# Supplementary Material (ESI) for Dalton Transactions # This journal is (c) The Royal Society of Chemistry 2009 data_global _journal_name_full 'Dalton Trans.' _journal_coden_Cambridge 0222 _publ_contact_author_name 'Peter Sadler' _publ_contact_author_email P.J.SADLER@WARWICK.AC.UK _publ_section_title ; Synthesis,characterisation and photochemistry of PtIV pyridyl azidoacetato complexes ; _publ_requested_coeditor_name S.Moggach@ed.ac.uk loop_ _publ_author_name 'Peter Sadler' 'Robert J. Deeth' 'Nicola J. Farrer' 'Fiona S. MacKay' 'Stephen A Moggach' ; S.Parsons ; 'Luca Salassa' 'Hui-Chung Tai' 'Peter Wood' #===END data_fm135a _database_code_depnum_ccdc_archive 'CCDC 709182' _audit_creation_date 04-07-16 _audit_creation_method CRYSTALS_ver_12.39 _oxford_structure_analysis_title 'fm135a in Cc' _chemical_name_systematic ? _chemical_melting_point ? _cell_length_a 19.3584(7) _cell_length_b 10.1802(4) _cell_length_c 13.8692(4) _cell_angle_alpha 90 _cell_angle_beta 113.816(2) _cell_angle_gamma 90 _cell_volume 2500.49(16) _symmetry_cell_setting Monoclinic _symmetry_space_group_name_H-M C2/c _symmetry_space_group_name_Hall ? loop_ _symmetry_equiv_pos_as_xyz x,y,z -x,-y,-z x+1/2,y+1/2,z -x+1/2,-y+1/2,-z -x,y,-z+1/2 x,-y,z+1/2 -x+1/2,y+1/2,-z+1/2 x+1/2,-y+1/2,z+1/2 loop_ _atom_type_symbol _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_Cromer_Mann_a1 _atom_type_scat_Cromer_Mann_b1 _atom_type_scat_Cromer_Mann_a2 _atom_type_scat_Cromer_Mann_b2 _atom_type_scat_Cromer_Mann_a3 _atom_type_scat_Cromer_Mann_b3 _atom_type_scat_Cromer_Mann_a4 _atom_type_scat_Cromer_Mann_b4 _atom_type_scat_Cromer_Mann_c _atom_type_scat_source C 0.0033 0.0016 2.3100 20.8439 1.0200 10.2075 1.5886 0.5687 0.8650 51.6512 0.2156 'International Tables Vol C 4.2.6.8 and 6.1.1.4' H 0.0000 0.0000 0.4930 10.5109 0.3229 26.1257 0.1402 3.1424 0.0408 57.7998 0.0030 'International Tables Vol C 4.2.6.8 and 6.1.1.4' N 0.0061 0.0033 12.2126 0.0057 3.1322 9.8933 2.0125 28.9975 1.1663 0.5826 -11.5290 'International Tables Vol C 4.2.6.8 and 6.1.1.4' Pt -1.7033 8.3905 27.0059 1.5129 17.7639 8.8117 15.7131 0.4246 5.7837 38.6103 11.6883 'International Tables Vol C 4.2.6.8 and 6.1.1.4' _cell_formula_units_Z 8 # Given Formula = C12 H8 N8 Pt1 # Dc = 2.44 Fooo = 1712.00 Mu = 112.30 M = 459.34 # Found Formula = C12 H8 N8 Pt1 # Dc = 2.44 FOOO = 1712.00 Mu = 112.30 M = 459.34 _chemical_formula_sum 'C12 H8 N8 Pt1' _chemical_formula_moiety 'C12 H8 N8 Pt1' _chemical_compound_source ? _chemical_formula_weight 459.34 _cell_measurement_reflns_used 4879 _cell_measurement_theta_min 2 _cell_measurement_theta_max 29 _cell_measurement_temperature 150 _exptl_crystal_description block _exptl_crystal_colour yellow _exptl_crystal_size_min 0.10 _exptl_crystal_size_mid 0.12 _exptl_crystal_size_max 0.26 _exptl_crystal_density_diffrn 2.440 _exptl_crystal_density_meas ? # Non-dispersive F(000): _exptl_crystal_F_000 1712 _exptl_absorpt_coefficient_mu 11.230 # Sheldrick geometric approximatio 0.26 0.33 