# Electronic Supplementary Material (ESI) for Dalton Transactions # This journal is © The Royal Society of Chemistry 2011 data_global _journal_name_full 'Dalton Trans.' _journal_coden_cambridge 0222 #TrackingRef '- Structure(2).cif' _audit_creation_method shelxl-97 _publ_contact_author_name 'Prof. Samar K. Das' _publ_contact_author_address ; School of Chemistry University of Hyderabad Hyderabad 500 046, India ; _publ_contact_author_email skdsc@uohyd.ernet.in _publ_contact_author_phone '91 40 23011007' _publ_contact_author_fax ? loop_ _publ_author_name _publ_author_address 'Monima Sarma' ; School of Chemistry University of Hyderabad Hyderabad 500 046, India ; 'Tanmay Chatterjee' ; School of Chemistry University of Hyderabad Hyderabad 500 046, India ; S.K.Das ; School of Chemistry University of Hyderabad Hyderabad 500 046, India ; data_Cu-TDE-W6(1P) _database_code_depnum_ccdc_archive 'CCDC 834664' #TrackingRef '- Structure(2).cif' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety 'C18 H35 Cu N5, O19 W6' _chemical_formula_sum 'C18 H35 Cu N5 O19 W6' _chemical_formula_weight 1792.13 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' W W -0.8490 6.8722 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting Orthorhombic _symmetry_space_group_name_H-M 'P 21 21 21' _symmetry_space_group_name_Hall 'P 2ac 2ab' loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x+1/2, -y, z+1/2' '-x, y+1/2, -z+1/2' 'x+1/2, -y+1/2, -z' _cell_length_a 11.0430(9) _cell_length_b 15.0977(12) _cell_length_c 20.7375(17) _cell_angle_alpha 90.00 _cell_angle_beta 90.00 _cell_angle_gamma 90.00 _cell_volume 3457.4(5) _cell_formula_units_Z 4 _cell_measurement_temperature 298(2) _cell_measurement_reflns_used 7409 _cell_measurement_theta_min 2.29 _cell_measurement_theta_max 25.90 _exptl_crystal_description Block _exptl_crystal_colour Red _exptl_crystal_size_max 0.22 _exptl_crystal_size_mid 0.12 _exptl_crystal_size_min 0.08 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 3.439 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 3204 _exptl_absorpt_coefficient_mu 20.561 _exptl_absorpt_correction_type Empirical _exptl_absorpt_correction_T_min 0.0930 _exptl_absorpt_correction_T_max 0.2900 _exptl_absorpt_process_details 'Bruker SADABS' _exptl_special_details ; ? ; _diffrn_ambient_temperature 298(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'CCD Area Detector' _diffrn_measurement_method 'Phi and Omega Scans' _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 32509 _diffrn_reflns_av_R_equivalents 0.0561 _diffrn_reflns_av_sigmaI/netI 0.0422 _diffrn_reflns_limit_h_min -13 _diffrn_reflns_limit_h_max 13 _diffrn_reflns_limit_k_min -17 _diffrn_reflns_limit_k_max 17 _diffrn_reflns_limit_l_min -24 _diffrn_reflns_limit_l_max 24 _diffrn_reflns_theta_min 1.67 _diffrn_reflns_theta_max 25.00 _reflns_number_total 6084 _reflns_number_gt 5612 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'Bruker SMART' _computing_cell_refinement 'Bruker SMART' _computing_data_reduction 'Bruker SAINT' _computing_structure_solution 'Bruker SHELXTL' _computing_structure_refinement 'Bruker SHELXTL' _computing_molecular_graphics 'Bruker SHELXTL' _computing_publication_material 'Bruker SHELXTL' _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^)+(0.0211P)^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_abs_structure_details 'Flack H D (1983), Acta Cryst. A39, 876-881' _refine_ls_abs_structure_Flack -0.002(13) _refine_ls_number_reflns 6084 _refine_ls_number_parameters 449 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0331 _refine_ls_R_factor_gt 0.0285 _refine_ls_wR_factor_ref 0.0547 _refine_ls_wR_factor_gt 0.0533 _refine_ls_goodness_of_fit_ref 1.016 _refine_ls_restrained_S_all 1.016 _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 C1 C 0.3698(11) 0.6629(8) 0.3455(5) 0.046(3) Uani 1 1 d . . . H1A H 0.3955 0.6659 0.3902 0.055 Uiso 1 1 calc R . . H1B H 0.3095 0.7087 0.3385 0.055 Uiso 1 1 calc R . . C2 C 0.4763(9) 0.6789(7) 0.3023(5) 0.035(3) Uani 1 1 d . . . H2A H 0.5043 0.7396 0.3066 0.042 Uiso 1 1 calc R . . H2B H 0.5423 0.6394 0.3134 0.042 Uiso 1 1 calc R . . C3 C 0.4852(9) 0.7002(7) 0.1881(5) 0.032(3) Uani 1 1 d . . . C4 C 0.4383(9) 0.6849(7) 0.1216(5) 0.033(3) Uani 1 1 d . . . H4A H 0.4997 0.6516 0.0986 0.040 Uiso 1 1 calc R . . H4B H 0.4331 0.7424 0.1009 0.040 Uiso 1 1 calc R . . C5 C 0.3182(9) 0.6383(8) 0.1098(5) 0.035(3) Uani 1 1 d . . . C6 C 0.2296(10) 0.4823(8) 0.1219(5) 0.044(3) Uani 1 1 d . . . H6A H 0.1513 0.5114 0.1209 0.052 Uiso 1 1 calc R . . H6B H 0.2452 0.4574 0.0796 0.052 Uiso 1 1 calc R . . C7 C 0.2294(10) 0.4128(8) 0.1700(5) 0.041(3) Uani 1 1 d . . . H7A H 0.3035 0.3785 0.1670 0.050 Uiso 1 1 calc R . . H7B H 0.1615 0.3733 0.1627 0.050 Uiso 1 1 calc R . . C8 C 0.1566(9) 0.4228(8) 0.2812(6) 0.040(3) Uani 1 1 d . . . C9 C 0.1557(10) 0.4651(8) 0.3468(5) 0.044(3) Uani 1 1 d . . . H9A H 0.2108 0.4316 0.3738 0.053 Uiso 1 1 calc R . . H9B H 0.0752 0.4570 0.3645 0.053 Uiso 1 1 calc R . . C10 C 0.1882(10) 0.5633(8) 0.3547(5) 0.040(3) Uani 1 1 d . . . C11 C 0.5943(10) 0.7585(8) 0.1924(6) 0.052(3) Uani 1 1 d . . . H11A H 0.5706 0.8161 0.2075 0.078 Uiso 1 1 calc R . . H11B H 0.6306 0.7638 0.1505 0.078 Uiso 1 1 calc R . . H11C H 0.6516 0.7331 0.2218 0.078 Uiso 1 1 calc R . . C12 C 0.2122(9) 0.6891(8) 0.1397(5) 0.038(3) Uani 1 1 d . . . H12A H 0.1373 0.6645 0.1246 0.058 Uiso 1 1 calc R . . H12B H 0.2170 0.7503 0.1275 0.058 Uiso 1 1 calc R . . H12C H 0.2160 0.6843 0.1858 0.058 Uiso 1 1 calc R . . C13 C 0.2963(10) 0.6338(9) 0.0363(5) 0.042(3) Uani 1 1 d . . . H13A H 0.3555 0.5956 0.0169 0.063 Uiso 1 1 calc R . . H13B H 0.3032 0.6921 0.0182 0.063 Uiso 1 1 calc R . . H13C H 0.2167 0.6109 0.0281 0.063 Uiso 1 1 calc R . . C14 C 0.0820(11) 0.3401(9) 0.2770(7) 0.067(4) Uani 1 1 d . . . H14A H 0.0058 0.3533 0.2569 0.101 Uiso 1 1 calc R . . H14B H 0.0680 0.3173 0.3196 0.101 Uiso 1 1 calc R . . H14C H 0.1244 0.2966 0.2518 0.101 Uiso 1 1 calc R . . C15 C 0.1795(11) 0.5864(10) 0.4261(6) 0.061(4) Uani 1 1 d . . . H15A H 0.2371 0.5517 0.4499 0.092 Uiso 1 1 calc R . . H15B H 0.0993 0.5738 0.4414 0.092 Uiso 1 1 calc R . . H15C H 0.1967 0.6482 0.4320 0.092 Uiso 1 1 calc R . . C16 C 0.0998(10) 0.6214(9) 0.3165(6) 0.052(3) Uani 1 1 d . . . H16A H 0.1198 0.6827 0.3229 0.078 Uiso 1 1 calc R . . H16B H 0.0186 0.6107 0.3312 0.078 Uiso 1 1 calc R . . H16C H 0.1055 0.6073 0.2715 0.078 Uiso 1 1 calc R . . C17 C 0.7372(10) 0.4293(13) 0.2690(6) 0.081(5) Uani 1 1 d . . . H17A H 0.7650 0.3944 0.2333 0.121 Uiso 1 1 calc R . . H17B H 0.7465 0.3961 0.3082 0.121 Uiso 1 1 calc R . . H17C H 0.7839 0.4828 0.2717 0.121 Uiso 1 1 calc R . . C18 C 0.6099(10) 0.4514(8) 0.2599(5) 0.037(3) Uani 1 1 d . . . Cu1 Cu 0.33105(11) 0.55577(9) 0.23633(6) 0.0306(3) Uani 1 1 d . . . N1 N 0.3157(7) 0.5753(6) 0.3325(4) 0.030(2) Uani 1 1 d . . . N2 N 0.4355(7) 0.6621(5) 0.2360(4) 0.0281(19) Uani 1 1 d . . . N3 N 0.3290(8) 0.5496(6) 0.1393(4) 0.034(2) Uani 1 1 d . . . N4 N 0.2195(7) 0.4544(6) 0.2362(5) 0.039(2) Uani 1 1 d . . . N5 N 0.5106(9) 0.4684(7) 0.2532(5) 0.048(3) Uani 1 1 d . . . O1 O 0.7266(7) 0.3153(6) -0.1372(4) 0.051(2) Uani 1 1 d . . . O2 O 0.6549(6) 0.4852(5) -0.0887(3) 0.0386(19) Uani 1 1 d . . . O3 O 0.8621(6) 0.3144(5) -0.0192(4) 0.0383(18) Uani 1 1 d . . . O4 O 0.8892(6) 0.4493(5) -0.0982(3) 0.0363(18) Uani 1 1 d . . . O5 O 0.6289(6) 0.3493(5) -0.0094(3) 0.0373(18) Uani 1 1 d . . . O6 O 0.5634(6) 