#------------------------------------------------------------------------------ #$Date: 2016-02-20 00:18:51 +0200 (Sat, 20 Feb 2016) $ #$Revision: 176760 $ #$URL: file:///home/coder/svn-repositories/cod/cif/2/01/53/2015319.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_2015319 loop_ _publ_author_name 'Kato, Masako' 'Okada, Yoshiko' 'Shishido, Yasuko' 'Kishi, Shinobu' _publ_section_title ; Dichloro(4,4'-dialkyl-2,2'-bipyridine-\k^2^N,N')platinum(II), where alkyl is pentyl and heptyl ; _journal_coeditor_code OB1249 _journal_issue 5 _journal_name_full 'Acta Crystallographica Section C' _journal_page_first m171 _journal_page_last m173 _journal_paper_doi 10.1107/S010827010600758X _journal_volume 62 _journal_year 2006 _chemical_formula_iupac '[Pt Cl2 (C20 H28 N2)]' _chemical_formula_moiety 'C20 H28 Cl2 N2 Pt' _chemical_formula_sum 'C20 H28 Cl2 N2 Pt' _chemical_formula_weight 562.45 _chemical_melting_point .483E-305 _chemical_name_systematic ; Dichloro(4,4'-dipentyl-2,2'-bipyridine-\k^2^N,N')platinum(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' _cell_angle_alpha 90.0000 _cell_angle_beta 94.3564(9) _cell_angle_gamma 90.0000 _cell_formula_units_Z 4 _cell_length_a 7.1791(19) _cell_length_b 13.853(4) _cell_length_c 20.609(5) _cell_measurement_reflns_used 6090 _cell_measurement_temperature 173.1 _cell_measurement_theta_max 27.5 _cell_measurement_theta_min 3.1 _cell_volume 2043.7(9) _computing_cell_refinement CrystalClear _computing_data_collection 'CrystalClear (Rigaku, 2001)' _computing_data_reduction 'CrystalStructure (Rigaku/MSC, 2004)' _computing_molecular_graphics 'ORTEPII (Johnson, 1976)' _computing_publication_material CrystalStructure _computing_structure_refinement 'SHELXL97 (Sheldrick, 1997)' _computing_structure_solution 'SIR92 (Altomare et al., 1994)' _diffrn_detector_area_resol_mean 14.71 _diffrn_measured_fraction_theta_full 0.968 _diffrn_measured_fraction_theta_max 0.968 _diffrn_measurement_device_type 'Rigaku Mercury CCD area-detector' _diffrn_measurement_method \w _diffrn_radiation_type 'Mo K\a' _diffrn_radiation_wavelength 0.71070 _diffrn_reflns_av_R_equivalents 0.098 _diffrn_reflns_limit_h_max 8 _diffrn_reflns_limit_h_min -9 _diffrn_reflns_limit_k_max 17 _diffrn_reflns_limit_k_min -17 _diffrn_reflns_limit_l_max 26 _diffrn_reflns_limit_l_min -26 _diffrn_reflns_number 15324 _diffrn_reflns_theta_full 27.48 _diffrn_reflns_theta_max 27.48 _exptl_absorpt_coefficient_mu 