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_process_details 'SADABS (Siemens, 1996)' _exptl_absorpt_correction_T_min 0.18 _exptl_absorpt_correction_T_max 0.33 _diffrn_measurement_device_type 'Bruker SMART' _diffrn_radiation_monochromator graphite _diffrn_radiation_type 'Mo K\a' _diffrn_radiation_wavelength 0.71073 _diffrn_measurement_method \w _computing_data_collection 'SMART (Siemens, 1993)' _computing_data_reduction 'SAINT (Siemens ,1995)' _computing_cell_refinement 'SAINT (Siemens ,1995)' _computing_structure_solution 'DIRDIF-96 (Beurskens et al 1996)' _computing_structure_refinement 'CRYSTALS (Betteridge et al 2003)' _computing_publication_material 'CRYSTALS (Betteridge et al 2003)' _computing_molecular_graphics 'CAMERON (Watkin et al 1996)' _diffrn_standards_interval_time ? _diffrn_standards_interval_count ? _diffrn_standards_number 0 _diffrn_standards_decay_% ? _diffrn_ambient_temperature 150 _diffrn_reflns_number 9019 _reflns_number_total 3057 _diffrn_reflns_av_R_equivalents 0.036 # Number of reflections with Friedels Law is 3057 # Number of reflections without Friedels Law is 0 # Theoretical number of reflections is about 3270 _diffrn_reflns_theta_min 2.300 _diffrn_reflns_theta_max 28.824 _diffrn_measured_fraction_theta_max 0.934 _diffrn_reflns_theta_full 27.095 _diffrn_measured_fraction_theta_full 0.998 _diffrn_reflns_limit_h_min -25 _diffrn_reflns_limit_h_max 22 _diffrn_reflns_limit_k_min -13 _diffrn_reflns_limit_k_max 11 _diffrn_reflns_limit_l_min -18 _diffrn_reflns_limit_l_max 18 _reflns_limit_h_min -25 _reflns_limit_h_max 23 _reflns_limit_k_min 0 _reflns_limit_k_max 13 _reflns_limit_l_min 0 _reflns_limit_l_max 18 _oxford_diffrn_Wilson_B_factor 0.00 _oxford_diffrn_Wilson_scale 0.00 _atom_sites_solution_primary direct #heavy,direct,difmap,geom # _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_diff_density_min -1.55 _refine_diff_density_max 3.83 _refine_ls_number_reflns 3057 _refine_ls_number_restraints 0 _refine_ls_number_parameters 190 #_refine_ls_R_factor_ref 0.0367 _refine_ls_wR_factor_ref 0.0825 _refine_ls_goodness_of_fit_ref 0.9328 #_reflns_number_all 3057 _refine_ls_R_factor_all 0.0367 _refine_ls_wR_factor_all 0.0825 # No actual I/u(I) cutoff was used for refinement. The # threshold below is used for "_gt" information ONLY: _reflns_threshold_expression I>2.00u(I) _reflns_number_gt 2725 _refine_ls_R_factor_gt 0.0326 _refine_ls_wR_factor_gt 0.0800 _refine_ls_shift/su_max 0.000642 # choose from: rm (reference molecule of known chirality), # ad (anomolous dispersion - Flack), rmad (rm and ad), # syn (from synthesis), unk (unknown) or . (not applicable). _chemical_absolute_configuration . _refine_ls_structure_factor_coef Fsqd _refine_ls_matrix_type full _refine_ls_hydrogen_treatment noref # none, undef, noref, refall, # refxyz, refU, constr or mixed _refine_ls_weighting_scheme calc _refine_ls_weighting_details ; p=P(6)*max(Fo^2^,0) + (1-P(6))Fc^2^ Method = SHELXL 97 (Sheldrick, 1997) W = 1. / [Sigma^2^(F*)+(P(1)p)^2^+P(2)p+P(4)+P(5)Sin(theta) ] P(i) are: 0.338E-01 0.00 0.00 0.00 0.00 0.333 ; _publ_section_exptl_refinement # see also _refine_ls_hydrogen ; H atoms placed geometrically after each cycle 912_ALERT_3_B Missing FCF Reflections Above STH/L=0.6 ........ 