0.6540(5) -0.0606(4) 0.055(2) Uani 1 1 d . . . O7 O 0.5559(6) 0.5103(4) 0.0251(3) 0.0308(16) Uani 1 1 d . . . O8 O 0.8152(6) 0.6099(5) -0.0648(3) 0.0388(19) Uani 1 1 d . . . O9 O 0.5081(6) 0.3687(5) 0.1122(4) 0.044(2) Uani 1 1 d . . . O10 O 0.7166(6) 0.6364(5) 0.0489(3) 0.0386(18) Uani 1 1 d . . . O11 O 0.6899(6) 0.5017(5) 0.1296(3) 0.0305(17) Uani 1 1 d . . . O12 O 0.8572(8) 0.6361(6) 0.1657(4) 0.056(2) Uani 1 1 d . . . O13 O 0.9228(6) 0.4654(5) 0.1208(3) 0.0365(18) Uani 1 1 d . . . O14 O 0.9516(6) 0.5990(5) 0.0402(3) 0.0330(17) Uani 1 1 d . . . O15 O 1.0122(7) 0.2920(6) 0.0929(4) 0.052(2) Uani 1 1 d . . . O16 O 0.7621(6) 0.3406(5) 0.0959(3) 0.0365(18) Uani 1 1 d . . . O17 O 1.0225(6) 0.4400(5) 0.0055(3) 0.0345(18) Uani 1 1 d . . . O18 O 1.0718(6) 0.5803(5) -0.0817(4) 0.049(2) Uani 1 1 d . . . O19 O 0.7903(6) 0.4750(5) 0.0160(3) 0.0300(16) Uani 1 1 d . . . W1 W 0.75127(4) 0.38029(3) -0.07135(2) 0.03512(12) Uani 1 1 d . . . W2 W 0.66056(4) 0.57975(3) -0.02850(2) 0.03458(12) Uani 1 1 d . . . W3 W 0.82783(4) 0.56848(3) 0.10216(2) 0.03422(12) Uani 1 1 d . . . W4 W 0.91863(4) 0.36934(3) 0.05933(2) 0.03381(11) Uani 1 1 d . . . W5 W 0.62774(4) 0.41209(3) 0.07057(2) 0.03093(11) Uani 1 1 d . . . W6 W 0.95105(4) 0.53698(3) -0.03970(2) 0.03204(11) 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 C1 0.058(8) 0.053(9) 0.027(6) -0.003(6) -0.001(6) 0.015(7) C2 0.043(6) 0.031(7) 0.031(6) 0.001(5) 0.001(5) -0.010(5) C3 0.037(6) 0.020(6) 0.038(6) 0.006(5) -0.002(5) 0.016(5) C4 0.043(6) 0.030(6) 0.027(6) 0.009(5) -0.002(5) 0.005(5) C5 0.024(5) 0.047(8) 0.033(6) 0.000(5) -0.002(5) 0.008(5) C6 0.046(7) 0.044(8) 0.041(7) -0.004(6) -0.013(6) -0.012(6) C7 0.042(7) 0.039(8) 0.043(7) -0.005(6) 0.000(5) -0.007(6) C8 0.021(5) 0.033(7) 0.065(8) 0.009(6) 0.007(5) 0.006(5) C9 0.029(6) 0.051(8) 0.053(8) 0.019(6) 0.012(5) -0.006(6) C10 0.039(6) 0.047(8) 0.033(6) -0.001(5) 0.013(5) 0.000(6) C11 0.057(8) 0.054(9) 0.045(8) -0.004(6) 0.004(6) -0.022(7) C12 0.033(6) 0.042(8) 0.041(7) 0.005(6) -0.003(5) -0.002(5) C13 0.043(6) 0.056(8) 0.027(6) 0.005(6) -0.011(5) -0.001(6) C14 0.049(8) 0.056(10) 0.097(12) 0.021(8) 0.017(8) -0.005(7) C15 0.060(8) 0.072(10) 0.051(8) 0.002(8) 0.013(7) 0.000(8) C16 0.043(7) 0.048(8) 0.066(9) 0.010(7) 0.013(6) 0.011(6) C17 0.050(8) 0.150(17) 0.042(8) 0.004(9) -0.012(6) 0.042(9) C18 0.040(7) 0.043(8) 0.029(6) 0.002(5) 0.002(5) 0.007(6) Cu1 0.0307(7) 0.0318(8) 0.0293(7) -0.0010(6) 0.0006(5) -0.0023(6) N1 0.032(5) 0.025(5) 0.034(5) -0.004(4) 0.009(4) -0.009(4) N2 0.037(5) 0.021(5) 0.026(5) -0.003(4) -0.004(4) -0.002(4) N3 0.040(5) 0.034(6) 0.029(5) -0.005(4) -0.010(4) 0.000(4) N4 0.038(5) 0.028(6) 0.051(6) 0.002(5) 0.005(5) -0.010(4) N5 0.044(6) 0.057(7) 0.042(6) 0.004(5) 0.007(5) 0.003(5) O1 0.049(5) 0.063(6) 0.041(5) -0.018(4) 0.006(4) -0.021(4) O2 0.035(4) 0.048(5) 0.033(4) 0.010(4) -0.002(3) -0.007(4) O3 0.039(4) 0.023(4) 0.053(5) -0.004(4) 0.004(4) -0.003(3) O4 0.031(4) 0.047(5) 0.031(4) -0.009(4) 0.004(3) -0.003(4) O5 0.037(4) 0.041(5) 0.034(4) -0.001(4) 0.004(3) -0.012(4) O6 0.034(4) 0.056(6) 0.074(6) 0.030(5) -0.005(4) 0.002(4) O7 0.030(4) 0.029(4) 0.034(4) 0.005(3) 0.005(3) 0.000(3) O8 0.034(4) 0.039(5) 0.044(5) 0.017(4) 0.002(4) -0.006(3) O9 0.038(4) 0.042(5) 0.052(5) 0.007(4) 0.015(4) -0.008(4) O10 0.041(4) 0.027(4) 0.048(5) -0.004(4) 0.004(4) 0.000(3) O11 0.034(4) 0.035(4) 0.022(4) 0.001(3) 0.010(3) 0.000(3) O12 0.063(5) 0.060(6) 0.046(5) -0.018(5) -0.001(4) 0.000(5) O13 0.033(4) 0.048(5) 0.028(4) -0.001(4) -0.008(3) -0.004(4) O14 0.028(4) 0.034(4) 0.038(4) -0.008(3) -0.001(3) -0.010(3) O15 0.045(5) 0.047(5) 0.064(6) 0.017(5) -0.002(4) 0.011(4) O16 0.041(4) 0.034(5) 0.034(4) 0.007(4) 0.003(3) 0.000(4) O17 0.025(4) 0.047(5) 0.031(4) -0.004(4) 0.000(3) 0.003(3) O18 0.039(4) 0.059(6) 0.048(5) 0.004(4) 0.009(4) -0.011(4) O19 0.032(4) 0.034(4) 0.024(3) 0.001(3) 0.007(3) -0.001(3) W1 0.0335(2) 0.0427(3) 0.0292(2) -0.0096(2) 0.0027(2) -0.0084(2) W2 0.0294(2) 0.0366(3) 0.0377(3) 0.0092(2) -0.00064(19) -0.0002(2) W3 0.0353(2) 0.0359(3) 0.0314(2) -0.0086(2) 0.0003(2) -0.0021(2) W4 0.0312(2) 0.0324(3) 0.0378(3) 0.0021(2) -0.00087(19) 0.0036(2) W5 0.0297(2) 0.0335(3) 0.0297(2) 0.0021(2) 0.00544(19) -0.00219(19) W6 0.0271(2) 0.0377(3) 0.0313(2) 0.0004(2) 0.00320(19) -0.0059(2) _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 C1 N1 1.477(14) . ? C1 C2 1.499(14) . ? C1 H1A 0.9700 . ? C1 H1B 0.9700 . ? C2 N2 1.468(12) . ? C2 H2A 0.9700 . ? C2 H2B 0.9700 . ? C3 N2 1.272(13) . ? C3 C4 1.492(14) . ? C3 C11 1.495(14) . ? C4 C5 1.521(14) . ? C4 H4A 0.9700 . ? C4 H4B 0.9700 . ? C5 N3 1.477(14) . ? C5 C12 1.530(14) . ? C5 C13 1.546(13) . ? C6 C7 1.448(15) . ? C6 N3 1.539(13) . ? C6 H6A 0.9700 . ? C6 H6B 0.9700 . ? C7 N4 1.515(13) . ? C7 H7A 0.9700 . ? C7 H7B 0.9700 . ? C8 N4 1.256(13) . ? C8 C14 1.499(16) . ? C8 C9 1.503(16) . ? C9 C10 1.534(16) . ? C9 H9A 0.9700 . ? C9 H9B 0.9700 . ? C10 N1 1.493(13) . ? C10 C15 1.524(15) . ? C10 C16 1.534(15) . ? C11 H11A 0.9600 . ? C11 H11B 0.9600 . ? C11 H11C 0.9600 . ? C12 H12A 0.9600 . ? C12 H12B 0.9600 . ? C12 H12C 0.9600 . ? C13 H13A 0.9600 . ? C13 H13B 0.9600 . ? C13 H13C 0.9600 . ? C14 H14A 0.9600 . ? C14 H14B 0.9600 . ? C14 H14C 0.9600 . ? C15 H15A 0.9600 . ? C15 H15B 0.9600 . ? C15 H15C 0.9600 . ? C16 H16A 0.9600 . ? C16 H16B 0.9600 . ? C16 H16C 0.9600 . ? C17 C18 1.458(14) . ? C17 H17A 0.9600 . ? C17 H17B 0.9600 . ? C17 H17C 0.9600 . ? C18 N5 1.134(12) . ? Cu1 N4 1.964(9) . ? Cu1 N2 1.977(8) . ? Cu1 N3 2.015(8) . ? Cu1 N1 2.023(8) . ? Cu1 N5 2.407(10) . ? O1 W1 1.703(7) . ? O2 W2 1.898(7) . ? O2 W1 1.942(7) . ? O3 W1 1.912(7) . ? O3 W4 1.931(7) . ? O4 W6 1.922(7) . ? O4 W1 1.928(7) . ? O5 W5 1.911(7) . ? O5 W1 1.922(7) . ? O6 W2 1.687(7) . ? O7 W2 1.916(6) . ? O7 W5 1.928(6) . ? O8 W2 1.921(7) . ? O8 W6 1.932(7) . ? O9 W5 1.709(6) . ? O10 W2 1.921(7) . ? O10 W3 1.944(7) . ? O11 W3 1.913(7) . ? O11 W5 1.949(7) . ? O12 W3 1.698(8) . ? O13 W3 1.916(7) . ? O13 W4 1.931(7) . ? O14 W6 1.904(7) . ? O14 W3 1.931(6) . ? O15 W4 1.708(7) . ? O16 W5 1.908(7) . ? O16 W4 1.936(7) . ? O17 W6 1.909(7) . ? O17 W4 1.924(7) . ? O18 W6 1.722(7) . ? O19 W3 2.315(7) . ? O19 W6 2.315(7) . ? O19 W4 2.315(7) . ? O19 W2 2.325(7) . ? O19 W5 2.325(7) . ? O19 W1 2.347(7) . ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag N1 C1 C2 110.7(9) . . ? N1 C1 H1A 109.5 . . ? C2 C1 H1A 109.5 . . ? N1 C1 H1B 109.5 . . ? C2 C1 H1B 109.5 . . ? H1A C1 H1B 108.1 . . ? N2 C2 C1 106.9(8) . . ? N2 C2 H2A 110.3 . . ? C1 C2 H2A 110.3 . . ? N2 C2 H2B 110.3 . . ? C1 C2 H2B 110.3 . . ? H2A C2 H2B 108.6 . . ? N2 C3 C4 120.1(10) . . ? N2 C3 C11 124.6(10) . . ? C4 C3 C11 115.2(10) . . ? C3 C4 C5 121.5(9) . . ? C3 C4 H4A 106.9 . . ? C5 C4 H4A 106.9 . . ? C3 C4 H4B 106.9 . . ? C5 C4 H4B 106.9 . . ? H4A C4 H4B 106.7 . . ? N3 C5 C4 106.4(8) . . ? N3 C5 C12 110.4(9) . . ? C4 C5 C12 111.8(9) . . ? N3 C5 C13 112.4(10) . . ? C4 C5 C13 108.4(9) . . ? C12 C5 C13 107.6(8) . . ? C7 C6 N3 108.6(9) . . ? C7 C6 H6A 110.0 . . ? N3 C6 H6A 110.0 . . ? C7 C6 H6B 110.0 . . ? N3 C6 H6B 110.0 . . ? H6A C6 H6B 108.4 . . ? C6 C7 N4 108.9(9) . . ? C6 C7 H7A 109.9 . . ? N4 C7 H7A 109.9 . . ? C6 C7 H7B 109.9 . . ? N4 C7 H7B 109.9 . . ? H7A C7 H7B 108.3 . . ? N4 C8 C14 125.3(12) . . ? N4 C8 C9 120.9(11) . . ? C14 C8 C9 113.8(10) . . ? C8 C9 C10 120.4(9) . . ? C8 C9 H9A 107.2 . . ? C10 C9 H9A 107.2 . . ? C8 C9 H9B 107.2 . . ? C10 C9 H9B 107.2 . . ? H9A C9 H9B 106.9 . . ? N1 C10 C15 109.4(9) . . ? N1 