(5) -0.016(5) -0.012(5) -0.001(4) C60 0.061(6) 0.041(6) 0.093(5) -0.013(5) -0.015(4) -0.007(4) C61 0.068(7) 0.037(6) 0.102(5) -0.008(6) -0.008(5) -0.008(5) C62 0.076(7) 0.046(6) 0.111(6) -0.014(6) -0.006(6) -0.017(5) C63 0.082(8) 0.055(7) 0.120(7) -0.013(7) -0.017(6) -0.019(6) C64 0.081(7) 0.064(7) 0.111(6) -0.016(7) -0.024(6) -0.024(5) N3 0.073(6) 0.057(6) 0.102(5) -0.015(6) -0.024(5) -0.016(5) N4 0.017(4) 0.007(3) 0.013(2) -0.0041(18) -0.002(3) -0.002(3) C65 0.035(5) 0.021(5) 0.022(4) -0.015(3) -0.004(6) 0.007(6) C66 0.108(11) 0.076(9) 0.054(7) -0.058(6) -0.014(10) 0.006(11) N5 0.112(10) 0.130(12) 0.117(9) -0.028(12) -0.020(15) 0.056(12) C67 0.111(11) 0.128(12) 0.119(9) -0.010(11) -0.030(16) 0.040(12) C68 0.148(14) 0.192(16) 0.115(9) 0.019(14) -0.024(17) 0.011(16) N6 0.132(13) 0.089(14) 0.290(19) 0.047(14) 0.050(16) 0.008(11) C69 0.095(13) 0.088(14) 0.246(17) 0.029(13) 0.032(14) 0.031(10) C70 0.069(11) 0.109(14) 0.215(17) -0.011(13) 0.027(16) 0.031(11) _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 1.738(7) . ? Mo1 O4 1.929(7) . ? Mo1 O1 1.931(7) . ? Mo1 O2 1.940(7) . ? Mo1 O3 1.942(7) . ? Mo1 N4 2.324(7) . ? O1 C1 1.380(12) . ? O2 C12 1.337(12) . ? O3 C23 1.383(12) . ? O4 C34 1.391(12) . ? C1 C2 1.380(14) . ? C1 C6 1.395(15) . ? C2 C3 1.394(13) . ? C2 C44 1.537(14) . ? C3 C4 1.390(14) . ? C4 C5 1.389(16) . ? C4 C7 1.506(15) . ? C5 C6 1.391(15) . ? C6 C11 1.497(16) . ? C7 C10 1.507(19) . ? C7 C9 1.508(18) . ? C7 C8 1.571(18) . ? C11 C13 1.535(16) . ? C12 C13 1.431(15) . ? C12 C17 1.433(14) . ? C13 C14 1.371(15) . ? C14 C15 1.417(16) . ? C15 C16 1.403(14) . ? C15 C18 1.525(14) . ? C16 C17 1.373(13) . ? C17 C22 1.507(14) . ? C18 C20 1.504(18) . ? C18 C21 1.510(19) . ? C18 C19 1.534(17) . ? C22 C24 1.512(14) . ? C23 C28 1.397(14) . ? C23 C24 1.429(15) . ? C24 C25 1.397(14) . ? C25 C26 1.369(15) . ? C26 C27 1.377(15) . ? C26 C29 1.519(16) . ? C27 C28 1.392(15) . ? C28 C33 1.527(15) . ? C29 C31 1.491(16) . ? C29 C30 1.506(17) . ? C29 C32 1.536(18) . ? C33 C35 1.494(15) . ? C34 C39 1.382(15) . ? C34 C35 1.427(14) . ? C35 C36 1.397(15) . ? C36 C37 1.385(16) . ? C37 C38 1.436(16) . ? C37 C40 1.563(16) . ? C38 C39 1.376(15) . ? C39 C44 1.533(14) . ? C40 C42 1.50(2) . ? C40 C43 1.511(17) . ? C40 C41 1.55(2) . ? N1 C45 1.361(11) . ? C45 C46 1.381(13) . ? C45 C50 1.425(13) . ? C46 C47 1.362(13) . ? C47 C48 1.405(15) . ? C48 C49 1.399(15) . ? C49 C50 1.354(13) . ? C50 C51 1.524(14) . ? C51 C52 1.532(19) . ? C52 C53 1.506(17) . ? C53 C54 1.390(19) . ? C53 C58 1.412(18) . ? C54 C55 1.362(16) . ? C55 C56 1.362(19) . ? C56 C57 1.41(2) . ? C57 C58 1.423(19) . ? C58 N2 1.465(18) . ? N2 C59 1.279(16) . ? C59 C60 1.45(2) . ? C60 N3 1.37(2) . ? C60 C61 1.42(2) . ? C61 C62 1.37(2) . ? C62 C63 1.40(2) . ? C63 C64 1.38(2) . ? C64 N3 1.33(2) . ? N4 C65 1.116(11) . ? C65 C66 1.456(14) . ? N5 C67 1.171(18) . ? C67 C68 1.47(2) . ? N6 C69 1.173(18) . ? C69 C70 1.47(2) . ? 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 O4 96.7(4) . . ? N1 Mo1 O1 98.6(4) . . ? O4 Mo1 O1 89.8(3) . . ? N1 Mo1 O2 97.9(4) . . ? O4 Mo1 O2 165.4(3) . . ? O1 Mo1 O2 89.0(2) . . ? N1 Mo1 O3 95.9(4) . . ? O4 Mo1 O3 89.4(2) . . ? O1 Mo1 O3 165.5(3) . . ? O2 Mo1 O3 88.1(3) . . ? N1 Mo1 N4 178.9(4) . . ? O4 Mo1 N4 83.4(3) . . ? O1 Mo1 N4 82.6(3) . . ? O2 Mo1 N4 82.0(3) . . ? O3 Mo1 N4 82.9(3) . . ? C1 O1 Mo1 130.1(6) . . ? C12 O2 Mo1 129.4(7) . . ? C23 O3 Mo1 129.7(7) . . ? C34 O4 Mo1 127.5(7) . . ? O1 C1 C2 119.7(9) . . ? O1 C1 C6 118.2(9) . . ? C2 C1 C6 122.1(10) . . ? C1 C2 C3 118.2(10) . . ? C1 C2 C44 122.3(9) . . ? C3 C2 C44 119.4(9) . . ? C4 C3 C2 123.0(10) . . ? C5 C4 C3 115.7(10) . . ? C5 C4 C7 121.6(11) . . ? C3 C4 C7 122.7(10) . . ? C4 C5 C6 124.4(11) . . ? C5 C6 C1 116.6(10) . . ? C5 C6 C11 122.2(10) . . ? C1 C6 C11 121.0(9) . . ? C4 C7 C10 114.3(10) . . ? C4 C7 C9 112.3(12) . . ? C10 C7 C9 110.9(11) . . ? C4 C7 C8 107.0(9) . . ? C10 C7 C8 106.4(13) . . ? C9 C7 C8 105.4(11) . . ? C6 C11 C13 112.2(7) . . ? O2 C12 C13 120.7(10) . . ? O2 C12 C17 119.8(10) . . ? C13 C12 C17 119.5(10) . . ? C14 C13 C12 118.8(11) . . ? C14 C13 C11 122.3(10) . . ? C12 C13 C11 118.9(9) . . ? C13 C14 C15 123.3(11) . . ? C16 C15 C14 116.0(10) . . ? C16 C15 C18 123.6(11) . . ? C14 C15 C18 120.3(11) . . ? C17 C16 C15 124.1(12) . . ? C16 C17 C12 118.3(10) . . ? C16 C17 C22 122.1(10) . . ? C12 C17 C22 119.5(9) . . ? C20 C18 C21 108.5(11) . . ? C20 C18 C15 110.4(12) . . ? C21 C18 C15 113.0(10) . . ? C20 C18 C19 107.4(12) . . ? C21 C18 C19 106.9(12) . . ? C15 C18 C19 110.6(10) . . ? C17 C22 C24 112.9(9) . . ? O3 C23 C28 120.4(9) . . ? O3 C23 C24 118.0(9) . . ? C28 C23 C24 121.6(10) . . ? C25 C24 C23 115.1(10) . . ? C25 C24 C22 123.8(10) . . ? C23 C24 C22 121.0(10) . . ? C26 C25 C24 125.9(11) . . ? C25 C26 C27 115.7(11) . . ? C25 C26 C29 121.2(11) . . ? C27 C26 C29 123.2(11) . . ? C26 C27 C28 124.2(11) . . ? C27 C28 C23 117.5(10) . . ? C27 C28 C33 122.6(10) . . ? C23 C28 C33 119.8(9) . . ? C31 C29 C30 111.2(12) . . ? C31 C29 C26 111.4(10) . . ? C30 C29 C26 113.8(11) . . ? C31 C29 C32 105.2(12) . . ? C30 C29 C32 105.2(11) . . ? C26 C29 C32 109.6(10) . . ? C35 C33 C28 113.3(7) . . ? C39 C34 O4 121.2(9) . . ? C39 C34 C35 121.5(10) . . ? O4 C34 C35 117.3(9) . . ? C36 C35 C34 117.1(10) . . ? C36 C35 C33 120.6(9) . . ? C34 C35 C33 122.2(9) . . ? C37 C36 C35 121.7(11) . . ? C36 C37 C38 120.1(11) . . ? C36 C37 C40 123.9(11) . . ? C38 C37 C40 115.9(11) . . ? C39 C38 C37 118.4(11) . . ? C38 C39 C34 121.1(11) . . ? C38 C39 C44 118.5(10) . . ? C34 C39 C44 120.4(10) . . ? C42 C40 C43 115.6(15) . . ? C42 C40 C41 108.8(12) . . ? C43 C40 C41 104.3(13) . . ? C42 C40 C37 109.3(12) . . ? C43 C40 C37 108.8(11) . . ? C41 C40 C37 109.9(12) . . ? C39 C44 C2 112.9(9) . . ? C45 N1 Mo1 171.9(7) . . ? N1 C45 C46 120.2(9) . . ? N1 C45 C50 119.9(9) . . ? C46 C45 C50 119.9(9) . . ? C47 C46 C45 120.9(10) . . ? C46 C47 C48 119.0(10) . . ? C49 C48 C47 120.7(10) . . ? C50 C49 C48 119.9(10) . . ? C49 C50 C45 119.4(10) . . ? C49 C50 C51 120.0(9) . . ? C45 C50 C51 120.3(8) . . ? C50 C51 C52 113.3(12) . . ? C53 C52 C51 113.5(11) . . ? C54 C53 C58 116.4(13) . . ? C54 C53 C52 124.3(13) . . ? C58 C53 C52 119.3(12) . . ? C55 C54 C53 124.3(16) . . ? C54 C55 C56 118.4(16) . . ? C55 C56 C57 122.8(14) . . ? C56 C57 C58 116.5(15) . . ? C53 C58 C57 121.5(14) . . ? C53 C58 N2 118.9(13) . . ? C57 C58 N2 119.2(13) . . ? C59 N2 C58 113.8(12) . . ? N2 C59 C60 117.8(16) . . ? N3 C60 C61 122.2(16) . . ? N3 C60 C59 113.1(17) . . ? C61 C60 C59 124.6(16) . . ? C62 C61 C60 118.6(18) . . ? C61 C62 C63 119.0(19) . . ? C64 C63 C62 118.3(18) . . ? N3 C64 C63 124.4(19) . . ? C64 N3 C60 117.1(17) . . ? C65 N4 Mo1 176.8(11) . . ? N4 C65 C66 179.1(16) . . ? N5 C67 C68 172(3) . . ? N6 C69 C70 170(4) . . ? _diffrn_measured_fraction_theta_max 0.997 _diffrn_reflns_theta_full 24.00 _diffrn_measured_fraction_theta_full 0.997 _refine_diff_density_max 2.533 _refine_diff_density_min -1.304 _refine_diff_density_rms 0.148 #===END data_2 _database_code_CSD 173185 _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_formula_moiety ? _chemical_formula_sum 'C128 H150 Mo2 N10 O8' _chemical_formula_weight 2148.46 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 trigonal _symmetry_space_group_name_H-M P32 loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-y, x-y, z+2/3' '-x+y, -x, z+1/3' _cell_length_a 16.7686(15) _cell_length_b 16.7686(15) _cell_length_c 34.515(3) _cell_angle_alpha 90.00 _cell_angle_beta 90.00 _cell_angle_gamma 120.00 _cell_volume 8404.9(13) _cell_formula_units_Z 3 _cell_measurement_temperature 160(2) _cell_measurement_reflns_used 16261 _cell_measurement_theta_min 1.77 _cell_measurement_theta_max 28.42 _exptl_crystal_description block _exptl_crystal_colour 'dark brown' _exptl_crystal_size_max 0.35 _exptl_crystal_size_mid 0.18 _exptl_crystal_size_min 0.13 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.273 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 3408 _exptl_absorpt_coefficient_mu 0.286 _exptl_absorpt_correction_type empirical _exptl_absorpt_correction_T_min 0.790 _exptl_absorpt_correction_T_max 0.928 _exptl_special_details ; ? ; _diffrn_ambient_temperature 160(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'Bruker SMART CCD diffractometer' _diffrn_measurement_method '\w rotation with narrow frames' _diffrn_detector_area_resol_mean ? _diffrn_standards_number 0 _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% 0 _diffrn_reflns_number 44602 _diffrn_reflns_av_R_equivalents 0.0930 _diffrn_reflns_av_sigmaI/netI 0.1544 _diffrn_reflns_limit_h_min -16 _diffrn_reflns_limit_h_max 19 _diffrn_reflns_limit_k_min -19 _diffrn_reflns_limit_k_max 15 _diffrn_reflns_limit_l_min -41 _diffrn_reflns_limit_l_max 41 _diffrn_reflns_theta_min 1.77 _diffrn_reflns_theta_max 25.00 _reflns_number_total 19554 _reflns_number_gt 13334 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'Bruker SMART' _computing_cell_refinement 'local programs' _computing_data_reduction 'Bruker SAINT' _computing_structure_solution 'Bruker SHELXTL' _computing_structure_refinement 'Bruker SHELXTL' _computing_molecular_graphics 'Bruker SHELXTL' _computing_publication_material 'SHELXTL and local programs' _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 w=1/[\s^2^(Fo^2^)+(0.0536P)^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 except H2A&B coords freely refined' _refine_ls_hydrogen_treatment mixed _refine_ls_extinction_method SHELXL _refine_ls_extinction_coef 0.00122(15) _refine_ls_extinction_expression 'Fc^*^=kFc[1+0.001xFc^2^\l^3^/sin(2\q)]^-1/4^' _refine_ls_abs_structure_details 'Flack H D (1983), Acta Cryst. A39, 876-881' _refine_ls_abs_structure_Flack -0.01(3) _refine_ls_number_reflns 19554 _refine_ls_number_parameters 1418 _refine_ls_number_restraints 353 _refine_ls_R_factor_all 0.1203 _refine_ls_R_factor_gt 0.0718 _refine_ls_wR_factor_ref 0.1429 _refine_ls_wR_factor_gt 0.1227 _refine_ls_goodness_of_fit_ref 1.026 _refine_ls_restrained_S_all 1.028 _refine_ls_shift/su_max 0.008 _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_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group Mo1 Mo 0.81994(4) 0.12487(4) 0.166749(17) 0.01979(16) Uani 1 d . . . Mo2 Mo 0.60594(4) 0.04920(4) 0.122759(18) 0.01942(16) Uani 1 d . . . N1 N 0.9270(4) 0.2218(4) 0.15932(16) 0.0197(14) Uani 1 d . . . C1 C 1.0132(5) 0.2988(5) 0.1547(2) 0.0199(17) Uani 1 d . . . C2 C 1.0490(6) 0.3601(6) 0.1859(3) 0.036(2) Uani 1 d . . . H2 H 1.0137 0.3478 0.2089 0.044 Uiso 1 calc R . . C3 C 1.1342(6) 0.4376(6) 0.1838(3) 0.046(2) Uani 1 d . . . H3 H 1.1583 0.4798 0.2048 0.055 Uiso 1 calc R . . C4 C 1.1841(6) 0.4522(6) 0.1496(3) 0.043(2) Uani 1 d . . . H4 H 1.2435 0.5052 0.1476 0.051 Uiso 1 calc R . . C5 C 1.1507(6) 0.3929(6) 0.1189(3) 0.043(2) Uani 1 d . . . H5 H 1.1862 0.4060 0.0959 0.052 Uiso 1 calc R . . C6 C 1.0640(5) 0.3125(5) 0.1212(2) 0.0270(19) Uani 1 d . . . C7 C 1.0326(5) 0.2468(5) 0.0872(2) 0.030(2) Uani 1 d . . . H7A H 1.0348 0.2805 0.0633 0.036 Uiso 1 calc R . . H7B H 0.9680 0.1977 0.0914 0.036 Uiso 1 calc R . . C8 C 1.0936(5) 0.2024(6) 0.0818(2) 0.034(2) Uani 1 d . . . H8A H 1.1589 0.2510 0.0846 0.041 Uiso 1 calc R . . H8B H 1.0794 0.1572 0.1029 0.041 Uiso 1 calc R . . C9 C 1.0823(6) 0.1547(6) 0.0438(2) 0.035(2) Uani 1 d . . . C10 C 1.1540(7) 0.1942(7) 0.0164(2) 0.045(2) Uani 1 d . . . H10 H 1.2081 0.2505 0.0225 0.055 Uiso 1 calc R . . C11 C 1.1481(7) 0.1542(7) -0.0183(3) 0.053(3) Uani 1 d . . . H11 H 1.1982 0.1813 -0.0360 0.063 Uiso 1 calc R . . C12 C 1.0678(7) 0.0728(7) -0.0279(3) 0.050(3) Uani 1 d . . . H12 H 1.0631 0.0452 -0.0524 0.060 Uiso 1 calc R . . C13 C 0.9945(6) 0.0313(6) -0.0020(3) 0.044(2) Uani 1 d . . . H13 H 0.9397 -0.0237 -0.0089 0.052 Uiso 1 calc R . . C14 C 1.0028(6) 0.0721(6) 0.0342(2) 0.038(2) Uani 1 d . . . N2 N 0.9335(5) 0.0268(6) 0.0607(2) 0.050(2) Uani 1 d D . . H2A H 0.933(6) 0.058(6) 0.086(2) 0.060 Uiso 1 d D . . H2B H 0.897(5) -0.025(5) 0.042(2) 0.060 Uiso 1 d D . . N3 N 0.5044(4) -0.0546(4) 0.12630(17) 0.0258(16) Uani 1 d . . . C15 C 0.4222(5) -0.1386(5) 0.1301(2) 0.0264(19) Uani 1 d . . . C16 C 0.3528(5) -0.1363(5) 0.1523(2) 0.0287(19) Uani 1 d . . . H16 H 0.3634 -0.0801 0.1636 0.034 Uiso 1 calc R . . C17 C 0.2696(6) -0.2161(6) 0.1577(3) 0.042(2) Uani 1 d . . . H17 H 0.2229 -0.2162 0.1733 0.051 Uiso 1 calc R . . C18 C 0.2558(5) -0.2947(6) 0.1401(2) 0.040(2) Uani 1 d . . . H18 H 0.1979 -0.3493 0.1431 0.048 Uiso 1 calc R . . C19 C 0.3234(5) -0.2981(6) 0.1178(2) 0.038(2) Uani 1 d . . . H19 H 0.3117 -0.3549 0.1068 0.046 Uiso 1 calc R . . C20 C 0.4072(6) -0.2196(5) 0.1117(2) 0.030(2) Uani 1 d . . . C21 C 0.4810(6) -0.2218(6) 0.0881(3) 0.050(3) Uani 1 d . . . H21A H 0.5302 -0.1569 0.0849 0.060 Uiso 1 calc R . . H21B H 0.5071 -0.2515 0.1046 0.060 Uiso 1 calc R . . C22 C 0.4677(8) -0.2609(10) 0.0532(5) 0.167(9) Uani 1 d . . . H22A H 0.5261 -0.2583 0.0461 0.200 Uiso 1 calc R . . H22B H 0.4600 -0.2197 0.0349 0.200 Uiso 1 calc R . . C23 C 0.3907(9) -0.3588(11) 0.0439(4) 0.095(5) Uani 1 d . . . C24 C 0.3167(10) -0.3679(10) 0.0248(4) 0.098(5) Uani 1 d . . . H24 H 0.3128 -0.3144 0.0194 0.117 Uiso 1 calc R . . C25 C 