# Electronic Supplementary Material (ESI) for CrystEngComm # This journal is © The Royal Society of Chemistry 2011 data_global _journal_coden_Cambridge 1350 _journal_volume ? _journal_page_first ? _journal_year ? loop_ _publ_author_name 'Shi, Lian-Xu' 'Xu, Xuan' 'Wu, Chuan-De' _publ_contact_author_name 'Dr Chuan-De Wu' _publ_contact_author_email cdwu@zju.edu.cn _publ_section_title ; Five intercalated coordination networks based on an identical anionic lamella of pyridine-tetracarboxylate linking up GdIII atoms and diverse hydrated cations ; # Attachment '- New1.cif' data_New1 _database_code_depnum_ccdc_archive 'CCDC 827206' #TrackingRef '- New1.cif' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C9 H10 Gd N O12' _chemical_formula_weight 481.43 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' Gd Gd -0.1653 3.9035 '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 8.7200(10) _cell_length_b 8.9690(12) _cell_length_c 9.4220(12) _cell_angle_alpha 77.951(11) _cell_angle_beta 80.690(10) _cell_angle_gamma 71.308(11) _cell_volume 679.06(15) _cell_formula_units_Z 2 _cell_measurement_temperature 293(2) _cell_measurement_reflns_used 4394 _cell_measurement_theta_min 3.16 _cell_measurement_theta_max 26.37 _exptl_crystal_description bloc _exptl_crystal_colour colorless _exptl_crystal_size_max 0.35 _exptl_crystal_size_mid 0.10 _exptl_crystal_size_min 0.07 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 2.355 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 462 _exptl_absorpt_coefficient_mu 4.954 _exptl_absorpt_correction_type empirical _exptl_absorpt_correction_T_min 0.557 _exptl_absorpt_correction_T_max 0.707 _exptl_absorpt_process_details ? _exptl_special_details ; ? ; _diffrn_ambient_temperature 293(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type ? _diffrn_measurement_method ? _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 4394 _diffrn_reflns_av_R_equivalents 0.0776 _diffrn_reflns_av_sigmaI/netI 0.1117 _diffrn_reflns_limit_h_min -10 _diffrn_reflns_limit_h_max 10 _diffrn_reflns_limit_k_min -11 _diffrn_reflns_limit_k_max 6 _diffrn_reflns_limit_l_min -10 _diffrn_reflns_limit_l_max 11 _diffrn_reflns_theta_min 3.16 _diffrn_reflns_theta_max 26.37 _reflns_number_total 2729 _reflns_number_gt 2291 _reflns_threshold_expression >2sigma(I) _computing_data_collection ? _computing_cell_refinement ? _computing_data_reduction ? _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics ? _computing_publication_material ? _refine_special_details ; Refinement of F^2^ against ALL reflections. The weighted R-factor wR and goodness of fit S are based on F^2^, conventional R-factors R are based on F, with F set to zero for negative F^2^. The threshold expression of F^2^ > 2sigma(F^2^) is used only for calculating R-factors(gt) etc. and is not relevant to the choice of reflections for refinement. R-factors based on F^2^ are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger. ; _refine_ls_structure_factor_coef Fsqd _refine_ls_matrix_type full _refine_ls_weighting_scheme calc _refine_ls_weighting_details 'calc w=1/[\s^2^(Fo^2^)+(0.0309P)^2^+31.3310P] 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 2729 _refine_ls_number_parameters 208 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0955 _refine_ls_R_factor_gt 0.0845 _refine_ls_wR_factor_ref 0.2034 _refine_ls_wR_factor_gt 0.1945 _refine_ls_goodness_of_fit_ref 1.023 _refine_ls_restrained_S_all 1.023 _refine_ls_shift/su_max 0.000 _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 Gd1 Gd 0.35480(9) 0.66438(9) 0.83314(8) 0.0318(3) Uani 1 1 d . . . O1 O 1.1601(14) 0.5969(14) 0.7299(12) 0.042(3) Uani 1 1 d . . . O2 O 0.9160(14) 0.5736(16) 0.7203(13) 0.048(3) Uani 1 1 d . . . O3 O 0.6283(13) 0.5594(13) 0.9713(12) 0.038(2) Uani 1 1 d . . . O4 O 0.5751(14) 0.7908(14) 0.8229(12) 0.040(3) Uani 1 1 d . . . O5 O 0.7736(14) 1.0663(12) 1.2640(12) 0.040(3) Uani 1 1 d . . . O6 O 0.8442(16) 0.8281(14) 1.4026(13) 0.049(3) Uani 1 1 d . . . O7 O 1.1425(14) 0.9057(15) 1.2279(13) 0.044(3) Uani 1 1 d . . . O8 O 1.3079(13) 0.7879(13) 1.0492(12) 0.037(2) Uani 1 1 d . . . O9 O 0.5176(15) 0.4233(14) 0.7416(13) 0.047(3) Uani 1 1 d . . . H9A H 0.5734 0.4495 0.6673 0.056 Uiso 1 1 d . . . H9B H 0.5558 0.3573 0.8115 0.056 Uiso 1 1 d . . . O10 O 0.4502(16) 0.7262(15) 0.5778(14) 0.050(3) Uani 1 1 d . . . H10C H 0.5489 0.7149 0.5623 0.060 Uiso 1 1 d . . . H10D H 0.4255 0.6598 0.5457 0.060 Uiso 1 1 d . . . OW1 O 0.7378(14) 0.5063(16) 0.5353(13) 0.047(3) Uani 1 1 d . . . H10E H 0.7913 0.5091 0.5980 0.057 Uiso 1 1 d . . . H10F H 0.7536 0.4925 0.4503 0.057 Uiso 1 1 d . . . OW2 O 0.2987(16) 1.0094(14) 0.3910(12) 0.044(3) Uani 1 1 d . . . H10A H 0.3499 1.0560 0.3260 0.053 Uiso 1 1 d . . . H10B H 0.2604 0.9742 0.3359 0.053 Uiso 1 1 d . . . H10G H 0.3418 0.9848 0.4669 0.053 Uiso 1 1 d . . . N1 N 1.0656(16) 0.7299(15) 0.9597(14) 0.035(3) Uani 1 1 d . . . C1 C 0.9518(18) 0.6940(18) 0.9070(17) 0.033(3) Uani 1 1 d . . . C2 C 0.7905(18) 0.7289(17) 0.9721(16) 0.030(3) Uani 1 1 d . . . C3 C 0.7555(19) 0.8004(19) 1.0939(18) 0.037(4) Uani 1 1 d . . . H3A H 0.6501 0.8240 1.1403 0.044 Uiso 1 1 calc R . . C4 C 0.874(2) 0.8380(18) 1.1491(18) 0.036(3) Uani 1 1 d . . . C5 C 1.030(2) 0.8001(18) 1.0773(17) 0.033(3) Uani 1 1 d . . . C6 C 1.011(2) 0.6125(19) 0.7710(19) 0.040(4) Uani 1 1 d . . . C7 C 0.6613(18) 0.690(2) 0.9143(17) 0.035(3) Uani 1 1 d . . . C8 C 0.8302(18) 0.9199(19) 1.2799(17) 0.034(3) Uani 1 1 d . . . C9 C 1.1679(19) 0.8382(19) 1.1242(17) 0.035(3) 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 Gd1 0.0325(4) 0.0198(4) 0.0409(5) -0.0113(3) -0.0021(3) -0.0016(3) O1 0.041(6) 0.038(7) 0.048(7) -0.029(5) 0.003(5) -0.005(5) O2 0.039(6) 0.054(8) 0.057(7) -0.036(6) 0.002(5) -0.009(6) O3 0.038(6) 0.024(6) 0.050(7) -0.012(5) -0.004(5) -0.005(5) O4 0.043(6) 0.028(6) 0.046(6) 0.002(5) -0.009(5) -0.008(5) O5 0.051(7) 0.015(5) 0.048(6) -0.011(5) -0.005(5) 0.003(5) O6 0.071(9) 0.027(6) 0.042(7) -0.009(5) -0.002(6) -0.006(6) O7 0.042(6) 0.041(7) 0.053(7) -0.029(6) -0.002(5) -0.004(5) O8 0.036(6) 0.026(6) 0.049(6) -0.014(5) -0.002(5) -0.005(5) O9 0.049(7) 0.030(6) 0.047(7) -0.014(5) -0.003(5) 0.011(5) O10 0.053(7) 0.034(7) 0.059(8) -0.014(6) -0.001(6) -0.005(6) OW1 0.042(7) 0.048(8) 0.051(7) -0.030(6) 0.001(5) -0.002(6) OW2 0.064(8) 0.034(7) 0.039(6) -0.013(5) -0.004(5) -0.018(6) N1 0.035(7) 0.022(7) 0.043(7) -0.015(6) -0.001(5) 0.001(5) C1 0.028(7) 0.019(7) 0.044(9) -0.010(6) 0.002(6) 0.002(6) C2 0.033(7) 0.018(7) 0.040(8) -0.011(6) 0.000(6) -0.004(6) C3 0.031(8) 0.024(8) 0.052(10) -0.019(7) 0.004(7) -0.001(6) C4 0.046(9) 0.015(7) 0.048(9) -0.007(6) -0.007(7) -0.008(7) C5 0.045(9) 0.015(7) 0.039(8) -0.006(6) -0.006(7) -0.005(6) C6 0.047(10) 0.021(8) 0.050(10) -0.014(7) -0.004(8) -0.001(7) C7 0.030(8) 0.031(9) 0.040(9) -0.014(7) 0.012(6) -0.009(7) C8 0.032(8) 0.024(8) 0.043(9) -0.013(7) 0.000(6) -0.001(6) C9 0.036(8) 0.025(8) 0.039(8) -0.006(7) -0.002(6) -0.002(7) _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 Gd1 O5 2.367(10) 2_677 ? Gd1 O1 2.374(11) 1_455 ? Gd1 O3 2.408(11) 2_667 ? Gd1 O9 2.419(11) . ? Gd1 O10 2.424(13) . ? Gd1 O8 2.433(11) 1_455 ? Gd1 O4 2.505(12) . ? Gd1 N1 2.549(13) 1_455 ? Gd1 O3 2.706(11) . ? Gd1 C7 2.985(16) . ? O1 C6 1.27(2) . ? O1 Gd1 2.373(11) 1_655 ? O2 C6 1.19(2) . ? O3 C7 1.282(19) . ? O3 Gd1 2.408(11) 2_667 ? O4 C7 1.25(2) . ? O5 C8 1.232(18) . ? O5 Gd1 2.367(10) 2_677 ? O6 C8 1.270(19) . ? O7 C9 1.209(19) . ? O8 C9 1.301(19) . ? O8 Gd1 2.433(11) 1_655 ? N1 C1 1.33(2) . ? N1 C5 1.332(19) . ? N1 Gd1 2.549(13) 1_655 ? C1 C2 1.40(2) . ? C1 C6 1.54(2) . ? C2 C3 1.37(2) . ? C2 C7 1.49(2) . ? C3 C4 1.39(2) . ? C4 C5 1.39(2) . ? C4 C8 1.50(2) . ? C5 C9 1.50(2) . ? 