# Supplementary Material (ESI) for Dalton Transactions # This journal is (c) The Royal Society of Chemistry 2008 data_global _journal_name_full 'Dalton Trans.' _journal_coden_Cambridge 0222 _journal_volume ? _journal_page_first ? _journal_year ? _publ_contact_author_name 'Vadim Kukushkin' _publ_contact_author_email KUKUSHKIN@VK2100.SPB.EDU _publ_section_title ; Facile cyanamide-ammonia coupling mediated by cis- and trans-[PtIIL2] centers and giving metal-bound guanidines ; loop_ _publ_author_name 'Vadim Kukushkin' 'Nadezhda A Bokach' 'Matti Haukka' 'Maxim L Kuznetsov' 'Marina R Tyan' ; Meng-Jiy Wang ; #===END======================================================================== data_cis_4 _database_code_depnum_ccdc_archive 'CCDC 686032' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety '2(C24 H20 B), C6 H24 N8 Pt, 2(C3 H6 O)' _chemical_formula_sum 'C60 H76 B2 N8 O2 Pt' _chemical_formula_weight 1158.00 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' B B 0.0013 0.0007 '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' Pt Pt -1.7033 8.3905 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting triclinic _symmetry_space_group_name_H-M 'P -1' _symmetry_space_group_name_Hall '-P 1' loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, -y, -z' _cell_length_a 11.1727(7) _cell_length_b 21.6856(14) _cell_length_c 23.5050(16) _cell_angle_alpha 93.241(3) _cell_angle_beta 95.434(4) _cell_angle_gamma 90.226(4) _cell_volume 5660.0(6) _cell_formula_units_Z 4 _cell_measurement_temperature 120(2) _cell_measurement_reflns_used 129531 _cell_measurement_theta_min 1.00 _cell_measurement_theta_max 25.03 _exptl_crystal_description needle _exptl_crystal_colour colorless _exptl_crystal_size_max 0.22 _exptl_crystal_size_mid 0.06 _exptl_crystal_size_min 0.05 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.359 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 2384 _exptl_absorpt_coefficient_mu 2.528 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.6087 _exptl_absorpt_correction_T_max 0.8819 _exptl_absorpt_process_details 'SADABS v.2.10 (Sheldrick, 2003)' _publ_section_exptl_refinement ; The crystal was poorly diffracting, which lowers the data quality and reduces the unique / Expected reflections ratio. All hydrogens were positioned geometrically and constrained to ride on their parent atoms, with N---H = 0.88-0.91 \%A, C---H = 0.95-0.98 and U~iso~ = 1.2-1.5 U~eq~(parent atom). ; _exptl_special_details ; ? ; _diffrn_ambient_temperature 120(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator 'horizontally mounted graphite crystal' _diffrn_measurement_device_type 'Nonius KappaCCD' _diffrn_measurement_device '95mm CCD camera on \k-goniostat' _diffrn_detector_area_resol_mean 9 _diffrn_measurement_method '\f scans and \w scans with \k offset' _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 40066 _diffrn_reflns_av_R_equivalents 0.1346 _diffrn_reflns_av_sigmaI/netI 0.1526 _diffrn_reflns_limit_h_min -13 _diffrn_reflns_limit_h_max 12 _diffrn_reflns_limit_k_min -25 _diffrn_reflns_limit_k_max 25 _diffrn_reflns_limit_l_min -27 _diffrn_reflns_limit_l_max 27 _diffrn_reflns_theta_min 2.55 _diffrn_reflns_theta_max 25.00 _reflns_number_total 16891 _reflns_number_gt 9759 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'Collect (Bruker AXS BV, 1997-2004)' _computing_cell_refinement 'Denzo/Scalepack (Otwinowski & Minor, 1997)' _computing_data_reduction 'Denzo/Scalepack (Otwinowski & Minor, 1997)' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1997)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'Diamond v.3.1d (Brandenburg, 2006)' _computing_publication_material 'SHELXL-97 (Sheldrick, 1997)' _refine_special_details ; Refinement of F^2^ against ALL reflections. The weighted R-factor wR and goodness of fit S are based on F^2^, conventional R-factors R are based on F, with F set to zero for negative F^2^. The threshold expression of F^2^ > 2sigma(F^2^) is used only for calculating R-factors(gt) etc. and is not relevant to the choice of reflections for refinement. R-factors based on F^2^ are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger. ; _refine_ls_structure_factor_coef Fsqd _refine_ls_matrix_type full _refine_ls_weighting_scheme calc _refine_ls_weighting_details 'calc w=1/[\s^2^(Fo^2^)+(0.0123P)^2^+48.2731P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens mixed _refine_ls_hydrogen_treatment constr _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 16891 _refine_ls_number_parameters 1335 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.1439 _refine_ls_R_factor_gt 0.0662 _refine_ls_wR_factor_ref 0.1473 _refine_ls_wR_factor_gt 0.1233 _refine_ls_goodness_of_fit_ref 1.061 _refine_ls_restrained_S_all 1.061 _refine_ls_shift/su_max 0.022 _refine_ls_shift/su_mean 0.000 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 0.76991(4) 0.12048(2) 0.24234(2) 0.03164(15) Uani 1 1 d . . . O1 O 0.0939(10) 0.4023(5) 0.3361(5) 0.088(4) Uani 1 1 d . . . O2 O 0.1574(10) 0.2845(5) 0.1872(5) 0.074(3) Uani 1 1 d . . . O3 O 0.4272(9) 0.7844(4) 0.1972(4) 0.065(3) Uani 1 1 d . . . O4 O 0.5539(9) 0.9026(5) 0.3451(4) 0.065(3) Uani 1 1 d . . . N1 N 0.6478(9) 0.1445(5) 0.2997(4) 0.049(3) Uani 1 1 d . . . H1A H 0.5797 0.1213 0.2913 0.073 Uiso 1 1 calc R . . H1B H 0.6296 0.1852 0.2975 0.073 Uiso 1 1 calc R . . H1C H 0.6800 0.1376 0.3358 0.073 Uiso 1 1 calc R . . N2 N 0.6878(8) 0.1798(4) 0.1848(4) 0.034(2) Uani 1 1 d . . . H2A H 0.7008 0.2196 0.1986 0.050 Uiso 1 1 calc R . . H2B H 0.6073 0.1719 0.1800 0.050 Uiso 1 1 calc R . . H2C H 0.7191 0.1742 0.1506 0.050 Uiso 1 1 calc R . . N3 N 0.8554(8) 0.0673(4) 0.3016(4) 0.029(2) Uani 1 1 d . . . H3 H 0.9315 0.0764 0.3117 0.035 Uiso 1 1 calc R . . N4 N 0.8830(8) 0.0959(4) 0.1836(4) 0.033(2) Uani 1 1 d . . . H4 H 0.8803 0.0568 0.1713 0.040 Uiso 1 1 calc R . . N5 N 0.7101(8) -0.0077(4) 0.3021(4) 0.038(3) Uani 1 1 d . . . H5A H 0.6739 0.0044 0.2697 0.045 Uiso 1 1 calc R . . H5B H 0.6805 -0.0388 0.3189 0.045 Uiso 1 1 calc R . . N6 N 0.8626(8) 0.0025(4) 0.3770(4) 0.034(2) Uani 1 1 d . . . N7 N 0.9870(9) 0.1855(5) 0.1884(5) 0.048(3) Uani 1 1 d . . . H7A H 0.9547 0.1980 0.2197 0.057 Uiso 1 1 calc R . . H7B H 1.0387 0.2095 0.1739 0.057 Uiso 1 1 calc R . . N8 N 1.0087(9) 0.1135(5) 0.1120(4) 0.042(3) Uani 1 1 d . . . C1 C 0.8121(11) 0.0219(6) 0.3261(5) 0.032(3) Uani 1 1 d . . . C2 C 0.8359(12) -0.0566(5) 0.3991(6) 0.048(4) Uani 1 1 d . . . H2D H 0.7753 -0.0511 0.4264 0.072 Uiso 1 1 calc R . . H2E H 0.9094 -0.0733 0.4183 0.072 Uiso 1 1 calc R . . H2F H 0.8049 -0.0853 0.3673 0.072 Uiso 1 1 calc R . . C3 C 0.9478(10) 0.0423(5) 0.4137(5) 0.039(3) Uani 1 1 d . . . H3A H 1.0298 0.0339 0.4039 0.058 Uiso 1 1 calc R . . H3B H 0.9419 0.0339 0.4539 0.058 Uiso 1 1 calc R . . H3C H 0.9288 0.0857 0.4079 0.058 Uiso 1 1 calc R . . C4 C 0.9569(11) 0.1293(6) 0.1623(6) 0.042(3) Uani 1 1 d . . . C5 C 1.1038(12) 0.1490(7) 0.0915(6) 0.059(4) Uani 1 1 d . . . H5D H 1.0692 0.1845 0.0719 0.088 Uiso 1 1 calc R . . H5E H 1.1463 0.1230 0.0647 0.088 Uiso 1 1 calc R . . H5F H 1.1603 0.1637 0.1239 0.088 Uiso 1 1 calc R . . C6 C 0.9525(12) 0.0643(6) 0.0763(6) 0.049(4) Uani 1 1 d . . . H6A H 0.9574 0.0261 0.0967 0.074 Uiso 1 1 calc R . . H6B H 0.9936 0.0587 0.0413 0.074 Uiso 1 1 calc R . . H6C H 0.8679 0.0742 0.0662 0.074 Uiso 1 1 calc R . . C7 C 1.3407(9) 0.1117(5) 0.2921(5) 0.027(3) Uani 1 1 d . . . C8 C 1.3307(11) 0.1657(6) 0.2636(5) 0.042(3) Uani 1 1 d . . . H8 H 1.2994 0.2010 0.2828 0.050 Uiso 1 1 calc R . . C9 C 1.3632(11) 0.1717(6) 0.2090(6) 0.045(4) Uani 1 1 d . . . H9 H 1.3546 0.2100 0.1914 0.054 Uiso 1 1 calc R . . C10 C 1.4085(11) 0.1209(7) 0.1807(6) 0.049(4) Uani 1 1 d . . . H10 H 1.4292 0.1237 0.1426 0.058 Uiso 1 1 calc R . . C11 C 1.4237(11) 0.0663(7) 0.2072(6) 0.051(4) Uani 1 1 d . . . H11 H 1.4570 0.0318 0.1877 0.061 Uiso 1 1 calc R . . C12 C 1.3911(10) 0.0612(6) 0.2617(5) 0.039(3) Uani 1 1 d . . . H12 H 1.4024 0.0231 0.2794 0.046 Uiso 1 1 calc R . . C13 C 1.4388(10) 0.1217(5) 0.3949(5) 0.029(3) Uani 1 1 d . . . C14 C 1.4758(11) 0.1836(6) 0.4119(5) 0.040(3) Uani 1 1 d . . . H14 H 1.4184 0.2155 0.4071 0.048 Uiso 1 1 calc R . . C15 C 1.5901(11) 0.1992(6) 0.4348(5) 0.037(3) Uani 1 1 d . . . H15 H 1.6119 0.2414 0.4428 0.045 Uiso 1 1 calc R . . C16 C 1.6740(11) 0.1533(6) 0.4464(5) 0.040(3) Uani 1 1 d . . . H16 H 1.7521 0.1637 0.4640 0.048 Uiso 1 1 calc R . . C17 C 1.6430(11) 0.0935(6) 0.4323(5) 0.039(3) Uani 1 1 d . . . H17 H 1.6999 0.0619 0.4397 0.047 Uiso 1 1 calc R . . C18 C 1.5291(10) 0.0783(5) 0.4070(5) 0.030(3) Uani 1 1 d . . . H18 H 1.5109 0.0360 0.3973 0.036 Uiso 1 1 calc R . . C19 C 1.2614(10) 0.0353(5) 0.3682(5) 0.029(3) Uani 1 1 d . . . C20 C 1.1830(10) 0.0038(5) 0.3256(5) 0.034(3) Uani 1 1 d . . . H20 H 1.1667 0.0220 0.2899 0.040 Uiso 1 1 calc R . . C21 C 1.1284(11) -0.0525(5) 0.3331(5) 0.038(3) Uani 1 1 d . . . H21 H 1.0756 -0.0718 0.3032 0.046 Uiso 1 1 calc R . . C22 C 1.1521(11) -0.0802(5) 0.3848(5) 0.037(3) Uani 1 1 d . . . H22 H 1.1175 -0.1192 0.3902 0.044 Uiso 1 1 calc R . . C23 C 1.2244(11) -0.0511(5) 0.4270(6) 0.040(3) Uani 1 1 d . . . H23 H 1.2390 -0.0695 0.4627 0.048 Uiso 1 1 calc R . . C24 C 1.2792(10) 0.0067(5) 0.4192(5) 0.033(3) Uani 1 1 d . . . H24 H 1.3295 0.0261 0.4500 0.039 Uiso 1 1 calc R . . C25 C 1.2017(9) 0.1503(5) 0.3774(5) 0.026(3) Uani 1 1 d . . . C26 C 1.1947(11) 0.1704(5) 0.4349(5) 0.037(3) Uani 1 1 d . . . H26 H 1.2594 0.1614 0.4623 0.045 Uiso 1 1 calc R . . C27 C 1.0958(11) 0.2031(6) 0.4535(6) 0.046(4) Uani 1 1 d . . . H27 H 1.0934 0.2152 0.4929 0.055 Uiso 1 1 calc R . . C28 C 1.0035(11) 0.2174(5) 0.4144(6) 0.040(3) Uani 1 1 d . . . H28 H 0.9374 0.2404 0.4267 0.048 Uiso 1 1 calc R . . C29 C 1.0044(11) 0.1992(5) 0.3573(6) 0.043(3) Uani 1 1 d . . . H29 H 0.9399 0.2087 0.3300 0.052 Uiso 1 1 calc R . . C30 C 1.1052(10) 0.1657(5) 0.3409(5) 0.034(3) Uani 1 1 d . . . H30 H 1.1059 0.1529 0.3016 0.041 Uiso 1 1 calc R . . C31 C 0.6204(12) 0.2924(5) 0.0916(5) 0.036(3) Uani 1 1 d . . . C32 C 0.7205(12) 0.2617(5) 0.0709(5) 0.042(3) Uani 1 1 d . . . H32 H 0.7974 0.2812 0.0765 0.051 Uiso 1 1 calc R . . C33 C 0.7086(14) 0.2029(6) 0.0423(5) 0.048(4) Uani 1 1 d . . . H33 H 0.7773 0.1837 0.0286 0.058 Uiso 1 1 calc R . . C34 C 0.5988(15) 0.1727(6) 0.0339(6) 0.056(4) Uani 1 1 d . . . H34 H 0.5915 0.1330 0.0146 0.067 Uiso 1 1 calc R . . C35 C 0.4977(14) 0.2018(6) 0.0545(6) 0.054(4) Uani 1 1 d . . . H35 H 0.4215 0.1817 0.0504 0.064 Uiso 1 1 calc R . . C36 C 0.5117(12) 0.2601(6) 0.0806(5) 0.042(3) Uani 1 1 d . . . H36 H 0.4415 0.2800 0.0921 0.050 Uiso 1 1 calc R . . C37 C 0.6710(11) 0.3382(5) 0.1949(5) 0.033(3) Uani 1 1 d . . . C38 C 0.7896(12) 0.3318(5) 0.2202(5) 0.042(3) Uani 1 1 d . . . H38 H 0.8541 0.3413 0.1984 0.050 Uiso 1 1 calc R . . C39 C 0.8175(13) 0.3120(6) 0.2760(6) 0.047(4) Uani 1 1 d . . . H39 H 0.8990 0.3096 0.2913 0.057 Uiso 1 1 calc R . . C40 C 0.7278(14) 0.2964(5) 0.3080(6) 0.047(4) Uani 1 1 d . . . H40 H 0.7462 0.2825 0.3454 0.057 Uiso 1 1 calc R . . C41 C 0.6108(13) 0.3008(5) 0.2855(6) 0.045(4) Uani 1 1 d . . . H41 H 0.5474 0.2906 0.3076 0.055 Uiso 1 1 calc R . . C42 C 0.5845(11) 0.3204(5) 0.2300(6) 0.039(3) Uani 1 1 d . . . H42 H 0.5025 0.3216 0.2152 0.046 Uiso 1 1 calc R . . C43 C 0.5194(10) 0.4017(5) 0.1258(5) 0.034(3) Uani 1 1 d . . . C44 C 0.4978(11) 0.4465(5) 0.1686(5) 0.037(3) Uani 1 1 d . . . H44 H 0.5480 0.4473 0.2036 0.044 Uiso 1 1 calc R . . C45 C 0.4070(12) 0.4899(6) 0.1627(6) 0.053(4) Uani 1 1 d . . . H45 H 0.3971 0.5200 0.1928 0.064 Uiso 1 1 calc R . . C46 C 0.3308(12) 0.4890(6) 0.1124(6) 0.046(4) Uani 1 1 d . . . H46 H 0.2667 0.5175 0.1083 0.055 Uiso 1 1 calc R . . C47 C 0.3492(11) 0.4466(6) 0.0691(6) 0.046(3) Uani 1 1 d . . . H47 H 0.2988 0.4466 0.0342 0.055 Uiso 1 1 calc R . . C48 C 0.4394(10) 0.4041(5) 0.0752(5) 0.036(3) Uani 1 1 d . . . H48 H 0.4488 0.3749 0.0442 0.043 Uiso 1 1 calc R . . C49 C 0.7437(10) 0.4038(5) 0.1080(5) 0.028(3) Uani 1 1 d . . . C50 C 0.8042(11) 0.4489(6) 0.1432(6) 0.039(3) Uani 1 1 d . . . H50 H 0.7927 0.4512 0.1828 0.047 Uiso 1 1 calc R . . C51 C 0.8807(11) 0.4907(6) 0.1233(6) 0.046(4) Uani 1 1 d . . . H51 H 0.9194 0.5214 0.1492 0.055 Uiso 1 1 calc R . . C52 C 0.9025(11) 0.4891(6) 0.0660(6) 0.044(3) Uani 1 1 d . . . H52 H 0.9566 0.5175 0.0524 0.053 Uiso 1 1 calc R . . C53 C 0.8431(11) 0.4451(6) 0.0302(6) 0.042(3) Uani 1 1 d . . . H53 H 0.8553 0.4428 -0.0093 0.051 Uiso 1 1 calc R . . C54 C 0.7648(11) 0.4034(5) 0.0507(6) 0.039(3) Uani 1 1 d . . . H54 H 0.7242 0.3737 0.0244 0.047 Uiso 1 1 calc R . . C55 C 0.1564(11) 0.3697(6) 0.3668(6) 0.046(4) Uani 1 1 d . . . C56 C 0.2338(11) 0.3198(6) 0.3461(7) 0.062(4) Uani 1 1 d . . . H56A H 0.2264 0.3173 0.3041 0.093 Uiso 1 1 calc R . . H56B H 0.2088 0.2804 0.3599 0.093 Uiso 1 1 calc R . . H56C H 0.3177 0.3287 0.3605 0.093 Uiso 1 1 calc R . . C57 C 0.1615(13) 0.3801(7) 0.4308(7) 0.068(4) Uani 1 1 d . . . H57A H 0.1385 0.4227 0.4405 0.102 Uiso 1 1 calc R . . H57B H 0.2434 0.3729 0.4478 0.102 Uiso 1 1 calc R . . H57C H 0.1058 0.3514 0.4458 0.102 Uiso 1 1 calc R . . C58 C 0.1398(13) 0.3340(7) 0.1684(7) 0.060(4) Uani 1 1 d . . . C59 C 0.0805(15) 0.3396(7) 0.1111(7) 0.082(5) Uani 1 1 d . . . H59A H 0.0539 0.2987 0.0948 0.123 Uiso 1 1 calc R . . H59B H 0.1370 0.3572 0.0868 0.123 Uiso 1 1 calc R . . H59C H 0.0108 0.3666 0.1130 0.123 Uiso 1 1 calc R . . C60 C 0.174(2) 0.3938(8) 0.2029(9) 0.138(10) Uani 1 1 d . . . H60A H 0.1497 0.3916 0.2417 0.206 Uiso 1 1 calc R . . H60B H 0.1341 0.4284 0.1844 0.206 Uiso 1 1 calc R . . H60C H 0.2617 0.3999 0.2050 0.206 Uiso 1 1 calc R . . C61 C 0.4274(13) 0.8354(7) 0.1779(6) 0.056(4) Uani 1 1 d . . . C62 C 0.4627(14) 0.8454(7) 0.1205(7) 0.074(5) Uani 1 1 d . . . H62A H 0.4843 0.8058 0.1022 0.111 Uiso 1 1 calc R . . H62B H 0.5320 0.8737 0.1237 0.111 Uiso 1 1 calc R . . H62C H 0.3954 0.8634 0.0975 0.111 Uiso 1 1 calc R . . C63 C 0.401(2) 0.8918(8) 0.2120(8) 0.141(10) Uani 1 1 d . . . H63A H 0.3764 0.8807 0.2490 0.211 Uiso 1 1 calc R . . H63B H 0.3367 0.9145 0.1914 0.211 Uiso 1 1 calc R . . H63C H 0.4738 0.9179 0.2183 0.211 Uiso 1 1 calc R . . C64 C 0.5077(10) 