7.105 _exptl_absorpt_correction_T_max 0.868 _exptl_absorpt_correction_T_min 0.578 _exptl_absorpt_correction_type numerical _exptl_absorpt_process_details '(NUMABS; Higashi, 1999)' _exptl_crystal_colour yellow _exptl_crystal_density_diffrn 1.828 _exptl_crystal_density_method 'not measured' _exptl_crystal_description needle _exptl_crystal_F_000 1096.00 _exptl_crystal_size_max 0.45 _exptl_crystal_size_mid 0.10 _exptl_crystal_size_min 0.10 _refine_diff_density_max 2.30 _refine_diff_density_min -3.54 _refine_ls_extinction_method none _refine_ls_goodness_of_fit_ref 0.970 _refine_ls_hydrogen_treatment constr _refine_ls_number_parameters 227 _refine_ls_number_reflns 4537 _refine_ls_R_factor_gt 0.0667 _refine_ls_shift/su_max 0.0010 _refine_ls_structure_factor_coef Fsqd _refine_ls_weighting_details 'w = 1/[\s^2^(Fo^2^)+(0.0864P)^2^] where P=(Fo^2^+2Fc^2^)/3' _refine_ls_weighting_scheme calc _refine_ls_wR_factor_ref 0.1801 _reflns_number_gt 3263 _reflns_number_total 4537 _reflns_threshold_expression F^2^>2\s(F^2^) _cod_data_source_file ob1249.cif _cod_data_source_block I _cod_original_cell_volume 2043.6(9) _cod_original_sg_symbol_H-M 'P 21/c' _cod_database_code 2015319 _cod_database_fobs_code 2015319 loop_ _symmetry_equiv_pos_site_id _symmetry_equiv_pos_as_xyz 1 +X,+Y,+Z 2 -X,1/2+Y,1/2-Z 3 -X,-Y,-Z 4 +X,1/2-Y,1/2+Z loop_ _atom_site_type_symbol _atom_site_label _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 Pt Pt1 0.29106(5) -0.07509(3) 0.58358(2) 0.02498(15) Uani d . 1.00 Cl Cl1 0.2288(4) -0.0410(2) 0.68869(14) 0.0402(6) Uani d . 1.00 Cl Cl2 0.4071(4) -0.2228(2) 0.61712(14) 0.0379(6) Uani d . 1.00 N N1 0.2012(11) 0.0540(6) 0.5472(4) 0.0253(18) Uani d . 1.00 N N2 0.3287(11) -0.0951(6) 0.4890(4) 0.0276(19) Uani d . 1.00 C C1 0.1427(13) 0.1276(8) 0.5823(5) 0.028(2) Uani d . 1.00 C C2 0.0892(13) 0.2146(7) 0.5532(5) 0.028(2) Uani d . 1.00 C C3 0.0913(13) 0.2278(7) 0.4871(5) 0.028(2) Uani d . 1.00 C C4 0.1536(13) 0.1496(7) 0.4508(5) 0.026(2) Uani d . 1.00 C C5 0.2090(13) 0.0659(6) 0.4818(5) 0.0201(19) Uani d . 1.00 C C6 0.2738(13) -0.0222(7) 0.4485(5) 0.027(2) Uani d . 1.00 C C7 0.2851(13) -0.0283(7) 0.3817(5) 0.027(2) Uani d . 1.00 C C8 0.3483(14) -0.1118(8) 0.3550(5) 0.029(2) Uani d . 1.00 C C9 0.4084(15) -0.1847(7) 0.3953(5) 0.032(2) Uani d . 1.00 C C10 0.3931(14) -0.1758(7) 0.4618(5) 0.028(2) Uani d . 1.00 C C11 0.0335(15) 0.3204(7) 0.4548(5) 0.030(2) Uani d . 