# Supplementary Material (ESI) for Dalton Transactions # This journal is (c) The Royal Society of Chemistry 2011 data_global _journal_name_full 'Dalton Trans.' _journal_coden_cambridge 0222 _publ_contact_author ; Prof. Osamu Sato Institute for Materials Chemistry and Engineering Kyushu University Kasuga 816-8580, Fukuoka Japan ; _publ_contact_author_phone 81-92-583-7787 _publ_contact_author_fax 81-92-583-7787 _publ_contact_author_email zhangwen@seu.edu.cn _publ_requested_joiurnal 'Dalton Transactions' _publ_requested_coeditor_name ? _publ_contact_letter ; Dear Sir or Madam: Please update the data of seven crystals. Yours sincerely, Osamu Sato ; _publ_contact_author_name 'Wen Zhang' _publ_author_name O.Sato #end of cif data_2_ccdc_671019 _database_code_depnum_ccdc_archive 'CCDC 671019' #TrackingRef '1.cif' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C20 H46.50 Cu2 Mo N16 O5.25' _chemical_formula_weight 818.25 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' Cu Cu 0.3201 1.2651 '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)/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 20.982(4) _cell_length_b 14.490(3) _cell_length_c 22.263(5) _cell_angle_alpha 90.00 _cell_angle_beta 96.22(3) _cell_angle_gamma 90.00 _cell_volume 6729(2) _cell_formula_units_Z 8 _cell_measurement_temperature 123(2) _cell_measurement_reflns_used 17182 _cell_measurement_theta_min 3.0 _cell_measurement_theta_max 27.5 _exptl_crystal_description block _exptl_crystal_colour purple _exptl_crystal_size_max 0.15 _exptl_crystal_size_mid 0.15 _exptl_crystal_size_min 0.10 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.615 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 3364 _exptl_absorpt_coefficient_mu 1.677 _exptl_absorpt_correction_type Multi-scan _exptl_absorpt_correction_T_min 0.729 _exptl_absorpt_correction_T_max 0.932 _exptl_absorpt_process_details SADABS _exptl_special_details ; ? ; _diffrn_ambient_temperature 123(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'Rigaku Saturn' _diffrn_measurement_method \w _diffrn_detector_area_resol_mean 7.31 _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 52486 _diffrn_reflns_av_R_equivalents 0.0423 _diffrn_reflns_av_sigmaI/netI 0.0410 _diffrn_reflns_limit_h_min -27 _diffrn_reflns_limit_h_max 25 _diffrn_reflns_limit_k_min -18 _diffrn_reflns_limit_k_max 18 _diffrn_reflns_limit_l_min -28 _diffrn_reflns_limit_l_max 24 _diffrn_reflns_theta_min 3.08 _diffrn_reflns_theta_max 27.48 _reflns_number_total 15078 _reflns_number_gt 13556 _reflns_threshold_expression >2sigma(I) _computing_data_collection CrystalClear _computing_cell_refinement CrystalClear _computing_data_reduction CrystalStructure _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics ? _computing_publication_material ? _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^)+(0.0331P)^2^+7.8040P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment constr _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 15078 _refine_ls_number_parameters 822 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0516 _refine_ls_R_factor_gt 0.0440 _refine_ls_wR_factor_ref 0.1033 _refine_ls_wR_factor_gt 0.0987 _refine_ls_goodness_of_fit_ref 1.149 _refine_ls_restrained_S_all 1.149 _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 0.378817(11) 0.749814(15) 0.157261(11) 0.00884(6) Uani 1 1 d . . . Mo2 Mo 0.123419(11) 0.261365(16) 0.341967(11) 0.00935(6) Uani 1 1 d . . . Cu1 Cu 0.168348(16) 0.93464(2) 0.124391(17) 0.01377(9) Uani 1 1 d . . . Cu2 Cu 0.355186(16) 0.94317(2) 0.351497(15) 0.01108(8) Uani 1 1 d . . . Cu3 Cu 0.146555(17) 0.44879(2) 0.144370(16) 0.01297(8) Uani 1 1 d . . . Cu4 Cu 0.336328(16) 0.44450(2) 0.374900(16) 0.01364(9) Uani 1 1 d . . . N1 N 0.11861(12) 0.87871(18) 0.05068(11) 0.0190(6) Uani 1 1 d . . . H1A H 0.1460 0.8517 0.0277 0.023 Uiso 1 1 calc R . . H1B H 0.0921 0.8349 0.0622 0.023 Uiso 1 1 calc R . . N2 N 0.10110(14) 0.9149(2) 0.19425(14) 0.0303(7) Uani 1 1 d . . . H2A H 0.0745 0.8672 0.1845 0.036 Uiso 1 1 calc R . . H2B H 0.1229 0.9039 0.2306 0.036 Uiso 1 1 calc R . . N3 N 0.23593(12) 1.02756(18) 0.15614(12) 0.0206(6) Uani 1 1 d . . . H3A H 0.2351 1.0363 0.1961 0.025 Uiso 1 1 calc R . . H3B H 0.2752 1.0077 0.1496 0.025 Uiso 1 1 calc R . . N4 N 0.11270(13) 1.04789(18) 0.10323(13) 0.0240(6) Uani 1 1 d . . . N5 N 0.23031(12) 0.83042(17) 0.13774(11) 0.0168(5) Uani 1 1 d . . . N6 N 0.25742(12) 0.94873(16) 0.35195(11) 0.0155(5) Uani 1 1 d . . . H6A H 0.2396 0.9801 0.3195 0.019 Uiso 1 1 calc R . . H6B H 0.2409 0.8913 0.3506 0.019 Uiso 1 1 calc R . . N7 N 0.40880(12) 1.03837(18) 0.30840(12) 0.0187(6) Uani 1 1 d . . . H7A H 0.4509 1.0255 0.3155 0.022 Uiso 1 1 calc R . . H7B H 0.3975 1.0375 0.2682 0.022 Uiso 1 1 calc R . . N8 N 0.40828(12) 0.86518(16) 0.41921(11) 0.0142(5) Uani 1 1 d . . . H8A H 0.3828 0.8239 0.4351 0.017 Uiso 1 1 calc R . . H8B H 0.4401 0.8346 0.4038 0.017 Uiso 1 1 calc R . . N9 N 0.35713(11) 1.04236(16) 0.41745(11) 0.0124(5) Uani 1 1 d . . . N10 N 0.35279(12) 0.85429(18) 0.28433(12) 0.0187(6) Uani 1 1 d . . . N11 N 0.38167(13) 0.97367(19) 0.13010(14) 0.0284(7) Uani 1 1 d . . . N12 N 0.29139(13) 0.59146(19) 0.21665(12) 0.0227(6) Uani 1 1 d . . . N13 N 0.44115(13) 0.54337(18) 0.13310(12) 0.0209(6) Uani 1 1 d . . . N14 N 0.32493(12) 0.71312(19) 0.01381(12) 0.0202(6) Uani 1 1 d . . . N15 N 0.50170(13) 0.78827(18) 0.07782(12) 0.0209(6) Uani 1 1 d . . . N16 N 0.50274(13) 0.7328(2) 0.26175(12) 0.0224(6) Uani 1 1 d . . . N17 N 0.09223(13) 0.36507(17) 0.07776(11) 0.0191(6) Uani 1 1 d . . . H17A H 0.1176 0.3230 0.0625 0.023 Uiso 1 1 calc R . . H17B H 0.0606 0.3354 0.0941 0.023 Uiso 1 1 calc R . . N18 N 0.24203(12) 0.43973(17) 0.13565(12) 0.0188(6) Uani 1 1 d . . . H18A H 0.2648 0.4632 0.1687 0.023 Uiso 1 1 calc R . . H18B H 0.2532 0.3802 0.1321 0.023 Uiso 1 1 calc R . . N19 N 0.09277(13) 0.54678(18) 0.18335(12) 0.0207(6) Uani 1 1 d . . . H19A H 0.0507 0.5341 0.1756 0.025 Uiso 1 1 calc R . . H19B H 0.1031 0.5480 0.2236 0.025 Uiso 1 1 calc R . . N20 N 0.14420(12) 0.54238(16) 0.07504(11) 0.0130(5) Uani 1 1 d . . . N21 N 0.14901(13) 0.3676(2) 0.21522(13) 0.0255(6) Uani 1 1 d . . . N22 N 0.27099(12) 0.54645(19) 0.34315(13) 0.0227(6) Uani 1 1 d . . . H22A H 0.2624 0.5422 0.3028 0.027 Uiso 1 1 calc R . . H22B H 0.2341 0.5395 0.3599 0.027 Uiso 1 1 calc R . . N23 N 0.39796(12) 0.38934(17) 0.31781(12) 0.0186(6) Uani 1 1 d . . . H23A H 0.4213 0.3435 0.3366 0.022 Uiso 1 1 calc R . . H23B H 0.3755 0.3661 0.2845 0.022 Uiso 1 1 calc R . . N24 N 0.35735(13) 0.43007(18) 0.46760(12) 0.0212(6) Uani 1 1 d . . . H24A H 0.3252 0.4529 0.4869 0.025 Uiso 1 1 calc R . . H24B H 0.3626 0.3701 0.4775 0.025 Uiso 1 1 calc R . . N25 N 0.40023(11) 0.55117(16) 0.38426(11) 0.0137(5) Uani 1 1 d . . . N26 N 0.27084(13) 0.34663(19) 0.36472(12) 0.0226(6) Uani 1 1 d . . . N27 N 0.21038(13) 0.11094(19) 0.27485(12) 0.0234(6) Uani 1 1 d . . . N28 N 0.11301(16) 0.4833(2) 0.37221(15) 0.0354(8) Uani 1 1 d . . . N29 N -0.00043(14) 0.2896(2) 0.42023(15) 0.0317(7) Uani 1 1 d . . . N30 N -0.00265(15) 0.2478(2) 0.23951(14) 0.0348(8) Uani 1 1 d . . . N31 N 0.06109(13) 0.05426(17) 0.36196(12) 0.0205(6) Uani 1 1 d . . . N32 N 0.17901(14) 0.2203(2) 0.48476(13) 0.0259(6) Uani 1 1 d . . . C1 C 0.08064(19) 0.9500(2) 0.01457(17) 0.0342(9) Uani 1 1 d . . . H1C H 0.0354 0.9417 0.0186 0.041 Uiso 1 1 calc R . . H1D H 0.0868 0.9434 -0.0278 0.041 Uiso 1 1 calc R . . C2 C 0.10162(19) 1.0456(2) 0.03638(17) 0.0368(10) Uani 1 1 d . . . H2C H 0.1408 1.0624 0.0196 0.044 Uiso 1 1 calc R . . H2D H 0.0688 1.0902 0.0225 0.044 Uiso 1 1 calc R . . C3 C 0.06502(17) 1.0018(3) 0.19498(18) 0.0369(9) Uani 1 1 d . . . H3C H 0.0894 1.0465 0.2204 0.044 Uiso 1 1 calc R . . H3D H 0.0247 0.9911 0.2115 0.044 Uiso 1 1 calc R . . C4 C 0.05241(17) 1.0384(3) 0.1320(2) 0.0378(10) Uani 1 1 d . . . H4A H 0.0235 0.9970 0.1081 0.045 Uiso 1 1 calc R . . H4B H 0.0317 1.0982 0.1329 0.045 Uiso 1 1 calc R . . C5 C 0.22008(17) 1.1139(2) 0.12285(17) 0.0303(8) Uani 1 1 d . . . H5A H 0.2303 1.1082 0.0815 0.036 Uiso 1 1 calc R . . H5B H 0.2447 1.1647 0.1419 0.036 Uiso 1 1 calc R . . C6 C 0.14954(18) 1.1316(2) 0.12370(19) 0.0366(9) Uani 1 1 d . . . H6C H 0.1408 1.1475 0.1643 0.044 Uiso 1 1 calc R . . H6D H 0.1364 1.1829 0.0973 0.044 Uiso 1 1 calc R . . C7 C 0.24381(14) 0.9959(2) 0.40832(14) 0.0185(6) Uani 1 1 d . . . H7C H 0.2491 0.9532 0.4420 0.022 Uiso 1 1 calc R . . H7D H 0.2001 1.0187 0.4043 0.022 Uiso 1 1 calc R . . C8 C 0.29037(14) 1.0753(2) 0.41921(14) 0.0164(6) Uani 1 1 d . . . H8C H 0.2805 1.1222 0.3885 0.020 Uiso 1 1 calc R . . H8D H 0.2861 1.1029 0.4583 0.020 Uiso 1 1 calc R . . C9 C 0.39458(16) 1.1297(2) 0.33389(15) 0.0227(7) Uani 1 1 d . . . H9A H 0.3519 1.1497 0.3182 0.027 Uiso 1 1 calc R . . H9B H 0.4252 1.1752 0.3230 0.027 Uiso 1 1 calc R . . C10 C 0.39909(15) 1.1193(2) 0.40158(15) 0.0201(7) Uani 1 1 d . . . H10A H 0.4431 1.1067 0.4175 0.024 Uiso 1 1 calc R . . H10B H 0.3859 1.1762 0.4195 0.024 Uiso 1 1 calc R . . C11 C 0.43479(14) 0.9313(2) 0.46585(14) 0.0164(6) Uani 1 1 d . . . H11A H 0.4713 0.9633 0.4525 0.020 Uiso 1 1 calc R . . H11B H 0.4488 0.8989 0.5031 0.020 Uiso 1 1 calc R . . C12 C 0.38247(14) 0.9996(2) 0.47614(13) 0.0153(6) Uani 1 1 d . . . H12A H 0.3481 0.9683 0.4937 0.018 Uiso 1 1 calc R . . H12B H 0.3995 1.0471 0.5041 0.018 Uiso 1 1 calc R . . C13 C 0.28067(14) 0.7985(2) 0.14400(13) 0.0138(6) Uani 1 1 d . . . C14 C 0.35990(13) 0.81569(19) 0.24046(13) 0.0129(6) Uani 1 1 d . . . C15 C 0.38394(13) 0.8953(2) 0.13934(14) 0.0158(6) Uani 1 1 d . . . C16 C 0.32332(14) 0.6460(2) 0.19658(13) 0.0144(6) Uani 1 1 d . . . C17 C 0.41939(14) 0.6148(2) 0.14039(13) 0.0145(6) Uani 1 1 d . . . C18 C 0.34300(14) 0.7247(2) 0.06403(14) 0.0149(6) Uani 1 1 d . . . C19 C 0.45999(14) 0.77497(19) 0.10649(13) 0.0136(6) Uani 1 1 d . . . C20 C 0.46003(14) 0.7384(2) 0.22535(14) 0.0157(6) Uani 1 1 d . . . C21 C 0.06535(15) 0.4294(2) 0.03000(14) 0.0186(6) Uani 1 1 d . . . H21A H 0.0292 0.4625 0.0432 0.022 Uiso 1 1 calc R . . H21B H 0.0507 0.3955 -0.0065 0.022 Uiso 1 1 calc R . . C22 C 0.11769(15) 0.4963(2) 0.01786(13) 0.0162(6) Uani 1 1 d . . . H22C H 0.1516 0.4634 0.0006 0.019 Uiso 1 1 calc R . . H22D H 0.1005 0.5424 -0.0111 0.019 Uiso 1 1 calc R . . C23 C 0.25605(15) 0.4917(2) 0.08141(15) 0.0215(7) Uani 1 1 d . . . H23C H 0.2505 0.4519 0.0462 0.026 Uiso 1 1 calc R . . H23D H 0.3001 0.5131 0.0865 0.026 Uiso 1 1 calc R . . C24 C 0.21128(15) 0.5729(2) 0.07256(14) 0.0188(6) Uani 1 1 d . . . H24C H 0.2226 0.6184 0.1039 0.023 Uiso 1 1 calc R . . H24D H 0.2153 0.6014 0.0338 0.023 Uiso 1 1 calc R . . C25 C 0.10786(16) 0.6364(2) 0.15632(15) 0.0232(7) Uani 1 1 d . . . H25A H 0.1508 0.6561 0.1715 0.028 Uiso 1 1 calc R . . H25B H 0.0777 0.6833 0.1662 0.028 Uiso 1 1 calc R . . C26 C 0.10290(16) 0.6216(2) 0.08888(14) 0.0214(7) Uani 1 1 d . . . H26A H 0.0587 0.6091 0.0735 0.026 Uiso 1 1 calc R . . H26B H 0.1165 0.6769 0.0693 0.026 Uiso 1 1 calc R . . C27 C 0.29999(16) 0.6376(2) 0.35986(16) 0.0247(7) Uani 1 1 d . . . H27A H 0.2945 0.6522 0.4015 0.030 Uiso 1 1 calc R . . H27B H 0.2794 0.6855 0.3342 0.030 Uiso 1 1 calc R . . C28 C 0.37081(14) 0.6325(2) 0.35177(15) 0.0186(6) Uani 1 1 d . . . H28A H 0.3761 0.6278 0.3091 0.022 Uiso 1 1 calc R . . H28B H 0.3921 0.6883 0.3674 0.022 Uiso 1 1 calc R . . C29 C 0.44044(15) 0.4640(2) 0.30119(15) 0.0203(7) Uani 1 1 d . . . H29A H 0.4184 0.5019 0.2696 0.024 Uiso 1 1 calc R . . H29B H 0.4784 0.4382 0.2864 0.024 Uiso 1 1 calc R . . C30 C 0.45903(14) 0.5216(2) 0.35734(14) 0.0183(6) Uani 1 1 d . . . H30A H 0.4863 0.4857 0.3866 0.022 Uiso 1 1 calc R . . H30B H 0.4829 0.5755 0.3468 0.022 Uiso 1 1 calc R . . C31 C 0.41735(16) 0.4820(2) 0.48501(14) 0.0224(7) Uani 1 1 d . . . H31A H 0.4541 0.4459 0.4759 0.027 Uiso 1 1 calc R . . H31B H 0.4218 0.4948 0.5280 0.027 Uiso 1 1 calc R . . C32 C 0.41427(15) 0.5708(2) 0.44989(14) 0.0198(7) Uani 1 1 d . . . H32A H 0.3810 0.6101 0.4631 0.024 Uiso 1 1 calc R . . H32B H 0.4548 0.6031 0.4573 0.024 Uiso 1 1 calc R . . C33 C 0.14170(14) 0.3306(2) 0.25956(15) 0.0191(6) Uani 1 1 d . . . C34 C 0.22069(14) 0.3137(2) 0.35691(13) 0.0158(6) Uani 1 1 d . . . C35 C 0.17913(14) 0.16166(19) 0.29858(13) 0.0138(6) Uani 1 1 d . . . C36 C 0.11445(16) 0.4053(2) 0.36205(16) 0.0228(7) Uani 1 1 d . . . C37 C 0.04252(14) 0.2803(2) 0.39315(15) 0.0182(6) Uani 1 1 d . . . C38 C 0.04147(15) 0.2519(2) 0.27478(15) 0.0200(7) Uani 1 1 d . . . C39 C 0.08383(14) 0.1254(2) 0.35603(14) 0.0149(6) Uani 1 1 d . . . C40 C 0.16055(14) 0.2330(2) 0.43461(15) 0.0168(6) Uani 1 1 d . . . O1 O 0.46615(11) 0.34532(16) 0.12921(10) 0.0252(5) Uani 1 1 d . . . O2 O 0.61969(11) 0.64710(17) 0.31223(12) 0.0333(6) Uani 1 1 d . . . O3 O 0.11379(11) 0.64317(16) 0.30352(10) 0.0254(5) Uani 1 1 d . . . O4 O 0.04340(12) 0.86121(16) 0.36553(10) 0.0272(5) Uani 1 1 d . . . O5 O 0.30778(12) 0.29452(17) 0.22216(11) 0.0299(6) Uani 1 1 d . . . O6 O 0.16773(12) 0.79170(17) 0.36332(12) 0.0339(6) Uani 1 1 d . . . O7 O 0.20461(12) 0.78787(18) 0.97328(11) 0.0318(6) Uani 1 1 d . . . O8 O 0.42528(15) 0.2362(2) 0.02793(13) 0.0486(8) Uani 1 1 d . . . O10 O 0.2649(2) 0.5492(3) 0.5195(2) 0.0288(15) Uani 0.515(7) 1 d P A 1 O10' O 0.2275(3) 0.5192(4) 0.4801(3) 0.0381(18) Uani 0.485(7) 1 d P A 2 O11 O 0.0155(4) 0.7238(4) 0.4444(3) 0.0616(19) Uani 0.50 1 d P . . O9 O 0.29677(18) 0.2149(2) 0.56341(16) 0.0379(13) Uani 0.849(11) 1 d P B 1 O9' O 0.3246(13) 0.243(2) 0.5360(16) 0.093(12) Uani 0.151(11) 1 d P B 2 loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 Mo1 0.00863(12) 0.00986(11) 0.00813(14) -0.00160(9) 0.00132(9) 0.00056(8) Mo2 0.00871(12) 0.00923(11) 0.01028(14) 0.00191(9) 0.00177(9) -0.00041(8) Cu1 0.01027(17) 0.01363(17) 0.0171(2) 0.00213(14) 0.00008(14) 0.00049(13) Cu2 0.01235(17) 0.01196(17) 0.00923(19) -0.00242(13) 0.00258(14) -0.00024(13) Cu3 0.01409(18) 0.01468(17) 0.01052(19) 0.00430(13) 0.00306(14) 0.00189(13) Cu4 0.01016(17) 0.01539(18) 0.0154(2) -0.00017(14) 0.00142(14) -0.00289(13) N1 0.0173(13) 0.0202(13) 0.0191(14) 0.0034(11) 0.0002(11) -0.0045(10) N2 0.0240(15) 0.0360(17) 0.0325(18) 0.0050(14) 0.0103(13) 0.0020(13) N3 0.0125(12) 0.0244(14) 0.0248(15) -0.0086(11) 0.0014(11) -0.0004(10) N4 0.0196(14) 0.0167(13) 0.0336(17) 0.0036(12) -0.0074(12) 0.0023(11) N5 0.0144(12) 0.0193(13) 0.0168(14) -0.0004(10) 0.0027(10) 0.0009(10) N6 0.0149(12) 0.0126(12) 0.0197(14) -0.0029(10) 0.0049(10) -0.0011(9) N7 0.0176(13) 0.0239(14) 0.0155(14) 0.0023(11) 0.0061(11) -0.0033(10) N8 0.0155(12) 0.0142(12) 0.0131(13) -0.0017(10) 0.0025(10) 0.0001(9) N9 0.0134(12) 0.0104(11) 0.0135(13) -0.0018(9) 0.0023(10) -0.0021(9) N10 0.0161(13) 0.0226(14) 0.0171(14) -0.0035(11) 0.0001(11) 0.0034(10) N11 0.0217(15) 0.0172(14) 0.049(2) 0.0040(13) 0.0168(14) 0.0029(11) N12 0.0271(15) 0.0256(14) 0.0154(14) 0.0023(11) 0.0027(11) -0.0049(12) N13 0.0211(14) 0.0190(13) 0.0234(15) -0.0005(11) 0.0059(11) 0.0021(11) N14 0.0184(13) 0.0268(14) 0.0150(15) -0.0056(11) -0.0003(11) 0.0024(11) N15 0.0198(14) 0.0178(13) 0.0259(16) 0.0016(11) 0.0063(12) 0.0014(11) N16 0.0173(13) 0.0343(16) 0.0152(15) -0.0035(12) -0.0004(11) 0.0067(11) N17 0.0270(14) 0.0144(12) 0.0158(14) 0.0030(10) 0.0012(11) -0.0011(11) N18 0.0162(13) 0.0153(12) 0.0248(15) 0.0035(11) 0.0014(11) 0.0015(10) N19 0.0167(13) 0.0279(15) 0.0179(15) -0.0044(11) 0.0040(11) 0.0029(11) N20 0.0150(12) 0.0125(11) 0.0117(13) 0.0013(9) 0.0026(10) -0.0012(9) N21 0.0252(15) 0.0270(15) 0.0246(16) 0.0113(12) 0.0042(12) -0.0004(12) N22 0.0133(13) 0.0323(16) 0.0224(15) 0.0087(12) 0.0022(11) 0.0004(11) N23 0.0152(12) 0.0163(12) 0.0244(15) -0.0053(11) 0.0024(11) -0.0006(10) N24 0.0204(14) 0.0229(14) 0.0202(15) 0.0056(11) 0.0016(11) 0.0005(11) N25 0.0128(12) 0.0134(12) 0.0146(14) -0.0006(10) 0.0004(10) -0.0008(9) N26 0.0203(14) 0.0287(15) 0.0189(15) 0.0004(11) 0.0025(11) -0.0094(11) N27 0.0247(15) 0.0266(15) 0.0192(15) -0.0003(12) 0.0036(12) 0.0064(12) N28 0.0427(19) 0.0178(15) 0.050(2) -0.0017(14) 0.0242(16) -0.0009(13) N29 0.0223(15) 0.0234(15) 0.053(2) -0.0126(14) 0.0178(14) -0.0057(12) N30 0.0290(17) 0.044(2) 0.0282(18) 0.0103(14) -0.0093(14) -0.0119(14) N31 0.0207(14) 0.0157(13) 