# Copyright The Royal Society of Chemistry, 1999 # CCDC Number: 186/1358 data_CRYSTALS_cif _audit_creation_date 98-06-29 _audit_creation_method CRYSTALS_ver_07-07-97 #**************************************************************************** # 1. SUBMISSION DETAILS _publ_contact_author 'Jean-Claude Daran' _publ_contact_author_address ; Laboratoire de Chimie de Coordination UPR-CNRS 8241 205, route de Narbonne 31077 Toulouse cedex, France ; _publ_contact_author_phone ' (33) 5 61 33 31 74 ' _publ_contact_author_fax ' (33) 5 61 55 30 03 ' _publ_contact_author_email ' daran@lcc-toulouse.fr ' _publ_requested_journal ; Journal of the Chemical Society, Dalton Trans ; #============================================================================= # 2. TITLE AND AUTHOR LIST _publ_section_title ; Structural and Complexation Properties of diselena Crown Ethers. Synthesis and X-ray Structure of a novel cationic palladium tetraselena complex. ; loop_ _publ_author_name _publ_author_address 'Bornet, C' ; Laboratoire de Synthese et d'Electrosynthese Organometalliques CNRS(LSEO, UMR 5632) Universite de Bourgogne, 6, boulevard Gabriel, 21000 Dijon, France ; 'Amardeil, R.' ; Laboratoire de Synthese et d'Electrosynthese Organometalliques CNRS(LSEO, UMR 5632) Universite de Bourgogne, 6, boulevard Gabriel, 21000 Dijon, France ; 'Meunier, P.' ; Laboratoire de Synthese et d'Electrosynthese Organometalliques CNRS(LSEO, UMR 5632) Universite de Bourgogne, 6, boulevard Gabriel, 21000 Dijon, France ; 'Daran, J.C.' ; Laboratoire de Chimie de Coordination UPR-CNRS 8241 205, route de Narbonne 31077 Toulouse cedex, France ; ## -----------------REFERENCES ----------------------## _publ_section_references ; Altomare, A., Cascarano, G., Giacovazzo G., Guagliardi A., Burla M.C., Polidori, G. & Camalli, M. (1994) SIR92 - a program for automatic solution of crystal structures by direct methods. J. Appl. Cryst. (27), 435,435 Prince, E. Mathematical Techniques in Crystallography, Springer-Verlag: Berlin, 1982 Stoe, IPDS Manual. Version 2.75. Stoe & Cie, Darmstadt,1996, Germany. Stoe, X-SHAPE, Crystal Optimisation for Numerical Absorption Correction, Revision 1.01. Stoe & Cie, Darmstadt,1996, Germany. Stoe, X-RED, Data Reduction for STADI4 and IPDS, Revision 1.08. Stoe & Cie, Darmstadt, 1996, Germany. Watkin, D.J., Prout, C.K. Carruthers, J.R. & Betteridge, P.W. (1996) CRYSTALS Issue 10. Chemical Crystallography Laboratory, OXFORD, UK. Watkin, D.J., Prout, C.K. & Pearce, L.J. (1996) CAMERON, Chemical Crystallography Laboratory, OXFORD, UK. ; #========================================================================== # Diffractometer