Supplementary Material (ESI) for Dalton Transactions This journal is (c) The Royal Society of Chemistry 2008 data_global _journal_name_full 'Dalton Trans.' _journal_coden_cambridge 0222 _publ_contact_author_name 'Prof. Mats Tilset' _publ_contact_author_address ; Department of Chemistry University of Oslo P.O. Box 1033 Blindern N-0315 Oslo Norway ; _publ_contact_author_email mats.tilset@kjemi.uio.no loop_ _publ_author_name _publ_author_address 'Kai C. Szeto' ; Department of Chemistry University of Oslo P.O. Box 1033 Blindern N-0315 Oslo Norway ; 'Kjell Ove Kongshaug' ; Norwegian University of Science and Technology Department of Materials Technology N-7491 Trondheim Norway ; 'Soeren Jakobsen' ; Department of Chemistry University of Oslo P.O. Box 1033 Blindern N-0315 Oslo Norway ; 'Mats Tilset' ; Department of Chemistry University of Oslo P.O. Box 1033 Blindern N-0315 Oslo Norway ; 'Karl Petter Lillerud' ; Department of Chemistry University of Oslo P.O. Box 1033 Blindern N-0315 Oslo Norway ; _publ_section_title ; Design, synthesis and characterization of a Pt-Gd metal-organic framework containing potentially catalytically active sites ; _publ_section_abstract ; Abstract A novel bimetallic coordination polymer {[(BPDC)PtCl2]3(Gd(H2O)3)2}.5H2O (BPDC = 2,2-bipyridine-5,5-dicarboxylate) has been designed and synthesized by hydrothermal methods. The new coordination polymer contains subunits of (BPDC)PtCl2 (1) where both N atoms of the BPDC ligand are attached to a square-planar Pt(II) center. The two remaining cis coordination sites at Pt(II) are occupied by chloride ions. The final structure (2) of the polymeric network is obtained when Gd(III) ions link together the (BPDC)PtCl2 units, which are organized in sheets, into larger blocks. These blocks are stacked along the crystallographic [010] direction and are held together by a hydrogen bonding scheme that involves carboxylate oxygen atoms and water molecules in the coordination sphere of Gd. The coordination polymer 2 can be obtained in a single-step reaction or in a two-step synthesis where the corresponding Pt complex (1) was first synthesized followed by reacting 1 with Gd(NO3)3.6H2O. In-situ high temperature powder X-ray diffraction shows that the crystalline coordination polymer transforms into an anhydrous modification at 100oC. This modification is stable to 350 oC, at which the structure starts to decompose. The coordination sphere around platinum in the polymer closely resembles organometallic Pt complexes that have been previously found to catalytically or stoichiometrically activate and functionalize hydrocarbon C H bonds in homogeneous systems. ; data_3genPt-Gd-MOF _database_code_depnum_ccdc_archive 'CCDC 672214' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety 'C36 H18 Cl6 Gd2 N6 O18 Pt3, 5(H2O)' _chemical_formula_sum 'C36 H40 Cl6 Gd2 N6 O23 Pt3' _chemical_formula_weight 2037.21 loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source Pt Pt -1.7033 8.3905 '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' Cl Cl 0.1484 0.1585 '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' N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 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' _symmetry_cell_setting Orthorhombic _symmetry_space_group_name_H-M 'P b c a' loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x+1/2, -y, z+1/2' '-x, y+1/2, -z+1/2' 'x+1/2, -y+1/2, -z' '-x, -y, -z' 'x-1/2, y, -z-1/2' 'x, -y-1/2, z-1/2' '-x-1/2, y-1/2, z' _cell_length_a 18.021(4) _cell_length_b 19.884(4) _cell_length_c 28.125(6) _cell_angle_alpha 90.00 _cell_angle_beta 90.00 _cell_angle_gamma 90.00 _cell_volume 10078(4) _cell_formula_units_Z 8 _cell_measurement_temperature 105(2) _cell_measurement_reflns_used 37175 _cell_measurement_theta_min 1.45 _cell_measurement_theta_max 18.67 _exptl_crystal_description Needle _exptl_crystal_colour Red _exptl_crystal_size_max 0.16 _exptl_crystal_size_mid 0.05 _exptl_crystal_size_min 0.05 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 2.685 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 7568 _exptl_absorpt_coefficient_mu 11.300 _exptl_absorpt_correction_type Empirical #_exptl_absorpt_correction_T_min 0.2700 #_exptl_absorpt_correction_T_max 0.6072 #_exptl_absorpt_process_details 'SADABS (Sheldrick, 1997)' _exptl_special_details ? _exptl_absorpt_process_details ; Sheldrick, G.M. (anon) SHELX97 Release 97-2 (1998) I/sigma threshold for reflections = 5.000 Delta(U)/lambda**2 = 0.000 Highest even order spherical harmonic = 6 Highest odd order spherical harmonic = 3 ; _exptl_absorpt_correction_T_min 0.2337 _exptl_absorpt_correction_T_max 0.6953 _exptl_absorpt_Rmerge_before 0.0945 _exptl_absorpt_Rmerge_after 0.0637 _diffrn_ambient_temperature 105(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 'Siemens Bruker SMART CCD' _diffrn_measurement_method '\w scan' _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% none _diffrn_reflns_number 37175 _diffrn_reflns_av_R_equivalents 0.1994 _diffrn_reflns_av_sigmaI/netI 0.0792 _diffrn_reflns_limit_h_min -16 _diffrn_reflns_limit_h_max 16 _diffrn_reflns_limit_k_min -17 _diffrn_reflns_limit_k_max 17 _diffrn_reflns_limit_l_min -25 _diffrn_reflns_limit_l_max 25 _diffrn_reflns_theta_min 1.45 _diffrn_reflns_theta_max 18.67 _reflns_number_total 3833 _reflns_number_gt 2529 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'SMART (Bruker, 1998)' _computing_cell_refinement 'SMART (Bruker, 1998)' _computing_data_reduction 'SAINT (Bruker, 2004)' _computing_structure_solution 'SHELXTL (Bruker, 2000)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'Diamond 3.0 (Crystal Impact GbR)' _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^)+(0.0432P)^2^+101.7131P] 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 3833 _refine_ls_number_parameters 475 _refine_ls_number_restraints 204 _refine_ls_R_factor_all 0.0933 _refine_ls_R_factor_gt 0.0488 _refine_ls_wR_factor_ref 0.1097 _refine_ls_wR_factor_gt 0.0941 _refine_ls_goodness_of_fit_ref 1.021 _refine_ls_restrained_S_all 1.001 _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 Pt1 Pt 0.43796(5) 0.32854(5) 0.69182(4) 0.0196(3) Uani 1 1 d U . . Pt2 Pt 0.98128(5) 0.33629(5) 0.30786(4) 0.0203(3) Uani 1 1 d U . . Pt3 Pt 1.02307(6) 0.49933(5) 0.69718(4) 0.0249(3) Uani 1 1 d U . . Gd1 Gd 0.85477(7) 0.34611(7) 0.52996(5) 0.0261(4) Uani 1 1 d U . . Gd2 Gd 0.56834(7) 0.38070(6) 0.46726(5) 0.0240(4) Uani 1 1 d U . . Cl1 Cl 0.3180(3) 0.3311(3) 0.7194(2) 0.0278(18) Uani 1 1 d U . . Cl2 Cl 0.3923(3) 0.3257(3) 0.6162(2) 0.0266(18) Uani 1 1 d U . . Cl3 Cl 1.0236(4) 0.3344(3) 0.3847(2) 0.0239(17) Uani 1 1 d U . . Cl4 Cl 1.1031(3) 0.3313(3) 0.2837(2) 0.0260(18) Uani 1 1 d U . . Cl5 Cl 1.0773(4) 0.4954(3) 0.6234(2) 0.0325(19) Uani 1 1 d U . . Cl6 Cl 1.1400(4) 0.4924(3) 0.7290(2) 0.0326(19) Uani 1 1 d U . . O1 O 0.4711(9) 0.3261(8) 0.9252(6) 0.024(4) Uani 1 1 d U . . O2 O 0.3726(9) 0.3499(8) 0.8824(6) 0.031(5) Uani 1 1 d U . . O3 O 0.7364(9) 0.3596(8) 0.5602(6) 0.025(5) Uani 1 1 d U . . O4 O 0.6217(9) 0.3345(8) 0.5353(6) 0.032(5) Uani 1 1 d U . . O5 O 0.7962(10) 0.3479(8) 0.4600(6) 0.040(5) Uani 1 1 d U . . O6 O 0.6864(9) 0.3823(8) 0.4356(6) 0.030(5) Uani 1 1 d U . . O7 O 0.9514(8) 0.3469(8) 0.0741(6) 0.023(5) Uani 1 1 d U . . O8 O 1.0536(9) 0.3443(8) 0.1167(6) 0.027(5) Uani 1 1 d U . . O9 O 0.9606(8) 0.5206(8) 0.9276(6) 0.021(5) Uani 1 1 d U . . O10 O 1.0660(9) 0.4875(8) 0.8924(6) 0.028(5) Uani 1 1 d U . . O11 O 0.8469(9) 0.4627(8) 0.5387(6) 0.032(5) Uani 1 1 d U . . O12 O 0.7458(10) 0.5238(9) 0.5493(6) 0.043(6) Uani 1 1 d U . . N1 N 0.4839(11) 0.3293(10) 0.7561(7) 0.021(6) Uiso 1 1 d . . . N2 N 0.5451(10) 0.3312(10) 0.6721(7) 0.020(6) Uiso 1 1 d . . . N3 N 0.8735(11) 0.3405(10) 0.3243(7) 0.023(6) Uiso 1 1 d . . . N4 N 0.9374(12) 0.3363(10) 0.2428(7) 0.026(6) Uiso 1 1 d . . . N5 N 0.9685(10) 0.5018(9) 0.7597(6) 0.010(5) Uiso 1 1 d . . . N6 N 0.9193(9) 0.5031(9) 0.6732(6) 0.014(5) Uiso 1 1 d . . . C1 C 0.4509(13) 0.3315(11) 0.7978(8) 0.018(7) Uiso 1 1 d . . . H1 H 0.3995 0.3360 0.7978 0.021 Uiso 1 1 calc R . . C2 C 0.4852(15) 0.3279(12) 0.8413(9) 0.028(7) Uiso 1 1 d . . . C3 C 0.5591(14) 0.3289(12) 0.7553(9) 0.022(7) Uiso 1 1 d . . . C4 C 0.4408(15) 0.3348(12) 0.8864(9) 0.026(7) Uiso 1 1 d . . . C5 C 0.5612(13) 0.3231(11) 