# Supplementary Material (ESI) for Journal of Materials Chemistry # This journal is (C) The Royal Society of Chemistry 2009 data_global _journal_name_full J.Mater.Chem. _journal_coden_Cambridge 1145 _journal_volume ? _journal_page_first ? _journal_year ? _publ_contact_author_name 'Slavi Sevov' _publ_contact_author_email SSEVOV@ND.EDU _publ_section_title ; Syntheses, structures, and magnetic properties of heterometallic coordination polymers with carboxyphosphonate linkers ; loop_ _publ_author_name 'Slavi Sevov' 'Zhi-Guo Gu.' # Attachment 'combined.cif' data_1-CuMn _database_code_depnum_ccdc_archive 'CCDC 742512' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C10 H32 Cu2 Mn2 N2 O24 P2' _chemical_formula_weight 863.28 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' Mn Mn 0.3368 0.7283 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting Monoclinic _symmetry_space_group_name_H-M P2(1)/n _symmetry_space_group_name_Hall '-P 2yn' loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x+1/2, y+1/2, -z+1/2' '-x, -y, -z' 'x-1/2, -y-1/2, z-1/2' _cell_length_a 10.1336(5) _cell_length_b 16.7572(8) _cell_length_c 16.2070(8) _cell_angle_alpha 90.00 _cell_angle_beta 95.402(2) _cell_angle_gamma 90.00 _cell_volume 2739.9(2) _cell_formula_units_Z 4 _cell_measurement_temperature 100(2) _cell_measurement_reflns_used 9908 _cell_measurement_theta_min 2.35 _cell_measurement_theta_max 28.38 _exptl_crystal_description block _exptl_crystal_colour blue _exptl_crystal_size_max 0.29 _exptl_crystal_size_mid 0.29 _exptl_crystal_size_min 0.27 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 2.093 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1744 _exptl_absorpt_coefficient_mu 2.653 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.6762 _exptl_absorpt_correction_T_max 0.6917 _exptl_absorpt_process_details 'SADABS; Bruker, 2000' _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 'Bruker Smart Apex CCD' _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 49131 _diffrn_reflns_av_R_equivalents 0.0274 _diffrn_reflns_av_sigmaI/netI 0.0168 _diffrn_reflns_limit_h_min -13 _diffrn_reflns_limit_h_max 13 _diffrn_reflns_limit_k_min -21 _diffrn_reflns_limit_k_max 22 _diffrn_reflns_limit_l_min -21 _diffrn_reflns_limit_l_max 18 _diffrn_reflns_theta_min 2.28 _diffrn_reflns_theta_max 28.41 _reflns_number_total 6807 _reflns_number_gt 6300 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'SMART (Bruker, 2000)' _computing_cell_refinement SMART _computing_data_reduction 'SAINT (Bruker, 2000)' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics SHELXTL _computing_publication_material 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^)+(0.0397P)^2^+12.4545P] 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 6807 _refine_ls_number_parameters 379 _refine_ls_number_restraints 142 _refine_ls_R_factor_all 0.0389 _refine_ls_R_factor_gt 0.0360 _refine_ls_wR_factor_ref 0.0944 _refine_ls_wR_factor_gt 0.0925 _refine_ls_goodness_of_fit_ref 1.035 _refine_ls_restrained_S_all 1.125 _refine_ls_shift/su_max 0.002 _refine_ls_shift/su_mean 0.000 loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_occupancy _atom_site_symmetry_multiplicity _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group Mn1 Mn 1.14457(4) 0.32809(3) 0.08722(3) 0.00944(10) Uani 1 1 d U . . Mn2 Mn 0.93417(4) 0.31244(3) 0.38256(3) 0.00894(10) Uani 1 1 d U . . Cu1 Cu 1.03882(3) 0.10726(2) 0.05715(2) 0.00757(9) Uani 1 1 d . . . Cu2 Cu 0.66335(4) 0.20985(2) 0.24057(2) 0.00930(9) Uani 1 1 d . . . P1 P 0.95634(7) 0.21037(4) 0.19949(5) 0.00800(14) Uani 1 1 d . . . P2 P 0.62336(7) 0.28295(4) 0.41190(5) 0.00853(14) Uani 1 1 d . . . C1 C 1.0857(3) -0.01215(18) 0.17424(19) 0.0101(5) Uani 1 1 d . . . H1A H 1.0597 -0.0578 0.1375 0.012 Uiso 1 1 calc R . . H1B H 1.0901 -0.0308 0.2324 0.012 Uiso 1 1 calc R . . C2 C 0.8492(3) 0.02386(18) 0.14528(18) 0.0099(5) Uani 1 1 d . . . H2A H 0.7989 0.0396 0.1922 0.012 Uiso 1 1 calc R . . H2B H 0.8493 -0.0351 0.1423 0.012 Uiso 1 1 calc R . . C3 C 1.0040(3) 0.11021(17) 0.23115(17) 0.0093(5) Uani 1 1 d . . . H3A H 1.0978 0.1103 0.2546 0.011 Uiso 1 1 calc R . . H3B H 0.9491 0.0925 0.2751 0.011 Uiso 1 1 calc R . . C4 C 1.2203(3) 0.01989(18) 0.15519(18) 0.0101(5) Uani 1 1 d . . . C5 C 0.7809(3) 0.05718(18) 0.06556(19) 0.0121(6) Uani 1 1 d . . . C6 C 0.4897(3) 0.1163(2) 0.3295(2) 0.0167(6) Uani 1 1 d . . . H6A H 0.4315 0.0790 0.2956 0.020 Uiso 1 1 calc R . . H6B H 0.4544 0.1219 0.3841 0.020 Uiso 1 1 calc R . . C7 C 0.3893(3) 0.2029(2) 0.21514(19) 0.0157(6) Uani 1 1 d . . . H7A H 0.3026 0.2189 0.2334 0.019 Uiso 1 1 calc R . . H7B H 0.3781 0.1509 0.1864 0.019 Uiso 1 1 calc R . . H8A H 0.4393 0.3093 0.3153 0.019 Uiso 1 1 d R . . H8B H 0.3991 0.2461 0.3822 0.019 Uiso 1 1 d R . . C8 C 0.4722(3) 0.26219(19) 0.34629(19) 0.0121(6) Uani 1 1 d . . . C9 C 0.6290(4) 0.0823(2) 0.3414(2) 0.0188(7) Uani 1 1 d . . . C10 C 0.4358(3) 0.2653(2) 0.15619(19) 0.0138(6) Uani 1 1 d . . . N1 N 0.9876(2) 0.05286(15) 0.16074(15) 0.0079(4) Uani 1 1 d . . . N2 N 0.4882(3) 0.19530(16) 0.28802(16) 0.0117(5) Uani 1 1 d . . . O1 O 1.2194(2) 0.07331(13) 0.09974(13) 0.0117(4) Uani 1 1 d U . . O2 O 1.3224(2) -0.00733(14) 0.19374(14) 0.0150(4) Uani 1 1 d U . . O3 O 0.8519(2) 0.09250(14) 0.01555(14) 0.0141(4) Uani 1 1 d U . . O4 O 0.6596(2) 0.04653(15) 0.05150(15) 0.0187(5) Uani 1 1 d U . . O5 O 0.8078(2) 0.21116(13) 0.17250(13) 0.0109(4) Uani 1 1 d U . . O6 O 0.9949(2) 0.26344(13) 0.27315(13) 0.0118(4) Uani 1 1 d U . . O7 O 1.0355(2) 0.22604(13) 0.12564(13) 0.0103(4) Uani 1 1 d U . . O8 O 0.7195(3) 0.11628(15) 0.30512(16) 0.0206(5) Uani 1 1 d U . . O9 O 0.6491(3) 0.02131(17) 0.38464(18) 0.0280(6) Uani 1 1 d U . . O10 O 0.5599(2) 0.28034(14) 0.16258(14) 0.0143(4) Uani 1 1 d U . . O11 O 0.3558(2) 0.29587(15) 0.10311(15) 0.0184(5) Uani 1 1 d U . . O12 O 0.7287(2) 0.29336(13) 0.35085(13) 0.0115(4) Uani 1 1 d U . . O13 O 0.6508(2) 0.21254(13) 0.46843(14) 0.0138(4) Uani 1 1 d U . . O14 O 0.5974(2) 0.36102(13) 0.45452(13) 0.0125(4) Uani 1 1 d U . . O15 O 0.9589(3) 0.38964(16) 0.05189(17) 0.0245(5) Uani 1 1 d U . . H15A H 0.9448 0.4248 0.0876 0.029 Uiso 1 1 d R . . H15B H 0.8915 0.3876 0.0169 0.029 Uiso 1 1 d R . . O16 O 1.2141(3) 0.45072(18) 0.05670(19) 0.0316(6) Uani 1 1 d U . . H16A H 1.2821 0.4759 0.0768 0.038 Uiso 1 1 d R . . H16B H 1.2164 0.4483 0.0046 0.038 Uiso 1 1 d R . . O17 O 1.1767(2) 0.35857(15) 0.21532(15) 0.0184(4) Uani 1 1 d U . . H17A H 1.2432 0.3835 0.2380 0.022 Uiso 1 1 d R . . H17B H 1.1403 0.3348 0.2532 0.022 Uiso 1 1 d R . . O18 O 1.1509(2) 0.32200(16) 0.41373(15) 0.0198(5) Uani 1 1 d U . . H18A H 1.2123 0.2936 0.4376 0.024 Uiso 1 1 d R . . H18B H 1.1683 0.3704 0.4257 0.024 Uiso 1 1 d R . . O19 O 0.9500(3) 0.19189(17) 0.44664(18) 0.0282(5) Uani 1 1 d U . . H19A H 0.8735 0.1880 0.4625 0.034 Uiso 1 1 d R . . H19B H 1.0029 0.2031 0.4887 0.034 Uiso 1 1 d R . . O20 O 0.9267(2) 0.36277(14) 0.50972(14) 0.0149(4) Uani 1 1 d U . . H20A H 0.8641 0.3786 0.5364 0.018 Uiso 1 1 d R . . H20B H 0.9941 0.3566 0.5442 0.018 Uiso 1 1 d R . . O21 O 0.9374(2) 0.43742(14) 0.34375(14) 0.0149(4) Uani 1 1 d U . . H21A H 0.8819 0.4740 0.3302 0.018 Uiso 1 1 d R . . H21B H 1.0138 0.4577 0.3448 0.018 Uiso 1 1 d R . . O22 O 0.7427(3) 0.29279(19) 0.02588(19) 0.0319(7) Uani 1 1 d . . . H22A H 0.7377 0.2739 0.0740 0.038 Uiso 1 1 d R . . H22B H 0.6789 0.2738 -0.0057 0.038 Uiso 1 1 d R . . O23 O 0.0445(4) 0.0302(3) 0.4289(3) 0.0579(11) Uani 1 1 d . . . H23A H 0.1279 0.0280 0.4371 0.069 Uiso 1 1 d R . . H23B H 0.0245 0.0715 0.4001 0.069 Uiso 1 1 d R . . O24 O 0.8808(5) 0.9466(3) 0.3355(4) 0.089(2) Uani 1 1 d . . . H24A H 0.8076 0.9659 0.3464 0.107 Uiso 1 1 d R . . H24B H 0.8663 0.9004 0.3153 0.107 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 Mn1 0.0101(2) 0.0113(2) 0.0070(2) -0.00321(16) 0.00193(15) -0.00058(16) Mn2 0.0077(2) 0.0116(2) 0.0077(2) -0.00279(16) 0.00199(15) -0.00130(16) Cu1 0.00917(17) 0.00807(17) 0.00581(16) 0.00022(12) 0.00251(12) -0.00052(12) Cu2 0.00850(17) 0.01092(17) 0.00878(17) -0.00028(13) 0.00249(13) 0.00066(13) P1 0.0089(3) 0.0080(3) 0.0075(3) -0.0019(3) 0.0029(3) -0.0006(3) P2 0.0092(3) 0.0090(3) 0.0076(3) -0.0013(3) 0.0019(3) -0.0004(3) C1 0.0096(13) 0.0091(13) 0.0118(13) 0.0011(10) 0.0018(10) 0.0005(10) C2 0.0079(13) 0.0102(13) 0.0119(13) 0.0003(10) 0.0023(10) -0.0009(10) C3 0.0121(13) 0.0097(13) 0.0063(12) -0.0014(10) 0.0017(10) -0.0001(10) C4 0.0101(13) 0.0100(13) 0.0107(13) -0.0033(10) 0.0036(10) 0.0008(10) C5 0.0118(13) 0.0114(13) 0.0128(14) -0.0010(11) -0.0003(11) 0.0000(11) C6 0.0220(16) 0.0145(15) 0.0139(15) -0.0001(12) 0.0028(12) -0.0076(12) C7 0.0123(14) 0.0234(16) 0.0113(14) -0.0023(12) -0.0001(11) -0.0064(12) C8 0.0090(13) 0.0171(15) 0.0102(13) -0.0022(11) 0.0008(10) 0.0018(11) C9 0.0292(18) 0.0114(14) 0.0169(15) -0.0017(12) 