# Electronic Supplementary Material (ESI) for Dalton Transactions # This journal is © The Royal Society of Chemistry 2013 ####################################################################### # # Cambridge Crystallographic Data Centre # CCDC # ####################################################################### # # This CIF contains data from an original supplementary publication # deposited with the CCDC, and may include chemical, crystal, # experimental, refinement, atomic coordinates, # anisotropic displacement parameters and molecular geometry data, # as required by the journal to which it was submitted. # # This CIF is provided on the understanding that it is used for bona # fide research purposes only. It may contain copyright material # of the CCDC or of third parties, and may not be copied or further # disseminated in any form, whether machine-readable or not, # except for the purpose of generating routine backup copies # on your local computer system. # # For further information on the CCDC, data deposition and # data retrieval see: # www.ccdc.cam.ac.uk # # Bona fide researchers may freely download Mercury and enCIFer # from this site to visualise CIF-encoded structures and # to carry out CIF format checking respectively. # data_a _audit_creation_date 2013-07-22 _audit_creation_method ; Olex2 1.1 (compiled 2011.11.01 svn.r2039, GUI svn.r3906) ; _chemical_name_common ? _chemical_name_systematic ; ? ; _chemical_formula_moiety 'C10 H21 Gd K3 N2 O15 P, 3(H2 O)' _chemical_formula_sum 'C10 H27 Gd K3 N2 O18 P' _chemical_formula_weight 768.86 _chemical_absolute_configuration ad _chemical_melting_point ? 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' K K 0.2009 0.2494 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' P P 0.1023 0.0942 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Gd Gd -0.1653 3.9035 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _space_group_crystal_system monoclinic _space_group_IT_number 4 _space_group_name_H-M_alt 'P 1 21 1' _space_group_name_Hall 'P 2yb' loop_ _space_group_symop_id _space_group_symop_operation_xyz 1 'x, y, z' 2 '-x, y+1/2, -z' _cell_length_a 10.4965(9) _cell_length_b 8.8178(5) _cell_length_c 14.8505(15) _cell_angle_alpha 90.00 _cell_angle_beta 110.161(10) _cell_angle_gamma 90.00 _cell_volume 1290.28(19) _cell_formula_units_Z 2 _cell_measurement_reflns_used ? _cell_measurement_temperature 446(2) _cell_measurement_theta_max ? _cell_measurement_theta_min ? _exptl_absorpt_coefficient_mu 3.196 _exptl_absorpt_correction_T_max 0.8566 _exptl_absorpt_correction_T_min 0.7406 _exptl_absorpt_correction_type MULTI-SCAN _exptl_absorpt_process_details ? _exptl_crystal_colour ? _exptl_crystal_density_diffrn 1.979 _exptl_crystal_density_meas ? _exptl_crystal_density_method 'not measured' _exptl_crystal_description ? _exptl_crystal_F_000 762 _exptl_crystal_size_max 0.10 _exptl_crystal_size_mid 0.08 _exptl_crystal_size_min 0.05 _exptl_special_details ; ? ; _diffrn_reflns_av_R_equivalents 0.0475 _diffrn_reflns_av_unetI/netI 0.0882 _diffrn_reflns_limit_h_max 13 _diffrn_reflns_limit_h_min -13 _diffrn_reflns_limit_k_max 10 _diffrn_reflns_limit_k_min -11 _diffrn_reflns_limit_l_max 18 _diffrn_reflns_limit_l_min -19 _diffrn_reflns_number 6996 _diffrn_reflns_theta_full 27.49 _diffrn_reflns_theta_max 27.49 _diffrn_reflns_theta_min 2.91 _diffrn_ambient_temperature 446.15 _diffrn_detector_area_resol_mean ? _diffrn_measured_fraction_theta_full 0.969 _diffrn_measured_fraction_theta_max 0.969 _diffrn_measurement_device_type ? _diffrn_measurement_method ? _diffrn_radiation_monochromator graphite _diffrn_radiation_type MoK\a _diffrn_radiation_wavelength 0.71073 _diffrn_source 'fine-focus sealed tube' _diffrn_standards_decay_% ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_number ? _reflns_number_gt 4322 _reflns_number_total 4785 _reflns_threshold_expression >2sigma(I) _computing_cell_refinement ? _computing_data_collection ? _computing_data_reduction ? _computing_molecular_graphics ; O. V. Dolomanov, L. J. Bourhis, R. J. Gildea, J. A. K. Howard and H. Puschmann, OLEX2: a complete structure solution, refinement and analysis program. J. Appl. Cryst. (2009). 42, 339-341. ; _computing_publication_material ; O. V. Dolomanov, L. J. Bourhis, R. J. Gildea, J. A. K. Howard and H. Puschmann, OLEX2: a complete structure solution, refinement and analysis program. J. Appl. Cryst. (2009). 42, 339-341. ; _computing_structure_refinement ; XL, G.M. Sheldrick, Acta Cryst. (2008). A64, 112-122 ; _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _refine_diff_density_max 1.005 _refine_diff_density_min -0.897 _refine_diff_density_rms 0.157 _refine_ls_abs_structure_details 'Flack H D (1983), Acta Cryst. A39, 876-881' _refine_ls_abs_structure_Flack -0.014(13) _refine_ls_extinction_coef ? _refine_ls_extinction_method none _refine_ls_goodness_of_fit_ref 0.949 _refine_ls_hydrogen_treatment mixed _refine_ls_matrix_type full _refine_ls_number_parameters 361 _refine_ls_number_reflns 4785 _refine_ls_number_restraints 22 _refine_ls_R_factor_all 0.0490 _refine_ls_R_factor_gt 0.0418 _refine_ls_restrained_S_all 0.947 _refine_ls_shift/su_max 0.001 _refine_ls_shift/su_mean 0.000 _refine_ls_structure_factor_coef Fsqd _refine_ls_weighting_details 'calc w=1/[\s^2^(Fo^2^)+(0.0204P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3' _refine_ls_weighting_scheme calc _refine_ls_wR_factor_gt 0.0768 _refine_ls_wR_factor_ref 0.0813 _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. ; _atom_sites_solution_hydrogens geom _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap 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 0.52721(3) -0.34136(5) 0.33451(2) 0.01251(9) Uani 1 1 d . . . P1 P 0.5842(2) -0.6819(2) 0.48378(15) 0.0183(5) Uani 1 1 d . . . K1 K 0.7601(2) -1.06839(19) 0.55520(13) 0.0252(4) Uani 1 1 d . . . K2 K 1.1115(2) -0.1947(2) 0.28743(13) 0.0269(4) Uani 1 1 d . . . K3 K 1.1030(2) 0.0296(2) 0.50917(14) 0.0263(4) Uani 1 1 d . . . N1 N 0.5719(7) -0.1722(6) 0.2053(4) 0.0142(14) Uani 1 1 d . . . N2 N 0.4470(7) -0.4708(6) 0.1641(4) 0.0150(14) Uani 1 1 d . . . O1 O 0.3495(6) -0.1637(6) 0.2532(4) 0.0187(13) Uani 1 1 d . . . O2 O 0.3067(6) 0.0816(6) 0.2142(4) 0.0280(14) Uani 1 1 d . . . O3 O 0.7391(6) -0.2101(6) 0.3891(4) 0.0189(12) Uani 1 1 d . . . O4 O 0.9197(6) -0.1235(7) 0.3602(5) 0.0336(16) Uani 1 1 d . . . O5 O 0.3231(6) -0.4840(6) 0.2952(4) 0.0197(13) Uani 1 1 d . . . O6 O 0.1188(6) -0.5296(8) 0.1883(4) 0.0383(17) Uani 1 1 d . . . O7 O 0.6928(6) -0.5026(6) 0.2982(4) 0.0243(13) Uani 1 1 d . . . O8 O 0.7323(6) -0.7232(6) 0.2406(4) 0.0264(14) Uani 1 1 d . . . O9 O 0.5960(6) -0.5154(6) 0.4581(4) 0.0271(14) Uani 1 1 d . . . O10 O 0.4890(6) -0.6968(6) 0.5405(4) 0.0238(13) Uani 1 1 d . . . O11 O 0.7198(6) -0.7549(6) 0.5300(4) 0.0285(14) Uani 1 1 d . . . C1 C 0.5200(9) -0.0224(9) 0.2194(7) 0.020(2) Uani 1 1 d . . . H1A H 0.5147 0.0426 0.1655 0.024 Uiso 1 1 calc R . . H1B H 0.5824 0.0238 0.2771 0.024 Uiso 1 1 calc R . . C2 C 0.3797(9) -0.0353(9) 0.2283(5) 0.0184(18) Uani 1 1 d . . . C3 C 0.7204(8) -0.1633(9) 0.2269(6) 0.0182(18) Uani 1 1 d . . . H3A H 0.7412 -0.0711 0.1991 0.022 Uiso 1 1 calc R . . H3B H 0.7487 -0.2485 0.1970 0.022 Uiso 1 1 calc R . . C4 C 0.7995(10) -0.1646(8) 0.3324(6) 0.0214(19) Uani 1 1 d . . . C5 C 0.2968(8) -0.4769(9) 0.1284(5) 0.0186(17) Uani 1 1 d . . . H5A H 0.2664 -0.5590 0.0824 0.022 Uiso 1 1 calc R . . H5B H 0.2608 -0.3828 0.0957 0.022 Uiso 1 1 calc R . . C6 C 0.2416(9) -0.5015(9) 0.2102(6) 0.0210(18) Uani 1 1 d . . . C7 C 0.5056(9) -0.6239(9) 0.1815(6) 0.018(2) Uani 1 1 d . . . H7A H 0.4967 -0.6716 0.1208 0.021 Uiso 1 1 calc R . . H7B H 0.4565 -0.6850 0.2130 0.021 Uiso 1 1 calc R . . C8 C 0.6550(9) -0.6170(9) 0.2442(5) 0.0170(17) Uani 1 1 d . . . C9 C 0.4967(9) -0.2213(9) 0.1063(6) 0.019(2) Uani 1 1 d . . . H9A H 0.5354 -0.1727 0.0630 0.023 Uiso 1 1 calc R . . H9B H 0.4029 -0.1889 0.0886 0.023 Uiso 1 1 calc R . . C10 C 0.5011(9) -0.3928(8) 0.0949(6) 0.018(2) Uani 1 1 d . . . H10A H 0.4470 -0.4210 0.0298 0.021 Uiso 1 1 calc R . . H10B H 0.5938 -0.4248 0.1067 0.021 Uiso 1 1 calc R . . O1W O 0.7788(7) -1.3745(8) 0.6255(4) 0.0394(19) Uani 1 1 d D . . O2W O 1.0135(8) -0.9863(10) 0.6849(5) 0.051(2) Uani 1 1 d D . . O3W O 0.8953(8) 0.2182(8) 0.4343(5) 0.052(2) Uani 1 1 d D . . O4W O 0.9458(7) -0.1405(7) 0.1001(5) 0.0322(15) Uani 1 1 d D . . O5W O -0.0849(7) 0.3872(7) 0.0268(5) 0.0325(15) Uani 1 1 d D . . O6W O 0.8089(8) 0.1403(11) 0.0968(4) 0.0463(19) Uani 1 1 d D . . O7W O 0.2435(7) 1.1465(11) 0.0113(4) 0.0387(15) Uani 1 1 d D . . H1 H 0.543(10) -0.747(10) 0.412(7) 0.046 Uiso 1 1 d . . . H1W1 H 0.712(4) -1.367(12) 0.645(5) 0.046 Uiso 1 1 d D . . H1W2 H 0.852(4) -1.358(14) 0.673(4) 0.046 Uiso 1 1 d D . . H2W1 H 1.094(4) -1.018(10) 0.694(7) 0.046 Uiso 1 1 d D . . H2W2 H 0.977(8) -1.043(9) 0.716(6) 0.046 Uiso 1 1 d D . . H3W1 H 0.855(7) 0.213(9) 0.3739(10) 0.046 Uiso 1 1 d D . . H3W2 H 0.837(6) 0.218(11) 0.462(5) 0.046 Uiso 1 1 d D . . H4W2 H 0.881(5) -0.200(7) 0.070(6) 0.046 Uiso 1 1 d D . . H5W1 H -0.107(7) 0.298(4) 0.037(6) 0.046 Uiso 1 1 d D . . H5W2 H -0.005(4) 0.407(8) 0.064(6) 0.046 Uiso 1 1 d D . . H6W2 H 0.776(6) 0.170(13) 0.140(4) 0.046 Uiso 1 1 d D . . H7W1 H 0.193(8) 1.068(7) -0.002(6) 0.046 Uiso 1 1 d D . . H7W2 H 0.282(8) 1.153(11) 0.0717(12) 0.046 Uiso 1 1 d D . . H4W1 H 0.914(7) -0.061(6) 0.116(7) 0.046 Uiso 1 1 d D . . H6W1 H 0.8954(13) 0.145(15) 0.121(5) 0.046 Uiso 1 1 d 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 0.01297(17) 0.01239(14) 0.01341(15) 0.0002(2) 0.00615(12) -0.0020(2) P1 0.0191(12) 0.0190(10) 0.0175(10) 0.0049(8) 0.0071(9) -0.0017(10) K1 0.0311(12) 0.0229(9) 0.0247(10) -0.0060(7) 0.0135(9) -0.0021(9) K2 0.0171(10) 0.0427(11) 0.0230(10) 0.0027(9) 0.0094(8) 0.0002(10) K3 0.0207(11) 0.0245(9) 0.0302(10) 0.0023(8) 0.0042(9) -0.0025(9) N1 0.012(4) 0.011(3) 0.022(4) -0.002(3) 0.009(3) -0.001(3) N2 0.020(4) 0.011(3) 0.012(3) -0.005(3) 0.004(3) -0.003(3) O1 