#------------------------------------------------------------------------------ #$Date: 2018-08-13 01:26:53 +0300 (Mon, 13 Aug 2018) $ #$Revision: 209639 $ #$URL: file:///home/coder/svn-repositories/cod/cif/2/01/23/2012394.cif $ #------------------------------------------------------------------------------ # # This file is available in the Crystallography Open Database (COD), # http://www.crystallography.net/ # # All data on this site have been placed in the public domain by the # contributors. # data_2012394 loop_ _publ_author_name 'Otto, Stefanus' 'Muller, Alfred Johannes' _publ_section_title ; cis-Dichlorobis(triethylarsine)platinum(II) and cis-dichlorobis(triethylphosphine)platinum(II) ; _journal_coden_ASTM ACSCEE _journal_issue 12 _journal_name_full ; Acta Crystallographica, Section C: Crystal Structure Communications ; _journal_page_first 1405 _journal_page_last 1407 _journal_paper_doi 10.1107/S0108270101016043 _journal_volume 57 _journal_year 2001 _chemical_formula_iupac '[Pt Cl2 (C6 H15 As)2]' _chemical_formula_moiety 'C12 H30 As2 Cl2 Pt' _chemical_formula_sum 'C12 H30 As2 Cl2 Pt' _chemical_formula_weight 590.19 _chemical_name_systematic cis-dichlorobis(triethylarsine)platinum(II) _space_group_crystal_system monoclinic _space_group_IT_number 14 _space_group_name_Hall '-P 2yn' _space_group_name_H-M_alt 'P 1 21/n 1' _atom_sites_solution_hydrogens geom _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _audit_creation_method SHELXL-97 _cell_angle_alpha 90.00 _cell_angle_beta 94.20(3) _cell_angle_gamma 90.00 _cell_formula_units_Z 4 _cell_length_a 8.0566(16) _cell_length_b 17.754(4) _cell_length_c 13.083(3) _cell_measurement_reflns_used 6559 _cell_measurement_temperature 293(2) _cell_measurement_theta_max 30.87 _cell_measurement_theta_min 2.29 _cell_volume 1866.4(6) _computing_cell_refinement 'SAINT (Siemens, 1995)' _computing_data_collection 'SMART (Siemens, 1995)' _computing_data_reduction SAINT _computing_molecular_graphics 'DIAMOND (Brandenburg, 1999)' _computing_publication_material SHELXL97 _computing_structure_refinement 'SHELXL97 (Sheldrick, 1997)' _computing_structure_solution 'SHELXS97 (Sheldrick, 1997)' _diffrn_ambient_temperature 293(2) _diffrn_detector_area_resol_mean ? _diffrn_measured_fraction_theta_full .917 _diffrn_measured_fraction_theta_max .917 _diffrn_measurement_device_type 'Siemens SMART CCD' _diffrn_measurement_method \w _diffrn_radiation_monochromator graphite _diffrn_radiation_source 'rotating anode' _diffrn_radiation_type MoK\a _diffrn_radiation_wavelength .71073 _diffrn_reflns_av_R_equivalents .0708 _diffrn_reflns_av_sigmaI/netI .0642 _diffrn_reflns_limit_h_max 11 _diffrn_reflns_limit_h_min -11 _diffrn_reflns_limit_k_max 24 _diffrn_reflns_limit_k_min -25 _diffrn_reflns_limit_l_max 17 _diffrn_reflns_limit_l_min -19 _diffrn_reflns_number 19330 _diffrn_reflns_theta_full 31.93 _diffrn_reflns_theta_max 