#------------------------------------------------------------------------------ #$Date: 2014-10-21 03:08:49 +0300 (Tue, 21 Oct 2014) $ #$Revision: 125578 $ #$URL: file:///home/coder/svn-repositories/cod/cif/7/03/28/7032866.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_7032866 loop_ _publ_author_name 'Lippard, Stephen J.' 'Johnstone, Timothy' 'Wilson, Justin J.' 'Alexander, Sarah M.' _publ_section_title ; Oxidative Halogenation of Cisplatin and Carboplatin: Synthesis, Spectroscopy, and Crystal and Molecular Structures of Pt(IV) Prodrugs ; _journal_name_full 'Dalton Trans.' _journal_paper_doi 10.1039/C4DT02627F _journal_year 2014 _chemical_formula_moiety 'Cl3 H9 N3 Pt, C3 H7 N O, Cl' _chemical_formula_sum 'C3 H16 Cl4 N4 O Pt' _chemical_formula_weight 461.09 _chemical_name_systematic ; 'fac-triamminetrichloroplatinum(IV) chloride mono(dimethylformamide)' ; _space_group_IT_number 14 _symmetry_cell_setting monoclinic _symmetry_space_group_name_Hall '-P 2yn' _symmetry_space_group_name_H-M '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 96.665(3) _cell_angle_gamma 90.00 _cell_formula_units_Z 4 _cell_length_a 6.3996(14) _cell_length_b 10.711(2) _cell_length_c 18.334(4) _cell_measurement_reflns_used 419 _cell_measurement_temperature 100(2) _cell_measurement_theta_max 28.54 _cell_measurement_theta_min 2.21 _cell_volume 1248.2(5) _computing_cell_refinement 'Bruker SMART' _computing_data_collection 'Bruker SMART' _computing_data_reduction 'Bruker SAINT' _computing_molecular_graphics 'Bruker SHELXTL' _computing_publication_material 'Bruker SHELXTL' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _diffrn_ambient_temperature 100(2) _diffrn_measured_fraction_theta_full 0.999 _diffrn_measured_fraction_theta_max 0.999 _diffrn_measurement_device_type 'CCD area detector' _diffrn_measurement_method 'phi and omega scans' _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 0.0696 _diffrn_reflns_av_sigmaI/netI 0.0421 _diffrn_reflns_limit_h_max 8 _diffrn_reflns_limit_h_min -8 _diffrn_reflns_limit_k_max 14 _diffrn_reflns_limit_k_min -14 _diffrn_reflns_limit_l_max 24 _diffrn_reflns_limit_l_min -24 _diffrn_reflns_number 23701 _diffrn_reflns_theta_full 28.54 _diffrn_reflns_theta_max 28.54 _diffrn_reflns_theta_min 2.21 _exptl_absorpt_coefficient_mu 12.070 _exptl_absorpt_correction_T_max 0.7943 _exptl_absorpt_correction_T_min 0.4097 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_process_details 'Blessing, 1995' _exptl_crystal_colour yellow _exptl_crystal_density_diffrn 2.453 _exptl_crystal_density_method 'not measured' _exptl_crystal_description prism _exptl_crystal_F_000 864 _exptl_crystal_size_max 