# Copyright The Royal Society of Chemistry, 1999 # CCDC Number :182/1126 # Beginning of CIF -- 8/07324D --------------------------------------- # # Ms: 8/07324D # TITLE: # "[{Cu(bipy)(H2O)Pt(CN)4}2].2H2O: The First Synthesis and # Crystal Structure of a Discrete Heterometallic Square Cyano-Bridged # Compound with Terminal Cyano Ligands." # AUTHORS: # Larry R. Falvello and Milagros Tomas # # data_global _audit_creation_method 'EDT' # SUBMISSION DETAILS _publ_contact_author_name 'Larry R. Falvello' _publ_contact_author_address ; Departamento de Qu\'imica Inorg\'anica Instituto de Ciencia de Materiales de Arag\'on Universidad de Zaragoza-CSIC E-50009 Zaragoza Spain ; _publ_contact_author_email falvello@cc.unizar.es _publ_contact_author_fax '34976 761187' _publ_contact_author_phone '34976 761179' _publ_contact_letter ; ; _publ_requested_journal ? _publ_requested_category ? # TITLE AND AUTHOR LIST _publ_section_title ; [{Cu(bipy)(H2O)Pt(CN)4}2].2H2O: The First Synthesis and Crystal Structure of a Discrete Heterometallic Square Cyano-Bridged Compound with Terminal Cyano Ligands ; _publ_section_title_footnote ; ; loop_ _publ_author_name _publ_author_address 'Falvello, Larry R.' ; Departamento de Qu\'imica Inorg\'anica Instituto de Ciencia de Materiales de Arag\'on Universidad de Zaragoza-CSIC E-50009 Zaragoza Spain ; 'Tom\'as, Milagros' ; Departamento de Qu\'imica Inorg\'anica Instituto de Ciencia de Materiales de Arag\'on Universidad de Zaragoza-CSIC E-50009 Zaragoza Spain ; #===================================================================== #===================================================================== #===================================================================== data_x _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_formula_moiety ? _chemical_formula_sum 'C28 H24 Cu2 N12 O4 Pt2' _chemical_formula_weight 1109.85 loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source 'C' 'C' 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'H' 'H' 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'N' 'N' 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'O' 'O' 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'Cu' 'Cu' 0.3201 1.2651 '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 2(1) / c' 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 8.5573(8) _cell_length_b 26.064(3) _cell_length_c 7.5950(7) _cell_angle_alpha 90.00 _cell_angle_beta 91.967(9) _cell_angle_gamma 90.00 _cell_volume 1693.0(3) _cell_formula_units_Z 2 _cell_measurement_temperature 299(2) _cell_measurement_reflns_used ? _cell_measurement_theta_min ? _cell_measurement_theta_max ? _exptl_crystal_description ? _exptl_crystal_colour ? _exptl_crystal_size_max 0.32 _exptl_crystal_size_mid 0.26 _exptl_crystal_size_min 0.12 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 