#------------------------------------------------------------------------------ #$Date: 2016-02-16 16:55:33 +0000 (Tue, 16 Feb 2016) $ #$Revision: 176466 $ #$URL: svn://www.crystallography.net/cod/cif/8/00/00/8000067.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_8000067 loop_ _publ_author_name 'Masako Kato' 'Shinobu Kishi' 'Yuki Wakamatsu' 'Yoshiko Sugi' 'Yoko Osamura' 'Tamami Koshiyama' 'Miki Hasegawa' _publ_section_title ; Outstanding Vapochromism and pH-dependent Coloration of Dicyano(4,4'- dicarboxy-2,2'-bipyridine)platinum(II) with a Three-dimensional Network Structure ; _journal_issue 10 _journal_name_full 'Chemistry Letters' _journal_page_first 1368 _journal_paper_doi 10.1246/cl.2005.1368 _journal_volume 34 _journal_year 2005 _chemical_formula_moiety 'C14 H16 N4 O8 Pt ' _chemical_formula_sum 'C14 H16 N4 O8 Pt' _chemical_formula_weight 563.39 _symmetry_cell_setting orthorhombic _symmetry_Int_Tables_number 63 _symmetry_space_group_name_Hall '-C 2c 2' _symmetry_space_group_name_H-M 'C m c m' _cell_angle_alpha 90 _cell_angle_beta 90 _cell_angle_gamma 90 _cell_formula_units_Z 4 _cell_length_a 17.2496(7) _cell_length_b 18.5822(7) _cell_length_c 6.4537(2) _cell_measurement_reflns_used 3196 _cell_measurement_temperature 173.1 _cell_measurement_theta_max 27.5 _cell_measurement_theta_min 3.2 _cell_volume 2068.64(13) _computing_cell_refinement CrystalClear _computing_data_collection CrystalClear _computing_data_reduction CrystalStructure _computing_publication_material 'CrystalStructure 3.6.0' _computing_structure_refinement SHELXL _computing_structure_solution SIR92 _diffrn_detector_area_resol_mean 7.31 _diffrn_measured_fraction_theta_full 0.9957 _diffrn_measured_fraction_theta_max 0.9957 _diffrn_measurement_device_type 'Rigaku Mercury' _diffrn_measurement_method \w _diffrn_radiation_type 'Mo K\a' _diffrn_radiation_wavelength 0.7107 _diffrn_reflns_av_R_equivalents 0.031 _diffrn_reflns_limit_h_max 22 _diffrn_reflns_limit_h_min 0 _diffrn_reflns_limit_k_max 24 _diffrn_reflns_limit_k_min 0 _diffrn_reflns_limit_l_max 8 _diffrn_reflns_limit_l_min 0 _diffrn_reflns_number 7948 _diffrn_reflns_theta_full 27.46 _diffrn_reflns_theta_max 27.46 _exptl_absorpt_coefficient_mu 6.800 _exptl_absorpt_correction_T_max 0.688 _exptl_absorpt_correction_T_min 0.371 _exptl_absorpt_correction_type numerical _exptl_absorpt_process_details ; Higashi, T. (1999). Program for Absorption Correction. Rigaku Corporation, Tokyo, Japan. ; _exptl_crystal_colour red _exptl_crystal_density_diffrn 1.809 _exptl_crystal_density_method 'not measured' _exptl_crystal_description needle _exptl_crystal_F_000 1080.00 _exptl_crystal_size_max 0.32 _exptl_crystal_size_mid 0.06 _exptl_crystal_size_min 