# Electronic Supplementary Material (ESI) for CrystEngComm # This journal is © The Royal Society of Chemistry 2011 data_global _journal_name_full CrystEngComm _journal_coden_cambridge 1350 _publ_contact_author_name 'Gui-lin Zhuang' _publ_contact_author_address ; College of Chemical Engineering and Materials Science Zhejiang University of Technology Hangzhou 310014 Zhejiang People's Republic of China ; _publ_contact_author_email glzhuang@zjut.edu.cn _publ_contact_author_fax 86-571-88871037 _publ_contact_author_phone 86-571-88871037 loop_ _publ_author_name _publ_author_address 'Gui-lin Zhuang' ; College of Chemical Engineering and Materials Science Zhejiang University of Technology Hangzhou 310014 Zhejiang People's Republic of China ; 'Wen-xian Chen' ; College of Chemical Engineering and Materials Science Zhejiang University of Technology Hangzhou 310014 Zhejiang People's Republic of China ; 'Gan-ning Zeng' ; College of Chemical Engineering and Materials Science Zhejiang University of Technology Hangzhou 310014 Zhejiang People's Republic of China ; 'Jian-guo Wang' ; College of Chemical Engineering and Materials Science Zhejiang University of Technology Hangzhou 310014 Zhejiang People's Republic of China ; ; Wu-lin Chen ; ; College of Chemical Engineering and Materials Science Zhejiang University of Technology Hangzhou 310014 Zhejiang People's Republic of China ; _publ_section_title ; Position of Substituent Dependent Dimensionality in Ln-Cu Heterometallic Coordination Polymers ; # Attachment 'complex1.cif' #TrackingRef 'complex1.cif' data_complex1 _database_code_depnum_ccdc_archive 'CCDC 834764' #TrackingRef 'complex1.cif' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C30 H48 Cu3 La2 N6 O27' _chemical_formula_weight 1393.18 loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Cu Cu 0.3201 1.2651 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' La La -0.2871 2.4523 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting Trigonal _symmetry_space_group_name_H-M P-3 loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-y, x-y, z' '-x+y, -x, z' '-x, -y, -z' 'y, -x+y, -z' 'x-y, x, -z' _cell_length_a 13.6224(3) _cell_length_b 13.6224(3) _cell_length_c 7.4935(3) _cell_angle_alpha 90.00 _cell_angle_beta 90.00 _cell_angle_gamma 120.00 _cell_volume 1204.27(6) _cell_formula_units_Z 1 _cell_measurement_temperature 173(2) _cell_measurement_reflns_used ? _cell_measurement_theta_min ? _cell_measurement_theta_max ? _exptl_crystal_description block _exptl_crystal_colour blue _exptl_crystal_size_max 0.35 _exptl_crystal_size_mid 0.30 _exptl_crystal_size_min 0.25 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.921 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 687 _exptl_absorpt_coefficient_mu 3.131 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.4070 _exptl_absorpt_correction_T_max 0.5082 _exptl_absorpt_process_details 'CrysAlis RED' _exptl_special_details ; CrysAlis RED, Oxford Diffraction Ltd., Version 1.171.32.5 (release 08-05-2007 CrysAlis171 .NET) (compiled May 8 2007,13:10:02) Empirical absorption correction using spherical harmonics, implemented in SCALE3 ABSPACK scaling algorithm. ; _diffrn_ambient_temperature 173(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'Enhance (Mo) X-ray Source' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'CrysAlis CCD, Oxford Diffraction Ltd.' _diffrn_measurement_method \w _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 9049 _diffrn_reflns_av_R_equivalents 0.0249 _diffrn_reflns_av_sigmaI/netI 0.0192 _diffrn_reflns_limit_h_min -16 _diffrn_reflns_limit_h_max 17 _diffrn_reflns_limit_k_min -17 _diffrn_reflns_limit_k_max 17 _diffrn_reflns_limit_l_min -9 _diffrn_reflns_limit_l_max 8 _diffrn_reflns_theta_min 2.72 _diffrn_reflns_theta_max 26.98 _reflns_number_total 1748 _reflns_number_gt 1636 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'CrysAlis CCD' _computing_cell_refinement 'CrysAlis RED' _computing_data_reduction 'CrysAlis RED' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'SHELXL-97 (Sheldrick, 1997)' _computing_publication_material 'SHELXL-97 (Sheldrick, 1997)' _refine_special_details ; Refinement of F^2^ against ALL reflections. The weighted R-factor wR and goodness of fit S are based on F^2^, conventional R-factors R are based on F, with F set to zero for negative F^2^. The threshold expression of F^2^ > 2sigma(F^2^) is used only for calculating R-factors(gt) etc. and is not relevant to the choice of reflections for refinement. R-factors based on F^2^ are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger. ; _refine_ls_structure_factor_coef Fsqd _refine_ls_matrix_type full _refine_ls_weighting_scheme calc _refine_ls_weighting_details 'calc w=1/[\s^2^(Fo^2^)+(0.0414P)^2^+1.0921P] 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 1748 _refine_ls_number_parameters 118 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0271 _refine_ls_R_factor_gt 0.0248 _refine_ls_wR_factor_ref 0.0682 _refine_ls_wR_factor_gt 0.0677 _refine_ls_goodness_of_fit_ref 1.101 _refine_ls_restrained_S_all 1.101 _refine_ls_shift/su_max 0.061 _refine_ls_shift/su_mean 0.002 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 La1 La 0.6667 0.3333 1.65898(2) 0.01754(5) Uani 1 3 d S . . Cu1 Cu 1.0000 0.5000 1.0000 0.02318(9) Uani 1 2 d S . . O1 O 0.75848(14) 0.55783(15) 0.7581(3) 0.0418(5) Uani 1 1 d . . . O2 O 0.82035(12) 0.45368(13) 0.8827(2) 0.0322(4) Uani 1 1 d . . . O3 O 0.92318(13) 0.40795(14) 1.2114(2) 0.0360(4) Uani 1 1 d . . . O4 O 0.82233(16) 0.40055(18) 1.4481(2) 0.0524(5) Uani 1 1 d . . . N1 N 0.96406(14) 0.61369(15) 1.1059(2) 0.0267(4) Uani 1 1 d . . . H1A H 1.0319 0.6769 1.1399 0.032 Uiso 1 1 calc R . . C1 C 0.82258(17) 0.54659(19) 0.8635(3) 0.0292(5) Uani 1 1 d . . . C2 C 0.9107(2) 0.6498(2) 0.9679(4) 0.0445(7) Uani 1 1 d . . . H2A H 0.8577 0.6606 1.0469 0.053 Uiso 1 1 calc R . . C3 C 0.8944(2) 0.5648(2) 1.2678(4) 0.0447(7) Uani 1 1 d . . . H3A H 0.8169 0.5481 1.2316 0.054 Uiso 1 1 calc R . . C4 C 0.87964(18) 0.4498(2) 1.3129(3) 0.0328(6) Uani 1 1 d . . . C5 C 0.9288(6) 0.6530(5) 1.4099(7) 0.0500(17) Uani 0.50 1 d P . . H5B H 0.9345 0.7219 1.3586 0.075 Uiso 0.50 1 calc PR . . H5C H 1.0025 0.6705 1.4589 0.075 Uiso 0.50 1 calc PR . . H5D H 0.8720 0.6246 1.5053 0.075 Uiso 0.50 1 calc PR . . C6 C 0.9565(9) 0.7412(7) 0.8974(17) 0.121(4) Uani 0.50 1 d P . . H6A H 1.0101 0.7980 0.9810 0.181 Uiso 0.50 1 calc PR . . H6B H 0.8994 0.7612 0.8624 0.181 Uiso 0.50 1 calc PR . . H6C H 0.9972 0.7389 0.7911 0.181 Uiso 0.50 1 calc PR . . O1W O 1.0844(11) 0.800(2) 1.511(3) 0.829(13) Uani 0.50 1 d P . . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 La1 0.02047(6) 0.02047(6) 0.01168(9) 0.000 0.000 0.01024(3) Cu1 0.02021(13) 0.03179(16) 0.01811(18) 0.00588(12) 0.00502(12) 0.01342(11) O1 0.0389(7) 0.0476(8) 0.0458(10) -0.0021(8) -0.0117(7) 0.0268(6) O2 0.0289(6) 0.0287(6) 0.0384(9) -0.0080(6) -0.0105(7) 0.0141(5) O3 0.0374(7) 0.0490(8) 0.0292(8) 0.0169(7) 0.0156(6) 0.0272(6) O4 0.0537(9) 0.0751(11) 0.0345(10) 0.0233(8) 0.0268(8) 0.0368(8) N1 0.0195(7) 0.0294(8) 0.0237(9) -0.0014(7) -0.0001(7) 0.0066(6) C1 0.0231(8) 0.0364(10) 0.0306(12) -0.0031(9) -0.0025(8) 0.0168(7) C2 0.0596(12) 0.0333(10) 0.0483(15) -0.0103(10) -0.0205(12) 0.0290(9) C3 0.0446(12) 0.0430(12) 0.0407(14) 0.0007(11) 0.0203(11) 0.0175(10) C4 0.0261(9) 0.0483(12) 0.0223(11) 0.0079(9) 0.0065(8) 0.0175(8) C5 0.078(3) 0.038(2) 0.019(2) -0.0019(19) 0.022(2) 0.017(2) C6 0.120(6) 0.062(5) 0.149(9) -0.011(5) -0.078(6) 0.022(5) O1W 0.189(8) 1.68(3) 0.556(16) -0.821(17) -0.153(10) 0.424(14) _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 La1 O4 2.4271(18) . ? La1 O4 2.4271(18) 3_665 ? La1 O4 2.4271(18) 2_655 ? La1 O2 2.5397(15) 3_666 ? La1 O2 2.5397(15) 1_556 ? La1 O2 2.5397(15) 2_656 ? La1 O1 2.7647(19) 3_666 ? La1 O1 2.7647(19) 2_656 ? La1 O1 2.7647(19) 1_556 ? La1 C1 3.022(2) 3_666 ? La1 C1 3.022(2) 1_556 ? La1 C1 3.022(2) 2_656 ? Cu1 O3 1.9661(16) 4_767 ? Cu1 O3 1.9661(16) . ? Cu1 N1 2.007(2) . ? Cu1 N1 2.007(2) 4_767 ? Cu1 O2 2.3696(16) . ? Cu1 O2 2.3696(16) 4_767 ? O1 C1 1.242(3) . ? O1 La1 2.7647(18) 1_554 ? O2 C1 1.259(3) . ? O2 La1 2.5397(15) 1_554 ? O3 C4 1.262(3) . ? O4 C4 1.249(3) . ? N1 C3 1.478(3) . ? N1 C2 1.483(3) . ? C1 C2 1.530(3) . ? C1 La1 3.022(2) 1_554 ? C2 C6 1.201(10) . ? C3 C5 1.495(6) . ? C3 C4 1.514(4) . ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag O4 La1 O4 82.19(7) . 3_665 ? O4 La1 O4 82.19(7) . 2_655 ? O4 La1 O4 82.19(7) 3_665 2_655 ? O4 La1 O2 120.22(7) . 3_666 ? O4 La1 O2 84.47(6) 3_665 3_666 ? O4 La1 O2 151.98(7) 2_655 3_666 ? O4 La1 O2 84.47(6) . 1_556 ? O4 La1 O2 151.98(7) 3_665 1_556 ? O4 La1 O2 120.22(7) 2_655 1_556 ? O2 La1 O2 81.15(6) 3_666 1_556 ? O4 La1 O2 151.98(7) . 2_656 ? O4 La1 O2 120.22(7) 3_665 2_656 ? O4 La1 O2 84.47(6) 2_655 2_656 ? O2 La1 O2 81.15(6) 3_666 2_656 ? O2 La1 O2 81.15(6) 1_556 2_656 ? O4 La1 O1 72.55(7) . 3_666 ? O4 La1 O1 86.04(7) 3_665 3_666 ? O4 La1 O1 153.35(6) 2_655 3_666 ? O2 La1 O1 48.51(6) 3_666 3_666 ? O2 La1 O1 66.44(6) 1_556 3_666 ? O2 La1 O1 122.00(6) 2_656 3_666 ? O4 La1 O1 153.35(6) . 2_656 ? O4 La1 O1 72.55(7) 3_665 2_656 ? O4 La1 O1 86.04(7) 2_655 2_656 ? O2 La1 O1 66.44(6) 3_666 2_656 ? O2 La1 O1 122.00(6) 1_556 2_656 ? O2 La1 O1 48.51(6) 2_656 2_656 ? O1 La1 O1 113.06(3) 3_666 2_656 ? O4 La1 O1 86.04(7) . 1_556 ? O4 La1 O1 153.35(6) 3_665 1_556 ? O4 La1 O1 72.55(7) 2_655 1_556 ? O2 La1 O1 122.00(6) 3_666 1_556 ? O2 La1 O1 48.51(6) 1_556 1_556 ? O2 La1 O1 66.44(6) 2_656 1_556 ? O1 La1 O1 113.06(3) 3_666 1_556 ? O1 La1 O1 113.06(3) 2_656 1_556 ? O4 La1 C1 96.39(7) . 3_666 ? O4 La1 C1 84.61(7) 3_665 3_666 ? O4 La1 C1 166.79(7) 2_655 3_666 ? O2 La1 C1 24.24(6) 3_666 3_666 ? O2 La1 C1 72.51(6) 1_556 3_666 ? O2 La1 C1 101.98(6) 2_656 3_666 ? O1 La1 C1 24.28(6) 3_666 3_666 ? O1 La1 C1 89.67(6) 2_656 3_666 ? O1 La1 C1 120.55(6) 1_556 3_666 ? O4 La1 C1 84.61(7) . 1_556 ? O4 La1 C1 166.79(7) 3_665 1_556 ? O4 La1 C1 96.39(7) 2_655 1_556 ? O2 La1 C1 101.98(6) 3_666 1_556 ? O2 La1 C1 24.24(6) 1_556 1_556 ? O2 La1 C1 72.51(6) 2_656 1_556 ? O1 La1 C1 89.67(6) 3_666 1_556 ? O1 La1 C1 120.55(6) 2_656 1_556 ? O1 La1 C1 24.28(6) 1_556 1_556 ? C1 La1 C1 96.54(6) 3_666 1_556 ? O4 La1 C1 166.79(7) . 2_656 ? O4 La1 C1 96.39(7) 3_665 2_656 ? O4 La1 C1 84.61(7) 2_655 2_656 ? O2 La1 C1 72.51(6) 3_666 2_656 ? O2 La1 C1 101.98(6) 1_556 2_656 ? O2 La1 C1 24.24(6) 2_656 2_656 ? O1 La1 C1 120.55(6) 3_666 2_656 ? O1 La1 C1 24.28(6) 2_656 2_656 ? O1 La1 C1 89.67(6) 1_556 2_656 ? C1 La1 C1 96.54(6) 3_666 2_656 ? C1 La1 C1 96.54(6) 1_556 2_656 ? O3 Cu1 O3 180.00(11) 4_767 . ? O3 Cu1 N1 94.82(8) 4_767 . ? O3 Cu1 N1 85.18(8) . . ? O3 Cu1 N1 85.18(8) 4_767 4_767 ? O3 Cu1 N1 94.82(8) . 4_767 ? N1 Cu1 N1 180.0 . 4_767 ? O3 Cu1 O2 91.18(6) 4_767 . ? O3 Cu1 O2 88.82(6) . . ? N1 Cu1 O2 74.58(7) . . ? N1 Cu1 O2 105.42(7) 4_767 . ? O3 Cu1 O2 88.82(6) 4_767 4_767 ? O3 Cu1 O2 91.18(6) . 4_767 ? N1 Cu1 O2 105.42(7) . 4_767 ? N1 Cu1 O2 74.58(7) 4_767 4_767 ? O2 Cu1 O2 180.00(4) . 4_767 ? C1 O1 La1 89.52(15) . 1_554 ? C1 O2 Cu1 105.79(12) . . ? C1 O2 La1 99.86(13) . 1_554 ? Cu1 O2 La1 145.58(8) . 1_554 ? C4 O3 Cu1 114.72(16) . . ? C4 O4 La1 157.5(2) . . ? C3 N1 C2 114.3(2) . . ? C3 N1 Cu1 109.02(16) . . ? C2 N1 Cu1 109.22(15) . . ? O1 C1 O2 122.1(2) . . ? O1 C1 C2 119.2(2) . . ? O2 C1 C2 118.6(2) . . ? O1 C1 La1 66.20(12) . 1_554 ? O2 C1 La1 55.90(11) . 1_554 ? C2 C1 La1 173.74(18) . 1_554 ? C6 C2 N1 124.3(5) . . ? C6 C2 C1 119.3(6) . . ? N1 C2 C1 110.0(2) . . ? N1 C3 C5 110.4(3) . . ? N1 C3 C4 111.9(2) . . ? C5 C3 C4 119.9(3) . . ? O4 C4 O3 123.7(3) . . ? O4 C4 C3 117.4(3) . . ? O3 C4 C3 118.9(2) . . ? _diffrn_measured_fraction_theta_max 0.994 _diffrn_reflns_theta_full 26.98 _diffrn_measured_fraction_theta_full 0.994 _refine_diff_density_max 0.942 _refine_diff_density_min -0.569 _refine_diff_density_rms 0.101 # Attachment 'complex2.cif' data_complex2 _database_code_depnum_ccdc_archive 'CCDC 834765' #TrackingRef 'complex2.cif' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C30 H48 Cu3 N6 O27 Pr2' _chemical_formula_weight 1397.18 loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Cu Cu 0.3201 1.2651 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Pr Pr -0.2180 2.8214 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting Trigonal _symmetry_space_group_name_H-M P-3 loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-y, x-y, z' '-x+y, -x, z' '-x, -y, -z' 'y, -x+y, -z' 'x-y, x, -z' _cell_length_a 13.6614(19) _cell_length_b 13.6614(19) _cell_length_c 7.4147(15) _cell_angle_alpha 90.00 _cell_angle_beta 90.00 _cell_angle_gamma 120.00 _cell_volume 1198.4(3) _cell_formula_units_Z 1 _cell_measurement_temperature 173(2) _cell_measurement_reflns_used ? _cell_measurement_theta_min ? _cell_measurement_theta_max ? _exptl_crystal_description block _exptl_crystal_colour blue _exptl_crystal_size_max 0.30 _exptl_crystal_size_mid 0.20 _exptl_crystal_size_min 0.20 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.936 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 691 _exptl_absorpt_coefficient_mu 3.397 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.4289 _exptl_absorpt_correction_T_max 0.5498 _exptl_absorpt_process_details 'CrysAlis RED' _exptl_special_details ; CrysAlis RED, Oxford Diffraction Ltd., Version 1.171.32.5 (release 08-05-2007 CrysAlis171 .NET) (compiled May 8 2007,13:10:02) Empirical absorption correction using spherical harmonics, implemented in SCALE3 ABSPACK scaling algorithm. ; _diffrn_ambient_temperature 173(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'Enhance (Mo) X-ray Source' _diffrn_radiation_monochromator 'CrysAlis CCD, Oxford Diffraction Ltd.' _diffrn_measurement_device_type /w _diffrn_measurement_method ? _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 10998 _diffrn_reflns_av_R_equivalents 0.0322 _diffrn_reflns_av_sigmaI/netI 0.0218 _diffrn_reflns_limit_h_min -17 _diffrn_reflns_limit_h_max 17 _diffrn_reflns_limit_k_min -17 _diffrn_reflns_limit_k_max 17 _diffrn_reflns_limit_l_min -9 _diffrn_reflns_limit_l_max 9 _diffrn_reflns_theta_min 3.24 _diffrn_reflns_theta_max 26.97 _reflns_number_total 1748 _reflns_number_gt 1703 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'CrysAlis CCD' _computing_cell_refinement 'CrysAlis RED' _computing_data_reduction 'CrysAlis RED' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'SHELXS-97 (Sheldrick, 1990)' _computing_publication_material 'SHELXS-97 (Sheldrick, 1990)' _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^)+(0.0385P)^2^+1.0764P] 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 1748 _refine_ls_number_parameters 118 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0239 _refine_ls_R_factor_gt 0.0232 _refine_ls_wR_factor_ref 0.0637 _refine_ls_wR_factor_gt 0.0630 _refine_ls_goodness_of_fit_ref 1.078 _refine_ls_restrained_S_all 1.078 _refine_ls_shift/su_max 0.041 _refine_ls_shift/su_mean 0.003 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 Pr1 Pr 1.3333 0.6667 0.659947(18) 0.02389(4) Uani 1 3 d S . . Cu1 Cu 1.0000 0.5000 0.0000 0.03035(8) Uani 1 2 d S . . O1 O 1.24429(14) 0.80070(15) -0.2412(3) 0.0550(5) Uani 1 1 d . . . O2 O 1.18097(12) 0.63404(13) -0.1203(2) 0.0451(4) Uani 1 1 d . . . O3 O 1.07844(13) 0.48536(13) 0.2117(2) 0.0462(4) Uani 1 1 d . . . O4 O 1.18052(16) 0.57937(17) 0.4492(2) 0.0633(6) Uani 1 1 d . . . N1 N 1.03667(12) 0.64959(14) 0.1062(2) 0.0336(4) Uani 1 1 d . . . H1A H 0.9708 0.6456 0.1402 0.040 Uiso 1 1 calc R . . C1 C 1.17936(17) 0.72437(18) -0.1374(3) 0.0394(5) Uani 1 1 d . . . C2 C 1.0902(2) 0.73845(19) -0.0333(4) 0.0559(6) Uani 1 1 d . . . H2A H 1.1431 0.7983 0.0476 0.067 Uiso 1 1 calc R . . C3 C 1.1070(2) 0.6708(2) 0.2691(3) 0.0551(6) Uani 1 1 d . . . H3A H 1.1826 0.7303 0.2325 0.066 Uiso 1 1 calc R . . C4 C 1.12209(17) 0.57065(19) 0.3149(3) 0.0409(5) Uani 1 1 d . . . C5 C 1.0731(5) 0.7242(5) 0.4116(7) 0.0689(13) Uani 0.50 1 d P . . H5B H 1.0674 0.7858 0.3607 0.103 Uiso 0.50 1 calc PR . . H5C H 1.1288 0.7521 0.5058 0.103 Uiso 0.50 1 calc PR . . H5D H 1.0013 0.6693 0.4604 0.103 Uiso 0.50 1 calc PR . . C6 C 1.0470(7) 0.7886(9) -0.0912(17) 0.188(4) Uani 0.50 1 d P . . H6A H 0.9939 0.7870 -0.0047 0.282 Uiso 0.50 1 calc PR . . H6B H 1.0082 0.7540 -0.2014 0.282 Uiso 0.50 1 calc PR . . H6C H 1.1038 0.8656 -0.1143 0.282 Uiso 0.50 1 calc PR . . O1W O 0.918(3) 0.703(3) 0.524(4) 1.09(4) Uani 1 1 d . . . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 Pr1 0.02723(5) 0.02723(5) 0.01722(7) 0.000 0.000 0.01361(3) Cu1 0.02799(12) 0.03122(13) 0.02570(13) 0.00022(11) -0.00716(11) 0.01021(10) O1 0.0470(8) 0.0464(8) 0.0589(10) 0.0127(7) 0.0156(8) 0.0138(7) O2 0.0408(6) 0.0400(6) 0.0542(8) 0.0011(6) 0.0154(6) 0.0199(5) O3 0.0500(7) 0.0410(7) 0.0393(7) 0.0006(6) -0.0192(6) 0.0165(6) O4 0.0627(9) 0.0693(10) 0.0445(8) -0.0052(8) -0.0306(7) 0.0231(8) N1 0.0262(6) 0.0427(7) 0.0322(7) -0.0003(6) 0.0013(6) 0.0175(5) C1 0.0309(8) 0.0356(9) 0.0392(10) 0.0003(8) 0.0038(8) 0.0073(7) C2 0.0728(12) 0.0419(9) 0.0628(14) 0.0128(9) 0.0248(11) 0.0360(8) C3 0.0573(10) 0.0637(12) 0.0510(12) -0.0248(10) -0.0267(9) 0.0353(9) C4 0.0335(8) 0.0489(10) 0.0292(9) -0.0001(8) -0.0081(7) 0.0122(8) C5 0.099(3) 0.108(3) 0.035(2) -0.030(2) -0.027(2) 0.078(2) C6 0.178(4) 0.205(6) 0.264(9) 0.160(6) 0.163(6) 0.158(4) O1W 0.99(5) 0.91(5) 0.82(3) -0.34(4) -0.49(3) 0.06(6) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag Pr1 O4 2.3941(16) 3_775 ? Pr1 O4 2.3941(17) . ? Pr1 O4 2.3941(16) 2_755 ? Pr1 O2 2.5017(16) 1_556 ? Pr1 O2 2.5017(16) 3_776 ? Pr1 O2 2.5017(16) 2_756 ? Pr1 O1 2.756(2) 1_556 ? Pr1 O1 2.756(2) 2_756 ? Pr1 O1 2.756(2) 3_776 ? Pr1 C1 2.994(2) 1_556 ? Pr1 C1 2.994(2) 3_776 ? Pr1 C1 2.994(2) 2_756 ? Cu1 O3 1.9665(16) 4_765 ? Cu1 O3 1.9665(16) . ? Cu1 N1 2.0059(18) . ? Cu1 N1 2.0059(18) 4_765 ? Cu1 O2 2.3946(14) . ? Cu1 O2 2.3946(14) 4_765 ? O1 C1 1.242(3) . ? O1 Pr1 2.756(2) 1_554 ? O2 C1 1.252(3) . ? O2 Pr1 2.5017(16) 1_554 ? O3 C4 1.267(3) . ? O4 C4 1.244(3) . ? N1 C3 1.480(3) . ? N1 C2 1.480(3) . ? C1 C2 1.533(4) . ? C1 Pr1 2.994(2) 1_554 ? C2 C6 1.187(11) . ? C3 C5 1.483(6) . ? C3 C4 1.520(4) . ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag O4 Pr1 O4 82.02(7) 3_775 . ? O4 Pr1 O4 82.02(7) 3_775 2_755 ? O4 Pr1 O4 82.02(7) . 2_755 ? O4 Pr1 O2 119.69(7) 3_775 1_556 ? O4 Pr1 O2 84.01(6) . 1_556 ? O4 Pr1 O2 152.14(7) 2_755 1_556 ? O4 Pr1 O2 84.01(6) 3_775 3_776 ? O4 Pr1 O2 152.14(7) . 3_776 ? O4 Pr1 O2 119.69(7) 2_755 3_776 ? O2 Pr1 O2 82.17(6) 1_556 3_776 ? O4 Pr1 O2 152.14(7) 3_775 2_756 ? O4 Pr1 O2 119.69(7) . 2_756 ? O4 Pr1 O2 84.01(6) 2_755 2_756 ? O2 Pr1 O2 82.17(6) 1_556 2_756 ? O2 Pr1 O2 82.17(6) 3_776 2_756 ? O4 Pr1 O1 72.00(6) 3_775 1_556 ? O4 Pr1 O1 86.55(7) . 1_556 ? O4 Pr1 O1 152.83(6) 2_755 1_556 ? O2 Pr1 O1 48.77(5) 1_556 1_556 ? O2 Pr1 O1 66.19(5) 3_776 1_556 ? O2 Pr1 O1 122.91(6) 2_756 1_556 ? O4 Pr1 O1 152.83(7) 3_775 2_756 ? O4 Pr1 O1 72.00(6) . 2_756 ? O4 Pr1 O1 86.55(7) 2_755 2_756 ? O2 Pr1 O1 66.19(5) 1_556 2_756 ? O2 Pr1 O1 122.91(6) 3_776 2_756 ? O2 Pr1 O1 48.77(5) 2_756 2_756 ? O1 Pr1 O1 113.20(3) 1_556 2_756 ? O4 Pr1 O1 86.55(7) 3_775 3_776 ? O4 Pr1 O1 152.83(7) . 3_776 ? O4 Pr1 O1 72.00(6) 2_755 3_776 ? O2 Pr1 O1 122.91(6) 1_556 3_776 ? O2 Pr1 O1 48.77(5) 3_776 3_776 ? O2 Pr1 O1 66.19(5) 2_756 3_776 ? O1 Pr1 O1 113.20(3) 1_556 3_776 ? O1 Pr1 O1 113.20(3) 2_756 3_776 ? O4 Pr1 C1 95.95(7) 3_775 1_556 ? O4 Pr1 C1 84.62(7) . 1_556 ? O4 Pr1 C1 166.64(6) 2_755 1_556 ? O2 Pr1 C1 24.27(6) 1_556 1_556 ? O2 Pr1 C1 72.97(5) 3_776 1_556 ? O2 Pr1 C1 102.92(6) 2_756 1_556 ? O1 Pr1 C1 24.50(5) 1_556 1_556 ? O1 Pr1 C1 89.53(5) 2_756 1_556 ? O1 Pr1 C1 121.18(5) 3_776 1_556 ? O4 Pr1 C1 84.62(7) 3_775 3_776 ? O4 Pr1 C1 166.64(6) . 3_776 ? O4 Pr1 C1 95.95(7) 2_755 3_776 ? O2 Pr1 C1 102.92(6) 1_556 3_776 ? O2 Pr1 C1 24.27(6) 3_776 3_776 ? O2 Pr1 C1 72.97(5) 2_756 3_776 ? O1 Pr1 C1 89.53(5) 1_556 3_776 ? O1 Pr1 C1 121.18(5) 2_756 3_776 ? O1 Pr1 C1 24.50(5) 3_776 3_776 ? C1 Pr1 C1 97.01(6) 1_556 3_776 ? O4 Pr1 C1 166.64(6) 3_775 2_756 ? O4 Pr1 C1 95.95(7) . 2_756 ? O4 Pr1 C1 84.62(7) 2_755 2_756 ? O2 Pr1 C1 72.97(5) 1_556 2_756 ? O2 Pr1 C1 102.92(6) 3_776 2_756 ? O2 Pr1 C1 24.27(6) 2_756 2_756 ? O1 Pr1 C1 121.18(5) 1_556 2_756 ? O1 Pr1 C1 24.50(5) 2_756 2_756 ? O1 Pr1 C1 89.53(5) 3_776 2_756 ? C1 Pr1 C1 97.01(6) 1_556 2_756 ? C1 Pr1 C1 97.01(6) 3_776 2_756 ? O3 Cu1 O3 180.00(10) 4_765 . ? O3 Cu1 N1 94.64(7) 4_765 . ? O3 Cu1 N1 85.36(7) . . ? O3 Cu1 N1 85.36(7) 4_765 4_765 ? O3 Cu1 N1 94.64(7) . 4_765 ? N1 Cu1 N1 180.00(9) . 4_765 ? O3 Cu1 O2 91.81(6) 4_765 . ? O3 Cu1 O2 88.19(6) . . ? N1 Cu1 O2 74.37(6) . . ? N1 Cu1 O2 105.63(6) 4_765 . ? O3 Cu1 O2 88.19(6) 4_765 4_765 ? O3 Cu1 O2 91.81(6) . 4_765 ? N1 Cu1 O2 105.63(6) . 4_765 ? N1 Cu1 O2 74.37(6) 4_765 4_765 ? O2 Cu1 O2 180.0 . 4_765 ? C1 O1 Pr1 88.53(16) . 1_554 ? C1 O2 Cu1 105.74(13) . . ? C1 O2 Pr1 100.48(13) . 1_554 ? Cu1 O2 Pr1 145.87(7) . 1_554 ? C4 O3 Cu1 114.75(16) . . ? C4 O4 Pr1 158.12(17) . . ? C3 N1 C2 113.81(17) . . ? C3 N1 Cu1 109.08(16) . . ? C2 N1 Cu1 109.31(14) . . ? O1 C1 O2 122.2(2) . . ? O1 C1 C2 119.0(2) . . ? O2 C1 C2 118.66(18) . . ? O1 C1 Pr1 66.97(14) . 1_554 ? O2 C1 Pr1 55.25(11) . 1_554 ? C2 C1 Pr1 173.03(14) . 1_554 ? C6 C2 N1 122.8(5) . . ? C6 C2 C1 123.1(6) . . ? N1 C2 C1 110.3(2) . . ? N1 C3 C5 110.2(3) . . ? N1 C3 C4 111.91(19) . . ? C5 C3 C4 120.0(3) . . ? O4 C4 O3 123.8(3) . . ? O4 C4 C3 117.5(2) . . ? O3 C4 C3 118.66(19) . . ? _diffrn_measured_fraction_theta_max 0.995 _diffrn_reflns_theta_full 26.97 _diffrn_measured_fraction_theta_full 0.995 _refine_diff_density_max 0.862 _refine_diff_density_min -0.452 _refine_diff_density_rms 0.098 # checkcif RESULTS (APPEND TO CIF) _vrf_PLAT306_complex2 ; PROBLEM:Isolated Oxygen Atom (H-atoms Missing ?) ....... O1W RESPONSE: The reason is that the o1w atom of guest water molecule cannot be added two hydrogen atoms via difference electron density map peaks ; # end Validation Reply Form # Attachment 'complex3.cif' data_complex3 _database_code_depnum_ccdc_archive 'CCDC 834766' #TrackingRef 'complex3.cif' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C30 H48 Cu3 N6 Nd2 O27' _chemical_formula_weight 1403.84 loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Cu Cu 0.3201 1.2651 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Nd Nd -0.1943 3.0179 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting Trigonal _symmetry_space_group_name_H-M P-3 loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-y, x-y, z' '-x+y, -x, z' '-x, -y, -z' 'y, -x+y, -z' 'x-y, x, -z' _cell_length_a 13.6319(19) _cell_length_b 13.6319(19) _cell_length_c 7.3817(15) _cell_angle_alpha 90.00 _cell_angle_beta 90.00 _cell_angle_gamma 120.00 _cell_volume 1188.0(3) _cell_formula_units_Z 1 _cell_measurement_temperature 298(2) _cell_measurement_reflns_used ? _cell_measurement_theta_min ? _cell_measurement_theta_max ? _exptl_crystal_description block _exptl_crystal_colour blue _exptl_crystal_size_max 0.30 _exptl_crystal_size_mid 0.25 _exptl_crystal_size_min 0.25 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.962 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 693 _exptl_absorpt_coefficient_mu 3.562 _exptl_absorpt_correction_type analytical _exptl_absorpt_correction_T_min 0.4146 _exptl_absorpt_correction_T_max 0.4696 _exptl_absorpt_process_details Tompa_analytical _exptl_special_details ; ; _diffrn_ambient_temperature 298(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'Rigaku RAXIS-CS Imaging Plate' _diffrn_measurement_method \w _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 11231 _diffrn_reflns_av_R_equivalents 0.0391 _diffrn_reflns_av_sigmaI/netI 0.0249 _diffrn_reflns_limit_h_min -17 _diffrn_reflns_limit_h_max 17 _diffrn_reflns_limit_k_min -17 _diffrn_reflns_limit_k_max 17 _diffrn_reflns_limit_l_min -8 _diffrn_reflns_limit_l_max 9 _diffrn_reflns_theta_min 3.25 _diffrn_reflns_theta_max 26.98 _reflns_number_total 1737 _reflns_number_gt 1667 _reflns_threshold_expression >2sigma(I) _computing_data_collection R-AXIS-SPIDER _computing_cell_refinement R-AXIS-SPIDER _computing_data_reduction R-AXIS-SPIDER _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'SHELXL-97 (Sheldrick, 1997)' _computing_publication_material 'SHELXL-97 (Sheldrick, 1997)' _refine_special_details ; Refinement of F^2^ against ALL reflections. The weighted R-factor wR and goodness of fit S are based on F^2^, conventional R-factors R are based on F, with F set to zero for negative F^2^. The threshold expression of F^2^ > 2sigma(F^2^) is used only for calculating R-factors(gt) etc. and is not relevant to the choice of reflections for refinement. R-factors