2.177 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1044 _exptl_absorpt_coefficient_mu 9.529 _exptl_absorpt_correction_type ? _exptl_absorpt_correction_T_min 0.370 _exptl_absorpt_correction_T_max 1.000 _exptl_special_details ; ? ; _diffrn_ambient_temperature 299(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'normal-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'Nonius CAD-4' _diffrn_measurement_method ? _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 4147 _diffrn_reflns_av_R_equivalents 0.0274 _diffrn_reflns_av_sigmaI/netI 0.0375 _diffrn_reflns_limit_h_min -11 _diffrn_reflns_limit_h_max 11 _diffrn_reflns_limit_k_min -33 _diffrn_reflns_limit_k_max 0 _diffrn_reflns_limit_l_min 0 _diffrn_reflns_limit_l_max 9 _diffrn_reflns_theta_min 2.38 _diffrn_reflns_theta_max 27.46 _reflns_number_total 3863 _reflns_number_gt 3125 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'CAD4/PC V2.0 (Nonius, 1996)' _computing_cell_refinement 'CAD4/PC V2.0 (Nonius, 1996)' _computing_data_reduction 'XCAD4B (Harms, 1996)' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'SHELXTL-PLUS Rel. 5.05 (Siemens, 1996)' _computing_publication_material 'SHELXL-97 (Sheldrick, 1997)' _refine_special_details ; Refinement of F^2^ against ALL reflections. The weighted R-factor wR and goodness of fit S are based on F^2^, conventional R-factors R are based on F, with F set to zero for negative F^2^. The threshold expression of F^2^ > 2sigma(F^2^) is used only for calculating R-factors(gt) etc. and is not relevant to the choice of reflections for refinement. R-factors based on F^2^ are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger. ; _refine_ls_structure_factor_coef Fsqd _refine_ls_matrix_type full _refine_ls_weighting_scheme 'calc w=1/[\s^2^(Fo^2^)+(0.0519P)^2^+4.3107P] 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 SHELXL _refine_ls_extinction_coef 0.0039(3) _refine_ls_extinction_expression 'Fc^*^=kFc[1+0.001xFc^2^\l^3^/sin(2\q)]^-1/4^' _refine_ls_number_reflns 3863 _refine_ls_number_parameters 222 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0545 _refine_ls_R_factor_gt 0.0383 _refine_ls_wR_factor_ref 0.1023 _refine_ls_wR_factor_gt 0.0933 _refine_ls_goodness_of_fit_ref 1.079 _refine_ls_restrained_S_all 1.079 _refine_ls_shift/su_max 0.006 _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_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group Pt1 Pt 0.16051(3) 0.393837(10) 0.22912(4) 0.03053(12) Uani 1 d . . . Cu1 Cu 0.34687(9) 0.57536(3) 0.11878(13) 0.0334(2) Uani 1 d . . . C1 C 0.2314(8) 0.4640(3) 0.1755(10) 0.0358(16) Uani 1 d . . . N1 N 0.2771(7) 0.5045(3) 0.1509(10) 0.0423(16) Uani 1 d . . . C2 C -0.0431(8) 0.4058(3) 0.1062(11) 0.0371(17) Uani 1 d . . . N2 N -0.1601(7) 0.4113(3) 0.0311(9) 0.0433(16) Uani 1 d . . . C3 C 0.0860(9) 0.3243(3) 0.2917(11) 