C10 C16 111.8(9) . . ? C15 C10 C16 109.4(10) . . ? N1 C10 C9 107.7(9) . . ? C15 C10 C9 108.1(10) . . ? C16 C10 C9 110.4(10) . . ? C3 C11 H11A 109.5 . . ? C3 C11 H11B 109.5 . . ? H11A C11 H11B 109.5 . . ? C3 C11 H11C 109.5 . . ? H11A C11 H11C 109.5 . . ? H11B C11 H11C 109.5 . . ? C5 C12 H12A 109.5 . . ? C5 C12 H12B 109.5 . . ? H12A C12 H12B 109.5 . . ? C5 C12 H12C 109.5 . . ? H12A C12 H12C 109.5 . . ? H12B C12 H12C 109.5 . . ? C5 C13 H13A 109.5 . . ? C5 C13 H13B 109.5 . . ? H13A C13 H13B 109.5 . . ? C5 C13 H13C 109.5 . . ? H13A C13 H13C 109.5 . . ? H13B C13 H13C 109.5 . . ? C8 C14 H14A 109.5 . . ? C8 C14 H14B 109.5 . . ? H14A C14 H14B 109.5 . . ? C8 C14 H14C 109.5 . . ? H14A C14 H14C 109.5 . . ? H14B C14 H14C 109.5 . . ? C10 C15 H15A 109.5 . . ? C10 C15 H15B 109.5 . . ? H15A C15 H15B 109.5 . . ? C10 C15 H15C 109.5 . . ? H15A C15 H15C 109.5 . . ? H15B C15 H15C 109.5 . . ? C10 C16 H16A 109.5 . . ? C10 C16 H16B 109.5 . . ? H16A C16 H16B 109.5 . . ? C10 C16 H16C 109.5 . . ? H16A C16 H16C 109.5 . . ? H16B C16 H16C 109.5 . . ? C18 C17 H17A 109.5 . . ? C18 C17 H17B 109.5 . . ? H17A C17 H17B 109.5 . . ? C18 C17 H17C 109.5 . . ? H17A C17 H17C 109.5 . . ? H17B C17 H17C 109.5 . . ? N5 C18 C17 179.5(14) . . ? N4 Cu1 N2 176.9(3) . . ? N4 Cu1 N3 87.5(4) . . ? N2 Cu1 N3 92.3(3) . . ? N4 Cu1 N1 93.5(4) . . ? N2 Cu1 N1 86.2(3) . . ? N3 Cu1 N1 172.1(3) . . ? N4 Cu1 N5 95.2(4) . . ? N2 Cu1 N5 88.0(3) . . ? N3 Cu1 N5 97.4(3) . . ? N1 Cu1 N5 90.3(3) . . ? C1 N1 C10 115.7(8) . . ? C1 N1 Cu1 106.0(6) . . ? C10 N1 Cu1 111.5(6) . . ? C3 N2 C2 121.3(9) . . ? C3 N2 Cu1 128.5(7) . . ? C2 N2 Cu1 108.5(6) . . ? C5 N3 C6 116.4(8) . . ? C5 N3 Cu1 111.9(6) . . ? C6 N3 Cu1 105.8(6) . . ? C8 N4 C7 123.7(10) . . ? C8 N4 Cu1 129.9(9) . . ? C7 N4 Cu1 106.2(6) . . ? C18 N5 Cu1 159.7(10) . . ? W2 O2 W1 118.2(3) . . ? W1 O3 W4 117.4(4) . . ? W6 O4 W1 118.0(3) . . ? W5 O5 W1 117.6(4) . . ? W2 O7 W5 117.1(3) . . ? W2 O8 W6 116.7(3) . . ? W2 O10 W3 116.4(4) . . ? W3 O11 W5 117.3(3) . . ? W3 O13 W4 117.6(3) . . ? W6 O14 W3 117.4(3) . . ? W5 O16 W4 117.4(3) . . ? W6 O17 W4 117.6(3) . . ? W3 O19 W6 90.1(3) . . ? W3 O19 W4 90.6(2) . . ? W6 O19 W4 90.2(2) . . ? W3 O19 W2 90.1(3) . . ? W6 O19 W2 90.0(2) . . ? W4 O19 W2 179.3(4) . . ? W3 O19 W5 90.7(2) . . ? W6 O19 W5 179.2(4) . . ? W4 O19 W5 90.1(2) . . ? W2 O19 W5 89.7(2) . . ? W3 O19 W1 179.7(4) . . ? W6 O19 W1 90.1(2) . . ? W4 O19 W1 89.6(3) . . ? W2 O19 W1 89.7(2) . . ? W5 O19 W1 89.1(2) . . ? O1 W1 O3 104.8(4) . . ? O1 W1 O5 106.4(3) . . ? O3 W1 O5 86.8(3) . . ? O1 W1 O4 101.9(3) . . ? O3 W1 O4 86.5(3) . . ? O5 W1 O4 151.7(3) . . ? O1 W1 O2 103.5(4) . . ? O3 W1 O2 151.6(3) . . ? O5 W1 O2 86.4(3) . . ? O4 W1 O2 86.5(3) . . ? O1 W1 O19 177.1(3) . . ? O3 W1 O19 76.3(3) . . ? O5 W1 O19 76.2(3) . . ? O4 W1 O19 75.5(3) . . ? O2 W1 O19 75.4(3) . . ? O6 W2 O2 102.7(4) . . ? O6 W2 O7 102.0(3) . . ? O2 W2 O7 87.1(3) . . ? O6 W2 O10 103.8(4) . . ? O2 W2 O10 153.5(3) . . ? O7 W2 O10 87.3(3) . . ? O6 W2 O8 104.7(3) . . ? O2 W2 O8 87.1(3) . . ? O7 W2 O8 153.3(3) . . ? O10 W2 O8 86.3(3) . . ? O6 W2 O19 178.5(3) . . ? O2 W2 O19 76.7(3) . . ? O7 W2 O19 76.7(3) . . ? O10 W2 O19 76.8(3) . . ? O8 W2 O19 76.6(3) . . ? O12 W3 O11 103.8(3) . . ? O12 W3 O13 103.1(4) . . ? O11 W3 O13 87.0(3) . . ? O12 W3 O14 103.7(3) . . ? O11 W3 O14 152.5(3) . . ? O13 W3 O14 86.6(3) . . ? O12 W3 O10 104.2(4) . . ? O11 W3 O10 86.8(3) . . ? O13 W3 O10 152.7(3) . . ? O14 W3 O10 86.8(3) . . ? O12 W3 O19 179.1(4) . . ? O11 W3 O19 76.4(3) . . ? O13 W3 O19 76.0(3) . . ? O14 W3 O19 76.0(3) . . ? O10 W3 O19 76.7(3) . . ? O15 W4 O17 104.7(3) . . ? O15 W4 O3 104.2(4) . . ? O17 W4 O3 86.7(3) . . ? O15 W4 O13 103.3(4) . . ? O17 W4 O13 87.3(3) . . ? O3 W4 O13 152.5(3) . . ? O15 W4 O16 103.2(3) . . ? O17 W4 O16 152.1(3) . . ? O3 W4 O16 86.9(3) . . ? O13 W4 O16 86.0(3) . . ? O15 W4 O19 178.8(3) . . ? O17 W4 O19 76.0(3) . . ? O3 W4 O19 76.7(3) . . ? O13 W4 O19 75.7(3) . . ? O16 W4 O19 76.1(3) . . ? O9 W5 O16 104.2(3) . . ? O9 W5 O5 104.7(3) . . ? O16 W5 O5 87.3(3) . . ? O9 W5 O7 102.9(3) . . ? O16 W5 O7 152.8(3) . . ? O5 W5 O7 87.7(3) . . ? O9 W5 O11 102.8(3) . . ? O16 W5 O11 86.9(3) . . ? O5 W5 O11 152.5(3) . . ? O7 W5 O11 85.3(3) . . ? O9 W5 O19 178.2(3) . . ? O16 W5 O19 76.4(3) . . ? O5 W5 O19 77.0(3) . . ? O7 W5 O19 76.5(3) . . ? O11 W5 O19 75.5(3) . . ? O18 W6 O14 104.6(3) . . ? O18 W6 O17 102.7(3) . . ? O14 W6 O17 87.1(3) . . ? O18 W6 O4 102.5(3) . . ? O14 W6 O4 152.9(3) . . ? O17 W6 O4 85.9(3) . . ? O18 W6 O8 104.4(3) . . ? O14 W6 O8 87.5(3) . . ? O17 W6 O8 152.9(3) . . ? O4 W6 O8 86.9(3) . . ? O18 W6 O19 178.5(3) . . ? O14 W6 O19 76.5(3) . . ? O17 W6 O19 76.2(3) . . ? O4 W6 O19 76.4(3) . . ? O8 W6 O19 76.7(3) . . ? loop_ _geom_hbond_atom_site_label_D _geom_hbond_atom_site_label_H _geom_hbond_atom_site_label_A _geom_hbond_distance_DH _geom_hbond_distance_HA _geom_hbond_distance_DA _geom_hbond_angle_DHA _geom_hbond_site_symmetry_A C2 H2B O4 0.97 2.39 3.195(13) 139.9 2_665 C9 H9A O18 0.97 2.58 3.424(13) 145.8 2_665 C7 H7A O9 0.97 2.53 3.370(13) 144.3 . C4 H4A O10 0.97 2.62 3.502(12) 151.5 . C13 H13A O7 0.96 2.57 3.428(13) 149.4 . _diffrn_measured_fraction_theta_max 1.000 _diffrn_reflns_theta_full 25.00 _diffrn_measured_fraction_theta_full 1.000 _refine_diff_density_max 0.849 _refine_diff_density_min -0.948 _refine_diff_density_rms 0.193 #END******************************************* data_Cu-TDE-Mo6 _database_code_depnum_ccdc_archive 'CCDC 834665' #TrackingRef '- Structure(2).cif' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety 'C18 H35 Cu N5, Mo6 O19' _chemical_formula_sum 'C18 H35 Cu Mo6 N5 O19' _chemical_formula_weight 1264.69 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 'P 21 21 21' _symmetry_space_group_name_Hall 'P 2ac 2ab' loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x+1/2, -y, z+1/2' '-x, y+1/2, -z+1/2' 'x+1/2, -y+1/2, -z' _cell_length_a 10.9162(7) _cell_length_b 14.9446(10) _cell_length_c 20.5098(13) _cell_angle_alpha 90.00 _cell_angle_beta 90.00 _cell_angle_gamma 90.00 _cell_volume 3345.9(4) _cell_formula_units_Z 4 _cell_measurement_temperature 100(2) _cell_measurement_reflns_used 8520 _cell_measurement_theta_min 2.31 _cell_measurement_theta_max 24.96 _exptl_crystal_description Block _exptl_crystal_colour Red _exptl_crystal_size_max 0.24 _exptl_crystal_size_mid 0.20 _exptl_crystal_size_min 0.08 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 2.511 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 2444 _exptl_absorpt_coefficient_mu 2.884 _exptl_absorpt_correction_type Empirical _exptl_absorpt_correction_T_min 0.5444 _exptl_absorpt_correction_T_max 0.8021 _exptl_absorpt_process_details 'Bruker SADABS' _exptl_special_details ; ? ; _diffrn_ambient_temperature 100(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'CCD Area Detector' _diffrn_measurement_method 'Phi and Omega Scans' _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 31768 _diffrn_reflns_av_R_equivalents 0.0334 _diffrn_reflns_av_sigmaI/netI 0.0234 _diffrn_reflns_limit_h_min -12 _diffrn_reflns_limit_h_max 12 _diffrn_reflns_limit_k_min -17 _diffrn_reflns_limit_k_max 17 _diffrn_reflns_limit_l_min -24 _diffrn_reflns_limit_l_max 24 _diffrn_reflns_theta_min 1.69 _diffrn_reflns_theta_max 24.99 _reflns_number_total 5812 _reflns_number_gt 5680 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'Bruker SMART' _computing_cell_refinement 'Bruker SMART' _computing_data_reduction 'Bruker