0.8421(9) 0.020(7) Uiso 1 1 d . . . H5 H 0.5860 0.3202 0.8710 0.024 Uiso 1 1 calc R . . C6 C 0.6027(13) 0.3225(10) 0.7983(8) 0.010(6) Uiso 1 1 d . . . H6 H 0.6541 0.3184 0.7977 0.012 Uiso 1 1 calc R . . C7 C 0.6684(14) 0.3354(12) 0.7011(9) 0.026(7) Uiso 1 1 d . . . H7 H 0.7011 0.3333 0.7267 0.032 Uiso 1 1 calc R . . C8 C 0.6695(13) 0.3444(11) 0.5689(8) 0.010(6) Uiso 1 1 d . . . C9 C 0.6460(13) 0.3402(11) 0.6190(8) 0.009(6) Uiso 1 1 d . . . C10 C 0.5716(12) 0.3327(10) 0.6278(8) 0.013(6) Uiso 1 1 d . . . H10 H 0.5389 0.3286 0.6023 0.015 Uiso 1 1 calc R . . C11 C 0.6965(14) 0.3412(12) 0.6545(9) 0.027(7) Uiso 1 1 d . . . H11 H 0.7470 0.3454 0.6485 0.032 Uiso 1 1 calc R . . C12 C 0.5934(15) 0.3329(13) 0.7093(10) 0.035(8) Uiso 1 1 d . . . C13 C 0.7510(16) 0.3632(13) 0.4272(10) 0.035(8) Uiso 1 1 d . . . C14 C 0.8471(13) 0.3476(11) 0.3679(8) 0.016(7) Uiso 1 1 d . . . H14 H 0.8803 0.3491 0.3933 0.019 Uiso 1 1 calc R . . C15 C 0.9778(14) 0.3370(11) 0.2010(8) 0.019(7) Uiso 1 1 d . . . H15 H 1.0293 0.3352 0.2018 0.023 Uiso 1 1 calc R . . C16 C 0.8634(14) 0.3422(12) 0.1571(9) 0.029(7) Uiso 1 1 d . . . H16 H 0.8384 0.3465 0.1283 0.035 Uiso 1 1 calc R . . C17 C 0.7711(13) 0.3529(11) 0.3773(9) 0.017(7) Uiso 1 1 d . . . C18 C 0.7243(14) 0.3494(11) 0.3409(9) 0.020(7) Uiso 1 1 d . . . H18 H 0.6735 0.3522 0.3465 0.024 Uiso 1 1 calc R . . C19 C 0.8242(12) 0.3387(11) 0.2877(8) 0.012(6) Uiso 1 1 d . . . C20 C 0.7489(13) 0.3417(12) 0.2958(9) 0.023(7) Uiso 1 1 d . . . H20 H 0.7156 0.3385 0.2707 0.027 Uiso 1 1 calc R . . C21 C 0.8595(13) 0.3377(11) 0.2413(8) 0.014(6) Uiso 1 1 d . . . C22 C 0.8238(13) 0.3379(11) 0.1987(8) 0.013(6) Uiso 1 1 d . . . H22 H 0.7723 0.3350 0.1977 0.016 Uiso 1 1 calc R . . C23 C 0.9404(13) 0.3404(11) 0.1577(8) 0.012(6) Uiso 1 1 d . . . C24 C 0.9844(16) 0.3433(12) 0.1132(10) 0.026(7) Uiso 1 1 d . . . C25 C 0.9949(11) 0.4996(10) 0.8024(8) 0.003(6) Uiso 1 1 d . . . H25 H 1.0460 0.4936 0.8043 0.004 Uiso 1 1 calc R . . C26 C 0.8948(14) 0.5038(11) 0.7559(9) 0.019(7) Uiso 1 1 d . . . C27 C 0.8196(15) 0.5016(13) 0.6159(10) 0.036(8) Uiso 1 1 d . . . C28 C 0.9972(14) 0.5040(13) 0.8896(9) 0.028(8) Uiso 1 1 d . . . C29 C 0.8040(14) 0.4958(13) 0.5658(9) 0.023(7) Uiso 1 1 d . . . C30 C 0.8636(12) 0.5029(10) 0.7095(7) 0.004(6) Uiso 1 1 d . . . C31 C 0.8520(13) 0.5061(11) 0.7966(8) 0.018(7) Uiso 1 1 d . . . H31 H 0.8006 0.5091 0.7941 0.022 Uiso 1 1 calc R . . C32 C 0.8933(13) 0.5005(11) 0.6294(8) 0.016(6) Uiso 1 1 d . . . H32 H 0.9282 0.4977 0.6051 0.019 Uiso 1 1 calc R . . C33 C 0.9611(12) 0.5045(12) 0.8431(9) 0.019(7) Uiso 1 1 d . . . C34 C 0.7911(13) 0.5064(12) 0.6979(9) 0.025(7) Uiso 1 1 d . . . H34 H 0.7559 0.5076 0.7220 0.030 Uiso 1 1 calc R . . C35 C 0.8840(13) 0.5041(12) 0.8395(9) 0.028(7) Uiso 1 1 d . . . H35 H 0.8550 0.5024 0.8668 0.033 Uiso 1 1 calc R . . C36 C 0.7677(14) 0.5081(13) 0.6514(9) 0.032(8) Uiso 1 1 d . . . H36 H 0.7178 0.5136 0.6441 0.039 Uiso 1 1 calc R . . OW1 O 0.5614(8) 0.2639(7) 0.4694(6) 0.025(4) Uani 1 1 d U . . OW2 O 0.6184(8) 0.4715(7) 0.5176(5) 0.024(5) Uani 1 1 d U . . OW3 O 0.4675(8) 0.4036(8) 0.5189(6) 0.024(4) Uani 1 1 d U . . OW4 O 0.9206(9) 0.2600(8) 0.4818(6) 0.030(5) Uani 1 1 d U . . OW5 O 0.8139(9) 0.2378(9) 0.5516(6) 0.045(6) Uani 1 1 d U . . OW6 O 0.9505(8) 0.4015(8) 0.4813(6) 0.032(5) Uani 1 1 d U . . OW7 O 1.0813(11) 0.4451(10) 0.5173(7) 0.061(6) Uani 1 1 d U . . OW8 O 1.1515(11) 0.3293(10) 0.4926(7) 0.064(6) Uani 1 1 d U . . OW9 O 0.7036(10) 0.1834(9) 0.6018(7) 0.051(6) Uani 1 1 d U . . OW10 O 0.6864(12) 0.6190(11) 0.4884(8) 0.083(8) Uani 1 1 d U . . OW11 O 0.7316(14) 0.0912(13) 0.3826(10) 0.113(9) 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 Pt1 0.0151(6) 0.0225(7) 0.0213(7) -0.0008(6) 0.0030(6) 0.0005(5) Pt2 0.0134(6) 0.0244(6) 0.0230(7) 0.0000(6) 0.0014(6) 0.0002(5) Pt3 0.0238(6) 0.0262(7) 0.0247(7) -0.0004(6) 0.0005(6) 0.0004(6) Gd1 0.0182(8) 0.0366(9) 0.0233(9) 0.0006(8) -0.0006(7) 0.0017(7) Gd2 0.0190(8) 0.0301(9) 0.0229(9) -0.0005(8) -0.0002(8) 0.0011(7) Cl1 0.024(3) 0.031(3) 0.028(3) -0.002(2) 0.003(2) 0.001(2) Cl2 0.022(3) 0.029(3) 0.029(3) 0.001(2) 0.001(2) 0.000(2) Cl3 0.021(3) 0.025(3) 0.025(3) 0.000(2) 