# Supplementary Material (ESI) for Dalton Transactions
# This journal is © The Royal Society of Chemistry 2000
# CCDC Number: 186/1941

data_pod1



_publ_requested_journal         'J. Chem. Soc. Dalton Trans.'



_title

;

Ternary adduct {[W(CN)8]3-,[Pt(en)2]2+,[W(CN)8]3-} in aqueos solution

and crystal struture of [Pt(en)2]3[W(CN)8]2.4H2O with infinite linear

W...Pt chains

;



_publ_contact_author       'Barbara Sieklucka'

_publ_contact_author_address      

;

Faculty of Chemistry

Jagiellonian University

ul. Ingardena 3

30-060 Krakow 

POLAND

;

_audit_contact_author_name    'Lasocha Wieslaw'

_audit_contact_author_address

;

Faculty of Chemistry

Jagiellonian University

ul. Ingardena 3

30-060 Krakow 

POLAND

;

_audit_contact_author_email         lasocha@chemia.uj.edu.pl

_audit_contact_author_fax           '48 12 6340515'

_audit_contact_author_phone         '48 12 6336377(2268)'



loop_

_publ_author_name

_publ_author_address

'Robert Podgajny'

;

Faculty of Chemistry

Jagiellonian University

ul. Ingardena 3

30-060 Krakow 

POLAND

;

'Barbara Sieklucka'

;

Faculty of Chemistry

Jagiellonian University

ul. Ingardena 3

30-060 Krakow 

POLAND

;

'Wieslaw Lasocha'

; Faculty of Chemistry

  Jagiellonian University

  ul. Ingardena 3

  30-060 Krakow 

  POLAND

;

_audit_creation_method            SHELXL-97 

_chemical_name_systematic 

; 

bis(ethane-1,2-amine)platinum(II) octacyanotungstate(V) tetrahydrate 

; 

_chemical_name_common             ? 

_chemical_formula_moiety          '3[Pt(C2H8N2)2]  2[W(CN)8] 4[H2O]'

_chemical_formula_sum 

 'C28 H56 N28 O4 Pt3 W2' 

_chemical_formula_weight          1802.06 

 

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' 

 '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' 

 'W'  'W'  -0.8490   6.8722 

 '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' 

 'H'  'H'   0.0000   0.0000 

 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 

 

_symmetry_cell_setting            ? 

_symmetry_space_group_name_H-M    ? 

 

loop_ 

 _symmetry_equiv_pos_as_xyz 

 'x, y, z' 

 '-x+3/4, -y+3/4, z' 

 '-x+3/4, y, -z+3/4' 

 'x, -y+3/4, -z+3/4' 

 'x, y+1/2, z+1/2' 

 '-x+3/4, -y+5/4, z+1/2' 

 '-x+3/4, y+1/2, -z+5/4' 

 'x, -y+5/4, -z+5/4' 

 'x+1/2, y, z+1/2' 

 '-x+5/4, -y+3/4, z+1/2' 

 '-x+5/4, y, -z+5/4' 

 'x+1/2, -y+3/4, -z+5/4' 

 'x+1/2, y+1/2, z' 

 '-x+5/4, -y+5/4, z' 

 '-x+5/4, y+1/2, -z+3/4' 

 'x+1/2, -y+5/4, -z+3/4' 

 '-x, -y, -z' 

 'x-3/4, y-3/4, -z' 

 'x-3/4, -y, z-3/4' 

 '-x, y-3/4, z-3/4' 

 '-x, -y+1/2, -z+1/2' 

 'x-3/4, y-1/4, -z+1/2' 

 'x-3/4, -y+1/2, z-1/4' 

 '-x, y-1/4, z-1/4' 

 '-x+1/2, -y, -z+1/2' 

 'x-1/4, y-3/4, -z+1/2' 

 'x-1/4, -y, z-1/4' 

 '-x+1/2, y-3/4, z-1/4' 

 '-x+1/2, -y+1/2, -z' 

 'x-1/4, y-1/4, -z' 

 'x-1/4, -y+1/2, z-3/4' 

 '-x+1/2, y-1/4, z-3/4' 

 

_cell_length_a                    18.329(3) 

_cell_length_b                    20.302(5) 

_cell_length_c                    27.084(7) 

_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     293(2) 

_cell_measurement_reflns_used     ? 

_cell_measurement_theta_min       ? 

_cell_measurement_theta_max       ? 

 

_exptl_crystal_description        ? 

_exptl_crystal_colour             orange

_exptl_crystal_size_max           .24mm

_exptl_crystal_size_mid           .22mm

_exptl_crystal_size_min           .20mm

_exptl_crystal_density_meas       ? 