0.0396(17) Uani 1 d . . . N3 N 0.0383(10) 0.2861(4) 0.3274(14) 0.068(2) Uani 1 d . . . C4 C 0.3688(9) 0.3813(3) 0.3449(11) 0.0423(19) Uani 1 d . . . N4 N 0.4893(9) 0.3751(4) 0.4090(12) 0.069(3) Uani 1 d . . . N5 N 0.5640(7) 0.5601(3) 0.2140(9) 0.0365(14) Uani 1 d . . . N6 N 0.4459(7) 0.6426(2) 0.0662(8) 0.0336(13) Uani 1 d . . . C5 C 0.6141(9) 0.5160(3) 0.2851(12) 0.045(2) Uani 1 d . . . H5 H 0.5443 0.4889 0.2935 0.054 Uiso 1 calc R . . C6 C 0.7667(10) 0.5095(4) 0.3467(13) 0.050(2) Uani 1 d . . . H6 H 0.8003 0.4786 0.3961 0.060 Uiso 1 calc R . . C7 C 0.8685(9) 0.5510(4) 0.3321(13) 0.055(2) Uani 1 d . . . H7 H 0.9719 0.5479 0.3726 0.066 Uiso 1 calc R . . C8 C 0.8179(8) 0.5952(3) 0.2600(11) 0.0423(19) Uani 1 d . . . H8 H 0.8868 0.6225 0.2489 0.051 Uiso 1 calc R . . C9 C 0.6646(7) 0.6004(3) 0.2023(10) 0.0353(17) Uani 1 d . . . C10 C 0.5962(8) 0.6468(3) 0.1240(10) 0.0337(15) Uani 1 d . . . C11 C 0.6760(10) 0.6937(4) 0.1080(13) 0.050(2) Uani 1 d . . . H11 H 0.7798 0.6967 0.1472 0.060 Uiso 1 calc R . . C12 C 0.6013(12) 0.7339(3) 0.0359(14) 0.056(2) Uani 1 d . . . H12 H 0.6525 0.7653 0.0273 0.067 Uiso 1 calc R . . C13 C 0.4487(11) 0.7292(3) -0.0257(14) 0.055(2) Uani 1 d . . . H13 H 0.3973 0.7570 -0.0778 0.066 Uiso 1 calc R . . C14 C 0.3740(10) 0.6837(4) -0.0100(14) 0.055(2) Uani 1 d . . . H14 H 0.2712 0.6806 -0.0524 0.066 Uiso 1 calc R . . O1 O 0.2483(6) 0.6034(2) 0.3688(8) 0.0416(13) Uani 1 d . . . H1A H 0.3260 0.6156 0.4207 0.04(3) Uiso 1 d R . . H1B H 0.1991 0.6328 0.3156 0.07(3) Uiso 1 d R . . O2 O 0.0973(10) 0.6964(3) 0.3278(12) 0.081(2) Uani 1 d . . . H2A H 0.0749 0.7120 0.4673 0.12(5) Uiso 1 d R . . H2B H 0.0802 0.7329 0.2617 0.17(7) Uiso 1 d R . . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 Pt1 0.02985(16) 0.02608(17) 0.03502(18) -0.00053(12) -0.00844(10) -0.00088(10) Cu1 0.0263(4) 0.0293(5) 0.0439(5) 0.0030(4) -0.0088(3) -0.0038(3) C1 0.033(3) 0.035(4) 0.038(4) 0.000(3) -0.006(3) 0.001(3) N1 0.037(3) 0.036(4) 0.052(4) 0.002(3) -0.011(3) -0.001(3) C2 0.032(4) 0.040(4) 0.038(4) 0.000(3) -0.006(3) -0.005(3) N2 0.036(3) 0.049(4) 0.045(4) 0.006(3) -0.009(3) -0.006(3) C3 0.044(4) 0.034(4) 0.041(4) 0.011(4) -0.002(3) 0.005(3) N3 0.068(5) 0.053(5) 0.084(7) 0.020(5) -0.001(5) -0.010(4) C4 0.035(4) 0.048(5) 0.043(4) -0.004(4) -0.008(3) 0.000(3) N4 0.046(4) 0.096(7) 0.061(5) -0.018(5) -0.021(4) 0.015(4) N5 0.027(3) 0.038(4) 0.043(4) 0.006(3) -0.006(2) -0.002(2) N6 0.036(3) 0.025(3) 0.040(3) 0.001(3) -0.003(2) -0.005(2) C5 0.038(4) 0.040(5) 0.057(5) -0.001(4) -0.010(4) 0.003(3) C6 0.043(4) 0.050(5) 0.057(6) -0.004(4) -0.012(4) 0.011(4) C7 0.028(4) 0.080(7) 0.055(5) 0.002(5) -0.011(4) 0.007(4) C8 0.025(3) 0.051(5) 0.051(5) -0.004(4) 0.002(3) -0.008(3) C9 0.023(3) 0.051(5) 0.032(4) -0.009(3) 0.003(3) -0.006(3) C10 0.035(3) 0.031(4) 0.035(4) -0.010(3) -0.001(3) -0.007(3) C11 