0.000(2) 0.000(2) Cl4 0.023(3) 0.027(3) 0.027(3) 0.002(2) 0.001(2) -0.001(2) Cl5 0.030(3) 0.035(3) 0.032(3) 0.002(2) 0.001(2) -0.001(2) Cl6 0.030(3) 0.034(3) 0.034(3) 0.002(2) -0.003(2) 0.002(2) O1 0.024(5) 0.025(5) 0.025(5) -0.001(3) -0.001(3) 0.002(3) O2 0.031(6) 0.032(5) 0.031(5) -0.001(3) 0.002(3) 0.001(3) O3 0.025(5) 0.026(5) 0.025(5) -0.001(3) 0.001(3) 0.001(3) O4 0.032(5) 0.032(5) 0.033(5) 0.000(3) -0.001(3) -0.002(3) O5 0.039(6) 0.042(6) 0.039(6) 0.001(3) 0.000(3) 0.002(3) O6 0.030(5) 0.031(5) 0.030(5) 0.000(3) 0.001(3) 0.002(3) O7 0.023(5) 0.023(5) 0.024(5) 0.000(3) 0.000(3) 0.001(3) O8 0.026(5) 0.027(5) 0.027(5) 0.002(3) 0.001(3) 0.000(3) O9 0.021(5) 0.021(5) 0.021(5) 0.000(3) 0.001(3) 0.000(3) O10 0.027(5) 0.029(5) 0.028(5) -0.001(3) 0.002(3) 0.000(3) O11 0.031(5) 0.033(5) 0.032(5) -0.002(3) 0.000(3) 0.001(3) O12 0.043(6) 0.044(6) 0.043(6) 0.001(3) 0.000(3) 0.001(3) OW1 0.024(5) 0.026(5) 0.025(5) -0.002(3) -0.001(3) -0.001(3) OW2 0.026(5) 0.022(5) 0.024(5) 0.001(3) 0.002(3) 0.001(3) OW3 0.024(5) 0.024(5) 0.025(5) 0.001(3) 0.002(3) 0.000(3) OW4 0.030(5) 0.030(5) 0.031(5) -0.001(3) 0.000(3) 0.001(3) OW5 0.044(6) 0.044(6) 0.045(6) 0.000(3) 0.001(3) 0.000(3) OW6 0.031(6) 0.035(6) 0.031(6) -0.002(3) 0.002(3) -0.002(3) OW7 0.061(7) 0.061(7) 0.062(7) 0.000(3) 0.000(3) -0.001(3) OW8 0.063(7) 0.063(7) 0.065(7) 0.001(3) 0.000(3) -0.001(3) OW9 0.050(6) 0.051(6) 0.052(6) 0.002(3) 0.002(3) 0.001(3) OW10 0.082(8) 0.082(8) 0.084(8) 0.001(3) -0.003(3) 0.000(3) OW11 0.111(10) 0.113(10) 0.114(10) 0.001(3) 0.001(3) -0.001(3) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag Pt1 N1 1.99(2) . ? Pt1 N2 2.010(19) . ? Pt1 Cl2 2.282(7) . ? Pt1 Cl1 2.297(6) . ? Pt1 Pt2 3.3692(16) 4_456 ? Pt2 N4 1.99(2) . ? Pt2 N3 1.998(19) . ? Pt2 Cl3 2.293(6) . ? Pt2 Cl4 2.301(6) . ? Pt2 Pt3 3.2727(16) 5_766 ? Pt3 N6 1.989(17) . ? Pt3 N5 2.016(18) . ? Pt3 Cl6 2.294(7) . ? Pt3 Cl5 2.295(7) . ? Gd1 O5 2.232(18) . ? Gd1 O3 2.313(16) . ? Gd1 O11 2.335(16) . ? Gd1 OW5 2.357(18) . ? Gd1 OW6 2.462(15) . ? Gd1 O1 2.479(16) 6_657 ? Gd1 OW4 2.484(16) . ? Gd1 O2 2.488(16) 6_657 ? Gd2 O6 2.307(17) . ? Gd2 O9 2.315(15) 2_664 ? Gd2 OW1 2.326(15) . ? Gd2 O4 2.330(17) . ? Gd2 OW3 2.370(15) . ? Gd2 OW2 2.465(15) . ? Gd2 O8 2.485(16) 6_556 ? Gd2 O7 2.499(15) 6_556 ? O1 C4 1.23(3) . ? O2 C4 1.27(3) . ? O3 C8 1.27(2) . ? O4 C8 1.29(2) . ? O5 C13 1.27(3) . ? O6 C13 1.25(3) . ? O7 C24 1.25(3) . ? O8 C24 1.25(3) . ? O9 C28 1.30(3) . ? O10 C28 1.28(3) . ? O11 C29 1.27(3) . ? O12 C29 1.27(3) . ? N1 C1 1.32(3) . ? N1 C3 1.36(3) . ? N2 C10 1.33(3) . ? N2 C12 1.36(3) . ? N3 C14 1.32(3) . ? N3 C19 1.36(3) . ? N4 C15 1.38(3) . ? N4 C21 1.40(3) . ? N5 C25 1.29(2) . ? N5 C26 1.33(3) . ? N6 C32 1.32(3) . ? N6 C30 1.43(3) . ? C1 C2 1.37(3) . ? C1 H1 0.9306 . ? C2 C5 1.37(3) . ? C2 C4 1.51(3) . ? C3 C12 1.44(3) . ? C3 C6 1.45(3) . ? C5 C6 1.44(3) . ? C5 H5 0.9294 . ? C6 H6 0.9300 . ? C7 C12 1.37(3) . ? C7 C11 1.41(3) . ? C7 H7 0.9313 . ? C8 C9 1.47(3) . ? C9 C11 1.35(3) . ? C9 C10 1.37(3) . ? C10 H10 0.9318 . ? C11 H11 0.9293 . ? C13 C17 1.46(3) . ? C14 C17 1.40(3) . ? C14 H14 0.9323 . ? C15 C23 1.39(3) . ? C15 H15 0.9290 . ? C16 C22 1.37(3) . ? C16 C23 1.39(3) . ? C16 H16 0.9308 . ? C17 C18 1.33(3) . ? C18 C20 1.35(3) . ? C18 H18 0.9306 . ? C19 C20 1.38(3) . ? C19 C21 1.45(3) . ? C20 H20 0.9287 . ? C21 C22 1.36(3) . ? C22 H22 0.9303 . ? C23 C24 1.48(3) . ? C24 Gd2 2.82(3) 6_656 ? C25 C33 1.30(3) . ? C25 H25 0.9301 . ? C26 C31 1.38(3) . ? C26 C30 1.42(3) . ? C27 C36 1.37(3) . ? C27 C32 1.38(3) . ? C27 C29 1.44(3) . ? C28 C33 1.46(3) . ? C30 C34 1.35(3) . ? C31 C35 1.34(3) . ? C31 H31 0.9309 . ? C32 H32 0.9305 . ? C33 C35 1.39(3) . ? C34 C36 1.37(3) . ? C34 H34 0.9286 . ? C35 H35 0.9294 . ? C36 H36 0.9288 . ? 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 Pt1 N2 81.4(8) . . ? N1 Pt1 Cl2 176.4(6) . . ? N1 Pt1 Cl1 94.9(6) . . ? N1 Pt1 C3 26.1(7) . . ? N1 Pt1 C12 55.4(8) . . ? N1 Pt1 C1 20.1(7) . . ? N1 Pt1 C10 102.2(7) . . ? N1 Pt1 Pt2 84.7(6) . 4_456 ? N1 Pt1 Pt3 65.7(6) . . ? N1 Pt1 Pt2 113.2(6) . . ? N1 C1 C2 126(2) . . ? N1 C3 C12 116(2) . . ? N1 C3 C6 122(2) . . ? N2 Pt1 Pt2 31.8(6) . . ? N2 Pt1 Pt3 23.3(6) . . ? N2 Pt1 Pt2 78.7(5) . 