0.019(3) 0.021(3) 0.020(3) 0.002(2) 0.012(3) -0.003(3) O2 0.030(4) 0.024(3) 0.033(4) 0.005(3) 0.015(3) 0.010(3) O3 0.018(3) 0.021(3) 0.019(3) -0.005(2) 0.009(3) -0.003(3) O4 0.016(3) 0.053(4) 0.036(4) -0.011(3) 0.014(3) -0.012(3) O5 0.019(3) 0.029(3) 0.010(3) 0.000(2) 0.003(2) -0.008(3) O6 0.018(4) 0.070(5) 0.029(4) -0.001(3) 0.011(3) -0.007(4) O7 0.020(4) 0.021(3) 0.028(3) -0.005(2) 0.003(3) 0.000(3) O8 0.029(4) 0.020(3) 0.030(3) -0.003(3) 0.011(3) 0.009(3) O9 0.025(4) 0.026(3) 0.030(3) 0.013(3) 0.009(3) -0.004(3) O10 0.020(3) 0.034(3) 0.018(3) 0.011(3) 0.008(3) -0.002(3) O11 0.024(4) 0.035(3) 0.024(3) 0.005(3) 0.004(3) 0.006(3) C1 0.022(5) 0.012(4) 0.032(5) -0.002(4) 0.016(5) -0.007(4) C2 0.016(5) 0.027(4) 0.012(4) 0.004(3) 0.005(4) 0.001(4) C3 0.019(5) 0.019(4) 0.021(4) -0.001(3) 0.012(4) -0.001(4) C4 0.034(6) 0.012(4) 0.022(4) -0.002(3) 0.015(4) 0.004(4) C5 0.018(5) 0.021(4) 0.019(4) -0.002(3) 0.009(4) -0.005(4) C6 0.021(5) 0.025(4) 0.019(4) 0.006(3) 0.009(4) 0.002(4) C7 0.024(5) 0.011(4) 0.014(4) -0.001(3) 0.000(4) 0.004(4) C8 0.017(5) 0.020(4) 0.012(4) 0.002(3) 0.003(3) -0.004(4) C9 0.026(5) 0.017(4) 0.016(4) -0.001(3) 0.011(4) 0.004(4) C10 0.022(5) 0.017(4) 0.015(4) 0.001(3) 0.006(4) -0.009(4) O1W 0.040(4) 0.043(5) 0.039(4) 0.000(3) 0.019(3) 0.003(4) O2W 0.027(4) 0.094(6) 0.032(4) 0.011(4) 0.010(4) 0.010(5) O3W 0.058(5) 0.072(5) 0.023(4) 0.001(3) 0.008(3) 0.043(4) O4W 0.032(4) 0.029(3) 0.035(4) -0.001(3) 0.012(3) -0.002(3) O5W 0.028(4) 0.036(4) 0.028(4) 0.004(3) 0.002(3) -0.005(3) O6W 0.068(5) 0.033(4) 0.051(4) -0.001(4) 0.037(4) 0.002(5) O7W 0.038(4) 0.035(4) 0.039(3) 0.007(4) 0.009(3) -0.005(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 Gd1 N1 2.597(6) . ? Gd1 N2 2.635(6) . ? Gd1 O1 2.416(6) . ? Gd1 O3 2.387(6) . ? Gd1 O5 2.377(6) . ? Gd1 O7 2.445(6) . ? Gd1 O9 2.310(5) . ? Gd1 O10 2.306(5) 2_656 ? P1 O9 1.532(6) . ? P1 O10 1.518(6) . ? P1 O11 1.496(6) . ? K1 O3 2.706(5) 1_545 ? K1 O5 2.754(6) 2_646 ? K1 O10 2.752(6) 2_646 ? K1 O11 2.802(6) . ? K1 O1W 2.876(7) . ? K1 O2W 2.789(8) . ? K2 O1 2.730(6) 1_655 ? K2 O4 2.667(6) . ? K2 O5 3.358(6) 1_655 ? K2 O6 3.312(7) 1_655 ? K2 O11 2.731(6) 2_756 ? K2 O1W 3.154(8) 2_766 ? K2 O2W 2.979(8) 2_756 ? K2 O4W 2.767(7) . ? K3 O3 2.928(6) 2_756 ? K3 O4 2.736(7) . ? K3 O7 2.938(6) 2_756 ? K3 O9 3.053(7) 2_756 ? K3 O11 3.292(6) 2_756 ? K3 O1W 2.822(6) 2_766 ? K3 O2W 3.066(7) 1_565 ? K3 O3W 2.869(7) 2_746 ? K3 O3W 2.661(7) . ? N1 C1 1.471(10) . ? N1 C3 1.481(10) . ? N1 C9 1.474(10) . ? N2 C5 1.481(10) . ? N2 C7 1.470(10) . ? N2 C10 1.502(9) . ? O1 K2 2.730(6) 1_455 ? O1 C2 1.265(9) . ? O2 C2 1.258(9) . ? O3 K1 2.706(5) 1_565 ? O3 K3 2.928(6) 2_746 ? O3 C4 1.281(9) . ? O4 C4 1.239(11) . ? O5 K1 2.754(6) 2_656 ? O5 K2 3.358(6) 1_455 ? O5 C6 1.266(9) . ? O6 K2 3.312(7) 1_455 ? O6 C6 1.241(10) . ? O7 K3 2.938(6) 2_746 ? O7 C8 1.264(9) . ? O8 C8 1.253(9) . ? O9 K3 3.053(7) 2_746 ? O10 Gd1 2.306(5) 2_646 ? O10 K1 2.752(6) 2_656 ? O11 K2 2.731(6) 2_746 ? O11 K3 3.292(6) 2_746 ? C1 C2 1.528(11) . ? C2 K2 3.518(8) 1_455 ? C3 C4 1.500(11) . ? C4 K3 3.492(8) 2_746 ? C5 C6 1.531(10) . ? C6 K2 3.403(9) 1_455 ? C7 C8 1.524(11) . ? C9 C10 1.524(11) . ? O1W K2 3.154(7) 2_736 ? O1W K3 2.822(6) 2_736 ? O2W K2 2.979(8) 2_746 ? O2W K3 3.066(7) 1_545 ? O3W K3 2.869(7) 2_756 ? 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 K1 Gd1 K1 105.40(3) 1_565 2_656 ? K1 Gd1 K2 103.90(4) 1_565 1_455 ? K2 Gd1 K1 54.33(4) 1_455 2_656 ? K3 Gd1 K1 60.44(4) 2_746 1_565 ? K3 Gd1 K1 108.23(4) 2_746 2_656 ? K3 Gd1 K2 154.94(4) 2_746 1_455 ? N1 Gd1 K1 149.49(15) . 2_656 ? N1 Gd1 K1 92.48(14) . 1_565 ? N1 Gd1 K2 97.84(15) . 1_455 ? N1 Gd1 K3 102.06(15) . 2_746 ? N1 Gd1 N2 67.61(19) . . ? N2 Gd1 K1 97.33(14) . 2_656 ? N2 Gd1 K1 157.24(14) . 1_565 ? N2 Gd1 K2 90.19(15) . 1_455 ? N2 Gd1 K3 111.37(15) . 2_746 ? O1 Gd1 K1 99.38(13) . 1_565 ? O1 Gd1 K1 88.34(13) . 2_656 ? O1 Gd1 K2 34.12(13) . 1_455 ? O1 Gd1 K3 156.24(13) . 2_746 ? O1 Gd1 N1 64.10(19) . . ? O1 Gd1 N2 82.21(19) . . ? O1 Gd1 O7 138.72(18) . . ? O3 Gd1 K1 38.66(12) . 1_565 ? O3 Gd1 K1 140.83(13) . 2_656 ? O3 Gd1 K2 132.29(13) . 1_455 ? O3 Gd1 K3 47.70(13) . 2_746 ? O3 Gd1 N1 65.68(19) . . ? O3 Gd1 N2 119.22(19) . . ? O3 Gd1 O1 108.89(19) . . ? O3 Gd1 O7 72.96(18) . . ? O5 Gd1 K1 34.07(13) . 2_656 ? O5 Gd1 K1 137.86(13) . 1_565 ? O5 Gd1 K2 49.58(14) . 1_455 ? O5 Gd1 K3 127.81(14) . 2_746 ? O5 Gd1 N1 119.97(19) . . ? O5 Gd1 N2 64.68(19) . . ? O5 Gd1 O1 75.25(18) . . ? O5 Gd1 O3 174.33(19) . . ? O5 Gd1 O7 106.7(2) . . ? O7 Gd1 K1 104.08(14) . 1_565 ? O7 Gd1 K1 116.74(14) . 2_656 ? O7 Gd1 K2 152.02(14) . 1_455 ? O7 Gd1 K3 48.06(14) . 2_746 ? O7 Gd1 N1 81.26(19) . . ? O7 Gd1 N2 63.4(2) . . ? O9 Gd1 K1 79.56(15) . 1_565 ? O9 Gd1 K1 57.72(16) . 2_656 ? O9 Gd1 K2 110.19(16) . 1_455 ? O9 Gd1 K3 50.61(16) . 2_746 ? O9 Gd1 N1 151.9(2) . . ? O9 Gd1 N2 112.6(2) . . ? O9 Gd1 O1 143.5(2) . . ? O9 Gd1 O3 93.0(2) . . ? O9 Gd1 O5 81.5(2) . . ? O9 Gd1 O7 74.8(2) . . ? O10 Gd1 K1 72.56(15) 2_656 2_656 ? O10 Gd1 K1 39.21(15) 2_656 1_565 ? O10 Gd1 K2 67.57(15) 2_656 1_455 ? O10 Gd1 K3 90.95(15) 2_656 2_746 ? O10 Gd1 N1 111.0(2) 2_656 . ? O10 Gd1 N2 157.6(2) 2_656 . ? O10 Gd1 O1 77.62(19) 2_656 . ? O10 Gd1 O3 77.13(19) 2_656 . ? O10 Gd1 O5 100.4(2) 2_656 . ? O10 Gd1 O7 139.0(2) 2_656 . ? O10 Gd1 O9 79.5(2) 2_656 . ? K1 P1 K1 130.58(7) 2_656 . ? K1 P1 K2 130.07(7) 2_656 2_746 ? K1 P1 K3 133.47(7) 2_656 2_746 ? K2 P1 K1 63.18(5) 2_746 . ? K3 P1 K1 95.77(7) 2_746 . ? K3 P1 K2 61.88(5) 2_746 2_746 ? O9 P1 K1 81.8(3) . 2_656 ? O9 P1 K1 147.7(3) . . ? O9 P1 K2 97.8(3) . 2_746 ? O9 P1 K3 52.0(3) . 2_746 ? O10 P1 K1 96.6(2) . . ? O10 P1 K1 45.3(2) . 2_656 ? O10 P1 K2 90.7(2) . 2_746 ? O10 P1 K3 140.0(3) . 2_746 ? O10 P1 O9 110.2(3) . . ? O11 P1 K1 159.6(3) . 2_656 ? O11 P1 K1 37.0(2) . . ? O11 P1 K2 36.7(2) . 2_746 ? O11 P1 K3 61.0(2) . 2_746 ? O11 P1 O9 112.4(4) . . ? O11 P1 O10 114.3(3) . . ? P1 K1 Gd1 54.71(4) 2_646 1_545 ? P1 K1 Gd1 101.62(6) . 1_545 ? P1 K1 P1 80.92(5) 2_646 . ? P1 K1 K2 57.58(5) . 2_746 ? P1 K1 K2 116.17(6) 2_646 2_746 ? P1 K1 K3 97.86(6) 2_646 2_736 ? P1 K1 K3 152.07(7) . 2_736 ? P1 K1 K3 97.86(6) . 1_545 ? P1 K1 K3 161.68(7) 2_646 1_545 ? K2 K1 Gd1 159.20(6) 2_746 1_545 ? K2 K1 K3 141.45(7) 2_746 2_736 ? K3 K1 Gd1 108.27(5) 1_545 1_545 ? K3 K1 Gd1 57.59(4) 2_736 1_545 ? K3 K1 K2 77.22(5) 1_545 2_746 ? K3 K1 K3 74.62(4) 1_545 2_736 ? O3 K1 Gd1 33.45(12) 1_545 1_545 ? O3 K1 P1 87.88(13) 1_545 2_646 ? O3 K1 P1 106.10(13) 1_545 . ? O3 K1 K2 145.01(13) 1_545 2_746 ? O3 K1 K3 74.83(13) 1_545 1_545 ? O3 K1 K3 46.08(12) 1_545 2_736 ? O3 K1 O5 155.67(18) 1_545 2_646 ? O3 K1 O10 64.84(16) 1_545 2_646 ? O3 K1 O11 111.90(17) 1_545 . ? O3 K1 O1W 82.60(17) 1_545 . ? O3 K1 O2W 120.5(2) 1_545 . ? O5 K1 Gd1 122.22(14) 2_646 1_545 ? O5 K1 P1 67.98(14) 2_646 2_646 ? O5 K1 P1 74.20(12) 2_646 . ? O5 K1 K2 56.11(13) 2_646 2_746 ? O5 K1 K3 129.50(14) 2_646 1_545 ? O5 K1 K3 131.44(13) 2_646 2_736 ? O5 K1 O11 76.47(17) 2_646 . ? O5 K1 O1W 87.82(17) 2_646 . ? O5 K1 O2W 82.2(2) 2_646 . ? O10 K1 Gd1 31.99(11) 2_646 1_545 ? O10 K1 P1 23.09(11) 2_646 2_646 ? O10 K1 P1 86.66(14) 2_646 . ? O10 K1 K2 135.25(13) 2_646 2_746 ? O10 K1 K3 82.52(12) 2_646 2_736 ? O10 K1 K3 138.97(12) 2_646 1_545 ? O10 K1 O5 91.08(18) 2_646 2_646 ? O10 K1 O11 105.31(19) 2_646 . ? O10 K1 O1W 74.66(19) 2_646 . ? O10 K1 O2W 166.8(2) 2_646 . ? O11 K1 Gd1 116.69(13) . 1_545 ? O11 K1 P1 18.77(13) . . ? O11 K1 P1 98.97(15) . 2_646 ? O11 K1 K2 43.07(12) . 2_746 ? O11 K1 K3 82.35(14) . 1_545 ? O11 K1 K3 151.53(14) . 2_736 ? O11 K1 O1W 164.28(19) . . ? O1W K1 Gd1 71.83(13) . 1_545 ? O1W K1 P1 74.74(15) . 2_646 ? O1W K1 P1 153.87(16) . . ? O1W K1 K2 126.48(14) . 2_746 ? O1W K1 K3 44.01(13) . 2_736 ? O1W K1 K3 108.24(15) . 1_545 ? O2W K1 Gd1 149.74(17) . 1_545 ? O2W K1 P1 148.12(16) . 2_646 ? O2W K1 P1 102.32(18) . . ? O2W K1 K2 48.15(17) . 2_746 ? O2W K1 K3 50.12(15) . 1_545 ? O2W K1 K3 93.34(18) . 2_736 ? O2W K1 O11 84.3(2) . . ? O2W K1 O1W 93.6(2) . . ? P1 K2 K3 58.65(5) 2_756 . ? O1 K2 P1 67.68(13) 1_655 2_756 ? O1 K2 K3 113.49(13) 1_655 . ? O1 K2 O5 56.33(14) 1_655 1_655 ? O1 K2 O6 81.00(16) 1_655 1_655 ? O1 K2 O11 83.25(18) 1_655 2_756 ? O1 K2 C2 18.37(17) 1_655 1_655 ? O1 K2 C6 61.14(18) 1_655 1_655 ? O1 K2 O1W 76.02(17) 1_655 2_766 ? O1 K2 O2W 126.0(2) 1_655 2_756 ? O1 K2 O4W 95.38(19) 1_655 . ? O4 K2 P1 98.68(15) . 2_756 ? O4 K2 K3 44.99(14) . . ? O4 K2 O1 156.8(2) . 1_655 ? O4 K2 O5 138.38(18) . 1_655 ? O4 K2 O6 121.76(19) . 1_655 ? O4 K2 O11 88.0(2) . 2_756 ? O4 K2 C2 142.0(2) . 1_655 ? O4 K2 C6 140.4(2) . 1_655 ? O4 K2 O1W 80.96(19) . 2_766 ? O4 K2 O2W 73.6(2) . 2_756 ? O4 K2 O4W 93.8(2) . . ? O5 K2 P1 69.38(10) 1_655 2_756 ? O5 K2 K3 124.62(10) 1_655 . ? O5 K2 C2 74.67(17) 1_655 1_655 ? O5 K2 C6 21.58(16) 1_655 1_655 ? O6 K2 P1 106.54(12) 1_655 2_756 ? O6 K2 K3 147.69(12) 1_655 . ? O6 K2 O5 38.90(14) 1_655 1_655 ? O6 K2 C2 95.87(17) 1_655 1_655 ? O6 K2 C6 21.25(17) 1_655 1_655 ? O11 K2 P1 19.14(13) 2_756 2_756 ? O11 K2 K3 56.75(13) 2_756 . ? O11 K2 O5 67.87(16) 2_756 1_655 ? O11 K2 O6 99.31(17) 2_756 1_655 ? O11 K2 C2 91.40(19) 2_756 1_655 ? O11 K2 C6 88.96(19) 2_756 1_655 ? O11 K2 O1W 75.32(18) 2_756 2_766 ? O11 K2 O2W 82.01(19) 2_756 2_756 ? O11 K2 O4W 178.0(2) 2_756 . ? C2 K2 P1 73.22(13) 1_655 2_756 ? C2 K2 K3 105.26(14) 1_655 . ? C6 K2 P1 90.79(15) 1_655 2_756 ? C6 K2 K3 145.39(15) 1_655 . ? C6 K2 C2 77.6(2) 1_655 1_655 ? O1W K2 P1 61.86(13) 2_766 2_756 ? O1W K2 K3 46.00(12) 2_766 . ? O1W K2 O5 121.50(17) 2_766 1_655 ? O1W K2 O6 156.84(18) 2_766 1_655 ? O1W K2 C2 62.23(18) 2_766 1_655 ? O1W K2 C6 135.9(2) 2_766 1_655 ? O2W K2 P1 100.24(16) 2_756 2_756 ? O2W K2 K3 100.56(14) 2_756 . ? O2W K2 O5 69.95(19) 2_756 1_655 ? O2W K2 O6 51.00(18) 2_756 1_655 ? O2W K2 C2 143.9(2) 2_756 1_655 ? O2W K2 C6 66.9(2) 2_756 1_655 ? O2W K2 O1W 146.32(18) 2_756 2_766 ? O4W K2 P1 160.45(16) . 2_756 ? O4W K2 K3 125.19(14) . . ? O4W K2 O5 110.19(16) . 1_655 ? O4W K2 O6 79.05(17) . 1_655 ? O4W K2 C2 87.70(19) . 1_655 ? O4W K2 C6 89.14(19) . 