0.0257(16) 0.0016(11) 0.0055(12) -0.0010(10) N32 0.0261(15) 0.0309(16) 0.0200(16) 0.0071(12) -0.0008(12) -0.0060(12) C1 0.039(2) 0.0286(19) 0.030(2) 0.0128(16) -0.0159(17) -0.0085(16) C2 0.041(2) 0.0247(18) 0.040(2) 0.0164(16) -0.0210(18) -0.0061(16) C3 0.0189(18) 0.043(2) 0.050(3) -0.0109(19) 0.0122(17) 0.0009(16) C4 0.0188(17) 0.0285(19) 0.065(3) 0.0005(18) -0.0012(18) 0.0117(15) C5 0.033(2) 0.0226(17) 0.035(2) -0.0021(15) 0.0027(16) -0.0131(15) C6 0.039(2) 0.0137(16) 0.052(3) 0.0040(16) -0.0147(19) 0.0023(15) C7 0.0150(15) 0.0218(16) 0.0200(17) -0.0006(13) 0.0080(12) 0.0005(12) C8 0.0199(15) 0.0156(14) 0.0142(16) -0.0033(12) 0.0040(12) 0.0038(12) C9 0.0236(17) 0.0187(15) 0.0265(19) 0.0063(13) 0.0064(14) -0.0070(13) C10 0.0206(16) 0.0129(14) 0.0270(18) -0.0025(12) 0.0037(13) -0.0071(12) C11 0.0181(15) 0.0176(14) 0.0128(16) -0.0027(12) -0.0011(12) -0.0006(11) C12 0.0183(15) 0.0179(14) 0.0098(15) -0.0026(11) 0.0021(12) 0.0006(12) C13 0.0133(14) 0.0171(14) 0.0113(15) -0.0008(11) 0.0028(11) -0.0022(11) C14 0.0130(13) 0.0145(13) 0.0111(15) -0.0030(11) 0.0002(11) 0.0025(11) C15 0.0100(13) 0.0168(15) 0.0216(17) -0.0017(12) 0.0062(12) 0.0012(11) C16 0.0148(14) 0.0178(14) 0.0105(15) -0.0018(11) 0.0002(11) 0.0005(11) C17 0.0146(14) 0.0152(14) 0.0141(15) -0.0007(11) 0.0027(11) -0.0015(11) C18 0.0132(14) 0.0138(14) 0.0180(17) -0.0032(12) 0.0031(12) -0.0005(11) C19 0.0157(14) 0.0100(13) 0.0149(16) 0.0003(11) 0.0011(12) 0.0014(11) C20 0.0142(14) 0.0196(15) 0.0142(16) -0.0022(12) 0.0050(12) 0.0017(11) C21 0.0189(15) 0.0209(15) 0.0153(16) 0.0014(12) -0.0012(12) -0.0015(12) C22 0.0220(15) 0.0161(14) 0.0108(15) 0.0018(11) 0.0026(12) 0.0021(12) C23 0.0169(15) 0.0279(17) 0.0209(18) -0.0013(14) 0.0068(13) 0.0011(13) C24 0.0234(16) 0.0184(15) 0.0150(16) 0.0039(12) 0.0034(13) -0.0077(12) C25 0.0238(17) 0.0181(15) 0.0270(19) -0.0083(13) 0.0004(14) 0.0063(13) C26 0.0270(17) 0.0146(14) 0.0217(18) -0.0005(12) -0.0009(13) 0.0071(12) C27 0.0284(18) 0.0222(16) 0.0239(19) 0.0047(14) 0.0046(14) 0.0121(14) C28 0.0201(16) 0.0130(14) 0.0227(17) 0.0008(12) 0.0020(13) 0.0013(12) C29 0.0156(15) 0.0225(16) 0.0239(18) -0.0025(13) 0.0078(13) 0.0015(12) C30 0.0111(14) 0.0180(15) 0.0263(18) 0.0024(13) 0.0040(12) -0.0015(11) C31 0.0217(16) 0.0315(18) 0.0134(16) 0.0000(13) -0.0012(13) -0.0003(14) C32 0.0213(16) 0.0195(15) 0.0171(17) -0.0058(12) -0.0037(13) -0.0025(12) C33 0.0152(15) 0.0200(15) 0.0220(18) 0.0050(13) 0.0020(13) 0.0001(12) C34 0.0177(15) 0.0167(14) 0.0137(16) -0.0008(11) 0.0051(12) -0.0050(12) C35 0.0152(14) 0.0139(14) 0.0123(15) 0.0030(11) 0.0020(11) -0.0011(11) C36 0.0228(17) 0.0180(16) 0.0291(19) 0.0035(13) 0.0099(14) -0.0007(13) C37 0.0146(14) 0.0144(14) 0.0258(18) -0.0047(12) 0.0037(13) -0.0037(11) C38 0.0162(15) 0.0240(16) 0.0192(18) 0.0045(13) -0.0013(13) -0.0058(12) C39 0.0130(14) 0.0154(14) 0.0171(16) 0.0014(12) 0.0047(12) 0.0028(11) C40 0.0131(14) 0.0168(14) 0.0207(18) 0.0024(12) 0.0025(12) -0.0019(11) O1 0.0304(13) 0.0235(12) 0.0222(13) -0.0013(10) 0.0053(10) -0.0018(10) O2 0.0190(12) 0.0330(14) 0.0478(17) 0.0167(12) 0.0035(11) 0.0021(10) O3 0.0277(13) 0.0230(12) 0.0247(13) -0.0013(10) -0.0006(10) 0.0045(10) O4 0.0369(14) 0.0201(12) 0.0246(13) 0.0001(10) 0.0026(11) 0.0028(10) O5 0.0314(14) 0.0291(13) 0.0284(14) -0.0018(11) -0.0002(11) 0.0088(11) O6 0.0279(13) 0.0290(13) 0.0433(16) 0.0020(12) -0.0029(12) -0.0050(11) O7 0.0259(13) 0.0373(15) 0.0327(15) -0.0001(12) 0.0048(11) 0.0057(11) O8 0.0530(19) 0.059(2) 0.0371(17) -0.0174(14) 0.0182(14) -0.0217(15) O10 0.022(3) 0.035(3) 0.030(3) -0.007(2) 0.005(2) 0.002(2) O10' 0.024(3) 0.046(3) 0.046(4) -0.006(3) 0.011(3) -0.001(2) O11 0.083(5) 0.038(4) 0.066(5) 0.002(3) 0.022(4) -0.001(3) O9 0.033(2) 0.043(2) 0.037(2) 0.0047(15) 0.0006(15) -0.0101(15) O9' 0.067(18) 0.08(2) 0.14(3) -0.020(18) 0.069(19) -0.039(15) _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 C16 2.146(3) . ? Mo1 C15 2.151(3) . ? Mo1 C14 2.158(3) . ? Mo1 C18 2.160(3) . ? Mo1 C20 2.161(3) . ? Mo1 C13 2.167(3) . ? Mo1 C19 2.174(3) . ? Mo1 C17 2.182(3) . ? Mo2 C36 2.145(3) . ? Mo2 C35 2.152(3) . ? Mo2 C38 2.158(3) . ? Mo2 C33 2.162(3) . ? Mo2 C37 2.162(3) . ? Mo2 C40 2.164(3) . ? Mo2 C34 2.169(3) . ? Mo2 C39 2.174(3) . ? Cu1 N5 1.994(3) . ? Cu1 N1 2.017(3) . ? Cu1 N3 2.026(3) . ? Cu1 N4 2.039(3) . ? Cu1 N2 2.229(3) . ? Cu2 N10 1.970(3) . ? Cu2 N9 2.052(2) . ? Cu2 N6 2.054(2) . ? Cu2 N7 2.079(3) . ? Cu2 N8 2.104(2) . ? Cu3 N21 1.964(3) . ? Cu3 N18 2.038(3) . ? Cu3 N20 2.051(2) . ? Cu3 N19 2.063(3) . ? Cu3 N17 2.146(3) . ? Cu4 N26 1.971(3) . ? Cu4 N25 2.042(2) . ? Cu4 N23 2.070(3) . ? Cu4 N24 2.074(3) . ? Cu4 N22 2.086(3) . ? N1 C1 1.487(4) . ? N2 C3 1.470(5) . ? N3 C5 1.474(4) . ? N4 C2 1.482(5) . ? N4 C6 1.483(4) . ? N4 C4 1.485(5) . ? N5 C13 1.148(4) . ? N6 C7 1.484(4) . ? N7 C9 1.483(4) . ? N8 C11 1.476(4) . ? N9 C8 1.485(4) . ? N9 C10 1.486(4) . ? N9 C12 1.491(4) . ? N10 C14 1.149(4) . ? N11 C15 1.154(4) . ? N12 C16 1.157(4) . ? N13 C17 1.150(4) . ? N14 C18 1.153(4) . ? N15 C19 1.154(4) . ? N16 C20 1.144(4) . ? N17 C21 1.479(4) . ? N18 C23 1.480(4) . ? N19 C25 1.479(4) . ? N20 C24 1.482(4) . ? N20 C26 1.490(4) . ? N20 C22 1.491(4) . ? N21 C33 1.148(4) . ? N22 C27 1.485(4) . ? N23 C29 1.474(4) . ? N24 C31 1.482(4) . ? N25 C28 1.482(4) . ? N25 C32 1.486(4) . ? N25 C30 1.492(4) . ? N26 C34 1.152(4) . ? N27 C35 1.151(4) . ? N28 C36 1.155(4) . ? N29 C37 1.145(4) . ? N30 C38 1.149(4) . ? N31 C39 1.150(4) . ? N32 C40 1.156(4) . ? C1 C2 1.516(5) . ? C3 C4 1.496(6) . ? C5 C6 1.504(5) . ? C7 C8 1.512(4) . ? C9 C10 1.507(4) . ? C11 C12 1.514(4) . ? C21 C22 1.511(4) . ? C23 C24 1.505(4) . ? C25 C26 1.509(5) . ? C27 C28 1.518(4) . ? C29 C30 1.519(4) . ? C31 C32 1.504(4) . ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag C16 Mo1 C15 143.42(11) . . ? C16 Mo1 C14 78.56(11) . . ? C15 Mo1 C14 75.12(11) . . ? C16 Mo1 C18 97.25(11) . . ? C15 Mo1 C18 90.36(11) . . ? C14 Mo1 C18 145.27(11) . . ? C16 Mo1 C20 94.68(11) . . ? C15 Mo1 C20 98.84(11) . . ? C14 Mo1 C20 68.67(11) . . ? C18 Mo1 C20 145.77(11) . . ? C16 Mo1 C13 74.58(11) . . ? C15 Mo1 C13 73.83(11) . . ? C14 Mo1 C13 73.29(11) . . ? C18 Mo1 C13 72.39(11) . . ? C20 Mo1 C13 141.84(11) . . ? C16 Mo1 C19 145.05(11) . . ? C15 Mo1 C19 71.43(10) . . ? C14 Mo1 C19 126.81(11) . . ? C18 Mo1 C19 74.89(11) . . ? C20 Mo1 C19 76.99(11) . . ? C13 Mo1 C19 131.38(11) . . ? C16 Mo1 C17 71.39(11) . . ? C15 Mo1 C17 144.94(11) . . ? C14 Mo1 C17 130.97(11) . . ? C18 Mo1 C17 77.59(11) . . ? C20 Mo1 C17 76.07(11) . . ? C13 Mo1 C17 130.63(11) . . ? C19 Mo1 C17 73.65(11) . . ? C36 Mo2 C35 144.13(11) . . ? C36 Mo2 C38 97.18(13) . . ? C35 Mo2 C38 94.42(12) . . ? C36 Mo2 C33 75.71(12) . . ? C35 Mo2 C33 77.05(11) . . ? C38 Mo2 C33 69.05(12) . . ? C36 Mo2 C37 71.05(11) . . ? C35 Mo2 C37 144.82(11) . . ? C38 Mo2 C37 76.18(12) . . ? C33 Mo2 C37 127.60(12) . . ? C36 Mo2 C40 90.94(12) . . ? C35 Mo2 C40 98.25(11) . . ? C38 Mo2 C40 145.73(11) . . ? C33 Mo2 C40 144.93(11) . . ? C37 Mo2 C40 75.16(12) . . ? C36 Mo2 C34 74.38(12) . . ? C35 Mo2 C34 75.85(11) . . ? C38 Mo2 C34 142.62(12) . . ? C33 Mo2 C34 73.59(12) . . ? C37 Mo2 C34 130.88(11) . . ? C40 Mo2 C34 71.60(11) . . ? C36 Mo2 C39 143.84(11) . . ? C35 Mo2 C39 71.99(11) . . ? C38 Mo2 C39 75.76(11) . . ? C33 Mo2 C39 130.45(12) . . ? C37 Mo2 C39 72.84(11) . . ? C40 Mo2 C39 78.14(11) . . ? C34 Mo2 C39 131.49(11) . . ? N5 Cu1 N1 95.07(11) . . ? N5 Cu1 N3 91.77(11) . . ? N1 Cu1 N3 146.27(11) . . ? N5 Cu1 N4 172.59(11) . . ? N1 Cu1 N4 84.41(11) . . ? N3 Cu1 N4 84.69(11) . . ? N5 Cu1 N2 104.52(11) . . ? N1 Cu1 N2 101.85(11) . . ? N3 Cu1 N2 108.30(12) . . ? N4 Cu1 N2 82.80(12) . . ? N10 Cu2 N9 176.35(10) . . ? N10 Cu2 N6 94.93(10) . . ? N9 Cu2 N6 84.92(10) . . ? N10 Cu2 N7 93.10(11) . . ? N9 Cu2 N7 84.01(10) . . ? N6 Cu2 N7 124.52(10) . . ? N10 Cu2 N8 99.25(10) . . ? N9 Cu2 N8 84.00(10) . . ? N6 Cu2 N8 117.98(10) . . ? N7 Cu2 N8 114.59(10) . . ? N21 Cu3 N18 95.58(11) . . ? N21 Cu3 N20 175.42(11) . . ? N18 Cu3 N20 85.11(10) . . ? N21 Cu3 N19 92.44(12) . . ? N18 Cu3 N19 132.28(11) . . ? N20 Cu3 N19 83.79(10) . . ? N21 Cu3 N17 100.49(11) . . ? N18 Cu3 N17 110.61(11) . . ? N20 Cu3 N17 83.46(10) . . ? N19 Cu3 N17 113.95(11) . . ? N26 Cu4 N25 176.81(11) . . ? N26 Cu4 N23 97.23(11) . . ? N25 Cu4 N23 84.72(10) . . ? N26 Cu4 N24 96.45(11) . . ? N25 Cu4 N24 84.74(10) . . ? N23 Cu4 N24 119.51(11) . . ? N26 Cu4 N22 92.65(11) . . ? N25 Cu4 N22 84.19(10) . . ? N23 Cu4 N22 119.79(11) . . ? N24 Cu4 N22 118.02(11) . . ? C1 N1 Cu1 111.1(2) . . ? C3 N2 Cu1 105.3(2) . . ? C5 N3 Cu1 106.1(2) . . ? C2 N4 C6 110.3(3) . . ? C2 N4 C4 112.5(3) . . ? C6 N4 C4 112.5(3) . . ? C2 N4 Cu1 103.7(2) . . ? C6 N4 Cu1 108.7(2) . . ? C4 N4 Cu1 108.6(2) . . ? C13 N5 Cu1 154.2(2) . . ? C7 N6 Cu2 107.81(18) . . ? C9 N7 Cu2 105.90(18) . . ? C11 N8 Cu2 106.59(18) . . ? C8 N9 C10 110.5(2) . . ? C8 N9 C12 111.0(2) . . ? C10 N9 C12 110.8(2) . . ? C8 N9 Cu2 107.37(17) . . ? C10 N9 Cu2 108.76(18) . . ? C12 N9 Cu2 108.27(17) . . ? C14 N10 Cu2 165.5(3) . . ? C21 N17 Cu3 105.85(18) . . ? C23 N18 Cu3 109.23(18) . . ? C25 N19 Cu3 106.37(19) . . ? C24 N20 C26 110.7(2) . . ? C24 N20 C22 111.7(2) . . ? C26 N20 C22 110.5(2) . . ? C24 N20 Cu3 106.23(18) . . ? C26 N20 Cu3 108.72(18) . . ? C22 N20 Cu3 108.82(17) . . ? C33 N21 Cu3 167.4(3) . . ? C27 N22 Cu4 107.98(19) . . ? C29 N23 Cu4 107.81(18) . . ? C31 N24 Cu4 106.99(19) . . ? C28 N25 C32 110.8(2) . . ? C28 N25 C30 110.6(2) . . ? C32 N25 C30 111.4(2) . . ? C28 N25 Cu4 108.54(18) . . ? C32 N25 Cu4 107.65(18) . . ? C30 N25 Cu4 107.72(17) . . ? C34 N26 Cu4 158.5(3) . . ? N1 C1 C2 110.0(3) . . ? N4 C2 C1 110.5(3) . . ? N2 C3 C4 109.4(3) . . ? N4 C4 C3 111.4(3) . . ? N3 C5 C6 107.9(3) . . ? N4 C6 C5 109.8(3) . . ? N6 C7 C8 107.8(2) . . ? N9 C8 C7 110.2(2) . . ? N7 C9 C10 107.5(2) . . ? N9 C10 C9 109.7(2) . . ? N8 C11 C12 107.8(2) . . ? N9 C12 C11 109.6(2) . . ? N5 C13 Mo1 175.2(3) . . ? N10 C14 Mo1 175.9(3) . . ? N11 C15 Mo1 174.7(3) . . ? N12 C16 Mo1 177.5(3) . . ? N13 C17 Mo1 178.2(3) . . ? N14 C18 Mo1 178.2(3) . . ? N15 C19 Mo1 177.8(3) . . ? N16 C20 Mo1 179.4(3) . . ? N17 C21 C22 107.8(2) . . ? N20 C22 C21 110.2(2) . . ? N18 C23 C24 109.2(2) . . ? N20 C24 C23 110.1(2) . . ? N19 C25 C26 106.6(2) . . ? N20 C26 C25 109.6(2) . . ? N22 C27 C28 107.9(2) . . ? N25 C28 C27 110.0(2) . . ? N23 C29 C30 107.8(2) . . ? N25 C30 C29 109.8(2) . . ? N24 C31 C32 108.1(3) . . ? N25 C32 C31 109.9(2) . . ? N21 C33 Mo2 177.5(3) . . ? N26 C34 Mo2 175.9(3) . . ? N27 C35 Mo2 177.5(3) . . ? N28 C36 Mo2 176.3(3) . . ? N29 C37 Mo2 179.4(3) . . ? N30 C38 Mo2 179.0(3) . . ? N31 C39 Mo2 177.6(3) . . ? N32 C40 Mo2 177.6(3) . . ? _diffrn_measured_fraction_theta_max 0.977 _diffrn_reflns_theta_full 27.48 _diffrn_measured_fraction_theta_full 0.977 _refine_diff_density_max 0.999 _refine_diff_density_min -0.582 _refine_diff_density_rms 0.090 #================================================================= data_1_ccdc_671020 _database_code_depnum_ccdc_archive 'CCDC 671020' #TrackingRef '1_and_4.cif' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C44 H66 Cu2 Mo N16 O15' _chemical_formula_weight 1282.15 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' Cu Cu 0.3201 1.2651 '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 13.055(3) _cell_length_b 24.419(5) _cell_length_c 18.402(4) _cell_angle_alpha 90.00 _cell_angle_beta 93.80(3) _cell_angle_gamma 90.00 _cell_volume 5853(2) _cell_formula_units_Z 4 _cell_measurement_temperature 123(2) _cell_measurement_reflns_used 9441 _cell_measurement_theta_min 3.1 _cell_measurement_theta_max 27.5 _exptl_crystal_description block _exptl_crystal_colour blue _exptl_crystal_size_max 0.10 _exptl_crystal_size_mid 0.05 _exptl_crystal_size_min 0.03 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.455 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 2648 _exptl_absorpt_coefficient_mu 1.005 _exptl_absorpt_correction_type Multi-scan _exptl_absorpt_correction_T_min 0.941 _exptl_absorpt_correction_T_max 0.970 _exptl_absorpt_process_details ; Jacobson, R. (1998) Private communication ; _exptl_special_details ; ? ; _diffrn_ambient_temperature 123(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'Rigaku Saturn' _diffrn_measurement_method \w _diffrn_detector_area_resol_mean 7.31 _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 37730 _diffrn_reflns_av_R_equivalents 0.0820 _diffrn_reflns_av_sigmaI/netI 0.0815 _diffrn_reflns_limit_h_min -15 _diffrn_reflns_limit_h_max 13 _diffrn_reflns_limit_k_min -29 _diffrn_reflns_limit_k_max 29 _diffrn_reflns_limit_l_min -20 _diffrn_reflns_limit_l_max 21 _diffrn_reflns_theta_min 3.43 _diffrn_reflns_theta_max 25.03 _reflns_number_total 10241 _reflns_number_gt 7805 _reflns_threshold_expression >2sigma(I) _computing_data_collection CrystalClear _computing_cell_refinement CrystalClear _computing_data_reduction CrystalStructure _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics ? _computing_publication_material ? _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. The ADP's of c38 c43 are abnormally shaped, probably due to the heavy atom effect.C43 and C38 therefore are RESTRAINED with ESD of 0.01 so that their Uij components approximate to isotropic behavior with the command ISOR. The hydrogen atoms which shold be bonded to the oxgen atoms of the solvent water molecules can not be located from the Fourier diffence map, and no geometrical information about the orientaions of the H atoms can be obtained. Therefore, these O atoms were left isolatedly. ; _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^)+(0.0610P)^2^+6.5517P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment constr _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 10241 _refine_ls_number_parameters 703 _refine_ls_number_restraints 54 _refine_ls_R_factor_all 0.1284 _refine_ls_R_factor_gt 0.0915 _refine_ls_wR_factor_ref 0.1919 _refine_ls_wR_factor_gt 0.1745 _refine_ls_goodness_of_fit_ref 1.271 _refine_ls_restrained_S_all 1.269 _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 0.25613(4) 0.14680(2) 0.74922(3) 0.01110(16) Uani 1 1 d . . . Cu1 Cu 0.25149(6) 0.30376(3) 0.55759(4) 0.0174(2) Uani 1 1 d . . . Cu2 Cu 0.24421(6) 0.30662(3) 0.93606(4) 0.0170(2) Uani 1 1 d . . . N1 N 0.3375(4) 0.2695(2) 0.4818(3) 0.0196(13) Uani 1 1 d . . . N2 N 0.0929(4) 0.3100(2) 0.5409(3) 0.0187(13) Uani 1 1 d . . . N3 N 0.3081(4) 0.3634(2) 0.6280(3) 0.0203(13) Uani 1 1 d . . . N4 N 0.2460(5) 0.3672(2) 0.4863(3) 0.0247(14) Uani 1 1 d . . . N5 N 0.2577(4) 0.2440(2) 0.6257(3) 0.0211(13) Uani 1 1 d U . . N6 N 0.1821(4) 0.3614(2) 0.8602(3) 0.0186(13) Uani 1 1 d . . . N7 N 0.1509(4) 0.2719(2) 1.0082(3) 0.0191(13) Uani 1 1 d . . . N8 N 0.3999(4) 0.3176(2) 0.9593(3) 0.0182(13) Uani 1 1 d . . . N9 N 0.2367(4) 0.3716(2) 1.0035(3) 0.0228(14) Uani 1 1 d . . . N10 N 0.2493(4) 0.2445(2) 0.8716(3) 0.0148(12) Uani 1 1 d . . . N11 N 0.0207(4) 0.1978(2) 0.7170(3) 0.0231(14) Uani 1 1 d U . . N12 N 0.4894(5) 0.1988(2) 0.7843(3) 0.0227(14) Uani 1 1 d . . . N13 N 0.1105(5) 0.0978(3) 0.8762(3) 0.0333(17) Uani 1 1 d . . . N14 N 0.3858(5) 0.0490(3) 0.8381(3) 0.0299(16) Uani 1 1 d . . . N15 N 0.1296(5) 0.0476(3) 0.6602(3) 0.0302(15) Uani 1 1 d U . . N16 N 0.3969(5) 0.0982(3) 0.6207(3) 0.0371(17) Uani 1 1 d . . . C1 C 0.3624(5) 0.2165(3) 0.4742(4) 0.0261(18) Uani 1 1 d . . . H1A H 0.3432 0.1917 0.5092 0.031 Uiso 1 1 calc R . . C2 C 0.4150(6) 0.1972(4) 0.4171(4) 0.035(2) Uani 1 1 d . . . H2A H 0.4318 0.1603 0.4137 0.042 Uiso 1 1 calc R . . C3 C 0.4420(6) 0.2339(3) 0.3651(4) 0.032(2) Uani 1 1 d . . . H3A H 0.4754 0.2219 0.3250 0.038 Uiso 1 1 calc R . . C4 C 0.4192(6) 0.2883(4) 0.3728(4) 0.032(2) Uani 1 1 d . . . H4A H 0.4394 0.3135 0.3387 0.038 Uiso 1 1 calc R . . C5 C 0.3667(5) 0.3056(3) 0.4309(3) 0.0225(17) Uani 1 1 d . . . C6 C 0.3412(6) 0.3638(3) 0.4459(4) 0.0314(19) Uani 1 1 d . . . H6A H 0.3313 0.3837 0.4003 0.038 Uiso 1 1 calc R . . H6B H 0.3978 0.3807 0.4745 0.038 Uiso 1 1 calc R . . C7 C 0.0202(6) 0.2914(3) 0.5824(4) 0.0245(17) Uani 1 1 d . . . H7A H 0.0394 0.2699 0.6226 0.029 Uiso 1 1 calc R . . C8 C -0.0815(6) 0.3031(3) 0.5676(4) 0.0299(18) Uani 1 1 d . . . H8A H -0.1309 0.2889 0.5966 0.036 Uiso 1 1 calc R . . C9 C -0.1093(6) 0.3362(3) 0.5094(4) 0.040(2) Uani 1 1 d . . . H9A H -0.1779 0.3454 0.4994 0.048 Uiso 1 1 calc R . . C10 C -0.0361(6) 0.3559(3) 0.4656(4) 0.0311(19) Uani 1 1 d . . . H10A H -0.0544 0.3781 0.4257 0.037 Uiso 1 1 calc R . . C11 C 0.0650(5) 0.3420(3) 0.4824(4) 0.0226(16) Uani 1 1 d . . . C12 C 0.1518(6) 0.3588(3) 0.4382(4) 0.037(2) Uani 1 1 d . . . H12A H 0.1638 0.3307 0.4025 0.044 Uiso 1 1 calc R . . H12B H 0.1341 0.3925 0.4124 0.044 Uiso 1 1 calc R . . C13 C 0.3504(5) 0.3564(3) 0.6966(4) 0.0284(18) Uani 1 1 d . . . H13A H 0.3570 0.3210 0.7149 0.034 Uiso 1 1 calc R . . C14 C 0.3841(6) 0.3992(4) 0.7402(5) 0.045(3) Uani 1 1 d . . . H14A H 0.4137 0.3932 0.7869 0.054 Uiso 1 1 calc R . . C15 C 0.3725(7) 0.4509(4) 0.7125(5) 0.050(3) Uani 1 1 d . . . H15A H 0.3938 0.4807 0.7411 0.060 Uiso 1 1 calc R . . C16 C 0.3294(6) 0.4598(3) 0.6421(5) 0.043(2) Uani 1 1 d . . . H16A H 0.3227 0.4949 0.6228 0.052 Uiso 1 1 calc R . . C17 C 0.2972(6) 0.4146(3) 0.6024(4) 0.0277(18) Uani 1 1 d . . . C18 C 0.2410(6) 0.4194(3) 0.5281(4) 0.035(2) Uani 1 1 d . . . H18A H 0.1698 0.4287 0.5338 0.043 Uiso 1 1 calc R . . H18B H 0.2713 0.4486 0.5011 0.043 Uiso 1 1 calc R . . C19 C 0.2575(5) 0.2099(3) 0.6688(3) 0.0134(14) Uani 1 1 d U . . C20 C 0.1413(5) 0.3503(3) 0.7928(3) 0.0215(16) Uani 1 1 d . . . H20A H 0.1397 0.3143 0.7763 0.026 Uiso 1 1 calc R . . C21 C 0.1015(6) 0.3915(4) 0.7476(4) 0.038(2) Uani 1 1 d . . . H21A H 0.0733 0.3832 0.7012 0.045 Uiso 1 1 calc R . . C22 C 0.1041(6) 0.4441(4) 0.7716(4) 0.041(2) Uani 1 1 d . . . H22A H 0.0776 0.4720 0.7416 0.049 Uiso 1 1 calc R . . C23 C 0.1463(6) 0.4559(3) 0.8409(4) 0.034(2) Uani 1 1 d . . . H23A H 0.1496 0.4917 0.8580 0.041 Uiso 1 1 calc R . . C24 C 0.1838(5) 0.4126(3) 0.8843(4) 0.0242(17) Uani 1 1 d . . . C25 C 0.2392(6) 0.4216(3) 0.9572(4) 0.0301(18) Uani 1 1 d . . . H25A H 0.3099 0.4315 0.9507 0.036 Uiso 1 1 calc R . . H25B H 0.2074 0.4518 0.9817 0.036 Uiso 1 1 calc R . . C26 C 0.1268(5) 0.2186(3) 1.0147(4) 0.0206(16) Uani 1 1 d . . . H26A H 0.1468 0.1941 0.9796 0.025 Uiso 1 1 calc R . . C27 C 0.0733(5) 0.1990(3) 1.0718(4) 0.0277(18) Uani 1 1 d . . . H27A H 0.0582 0.1620 1.0761 0.033 Uiso 1 1 calc R . . C28 C 0.0433(5) 0.2365(3) 1.1220(4) 0.0291(19) Uani 1 1 d . . . H28A H 0.0072 0.2246 1.1609 0.035 Uiso 1 1 calc R . . C29 C 0.0657(5) 0.2913(3) 1.1158(4) 0.0251(17) Uani 1 1 d . . . H29A H 0.0453 0.3165 1.1499 0.030 Uiso 1 1 calc R . . C30 C 0.1192(5) 0.3077(3) 1.0576(3) 0.0216(16) Uani 1 1 d . . . C31 C 0.1403(6) 0.3673(3) 1.0411(4) 0.0306(19) Uani 1 1 d . . . H31A H 0.0838 0.3823 1.0105 0.037 Uiso 1 1 calc R . . H31B H 0.1464 0.3881 1.0861 0.037 Uiso 1 1 calc R . . C32 C 0.4786(5) 0.2986(3) 0.9226(3) 0.0204(16) Uani 1 1 d . . . H32A H 0.4644 0.2764 0.8821 0.024 Uiso 1 1 calc R . . C33 C 0.5784(6) 0.3110(3) 0.9429(4) 0.0263(17) Uani 1 1 d . . . H33A H 0.6312 0.2969 0.9169 0.032 Uiso 1 1 calc R . . C34 C 0.6005(5) 0.3444(3) 1.0019(4) 0.0277(18) Uani 1 1 d . . . H34A H 0.6681 0.3532 1.0166 0.033 Uiso 1 1 calc R . . C35 C 0.5192(6) 0.3648(3) 1.0391(4) 0.0310(19) Uani 1 1 d . . . H35A H 0.5321 0.3877 1.0790 0.037 Uiso 1 1 calc R . . C36 C 0.4200(5) 0.3510(3) 1.0169(3) 0.0205(16) Uani 1 1 d . . . C37 C 0.3285(5) 0.3687(3) 1.0553(4) 0.0275(18) Uani 1 1 d . . . H37A H 0.3162 0.3429 1.0938 0.033 Uiso 1 1 calc R . . H37B H 0.3414 0.4044 1.0772 0.033 Uiso 1 1 calc R . . C38 C 0.1025(5) 0.1795(3) 0.7274(3) 0.0175(15) Uani 1 1 d U . . C39 C 0.4095(5) 0.1810(3) 0.7724(3) 0.0157(15) Uani 1 1 d . . . C40 C 0.2517(5) 0.2110(3) 0.8295(3) 0.0147(15) Uani 1 1 d . . . C41 C 0.1630(5) 0.1146(3) 0.8331(4) 0.0197(16) Uani 1 1 d . . . C42 C 0.3406(5) 0.0826(3) 0.8067(3) 0.0171(15) Uani 1 1 d . . . C43 C 0.1742(5) 0.0822(3) 0.6908(3) 0.0185(15) Uani 1 1 d U . . C44 C 0.3495(6) 0.1144(3) 0.6652(4) 0.0224(16) Uani 1 1 d . . . O1 O 0.4829(4) 0.9739(2) 0.9335(3) 0.0431(15) Uani 1 1 d . . . O2 O 0.0281(4) 0.9739(2) 0.5663(3) 0.0374(14) Uani 1 1 d . . . O3 O 0.0351(4) 0.0535(2) 0.0068(3) 0.0395(14) Uani 1 1 d . . . O4 O 0.4481(5) 0.0477(3) 0.4886(3) 0.0531(18) Uani 1 1 d . . . O5 O 0.6421(5) 0.3706(2) 0.7495(3) 0.0511(16) Uani 1 1 d . . . O6 O 0.6248(4) 0.4631(2) 0.8382(3) 0.0489(16) Uani 1 1 d . . . O7 O 0.8583(5) 0.3793(3) 0.7595(4) 0.073(2) Uani 1 1 d . . . O8 O 0.5783(5) 0.5393(2) 0.7205(4) 0.0603(18) Uani 1 1 d . . . O9 O 0.1481(5) 0.0477(3) 0.1377(3) 0.0489(16) Uani 1 1 d . . . O10 O 0.6774(4) 0.2603(2) 0.7907(3) 0.0342(13) Uani 1 1 d . . . O11 O 0.8037(4) 0.2110(2) 0.6967(3) 0.0398(14) Uani 1 1 d . . . O12 O 0.3359(5) 0.0348(4) 0.3614(4) 0.087(3) Uani 1 1 d . . . O13 O 0.7339(4) 0.6119(2) 0.7378(3) 0.0501(16) Uani 1 1 d . . . O14 O 0.6412(5) 0.9663(3) 0.8436(4) 0.076(2) Uani 1 1 d . . . O15 O 0.4043(5) 0.9525(3) 0.2706(5) 0.081(2) Uani 1 1 d . . . 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 0.0145(3) 0.0087(3) 0.0102(3) -0.0003(2) 0.0014(2) 0.0002(3) Cu1 0.0242(5) 0.0125(5) 0.0156(4) 0.0036(3) 0.0021(4) -0.0012(4) Cu2 0.0219(5) 0.0130(5) 0.0161(4) -0.0045(3) 0.0024(4) 0.0017(4) N1 0.022(3) 0.022(4) 0.015(3) 0.001(3) 0.003(2) 0.000(3) N2 0.025(3) 0.017(3) 0.013(3) 0.002(2) -0.004(3) -0.002(3) N3 0.019(3) 0.020(4) 0.022(3) -0.008(3) 0.005(3) -0.002(3) N4 0.031(4) 0.017(4) 0.026(3) 0.012(3) 0.004(3) 0.001(3) N5 0.026(3) 0.018(3) 0.020(3) 0.003(3) 0.006(2) -0.004(3) N6 0.020(3) 0.017(3) 0.019(3) -0.001(2) -0.002(2) 0.006(3) N7 0.011(3) 0.027(4) 0.019(3) -0.004(3) -0.001(2) 0.003(3) N8 0.020(3) 0.021(3) 0.014(3) 0.000(2) 0.000(2) -0.002(3) N9 0.027(3) 0.023(4) 0.019(3) -0.006(3) 0.005(3) 0.001(3) N10 0.018(3) 0.017(3) 0.010(3) -0.006(3) 0.002(2) -0.002(2) N11 0.020(3) 0.030(3) 0.020(3) 0.008(3) 0.003(2) 0.004(3) N12 0.024(4) 0.021(4) 0.023(3) 0.000(3) 0.006(3) -0.001(3) N13 0.040(4) 0.021(4) 0.043(4) 0.013(3) 0.027(3) 0.001(3) N14 0.041(4) 0.022(4) 0.024(3) 0.003(3) -0.012(3) 0.002(3) N15 0.035(3) 0.023(3) 0.030(3) 0.000(2) -0.011(3) -0.006(3) N16 0.055(5) 0.017(4) 0.042(4) -0.010(3) 0.023(4) -0.008(3) C1 0.021(4) 0.035(5) 0.021(4) 0.003(3) -0.006(3) 0.002(3) C2 0.028(4) 0.050(6) 0.028(4) 0.007(4) 0.007(4) 0.009(4) C3 0.031(5) 0.042(6) 0.023(4) -0.006(4) 0.004(3) 0.018(4) C4 0.026(4) 0.054(6) 0.016(4) 0.012(4) 0.007(3) 0.000(4) C5 0.018(4) 0.030(5) 0.019(4) 0.010(3) -0.004(3) -0.001(3) C6 0.031(4) 0.034(5) 0.029(4) 0.012(4) 0.006(3) -0.011(4) C7 0.029(4) 0.021(4) 0.023(4) 0.005(3) -0.007(3) -0.003(3) C8 0.026(4) 0.025(5) 0.038(5) -0.004(4) 0.000(4) -0.002(3) C9 0.030(5) 0.038(5) 0.050(5) -0.001(4) -0.018(4) 0.002(4) C10 0.038(5) 0.027(5) 0.026(4) 0.010(3) -0.011(4) -0.001(4) C11 0.029(4) 0.013(4) 0.025(4) 0.004(3) -0.003(3) 0.001(3) C12 0.051(5) 0.036(5) 0.023(4) 0.024(4) -0.006(4) -0.006(4) C13 0.021(4) 0.032(5) 0.034(4) -0.019(4) 0.015(3) 0.002(3) C14 0.031(5) 0.069(8) 0.036(5) -0.030(5) 0.009(4) -0.013(5) C15 0.040(5) 0.064(8) 0.049(6) -0.034(5) 0.015(5) -0.028(5) C16 0.045(5) 0.022(5) 0.066(6) -0.016(4) 0.019(5) -0.010(4) C17 0.029(4) 0.017(4) 0.039(5) -0.006(3) 0.015(4) -0.001(3) C18 0.045(5) 0.021(5) 0.042(5) 0.011(4) 0.012(4) -0.002(4) C19 0.015(3) 0.008(3) 0.016(3) -0.005(3) -0.003(3) -0.002(3) C20 0.021(4) 0.025(4) 0.019(4) 0.001(3) 0.004(3) 0.002(3) C21 0.028(5) 0.050(6) 0.036(5) 0.015(4) 0.009(4) -0.001(4) C22 0.041(5) 0.047(6) 0.037(5) 0.028(4) 0.013(4) 0.013(4) C23 0.041(5) 0.016(4) 0.046(5) 0.009(4) 0.012(4) -0.002(4) C24 0.020(4) 0.022(4) 0.032(4) 0.002(3) 0.014(3) -0.003(3) C25 0.037(5) 0.018(4) 0.037(4) -0.007(3) 0.010(4) -0.004(4) C26 0.013(4) 0.025(4) 0.025(4) -0.002(3) 0.001(3) -0.004(3) C27 0.029(4) 0.022(4) 0.033(4) 0.011(3) 0.003(3) -0.008(3) C28 0.019(4) 0.049(6) 0.021(4) -0.003(4) 0.009(3) -0.001(4) C29 0.012(4) 0.031(5) 0.032(4) -0.005(4) 0.005(3) 0.003(3) C30 0.024(4) 0.026(4) 0.015(3) -0.005(3) 0.007(3) -0.001(3) C31 0.028(4) 0.042(5) 0.024(4) -0.010(4) 0.016(3) 0.004(4) C32 0.022(4) 0.023(4) 0.017(3) -0.006(3) 0.000(3) -0.002(3) C33 0.024(4) 0.026(5) 0.028(4) 0.001(3) 0.000(3) 0.005(3) C34 0.021(4) 0.023(4) 0.038(4) 0.005(4) -0.009(3) 0.000(3) C35 0.034(5) 0.025(5) 0.032(4) -0.003(4) -0.016(4) 0.002(4) C36 0.025(4) 0.018(4) 0.019(4) 0.004(3) 0.002(3) 0.002(3) C37 0.031(4) 0.022(4) 0.030(4) -0.008(3) 0.004(3) -0.001(3) C38 0.024(3) 0.015(3) 0.013(3) 0.009(3) 0.007(3) -0.001(3) C39 0.021(4) 0.016(4) 0.011(3) 0.003(3) 0.008(3) 0.005(3) C40 0.012(3) 0.018(4) 0.014(3) 0.001(3) 0.000(3) -0.003(3) C41 0.014(4) 0.020(4) 0.023(4) 0.004(3) -0.011(3) 0.006(3) C42 0.018(4) 0.017(4) 0.017(4) 0.000(3) 0.006(3) -0.003(3) C43 0.022(3) 0.012(3) 0.020(3) 0.004(2) -0.007(3) 0.000(3) C44 0.032(4) 0.009(4) 0.027(4) -0.005(3) 0.008(3) -0.003(3) O1 0.044(3) 0.044(4) 0.041(3) 0.022(3) -0.001(3) 0.014(3) O2 0.037(3) 0.039(4) 0.036(3) -0.016(3) 0.003(3) -0.008(3) O3 0.042(3) 0.040(4) 0.038(3) 0.011(3) 0.010(3) -0.002(3) O4 0.055(4) 0.065(5) 0.040(3) -0.019(3) 0.009(3) 0.005(3) O5 0.053(4) 0.035(4) 0.065(4) 0.002(3) 0.000(3) 0.001(3) O6 0.046(4) 0.044(4) 0.057(4) -0.011(3) 0.013(3) -0.005(3) O7 0.047(4) 0.086(6) 0.087(5) 0.033(4) 0.015(4) 0.005(4) O8 0.040(4) 0.031(4) 0.110(5) -0.001(4) 0.012(4) 0.002(3) O9 0.052(4) 0.054(4) 0.039(3) -0.004(3) -0.008(3) -0.007(3) O10 0.021(3) 0.038(3) 0.045(3) -0.009(3) 0.007(2) -0.001(2) O11 0.027(3) 0.055(4) 0.037(3) -0.006(3) 0.001(2) 0.012(3) O12 0.061(5) 0.131(8) 0.067(5) -0.025(5) -0.017(4) 0.018(5) O13 0.038(4) 0.040(4) 0.073(4) 0.004(3) 0.007(3) -0.001(3) O14 0.054(4) 0.113(7) 0.064(4) -0.017(4) 0.020(4) 0.001(4) O15 0.028(4) 0.056(5) 0.157(7) -0.004(5) 0.000(4) -0.001(3) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag Mo1 C19 2.139(7) . ? Mo1 C43 2.154(7) . ? Mo1 C42 2.154(7) . ? Mo1 C40 2.157(7) . ? Mo1 C38 2.171(7) . ? Mo1 C41 2.174(7) . ? Mo1 C44 2.180(7) . ? Mo1 C39 2.185(7) . ? Cu1 N5 1.923(6) . ? Cu1 N4 2.028(5) . ? Cu1 N1 2.028(5) . ? Cu1 N3 2.053(5) . ? Cu1 N2 2.078(6) . ? Cu2 N10 1.929(5) . ? Cu2 N9 2.021(6) . ? Cu2 N7 2.044(6) . ? Cu2 N6 2.060(5) . ? Cu2 N8 2.066(5) . ? N1 C1 1.344(9) . ? N1 C5 1.360(8) . ? N2 C7 1.336(9) . ? N2 C11 1.359(8) . ? N3 C17 1.343(9) . ? N3 C13 1.354(9) . ? N4 C12 1.481(9) . ? N4 C18 1.493(9) . ? N4 C6 1.493(9) . ? N5 C19 1.148(8) . ? N6 C24 1.327(9) . ? N6 C20 1.344(8) . ? N7 C30 1.345(8) . ? N7 C26 1.346(9) . ? N8 C36 1.349(8) . ? N8 C32 1.349(8) . ? N9 C31 1.480(8) . ? N9 C37 1.483(9) . ? N9 C25 1.489(9) . ? N10 C40 1.129(8) . ? N11 C38 1.163(8) . ? N12 C39 1.138(8) . ? N13 C41 1.158(9) . ? N14 C42 1.143(8) . ? N15 C43 1.151(8) . ? N16 C44 1.130(9) . ? C1 C2 1.377(10) . ? C2 C3 1.373(10) . ? C3 C4 1.371(11) . ? C4 C5 1.374(10) . ? C5 C6 1.490(10) . ? C7 C8 1.368(10) . ? C8 C9 1.372(10) . ? C9 C10 1.377(11) . ? C10 C11 1.379(10) . ? C11 C12 1.495(10) . ? C13 C14 1.373(10) . ? C14 C15 1.366(13) . ? C15 C16 1.395(12) . ? C16 C17 1.373(10) . ? C17 C18 1.511(10) . ? C20 C21 1.383(10) . ? C21 C22 1.357(12) . ? C22 C23 1.387(11) . ? C23 C24 1.394(10) . ? C24 C25 1.498(10) . ? C26 C27 1.386(9) . ? C27 C28 1.375(10) . ? C28 C29 1.375(10) . ? C29 C30 1.377(9) . ? C30 C31 1.515(10) . ? C32 C33 1.366(9) . ? C33 C34 1.374(10) . ? C34 C35 1.393(10) . ? C35 C36 1.375(10) . ? C36 C37 1.491(9) . ? 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 C19 Mo1 C43 102.1(2) . . ? C19 Mo1 C42 146.8(2) . . ? C43 Mo1 C42 86.2(2) . . ? C19 Mo1 C40 87.2(2) . . ? C43 Mo1 C40 147.1(2) . . ? C42 Mo1 C40 103.2(2) . . ? C19 Mo1 C38 69.9(2) . . ? C43 Mo1 C38 75.8(3) . . ? C42 Mo1 C38 142.7(2) . . ? C40 Mo1 C38 78.1(2) . . ? C19 Mo1 C41 141.5(2) . . ? C43 Mo1 C41 78.9(3) . . ? C42 Mo1 C41 71.4(2) . . ? C40 Mo1 C41 74.6(2) . . ? C38 Mo1 C41 73.2(2) . . ? C19 Mo1 C44 74.9(2) . . ? C43 Mo1 C44 70.3(3) . . ? C42 Mo1 C44 78.0(2) . . ? C40 Mo1 C44 142.3(2) . . ? C38 Mo1 C44 123.7(2) . . ? C41 Mo1 C44 137.5(2) . . ? C19 Mo1 C39 79.0(2) . . ? C43 Mo1 C39 142.7(3) . . ? C42 Mo1 C39 75.5(2) . . ? C40 Mo1 C39 69.8(2) . . ? C38 Mo1 C39 136.0(2) . . ? C41 Mo1 C39 123.2(2) . . ? C44 Mo1 C39 74.3(2) . . ? N5 Cu1 N4 179.5(3) . . ? N5 Cu1 N1 97.7(2) . . ? N4 Cu1 N1 82.4(2) . . ? N5 Cu1 N3 97.4(2) . . ? N4 Cu1 N3 82.1(2) . . ? N1 Cu1 N3 122.3(2) . . ? N5 Cu1 N2 98.7(2) . . ? N4 Cu1 N2 81.7(2) . . ? N1 Cu1 N2 121.3(2) . . ? N3 Cu1 N2 110.8(2) . . ? N10 Cu2 N9 179.2(2) . . ? N10 Cu2 N7 96.9(2) . . ? N9 Cu2 N7 82.6(2) . . ? N10 Cu2 N6 97.0(2) . . ? N9 Cu2 N6 82.7(2) . . ? N7 Cu2 N6 119.0(2) . . ? N10 Cu2 N8 98.9(2) . . ? N9 Cu2 N8 81.8(2) . . ? N7 Cu2 N8 122.6(2) . . ? N6 Cu2 N8 113.2(2) . . ? C1 N1 C5 118.2(6) . . ? C1 N1 Cu1 128.1(5) . . ? C5 N1 Cu1 113.6(5) . . ? C7 N2 C11 118.9(6) . . ? C7 N2 Cu1 129.0(4) . . ? C11 N2 Cu1 111.8(4) . . ? C17 N3 C13 118.1(6) . . ? C17 N3 Cu1 114.4(5) . . ? C13 N3 Cu1 127.4(5) . . ? C12 N4 C18 111.3(6) . . ? C12 N4 C6 112.4(6) . . ? C18 N4 C6 111.7(6) . . ? C12 N4 Cu1 105.9(4) . . ? C18 N4 Cu1 108.6(4) . . ? C6 N4 Cu1 106.6(4) . . ? C19 N5 Cu1 176.0(6) . . ? C24 N6 C20 119.6(6) . . ? C24 N6 Cu2 112.8(4) . . ? C20 N6 Cu2 127.5(5) . . ? C30 N7 C26 119.0(6) . . ? C30 N7 Cu2 113.1(5) . . ? C26 N7 Cu2 127.6(5) . . ? C36 N8 C32 119.1(6) . . ? C36 N8 Cu2 112.2(4) . . ? C32 N8 Cu2 128.5(4) . . ? C31 N9 C37 111.8(5) . . ? C31 N9 C25 112.2(6) . . ? C37 N9 C25 111.0(6) . . ? C31 N9 Cu2 108.0(4) . . ? C37 N9 Cu2 106.7(4) . . ? C25 N9 Cu2 106.8(4) . . ? C40 N10 Cu2 174.6(5) . . ? N1 C1 C2 123.1(7) . . ? C3 C2 C1 118.1(8) . . ? C4 C3 C2 119.6(7) . . ? C3 C4 C5 120.1(7) . . ? N1 C5 C4 120.9(7) . . ? N1 C5 C6 114.5(6) . . ? C4 C5 C6 124.6(7) . . ? C5 C6 N4 110.4(6) . . ? N2 C7 C8 122.2(7) . . ? C7 C8 C9 118.7(7) . . ? C8 C9 C10 120.4(7) . . ? C9 C10 C11 118.2(7) . . ? N2 C11 C10 121.5(7) . . ? N2 C11 C12 114.6(6) . . ? C10 C11 C12 123.9(6) . . ? N4 C12 C11 110.0(5) . . ? N3 C13 C14 123.0(8) . . ? C15 C14 C13 117.5(8) . . ? C14 C15 C16 121.2(8) . . ? C17 C16 C15 117.4(8) . . ? N3 C17 C16 122.7(7) . . ? N3 C17 C18 115.0(6) . . ? C16 C17 C18 122.2(7) . . ? N4 C18 C17 111.5(6) . . ? N5 C19 Mo1 179.6(6) . . ? N6 C20 C21 121.3(7) . . ? C22 C21 C20 119.5(8) . . ? C21 C22 C23 119.7(7) . . ? C22 C23 C24 118.1(7) . . ? N6 C24 C23 121.8(7) . . ? N6 C24 C25 115.8(6) . . ? C23 C24 C25 122.1(7) . . ? N9 C25 C24 111.3(6) . . ? N7 C26 C27 122.2(7) . . ? C28 C27 C26 117.4(7) . . ? C27 C28 C29 121.3(7) . . ? C28 C29 C30 118.0(7) . . ? N7 C30 C29 122.1(7) . . ? N7 C30 C31 114.9(6) . . ? C29 C30 C31 122.9(6) . . ? N9 C31 C30 109.5(6) . . ? N8 C32 C33 122.1(6) . . ? C32 C33 C34 119.6(7) . . ? C33 C34 C35 118.3(7) . . ? C36 C35 C34 120.0(7) . . ? N8 C36 C35 120.8(6) . . ? N8 C36 C37 115.3(6) . . ? C35 C36 C37 123.8(6) . . ? N9 C37 C36 110.3(5) . . ? N11 C38 Mo1 178.4(6) . . ? N12 C39 Mo1 179.8(7) . . ? N10 C40 Mo1 179.9(7) . . ? N13 C41 Mo1 177.6(6) . . ? N14 C42 Mo1 178.9(6) . . ? N15 C43 Mo1 179.2(7) . . ? N16 C44 Mo1 178.8(7) . . ? _diffrn_measured_fraction_theta_max 0.991 _diffrn_reflns_theta_full 25.03 _diffrn_measured_fraction_theta_full 0.991 _refine_diff_density_max 0.659 _refine_diff_density_min -0.464 _refine_diff_density_rms 0.108 #end of cif data_5_ccdc_671021 _database_code_depnum_ccdc_archive 'CCDC 671021' #TrackingRef '1.cif' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C24 H52 Cu2 Mo N16 O4' _chemical_formula_weight 851.84 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' Cu Cu 0.3201 1.2651 '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 C2/c loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, y, -z+1/2' 'x+1/2, y+1/2, z' '-x+1/2, y+1/2, -z+1/2' '-x, -y, -z' 'x, -y, z-1/2' '-x+1/2, -y+1/2, -z' 'x+1/2, -y+1/2, z-1/2' _cell_length_a 14.1417(8) _cell_length_b 14.4240(9) _cell_length_c 18.5187(5) _cell_angle_alpha 90.00 _cell_angle_beta 106.966(2) _cell_angle_gamma 90.00 _cell_volume 3613.0(3) _cell_formula_units_Z 4 _cell_measurement_temperature 173(2) _cell_measurement_reflns_used 398 _cell_measurement_theta_min 4.1 _cell_measurement_theta_max 27.2 _exptl_crystal_description block _exptl_crystal_colour purple _exptl_crystal_size_max 0.30 _exptl_crystal_size_mid 0.30 _exptl_crystal_size_min 0.20 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.566 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1760 _exptl_absorpt_coefficient_mu 