0.8731(6) 0.3784(6) 0.036(3) Uani 1 1 d . . . C65 C 0.4207(11) 0.8202(5) 0.3599(6) 0.043(3) Uani 1 1 d . . . H65A H 0.3389 0.8327 0.3669 0.065 Uiso 1 1 calc R . . H65B H 0.4432 0.7842 0.3819 0.065 Uiso 1 1 calc R . . H65C H 0.4237 0.8094 0.3190 0.065 Uiso 1 1 calc R . . C66 C 0.5351(12) 0.8855(6) 0.4429(6) 0.054(4) Uani 1 1 d . . . H66A H 0.5913 0.8545 0.4579 0.081 Uiso 1 1 calc R . . H66B H 0.4603 0.8833 0.4614 0.081 Uiso 1 1 calc R . . H66C H 0.5711 0.9268 0.4507 0.081 Uiso 1 1 calc R . . B1 B 1.3137(12) 0.1057(6) 0.3579(6) 0.032(4) Uani 1 1 d . . . B2 B 0.6390(12) 0.3576(6) 0.1299(6) 0.032(3) Uani 1 1 d . . . Pt1B Pt 0.83292(4) 0.61974(2) 0.24735(2) 0.03107(15) Uani 1 1 d . . . N1B N 0.8933(9) 0.6806(4) 0.1913(4) 0.041(3) Uani 1 1 d . . . H1B1 H 0.8609 0.7184 0.1979 0.062 Uiso 1 1 calc R . . H1B2 H 0.8707 0.6665 0.1546 0.062 Uiso 1 1 calc R . . H1B3 H 0.9749 0.6836 0.1967 0.062 Uiso 1 1 calc R . . N2B N 0.9816(8) 0.6441(4) 0.3048(4) 0.039(3) Uani 1 1 d . . . H2B1 H 0.9670 0.6342 0.3406 0.059 Uiso 1 1 calc R . . H2B2 H 0.9955 0.6855 0.3046 0.059 Uiso 1 1 calc R . . H2B3 H 1.0472 0.6233 0.2942 0.059 Uiso 1 1 calc R . . N3B N 0.6947(8) 0.5948(4) 0.1877(4) 0.040(3) Uani 1 1 d . . . H3B4 H 0.6900 0.5557 0.1755 0.048 Uiso 1 1 calc R . . N4B N 0.7712(9) 0.5653(4) 0.3050(4) 0.033(2) Uani 1 1 d . . . H4B H 0.6983 0.5734 0.3144 0.040 Uiso 1 1 calc R . . N5B N 0.5937(9) 0.6836(4) 0.1941(4) 0.043(3) Uani 1 1 d . . . H5B1 H 0.6354 0.6942 0.2269 0.051 Uiso 1 1 calc R . . H5B2 H 0.5382 0.7084 0.1796 0.051 Uiso 1 1 calc R . . N6B N 0.5439(9) 0.6150(4) 0.1155(4) 0.040(3) Uani 1 1 d . . . N7B N 0.9151(8) 0.4918(4) 0.3040(4) 0.038(3) Uani 1 1 d . . . H7B1 H 0.9349 0.5048 0.2713 0.045 Uiso 1 1 calc R . . H7B2 H 0.9538 0.4607 0.3195 0.045 Uiso 1 1 calc R . . N8B N 0.7952(8) 0.4993(4) 0.3810(4) 0.034(2) Uani 1 1 d . . . C1B C 0.6146(10) 0.6303(5) 0.1667(5) 0.033(3) Uani 1 1 d . . . C2B C 0.4448(12) 0.6509(6) 0.0965(6) 0.056(4) Uani 1 1 d . . . H2D1 H 0.4040 0.6664 0.1294 0.083 Uiso 1 1 calc R . . H2D2 H 0.3887 0.6255 0.0704 0.083 Uiso 1 1 calc R . . H2D3 H 0.4728 0.6859 0.0764 0.083 Uiso 1 1 calc R . . C3B C 0.5879(11) 0.5659(6) 0.0792(5) 0.043(3) Uani 1 1 d . . . H3B1 H 0.5882 0.5271 0.0988 0.064 Uiso 1 1 calc R . . H3B2 H 0.6699 0.5758 0.0709 0.064 Uiso 1 1 calc R . . H3B3 H 0.5356 0.5613 0.0433 0.064 Uiso 1 1 calc R . . C4B C 0.8248(11) 0.5196(5) 0.3304(5) 0.033(3) Uani 1 1 d . . . C5B C 0.8322(12) 0.4390(6) 0.4010(6) 0.053(4) Uani 1 1 d . . . H5D1 H 0.8509 0.4118 0.3684 0.080 Uiso 1 1 calc R . . H5D2 H 0.7668 0.4207 0.4196 0.080 Uiso 1 1 calc R . . H5D3 H 0.9037 0.4440 0.4285 0.080 Uiso 1 1 calc R . . C6B C 0.7223(10) 0.5372(5) 0.4173(5) 0.039(3) Uani 1 1 d . . . H6D1 H 0.7384 0.5809 0.4126 0.058 Uiso 1 1 calc R . . H6D2 H 0.7425 0.5279 0.4574 0.058 Uiso 1 1 calc R . . H6D3 H 0.6370 0.5280 0.4064 0.058 Uiso 1 1 calc R . . C7B C 1.0324(11) 0.9001(5) 0.1248(5) 0.037(3) Uani 1 1 d . . . C8B C 1.0691(10) 0.9455(5) 0.1662(5) 0.037(3) Uani 1 1 d . . . H8B H 1.0312 0.9481 0.2008 0.044 Uiso 1 1 calc R . . C9B C 1.1614(12) 0.9884(6) 0.1590(6) 0.048(4) Uani 1 1 d . . . H9B H 1.1840 1.0197 0.1879 0.058 Uiso 1 1 calc R . . C10B C 1.2188(12) 0.9840(6) 0.1087(6) 0.046(4) Uani 1 1 d . . . H10B H 1.2814 1.0123 0.1033 0.055 Uiso 1 1 calc R . . C11B C 1.1845(12) 0.9388(6) 0.0671(6) 0.045(3) Uani 1 1 d . . . H11B H 1.2240 0.9357 0.0330 0.054 Uiso 1 1 calc R . . C12B C 1.0931(10) 0.8977(5) 0.0743(5) 0.032(3) Uani 1 1 d . . . H12B H 1.0703 0.8671 0.0447 0.039 Uiso 1 1 calc R . . C13B C 0.9121(11) 0.7902(5) 0.0942(5) 0.032(3) Uani 1 1 d . . . C14B C 1.0139(11) 0.7571(5) 0.0840(5) 0.037(3) Uani 1 1 d . . . H14B H 1.0898 0.7755 0.0964 0.044 Uiso 1 1 calc R . . C15B C 1.0124(14) 0.6975(6) 0.0564(6) 0.049(4) Uani 1 1 d . . . H15B H 1.0850 0.6766 0.0501 0.059 Uiso 1 1 calc R . . C16B C 0.9005(16) 0.6704(6) 0.0387(6) 0.058(4) Uani 1 1 d . . . H16B H 0.8969 0.6301 0.0206 0.070 Uiso 1 1 calc R . . C17B C 0.7939(13) 0.7015(6) 0.0472(6) 0.052(4) Uani 1 1 d . . . H17B H 0.7181 0.6828 0.0348 0.062 Uiso 1 1 calc R . . C18B C 0.8009(12) 0.7603(5) 0.0743(5) 0.039(3) Uani 1 1 d . . . H18B H 0.7283 0.7815 0.0797 0.047 Uiso 1 1 calc R . . C19B C 0.9071(11) 0.8382(5) 0.1970(5) 0.031(3) Uani 1 1 d . . . C20B C 1.0103(11) 0.8207(5) 0.2297(5) 0.037(3) Uani 1 1 d . . . H20B H 1.0849 0.8214 0.2135 0.045 Uiso 1 1 calc R . . C21B C 1.0086(13) 0.8021(5) 0.2860(6) 0.047(4) Uani 1 1 d . . . H21B H 1.0816 0.7933 0.3080 0.056 Uiso 1 1 calc R . . C22B C 0.8989(14) 0.7965(6) 0.3095(6) 0.050(4) Uani 1 1 d . . . H22B H 0.8957 0.7826 0.3469 0.060 Uiso 1 1 calc R . . C23B C 0.7961(13) 0.8118(6) 0.2769(7) 0.053(4) Uani 1 1 d . . . H23B H 0.7206 0.8088 0.2921 0.064 Uiso 1 1 calc R . . C24B C 0.8006(12) 0.8317(5) 0.2219(5) 0.039(3) Uani 1 1 d . . . H24B H 0.7274 0.8412 0.2004 0.047 Uiso 1 1 calc R . . C25B C 0.8003(10) 0.9017(5) 0.1084(5) 0.035(3) Uani 1 1 d . . . C26B C 0.7569(10) 0.9483(5) 0.1447(5) 0.035(3) Uani 1 1 d . . . H26B H 0.7858 0.9506 0.1841 0.042 Uiso 1 1 calc R . . C27B C 0.6739(10) 0.9910(6) 0.1251(6) 0.047(4) Uani 1 1 d . . . H27B H 0.6484 1.0225 0.1509 0.056 Uiso 1 1 calc R . . C28B C 0.6265(11) 0.9884(6) 0.0672(6) 0.042(3) Uani 1 1 d . . . H28B H 0.5681 1.0171 0.0534 0.051 Uiso 1 1 calc R . . C29B C 0.6684(11) 0.9426(6) 0.0315(6) 0.044(3) Uani 1 1 d . . . H29B H 0.6385 0.9396 -0.0078 0.053 Uiso 1 1 calc R . . C30B C 0.7519(11) 0.9016(5) 0.0514(5) 0.035(3) Uani 1 1 d . . . H30B H 0.7789 0.8712 0.0249 0.042 Uiso 1 1 calc R . . C31B C 0.3888(10) 0.5323(5) 0.3758(5) 0.028(3) Uani 1 1 d . . . C32B C 0.4448(10) 0.4990(5) 0.3331(5) 0.039(3) Uani 1 1 d . . . H32B H 0.4459 0.5150 0.2964 0.046 Uiso 1 1 calc R . . C33B C 0.4988(11) 0.4428(5) 0.3440(5) 0.041(3) Uani 1 1 d . . . H33B H 0.5377 0.4217 0.3145 0.049 Uiso 1 1 calc R . . C34B C 0.4981(11) 0.4165(6) 0.3958(6) 0.040(3) Uani 1 1 d . . . H34B H 0.5324 0.3771 0.4016 0.048 Uiso 1 1 calc R . . C35B C 0.4462(11) 0.4491(5) 0.4392(6) 0.041(3) Uani 1 1 d . . . H35B H 0.4468 0.4328 0.4759 0.049 Uiso 1 1 calc R . . C36B C 0.3926(10) 0.5063(5) 0.4288(5) 0.033(3) Uani 1 1 d . . . H36B H 0.3575 0.5282 0.4591 0.039 Uiso 1 1 calc R . . C37B C 0.2245(10) 0.6217(5) 0.4026(5) 0.031(3) Uani 1 1 d . . . C38B C 0.1400(9) 0.5796(5) 0.4167(5) 0.032(3) Uani 1 1 d . . . H38B H 0.1525 0.5370 0.4080 0.038 Uiso 1 1 calc R . . C39B C 0.0382(11) 0.5968(6) 0.4430(5) 0.041(3) Uani 1 1 d . . . H39B H -0.0146 0.5660 0.4539 0.050 Uiso 1 1 calc R . . C40B C 0.0131(12) 0.6591(6) 0.4534(5) 0.044(3) Uani 1 1 d . . . H40B H -0.0595 0.6714 0.4686 0.052 Uiso 1 1 calc R . . C41B C 0.0964(11) 0.7029(6) 0.4410(6) 0.045(4) Uani 1 1 d . . . H41B H 0.0831 0.7454 0.4501 0.054 Uiso 1 1 calc R . . C42B C 0.2000(10) 0.6848(5) 0.4153(5) 0.036(3) Uani 1 1 d . . . H42B H 0.2548 0.7155 0.4063 0.043 Uiso 1 1 calc R . . C43B C 0.4573(10) 0.6477(5) 0.3847(5) 0.030(3) Uani 1 1 d . . . C44B C 0.4874(11) 0.6692(5) 0.4398(5) 0.032(3) Uani 1 1 d . . . H44B H 0.4348 0.6602 0.4678 0.038 Uiso 1 1 calc R . . C45B C 0.5929(11) 0.7042(5) 0.4576(5) 0.035(3) Uani 1 1 d . . . H45B H 0.6093 0.7186 0.4965 0.042 Uiso 1 1 calc R . . C46B C 0.6707(11) 0.7169(5) 0.4186(6) 0.039(3) Uani 1 1 d . . . H46B H 0.7420 0.7402 0.4298 0.047 Uiso 1 1 calc R . . C47B C 0.6431(12) 0.6946(5) 0.3610(6) 0.047(4) Uani 1 1 d . . . H47B H 0.6962 0.7023 0.3329 0.056 Uiso 1 1 calc R . . C48B C 0.5344(11) 0.6604(5) 0.3457(5) 0.035(3) Uani 1 1 d . . . H48B H 0.5155 0.6460 0.3070 0.042 Uiso 1 1 calc R . . C49B C 0.2807(9) 0.6090(5) 0.2991(5) 0.027(3) Uani 1 1 d . . . C50B C 0.2814(11) 0.6640(6) 0.2705(6) 0.044(4) Uani 1 1 d . . . H50B H 0.3215 0.6991 0.2897 0.053 Uiso 1 1 calc R . . C51B C 0.2271(10) 0.6697(6) 0.2162(6) 0.038(3) Uani 1 1 d . . . H51B H 0.2309 0.7079 0.1985 0.046 Uiso 1 1 calc R . . C52B C 0.1681(13) 0.6206(7) 0.1878(6) 0.062(5) Uani 1 1 d . . . H52B H 0.1317 0.6242 0.1500 0.074 Uiso 1 1 calc R . . C53B C 0.1607(11) 0.5652(6) 0.2140(5) 0.039(3) Uani 1 1 d . . . H53B H 0.1189 0.5310 0.1942 0.047 Uiso 1 1 calc R . . C54B C 0.2152(10) 0.5595(5) 0.2700(5) 0.033(3) Uani 1 1 d . . . H54B H 0.2075 0.5219 0.2882 0.040 Uiso 1 1 calc R . . B1B B 0.9128(13) 0.8562(7) 0.1305(6) 0.036(4) Uani 1 1 d . . . B2B B 0.3382(13) 0.6023(6) 0.3655(6) 0.030(3) Uani 1 1 d . . . 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 0.0343(3) 0.0267(3) 0.0345(3) 0.0027(2) 0.0060(2) 0.0005(2) O1 0.080(8) 0.097(9) 0.093(9) 0.039(7) 0.022(7) 0.054(7) O2 0.102(9) 0.049(7) 0.071(8) 0.019(6) -0.010(6) 0.001(6) O3 0.076(8) 0.040(6) 0.084(8) 0.021(5) 0.023(6) 0.027(5) O4 0.076(8) 0.082(8) 0.040(6) 0.013(5) 0.012(5) -0.032(6) N1 0.037(7) 0.072(8) 0.037(7) 0.001(6) 0.010(5) -0.007(6) N2 0.035(6) 0.037(6) 0.030(6) 0.012(5) -0.001(5) 0.007(5) N3 0.017(5) 0.024(5) 0.048(7) 0.013(5) 0.002(4) -0.006(4) N4 0.036(6) 0.024(6) 0.041(7) -0.003(4) 0.019(5) -0.017(5) N5 0.023(6) 0.034(6) 0.057(7) 0.003(5) 0.006(5) -0.006(5) N6 0.034(6) 0.025(6) 0.043(7) -0.003(5) 0.009(5) -0.001(5) N7 0.049(8) 0.040(7) 0.053(8) -0.010(6) 0.011(6) -0.009(5) N8 0.047(7) 0.045(7) 0.034(7) -0.003(5) 0.015(5) -0.002(6) C1 0.027(8) 0.043(8) 0.026(7) -0.005(6) 0.000(6) 0.014(6) C2 0.062(10) 0.020(7) 0.062(10) 0.013(6) -0.002(7) 0.000(6) C3 0.039(8) 0.043(8) 0.039(8) 0.014(6) 0.016(6) 0.013(6) C4 0.033(8) 0.035(8) 0.054(10) 0.000(7) -0.001(7) 0.011(6) C5 0.054(10) 0.067(10) 0.058(11) -0.002(8) 0.026(8) -0.007(8) C6 0.060(10) 0.041(8) 0.048(9) -0.006(7) 0.014(7) 0.002(7) C7 0.014(6) 0.034(7) 0.034(7) 0.002(5) 0.007(5) -0.001(5) C8 0.037(8) 0.058(9) 0.031(8) 0.002(6) 0.010(6) 0.005(7) C9 0.028(8) 0.050(9) 0.056(10) 0.007(7) 0.005(7) -0.011(7) C10 0.023(8) 0.076(11) 0.048(9) 0.017(8) 0.007(6) -0.018(7) C11 0.045(9) 0.073(11) 0.033(9) -0.010(7) 0.005(7) 0.009(7) C12 0.024(7) 0.054(9) 0.037(9) -0.002(6) 0.004(6) -0.002(6) C13 0.028(7) 0.031(7) 0.029(7) -0.004(5) 0.012(5) -0.001(6) C14 0.031(8) 0.058(9) 0.031(8) 0.008(6) -0.003(6) 0.015(7) C15 0.039(8) 0.034(7) 0.039(8) -0.003(6) 0.007(6) -0.001(6) C16 0.029(7) 0.060(9) 0.030(8) -0.003(6) 0.006(6) 0.004(7) C17 0.047(9) 0.044(8) 0.027(7) 0.003(6) 0.005(6) 0.010(7) C18 0.025(7) 0.031(7) 0.035(7) 0.006(5) -0.001(5) 0.006(6) C19 0.031(7) 0.030(7) 0.029(7) 0.003(5) 0.011(5) 0.008(6) C20 0.039(8) 0.031(7) 0.031(7) 0.007(5) 0.005(6) 0.007(6) C21 0.036(8) 0.038(8) 0.040(8) -0.004(6) 0.005(6) -0.008(6) C22 0.050(9) 0.028(7) 0.032(8) 0.002(6) 0.001(6) 0.006(6) C23 0.041(8) 0.037(8) 0.044(9) 0.013(6) 0.007(6) 0.014(6) C24 0.031(7) 0.037(7) 0.030(7) 0.009(5) 0.001(5) -0.002(6) C25 0.018(6) 0.015(6) 0.043(8) -0.006(5) 0.007(5) 0.002(5) C26 0.036(8) 0.037(7) 0.038(8) 0.002(6) -0.001(6) 0.005(6) C27 0.043(9) 0.040(8) 0.054(9) -0.005(7) 0.010(7) 0.002(7) C28 0.025(8) 0.028(7) 0.064(10) -0.003(6) 0.002(6) -0.002(6) C29 0.036(8) 0.028(7) 0.065(10) 0.004(6) 0.002(7) 0.008(6) C30 0.031(7) 0.031(7) 0.038(8) 0.005(5) -0.007(6) 0.000(6) C31 0.051(9) 0.030(7) 0.031(7) 0.010(5) 0.011(6) 0.012(7) C32 0.063(10) 0.031(8) 0.035(8) 0.013(6) 0.006(7) 0.002(7) C33 0.088(12) 0.023(7) 0.037(8) -0.001(6) 0.022(7) 0.015(7) C34 0.100(13) 0.032(8) 0.033(8) 0.003(6) -0.013(8) -0.024(9) C35 0.061(11) 0.040(9) 0.058(10) 0.000(7) -0.002(8) -0.006(8) C36 0.044(9) 0.043(8) 0.038(8) 0.011(6) -0.007(6) -0.011(7) C37 0.039(8) 0.022(6) 0.037(8) 0.003(5) 0.003(6) 0.002(6) C38 0.060(10) 0.026(7) 0.040(9) 0.006(6) 0.005(7) -0.007(6) C39 0.053(10) 0.035(8) 0.050(10) -0.003(7) -0.012(8) -0.007(7) C40 0.077(12) 0.033(8) 0.029(8) 0.001(6) -0.006(8) 0.002(7) C41 0.069(11) 0.021(7) 0.048(9) 0.003(6) 0.019(7) 0.013(7) C42 0.040(8) 0.029(7) 0.046(9) 0.004(6) -0.005(6) 0.005(6) C43 0.038(8) 0.025(7) 0.039(8) 0.002(5) 0.009(6) -0.007(6) C44 0.053(9) 0.034(7) 0.024(7) 0.012(5) 0.001(6) 0.010(6) C45 0.069(10) 0.056(9) 0.035(8) -0.001(7) 0.007(7) 0.031(8) C46 0.053(9) 0.047(8) 0.039(9) 0.003(7) 0.006(7) 0.014(7) C47 0.041(8) 0.049(8) 0.046(9) 0.002(7) -0.005(6) 0.012(7) C48 0.039(8) 0.036(7) 0.033(8) 0.002(5) 0.008(6) 0.001(6) C49 0.029(7) 0.024(7) 0.030(8) 0.001(5) 0.001(5) 0.010(5) C50 0.037(8) 0.040(8) 0.043(9) 0.009(6) 0.009(6) 0.008(7) C51 0.039(8) 0.027(7) 0.071(11) 0.007(7) -0.007(7) -0.003(6) C52 0.039(9) 0.043(8) 0.056(10) 0.021(7) 0.020(7) 0.005(7) C53 0.032(8) 0.055(9) 0.041(9) 0.004(7) 0.007(6) 0.000(7) C54 0.037(8) 0.031(7) 0.047(9) 0.009(6) -0.006(6) 0.006(6) C55 0.035(8) 0.038(8) 0.067(11) 0.013(7) 0.009(7) -0.004(7) C56 0.033(9) 0.055(10) 0.097(13) 0.001(8) 0.001(8) 0.005(7) C57 0.060(11) 0.078(12) 0.070(12) 0.014(9) 0.019(8) -0.009(8) C58 0.063(11) 0.047(10) 0.074(12) 0.019(8) 0.029(9) 0.004(8) C59 0.106(15) 0.063(11) 0.077(13) 0.022(9) -0.007(11) 0.007(10) C60 0.27(3) 0.038(11) 0.101(17) 0.007(10) 0.011(17) -0.062(14) C61 0.059(10) 0.051(10) 0.054(10) 0.007(8) -0.012(8) 0.019(8) C62 0.083(13) 0.052(10) 0.089(15) 0.021(9) 0.013(10) 0.001(9) C63 0.26(3) 0.061(13) 0.083(15) -0.012(11) -0.050(16) 0.062(15) C64 0.025(7) 0.035(8) 0.049(9) 0.005(6) 0.003(6) 0.000(6) C65 0.038(8) 0.041(8) 0.051(9) 0.010(6) 0.002(6) -0.003(6) C66 0.067(10) 0.044(9) 0.053(10) 0.007(7) 0.009(8) -0.011(7) B1 0.025(8) 0.031(8) 0.039(9) -0.002(6) 0.003(6) 0.006(6) B2 0.031(9) 0.034(8) 0.033(9) 0.000(6) 0.006(6) -0.003(7) Pt1B 0.0333(3) 0.0265(3) 0.0334(3) 0.0029(2) 0.0025(2) 0.0044(2) N1B 0.057(7) 0.025(6) 0.040(7) 0.001(5) 0.000(5) 0.011(5) N2B 0.029(6) 0.043(6) 0.043(7) 0.007(5) -0.009(5) 0.013(5) N3B 0.040(6) 0.027(6) 0.050(7) 0.008(5) -0.019(5) 0.003(5) N4B 0.036(6) 0.024(6) 0.041(7) 0.009(5) 0.009(5) -0.001(5) N5B 0.040(7) 0.039(7) 0.047(7) 0.001(5) -0.007(5) 0.005(5) N6B 0.040(7) 0.045(6) 0.031(6) 0.003(5) -0.007(5) 0.005(5) N7B 0.045(7) 0.026(6) 0.043(7) 0.009(5) 0.007(5) 0.021(5) N8B 0.035(6) 0.024(6) 0.042(7) 0.003(5) -0.002(5) 0.002(5) C1B 0.026(7) 0.035(7) 0.037(8) -0.008(6) 0.005(6) 0.001(6) C2B 0.052(9) 0.057(9) 0.054(10) -0.005(7) -0.010(7) 0.018(7) C3B 0.050(9) 0.047(8) 0.028(7) -0.015(6) -0.004(6) 0.003(7) C4B 0.041(8) 0.018(6) 0.038(8) 0.001(5) -0.006(6) -0.005(6) C5B 0.059(10) 0.043(9) 0.061(10) 0.028(7) 0.008(7) 0.013(7) C6B 0.038(8) 0.043(8) 0.037(8) -0.002(6) 0.015(6) 0.008(6) C7B 0.039(8) 0.026(7) 