0.043(4) 0.044(5) 0.065(6) -0.010(4) 0.004(4) -0.012(4) C12 0.070(6) 0.029(4) 0.069(6) 0.004(4) 0.004(5) -0.016(4) C13 0.064(6) 0.034(5) 0.066(6) 0.015(4) 0.000(5) -0.002(4) C14 0.044(4) 0.051(5) 0.068(6) 0.015(5) -0.009(4) -0.001(4) O1 0.036(3) 0.041(3) 0.047(3) -0.003(3) -0.011(2) 0.002(2) O2 0.101(6) 0.059(5) 0.083(6) 0.003(4) 0.015(5) 0.032(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 Pt1 C2 1.973(7) . ? Pt1 C1 1.973(8) . ? Pt1 C3 1.985(8) . ? Pt1 C4 1.987(8) . ? Cu1 N1 1.958(7) . ? Cu1 N2 1.961(6) 3_565 ? Cu1 N6 1.994(6) . ? Cu1 N5 2.010(6) . ? Cu1 O1 2.228(6) . ? C1 N1 1.145(10) . ? C2 N2 1.144(10) . ? N2 Cu1 1.961(6) 3_565 ? C3 N3 1.114(11) . ? C4 N4 1.136(10) . ? N5 C5 1.334(10) . ? N5 C9 1.362(9) . ? N6 C10 1.349(9) . ? N6 C14 1.354(10) . ? C5 C6 1.382(11) . ? C5 H5 0.9300 . ? C6 C7 1.394(14) . ? C6 H6 0.9300 . ? C7 C8 1.341(13) . ? C7 H7 0.9300 . ? C8 C9 1.375(9) . ? C8 H8 0.9300 . ? C9 C10 1.463(11) . ? C10 C11 1.407(11) . ? C11 C12 1.335(13) . ? C11 H11 0.9300 . ? C12 C13 1.378(13) . ? C12 H12 0.9300 . ? C13 C14 1.354(12) . ? C13 H13 0.9300 . ? C14 H14 0.9300 . ? O1 H1A 0.8241 . ? O1 H1B 0.9552 . ? O2 H2A 1.1581 . ? O2 H2B 1.0847 . ? 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 C2 Pt1 C1 91.7(3) . . ? C2 Pt1 C3 88.4(3) . . ? C1 Pt1 C3 177.8(3) . . ? C2 Pt1 C4 178.0(3) . . ? C1 Pt1 C4 88.1(3) . . ? C3 Pt1 C4 92.0(3) . . ? N1 Cu1 N2 89.6(3) . 3_565 ? N1 Cu1 N6 171.0(3) . . ? N2 Cu1 N6 94.1(3) 3_565 . ? N1 Cu1 N5 92.9(3) . . ? N2 Cu1 N5 165.6(3) 3_565 . ? N6 Cu1 N5 81.5(3) . . ? N1 Cu1 O1 94.5(3) . . ? N2 Cu1 O1 96.4(3) 3_565 . ? N6 Cu1 O1 93.3(2) . . ? N5 Cu1 O1 97.5(2) . . ? N1 C1 Pt1 176.9(7) . . ? C1 N1 Cu1 176.7(7) . . ? N2 C2 Pt1 177.6(8) . . ? C2 N2 Cu1 173.4(7) . 3_565 ? N3 C3 Pt1 177.2(8) . . ? N4 C4 Pt1 178.3(9) . . ? C5 N5 C9 119.6(6) . . ? C5 N5 Cu1 126.6(5) . . ? C9 N5 Cu1 113.8(5) . . ? C10 N6 C14 119.3(7) . . ? C10 N6 Cu1 114.4(5) . . ? C14 N6 Cu1 126.2(5) . . ? N5 C5 C6 122.0(8) . . ? N5 C5 H5 119.0 . . ? C6 C5 H5 119.0 . . ? C5 C6 C7 117.6(8) . . ? C5 C6 H6 121.2 . . ? C7 C6 H6 121.2 . . ? C8 C7 C6 120.2(7) . . ? C8 C7 H7 119.9 . . ? C6 C7 H7 119.9 . . ? C7 C8 C9 120.4(8) . . ? C7 C8 H8 119.8 . . ? C9 C8 H8 119.8 . . ? N5 C9 C8 120.1(8) . . ? N5 C9 C10 114.8(6) . . ? C8 C9 C10 125.1(7) . . ? N6 C10 C11 120.2(7) . . ? N6 C10 C9 115.4(6) . . ? C11 C10 C9 124.4(7) . . ? C12 C11 C10 119.4(8) . . ? C12 C11 H11 120.3 . . ? C10 C11 H11 120.3 . . ? C11 C12 C13 120.2(8) . . ? C11 C12 H12 119.9 . . ? C13 C12 H12 119.9 . . ? C14 C13 C12 119.6(8) . . ? C14 C13 H13 120.2 . . ? C12 C13 H13 120.2 . . ? N6 C14 C13 121.3(8) . . ? N6 C14 H14 119.3 . . ? C13 C14 H14 119.3 . . ? Cu1 O1 H1A 102.2 . . ? Cu1 O1 H1B 94.4 . . ? H1A O1 H1B 103.4 . . ? H2A O2 H2B 95.1 . . ? loop_ _geom_torsion_atom_site_label_1 _geom_torsion_atom_site_label_2 _geom_torsion_atom_site_label_3 _geom_torsion_atom_site_label_4 _geom_torsion _geom_torsion_site_symmetry_1 _geom_torsion_site_symmetry_2 _geom_torsion_site_symmetry_3 _geom_torsion_site_symmetry_4 _geom_torsion_publ_flag C2 Pt1 C1 N1 156(14) . . . . ? C3 Pt1 C1 N1 65(17) . . . . ? C4 Pt1 C1 N1 -26(14) . . . . ? Pt1 C1 N1 Cu1 -83(18) . . . . ? N2 Cu1 N1 C1 -79(11) 3_565 . . . ? N6 Cu1 N1 C1 166(10) . . . . ? N5 Cu1 N1 C1 115(11) . . . . ? O1 Cu1 N1 C1 17(11) . . . . ? C1 Pt1 C2 N2 121(18) . . . . ? C3 Pt1 C2 N2 -61(18) . . . . ? C4 Pt1 C2 N2 38(23) . . . . ? Pt1 C2 N2 Cu1 -77(20) . . . 3_565 ? C2 Pt1 C3 N3 -36(18) . . . . ? C1 Pt1 C3 N3 55(21) . . . . ? C4 Pt1 C3 N3 146(18) . . . . ? C2 Pt1 C4 N4 66(34) . . . . ? C1 Pt1 C4 N4 -17(29) . . . . ? C3 Pt1 C4 N4 165(29) . . . . ? N1 Cu1 N5 C5 -5.9(8) . . . . ? N2 Cu1 N5 C5 -105.9(13) 3_565 . . . ? N6 Cu1 N5 C5 -178.8(8) . . . . ? O1 Cu1 N5 C5 89.0(7) . . . . ? N1 Cu1 N5 C9 174.5(6) . . . . ? N2 Cu1 N5 C9 74.5(13) 3_565 . . . ? N6 Cu1 N5 C9 1.7(5) . . . . ? O1 Cu1 N5 C9 -90.6(5) . . . . ? N1 Cu1 N6 C10 -55.7(19) . . . . ? N2 Cu1 N6 C10 -169.8(5) 3_565 . . . ? N5 Cu1 N6 C10 -3.5(5) . . . . ? O1 Cu1 N6 C10 93.6(5) . . . . ? N1 Cu1 N6 C14 128.6(16) . . . . ? N2 Cu1 N6 C14 14.5(8) 3_565 . . . ? N5 Cu1 N6 C14 -179.3(8) . . . . ? O1 Cu1 N6 C14 -82.2(8) . . . . ? C9 N5 C5 C6 -0.6(13) . . . . ? Cu1 N5 C5 C6 179.9(7) . . . . ? N5 C5 C6 C7 0.0(14) . . . . ? C5 C6 C7 C8 -0.2(15) . . . . ? C6 C7 C8 C9 1.0(14) . . . . ? C5 N5 C9 C8 1.4(11) . . . . ? Cu1 N5 C9 C8 -179.0(6) . . . . ? C5 N5 C9 C10 -179.3(7) . . . . ? Cu1 N5 C9 C10 0.3(8) . . . . ? C7 C8 C9 N5 -1.6(12) . . . . ? C7 C8 C9 C10 179.1(8) . . . . ? C14 N6 C10 C11 1.2(12) . . . . ? Cu1 N6 C10 C11 -174.9(6) . . . . ? C14 N6 C10 C9 -179.2(8) . . . . ? Cu1 N6 C10 C9 4.7(8) . . . . ? N5 C9 C10 N6 -3.3(10) . . . . ? C8 C9 C10 N6 176.0(7) . . . . ? N5 C9 C10 C11 176.3(8) . . . . ? C8 C9 C10 C11 -4.5(12) . . . . ? N6 C10 C11 C12 0.3(13) . . . . ? C9 C10 C11 C12 -179.2(8) . . . . ? C10 C11 C12 C13 -1.5(15) . . . . ? C11 C12 C13 C14 1.1(16) . . . . ? C10 N6 C14 C13 -1.5(14) . . . . ? Cu1 N6 C14 C13 174.1(8) . . . . ? C12 C13 C14 N6 0.4(16) . . . . ? loop_ _geom_hbond_atom_site_label_D _geom_hbond_atom_site_label_H _geom_hbond_atom_site_label_A _geom_hbond_distance_DH _geom_hbond_distance_HA _geom_hbond_distance_DA _geom_hbond_angle_DHA _geom_hbond_site_symmetry_A O1 H1A N4 0.82 2.02 2.818(9) 162.1 3_666 O1 H1B O2 0.96 1.88 2.758(9) 152.2 . O2 H2A N3 1.16 1.86 2.936(13) 151.9 3_566 O2 H2B N3 1.08 1.83 2.847(12) 154.1 2 _diffrn_measured_fraction_theta_max 0.977 _diffrn_reflns_theta_full 27.46 _diffrn_measured_fraction_theta_full 0.977 _refine_diff_density_max 1.309 _refine_diff_density_min -1.203 _refine_diff_density_rms 0.203 # # End of CIF -- 8/07324D ---------------------------------------------