216 #=============================================================================== Resolution & Completeness Statistics (Cumulative) #=============================================================================== Theta sin(th)/Lambda Complete Expected Measured Missing #------------------------------------------------------------------------------- 20.82 0.500 1.000 1309 1309 0 23.01 0.550 1.000 1742 1742 0 25.24 0.600 1.000 2270 2269 1 #----------------------------------------------------------- ACTA Min. Res. ---- 27.51 0.650 0.996 2881 2869 12 29.84 0.700 0.934 3274 3057 217 094_ALERT_2_C Ratio of Maximum / Minimum Residual Density .... 2.47 The difference map is noisy around the Pt atom. 125_ALERT_4_C No _symmetry_space_group_name_Hall Given ....... ? 342_ALERT_3_C Low Bond Precision on C-C bonds (x 1000) Ang ... 10 764_ALERT_4_C Overcomplete CIF Bond List Detected (Rep/Expd) . 1.17 Ratio 779_ALERT_2_C Suspect or Irrelevant (Bond) Angle in CIF ...... 40.60 Deg. N121 -C131 -PT1 1.555 1.555 1.555 779_ALERT_2_C Suspect or Irrelevant (Bond) Angle in CIF ...... 40.60 Deg. N11 -C141 -PT1 1.555 1.555 1.555 779_ALERT_2_C Suspect or Irrelevant (Bond) Angle in CIF ...... 37.50 Deg. N12 -N22 -PT1 1.555 1.555 1.555 797_ALERT_4_C N-Atom in CIF Coordinate List out of Sequence .. N12 911_ALERT_3_C Missing FCF Refl. Between TH(Min) & STH/L=0.6 .. 1 No action. ; # Uequiv = arithmetic mean of Ui i.e. Ueqiv = (U1+U2+U3)/3 # Replace last . with number of unfound hydrogen atoms attached to an atom. # ..._refinement_flags_... # . no refinement constraints S special position constraint on site # G rigid group refinement of site R riding atom # D distance or angle restraint on site T thermal displacement constraints # U Uiso or Uij restraint (rigid bond) P partial occupancy constraint 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_occupancy _atom_site_adp_type _atom_site_refinement_flags_posn _atom_site_refinement_flags_adp _atom_site_refinement_flags_occupancy _atom_site_disorder_assembly _atom_site_disorder_group _atom_site_attached_hydrogens Pt1 Pt -0.045971(12) 0.48585(2) 0.329248(16) 0.0187 1.0000 Uani . . . . . . N11 N 0.0629(3) 0.4857(4) 0.4320(4) 0.0210 1.0000 Uani . . . . . . C21 C 0.1096(4) 0.3848(6) 0.4736(5) 0.0278 1.0000 Uani . . . . . . C31 C 0.1847(4) 0.4026(7) 0.5412(5) 0.0302 1.0000 Uani . . . . . . C41 C 0.2138(4) 0.5256(7) 0.5702(5) 0.0283 1.0000 Uani . . . . . . C51 C 0.1654(3) 0.6355(6) 0.5290(5) 0.0236 1.0000 Uani . . . . . . C61 C 0.1880(4) 0.7710(7) 0.5543(5) 0.0305 1.0000 Uani . . . . . . C71 C 0.1394(4) 0.8706(6) 0.5112(5) 0.0304 1.0000 Uani . . . . . . C81 C 0.0627(4) 0.8460(6) 0.4403(5) 0.0257 1.0000 Uani . . . . . . C91 C 0.0080(4) 0.9437(6) 0.3942(5) 0.0295 1.0000 Uani . . . . . . C101 C -0.0644(4) 0.9084(6) 0.3314(5) 0.0317 1.0000 Uani . . . . . . C111 C -0.0836(4) 0.7756(6) 0.3089(5) 0.0248 1.0000 Uani . . . . . . N121 N -0.0316(3) 0.6810(5) 0.3504(4) 0.0219 1.0000 Uani . . . . . . C131 C 0.0403(3) 0.7150(6) 0.4166(4) 0.0211 1.0000 Uani . . . . . . C141 C 0.0915(3) 0.6104(5) 0.4612(5) 0.0216 1.0000 Uani . . . . . . N12 N -0.0510(3) 0.2860(5) 0.3248(4) 0.0269 1.0000 Uani . . . . . . N22 N -0.0903(3) 0.2285(5) 0.2482(5) 0.0294 1.0000 Uani . . . . . . N32 N -0.1268(4) 0.1626(5) 0.1773(5) 0.0393 1.0000 Uani . . . . . . N13 N -0.1533(3) 0.5120(5) 0.2230(5) 0.0280 1.0000 Uani . . . . . . N23 N -0.2038(3) 0.4393(5) 0.2093(4) 0.0268 1.0000 Uani . . . . . . N33 N -0.2576(3) 0.3746(6) 0.1892(5) 0.0399 1.0000 Uani . . . . . . H21 H 0.0908 0.2979 0.4563 0.0346 1.0000 Uiso . . . . . . H31 H 0.2163 0.3282 0.5677 0.0346 1.0000 Uiso . . . . . . H41 H 0.2652 0.5374 0.6167 0.0310 1.0000 Uiso . . . . . . H61 H 0.2382 0.7902 0.6022 0.0338 1.0000 Uiso . . . . . . H71 H 0.1562 0.9586 0.5282 0.0347 1.0000 Uiso . . . . . . H91 H 0.0213 1.0339 0.4066 0.0362 1.0000 Uiso . . . . . . H101 H -0.1020 0.9742 0.3027 0.0377 1.0000 Uiso . . . . . . H111 H -0.1339 0.7525 0.2639 0.0275 1.0000 Uiso . . . . . . 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 0.01733(13) 0.01692(12) 0.01994(13) 0.00036(7) 0.00563(9) -0.00022(8) N11 0.019(2) 0.021(2) 0.022(2) -0.0018(18) 0.0074(19) 0.0001(19) C21 0.034(4) 0.025(3) 0.028(3) 0.006(2) 0.016(3) 0.008(3) C31 0.026(3) 0.030(3) 0.030(3) 0.005(3) 0.007(3) 0.010(3) C41 0.018(3) 0.036(3) 0.023(3) -0.002(2) 0.000(2) 0.001(3) C51 0.022(3) 0.024(3) 0.023(3) -0.002(2) 0.007(2) 0.000(2) C61 0.021(3) 0.036(4) 0.027(3) -0.008(3) 0.002(3) -0.005(3) C71 0.028(3) 0.028(3) 0.031(3) -0.007(3) 0.007(3) -0.006(3) C81 0.034(3) 0.020(3) 0.027(3) -0.003(2) 0.015(3) -0.004(2) C91 0.039(4) 0.014(3) 0.038(3) 0.003(2) 0.018(3) 0.001(3) C101 0.036(4) 0.020(3) 0.039(4) 0.004(3) 0.014(3) 0.006(3) C111 0.020(3) 0.022(3) 0.027(3) 0.002(2) 0.004(2) 0.005(2) N121 0.024(3) 0.018(2) 0.025(2) 0.0007(19) 0.012(2) 0.000(2) C131 0.020(3) 0.021(3) 0.021(3) 0.000(2) 0.007(2) -0.001(2) C141 0.022(3) 0.018(3) 0.025(3) 0.002(2) 0.010(2) 0.003(2) N12 0.028(3) 0.018(2) 0.031(3) 0.004(2) 0.009(2) 0.000(2) N22 0.024(3) 0.019(2) 0.041(3) 0.007(2) 0.009(2) 0.003(2) N32 0.040(4) 0.021(3) 0.043(3) -0.003(2) 0.002(3) -0.007(2) N13 0.023(3) 0.026(3) 0.028(3) 0.004(2) 0.004(2) 0.000(2) N23 0.027(3) 0.026(3) 0.022(2) 0.001(2) 0.004(2) 0.004(2) N33 0.023(3) 0.035(3) 0.054(4) -0.002(3) 0.009(3) -0.006(2) _refine_ls_extinction_method None _oxford_refine_ls_scale 0.09586(3) loop_ _geom_bond_atom_site_label_1 _geom_bond_site_symmetry_1 _geom_bond_atom_site_label_2 _geom_bond_site_symmetry_2 _geom_bond_distance _geom_bond_publ_flag Pt1 . Pt1 5_555 3.3406(4) yes Pt1 . N11 . 2.011(6) yes Pt1 . N121 . 2.011(5) yes Pt1 . C131 . 2.841(6) yes Pt1 . C141 . 2.847(6) yes Pt1 . N12 . 2.037(5) yes Pt1 . N22 . 2.844(5) yes Pt1 . N13 . 2.022(6) yes N11 . C21 . 