1_655 ? O4W K2 O1W 105.76(18) . 2_766 ? O4W K2 O2W 97.7(2) . 2_756 ? P1 K3 K2 59.48(5) 2_756 . ? O3 K3 P1 92.33(12) 2_756 2_756 ? O3 K3 K2 131.67(12) 2_756 . ? O3 K3 O7 58.65(15) 2_756 2_756 ? O3 K3 O9 69.44(15) 2_756 2_756 ? O3 K3 O11 115.75(16) 2_756 2_756 ? O3 K3 C4 20.72(17) 2_756 2_756 ? O3 K3 O2W 83.2(2) 2_756 1_565 ? O4 K3 P1 98.17(15) . 2_756 ? O4 K3 K2 43.56(14) . . ? O4 K3 O3 156.85(19) . 2_756 ? O4 K3 O7 144.44(19) . 2_756 ? O4 K3 O9 117.71(18) . 2_756 ? O4 K3 O11 76.32(18) . 2_756 ? O4 K3 C4 152.5(2) . 2_756 ? O4 K3 O1W 86.2(2) . 2_766 ? O4 K3 O2W 109.2(2) . 1_565 ? O4 K3 O3W 72.3(2) . 2_746 ? O7 K3 P1 65.56(13) 2_756 2_756 ? O7 K3 K2 123.79(13) 2_756 . ? O7 K3 O9 57.64(17) 2_756 2_756 ? O7 K3 O11 80.30(16) 2_756 2_756 ? O7 K3 C4 58.17(18) 2_756 2_756 ? O7 K3 O2W 60.12(18) 2_756 1_565 ? O9 K3 P1 23.30(11) 2_756 2_756 ? O9 K3 K2 75.08(11) 2_756 . ? O9 K3 O11 46.53(15) 2_756 2_756 ? O9 K3 C4 86.9(2) 2_756 2_756 ? O9 K3 O2W 117.56(19) 2_756 1_565 ? O11 K3 P1 23.43(11) 2_756 2_756 ? O11 K3 K2 43.92(10) 2_756 . ? O11 K3 C4 130.9(2) 2_756 2_756 ? C4 K3 P1 108.36(17) 2_756 2_756 ? C4 K3 K2 151.75(15) 2_756 . ? O1W K3 P1 64.77(16) 2_766 2_756 ? O1W K3 K2 53.51(15) 2_766 . ? O1W K3 O3 79.72(18) 2_766 2_756 ? O1W K3 O7 111.55(19) 2_766 2_756 ? O1W K3 O9 57.85(19) 2_766 2_756 ? O1W K3 O11 71.93(19) 2_766 2_756 ? O1W K3 C4 98.5(2) 2_766 2_756 ? O1W K3 O2W 162.8(2) 2_766 1_565 ? O1W K3 O3W 122.3(2) 2_766 2_746 ? O2W K3 P1 118.44(15) 1_565 2_756 ? O2W K3 K2 143.58(18) 1_565 . ? O2W K3 O11 118.24(18) 1_565 2_756 ? O2W K3 C4 64.3(2) 1_565 2_756 ? O3W K3 P1 155.05(18) . 2_756 ? O3W K3 P1 66.32(17) 2_746 2_756 ? O3W K3 K2 102.71(15) . . ? O3W K3 K2 76.10(15) 2_746 . ? O3W K3 O3 87.8(2) . 2_756 ? O3W K3 O3 130.83(18) 2_746 2_756 ? O3W K3 O4 74.0(2) . . ? O3W K3 O7 72.18(18) 2_746 2_756 ? O3W K3 O7 133.2(2) . 2_756 ? O3W K3 O9 85.8(2) 2_746 2_756 ? O3W K3 O9 143.3(2) . 2_756 ? O3W K3 O11 51.35(19) 2_746 2_756 ? O3W K3 O11 146.48(19) . 2_756 ? O3W K3 C4 78.8(2) . 2_756 ? O3W K3 C4 124.8(2) 2_746 2_756 ? O3W K3 O1W 90.8(2) . 2_766 ? O3W K3 O2W 71.4(2) 2_746 1_565 ? O3W K3 O2W 86.4(2) . 1_565 ? O3W K3 O3W 129.92(14) . 2_746 ? C1 N1 Gd1 103.9(4) . . ? C1 N1 C3 109.6(6) . . ? C1 N1 C9 108.0(6) . . ? C3 N1 Gd1 108.4(4) . . ? C9 N1 Gd1 113.4(5) . . ? C9 N1 C3 113.1(6) . . ? C5 N2 Gd1 108.0(4) . . ? C5 N2 C10 112.2(6) . . ? C7 N2 Gd1 104.7(4) . . ? C7 N2 C5 111.0(6) . . ? C7 N2 C10 107.9(6) . . ? C10 N2 Gd1 112.8(4) . . ? Gd1 O1 K2 116.1(2) . 1_455 ? C2 O1 Gd1 119.9(5) . . ? C2 O1 K2 118.8(5) . 1_455 ? Gd1 O3 K1 107.9(2) . 1_565 ? Gd1 O3 K3 95.22(18) . 2_746 ? K1 O3 K3 92.18(16) 1_565 2_746 ? C4 O3 Gd1 122.9(5) . . ? C4 O3 K1 123.4(5) . 1_565 ? C4 O3 K3 105.3(5) . 2_746 ? K2 O4 K3 91.5(2) . . ? C4 O4 K2 128.4(5) . . ? C4 O4 K3 139.9(5) . . ? Gd1 O5 K1 117.0(2) . 2_656 ? Gd1 O5 K2 97.81(18) . 1_455 ? K1 O5 K2 80.98(16) 2_656 1_455 ? C6 O5 Gd1 123.4(5) . . ? C6 O5 K1 118.6(5) . 2_656 ? C6 O5 K2 81.2(5) . 1_455 ? C6 O6 K2 83.5(5) . 1_455 ? Gd1 O7 K3 93.71(18) . 2_746 ? C8 O7 Gd1 120.8(5) . . ? C8 O7 K3 131.2(5) . 2_746 ? Gd1 O9 K3 93.60(19) . 2_746 ? P1 O9 Gd1 143.5(4) . . ? P1 O9 K3 104.7(3) . 2_746 ? Gd1 O10 K1 108.8(2) 2_646 2_656 ? P1 O10 Gd1 137.7(3) . 2_646 ? P1 O10 K1 111.6(3) . 2_656 ? P1 O11 K1 124.2(3) . . ? P1 O11 K2 124.1(3) . 2_746 ? P1 O11 K3 95.6(3) . 2_746 ? K1 O11 K3 135.0(2) . 2_746 ? K2 O11 K1 92.45(18) 2_746 . ? K2 O11 K3 79.33(16) 2_746 2_746 ? N1 C1 C2 111.1(6) . . ? O1 C2 K2 42.9(4) . 1_455 ? O1 C2 C1 115.9(7) . . ? O2 C2 K2 82.8(5) . 1_455 ? O2 C2 O1 125.7(8) . . ? O2 C2 C1 118.3(7) . . ? C1 C2 K2 158.4(5) . 1_455 ? N1 C3 C4 112.8(6) . . ? O3 C4 K3 54.0(4) . 2_746 ? O3 C4 C3 117.9(8) . . ? O4 C4 K3 88.5(5) . 2_746 ? O4 C4 O3 123.5(8) . . ? O4 C4 C3 118.6(7) . . ? C3 C4 K3 129.6(5) . 2_746 ? N2 C5 C6 111.6(7) . . ? O5 C6 K2 77.2(5) . 1_455 ? O5 C6 C5 117.6(8) . . ? O6 C6 K2 75.3(5) . 1_455 ? O6 C6 O5 124.7(8) . . ? O6 C6 C5 117.6(7) . . ? C5 C6 K2 117.4(5) . 1_455 ? N2 C7 C8 110.5(7) . . ? O7 C8 C7 116.8(7) . . ? O8 C8 O7 123.9(8) . . ? O8 C8 C7 119.3(7) . . ? N1 C9 C10 112.1(7) . . ? N2 C10 C9 110.2(7) . . ? K1 O1W K2 163.5(3) . 2_736 ? K3 O1W K1 90.91(19) 2_736 . ? K3 O1W K2 80.49(18) 2_736 2_736 ? K1 O2W K2 87.6(2) . 2_746 ? K1 O2W K3 85.6(2) . 1_545 ? K2 O2W K3 110.9(2) 2_746 1_545 ? K3 O3W K3 123.6(3) . 2_756 ? _database_code_depnum_ccdc_archive 'CCDC 951555' ####################################################################### # # Cambridge Crystallographic Data Centre # CCDC # ####################################################################### # # This CIF contains data from an original supplementary publication # deposited with the CCDC, and may include chemical, crystal, # experimental, refinement, atomic coordinates, # anisotropic displacement parameters and molecular geometry data, # as required by the journal to which it was submitted. # # This CIF is provided on the understanding that it is used for bona # fide research purposes only. It may contain copyright material # of the CCDC or of third parties, and may not be copied or further # disseminated in any form, whether machine-readable or not, # except for the purpose of generating routine backup copies # on your local computer system. # # For further information on the CCDC, data deposition and # data retrieval see: # www.ccdc.cam.ac.uk # # Bona fide researchers may freely download Mercury and enCIFer # from this site to visualise CIF-encoded structures and # to carry out CIF format checking respectively. # data_sad _audit_creation_date 2013-07-22 _audit_creation_method ; Olex2 1.1 (compiled 2011.11.01 svn.r2039, GUI svn.r3906) ; _chemical_name_common ? _chemical_name_systematic ; ? ; _chemical_formula_moiety 'C16 H22 Gd N2 Na O17, 2(H2 O), 2(H4 N)' _chemical_formula_sum 'C16 H34 Gd N4 Na O19' _chemical_formula_weight 766.71 _chemical_melting_point ? 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' Gd Gd -0.1653 3.9035 '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' Na Na 0.0362 0.0249 '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' _space_group_crystal_system monoclinic _space_group_IT_number 14 _space_group_name_H-M_alt 'P 1 21/c 1' _space_group_name_Hall '-P 2ybc' loop_ _space_group_symop_id _space_group_symop_operation_xyz 1 'x, y, z' 2 '-x, y+1/2, -z+1/2' 3 '-x, -y, -z' 4 'x, -y-1/2, z-1/2' _cell_length_a 9.3301(5) _cell_length_b 21.3075(13) _cell_length_c 14.0657(10) _cell_angle_alpha 90.00 _cell_angle_beta 106.248(6) _cell_angle_gamma 90.00 _cell_volume 2684.6(3) _cell_formula_units_Z 4 _cell_measurement_reflns_used ? _cell_measurement_temperature 173(2) _cell_measurement_theta_max ? _cell_measurement_theta_min ? _exptl_absorpt_coefficient_mu 2.580 _exptl_absorpt_correction_T_max 0.8818 _exptl_absorpt_correction_T_min 0.8818 _exptl_absorpt_correction_type ? _exptl_absorpt_process_details ? _exptl_crystal_colour ? _exptl_crystal_density_diffrn 1.897 _exptl_crystal_density_meas ? _exptl_crystal_density_method 'not measured' _exptl_crystal_description ? _exptl_crystal_F_000 1540 _exptl_crystal_size_max 0.05 _exptl_crystal_size_mid 0.05 _exptl_crystal_size_min 0.05 _exptl_special_details ; ? ; _diffrn_reflns_av_R_equivalents 0.1205 _diffrn_reflns_av_unetI/netI 0.1304 _diffrn_reflns_limit_h_max 11 _diffrn_reflns_limit_h_min -9 _diffrn_reflns_limit_k_max 25 _diffrn_reflns_limit_k_min -25 _diffrn_reflns_limit_l_max 12 _diffrn_reflns_limit_l_min -17 _diffrn_reflns_number 18172 _diffrn_reflns_theta_full 26.00 _diffrn_reflns_theta_max 26.00 _diffrn_reflns_theta_min 2.97 _diffrn_ambient_temperature 173(2) _diffrn_detector_area_resol_mean ? _diffrn_measured_fraction_theta_full 0.984 _diffrn_measured_fraction_theta_max 0.984 _diffrn_measurement_device_type ? _diffrn_measurement_method ? _diffrn_radiation_monochromator graphite _diffrn_radiation_type MoK\a _diffrn_radiation_wavelength 0.71073 _diffrn_source 'fine-focus sealed tube' _diffrn_standards_decay_% ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_number ? _reflns_number_gt 3657 _reflns_number_total 5201 _reflns_threshold_expression >2sigma(I) _computing_cell_refinement ? _computing_data_collection ? _computing_data_reduction ? _computing_molecular_graphics ; O. V. Dolomanov, L. J. Bourhis, R. J. Gildea, J. A. K. Howard and H. Puschmann, OLEX2: a complete structure solution, refinement and analysis program. J. Appl. Cryst. (2009). 42, 339-341. ; _computing_publication_material ; O. V. Dolomanov, L. J. Bourhis, R. J. Gildea, J. A. K. Howard and H. Puschmann, OLEX2: a complete structure solution, refinement and analysis program. J. Appl. Cryst. (2009). 