data_global _journal_name_full CrystEngComm _journal_coden_Cambridge 1350 _publ_contact_author_name 'Sato, Osamu' _publ_contact_author_email sato@cm.kyushu-u.ac.jp _publ_section_title ; A one-dimensional homochiral Mo(IV)-Cu(II) coordination polymer: spontaneous resolution and photoresponsive properties ; loop_ _publ_author_name W.Zhang H.-L.Sun O.Sato #===END OF CIF data_2 _database_code_depnum_ccdc_archive 'CCDC 671018' #TrackingRef '- compound_1-2.cif' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C36 H86 Cu4 Mo2 N30 O12' _chemical_formula_weight 1577.39 loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Cu Cu 0.3201 1.2651 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Mo Mo -1.6832 0.6857 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting triclinic _symmetry_space_group_name_H-M P-1 loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, -y, -z' _cell_length_a 9.850(2) _cell_length_b 11.607(2) _cell_length_c 14.313(3) _cell_angle_alpha 90.89(3) _cell_angle_beta 104.70(3) _cell_angle_gamma 93.75(3) _cell_volume 1578.5(6) _cell_formula_units_Z 1 _cell_measurement_temperature 123(2) _cell_measurement_reflns_used 4864 _cell_measurement_theta_min 3.2 _cell_measurement_theta_max 27.5 _exptl_crystal_description platelet _exptl_crystal_colour blue _exptl_crystal_size_max 0.20 _exptl_crystal_size_mid 0.10 _exptl_crystal_size_min 0.08 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.659 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 808 _exptl_absorpt_coefficient_mu 1.784 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.692 _exptl_absorpt_correction_T_max 0.758 _exptl_absorpt_process_details ? _exptl_special_details ; Jacobson, R. (1998) Private communication ; _diffrn_ambient_temperature 123(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'Rigaku Saturn' _diffrn_measurement_method \w _diffrn_detector_area_resol_mean 7.31 _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 10685 _diffrn_reflns_av_R_equivalents 0.0244 _diffrn_reflns_av_sigmaI/netI 0.0367 _diffrn_reflns_limit_h_min -11 _diffrn_reflns_limit_h_max 11 _diffrn_reflns_limit_k_min -13 _diffrn_reflns_limit_k_max 13 _diffrn_reflns_limit_l_min -17 _diffrn_reflns_limit_l_max 15 _diffrn_reflns_theta_min 3.17 _diffrn_reflns_theta_max 25.00 _reflns_number_total 5441 _reflns_number_gt 4638 _reflns_threshold_expression >2sigma(I) _computing_data_collection CrystalClear _computing_cell_refinement CrystalClear _computing_data_reduction CrystalStructure _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics ? _computing_publication_material ? _refine_special_details ; Refinement of F^2^ against ALL reflections. The weighted R-factor wR and goodness of fit S are based on F^2^, conventional R-factors R are based on F, with F set to zero for negative F^2^. The threshold expression of F^2^ > 2sigma(F^2^) is used only for calculating R-factors(gt) etc. and is not relevant to the choice of reflections for refinement. R-factors based on F^2^ are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger. ; _refine_ls_structure_factor_coef Fsqd _refine_ls_matrix_type full _refine_ls_weighting_scheme calc _refine_ls_weighting_details 'calc w=1/[\s^2^(Fo^2^)+(0.0435P)^2^+0.6268P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment constr _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 5441 _refine_ls_number_parameters 379 _refine_ls_number_restraints 1 _refine_ls_R_factor_all 0.0385 _refine_ls_R_factor_gt 0.0307 _refine_ls_wR_factor_ref 0.0807 _refine_ls_wR_factor_gt 0.0771 _refine_ls_goodness_of_fit_ref 1.092 _refine_ls_restrained_S_all 1.092 _refine_ls_shift/su_max 0.001 _refine_ls_shift/su_mean 0.000 loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_occupancy _atom_site_symmetry_multiplicity _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group Mo1 Mo 0.29341(3) 0.69181(2) 0.269459(18) 0.00671(9) Uani 1 1 d . . . Cu1 Cu 0.34192(4) 0.31743(3) 0.08144(3) 0.01101(11) Uani 1 1 d . . . Cu2 Cu 0.78773(4) 0.66216(3) 0.52884(3) 0.01061(11) Uani 1 1 d . . . N1 N 0.5196(3) 0.2484(3) 0.1630(2) 0.0193(7) Uani 1 1 d . . . H1A H 0.5969 0.2914 0.1583 0.023 Uiso 1 1 calc R . . H1B H 0.5177 0.2485 0.2256 0.023 Uiso 1 1 calc R . . N2 N 0.4045(3) 0.3713(2) -0.0464(2) 0.0180(6) Uani 1 1 d . . . H2A H 0.3748 0.4415 -0.0636 0.022 Uiso 1 1 calc R . . H2B H 0.4988 0.3745 -0.0358 0.022 Uiso 1 1 calc R . . N3 N 0.1299(3) 0.3090(2) 0.0655(2) 0.0163(6) Uani 1 1 d . . . H3A H 0.1104 0.3398 