1.336(8) yes N11 . C141 . 1.379(7) yes C21 . C31 . 1.386(9) yes C21 . H21 . 0.950 no C31 . C41 . 1.365(9) yes C31 . H31 . 0.950 no C41 . C51 . 1.423(9) yes C41 . H41 . 0.950 no C51 . C61 . 1.447(9) yes C51 . C141 . 1.382(8) yes C61 . C71 . 1.348(9) yes C61 . H61 . 0.950 no C71 . C81 . 1.432(9) yes C71 . H71 . 0.950 no C81 . C91 . 1.405(9) yes C81 . C131 . 1.400(8) yes C91 . C101 . 1.366(10) yes C91 . H91 . 0.950 no C101 . C111 . 1.403(9) yes C101 . H101 . 0.950 no C111 . N121 . 1.344(7) yes C111 . H111 . 0.950 no N121 . C131 . 1.368(7) yes C131 . C141 . 1.416(8) yes N12 . N22 . 1.182(7) yes N22 . N32 . 1.164(8) yes N13 . N23 . 1.179(8) yes N23 . N33 . 1.167(8) yes loop_ _geom_angle_atom_site_label_1 _geom_angle_site_symmetry_1 _geom_angle_atom_site_label_2 _geom_angle_site_symmetry_2 _geom_angle_atom_site_label_3 _geom_angle_site_symmetry_3 _geom_angle _geom_angle_publ_flag Pt1 5_555 Pt1 . N11 . 77.41(14) yes Pt1 5_555 Pt1 . N121 . 90.97(13) yes N11 . Pt1 . N121 . 81.6(2) yes Pt1 5_555 Pt1 . C131 . 84.42(11) yes N11 . Pt1 . C131 . 55.30(18) yes N121 . Pt1 . C131 . 26.30(18) yes Pt1 5_555 Pt1 . C141 . 79.33(11) yes N11 . Pt1 . C141 . 26.49(17) yes N121 . Pt1 . C141 . 55.12(18) yes C131 . Pt1 . C141 . 28.82(16) yes Pt1 5_555 Pt1 . N12 . 90.65(14) yes N11 . Pt1 . N12 . 92.5(2) yes N121 . Pt1 . N12 . 173.4(2) yes C131 . Pt1 . N12 . 147.79(19) yes C141 . Pt1 . N12 . 119.02(19) yes Pt1 5_555 Pt1 . N22 . 84.02(11) yes N11 . Pt1 . N22 . 110.01(17) yes N121 . Pt1 . N22 . 165.86(18) yes C131 . Pt1 . N22 . 163.17(16) yes C141 . Pt1 . N22 . 135.98(16) yes Pt1 5_555 Pt1 . N13 . 100.60(17) yes N11 . Pt1 . N13 . 172.22(19) yes N121 . Pt1 . N13 . 91.0(2) yes C131 . Pt1 . N13 . 117.19(19) yes C141 . Pt1 . N13 . 145.96(18) yes N12 . Pt1 . N22 . 20.68(18) yes N12 . Pt1 . N13 . 95.0(2) yes N22 . Pt1 . N13 . 77.05(18) yes Pt1 . N11 . C21 . 129.8(4) yes Pt1 . N11 . C141 . 112.9(4) yes C21 . N11 . C141 . 117.3(6) yes N11 . C21 . C31 . 122.3(6) yes N11 . C21 . H21 . 118.869 no C31 . C21 . H21 . 118.869 no C21 . C31 . C41 . 121.0(6) yes C21 . C31 . H31 . 119.517 no C41 . C31 . H31 . 119.517 no C31 . C41 . C51 . 118.4(6) yes C31 . C41 . H41 . 120.791 no C51 . C41 . H41 . 120.790 no C41 . C51 . C61 . 124.5(6) yes C41 . C51 . C141 . 117.4(6) yes C61 . C51 . C141 . 118.0(5) yes C51 . C61 . C71 . 121.3(6) yes C51 . C61 . H61 . 119.325 no C71 . C61 . H61 . 119.326 no C61 . C71 . C81 . 121.2(6) yes C61 . C71 . H71 . 119.395 no C81 . C71 . H71 . 119.396 no C71 . C81 . C91 . 124.8(6) yes C71 . C81 . C131 . 117.6(6) yes C91 . C81 . C131 . 117.5(6) yes C81 . C91 . C101 . 119.7(6) yes C81 . C91 . H91 . 120.159 no C101 . C91 . H91 . 120.159 no C91 . C101 . C111 . 120.5(6) yes C91 . C101 . H101 . 119.758 no C111 . C101 . H101 . 119.758 no C101 . C111 . N121 . 120.6(6) yes C101 . C111 . H111 . 119.683 no N121 . C111 . H111 . 119.683 no C111 . N121 . Pt1 . 127.6(4) yes C111 . N121 . C131 . 119.3(5) yes Pt1 . N121 . C131 . 113.1(4) yes C81 . C131 . N121 . 122.3(6) yes C81 . C131 . Pt1 . 