31.93 _diffrn_reflns_theta_min 1.94 _diffrn_standards_decay_% none _diffrn_standards_number 'First 50 frames repeated after data collection.' _exptl_absorpt_coefficient_mu 11.306 _exptl_absorpt_correction_T_max .651 _exptl_absorpt_correction_T_min .328 _exptl_absorpt_correction_type empirical _exptl_absorpt_process_details '(SADABS; Sheldrick, 1996)' _exptl_crystal_colour colourless _exptl_crystal_density_diffrn 2.100 _exptl_crystal_density_method 'not measured' _exptl_crystal_description rectangular _exptl_crystal_F_000 1120 _exptl_crystal_size_max .119 _exptl_crystal_size_mid .112 _exptl_crystal_size_min .038 _exptl_special_details ; For both complexes, the intensity data were collected on a Siemens SMART CCD diffractometer using an exposure time of 15 s per frame for (I) and 20 s per frame for (II). A total of 1890 frames with a frame width of 0.25\% were collected for (I) and 2250 frames with a frame width of 0.20\% were collected for (II). A completeness of 98.9% was accomplished up to \q = 30.50\% for (I), while the completeness was 99.0% at \q = 30.51\% for (II). The first 50 frames were recollected at the end of each data collection to check for decay; no decay was found for either data collection. ; _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. ; _refine_diff_density_max 1.139 _refine_diff_density_min -2.048 _refine_ls_extinction_method none _refine_ls_goodness_of_fit_ref .930 _refine_ls_hydrogen_treatment constr _refine_ls_matrix_type full _refine_ls_number_parameters 162 _refine_ls_number_reflns 5905 _refine_ls_number_restraints 0 _refine_ls_restrained_S_all .930 _refine_ls_R_factor_all .0584 _refine_ls_R_factor_gt .0343 _refine_ls_shift/su_max .002 _refine_ls_shift/su_mean .000 _refine_ls_structure_factor_coef Fsqd _refine_ls_weighting_details 'calc w = 1/[\s^2^(Fo^2^)+(0.0281P)^2^] where P = (Fo^2^+2Fc^2^)/3' _refine_ls_weighting_scheme calc _refine_ls_wR_factor_gt .0661 _refine_ls_wR_factor_ref .0720 _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. ; _reflns_number_gt 4285 _reflns_number_total 5905 _reflns_threshold_expression I>2\s(I) _cod_depositor_comments ; Adding additional information after consulting the original supplementary material. Antanas Vaitkus, 2018-08-13 The following automatic conversions were performed: '_symmetry_cell_setting' value 'Monoclinic' changed to 'monoclinic' according to '/home/saulius/struct/CIF-dictionaries/cif_core.dic' dictionary named 'cif_core.dic' version 2.4.1 from 2010-06-29. '_geom_bond_publ_flag' value 'Yes' changed to 'yes' according to '/home/saulius/struct/CIF-dictionaries/cif_core.dic' dictionary named 'cif_core.dic' version 2.4.1 from 2010-06-29 (4 times). Automatic conversion script Id: cif_fix_enum 1527 2010-12-29 10:47:43Z saulius ; _cod_original_sg_symbol_H-M 'P 21/n' _cod_database_code 2012394 loop_ _space_group_symop_id _space_group_symop_operation_xyz 1 x,y,z 2 -x+1/2,y+1/2,-z+1/2 3 -x,-y,-z 4 x-1/2,-y-1/2,z-1/2 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_calc_flag _atom_site_refinement_flags _atom_site_occupancy _atom_site_disorder_assembly _atom_site_disorder_group Pt Pt .23175(2) .197343(9) .191580(13) .02951(6) Uani d . 