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 O5 Gd1 O1 87.1(4) 2_677 1_455 ? O5 Gd1 O3 149.4(4) 2_677 2_667 ? O1 Gd1 O3 91.2(4) 1_455 2_667 ? O5 Gd1 O9 137.5(4) 2_677 . ? O1 Gd1 O9 77.9(4) 1_455 . ? O3 Gd1 O9 71.2(4) 2_667 . ? O5 Gd1 O10 69.1(4) 2_677 . ? O1 Gd1 O10 81.5(4) 1_455 . ? O3 Gd1 O10 140.7(4) 2_667 . ? O9 Gd1 O10 69.5(4) . . ? O5 Gd1 O8 79.4(4) 2_677 1_455 ? O1 Gd1 O8 126.8(4) 1_455 1_455 ? O3 Gd1 O8 77.4(4) 2_667 1_455 ? O9 Gd1 O8 140.5(4) . 1_455 ? O10 Gd1 O8 136.6(4) . 1_455 ? O5 Gd1 O4 78.1(4) 2_677 . ? O1 Gd1 O4 153.9(4) 1_455 . ? O3 Gd1 O4 112.5(4) 2_667 . ? O9 Gd1 O4 98.6(4) . . ? O10 Gd1 O4 73.2(4) . . ? O8 Gd1 O4 71.8(4) 1_455 . ? O5 Gd1 N1 74.3(4) 2_677 1_455 ? O1 Gd1 N1 63.1(4) 1_455 1_455 ? O3 Gd1 N1 77.8(4) 2_667 1_455 ? O9 Gd1 N1 129.0(4) . 1_455 ? O10 Gd1 N1 129.7(4) . 1_455 ? O8 Gd1 N1 63.7(4) 1_455 1_455 ? O4 Gd1 N1 130.7(4) . 1_455 ? O5 Gd1 O3 125.3(4) 2_677 . ? O1 Gd1 O3 147.3(4) 1_455 . ? O3 Gd1 O3 63.6(4) 2_667 . ? O9 Gd1 O3 74.3(4) . . ? O10 Gd1 O3 104.3(4) . . ? O8 Gd1 O3 70.5(3) 1_455 . ? O4 Gd1 O3 49.9(3) . . ? N1 Gd1 O3 125.0(4) 1_455 . ? O5 Gd1 C7 101.0(4) 2_677 . ? O1 Gd1 C7 164.8(4) 1_455 . ? O3 Gd1 C7 88.3(4) 2_667 . ? O9 Gd1 C7 87.5(4) . . ? O10 Gd1 C7 89.4(4) . . ? O8 Gd1 C7 67.8(4) 1_455 . ? O4 Gd1 C7 24.5(4) . . ? N1 Gd1 C7 131.3(4) 1_455 . ? O3 Gd1 C7 25.4(4) . . ? C6 O1 Gd1 130.3(10) . 1_655 ? C7 O3 Gd1 150.1(11) . 2_667 ? C7 O3 Gd1 89.5(9) . . ? Gd1 O3 Gd1 116.4(4) 2_667 . ? C7 O4 Gd1 99.7(10) . . ? C8 O5 Gd1 162.6(11) . 2_677 ? C9 O8 Gd1 125.7(10) . 1_655 ? C1 N1 C5 120.9(13) . . ? C1 N1 Gd1 119.4(9) . 1_655 ? C5 N1 Gd1 119.7(10) . 1_655 ? N1 C1 C2 121.6(14) . . ? N1 C1 C6 115.0(13) . . ? C2 C1 C6 123.4(14) . . ? C3 C2 C1 117.1(14) . . ? C3 C2 C7 120.6(13) . . ? C1 C2 C7 122.3(13) . . ? C2 C3 C4 121.4(15) . . ? C3 C4 C5 117.6(14) . . ? C3 C4 C8 119.8(14) . . ? C5 C4 C8 122.6(14) . . ? N1 C5 C4 121.5(15) . . ? N1 C5 C9 115.9(14) . . ? C4 C5 C9 122.7(14) . . ? O2 C6 O1 129.4(16) . . ? O2 C6 C1 118.5(15) . . ? O1 C6 C1 112.1(14) . . ? O4 C7 O3 120.6(15) . . ? O4 C7 C2 120.2(14) . . ? O3 C7 C2 118.8(14) . . ? O4 C7 Gd1 55.8(8) . . ? O3 C7 Gd1 65.0(8) . . ? C2 C7 Gd1 167.9(10) . . ? O5 C8 O6 124.4(14) . . ? O5 C8 C4 119.8(14) . . ? O6 C8 C4 115.6(14) . . ? O7 C9 O8 126.1(15) . . ? O7 C9 C5 119.0(14) . . ? O8 C9 C5 114.8(14) . . ? loop_ _geom_hbond_atom_site_label_D _geom_hbond_atom_site_label_H _geom_hbond_atom_site_label_A _geom_hbond_distance_DH _geom_hbond_distance_HA _geom_hbond_distance_DA _geom_hbond_angle_DHA _geom_hbond_site_symmetry_A O9 H9A OW1 0.82 1.87 2.669(18) 164.4 . O9 H9B O8 0.82 1.91 2.712(16) 166.2 2_767 O10 H10C OW1 0.83 2.09 2.679(17) 128.0 . OW1 H10E O2 0.82 1.98 2.781(17) 164.7 . OW1 H10F O1 0.82 1.96 2.758(15) 163.2 2_766 OW2 H10A O4 0.82 1.94 2.743(16) 166.3 2_676 OW2 H10B O7 0.82 1.86 2.677(16) 171.1 1_454 OW2 H10G O10 0.82 2.30 2.834(18) 123.9 . OW2 H10G O5 0.82 2.58 3.180(16) 131.8 2_677 _diffrn_measured_fraction_theta_max 0.985 _diffrn_reflns_theta_full 26.37 _diffrn_measured_fraction_theta_full 0.985 _refine_diff_density_max 4.045 _refine_diff_density_min -2.934 _refine_diff_density_rms 0.358 # Attachment '- New2.cif' data_New2 _database_code_depnum_ccdc_archive 'CCDC 827207' #TrackingRef '- New2.cif' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C18 H30 Gd2 N2 O30 Zn' _chemical_formula_weight 1134.31 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' Zn Zn 0.2839 1.4301 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Gd Gd -0.1653 3.9035 '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 8.6761(12) _cell_length_b 9.3984(14) _cell_length_c 10.5809(17) _cell_angle_alpha 92.225(11) _cell_angle_beta 102.987(10) _cell_angle_gamma 109.636(9) _cell_volume 785.7(2) _cell_formula_units_Z 1 _cell_measurement_temperature 296(2) _cell_measurement_reflns_used 9100 _cell_measurement_theta_min 1.99 _cell_measurement_theta_max 25.06 _exptl_crystal_description Bloc _exptl_crystal_colour Colorless _exptl_crystal_size_max 0.21 _exptl_crystal_size_mid 0.05 _exptl_crystal_size_min 0.05 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 2.397 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 550 _exptl_absorpt_coefficient_mu 5.053 _exptl_absorpt_correction_type empirical _exptl_absorpt_correction_T_min 0.746 _exptl_absorpt_correction_T_max 0.777 _exptl_absorpt_process_details ? _exptl_special_details ; ? ; _diffrn_ambient_temperature 296(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type ? _diffrn_measurement_method ? _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 9100 _diffrn_reflns_av_R_equivalents 0.0976 _diffrn_reflns_av_sigmaI/netI 0.1144 _diffrn_reflns_limit_h_min -10 _diffrn_reflns_limit_h_max 10 _diffrn_reflns_limit_k_min -11 _diffrn_reflns_limit_k_max 11 _diffrn_reflns_limit_l_min -12 _diffrn_reflns_limit_l_max 12 _diffrn_reflns_theta_min 1.99 _diffrn_reflns_theta_max 25.06 _reflns_number_total 2772 _reflns_number_gt 2146 _reflns_threshold_expression >2sigma(I) _computing_data_collection ? _computing_cell_refinement ? _computing_data_reduction ? _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics ? _computing_publication_material ? _refine_special_details ; Refinement of F^2^ against ALL reflections. The weighted R-factor wR and goodness of fit S are based on F^2^, conventional R-factors R are based on F, with F set to zero for negative F^2^. The threshold expression of F^2^ > 2sigma(F^2^) is used only for calculating R-factors(gt) etc. and is not relevant to the choice of reflections for refinement. R-factors based on F^2^ are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger. ; _refine_ls_structure_factor_coef Fsqd _refine_ls_matrix_type full _refine_ls_weighting_scheme calc _refine_ls_weighting_details 'calc w=1/[\s^2^(Fo^2^)+(0.0346P)^2^+52.4967P] 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 2772 _refine_ls_number_parameters 241 _refine_ls_number_restraints 12 _refine_ls_R_factor_all 0.1160 _refine_ls_R_factor_gt 0.0837 _refine_ls_wR_factor_ref 0.1968 _refine_ls_wR_factor_gt 0.1813 _refine_ls_goodness_of_fit_ref 1.013 _refine_ls_restrained_S_all 1.012 _refine_ls_shift/su_max 0.000 _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 Gd1 Gd 0.28106(11) 0.84168(10) 0.35600(9) 0.0245(3) Uani 1 1 d . . . Zn1 Zn -0.5000 0.5000 0.0000 0.0632(12) Uani 1 2 d S . . O1 O -0.3257(15) 1.2748(14) 0.4437(12) 0.032(3) Uani 1 1 d . . . O2 O -0.2345(17) 1.3972(17) 0.2861(14) 0.046(4) Uani 1 1 d . . . O3 O 0.061(3) 1.3858(19) 0.1465(15) 0.069(5) Uani 1 1 d . . . O4 O 0.1190(17) 1.5873(15) 0.2901(15) 0.044(4) Uani 1 1 d . . . O5 O 0.3914(14) 1.0636(13) 0.5274(12) 0.029(3) Uani 1 1 d . . . O6 O 0.5039(16) 1.2769(16) 0.6598(14) 0.039(3) Uani 1 1 d . . . O7 O 0.1986(17) 1.0581(17) 0.7403(13) 0.042(4) Uani 1 1 d . . . O8 O -0.0588(15) 1.0707(15) 0.7279(13) 0.035(3) Uani 1 1 d U . . O9 O 0.4109(18) 1.0695(15) 0.2630(14) 0.048(4) Uani 1 1 d . . . H9A H 0.4650 1.1509 0.3194 0.057 Uiso 1 1 d . . . H9B H 0.4510 1.0721 0.2028 0.057 Uiso 1 1 d . . . O10 O 0.237(2) 0.7858(17) 0.1231(15) 0.057(4) Uani 1 1 d . . . H10A H 0.3143 0.8599 0.0910 0.069 Uiso 1 1 d . . . H10B H 0.2334 0.6934 0.1160 0.069 Uiso 1 1 d . . . O11 O -0.250(2) 0.494(2) 0.0315(15) 0.067(5) Uani 1 1 d . . . H11A