Supplementary Material (ESI) for Chemical Communications This journal is © The Royal Society of Chemistry 2001 data_global _journal_coden_Cambridge 182 _publ_requested_journal 'Chemical Communications' loop_ _publ_author_name 'Burkholder, Eric' 'Zubieta, Jon' _publ_contact_author_name 'Prof Jon Zubieta' _publ_contact_author_address ; Department of Chemistry Syracuse University Syracuse New York 13244 UNITED STATES OF AMERICA ; _publ_contact_author_email 'JAZUBIET@SYR.EDU' _publ_section_title ; Solid State Coordination Chemistry: Construction of 2D Networks and 3D Frameworks from Phosphomolybdate Clusters and Binuclear Cu(II) Complexes. The Syntheses and Structures of [{Cu2(tpypyz)(H2O)2}Mo5O15(HOPO3)2].nH2)(n = 2 and 3; tpypyz = tetra(2-pyridyl)pyrazine) ; data_compound_1 _database_code_CSD 167763 _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C24 H26 Cu2 Mo5 N6 O27 P2' _chemical_formula_weight 1499.23 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' 'P' 'P' 0.1023 0.0942 '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 ? _symmetry_space_group_name_H-M ? loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, -y, -z' _cell_length_a 11.0736(5) _cell_length_b 11.0775(5) _cell_length_c 17.7972(8) _cell_angle_alpha 85.178(1) _cell_angle_beta 79.964(1) _cell_angle_gamma 68.271(1) _cell_volume 1996.5(2) _cell_formula_units_Z 2 _cell_measurement_temperature 90(2) _cell_measurement_reflns_used ? _cell_measurement_theta_min ? _cell_measurement_theta_max ? _exptl_crystal_description ? _exptl_crystal_colour 'dark green' _exptl_crystal_size_max ? _exptl_crystal_size_mid ? _exptl_crystal_size_min ? _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 2.494 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1452 _exptl_absorpt_coefficient_mu 2.752 _exptl_absorpt_correction_type ? _exptl_absorpt_correction_T_min ? _exptl_absorpt_correction_T_max ? _exptl_absorpt_process_details ? _exptl_special_details ; ? ; _diffrn_ambient_temperature 293(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type ? _diffrn_measurement_method ? _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 9465 _diffrn_reflns_av_R_equivalents 0.0219 _diffrn_reflns_av_sigmaI/netI 0.0300 _diffrn_reflns_limit_h_min -12 _diffrn_reflns_limit_h_max 12 _diffrn_reflns_limit_k_min -12 _diffrn_reflns_limit_k_max 11 _diffrn_reflns_limit_l_min -14 _diffrn_reflns_limit_l_max 19 _diffrn_reflns_theta_min 1.16 _diffrn_reflns_theta_max 23.28 _reflns_number_total 5720 _reflns_number_gt 5075 _reflns_threshold_expression >2sigma(I) _computing_data_collection ? _computing_cell_refinement ? _computing_data_reduction ? _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^)+(0.0431P)^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 mixed _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 5720 _refine_ls_number_parameters 629 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0310 _refine_ls_R_factor_gt 0.0259 _refine_ls_wR_factor_ref 0.0687 _refine_ls_wR_factor_gt 0.0668 _refine_ls_goodness_of_fit_ref 1.067 _refine_ls_restrained_S_all 1.067 _refine_ls_shift/su_max 2.761 _refine_ls_shift/su_mean 0.007 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 0.25543(4) 0.05650(3) 0.29454(2) 0.00647(11) Uani 1 1 d . . . Mo2 Mo 0.26463(4) -0.27776(4) 0.31391(2) 0.00623(11) Uani 1 1 d . . . Mo3 Mo 0.58199(4) -0.46953(4) 0.26650(2) 0.00754(11) Uani 1 1 d . . . Mo4 Mo 0.75122(4) -0.28140(4) 0.18410(2) 0.00674(11) Uani 1 1 d . . . Mo5 Mo 0.54373(4) 0.03571(4) 0.18760(2) 0.00637(11) Uani 1 1 d . . . Cu1 Cu 1.07316(5) 0.55509(5) 0.27307(3) 0.00869(14) Uani 1 1 d . . . Cu2 Cu 0.80046(5) 0.14644(5) 0.22186(3) 0.00895(14) Uani 1 1 d . . . P1 P 0.51515(11) -0.16963(11) 0.34396(7) 0.0066(3) Uani 1 1 d . . . P2 P 0.42662(11) -0.19549(11) 0.15683(7) 0.0066(2) Uani 1 1 d . . . O1 O 1.2695(3) 0.3924(4) 0.3100(2) 0.0124(8) Uani 1 1 d . . . O2 O 0.9709(4) -0.0486(4) 0.2104(2) 0.0181(9) Uani 1 1 d . . . O3 O 0.5975(3) -0.2245(3) 0.41084(17) 0.0107(7) Uani 1 1 d . . . O4 O 0.3962(3) -0.0512(3) 0.36874(16) 0.0082(7) Uani 1 1 d . . . O5 O 0.4678(3) -0.2752(3) 0.32278(16) 0.0070(7) Uani 1 1 d . . . O6 O 0.6079(3) -0.1370(3) 0.27769(16) 0.0065(6) Uani 1 1 d . . . O7 O 0.6611(3) 0.0881(3) 0.21300(17) 0.0095(7) Uani 1 1 d . . . O8 O 0.5001(3) 0.1236(3) 0.10747(17) 0.0114(7) Uani 1 1 d . . . O9 O 0.6668(3) -0.1177(3) 0.13335(16) 0.0082(7) Uani 1 1 d . . . O10 O 0.3946(3) 0.1254(3) 0.26025(17) 0.0085(7) Uani 1 1 d . . . O11 O 0.4135(3) -0.0681(3) 0.19299(16) 0.0075(7) Uani 1 1 d . . . O12 O 0.4362(3) -0.1746(3) 0.06858(17) 0.0105(7) Uani 1 1 d . . . O13 O 0.3059(3) -0.2264(3) 0.19004(16) 0.0080(7) Uani 1 1 d . . . O14 O 0.8288(3) -0.3737(3) 0.10573(17) 0.0101(7) Uani 1 1 d . . . O15 O 0.7254(3) -0.4077(3) 0.25761(17) 0.0079(7) Uani 1 1 d . . . O16 O 0.6098(3) -0.5556(3) 0.35014(17) 0.0122(7) Uani 1 1 d . . . O17 O 0.6403(3) -0.5847(3) 0.19898(18) 0.0124(7) Uani 1 1 d . . . O18 O 0.5550(3) -0.3065(3) 0.17041(16) 0.0071(7) Uani 1 1 d . . . O19 O 0.3971(3) -0.4369(3) 0.27395(17) 0.0075(7) Uani 1 1 d . . . O20 O 0.2541(3) -0.3188(3) 0.40885(17) 0.0109(7) Uani 1 1 d . . . O21 O 0.2071(3) -0.0976(3) 0.31901(17) 0.0093(7) Uani 1 1 d . . . O22 O 0.1652(3) 0.1117(3) 0.22204(17) 0.0126(7) Uani 1 1 d . . . O23 O 0.1622(3) 0.1582(3) 0.36690(17) 0.0119(7) Uani 1 1 d . . . O24 O 0.1309(3) -0.3056(3) 0.28875(17) 0.0095(7) Uani 1 1 d . . . O25 O 0.8785(3) -0.2570(3) 0.21595(17) 0.0100(7) Uani 1 1 d . . . O99 O 0.4672(4) 0.6534(4) 0.5028(3) 0.0296(10) Uani 1 1 d . . . O100 O 0.3296(4) 0.0619(3) 0.0212(3) 0.0152(8) Uani 1 1 d . . . N1 N 0.9625(3) 0.5613(3) 0.3736(2) 0.0070(8) Uani 1 1 d . . . N2 N 1.0016(3) 0.4243(3) 0.2574(2) 0.0060(8) Uani 1 1 d . . . N3 N 1.1576(3) 0.5099(3) 0.1663(2) 0.0093(8) Uani 1 1 d . . . N4 N 0.7822(4) 0.1351(3) 0.3350(2) 0.0101(8) Uani 1 1 d . . . N5 N 0.8937(3) 0.2584(3) 0.2362(2) 0.0090(14) Uani 1.000(14) 1 d . . . N6 N 0.8564(4) 0.1851(3) 0.1134(2) 0.0097(8) Uani 1 1 d . . . C1 C 0.9404(4) 0.6458(4) 0.4285(3) 0.0106(10) Uani 1 1 d . . . H1 H 0.9839 0.7043 0.4209 0.013 Uiso 1 1 calc R . . C2 C 0.8559(4) 0.6498(4) 0.4957(3) 0.0098(10) Uani 1 1 d . . . H2 H 0.8436 0.7088 0.5331 0.012 Uiso 1 1 calc R . . C3 C 0.7894(4) 0.5634(4) 0.5064(3) 0.0101(10) Uani 1 1 d . . . H3 H 0.7312 0.5641 0.5510 0.012 Uiso 1 1 calc R . . C4 C 0.8111(4) 0.4759(4) 0.4494(2) 0.0085(10) Uani 1 1 d . . . H4 H 0.7661 0.4188 0.4547 0.010 Uiso 1 1 calc R . . C5 C 0.9009(4) 0.4752(4) 0.3846(2) 0.0060(10) Uani 1 1 d . . . C6 C 0.9306(4) 0.3897(4) 0.3181(2) 0.0079(10) Uani 1 1 d . . . C7 C 1.0226(4) 0.3809(4) 0.1863(2) 0.0059(10) Uani 1 1 d . . . C8 C 1.1288(4) 0.4154(4) 0.1368(3) 0.0082(10) Uani 1 1 d . . . C9 C 1.2030(4) 0.3501(4) 0.0724(3) 0.0116(10) Uani 1 1 d . . . H9 H 1.1841 0.2837 0.0545 0.014 Uiso 1 1 calc R . . C10 C 1.3070(5) 0.3843(5) 0.0341(3) 0.0171(11) Uani 1 1 d . . . H10 H 1.3586 0.3414 -0.0096 0.020 Uiso 1 1 calc R . . C11 C 1.3316(4) 0.4838(4) 0.0628(3) 0.0144(11) Uani 1 1 d . . . H11 H 1.3978 0.5112 0.0371 0.017 Uiso 1 1 calc R . . C12 C 1.2577(4) 0.5420(4) 0.1295(3) 0.0119(10) Uani 1 1 d . . . H12 H 1.2782 0.6057 0.1496 0.014 Uiso 1 1 calc R . . C13 C 0.8331(4) 0.1359(4) 0.0534(3) 0.0132(11) Uani 1 1 d . . . H13 H 0.7851 0.0813 0.0623 0.016 Uiso 1 1 calc R . . C14 C 0.8780(5) 0.1635(5) -0.0209(3) 0.0156(11) Uani 1 1 d . . . H14 H 0.8663 0.1233 -0.0615 0.019 Uiso 1 1 calc R . . C15 C 0.9406(4) 0.2520(4) -0.0336(3) 0.0125(10) Uani 1 1 d . . . H15 H 0.9697 0.2740 -0.0832 0.015 Uiso 1 1 calc R . . C16 C 0.9600(4) 0.3081(4) 0.0282(2) 0.0088(10) Uani 1 1 d . . . H16 H 0.9975 0.3716 0.0205 0.011 Uiso 1 1 calc R . . C17 C 0.9227(4) 0.2678(4) 0.1011(3) 0.0083(10) Uani 1 1 d . . . C18 C 0.9481(4) 0.3067(4) 0.1735(3) 0.0085(16) Uani 1.000(16) 1 d . . . C19 C 0.8916(4) 0.2859(4) 0.3080(2) 0.0067(10) Uani 1 1 d . . . C20 C 0.8469(4) 0.1984(4) 0.3650(3) 0.0071(10) Uani 