0.0072(13) 0.0016(13) C10 0.0115(14) 0.0211(16) 0.0090(13) -0.0033(12) 0.0012(10) 0.0002(12) N1 0.0085(11) 0.0073(11) 0.0083(11) -0.0006(9) 0.0021(8) -0.0003(9) N2 0.0118(12) 0.0138(12) 0.0095(11) -0.0016(10) 0.0008(9) -0.0028(10) O1 0.0110(8) 0.0125(8) 0.0120(8) 0.0004(7) 0.0030(6) -0.0007(7) O2 0.0128(8) 0.0158(8) 0.0164(8) 0.0009(7) 0.0017(7) 0.0019(7) O3 0.0136(8) 0.0160(8) 0.0126(8) 0.0020(7) 0.0006(7) -0.0016(7) O4 0.0151(8) 0.0197(9) 0.0207(9) 0.0036(7) -0.0011(7) -0.0015(7) O5 0.0099(8) 0.0128(8) 0.0104(8) -0.0007(6) 0.0026(6) 0.0007(6) O6 0.0130(8) 0.0124(8) 0.0104(8) -0.0029(6) 0.0032(6) -0.0018(7) O7 0.0113(7) 0.0100(8) 0.0102(7) -0.0013(6) 0.0041(6) -0.0008(6) O8 0.0218(9) 0.0198(9) 0.0212(9) 0.0039(7) 0.0077(7) 0.0045(7) O9 0.0322(10) 0.0240(9) 0.0287(10) 0.0047(8) 0.0069(8) 0.0014(8) O10 0.0119(8) 0.0166(8) 0.0144(8) 0.0019(7) 0.0013(7) 0.0000(7) O11 0.0163(8) 0.0243(9) 0.0146(8) 0.0007(7) 0.0014(7) 0.0018(7) O12 0.0106(8) 0.0133(8) 0.0110(8) -0.0027(6) 0.0027(6) -0.0015(6) O13 0.0158(8) 0.0126(8) 0.0130(8) 0.0006(7) 0.0008(7) 0.0009(7) O14 0.0160(8) 0.0116(8) 0.0104(8) -0.0014(6) 0.0042(6) 0.0006(7) O15 0.0239(7) 0.0224(9) 0.0269(9) -0.0020(8) 0.0006(7) 0.0061(7) O16 0.0371(9) 0.0268(8) 0.0312(9) 0.0048(8) 0.0050(8) -0.0080(8) O17 0.0205(8) 0.0199(9) 0.0154(6) -0.0050(6) 0.0050(6) -0.0051(7) O18 0.0143(7) 0.0249(9) 0.0198(9) -0.0055(7) -0.0004(7) 0.0011(7) O19 0.0355(10) 0.0234(8) 0.0277(9) 0.0058(7) 0.0134(8) 0.0049(8) O20 0.0141(8) 0.0182(8) 0.0129(7) -0.0029(6) 0.0031(6) 0.0000(7) O21 0.0131(8) 0.0142(7) 0.0178(8) 0.0001(6) 0.0034(7) -0.0002(7) O22 0.0278(15) 0.0398(17) 0.0266(15) 0.0059(12) -0.0045(11) -0.0042(13) O23 0.063(3) 0.057(3) 0.054(2) 0.013(2) 0.0050(19) 0.018(2) O24 0.076(3) 0.033(2) 0.170(6) 0.015(3) 0.068(4) 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 Mn1 O13 2.049(2) 4_665 ? Mn1 O17 2.133(2) . ? Mn1 O7 2.160(2) . ? Mn1 O15 2.175(3) . ? Mn1 O11 2.199(2) 1_655 ? Mn1 O16 2.243(3) . ? Mn2 O6 2.098(2) . ? Mn2 O12 2.121(2) . ? Mn2 O21 2.188(2) . ? Mn2 O18 2.213(2) . ? Mn2 O20 2.235(2) . ? Mn2 O19 2.270(3) . ? Cu1 O14 1.894(2) 4_665 ? Cu1 O3 1.965(2) . ? Cu1 O1 1.978(2) . ? Cu1 N1 2.021(2) . ? Cu1 O7 2.281(2) . ? Cu2 O5 1.914(2) . ? Cu2 O8 1.940(3) . ? Cu2 O10 1.960(2) . ? Cu2 N2 2.015(3) . ? Cu2 O12 2.317(2) . ? P1 O6 1.510(2) . ? P1 O7 1.525(2) . ? P1 O5 1.527(2) . ? P1 C3 1.807(3) . ? P2 O13 1.504(2) . ? P2 O14 1.514(2) . ? P2 O12 1.532(2) . ? P2 C8 1.814(3) . ? C1 N1 1.477(4) . ? C1 C4 1.524(4) . ? C1 H1A 0.9900 . ? C1 H1B 0.9900 . ? C2 N1 1.483(4) . ? C2 C5 1.514(4) . ? C2 H2A 0.9900 . ? C2 H2B 0.9900 . ? C3 N1 1.489(4) . ? C3 H3A 0.9900 . ? C3 H3B 0.9900 . ? C4 O2 1.244(4) . ? C4 O1 1.268(4) . ? C5 O4 1.241(4) . ? C5 O3 1.279(4) . ? C6 N2 1.484(4) . ? C6 C9 1.517(5) . ? C6 H6A 0.9900 . ? C6 H6B 0.9900 . ? C7 N2 1.481(4) . ? C7 C10 1.520(5) . ? C7 H7A 0.9900 . ? C7 H7B 0.9900 . ? C8 N2 1.484(4) . ? C8 H8A 0.9768 . ? C8 H8B 1.0213 . ? C9 O9 1.245(4) . ? C9 O8 1.270(4) . ? C10 O11 1.236(4) . ? C10 O10 1.278(4) . ? O11 Mn1 2.199(2) 1_455 ? O13 Mn1 2.049(2) 4_566 ? O14 Cu1 1.894(2) 4_566 ? O15 H15A 0.8476 . ? O15 H15B 0.8469 . ? O16 H16A 0.8460 . ? O16 H16B 0.8478 . ? O17 H17A 0.8464 . ? O17 H17B 0.8458 . ? O18 H18A 0.8467 . ? O18 H18B 0.8484 . ? O19 H19A 0.8427 . ? O19 H19B 0.8482 . ? O20 H20A 0.8436 . ? O20 H20B 0.8471 . ? O21 H21A 0.8467 . ? O21 H21B 0.8440 . ? O22 H22A 0.8480 . ? O22 H22B 0.8470 . ? O23 H23A 0.8437 . ? O23 H23B 0.8485 . ? O24 H24A 0.8434 . ? O24 H24B 0.8486 . ? 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 O13 Mn1 O17 168.20(10) 4_665 . ? O13 Mn1 O7 94.00(9) 4_665 . ? O17 Mn1 O7 86.81(9) . . ? O13 Mn1 O15 90.72(10) 4_665 . ? O17 Mn1 O15 101.06(10) . . ? O7 Mn1 O15 89.87(9) . . ? O13 Mn1 O11 84.99(9) 4_665 1_655 ? O17 Mn1 O11 83.52(9) . 1_655 ? O7 Mn1 O11 106.91(9) . 1_655 ? O15 Mn1 O11 162.91(10) . 1_655 ? O13 Mn1 O16 93.39(10) 4_665 . ? O17 Mn1 O16 88.45(11) . . ? O7 Mn1 O16 165.73(10) . . ? O15 Mn1 O16 77.84(11) . . ? O11 Mn1 O16 85.89(11) 1_655 . ? O6 Mn2 O12 95.48(8) . . ? O6 Mn2 O21 96.79(9) . . ? O12 Mn2 O21 96.62(9) . . ? O6 Mn2 O18 81.81(9) . . ? O12 Mn2 O18 175.39(9) . . ? O21 Mn2 O18 87.43(9) . . ? O6 Mn2 O20 164.83(9) . . ? O12 Mn2 O20 99.36(8) . . ? O21 Mn2 O20 84.64(9) . . ? O18 Mn2 O20 83.17(9) . . ? O6 Mn2 O19 91.41(9) . . ? O12 Mn2 O19 90.14(10) . . ? O21 Mn2 O19 168.81(10) . . ? O18 Mn2 O19 86.21(11) . . ? O20 Mn2 O19 85.48(10) . . ? O14 Cu1 O3 96.08(9) 4_665 . ? O14 Cu1 O1 91.77(9) 4_665 . ? O3 Cu1 O1 156.03(10) . . ? O14 Cu1 N1 169.27(10) 4_665 . ? O3 Cu1 N1 85.04(10) . . ? O1 Cu1 N1 83.22(9) . . ? O14 Cu1 O7 101.69(9) 4_665 . ? O3 Cu1 O7 102.64(9) . . ? O1 Cu1 O7 97.86(9) . . ? N1 Cu1 O7 88.43(9) . . ? O5 Cu2 O8 96.80(10) . . ? O5 Cu2 O10 90.76(9) . . ? O8 Cu2 O10 161.18(11) . . ? O5 Cu2 N2 166.03(10) . . ? O8 Cu2 N2 85.46(11) . . ? O10 Cu2 N2 83.23(10) . . ? O5 Cu2 O12 105.01(9) . . ? O8 Cu2 O12 91.38(10) . . ? O10 Cu2 O12 103.31(9) . . ? N2 Cu2 O12 88.67(9) . . ? O6 P1 O7 113.77(13) . . ? O6 P1 O5 113.32(12) . . ? O7 P1 O5 110.53(12) . . ? O6 P1 C3 106.27(13) . . ? O7 P1 C3 103.68(13) . . ? O5 P1 C3 108.60(13) . . ? O13 P2 O14 115.48(13) . . ? O13 P2 O12 112.51(13) . . ? O14 P2 O12 110.95(13) . . ? O13 P2 C8 107.71(14) . . ? O14 P2 C8 105.07(14) . . ? O12 P2 C8 104.14(13) . . ? N1 C1 C4 108.2(2) . . ? N1 C1 H1A 110.1 . . ? C4 C1 H1A 110.1 . . ? N1 C1 H1B 110.1 . . ? C4 C1 H1B 110.1 . . ? H1A C1 H1B 108.4 . . ? N1 C2 C5 111.9(2) . . ? N1 C2 H2A 109.2 . . ? C5 C2 H2A 109.2 . . ? N1 C2 H2B 109.2 . . ? C5 C2 H2B 109.2 . . ? H2A C2 H2B 107.9 . . ? N1 C3 P1 111.98(19) . . ? N1 C3 H3A 109.2 . . ? P1 C3 H3A 109.2 . . ? N1 C3 H3B 109.2 . . ? P1 C3 H3B 109.2 . . ? H3A C3 H3B 107.9 . . ? O2 C4 O1 124.4(3) . . ? O2 C4 C1 119.1(3) . . ? O1 C4 C1 116.5(3) . . ? O4 C5 O3 123.8(3) . . ? O4 C5 C2 118.0(3) . . ? O3 C5 C2 118.2(3) . . ? N2 C6 C9 111.3(3) . . ? N2 C6 H6A 109.4 . . ? C9 C6 H6A 109.4 . . ? N2 C6 H6B 109.4 . . ? C9 C6 H6B 109.4 . . ? H6A C6 H6B 108.0 . . ? N2 C7 C10 109.5(2) . . ? N2 C7 H7A 109.8 . . ? C10 C7 H7A 109.8 . . ? N2 C7 H7B 109.8 . . ? C10 C7 H7B 109.8 . . ? H7A C7 H7B 108.2 . . ? N2 C8 P2 112.4(2) . . ? N2 C8 H8A 109.6 . . ? P2 C8 H8A 112.0 . . ? N2 C8 H8B 107.0 . . ? P2 C8 H8B 109.5 . . ? H8A C8 H8B 105.9 . . ? O9 C9 O8 122.8(3) . . ? O9 C9 C6 118.7(3) . . ? O8 C9 C6 118.5(3) . . ? O11 C10 O10 123.4(3) . . ? O11 C10 C7 120.1(3) . . ? O10 C10 C7 116.5(3) . . ? C1 N1 C2 113.3(2) . . ? C1 N1 C3 109.7(2) . . ? C2 N1 C3 112.1(2) . . ? C1 N1 Cu1 103.52(17) . . ? C2 N1 Cu1 108.68(17) . . ? C3 N1 Cu1 109.07(17) . . ? C7 N2 C6 114.6(2) . . ? C7 N2 C8 109.7(2) . . ? C6 N2 C8 112.5(2) . . ? C7 N2 Cu2 103.86(19) . . ? C6 N2 Cu2 108.0(2) . . ? C8 N2 Cu2 107.69(19) . . ? C4 O1 Cu1 113.27(19) . . ? C5 O3 Cu1 115.0(2) . . ? P1 O5 Cu2 128.41(13) . . ? P1 O6 Mn2 145.48(14) . . ? P1 O7 Mn1 133.16(13) . . ? P1 O7 Cu1 105.35(11) . . ? Mn1 O7 Cu1 121.28(10) . . ? C9 O8 Cu2 115.1(2) . . ? C10 O10 Cu2 113.3(2) . . ? C10 O11 Mn1 138.6(2) . 1_455 ? P2 O12 Mn2 126.04(13) . . ? P2 O12 Cu2 105.27(11) . . ? Mn2 O12 Cu2 118.73(10) . . ? P2 O13 Mn1 144.40(15) . 4_566 ? P2 O14 Cu1 136.50(14) . 4_566 ? Mn1 O15 H15A 110.3 . . ? Mn1 O15 H15B 141.4 . . ? H15A O15 H15B 108.0 . . ? Mn1 O16 H16A 129.3 . . ? Mn1 O16 H16B 102.4 . . ? H16A O16 H16B 108.0 . . ? Mn1 O17 H17A 125.7 . . ? Mn1 O17 H17B 123.9 . . ? H17A O17 H17B 107.4 . . ? Mn2 O18 H18A 137.2 . . ? Mn2 O18 H18B 107.5 . . ? H18A O18 H18B 107.8 . . ? Mn2 O19 H19A 100.5 . . ? Mn2 O19 H19B 100.5 . . ? H19A O19 H19B 107.6 . . ? Mn2 O20 H20A 133.2 . . ? Mn2 O20 H20B 117.8 . . ? H20A O20 H20B 107.4 . . ? Mn2 O21 H21A 137.8 . . ? Mn2 O21 H21B 114.6 . . ? H21A O21 H21B 107.4 . . ? H22A O22 H22B 107.9 . . ? H23A O23 H23B 107.8 . . ? H24A O24 H24B 107.8 . . ? _diffrn_measured_fraction_theta_max 0.988 _diffrn_reflns_theta_full 28.41 _diffrn_measured_fraction_theta_full 0.988 _refine_diff_density_max 1.551 _refine_diff_density_min -1.998 _refine_diff_density_rms 0.121 #===END data_2-CuCo _database_code_depnum_ccdc_archive 'CCDC 742513' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C10 H32 Co2 Cu2 N2 O24 P2' _chemical_formula_weight 871.26 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' Co Co 0.3494 0.9721 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting Monoclinic _symmetry_space_group_name_H-M P2(1)/n _symmetry_space_group_name_Hall '-P 2yn' loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x+1/2, y+1/2, -z+1/2' '-x, -y, -z' 'x-1/2, -y-1/2, z-1/2' _cell_length_a 10.0105(4) _cell_length_b 16.7050(7) _cell_length_c 15.9762(7) _cell_angle_alpha 90.00 _cell_angle_beta 95.628(2) _cell_angle_gamma 90.00 _cell_volume 2658.75(19) _cell_formula_units_Z 4 _cell_measurement_temperature 100(2) _cell_measurement_reflns_used 9930 _cell_measurement_theta_min 2.30 _cell_measurement_theta_max 28.35 _exptl_crystal_description block _exptl_crystal_colour purple _exptl_crystal_size_max 0.32 _exptl_crystal_size_mid 0.29 _exptl_crystal_size_min 0.26 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 2.177 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1760 _exptl_absorpt_coefficient_mu 3.032 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.6426 _exptl_absorpt_correction_T_max 0.6591 _exptl_absorpt_process_details 'SADABS; Bruker, 2000' _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 'Bruker Smart Apex CCD' _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 25375 _diffrn_reflns_av_R_equivalents 0.0281 _diffrn_reflns_av_sigmaI/netI 0.0233 _diffrn_reflns_limit_h_min -13 _diffrn_reflns_limit_h_max 13 _diffrn_reflns_limit_k_min -22 _diffrn_reflns_limit_k_max 17 _diffrn_reflns_limit_l_min -21 _diffrn_reflns_limit_l_max 21 _diffrn_reflns_theta_min 1.77 _diffrn_reflns_theta_max 28.36 _reflns_number_total 6646 _reflns_number_gt 6206 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'SMART (Bruker, 2000)' _computing_cell_refinement SMART _computing_data_reduction 'SAINT (Bruker, 2000)' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics SHELXTL _computing_publication_material 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^)+(0.0443P)^2^+10.7407P] 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 6646 _refine_ls_number_parameters 379 _refine_ls_number_restraints 142 _refine_ls_R_factor_all 0.0430 _refine_ls_R_factor_gt 0.0405 _refine_ls_wR_factor_ref 0.1080 _refine_ls_wR_factor_gt 0.1066 _refine_ls_goodness_of_fit_ref 1.172 _refine_ls_restrained_S_all 1.266 _refine_ls_shift/su_max 0.006 _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 Co1 Co 1.14905(5) 0.32459(3) 0.09276(3) 0.01044(11) Uani 1 1 d U . . Co2 Co 0.93825(4) 0.31174(3) 0.38643(3) 0.00796(11) Uani 1 1 d U . . Cu1 Cu 1.04302(4) 0.10440(2) 0.06168(2) 0.00748(10) Uani 1 1 d . . . Cu2 Cu 0.66745(4) 0.20791(3) 0.24580(3) 0.00912(10) Uani 1 1 d . . . P1 P 0.96113(8) 0.20743(5) 0.20458(5) 0.00743(16) Uani 1 1 d . . . P2 P 0.62907(8) 0.28281(5) 0.41787(5) 0.00749(16) Uani 1 1 d . . . C1 C 1.0912(3) -0.0157(2) 0.1798(2) 0.0097(6) Uani 1 1 d . . . H1A H 1.0648 -0.0611 0.1420 0.012 Uiso 1 1 calc R . . H1B H 1.0956 -0.0348 0.2387 0.012 Uiso 1 1 calc R . . C2 C 0.8515(3) 0.0208(2) 0.1509(2) 0.0087(6) Uani 1 1 d . . . H2A H 0.8010 0.0371 0.1984 0.010 Uiso 1 1 calc R . . H2B H 0.8513 -0.0384 0.1484 0.010 Uiso 1 1 calc R . . C3 C 1.0101(3) 0.1071(2) 0.2379(2) 0.0089(6) Uani 1 1 d . . . H3A H 1.1054 0.1073 0.2614 0.011 Uiso 1 1 calc R . . H3B H 0.9552 0.0897 0.2828 0.011 Uiso 1 1 calc R . . C4 C 1.2273(3) 0.0168(2) 0.1611(2) 0.0097(6) Uani 1 1 d . . . C5 C 0.7819(3) 0.0537(2) 0.0697(2) 0.0109(6) Uani 1 1 d . . . C6 C 0.4925(4) 0.1151(2) 0.3372(2) 0.0188(8) Uani 1 1 d . . . H6A H 0.4328 0.0774 0.3035 0.023 Uiso 1 1 calc R . . H6B H 0.4576 0.1217 0.3926 0.023 Uiso 1 1 calc R . . C7 C 0.3906(4) 0.2007(3) 0.2198(2) 0.0182(8) Uani 1 1 d . . . H7A H 0.3026 0.2164 0.2381 0.022 Uiso 1 1 calc R . . H7B H 0.3797 0.1484 0.1908 0.022 Uiso 1 1 calc R . . H8A H 0.4406 0.3071 0.3199 0.022 Uiso 1 1 d R . . H8B H 0.4004 0.2439 0.3869 0.022 Uiso 1 1 d R . . C8 C 0.4759(3) 0.2618(2) 0.3518(2) 0.0123(6) Uani 1 1 d . . . C9 C 0.6331(5) 0.0805(2) 0.3495(3) 0.0217(8) Uani 1 1 d . . . C10 C 0.4366(4) 0.2631(2) 0.1600(2) 0.0151(7) Uani 1 1 d . . . N1 N 0.9922(3) 0.04967(17) 0.16643(17) 0.0076(5) Uani 1 1 d . . . N2 N 0.4909(3) 0.19366(19) 0.29379(19) 0.0115(6) Uani 1 1 d . . . O1 O 1.2257(2) 0.06990(15) 0.10452(16) 0.0116(5) Uani 1 1 d U . . O2 O 1.3309(3) -0.00932(16) 0.20112(16) 0.0141(5) Uani 1 1 d U . . O3 O 0.8542(3) 0.08869(16) 0.01898(16) 0.0126(5) Uani 1 1 d U . . O4 O 0.6596(3) 0.04345(17) 0.05507(17) 0.0169(5) Uani 1 1 d U . . O5 O 0.8112(2) 0.20709(15) 0.17560(15) 0.0101(5) Uani 1 1 d U . . O6 O 0.9982(2) 0.26174(15) 0.27877(15) 0.0108(5) Uani 1 1 d U . . O7 O 1.0423(2) 0.22262(14) 0.13025(15) 0.0093(4) Uani 1 1 d U . . O8 O 0.7251(3) 0.11463(18) 0.31295(19) 0.0221(6) Uani 1 1 d U . . O9 O 0.6530(4) 0.0198(2) 0.3938(2) 0.0321(7) Uani 1 1 d U . . O10 O 0.5626(3) 0.27865(16) 0.16688(16) 0.0140(5) Uani 1 1 d U . . O11 O 0.3557(3) 0.29421(18) 0.10632(18) 0.0195(6) Uani 1 1 d U . . O12 O 0.7359(2) 0.29133(15) 0.35601(15) 0.0103(5) Uani 1 1 d U . . O13 O 0.6551(3) 0.21270(15) 0.47640(16) 0.0128(5) Uani 1 1 d U . . O14 O 0.6045(3) 0.36243(15) 0.45915(16) 0.0128(5) Uani 1 1 d U . . O15 O 0.9682(3) 0.3828(2) 0.0594(2) 0.0275(6) Uani 1 1 d U . . H15A H 0.9541 0.4180 0.0951 0.033 Uiso 1 1 d R . . H15B H 0.9008 0.3808 0.0244 0.033 Uiso 1 1 d R . . O16 O 1.2253(4) 0.4446(2) 0.0659(2) 0.0377(7) Uani 1 1 d U . . H16A H 1.2933 0.4697 0.0859 0.045 Uiso 1 1 d R . . H16B H 1.2276 0.4421 0.0138 0.045 Uiso 1 1 d R . . O17 O 1.1768(3) 0.35452(17) 0.21522(17) 0.0178(5) Uani 1 1 d U . . H17A H 1.2433 0.3794 0.2379 0.021 Uiso 1 1 d R . . H17B H 1.1404 0.3307 0.2531 0.021 Uiso 1 1 d R . . O18 O 1.1480(3) 0.32626(17) 0.41468(17) 0.0164(5) Uani 1 1 d U . . H18A H 1.2094 0.2979 0.4386 0.020 Uiso 1 1 d R . . H18B H 1.1654 0.3747 0.4266 0.020 Uiso 1 1 d R . . O19 O 0.9533(3) 0.19731(18) 0.44767(19) 0.0216(5) Uani 1 1 d U . . H19A H 0.8767 0.1934 0.4636 0.026 Uiso 1 1 d R . . H19B H 1.0062 0.2086 0.4898 0.026 Uiso 1 1 d R . . O20 O 0.9261(3) 0.36223(16) 0.50902(16) 0.0141(5) Uani 1 1 d U . . H20A H 0.8635 0.3781 0.5357 0.017 Uiso 1 1 d R . . H20B H 0.9935 0.3560 0.5435 0.017 Uiso 1 1 d R . . O21 O 0.9321(3) 0.42908(16) 0.34146(16) 0.0138(4) Uani 1 1 d U . . H21A H 0.8766 0.4657 0.3279 0.017 Uiso 1 1 d R . . H21B H 1.0085 0.4493 0.3425 0.017 Uiso 1 1 d R . . O22 O 0.7500(4) 0.2881(2) 0.0257(2) 0.0320(8) Uani 1 1 d . . . H22A H 0.7450 0.2693 0.0738 0.038 Uiso 1 1 d R . . H22B H 0.6862 0.2692 -0.0059 0.038 Uiso 1 1 d R . . O23 O 0.0511(15) 0.0349(8) 0.4387(8) 0.217(7) Uani 1 1 d . . . H23A H 0.1345 0.0327 0.4468 0.261 Uiso 1 1 d R . . H23B H 0.0311 0.0762 0.4099 0.261 Uiso 1 1 d R . . O24 O 0.9151(8) 0.9458(4) 0.3742(5) 0.104(2) Uani 1 1 d . . . H24A H 0.8419 0.9650 0.3851 0.124 Uiso 1 1 d R . . H24B H 0.9006 0.8995 0.3540 0.124 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 Co1 0.0121(2) 0.0129(2) 0.0064(2) -0.00380(16) 0.00096(16) -0.00100(17) Co2 0.0072(2) 0.0096(2) 0.0071(2) -0.00232(16) 0.00050(15) -0.00107(16) Cu1 0.00957(19) 0.00738(19) 0.00570(19) 0.00039(14) 0.00184(14) -0.00071(14) Cu2 0.00951(19) 0.0096(2) 0.0085(2) -0.00035(14) 0.00190(14) 0.00045(14) P1 0.0090(4) 0.0068(4) 0.0067(4) -0.0014(3) 0.0019(3) -0.0005(3) P2 0.0082(4) 0.0075(4) 0.0067(4) -0.0007(3) 0.0009(3) -0.0008(3) C1 0.0094(14) 0.0073(14) 0.0126(15) 0.0009(12) 0.0019(12) 0.0018(11) C2 0.0068(14) 0.0095(14) 0.0101(14) 0.0003(12) 0.0014(11) -0.0012(11) C3 0.0118(15) 0.0086(15) 0.0063(14) -0.0006(11) 0.0009(11) 0.0006(12) C4 0.0107(14) 0.0084(15) 0.0103(14) -0.0041(12) 0.0027(11) -0.0005(12) C5 0.0130(15) 0.0076(14) 0.0117(15) -0.0005(12) -0.0009(12) 0.0005(12) C6 0.027(2) 0.0150(17) 0.0150(17) 0.0000(14) 0.0040(14) -0.0110(15) C7 0.0121(16) 0.030(2) 0.0119(16) -0.0011(15) -0.0012(13) -0.0083(15) C8 0.0098(15) 0.0166(17) 0.0107(15) -0.0023(13) 0.0016(12) 0.0012(13) C9 0.040(2) 0.0107(17) 0.0164(18) -0.0018(14) 0.0106(16) 0.0002(16) C10 0.0117(15) 0.0254(19) 0.0081(15) -0.0039(14) 0.0011(12) -0.0020(14) N1 0.0080(12) 0.0072(12) 0.0077(12) -0.0005(10) 0.0016(9) 0.0007(10) N2 0.0114(13) 0.0139(14) 0.0091(13) -0.0012(11) -0.0004(10) -0.0043(11) O1 0.0112(8) 0.0118(8) 0.0120(8) 0.0003(7) 0.0019(7) -0.0005(7) O2 0.0122(8) 0.0143(9) 0.0156(9) 0.0001(7) 0.0010(7) 0.0016(7) O3 0.0126(8) 0.0136(9) 0.0115(8) 0.0015(7) -0.0002(7) -0.0016(7) O4 0.0147(9) 0.0169(9) 0.0184(9) 0.0024(8) -0.0013(7) -0.0009(7) O5 0.0094(8) 0.0112(8) 0.0098(8) -0.0008(7) 0.0013(7) 0.0005(7) O6 0.0115(8) 0.0112(8) 0.0101(8) -0.0027(7) 0.0025(7) -0.0017(7) O7 0.0104(8) 0.0090(8) 0.0087(8) -0.0010(7) 0.0027(7) -0.0006(7) O8 0.0251(10) 0.0207(10) 0.0218(9) 0.0034(8) 0.0078(8) 0.0053(8) O9 0.0380(11) 0.0279(11) 0.0311(11) 0.0033(9) 0.0067(9) 0.0008(9) O10 0.0117(8) 0.0165(9) 0.0138(9) 0.0017(7) 0.0011(7) 0.0003(7) O11 0.0165(9) 0.0261(10) 0.0156(9) 0.0004(8) 0.0012(8) 0.0008(8) O12 0.0098(8) 0.0121(8) 0.0093(8) -0.0011(7) 0.0024(7) -0.0018(7) O13 0.0151(9) 0.0120(9) 0.0112(8) 0.0007(7) 0.0000(7) 0.0007(7) O14 0.0161(9) 0.0115(9) 0.0115(8) -0.0005(7) 0.0038(7) 0.0000(7) O15 0.0275(8) 0.0260(10) 0.0283(10) -0.0010(8) -0.0007(7) 0.0070(7) O16 0.0448(10) 0.0333(9) 0.0359(10) 0.0060(8) 0.0076(9) -0.0111(9) O17 0.0197(9) 0.0188(9) 0.0152(7) -0.0063(7) 0.0038(7) -0.0049(8) O18 0.0123(7) 0.0202(9) 0.0162(9) -0.0035(7) -0.0007(7) 0.0001(7) O19 0.0253(10) 0.0193(8) 0.0215(9) 0.0047(7) 0.0084(8) 0.0029(8) O20 0.0130(8) 0.0172(8) 0.0122(7) -0.0029(7) 0.0020(7) 0.0003(7) O21 0.0127(8) 