# Electronic Supplementary Material (ESI) for Dalton Transactions # This journal is © The Royal Society of Chemistry 2011 data_global _journal_name_full 'Dalton Trans.' _journal_coden_cambridge 0222 _journal_year ? _journal_volume ? _journal_page_first ? loop_ _publ_author_name _publ_author_address C.Lemouchi ; Laboratoire MOLTECH-Anjou, Universit\'e d'Angers, CNRS, 2 Boulevard Lavoisier, 49045 Angers, France ; L.Zorina ; Institute of Solid State Physics, RAS, 142432 Chernogolovka, Russia ; P.Zwietek ; Laboratoire de Physique des Solides, CNRS, Universit\'e de Paris-Sud, 91405 Orsay, France ; P.Batail ; Laboratoire MOLTECH-Anjou, Universit\'e d'Angers, CNRS, 2 Boulevard Lavoisier, 49045 Angers, France ; _publ_contact_author_address ; Laboratoire MOLTECH-Anjou, Universit\'e d'Angers, CNRS, 2 Boulevard Lavoisier, 49045 Angers, France ; _publ_contact_author_email patrick.batail@univ-angers.fr _publ_contact_author_name 'Dr. Patrick Batail' data_(1-pyr-diethynilbicyclo[2,2,2]octaneH+)2[OH2]2[Pt(CN)4]2- _database_code_depnum_ccdc_archive 'CCDC 815402' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_compound_source 'synthesis as described' _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety '2(C17 H18 N), C4 N4 Pt, 2(H2 O)' _chemical_formula_sum 'C38 H40 N6 O2 Pt' _chemical_formula_weight 807.85 loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Pt Pt -1.7033 8.3905 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting monoclinic _symmetry_space_group_name_H-M 'P 21/c' _symmetry_space_group_name_Hall '-P 2ybc' loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, y+1/2, -z+1/2' '-x, -y, -z' 'x, -y-1/2, z-1/2' _cell_length_a 13.5093(7) _cell_length_b 10.2580(3) _cell_length_c 13.9549(6) _cell_angle_alpha 90.00 _cell_angle_beta 109.925(5) _cell_angle_gamma 90.00 _cell_volume 1818.09(14) _cell_formula_units_Z 2 _cell_measurement_temperature 295(2) _cell_measurement_reflns_used 20763 _cell_measurement_theta_min 4 _cell_measurement_theta_max 30 _exptl_crystal_description plate _exptl_crystal_colour colorless _exptl_crystal_size_max 0.31 _exptl_crystal_size_mid 0.23 _exptl_crystal_size_min 0.15 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.476 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 808 _exptl_absorpt_coefficient_mu 3.899 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.312 _exptl_absorpt_correction_T_max 0.361 _exptl_absorpt_process_details sadabs _exptl_special_details ; ? ; _diffrn_ambient_temperature 295(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'Bruker Nonius KappaCCD' _diffrn_measurement_method 'combined \f and \w-scans' _diffrn_measurement_device '\k-geometry diffractometer' _diffrn_detector_area_resol_mean 9 _diffrn_standards_decay_% 0 _diffrn_reflns_number 49306 _diffrn_reflns_av_R_equivalents 0.0292 _diffrn_reflns_av_sigmaI/netI 0.0239 _diffrn_reflns_limit_h_min -20 _diffrn_reflns_limit_h_max 21 _diffrn_reflns_limit_k_min -16 _diffrn_reflns_limit_k_max 16 _diffrn_reflns_limit_l_min -22 _diffrn_reflns_limit_l_max 