details #========================================================================== _diffrn_measurement_device-type 'Stoe IPDS ' _computing_data_collection 'Stoe IPDS software (Stoe, 1996)' _computing_data_reduction 'XRED (Stoe, 1.08, 1996)' _computing_cell_refinement 'Stoe IPDS software (Stoe, 1996)' #========================================================================== # General computing #========================================================================== _computing_structure_refinement ; CRYSTALS Issue 10 (Watkin, Prout, Carruthers & Betteridge, 1996) ; _computing_publication_material ; CRYSTALS Issue 10 (Watkin, Prout, Carruthers & Betteridge, 1996) ; _computing_molecular_graphics ; CAMERON (Watkin, Prout & Pearce, 1996) ; _computing_structure_solution 'SIR92 (Giacovazzo et al, 1992)' #========================================================================== _chemical_name_systematic ; ? ; _symmetry_cell_setting 'Monoclinic ' _symmetry_space_group_name_H-M 'C 1 2/c 1 ' loop_ _symmetry_equiv_pos_as_xyz 'x,y,z' '-x,-y,-z' 'x+1/2,y+1/2,z' '-x+1/2,-y+1/2,-z' '-x,y,-z+1/2' 'x,-y,z+1/2' '-x+1/2,y+1/2,-z+1/2' 'x+1/2,-y+1/2,z+1/2' loop_ _atom_type_symbol _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_Cromer_Mann_a1 _atom_type_scat_Cromer_Mann_b1 _atom_type_scat_Cromer_Mann_a2 _atom_type_scat_Cromer_Mann_b2 _atom_type_scat_Cromer_Mann_a3 _atom_type_scat_Cromer_Mann_b3 _atom_type_scat_Cromer_Mann_a4 _atom_type_scat_Cromer_Mann_b4 _atom_type_scat_Cromer_Mann_c _atom_type_scat_source 'C ' 0.0020 0.0020 2.3100 20.8439 1.0200 10.2075 1.5886 0.5687 0.8650 51.6512 0.2156 'International_Tables_Vol_IV_Table_2.2B' 'H ' 0.0000 0.0000 0.4930 10.5109 0.3229 26.1257 0.1402 3.1424 0.0408 57.7997 0.0030 'International_Tables_Vol_IV_Table_2.2B' 'O ' 0.0080 0.0060 3.0485 13.2771 2.2868 5.7011 1.5463 0.3239 0.8670 32.9089 0.2508 'International_Tables_Vol_IV_Table_2.2B' 'F ' 0.0140 0.0100 3.5392 10.2825 2.6412 4.2944 1.5170 0.2615 1.0243 26.1476 0.2776 'International_Tables_Vol_IV_Table_2.2B' 'P ' 0.0900 0.0950 6.4345 1.9067 4.1791 27.1570 1.7800 0.5260 1.4908 68.1645 1.1149 'International_Tables_Vol_IV_Table_2.2B' 'Se ' -0.1780 2.2230 17.0006 2.4098 5.8196 0.2726 3.9731 15.2372 4.3543 43.8163 2.8409 'International_Tables_Vol_IV_Table_2.2B' 'Pd ' -1.1770 1.0070 19.3319 0.6987 15.5017 7.9893 5.2954 25.2052 0.6058 76.8986 5.2659 'International_Tables_Vol_IV_Table_2.2B' _chemical_formula_sum ' C16 H20 Pd0.50 Se2 O3.50 P1 F6 ' _chemical_formula_moiety ' C16 H20 Pd0.50 Se2 O3.50 P1 F6 ' _chemical_compound_source ; synthetis