H -0.2176 0.5485 -0.0325 0.080 Uiso 1 1 d . . . H11B H -0.1428 0.4982 0.0849 0.080 Uiso 1 1 d . . . O12 O -0.598(3) 0.266(2) -0.0239(18) 0.096(8) Uani 1 1 d . . . H12A H -0.6077 0.2294 -0.1033 0.115 Uiso 1 1 d . . . H12B H -0.5216 0.2450 0.0172 0.115 Uiso 1 1 d . . . O13 O -0.505(2) 0.5162(19) -0.1959(15) 0.064(5) Uani 1 1 d . . . H13A H -0.5182 0.4389 -0.2318 0.077 Uiso 1 1 d . . . H13B H -0.5997 0.5271 -0.2180 0.077 Uiso 1 1 d . . . OW1 O 0.344(3) 0.909(2) -0.0795(19) 0.084(6) Uani 1 1 d . . . H10C H 0.2497 0.9275 -0.1106 0.101 Uiso 1 1 d . . . H10D H 0.3109 0.8169 -0.1169 0.101 Uiso 1 1 d . . . OW2 O -0.874(4) 0.126(3) 0.0729(19) 0.122(10) Uani 1 1 d . . . H10E H -0.9174 0.1576 0.1066 0.146 Uiso 1 1 d . . . H10F H -0.7597 0.1795 0.1043 0.146 Uiso 1 1 d . . . N1 N -0.0463(17) 1.2242(15) 0.5275(14) 0.024(3) Uani 1 1 d . . . C1 C -0.051(2) 1.3016(18) 0.4271(16) 0.022(4) Uani 1 1 d . . . C2 C 0.085(2) 1.351(2) 0.3679(17) 0.024(4) Uani 1 1 d . . . C3 C 0.226(2) 1.312(2) 0.4204(17) 0.027(4) Uani 1 1 d . . . H3A H 0.3202 1.3453 0.3858 0.032 Uiso 1 1 calc R . . C4 C 0.230(2) 1.225(2) 0.5214(18) 0.028(4) Uani 1 1 d . . . C5 C 0.091(2) 1.1842(19) 0.5764(18) 0.025(4) Uani 1 1 d . . . C6 C -0.214(2) 1.330(2) 0.3814(18) 0.030(4) Uani 1 1 d . . . C7 C 0.088(2) 1.448(2) 0.2609(19) 0.032(4) Uani 1 1 d . . . C8 C 0.379(2) 1.181(2) 0.5743(18) 0.032(5) Uani 1 1 d . . . C9 C 0.079(2) 1.097(2) 0.6908(17) 0.026(4) Uani 1 1 d U . . 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 Gd1 0.0164(4) 0.0302(5) 0.0341(6) 0.0063(4) 0.0141(4) 0.0121(4) Zn1 0.076(3) 0.077(3) 0.049(2) -0.012(2) -0.005(2) 0.059(3) O1 0.027(7) 0.044(8) 0.035(8) 0.012(6) 0.010(6) 0.023(6) O2 0.031(7) 0.078(11) 0.047(9) 0.032(8) 0.022(7) 0.032(8) O3 0.129(17) 0.065(11) 0.042(10) 0.014(8) 0.035(10) 0.062(12) O4 0.040(8) 0.032(8) 0.066(10) 0.014(7) 0.028(8) 0.011(6) O5 0.024(6) 0.033(7) 0.036(7) 0.012(6) 0.017(6) 0.013(6) O6 0.030(7) 0.049(9) 0.050(9) -0.003(7) 0.012(7) 0.029(7) O7 0.042(8) 0.065(10) 0.042(8) 0.017(7) 0.020(7) 0.038(8) O8 0.026(6) 0.045(7) 0.049(7) 0.012(5) 0.019(5) 0.025(5) O9 0.048(9) 0.032(8) 0.050(9) 0.008(7) 0.015(7) -0.004(7) O10 0.069(11) 0.048(9) 0.058(11) 0.010(8) 0.029(9) 0.015(8) O11 0.058(10) 0.124(16) 0.045(10) 0.035(10) 0.006(8) 0.067(11) O12 0.14(2) 0.072(13) 0.066(13) -0.028(10) -0.042(13) 0.076(14) O13 0.078(12) 0.067(11) 0.049(10) -0.021(8) -0.022(9) 0.057(10) OW1 0.142(19) 0.079(13) 0.080(14) 0.034(11) 0.057(13) 0.080(14) OW2 0.25(3) 0.111(18) 0.059(13) 0.029(12) 0.050(17) 0.13(2) N1 0.019(7) 0.026(8) 0.037(9) 0.010(7) 0.016(7) 0.015(6) C1 0.019(8) 0.019(8) 0.028(10) 0.001(7) 0.010(7) 0.005(7) C2 0.016(8) 0.031(10) 0.030(10) -0.001(8) 0.007(8) 0.013(7) C3 0.024(9) 0.035(10) 0.036(11) 0.008(8) 0.017(8) 0.022(8) C4 0.019(9) 0.033(10) 0.036(11) 0.001(8) 0.019(8) 0.007(8) C5 0.014(8) 0.023(9) 0.041(11) 0.006(8) 0.012(8) 0.008(7) C6 0.028(9) 0.042(11) 0.031(11) 0.019(9) 0.017(9) 0.019(8) C7 0.023(9) 0.040(11) 0.046(13) 0.011(10) 0.021(9) 0.020(9) C8 0.021(10) 0.041(12) 0.049(14) 0.012(10) 0.023(9) 0.019(9) C9 0.023(7) 0.029(7) 0.033(8) -0.003(6) 0.012(6) 0.017(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 Gd1 O4 2.313(14) 1_545 ? Gd1 O8 2.354(12) 2_576 ? Gd1 O10 2.416(16) . ? Gd1 O9 2.422(13) . ? Gd1 O1 2.437(12) 2_576 ? Gd1 O5 2.478(13) . ? Gd1 O6 2.505(11) 2_676 ? Gd1 N1 2.528(12) 2_576 ? Gd1 O5 2.651(12) 2_676 ? Gd1 C8 2.955(16) 2_676 ? Zn1 O12 2.059(19) . ? Zn1 O12 2.059(19) 2_465 ? Zn1 O13 2.076(17) . ? Zn1 O13 2.076(17) 2_465 ? Zn1 O11 2.141(15) 2_465 ? Zn1 O11 2.141(15) . ? O1 C6 1.27(2) . ? O1 Gd1 2.437(12) 2_576 ? O2 C6 1.22(2) . ? O3 C7 1.26(2) . ? O4 C7 1.26(2) . ? O4 Gd1 2.313(13) 1_565 ? O5 C8 1.239(19) . ? O5 Gd1 2.651(12) 2_676 ? O6 C8 1.28(2) . ? O6 Gd1 2.505(11) 2_676 ? O7 C9 1.23(2) . ? O8 C9 1.29(2) . ? O8 Gd1 2.354(12) 2_576 ? N1 C1 1.31(2) . ? N1 C5 1.37(2) . ? N1 Gd1 2.528(12) 2_576 ? C1 C2 1.41(2) . ? C1 C6 1.50(2) . ? C2 C3 1.40(2) . ? C2 C7 1.48(2) . ? C3 C4 1.37(2) . ? C4 C5 1.40(2) . ? C4 C8 1.49(2) . ? C5 C9 1.49(2) . ? C8 Gd1 2.955(16) 2_676 ? 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 Gd1 O8 94.7(5) 1_545 2_576 ? O4 Gd1 O10 70.4(5) 1_545 . ? O8 Gd1 O10 78.1(5) 2_576 . ? O4 Gd1 O9 139.6(5) 1_545 . ? O8 Gd1 O9 75.3(5) 2_576 . ? O10 Gd1 O9 69.3(5) . . ? O4 Gd1 O1 76.8(5) 1_545 2_576 ? O8 Gd1 O1 127.1(4) 2_576 2_576 ? O10 Gd1 O1 140.4(5) . 2_576 ? O9 Gd1 O1 140.1(5) . 2_576 ? O4 Gd1 O5 148.6(4) 1_545 . ? O8 Gd1 O5 86.7(4) 2_576 . ? O10 Gd1 O5 139.8(4) . . ? O9 Gd1 O5 70.9(4) . . ? O1 Gd1 O5 77.5(4) 2_576 . ? O4 Gd1 O6 76.8(5) 1_545 2_676 ? O8 Gd1 O6 154.9(4) 2_576 2_676 ? O10 Gd1 O6 76.8(5) . 2_676 ? O9 Gd1 O6 95.8(5) . 2_676 ? O1 Gd1 O6 74.5(4) 2_576 2_676 ? O5 Gd1 O6 113.0(4) . 2_676 ? O4 Gd1 N1 72.9(5) 1_545 2_576 ? O8 Gd1 N1 64.6(4) 2_576 2_576 ? O10 Gd1 N1 124.2(5) . 2_576 ? O9 Gd1 N1 131.1(5) . 2_576 ? O1 Gd1 N1 63.0(4) 2_576 2_576 ? O5 Gd1 N1 79.6(4) . 2_576 ? O6 Gd1 N1 132.0(4) 2_676 2_576 ? O4 Gd1 O5 122.6(4) 1_545 2_676 ? O8 Gd1 O5 142.6(4) 2_576 2_676 ? O10 Gd1 O5 110.0(5) . 2_676 ? O9 Gd1 O5 74.1(4) . 2_676 ? O1 Gd1 O5 70.2(4) 2_576 2_676 ? O5 Gd1 O5 63.3(4) . 2_676 ? O6 Gd1 O5 50.1(4) 2_676 2_676 ? N1 Gd1 O5 125.1(4) 2_576 2_676 ? O4 Gd1 C8 99.5(5) 1_545 2_676 ? O8 Gd1 C8 161.4(5) 2_576 2_676 ? O10 Gd1 C8 95.2(5) . 2_676 ? O9 Gd1 C8 86.0(5) . 2_676 ? O1 Gd1 C8 68.6(4) 2_576 2_676 ? O5 Gd1 C8 87.6(5) . 2_676 ? O6 Gd1 C8 25.5(4) 2_676 2_676 ? N1 Gd1 C8 131.4(5) 2_576 2_676 ? O5 Gd1 C8 24.8(4) 2_676 2_676 ? O12 Zn1 O12 179.999(2) . 2_465 ? O12 Zn1 O13 94.5(7) . . ? O12 Zn1 O13 85.5(7) 2_465 . ? O12 Zn1 O13 85.5(7) . 2_465 ? O12 Zn1 O13 94.5(7) 2_465 2_465 ? O13 Zn1 O13 180.0(10) . 2_465 ? O12 Zn1 O11 90.0(8) . 2_465 ? O12 Zn1 O11 90.0(8) 2_465 2_465 ? O13 Zn1 O11 91.4(6) . 2_465 ? O13 Zn1 O11 88.6(6) 2_465 2_465 ? O12 Zn1 O11 90.0(8) . . ? O12 Zn1 O11 90.0(8) 2_465 . ? O13 Zn1 O11 88.6(6) . . ? O13 Zn1 O11 91.4(6) 2_465 . ? O11 Zn1 O11 180.000(1) 2_465 . ? C6 O1 Gd1 124.9(11) . 2_576 ? C7 O4 Gd1 157.5(12) . 1_565 ? C8 O5 Gd1 149.3(12) . . ? C8 O5 Gd1 91.5(11) . 2_676 ? Gd1 O5 Gd1 116.7(4) . 2_676 ? C8 O6 Gd1 97.3(9) . 2_676 ? C9 O8 Gd1 127.0(11) . 2_576 ? C1 N1 C5 120.6(13) . . ? C1 N1 Gd1 121.2(10) . 2_576 ? C5 N1 Gd1 118.1(10) . 2_576 ? N1 C1 C2 122.1(15) . . ? N1 C1 C6 114.0(13) . . ? C2 C1 C6 123.9(15) . . ? C3 C2 C1 116.9(15) . . ? C3 C2 C7 119.5(14) . . ? C1 C2 C7 123.5(15) . . ? C4 C3 C2 121.5(15) . . ? C3 C4 C5 117.7(16) . . ? C3 C4 C8 121.1(14) . . ? C5 C4 C8 121.2(16) . . ? N1 C5 C4 121.2(16) . . ? N1 C5 C9 114.4(13) . . ? C4 C5 C9 124.4(15) . . ? O2 C6 O1 124.2(17) . . ? O2 C6 C1 119.6(15) . . ? O1 C6 C1 116.1(14) . . ? O4 C7 O3 124.2(18) . . ? O4 C7 C2 117.8(17) . . ? O3 C7 C2 118.0(17) . . ? O5 C8 O6 120.5(15) . . ? O5 C8 C4 121.2(18) . . ? O6 C8 C4 117.8(15) . . ? O5 C8 Gd1 63.8(9) . 2_676 ? O6 C8 Gd1 57.2(8) . 2_676 ? C4 C8 Gd1 165.3(12) . 