0.0127(7) 0.0163(8) 0.0006(7) 0.0022(7) -0.0001(7) O22 0.0336(18) 0.0380(19) 0.0224(16) 0.0010(14) -0.0076(13) -0.0016(15) O23 0.290(17) 0.143(11) 0.199(13) 0.041(10) -0.081(12) 0.004(11) O24 0.148(7) 0.038(3) 0.129(6) -0.012(4) 0.035(5) 0.012(4) _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 Co1 O13 1.967(3) 4_665 ? Co1 O17 2.012(3) . ? Co1 O15 2.078(3) . ? Co1 O11 2.121(3) 1_655 ? Co1 O7 2.128(2) . ? Co1 O16 2.202(4) . ? Co2 O6 2.054(2) . ? Co2 O12 2.065(2) . ? Co2 O21 2.086(3) . ? Co2 O18 2.118(3) . ? Co2 O19 2.146(3) . ? Co2 O20 2.147(3) . ? Cu1 O14 1.889(3) 4_665 ? Cu1 O3 1.963(3) . ? Cu1 O1 1.974(3) . ? Cu1 N1 2.015(3) . ? Cu1 O7 2.259(2) . ? Cu2 O5 1.909(2) . ? Cu2 O8 1.947(3) . ? Cu2 O10 1.957(3) . ? Cu2 N2 2.008(3) . ? Cu2 O12 2.297(2) . ? P1 O6 1.510(3) . ? P1 O7 1.524(2) . ? P1 O5 1.526(3) . ? P1 C3 1.811(3) . ? P2 O13 1.505(3) . ? P2 O14 1.515(3) . ? P2 O12 1.532(3) . ? P2 C8 1.809(4) . ? C1 N1 1.476(4) . ? C1 C4 1.523(5) . ? C1 H1A 0.9900 . ? C1 H1B 0.9900 . ? C2 N1 1.486(4) . ? C2 C5 1.516(5) . ? C2 H2A 0.9900 . ? C2 H2B 0.9900 . ? C3 N1 1.489(4) . ? C3 H3A 0.9900 . ? C3 H3B 0.9900 . ? C4 O2 1.243(4) . ? C4 O1 1.266(4) . ? C5 O4 1.235(4) . ? C5 O3 1.279(4) . ? C6 N2 1.483(5) . ? C6 C9 1.516(6) . ? C6 H6A 0.9900 . ? C6 H6B 0.9900 . ? C7 N2 1.479(5) . ? C7 C10 1.515(5) . ? C7 H7A 0.9900 . ? C7 H7B 0.9900 . ? C8 N2 1.485(5) . ? C8 H8A 0.9595 . ? C8 H8B 1.0282 . ? C9 O9 1.240(5) . ? C9 O8 1.273(5) . ? C10 O11 1.235(5) . ? C10 O10 1.282(4) . ? O11 Co1 2.121(3) 1_455 ? O13 Co1 1.967(3) 4_566 ? O14 Cu1 1.889(3) 4_566 ? O15 H15A 0.8405 . ? O15 H15B 0.8342 . ? O16 H16A 0.8364 . ? O16 H16B 0.8358 . ? O17 H17A 0.8366 . ? O17 H17B 0.8373 . ? O18 H18A 0.8375 . ? O18 H18B 0.8448 . ? O19 H19A 0.8332 . ? O19 H19B 0.8355 . ? O20 H20A 0.8349 . ? O20 H20B 0.8345 . ? O21 H21A 0.8398 . ? O21 H21B 0.8349 . ? O22 H22A 0.8374 . ? O22 H22B 0.8357 . ? O23 H23A 0.8329 . ? O23 H23B 0.8424 . ? O24 H24A 0.8348 . ? O24 H24B 0.8442 . ? 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 O13 Co1 O17 169.57(11) 4_665 . ? O13 Co1 O15 90.72(12) 4_665 . ? O17 Co1 O15 99.61(13) . . ? O13 Co1 O11 84.30(11) 4_665 1_655 ? O17 Co1 O11 85.40(11) . 1_655 ? O15 Co1 O11 162.72(13) . 1_655 ? O13 Co1 O7 94.32(10) 4_665 . ? O17 Co1 O7 87.17(11) . . ? O15 Co1 O7 89.88(12) . . ? O11 Co1 O7 106.96(11) 1_655 . ? O13 Co1 O16 93.46(13) 4_665 . ? O17 Co1 O16 86.91(13) . . ? O15 Co1 O16 80.44(14) . . ? O11 Co1 O16 83.35(13) 1_655 . ? O7 Co1 O16 167.64(12) . . ? O6 Co2 O12 95.53(10) . . ? O6 Co2 O21 95.45(10) . . ? O12 Co2 O21 94.53(10) . . ? O6 Co2 O18 81.95(10) . . ? O12 Co2 O18 176.75(11) . . ? O21 Co2 O18 87.77(11) . . ? O6 Co2 O19 90.36(11) . . ? O12 Co2 O19 89.05(11) . . ? O21 Co2 O19 172.84(11) . . ? O18 Co2 O19 88.92(12) . . ? O6 Co2 O20 166.18(10) . . ? O12 Co2 O20 97.91(10) . . ? O21 Co2 O20 86.71(10) . . ? O18 Co2 O20 84.50(10) . . ? O19 Co2 O20 86.66(11) . . ? O14 Cu1 O3 97.04(11) 4_665 . ? O14 Cu1 O1 90.96(11) 4_665 . ? O3 Cu1 O1 155.33(11) . . ? O14 Cu1 N1 169.58(11) 4_665 . ? O3 Cu1 N1 85.13(11) . . ? O1 Cu1 N1 83.12(11) . . ? O14 Cu1 O7 100.43(10) 4_665 . ? O3 Cu1 O7 103.68(10) . . ? O1 Cu1 O7 97.71(10) . . ? N1 Cu1 O7 88.90(10) . . ? O5 Cu2 O8 96.78(11) . . ? O5 Cu2 O10 90.78(11) . . ? O8 Cu2 O10 161.75(12) . . ? O5 Cu2 N2 164.91(11) . . ? O8 Cu2 N2 85.37(13) . . ? O10 Cu2 N2 83.16(12) . . ? O5 Cu2 O12 105.63(10) . . ? O8 Cu2 O12 90.76(11) . . ? O10 Cu2 O12 103.20(10) . . ? N2 Cu2 O12 89.24(10) . . ? O6 P1 O7 113.75(14) . . ? O6 P1 O5 113.52(14) . . ? O7 P1 O5 110.32(14) . . ? O6 P1 C3 106.64(15) . . ? O7 P1 C3 103.50(15) . . ? O5 P1 C3 108.40(15) . . ? O13 P2 O14 115.99(15) . . ? O13 P2 O12 112.56(15) . . ? O14 P2 O12 110.63(14) . . ? O13 P2 C8 107.27(16) . . ? O14 P2 C8 105.06(16) . . ? O12 P2 C8 104.30(15) . . ? N1 C1 C4 108.0(3) . . ? N1 C1 H1A 110.1 . . ? C4 C1 H1A 110.1 . . ? N1 C1 H1B 110.1 . . ? C4 C1 H1B 110.1 . . ? H1A C1 H1B 108.4 . . ? N1 C2 C5 112.0(3) . . ? N1 C2 H2A 109.2 . . ? C5 C2 H2A 109.2 . . ? N1 C2 H2B 109.2 . . ? C5 C2 H2B 109.2 . . ? H2A C2 H2B 107.9 . . ? N1 C3 P1 111.2(2) . . ? N1 C3 H3A 109.4 . . ? P1 C3 H3A 109.4 . . ? N1 C3 H3B 109.4 . . ? P1 C3 H3B 109.4 . . ? H3A C3 H3B 108.0 . . ? O2 C4 O1 124.4(3) . . ? O2 C4 C1 119.4(3) . . ? O1 C4 C1 116.1(3) . . ? O4 C5 O3 123.8(3) . . ? O4 C5 C2 118.4(3) . . ? O3 C5 C2 117.8(3) . . ? N2 C6 C9 111.5(3) . . ? N2 C6 H6A 109.3 . . ? C9 C6 H6A 109.3 . . ? N2 C6 H6B 109.3 . . ? C9 C6 H6B 109.3 . . ? H6A C6 H6B 108.0 . . ? N2 C7 C10 109.5(3) . . ? N2 C7 H7A 109.8 . . ? C10 C7 H7A 109.8 . . ? N2 C7 H7B 109.8 . . ? C10 C7 H7B 109.8 . . ? H7A C7 H7B 108.2 . . ? N2 C8 P2 112.4(2) . . ? N2 C8 H8A 109.1 . . ? P2 C8 H8A 113.8 . . ? N2 C8 H8B 104.0 . . ? P2 C8 H8B 111.4 . . ? H8A C8 H8B 105.4 . . ? O9 C9 O8 123.0(4) . . ? O9 C9 C6 118.8(4) . . ? O8 C9 C6 118.2(4) . . ? O11 C10 O10 123.1(4) . . ? O11 C10 C7 120.6(3) . . ? O10 C10 C7 116.3(3) . . ? C1 N1 C2 113.3(3) . . ? C1 N1 C3 109.7(3) . . ? C2 N1 C3 112.2(3) . . ? C1 N1 Cu1 103.6(2) . . ? C2 N1 Cu1 108.7(2) . . ? C3 N1 Cu1 108.9(2) . . ? C7 N2 C6 114.8(3) . . ? C7 N2 C8 109.6(3) . . ? C6 N2 C8 112.6(3) . . ? C7 N2 Cu2 103.8(2) . . ? C6 N2 Cu2 108.3(2) . . ? C8 N2 Cu2 107.1(2) . . ? C4 O1 Cu1 113.5(2) . . ? C5 O3 Cu1 115.3(2) . . ? P1 O5 Cu2 126.66(15) . . ? P1 O6 Co2 146.33(16) . . ? P1 O7 Co1 132.32(15) . . ? P1 O7 Cu1 105.05(13) . . ? Co1 O7 Cu1 122.52(11) . . ? C9 O8 Cu2 115.0(3) . . ? C10 O10 Cu2 113.2(2) . . ? C10 O11 Co1 137.6(3) . 1_455 ? P2 O12 Co2 126.45(15) . . ? P2 O12 Cu2 105.29(13) . . ? Co2 O12 Cu2 119.51(11) . . ? P2 O13 Co1 144.48(17) . 4_566 ? P2 O14 Cu1 135.68(16) . 4_566 ? Co1 O15 H15A 110.7 . . ? Co1 O15 H15B 141.3 . . ? H15A O15 H15B 107.8 . . ? Co1 O16 H16A 131.8 . . ? Co1 O16 H16B 101.2 . . ? H16A O16 H16B 107.8 . . ? Co1 O17 H17A 125.0 . . ? Co1 O17 H17B 123.9 . . ? H17A O17 H17B 107.8 . . ? Co2 O18 H18A 134.4 . . ? Co2 O18 H18B 109.6 . . ? H18A O18 H18B 108.3 . . ? Co2 O19 H19A 100.6 . . ? Co2 O19 H19B 100.2 . . ? H19A O19 H19B 107.5 . . ? Co2 O20 H20A 134.7 . . ? Co2 O20 H20B 116.0 . . ? H20A O20 H20B 107.5 . . ? Co2 O21 H21A 140.3 . . ? Co2 O21 H21B 112.2 . . ? H21A O21 H21B 107.0 . . ? H22A O22 H22B 107.5 . . ? H23A O23 H23B 107.6 . . ? H24A O24 H24B 108.1 . . ? _diffrn_measured_fraction_theta_max 1.000 _diffrn_reflns_theta_full 28.36 _diffrn_measured_fraction_theta_full 1.000 _refine_diff_density_max 2.141 _refine_diff_density_min -1.804 _refine_diff_density_rms 0.139 #===END data_3-CuCd _database_code_depnum_ccdc_archive 'CCDC 742514' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C10 H32 Cd2 Cu2 N2 O24 P2' _chemical_formula_weight 978.20 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' Cd Cd -0.8075 1.2024 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting Monoclinic _symmetry_space_group_name_H-M P2(1)/n _symmetry_space_group_name_Hall '-P 2yn' loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x+1/2, y+1/2, -z+1/2' '-x, -y, -z' 'x-1/2, -y-1/2, z-1/2' _cell_length_a 10.2176(4) _cell_length_b 16.7881(7) _cell_length_c 16.2442(6) _cell_angle_alpha 90.00 _cell_angle_beta 95.647(2) _cell_angle_gamma 90.00 _cell_volume 2772.91(19) _cell_formula_units_Z 4 _cell_measurement_temperature 100(2) _cell_measurement_reflns_used 9867 _cell_measurement_theta_min 2.52 _cell_measurement_theta_max 28.33 _exptl_crystal_description block _exptl_crystal_colour blue _exptl_crystal_size_max 0.30 _exptl_crystal_size_mid 0.26 _exptl_crystal_size_min 0.26 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 2.343 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1928 _exptl_absorpt_coefficient_mu 3.245 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.6418 _exptl_absorpt_correction_T_max 0.6594 _exptl_absorpt_process_details 'SADABS; Bruker, 2000' _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 'Bruker Smart Apex CCD' _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 25780 _diffrn_reflns_av_R_equivalents 0.0257 _diffrn_reflns_av_sigmaI/netI 0.0244 _diffrn_reflns_limit_h_min -13 _diffrn_reflns_limit_h_max 8 _diffrn_reflns_limit_k_min -22 _diffrn_reflns_limit_k_max 22 _diffrn_reflns_limit_l_min -21 _diffrn_reflns_limit_l_max 21 _diffrn_reflns_theta_min 1.75 _diffrn_reflns_theta_max 28.33 _reflns_number_total 6841 _reflns_number_gt 6312 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'SMART (Bruker, 2000)' _computing_cell_refinement SMART _computing_data_reduction 'SAINT (Bruker, 2000)' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics SHELXTL _computing_publication_material 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^)+(0.0465P)^2^+25.2271P] 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 6841 _refine_ls_number_parameters 379 _refine_ls_number_restraints 142 _refine_ls_R_factor_all 0.0481 _refine_ls_R_factor_gt 0.0446 _refine_ls_wR_factor_ref 0.1188 _refine_ls_wR_factor_gt 0.1169 _refine_ls_goodness_of_fit_ref 1.165 _refine_ls_restrained_S_all 1.217 _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 Cd1 Cd 1.14428(4) 0.33033(3) 0.08846(3) 0.01886(11) Uani 1 1 d U . . Cd2 Cd 0.93467(3) 0.31260(2) 0.38595(2) 0.00972(10) Uani 1 1 d U . . Cu1 Cu 1.03883(5) 0.10693(3) 0.05720(3) 0.00650(12) Uani 1 1 d . . . Cu2 Cu 0.66444(6) 0.20865(4) 0.24216(4) 0.00977(13) Uani 1 1 d . . . P1 P 0.95663(12) 0.20851(7) 0.19936(8) 0.0082(2) Uani 1 1 d . . . P2 P 0.62132(12) 0.28116(7) 0.41207(8) 0.0085(2) Uani 1 1 d . . . C1 C 1.0859(5) -0.0135(3) 0.1733(3) 0.0088(8) Uani 1 1 d . . . H1A H 1.0597 -0.0590 0.1366 0.011 Uiso 1 1 calc R . . H1B H 1.0907 -0.0321 0.2314 0.011 Uiso 1 1 calc R . . C2 C 0.8508(4) 0.0222(3) 0.1447(3) 0.0093(9) Uani 1 1 d . . . H2A H 0.8010 0.0386 0.1912 0.011 Uiso 1 1 calc R . . H2B H 0.8508 -0.0367 0.1424 0.011 Uiso 1 1 calc R . . C3 C 1.0046(5) 0.1085(3) 0.2304(3) 0.0091(8) Uani 1 1 d . . . H3A H 1.0977 0.1087 0.2540 0.011 Uiso 1 1 calc R . . H3B H 0.9504 0.0905 0.2741 0.011 Uiso 1 1 calc R . . C4 C 1.2196(5) 0.0184(3) 0.1542(3) 0.0099(9) Uani 1 1 d . . . C5 C 0.7833(5) 0.0548(3) 0.0646(3) 0.0112(9) Uani 1 1 d . . . C6 C 0.4927(6) 0.1132(3) 0.3288(4) 0.0217(12) Uani 1 1 d . . . H6A H 0.4361 0.0759 0.2942 0.026 Uiso 1 1 calc R . . H6B H 0.4569 0.1177 0.3831 0.026 Uiso 1 1 calc R . . C7 C 0.3921(5) 0.2006(4) 0.2151(3) 0.0187(11) Uani 1 1 d . . . H7A H 0.3056 0.2161 0.2328 0.022 Uiso 1 1 calc R . . H7B H 0.3819 0.1488 0.1862 0.022 Uiso 1 1 calc R . . H8A H 0.4421 0.3070 0.3153 0.022 Uiso 1 1 d R . . H8B H 0.4019 0.2438 0.3822 0.022 Uiso 1 1 d R . . C8 C 0.4712(5) 0.2587(3) 0.3469(3) 0.0126(9) Uani 1 1 d . . . C9 C 0.6316(7) 0.0803(3) 0.3413(4) 0.0273(14) Uani 1 1 d . . . C10 C 0.4386(5) 0.2635(4) 0.1570(3) 0.0168(10) Uani 1 1 d . . . N1 N 0.9887(4) 0.0514(2) 0.1599(2) 0.0074(7) Uani 1 1 d . . . N2 N 0.4895(4) 0.1932(3) 0.2882(3) 0.0131(8) Uani 1 1 d . . . O1 O 1.2189(3) 0.0720(2) 0.0996(2) 0.0110(7) Uani 1 1 d U . . O2 O 1.3212(4) -0.0097(2) 0.1919(2) 0.0145(7) Uani 1 1 d U . . O3 O 0.8534(4) 0.0901(2) 0.0150(2) 0.0127(7) Uani 1 1 d U . . O4 O 0.6632(4) 0.0434(2) 0.0502(2) 0.0165(8) Uani 1 1 d U . . O5 O 0.8087(3) 0.2103(2) 0.1751(2) 0.0114(7) Uani 1 1 d U . . O6 O 1.0012(3) 0.2617(2) 0.2719(2) 0.0121(7) Uani 1 1 d U . . O7 O 1.0310(3) 0.2234(2) 0.1239(2) 0.0102(6) Uani 1 1 d U . . O8 O 0.7212(4) 0.1152(3) 0.3056(3) 0.0251(9) Uani 1 1 d U . . O9 O 0.6528(6) 0.0202(3) 0.3845(3) 0.0409(12) Uani 1 1 d U . . O10 O 0.5612(4) 0.2788(2) 0.1645(2) 0.0155(7) Uani 1 1 d U . . O11 O 0.3598(4) 0.2948(3) 0.1038(3) 0.0220(8) Uani 1 1 d U . . O12 O 0.7226(4) 0.2934(2) 0.3497(2) 0.0128(7) Uani 1 1 d U . . O13 O 0.6541(4) 0.2109(2) 0.4669(2) 0.0170(8) Uani 1 1 d U . . O14 O 0.5951(3) 0.3585(2) 0.4551(2) 0.0115(7) Uani 1 1 d U . . O15 O 0.9545(5) 0.3935(3) 0.0475(3) 0.0306(7) Uani 1 1 d U . . H15A H 0.9404 0.4286 0.0833 0.037 Uiso 1 1 d R . . H15B H 0.8871 0.3915 0.0125 0.037 Uiso 1 1 d R . . O16 O 1.2171(5) 0.4582(3) 0.0602(3) 0.0382(8) Uani 1 1 d U . . H16A H 1.2851 0.4833 0.0803 0.046 Uiso 1 1 d R . . H16B H 1.2194 0.4557 0.0081 0.046 Uiso 1 1 d R . . O17 O 1.1827(4) 0.3556(3) 0.2192(3) 0.0227(6) Uani 1 1 d U . . H17A H 1.2492 0.3805 0.2419 0.027 Uiso 1 1 d R . . H17B H 1.1463 0.3318 0.2571 0.027 Uiso 1 1 d R . . O18 O 1.1598(4) 0.3201(2) 0.4157(2) 0.0179(6) Uani 1 1 d U . . H18A H 1.2211 0.2918 0.4396 0.022 Uiso 1 1 d R . . H18B H 1.1771 0.3685 0.4277 0.022 Uiso 1 1 d R . . O19 O 0.9519(5) 0.1877(3) 0.4513(3) 0.0278(7) Uani 1 1 d U . . H19A H 0.8754 0.1838 0.4672 0.033 Uiso 1 1 d R . . H19B H 1.0048 0.1990 0.4934 0.033 Uiso 1 1 d R . . O20 O 0.9328(4) 0.3661(2) 0.5174(2) 0.0136(6) Uani 1 1 d U . . H20A H 0.8702 0.3819 0.5441 0.016 Uiso 1 1 d R . . H20B H 1.0002 0.3599 0.5519 0.016 Uiso 1 1 d R . . O21 O 0.9372(4) 0.4416(2) 0.3428(2) 0.0144(6) Uani 1 1 d U . . H21A H 0.8817 0.4782 0.3292 0.017 Uiso 1 1 d R . . H21B H 1.0136 0.4618 0.3438 0.017 Uiso 1 1 d R . . O22 O 0.7458(5) 0.2940(3) 0.0291(3) 0.0330(11) Uani 1 1 d . . . H22A H 0.7409 0.2751 0.0773 0.040 Uiso 1 1 d R . . H22B H 0.6821 0.2750 -0.0024 0.040 Uiso 1 1 d R . . O23 O 0.0431(9) 0.0283(5) 0.4281(5) 0.076(2) Uani 1 1 d . . . H23A H 0.1265 0.0261 0.4363 0.092 Uiso 1 1 d R . . H23B H 0.0231 0.0696 0.3993 0.092 Uiso 1 1 d R . . O24 O 0.8905(12) 0.9472(5) 0.3388(8) 0.137(6) Uani 1 1 d . . . H24A H 0.8172 0.9665 0.3497 0.164 Uiso 1 1 d R . . H24B H 0.8759 0.9009 0.3186 0.164 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 Cd1 0.0194(2) 0.0218(2) 0.0156(2) -0.00475(15) 0.00302(15) -0.00220(15) Cd2 0.00725(16) 0.01279(18) 0.00935(17) -0.00406(12) 0.00195(12) -0.00129(12) Cu1 0.0073(3) 0.0066(3) 0.0059(3) -0.0004(2) 0.00232(19) -0.00082(19) Cu2 0.0096(3) 0.0096(3) 0.0106(3) -0.0018(2) 0.0031(2) 0.0003(2) P1 0.0089(5) 0.0079(5) 0.0083(5) -0.0029(4) 0.0033(4) -0.0007(4) P2 0.0074(5) 0.0081(5) 0.0101(5) -0.0021(4) 0.0011(4) 0.0000(4) C1 0.008(2) 0.006(2) 0.012(2) -0.0002(17) 0.0030(16) 0.0005(16) C2 0.006(2) 0.010(2) 0.013(2) 0.0001(17) 0.0035(16) -0.0019(16) C3 0.012(2) 0.009(2) 0.007(2) -0.0023(17) 0.0037(16) 0.0001(17) C4 0.008(2) 0.010(2) 0.012(2) -0.0044(17) 0.0031(16) 0.0011(17) C5 0.010(2) 0.009(2) 0.014(2) -0.0010(18) -0.0004(17) -0.0003(17) C6 0.031(3) 0.015(3) 0.019(3) -0.003(2) 0.005(2) -0.014(2) C7 0.012(2) 0.030(3) 0.013(2) -0.005(2) 0.0001(19) -0.009(2) C8 0.009(2) 0.018(2) 0.012(2) -0.0052(19) 0.0028(17) -0.0010(18) C9 0.046(4) 0.010(2) 0.029(3) 0.000(2) 0.020(3) 0.001(2) C10 0.013(2) 0.027(3) 0.010(2) -0.007(2) -0.0012(18) 0.000(2) N1 0.0064(17) 0.0077(18) 0.0082(18) -0.0011(14) 0.0013(14) 0.0005(14) N2 0.0123(19) 0.016(2) 0.011(2) -0.0040(16) 0.0016(15) -0.0059(16) O1 0.0104(10) 0.0112(10) 0.0118(10) 0.0002(8) 0.0029(8) -0.0003(8) O2 0.0130(10) 0.0148(11) 0.0158(11) 0.0002(9) 0.0016(8) 0.0008(8) O3 0.0124(10) 0.0135(10) 0.0121(10) 0.0005(8) 0.0007(8) -0.0013(8) O4 0.0143(11) 0.0172(11) 0.0177(11) 0.0017(9) -0.0001(9) -0.0007(9) O5 0.0109(10) 0.0122(10) 0.0111(10) -0.0010(8) 0.0016(8) 0.0007(8) O6 0.0129(10) 0.0121(10) 0.0114(10) -0.0029(8) 0.0024(8) -0.0012(8) O7 0.0113(10) 0.0097(10) 0.0100(10) -0.0013(8) 0.0031(8) -0.0005(8) O8 0.0262(12) 0.0243(12) 0.0257(12) 0.0022(9) 0.0066(9) 0.0030(9) O9 0.0430(15) 0.0387(15) 0.0416(15) 0.0025(10) 0.0072(10) 0.0014(10) O10 0.0147(11) 0.0165(11) 0.0156(11) 0.0005(9) 0.0020(8) -0.0007(9) O11 0.0210(12) 0.0253(12) 0.0198(12) -0.0001(9) 0.0018(9) 0.0011(9) O12 0.0118(10) 0.0142(10) 0.0127(10) -0.0034(8) 0.0024(8) -0.0012(8) O13 0.0173(11) 0.0155(11) 0.0178(11) 0.0001(9) -0.0001(9) 0.0006(9) O14 0.0134(10) 0.0108(10) 0.0105(10) -0.0003(8) 0.0032(8) 0.0002(8) O15 0.0310(8) 0.0300(12) 0.0304(11) -0.0009(9) 0.0016(8) 0.0039(8) O16 0.0419(11) 0.0349(10) 0.0382(12) 0.0055(9) 0.0061(10) -0.0077(9) O17 0.0231(11) 0.0236(11) 0.0220(7) -0.0051(8) 0.0054(8) -0.0022(9) O18 0.0132(7) 0.0216(11) 0.0187(11) -0.0033(9) -0.0001(8) 0.0012(8) O19 0.0328(12) 0.0227(8) 0.0289(12) 0.0046(8) 0.0087(9) 0.0016(9) O20 0.0131(10) 0.0164(10) 0.0114(8) -0.0018(7) 0.0017(8) 0.0001(8) O21 0.0131(10) 0.0148(8) 0.0156(10) -0.0005(8) 0.0021(8) -0.0002(8) O22 0.030(2) 0.040(3) 0.028(2) 0.005(2) -0.0020(19) 0.000(2) O23 0.088(6) 0.061(5) 0.080(5) 0.016(4) 0.007(4) 0.018(4) O24 0.156(10) 0.034(4) 0.245(14) 0.019(6) 0.146(11) 0.019(5) _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 Cd1 O13 2.105(4) 4_665 ? Cd1 O17 2.164(4) . ? Cd1 O7 2.242(3) . ? Cd1 O15 2.252(5) . ? Cd1 O11 2.272(4) 1_655 ? Cd1 O16 2.332(5) . ? Cd2 O6 2.208(3) . ? Cd2 O12 2.212(4) . ? Cd2 O21 2.277(4) . ? Cd2 O18 2.307(4) . ? Cd2 O20 2.318(4) . ? Cd2 O19 2.349(4) . ? Cu1 O14 1.899(4) 4_665 ? Cu1 O3 1.971(4) . ? Cu1 O1 1.988(4) . ? Cu1 N1 2.021(4) . ? Cu1 O7 2.240(3) . ? Cu2 O5 1.917(4) . ? Cu2 O8 1.934(4) . ? Cu2 O10 1.956(4) . ? Cu2 N2 2.022(4) . ? Cu2 O12 2.286(4) . ? P1 O6 1.512(4) . ? P1 O5 1.524(4) . ? P1 O7 1.525(4) . ? P1 C3 1.807(5) . ? P2 O13 1.496(4) . ? P2 O14 1.511(4) . ? P2 O12 1.532(4) . ? P2 C8 1.815(5) . ? C1 N1 1.476(6) . ? C1 C4 1.528(6) . ? C2 N1 1.490(6) . ? C2 C5 1.514(7) . ? C3 N1 1.489(6) . ? C4 O2 1.245(6) . ? C4 O1 1.263(6) . ? C5 O4 1.242(6) . ? C5 O3 1.274(6) . ? C6 N2 1.495(7) . ? C6 C9 1.518(10) . ? C7 N2 1.477(7) . ? C7 C10 1.524(8) . ? C8 N2 1.480(6) . ? C9 O9 1.236(8) . ? C9 O8 1.275(8) . ? C10 O11 1.238(7) . ? C10 O10 1.273(6) . ? O11 Cd1 2.272(4) 1_455 ? O13 Cd1 2.105(4) 4_566 ? O14 Cu1 1.899(4) 4_566 ? 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 O13 Cd1 O17 164.78(16) 4_665 . ? O13 Cd1 O7 92.96(14) 4_665 . ? O17 Cd1 O7 87.32(15) . . ? O13 Cd1 O15 89.84(16) 4_665 . ? O17 Cd1 O15 105.38(17) . . ? O7 Cd1 O15 90.09(16) . . ? O13 Cd1 O11 83.17(15) 4_665 1_655 ? O17 Cd1 O11 82.15(16) . 1_655 ? O7 Cd1 O11 106.32(14) . 