as described ; _cell_length_a 13.8454(10) _cell_length_b 15.9185(15) _cell_length_c 19.7817(13) _cell_angle_alpha 90.00 _cell_angle_beta 95.472(7) _cell_angle_gamma 90.00 _cell_volume 4340.0(6) _cell_formula_units_Z 4 _cell_measurement_temperature 180(2) _cell_measurement_reflns_used 5000 _cell_measurement_theta_min 1.7 _cell_measurement_theta_max 23.9 _exptl_crystal_description box _exptl_crystal_colour yellow _exptl_crystal_size_max 0.50 _exptl_crystal_size_mid 0.30 _exptl_crystal_size_min 0.25 _exptl_crystal_density_meas 'not measured' _exptl_crystal_density_diffrn 1.926 _exptl_crystal_density_method none _exptl_crystal_F_000 2426 _exptl_absorpt_coefficient_mu 3.907 _exptl_absorpt_correction_type numerical _exptl_absorpt_correction_T_min 0.5074 _exptl_absorpt_correction_T_max 0.5716 _exptl_special_details ; The data were collected on a Stoe Imaging Plate Diffraction System (IPDS) equipped with an Oxford Cryosystems cooler device. The crystal-to-detector distance was 80 mm. 200 exposures (2 min per exposure) were obtained with 0 < \f < 200\% and with the crystals rotated through 1\% in \f. Coverage of the unique set was over 98% complete to at least 24\%. Crystal decay was monitored by measuring 200 reflexions per image. ; _diffrn_ambient_temperature 180(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 'Stoe IPDS' _diffrn_measurement_method \f _diffrn_standards_number 200 _diffrn_standards_interval_count 'every image' _diffrn_standards_interval_time ? _diffrn_standards_decay_% negligible _diffrn_reflns_number 13219 _diffrn_reflns_av_R_equivalents 0.0394 _diffrn_reflns_av_sigmaI/netI 0.0834 _diffrn_reflns_limit_h_min -15 _diffrn_reflns_limit_h_max 15 _diffrn_reflns_limit_k_min -18 _diffrn_reflns_limit_k_max 18 _diffrn_reflns_limit_l_min -22 _diffrn_reflns_limit_l_max 22 _diffrn_reflns_theta_min 1.95 _diffrn_reflns_theta_max 23.96 _reflns_number_total 3316 _reflns_number_observed 2589 _reflns_observed_criterion >2sigma(I) _refine_ls_number_reflns 2589 _refine_ls_structure_factor_coef F _refine_ls_matrix_type full _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment riding _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_diff_density_min -1.77 _refine_diff_density_max 1.73 _refine_ls_number_parameters 256 _refine_ls_R_factor_obs 0.0414 _refine_ls_wR_factor_obs 0.0489 _refine_ls_goodness_of_fit_obs 1.0725 _refine_ls_shift/su_max 0.027 _refine_ls_weighting_scheme calc _refine_ls_weighting_details ; Robust-resistant weighting scheme (Prince E, 1982): w=y[1-(\DF/6\s(Fo^2^)]^2^' where y=1/\SArTr(x) with 3 coefficients Ar(2.64, -0.407, 2.17) for