1.562 _exptl_absorpt_correction_type Multi-scan _exptl_absorpt_correction_T_min 0.202 _exptl_absorpt_correction_T_max 0.642 _exptl_absorpt_process_details SADABS _exptl_special_details ; ? ; _diffrn_ambient_temperature 173(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'Rigaku RAXIS-RAPID' _diffrn_measurement_method \w _diffrn_detector_area_resol_mean 5 _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 15670 _diffrn_reflns_av_R_equivalents 0.0987 _diffrn_reflns_av_sigmaI/netI 0.0671 _diffrn_reflns_limit_h_min -18 _diffrn_reflns_limit_h_max 18 _diffrn_reflns_limit_k_min -16 _diffrn_reflns_limit_k_max 18 _diffrn_reflns_limit_l_min -23 _diffrn_reflns_limit_l_max 23 _diffrn_reflns_theta_min 3.01 _diffrn_reflns_theta_max 27.33 _reflns_number_total 3943 _reflns_number_gt 3254 _reflns_threshold_expression >2sigma(I) _computing_data_collection PROCESS-AUTO _computing_cell_refinement PROCESS-AUTO _computing_data_reduction CrystalStructure _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'Bruker SHELXTL V5.1 (Sheldrick, 1998)' _computing_publication_material 'SHELXL-97 (Sheldrick, 1997)' _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^)+(0.0535P)^2^+13.6239P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment constr _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 3943 _refine_ls_number_parameters 233 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0669 _refine_ls_R_factor_gt 0.0502 _refine_ls_wR_factor_ref 0.1236 _refine_ls_wR_factor_gt 0.1150 _refine_ls_goodness_of_fit_ref 1.078 _refine_ls_restrained_S_all 1.078 _refine_ls_shift/su_max 0.000 _refine_ls_shift/su_mean 0.000 loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_occupancy _atom_site_symmetry_multiplicity _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group Mo1 Mo 0.0000 0.19573(3) 0.2500 0.01242(13) Uani 1 2 d S . . Cu1 Cu 0.30059(4) 0.44192(4) 0.36488(3) 0.02044(16) Uani 1 1 d . . . N1 N 0.2720(3) 0.4265(3) 0.2515(2) 0.0238(8) Uani 1 1 d . . . H1A H 0.2144 0.3955 0.2347 0.029 Uiso 1 1 calc R . . H1D H 0.2619 0.4834 0.2308 0.029 Uiso 1 1 calc R . . N2 N 0.3608(3) 0.3086(3) 0.38323(18) 0.0195(7) Uani 1 1 d . . . H2C H 0.3085 0.2690 0.3700 0.023 Uiso 1 1 calc R . . N3 N 0.3367(3) 0.4474(2) 0.4797(2) 0.0212(7) Uani 1 1 d . . . H3C H 0.3982 0.4728 0.4968 0.025 Uiso 1 1 calc R . . N4 N 0.2461(3) 0.5765(3) 0.3514(2) 0.0259(8) Uani 1 1 d . . . H4A H 0.2966 0.6138 0.3502 0.031 Uiso 1 1 calc R . . H4D H 0.2016 0.5796 0.3054 0.031 Uiso 1 1 calc R . . N5 N 0.1361(3) 0.3727(3) 0.3484(2) 0.0258(8) Uani 1 1 d . . . N6 N 0.2354(3) 0.1208(3) 0.3262(2) 0.0221(8) Uani 1 1 d . . . N7 N -0.0184(3) 0.0208(3) 0.3672(2) 0.0248(8) Uani 1 1 d . . . N8 N -0.1171(3) 0.2788(3) 0.3685(2) 0.0336(10) Uani 1 1 d . . . C1 C 0.3460(4) 0.3784(3) 0.2205(3) 0.0274(10) Uani 1 1 d . . . H1B H 0.4055 0.4158 0.2310 0.033 Uiso 1 1 calc R . . H1C H 0.3191 0.3729 0.1662 0.033 Uiso 1 1 calc R . . C2 C 0.3729(3) 0.2815(3) 0.2546(2) 0.0267(10) Uani 1 1 d . . . H2A H 0.3124 0.2459 0.2464 0.032 Uiso 1 1 calc R . . H2B H 0.4130 0.2507 0.2274 0.032 Uiso 1 1 calc R . . C3 C 0.4287(3) 0.2789(3) 0.3392(2) 0.0264(10) Uani 1 1 d . . . H3A H 0.4525 0.2166 0.3538 0.032 Uiso 1 1 calc R . . H3B H 0.4854 0.3201 0.3498 0.032 Uiso 1 1 calc R . . C4 C 0.4078(3) 0.2945(3) 0.4661(2) 0.0269(10) Uani 1 1 d . . . H4B H 0.4747 0.3186 0.4812 0.032 Uiso 1 1 calc R . . H4C H 0.4099 0.2291 0.4786 0.032 Uiso 1 1 calc R . . C5 C 0.3441(3) 0.3468(3) 0.5058(2) 0.0223(9) Uani 1 1 d . . . H5B H 0.3735 0.3437 0.5600 0.027 Uiso 1 1 calc R . . H5C H 0.2788 0.3193 0.4934 0.027 Uiso 1 1 calc R . . C6 C 0.2694(4) 0.5022(3) 0.5127(3) 0.0283(10) Uani 1 1 d . . . H6A H 0.2942 0.4997 0.5673 0.034 Uiso 1 1 calc R . . H6B H 0.2042 0.4741 0.4978 0.034 Uiso 1 1 calc R . . C7 C 0.2606(4) 0.6043(3) 0.4872(3) 0.0289(10) Uani 1 1 d . . . H7A H 0.2308 0.6396 0.5195 0.035 Uiso 1 1 calc R . . H7B H 0.3264 0.6289 0.4937 0.035 Uiso 1 1 calc R . . C8 C 0.1993(4) 0.6176(3) 0.4053(2) 0.0274(10) Uani 1 1 d . . . H8A H 0.1348 0.5896 0.3980 0.033 Uiso 1 1 calc R . . H8B H 0.1895 0.6834 0.3950 0.033 Uiso 1 1 calc R . . C9 C 0.0867(3) 0.3122(3) 0.3144(2) 0.0183(8) Uani 1 1 d . . . C10 C 0.1527(3) 0.1461(3) 0.3000(2) 0.0176(8) Uani 1 1 d . . . C11 C -0.0087(3) 0.0799(3) 0.3259(2) 0.0193(8) Uani 1 1 d . . . C12 C -0.0763(3) 0.2495(3) 0.3279(2) 0.0195(8) Uani 1 1 d . . . O1 O 0.4501(14) 0.959(2) 0.443(2) 0.134(14) Uani 0.61(5) 1 d P A 1 O1' O 0.4273(13) 1.0022(13) 0.3997(12) 0.064(7) Uani 0.39(5) 1 d P A 2 O2 O 0.0672(14) 0.5351(15) 0.183(3) 0.23(3) Uani 0.65(4) 1 d P B 1 O2' O 0.030(2) 0.5628(15) 0.2372(11) 0.074(11) Uani 0.35(4) 1 d P . 2 loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 Mo1 0.0101(2) 0.0153(2) 0.0117(2) 0.000 0.00304(16) 0.000 Cu1 0.0213(3) 0.0227(3) 0.0178(3) 0.00086(18) 0.0066(2) -0.0004(2) N1 0.0241(19) 0.024(2) 0.0238(19) 0.0044(14) 0.0080(15) -0.0059(16) N2 0.0160(17) 0.0243(19) 0.0157(16) -0.0025(13) 0.0009(13) -0.0026(15) N3 0.0186(18) 0.0220(19) 0.0239(18) 0.0032(14) 0.0076(14) 0.0001(15) N4 0.031(2) 0.031(2) 0.0194(18) 0.0015(15) 0.0120(15) -0.0017(17) N5 0.0188(19) 0.031(2) 0.029(2) -0.0047(16) 0.0084(15) -0.0041(16) N6 0.0177(19) 0.0245(19) 0.0247(18) -0.0027(14) 0.0071(14) -0.0031(15) N7 0.0213(19) 0.029(2) 0.0228(19) 0.0030(15) 0.0048(14) -0.0063(16) N8 0.027(2) 0.049(3) 0.028(2) -0.0062(18) 0.0140(17) -0.0014(19) C1 0.030(3) 0.032(3) 0.026(2) -0.0049(18) 0.0173(19) -0.009(2) C2 0.019(2) 0.038(3) 0.024(2) -0.0064(18) 0.0083(17) -0.0026(19) C3 0.016(2) 0.036(3) 0.027(2) -0.0055(18) 0.0050(17) 0.0015(19) C4 0.026(2) 0.031(3) 0.022(2) 0.0009(17) 0.0056(18) 0.003(2) C5 0.027(2) 0.021(2) 0.019(2) 0.0033(16) 0.0069(17) 0.0008(18) C6 0.035(3) 0.030(3) 0.024(2) 0.0040(18) 0.0133(19) 0.010(2) C7 0.033(3) 0.026(2) 0.029(2) -0.0022(18) 0.0096(19) 0.004(2) C8 0.030(3) 0.025(2) 0.027(2) 0.0045(18) 0.0083(19) 0.011(2) C9 0.0142(18) 0.023(2) 0.0170(19) 0.0009(15) 0.0035(14) 0.0009(17) C10 0.018(2) 0.020(2) 0.0162(19) -0.0024(15) 0.0064(15) -0.0026(16) C11 0.0135(19) 0.025(2) 0.0185(19) -0.0009(16) 0.0028(15) -0.0012(17) C12 0.018(2) 0.023(2) 0.018(2) -0.0037(15) 0.0059(16) -0.0008(17) O1 0.094(11) 0.15(2) 0.15(3) -0.09(2) 0.022(13) -0.014(12) O1' 0.057(9) 0.056(10) 0.055(11) -0.006(8) -0.020(7) -0.001(7) O2 0.064(10) 0.094(12) 0.45(7) 0.04(2) -0.08(2) -0.004(9) O2' 0.048(15) 0.056(10) 0.082(18) -0.010(8) -0.035(11) -0.002(7) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag Mo1 C12 2.180(4) . ? Mo1 C12 2.180(4) 2 ? Mo1 C10 2.206(4) 2 ? Mo1 C10 2.206(4) . ? Mo1 C11 2.209(4) 2 ? Mo1 C11 2.209(4) . ? Mo1 C9 2.212(4) . ? Mo1 C9 2.212(4) 2 ? Cu1 N1 2.031(4) . ? Cu1 N3 2.038(4) . ? Cu1 N4 2.077(4) . ? Cu1 N2 2.090(4) . ? Cu1 N5 2.467(4) . ? N1 C1 1.502(6) . ? N2 C3 1.492(5) . ? N2 C4 1.498(5) . ? N3 C6 1.499(5) . ? N3 C5 1.523(5) . ? N4 C8 1.474(5) . ? N5 C9 1.179(6) . ? N6 C10 1.186(5) . ? N7 C11 1.179(6) . ? N8 C12 1.155(5) . ? C1 C2 1.536(7) . ? C2 C3 1.535(6) . ? C4 C5 1.518(6) . ? C6 C7 1.541(6) . ? C7 C8 1.523(6) . ? O2' O2' 1.09(7) 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 C12 Mo1 C12 138.3(2) . 2 ? C12 Mo1 C10 77.33(15) . 2 ? C12 Mo1 C10 116.77(15) 2 2 ? C12 Mo1 C10 116.77(15) . . ? C12 Mo1 C10 77.33(15) 2 . ? C10 Mo1 C10 142.1(2) 2 . ? C12 Mo1 C11 145.07(15) . 2 ? C12 Mo1 C11 73.65(15) 2 2 ? C10 Mo1 C11 73.54(15) 2 2 ? C10 Mo1 C11 78.01(15) . 2 ? C12 Mo1 C11 73.65(15) . . ? C12 Mo1 C11 145.07(15) 2 . ? C10 Mo1 C11 78.01(15) 2 . ? C10 Mo1 C11 73.54(15) . . ? C11 Mo1 C11 81.7(2) 2 . ? C12 Mo1 C9 71.13(15) . . ? C12 Mo1 C9 77.47(15) 2 . ? C10 Mo1 C9 142.51(14) 2 . ? C10 Mo1 C9 72.52(15) . . ? C11 Mo1 C9 142.39(14) 2 . ? C11 Mo1 C9 110.88(15) . . ? C12 Mo1 C9 77.47(15) . 2 ? C12 Mo1 C9 71.13(15) 2 2 ? C10 Mo1 C9 72.52(15) 2 2 ? C10 Mo1 C9 142.51(15) . 2 ? C11 Mo1 C9 110.88(15) 2 2 ? C11 Mo1 C9 142.39(14) . 2 ? C9 Mo1 C9 81.2(2) . 2 ? N1 Cu1 N3 175.05(15) . . ? N1 Cu1 N4 91.33(15) . . ? N3 Cu1 N4 93.46(14) . . ? N1 Cu1 N2 90.91(14) . . ? N3 Cu1 N2 84.26(13) . . ? N4 Cu1 N2 177.18(15) . . ? N1 Cu1 N5 86.06(13) . . ? N3 Cu1 N5 94.90(13) . . ? N4 Cu1 N5 93.43(15) . . ? N2 Cu1 N5 88.43(14) . . ? C1 N1 Cu1 119.6(3) . . ? C3 N2 C4 110.9(3) . . ? C3 N2 Cu1 118.2(3) . . ? C4 N2 Cu1 109.2(3) . . ? C6 N3 C5 111.4(3) . . ? C6 N3 Cu1 116.8(3) . . ? C5 N3 Cu1 105.5(2) . . ? C8 N4 Cu1 121.2(3) . . ? C9 N5 Cu1 139.1(3) . . ? N1 C1 C2 112.3(3) . . ? C3 C2 C1 115.7(4) . . ? N2 C3 C2 109.2(3) . . ? N2 C4 C5 106.2(4) . . ? C4 C5 N3 108.4(3) . . ? N3 C6 C7 112.5(4) . . ? C8 C7 C6 113.4(4) . . ? N4 C8 C7 112.7(4) . . ? N5 C9 Mo1 177.5(4) . . ? N6 C10 Mo1 178.7(4) . . ? N7 C11 Mo1 175.7(4) . . ? N8 C12 Mo1 179.2(4) . . ? _diffrn_measured_fraction_theta_max 0.966 _diffrn_reflns_theta_full 27.33 _diffrn_measured_fraction_theta_full 0.966 _refine_diff_density_max 0.900 _refine_diff_density_min -1.258 _refine_diff_density_rms 0.130 #end of cif data_7_ccdc_671022 _database_code_depnum_ccdc_archive 'CCDC 671022' #TrackingRef '1.cif' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C44 H36 Cl Cu2 Mo N16 O4' _chemical_formula_weight 1111.36 loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Cl Cl 0.1484 0.1585 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Cu Cu 0.3201 1.2651 '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)/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 18.132(3) _cell_length_b 17.736(2) _cell_length_c 15.286(2) _cell_angle_alpha 90.00 _cell_angle_beta 110.075(2) _cell_angle_gamma 90.00 _cell_volume 4617(1) _cell_formula_units_Z 4 _cell_measurement_temperature 123(2) _cell_measurement_reflns_used 13340 _cell_measurement_theta_min 3.0 _cell_measurement_theta_max 27.5 _exptl_crystal_description block _exptl_crystal_colour green _exptl_crystal_size_max 0.10 _exptl_crystal_size_mid 0.10 _exptl_crystal_size_min 0.08 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.599 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 2244 _exptl_absorpt_coefficient_mu 1.300 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.859 _exptl_absorpt_correction_T_max 0.958 _exptl_absorpt_process_details ? _exptl_special_details ; Jacobson, R. (1998) Private communication ; _diffrn_ambient_temperature 123(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'Rigaku Saturn' _diffrn_measurement_method \w _diffrn_detector_area_resol_mean 7.31 _diffrn_standards_number 36616 _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 36616 _diffrn_reflns_av_R_equivalents 0.0443 _diffrn_reflns_av_sigmaI/netI 0.0438 _diffrn_reflns_limit_h_min -23 _diffrn_reflns_limit_h_max 23 _diffrn_reflns_limit_k_min -22 _diffrn_reflns_limit_k_max 21 _diffrn_reflns_limit_l_min -18 _diffrn_reflns_limit_l_max 19 _diffrn_reflns_theta_min 3.02 _diffrn_reflns_theta_max 27.48 _reflns_number_total 10520 _reflns_number_gt 8601 _reflns_threshold_expression >2sigma(I) _computing_data_collection CrystalClear _computing_cell_refinement CrystalClear _computing_data_reduction CrystalStructure _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics ? _computing_publication_material ? _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^)+(0.0367P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment constr _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 10520 _refine_ls_number_parameters 613 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0450 _refine_ls_R_factor_gt 0.0322 _refine_ls_wR_factor_ref 0.0781 _refine_ls_wR_factor_gt 0.0727 _refine_ls_goodness_of_fit_ref 1.046 _refine_ls_restrained_S_all 1.046 _refine_ls_shift/su_max 0.002 _refine_ls_shift/su_mean 0.000 loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_occupancy _atom_site_symmetry_multiplicity _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group Mo1 Mo 0.249524(10) 0.545406(10) 0.753272(11) 0.00798(5) Uani 1 1 d . . . Cu1 Cu 0.454153(15) 0.686175(14) 0.646831(18) 0.01318(7) Uani 1 1 d . . . Cu2 Cu 0.047633(15) 0.671479(14) 0.875552(18) 0.01198(7) Uani 1 1 d . . . Cl1 Cl 0.25760(3) 0.41839(3) 0.23262(4) 0.01854(12) Uani 1 1 d . . . N1 N 0.46603(11) 0.63283(10) 0.53446(13) 0.0163(4) Uani 1 1 d . . . N2 N 0.53670(11) 0.67884(9) 0.77929(12) 0.0151(4) Uani 1 1 d . . . N3 N 0.39201(11) 0.78574(10) 0.63057(13) 0.0176(4) Uani 1 1 d . . . N4 N 0.53542(10) 0.75488(9) 0.62715(12) 0.0115(4) Uani 1 1 d . . . N5 N 0.37461(11) 0.62013(10) 0.66456(13) 0.0181(4) Uani 1 1 d . . . N6 N -0.03336(11) 0.65983(10) 0.74230(12) 0.0149(4) Uani 1 1 d . . . N7 N 0.10815(11) 0.77177(9) 0.88654(13) 0.0168(4) Uani 1 1 d . . . N8 N 0.03226(10) 0.62108(9) 0.98887(12) 0.0133(4) Uani 1 1 d . . . N9 N -0.03533(10) 0.74204(9) 0.88853(11) 0.0109(4) Uani 1 1 d . . . N10 N 0.12785(11) 0.60485(9) 0.85838(12) 0.0146(4) Uani 1 1 d . . . N11 N 0.15765(11) 0.69597(10) 0.63906(14) 0.0221(4) Uani 1 1 d . . . N12 N 0.33630(11) 0.69366(10) 0.87840(14) 0.0227(5) Uani 1 1 d . . . N13 N 0.21685(12) 0.39016(11) 0.85394(14) 0.0231(5) Uani 1 1 d . . . N14 N 0.07815(11) 0.48080(10) 0.61420(14) 0.0208(4) Uani 1 1 d . . . N15 N 0.28998(12) 0.41099(11) 0.62669(14) 0.0245(5) Uani 1 1 d . . . N16 N 0.42335(11) 0.48505(10) 0.88941(14) 0.0215(4) Uani 1 1 d . . . C1 C 0.41617(15) 0.58332(13) 0.47736(17) 0.0262(6) Uani 1 1 d . . . H1A H 0.3714 0.5691 0.4898 0.031 Uiso 1 1 calc R . . C2 C 0.42917(18) 0.55296(14) 0.40122(19) 0.0381(7) Uani 1 1 d . . . H2A H 0.3936 0.5192 0.3623 0.046 Uiso 1 1 calc R . . C3 C 0.49624(19) 0.57360(14) 0.38369(18) 0.0390(7) Uani 1 1 d . . . H3A H 0.5065 0.5534 0.3329 0.047 Uiso 1 1 calc R . . C4 C 0.54783(16) 0.62420(13) 0.44156(17) 0.0262(6) Uani 1 1 d . . . H4A H 0.5934 0.6383 0.4309 0.031 Uiso 1 1 calc R . . C5 C 0.53030(13) 0.65369(11) 0.51618(16) 0.0157(5) Uani 1 1 d . . . C6 C 0.58236(12) 0.70834(12) 0.58395(15) 0.0146(5) Uani 1 1 d . . . H6A H 0.6227 0.6811 0.6321 0.017 Uiso 1 1 calc R . . H6B H 0.6079 0.7409 0.5521 0.017 Uiso 1 1 calc R . . C7 C 0.54106(14) 0.62728(12) 0.84556(16) 0.0206(5) Uani 1 1 d . . . H7A H 0.4994 0.5940 0.8363 0.025 Uiso 1 1 calc R . . C8 C 0.60470(15) 0.62209(13) 0.92618(16) 0.0224(5) Uani 1 1 d . . . H8A H 0.6060 0.5859 0.9708 0.027 Uiso 1 1 calc R . . C9 C 0.66687(15) 0.67118(13) 0.94037(16) 0.0237(6) Uani 1 1 d . . . H9A H 0.7109 0.6681 0.9941 0.028 Uiso 1 1 calc R . . C10 C 0.66242(14) 0.72502(12) 0.87313(15) 0.0186(5) Uani 1 1 d . . . H10B H 0.7033 0.7590 0.8814 0.022 Uiso 1 1 calc R . . C11 C 0.59642(13) 0.72760(11) 0.79355(14) 0.0145(5) Uani 1 1 d . . . C12 C 0.58573(13) 0.78536(12) 0.71838(14) 0.0151(5) Uani 1 1 d . . . H12A H 0.5617 0.8303 0.7329 0.018 Uiso 1 1 calc R . . H12B H 0.6365 0.7993 0.7153 0.018 Uiso 1 1 calc R . . C13 C 0.32975(14) 0.80238(13) 0.65479(18) 0.0253(6) Uani 1 1 d . . . H13A H 0.3080 0.7649 0.6809 0.030 Uiso 1 1 calc R . . C14 C 0.29653(15) 0.87377(13) 0.64225(18) 0.0277(6) Uani 1 1 d . . . H14A H 0.2532 0.8841 0.6596 0.033 Uiso 1 1 calc R . . C15 C 0.32914(14) 0.92939(13) 0.60338(17) 0.0239(5) Uani 1 1 d . . . H15A H 0.3075 0.9775 0.5937 0.029 Uiso 1 1 calc R . . C16 C 0.39421(14) 0.91273(12) 0.57909(15) 0.0187(5) Uani 1 1 d . . . H16A H 0.4175 0.9495 0.5538 0.022 Uiso 1 1 calc R . . C17 C 0.42387(13) 0.83994(12) 0.59329(15) 0.0140(5) Uani 1 1 d . . . C18 C 0.49099(12) 0.81529(11) 0.56398(15) 0.0136(4) Uani 1 1 d . . . H18A H 0.4712 0.7967 0.5004 0.016 Uiso 1 1 calc R . . H18B H 0.5253 0.8578 0.5664 0.016 Uiso 1 1 calc R . . C19 C -0.03410(14) 0.60858(12) 0.67700(15) 0.0173(5) Uani 1 1 d . . . H19A H 0.0065 0.5736 0.6906 0.021 Uiso 1 1 calc R . . C20 C -0.09224(14) 0.60572(12) 0.59128(16) 0.0205(5) Uani 1 1 d . . . H20A H -0.0909 0.5699 0.5475 0.025 Uiso 1 1 calc R . . C21 C -0.15295(14) 0.65732(12) 0.57143(16) 0.0207(5) Uani 1 1 d . . . H21A H -0.1938 0.6558 0.5145 0.025 Uiso 1 1 calc R . . C22 C -0.15223(13) 0.71120(12) 0.63708(15) 0.0164(5) Uani 1 1 d . . . H22A H -0.1921 0.7469 0.6246 0.020 Uiso 1 1 calc R . . C23 C -0.09107(13) 0.71100(11) 0.72176(15) 0.0134(4) Uani 1 1 d . . . C24 C -0.08378(13) 0.77022(12) 0.79511(14) 0.0150(5) Uani 1 1 d . . . H24A H -0.0598 0.8152 0.7806 0.018 Uiso 1 1 calc R . . H24B H -0.1356 0.7836 0.7953 0.018 Uiso 1 1 calc R . . C25 C 0.16994(14) 0.78728(13) 0.86154(17) 0.0233(5) Uani 1 1 d . . . H25A H 0.1924 0.7486 0.8381 0.028 Uiso 1 1 calc R . . C26 C 0.20199(15) 0.85887(13) 0.86921(18) 0.0271(6) Uani 1 1 d . . . H26A H 0.2449 0.8682 0.8507 0.033 Uiso 1 1 calc R . . C27 C 0.16907(15) 0.91620(13) 0.90494(17) 0.0249(6) Uani 1 1 d . . . H27A H 0.1901 0.9646 0.9118 0.030 Uiso 1 1 calc R . . C28 C 0.10434(13) 0.90055(12) 0.93032(15) 0.0177(5) Uani 1 1 d . . . H28A H 0.0807 0.9384 0.9536 0.021 Uiso 1 1 calc R . . C29 C 0.07542(13) 0.82786(11) 0.92045(14) 0.0133(4) Uani 1 1 d . . . C30 C 0.00755(12) 0.80485(11) 0.94930(14) 0.0126(4) Uani 1 1 d . . . H30A H 0.0265 0.7887 1.0138 0.015 Uiso 1 1 calc R . . H30B H -0.0275 0.8473 0.9436 0.015 Uiso 1 1 calc R . . C31 C 0.07937(13) 0.57155(12) 1.04900(15) 0.0179(5) Uani 1 1 d . . . H31A H 0.1241 0.5545 1.0386 0.022 Uiso 1 1 calc R . . C32 C 0.06366(14) 0.54511(13) 1.12562(16) 0.0227(5) Uani 1 1 d . . . H32A H 0.0978 0.5116 1.1668 0.027 Uiso 1 1 calc R . . C33 C -0.00373(15) 0.56926(13) 1.14004(17) 0.0245(6) Uani 1 1 d . . . H33A H -0.0158 0.5517 1.1909 0.029 Uiso 1 1 calc R . . C34 C -0.05290(14) 0.61953(12) 1.07851(16) 0.0188(5) Uani 1 1 d . . . H34A H -0.0987 0.6360 1.0869 0.023 Uiso 1 1 calc R . . C35 C -0.03283(13) 0.64515(11) 1.00387(15) 0.0133(4) Uani 1 1 d . . . C36 C -0.08349(12) 0.69849(12) 0.93196(15) 0.0142(5) Uani 1 1 d . . . H36A H -0.1233 0.6703 0.8844 0.017 Uiso 1 1 calc R . . H36B H -0.1098 0.7329 0.9610 0.017 Uiso 1 1 calc R . . C37 C 0.32922(13) 0.59213(11) 0.69033(15) 0.0138(4) Uani 1 1 d . . . C38 C 0.17144(13) 0.58060(11) 0.82673(14) 0.0125(4) Uani 1 1 d . . . C39 C 0.18936(12) 0.64254(12) 0.67559(15) 0.0130(4) Uani 1 1 d . . . C40 C 0.30611(12) 0.64098(12) 0.83808(15) 0.0139(5) Uani 1 1 d . . . C41 C 0.22877(12) 0.44435(12) 0.82038(15) 0.0141(5) Uani 1 1 d . . . C42 C 0.13736(13) 0.50434(11) 0.66184(15) 0.0136(4) Uani 1 1 d . . . C43 C 0.27503(12) 0.45740(12) 0.66983(15) 0.0143(5) Uani 1 1 d . . . C44 C 0.36230(13) 0.50612(11) 0.84305(15) 0.0132(4) Uani 1 1 d . . . O1 O 0.23210(11) 0.46477(11) 0.29317(14) 0.0435(5) Uani 1 1 d . . . O2 O 0.24475(9) 0.33995(10) 0.24830(11) 0.0266(4) Uani 1 1 d . . . O3 O 0.21324(10) 0.43720(9) 0.13675(11) 0.0277(4) Uani 1 1 d . . . O4 O 0.34004(9) 0.43033(8) 0.24989(11) 0.0211(4) Uani 1 1 d . . . 