1 . . As1 As .34578(5) .07684(2) .22491(3) .03068(10) Uani d . 1 . . As2 As .48241(6) .26115(2) .16514(4) .03327(11) Uani d . 1 . . Cl1 Cl .08491(18) .31085(7) .17214(12) .0565(4) Uani d . 1 . . Cl2 Cl -.01854(15) .13713(8) .22449(12) .0573(4) Uani d . 1 . . C111 C .5813(6) .0591(2) .2122(4) .0434(12) Uani d . 1 . . H11A H .6046 .0683 .1415 .059(5) Uiso calc R 1 . . H11B H .6439 .0958 .2542 .059(5) Uiso calc R 1 . . C112 C .6456(7) -.0192(3) .2422(5) .0681(18) Uani d . 1 . . H11C H .6388 -.0264 .3145 .092(5) Uiso calc R 1 . . H11D H .7594 -.0238 .2258 .092(5) Uiso calc R 1 . . H11E H .5792 -.0565 .2053 .092(5) Uiso calc R 1 . . C121 C .3091(7) .0442(3) .3639(4) .0455(12) Uani d . 1 . . H12A H .1903 .0427 .3717 .059(5) Uiso calc R 1 . . H12B H .3520 -.0065 .3739 .059(5) Uiso calc R 1 . . C122 C .3904(10) .0946(4) .4449(4) .081(2) Uani d . 1 . . H12C H .5083 .0957 .4383 .092(5) Uiso calc R 1 . . H12D H .3690 .0756 .5114 .092(5) Uiso calc R 1 . . H12E H .3460 .1445 .4368 .092(5) Uiso calc R 1 . . C131 C .2339(7) -.0035(3) .1456(4) .0482(13) Uani d . 1 . . H13A H .2885 -.0509 .1636 .059(5) Uiso calc R 1 . . H13B H .1199 -.0070 .1643 .059(5) Uiso calc R 1 . . C132 C .2333(9) .0077(4) .0309(5) .0701(18) Uani d . 1 . . H13C H .1811 .0549 .0125 .092(5) Uiso calc R 1 . . H13D H .1727 -.0326 -.0036 .092(5) Uiso calc R 1 . . H13E H .3457 .0079 .0111 .092(5) Uiso calc R 1 . . C211 C .4630(7) .3668(3) .1233(4) .0542(14) Uani d . 1 . . H21A H .3913 .3925 .1684 .059(5) Uiso calc R 1 . . H21B H .5721 .3900 .1321 .059(5) Uiso calc R 1 . . C212 C .3950(9) .3786(3) .0145(5) .0706(18) Uani d . 1 . . H21C H .4748 .3615 -.0313 .092(5) Uiso calc R 1 . . H21D H .3729 .4312 .0031 .092(5) Uiso calc R 1 . . H21E H .2936 .3505 .0023 .092(5) Uiso calc R 1 . . C221 C .6271(6) .2693(3) .2907(4) .0514(14) Uani d . 1 . . H22A H .6623 .2193 .3128 .059(5) Uiso calc R 1 . . H22B H .7257 .2977 .2766 .059(5) Uiso calc R 1 . . C222 C .5421(9) .3078(3) .3771(5) .0688(18) Uani d . 1 . . H22C H .5240 .3600 .3606 .092(5) Uiso calc R 1 . . H22D H .6116 .3038 .4397 .092(5) Uiso calc R 1 . . H22E H .4371 .2838 .3855 .092(5) Uiso calc R 1 . . C231 C .6287(6) .2227(3) .0649(4) .0400(11) Uani d . 1 . . H23A H .7011 .2631 .0454 .059(5) Uiso calc R 1 . . H23B H .6985 .1834 .0967 .059(5) Uiso calc R 1 . . C232 C .5369(8) .1912(3) -.0309(5) .0606(16) Uani d . 1 . . H23C H .4677 .1500 -.0127 .092(5) Uiso calc R 1 . . H23D H .6159 .1737 -.0770 .092(5) Uiso calc R 1 . . H23E H .4690 .2299 -.0637 .092(5) Uiso calc R 1 . . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_12 _atom_site_aniso_U_13 _atom_site_aniso_U_23 Pt .02428(9) .03401(9) .03033(9) .00395(7) .00265(6) .00006(7) As1 .0277(2) .0305(2) .0341(2) .00035(17) .00402(18) .00045(18) As2 .0317(2) .0325(2) .0359(2) -.00120(18) .00457(19) -.00042(19) Cl1 .0492(8) .0485(7) .0729(10) .0213(6) .0117(7) .0099(6) Cl2 .0249(6) .0626(8) .0854(10) .0004(6) .0094(6) .0121(7) C111 .034(3) .034(2) .064(3) .005(2) .013(2) .006(2) C112 .049(3) .058(3) .100(5) .025(3) .022(3) .030(3) C121 .049(3) .048(3) .040(3) .001(2) .010(2) .007(2) C122 .129(7) .073(4) .040(3) -.008(4) -.003(4) -.002(3) C131 .048(3) .041(3) .055(3) -.005(2) -.005(2) -.008(2) C132 .081(5) .077(4) .051(4) -.012(4) -.004(3) -.016(3) C211 .064(4) .036(3) .064(4) -.001(2) .015(3) .004(3) C212 .095(5) .053(3) .065(4) .017(3) .017(4) .016(3) C221 .043(3) .051(3) .057(3) -.001(2) -.010(3) -.004(3) C222 .078(5) .084(4) .044(3) .002(3) -.002(3) -.019(3) C231 .034(3) .044(2) .044(3) .001(2) .013(2) .005(2) C232 .071(4) .059(3) .053(4) .002(3) .019(3) -.011(3) loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source C C .0033 .0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' H H .0000 .0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Cl Cl .1484 .1585 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' As As .0499 2.0058 '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' loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle _geom_angle_publ_flag Cl1 Pt Cl2 . . 88.74(5) yes As1 Pt As2 . . 97.85(2) yes As1 Pt Cl1 . . 171.37(4) yes As2 Pt Cl2 . . 177.45(4) yes As1 Pt Cl2 . . 83.18(4) yes As2 Pt Cl1 . . 90.11(4) yes C111 As1 C131 . . 104.6(2) yes C111 As1 C121 . . 104.3(2) yes C131 As1 C121 . . 100.5(2) yes C111 As1 Pt . . 120.08(13) ? C131 As1 Pt . . 114.09(15) ? C121 As1 Pt . . 111.00(15) ? C221 As2 C231 . . 103.9(2) yes C221 As2 C211 . . 101.2(2) yes C231 As2 C211 . . 100.8(2) yes C221 As2 Pt . . 112.16(17) ? C231 As2 Pt . . 119.72(14) ? C211 As2 Pt . . 116.67(18) ? C112 C111 As1 . . 116.2(4) ? C112 C111 H11A . . 108.2 ? As1 C111 H11A . . 108.2 ? C112 C111 H11B . . 108.2 ? As1 C111 H11B . . 108.2 ? H11A C111 H11B . . 107.4 ? C111 C112 H11C . . 109.5 ? C111 C112 H11D . . 109.5 ? H11C C112 H11D . . 109.5 ? C111 C112 H11E . . 109.5 ? H11C C112 H11E . . 109.5 ? H11D C112 H11E . . 109.5 ? C122 C121 As1 . . 113.2(4) ? C122 C121 H12A . . 108.9 ? As1 C121 H12A . . 108.9 ? C122 C121 H12B . . 108.9 ? As1 C121 H12B . . 108.9 ? H12A C121 H12B . . 107.8 ? C121 C122 H12C . . 109.5 ? C121 C122 H12D . . 109.5 ? H12C C122 H12D . . 109.5 ? C121 C122 H12E . . 109.5 ? H12C C122 H12E . . 109.5 ? H12D C122 H12E . . 109.5 ? C132 C131 As1 . . 113.6(4) ? C132 C131 H13A . . 108.9 ? As1 C131 H13A . . 108.9 ? C132 C131 H13B . . 108.9 ? As1 C131 H13B . . 108.9 ? H13A C131 H13B . . 107.7 ? C131 C132 H13C . . 109.5 ? C131 C132 H13D . . 109.5 ? H13C C132 H13D . . 109.5 ? C131 C132 H13E . . 