0.2457(9) -0.4533(10) 0.0127(3) 0.083(4) Uani 1 d . . . H25 H 0.1948 -0.4583 -0.0015 0.100 Uiso 1 calc R . . C26 C 0.2512(9) -0.5293(9) 0.0217(3) 0.081(4) Uani 1 d . . . H26 H 0.2033 -0.5880 0.0136 0.097 Uiso 1 calc R . . C27 C 0.3227(8) -0.5242(9) 0.0419(3) 0.075(4) Uani 1 d . . . H27 H 0.3225 -0.5791 0.0490 0.089 Uiso 1 calc R . . C28 C 0.3953(8) -0.4406(11) 0.0523(3) 0.084(4) Uani 1 d . . . N4 N 0.4718(8) -0.4366(10) 0.0720(3) 0.137(5) Uani 1 d . . . O1 O 0.7539(3) 0.1620(3) 0.12563(12) 0.0171(11) Uani 1 d . . . O2 O 0.7738(3) 0.1747(3) 0.20519(13) 0.0217(12) Uani 1 d . . . O3 O 0.8542(3) 0.0777(3) 0.21120(14) 0.0230(12) Uani 1 d . . . O4 O 0.8445(3) 0.0389(3) 0.13774(14) 0.0230(12) Uani 1 d . . . O5 O 0.6759(3) 0.0111(3) 0.16072(13) 0.0191(11) Uani 1 d . . . O6 O 0.5894(3) 0.1114(3) 0.16679(13) 0.0217(12) Uani 1 d . . . O7 O 0.5556(3) 0.1119(3) 0.09295(13) 0.0200(11) Uani 1 d . . . O8 O 0.6430(3) 0.0300(3) 0.07144(12) 0.0199(11) Uani 1 d . . . C29 C 0.8002(5) 0.2483(4) 0.1085(2) 0.0159(16) Uani 1 d . . . C30 C 0.8370(5) 0.2576(5) 0.0722(2) 0.0214(18) Uani 1 d . . . C31 C 0.8884(5) 0.3454(5) 0.0556(2) 0.0232(17) Uani 1 d . . . H31 H 0.9132 0.3510 0.0304 0.028 Uiso 1 calc R . . C32 C 0.9040(5) 0.4240(5) 0.0750(2) 0.0294(19) Uani 1 d . . . C33 C 0.8637(5) 0.4121(5) 0.1113(2) 0.0267(19) Uani 1 d . . . H33 H 0.8724 0.4650 0.1250 0.032 Uiso 1 calc R . . C34 C 0.8112(5) 0.3261(5) 0.1285(2) 0.0208(17) Uani 1 d . . . C35 C 0.9633(6) 0.5201(5) 0.0577(3) 0.041(2) Uani 1 d . . . C36 C 1.0484(7) 0.5730(7) 0.0814(3) 0.084(4) Uani 1 d . . . H36A H 1.0315 0.5750 0.1084 0.126 Uiso 1 calc R . . H36B H 1.0841 0.6359 0.0713 0.126 Uiso 1 calc R . . H36C H 1.0856 0.5430 0.0800 0.126 Uiso 1 calc R . . C37 C 0.9079(8) 0.5705(7) 0.0581(3) 0.082(4) Uani 1 d . . . H37A H 0.8910 0.5754 0.0848 0.123 Uiso 1 calc R . . H37B H 0.8519 0.5358 0.0425 0.123 Uiso 1 calc R . . H37C H 0.9454 0.6322 0.0471 0.123 Uiso 1 calc R . . C38 C 0.9907(8) 0.5178(6) 0.0165(3) 0.071(4) Uani 1 d . . . H38A H 1.0253 0.5807 0.0064 0.107 Uiso 1 calc R . . H38B H 0.9354 0.4819 0.0007 0.107 Uiso 1 calc R . . H38C H 1.0293 0.4892 0.0155 0.107 Uiso 1 calc R . . C39 C 0.7677(5) 0.3206(5) 0.1675(2) 0.0249(18) Uani 1 d . . . H39A H 0.7117 0.2591 0.1696 0.030 Uiso 1 calc R . . H39B H 0.7474 0.3668 0.1678 0.030 Uiso 1 calc R . . C40 C 0.8205(5) 0.2597(5) 0.2219(2) 0.0214(17) Uani 1 d . . . C41 C 0.8269(5) 0.3355(5) 0.2036(2) 0.0231(18) Uani 1 d . . . C42 C 0.8822(5) 0.4211(6) 0.2184(2) 0.0281(19) Uani 1 d . . . H42 H 0.8857 0.4728 0.2054 0.034 Uiso 1 calc R . . C43 C 0.9353(6) 0.4355(5) 0.2528(2) 0.032(2) Uani 1 d . . . C44 C 0.9235(5) 0.3576(5) 0.2723(2) 0.031(2) Uani 1 d . . . H44 H 0.9552 0.3646 0.2960 0.037 Uiso 1 calc R . . C45 C 0.8649(5) 0.2684(5) 0.2574(2) 0.0272(19) Uani 1 d . . . C46 C 1.0062(7) 0.5341(6) 0.2670(3) 0.052(3) Uani 1 d . . . C47 C 1.0564(8) 0.5968(7) 0.2333(4) 0.084(4) Uani 1 d . . . H47A H 1.1067 0.6553 0.2430 0.127 Uiso 1 calc R . . H47B H 1.0134 0.6082 0.2183 0.127 Uiso 1 calc R . . H47C H 1.0815 0.5674 0.2166 0.127 Uiso 1 calc R . . C48 C 0.9518(8) 0.5697(8) 0.2890(4) 0.106(5) Uani 1 d . . . H48A H 0.9250 0.5323 0.3123 0.160 Uiso 1 calc R . . H48B H 0.9025 0.5657 0.2725 0.160 Uiso 1 calc R . . H48C H 0.9929 0.6340 0.2965 0.160 Uiso 1 calc R . . C49 C 1.0794(7) 0.5311(7) 0.2916(3) 0.072(4) Uani 1 d . . . H49A H 1.0532 0.5034 0.3167 0.108 Uiso 1 calc R . . H49B H 1.1308 0.5939 0.2955 0.108 Uiso 1 calc R . . H49C H 1.1017 0.4942 0.2784 0.108 Uiso 1 calc R . . C50 C 0.8606(5) 0.1837(6) 0.2764(2) 0.031(2) Uani 1 d . . . H50A H 0.8621 0.1904 0.3050 0.037 Uiso 1 calc R . . H50B H 0.8020 0.1280 0.2693 0.037 Uiso 1 calc R . . C51 C 0.9365(5) 0.1252(5) 0.2312(2) 0.0267(19) Uani 1 d . . . C52 C 0.9405(5) 0.1727(5) 0.2636(2) 0.0274(18) Uani 1 d . . . C53 C 1.0251(5) 0.2229(5) 0.2820(2) 0.0271(19) Uani 1 d . . . H53 H 1.0282 0.2563 0.3048 0.032 Uiso 1 calc R . . C54 C 1.1064(5) 0.2267(5) 0.2689(2) 0.0319(19) Uani 1 d . . . C55 C 1.0975(5) 0.1770(5) 0.2359(2) 0.030(2) Uani 1 d . . . H55 H 1.1511 0.1784 0.2260 0.036 Uiso 1 calc R . . C56 C 1.0142(5) 0.1240(5) 0.2157(2) 0.0270(19) Uani 1 d . . . C57 C 1.1997(6) 0.2890(6) 0.2883(2) 0.038(2) Uani 1 d . . . C58 C 1.2202(7) 0.3862(7) 0.2871(4) 0.096(5) Uani 1 d . . . H58A H 1.2841 0.4272 0.2952 0.144 Uiso 1 calc R . . H58B H 1.1786 0.3937 0.3048 0.144 Uiso 1 calc R . . H58C H 1.2114 0.4018 0.2607 0.144 Uiso 1 calc R . . C59 C 1.2773(7) 0.2863(9) 0.2701(4) 0.102(5) Uani 1 d . . . H59A H 1.2770 0.2966 0.2422 0.153 Uiso 1 calc R . . H59B H 1.2717 0.2261 0.2747 0.153 Uiso 1 calc R . . H59C H 1.3352 0.3346 0.2813 0.153 Uiso 1 calc R . . C60 C 1.1940(7) 0.2653(8) 0.3312(3) 0.080(4) Uani 1 d . . . H60A H 1.1853 0.2033 0.3342 0.119 Uiso 1 calc R . . H60B H 1.1419 0.2674 0.3430 0.119 Uiso 1 calc R . . H60C H 1.2512 0.3099 0.3442 0.119 Uiso 1 calc R . . C61 C 1.0109(5) 0.0809(5) 0.1777(2) 0.0265(19) Uani 1 d . . . H61A H 1.0699 0.0815 0.1743 0.032 Uiso 1 calc R . . H61B H 1.0082 0.1210 0.1572 0.032 Uiso 1 calc R . . C62 C 0.8536(5) -0.0325(5) 0.1514(2) 0.0227(18) Uani 1 d . . . C63 C 0.9344(5) -0.0153(5) 0.1702(2) 0.0276(19) Uani 1 d . . . C64 C 0.9421(5) -0.0908(6) 0.1822(2) 0.033(2) Uani 1 d . . . H64 H 0.9970 -0.0791 0.1951 0.040 Uiso 1 calc R . . C65 C 0.8744(6) -0.1817(6) 0.1764(2) 0.032(2) Uani 1 d . . . C66 C 0.7949(6) -0.1941(5) 0.1588(2) 0.032(2) Uani 1 d . . . H66 H 0.7461 -0.2554 0.1549 0.038 Uiso 1 calc R . . C67 C 0.7816(5) -0.1231(5) 0.1465(2) 0.0256(18) Uani 1 d . . . C68 C 0.8853(6) -0.2625(6) 0.1892(3) 0.0531(19) Uani 1 d DU . . C69 C 0.8638(11) -0.3287(9) 0.1571(4) 0.061(3) Uani 0.705(8) d PDU A 1 H69A H 0.8720 -0.3797 0.1660 0.091 Uiso 0.705(8) calc PR A 1 H69B H 0.9052 -0.2976 0.1353 0.091 Uiso 0.705(8) calc PR A 1 H69C H 0.7999 -0.3527 0.1489 0.091 Uiso 0.705(8) calc PR A 1 C70 C 0.9822(8) -0.2299(8) 0.2059(4) 0.053(3) Uani 0.705(8) d PDU A 1 H70A H 0.9946 -0.1857 0.2269 0.080 Uiso 0.705(8) calc PR A 1 H70B H 1.0283 -0.2003 0.1854 0.080 Uiso 0.705(8) calc PR A 1 H70C H 0.9851 -0.2829 0.2161 0.080 Uiso 0.705(8) calc PR A 1 C71 C 0.8173(9) -0.3090(9) 0.2236(4) 0.060(3) Uani 0.705(8) d PDU A 1 H71A H 0.8331 -0.2644 0.2447 0.090 Uiso 0.705(8) calc PR A 1 H71B H 0.8219 -0.3618 0.2329 0.090 Uiso 0.705(8) calc PR A 1 H71C H 0.7542 -0.3301 0.2149 0.090 Uiso 0.705(8) calc PR A 1 C69A C 0.8013(15) -0.3584(13) 0.1799(9) 0.058(4) Uani 0.295(8) d PDU A 2 H69D H 0.7816 -0.3592 0.1531 0.086 Uiso 0.295(8) calc PR A 2 H69E H 0.7506 -0.3706 0.1975 0.086 Uiso 0.295(8) calc PR A 2 H69F H 0.8185 -0.4059 0.1832 0.086 Uiso 0.295(8) calc PR A 2 C70A C 0.9599(17) -0.2639(19) 0.1627(7) 0.054(3) Uani 0.295(8) d PDU A 2 H70D H 0.9425 -0.2656 0.1355 0.081 Uiso 0.295(8) calc PR A 2 H70E H 0.9646 -0.3186 0.1686 0.081 Uiso 0.295(8) calc PR A 2 H70F H 1.0194 -0.2084 0.1674 0.081 Uiso 0.295(8) calc PR A 2 C71A C 0.914(2) -0.258(2) 0.2308(5) 0.060(4) Uani 0.295(8) d PDU A 2 H71D H 0.9201 -0.3121 0.2367 0.090 Uiso 0.295(8) calc PR A 2 H71E H 0.8675 -0.2577 0.2478 0.090 Uiso 0.295(8) calc PR A 2 H71F H 0.9734 -0.2020 0.2350 0.090 Uiso 0.295(8) calc PR A 2 C72 C 0.6886(5) -0.1415(5) 0.1320(2) 0.030(2) Uani 1 d . . . H72A H 0.6973 -0.0907 0.1147 0.036 Uiso 1 calc R . . H72B H 0.6594 -0.1993 0.1168 0.036 Uiso 1 calc R . . C73 C 0.6280(5) -0.0719(5) 0.1806(2) 0.0202(17) Uani 1 d . . . C74 C 0.6262(5) -0.1498(5) 0.1649(2) 0.0214(17) Uani 1 d . . . C75 C 0.5704(5) -0.2346(5) 0.1830(2) 0.031(2) Uani 1 d . . . H75 H 0.5693 -0.2879 0.1730 0.037 Uiso 1 calc R . . C76 C 0.5165(6) -0.2432(6) 0.2151(3) 0.038(2) Uani 1 d . . . C77 C 0.5195(5) -0.1649(5) 0.2306(2) 0.0248(19) Uani 1 d . . . H77 H 0.4830 -0.1701 0.2525 0.030 Uiso 1 calc R . . C78 C 0.5760(5) -0.0787(5) 0.2137(2) 0.0225(18) Uani 1 d . . . C79 C 0.4527(6) -0.3382(6) 0.2337(2) 0.053(2) Uani 1 d DU . . C80 C 0.3554(9) -0.3503(11) 0.2371(5) 0.062(4) Uani 0.609(12) d PDU B 1 H80A H 0.3580 -0.3012 0.2534 0.093 Uiso 0.609(12) calc PR B 1 H80B H 0.3135 -0.4102 0.2488 0.093 Uiso 0.609(12) calc PR B 1 H80C H 0.3329 -0.3471 0.2113 0.093 Uiso 0.609(12) calc PR B 1 C81 C 0.4863(13) -0.3419(12) 0.2735(4) 0.076(5) Uani 0.609(12) d PDU B 1 H81A H 0.4930 -0.2896 0.2888 0.114 Uiso 0.609(12) calc PR B 1 H81B H 0.5460 -0.3390 0.2716 0.114 Uiso 0.609(12) calc PR B 1 H81C H 0.4418 -0.3995 0.2862 0.114 Uiso 0.609(12) calc PR B 1 C82 C 0.4410(14) -0.4190(10) 0.2097(5) 0.080(5) Uani 0.609(12) d PDU B 1 H82A H 0.4204 -0.4149 0.1836 0.120 Uiso 0.609(12) calc PR B 1 H82B H 0.3951 -0.4766 0.2219 0.120 Uiso 0.609(12) calc PR B 1 H82C H 0.5000 -0.4177 0.2081 0.120 Uiso 0.609(12) calc PR B 1 C80A C 0.4026(19) -0.3324(17) 0.2697(6) 0.080(6) Uani 0.391(12) d PDU B 2 H80D H 0.4477 -0.2895 0.2884 0.119 Uiso 0.391(12) calc PR B 2 H80E H 0.3675 -0.3935 0.2815 0.119 Uiso 0.391(12) calc PR B 2 H80F H 0.3604 -0.3104 0.2622 0.119 Uiso 0.391(12) calc PR B 2 C81A C 0.5169(14) -0.3705(16) 0.2499(8) 0.063(5) Uani 0.391(12) d PDU B 2 H81D H 0.5578 -0.3264 0.2694 0.095 Uiso 0.391(12) calc PR B 2 H81E H 0.5538 -0.3745 0.2288 0.095 Uiso 0.391(12) calc PR B 2 H81F H 0.4802 -0.4312 0.2619 0.095 Uiso 0.391(12) calc PR B 2 C82A C 0.3909(16) -0.4010(13) 0.2034(5) 0.051(5) Uani 0.391(12) d PDU B 2 H82D H 0.3516 -0.3777 0.1936 0.076 Uiso 0.391(12) calc PR B 2 H82E H 0.3524 -0.4625 0.2144 0.076 Uiso 0.391(12) calc PR B 2 H82F H 0.4279 -0.4043 0.1821 0.076 Uiso 0.391(12) calc PR B 2 C83 C 0.5799(5) 0.0065(5) 0.2328(2) 0.0235(18) Uani 1 d . . . H83A H 0.5785 -0.0013 0.2613 0.028 Uiso 1 calc R . . H83B H 0.6397 0.0613 0.2262 0.028 Uiso 1 calc R . . C84 C 0.5135(5) 0.0804(5) 0.18987(19) 0.0204(17) Uani 1 d . . . C85 C 0.5031(5) 0.0258(5) 0.2215(2) 0.0222(17) Uani 1 d . . . C86 C 0.4227(5) -0.0082(5) 0.2429(2) 0.0237(17) Uani 1 d . . . H86 H 0.4143 -0.0469 0.2644 0.028 Uiso 1 calc R . . C87 C 0.3532(5) 0.0123(5) 0.2340(2) 0.0251(18) Uani 1 d . . . C88 C 0.3687(5) 0.0711(5) 0.2027(2) 0.0253(18) Uani 1 d . . . H88 H 0.3238 0.0879 0.1964 0.030 Uiso 1 calc R . . C89 C 0.4478(5) 0.1054(5) 0.18063(19) 0.0196(16) Uani 1 d . . . C90 C 0.2635(6) -0.0302(5) 0.2568(2) 0.0298(19) Uani 1 d . . . C91 C 0.2826(7) 0.0060(7) 0.2974(3) 0.066(3) Uani 1 d . . . H91A H 0.2253 -0.0235 0.3124 0.099 Uiso 1 calc R . . H91B H 0.3074 0.0727 0.2970 0.099 Uiso 1 calc R . . H91C H 0.3275 -0.0076 0.3093 0.099 Uiso 1 calc R . . C92 C 0.1941(7) -0.0063(8) 0.2392(3) 0.071(3) Uani 1 d . . . H92A H 0.1783 -0.0315 0.2129 0.107 Uiso 1 calc R . . H92B H 0.2214 0.0608 0.2382 0.107 Uiso 1 calc R . . H92C H 0.1384 -0.0329 0.2551 0.107 Uiso 1 calc R . . C93 C 0.2176(6) -0.1350(6) 0.2571(3) 0.054(3) Uani 1 d . . . H93A H 0.2557 -0.1534 0.2718 0.081 Uiso 1 calc R . . H93B H 0.2107 -0.1576 0.2304 0.081 Uiso 1 calc R . . H93C H 0.1567 -0.1613 0.2693 0.081 Uiso 1 calc R . . C94 C 0.4581(5) 0.1623(5) 0.1451(2) 0.0263(18) Uani 1 d . . . H94A H 0.5242 0.2038 0.1395 0.032 Uiso 1 calc R . . H94B H 0.4294 0.2007 0.1499 0.032 Uiso 1 calc R . . C95 C 0.4627(5) 0.0740(5) 0.0866(2) 0.0213(17) Uani 1 d . . . C96 C 0.4118(5) 0.0991(5) 0.1108(2) 0.0220(18) Uani 1 d . . . C97 C 0.3174(5) 0.0556(5) 0.1064(2) 0.0222(17) Uani 1 d . . . H97 H 0.2830 0.0716 0.1234 0.027 Uiso 1 calc R . . C98 C 0.2711(5) -0.0101(5) 0.0784(2) 0.0275(18) Uani 1 d . . . C99 C 0.3234(5) -0.0336(5) 0.0547(2) 0.0248(18) Uani 1 d . . . H99 H 0.2927 -0.0803 0.0358 0.030 Uiso 1 calc R . . C100 C 0.4187(5) 0.0081(5) 0.0576(2) 0.0203(17) Uani 1 d . . . C101 C 0.1657(5) -0.0616(6) 0.0741(3) 0.038(2) Uani 1 d . . . C102 C 0.1417(6) -0.0459(8) 0.0340(3) 0.070(3) Uani 1 d . . . H10A H 0.1706 -0.0668 0.0149 0.105 Uiso 1 calc R . . H10B H 0.1641 0.0199 0.0302 0.105 Uiso 1 calc R . . H10C H 0.0747 -0.0806 0.0306 0.105 Uiso 1 calc R . . C103 C 0.1294(6) -0.1621(6) 0.0807(4) 0.072(4) Uani 1 d . . . H10D H 0.0620 -0.1949 0.0802 0.108 Uiso 1 calc R . . H10E H 0.1505 -0.1710 0.1060 0.108 Uiso 1 calc R . . H10F H 0.1521 -0.1863 0.0603 0.108 Uiso 1 calc R . . C104 C 0.1213(6) -0.0267(7) 0.1029(3) 0.069(3) Uani 1 d . . . H10G H 0.1450 0.0391 0.0987 0.103 Uiso 1 calc R . . H10H H 0.1358 -0.0365 0.1294 0.103 Uiso 1 calc R . . H10I H 0.0543 -0.0604 0.0992 0.103 Uiso 1 calc R . . C105 C 0.4719(5) -0.0250(5) 0.0328(2) 0.0213(17) Uani 1 d . . . H10A' H 0.4819 -0.0691 0.0482 0.026 Uiso 1 calc R . . H10B' H 0.4334 -0.0588 0.0102 0.026 Uiso 1 calc R . . C106 C 0.6453(5) 0.0731(5) 0.03765(19) 0.0176(16) Uani 1 d . . . C107 C 0.5641(5) 0.0500(5) 0.01812(19) 0.0199(17) Uani 1 d . . . C108 C 0.5690(5) 0.0991(5) -0.0152(2) 0.0236(17) Uani 1 d . . . H108 H 0.5138 0.0826 -0.0290 0.028 Uiso 1 calc R . . C109 C 0.6520(5) 0.1719(5) -0.0292(2) 0.0268(18) Uani 1 d . . . C110 C 0.7306(5) 0.1912(5) -0.0090(2) 0.0221(17) Uani 1 d . . . H110 H 0.7879 0.2393 -0.0183 0.027 Uiso 1 calc R . . C111 C 0.7306(5) 0.1445(5) 0.0241(2) 0.0230(17) Uani 1 d . . . C112 C 0.6531(6) 0.2222(6) -0.0673(2) 0.035(2) Uani 1 d . . . C113 C 0.6570(9) 0.1691(8) -0.1014(3) 0.083(4) Uani 1 d . . . H11A H 0.7094 0.1590 -0.0985 0.124 Uiso 1 calc R . . H11B H 0.6644 0.2040 -0.1252 0.124 Uiso 1 calc R . . H11C H 0.5999 0.1096 -0.1028 0.124 Uiso 1 calc R . . C114 C 0.5695(7) 0.2338(8) -0.0696(3) 