0.1183 0.020 Uiso 1 1 calc R . . H3B H 0.0879 0.3487 0.0139 0.020 Uiso 1 1 calc R . . N4 N 0.3010(3) 0.1607(2) 0.0100(2) 0.0204(7) Uani 1 1 d . . . N5 N 0.3695(3) 0.4628(2) 0.1579(2) 0.0153(6) Uani 1 1 d . . . N6 N 0.9196(3) 0.6287(2) 0.4468(2) 0.0175(6) Uani 1 1 d . . . H6A H 1.0075 0.6248 0.4843 0.021 Uiso 1 1 calc R . . H6B H 0.8925 0.5606 0.4144 0.021 Uiso 1 1 calc R . . N7 N 0.7987(3) 0.8240(2) 0.47891(19) 0.0136(6) Uani 1 1 d . . . H7 H 0.7181 0.8321 0.4322 0.016 Uiso 1 1 calc R . . N8 N 0.7204(3) 0.7403(2) 0.6339(2) 0.0217(7) Uani 1 1 d . . . H8A H 0.6408 0.7023 0.6404 0.026 Uiso 1 1 calc R . . H8B H 0.7859 0.7385 0.6905 0.026 Uiso 1 1 calc R . . N9 N 0.1987(3) 0.4827(2) 0.3989(2) 0.0150(6) Uani 1 1 d . . . N10 N 0.5432(3) 0.9040(3) 0.2994(2) 0.0219(7) Uani 1 1 d . . . N11 N 0.2872(3) 0.8004(2) 0.4831(2) 0.0206(7) Uani 1 1 d . . . N12 N 0.5861(3) 0.6133(2) 0.4186(2) 0.0140(6) Uani 1 1 d . . . N13 N 0.0994(3) 0.9182(3) 0.2309(2) 0.0211(7) Uani 1 1 d . . . N14 N 0.2952(3) 0.7581(3) 0.0454(2) 0.0201(7) Uani 1 1 d . . . N15 N -0.0154(3) 0.5816(2) 0.1362(2) 0.0195(7) Uani 1 1 d . . . C1 C 0.5247(4) 0.1276(3) 0.1272(3) 0.0212(8) Uani 1 1 d . . . H1C H 0.5681 0.0807 0.1806 0.025 Uiso 1 1 calc R . . H1D H 0.5806 0.1273 0.0804 0.025 Uiso 1 1 calc R . . C2 C 0.3764(4) 0.0780(3) 0.0808(3) 0.0258(9) Uani 1 1 d . . . H2C H 0.3794 0.0049 0.0478 0.031 Uiso 1 1 calc R . . H2D H 0.3262 0.0639 0.1302 0.031 Uiso 1 1 calc R . . C3 C 0.3378(4) 0.2837(3) -0.1223(3) 0.0251(9) Uani 1 1 d . . . H3C H 0.3820 0.2895 -0.1756 0.030 Uiso 1 1 calc R . . H3D H 0.2387 0.2958 -0.1467 0.030 Uiso 1 1 calc R . . C4 C 0.3549(4) 0.1661(3) -0.0793(3) 0.0250(9) Uani 1 1 d . . . H4A H 0.3034 0.1075 -0.1265 0.030 Uiso 1 1 calc R . . H4B H 0.4535 0.1503 -0.0631 0.030 Uiso 1 1 calc R . . C5 C 0.0783(4) 0.1863(3) 0.0520(3) 0.0266(9) Uani 1 1 d . . . H5A H -0.0232 0.1792 0.0275 0.032 Uiso 1 1 calc R . . H5B H 0.1030 0.1478 0.1131 0.032 Uiso 1 1 calc R . . C6 C 0.1460(4) 0.1329(3) -0.0187(3) 0.0305(9) Uani 1 1 d . . . H6C H 0.1262 0.0498 -0.0216 0.037 Uiso 1 1 calc R . . H6D H 0.1071 0.1617 -0.0825 0.037 Uiso 1 1 calc R . . C7 C 0.9163(4) 0.7226(3) 0.3784(3) 0.0199(8) Uani 1 1 d . . . H7A H 0.8321 0.7120 0.3254 0.024 Uiso 1 1 calc R . . H7B H 0.9978 0.7229 0.3520 0.024 Uiso 1 1 calc R . . C8 C 0.9170(4) 0.8350(3) 0.4331(3) 0.0196(8) Uani 1 1 d . . . H8C H 1.0053 0.8495 0.4818 0.023 Uiso 1 1 calc R . . H8D H 0.9056 0.8986 0.3892 0.023 Uiso 1 1 calc R . . C9 C 0.8022(4) 0.9069(3) 0.5589(3) 0.0214(8) Uani 1 1 d . . . H9A H 0.7805 0.9826 0.5340 0.026 Uiso 1 1 calc R . . H9B H 0.8949 0.9134 0.6035 0.026 Uiso 1 1 calc R . . C10 C 0.6934(4) 0.8616(3) 0.6097(3) 0.0254(9) Uani 1 1 d . . . H10A H 0.7006 0.9077 0.6681 0.030 Uiso 1 1 calc R . . H10B H 0.5996 0.8655 0.5678 0.030 Uiso 1 1 calc R . . C11 C 0.3490(3) 0.5430(3) 0.1986(2) 0.0105(7) Uani 1 1 d . . . C12 C 0.4851(3) 0.6394(3) 0.3649(2) 0.0102(7) Uani 1 1 d . . . C13 C 0.2249(3) 0.5549(3) 0.3515(2) 0.0119(7) Uani 1 1 d . . . C14 C 0.4538(3) 0.8311(3) 0.2856(2) 0.0137(7) Uani 1 1 d . . . C15 C 0.2880(3) 0.7650(3) 0.4077(2) 0.0130(7) Uani 1 1 d . . . C16 C 0.1662(3) 0.8389(3) 0.2439(2) 0.0128(7) Uani 1 1 d . . . C17 C 0.2967(3) 0.7373(3) 0.1237(2) 0.0120(7) Uani 1 1 d . . . C18 C 0.0900(3) 0.6216(3) 0.1840(2) 0.0113(7) Uani 1 1 d . . . O1 O 0.4272(2) 0.6435(2) 0.62644(17) 0.0205(6) Uani 1 1 d . . . H1E H 0.3985 0.6716 0.5757 0.025 Uiso 1 1 d R . . H1F H 0.4326 0.5796 0.6019 0.025 Uiso 1 1 d R . . O2 O 0.7593(3) 0.4116(2) 0.10704(18) 0.0281(6) Uani 1 1 d . . . H2E H 0.7863 0.4331 0.0578 0.034 Uiso 1 1 d R . . H2F H 0.8186 0.4097 0.1616 0.034 Uiso 1 1 d R . . O3 O 0.8830(3) 0.0717(2) 0.20642(19) 0.0303(6) Uani 1 1 d . . . H3E H 0.8407 0.0740 0.2588 0.036 Uiso 1 1 d R . . H3F H 0.9418 0.0166 0.2076 0.036 Uiso 1 1 d R . . O4 O 0.7492(3) 0.0881(2) 0.34834(18) 0.0312(7) Uani 1 1 d . . . H4F H 0.6797 0.0327 0.3305 0.037 Uiso 1 1 d R . . H4E H 0.7354 0.1299 0.3949 0.037 Uiso 1 1 d R . . O5 O 0.0068(4) 0.7083(3) 0.7651(2) 0.0479(8) Uani 1 1 d D . . H5C H -0.0008 0.7855 0.7576 0.072 Uiso 1 1 d RD . . H5F H 0.0741 0.7594 0.7856 0.072 Uiso 1 1 d R . . O6 O 0.8535(4) 0.3961(3) 0.3593(4) 0.1017(19) Uani 1 1 d . . . H6F H 0.7972 0.3369 0.3572 0.153 Uiso 1 1 d R . . H6E H 0.9094 0.3834 0.3244 0.153 Uiso 1 1 d R . . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 Mo1 0.00755(14) 0.00573(14) 0.00656(15) 0.00006(10) 0.00113(10) 0.00108(10) Cu1 0.0106(2) 0.0096(2) 0.0127(2) -0.00372(16) 0.00264(16) 0.00237(16) Cu2 0.0107(2) 0.0102(2) 0.0111(2) 0.00294(16) 0.00287(16) 0.00021(16) N1 0.0189(16) 0.0263(17) 0.0133(15) 0.0000(13) 0.0034(12) 0.0100(13) N2 0.0178(15) 0.0198(16) 0.0186(16) 0.0014(13) 0.0072(12) 0.0062(13) N3 0.0151(15) 0.0182(15) 0.0160(15) 0.0010(12) 0.0032(12) 0.0067(12) N4 0.0147(15) 0.0158(15) 0.0305(18) -0.0086(13) 0.0060(13) 0.0012(13) N5 0.0158(15) 0.0144(15) 0.0151(15) -0.0018(12) 0.0022(12) 0.0030(12) N6 0.0153(15) 0.0159(15) 0.0236(16) 0.0024(13) 0.0086(13) 0.0028(12) N7 0.0118(14) 0.0141(14) 0.0141(15) -0.0004(12) 0.0020(11) 0.0009(12) N8 0.0271(17) 0.0215(16) 0.0174(16) -0.0003(13) 0.0087(13) -0.0042(14) N9 0.0141(15) 0.0154(15) 0.0151(15) 0.0037(13) 0.0027(12) 0.0010(12) N10 0.0232(17) 0.0154(16) 0.0231(17) 0.0037(13) 0.0002(13) -0.0053(14) N11 0.0300(18) 0.0180(16) 0.0146(16) -0.0003(13) 0.0047(13) 0.0120(14) N12 0.0115(15) 0.0123(14) 0.0158(15) -0.0012(12) -0.0010(12) 0.0020(12) N13 0.0246(17) 0.0172(16) 0.0192(16) -0.0025(13) -0.0005(13) 0.0101(14) N14 0.0225(16) 0.0217(16) 0.0161(17) 0.0044(13) 0.0053(13) 0.0002(13) N15 0.0167(16) 0.0189(16) 0.0202(16) 0.0040(13) -0.0004(13) 0.0011(13) C1 0.028(2) 0.0191(19) 0.0192(19) 0.0063(15) 0.0068(16) 0.0166(16) C2 0.033(2) 0.0141(18) 0.037(2) 0.0019(17) 0.0214(19) 0.0021(17) C3 0.022(2) 0.037(2) 0.0170(19) -0.0027(17) 0.0047(16) 0.0108(18) C4 0.0208(19) 0.028(2) 0.026(2) -0.0113(17) 0.0052(16) 0.0051(17) C5 0.0157(19) 0.022(2) 0.044(2) -0.0040(18) 0.0134(17) -0.0043(16) C6 0.020(2) 0.027(2) 0.044(3) -0.0137(19) 0.0092(18) -0.0082(17) C7 0.0181(18) 0.0229(19) 0.0212(19) 0.0050(15) 0.0099(15) -0.0002(15) C8 0.0183(18) 0.0156(18) 0.026(2) 0.0073(15) 0.0083(15) -0.0012(15) C9 0.027(2) 0.0097(17) 0.027(2) -0.0032(15) 0.0086(16) -0.0037(15) C10 0.032(2) 0.0186(19) 0.028(2) -0.0108(16) 0.0125(17) 0.0011(17) C11 0.0111(16) 0.0111(16) 0.0095(16) 0.0048(14) 0.0026(13) 0.0008(13) C12 0.0123(17) 0.0068(15) 0.0126(17) 0.0000(13) 0.0057(14) -0.0008(13) C13 0.0079(16) 0.0134(17) 0.0123(17) -0.0025(14) -0.0011(13) 0.0012(13) C14 0.0158(18) 0.0136(17) 0.0122(17) 0.0054(14) 0.0034(14) 0.0048(15) C15 0.0143(17) 0.0072(16) 0.0161(18) 0.0031(14) 0.0007(14) 0.0030(13) C16 0.0143(17) 0.0164(18) 0.0067(16) -0.0034(13) 0.0012(13) 0.0001(15) C17 0.0114(16) 0.0097(16) 0.0144(19) 0.0004(14) 0.0024(13) -0.0002(13) C18 0.0141(17) 0.0099(16) 0.0104(17) 0.0020(13) 0.0035(14) 0.0033(14) O1 0.0254(14) 0.0193(13) 0.0177(13) 0.0035(10) 0.0054(11) 0.0082(11) O2 0.0249(14) 0.0354(16) 0.0209(14) 0.0010(12) 0.0022(11) -0.0055(12) O3 0.0321(15) 0.0303(15) 0.0344(16) 0.0017(13) 0.0174(13) 0.0107(13) O4 0.0354(16) 0.0329(16) 0.0276(15) -0.0208(12) 0.0180(12) -0.0157(13) O5 0.078(2) 0.0291(17) 0.0361(18) -0.0038(14) 0.0181(17) -0.0110(16) O6 0.066(3) 0.044(2) 0.224(6) -0.066(3) 0.103(3) -0.031(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 C14 2.152(4) . ? Mo1 C15 2.155(3) . ? Mo1 C11 2.160(3) . ? Mo1 C12 2.161(3) . ? Mo1 C13 2.163(3) . ? Mo1 C18 2.165(3) . ? Mo1 C16 2.165(3) . ? Mo1 C17 2.168(3) . ? Cu1 N5 1.962(3) . ? Cu1 N4 2.038(3) . ? Cu1 N3 2.038(3) . ? Cu1 N1 2.060(3) . ? Cu1 N2 2.163(3) . ? Cu2 N9 1.982(3) 2_666 ? Cu2 N6 2.010(3) . ? Cu2 N8 2.016(3) . ? Cu2 N7 2.026(3) . ? Cu2 N12 2.234(3) . ? N1 C1 1.494(4) . ? N1 H1A 0.9000 . ? N1 H1B 0.9000 . ? N2 C3 1.470(5) . ? N2 H2A 0.9000 . ? N2 H2B 0.9000 . ? N3 C5 1.473(4) . ? N3 H3A 0.9000 . ? N3 H3B 0.9000 . ? N4 C6 1.488(5) . ? N4 C2 1.497(5) . ? N4 C4 1.506(5) . ? N5 C11 1.146(4) . ? N6 C7 1.473(4) . ? N6 H6A 0.9000 . ? N6 H6B 0.9000 . ? N7 C8 1.475(4) . ? N7 C9 1.476(4) . ? N7 H7 0.9100 . ? N8 C10 1.480(5) . ? N8 H8A 0.9000 . ? N8 H8B 0.9000 . ? N9 C13 1.144(4) . ? N9 Cu2 1.982(3) 2_666 ? N10 C14 1.157(4) . ? N11 C15 1.152(4) . ? N12 C12 1.154(4) . ? N13 C16 1.157(4) . ? N14 C17 1.147(4) . ? N15 C18 1.152(4) . ? C1 C2 1.514(5) . ? C1 H1C 0.9700 . ? C1 H1D 0.9700 . ? C2 H2C 0.9700 . ? C2 H2D 0.9700 . ? C3 C4 1.509(5) . ? C3 H3C 0.9700 . ? C3 H3D 0.9700 . ? C4 H4A 0.9700 . ? C4 H4B 0.9700 . ? C5 C6 1.494(5) . ? C5 H5A 0.9700 . ? C5 H5B 0.9700 . ? C6 H6C 0.9700 . ? C6 H6D 0.9700 . ? C7 C8 1.509(5) . ? C7 H7A 0.9700 . ? C7 H7B 0.9700 . ? C8 H8C 0.9700 . ? C8 H8D 0.9700 . ? C9 C10 1.512(5) . ? C9 H9A 0.9700 . ? C9 H9B 0.9700 . ? C10 H10A 0.9700 . ? C10 H10B 0.9700 . ? O1 H1E 0.7926 . ? O1 H1F 0.8262 . ? O2 H2E 0.8499 . ? O2 H2F 0.8503 . ? O3 H3E 0.9463 . ? O3 H3F 0.8881 . ? O4 H4F 0.8927 . ? O4 H4E 0.8613 . ? O5 H5C 0.9107 . ? O5 H5F 0.8500 . ? O6 H6F 0.8500 . ? O6 H6E 0.8499 . ? 