SAINT' _computing_structure_solution 'Bruker SHELXTL' _computing_structure_refinement 'Bruker SHELXTL' _computing_molecular_graphics 'Bruker SHELXTL' _computing_publication_material 'Bruker SHELXTL' _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^)+(0.0175P)^2^+0.8381P] 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 mixed _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 0.464(11) _refine_ls_number_reflns 5812 _refine_ls_number_parameters 458 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0172 _refine_ls_R_factor_gt 0.0165 _refine_ls_wR_factor_ref 0.0370 _refine_ls_wR_factor_gt 0.0368 _refine_ls_goodness_of_fit_ref 1.043 _refine_ls_restrained_S_all 1.043 _refine_ls_shift/su_max 0.004 _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 C1 C 0.3783(3) 0.1623(2) 0.65109(16) 0.0155(7) Uani 1 1 d . . . H1A H 0.3187 0.2119 0.6553 0.019 Uiso 1 1 calc R . . H1B H 0.4080 0.1610 0.6055 0.019 Uiso 1 1 calc R . . C2 C 0.4854(3) 0.1773(2) 0.69734(16) 0.0148(7) Uani 1 1 d . . . H2A H 0.5526 0.1349 0.6874 0.018 Uiso 1 1 calc R . . H2B H 0.5171 0.2391 0.6927 0.018 Uiso 1 1 calc R . . C3 C 0.4901(3) 0.2004(2) 0.81311(17) 0.0135(7) Uani 1 1 d . . . C4 C 0.4404(3) 0.1884(2) 0.88093(15) 0.0145(7) Uani 1 1 d . . . H4A H 0.4347 0.2485 0.9010 0.017 Uiso 1 1 calc R . . H4B H 0.5020 0.1543 0.9062 0.017 Uiso 1 1 calc R . . C5 C 0.3165(3) 0.1422(2) 0.89056(16) 0.0145(7) Uani 1 1 d . . . C6 C 0.2285(3) -0.0146(2) 0.87946(16) 0.0178(8) Uani 1 1 d . . . H6A H 0.1485 0.0166 0.8809 0.021 Uiso 1 1 calc R . . H6B H 0.2449 -0.0402 0.9231 0.021 Uiso 1 1 calc R . . C7 C 0.2248(3) -0.0886(2) 0.82887(16) 0.0164(7) Uani 1 1 d . . . H7A H 0.2989 -0.1264 0.8324 0.020 Uiso 1 1 calc R . . H7B H 0.1519 -0.1269 0.8358 0.020 Uiso 1 1 calc R . . C8 C 0.1539(3) -0.0777(2) 0.71787(16) 0.0179(8) Uani 1 1 d . . . C9 C 0.1532(3) -0.0335(2) 0.65135(16) 0.0196(8) Uani 1 1 d . . . H9A H 0.0695 -0.0404 0.6335 0.024 Uiso 1 1 calc R . . H9B H 0.2083 -0.0690 0.6230 0.024 Uiso 1 1 calc R . . C10 C 0.1890(3) 0.0650(2) 0.64279(16) 0.0166(8) Uani 1 1 d . . . C11 C 0.6037(3) 0.2578(2) 0.80805(17) 0.0176(7) Uani 1 1 d . . . H11A H 0.6606 0.2310 0.7767 0.026 Uiso 1 1 calc R . . H11B H 0.6432 0.2617 0.8509 0.026 Uiso 1 1 calc R . . H11C H 0.5809 0.3179 0.7933 0.026 Uiso 1 1 calc R . . C12 C 0.2116(3) 0.1924(2) 0.85784(17) 0.0176(8) Uani 1 1 d . . . H12A H 0.2249 0.1937 0.8106 0.026 Uiso 1 1 calc R . . H12B H 0.2084 0.2538 0.8746 0.026 Uiso 1 1 calc R . . H12C H 0.1340 0.1621 0.8673 0.026 Uiso 1 1 calc R . . C13 C 0.2920(3) 0.1367(3) 0.96451(16) 0.0181(8) Uani 1 1 d . . . H13A H 0.2081 0.1159 0.9720 0.027 Uiso 1 1 calc R . . H13B H 0.3026 0.1960 0.9840 0.027 Uiso 1 1 calc R . . H13C H 0.3498 0.0947 0.9845 0.027 Uiso 1 1 calc R . . C14 C 0.0765(3) -0.1602(2) 0.72356(18) 0.0241(8) Uani 1 1 d . . . H14A H 0.1232 -0.2072 0.7457 0.036 Uiso 1 1 calc R . . H14B H 0.0531 -0.1807 0.6799 0.036 Uiso 1 1 calc R . . H14C H 0.0026 -0.1465 0.7488 0.036 Uiso 1 1 calc R . . C15 C 0.1821(3) 0.0884(3) 0.57035(17) 0.0234(8) Uani 1 1 d . . . H15A H 0.2038 0.1515 0.5642 0.035 Uiso 1 1 calc R . . H15B H 0.0986 0.0781 0.5545 0.035 Uiso 1 1 calc R . . H15C H 0.2394 0.0507 0.5459 0.035 Uiso 1 1 calc R . . C16 C 0.1024(3) 0.1251(3) 0.68235(17) 0.0220(8) Uani 1 1 d . . . H16A H 0.1062 0.1082 0.7285 0.033 Uiso 1 1 calc R . . H16B H 0.0184 0.1177 0.6664 0.033 Uiso 1 1 calc R . . H16C H 0.1273 0.1877 0.6775 0.033 Uiso 1 1 calc R . . C17 C 0.6112(3) -0.0494(2) 0.73915(16) 0.0185(8) Uani 1 1 d . . . C18 C 0.7393(3) -0.0704(3) 0.72916(18) 0.0312(10) Uani 1 1 d . . . H18A H 0.7679 -0.1096 0.7643 0.047 Uiso 1 1 calc R . . H18B H 0.7873 -0.0150 0.7293 0.047 Uiso 1 1 calc R . . H18C H 0.7494 -0.1008 0.6872 0.047 Uiso 1 1 calc R . . Cu1 Cu 0.33395(4) 0.05565(3) 0.763653(19) 0.01248(9) Uani 1 1 d . . . H1 H 0.355(4) 0.044(3) 0.6529(18) 0.011(11) Uiso 1 1 d . . . H3 H 0.394(4) 0.031(3) 0.872(2) 0.038(13) Uiso 1 1 d . . . Mo1 Mo 0.62628(3) 0.908243(19) 0.928945(14) 0.01238(6) Uani 1 1 d . . . Mo2 Mo 0.91991(3) 0.868503(19) 0.942338(14) 0.01375(7) Uani 1 1 d . . . Mo3 Mo 0.94840(3) 1.042300(19) 1.037896(13) 0.01237(7) Uani 1 1 d . . . Mo4 Mo 0.65559(3) 1.08192(2) 1.024620(14) 0.01415(7) Uani 1 1 d . . . Mo5 Mo 0.82543(3) 1.066360(19) 0.893327(14) 0.01395(7) Uani 1 1 d . . . Mo6 Mo 0.74954(3) 0.88371(2) 1.073376(14) 0.01430(7) Uani 1 1 d . . . N1 N 0.3181(3) 0.0763(2) 0.66726(14) 0.0151(7) Uani 1 1 d . . . N2 N 0.4397(2) 0.16257(18) 0.76401(13) 0.0133(6) Uani 1 1 d . . . N3 N 0.3268(3) 0.04967(19) 0.86176(13) 0.0143(6) Uani 1 1 d . . . N4 N 0.2191(2) -0.04627(19) 0.76415(14) 0.0151(6) Uani 1 1 d . . . N5 N 0.5093(3) -0.0340(2) 0.74626(14) 0.0191(6) Uani 1 1 d . . . O1 O 0.5077(2) 0.86627(16) 0.88636(11) 0.0186(5) Uani 1 1 d . . . O2 O 0.7622(2) 0.83982(16) 0.90132(12) 0.0179(5) Uani 1 1 d . . . O3 O 0.5513(2) 1.01283(14) 0.96984(11) 0.0146(5) Uani 1 1 d . . . O4 O 0.6219(2) 0.85023(16) 1.00879(11) 0.0177(5) Uani 1 1 d . . . O5 O 0.6894(2) 1.00166(16) 0.86708(11) 0.0168(5) Uani 1 1 d . . . O6 O 1.0125(2) 0.79146(16) 0.90959(11) 0.0188(5) Uani 1 1 d . . . O7 O 0.9281(2) 0.96374(15) 0.87807(10) 0.0162(5) Uani 1 1 d . . . O8 O 0.8555(2) 0.81203(15) 1.01934(11) 0.0161(5) Uani 1 1 d . . . O9 O 0.8589(2) 1.13247(16) 0.82940(11) 0.0207(6) Uani 1 1 d . . . O10 O 1.0232(2) 0.93829(16) 0.99654(11) 0.0164(5) Uani 1 1 d . . . O11 O 0.9545(2) 1.10072(16) 0.95834(11) 0.0173(5) Uani 1 1 d . . . O12 O 1.0672(2) 1.08349(16) 1.08145(11) 0.0173(5) Uani 1 1 d . . . O13 O 0.8123(2) 1.11191(15) 1.06524(11) 0.0162(5) Uani 1 1 d . . . O14 O 0.8849(2) 0.95113(16) 1.09999(11) 0.0161(5) Uani 1 1 d . . . O15 O 0.5593(2) 1.15882(16) 1.05592(11) 0.0198(5) Uani 1 1 d . . . O16 O 0.7198(2) 1.13921(15) 0.94778(11) 0.0145(5) Uani 1 1 d . . . O17 O 0.6457(2) 0.98678(15) 1.08819(10) 0.0159(5) Uani 1 1 d . . . O18 O 0.7215(2) 0.81832(17) 1.13868(11) 0.0196(6) Uani 1 1 d . . . O19 O 0.7874(2) 0.97563(16) 0.98328(11) 0.0133(5) 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 C1 0.0185(18) 0.0119(18) 0.0161(18) 0.0040(14) 0.0005(15) -0.0011(15) C2 0.0158(18) 0.0145(18) 0.0141(17) 0.0000(14) 0.0037(14) -0.0009(14) C3 0.0124(17) 0.0065(16) 0.0216(18) 0.0020(14) 0.0012(14) 0.0036(13) C4 0.0143(17) 0.0121(16) 0.0170(17) -0.0009(13) -0.0021(14) 0.0001(14) C5 0.0136(17) 0.0121(17) 0.0180(17) -0.0005(14) 0.0016(14) 0.0001(14) C6 0.0155(18) 0.022(2) 0.0163(18) 0.0038(15) 0.0011(15) -0.0068(15) C7 0.0151(18) 0.0162(18) 0.0181(17) 0.0038(15) -0.0003(14) -0.0033(15) C8 0.0092(17) 0.023(2) 0.0218(19) -0.0032(15) 0.0010(14) 0.0042(15) C9 0.0149(19) 0.024(2) 0.0205(18) -0.0061(16) -0.0024(15) -0.0013(16) C10 0.0138(18) 0.022(2) 0.0136(17) -0.0039(14) -0.0061(14) 0.0035(15) C11 0.0178(18) 0.0168(18) 0.0181(18) 0.0010(14) -0.0018(15) -0.0006(15) C12 0.0146(17) 0.0182(19) 0.0200(18) 0.0001(15) 0.0003(15) 0.0004(14) C13 0.0153(17) 0.026(2) 0.0129(17) -0.0018(15) 0.0051(14) -0.0010(15) C14 0.0197(19) 0.021(2) 0.032(2) -0.0019(16) -0.0022(17) -0.0048(16) C15 0.0233(19) 0.027(2) 0.0204(19) -0.0012(17) -0.0071(16) -0.0003(17) C16 0.0185(19) 0.026(2) 0.0211(19) 0.0012(16) -0.0049(15) 0.0056(16) C17 0.021(2) 0.0212(19) 0.0137(17) 0.0028(15) -0.0034(15) 0.0024(15) C18 0.025(2) 0.049(3) 0.019(2) 0.0002(19) 0.0020(17) 0.0096(19) Cu1 0.0125(2) 0.0133(2) 0.01163(19) 0.00003(16) -0.00012(16) -0.00123(17) Mo1 0.01155(13) 0.01334(14) 0.01225(14) -0.00113(12) -0.00208(12) -0.00056(11) Mo2 0.01259(14) 