1 1 d . . . C21 C 0.8753(4) 0.1719(4) 0.4375(3) 0.0096(10) Uani 1 1 d . . . H21 H 0.9245 0.2116 0.4561 0.012 Uiso 1 1 calc R . . C22 C 0.8296(4) 0.0839(4) 0.4837(3) 0.0119(10) Uani 1 1 d . . . H22 H 0.8472 0.0654 0.5335 0.014 Uiso 1 1 calc R . . C23 C 0.7585(5) 0.0255(5) 0.4543(3) 0.0165(11) Uani 1 1 d . . . H23 H 0.7241 -0.0304 0.4845 0.020 Uiso 1 1 calc R . . C24 C 0.7388(5) 0.0511(4) 0.3791(3) 0.0162(11) Uani 1 1 d . . . H24 H 0.6940 0.0087 0.3586 0.019 Uiso 1 1 calc R . . H1A H 1.295(6) 0.327(6) 0.294(3) 0.03(2) Uiso 1 1 d . . . H1B H 1.319(6) 0.440(6) 0.299(4) 0.05(2) Uiso 1 1 d . . . H2A H 0.974(6) -0.127(6) 0.225(3) 0.034(18) Uiso 1 1 d . . . H2B H 1.029(5) -0.062(5) 0.220(3) 0.001(17) Uiso 1 1 d . . . H10A H 0.335(5) 0.077(5) -0.018(3) 0.000(15) Uiso 1 1 d . . . H10B H 0.365(9) 0.094(9) 0.039(5) 0.11(4) Uiso 1 1 d . . . H99A H 0.462(6) 0.623(5) 0.539(3) 0.021(19) Uiso 1 1 d . . . H99B H 0.394(7) 0.651(6) 0.476(4) 0.07(2) Uiso 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 0.0052(2) 0.0054(2) 0.0091(2) -0.00024(16) -0.00029(16) -0.00264(16) Mo2 0.0057(2) 0.0057(2) 0.0083(2) 0.00026(16) -0.00035(16) -0.00365(16) Mo3 0.0055(2) 0.0060(2) 0.0110(2) 0.00080(17) -0.00078(16) -0.00245(17) Mo4 0.0049(2) 0.0072(2) 0.0081(2) 0.00074(16) -0.00036(16) -0.00270(17) Mo5 0.0064(2) 0.0070(2) 0.0072(2) 0.00050(16) -0.00078(16) -0.00434(17) Cu1 0.0094(3) 0.0098(3) 0.0094(3) -0.0018(2) 0.0010(2) -0.0071(2) Cu2 0.0108(3) 0.0124(3) 0.0078(3) -0.0002(2) -0.0004(2) -0.0094(2) P1 0.0065(6) 0.0069(6) 0.0071(6) 0.0012(5) -0.0012(5) -0.0035(5) P2 0.0070(6) 0.0070(6) 0.0064(6) -0.0001(5) -0.0010(5) -0.0031(5) O1 0.0120(19) 0.0076(19) 0.019(2) -0.0007(16) 0.0003(15) -0.0059(17) O2 0.014(2) 0.016(2) 0.024(2) 0.0029(16) -0.0082(18) -0.0047(18) O3 0.0119(17) 0.0138(17) 0.0075(17) 0.0019(14) -0.0053(13) -0.0049(14) O4 0.0098(17) 0.0081(16) 0.0080(17) -0.0002(13) -0.0010(13) -0.0047(13) O5 0.0046(16) 0.0082(15) 0.0084(17) 0.0004(13) 0.0013(12) -0.0036(13) O6 0.0055(16) 0.0082(15) 0.0060(16) 0.0022(13) -0.0007(12) -0.0034(13) O7 0.0095(17) 0.0098(16) 0.0106(17) -0.0007(13) 0.0008(13) -0.0060(14) O8 0.0141(17) 0.0080(16) 0.0108(18) 0.0013(13) -0.0001(14) -0.0035(14) O9 0.0086(16) 0.0095(16) 0.0066(17) 0.0010(13) 0.0000(13) -0.0042(13) O10 0.0086(16) 0.0092(16) 0.0099(17) 0.0010(13) 0.0012(13) -0.0071(14) O11 0.0064(16) 0.0070(15) 0.0089(17) 0.0018(13) -0.0016(13) -0.0024(13) O12 0.0114(17) 0.0115(16) 0.0091(17) -0.0019(13) -0.0018(13) -0.0042(14) O13 0.0072(16) 0.0069(15) 0.0112(17) 0.0002(13) -0.0032(13) -0.0032(13) O14 0.0094(17) 0.0122(16) 0.0088(17) -0.0006(13) 0.0019(13) -0.0056(14) O15 0.0053(16) 0.0094(16) 0.0102(17) 0.0041(13) -0.0019(13) -0.0045(13) O16 0.0102(17) 0.0096(16) 0.0151(18) 0.0038(14) -0.0022(14) -0.0024(14) O17 0.0099(17) 0.0110(16) 0.0158(18) -0.0038(14) -0.0027(14) -0.0021(14) O18 0.0076(16) 0.0059(15) 0.0088(17) -0.0015(13) -0.0009(13) -0.0034(13) O19 0.0070(16) 0.0040(15) 0.0125(17) -0.0001(13) -0.0026(13) -0.0026(13) O20 0.0129(17) 0.0092(16) 0.0117(18) -0.0004(13) 0.0009(13) -0.0064(14) O21 0.0079(16) 0.0075(16) 0.0123(17) -0.0020(13) -0.0012(13) -0.0022(13) O22 0.0105(17) 0.0118(17) 0.0140(18) 0.0018(14) -0.0016(14) -0.0029(14) O23 0.0114(17) 0.0106(16) 0.0139(18) -0.0037(14) 0.0024(14) -0.0053(14) O24 0.0068(16) 0.0090(16) 0.0132(18) 0.0000(13) 0.0004(13) -0.0044(13) O25 0.0080(16) 0.0118(16) 0.0119(17) 0.0008(14) -0.0007(13) -0.0062(14) O99 0.025(2) 0.048(3) 0.020(2) 0.015(2) -0.0046(19) -0.021(2) O100 0.021(2) 0.0159(19) 0.007(2) -0.0004(17) -0.0010(17) -0.0053(16) N1 0.0054(19) 0.0068(19) 0.011(2) 0.0000(16) -0.0026(16) -0.0038(16) N2 0.0048(19) 0.0052(19) 0.007(2) 0.0001(16) 0.0012(15) -0.0012(16) N3 0.009(2) 0.012(2) 0.010(2) 0.0048(17) -0.0019(16) -0.0077(17) N4 0.011(2) 0.010(2) 0.011(2) 0.0012(17) -0.0010(16) -0.0056(17) N5 0.004(2) 0.009(2) 0.011(3) -0.0005(17) -0.0019(16) 0.0011(17) N6 0.010(2) 0.013(2) 