4_456 ? N2 Pt1 C1 101.5(7) . . ? N2 Pt1 C3 55.4(8) . . ? N2 Pt1 Cl2 95.1(6) . . ? N2 Pt1 Cl1 175.4(6) . . ? N2 C10 C9 121(2) . . ? N2 C12 C7 120(2) . . ? N2 C12 C3 115(2) . . ? N3 Pt2 Cl3 96.1(6) . . ? N3 Pt2 Cl4 176.2(6) . . ? N3 Pt2 C15 102.2(7) . . ? N3 Pt2 Pt3 86.9(6) . 5_766 ? N3 Pt2 Pt1 79.3(6) . 4_556 ? N3 Pt2 Pt3 80.3(6) . . ? N3 C14 C17 122(2) . . ? N3 C19 C20 121(2) . . ? N3 C19 C21 113(2) . . ? N4 Pt2 N3 80.0(8) . . ? N4 Pt2 Cl3 175.9(6) . . ? N4 Pt2 Cl4 96.2(6) . . ? N4 Pt2 C19 55.3(7) . . ? N4 Pt2 C14 101.5(8) . . ? N4 Pt2 Pt3 87.2(6) . 5_766 ? N4 Pt2 Pt1 84.9(6) . 4_556 ? N4 Pt2 Pt3 154.7(6) . . ? N4 Pt2 Pt1 114.4(6) . . ? N4 C15 C23 119(2) . . ? N4 C21 C19 114(2) . . ? N5 Pt3 Cl6 96.3(5) . . ? N5 Pt3 Cl5 176.0(5) . . ? N5 Pt3 Cl6 96.3(5) . . ? N5 Pt3 Cl5 176.0(5) . . ? N5 Pt3 C30 53.9(6) . . ? N5 Pt3 Pt1 63.6(5) . . ? N5 Pt3 Pt2 90.1(5) . 5_766 ? N5 Pt3 C32 100.0(7) . . ? N5 Pt3 Pt2 144.1(5) . . ? N5 C25 C33 130(2) . . ? N5 C26 C31 119(2) . . ? N5 C26 C30 118(2) . . ? N6 Pt3 N5 80.6(8) . . ? N6 Pt3 Cl6 176.6(5) . . ? N6 Pt3 Cl5 95.4(5) . . ? N6 Pt3 N5 80.6(8) . . ? N6 Pt3 Cl6 176.6(5) . . ? N6 Pt3 Cl5 95.4(5) . . ? N6 Pt3 C26 55.4(7) . . ? N6 Pt3 C25 100.1(7) . . ? N6 Pt3 C32 19.4(7) . . ? N6 Pt3 Pt2 85.7(5) . 5_766 ? N6 Pt3 Pt2 67.9(5) . . ? N6 C32 C27 127(2) . . ? C1 N1 C3 118(2) . . ? C1 N1 Pt1 128.5(17) . . ? C1 Pt1 C10 122.3(6) . . ? C1 Pt1 Pt2 89.9(4) . 4_456 ? C1 Pt1 Pt3 84.6(5) . . ? C1 Pt1 Pt2 133.3(5) . . ? C1 C2 C5 118(2) . . ? C1 C2 C4 120(2) . . ? C2 C1 Pt1 157.3(18) . . ? C2 C1 Pt1 157.3(18) . . ? C2 C4 Gd1 178.7(19) . 6_557 ? C2 C5 C6 120(2) . . ? C3 Pt1 C1 46.2(7) . . ? C3 Pt1 C12 29.3(7) . . ? C3 Pt1 C10 76.1(7) . . ? C3 Pt1 Pt3 41.8(5) . . ? C3 Pt1 Pt2 87.1(5) . . ? C3 N1 Pt1 113.8(16) . . ? C3 C12 Pt1 74.4(15) . . ? C4 O1 Gd1 93.0(15) . 6_557 ? C4 O2 Gd1 91.7(15) . 6_557 ? C5 C2 C4 122(2) . . ? C5 C6 C3 116(2) . . ? C6 C3 Pt1 161.6(18) . . ? C7 C12 C3 125(3) . . ? C7 C12 Pt1 160(2) . . ? C8 O3 Gd1 157.0(15) . . ? C8 O4 Gd2 144.6(15) . . ? C9 C10 Pt1 153.3(17) . . ? C9 C11 C7 116(2) . . ? C10 Pt1 Pt2 81.0(4) . 4_456 ? C10 Pt1 Pt3 40.4(4) . . ? C10 Pt1 Pt2 11.0(4) . . ? C10 N2 C12 119(2) . . ? C10 N2 Pt1 127.0(16) . . ? C10 C9 C8 117(2) . . ? Cl1 Pt1 C12 150.1(6) . . ? Cl1 Pt1 C1 74.7(5) . . ? Cl1 Pt1 C10 162.7(5) . . ? Cl1 Pt1 C3 121.0(5) . . ? Cl1 Pt1 Pt2 103.82(17) . 4_456 ? Cl1 Pt1 Pt3 152.15(17) . . ? Cl1 Pt1 Pt2 151.88(17) . . ? C11 C9 C10 122(2) . . ? C11 C9 C8 121(2) . . ? Cl2 Pt1 Cl1 88.6(2) . . ? Cl2 Pt1 C3 150.4(5) . . ? Cl2 Pt1 C12 121.2(6) . . ? Cl2 Pt1 C1 163.3(5) . . ? C12 Pt1 C1 75.5(7) . . ? Cl2 Pt1 C10 74.4(5) . . ? C12 Pt1 C10 46.8(7) . . ? Cl2 Pt1 Pt2 93.57(17) . 4_456 ? C12 Pt1 Pt2 78.5(5) . 4_456 ? Cl2 Pt1 Pt3 111.32(16) . . ? C12 Pt1 Pt3 18.4(5) . . ? Cl2 Pt1 Pt2 63.38(16) . . ? C12 Pt1 Pt2 57.8(5) . . ? C12 N2 Pt1 113.7(17) . . ? C12 C3 C6 122(2) . . ? C12 C3 Pt1 76.3(15) . . ? C12 C7 C11 121(2) . . ? Cl3 Pt2 Cl4 87.7(2) . . ? Cl3 Pt2 C21 149.9(5) . . ? Cl3 Pt2 C19 120.8(5) . . ? Cl3 Pt2 Cl4 87.7(2) . . ? Cl3 Pt2 C21 149.9(5) . . ? Cl3 Pt2 C19 120.8(5) . . ? Cl3 Pt2 C14 74.6(5) . . ? Cl3 Pt2 C15 161.8(5) . . ? Cl3 Pt2 Pt3 93.75(16) . 5_766 ? Cl3 Pt2 Pt1 93.35(16) . 4_556 ? Cl3 Pt2 Pt3 23.18(16) . . ? Cl3 Pt2 Pt1 61.64(16) . . ? C13 O5 Gd1 161.6(18) . . ? C13 O6 Gd2 158.5(17) . . ? Cl4 Pt2 C21 122.3(5) . . ? Cl4 Pt2 C19 151.4(5) . . ? Cl4 Pt2 C21 122.3(5) . . ? Cl4 Pt2 C19 151.4(5) . . ? Cl4 Pt2 C14 162.2(5) . . ? Cl4 Pt2 C15 74.0(5) . . ? C14 Pt2 C15 123.6(7) . . ? Cl4 Pt2 Pt3 93.06(16) . 5_766 ? C14 Pt2 Pt3 85.9(4) . 5_766 ? Cl4 Pt2 Pt1 100.35(16) . 4_556 ? C14 Pt2 Pt1 83.3(4) . 4_556 ? Cl4 Pt2 Pt3 103.44(16) . . ? C14 Pt2 Pt3 59.1(5) . . ? Cl4 Pt2 Pt1 149.26(16) . . ? C14 Pt2 Pt1 13.8(5) . . ? C14 N3 C19 118(2) . . ? C14 N3 Pt2 124.6(16) . . ? C14 C17 C13 116(2) . . ? C15 C23 C24 119(2) . . ? C15 Pt2 Pt3 87.2(4) . 5_766 ? C15 Pt2 Pt1 90.1(4) . 4_556 ? C15 Pt2 Pt3 163.1(4) . . ? C15 Pt2 Pt1 136.6(5) . . ? Cl5 Pt3 C26 150.8(5) . . ? Cl5 Pt3 C30 122.1(5) . . ? Cl5 Pt3 C32 76.1(5) . . ? Cl5 Pt3 C25 164.4(4) . . ? Cl5 Pt3 Pt2 90.31(17) . 