0.045(9) 0.010(6) -0.001(6) 0.008(6) C8B 0.029(7) 0.039(8) 0.042(8) 0.007(6) 0.001(6) -0.001(6) C9B 0.053(9) 0.037(8) 0.051(10) 0.001(6) -0.011(7) -0.011(7) C10B 0.043(9) 0.050(9) 0.047(10) 0.012(7) 0.010(7) -0.003(7) C11B 0.044(9) 0.052(9) 0.039(9) 0.007(7) 0.010(7) 0.004(7) C12B 0.027(7) 0.034(7) 0.036(8) -0.010(6) 0.012(6) -0.002(6) C13B 0.033(8) 0.037(7) 0.026(7) 0.009(5) -0.004(5) 0.001(6) C14B 0.043(8) 0.025(7) 0.042(8) 0.001(6) 0.004(6) 0.005(6) C15B 0.075(11) 0.034(8) 0.040(9) 0.003(6) 0.015(7) 0.011(8) C16B 0.106(14) 0.029(8) 0.041(9) 0.002(6) 0.006(9) 0.005(9) C17B 0.066(11) 0.032(8) 0.053(10) 0.006(7) -0.015(8) -0.009(7) C18B 0.044(9) 0.029(7) 0.046(9) 0.009(6) 0.008(6) 0.002(6) C19B 0.035(8) 0.018(6) 0.043(8) 0.001(5) 0.013(6) 0.002(5) C20B 0.050(9) 0.023(7) 0.039(8) -0.005(5) 0.005(6) -0.009(6) C21B 0.064(10) 0.032(8) 0.043(9) 0.005(6) -0.003(7) -0.004(7) C22B 0.081(12) 0.044(9) 0.028(8) 0.009(6) 0.013(8) 0.004(8) C23B 0.060(11) 0.033(8) 0.070(12) 0.003(7) 0.025(8) 0.007(7) C24B 0.055(10) 0.031(7) 0.032(8) 0.001(6) 0.004(7) 0.004(6) C25B 0.033(8) 0.030(7) 0.044(9) 0.003(6) 0.008(6) -0.008(6) C26B 0.036(8) 0.029(7) 0.040(8) -0.003(6) 0.009(6) 0.002(6) C27B 0.028(8) 0.037(8) 0.080(12) 0.002(7) 0.023(7) 0.007(6) C28B 0.032(8) 0.036(8) 0.057(10) 0.004(7) -0.008(7) 0.002(6) C29B 0.036(8) 0.052(9) 0.042(8) 0.003(7) -0.004(6) -0.005(7) C30B 0.046(8) 0.027(7) 0.033(8) 0.006(5) 0.009(6) 0.001(6) C31B 0.023(7) 0.026(6) 0.035(8) 0.003(5) -0.003(5) -0.005(5) C32B 0.043(8) 0.041(8) 0.033(8) 0.003(6) 0.006(6) 0.015(6) C33B 0.044(8) 0.041(8) 0.034(8) -0.015(6) -0.001(6) 0.026(6) C34B 0.044(9) 0.029(7) 0.047(9) 0.002(6) -0.004(7) -0.001(6) C35B 0.043(8) 0.032(7) 0.046(9) 0.007(6) -0.006(6) -0.003(6) C36B 0.033(8) 0.033(7) 0.031(8) -0.003(6) 0.000(6) 0.002(6) C37B 0.039(8) 0.028(7) 0.027(7) 0.010(5) -0.002(5) 0.002(6) C38B 0.016(7) 0.034(7) 0.045(8) 0.000(6) 0.001(5) -0.005(6) C39B 0.035(8) 0.048(9) 0.042(8) 0.015(6) 0.001(6) -0.007(6) C40B 0.041(8) 0.046(9) 0.044(9) -0.006(6) 0.011(6) 0.005(7) C41B 0.037(9) 0.045(9) 0.054(10) 0.001(7) 0.010(7) 0.005(7) C42B 0.031(8) 0.031(7) 0.048(8) 0.001(6) 0.016(6) -0.003(6) C43B 0.035(8) 0.025(7) 0.032(8) 0.010(5) 0.008(6) 0.015(6) C44B 0.036(8) 0.024(6) 0.035(8) -0.002(5) 0.007(6) 0.005(6) C45B 0.039(8) 0.041(8) 0.024(7) -0.003(5) 0.000(6) 0.014(6) C46B 0.037(8) 0.035(8) 0.045(9) -0.006(6) 0.002(7) 0.001(6) C47B 0.057(10) 0.028(7) 0.061(10) 0.010(7) 0.027(7) 0.008(7) C48B 0.037(8) 0.036(7) 0.032(8) -0.001(6) 0.000(6) 0.012(6) C49B 0.015(6) 0.032(7) 0.033(7) 0.000(5) -0.001(5) 0.010(5) C50B 0.040(9) 0.034(8) 0.057(10) -0.002(6) 0.004(7) 0.011(6) C51B 0.028(8) 0.044(8) 0.043(9) 0.014(7) 0.001(6) 0.013(6) C52B 0.056(10) 0.087(12) 0.045(10) 0.010(9) 0.011(8) 0.045(9) C53B 0.040(8) 0.042(8) 0.033(8) 0.004(6) -0.003(6) 0.008(6) C54B 0.024(7) 0.027(7) 0.049(9) 0.002(6) 0.009(6) 0.004(5) B1B 0.033(9) 0.038(9) 0.036(9) 0.002(7) 0.002(7) 0.002(7) B2B 0.038(9) 0.029(8) 0.025(8) 0.000(6) 0.015(6) 0.000(7) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; 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 N4 2.009(9) . ? Pt1 N3 2.031(9) . ? Pt1 N1 2.056(10) . ? Pt1 N2 2.073(8) . ? O1 C55 1.215(15) . ? O2 C58 1.195(15) . ? O3 C61 1.218(15) . ? O4 C64 1.191(14) . ? N1 H1A 0.9100 . ? N1 H1B 0.9100 . ? N1 H1C 0.9100 . ? N2 H2A 0.9100 . ? N2 H2B 0.9100 . ? N2 H2C 0.9100 . ? N3 C1 1.284(14) . ? N3 H3 0.8800 . ? N4 C4 1.253(15) . ? N4 H4 0.8800 . ? N5 C1 1.364(14) . ? N5 H5A 0.8800 . ? N5 H5B 0.8800 . ? N6 C1 1.364(14) . ? N6 C2 1.449(14) . ? N6 C3 1.467(15) . ? N7 C4 1.359(15) . ? N7 H7A 0.8800 . ? N7 H7B 0.8800 . ? N8 C4 1.392(16) . ? N8 C6 1.425(15) . ? N8 C5 1.445(15) . ? C2 H2D 0.9800 . ? C2 H2E 0.9800 . ? C2 H2F 0.9800 . ? C3 H3A 0.9800 . ? C3 H3B 0.9800 . ? C3 H3C 0.9800 . ? C5 H5D 0.9800 . ? C5 H5E 0.9800 . ? C5 H5F 0.9800 . ? C6 H6A 0.9800 . ? C6 H6B 0.9800 . ? C6 H6C 0.9800 . ? C7 C8 1.381(16) . ? C7 C12 1.422(16) . ? C7 B1 1.616(19) . ? C8 C9 1.378(17) . ? C8 H8 0.9500 . ? C9 C10 1.378(18) . ? C9 H9 0.9500 . ? C10 C11 1.373(17) . ? C10 H10 0.9500 . ? C11 C12 1.377(17) . ? C11 H11 0.9500 . ? C12 H12 0.9500 . ? C13 C18 1.402(14) . ? C13 C14 1.425(16) . ? C13 B1 1.600(17) . ? C14 C15 1.372(15) . ? C14 H14 0.9500 . ? C15 C16 1.391(16) . ? C15 H15 0.9500 . ? C16 C17 1.355(16) . ? C16 H16 0.9500 . ? C17 C18 1.383(15) . ? C17 H17 0.9500 . ? C18 H18 0.9500 . ? C19 C24 1.379(15) . ? C19 C20 1.411(16) . ? C19 B1 1.671(18) . ? C20 C21 1.390(15) . ? C20 H20 0.9500 . ? C21 C22 1.389(16) . ? C21 H21 0.9500 . ? C22 C23 1.345(16) . ? C22 H22 0.9500 . ? C23 C24 1.421(16) . ? C23 H23 0.9500 . ? C24 H24 0.9500 . ? C25 C30 1.368(14) . ? C25 C26 1.405(16) . ? C25 B1 1.666(16) . ? C26 C27 1.407(16) . ? C26 H26 0.9500 . ? C27 C28 1.364(16) . ? C27 H27 0.9500 . ? C28 C29 1.380(17) . ? C28 H28 0.9500 . ? C29 C30 1.415(15) . ? C29 H29 0.9500 . ? C30 H30 0.9500 . ? C31 C36 1.395(16) . ? C31 C32 1.416(16) . ? C31 B2 1.634(18) . ? C32 C33 1.406(17) . ? C32 H32 0.9500 . ? C33 C34 1.381(18) . ? C33 H33 0.9500 . ? C34 C35 1.408(19) . ? C34 H34 0.9500 . ? C35 C36 1.375(17) . ? C35 H35 0.9500 . ? C36 H36 0.9500 . ? C37 C42 1.395(16) . ? C37 C38 1.410(16) . ? C37 B2 1.617(18) . ? C38 C39 1.411(17) . ? C38 H38 0.9500 . ? C39 C40 1.361(18) . ? C39 H39 0.9500 . ? C40 C41 1.368(17) . ? C40 H40 0.9500 . ? C41 C42 1.400(17) . ? C41 H41 0.9500 . ? C42 H42 0.9500 . ? C43 C44 1.397(16) . ? C43 C48 1.422(16) . ? C43 B2 1.645(17) . ? C44 C45 1.390(15) . ? C44 H44 0.9500 . ? C45 C46 1.389(17) . ? C45 H45 0.9500 . ? C46 C47 1.363(17) . ? C46 H46 0.9500 . ? C47 C48 1.372(15) . ? C47 H47 0.9500 . ? C48 H48 0.9500 . ? C49 C50 1.378(16) . ? C49 C54 1.390(16) . ? C49 B2 1.672(18) . ? C50 C51 1.375(16) . ? C50 H50 0.9500 . ? C51 C52 1.390(18) . ? C51 H51 0.9500 . ? C52 C53 1.363(17) . ? C52 H52 0.9500 . ? C53 C54 1.391(16) . ? C53 H53 0.9500 . ? C54 H54 0.9500 . ? C55 C56 1.476(17) . ? C55 C57 1.505(19) . ? C56 H56A 0.9800 . ? C56 H56B 0.9800 . ? C56 H56C 0.9800 . ? C57 H57A 0.9800 . ? C57 H57B 0.9800 . ? C57 H57C 0.9800 . ? C58 C59 1.46(2) . ? C58 C60 1.52(2) . ? C59 H59A 0.9800 . ? C59 H59B 0.9800 . ? C59 H59C 0.9800 . ? C60 H60A 0.9800 . ? C60 H60B 0.9800 . ? C60 H60C 0.9800 . ? C61 C62 1.47(2) . ? C61 C63 1.47(2) . ? C62 H62A 0.9800 . ? C62 H62B 0.9800 . ? C62 H62C 0.9800 . ? C63 H63A 0.9800 . ? C63 H63B 0.9800 . ? C63 H63C 0.9800 . ? C64 C65 1.519(16) . ? C64 C66 1.525(18) . ? C65 H65A 0.9800 . ? C65 H65B 0.9800 . ? C65 H65C 0.9800 . ? C66 H66A 0.9800 . ? C66 H66B 0.9800 . ? C66 H66C 0.9800 . ? Pt1B N4B 2.015(9) . ? Pt1B N3B 2.035(9) . ? Pt1B N1B 2.072(10) . ? Pt1B N2B 2.085(9) . ? N1B H1B1 0.9100 . ? N1B H1B2 0.9100 . ? N1B H1B3 0.9100 . ? N2B H2B1 0.9100 . ? N2B H2B2 0.9100 . ? N2B H2B3 0.9100 . ? N3B C1B 1.267(13) . ? N3B H3B4 0.8800 . ? N4B C4B 1.303(13) . ? N4B H4B 0.8800 . ? N5B C1B 1.323(14) . ? N5B H5B1 0.8800 . ? N5B H5B2 0.8800 . ? N6B C1B 1.398(14) . ? N6B C2B 1.408(14) . ? N6B C3B 1.445(14) . ? N7B C4B 1.359(14) . ? N7B H7B1 0.8800 . ? N7B H7B2 0.8800 . ? N8B C4B 1.360(15) . ? N8B C6B 1.457(14) . ? N8B C5B 1.464(13) . ? C2B H2D1 0.9800 . ? C2B H2D2 0.9800 . ? C2B H2D3 0.9800 . ? C3B H3B1 0.9800 . ? C3B H3B2 0.9800 . ? C3B H3B3 0.9800 . ? C5B H5D1 0.9800 . ? C5B H5D2 0.9800 . ? C5B H5D3 0.9800 . ? C6B H6D1 0.9800 . ? C6B H6D2 0.9800 . ? C6B H6D3 0.9800 . ? C7B C8B 1.379(16) . ? C7B C12B 1.420(16) . ? C7B B1B 1.658(19) . ? C8B C9B 1.414(16) . ? C8B H8B 0.9500 . ? C9B C10B 1.396(18) . ? C9B H9B 0.9500 . ? C10B C11B 1.371(17) . ? C10B H10B 0.9500 . ? C11B C12B 1.382(16) . ? C11B H11B 0.9500 . ? C12B H12B 0.9500 . ? C13B C14B 1.381(15) . ? C13B C18B 1.426(16) . ? C13B B1B 1.623(18) . ? C14B C15B 1.412(16) . ? C14B H14B 0.9500 . ? C15B C16B 1.396(19) . ? C15B H15B 0.9500 . ? C16B C17B 1.396(19) . ? C16B H16B 0.9500 . ? C17B C18B 1.392(17) . ? C17B H17B 0.9500 . ? C18B H18B 0.9500 . ? C19B C24B 1.385(16) . ? C19B C20B 1.390(15) . ? C19B B1B 1.639(19) . ? C20B C21B 1.407(17) . ? C20B H20B 0.9500 . ? C21B C22B 1.398(18) . ? C21B H21B 0.9500 . ? C22B C23B 1.372(18) . ? C22B H22B 0.9500 . ? C23B C24B 1.390(18) . ? C23B H23B 0.9500 . ? C24B H24B 0.9500 . ? C25B C30B 1.397(16) . ? C25B C26B 1.404(16) . ? C25B B1B 1.663(17) . ? C26B C27B 1.379(15) . ? C26B H26B 0.9500 . ? C27B C28B 1.411(18) . ? C27B H27B 0.9500 . ? C28B C29B 1.377(17) . ? C28B H28B 0.9500 . ? C29B C30B 1.361(15) . ? C29B H29B 0.9500 . ? C30B H30B 0.9500 . ? C31B C36B 1.394(15) . ? C31B C32B 1.400(16) . ? C31B B2B 1.644(16) . ? C32B C33B 1.387(15) . ? C32B H32B 0.9500 . ? C33B C34B 1.374(16) . ? C33B H33B 0.9500 . ? C34B C35B 1.381(17) . ? C34B H34B 0.9500 . ? C35B C36B 1.404(15) . ? C35B H35B 0.9500 . ? C36B H36B 0.9500 . ? C37B C38B 1.385(15) . ? C37B C42B 1.418(15) . ? C37B B2B 1.650(17) . ? C38B C39B 1.387(16) . ? C38B H38B 0.9500 . ? C39B C40B 1.394(16) . ? C39B H39B 0.9500 . ? C40B C41B 1.388(17) . ? C40B H40B 0.9500 . ? C41B C42B 1.403(16) . ? C41B H41B 0.9500 . ? C42B H42B 0.9500 . ? C43B C48B 1.354(16) . ? C43B C44B 1.363(15) . ? C43B B2B 1.664(19) . ? C44B C45B 1.415(16) . ? C44B H44B 0.9500 . ? C45B C46B 1.359(16) . ? C45B H45B 0.9500 . ? C46B C47B 1.418(18) . ? C46B H46B 0.9500 . ? C47B C48B 1.426(17) . ? C47B H47B 0.9500 . ? C48B H48B 0.9500 . ? C49B C54B 1.403(15) . ? C49B C50B 1.403(16) . ? C49B B2B 1.646(17) . ? C50B C51B 1.373(17) . ? C50B H50B 0.9500 . ? C51B C52B 1.358(18) . ? C51B H51B 0.9500 . ? C52B C53B 1.387(18) . ? C52B H52B 0.9500 . ? C53B C54B 1.407(16) . ? C53B H53B 0.9500 . ? C54B H54B 0.9500 . ? 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 N4 Pt1 N3 92.6(4) . . ? N4 Pt1 N1 177.4(4) . . ? N3 Pt1 N1 89.0(4) . . ? N4 Pt1 N2 88.4(4) . . ? N3 Pt1 N2 176.2(4) . . ? N1 Pt1 N2 90.1(4) . . ? Pt1 N1 H1A 109.5 . . ? Pt1 N1 H1B 109.5 . . ? H1A N1 H1B 109.5 . . ? Pt1 N1 H1C 109.5 . . ? H1A N1 H1C 109.5 . . ? H1B N1 H1C 109.5 . . ? Pt1 N2 H2A 109.5 . . ? Pt1 N2 H2B 109.5 . . ? H2A N2 H2B 109.5 . . ? Pt1 N2 H2C 109.5 . . ? H2A N2 H2C 109.5 . . ? H2B N2 H2C 109.5 . . ? C1 N3 Pt1 128.0(8) . . ? C1 N3 H3 116.0 . . ? Pt1 N3 H3 116.0 . . ? C4 N4 Pt1 128.1(8) . . ? C4 N4 H4 115.9 . . ? Pt1 N4 H4 115.9 . . ? C1 N5 H5A 120.0 . . ? C1 N5 H5B 120.0 . . ? H5A N5 H5B 120.0 . . ? C1 N6 C2 123.7(11) . . ? C1 N6 C3 120.5(10) . . ? C2 N6 C3 115.8(10) . . ? C4 N7 H7A 120.0 . . ? C4 N7 H7B 120.0 . . ? H7A N7 H7B 120.0 . . ? C4 N8 C6 116.6(11) . . ? C4 N8 C5 123.4(11) . . ? C6 N8 C5 119.5(11) . . ? N3 C1 N5 120.1(11) . . ? N3 C1 N6 122.3(11) . . ? N5 C1 N6 117.6(12) . . ? N6 C2 H2D 109.5 . . ? N6 C2 H2E 109.5 . . ? H2D C2 H2E 109.5 . . ? N6 C2 H2F 109.5 . . ? H2D C2 H2F 109.5 . . ? H2E C2 H2F 109.5 . . ? N6 C3 H3A 109.5 . . ? N6 C3 H3B 109.5 . . ? H3A C3 H3B 109.5 . . ? N6 C3 H3C 109.5 . . ? H3A C3 H3C 109.5 . . ? H3B C3 H3C 109.5 . . ? N4 C4 N7 119.1(12) . . ? N4 C4 N8 124.1(12) . . ? N7 C4 N8 116.8(12) . . ? N8 C5 H5D 109.5 . . ? N8 C5 H5E 109.5 . . ? H5D C5 H5E 109.5 . . ? N8 C5 H5F 109.5 . . ? H5D C5 H5F 109.5 . . ? H5E C5 H5F 109.5 . . ? N8 C6 H6A 109.5 . . ? N8 C6 H6B 109.5 . . ? H6A C6 H6B 109.5 . . ? N8 C6 H6C 109.5 . . ? H6A C6 H6C 109.5 . . ? H6B C6 H6C 109.5 . . ? C8 C7 C12 115.2(11) . . ? C8 C7 B1 124.5(11) . . ? C12 C7 B1 119.9(10) . . ? C9 C8 C7 124.2(13) . . ? C9 C8 H8 117.9 . . ? C7 C8 H8 117.9 . . ? C10 C9 C8 118.5(13) . . ? C10 C9 H9 120.7 . . ? C8 C9 H9 120.7 . . ? C11 C10 C9 120.3(14) . . ? C11 C10 H10 119.9 . . ? C9 C10 H10 119.9 . . ? C10 C11 C12 120.4(13) . . ? C10 C11 H11 119.8 . . ? C12 C11 H11 119.8 . . ? C11 C12 C7 121.4(12) . . ? C11 C12 H12 119.3 . . ? C7 C12 H12 119.3 . . ? C18 C13 C14 113.1(10) . . ? C18 C13 B1 124.0(10) . . ? C14 C13 B1 122.3(10) . . ? C15 C14 C13 123.3(11) . . ? C15 C14 H14 118.4 . . ? C13 C14 H14 118.4 . . ? C14 C15 C16 119.9(12) . . ? C14 C15 H15 120.0 . . ? C16 C15 H15 120.0 . . ? C17 C16 C15 119.2(12) . . ? C17 C16 H16 120.4 . . ? C15 C16 H16 120.4 . . ? C16 C17 C18 120.4(11) . . ? C16 C17 H17 119.8 . . ? C18 C17 H17 119.8 . . ? C17 C18 C13 123.8(11) . . ? C17 C18 H18 118.1 . . ? C13 C18 H18 118.1 . . ? C24 C19 C20 115.0(11) . . ? C24 C19 B1 124.2(11) . . ? C20 C19 B1 120.5(10) . . ? C21 C20 C19 123.5(11) . . ? C21 C20 H20 118.3 . . ? C19 C20 H20 118.3 . . ? C22 C21 C20 119.1(11) . . ? C22 C21 H21 120.4 . . ? C20 C21 H21 120.4 . . ? C23 C22 C21 119.3(12) . . ? C23 C22 H22 120.3 . . ? C21 C22 H22 120.3 . . ? C22 C23 C24 121.2(12) . . ? C22 C23 H23 119.4 . . ? C24 C23 H23 119.4 . . ? C19 C24 C23 121.8(11) . . ? C19 C24 H24 119.1 . . ? C23 C24 H24 119.1 . . ? C30 C25 C26 114.6(10) . . ? C30 C25 B1 123.8(11) . . ? C26 C25 B1 121.4(10) . . ? C25 C26 C27 122.8(11) . . ? C25 C26 H26 118.6 . . ? C27 C26 H26 118.6 . . ? C28 C27 C26 119.3(13) . . ? C28 C27 H27 120.4 . . ? C26 C27 H27 120.4 . . ? C27 C28 C29 121.1(12) . . ? C27 C28 H28 119.5 . . ? C29 C28 H28 119.5 . . ? C28 C29 C30 117.4(11) . . ? C28 C29 H29 121.3 . . ? C30 C29 H29 121.3 . . ? C25 C30 C29 124.9(12) . . ? C25 C30 H30 117.6 . . ? C29 C30 H30 117.6 . . ? C36 C31 C32 114.6(12) . . ? C36 C31 B2 124.9(11) . . ? C32 C31 B2 120.3(12) . . ? C33 C32 C31 121.4(13) . . ? C33 C32 H32 119.3 . . ? C31 C32 H32 119.3 . . ? C34 C33 C32 121.2(13) . . ? C34 C33 H33 119.4 . . ? C32 C33 H33 119.4 . . ? C33 C34 C35 118.8(13) . . ? C33 C34 H34 120.6 . . ? C35 C34 H34 120.6 . . ? C36 C35 C34 118.6(14) . . ? C36 C35 H35 120.7 . . ? C34 C35 H35 120.7 . . ? C35 C36 C31 125.4(13) . . ? C35 C36 H36 117.3 . . ? C31 C36 H36 117.3 . . ? C42 C37 C38 112.9(11) . . ? C42 C37 B2 123.4(11) . . ? C38 C37 B2 123.4(11) . . ? C37 C38 C39 123.4(13) . . ? C37 C38 H38 118.3 . . ? C39 C38 H38 118.3 . . ? C40 C39 C38 120.1(13) . . ? C40 C39 H39 119.9 . . ? C38 C39 H39 119.9 . . ? C39 C40 C41 119.2(13) . . ? C39 C40 H40 120.4 . . ? C41 C40 H40 120.4 . . ? C40 C41 C42 120.1(13) . . ? C40 C41 H41 120.0 . . ? C42 C41 H41 120.0 . . ? C37 C42 C41 124.3(12) . . ? C37 C42 H42 117.9 . . ? C41 C42 H42 117.9 . . ? C44 C43 C48 114.0(10) . . ? C44 C43 B2 122.5(11) . . ? C48 C43 B2 122.8(11) . . ? C45 C44 C43 123.5(11) . . ? C45 C44 H44 118.2 . . ? C43 C44 H44 118.2 . . ? C46 C45 C44 119.5(12) . . ? C46 C45 H45 120.3 . . ? C44 C45 H45 120.3 . . ? C47 C46 C45 119.2(12) . . ? C47 C46 H46 120.4 . . ? C45 C46 H46 120.4 . . ? C46 C47 C48 120.9(12) . . ? C46 C47 H47 119.5 . . ? C48 C47 H47 119.5 . . ? C47 C48 C43 122.8(12) . . ? C47 C48 H48 118.6 . . ? C43 C48 H48 118.6 . . ? C50 C49 C54 115.4(11) . . ? C50 C49 B2 123.2(11) . . ? C54 C49 B2 121.0(11) . . ? C51 C50 C49 122.5(13) . . ? C51 C50 H50 118.7 . . ? C49 C50 H50 118.7 . . ? C50 C51 C52 121.4(13) . . ? C50 C51 H51 119.3 . . ? C52 C51 H51 119.3 . . ? C53 C52 C51 117.2(12) . . ? C53 C52 H52 121.4 . . ? C51 C52 H52 121.4 . . ? C52 C53 C54 121.0(13) . . ? C52 C53 H53 119.5 . . ? C54 C53 H53 119.5 . . ? C49 C54 C53 122.5(12) . . ? C49 C54 H54 118.8 . . ? C53 C54 H54 118.8 . . ? O1 C55 C56 124.7(14) . . ? O1 C55 C57 119.9(13) . . ? C56 C55 C57 115.3(12) . . ? C55 C56 H56A 109.5 . . ? C55 C56 H56B 109.5 . . ? H56A C56 H56B 109.5 . . ? C55 C56 H56C 109.5 . . ? H56A C56 H56C 109.5 . . ? H56B C56 H56C 109.5 . . ? C55 C57 H57A 109.5 . . ? C55 C57 H57B 109.5 . . ? H57A C57 H57B 109.5 . . ? C55 C57 H57C 109.5 . . ? H57A C57 H57C 109.5 . . ? H57B C57 H57C 109.5 . . ? O2 C58 C59 120.8(15) . . ? O2 C58 C60 122.3(16) . . ? C59 C58 C60 116.8(14) . . ? C58 C59 H59A 109.5 . . ? C58 C59 H59B 109.5 . . ? H59A C59 H59B 109.5 . . ? C58 C59 H59C 109.5 . . ? H59A C59 H59C 109.5 . . ? H59B C59 H59C 109.5 . . ? C58 C60 H60A 109.5 . . ? C58 C60 H60B 109.5 . . ? H60A C60 H60B 109.5 . . ? C58 C60 H60C 109.5 . . ? H60A C60 H60C 109.5 . . ? H60B C60 H60C 109.5 . . ? O3 C61 C62 122.3(14) . . ? O3 C61 C63 122.4(16) . . ? C62 C61 C63 115.1(15) . . ? C61 C62 H62A 109.5 . . ? C61 C62 H62B 109.5 . . ? H62A C62 H62B 109.5 . . ? C61 C62 H62C 109.5 . . ? H62A C62 H62C 109.5 . . ? H62B C62 H62C 109.5 . . ? C61 C63 H63A 109.5 . . ? C61 C63 H63B 109.5 . . ? H63A C63 H63B 109.5 . . ? C61 C63 H63C 109.5 . . ? H63A C63 H63C 109.5 . . ? H63B C63 H63C 109.5 . . ? O4 C64 C65 122.7(12) . . ? O4 C64 C66 121.6(12) . . ? C65 C64 C66 115.7(11) . . ? C64 C65 H65A 109.5 . . ? C64 C65 H65B 109.5 . . ? H65A C65 H65B 109.5 . . ? C64 C65 H65C 109.5 . . ? H65A C65 H65C 109.5 . . ? H65B C65 H65C 109.5 . . ? C64 C66 H66A 109.5 . . ? C64 C66 H66B 109.5 . . ? H66A C66 H66B 109.5 . . ? C64 C66 H66C 109.5 . . ? H66A C66 H66C 109.5 . . ? H66B C66 H66C 109.5 . . ? C13 B1 C7 105.1(10) . . ? C13 B1 C25 112.8(10) . . ? C7 B1 C25 113.6(9) . . ? C13 B1 C19 112.9(9) . . ? C7 B1 C19 111.2(10) . . ? C25 B1 C19 101.6(9) . . ? C37 B2 C31 105.2(9) . . ? C37 B2 C43 110.2(10) . . ? C31 B2 C43 113.4(10) . . ? C37 B2 C49 112.6(10) . . ? C31 B2 C49 113.5(10) . . ? C43 B2 C49 102.1(9) . . ? N4B Pt1B N3B 92.1(4) . . ? N4B Pt1B N1B 176.3(4) . . ? N3B Pt1B N1B 89.2(4) . . ? N4B Pt1B N2B 90.1(4) . . ? N3B Pt1B N2B 176.6(4) . . ? N1B Pt1B N2B 88.8(4) . . ? Pt1B N1B H1B1 109.5 . . ? Pt1B N1B H1B2 109.5 . . ? H1B1 N1B H1B2 109.5 . . ? Pt1B N1B H1B3 109.5 . . ? H1B1 N1B H1B3 109.5 . . ? H1B2 N1B H1B3 109.5 . . ? Pt1B N2B H2B1 109.5 . . ? Pt1B N2B H2B2 109.5 . . ? H2B1 N2B H2B2 109.5 . . ? Pt1B N2B H2B3 109.5 . . ? H2B1 N2B H2B3 109.5 . . ? H2B2 N2B H2B3 109.5 . . ? C1B N3B Pt1B 126.1(8) . . ? C1B N3B H3B4 117.0 . . ? Pt1B N3B H3B4 117.0 . . ? C4B N4B Pt1B 128.7(9) . . ? C4B N4B H4B 115.6 . . ? Pt1B N4B H4B 115.6 . . ? C1B N5B H5B1 120.0 . . ? C1B N5B H5B2 120.0 . . ? H5B1 N5B H5B2 120.0 . . ? C1B N6B C2B 121.9(10) . . ? C1B N6B C3B 116.2(9) . . ? C2B N6B C3B 121.4(10) . . ? C4B N7B H7B1 120.0 . . ? C4B N7B H7B2 120.0 . . ? H7B1 N7B H7B2 120.0 . . ? C4B N8B C6B 120.6(9) . . ? C4B N8B C5B 122.3(10) . . ? C6B N8B C5B 117.0(10) . . ? N3B C1B N5B 119.7(11) . . ? N3B C1B N6B 122.5(10) . . ? N5B C1B N6B 117.7(10) . . ? N6B C2B H2D1 109.5 . . ? N6B C2B H2D2 109.5 . . ? H2D1 C2B H2D2 109.5 . . ? N6B C2B H2D3 109.5 . . ? H2D1 C2B H2D3 109.5 . . ? H2D2 C2B H2D3 109.5 . . ? N6B C3B H3B1 109.5 . . ? N6B C3B H3B2 109.5 . . ? H3B1 C3B H3B2 109.5 . . ? N6B C3B H3B3 109.5 . . ? H3B1 C3B H3B3 109.5 . . ? H3B2 C3B H3B3 109.5 . . ? N4B C4B N7B 116.9(11) . . ? N4B C4B N8B 123.5(11) . . ? N7B C4B N8B 119.6(10) . . ? N8B C5B H5D1 109.5 . . ? N8B C5B H5D2 109.5 . . ? H5D1 C5B H5D2 109.5 . . ? N8B C5B H5D3 109.5 . . ? H5D1 C5B H5D3 109.5 . . ? H5D2 C5B H5D3 109.5 . . ? N8B C6B H6D1 109.5 . . ? N8B C6B H6D2 109.5 . . ? H6D1 C6B H6D2 109.5 . . ? N8B C6B H6D3 109.5 . . ? H6D1 C6B H6D3 109.5 . . ? H6D2 C6B H6D3 109.5 . . ? C8B C7B C12B 116.7(11) . . ? C8B C7B B1B 121.2(11) . . ? C12B C7B B1B 121.7(11) . . ? C7B C8B C9B 122.1(12) . . ? C7B C8B H8B 118.9 . . ? C9B C8B H8B 118.9 . . ? C10B C9B C8B 119.1(12) . . ? C10B C9B H9B 120.5 . . ? C8B C9B H9B 120.5 . . ? C11B C10B C9B 119.8(13) . . ? C11B C10B H10B 120.1 . . ? C9B C10B H10B 120.1 . . ? C10B C11B C12B 120.7(13) . . ? C10B C11B H11B 119.7 . . ? C12B C11B H11B 119.7 . . ? C11B C12B C7B 121.7(11) . . ? C11B C12B H12B 119.2 . . ? C7B C12B H12B 119.2 . . ? C14B C13B C18B 115.2(12) . . ? C14B C13B B1B 124.5(11) . . ? C18B C13B B1B 120.1(11) . . ? C13B C14B C15B 124.3(13) . . ? C13B C14B H14B 117.9 . . ? C15B C14B H14B 117.9 . . ? C16B C15B C14B 117.6(13) . . ? C16B C15B H15B 121.2 . . ? C14B C15B H15B 121.2 . . ? C17B C16B C15B 121.2(13) . . ? C17B C16B H16B 119.4 . . ? C15B C16B H16B 119.4 . . ? C18B C17B C16B 118.6(13) . . ? C18B C17B H17B 120.7 . . ? C16B C17B H17B 120.7 . . ? C17B C18B C13B 123.0(12) . . ? C17B C18B H18B 118.5 . . ? C13B C18B H18B 118.5 . . ? C24B C19B C20B 115.4(12) . . ? C24B C19B B1B 123.3(11) . . ? C20B C19B B1B 120.8(11) . . ? C19B C20B C21B 122.6(12) . . ? C19B C20B H20B 118.7 . . ? C21B C20B H20B 118.7 . . ? C22B C21B C20B 119.7(12) . . ? C22B C21B H21B 120.1 . . ? C20B C21B H21B 120.1 . . ? C23B C22B C21B 118.0(14) . . ? C23B C22B H22B 121.0 . . ? C21B C22B H22B 121.0 . . ? C22B C23B C24B 121.0(14) . . ? C22B C23B H23B 119.5 . . ? C24B C23B H23B 119.5 . . ? C19B C24B C23B 123.0(12) . . ? C19B C24B H24B 118.5 . . ? C23B C24B H24B 118.5 . . ? C30B C25B C26B 114.7(11) . . ? C30B C25B B1B 123.0(11) . . ? C26B C25B B1B 121.8(11) . . ? C27B C26B C25B 122.3(12) . . ? C27B C26B H26B 118.8 . . ? C25B C26B H26B 118.8 . . ? C26B C27B C28B 120.7(12) . . ? C26B C27B H27B 119.6 . . ? C28B C27B H27B 119.6 . . ? C29B C28B C27B 117.2(11) . . ? C29B C28B H28B 121.4 . . ? C27B C28B H28B 121.4 . . ? C30B C29B C28B 121.2(12) . . ? C30B C29B H29B 119.4 . . ? C28B C29B H29B 119.4 . . ? C29B C30B C25B 123.8(12) . . ? C29B C30B H30B 118.1 . . ? C25B C30B H30B 118.1 . . ? C36B C31B C32B 116.3(10) . . ? C36B C31B B2B 122.4(10) . . ? C32B C31B B2B 120.8(10) . . ? C33B C32B C31B 120.7(11) . . ? C33B C32B H32B 119.7 . . ? C31B C32B H32B 119.7 . . ? C34B C33B C32B 122.5(11) . . ? C34B C33B H33B 118.8 . . ? C32B C33B H33B 118.8 . . ? C33B C34B C35B 118.1(11) . . ? C33B C34B H34B 120.9 . . ? C35B C34B H34B 120.9 . . ? C34B C35B C36B 119.8(12) . . ? C34B C35B H35B 120.1 . . ? C36B C35B H35B 120.1 . . ? C31B C36B C35B 122.5(11) . . ? C31B C36B H36B 118.7 . . ? C35B C36B H36B 118.7 . . ? C38B C37B C42B 116.0(11) . . ? C38B C37B B2B 123.4(10) . . ? C42B C37B B2B 120.2(10) . . ? C37B C38B C39B 123.3(11) . . ? C37B C38B H38B 118.4 . . ? C39B C38B H38B 118.4 . . ? C38B C39B C40B 120.0(12) . . ? C38B C39B H39B 120.0 . . ? C40B C39B H39B 120.0 . . ? C41B C40B C39B 118.6(12) . . ? C41B C40B H40B 120.7 . . ? C39B C40B H40B 120.7 . . ? C40B C41B C42B 120.5(12) . . ? C40B C41B H41B 119.7 . . ? C42B C41B H41B 119.7 . . ? C41B C42B C37B 121.4(11) . . ? C41B C42B H42B 119.3 . . ? C37B C42B H42B 119.3 . . ? C48B C43B C44B 117.2(12) . . ? C48B C43B B2B 119.9(11) . . ? C44B C43B B2B 122.7(11) . . ? C43B C44B C45B 123.4(12) . . ? C43B C44B H44B 118.3 . . ? C45B C44B H44B 118.3 . . ? C46B C45B C44B 119.5(12) . . ? C46B C45B H45B 120.2 . . ? C44B C45B H45B 120.2 . . ? C45B C46B C47B 118.6(12) . . ? C45B C46B H46B 120.7 . . ? C47B C46B H46B 120.7 . . ? C46B C47B C48B 119.1(12) . . ? C46B C47B H47B 120.5 . . ? C48B C47B H47B 120.5 . . ? C43B C48B C47B 122.2(12) . . ? C43B C48B H48B 118.9 . . ? C47B C48B H48B 118.9 . . ? C54B C49B C50B 116.0(11) . . ? C54B C49B B2B 119.6(10) . . ? C50B C49B B2B 124.0(11) . . ? C51B C50B C49B 123.2(12) . . ? C51B C50B H50B 118.4 . . ? C49B C50B H50B 118.4 . . ? C52B C51B C50B 119.8(13) . . ? C52B C51B H51B 120.1 . . ? C50B C51B H51B 120.1 . . ? C51B C52B C53B 120.1(13) . . ? C51B C52B H52B 119.9 . . ? C53B C52B H52B 119.9 . . ? C52B C53B C54B 120.1(13) . . ? C52B C53B H53B 120.0 . . ? C54B C53B H53B 120.0 . . ? C49B C54B C53B 120.6(11) . . ? C49B C54B H54B 119.7 . . ? C53B C54B H54B 119.7 . . ? C13B B1B C19B 104.6(10) . . ? C13B B1B C7B 114.3(11) . . ? C19B B1B C7B 110.4(10) . . ? C13B B1B C25B 113.2(10) . . ? C19B B1B C25B 112.3(10) . . ? C7B B1B C25B 102.3(10) . . ? C31B B2B C49B 111.7(9) . . ? C31B B2B C37B 114.0(9) . . ? C49B B2B C37B 102.5(9) . . ? C31B B2B C43B 103.9(9) . . ? C49B B2B C43B 113.9(10) . . ? C37B B2B C43B 111.2(10) . . ? loop_ _geom_hbond_atom_site_label_D _geom_hbond_atom_site_label_H _geom_hbond_atom_site_label_A _geom_hbond_distance_DH _geom_hbond_distance_HA _geom_hbond_distance_DA _geom_hbond_angle_DHA _geom_hbond_site_symmetry_A _geom_hbond_publ_flag N5 H5B O4 0.88 2.06 2.896(13) 158.8 1_545 yes N7 H7B O2 0.88 2.08 2.865(15) 147.3 1_655 yes N5B H5B2 O3 0.88 2.11 2.879(13) 145.2 . yes N7B H7B2 O1 0.88 2.04 2.869(12) 156.7 1_655 yes _diffrn_measured_fraction_theta_max 0.847 _diffrn_reflns_theta_full 25.00 _diffrn_measured_fraction_theta_full 0.848 _refine_diff_density_max 1.295 _refine_diff_density_min -1.174 _refine_diff_density_rms 0.140 #===END======================================================================== data_cis_7 _database_code_depnum_ccdc_archive 'CCDC 686033' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety 'C6 H22 N6 Pt, 2(C6 H2 N3 O7)' _chemical_formula_sum 'C18 H26 N12 O14 Pt' _chemical_formula_weight 829.60 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' Pt Pt -1.7033 8.3905 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting orthorhombic _symmetry_space_group_name_H-M 'P b c n' _symmetry_space_group_name_Hall '-P 2n 2ab' loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x+1/2, -y+1/2, z+1/2' 'x+1/2, -y+1/2, -z' '-x, y, -z+1/2' '-x, -y, -z' 'x-1/2, y-1/2, -z-1/2' '-x-1/2, y-1/2, z' 'x, -y, z-1/2' _cell_length_a 15.4875(2) _cell_length_b 13.1388(2) _cell_length_c 27.7590(5) _cell_angle_alpha 90.00 _cell_angle_beta 90.00 _cell_angle_gamma 90.00 _cell_volume 5648.60(15) _cell_formula_units_Z 8 _cell_measurement_temperature 120(2) _cell_measurement_reflns_used 7025 _cell_measurement_theta_min 2.91 _cell_measurement_theta_max 27.48 _exptl_crystal_description block _exptl_crystal_colour yellow _exptl_crystal_size_max 0.12 _exptl_crystal_size_mid 0.09 _exptl_crystal_size_min 0.08 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.951 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 3264 _exptl_absorpt_coefficient_mu 5.058 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.5750 _exptl_absorpt_correction_T_max 0.6653 _exptl_absorpt_process_details 'Xprep in Shelxtl v.6.14-1 (Sheldrick, 2005)' _publ_section_exptl_refinement ; Oxygens in three of the NO~2~ groups (N10, N11, N12)were disordered over two sites. The NH~2~ and NH hydrogens were located from the difference Fourier map but constrained to ride on their parent atom, with U~iso~ = 1.5 U~eq~(parent atom). Other hydrogens were positioned geometrically and were also constrained to ride on their parent atoms, with N---H = 0.91 \%A, C---H =0.95-0.99 \%A, and U~iso~ = 1.2-1.5 U~eq~(parent atom). ; _exptl_special_details ; ? ; _diffrn_ambient_temperature 120(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator 'horizontally mounted graphite crystal' _diffrn_measurement_device_type 'Nonius KappaCCD' _diffrn_measurement_device '95mm CCD camera on \k-goniostat' _diffrn_detector_area_resol_mean 9 _diffrn_measurement_method '\f scans and \w scans with \k offset' _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 67832 _diffrn_reflns_av_R_equivalents 0.0550 _diffrn_reflns_av_sigmaI/netI 0.0342 _diffrn_reflns_limit_h_min -15 _diffrn_reflns_limit_h_max 20 _diffrn_reflns_limit_k_min -17 _diffrn_reflns_limit_k_max 17 _diffrn_reflns_limit_l_min -36 _diffrn_reflns_limit_l_max 36 _diffrn_reflns_theta_min 3.00 _diffrn_reflns_theta_max 27.59 _reflns_number_total 6468 _reflns_number_gt 4492 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'Collect (Nonius BV, 1997-2000)' _computing_cell_refinement 'Denzo/Scalepack (Otwinowski & Minor, 1997)' _computing_data_reduction 'Denzo/Scalepack (Otwinowski & Minor, 1997)' _computing_structure_solution 'SIR2004 (Burla et al., 2005)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'Diamond v.3.1d (Crystal Impact GbR, 2006)' _computing_publication_material 'SHELXL-97 (Sheldrick, 1997)' _refine_special_details ; Refinement of F^2^ against ALL reflections. The weighted R-factor wR and goodness of fit S are based on F^2^, conventional R-factors R are based on F, with F set to zero for negative F^2^. The threshold expression of F^2^ > 2sigma(F^2^) is used only for calculating R-factors(gt) etc. and is not relevant to the choice of reflections for refinement. R-factors based on F^2^ are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger. ; _refine_ls_structure_factor_coef Fsqd _refine_ls_matrix_type full _refine_ls_weighting_scheme calc _refine_ls_weighting_details 'calc w=1/[\s^2^(Fo^2^)+(0.0276P)^2^+10.6898P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment constr _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 6468 _refine_ls_number_parameters 444 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0583 _refine_ls_R_factor_gt 0.0299 _refine_ls_wR_factor_ref 0.0712 _refine_ls_wR_factor_gt 0.0631 _refine_ls_goodness_of_fit_ref 1.059 _refine_ls_restrained_S_all 1.059 _refine_ls_shift/su_max 0.014 _refine_ls_shift/su_mean 0.000 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 0.209410(9) 0.125306(13) 0.574549(5) 0.02575(6) Uani 1 1 d . . . O1 O 0.70564(17) 0.4339(2) 0.56355(10) 0.0297(7) Uani 1 1 d . . . O2 O 0.8738(2) 0.4113(3) 0.58104(13) 0.0446(8) Uani 1 1 d . . . O3 O 0.9220(2) 