109.5 ? H13C C132 H13E . . 109.5 ? H13D C132 H13E . . 109.5 ? C212 C211 As2 . . 114.5(4) ? C212 C211 H21A . . 108.6 ? As2 C211 H21A . . 108.6 ? C212 C211 H21B . . 108.6 ? As2 C211 H21B . . 108.6 ? H21A C211 H21B . . 107.6 ? C211 C212 H21C . . 109.5 ? C211 C212 H21D . . 109.5 ? H21C C212 H21D . . 109.5 ? C211 C212 H21E . . 109.5 ? H21C C212 H21E . . 109.5 ? H21D C212 H21E . . 109.5 ? C222 C221 As2 . . 112.7(4) ? C222 C221 H22A . . 109.1 ? As2 C221 H22A . . 109.1 ? C222 C221 H22B . . 109.1 ? As2 C221 H22B . . 109.1 ? H22A C221 H22B . . 107.8 ? C221 C222 H22C . . 109.5 ? C221 C222 H22D . . 109.5 ? H22C C222 H22D . . 109.5 ? C221 C222 H22E . . 109.5 ? H22C C222 H22E . . 109.5 ? H22D C222 H22E . . 109.5 ? C232 C231 As2 . . 113.8(4) ? C232 C231 H23A . . 108.8 ? As2 C231 H23A . . 108.8 ? C232 C231 H23B . . 108.8 ? As2 C231 H23B . . 108.8 ? H23A C231 H23B . . 107.7 ? C231 C232 H23C . . 109.5 ? C231 C232 H23D . . 109.5 ? H23C C232 H23D . . 109.5 ? C231 C232 H23E . . 109.5 ? H23C C232 H23E . . 109.5 ? H23D C232 H23E . . 109.5 ? loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_site_symmetry_2 _geom_bond_distance _geom_bond_publ_flag Pt Cl1 . 2.3412(12) yes Pt Cl2 . 2.3498(13) yes Pt As1 . 2.3563(6) yes Pt As2 . 2.3630(6) yes As1 C111 . 1.942(5) yes As1 C131 . 1.946(4) yes As1 C121 . 1.952(5) yes As2 C221 . 1.949(5) yes As2 C231 . 1.950(5) yes As2 C211 . 1.957(5) yes C111 C112 . 1.525(6) ? C111 H11A . .9700 ? C111 H11B . .9700 ? C112 H11C . .9600 ? C112 H11D . .9600 ? C112 H11E . .9600 ? C121 C122 . 1.500(7) ? C121 H12A . .9700 ? C121 H12B . .9700 ? C122 H12C . .9600 ? C122 H12D . .9600 ? C122 H12E . .9600 ? C131 C132 . 1.514(8) ? C131 H13A . .9700 ? C131 H13B . .9700 ? C132 H13C . .9600 ? C132 H13D . .9600 ? C132 H13E . .9600 ? C211 C212 . 1.501(8) ? C211 H21A . .9700 ? C211 H21B . .9700 ? C212 H21C . .9600 ? C212 H21D . .9600 ? C212 H21E . .9600 ? C221 C222 . 1.525(8) ? C221 H22A . .9700 ? C221 H22B . .9700 ? C222 H22C . .9600 ? C222 H22D . .9600 ? C222 H22E . .9600 ? C231 C232 . 1.515(7) ? C231 H23A . .9700 ? C231 H23B . .9700 ? C232 H23C . .9600 ? C232 H23D . .9600 ? C232 H23E . .9600 ? 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_site_symmetry_1 _geom_torsion_site_symmetry_2 _geom_torsion_site_symmetry_3 _geom_torsion_site_symmetry_4 _geom_torsion _geom_torsion_publ_flag Cl2 Pt As1 C111 . . . . 177.4(2) yes Cl2 Pt As1 C121 . . . . -60.69(17) yes Cl2 Pt As1 C131 . . . . 52.0(2) yes Cl1 Pt As2 C211 . . . . -7.68(19) yes Cl1 Pt As2 C221 . . . . 108.44(17) yes Cl1 Pt As2 C231 . . . . -129.54(17) yes As1 Pt As2 C211 . . . . 175.68(19) yes As1 Pt As2 C221 . . . . -68.20(17) yes As1 Pt As2 C231 . . . . 53.83(16) yes As2 Pt As1 C111 . . . . -4.96(19) yes As2 Pt As1 C121 . . . . 116.96(17) yes As2 Pt As1 C131 . . . . -130.3(2) yes loop_ _cod_related_entry_id _cod_related_entry_database _cod_related_entry_code 1 ChemSpider 30652334