based on F^2^ are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger. ; _refine_ls_structure_factor_coef Fsqd _refine_ls_matrix_type full _refine_ls_weighting_scheme calc _refine_ls_weighting_details 'calc w=1/[\s^2^(Fo^2^)+(0.0382P)^2^+1.8774P] 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 1737 _refine_ls_number_parameters 118 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0296 _refine_ls_R_factor_gt 0.0284 _refine_ls_wR_factor_ref 0.0743 _refine_ls_wR_factor_gt 0.0733 _refine_ls_goodness_of_fit_ref 1.096 _refine_ls_restrained_S_all 1.096 _refine_ls_shift/su_max 0.045 _refine_ls_shift/su_mean 0.003 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 Nd1 Nd 0.6667 0.3333 0.66008(2) 0.02653(5) Uani 1 3 d S . . Cu1 Cu 0.5000 0.0000 1.0000 0.03364(10) Uani 1 2 d S . . O1 O 0.80034(19) 0.24473(19) 0.7572(3) 0.0611(7) Uani 1 1 d . . . O2 O 0.63414(15) 0.18181(15) 0.8789(3) 0.0484(5) Uani 1 1 d . . . O3 O 0.48572(16) 0.07865(17) 1.2127(3) 0.0489(5) Uani 1 1 d . . . O4 O 0.5804(2) 0.1811(2) 1.4504(3) 0.0674(7) Uani 1 1 d . . . N1 N 0.64974(17) 0.03706(16) 1.1060(3) 0.0370(5) Uani 1 1 d . . . H1A H 0.6457 -0.0291 1.1398 0.044 Uiso 1 1 calc R . . C1 C 0.7243(2) 0.1795(2) 0.8617(4) 0.0437(7) Uani 1 1 d . . . C2 C 0.7383(2) 0.0902(3) 0.9647(5) 0.0603(8) Uani 1 1 d . . . H2A H 0.7956 0.1448 1.0479 0.072 Uiso 1 1 calc R . . C3 C 0.6706(3) 0.1066(3) 1.2700(5) 0.0601(8) Uani 1 1 d . . . H3A H 0.7305 0.1822 1.2334 0.072 Uiso 1 1 calc R . . C4 C 0.5715(2) 0.1230(2) 1.3157(3) 0.0432(7) Uani 1 1 d . . . C5 C 0.7247(6) 0.0724(6) 1.4105(8) 0.0707(18) Uani 0.50 1 d P . . H5A H 0.7856 0.0661 1.3576 0.106 Uiso 0.50 1 calc PR . . H5C H 0.6697 0.0006 1.4603 0.106 Uiso 0.50 1 calc PR . . H5D H 0.7538 0.1283 1.5049 0.106 Uiso 0.50 1 calc PR . . C6 C 0.7946(9) 0.0531(9) 0.916(2) 0.205(5) Uani 0.50 1 d P . . H6A H 0.7903 -0.0015 1.0026 0.307 Uiso 0.50 1 calc PR . . H6B H 0.8717 0.1132 0.9054 0.307 Uiso 0.50 1 calc PR . . H6C H 0.7682 0.0172 0.8005 0.307 Uiso 0.50 1 calc PR . . O1W O 0.710(4) -0.094(3) 1.539(5) 0.99(4) Uani 0.50 1 d P . . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 Nd1 0.03111(6) 0.03111(6) 0.01737(9) 0.000 0.000 0.01555(3) Cu1 0.03551(17) 0.03152(17) 0.02733(18) -0.00768(14) 0.00056(15) 0.01184(13) O1 0.0524(10) 0.0530(11) 0.0655(13) 0.0167(10) 0.0135(10) 0.0171(9) O2 0.0444(8) 0.0437(8) 0.0561(11) 0.0159(8) -0.0005(8) 0.0212(7) O3 0.0455(8) 0.0538(9) 0.0402(9) -0.0201(8) 0.0002(8) 0.0196(7) O4 0.0740(13) 0.0671(12) 0.0465(11) -0.0313(10) -0.0058(10) 0.0243(10) N1 0.0454(9) 0.0307(8) 0.0350(10) 0.0003(7) -0.0015(8) 0.0191(7) C1 0.0411(12) 0.0338(11) 0.0432(14) 0.0049(10) 0.0012(11) 0.0089(9) C2 0.0471(11) 0.0753(15) 0.070(2) 0.0259(14) 0.0128(13) 0.0390(11) C3 0.0685(15) 0.0606(14) 0.0575(17) -0.0303(13) -0.0284(13) 0.0370(12) C4 0.0533(13) 0.0369(11) 0.0281(11) -0.0100(9) -0.0008(10) 0.0140(10) C5 0.108(4) 0.097(4) 0.039(3) -0.027(3) -0.028(3) 0.075(3) C6 0.205(6) 0.190(6) 0.310(13) 0.184(7) 0.175(8) 0.166(5) O1W 1.30(6) 0.45(3) 0.79(3) -0.33(3) -0.79(4) 0.12(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 Nd1 O4 2.376(2) 2_654 ? Nd1 O4 2.376(2) 1_554 ? Nd1 O4 2.376(2) 3_664 ? Nd1 O2 2.481(2) . ? Nd1 O2 2.481(2) 2_655 ? Nd1 O2 2.481(2) 3_665 ? Nd1 O1 2.738(3) . ? Nd1 O1 2.738(3) 3_665 ? Nd1 O1 2.738(3) 2_655 ? Nd1 C1 2.979(3) . ? Nd1 C1 2.979(3) 2_655 ? Nd1 C1 2.979(3) 3_665 ? Cu1 O3 1.965(2) 4_657 ? Cu1 O3 1.965(2) . ? Cu1 N1 2.001(2) . ? Cu1 N1 2.001(2) 4_657 ? Cu1 O2 2.3986(18) 4_657 ? Cu1 O2 2.3986(18) . ? O1 C1 1.240(3) . ? O2 C1 1.251(4) . ? O3 C4 1.267(3) . ? O4 C4 1.238(3) . ? O4 Nd1 2.376(2) 1_556 ? N1 C3 1.475(4) . ? N1 C2 1.482(4) . ? C1 C2 1.527(5) . ? C2 C6 1.166(13) . ? C3 C5 1.476(8) . ? C3 C4 1.515(5) . ? 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 O4 Nd1 O4 82.14(9) 2_654 1_554 ? O4 Nd1 O4 82.14(9) 2_654 3_664 ? O4 Nd1 O4 82.14(9) 1_554 3_664 ? O4 Nd1 O2 119.85(8) 2_654 . ? O4 Nd1 O2 83.85(8) 1_554 . ? O4 Nd1 O2 151.89(9) 3_664 . ? O4 Nd1 O2 83.85(8) 2_654 2_655 ? O4 Nd1 O2 151.89(9) 1_554 2_655 ? O4 Nd1 O2 119.85(8) 3_664 2_655 ? O2 Nd1 O2 82.20(8) . 2_655 ? O4 Nd1 O2 151.89(9) 2_654 3_665 ? O4 Nd1 O2 119.85(8) 1_554 3_665 ? O4 Nd1 O2 83.85(8) 3_664 3_665 ? O2 Nd1 O2 82.20(8) . 3_665 ? O2 Nd1 O2 82.20(8) 2_655 3_665 ? O4 Nd1 O1 71.90(8) 2_654 . ? O4 Nd1 O1 86.19(9) 1_554 . ? O4 Nd1 O1 152.76(8) 3_664 . ? O2 Nd1 O1 48.97(6) . . ? O2 Nd1 O1 66.28(7) 2_655 . ? O2 Nd1 O1 123.18(7) 3_665 . ? O4 Nd1 O1 152.76(8) 2_654 3_665 ? O4 Nd1 O1 71.90(8) 1_554 3_665 ? O4 Nd1 O1 86.19(9) 3_664 3_665 ? O2 Nd1 O1 66.28(7) . 3_665 ? O2 Nd1 O1 123.18(7) 2_655 3_665 ? O2 Nd1 O1 48.97(7) 3_665 3_665 ? O1 Nd1 O1 113.40(4) . 3_665 ? O4 Nd1 O1 86.19(9) 2_654 2_655 ? O4 Nd1 O1 152.76(8) 1_554 2_655 ? O4 Nd1 O1 71.90(8) 3_664 2_655 ? O2 Nd1 O1 123.18(7) . 2_655 ? O2 Nd1 O1 48.97(6) 2_655 2_655 ? O2 Nd1 O1 66.28(7) 3_665 2_655 ? O1 Nd1 O1 113.40(4) . 2_655 ? O1 Nd1 O1 113.40(4) 3_665 2_655 ? O4 Nd1 C1 95.96(8) 2_654 . ? O4 Nd1 C1 84.29(9) 1_554 . ? O4 Nd1 C1 166.43(8) 3_664 . ? O2 Nd1 C1 24.37(7) . . ? O2 Nd1 C1 73.06(7) 2_655 . ? O2 Nd1 C1 103.09(7) 3_665 . ? O1 Nd1 C1 24.60(7) . . ? O1 Nd1 C1 89.67(7) 3_665 . ? O1 Nd1 C1 121.50(7) 2_655 . ? O4 Nd1 C1 84.29(9) 2_654 2_655 ? O4 Nd1 C1 166.43(8) 1_554 2_655 ? O4 Nd1 C1 95.96(8) 3_664 2_655 ? O2 Nd1 C1 103.09(7) . 2_655 ? O2 Nd1 C1 24.37(7) 2_655 2_655 ? O2 Nd1 C1 73.06(7) 3_665 2_655 ? O1 Nd1 C1 89.67(7) . 2_655 ? O1 Nd1 C1 121.50(7) 3_665 2_655 ? O1 Nd1 C1 24.60(7) 2_655 2_655 ? C1 Nd1 C1 97.22(8) . 2_655 ? O4 Nd1 C1 166.43(8) 2_654 3_665 ? O4 Nd1 C1 95.96(8) 1_554 3_665 ? O4 Nd1 C1 84.29(9) 3_664 3_665 ? O2 Nd1 C1 73.06(7) . 3_665 ? O2 Nd1 C1 103.09(7) 2_655 3_665 ? O2 Nd1 C1 24.37(7) 3_665 3_665 ? O1 Nd1 C1 121.50(7) . 3_665 ? O1 Nd1 C1 24.60(7) 3_665 3_665 ? O1 Nd1 C1 89.67(7) 2_655 3_665 ? C1 Nd1 C1 97.22(8) . 3_665 ? C1 Nd1 C1 97.22(8) 2_655 3_665 ? O3 Cu1 O3 180.0 4_657 . ? O3 Cu1 N1 94.78(9) 4_657 . ? O3 Cu1 N1 85.22(9) . . ? O3 Cu1 N1 85.22(9) 4_657 4_657 ? O3 Cu1 N1 94.78(9) . 4_657 ? N1 Cu1 N1 180.0 . 4_657 ? O3 Cu1 O2 88.07(8) 4_657 4_657 ? O3 Cu1 O2 91.93(8) . 4_657 ? N1 Cu1 O2 105.64(8) . 4_657 ? N1 Cu1 O2 74.36(8) 4_657 4_657 ? O3 Cu1 O2 91.93(8) 4_657 . ? O3 Cu1 O2 88.07(8) . . ? N1 Cu1 O2 74.36(8) . . ? N1 Cu1 O2 105.64(8) 4_657 . ? O2 Cu1 O2 180.00(8) 4_657 . ? C1 O1 Nd1 88.7(2) . . ? C1 O2 Cu1 105.26(16) . . ? C1 O2 Nd1 100.69(16) . . ? Cu1 O2 Nd1 146.04(9) . . ? C4 O3 Cu1 114.9(2) . . ? C4 O4 Nd1 158.2(2) . 1_556 ? C3 N1 C2 114.5(2) . . ? C3 N1 Cu1 109.15(19) . . ? C2 N1 Cu1 109.11(18) . . ? O1 C1 O2 121.7(3) . . ? O1 C1 C2 119.2(3) . . ? O2 C1 C2 119.0(2) . . ? O1 C1 Nd1 66.75(18) . . ? O2 C1 Nd1 54.94(14) . . ? C2 C1 Nd1 172.99(18) . . ? C6 C2 N1 123.8(7) . . ? C6 C2 C1 124.4(7) . . ? N1 C2 C1 110.1(3) . . ? N1 C3 C5 109.9(4) . . ? N1 C3 C4 112.2(2) . . ? C5 C3 C4 120.9(4) . . ? O4 C4 O3 124.0(3) . . ? O4 C4 C3 117.6(3) . . ? O3 C4 C3 118.3(2) . . ? _diffrn_measured_fraction_theta_max 0.997 _diffrn_reflns_theta_full 26.98 _diffrn_measured_fraction_theta_full 0.997 _refine_diff_density_max 1.400 _refine_diff_density_min -0.682 _refine_diff_density_rms 0.105 # Attachment 'complex4.cif' data_complex4 _database_code_depnum_ccdc_archive 'CCDC 834767' #TrackingRef 'complex4.cif' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C20 H48 Cu La2 N4 O26' _chemical_formula_weight 1101.98 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' La La -0.2871 2.4523 '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 6.9904(4) _cell_length_b 9.6565(4) _cell_length_c 14.2151(6) _cell_angle_alpha 82.948(4) _cell_angle_beta 85.238(4) _cell_angle_gamma 76.655(4) _cell_volume 925.10(8) _cell_formula_units_Z 1 _cell_measurement_temperature 173(2) _cell_measurement_reflns_used ? _cell_measurement_theta_min ? _cell_measurement_theta_max ? _exptl_crystal_description block _exptl_crystal_colour blue _exptl_crystal_size_max 0.10 _exptl_crystal_size_mid 0.10 _exptl_crystal_size_min 0.05 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.978 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 547 _exptl_absorpt_coefficient_mu 2.936 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.7578 _exptl_absorpt_correction_T_max 0.8671 _exptl_absorpt_process_details 'CrysAlis RED' _exptl_special_details ; CrysAlis RED, Oxford Diffraction Ltd., Version 1.171.32.5 (release 08-05-2007 CrysAlis171 .NET) (compiled May 8 2007,13:10:02) Empirical absorption correction using spherical harmonics, implemented in SCALE3 ABSPACK scaling algorithm. ; _diffrn_ambient_temperature 173(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'Enhance (Mo) X-ray Source' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'CrysAlis CCD, Oxford Diffraction Ltd.' _diffrn_measurement_method \w _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 8687 _diffrn_reflns_av_R_equivalents 0.0284 _diffrn_reflns_av_sigmaI/netI 0.0430 _diffrn_reflns_limit_h_min -8 _diffrn_reflns_limit_h_max 8 _diffrn_reflns_limit_k_min -11 _diffrn_reflns_limit_k_max 11 _diffrn_reflns_limit_l_min -17 _diffrn_reflns_limit_l_max 17 _diffrn_reflns_theta_min 2.48 _diffrn_reflns_theta_max 26.00 _reflns_number_total 3633 _reflns_number_gt 3190 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'CrysAlis CCD' _computing_cell_refinement 'CrysAlis RED' _computing_data_reduction 'CrysAlis RED' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'SHELXL-97 (Sheldrick, 1997)' _computing_publication_material 'SHELXL-97 (Sheldrick, 1997)' _refine_special_details ; Refinement of F^2^ against ALL reflections. The weighted R-factor wR and goodness of fit S are based on F^2^, conventional R-factors R are based on F, with F set to zero for negative F^2^. The threshold expression of F^2^ > 2sigma(F^2^) is used only for calculating R-factors(gt) etc. and is not relevant to the choice of reflections for refinement. R-factors based on F^2^ are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger. ; _refine_ls_structure_factor_coef Fsqd _refine_ls_matrix_type full _refine_ls_weighting_scheme calc _refine_ls_weighting_details 'calc w=1/[\s^2^(Fo^2^)+(0.0308P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment constr _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 3633 _refine_ls_number_parameters 241 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0300 _refine_ls_R_factor_gt 0.0237 _refine_ls_wR_factor_ref 0.0599 _refine_ls_wR_factor_gt 0.0591 _refine_ls_goodness_of_fit_ref 1.046 _refine_ls_restrained_S_all 1.046 _refine_ls_shift/su_max 0.012 _refine_ls_shift/su_mean 0.001 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 La1 La 0.72315(3) 1.59550(2) 1.904314(15) 0.00809(7) Uani 1 1 d . . . Cu1 Cu 0.5000 1.5000 1.5000 0.01422(15) Uani 1 2 d S . . O1 O 0.5980(4) 2.0837(3) 1.8919(2) 0.0196(6) Uani 1 1 d . . . N1 N 0.4034(4) 1.8076(3) 1.8227(2) 0.0117(6) Uani 1 1 d . . . O1W O 0.9569(4) 1.3688(3) 1.85179(19) 0.0186(6) Uani 1 1 d . . . C1 C 0.5865(5) 1.9566(4) 1.8886(3) 0.0130(8) Uani 1 1 d . . . O2W O 0.8649(4) 1.6502(3) 1.73385(18) 0.0179(6) Uani 1 1 d . . . O2 O 0.7327(4) 1.8520(3) 1.89123(18) 0.0163(6) Uani 1 1 d . . . N2 N 0.3838(4) 1.3617(3) 1.5942(2) 0.0138(7) Uani 1 1 d . . . C2 C 0.3861(5) 1.9249(4) 1.8805(3) 0.0153(8) Uani 1 1 d . . . H2A H 0.3293 1.8991 1.9446 0.018 Uiso 1 1 calc R . . H2B H 0.2962 2.0115 1.8514 0.018 Uiso 1 1 calc R . . O3 O 0.3635(3) 1.6136(3) 1.97135(17) 0.0116(5) Uani 1 1 d . . . O3W O 0.6672(3) 1.6825(3) 2.07383(17) 0.0125(5) Uani 1 1 d . . . C3 C 0.4371(6) 1.8617(4) 1.7228(3) 0.0172(8) Uani 1 1 d . . . H3A H 0.3202 1.9329 1.7019 0.026 Uiso 1 1 calc R . . H3B H 0.4625 1.7821 1.6835 0.026 Uiso 1 1 calc R . . H3C H 0.5509 1.9060 1.7165 0.026 Uiso 1 1 calc R . . O4 O 0.0655(3) 1.6016(3) 1.94095(18) 0.0144(6) Uani 1 1 d . . . O4W O 0.9059(5) 0.1333(3) 0.7681(2) 0.0353(8) Uani 1 1 d . . . C4 C 0.2206(5) 1.7556(4) 1.8337(3) 0.0130(8) Uani 1 1 d . . . H4A H 0.2087 1.7083 1.7771 0.016 Uiso 1 1 calc R . . H4B H 0.1068 1.8380 1.8376 0.016 Uiso 1 1 calc R . . O5W O 0.9228(4) 0.9096(3) 0.63792(19) 0.0237(6) Uani 1 1 d . . . O5 O 0.5428(4) 1.4800(3) 1.80067(17) 0.0131(5) Uani 1 1 d . . . C5 C 0.2150(5) 1.6520(4) 1.9207(2) 0.0103(7) Uani 1 1 d . . . O6 O 0.6613(4) 1.4884(3) 1.65005(18) 0.0172(6) Uani 1 1 d . . . C6 C 0.5398(5) 1.4620(4) 1.7146(3) 0.0123(8) Uani 1 1 d . . . O7 O 0.6751(4) 1.3306(3) 1.45581(18) 0.0200(6) Uani 1 1 d . . . C7 C 0.3614(5) 1.4104(4) 1.6898(3) 0.0154(8) Uani 1 1 d . . . H7A H 0.3406 1.3305 1.7373 0.019 Uiso 1 1 calc R . . H7B H 0.2430 1.4893 1.6934 0.019 Uiso 1 1 calc R . . O8 O 0.7544(4) 1.0931(3) 1.48595(19) 0.0249(7) Uani 1 1 d . . . C8 C 0.1899(6) 1.3503(5) 1.5650(3) 0.0260(10) Uani 1 1 d . . . H8A H 0.1360 1.2833 1.6112 0.039 Uiso 1 1 calc R . . H8B H 0.2059 1.3154 1.5023 0.039 Uiso 1 1 calc R . . H8C H 0.0996 1.4447 1.5621 0.039 Uiso 1 1 calc R . . C9 C 0.5274(6) 1.2216(4) 1.5939(3) 0.0198(9) Uani 1 1 d . . . H9A H 0.4549 1.1439 1.5997 0.024 Uiso 1 1 calc R . . H9B H 0.6086 1.2068 1.6497 0.024 Uiso 1 1 calc R . . C10 C 0.6601(6) 1.2134(4) 1.5049(3) 0.0171(8) Uani 1 1 d . . . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 La1 0.00561(10) 0.00961(11) 0.00943(11) -0.00077(7) 0.00018(7) -0.00283(7) Cu1 0.0170(3) 0.0140(3) 0.0111(3) -0.0006(3) 0.0011(3) -0.0034(3) O1 0.0163(14) 0.0132(15) 0.0310(16) -0.0071(12) 0.0033(12) -0.0057(11) N1 0.0116(15) 0.0138(16) 0.0107(16) 0.0003(13) 0.0002(12) -0.0059(12) O1W 0.0145(13) 0.0177(15) 0.0228(15) -0.0058(12) -0.0015(11) 0.0002(11) C1 0.0171(19) 0.012(2) 0.0100(18) -0.0028(15) 0.0005(14) -0.0027(15) O2W 0.0176(14) 0.0231(15) 0.0135(14) 0.0007(11) 0.0004(11) -0.0076(11) O2 0.0127(13) 0.0142(14) 0.0222(15) -0.0023(11) -0.0024(11) -0.0027(11) N2 0.0157(16) 0.0149(17) 0.0110(16) -0.0020(13) -0.0016(12) -0.0031(13) C2 0.0124(18) 0.013(2) 0.020(2) -0.0021(16) -0.0014(15) -0.0009(15) O3 0.0078(12) 0.0134(14) 0.0131(13) 0.0001(10) -0.0014(10) -0.0016(10) O3W 0.0107(12) 0.0133(14) 0.0139(13) -0.0031(10) 0.0000(10) -0.0026(10) C3 0.019(2) 0.020(2) 0.0119(19) 0.0044(16) -0.0028(15) -0.0062(16) O4 0.0086(12) 0.0158(14) 0.0200(14) -0.0004(11) -0.0002(10) -0.0060(10) O4W 0.0394(19) 0.0301(19) 0.041(2) -0.0082(15) 0.0082(15) -0.0184(15) C4 0.0110(18) 0.015(2) 0.0128(19) 0.0003(15) -0.0021(14) -0.0032(15) O5W 0.0255(16) 0.0232(16) 0.0200(15) 0.0037(12) 0.0041(12) -0.0055(12) O5 0.0151(13) 0.0145(14) 0.0107(13) -0.0018(10) -0.0012(10) -0.0047(10) C5 0.0088(17) 0.0073(18) 0.0143(19) -0.0053(14) 0.0007(14) 0.0009(14) O6 0.0144(13) 0.0267(16) 0.0131(14) -0.0029(11) 0.0013(11) -0.0100(11) C6 0.0133(18) 0.0079(18) 0.015(2) -0.0015(15) -0.0019(14) -0.0001(14) O7 0.0238(15) 0.0167(15) 0.0168(15) -0.0004(12) 0.0033(11) -0.0011(12) C7 0.0159(19) 0.020(2) 0.0117(19) -0.0024(16) -0.0005(15) -0.0067(16) O8 0.0309(17) 0.0163(15) 0.0219(16) -0.0001(12) 0.0021(13) 0.0036(12) C8 0.023(2) 0.040(3) 0.020(2) -0.0029(19) -0.0063(17) -0.0146(19) C9 0.027(2) 0.015(2) 0.016(2) -0.0010(16) 0.0026(17) -0.0037(17) C10 0.017(2) 0.019(2) 0.014(2) -0.0023(16) -0.0009(15) -0.0021(16) _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 La1 O2 2.477(2) . ? La1 O4 2.507(2) 1_655 ? La1 O5 2.523(2) . ? La1 O1W 2.562(2) . ? La1 O2W 2.581(2) . ? La1 O3 2.588(2) . ? La1 O3W 2.618(2) . ? La1 O3 2.660(2) 2_689 ? La1 N1 2.876(3) . ? La1 O4 2.976(3) 2_689 ? Cu1 O7 1.941(2) 2_688 ? Cu1 O7 1.941(2) . ? Cu1 N2 2.029(3) . ? Cu1 N2 2.029(3) 2_688 ? O1 C1 1.255(4) . ? N1 C2 1.457(5) . ? N1 C4 1.468(4) . ? N1 C3 1.471(4) . ? C1 O2 1.260(4) . ? C1 C2 1.517(5) . ? N2 C7 1.476(5) . ? N2 C8 1.481(5) . ? N2 C9 1.487(5) . ? O3 C5 1.271(4) . ? O3 La1 2.660(2) 2_689 ? O4 C5 1.250(4) . ? O4 La1 2.507(2) 1_455 ? O4 La1 2.976(3) 2_689 ? C4 C5 1.496(5) . ? O5 C6 1.259(4) . ? O6 C6 1.242(4) . ? C6 C7 1.527(5) . ? O7 C10 1.276(5) . ? O8 C10 1.245(4) . ? C9 C10 1.505(5) . ? 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 O2 La1 O4 74.10(8) . 1_655 ? O2 La1 O5 126.56(8) . . ? O4 La1 O5 140.97(8) 1_655 . ? O2 La1 O1W 134.89(8) . . ? O4 La1 O1W 72.01(8) 1_655 . ? O5 La1 O1W 71.28(8) . . ? O2 La1 O2W 75.31(8) . . ? O4 La1 O2W 80.90(8) 1_655 . ? O5 La1 O2W 74.94(8) . . ? O1W La1 O2W 70.71(8) . . ? O2 La1 O3 99.14(8) . . ? O4 La1 O3 145.55(8) 1_655 . ? O5 La1 O3 70.19(8) . . ? O1W La1 O3 125.51(8) . . ? O2W La1 O3 130.98(8) . . ? O2 La1 O3W 70.84(8) . . ? O4 La1 O3W 78.04(8) 1_655 . ? O5 La1 O3W 136.92(8) . . ? O1W La1 O3W 128.06(8) . . ? O2W La1 O3W 143.85(8) . . ? O3 La1 O3W 68.00(7) . . ? O2 La1 O3 141.32(8) . 