0.080(4) Uani 1 d . . . H11D H 0.5762 0.2738 -0.0915 0.120 Uiso 1 calc R . . H11E H 0.5639 0.2615 -0.0455 0.120 Uiso 1 calc R . . H11F H 0.5143 0.1734 -0.0732 0.120 Uiso 1 calc R . . C115 C 0.7385(7) 0.3194(7) -0.0683(3) 0.065(3) Uani 1 d . . . H11G H 0.7943 0.3146 -0.0663 0.097 Uiso 1 calc R . . H11H H 0.7361 0.3556 -0.0465 0.097 Uiso 1 calc R . . H11I H 0.7395 0.3497 -0.0927 0.097 Uiso 1 calc R . . C116 C 0.8166(5) 0.1735(5) 0.0468(2) 0.0216(17) Uani 1 d . . . H11A' H 0.8688 0.1899 0.0289 0.026 Uiso 1 calc R . . H11B' H 0.8091 0.1221 0.0634 0.026 Uiso 1 calc R . . N5 N 0.4093(12) 0.3202(11) 0.0660(4) 0.163(6) Uani 1 d DU . . C117 C 0.3981(11) 0.2623(10) 0.0445(4) 0.110(4) Uani 1 d DU . . C118 C 0.3839(8) 0.1913(8) 0.0182(3) 0.083(4) Uani 1 d DU . . H11J H 0.4266 0.2179 -0.0037 0.125 Uiso 1 calc R . . H11K H 0.3204 0.1611 0.0086 0.125 Uiso 1 calc R . . H11L H 0.3948 0.1460 0.0314 0.125 Uiso 1 calc R . . N6 N 0.6872(6) 0.7019(9) 0.0556(4) 0.117(4) Uani 1 d DU . . C119 C 0.7658(7) 0.7347(8) 0.0556(3) 0.071(3) Uani 1 d DU . . C120 C 0.8632(6) 0.7802(7) 0.0546(3) 0.073(3) Uani 1 d DU . . H12A H 0.8841 0.7893 0.0276 0.110 Uiso 1 calc R . . H12B H 0.8845 0.7427 0.0680 0.110 Uiso 1 calc R . . H12C H 0.8886 0.8402 0.0675 0.110 Uiso 1 calc R . . N7 N 0.2581(6) 0.1996(7) 0.1612(3) 0.086(3) Uani 1 d DU . . C121 C 0.3030(7) 0.2780(7) 0.1580(3) 0.071(3) Uani 1 d DU . . C122 C 0.3613(10) 0.3732(7) 0.1516(4) 0.117(5) Uani 1 d DU . . H12D H 0.4255 0.3874 0.1510 0.175 Uiso 1 calc R . . H12E H 0.3532 0.4079 0.1726 0.175 Uiso 1 calc R . . H12F H 0.3456 0.3904 0.1268 0.175 Uiso 1 calc R . . N8 N 0.6998(12) 0.9525(12) 0.3104(4) 0.164(5) Uani 1 d DU . . C123 C 0.7265(11) 0.9224(11) 0.2872(3) 0.109(4) Uani 1 d DU . . C124 C 0.7583(7) 0.8839(7) 0.2589(3) 0.061(3) Uani 1 d DU . . H12G H 0.8258 0.9182 0.2584 0.092 Uiso 1 calc R . . H12H H 0.7345 0.8875 0.2334 0.092 Uiso 1 calc R . . H12I H 0.7367 0.8193 0.2653 0.092 Uiso 1 calc R . . N9 N 0.613(3) 0.547(2) 0.1412(16) 0.71(3) Uani 1 d DU . . C125 C 0.617(4) 0.486(3) 0.1278(16) 0.71(3) Uani 1 d DU . . C126 C 0.619(2) 0.406(2) 0.1151(13) 0.71(3) Uani 1 d DU . . H12J H 0.6798 0.4141 0.1203 1.062 Uiso 1 calc R . . H12K H 0.6063 0.3979 0.0872 1.062 Uiso 1 calc R . . H12L H 0.5720 0.3522 0.1291 1.062 Uiso 1 calc R . . N10 N 0.6444(11) 0.3069(10) 0.0536(4) 0.157(5) Uani 1 d DU . . C127 C 0.6474(18) 0.3664(13) 0.0354(7) 0.205(7) Uani 1 d DU . . C128 C 0.6534(17) 0.4481(13) 0.0211(6) 0.238(9) Uani 1 d DU . . H12M H 0.7133 0.4859 0.0086 0.356 Uiso 1 calc R . . H12N H 0.6468 0.4826 0.0426 0.356 Uiso 1 calc R . . H12O H 0.6042 0.4327 0.0022 0.356 Uiso 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 0.0151(4) 0.0201(4) 0.0227(4) 0.0004(3) -0.0001(3) 0.0076(3) Mo2 0.0168(4) 0.0193(4) 0.0205(3) -0.0012(3) -0.0007(3) 0.0077(3) N1 0.015(3) 0.023(4) 0.019(3) 0.001(3) 0.000(3) 0.008(3) C1 0.023(4) 0.014(4) 0.023(4) 0.004(3) 0.004(3) 0.010(4) C2 0.035(5) 0.036(5) 0.037(5) 0.002(4) 0.003(4) 0.017(5) C3 0.036(5) 0.032(5) 0.058(6) -0.009(5) -0.003(5) 0.008(5) C4 0.031(5) 0.029(5) 0.052(6) -0.005(5) 0.005(5) 0.002(4) C5 0.032(5) 0.048(6) 0.033(5) 0.011(4) 0.015(4) 0.007(5) C6 0.017(4) 0.021(4) 0.030(5) 0.005(4) 0.004(4) 0.001(4) C7 0.026(5) 0.024(4) 0.030(5) -0.003(4) 0.005(4) 0.005(4) C8 0.025(5) 0.035(5) 0.038(5) -0.006(4) -0.004(4) 0.013(4) C9 0.046(6) 0.040(5) 0.032(5) 0.006(4) 0.006(4) 0.031(5) C10 0.056(6) 0.070(7) 0.035(6) 0.002(5) 0.002(5) 0.050(6) C11 0.053(7) 0.077(8) 0.044(6) 0.020(6) 0.016(5) 0.046(7) C12 0.058(7) 0.079(8) 0.042(6) 0.002(6) -0.001(5) 0.057(7) C13 0.046(6) 0.044(6) 0.056(6) 0.009(5) 0.002(5) 0.033(5) C14 0.048(6) 0.047(6) 0.029(5) 0.007(4) 0.008(4) 0.032(5) N2 0.042(5) 0.054(6) 0.051(5) -0.012(4) -0.006(4) 0.023(5) N3 0.025(4) 0.018(4) 0.030(4) 0.005(3) 0.001(3) 0.007(3) C15 0.018(4) 0.025(5) 0.032(5) 0.000(4) -0.004(4) 0.007(4) C16 0.021(4) 0.030(5) 0.029(5) -0.007(4) -0.003(4) 0.007(4) C17 0.024(5) 0.025(5) 0.062(6) -0.003(4) 0.014(4) 0.001(4) C18 0.020(5) 0.024(5) 0.053(6) -0.006(4) -0.003(4) -0.007(4) C19 0.019(5) 0.024(5) 0.054(6) -0.005(4) 0.006(4) -0.002(4) C20 0.040(5) 0.023(5) 0.024(5) -0.006(4) -0.003(4) 0.014(4) C21 0.038(6) 0.028(5) 0.064(7) -0.017(5) 0.013(5) 0.002(5) C22 0.050(8) 0.121(13) 0.25(2) -0.150(14) 0.043(10) -0.017(8) C23 0.046(8) 0.103(11) 0.100(11) -0.081(9) 0.013(7) 0.009(8) C24 0.089(11) 0.071(10) 0.104(11) -0.023(8) 0.018(9) 0.018(9) C25 0.086(10) 0.088(10) 0.054(8) -0.011(7) -0.005(7) 0.028(9) C26 0.076(9) 0.071(9) 0.046(7) -0.022(7) 0.000(6) -0.001(8) C27 0.064(8) 0.083(9) 0.045(7) 0.008(6) 0.007(6) 0.012(7) C28 0.041(7) 0.107(11) 0.071(9) -0.045(8) 0.005(6) 0.012(8) N4 0.086(9) 0.228(15) 0.094(9) -0.069(9) -0.021(7) 0.077(10) O1 0.015(3) 0.020(3) 0.017(3) 0.002(2) 0.001(2) 0.009(2) O2 0.017(3) 0.024(3) 0.021(3) -0.004(2) 0.000(2) 0.008(2) O3 0.020(3) 0.025(3) 0.027(3) 0.004(2) -0.001(2) 0.014(2) O4 0.019(3) 0.018(3) 0.033(3) 0.003(2) 0.005(2) 0.010(2) O5 0.015(3) 0.012(3) 0.025(3) -0.001(2) -0.001(2) 0.004(2) O6 0.017(3) 0.023(3) 0.024(3) -0.001(2) 0.002(2) 0.009(2) O7 0.014(3) 0.023(3) 0.023(3) -0.001(2) 0.001(2) 0.009(2) O8 0.024(3) 0.022(3) 0.017(3) -0.003(2) -0.002(2) 0.013(2) C29 0.012(4) 0.009(4) 0.025(4) 0.003(3) -0.003(3) 0.004(3) C30 0.021(4) 0.018(4) 0.024(5) -0.002(3) -0.002(3) 0.009(4) C31 0.019(4) 0.023(4) 0.024(4) -0.003(3) 0.001(3) 0.008(4) C32 0.036(5) 0.023(4) 0.025(5) 0.003(4) -0.003(4) 0.012(4) C33 0.030(5) 0.021(4) 0.033(5) -0.005(4) -0.002(4) 0.016(4) C34 0.020(4) 0.022(4) 0.021(4) 0.001(3) -0.003(3) 0.011(4) C35 0.052(6) 0.013(4) 0.052(6) -0.005(4) -0.003(5) 0.013(4) C36 0.070(8) 0.029(6) 0.101(9) 0.020(6) -0.009(7) -0.015(6) C37 0.096(9) 0.047(7) 0.108(10) 0.044(7) 0.023(8) 0.040(7) C38 0.116(10) 0.017(5) 0.052(7) 0.019(5) 0.026(6) 0.012(6) C39 0.028(5) 0.021(4) 0.031(5) -0.002(4) -0.001(4) 0.017(4) C40 0.011(4) 0.031(5) 0.022(4) -0.008(4) 0.002(3) 0.010(4) C41 0.021(4) 0.028(5) 0.022(4) -0.003(4) 0.003(3) 0.014(4) C42 0.033(5) 0.036(5) 0.025(4) -0.001(4) -0.002(4) 0.025(4) C43 0.043(5) 0.030(5) 0.033(5) -0.004(4) -0.004(4) 0.026(4) C44 0.035(5) 0.041(5) 0.020(4) -0.015(4) -0.014(4) 0.021(4) C45 0.027(4) 0.029(5) 0.031(5) -0.005(4) 0.002(4) 0.017(4) C46 0.072(7) 0.033(6) 0.055(6) -0.019(5) -0.028(6) 0.029(6) C47 0.090(9) 0.023(6) 0.120(11) -0.016(6) -0.046(8) 0.014(6) C48 0.078(9) 0.069(8) 0.178(13) -0.077(10) -0.012(9) 0.041(8) C49 0.082(8) 0.035(6) 0.087(9) -0.023(6) -0.052(7) 0.021(6) C50 0.027(5) 0.044(5) 0.019(4) 0.003(4) -0.002(4) 0.015(4) C51 0.026(5) 0.022(4) 0.029(5) 0.003(4) -0.012(4) 0.010(4) C52 0.028(5) 0.034(5) 0.022(4) 0.005(4) -0.006(4) 0.017(4) C53 0.032(5) 0.027(4) 0.029(5) 0.006(4) -0.002(4) 0.020(4) C54 0.026(5) 0.030(5) 0.034(5) 0.002(4) -0.009(4) 0.010(4) C55 0.021(4) 0.032(5) 0.044(5) 0.006(4) 0.000(4) 0.019(4) C56 0.025(5) 0.022(4) 0.035(5) -0.003(4) 0.002(4) 0.013(4) C57 0.026(5) 0.035(5) 0.045(6) -0.004(4) -0.013(4) 0.010(4) C58 0.053(7) 0.035(7) 0.156(13) 0.011(7) -0.046(8) -0.011(6) C59 0.031(6) 0.134(12) 0.139(12) -0.067(10) -0.028(7) 0.041(8) C60 0.053(7) 0.086(9) 0.060(8) 0.008(6) -0.029(6) 0.005(6) C61 0.017(4) 0.025(5) 0.038(5) 0.006(4) 0.004(4) 0.011(4) C62 0.022(4) 0.029(5) 0.020(4) 0.000(4) 0.005(3) 0.015(4) C63 0.027(5) 0.032(5) 0.026(5) 0.004(4) 0.007(4) 0.017(4) C64 0.024(5) 0.040(5) 0.046(5) 0.007(4) 0.003(4) 0.024(4) C65 0.030(5) 0.034(5) 0.040(5) 0.009(4) 0.005(4) 0.021(4) C66 0.043(6) 0.017(4) 0.039(5) 0.004(4) 0.008(4) 0.018(4) C67 0.029(5) 0.034(5) 0.018(4) 0.005(4) 0.002(4) 0.020(4) C68 0.060(4) 0.036(4) 0.080(5) 0.017(3) 0.002(4) 0.037(4) C69 0.075(6) 0.039(5) 0.087(6) 0.011(4) -0.004(5) 0.043(5) C70 0.065(5) 0.037(5) 0.080(6) 0.021(5) -0.001(4) 0.042(5) C71 0.066(5) 0.038(6) 0.082(6) 0.024(5) 0.002(5) 0.032(5) C69A 0.068(6) 0.034(6) 0.083(7) 0.017(6) 0.000(6) 0.036(5) C70A 0.064(6) 0.038(6) 0.086(7) 0.014(6) -0.001(6) 0.046(5) C71A 0.066(7) 0.042(6) 0.082(5) 0.019(5) 0.000(5) 0.034(6) C72 0.034(5) 0.019(4) 0.033(5) 0.004(4) 0.009(4) 0.011(4) C73 0.015(4) 0.016(4) 0.025(4) 0.006(3) -0.002(3) 0.005(3) C74 0.016(4) 0.022(4) 0.024(4) 0.004(4) 0.003(3) 0.008(4) C75 0.025(5) 0.026(5) 0.036(5) 0.002(4) -0.004(4) 0.008(4) C76 0.021(5) 0.030(5) 0.056(6) 0.011(4) 0.000(4) 0.007(4) C77 0.022(4) 0.025(5) 0.020(4) 0.013(4) 0.005(3) 0.007(4) C78 0.015(4) 0.032(5) 0.020(4) -0.004(4) -0.004(3) 0.011(4) C79 0.062(5) 0.031(4) 0.052(5) 0.022(4) 0.019(4) 0.013(4) C80 0.054(7) 0.051(8) 0.054(9) 0.031(7) 0.026(6) 0.006(7) C81 0.080(9) 0.050(8) 0.068(7) 0.037(6) 0.004(7) 0.010(8) C82 0.081(11) 0.027(7) 0.097(9) 0.008(7) 0.033(9) 0.001(7) C80A 0.081(11) 0.048(10) 0.068(9) 0.022(8) 0.044(8) 0.001(9) C81A 0.081(11) 0.031(10) 0.059(12) 0.032(9) 0.001(8) 0.013(8) C82A 0.057(12) 0.018(9) 0.060(9) 0.029(6) 0.014(7) 0.006(8) C83 0.020(4) 0.034(5) 0.016(4) 0.004(3) 0.002(3) 0.012(4) C84 0.023(4) 0.034(5) 0.013(4) -0.010(3) -0.001(3) 0.022(4) C85 0.013(4) 0.024(4) 0.022(4) -0.007(3) 0.001(3) 0.004(3) C86 0.023(4) 0.022(4) 0.020(4) -0.007(3) -0.004(3) 0.008(4) C87 0.015(4) 0.033(5) 0.025(4) -0.006(4) -0.005(3) 0.011(4) C88 0.022(4) 0.024(4) 0.028(5) -0.005(4) -0.003(4) 0.011(4) C89 0.023(4) 0.022(4) 0.013(4) -0.005(3) 0.004(3) 0.010(3) C90 0.037(5) 0.022(4) 0.027(5) -0.003(4) 0.008(4) 0.013(4) C91 0.055(7) 0.076(8) 0.050(6) -0.006(6) 0.029(5) 0.020(6) C92 0.047(6) 0.100(9) 0.083(8) 0.050(7) 0.025(6) 0.049(7) C93 0.025(5) 0.047(6) 0.067(7) 0.003(5) 0.015(5) 0.001(5) C94 0.011(4) 0.020(4) 0.044(5) -0.008(4) 0.006(4) 0.005(3) C95 0.026(4) 0.017(4) 0.013(4) 0.008(3) 0.005(3) 0.005(4) C96 0.026(4) 0.024(4) 0.020(4) 0.002(3) -0.005(3) 0.015(4) C97 0.018(4) 0.024(4) 0.029(4) 0.009(4) 0.001(3) 0.014(4) C98 0.018(4) 0.028(5) 0.035(5) 0.003(4) -0.004(4) 0.010(4) C99 0.029(5) 0.024(4) 0.023(4) -0.004(3) -0.008(4) 0.014(4) C100 0.016(4) 0.023(4) 0.020(4) 0.005(3) -0.002(3) 0.008(4) C101 0.025(5) 0.042(5) 0.049(6) -0.008(4) -0.010(4) 0.019(4) C102 0.030(6) 0.121(10) 0.062(7) -0.009(7) -0.015(5) 0.040(7) C103 0.032(6) 0.033(6) 0.144(11) 0.018(6) -0.013(6) 0.011(5) C104 0.014(5) 0.080(8) 0.102(9) -0.026(7) -0.002(5) 0.017(5) C105 0.021(4) 0.022(4) 0.015(4) -0.008(3) -0.005(3) 0.006(4) C106 0.023(4) 0.023(4) 0.015(4) -0.008(3) -0.005(3) 0.018(4) C107 0.016(4) 0.027(4) 0.014(4) -0.004(3) 0.005(3) 0.008(3) C108 0.023(4) 0.023(4) 0.028(4) 0.000(3) 0.001(3) 0.014(4) C109 0.029(5) 0.033(5) 0.026(4) 0.001(4) 0.004(4) 0.020(4) C110 0.019(4) 0.022(4) 0.025(4) 0.001(3) 0.005(3) 0.010(3) C111 0.023(4) 0.027(4) 0.022(4) -0.006(3) 0.002(3) 0.014(4) C112 0.035(5) 0.050(6) 0.027(5) 0.010(4) 0.003(4) 0.027(5) C113 0.142(12) 0.078(9) 0.025(6) 0.012(6) 0.001(6) 0.052(8) C114 0.049(7) 0.104(9) 0.090(9) 0.069(7) 0.016(6) 0.041(7) C115 0.073(8) 0.059(7) 0.066(8) 0.029(6) 0.006(6) 0.036(6) C116 0.020(4) 0.029(5) 0.020(4) -0.002(3) 0.001(3) 0.016(4) N5 0.181(12) 0.146(13) 0.150(13) -0.029(8) -0.007(11) 0.073(11) C117 0.121(9) 0.112(12) 0.106(12) 0.010(7) -0.012(9) 0.065(10) C118 0.088(8) 0.093(9) 0.097(9) 0.038(6) 0.016(7) 0.066(8) N6 0.064(4) 0.144(10) 0.120(8) -0.043(8) 0.005(7) 0.035(7) C119 0.064(4) 0.072(7) 0.072(7) -0.009(6) -0.002(7) 0.031(6) C120 0.065(4) 0.074(8) 0.091(8) -0.002(6) -0.011(6) 0.042(6) N7 0.059(7) 0.081(5) 0.119(8) -0.027(7) 0.005(6) 0.035(5) C121 0.067(8) 0.078(5) 0.082(7) -0.022(7) -0.016(6) 0.046(6) C122 0.143(12) 0.078(5) 0.113(10) -0.015(8) -0.022(9) 0.044(8) N8 0.242(13) 0.236(13) 0.103(10) -0.010(9) 0.019(10) 0.186(11) C123 0.163(11) 0.152(11) 0.066(9) -0.001(8) -0.006(8) 0.121(8) C124 0.072(7) 0.074(7) 0.050(6) 0.019(5) -0.002(5) 0.045(6) N9 0.170(16) 0.38(4) 1.19(6) 0.54(5) -0.22(3) -0.16(3) C125 0.189(15) 0.38(4) 1.16(6) 0.56(5) -0.21(3) -0.16(3) C126 0.194(19) 0.39(4) 1.14(6) 0.56(5) -0.20(3) -0.15(3) N10 0.178(12) 0.165(14) 0.139(13) 0.035(9) -0.022(10) 0.094(12) C127 0.242(15) 0.190(16) 0.188(15) 0.068(11) -0.020(13) 0.110(14) C128 0.290(19) 0.202(18) 0.205(17) 0.108(14) -0.007(15) 0.111(16) _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 1.735(6) . ? Mo1 O2 1.925(5) . ? Mo1 O3 1.940(5) . ? Mo1 O4 1.961(5) . ? Mo1 O1 2.078(4) . ? Mo1 O5 2.216(5) . ? Mo2 N3 1.727(6) . ? Mo2 O6 1.940(5) . ? Mo2 O7 1.940(5) . ? Mo2 O8 1.957(4) . ? Mo2 O5 2.061(5) . ? Mo2 O1 2.247(4) . ? N1 C1 1.385(9) . ? C1 C6 1.384(10) . ? C1 C2 1.401(10) . ? C2 C3 1.370(11) . ? C3 C4 1.395(11) . ? C4 C5 1.368(11) . ? C5 C6 1.406(10) . ? C6 C7 1.513(10) . ? C7 C8 1.547(10) . ? C8 C9 1.500(10) . ? C9 C14 1.399(11) . ? C9 C10 1.406(11) . ? C10 C11 1.352(12) . ? C11 C12 1.396(13) . ? C12 C13 1.391(12) . ? C13 C14 1.399(11) . ? C14 N2 1.372(11) . ? N3 C15 1.400(9) . ? C15 C20 1.403(10) . ? C15 C16 1.411(10) . ? C16 C17 1.380(10) . ? C17 C18 1.362(11) . ? C18 C19 1.395(11) . ? C19 C20 1.379(10) . ? C20 C21 1.497(11) . ? C21 C22 1.337(14) . ? C22 C23 1.532(16) . ? C23 C24 1.345(18) . ? C23 C28 1.442(19) . ? C24 C25 1.392(16) . ? C25 C26 1.360(16) . ? C26 C27 1.352(16) . ? C27 C28 1.367(15) . ? C28 N4 1.422(16) . ? O1 C29 1.387(8) . ? O2 C40 1.365(8) . ? O3 C51 1.386(8) . ? O4 C62 1.365(8) . ? O5 C73 1.391(8) . ? O6 C84 1.365(8) . ? O7 C95 1.373(8) . ? O8 C106 1.362(8) . ? C29 C30 1.371(9) . ? C29 C34 