162.9(5) yes N121 . C131 . Pt1 . 40.6(3) yes C81 . C131 . C141 . 121.3(6) yes N121 . C131 . C141 . 116.5(5) yes Pt1 . C131 . C141 . 75.8(3) yes C131 . C141 . C51 . 120.5(5) yes C131 . C141 . N11 . 115.9(5) yes C51 . C141 . N11 . 123.6(5) yes C131 . C141 . Pt1 . 75.3(3) yes C51 . C141 . Pt1 . 164.1(4) yes N11 . C141 . Pt1 . 40.6(3) yes Pt1 . N12 . N22 . 121.8(4) yes N12 . N22 . Pt1 . 37.5(3) yes N12 . N22 . N32 . 174.5(6) yes Pt1 . N22 . N32 . 148.1(5) yes Pt1 . N13 . N23 . 125.1(4) yes N13 . N23 . N33 . 174.2(7) yes # Attachment 'cif files (1-6)-2.cif' data_fm171a _database_code_depnum_ccdc_archive 'CCDC 709183' _audit_creation_date 04-31-01 _audit_creation_method CRYSTALS_ver_12-03-99 # fm171a in C2/c _publ_section_exptl_refinement ; H atoms placed geometrically after each cycle 063_ALERT_3_B Crystal Probably too Large for Beam Size ....... 0.82 mm The sample was a needle-like crystal mounted roughly about its axis. #=============================================================================== 062_ALERT_4_C Rescale T(min) & T(max) by ..................... 0.30 125_ALERT_4_C No _symmetry_space_group_name_Hall Given ....... ? 764_ALERT_4_C Overcomplete CIF Bond list Detected (Rep/Expd) . 1.15 Ratio 779_ALERT_2_C Suspect or Irrelevant (Bond) Angle in CIF ...... 39.09 Deg. PT1 -N8 -N7 1.555 1.555 1.555 noted, no action. ; _chemical_name_systematic # IUPAC name, in full ; ? ; _chemical_melting_point ? _refine_ls_matrix_type full _atom_sites_solution_primary Patterson _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment noref # General computing #============================================================= _computing_structure_refinement ; CRYSTALS (Watkin et al 2003) ; _computing_publication_material ; CRYSTALS (Watkin et al 2003) ; _computing_molecular_graphics ; CAMERON (Watkin et al 1996) ; #============================================================= _cell_length_a 10.9346(5) _cell_angle_alpha 90 _cell_length_b 15.3328(8) _cell_angle_beta 94.717(3) _cell_length_c 7.0453(4) _cell_angle_gamma 90 _cell_volume 1177.20(11) _symmetry_cell_setting Monoclinic _symmetry_space_group_name_H-M C2/c loop_ _symmetry_equiv_pos_as_xyz x,y,z -x,-y,-z x+1/2,y+1/2,z -x+1/2,-y+1/2,-z -x,y,-z+1/2 x,-y,z+1/2 -x+1/2,y+1/2,-z+1/2 x+1/2,-y+1/2,z+1/2 # choose from: rm (reference molecule of # known chirality), ad (anomolous # dispersion - ie. Flack param), rmad # (both rm and ad), syn (known from # synthetic pathway), unk (unknown) # or . (not applicable). _chemical_absolute_configuration . loop_ _atom_type_symbol _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_Cromer_Mann_a1 _atom_type_scat_Cromer_Mann_b1 _atom_type_scat_Cromer_Mann_a2 _atom_type_scat_Cromer_Mann_b2 _atom_type_scat_Cromer_Mann_a3 _atom_type_scat_Cromer_Mann_b3 _atom_type_scat_Cromer_Mann_a4 _atom_type_scat_Cromer_Mann_b4 _atom_type_scat_Cromer_Mann_c _atom_type_scat_source 'C ' 0.0033 0.0016 2.3100 20.8439 1.0200 10.2075 1.5886 0.5687 0.8650 51.6512 0.2156 