1_655 ? O15 Cd1 O11 162.42(17) . 1_655 ? O13 Cd1 O16 94.13(17) 4_665 . ? O17 Cd1 O16 88.98(18) . . ? O7 Cd1 O16 166.04(16) . . ? O15 Cd1 O16 77.93(19) . . ? O11 Cd1 O16 86.47(18) 1_655 . ? O6 Cd2 O12 95.43(13) . . ? O6 Cd2 O21 95.50(13) . . ? O12 Cd2 O21 95.57(14) . . ? O6 Cd2 O18 79.30(13) . . ? O12 Cd2 O18 173.73(14) . . ? O21 Cd2 O18 88.36(14) . . ? O6 Cd2 O20 162.59(13) . . ? O12 Cd2 O20 101.82(13) . . ? O21 Cd2 O20 85.25(13) . . ? O18 Cd2 O20 83.34(13) . . ? O6 Cd2 O19 91.05(15) . . ? O12 Cd2 O19 91.04(16) . . ? O21 Cd2 O19 170.21(15) . . ? O18 Cd2 O19 85.71(16) . . ? O20 Cd2 O19 86.34(15) . . ? O14 Cu1 O3 95.94(15) 4_665 . ? O14 Cu1 O1 92.49(15) 4_665 . ? O3 Cu1 O1 154.62(15) . . ? O14 Cu1 N1 170.17(16) 4_665 . ? O3 Cu1 N1 84.70(15) . . ? O1 Cu1 N1 83.06(15) . . ? O14 Cu1 O7 100.62(14) 4_665 . ? O3 Cu1 O7 102.37(14) . . ? O1 Cu1 O7 99.51(14) . . ? N1 Cu1 O7 88.79(14) . . ? O5 Cu2 O8 96.16(17) . . ? O5 Cu2 O10 91.19(16) . . ? O8 Cu2 O10 161.05(18) . . ? O5 Cu2 N2 165.83(16) . . ? O8 Cu2 N2 85.90(19) . . ? O10 Cu2 N2 82.86(17) . . ? O5 Cu2 O12 105.55(14) . . ? O8 Cu2 O12 93.20(17) . . ? O10 Cu2 O12 101.64(15) . . ? N2 Cu2 O12 88.29(15) . . ? O6 P1 O5 113.8(2) . . ? O6 P1 O7 113.2(2) . . ? O5 P1 O7 110.4(2) . . ? O6 P1 C3 106.2(2) . . ? O5 P1 C3 109.0(2) . . ? O7 P1 C3 103.5(2) . . ? O13 P2 O14 116.3(2) . . ? O13 P2 O12 111.9(2) . . ? O14 P2 O12 110.7(2) . . ? O13 P2 C8 108.1(2) . . ? O14 P2 C8 105.7(2) . . ? O12 P2 C8 103.3(2) . . ? N1 C1 C4 108.2(4) . . ? N1 C2 C5 111.5(4) . . ? N1 C3 P1 112.2(3) . . ? O2 C4 O1 124.2(5) . . ? O2 C4 C1 119.1(4) . . ? O1 C4 C1 116.7(4) . . ? O4 C5 O3 124.0(5) . . ? O4 C5 C2 117.6(4) . . ? O3 C5 C2 118.3(4) . . ? N2 C6 C9 111.5(5) . . ? N2 C7 C10 109.3(4) . . ? N2 C8 P2 112.2(3) . . ? O9 C9 O8 122.7(7) . . ? O9 C9 C6 118.9(6) . . ? O8 C9 C6 118.4(5) . . ? O11 C10 O10 123.2(5) . . ? O11 C10 C7 120.4(5) . . ? O10 C10 C7 116.4(5) . . ? C1 N1 C3 109.9(4) . . ? C1 N1 C2 113.2(4) . . ? C3 N1 C2 111.7(4) . . ? C1 N1 Cu1 103.9(3) . . ? C3 N1 Cu1 108.7(3) . . ? C2 N1 Cu1 109.1(3) . . ? C7 N2 C8 109.7(4) . . ? C7 N2 C6 114.5(4) . . ? C8 N2 C6 112.5(4) . . ? C7 N2 Cu2 104.0(3) . . ? C8 N2 Cu2 108.4(3) . . ? C6 N2 Cu2 107.3(3) . . ? C4 O1 Cu1 113.2(3) . . ? C5 O3 Cu1 115.3(3) . . ? P1 O5 Cu2 130.7(2) . . ? P1 O6 Cd2 142.1(2) . . ? P1 O7 Cu1 106.89(18) . . ? P1 O7 Cd1 130.4(2) . . ? Cu1 O7 Cd1 122.04(15) . . ? C9 O8 Cu2 115.1(4) . . ? C10 O10 Cu2 113.8(4) . . ? C10 O11 Cd1 138.1(4) . 1_455 ? P2 O12 Cd2 123.5(2) . . ? P2 O12 Cu2 106.27(19) . . ? Cd2 O12 Cu2 117.92(16) . . ? P2 O13 Cd1 142.1(2) . 4_566 ? P2 O14 Cu1 138.5(2) . 4_566 ? _diffrn_measured_fraction_theta_max 0.988 _diffrn_reflns_theta_full 28.33 _diffrn_measured_fraction_theta_full 0.988 _refine_diff_density_max 1.914 _refine_diff_density_min -2.708 _refine_diff_density_rms 0.195 #===END data_4-CuLa _database_code_depnum_ccdc_archive 'CCDC 742515' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C24 H62 Cu4 La4 N4 O55 P4' _chemical_formula_weight 2220.46 loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 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' La La -0.2871 2.4523 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting Monoclinic _symmetry_space_group_name_H-M P2(1)/c _symmetry_space_group_name_Hall '-P 2ybc' loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, y+1/2, -z+1/2' '-x, -y, -z' 'x, -y-1/2, z-1/2' _cell_length_a 8.3028(3) _cell_length_b 20.6398(8) _cell_length_c 9.4630(4) _cell_angle_alpha 90.00 _cell_angle_beta 109.867(2) _cell_angle_gamma 90.00 _cell_volume 1525.14(10) _cell_formula_units_Z 1 _cell_measurement_temperature 100(2) _cell_measurement_reflns_used 9912 _cell_measurement_theta_min 2.49 _cell_measurement_theta_max 28.28 _exptl_crystal_description block _exptl_crystal_colour blue _exptl_crystal_size_max 0.31 _exptl_crystal_size_mid 0.30 _exptl_crystal_size_min 0.28 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 2.418 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1078 _exptl_absorpt_coefficient_mu 4.337 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.5624 _exptl_absorpt_correction_T_max 0.5819 _exptl_absorpt_process_details 'SADABS; Bruker, 2000' _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 'Bruker Smart Apex CCD' _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 22739 _diffrn_reflns_av_R_equivalents 0.0293 _diffrn_reflns_av_sigmaI/netI 0.0225 _diffrn_reflns_limit_h_min -11 _diffrn_reflns_limit_h_max 11 _diffrn_reflns_limit_k_min -23 _diffrn_reflns_limit_k_max 27 _diffrn_reflns_limit_l_min -12 _diffrn_reflns_limit_l_max 12 _diffrn_reflns_theta_min 1.97 _diffrn_reflns_theta_max 28.31 _reflns_number_total 3784 _reflns_number_gt 3562 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'SMART (Bruker, 2000)' _computing_cell_refinement SMART _computing_data_reduction 'SAINT (Bruker, 2000)' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics SHELXTL _computing_publication_material 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^)+(0.0143P)^2^+8.8866P] 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 3784 _refine_ls_number_parameters 224 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0313 _refine_ls_R_factor_gt 0.0290 _refine_ls_wR_factor_ref 0.0664 _refine_ls_wR_factor_gt 0.0656 _refine_ls_goodness_of_fit_ref 1.159 _refine_ls_restrained_S_all 1.159 _refine_ls_shift/su_max 0.005 _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 Cu1 Cu 0.96315(6) 0.29679(2) 1.05105(5) 0.01110(10) Uani 1 1 d . . . La1 La 0.62315(2) 0.148386(10) 1.10107(2) 0.00837(6) Uani 1 1 d . . . P1 P 0.79087(12) 0.19982(5) 0.80559(11) 0.01103(18) Uani 1 1 d . . . C1 C 1.2192(5) 0.18952(19) 0.8225(4) 0.0138(7) Uani 1 1 d . . . C2 C 1.1430(5) 0.12146(19) 0.7922(4) 0.0142(7) Uani 1 1 d . . . H2A H 1.2207 0.0930 0.7608 0.017 Uiso 1 1 calc R . . H2B H 1.1328 0.1035 0.8858 0.017 Uiso 1 1 calc R . . C3 C 0.9440(5) 0.06777(18) 0.5637(4) 0.0130(7) Uani 1 1 d . . . H3A H 0.8938 0.0302 0.5989 0.016 Uiso 1 1 calc R . . H3B H 1.0549 0.0542 0.5557 0.016 Uiso 1 1 calc R . . C4 C 0.8235(5) 0.09003(19) 0.4107(4) 0.0127(7) Uani 1 1 d . . . C5 C 0.8294(5) 0.12177(18) 0.7363(4) 0.0120(7) Uani 1 1 d . . . H5A H 0.8570 0.0904 0.8196 0.014 Uiso 1 1 d R . . H5B H 0.7229 0.1074 0.6575 0.014 Uiso 1 1 d R . . C6 C 0.4308(4) 0.00243(18) 1.0381(4) 0.0117(7) Uani 1 1 d . . . N1 N 0.9713(4) 0.12213(15) 0.6727(3) 0.0108(6) Uani 1 1 d . . . O1 O 1.1575(3) 0.23291(13) 0.7217(3) 0.0137(5) Uani 1 1 d . . . O2 O 1.3416(3) 0.19929(14) 0.9411(3) 0.0149(6) Uani 1 1 d . . . O3 O 0.8007(3) 0.15176(13) 0.3912(3) 0.0122(5) Uani 1 1 d . . . O4 O 0.7552(3) 0.05110(13) 0.3092(3) 0.0159(6) Uani 1 1 d . . . O5 O 0.6433(3) 0.19051(13) 0.8637(3) 0.0130(5) Uani 1 1 d . . . O6 O 0.9565(3) 0.21906(13) 0.9351(3) 0.0129(5) Uani 1 1 d . . . O7 O 0.7516(3) 0.24420(13) 0.6697(3) 0.0114(5) Uani 1 1 d . . . O8 O 0.9516(3) 0.13147(15) 1.1489(3) 0.0206(6) Uani 1 1 d . . . H8A H 1.0106 0.1394 1.2400 0.025 Uiso 1 1 d R . . H8B H 1.0043 0.1475 1.0942 0.025 Uiso 1 1 d R . . O9 O 0.4564(3) 0.19119(14) 1.2643(3) 0.0156(6) Uani 1 1 d . . . H9A H 0.4845 0.2260 1.3147 0.019 Uiso 1 1 d R . . H9B H 0.3478 0.1885 1.2337 0.019 Uiso 1 1 d R . . O10 O 0.4087(3) 0.05738(13) 1.0877(3) 0.0133(5) Uani 1 1 d . . . O11 O 0.6499(4) 0.04802(14) 0.9567(3) 0.0171(6) Uani 1 1 d . . . O12 O 0.0000 0.5000 0.5000 0.064(3) Uani 0.70 2 d SP A 1 H12A H 0.0899 0.5169 0.4922 0.064 Uiso 0.35 1 d PR A 1 H12B H -0.0466 0.5280 0.5397 0.064 Uiso 0.35 1 d PR A 1 O12' O 0.0885(17) 0.4751(6) 0.6349(17) 0.063(4) Uani 0.40 1 d P B 2 H12C H 0.1963 0.4699 0.6610 0.063 Uiso 0.40 1 d PR B 2 H12D H 0.0523 0.4509 0.6902 0.063 Uiso 0.40 1 d PR B 2 O13 O 1.1955(4) 0.34616(17) 0.9491(4) 0.0275(7) Uani 1 1 d . . . H13A H 1.1131 0.3698 0.9164 0.033 Uiso 1 1 d R . . H13B H 1.2132 0.3231 0.8840 0.033 Uiso 1 1 d R . . O14 O 0.3796(7) 0.0415(3) 0.4029(6) 0.0705(16) Uani 1 1 d . . . H14A H 0.4045 0.0494 0.3246 0.085 Uiso 1 1 d R . . H14B H 0.3724 0.0775 0.4438 0.085 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 Cu1 0.0142(2) 0.0088(2) 0.0076(2) -0.00104(16) 0.00022(16) 0.00016(16) La1 0.00975(9) 0.00704(10) 0.00675(10) 0.00005(7) 0.00077(7) -0.00105(7) P1 0.0134(4) 0.0094(4) 0.0095(4) -0.0003(3) 0.0029(3) 0.0010(3) C1 0.0127(16) 0.0167(19) 0.0125(18) 0.0018(14) 0.0048(13) 0.0025(14) C2 0.0128(16) 0.0127(18) 0.0122(18) 0.0006(14) -0.0021(13) 0.0035(14) C3 0.0172(17) 0.0079(16) 0.0109(17) -0.0015(13) 0.0008(13) 0.0021(13) C4 0.0128(16) 0.0124(18) 0.0118(18) -0.0006(14) 0.0027(13) 0.0003(13) C5 0.0172(17) 0.0091(17) 0.0097(17) 0.0009(13) 0.0046(13) -0.0001(13) C6 0.0122(16) 0.0118(17) 0.0085(16) 0.0003(13) 0.0000(12) -0.0008(13) N1 0.0130(14) 0.0089(15) 0.0081(14) -0.0012(11) 0.0007(11) -0.0006(11) O1 0.0130(12) 0.0137(13) 0.0116(13) 0.0015(10) 