0.09 _exptl_crystal_size_mid 0.05 _exptl_crystal_size_min 0.02 _refine_diff_density_max 2.064 _refine_diff_density_min -1.050 _refine_diff_density_rms 0.221 _refine_ls_extinction_method none _refine_ls_goodness_of_fit_ref 1.073 _refine_ls_hydrogen_treatment constr _refine_ls_matrix_type full _refine_ls_number_parameters 123 _refine_ls_number_reflns 3185 _refine_ls_number_restraints 0 _refine_ls_restrained_S_all 1.073 _refine_ls_R_factor_all 0.0456 _refine_ls_R_factor_gt 0.0325 _refine_ls_shift/su_max 0.001 _refine_ls_shift/su_mean 0.000 _refine_ls_structure_factor_coef Fsqd _refine_ls_weighting_details 'calc w=1/[\s^2^(Fo^2^)+(0.0295P)^2^+3.6382P] where P=(Fo^2^+2Fc^2^)/3' _refine_ls_weighting_scheme calc _refine_ls_wR_factor_gt 0.0674 _refine_ls_wR_factor_ref 0.0728 _reflns_number_gt 2632 _reflns_number_total 3185 _reflns_threshold_expression >2sigma(I) _iucr_refine_instructions_details ; TITL tj3 in P2(1)/n CELL 0.71073 6.3996 10.7114 18.3341 90.000 96.665 90.000 ZERR 4.00 0.0014 0.0023 0.0040 0.000 0.003 0.000 LATT 1 SYMM 0.5-X, 0.5+Y, 0.5-Z SFAC C H N O CL PT UNIT 12 64 16 4 16 4 TEMP -173 L.S. 10 ACTA SIZE 0.09 0.05 0.02 BOND FMAP 2 PLAN 5 WGHT 0.029500 3.638200 FVAR 0.07853 PT1 6 1.194707 0.412786 0.318949 11.00000 0.01464 0.01388 = 0.01501 0.00121 0.00196 -0.00008 CL1 5 0.953793 0.575054 0.312324 11.00000 0.02361 0.02014 = 0.02624 0.00424 0.00394 0.00627 CL2 5 0.933299 0.268975 0.283735 11.00000 0.02114 0.02044 = 0.02187 -0.00174 0.00041 -0.00459 CL3 5 1.260585 0.441040 0.198756 11.00000 0.02770 0.03104 = 0.01917 0.00656 0.00730 0.00171 N1 3 1.408793 0.269338 0.326453 11.00000 0.01654 0.02160 = 0.01731 0.00072 0.00183 0.00537 AFIX 137 H1A 2 1.521177 0.289896 0.359311 11.00000 -1.50000 H1B 2 1.452673 0.255681 0.281664 11.00000 -1.50000 H1C 2 1.347443 0.198842 0.341710 11.00000 -1.50000 AFIX 0 N2 3 1.427338 0.540832 0.351349 11.00000 0.01661 0.02062 = 0.03049 0.00240 0.00271 -0.00652 AFIX 137 H2A 2 1.372071 0.604843 0.375527 11.00000 -1.50000 H2B 2 1.481517 0.571013 0.311120 11.00000 -1.50000 H2C 2 1.531171 0.503193 0.381711 11.00000 -1.50000 AFIX 0 N3 3 1.144223 0.385408 0.426119 11.00000 0.01823 0.02299 = 0.01231 0.00214 0.00135 -0.00035 AFIX 137 H3A 2 1.200238 0.310802 0.442047 11.00000 -1.50000 H3B 2 1.003488 0.385329 0.429522 11.00000 -1.50000 H3C 2 1.206523 0.447934 0.454384 11.00000 -1.50000 AFIX 0 REM ************************Counter-Ion*************************** CL1C 5 0.682888 0.368534 0.479083 11.00000 0.02158 0.02902 = 0.02632 -0.00815 0.00215 -0.00063 REM **************************Solvent***************************** O1S 4 1.271011 0.135023 0.442787 11.00000 0.04006 0.02500 = 