5_766 ? Cl5 Pt3 Pt1 112.49(16) . . ? Cl5 Pt3 Pt2 32.14(16) . . ? C15 N4 C21 120(2) . . ? C15 N4 Pt2 124.8(17) . . ? Cl6 Pt3 Cl5 87.7(2) . . ? Cl6 Pt3 C26 121.5(5) . . ? Cl6 Pt3 C30 150.1(5) . . ? Cl6 Pt3 C25 76.8(4) . . ? Cl6 Pt3 C32 163.5(5) . . ? Cl6 Pt3 Pt2 95.68(17) . 5_766 ? Cl6 Pt3 Pt2 95.68(17) . 5_766 ? Cl6 Pt3 Pt1 149.47(17) . . ? Cl6 Pt3 Pt2 114.62(17) . . ? C16 C23 C15 120(2) . . ? C16 C23 C24 122(2) . . ? C17 C14 Pt2 156.0(17) . . ? C17 C18 C20 121(2) . . ? C18 C17 C14 118(2) . . ? C18 C17 C13 126(2) . . ? C18 C20 C19 119(2) . . ? C19 Pt2 C14 46.3(6) . . ? C19 Pt2 C15 77.5(6) . . ? C19 Pt2 Pt3 87.2(4) . 5_766 ? C19 Pt2 Pt1 77.9(4) . 4_556 ? C19 Pt2 Pt3 104.3(4) . . ? C19 Pt2 Pt1 59.1(4) . . ? C19 N3 Pt2 117.4(15) . . ? C19 C21 Pt2 75.6(13) . . ? C20 C19 C21 126(2) . . ? C20 C19 Pt2 159.1(17) . . ? C21 C19 Pt2 75.3(13) . . ? C21 C22 C16 120(2) . . ? C21 Pt2 C14 75.4(6) . . ? C21 Pt2 C19 29.2(6) . . ? C21 Pt2 C15 48.3(7) . . ? C21 Pt2 Pt3 86.8(4) . 5_766 ? C21 Pt2 Pt1 80.5(4) . 4_556 ? C21 Pt2 Pt3 131.9(5) . . ? C21 Pt2 Pt1 88.3(5) . . ? C21 N4 Pt2 115.1(15) . . ? C22 C16 C23 120(2) . . ? C22 C21 N4 120(2) . . ? C22 C21 C19 126(2) . . ? C22 C21 Pt2 158.7(18) . . ? C23 C15 Pt2 152.2(17) . . ? C23 C24 Gd2 166.9(17) . 6_656 ? C24 O7 Gd2 91.4(15) . 6_656 ? C24 O8 Gd2 92.1(15) . 6_656 ? C25 Pt3 C32 119.5(6) . . ? C25 Pt3 Pt2 92.1(4) . 5_766 ? C25 Pt3 Pt1 81.6(4) . . ? C25 Pt3 Pt2 158.8(4) . . ? C25 C33 C35 114(2) . . ? C25 C33 C28 125(2) . . ? C25 N5 C26 116.3(19) . . ? C25 N5 Pt3 129.0(15) . . ? C26 Pt3 C30 28.7(6) . . ? C26 Pt3 C25 44.7(6) . . ? C26 Pt3 C32 74.7(6) . . ? C26 Pt3 Pt2 88.5(5) . 5_766 ? C26 Pt3 Pt1 40.9(5) . . ? C26 Pt3 Pt2 120.8(5) . . ? C26 N5 Pt3 114.6(15) . . ? C26 C30 N6 112.1(18) . . ? C26 C30 Pt3 73.5(13) . . ? C27 C32 Pt3 156.8(18) . . ? C28 O9 Gd2 136.5(15) . 2_665 ? C29 O11 Gd1 128.0(15) . . ? C30 Pt3 C25 73.4(6) . . ? C30 Pt3 C32 46.0(6) . . ? C30 Pt3 Pt2 87.5(4) . 5_766 ? C30 Pt3 Pt1 20.7(4) . . ? C30 Pt3 Pt2 93.2(4) . . ? C30 N6 Pt3 114.7(14) . . ? C32 Pt3 Pt2 86.9(4) . 5_766 ? C32 Pt3 Pt1 41.9(5) . . ? C32 Pt3 Pt2 49.2(5) . . ? C32 N6 C30 114.6(18) . . ? C32 N6 Pt3 130.5(16) . . ? C30 C26 Pt3 77.8(13) . . ? C30 C34 C36 122(2) . . ? C31 C26 C30 123(2) . . ? C31 C26 Pt3 159.6(18) . . ? C31 C35 C33 120(2) . . ? C32 C27 C29 117(2) . . ? C33 C25 Pt3 161.2(16) . . ? C34 C30 C26 127(2) . . ? C34 C30 N6 121(2) . . ? C34 C30 Pt3 159.1(17) . . ? C34 C36 C27 119(3) . . ? C35 C31 C26 120(2) . . ? C35 C33 C28 121(2) . . ? C36 C27 C32 117(3) . . ? C36 C27 C29 126(3) . . ? Pt1 Pt2 Pt3 106.76(3) 4_556 . ? Pt1 Pt2 Pt1 80.34(3) 4_556 . ? Pt1 Pt3 Pt2 80.650(11) . . ? Pt2 Pt1 Pt3 94.45(3) 4_456 . ? Pt2 Pt1 Pt2 81.76(3) 4_456 . ? Pt2 Pt3 Pt1 106.43(3) 5_766 . ? Pt2 Pt3 Pt2 103.88(3) 5_766 . ? Pt3 Pt1 Pt2 50.771(12) . . ? Pt3 Pt2 Pt1 165.05(4) 5_766 4_556 ? Pt3 Pt2 Pt3 76.12(3) 5_766 . ? Pt3 Pt2 Pt1 91.52(3) 5_766 . ? Pt3 Pt2 Pt1 48.579(12) . . ? O1 Gd1 OW4 76.3(5) 6_657 . ? O1 Gd1 O2 52.5(5) 6_657 6_657 ? O1 Gd1 C4 25.8(6) 6_657 6_657 ? O1 C4 O2 123(2) . . ? O1 C4 C2 120(2) . . ? O1 C4 Gd1 61.2(13) . 6_557 ? O2 Gd1 C4 26.7(6) 6_657 6_657 ? O2 C4 C2 117(2) . . ? O2 C4 Gd1 61.6(13) . 6_557 ? O3 Gd1 O2 75.6(6) . 6_657 ? O3 Gd1 O11 77.9(6) . . ? O3 Gd1 OW5 73.9(6) . . ? O3 Gd1 OW6 143.0(5) . . ? O3 Gd1 O1 127.7(5) . 6_657 ? O3 Gd1 OW4 136.2(5) . . ? O3 Gd1 C4 102.0(7) . 6_657 ? O3 C8 O4 122(2) . . ? O3 C8 C9 118(2) . . ? O4 Gd2 OW3 83.6(5) . . ? O4 Gd2 OW2 70.5(5) . . ? O4 Gd2 O8 135.2(5) . 6_556 ? O4 Gd2 O7 128.6(5) . 6_556 ? O4 Gd2 C24 140.9(7) . 6_556 ? O4 C8 C9 120(2) . . ? O5 Gd1 O3 83.4(6) . . ? O5 Gd1 O11 92.8(6) . . ? O5 Gd1 OW5 95.4(6) . . ? O5 Gd1 OW6 80.5(6) . . ? O5 Gd1 O1 148.3(6) . 6_657 ? O5 Gd1 OW4 75.9(6) . . ? O5 Gd1 O2 159.0(6) . 6_657 ? O5 Gd1 C4 173.7(7) . 6_657 ? O5 C13 C17 120(3) . . ? O6 Gd2 O9 90.6(5) . 2_664 ? O6 Gd2 OW1 94.2(5) . . ? O6 Gd2 O4 86.6(6) . . ? O6 Gd2 OW3 160.2(6) . . ? O6 Gd2 OW2 82.7(5) . . ? O6 Gd2 O8 74.7(6) . 6_556 ? O6 Gd2 O7 127.0(6) . 6_556 ? O6 Gd2 C24 100.9(7) . 6_556 ? O6 C13 O5 122(3) . . ? O6 C13 C17 117(3) . . ? O7 C24 Gd2 62.3(13) . 