0.0006(10) -0.0021(10) O2 0.0095(11) 0.0179(14) 0.0138(13) 0.0017(11) -0.0006(10) 0.0004(10) O3 0.0159(12) 0.0098(12) 0.0081(12) 0.0006(10) 0.0004(9) -0.0003(10) O4 0.0191(13) 0.0123(13) 0.0123(13) -0.0003(10) 0.0002(10) -0.0016(11) O5 0.0130(12) 0.0131(13) 0.0121(13) 0.0001(10) 0.0032(10) -0.0003(10) O6 0.0173(12) 0.0100(13) 0.0105(13) -0.0003(10) 0.0034(10) -0.0001(10) O7 0.0139(12) 0.0114(13) 0.0086(12) 0.0020(10) 0.0033(9) 0.0024(10) O8 0.0133(13) 0.0289(17) 0.0169(15) 0.0100(12) 0.0018(11) -0.0039(11) O9 0.0140(12) 0.0168(14) 0.0162(14) -0.0057(11) 0.0053(10) -0.0009(10) O10 0.0139(12) 0.0098(13) 0.0156(14) -0.0018(10) 0.0044(10) -0.0007(10) O11 0.0223(14) 0.0130(14) 0.0201(15) -0.0044(11) 0.0128(11) -0.0081(11) O12 0.038(5) 0.068(7) 0.103(9) -0.057(7) 0.044(6) -0.034(5) O12' 0.069(9) 0.038(7) 0.105(11) -0.030(7) 0.059(8) -0.029(6) O13 0.0235(15) 0.0369(19) 0.0228(17) -0.0066(14) 0.0085(13) 0.0056(14) O14 0.105(4) 0.057(3) 0.077(4) 0.027(3) 0.067(3) 0.032(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 Cu1 O6 1.934(3) . ? Cu1 O1 1.953(3) 4_566 ? Cu1 O3 1.962(3) 4_566 ? Cu1 N1 2.019(3) 4_566 ? Cu1 O13 2.637(3) . ? La1 O7 2.450(3) 4_566 ? La1 O5 2.466(3) . ? La1 O11 2.532(3) . ? La1 O2 2.540(3) 1_455 ? La1 O9 2.557(3) . ? La1 O10 2.562(3) . ? La1 O8 2.632(3) . ? La1 O3 2.639(3) 1_556 ? La1 O4 2.765(3) 1_556 ? La1 C4 3.080(4) 1_556 ? P1 O5 1.517(3) . ? P1 O7 1.521(3) . ? P1 O6 1.551(3) . ? P1 C5 1.808(4) . ? C1 O2 1.248(4) . ? C1 O1 1.282(5) . ? C1 C2 1.527(5) . ? C2 N1 1.488(4) . ? C2 H2A 0.9900 . ? C2 H2B 0.9900 . ? C3 N1 1.488(5) . ? C3 C4 1.525(5) . ? C3 H3A 0.9900 . ? C3 H3B 0.9900 . ? C4 O4 1.233(5) . ? C4 O3 1.292(5) . ? C4 La1 3.080(4) 1_554 ? C5 N1 1.494(5) . ? C5 H5A 0.9848 . ? C5 H5B 0.9886 . ? C6 O11 1.248(5) 3_657 ? C6 O10 1.264(5) . ? C6 C6 1.554(7) 3_657 ? N1 Cu1 2.019(3) 4_565 ? O1 Cu1 1.953(3) 4_565 ? O2 La1 2.540(3) 1_655 ? O3 Cu1 1.962(3) 4_565 ? O3 La1 2.639(3) 1_554 ? O4 La1 2.765(3) 1_554 ? O7 La1 2.450(3) 4_565 ? O8 H8A 0.8501 . ? O8 H8B 0.8500 . ? O9 H9A 0.8501 . ? O9 H9B 0.8499 . ? O11 C6 1.248(5) 3_657 ? O12 H12A 0.8500 . ? O12 H12B 0.8500 . ? O12' H12C 0.8500 . ? O12' H12D 0.8500 . ? O13 H13A 0.8106 . ? O13 H13B 0.8299 . ? O14 H14A 0.8500 . ? O14 H14B 0.8500 . ? 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 O6 Cu1 O1 93.70(11) . 4_566 ? O6 Cu1 O3 97.60(11) . 4_566 ? O1 Cu1 O3 164.94(11) 4_566 4_566 ? O6 Cu1 N1 179.71(13) . 4_566 ? O1 Cu1 N1 86.03(12) 4_566 4_566 ? O3 Cu1 N1 82.65(11) 4_566 4_566 ? O6 Cu1 O13 89.79(11) . . ? O1 Cu1 O13 85.53(11) 4_566 . ? O3 Cu1 O13 84.59(11) 4_566 . ? N1 Cu1 O13 90.08(12) 4_566 . ? O7 La1 O5 76.38(9) 4_566 . ? O7 La1 O11 140.65(9) 4_566 . ? O5 La1 O11 75.63(9) . . ? O7 La1 O2 90.76(9) 4_566 1_455 ? O5 La1 O2 69.20(9) . 1_455 ? O11 La1 O2 104.39(9) . 1_455 ? O7 La1 O9 78.66(9) 4_566 . ? O5 La1 O9 130.27(9) . . ? O11 La1 O9 140.65(9) . . ? O2 La1 O9 68.87(9) 1_455 . ? O7 La1 O10 155.39(9) 4_566 . ? O5 La1 O10 118.33(9) . . ? O11 La1 O10 63.91(9) . . ? O2 La1 O10 77.90(9) 1_455 . ? O9 La1 O10 76.89(9) . . ? O7 La1 O8 75.06(9) 4_566 . ? O5 La1 O8 79.42(9) . . ? O11 La1 O8 73.06(9) . . ? O2 La1 O8 147.91(9) 1_455 . ? O9 La1 O8 133.18(9) . . ? O10 La1 O8 125.00(9) . . ? O7 La1 O3 70.21(8) 4_566 1_556 ? O5 La1 O3 138.71(8) . 1_556 ? O11 La1 O3 117.55(9) . 1_556 ? O2 La1 O3 133.19(9) 1_455 1_556 ? O9 La1 O3 65.67(8) . 1_556 ? O10 La1 O3 101.77(8) . 1_556 ? O8 La1 O3 69.20(9) . 1_556 ? O7 La1 O4 115.90(8) 4_566 1_556 ? O5 La1 O4 140.48(9) . 1_556 ? O11 La1 O4 72.77(9) . 1_556 ? O2 La1 O4 141.87(9) 1_455 1_556 ? O9 La1 O4 89.19(9) . 1_556 ? O10 La1 O4 66.64(8) . 1_556 ? O8 La1 O4 69.16(9) . 1_556 ? O3 La1 O4 48.10(8) 1_556 1_556 ? O7 La1 C4 93.21(9) 4_566 1_556 ? O5 La1 C4 145.30(9) . 1_556 ? O11 La1 C4 94.31(10) . 1_556 ? O2 La1 C4 144.94(10) 1_455 1_556 ? O9 La1 C4 77.81(9) . 1_556 ? O10 La1 C4 84.37(9) . 1_556 ? O8 La1 C4 65.89(9) . 1_556 ? O3 La1 C4 24.59(9) 1_556 1_556 ? O4 La1 C4 23.56(9) 1_556 1_556 ? O5 P1 O7 114.54(15) . . ? O5 P1 O6 110.77(16) . . ? O7 P1 O6 113.06(15) . . ? O5 P1 C5 106.43(17) . . ? O7 P1 C5 104.11(16) . . ? O6 P1 C5 107.21(16) . . ? O2 C1 O1 123.6(4) . . ? O2 C1 C2 118.5(3) . . ? O1 C1 C2 117.8(3) . . ? N1 C2 C1 111.3(3) . . ? N1 C2 H2A 109.4 . . ? C1 C2 H2A 109.4 . . ? N1 C2 H2B 109.4 . . ? C1 C2 H2B 109.4 . . ? H2A C2 H2B 108.0 . . ? N1 C3 C4 109.1(3) . . ? N1 C3 H3A 109.9 . . ? C4 C3 H3A 109.9 . . ? N1 C3 H3B 109.9 . . ? C4 C3 H3B 109.9 . . ? H3A C3 H3B 108.3 . . ? O4 C4 O3 121.7(3) . . ? O4 C4 C3 121.6(3) . . ? O3 C4 C3 116.7(3) . . ? O4 C4 La1 63.7(2) . 1_554 ? O3 C4 La1 58.22(18) . 1_554 ? C3 C4 La1 171.6(3) . 1_554 ? N1 C5 P1 113.7(3) . . ? N1 C5 H5A 108.9 . . ? P1 C5 H5A 108.5 . . ? N1 C5 H5B 108.8 . . ? P1 C5 H5B 108.5 . . ? H5A C5 H5B 108.2 . . ? O11 C6 O10 125.9(4) 3_657 . ? O11 C6 C6 117.1(4) 3_657 3_657 ? O10 C6 C6 117.0(4) . 3_657 ? C3 N1 C2 113.6(3) . . ? C3 N1 C5 108.7(3) . . ? C2 N1 C5 112.1(3) . . ? C3 N1 Cu1 105.2(2) . 4_565 ? C2 N1 Cu1 106.2(2) . 4_565 ? C5 N1 Cu1 110.8(2) . 4_565 ? C1 O1 Cu1 113.9(2) . 4_565 ? C1 O2 La1 140.5(3) . 1_655 ? C4 O3 Cu1 113.3(2) . 4_565 ? C4 O3 La1 97.2(2) . 1_554 ? Cu1 O3 La1 144.20(13) 4_565 1_554 ? C4 O4 La1 92.7(2) . 1_554 ? P1 O5 La1 133.49(15) . . ? P1 O6 Cu1 120.48(16) . . ? P1 O7 La1 135.90(15) . 4_565 ? La1 O8 H8A 110.8 . . ? La1 O8 H8B 124.1 . . ? H8A O8 H8B 107.7 . . ? La1 O9 H9A 122.0 . . ? La1 O9 H9B 120.1 . . ? H9A O9 H9B 107.7 . . ? C6 O10 La1 119.3(2) . . ? C6 O11 La1 121.0(2) 3_657 . ? H12A O12 H12B 107.7 . . ? H12C O12' H12D 107.7 . . ? Cu1 O13 H13A 75.2 . . ? Cu1 O13 H13B 112.7 . . ? H13A O13 H13B 113.6 . . ? H14A O14 H14B 107.7 . . ? _diffrn_measured_fraction_theta_max 0.998 _diffrn_reflns_theta_full 28.31 _diffrn_measured_fraction_theta_full 0.998 _refine_diff_density_max 1.871 _refine_diff_density_min -1.148 _refine_diff_density_rms 0.143 #===END data_5-CuNd _database_code_depnum_ccdc_archive 'CCDC 742516' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C24 H62 Cu4 N4 Nd4 O55 P4' _chemical_formula_weight 2241.78 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' Nd Nd -0.1943 3.0179 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting Monoclinic _symmetry_space_group_name_H-M P2(1)/c loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, y+1/2, -z+1/2' '-x, -y, -z' 'x, -y-1/2, z-1/2' _cell_length_a 8.2368(2) _cell_length_b 20.3660(5) _cell_length_c 9.4063(2) _cell_angle_alpha 90.00 _cell_angle_beta 110.2860(10) _cell_angle_gamma 90.00 _cell_volume 1480.04(6) _cell_formula_units_Z 1 _cell_measurement_temperature 100(2) _cell_measurement_reflns_used 8592 _cell_measurement_theta_min 2.84 _cell_measurement_theta_max 28.41 _exptl_crystal_description block _exptl_crystal_colour blue _exptl_crystal_size_max 0.22 _exptl_crystal_size_mid 0.20 _exptl_crystal_size_min 0.18 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 2.515 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1090 _exptl_absorpt_coefficient_mu 5.090 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.4782 _exptl_absorpt_correction_T_max 0.5156 _exptl_absorpt_process_details 'SADABS; Bruker, 2000' _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 'Bruker Smart Apex CCD' _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 14194 _diffrn_reflns_av_R_equivalents 0.0223 _diffrn_reflns_av_sigmaI/netI 0.0209 _diffrn_reflns_limit_h_min -11 _diffrn_reflns_limit_h_max 10 _diffrn_reflns_limit_k_min -27 _diffrn_reflns_limit_k_max 23 _diffrn_reflns_limit_l_min -11 _diffrn_reflns_limit_l_max 12 _diffrn_reflns_theta_min 2.00 _diffrn_reflns_theta_max 28.42 _reflns_number_total 3688 _reflns_number_gt 3458 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'SMART (Bruker, 2000)' _computing_cell_refinement SMART _computing_data_reduction 'SAINT (Bruker, 2000)' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics SHELXTL _computing_publication_material 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^)+(0.0219P)^2^+6.1436P] 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 3688 _refine_ls_number_parameters 223 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0253 _refine_ls_R_factor_gt 0.0235 _refine_ls_wR_factor_ref 0.0584 _refine_ls_wR_factor_gt 0.0576 _refine_ls_goodness_of_fit_ref 1.076 _refine_ls_restrained_S_all 1.076 _refine_ls_shift/su_max 0.011 _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 Cu1 Cu 0.96034(5) 0.297092(19) 1.04591(4) 0.01111(9) Uani 1 1 d . . . Nd1 Nd 0.61932(2) 0.148084(8) 1.097201(17) 0.00693(5) Uani 1 1 d . . . P1 P 0.78227(11) 0.19938(4) 0.80036(9) 0.00992(15) Uani 1 1 d . . . C1 C 1.2174(4) 0.18958(16) 0.8204(4) 0.0120(6) Uani 1 1 d . . . C2 C 1.1387(4) 0.12100(16) 0.7909(4) 0.0120(6) Uani 1 1 d . . . H2A H 1.2173 0.0914 0.7618 0.014 Uiso 1 1 calc R . . H2B H 1.1265 0.1037 0.8850 0.014 Uiso 1 1 calc R . . C3 