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 0.00728(9) 0.00795(10) 0.00949(9) 0.00015(7) 0.00387(7) -0.00001(7) Cu1 0.01303(14) 0.01189(14) 0.01751(14) 0.00231(11) 0.00896(11) -0.00128(10) Cu2 0.01155(14) 0.01173(14) 0.01466(13) -0.00212(11) 0.00708(11) 0.00116(10) Cl1 0.0148(3) 0.0197(3) 0.0218(3) -0.0016(2) 0.0072(2) 0.0014(2) N1 0.0166(10) 0.0147(9) 0.0183(10) -0.0017(8) 0.0071(8) -0.0016(8) N2 0.0188(10) 0.0139(9) 0.0154(9) 0.0034(8) 0.0093(8) 0.0038(8) N3 0.0179(10) 0.0152(9) 0.0233(10) 0.0049(8) 0.0117(9) 0.0022(8) N4 0.0124(9) 0.0112(9) 0.0108(9) 0.0013(7) 0.0036(7) -0.0006(7) N5 0.0182(11) 0.0146(10) 0.0254(11) 0.0042(8) 0.0124(9) 0.0019(8) N6 0.0176(10) 0.0137(9) 0.0157(9) -0.0037(8) 0.0085(8) -0.0019(8) N7 0.0182(10) 0.0131(9) 0.0219(10) -0.0031(8) 0.0103(8) -0.0012(8) N8 0.0145(10) 0.0121(9) 0.0153(9) -0.0003(7) 0.0078(8) 0.0007(7) N9 0.0099(9) 0.0112(9) 0.0108(9) -0.0026(7) 0.0024(7) 0.0003(7) N10 0.0155(10) 0.0127(9) 0.0175(9) -0.0018(8) 0.0080(8) -0.0006(8) N11 0.0173(11) 0.0200(10) 0.0228(11) 0.0017(9) -0.0010(9) 0.0010(9) N12 0.0177(11) 0.0201(10) 0.0235(11) -0.0043(9) -0.0015(9) -0.0001(9) N13 0.0230(12) 0.0214(11) 0.0237(11) 0.0061(9) 0.0063(9) -0.0035(9) N14 0.0181(11) 0.0201(10) 0.0234(11) -0.0062(9) 0.0059(9) -0.0007(8) N15 0.0218(11) 0.0259(11) 0.0270(11) -0.0088(9) 0.0097(9) 0.0025(9) N16 0.0189(11) 0.0172(10) 0.0274(11) 0.0054(9) 0.0069(9) 0.0013(8) C1 0.0238(14) 0.0209(13) 0.0302(14) -0.0052(11) 0.0045(11) -0.0089(10) C2 0.053(2) 0.0282(15) 0.0274(15) -0.0123(12) 0.0070(14) -0.0137(14) C3 0.071(2) 0.0260(15) 0.0278(15) -0.0111(12) 0.0276(15) -0.0040(14) C4 0.0403(16) 0.0202(13) 0.0255(13) -0.0010(11) 0.0208(12) -0.0009(11) C5 0.0189(12) 0.0107(11) 0.0188(11) 0.0017(9) 0.0084(10) 0.0002(9) C6 0.0109(11) 0.0174(11) 0.0174(11) 0.0028(9) 0.0074(9) 0.0009(9) C7 0.0259(14) 0.0176(12) 0.0246(13) 0.0074(10) 0.0166(11) 0.0059(10) C8 0.0386(16) 0.0162(12) 0.0163(12) 0.0050(10) 0.0145(11) 0.0086(11) C9 0.0355(16) 0.0206(12) 0.0114(11) -0.0028(10) 0.0035(11) 0.0117(11) C10 0.0245(13) 0.0144(11) 0.0151(11) -0.0033(9) 0.0044(10) 0.0022(10) C11 0.0198(12) 0.0121(11) 0.0119(10) -0.0006(9) 0.0060(9) 0.0030(9) C12 0.0171(12) 0.0131(11) 0.0128(11) -0.0005(9) 0.0021(9) -0.0025(9) C13 0.0235(14) 0.0208(12) 0.0378(15) 0.0077(11) 0.0187(12) 0.0030(10) C14 0.0220(14) 0.0282(14) 0.0387(15) 0.0025(12) 0.0181(12) 0.0073(11) C15 0.0279(14) 0.0159(12) 0.0297(14) 0.0016(11) 0.0123(12) 0.0088(10) C16 0.0239(13) 0.0123(11) 0.0202(12) 0.0023(9) 0.0078(10) 0.0008(9) C17 0.0127(11) 0.0153(11) 0.0128(10) -0.0008(9) 0.0028(9) 0.0000(9) C18 0.0149(11) 0.0131(11) 0.0127(10) 0.0018(9) 0.0047(9) 0.0004(9) C19 0.0242(13) 0.0128(11) 0.0197(12) -0.0025(9) 0.0134(10) 0.0001(9) C20 0.0337(15) 0.0157(12) 0.0163(11) -0.0038(10) 0.0139(11) -0.0067(10) C21 0.0288(14) 0.0182(12) 0.0131(11) -0.0008(9) 0.0047(10) -0.0084(10) C22 0.0195(12) 0.0138(11) 0.0143(11) 0.0027(9) 0.0037(9) -0.0019(9) C23 0.0157(12) 0.0119(11) 0.0142(11) 0.0005(9) 0.0073(9) -0.0014(9) C24 0.0163(12) 0.0141(11) 0.0124(11) -0.0017(9) 0.0020(9) 0.0011(9) C25 0.0223(13) 0.0170(12) 0.0366(15) -0.0057(11) 0.0178(12) -0.0005(10) C26 0.0246(14) 0.0242(13) 0.0399(16) -0.0014(12) 0.0207(12) -0.0056(11) C27 0.0309(15) 0.0140(12) 0.0340(14) -0.0015(11) 0.0165(12) -0.0059(10) C28 0.0207(13) 0.0125(11) 0.0216(12) -0.0026(9) 0.0094(10) 0.0003(9) C29 0.0145(11) 0.0141(11) 0.0107(10) 0.0000(9) 0.0037(9) 0.0004(9) C30 0.0158(11) 0.0106(10) 0.0127(10) -0.0041(9) 0.0066(9) -0.0007(9) C31 0.0141(12) 0.0183(11) 0.0216(12) 0.0003(10) 0.0064(10) 0.0040(9) C32 0.0238(13) 0.0229(13) 0.0210(12) 0.0068(10) 0.0070(10) 0.0065(10) C33 0.0360(15) 0.0197(12) 0.0225(13) 0.0074(10) 0.0159(12) 0.0006(11) C34 0.0203(12) 0.0172(12) 0.0247(12) -0.0010(10) 0.0150(10) -0.0006(10) C35 0.0136(11) 0.0108(10) 0.0162(11) -0.0034(9) 0.0063(9) -0.0005(8) C36 0.0110(11) 0.0153(11) 0.0176(11) -0.0011(9) 0.0065(9) 0.0006(9) C37 0.0134(11) 0.0102(10) 0.0181(11) 0.0023(9) 0.0057(9) 0.0027(9) C38 0.0141(11) 0.0106(10) 0.0124(10) 0.0003(9) 0.0041(9) -0.0027(9) C39 0.0107(11) 0.0145(11) 0.0124(10) -0.0005(9) 0.0022(9) -0.0021(9) C40 0.0101(11) 0.0135(11) 0.0166(11) 0.0019(9) 0.0025(9) 0.0039(9) C41 0.0115(11) 0.0165(11) 0.0135(11) -0.0009(9) 0.0031(9) 0.0001(9) C42 0.0151(12) 0.0123(11) 0.0148(11) -0.0001(9) 0.0071(9) 0.0035(9) C43 0.0135(11) 0.0143(11) 0.0153(11) -0.0012(9) 0.0053(9) -0.0010(9) C44 0.0138(12) 0.0111(11) 0.0167(11) 0.0027(9) 0.0079(9) -0.0005(9) O1 0.0419(13) 0.0540(13) 0.0429(12) -0.0128(10) 0.0251(10) 0.0118(10) O2 0.0197(10) 0.0251(9) 0.0333(10) 0.0106(7) 0.0070(8) -0.0043(7) O3 0.0218(10) 0.0282(9) 0.0271(10) 0.0089(8) 0.0008(8) -0.0017(7) O4 0.0143(9) 0.0207(8) 0.0267(9) -0.0073(7) 0.0049(7) -0.0037(7) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag Mo1 C44 2.150(2) . ? Mo1 C37 2.158(2) . ? Mo1 C42 2.161(2) . ? Mo1 C41 2.161(2) . ? Mo1 C39 2.163(2) . ? Mo1 C43 2.164(2) . ? Mo1 C40 2.167(2) . ? Mo1 C38 2.179(2) . ? Cu1 N5 1.9478(18) . ? Cu1 N4 2.0127(17) . ? Cu1 N1 2.0362(18) . ? Cu1 N3 2.0634(18) . ? Cu1 N2 2.068(2) . ? Cu2 N10 1.9604(18) . ? Cu2 N9 2.0183(17) . ? Cu2 N8 2.0515(18) . ? Cu2 N7 2.0663(18) . ? Cu2 N6 2.072(2) . ? Cl1 O1 1.4285(18) . ? Cl1 O4 1.4416(16) . ? Cl1 O2 1.4442(18) . ? Cl1 O3 1.4479(17) . ? N1 C5 1.340(3) . ? N1 C1 1.345(3) . ? N2 C11 1.344(3) . ? N2 C7 1.347(3) . ? N3 C13 1.336(3) . ? N3 C17 1.345(3) . ? N4 C18 1.482(3) . ? N4 C12 1.482(3) . ? N4 C6 1.493(3) . ? N5 C37 1.141(3) . ? N6 C23 1.339(3) . ? N6 C19 1.347(3) . ? N7 C25 1.331(3) . ? N7 C29 1.350(3) . ? N8 C31 1.344(3) . ? N8 C35 1.347(3) . ? N9 C36 1.482(3) . ? N9 C24 1.483(3) . ? N9 C30 1.487(3) . ? N10 C38 1.143(3) . ? N11 C39 1.149(3) . ? N12 C40 1.149(3) . ? N13 C41 1.144(3) . ? N14 C42 1.149(3) . ? N15 C43 1.144(3) . ? N16 C44 1.153(3) . ? C1 C2 1.374(4) . ? C2 C3 1.381(4) . ? C3 C4 1.377(4) . ? C4 C5 1.387(3) . ? C5 C6 1.494(3) . ? C7 C8 1.372(3) . ? C8 C9 1.381(3) . ? C9 C10 1.385(3) . ? C10 C11 1.384(3) . ? C11 C12 1.501(3) . ? C13 C14 1.387(3) . ? C14 C15 1.385(3) . ? C15 C16 1.385(3) . ? C16 C17 1.387(3) . ? C17 C18 1.499(3) . ? C19 C20 1.372(3) . ? C20 C21 1.383(3) . ? C21 C22 1.382(3) . ? C22 C23 1.386(3) . ? C23 C24 1.509(3) . ? C25 C26 1.384(3) . ? C26 C27 1.383(3) . ? C27 C28 1.385(3) . ? C28 C29 1.380(3) . ? C29 C30 1.499(3) . ? C31 C32 1.379(3) . ? C32 C33 1.382(3) . ? C33 C34 1.378(3) . ? C34 C35 1.388(3) . ? C35 C36 1.501(3) . ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag C44 Mo1 C37 76.90(8) . . ? C44 Mo1 C42 141.39(8) . . ? C37 Mo1 C42 117.83(8) . . ? C44 Mo1 C41 73.19(8) . . ? C37 Mo1 C41 141.49(8) . . ? C42 Mo1 C41 75.46(8) . . ? C44 Mo1 C39 142.98(8) . . ? C37 Mo1 C39 74.82(8) . . ? C42 Mo1 C39 74.22(8) . . ? C41 Mo1 C39 141.62(8) . . ? C44 Mo1 C43 78.09(8) . . ? C37 Mo1 C43 72.71(8) . . ? C42 Mo1 C43 73.72(8) . . ? C41 Mo1 C43 77.81(8) . . ? C39 Mo1 C43 114.87(8) . . ? C44 Mo1 C40 73.76(8) . . ? C37 Mo1 C40 73.39(8) . . ? C42 Mo1 C40 142.95(8) . . ? C41 Mo1 C40 119.25(8) . . ? C39 Mo1 C40 75.60(8) . . ? C43 Mo1 C40 139.82(8) . . ? C44 Mo1 C38 114.07(8) . . ? C37 Mo1 C38 140.62(8) . . ? C42 Mo1 C38 78.23(8) . . ? C41 Mo1 C38 75.12(8) . . ? C39 Mo1 C38 76.12(8) . . ? C43 Mo1 C38 144.95(8) . . ? C40 Mo1 C38 74.07(8) . . ? N5 Cu1 N4 179.34(8) . . ? N5 Cu1 N1 97.80(8) . . ? N4 Cu1 N1 81.97(7) . . ? N5 Cu1 N3 97.56(7) . . ? N4 Cu1 N3 82.03(7) . . ? N1 Cu1 N3 120.50(7) . . ? N5 Cu1 N2 98.49(8) . . ? N4 Cu1 N2 82.15(7) . . ? N1 Cu1 N2 123.11(7) . . ? N3 Cu1 N2 110.71(7) . . ? N10 Cu2 N9 177.78(7) . . ? N10 Cu2 N8 99.94(7) . . ? N9 Cu2 N8 82.26(7) . . ? N10 Cu2 N7 97.59(7) . . ? N9 Cu2 N7 81.44(7) . . ? N8 Cu2 N7 121.92(7) . . ? N10 Cu2 N6 96.68(7) . . ? N9 Cu2 N6 81.83(7) . . ? N8 Cu2 N6 122.05(7) . . ? N7 Cu2 N6 110.07(7) . . ? O1 Cl1 O4 110.03(11) . . ? O1 Cl1 O2 109.92(11) . . ? O4 Cl1 O2 109.10(9) . . ? O1 Cl1 O3 109.41(11) . . ? O4 Cl1 O3 109.41(10) . . ? O2 Cl1 O3 108.95(10) . . ? C5 N1 C1 118.9(2) . . ? C5 N1 Cu1 113.51(14) . . ? C1 N1 Cu1 127.49(17) . . ? C11 N2 C7 118.6(2) . . ? C11 N2 Cu1 112.98(14) . . ? C7 N2 Cu1 127.96(16) . . ? C13 N3 C17 119.09(19) . . ? C13 N3 Cu1 129.35(15) . . ? C17 N3 Cu1 111.50(15) . . ? C18 N4 C12 111.78(16) . . ? C18 N4 C6 112.12(16) . . ? C12 N4 C6 110.97(17) . . ? C18 N4 Cu1 105.85(13) . . ? C12 N4 Cu1 109.03(13) . . ? C6 N4 Cu1 106.81(12) . . ? C37 N5 Cu1 165.05(19) . . ? C23 N6 C19 118.41(19) . . ? C23 N6 Cu2 113.33(14) . . ? C19 N6 Cu2 128.26(15) . . ? C25 N7 C29 118.84(19) . . ? C25 N7 Cu2 129.10(15) . . ? C29 N7 Cu2 111.99(14) . . ? C31 N8 C35 118.62(19) . . ? C31 N8 Cu2 128.57(15) . . ? C35 N8 Cu2 112.75(14) . . ? C36 N9 C24 111.19(16) . . ? C36 N9 C30 111.87(16) . . ? C24 N9 C30 111.03(16) . . ? C36 N9 Cu2 107.12(12) . . ? C24 N9 Cu2 109.24(13) . . ? C30 N9 Cu2 106.16(12) . . ? C38 N10 Cu2 159.43(17) . . ? N1 C1 C2 122.2(2) . . ? C1 C2 C3 118.6(2) . . ? C4 C3 C2 119.8(2) . . ? C3 C4 C5 118.5(2) . . ? N1 C5 C4 121.9(2) . . ? N1 C5 C6 114.97(19) . . ? C4 C5 C6 123.1(2) . . ? N4 C6 C5 110.19(17) . . ? N2 C7 C8 122.4(2) . . ? C7 C8 C9 119.2(2) . . ? C8 C9 C10 118.8(2) . . ? C11 C10 C9 119.2(2) . . ? N2 C11 C10 121.8(2) . . ? N2 C11 C12 115.46(19) . . ? C10 C11 C12 122.7(2) . . ? N4 C12 C11 110.32(17) . . ? N3 C13 C14 122.1(2) . . ? C15 C14 C13 118.7(2) . . ? C14 C15 C16 119.5(2) . . ? C15 C16 C17 118.5(2) . . ? N3 C17 C16 122.1(2) . . ? N3 C17 C18 115.42(18) . . ? C16 C17 C18 122.4(2) . . ? N4 C18 C17 109.36(17) . . ? N6 C19 C20 122.8(2) . . ? C19 C20 C21 118.6(2) . . ? C22 C21 C20 119.3(2) . . ? C21 C22 C23 118.8(2) . . ? N6 C23 C22 122.10(19) . . ? N6 C23 C24 115.83(19) . . ? C22 C23 C24 122.03(19) . . ? N9 C24 C23 110.65(17) . . ? N7 C25 C26 122.4(2) . . ? C27 C26 C25 118.8(2) . . ? C26 C27 C28 119.0(2) . . ? C29 C28 C27 118.9(2) . . ? N7 C29 C28 122.0(2) . . ? N7 C29 C30 115.20(18) . . ? C28 C29 C30 122.79(19) . . ? N9 C30 C29 109.03(16) . . ? N8 C31 C32 122.3(2) . . ? C31 C32 C33 118.8(2) . . ? C34 C33 C32 119.5(2) . . ? C33 C34 C35 118.8(2) . . ? N8 C35 C34 121.9(2) . . ? N8 C35 C36 115.26(19) . . ? C34 C35 C36 122.8(2) . . ? N9 C36 C35 110.48(17) . . ? N5 C37 Mo1 173.8(2) . . ? N10 C38 Mo1 172.83(18) . . ? N11 C39 Mo1 176.11(19) . . ? N12 C40 Mo1 175.99(19) . . ? N13 C41 Mo1 178.4(2) . . ? N14 C42 Mo1 178.33(19) . . ? N15 C43 Mo1 178.7(2) . . ? N16 C44 Mo1 178.39(19) . . ? _diffrn_measured_fraction_theta_max 0.995 _diffrn_reflns_theta_full 27.48 _diffrn_measured_fraction_theta_full 0.995 _refine_diff_density_max 0.528 _refine_diff_density_min -0.544 _refine_diff_density_rms 0.079 #end of cif #end of cif data_3_ccdc_715890 _database_code_depnum_ccdc_archive 'CCDC 715890' #TrackingRef '1.cif' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C16 H42 Cu2 Mo N16 O5' _chemical_formula_weight 761.68 loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Cu Cu 0.3201 1.2651 '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 11.193(1) _cell_length_b 8.968(1) _cell_length_c 30.498(4) _cell_angle_alpha 90.00 _cell_angle_beta 91.082(2) _cell_angle_gamma 90.00 _cell_volume 3060.7(7) _cell_formula_units_Z 4 _cell_measurement_temperature 123(2) _cell_measurement_reflns_used 8906 _cell_measurement_theta_min 3.0 _cell_measurement_theta_max 27.5 _exptl_crystal_description needle _exptl_crystal_colour purple _exptl_crystal_size_max 0.25 _exptl_crystal_size_mid 0.20 _exptl_crystal_size_min 0.10 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.653 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1560 _exptl_absorpt_coefficient_mu 1.836 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.655 _exptl_absorpt_correction_T_max 0.801 _exptl_absorpt_process_details SADABS _exptl_special_details ; Jacobson, R. (1998) Private communication ; _diffrn_ambient_temperature 123(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'Rigaku Saturn' _diffrn_measurement_method \w _diffrn_detector_area_resol_mean 7.31 _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 23577 _diffrn_reflns_av_R_equivalents 0.0416 _diffrn_reflns_av_sigmaI/netI 0.0472 _diffrn_reflns_limit_h_min -12 _diffrn_reflns_limit_h_max 14 _diffrn_reflns_limit_k_min -11 _diffrn_reflns_limit_k_max 11 _diffrn_reflns_limit_l_min -39 _diffrn_reflns_limit_l_max 39 _diffrn_reflns_theta_min 3.03 _diffrn_reflns_theta_max 27.48 _reflns_number_total 6851 _reflns_number_gt 6393 _reflns_threshold_expression >2sigma(I) _computing_data_collection CrystalClear _computing_cell_refinement CrystalClear _computing_data_reduction CrystalStructure _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics ? _computing_publication_material ? _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^)+(0.0331P)^2^+2.3995P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment constr _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 6851 _refine_ls_number_parameters 364 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0317 _refine_ls_R_factor_gt 0.0292 _refine_ls_wR_factor_ref 0.0820 _refine_ls_wR_factor_gt 0.0799 _refine_ls_goodness_of_fit_ref 1.097 _refine_ls_restrained_S_all 1.097 _refine_ls_shift/su_max 0.002 _refine_ls_shift/su_mean 0.000 loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_occupancy _atom_site_symmetry_multiplicity _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group Mo1 Mo 0.986129(17) 1.143941(19) 0.136257(6) 0.00623(6) Uani 1 1 d . . . Cu1 Cu 0.93716(3) 0.63641(3) 0.222046(9) 0.01046(8) Uani 1 1 d . . . Cu2 Cu 0.0000 0.5000 0.0000 0.01142(10) Uani 1 2 d S . . N1 N 1.00813(18) 0.6545(2) 0.28310(7) 0.0143(4) Uani 1 1 d . . . H1A H 0.9636 0.7162 0.2994 0.017 Uiso 1 1 calc R . . H1B H 1.0106 0.5646 0.2962 0.017 Uiso 1 1 calc R . . N2 N 1.10932(18) 0.6420(2) 0.20258(7) 0.0141(4) Uani 1 1 d . . . H2A H 1.1235 0.5657 0.1842 0.017 Uiso 1 1 calc R . . H2B H 1.1239 0.7279 0.1884 0.017 Uiso 