42, 339-341. ; _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _refine_diff_density_max 1.722 _refine_diff_density_min -1.421 _refine_diff_density_rms 0.170 _refine_ls_extinction_coef ? _refine_ls_extinction_method none _refine_ls_goodness_of_fit_ref 1.007 _refine_ls_hydrogen_treatment mixed _refine_ls_matrix_type full _refine_ls_number_parameters 472 _refine_ls_number_reflns 5201 _refine_ls_number_restraints 25 _refine_ls_R_factor_all 0.0954 _refine_ls_R_factor_gt 0.0594 _refine_ls_restrained_S_all 1.005 _refine_ls_shift/su_max 0.000 _refine_ls_shift/su_mean 0.000 _refine_ls_structure_factor_coef Fsqd _refine_ls_weighting_details 'calc w=1/[\s^2^(Fo^2^)+(0.0077P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3' _refine_ls_weighting_scheme calc _refine_ls_wR_factor_gt 0.0961 _refine_ls_wR_factor_ref 0.1111 _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. ; _atom_sites_solution_hydrogens geom _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap 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 0.16495(4) 0.356727(19) 0.64894(3) 0.01905(13) Uani 1 1 d . . . O4 O -0.0699(5) 0.3466(2) 0.5253(4) 0.0241(14) Uani 1 1 d . . . O5 O 0.1682(6) 0.4684(3) 0.3796(4) 0.0273(14) Uani 1 1 d . . . N2 N 0.0818(6) 0.2409(3) 0.5787(5) 0.0202(16) Uani 1 1 d . . . O7 O 0.2150(5) 0.4266(3) 0.9535(4) 0.0265(14) Uani 1 1 d . . . O8 O -0.2837(5) 0.2978(3) 0.4613(4) 0.0316(15) Uani 1 1 d . . . O10 O 0.0494(5) 0.4494(3) 0.6963(4) 0.0233(13) Uani 1 1 d D . . H10 H -0.016(6) 0.474(3) 0.661(2) 0.035 Uiso 1 1 d D . . O11 O 0.0053(5) 0.3226(2) 0.7440(4) 0.0232(13) Uani 1 1 d . . . O12 O 0.2770(6) 0.5435(3) 0.8095(5) 0.0352(16) Uani 1 1 d . . . O13 O 0.4091(6) 0.1746(3) 0.7465(4) 0.0307(15) Uani 1 1 d . . . N1 N 0.2857(6) 0.3254(3) 0.5083(5) 0.0212(16) Uani 1 1 d . . . O15 O 0.5783(6) 0.4358(3) 0.5992(5) 0.0386(17) Uani 1 1 d . . . C16 C -0.0964(8) 0.3455(4) 0.7770(6) 0.024(2) Uani 1 1 d . . . O17 O 0.3301(5) 0.2742(3) 0.7227(4) 0.0244(14) Uani 1 1 d . . . O18 O 0.1447(5) 0.4373(3) 0.5254(4) 0.0224(13) Uani 1 1 d . . . O20 O -0.2044(6) 0.3153(3) 0.7900(5) 0.0368(16) Uani 1 1 d . . . O21 O 0.1076(6) 0.6192(3) 0.7841(5) 0.0383(17) Uani 1 1 d . . . H21 H 0.189(10) 0.650(5) 0.774(7) 0.057 Uiso 1 1 d . . . C22 C 0.4461(9) 0.3422(4) 0.5379(7) 0.028(2) Uani 1 1 d . . . H22A H 0.495(8) 0.345(4) 0.494(6) 0.033 Uiso 1 1 d . . . H22B H 0.495(8) 0.309(4) 0.578(6) 0.033 Uiso 1 1 d . . . C25 C 0.1714(8) 0.4286(4) 0.4434(7) 0.026(2) Uani 1 1 d . . . C26 C 0.1915(8) 0.4220(4) 0.8609(6) 0.0205(19) Uani 1 1 d . . . C27 C 0.0436(8) 0.4519(4) 0.7980(6) 0.0201(19) Uani 1 1 d D . . O28 O 0.4071(5) 0.4024(3) 0.6705(4) 0.0284(15) Uani 1 1 d . . . O29 O 0.2740(6) 0.3950(3) 0.8176(4) 0.0253(14) Uani 1 1 d . . . C30 C 0.4797(9) 0.3996(4) 0.6069(7) 0.026(2) Uani 1 1 d . . . C32 C -0.0887(9) 0.4149(4) 0.8085(7) 0.023(2) Uani 1 1 d . . . H32A H -0.171(8) 0.432(4) 0.769(6) 0.028 Uiso 1 1 d . . . H32B H -0.103(7) 0.418(4) 0.876(6) 0.028 Uiso 1 1 d . . . C33 C 0.3113(8) 0.2155(4) 0.7099(7) 0.028(2) Uani 1 1 d . . . C34 C 0.1586(9) 0.1936(4) 0.6506(7) 0.024(2) Uani 1 1 d . . . H34A H 0.166(7) 0.151(4) 0.613(6) 0.029 Uiso 1 1 d . . . H34B H 0.118(8) 0.180(4) 0.692(6) 0.029 Uiso 1 1 d . . . C37 C 0.2074(10) 0.3610(4) 0.4207(7) 0.027(2) Uani 1 1 d . . . H37A H 0.117(8) 0.337(4) 0.390(6) 0.033 Uiso 1 1 d . . . H37B H 0.262(8) 0.360(4) 0.371(6) 0.033 Uiso 1 1 d . . . C38 C 0.1521(9) 0.5620(4) 0.8062(6) 0.025(2) Uani 1 1 d . . . C39 C 0.0344(9) 0.5198(4) 0.8292(7) 0.024(2) Uani 1 1 d . . . H39A H -0.075(8) 0.541(4) 0.792(6) 0.029 Uiso 1 1 d . . . H39B H 0.026(8) 0.529(4) 0.890(6) 0.029 Uiso 1 1 d . . . C41 C -0.0811(9) 0.2379(4) 0.5587(7) 0.028(2) Uani 1 1 d . . . H41A H -0.111(8) 0.234(4) 0.621(6) 0.034 Uiso 1 1 d . . . H41B H -0.145(8) 0.203(4) 0.511(6) 0.034 Uiso 1 1 d . . . C42 C 0.1195(9) 0.2322(4) 0.4833(7) 0.024(2) Uani 1 1 d . . . H42A H 0.035(8) 0.248(4) 0.427(6) 0.029 Uiso 1 1 d . . . H42B H 0.118(8) 0.190(4) 0.479(6) 0.029 Uiso 1 1 d . . . C49 C -0.1544(9) 0.2985(4) 0.5107(6) 0.026(2) Uani 1 1 d . . . O4W O 0.4920(6) 0.3793(3) 1.0373(4) 0.0362(16) Uani 1 1 d D . . H4WA H 0.402(3) 0.391(4) 1.025(5) 0.054 Uiso 1 1 d D . . H4WB H 0.526(7) 0.370(4) 1.0981(19) 0.054 Uiso 1 1 d D . . Na3 Na 0.4620(3) 0.47387(16) 0.7977(3) 0.0306(8) Uani 1 1 d . . . N4 N 0.5703(6) 0.3110(3) 0.8814(5) 0.0267(18) Uani 1 1 d D . . H4A H 0.616(5) 0.2786(16) 0.911(4) 0.032 Uiso 1 1 d D . . H4B H 0.539(6) 0.332(2) 0.923(3) 0.032 Uiso 1 1 d D . . H4C H 0.498(4) 0.300(3) 0.833(3) 0.032 Uiso 1 1 d D . . H4D H 0.632(5) 0.332(2) 0.860(4) 0.032 Uiso 1 1 d D . . O19 O 0.6440(7) 0.4624(4) 0.9451(5) 0.0406(18) Uani 1 1 d . . . H3 H 0.603(11) 0.450(5) 0.983(8) 0.061 Uiso 1 1 d . . . H19 H 0.711(9) 0.502(5) 0.971(7) 0.061 Uiso 1 1 d . . . O23 O 0.6941(7) 0.1997(3) 0.7240(6) 0.0390(19) Uani 1 1 d . . . H23A H 0.716(10) 0.236(5) 0.729(8) 0.058 Uiso 1 1 d . . . H23B H 0.640(11) 0.194(5) 0.750(8) 0.058 Uiso 1 1 d . . . N3 N 0.2843(6) 0.5575(3) 0.5538(5) 0.0241(17) Uani 1 1 d D . . H3A H 0.228(5) 0.5263(16) 0.553(4) 0.029 Uiso 1 1 d D . . H3B H 0.316(5) 0.557(3) 0.502(2) 0.029 Uiso 1 1 d D . . H3C H 0.235(5) 0.5912(14) 0.554(4) 0.029 Uiso 1 1 d D . . H3D H 0.360(4) 0.557(3) 0.604(2) 0.029 Uiso 1 1 d D . . O31 O 0.5654(7) 0.5477(3) 0.7168(5) 0.0369(17) Uani 1 1 d . . . H31A H 0.629(10) 0.535(5) 0.685(7) 0.055 Uiso 1 1 d . . . H31B H 0.601(9) 0.583(4) 0.739(7) 0.044 Uiso 1 1 d . . . C1 C 0.2702(9) 0.2566(4) 0.4855(7) 0.026(2) Uani 1 1 d . . . H1A H 0.341(8) 0.236(4) 0.521(6) 0.031 Uiso 1 1 d . . . H1B H 0.285(8) 0.252(4) 0.419(6) 0.031 Uiso 1 1 d . . . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 Gd1 0.0192(2) 0.0158(2) 0.0206(2) -0.0005(2) 0.00303(15) -0.00002(18) O4 0.019(3) 0.015(3) 0.031(4) 0.001(3) -0.003(2) 0.000(2) O5 0.036(3) 0.022(4) 0.025(4) 0.005(3) 0.009(3) 0.004(3) N2 0.019(3) 0.017(4) 0.021(4) 0.000(3) 0.000(3) 0.000(3) O7 0.033(3) 0.024(4) 0.018(4) 0.004(3) 0.001(2) -0.002(3) O8 0.020(3) 0.027(4) 0.042(4) -0.004(3) -0.002(3) 0.005(3) O10 0.025(3) 0.017(3) 0.024(4) -0.001(3) -0.001(2) -0.003(2) O11 0.023(3) 0.016(3) 0.030(4) -0.007(3) 0.006(3) 0.000(2) O12 0.025(3) 0.022(4) 0.058(5) -0.002(3) 0.009(3) 0.001(3) O13 0.027(3) 0.023(4) 0.035(4) 0.007(3) -0.002(3) 0.002(3) N1 0.015(3) 0.019(4) 0.028(4) 0.003(3) 0.004(3) -0.003(3) O15 0.040(4) 0.037(4) 0.042(4) -0.010(3) 0.017(3) -0.016(3) C16 0.023(4) 0.020(5) 0.024(5) 0.003(4) 0.000(4) 0.000(4) O17 0.020(3) 0.017(3) 0.033(4) -0.005(3) 0.003(2) 0.001(2) O18 0.027(3) 0.019(3) 0.023(4) 0.004(3) 0.010(3) -0.002(2) O20 0.036(3) 0.024(4) 0.058(5) -0.010(3) 0.025(3) -0.007(3) O21 0.032(4) 0.013(3) 0.070(5) 0.001(3) 0.014(3) 0.002(3) C22 0.025(5) 0.025(6) 0.033(6) 0.003(5) 0.008(4) 0.004(4) C25 0.026(5) 0.022(5) 0.030(6) 0.004(5) 0.009(4) -0.002(4) C26 0.024(4) 0.012(5) 0.022(5) 0.004(4) 0.001(4) -0.005(3) C27 0.017(4) 0.026(5) 0.016(5) 0.004(4) 0.002(3) 0.001(3) O28 0.027(3) 0.033(4) 0.026(4) -0.008(3) 0.008(3) -0.015(3) O29 0.030(3) 0.022(4) 0.021(4) 0.000(3) 0.002(3) 0.001(3) C30 0.022(5) 0.022(5) 0.028(6) 0.002(4) -0.003(4) 0.000(4) C32 0.031(5) 0.020(5) 0.018(5) 0.001(4) 0.006(4) 0.001(4) C33 0.023(5) 0.032(6) 0.028(6) 0.004(5) 0.007(4) -0.002(4) C34 0.025(5) 0.016(5) 0.026(6) -0.002(4) 0.001(4) -0.003(4) C37 0.037(5) 0.018(5) 0.025(6) 0.004(4) 0.006(4) 0.000(4) C38 0.032(5) 0.026(5) 0.015(5) -0.011(4) -0.001(4) 0.002(4) C39 0.025(4) 0.025(5) 0.021(5) -0.006(4) 0.006(4) 0.000(4) C41 0.024(5) 0.019(5) 0.038(6) -0.004(5) 0.004(4) -0.010(4) C42 0.025(5) 0.024(5) 0.024(5) -0.005(5) 0.005(4) 0.001(4) C49 0.028(5) 0.024(5) 0.023(5) -0.008(4) 0.001(4) 0.004(4) O4W 0.025(3) 0.046(4) 0.031(4) 0.000(4) -0.003(3) 0.001(3) Na3 0.0296(18) 0.020(2) 0.037(2) -0.0008(17) 0.0014(15) -0.0015(14) N4 0.015(3) 0.020(4) 0.042(5) -0.002(4) 0.002(3) 0.004(3) O19 0.036(4) 0.046(5) 0.034(5) -0.003(4) 0.001(3) -0.010(3) O23 0.044(5) 0.021(4) 0.057(5) -0.009(4) 0.023(3) -0.006(3) N3 0.027(4) 0.015(4) 0.027(4) 0.004(3) 0.003(3) 0.000(3) O31 0.045(4) 0.023(4) 0.046(5) -0.009(4) 0.019(3) -0.006(3) C1 0.025(5) 0.018(5) 0.037(6) 0.009(5) 0.013(4) 0.011(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 2.396(5) . ? Gd1 N2 2.690(7) . ? Gd1 O10 2.431(5) . ? Gd1 O11 2.377(5) . ? Gd1 N1 2.622(7) . ? Gd1 O17 2.378(5) . ? Gd1 O18 2.413(5) . ? Gd1 O28 2.400(5) . ? Gd1 O29 2.445(5) . ? Gd1 Na3 3.879(3) . ? O4 C49 1.274(9) . ? O5 C25 1.228(9) . ? N2 C34 1.465(10) . ? N2 C41 1.468(9) . ? N2 C42 1.490(11) . ? O7 C26 1.263(9) . ? O8 C49 1.212(9) . ? O10 C27 1.447(9) . ? O11 C16 1.265(9) . ? O12 C38 1.219(9) . ? O12 Na3 2.317(6) . ? O13 C33 1.262(9) . ? N1 C22 1.481(10) . ? N1 C37 1.457(10) . ? N1 C1 1.500(11) . ? O15 C30 1.228(9) . ? C16 O20 1.252(9) . ? C16 C32 1.539(11) . ? O17 C33 1.268(10) . ? O18 C25 1.259(10) . ? O21 C38 1.298(10) . ? C22 C30 1.539(12) . ? C25 C37 1.534(12) . ? C26 C27 1.553(10) . ? C26 O29 1.247(9) . ? C26 Na3 3.104(8) . ? C27 C32 1.507(11) . ? C27 C39 1.522(11) . ? O28 C30 1.266(10) . ? O28 Na3 2.296(6) . ? O29 Na3 2.502(6) . ? C33 C34 1.510(11) . ? C38 C39 1.521(12) . ? C41 C49 1.526(12) . ? C42 C1 1.492(12) . ? Na3 O19 2.296(7) . ? Na3 O31 2.306(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 O4 Gd1 N2 62.58(18) . . ? O4 Gd1 O10 83.49(17) . . ? O4 Gd1 N1 85.87(18) . . ? O4 Gd1 O18 70.73(17) . . ? O4 Gd1 O28 139.99(19) . . ? O4 Gd1 O29 141.46(18) . . ? O4 Gd1 Na3 145.09(14) . . ? N2 Gd1 Na3 151.33(13) . . ? O10 Gd1 N2 137.86(17) . . ? O10 Gd1 N1 136.9(2) . . ? O10 Gd1 O29 63.85(18) . . ? O10 Gd1 Na3 68.54(12) . . ? O11 Gd1 O4 77.92(18) . . ? O11 Gd1 N2 76.36(19) . . ? O11 Gd1 O10 72.47(18) . . ? O11 Gd1 N1 144.63(19) . . ? O11 Gd1 O17 87.69(18) . . ? O11 Gd1 O18 133.47(17) . . ? O11 Gd1 O28 140.26(18) . . ? O11 Gd1 O29 73.28(18) . . ? O11 Gd1 Na3 111.06(14) . . ? N1 Gd1 N2 68.3(2) . . ? N1 Gd1 Na3 100.25(14) . . ? O17 Gd1 O4 126.84(18) . . ? O17 Gd1 N2 64.32(18) . . ? O17 Gd1 O10 139.88(19) . . ? O17 Gd1 N1 77.2(2) . . ? O17 Gd1 O18 138.73(18) . . ? O17 Gd1 O28 76.84(19) . . ? O17 Gd1 O29 77.30(18) . . ? O17 Gd1 Na3 87.86(13) . . ? O18 Gd1 N2 115.57(19) . . ? O18 Gd1 O10 70.61(18) . . ? O18 Gd1 N1 66.49(19) . . ? O18 Gd1 O29 112.92(18) . . ? O18 Gd1 Na3 80.25(13) . . ? O28 Gd1 N2 125.63(19) . . ? O28 Gd1 O10 96.32(18) . . ? O28 Gd1 N1 67.09(19) . . ? O28 Gd1 O18 71.57(18) . . ? O28 Gd1 O29 67.72(18) . . ? O28 Gd1 Na3 33.45(14) . . ? O29 Gd1 N2 131.38(19) . . ? O29 Gd1 N1 131.85(18) . . ? O29 Gd1 Na3 38.88(14) . . ? C49 O4 Gd1 126.0(5) . . ? C34 N2 Gd1 110.0(5) . . ? C34 N2 C41 112.5(7) . . ? C34 N2 C42 110.0(7) . . ? C41 N2 Gd1 106.7(5) . . ? C41 N2 C42 108.3(6) . . ? C42 N2 Gd1 109.2(5) . . ? C27 O10 Gd1 116.3(4) . . ? C16 O11 Gd1 137.8(5) . . ? C38 O12 Na3 158.1(6) . . ? C22 N1 Gd1 109.9(5) . . ? C22 N1 C1 109.0(6) . . ? C37 N1 Gd1 106.6(5) . . ? C37 N1 C22 109.9(7) . . ? C37 N1 C1 109.4(7) . . ? C1 N1 Gd1 112.0(5) . . ? O11 C16 C32 119.8(7) . . ? O20 C16 O11 124.9(8) . . ? O20 C16 C32 115.3(7) . . ? C33 O17 Gd1 128.4(5) . . ? C25 O18 Gd1 124.0(6) . . ? N1 C22 C30 112.4(7) . . ? O5 C25 O18 126.7(8) . . ? O5 C25 C37 117.3(8) . . ? O18 C25 C37 116.0(8) . . ? O7 C26 C27 115.2(7) . . ? O7 C26 Na3 110.3(5) . . ? C27 C26 Na3 110.8(5) . . ? O29 C26 O7 125.9(7) . . ? O29 C26 C27 118.9(7) . . ? O29 C26 Na3 50.4(4) . . ? O10 C27 C26 105.9(6) . . ? O10 C27 C32 