1.00 C C12 0.2009(15) 0.3892(8) 0.4492(5) 0.033(2) Uani d . 1.00 C C13 0.145(2) 0.4801(8) 0.4119(7) 0.048(3) Uani d . 1.00 C C14 0.305(2) 0.5528(9) 0.4137(8) 0.054(3) Uani d . 1.00 C C15 0.468(2) 0.5176(12) 0.3781(8) 0.073(5) Uani d . 1.00 C C16 0.3572(16) -0.1205(9) 0.2813(5) 0.038(2) Uani d . 1.00 C C17 0.1605(17) -0.1332(8) 0.2480(5) 0.037(2) Uani d . 1.00 C C18 0.0697(15) -0.2271(8) 0.2671(5) 0.033(2) Uani d . 1.00 C C19 -0.1311(17) -0.2384(9) 0.2385(6) 0.043(2) Uani d . 1.00 C C20 -0.223(2) -0.3309(11) 0.2631(7) 0.060(4) Uani d . 1.00 H H1 0.1377 0.1203 0.6279 0.034 Uiso c R 1.00 H H2 0.0504 0.2661 0.5794 0.034 Uiso c R 1.00 H H4 0.1573 0.1550 0.4049 0.031 Uiso c R 1.00 H H7 0.2491 0.0250 0.3546 0.033 Uiso c R 1.00 H H9 0.4606 -0.2415 0.3782 0.038 Uiso c R 1.00 H H10 0.4293 -0.2287 0.4893 0.033 Uiso c R 1.00 H H11A -0.0607 0.3524 0.4802 0.036 Uiso c R 1.00 H H11B -0.0254 0.3067 0.4108 0.036 Uiso c R 1.00 H H12A 0.2538 0.4069 0.4934 0.039 Uiso c R 1.00 H H12B 0.2994 0.3554 0.4269 0.039 Uiso c R 1.00 H H13A 0.0364 0.5099 0.4310 0.058 Uiso c R 1.00 H H13B 0.1071 0.4633 0.3661 0.058 Uiso c R 1.00 H H14A 0.2587 0.6142 0.3938 0.065 Uiso c R 1.00 H H14B 0.3484 0.5662 0.4596 0.065 Uiso c R 1.00 H H15A 0.5649 0.5676 0.3793 0.088 Uiso c R 1.00 H H15B 0.4260 0.5033 0.3328 0.088 Uiso c R 1.00 H H15C 0.5196 0.4589 0.3992 0.088 Uiso c R 1.00 H H16A 0.4355 -0.1765 0.2713 0.045 Uiso c R 1.00 H H16B 0.4152 -0.0617 0.2644 0.045 Uiso c R 1.00 H H17A 0.0814 -0.0784 0.2599 0.045 Uiso c R 1.00 H H17B 0.1678 -0.1320 0.2003 0.045 Uiso c R 1.00 H H18A 0.0715 -0.2303 0.3152 0.040 Uiso c R 1.00 H H18B 0.1446 -0.2819 0.2525 0.040 Uiso c R 1.00 H H19A -0.1326 -0.2407 0.1904 0.051 Uiso c R 1.00 H H19B -0.2047 -0.1815 0.2504 0.051 Uiso c R 1.00 H H20A -0.3507 -0.3361 0.2433 0.072 Uiso c R 1.00 H H20B -0.2247 -0.3280 0.3106 0.072 Uiso c R 1.00 H H20C -0.1505 -0.3874 0.2511 0.072 Uiso c R 1.00 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 PT1 0.0229(2) 0.0251(2) 0.0259(2) -0.00473(14) -0.00454(16) 0.00285(16) CL1 0.0521(18) 0.0394(15) 0.0288(14) -0.0014(14) 0.0007(12) 0.0029(12) CL2 0.0408(15) 0.0307(14) 0.0406(15) 0.0015(12) -0.0067(12) 0.0102(12) N1 0.022(4) 0.022(4) 0.031(4) -0.003(3) -0.007(3) 0.001(3) N2 0.020(4) 0.030(4) 0.031(4) 0.000(3) -0.009(3) -0.009(3) C1 0.018(4) 0.041(6) 0.025(5) -0.006(4) 0.003(3) -0.005(4) C2 0.020(4) 0.025(5) 0.039(6) -0.003(4) 0.000(4) -0.008(4) C3 0.021(5) 0.024(5) 