1.403(10) . ? C30 C31 1.404(10) . ? C30 C116 1.548(10) . ? C31 C32 1.382(10) . ? C32 C33 1.389(10) . ? C32 C35 1.530(11) . ? C33 C34 1.391(10) . ? C34 C39 1.511(10) . ? C35 C36 1.493(13) . ? C35 C38 1.502(12) . ? C35 C37 1.536(12) . ? C39 C41 1.535(10) . ? C40 C41 1.375(10) . ? C40 C45 1.404(10) . ? C41 C42 1.359(10) . ? C42 C43 1.431(10) . ? C43 C44 1.394(11) . ? C43 C46 1.556(12) . ? C44 C45 1.413(10) . ? C45 C50 1.533(10) . ? C46 C49 1.512(12) . ? C46 C47 1.511(14) . ? C46 C48 1.520(13) . ? C50 C52 1.508(10) . ? C51 C52 1.353(10) . ? C51 C56 1.417(10) . ? C52 C53 1.391(10) . ? C53 C54 1.407(11) . ? C54 C55 1.375(10) . ? C54 C57 1.535(10) . ? C55 C56 1.409(10) . ? C56 C61 1.486(10) . ? C57 C59 1.465(12) . ? C57 C58 1.489(12) . ? C57 C60 1.525(12) . ? C61 C63 1.499(10) . ? C62 C63 1.397(10) . ? C62 C67 1.399(10) . ? C63 C64 1.397(10) . ? C64 C65 1.387(11) . ? C65 C66 1.384(11) . ? C65 C68 1.520(11) . ? C66 C67 1.382(10) . ? C67 C72 1.515(10) . ? C68 C69 1.477(11) . ? C68 C71A 1.506(14) . ? C68 C70 1.544(11) . ? C68 C69A 1.552(15) . ? C68 C70A 1.557(14) . ? C68 C71 1.561(11) . ? C72 C74 1.503(10) . ? C73 C74 1.399(10) . ? C73 C78 1.407(10) . ? C74 C75 1.398(10) . ? C75 C76 1.393(11) . ? C76 C77 1.395(11) . ? C76 C79 1.546(11) . ? C77 C78 1.397(10) . ? C78 C83 1.545(10) . ? C79 C82A 1.478(14) . ? C79 C81 1.497(12) . ? C79 C82 1.515(12) . ? C79 C80A 1.529(14) . ? C79 C81A 1.532(14) . ? C79 C80 1.544(12) . ? C83 C85 1.528(10) . ? C84 C85 1.379(10) . ? C84 C89 1.397(9) . ? C85 C86 1.384(9) . ? C86 C87 1.404(10) . ? C87 C88 1.397(10) . ? C87 C90 1.523(10) . ? C88 C89 1.381(9) . ? C89 C94 1.510(10) . ? C90 C91 1.495(11) . ? C90 C93 1.526(11) . ? C90 C92 1.533(11) . ? C94 C96 1.519(10) . ? C95 C100 1.396(10) . ? C95 C96 1.400(10) . ? C96 C97 1.382(9) . ? C97 C98 1.377(10) . ? C98 C99 1.393(10) . ? C98 C101 1.538(10) . ? C99 C100 1.390(10) . ? C100 C105 1.530(10) . ? C101 C103 1.496(11) . ? C101 C102 1.502(12) . ? C101 C104 1.524(12) . ? C105 C107 1.511(9) . ? C106 C107 1.390(9) . ? C106 C111 1.409(9) . ? C107 C108 1.394(9) . ? C108 C109 1.401(10) . ? C109 C110 1.378(10) . ? C109 C112 1.557(10) . ? C110 C111 1.386(9) . ? C111 C116 1.493(9) . ? C112 C113 1.497(12) . ? C112 C114 1.508(12) . ? C112 C115 1.541(12) . ? N5 C117 1.159(9) . ? C117 C118 1.420(10) . ? N6 C119 1.147(9) . ? C119 C120 1.417(9) . ? N7 C121 1.148(9) . ? C121 C122 1.411(9) . ? N8 C123 1.152(9) . ? C123 C124 1.412(9) . ? N9 C125 1.156(10) . ? C125 C126 1.418(11) . ? N10 C127 1.159(9) . ? C127 C128 1.412(10) . ? 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 O2 98.5(2) . . ? N1 Mo1 O3 96.9(2) . . ? O2 Mo1 O3 84.1(2) . . ? N1 Mo1 O4 96.5(2) . . ? O2 Mo1 O4 161.6(2) . . ? O3 Mo1 O4 83.7(2) . . ? N1 Mo1 O1 94.3(2) . . ? O2 Mo1 O1 87.17(19) . . ? O3 Mo1 O1 166.67(18) . . ? O4 Mo1 O1 102.17(19) . . ? N1 Mo1 O5 164.6(2) . . ? O2 Mo1 O5 86.36(18) . . ? O3 Mo1 O5 98.08(19) . . ? O4 Mo1 O5 81.85(18) . . ? O1 Mo1 O5 71.26(17) . . ? N3 Mo2 O6 98.8(2) . . ? N3 Mo2 O7 96.1(2) . . ? O6 Mo2 O7 84.62(19) . . ? N3 Mo2 O8 97.6(2) . . ? O6 Mo2 O8 160.13(19) . . ? O7 Mo2 O8 82.49(19) . . ? N3 Mo2 O5 94.0(2) . . ? O6 Mo2 O5 85.70(19) . . ? O7 Mo2 O5 166.95(19) . . ? O8 Mo2 O5 104.34(18) . . ? N3 Mo2 O1 164.3(2) . . ? O6 Mo2 O1 84.70(18) . . ? O7 Mo2 O1 99.44(17) . . ? O8 Mo2 O1 82.58(17) . . ? O5 Mo2 O1 70.91(17) . . ? C1 N1 Mo1 178.1(5) . . ? C6 C1 N1 121.4(7) . . ? C6 C1 C2 121.1(7) . . ? N1 C1 C2 117.4(7) . . ? C3 C2 C1 121.1(8) . . ? C2 C3 C4 117.4(8) . . ? C5 C4 C3 122.4(8) . . ? C4 C5 C6 120.2(8) . . ? C1 C6 C5 117.6(7) . . ? C1 C6 C7 124.4(6) . . ? C5 C6 C7 118.0(7) . . ? C6 C7 C8 111.8(6) . . ? C9 C8 C7 115.1(6) . . ? C14 C9 C10 118.4(8) . . ? C14 C9 C8 122.5(8) . . ? C10 C9 C8 119.1(8) . . ? C11 C10 C9 121.9(10) . . ? C10 C11 C12 119.3(9) . . ? C13 C12 C11 121.1(9) . . ? C12 C13 C14 118.8(9) . . ? N2 C14 C9 121.0(8) . . ? N2 C14 C13 118.4(9) . . ? C9 C14 C13 120.5(8) . . ? C15 N3 Mo2 178.7(6) . . ? N3 C15 C20 122.8(7) . . ? N3 C15 C16 115.7(7) . . ? C20 C15 C16 121.5(7) . . ? C17 C16 C15 119.6(8) . . ? C18 C17 C16 118.6(8) . . ? C17 C18 C19 122.5(8) . . ? C20 C19 C18 120.4(8) . . ? C19 C20 C15 117.3(8) . . ? C19 C20 C21 121.3(7) . . ? C15 C20 C21 121.3(7) . . ? C22 C21 C20 124.4(9) . . ? C21 C22 C23 124.0(13) . . ? C24 C23 C28 118.5(12) . . ? C24 C23 C22 117.3(17) . . ? C28 C23 C22 124.0(15) . . ? C23 C24 C25 121.9(15) . . ? C26 C25 C24 118.2(14) . . ? C27 C26 C25 122.2(12) . . ? C26 C27 C28 120.5(14) . . ? C27 C28 N4 119.6(15) . . ? C27 C28 C23 118.5(13) . . ? N4 C28 C23 121.8(13) . . ? C29 O1 Mo1 120.0(4) . . ? C29 O1 Mo2 131.8(4) . . ? Mo1 O1 Mo2 107.91(19) . . ? C40 O2 Mo1 126.9(4) . . ? C51 O3 Mo1 125.0(4) . . ? C62 O4 Mo1 128.7(4) . . ? C73 O5 Mo2 119.4(4) . . ? C73 O5 Mo1 130.6(4) . . ? Mo2 O5 Mo1 109.7(2) . . ? C84 O6 Mo2 127.5(4) . . ? C95 O7 Mo2 122.3(4) . . ? C106 O8 Mo2 127.9(4) . . ? C30 C29 O1 119.5(6) . . ? C30 C29 C34 120.0(6) . . ? O1 C29 C34 120.5(6) . . ? C29 C30 C31 119.9(7) . . ? C29 C30 C116 122.2(6) . . ? C31 C30 C116 117.6(6) . . ? C32 C31 C30 121.7(7) . . ? C31 C32 C33 117.0(7) . . ? C31 C32 C35 121.9(7) . . ? C33 C32 C35 121.1(7) . . ? C32 C33 C34 122.9(7) . . ? C33 C34 C29 118.4(7) . . ? C33 C34 C39 118.6(7) . . ? C29 C34 C39 123.0(7) . . ? C36 C35 C38 108.6(9) . . ? C36 C35 C32 109.7(7) . . ? C38 C35 C32 112.9(7) . . ? C36 C35 C37 109.3(8) . . ? C38 C35 C37 107.4(8) . . ? C32 C35 C37 108.8(7) . . ? C34 C39 C41 117.4(6) . . ? O2 C40 C41 120.6(6) . . ? O2 C40 C45 118.4(7) . . ? C41 C40 C45 120.9(7) . . ? C42 C41 C40 120.0(7) . . ? C42 C41 C39 121.4(7) . . ? C40 C41 C39 118.6(7) . . ? C41 C42 C43 121.9(7) . . ? C44 C43 C42 117.3(7) . . ? C44 C43 C46 121.2(7) . . ? C42 C43 C46 121.5(7) . . ? C43 C44 C45 121.0(7) . . ? C40 C45 C44 118.6(7) . . ? C40 C45 C50 120.0(7) . . ? C44 C45 C50 120.8(7) . . ? C49 C46 C47 106.0(9) . . ? C49 C46 C48 112.9(9) . . ? C47 C46 C48 110.3(9) . . ? C49 C46 C43 110.1(7) . . ? C47 C46 C43 111.0(7) . . ? C48 C46 C43 106.6(8) . . ? C52 C50 C45 110.7(6) . . ? C52 C51 O3 119.4(7) . . ? C52 C51 C56 123.0(7) . . ? O3 C51 C56 117.5(7) . . ? C51 C52 C53 118.0(7) . . ? C51 C52 C50 122.0(7) . . ? C53 C52 C50 119.4(7) . . ? C52 C53 C54 123.4(7) . . ? C55 C54 C53 115.6(7) . . ? C55 C54 C57 122.6(7) . . ? C53 C54 C57 121.6(7) . . ? C54 C55 C56 124.3(7) . . ? C55 C56 C51 115.6(7) . . ? C55 C56 C61 121.8(7) . . ? C51 C56 C61 122.0(7) . . ? C59 C57 C58 107.4(9) . . ? C59 C57 C60 110.4(9) . . ? C58 C57 C60 105.2(9) . . ? C59 C57 C54 114.3(8) . . ? C58 C57 C54 109.4(7) . . ? C60 C57 C54 109.8(7) . . ? C56 C61 C63 118.6(6) . . ? O4 C62 C63 120.1(7) . . ? O4 C62 C67 119.8(7) . . ? C63 C62 C67 120.1(7) . . ? C62 C63 C64 118.0(7) . . ? C62 C63 C61 121.5(7) . . ? C64 C63 C61 120.5(7) . . ? C65 C64 C63 123.9(7) . . ? C66 C65 C64 115.2(7) . . ? C66 C65 C68 122.0(8) . . ? C64 C65 C68 122.8(7) . . ? C67 C66 C65 124.3(8) . . ? C66 C67 C62 118.4(7) . . ? C66 C67 C72 121.2(7) . . ? C62 C67 C72 120.1(7) . . ? C69 C68 C71A 134.6(14) . . ? C69 C68 C65 111.1(8) . . ? C71A C68 C65 114.3(13) . . ? C69 C68 C70 111.5(9) . . ? C71A C68 C70 51.0(12) . . ? C65 C68 C70 111.5(8) . . ? C69 C68 C69A 46.6(11) . . ? C71A C68 C69A 110.5(14) . . ? C65 C68 C69A 114.3(12) . . ? C70 C68 C69A 134.0(13) . . ? C69 C68 C70A 56.4(11) . . ? C71A C68 C70A 108.6(14) . . ? C65 C68 C70A 107.4(11) . . ? C70 C68 C70A 61.0(11) . . ? C69A C68 C70A 100.6(13) . . ? C69 C68 C71 110.6(9) . . ? C71A C68 C71 55.5(12) . . ? C65 C68 C71 106.4(7) . . ? C70 C68 C71 105.5(9) . . ? C69A C68 C71 65.2(12) . . ? C70A C68 C71 146.2(12) . . ? C74 C72 C67 111.6(6) . . ? O5 C73 C74 118.4(6) . . ? O5 C73 C78 120.4(6) . . ? C74 C73 C78 121.0(6) . . ? C75 C74 C73 117.9(7) . . ? C75 C74 C72 120.7(7) . . ? C73 C74 C72 121.1(7) . . ? C76 C75 C74 122.1(8) . . ? C75 C76 C77 119.3(7) . . ? C75 C76 C79 121.2(8) . . ? C77 C76 C79 119.5(8) . . ? C76 C77 C78 120.1(7) . . ? C77 C78 C73 119.6(7) . . ? C77 C78 C83 118.1(6) . . ? C73 C78 C83 122.2(6) . . ? C82A C79 C81 139.8(12) . . ? C82A C79 C82 41.0(10) . . ? C81 C79 C82 110.3(11) . . ? C82A C79 C80A 114.1(13) . . ? C81 C79 C80A 59.2(12) . . ? C82 C79 C80A 132.2(13) . . ? C82A C79 C81A 111.9(12) . . ? C81 C79 C81A 46.0(10) . . ? C82 C79 C81A 71.5(12) . . ? C80A C79 C81A 103.4(13) . . ? C82A C79 C80 69.1(11) . . ? C81 C79 C80 108.6(10) . . ? C82 C79 C80 105.6(10) . . ? C80A C79 C80 50.8(11) . . ? C81A C79 C80 144.0(12) . . ? C82A C79 C76 108.5(10) . . ? C81 C79 C76 110.0(9) . . ? C82 C79 C76 114.1(9) . . ? C80A C79 C76 113.0(11) . . ? C81A C79 C76 105.5(10) . . ? C80 C79 C76 108.0(8) . . ? C85 C83 C78 115.9(6) . . ? O6 C84 C85 120.0(6) . . ? O6 C84 C89 118.5(6) . . ? C85 C84 C89 121.5(7) . . ? C84 C85 C86 117.9(7) . . ? C84 C85 C83 120.2(6) . . ? C86 C85 C83 121.8(7) . . ? C85 C86 C87 122.7(7) . . ? C88 C87 C86 117.2(7) . . ? C88 C87 C90 121.4(7) . . ? C86 C87 C90 121.3(7) . . ? C89 C88 C87 121.3(7) . . ? C88 C89 C84 119.2(7) . . ? C88 C89 C94 119.5(6) . . ? C84 C89 C94 121.1(6) . . ? C91 C90 C87 109.5(7) . . ? C91 C90 C93 110.1(7) . . ? C87 C90 C93 110.7(6) . . ? C91 C90 C92 107.7(8) . . ? C87 C90 C92 111.9(6) . . ? C93 C90 C92 106.9(8) . . ? C89 C94 C96 109.6(6) . . ? O7 C95 C100 120.6(6) . . ? O7 C95 C96 119.1(6) . . ? C100 C95 C96 120.2(7) . . ? C97 C96 C95 119.1(7) . . ? C97 C96 C94 120.3(7) . . ? C95 C96 C94 120.0(6) . . ? C98 C97 C96 122.6(7) . . ? C97 C98 C99 117.1(7) . . ? C97 C98 C101 123.2(7) . . ? C99 C98 C101 119.6(7) . . ? C100 C99 C98 122.9(7) . . ? C99 C100 C95 118.0(7) . . ? C99 C100 C105 120.6(6) . . ? C95 C100 C105 121.0(6) . . ? C103 C101 C102 110.2(8) . . ? C103 C101 C104 109.4(8) . . ? C102 C101 C104 108.0(8) . . ? C103 C101 C98 108.9(7) . . ? C102 C101 C98 108.9(7) . . ? C104 C101 C98 111.5(7) . . ? C107 C105 C100 115.1(6) . . ? O8 C106 C107 120.2(6) . . ? O8 C106 C111 118.9(6) . . ? C107 C106 C111 120.8(6) . . ? C106 C107 C108 118.5(6) . . ? C106 C107 C105 121.4(6) . . ? C108 C107 C105 120.1(6) . . ? C107 C108 C109 122.5(7) . . ? C110 C109 C108 116.6(7) . . ? C110 C109 C112 123.3(7) . . ? C108 C109 C112 120.0(7) . . ? C109 C110 C111 123.7(7) . . ? C110 C111 C106 117.9(6) . . ? C110 C111 C116 121.5(7) . . ? C106 C111 C116 120.5(6) . . ? C113 C112 C114 110.8(9) . . ? C113 C112 C115 108.5(8) . . ? C114 C112 C115 107.2(8) . . ? C113 C112 C109 109.4(7) . . ? C114 C112 C109 110.7(7) . . ? C115 C112 C109 110.2(7) . . ? C111 C116 C30 109.4(6) . . ? N5 C117 C118 180(2) . . ? N6 C119 C120 176.4(15) . . ? N7 C121 C122 175.7(14) . . ? N8 C123 C124 179(2) . . ? N9 C125 C126 174(6) . . ? N10 C127 C128 168(3) . . ? _diffrn_measured_fraction_theta_max 1.000 _diffrn_reflns_theta_full 25.00 _diffrn_measured_fraction_theta_full 1.000 _refine_diff_density_max 0.588 _refine_diff_density_min -0.646 _refine_diff_density_rms 0.093 #===END data_3 _database_code_CSD 173186 _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C156 H187 Mo2 N9 O10' _chemical_formula_weight 2540.03 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 P21/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 23.3956(17) _cell_length_b 31.216(2) _cell_length_c 21.2594(15) _cell_angle_alpha 90.00 _cell_angle_beta 107.908(2) _cell_angle_gamma 90.00 _cell_volume 14773.7(18) _cell_formula_units_Z 4 _cell_measurement_temperature 160(2) _cell_measurement_reflns_used 44542 _cell_measurement_theta_min 2.57 _cell_measurement_theta_max 29.17 _exptl_crystal_description needle _exptl_crystal_colour red _exptl_crystal_size_max 0.22 _exptl_crystal_size_mid 0.07 _exptl_crystal_size_min 0.05 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.142 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 5400 _exptl_absorpt_coefficient_mu 0.228 _exptl_absorpt_correction_type empirical _exptl_absorpt_correction_T_min 0.952 _exptl_absorpt_correction_T_max 0.989 _exptl_absorpt_process_details ? _exptl_special_details ; ? ; _diffrn_ambient_temperature 160(2) _diffrn_radiation_wavelength 0.68780 _diffrn_radiation_type synchrotron _diffrn_radiation_source 'Daresbury SRS Station 9.8' _diffrn_radiation_monochromator 'silicon 111' _diffrn_measurement_device_type 'Bruker SMART CCD diffractometer' _diffrn_measurement_method '\w rotation with narrow frames' _diffrn_detector_area_resol_mean ? _diffrn_standards_number 0 _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% 0 _diffrn_reflns_number 83968 _diffrn_reflns_av_R_equivalents 0.0786 _diffrn_reflns_av_sigmaI/netI 0.1016 _diffrn_reflns_limit_h_min -21 _diffrn_reflns_limit_h_max 29 _diffrn_reflns_limit_k_min -35 _diffrn_reflns_limit_k_max 39 _diffrn_reflns_limit_l_min -27 _diffrn_reflns_limit_l_max 26 _diffrn_reflns_theta_min 1.59 _diffrn_reflns_theta_max 26.00 _reflns_number_total 31474 _reflns_number_gt 18014 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'Bruker SMART' _computing_cell_refinement 'local programs' _computing_data_reduction 'Bruker SAINT' _computing_structure_solution 'Bruker SHELXTL' _computing_structure_refinement 'Bruker SHELXTL' _computing_molecular_graphics 'Bruker SHELXTL' _computing_publication_material 'SHELXTL and local programs' _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^)+(0.1030P)^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 