1 1 calc R . . N3 N 0.76770(18) 0.6136(2) 0.24218(6) 0.0123(4) Uani 1 1 d . . . H3A H 0.7649 0.5459 0.2639 0.015 Uiso 1 1 calc R . . H3B H 0.7410 0.7012 0.2525 0.015 Uiso 1 1 calc R . . N4 N 0.86373(19) 0.6183(2) 0.16117(6) 0.0148(4) Uani 1 1 d . . . H4A H 0.8967 0.6854 0.1431 0.018 Uiso 1 1 calc R . . H4B H 0.8767 0.5265 0.1503 0.018 Uiso 1 1 calc R . . N5 N 0.91390(18) 0.9000(2) 0.21295(6) 0.0129(4) Uani 1 1 d . . . N6 N 0.03291(18) 0.7069(2) 0.02426(7) 0.0144(4) Uani 1 1 d . . . H6A H 0.0545 0.7686 0.0025 0.017 Uiso 1 1 calc R . . H6B H -0.0333 0.7438 0.0366 0.017 Uiso 1 1 calc R . . N7 N 0.16063(18) 0.4499(2) 0.02703(7) 0.0130(4) Uani 1 1 d . . . H7A H 0.1511 0.3932 0.0510 0.016 Uiso 1 1 calc R . . H7B H 0.2045 0.3984 0.0078 0.016 Uiso 1 1 calc R . . N8 N 0.4500(2) 0.1726(2) 0.03814(7) 0.0202(5) Uani 1 1 d . . . H8A H 0.5100 0.2391 0.0405 0.024 Uiso 1 1 calc R . . H8B H 0.3862 0.2187 0.0259 0.024 Uiso 1 1 calc R . . N9 N 0.4872(2) -0.1201(2) 0.05511(7) 0.0198(5) Uani 1 1 d . . . H9A H 0.4163 -0.1671 0.0557 0.024 Uiso 1 1 calc R . . H9B H 0.5457 -0.1889 0.0566 0.024 Uiso 1 1 calc R . . N10 N 0.85234(19) 0.8644(2) 0.08491(7) 0.0154(4) Uani 1 1 d . . . N11 N 0.69813(19) 1.2037(2) 0.15365(7) 0.0172(4) Uani 1 1 d . . . N12 N 0.9752(2) 1.3405(2) 0.22794(7) 0.0169(4) Uani 1 1 d . . . N13 N 1.22045(19) 0.9356(2) 0.16349(7) 0.0175(4) Uani 1 1 d . . . N14 N 1.12529(19) 1.0931(2) 0.04231(7) 0.0172(4) Uani 1 1 d . . . N15 N 0.89414(19) 1.4164(2) 0.07046(7) 0.0162(4) Uani 1 1 d . . . N16 N 1.20554(19) 1.3930(2) 0.13472(7) 0.0160(4) Uani 1 1 d . . . C1 C 1.1301(2) 0.7149(3) 0.27884(9) 0.0195(5) Uani 1 1 d . . . H1C H 1.1752 0.7017 0.3060 0.023 Uiso 1 1 calc R . . H1D H 1.1270 0.8204 0.2720 0.023 Uiso 1 1 calc R . . C2 C 1.1877(2) 0.6299(3) 0.24226(9) 0.0194(5) Uani 1 1 d . . . H2C H 1.2658 0.6714 0.2364 0.023 Uiso 1 1 calc R . . H2D H 1.1976 0.5261 0.2505 0.023 Uiso 1 1 calc R . . C3 C 0.6912(2) 0.5646(3) 0.20487(8) 0.0160(5) Uani 1 1 d . . . H3C H 0.6082 0.5886 0.2102 0.019 Uiso 1 1 calc R . . H3D H 0.6979 0.4577 0.2008 0.019 Uiso 1 1 calc R . . C4 C 0.7338(2) 0.6460(3) 0.16449(8) 0.0177(5) Uani 1 1 d . . . H4C H 0.6920 0.6093 0.1385 0.021 Uiso 1 1 calc R . . H4D H 0.7185 0.7521 0.1671 0.021 Uiso 1 1 calc R . . C5 C 0.1302(2) 0.6950(3) 0.05738(8) 0.0163(5) Uani 1 1 d . . . H5A H 0.0998 0.6561 0.0847 0.020 Uiso 1 1 calc R . . H5B H 0.1652 0.7922 0.0630 0.020 Uiso 1 1 calc R . . C6 C 0.2226(2) 0.5904(3) 0.03910(8) 0.0161(5) Uani 1 1 d . . . H6C H 0.2589 0.6341 0.0135 0.019 Uiso 1 1 calc R . . H6D H 0.2849 0.5710 0.0609 0.019 Uiso 1 1 calc R . . C7 C 0.4196(3) 0.1163(3) 0.08207(9) 0.0249(6) Uani 1 1 d . . . H7C H 0.3363 0.0864 0.0825 0.030 Uiso 1 1 calc R . . H7D H 0.4321 0.1938 0.1039 0.030 Uiso 1 1 calc R . . C8 C 0.4987(3) -0.0151(3) 0.09222(8) 0.0224(6) Uani 1 1 d . . . H8C H 0.5811 0.0171 0.0958 0.027 Uiso 1 1 calc R . . H8D H 0.4743 -0.0628 0.1191 0.027 Uiso 1 1 calc R . . C9 C 0.9383(2) 0.9871(2) 0.18692(7) 0.0097(4) Uani 1 1 d . . . C10 C 0.9005(2) 0.9634(3) 0.10158(7) 0.0105(4) Uani 1 1 d . . . C11 C 0.7978(2) 1.1804(3) 0.14761(7) 0.0112(4) Uani 1 1 d . . . C12 C 0.9828(2) 1.2736(2) 0.19562(7) 0.0108(4) Uani 1 1 d . . . C13 C 1.1390(2) 1.0093(2) 0.15431(8) 0.0114(5) Uani 1 1 d . . . C14 C 1.0771(2) 1.1099(2) 0.07476(7) 0.0106(4) Uani 1 1 d . . . C15 C 0.9217(2) 1.3205(3) 0.09378(7) 0.0103(4) Uani 1 1 d . . . C16 C 1.1313(2) 1.3044(3) 0.13545(7) 0.0110(4) Uani 1 1 d . . . Cu3 Cu 0.5000 0.0000 0.0000 0.01694(11) Uani 1 2 d S . . O1 O 0.72225(15) 0.0659(2) 0.01432(6) 0.0187(4) Uani 1 1 d . . . O2 O 0.68433(15) 0.67226(19) 0.04170(6) 0.0163(4) Uani 1 1 d . . . O3 O 0.60357(16) 0.4116(2) 0.07958(6) 0.0201(4) Uani 1 1 d . . . O4 O 0.43944(16) 0.7891(2) 0.18375(6) 0.0219(4) Uani 1 1 d . . . O5 O 0.43901(19) 0.5226(3) 0.13543(9) 0.0490(7) Uani 1 1 d . . . 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 0.00631(12) 0.00567(10) 0.00673(10) 0.00039(6) 0.00004(7) 0.00026(6) Cu1 0.00978(16) 0.01267(14) 0.00896(14) -0.00004(10) 0.00115(11) -0.00084(10) Cu2 0.0116(2) 0.00886(19) 0.0138(2) -0.00115(14) -0.00129(16) 0.00238(15) N1 0.0140(11) 0.0159(10) 0.0128(10) -0.0014(8) 0.0001(8) 0.0032(8) N2 0.0153(11) 0.0098(9) 0.0175(10) 0.0014(7) 0.0045(8) 0.0006(8) N3 0.0130(11) 0.0132(9) 0.0106(9) 0.0007(7) 0.0003(8) -0.0017(8) N4 0.0191(11) 0.0135(9) 0.0121(10) -0.0008(7) 0.0024(8) -0.0019(8) N5 0.0155(11) 0.0101(9) 0.0131(9) -0.0014(8) 0.0029(8) 0.0011(8) N6 0.0165(11) 0.0104(9) 0.0163(10) -0.0005(8) -0.0011(8) 0.0026(8) N7 0.0135(10) 0.0110(9) 0.0145(10) 0.0015(8) 0.0007(8) 0.0016(8) N8 0.0180(12) 0.0200(11) 0.0223(11) -0.0075(9) -0.0076(9) 0.0067(9) N9 0.0145(12) 0.0206(11) 0.0245(12) -0.0004(9) 0.0000(9) 0.0001(9) N10 0.0168(11) 0.0166(10) 0.0130(10) -0.0013(8) 0.0013(8) -0.0021(8) N11 0.0160(12) 0.0206(11) 0.0148(10) 0.0022(8) 0.0009(8) 0.0011(9) N12 0.0203(12) 0.0148(10) 0.0156(10) -0.0021(8) 0.0004(9) -0.0035(8) N13 0.0141(11) 0.0150(10) 0.0235(11) 0.0054(8) -0.0001(9) 0.0009(9) N14 0.0181(11) 0.0163(10) 0.0173(11) 0.0008(8) 0.0030(9) 0.0021(8) N15 0.0163(11) 0.0173(10) 0.0152(10) 0.0033(8) 0.0015(8) 0.0029(8) N16 0.0161(11) 0.0155(10) 0.0164(10) -0.0002(8) -0.0001(8) -0.0024(9) C1 0.0165(13) 0.0192(12) 0.0226(13) -0.0027(10) -0.0056(10) -0.0023(10) C2 0.0102(13) 0.0232(13) 0.0247(14) 0.0045(10) 0.0010(10) 0.0016(10) C3 0.0139(13) 0.0178(12) 0.0163(12) -0.0004(9) -0.0011(9) -0.0048(10) C4 0.0187(14) 0.0222(13) 0.0121(11) 0.0011(9) -0.0056(10) -0.0037(10) C5 0.0212(14) 0.0130(11) 0.0146(11) -0.0024(9) -0.0026(10) -0.0009(10) C6 0.0139(13) 0.0139(11) 0.0203(12) 0.0012(9) -0.0025(10) -0.0015(10) C7 0.0170(14) 0.0304(15) 0.0276(15) -0.0123(12) 0.0076(11) -0.0041(11) C8 0.0241(15) 0.0303(14) 0.0131(12) -0.0003(10) 0.0031(11) -0.0061(11) C9 0.0084(11) 0.0096(10) 0.0112(11) -0.0039(8) 0.0007(9) 0.0017(8) C10 0.0112(12) 0.0128(11) 0.0076(10) 0.0011(8) 0.0016(8) 0.0007(9) C11 0.0128(12) 0.0117(10) 0.0091(10) 0.0007(8) -0.0006(9) 0.0010(9) C12 0.0109(12) 0.0087(10) 0.0129(11) 0.0024(8) 0.0002(9) -0.0006(8) C13 0.0119(12) 0.0101(10) 0.0122(11) 0.0016(8) 0.0002(9) -0.0027(9) C14 0.0106(12) 0.0084(10) 0.0128(11) 0.0018(8) -0.0006(9) 0.0010(9) C15 0.0090(11) 0.0123(10) 0.0097(10) -0.0006(8) 0.0019(8) 0.0005(9) C16 0.0120(12) 0.0118(11) 0.0092(10) 0.0000(8) 0.0004(9) 0.0012(9) Cu3 0.0234(3) 0.0147(2) 0.0125(2) -0.00413(15) -0.00566(17) 0.00744(17) O1 0.0153(9) 0.0244(9) 0.0164(9) -0.0011(7) 0.0014(7) 0.0046(7) O2 0.0162(9) 0.0160(8) 0.0167(9) -0.0020(7) -0.0015(7) 0.0005(7) O3 0.0185(10) 0.0170(9) 0.0248(10) 0.0005(7) -0.0029(8) -0.0012(7) O4 0.0165(10) 0.0283(10) 0.0210(9) 0.0025(8) -0.0005(7) 0.0063(8) O5 0.0181(12) 0.0667(17) 0.0628(17) -0.0408(14) 0.0140(11) -0.0162(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 C10 2.149(2) . ? Mo1 C12 2.152(2) . ? Mo1 C13 2.158(2) . ? Mo1 C15 2.161(2) . ? Mo1 C9 2.164(2) . ? Mo1 C11 2.168(2) . ? Mo1 C16 2.171(2) . ? Mo1 C14 2.173(2) . ? Cu1 N3 2.015(2) . ? Cu1 N1 2.017(2) . ? Cu1 N4 2.023(2) . ? Cu1 N2 2.028(2) . ? Cu1 N5 2.394(2) . ? Cu2 N7 2.014(2) 3_565 ? Cu2 N7 2.014(2) . ? Cu2 N6 2.029(2) 3_565 ? Cu2 N6 2.029(2) . ? N1 C1 1.476(3) . ? N2 C2 1.485(3) . ? N3 C3 1.478(3) . ? N4 C4 1.481(3) . ? N5 C9 1.150(3) . ? N6 C5 1.475(3) . ? N7 C6 1.481(3) . ? N8 C7 1.478(4) . ? N8 Cu3 2.022(2) . ? N9 C8 1.476(3) . ? N9 Cu3 2.003(2) . ? N10 C10 1.152(3) . ? N11 C11 1.153(3) . ? N12 C12 1.159(3) . ? N13 C13 1.156(3) . ? N14 C14 1.146(3) . ? N15 C15 1.154(3) . ? N16 C16 1.150(3) . ? C1 C2 1.506(4) . ? C3 C4 1.516(3) . ? C5 C6 1.511(3) . ? C7 C8 1.502(4) . ? Cu3 N9 2.003(2) 3_655 ? Cu3 N8 2.022(2) 3_655 ? 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 C10 Mo1 C12 143.71(8) . . ? C10 Mo1 C13 92.76(9) . . ? C12 Mo1 C13 96.54(9) . . ? C10 Mo1 C15 96.67(9) . . ? C12 Mo1 C15 95.61(8) . . ? C13 Mo1 C15 144.81(9) . . ? C10 Mo1 C9 75.38(8) . . ? C12 Mo1 C9 75.05(8) . . ? C13 Mo1 C9 70.12(9) . . ? C15 Mo1 C9 145.06(8) . . ? C10 Mo1 C11 76.48(9) . . ? C12 Mo1 C11 75.63(9) . . ? C13 Mo1 C11 144.37(8) . . ? C15 Mo1 C11 70.77(8) . . ? C9 Mo1 C11 74.30(9) . . ? C10 Mo1 C16 145.14(8) . . ? C12 Mo1 C16 71.12(9) . . ? C13 Mo1 C16 77.51(9) . . ? C15 Mo1 C16 75.47(9) . . ? C9 Mo1 C16 129.37(9) . . ? C11 Mo1 C16 129.21(9) . . ? C10 Mo1 C14 71.41(8) . . ? C12 Mo1 C14 144.88(9) . . ? C13 Mo1 C14 76.06(9) . . ? C15 Mo1 C14 75.06(8) . . ? C9 Mo1 C14 130.64(8) . . ? C11 Mo1 C14 129.21(9) . . ? C16 Mo1 C14 73.76(9) . . ? N3 Cu1 N1 94.79(8) . . ? N3 Cu1 N4 84.44(9) . . ? N1 Cu1 N4 179.22(8) . . ? N3 Cu1 N2 175.51(8) . . ? N1 Cu1 N2 84.75(9) . . ? N4 Cu1 N2 96.03(9) . . ? N3 Cu1 N5 91.98(7) . . ? N1 Cu1 N5 93.87(8) . . ? N4 Cu1 N5 86.07(8) . . ? N2 Cu1 N5 92.50(7) . . ? N7 Cu2 N7 180.00(10) 3_565 . ? N7 Cu2 N6 84.26(8) 3_565 3_565 ? N7 Cu2 N6 95.74(8) . 3_565 ? N7 Cu2 N6 95.74(8) 3_565 . ? N7 Cu2 N6 84.26(8) . . ? N6 Cu2 N6 180.00(11) 3_565 . ? C1 N1 Cu1 107.27(15) . . ? C2 N2 Cu1 108.03(15) . . ? C3 N3 Cu1 109.31(15) . . ? C4 N4 Cu1 107.83(15) . . ? C9 N5 Cu1 136.38(17) . . ? C5 N6 Cu2 108.08(14) . . ? C6 N7 Cu2 108.80(14) . . ? C7 N8 Cu3 109.33(17) . . ? C8 N9 Cu3 107.09(16) . . ? N1 C1 C2 106.8(2) . . ? N2 C2 C1 108.2(2) . . ? N3 C3 C4 107.18(19) . . ? N4 C4 C3 107.4(2) . . ? N6 C5 C6 107.08(19) . . ? N7 C6 C5 107.4(2) . . ? N8 C7 C8 108.0(2) . . ? N9 C8 C7 107.4(2) . . ? N5 C9 Mo1 177.77(19) . . ? N10 C10 Mo1 176.6(2) . . ? N11 C11 Mo1 178.2(2) . . ? N12 C12 Mo1 176.5(2) . . ? N13 C13 Mo1 179.0(2) . . ? N14 C14 Mo1 179.5(2) . . ? N15 C15 Mo1 176.0(2) . . ? N16 C16 Mo1 177.8(2) . . ? N9 Cu3 N9 180.00(13) . 3_655 ? N9 Cu3 N8 95.52(9) . 3_655 ? N9 Cu3 N8 84.48(9) 3_655 3_655 ? N9 Cu3 N8 84.48(9) . . ? N9 Cu3 N8 95.52(9) 3_655 . ? N8 Cu3 N8 180.00(17) 3_655 . ? _diffrn_measured_fraction_theta_max 0.975 _diffrn_reflns_theta_full 27.48 _diffrn_measured_fraction_theta_full 0.975 _refine_diff_density_max 0.866 _refine_diff_density_min -0.664 _refine_diff_density_rms 0.094 #end of cif data_4_ccdc_715891 _database_code_depnum_ccdc_archive 'CCDC 715891' #TrackingRef '1_and_4.cif' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C60 H148 Cu6 Mo3 N42 O23' _chemical_formula_weight 2495.18 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' Cu Cu 0.3201 1.2651 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Mo Mo -1.6832 0.6857 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting Orthorhombic _symmetry_space_group_name_H-M C222(1) loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, -y, z+1/2' '-x, y, -z+1/2' 'x, -y, -z' 'x+1/2, y+1/2, z' '-x+1/2, -y+1/2, z+1/2' '-x+1/2, y+1/2, -z+1/2' 'x+1/2, -y+1/2, -z' _cell_length_a 13.423(3) _cell_length_b 28.041(6) _cell_length_c 30.947(6) _cell_angle_alpha 90.00 _cell_angle_beta 90.00 _cell_angle_gamma 90.00 _cell_volume 11648(4) _cell_formula_units_Z 4 _cell_measurement_temperature 123(2) _cell_measurement_reflns_used 17043 _cell_measurement_theta_min 3.0 _cell_measurement_theta_max 27.5 _exptl_crystal_description chunk _exptl_crystal_colour green _exptl_crystal_size_max 0.20 _exptl_crystal_size_mid 0.15 _exptl_crystal_size_min 0.15 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.405 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 5132 _exptl_absorpt_coefficient_mu 1.459 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.8741 _exptl_absorpt_correction_T_max 1.0000 _exptl_absorpt_process_details ? _exptl_special_details ; ? ; _diffrn_ambient_temperature 123(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'Rigaku Saturn' _diffrn_measurement_method \w _diffrn_detector_area_resol_mean 7.31 _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 42169 _diffrn_reflns_av_R_equivalents 0.0515 _diffrn_reflns_av_sigmaI/netI 0.0652 _diffrn_reflns_limit_h_min -14 _diffrn_reflns_limit_h_max 17 _diffrn_reflns_limit_k_min -36 _diffrn_reflns_limit_k_max 36 _diffrn_reflns_limit_l_min -34 _diffrn_reflns_limit_l_max 40 _diffrn_reflns_theta_min 3.01 _diffrn_reflns_theta_max 27.48 _reflns_number_total 13300 _reflns_number_gt 12610 _reflns_threshold_expression >2sigma(I) _computing_data_collection CrystalClear _computing_cell_refinement CrystalClear _computing_data_reduction CrystalStructure _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics ? _computing_publication_material ? _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. ; # SQUEEZE RESULTS (APPEND TO CIF) # Note: Data are Listed for all Voids in the P1 Unit Cell # i.e. Centre of Gravity, Solvent Accessible Volume, # Recovered number of Electrons in the Void and # Details about the Squeezed Material loop_ _platon_squeeze_void_nr _platon_squeeze_void_average_x _platon_squeeze_void_average_y _platon_squeeze_void_average_z _platon_squeeze_void_volume _platon_squeeze_void_count_electrons _platon_squeeze_void_content 1 0.671 0.000 0.000 55 12 ' ' 2 0.500 0.040 0.250 190 27 ' ' 3 0.329 0.000 0.500 55 12 ' ' 4 0.500 -0.040 0.750 190 27 ' ' 5 0.427 0.035 0.615 6 2 ' ' 6 0.573 0.035 0.885 7 2 ' ' 7 0.687 0.114 0.072 7 3 ' ' 8 0.313 0.114 0.428 7 2 ' ' 9 0.000 0.151 0.750 10 0 ' ' 10 0.500 0.349 0.250 10 0 ' ' 11 0.000 0.460 0.750 190 27 ' ' 12 0.812 0.392 0.571 8 4 ' ' 13 0.187 0.392 0.929 8 4 ' ' 14 0.830 0.502 0.498 53 11 ' ' 15 0.170 0.502 1.002 53 10 ' ' 16 0.069 0.465 0.115 7 3 ' ' 17 0.931 0.465 0.385 7 2 ' ' 18 1.000 0.540 0.250 190 26 ' ' 19 0.927 0.535 0.615 6 2 ' ' 20 0.073 0.535 0.885 7 2 ' ' 21 0.187 0.614 0.072 7 3 ' ' 22 0.813 0.614 0.428 7 2 ' ' 23 0.500 0.651 0.750 10 0 ' ' 24 0.000 0.849 0.250 10 0 ' ' 25 0.313 0.886 0.572 6 2 ' ' 26 0.687 0.886 0.928 6 2 ' ' 27 0.573 0.965 0.115 7 2 ' ' 28 0.427 0.965 0.385 6 2 ' ' _platon_squeeze_details ; The porous structure contains a few solvent water molecules and some of which can not be modeled unambiguously. Their contribution to the calculated structure factors was masked by using Platon SQUEEZE. ; _publ_section_exptl_refinement ; The ADP's of the ring of cu3-n8-c16-c17-c18-n8 abnormally shaped, may be due to the heavy atom effect.Therefore atoms except metal atom in the ring are RESTRAINED to have similar ADP by using SIMU command with ESD of 0.01; C18 and N9 are RESTRAINED with ESD of 0.01 so that their Uij components approximate to isotropic behavior by using the command ISOR. The hydrogen atoms which should be bonded to the oxgen atoms of the solvent water molecules can not be located from the Fourier diffence map, and no geometrical information about the orientaions of the H atoms can be obtained. Therefore, these O atoms were leaved isolatedly. ; _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^)+(0.0478P)^2^+21.0515P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment constr _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_abs_structure_details 'Flack H D (1983), Acta Cryst. A39, 876-881' _refine_ls_abs_structure_Flack 0.035(12) _refine_ls_number_reflns 13300 _refine_ls_number_parameters 605 _refine_ls_number_restraints 30 _refine_ls_R_factor_all 0.0492 _refine_ls_R_factor_gt 0.0457 _refine_ls_wR_factor_ref 0.1157 _refine_ls_wR_factor_gt 0.1128 _refine_ls_goodness_of_fit_ref 1.082 _refine_ls_restrained_S_all 1.085 _refine_ls_shift/su_max 0.003 _refine_ls_shift/su_mean 0.000 loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_occupancy _atom_site_symmetry_multiplicity _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group Mo1 Mo 0.51480(3) 0.339314(13) 1.006019(11) 0.01366(8) Uani 1 1 d . . . Mo2 Mo 0.5000 0.29319(2) 0.7500 0.01586(12) Uani 1 2 d S . . Cu1 Cu 0.80678(4) 0.26220(2) 1.101580(17) 0.01935(13) Uani 1 1 d . . . Cu2 Cu 0.74503(4) 0.24995(2) 0.893438(17) 0.01993(13) Uani 1 1 d . . . Cu3 Cu 0.46425(4) 0.43730(2) 0.856463(18) 0.02122(13) Uani 1 1 d . . . N1 N 0.7938(3) 0.19235(15) 1.11883(14) 0.0294(10) Uani 1 1 d . . . H1A H 0.7967 0.1751 1.0943 0.035 Uiso 1 1 calc R . . H1B H 0.8485 0.1849 1.1343 0.035 Uiso 1 1 calc R . . N2 N 0.7444(3) 0.28505(14) 1.15834(12) 0.0186(8) Uani 1 1 d . . . H2 H 0.7939 0.2843 1.1784 0.022 Uiso 1 1 calc R . . N3 N 0.8674(3) 0.32652(17) 1.09030(15) 0.0337(11) Uani 1 1 d . . . H3A H 0.9248 0.3277 1.1053 0.040 Uiso 1 1 calc R . . H3B H 0.8840 0.3273 1.0621 0.040 