0.01329(15) 0.01536(15) -0.00069(12) 0.00018(11) 0.00170(12) Mo3 0.01016(14) 0.01391(15) 0.01303(14) -0.00017(11) -0.00158(12) -0.00201(12) Mo4 0.01217(14) 0.01512(15) 0.01516(15) -0.00357(12) -0.00044(12) 0.00153(12) Mo5 0.01455(15) 0.01429(16) 0.01300(14) 0.00322(11) -0.00050(12) -0.00080(12) Mo6 0.01318(14) 0.01746(16) 0.01226(14) 0.00333(12) -0.00078(12) -0.00292(12) N1 0.0143(16) 0.0157(17) 0.0153(15) 0.0004(13) 0.0009(12) 0.0032(14) N2 0.0105(14) 0.0132(14) 0.0162(14) 0.0019(12) 0.0028(12) 0.0020(11) N3 0.0100(15) 0.0187(16) 0.0142(14) 0.0009(12) 0.0003(12) 0.0014(13) N4 0.0139(14) 0.0104(15) 0.0209(15) -0.0005(12) 0.0004(12) 0.0014(11) N5 0.0224(17) 0.0191(16) 0.0158(15) 0.0035(13) -0.0028(12) -0.0002(13) O1 0.0149(12) 0.0225(13) 0.0183(13) -0.0021(11) -0.0038(10) -0.0012(10) O2 0.0143(12) 0.0186(13) 0.0208(13) -0.0069(10) -0.0035(10) 0.0004(10) O3 0.0123(11) 0.0132(11) 0.0183(12) -0.0001(10) 0.0014(10) 0.0008(10) O4 0.0162(12) 0.0196(13) 0.0172(12) 0.0020(10) -0.0022(10) -0.0041(10) O5 0.0176(12) 0.0199(13) 0.0129(12) 0.0010(10) -0.0036(10) -0.0033(11) O6 0.0165(13) 0.0188(13) 0.0212(13) -0.0025(10) -0.0004(10) 0.0027(10) O7 0.0157(12) 0.0196(13) 0.0132(11) -0.0007(10) 0.0023(10) 0.0014(11) O8 0.0159(12) 0.0158(12) 0.0165(12) 0.0030(10) -0.0012(10) 0.0021(10) O9 0.0216(13) 0.0210(13) 0.0194(13) 0.0056(11) 0.0024(11) 0.0016(11) O10 0.0146(12) 0.0179(13) 0.0167(12) -0.0018(10) -0.0020(10) 0.0003(10) O11 0.0177(12) 0.0178(12) 0.0165(12) 0.0031(10) -0.0012(10) -0.0049(11) O12 0.0157(12) 0.0181(12) 0.0180(12) -0.0009(10) -0.0008(10) -0.0022(11) O13 0.0133(12) 0.0161(12) 0.0191(12) -0.0058(10) -0.0013(10) 0.0005(10) O14 0.0161(12) 0.0197(13) 0.0126(11) 0.0005(10) -0.0020(10) -0.0017(10) O15 0.0187(13) 0.0172(12) 0.0236(13) -0.0056(10) 0.0021(11) -0.0006(11) O16 0.0154(12) 0.0116(12) 0.0166(12) 0.0005(10) -0.0005(10) 0.0005(10) O17 0.0128(12) 0.0201(13) 0.0149(12) -0.0003(10) 0.0024(10) 0.0002(10) O18 0.0174(13) 0.0237(14) 0.0178(13) 0.0050(11) -0.0006(10) -0.0046(11) O19 0.0124(11) 0.0138(12) 0.0139(11) -0.0020(9) -0.0020(9) -0.0001(9) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag C1 N1 1.481(4) . ? C1 C2 1.522(5) . ? C1 H1A 0.9900 . ? C1 H1B 0.9900 . ? C2 N2 1.472(4) . ? C2 H2A 0.9900 . ? C2 H2B 0.9900 . ? C3 N2 1.279(4) . ? C3 C4 1.504(5) . ? C3 C11 1.512(4) . ? C4 C5 1.532(5) . ? C4 H4A 0.9900 . ? C4 H4B 0.9900 . ? C5 N3 1.507(4) . ? C5 C12 1.525(5) . ? C5 C13 1.542(4) . ? C6 N3 1.485(4) . ? C6 C7 1.518(5) . ? C6 H6A 0.9900 . ? C6 H6B 0.9900 . ? C7 N4 1.472(4) . ? C7 H7A 0.9900 . ? C7 H7B 0.9900 . ? C8 N4 1.276(4) . ? C8 C14 1.499(5) . ? C8 C9 1.516(5) . ? C9 C10 1.534(5) . ? C9 H9A 0.9900 . ? C9 H9B 0.9900 . ? C10 N1 1.505(4) . ? C10 C15 1.528(5) . ? C10 C16 1.536(5) . ? C11 H11A 0.9800 . ? C11 H11B 0.9800 . ? C11 H11C 0.9800 . ? C12 H12A 0.9800 . ? C12 H12B 0.9800 . ? C12 H12C 0.9800 . ? C13 H13A 0.9800 . ? C13 H13B 0.9800 . ? C13 H13C 0.9800 . ? C14 H14A 0.9800 . ? C14 H14B 0.9800 . ? C14 H14C 0.9800 . ? C15 H15A 0.9800 . ? C15 H15B 0.9800 . ? C15 H15C 0.9800 . ? C16 H16A 0.9800 . ? C16 H16B 0.9800 . ? C16 H16C 0.9800 . ? C17 N5 1.145(4) . ? C17 C18 1.447(5) . ? C18 H18A 0.9800 . ? C18 H18B 0.9800 . ? C18 H18C 0.9800 . ? Cu1 N2 1.971(3) . ? Cu1 N4 1.973(3) . ? Cu1 N1 2.008(3) . ? Cu1 N3 2.016(3) . ? Cu1 N5 2.364(3) . ? Mo1 O1 1.683(2) . ? Mo1 O4 1.854(2) . ? Mo1 O2 1.889(2) . ? Mo1 O3 1.954(2) . ? Mo1 O5 2.008(2) . ? Mo1 O19 2.313(2) . ? Mo2 O6 1.673(2) . ? Mo2 O10 1.896(2) . ? Mo2 O8 1.924(2) . ? Mo2 O7 1.942(2) . ? Mo2 O2 1.964(2) . ? Mo2 O19 2.315(2) . ? Mo3 O12 1.690(2) . ? Mo3 O11 1.852(2) . ? Mo3 O13 1.898(2) . ? Mo3 O10 1.950(2) . ? Mo3 O14 1.990(2) . ? Mo3 O19 2.310(2) . ? Mo4 O15 1.685(2) . ? Mo4 O3 1.904(2) . ? Mo4 O16 1.926(2) . ? Mo4 O17 1.932(2) . ? Mo4 O13 1.955(2) . ? Mo4 O19 2.305(2) . ? Mo5 O9 1.682(2) . ? Mo5 O5 1.852(2) . ? Mo5 O7 1.925(2) . ? Mo5 O16 1.939(2) . ? Mo5 O11 2.007(2) . ? Mo5 O19 2.327(2) . ? Mo6 O18 1.686(2) . ? Mo6 O14 1.870(2) . ? Mo6 O8 1.927(2) . ? Mo6 O17 1.936(2) . ? Mo6 O4 1.986(2) . ? Mo6 O19 2.339(2) . ? N1 H1 0.70(4) . ? N3 H3 0.81(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 N1 C1 C2 109.2(3) . . ? N1 C1 H1A 109.8 . . ? C2 C1 H1A 109.8 . . ? N1 C1 H1B 109.8 . . ? C2 C1 H1B 109.8 . . ? H1A C1 H1B 108.3 . . ? N2 C2 C1 107.2(3) . . ? N2 C2 H2A 110.3 . . ? C1 C2 H2A 110.3 . . ? N2 C2 H2B 110.3 . . ? C1 C2 H2B 110.3 . . ? H2A C2 H2B 108.5 . . ? N2 C3 C4 121.4(3) . . ? N2 C3 C11 123.3(3) . . ? C4 C3 C11 115.3(3) . . ? C3 C4 C5 119.4(3) . . ? C3 C4 H4A 107.5 . . ? C5 C4 H4A 107.5 . . ? C3 C4 H4B 107.5 . . ? C5 C4 H4B 107.5 . . ? H4A C4 H4B 107.0 . . ? N3 C5 C12 109.6(3) . . ? N3 C5 C4 107.3(3) . . ? C12 C5 C4 112.6(3) . . ? N3 C5 C13 110.5(3) . . ? C12 C5 C13 109.2(3) . . ? C4 C5 C13 107.7(3) . . ? N3 C6 C7 108.9(3) . . ? N3 C6 H6A 109.9 . . ? C7 C6 H6A 109.9 . . ? N3 C6 H6B 109.9 . . ? C7 C6 H6B 109.9 . . ? H6A C6 H6B 108.3 . . ? N4 C7 C6 107.7(3) . . ? N4 C7 H7A 110.2 . . ? C6 C7 H7A 110.2 . . ? N4 C7 H7B 110.2 . . ? C6 C7 H7B 110.2 . . ? H7A C7 H7B 108.5 . . ? N4 C8 C14 124.0(3) . . ? N4 C8 C9 120.8(3) . . ? C14 C8 C9 115.2(3) . . ? C8 C9 C10 121.3(3) . . ? C8 C9 H9A 107.0 . . ? C10 C9 H9A 107.0 . . ? C8 C9 H9B 107.0 . . ? C10 C9 H9B 107.0 . . ? H9A C9 H9B 106.7 . . ? N1 C10 C15 110.2(3) . . ? N1 C10 C9 107.9(3) . . ? C15 C10 C9 108.6(3) . . ? N1 C10 C16 109.6(3) . . ? C15 C10 C16 110.4(3) . . ? C9 C10 C16 110.1(3) . . ? C3 C11 H11A 109.5 . . ? C3 C11 H11B 109.5 . . ? H11A C11 H11B 109.5 . . ? C3 C11 H11C 109.5 . . ? H11A C11 H11C 109.5 . . ? H11B C11 H11C 109.5 . . ? C5 C12 H12A 109.5 . . ? C5 C12 H12B 109.5 . . ? H12A C12 H12B 109.5 . . ? C5 C12 H12C 109.5 . . ? H12A C12 H12C 109.5 . . ? H12B C12 H12C 109.5 . . ? C5 C13 H13A 109.5 . . ? C5 C13 H13B 109.5 . . ? H13A C13 H13B 109.5 . . ? C5 C13 H13C 109.5 . . ? H13A C13 H13C 109.5 . . ? H13B C13 H13C 109.5 . . ? C8 C14 H14A 109.5 . . ? C8 C14 H14B 109.5 . . ? H14A C14 H14B 109.5 . . ? C8 C14 H14C 109.5 . . ? H14A C14 H14C 109.5 . . ? H14B C14 H14C 109.5 . . ? C10 C15 H15A 109.5 . . ? C10 C15 H15B 109.5 . . ? H15A C15 H15B 109.5 . . ? C10 C15 H15C 109.5 . . ? H15A C15 H15C 109.5 . . ? H15B C15 H15C 109.5 . . ? C10 C16 H16A 109.5 . . ? C10 C16 H16B 109.5 . . ? H16A C16 H16B 109.5 . . ? C10 C16 H16C 109.5 . . ? H16A C16 H16C 109.5 . . ? H16B C16 H16C 109.5 . . ? N5 C17 C18 178.8(4) . . ? C17 C18 H18A 109.5 . . ? C17 C18 H18B 109.5 . . ? H18A C18 H18B 109.5 . . ? C17 C18 H18C 109.5 . . ? H18A C18 H18C 109.5 . . ? H18B C18 H18C 109.5 . . ? N2 Cu1 N4 176.35(11) . . ? N2 Cu1 N1 85.97(12) . . ? N4 Cu1 N1 93.95(12) . . ? N2 Cu1 N3 93.15(12) . . ? N4 Cu1 N3 86.33(12) . . ? N1 Cu1 N3 170.45(13) . . ? N2 Cu1 N5 89.20(11) . . ? N4 Cu1 N5 94.45(11) . . ? N1 Cu1 N5 90.47(12) . . ? N3 Cu1 N5 99.03(11) . . ? O1 Mo1 O4 105.34(11) . . ? O1 Mo1 O2 104.27(10) . . ? O4 Mo1 O2 91.83(11) . . ? O1 Mo1 O3 101.47(10) . . ? O4 Mo1 O3 89.10(10) . . ? O2 Mo1 O3 153.01(10) . . ? O1 Mo1 O5 101.24(10) . . ? O4 Mo1 O5 153.14(10) . . ? O2 Mo1 O5 85.27(10) . . ? O3 Mo1 O5 81.88(9) . . ? O1 Mo1 O19 175.79(11) . . ? O4 Mo1 O19 78.31(9) . . ? O2 Mo1 O19 77.47(9) . . ? O3 Mo1 O19 76.32(9) . . ? O5 Mo1 O19 74.99(9) . . ? O6 Mo2 O10 104.76(11) . . ? O6 Mo2 O8 104.39(11) . . ? O10 Mo2 O8 88.70(10) . . ? O6 Mo2 O7 101.78(11) . . ? O10 Mo2 O7 88.14(10) . . ? O8 Mo2 O7 153.58(10) . . ? O6 Mo2 O2 101.97(11) . . ? O10 Mo2 O2 153.22(10) . . ? O8 Mo2 O2 86.30(10) . . ? O7 