except H9 coords freely refined' _refine_ls_hydrogen_treatment mixed _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 31474 _refine_ls_number_parameters 1741 _refine_ls_number_restraints 382 _refine_ls_R_factor_all 0.1227 _refine_ls_R_factor_gt 0.0670 _refine_ls_wR_factor_ref 0.1869 _refine_ls_wR_factor_gt 0.1624 _refine_ls_goodness_of_fit_ref 0.953 _refine_ls_restrained_S_all 0.952 _refine_ls_shift/su_max 0.020 _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 0.685583(14) 0.971029(10) 0.742609(14) 0.02284(9) Uani 1 1 d . . . Mo2 Mo 0.683088(14) 1.029714(10) 0.882755(14) 0.02271(9) Uani 1 1 d . . . O1 O 0.69018(11) 0.96479(8) 0.84074(11) 0.0247(6) Uani 1 1 d . . . O2 O 0.59994(11) 0.97466(8) 0.72258(11) 0.0243(5) Uani 1 1 d . . . O3 O 0.67127(11) 0.98914(8) 0.65224(11) 0.0251(6) Uani 1 1 d . . . O4 O 0.76773(11) 0.98563(8) 0.75072(11) 0.0274(6) Uani 1 1 d . . . O5 O 0.68819(11) 1.03586(8) 0.78888(11) 0.0253(6) Uani 1 1 d . . . O6 O 0.59775(11) 1.02453(8) 0.84485(11) 0.0240(5) Uani 1 1 d . . . O7 O 0.66889(11) 1.01211(8) 0.96407(11) 0.0255(6) Uani 1 1 d . . . O8 O 0.76652(11) 1.01683(8) 0.93111(11) 0.0252(6) Uani 1 1 d . . . C1 C 0.69027(16) 0.92312(11) 0.86597(16) 0.0212(8) Uani 1 1 d . . . C2 C 0.74481(16) 0.90491(12) 0.90073(17) 0.0239(8) Uani 1 1 d . . . C3 C 0.74502(18) 0.86243(13) 0.91998(18) 0.0327(9) Uani 1 1 d . . . H3 H 0.7822 0.8495 0.9437 0.039 Uiso 1 1 calc R . . C4 C 0.69269(19) 0.83785(12) 0.9058(2) 0.0346(10) Uani 1 1 d . A . C5 C 0.63900(18) 0.85835(12) 0.87259(17) 0.0296(9) Uani 1 1 d . . . H5 H 0.6026 0.8427 0.8635 0.036 Uiso 1 1 calc R . . C6 C 0.63654(17) 0.90068(12) 0.85217(16) 0.0253(8) Uani 1 1 d . . . C7 C 0.6933(2) 0.79102(15) 0.9279(3) 0.0553(13) Uani 1 1 d DU . . C8 C 0.7476(7) 0.7687(7) 0.9196(10) 0.065(4) Uani 0.50(2) 1 d PDU A 1 H8A H 0.7480 0.7388 0.9338 0.097 Uiso 0.50(2) 1 calc PR A 1 H8B H 0.7841 0.7831 0.9465 0.097 Uiso 0.50(2) 1 calc PR A 1 H8C H 0.7460 0.7696 0.8730 0.097 Uiso 0.50(2) 1 calc PR A 1 C9 C 0.6333(7) 0.7685(5) 0.9014(16) 0.127(10) Uani 0.50(2) 1 d PDU A 1 H9A H 0.6371 0.7389 0.9178 0.190 Uiso 0.50(2) 1 calc PR A 1 H9B H 0.6210 0.7683 0.8530 0.190 Uiso 0.50(2) 1 calc PR A 1 H9C H 0.6032 0.7836 0.9164 0.190 Uiso 0.50(2) 1 calc PR A 1 C10 C 0.7057(12) 0.7928(5) 1.0048(6) 0.087(5) Uani 0.50(2) 1 d PDU A 1 H10A H 0.7067 0.7637 1.0221 0.131 Uiso 0.50(2) 1 calc PR A 1 H10B H 0.6737 0.8092 1.0147 0.131 Uiso 0.50(2) 1 calc PR A 1 H10C H 0.7444 0.8068 1.0255 0.131 Uiso 0.50(2) 1 calc PR A 1 C8A C 0.7549(6) 0.7703(8) 0.9492(13) 0.091(7) Uani 0.50(2) 1 d PDU A 2 H8A1 H 0.7514 0.7406 0.9626 0.137 Uiso 0.50(2) 1 calc PR A 2 H8A2 H 0.7814 0.7862 0.9867 0.137 Uiso 0.50(2) 1 calc PR A 2 H8A3 H 0.7717 0.7708 0.9123 0.137 Uiso 0.50(2) 1 calc PR A 2 C9A C 0.6554(10) 0.7652(5) 0.8639(8) 0.082(6) Uani 0.50(2) 1 d PDU A 2 H9A1 H 0.6543 0.7348 0.8750 0.122 Uiso 0.50(2) 1 calc PR A 2 H9A2 H 0.6742 0.7685 0.8289 0.122 Uiso 0.50(2) 1 calc PR A 2 H9A3 H 0.6143 0.7765 0.8486 0.122 Uiso 0.50(2) 1 calc PR A 2 C10A C 0.6620(13) 0.7872(5) 0.9793(12) 0.100(6) Uani 0.50(2) 1 d PDU A 2 H10D H 0.6627 0.7573 0.9934 0.150 Uiso 0.50(2) 1 calc PR A 2 H10E H 0.6203 0.7968 0.9609 0.150 Uiso 0.50(2) 1 calc PR A 2 H10F H 0.6826 0.8051 1.0175 0.150 Uiso 0.50(2) 1 calc PR A 2 C11 C 0.57556(17) 0.92048(12) 0.81841(16) 0.0263(8) Uani 1 1 d . . . H11A H 0.5787 0.9518 0.8259 0.032 Uiso 1 1 calc R . . H11B H 0.5467 0.9093 0.8400 0.032 Uiso 1 1 calc R . . C12 C 0.56123(16) 0.94143(11) 0.69928(17) 0.0248(8) Uani 1 1 d . . . C13 C 0.54969(16) 0.91251(12) 0.74395(17) 0.0258(8) Uani 1 1 d . . . C14 C 0.51257(17) 0.87733(12) 0.71870(17) 0.0281(8) Uani 1 1 d . . . H14 H 0.5052 0.8570 0.7485 0.034 Uiso 1 1 calc R . . C15 C 0.48620(17) 0.87142(12) 0.65081(18) 0.0295(9) Uani 1 1 d . . . C16 C 0.49745(17) 0.90157(13) 0.60871(17) 0.0300(9) Uani 1 1 d . . . H16 H 0.4792 0.8980 0.5625 0.036 Uiso 1 1 calc R . . C17 C 0.53453(17) 0.93712(12) 0.63101(17) 0.0281(9) Uani 1 1 d . . . C18 C 0.44452(19) 0.83319(13) 0.62261(19) 0.0368(10) Uani 1 1 d . . . C19 C 0.4452(3) 0.79999(15) 0.6753(2) 0.0632(16) Uani 1 1 d . . . H19A H 0.4199 0.7757 0.6548 0.095 Uiso 1 1 calc R . . H19B H 0.4298 0.8129 0.7089 0.095 Uiso 1 1 calc R . . H19C H 0.4865 0.7901 0.6960 0.095 Uiso 1 1 calc R . . C20 C 0.3802(2) 0.84988(17) 0.5944(3) 0.0665(16) Uani 1 1 d . . . H20A H 0.3535 0.8262 0.5739 0.100 Uiso 1 1 calc R . . H20B H 0.3788 0.8719 0.5611 0.100 Uiso 1 1 calc R . . H20C H 0.3672 0.8623 0.6301 0.100 Uiso 1 1 calc R . . C21 C 0.4637(3) 0.81150(16) 0.5683(2) 0.0627(15) Uani 1 1 d . . . H21A H 0.5054 0.8019 0.5861 0.094 Uiso 1 1 calc R . . H21B H 0.4602 0.8319 0.5322 0.094 Uiso 1 1 calc R . . H21C H 0.4376 0.7868 0.5514 0.094 Uiso 1 1 calc R . . C22 C 0.54853(16) 0.96869(12) 0.58367(16) 0.0274(8) Uani 1 1 d . . . H22A H 0.5584 0.9969 0.6056 0.033 Uiso 1 1 calc R . . H22B H 0.5126 0.9723 0.5445 0.033 Uiso 1 1 calc R . . C23 C 0.66022(17) 0.96225(12) 0.59901(16) 0.0262(8) Uani 1 1 d . . . C24 C 0.60090(17) 0.95342(12) 0.56148(17) 0.0279(8) Uani 1 1 d . . . C25 C 0.59107(18) 0.92733(13) 0.50606(17) 0.0331(9) Uani 1 1 d . . . H25 H 0.5509 0.9219 0.4796 0.040 Uiso 1 1 calc R . . C26 C 0.63764(19) 0.90889(14) 0.48795(18) 0.0358(10) Uani 1 1 d . . . C27 C 0.69602(18) 0.91674(13) 0.52843(18) 0.0326(9) Uani 1 1 d . . . H27 H 0.7286 0.9038 0.5178 0.039 Uiso 1 1 calc R . . C28 C 0.70817(17) 0.94295(13) 0.58395(17) 0.0297(9) Uani 1 1 d . . . C29 C 0.6248(2) 0.88119(16) 0.4253(2) 0.0518(13) Uani 1 1 d . . . C30 C 0.5757(3) 0.84938(19) 0.4227(3) 0.083(2) Uani 1 1 d . . . H30A H 0.5884 0.8305 0.4613 0.125 Uiso 1 1 calc R . . H30B H 0.5677 0.8322 0.3823 0.125 Uiso 1 1 calc R . . H30C H 0.5392 0.8647 0.4226 0.125 Uiso 1 1 calc R . . C31 C 0.6805(3) 0.85828(19) 0.4198(3) 0.0698(17) Uani 1 1 d . . . H31A H 0.7105 0.8795 0.4171 0.105 Uiso 1 1 calc R . . H31B H 0.6696 0.8404 0.3800 0.105 Uiso 1 1 calc R . . H31C H 0.6972 0.8402 0.4588 0.105 Uiso 1 1 calc R . . C32 C 0.6025(3) 0.9114(2) 0.3655(2) 0.0744(18) Uani 1 1 d . . . H32A H 0.5670 0.9270 0.3682 0.112 Uiso 1 1 calc R . . H32B H 0.5921 0.8945 0.3246 0.112 Uiso 1 1 calc R . . H32C H 0.6343 0.9318 0.3656 0.112 Uiso 1 1 calc R . . C33 C 0.77198(17) 0.94586(13) 0.63032(18) 0.0299(9) Uani 1 1 d . . . H33A H 0.7742 0.9289 0.6704 0.036 Uiso 1 1 calc R . . H33B H 0.7988 0.9319 0.6084 0.036 Uiso 1 1 calc R . . C34 C 0.79268(16) 1.00795(13) 0.71106(16) 0.0265(8) Uani 1 1 d . . . C35 C 0.79662(16) 0.98988(12) 0.65219(17) 0.0274(8) Uani 1 1 d . . . C36 C 0.82476(18) 1.01319(14) 0.61415(18) 0.0343(10) Uani 1 1 d . . . H36 H 0.8278 1.0009 0.5744 0.041 Uiso 1 1 calc R . . C37 C 0.84867(19) 1.05396(14) 0.6323(2) 0.0377(10) Uani 1 1 d . . . C38 C 0.84193(18) 1.07121(13) 0.68981(18) 0.0338(9) Uani 1 1 d . . . H38 H 0.8577 1.0989 0.7033 0.041 Uiso 1 1 calc R . . C39 C 0.81324(17) 1.04964(12) 0.72817(17) 0.0281(9) Uani 1 1 d . . . C40 C 0.8819(3) 1.07856(17) 0.5931(3) 0.0603(15) Uani 1 1 d . . . C41 C 0.9468(4) 1.0855(4) 0.6362(4) 0.166(5) Uani 1 1 d . . . H41A H 0.9471 1.1011 0.6764 0.250 Uiso 1 1 calc R . . H41B H 0.9683 1.1022 0.6116 0.250 Uiso 1 1 calc R . . H41C H 0.9666 1.0577 0.6483 0.250 Uiso 1 1 calc R . . C42 C 0.8552(5) 1.1234(2) 0.5769(5) 0.156(5) Uani 1 1 d . . . H42A H 0.8518 1.1369 0.6172 0.234 Uiso 1 1 calc R . . H42B H 0.8153 1.1213 0.5442 0.234 Uiso 1 1 calc R . . H42C H 0.8814 1.1408 0.5588 0.234 Uiso 1 1 calc R . . C43 C 0.8813(4) 1.0573(2) 0.5297(3) 0.100(3) Uani 1 1 d . . . H43A H 0.8951 1.0276 0.5387 0.149 Uiso 1 1 calc R . . H43B H 0.9080 1.0727 0.5101 0.149 Uiso 1 1 calc R . . H43C H 0.8403 1.0575 0.4990 0.149 Uiso 1 1 calc R . . C44 C 0.79981(17) 1.07168(12) 0.78515(17) 0.0291(9) Uani 1 1 d . . . H44A H 0.8325 1.0921 0.8061 0.035 Uiso 1 1 calc R . . H44B H 0.7981 1.0501 0.8187 0.035 Uiso 1 1 calc R . . C45 C 0.68633(17) 1.07692(12) 0.76087(16) 0.0237(8) Uani 1 1 d . . . C46 C 0.74054(17) 1.09552(12) 0.76178(16) 0.0255(8) Uani 1 1 d . . . C47 C 0.73861(19) 1.13733(13) 0.73827(18) 0.0351(10) Uani 1 1 d . . . H47 H 0.7752 1.1506 0.7383 0.042 Uiso 1 1 calc R . . C48 C 0.6855(2) 1.16052(13) 0.71469(19) 0.0365(10) Uani 1 1 d . B . C49 C 0.63288(18) 1.13976(13) 0.71406(18) 0.0321(9) Uani 1 1 d . . . H49 H 0.5959 1.1547 0.6975 0.038 Uiso 1 1 calc R . . C50 C 0.63191(16) 1.09790(12) 0.73666(16) 0.0248(8) Uani 1 1 d . . . C51 C 0.6860(2) 1.20674(15) 0.6904(3) 0.0592(14) Uani 1 1 d DU . . C52 C 0.7285(4) 1.2336(3) 0.7428(5) 0.082(3) Uani 0.793(11) 1 d PDU B 1 H52A H 0.7679 1.2197 0.7576 0.122 Uiso 0.793(11) 1 calc PR B 1 H52B H 0.7128 1.2368 0.7803 0.122 Uiso 0.793(11) 1 calc PR B 1 H52C H 0.7324 1.2619 0.7246 0.122 Uiso 0.793(11) 1 calc PR B 1 C53 C 0.7107(5) 1.2056(3) 0.6297(4) 0.103(3) Uani 0.793(11) 1 d PDU B 1 H53A H 0.6835 1.1886 0.5941 0.154 Uiso 0.793(11) 1 calc PR B 1 H53B H 0.7507 1.1925 0.6430 0.154 Uiso 0.793(11) 1 calc PR B 1 H53C H 0.7132 1.2348 0.6140 0.154 Uiso 0.793(11) 1 calc PR B 1 C54 C 0.6243(3) 1.2256(2) 0.6648(6) 0.098(4) Uani 0.793(11) 1 d PDU B 1 H54A H 0.5988 1.2068 0.6307 0.147 Uiso 0.793(11) 1 calc PR B 1 H54B H 0.6266 1.2539 0.6458 0.147 Uiso 0.793(11) 1 calc PR B 1 H54C H 0.6071 1.2284 0.7012 0.147 Uiso 0.793(11) 1 calc PR B 1 C52A C 0.7455(9) 1.2269(10) 0.706(2) 0.086(11) Uani 0.207(11) 1 d PDU B 2 H52D H 0.7410 1.2563 0.6886 0.129 Uiso 0.207(11) 1 calc PR B 2 H52E H 0.7707 1.2104 0.6854 0.129 Uiso 0.207(11) 1 calc PR B 2 H52F H 0.7643 1.2276 0.7539 0.129 Uiso 0.207(11) 1 calc PR B 2 C53A C 0.6446(15) 1.2109(11) 0.6191(10) 0.092(11) Uani 0.207(11) 1 d PDU B 2 H53D H 0.6067 1.1960 0.6146 0.138 Uiso 0.207(11) 1 calc PR B 2 H53E H 0.6641 1.1981 0.5889 0.138 Uiso 0.207(11) 1 calc PR B 2 H53F H 0.6365 1.2413 0.6081 0.138 Uiso 0.207(11) 1 calc PR B 2 C54A C 0.6492(16) 1.2326(8) 0.7298(17) 0.093(10) Uani 0.207(11) 1 d PDU B 2 H54D H 0.6095 1.2196 0.7215 0.140 Uiso 0.207(11) 1 calc PR B 2 H54E H 0.6447 1.2624 0.7148 0.140 Uiso 0.207(11) 1 calc PR B 2 H54F H 0.6709 1.2316 0.7772 0.140 Uiso 0.207(11) 1 calc PR B 2 C55 C 0.57207(17) 1.07761(12) 0.73140(17) 0.0278(9) Uani 1 1 d . . . H55A H 0.5761 1.0463 0.7269 0.033 Uiso 1 1 calc R . . H55B H 0.5425 1.0879 0.6901 0.033 Uiso 1 1 calc R . . C56 C 0.55800(16) 1.05714(11) 0.84101(17) 0.0244(8) Uani 1 1 d . . . C57 C 0.54634(16) 1.08552(12) 0.78795(16) 0.0257(8) Uani 1 1 d . . . C58 C 0.50863(17) 1.12021(12) 0.78756(17) 0.0294(9) Uani 1 1 d . . . H58 H 0.5013 1.1404 0.7526 0.035 Uiso 1 1 calc R . . C59 C 0.48140(18) 1.12625(12) 0.83640(18) 0.0295(9) Uani 1 1 d . . . C60 C 0.49243(17) 1.09618(12) 0.88695(18) 0.0300(9) Uani 1 1 d . . . H60 H 0.4734 1.0995 0.9202 0.036 Uiso 1 1 calc R . . C61 C 0.53055(17) 1.06120(12) 0.89037(17) 0.0264(8) Uani 1 1 d . . . C62 C 0.4384(2) 1.16386(13) 0.8350(2) 0.0380(10) Uani 1 1 d . . . C63 C 0.3751(2) 1.14631(17) 0.8249(3) 0.0678(16) Uani 1 1 d . . . H63A H 0.3761 1.1258 0.8601 0.102 Uiso 1 1 calc R . . H63B H 0.3609 1.1319 0.7819 0.102 Uiso 1 1 calc R . . H63C H 0.3480 1.1700 0.8262 0.102 Uiso 1 1 calc R . . C64 C 0.4359(3) 1.19596(15) 0.7801(3) 0.0606(15) Uani 1 1 d . . . H64A H 0.4080 1.2192 0.7814 0.091 Uiso 1 1 calc R . . H64B H 0.4220 1.1815 0.7372 0.091 Uiso 1 1 calc R . . H64C H 0.4760 1.2079 0.7865 0.091 Uiso 1 1 calc R . . C65 C 0.4577(3) 1.18767(17) 0.9008(2) 0.0665(17) Uani 1 1 d . . . H65A H 0.4961 1.2021 0.9062 0.100 Uiso 1 1 calc R . . H65B H 0.4622 1.1672 0.9370 0.100 Uiso 1 1 calc R . . H65C H 0.4271 1.2090 0.9015 0.100 Uiso 1 1 calc R . . C66 C 0.54526(16) 1.03051(12) 0.94848(16) 0.0267(8) Uani 1 1 d . . . H66A H 0.5561 1.0022 0.9345 0.032 Uiso 1 1 calc R . . H66B H 0.5094 1.0267 0.9633 0.032 Uiso 1 1 calc R . . C67 C 0.65628(17) 1.03951(12) 1.00809(17) 0.0251(8) Uani 1 1 d . . . C68 C 0.59719(17) 1.04740(12) 1.00564(17) 0.0243(8) Uani 1 1 d . . . C69 C 0.58564(18) 1.07360(13) 1.05293(18) 0.0316(9) Uani 1 1 d . . . H69 H 0.5452 1.0782 1.0517 0.038 Uiso 1 1 calc R . . C70 C 0.63174(19) 1.09343(13) 1.10246(18) 0.0339(9) Uani 1 1 d . . . C71 C 0.69002(18) 1.08632(13) 1.10147(18) 0.0335(9) Uani 1 1 d . . . H71 H 0.7220 1.0999 1.1342 0.040 Uiso 1 1 calc R . . C72 C 0.70416(17) 1.06057(12) 1.05548(17) 0.0266(8) Uani 1 1 d . . . C73 C 0.6171(2) 1.12032(16) 1.1559(2) 0.0487(12) Uani 1 1 d . . . C74 C 0.6724(2) 1.1460(2) 1.1974(3) 0.081(2) Uani 1 1 d . . . H74A H 0.7036 1.1262 1.2223 0.122 Uiso 1 1 calc R . . H74B H 0.6606 1.1648 1.2282 0.122 Uiso 1 1 calc R . . H74C H 0.6880 1.1634 1.1679 0.122 Uiso 1 1 calc R . . C75 C 0.5979(3) 1.09006(19) 1.2023(3) 0.0695(17) Uani 1 1 d . . . H75A H 0.5629 1.0734 1.1769 0.104 Uiso 1 1 calc R . . H75B H 0.5875 1.1068 1.2362 0.104 Uiso 1 1 calc R . . H75C H 0.6311 1.0706 1.2236 0.104 Uiso 1 1 calc R . . C76 C 0.5662(3) 1.15187(16) 1.1244(3) 0.0617(15) Uani 1 1 d . . . H76A H 0.5784 1.1708 1.0940 0.093 Uiso 1 1 calc R . . H76B H 0.5576 1.1690 1.1590 0.093 Uiso 1 1 calc R . . H76C H 0.5302 1.1359 1.0999 0.093 Uiso 1 1 calc R . . C77 C 0.76708(17) 1.05774(12) 1.05216(17) 0.0284(9) Uani 1 1 d . . . H77A H 0.7940 1.0723 1.0916 0.034 Uiso 1 1 calc R . . H77B H 0.7691 1.0739 1.0128 0.034 Uiso 1 1 calc R . . C78 C 0.78970(15) 0.99405(12) 0.98874(16) 0.0239(8) Uani 1 1 d . . . C79 C 0.79120(16) 1.01357(12) 1.04871(17) 0.0262(8) Uani 1 1 d . . . C80 C 0.81385(17) 0.98985(13) 1.10686(17) 0.0301(9) Uani 1 1 d . . . H80 H 0.8149 1.0026 1.1478 0.036 Uiso 1 1 calc R . . C81 C 0.83486(17) 0.94819(13) 1.10686(17) 0.0298(9) Uani 1 1 d . C . C82 C 0.83326(17) 0.93034(13) 1.04618(18) 0.0303(9) Uani 1 1 d . . . H82 H 0.8482 0.9021 1.0452 0.036 Uiso 1 1 calc R . . C83 C 0.81040(16) 0.95264(12) 0.98691(17) 0.0257(8) Uani 1 1 d . . . C84 C 0.8574(2) 0.92326(14) 1.17232(18) 0.0385(10) Uani 1 1 d DU . . C85 C 0.9144(3) 0.9453(2) 1.2164(3) 0.0534(19) Uani 0.756(7) 1 d PDU C 1 H85A H 0.9055 0.9753 1.2232 0.080 Uiso 0.756(7) 1 calc PR C 1 H85B H 0.9459 0.9440 1.1949 0.080 Uiso 0.756(7) 1 calc PR C 1 H85C H 0.9283 0.9306 1.2592 0.080 Uiso 0.756(7) 1 calc PR C 1 C86 C 0.8100(3) 0.9248(2) 1.2079(3) 0.0512(18) Uani 0.756(7) 1 d PDU C 1 H86A H 0.8008 0.9547 1.2150 0.077 Uiso 0.756(7) 1 calc PR C 1 H86B H 0.8253 0.9102 1.2507 0.077 Uiso 0.756(7) 1 calc PR C 1 H86C H 0.7735 0.9104 1.1809 0.077 Uiso 0.756(7) 1 calc PR C 1 C87 C 0.8714(3) 0.87735(19) 1.1624(3) 0.0527(19) Uani 0.756(7) 1 d PDU C 1 H87A H 0.9020 0.8760 1.1398 0.079 Uiso 0.756(7) 1 calc PR C 1 H87B H 0.8348 0.8629 1.1356 0.079 Uiso 0.756(7) 1 calc PR C 1 H87C H 0.8864 0.8631 1.2055 0.079 Uiso 0.756(7) 1 calc PR C 1 C85A C 0.8595(12) 0.9481(7) 1.2341(7) 0.073(7) Uani 0.244(7) 1 d PDU C 2 H85D H 0.8194 0.9593 1.2301 0.109 Uiso 0.244(7) 1 calc PR C 2 H85E H 0.8878 0.9719 1.2396 0.109 Uiso 0.244(7) 1 calc PR C 2 H85F H 0.8725 0.9291 1.2726 0.109 Uiso 0.244(7) 1 calc PR C 2 C86A C 0.8167(9) 0.8826(6) 1.1688(10) 0.069(7) Uani 0.244(7) 1 d PDU C 2 H86D H 0.7757 0.8916 1.1650 0.103 Uiso 0.244(7) 1 calc PR C 2 H86E H 0.8328 0.8654 1.2090 0.103 Uiso 0.244(7) 1 calc PR C 2 H86F H 0.8163 0.8653 1.1301 0.103 Uiso 0.244(7) 1 calc PR C 2 C87A C 0.9190(7) 0.9057(6) 1.1787(8) 0.049(5) Uani 0.244(7) 1 d PDU C 2 H87D H 0.9175 0.8891 1.1391 0.073 Uiso 0.244(7) 1 calc PR C 2 H87E H 0.9322 0.8872 1.2177 0.073 Uiso 0.244(7) 1 calc PR C 2 H87F H 0.9474 0.9295 1.1834 0.073 Uiso 0.244(7) 1 calc PR C 2 C88 C 0.80277(17) 0.93053(12) 0.92152(16) 0.0250(8) Uani 1 1 d . . . H88A H 0.8372 0.9112 0.9256 0.030 Uiso 1 1 calc R . . H88B H 0.8021 0.9522 0.8873 0.030 Uiso 1 1 calc R . . N1 N 0.69014(13) 0.91692(10) 0.72897(13) 0.0239(7) Uani 1 1 d . . . C89 C 0.69485(17) 0.87322(12) 0.71810(18) 0.0278(8) Uani 1 1 d . . . C90 C 0.64421(19) 0.85152(13) 0.6782(2) 0.0393(10) Uani 1 1 d . . . H90 H 0.6077 0.8666 0.6587 0.047 Uiso 1 1 calc R . . C91 C 0.6477(2) 0.80858(15) 0.6676(3) 0.0585(15) Uani 1 1 d . . . H91 H 0.6135 0.7938 0.6403 0.070 Uiso 1 1 calc R . . C92 C 0.7004(2) 0.78634(16) 0.6962(3) 0.0620(15) Uani 1 1 d . . . H92 H 0.7022 0.7563 0.6898 0.074 Uiso 1 1 calc R . . C93 C 0.7505(2) 0.80821(15) 0.7341(2) 0.0481(12) Uani 1 1 d . . . H93 H 0.7867 0.7927 0.7530 0.058 Uiso 1 1 calc R . . C94 C 0.74994(18) 0.85148(13) 0.74528(18) 0.0321(9) Uani 1 1 d . . . C95 C 0.80626(17) 0.87428(13) 0.78427(18) 0.0329(9) Uani 1 1 d . . . H95A H 0.8187 0.8634 0.8302 0.039 Uiso 1 1 calc R . . H95B H 0.7975 0.9052 0.7857 0.039 Uiso 1 1 calc R . . C96 C 0.85866(18) 0.86859(15) 0.75552(19) 0.0387(10) Uani 1 1 d . . . H96A H 0.8698 0.8379 0.7569 0.046 Uiso 1 1 calc R . . H96B H 0.8459 0.8779 0.7088 0.046 Uiso 1 1 calc R . . C97 C 0.91245(19) 0.89448(15) 0.7943(2) 0.0390(10) Uani 1 1 d . . . C98 C 0.9266(2) 0.93237(17) 0.7708(2) 0.0576(14) Uani 1 1 d . . . H98 H 0.9029 0.9424 0.7287 0.069 Uiso 1 1 calc R . . C99 C 0.9754(3) 0.95663(18) 0.8076(3) 0.0660(16) Uani 1 1 d . . . H99 H 0.9851 0.9827 0.7903 0.079 Uiso 1 1 calc R . . C100 C 1.0091(2) 0.94278(18) 0.8688(3) 0.0663(16) Uani 1 1 d . . . H100 H 1.0431 0.9589 0.8933 0.080 Uiso 1 1 calc R . . C101 C 0.9941(2) 0.90562(17) 0.8950(2) 0.0580(14) Uani 1 1 d . . . H101 H 1.0167 0.8968 0.9383 0.070 Uiso 1 1 calc R . . C102 C 0.94576(19) 0.88091(15) 0.8582(2) 0.0415(11) Uani 1 1 d . . . N2 N 0.93162(16) 0.84083(12) 0.88004(17) 0.0427(9) Uani 1 1 d . . . C103 C 0.9354(2) 0.83217(15) 0.9409(2) 0.0444(11) Uani 1 1 d . . . H103 H 0.9471 0.8542 0.9733 0.053 Uiso 1 1 calc R . . C104 C 0.9223(2) 0.79051(15) 0.9605(2) 0.0446(11) Uani 1 1 d . . . C105 C 0.9061(2) 0.75641(16) 0.9138(2) 0.0514(13) Uani 1 1 d . . . C106 C 0.8940(2) 0.71567(17) 0.9332(3) 0.0595(14) Uani 1 1 d . . . C107 C 0.8964(2) 0.71058(17) 0.9978(3) 0.0592(14) Uani 1 1 d . . . H107 H 0.8883 0.6828 1.0112 0.071 Uiso 1 1 calc R . . C108 C 0.9098(2) 0.74310(17) 1.0462(2) 0.0527(13) Uani 1 1 d . . . C109 C 0.9230(2) 0.78277(16) 1.0259(2) 0.0475(12) Uani 1 1 d . . . H109 H 0.9329 0.8056 1.0570 0.057 Uiso 1 1 calc R . . O9 O 0.90298(19) 0.76345(11) 0.85018(17) 0.0641(10) Uani 1 1 d D . . H9 H 0.915(3) 0.7905(9) 0.855(3) 0.096 Uiso 1 1 d D . . C110 C 0.8791(4) 0.67845(19) 0.8834(3) 0.083(2) Uani 1 1 d . . . C111 C 0.8673(5) 0.6370(2) 0.9160(4) 0.140(4) Uani 1 1 d . . . H11C H 0.9050 0.6266 0.9470 0.210 Uiso 1 1 calc R . . H11D H 0.8510 0.6153 0.8819 0.210 Uiso 1 1 calc R . . H11E H 0.8384 0.6426 0.9399 0.210 Uiso 1 1 calc R . . C112 C 0.9313(4) 0.6699(2) 0.8568(3) 0.102(3) Uani 1 1 d . . . H11F H 0.9365 0.6945 0.8303 0.154 Uiso 1 1 calc R . . H11G H 0.9230 0.6442 0.8292 0.154 Uiso 1 1 calc R . . H11H H 0.9681 0.6657 0.8938 0.154 Uiso 1 1 calc R . . C113 C 0.8216(3) 0.6879(2) 0.8265(4) 0.107(3) Uani 1 1 d . . . H11I H 0.7899 0.6973 0.8447 0.161 Uiso 1 1 calc R . . H11J H 0.8085 0.6619 0.8002 0.161 Uiso 1 1 calc R . . H11K H 0.8295 0.7106 0.7984 0.161 Uiso 1 1 calc R . . C114 C 0.9080(3) 0.73337(18) 1.1161(3) 0.0606(14) Uani 1 1 d . . . C115 C 0.8442(3) 0.7180(3) 1.1121(3) 0.109(3) Uani 1 1 d . . . H11L H 0.8355 0.6911 1.0873 0.163 Uiso 1 1 calc R . . H11M H 0.8149 0.7398 1.0897 0.163 Uiso 1 1 calc R . . H11N H 0.8419 0.7135 1.1569 0.163 Uiso 1 1 calc R . . C116 C 0.9237(3) 0.7724(2) 1.1607(3) 0.091(2) Uani 1 1 d . . . H11O H 0.9196 0.7654 1.2040 0.137 Uiso 1 1 calc R . . H11P H 0.8964 0.7959 1.1409 0.137 Uiso 1 1 calc R . . H11Q H 0.9652 0.7811 1.1659 0.137 Uiso 1 1 calc R . . C117 C 0.9524(3) 0.69816(19) 1.1483(3) 0.0775(18) Uani 1 1 d . . . H11R H 0.9504 0.6926 1.1930 0.116 Uiso 1 1 calc R . . H11S H 0.9932 0.7072 1.1509 0.116 Uiso 1 1 calc R . . H11T H 0.9423 0.6719 1.1219 0.116 Uiso 1 1 calc R . . N3 N 0.68495(13) 1.08385(10) 0.89887(13) 0.0231(7) Uani 1 1 d . . . C118 C 0.68816(18) 1.12721(12) 0.91601(17) 0.0287(9) Uani 1 1 d . . . C119 C 0.6394(2) 1.14681(13) 0.9284(2) 0.0397(10) Uani 1 1 d . . . H119 H 0.6040 1.1308 0.9248 0.048 Uiso 1 1 calc R . . C120 C 0.6424(2) 1.18927(16) 0.9458(3) 0.0586(14) Uani 1 1 d . . . H120 H 0.6090 1.2027 0.9540 0.070 Uiso 1 1 calc R . . C121 C 0.6939(3) 1.21238(16) 0.9513(3) 0.0603(15) Uani 1 1 d . . . H121 H 0.6959 1.2417 0.9636 0.072 Uiso 1 1 calc R . . C122 C 0.7424(2) 1.19321(15) 0.9391(2) 0.0495(13) Uani 1 1 d . . . H122 H 0.7771 1.2099 0.9423 0.059 Uiso 1 1 calc R . . C123 C 0.74215(19) 1.15014(13) 0.92234(18) 0.0338(10) Uani 1 1 d . . . C124 C 0.79430(18) 1.12984(13) 0.90960(18) 0.0349(10) Uani 1 1 d . . . H12A H 0.8023 1.1451 0.8723 0.042 Uiso 1 1 calc R . . H12B H 0.7832 1.1000 0.8950 0.042 Uiso 1 1 calc R . . C125 C 0.8534(2) 1.12858(15) 0.96783(18) 0.0420(12) Uani 1 1 d . . . H12C H 0.8683 1.1581 0.9798 0.050 Uiso 1 1 calc R . . H12D H 0.8461 1.1152 1.0069 0.050 Uiso 1 1 calc R . . C126 C 0.89953(19) 1.10311(15) 0.9479(2) 0.0411(11) Uani 1 1 d . . . C127 C 0.9062(2) 1.05964(16) 0.9616(2) 0.0501(13) Uani 1 1 d . . . H127 H 0.8824 1.0463 0.9851 0.060 Uiso 1 1 calc R . . C128 C 0.9467(3) 1.03550(18) 0.9417(3) 0.0655(16) Uani 1 1 d . . . H128 H 0.9502 1.0057 0.9508 0.079 Uiso 1 1 calc R . . C129 C 0.9820(3) 1.0545(2) 0.9086(3) 0.0746(17) Uani 1 1 d . . . H129 H 1.0115 1.0381 0.8970 0.090 Uiso 1 1 calc R . . C130 C 0.9748(2) 1.09742(18) 0.8922(3) 0.0636(15) Uani 1 1 d . . . H130 H 0.9984 1.1104 0.8682 0.076 Uiso 1 1 calc R . . C131 C 0.9327(2) 1.12157(15) 0.9110(2) 0.0443(11) Uani 1 1 d . . . N4 N 0.92150(17) 1.16482(12) 0.89269(17) 0.0435(9) Uani 1 1 d . . . C132 C 0.9177(2) 1.17699(15) 0.8339(2) 0.0458(11) Uani 1 1 d . . . H132 H 0.9244 1.1565 0.8039 0.055 Uiso 1 1 calc R . . C133 C 0.9036(2) 1.22057(15) 0.8114(2) 0.0425(11) Uani 1 1 d . . . C134 C 0.8911(2) 1.25211(17) 0.8520(2) 0.0500(12) Uani 1 1 d . . . C135 C 0.8760(2) 1.29388(17) 0.8290(3) 0.0562(13) Uani 1 1 d . . . C136 C 0.8752(2) 1.30207(17) 0.7652(3) 0.0559(14) Uani 1 1 d . . . H136 H 0.8659 1.3304 0.7492 0.067 Uiso 1 1 calc R . . C137 C 0.8870(2) 1.27212(18) 0.7222(2) 0.0563(14) Uani 1 1 d . . . C138 C 0.9013(2) 1.23078(16) 0.7468(2) 0.0519(13) Uani 1 1 d . . . H138 H 0.9096 1.2093 0.7192 0.062 Uiso 1 1 calc R . . O10 O 0.89207(19) 1.24189(12) 0.91451(16) 0.0630(10) Uani 1 1 d . . . H10 H 0.9024 1.2162 0.9223 0.094 Uiso 1 1 calc R . . C139 C 0.8631(3) 1.32912(19) 0.8739(3) 0.0767(18) Uani 1 1 d . . . C140 C 0.8505(4) 1.3722(2) 0.8370(4) 0.116(3) Uani 1 1 d . . . H14A H 0.8858 1.3808 0.8244 0.174 Uiso 1 1 calc R . . H14B H 0.8420 1.3941 0.8660 0.174 Uiso 1 1 calc R . . H14C H 0.8158 1.3692 0.7973 0.174 Uiso 1 1 calc R . . C141 C 0.8088(3) 1.3166(2) 0.8952(4) 0.106(3) Uani 1 1 d . . . H14D H 0.7748 1.3101 0.8560 0.159 Uiso 1 1 calc R . . H14E H 0.7982 1.3403 0.9196 0.159 Uiso 1 1 calc R . . H14F H 0.8186 1.2912 0.9237 0.159 Uiso 1 1 calc R . . C142 C 0.9202(3) 1.3354(2) 0.9346(3) 0.088(2) Uani 1 1 d . . . H14G H 0.9292 1.3088 0.9601 0.132 Uiso 1 1 calc R . . H14H H 0.9131 1.3585 0.9626 0.132 Uiso 1 1 calc R . . H14I H 0.9543 1.3431 0.9192 0.132 Uiso 1 1 calc R . . C143 C 0.8847(3) 1.2848(2) 0.6517(3) 0.0741(18) Uani 1 1 d . . . C144 C 0.8829(6) 1.2483(3) 0.6087(3) 0.183(6) Uani 1 1 d . . . H14J H 0.8715 1.2580 0.5626 0.274 Uiso 1 1 calc R . . H14K H 0.8534 1.2274 0.6140 0.274 Uiso 1 1 calc R . . H14L H 0.9227 1.2349 0.6205 0.274 Uiso 1 1 calc R . . C145 C 0.8237(4) 1.3087(3) 0.6197(3) 0.130(3) Uani 1 1 d . . . H14M H 0.8200 1.3325 0.6482 0.194 Uiso 1 1 calc R . . H14N H 0.7903 1.2887 0.6146 0.194 Uiso 1 1 calc R . . H14O H 0.8226 1.3198 0.5762 0.194 Uiso 1 1 calc R . . C146 C 0.9325(4) 1.3159(3) 0.6531(4) 0.132(4) Uani 1 1 d . . . H14P H 0.9718 1.3025 0.6729 0.198 Uiso 1 1 calc R . . H14Q H 0.9288 1.3409 0.6795 0.198 Uiso 1 1 calc R . . H14R H 0.9288 1.3250 0.6079 0.198 Uiso 1 1 calc R . . N5 N 0.6878(6) 0.9648(5) 0.2726(6) 0.292(8) Uani 1 1 d DU . . C147 C 0.6618(5) 0.9728(3) 0.2205(4) 0.129(3) Uani 1 1 d DU . . C148 C 0.6298(5) 0.9798(3) 0.1552(4) 0.148(4) Uani 1 1 d DU . . H14S H 0.6249 0.9527 0.1309 0.222 Uiso 1 1 calc R . . H14T H 0.6516 1.0002 0.1360 0.222 Uiso 1 1 calc R . . H14U H 0.5903 0.9915 0.1523 0.222 Uiso 1 1 calc R . . N6 N 0.5724(2) 1.08513(16) 0.56207(19) 0.0692(14) Uani 1 1 d DU . . C149 C 0.6216(2) 1.08199(16) 0.5698(2) 0.0487(12) Uani 1 1 d DU . . C150 C 0.6853(2) 1.07867(18) 0.5790(2) 0.0621(15) Uani 1 1 d DU . . H15A H 0.6925 1.0814 0.5362 0.093 Uiso 1 1 calc R . . H15B H 0.7000 1.0508 0.5986 0.093 Uiso 1 1 calc R . . H15C H 0.7065 1.1016 0.6085 0.093 Uiso 1 1 calc R . . N7 N 0.56858(19) 0.91333(16) 0.9802(2) 0.0645(13) Uani 1 1 d DU . . C151 C 0.6183(2) 0.91534(15) 1.0042(2) 0.0436(11) Uani 1 1 d DU . . C152 C 0.6823(2) 0.91701(17) 1.0350(2) 0.0531(13) Uani 1 1 d DU . . H15D H 0.6928 0.9022 1.0777 0.080 Uiso 1 1 calc R . . H15E H 0.6953 0.9470 1.0419 0.080 Uiso 1 1 calc R . . H15F H 0.7025 0.9030 1.0064 0.080 Uiso 1 1 calc R . . N8 N 0.9013(10) 0.9871(8) 0.3931(14) 0.227(12) Uani 0.50 1 d PDU . . C153 C 0.8553(10) 0.9808(7) 0.3947(11) 0.143(8) Uani 0.50 1 d PDU . . C154 C 0.8048(7) 0.9676(4) 0.4118(7) 0.101(5) Uani 0.50 1 d PDU . . H15G H 0.7815 0.9927 0.4166 0.152 Uiso 0.50 1 calc PR . . H15H H 0.8178 0.9518 0.4537 0.152 Uiso 0.50 1 calc PR . . H15I H 0.7799 0.9489 0.3770 0.152 Uiso 0.50 1 calc PR . . N9 N 0.2774(6) 0.9435(5) 0.5837(10) 0.271(8) Uani 1 1 d DU . . C155 C 0.3230(7) 0.9569(4) 0.5938(8) 0.180(6) Uani 1 1 d DU . . C156 C 0.3810(7) 0.9748(4) 0.6155(10) 0.289(11) Uani 1 1 d DU . . H15J H 0.3818 0.9983 0.6462 0.433 Uiso 1 1 calc R . . H15K H 0.3917 0.9857 0.5773 0.433 Uiso 1 1 calc R . . H15L H 0.4100 0.9528 0.6380 0.433 Uiso 1 1 calc R . . N10 N 0.8936(6) 0.5857(4) 1.0672(6) 0.083(3) Uani 0.50 1 d PDU . . C157 C 0.9384(6) 0.5726(4) 1.0869(8) 0.085(4) Uani 0.50 1 d PDU . . C158 C 0.9969(7) 0.5559(6) 1.1105(16) 0.217(12) Uani 0.50 1 d PDU . . 