0.4746(3) 0.64749(13) 0.0472(9) Uani 1 1 d . . . O4 O 0.7460(3) 0.5255(3) 0.78307(14) 0.0612(12) Uani 1 1 d . . . O5 O 0.6076(2) 0.5382(3) 0.77552(13) 0.0531(9) Uani 1 1 d . . . O6 O 0.47151(19) 0.4775(3) 0.62666(12) 0.0430(8) Uani 1 1 d . . . O7 O 0.5356(2) 0.4022(3) 0.56937(14) 0.0607(11) Uani 1 1 d . . . O8 O 0.70127(18) 0.1468(2) 0.48620(11) 0.0310(7) Uani 1 1 d . A . O9 O 0.8719(5) 0.180(3) 0.4905(3) 0.062(5) Uani 0.82(8) 1 d P A 1 O9B O 0.875(2) 0.128(7) 0.4908(13) 0.037(13) Uani 0.18(8) 1 d P A 2 O10 O 0.9283(2) 0.1420(3) 0.55998(16) 0.0645(12) Uani 1 1 d . A . O11 O 0.784(3) 0.243(5) 0.706(2) 0.041(7) Uani 0.5(3) 1 d P B 3 O11B O 0.799(9) 0.236(4) 0.696(4) 0.054(14) Uani 0.5(3) 1 d P B 4 O12 O 0.6495(3) 0.2430(3) 0.70511(13) 0.0626(12) Uani 1 1 d . B . O13 O 0.4859(2) 0.1401(3) 0.56872(13) 0.0602(11) Uani 1 1 d . C . O15 O 0.5294(3) 0.1887(6) 0.50090(19) 0.046(2) Uani 0.624(11) 1 d P C 5 O15B O 0.5429(6) 0.0893(10) 0.5040(3) 0.055(4) Uani 0.376(11) 1 d P C 6 N1 N 0.1123(2) 0.0846(3) 0.52812(13) 0.0365(9) Uani 1 1 d . . . H1A H 0.0936 0.0208 0.5354 0.055 Uiso 1 1 calc R . . H1B H 0.1325 0.0858 0.4973 0.055 Uiso 1 1 calc R . . H1C H 0.0677 0.1293 0.5310 0.055 Uiso 1 1 calc R . . N2 N 0.3021(2) 0.0800(3) 0.52620(13) 0.0311(8) Uani 1 1 d . . . H2A H 0.3525 0.1128 0.5327 0.047 Uiso 1 1 calc R . . H2B H 0.2846 0.0955 0.4958 0.047 Uiso 1 1 calc R . . H2C H 0.3102 0.0116 0.5287 0.047 Uiso 1 1 calc R . . N3 N 0.3014(2) 0.1583(3) 0.62193(14) 0.0347(9) Uani 1 1 d . . . H3D H 0.3349 0.1051 0.6387 0.052 Uiso 1 1 d R . . N4 N 0.1248(2) 0.1684(3) 0.62509(13) 0.0311(8) Uani 1 1 d . . . H4D H 0.1131 0.1242 0.6504 0.047 Uiso 1 1 d R . . N5 N 0.3104(3) 0.3304(3) 0.60907(16) 0.0477(11) Uani 1 1 d . . . H5D H 0.2782 0.3263 0.5787 0.072 Uiso 1 1 d R . . H5E H 0.3555 0.3777 0.6160 0.072 Uiso 1 1 d R . . N6 N 0.0790(2) 0.3244(3) 0.59706(14) 0.0359(9) Uani 1 1 d . . . H6D H 0.0370 0.3761 0.6028 0.054 Uiso 1 1 d R . . H6E H 0.1161 0.3253 0.5713 0.054 Uiso 1 1 d R . . N7 N 0.8619(2) 0.4472(3) 0.62102(15) 0.0318(8) Uani 1 1 d . . . N8 N 0.6800(3) 0.5213(3) 0.75887(14) 0.0428(10) Uani 1 1 d . . . N9 N 0.5375(2) 0.4505(3) 0.60758(13) 0.0333(9) Uani 1 1 d . . . N10 N 0.8672(2) 0.1675(3) 0.53315(17) 0.0420(10) Uani 1 1 d . . . N11 N 0.7175(4) 0.2323(3) 0.68312(16) 0.0456(11) Uani 1 1 d . . . N12 N 0.5451(3) 0.1554(4) 0.54241(15) 0.0473(11) Uani 1 1 d . . . C1 C 0.3333(3) 0.2459(4) 0.63287(16) 0.0389(12) Uani 1 1 d . . . C2 C 0.3987(4) 0.2558(5) 0.6738(2) 0.0599(16) Uani 1 1 d . . . H2D H 0.4474 0.2984 0.6625 0.072 Uiso 1 1 calc R . . H2E H 0.3708 0.2922 0.7009 0.072 Uiso 1 1 calc R . . C3 C 0.4349(4) 0.1559(5) 0.6926(2) 0.0645(18) Uani 1 1 d . . . H3A H 0.3894 0.1183 0.7095 0.097 Uiso 1 1 calc R . . H3B H 0.4825 0.1698 0.7149 0.097 Uiso 1 1 calc R . . H3C H 0.4562 0.1151 0.6656 0.097 Uiso 1 1 calc R . . C4 C 0.0818(3) 0.2511(3) 0.63077(16) 0.0289(10) Uani 1 1 d . . . C5 C 0.0383(3) 0.2738(4) 0.67819(16) 0.0377(11) Uani 1 1 d . . . H5A H 0.0288 0.2098 0.6962 0.045 Uiso 1 1 calc R . . H5B H -0.0186 0.3060 0.6724 0.045 Uiso 1 1 calc R . . C6 C 0.0954(4) 0.3456(5) 0.70772(19) 0.0578(16) Uani 1 1 d . . . H6A H 0.1510 0.3128 0.7141 0.087 Uiso 1 1 calc R . . H6B H 0.0668 0.3614 0.7383 0.087 Uiso 1 1 calc R . . H6C H 0.1049 0.4087 0.6896 0.087 Uiso 1 1 calc R . . C7 C 0.7007(2) 0.4489(3) 0.60736(15) 0.0247(9) Uani 1 1 d . . . C8 C 0.7739(3) 0.4587(3) 0.63978(16) 0.0264(9) Uani 1 1 d . . . C9 C 0.7673(3) 0.4812(3) 0.68815(17) 0.0296(10) Uani 1 1 d . . . H9 H 0.8178 0.4869 0.7075 0.036 Uiso 1 1 calc R . . C10 C 0.6869(3) 0.4954(3) 0.70821(16) 0.0318(10) Uani 1 1 d . . . C11 C 0.6119(3) 0.4865(3) 0.68122(15) 0.0289(10) Uani 1 1 d . . . H11 H 0.5569 0.4970 0.6955 0.035 Uiso 1 1 calc R . . C12 C 0.6193(3) 0.4623(3) 0.63339(15) 0.0255(9) Uani 1 1 d . . . C13 C 0.7055(3) 0.1659(3) 0.53019(16) 0.0275(9) Uani 1 1 d . . . C14 C 0.7851(3) 0.1806(3) 0.55707(17) 0.0306(10) Uani 1 1 d . A . C15 C 0.7886(3) 0.2015(3) 0.60591(17) 0.0338(10) Uani 1 1 d . . . H15 H 0.8428 0.2092 0.6215 0.041 Uiso 1 1 calc R A . C16 C 0.7140(3) 0.2109(3) 0.63148(16) 0.0342(10) Uani 1 1 d . A . C17 C 0.6343(3) 0.1961(3) 0.60997(16) 0.0342(10) Uani 1 1 d . . . H17 H 0.5827 0.2017 0.6283 0.041 Uiso 1 1 calc R A . C18 C 0.6310(3) 0.1733(3) 0.56191(15) 0.0310(10) Uani 1 1 d . A . 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 0.02732(9) 0.02667(9) 0.02326(9) -0.00160(7) 0.00108(7) -0.00085(7) O1 0.0267(15) 0.0355(18) 0.0268(16) -0.0012(13) -0.0009(12) 0.0016(13) O2 0.0280(16) 0.055(2) 0.051(2) -0.0107(17) 0.0028(16) 0.0016(16) O3 0.0295(17) 0.059(2) 0.053(2) 0.0005(18) -0.0106(16) -0.0063(16) O4 0.062(2) 0.081(3) 0.041(2) -0.020(2) -0.0207(19) 0.010(2) O5 0.057(2) 0.070(3) 0.0323(19) -0.0129(18) 0.0082(18) -0.002(2) O6 0.0260(16) 0.060(2) 0.043(2) -0.0121(17) 0.0032(15) 0.0044(15) O7 0.0371(19) 0.095(3) 0.050(2) -0.019(2) -0.0035(17) 0.000(2) O8 0.0342(16) 0.0316(17) 0.0272(16) -0.0010(12) -0.0006(13) -0.0003(13) O9 0.037(3) 0.105(17) 0.045(4) 0.018(5) 0.013(3) 0.011(5) O9B 0.025(11) 0.04(3) 0.044(13) 0.028(14) -0.020(12) -0.004(13) O10 0.034(2) 0.081(3) 0.079(3) 0.014(2) -0.0038(19) 0.008(2) O11 0.069(12) 0.039(11) 0.014(11) -0.009(7) -0.005(8) 0.002(7) O11B 0.10(3) 0.029(7) 0.03(2) -0.014(11) -0.03(2) 0.009(12) O12 0.100(3) 0.055(3) 0.033(2) -0.0070(18) 0.012(2) -0.020(2) O13 0.0381(19) 0.098(3) 0.045(2) -0.011(2) 0.0126(17) -0.016(2) O15 0.027(3) 0.082(6) 0.029(3) 0.004(3) 0.001(2) 0.002(3) O15B 0.046(6) 0.085(10) 0.033(6) -0.015(5) -0.001(4) -0.013(6) N1 0.0293(19) 0.049(2) 0.031(2) -0.0092(18) 0.0044(16) -0.0047(17) N2 0.0315(19) 0.031(2) 0.031(2) -0.0017(16) 0.0027(16) -0.0003(16) N3 0.035(2) 0.041(2) 0.029(2) -0.0007(17) -0.0066(16) 0.0010(17) N4 0.0335(19) 0.032(2) 0.028(2) 0.0004(16) 0.0038(16) -0.0017(17) N5 0.055(3) 0.046(3) 0.042(3) -0.001(2) -0.009(2) -0.025(2) N6 0.035(2) 0.039(2) 0.034(2) 0.0035(19) 0.0062(17) 0.0074(18) N7 0.0258(18) 0.026(2) 0.044(2) 0.0029(17) -0.0052(17) -0.0011(15) N8 0.057(3) 0.040(2) 0.032(2) -0.0058(18) -0.007(2) -0.002(2) N9 0.031(2) 0.046(2) 0.023(2) -0.0023(17) 0.0004(16) 0.0033(18) N10 0.028(2) 0.041(2) 0.057(3) -0.002(2) -0.006(2) 0.0074(18) N11 0.085(4) 0.020(2) 0.032(2) 0.0024(17) -0.015(3) -0.007(2) N12 0.034(2) 0.081(3) 0.027(2) 0.002(2) 0.0015(19) -0.010(2) C1 0.037(2) 0.058(3) 0.022(2) -0.001(2) 0.000(2) -0.016(2) C2 0.067(4) 0.076(4) 0.037(3) 0.003(3) -0.010(3) -0.024(3) C3 0.050(3) 0.108(5) 0.035(3) 0.003(3) -0.011(3) 0.004(3) C4 0.026(2) 0.034(3) 0.027(2) -0.0025(19) 0.0006(18) -0.0039(19) C5 0.036(2) 0.044(3) 0.033(3) 0.003(2) 0.007(2) 0.004(2) C6 0.055(3) 0.090(5) 0.029(3) -0.016(3) 0.004(2) -0.010(3) C7 0.028(2) 0.017(2) 0.029(2) 0.0012(16) 0.0013(18) -0.0012(17) C8 0.025(2) 0.019(2) 0.035(3) 0.0007(18) -0.0014(18) 0.0009(17) C9 0.034(2) 0.019(2) 0.035(3) 0.0009(19) -0.009(2) 0.0018(18) C10 0.045(3) 0.023(2) 0.027(2) -0.0029(18) -0.005(2) 0.003(2) C11 0.029(2) 0.025(2) 0.032(2) 0.0010(19) 0.0034(19) 0.0012(18) C12 0.025(2) 0.026(2) 0.025(2) 0.0014(17) -0.0017(18) 0.0004(18) C13 0.031(2) 0.021(2) 0.031(2) 0.0044(17) -0.0021(19) 0.0008(18) C14 0.031(2) 0.020(2) 0.041(3) -0.0013(19) -0.003(2) 0.0028(19) C15 0.043(3) 0.017(2) 0.042(3) 0.0022(19) -0.013(2) 0.000(2) C16 0.053(3) 0.020(2) 0.029(2) 0.0028(18) -0.008(2) 0.000(2) C17 0.047(3) 0.024(2) 0.032(2) 0.0068(19) 0.003(2) -0.001(2) C18 0.036(2) 0.029(2) 0.027(2) 0.0053(18) -0.0016(19) -0.004(2) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; 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 N3 1.987(4) . ? Pt1 N4 2.001(3) . ? Pt1 N1 2.052(4) . ? Pt1 N2 2.053(3) . ? O1 C7 1.234(5) . ? O2 N7 1.220(5) . ? O3 N7 1.239(5) . ? O4 N8 1.224(5) . ? O5 N8 1.234(5) . ? O6 N9 1.205(4) . ? O7 N9 1.236(5) . ? O8 C13 1.248(5) . ? O9 N10 1.197(13) . ? O9B N10 1.29(7) . ? O10 N10 1.250(5) . ? O11 N11 1.22(5) . ? O11B N11 1.31(10) . ? O12 N11 1.225(6) . ? O13 N12 1.190(5) . ? O15 N12 1.257(6) . ? O15B N12 1.375(11) . ? N1 H1A 0.9100 . ? N1 H1B 0.9100 . ? N1 H1C 0.9100 . ? N2 H2A 0.9100 . ? N2 H2B 0.9100 . ? N2 H2C 0.9100 . ? N3 C1 1.288(6) . ? N3 H3D 0.9870 . ? N4 C4 1.284(5) . ? N4 H4D 0.9289 . ? N5 C1 1.340(6) . ? N5 H5D 0.9826 . ? N5 H5E 0.9549 . ? N6 C4 1.344(6) . ? N6 H6D 0.9541 . ? N6 H6E 0.9177 . ? N7 C8 1.467(5) . ? N8 C10 1.451(6) . ? N9 C12 1.463(5) . ? N10 C14 1.444(6) . ? N11 C16 1.462(6) . ? N12 C18 1.455(6) . ? C1 C2 1.528(7) . ? C2 C3 1.521(8) . ? C2 H2D 0.9900 . ? C2 H2E 0.9900 . ? C3 H3A 0.9800 . ? C3 H3B 0.9800 . ? C3 H3C 0.9800 . ? C4 C5 1.509(6) . ? C5 C6 1.531(7) . ? C5 H5A 0.9900 . ? C5 H5B 0.9900 . ? C6 H6A 0.9800 . ? C6 H6B 0.9800 . ? C6 H6C 0.9800 . ? C7 C8 1.453(6) . ? C7 C12 1.464(6) . ? C8 C9 1.379(6) . ? C9 C10 1.377(6) . ? C9 H9 0.9500 . ? C10 C11 1.387(6) . ? C11 C12 1.370(6) . ? C11 H11 0.9500 . ? C13 C18 1.454(6) . ? C13 C14 1.455(6) . ? C14 C15 1.384(7) . ? C15 C16 1.362(6) . ? C15 H15 0.9500 . ? C16 C17 1.385(6) . ? C17 C18 1.368(6) . ? C17 H17 0.9500 . ? 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 N3 Pt1 N4 86.77(15) . . ? N3 Pt1 N1 176.78(16) . . ? N4 Pt1 N1 91.95(15) . . ? N3 Pt1 N2 89.69(15) . . ? N4 Pt1 N2 176.25(14) . . ? N1 Pt1 N2 91.52(14) . . ? Pt1 N1 H1A 109.5 . . ? Pt1 N1 H1B 109.5 . . ? H1A N1 H1B 109.5 . . ? Pt1 N1 H1C 109.5 . . ? H1A N1 H1C 109.5 . . ? H1B N1 H1C 109.5 . . ? Pt1 N2 H2A 109.5 . . ? Pt1 N2 H2B 109.5 . . ? H2A N2 H2B 109.5 . . ? Pt1 N2 H2C 109.5 . . ? H2A N2 H2C 109.5 . . ? H2B N2 H2C 109.5 . . ? C1 N3 Pt1 128.7(3) . . ? C1 N3 H3D 108.7 . . ? Pt1 N3 H3D 122.3 . . ? C4 N4 Pt1 131.7(3) . . ? C4 N4 H4D 109.5 . . ? Pt1 N4 H4D 118.8 . . ? C1 N5 H5D 120.8 . . ? C1 N5 H5E 104.4 . . ? H5D N5 H5E 125.5 . . ? C4 N6 H6D 114.6 . . ? C4 N6 H6E 122.1 . . ? H6D N6 H6E 123.2 . . ? O2 N7 O3 122.6(4) . . ? O2 N7 C8 120.1(4) . . ? O3 N7 C8 117.2(4) . . ? O4 N8 O5 123.1(4) . . ? O4 N8 C10 118.8(4) . . ? O5 N8 C10 118.2(4) . . ? O6 N9 O7 120.5(4) . . ? O6 N9 C12 119.2(4) . . ? O7 N9 C12 119.7(4) . . ? O9 N10 O10 125.5(7) . . ? O10 N10 O9B 111(3) . . ? O9 N10 C14 119.4(7) . . ? O10 N10 C14 115.1(4) . . ? O9B N10 C14 123.6(14) . . ? O11 N11 O12 117(3) . . ? O12 N11 O11B 133(6) . . ? O11 N11 C16 125(3) . . ? O12 N11 C16 118.6(5) . . ? O11B N11 C16 108(6) . . ? O13 N12 O15 118.2(5) . . ? O13 N12 O15B 110.5(6) . . ? O15 N12 O15B 60.3(5) . . ? O13 N12 C18 120.2(4) . . ? O15 N12 C18 117.5(4) . . ? O15B N12 C18 114.4(5) . . ? N3 C1 N5 121.5(4) . . ? N3 C1 C2 120.4(5) . . ? N5 C1 C2 118.1(4) . . ? C3 C2 C1 115.2(5) . . ? C3 C2 H2D 108.5 . . ? C1 C2 H2D 108.5 . . ? C3 C2 H2E 108.5 . . ? C1 C2 H2E 108.5 . . ? H2D C2 H2E 107.5 . . ? C2 C3 H3A 109.5 . . ? C2 C3 H3B 109.5 . . ? H3A C3 H3B 109.5 . . ? C2 C3 H3C 109.5 . . ? H3A C3 H3C 109.5 . . ? H3B C3 H3C 109.5 . . ? N4 C4 N6 122.5(4) . . ? N4 C4 C5 120.4(4) . . ? N6 C4 C5 116.8(4) . . ? C4 C5 C6 109.3(4) . . ? C4 C5 H5A 109.8 . . ? C6 C5 H5A 109.8 . . ? C4 C5 H5B 109.8 . . ? C6 C5 H5B 109.8 . . ? H5A C5 H5B 108.3 . . ? C5 C6 H6A 109.5 . . ? C5 C6 H6B 109.5 . . ? H6A C6 H6B 109.5 . . ? C5 C6 H6C 109.5 . . ? H6A C6 H6C 109.5 . . ? H6B C6 H6C 109.5 . . ? O1 C7 C8 125.1(4) . . ? O1 C7 C12 124.0(4) . . ? C8 C7 C12 110.8(4) . . ? C9 C8 C7 124.3(4) . . ? C9 C8 N7 115.9(4) . . ? C7 C8 N7 119.8(4) . . ? C10 C9 C8 119.3(4) . . ? C10 C9 H9 120.3 . . ? C8 C9 H9 120.3 . . ? C9 C10 C11 121.8(4) . . ? C9 C10 N8 119.3(4) . . ? C11 C10 N8 118.8(4) . . ? C12 C11 C10 118.3(4) . . ? C12 C11 H11 120.9 . . ? C10 C11 H11 120.9 . . ? C11 C12 N9 115.3(4) . . ? C11 C12 C7 125.3(4) . . ? N9 C12 C7 119.4(4) . . ? O8 C13 C18 124.4(4) . . ? O8 C13 C14 124.9(4) . . ? C18 C13 C14 110.7(4) . . ? C15 C14 N10 116.1(4) . . ? C15 C14 C13 124.2(4) . . ? N10 C14 C13 119.7(4) . . ? C16 C15 C14 119.7(4) . . ? C16 C15 H15 120.1 . . ? C14 C15 H15 120.1 . . ? C15 C16 C17 121.3(4) . . ? C15 C16 N11 119.8(4) . . ? C17 C16 N11 118.9(4) . . ? C18 C17 C16 118.9(4) . . ? C18 C17 H17 120.5 . . ? C16 C17 H17 120.5 . . ? C17 C18 C13 125.2(4) . . ? C17 C18 N12 115.6(4) . . ? C13 C18 N12 119.3(4) . . ? loop_ _geom_hbond_atom_site_label_D _geom_hbond_atom_site_label_H _geom_hbond_atom_site_label_A _geom_hbond_distance_DH _geom_hbond_distance_HA _geom_hbond_distance_DA _geom_hbond_angle_DHA _geom_hbond_site_symmetry_A N1 H1A O9B 0.91 2.14 2.85(10) 134.0 5_656 N1 H1B O1 0.91 2.05 2.937(5) 164.1 3_456 N1 H1B O7 0.91 2.39 2.960(5) 120.9 3_456 N1 H1C O10 0.91 2.31 3.077(5) 141.9 1_455 N1 H1C O15 0.91 2.62 3.341(8) 137.0 3_456 N2 H2A O13 0.91 2.32 3.182(5) 157.2 . N2 H2B O1 0.91 2.09 2.911(5) 149.9 3_456 N2 H2B O2 0.91 2.54 3.179(5) 127.5 3_456 N2 H2C O8 0.91 2.13 3.000(5) 159.9 5_656 N5 H5E O6 0.95 2.24 3.194(5) 173.3 . N4 H4D O5 0.93 2.35 3.257(5) 165.8 6_557 N4 H4D O6 0.93 2.42 2.918(5) 113.5 7_655 N6 H6E O8 0.92 2.10 3.011(5) 170.7 3_456 N6 H6E O15B 0.92 2.63 3.078(11) 110.8 3_456 N5 H5D O8 0.98 2.19 3.153(5) 167.2 3_456 N5 H5D O9 0.98 2.41 2.927(10) 112.4 3_456 N5 H5D O9B 0.98 2.52 3.00(3) 109.9 3_456 _diffrn_measured_fraction_theta_max 0.987 _diffrn_reflns_theta_full 27.59 _diffrn_measured_fraction_theta_full 0.987 _refine_diff_density_max 1.374 _refine_diff_density_min -0.908 _refine_diff_density_rms 0.109 #===END======================================================================== data_cis_9 _database_code_depnum_ccdc_archive 'CCDC 686034' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety 'C14 H20 N6 Pt, 2(C6 H2 N3 O7)' _chemical_formula_sum 'C26 H24 N12 O14 Pt' _chemical_formula_weight 923.66 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' Pt Pt -1.7033 8.3905 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting monoclinic _symmetry_space_group_name_H-M 'C 2/c' _symmetry_space_group_name_Hall '-C 2yc' loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, y, -z+1/2' 'x+1/2, y+1/2, z' '-x+1/2, y+1/2, -z+1/2' '-x, -y, -z' 'x, -y, z-1/2' '-x+1/2, -y+1/2, -z' 'x+1/2, -y+1/2, z-1/2' _cell_length_a 22.0651(8) _cell_length_b 7.2725(2) _cell_length_c 22.7185(8) _cell_angle_alpha 90.00 _cell_angle_beta 117.4720(10) _cell_angle_gamma 90.00 _cell_volume 3234.51(19) _cell_formula_units_Z 4 _cell_measurement_temperature 120(2) _cell_measurement_reflns_used 