#------------------------------------------------------------------------------ #$Date: 2011-09-10 04:16:28 +0100 (Sat, 10 Sep 2011) $ #$Revision: 25271 $ #$URL: svn://www.crystallography.net/cod/cif/2/2006938.cif $ #------------------------------------------------------------------------------ # # This file is available in the Crystallography Open Database (COD), # http://www.crystallography.net/. The original data for this entry # were provided by IUCr Journals, http://journals.iucr.org/. # # The file may be used within the scientific community so long as # proper attribution is given to the journal article from which the # data were obtained. # data_2006938 loop_ _publ_author_name 'Marzotto, A.' 'Clemente, D. A.' 'Valle, G.' _publ_contact_author ; Prof Armando Marzotto Dipartimento di Chimica Inorganica, Metallorganica ed Analitica Universit\`a degli Studi di Padova Via Loredan n. 4 I-35131 Padova Italy ; _publ_section_title ; Platinum(II) Complexes of Piperazine (and Derivatives): trans-Dichlorobis(N-methylpiperazine-N')platinum(II) ; _journal_issue 1 _journal_name_full 'Acta Crystallographica Section C' _journal_page_first 27 _journal_page_last 29 _journal_volume 54 _journal_year 1998 _chemical_formula_iupac '[Pt Cl2 (C5 H12 N2)2]' _chemical_formula_moiety 'C10 H24 Cl2 N4 Pt' _chemical_formula_sum 'C10 H24 Cl2 N4 Pt' _chemical_formula_weight 466.32 _chemical_name_systematic ; trans-[bis(N-methylpiperazine)dichloroplatinum(II)] ; _space_group_IT_number 14 _symmetry_cell_setting monoclinic _symmetry_space_group_name_Hall '-P 2ybc' _symmetry_space_group_name_H-M 'P 1 21/c 1' _audit_creation_method 'SHELXL-93 and manual form' _cell_angle_alpha 90.00 _cell_angle_beta 95.10(4) _cell_angle_gamma 90.00 _cell_formula_units_Z 2 _cell_length_a 6.451(2) _cell_length_b 13.307(2) _cell_length_c 8.885(2) _cell_measurement_reflns_used 25 _cell_measurement_temperature 293(2) _cell_measurement_theta_max 15 _cell_measurement_theta_min 10 _cell_volume 759.7(3) _computing_cell_refinement 'Philips PW1100/20 software' _computing_data_collection 'Philips PW1100/20 software' _computing_data_reduction 'RIFLUP80 (Biagini et al., 1980)' _computing_molecular_graphics 'ORTEPII (Johnson, 1976)' _computing_structure_refinement 'SHELXL93 (Sheldrick, 1993)' _computing_structure_solution 'using coordinates of isomorphous Pd-complex' _diffrn_ambient_temperature 293(2) _diffrn_measurement_device 'Philips PW1100/20 diffractometer' _diffrn_measurement_method \q/2\q _diffrn_radiation_monochromator graphite _diffrn_radiation_source 'fine-focus sealed X-ray tube' _diffrn_radiation_type 'Mo K\a' _diffrn_radiation_wavelength 0.71070 _diffrn_reflns_av_R_equivalents 0.0178 _diffrn_reflns_av_sigmaI/netI 0.0223 _diffrn_reflns_limit_h_max 8 _diffrn_reflns_limit_h_min -8 _diffrn_reflns_limit_k_max 17 _diffrn_reflns_limit_k_min 0 _diffrn_reflns_limit_l_max 11 _diffrn_reflns_limit_l_min 0 _diffrn_reflns_number 1942 _diffrn_reflns_theta_max 27.99 _diffrn_reflns_theta_min 2.76 _diffrn_standards_decay_% 0 _diffrn_standards_interval_time 90 _diffrn_standards_number 3 _exptl_absorpt_coefficient_mu 9.573 _exptl_absorpt_correction_T_max 0.091 _exptl_absorpt_correction_T_min 0.049 _exptl_absorpt_correction_type 'semi-empirical, \y scans (North, Phillips & Mathews, 1968)' _exptl_crystal_colour Yellow _exptl_crystal_density_diffrn 2.039 _exptl_crystal_density_meas 'not measured' _exptl_crystal_description prism _exptl_crystal_F_000 448 _exptl_crystal_size_max 0.30 _exptl_crystal_size_mid 0.30 _exptl_crystal_size_min 0.25 _refine_diff_density_max 1.218 _refine_diff_density_min -1.869 _refine_ls_extinction_method none _refine_ls_goodness_of_fit_all 1.018 _refine_ls_goodness_of_fit_obs 1.104 _refine_ls_hydrogen_treatment 'H atoms riding with fixed U' _refine_ls_matrix_type full _refine_ls_number_parameters 79 _refine_ls_number_reflns 1837 _refine_ls_number_restraints 0 _refine_ls_restrained_S_all 1.018 _refine_ls_restrained_S_obs 1.104 _refine_ls_R_factor_all 0.0441 _refine_ls_R_factor_obs 0.0242 _refine_ls_shift/esd_max 0.000 _refine_ls_shift/esd_mean 0.000 _refine_ls_structure_factor_coef Fsqd _refine_ls_weighting_scheme 'calc w = 1/[\s^2^(Fo^2^)+(0.0439P)^2^] where P=(Fo^2^+2Fc^2^)/3' _refine_ls_wR_factor_all 0.0706 _refine_ls_wR_factor_obs 0.0635 _reflns_number_observed 1289 _reflns_number_total 1837 _reflns_observed_criterion I>2sigma(I) _[local]_cod_data_source_file ln1009.cif _[local]_cod_data_source_block apt10n _[local]_cod_cif_authors_sg_H-M 'P 21/c ' _cod_database_code 2006938 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' 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 0.03351(14) 0.03215(14) 0.03267(15) -0.00280(9) 0.00179(9) -0.00334(9) Cl1 0.0541(7) 0.0536(6) 0.0385(6) -0.0108(6) 0.0105(6) -0.0058(5) N1 0.037(2) 0.037(2) 0.036(2) -0.0028(15) 0.007(2) -0.004(2) N2 0.043(2) 0.035(2) 0.045(2) -0.006(2) 0.001(2) -0.002(2) C1 0.033(2) 0.037(2) 0.053(3) 0.002(2) 0.005(2) -0.006(2) C2 0.046(3) 0.030(2) 0.047(3) 0.002(2) 0.007(2) 0.003(2) C3 0.027(2) 0.046(3) 0.058(3) -0.003(2) 0.001(2) -0.005(2) C4 0.034(3) 0.036(2) 0.047(3) 0.004(2) 0.002(2) -0.006(2) C5 0.055(3) 0.042(3) 0.080(5) -0.014(2) 0.003(3) -0.003(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_thermal_displace_type _atom_site_calc_flag _atom_site_refinement_flags _atom_site_occupancy _atom_site_type_symbol Pt 0 0 0 0.03285(10) Uani d S 1 Pt Cl1 0.0694(2) -0.02579(10) -0.2466(2) 0.0484(3) Uani d . 1 Cl N1 0.1920(6) 0.1236(2) 0.0027(4) 0.0363(8) Uani d . 1 N H1 0.2410(6) 0.1267(2) -0.0901(4) 0.044 Uiso calc R 1 H N2 0.4073(6) 0.2970(3) 0.1440(5) 0.0409(9) Uani d . 