0.02244 0.00567 0.00502 -0.00076 N1S 3 1.236183 0.061167 0.556120 11.00000 0.02506 0.01754 = 0.02119 0.00202 -0.00103 0.00219 C3S 1 1.264283 0.048091 0.486343 11.00000 0.02071 0.02024 = 0.02698 -0.00278 0.00414 0.00005 AFIX 41 H3S 2 1.280450 -0.034191 0.468490 11.00000 -1.20000 AFIX 0 C2S 1 1.227583 -0.045150 0.604984 11.00000 0.02950 0.02248 = 0.03495 0.00823 0.00260 0.00221 AFIX 137 H2S1 2 1.236043 -0.122649 0.577069 11.00000 -1.50000 H2S2 2 1.094982 -0.043354 0.626862 11.00000 -1.50000 H2S3 2 1.345929 -0.041108 0.643956 11.00000 -1.50000 AFIX 0 C1S 1 1.210903 0.184618 0.585780 11.00000 0.05287 0.02288 = 0.02818 -0.00650 0.00059 0.00480 AFIX 137 H1S1 2 1.318602 0.240349 0.570072 11.00000 -1.50000 H1S2 2 1.225978 0.180359 0.639529 11.00000 -1.50000 H1S3 2 1.070996 0.216814 0.567841 11.00000 -1.50000 HKLF 4 REM tj3 in P2(1)/n REM R1 = 0.0325 for 2632 Fo > 4sig(Fo) and 0.0456 for all 3185 data REM 123 parameters refined using 0 restraints END WGHT 0.0295 3.6382 REM Highest difference peak 2.064, deepest hole -1.050, 1-sigma level 0.221 Q1 1 1.0810 0.4609 0.3247 11.00000 0.05 2.06 Q2 1 1.3190 0.4578 0.3119 11.00000 0.05 2.02 Q3 1 1.1908 0.4109 0.2745 11.00000 0.05 2.01 Q4 1 1.0780 0.3635 0.3198 11.00000 0.05 1.83 Q5 1 1.3268 0.3601 0.3092 11.00000 0.05 1.80 ; _[local]_cod_data_source_file c4dt02627f2.cif _[local]_cod_data_source_block ESI5 _[local]_cod_cif_authors_sg_H-M P2(1)/n _cod_depositor_comments ; The following automatic conversions were performed: '_symmetry_cell_setting' value 'Monoclinic' changed to 'monoclinic' according to /usr/data/users/saulius/crontab/automatic-downloads/rss-feeds/RSC/lib/dictionaries/cif_core.dic dictionary named 'cif_core.dic' version 2.4.2 from 2011-04-26. Automatic conversion script Id: cif_fix_values 2827 2014-09-09 07:05:25Z andrius ; _cod_original_cell_volume 1248.3(5) _cod_database_code 7032866 loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x+1/2, y+1/2, -z+1/2' '-x, -y, -z' '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_occupancy _atom_site_symmetry_multiplicity _atom_site_calc_flag _atom_site_refinement_flags Pt1 Pt 1.19471(3) 0.412786(19) 0.318949(12) 0.01449(7) Uani 1 1 d . Cl1 Cl 0.9538(2) 0.57505(13) 0.31232(9) 0.0233(3) Uani 1 1 d . Cl2 Cl 0.9333(2) 0.26898(13) 0.28373(8) 0.0213(3) Uani 1 1 d . Cl3 Cl 1.2606(2) 0.44104(15) 0.19876(8) 0.0256(3) Uani 1 1 d . N1 N 1.4088(7) 0.2693(4) 0.3265(3) 0.0185(10) Uani 1 1 d . H1A H 1.5212 0.2899 0.3593 0.028 Uiso 1 1 calc R H1B H 1.4527 0.2557 0.2817 0.028 Uiso 1 1 calc R H1C H 1.3474 0.1988 0.3417 0.028 Uiso 1 1 calc R N2 N 1.4273(8) 0.5408(5) 0.3513(3) 0.0226(11) Uani 1 1 d . H2A H 1.3721 0.6048 0.3755 