C 0.9400(4) 0.06678(15) 0.5596(3) 0.0112(6) Uani 1 1 d . . . H3A H 0.8893 0.0287 0.5949 0.013 Uiso 1 1 calc R . . H3B H 1.0526 0.0532 0.5533 0.013 Uiso 1 1 calc R . . C4 C 0.8191(4) 0.08864(16) 0.4043(4) 0.0112(6) Uani 1 1 d . . . C5 C 0.8201(4) 0.12087(15) 0.7284(4) 0.0106(6) Uani 1 1 d . . . H5A H 0.8478 0.0895 0.8116 0.013 Uiso 1 1 d R . . H5B H 0.7136 0.1066 0.6496 0.013 Uiso 1 1 d R . . C6 C 0.4304(4) 0.00264(16) 1.0380(3) 0.0102(6) Uani 1 1 d . . . N1 N 0.9659(3) 0.12175(13) 0.6679(3) 0.0094(5) Uani 1 1 d . . . O1 O 1.1560(3) 0.23333(11) 0.7188(3) 0.0121(4) Uani 1 1 d . . . O2 O 1.3417(3) 0.19970(12) 0.9410(3) 0.0128(4) Uani 1 1 d . . . O3 O 0.7960(3) 0.15119(11) 0.3832(3) 0.0126(4) Uani 1 1 d . . . O4 O 0.7515(3) 0.04930(12) 0.3017(3) 0.0145(5) Uani 1 1 d . . . O5 O 0.6372(3) 0.18955(11) 0.8619(3) 0.0113(4) Uani 1 1 d . . . O6 O 0.9522(3) 0.21860(11) 0.9292(3) 0.0121(4) Uani 1 1 d . . . O7 O 0.7390(3) 0.24497(11) 0.6646(3) 0.0111(4) Uani 1 1 d . . . O8 O 0.9423(3) 0.13107(13) 1.1433(3) 0.0179(5) Uani 1 1 d . . . H8A H 1.0012 0.1390 1.2344 0.022 Uiso 1 1 d R . . H8B H 0.9949 0.1471 1.0886 0.022 Uiso 1 1 d R . . O9 O 0.4540(3) 0.18818(12) 1.2594(3) 0.0136(5) Uani 1 1 d . . . H9A H 0.4820 0.2230 1.3098 0.016 Uiso 1 1 d R . . H9B H 0.3454 0.1854 1.2288 0.016 Uiso 1 1 d R . . O10 O 0.4064(3) 0.05853(11) 1.0854(3) 0.0115(4) Uani 1 1 d . . . O11 O 0.6482(3) 0.04905(11) 0.9550(3) 0.0146(5) Uani 1 1 d . . . O12 O 0.0000 0.5000 0.5000 0.039(2) Uani 0.70 2 d SP A 1 H12A H 0.0899 0.5169 0.4922 0.039 Uiso 0.35 1 d PR A 1 H12B H -0.0466 0.5280 0.5397 0.039 Uiso 0.35 1 d PR A 1 O12' O 0.074(2) 0.4769(8) 0.619(2) 0.139(10) Uani 0.40 1 d P B 2 H12C H 0.1817 0.4717 0.6456 0.139 Uiso 0.40 1 d PR B 2 H12D H 0.0377 0.4526 0.6747 0.139 Uiso 0.40 1 d PR B 2 O13 O 1.1933(4) 0.34655(14) 0.9461(3) 0.0239(6) Uani 1 1 d . . . H13A H 1.1110 0.3702 0.9134 0.029 Uiso 1 1 d R . . H13B H 1.2111 0.3235 0.8810 0.029 Uiso 1 1 d R . . O14 O 0.3784(5) 0.04127(18) 0.4002(4) 0.0491(10) Uani 1 1 d . . . H14A H 0.4032 0.0492 0.3219 0.059 Uiso 1 1 d R . . H14B H 0.3711 0.0773 0.4411 0.059 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 Cu1 0.01365(19) 0.00979(18) 0.00805(17) -0.00108(14) 0.00142(15) 0.00056(14) Nd1 0.00809(9) 0.00615(8) 0.00576(8) -0.00014(5) 0.00140(6) -0.00099(6) P1 0.0121(4) 0.0091(4) 0.0085(4) 0.0005(3) 0.0035(3) 0.0013(3) C1 0.0091(14) 0.0154(15) 0.0108(14) 0.0014(12) 0.0025(12) -0.0002(12) C2 0.0130(15) 0.0111(14) 0.0091(14) 0.0003(12) 0.0002(12) 0.0020(12) C3 0.0138(15) 0.0097(14) 0.0072(13) -0.0016(11) -0.0002(12) 0.0022(12) C4 0.0112(14) 0.0128(15) 0.0103(14) 0.0017(12) 0.0045(12) 0.0024(12) C5 0.0146(15) 0.0081(14) 0.0095(14) -0.0003(11) 0.0046(12) -0.0014(11) C6 0.0095(14) 0.0121(14) 0.0073(13) 0.0009(11) 0.0006(11) -0.0013(11) N1 0.0105(12) 0.0100(12) 0.0073(11) -0.0014(10) 0.0024(10) 0.0008(10) O1 0.0107(11) 0.0131(11) 0.0109(10) 0.0017(9) 0.0020(9) -0.0018(9) O2 0.0099(11) 0.0152(11) 0.0109(11) 0.0014(9) 0.0004(9) 0.0005(9) O3 0.0157(12) 0.0113(11) 0.0088(10) 0.0013(8) 0.0018(9) 0.0017(9) O4 0.0147(11) 0.0148(11) 0.0107(11) -0.0013(9) 0.0002(9) -0.0010(9) O5 0.0127(11) 0.0121(11) 0.0091(10) 0.0003(8) 0.0037(9) 0.0010(9) O6 0.0143(11) 0.0107(10) 0.0104(10) -0.0015(9) 0.0029(9) 0.0006(9) O7 0.0148(11) 0.0101(10) 0.0085(10) 0.0014(8) 0.0040(9) 0.0021(9) O8 0.0137(12) 0.0273(14) 0.0119(11) 0.0054(10) 0.0034(10) -0.0028(10) O9 0.0113(11) 0.0152(11) 0.0137(11) -0.0051(9) 0.0034(9) -0.0009(9) O10 0.0116(11) 0.0102(10) 0.0123(11) -0.0007(8) 0.0039(9) -0.0002(8) O11 0.0196(12) 0.0102(11) 0.0176(12) -0.0038(9) 0.0108(10) -0.0065(9) O12 0.025(4) 0.047(5) 0.048(5) -0.030(4) 0.016(4) -0.012(3) O12' 0.143(18) 0.087(13) 0.26(3) -0.106(16) 0.16(2) -0.078(13) O13 0.0229(14) 0.0283(15) 0.0222(14) -0.0047(11) 0.0101(12) 0.0038(11) O14 0.075(3) 0.0360(19) 0.055(2) 0.0138(17) 0.047(2) 0.0160(18) _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 Cu1 O6 1.927(2) . ? Cu1 O1 1.952(2) 4_566 ? Cu1 O3 1.962(2) 4_566 ? Cu1 N1 2.004(3) 4_566 ? Cu1 O13 2.613(3) . ? Nd1 O7 2.384(2) 4_566 ? Nd1 O5 2.420(2) . ? Nd1 O11 2.477(2) . ? Nd1 O2 2.483(2) 1_455 ? Nd1 O10 2.506(2) . ? Nd1 O9 2.508(2) . ? Nd1 O8 2.566(2) . ? Nd1 O3 2.577(2) 1_556 ? Nd1 O4 2.735(2) 1_556 ? Nd1 C4 3.037(3) 1_556 ? P1 O5 1.511(2) . ? P1 O7 1.518(2) . ? P1 O6 1.550(2) . ? P1 C5 1.805(3) . ? C1 O2 1.254(4) . ? C1 O1 1.276(4) . ? C1 C2 1.524(5) . ? C2 N1 1.490(4) . ? C2 H2A 0.9900 . ? C2 H2B 0.9900 . ? C3 N1 1.479(4) . ? C3 C4 1.522(4) . ? C3 H3A 0.9900 . ? C3 H3B 0.9900 . ? C4 O4 1.229(4) . ? C4 O3 1.293(4) . ? C4 Nd1 3.037(3) 1_554 ? C5 N1 1.496(4) . ? C5 H5A 0.9746 . ? C5 H5B 0.9763 . ? C6 O11 1.249(4) 3_657 ? C6 O10 1.263(4) . ? C6 C6 1.551(6) 3_657 ? N1 Cu1 2.004(3) 4_565 ? O1 Cu1 1.952(2) 4_565 ? O2 Nd1 2.483(2) 1_655 ? O3 Cu1 1.962(2) 4_565 ? O3 Nd1 2.577(2) 1_554 ? O4 Nd1 2.735(2) 1_554 ? O7 Nd1 2.384(2) 4_565 ? O8 H8A 0.8411 . ? O8 H8B 0.8452 . ? O9 H9A 0.8397 . ? O9 H9B 0.8411 . ? O11 C6 1.249(4) 3_657 ? O12 H12A 0.8430 . ? O12 H12B 0.8428 . ? O12' H12C 0.8414 . ? O12' H12D 0.8437 . ? O13 H13A 0.8009 . ? O13 H13B 0.8236 . ? O14 H14A 0.8457 . ? O14 H14B 0.8404 . ? 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 O6 Cu1 O1 93.85(10) . 4_566 ? O6 Cu1 O3 97.04(10) . 4_566 ? O1 Cu1 O3 165.42(10) 4_566 4_566 ? O6 Cu1 N1 179.19(10) . 4_566 ? O1 Cu1 N1 86.34(10) 4_566 4_566 ? O3 Cu1 N1 82.91(10) 4_566 4_566 ? O6 Cu1 O13 90.00(9) . . ? O1 Cu1 O13 85.69(9) 4_566 . ? O3 Cu1 O13 84.65(9) 4_566 . ? N1 Cu1 O13 90.80(10) 4_566 . ? O7 Nd1 O5 76.93(8) 4_566 . ? O7 Nd1 O11 141.20(7) 4_566 . ? O5 Nd1 O11 75.09(8) . . ? O7 Nd1 O2 88.94(8) 4_566 1_455 ? O5 Nd1 O2 69.30(8) . 1_455 ? O11 Nd1 O2 105.45(8) . 1_455 ? O7 Nd1 O10 153.53(7) 4_566 . ? O5 Nd1 O10 118.47(8) . . ? O11 Nd1 O10 65.17(7) . . ? O2 Nd1 O10 78.17(8) 1_455 . ? O7 Nd1 O9 78.60(8) 4_566 . ? O5 Nd1 O9 131.34(8) . . ? O11 Nd1 O9 140.15(8) . . ? O2 Nd1 O9 68.84(8) 1_455 . ? O10 Nd1 O9 75.21(7) . . ? O7 Nd1 O8 76.69(8) 4_566 . ? O5 Nd1 O8 79.26(8) . . ? O11 Nd1 O8 72.14(8) . . ? O2 Nd1 O8 147.72(8) 1_455 . ? O10 Nd1 O8 125.29(8) . . ? O9 Nd1 O8 133.70(8) . . ? O7 Nd1 O3 70.63(7) 4_566 1_556 ? O5 Nd1 O3 138.98(8) . 1_556 ? O11 Nd1 O3 117.29(8) . 1_556 ? O2 Nd1 O3 132.70(7) 1_455 1_556 ? O10 Nd1 O3 101.39(7) . 1_556 ? O9 Nd1 O3 65.57(8) . 1_556 ? O8 Nd1 O3 69.50(8) . 1_556 ? O7 Nd1 O4 117.25(7) 4_566 1_556 ? O5 Nd1 O4 139.84(7) . 1_556 ? O11 Nd1 O4 72.04(8) . 1_556 ? O2 Nd1 O4 142.00(7) 1_455 1_556 ? O10 Nd1 O4 66.27(7) . 1_556 ? O9 Nd1 O4 88.81(7) . 1_556 ? O8 Nd1 O4 69.23(7) . 1_556 ? O3 Nd1 O4 48.77(7) 1_556 1_556 ? O7 Nd1 C4 94.22(8) 4_566 1_556 ? O5 Nd1 C4 145.52(8) . 1_556 ? O11 Nd1 C4 93.86(8) . 1_556 ? O2 Nd1 C4 144.67(8) 1_455 1_556 ? O10 Nd1 C4 83.81(8) . 1_556 ? O9 Nd1 C4 77.32(8) . 1_556 ? O8 Nd1 C4 66.26(8) . 1_556 ? O3 Nd1 C4 24.95(8) 1_556 1_556 ? O4 Nd1 C4 23.86(8) 1_556 1_556 ? O5 P1 O7 114.64(13) . . ? O5 P1 O6 110.69(13) . . ? O7 P1 O6 112.85(13) . . ? O5 P1 C5 106.78(14) . . ? O7 P1 C5 104.30(14) . . ? O6 P1 C5 106.88(14) . . ? O2 C1 O1 123.4(3) . . ? O2 C1 C2 118.5(3) . . ? O1 C1 C2 118.1(3) . . ? N1 C2 C1 111.3(3) . . ? N1 C2 H2A 109.4 . . ? C1 C2 H2A 109.4 . . ? N1 C2 H2B 109.4 . . ? C1 C2 H2B 109.4 . . ? H2A C2 H2B 108.0 . . ? N1 C3 C4 109.3(3) . . ? N1 C3 H3A 109.8 . . ? C4 C3 H3A 109.8 . . ? N1 C3 H3B 109.8 . . ? C4 C3 H3B 109.8 . . ? H3A C3 H3B 108.3 . . ? O4 C4 O3 121.3(3) . . ? O4 C4 C3 122.0(3) . . ? O3 C4 C3 116.6(3) . . ? O4 C4 Nd1 64.19(17) . 1_554 ? O3 C4 Nd1 57.23(16) . 1_554 ? C3 C4 Nd1 171.2(2) . 1_554 ? N1 C5 P1 113.4(2) . . ? N1 C5 H5A 108.6 . . ? P1 C5 H5A 107.6 . . ? N1 C5 H5B 110.1 . . ? P1 C5 H5B 108.8 . . ? H5A C5 H5B 108.2 . . ? O11 C6 O10 126.4(3) 3_657 . ? O11 C6 C6 116.4(3) 3_657 3_657 ? O10 C6 C6 117.1(3) . 3_657 ? C3 N1 C2 113.4(2) . . ? C3 N1 C5 108.0(2) . . ? C2 N1 C5 112.4(2) . . ? C3 N1 Cu1 105.12(19) . 4_565 ? C2 N1 Cu1 106.20(19) . 4_565 ? C5 N1 Cu1 111.43(19) . 4_565 ? C1 O1 Cu1 113.6(2) . 4_565 ? C1 O2 Nd1 139.6(2) . 1_655 ? C4 O3 Cu1 112.6(2) . 4_565 ? C4 O3 Nd1 97.82(19) . 1_554 ? Cu1 O3 Nd1 144.56(11) 4_565 1_554 ? C4 O4 Nd1 91.96(19) . 1_554 ? P1 O5 Nd1 134.69(13) . . ? P1 O6 Cu1 119.91(14) . . ? P1 O7 Nd1 137.51(13) . 4_565 ? Nd1 O8 H8A 110.2 . . ? Nd1 O8 H8B 124.4 . . ? H8A O8 H8B 108.0 . . ? Nd1 O9 H9A 121.1 . . ? Nd1 O9 H9B 120.5 . . ? H9A O9 H9B 107.5 . . ? C6 O10 Nd1 118.63(19) . . ? C6 O11 Nd1 120.6(2) 3_657 . ? H12A O12 H12B 108.1 . . ? H12B O12' H12C 134.7 . . ? H12B O12' H12D 114.4 . . ? H12C O12' H12D 108.0 . . ? Cu1 O13 H13A 74.9 . . ? Cu1 O13 H13B 112.9 . . ? H13A O13 H13B 113.7 . . ? H14A O14 H14B 108.0 . . ? _diffrn_measured_fraction_theta_max 0.989 _diffrn_reflns_theta_full 28.42 _diffrn_measured_fraction_theta_full 0.989 _refine_diff_density_max 1.550 _refine_diff_density_min -1.174 _refine_diff_density_rms 0.137