_exptl_crystal_density_diffrn     2.365 

_exptl_crystal_density_method     'not measured' 

_exptl_crystal_F_000              6608 

_exptl_absorpt_coefficient_mu     12.909 

_exptl_absorpt_correction_type    ? 

_exptl_absorpt_correction_T_min   ? 

_exptl_absorpt_correction_T_max   ? 

 

_exptl_special_details 

; 

 ? 

; 

 

_diffrn_ambient_temperature       293(2) 

_diffrn_radiation_wavelength      0.70930 

_diffrn_radiation_type            ? 

_diffrn_radiation_source          'fine-focus sealed tube' 

_diffrn_radiation_monochromator   graphite 

_diffrn_measurement_device_type   'KM4'

_diffrn_measurement_method        omega-2theta

_diffrn_detector_area_resol_mean  ? 

_diffrn_standards_number          2 

_diffrn_standards_interval_count  ? 

_diffrn_standards_interval_time   2hrs? 

_diffrn_standards_decay_%         'not observed' 

_diffrn_reflns_number             5297 

_diffrn_reflns_av_R_equivalents   0.0818 

_diffrn_reflns_av_sigmaI/netI     0.0681 

_diffrn_reflns_limit_h_min        -23 

_diffrn_reflns_limit_h_max        0 

_diffrn_reflns_limit_k_min        -20 

_diffrn_reflns_limit_k_max        25 

_diffrn_reflns_limit_l_min        -34 

_diffrn_reflns_limit_l_max        20 

_diffrn_reflns_theta_min          1.67 

_diffrn_reflns_theta_max          26.99 

_reflns_number_total              2747 

_reflns_number_gt                 2137 

_reflns_threshold_expression      >2sigma(I) 

 

_computing_data_collection        ? 

_computing_cell_refinement        ? 

_computing_data_reduction         ? 

_computing_structure_solution     'SHELXS-97 (Sheldrick, 1990)' 

_computing_structure_refinement   'SHELXL-97 (Sheldrick, 1997)' 

_computing_molecular_graphics     'PLUTON, ORTEP' 

_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 w=1/[\s^2^(Fo^2^)+(0.0441P)^2^+291.3104P] 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        0.000096(8) 

_refine_ls_extinction_expression 

 'Fc^*^=kFc[1+0.001xFc^2^\l^3^/sin(2\q)]^-1/4^' 

_refine_ls_number_reflns          2747 

_refine_ls_number_parameters      159 

_refine_ls_number_restraints      15 

_refine_ls_R_factor_all           0.0748 

_refine_ls_R_factor_gt            0.0574 

_refine_ls_wR_factor_ref          0.1499 

_refine_ls_wR_factor_gt           0.1429 

_refine_ls_goodness_of_fit_ref    1.319 

_refine_ls_restrained_S_all       1.315 

_refine_ls_shift/su_max           0.195 

_refine_ls_shift/su_mean          0.011 

 

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 

W1 W 0.3750 0.3750 0.64287(2) 0.0269(2) Uani 1 d S . . 

C1 C 0.4814(7) 0.4092(7) 0.6181(4) 0.035(3) Uani 1 d . . . 

N1 N 0.5343(7) 0.4302(9) 0.6056(5) 0.061(4) Uani 1 d . . . 

C2 C 0.3173(8) 0.4623(8) 0.6674(5) 0.047(3) Uani 1 d . . . 

N2 N 0.2859(7) 0.5066(7) 0.6802(6) 0.065(4) Uani 1 d . . . 

N3 N 0.3411(8) 0.4654(8) 0.5443(5) 0.066(4) Uani 1 d . . . 

C3 C 0.3528(7) 0.4331(8) 0.5788(5) 0.041(3) Uani 1 d . . . 

N4 N 0.4669(7) 0.4223(12) 0.7406(5) 0.083(7) Uani 1 d . . . 

C4 C 0.4362(7) 0.4042(10) 0.7069(5) 0.054(4) Uani 1 d . . . 

Pt2 Pt 0.3750 0.3750 0.8750 0.0407(3) Uani 1 d S . . 

N21 N 0.3791(7) 0.4493(7) 0.9240(4) 0.055(3) Uani 1 d . . . 

H21A H 0.3477 0.4409 0.9488 0.066 Uiso 1 calc R . . 

H21B H 0.4242 0.4514 0.9369 0.066 Uiso 1 calc R . . 

C21 C 0.3604(9) 0.5142(10) 0.9011(6) 0.061(4) Uani 1 d . . . 

H21C H 0.3823 0.5498 0.9199 0.074 Uiso 1 calc R . . 