0.06 _refine_diff_density_max 1.93 _refine_diff_density_min -2.25 _refine_ls_goodness_of_fit_ref 1.258 _refine_ls_hydrogen_treatment constr _refine_ls_number_parameters 72 _refine_ls_number_reflns 1337 _refine_ls_R_factor_gt 0.0300 _refine_ls_shift/su_max 0.0010 _refine_ls_structure_factor_coef Fsqd _refine_ls_weighting_details 'w = 1/[\s^2^(Fo^2^)+(0.0350P)^2^+16.4306P] where P=(Fo^2^+2Fc^2^)/3' _refine_ls_weighting_scheme calc _refine_ls_wR_factor_ref 0.1000 _reflns_number_gt 1161 _reflns_number_total 1337 _reflns_threshold_expression F^2^>2.0\s(F^2^) _cod_original_formula_sum 'C14 H16 N4 O8 Pt ' _cod_database_code 8000067 loop_ _symmetry_equiv_pos_site_id _symmetry_equiv_pos_as_xyz 1 +X,+Y,+Z 2 -X,+Y,+Z 3 +X,-Y,1/2+Z 4 -X,-Y,1/2+Z 5 -X,-Y,-Z 6 +X,-Y,-Z 7 -X,+Y,1/2-Z 8 +X,+Y,1/2-Z 9 1/2+X,1/2+Y,+Z 10 1/2-X,1/2+Y,+Z 11 1/2+X,1/2-Y,1/2+Z 12 1/2-X,1/2-Y,1/2+Z 13 1/2-X,1/2-Y,-Z 14 1/2+X,1/2-Y,-Z 15 1/2-X,1/2+Y,1/2-Z 16 1/2+X,1/2+Y,1/2-Z 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_symmetry_multiplicity _atom_site_calc_flag _atom_site_refinement_flags Pt1 Pt 0.0000 0.00649(2) 0.2500 0.0175(2) Uani 1.00 4 d S O1 O 0.2891(5) -0.2565(4) 0.2500 0.044(2) Uani 1.00 2 d S O2 O 0.1844(5) -0.3259(4) 0.2500 0.065(3) Uani 1.00 2 d S O3 O 0.3095 0.0222 0.2500 0.152 Uiso 1.00 2 d R O4 O 0.0000 0.3754 0.7500 0.152 Uiso 1.00 4 d R O5 O 0.0000 0.3003 0.2500 0.152 Uiso 1.00 4 d R N1 N 0.0770(4) -0.0778(3) 0.2500 0.017(2) Uani 1.00 2 d S N2 N 0.1221(6) 0.1282(4) 0.2500 0.034(2) Uani 1.00 2 d S C1 C 0.1538(5) -0.0729(5) 0.2500 0.024(2) Uani 1.00 2 d S C2 C 0.2005(6) -0.1327(5) 0.2500 0.027(2) Uani 1.00 2 d S C3 C 0.1676(6) -0.1995(5) 0.2500 0.027(2) Uani 1.00 2 d S C4 C 0.0875(6) -0.2057(5) 0.2500 0.026(2) Uani 1.00 2 d S C5 C 0.0437(5) -0.1437(4) 0.2500 0.022(2) Uani 1.00 2 d S C6 C 0.2140(6) -0.2683(5) 0.2500 0.031(2) Uani 1.00 2 d S C7 C 0.0769(5) 0.0829(4) 0.2500 0.021(2) Uani 1.00 2 d S H1 H 0.1767 -0.0276 0.2500 0.028 Uiso 1.00 2 c R H2 H 0.2542 -0.1278 0.2500 0.032 Uiso 1.00 2 c R H3 H 0.3122 -0.2951 0.2500 0.053 Uiso 1.00 2 c R H4 H 0.0639 -0.2507 0.2500 0.032 Uiso 1.00 2 c R 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 0.0164(2) 0.0147(2) 0.0214(3) 0.0000 0.0000 0.0000 O1 0.039(5) 0.030(4) 0.064(6) 0.015(3) 0.0000 0.0000 O2 0.045(5) 0.025(4) 0.123(9) 0.010(4) 0.0000 0.0000 N1 0.015(4) 0.015(3) 0.020(4) 0.001(3) 0.0000 0.0000 N2 0.038(5) 0.026(4) 0.038(5) -0.013(4) 0.0000 0.0000 C1 0.023(5) 0.019(4) 0.029(5) 0.001(3) 0.0000 0.0000 C2 0.018(5) 0.030(5) 0.032(6) 0.005(4) 0.0000 0.0000 C3 0.028(5) 0.025(4) 0.029(5) 0.009(4) 0.0000 0.0000 C4 0.028(5) 0.018(4) 0.033(6) 0.003(4) 0.0000 0.0000 C5 0.021(5) 0.016(4) 0.028(5) 0.001(3) 0.0000 0.0000 C6 0.028(6) 