0.008(2) -0.0025(17) -0.0026(16) -0.0040(17) C1 0.007(2) 0.009(2) 0.018(3) 0.002(2) -0.005(2) -0.006(2) C2 0.009(2) 0.009(2) 0.011(3) -0.001(2) -0.0027(19) -0.002(2) C3 0.010(2) 0.014(2) 0.005(2) 0.001(2) -0.0015(19) -0.003(2) C4 0.010(2) 0.008(2) 0.010(3) 0.007(2) -0.005(2) -0.006(2) C5 0.008(2) 0.005(2) 0.004(2) 0.0007(18) -0.0052(19) -0.0009(19) C6 0.006(2) 0.010(2) 0.009(2) 0.0024(19) -0.0034(19) -0.0027(19) C7 0.004(2) 0.002(2) 0.010(3) 0.0032(19) 0.0007(18) -0.0005(18) C8 0.008(2) 0.005(2) 0.011(3) -0.0001(19) -0.0044(19) -0.0008(19) C9 0.005(2) 0.015(3) 0.016(3) -0.004(2) -0.002(2) -0.004(2) C10 0.012(3) 0.021(3) 0.019(3) -0.001(2) -0.002(2) -0.007(2) C11 0.008(2) 0.018(3) 0.018(3) -0.003(2) 0.005(2) -0.008(2) C12 0.014(3) 0.011(2) 0.015(3) 0.002(2) -0.004(2) -0.010(2) C13 0.013(3) 0.015(3) 0.014(3) -0.003(2) -0.002(2) -0.008(2) C14 0.017(3) 0.021(3) 0.013(3) -0.003(2) -0.004(2) -0.010(2) C15 0.011(2) 0.018(3) 0.009(3) 0.002(2) -0.0013(19) -0.006(2) C16 0.008(2) 0.012(2) 0.009(3) 0.002(2) -0.0024(19) -0.005(2) C17 0.004(2) 0.005(2) 0.013(3) 0.0010(19) 0.0013(19) 0.0002(19) C18 0.003(3) 0.009(3) 0.009(3) -0.002(2) 0.0006(19) 0.002(2) C19 0.004(2) 0.005(2) 0.008(3) -0.0002(19) -0.0023(18) 0.0018(19) C20 0.003(2) 0.004(2) 0.013(3) -0.0018(19) 0.0024(19) -0.0025(19) C21 0.007(2) 0.008(2) 0.012(3) -0.001(2) -0.0012(19) 0.000(2) C22 0.010(3) 0.011(2) 0.011(3) 0.001(2) 0.000(2) 0.000(2) C23 0.023(3) 0.013(3) 0.013(3) 0.003(2) 0.003(2) -0.010(2) C24 0.022(3) 0.016(3) 0.018(3) -0.002(2) 0.001(2) -0.016(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 Mo1 O22 1.703(3) . ? Mo1 O23 1.707(3) . ? Mo1 O10 1.948(3) . ? Mo1 O21 1.965(3) . ? Mo1 O4 2.162(3) . ? Mo1 O11 2.401(3) . ? Mo2 O20 1.708(3) . ? Mo2 O24 1.756(3) . ? Mo2 O21 1.862(3) . ? Mo2 O19 1.923(3) . ? Mo2 O13 2.241(3) . ? Mo2 O5 2.293(3) . ? Mo3 O17 1.693(3) . ? Mo3 O16 1.710(3) . ? Mo3 O19 1.925(3) . ? Mo3 O15 1.928(3) . ? Mo3 O5 2.268(3) . ? Mo3 O18 2.352(3) . ? Mo4 O14 1.703(3) . ? Mo4 O25 1.722(3) . ? Mo4 O15 1.899(3) . ? Mo4 O9 1.934(3) . ? Mo4 O6 2.345(3) . ? Mo4 O18 2.346(3) . ? Mo5 O8 1.695(3) . ? Mo5 O7 1.743(3) . ? Mo5 O10 1.909(3) . ? Mo5 O9 1.944(3) . ? Mo5 O11 2.139(3) . ? Mo5 O6 2.369(3) . ? Cu1 O24 1.932(3) 1_665 ? Cu1 N2 1.949(3) . ? Cu1 N1 1.975(4) . ? Cu1 N3 1.982(4) . ? Cu1 O1 2.409(3) . ? Cu2 O7 1.915(3) . ? Cu2 N5 1.939(4) . ? Cu2 N6 1.984(4) . ? Cu2 N4 1.986(4) . ? Cu2 O2 2.279(4) . ? P1 O4 1.505(3) . ? P1 O6 1.535(3) . ? P1 O5 1.544(3) . ? P1 O3 1.570(3) . ? P2 O13 1.511(3) . ? P2 O18 1.538(3) . ? P2 O11 1.547(3) . ? P2 O12 1.559(3) . ? O24 Cu1 1.932(3) 1_445 ? N1 C1 1.338(6) . ? N1 C5 1.348(5) . ? N2 C6 1.337(5) . ? N2 C7 1.343(6) . ? N3 C12 1.337(6) . ? N3 C8 1.369(5) . ? N4 C24 1.339(6) . ? N4 C20 1.364(5) . ? N5 C19 1.333(6) . ? N5 C18 1.341(6) . ? N6 C13 1.341(6) . ? N6 C17 1.354(6) . ? C1 C2 1.377(6) . ? C2 C3 1.392(6) . ? C3 C4 1.391(6) . ? C4 C5 1.382(6) . ? C5 C6 1.493(6) . ? C6 C19 1.404(6) . ? C7 C18 1.416(6) . ? C7 C8 1.490(6) . ? C8 C9 1.372(6) . ? C9 C10 1.393(6) . ? C10 C11 1.384(6) . ? C11 C12 1.376(6) . ? C13 C14 1.381(7) . ? C14 C15 1.380(6) . ? C15 C16 1.392(6) . ? C16 C17 1.381(6) . ? C17 C18 1.496(6) . ? C19 C20 1.493(6) . ? C20 C21 1.363(6) . ? C21 C22 1.403(6) . ? C22 C23 1.375(6) . ? C23 C24 1.382(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 O22 Mo1 O23 102.72(14) . . ? O22 Mo1 O10 99.94(13) . . ? O23 Mo1 O10 101.89(13) . . ? O22 Mo1 O21 95.30(13) . . ? O23 Mo1 O21 102.45(13) . . ? O10 Mo1 O21 147.54(12) . . ? O22 Mo1 O4 166.47(13) . . ? O23 Mo1 O4 90.60(13) . . ? O10 Mo1 O4 79.32(11) . . ? O21 Mo1 O4 79.27(11) . . ? O22 Mo1 O11 81.22(12) . . ? O23 Mo1 O11 169.96(12) . . ? O10 Mo1 O11 68.20(11) . . ? O21 Mo1 O11 86.23(11) . . ? O4 Mo1 O11 86.03(10) . . ? O20 Mo2 O24 102.22(14) . . ? O20 Mo2 O21 100.30(13) . . ? O24 Mo2 O21 103.90(13) . . ? O20 Mo2 O19 99.10(13) . . ? O24 Mo2 O19 96.08(13) . . ? O21 Mo2 O19 148.37(13) . . ? O20 Mo2 O13 172.40(12) . . ? O24 