Uiso 1 1 calc R . . N4 N 0.6388(3) 0.20345(15) 0.91231(13) 0.0245(9) Uani 1 1 d . . . H4A H 0.6316 0.2071 0.9410 0.029 Uiso 1 1 calc R . . H4B H 0.5814 0.2132 0.9002 0.029 Uiso 1 1 calc R . . N5 N 0.7828(3) 0.20970(17) 0.83944(13) 0.0281(10) Uani 1 1 d . . . H5 H 0.7398 0.2184 0.8182 0.034 Uiso 1 1 calc R . . N6 N 0.8112(3) 0.30865(16) 0.87078(13) 0.0280(10) Uani 1 1 d . . . H6A H 0.7685 0.3227 0.8524 0.034 Uiso 1 1 calc R . . H6B H 0.8195 0.3287 0.8932 0.034 Uiso 1 1 calc R . . N7 N 0.6084(3) 0.43236(18) 0.84020(15) 0.0332(10) Uani 1 1 d . . . H7A H 0.6187 0.4029 0.8295 0.040 Uiso 1 1 calc R . . H7B H 0.6195 0.4531 0.8185 0.040 Uiso 1 1 calc R . . N8 N 0.4882(4) 0.49609(15) 0.89381(15) 0.0329(10) Uani 1 1 d . . . H8 H 0.4933 0.5214 0.8755 0.039 Uiso 1 1 calc R . . N9 N 0.3168(4) 0.4546(2) 0.8515(2) 0.0554(15) Uani 1 1 d U . . H9A H 0.2946 0.4420 0.8266 0.066 Uiso 1 1 calc R . . H9B H 0.2849 0.4392 0.8730 0.066 Uiso 1 1 calc R . . N10 N 0.6694(3) 0.27353(16) 1.06322(13) 0.0260(9) Uani 1 1 d . . . N11 N 0.6762(3) 0.29314(15) 0.93709(12) 0.0236(9) Uani 1 1 d . . . N12 N 0.4717(3) 0.39125(14) 0.91195(12) 0.0238(9) Uani 1 1 d . . . N13 N 0.6948(3) 0.41955(14) 0.99865(13) 0.0249(9) Uani 1 1 d . . . N14 N 0.5137(3) 0.39113(14) 1.10255(12) 0.0255(9) Uani 1 1 d . . . N15 N 0.3682(3) 0.27578(16) 1.06938(13) 0.0272(10) Uani 1 1 d . . . N16 N 0.3887(3) 0.26256(18) 0.94739(13) 0.0314(11) Uani 1 1 d . . . N17 N 0.3007(4) 0.3973(2) 1.00786(16) 0.0457(13) Uani 1 1 d . . . N18 N 0.4409(3) 0.38355(15) 0.81319(12) 0.0228(9) Uani 1 1 d . . . N19 N 0.6600(3) 0.20323(15) 0.75029(14) 0.0289(9) Uani 1 1 d . . . N20 N 0.5099(3) 0.24801(14) 0.65126(11) 0.0239(8) Uani 1 1 d . . . N21 N 0.2954(3) 0.34106(16) 0.71018(13) 0.0259(9) Uani 1 1 d . . . C1 C 0.7082(4) 0.17500(19) 1.1432(2) 0.0381(14) Uani 1 1 d . . . H1C H 0.7185 0.1418 1.1507 0.046 Uiso 1 1 calc R . . H1D H 0.6489 0.1771 1.1254 0.046 Uiso 1 1 calc R . . C2 C 0.6927(4) 0.2036(2) 1.18405(17) 0.0351(13) Uani 1 1 d . . . H2A H 0.7537 0.2031 1.2008 0.042 Uiso 1 1 calc R . . H2B H 0.6410 0.1885 1.2012 0.042 Uiso 1 1 calc R . . C3 C 0.6633(4) 0.2552(2) 1.17554(17) 0.0294(11) Uani 1 1 d . . . H3C H 0.6084 0.2555 1.1552 0.035 Uiso 1 1 calc R . . H3D H 0.6397 0.2691 1.2023 0.035 Uiso 1 1 calc R . . C4 C 0.7052(4) 0.33518(19) 1.15824(16) 0.0298(11) Uani 1 1 d . . . H4C H 0.6793 0.3426 1.1867 0.036 Uiso 1 1 calc R . . H4D H 0.6503 0.3373 1.1379 0.036 Uiso 1 1 calc R . . C5 C 0.7838(5) 0.37235(18) 1.14611(18) 0.0362(14) Uani 1 1 d . . . H5A H 0.7582 0.4038 1.1529 0.043 Uiso 1 1 calc R . . H5B H 0.8426 0.3672 1.1637 0.043 Uiso 1 1 calc R . . C6 C 0.8134(4) 0.37130(18) 1.09957(18) 0.0319(12) Uani 1 1 d . . . H6C H 0.7545 0.3733 1.0815 0.038 Uiso 1 1 calc R . . H6D H 0.8558 0.3984 1.0931 0.038 Uiso 1 1 calc R . . C7 C 0.6465(4) 0.15169(19) 0.90423(18) 0.0332(12) Uani 1 1 d . . . H7C H 0.5840 0.1365 0.9118 0.040 Uiso 1 1 calc R . . H7D H 0.6983 0.1383 0.9224 0.040 Uiso 1 1 calc R . . C8 C 0.6703(4) 0.1415(2) 0.85724(19) 0.0379(14) Uani 1 1 d . . . H8A H 0.6648 0.1075 0.8521 0.046 Uiso 1 1 calc R . . H8B H 0.6215 0.1574 0.8391 0.046 Uiso 1 1 calc R . . C9 C 0.7717(4) 0.1577(2) 0.84463(18) 0.0369(14) Uani 1 1 d . . . H9C H 0.8186 0.1469 0.8664 0.044 Uiso 1 1 calc R . . H9D H 0.7895 0.1424 0.8176 0.044 Uiso 1 1 calc R . . C10 C 0.8841(4) 0.2195(2) 0.82272(16) 0.0349(14) Uani 1 1 d . . . H10A H 0.8953 0.1996 0.7975 0.042 Uiso 1 1 calc R . . H10B H 0.9322 0.2101 0.8445 0.042 Uiso 1 1 calc R . . C11 C 0.9037(4) 0.2707(2) 0.81051(17) 0.0390(15) Uani 1 1 d . . . H11A H 0.8515 0.2813 0.7911 0.047 Uiso 1 1 calc R . . H11B H 0.9662 0.2723 0.7948 0.047 Uiso 1 1 calc R . . C12 C 0.9087(4) 0.3046(2) 0.84837(17) 0.0338(13) Uani 1 1 d . . . H12A H 0.9586 0.2933 0.8687 0.041 Uiso 1 1 calc R . . H12B H 0.9291 0.3358 0.8382 0.041 Uiso 1 1 calc R . . C13 C 0.6852(5) 0.4411(3) 0.8739(2) 0.0505(17) Uani 1 1 d . . . H13A H 0.7510 0.4384 0.8611 0.061 Uiso 1 1 calc R . . H13B H 0.6794 0.4171 0.8963 0.061 Uiso 1 1 calc R . . C14 C 0.6733(4) 0.4895(2) 0.8934(2) 0.0454(16) Uani 1 1 d . . . H14A H 0.7311 0.4962 0.9112 0.055 Uiso 1 1 calc R . . H14B H 0.6719 0.5129 0.8703 0.055 Uiso 1 1 calc R . . C15 C 0.5821(5) 0.4953(2) 0.9202(2) 0.0411(15) Uani 1 1 d . . . H15A H 0.5870 0.5248 0.9364 0.049 Uiso 1 1 calc R . . H15B H 0.5784 0.4693 0.9408 0.049 Uiso 1 1 calc R . . C16 C 0.4014(5) 0.5053(2) 0.9217(2) 0.0482(17) Uani 1 1 d U . . H16A H 0.4202 0.5283 0.9437 0.058 Uiso 1 1 calc R . . H16B H 0.3834 0.4759 0.9363 0.058 Uiso 1 1 calc R . . C17 C 0.3087(6) 0.5245(3) 0.8970(3) 0.070(2) Uani 1 1 d U . . H17A H 0.2508 0.5205 0.9154 0.085 Uiso 1 1 calc R . . H17B H 0.3176 0.5584 0.8925 0.085 Uiso 1 1 calc R . . C18 C 0.2859(7) 0.5009(3) 0.8526(3) 0.078(2) Uani 1 1 d U . . H18A H 0.2148 0.5022 0.8472 0.094 Uiso 1 1 calc R . . H18B H 0.3192 0.5187 0.8299 0.094 Uiso 1 1 calc R . . C19 C 0.6166(3) 0.29663(18) 1.04277(14) 0.0189(9) Uani 1 1 d . . . C20 C 0.6218(3) 0.30907(16) 0.96136(14) 0.0168(9) Uani 1 1 d . . . C21 C 0.4897(4) 0.37389(15) 0.94484(13) 0.0177(9) Uani 1 1 d . . . C22 C 0.6304(3) 0.39296(16) 1.00290(15) 0.0183(9) Uani 1 1 d . . . C23 C 0.5152(3) 0.37416(15) 1.06883(14) 0.0185(9) Uani 1 1 d . . . C24 C 0.4206(3) 0.29775(17) 1.04770(14) 0.0181(9) Uani 1 1 d . . . C25 C 0.4340(3) 0.28785(18) 0.96882(14) 0.0200(10) Uani 1 1 d . . . C26 C 0.3780(4) 0.3788(2) 1.00779(16) 0.0285(12) Uani 1 1 d . . . C27 C 0.4553(3) 0.35223(18) 0.79049(14) 0.0198(10) Uani 1 1 d . . . C28 C 0.6037(4) 0.23466(17) 0.74936(15) 0.0214(10) Uani 1 1 d . . . C29 C 0.5058(3) 0.26544(16) 0.68474(13) 0.0175(9) Uani 1 1 d . . . C30 C 0.3637(3) 0.32190(18) 0.72348(14) 0.0196(9) Uani 1 1 d . . . O1 O 0.8219(4) 0.5000 1.0000 0.0393(14) Uani 1 2 d S . . O2 O 0.6534(4) 0.10084(15) 0.75388(14) 0.0466(11) Uani 1 1 d . . . O3 O 0.8516(3) 0.07370(16) 0.74842(16) 0.0496(11) Uani 1 1 d . . . O4 O 0.8573(3) 0.38189(16) 0.94021(13) 0.0415(10) Uani 1 1 d . . . O5 O 0.4957(5) 0.5760(2) 0.81274(13) 0.0747(17) Uani 1 1 d . . . O6 O 0.6567(4) 0.18497(19) 1.01093(17) 0.0635(15) Uani 1 1 d . . . O7 O 0.2251(4) 0.4196(2) 0.76637(17) 0.0672(16) Uani 1 1 d . . . O8 O 1.0084(7) 0.4320(2) 0.9001(2) 0.112(3) Uani 1 1 d . . . O9 O 0.9636(6) 0.3405(5) 1.0015(3) 0.228(7) Uani 1 1 d . . . O10 O 0.9859(6) 0.4356(4) 1.1970(3) 0.169(5) Uani 1 1 d . . . O11 O 0.9759(5) 0.4496(3) 1.0392(2) 0.121(3) Uani 1 1 d . . . O12 O 0.6059(7) 0.4819(3) 0.7519(4) 0.148(3) Uani 1 1 d . . . 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 0.01044(17) 0.01976(18) 0.01078(15) 0.00061(13) 0.00009(13) -0.00025(14) Mo2 0.0130(3) 0.0242(3) 0.0104(2) 0.000 0.00054(19) 0.000 Cu1 0.0176(3) 0.0258(3) 0.0147(3) -0.0031(2) -0.0015(2) 0.0059(2) Cu2 0.0150(3) 0.0321(3) 0.0127(2) -0.0011(2) 0.0002(2) 0.0072(2) Cu3 0.0261(3) 0.0198(3) 0.0178(3) 0.0018(2) -0.0007(2) 0.0013(2) N1 0.030(2) 0.024(2) 0.034(2) -0.0040(18) -0.0043(19) 0.0071(19) N2 0.0186(19) 0.021(2) 0.0167(18) -0.0013(15) -0.0003(15) 0.0011(16) N3 0.027(2) 0.041(3) 0.033(3) 0.007(2) 0.0080(19) 0.001(2) N4 0.020(2) 0.033(2) 0.020(2) -0.0042(17) -0.0001(16) 0.0006(18) N5 0.020(2) 0.045(3) 0.019(2) -0.0099(19) -0.0057(16) 0.017(2) N6 0.019(2) 0.046(3) 0.019(2) 0.0043(18) 0.0007(16) 0.009(2) N7 0.033(3) 0.034(3) 0.033(2) 0.001(2) 0.003(2) 0.001(2) N8 0.042(3) 0.019(2) 0.038(2) -0.0022(17) -0.003(2) -0.005(2) N9 0.053(3) 0.055(3) 0.058(3) -0.018(2) -0.016(2) 0.015(2) N10 0.020(2) 0.036(3) 0.022(2) 0.0014(18) -0.0061(17) 0.0041(18) N11 0.025(2) 0.027(2) 0.0195(19) -0.0027(17) 0.0029(17) -0.0032(18) N12 0.031(2) 0.020(2) 0.021(2) 0.0010(15) -0.0023(17) -0.0010(18) N13 0.022(2) 0.026(2) 0.026(2) 0.0021(17) -0.0048(17) -0.0052(18) N14 0.027(2) 0.029(2) 0.0205(19) -0.0030(16) -0.0031(18) 0.0041(18) N15 0.023(2) 0.038(3) 0.020(2) 0.0010(18) 0.0015(17) -0.0069(19) N16 0.028(2) 0.049(3) 0.018(2) -0.0029(19) 0.0029(17) -0.017(2) N17 0.033(3) 0.071(4) 0.033(3) 0.013(3) 0.006(2) 0.017(3) N18 0.019(2) 0.033(2) 0.0170(19) 0.0043(17) -0.0018(15) 0.0034(18) N19 0.032(2) 0.038(2) 0.0165(18) -0.001(2) 0.0027(17) 0.009(2) N20 0.022(2) 0.030(2) 0.0192(18) 0.0032(16) 0.0023(16) -0.0016(18) N21 0.019(2) 0.036(2) 0.023(2) -0.0014(18) -0.0053(16) -0.0041(19) C1 0.034(3) 0.024(3) 0.056(4) 0.002(3) -0.017(3) -0.008(2) C2 0.026(3) 0.045(3) 0.034(3) 0.016(3) -0.004(2) -0.007(3) C3 0.018(3) 0.040(3) 0.030(3) 0.001(2) 0.004(2) 0.000(2) C4 0.033(3) 0.034(3) 0.023(2) -0.001(2) 0.004(2) 0.014(2) C5 0.062(4) 0.018(2) 0.028(3) -0.006(2) -0.008(3) 0.004(2) C6 0.034(3) 0.024(3) 0.038(3) 0.008(2) -0.007(2) 0.000(2) C7 0.032(3) 0.030(3) 0.038(3) -0.002(2) -0.006(2) 0.001(2) C8 0.034(3) 0.042(3) 0.037(3) -0.018(3) -0.011(3) 0.009(3) C9 0.032(3) 0.048(3) 0.030(3) -0.021(3) -0.010(2) 0.022(3) C10 0.026(3) 0.064(4) 0.014(2) -0.004(2) 0.0021(19) 0.015(3) C11 0.025(3) 0.072(5) 0.020(3) 0.009(3) 0.005(2) 0.018(3) C12 0.019(3) 0.057(4) 0.026(3) 0.006(2) 0.004(2) 0.001(2) C13 0.025(3) 0.058(4) 0.068(5) -0.010(3) -0.012(3) 0.001(3) C14 0.034(3) 0.040(4) 0.062(4) -0.014(3) -0.023(3) -0.007(3) C15 0.060(4) 0.030(3) 0.033(3) -0.009(2) -0.010(3) -0.003(3) C16 0.050(4) 0.029(3) 0.065(4) -0.019(3) 0.009(3) -0.005(3) C17 0.056(4) 0.058(4) 0.097(5) -0.041(4) -0.001(4) 0.011(3) C18 0.069(3) 0.080(4) 0.086(4) -0.015(3) -0.012(3) 0.015(3) C19 0.013(2) 0.027(3) 0.017(2) -0.0011(18) 0.0000(17) -0.0023(19) C20 0.016(2) 0.016(2) 0.018(2) -0.0005(17) 0.0000(17) -0.0021(18) C21 0.019(2) 0.017(2) 0.018(2) -0.0020(16) 0.0020(18) -0.0006(18) C22 0.017(2) 0.023(2) 0.015(2) -0.0036(18) -0.0057(17) -0.0042(18) C23 0.016(2) 0.019(2) 0.020(2) 0.0043(17) -0.0015(18) -0.0022(19) C24 0.020(2) 0.023(2) 0.011(2) -0.0015(17) -0.0003(17) -0.0005(19) C25 0.018(2) 0.029(3) 0.013(2) -0.0001(19) 0.0030(17) -0.008(2) C26 0.017(2) 0.049(3) 0.020(2) 0.005(2) 0.0024(19) 0.011(2) C27 0.015(2) 0.031(3) 0.013(2) 0.0030(18) 0.0004(16) -0.0011(18) C28 0.021(2) 0.035(3) 0.0080(17) 0.002(2) 0.0040(17) -0.005(2) C29 0.014(2) 0.025(2) 0.0138(19) 0.0001(16) 0.0028(17) 0.0006(19) C30 0.017(2) 0.030(3) 0.012(2) -0.0046(17) -0.0012(17) -0.005(2) O1 0.020(3) 0.026(3) 0.072(4) 0.006(3) 0.000 0.000 O2 0.064(3) 0.046(2) 0.029(2) -0.001(2) 0.001(2) 0.005(2) O3 0.051(3) 0.056(3) 0.042(2) -0.005(2) 0.003(2) 0.009(2) O4 0.025(2) 0.065(3) 0.035(2) -0.005(2) 0.0021(17) -0.001(2) O5 0.084(4) 0.113(5) 0.027(2) -0.016(3) -0.003(3) 0.014(4) O6 0.055(3) 0.065(3) 0.071(3) -0.036(3) 0.008(3) -0.010(3) O7 0.055(3) 0.074(4) 0.072(4) -0.028(3) -0.013(3) 0.018(3) O8 0.138(7) 0.092(5) 0.107(5) 0.012(4) 0.040(5) -0.042(5) O9 0.120(6) 0.432(16) 0.131(6) 0.208(9) 0.095(5) 0.176(9) O10 0.068(5) 0.290(12) 0.149(7) 0.134(8) -0.027(5) -0.054(7) O11 0.071(5) 0.154(7) 0.139(6) 0.062(5) -0.024(5) -0.002(5) O12 0.136(8) 0.117(7) 0.192(8) 0.019(7) 0.042(7) 0.002(6) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag Mo1 C25 2.141(5) . ? Mo1 C19 2.144(5) . ? Mo1 C26 2.145(5) . ? Mo1 C24 2.150(5) . ? Mo1 C21 2.154(4) . ? Mo1 C22 2.163(5) . ? Mo1 C20 2.166(5) . ? Mo1 C23 2.176(4) . ? Mo2 C28 2.152(5) 3_656 ? Mo2 C28 2.152(5) . ? Mo2 C30 2.160(5) 3_656 ? Mo2 C30 2.160(5) . ? Mo2 C27 2.162(5) 3_656 ? Mo2 C27 2.162(5) . ? Mo2 C29 2.166(4) 3_656 ? Mo2 C29 2.166(4) . ? Cu1 N16 1.997(4) 8_557 ? Cu1 N3 2.010(5) . ? Cu1 N1 2.038(4) . ? Cu1 N2 2.049(4) . ? Cu1 N10 2.216(4) . ? Cu2 N6 1.998(5) . ? Cu2 N4 2.019(4) . ? Cu2 N11 2.036(4) . ? Cu2 N5 2.079(4) . ? Cu2 N15 2.139(4) 8_557 ? Cu3 N7 2.005(5) . ? Cu3 N8 2.039(4) . ? Cu3 N18 2.040(4) . ? Cu3 N9 2.043(6) . ? Cu3 N12 2.151(4) . ? N1 C1 1.458(7) . ? N2 C3 1.474(6) . ? N2 C4 1.501(6) . ? N3 C6 1.478(7) . ? N4 C7 1.476(7) . ? N5 C9 1.476(8) . ? N5 C10 1.480(7) . ? N6 C12 1.486(6) . ? N7 C13 1.486(7) . ? N8 C16 1.474(8) . ? N8 C15 1.501(7) . ? N9 C18 1.364(10) . ? N10 C19 1.150(6) . ? N11 C20 1.139(6) . ? N12 C21 1.154(5) . ? N13 C22 1.150(6) . ? N14 C23 1.147(6) . ? N15 C24 1.151(6) . ? N15 Cu2 2.139(4) 8_457 ? N16 C25 1.146(6) . ? N16 Cu1 1.997(4) 8_457 ? N17 C26 1.160(7) . ? N18 C27 1.141(6) . ? N19 C28 1.162(6) . ? N20 C29 1.147(5) . ? N21 C30 1.140(6) . ? C1 C2 1.511(8) . ? C2 C3 1.521(8) . ? C4 C5 1.530(8) . ? C5 C6 1.494(8) . ? C7 C8 1.516(8) . ? C8 C9 1.487(9) . ? C10 C11 1.509(9) . ? C11 C12 1.510(8) . ? C13 C14 1.493(9) . ? C14 C15 1.488(9) . ? C16 C17 1.557(11) . ? C17 C18 1.555(11) . ? 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 C25 Mo1 C19 103.41(19) . . ? C25 Mo1 C26 85.9(2) . . ? C19 Mo1 C26 145.15(18) . . ? C25 Mo1 C24 70.08(16) . . ? C19 Mo1 C24 75.77(17) . . ? C26 Mo1 C24 76.17(19) . . ? C25 Mo1 C21 75.61(17) . . ? C19 Mo1 C21 144.85(17) . . ? C26 Mo1 C21 69.88(18) . . ? C24 Mo1 C21 132.80(18) . . ? C25 Mo1 C22 143.90(17) . . ? C19 Mo1 C22 87.39(18) . . ? C26 Mo1 C22 104.8(2) . . ? C24 Mo1 C22 145.66(17) . . ? C21 Mo1 C22 76.12(17) . . ? C25 Mo1 C20 74.26(17) . . ? C19 Mo1 C20 72.36(17) . . ? C26 Mo1 C20 141.82(18) . . ? C24 Mo1 C20 124.10(17) . . ? C21 Mo1 C20 73.69(17) . . ? C22 Mo1 C20 76.59(17) . . ? C25 Mo1 C23 141.68(17) . . ? C19 Mo1 C23 77.00(17) . . ? C26 Mo1 C23 75.37(19) . . ? C24 Mo1 C23 73.08(17) . . ? C21 Mo1 C23 125.71(16) . . ? C22 Mo1 C23 74.08(17) . . ? C20 Mo1 C23 138.08(17) . . ? C28 Mo2 C28 80.6(2) 3_656 . ? C28 Mo2 C30 145.93(18) 3_656 3_656 ? C28 Mo2 C30 74.93(18) . 3_656 ? C28 Mo2 C30 74.93(18) 3_656 . ? C28 Mo2 C30 145.93(18) . . ? C30 Mo2 C30 136.2(3) 3_656 . ? C28 Mo2 C27 140.28(18) 3_656 3_656 ? C28 Mo2 C27 113.51(17) . 3_656 ? C30 Mo2 C27 72.51(17) 3_656 3_656 ? C30 Mo2 C27 74.31(17) . 3_656 ? C28 Mo2 C27 113.51(17) 3_656 . ? C28 Mo2 C27 140.28(18) . . ? C30 Mo2 C27 74.31(17) 3_656 . ? C30 Mo2 C27 72.51(17) . . ? C27 Mo2 C27 80.0(2) 3_656 . ? C28 Mo2 C29 72.19(18) 3_656 3_656 ? C28 Mo2 C29 76.00(17) . 3_656 ? C30 Mo2 C29 79.06(16) 3_656 3_656 ? C30 Mo2 C29 117.23(17) . 3_656 ? C27 Mo2 C29 145.67(17) 3_656 3_656 ? C27 Mo2 C29 74.01(17) . 3_656 ? C28 Mo2 C29 76.00(17) 3_656 . ? C28 Mo2 C29 72.19(18) . . ? C30 Mo2 C29 117.23(17) 3_656 . ? C30 Mo2 C29 79.06(16) . . ? C27 Mo2 C29 74.01(17) 3_656 . ? C27 Mo2 C29 145.67(17) . . ? C29 Mo2 C29 137.9(2) 3_656 . ? N16 Cu1 N3 87.5(2) 8_557 . ? N16 Cu1 N1 84.94(19) 8_557 . ? N3 Cu1 N1 160.56(19) . . ? N16 Cu1 N2 169.87(17) 8_557 . ? N3 Cu1 N2 91.94(17) . . ? N1 Cu1 N2 92.34(16) . . ? N16 Cu1 N10 95.83(17) 8_557 . ? N3 Cu1 N10 96.63(18) . . ? N1 Cu1 N10 101.95(18) . . ? N2 Cu1 N10 94.28(16) . . ? N6 Cu2 N4 161.46(17) . . ? N6 Cu2 N11 86.82(17) . . ? N4 Cu2 N11 82.64(16) . . ? N6 Cu2 N5 93.25(18) . . ? N4 Cu2 N5 93.11(18) . . ? N11 Cu2 N5 165.21(16) . . ? N6 Cu2 N15 97.06(17) . 8_557 ? N4 Cu2 N15 99.92(17) . 8_557 ? N11 Cu2 N15 101.20(17) . 8_557 ? N5 Cu2 N15 93.47(16) . 8_557 ? N7 Cu3 N8 92.6(2) . . ? N7 Cu3 N18 86.15(18) . . ? N8 Cu3 N18 173.48(17) . . ? N7 Cu3 N9 158.9(2) . . ? N8 Cu3 N9 90.2(2) . . ? N18 Cu3 N9 88.7(2) . . ? N7 Cu3 N12 96.55(18) . . ? N8 Cu3 N12 91.46(17) . . ? N18 Cu3 N12 95.03(16) . . ? N9 Cu3 N12 104.3(2) . . ? C1 N1 Cu1 121.6(3) . . ? C3 N2 C4 105.9(4) . . ? C3 N2 Cu1 115.7(3) . . ? C4 N2 Cu1 115.8(3) . . ? C6 N3 Cu1 122.0(3) . . ? C7 N4 Cu2 122.5(3) . . ? C9 N5 C10 108.3(4) . . ? C9 N5 Cu2 115.1(3) . . ? C10 N5 Cu2 113.9(3) . . ? C12 N6 Cu2 119.5(4) . . ? C13 N7 Cu3 118.8(4) . . ? C16 N8 C15 110.3(4) . . ? C16 N8 Cu3 110.4(4) . . ? C15 N8 Cu3 115.4(3) . . ? C18 N9 Cu3 121.3(6) . . ? C19 N10 Cu1 152.7(4) . . ? C20 N11 Cu2 164.1(4) . . ? C21 N12 Cu3 165.3(4) . . ? C24 N15 Cu2 165.1(4) . 8_457 ? C25 N16 Cu1 161.2(5) . 