Mo2 O2 84.80(10) . . ? O6 Mo2 O19 177.47(10) . . ? O10 Mo2 O19 77.21(9) . . ? O8 Mo2 O19 77.13(9) . . ? O7 Mo2 O19 76.59(9) . . ? O2 Mo2 O19 76.03(9) . . ? O12 Mo3 O11 105.45(11) . . ? O12 Mo3 O13 104.15(10) . . ? O11 Mo3 O13 91.73(10) . . ? O12 Mo3 O10 101.47(10) . . ? O11 Mo3 O10 88.71(10) . . ? O13 Mo3 O10 153.27(10) . . ? O12 Mo3 O14 100.26(10) . . ? O11 Mo3 O14 154.08(10) . . ? O13 Mo3 O14 85.04(10) . . ? O10 Mo3 O14 83.02(10) . . ? O12 Mo3 O19 175.40(10) . . ? O11 Mo3 O19 78.66(10) . . ? O13 Mo3 O19 77.54(9) . . ? O10 Mo3 O19 76.35(9) . . ? O14 Mo3 O19 75.53(9) . . ? O15 Mo4 O3 102.80(11) . . ? O15 Mo4 O16 103.64(11) . . ? O3 Mo4 O16 88.62(9) . . ? O15 Mo4 O17 102.13(11) . . ? O3 Mo4 O17 88.04(9) . . ? O16 Mo4 O17 154.12(9) . . ? O15 Mo4 O13 103.14(11) . . ? O3 Mo4 O13 154.05(9) . . ? O16 Mo4 O13 85.88(10) . . ? O17 Mo4 O13 85.98(10) . . ? O15 Mo4 O19 179.15(10) . . ? O3 Mo4 O19 77.44(9) . . ? O16 Mo4 O19 77.17(9) . . ? O17 Mo4 O19 77.05(9) . . ? O13 Mo4 O19 76.61(9) . . ? O9 Mo5 O5 104.74(11) . . ? O9 Mo5 O7 102.40(11) . . ? O5 Mo5 O7 90.21(10) . . ? O9 Mo5 O16 104.38(11) . . ? O5 Mo5 O16 89.08(10) . . ? O7 Mo5 O16 152.48(9) . . ? O9 Mo5 O11 102.41(11) . . ? O5 Mo5 O11 152.84(10) . . ? O7 Mo5 O11 84.44(10) . . ? O16 Mo5 O11 83.74(9) . . ? O9 Mo5 O19 177.62(10) . . ? O5 Mo5 O19 77.48(9) . . ? O7 Mo5 O19 76.61(9) . . ? O16 Mo5 O19 76.38(9) . . ? O11 Mo5 O19 75.38(9) . . ? O18 Mo6 O14 102.95(11) . . ? O18 Mo6 O8 104.11(11) . . ? O14 Mo6 O8 89.60(10) . . ? O18 Mo6 O17 103.30(11) . . ? O14 Mo6 O17 89.32(10) . . ? O8 Mo6 O17 152.09(9) . . ? O18 Mo6 O4 104.85(11) . . ? O14 Mo6 O4 152.20(10) . . ? O8 Mo6 O4 84.11(10) . . ? O17 Mo6 O4 83.96(10) . . ? O18 Mo6 O19 179.42(11) . . ? O14 Mo6 O19 76.97(9) . . ? O8 Mo6 O19 76.47(9) . . ? O17 Mo6 O19 76.13(9) . . ? O4 Mo6 O19 75.23(9) . . ? C1 N1 C10 115.9(3) . . ? C1 N1 Cu1 108.4(2) . . ? C10 N1 Cu1 113.1(2) . . ? C1 N1 H1 104(3) . . ? C10 N1 H1 109(3) . . ? Cu1 N1 H1 105(3) . . ? C3 N2 C2 121.3(3) . . ? C3 N2 Cu1 127.8(2) . . ? C2 N2 Cu1 108.4(2) . . ? C6 N3 C5 116.3(3) . . ? C6 N3 Cu1 107.5(2) . . ? C5 N3 Cu1 110.7(2) . . ? C6 N3 H3 111(3) . . ? C5 N3 H3 106(3) . . ? Cu1 N3 H3 104(3) . . ? C8 N4 C7 122.4(3) . . ? C8 N4 Cu1 129.4(2) . . ? C7 N4 Cu1 108.1(2) . . ? C17 N5 Cu1 156.9(3) . . ? Mo1 O2 Mo2 116.23(11) . . ? Mo4 O3 Mo1 115.89(11) . . ? Mo1 O4 Mo6 116.97(12) . . ? Mo5 O5 Mo1 117.01(11) . . ? Mo5 O7 Mo2 116.54(11) . . ? Mo2 O8 Mo6 116.59(11) . . ? Mo2 O10 Mo3 116.37(11) . . ? Mo3 O11 Mo5 116.07(11) . . ? Mo3 O13 Mo4 115.68(11) . . ? Mo6 O14 Mo3 117.22(11) . . ? Mo4 O16 Mo5 115.98(11) . . ? Mo4 O17 Mo6 116.55(11) . . ? Mo4 O19 Mo3 89.96(8) . . ? Mo4 O19 Mo1 90.14(8) . . ? Mo3 O19 Mo1 179.70(13) . . ? Mo4 O19 Mo2 179.67(12) . . ? Mo3 O19 Mo2 89.94(8) . . ? Mo1 O19 Mo2 89.96(8) . . ? Mo4 O19 Mo5 90.08(8) . . ? Mo3 O19 Mo5 89.86(8) . . ? Mo1 O19 Mo5 90.42(8) . . ? Mo2 O19 Mo5 90.23(8) . . ? Mo4 O19 Mo6 90.21(8) . . ? Mo3 O19 Mo6 90.27(8) . . ? Mo1 O19 Mo6 89.46(8) . . ? Mo2 O19 Mo6 89.48(8) . . ? Mo5 O19 Mo6 179.68(12) . . ? _diffrn_measured_fraction_theta_max 0.991 _diffrn_reflns_theta_full 24.99 _diffrn_measured_fraction_theta_full 0.991 _refine_diff_density_max 0.333 _refine_diff_density_min -0.418 _refine_diff_density_rms 0.077 #END============================================= #END******************************************************* data_Cu-TDE-W6(1M) _database_code_depnum_ccdc_archive 'CCDC 849786' #TrackingRef '- Structure(2).cif' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety 'C18 H35 Cu N5, O19 W6' _chemical_formula_sum 'C18 H35 Cu N5 O19 W6' _chemical_formula_weight 1792.15 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' W W -0.8490 6.8722 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting orthorhombic _symmetry_space_group_name_H-M 'P 21 21 21' loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x+1/2, -y, z+1/2' '-x, y+1/2, -z+1/2' 'x+1/2, -y+1/2, -z' _cell_length_a 11.0347(10) _cell_length_b 15.0878(13) _cell_length_c 20.7320(18) _cell_angle_alpha 90.00 _cell_angle_beta 90.00 _cell_angle_gamma 90.00 _cell_volume 3451.7(5) _cell_formula_units_Z 4 _cell_measurement_temperature 293(2) _cell_measurement_reflns_used 6643 _cell_measurement_theta_min 2.29 _cell_measurement_theta_max 24.94 _exptl_crystal_description block _exptl_crystal_colour red _exptl_crystal_size_max 0.22 _exptl_crystal_size_mid 0.20 _exptl_crystal_size_min 0.12 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 3.449 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 3212 _exptl_absorpt_coefficient_mu 20.596 _exptl_absorpt_correction_type empirical _exptl_absorpt_correction_T_min 0.0928 _exptl_absorpt_correction_T_max 0.1913 _exptl_absorpt_process_details Bruker-SADABS _exptl_special_details ; ? ; _diffrn_ambient_temperature 293(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'CCD area detector' _diffrn_measurement_method 'phi and omega scans' _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 33303 _diffrn_reflns_av_R_equivalents 0.0523 _diffrn_reflns_av_sigmaI/netI 0.0371 _diffrn_reflns_limit_h_min -13 _diffrn_reflns_limit_h_max 13 _diffrn_reflns_limit_k_min -17 _diffrn_reflns_limit_k_max 17 _diffrn_reflns_limit_l_min -24 _diffrn_reflns_limit_l_max 24 _diffrn_reflns_theta_min 1.67 _diffrn_reflns_theta_max 25.00 _reflns_number_total 6070 _reflns_number_gt 5893 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'Bruker SMART' _computing_cell_refinement 'Bruker SMART' _computing_data_reduction 'Bruker SAINT' _computing_structure_solution 'Bruker SHELXTL' _computing_structure_refinement 'Bruker SHELXTL' _computing_molecular_graphics 'Bruker SHELXTL' _computing_publication_material 'Bruker SHELXTL' _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^)+(0.0250P)^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_abs_structure_details 'Flack H D (1983), Acta Cryst. A39, 876-881' _refine_ls_abs_structure_Flack -0.016(12) _refine_ls_number_reflns 6070 _refine_ls_number_parameters 449 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0250 _refine_ls_R_factor_gt 0.0238 _refine_ls_wR_factor_ref 0.0564 _refine_ls_wR_factor_gt 0.0559 _refine_ls_goodness_of_fit_ref 1.076 _refine_ls_restrained_S_all 1.076 _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 C1 C 0.1295(10) 0.8369(6) 0.6535(5) 0.037(2) Uani 1 1 d . . . H1A H 0.1893 0.7904 0.6591 0.044 Uiso 1 1 calc R . . H1B H 0.1019 0.8356 0.6090 0.044 Uiso 1 1 calc R . . C2 C 0.0236(9) 0.8211(6) 0.6983(4) 0.030(2) Uani 1 1 d . . . H2A H -0.0427 0.8605 0.6875 0.037 Uiso 1 1 calc R . . H2B H -0.0046 0.7604 0.6943 0.037 Uiso 1 1 calc R . . C3 C 0.0147(8) 0.8012(6) 0.8120(5) 0.028(2) Uani 1 1 d . . . C4 C 0.0620(8) 0.8154(6) 0.8785(4) 0.029(2) Uani 1 1 d . . . H4A H 0.0670 0.7576 0.8988 0.035 Uiso 1 1 calc R . . H4B H 0.0006 0.8485 0.9018 0.035 Uiso 1 1 calc R . . C5 C 0.1823(8) 0.8617(6) 0.8909(5) 0.032(2) Uani 1 1 d . . . C6 C 0.2694(9) 1.0157(7) 0.8775(5) 0.036(2) Uani 1 1 d . . . H6A H 0.3472 0.9858 0.8780 0.043 Uiso 1 1 calc R . . H6B H 0.2547 1.0400 0.9201 0.043 Uiso 1 1 calc R . . C7 C 0.2713(9) 1.0893(6) 0.8285(5) 0.035(2) Uani 1 1 d . . . H7A H 0.1978 1.1243 0.8315 0.042 Uiso 1 1 calc R . . H7B H 0.3402 1.1279 0.8358 0.042 Uiso 1 1 calc R . . C8 C 0.3434(8) 1.0757(7) 0.7183(5) 0.037(2) Uani 1 1 d . . . C9 C 0.3461(10) 1.0343(7) 0.6524(5) 0.042(3) Uani 1 1 d . . . H9A H 0.4274 1.0417 0.6354 0.050 Uiso 1 1 calc R . . H9B H 0.2923 