2_676 ? O7 C9 O8 126.4(17) . . ? O7 C9 C5 118.0(15) . . ? O8 C9 C5 115.5(15) . . ? loop_ _geom_hbond_atom_site_label_D _geom_hbond_atom_site_label_H _geom_hbond_atom_site_label_A _geom_hbond_distance_DH _geom_hbond_distance_HA _geom_hbond_distance_DA _geom_hbond_angle_DHA _geom_hbond_site_symmetry_A O9 H9A O1 0.87 1.94 2.718(19) 147.7 1_655 O9 H9B OW1 0.79 2.39 3.15(2) 160.4 2_675 O10 H10A OW1 0.93 1.93 2.68(2) 136.1 . O10 H10B O11 0.86 2.37 3.09(2) 141.9 2_565 O10 H10B O4 0.86 2.38 2.728(19) 104.6 1_545 O11 H11A O3 0.90 1.98 2.79(2) 149.9 2_575 O11 H11A O13 0.90 2.61 2.95(2) 103.1 . O11 H11B O3 0.96 2.34 3.20(2) 149.8 1_545 O11 H11B O2 0.96 2.55 2.87(2) 99.6 1_545 O11 H11B O4 0.96 2.63 3.53(2) 156.2 1_545 O12 H12A O7 0.87 2.21 2.91(2) 137.7 1_444 O12 H12B OW1 0.79 2.45 3.19(2) 157.1 2_565 O13 H13A O6 0.77 1.96 2.700(19) 163.5 1_444 O13 H13B O2 0.85 1.83 2.650(19) 161.9 2_475 OW1 H10C O7 0.89 2.10 2.74(2) 128.7 1_554 OW1 H10D O2 0.86 2.45 3.27(2) 160.5 2_575 OW2 H10E O3 0.69 2.24 2.80(2) 137.9 1_445 OW2 H10F O12 0.92 2.16 2.76(4) 122.1 . OW2 H10F O9 0.92 2.47 3.03(3) 118.9 1_445 _diffrn_measured_fraction_theta_max 0.990 _diffrn_reflns_theta_full 25.06 _diffrn_measured_fraction_theta_full 0.990 _refine_diff_density_max 5.949 _refine_diff_density_min -4.101 _refine_diff_density_rms 0.361 # Attachment '- New3.cif' data_New3 _database_code_depnum_ccdc_archive 'CCDC 827208' #TrackingRef '- New3.cif' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C18 H30 Cu Gd2 N2 O30' _chemical_formula_weight 1132.48 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' Gd Gd -0.1653 3.9035 '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 8.6552(10) _cell_length_b 9.2760(11) _cell_length_c 10.6950(11) _cell_angle_alpha 93.603(6) _cell_angle_beta 101.819(6) _cell_angle_gamma 109.742(6) _cell_volume 782.89(15) _cell_formula_units_Z 1 _cell_measurement_temperature 296(2) _cell_measurement_reflns_used 7707 _cell_measurement_theta_min 1.97 _cell_measurement_theta_max 25.05 _exptl_crystal_description Bloc _exptl_crystal_colour Blue _exptl_crystal_size_max 0.19 _exptl_crystal_size_mid 0.06 _exptl_crystal_size_min 0.05 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 2.402 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 549 _exptl_absorpt_coefficient_mu 4.984 _exptl_absorpt_correction_type empirical _exptl_absorpt_correction_T_min 0.705 _exptl_absorpt_correction_T_max 0.779 _exptl_absorpt_process_details ? _exptl_special_details ; ? ; _diffrn_ambient_temperature 296(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type ? _diffrn_measurement_method ? _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 7707 _diffrn_reflns_av_R_equivalents 0.0511 _diffrn_reflns_av_sigmaI/netI 0.0630 _diffrn_reflns_limit_h_min -10 _diffrn_reflns_limit_h_max 10 _diffrn_reflns_limit_k_min -11 _diffrn_reflns_limit_k_max 11 _diffrn_reflns_limit_l_min -12 _diffrn_reflns_limit_l_max 12 _diffrn_reflns_theta_min 1.97 _diffrn_reflns_theta_max 25.05 _reflns_number_total 2661 _reflns_number_gt 2223 _reflns_threshold_expression >2sigma(I) _computing_data_collection ? _computing_cell_refinement ? _computing_data_reduction ? _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics ? _computing_publication_material ? _refine_special_details ; Refinement of F^2^ against ALL reflections. The weighted R-factor wR and goodness of fit S are based on F^2^, conventional R-factors R are based on F, with F set to zero for negative F^2^. The threshold expression of F^2^ > 2sigma(F^2^) is used only for calculating R-factors(gt) etc. and is not relevant to the choice of reflections for refinement. R-factors based on F^2^ are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger. ; _refine_ls_structure_factor_coef Fsqd _refine_ls_matrix_type full _refine_ls_weighting_scheme calc _refine_ls_weighting_details 'calc w=1/[\s^2^(Fo^2^)+(0.0689P)^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 2661 _refine_ls_number_parameters 241 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0571 _refine_ls_R_factor_gt 0.0457 _refine_ls_wR_factor_ref 0.1144 _refine_ls_wR_factor_gt 0.1089 _refine_ls_goodness_of_fit_ref 1.048 _refine_ls_restrained_S_all 1.048 _refine_ls_shift/su_max 0.000 _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 Gd1 Gd 0.28741(5) 0.83912(5) 0.35525(4) 0.02434(18) Uani 1 1 d . . . Cu1 Cu -0.5000 0.5000 0.0000 0.0610(6) Uani 1 2 d S . . O1 O -0.3244(7) 1.2800(7) 0.4493(5) 0.0295(14) Uani 1 1 d . . . O2 O -0.2330(8) 1.3986(8) 0.2898(6) 0.0446(17) Uani 1 1 d . . . O3 O 0.0498(13) 1.3639(8) 0.1507(7) 0.070(3) Uani 1 1 d . . . O4 O 0.1216(8) 1.5808(7) 0.2787(6) 0.0386(16) Uani 1 1 d . . . O5 O 0.3876(7) 1.0626(6) 0.5277(5) 0.0308(14) Uani 1 1 d . . . O6 O 0.4971(8) 1.2813(7) 0.6585(6) 0.0375(15) Uani 1 1 d . . . O7 O 0.1940(8) 1.0687(8) 0.7432(6) 0.0427(17) Uani 1 1 d . . . O8 O -0.0621(7) 1.0813(7) 0.7317(5) 0.0316(14) Uani 1 1 d . . . O9 O 0.4143(9) 1.0719(7) 0.2678(6) 0.051(2) Uani 1 1 d . . . H9A H 0.4650 1.1509 0.3194 0.061 Uiso 1 1 d . . . H9B H 0.4510 1.0721 0.2028 0.061 Uiso 1 1 d . . . O10 O 0.2655(11) 0.7884(8) 0.1267(7) 0.060(2) Uani 1 1 d . . . H10A H 0.3143 0.8599 0.0910 0.072 Uiso 1 1 d . . . H10B H 0.2334 0.6934 0.1160 0.072 Uiso 1 1 d . . . O11 O -0.2216(11) 0.4920(9) 0.0239(7) 0.060(2) Uani 1 1 d . . . H11A H -0.2176 0.5485 -0.0325 0.072 Uiso 1 1 d . . . H11B H -0.1428 0.4982 0.0849 0.072 Uiso 1 1 d . . . O12 O -0.5991(12) 0.2718(9) -0.0297(7) 0.075(3) Uani 1 1 d . . . H12A H -0.6077 0.2294 -0.1033 0.090 Uiso 1 1 d . . . H12B H -0.5216 0.2450 0.0172 0.090 Uiso 1 1 d . . . O13 O -0.5102(10) 0.5165(9) -0.1860(7) 0.058(2) Uani 1 1 d . . . H13A H -0.5182 0.4389 -0.2318 0.070 Uiso 1 1 d . . . H13B H -0.5997 0.5271 -0.2180 0.070 Uiso 1 1 d . . . OW1 O 0.3412(15) 0.9102(11) -0.0921(9) 0.087(3) Uani 1 1 d . . . H10C H 0.2497 0.9275 -0.1106 0.105 Uiso 1 1 d . . . H10D H 0.3109 0.8169 -0.1169 0.105 Uiso 1 1 d . . . OW2 O -0.8579(17) 0.1231(11) 0.0733(8) 0.105(4) Uani 1 1 d . . . H10E H -0.9174 0.1576 0.1066 0.126 Uiso 1 1 d . . . H10F H -0.7597 0.1795 0.1043 0.126 Uiso 1 1 d . . . N1 N -0.0503(8) 1.2244(7) 0.5305(6) 0.0210(15) Uani 1 1 d . . . C1 C -0.0518(10) 1.3042(9) 0.4298(7) 0.0233(18) Uani 1 1 d . . . C2 C 0.0841(10) 1.3517(9) 0.3708(8) 0.0239(18) Uani 1 1 d . . . C3 C 0.2206(11) 1.3106(9) 0.4201(8) 0.0269(19) Uani 1 1 d . . . H3A H 0.3126 1.3389 0.3827 0.032 Uiso 1 1 calc R . . C4 C 0.2253(10) 1.2279(9) 0.5244(7) 0.0230(18) Uani 1 1 d . . . C5 C 0.0851(10) 1.1898(9) 0.5777(8) 0.0256(19) Uani 1 1 d . . . C6 C -0.2178(10) 1.3313(9) 0.3858(8) 0.0250(19) Uani 1 1 d . . . C7 C 0.0858(10) 1.4404(10) 0.2573(8) 0.0274(19) Uani 1 1 d . . . C8 C 0.3747(10) 1.1845(10) 0.5754(8) 0.0262(19) Uani 1 1 d . . . C9 C 0.0728(11) 1.1050(10) 0.6948(8) 0.028(2) 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 Gd1 0.0141(2) 0.0280(3) 0.0341(3) 0.00973(17) 0.00643(16) 0.01015(17) Cu1 0.0767(15) 0.0615(13) 0.0470(11) -0.0162(9) -0.0216(10) 0.0531(12) O1 0.017(3) 0.041(4) 0.035(3) 0.018(3) 0.007(2) 0.013(3) O2 0.023(3) 0.066(5) 0.061(4) 0.040(4) 0.016(3) 0.028(3) O3 0.140(9) 0.053(5) 0.033(4) 0.010(4) 0.023(5) 0.053(5) O4 0.037(4) 0.025(3) 0.048(4) 0.009(3) 0.007(3) 0.005(3) O5 0.022(3) 0.030(3) 0.042(4) 0.005(3) 0.010(3) 0.010(3) O6 0.025(3) 0.042(4) 0.048(4) -0.002(3) 0.000(3) 0.023(3) O7 0.030(4) 0.073(5) 0.045(4) 0.024(3) 0.014(3) 0.039(4) O8 0.020(3) 0.047(4) 0.039(3) 0.020(3) 0.015(3) 0.019(3) O9 0.054(5) 0.039(4) 0.039(4) 0.013(3) 0.003(3) -0.004(3) O10 0.101(7) 0.037(4) 0.047(4) 0.015(3) 0.029(4) 0.025(4) O11 0.072(6) 0.073(5) 0.049(4) 0.019(4) 0.003(4) 0.048(5) O12 0.097(7) 0.064(5) 0.060(5) -0.023(4) -0.032(5) 0.061(5) O13 0.058(5) 0.072(5) 0.048(4) -0.015(4) -0.016(4) 0.050(4) OW1 0.130(9) 0.081(6) 0.081(6) 0.037(5) 0.035(6) 0.066(6) OW2 0.222(13) 0.096(7) 0.057(5) 0.030(5) 0.046(7) 0.121(8) N1 0.009(3) 0.025(4) 0.033(4) 0.009(3) 0.005(3) 0.009(3) C1 0.018(4) 0.027(4) 0.025(4) 0.003(3) 0.006(3) 0.008(4) C2 0.014(4) 0.026(4) 0.030(4) 0.007(3) 0.005(3) 0.006(3) C3 0.022(5) 0.034(5) 0.033(5) 0.009(4) 0.013(4) 0.017(4) C4 0.016(4) 0.021(4) 