8_457 ? C27 N18 Cu3 161.2(4) . . ? N1 C1 C2 111.4(4) . . ? C1 C2 C3 113.3(4) . . ? N2 C3 C2 114.3(4) . . ? N2 C4 C5 113.3(4) . . ? C6 C5 C4 114.0(4) . . ? N3 C6 C5 109.5(4) . . ? N4 C7 C8 111.3(5) . . ? C9 C8 C7 112.8(5) . . ? N5 C9 C8 115.0(4) . . ? N5 C10 C11 115.1(5) . . ? C10 C11 C12 114.3(4) . . ? N6 C12 C11 111.8(5) . . ? N7 C13 C14 111.0(5) . . ? C15 C14 C13 114.4(5) . . ? C14 C15 N8 112.9(5) . . ? N8 C16 C17 113.8(6) . . ? C18 C17 C16 116.4(6) . . ? N9 C18 C17 111.5(7) . . ? N10 C19 Mo1 178.3(4) . . ? N11 C20 Mo1 178.2(4) . . ? N12 C21 Mo1 176.6(4) . . ? N13 C22 Mo1 174.8(4) . . ? N14 C23 Mo1 177.5(4) . . ? N15 C24 Mo1 178.3(4) . . ? N16 C25 Mo1 175.8(5) . . ? N17 C26 Mo1 175.2(6) . . ? N18 C27 Mo2 173.4(4) . . ? N19 C28 Mo2 178.0(4) . . ? N20 C29 Mo2 175.8(4) . . ? N21 C30 Mo2 173.8(4) . . ? _diffrn_measured_fraction_theta_max 0.997 _diffrn_reflns_theta_full 27.48 _diffrn_measured_fraction_theta_full 0.997 _refine_diff_density_max 1.228 _refine_diff_density_min -1.233 _refine_diff_density_rms 0.108 #end of cif #end of cif data_6_ccdc_773794 _database_code_depnum_ccdc_archive 'CCDC 773794' #TrackingRef '1.cif' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C17 H37 Cu2 Mo N14 O3.50' _chemical_formula_weight 716.63 loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Cu Cu 0.3201 1.2651 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Mo Mo -1.6832 0.6857 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting Triclinic _symmetry_space_group_name_H-M P-1 loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, -y, -z' _cell_length_a 8.8590(18) _cell_length_b 10.339(2) _cell_length_c 17.049(3) _cell_angle_alpha 72.71(3) _cell_angle_beta 80.79(3) _cell_angle_gamma 75.28(3) _cell_volume 1436.0(5) _cell_formula_units_Z 2 _cell_measurement_temperature 123(2) _cell_measurement_reflns_used 4446 _cell_measurement_theta_min 3.2 _cell_measurement_theta_max 27.5 _exptl_crystal_description platelet _exptl_crystal_colour blue _exptl_crystal_size_max 0.10 _exptl_crystal_size_mid 0.10 _exptl_crystal_size_min 0.04 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.657 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 730 _exptl_absorpt_coefficient_mu 1.945 _exptl_absorpt_correction_type Multi-scan _exptl_absorpt_correction_T_min 0.744 _exptl_absorpt_correction_T_max 0.927 _exptl_absorpt_process_details SADABS _exptl_special_details ; We spilt the 1,2-ethylenediamine group to two parts and using the same occupation and same thermal factor for both parts during the refinement. ; _diffrn_ambient_temperature 123(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'Rigaku Saturn' _diffrn_measurement_method \w _diffrn_detector_area_resol_mean 7.31 _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 11685 _diffrn_reflns_av_R_equivalents 0.0509 _diffrn_reflns_av_sigmaI/netI 0.0907 _diffrn_reflns_limit_h_min -11 _diffrn_reflns_limit_h_max 11 _diffrn_reflns_limit_k_min -12 _diffrn_reflns_limit_k_max 12 _diffrn_reflns_limit_l_min -19 _diffrn_reflns_limit_l_max 22 _diffrn_reflns_theta_min 3.21 _diffrn_reflns_theta_max 27.48 _reflns_number_total 6307 _reflns_number_gt 4661 _reflns_threshold_expression >2sigma(I) _computing_data_collection CrystalClear _computing_cell_refinement CrystalClear _computing_data_reduction CrystalStructure _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics ? _computing_publication_material ? _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^)+(0.0328P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment constr _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 6307 _refine_ls_number_parameters 352 _refine_ls_number_restraints 60 _refine_ls_R_factor_all 0.0497 _refine_ls_R_factor_gt 0.0392 _refine_ls_wR_factor_ref 0.0934 _refine_ls_wR_factor_gt 0.0912 _refine_ls_goodness_of_fit_ref 0.942 _refine_ls_restrained_S_all 0.938 _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 0.68053(4) 0.61471(3) 0.181348(19) 0.00609(9) Uani 1 1 d . . . Cu1 Cu 0.25733(5) 0.34216(4) 0.14053(3) 0.00768(11) Uani 1 1 d . . . Cu2 Cu 1.0000 1.0000 0.0000 0.01056(15) Uani 1 2 d S . . Cu3 Cu 0.5000 0.5000 0.5000 0.0275(2) Uani 1 2 d S . . N1 N 0.9240(4) 0.9150(3) -0.0759(2) 0.0118(7) Uani 1 1 d . . . H1A H 0.8631 0.8575 -0.0448 0.014 Uiso 1 1 calc R . . H1B H 0.8630 0.9839 -0.1109 0.014 Uiso 1 1 calc R . . N2 N 1.1495(4) 0.8134(3) 0.04331(19) 0.0118(7) Uani 1 1 d . . . H2A H 1.2140 0.8254 0.0751 0.014 Uiso 1 1 calc R . . H2B H 1.0926 0.7535 0.0758 0.014 Uiso 1 1 calc R . . N3 N 0.7210(4) 0.6455(3) -0.01960(19) 0.0124(7) Uani 1 1 d . . . N4 N 1.0532(4) 0.4843(3) 0.1321(2) 0.0138(7) Uani 1 1 d . . . N5 N 0.8090(4) 0.9049(3) 0.1071(2) 0.0187(8) Uani 1 1 d . . . N6 N 0.2000(4) 0.2976(3) 0.26498(19) 0.0152(7) Uani 1 1 d . . . H6A H 0.1437 0.3759 0.2772 0.018 Uiso 1 1 calc R . . H6B H 0.1375 0.2364 0.2785 0.018 Uiso 1 1 calc R . . N7 N 0.4102(4) 0.1562(3) 0.1551(2) 0.0159(7) Uani 1 1 d . . . H7C H 0.3546 0.0902 0.1657 0.019 Uiso 1 1 calc R . . H7D H 0.4681 0.1556 0.1067 0.019 Uiso 1 1 calc R . . N8 N 0.4220(4) 0.4628(3) 0.14419(19) 0.0111(7) Uani 1 1 d . . . N11 N 0.7723(4) 0.2873(3) 0.2924(2) 0.0208(8) Uani 1 1 d . . . N12 N 0.8708(6) 0.6389(5) 0.3264(2) 0.0439(12) Uani 1 1 d . . . N13 N 0.4347(5) 0.5926(5) 0.3505(3) 0.0386(11) Uani 1 1 d . . . N14 N 0.3754(5) 0.8749(4) 0.1422(3) 0.0378(11) Uani 1 1 d . . . C1 C 1.0447(5) 0.8370(4) -0.1253(2) 0.0136(8) Uani 1 1 d . . . H1C H 1.1100 0.8979 -0.1605 0.016 Uiso 1 1 calc R . . H1D H 0.9940 0.8057 -0.1605 0.016 Uiso 1 1 calc R . . C2 C 1.1457(5) 0.7136(4) -0.0713(2) 0.0137(8) Uani 1 1 d . . . H2C H 1.2137 0.6590 -0.1059 0.016 Uiso 1 1 calc R . . H2D H 1.0787 0.6560 -0.0344 0.016 Uiso 1 1 calc R . . C3 C 1.2463(4) 0.7494(4) -0.0202(2) 0.0140(8) Uani 1 1 d . . . H3A H 1.3184 0.6657 0.0064 0.017 Uiso 1 1 calc R . . H3B H 1.3077 0.8132 -0.0561 0.017 Uiso 1 1 calc R . . C4 C 0.3321(5) 0.2401(5) 0.3176(3) 0.0257(10) Uani 1 1 d . . . H4A H 0.2911 0.2260 0.3750 0.031 Uiso 1 1 calc R . . H4B H 0.3982 0.3066 0.3053 0.031 Uiso 1 1 calc R . . C5 C 0.4295(5) 0.1044(4) 0.3046(3) 0.0288(11) Uani 1 1 d . . . H5A H 0.3610 0.0408 0.3127 0.035 Uiso 1 1 calc R . . H5B H 0.5034 0.0646 0.3462 0.035 Uiso 1 1 calc R . . C6 C 0.5193(5) 0.1158(4) 0.2205(3) 0.0194(9) Uani 1 1 d . . . H6C H 0.5821 0.1847 0.2098 0.023 Uiso 1 1 calc R . . H6D H 0.5896 0.0273 0.2195 0.023 Uiso 1 1 calc R . . C10 C 0.7033(4) 0.6367(4) 0.0499(2) 0.0100(8) Uani 1 1 d . . . C11 C 0.9243(4) 0.5324(4) 0.1463(2) 0.0113(8) Uani 1 1 d . . . C12 C 0.7652(4) 0.8040(4) 0.1337(2) 0.0112(8) Uani 1 1 d . . . C13 C 0.7409(4) 0.4001(4) 0.2524(2) 0.0119(8) Uani 1 1 d . . . C14 C 0.8004(5) 0.6331(4) 0.2766(2) 0.0195(9) Uani 1 1 d . . . C15 C 0.5180(5) 0.6040(4) 0.2905(3) 0.0187(9) Uani 1 1 d . . . C16 C 0.5131(4) 0.5146(4) 0.1579(2) 0.0101(8) Uani 1 1 d . . . C17 C 0.4831(5) 0.7860(4) 0.1530(3) 0.0214(10) Uani 1 1 d . . . N9 N 0.3506(14) 0.3725(12) 0.5142(8) 0.0250(14) Uani 0.50 1 d PU A 1 H9C H 0.2672 0.4004 0.5476 0.030 Uiso 0.50 1 calc PR A 1 H9D H 0.3160 0.3890 0.4645 0.030 Uiso 0.50 1 calc PR A 1 C7 C 0.4011(13) 0.2188(11) 0.5464(7) 0.0250(14) Uani 0.50 1 d PU A 1 H7A H 0.3187 0.1754 0.5424 0.030 Uiso 0.50 1 calc PR A 1 H7B H 0.4190 0.1955 0.6041 0.030 Uiso 0.50 1 calc PR A 1 C8 C 0.5491(13) 0.1641(11) 0.4982(7) 0.0250(14) Uani 0.50 1 d PU A 1 H8A H 0.5682 0.0635 0.5134 0.030 Uiso 0.50 1 calc PR A 1 H8B H 0.5336 0.1972 0.4399 0.030 Uiso 0.50 1 calc PR A 1 C9 C 0.6918(14) 0.2058(11) 0.5117(7) 0.0250(14) Uani 0.50 1 d PU A 1 H9A H 0.6984 0.1860 0.5705 0.030 Uiso 0.50 1 calc PR A 1 H9B H 0.7847 0.1502 0.4894 0.030 Uiso 0.50 1 calc PR A 1 N10 N 0.6897(19) 0.3555(11) 0.4724(9) 0.0250(14) Uani 0.50 1 d PU A 1 H10A H 0.7004 0.3686 0.4174 0.030 Uiso 0.50 1 calc PR A 1 H10B H 0.7752 0.3736 0.4857 0.030 Uiso 0.50 1 calc PR A 1 N9' N 0.3875(17) 0.3506(13) 0.5143(9) 0.0388(19) Uani 0.50 1 d PU A 2 H9'C H 0.3025 0.3661 0.5498 0.047 Uiso 0.50 1 calc PR A 2 H9'D H 0.3520 0.3632 0.4654 0.047 Uiso 0.50 1 calc PR A 2 C7' C 0.4636(15) 0.2009(12) 0.5429(8) 0.0388(19) Uani 0.50 1 d PU A 2 H7'A H 0.4833 0.1792 0.6002 0.047 Uiso 0.50 1 calc PR A 2 H7'B H 0.3926 0.1455 0.5396 0.047 Uiso 0.50 1 calc PR A 2 C8' C 0.6120(16) 0.1631(13) 0.4940(8) 0.0388(19) Uani 0.50 1 d PU A 2 H8'A H 0.5942 0.1946 0.4360 0.047 Uiso 0.50 1 calc PR A 2 H8'B H 0.6459 0.0627 0.5083 0.047 Uiso 0.50 1 calc PR A 2 C9' C 0.7415(16) 0.2238(13) 0.5069(8) 0.0388(19) Uani 0.50 1 d PU A 2 H9'A H 0.7507 0.2029 0.5656 0.047 Uiso 0.50 1 calc PR A 2 H9'B H 0.8402 0.1814 0.4816 0.047 Uiso 0.50 1 calc PR A 2 N10' N 0.709(2) 0.3791(13) 0.4701(10) 0.0388(19) Uani 0.50 1 d PU A 2 H10C H 0.7208 0.3947 0.4149 0.047 Uiso 0.50 1 calc PR A 2 H10D H 0.7853 0.4102 0.4835 0.047 Uiso 0.50 1 calc PR A 2 O1 O 0.0106(4) 0.0563(3) 0.3550(2) 0.0430(9) Uani 1 1 d . . . O2 O 0.0891(5) 0.8417(4) 0.2734(3) 0.0748(15) Uani 1 1 d . . . O3 O 0.0907(8) 0.1282(6) 0.4932(4) 0.0333(16) Uani 0.50 1 d P . . O4 O 0.1536(14) 0.4943(11) 0.3694(11) 0.146(6) Uani 0.50 1 d P . . O5 O 0.0239(13) 0.6202(12) 0.4749(8) 0.117(5) Uani 0.50 1 d P . . 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 0.00716(15) 0.00608(17) 0.00579(16) -0.00234(12) -0.00052(11) -0.00194(11) Cu1 0.0079(2) 0.0089(2) 0.0067(2) -0.00296(18) -0.00045(17) -0.00175(17) Cu2 0.0116(3) 0.0088(3) 0.0130(3) -0.0057(3) -0.0043(3) 0.0002(3) Cu3 0.0448(5) 0.0169(4) 0.0142(4) -0.0046(3) 0.0063(4) -0.0002(4) N1 0.0152(17) 0.0068(16) 0.0148(17) -0.0052(13) -0.0018(13) -0.0020(13) N2 0.0160(17) 0.0090(16) 0.0117(16) -0.0033(13) -0.0048(13) -0.0027(13) N3 0.0160(17) 0.0127(17) 0.0103(17) -0.0038(14) -0.0018(13) -0.0051(13) N4 0.0139(18) 0.0129(17) 0.0150(17) -0.0048(14) -0.0028(13) -0.0013(13) N5 0.0210(19) 0.0127(18) 0.022(2) -0.0047(15) 0.0008(15) -0.0049(15) N6 0.0171(18) 0.0199(18) 0.0084(16) -0.0055(14) 0.0002(13) -0.0024(14) N7 0.0172(18) 0.0137(17) 0.0187(18) -0.0079(15) -0.0040(14) -0.0011(14) N8 0.0111(16) 0.0145(17) 0.0102(16) -0.0061(14) -0.0012(13) -0.0037(13) N11 0.032(2) 0.0133(19) 0.0150(18) -0.0028(16) -0.0019(16) -0.0032(16) N12 0.061(3) 0.068(3) 0.017(2) -0.003(2) -0.010(2) -0.046(3) N13 0.031(2) 0.062(3) 0.030(2) -0.024(2) 0.0121(19) -0.018(2) N14 0.027(2) 0.016(2) 0.077(3) -0.014(2) -0.027(2) 0.0009(17) C1 0.017(2) 0.011(2) 0.014(2) -0.0051(16) 0.0006(16) -0.0041(16) C2 0.018(2) 0.012(2) 0.0117(19) -0.0072(16) 0.0000(16) -0.0001(16) C3 0.013(2) 0.012(2) 0.014(2) -0.0037(16) -0.0005(16) 0.0003(15) C4 0.024(2) 0.041(3) 0.008(2) -0.004(2) -0.0023(17) -0.002(2) C5 0.027(3) 0.027(3) 0.024(2) 0.010(2) -0.013(2) -0.006(2) C6 0.017(2) 0.012(2) 0.027(2) -0.0027(18) -0.0067(18) 0.0028(16) C10 0.0126(19) 0.0073(19) 0.0110(19) -0.0004(15) -0.0010(15) -0.0061(15) C11 0.0133(19) 0.0118(19) 0.0087(18) -0.0008(15) -0.0004(15) -0.0054(15) C12 0.0107(19) 0.012(2) 0.0093(19) -0.0040(16) 0.0030(14) -0.0010(15) C13 0.016(2) 0.017(2) 0.0041(17) -0.0042(16) 0.0000(14) -0.0046(16) C14 0.026(2) 0.029(2) 0.008(2) -0.0024(18) 0.0013(17) -0.0193(19) C15 0.016(2) 0.025(2) 0.021(2) -0.0155(19) 0.0001(17) -0.0042(17) C16 0.0122(19) 0.0058(18) 0.0080(18) 0.0014(15) 0.0003(14) 0.0007(14) C17 0.018(2) 0.010(2) 0.044(3) -0.012(2) -0.012(2) -0.0034(17) N9 0.037(3) 0.018(3) 0.015(2) -0.007(2) -0.001(2) 0.0044(19) C7 0.037(3) 0.018(3) 0.015(2) -0.007(2) -0.001(2) 0.0044(19) C8 0.037(3) 0.018(3) 0.015(2) -0.007(2) -0.001(2) 0.0044(19) C9 0.037(3) 0.018(3) 0.015(2) -0.007(2) -0.001(2) 0.0044(19) N10 0.037(3) 0.018(3) 0.015(2) -0.007(2) -0.001(2) 0.0044(19) N9' 0.055(4) 0.027(3) 0.026(3) -0.007(2) -0.002(3) 0.003(2) C7' 0.055(4) 0.027(3) 0.026(3) -0.007(2) -0.002(3) 0.003(2) C8' 0.055(4) 0.027(3) 0.026(3) -0.007(2) -0.002(3) 0.003(2) C9' 0.055(4) 0.027(3) 0.026(3) -0.007(2) -0.002(3) 0.003(2) N10' 0.055(4) 0.027(3) 0.026(3) -0.007(2) -0.002(3) 0.003(2) O1 0.034(2) 0.046(2) 0.041(2) -0.0112(18) -0.0140(17) 0.0109(17) O2 0.045(3) 0.063(3) 0.121(5) -0.032(3) 0.000(3) -0.015(2) O3 0.034(4) 0.033(4) 0.030(4) -0.010(3) -0.006(3) 0.003(3) O4 0.077(9) 0.064(7) 0.31(2) -0.035(9) -0.107(11) -0.005(6) O5 0.094(9) 0.131(9) 0.145(11) -0.096(9) -0.092(8) 0.063(7) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag Mo1 C17 2.149(4) . ? Mo1 C14 2.154(4) . ? Mo1 C16 2.156(4) . ? Mo1 C15 2.156(4) . ? Mo1 C12 2.158(4) . ? Mo1 C13 2.164(4) . ? Mo1 C10 2.165(4) . ? Mo1 C11 2.168(4) . ? Cu1 N3 2.008(3) 2_665 ? Cu1 N4 2.015(3) 1_455 ? Cu1 N7 2.023(3) . ? Cu1 N6 2.041(3) . ? Cu1 N8 2.165(3) . ? Cu2 N1 2.038(3) 2_775 ? Cu2 N1 2.038(3) . ? Cu2 N2 2.047(3) . ? Cu2 N2 2.047(3) 2_775 ? Cu2 N5 2.440(4) 2_775 ? Cu2 N5 2.440(4) . ? Cu3 N9' 1.980(18) 2_666 ? Cu3 N9' 1.980(18) . ? Cu3 N9 2.035(16) . ? Cu3 N9 2.035(16) 2_666 ? Cu3 N10' 2.040(18) . ? Cu3 N10' 2.040(18) 2_666 ? Cu3 N10 2.041(15) . ? Cu3 N10 2.041(15) 2_666 ? N1 C1 1.477(5) . ? N2 C3 1.479(5) . ? N3 C10 1.149(5) . ? N3 Cu1 2.008(3) 2_665 ? N4 C11 1.142(5) . ? N4 Cu1 2.015(3) 1_655 ? N5 C12 1.146(5) . ? N6 C4 1.480(5) . ? N7 C6 1.489(5) . ? N8 C16 1.161(5) . ? N11 C13 1.151(5) . ? N12 C14 1.155(5) . ? N13 C15 1.156(5) . ? N14 C17 1.140(5) . ? C1 C2 1.504(5) . ? C2 C3 1.516(5) . ? C4 C5 1.507(6) . ? C5 C6 1.511(6) . ? N9 C7 1.492(13) . ? C7 C8 1.507(12) . ? C8 C9 1.506(14) . ? C9 N10 1.489(14) . ? N9' C7' 1.488(14) . ? C7' C8' 1.469(15) . ? C8' C9' 1.513(17) . ? C9' N10' 1.510(16) . ? 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 C17 Mo1 C14 110.52(16) . . ? C17 Mo1 C16 78.62(14) . . ? C14 Mo1 C16 143.84(14) . . ? C17 Mo1 C15 72.29(18) . . ? C14 Mo1 C15 72.90(15) . . ? C16 Mo1 C15 77.36(14) . . ? C17 Mo1 C12 71.47(15) . . ? C14 Mo1 C12 72.85(15) . . ? C16 Mo1 C12 140.41(14) . . ? C15 Mo1 C12 115.80(14) . . ? C17 Mo1 C13 141.67(16) . . ? C14 Mo1 C13 79.10(15) . . ? C16 Mo1 C13 74.03(14) . . ? C15 Mo1 C13 75.87(15) . . ? C12 Mo1 C13 143.73(15) . . ? C17 Mo1 C10 83.54(16) . . ? C14 Mo1 C10 141.59(14) . . ? C16 Mo1 C10 72.50(14) . . ? C15 Mo1 C10 144.45(15) . . ? C12 Mo1 C10 78.81(14) . . ? C13 Mo1 C10 112.42(13) . . ? C17 Mo1 C11 145.47(16) . . ? C14 Mo1 C11 76.99(15) . . ? C16 Mo1 C11 115.91(13) . . ? C15 Mo1 C11 139.35(15) . . ? C12 Mo1 C11 79.45(14) . . ? C13 Mo1 C11 72.11(14) . . ? C10 Mo1 C11 72.71(14) . . ? N3 Cu1 N4 92.31(14) 2_665 1_455 ? N3 Cu1 N7 87.14(13) 2_665 . ? N4 Cu1 N7 160.16(13) 1_455 . ? N3 Cu1 N6 165.85(13) 2_665 . ? N4 Cu1 N6 85.80(13) 1_455 . ? N7 Cu1 N6 89.90(14) . . ? N3 Cu1 N8 100.90(12) 2_665 . ? N4 Cu1 N8 102.18(12) 1_455 . ? N7 Cu1 N8 97.39(12) . . ? N6 Cu1 N8 93.20(13) . . ? N1 Cu2 N1 180.0 2_775 . ? N1 Cu2 N2 91.07(12) 2_775 . ? N1 Cu2 N2 88.93(12) . . ? N1 Cu2 N2 88.93(12) 2_775 2_775 ? N1 Cu2 N2 91.07(12) . 2_775 ? N2 Cu2 N2 180.00(18) . 2_775 ? N1 Cu2 N5 87.22(12) 2_775 2_775 ? N1 Cu2 N5 92.78(12) . 2_775 ? N2 Cu2 N5 94.89(12) . 2_775 ? N2 Cu2 N5 85.11(12) 2_775 2_775 ? N1 Cu2 N5 92.78(12) 2_775 . ? N1 Cu2 N5 87.22(12) . . ? N2 Cu2 N5 85.11(12) . . ? N2 Cu2 N5 94.89(12) 2_775 . ? N5 Cu2 N5 180.0 2_775 . ? N9' Cu3 N9' 180.0(8) 2_666 . ? N9' Cu3 N9 170.2(4) 2_666 . ? N9' Cu3 N9 9.8(4) . . ? N9' Cu3 N9 9.8(4) 2_666 2_666 ? N9' Cu3 N9 170.2(4) . 2_666 ? N9 Cu3 N9 180.0(7) . 2_666 ? N9' Cu3 N10' 87.8(4) 2_666 . ? N9' Cu3 N10' 92.2(4) . . ? N9 Cu3 N10' 101.7(4) . . ? N9 Cu3 N10' 78.3(4) 2_666 . ? N9' Cu3 N10' 92.2(4) 2_666 2_666 ? N9' Cu3 N10' 87.8(4) . 2_666 ? N9 Cu3 N10' 78.3(4) . 2_666 ? N9 Cu3 N10' 101.7(4) 2_666 2_666 ? N10' Cu3 N10' 180.000(3) . 2_666 ? N9' Cu3 N10 96.9(5) 2_666 . ? N9' Cu3 N10 83.1(5) . . ? N9 Cu3 N10 92.6(4) . . ? N9 Cu3 N10 87.4(4) 2_666 . ? N10' Cu3 N10 9.1(6) . . ? N10' Cu3 N10 170.9(6) 2_666 . ? N9' Cu3 N10 83.1(5) 2_666 2_666 ? N9' Cu3 N10 96.9(5) . 2_666 ? N9 Cu3 N10 87.4(4) . 2_666 ? N9 Cu3 N10 92.6(4) 2_666 2_666 ? N10' Cu3 N10 170.9(6) . 2_666 ? N10' Cu3 N10 9.1(6) 2_666 2_666 ? N10 Cu3 N10 180.000(2) . 2_666 ? C1 N1 Cu2 117.3(2) . . ? C3 N2 Cu2 115.8(2) . . ? C10 N3 Cu1 177.4(3) . 2_665 ? C11 N4 Cu1 158.9(3) . 1_655 ? C12 N5 Cu2 139.3(3) . . ? C4 N6 Cu1 116.5(3) . . ? C6 N7 Cu1 117.3(2) . . ? C16 N8 Cu1 169.8(3) . . ? N1 C1 C2 111.6(3) . . ? C1 C2 C3 114.6(3) . . ? N2 C3 C2 111.4(3) . . ? N6 C4 C5 112.3(4) . . ? C4 C5 C6 114.5(4) . . ? N7 C6 C5 110.7(3) . . ? N3 C10 Mo1 177.5(3) . . ? N4 C11 Mo1 176.3(3) . . ? N5 C12 Mo1 178.7(3) . . ? N11 C13 Mo1 177.9(3) . . ? N12 C14 Mo1 176.8(4) . . ? N13 C15 Mo1 177.0(4) . . ? N8 C16 Mo1 178.8(3) . . ? N14 C17 Mo1 176.3(5) . . ? C7 N9 Cu3 121.6(8) . . ? N9 C7 C8 110.6(9) . . ? C9 C8 C7 114.0(9) . . ? N10 C9 C8 112.8(9) . . ? C9 N10 Cu3 118.7(9) . . ? C7' N9' Cu3 122.4(10) . . ? C8' C7' N9' 112.6(10) . . ? C7' C8' C9' 113.5(11) . . ? N10' C9' C8' 111.3(11) . . ? C9' N10' Cu3 120.0(10) . . ? _diffrn_measured_fraction_theta_max 0.956 _diffrn_reflns_theta_full 27.48 _diffrn_measured_fraction_theta_full 0.956 _refine_diff_density_max 1.638 _refine_diff_density_min -0.893 _refine_diff_density_rms 0.134