# ic991137x.cif #============================================================================== data_global #============================================================================== # 1. SUBMISSION DETAILS _publ_contact_author # Name and address of author for correspondence ; G\"udel, Hans-Ueli Departement f\"ur Chemie und Biochemie Universit\"at Bern Freiestr. 3 CH-3012 Bern Schweiz ; _publ_contact_author_phone '+41 31 631 42 49' _publ_contact_author_fax '+41 31 631 43 99' _publ_contact_author_email hans-ulrich.guedel@iac.unibe.ch _publ_requested_journal 'Inorganic Chemistry' _publ_section_title ; Crystal Structure and optical Spectroscopy of Er~2~[Pt(CN)~4~]~3~.21H~2~O and Er~2~[Pt(CN)~4~]~2~.SO~4~.11.5H~2~O ; #============================================================================== data_red #============================================================================== _audit_creation_method SHELXL-97 _chemical_name_systematic ? _chemical_name_common ? _chemical_formula_moiety Er~2~[Pt(CN)~4~]~3~.21H~2~O _chemical_formula_sum 'C12 H42 Er2 N12 O21 Pt3' _chemical_formula_weight 1610.37 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' 'Er' 'Er' -0.2586 4.9576 '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 orthorhombic _symmetry_space_group_name_H-M Pbcn loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x+1/2, -y+1/2, z+1/2' '-x, y, -z+1/2' 'x+1/2, -y+1/2, -z' '-x, -y, -z' 'x-1/2, y-1/2, -z-1/2' 'x, -y, z-1/2' '-x-1/2, y-1/2, z' _cell_length_a 15.4848(3) _cell_length_b 13.8186(2) _cell_length_c 19.07820(10) _cell_angle_alpha 90.00 _cell_angle_beta 90.00 _cell_angle_gamma 90.00 _cell_volume 4082.32(10) _cell_formula_units_Z 4 _exptl_crystal_description plate _exptl_crystal_colour red _exptl_crystal_size_max 0.10 _exptl_crystal_size_mid 0.08 _exptl_crystal_size_min 0.06 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 2.620 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 2944 _exptl_absorpt_coefficient_mu 14.392 _exptl_absorpt_correction_type 'empirical using SADABS (Sheldrick, 1996)' _exptl_absorpt_correction_T_min 0.3271 _exptl_absorpt_correction_T_max 0.4789 _exptl_special_details ? _diffrn_ambient_temperature 293(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type ;Siemens SMART CCD area-detector diffractometer ; _diffrn_measurement_method ; \w scans, 1271 frames, 0.3\%, 10 seconds, detector distance 5.18 cm, detector angle 27% ; _diffrn_detector_area_resol_mean ? _diffrn_standards_number 0 _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 4516 _diffrn_reflns_av_R_equivalents 0.0442 _diffrn_reflns_av_sigmaI/netI 0.0220 _diffrn_reflns_limit_h_min 0 _diffrn_reflns_limit_h_max 19 _diffrn_reflns_limit_k_min 0 _diffrn_reflns_limit_k_max 17 _diffrn_reflns_limit_l_min 0 _diffrn_reflns_limit_l_max 24 _diffrn_reflns_theta_min 1.98 _diffrn_reflns_theta_max 27.51 _diffrn_measured_fraction_theta_max 0.868 _diffrn_reflns_theta_full 27.51 _diffrn_measured_fraction_theta_full 0.868 _reflns_number_total 4516 _reflns_number_gt 3401 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'SMART (Siemens, 1996)' _computing_cell_refinement 'SMART (Siemens, 1996)' _computing_data_reduction 'SAINT (Siemens, 1996)' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'ATOMS Version 4.1 (Dowty, 1998)' _computing_publication_material 'SHELXL-97 (Sheldrick, 1997)' _refine_special_details ; The hydrogen atoms could not be located. 