0.034(5) 0.002(3) 0.007(3) 0.008(3) C5 0.016(4) 0.027(5) 0.035(5) 0.005(4) 0.011(4) 0.007(4) C6 0.018(4) 0.022(4) 0.039(5) 0.009(4) 0.007(4) 0.010(4) C7 0.016(4) 0.040(5) 0.033(5) 0.009(4) 0.006(3) 0.017(4) C8 0.015(4) 0.040(5) 0.033(5) 0.010(4) 0.016(4) 0.014(4) C9 0.022(5) 0.038(5) 0.028(5) 0.010(4) 0.003(4) 0.017(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 Gd1 O4 2.328(6) 1_545 ? Gd1 O8 2.352(6) 2_576 ? Gd1 O9 2.411(6) . ? Gd1 O10 2.417(7) . ? Gd1 O1 2.438(5) 2_576 ? Gd1 O5 2.470(6) . ? Gd1 O6 2.499(6) 2_676 ? Gd1 N1 2.521(6) 2_576 ? Gd1 O5 2.644(6) 2_676 ? Gd1 C8 2.952(8) 2_676 ? Cu1 O12 1.973(8) 2_465 ? Cu1 O12 1.973(8) . ? Cu1 O13 1.991(7) 2_465 ? Cu1 O13 1.991(7) . ? Cu1 O11 2.398(8) . ? Cu1 O11 2.398(8) 2_465 ? O1 C6 1.241(10) . ? O1 Gd1 2.438(5) 2_576 ? O2 C6 1.242(10) . ? O3 C7 1.226(10) . ? O4 C7 1.227(10) . ? O4 Gd1 2.328(6) 1_565 ? O5 C8 1.260(10) . ? O5 Gd1 2.644(6) 2_676 ? O6 C8 1.261(10) . ? O6 Gd1 2.499(6) 2_676 ? O7 C9 1.232(10) . ? O8 C9 1.262(10) . ? O8 Gd1 2.352(6) 2_576 ? N1 C5 1.328(11) . ? N1 C1 1.344(10) . ? N1 Gd1 2.521(6) 2_576 ? C1 C2 1.402(11) . ? C1 C6 1.526(11) . ? C2 C3 1.376(12) . ? C2 C7 1.508(11) . ? C3 C4 1.395(11) . ? C4 C5 1.393(11) . ? C4 C8 1.490(12) . ? C5 C9 1.523(12) . ? C8 Gd1 2.952(8) 2_676 ? 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 Gd1 O8 91.4(2) 1_545 2_576 ? O4 Gd1 O9 137.9(2) 1_545 . ? O8 Gd1 O9 74.9(2) 2_576 . ? O4 Gd1 O10 70.5(2) 1_545 . ? O8 Gd1 O10 78.8(2) 2_576 . ? O9 Gd1 O10 67.9(2) . . ? O4 Gd1 O1 78.6(2) 1_545 2_576 ? O8 Gd1 O1 127.07(19) 2_576 2_576 ? O9 Gd1 O1 141.0(2) . 2_576 ? O10 Gd1 O1 140.3(2) . 2_576 ? O4 Gd1 O5 149.3(2) 1_545 . ? O8 Gd1 O5 87.9(2) 2_576 . ? O9 Gd1 O5 71.2(2) . . ? O10 Gd1 O5 138.9(2) . . ? O1 Gd1 O5 77.47(19) 2_576 . ? O4 Gd1 O6 77.3(2) 1_545 2_676 ? O8 Gd1 O6 154.1(2) 2_576 2_676 ? O9 Gd1 O6 97.9(3) . 2_676 ? O10 Gd1 O6 75.5(3) . 2_676 ? O1 Gd1 O6 73.9(2) 2_576 2_676 ? O5 Gd1 O6 113.66(19) . 2_676 ? O4 Gd1 N1 74.4(2) 1_545 2_576 ? O8 Gd1 N1 64.4(2) 2_576 2_576 ? O9 Gd1 N1 129.0(2) . 2_576 ? O10 Gd1 N1 127.6(3) . 2_576 ? O1 Gd1 N1 62.81(19) 2_576 2_576 ? O5 Gd1 N1 77.67(19) . 2_576 ? O6 Gd1 N1 131.8(2) 2_676 2_576 ? O4 Gd1 O5 124.1(2) 1_545 2_676 ? O8 Gd1 O5 144.25(19) 2_576 2_676 ? O9 Gd1 O5 75.1(2) . 2_676 ? O10 Gd1 O5 107.1(2) . 2_676 ? O1 Gd1 O5 70.61(18) 2_576 2_676 ? O5 Gd1 O5 64.1(2) . 2_676 ? O6 Gd1 O5 50.16(18) 2_676 2_676 ? N1 Gd1 O5 124.65(19) 2_576 2_676 ? O4 Gd1 C8 100.1(2) 1_545 2_676 ? O8 Gd1 C8 162.6(2) 2_576 2_676 ? O9 Gd1 C8 87.8(2) . 2_676 ? O10 Gd1 C8 92.7(3) . 2_676 ? O1 Gd1 C8 68.6(2) 2_576 2_676 ? O5 Gd1 C8 88.8(2) . 2_676 ? O6 Gd1 C8 25.0(2) 2_676 2_676 ? N1 Gd1 C8 131.3(2) 2_576 2_676 ? O5 Gd1 C8 25.26(19) 2_676 2_676 ? O12 Cu1 O12 180.0(6) 2_465 . ? O12 Cu1 O13 93.7(3) 2_465 2_465 ? O12 Cu1 O13 86.3(3) . 2_465 ? O12 Cu1 O13 86.3(3) 2_465 . ? O12 Cu1 O13 93.7(3) . . ? O13 Cu1 O13 180.0 2_465 . ? O12 Cu1 O11 89.3(3) 2_465 . ? O12 Cu1 O11 90.7(3) . . ? O13 Cu1 O11 91.4(3) 2_465 . ? O13 Cu1 O11 88.6(3) . . ? O12 Cu1 O11 90.7(3) 2_465 2_465 ? O12 Cu1 O11 89.3(3) . 2_465 ? O13 Cu1 O11 88.6(3) 2_465 2_465 ? O13 Cu1 O11 91.4(3) . 2_465 ? O11 Cu1 O11 180.0 . 2_465 ? C6 O1 Gd1 126.9(5) . 2_576 ? C7 O4 Gd1 158.1(6) . 1_565 ? C8 O5 Gd1 149.8(6) . . ? C8 O5 Gd1 91.2(5) . 2_676 ? Gd1 O5 Gd1 115.9(2) . 2_676 ? C8 O6 Gd1 98.0(5) . 2_676 ? C9 O8 Gd1 127.3(5) . 2_576 ? C5 N1 C1 119.4(7) . . ? C5 N1 Gd1 119.0(5) . 2_576 ? C1 N1 Gd1 121.3(5) . 2_576 ? N1 C1 C2 122.6(8) . . ? N1 C1 C6 112.7(7) . . ? C2 C1 C6 124.7(7) . . ? C3 C2 C1 116.5(7) . . ? C3 C2 C7 119.7(7) . . ? C1 C2 C7 123.8(7) . . ? C2 C3 C4 122.0(8) . . ? C5 C4 C3 116.7(8) . . ? C5 C4 C8 122.5(7) . . ? C3 C4 C8 120.8(7) . . ? N1 C5 C4 122.7(8) . . ? N1 C5 C9 114.0(7) . . ? C4 C5 C9 123.3(8) . . ? O1 C6 O2 127.3(8) . . ? O1 C6 C1 115.6(7) . . ? O2 C6 C1 117.1(7) . . ? O4 C7 O3 125.8(8) . . ? O4 C7 C2 118.0(7) . . ? O3 C7 C2 116.2(8) . . ? O5 C8 O6 120.1(8) . . ? O5 C8 C4 121.4(7) . . ? O6 C8 C4 118.0(8) . . ? O5 C8 Gd1 63.6(4) . 2_676 ? O6 C8 Gd1 57.0(4) . 2_676 ? C4 C8 Gd1 166.1(6) . 2_676 ? O7 C9 O8 127.5(8) . . ? O7 C9 C5 117.3(8) . . ? O8 C9 C5 115.2(7) . . ? loop_ _geom_hbond_atom_site_label_D _geom_hbond_atom_site_label_H _geom_hbond_atom_site_label_A _geom_hbond_distance_DH _geom_hbond_distance_HA _geom_hbond_distance_DA _geom_hbond_angle_DHA _geom_hbond_site_symmetry_A O9 H9A O1 0.82 1.99 2.719(8) 148.0 1_655 O9 H9B OW1 0.82 2.32 3.078(13) 154.5 2_675 O10 H10A OW1 0.82 2.08 2.764(11) 140.4 . O10 H10B O11 0.82 2.17 2.839(10) 138.8 2_565 O10 H10B O4 0.82 2.30 2.739(9) 114.0 1_545 O11 H11A O3 0.82 2.11 2.755(12) 135.3 2_575 O11 H11A O13 0.82 2.63 3.080(10) 115.8 . O11 H11B O3 0.82 2.42 3.091(11) 139.0 1_545 O11 H11B O2 0.82 2.59 3.035(10) 114.9 1_545 O11 H11B O4 0.82 2.61 3.417(10) 167.8 1_545 O12 H12A O7 0.83 2.16 2.832(9) 137.2 1_444 O12 H12B OW1 0.87 2.51 3.341(12) 160.3 2_565 O13 H13A O6 0.82 1.87 2.686(9) 170.7 1_444 O13 H13B O2 0.82 1.86 2.660(9) 165.7 2_475 OW1 H10C O7 0.85 2.18 2.750(11) 124.1 1_554 OW1 H10D O2 0.82 2.45 3.188(12) 150.5 2_575 OW2 H10E O3 0.82 2.07 2.748(11) 140.8 1_445 OW2 H10F O12 0.82 2.21 2.693(16) 118.0 . OW2 H10F O9 0.82 2.55 2.996(13) 116.1 1_445 _diffrn_measured_fraction_theta_max 0.958 _diffrn_reflns_theta_full 25.05 _diffrn_measured_fraction_theta_full 0.958 _refine_diff_density_max 1.348 _refine_diff_density_min -2.007 _refine_diff_density_rms 0.206 # Attachment '- New4.cif' data_New4 _database_code_depnum_ccdc_archive 'CCDC 827209' #TrackingRef '- New4.cif' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C18 H28 Co Gd2 N2 O29' _chemical_formula_weight 1109.85 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' Co Co 0.3494 0.9721 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Gd Gd -0.1653 3.9035 '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 8.7113(3) _cell_length_b 9.1913(4) _cell_length_c 10.5321(4) _cell_angle_alpha 86.054(2) _cell_angle_beta 77.189(2) _cell_angle_gamma 71.101(2) _cell_volume 777.96(5) _cell_formula_units_Z 1 _cell_measurement_temperature 296(2) _cell_measurement_reflns_used 7342 _cell_measurement_theta_min 1.98 _cell_measurement_theta_max 25.06 _exptl_crystal_description Bloc _exptl_crystal_colour Pink _exptl_crystal_size_max 0.27 _exptl_crystal_size_mid 0.11 _exptl_crystal_size_min 0.08 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 2.369 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 537 _exptl_absorpt_coefficient_mu 4.861 _exptl_absorpt_correction_type empirical _exptl_absorpt_correction_T_min 0.532 _exptl_absorpt_correction_T_max 0.678 _exptl_absorpt_process_details ? _exptl_special_details ; ? ; _diffrn_ambient_temperature 296(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type ? _diffrn_measurement_method ? _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 7342 _diffrn_reflns_av_R_equivalents 0.0248 _diffrn_reflns_av_sigmaI/netI 0.0292 _diffrn_reflns_limit_h_min -10 _diffrn_reflns_limit_h_max 10 _diffrn_reflns_limit_k_min -10 _diffrn_reflns_limit_k_max 10 _diffrn_reflns_limit_l_min -12 _diffrn_reflns_limit_l_max 12 _diffrn_reflns_theta_min 1.98 _diffrn_reflns_theta_max 25.06 _reflns_number_total 2690 _reflns_number_gt 2496 _reflns_threshold_expression >2sigma(I) _computing_data_collection ? _computing_cell_refinement ? _computing_data_reduction ? _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics ? _computing_publication_material ? _refine_special_details ; Refinement of F^2^ against ALL reflections. The