3586 _cell_measurement_theta_min 1.00 _cell_measurement_theta_max 27.48 _exptl_crystal_description block _exptl_crystal_colour yellow _exptl_crystal_size_max 0.18 _exptl_crystal_size_mid 0.10 _exptl_crystal_size_min 0.05 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.897 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1816 _exptl_absorpt_coefficient_mu 4.428 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.5029 _exptl_absorpt_correction_T_max 0.8090 _exptl_absorpt_process_details 'SORTAV (Blessing, 1995)' _publ_section_exptl_refinement ; All hydrogens were positioned geometrically and constrained to ride on their parent atoms, with C---H =0.95 \%A, N---H 0.88-0.91 \%A and with U~iso~ = 1.2-1.5 U~eq~(parent atom). ; _exptl_special_details ; ? ; _diffrn_ambient_temperature 120(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator 'horizontally mounted graphite crystal' _diffrn_measurement_device_type 'Nonius KappaCCD' _diffrn_measurement_device '95mm CCD camera on \k-goniostat' _diffrn_detector_area_resol_mean 9 _diffrn_measurement_method '\f scans and \w scans with \k offset' _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 14957 _diffrn_reflns_av_R_equivalents 0.0901 _diffrn_reflns_av_sigmaI/netI 0.0510 _diffrn_reflns_limit_h_min -24 _diffrn_reflns_limit_h_max 26 _diffrn_reflns_limit_k_min -8 _diffrn_reflns_limit_k_max 8 _diffrn_reflns_limit_l_min -27 _diffrn_reflns_limit_l_max 27 _diffrn_reflns_theta_min 2.99 _diffrn_reflns_theta_max 25.75 _reflns_number_total 3074 _reflns_number_gt 2901 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'Collect (Bruker AXS BV, 1997-2004)' _computing_cell_refinement 'Denzo/Scalepack (Otwinowski & Minor, 1997)' _computing_data_reduction 'Denzo/Scalepack (Otwinowski & Minor, 1997)' _computing_structure_solution 'SIR2004 (Burla et al., 2005)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'Diamond v.3.1d (Brandenburg, 2006)' _computing_publication_material 'SHELXL-97 (Sheldrick, 1997)' _refine_special_details ; Refinement of F^2^ against ALL reflections. The weighted R-factor wR and goodness of fit S are based on F^2^, conventional R-factors R are based on F, with F set to zero for negative F^2^. The threshold expression of F^2^ > 2sigma(F^2^) is used only for calculating R-factors(gt) etc. and is not relevant to the choice of reflections for refinement. R-factors based on F^2^ are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger. ; _refine_ls_structure_factor_coef Fsqd _refine_ls_matrix_type full _refine_ls_weighting_scheme calc _refine_ls_weighting_details 'calc w=1/[\s^2^(Fo^2^)+(0.0363P)^2^+11.2345P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment constr _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 3074 _refine_ls_number_parameters 241 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0346 _refine_ls_R_factor_gt 0.0312 _refine_ls_wR_factor_ref 0.0759 _refine_ls_wR_factor_gt 0.0734 _refine_ls_goodness_of_fit_ref 1.064 _refine_ls_restrained_S_all 1.064 _refine_ls_shift/su_max 0.001 _refine_ls_shift/su_mean 0.000 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 0.5000 0.05707(3) -0.2500 0.01848(10) Uani 1 2 d S . . O1 O 0.57401(15) -0.2609(4) 0.15919(15) 0.0273(7) Uani 1 1 d . . . N1 N 0.54568(17) 0.2583(5) -0.18126(16) 0.0216(7) Uani 1 1 d . . . H1A H 0.5145 0.3100 -0.1706 0.032 Uiso 1 1 calc R . . H1B H 0.5627 0.3459 -0.1982 0.032 Uiso 1 1 calc R . . H1C H 0.5803 0.2089 -0.1442 0.032 Uiso 1 1 calc R . . C1 C 0.5409(2) -0.1765(6) -0.12885(19) 0.0212(8) Uani 1 1 d . . . O2 O 0.56826(16) -0.5462(4) 0.22968(16) 0.0267(7) Uani 1 1 d . . . N2 N 0.54645(17) -0.1397(5) -0.18215(16) 0.0212(7) Uani 1 1 d . . . C2 C 0.5798(2) -0.3349(6) -0.08576(19) 0.0231(9) Uani 1 1 d . . . O3 O 0.65622(18) -0.7244(5) 0.27299(18) 0.0418(9) Uani 1 1 d . . . N3 N 0.5000(2) -0.0833(6) -0.1110(2) 0.0323(9) Uani 1 1 d . . . H3A H 0.4751 0.0080 -0.1358 0.039 Uiso 1 1 calc R . . H3B H 0.4979 -0.1131 -0.0744 0.039 Uiso 1 1 calc R . . C3 C 0.5499(2) -0.4510(6) -0.0578(2) 0.0246(10) Uani 1 1 d . . . H3 H 0.5056 -0.4242 -0.0629 0.030 Uiso 1 1 calc R . . O4 O 0.81029(17) -0.7812(5) 0.18260(17) 0.0353(8) Uani 1 1 d . . . N4 N 0.6310(2) -0.1275(6) 0.0776(2) 0.0319(9) Uani 1 1 d . . . C4 C 0.5844(3) -0.6050(7) -0.0225(2) 0.0283(10) Uani 1 1 d . . . H4 H 0.5632 -0.6849 -0.0044 0.034 Uiso 1 1 calc R . . O5 O 0.81272(17) -0.5739(4) 0.11483(16) 0.0282(7) Uani 1 1 d . . . N5 N 0.62299(19) -0.6018(5) 0.23356(18) 0.0251(8) Uani 1 1 d . . . C5 C 0.6499(2) -0.6432(6) -0.0135(2) 0.0287(10) Uani 1 1 d . . . H5 H 0.6735 -0.7490 0.0107 0.034 Uiso 1 1 calc R . . O6 O 0.6732(2) -0.0264(6) 0.0745(3) 0.0645(14) Uani 1 1 d . . . N6 N 0.78912(18) -0.6377(5) 0.15037(17) 0.0243(8) Uani 1 1 d . . . C6 C 0.6807(2) -0.5255(7) -0.0403(2) 0.0293(10) Uani 1 1 d . . . H6 H 0.7256 -0.5506 -0.0338 0.035 Uiso 1 1 calc R . . O7 O 0.56874(18) -0.1024(5) 0.04626(16) 0.0364(8) Uani 1 1 d . . . C7 C 0.6459(2) -0.3715(6) -0.0764(2) 0.0266(9) Uani 1 1 d . . . H7 H 0.6670 -0.2915 -0.0946 0.032 Uiso 1 1 calc R . . C8 C 0.6205(2) -0.3499(6) 0.1565(2) 0.0224(9) Uani 1 1 d . . . C9 C 0.6494(2) -0.5223(6) 0.1917(2) 0.0212(9) Uani 1 1 d . . . C10 C 0.7035(2) -0.6125(6) 0.1902(2) 0.0230(9) Uani 1 1 d . . . H10 H 0.7203 -0.7232 0.2146 0.028 Uiso 1 1 calc R . . C11 C 0.7334(2) -0.5422(6) 0.1533(2) 0.0223(9) Uani 1 1 d . . . C12 C 0.7096(2) -0.3796(6) 0.1180(2) 0.0232(9) Uani 1 1 d . . . H12 H 0.7310 -0.3293 0.0938 0.028 Uiso 1 1 calc R . . C13 C 0.6551(2) -0.2929(6) 0.1186(2) 0.0223(9) Uani 1 1 d . . . 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 0.01844(14) 0.01662(14) 0.02328(14) 0.000 0.01210(10) 0.000 O1 0.0250(16) 0.0243(16) 0.0401(17) 0.0052(13) 0.0213(14) 0.0055(14) N1 0.0203(17) 0.0233(18) 0.0268(17) -0.0016(14) 0.0158(15) 0.0003(15) C1 0.022(2) 0.019(2) 0.026(2) -0.0004(16) 0.0132(17) 0.0028(18) O2 0.0211(16) 0.0283(19) 0.0379(17) -0.0012(12) 0.0198(14) -0.0013(13) N2 0.0176(17) 0.0245(19) 0.0215(16) -0.0012(14) 0.0089(14) -0.0022(15) C2 0.025(2) 0.022(2) 0.021(2) -0.0029(17) 0.0100(17) 0.0015(19) O3 0.040(2) 0.045(2) 0.051(2) 0.0259(17) 0.0304(17) 0.0178(18) N3 0.040(2) 0.033(2) 0.035(2) 0.0115(17) 0.0256(19) 0.0159(19) C3 0.026(2) 0.024(2) 0.027(2) -0.0010(17) 0.0141(19) 0.0018(18) O4 0.0338(18) 0.0312(19) 0.0477(19) 0.0129(15) 0.0245(16) 0.0151(16) N4 0.037(2) 0.028(2) 0.042(2) 0.0092(17) 0.0276(19) 0.0107(19) C4 0.038(3) 0.024(2) 0.025(2) 0.0003(17) 0.016(2) -0.003(2) O5 0.0217(15) 0.0330(18) 0.0377(18) 0.0024(13) 0.0203(14) 0.0038(13) N5 0.0232(19) 0.0244(19) 0.0311(19) 0.0014(16) 0.0154(16) -0.0043(17) C5 0.036(3) 0.022(2) 0.025(2) 0.0005(17) 0.0114(19) 0.004(2) O6 0.053(3) 0.042(3) 0.112(4) 0.042(2) 0.049(3) 0.011(2) N6 0.0192(18) 0.027(2) 0.0291(19) -0.0002(15) 0.0130(15) 0.0016(16) C6 0.023(2) 0.031(3) 0.034(2) 0.0036(19) 0.0125(19) 0.009(2) O7 0.036(2) 0.045(2) 0.0355(18) 0.0119(15) 0.0221(16) 0.0211(17) C7 0.026(2) 0.024(2) 0.034(2) 0.0002(18) 0.0179(19) 0.001(2) C8 0.019(2) 0.022(2) 0.027(2) -0.0026(17) 0.0104(17) -0.0004(18) C9 0.018(2) 0.021(2) 0.030(2) 0.0001(17) 0.0158(18) 0.0007(18) C10 0.021(2) 0.021(2) 0.027(2) 0.0012(17) 0.0115(17) 0.0010(18) C11 0.019(2) 0.023(2) 0.027(2) -0.0010(16) 0.0123(18) 0.0032(17) C12 0.020(2) 0.024(2) 0.028(2) 0.0010(17) 0.0136(18) -0.0024(19) C13 0.021(2) 0.020(2) 0.028(2) -0.0003(16) 0.0126(17) 0.0025(18) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; 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 N2 2.004(3) . yes Pt1 N2 2.004(4) 2_654 ? Pt1 N1 2.036(3) . yes Pt1 N1 2.036(3) 2_654 ? O1 C8 1.238(5) . yes N1 H1A 0.9100 . ? N1 H1B 0.9100 . ? N1 H1C 0.9100 . ? C1 N2 1.300(5) . yes C1 N3 1.333(6) . yes C1 C2 1.499(6) . yes O2 N5 1.238(5) . ? C2 C3 1.392(6) . ? C2 C7 1.399(6) . ? O3 N5 1.237(5) . ? N3 H3A 0.8800 . ? N3 H3B 0.8800 . ? C3 C4 1.382(6) . ? C3 H3 0.9500 . ? O4 N6 1.236(5) . ? N4 O6 1.214(6) . ? N4 O7 1.235(5) . ? N4 C13 1.463(6) . ? C4 C5 1.392(7) . ? C4 H4 0.9500 . ? O5 N6 1.236(5) . ? N5 C9 1.446(6) . ? C5 C6 1.395(7) . ? C5 H5 0.9500 . ? N6 C11 1.440(6) . ? C6 C7 1.391(7) . ? C6 H6 0.9500 . ? C7 H7 0.9500 . ? C8 C13 1.449(6) . ? C8 C9 1.465(6) . ? C9 C10 1.375(6) . ? C10 C11 1.382(6) . ? C10 H10 0.9500 . ? C11 C12 1.388(6) . ? C12 C13 1.363(6) . ? C12 H12 0.9500 . ? 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 N2 Pt1 N2 88.9(2) . 2_654 ? N2 Pt1 N1 91.52(15) . . yes N2 Pt1 N1 179.07(13) 2_654 . ? N2 Pt1 N1 179.07(13) . 2_654 ? N2 Pt1 N1 91.52(15) 2_654 2_654 ? N1 Pt1 N1 88.1(2) . 2_654 ? Pt1 N1 H1A 109.5 . . ? Pt1 N1 H1B 109.5 . . ? H1A N1 H1B 109.5 . . ? Pt1 N1 H1C 109.5 . . ? H1A N1 H1C 109.5 . . ? H1B N1 H1C 109.5 . . ? N2 C1 N3 123.2(4) . . yes N2 C1 C2 119.7(4) . . ? N3 C1 C2 117.1(4) . . ? C1 N2 Pt1 129.0(3) . . yes C3 C2 C7 119.7(4) . . ? C3 C2 C1 121.0(4) . . ? C7 C2 C1 119.2(4) . . ? C1 N3 H3A 120.0 . . ? C1 N3 H3B 120.0 . . ? H3A N3 H3B 120.0 . . ? C4 C3 C2 120.4(4) . . ? C4 C3 H3 119.8 . . ? C2 C3 H3 119.8 . . ? O6 N4 O7 123.8(4) . . ? O6 N4 C13 118.1(4) . . ? O7 N4 C13 118.0(4) . . ? C3 C4 C5 120.2(5) . . ? C3 C4 H4 119.9 . . ? C5 C4 H4 119.9 . . ? O3 N5 O2 121.4(4) . . ? O3 N5 C9 118.7(4) . . ? O2 N5 C9 119.9(4) . . ? C4 C5 C6 119.7(4) . . ? C4 C5 H5 120.1 . . ? C6 C5 H5 120.1 . . ? O5 N6 O4 123.1(4) . . ? O5 N6 C11 118.4(4) . . ? O4 N6 C11 118.5(4) . . ? C7 C6 C5 120.3(4) . . ? C7 C6 H6 119.9 . . ? C5 C6 H6 119.9 . . ? C6 C7 C2 119.7(4) . . ? C6 C7 H7 120.2 . . ? C2 C7 H7 120.2 . . ? O1 C8 C13 123.7(4) . . ? O1 C8 C9 125.7(4) . . ? C13 C8 C9 110.6(4) . . ? C10 C9 N5 116.3(4) . . ? C10 C9 C8 124.0(4) . . ? N5 C9 C8 119.6(4) . . ? C9 C10 C11 120.0(4) . . ? C9 C10 H10 120.0 . . ? C11 C10 H10 120.0 . . ? C10 C11 C12 120.4(4) . . ? C10 C11 N6 120.4(4) . . ? C12 C11 N6 119.2(4) . . ? C13 C12 C11 119.3(4) . . ? C13 C12 H12 120.4 . . ? C11 C12 H12 120.4 . . ? C12 C13 C8 125.6(4) . . ? C12 C13 N4 115.9(4) . . ? C8 C13 N4 118.5(4) . . ? loop_ _geom_hbond_atom_site_label_D _geom_hbond_atom_site_label_H _geom_hbond_atom_site_label_A _geom_hbond_distance_DH _geom_hbond_distance_HA _geom_hbond_distance_DA _geom_hbond_angle_DHA _geom_hbond_site_symmetry_A _geom_hbond_publ_flag N1 H1A O1 0.91 2.11 2.906(5) 144.9 5_655 yes N1 H1A O2 0.91 2.41 3.060(5) 128.1 5_655 yes N1 H1B O2 0.91 2.24 3.107(5) 159.8 6 yes N1 H1C O5 0.91 2.35 3.080(5) 137.1 7_645 yes N3 H3A O1 0.88 2.08 2.912(5) 158.6 5_655 yes N3 H3B O7 0.88 2.43 2.889(5) 113.1 5_655 yes N3 H3B O7 0.88 2.45 3.176(5) 139.8 . yes _diffrn_measured_fraction_theta_max 0.996 _diffrn_reflns_theta_full 25.75 _diffrn_measured_fraction_theta_full 0.996 _refine_diff_density_max 1.329 _refine_diff_density_min -2.055 _refine_diff_density_rms 0.141 # Attachment 'ms_new.cif' #Facile cyanamide-ammonia coupling mediated by cis- and trans-[PtIIL2] centers #and giving metal-bound guanidines #by Marina R. Tyan, Nadezhda A. Bokach, Meng-Jiy Wang, Matti Haukka, and #Vadim Yu. Kukushkin data_trans_1 _database_code_depnum_ccdc_archive 'CCDC 686035' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety 'C6 H18 Cl2 N6 Pt' _chemical_formula_sum 'C6 H18 Cl2 N6 Pt' _chemical_formula_weight 440.25 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' _symmetry_cell_setting monoclinic _symmetry_space_group_name_H-M 'P 21/c' _symmetry_space_group_name_Hall '-P 2ybc' 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' _cell_length_a 8.5921(2) _cell_length_b 5.9196(2) _cell_length_c 13.0020(2) _cell_angle_alpha 90.00 _cell_angle_beta 107.153(5) _cell_angle_gamma 90.00 _cell_volume 631.89(3) _cell_formula_units_Z 2 _cell_measurement_temperature 120(2) _cell_measurement_reflns_used 2911 _cell_measurement_theta_min 1.00 _cell_measurement_theta_max 28.70 _exptl_crystal_description block _exptl_crystal_colour yellow _exptl_crystal_size_max 0.30 _exptl_crystal_size_mid 0.30 _exptl_crystal_size_min 0.24 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 2.314 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 416 _exptl_absorpt_coefficient_mu 11.506 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.0381 _exptl_absorpt_correction_T_max 0.0654 _exptl_absorpt_process_details 'SADABS v.2.10 (Sheldrick, 2003)' _publ_section_exptl_refinement ; The Pt atom is located on a center of symmetry (inversion centre) and is coordinated by two N atoms and two Cl atoms in a slightly distorted square planar geometry. The NH~2~ and NH hydrogen atoms were located from the difference Fourier map but constrained to ride on their parent atom, with U~iso~ = 1.5 U~eq~(parent atom). Other hydrogen atoms were positioned geometrically and were also constrained to ride on their parent atoms, with C---H = 0.98 \%A, and U~iso~ = 1.5 U~eq~(parent atom). Due to the irregular crystal the crystal faces could not be determined accurately. Therefore, the analytical absorption correction was not satisfactory and the final absorption correction was carried out by multi-scan method. The highest peak is located 1.23 \%A from atom H3A and the deepest hole is located 0.80 \%A from atom Pt1. ; _exptl_special_details ; ? ; _diffrn_ambient_temperature 120(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator 'horizontally mounted graphite crystal' _diffrn_measurement_device_type 'Nonius KappaCCD' _diffrn_measurement_device '95mm CCD camera on \k-goniostat' _diffrn_detector_area_resol_mean 9 _diffrn_measurement_method '\f scans and \w scans with \k offset' _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 13106 _diffrn_reflns_av_R_equivalents 0.0356 _diffrn_reflns_av_sigmaI/netI 0.0190 _diffrn_reflns_limit_h_min -11 _diffrn_reflns_limit_h_max 11 _diffrn_reflns_limit_k_min -7 _diffrn_reflns_limit_k_max 7 _diffrn_reflns_limit_l_min -17 _diffrn_reflns_limit_l_max 17 _diffrn_reflns_theta_min 2.48 _diffrn_reflns_theta_max 28.72 _reflns_number_total 1629 _reflns_number_gt 1360 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'Collect (Bruker AXS BV, 1997-2004)' _computing_cell_refinement 'Denzo/Scalepack (Otwinowski & Minor, 1997)' _computing_data_reduction 'Denzo/Scalepack (Otwinowski & Minor, 