109.6(6) . . ? O10 C27 C39 109.9(7) . . ? C32 C27 C26 110.5(7) . . ? C32 C27 C39 110.9(7) . . ? C39 C27 C26 109.8(7) . . ? C30 O28 Gd1 124.2(5) . . ? C30 O28 Na3 122.3(5) . . ? Na3 O28 Gd1 111.4(2) . . ? Gd1 O29 Na3 103.3(2) . . ? C26 O29 Gd1 118.8(5) . . ? C26 O29 Na3 107.0(5) . . ? O15 C30 C22 117.9(8) . . ? O15 C30 O28 126.6(9) . . ? O28 C30 C22 115.3(8) . . ? C27 C32 C16 116.6(7) . . ? O13 C33 O17 124.5(7) . . ? O13 C33 C34 118.4(8) . . ? O17 C33 C34 117.0(7) . . ? N2 C34 C33 111.9(7) . . ? N1 C37 C25 113.6(7) . . ? O12 C38 O21 123.4(8) . . ? O12 C38 C39 122.8(8) . . ? O21 C38 C39 113.8(7) . . ? C38 C39 C27 113.4(7) . . ? N2 C41 C49 111.1(7) . . ? N2 C42 C1 113.4(7) . . ? O4 C49 C41 115.4(7) . . ? O8 C49 O4 124.9(8) . . ? O8 C49 C41 119.7(8) . . ? O12 Na3 Gd1 90.95(16) . . ? O12 Na3 C26 61.7(2) . . ? O12 Na3 O29 82.1(2) . . ? C26 Na3 Gd1 53.83(17) . . ? O28 Na3 Gd1 35.19(13) . . ? O28 Na3 O12 118.2(2) . . ? O28 Na3 C26 88.0(2) . . ? O28 Na3 O29 68.3(2) . . ? O28 Na3 O19 125.5(3) . . ? O28 Na3 O31 95.8(3) . . ? O29 Na3 Gd1 37.84(13) . . ? O29 Na3 C26 22.59(19) . . ? O19 Na3 Gd1 130.9(2) . . ? O19 Na3 O12 112.4(3) . . ? O19 Na3 C26 99.1(2) . . ? O19 Na3 O29 101.1(2) . . ? O19 Na3 O31 102.2(3) . . ? O31 Na3 Gd1 120.5(2) . . ? O31 Na3 O12 91.2(3) . . ? O31 Na3 C26 150.5(3) . . ? O31 Na3 O29 156.5(3) . . ? C42 C1 N1 112.2(7) . . ? _database_code_depnum_ccdc_archive 'CCDC 951556' ####################################################################### # # Cambridge Crystallographic Data Centre # CCDC # ####################################################################### # # This CIF contains data from an original supplementary publication # deposited with the CCDC, and may include chemical, crystal, # experimental, refinement, atomic coordinates, # anisotropic displacement parameters and molecular geometry data, # as required by the journal to which it was submitted. # # This CIF is provided on the understanding that it is used for bona # fide research purposes only. It may contain copyright material # of the CCDC or of third parties, and may not be copied or further # disseminated in any form, whether machine-readable or not, # except for the purpose of generating routine backup copies # on your local computer system. # # For further information on the CCDC, data deposition and # data retrieval see: # www.ccdc.cam.ac.uk # # Bona fide researchers may freely download Mercury and enCIFer # from this site to visualise CIF-encoded structures and # to carry out CIF format checking respectively. # data_a _audit_creation_date 2013-07-23 _audit_creation_method ; Olex2 1.1 (compiled 2011.11.01 svn.r2039, GUI svn.r3906) ; _chemical_name_common ? _chemical_name_systematic ; ? ; _chemical_formula_moiety 'C20 H33 Gd2 N4 Na8.5 O39 P2, 2(Cl), 3(O), 0.5(Cl O2)' _chemical_formula_sum 'C20 H33 Cl2.50 Gd2 N4 Na8.50 O43 P2' _chemical_formula_weight 1677.98 _chemical_melting_point ? 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' Cl Cl 0.1484 0.1585 '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' N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Na Na 0.0362 0.0249 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' P P 0.1023 0.0942 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _space_group_crystal_system triclinic _space_group_IT_number 2 _space_group_name_H-M_alt 'P -1' _space_group_name_Hall '-P 1' loop_ _space_group_symop_id _space_group_symop_operation_xyz 1 'x, y, z' 2 '-x, -y, -z' _cell_length_a 10.4283(9) _cell_length_b 16.3350(12) _cell_length_c 17.3916(12) _cell_angle_alpha 94.063(6) _cell_angle_beta 103.853(7) _cell_angle_gamma 93.889(6) _cell_volume 2858.2(4) _cell_formula_units_Z 2 _cell_measurement_reflns_used ? _cell_measurement_temperature 173(2) _cell_measurement_theta_max ? _cell_measurement_theta_min ? _exptl_absorpt_coefficient_mu 2.647 _exptl_absorpt_correction_T_max 0.7777 _exptl_absorpt_correction_T_min 0.6196 _exptl_absorpt_correction_type MULTI-SCAN _exptl_absorpt_process_details ? _exptl_crystal_colour ? _exptl_crystal_density_diffrn 1.950 _exptl_crystal_density_meas ? _exptl_crystal_density_method 'not measured' _exptl_crystal_description ? _exptl_crystal_F_000 1638 _exptl_crystal_size_max 0.20 _exptl_crystal_size_mid 0.10 _exptl_crystal_size_min 0.10 _exptl_special_details ; ? ; _diffrn_reflns_av_R_equivalents 0.0494 _diffrn_reflns_av_unetI/netI 0.0838 _diffrn_reflns_limit_h_max 12 _diffrn_reflns_limit_h_min -12 _diffrn_reflns_limit_k_max 19 _diffrn_reflns_limit_k_min -19 _diffrn_reflns_limit_l_max 21 _diffrn_reflns_limit_l_min -20 _diffrn_reflns_number 20606 _diffrn_reflns_theta_full 25.50 _diffrn_reflns_theta_max 25.50 _diffrn_reflns_theta_min 3.00 _diffrn_ambient_temperature 446(2) _diffrn_detector_area_resol_mean ? _diffrn_measured_fraction_theta_full 0.997 _diffrn_measured_fraction_theta_max 0.997 _diffrn_measurement_device_type ? _diffrn_measurement_method ? _diffrn_radiation_monochromator graphite _diffrn_radiation_type 'MO K\a' _diffrn_radiation_wavelength 0.71073 _diffrn_source 'fine-focus sealed tube' _diffrn_source_current n/a _diffrn_source_voltage n/a _diffrn_standards_decay_% ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_number ? _reflns_number_gt 7523 _reflns_number_total 10596 _reflns_threshold_expression >2sigma(I) _computing_cell_refinement ? _computing_data_collection ? _computing_data_reduction ? _computing_molecular_graphics ; O. V. Dolomanov, L. J. Bourhis, R. J. Gildea, J. A. K. Howard and H. Puschmann, OLEX2: a complete structure solution, refinement and analysis program. J. Appl. Cryst. (2009). 42, 339-341. ; _computing_publication_material ; O. V. Dolomanov, L. J. Bourhis, R. J. Gildea, J. A. K. Howard and H. Puschmann, OLEX2: a complete structure solution, refinement and analysis program. J. Appl. Cryst. (2009). 42, 339-341. ; _computing_structure_refinement ; XL, G.M. Sheldrick, Acta Cryst. (2008). A64, 112-122 ; _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _refine_diff_density_max 1.815 _refine_diff_density_min -1.468 _refine_diff_density_rms 0.166 _refine_ls_extinction_coef ? _refine_ls_extinction_method none _refine_ls_goodness_of_fit_ref 1.060 _refine_ls_hydrogen_treatment mixed _refine_ls_matrix_type full _refine_ls_number_parameters 780 _refine_ls_number_reflns 10596 _refine_ls_number_restraints 14 _refine_ls_R_factor_all 0.0790 _refine_ls_R_factor_gt 0.0518 _refine_ls_restrained_S_all 1.064 _refine_ls_shift/su_max 0.006 _refine_ls_shift/su_mean 0.000 _refine_ls_structure_factor_coef Fsqd _refine_ls_weighting_details 'calc w=1/[\s^2^(Fo^2^)+(0.0224P)^2^+10.8073P] where P=(Fo^2^+2Fc^2^)/3' _refine_ls_weighting_scheme calc _refine_ls_wR_factor_gt 0.1011 _refine_ls_wR_factor_ref 0.1142 _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. ; _atom_sites_solution_hydrogens geom _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap 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 -1.96162(3) -0.16809(2) -0.48366(2) 0.00955(10) Uani 1 1 d . . . Gd2 Gd -1.53549(3) 0.16504(2) -0.01881(2) 0.01321(11) Uani 1 1 d . . . Na1 Na -1.5888(4) -0.0464(2) -0.3222(3) 0.0430(10) Uani 1 1 d . . . Na2 Na -1.7695(3) 0.3945(2) 0.2375(2) 0.0373(9) Uani 1 1 d . . . Na3 Na -1.9338(3) 0.22047(18) 0.16483(18) 0.0174(7) Uani 1 1 d . . . Na4 Na -1.7281(3) -0.3902(2) -0.7459(2) 0.0334(9) Uani 1 1 d . . . Na5 Na -1.8746(3) -0.23459(19) -0.81478(18) 0.0224(7) Uani 1 1 d . . . Na6 Na -1.3574(3) -0.2291(2) -0.2977(2) 0.0298(8) Uani 1 1 d . . . Na7 Na -1.4178(3) 0.17953(18) -0.31041(18) 0.0201(7) Uani 1 1 d . . . Na8 Na -1.7242(3) -0.00673(18) -0.11458(18) 0.0190(7) Uani 1 1 d . . . Na9 Na -1.5000 0.0000 -0.5000 0.0212(10) Uani 1 2 d S . . P1 P -2.04106(18) 0.01436(11) -0.37446(12) 0.0117(4) Uani 1 1 d . . . H1 H -1.9708 0.0527 -0.3374 0.014 Uiso 1 1 calc R . . P2 P -1.6206(2) 0.00464(15) 0.09413(13) 0.0228(5) Uani 1 1 d . . . H2 H -1.7017 -0.0349 0.0770 0.027 Uiso 1 1 calc R A 1 Cl1 Cl -1.8629(3) 0.50411(16) -0.2294(2) 0.0763(12) Uani 1 1 d . . . Cl2 Cl -1.2828(3) 0.50630(17) 0.5026(2) 0.0626(9) Uani 1 1 d . . . N1 N -2.0404(5) -0.3020(4) -0.5794(4) 0.0119(13) Uani 1 1 d . . . N2 N -1.8975(5) -0.3008(4) -0.4120(3) 0.0096(13) Uani 1 1 d . . . N3 N -1.6185(6) 0.2970(4) -0.0843(4) 0.0148(14) Uani 1 1 d . . . N4 N -1.4322(5) 0.2955(4) 0.0750(4) 0.0149(14) Uani 1 1 d . . . O1 O -1.8090(5) -0.2165(3) -0.5606(3) 0.0152(11) Uani 1 1 d . . . O2 O -1.7849(5) -0.2630(3) -0.6797(3) 0.0187(12) Uani 1 1 d . . . O3 O -2.1774(5) -0.1683(3) -0.5754(3) 0.0156(11) Uani 1 1 d . . . O4 O -2.3662(5) -0.2347(3) -0.6466(3) 0.0253(14) Uani 1 1 d . . . O5 O -1.7484(4) -0.1566(3) -0.3968(3) 0.0155(11) Uani 1 1 d . . . O6 O -1.5749(5) -0.2051(3) -0.3174(3) 0.0218(13) Uani 1 1 d . . . O7 O -2.1225(4) -0.2303(3) -0.4174(3) 0.0139(11) Uani 1 1 d . . . O8 O -2.1476(5) -0.2776(3) -0.3039(3) 0.0174(12) Uani 1 1 d . . . O9 O -1.9755(5) -0.0641(3) -0.3897(3) 0.0153(11) Uani 1 1 d . . . O10 O -2.1504(5) -0.0010(3) -0.3313(3) 0.0215(13) Uani 1 1 d . . . O11 O -1.7214(5) 0.1418(3) -0.1283(3) 0.0184(12) Uani 1 1 d . . . O12 O -1.9260(5) 0.1747(3) -0.1781(3) 0.0251(13) Uani 1 1 d . . . O20 O -2.0860(4) 0.0583(3) -0.4501(3) 0.0166(12) Uani 1 1 d . . . O13 O -1.3810(5) 0.2315(3) -0.0788(3) 0.0196(12) Uani 1 1 d . . . O14 O -1.3533(5) 0.2836(3) -0.1890(3) 0.0241(13) Uani 1 1 d . . . O15 O -1.3507(5) 0.1423(3) 0.0839(3) 0.0175(12) Uani 1 1 d . . . O16 O -1.1541(5) 0.1848(3) 0.1633(3) 0.0202(12) Uani 1 1 d . . . O17 O -1.6828(5) 0.2181(3) 0.0532(3) 0.0182(12) Uani 1 1 d . . . O18 O -1.7121(5) 0.2757(3) 0.1670(3) 0.0213(13) Uani 1 1 d . . . O19 O -1.6358(5) 0.0501(3) 0.0206(3) 0.0183(12) Uani 1 1 d . . . O21 O -1.5157(5) -0.0560(3) 0.1003(3) 0.0190(12) Uani 1 1 d . . . O22 O -1.6316(12) 0.0312(7) 0.1722(7) 0.023(4) Uani 0.454(13) 1 d PU . 