22 _diffrn_reflns_theta_min 3.69 _diffrn_reflns_theta_max 34.97 _reflns_number_total 7949 _reflns_number_gt 4810 _reflns_threshold_expression >2\s(I) _computing_data_collection 'Collect (Nonius BV, 1997-2000)' _computing_cell_refinement 'Dirax/lsq (Duisenberg & Schreurs, 1989-2000)' _computing_data_reduction 'EvalCCD (Duisenberg & Schreurs 1990-2000)' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1997)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics ? _computing_publication_material 'WinGX publication routines (Farrugia, 1999)' _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^ > 2\s(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^)+(0.0141P)^2^+1.2071P] 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 mixed _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 7949 _refine_ls_number_parameters 221 _refine_ls_number_restraints 1 _refine_ls_R_factor_all 0.0603 _refine_ls_R_factor_gt 0.0221 _refine_ls_wR_factor_ref 0.0503 _refine_ls_wR_factor_gt 0.0423 _refine_ls_goodness_of_fit_ref 1.018 _refine_ls_restrained_S_all 1.018 _refine_ls_shift/su_max 0.004 _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 Pt01 Pt 0.0000 0.5000 0.5000 0.03239(3) Uani 1 2 d S . . N01 N -0.04775(17) 0.7956(2) 0.44870(16) 0.0509(5) Uani 1 1 d . . . N02 N 0.12781(14) 0.4980(2) 0.34931(14) 0.0503(4) Uani 1 1 d . . . C02 C 0.08269(14) 0.4974(2) 0.40580(13) 0.0385(4) Uani 1 1 d . . . C01 C -0.03108(16) 0.6870(2) 0.46844(16) 0.0411(5) Uani 1 1 d . . . C1 C 0.32849(18) 0.8506(2) 0.54390(18) 0.0479(5) Uani 1 1 d . . . H1 H 0.2824 0.8767 0.5768 0.057 Uiso 1 1 calc R . . C2 C 0.38707(16) 0.8174(2) 0.50200(16) 0.0381(4) Uani 1 1 d . . . C3 C 0.46209(15) 0.77145(18) 0.45372(14) 0.0304(4) Uani 1 1 d . . . C4 C 0.42408(16) 0.6424(2) 0.39732(16) 0.0389(4) Uani 1 1 d . . . H4A H 0.4141 0.5785 0.4444 0.047 Uiso 1 1 calc R . . H4B H 0.3569 0.6559 0.3436 0.047 Uiso 1 1 calc R . . C5 C 0.47483(16) 0.8712(2) 0.37617(16) 0.0378(4) Uani 1 1 d . . . H5A H 0.4067 0.8887 0.3251 0.045 Uiso 1 1 calc R . . H5B H 0.5020 0.9524 0.4108 0.045 Uiso 1 1 calc R . . C6 C 0.57056(16) 0.7498(2) 0.53508(14) 0.0398(5) Uani 1 1 d . . . H6A H 0.5945 0.8302 0.5724 0.048 Uiso 1 1 calc R . . H6B H 0.5651 0.6841 0.5831 0.048 Uiso 1 1 calc R . . C7 C 0.50451(16) 0.59100(19) 0.35114(15) 0.0358(4) Uani 1 1 d . . . H7A H 0.4706 0.5785 0.2783 0.043 Uiso 1 1 calc R . . H7B H 0.5314 0.5074 0.3813 0.043 Uiso 1 1 calc R . . C8 C 0.55017(16) 0.81952(19) 0.32430(15) 0.0354(4) Uani 1 1 d . . . H8A H 0.6068 0.8815 0.3331 0.042 Uiso 1 1 calc R . . H8B H 0.5127 0.8092 0.2518 0.042 Uiso 1 1 calc R . . C9 C 0.65065(15) 0.7056(2) 0.48615(14) 0.0376(4) Uani 1 1 d . . . H9A H 0.6824 0.6239 0.5164 0.045 Uiso 1 1 calc R . . H9B H 0.7061 0.7702 0.4987 0.045 Uiso 1 1 calc R . . C10 C 0.59593(13) 0.68788(17) 0.37071(12) 0.0266(3) Uani 1 1 d . . . C11 C 0.67136(14) 0.63723(19) 0.32576(13) 0.0324(4) Uani 1 1 d . . . C12 C 0.73283(15) 0.5909(2) 0.29098(14) 0.0352(4) Uani 1 1 d . . . C13 C 0.80154(14) 0.5340(2) 