1.0683 0.6249 0.050 Uiso 1 1 calc R . . C10 C 0.3121(9) 0.9361(7) 0.6449(5) 0.038(2) Uani 1 1 d . . . C11 C -0.0943(8) 0.7436(6) 0.8076(5) 0.040(3) Uani 1 1 d . . . H11A H -0.0880 0.7063 0.7702 0.059 Uiso 1 1 calc R . . H11B H -0.1655 0.7799 0.8041 0.059 Uiso 1 1 calc R . . H11C H -0.0999 0.7074 0.8456 0.059 Uiso 1 1 calc R . . C12 C 0.2879(8) 0.8094(7) 0.8593(5) 0.036(2) Uani 1 1 d . . . H12A H 0.2755 0.8064 0.8135 0.055 Uiso 1 1 calc R . . H12B H 0.2904 0.7505 0.8767 0.055 Uiso 1 1 calc R . . H12C H 0.3632 0.8389 0.8681 0.055 Uiso 1 1 calc R . . C13 C 0.2030(9) 0.8677(8) 0.9630(4) 0.040(3) Uani 1 1 d . . . H13A H 0.2831 0.8899 0.9712 0.060 Uiso 1 1 calc R . . H13B H 0.1945 0.8100 0.9819 0.060 Uiso 1 1 calc R . . H13C H 0.1445 0.9072 0.9817 0.060 Uiso 1 1 calc R . . C14 C 0.4183(9) 1.1604(7) 0.7236(6) 0.057(3) Uani 1 1 d . . . H14A H 0.3657 1.2095 0.7326 0.085 Uiso 1 1 calc R . . H14B H 0.4601 1.1707 0.6837 0.085 Uiso 1 1 calc R . . H14C H 0.4762 1.1542 0.7579 0.085 Uiso 1 1 calc R . . C15 C 0.3205(10) 0.9146(8) 0.5736(5) 0.049(3) Uani 1 1 d . . . H15A H 0.3179 0.8515 0.5677 0.073 Uiso 1 1 calc R . . H15B H 0.3952 0.9373 0.5566 0.073 Uiso 1 1 calc R . . H15C H 0.2536 0.9414 0.5513 0.073 Uiso 1 1 calc R . . C16 C 0.3987(9) 0.8782(8) 0.6829(5) 0.049(3) Uani 1 1 d . . . H16A H 0.4018 0.8983 0.7268 0.073 Uiso 1 1 calc R . . H16B H 0.4781 0.8818 0.6642 0.073 Uiso 1 1 calc R . . H16C H 0.3711 0.8179 0.6818 0.073 Uiso 1 1 calc R . . C17 C -0.2358(9) 1.0719(11) 0.7301(5) 0.066(4) Uani 1 1 d . . . H17A H -0.2514 1.0807 0.6850 0.099 Uiso 1 1 calc R . . H17B H -0.2532 1.1256 0.7532 0.099 Uiso 1 1 calc R . . H17C H -0.2865 1.0251 0.7461 0.099 Uiso 1 1 calc R . . C18 C -0.1105(9) 1.0486(7) 0.7392(5) 0.038(2) Uani 1 1 d . . . Cu1 Cu 0.16876(10) 0.94431(7) 0.76358(5) 0.0246(2) Uani 1 1 d . . . N1 N 0.1847(7) 0.9241(5) 0.6679(3) 0.0278(17) Uani 1 1 d . . . N2 N 0.0645(7) 0.8378(5) 0.7639(4) 0.0283(18) Uani 1 1 d . . . N3 N 0.1721(7) 0.9517(5) 0.8605(3) 0.0254(17) Uani 1 1 d . . . N4 N 0.2802(6) 1.0465(5) 0.7642(4) 0.0299(18) Uani 1 1 d . . . N5 N -0.0106(8) 1.0321(6) 0.7466(4) 0.042(2) Uani 1 1 d . . . O1 O 0.9358(6) -0.1551(4) 1.0608(4) 0.0456(19) Uani 1 1 d . . . O2 O 0.8457(5) 0.0150(4) 1.0892(3) 0.0330(16) Uani 1 1 d . . . O3 O 0.7820(6) -0.1349(4) 0.9503(3) 0.0336(15) Uani 1 1 d . . . O4 O 0.9447(5) -0.0106(4) 0.9744(3) 0.0303(15) Uani 1 1 d . . . O5 O 0.6843(5) -0.1101(4) 1.0650(3) 0.0301(15) Uani 1 1 d . . . O6 O 0.7729(6) 0.1862(5) 1.1366(4) 0.051(2) Uani 1 1 d . . . O7 O 0.6106(5) 0.0497(4) 1.0985(3) 0.0323(15) Uani 1 1 d . . . O8 O 0.8712(6) 0.1505(4) 1.0093(3) 0.0328(15) Uani 1 1 d . . . O9 O 0.4297(6) -0.0795(4) 1.0824(3) 0.0386(17) Uani 1 1 d . . . O10 O 0.6377(6) 0.1857(4) 1.0185(3) 0.0329(16) Uani 1 1 d . . . O11 O 0.4762(5) 0.0601(4) 0.9944(3) 0.0308(15) Uani 1 1 d . . . O12 O 0.4887(6) 0.2078(5) 0.9080(4) 0.048(2) Uani 1 1 d . . . O13 O 0.5760(6) 0.0353(4) 0.8795(3) 0.0287(14) Uani 1 1 d . . . O14 O 0.7368(5) 0.1595(4) 0.9042(3) 0.0325(15) Uani 1 1 d . . . O15 O 0.6449(7) -0.1350(5) 0.8339(4) 0.051(2) Uani 1 1 d . . . O16 O 0.5495(6) -0.0992(4) 0.9595(3) 0.0308(15) Uani 1 1 d . . . O17 O 0.8100(6) -0.0010(4) 0.8700(3) 0.0323(15) Uani 1 1 d . . . O18 O 0.9909(6) 0.1305(5) 0.8876(3) 0.0390(17) Uani 1 1 d . . . O19 O 0.7106(5) 0.0250(4) 0.9844(3) 0.0228(12) Uani 1 1 d . . . W1 W 0.83958(3) -0.07993(3) 1.028282(19) 0.02860(10) Uani 1 1 d . . . W2 W 0.74889(3) 0.11965(3) 1.071402(19) 0.02919(10) Uani 1 1 d . . . W3 W 0.58118(3) 0.13078(2) 0.940770(19) 0.02785(10) Uani 1 1 d . . . W4 W 0.67208(3) -0.06844(3) 0.897620(19) 0.02819(10) Uani 1 1 d . . . W5 W 0.54900(3) -0.03722(2) 1.039677(18) 0.02608(9) Uani 1 1 d . . . W6 W 0.87221(3) 0.08806(2) 0.929272(18) 0.02506(9) 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 C1 0.060(7) 0.026(5) 0.024(5) -0.005(4) -0.003(5) 0.007(5) C2 0.043(6) 0.027(5) 0.022(5) 0.001(4) 0.000(4) -0.008(4) C3 0.033(5) 0.017(4) 0.033(5) 0.005(4) -0.004(4) 0.009(4) C4 0.040(5) 0.027(5) 0.021(5) 0.004(4) -0.005(4) 0.000(4) C5 0.035(5) 0.036(5) 0.024(5) 0.010(4) -0.006(4) -0.004(5) C6 0.040(6) 0.040(6) 0.027(5) -0.007(5) -0.012(4) -0.014(5) C7 0.031(5) 0.029(5) 0.046(6) -0.003(5) -0.002(5) -0.008(4) C8 0.021(5) 0.035(6) 0.054(7) 0.002(5) -0.004(5) -0.002(4) C9 0.042(6) 0.049(7) 0.034(6) 0.018(5) 0.008(5) -0.014(5) C10 0.046(6) 0.041(6) 0.026(5) 0.001(4) 0.015(5) 0.009(5) C11 0.037(6) 0.037(6) 0.045(7) 0.000(5) 0.002(5) -0.011(5) C12 0.036(5) 0.036(6) 0.037(6) -0.007(5) -0.009(5) 0.009(5) C13 0.040(6) 0.056(7) 0.025(5) 0.004(5) -0.006(5) 0.002(5) C14 0.041(6) 0.047(7) 0.082(10) 0.017(7) 0.004(6) -0.013(5) C15 0.048(6) 0.067(8) 0.030(6) -0.012(6) 0.016(5) 0.005(6) C16 0.043(6) 0.062(7) 0.041(7) -0.002(6) 0.013(5) 0.015(6) C17 0.051(7) 0.114(11) 0.033(7) -0.009(7) -0.001(6) 0.034(7) C18 0.047(7) 0.045(6) 0.021(5) 0.005(5) 0.009(5) 0.009(5) Cu1 0.0286(6) 0.0225(6) 0.0227(6) -0.0011(4) 0.0005(5) -0.0024(5) N1 0.033(4) 0.031(4) 0.019(4) -0.002(3) 0.003(3) -0.002(4) N2 0.035(4) 0.026(4) 0.024(4) 0.007(3) -0.009(4) -0.006(3) N3 0.028(4) 0.029(4) 0.019(4) 0.000(3) -0.003(3) -0.003(3) N4 0.029(4) 0.023(4) 0.037(5) 0.000(4) 0.001(4) -0.004(3) N5 0.044(5) 0.046(5) 0.037(5) -0.002(4) 0.007(4) 0.002(4) O1 0.037(4) 0.044(4) 0.056(5) 0.025(4) -0.009(4) -0.002(3) O2 0.032(3) 0.050(4) 0.018(3) 0.010(3) -0.006(3) -0.008(3) O3 0.038(4) 0.021(3) 0.042(4) 0.000(3) 0.002(3) -0.005(3) O4 0.019(3) 0.041(4) 0.031(4) 0.005(3) 0.001(3) 0.003(3) O5 0.029(3) 0.032(4) 0.029(4) 0.013(3) 0.003(3) -0.009(3) O6 0.044(4) 0.066(5) 0.042(5) -0.018(4) 0.010(4) -0.016(4) O7 0.027(3) 0.042(4) 0.028(4) -0.006(3) 0.009(3) -0.008(3) O8 0.038(4) 0.032(4) 0.029(4) -0.010(3) 0.006(3) -0.010(3) O9 0.032(4) 0.044(4) 0.040(4) 0.006(3) 0.008(3) -0.014(3) O10 0.035(4) 0.025(3) 0.038(4) -0.009(3) 0.001(3) -0.003(3) O11 0.026(3) 0.038(4) 0.028(4) -0.003(3) 0.002(3) -0.004(3) O12 0.036(4) 0.045(4) 0.064(5) 0.009(4) -0.007(4) 0.015(3) O13 0.037(3) 0.031(3) 0.018(3) -0.005(3) -0.005(3) 0.007(3) O14 0.034(4) 0.031(4) 0.032(4) 0.005(3) 0.006(3) 0.005(3) O15 0.063(5) 0.046(5) 0.045(5) -0.027(4) -0.002(4) -0.003(4) O16 0.034(3) 0.028(3) 0.030(4) -0.008(3) -0.002(3) -0.010(3) O17 0.038(4) 0.036(4) 0.023(3) -0.008(3) 0.009(3) -0.004(3) O18 0.033(3) 0.044(4) 0.040(4) 0.006(3) 0.010(3) -0.006(3) O19 0.026(3) 0.021(3) 0.021(3) -0.003(2) 0.005(2) -0.002(2) W1 0.02607(19) 0.0295(2) 0.0302(2) 0.00853(18) -0.00093(16) -0.00013(17) W2 0.0302(2) 0.0350(2) 0.0223(2) -0.00894(17) 0.00291(17) -0.00817(17) W3 0.02805(19) 0.02576(19) 0.0297(2) 0.00181(17) -0.00087(16) 0.00346(16) W4 0.0324(2) 0.0281(2) 0.0241(2) -0.00848(16) -0.00006(17) -0.00157(17) W5 0.02383(18) 0.0300(2) 0.0244(2) 0.00025(16) 0.00268(16) -0.00549(16) W6 0.02671(19) 0.02604(19) 0.02243(19) 0.00213(16) 0.00529(16) -0.00200(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 C1 N1 1.481(12) . ? C1 C2 1.512(13) . ? C1 H1A 0.9700 . ? C1 H1B 0.9700 . ? C2 N2 1.455(11) . ? C2 H2A 0.9700 . ? C2 H2B 0.9700 . ? C3 N2 1.265(11) . ? C3 C11 1.486(12) . ? C3 C4 1.490(12) . ? C4 C5 1.522(13) . ? C4 H4A 0.9700 . ? C4 H4B 0.9700 . ? C5 N3 1.502(12) . ? C5 C13 1.516(13) . ? C5 C12 1.552(13) . ? C6 N3 1.487(11) . ? C6 C7 1.504(14) . ? C6 H6A 0.9700 . ? C6 H6B 0.9700 . ? C7 N4 1.485(12) . ? C7 H7A 0.9700 . ? C7 H7B 0.9700 . ? C8 N4 1.260(12) . ? C8 C9 1.503(15) . ? C8 C14 1.525(13) . ? C9 C10 1.536(14) . ? C9 H9A 0.9700 . ? C9 H9B 0.9700 . ? C10 N1 