H21D H 0.3079 0.5204 0.9009 0.074 Uiso 1 calc R . . 

Pt1 Pt 0.31508(4) 0.1250 0.6250 0.0552(3) Uani 1 d S . . 

N11 N 0.3882(7) 0.1351(7) 0.5689(4) 0.052(3) Uani 1 d . . . 

H11A H 0.4069 0.1761 0.5689 0.062 Uiso 1 calc R . . 

H11B H 0.4251 0.1063 0.5727 0.062 Uiso 1 calc R . . 

N12 N 0.2399(10) 0.1387(12) 0.5713(7) 0.110(7) Uani 1 d DU . . 

H12A H 0.2089 0.1044 0.5712 0.132 Uiso 1 calc R A 1 

H12B H 0.2139 0.1752 0.5781 0.132 Uiso 1 calc R A 1 

C11 C 0.3492(16) 0.1221(19) 0.5210(7) 0.156(17) Uani 1 d D . . 

H11C H 0.3749 0.1441 0.4944 0.187 Uiso 1 calc R B 1 

H11D H 0.3499 0.0751 0.5143 0.187 Uiso 1 calc R B 1 

C12 C 0.2721(15) 0.1455(18) 0.5223(9) 0.096(3) Uani 0.50 d PDU C 1 

H12C H 0.2705 0.1914 0.5123 0.115 Uiso 0.50 calc PR C 1 

H12D H 0.2435 0.1203 0.4987 0.115 Uiso 0.50 calc PR C 1 

C121 C 0.2818(16) 0.1622(15) 0.5287(10) 0.096(3) Uani 0.50 d PDU C 2 

H12E H 0.2952 0.2079 0.5339 0.115 Uiso 0.50 calc PR C 2 

H12F H 0.2516 0.1599 0.4994 0.115 Uiso 0.50 calc PR C 2 

O5 O 0.6078(12) 0.0264(9) 0.1889(5) 0.107(6) Uani 1 d D . . 

H51 H 0.633(11) 0.014(10) 0.218(5) 0.129 Uiso 1 d D . . 

H52 H 0.604(13) -0.012(6) 0.169(7) 0.129 Uiso 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 

W1 0.0270(3) 0.0261(3) 0.0277(3) 0.000 0.000 0.0005(3) 

C1 0.045(6) 0.031(7) 0.029(6) 0.005(5) 0.002(5) -0.005(5) 

N1 0.043(7) 0.078(12) 0.061(8) 0.005(8) 0.010(6) -0.015(7) 

C2 0.043(7) 0.048(9) 0.050(8) -0.003(7) -0.009(6) -0.011(7) 

N2 0.059(8) 0.046(8) 0.089(10) -0.029(9) 0.002(7) 0.027(7) 

N3 0.080(9) 0.061(10) 0.058(8) 0.019(8) -0.013(7) -0.004(8) 

C3 0.048(7) 0.040(8) 0.035(6) 0.004(6) 0.004(5) -0.007(6) 

N4 0.053(8) 0.15(2) 0.045(7) -0.042(10) -0.001(6) -0.012(9) 

C4 0.035(7) 0.079(13) 0.047(8) 0.002(8) 0.001(6) -0.016(7) 

Pt2 0.0370(5) 0.0460(6) 0.0392(5) 0.000 0.000 0.000 

N21 0.052(6) 0.065(9) 0.049(6) -0.010(7) 0.002(6) -0.017(7) 

C21 0.059(10) 0.059(10) 0.066(9) -0.019(10) 0.011(8) 0.006(8) 

Pt1 0.0358(4) 0.0656(6) 0.0642(5) 0.0227(5) 0.000 0.000 

N11 0.056(7) 0.037(7) 0.062(7) 0.006(7) 0.004(6) -0.020(6) 

N12 0.086(12) 0.13(2) 0.114(9) 0.042(12) -0.038(8) -0.032(12) 

C11 0.18(3) 0.24(5) 0.048(10) -0.013(19) -0.022(15) -0.03(3) 

C12 0.138(5) 0.073(5) 0.076(5) 0.027(5) -0.073(5) -0.090(5) 

C121 0.138(5) 0.073(5) 0.076(5) 0.027(5) -0.073(5) -0.090(5) 

O5 0.181(18) 0.087(12) 0.055(7) -0.009(8) -0.016(9) 0.018(13) 

 

_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 

W1 C3 2.137(14) . ? 

W1 C3 2.137(14) 2 ? 

W1 C4 2.148(15) . ? 

W1 C4 2.148(15) 2 ? 