0.037(5) -0.002(4) -0.002(4) -0.003(4) C4 0.016(4) 0.035(5) 0.025(5) 0.001(4) -0.001(3) 0.001(4) C5 0.016(4) 0.018(4) 0.026(4) -0.005(3) -0.002(3) 0.010(3) C6 0.016(4) 0.028(5) 0.037(5) -0.006(4) -0.007(4) 0.007(4) C7 0.021(4) 0.027(5) 0.032(5) -0.004(4) -0.008(4) 0.010(4) C8 0.021(5) 0.029(5) 0.035(5) -0.004(4) -0.003(4) -0.004(4) C9 0.039(6) 0.025(5) 0.030(5) 0.002(4) -0.002(4) -0.013(4) C10 0.027(5) 0.023(5) 0.034(5) 0.004(4) 0.009(4) 0.009(4) C11 0.037(6) 0.022(5) 0.030(5) -0.001(4) -0.005(4) 0.001(4) C12 0.035(6) 0.030(5) 0.032(6) -0.004(4) -0.001(4) -0.004(4) C13 0.057(8) 0.026(6) 0.062(9) -0.002(6) 0.009(6) 0.002(6) C14 0.058(9) 0.032(7) 0.073(11) -0.007(6) 0.016(7) 0.006(6) C15 0.095(13) 0.057(10) 0.072(12) -0.006(9) 0.033(10) 0.012(9) C16 0.036(6) 0.038(6) 0.038(6) -0.007(5) -0.002(5) 0.007(5) C17 0.052(7) 0.033(6) 0.027(5) -0.006(5) 0.001(5) -0.004(4) C18 0.030(5) 0.042(6) 0.027(5) -0.002(5) -0.005(4) -0.003(5) C19 0.046(7) 0.040(7) 0.040(7) -0.007(5) -0.004(5) -0.009(5) C20 0.044(8) 0.068(10) 0.068(10) -0.021(7) 0.001(7) -0.020(8) loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source C C 0.003 0.002 ; International Tables for Crystallography (1992, Vol. C, Tables 4.2.6.8 and 6.1.1.4) ; H H 0.000 0.000 ; International Tables for Crystallography (1992, Vol. C, Table 6.1.1.4) ; Cl Cl 0.148 0.159 ; International Tables for Crystallography (1992, Vol. C, Tables 4.2.6.8 and 6.1.1.4) ; N N 0.006 0.003 ; International Tables for Crystallography (1992, Vol. C, Tables 4.2.6.8 and 6.1.1.4) ; Pt Pt -1.703 8.390 ; International Tables for Crystallography (1992, 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 _geom_angle_publ_flag Cl1 Pt1 Cl2 89.50(11) yes Cl1 Pt1 N1 95.1(2) yes Cl1 Pt1 N2 174.7(2) yes Cl2 Pt1 N1 175.1(2) yes Cl2 Pt1 N2 95.6(2) yes N1 Pt1 N2 79.9(3) yes Pt1 N1 C1 125.3(7) ? Pt1 N1 C5 115.9(6) ? C1 N1 C5 118.8(8) ? PT1 N2 C6 116.2(7) ? PT1 N2 C10 126.4(7) ? C6 N2 C10 117.2(9) ? N1 C1 C2 121.1(9) ? N1 C1 H1 119.4 ? C2 C1 H1 119.4 ? C1 C2 C3 121.3(10) ? C1 C2 H2 119.3 ? C3 C2 H2 119.3 ? C2 C3 C4 116.9(9) ? C2 C3 C11 122.2(9) ? C4 C3 C11 120.9(9) ? C3 C4 C5 119.7(9) ? C3 C4 H4 120.2 ? C5 C4 H4 120.2 ? N1 C5 C4 122.2(9) ? N1 C5 C6 113.2(8) ? C4 C5 C6 124.6(9) ? N2 C6 C5 114.5(9) ? N2 C6 C7 122.1(9) ? C5 C6 C7 123.4(9) ? C6 C7 C8 119.7(10) ? C6 C7 H7 120.1 ? C8 C7 H7 120.1 ? C7 C8 C9 118.7(10) ? C7 C8 C16 120.3(10) ? C9 C8 C16 120.9(10) ? C8 C9 C10 119.5(10) ? C8 