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 C14 Mo1 C15 79.81(13) . . ? C14 Mo1 C11 110.59(12) . . ? C15 Mo1 C11 143.91(11) . . ? C14 Mo1 C12 71.36(12) . . ? C15 Mo1 C12 76.97(12) . . ? C11 Mo1 C12 74.36(12) . . ? C14 Mo1 C13 140.32(12) . . ? C15 Mo1 C13 72.13(12) . . ? C11 Mo1 C13 79.73(12) . . ? C12 Mo1 C13 75.33(12) . . ? C14 Mo1 C18 145.24(12) . . ? C15 Mo1 C18 113.57(12) . . ? C11 Mo1 C18 78.14(12) . . ? C12 Mo1 C18 141.31(12) . . ? C13 Mo1 C18 73.39(12) . . ? C14 Mo1 C16 79.17(12) . . ? C15 Mo1 C16 71.94(12) . . ? C11 Mo1 C16 142.78(11) . . ? C12 Mo1 C16 140.23(12) . . ? C13 Mo1 C16 116.37(12) . . ? C18 Mo1 C16 75.45(12) . . ? C14 Mo1 C17 74.46(12) . . ? C15 Mo1 C17 142.65(12) . . ? C11 Mo1 C17 71.87(12) . . ? C12 Mo1 C17 118.27(12) . . ? C13 Mo1 C17 142.35(12) . . ? C18 Mo1 C17 76.93(12) . . ? C16 Mo1 C17 76.94(12) . . ? N5 Cu1 N4 174.49(12) . . ? N5 Cu1 N3 92.11(12) . . ? N4 Cu1 N3 84.07(12) . . ? N5 Cu1 N1 95.13(12) . . ? N4 Cu1 N1 85.36(12) . . ? N3 Cu1 N1 140.14(12) . . ? N5 Cu1 N2 101.78(12) . . ? N4 Cu1 N2 83.43(12) . . ? N3 Cu1 N2 113.76(11) . . ? N1 Cu1 N2 102.99(11) . . ? N9 Cu2 N6 98.19(11) 2_666 . ? N9 Cu2 N8 89.86(12) 2_666 . ? N6 Cu2 N8 157.33(13) . . ? N9 Cu2 N7 168.90(11) 2_666 . ? N6 Cu2 N7 84.50(11) . . ? N8 Cu2 N7 83.86(11) . . ? N9 Cu2 N12 97.97(11) 2_666 . ? N6 Cu2 N12 97.69(11) . . ? N8 Cu2 N12 102.15(12) . . ? N7 Cu2 N12 92.30(11) . . ? C1 N1 Cu1 109.1(2) . . ? C1 N1 H1A 109.9 . . ? Cu1 N1 H1A 109.9 . . ? C1 N1 H1B 109.9 . . ? Cu1 N1 H1B 109.9 . . ? H1A N1 H1B 108.3 . . ? C3 N2 Cu1 105.7(2) . . ? C3 N2 H2A 110.6 . . ? Cu1 N2 H2A 110.6 . . ? C3 N2 H2B 110.6 . . ? Cu1 N2 H2B 110.6 . . ? H2A N2 H2B 108.7 . . ? C5 N3 Cu1 107.6(2) . . ? C5 N3 H3A 110.2 . . ? Cu1 N3 H3A 110.2 . . ? C5 N3 H3B 110.2 . . ? Cu1 N3 H3B 110.2 . . ? H3A N3 H3B 108.5 . . ? C6 N4 C2 112.5(3) . . ? C6 N4 C4 109.1(3) . . ? C2 N4 C4 112.1(3) . . ? C6 N4 Cu1 108.8(2) . . ? C2 N4 Cu1 104.9(2) . . ? C4 N4 Cu1 109.3(2) . . ? C11 N5 Cu1 162.4(3) . . ? C7 N6 Cu2 108.1(2) . . ? C7 N6 H6A 110.1 . . ? Cu2 N6 H6A 110.1 . . ? C7 N6 H6B 110.1 . . ? Cu2 N6 H6B 110.1 . . ? H6A N6 H6B 108.4 . . ? C8 N7 C9 117.0(3) . . ? C8 N7 Cu2 108.31(19) . . ? C9 N7 Cu2 108.2(2) . . ? C8 N7 H7 107.7 . . ? C9 N7 H7 107.7 . . ? Cu2 N7 H7 107.7 . . ? C10 N8 Cu2 110.1(2) . . ? C10 N8 H8A 109.6 . . ? Cu2 N8 H8A 109.6 . . ? C10 N8 H8B 109.6 . . ? Cu2 N8 H8B 109.6 . . ? H8A N8 H8B 108.2 . . ? C13 N9 Cu2 160.2(3) . 2_666 ? C12 N12 Cu2 150.1(2) . . ? N1 C1 C2 109.2(3) . . ? N1 C1 H1C 109.8 . . ? C2 C1 H1C 109.8 . . ? N1 C1 H1D 109.8 . . ? C2 C1 H1D 109.8 . . ? H1C C1 H1D 108.3 . . ? N4 C2 C1 109.8(3) . . ? N4 C2 H2C 109.7 . . ? C1 C2 H2C 109.7 . . ? N4 C2 H2D 109.7 . . ? C1 C2 H2D 109.7 . . ? H2C C2 H2D 108.2 . . ? N2 C3 C4 108.3(3) . . ? N2 C3 H3C 110.0 . . ? C4 C3 H3C 110.0 . . ? N2 C3 H3D 110.0 . . ? C4 C3 H3D 110.0 . . ? H3C C3 H3D 108.4 . . ? N4 C4 C3 110.4(3) . . ? N4 C4 H4A 109.6 . . ? C3 C4 H4A 109.6 . . ? N4 C4 H4B 109.6 . . ? C3 C4 H4B 109.6 . . ? H4A C4 H4B 108.1 . . ? N3 C5 C6 107.4(3) . . ? N3 C5 H5A 110.2 . . ? C6 C5 H5A 110.2 . . ? N3 C5 H5B 110.2 . . ? C6 C5 H5B 110.2 . . ? H5A C5 H5B 108.5 . . ? N4 C6 C5 110.5(3) . . ? N4 C6 H6C 109.5 . . ? C5 C6 H6C 109.5 . . ? N4 C6 H6D 109.5 . . ? C5 C6 H6D 109.5 . . ? H6C C6 H6D 108.1 . . ? N6 C7 C8 107.6(3) . . ? N6 C7 H7A 110.2 . . ? C8 C7 H7A 110.2 . . ? N6 C7 H7B 110.2 . . ? C8 C7 H7B 110.2 . . ? H7A C7 H7B 108.5 . . ? N7 C8 C7 107.2(3) . . ? N7 C8 H8C 110.3 . . ? C7 C8 H8C 110.3 . . ? N7 C8 H8D 110.3 . . ? C7 C8 H8D 110.3 . . ? H8C C8 H8D 108.5 . . ? N7 C9 C10 107.2(3) . . ? N7 C9 H9A 110.3 . . ? C10 C9 H9A 110.3 . . ? N7 C9 H9B 110.3 . . ? C10 C9 H9B 110.3 . . ? H9A C9 H9B 108.5 . . ? N8 C10 C9 107.8(3) . . ? N8 C10 H10A 110.2 . . ? C9 C10 H10A 110.2 . . ? N8 C10 H10B 110.2 . . ? C9 C10 H10B 110.2 . . ? H10A C10 H10B 108.5 . . ? N5 C11 Mo1 175.6(3) . . ? N12 C12 Mo1 177.6(3) . . ? N9 C13 Mo1 174.9(3) . . ? N10 C14 Mo1 176.2(3) . . ? N11 C15 Mo1 177.4(3) . . ? N13 C16 Mo1 179.3(3) . . ? N14 C17 Mo1 177.6(3) . . ? N15 C18 Mo1 177.1(3) . . ? H1E O1 H1F 93.4 . . ? H2E O2 H2F 120.0 . . ? H3E O3 H3F 115.8 . . ? H4F O4 H4E 109.6 . . ? H5C O5 H5F 55.7 . . ? H6F O6 H6E 109.5 . . ? _diffrn_measured_fraction_theta_max 0.980 _diffrn_reflns_theta_full 25.00 _diffrn_measured_fraction_theta_full 0.980 _refine_diff_density_max 1.327 _refine_diff_density_min -1.278 _refine_diff_density_rms 0.090 #===END OF CIF # Attachment '- compound_1-2.cif' data_1 _database_code_depnum_ccdc_archive 'CCDC 773228' #TrackingRef '- compound_1-2.cif' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C20 H43 Cu2 Mo N15 O4' _chemical_formula_weight 780.71 loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Cu Cu 0.3201 1.2651 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Mo Mo -1.6832 0.6857 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting Monoclinic _symmetry_space_group_name_H-M P2(1) loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, y+1/2, -z' _cell_length_a 10.206(2) _cell_length_b 14.185(3) _cell_length_c 10.777(2) _cell_angle_alpha 90.00 _cell_angle_beta 93.69(3) _cell_angle_gamma 90.00 _cell_volume 1557.0(5) _cell_formula_units_Z 2 _cell_measurement_temperature 123(2) _cell_measurement_reflns_used 5685 _cell_measurement_theta_min 3.0 _cell_measurement_theta_max 27.5 _exptl_crystal_description prism _exptl_crystal_colour blue _exptl_crystal_size_max 0.15 _exptl_crystal_size_mid 0.12 _exptl_crystal_size_min 0.12 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.665 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 800 _exptl_absorpt_coefficient_mu 1.804 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.594 _exptl_absorpt_correction_T_max 0.656 _exptl_absorpt_process_details ? _exptl_special_details ; Jacobson, R. (1998) Private communication ; _diffrn_ambient_temperature 123(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'Rigaku Saturn' _diffrn_measurement_method \w _diffrn_detector_area_resol_mean 7.31 _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 10513 _diffrn_reflns_av_R_equivalents 0.0260 _diffrn_reflns_av_sigmaI/netI 0.0446 _diffrn_reflns_limit_h_min -11 _diffrn_reflns_limit_h_max 11 _diffrn_reflns_limit_k_min -16 _diffrn_reflns_limit_k_max 16 _diffrn_reflns_limit_l_min -12 _diffrn_reflns_limit_l_max 12 _diffrn_reflns_theta_min 3.03 _diffrn_reflns_theta_max 24.99 _reflns_number_total 5040 _reflns_number_gt 4761 _reflns_threshold_expression >2sigma(I) _computing_data_collection CrystalClear _computing_cell_refinement CrystalClear _computing_data_reduction CrystalStructure _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics ? _computing_publication_material ? _refine_special_details ; Refinement of F^2^ against ALL reflections. The weighted R-factor wR and goodness of fit S are based on F^2^, conventional R-factors R are based on F, with F set to zero for negative F^2^. The threshold expression of F^2^ > 2sigma(F^2^) is used only for calculating R-factors(gt) etc. and is not relevant to the choice of reflections for refinement. R-factors based on F^2^ are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger. ; _refine_ls_structure_factor_coef Fsqd _refine_ls_matrix_type full _refine_ls_weighting_scheme calc _refine_ls_weighting_details 'calc w=1/[\s^2^(Fo^2^)+(0.0199P)^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_coef ? _refine_ls_abs_structure_details 'Flack H D (1983), Acta Cryst. A39, 876-881' _refine_ls_abs_structure_Flack 0.014(9) _refine_ls_number_reflns 5040 _refine_ls_number_parameters 379 _refine_ls_number_restraints 2 _refine_ls_R_factor_all 0.0231 _refine_ls_R_factor_gt 0.0218 _refine_ls_wR_factor_ref 0.0486 _refine_ls_wR_factor_gt 0.0484 _refine_ls_goodness_of_fit_ref 1.000 _refine_ls_restrained_S_all 1.008 _refine_ls_shift/su_max 0.001 _refine_ls_shift/su_mean 0.000 loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_occupancy _atom_site_symmetry_multiplicity _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group Mo1 Mo 0.19083(2) 0.554568(17) 0.30064(3) 0.00604(7) Uani 1 1 d . . . Cu1 Cu -0.21668(4) 0.34681(3) 0.22702(4) 0.00862(10) Uani 1 1 d . . . Cu2 Cu 0.11748(4) 0.32902(3) 0.66963(4) 0.00931(10) Uani 1 1 d . . . N1 N -0.2630(2) 0.3347(2) 0.0357(2) 0.0135(6) Uani 1 1 d . . . H1A H -0.2800 0.3918 0.0020 0.016 Uiso 1 1 calc R . . H1B H -0.1959 0.3085 -0.0021 0.016 Uiso 1 1 calc R . . N2 N -0.3536(3) 0.4062(2) 0.3360(3) 0.0172(7) Uani 1 1 d . . . H2A H -0.3142 0.4448 0.3932 0.021 Uiso 1 1 calc R . . H2B H -0.4128 0.4397 0.2888 0.021 Uiso 1 1 calc R . . N3 N -0.0627(3) 0.2625(2) 0.2994(3) 0.0147(7) Uani 1 1 d . . . H3A H 0.0107 0.2740 0.2598 0.018 Uiso 1 1 calc R . . H3B H -0.0461 0.2743 0.3809 0.018 Uiso 1 1 calc R . . N4 N -0.3273(2) 0.2268(2) 0.2391(2) 0.0096(6) Uani 1 1 d . . . N5 N -0.0964(3) 0.4550(2) 0.2249(3) 0.0137(6) Uani 1 1 d . . . N6 N 0.2776(3) 0.2962(2) 0.5845(3) 0.0168(7) Uani 1 1 d . . . H6A H 0.2613 0.3078 0.5029 0.020 