W1 C2 2.168(17) . ? 

W1 C2 2.168(17) 2 ? 

W1 C1 2.176(13) . ? 

W1 C1 2.176(13) 2 ? 

C1 N1 1.112(17) . ? 

C2 N2 1.122(19) . ? 

N3 C3 1.162(18) . ? 

N4 C4 1.135(18) . ? 

Pt2 N21 2.009(13) . ? 

Pt2 N21 2.009(13) 3_556 ? 

Pt2 N21 2.009(13) 4_556 ? 

Pt2 N21 2.009(13) 2 ? 

N21 C21 1.50(2) . ? 

C21 C21 1.51(3) 3_556 ? 

Pt1 N12 2.024(16) . ? 

Pt1 N12 2.024(16) 8_545 ? 

Pt1 N11 2.037(12) 8_545 ? 

Pt1 N11 2.037(12) . ? 

N11 C11 1.50(2) . ? 

N12 C12 1.46(3) . ? 

N12 C121 1.46(3) . ? 

C11 C12 1.492(16) . ? 

C11 C121 1.495(16) . ? 

 

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 

C3 W1 C3 71.4(8) . 2 ? 

C3 W1 C4 127.1(6) . . ? 

C3 W1 C4 135.1(6) 2 . ? 

C3 W1 C4 135.1(6) . 2 ? 

C3 W1 C4 127.1(6) 2 2 ? 

C4 W1 C4 72.4(7) . 2 ? 

C3 W1 C2 72.8(6) . . ? 

C3 W1 C2 142.4(5) 2 . ? 

C4 W1 C2 77.4(6) . . ? 

C4 W1 C2 74.0(7) 2 . ? 

C3 W1 C2 142.4(5) . 2 ? 

C3 W1 C2 72.8(6) 2 2 ? 

C4 W1 C2 74.0(7) . 2 ? 

C4 W1 C2 77.4(6) 2 2 ? 

C2 W1 C2 144.4(8) . 2 ? 

C3 W1 C1 75.2(5) . . ? 

C3 W1 C1 75.8(5) 2 . ? 

C4 W1 C1 72.1(5) . . ? 

C4 W1 C1 143.5(5) 2 . ? 

C2 W1 C1 105.7(5) . . ? 

C2 W1 C1 85.3(5) 2 . ? 

C3 W1 C1 75.8(5) . 2 ? 

C3 W1 C1 75.2(5) 2 2 ? 

C4 W1 C1 143.5(5) . 2 ? 

C4 W1 C1 72.1(5) 2 2 ? 

C2 W1 C1 85.3(5) . 2 ? 

C2 W1 C1 105.7(5) 2 2 ? 

C1 W1 C1 144.1(6) . 2 ? 

N1 C1 W1 176.1(14) . . ? 

N2 C2 W1 178.3(14) . . ? 

N3 C3 W1 179.0(13) . . ? 

N4 C4 W1 177(2) . . ? 

N21 Pt2 N21 82.8(8) . 3_556 ? 

N21 Pt2 N21 175.7(8) . 4_556 ? 

N21 Pt2 N21 97.4(8) 3_556 4_556 ? 

N21 Pt2 N21 97.4(8) . 2 ? 

N21 Pt2 N21 175.7(8) 3_556 2 ? 

N21 Pt2 N21 82.8(8) 4_556 2 ? 

C21 N21 Pt2 112.3(9) . . ? 

N21 C21 C21 107.8(9) . 3_556 ? 

N12 Pt1 N12 94.1(12) . 8_545 ? 

N12 Pt1 N11 177.0(8) . 8_545 ? 

N12 Pt1 N11 84.1(7) 8_545 8_545 ? 

N12 Pt1 N11 84.1(7) . . ? 

N12 Pt1 N11 177.0(8) 8_545 . ? 

N11 Pt1 N11 97.7(7) 8_545 . ? 

C11 N11 Pt1 108.2(13) . . ? 

C12 N12 C121 16.5(15) . . ? 

C12 N12 Pt1 113.0(15) . . ? 

C121 N12 Pt1 104.7(15) . . ? 

C12 C11 C121 16.2(14) . . ? 

C12 C11 N11 112.1(18) . . ? 

C121 C11 N11 100.2(19) . . ? 

N12 C12 C11 112(2) . . ? 

N12 C121 C11 112(2) . . ? 

 

_diffrn_measured_fraction_theta_max    0.229 

_diffrn_reflns_theta_full              26.99 

_diffrn_measured_fraction_theta_full   0.229 

_refine_diff_density_max    2.499 

_refine_diff_density_min   -1.866 

_refine_diff_density_rms    0.247