6_656 ? O7 C24 C23 119(2) . . ? O7 Gd2 C24 26.4(6) 6_556 6_556 ? O8 Gd2 O7 52.4(5) 6_556 6_556 ? O8 Gd2 C24 26.3(6) 6_556 6_556 ? O8 C24 O7 123(2) . . ? O8 C24 C23 118(2) . . ? O8 C24 Gd2 61.6(13) . 6_656 ? O9 Gd2 OW1 147.7(6) 2_664 . ? O9 Gd2 O4 145.3(6) 2_664 . ? O9 Gd2 OW3 87.7(5) 2_664 . ? O9 Gd2 OW2 74.8(5) 2_664 . ? O9 Gd2 O8 76.4(5) 2_664 6_556 ? O9 Gd2 O7 79.3(5) 2_664 6_556 ? O9 Gd2 C24 73.5(6) 2_664 6_556 ? O9 C28 C33 121(2) . . ? O10 C28 O9 120(2) . . ? O10 C28 C33 119(2) . . ? O11 Gd1 OW5 149.4(6) . . ? O11 Gd1 OW6 70.0(5) . . ? O11 Gd1 O1 99.0(5) . 6_657 ? O11 Gd1 OW4 140.4(6) . . ? O11 Gd1 O2 82.7(6) . 6_657 ? O11 Gd1 C4 91.4(7) . 6_657 ? O11 C29 O12 121(2) . . ? O11 C29 C27 121(2) . . ? O12 C29 C27 119(2) . . ? OW1 Gd2 O4 66.9(6) . . ? OW1 Gd2 OW3 97.8(5) . . ? OW1 Gd2 OW2 137.4(5) . . ? OW1 Gd2 O8 74.2(5) . 6_556 ? OW1 Gd2 O7 72.4(5) . 6_556 ? OW1 Gd2 C24 74.2(6) . 6_556 ? OW2 Gd2 O8 143.0(5) . 6_556 ? OW2 Gd2 O7 140.6(5) . 6_556 ? OW3 Gd2 OW2 77.7(5) . . ? OW3 Gd2 O8 123.9(5) . 6_556 ? OW3 Gd2 O7 72.0(5) . 6_556 ? OW3 Gd2 C24 97.6(7) . 6_556 ? OW4 Gd1 O2 120.0(5) . 6_657 ? OW4 Gd1 C4 97.9(7) . 6_657 ? OW5 Gd1 OW6 140.5(6) . . ? OW5 Gd1 O1 89.2(6) . 6_657 ? OW5 Gd1 OW4 70.2(6) . . ? OW5 Gd1 O2 79.1(6) . 6_657 ? OW5 Gd1 C4 83.3(7) . 6_657 ? OW6 Gd1 O1 76.2(5) . 6_657 ? OW6 Gd1 OW4 70.8(5) . . ? OW6 Gd1 O2 116.6(5) . 6_657 ? OW6 Gd1 C4 96.5(7) . 6_657 ? N1 C1 H1 116.9 . . ? C2 C2 H1 117.0 . . ? C2 C5 H5 120.0 . . ? C6 C5 H5 120.0 . . ? C5 C6 H6 122.2 . . ? C3 C6 H6 122.2 . . ? C12 C7 H7 119.4 . . ? C11 C7 H7 119.7 . . ? C7 C11 H11 121.9 . . ? C9 C11 H11 121.8 . . ? N2 C10 H10 119.4 . . ? C9 C10 H10 119.3 . . ? N3 C14 H14 118.9 . . ? C17 C14 H14 118.8 . . ? N4 C15 H15 120.2 . . ? C23 C15 H15 120.4 . . ? C23 C16 H16 119.8 . . ? C22 C16 H16 119.7 . . ? C16 C22 H22 119.8 . . ? C21 C22 H22 119.9 . . ? C19 C20 H20 120.5 . . ? C18 C20 H20 120.6 . . ? C17 C18 H18 119.4 . . ? C20 C18 H18 119.2 . . ? N5 C25 H25 115.0 . . ? C33 C25 H25 115.0 . . ? N6 C32 H32 116.6 . . ? C27 C32 H32 116.7 . . ? C33 C35 H35 120.1 . . ? C31 C35 H35 120.3 . . ? C35 C31 H31 120.0 . . ? C26 C31 H31 120.0 . . ? C30 C34 H34 119.1 . . ? C36 C34 H34 119.0 . . ? C34 C36 H36 120.7 . . ? C27 C36 H36 120.7 . . ? _diffrn_measured_fraction_theta_max 0.995 _diffrn_reflns_theta_full 18.67 _diffrn_measured_fraction_theta_full 0.995 _refine_diff_density_max 1.438 _refine_diff_density_min -0.864 _refine_diff_density_rms 0.221 _vrf_THETM01_3genPt-Gd-MOF ; PROBLEM: The value of sine(theta_max)/wavelength is less than 0.550 RESPONSE: We have a sample limiting system. The crystal quality is poor. Many crystals were tested, and the reported collection is the best of the series. ; _vrf_PLAT023_3genPt-Gd-MOF ; PROBLEM: Resolution (too) Low [sin(th)/Lambda < 0.6]..... 18.67 Deg. RESPONSE: This problem is related to_THETM01. We have a sample limiting system. Many crystals were tested, and the reported collection is the best of the series. ; _vrf_PLAT027_3genPt-Gd-MOF ; PROBLEM: diffrn_reflns_theta_full (too) Low ............ 18.67 Deg. RESPONSE: This problem is related to_THETM01 and _PLAT023 We have a sample limiting system. Many crystals were tested, and the reported collection is the best of the series. ; _vrf_PLAT201_3genPt-Gd-MOF ; PROBLEM: Isotropic non-H Atoms in Main Residue(s) ....... 42 RESPONSE: This problem is related to_THETM01 and _PLAT023 The lack of high angle data prevents anisotropic refinement ot the displacement parameters of the lighter elements. Combination of poor crystal quality and presence of heavy elements like Pt and Gd together with organic species have caused problem to obtain reliable anisotropic displacement parameters in the organic part. ; _vrf_PLAT220_3genPt-Gd-MOF ; PROBLEM: Large Non-Solvent C Ueq(max)/Ueq(min) ... 10.00 Ratio RESPONSE: This problem is related to_THETM01 and _PLAT023 The lack of high angle data prevents high quality refinement ot the displacement parameters of the lighter elements. Combination of poor crystal quality and presence of heavy elements like Pt and Gd together with organic species have also caused problem to refine displacement parameters in the organic part. ; _vrf_PLAT222_3genPt-Gd-MOF ; PROBLEM: Large Non-Solvent H Ueq(max)/Ueq(min) ... 