#------------------------------------------------------------------------------ #$Date: 2014-07-12 07:06:18 +0300 (Sat, 12 Jul 2014) $ #$Revision: 120112 $ #$URL: file:///home/coder/svn-repositories/cod/cif/7/01/56/7015632.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_7015632 loop_ _publ_author_name 'Francisco, Carla' 'Gama, Sofia' 'Mendes, Filipa' 'Marques, Fernanda' 'Cordeiro Dos Santos, Isabel' 'Paulo, Ant\'onio' 'Santos, Isabel' 'Coimbra, Joana' 'Gabano, Elisabetta' 'Ravera, Mauro' _publ_section_title ; Pt(ii) complexes with bidentate and tridentate pyrazolyl-containing chelators: synthesis, structural characterization and biological studies. ; _journal_issue 21 _journal_name_full 'Dalton transactions (Cambridge, England : 2003)' _journal_page_first 5781 _journal_page_last 5792 _journal_volume 40 _journal_year 2011 _chemical_formula_sum 'C5 H9 Cl2 N3 Pt' _chemical_formula_weight 377.14 _chemical_name_systematic ; ? ; _space_group_IT_number 29 _symmetry_cell_setting orthorhombic _symmetry_space_group_name_Hall 'P 2c -2ac' _symmetry_space_group_name_H-M 'P c a 21' _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 90.00 _cell_angle_gamma 90.00 _cell_formula_units_Z 4 _cell_length_a 16.7647(8) _cell_length_b 6.2596(3) _cell_length_c 8.2202(4) _cell_measurement_reflns_used 2635 _cell_measurement_temperature 150(2) _cell_measurement_theta_max 28.22 _cell_measurement_theta_min 2.43 _cell_volume 862.63(7) _computing_cell_refinement 'Bruker SAINT, (Bruker, 2004)' _computing_data_collection 'Bruker SMART, (Bruker, 2004)' _computing_data_reduction 'Bruker SAINT, (Bruker, 2004)' _computing_molecular_graphics ORTEP3(Farrugia,1997) _computing_publication_material 'WinGX (Farrugia, 1999)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_structure_solution 'SIR97 (Altomare, 1999)' _diffrn_ambient_temperature 150(2) _diffrn_measured_fraction_theta_full 0.999 _diffrn_measured_fraction_theta_max 0.999 _diffrn_measurement_device_type 'Bruker-APEXII CCD' _diffrn_measurement_method '\f and \w' _diffrn_radiation_monochromator graphite _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_type MoK\a _diffrn_radiation_wavelength 0.71073 _diffrn_reflns_av_R_equivalents 0.0383 _diffrn_reflns_av_sigmaI/netI 0.0463 _diffrn_reflns_limit_h_max 18 _diffrn_reflns_limit_h_min -20 _diffrn_reflns_limit_k_max 7 _diffrn_reflns_limit_k_min -7 _diffrn_reflns_limit_l_max 7 _diffrn_reflns_limit_l_min -10 _diffrn_reflns_number 4918 _diffrn_reflns_theta_full 25.66 _diffrn_reflns_theta_max 25.66 _diffrn_reflns_theta_min 3.25 _exptl_absorpt_coefficient_mu 16.822 _exptl_absorpt_correction_T_max 0.7296 _exptl_absorpt_correction_T_min 0.1738 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_process_details '(SADABS; Sheldrick, 2004)' _exptl_crystal_colour colourless _exptl_crystal_density_diffrn 2.904 _exptl_crystal_density_method 'not measured' _exptl_crystal_description plate _exptl_crystal_F_000 688 _exptl_crystal_size_max 0.16 _exptl_crystal_size_mid 0.12 _exptl_crystal_size_min 0.02 _refine_diff_density_max 0.853 _refine_diff_density_min -0.739 _refine_diff_density_rms 0.129 _refine_ls_abs_structure_details 'Flack H D (1983), Acta Cryst. A39, 876-881' _refine_ls_abs_structure_Flack -0.001(10) _refine_ls_extinction_method none _refine_ls_goodness_of_fit_ref 0.980 _refine_ls_hydrogen_treatment constr _refine_ls_matrix_type full _refine_ls_number_parameters 100 _refine_ls_number_reflns 1551 _refine_ls_number_restraints 1 _refine_ls_restrained_S_all 0.980 _refine_ls_R_factor_all 0.0215 _refine_ls_R_factor_gt 0.0195 _refine_ls_shift/su_max 0.000 _refine_ls_shift/su_mean 0.000 _refine_ls_structure_factor_coef Fsqd _refine_ls_weighting_details 'calc w=1/[\s^2^(Fo^2^)+(0.0000P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3' _refine_ls_weighting_scheme calc _refine_ls_wR_factor_gt 0.0417 _refine_ls_wR_factor_ref 0.0424 _reflns_number_gt 