C9 H9 120.2 ? C10 C9 H9 120.3 ? N2 C10 C9 122.6(9) ? N2 C10 H10 118.7 ? C9 C10 H10 118.7 ? C3 C11 C12 111.9(8) ? C3 C11 H11A 109.2 ? C3 C11 H11B 109.2 ? C12 C11 H11A 109.2 ? C12 C11 H11B 109.2 ? H11A C11 H11B 107.9 ? C11 C12 C13 112.0(9) ? C11 C12 H12A 109.2 ? C11 C12 H12B 109.2 ? C13 C12 H12A 109.2 ? C13 C12 H12B 109.2 ? H12A C12 H12B 107.9 ? C12 C13 C14 111.5(11) ? C12 C13 H13A 109.3 ? C12 C13 H13B 109.3 ? C14 C13 H13A 109.3 ? C14 C13 H13B 109.3 ? H13A C13 H13B 108.0 ? C13 C14 C15 112.6(12) ? C13 C14 H14A 109.1 ? C13 C14 H14B 109.1 ? C15 C14 H14A 109.1 ? C15 C14 H14B 109.1 ? H14A C14 H14B 107.8 ? C14 C15 H15A 109.5 ? C14 C15 H15B 109.5 ? C14 C15 H15C 109.5 ? H15A C15 H15B 109.5 ? H15A C15 H15C 109.5 ? H15B C15 H15C 109.5 ? C8 C16 C17 110.3(9) ? C8 C16 H16A 109.6 ? C8 C16 H16B 109.6 ? C17 C16 H16A 109.6 ? C17 C16 H16B 109.6 ? H16A C16 H16B 108.1 ? C16 C17 C18 112.4(9) ? C16 C17 H17A 109.1 ? C16 C17 H17B 109.1 ? C18 C17 H17A 109.1 ? C18 C17 H17B 109.1 ? H17A C17 H17B 107.9 ? C17 C18 C19 113.5(9) ? C17 C18 H18A 108.9 ? C17 C18 H18B 108.9 ? C19 C18 H18A 108.9 ? C19 C18 H18B 108.9 ? H18A C18 H18B 107.7 ? C18 C19 C20 111.8(10) ? C18 C19 H19A 109.3 ? C18 C19 H19B 109.3 ? C20 C19 H19A 109.3 ? C20 C19 H19B 109.3 ? H19A C19 H19B 107.9 ? C19 C20 H20A 109.5 ? C19 C20 H20B 109.5 ? C19 C20 H20C 109.5 ? H20A C20 H20B 109.5 ? H20A C20 H20C 109.5 ? H20B C20 H20C 109.5 ? loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_publ_flag Pt1 Cl1 2.294(3) yes Pt1 Cl2 2.295(2) yes Pt1 N1 2.026(8) yes Pt1 N2 2.007(9) yes N1 C1 1.336(14) ? N1 C5 1.362(13) ? N2 C6 1.350(13) ? N2 C10 1.348(13) ? C1 C2 1.387(15) ? C1 H1 0.950 ? C2 C3 1.375(15) ? C2 H2 0.950 ? C3 C4 1.409(15) ? C3 C11 1.490(14) ? C4 C5 1.370(14) ? C4 H4 0.950 ? C5 C6 1.491(14) ? C6 C7 1.388(15) ? C7 C8 1.372(15) ? C7 H7 0.950 ? C8 C9 1.358(15) ? C8 C16 1.529(16) ? C9 C10 1.389(16) ? C9 H9 0.950 ? C10 H10 0.950 ? C11 C12 1.546(15) ? C11 H11A 0.990 ? C11 H11B 0.990 ? C12 C13 1.513(17) ? C12 H12A 0.990 ? C12 H12B 0.990 ? C13 C14 1.53(2) ? C13 H13A 0.990 ? C13 H13B 0.990 ? C14 C15 1.51(2) ? C14 H14A 0.990 ? C14 H14B 0.990 ? C15 H15A 0.980 ? C15 H15B 0.980 ? C15 H15C 0.980 ? C16 C17 1.532(16) ? C16 H16A 0.990 ? C16 H16B 0.990 ? C17 C18 1.521(17) ? C17 H17A 0.990 ? C17 H17B 0.990 ? C18 C19 1.524(16) ? C18 H18A 0.990 ? C18 H18B 0.990 ? C19 C20 1.54(2) ? C19 H19A 0.990 ? C19 H19B 0.990 ? C20 H20A 0.980 ? C20 H20B 0.980 ? C20 H20C 0.980 ?