0.24451(14) 0.0368(5) Uani 1 1 d . . . C14 C 0.82100(16) 0.4000(2) 0.25088(17) 0.0431(5) Uani 1 1 d . . . H14 H 0.7927 0.3472 0.2892 0.052 Uiso 1 1 calc R . . C15 C 0.88192(18) 0.3471(3) 0.2003(2) 0.0538(6) Uani 1 1 d . . . H15 H 0.8942 0.2577 0.2027 0.065 Uiso 1 1 calc R . . N16 N 0.92369(16) 0.4249(3) 0.14738(15) 0.0571(6) Uani 1 1 d . . . H16 H 0.9608 0.3898 0.1150 0.069 Uiso 1 1 calc R . . C17 C 0.9110(2) 0.5530(3) 0.14204(18) 0.0563(6) Uani 1 1 d . . . H17 H 0.9439 0.6035 0.1063 0.068 Uiso 1 1 calc R . . C18 C 0.84889(17) 0.6103(3) 0.18959(16) 0.0452(5) Uani 1 1 d . . . H18 H 0.8383 0.7000 0.1853 0.054 Uiso 1 1 calc R . . O21 O 0.1851(2) 0.9757(3) 0.66711(18) 0.0834(8) Uani 1 1 d D . . H21A H 0.176(4) 0.981(4) 0.720(3) 0.125 Uiso 1 1 d D . . H21B H 0.164(4) 1.041(3) 0.636(3) 0.125 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 Pt01 0.02554(4) 0.04715(6) 0.02358(4) 0.00037(6) 0.00721(3) -0.00227(6) N01 0.0534(11) 0.0547(13) 0.0526(11) 0.0031(10) 0.0284(10) -0.0030(10) N02 0.0419(8) 0.0730(13) 0.0408(8) 0.0062(11) 0.0202(7) 0.0039(11) C02 0.0316(7) 0.0520(11) 0.0312(7) 0.0041(11) 0.0095(6) -0.0002(11) C01 0.0343(9) 0.0582(14) 0.0338(9) -0.0003(9) 0.0156(7) -0.0050(9) C1 0.0442(11) 0.0565(14) 0.0485(12) -0.0093(10) 0.0230(10) 0.0017(10) C2 0.0390(10) 0.0393(11) 0.0387(10) -0.0046(8) 0.0167(8) -0.0003(8) C3 0.0337(9) 0.0293(9) 0.0296(8) -0.0045(7) 0.0126(7) 0.0029(7) C4 0.0406(10) 0.0356(10) 0.0453(11) -0.0091(8) 0.0209(9) -0.0091(8) C5 0.0376(9) 0.0319(10) 0.0482(11) 0.0084(8) 0.0201(9) 0.0097(8) C6 0.0394(10) 0.0523(13) 0.0244(8) -0.0053(8) 0.0064(8) 0.0039(9) C7 0.0419(10) 0.0284(9) 0.0389(10) -0.0075(8) 0.0161(8) -0.0036(8) C8 0.0439(10) 0.0291(9) 0.0382(9) 0.0067(7) 0.0206(8) 0.0054(8) C9 0.0333(9) 0.0490(12) 0.0271(8) -0.0051(8) 0.0060(7) 0.0055(8) C10 0.0292(8) 0.0257(8) 0.0249(7) -0.0012(6) 0.0089(6) 0.0028(6) C11 0.0329(8) 0.0335(10) 0.0286(8) -0.0027(7) 0.0076(7) 0.0021(7) C12 0.0314(8) 0.0405(11) 0.0316(8) -0.0041(8) 0.0081(7) 0.0027(8) C13 0.0248(7) 0.0560(14) 0.0275(8) -0.0042(7) 0.0063(6) 0.0056(7) C14 0.0287(9) 0.0512(13) 0.0487(12) -0.0094(10) 0.0124(8) 0.0005(9) C15 0.0388(11) 0.0556(15) 0.0617(15) -0.0184(12) 0.0102(11) 0.0071(11) N16 0.0354(10) 0.0925(18) 0.0451(11) -0.0192(12) 0.0158(9) 0.0101(11) C17 0.0395(12) 0.095(2) 0.0374(12) 0.0088(12) 0.0172(10) 0.0112(13) C18 0.0392(11) 0.0583(14) 0.0372(10) 0.0084(10) 0.0117(9) 0.0113(10) O21 0.0919(16) 0.110(2) 0.0670(13) 0.0071(12) 0.0518(13) 0.0431(14) _geom_special_details ; All s.u.'s (except the s.u. in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell s.u.'s are taken into account individually in the estimation of s.u.'s in distances, angles and torsion angles; correlations between s.u.'s in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell s.u.'s is used for estimating s.u.'s 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 Pt01 C01 1.981(3) . ? Pt01 C01 1.981(3) 3_566 ? Pt01 C02 1.9943(18) . ? Pt01 C02 1.9943(18) 3_566 ? N01 C01 1.151(3) . ? N02 C02 1.149(2) . ? C1 C2 