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^)+(0.0171P)^2^+33.8859P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens none _refine_ls_hydrogen_treatment undef _refine_ls_extinction_method SHELXL _refine_ls_extinction_coef 0.000892(18) _refine_ls_extinction_expression 'Fc^*^=kFc[1+0.001xFc^2^\l^3^/sin(2\q)]^-1/4^' _refine_ls_number_reflns 4516 _refine_ls_number_parameters 229 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0490 _refine_ls_R_factor_gt 0.0274 _refine_ls_wR_factor_ref 0.0677 _refine_ls_wR_factor_gt 0.0593 _refine_ls_goodness_of_fit_ref 1.165 _refine_ls_restrained_S_all 1.165 _refine_ls_shift/su_max 0.021 _refine_ls_shift/su_mean 0.001 _refine_diff_density_max 1.498 _refine_diff_density_min -0.758 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 Er Er -0.172192(18) -0.34997(2) -0.011561(15) 0.02003(9) Uani 1 d . . . O1 O -0.0334(3) -0.3972(4) 0.0121(3) 0.0367(13) Uani 1 d . . . O2 O -0.2078(4) -0.2770(4) 0.0952(3) 0.0431(15) Uani 1 d . . . O3 O -0.1833(4) -0.4878(4) -0.0816(3) 0.0414(15) Uani 1 d . . . O4 O -0.0954(4) -0.3242(4) -0.1203(3) 0.0405(14) Uani 1 d . . . O5 O -0.2632(3) -0.2407(4) -0.0766(3) 0.0389(14) Uani 1 d . . . O6 O -0.1745(4) -0.4759(4) 0.0761(3) 0.0418(14) Uani 1 d . . . Pt1 Pt 0.0000 0.0000 0.0000 0.01481(9) Uani 1 d S . . Pt2 Pt -0.000697(18) 0.005027(18) -0.167118(14) 0.02174(8) Uani 1 d . . . C1 C -0.0623(4) -0.1259(4) -0.0025(3) 0.0197(14) Uani 1 d . . . C2 C 0.1130(4) -0.0673(5) 0.0000(3) 0.0214(15) Uani 1 d . . . C3 C -0.1181(5) -0.0535(5) -0.1638(4) 0.0260(15) Uani 1 d . . . C4 C -0.0524(5) 0.1376(5) -0.1646(4) 0.0290(16) Uani 1 d . . . C5 C 0.1200(5) 0.0591(5) -0.1676(4) 0.0279(16) Uani 1 d . . . C6 C 0.0474(5) -0.1288(5) -0.1660(4) 0.0284(16) Uani 1 d . . . N1 N -0.1004(4) -0.1968(4) -0.0054(3) 0.0291(14) Uani 1 d . . . N2 N 0.1798(4) -0.1025(4) 0.0014(3) 0.0305(14) Uani 1 d . . . N3 N -0.1837(5) -0.0892(5) -0.1588(4) 0.0409(17) Uani 1 d . . . N4 N -0.0861(5) 0.2115(5) -0.1615(4) 0.049(2) Uani 1 d . . . N5 N 0.1885(5) 0.0859(6) -0.1661(4) 0.049(2) Uani 1 d . . . N6 N 0.0731(5) -0.2062(5) -0.1628(4) 0.050(2) Uani 1 d . . . O1W O 0.1176(4) -0.3348(4) -0.0474(3) 0.0463(15) Uani 1 d . . . O2W O -0.0483(4) 0.4130(4) -0.1370(3) 0.0422(14) Uani 1 d . . . O3W O 0.0000 0.5221(7) -0.2500 0.056(3) Uani 1 d S . . O4W O 0.3509(4) 0.1387(5) -0.2439(3) 0.0530(17) Uani 1 d . . . O5W O -0.3021(6) -0.1489(9) -0.2750(4) 0.118(4) Uani 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 Er 0.01536(14) 0.01623(14) 0.02851(16) -0.00011(12) -0.00006(13) -0.00338(12) O1 0.021(3) 0.038(3) 0.051(3) 0.009(3) -0.001(2) 0.002(2) O2 0.050(4) 0.036(3) 0.044(4) -0.009(3) 0.011(3) -0.010(3) O3 0.034(3) 0.032(3) 0.057(4) -0.020(3) 0.007(3) -0.008(3) O4 0.045(3) 0.040(3) 0.037(3) -0.001(3) 0.007(3) -0.014(3) O5 0.027(3) 0.034(3) 0.055(4) 0.017(3) -0.009(3) -0.006(2) O6 0.040(3) 0.038(3) 0.048(4) 0.020(3) 0.007(3) 0.002(3) Pt1 0.01129(16) 0.01258(16) 0.0206(2) -0.00052(12) -0.00097(13) -0.00031(12) Pt2 0.02285(14) 0.02191(14) 0.02045(16) -0.00076(10) 0.00150(10) -0.00044(10) C1 