the Chebyshev polynomial ArTr(x) where x was Fc/Fc(max). ; # Uequiv = arithmetic mean of Ui # i.e. Ueqiv = (U1+U2+U3)/3 loop_ _atom_site_label _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_occupancy _atom_site_thermal_displace_type Pd1 0.7500 0.2500 0.5000 0.0269 1.0000 Uani Se1 0.76584(5) 0.10280(4) 0.52943(3) 0.0401 1.0000 Uani Se2 0.74767(4) 0.21493(3) 0.38093(3) 0.0278 1.0000 Uani O1 0.9577(3) 0.2269(3) 0.5366(3) 0.0548 1.0000 Uani O2 0.9527(4) 0.3924(3) 0.4758(3) 0.0572 1.0000 Uani O3 0.8482(3) 0.3778(2) 0.3409(2) 0.0366 1.0000 Uani C1 0.7620(4) 0.0484(3) 0.4430(3) 0.0296 1.0000 Uani C2 0.7480(4) 0.0940(4) 0.3828(3) 0.0332 1.0000 Uani C3 0.7366(5) 0.0524(4) 0.3205(3) 0.0432 1.0000 Uani C4 0.7404(6) -0.0349(4) 0.3195(4) 0.0535 1.0000 Uani C5 0.7551(5) -0.0795(4) 0.3799(4) 0.0504 1.0000 Uani C6 0.7645(4) -0.0386(4) 0.4421(3) 0.0394 1.0000 Uani C11 0.8965(6) 0.0876(5) 0.5648(4) 0.0677 1.0000 Uani C12 0.9666(5) 0.1317(5) 0.5322(4) 0.0639 1.0000 Uani C13 1.0375(7) 0.2734(6) 0.5316(5) 0.0750 1.0000 Uani C14 1.0176(6) 0.3597(6) 0.5337(5) 0.0837 1.0000 Uani C15 0.9942(5) 0.4146(4) 0.4176(5) 0.0658 1.0000 Uani C16 0.9184(5) 0.4414(4) 0.3605(4) 0.0480 1.0000 Uani C17 0.8855(5) 0.3041(4) 0.3116(3) 0.0387 1.0000 Uani C18 0.8827(4) 0.2311(4) 0.3593(3) 0.0336 1.0000 Uani P1 1.17344(12) 0.1569(1) 0.36048(8) 0.0382 1.0000 Uani F11 1.2298(4) 0.1813(5) 0.4301(3) 0.1121 1.0000 Uani F12 1.1171(4) 0.1361(4) 0.2898(2) 0.0888 1.0000 Uani F13 1.2267(5) 0.0705(4) 0.3601(4) 0.1216 1.0000 Uani F14 1.1183(4) 0.2438(3) 0.3593(3) 0.0731 1.0000 Uani F15 1.0905(3) 0.1150(3) 0.3993(3) 0.0662 1.0000 Uani F16 1.2558(3) 0.1994(3) 0.3217(3) 0.0734 1.0000 Uani O21 0.5000 0.3192(15) 0.2500 0.205(8) 1.0000 Uiso C211 0.454(3) 0.409(3) 0.261(2) 0.176(16) 0.5000 Uiso C212 0.5000 0.464(2) 0.2500 0.180(11) 1.0000 Uiso C221 0.529(2) 0.229(2) 0.2236(17) 0.14(1) 0.5000 Uiso C222 0.5000 0.1673(17) 0.2500 0.142(8) 1.0000 Uiso H31 0.7267 0.0832 0.2791 0.0508 1.0000 Uiso H41 0.7323 -0.0644 0.2772 0.0614 1.0000 Uiso H51 0.7592 -0.1397 0.3784 0.0529 1.0000 Uiso H61 0.7725 -0.0703 0.4834 0.0456 1.0000 Uiso H111 0.9016 0.1037 0.6115 0.0792 1.0000 Uiso H112 0.9113 0.0289 0.5611 0.0792 1.0000 Uiso H121 1.0297 0.1174 0.5541 0.0799 1.0000 Uiso H122 0.9622 0.1171 0.4858 0.0799 1.0000 Uiso H131 1.0839 0.2602 0.5698 0.0895 1.0000 Uiso H132 1.0639 0.2605 0.4904 0.0895 1.0000 Uiso H141 1.0787 0.3891 0.5340 0.0975 1.0000 Uiso H142 0.9889 0.3718 0.5746 0.0975 1.0000 Uiso H151 1.0382 0.4609 0.4272 0.0653 1.0000 Uiso H152 1.0298 0.3676 0.4019 0.0653 1.0000 Uiso H161 0.9515 0.4557 0.3217 0.0563 1.0000 Uiso H162 