1.494(12) . ? C10 C16 1.515(14) . ? C10 C15 1.517(13) . ? C11 H11A 0.9600 . ? C11 H11B 0.9600 . ? C11 H11C 0.9600 . ? C12 H12A 0.9600 . ? C12 H12B 0.9600 . ? C12 H12C 0.9600 . ? C13 H13A 0.9600 . ? C13 H13B 0.9600 . ? C13 H13C 0.9600 . ? C14 H14A 0.9600 . ? C14 H14B 0.9600 . ? C14 H14C 0.9600 . ? C15 H15A 0.9600 . ? C15 H15B 0.9600 . ? C15 H15C 0.9600 . ? C16 H16A 0.9600 . ? C16 H16B 0.9600 . ? C16 H16C 0.9600 . ? C17 C18 1.439(14) . ? C17 H17A 0.9600 . ? C17 H17B 0.9600 . ? C17 H17C 0.9600 . ? C18 N5 1.141(12) . ? Cu1 N4 1.972(7) . ? Cu1 N2 1.976(7) . ? Cu1 N3 2.013(7) . ? Cu1 N1 2.015(7) . ? Cu1 N5 2.407(9) . ? O1 W1 1.693(6) . ? O2 W1 1.911(7) . ? O2 W2 1.942(7) . ? O3 W4 1.916(7) . ? O3 W1 1.924(6) . ? O4 W1 1.920(6) . ? O4 W6 1.932(6) . ? O5 W5 1.927(6) . ? O5 W1 1.929(6) . ? O6 W2 1.704(7) . ? O7 W5 1.915(6) . ? O7 W2 1.938(6) . ? O8 W6 1.908(6) . ? O8 W2 1.923(6) . ? O9 W5 1.710(6) . ? O10 W3 1.916(6) . ? O10 W2 1.924(7) . ? O11 W5 1.919(6) . ? O11 W3 1.928(6) . ? O12 W3 1.689(7) . ? O13 W3 1.922(6) . ? O13 W4 1.927(6) . ? O14 W6 1.914(6) . ? O14 W3 1.927(6) . ? O15 W4 1.687(7) . ? O16 W5 1.907(6) . ? O16 W4 1.921(6) . ? O17 W4 1.919(6) . ? O17 W6 1.945(6) . ? O18 W6 1.695(6) . ? O19 W1 2.315(6) . ? O19 W5 2.318(6) . ? O19 W6 2.322(6) . ? O19 W3 2.325(6) . ? O19 W4 2.325(6) . ? O19 W2 2.339(6) . ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag N1 C1 C2 109.5(8) . . ? N1 C1 H1A 109.8 . . ? C2 C1 H1A 109.8 . . ? N1 C1 H1B 109.8 . . ? C2 C1 H1B 109.8 . . ? H1A C1 H1B 108.2 . . ? N2 C2 C1 108.0(7) . . ? N2 C2 H2A 110.1 . . ? C1 C2 H2A 110.1 . . ? N2 C2 H2B 110.1 . . ? C1 C2 H2B 110.1 . . ? H2A C2 H2B 108.4 . . ? N2 C3 C11 123.9(9) . . ? N2 C3 C4 120.9(8) . . ? C11 C3 C4 115.1(9) . . ? C3 C4 C5 121.8(8) . . ? C3 C4 H4A 106.9 . . ? C5 C4 H4A 106.9 . . ? C3 C4 H4B 106.9 . . ? C5 C4 H4B 106.9 . . ? H4A C4 H4B 106.7 . . ? N3 C5 C13 111.7(9) . . ? N3 C5 C4 106.2(7) . . ? C13 C5 C4 109.0(8) . . ? N3 C5 C12 109.8(8) . . ? C13 C5 C12 109.5(8) . . ? C4 C5 C12 110.5(8) . . ? N3 C6 C7 109.2(7) . . ? N3 C6 H6A 109.8 . . ? C7 C6 H6A 109.8 . . ? N3 C6 H6B 109.8 . . ? C7 C6 H6B 109.8 . . ? H6A C6 H6B 108.3 . . ? N4 C7 C6 106.6(7) . . ? N4 C7 H7A 110.4 . . ? C6 C7 H7A 110.4 . . ? N4 C7 H7B 110.4 . . ? C6 C7 H7B 110.4 . . ? H7A C7 H7B 108.6 . . ? N4 C8 C9 123.5(9) . . ? N4 C8 C14 122.5(10) . . ? C9 C8 C14 113.8(9) . . ? C8 C9 C10 119.2(8) . . ? C8 C9 H9A 107.5 . . ? C10 C9 H9A 107.5 . . ? C8 C9 H9B 107.5 . . ? C10 C9 H9B 107.5 . . ? H9A C9 H9B 107.0 . . ? N1 C10 C16 111.0(8) . . ? N1 C10 C15 110.0(9) . . ? C16 C10 C15 110.2(9) . . ? N1 C10 C9 108.3(8) . . ? C16 C10 C9 110.4(9) . . ? C15 C10 C9 106.8(9) . . ? C3 C11 H11A 109.5 . . ? C3 C11 H11B 109.5 . . ? H11A C11 H11B 109.5 . . ? C3 C11 H11C 109.5 . . ? H11A C11 H11C 109.5 . . ? H11B C11 H11C 109.5 . . ? C5 C12 H12A 109.5 . . ? C5 C12 H12B 109.5 . . ? H12A C12 H12B 109.5 . . ? C5 C12 H12C 109.5 . . ? H12A C12 H12C 109.5 . . ? H12B C12 H12C 109.5 . . ? C5 C13 H13A 109.5 . . ? C5 C13 H13B 109.5 . . ? H13A C13 H13B 109.5 . . ? C5 C13 H13C 109.5 . . ? H13A C13 H13C 109.5 . . ? H13B C13 H13C 109.5 . . ? C8 C14 H14A 109.5 . . ? C8 C14 H14B 109.5 . . ? H14A C14 H14B 109.5 . . ? C8 C14 H14C 109.5 . . ? H14A C14 H14C 109.5 . . ? H14B C14 H14C 109.5 . . ? C10 C15 H15A 109.5 . . ? C10 C15 H15B 109.5 . . ? H15A C15 H15B 109.5 . . ? C10 C15 H15C 109.5 . . ? H15A C15 H15C 109.5 . . ? H15B C15 H15C 109.5 . . ? C10 C16 H16A 109.5 . . ? C10 C16 H16B 109.5 . . ? H16A C16 H16B 109.5 . . ? C10 C16 H16C 109.5 . . ? H16A C16 H16C 109.5 . . ? H16B C16 H16C 109.5 . . ? C18 C17 H17A 109.5 . . ? C18 C17 H17B 109.5 . . ? H17A C17 H17B 109.5 . . ? C18 C17 H17C 109.5 . . ? H17A C17 H17C 109.5 . . ? H17B C17 H17C 109.5 . . ? N5 C18 C17 178.4(13) . . ? N4 Cu1 N2 177.0(3) . . ? N4 Cu1 N3 86.5(3) . . ? N2 Cu1 N3 93.0(3) . . ? N4 Cu1 N1 94.0(3) . . ? N2 Cu1 N1 86.1(3) . . ? N3 Cu1 N1 171.8(3) . . ? N4 Cu1 N5 94.8(3) . . ? N2 Cu1 N5 88.2(3) . . ? N3 Cu1 N5 97.5(3) . . ? N1 Cu1 N5 90.6(3) . . ? C1 N1 C10 115.5(7) . . ? C1 N1 Cu1 107.3(6) . . ? C10 N1 Cu1 112.2(6) . . ? C3 N2 C2 121.7(8) . . ? C3 N2 Cu1 127.7(7) . . ? C2 N2 Cu1 108.5(5) . . ? C6 N3 C5 115.7(7) . . ? C6 N3 Cu1 106.6(6) . . ? C5 N3 Cu1 111.7(5) . . ? C8 N4 C7 124.3(8) . . ? C8 N4 Cu1 127.9(7) . . ? C7 N4 Cu1 107.7(6) . . ? C18 N5 Cu1 159.1(9) . . ? W1 O2 W2 117.6(3) . . ? W4 O3 W1 117.5(3) . . ? W1 O4 W6 116.8(3) . . ? W5 O5 W1 116.5(3) . . ? W5 O7 W2 117.9(3) . . ? W6 O8 W2 117.8(3) . . ? W3 O10 W2 117.6(3) . . ? W5 O11 W3 117.0(3) . . ? W3 O13 W4 117.6(3) . . ? W6 O14 W3 117.5(3) . . ? W5 O16 W4 117.7(3) . . ? W4 O17 W6 117.3(3) . . ? W1 O19 W5 90.1(2) . . ? W1 O19 W6 90.1(2) . . ? W5 O19 W6 179.7(3) . . ? W1 O19 W3 179.7(3) . . ? W5 O19 W3 89.9(2) . . ? W6 O19 W3 89.9(2) . . ? W1 O19 W4 90.1(2) . . ? W5 O19 W4 89.8(2) . . ? W6 O19 W4 90.4(2) . . ? W3 O19 W4 90.2(2) . . ? W1 O19 W2 90.2(2) . . ? W5 O19 W2 90.3(2) . . ? W6 O19 W2 89.5(2) . . ? W3 O19 W2 89.5(2) . . ? W4 O19 W2 179.7(3) . . ? O1 W1 O2 102.5(3) . . ? O1 W1 O4 102.5(3) . . ? O2 W1 O4 87.4(3) . . ? O1 W1 O3 104.7(3) . . ? O2 W1 O3 152.9(3) . . ? O4 W1 O3 86.9(3) . . ? O1 W1 O5 104.0(3) . . ? O2 W1 O5 87.0(3) . . ? O4 W1 O5 153.4(2) . . ? O3 W1 O5 86.3(3) . . ? O1 W1 O19 178.9(3) . . ? O2 W1 O19 76.6(2) . . ? O4 W1 O19 76.7(2) . . ? O3 W1 O19 76.2(2) . . ? O5 W1 O19 76.7(2) . . ? O6 W2 O8 106.2(3) . . ? O6 W2 O10 104.2(3) . . ? O8 W2 O10 86.6(3) . . ? O6 W2 O7 102.4(3) . . ? O8 W2 O7 151.5(3) . . ? O10 W2 O7 86.9(3) . . ? O6 W2 O2 104.0(3) . . ? O8 W2 O2 86.4(3) . . ? O10 W2 O2 151.7(3) . . ? O7 W2 O2 86.3(3) . . ? O6 W2 O19 177.7(3) . . ? O8 W2 O19 76.0(2) . . ? O10 W2 O19 76.2(2) . . ? O7 W2 O19 75.4(2) . . ? O2 W2 O19 75.5(2) . . ? O12 W3 O10 103.7(3) . . ? O12 W3 O13 103.4(3) . . ? O10 W3 O13 152.8(3) . . ? O12 W3 O14 103.1(3) . . ? O10 W3 O14 86.8(3) . . ? O13 W3 O14 86.3(3) . . ? O12 W3 O11 104.4(3) . . ? O10 W3 O11 87.1(3) . . ? O13 W3 O11 87.0(3) . . ? O14 W3 O11 152.5(3) . . ? O12 W3 O19 179.1(3) . . ? O10 W3 O19 76.7(2) . . ? O13 W3 O19 76.1(2) . . ? O14 W3 O19 76.1(2) . . ? O11 W3 O19 76.4(2) . . ? O15 W4 O3 104.4(3) . . ? O15 W4 O17 102.9(3) . . ? O3 W4 O17 86.9(3) . . ? O15 W4 O16 104.7(3) . . ? O3 W4 O16 86.5(3) . . ? O17 W4 O16 152.4(3) . . ? O15 W4 O13 103.4(3) . . ? O3 W4 O13 152.2(3) . . ? O17 W4 O13 87.0(3) . . ? O16 W4 O13 86.5(3) . . ? O15 W4 O19 179.1(3) . . ? O3 W4 O19 76.1(2) . . ? O17 W4 O19 76.4(2) . . ? O16 W4 O19 76.0(2) . . ? O13 W4 O19 76.0(2) . . ? O9 W5 O16 105.7(3) . . ? O9 W5 O7 101.5(3) . . ? O16 W5 O7 152.8(3) . . ? O9 W5 O11 102.5(3) . . ? O16 W5 O11 87.1(3) . . ? O7 W5 O11 86.4(3) . . ? O9 W5 O5 104.0(3) . . ? O16 W5 O5 87.4(3) . . ? O7 W5 O5 86.7(3) . . ? O11 W5 O5 153.4(2) . . ? O9 W5 O19 177.8(3) . . ? O16 W5 O19 76.4(2) . . ? O7 W5 O19 76.4(2) . . ? O11 W5 O19 76.7(2) . . ? O5 W5 O19 76.7(2) . . ? O18 W6 O8 105.1(3) . . ? O18 W6 O14 104.6(3) . . ? O8 W6 O14 87.4(3) . . ? O18 W6 O4 102.6(3) . . ? O8 W6 O4 87.8(3) . . ? O14 W6 O4 152.7(3) . . ? O18 W6 O17 102.2(3) . . ? O8 W6 O17 152.6(3) . . ? O14 W6 O17 86.7(3) . . ? O4 W6 O17 85.4(3) . . ? O18 W6 O19 177.9(3) . . ? O8 W6 O19 76.7(2) . . ? O14 W6 O19 76.4(2) . . ? O4 W6 O19 76.3(2) . . ? O17 W6 O19 75.9(2) . . ? _diffrn_measured_fraction_theta_max 1.000 _diffrn_reflns_theta_full 25.00 _diffrn_measured_fraction_theta_full 1.000 _refine_diff_density_max 0.919 _refine_diff_density_min -1.545 _refine_diff_density_rms 0.306