weighted R-factor wR and goodness of fit S are based on F^2^, conventional R-factors R are based on F, with F set to zero for negative F^2^. The threshold expression of F^2^ > 2sigma(F^2^) is used only for calculating R-factors(gt) etc. and is not relevant to the choice of reflections for refinement. R-factors based on F^2^ are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger. ; _refine_ls_structure_factor_coef Fsqd _refine_ls_matrix_type full _refine_ls_weighting_scheme calc _refine_ls_weighting_details 'calc w=1/[\s^2^(Fo^2^)+(0.0423P)^2^+0.9299P] 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 2690 _refine_ls_number_parameters 241 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0279 _refine_ls_R_factor_gt 0.0250 _refine_ls_wR_factor_ref 0.0659 _refine_ls_wR_factor_gt 0.0639 _refine_ls_goodness_of_fit_ref 1.047 _refine_ls_restrained_S_all 1.047 _refine_ls_shift/su_max 0.000 _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 Gd1 Gd 0.78572(2) 0.13028(2) 0.145297(18) 0.01554(9) Uani 1 1 d . . . Co1 Co 0.0000 0.5000 0.5000 0.0231(2) Uani 1 2 d S . . O1 O 0.1820(4) 0.7229(3) 0.0543(3) 0.0205(6) Uani 1 1 d . . . O2 O 0.2834(4) 0.5772(4) 0.2123(3) 0.0322(8) Uani 1 1 d . . . O3 O 0.6341(4) 0.3790(4) 0.2043(3) 0.0305(8) Uani 1 1 d . . . O4 O 0.5812(5) 0.5659(4) 0.3454(3) 0.0352(8) Uani 1 1 d . . . O5 O 1.0014(4) 0.7497(4) -0.1710(3) 0.0269(7) Uani 1 1 d . . . O6 O 0.8923(4) 0.9420(3) -0.0334(3) 0.0212(7) Uani 1 1 d . . . O7 O 0.4388(4) 0.9630(4) -0.2382(3) 0.0244(7) Uani 1 1 d . . . O8 O 0.6929(6) 0.9745(6) -0.2548(5) 0.0684(16) Uani 1 1 d . . . O9 O 0.7499(5) 0.1458(4) 0.3833(3) 0.0343(8) Uani 1 1 d . . . H9A H 0.8218 0.1138 0.4256 0.041 Uiso 1 1 d . . . H9B H 0.6571 0.1571 0.4272 0.041 Uiso 1 1 d . . . O10 O 0.9199(4) -0.1160(4) 0.2312(3) 0.0352(8) Uani 1 1 d . . . H10A H 0.9926 -0.1780 0.1801 0.042 Uiso 1 1 d . . . H10B H 0.9046 -0.1659 0.2981 0.042 Uiso 1 1 d . . . O11 O 0.0166(4) 0.4934(4) 0.3014(3) 0.0319(8) Uani 1 1 d . . . H11A H 0.0206 0.4164 0.2648 0.038 Uiso 1 1 d . . . H11B H 0.0999 0.5134 0.2633 0.038 Uiso 1 1 d . . . O12 O 0.2146(4) 0.5671(4) 0.4837(3) 0.0336(8) Uani 1 1 d . . . H12A H 0.2610 0.5761 0.4081 0.040 Uiso 1 1 d . . . H12B H 0.2857 0.5303 0.5266 0.040 Uiso 1 1 d . . . O13 O 0.1352(5) 0.2635(4) 0.5082(4) 0.0383(9) Uani 1 1 d . . . H13A H 0.2335 0.2344 0.5121 0.046 Uiso 1 1 d . . . H13B H 0.1283 0.2064 0.4547 0.046 Uiso 1 1 d . . . OW1 O 0.4478(5) 0.1684(4) 0.5509(3) 0.0327(8) Uani 1 1 d . . . H10C H 0.4522 0.0911 0.5954 0.039 Uiso 1 1 d . . . H10D H 0.4431 0.2401 0.5952 0.039 Uiso 1 1 d . . . OW2 O 0.0661(10) 0.0197(10) 0.4445(7) 0.047(2) Uani 0.50 1 d P . . N1 N 0.4564(4) 0.7893(4) -0.0327(3) 0.0168(7) Uani 1 1 d . . . C1 C 0.4577(5) 0.6928(5) 0.0676(4) 0.0171(9) Uani 1 1 d . . . C2 C 0.5961(5) 0.6296(5) 0.1236(4) 0.0172(9) Uani 1 1 d . . . C3 C 0.7355(5) 0.6751(5) 0.0703(4) 0.0193(9) Uani 1 1 d . . . H3A H 0.8299 0.6375 0.1053 0.023 Uiso 1 1 calc R . . C4 C 0.7346(5) 0.7749(5) -0.0337(4) 0.0178(9) Uani 1 1 d . . . C5 C 0.5919(5) 0.8285(5) -0.0856(4) 0.0182(9) Uani 1 1 d . . . C6 C 0.2958(5) 0.6603(5) 0.1163(4) 0.0185(9) Uani 1 1 d . . . C7 C 0.6012(5) 0.5168(5) 0.2342(4) 0.0188(9) Uani 1 1 d . . . C8 C 0.8834(5) 0.8271(5) -0.0856(4) 0.0187(9) Uani 1 1 d . . . C9 C 0.5765(6) 0.9313(6) -0.2024(4) 0.0250(10) 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 Gd1 0.01011(14) 0.01911(13) 0.01837(14) 0.00037(8) -0.00339(8) -0.00576(9) Co1 0.0189(5) 0.0305(5) 0.0216(5) -0.0005(4) -0.0024(3) -0.0115(4) O1 0.0109(16) 0.0300(17) 0.0214(16) 0.0030(13) -0.0046(12) -0.0073(13) O2 0.0221(19) 0.049(2) 0.0312(19) 0.0187(16) -0.0101(15) -0.0196(16) O3 0.032(2) 0.0182(17) 0.036(2) 0.0003(14) -0.0044(15) -0.0034(14) O4 0.054(3) 0.0338(19) 0.0224(19) 0.0012(14) -0.0128(16) -0.0173(17) O5 0.0174(18) 0.0376(19) 0.0292(18) -0.0109(14) 0.0021(14) -0.0157(14) O6 0.0194(17) 0.0235(16) 0.0249(17) 0.0013(13) -0.0090(13) -0.0100(13) O7 0.0153(17) 0.0336(18) 0.0286(18) 0.0093(14) -0.0086(13) -0.0126(14) O8 0.042(3) 0.119(4) 0.071(3) 0.066(3) -0.037(2) -0.058(3) O9 0.027(2) 0.045(2) 0.0290(19) 0.0039(15) -0.0065(15) -0.0099(16) O10 0.030(2) 0.0298(19) 0.0281(19) 0.0053(15) 0.0054(15) 0.0063(15) O11 0.032(2) 0.045(2) 0.0264(18) -0.0061(15) 0.0022(15) -0.0268(17) O12 0.0230(19) 0.053(2) 0.0279(19) 0.0086(16) -0.0051(14) -0.0187(17) O13 0.029(2) 0.038(2) 0.050(2) -0.0056(17) -0.0124(17) -0.0087(16) OW1 0.041(2) 0.0278(18) 0.0302(19) 0.0010(14) -0.0107(16) -0.0106(16) OW2 0.038(5) 0.064(5) 0.043(5) 0.003(4) -0.016(4) -0.016(4) N1 0.0137(19) 0.0222(19) 0.0157(18) 0.0023(14) -0.0035(14) -0.0077(15) C1 0.014(2) 0.020(2) 0.019(2) -0.0049(17) -0.0015(17) -0.0067(17) C2 0.014(2) 0.020(2) 0.018(2) -0.0054(16) -0.0018(16) -0.0050(17) C3 0.014(2) 0.025(2) 0.021(2) -0.0009(17) -0.0058(17) -0.0076(17) C4 0.015(2) 0.019(2) 0.021(2) -0.0032(17) -0.0026(17) -0.0069(17) C5 0.015(2) 0.021(2) 0.021(2) -0.0005(17) -0.0024(17) -0.0100(17) C6 0.019(2) 0.017(2) 0.019(2) 0.0005(17) -0.0018(17) -0.0068(18) C7 0.008(2) 0.029(2) 0.020(2) 0.0017(18) -0.0026(16) -0.0071(17) C8 0.015(2) 0.026(2) 0.019(2) 0.0037(18) -0.0080(18) -0.0092(18) C9 0.019(3) 0.039(3) 0.024(2) 0.008(2) -0.0053(19) -0.021(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 Gd1 O3 2.287(3) . ? Gd1 O7 2.375(3) 2_665 ? Gd1 O10 2.405(3) . ? Gd1 O1 2.431(3) 2_665 ? Gd1 O6 2.456(3) 1_545 ? Gd1 O9 2.465(3) . ? Gd1 O5 2.514(3) 2_765 ? Gd1 N1 2.526(3) 2_665 ? Gd1 O6 2.671(3) 2_765 ? Gd1 C8 2.958(4) 2_765 ? Co1 O11 2.069(3) . ? Co1 O11 2.069(3) 2_566 ? Co1 O13 2.116(4) . ? Co1 O13 2.116(4) 2_566 ? Co1 O12 2.120(3) . ? Co1 O12 2.120(3) 2_566 ? O1 C6 1.268(5) . ? O1 Gd1 2.431(3) 2_665 ? O2 C6 1.231(5) . ? O3 C7 1.252(5) . ? O4 C7 1.239(5) . ? O5 C8 1.255(5) . ? O5 Gd1 2.514(3) 2_765 ? O6 C8 1.255(5) . ? O6 Gd1 2.456(3) 1_565 ? O6 Gd1 2.671(3) 2_765 ? O7 C9 1.275(6) . ? O7 Gd1 2.375(3) 2_665 ? O8 C9 1.213(6) . ? OW2 OW2 1.563(16) 2_556 ? N1 C1 1.331(5) . ? N1 C5 1.338(5) . ? N1 Gd1 2.526(3) 2_665 ? C1 C2 1.398(6) . ? C1 C6 1.507(6) . ? C2 C3 1.399(6) . ? C2 C7 1.504(6) . ? C3 C4 1.379(6) . ? C4 C5 1.398(6) . ? C4 C8 1.504(6) . ? C5 C9 1.502(6) . ? C8 Gd1 2.958(4) 2_765 ? 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 O3 Gd1 O7 93.04(12) . 2_665 ? O3 Gd1 O10 142.81(12) . . ? O7 Gd1 O10 76.78(12) 2_665 . ? O3 Gd1 O1 75.21(11) . 2_665 ? O7 Gd1 O1 127.44(10) 2_665 2_665 ? O10 Gd1 O1 138.81(11) . 2_665 ? O3 Gd1 O6 145.22(11) . 1_545 ? O7 Gd1 O6 93.18(10) 2_665 1_545 ? O10 Gd1 O6 71.77(11) . 1_545 ? O1 Gd1 O6 73.89(10) 2_665 1_545 ? O3 Gd1 O9 73.23(12) . . ? O7 Gd1 O9 73.67(11) 2_665 . ? O10 Gd1 O9 69.58(12) . . ? O1 Gd1 O9 142.81(11) 2_665 . ? O6 Gd1 O9 141.06(11) 1_545 . ? O3 Gd1 O5 75.85(12) . 2_765 ? O7 Gd1 O5 150.17(11) 2_665 2_765 ? O10 Gd1 O5 95.30(13) . 2_765 ? O1 Gd1 O5 77.04(10) 2_665 2_765 ? O6 Gd1 O5 111.84(10) 1_545 2_765 ? O9 Gd1 O5 76.61(11) . 2_765 ? O3 Gd1 N1 72.24(12) . 2_665 ? O7 Gd1 N1 64.05(10) 2_665 2_665 ? O10 Gd1 N1 129.75(12) . 2_665 ? O1 Gd1 N1 63.57(10) 2_665 2_665 ? O6 Gd1 N1 79.95(10) 1_545 2_665 ? O9 Gd1 N1 122.62(11) . 2_665 ? O5 Gd1 N1 134.10(11) 2_765 2_665 ? O3 Gd1 O6 120.26(11) . 2_765 ? O7 Gd1 O6 146.40(10) 2_665 2_765 ? O10 Gd1 O6 73.64(11) . 2_765 ? O1 Gd1 O6 70.76(9) 2_665 2_765 ? O6 Gd1 O6 62.66(10) 1_545 2_765 ? O9 Gd1 O6 109.64(10) . 2_765 ? O5 Gd1 O6 49.77(9) 2_765 2_765 ? N1 Gd1 O6 127.18(10) 2_665 2_765 ? O3 Gd1 C8 97.12(12) . 2_765 ? O7 Gd1 C8 161.85(11) 2_665 2_765 ? O10 Gd1 C8 86.09(12) . 