0.034 Uiso 1 1 calc R H2B H 1.4815 0.5710 0.3111 0.034 Uiso 1 1 calc R H2C H 1.5312 0.5032 0.3817 0.034 Uiso 1 1 calc R N3 N 1.1442(8) 0.3854(5) 0.4261(3) 0.0179(10) Uani 1 1 d . H3A H 1.2002 0.3108 0.4420 0.027 Uiso 1 1 calc R H3B H 1.0035 0.3853 0.4295 0.027 Uiso 1 1 calc R H3C H 1.2065 0.4479 0.4544 0.027 Uiso 1 1 calc R Cl1C Cl 0.6829(2) 0.36853(15) 0.47908(9) 0.0257(3) Uani 1 1 d . O1S O 1.2710(8) 0.1350(4) 0.4428(2) 0.0291(10) Uani 1 1 d . N1S N 1.2362(8) 0.0612(5) 0.5561(3) 0.0216(11) Uani 1 1 d . C3S C 1.2643(10) 0.0481(6) 0.4863(4) 0.0225(13) Uani 1 1 d . H3S H 1.2805 -0.0342 0.4685 0.027 Uiso 1 1 calc . C2S C 1.2276(11) -0.0452(6) 0.6050(4) 0.0291(15) Uani 1 1 d . H2S1 H 1.2360 -0.1226 0.5771 0.044 Uiso 1 1 calc R H2S2 H 1.0950 -0.0434 0.6269 0.044 Uiso 1 1 calc R H2S3 H 1.3459 -0.0411 0.6440 0.044 Uiso 1 1 calc R C1S C 1.2109(13) 0.1846(6) 0.5858(4) 0.0350(17) Uani 1 1 d . H1S1 H 1.3186 0.2403 0.5701 0.052 Uiso 1 1 calc R H1S2 H 1.2260 0.1804 0.6395 0.052 Uiso 1 1 calc R H1S3 H 1.0710 0.2168 0.5678 0.052 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 0.01464(11) 0.01388(11) 0.01501(12) 0.00121(9) 0.00196(8) -0.00008(9) Cl1 0.0236(7) 0.0201(7) 0.0262(8) 0.0042(6) 0.0039(6) 0.0063(6) Cl2 0.0211(7) 0.0204(7) 0.0219(7) -0.0017(6) 0.0004(6) -0.0046(6) Cl3 0.0277(8) 0.0310(8) 0.0192(7) 0.0066(6) 0.0073(6) 0.0017(7) N1 0.017(2) 0.022(2) 0.017(3) 0.001(2) 0.0018(19) 0.005(2) N2 0.017(2) 0.021(2) 0.030(3) 0.002(2) 0.003(2) -0.007(2) N3 0.018(2) 0.023(2) 0.012(2) 0.0021(19) 0.0014(19) 0.000(2) Cl1C 0.0216(7) 0.0290(7) 0.0263(8) -0.0082(6) 0.0021(6) -0.0006(6) O1S 0.040(3) 0.025(2) 0.022(2) 0.0057(19) 0.005(2) -0.001(2) N1S 0.025(3) 0.018(2) 0.021(3) 0.002(2) -0.001(2) 0.002(2) C3S 0.021(3) 0.020(3) 0.027(3) -0.003(3) 0.004(3) 0.000(3) C2S 0.029(4) 0.022(3) 0.035(4) 0.008(3) 0.003(3) 0.002(3) C1S 0.053(5) 0.023(3) 0.028(4) -0.007(3) 0.001(3) 0.005(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' O O 0.0106 0.0060 '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 N3 Pt1 N1 90.39(19) N3 Pt1 N2 90.5(2) N1 Pt1 N2 91.4(2) N3 Pt1 Cl2 89.02(14) N1 Pt1 Cl2 88.61(15) N2 Pt1 Cl2 179.47(15) N3 Pt1 Cl3 178.42(14) N1 Pt1 Cl3 88.15(14) N2 Pt1 Cl3 88.97(16) Cl2 Pt1 Cl3 91.56(6) N3 Pt1 Cl1 88.83(14) N1 Pt1 Cl1 179.16(14) N2 Pt1 Cl1 88.27(15) Cl2 Pt1 Cl1 91.70(6) Cl3 Pt1 Cl1 92.62(6) C3S N1S C1S 119.7(5) C3S N1S C2S 122.2(5) C1S N1S C2S 118.1(6) O1S C3S N1S 124.6(6) loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance Pt1 N3 2.049(5) Pt1 N1 2.053(5) Pt1 N2 2.060(5) Pt1 Cl2 2.3103(14) Pt1 Cl3 2.3110(16) Pt1 Cl1 2.3172(14) O1S C3S 1.231(8) N1S C3S 1.320(8) N1S C1S 1.446(8) N1S C2S 1.454(8)