1 C1 C -1.9974(7) -0.2864(4) -0.6516(4) 0.0136(16) Uani 1 1 d . . . H1A H -2.0521 -0.2458 -0.6807 0.016 Uiso 1 1 calc R . . H1B H -2.0090 -0.3381 -0.6868 0.016 Uiso 1 1 calc R . . C2 C -1.8521(7) -0.2531(4) -0.6291(5) 0.0138(16) Uani 1 1 d . . . C3 C -2.1858(7) -0.3154(4) -0.5981(4) 0.0139(16) Uani 1 1 d . . . H3A H -2.2131 -0.3425 -0.5547 0.017 Uiso 1 1 calc R . . H3B H -2.2178 -0.3523 -0.6477 0.017 Uiso 1 1 calc R . . C4 C -2.2484(7) -0.2335(4) -0.6084(4) 0.0141(16) Uani 1 1 d . . . C5 C -1.7516(7) -0.3023(4) -0.3924(5) 0.0158(17) Uani 1 1 d . . . H5A H -1.7237 -0.3247 -0.4396 0.019 Uiso 1 1 calc R . . H5B H -1.7237 -0.3385 -0.3492 0.019 Uiso 1 1 calc R . . C6 C -1.6851(7) -0.2148(5) -0.3659(4) 0.0126(16) Uani 1 1 d . . . C7 C -1.9417(7) -0.2907(5) -0.3381(4) 0.0145(16) Uani 1 1 d . . . H7A H -1.8808 -0.2487 -0.3005 0.017 Uiso 1 1 calc R . . H7B H -1.9385 -0.3434 -0.3132 0.017 Uiso 1 1 calc R . . C8 C -2.0818(7) -0.2644(5) -0.3536(5) 0.0186(18) Uani 1 1 d . . . C9 C -1.9767(7) -0.3753(4) -0.5458(4) 0.0152(16) Uani 1 1 d . . . H9A H -1.8865 -0.3750 -0.5548 0.018 Uiso 1 1 calc R . . H9B H -2.0286 -0.4261 -0.5744 0.018 Uiso 1 1 calc R . . C10 C -1.9675(7) -0.3771(4) -0.4583(4) 0.0127(16) Uani 1 1 d . . . H10A H -2.0579 -0.3844 -0.4498 0.015 Uiso 1 1 calc R . . H10B H -1.9199 -0.4249 -0.4388 0.015 Uiso 1 1 calc R . . C11 C -1.7625(7) 0.2839(5) -0.1167(5) 0.0183(18) Uani 1 1 d . . . H11A H -1.7886 0.3177 -0.1620 0.022 Uiso 1 1 calc R . . H11B H -1.8075 0.3024 -0.0754 0.022 Uiso 1 1 calc R . . C12 C -1.8080(7) 0.1937(5) -0.1446(4) 0.0154(17) Uani 1 1 d . . . C13 C -1.5519(7) 0.3067(5) -0.1508(5) 0.0190(18) Uani 1 1 d . . . H13A H -1.5402 0.3662 -0.1578 0.023 Uiso 1 1 calc R . . H13B H -1.6113 0.2795 -0.2004 0.023 Uiso 1 1 calc R . . C14 C -1.4182(7) 0.2721(4) -0.1394(5) 0.0157(17) Uani 1 1 d . . . C15 C -1.2906(7) 0.2870(5) 0.1078(5) 0.0169(17) Uani 1 1 d . . . H15A H -1.2602 0.3210 0.1593 0.020 Uiso 1 1 calc R . . H15B H -1.2396 0.3082 0.0711 0.020 Uiso 1 1 calc R . . C16 C -1.2618(7) 0.1971(5) 0.1205(5) 0.0164(17) Uani 1 1 d . . . C17 C -1.5000(7) 0.2999(5) 0.1410(5) 0.0181(17) Uani 1 1 d . . . H17A H -1.4978 0.3583 0.1610 0.022 Uiso 1 1 calc R . . H17B H -1.4496 0.2708 0.1851 0.022 Uiso 1 1 calc R . . C18 C -1.6440(7) 0.2627(4) 0.1185(5) 0.0172(17) Uani 1 1 d . . . C19 C -1.5863(7) 0.3697(5) -0.0243(5) 0.0174(17) Uani 1 1 d . . . H19A H -1.6532 0.3695 0.0076 0.021 Uiso 1 1 calc R . . H19B H -1.5916 0.4206 -0.0522 0.021 Uiso 1 1 calc R . . C20 C -1.4482(7) 0.3707(4) 0.0315(5) 0.0169(17) Uani 1 1 d . . . H20A H -1.3807 0.3751 0.0001 0.020 Uiso 1 1 calc R . . H20B H -1.4327 0.4198 0.0703 0.020 Uiso 1 1 calc R . . O1W O -1.4325(5) 0.1380(3) -0.4452(3) 0.0230(13) Uani 1 1 d . . . O2W O -1.7553(5) -0.1066(3) -0.7637(3) 0.0217(13) Uani 1 1 d . . . O3W O -1.7679(5) -0.0592(3) -0.2505(3) 0.0216(12) Uani 1 1 d . . . O4W O -1.6881(5) 0.0243(3) -0.4423(3) 0.0249(13) Uani 1 1 d . . . O5W O -1.5593(5) 0.0925(3) -0.2568(3) 0.0207(12) Uani 1 1 d . . . O6W O -1.6762(8) 0.4972(4) 0.1675(8) 0.110(4) Uani 1 1 d U . . O7W O -1.8317(6) 0.5044(3) 0.3155(4) 0.0379(17) Uani 1 1 d . . . O8W O -1.9754(6) 0.3684(4) 0.1436(4) 0.0346(15) Uani 1 1 d . . . O9W O -1.8190(5) 0.1083(3) 0.2224(3) 0.0243(13) Uani 1 1 d . . . O10W O -1.9435(5) 0.1431(3) 0.0377(3) 0.0269(14) Uani 1 1 d . . . O11W O -1.5745(6) 0.3801(4) 0.3299(5) 0.064(2) Uani 1 1 d . . . O12W O -1.3850(5) -0.2232(4) -0.4426(3) 0.0274(14) Uani 1 1 d . . . H12A H -1.4071 -0.2726 -0.4666 0.041 Uiso 1 1 d R . . H12B H -1.4472 -0.1913 -0.4605 0.041 Uiso 1 1 d R . . O13W O -1.9427(6) -0.3819(4) -0.8347(4) 0.0346(15) Uani 1 1 d . . . O14W O -1.8942(6) -0.2527(5) -0.9558(4) 0.0454(18) Uani 1 1 d . . . H14W H -1.9426 -0.2142 -0.9810 0.068 Uiso 1 1 d R . . O15W O -1.5146(7) -0.3832(5) -0.6634(5) 0.061(2) Uani 1 1 d D . . H15W H -1.4598 -0.3307 -0.6604 0.091 Uiso 1 1 d RD . . O16W O -1.4063(5) -0.0598(3) -0.3795(3) 0.0246(13) Uani 1 1 d . . . O17W O -1.9526(5) 0.0122(3) -0.1251(4) 0.0291(14) Uani 1 1 d . . . H17C H -2.0002 -0.0349 -0.1414 0.044 Uiso 1 1 d R . . H17D H -1.9632 0.0297 -0.0784 0.044 Uiso 1 1 d R . . O18W O -1.5056(9) 0.3808(5) 0.4996(6) 0.088(3) Uani 1 1 d . . . O20W O -1.9484(6) -0.0070(4) 0.0215(4) 0.0428(18) Uani 1 1 d . . . O22A O -1.7456(9) -0.0099(6) 0.1171(6) 0.017(3) Uani 0.546(13) 1 d PU . 2 Cl3 Cl -1.8415(8) 0.5066(4) 0.0058(4) 0.083(2) Uani 0.50 1 d P . . O1C O -1.5793(12) -0.4904(8) -0.2567(8) 0.047(3) Uani 0.65 1 d P . . O1E O -1.633(2) -0.4840(14) -0.3078(17) 0.053(7) Uani 0.35 1 d P . . H4 H -1.536(10) -0.374(5) -0.619(3) 0.063 Uiso 1 1 d D . . O1A O -1.9041(19) 0.5765(8) 0.0100(8) 0.058(5) Uani 0.50 1 d P . . O1B O -1.959(3) 0.4292(10) -0.0031(10) 0.101(8) 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 Gd1 0.00855(19) 0.00912(19) 0.0113(2) 0.00068(15) 0.00330(15) 0.00024(13) Gd2 0.0116(2) 0.0109(2) 0.0157(2) 0.00145(16) 0.00068(16) 0.00071(14) Na1 0.049(2) 0.0200(19) 0.072(3) -0.0098(18) 0.045(2) -0.0084(16) Na2 0.0260(19) 0.024(2) 0.065(3) -0.0065(18) 0.0188(18) 0.0023(15) Na3 0.0131(15) 0.0203(17) 0.0193(17) 0.0024(13) 0.0047(13) 0.0010(12) Na4 0.0225(18) 0.0192(18) 0.063(3) 0.0028(17) 0.0204(18) 0.0011(14) Na5 0.0164(16) 0.0282(19) 0.0204(18) -0.0028(14) 0.0010(13) 0.0045(13) Na6 0.0163(17) 0.052(2) 0.025(2) 0.0100(17) 0.0074(14) 0.0109(15) Na7 0.0209(17) 0.0230(18) 0.0173(17) 0.0025(14) 0.0061(13) 0.0009(13) Na8 0.0204(17) 0.0202(17) 0.0150(17) 0.0012(13) 0.0014(13) 0.0031(13) Na9 0.021(2) 0.022(2) 0.021(3) 0.003(2) 0.0068(19) 0.0014(18) P1 0.0127(10) 0.0102(10) 0.0129(10) -0.0008(8) 0.0053(8) -0.0003(7) P2 0.0202(12) 0.0396(14) 0.0151(12) 0.0103(10) 0.0109(9) 0.0155(10) Cl1 0.0371(16) 0.0314(15) 0.169(4) -0.0134(18) 0.051(2) -0.0056(12) Cl2 0.0497(17) 0.0459(17) 0.098(3) 0.0151(17) 0.0283(17) -0.0037(13) N1 0.008(3) 0.014(3) 0.017(4) 0.001(3) 0.008(3) 0.003(2) N2 0.006(3) 0.016(3) 0.008(3) 0.003(3) 0.002(2) 0.003(2) N3 0.014(3) 0.014(3) 0.018(4) -0.001(3) 0.006(3) -0.001(3) N4 0.010(3) 0.017(4) 0.020(4) 0.001(3) 0.007(3) 0.004(3) O1 0.013(3) 0.014(3) 0.018(3) -0.007(2) 0.007(2) -0.006(2) O2 0.014(3) 0.019(3) 0.025(3) -0.002(2) 0.011(2) -0.004(2) O3 0.017(3) 0.015(3) 0.014(3) -0.001(2) 0.003(2) 0.001(2) O4 0.012(3) 0.025(3) 0.032(4) -0.004(3) -0.007(3) 0.001(2) O5 0.011(3) 0.017(3) 0.017(3) 0.002(2) 0.001(2) 0.002(2) O6 0.011(3) 0.029(3) 0.023(3) 0.000(3) -0.001(2) 0.001(2) O7 0.011(3) 0.020(3) 0.013(3) 0.006(2) 0.005(2) 0.003(2) O8 0.015(3) 0.020(3) 0.019(3) 0.003(2) 0.009(2) -0.002(2) O9 0.020(3) 0.017(3) 0.013(3) 0.001(2) 0.009(2) 0.005(2) O10 0.028(3) 0.020(3) 0.022(3) 0.003(2) 0.017(3) 0.004(2) O11 0.014(3) 0.022(3) 0.019(3) 0.002(2) 0.002(2) 0.005(2) O12 0.012(3) 0.032(4) 0.027(3) -0.001(3) -0.002(2) 0.002(2) O20 0.011(3) 0.023(3) 0.016(3) 0.006(2) 0.002(2) 0.000(2) O13 0.018(3) 0.018(3) 0.027(3) 0.007(3) 0.011(2) 0.007(2) O14 0.024(3) 0.028(3) 0.024(3) -0.004(3) 0.016(3) -0.003(2) O15 0.018(3) 0.016(3) 0.017(3) 0.001(2) -0.001(2) 0.002(2) O16 0.015(3) 0.024(3) 0.018(3) 0.007(2) -0.004(2) -0.001(2) O17 0.019(3) 0.017(3) 0.018(3) -0.001(2) 0.006(2) -0.005(2) O18 0.023(3) 0.017(3) 0.029(3) -0.003(2) 0.018(3) 0.002(2) O19 0.019(3) 0.014(3) 0.017(3) 0.007(2) -0.004(2) 0.000(2) O21 0.022(3) 0.015(3) 0.019(3) 0.001(2) 0.001(2) 0.005(2) O22 0.037(9) 0.028(8) 0.009(7) 0.007(5) 0.011(6) 0.021(6) C1 0.012(4) 0.014(4) 0.015(4) 0.000(3) 0.004(3) 0.000(3) C2 0.012(4) 0.014(4) 0.015(4) 0.000(3) 0.002(3) 0.003(3) C3 0.013(4) 0.013(4) 0.013(4) -0.001(3) 0.000(3) 0.000(3) C4 0.019(4) 0.012(4) 0.010(4) 0.001(3) 0.003(3) -0.001(3) C5 0.016(4) 0.015(4) 0.015(4) -0.004(3) 0.003(3) 0.002(3) C6 0.016(4) 0.017(4) 0.006(4) 0.000(3) 0.006(3) 0.001(3) C7 0.017(4) 0.015(4) 0.014(4) 0.006(3) 0.007(3) 0.000(3) C8 0.012(4) 0.019(4) 0.022(5) -0.010(4) 0.004(3) -0.005(3) C9 0.017(4) 0.009(4) 0.022(4) 0.002(3) 0.009(3) 0.002(3) C10 0.006(4) 0.012(4) 0.020(4) -0.003(3) 0.006(3) -0.005(3) C11 0.013(4) 0.024(5) 0.021(5) 0.007(4) 0.006(3) 0.011(3) C12 0.020(4) 0.016(4) 0.012(4) 0.002(3) 0.005(3) 0.003(3) C13 0.017(4) 0.021(4) 0.023(5) 0.007(4) 0.011(3) 0.004(3) C14 0.021(4) 0.010(4) 0.016(4) -0.003(3) 0.006(3) -0.002(3) C15 0.017(4) 0.018(4) 0.016(4) -0.002(3) 0.006(3) -0.004(3) C16 0.021(5) 0.019(4) 0.013(4) -0.003(3) 0.014(4) -0.001(3) C17 0.020(4) 0.018(4) 0.017(4) -0.006(3) 0.009(3) -0.003(3) C18 0.020(4) 0.009(4) 0.024(5) 0.007(3) 0.005(4) 0.006(3) C19 0.017(4) 0.015(4) 0.023(5) 0.000(3) 0.011(3) 0.000(3) C20 0.018(4) 0.012(4) 0.021(4) -0.001(3) 0.008(3) -0.005(3) O1W 0.021(3) 0.025(3) 0.021(3) -0.002(3) 0.005(2) -0.006(2) O2W 0.024(3) 0.018(3) 0.028(3) 0.009(3) 0.012(3) 0.006(2) O3W 0.023(3) 0.026(3) 0.014(3) -0.006(2) 0.005(2) 0.002(2) O4W 0.021(3) 0.018(3) 0.035(4) 0.003(3) 0.007(3) 0.000(2) O5W 0.020(3) 0.024(3) 0.018(3) 0.004(2) 0.004(2) 0.001(2) O6W 0.071(6) 0.022(4) 0.259(12) -0.016(6) 0.095(7) 0.001(4) O7W 0.040(4) 0.018(3) 0.065(5) -0.003(3) 0.031(3) 0.003(3) O8W 0.036(4) 0.022(3) 0.042(4) 0.005(3) 0.003(3) 0.002(3) O9W 0.033(3) 0.026(3) 0.021(3) 0.012(3) 0.015(3) 0.017(3) O10W 0.031(3) 0.025(3) 0.024(3) 0.000(3) 0.008(3) -0.002(3) O11W 0.038(4) 0.035(4) 0.112(7) 0.011(4) 0.004(4) -0.007(3) O12W 0.024(3) 0.031(4) 0.030(4) 0.011(3) 0.006(3) 0.011(3) O13W 0.034(4) 0.035(4) 0.032(4) -0.007(3) 0.008(3) -0.005(3) O14W 0.042(4) 0.064(5) 0.032(4) 0.002(4) 0.008(3) 0.026(3) O15W 0.041(4) 0.045(5) 0.092(7) 0.012(4) 0.009(4) -0.005(3) O16W 0.021(3) 0.034(4) 0.017(3) 0.004(3) 0.003(2) -0.001(2) O17W 0.016(3) 0.025(3) 0.042(4) -0.015(3) 0.003(3) -0.002(2) O18W 0.101(7) 0.065(6) 0.100(8) -0.027(5) 0.045(6) -0.018(5) O20W 0.038(4) 0.052(5) 0.039(5) 0.008(4) 0.007(3) 0.008(4) O22A 0.017(6) 0.024(6) 0.019(6) 0.010(5) 0.015(5) 0.011(4) Cl3 0.149(7) 0.041(4) 0.071(5) 0.008(3) 0.048(5) 0.021(4) O1C 0.040(8) 0.043(7) 0.055(9) -0.003(7) 0.011(6) -0.004(6) O1E 0.023(13) 0.033(12) 0.11(2) 0.018(15) 0.019(13) 0.005(10) O1A 0.120(14) 0.029(8) 0.024(8) -0.015(6) 0.038(9) -0.048(9) O1B 0.22(2) 0.024(9) 0.057(13) 0.001(8) 0.038(14) -0.027(12) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag Gd1 N1 2.611(6) . ? Gd1 N2 2.622(6) . ? Gd1 O1 2.447(5) . ? Gd1 O3 2.427(5) . ? Gd1 O5 2.358(5) . ? Gd1 