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 0.01733(17) 0.02916(18) 0.01723(14) -0.00174(13) -0.00175(12) -0.00239(14) Mo2 0.01876(17) 0.02770(18) 0.01640(14) -0.00037(13) -0.00233(12) -0.00046(14) O1 0.0221(14) 0.0283(14) 0.0194(11) 0.0022(10) -0.0002(10) -0.0032(11) O2 0.0161(13) 0.0271(14) 0.0235(12) -0.0019(10) -0.0030(10) -0.0016(11) O3 0.0233(14) 0.0321(14) 0.0163(11) -0.0021(10) 0.0010(10) -0.0036(11) O4 0.0203(14) 0.0348(15) 0.0198(12) -0.0023(11) -0.0046(10) -0.0040(11) O5 0.0210(14) 0.0302(15) 0.0197(12) 0.0028(10) -0.0011(10) -0.0050(11) O6 0.0189(13) 0.0285(14) 0.0194(11) -0.0008(10) -0.0017(10) 0.0007(11) O7 0.0239(14) 0.0318(14) 0.0158(11) -0.0008(10) -0.0015(10) 0.0009(11) O8 0.0196(14) 0.0347(15) 0.0173(11) 0.0000(10) -0.0003(10) 0.0012(11) C1 0.0145(18) 0.029(2) 0.0171(16) -0.0035(14) 0.0004(14) 0.0030(14) C2 0.0174(19) 0.029(2) 0.0228(17) -0.0039(15) 0.0026(15) 0.0008(15) C3 0.022(2) 0.037(2) 0.031(2) 0.0018(17) -0.0039(17) 0.0045(17) C4 0.032(2) 0.027(2) 0.039(2) 0.0025(17) 0.0029(19) -0.0010(18) C5 0.025(2) 0.030(2) 0.0284(19) -0.0003(16) -0.0008(16) -0.0053(16) C6 0.020(2) 0.033(2) 0.0185(16) -0.0031(15) -0.0004(15) 0.0003(16) C7 0.041(3) 0.034(3) 0.078(3) 0.013(2) -0.001(3) -0.002(2) C8 0.077(9) 0.023(6) 0.088(11) 0.015(8) 0.015(8) 0.017(7) C9 0.057(8) 0.044(9) 0.23(2) 0.060(12) -0.021(11) -0.025(7) C10 0.112(15) 0.061(9) 0.103(7) 0.055(7) 0.053(8) 0.015(9) C8A 0.052(7) 0.061(10) 0.131(19) 0.032(13) -0.014(8) 0.004(6) C9A 0.073(11) 0.032(6) 0.105(9) 0.006(7) -0.022(7) -0.020(7) C10A 0.127(16) 0.059(9) 0.131(13) 0.031(9) 0.065(13) -0.021(10) C11 0.020(2) 0.031(2) 0.0227(17) 0.0004(15) -0.0011(15) -0.0033(16) C12 0.0146(18) 0.028(2) 0.0263(18) -0.0033(15) -0.0018(15) -0.0019(15) C13 0.0173(19) 0.032(2) 0.0224(17) -0.0022(15) -0.0018(15) 0.0031(16) C14 0.021(2) 0.033(2) 0.0260(18) 0.0010(16) 0.0016(16) -0.0008(16) C15 0.024(2) 0.029(2) 0.0281(19) -0.0059(16) -0.0029(16) -0.0007(16) C16 0.019(2) 0.041(2) 0.0211(17) -0.0053(16) -0.0066(15) -0.0015(17) C17 0.019(2) 0.036(2) 0.0235(18) 0.0012(16) -0.0022(15) 0.0004(16) C18 0.031(2) 0.038(2) 0.033(2) -0.0044(18) -0.0034(18) -0.0106(19) C19 0.074(4) 0.044(3) 0.053(3) 0.001(2) -0.007(3) -0.027(3) C20 0.031(3) 0.063(4) 0.083(4) -0.006(3) -0.015(3) -0.018(2) C21 0.070(4) 0.055(3) 0.059(3) -0.027(3) 0.013(3) -0.023(3) C22 0.0154(18) 0.038(2) 0.0203(16) -0.0012(16) -0.0074(14) -0.0001(17) C23 0.022(2) 0.033(2) 0.0176(16) -0.0010(14) -0.0025(15) -0.0043(16) C24 0.024(2) 0.033(2) 0.0205(17) -0.0006(15) -0.0015(15) -0.0007(16) C25 0.020(2) 0.048(3) 0.0228(18) -0.0056(17) -0.0058(16) -0.0061(18) C26 0.031(2) 0.044(3) 0.0270(19) -0.0118(18) 0.0008(18) -0.0057(19) C27 0.026(2) 0.041(2) 0.0274(19) -0.0062(17) 0.0031(17) -0.0014(18) C28 0.021(2) 0.039(2) 0.0236(18) -0.0026(16) -0.0016(16) -0.0049(17) C29 0.043(3) 0.067(3) 0.040(2) -0.029(2) 0.003(2) -0.015(2) C30 0.077(5) 0.087(5) 0.088(4) -0.055(4) 0.028(4) -0.037(4) C31 0.056(4) 0.087(4) 0.063(3) -0.049(3) 0.012(3) -0.004(3) C32 0.074(4) 0.104(5) 0.034(3) -0.021(3) 0.000(3) -0.005(4) C33 0.019(2) 0.042(2) 0.0257(18) -0.0060(17) 0.0015(16) 0.0029(17) C34 0.0131(18) 0.043(2) 0.0182(16) 0.0038(16) -0.0034(14) -0.0008(16) C35 0.0150(19) 0.037(2) 0.0239(18) 0.0001(16) -0.0031(15) -0.0021(16) C36 0.025(2) 0.053(3) 0.0230(18) -0.0025(18) 0.0042(17) -0.0015(19) C37 0.031(2) 0.048(3) 0.033(2) 0.0042(19) 0.0075(19) -0.006(2) C38 0.027(2) 0.041(2) 0.030(2) 0.0006(17) 0.0022(17) -0.0106(18) C39 0.0172(19) 0.038(2) 0.0215(17) 0.0007(16) -0.0051(15) -0.0025(16) C40 0.072(4) 0.064(4) 0.057(3) -0.003(3) 0.038(3) -0.023(3) C41 0.108(8) 0.294(13) 0.106(6) -0.020(7) 0.046(6) -0.127(9) C42 0.317(15) 0.051(4) 0.182(9) 0.026(5) 0.196(10) 0.002(6) C43 0.163(8) 0.074(4) 0.098(5) -0.006(4) 0.094(5) -0.033(5) C44 0.025(2) 0.034(2) 0.0221(17) -0.0014(15) -0.0023(16) -0.0079(17) C45 0.024(2) 0.030(2) 0.0156(16) -0.0041(14) 0.0033(15) -0.0021(16) C46 0.023(2) 0.031(2) 0.0153(16) -0.0010(14) -0.0042(15) -0.0052(16) C47 0.028(2) 0.038(2) 0.030(2) 0.0031(17) -0.0048(17) -0.0125(18) C48 0.035(3) 0.033(2) 0.031(2) 0.0054(17) -0.0048(18) -0.0042(19) C49 0.025(2) 0.037(2) 0.0267(19) 0.0038(17) -0.0030(16) 0.0002(17) C50 0.0188(19) 0.036(2) 0.0155(16) 0.0004(15) -0.0011(14) 0.0005(16) C51 0.048(3) 0.042(3) 0.070(3) 0.026(2) -0.008(3) -0.007(2) C52 0.066(6) 0.031(4) 0.119(7) 0.009(5) -0.014(5) -0.005(4) C53 0.138(10) 0.069(6) 0.097(6) 0.051(4) 0.028(6) -0.012(5) C54 0.054(5) 0.045(5) 0.152(10) 0.050(6) -0.031(5) -0.006(3) C52A 0.060(12) 0.027(17) 0.15(3) 0.047(19) 0.004(13) -0.002(11) C53A 0.09(2) 0.09(2) 0.080(12) 0.056(15) -0.005(12) -0.002(18) C54A 0.12(3) 0.032(15) 0.14(2) 0.023(15) 0.05(2) 0.008(15) C55 0.020(2) 0.034(2) 0.0211(17) 0.0051(15) -0.0064(15) 0.0026(16) C56 0.0192(19) 0.0226(19) 0.0233(17) -0.0037(14) -0.0053(15) -0.0003(15) C57 0.0186(19) 0.033(2) 0.0194(16) -0.0023(15) -0.0032(15) -0.0022(16) C58 0.026(2) 0.032(2) 0.0230(18) 0.0008(16) -0.0033(16) 0.0021(17) C59 0.025(2) 0.029(2) 0.0287(19) -0.0027(16) -0.0011(16) 0.0023(16) C60 0.024(2) 0.037(2) 0.0269(18) -0.0037(16) 0.0033(16) 0.0017(17) C61 0.025(2) 0.028(2) 0.0214(17) 0.0022(15) -0.0006(16) 0.0001(16) C62 0.039(3) 0.039(2) 0.033(2) 0.0006(18) 0.0067(19) 0.012(2) C63 0.039(3) 0.061(4) 0.100(4) 0.011(3) 0.017(3) 0.019(3) C64 0.074(4) 0.045(3) 0.064(3) 0.013(2) 0.023(3) 0.025(3) C65 0.081(4) 0.060(3) 0.048(3) -0.011(2) 0.004(3) 0.031(3) C66 0.0194(19) 0.033(2) 0.0229(17) 0.0002(16) -0.0004(15) -0.0033(16) C67 0.0184(19) 0.030(2) 0.0210(17) 0.0043(14) -0.0025(15) 0.0022(15) C68 0.020(2) 0.026(2) 0.0221(17) 0.0056(15) 0.0004(15) -0.0015(15) C69 0.024(2) 0.039(2) 0.0290(19) 0.0011(17) 0.0050(17) 0.0057(17) C70 0.028(2) 0.039(2) 0.030(2) -0.0084(17) 0.0030(17) 0.0021(18) C71 0.026(2) 0.041(2) 0.0251(18) -0.0090(17) -0.0040(17) 0.0029(18) C72 0.020(2) 0.032(2) 0.0218(17) -0.0011(15) -0.0037(15) 0.0024(16) C73 0.033(3) 0.065(3) 0.045(3) -0.022(2) 0.007(2) 0.006(2) C74 0.045(3) 0.112(5) 0.080(4) -0.071(4) 0.010(3) -0.001(3) C75 0.071(4) 0.093(4) 0.050(3) -0.010(3) 0.027(3) 0.019(3) C76 0.062(4) 0.056(3) 0.062(3) -0.023(3) 0.012(3) 0.016(3) C77 0.019(2) 0.037(2) 0.0225(17) -0.0023(16) -0.0033(15) -0.0043(16) C78 0.0105(17) 0.036(2) 0.0212(17) 0.0055(15) -0.0012(14) 0.0007(15) C79 0.0142(19) 0.038(2) 0.0219(17) -0.0026(15) -0.0015(15) -0.0014(16) C80 0.024(2) 0.043(2) 0.0167(16) 0.0002(16) -0.0024(15) -0.0012(18) C81 0.018(2) 0.045(2) 0.0214(18) 0.0065(17) -0.0017(15) 0.0056(17) C82 0.020(2) 0.036(2) 0.0299(19) 0.0024(16) -0.0004(16) 0.0039(16) C83 0.0163(19) 0.036(2) 0.0212(17) -0.0008(15) 0.0011(15) -0.0026(16) C84 0.033(2) 0.050(3) 0.0254(19) 0.0109(18) -0.0017(17) 0.0077(19) C85 0.040(4) 0.074(5) 0.032(3) 0.010(3) -0.010(3) 0.005(3) C86 0.049(4) 0.068(5) 0.036(3) 0.019(3) 0.014(3) 0.011(3) C87 0.062(5) 0.055(4) 0.035(3) 0.015(3) 0.005(3) 0.013(3) C85A 0.10(2) 0.096(14) 0.021(8) 0.028(7) 0.008(10) 0.047(12) C86A 0.047(11) 0.087(13) 0.066(13) 0.050(10) 0.008(11) 0.004(9) C87A 0.035(8) 0.070(14) 0.031(9) 0.013(9) -0.004(8) 0.007(8) C88 0.020(2) 0.030(2) 0.0217(17) -0.0017(15) 0.0022(15) 0.0016(15) N1 0.0128(15) 0.0392(19) 0.0155(13) -0.0027(13) -0.0017(12) -0.0028(13) C89 0.019(2) 0.030(2) 0.0311(19) -0.0043(16) 0.0026(16) -0.0006(16) C90 0.023(2) 0.037(2) 0.049(2) -0.008(2) -0.0031(19) 0.0011(18) C91 0.028(3) 0.045(3) 0.087(4) -0.022(3) -0.004(3) -0.001(2) C92 0.047(3) 0.033(3) 0.099(4) -0.016(3) 0.012(3) -0.002(2) C93 0.029(3) 0.043(3) 0.066(3) -0.002(2) 0.005(2) 0.009(2) C94 0.023(2) 0.037(2) 0.031(2) -0.0037(17) 0.0010(17) 0.0047(17) C95 0.022(2) 0.041(2) 0.0289(19) -0.0049(17) -0.0023(17) 0.0067(17) C96 0.023(2) 0.058(3) 0.027(2) -0.0074(19) -0.0041(17) 0.0038(19) C97 0.023(2) 0.053(3) 0.034(2) -0.002(2) 0.0002(18) 0.004(2) C98 0.040(3) 0.070(4) 0.050(3) 0.010(3) -0.005(2) -0.001(3) C99 0.055(4) 0.069(4) 0.061(3) 0.013(3) -0.002(3) -0.014(3) C100 0.046(3) 0.067(4) 0.064(3) 0.006(3) -0.014(3) -0.015(3) C101 0.046(3) 0.061(3) 0.046(3) 0.000(2) -0.018(2) -0.002(3) C102 0.025(2) 0.049(3) 0.039(2) -0.005(2) -0.0064(19) 0.003(2) N2 0.030(2) 0.052(2) 0.0336(19) -0.0021(17) -0.0090(16) 0.0049(17) C103 0.027(2) 0.052(3) 0.041(2) -0.005(2) -0.009(2) 0.004(2) C104 0.029(3) 0.055(3) 0.039(2) -0.002(2) -0.0060(19) 0.006(2) C105 0.040(3) 0.053(3) 0.051(3) -0.001(2) 0.000(2) 0.011(2) C106 0.050(3) 0.052(3) 0.063(3) -0.003(3) -0.003(3) 0.009(3) C107 0.043(3) 0.050(3) 0.075(4) 0.003(3) 0.003(3) 0.009(2) C108 0.035(3) 0.062(3) 0.054(3) 0.012(3) 0.003(2) 0.011(2) C109 0.032(3) 0.055(3) 0.048(3) -0.001(2) 0.002(2) 0.006(2) O9 0.074(3) 0.061(2) 0.0439(19) -0.0131(18) -0.0024(18) 0.005(2) C110 0.107(6) 0.047(4) 0.077(4) -0.013(3) 0.001(4) 0.004(4) C111 0.214(12) 0.053(5) 0.125(7) -0.018(4) 0.009(7) -0.014(5) C112 0.116(7) 0.082(5) 0.092(5) -0.026(4) 0.008(5) 0.039(4) C113 0.099(6) 0.079(5) 0.107(5) -0.040(4) -0.025(5) -0.004(4) C114 0.049(3) 0.070(4) 0.063(3) 0.015(3) 0.017(3) 0.012(3) C115 0.053(4) 0.174(8) 0.099(5) 0.073(5) 0.022(4) 0.021(5) C116 0.116(6) 0.108(6) 0.057(4) 0.014(4) 0.037(4) 0.023(5) C117 0.061(4) 0.092(5) 0.067(4) 0.022(3) 0.001(3) 0.018(3) N3 0.0148(16) 0.0323(18) 0.0161(13) 0.0024(12) -0.0039(12) 0.0021(13) C118 0.024(2) 0.032(2) 0.0211(17) 0.0028(15) -0.0052(15) 0.0006(17) C119 0.030(2) 0.035(2) 0.045(2) -0.0049(19) 0.000(2) -0.0006(19) C120 0.046(3) 0.048(3) 0.071(3) -0.020(3) 0.002(3) 0.010(2) C121 0.060(4) 0.032(3) 0.076(4) -0.014(2) 0.001(3) -0.007(3) C122 0.048(3) 0.039(3) 0.049(3) -0.004(2) -0.004(2) -0.012(2) C123 0.033(2) 0.033(2) 0.0247(19) -0.0004(16) -0.0060(17) -0.0042(18) C124 0.026(2) 0.044(3) 0.0257(19) -0.0029(17) -0.0053(17) -0.0102(18) C125 0.037(3) 0.060(3) 0.0171(18) -0.0005(18) -0.0085(17) -0.021(2) C126 0.022(2) 0.057(3) 0.030(2) 0.002(2) -0.0114(18) -0.010(2) C127 0.031(3) 0.062(3) 0.043(3) 0.012(2) -0.009(2) -0.012(2) C128 0.050(4) 0.062(4) 0.071(4) 0.017(3) 0.000(3) 0.004(3) C129 0.060(4) 0.068(4) 0.090(4) 0.009(3) 0.015(3) 0.011(3) C130 0.045(3) 0.068(4) 0.070(4) 0.011(3) 0.007(3) -0.004(3) C131 0.030(3) 0.053(3) 0.037(2) 0.000(2) -0.008(2) -0.009(2) N4 0.036(2) 0.058(3) 0.0340(19) 0.0020(17) 0.0066(17) -0.0151(18) C132 0.044(3) 0.050(3) 0.043(3) -0.004(2) 0.012(2) -0.008(2) C133 0.040(3) 0.050(3) 0.035(2) 0.000(2) 0.008(2) -0.012(2) C134 0.043(3) 0.061(3) 0.044(3) -0.003(2) 0.010(2) -0.009(2) C135 0.052(3) 0.052(3) 0.056(3) -0.005(2) 0.004(3) -0.003(2) C136 0.049(3) 0.050(3) 0.058(3) 0.000(2) 0.000(3) -0.008(2) C137 0.051(3) 0.065(4) 0.043(3) 0.010(2) 0.000(2) -0.016(3) C138 0.057(3) 0.059(3) 0.039(2) -0.005(2) 0.015(2) -0.016(3) O10 0.078(3) 0.070(3) 0.0440(19) -0.0059(17) 0.0227(19) -0.006(2) C139 0.083(5) 0.061(4) 0.081(4) -0.014(3) 0.018(4) 0.006(3) C140 0.140(8) 0.056(4) 0.137(7) -0.010(4) 0.021(6) 0.023(4) C141 0.087(6) 0.104(6) 0.141(7) -0.037(5) 0.056(5) 0.007(4) C142 0.106(6) 0.071(4) 0.082(4) -0.036(3) 0.021(4) -0.006(4) C143 0.084(5) 0.083(4) 0.046(3) 0.017(3) 0.006(3) -0.027(4) C144 0.413(19) 0.108(7) 0.052(4) -0.007(4) 0.107(8) -0.027(9) C145 0.106(7) 0.200(9) 0.067(4) 0.057(5) 0.005(4) 0.004(6) C146 0.095(7) 0.210(10) 0.087(5) 0.035(6) 0.023(5) -0.073(6) N5 0.216(15) 0.46(2) 0.143(8) 0.074(11) -0.026(9) -0.034(13) C147 0.139(9) 0.153(9) 0.085(5) 0.002(6) 0.021(6) 0.001(6) C148 0.192(12) 0.096(6) 0.120(6) 0.004(5) -0.007(7) -0.002(6) N6 0.043(3) 0.109(4) 0.038(2) 0.005(2) -0.013(2) -0.001(3) C149 0.043(3) 0.063(3) 0.026(2) 0.005(2) -0.009(2) -0.006(2) C150 0.046(3) 0.086(4) 0.041(3) 0.017(3) -0.007(2) -0.005(3) N7 0.033(2) 0.108(4) 0.049(2) -0.001(2) 0.007(2) 0.000(2) C151 0.036(3) 0.060(3) 0.035(2) 0.005(2) 0.012(2) 0.002(2) C152 0.033(3) 0.071(4) 0.050(3) 0.016(2) 0.005(2) 0.001(2) N8 0.24(3) 0.182(17) 0.31(3) -0.165(18) 0.16(2) -0.110(19) C153 0.19(2) 0.107(13) 0.142(15) -0.093(12) 0.060(16) -0.055(15) C154 0.091(10) 0.070(9) 0.111(12) -0.029(8) -0.016(9) 0.027(8) N9 0.149(11) 0.346(18) 0.314(17) -0.010(13) 0.065(14) 0.103(11) C155 0.178(13) 0.178(13) 0.219(14) 0.012(10) 0.111(15) 0.103(10) C156 0.253(16) 0.097(9) 0.61(3) -0.018(13) 0.28(2) 0.016(10) N10 0.085(8) 0.094(9) 0.081(7) 0.020(6) 0.041(7) -0.026(7) C157 0.081(8) 0.061(9) 0.117(12) 0.009(7) 0.037(10) -0.039(7) C158 0.085(10) 0.088(13) 0.47(4) 0.051(18) 0.074(19) -0.024(9) _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 1.723(3) . ? Mo1 O2 1.919(2) . ? Mo1 O4 1.931(3) . ? Mo1 O3 1.931(2) . ? Mo1 O1 2.065(2) . ? Mo1 O5 2.243(2) . ? Mo2 N3 1.722(3) . ? Mo2 O6 1.916(2) . ? Mo2 O7 1.937(2) . ? Mo2 O8 1.948(2) . ? Mo2 O5 2.045(2) . ? Mo2 O1 2.241(2) . ? O1 C1 1.407(4) . ? O2 C12 1.366(4) . ? O3 C23 1.368(4) . ? O4 C34 1.356(4) . ? O5 C45 1.408(4) . ? O6 C56 1.364(4) . ? O7 C67 1.365(4) . ? O8 C78 1.376(4) . ? C1 C2 1.385(5) . ? C1 C6 1.389(5) . ? C2 C3 1.387(5) . ? C2 C88 1.518(5) . ? C3 C4 1.397(6) . ? C4 C5 1.393(5) . ? C4 C7 1.534(6) . ? C5 C6 1.386(5) . ? C6 C11 1.517(5) . ? C7 C10A 1.495(12) . ? C7 C8 1.507(12) . ? C7 C9 1.514(11) . ? C7 C8A 1.517(13) . ? C7 C10 1.571(12) . ? C7 C9A 1.594(11) . ? C11 C13 1.531(5) . ? C12 C13 1.396(5) . ? C12 C17 1.399(5) . ? C13 C14 1.400(5) . ? C14 C15 1.397(5) . ? C15 C16 1.379(5) . ? C15 C18 1.541(5) . ? C17 C16 1.399(5) . ? C17 C22 1.515(5) . ? C18 C21 1.521(6) . ? C18 C19 1.522(6) . ? C18 C20 1.529(6) . ? C22 C24 1.519(5) . ? C23 C28 1.395(5) . ? C23 C24 1.399(5) . ? C24 C25 1.392(5) . ? C25 C26 1.387(6) . ? C26 C27 1.394(5) . ? C26 C29 1.537(5) . ? C27 C28 1.392(5) . ? C28 C33 1.518(5) . ? C29 C30 1.505(7) . ? C29 C31 1.522(7) . ? C29 C32 1.539(7) . ? C33 C35 1.507(5) . ? C34 C39 1.396(5) . ? C34 C35 1.401(5) . ? C35 C36 1.394(5) . ? C36 C37 1.396(6) . ? C37 C38 1.389(6) . ? C37 C40 1.512(6) . ? C38 C39 1.380(5) . ? C39 C44 1.508(5) . ? C40 C43 1.499(7) . ? C40 C41 1.528(9) . ? C40 C42 1.529(9) . ? C44 C46 1.516(5) . ? C45 C50 1.383(5) . ? C45 C46 1.390(5) . ? C46 C47 1.393(5) . ? C47 C48 1.391(6) . ? C48 C49 1.388(6) . ? C48 