1 N C1 0.0884(8) 0.2214(3) 0.0261(6) 0.0408(11) Uani d . 1 C H1A 0.0276(8) 0.2201(3) 0.1221(6) 0.049 Uiso calc R 1 H H1B -0.0234(8) 0.2310(3) -0.0531(6) 0.049 Uiso calc R 1 H C2 0.2387(8) 0.3086(3) 0.0249(6) 0.0408(11) Uani d . 1 C H2A 0.2958(8) 0.3118(3) -0.0724(6) 0.049 Uiso calc R 1 H H2B 0.1653(8) 0.3709(3) 0.0396(6) 0.049 Uiso calc R 1 H C3 0.5201(7) 0.2046(3) 0.1150(6) 0.0440(11) Uani d . 1 C H3A 0.6340(7) 0.1957(3) 0.1927(6) 0.053 Uiso calc R 1 H H3B 0.5785(7) 0.2098(3) 0.0184(6) 0.053 Uiso calc R 1 H C4 0.3763(7) 0.1144(3) 0.1135(6) 0.0391(10) Uani d . 1 C H4A 0.4536(7) 0.0547(3) 0.0902(6) 0.047 Uiso calc R 1 H H4B 0.3298(7) 0.1057(3) 0.2135(6) 0.047 Uiso calc R 1 H C5 0.5497(9) 0.3825(4) 0.1440(7) 0.059(2) Uani d . 1 C H5A 0.6559(9) 0.3758(4) 0.2262(7) 0.089 Uiso calc R 1 H H5B 0.4738(9) 0.4437(4) 0.1556(7) 0.089 Uiso calc R 1 H H5C 0.6128(9) 0.3842(4) 0.0502(7) 0.089 Uiso calc R 1 H loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source Pt Pt -1.7033 8.3905 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Cl Cl 0.1484 0.1585 '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' 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' loop_ _diffrn_standard_refln_index_h _diffrn_standard_refln_index_k _diffrn_standard_refln_index_l -1 4 4 3 3 3 2 3 1 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 N1 Pt Cl1 3 3 87.84(11) no N1 Pt Cl1 . 3 92.16(11) no N1 Pt Cl1 3 . 92.16(11) yes N1 Pt Cl1 . . 87.84(11) yes Cl1 Pt Cl1 3 . 180.0 no C4 N1 C1 . . 108.9(4) yes C4 N1 Pt . . 112.9(3) yes C1 N1 Pt . . 115.1(3) yes C2 N2 C5 . . 110.3(4) yes C2 N2 C3 . . 108.2(4) yes C5 N2 C3 . . 109.3(4) yes N1 C1 C2 . . 112.0(4) yes N2 C2 C1 . . 110.6(4) yes N2 C3 C4 . . 110.7(4) yes N1 C4 C3 . . 113.3(4) yes 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 N1 3 2.058(3) no Pt N1 . 2.058(3) yes Pt Cl1 3 2.3005(15) no Pt Cl1 . 2.3005(15) yes N1 C4 . 1.479(5) yes N1 C1 . 1.486(5) yes N2 C2 . 1.457(6) yes N2 C5 . 1.462(6) yes N2 C3 . 1.464(6) yes C1 C2 . 1.513(6) yes C3 C4 . 1.517(6) yes loop_ _geom_contact_atom_site_label_1 _geom_contact_atom_site_label_2 _geom_contact_distance Pt C4 2.965(4) Cl1 H1 2.646(3) N1 N2 2.919(5) N1 H2A 2.692(5) N1 C3 2.502(6) N1 H3B 2.737(6) H1 H1A 2.730(6) H1 C2 2.628(5) H1 C3 2.656(6) H1 H3B 2.553(6) H1 H4B 2.722(6) N2 H1A 2.645(6) N2 H4B 2.677(6) C1 C3 2.835(7) C1 H4B 2.666(7) H1A H2A 2.828(7) H1A C4 2.659(7) H1A H4B 2.548(6) C2 H3B 2.561(7) C2 C4 2.822(6) C2 H5B 2.563(7) C2 H5C 2.606(8) H2A C3 2.544(7) H2A C5 2.589(8) H2A H5B 2.844(7) H2B C5 2.574(8) H2B H5C 2.885(8) C3 H5A 2.604(7) C3 H5C 2.542(7) H3A C5 2.573(7) H3A H5C 2.808(7) H3B H4B 2.827(7) H3B C5 2.569(7) H3B H5A 2.894(7) 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_publ_flag N1 C1 C2 N2 -59.7(5) yes N2 C3 C4 N1 56.5(6) yes