O7 2.457(4) . ? Gd1 O9 2.309(5) . ? Gd1 O20 2.289(5) 2_154 ? Gd2 N3 2.611(6) . ? Gd2 N4 2.592(6) . ? Gd2 O11 2.358(5) . ? Gd2 O13 2.365(5) . ? Gd2 O15 2.363(5) . ? Gd2 O17 2.372(5) . ? Gd2 O19 2.312(5) . ? Gd2 O21 2.366(5) 2_255 ? Na1 O5 2.434(6) . ? Na1 O6 2.614(6) . ? Na1 O22 3.019(13) 2_255 ? Na1 C6 2.850(8) . ? Na1 O3W 2.487(6) . ? Na1 O4W 2.496(7) . ? Na1 O5W 2.430(6) . ? Na1 O16W 2.366(6) . ? Na2 O8 2.510(6) 2_155 ? Na2 O18 2.409(6) . ? Na2 O6W 2.424(10) . ? Na2 O7W 2.390(7) . ? Na2 O8W 2.357(7) . ? Na2 O11W 2.309(8) . ? Na3 O8 2.456(6) 2_155 ? Na3 O16 2.325(5) 1_455 ? Na3 O18 2.415(5) . ? Na3 O8W 2.520(6) . ? Na3 O9W 2.404(6) . ? Na3 O10W 2.444(6) . ? Na4 O2 2.480(6) . ? Na4 O14 2.361(6) 2_254 ? Na4 O6W 2.465(9) 1_544 ? Na4 O7W 2.416(7) 1_544 ? Na4 O13W 2.413(7) . ? Na4 O15W 2.333(8) . ? Na5 O2 2.402(6) . ? Na5 O12 2.338(6) 2_154 ? Na5 O14 2.546(6) 2_254 ? Na5 O2W 2.358(6) . ? Na5 O13W 2.439(7) . ? Na5 O14W 2.407(7) . ? Na6 O6 2.277(6) . ? Na6 O8 2.400(6) 1_655 ? Na6 O18 2.408(6) 2_255 ? Na6 O9W 2.642(7) 2_255 ? Na6 O11W 2.505(8) 2_255 ? Na6 O12W 2.478(6) . ? Na7 O2 2.484(5) 2_254 ? Na7 O4 2.451(6) 2_154 ? Na7 O14 2.541(6) . ? Na7 O1W 2.359(6) . ? Na7 O2W 2.394(6) 2_254 ? Na7 O5W 2.373(6) . ? Na8 O11 2.453(6) . ? Na8 O15 2.449(6) 2_255 ? Na8 O19 2.403(6) . ? Na8 O21 2.587(6) 2_255 ? Na8 C16 3.097(8) 2_255 ? Na8 O3W 2.382(6) . ? Na8 O17W 2.388(6) . ? Na9 O1W 2.377(5) 2_254 ? Na9 O1W 2.377(5) . ? Na9 O4W 2.451(5) . ? Na9 O4W 2.451(5) 2_254 ? Na9 O16W 2.396(5) 2_254 ? Na9 O16W 2.396(5) . ? P1 O9 1.529(5) . ? P1 O10 1.524(5) . ? P1 O20 1.532(5) . ? P2 O19 1.506(5) . ? P2 O21 1.515(5) . ? P2 O22 1.429(11) . ? P2 O22A 1.461(8) . ? N1 C1 1.465(9) . ? N1 C3 1.470(8) . ? N1 C9 1.496(9) . ? N2 C5 1.480(8) . ? N2 C7 1.469(9) . ? N2 C10 1.480(9) . ? N3 C11 1.467(9) . ? N3 C13 1.496(9) . ? N3 C19 1.488(9) . ? N4 C15 1.469(9) . ? N4 C17 1.486(9) . ? N4 C20 1.486(9) . ? O1 C2 1.259(9) . ? O2 Na7 2.484(5) 2_254 ? O2 C2 1.258(8) . ? O3 C4 1.271(8) . ? O4 Na7 2.451(6) 2_154 ? O4 C4 1.247(8) . ? O5 C6 1.271(8) . ? O6 C6 1.244(8) . ? O7 C8 1.271(9) . ? O8 Na2 2.510(6) 2_155 ? O8 Na3 2.456(6) 2_155 ? O8 Na6 2.400(6) 1_455 ? O8 C8 1.247(9) . ? O11 C12 1.276(8) . ? O12 Na5 2.338(6) 2_154 ? O12 C12 1.237(8) . ? O20 Gd1 2.289(5) 2_154 ? O13 C14 1.280(9) . ? O14 Na4 2.361(6) 2_254 ? O14 Na5 2.546(6) 2_254 ? O14 C14 1.233(8) . ? O15 Na8 2.449(6) 2_255 ? O15 C16 1.262(9) . ? O16 Na3 2.325(5) 1_655 ? O16 C16 1.228(9) . ? O17 C18 1.268(9) . ? O18 Na6 2.408(6) 2_255 ? O18 C18 1.243(9) . ? O21 Gd2 2.366(5) 2_255 ? O21 Na8 2.587(6) 2_255 ? O22 Na1 3.019(13) 2_255 ? C1 C2 1.523(10) . ? C3 C4 1.530(10) . ? C5 C6 1.534(10) . ? C7 C8 1.518(10) . ? C9 C10 1.503(10) . ? C11 C12 1.525(10) . ? C13 C14 1.515(10) . ? C15 C16 1.540(10) . ? C16 Na8 3.097(8) 2_255 ? C17 C18 1.529(10) . ? C19 C20 1.530(10) . ? O2W Na7 2.394(6) 2_254 ? O6W Na4 2.465(9) 1_566 ? O7W Na4 2.416(7) 1_566 ? O9W Na6 2.642(7) 2_255 ? O11W Na6 2.505(8) 2_255 ? O20W O20W 1.202(11) 2_155 ? Cl3 O1A 1.358(18) . ? Cl3 O1B 1.67(2) . ? O1C O1E 0.95(2) . ? O1A O1B 1.40(3) 2_165 ? O1B O1A 1.40(3) 2_165 ? 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 N1 Gd1 N2 68.17(18) . . ? O1 Gd1 N1 62.90(16) . . ? O1 Gd1 N2 81.18(17) . . ? O1 Gd1 O7 137.00(16) . . ? O3 Gd1 N1 64.57(17) . . ? O3 Gd1 N2 119.48(17) . . ? O3 Gd1 O1 107.32(16) . . ? O3 Gd1 O7 73.92(16) . . ? O5 Gd1 N1 118.87(17) . . ? O5 Gd1 N2 65.21(17) . . ? O5 Gd1 O1 72.79(17) . . ? O5 Gd1 O3 175.31(16) . . ? O5 Gd1 O7 109.32(16) . . ? O7 Gd1 N1 81.07(17) . . ? O7 Gd1 N2 63.25(16) . . ? O9 Gd1 N1 156.46(17) . . ? O9 Gd1 N2 108.86(18) . . ? O9 Gd1 O1 140.63(16) . . ? O9 Gd1 O3 100.39(17) . . ? O9 Gd1 O5 77.37(17) . . ? O9 Gd1 O7 77.18(17) . . ? O20 Gd1 N1 111.99(18) 2_154 . ? O20 Gd1 N2 152.00(16) 2_154 . ? O20 Gd1 O1 75.00(17) 2_154 . ? O20 Gd1 O3 82.14(16) 2_154 . ? O20 Gd1 O5 93.42(17) 2_154 . ? O20 Gd1 O7 144.44(16) 2_154 . ? O20 Gd1 O9 81.84(18) 2_154 . ? N3 Gd2 Na8 110.99(14) . . ? N4 Gd2 Na8 166.28(13) . . ? N4 Gd2 N3 69.92(19) . . ? O11 Gd2 Na8 46.23(13) . . ? O11 Gd2 N3 64.76(18) . . ? O11 Gd2 N4 132.35(18) . . ? O11 Gd2 O13 100.31(18) . . ? O11 Gd2 O15 161.68(18) . . ? O11 Gd2 O17 86.18(17) . . ? O11 Gd2 O21 75.18(17) . 2_255 ? O13 Gd2 Na8 119.49(14) . . ? O13 Gd2 N3 66.81(17) . . ? O13 Gd2 N4 73.85(18) . . ? O13 Gd2 O17 131.57(17) . . ? O13 Gd2 O21 77.40(18) . 2_255 ? O15 Gd2 Na8 115.73(13) . . ? O15 Gd2 N3 133.07(18) . . ? O15 Gd2 N4 65.85(18) . . ? O15 Gd2 O13 86.28(17) . . ? O15 Gd2 O17 102.31(18) . . ? O15 Gd2 O21 89.82(17) . 2_255 ? O17 Gd2 Na8 99.59(13) . . ? O17 Gd2 N3 73.43(18) . . ? O17 Gd2 N4 67.21(17) . . ? O19 Gd2 Na8 44.98(14) . . ? O19 Gd2 N3 135.09(17) . . ? O19 Gd2 N4 124.29(19) . . ? O19 Gd2 O11 81.86(17) . . ? O19 Gd2 O13 153.02(18) . . ? O19 Gd2 O15 84.63(17) . . ? O19 Gd2 O17 75.29(18) . . ? O19 Gd2 O21 77.23(18) . 2_255 ? O21 Gd2 Na8 49.47(13) 2_255 . ? O21 Gd2 N3 118.43(18) 2_255 . ? O21 Gd2 N4 143.07(17) 2_255 . ? O21 Gd2 O17 148.62(17) 2_255 . ? Na6 Na1 Na7 117.60(11) . . ? Na6 Na1 Na8 108.93(11) . . ? Na7 Na1 Na8 95.30(10) . . ? Na9 Na1 Na6 91.10(9) . . ? Na9 Na1 Na7 66.69(7) . . ? Na9 Na1 Na8 158.08(11) . . ? O5 Na1 Na6 81.23(15) . . ? O5 Na1 Na7 148.9(2) . . ? O5 Na1 Na8 101.68(15) . . ? O5 Na1 Na9 89.80(17) . . ? O5 Na1 O6 52.21(17) . . ? O5 Na1 O22 135.5(3) . 2_255 ? O5 Na1 C6 26.36(18) . . ? O5 Na1 O3W 73.93(19) . . ? O5 Na1 O4W 80.2(2) . . ? O6 Na1 Na6 33.39(12) . . ? O6 Na1 Na7 150.99(17) . . ? O6 Na1 Na8 96.63(16) . . ? O6 Na1 Na9 105.13(16) . . ? O6 Na1 O22 85.3(3) . 2_255 ? O6 Na1 C6 25.87(18) . . ? O22 Na1 Na6 64.4(2) 2_255 . ? O22 Na1 Na7 75.3(2) 2_255 . ? O22 Na1 Na8 66.9(2) 2_255 . ? O22 Na1 Na9 116.9(2) 2_255 . ? C6 Na1 Na6 56.69(17) . . ? C6 Na1 Na7 165.22(19) . . ? C6 Na1 Na8 99.46(17) . . ? C6 Na1 Na9 98.99(17) . . ? C6 Na1 O22 110.1(3) . 2_255 ? O3W Na1 Na6 113.72(17) . . ? O3W Na1 Na7 114.74(17) . . ? O3W Na1 Na8 29.55(13) . . ? O3W Na1 Na9 147.0(2) . . ? O3W Na1 O6 87.54(19) . . ? O3W Na1 O22 94.0(3) . 2_255 ? O3W Na1 C6 79.1(2) . . ? O3W Na1 O4W 104.3(2) . . ? O4W Na1 Na6 130.52(18) . . ? O4W Na1 Na7 68.78(15) . . ? O4W Na1 Na8 119.56(17) . . ? O4W Na1 Na9 43.66(13) . . ? O4W Na1 O6 125.8(2) . . ? O4W Na1 O22 143.8(3) . 2_255 ? O4W Na1 C6 103.9(2) . . ? O5W Na1 Na6 131.60(19) . . ? O5W Na1 Na7 34.05(13) . . ? O5W Na1 Na8 61.78(15) . . ? O5W Na1 Na9 98.41(16) . . ? O5W Na1 O5 145.5(2) . . ? O5W Na1 O6 151.1(3) . . ? O5W Na1 O22 69.1(3) . 2_255 ? O5W Na1 C6 160.5(2) . . ? O5W Na1 O3W 81.5(2) . . ? O5W Na1 O4W 83.0(2) . . ? O16W Na1 Na6 54.52(15) . . ? O16W Na1 Na7 74.36(16) . . ? O16W Na1 Na8 147.7(2) . . ? O16W Na1 Na9 42.13(14) . . ? O16W Na1 O5 102.3(2) . . ? O16W Na1 O6 81.5(2) . . ? O16W Na1 O22 80.8(3) . 2_255 ? O16W Na1 C6 92.6(2) . . ? O16W Na1 O3W 168.2(3) . . ? O16W Na1 O4W 85.7(2) . . ? O16W Na1 O5W 106.2(2) . . ? Na3 Na2 Na4 152.32(14) . 1_566 ? Na6 Na2 Na3 62.28(10) 2_255 . ? Na6 Na2 Na4 145.40(14) 2_255 1_566 ? O8 Na2 Na3 48.75(14) 2_155 . ? O8 Na2 Na4 140.85(19) 2_155 1_566 ? O8 Na2 Na6 47.54(14) 2_155 2_255 ? O18 Na2 Na3 48.10(14) . . ? O18 Na2 Na4 141.34(19) . 1_566 ? O18 Na2 Na6 48.03(16) . 2_255 ? O18 Na2 O8 77.45(19) . 2_155 ? O18 Na2 O6W 96.7(3) . . ? O6W Na2 Na3 128.0(3) . . ? O6W Na2 Na4 44.8(2) . 1_566 ? O6W Na2 Na6 127.1(2) . 2_255 ? O6W Na2 O8 173.9(3) . 2_155 ? O7W Na2 Na3 128.76(19) . . ? O7W Na2 Na4 43.60(16) . 1_566 ? O7W Na2 Na6 127.7(2) . 2_255 ? O7W Na2 O8 97.5(2) . 2_155 ? O7W Na2 O18 174.9(3) . . ? O7W Na2 O6W 88.3(3) . . ? O8W Na2 Na3 50.80(16) . . ? O8W Na2 Na4 101.52(19) . 1_566 ? O8W Na2 Na6 113.08(19) . 2_255 ? O8W Na2 O8 84.7(2) . 2_155 ? O8W Na2 O18 83.7(2) . . ? O8W Na2 O6W 96.4(3) . . ? O8W Na2 O7W 96.7(2) . . ? O11W Na2 Na3 112.9(2) . . ? O11W Na2 Na4 94.8(2) . 1_566 ? O11W Na2 Na6 50.65(19) . 2_255 ? O11W Na2 O8 82.0(2) . 2_155 ? O11W Na2 O18 84.3(3) . . ? O11W Na2 O6W 96.0(3) . . ? O11W Na2 O7W 94.3(3) . . ? O11W Na2 O8W 163.7(3) . . ? Na2 Na3 Na6 58.78(10) . 2_255 ? O8 Na3 Na2 50.22(14) 2_155 . ? O8 Na3 Na6 45.94(13) 2_155 2_255 ? O8 Na3 O8W 82.4(2) 2_155 . ? O16 Na3 Na2 125.45(18) 1_455 . ? O16 Na3 Na6 136.16(18) 1_455 2_255 ? O16 Na3 O8 99.5(2) 1_455 2_155 ? O16 Na3 O18 172.6(2) 1_455 . ? O16 Na3 O8W 92.5(2) 1_455 . ? O16 Na3 O9W 104.0(2) 1_455 . ? O16 Na3 O10W 94.9(2) 1_455 . ? O18 Na3 Na2 47.94(14) . . ? O18 Na3 Na6 46.19(15) . 2_255 ? O18 Na3 O8 78.38(19) . 2_155 ? O18 Na3 O8W 80.2(2) . . ? O18 Na3 O10W 88.9(2) . . ? O8W Na3 Na2 46.44(16) . . ? O8W Na3 Na6 105.21(17) . 2_255 ? O9W Na3 Na2 110.57(18) . . ? O9W Na3 Na6 51.81(16) . 2_255 ? O9W Na3 O8 79.2(2) . 2_155 ? O9W Na3 O18 82.65(19) . . ? O9W Na3 O8W 157.0(2) . . ? O9W Na3 O10W 84.8(2) . . ? O10W Na3 Na2 128.38(17) . . ? O10W Na3 Na6 114.98(17) . 2_255 ? O10W Na3 O8 160.6(2) . 2_155 ? O10W Na3 O8W 110.0(2) . . ? Na2 Na4 Na7 161.54(13) 1_544 2_254 ? Na5 Na4 Na2 140.78(14) . 1_544 ? Na5 Na4 Na7 57.60(9) . 2_254 ? O2 Na4 Na2 144.46(17) . 1_544 ? O2 Na4 Na5 47.84(15) . . ? O2 Na4 Na7 42.97(13) . 2_254 ? O14 Na4 Na2 138.8(2) 2_254 1_544 ? O14 Na4 Na5 51.68(15) 2_254 . ? O14 Na4 Na7 44.09(15) 2_254 2_254 ? O14 Na4 O2 76.2(2) 2_254 . ? O14 Na4 O6W 95.0(3) 2_254 1_544 ? O14 Na4 O7W 174.7(3) 2_254 1_544 ? O14 Na4 O13W 87.5(2) 2_254 . ? O6W Na4 Na2 43.9(2) 1_544 1_544 ? O6W Na4 Na5 122.6(3) 1_544 . ? O6W Na4 Na7 132.1(2) 1_544 2_254 ? O6W Na4 O2 169.9(3) 1_544 . ? O7W Na4 Na2 43.03(16) 1_544 1_544 ? O7W Na4 Na5 123.28(18) 1_544 . ? O7W Na4 Na7 136.5(2) 1_544 2_254 ? O7W Na4 O2 101.5(2) 1_544 . ? O7W Na4 O6W 86.8(3) 1_544 1_544 ? O13W Na4 Na2 91.95(18) . 1_544 ? O13W Na4 Na5 48.92(16) . . ? O13W Na4 Na7 106.49(18) . 2_254 ? O13W Na4 O2 82.7(2) . . ? O13W Na4 O6W 92.0(3) . 1_544 ? O13W Na4 O7W 87.4(2) . 1_544 ? O15W Na4 Na2 94.1(2) . 1_544 ? O15W Na4 Na5 124.9(2) . . ? O15W Na4 Na7 67.5(2) . 2_254 ? O15W Na4 O2 93.7(3) . . ? O15W Na4 O14 86.5(3) . 2_254 ? O15W Na4 O6W 90.8(3) . 1_544 ? O15W Na4 O7W 98.5(3) . 1_544 ? O15W Na4 O13W 173.6(3) . . ? Na4 Na5 Na7 67.63(10) . 