0.025(5) 0.039(6) 0.009(4) 0.0000 0.0000 C7 0.022(5) 0.021(4) 0.021(5) 0.001(3) 0.0000 0.0000 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) ; N N 0.006 0.003 ; International Tables for Crystallography (1992, Vol. C, Tables 4.2.6.8 and 6.1.1.4) ; O O 0.011 0.006 ; 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_site_symmetry_1 _geom_angle_site_symmetry_2 _geom_angle_site_symmetry_3 N1 Pt1 N1 80.6(3) 55502 . . Pt1 N1 C1 126.4(5) . . . Pt1 N1 C5 114.5(6) . . . C7 Pt1 N1 96.6(3) . . . C7 Pt1 N1 177.2(3) 55502 . . Pt1 N1 C1 126.4(5) . 55502 55502 Pt1 N1 C5 114.5(6) . 55502 55502 C7 Pt1 N1 177.2(3) . . 55502 C7 Pt1 N1 96.6(3) 55502 . 55502 Pt1 C7 N2 179.7(7) . . . C7 Pt1 C7 86.1(4) 55502 . . Pt1 C7 N2 179.7(5) . 55502 55502 O1 C6 O2 125(1) . . . O1 C6 C3 112.5(8) . . . H3 O1 C6 109.4578 . . . O2 C6 C3 122(1) . . . C5 N1 C1 119.0(7) . . . N1 C1 H1 118.9608 . . . N1 C1 C2 122.1(8) . . . N1 C5 C5 115.2(7) . . 55502 N1 C5 C4 121.6(8) . . . H1 C1 C2 118.9582 . . . C1 C2 C3 119.4(9) . . . C1 C2 H2 120.2797 . . . C2 C3 C6 123.4(9) . . . H2 C2 C3 120.2721 . . . C2 C3 C4 119.4(9) . . . C3 C4 C5 118.5(8) . . . C6 C3 C4 117.3(8) . . . C3 C4 H4 120.7502 . . . C4 C5 C5 123.3(8) . . 55502 H4 C4 C5 120.7505 . . . C5 C5 N1 115.2(7) . 55502 55502 C5 C5 C4 123.3(8) . 55502 55502 loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 Pt1 N1 2.053(7) . Pt1 N1 2.053(7) 55502 Pt1 C7 1.944(9) . Pt1 C7 1.944(9) 55502 O1 C6 1.31(1) . O1 H3 0.8200 . O2 C6 1.19(1) . N1 C1 1.33(1) . N1 C5 1.35(1) . N2 C7 1.15(1) . C1 C2 1.37(1) . C1 H1 0.9301 . C2 C3 1.37(1) . C2 H2 0.9300 . C3 C4 1.39(1) . C3 C6 1.51(1) . C4 C5 1.38(1) . C4 H4 0.9300 . C5 C5 1.51(1) 55502 loop_ _geom_contact_atom_site_label_1 _geom_contact_atom_site_label_2 _geom_contact_distance _geom_contact_site_symmetry_2 Pt1 Pt1 3.23585(4) 55403 Pt1 Pt1 3.23585(4) 55503 Pt1 N2 3.090(9) . Pt1 N2 3.090(9) 55502 Pt1 C1 3.036(9) . Pt1 C1 3.036(9) 55502 Pt1 C5 2.890(8) . Pt1 C5 2.890(8) 55502 Pt1 H1 3.1126 . Pt1 H1 3.1126 55502 O1 O1 3.506(5) 54412 O1 O1 3.506(5) 54512 O1 O2 2.22(1) . O1 N2 2.63(1) 54510 O1 C2 2.76(1) . O1 C3 2.35(1) . O1 C3 3.411(4) 54412 O1 C3 3.411(4) 54512 O1 C6 3.260(2) 54412 O1 C6 3.260(2) 54512 O1 H2 2.4674 . O2 O3 2.8254 54510 O2 O4 3.3109 55403 O2 N2 3.45(1) 54510 O2 C2 3.60(1) . O2 C3 2.37(1) . O2 C4 2.79(1) . O2 H2 3.5041 54412 O2 H2 3.5041 54512 O2 H2 3.5041 54513 O2 H2 3.5041 54613 O2 H3 2.2778 . O2 H4 2.5038 . O3 O2 2.8254 55510 O3 O3 3.3307 55403 O3 O3 3.3307 55503 O3 O3 3.3307 55506 O3 O3 3.3307 55606 O3 C1 3.2152 . O3 C2 3.4381 . O3 H1 2.4711 . O3 H2 2.9456 . O4 O2 3.3109 55503 O4 O2 3.3109 55504 O4 O5 3.5157 . O4 O5 3.5157 55601 O4 O5 3.5157 55502 O4 O5 3.5157 55507 O4 O5 3.5157 55508 O4 C4 