Mo2 O13 85.05(12) . . ? O21 Mo2 O13 79.86(12) . . ? O19 Mo2 O13 77.69(11) . . ? O20 Mo2 O5 86.07(12) . . ? O24 Mo2 O5 165.95(12) . . ? O21 Mo2 O5 85.46(11) . . ? O19 Mo2 O5 71.19(11) . . ? O13 Mo2 O5 86.37(10) . . ? O17 Mo3 O16 104.14(14) . . ? O17 Mo3 O19 98.78(13) . . ? O16 Mo3 O19 98.82(13) . . ? O17 Mo3 O15 101.43(14) . . ? O16 Mo3 O15 96.60(13) . . ? O19 Mo3 O15 150.67(12) . . ? O17 Mo3 O5 159.78(13) . . ? O16 Mo3 O5 95.09(12) . . ? O19 Mo3 O5 71.74(11) . . ? O15 Mo3 O5 82.19(11) . . ? O17 Mo3 O18 89.97(12) . . ? O16 Mo3 O18 163.37(12) . . ? O19 Mo3 O18 87.45(11) . . ? O15 Mo3 O18 71.61(11) . . ? O5 Mo3 O18 72.14(10) . . ? O14 Mo4 O25 102.64(14) . . ? O14 Mo4 O15 101.76(13) . . ? O25 Mo4 O15 99.52(13) . . ? O14 Mo4 O9 98.91(13) . . ? O25 Mo4 O9 102.73(13) . . ? O15 Mo4 O9 145.33(12) . . ? O14 Mo4 O6 168.12(12) . . ? O25 Mo4 O6 87.43(12) . . ? O15 Mo4 O6 82.48(11) . . ? O9 Mo4 O6 72.39(11) . . ? O14 Mo4 O18 89.47(12) . . ? O25 Mo4 O18 166.68(12) . . ? O15 Mo4 O18 72.22(11) . . ? O9 Mo4 O18 80.50(11) . . ? O6 Mo4 O18 81.21(10) . . ? O8 Mo5 O7 104.43(14) . . ? O8 Mo5 O10 100.03(13) . . ? O7 Mo5 O10 100.37(13) . . ? O8 Mo5 O9 94.76(13) . . ? O7 Mo5 O9 96.74(13) . . ? O10 Mo5 O9 153.74(12) . . ? O8 Mo5 O11 96.00(12) . . ? O7 Mo5 O11 159.55(12) . . ? O10 Mo5 O11 74.87(11) . . ? O9 Mo5 O11 82.15(11) . . ? O8 Mo5 O6 163.26(12) . . ? O7 Mo5 O6 87.30(11) . . ? O10 Mo5 O6 89.31(11) . . ? O9 Mo5 O6 71.69(11) . . ? O11 Mo5 O6 72.91(10) . . ? O24 Cu1 N2 175.69(13) 1_665 . ? O24 Cu1 N1 97.34(13) 1_665 . ? N2 Cu1 N1 80.99(14) . . ? O24 Cu1 N3 100.75(14) 1_665 . ? N2 Cu1 N3 80.79(14) . . ? N1 Cu1 N3 161.73(14) . . ? O24 Cu1 O1 92.10(13) 1_665 . ? N2 Cu1 O1 92.01(14) . . ? N1 Cu1 O1 95.65(13) . . ? N3 Cu1 O1 86.31(13) . . ? O7 Cu2 N5 161.36(14) . . ? O7 Cu2 N6 100.93(14) . . ? N5 Cu2 N6 80.81(15) . . ? O7 Cu2 N4 96.77(14) . . ? N5 Cu2 N4 81.50(15) . . ? N6 Cu2 N4 162.07(15) . . ? O7 Cu2 O2 98.66(14) . . ? N5 Cu2 O2 99.94(15) . . ? N6 Cu2 O2 88.38(14) . . ? N4 Cu2 O2 91.80(14) . . ? O4 P1 O6 111.39(16) . . ? O4 P1 O5 108.39(16) . . ? O6 P1 O5 111.97(17) . . ? O4 P1 O3 110.52(17) . . ? O6 P1 O3 106.26(17) . . ? O5 P1 O3 108.26(16) . . ? O13 P2 O18 112.39(17) . . ? O13 P2 O11 107.46(17) . . ? O18 P2 O11 111.23(16) . . ? O13 P2 O12 110.98(17) . . ? O18 P2 O12 105.92(17) . . ? O11 P2 O12 108.84(16) . . ? P1 O4 Mo1 123.14(17) . . ? P1 O5 Mo3 130.59(16) . . ? P1 O5 Mo2 133.37(16) . . ? Mo3 O5 Mo2 95.05(10) . . ? P1 O6 Mo4 125.77(16) . . ? P1 O6 Mo5 125.40(16) . . ? Mo4 O6 Mo5 92.71(10) . . ? Mo5 O7 Cu2 169.84(19) . . ? Mo4 O9 Mo5 123.14(15) . . ? Mo5 O10 Mo1 121.10(15) . . ? P2 O11 Mo5 133.04(18) . . ? P2 O11 Mo1 130.72(16) . . ? Mo5 O11 Mo1 95.26(11) . . ? P2 O13 Mo2 122.03(16) . . ? Mo4 O15 Mo3 124.03(15) . . ? P2 O18 Mo4 125.48(16) . . ? P2 O18 Mo3 127.36(17) . . ? Mo4 O18 Mo3 92.02(10) . . ? Mo2 O19 Mo3 121.91(14) . . ? Mo2 O21 Mo1 145.54(17) . . ? Mo2 O24 Cu1 141.48(17) . 1_445 ? C1 N1 C5 118.8(4) . . ? C1 N1 Cu1 125.7(3) . . ? C5 N1 Cu1 115.4(3) . . ? C6 N2 C7 125.5(4) . . ? C6 N2 Cu1 116.9(3) . . ? C7 N2 Cu1 117.5(3) . . ? C12 N3 C8 118.6(4) . . ? C12 N3 Cu1 125.0(3) . . ? C8 N3 Cu1 114.7(3) . . ? C24 N4 C20 119.2(4) . . ? C24 N4 Cu2 125.0(3) . . ? C20 N4 Cu2 114.1(3) . . ? C19 N5 C18 125.8(4) . . ? C19 N5 Cu2 116.5(3) . . ? C18 N5 Cu2 117.6(3) . . ? C13 N6 C17 119.3(4) . . ? C13 N6 Cu2 124.9(3) . . ? C17 N6 Cu2 115.8(3) . . ? N1 C1 C2 122.9(4) . . ? C1 C2 C3 118.4(4) . . ? C4 C3 C2 119.1(4) . . ? C5 C4 C3 118.9(4) . . ? N1 C5 C4 121.8(4) . . ? N1 C5 C6 113.4(4) . . ? C4 C5 C6 124.5(4) . . ? N2 C6 C19 116.1(4) . . ? N2 C6 C5 112.7(4) . . ? C19 C6 C5 131.1(4) . . ? N2 C7 C18 116.1(4) . . ? N2 C7 C8 111.4(4) . . ? C18 C7 C8 132.4(4) . . ? N3 C8 C9 121.6(4) . . ? N3 C8 C7 113.4(4) . . ? C9 C8 C7 124.5(4) . . ? C8 C9 C10 119.4(4) . . ? C11 C10 C9 118.3(5) . . ? C12 C11 C10 119.9(4) . . ? N3 C12 C11 122.0(4) . . ? N6 C13 C14 122.2(4) . . ? C15 C14 C13 118.5(4) . . ? C14 