0.016(3) 0.016(3) 0.027(4) -0.003(3) 0.001(3) -0.004(2) C2 0.014(3) 0.023(3) 0.027(4) -0.002(3) -0.004(3) -0.002(3) C3 0.027(4) 0.028(4) 0.023(4) 0.000(3) 0.004(3) 0.001(3) C4 0.029(4) 0.027(4) 0.031(4) 0.002(3) 0.002(3) 0.001(3) C5 0.026(4) 0.026(4) 0.032(4) -0.004(3) -0.001(3) -0.004(3) C6 0.031(4) 0.027(4) 0.027(4) -0.003(3) 0.000(3) -0.003(3) N1 0.032(3) 0.024(3) 0.031(4) 0.000(3) 0.002(3) -0.003(3) N2 0.022(3) 0.030(3) 0.040(4) 0.002(3) 0.000(3) 0.004(3) N3 0.036(4) 0.041(4) 0.046(4) 0.000(3) 0.010(3) -0.004(3) N4 0.051(5) 0.035(4) 0.062(5) -0.006(4) 0.009(4) 0.007(4) N5 0.037(4) 0.051(5) 0.060(5) -0.004(4) 0.000(4) -0.013(4) N6 0.059(5) 0.032(4) 0.058(5) -0.006(4) 0.002(4) 0.005(4) O1W 0.037(3) 0.041(3) 0.061(4) 0.006(3) 0.006(3) -0.006(3) O2W 0.039(3) 0.042(3) 0.046(4) -0.005(3) 0.003(3) 0.000(3) O3W 0.068(7) 0.047(5) 0.054(6) 0.000 0.011(5) 0.000 O4W 0.058(4) 0.054(4) 0.047(4) -0.007(3) 0.012(3) -0.014(3) O5W 0.116(8) 0.177(11) 0.062(5) -0.043(6) -0.024(5) 0.008(8) _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 Er O1 2.292(5) . ? Er O3 2.334(5) . ? Er O2 2.339(5) . ? Er N2 2.392(6) 4_445 ? Er N1 2.393(6) . ? Er O5 2.409(5) . ? Er O6 2.414(5) . ? Er O4 2.417(5) . ? Pt1 C2 1.981(6) . ? Pt1 C1 1.990(6) . ? Pt2 C3 1.990(7) . ? Pt2 C6 1.993(7) . ? Pt2 C4 2.000(7) . ? Pt2 C5 2.013(7) . ? Pt1 Pt2 3.1891(3) . ? Pt2 Pt2 3.1625(5) 3_554 ? C1 N1 1.145(8) . ? C2 N2 1.143(8) . ? C3 N3 1.134(10) . ? C4 N4 1.148(10) . ? C5 N5 1.124(10) . ? C6 N6 1.144(10) . ? 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 O1 Er O3 87.1(2) . . ? O1 Er O2 99.9(2) . . ? O3 Er O2 146.5(2) . . ? O1 Er N2 143.56(19) . 4_445 ? O3 Er N2 75.6(2) . 4_445 ? O2 Er N2 79.7(2) . 4_445 ? O1 Er N1 78.8(2) . . ? O3 Er N1 141.6(2) . . ? O2 Er N1 71.7(2) . . ? N2 Er N1 133.2(2) 4_445 . ? O1 Er O5 145.95(18) . . ? O3 Er O5 100.0(2) . . ? O2 Er O5 92.3(2) . . ? N2 Er O5 69.76(19) 4_445 . ? N1 Er O5 75.08(19) . . ? O1 Er O6 70.8(2) . . ? O3 Er O6 78.9(2) . . ? O2 Er O6 72.8(2) . . ? N2 Er O6 74.4(2) 4_445 . ? N1 Er O6 127.6(2) . . ? O5 Er O6 143.14(19) . . ? O1 Er O4 75.5(2) . . ? O3 Er O4 70.42(19) . . ? O2 Er O4 143.11(19) . . ? N2 Er O4 125.6(2) 4_445 . ? N1 Er O4 71.54(19) . . ? O5 Er O4 75.72(19) . . ? O6 Er O4 135.1(2) . . ? C2 Pt1 C1 91.0(3) . . ? C2 Pt1 C1 89.0(3) . 5 ? C3 Pt2 C6 87.9(3) . . ? C3 Pt2 C4 90.3(3) . . ? C6 Pt2 C4 177.4(3) . . ? C3 Pt2 C5 177.3(3) . . ? C6 Pt2 C5 89.8(3) . . ? C4 Pt2 C5 91.8(3) . . ? Pt2 Pt2 Pt1 178.621(7) 3_554 . ? N1 C1 Pt1 177.5(6) . . ? N2 C2 Pt1 176.9(6) . . ? N3 C3 Pt2 176.4(7) . . ? N4 C4 Pt2 176.2(7) . . ? N5 C5 Pt2 176.9(7) . . ? N6 C6 Pt2 177.2(7) . . ? C1 N1 Er 176.7(5) . . ? C2 N2 Er 170.2(6) . 4_545 ? 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 Pt2 C3 -51.9(3) 5 . . . ? C2 Pt1 Pt2 C3 128.1(3) . . . . ? C1 Pt1 Pt2 C3 37.1(3) . . . . ? C1 Pt1 Pt2 C3 -142.9(3) 5 . . . ? C2 Pt1 Pt2 C6 -139.9(3) 5 . . . ? C2 Pt1 Pt2 C6 40.1(3) . . . . ? C1 Pt1 Pt2 C6 -50.9(3) . . . . ? C1 Pt1 Pt2 C6 129.1(3) 5 . . . ? C2 Pt1 Pt2 C4 38.4(3) 5 . . . ? C2 Pt1 Pt2 C4 -141.6(3) . . . . ? C1 Pt1 Pt2 C4 127.4(3) . . . . ? C1 Pt1 Pt2 C4 -52.6(3) 5 . . . ? C2 Pt1 Pt2 C5 130.3(3) 5 . . . ? C2 Pt1 Pt2 C5 -49.7(3) . . . . ? C1 Pt1 Pt2 C5 -140.8(3) . . . . ? C1 Pt1 Pt2 C5 39.2(3) 5 . . . ?