3.4957 55503 O4 C4 3.4957 55504 O4 H4 2.5658 55503 O4 H4 2.5658 55504 O5 O4 3.5157 55401 O5 O4 3.5157 . O5 O4 3.5157 55402 O5 O4 3.5157 55502 O5 O4 3.5157 55507 O5 O4 3.5157 55607 O5 O4 3.5157 55508 O5 O4 3.5157 55608 O5 H4 3.5322 55403 O5 H4 3.5322 55503 O5 H4 3.5322 55404 O5 H4 3.5322 55504 N1 N1 2.66(1) 55502 N1 N2 3.449(4) 55403 N1 N2 3.449(4) 55503 N1 C2 2.36(1) . N1 C3 2.75(1) . N1 C4 2.38(1) . N1 C5 2.41(1) 55502 N1 C7 2.99(1) . N1 C7 3.2283(3) 55403 N1 C7 3.2283(3) 55503 N1 H1 1.9558 . N1 H2 3.1946 . N1 H4 3.2217 . N2 O1 2.63(1) 55510 N2 O2 3.45(1) 55510 N2 N1 3.449(4) 55403 N2 N1 3.449(4) 55503 N2 C1 3.430(4) 55403 N2 C1 3.430(4) 55503 N2 C2 3.500(5) 55403 N2 C2 3.500(5) 55503 N2 C3 3.576(5) 55403 N2 C3 3.576(5) 55503 N2 C4 3.584(5) 55403 N2 C4 3.584(5) 55503 N2 C5 3.511(5) 55403 N2 C5 3.511(5) 55503 N2 C6 3.42(1) 55510 N2 C7 3.53(1) 55502 N2 H1 3.0446 . N2 H3 1.8213 55510 C1 N2 3.430(4) 55403 C1 N2 3.430(4) 55503 C1 C3 2.36(1) . C1 C4 2.72(1) . C1 C5 2.31(1) . C1 C7 3.18(1) . C1 C7 3.494(5) 55403 C1 C7 3.494(5) 55503 C1 H2 2.0090 . C2 N2 3.500(5) 55403 C2 N2 3.500(5) 55503 C2 C4 2.38(1) . C2 C5 2.71(1) . C2 C6 2.53(1) . C2 H1 1.9963 . C2 H3 3.5800 . C2 H3 3.5013 54412 C2 H3 3.5013 54512 C2 H4 3.2191 . C3 O1 3.411(4) 54412 C3 O1 3.411(4) 54512 C3 N2 3.576(5) 55403 C3 N2 3.576(5) 55503 C3 C5 2.38(1) . C3 H1 3.1985 . C3 H2 2.0021 . C3 H3 3.0623 . C3 H3 3.2472 54412 C3 H3 3.2472 54512 C3 H4 2.0260 . C4 O4 3.4957 55403 C4 N2 3.584(5) 55403 C4 N2 3.584(5) 55503 C4 C4 3.02(1) 55502 C4 C5 2.54(1) 55502 C4 C6 2.47(1) . C4 H2 3.2193 . C4 H4 2.7421 55502 C5 N1 2.41(1) 55502 C5 N2 3.511(5) 55403 C5 N2 3.511(5) 55503 C5 C4 2.54(1) 55502 C5 C7 3.467(4) 55403 C5 C7 3.467(4) 55503 C5 H1 3.1490 . C5 H4 2.0196 . C5 H4 2.7199 55502 C6 O1 3.260(2) 54412 C6 O1 3.260(2) 54512 C6 N2 3.42(1) 54510 C6 C6 3.524(6) 54412 C6 C6 3.524(6) 54512 C6 H2 2.7020 . C6 H3 1.7658 . C6 H3 3.4649 54412 C6 H3 3.4649 54512 C6 H4 2.6097 . C7 N1 3.2283(3) 55403 C7 N1 3.2283(3) 55503 C7 N2 3.53(1) 55502 C7 C1 3.494(5) 55403 C7 C1 3.494(5) 55503 C7 C5 3.467(4) 55403 C7 C5 3.467(4) 55503 C7 C7 2.65(1) 55502 C7 H1 2.6789 . C7 H3 2.9656 55510 H2 O2 3.5041 54412 H2 O2 3.5041 54512 H3 N2 1.8213 54510 H3 C2 3.5013 54412 H3 C2 3.5013 54512 H3 C3 3.2472 54412 H3 C3 3.2472 54512 H3 C6 3.4649 54412 H3 C6 3.4649 54512 H3 C7 2.9656 54510 H4 O4 2.5658 55403 H4 O5 3.5322 55403 H4 O5 3.5322 55503 H4 C4 2.7421 55502 H4 C5 2.7199 55502 loop_ _geom_hbond_atom_site_label_D _geom_hbond_atom_site_label_H _geom_hbond_atom_site_label_A _geom_hbond_site_symmetry_A _geom_hbond_distance_DH _geom_hbond_distance_HA _geom_hbond_distance_DA _geom_hbond_angle_DHA _geom_hbond_publ_flag O1 H3 N2 10_545 0.82 1.82 2.63(1) 170 yes