C15 C16 119.6(4) . . ? C17 C16 C15 118.8(4) . . ? N6 C17 C16 121.2(4) . . ? N6 C17 C18 112.6(4) . . ? C16 C17 C18 126.2(4) . . ? N5 C18 C7 115.8(4) . . ? N5 C18 C17 113.1(4) . . ? C7 C18 C17 131.1(4) . . ? N5 C19 C6 116.4(4) . . ? N5 C19 C20 112.9(4) . . ? C6 C19 C20 130.7(4) . . ? C21 C20 N4 121.3(4) . . ? C21 C20 C19 125.9(4) . . ? N4 C20 C19 112.5(4) . . ? C20 C21 C22 119.3(4) . . ? C23 C22 C21 119.0(4) . . ? C22 C23 C24 119.0(4) . . ? N4 C24 C23 122.0(4) . . ? _diffrn_measured_fraction_theta_max 0.994 _diffrn_reflns_theta_full 23.28 _diffrn_measured_fraction_theta_full 0.994 _refine_diff_density_max 0.626 _refine_diff_density_min -0.527 _refine_diff_density_rms 0.113 #===END data_compound_2 _database_code_CSD 167764 _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C24 H28 Cu2 Mo5 N6 O28 P2' _chemical_formula_weight 1517.24 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' 'P' 'P' 0.1023 0.0942 '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' 'O' 'O' 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting ? _symmetry_space_group_name_H-M ? 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 18.3609(1) _cell_length_b 16.0705(1) _cell_length_c 13.4127(9) _cell_angle_alpha 90.00 _cell_angle_beta 102.6690(1) _cell_angle_gamma 90.00 _cell_volume 3861.3(4) _cell_formula_units_Z 4 _cell_measurement_temperature 90(2) _cell_measurement_reflns_used ? _cell_measurement_theta_min ? _cell_measurement_theta_max ? _exptl_crystal_description ? _exptl_crystal_colour 'dark green' _exptl_crystal_size_max ? _exptl_crystal_size_mid ? _exptl_crystal_size_min ? _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 2.610 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 2944 _exptl_absorpt_coefficient_mu 2.849 _exptl_absorpt_correction_type ? _exptl_absorpt_correction_T_min ? _exptl_absorpt_correction_T_max ? _exptl_absorpt_process_details ? _exptl_special_details ; ? ; _diffrn_ambient_temperature 293(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type ? _diffrn_measurement_method ? _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 8980 _diffrn_reflns_av_R_equivalents 0.0466 _diffrn_reflns_av_sigmaI/netI 0.0524 _diffrn_reflns_limit_h_min -19 _diffrn_reflns_limit_h_max 20 _diffrn_reflns_limit_k_min -15 _diffrn_reflns_limit_k_max 17 _diffrn_reflns_limit_l_min -14 _diffrn_reflns_limit_l_max 14 _diffrn_reflns_theta_min 1.70 _diffrn_reflns_theta_max 23.28 _reflns_number_total 2789 _reflns_number_gt 2168 _reflns_threshold_expression >2sigma(I) _computing_data_collection ? _computing_cell_refinement ? _computing_data_reduction ? _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^)+(0.0543P)^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 mixed _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 2789 _refine_ls_number_parameters 310 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0475 _refine_ls_R_factor_gt 0.0320 _refine_ls_wR_factor_ref 0.0981 _refine_ls_wR_factor_gt 0.0802 _refine_ls_goodness_of_fit_ref 1.086 _refine_ls_restrained_S_all 1.086 _refine_ls_shift/su_max 2.665 _refine_ls_shift/su_mean 0.014 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 -0.07622(4) 0.35749(4) 0.31895(5) 0.0083(2) Uani 1 1 d . . . Mo2 Mo -0.09771(4) 0.15713(4) 0.38106(5) 0.0074(2) Uani 1 1 d . . . Mo3 Mo 0.0000 0.03578(6) 0.2500 0.0057(2) Uani 1 2 d S . . Cu1 Cu 0.15246(5) -0.11092(6) 0.35251(7) 0.0083(3) Uani 1 1 d . . . P1 P 0.07867(11) 0.21494(12) 0.36371(15) 0.0069(5) Uani 1 1 d . . . O1 O 0.2057(3) -0.0741(3) 0.2183(4) 0.0166(13) Uani 1 1 d . . . O2 O 0.0733(3) -0.0327(3) 0.2994(4) 0.0093(12) Uani 1 1 d . . . O3 O 0.1181(3) 0.1845(3) 0.4724(4) 0.0146(13) Uani 1 1 d . . . O4 O -0.0027(3) 0.2366(3) 0.3654(4) 0.0068(11) Uani 1 1 d . . . O5 O 0.0000 0.3869(4) 0.2500 0.0115(17) Uani 1 2 d S . . O6 O -0.0824(3) 0.1564(3) 0.5110(4) 0.0113(12) Uani 1 1 d . . . O7 O -0.0251(3) 0.0692(3) 0.3716(4) 0.0074(12) Uani 1 1 d . . . O8 O -0.0811(3) 0.1431(3) 0.2114(4) 0.0078(12) Uani 1 1 d . . . O9 O -0.1791(3) 0.1022(3) 0.3429(4) 0.0116(12) Uani 1 1 d . . . O10 O -0.1357(3) 0.2667(3) 0.3535(4) 0.0092(12) Uani 1 1 d . . . O11 O -0.1428(3) 0.4311(3) 0.2777(4) 0.0134(13) Uani 1 1 d . . . O12 O -0.1181(3) 0.2907(3) 0.1645(4) 0.0082(12) Uani 1 1 d . . . O13 O -0.0353(3) 0.3922(3) 0.4388(4) 0.0121(12) Uani 1 1 d . . . O100 O 0.1026(7) 0.0514(8) 0.5434(9) 0.033(3) Uani 0.50 1 d P . . O101 O 0.2289(3) 0.2197(3) 0.6281(5) 0.0259(15) Uani 1 1 d . . . C1 C 0.2326(4) 0.0448(5) 0.4242(6) 0.0112(18) Uani 1 1 d . . . H1 H 0.1932 0.0727 0.3821 0.013 Uiso 1 1 calc R . . C2 C 0.2840(4) -0.0761(5) 0.5028(6) 0.013(3) Uani 1.00(3) 1 d . . . C3 C 0.3505(4) -0.0365(5) 0.5445(6) 0.0107(18) Uani 1 1 d . . . H3 H 0.3903 -0.0660 0.5836 0.013 Uiso 1 1 calc R . . C4 C 0.2698(4) -0.1680(5) 0.5111(6) 0.0081(17) Uani 1 1 d . . . C5 C 0.1981(4) -0.2746(5) 0.4139(6) 0.0078(17) Uani 1 1 d . . . C6 C 0.1437(4) -0.2853(5) 0.3148(5) 0.0063(17) Uani 1 1 d . . . C7 C 0.1305(4) -0.3587(5) 0.2594(6) 0.0099(18) Uani 1 1 d . . . H7 H 0.1568 -0.4067 0.2835 0.012 Uiso 1 1 calc R . . C8 C 0.0610(4) -0.2149(5) 0.1878(6) 0.0113(18) Uani 1 1 d . . . H8 H 0.0384 -0.1656 0.1609 0.014 Uiso 1 1 calc R . . C9 C 0.0426(4) -0.2888(5) 0.1332(6) 0.0117(18) Uani 1 1 d . . . H9 H 0.0062 -0.2892 0.0728 0.014 Uiso 1 1 calc R . . C10 C 0.0788(4) -0.3601(5) 0.1697(6) 0.0108(18) Uani 1 1 d . . . H10 H 0.0682 -0.4096 0.1335 0.013 Uiso 1 1 calc R . . C11 C 0.2965(5) 0.0888(5) 0.4677(6) 0.016(3) Uani 1.00(3) 1 d . . . H11 H 0.2990 0.1458 0.4570 0.019 Uiso 1 1 calc R . . C12 C 0.3570(4) 0.0471(5) 0.5275(6) 0.0104(18) Uani 1 1 d . . . H12 H 0.4009 0.0753 0.5554 0.012 Uiso 1 1 calc R . . N1 N 0.2259(3) -0.0359(4) 0.4406(5) 0.0084(15) Uani 1 1 d . . . N2 N 0.1101(3) -0.2132(4) 0.2779(4) 0.0078(15) Uani 1 1 d . . . N3 N 0.2191(3) -0.1946(4) 0.4308(4) 0.0076(15) 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 0.0085(4) 0.0057(4) 0.0107(4) -0.0009(3) 0.0020(3) 0.0013(3) Mo2 0.0077(4) 0.0070(4) 0.0082(4) -0.0007(3) 0.0031(3) -0.0014(3) Mo3 0.0064(5) 0.0039(5) 0.0068(5) 0.000 0.0013(4) 0.000 Cu1 0.0086(5) 0.0043(5) 0.0102(5) 0.0000(4) -0.0017(4) 0.0011(4) P1 0.0073(11) 0.0060(11) 0.0071(10) -0.0009(9) 0.0014(8) 0.0006(9) O1 0.018(3) 0.020(3) 0.014(3) -0.002(3) 0.008(2) 0.001(3) O2 0.009(3) 0.007(3) 0.011(3) -0.001(2) 0.001(2) 0.000(2) O3 0.018(3) 0.017(3) 0.007(3) -0.003(3) -0.002(2) 0.009(3) O4 0.006(3) 0.004(3) 0.010(3) 0.001(2) 0.003(2) 0.000(2) O5 0.013(4) 0.006(4) 0.017(4) 0.000 0.006(3) 0.000 O6 0.009(3) 0.011(3) 0.014(3) -0.002(2) 0.003(2) 0.001(2) O7 0.009(3) 0.006(3) 0.006(3) -0.002(2) 0.000(2) 0.000(2) O8 0.010(3) 0.006(3) 0.008(3) 0.000(2) 0.003(2) 0.000(2) O9 0.010(3) 0.012(3) 0.013(3) -0.001(2) 0.004(2) -0.003(2) O10 0.007(3) 0.007(3) 0.013(3) -0.001(2) 0.002(2) 0.000(2) O11 0.015(3) 0.009(3) 0.016(3) 0.001(2) 0.002(2) 0.002(2) O12 0.006(3) 0.005(3) 0.012(3) 0.003(2) 0.000(2) 0.002(2) O13 0.011(3) 0.009(3) 0.016(3) -0.003(2) 0.001(2) 0.001(2) O100 0.038(8) 0.030(8) 0.029(7) 0.004(6) 0.003(6) -0.001(7) O101 0.023(4) 0.017(4) 0.040(4) 0.013(3) 0.012(3) 0.003(3) C1 0.013(5) 0.006(5) 0.016(5) 0.001(4) 0.006(4) 0.006(4) C2 0.019(6) 0.009(5) 0.014(5) -0.002(4) 0.009(4) 0.005(4) C3 0.006(4) 0.017(5) 0.011(4) 0.001(4) 0.006(3) 0.004(4) C4 0.005(4) 0.008(5) 0.010(4) -0.004(3) -0.001(3) 0.003(3) C5 0.003(4) 0.009(5) 0.012(4) 0.003(4) 0.003(3) 0.002(3) C6 0.006(4) 0.006(4) 0.009(4) -0.001(3) 0.005(3) -0.001(3) C7 0.015(5) 0.006(5) 0.011(4) 0.005(3) 0.009(4) 0.005(3) C8 0.012(4) 0.015(5) 0.008(4) 0.006(4) 0.005(3) 0.000(4) C9 0.013(4) 0.016(5) 0.007(4) -0.002(4) 0.003(3) -0.005(4) C10 0.011(4) 0.011(5) 0.011(4) -0.001(4) 0.004(3) -0.002(4) C11 0.024(6) 0.001(5) 0.022(5) -0.001(4) 0.008(4) -0.001(4) C12 0.013(4) 0.004(4) 0.015(4) -0.001(4) 0.005(3) -0.002(4) N1 0.009(4) 0.008(4) 0.008(3) -0.001(3) 0.003(3) 0.002(3) N2 0.006(3) 0.014(4) 0.006(3) 0.002(3) 