2_765 ? O1 Gd1 C8 70.00(10) 2_665 2_765 ? O6 Gd1 C8 87.03(11) 1_545 2_765 ? O9 Gd1 C8 94.89(11) . 2_765 ? O5 Gd1 C8 24.86(11) 2_765 2_765 ? N1 Gd1 C8 133.56(11) 2_665 2_765 ? O6 Gd1 C8 25.10(10) 2_765 2_765 ? O11 Co1 O11 180.0(2) . 2_566 ? O11 Co1 O13 93.06(14) . . ? O11 Co1 O13 86.94(14) 2_566 . ? O11 Co1 O13 86.94(14) . 2_566 ? O11 Co1 O13 93.06(14) 2_566 2_566 ? O13 Co1 O13 180.0 . 2_566 ? O11 Co1 O12 94.91(13) . . ? O11 Co1 O12 85.09(13) 2_566 . ? O13 Co1 O12 92.73(14) . . ? O13 Co1 O12 87.27(14) 2_566 . ? O11 Co1 O12 85.09(13) . 2_566 ? O11 Co1 O12 94.91(13) 2_566 2_566 ? O13 Co1 O12 87.27(14) . 2_566 ? O13 Co1 O12 92.73(14) 2_566 2_566 ? O12 Co1 O12 180.0 . 2_566 ? C6 O1 Gd1 125.0(3) . 2_665 ? C7 O3 Gd1 159.9(3) . . ? C8 O5 Gd1 97.8(2) . 2_765 ? C8 O6 Gd1 148.8(3) . 1_565 ? C8 O6 Gd1 90.4(3) . 2_765 ? Gd1 O6 Gd1 117.34(10) 1_565 2_765 ? C9 O7 Gd1 127.0(3) . 2_665 ? C1 N1 C5 120.3(4) . . ? C1 N1 Gd1 120.2(3) . 2_665 ? C5 N1 Gd1 118.9(3) . 2_665 ? N1 C1 C2 122.8(4) . . ? N1 C1 C6 114.0(4) . . ? C2 C1 C6 123.2(4) . . ? C1 C2 C3 116.5(4) . . ? C1 C2 C7 123.4(4) . . ? C3 C2 C7 120.0(4) . . ? C4 C3 C2 120.8(4) . . ? C3 C4 C5 118.5(4) . . ? C3 C4 C8 119.7(4) . . ? C5 C4 C8 121.7(4) . . ? N1 C5 C4 121.0(4) . . ? N1 C5 C9 114.8(4) . . ? C4 C5 C9 124.2(4) . . ? O2 C6 O1 125.2(4) . . ? O2 C6 C1 118.4(4) . . ? O1 C6 C1 116.4(4) . . ? O4 C7 O3 125.6(4) . . ? O4 C7 C2 117.9(4) . . ? O3 C7 C2 116.4(4) . . ? O6 C8 O5 121.2(4) . . ? O6 C8 C4 118.1(4) . . ? O5 C8 C4 120.4(4) . . ? O6 C8 Gd1 64.5(2) . 2_765 ? O5 C8 Gd1 57.4(2) . 2_765 ? C4 C8 Gd1 165.9(3) . 2_765 ? O8 C9 O7 126.1(4) . . ? O8 C9 C5 118.9(4) . . ? O7 C9 C5 115.0(4) . . ? loop_ _geom_hbond_atom_site_label_D _geom_hbond_atom_site_label_H _geom_hbond_atom_site_label_A _geom_hbond_distance_DH _geom_hbond_distance_HA _geom_hbond_distance_DA _geom_hbond_angle_DHA _geom_hbond_site_symmetry_A O9 H9A OW2 0.81 1.98 2.739(8) 155.0 2_656 O9 H9A OW2 0.81 2.07 2.822(9) 153.1 1_655 O9 H9B OW1 0.82 1.97 2.779(5) 172.5 . O10 H10A O1 0.82 1.88 2.679(4) 165.0 1_645 O10 H10B O13 0.82 2.17 2.988(5) 170.1 2_656 O11 H11A O5 0.82 1.96 2.765(4) 171.4 2_665 O11 H11B O2 0.82 1.84 2.639(5) 167.3 . O12 H12A O2 0.82 2.03 2.788(5) 154.0 . O12 H12B O4 0.82 1.95 2.758(5) 168.5 2_666 O13 H13A OW1 0.82 1.89 2.707(5) 170.6 . O13 H13B OW2 0.82 1.98 2.663(9) 141.0 . O13 H13B O8 0.82 2.64 3.326(7) 142.0 2_665 OW1 H10C O7 0.82 2.05 2.818(4) 157.2 1_546 OW1 H10D O4 0.82 1.86 2.658(5) 164.0 2_666 _diffrn_measured_fraction_theta_max 0.973 _diffrn_reflns_theta_full 25.06 _diffrn_measured_fraction_theta_full 0.973 _refine_diff_density_max 1.612 _refine_diff_density_min -0.940 _refine_diff_density_rms 0.138 # Attachment '- New5.cif' data_New5 _database_code_depnum_ccdc_archive 'CCDC 827210' #TrackingRef '- New5.cif' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C18 H28 Gd2 Mn N2 O29' _chemical_formula_weight 1105.86 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' Mn Mn 0.3368 0.7283 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Gd Gd -0.1653 3.9035 '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 8.71960(10) _cell_length_b 9.2220(2) _cell_length_c 10.5926(2) _cell_angle_alpha 86.0030(10) _cell_angle_beta 77.1680(10) _cell_angle_gamma 71.0900(10) _cell_volume 785.68(2) _cell_formula_units_Z 1 _cell_measurement_temperature 296(2) _cell_measurement_reflns_used 10334 _cell_measurement_theta_min 1.97 _cell_measurement_theta_max 25.05 _exptl_crystal_description Bloc _exptl_crystal_colour Pink _exptl_crystal_size_max 0.18 _exptl_crystal_size_mid 0.065 _exptl_crystal_size_min 0.015 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 2.337 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 535 _exptl_absorpt_coefficient_mu 4.687 _exptl_absorpt_correction_type empirical _exptl_absorpt_correction_T_min 0.701 _exptl_absorpt_correction_T_max 0.932 _exptl_absorpt_process_details ? _exptl_special_details ; ? ; _diffrn_ambient_temperature 296(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type ? _diffrn_measurement_method ? _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 10334 _diffrn_reflns_av_R_equivalents 0.0263 _diffrn_reflns_av_sigmaI/netI 0.0247 _diffrn_reflns_limit_h_min -10 _diffrn_reflns_limit_h_max 10 _diffrn_reflns_limit_k_min -10 _diffrn_reflns_limit_k_max 10 _diffrn_reflns_limit_l_min -12 _diffrn_reflns_limit_l_max 12 _diffrn_reflns_theta_min 1.97 _diffrn_reflns_theta_max 25.05 _reflns_number_total 2787 _reflns_number_gt 2595 _reflns_threshold_expression >2sigma(I) _computing_data_collection ? _computing_cell_refinement ? _computing_data_reduction ? _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics ? _computing_publication_material ? _refine_special_details ; Refinement of F^2^ against ALL reflections. The weighted R-factor wR and goodness of fit S are based on F^2^, conventional R-factors R are based on F, with F set to zero for negative F^2^. The threshold expression of F^2^ > 2sigma(F^2^) is used only for calculating R-factors(gt) etc. and is not relevant to the choice of reflections for refinement. R-factors based on F^2^ are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger. ; _refine_ls_structure_factor_coef Fsqd _refine_ls_matrix_type full _refine_ls_weighting_scheme calc _refine_ls_weighting_details 'calc w=1/[\s^2^(Fo^2^)+(0.0263P)^2^+0.1939P] 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 2787 _refine_ls_number_parameters 241 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0208 _refine_ls_R_factor_gt 0.0184 _refine_ls_wR_factor_ref 0.0449 _refine_ls_wR_factor_gt 0.0440 _refine_ls_goodness_of_fit_ref 1.048 _refine_ls_restrained_S_all 1.048 _refine_ls_shift/su_max 0.000 _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 Gd1 Gd 0.785628(17) 0.131410(16) 0.144622(14) 0.01459(6) Uani 1 1 d . . . Mn1 Mn 0.0000 0.5000 0.5000 0.02453(17) Uani 1 2 d S . . O1 O 0.1817(2) 0.7234(2) 0.0543(2) 0.0195(5) Uani 1 1 d . . . O2 O 0.2827(3) 0.5772(3) 0.2111(2) 0.0335(6) Uani 1 1 d . . . O3 O 0.6354(3) 0.3808(2) 0.2038(2) 0.0296(6) Uani 1 1 d . . . O4 O 0.5772(3) 0.5672(3) 0.3439(2) 0.0332(6) Uani 1 1 d . . . O5 O 0.9995(3) 0.7518(3) -0.1684(2) 0.0268(5) Uani 1 1 d . . . O6 O 0.8901(3) 0.9440(2) -0.0317(2) 0.0206(5) Uani 1 1 d . . . O7 O 0.4397(3) 0.9602(3) -0.2386(2) 0.0244(5) Uani 1 1 d . . . O8 O 0.6928(4) 0.9734(4) -0.2536(3) 0.0654(11) Uani 1 1 d . . . O9 O 0.7511(3) 0.1469(3) 0.3815(2) 0.0305(6) Uani 1 1 d . . . H9A H 0.8218 0.1138 0.4256 0.037 Uiso 1 1 d . . . H9B H 0.6571 0.1571 0.4272 0.037 Uiso 1 1 d . . . O10 O 0.9195(3) -0.1138(3) 0.2300(2) 0.0345(6) Uani 1 1 d . . . H10A H 0.9926 -0.1780 0.1801 0.041 Uiso 1 1 d . . . H10B H 0.9046 -0.1659 0.2981 0.041 Uiso 1 1 d . . . O11 O 0.0159(3) 0.4925(3) 0.2939(2) 0.0323(6) Uani 1 1 d . . . H11A H 0.0206 0.4164 0.2648 0.039 Uiso 1 1 d . . . H11B H 0.0999 0.5134 0.2633 0.039 Uiso 1 1 d . . . O12 O 0.2245(3) 0.5648(3) 0.4830(2) 0.0380(7) Uani 1 1 d . . . H12A H 0.2610 0.5761 0.4081 0.046 Uiso 1 1 d . . . H12B H 0.2857 0.5303 0.5266 0.046 Uiso 1 1 d . . . O13 O 0.1423(3) 0.2520(3) 0.5092(3) 0.0431(7) Uani 1 1 d . . . H13A H 0.2335 0.2344 0.5121 0.052 Uiso 1 1 d . . . H13B H 0.1283 0.2064 0.4547 0.052 Uiso 1 1 d . . . OW1 O 0.4538(3) 0.1655(3) 0.5528(2) 0.0326(6) Uani 1 1 d . . . H10C H 0.4522 0.0911 0.5954 0.039 Uiso 1 1 d . . . H10D H 0.4431 0.2401 0.5952 0.039 Uiso 1 1 d . . . OW2 O 0.0696(7) 0.0116(7) 0.4414(5) 0.0479(15) Uani 0.50 1 d P . . N1 N 0.4564(3) 0.7881(3) -0.0330(2) 0.0158(5) Uani 1 1 d . . . C1 C 0.4578(4) 0.6921(3) 0.0667(3) 0.0154(6) Uani 1 1 d . . . C2 C 0.5955(4) 0.6306(3) 0.1225(3) 0.0161(6) Uani 1 1 d . . . C3 C 0.7344(4) 0.6762(3) 0.0713(3) 0.0182(7) Uani 1 1 d . . . H3A H 0.8280 0.6396 0.1071 0.022 Uiso 1 1 calc R . . C4 C 0.7330(4) 0.7762(3) -0.0328(3) 0.0170(7) Uani 1 1 d . . . C5 C 0.5919(4) 0.8280(3) -0.0850(3) 0.0164(6) Uani 1 1 d . . . C6 C 0.2950(4) 0.6601(3) 0.1151(3) 0.0186(7) Uani 1 1 d . . . C7 C 0.6017(4) 0.5175(3) 0.2329(3) 0.0183(7) Uani 1 1 d . . . C8 C 0.8820(4) 0.8285(3) -0.0839(3) 0.0176(7) Uani 1 1 d . . . C9 C 0.5758(4) 0.9297(4) -0.2016(3) 0.0242(7) 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 Gd1 0.01230(9) 0.01628(9) 0.01620(10) 0.00272(6) -0.00385(6) -0.00591(6) Mn1 0.0231(4) 0.0291(4) 0.0226(4) 0.0013(3) -0.0038(3) -0.0109(3) O1 0.0127(11) 0.0258(12) 0.0198(12) 0.0060(9) -0.0031(10) -0.0072(9) O2 0.0240(13) 0.0505(16) 0.0311(15) 0.0251(12) -0.0109(11) -0.0207(12) O3 0.0311(14) 0.0167(12) 0.0343(15) 0.0021(10) -0.0028(12) -0.0017(10) O4 0.0516(17) 0.0325(14) 0.0193(14) 0.0028(10) -0.0110(12) -0.0169(13) O5 0.0199(13) 0.0341(13) 0.0288(14) -0.0107(11) 0.0020(11) -0.0144(11) O6 0.0212(12) 0.0220(12) 0.0222(13) -0.0005(9) -0.0056(10) -0.0110(10) O7 0.0188(12) 0.0336(13) 0.0239(13) 0.0128(10) -0.0090(10) -0.0125(10) O8 0.0420(18) 0.112(3) 0.066(2) 0.065(2) -0.0323(16) -0.0562(19) O9 0.0265(13) 0.0389(14) 0.0246(14) 0.0023(11) -0.0068(11) -0.0081(11) O10 0.0341(15) 0.0269(13) 0.0253(14) 0.0091(10) 0.0044(12) 0.0045(11) O11 0.0350(15) 0.0420(15) 0.0268(14) -0.0037(11) 0.0012(11) -0.0257(12) O12 0.0281(14) 0.0625(18) 0.0273(15) 0.0144(13) -0.0065(12) -0.0221(14) O13 0.0376(16) 0.0396(16) 0.0555(19) -0.0016(13) -0.0172(14) -0.0118(13) OW1 0.0410(16) 0.0275(13) 0.0300(15) 0.0023(11) -0.0104(12) -0.0103(12) OW2 0.046(4) 0.062(4) 0.044(4) 0.004(3) -0.017(3) -0.023(3) N1 0.0131(13) 0.0184(13) 0.0161(14) 0.0024(10) -0.0019(11) -0.0065(11) C1 0.0142(16) 0.0176(15) 0.0137(16) 0.0000(12) -0.0011(13) -0.0053(13) C2 0.0162(16) 0.0165(15) 0.0155(16) -0.0011(12) -0.0036(13) -0.0046(13) C3 0.0147(16) 0.0228(16) 0.0181(17) 0.0018(13) -0.0066(13) -0.0056(13) C4 0.0157(16) 0.0202(16) 0.0168(17) -0.0022(12) -0.0019(13) -0.0085(13) C5 0.0135(16) 0.0202(16) 0.0171(17) 0.0019(12) -0.0022(13) -0.0084(13) C6 0.0159(17) 0.0219(16) 0.0184(17) 0.0020(13) -0.0023(14) -0.0079(14) C7 0.0120(16) 0.0230(17) 0.0207(18) 0.0034(13) -0.0068(13) -0.0049(13) C8 0.0162(17) 0.0236(17) 0.0184(17) 0.0060(13) -0.0094(14) -0.0112(14) C9 0.0217(18) 0.0316(19) 0.0238(19) 0.0076(15) -0.0062(15) -0.0154(15) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag Gd1 O3 2.298(2) . ? Gd1 O7 2.378(2) 2_665 ? Gd1 O10 2.402(2) . ? Gd1 O1 2.429(2) 2_665 ? Gd1 O6 2.445(2) 1_545 ? Gd1 O9 2.469(2) . ? Gd1 O5 2.508(2) 2_765 ? Gd1 N1 2.525(2) 2_665 ? Gd1 O6 2.692(2) 2_765 ? Gd1 C8 2.964(3) 2_765 ? Mn1 O11 2.161(2) . ? Mn1 O11 2.161(2) 2_566 ? Mn1 O12 2.193(2) 2_566 ? Mn1 O12 2.193(2) . ? Mn1 O13 2.228(3) 2_566 ? Mn1 O13 2.228(3) . ? O1 C6 1.260(4) . ? O1 Gd1 2.429(2) 2_665 ? O2 C6 1.235(4) . ? O3 C7 1.243(4) . ? O4 C7 1.240(4) . ? O5 C8 1.250(4) . ? O5 Gd1 2.508(2) 2_765 ? O6 C8 1.263(4) . ? O6 Gd1 2.445(2) 1_565 ? O6 Gd1 2.692(2) 2_765 ? O7 C9 1.271(4) . ? O7 Gd1 2.378(2) 2_665 ? O8 C9 1.222(4) . ? OW2 OW2 1.588(11) 2_556 ? N1 C1 1.330(4) . ? N1 C5 1.341(4) . ? N1 Gd1 2.525(2) 2_665 ? C1 C2 1.392(4) . ? C1 C6 1.514(4) . ? C2 C3 1.394(4) . ? C2 C7 1.510(4) . ? C3 C4 1.387(4) . ? C4 C5 1.390(4) . ? C4 C8 1.507(4) . ? C5 C9 1.501(4) . ? C8 Gd1 2.964(3) 2_765 ? 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 O3 Gd1 O7 93.07(8) . 2_665 ? O3 Gd1 O10 142.64(9) . . ? O7 Gd1 O10 76.94(8) 2_665 . ? O3 Gd1 O1 75.45(8) . 2_665 ? O7 Gd1 O1 127.53(7) 2_665 2_665 ? O10 Gd1 O1 138.60(7) . 2_665 ? O3 Gd1 O6 145.50(8) . 1_545 ? O7 Gd1 O6 93.27(7) 2_665 1_545 ? O10 Gd1 O6 71.69(8) . 1_545 ? O1 Gd1 O6 73.86(7) 2_665 1_545 ? O3 Gd1 O9 73.12(8) . . ? O7 Gd1 O9 73.57(8) 2_665 . ? O10 Gd1 O9 69.52(8) . . ? O1 Gd1 O9 142.96(8) 2_665 . ? O6 Gd1 O9 140.91(7) 1_545 . ? O3 Gd1 O5 75.98(8) . 2_765 ? O7 Gd1 O5 150.19(8) 2_665 2_765 ? O10 Gd1 O5 94.91(9) . 2_765 ? O1 Gd1 O5 77.09(7) 2_665 2_765 ? O6 Gd1 O5 111.57(7) 1_545 2_765 ? O9 Gd1 O5 76.72(8) . 2_765 ? O3 Gd1 N1 72.60(8) . 2_665 ? O7 Gd1 N1 64.14(7) 2_665 2_665 ? O10 Gd1 N1 129.82(8) . 2_665 ? O1 Gd1 N1 63.56(7) 2_665 2_665 ? O6 Gd1 N1 79.87(7) 1_545 2_665 ? O9 Gd1 N1 122.79(8) . 2_665 ? O5 Gd1 N1 134.33(8) 2_765 2_665 ? O3 Gd1 O6 120.39(7) . 2_765 ? O7 Gd1 O6 146.21(7) 2_665 2_765 ? O10 Gd1 O6 73.29(7) . 2_765 ? O1 Gd1 O6 70.81(7) 2_665 2_765 ? O6 Gd1 O6 62.46(7) 1_545 2_765 ? O9 Gd1 O6 109.62(7) . 2_765 ? O5 Gd1 O6 49.68(7) 2_765 2_765 ? N1 Gd1 O6 127.09(7) 2_665 2_765 ? O3 Gd1 C8 97.10(8) . 2_765 ? O7 Gd1 C8 161.69(8) 2_665 2_765 ? O10 Gd1 C8 85.79(8) . 2_765 ? O1 Gd1 C8 70.06(7) 2_665 2_765 ? O6 Gd1 C8 86.96(8) 1_545 2_765 ? O9 Gd1 C8 94.84(8) . 2_765 ? O5 Gd1 C8 24.66(8) 2_765 2_765 ? N1 Gd1 C8 133.62(8) 2_665 2_765 ? O6 Gd1 C8 25.22(7) 2_765 2_765 ? O11 Mn1 O11 179.999(6) . 2_566 ? O11 Mn1 O12 84.68(9) . 2_566 ? O11 Mn1 O12 95.32(9) 2_566 2_566 ? O11 Mn1 O12 95.32(9) . . ? O11 Mn1 O12 84.68(9) 2_566 . ? O12 Mn1 O12 180.0 2_566 . ? O11 Mn1 O13 86.85(10) . 2_566 ? O11 Mn1 O13 93.15(10) 2_566 2_566 ? O12 Mn1 O13 91.64(10) 2_566 2_566 ? O12 Mn1 O13 88.36(10) . 2_566 ? O11 Mn1 O13 93.15(10) . . ? O11 Mn1 O13 86.85(10) 2_566 . ? O12 Mn1 O13 88.36(10) 2_566 . ? O12 Mn1 O13 91.64(10) . . ? O13 Mn1 O13 180.0 2_566 . ? C6 O1 Gd1 125.06(18) . 2_665 ? C7 O3 Gd1 160.8(2) . . ? C8 O5 Gd1 98.53(17) . 2_765 ? C8 O6 Gd1 149.4(2) . 1_565 ? C8 O6 Gd1 89.49(18) . 2_765 ? Gd1 O6 Gd1 117.53(7) 1_565 2_765 ? C9 O7 Gd1 126.53(19) . 2_665 ? C1 N1 C5 120.1(3) . . ? C1 N1 Gd1 120.30(18) . 2_665 ? C5 N1 Gd1 119.11(19) . 2_665 ? N1 C1 C2 122.6(3) . . ? N1 C1 C6 113.6(3) . . ? C2 C1 C6 123.7(3) . . ? C1 C2 C3 117.3(3) . . ? C1 C2 C7 123.5(3) . . ? C3 C2 C7 119.2(3) . . ? C4 C3 C2 120.1(3) . . ? C3 C4 C5 118.7(3) . . ? C3 C4 C8 119.3(3) . . ? C5 C4 C8 121.9(3) . . ? N1 C5 C4 121.1(3) . . ? N1 C5 C9 114.2(3) . . ? C4 C5 C9 124.6(3) . . ? O2 C6 O1 125.4(3) . . ? O2 C6 C1 118.1(3) . . ? O1 C6 C1 116.5(3) . . ? O4 C7 O3 125.4(3) . . ? O4 C7 C2 117.9(3) . . ? O3 C7 C2 116.6(3) . . ? O5 C8 O6 121.4(3) . . ? O5 C8 C4 120.3(3) . . ? O6 C8 C4 118.1(3) . . ? O5 C8 Gd1 56.82(14) . 2_765 ? O6 C8 Gd1 65.30(15) . 2_765 ? C4 C8 Gd1 165.8(2) . 2_765 ? O8 C9 O7 125.8(3) . . ? O8 C9 C5 118.4(3) . . ? O7 C9 C5 115.8(3) . . ? loop_ _geom_hbond_atom_site_label_D _geom_hbond_atom_site_label_H _geom_hbond_atom_site_label_A _geom_hbond_distance_DH _geom_hbond_distance_HA _geom_hbond_distance_DA _geom_hbond_angle_DHA _geom_hbond_site_symmetry_A O9 H9A OW2 0.82 1.97 2.746(6) 157.3 2_656 O9 H9A OW2 0.82 2.10 2.845(6) 150.9 1_655 O9 H9B OW1 0.83 1.95 2.776(3) 171.9 . O10 H10A O1 0.83 1.88 2.687(3) 163.7 1_645 O10 H10B O13 0.85 2.14 2.973(4) 167.6 2_656 O11 H11A O5 0.77 1.99 2.748(3) 168.1 2_665 O11 H11B O2 0.81 1.83 2.640(3) 172.8 . O12 H12A O2 0.80 2.05 2.813(3) 158.6 . O12 H12B O4 0.76 1.99 2.750(4) 172.8 2_666 O13 H13A OW1 0.77 1.95 2.707(4) 167.8 . O13 H13B OW2 0.79 2.04 2.677(6) 137.4 . O13 H13B O8 0.79 2.66 3.292(5) 138.7 2_665 OW1 H10C O7 0.80 2.06 2.816(3) 157.0 1_546 OW1 H10D O4 0.82 1.87 2.676(3) 167.1 2_666 _diffrn_measured_fraction_theta_max 0.999 _diffrn_reflns_theta_full 25.05 _diffrn_measured_fraction_theta_full 0.999 _refine_diff_density_max 0.655 _refine_diff_density_min -0.719 _refine_diff_density_rms 0.091