0.8854 0.4894 0.3757 0.0563 1.0000 Uiso H171 0.9517 0.3139 0.3027 0.0467 1.0000 Uiso H172 0.8473 0.2915 0.2699 0.0467 1.0000 Uiso H181 0.9233 0.2425 0.4001 0.0411 1.0000 Uiso H182 0.9045 0.1815 0.3380 0.0411 1.0000 Uiso 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 Pd1 0.0313(3) 0.0235(3) 0.0268(3) 0.0030(2) 0.0077(2) 0.0087(2) Se1 0.0624(4) 0.0265(3) 0.0322(3) 0.0048(2) 0.0089(3) 0.0138(3) Se2 0.0279(3) 0.0285(3) 0.0272(3) 0.0021(2) 0.0035(2) 0.0032(2) O1 0.032(2) 0.068(3) 0.062(3) -0.020(2) -0.004(2) 0.011(2) O2 0.057(3) 0.042(3) 0.068(3) -0.014(2) -0.016(3) 0.011(2) O3 0.043(2) 0.028(2) 0.039(2) -0.0031(16) 0.0094(18) -0.0016(17 C1 0.020(3) 0.031(3) 0.039(3) -0.001(2) 0.007(2) -0.005(2) C2 0.028(3) 0.034(3) 0.037(3) -0.003(2) 0.001(2) -0.003(2) C3 0.046(4) 0.040(3) 0.044(3) -0.006(3) 0.003(3) -0.008(3) C4 0.073(5) 0.041(4) 0.047(4) -0.015(3) 0.005(3) -0.013(3) C5 0.052(4) 0.024(3) 0.075(5) -0.007(3) 0.007(3) -0.011(3) C6 0.038(3) 0.031(3) 0.049(4) 0.003(3) 0.007(3) -0.001(3) C11 0.075(6) 0.050(4) 0.072(5) 0.006(4) -0.026(4) 0.015(4) C12 0.048(4) 0.071(5) 0.073(5) 0.028(4) 0.008(4) 0.045(4) C13 0.060(5) 0.084(6) 0.077(6) 0.019(5) -0.014(4) -0.004(5) C14 0.058(5) 0.073(6) 0.110(7) -0.050(5) -0.048(5) 0.017(4) C15 0.029(4) 0.043(4) 0.122(8) -0.040(4) -0.008(4) 0.008(3) C16 0.045(4) 0.034(3) 0.068(4) -0.012(3) 0.019(3) -0.010(3) C17 0.047(4) 0.028(3) 0.044(3) -0.004(2) 0.021(3) -0.010(3) C18 0.036(3) 0.033(3) 0.034(3) -0.002(2) 0.013(2) 0.001(2) P1 0.0384(9) 0.0367(8) 0.0401(8) 0.0080(6) 0.0076(7) 0.0056(7) F11 0.094(4) 0.175(7) 0.061(3) 0.023(4) -0.026(3) -0.048(4) F12 0.117(4) 0.090(4) 0.055(3) -0.010(3) -0.012(3) -0.032(3) F13 0.118(5) 0.074(4) 0.186(7) 0.055(4) 0.080(5) 0.063(4) F14 0.082(3) 0.044(2) 0.098(4) 0.002(2) 0.033(3) 0.014(2) F15 0.059(3) 0.060(3) 0.084(3) 0.021(2) 0.029(2) -0.007(2) F16 0.051(3) 0.088(3) 0.085(3) 0.030(3) 0.029(2) 0.008(2) loop_ _geom_bond_atom_site_label_1 _geom_bond_site_symmetry_1 _geom_bond_atom_site_label_2 _geom_bond_site_symmetry_2 _geom_bond_distance _geom_bond_publ_flag Pd1 . Se1 . 2.4191(5) yes Pd1 . Se1 4_656 2.4191(5) yes Pd1 . Se2 . 2.4183(5) yes Pd1 . Se2 4_656 2.4183(5) yes Se1 . C1 . 1.913(5) yes Se1 . C11 . 1.892(8) yes Se2 . C2 . 1.924(6) yes Se2 . C18 . 1.974(6) yes O1 . C12 . 1.52(1) yes O1 . C13 . 1.34(1) yes O2 . C14 . 1.48(1) yes O2 . C15 . 1.382(11) yes O3 . C16 . 1.431(7) yes O3 . C17 . 1.426(7) yes C1 . C2 . 1.393(8) yes C1 . C6 . 1.386(8) yes C2 . C3 . 1.395(9) yes C3 . C4 . 1.39(1) yes C4 . C5 . 1.386(11) yes C5 . C6 . 1.39(1) yes C11 . C12 . 1.403(12) yes C13 . C14 . 1.402(14) yes C15 . C16 . 