0.005(3) 0.002(3) N3 0.008(4) 0.006(4) 0.009(4) -0.002(3) 0.003(3) -0.003(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 O11 1.703(5) . ? Mo1 O13 1.711(5) . ? Mo1 O5 1.8986(19) . ? Mo1 O10 1.939(5) . ? Mo1 O12 2.310(5) . ? Mo1 O4 2.370(5) . ? Mo2 O6 1.704(5) . ? Mo2 O9 1.714(5) . ? Mo2 O10 1.900(5) . ? Mo2 O7 1.966(5) . ? Mo2 O4 2.208(5) . ? Mo2 O8 2.372(5) . ? Mo3 O2 1.752(5) 2 ? Mo3 O2 1.752(5) . ? Mo3 O7 1.868(5) 2 ? Mo3 O7 1.868(5) . ? Mo3 O8 2.263(5) 2 ? Mo3 O8 2.263(5) . ? Cu1 O2 1.936(5) . ? Cu1 N3 1.961(6) . ? Cu1 N2 1.991(6) . ? Cu1 N1 1.993(6) . ? Cu1 O1 2.306(5) . ? P1 O12 1.507(5) 2 ? P1 O4 1.539(5) . ? P1 O8 1.540(5) 2 ? P1 O3 1.558(5) . ? O5 Mo1 1.8986(19) 2 ? O8 P1 1.540(5) 2 ? O12 P1 1.507(5) 2 ? C1 N1 1.326(10) . ? C1 C11 1.384(11) . ? C2 N1 1.364(10) . ? C2 C3 1.382(11) . ? C2 C4 1.507(11) . ? C3 C12 1.372(11) . ? C4 N3 1.330(9) . ? C4 C5 1.397(10) 7_546 ? C5 N3 1.348(9) . ? C5 C4 1.397(10) 7_546 ? C5 C6 1.487(10) . ? C6 N2 1.355(9) . ? C6 C7 1.387(10) . ? C7 C10 1.359(10) . ? C8 N2 1.341(9) . ? C8 C9 1.396(10) . ? C9 C10 1.361(10) . ? C11 C12 1.391(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 O11 Mo1 O13 102.4(2) . . ? O11 Mo1 O5 102.8(2) . . ? O13 Mo1 O5 99.07(19) . . ? O11 Mo1 O10 101.5(2) . . ? O13 Mo1 O10 100.1(2) . . ? O5 Mo1 O10 144.8(3) . . ? O11 Mo1 O12 87.5(2) . . ? O13 Mo1 O12 170.0(2) . . ? O5 Mo1 O12 79.33(17) . . ? O10 Mo1 O12 76.71(19) . . ? O11 Mo1 O4 168.9(2) . . ? O13 Mo1 O4 85.0(2) . . ? O5 Mo1 O4 83.9(2) . . ? O10 Mo1 O4 68.79(19) . . ? O12 Mo1 O4 85.02(17) . . ? O6 Mo2 O9 103.8(2) . . ? O6 Mo2 O10 100.2(2) . . ? O9 Mo2 O10 99.2(2) . . ? O6 Mo2 O7 95.7(2) . . ? O9 Mo2 O7 99.8(2) . . ? O10 Mo2 O7 151.5(2) . . ? O6 Mo2 O4 98.3(2) . . ? O9 Mo2 O4 157.6(2) . . ? O10 Mo2 O4 73.1(2) . . ? O7 Mo2 O4 81.30(19) . . ? O6 Mo2 O8 162.5(2) . . ? O9 Mo2 O8 87.3(2) . . ? O10 Mo2 O8 91.16(19) . . ? O7 Mo2 O8 68.78(18) . . ? O4 Mo2 O8 72.14(17) . . ? O2 Mo3 O2 102.2(3) 2 . ? O2 Mo3 O7 99.6(2) 2 2 ? O2 Mo3 O7 101.2(2) . 2 ? O2 Mo3 O7 101.2(2) 2 . ? O2 Mo3 O7 99.6(2) . . ? O7 Mo3 O7 146.6(3) 2 . ? O2 Mo3 O8 167.8(2) 2 2 ? O2 Mo3 O8 88.8(2) . 2 ? O7 Mo3 O8 72.82(19) 2 2 ? O7 Mo3 O8 81.82(19) . 2 ? O2 Mo3 O8 88.8(2) 2 . ? O2 Mo3 O8 167.8(2) . . ? O7 Mo3 O8 81.82(19) 2 . ? O7 Mo3 O8 72.82(19) . . ? O8 Mo3 O8 80.7(2) 2 . ? O2 Cu1 N3 166.5(2) . . ? O2 Cu1 N2 99.9(2) . . ? N3 Cu1 N2 80.4(2) . . ? O2 Cu1 N1 100.4(2) . . ? N3 Cu1 N1 80.5(3) . . ? N2 Cu1 N1 159.4(3) . . ? O2 Cu1 O1 87.6(2) . . ? N3 Cu1 O1 105.8(2) . . ? N2 Cu1 O1 90.3(2) . . ? N1 Cu1 O1 87.7(2) . . ? O12 P1 O4 110.1(3) 2 . ? O12 P1 O8 110.9(3) 2 2 ? O4 P1 O8 110.3(3) . 2 ? O12 P1 O3 109.8(3) 2 . ? O4 P1 O3 108.1(3) . . ? O8 P1 O3 107.6(3) 2 . ? Mo3 O2 Cu1 178.4(3) . . ? P1 O4 Mo2 131.3(3) . . ? P1 O4 Mo1 132.8(3) . . ? Mo2 O4 Mo1 94.74(18) . . ? Mo1 O5 Mo1 151.2(4) . 2 ? Mo3 O7 Mo2 124.3(3) . . ? P1 O8 Mo3 127.5(3) 2 . ? P1 O8 Mo2 125.8(3) 2 . ? Mo3 O8 Mo2 94.00(17) . . ? Mo2 O10 Mo1 122.8(3) . . ? P1 O12 Mo1 121.1(3) 2 . ? N1 C1 C11 122.0(7) . . ? N1 C2 C3 122.2(7) . . ? N1 C2 C4 112.6(7) . . ? C3 C2 C4 125.0(7) . . ? C12 C3 C2 119.0(7) . . ? N3 C4 C5 118.7(7) . 7_546 ? N3 C4 C2 110.9(7) . . ? C5 C4 C2 130.4(7) 7_546 . ? N3 C5 C4 116.7(7) . 7_546 ? N3 C5 C6 111.9(6) . . ? C4 C5 C6 131.4(7) 7_546 . ? N2 C6 C7 121.3(7) . . ? N2 C6 C5 113.0(6) . . ? C7 C6 C5 125.6(7) . . ? C10 C7 C6 119.7(7) . . ? N2 C8 C9 121.9(7) . . ? C10 C9 C8 119.0(7) . . ? C7 C10 C9 119.7(8) . . ? C1 C11 C12 119.5(7) . . ? C3 C12 C11 118.7(7) . . ? C1 N1 C2 118.5(7) . . ? C1 N1 Cu1 124.6(5) . . ? C2 N1 Cu1 114.4(5) . . ? C8 N2 C6 118.3(7) . . ? C8 N2 Cu1 125.6(5) . . ? C6 N2 Cu1 115.2(5) . . ? C4 N3 C5 124.6(6) . . ? C4 N3 Cu1 117.2(5) . . ? C5 N3 Cu1 116.2(5) . . ? _diffrn_measured_fraction_theta_max 0.999 _diffrn_reflns_theta_full 23.28 _diffrn_measured_fraction_theta_full 0.999 _refine_diff_density_max 2.231 _refine_diff_density_min -0.740 _refine_diff_density_rms 0.198 #===END