1997)' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1997)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'Diamond v.3.1e (Brandenburg, 2007)' _computing_publication_material 'SHELXL-97 (Sheldrick, 1997)' _refine_special_details ; Refinement of F^2^ against ALL reflections. The weighted R-factor wR and goodness of fit S are based on F^2^, conventional R-factors R are based on F, with F set to zero for negative F^2^. The threshold expression of F^2^ > 2sigma(F^2^) is used only for calculating R-factors(gt) etc. and is not relevant to the choice of reflections for refinement. R-factors based on F^2^ are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger. ; _refine_ls_structure_factor_coef Fsqd _refine_ls_matrix_type full _refine_ls_weighting_scheme calc _refine_ls_weighting_details 'calc w=1/[\s^2^(Fo^2^)+(0.0169P)^2^+0.9780P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens mixed _refine_ls_hydrogen_treatment constr _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 1629 _refine_ls_number_parameters 72 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0231 _refine_ls_R_factor_gt 0.0172 _refine_ls_wR_factor_ref 0.0401 _refine_ls_wR_factor_gt 0.0380 _refine_ls_goodness_of_fit_ref 1.107 _refine_ls_restrained_S_all 1.107 _refine_ls_shift/su_max 0.001 _refine_ls_shift/su_mean 0.000 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 1.0000 0.0000 1.0000 0.01099(6) Uani 1 2 d S . . Cl1 Cl 1.20726(9) -0.25417(13) 1.01399(6) 0.02133(14) Uani 1 1 d . . . N1 N 1.1455(3) 0.1911(4) 1.11853(18) 0.0145(5) Uani 1 1 d . . . H1N H 1.2034 0.3312 1.1083 0.022 Uiso 1 1 d R . . N2 N 1.1228(4) -0.0293(5) 1.2584(2) 0.0270(7) Uani 1 1 d . . . H2N H 1.1711 -0.0996 1.3173 0.040 Uiso 1 1 d R . . H2M H 1.0520 -0.1282 1.2119 0.040 Uiso 1 1 d R . . N3 N 1.3019(3) 0.2725(4) 1.29465(18) 0.0197(5) Uani 1 1 d . . . C1 C 1.1912(3) 0.1469(5) 1.2219(2) 0.0138(5) Uani 1 1 d . . . C2 C 1.3923(5) 0.4500(6) 1.2595(3) 0.0300(8) Uani 1 1 d . . . H2A H 1.4212 0.3988 1.1958 0.045 Uiso 1 1 calc R . . H2B H 1.4918 0.4844 1.3175 0.045 Uiso 1 1 calc R . . H2C H 1.3247 0.5860 1.2416 0.045 Uiso 1 1 calc R . . C3 C 1.3417(4) 0.2297(6) 1.4093(2) 0.0237(7) Uani 1 1 d . . . H3A H 1.2411 0.2132 1.4295 0.036 Uiso 1 1 calc R . . H3B H 1.4051 0.3565 1.4490 0.036 Uiso 1 1 calc R . . H3C H 1.4059 0.0906 1.4270 0.036 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 0.01262(8) 0.01198(8) 0.00704(8) -0.00040(5) 0.00085(5) -0.00072(6) Cl1 0.0199(3) 0.0216(3) 0.0187(3) -0.0036(3) -0.0001(2) 0.0064(3) N1 0.0147(12) 0.0150(11) 0.0121(10) -0.0020(9) 0.0012(9) -0.0030(9) N2 0.0303(16) 0.0343(16) 0.0130(12) 0.0018(11) 0.0014(11) -0.0176(12) N3 0.0227(13) 0.0202(12) 0.0120(11) -0.0003(10) -0.0014(10) -0.0058(11) C1 0.0102(13) 0.0175(13) 0.0135(12) -0.0023(11) 0.0029(10) -0.0004(11) C2 0.034(2) 0.0263(16) 0.0221(16) 0.0044(14) -0.0035(15) -0.0124(15) C3 0.0244(16) 0.0338(17) 0.0105(13) -0.0047(13) 0.0013(12) -0.0093(15) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; 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 2.020(2) 3_757 ? Pt1 N1 2.020(2) . yes Pt1 Cl1 2.2971(7) 3_757 ? Pt1 Cl1 2.2972(7) . yes N1 C1 1.310(3) . yes N1 H1N 0.9960 . ? N2 C1 1.351(4) . yes N2 H2N 0.8619 . ? N2 H2M 0.9282 . ? N3 C1 1.350(4) . yes N3 C3 1.451(3) . ? N3 C2 1.458(4) . ? C2 H2A 0.9800 . ? C2 H2B 0.9800 . ? C2 H2C 0.9800 . ? C3 H3A 0.9800 . ? C3 H3B 0.9800 . ? C3 H3C 0.9800 . ? 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 N1 180.0 3_757 . ? N1 Pt1 Cl1 90.88(7) 3_757 3_757 ? N1 Pt1 Cl1 89.12(7) . 3_757 yes N1 Pt1 Cl1 89.12(7) 3_757 . ? N1 Pt1 Cl1 90.88(7) . . yes Cl1 Pt1 Cl1 180.0 3_757 . ? C1 N1 Pt1 127.0(2) . . ? C1 N1 H1N 107.0 . . ? Pt1 N1 H1N 125.9 . . ? C1 N2 H2N 122.6 . . ? C1 N2 H2M 121.8 . . ? H2N N2 H2M 109.0 . . ? C1 N3 C3 121.9(3) . . ? C1 N3 C2 120.5(2) . . ? C3 N3 C2 117.5(3) . . ? N1 C1 N3 123.0(3) . . yes N1 C1 N2 119.0(3) . . yes N3 C1 N2 117.9(3) . . ? N3 C2 H2A 109.5 . . ? N3 C2 H2B 109.5 . . ? H2A C2 H2B 109.5 . . ? N3 C2 H2C 109.5 . . ? H2A C2 H2C 109.5 . . ? H2B C2 H2C 109.5 . . ? N3 C3 H3A 109.5 . . ? N3 C3 H3B 109.5 . . ? H3A C3 H3B 109.5 . . ? N3 C3 H3C 109.5 . . ? H3A C3 H3C 109.5 . . ? H3B C3 H3C 109.5 . . ? _diffrn_measured_fraction_theta_max 0.998 _diffrn_reflns_theta_full 28.72 _diffrn_measured_fraction_theta_full 0.998 _refine_diff_density_max 0.609 _refine_diff_density_min -1.393 _refine_diff_density_rms 0.148 #===END======================================================================== data_trans_3 _database_code_depnum_ccdc_archive 'CCDC 686036' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety 'C12 H26 Cl2 N6 Pt' _chemical_formula_sum 'C12 H26 Cl2 N6 Pt' _chemical_formula_weight 520.38 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' _symmetry_cell_setting monoclinic _symmetry_space_group_name_H-M 'P 21/n' _symmetry_space_group_name_Hall '-P 2yn' 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' _cell_length_a 11.6603(4) _cell_length_b 8.1283(8) _cell_length_c 17.8991(15) _cell_angle_alpha 90.00 _cell_angle_beta 93.383(6) _cell_angle_gamma 90.00 _cell_volume 1693.5(2) _cell_formula_units_Z 4 _cell_measurement_temperature 120(2) _cell_measurement_reflns_used 7770 _cell_measurement_theta_min 2.91 _cell_measurement_theta_max 27.48 _exptl_crystal_description green _exptl_crystal_colour block _exptl_crystal_size_max 0.18 _exptl_crystal_size_mid 0.15 _exptl_crystal_size_min 0.09 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 2.041 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1008 _exptl_absorpt_coefficient_mu 8.604 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.2627 _exptl_absorpt_correction_T_max 0.4595 _exptl_absorpt_process_details 'SADABS v.2.10 (Sheldrick, 2003)' _publ_section_exptl_refinement ; The X atom is coordinated by two N atoms and two Cl atoms in a slightly distorted square planar geometry. The NH~2~ and NH hydrogen atoms were located from the difference Fourier map but constrained to ride on their parent atom, with U~iso~ = 1.5 U~eq~(parent atom). Other hydrogen atoms were positioned geometrically and were also constrained to ride on their parent atoms, with C---H = 0.99 \%A, and U~iso~ = 1.2 U~eq~(parent atom). The highest peak is located 0.91 \%A from atom Pt1 and the deepest hole is located 0.74 \%A from atom Pt1. ; _exptl_special_details ; ? ; _diffrn_ambient_temperature 120(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator 'horizontally mounted graphite crystal' _diffrn_measurement_device_type 'Nonius KappaCCD' _diffrn_measurement_device '95mm CCD camera on \k-goniostat' _diffrn_detector_area_resol_mean 9 _diffrn_measurement_method '\f scans and \w scans with \k offset' _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 42548 _diffrn_reflns_av_R_equivalents 0.0465 _diffrn_reflns_av_sigmaI/netI 0.0256 _diffrn_reflns_limit_h_min -14 _diffrn_reflns_limit_h_max 15 _diffrn_reflns_limit_k_min -10 _diffrn_reflns_limit_k_max 10 _diffrn_reflns_limit_l_min -23 _diffrn_reflns_limit_l_max 23 _diffrn_reflns_theta_min 2.14 _diffrn_reflns_theta_max 27.50 _reflns_number_total 3898 _reflns_number_gt 3344 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'Collect (Bruker AXS BV, 1997-2004)' _computing_cell_refinement 'EvalCCD (Duisenberg, 1998-2003)' _computing_data_reduction 'EvalCCD (Duisenberg, 1998-2003)' _computing_structure_solution 'SIR97 (Altomare et al., 1997)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'Diamond v.3.1e (Brandenburg, 2007)' _computing_publication_material 'SHELXL-97 (Sheldrick, 1997)' _refine_special_details ; Refinement of F^2^ against ALL reflections. The weighted R-factor wR and goodness of fit S are based on F^2^, conventional R-factors R are based on F, with F set to zero for negative F^2^. The threshold expression of F^2^ > 2sigma(F^2^) is used only for calculating R-factors(gt) etc. and is not relevant to the choice of reflections for refinement. R-factors based on F^2^ are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger. ; _refine_ls_structure_factor_coef Fsqd _refine_ls_matrix_type full _refine_ls_weighting_scheme calc _refine_ls_weighting_details 'calc w=1/[\s^2^(Fo^2^)+(0.0083P)^2^+1.5419P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens mixed _refine_ls_hydrogen_treatment constr _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 3898 _refine_ls_number_parameters 190 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0300 _refine_ls_R_factor_gt 0.0190 _refine_ls_wR_factor_ref 0.0314 _refine_ls_wR_factor_gt 0.0295 _refine_ls_goodness_of_fit_ref 1.074 _refine_ls_restrained_S_all 1.074 _refine_ls_shift/su_max 0.003 _refine_ls_shift/su_mean 0.000 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 0.107156(9) 0.268708(11) 0.603096(6) 0.01317(3) Uani 1 1 d . . . Cl1 Cl 0.30052(5) 0.20914(8) 0.61319(4) 0.02124(14) Uani 1 1 d . . . Cl2 Cl -0.08158(6) 0.35036(7) 0.59235(4) 0.01873(14) Uani 1 1 d . . . N1 N 0.09681(18) 0.2760(2) 0.71544(12) 0.0153(5) Uani 1 1 d . . . H1N H 0.0480 0.3555 0.7281 0.023 Uiso 1 1 d R . . N2 N 0.2055(2) 0.0544(3) 0.75716(13) 0.0210(5) Uani 1 1 d . . . H2N H 0.2405 0.0523 0.7117 0.032 Uiso 1 1 d R . . H2M H 0.2238 -0.0336 0.7913 0.032 Uiso 1 1 d R . . N3 N 0.09787(18) 0.1921(3) 0.84079(12) 0.0153(5) Uani 1 1 d . . . N4 N 0.10920(19) 0.2685(3) 0.49106(12) 0.0173(5) Uani 1 1 d . . . H4N H 0.0840 0.3742 0.4696 0.026 Uiso 1 1 d R . . N5 N 0.1767(2) 0.0062(3) 0.47479(14) 0.0248(6) Uani 1 1 d . . . H5N H 0.1914 0.0071 0.5268 0.037 Uiso 1 1 d R . . H5M H 0.1547 -0.0883 0.4572 0.037 Uiso 1 1 d R . . N6 N 0.10952(19) 0.1550(3) 0.37152(12) 0.0178(5) Uani 1 1 d . . . C1 C 0.1330(2) 0.1780(3) 0.76970(15) 0.0148(5) Uani 1 1 d . . . C2 C 0.0051(2) 0.3087(3) 0.85493(15) 0.0190(6) Uani 1 1 d . . . H2A H -0.0536 0.3057 0.8127 0.023 Uiso 1 1 calc R . . H2B H 0.0366 0.4217 0.8586 0.023 Uiso 1 1 calc R . . C3 C -0.0497(2) 0.2651(4) 0.92670(15) 0.0240(6) Uani 1 1 d . . . H3A H -0.0876 0.1565 0.9211 0.029 Uiso 1 1 calc R . . H3B H -0.1092 0.3477 0.9368 0.029 Uiso 1 1 calc R . . C4 C 0.0391(2) 0.2598(4) 0.99200(16) 0.0272(7) Uani 1 1 d . . . H4A H 0.0726 0.3706 1.0005 0.033 Uiso 1 1 calc R . . H4B H 0.0022 0.2260 1.0380 0.033 Uiso 1 1 calc R . . C5 C 0.1329(2) 0.1389(4) 0.97542(16) 0.0242(6) Uani 1 1 d . . . H5A H 0.1931 0.1404 1.0168 0.029 Uiso 1 1 calc R . . H5B H 0.1004 0.0264 0.9720 0.029 Uiso 1 1 calc R . . C6 C 0.1858(2) 0.1811(3) 0.90311(15) 0.0189(6) Uani 1 1 d . . . H6A H 0.2266 0.2877 0.9087 0.023 Uiso 1 1 calc R . . H6B H 0.2428 0.0958 0.8917 0.023 Uiso 1 1 calc R . . C7 C 0.1286(2) 0.1455(3) 0.44666(15) 0.0155(6) Uani 1 1 d . . . C8 C 0.0059(2) 0.2364(3) 0.33895(15) 0.0194(6) Uani 1 1 d . . . H8A H -0.0209 0.3190 0.3746 0.023 Uiso 1 1 calc R . . H8B H -0.0559 0.1539 0.3300 0.023 Uiso 1 1 calc R . . C9 C 0.0295(2) 0.3196(3) 0.26633(16) 0.0219(6) Uani 1 1 d . . . H9A H 0.0834 0.4122 0.2765 0.026 Uiso 1 1 calc R . . H9B H -0.0430 0.3652 0.2434 0.026 Uiso 1 1 calc R . . C10 C 0.0809(2) 0.2008(3) 0.21159(16) 0.0226(6) Uani 1 1 d . . . H10A H 0.0227 0.1178 0.1950 0.027 Uiso 1 1 calc R . . H10B H 0.1036 0.2618 0.1669 0.027 Uiso 1 1 calc R . . C11 C 0.1849(2) 0.1154(3) 0.24844(16) 0.0230(6) Uani 1 1 d . . . H11A H 0.2130 0.0313 0.2139 0.028 Uiso 1 1 calc R . . H11B H 0.2471 0.1969 0.2584 0.028 Uiso 1 1 calc R . . C12 C 0.1570(2) 0.0341(3) 0.32097(15) 0.0203(6) Uani 1 1 d . . . H12A H 0.1005 -0.0552 0.3107 0.024 Uiso 1 1 calc R . . H12B H 0.2275 -0.0150 0.3451 0.024 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 0.01668(6) 0.01280(5) 0.00987(5) 0.00052(4) -0.00057(3) -0.00102(4) Cl1 0.0170(3) 0.0310(4) 0.0158(3) -0.0004(3) 0.0012(3) -0.0014(3) Cl2 0.0203(3) 0.0162(3) 0.0192(4) 0.0007(3) -0.0032(3) 0.0027(2) N1 0.0182(12) 0.0152(11) 0.0125(11) 0.0006(9) 0.0000(9) 0.0021(9) N2 0.0266(14) 0.0196(12) 0.0172(13) 0.0034(10) 0.0043(10) 0.0077(9) N3 0.0162(12) 0.0175(11) 0.0122(12) 0.0010(9) -0.0003(9) 0.0026(8) N4 0.0254(13) 0.0128(11) 0.0132(11) 0.0026(9) -0.0025(9) 0.0021(9) N5 0.0442(16) 0.0137(12) 0.0154(14) 0.0003(9) -0.0067(11) 0.0025(10) N6 0.0239(13) 0.0189(12) 0.0103(12) -0.0008(9) -0.0012(10) 0.0084(9) C1 0.0136(14) 0.0166(13) 0.0139(14) -0.0010(10) -0.0012(11) -0.0042(10) C2 0.0198(15) 0.0219(14) 0.0154(15) 0.0012(11) 0.0006(11) 0.0046(11) C3 0.0237(16) 0.0316(16) 0.0173(15) -0.0009(13) 0.0048(11) 0.0050(12) C4 0.0290(17) 0.0383(18) 0.0148(14) -0.0024(13) 0.0052(12) -0.0008(13) C5 0.0233(16) 0.0361(17) 0.0127(16) 0.0031(13) -0.0034(12) -0.0009(12) C6 0.0179(15) 0.0226(14) 0.0159(15) 0.0001(11) -0.0022(11) -0.0004(11) C7 0.0164(14) 0.0153(13) 0.0148(15) 0.0006(11) -0.0004(11) -0.0028(10) C8 0.0194(14) 0.0199(14) 0.0185(14) -0.0027(12) -0.0032(11) 0.0024(11) C9 0.0233(16) 0.0219(14) 0.0196(16) 0.0010(12) -0.0055(12) 0.0019(11) C10 0.0279(16) 0.0246(15) 0.0151(15) 0.0023(12) -0.0016(12) -0.0019(12) C11 0.0246(16) 0.0269(15) 0.0179(16) -0.0040(12) 0.0046(12) 0.0021(12) C12 0.0279(17) 0.0178(14) 0.0152(15) -0.0020(11) 0.0007(12) 0.0050(11) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; 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 N4 2.007(2) . yes Pt1 N1 2.022(2) . yes Pt1 Cl2 2.2959(6) . yes Pt1 Cl1 2.3027(7) . yes N1 C1 1.306(3) . yes N1 H1N 0.8994 . ? N2 C1 1.340(3) . yes N2 H2N 0.9328 . ? N2 H2M 0.9570 . ? N3 C1 1.364(3) . yes N3 C2 1.471(3) . ? N3 C6 1.473(3) . ? N4 C7 1.305(3) . yes N4 H4N 0.9793 . ? N5 C7 1.348(3) . yes N5 H5N 0.9373 . ? N5 H5M 0.8630 . ? N6 C7 1.353(3) . yes N6 C12 1.466(3) . ? N6 C8 1.468(3) . ? C2 C3 1.510(4) . ? C2 H2A 0.9900 . ? C2 H2B 0.9900 . ? C3 C4 1.516(4) . ? C3 H3A 0.9900 . ? C3 H3B 0.9900 . ? C4 C5 1.513(4) . ? C4 H4A 0.9900 . ? C4 H4B 0.9900 . ? C5 C6 1.506(4) . ? C5 H5A 0.9900 . ? C5 H5B 0.9900 . ? C6 H6A 0.9900 . ? C6 H6B 0.9900 . ? C8 C9 1.505(4) . ? C8 H8A 0.9900 . ? C8 H8B 0.9900 . ? C9 C10 1.523(4) . ? C9 H9A 0.9900 . ? C9 H9B 0.9900 . ? C10 C11 1.514(4) . ? C10 H10A 0.9900 . ? C10 H10B 0.9900 . ? C11 C12 1.509(4) . ? C11 H11A 0.9900 . ? C11 H11B 0.9900 . ? C12 H12A 0.9900 . ? C12 H12B 0.9900 . ? 