C51 1.534(6) . ? C49 C50 1.395(5) . ? C50 C55 1.509(5) . ? C51 C52A 1.469(17) . ? C51 C54 1.498(9) . ? C51 C52 1.500(8) . ? C51 C53A 1.534(17) . ? C51 C53 1.568(10) . ? C51 C54A 1.592(18) . ? C55 C57 1.521(5) . ? C56 C57 1.394(5) . ? C56 C61 1.394(5) . ? C57 C58 1.395(5) . ? C58 C59 1.388(5) . ? C59 C60 1.390(5) . ? C59 C62 1.540(5) . ? C60 C61 1.398(5) . ? C61 C66 1.517(5) . ? C62 C65 1.524(6) . ? C62 C64 1.526(6) . ? C62 C63 1.530(7) . ? C66 C68 1.524(5) . ? C67 C68 1.389(5) . ? C67 C72 1.417(5) . ? C68 C69 1.386(5) . ? C69 C70 1.399(5) . ? C70 C71 1.388(6) . ? C70 C73 1.534(6) . ? C71 C72 1.382(5) . ? C72 C77 1.498(5) . ? C73 C75 1.529(7) . ? C73 C76 1.532(7) . ? C73 C74 1.546(7) . ? C77 C79 1.500(5) . ? C78 C83 1.385(5) . ? C78 C79 1.404(5) . ? C79 C80 1.398(5) . ? C80 C81 1.390(5) . ? C81 C82 1.395(5) . ? C81 C84 1.539(5) . ? C82 C83 1.394(5) . ? C83 C88 1.513(5) . ? C84 C87 1.499(7) . ? C84 C87A 1.507(14) . ? C84 C85A 1.513(14) . ? C84 C86 1.523(7) . ? C84 C85 1.537(7) . ? C84 C86A 1.576(15) . ? N1 C89 1.393(5) . ? C89 C90 1.401(5) . ? C89 C94 1.414(5) . ? C90 C91 1.366(6) . ? C91 C92 1.383(7) . ? C92 C93 1.381(7) . ? C93 C94 1.373(6) . ? C94 C95 1.503(5) . ? C95 C96 1.539(6) . ? C96 C97 1.509(6) . ? C97 C98 1.364(6) . ? C97 C102 1.407(6) . ? C98 C99 1.392(7) . ? C99 C100 1.367(7) . ? C100 C101 1.379(7) . ? C101 C102 1.393(6) . ? C102 N2 1.409(6) . ? N2 C103 1.299(5) . ? C103 C104 1.427(6) . ? C104 C109 1.406(6) . ? C104 C105 1.425(6) . ? C105 O9 1.351(6) . ? C105 C106 1.392(7) . ? C106 C107 1.366(7) . ? C106 C110 1.537(7) . ? C107 C108 1.410(7) . ? C108 C109 1.377(7) . ? C108 C114 1.530(7) . ? C110 C112 1.518(10) . ? C110 C111 1.533(9) . ? C110 C113 1.537(9) . ? C114 C116 1.518(8) . ? C114 C117 1.523(7) . ? C114 C115 1.544(8) . ? N3 C118 1.398(5) . ? C118 C119 1.388(6) . ? C118 C123 1.422(6) . ? C119 C120 1.372(6) . ? C120 C121 1.377(7) . ? C121 C122 1.377(7) . ? C122 C123 1.390(6) . ? C123 C124 1.472(6) . ? C124 C125 1.548(5) . ? C125 C126 1.502(7) . ? C126 C127 1.386(6) . ? C126 C131 1.387(6) . ? C127 C128 1.375(8) . ? C128 C129 1.374(8) . ? C129 C130 1.382(8) . ? C130 C131 1.392(7) . ? C131 N4 1.407(6) . ? N4 C132 1.283(5) . ? C132 C133 1.446(6) . ? C133 C138 1.394(6) . ? C133 C134 1.399(6) . ? C134 O10 1.359(5) . ? C134 C135 1.399(7) . ? C135 C136 1.375(7) . ? C135 C139 1.546(8) . ? C136 C137 1.394(7) . ? C137 C138 1.394(7) . ? C137 C143 1.534(7) . ? C139 C141 1.525(9) . ? C139 C140 1.539(9) . ? C139 C142 1.558(9) . ? C143 C144 1.454(9) . ? C143 C146 1.475(8) . ? C143 C145 1.568(10) . ? N5 C147 1.115(10) . ? C147 C148 1.377(9) . ? N6 C149 1.116(6) . ? C149 C150 1.445(7) . ? N7 C151 1.119(5) . ? C151 C152 1.440(6) . ? N8 C153 1.104(14) . ? C153 C154 1.401(13) . ? N9 C155 1.104(13) . ? C155 C156 1.408(12) . ? N10 C157 1.081(11) . ? C157 C158 1.405(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 N1 Mo1 O2 97.76(12) . . ? N1 Mo1 O4 97.77(12) . . ? O2 Mo1 O4 161.52(10) . . ? N1 Mo1 O3 96.92(12) . . ? O2 Mo1 O3 84.95(10) . . ? O4 Mo1 O3 83.29(10) . . ? N1 Mo1 O1 95.22(11) . . ? O2 Mo1 O1 87.50(10) . . ? O4 Mo1 O1 101.00(10) . . ? O3 Mo1 O1 166.47(10) . . ? N1 Mo1 O5 164.55(11) . . ? O2 Mo1 O5 85.97(10) . . ? O4 Mo1 O5 81.70(10) . . ? O3 Mo1 O5 98.35(9) . . ? O1 Mo1 O5 69.88(9) . . ? N3 Mo2 O6 97.24(12) . . ? N3 Mo2 O7 95.83(12) . . ? O6 Mo2 O7 84.77(10) . . ? N3 Mo2 O8 97.91(12) . . ? O6 Mo2 O8 161.77(10) . . ? O7 Mo2 O8 83.65(10) . . ? N3 Mo2 O5 95.54(11) . . ? O6 Mo2 O5 87.91(10) . . ? O7 Mo2 O5 167.17(10) . . ? O8 Mo2 O5 100.64(10) . . ? N3 Mo2 O1 165.04(12) . . ? O6 Mo2 O1 87.21(9) . . ? O7 Mo2 O1 98.81(10) . . ? O8 Mo2 O1 80.72(9) . . ? O5 Mo2 O1 70.26(9) . . ? C1 O1 Mo1 117.77(19) . . ? C1 O1 Mo2 132.50(19) . . ? Mo1 O1 Mo2 109.28(10) . . ? C12 O2 Mo1 124.5(2) . . ? C23 O3 Mo1 125.0(2) . . ? C34 O4 Mo1 132.3(2) . . ? C45 O5 Mo2 119.6(2) . . ? C45 O5 Mo1 129.99(19) . . ? Mo2 O5 Mo1 109.97(10) . . ? C56 O6 Mo2 124.4(2) . . ? C67 O7 Mo2 124.5(2) . . ? C78 O8 Mo2 129.3(2) . . ? C2 C1 C6 122.1(3) . . ? C2 C1 O1 118.4(3) . . ? C6 C1 O1 119.4(3) . . ? C1 C2 C3 118.0(3) . . ? C1 C2 C88 122.2(3) . . ? C3 C2 C88 119.7(3) . . ? C2 C3 C4 122.6(4) . . ? C5 C4 C3 116.8(4) . . ? C5 C4 C7 121.0(4) . . ? C3 C4 C7 122.2(4) . . ? C6 C5 C4 122.7(4) . . ? C5 C6 C1 117.8(3) . . ? C5 C6 C11 118.6(3) . . ? C1 C6 C11 123.5(3) . . ? C10A C7 C8 132.0(12) . . ? C10A C7 C9 68.3(11) . . ? C8 C7 C9 117.4(12) . . ? C10A C7 C8A 112.4(11) . . ? C8 C7 C8A 23.0(11) . . ? C9 C7 C8A 126.9(14) . . ? C10A C7 C4 109.8(7) . . ? C8 C7 C4 109.5(9) . . ? C9 C7 C4 114.1(7) . . ? C8A C7 C4 114.5(11) . . ? C10A C7 C10 38.5(8) . . ? C8 C7 C10 104.3(9) . . ? C9 C7 C10 104.9(11) . . ? C8A C7 C10 81.3(10) . . ? C4 C7 C10 105.4(6) . . ? C10A C7 C9A 108.4(9) . . ? C8 C7 C9A 86.2(11) . . ? C9 C7 C9A 40.5(10) . . ? C8A C7 C9A 105.6(10) . . ? C4 C7 C9A 105.7(7) . . ? C10 C7 C9A 141.5(9) . . ? C6 C11 C13 116.0(3) . . ? O2 C12 C13 119.3(3) . . ? O2 C12 C17 118.9(3) . . ? C13 C12 C17 121.7(3) . . ? C12 C13 C14 118.2(3) . . ? C12 C13 C11 120.1(3) . . ? C14 C13 C11 121.7(3) . . ? C15 C14 C13 121.6(4) . . ? C16 C15 C14 118.0(3) . . ? C16 C15 C18 120.0(3) . . ? C14 C15 C18 122.0(4) . . ? C15 C16 C17 123.0(3) . . ? C16 C17 C12 117.4(3) . . ? C16 C17 C22 122.0(3) . . ? C12 C17 C22 120.5(3) . . ? C21 C18 C19 108.5(4) . . ? C21 C18 C20 109.7(4) . . ? C19 C18 C20 107.9(4) . . ? C21 C18 C15 110.0(4) . . ? C19 C18 C15 112.3(3) . . ? C20 C18 C15 108.5(4) . . ? C17 C22 C24 111.2(3) . . ? O3 C23 C28 119.6(3) . . ? O3 C23 C24 119.6(3) . . ? C28 C23 C24 120.7(3) . . ? C25 C24 C23 118.3(4) . . ? C25 C24 C22 120.5(3) . . ? C23 C24 C22 121.0(3) . . ? C26 C25 C24 122.6(4) . . ? C25 C26 C27 117.4(3) . . ? C25 C26 C29 120.8(4) . . ? C27 C26 C29 121.8(4) . . ? C28 C27 C26 122.2(4) . . ? C27 C28 C23 118.7(3) . . ? C27 C28 C33 119.3(4) . . ? C23 C28 C33 121.7(3) . . ? C30 C29 C31 110.4(5) . . ? C30 C29 C26 110.3(4) . . ? C31 C29 C26 112.8(4) . . ? C30 C29 C32 108.2(5) . . ? C31 C29 C32 107.7(5) . . ? C26 C29 C32 107.3(4) . . ? C35 C33 C28 117.5(3) . . ? O4 C34 C39 119.8(3) . . ? O4 C34 C35 120.5(3) . . ? C39 C34 C35 119.7(3) . . ? C36 C35 C34 118.7(4) . . ? C36 C35 C33 120.1(3) . . ? C34 C35 C33 121.2(3) . . ? C35 C36 C37 122.4(4) . . ? C38 C37 C36 116.9(4) . . ? C38 C37 C40 120.3(4) . . ? C36 C37 C40 122.8(4) . . ? C39 C38 C37 122.6(4) . . ? C38 C39 C34 119.5(4) . . ? C38 C39 C44 120.7(4) . . ? C34 C39 C44 119.6(3) . . ? C43 C40 C37 113.9(4) . . ? C43 C40 C41 109.6(6) . . ? C37 C40 C41 109.0(5) . . ? C43 C40 C42 108.2(5) . . ? C37 C40 C42 110.3(5) . . ? C41 C40 C42 105.5(7) . . ? C39 C44 C46 110.9(3) . . ? C50 C45 C46 122.6(4) . . ? C50 C45 O5 119.6(3) . . ? C46 C45 O5 117.7(3) . . ? C45 C46 C47 117.2(4) . . ? C45 C46 C44 122.6(3) . . ? C47 C46 C44 120.2(3) . . ? C48 C47 C46 122.9(4) . . ? C49 C48 C47 116.9(4) . . ? C49 C48 C51 122.3(4) . . ? C47 C48 C51 120.8(4) . . ? C48 C49 C50 122.8(4) . . ? C45 C50 C49 117.5(4) . . ? C45 C50 C55 123.8(3) . . ? C49 C50 C55 118.7(3) . . ? C52A C51 C54 130.8(13) . . ? C52A C51 C52 39.5(15) . . ? C54 C51 C52 113.2(7) . . ? C52A C51 C53A 116.8(18) . . ? C54 C51 C53A 50.4(14) . . ? C52 C51 C53A 139.4(13) . . ? C52A C51 C48 115.7(13) . . ? C54 C51 C48 112.7(5) . . ? C52 C51 C48 110.4(5) . . ? C53A C51 C48 110.1(13) . . ? C52A C51 C53 68.4(17) . . ? C54 C51 C53 105.5(6) . . ? C52 C51 C53 107.3(7) . . ? C53A C51 C53 57.9(14) . . ? C48 C51 C53 107.3(5) . . ? C52A C51 C54A 107.0(18) . . ? C54 C51 C54A 51.3(13) . . ? C52 C51 C54A 70.6(14) . . ? C53A C51 C54A 101.4(17) . . ? C48 C51 C54A 103.8(11) . . ? C53 C51 C54A 147.1(11) . . ? C50 C55 C57 117.2(3) . . ? O6 C56 C57 118.9(3) . . ? O6 C56 C61 119.1(3) . . ? C57 C56 C61 122.0(3) . . ? C56 C57 C58 117.7(3) . . ? C56 C57 C55 120.7(3) . . ? C58 C57 C55 121.6(3) . . ? C59 C58 C57 122.4(3) . . ? C58 C59 C60 117.9(4) . . ? C58 C59 C62 122.5(3) . . ? C60 C59 C62 119.6(4) . . ? C59 C60 C61 122.1(4) . . ? C56 C61 C60 117.8(3) . . ? C56 C61 C66 120.9(3) . . ? C60 C61 C66 121.1(3) . . ? C65 C62 C64 108.2(4) . . ? C65 C62 C63 107.7(4) . . ? C64 C62 C63 108.6(4) . . ? C65 C62 C59 110.3(3) . . ? C64 C62 C59 112.7(4) . . ? C63 C62 C59 109.1(4) . . ? C61 C66 C68 110.9(3) . . ? O7 C67 C68 120.5(3) . . ? O7 C67 C72 119.2(3) . . ? C68 C67 C72 120.3(3) . . ? C69 C68 C67 119.4(3) . . ? C69 C68 C66 119.8(3) . . ? C67 C68 C66 120.6(3) . . ? C68 C69 C70 122.0(4) . . ? C71 C70 C69 116.8(4) . . ? C71 C70 C73 122.8(4) . . ? C69 C70 C73 120.3(4) . . ? C72 C71 C70 123.6(4) . . ? C71 C72 C67 117.6(4) . . ? C71 C72 C77 121.3(3) . . ? C67 C72 C77 120.8(3) . . ? C75 C73 C76 109.7(4) . . ? C75 C73 C70 108.4(4) . . ? C76 C73 C70 110.3(4) . . ? C75 C73 C74 108.3(4) . . ? C76 C73 C74 108.5(5) . . ? C70 C73 C74 111.6(4) . . ? C72 C77 C79 116.5(3) . . ? O8 C78 C83 120.2(3) . . ? O8 C78 C79 118.5(3) . . ? C83 C78 C79 121.3(3) . . ? C80 C79 C78 118.0(4) . . ? C80 C79 C77 119.3(3) . . ? C78 C79 C77 122.6(3) . . ? C81 C80 C79 122.2(3) . . ? C80 C81 C82 117.7(3) . . ? C80 C81 C84 119.7(3) . . ? C82 C81 C84 122.6(4) . . ? C83 C82 C81 122.0(4) . . ? C78 C83 C82 118.7(3) . . ? C78 C83 C88 120.5(3) . . ? C82 C83 C88 120.5(3) . . ? C87 C84 C87A 54.7(8) . . ? C87 C84 C85A 131.4(8) . . ? C87A C84 C85A 109.5(11) . . ? C87 C84 C86 108.8(5) . . ? C87A C84 C86 142.0(7) . . ? C85A C84 C86 52.2(11) . . ? C87 C84 C85 109.2(5) . . ? C87A C84 C85 58.7(8) . . ? C85A C84 C85 56.8(11) . . ? C86 C84 C85 108.2(5) . . ? C87 C84 C81 112.7(4) . . ? C87A C84 C81 108.5(7) . . ? C85A C84 C81 115.9(8) . . ? C86 C84 C81 109.5(4) . . ? C85 C84 C81 108.5(4) . . ? C87 C84 C86A 51.5(9) . . ? C87A C84 C86A 105.0(11) . . ? C85A C84 C86A 108.2(13) . . ? C86 C84 C86A 61.7(9) . . ? C85 C84 C86A 142.1(8) . . ? C81 C84 C86A 109.3(8) . . ? C83 C88 C2 110.5(3) . . ? C89 N1 Mo1 179.0(3) . . ? N1 C89 C90 118.6(3) . . ? N1 C89 C94 120.7(3) . . ? C90 C89 C94 120.7(4) . . ? C91 C90 C89 119.5(4) . . ? C90 C91 C92 120.7(4) . . ? C93 C92 C91 119.4(4) . . ? C94 C93 C92 122.4(4) . . ? C93 C94 C89 117.3(4) . . ? C93 C94 C95 120.6(4) . . ? C89 C94 C95 122.2(4) . . ? C94 C95 C96 113.4(3) . . ? C97 C96 C95 110.7(3) . . ? C98 C97 C102 119.3(4) . . ? C98 C97 C96 121.3(4) . . ? C102 C97 C96 119.2(4) . . ? C97 C98 C99 121.0(5) . . ? C100 C99 C98 119.8(5) . . ? C99 C100 C101 120.4(5) . . ? C100 C101 C102 120.2(4) . . ? C101 C102 C97 119.2(5) . . ? C101 C102 N2 122.6(4) . . ? C97 C102 N2 118.0(4) . . ? C103 N2 C102 124.2(4) . . ? N2 C103 C104 121.7(4) . . ? C109 C104 C105 118.7(5) . . ? C109 C104 C103 120.5(4) . . ? C105 C104 C103 120.8(4) . . ? O9 C105 C106 119.4(5) . . ? O9 C105 C104 119.8(5) . . ? C106 C105 C104 120.8(5) . . ? C107 C106 C105 117.0(5) . . ? C107 C106 C110 122.3(5) . . ? C105 C106 C110 120.7(5) . . ? C106 C107 C108 125.5(5) . . ? C109 C108 C107 116.1(5) . . ? C109 C108 C114 123.9(5) . . ? C107 C108 C114 120.0(5) . . ? C108 C109 C104 121.9(5) . . ? C112 C110 C111 107.3(6) . . ? C112 C110 C113 110.6(6) . . ? C111 C110 C113 106.4(6) . . ? C112 C110 C106 110.5(6) . . ? C111 C110 C106 111.2(6) . . ? C113 C110 C106 110.7(5) . . ? C116 C114 C117 107.3(5) . . ? C116 C114 C108 112.0(5) . . ? C117 C114 C108 111.3(5) . . ? C116 C114 C115 109.0(6) . . ? C117 C114 C115 108.3(5) . . ? C108 C114 C115 108.8(5) . . ? C118 N3 Mo2 176.5(2) . . ? C119 C118 N3 119.7(4) . . ? C119 C118 C123 121.2(4) . . ? N3 C118 C123 119.2(4) . . ? C120 C119 C118 120.0(4) . . ? C119 C120 C121 120.0(5) . . ? C120 C121 C122 120.4(5) . . ? C121 C122 C123 122.0(5) . . ? C122 C123 C118 116.4(4) . . ? C122 C123 C124 121.7(4) . . ? C118 C123 C124 121.9(4) . . ? C123 C124 C125 116.8(3) . . ? C126 C125 C124 109.3(3) . . ? C127 C126 C131 118.6(5) . . ? C127 C126 C125 120.2(4) . . ? C131 C126 C125 121.0(4) . . ? C128 C127 C126 121.0(5) . . ? C129 C128 C127 120.1(5) . . ? C128 C129 C130 120.1(6) . . ? C129 C130 C131 119.7(6) . . ? C126 C131 C130 120.3(5) . . ? C126 C131 N4 117.7(5) . . ? C130 C131 N4 121.9(5) . . ? C132 N4 C131 120.3(4) . . ? N4 C132 C133 122.8(4) . . ? C138 C133 C134 119.7(4) . . ? C138 C133 C132 118.5(4) . . ? C134 C133 C132 121.8(4) . . ? O10 C134 C133 119.6(4) . . ? O10 C134 C135 119.2(5) . . ? C133 C134 C135 121.2(4) . . ? C136 C135 C134 116.4(5) . . ? C136 C135 C139 122.1(5) . . ? C134 C135 C139 121.5(5) . . ? C135 C136 C137 125.3(5) . . ? C136 C137 C138 116.6(5) . . ? C136 C137 C143 120.9(5) . . ? C138 C137 C143 122.6(5) . . ? C137 C138 C133 120.9(5) . . ? C141 C139 C140 109.2(6) . . ? C141 C139 C135 109.8(5) . . ? C140 C139 C135 110.5(5) . . ? C141 C139 C142 111.5(6) . . ? C140 C139 C142 107.0(6) . . ? C135 C139 C142 108.7(5) . . ? C144 C143 C146 113.7(8) . . ? C144 C143 C137 113.4(5) . . ? C146 C143 C137 110.6(5) . . ? C144 C143 C145 104.7(7) . . ? C146 C143 C145 106.2(6) . . ? C137 C143 C145 107.5(6) . . ? N5 C147 C148 176.2(14) . . ? N6 C149 C150 178.9(6) . . ? N7 C151 C152 178.8(6) . . ? N8 C153 C154 165(4) . . ? N9 C155 C156 172(2) . . ? N10 C157 C158 178(2) . . ? _diffrn_measured_fraction_theta_max 0.983 _diffrn_reflns_theta_full 26.00 _diffrn_measured_fraction_theta_full 0.983 _refine_diff_density_max 1.808 _refine_diff_density_min -1.655 _refine_diff_density_rms 0.109 #===END