1.183(3) . ? C1 H1 0.9300 . ? C2 C3 1.473(3) . ? C3 C6 1.533(3) . ? C3 C4 1.536(3) . ? C3 C5 1.541(3) . ? C4 C7 1.534(3) . ? C4 H4A 0.9700 . ? C4 H4B 0.9700 . ? C5 C8 1.531(3) . ? C5 H5A 0.9700 . ? C5 H5B 0.9700 . ? C6 C9 1.531(3) . ? C6 H6A 0.9700 . ? C6 H6B 0.9700 . ? C7 C10 1.535(3) . ? C7 H7A 0.9700 . ? C7 H7B 0.9700 . ? C8 C10 1.534(2) . ? C8 H8A 0.9700 . ? C8 H8B 0.9700 . ? C9 C10 1.537(2) . ? C9 H9A 0.9700 . ? C9 H9B 0.9700 . ? C10 C11 1.462(2) . ? C11 C12 1.194(3) . ? C12 C13 1.426(3) . ? C13 C18 1.394(3) . ? C13 C14 1.397(3) . ? C14 C15 1.366(3) . ? C14 H14 0.9300 . ? C15 N16 1.336(4) . ? C15 H15 0.9300 . ? N16 C17 1.325(4) . ? N16 H16 0.8600 . ? C17 C18 1.367(3) . ? C17 H17 0.9300 . ? C18 H18 0.9300 . ? O21 H21A 0.79(3) . ? O21 H21B 0.79(3) . ? 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 C01 Pt01 C01 180.0 . 3_566 ? C01 Pt01 C02 89.44(9) . . ? C01 Pt01 C02 90.56(9) 3_566 . ? C01 Pt01 C02 90.56(9) . 3_566 ? C01 Pt01 C02 89.44(9) 3_566 3_566 ? C02 Pt01 C02 180.0 . 3_566 ? N02 C02 Pt01 177.86(18) . . ? N01 C01 Pt01 178.44(19) . . ? C2 C1 H1 180.0 . . ? C1 C2 C3 177.2(2) . . ? C2 C3 C6 109.92(16) . . ? C2 C3 C4 110.39(16) . . ? C6 C3 C4 108.83(16) . . ? C2 C3 C5 111.55(16) . . ? C6 C3 C5 108.00(17) . . ? C4 C3 C5 108.07(16) . . ? C7 C4 C3 110.53(16) . . ? C7 C4 H4A 109.5 . . ? C3 C4 H4A 109.5 . . ? C7 C4 H4B 109.5 . . ? C3 C4 H4B 109.5 . . ? H4A C4 H4B 108.1 . . ? C8 C5 C3 110.68(15) . . ? C8 C5 H5A 109.5 . . ? C3 C5 H5A 109.5 . . ? C8 C5 H5B 109.5 . . ? C3 C5 H5B 109.5 . . ? H5A C5 H5B 108.1 . . ? C9 C6 C3 110.78(15) . . ? C9 C6 H6A 109.5 . . ? C3 C6 H6A 109.5 . . ? C9 C6 H6B 109.5 . . ? C3 C6 H6B 109.5 . . ? H6A C6 H6B 108.1 . . ? C4 C7 C10 110.17(15) . . ? C4 C7 H7A 109.6 . . ? C10 C7 H7A 109.6 . . ? C4 C7 H7B 109.6 . . ? C10 C7 H7B 109.6 . . ? H7A C7 H7B 108.1 . . ? C5 C8 C10 110.05(15) . . ? C5 C8 H8A 109.7 . . ? C10 C8 H8A 109.7 . . ? C5 C8 H8B 109.7 . . ? C10 C8 H8B 109.7 . . ? H8A C8 H8B 108.2 . . ? C6 C9 C10 109.98(15) . . ? C6 C9 H9A 109.7 . . ? C10 C9 H9A 109.7 . . ? C6 C9 H9B 109.7 . . ? C10 C9 H9B 109.7 . . ? H9A C9 H9B 108.2 . . ? C11 C10 C8 111.80(15) . . ? C11 C10 C7 109.25(15) . . ? C8 C10 C7 108.10(15) . . ? C11 C10 C9 109.58(14) . . ? C8 C10 C9 108.60(15) . . ? C7 C10 C9 109.48(15) . . ? C12 C11 C10 177.2(2) . . ? C11 C12 C13 176.9(2) . . ? C18 C13 C14 118.41(19) . . ? C18 C13 C12 120.8(2) . . ? C14 C13 C12 120.75(19) . . ? C15 C14 C13 119.4(2) . . ? C15 C14 H14 120.3 . . ? C13 C14 H14 120.3 . . ? N16 C15 C14 119.4(2) . . ? N16 C15 H15 120.3 . . ? C14 C15 H15 120.3 . . ? C17 N16 C15 123.6(2) . . ? C17 N16 H16 118.2 . . ? C15 N16 H16 118.2 . . ? N16 C17 C18 119.2(3) . . ? N16 C17 H17 120.4 . . ? C18 C17 H17 120.4 . . ? C17 C18 C13 119.9(2) . . ? C17 C18 H18 120.0 . . ? C13 C18 H18 120.0 . . ? H21A O21 H21B 108(4) . . ? _diffrn_measured_fraction_theta_max 0.995 _diffrn_reflns_theta_full 34.97 _diffrn_measured_fraction_theta_full 0.995 _refine_diff_density_max 0.961 _refine_diff_density_min -0.992 _refine_diff_density_rms 0.092