Uiso 1 1 calc R . . H6B H 0.3417 0.3360 0.6121 0.020 Uiso 1 1 calc R . . N7 N 0.2021(3) 0.2815(3) 0.8342(3) 0.0318(9) Uani 1 1 d . . . H7 H 0.1403 0.2419 0.8620 0.048 Uiso 1 1 d R . . N8 N -0.0355(3) 0.3697(2) 0.7620(3) 0.0151(7) Uani 1 1 d . . . H8A H -0.0964 0.3953 0.7080 0.018 Uiso 1 1 calc R . . H8B H -0.0715 0.3186 0.7960 0.018 Uiso 1 1 calc R . . N9 N 0.1021(3) 0.4447(2) 0.5520(2) 0.0114(6) Uani 1 1 d . . . N10 N 0.2394(3) 0.3245(2) 0.2730(3) 0.0150(6) Uani 1 1 d . . . N11 N -0.0001(3) 0.7143(2) 0.4184(3) 0.0140(6) Uani 1 1 d . . . N12 N 0.4533(3) 0.5320(2) 0.4955(3) 0.0151(7) Uani 1 1 d . . . N13 N 0.4252(3) 0.5234(2) 0.1044(3) 0.0165(7) Uani 1 1 d . . . N14 N 0.0686(3) 0.6730(2) 0.0546(3) 0.0151(7) Uani 1 1 d . . . N15 N 0.3363(3) 0.7631(2) 0.2993(3) 0.0165(7) Uani 1 1 d . . . C1 C -0.3809(3) 0.2737(3) 0.0218(3) 0.0160(8) Uani 1 1 d . . . H1C H -0.3932 0.2511 -0.0631 0.019 Uiso 1 1 calc R . . H1D H -0.4583 0.3092 0.0411 0.019 Uiso 1 1 calc R . . C2 C -0.3614(3) 0.1911(2) 0.1103(3) 0.0154(8) Uani 1 1 d . . . H2C H -0.4412 0.1539 0.1095 0.018 Uiso 1 1 calc R . . H2D H -0.2914 0.1511 0.0840 0.018 Uiso 1 1 calc R . . C3 C -0.4181(3) 0.3274(2) 0.3969(3) 0.0143(8) Uani 1 1 d . . . H3C H -0.4986 0.3490 0.4308 0.017 Uiso 1 1 calc R . . H3D H -0.3607 0.3028 0.4645 0.017 Uiso 1 1 calc R . . C4 C -0.4483(3) 0.2515(2) 0.3015(3) 0.0140(8) Uani 1 1 d . . . H4A H -0.4818 0.1961 0.3416 0.017 Uiso 1 1 calc R . . H4B H -0.5151 0.2736 0.2402 0.017 Uiso 1 1 calc R . . C5 C -0.1048(3) 0.1639(2) 0.2800(3) 0.0152(8) Uani 1 1 d . . . H5A H -0.0502 0.1223 0.3327 0.018 Uiso 1 1 calc R . . H5B H -0.0966 0.1458 0.1941 0.018 Uiso 1 1 calc R . . C6 C -0.2461(3) 0.1565(2) 0.3123(3) 0.0122(7) Uani 1 1 d . . . H6C H -0.2786 0.0934 0.2939 0.015 Uiso 1 1 calc R . . H6D H -0.2522 0.1679 0.4005 0.015 Uiso 1 1 calc R . . C7 C 0.3297(4) 0.1994(3) 0.5970(4) 0.0282(10) Uani 1 1 d . . . H7A H 0.2810 0.1592 0.5376 0.034 Uiso 1 1 calc R . . H7B H 0.4206 0.1996 0.5758 0.034 Uiso 1 1 calc R . . C8 C 0.3227(5) 0.1588(3) 0.7219(4) 0.0425(12) Uani 1 1 d D . . H8C H 0.2459 0.1184 0.7201 0.051 Uiso 1 1 calc R . . H8D H 0.3988 0.1185 0.7371 0.051 Uiso 1 1 calc R . . C9 C 0.3167(5) 0.2209(4) 0.8279(4) 0.0501(14) Uani 1 1 d D . . H9A H 0.3938 0.2610 0.8307 0.060 Uiso 1 1 calc R . . H9B H 0.3230 0.1823 0.9024 0.060 Uiso 1 1 calc R . . C10 C 0.2130(4) 0.3535(3) 0.9290(3) 0.0288(10) Uani 1 1 d . . . H10A H 0.2714 0.4022 0.9019 0.035 Uiso 1 1 calc R . . H10B H 0.2544 0.3257 1.0039 0.035 Uiso 1 1 calc R . . C11 C 0.0906(5) 0.3983(4) 0.9613(5) 0.0506(14) Uani 1 1 d . . . H11A H 0.1137 0.4485 1.0199 0.061 Uiso 1 1 calc R . . H11B H 0.0414 0.3519 1.0054 0.061 Uiso 1 1 calc R . . C12 C -0.0005(3) 0.4391(3) 0.8618(3) 0.0197(8) Uani 1 1 d . . . H12A H -0.0799 0.4604 0.8980 0.024 Uiso 1 1 calc R . . H12B H 0.0407 0.4935 0.8259 0.024 Uiso 1 1 calc R . . C13 C 0.0024(3) 0.4926(2) 0.2464(3) 0.0120(7) Uani 1 1 d . . . C14 C 0.1298(3) 0.4873(2) 0.4678(3) 0.0086(7) Uani 1 1 d . . . C15 C 0.2258(3) 0.4050(2) 0.2790(3) 0.0087(7) Uani 1 1 d . . . C16 C 0.0659(3) 0.6562(2) 0.3818(3) 0.0092(7) Uani 1 1 d . . . C17 C 0.3631(3) 0.5406(2) 0.4269(3) 0.0104(7) Uani 1 1 d . . . C18 C 0.3420(3) 0.5352(2) 0.1689(3) 0.0105(8) Uani 1 1 d . . . C19 C 0.1114(3) 0.6277(2) 0.1363(3) 0.0096(7) Uani 1 1 d . . . C20 C 0.2901(3) 0.6897(2) 0.3019(3) 0.0102(7) Uani 1 1 d . . . O1 O 0.6178(2) 0.51052(18) 0.9204(2) 0.0196(6) Uani 1 1 d . . . H1E H 0.5646 0.5175 0.9814 0.029 Uiso 1 1 d R . . H1F H 0.5725 0.4860 0.8591 0.029 Uiso 1 1 d R . . O2 O 0.2337(3) 0.11843(19) 0.2522(3) 0.0307(7) Uani 1 1 d . . . H2E H 0.2505 0.1831 0.2537 0.046 Uiso 1 1 d R . . H2F H 0.2855 0.0827 0.1965 0.046 Uiso 1 1 d R . . O3 O 0.5006(2) 0.92207(17) 0.2874(2) 0.0198(6) Uani 1 1 d . . . H3E H 0.5059 0.9619 0.3519 0.030 Uiso 1 1 d R . . H3F H 0.4494 0.8764 0.3104 0.030 Uiso 1 1 d R . . O4 O 0.8016(2) 0.48604(19) 0.5632(2) 0.0267(6) Uani 1 1 d . . . H4F H 0.8043 0.5369 0.6163 0.040 Uiso 1 1 d R . . H4E H 0.8821 0.4968 0.5437 0.040 Uiso 1 1 d R . . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 Mo1 0.00586(13) 0.00557(14) 0.00675(13) 0.00036(13) 0.00090(10) -0.00059(13) Cu1 0.00729(19) 0.0082(2) 0.0103(2) -0.00011(17) -0.00027(16) -0.00179(17) Cu2 0.0086(2) 0.0110(2) 0.0084(2) 0.00079(16) 0.00089(16) 0.00058(16) N1 0.0164(14) 0.0148(16) 0.0095(14) -0.0008(13) 0.0021(11) -0.0003(13) N2 0.0172(16) 0.0116(16) 0.0231(18) -0.0048(13) 0.0041(14) -0.0004(13) N3 0.0117(15) 0.0145(17) 0.0174(16) 0.0032(13) -0.0012(13) -0.0021(13) N4 0.0084(14) 0.0118(15) 0.0087(15) -0.0001(12) 0.0004(11) -0.0012(12) N5 0.0099(16) 0.0111(15) 0.0202(17) 0.0038(13) 0.0008(13) 0.0022(13) N6 0.0124(15) 0.0249(18) 0.0132(15) 0.0043(13) 0.0019(12) 0.0062(13) N7 0.041(2) 0.041(2) 0.0124(17) -0.0017(17) -0.0069(15) 0.0235(18) N8 0.0153(15) 0.0171(17) 0.0134(15) 0.0007(13) 0.0038(12) -0.0005(13) N9 0.0105(15) 0.0131(15) 0.0113(16) 0.0028(13) 0.0061(12) -0.0006(12) N10 0.0100(14) 0.0143(17) 0.0210(17) -0.0011(13) 0.0044(12) 0.0018(12) N11 0.0160(16) 0.0143(16) 0.0112(16) 0.0007(13) -0.0028(12) 0.0029(14) N12 0.0150(15) 0.0180(18) 0.0122(15) -0.0006(12) 0.0003(13) 0.0002(12) N13 0.0154(16) 0.0215(18) 0.0136(16) -0.0019(13) 0.0095(13) 0.0001(13) N14 0.0125(15) 0.0150(16) 0.0179(17) 0.0030(13) 0.0017(13) 0.0022(13) N15 0.0178(16) 0.0152(18) 0.0167(17) -0.0028(13) 0.0031(13) -0.0034(14) C1 0.0119(17) 0.028(2) 0.0085(18) -0.0057(16) 0.0003(14) -0.0041(16) C2 0.0137(18) 0.0161(19) 0.0162(19) -0.0043(15) 0.0003(15) -0.0026(15) C3 0.0138(17) 0.0150(19) 0.0151(18) -0.0011(15) 0.0086(14) 0.0033(15) C4 0.0122(18) 0.018(2) 0.0120(18) -0.0008(15) 0.0068(15) -0.0026(15) C5 0.0162(19) 0.0135(19) 0.0158(19) 0.0042(15) 0.0004(15) 0.0018(16) C6 0.0137(18) 0.0096(17) 0.0137(18) 0.0025(14) 0.0040(14) 0.0018(14) C7 0.025(2) 0.026(2) 0.034(2) -0.0066(19) 0.0016(19) 0.0133(18) C8 0.051(3) 0.032(3) 0.047(3) 0.013(2) 0.020(2) 0.027(2) C9 0.076(4) 0.050(3) 0.021(2) -0.003(2) -0.022(2) 0.041(3) C10 0.028(2) 0.039(3) 0.019(2) -0.008(2) -0.0058(17) -0.002(2) C11 0.055(3) 0.051(3) 0.043(3) -0.028(3) -0.015(2) 0.016(3) C12 0.020(2) 0.016(2) 0.024(2) -0.0029(17) 0.0067(17) -0.0035(16) C13 0.0162(19) 0.0091(17) 0.0108(18) 0.0006(14) 0.0016(15) 0.0015(15) C14 0.0052(17) 0.0079(17) 0.0128(18) -0.0051(14) 0.0007(14) 0.0018(13) C15 0.0049(16) 0.0122(19) 0.0094(17) -0.0013(14) 0.0042(13) -0.0006(14) C16 0.0088(17) 0.0119(18) 0.0063(17) 0.0029(14) -0.0040(13) -0.0030(15) C17 0.0096(16) 0.0090(19) 0.0131(17) 0.0013(14) 0.0059(14) -0.0015(14) C18 0.0135(17) 0.005(2) 0.0123(17) -0.0008(13) -0.0052(14) -0.0020(14) C19 0.0122(18) 0.0074(17) 0.0096(17) -0.0034(15) 0.0029(14) -0.0046(14) C20 0.0081(17) 0.0123(19) 0.0103(18) -0.0029(14) 0.0012(14) 0.0005(15) O1 0.0198(14) 0.0242(14) 0.0154(14) -0.0026(11) 0.0057(11) 0.0017(11) O2 0.0382(17) 0.0119(15) 0.0437(19) 0.0010(13) 0.0168(15) -0.0009(13) O3 0.0254(14) 0.0174(14) 0.0165(14) -0.0012(11) 0.0010(11) -0.0106(12) O4 0.0172(14) 0.0314(16) 0.0314(16) -0.0070(13) 0.0014(12) 0.0010(12) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag Mo1 C16 2.148(4) . ? Mo1 C13 2.160(4) . ? Mo1 C17 2.162(3) . ? Mo1 C19 2.165(4) . ? Mo1 C14 2.165(3) . ? Mo1 C15 2.166(3) . ? Mo1 C20 2.168(4) . ? Mo1 C18 2.180(3) . ? Cu1 N5 1.966(3) . ? Cu1 N4 2.051(3) . ? Cu1 N2 2.062(3) . ? Cu1 N3 2.086(3) . ? Cu1 N1 2.092(3) . ? Cu2 N6 1.981(3) . ? Cu2 N8 1.990(3) . ? Cu2 N7 2.037(3) . ? Cu2 N9 2.073(3) . ? Cu2 N11 2.199(3) 2_546 ? N1 C1 1.482(4) . ? N1 H1A 0.9000 . ? N1 H1B 0.9000 . ? N2 C3 1.473(4) . ? N2 H2A 0.9000 . ? N2 H2B 0.9000 . ? N3 C5 1.474(4) . ? N3 H3A 0.9000 . ? N3 H3B 0.9000 . ? N4 C4 1.485(4) . ? N4 C6 1.490(4) . ? N4 C2 1.497(4) . ? N5 C13 1.152(4) . ? N6 C7 1.475(5) . ? N6 H6A 0.9000 . ? N6 H6B 0.9000 . ? N7 C10 1.444(5) . ? N7 C9 1.456(5) . ? N7 H7 0.9100 . ? N8 C12 1.486(4) . ? N8 H8A 0.9000 . ? N8 H8B 0.9000 . ? N9 C14 1.141(4) . ? N10 C15 1.154(4) . ? N11 C16 1.150(4) . ? N11 Cu2 2.199(3) 2_556 ? N12 C17 1.150(4) . ? N13 C18 1.145(4) . ? N14 C19 1.153(4) . ? N15 C20 1.145(4) . ? C1 C2 1.515(5) . ? C1 H1C 0.9700 . ? C1 H1D 0.9700 . ? C2 H2C 0.9700 . ? C2 H2D 0.9700 . ? C3 C4 1.507(5) . ? C3 H3C 0.9700 . ? C3 H3D 0.9700 . ? C4 H4A 0.9700 . ? C4 H4B 0.9700 . ? C5 C6 1.509(4) . ? C5 H5A 0.9700 . ? C5 H5B 0.9700 . ? C6 H6C 0.9700 . ? C6 H6D 0.9700 . ? C7 C8 1.470(5) . ? C7 H7A 0.9700 . ? C7 H7B 0.9700 . ? C8 C9 1.447(5) . ? C8 H8C 0.9700 . ? C8 H8D 0.9700 . ? C9 H9A 0.9700 . ? C9 H9B 0.9700 . ? C10 C11 1.464(6) . ? C10 H10A 0.9700 . ? C10 H10B 0.9700 . ? C11 C12 1.490(6) . ? C11 H11A 0.9700 . ? C11 H11B 0.9700 . ? C12 H12A 0.9700 . ? C12 H12B 0.9700 . ? O1 H1E 0.8844 . ? O1 H1F 0.8556 . ? O2 H2E 0.9334 . ? O2 H2F 0.9679 . ? O3 H3E 0.8950 . ? O3 H3F 0.8784 . ? O4 H4F 0.9198 . ? O4 H4E 0.8739 . ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag C16 Mo1 C13 80.90(12) . . ? C16 Mo1 C17 106.58(12) . . ? C13 Mo1 C17 143.77(12) . . ? C16 Mo1 C19 79.05(12) . . ? C13 Mo1 C19 72.15(12) . . ? C17 Mo1 C19 143.67(12) . . ? C16 Mo1 C14 75.34(12) . . ? C13 Mo1 C14 75.36(12) . . ? C17 Mo1 C14 72.64(11) . . ? C19 Mo1 C14 141.19(12) . . ? C16 Mo1 C15 143.85(12) . . ? C13 Mo1 C15 73.87(12) . . ? C17 Mo1 C15 81.10(12) . . ? C19 Mo1 C15 115.90(12) . . ? C14 Mo1 C15 73.53(11) . . ? C16 Mo1 C20 72.15(12) . . ? C13 Mo1 C20 140.26(12) . . ? C17 Mo1 C20 73.51(12) . . ? C19 Mo1 C20 74.43(12) . . ? C14 Mo1 C20 122.94(12) . . ? C15 Mo1 C20 141.85(13) . . ? C16 Mo1 C18 144.40(12) . . ? C13 Mo1 C18 115.32(12) . . ? C17 Mo1 C18 79.47(11) . . ? C19 Mo1 C18 76.79(12) . . ? C14 Mo1 C18 137.72(12) . . ? C15 Mo1 C18 71.23(12) . . ? C20 Mo1 C18 76.42(12) . . ? N5 Cu1 N4 174.25(11) . . ? N5 Cu1 N2 97.73(12) . . ? N4 Cu1 N2 84.64(11) . . ? N5 Cu1 N3 89.76(11) . . ? N4 Cu1 N3 84.56(11) . . ? N2 Cu1 N3 122.91(12) . . ? N5 Cu1 N1 98.87(12) . . ? N4 Cu1 N1 84.50(11) . . ? N2 Cu1 N1 118.43(11) . . ? N3 Cu1 N1 116.00(12) . . ? N6 Cu2 N8 175.65(13) . . ? N6 Cu2 N7 90.53(13) . . ? N8 Cu2 N7 87.87(13) . . ? N6 Cu2 N9 86.27(11) . . ? N8 Cu2 N9 92.62(11) . . ? N7 Cu2 N9 143.66(14) . . ? N6 Cu2 N11 93.96(12) . 2_546 ? N8 Cu2 N11 90.39(11) . 2_546 ? N7 Cu2 N11 108.63(14) . 2_546 ? N9 Cu2 N11 107.70(11) . 2_546 ? C1 N1 Cu1 106.15(19) . . ? C1 N1 H1A 110.5 . . ? Cu1 N1 H1A 110.5 . . ? C1 N1 H1B 110.5 . . ? Cu1 N1 H1B 110.5 . . ? H1A N1 H1B 108.7 . . ? C3 N2 Cu1 106.4(2) . . ? C3 N2 H2A 110.4 . . ? Cu1 N2 H2A 110.4 . . ? C3 N2 H2B 110.4 . . ? Cu1 N2 H2B 110.4 . . ? H2A N2 H2B 108.6 . . ? C5 N3 Cu1 106.6(2) . . ? C5 N3 H3A 110.4 . . ? Cu1 N3 H3A 110.4 . . ? C5 N3 H3B 110.4 . . ? Cu1 N3 H3B 110.4 . . ? H3A N3 H3B 108.6 . . ? C4 N4 C6 111.7(3) . . ? C4 N4 C2 110.4(3) . . ? C6 N4 C2 110.6(3) . . ? C4 N4 Cu1 108.1(2) . . ? C6 N4 Cu1 107.43(19) . . ? C2 N4 Cu1 108.53(19) . . ? C13 N5 Cu1 154.0(3) . . ? C7 N6 Cu2 118.7(2) . . ? C7 N6 H6A 107.7 . . ? Cu2 N6 H6A 107.7 . . ? C7 N6 H6B 107.7 . . ? Cu2 N6 H6B 107.7 . . ? H6A N6 H6B 107.1 . . ? C10 N7 C9 115.1(3) . . ? C10 N7 Cu2 113.0(3) . . ? C9 N7 Cu2 116.9(3) . . ? C10 N7 H7 103.1 . . ? C9 N7 H7 103.1 . . ? Cu2 N7 H7 103.1 . . ? C12 N8 Cu2 113.2(2) . . ? C12 N8 H8A 108.9 . . ? Cu2 N8 H8A 108.9 . . ? C12 N8 H8B 108.9 . . ? Cu2 N8 H8B 108.9 . . ? H8A N8 H8B 107.8 . . ? C14 N9 Cu2 153.2(3) . . ? C16 N11 Cu2 134.2(3) . 2_556 ? N1 C1 C2 108.3(3) . . ? N1 C1 H1C 110.0 . . ? C2 C1 H1C 110.0 . . ? N1 C1 H1D 110.0 . . ? C2 C1 H1D 110.0 . . ? H1C C1 H1D 108.4 . . ? N4 C2 C1 109.6(3) . . ? N4 C2 H2C 109.8 . . ? C1 C2 H2C 109.8 . . ? N4 C2 H2D 109.8 . . ? C1 C2 H2D 109.8 . . ? H2C C2 H2D 108.2 . . ? N2 C3 C4 108.4(3) . . ? N2 C3 H3C 110.0 . . ? C4 C3 H3C 110.0 . . ? N2 C3 H3D 110.0 . . ? C4 C3 H3D 110.0 . . ? H3C C3 H3D 108.4 . . ? N4 C4 C3 109.8(3) . . ? N4 C4 H4A 109.7 . . ? C3 C4 H4A 109.7 . . ? N4 C4 H4B 109.7 . . ? C3 C4 H4B 109.7 . . ? H4A C4 H4B 108.2 . . ? N3 C5 C6 107.9(3) . . ? N3 C5 H5A 110.1 . . ? C6 C5 H5A 110.1 . . ? N3 C5 H5B 110.1 . . ? C6 C5 H5B 110.1 . . ? H5A C5 H5B 108.4 . . ? N4 C6 C5 109.8(3) . . ? N4 C6 H6C 109.7 . . ? C5 C6 H6C 109.7 . . ? N4 C6 H6D 109.7 . . ? C5 C6 H6D 109.7 . . ? H6C C6 H6D 108.2 . . ? C8 C7 N6 114.2(3) . . ? C8 C7 H7A 108.7 . . ? N6 C7 H7A 108.7 . . ? C8 C7 H7B 108.7 . . ? N6 C7 H7B 108.7 . . ? H7A C7 H7B 107.6 . . ? C9 C8 C7 119.4(4) . . ? C9 C8 H8C 107.5 . . ? C7 C8 H8C 107.5 . . ? C9 C8 H8D 107.5 . . ? C7 C8 H8D 107.5 . . ? H8C C8 H8D 107.0 . . ? C8 C9 N7 118.1(4) . . ? C8 C9 H9A 107.8 . . ? N7 C9 H9A 107.8 . . ? C8 C9 H9B 107.8 . . ? N7 C9 H9B 107.8 . . ? H9A C9 H9B 107.1 . . ? N7 C10 C11 116.6(3) . . ? N7 C10 H10A 108.2 . . ? C11 C10 H10A 108.2 . . ? N7 C10 H10B 108.2 . . ? C11 C10 H10B 108.2 . . ? H10A C10 H10B 107.3 . . ? C10 C11 C12 120.0(4) . . ? C10 C11 H11A 107.3 . . ? C12 C11 H11A 107.3 . . ? C10 C11 H11B 107.3 . . ? C12 C11 H11B 107.3 . . ? H11A C11 H11B 106.9 . . ? N8 C12 C11 111.9(3) . . ? N8 C12 H12A 109.2 . . ? C11 C12 H12A 109.2 . . ? N8 C12 H12B 109.2 . . ? C11 C12 H12B 109.2 . . ? H12A C12 H12B 107.9 . . ? N5 C13 Mo1 174.8(3) . . ? N9 C14 Mo1 174.0(3) . . ? N10 C15 Mo1 175.9(3) . . ? N11 C16 Mo1 175.5(3) . . ? N12 C17 Mo1 178.6(3) . . ? N13 C18 Mo1 176.7(3) . . ? N14 C19 Mo1 174.6(3) . . ? N15 C20 Mo1 176.1(3) . . ? H1E O1 H1F 107.0 . . ? H2E O2 H2F 114.7 . . ? H3E O3 H3F 104.6 . . ? H4F O4 H4E 91.3 . . ? _diffrn_measured_fraction_theta_max 0.991 _diffrn_reflns_theta_full 24.99 _diffrn_measured_fraction_theta_full 0.991 _refine_diff_density_max 0.829 _refine_diff_density_min -0.407 _refine_diff_density_rms 0.063