2_689 ? O4 La1 O3 103.56(8) 1_655 2_689 ? O5 La1 O3 79.98(8) . 2_689 ? O1W La1 O3 76.07(8) . 2_689 ? O2W La1 O3 143.26(8) . 2_689 ? O3 La1 O3 60.53(9) . 2_689 ? O3W La1 O3 70.96(7) . 2_689 ? O2 La1 N1 60.36(8) . . ? O4 La1 N1 133.22(8) 1_655 . ? O5 La1 N1 70.65(8) . . ? O1W La1 N1 135.57(8) . . ? O2W La1 N1 78.00(8) . . ? O3 La1 N1 58.66(8) . . ? O3W La1 N1 95.66(8) . . ? O3 La1 N1 118.19(8) 2_689 . ? O2 La1 O4 118.42(8) . 2_689 ? O4 La1 O4 58.18(9) 1_655 2_689 ? O5 La1 O4 115.00(7) . 2_689 ? O1W La1 O4 64.66(8) . 2_689 ? O2W La1 O4 126.18(8) . 2_689 ? O3 La1 O4 99.74(7) . 2_689 ? O3W La1 O4 63.55(7) . 2_689 ? O3 La1 O4 45.38(7) 2_689 2_689 ? N1 La1 O4 155.66(7) . 2_689 ? O7 Cu1 O7 180.000(2) 2_688 . ? O7 Cu1 N2 94.23(11) 2_688 . ? O7 Cu1 N2 85.77(11) . . ? O7 Cu1 N2 85.77(11) 2_688 2_688 ? O7 Cu1 N2 94.23(11) . 2_688 ? N2 Cu1 N2 180.000(1) . 2_688 ? C2 N1 C4 109.8(3) . . ? C2 N1 C3 108.3(3) . . ? C4 N1 C3 109.3(3) . . ? C2 N1 La1 102.4(2) . . ? C4 N1 La1 110.9(2) . . ? C3 N1 La1 115.8(2) . . ? O1 C1 O2 123.8(4) . . ? O1 C1 C2 119.0(3) . . ? O2 C1 C2 117.2(3) . . ? C1 O2 La1 126.4(2) . . ? C7 N2 C8 109.7(3) . . ? C7 N2 C9 110.1(3) . . ? C8 N2 C9 110.7(3) . . ? C7 N2 Cu1 110.0(2) . . ? C8 N2 Cu1 110.6(2) . . ? C9 N2 Cu1 105.8(2) . . ? N1 C2 C1 110.4(3) . . ? C5 O3 La1 123.8(2) . . ? C5 O3 La1 104.0(2) . 2_689 ? La1 O3 La1 119.47(9) . 2_689 ? C5 O4 La1 148.8(2) . 1_455 ? C5 O4 La1 89.3(2) . 2_689 ? La1 O4 La1 121.82(9) 1_455 2_689 ? N1 C4 C5 111.9(3) . . ? C6 O5 La1 139.3(2) . . ? O4 C5 O3 121.0(3) . . ? O4 C5 C4 119.2(3) . . ? O3 C5 C4 119.8(3) . . ? O6 C6 O5 126.1(3) . . ? O6 C6 C7 119.0(3) . . ? O5 C6 C7 114.8(3) . . ? C10 O7 Cu1 114.5(2) . . ? N2 C7 C6 112.9(3) . . ? N2 C9 C10 112.0(3) . . ? O8 C10 O7 124.2(3) . . ? O8 C10 C9 117.9(3) . . ? O7 C10 C9 117.8(3) . . ? _diffrn_measured_fraction_theta_max 0.999 _diffrn_reflns_theta_full 26.00 _diffrn_measured_fraction_theta_full 0.999 _refine_diff_density_max 0.813 _refine_diff_density_min -0.503 _refine_diff_density_rms 0.111 # checkcif RESULTS (APPEND TO CIF) _vrf_PLAT306_complex4 ; PROBLEM:Isolated Oxygen Atom (H-atoms Missing ?) ....... O4W Isolated Oxygen Atom (H-atoms Missing ?) ....... O5W RESPONSE: The reason is that the oxygen atom of guest water molecule cannot be added two hydrogen atoms via difference electron density map peaks ; # end Validation Reply Form # Attachment 'complex5.cif' data_complex5 _database_code_depnum_ccdc_archive 'CCDC 834768' #TrackingRef 'complex5.cif' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C20 H48 Cu N4 O26 Pr2' _chemical_formula_weight 1105.98 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' Pr Pr -0.2180 2.8214 '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 6.9645(14) _cell_length_b 9.7081(19) _cell_length_c 14.259(3) _cell_angle_alpha 82.88(3) _cell_angle_beta 85.24(3) _cell_angle_gamma 76.75(3) _cell_volume 929.7(3) _cell_formula_units_Z 1 _cell_measurement_temperature 298(2) _cell_measurement_reflns_used ? _cell_measurement_theta_min ? _cell_measurement_theta_max ? _exptl_crystal_description block _exptl_crystal_colour blue _exptl_crystal_size_max 0.10 _exptl_crystal_size_mid 0.05 _exptl_crystal_size_min 0.05 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.975 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 551 _exptl_absorpt_coefficient_mu 3.244 _exptl_absorpt_correction_type analytical _exptl_absorpt_correction_T_min 0.7374 _exptl_absorpt_correction_T_max 0.8546 _exptl_absorpt_process_details Tompa_analytical _exptl_special_details ; ? ; _diffrn_ambient_temperature 298(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'Rigaku RAXIS-CS Imaging Plate' _diffrn_measurement_method \w _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 8093 _diffrn_reflns_av_R_equivalents 0.0340 _diffrn_reflns_av_sigmaI/netI 0.0456 _diffrn_reflns_limit_h_min -8 _diffrn_reflns_limit_h_max 8 _diffrn_reflns_limit_k_min -11 _diffrn_reflns_limit_k_max 11 _diffrn_reflns_limit_l_min -16 _diffrn_reflns_limit_l_max 17 _diffrn_reflns_theta_min 3.01 _diffrn_reflns_theta_max 26.00 _reflns_number_total 3640 _reflns_number_gt 3211 _reflns_threshold_expression >2sigma(I) _computing_data_collection R-AXIS-SPIDER _computing_cell_refinement R-AXIS-SPIDER _computing_data_reduction R-AXIS-SPIDER _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'SHELXL-97 (Sheldrick, 1997)' _computing_publication_material 'SHELXL-97 (Sheldrick, 1997)' _refine_special_details ; Refinement of F^2^ against ALL reflections. The weighted R-factor wR and goodness of fit S are based on F^2^, conventional R-factors R are based on F, with F set to zero for negative F^2^. The threshold expression of F^2^ > 2sigma(F^2^) is used only for calculating R-factors(gt) etc. and is not relevant to the choice of reflections for refinement. R-factors based on F^2^ are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger. ; _refine_ls_structure_factor_coef Fsqd _refine_ls_matrix_type full _refine_ls_weighting_scheme calc _refine_ls_weighting_details 'calc w=1/[\s^2^(Fo^2^)+(0.0460P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment constr _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 3640 _refine_ls_number_parameters 241 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0366 _refine_ls_R_factor_gt 0.0297 _refine_ls_wR_factor_ref 0.0807 _refine_ls_wR_factor_gt 0.0768 _refine_ls_goodness_of_fit_ref 1.088 _refine_ls_restrained_S_all 1.088 _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 Pr1 Pr 0.28469(4) 0.90118(2) 0.596311(16) 0.01559(9) Uani 1 1 d . . . Cu1 Cu 0.5000 1.0000 1.0000 0.0259(2) Uani 1 2 d S . . O3W O 0.3345(5) 0.8175(3) 0.4289(2) 0.0226(7) Uani 1 1 d . . . O5 O 0.3575(5) 1.1079(3) 0.4692(2) 0.0208(7) Uani 1 1 d . . . N2 N 0.3995(6) 1.3065(4) 0.3228(3) 0.0194(8) Uani 1 1 d . . . O4 O 0.4575(5) 1.0194(3) 0.6991(2) 0.0244(7) Uani 1 1 d . . . O6 O 0.0547(5) 1.1041(3) 0.4394(2) 0.0247(7) Uani 1 1 d . . . O2 O 0.3243(6) 1.1688(4) 1.0429(2) 0.0362(9) Uani 1 1 d . . . O2W O 0.1408(6) 0.8487(4) 0.7632(2) 0.0296(8) Uani 1 1 d . . . O3 O 0.3375(6) 1.0113(4) 0.8489(2) 0.0323(8) Uani 1 1 d . . . O7 O 0.7288(5) 1.3501(3) 0.3911(3) 0.0275(8) Uani 1 1 d . . . C6 C 0.2080(6) 1.1508(4) 0.4198(3) 0.0170(9) Uani 1 1 d . . . O1W O 0.0503(5) 1.1252(3) 0.6453(3) 0.0304(8) Uani 1 1 d . . . O8 O 0.5952(6) 1.5811(3) 0.3922(3) 0.0343(9) Uani 1 1 d . . . N1 N 0.6175(6) 1.1379(4) 0.9051(3) 0.0246(9) Uani 1 1 d . . . C10 C 0.5835(7) 1.4542(5) 0.3885(3) 0.0223(10) Uani 1 1 d . . . C9 C 0.3826(7) 1.4232(5) 0.3826(4) 0.0250(10) Uani 1 1 d . . . H9A H 0.3297 1.3962 0.4455 0.030 Uiso 1 1 calc R . . H9B H 0.2928 1.5079 0.3555 0.030 Uiso 1 1 calc R . . C5 C 0.4592(7) 1.0372(5) 0.7849(3) 0.0228(10) Uani 1 1 d . . . C7 C 0.2166(7) 1.2546(5) 0.3337(3) 0.0219(10) Uani 1 1 d . . . H7A H 0.2050 1.2094 0.2781 0.026 Uiso 1 1 calc R . . H7B H 0.1050 1.3350 0.3374 0.026 Uiso 1 1 calc R . . C1 C 0.3385(9) 1.2855(6) 0.9943(4) 0.0331(12) Uani 1 1 d . . . O1 O 0.2447(7) 1.4041(4) 1.0128(3) 0.0494(11) Uani 1 1 d . . . C8 C 0.4349(8) 1.3608(6) 0.2230(3) 0.0302(12) Uani 1 1 d . . . H8A H 0.4461 1.2857 0.1837 0.045 Uiso 1 1 calc R . . H8B H 0.5551 1.3946 0.2162 0.045 Uiso 1 1 calc R . . H8C H 0.3266 1.4375 0.2043 0.045 Uiso 1 1 calc R . . C4 C 0.6367(8) 1.0912(5) 0.8095(3) 0.0261(11) Uani 1 1 d . . . H4A H 0.7545 1.0158 0.8046 0.031 Uiso 1 1 calc R . . H4B H 0.6539 1.1703 0.7633 0.031 Uiso 1 1 calc R . . C2 C 0.4746(9) 1.2771(5) 0.9062(4) 0.0346(13) Uani 1 1 d . . . H2A H 0.3960 1.2930 0.8512 0.042 Uiso 1 1 calc R . . H2B H 0.5468 1.3522 0.9017 0.042 Uiso 1 1 calc R . . C3 C 0.8128(9) 1.1480(7) 0.9336(4) 0.0432(15) Uani 1 1 d . . . H3A H 0.8660 1.2133 0.8883 0.065 Uiso 1 1 calc R . . H3B H 0.9006 1.0558 0.9360 0.065 Uiso 1 1 calc R . . H3C H 0.7985 1.1816 0.9949 0.065 Uiso 1 1 calc R . . O5W O -0.0786(7) 1.4074(5) 1.1378(3) 0.0505(12) Uani 1 1 d . . . O4W O 0.9077(8) 1.6355(5) 0.2718(3) 0.0562(13) Uani 1 1 d . . . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 Pr1 0.01283(14) 0.01709(13) 0.01704(13) -0.00301(9) 0.00158(9) -0.00393(9) Cu1 0.0322(5) 0.0253(4) 0.0189(4) -0.0018(3) 0.0023(3) -0.0054(4) O3W 0.0216(18) 0.0231(16) 0.0232(16) -0.0067(13) 0.0026(14) -0.0045(13) O5 0.0148(17) 0.0231(16) 0.0219(15) 0.0005(13) 0.0003(13) -0.0011(12) N2 0.018(2) 0.0224(19) 0.0181(18) -0.0011(15) 0.0001(15) -0.0058(15) O4 0.0260(19) 0.0296(17) 0.0185(16) -0.0033(14) -0.0010(14) -0.0077(14) O6 0.0170(18) 0.0253(16) 0.0315(18) -0.0001(14) 0.0001(14) -0.0060(13) O2 0.044(3) 0.031(2) 0.0268(18) 0.0034(16) 0.0073(17) -0.0020(17) O2W 0.034(2) 0.0352(19) 0.0214(16) -0.0036(15) 0.0036(15) -0.0136(16) O3 0.032(2) 0.044(2) 0.0244(17) -0.0062(16) 0.0061(16) -0.0174(17) O7 0.0243(19) 0.0188(16) 0.0391(19) -0.0032(15) -0.0012(15) -0.0047(13) C6 0.013(2) 0.019(2) 0.019(2) -0.0066(18) 0.0022(18) -0.0037(17) O1W 0.028(2) 0.0267(17) 0.0355(19) -0.0102(15) -0.0047(16) 0.0011(14) O8 0.030(2) 0.0181(16) 0.056(2) -0.0123(16) 0.0048(18) -0.0062(14) N1 0.029(2) 0.028(2) 0.0174(18) -0.0014(16) 0.0000(17) -0.0085(17) C10 0.024(3) 0.020(2) 0.023(2) -0.0039(19) 0.0046(19) -0.0063(19) C9 0.019(3) 0.022(2) 0.032(3) -0.005(2) 0.000(2) -0.0015(18) C5 0.022(3) 0.021(2) 0.023(2) -0.0016(19) -0.003(2) -0.0017(18) C7 0.016(2) 0.019(2) 0.029(2) 0.0050(19) -0.0026(19) -0.0036(17) C1 0.036(3) 0.037(3) 0.025(2) -0.007(2) -0.003(2) -0.004(2) O1 0.061(3) 0.033(2) 0.042(2) 0.0000(19) 0.008(2) 0.0088(19) C8 0.032(3) 0.034(3) 0.024(2) 0.005(2) 0.000(2) -0.011(2) C4 0.027(3) 0.037(3) 0.018(2) -0.006(2) 0.004(2) -0.014(2) C2 0.047(4) 0.027(3) 0.027(3) 0.002(2) 0.003(2) -0.004(2) C3 0.038(4) 0.065(4) 0.035(3) -0.009(3) -0.013(3) -0.023(3) O5W 0.044(3) 0.050(2) 0.045(2) 0.013(2) 0.011(2) -0.001(2) O4W 0.065(3) 0.050(3) 0.063(3) -0.017(2) 0.011(3) -0.030(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 Pr1 O7 2.446(3) 2_676 ? Pr1 O6 2.472(3) 2_576 ? Pr1 O4 2.501(3) . ? Pr1 O1W 2.538(4) . ? Pr1 O2W 2.542(3) . ? Pr1 O5 2.574(3) 2_676 ? Pr1 O3W 2.587(3) . ? Pr1 O5 2.643(3) . ? Pr1 N2 2.836(4) 2_676 ? Cu1 O2 1.940(4) . ? Cu1 O2 1.940(4) 2_677 ? Cu1 N1 2.041(4) 2_677 ? Cu1 N1 2.041(4) . ? O5 C6 1.266(5) . ? O5 Pr1 2.574(3) 2_676 ? N2 C7 1.463(5) . ? N2 C8 1.476(6) . ? N2 C9 1.478(6) . ? N2 Pr1 2.836(4) 2_676 ? O4 C5 1.257(6) . ? O6 C6 1.250(5) . ? O6 Pr1 2.472(3) 2_576 ? O2 C1 1.273(6) . ? O3 C5 1.235(6) . ? O7 C10 1.255(6) . ? O7 Pr1 2.446(3) 2_676 ? C6 C7 1.496(6) . ? O8 C10 1.261(5) . ? N1 C4 1.476(6) . ? N1 C3 1.479(7) . ? N1 C2 1.484(7) . ? C10 C9 1.508(6) . ? C5 C4 1.530(6) . ? C1 O1 1.234(7) . ? C1 C2 1.508(7) . ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag O7 Pr1 O6 73.67(11) 2_676 2_576 ? O7 Pr1 O4 127.89(11) 2_676 . ? O6 Pr1 O4 139.55(12) 2_576 . ? O7 Pr1 O1W 134.52(12) 2_676 . ? O6 Pr1 O1W 71.20(11) 2_576 . ? O4 Pr1 O1W 70.77(12) . . ? O7 Pr1 O2W 75.37(12) 2_676 . ? O6 Pr1 O2W 80.24(11) 2_576 . ? O4 Pr1 O2W 74.91(11) . . ? O1W Pr1 O2W 71.03(12) . . ? O7 Pr1 O5 101.48(11) 2_676 2_676 ? O6 Pr1 O5 146.47(11) 2_576 2_676 ? O4 Pr1 O5 69.82(11) . 2_676 ? O1W Pr1 O5 123.71(11) . 2_676 ? O2W Pr1 O5 131.58(11) . 2_676 ? O7 Pr1 O3W 70.89(11) 2_676 . ? O6 Pr1 O3W 77.43(11) 2_576 . ? O4 Pr1 O3W 138.29(10) . . ? O1W Pr1 O3W 126.37(11) . . ? O2W Pr1 O3W 143.54(10) . . ? O5 Pr1 O3W 69.84(10) 2_676 . ? O7 Pr1 O5 140.39(11) 2_676 . ? O6 Pr1 O5 101.07(10) 2_576 . ? O4 Pr1 O5 81.91(10) . . ? O1W Pr1 O5 75.02(11) . . ? O2W Pr1 O5 143.59(11) . . ? O5 Pr1 O5 61.08(12) 2_676 . ? O3W Pr1 O5 69.69(10) . . ? O7 Pr1 N2 61.02(11) 2_676 2_676 ? O6 Pr1 N2 133.38(10) 2_576 2_676 ? O4 Pr1 N2 71.71(11) . 2_676 ? O1W Pr1 N2 136.38(11) . 2_676 ? O2W Pr1 N2 78.45(12) . 2_676 ? O5 Pr1 N2 59.76(10) 2_676 2_676 ? O3W Pr1 N2 96.60(11) . 2_676 ? O5 Pr1 N2 120.34(10) . 2_676 ? O2 Cu1 O2 180.00(19) . 2_677 ? O2 Cu1 N1 94.37(16) . 2_677 ? O2 Cu1 N1 85.63(16) 2_677 2_677 ? O2 Cu1 N1 85.63(16) . . ? O2 Cu1 N1 94.37(16) 2_677 . ? N1 Cu1 N1 180.000(1) 2_677 . ? C6 O5 Pr1 124.0(3) . 2_676 ? C6 O5 Pr1 107.6(2) . . ? Pr1 O5 Pr1 118.92(12) 2_676 . ? C7 N2 C8 109.7(4) . . ? C7 N2 C9 109.7(4) . . ? C8 N2 C9 108.9(4) . . ? C7 N2 Pr1 110.9(2) . 2_676 ? C8 N2 Pr1 115.7(3) . 2_676 ? C9 N2 Pr1 101.6(3) . 2_676 ? C5 O4 Pr1 139.3(3) . . ? C6 O6 Pr1 150.1(3) . 2_576 ? C1 O2 Cu1 115.2(3) . . ? C10 O7 Pr1 126.2(3) . 2_676 ? O6 C6 O5 121.4(4) . . ? O6 C6 C7 118.8(4) . . ? O5 C6 C7 119.7(4) . . ? C4 N1 C3 109.9(4) . . ? C4 N1 C2 109.7(4) . . ? C3 N1 C2 110.8(4) . . ? C4 N1 Cu1 110.3(3) . . ? C3 N1 Cu1 110.5(3) . . ? C2 N1 Cu1 105.5(3) . . ? O7 C10 O8 124.2(5) . . ? O7 C10 C9 117.2(4) . . ? O8 C10 C9 118.6(4) . . ? N2 C9 C10 109.5(4) . . ? O3 C5 O4 126.5(4) . . ? O3 C5 C4 118.9(4) . . ? O4 C5 C4 114.5(4) . . ? N2 C7 C6 112.8(4) . . ? O1 C1 O2 124.5(5) . . ? O1 C1 C2 118.1(5) . . ? O2 C1 C2 117.3(5) . . ? N1 C4 C5 113.7(4) . . ? N1 C2 C1 112.8(4) . . ? _diffrn_measured_fraction_theta_max 0.997 _diffrn_reflns_theta_full 26.00 _diffrn_measured_fraction_theta_full 0.997 _refine_diff_density_max 1.386 _refine_diff_density_min -0.692 _refine_diff_density_rms 0.138 # checkcif RESULTS (APPEND TO CIF) _vrf_PLAT306_complex5 ; PROBLEM:Isolated Oxygen Atom (H-atoms Missing ?) ....... O4W Isolated Oxygen Atom (H-atoms Missing ?) ....... O5W RESPONSE: The reason is that the oxygen atom of guest water molecule cannot be added two hydrogen atoms via difference electron density map peaks ; # end Validation Reply Form # Attachment 'complex6.cif' data_complex6 _database_code_depnum_ccdc_archive 'CCDC 834769' #TrackingRef 'complex6.cif' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C20 H48 Cu N4 Nd2 O26' _chemical_formula_weight 1112.64 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' Nd Nd -0.1943 3.0179 '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 6.9007(2) _cell_length_b 9.6327(4) _cell_length_c 14.1655(4) _cell_angle_alpha 82.820(3) _cell_angle_beta 84.971(2) _cell_angle_gamma 76.703(3) _cell_volume 907.49(5) _cell_formula_units_Z 1 _cell_measurement_temperature 173(2) _cell_measurement_reflns_used ? _cell_measurement_theta_min ? _cell_measurement_theta_max ? _exptl_crystal_description block _exptl_crystal_colour blue _exptl_crystal_size_max 0.20 _exptl_crystal_size_mid 0.10 _exptl_crystal_size_min 0.10 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 2.036 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 553 _exptl_absorpt_coefficient_mu 3.500 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.5412 _exptl_absorpt_correction_T_max 0.7210 _exptl_absorpt_process_details 'CrysAlis RED' _exptl_special_details ; CrysAlis RED, Oxford Diffraction Ltd., Version 1.171.32.5 (release 08-05-2007 CrysAlis171 .NET) (compiled May 8 2007,13:10:02) Empirical absorption correction using spherical harmonics, implemented in SCALE3 ABSPACK scaling algorithm. ; _diffrn_ambient_temperature 173(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'Enhance (Mo) X-ray Source' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'CrysAlis CCD, Oxford Diffraction Ltd.' _diffrn_measurement_method \w _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 7634 _diffrn_reflns_av_R_equivalents 0.0213 _diffrn_reflns_av_sigmaI/netI 0.0361 _diffrn_reflns_limit_h_min -8 _diffrn_reflns_limit_h_max 8 _diffrn_reflns_limit_k_min -11 _diffrn_reflns_limit_k_max 11 _diffrn_reflns_limit_l_min -17 _diffrn_reflns_limit_l_max 17 _diffrn_reflns_theta_min 2.19 _diffrn_reflns_theta_max 26.00 _reflns_number_total 3570 _reflns_number_gt 3195 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'CrysAlis CCD' _computing_cell_refinement 'CrysAlis RED' _computing_data_reduction 'CrysAlis RED' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'SHELXL-97 (Sheldrick, 1997)' _computing_publication_material 'SHELXL-97 (Sheldrick, 1997)' _refine_special_details ; Refinement of F^2^ against ALL reflections. The weighted R-factor wR and goodness of fit S are based on F^2^, conventional R-factors R are based on F, with F set to zero for negative F^2^. The threshold expression of F^2^ > 2sigma(F^2^) is used only for calculating R-factors(gt) etc. and is not relevant to the choice of reflections for refinement. R-factors based on F^2^ are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger. ; _refine_ls_structure_factor_coef Fsqd _refine_ls_matrix_type full _refine_ls_weighting_scheme calc _refine_ls_weighting_details 'calc w=1/[\s^2^(Fo^2^)+(0.0323P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment constr _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 3570 _refine_ls_number_parameters 241 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0262 _refine_ls_R_factor_gt 0.0218 _refine_ls_wR_factor_ref 0.0562 _refine_ls_wR_factor_gt 0.0556 _refine_ls_goodness_of_fit_ref 1.025 _refine_ls_restrained_S_all 1.025 _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 Nd1 Nd 0.28519(3) 0.40096(2) 0.096305(12) 0.00763(6) Uani 1 1 d . . . Cu1 Cu 0.5000 0.5000 0.5000 0.01345(14) Uani 1 2 d S . . O4 O 0.4561(3) 0.5190(3) 0.19791(16) 0.0128(5) Uani 1 1 d . . . O3W O 0.3342(3) 0.3194(3) -0.07000(15) 0.0116(5) Uani 1 1 d . . . O2 O 0.3242(4) 0.6707(3) 0.54449(17) 0.0198(6) Uani 1 1 d . . . N2 N 0.5979(4) 0.1942(3) 0.17698(19) 0.0107(6) Uani 1 1 d . . . O6 O 0.9476(3) 0.3958(3) 0.06064(16) 0.0132(5) Uani 1 1 d . . . O5 O 0.6427(3) 0.3925(3) 0.03000(15) 0.0102(5) Uani 1 1 d . . . O2W O 0.1404(4) 0.3475(3) 0.26256(17) 0.0167(6) Uani 1 1 d . . . O1W O 0.0508(3) 0.6237(3) 0.14490(17) 0.0158(5) Uani 1 1 d . . . O3 O 0.3361(4) 0.5109(3) 0.34963(17) 0.0170(6) Uani 1 1 d . . . O7 O 0.2695(3) 0.1497(3) 0.10741(17) 0.0141(5) Uani 1 1 d . . . C6 C 0.7924(5) 0.3493(4) 0.0801(2) 0.0096(7) Uani 1 1 d . . . N1 N 0.6178(4) 0.6381(3) 0.40467(19) 0.0121(6) Uani 1 1 d . . . O1 O 0.2470(4) 0.9079(3) 0.51430(18) 0.0239(6) Uani 1 1 d . . . C5 C 0.4592(5) 0.5375(4) 0.2847(2) 0.0119(7) Uani 1 1 d . . . C1 C 0.3392(5) 0.7870(4) 0.4950(2) 0.0164(8) Uani 1 1 d . . . O8 O 0.4044(4) -0.0825(3) 0.10724(18) 0.0180(6) Uani 1 1 d . . . O4W O 1.0784(4) 0.0885(3) 0.35995(18) 0.0237(6) Uani 1 1 d . . . O5W O 0.0942(4) 0.8627(3) 0.2299(2) 0.0330(7) Uani 1 1 d . . . C9 C 0.6179(5) 0.0767(4) 0.1181(3) 0.0146(8) Uani 1 1 d . . . H9A H 0.7096 -0.0099 0.1468 0.018 Uiso 1 1 calc R . . H9B H 0.6749 0.1038 0.0536 0.018 Uiso 1 1 calc R . . C7 C 0.7819(5) 0.2465(4) 0.1679(2) 0.0123(7) Uani 1 1 d . . . H7A H 0.8977 0.1641 0.1657 0.015 Uiso 1 1 calc R . . H7B H 0.7899 0.2949 0.2247 0.015 Uiso 1 1 calc R . . C8 C 0.5625(5) 0.1375(4) 0.2771(2) 0.0160(8) Uani 1 1 d . . . H8A H 0.6810 0.0662 0.2979 0.024 Uiso 1 1 calc R . . H8B H 0.4478 0.0923 0.2825 0.024 Uiso 1 1 calc R . . H8C H 0.5351 0.2162 0.3174 0.024 Uiso 1 1 calc R . . C10 C 0.4155(5) 0.0445(4) 0.1106(2) 0.0128(7) Uani 1 1 d . . . C4 C 0.6395(5) 0.5902(4) 0.3086(2) 0.0138(7) Uani 1 1 d . . . H4A H 0.7600 0.5118 0.3042 0.017 Uiso 1 1 calc R . . H4B H 0.6590 0.6709 0.2609 0.017 Uiso 1 1 calc R . . C2 C 0.4741(6) 0.7786(4) 0.4049(2) 0.0186(8) Uani 1 1 d . . . H2A H 0.3917 0.7938 0.3491 0.022 Uiso 1 1 calc R . . H2B H 0.5484 0.8561 0.3989 0.022 Uiso 1 1 calc R . . C3 C 0.8146(6) 0.6497(5) 0.4330(3) 0.0229(9) Uani 1 1 d . . . H3A H 0.8692 0.7165 0.3860 0.034 Uiso 1 1 calc R . . H3B H 0.9059 0.5550 0.4360 0.034 Uiso 1 1 calc R . . H3C H 0.7990 0.6851 0.4958 0.034 Uiso 1 1 calc 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 Nd1 0.00612(9) 0.00867(10) 0.00831(10) -0.00183(6) -0.00015(6) -0.00171(6) Cu1 0.0174(3) 0.0126(3) 0.0094(3) -0.0010(2) 0.0007(2) -0.0020(3) O4 0.0149(12) 0.0161(13) 0.0087(12) -0.0034(10) -0.0012(9) -0.0047(10) O3W 0.0116(12) 0.0129(13) 0.0105(12) -0.0032(10) -0.0004(9) -0.0021(10) O2 0.0239(14) 0.0168(14) 0.0152(13) 0.0006(11) 0.0030(10) 0.0000(11) N2 0.0114(14) 0.0121(15) 0.0098(14) -0.0009(12) 0.0002(11) -0.0056(12) O6 0.0114(12) 0.0112(13) 0.0171(12) -0.0004(10) -0.0013(10) -0.0034(10) O5 0.0076(11) 0.0115(13) 0.0106(11) 0.0003(9) -0.0031(9) -0.0002(10) O2W 0.0156(13) 0.0205(14) 0.0132(12) -0.0001(11) 0.0001(10) -0.0038(11) O1W 0.0130(12) 0.0143(13) 0.0184(13) -0.0047(10) -0.0019(10) 0.0021(10) O3 0.0168(13) 0.0219(15) 0.0136(12) -0.0026(11) 0.0023(10) -0.0074(11) O7 0.0121(12) 0.0113(13) 0.0191(13) -0.0018(10) -0.0019(10) -0.0022(10) C6 0.0077(16) 0.0077(17) 0.0132(17) -0.0050(13) 0.0003(13) 0.0001(13) N1 0.0138(15) 0.0138(16) 0.0095(14) -0.0022(12) -0.0008(11) -0.0039(12) O1 0.0286(15) 0.0173(15) 0.0208(14) -0.0011(11) 0.0001(11) 0.0042(12) C5 0.0115(17) 0.0078(17) 0.0147(18) -0.0008(14) -0.0018(14) 0.0011(14) C1 0.0167(19) 0.020(2) 0.0123(17) -0.0028(15) -0.0037(14) -0.0016(16) O8 0.0168(13) 0.0096(13) 0.0283(14) -0.0071(11) 0.0015(11) -0.0028(11) O4W 0.0254(15) 0.0243(16) 0.0184(14) 0.0031(12) 0.0010(11) -0.0033(12) O5W 0.0391(18) 0.0274(18) 0.0372(18) -0.0059(14) 0.0052(14) -0.0185(14) C9 0.0113(17) 0.0126(19) 0.0194(18) -0.0034(15) -0.0009(14) -0.0008(14) C7 0.0092(16) 0.0109(18) 0.0160(17) 0.0014(14) -0.0018(13) -0.0017(14) C8 0.0161(18) 0.017(2) 0.0145(18) 0.0039(15) -0.0022(14) -0.0046(15) C10 0.0142(18) 0.0146(19) 0.0094(16) -0.0019(14) 0.0016(13) -0.0035(15) C4 0.0152(18) 0.0161(19) 0.0113(17) -0.0040(14) 0.0017(14) -0.0058(15) C2 0.026(2) 0.0128(19) 0.0152(18) -0.0008(15) 0.0017(15) -0.0025(16) C3 0.022(2) 0.035(2) 0.0160(19) -0.0045(17) -0.0048(15) -0.0127(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 Nd1 O7 2.433(2) . ? Nd1 O6 2.439(2) 1_455 ? Nd1 O4 2.465(2) . ? Nd1 O1W 2.504(2) . ? Nd1 O2W 2.516(2) . ? Nd1 O3W 2.546(2) . ? Nd1 O5 2.549(2) . ? Nd1 O5 2.611(2) 2_665 ? Nd1 N2 2.796(3) . ? Cu1 O2 1.944(2) 2_666 ? Cu1 O2 1.944(2) . ? Cu1 N1 2.027(3) 2_666 ? Cu1 N1 2.027(3) . ? O4 C5 1.267(4) . ? O2 C1 1.265(4) . ? N2 C7 1.460(4) . ? N2 C9 1.463(4) . ? N2 C8 1.476(4) . ? O6 C6 1.249(4) . ? O6 Nd1 2.439(2) 1_655 ? O5 C6 1.265(4) . ? O5 Nd1 2.611(2) 2_665 ? O3 C5 1.239(4) . ? O7 C10 1.254(4) . ? C6 C7 1.498(5) . ? N1 C4 1.475(4) . ? N1 C3 1.482(5) . ? N1 C2 1.483(5) . ? O1 C1 1.243(5) . ? C5 C4 1.526(5) . ? C1 C2 1.511(5) . ? O8 C10 1.250(4) . ? C9 C10 1.514(5) . ? 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 O7 Nd1 O6 73.19(8) . 1_455 ? O7 Nd1 O4 128.68(8) . . ? O6 Nd1 O4 139.61(8) 1_455 . ? O7 Nd1 O1W 134.34(8) . . ? O6 Nd1 O1W 71.15(8) 1_455 . ? O4 Nd1 O1W 70.78(8) . . ? O7 Nd1 O2W 75.46(8) . . ? O6 Nd1 O2W 80.32(8) 1_455 . ? O4 Nd1 O2W 75.20(8) . . ? O1W Nd1 O2W 71.28(8) . . ? O7 Nd1 O3W 70.66(8) . . ? O6 Nd1 O3W 77.07(7) 1_455 . ? O4 Nd1 O3W 138.31(8) . . ? O1W Nd1 O3W 125.92(7) . . ? O2W Nd1 O3W 143.41(8) . . ? O7 Nd1 O5 101.76(8) . . ? O6 Nd1 O5 146.09(8) 1_455 . ? O4 Nd1 O5 69.96(7) . . ? O1W Nd1 O5 123.70(8) . . ? O2W Nd1 O5 131.87(7) . . ? O3W Nd1 O5 69.83(7) . . ? O7 Nd1 O5 140.12(8) . 2_665 ? O6 Nd1 O5 100.84(7) 1_455 2_665 ? O4 Nd1 O5 81.74(7) . 2_665 ? O1W Nd1 O5 74.81(7) . 2_665 ? O2W Nd1 O5 143.66(8) . 2_665 ? O3W Nd1 O5 69.60(7) . 2_665 ? O5 Nd1 O5 61.04(8) . 2_665 ? O7 Nd1 N2 61.46(8) . . ? O6 Nd1 N2 133.26(8) 1_455 . ? O4 Nd1 N2 71.87(8) . . ? O1W Nd1 N2 136.38(8) . . ? O2W Nd1 N2 78.11(8) . . ? O3W Nd1 N2 97.10(8) . . ? O5 Nd1 N2 60.26(7) . . ? O5 Nd1 N2 120.76(7) 2_665 . ? O2 Cu1 O2 180.000(1) 2_666 . ? O2 Cu1 N1 85.60(11) 2_666 2_666 ? O2 Cu1 N1 94.40(11) . 2_666 ? O2 Cu1 N1 94.40(11) 2_666 . ? O2 Cu1 N1 85.60(11) . . ? N1 Cu1 N1 180.000(1) 2_666 . ? C5 O4 Nd1 139.9(2) . . ? C1 O2 Cu1 114.7(2) . . ? C7 N2 C9 110.0(3) . . ? C7 N2 C8 108.9(3) . . ? C9 N2 C8 107.8(3) . . ? C7 N2 Nd1 111.03(19) . . ? C9 N2 Nd1 102.37(19) . . ? C8 N2 Nd1 116.4(2) . . ? C6 O6 Nd1 150.3(2) . 1_655 ? C6 O5 Nd1 123.3(2) . . ? C6 O5 Nd1 108.0(2) . 2_665 ? Nd1 O5 Nd1 118.96(8) . 2_665 ? C10 O7 Nd1 126.1(2) . . ? O6 C6 O5 121.4(3) . . ? O6 C6 C7 118.5(3) . . ? O5 C6 C7 120.0(3) . . ? C4 N1 C3 109.6(3) . . ? C4 N1 C2 109.7(3) . . ? C3 N1 C2 110.3(3) . . ? C4 N1 Cu1 110.4(2) . . ? C3 N1 Cu1 110.7(2) . . ? C2 N1 Cu1 106.0(2) . . ? O3 C5 O4 125.9(3) . . ? O3 C5 C4 119.3(3) . . ? O4 C5 C4 114.7(3) . . ? O1 C1 O2 124.4(3) . . ? O1 C1 C2 117.6(3) . . ? O2 C1 C2 118.0(3) . . ? N2 C9 C10 109.7(3) . . ? N2 C7 C6 111.9(3) . . ? O8 C10 O7 124.6(3) . . ? O8 C10 C9 118.9(3) . . ? O7 C10 C9 116.5(3) . . ? N1 C4 C5 112.8(3) . . ? N1 C2 C1 111.8(3) . . ? _diffrn_measured_fraction_theta_max 1.000 _diffrn_reflns_theta_full 26.00 _diffrn_measured_fraction_theta_full 1.000 _refine_diff_density_max 0.895 _refine_diff_density_min -0.519 _refine_diff_density_rms 0.109 _vrf_PLAT306_complex6 ; PROBLEM:Isolated Oxygen Atom (H-atoms Missing ?) ....... O4W Isolated Oxygen Atom (H-atoms Missing ?) ....... O5W RESPONSE: The reason is that the oxygen atom of guest water molecule cannot be added two hydrogen atoms via difference electron density map peaks ; # end Validation Reply Form