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 N4 Pt1 N1 176.81(9) . . yes N4 Pt1 Cl2 89.10(6) . . ? N1 Pt1 Cl2 87.81(6) . . ? N4 Pt1 Cl1 90.51(7) . . ? N1 Pt1 Cl1 92.51(6) . . ? Cl2 Pt1 Cl1 175.32(2) . . yes C1 N1 Pt1 133.29(18) . . ? C1 N1 H1N 115.6 . . ? Pt1 N1 H1N 110.3 . . ? C1 N2 H2N 118.2 . . ? C1 N2 H2M 124.9 . . ? H2N N2 H2M 116.8 . . ? C1 N3 C2 118.6(2) . . ? C1 N3 C6 117.9(2) . . ? C2 N3 C6 113.3(2) . . ? C7 N4 Pt1 128.43(18) . . ? C7 N4 H4N 119.4 . . ? Pt1 N4 H4N 111.8 . . ? C7 N5 H5N 114.3 . . ? C7 N5 H5M 120.2 . . ? H5N N5 H5M 113.7 . . ? C7 N6 C12 122.0(2) . . ? C7 N6 C8 120.3(2) . . ? C12 N6 C8 112.9(2) . . yes N1 C1 N2 120.8(2) . . yes N1 C1 N3 122.7(2) . . yes N2 C1 N3 116.5(2) . . ? N3 C2 C3 110.3(2) . . ? N3 C2 H2A 109.6 . . ? C3 C2 H2A 109.6 . . ? N3 C2 H2B 109.6 . . ? C3 C2 H2B 109.6 . . ? H2A C2 H2B 108.1 . . ? C2 C3 C4 111.0(2) . . ? C2 C3 H3A 109.4 . . ? C4 C3 H3A 109.4 . . ? C2 C3 H3B 109.4 . . ? C4 C3 H3B 109.4 . . ? H3A C3 H3B 108.0 . . ? C5 C4 C3 109.7(2) . . ? C5 C4 H4A 109.7 . . ? C3 C4 H4A 109.7 . . ? C5 C4 H4B 109.7 . . ? C3 C4 H4B 109.7 . . ? H4A C4 H4B 108.2 . . ? C6 C5 C4 111.0(2) . . ? C6 C5 H5A 109.4 . . ? C4 C5 H5A 109.4 . . ? C6 C5 H5B 109.4 . . ? C4 C5 H5B 109.4 . . ? H5A C5 H5B 108.0 . . ? N3 C6 C5 111.3(2) . . ? N3 C6 H6A 109.4 . . ? C5 C6 H6A 109.4 . . ? N3 C6 H6B 109.4 . . ? C5 C6 H6B 109.4 . . ? H6A C6 H6B 108.0 . . ? N4 C7 N5 120.0(2) . . yes N4 C7 N6 122.5(2) . . yes N5 C7 N6 117.4(2) . . yes N6 C8 C9 110.9(2) . . ? N6 C8 H8A 109.5 . . ? C9 C8 H8A 109.5 . . ? N6 C8 H8B 109.5 . . ? C9 C8 H8B 109.5 . . ? H8A C8 H8B 108.0 . . ? C8 C9 C10 111.7(2) . . ? C8 C9 H9A 109.3 . . ? C10 C9 H9A 109.3 . . ? C8 C9 H9B 109.3 . . ? C10 C9 H9B 109.3 . . ? H9A C9 H9B 107.9 . . ? C11 C10 C9 110.2(2) . . ? C11 C10 H10A 109.6 . . ? C9 C10 H10A 109.6 . . ? C11 C10 H10B 109.6 . . ? C9 C10 H10B 109.6 . . ? H10A C10 H10B 108.1 . . ? C12 C11 C10 111.5(2) . . ? C12 C11 H11A 109.3 . . ? C10 C11 H11A 109.3 . . ? C12 C11 H11B 109.3 . . ? C10 C11 H11B 109.3 . . ? H11A C11 H11B 108.0 . . ? N6 C12 C11 110.3(2) . . ? N6 C12 H12A 109.6 . . ? C11 C12 H12A 109.6 . . ? N6 C12 H12B 109.6 . . ? C11 C12 H12B 109.6 . . ? H12A C12 H12B 108.1 . . ? loop_ _geom_hbond_atom_site_label_D _geom_hbond_atom_site_label_H _geom_hbond_atom_site_label_A _geom_hbond_distance_DH _geom_hbond_distance_HA _geom_hbond_distance_DA _geom_hbond_angle_DHA _geom_hbond_site_symmetry_A _geom_hbond_publ_flag N2 H2N Cl1 0.93 2.32 3.129(2) 145.2 . yes N2 H2M N1 0.96 2.61 3.247(3) 124.2 2_546 yes N2 H2M Cl1 0.96 2.73 3.645(2) 161.2 2_546 yes N4 H4N Cl2 0.98 2.50 3.446(2) 162.9 3_566 yes N5 H5N Cl1 0.94 2.54 3.244(3) 131.6 . yes N5 H5M Cl2 0.86 2.44 3.304(2) 176.9 3_556 yes _diffrn_measured_fraction_theta_max 0.999 _diffrn_reflns_theta_full 27.50 _diffrn_measured_fraction_theta_full 0.999 _refine_diff_density_max 0.717 _refine_diff_density_min -0.601 _refine_diff_density_rms 0.117 #===END======================================================================== data_trans_4 _database_code_depnum_ccdc_archive 'CCDC 686037' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety 'C6 H24 N8 Pt, 2(C6 H2 N3 O7)' _chemical_formula_sum 'C18 H28 N14 O14 Pt' _chemical_formula_weight 859.63 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' Pt Pt -1.7033 8.3905 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting monoclinic _symmetry_space_group_name_H-M 'P 21/c' _symmetry_space_group_name_Hall '-P 2ybc' 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' _cell_length_a 7.1799(4) _cell_length_b 25.9606(16) _cell_length_c 8.3485(10) _cell_angle_alpha 90.00 _cell_angle_beta 114.039(5) _cell_angle_gamma 90.00 _cell_volume 1421.1(2) _cell_formula_units_Z 2 _cell_measurement_temperature 120(2) _cell_measurement_reflns_used 6126 _cell_measurement_theta_min 1.00 _cell_measurement_theta_max 27.48 _exptl_crystal_description plate _exptl_crystal_colour yellow _exptl_crystal_size_max 0.29 _exptl_crystal_size_mid 0.12 _exptl_crystal_size_min 0.05 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 2.009 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 848 _exptl_absorpt_coefficient_mu 5.032 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.3222 _exptl_absorpt_correction_T_max 0.7870 _exptl_absorpt_process_details 'SADABS v.2.10 (Sheldrick, 2003)' _publ_section_exptl_refinement ; The NH and NH~3~ hydrogens were located from the difference Fourier map but constrained to ride on their parent atom, with U~iso~ = 1.5 U~eq~(parent atom). Other hydrogens were positioned geometrically and were also constrained to ride on their parent atoms, with C---H =0.95-0.98 \%A, and U~iso~ = 1.2-1.5 U~eq~(parent atom). ; _exptl_special_details ; ? ; _diffrn_ambient_temperature 120(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator 'horizontally mounted graphite crystal' _diffrn_measurement_device_type 'Nonius KappaCCD' _diffrn_measurement_device '95mm CCD camera on \k-goniostat' _diffrn_detector_area_resol_mean 9 _diffrn_measurement_method '\f scans and \w scans with \k offset' _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 25722 _diffrn_reflns_av_R_equivalents 0.0424 _diffrn_reflns_av_sigmaI/netI 0.0279 _diffrn_reflns_limit_h_min -9 _diffrn_reflns_limit_h_max 8 _diffrn_reflns_limit_k_min -33 _diffrn_reflns_limit_k_max 33 _diffrn_reflns_limit_l_min -10 _diffrn_reflns_limit_l_max 10 _diffrn_reflns_theta_min 2.78 _diffrn_reflns_theta_max 27.59 _reflns_number_total 3280 _reflns_number_gt 2347 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'Collect (Nonius BV, 1997-2000)' _computing_cell_refinement 'Denzo/Scalepack (Otwinowski & Minor, 1997)' _computing_data_reduction 'Denzo/Scalepack (Otwinowski & Minor, 1997)' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1997)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'Diamond v.3.1d (Crystal Impact GbR, 2006)' _computing_publication_material 'SHELXL-97 (Sheldrick, 1997)' _refine_special_details ; Refinement of F^2^ against ALL reflections. The weighted R-factor wR and goodness of fit S are based on F^2^, conventional R-factors R are based on F, with F set to zero for negative F^2^. The threshold expression of F^2^ > 2sigma(F^2^) is used only for calculating R-factors(gt) etc. and is not relevant to the choice of reflections for refinement. R-factors based on F^2^ are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger. ; _refine_ls_structure_factor_coef Fsqd _refine_ls_matrix_type full _refine_ls_weighting_scheme calc _refine_ls_weighting_details 'calc w=1/[\s^2^(Fo^2^)+(0.0167P)^2^+4.5991P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment constr _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 3280 _refine_ls_number_parameters 219 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0467 _refine_ls_R_factor_gt 0.0254 _refine_ls_wR_factor_ref 0.0576 _refine_ls_wR_factor_gt 0.0512 _refine_ls_goodness_of_fit_ref 1.038 _refine_ls_restrained_S_all 1.038 _refine_ls_shift/su_max 0.000 _refine_ls_shift/su_mean 0.000 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 -0.5000 0.0000 0.5000 0.01879(6) Uani 1 2 d S . . O1 O 0.0740(5) 0.07642(13) 0.6404(6) 0.0632(13) Uani 1 1 d . . . O2 O 0.3443(10) 0.04215(15) 0.9440(7) 0.0977(19) Uani 1 1 d . . . O3 O 0.4264(7) 0.09261(16) 1.1569(6) 0.0816(15) Uani 1 1 d . . . O4 O 0.5108(5) 0.26895(12) 1.0656(4) 0.0420(8) Uani 1 1 d . . . O5 O 0.3020(5) 0.30645(11) 0.8286(4) 0.0419(8) Uani 1 1 d . . . O6 O -0.1528(9) 0.2088(2) 0.3594(6) 0.117(3) Uani 1 1 d . . . O7 O -0.1539(9) 0.1298(2) 0.3554(5) 0.108(2) Uani 1 1 d . . . N1 N -0.2828(5) 0.01730(13) 0.4099(4) 0.0247(7) Uani 1 1 d . . . H1A H -0.2526 -0.0099 0.3880 0.037 Uiso 1 1 d R . . H1B H -0.3521 0.0418 0.3108 0.037 Uiso 1 1 d R . . H1C H -0.1908 0.0397 0.4736 0.037 Uiso 1 1 d R . . N2 N -0.3442(5) 0.03717(12) 0.7285(4) 0.0226(7) Uani 1 1 d . . . H2N H -0.2617 0.0180 0.8234 0.034 Uiso 1 1 d R . . N3 N -0.4087(6) 0.11800(13) 0.6144(5) 0.0314(8) Uani 1 1 d . . . H3D H -0.4936 0.1039 0.5047 0.047 Uiso 1 1 d R . . H3E H -0.3992 0.1544 0.6045 0.047 Uiso 1 1 d R . . N4 N -0.2036(5) 0.10694(13) 0.9089(4) 0.0279(8) Uani 1 1 d . . . N5 N 0.3569(7) 0.08425(14) 0.9978(7) 0.0423(10) Uani 1 1 d . . . N6 N 0.3706(5) 0.26761(13) 0.9173(5) 0.0299(8) Uani 1 1 d . . . N7 N -0.0928(7) 0.16908(19) 0.4296(5) 0.0436(11) Uani 1 1 d . . . C1 C -0.3192(6) 0.08618(15) 0.7510(5) 0.0234(8) Uani 1 1 d . . . C2 C -0.1765(7) 0.16243(16) 0.9359(6) 0.0300(9) Uani 1 1 d . . . H2A H -0.0805 0.1748 0.8883 0.045 Uiso 1 1 calc R . . H2B H -0.1226 0.1700 1.0617 0.045 Uiso 1 1 calc R . . H2C H -0.3081 0.1797 0.8759 0.045 Uiso 1 1 calc R . . C3 C -0.0847(7) 0.07288(18) 1.0533(6) 0.0395(11) Uani 1 1 d . . . H3A H -0.1766 0.0538 1.0922 0.059 Uiso 1 1 calc R . . H3B H 0.0104 0.0934 1.1510 0.059 Uiso 1 1 calc R . . H3C H -0.0078 0.0485 1.0138 0.059 Uiso 1 1 calc R . . C4 C 0.1329(6) 0.11966(16) 0.6996(7) 0.0350(11) Uani 1 1 d . . . C5 C 0.2807(6) 0.12807(15) 0.8792(6) 0.0287(9) Uani 1 1 d . . . C6 C 0.3555(6) 0.17480(15) 0.9506(5) 0.0249(8) Uani 1 1 d . . . H6 H 0.4540 0.1775 1.0682 0.030 Uiso 1 1 calc R . . C7 C 0.2848(6) 0.21826(14) 0.8482(5) 0.0229(8) Uani 1 1 d . . . C8 C 0.1357(6) 0.21562(16) 0.6793(5) 0.0251(9) Uani 1 1 d . . . H8 H 0.0840 0.2461 0.6131 0.030 Uiso 1 1 calc R . . C9 C 0.0639(6) 0.16825(18) 0.6091(6) 0.0292(10) Uani 1 1 d . . . 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 0.02077(10) 0.01170(9) 0.01999(10) -0.00084(11) 0.00431(7) -0.00068(11) O1 0.0268(17) 0.0258(18) 0.121(4) -0.035(2) 0.013(2) -0.0032(14) O2 0.216(6) 0.021(2) 0.094(4) 0.014(2) 0.103(4) 0.024(3) O3 0.084(3) 0.043(2) 0.073(3) 0.023(2) -0.014(3) -0.010(2) O4 0.047(2) 0.0264(17) 0.0356(17) -0.0052(14) -0.0005(15) -0.0073(15) O5 0.057(2) 0.0153(15) 0.0408(19) 0.0047(14) 0.0070(16) -0.0037(14) O6 0.131(5) 0.074(4) 0.060(3) -0.030(3) -0.047(3) 0.057(3) O7 0.179(6) 0.089(4) 0.033(2) -0.014(2) 0.020(3) -0.097(4) N1 0.0259(17) 0.0182(15) 0.0269(18) -0.0023(13) 0.0076(14) -0.0020(13) N2 0.0269(17) 0.0176(16) 0.0202(16) -0.0006(13) 0.0063(14) -0.0019(13) N3 0.044(2) 0.0171(17) 0.0271(18) 0.0019(14) 0.0081(16) 0.0013(16) N4 0.0359(19) 0.0202(17) 0.0252(18) -0.0026(14) 0.0100(15) -0.0039(15) N5 0.050(3) 0.018(2) 0.073(3) 0.009(2) 0.040(2) 0.0042(18) N6 0.036(2) 0.0207(18) 0.031(2) -0.0016(15) 0.0123(16) -0.0034(16) N7 0.041(2) 0.060(3) 0.031(2) -0.022(2) 0.015(2) -0.017(2) C1 0.024(2) 0.024(2) 0.024(2) -0.0024(16) 0.0110(16) -0.0010(16) C2 0.039(2) 0.023(2) 0.032(2) -0.0084(18) 0.019(2) -0.0075(19) C3 0.044(3) 0.032(3) 0.030(2) -0.002(2) 0.002(2) -0.004(2) C4 0.023(2) 0.023(2) 0.067(3) -0.017(2) 0.026(2) -0.0052(18) C5 0.028(2) 0.017(2) 0.048(3) 0.0057(18) 0.022(2) 0.0029(16) C6 0.0230(19) 0.023(2) 0.031(2) 0.0027(17) 0.0142(17) 0.0017(16) C7 0.027(2) 0.0153(18) 0.029(2) -0.0044(16) 0.0135(17) -0.0031(16) C8 0.030(2) 0.022(2) 0.024(2) -0.0004(16) 0.0123(17) 0.0029(17) C9 0.020(2) 0.035(2) 0.032(2) -0.0105(19) 0.0104(18) -0.0045(18) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; 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 N2 2.020(3) . ? Pt1 N2 2.020(3) 3_456 ? Pt1 N1 2.038(3) . ? Pt1 N1 2.038(3) 3_456 ? O1 C4 1.230(5) . ? O2 N5 1.171(6) . ? O3 N5 1.233(6) . ? O4 N6 1.238(5) . ? O5 N6 1.229(4) . ? O6 N7 1.177(6) . ? O7 N7 1.182(6) . ? N1 H1A 0.7827 . ? N1 H1B 1.0015 . ? N1 H1C 0.8769 . ? N2 C1 1.288(5) . ? N2 H2N 0.9181 . ? N3 C1 1.341(5) . ? N3 H3D 0.9430 . ? N3 H3E 0.9538 . ? N4 C1 1.352(5) . ? N4 C3 1.458(5) . ? N4 C2 1.459(5) . ? N5 C5 1.460(6) . ? N6 C7 1.437(5) . ? N7 C9 1.462(6) . ? C2 H2A 0.9800 . ? C2 H2B 0.9800 . ? C2 H2C 0.9800 . ? C3 H3A 0.9800 . ? C3 H3B 0.9800 . ? C3 H3C 0.9800 . ? C4 C9 1.450(6) . ? C4 C5 1.458(6) . ? C5 C6 1.362(6) . ? C6 C7 1.381(5) . ? C6 H6 0.9500 . ? C7 C8 1.382(6) . ? C8 C9 1.369(6) . ? C8 H8 0.9500 . ? 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 N2 Pt1 N2 180.00(19) . 3_456 ? N2 Pt1 N1 91.75(13) . . ? N2 Pt1 N1 88.25(13) 3_456 . ? N2 Pt1 N1 88.25(13) . 3_456 ? N2 Pt1 N1 91.75(13) 3_456 3_456 ? N1 Pt1 N1 180.0 . 3_456 ? Pt1 N1 H1A 102.3 . . ? Pt1 N1 H1B 104.3 . . ? H1A N1 H1B 118.2 . . ? Pt1 N1 H1C 115.0 . . ? H1A N1 H1C 121.8 . . ? H1B N1 H1C 94.5 . . ? C1 N2 Pt1 126.9(3) . . ? C1 N2 H2N 113.9 . . ? Pt1 N2 H2N 118.1 . . ? C1 N3 H3D 118.9 . . ? C1 N3 H3E 131.2 . . ? H3D N3 H3E 109.9 . . ? C1 N4 C3 119.0(3) . . ? C1 N4 C2 122.3(3) . . ? C3 N4 C2 118.4(3) . . ? O2 N5 O3 120.8(5) . . ? O2 N5 C5 121.2(5) . . ? O3 N5 C5 117.9(4) . . ? O5 N6 O4 122.9(4) . . ? O5 N6 C7 119.3(3) . . ? O4 N6 C7 117.9(3) . . ? O6 N7 O7 120.8(5) . . ? O6 N7 C9 119.8(4) . . ? O7 N7 C9 119.4(5) . . ? N2 C1 N3 119.6(4) . . ? N2 C1 N4 122.0(4) . . ? N3 C1 N4 118.4(4) . . ? N4 C2 H2A 109.5 . . ? N4 C2 H2B 109.5 . . ? H2A C2 H2B 109.5 . . ? N4 C2 H2C 109.5 . . ? H2A C2 H2C 109.5 . . ? H2B C2 H2C 109.5 . . ? N4 C3 H3A 109.5 . . ? N4 C3 H3B 109.5 . . ? H3A C3 H3B 109.5 . . ? N4 C3 H3C 109.5 . . ? H3A C3 H3C 109.5 . . ? H3B C3 H3C 109.5 . . ? O1 C4 C9 126.6(5) . . ? O1 C4 C5 122.5(5) . . ? C9 C4 C5 110.9(4) . . ? C6 C5 C4 125.1(4) . . ? C6 C5 N5 115.2(4) . . ? C4 C5 N5 119.7(4) . . ? C5 C6 C7 118.5(4) . . ? C5 C6 H6 120.8 . . ? C7 C6 H6 120.8 . . ? C6 C7 C8 121.9(4) . . ? C6 C7 N6 119.4(4) . . ? C8 C7 N6 118.7(4) . . ? C9 C8 C7 118.8(4) . . ? C9 C8 H8 120.6 . . ? C7 C8 H8 120.6 . . ? C8 C9 C4 124.7(4) . . ? C8 C9 N7 115.1(4) . . ? C4 C9 N7 120.2(4) . . ? loop_ _geom_hbond_atom_site_label_D _geom_hbond_atom_site_label_H _geom_hbond_atom_site_label_A _geom_hbond_distance_DH _geom_hbond_distance_HA _geom_hbond_distance_DA _geom_hbond_angle_DHA _geom_hbond_site_symmetry_A N1 H1A O1 0.78 2.22 2.976(5) 162.6 3_556 N1 H1B O3 1.00 2.06 3.009(5) 156.8 1_454 N1 H1C O7 0.88 2.59 3.151(5) 122.3 . N1 H1C O1 0.88 2.08 2.933(5) 165.6 . N1 H1C O7 0.88 2.59 3.151(5) 122.3 . N3 H3E O4 0.95 2.08 2.987(5) 159.1 4_465 N3 H3E O5 0.95 2.63 3.133(5) 113.4 4_465 N3 H3E N6 0.95 2.68 3.451(5) 138.7 4_465 _diffrn_measured_fraction_theta_max 0.998 _diffrn_reflns_theta_full 27.59 _diffrn_measured_fraction_theta_full 0.998 _refine_diff_density_max 0.908 _refine_diff_density_min -0.796 _refine_diff_density_rms 0.104