1.526(11) yes C17 . C18 . 1.499(8) yes P1 . F11 . 1.565(5) yes P1 . F12 . 1.570(5) yes P1 . F13 . 1.561(5) yes P1 . F14 . 1.579(4) yes P1 . F15 . 1.588(4) yes P1 . F16 . 1.586(4) yes O21 . C211 . 1.59(4) yes O21 . C211 5_655 1.59(4) yes O21 . C221 . 1.59(4) yes O21 . C221 5_655 1.59(4) yes C211 . C211 5_655 1.39(8) yes C211 . C212 . 1.11(4) yes C221 . C221 5_655 1.37(6) yes C221 . C222 . 1.20(3) yes loop_ _geom_angle_atom_site_label_1 _geom_angle_site_symmetry_1 _geom_angle_atom_site_label_2 _geom_angle_site_symmetry_2 _geom_angle_atom_site_label_3 _geom_angle_site_symmetry_3 _geom_angle _geom_angle_publ_flag Se1 . Pd1 . Se1 4_656 180. yes Se1 . Pd1 . Se2 . 90.189(19) yes Se1 4_656 Pd1 . Se2 . 89.811(19) yes Se1 . Pd1 . Se2 4_656 89.811(19) yes Se1 4_656 Pd1 . Se2 4_656 90.189(19) yes Se2 . Pd1 . Se2 4_656 180. yes Pd1 . Se1 . C1 . 103.25(16) yes Pd1 . Se1 . C11 . 105.9(2) yes C1 . Se1 . C11 . 102.5(3) yes Pd1 . Se2 . C2 . 102.28(18) yes Pd1 . Se2 . C18 . 104.86(17) yes C2 . Se2 . C18 . 97.7(2) yes C12 . O1 . C13 . 118.3(6) yes C14 . O2 . C15 . 117.7(6) yes C16 . O3 . C17 . 115.4(4) yes Se1 . C1 . C2 . 121.2(4) yes Se1 . C1 . C6 . 117.8(4) yes C2 . C1 . C6 . 120.8(5) yes Se2 . C2 . C1 . 122.5(4) yes Se2 . C2 . C3 . 117.3(5) yes C1 . C2 . C3 . 120.1(5) yes C2 . C3 . C4 . 119.1(6) yes C3 . C4 . C5 . 120.1(6) yes C4 . C5 . C6 . 121.2(6) yes C1 . C6 . C5 . 118.6(6) yes Se1 . C11 . C12 . 116.4(5) yes O1 . C12 . C11 . 114.2(6) yes O1 . C13 . C14 . 111.9(8) yes O2 . C14 . C13 . 115.4(6) yes O2 . C15 . C16 . 112.1(5) yes O3 . C16 . C15 . 113.8(6) yes O3 . C17 . C18 . 110.4(5) yes Se2 . C18 . C17 . 108.7(4) yes F11 . P1 . F12 . 177.7(4) yes F11 . P1 . F13 . 91.5(5) yes F12 . P1 . F13 . 90.3(4) yes F11 . P1 . F14 . 89.7(4) yes F12 . P1 . F14 . 88.5(3) yes F13 . P1 . F14 . 178.8(4) yes F11 . P1 . F15 . 90.1(3) yes F12 . P1 . F15 . 91.3(3) yes F13 . P1 . F15 . 89.8(3) yes F14 . P1 . F15 . 90.2(2) yes F11 . P1 . F16 . 89.9(3) yes F12 . P1 . F16 . 88.7(3) yes F13 . P1 . F16 . 90.7(3) yes F14 . P1 . F16 . 89.3(3) yes F15 . P1 . F16 . 179.5(3) yes C211 . O21 . C211 5_655 51.8(31) yes C211 . O21 . C221 . 166.9(20) yes C211 5_655 O21 . C221 . 130.5(19) yes C211 . O21 . C221 5_655 130.5(19) yes C211 5_655 O21 . C221 5_655 166.9(20) yes C221 . O21 . C221 5_655 51.1(24) yes O21 . C211 . C211 5_655 64.1(16) yes O21 . C211 . C212 . 115.6(37) yes C211 5_655 C211 . C212 . 51.5(26) yes C211 . C212 . C211 5_655 77.0(52) yes O21 . C221 . C221 5_655 64.5(12) yes O21 . C221 . C222 . 119.5(26) yes C221 5_655 C221 . C222 . 55.1(18) yes C221 . C222 . C221 5_655 69.8(36) yes #====END