9.75 Ratio RESPONSE: This problem is related to_PLAT220. The reported Hydrogen atoms are calculated using the HFIX command in SHELX-97 (Sheldrick, 1997). The displacement parameter of Hydrogen is depended of the host Carbon atom. ; _vrf_PLAT306_3genPt-Gd-MOF ; PROBLEM: Isolated Oxygen Atom (H-atoms Missing ?) ....... OW7 RESPONSE: The isolated OW-atoms are solvent water molecules located in the nano pores. It is not possible to locate Hydrogen atoms to all water molecules. This might be due to the low resolution or disorder in the orientation of the water molecules. ; _vrf_PLAT762_3genPt-Gd-MOF ; PROBLEM: CIF Contains no X-Y-H or H-Y-H Angles .......... ? RESPONSE: No X-H angles have been refiend. ; _vrf_RINTA01_3genPt-Gd-MOF ; PROBLEM: The value of Rint is greater than 0.15 RESPONSE: This problem is addressed to the poor crystal quality. ; _vrf_PLAT020_3genPt-Gd-MOF ; PROBLEM: The value of Rint is greater than 0.10 ......... 0.20 RESPONSE: This problem is addressed to the poor crystal quality. ; _vrf_PLAT342_3genPt-Gd-MOF ; PROBLEM: Low Bond Precision on C-C bonds (x 1000) Ang ... 34 RESPONSE: The lack of high resolution data prevents high quality refinement of the lighter elements. Combination of poor crystal quality and presence of heavy elements like Pt and Gd together with organic species may affect the refinement quality of the realtively weakly scattering elements. ; _vrf_PLAT430_3genPt-Gd-MOF ; PROBLEM: Short Inter D...A Contact OW1 .. OW8 .. 2.71 Ang. RESPONSE: D...A distances around this value are typical for free water molecules confined in solids and have been reported before (Natheret al., Acta Cryst. (2001). C57, 111-112). ; _vrf_REFNR01_3genPt-Gd-MOF ; PROBLEM: Ratio of reflections to parameters is < 10 for a centrosymmetric structure. RESPONSE: The lack of high angle data reducses also the number of observed reflections. ; _vrf_PLAT431_3genPt-Gd-MOF ; PROBLEM: Short Inter HL..A Contact Cl5 .. OW7 .. 3.15 Ang. RESPONSE: HL..A distances around this value has been reported before (Bolte et al., Acta Cryst. (2000). C56, 1338-1342). ; _vrf_PLAT720_3genPt-Gd-MOF ; PROBLEM: Number of Unusual/Non-Standard Label(s) ........ 11 RESPONSE: These labels are used to distinguish Oxygen atoms from water and carboxylate. ; _vrf_PLAT088_3genPt-Gd-MOF ; PROBLEM: Poor Data / Parameter Ratio .................... 8.07 RESPONSE: The lack of high angle data and the complexity of the structure result in poor data/parameter ratio. ; _vrf_PLAT241_3genPt-Gd-MOF ; PROBLEM: check High Ueq as Compared to Neighbors for C16 RESPONSE: This problem is related to_THETM01 and _PLAT023 The lack of high angle data prevents high quality refinement ot the displacement parameters of the lighter elements. Combination of poor crystal quality and presence of heavy elements like Pt and Gd together with organic species have also caused problem to refine displacement parameters in the organic part. ; _vrf_PLAT068_3genPt-Gd-MOF ; PROBLEM: Reported F000 Differs from Calcd (or Missing) ... ? RESPONSE: The reported value is considering Hydrogen atoms in water which is not located from the electron density map. ; _vrf_CHEMW03_3genPt-Gd-MOF ; RESPONSE: The reported value is considering Hydrogen atoms in water which is not located from the electron density map. ; _vrf_PLAT041_3genPt-Gd-MOF ; PROBLEM: Calc. and Rep. SumFormula Strings Differs .... ? RESPONSE: The reported string is considering Hydrogen atoms in water which is not located from the electron density map. ; _vrf_PLAT042_3genPt-Gd-MOF ; PROBLEM: Calc. and Rep. MoietyFormula Strings Differs .... ? RESPONSE: The reported string is considering Hydrogen atoms in water which is not located from the electron density map. ; _vrf_PLAT043_3genPt-Gd-MOF ; PROBLEM: Check Reported Molecular Weight ................ 2037.21 RESPONSE: The reported value is considering Hydrogen atoms in water which is not located from the electron density map. ; _vrf_PLAT044_3genPt-Gd-MOF ; PROBLEM: Calculated and Reported Dx Differ .............. ? RESPONSE: The reported value is considering Hydrogen atoms in water which is omitted in the refinement. ;