2_254 ? O2 Na5 Na4 49.94(15) . . ? O2 Na5 Na7 48.26(13) . 2_254 ? O2 Na5 O14 74.29(19) . 2_254 ? O2 Na5 O13W 83.8(2) . . ? O2 Na5 O14W 153.4(2) . . ? O12 Na5 Na4 139.82(19) 2_154 . ? O12 Na5 Na7 127.95(19) 2_154 2_254 ? O12 Na5 O2 108.5(2) 2_154 . ? O12 Na5 O14 173.2(2) 2_154 2_254 ? O12 Na5 O2W 90.0(2) 2_154 . ? O12 Na5 O13W 103.4(2) 2_154 . ? O12 Na5 O14W 96.6(2) 2_154 . ? O14 Na5 Na4 46.68(14) 2_254 . ? O14 Na5 Na7 49.22(14) 2_254 2_254 ? O2W Na5 Na4 113.76(17) . . ? O2W Na5 Na7 46.15(14) . 2_254 ? O2W Na5 O2 80.1(2) . . ? O2W Na5 O14 84.38(19) . 2_254 ? O2W Na5 O13W 161.7(2) . . ? O2W Na5 O14W 108.9(3) . . ? O13W Na5 Na4 48.23(16) . . ? O13W Na5 Na7 115.82(18) . 2_254 ? O13W Na5 O14 82.9(2) . 2_254 ? O14W Na5 Na4 104.7(2) . . ? O14W Na5 Na7 120.5(2) . 2_254 ? O14W Na5 O14 81.7(2) . 2_254 ? O14W Na5 O13W 82.2(2) . . ? Na2 Na6 Na1 160.47(13) 2_255 . ? Na2 Na6 Na3 58.94(10) 2_255 2_255 ? Na3 Na6 Na1 123.80(13) 2_255 . ? O6 Na6 Na1 39.18(15) . . ? O6 Na6 Na2 125.79(19) . 2_255 ? O6 Na6 Na3 145.3(2) . 2_255 ? O6 Na6 O8 166.4(3) . 1_655 ? O6 Na6 O18 107.5(2) . 2_255 ? O6 Na6 O9W 116.9(2) . 2_255 ? O6 Na6 O11W 89.3(2) . 2_255 ? O6 Na6 O12W 87.4(2) . . ? O8 Na6 Na1 147.68(17) 1_655 . ? O8 Na6 Na2 50.51(14) 1_655 2_255 ? O8 Na6 Na3 47.34(15) 1_655 2_255 ? O8 Na6 O18 79.61(19) 1_655 2_255 ? O8 Na6 O9W 75.61(18) 1_655 2_255 ? O8 Na6 O11W 80.3(2) 1_655 2_255 ? O8 Na6 O12W 83.2(2) 1_655 . ? O18 Na6 Na1 117.42(17) 2_255 . ? O18 Na6 Na2 48.05(15) 2_255 2_255 ? O18 Na6 Na3 46.35(13) 2_255 2_255 ? O18 Na6 O9W 77.95(19) 2_255 2_255 ? O18 Na6 O11W 80.2(3) 2_255 2_255 ? O18 Na6 O12W 159.5(2) 2_255 . ? O9W Na6 Na1 81.31(15) 2_255 . ? O9W Na6 Na2 104.57(16) 2_255 2_255 ? O9W Na6 Na3 45.64(13) 2_255 2_255 ? O11W Na6 Na1 127.51(19) 2_255 . ? O11W Na6 Na2 45.47(19) 2_255 2_255 ? O11W Na6 Na3 104.4(2) 2_255 2_255 ? O11W Na6 O9W 149.9(2) 2_255 2_255 ? O12W Na6 Na1 83.02(16) . . ? O12W Na6 Na2 111.82(19) . 2_255 ? O12W Na6 Na3 124.69(16) . 2_255 ? O12W Na6 O9W 108.4(2) . 2_255 ? O12W Na6 O11W 86.0(3) . 2_255 ? Na1 Na7 Na9 51.93(7) . . ? Na4 Na7 Na1 166.96(12) 2_254 . ? Na4 Na7 Na9 141.12(10) 2_254 . ? Na5 Na7 Na1 120.51(12) 2_254 . ? Na5 Na7 Na4 54.77(9) 2_254 2_254 ? Na5 Na7 Na9 126.93(10) 2_254 . ? O2 Na7 Na1 145.11(17) 2_254 . ? O2 Na7 Na4 42.88(14) 2_254 2_254 ? O2 Na7 Na5 46.18(14) 2_254 2_254 ? O2 Na7 Na9 105.96(15) 2_254 . ? O2 Na7 O14 73.02(18) 2_254 . ? O4 Na7 Na1 91.30(16) 2_154 . ? O4 Na7 Na4 88.11(16) 2_154 2_254 ? O4 Na7 Na5 138.63(18) 2_154 2_254 ? O4 Na7 Na9 92.92(15) 2_154 . ? O4 Na7 O2 119.0(2) 2_154 2_254 ? O4 Na7 O14 91.2(2) 2_154 . ? O14 Na7 Na1 126.75(16) . . ? O14 Na7 Na4 40.27(14) . 2_254 ? O14 Na7 Na5 49.34(14) . 2_254 ? O14 Na7 Na9 175.71(16) . . ? O1W Na7 Na1 80.72(16) . . ? O1W Na7 Na4 112.26(17) . 2_254 ? O1W Na7 Na5 120.61(17) . 2_254 ? O1W Na7 Na9 29.16(13) . . ? O1W Na7 O2 83.49(19) . 2_254 ? O1W Na7 O4 87.9(2) . 2_154 ? O1W Na7 O14 152.5(2) . . ? O1W Na7 O2W 105.4(2) . 2_254 ? O1W Na7 O5W 111.6(2) . . ? O2W Na7 Na1 76.70(15) 2_254 . ? O2W Na7 Na4 100.02(16) 2_254 2_254 ? O2W Na7 Na5 45.27(15) 2_254 2_254 ? O2W Na7 Na9 91.95(16) 2_254 . ? O2W Na7 O2 77.82(19) 2_254 2_254 ? O2W Na7 O4 160.2(2) 2_254 2_154 ? O2W Na7 O14 83.8(2) 2_254 . ? O5W Na7 Na1 34.98(15) . . ? O5W Na7 Na4 132.75(18) . 2_254 ? O5W Na7 Na5 113.30(17) . 2_254 ? O5W Na7 Na9 84.89(15) . . ? O5W Na7 O2 159.4(2) . 2_254 ? O5W Na7 O4 76.9(2) . 2_154 ? O5W Na7 O14 94.8(2) . . ? O5W Na7 O2W 84.45(19) . 2_254 ? Gd2 Na8 Na1 103.36(8) . . ? O11 Na8 Gd2 43.95(12) . . ? O11 Na8 Na1 91.03(15) . . ? O11 Na8 O21 69.70(17) . 2_255 ? O11 Na8 C16 172.8(2) . 2_255 ? O15 Na8 Gd2 119.10(15) 2_255 . ? O15 Na8 Na1 85.49(15) 2_255 . ? O15 Na8 O11 161.2(2) 2_255 . ? O15 Na8 O21 92.05(18) 2_255 2_255 ? O15 Na8 C16 22.68(18) 2_255 2_255 ? O19 Na8 Gd2 42.86(12) . . ? O19 Na8 Na1 137.82(16) . . ? O19 Na8 O11 78.10(19) . . ? O19 Na8 O15 92.12(19) . 2_255 ? O19 Na8 O21 71.53(18) . 2_255 ? O19 Na8 C16 109.1(2) . 2_255 ? O21 Na8 Gd2 44.05(12) 2_255 . ? O21 Na8 Na1 66.49(14) 2_255 . ? O21 Na8 C16 111.3(2) 2_255 2_255 ? C16 Na8 Gd2 141.63(17) 2_255 . ? C16 Na8 Na1 83.03(15) 2_255 . ? O3W Na8 Gd2 129.71(16) . . ? O3W Na8 Na1 30.99(14) . . ? O3W Na8 O11 100.6(2) . . ? O3W Na8 O15 85.9(2) . 2_255 ? O3W Na8 O19 168.7(2) . . ? O3W Na8 O21 97.42(19) . 2_255 ? O3W Na8 C16 72.2(2) . 2_255 ? O3W Na8 O17W 92.1(2) . . ? O17W Na8 Gd2 109.28(17) . . ? O17W Na8 Na1 119.64(18) . . ? O17W Na8 O11 80.01(19) . . ? O17W Na8 O15 117.7(2) . 2_255 ? O17W Na8 O19 98.7(2) . . ? O17W Na8 O21 149.4(2) . 2_255 ? O17W Na8 C16 99.3(2) . 2_255 ? Na1 Na9 Na1 180.000(1) . 2_254 ? Na1 Na9 Na7 118.62(7) 2_254 . ? Na1 Na9 Na7 61.38(7) . . ? Na1 Na9 Na7 61.38(7) 2_254 2_254 ? Na1 Na9 Na7 118.62(7) . 2_254 ? Na7 Na9 Na7 180.0 2_254 . ? O1W Na9 Na1 89.90(14) . . ? O1W Na9 Na1 90.10(14) 2_254 . ? O1W Na9 Na1 89.90(14) 2_254 2_254 ? O1W Na9 Na1 90.10(14) . 2_254 ? O1W Na9 Na7 151.09(13) . 2_254 ? O1W Na9 Na7 28.91(13) 2_254 2_254 ? O1W Na9 Na7 151.09(13) 2_254 . ? O1W Na9 Na7 28.91(13) . . ? O1W Na9 O1W 180.000(1) 2_254 . ? O1W Na9 O4W 81.65(17) . . ? O1W Na9 O4W 81.65(17) 2_254 2_254 ? O1W Na9 O4W 98.35(17) 2_254 . ? O1W Na9 O4W 98.35(17) . 2_254 ? O1W Na9 O16W 94.68(19) . . ? O1W Na9 O16W 85.32(19) 2_254 . ? O1W Na9 O16W 85.32(19) . 2_254 ? O1W Na9 O16W 94.68(19) 2_254 2_254 ? O4W Na9 Na1 135.32(14) 2_254 . ? O4W Na9 Na1 44.68(14) . . ? O4W Na9 Na1 44.68(14) 2_254 2_254 ? O4W Na9 Na1 135.32(14) . 2_254 ? O4W Na9 Na7 114.47(13) 2_254 . ? O4W Na9 Na7 65.53(13) . . ? O4W Na9 Na7 65.53(13) 2_254 2_254 ? O4W Na9 Na7 114.47(13) . 2_254 ? O4W Na9 O4W 180.000(1) 2_254 . ? O16W Na9 Na1 41.48(14) 2_254 2_254 ? O16W Na9 Na1 41.48(14) . . ? O16W Na9 Na1 138.52(14) . 2_254 ? O16W Na9 Na1 138.52(14) 2_254 . ? O16W Na9 Na7 70.36(14) 2_254 2_254 ? O16W Na9 Na7 109.64(14) . 2_254 ? O16W Na9 Na7 109.64(14) 2_254 . ? O16W Na9 Na7 70.36(14) . . ? O16W Na9 O4W 93.92(18) 2_254 . ? O16W Na9 O4W 86.08(18) . . ? O16W Na9 O4W 93.92(18) . 2_254 ? O16W Na9 O4W 86.08(18) 2_254 2_254 ? O16W Na9 O16W 180.00(16) . 2_254 ? O9 P1 O20 112.2(3) . . ? O10 P1 O9 112.1(3) . . ? O10 P1 O20 113.2(3) . . ? O19 P2 O21 112.4(3) . . ? O22 P2 O19 130.6(5) . . ? O22 P2 O21 109.1(5) . . ? O22 P2 O22A 59.2(6) . . ? O22A P2 O19 112.5(4) . . ? O22A P2 O21 124.6(4) . . ? C1 N1 Gd1 105.3(4) . . ? C1 N1 C3 109.8(5) . . ? C1 N1 C9 108.6(5) . . ? C3 N1 Gd1 109.5(4) . . ? C3 N1 C9 111.4(5) . . ? C9 N1 Gd1 112.0(4) . . ? C5 N2 Gd1 109.1(4) . . ? C5 N2 C10 112.7(5) . . ? C7 N2 Gd1 104.7(4) . . ? C7 N2 C5 109.3(5) . . ? C7 N2 C10 108.2(5) . . ? C10 N2 Gd1 112.7(4) . . ? C11 N3 Gd2 108.7(4) . . ? C11 N3 C13 109.5(6) . . ? C11 N3 C19 109.7(6) . . ? C13 N3 Gd2 106.5(4) . . ? C19 N3 Gd2 110.3(4) . . ? C19 N3 C13 112.1(6) . . ? C15 N4 Gd2 108.8(4) . . ? C15 N4 C17 109.0(6) . . ? C15 N4 C20 109.8(5) . . ? C17 N4 Gd2 107.5(4) . . ? C17 N4 C20 110.8(6) . . ? C20 N4 Gd2 110.8(4) . . ? C2 O1 Gd1 120.8(4) . . ? Na4 O2 Na7 94.15(19) . 2_254 ? Na5 O2 Na4 82.2(2) . . ? Na5 O2 Na7 85.56(18) . 2_254 ? C2 O2 Na4 131.0(5) . . ? C2 O2 Na5 119.8(4) . . ? C2 O2 Na7 128.1(5) . 2_254 ? C4 O3 Gd1 123.7(5) . . ? C4 O4 Na7 155.6(5) . 2_154 ? Gd1 O5 Na1 137.1(2) . . ? C6 O5 Gd1 127.1(5) . . ? C6 O5 Na1 95.4(4) . . ? Na6 O6 Na1 107.4(2) . . ? C6 O6 Na1 87.7(4) . . ? C6 O6 Na6 144.5(5) . . ? C8 O7 Gd1 119.8(4) . . ? Na3 O8 Na2 81.03(19) 2_155 2_155 ? Na6 O8 Na2 81.95(18) 1_455 2_155 ? Na6 O8 Na3 86.7(2) 1_455 2_155 ? C8 O8 Na2 140.2(5) . 2_155 ? C8 O8 Na3 120.8(5) . 2_155 ? C8 O8 Na6 128.3(5) . 1_455 ? P1 O9 Gd1 145.2(3) . . ? Gd2 O11 Na8 89.82(18) . . ? C12 O11 Gd2 122.6(5) . . ? C12 O11 Na8 136.2(5) . . ? C12 O12 Na5 135.9(5) . 2_154 ? P1 O20 Gd1 144.5(3) . 2_154 ? C14 O13 Gd2 121.7(4) . . ? Na4 O14 Na5 81.64(18) 2_254 2_254 ? Na4 O14 Na7 95.6(2) 2_254 . ? Na7 O14 Na5 81.44(18) . 2_254 ? C14 O14 Na4 141.1(5) . 2_254 ? C14 O14 Na5 125.8(5) . 2_254 ? C14 O14 Na7 113.7(5) . . ? Gd2 O15 Na8 124.8(2) . 2_255 ? C16 O15 Gd2 125.0(5) . . ? C16 O15 Na8 108.9(5) . 2_255 ? C16 O16 Na3 135.1(5) . 1_655 ? C18 O17 Gd2 123.2(5) . . ? Na2 O18 Na3 83.96(18) . . ? Na6 O18 Na2 83.9(2) 2_255 . ? Na6 O18 Na3 87.46(19) 2_255 . ? C18 O18 Na2 136.4(5) . . ? C18 O18 Na3 129.9(5) . . ? C18 O18 Na6 118.9(5) . 2_255 ? Gd2 O19 Na8 92.16(19) . . ? P2 O19 Gd2 137.6(3) . . ? P2 O19 Na8 126.8(3) . . ? Gd2 O21 Na8 86.48(17) 2_255 2_255 ? P2 O21 Gd2 137.3(3) . 2_255 ? P2 O21 Na8 116.0(3) . 2_255 ? P2 O22 Na1 126.1(6) . 2_255 ? N1 C1 C2 109.3(6) . . ? O1 C2 C1 116.6(6) . . ? O2 C2 O1 125.0(7) . . ? O2 C2 C1 118.4(7) . . ? N1 C3 C4 110.7(6) . . ? O3 C4 C3 117.5(6) . . ? O4 C4 O3 123.9(7) . . ? O4 C4 C3 118.6(6) . . ? N2 C5 C6 109.9(6) . . ? O5 C6 Na1 58.2(4) . . ? O5 C6 C5 116.1(6) . . ? O6 C6 Na1 66.4(4) . . ? O6 C6 O5 124.6(7) . . ? O6 C6 C5 119.3(7) . . ? C5 C6 Na1 173.9(5) . . ? N2 C7 C8 111.3(6) . . ? O7 C8 C7 116.3(6) . . ? O8 C8 O7 125.2(7) . . ? O8 C8 C7 118.5(7) . . ? N1 C9 C10 112.8(6) . . ? N2 C10 C9 112.1(6) . . ? N3 C11 C12 112.0(6) . . ? O11 C12 C11 117.0(7) . . ? O12 C12 O11 124.1(7) . . ? O12 C12 C11 118.8(6) . . ? N3 C13 C14 115.2(6) . . ? O13 C14 C13 117.1(6) . . ? O14 C14 O13 124.3(7) . . ? O14 C14 C13 118.6(7) . . ? N4 C15 C16 112.5(6) . . ? O15 C16 Na8 48.5(4) . 2_255 ? O15 C16 C15 116.4(7) . . ? O16 C16 Na8 77.3(4) . 2_255 ? O16 C16 O15 125.8(7) . . ? O16 C16 C15 117.8(7) . . ? C15 C16 Na8 164.9(5) . 2_255 ? N4 C17 C18 114.5(6) . . ? O17 C18 C17 117.3(7) . . ? O18 C18 O17 125.1(7) . . ? O18 C18 C17 117.5(7) . . ? N3 C19 C20 112.7(6) . . ? N4 C20 C19 112.2(6) . . ? Na7 O1W Na9 121.9(2) . . ? Na5 O2W Na7 88.6(2) . 2_254 ? Na8 O3W Na1 119.5(2) . . ? Na9 O4W Na1 91.67(18) . . ? Na7 O5W Na1 111.0(2) . . ? Na2 O6W Na4 91.3(4) . 1_566 ? Na2 O7W Na4 93.4(2) . 1_566 ? Na2 O8W Na3 82.8(2) . . ? Na3 O9W Na6 82.55(19) . 2_255 ? Na2 O11W Na6 83.9(3) . 2_255 ? Na4 O13W Na5 82.8(2) . . ? Na1 O16W Na9 96.4(2) . . ? O1A Cl3 O1B 105.2(10) . . ? Cl3 O1A O1B 119.6(12) . 2_165 ? O1A O1B Cl3 135.1(15) 2_165 . ? _database_code_depnum_ccdc_archive 'CCDC 951762'