1463 _reflns_number_total 1551 _reflns_threshold_expression >2sigma(I) _[local]_cod_data_source_file c0dt01785j.txt _[local]_cod_data_source_block eg261 _[local]_cod_cif_authors_sg_H-M 'Pca2(1) ' _cod_depositor_comments ; The following automatic conversions were performed: '_symmetry_cell_setting' value 'Orthorhombic' changed to 'orthorhombic' according to '/home/saulius/struct/CIF-dictionaries/cif_core.dic' dictionary named 'cif_core.dic' version 2.4.1 from 2010-06-29. Automatic conversion script Id: cif_fix_enum 1555 2011-01-17 13:19:09Z saulius ; _cod_database_code 7015632 loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, -y, z+1/2' 'x+1/2, -y, z' '-x+1/2, y, 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_occupancy _atom_site_symmetry_multiplicity _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group Pt1 Pt 0.508086(10) 0.20644(3) 0.78260(9) 0.01293(8) Uani 1 1 d . . . Cl1 Cl 0.55884(10) 0.5219(2) 0.88576(19) 0.0209(3) Uani 1 1 d . . . Cl2 Cl 0.63360(10) 0.0946(3) 0.71122(19) 0.0245(4) Uani 1 1 d . . . N1 N 0.3964(3) 0.3031(7) 0.8406(6) 0.0166(12) Uani 1 1 d . . . N2 N 0.3311(3) 0.2350(8) 0.7608(8) 0.0189(13) Uani 1 1 d . . . N3 N 0.4682(3) -0.0762(8) 0.6893(6) 0.0178(12) Uani 1 1 d . . . H3A H 0.4853 -0.0843 0.5830 0.021 Uiso 1 1 calc R . . H3B H 0.4931 -0.1846 0.7452 0.021 Uiso 1 1 calc R . . C1 C 0.3706(4) 0.4427(10) 0.9507(7) 0.0204(15) Uani 1 1 d . . . H1 H 0.4036 0.5144 1.0271 0.025 Uiso 1 1 calc R . . C2 C 0.2903(4) 0.4683(9) 0.9384(7) 0.0201(15) Uani 1 1 d . . . H2 H 0.2578 0.5600 1.0024 0.024 Uiso 1 1 calc R . . C3 C 0.2653(4) 0.3360(10) 0.8155(7) 0.0216(18) Uani 1 1 d . . . H3 H 0.2123 0.3190 0.7768 0.026 Uiso 1 1 calc R . . C4 C 0.3358(4) 0.0736(10) 0.6306(7) 0.0195(15) Uani 1 1 d . . . H4A H 0.3631 0.1351 0.5347 0.023 Uiso 1 1 calc R . . H4B H 0.2814 0.0306 0.5974 0.023 Uiso 1 1 calc R . . C5 C 0.3815(4) -0.1206(10) 0.6908(7) 0.0217(15) Uani 1 1 d . . . H5A H 0.3643 -0.1563 0.8028 0.026 Uiso 1 1 calc R . . H5B H 0.3699 -0.2447 0.6200 0.026 Uiso 1 1 calc 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_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 Pt1 0.01207(12) 0.01177(13) 0.01495(11) 0.0018(2) -0.0008(3) 0.00071(7) Cl1 0.0210(9) 0.0152(9) 0.0264(8) -0.0007(6) -0.0041(7) -0.0025(6) Cl2 0.0145(9) 0.0241(10) 0.0350(8) 0.0060(7) 0.0051(7) 0.0052(6) N1 0.016(3) 0.014(3) 0.021(3) 0.000(2) -0.002(2) -0.006(2) N2 0.015(3) 0.015(3) 0.027(4) 0.002(3) 0.004(3) -0.0033(17) N3 0.026(3) 0.014(3) 0.013(2) -0.004(2) 0.004(2) 0.000(2) C1 0.020(4) 0.022(4) 0.020(3) -0.001(3) 0.003(3) 0.000(3) C2 0.022(4) 0.018(4) 0.020(3) 0.001(3) 0.007(3) 0.002(3) C3 0.017(3) 0.018(4) 0.030(5) 0.005(3) 0.002(3) 0.000(2) C4 0.015(4) 0.027(4) 0.016(3) -0.004(3) 0.001(3) -0.010(3) C5 0.035(4) 0.016(4) 0.014(3) -0.005(3) 0.007(3) -0.009(3) loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source 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' N N 0.0061 0.0033 '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' 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 _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag N1 Pt1 N3 92.6(2) . . ? N1 Pt1 Cl2 178.72(14) . . ? N3 Pt1 Cl2 86.54(17) . . ? N1 Pt1 Cl1 89.92(14) . . ? N3 Pt1 Cl1 177.50(16) . . ? Cl2 Pt1 Cl1 90.96(6) . . ? C1 N1 N2 106.0(6) . . ? C1 N1 Pt1 131.1(4) . . ? N2 N1 Pt1 122.9(4) . . ? N1 N2 C3 110.7(6) . . ? N1 N2 C4 121.8(5) . . ? C3 N2 C4 127.5(6) . . ? C5 N3 Pt1 118.8(4) . . ? N1 C1 C2 110.4(6) . . ? C1 C2 C3 106.6(6) . . ? N2 C3 C2 106.2(6) . . ? N2 C4 C5 109.8(5) . . ? N3 C5 C4 110.0(5) . . ? loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag Pt1 N1 2.025(5) . ? Pt1 N3 2.041(5) . ? Pt1 Cl2 2.2938(16) . ? Pt1 Cl1 2.3113(16) . ? N1 C1 1.330(7) . ? N1 N2 1.347(7) . ? N2 C3 1.348(8) . ? N2 C4 1.473(8) . ? N3 C5 1.480(9) . ? C1 C2 1.359(9) . ? C2 C3 1.371(8) . ? C4 C5 1.520(9) . ? _journal_paper_doi 10.1039/c0dt01785j