International_Tables_Vol_IV_Table_2.2B 'H ' 0.0000 0.0000 0.4930 10.5109 0.3229 26.1257 0.1402 3.1424 0.0408 57.7998 0.0030 International_Tables_Vol_IV_Table_2.2B 'N ' 0.0061 0.0033 12.2126 0.0057 3.1322 9.8933 2.0125 28.9975 1.1663 0.5826 -11.5290 International_Tables_Vol_IV_Table_2.2B 'Pt ' -1.7033 8.3905 27.0059 1.5129 17.7639 8.8117 15.7131 0.4246 5.7837 38.6103 11.6883 International_Tables_Vol_IV_Table_2.2B _cell_formula_units_Z 4 _chemical_formula_sum ' C10 H8 N8 Pt1 ' _chemical_formula_moiety ' C10 H8 N8 Pt1 ' _chemical_compound_source ; ? ; _chemical_formula_weight 435.32 _cell_measurement_reflns_used 5771 _cell_measurement_theta_min 2 _cell_measurement_theta_max 29 _cell_measurement_temperature 150 _exptl_crystal_description ' needle ' _exptl_crystal_colour ' orange ' _exptl_crystal_size_min 0.10 _exptl_crystal_size_mid 0.10 _exptl_crystal_size_max 0.82 _exptl_crystal_density_diffrn 2.456 _exptl_crystal_density_meas ? # Non-dispersive F(000): _exptl_crystal_F_000 808 _exptl_absorpt_coefficient_mu 11.919 _diffrn_measurement_device_type ; Bruker SMART ; _diffrn_radiation_monochromator graphite _computing_data_collection ; SMART (Siemens, 1993) ; _computing_data_reduction ; SAINT (Siemens ,1995) ; _computing_cell_refinement ; SAINT (Siemens ,1995) ; _computing_structure_solution ; SHELXS 86 (Sheldrick, 1986) ; _diffrn_measurement_method \w _exptl_absorpt_correction_type multi-scan _exptl_absorpt_process_details ; SADABS (Siemens, 1996) ; _exptl_absorpt_correction_T_min 0.470 _exptl_absorpt_correction_T_max 1.000 # Sheldrick geometric definitions 0.30 0.30 _diffrn_standards_interval_time 0 _diffrn_standards_interval_count 0 _diffrn_standards_number 0 _diffrn_standards_decay_% 0.00 _diffrn_ambient_temperature 150 _diffrn_reflns_number 6926 _reflns_number_total 1453 _diffrn_reflns_av_R_equivalents 0.03 # Number of reflections with Friedels Law is 1453 # Number of reflections without Friedels Law is 0 # Theoretical number of reflections is about 1526 _diffrn_reflns_theta_min 2.293 _diffrn_reflns_theta_max 28.731 _diffrn_measured_fraction_theta_max 0.947 _diffrn_reflns_theta_full 27.294 _diffrn_measured_fraction_theta_full 0.998 _diffrn_reflns_limit_h_min -14 _diffrn_reflns_limit_h_max 14 _diffrn_reflns_limit_k_min -20 _diffrn_reflns_limit_k_max 20 _diffrn_reflns_limit_l_min -9 _diffrn_reflns_limit_l_max 9 _reflns_limit_h_min -14 _reflns_limit_h_max 14 _reflns_limit_k_min 0 _reflns_limit_k_max 20 _reflns_limit_l_min 0 _reflns_limit_l_max 9 _refine_diff_density_min -1.00 _refine_diff_density_max 1.48 _refine_ls_number_reflns 1452 _refine_ls_number_restraints 0 _refine_ls_number_parameters 87 #_refine_ls_R_factor_ref 0.0207 _refine_ls_wR_factor_ref 0.0478 _refine_ls_goodness_of_fit_ref 0.8097 #_reflns_number_all 1452 _refine_ls_R_factor_all 0.0207 _refine_ls_wR_factor_all 0.0478 # No actual I/u(I) cutoff was used for refinement. The # threshold below is used for "_gt" information ONLY: _reflns_threshold_expression I>2.00u(I) _reflns_number_gt 1386 _refine_ls_R_factor_gt 0.0192 _refine_ls_wR_factor_gt 0.0471 _refine_ls_shift/su_max 0.001738 _refine_ls_structure_factor_coef Fsqd _refine_ls_weighting_scheme calc _refine_ls_weighting_details ; p=P(6)*max(Fo^2^,0) + (1-P(6))Fc^2^ Method = SHELXL 97 (Sheldrick, 1997) W = 1. / [Sigma^2^(F*)+(P(1)p)^2^+P(2)p+P(4)+P(5)Sin(theta) ] P(i) are: 0.00 0.00 0.00 0.00 0.00 0.333 ; _diffrn_radiation_type 'Mo K\a' _diffrn_radiation_wavelength 0.71073 ## -------------------REFERENCES ----------------------## ## Insert your own references - in alphabetic order _publ_section_references ; Betteridge, P.W., Carruthers, J.R., Cooper, R.I., Prout, K., Watkin, D.J. (2003). J. Appl. Cryst. 36, 1487. Siemens Industrial Automation, Inc (1993) SMART: Area-Detector Software Package; Madison, WI. Siemens Industrial Automation, Inc (1995). SAINT: Area-Detector Integration Software.; Madison, WI. Siemens Industrial Automation, Inc (1996). SADABS: Area-Detector Absorption Correction;: Madison, WI. Sheldrick, G.M. (1986). SHELXS86. Program for the solution of crystal structures. Univ. of Gottingen, Federal Republic of Germany. Sheldrick, G.M. (1997). SHELXL-97. Program for the refinement of crystal structures. Univ. of Gottingen, Federal Republic of Germany. Watkin, D.J., Prout, C.K. & Pearce, L.J. (1996) CAMERON, Chemical Crystallography Laboratory, OXFORD, UK. ; # Uequiv = arithmetic mean of Ui # i.e. Ueqiv = (U1+U2+U3)/3 # Replace trailing . with the number of unfound # hydrogen atoms attaced to relavent atom 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_occupancy _atom_site_adp_type _atom_site_refinement_flags_posn _atom_site_refinement_flags_adp _atom_site_refinement_flags_occupancy _atom_site_refinement_disorder_assembly _atom_site_refinement_disorder_group _atom_site_attached_hydrogens Pt1 Pt 0.5000 0.608369(11) 0.7500 0.0164 1.0000 Uani S T . . . . N1 N 0.3882(3) 0.50833(19) 0.6727(4) 0.0193 1.0000 Uani . . . . . . C2 C 0.4356(3) 0.4279(2) 0.7102(5) 0.0199 1.0000 Uani . . . . . . C3 C 0.3646(4) 0.3537(3) 0.6771(5) 0.0248 1.0000 Uani . . . . . . C4 C 0.2435(3) 0.3628(3) 0.6026(6) 0.0268 1.0000 Uani . . . . . . C5 C 0.1971(3) 0.4449(3) 0.5625(5) 0.0271 1.0000 Uani . . . . . . C6 C 0.2709(3) 0.5170(2) 0.6001(5) 0.0236 1.0000 Uani . . . . . . N7 N 0.6236(3) 0.7011(2) 0.8437(5) 0.0252 1.0000 Uani . . . . . . N8 N 0.5886(3) 0.7646(2) 0.9201(5) 0.0260 1.0000 Uani . . . . . . N9 N 0.5632(3) 0.8276(3) 0.9958(6) 0.0385 1.0000 Uani . . . . . . H31 H 0.3999 0.2945 0.7065 0.0298 1.0000 Uiso . . . . . . H41 H 0.1906 0.3101 0.5782 0.0323 1.0000 Uiso . . . . . . H51 H 0.1107 0.4522 0.5065 0.0323 1.0000 Uiso . . . . . . H61 H 0.2367 0.5766 0.5731 0.0281 1.0000 Uiso . . . . . . 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 0.01516(10) 0.01461(10) 0.01937(11) 0.0000 0.00038(6) 0.0000 N1 0.0186(12) 0.0175(14) 0.0216(14) 0.0002(11) 0.0013(10) -0.0035(11) C2 0.0202(16) 0.0209(17) 0.0186(15) 0.0001(13) 0.0024(12) 0.0004(13) C3 0.0299(18) 0.0217(18) 0.0230(17) -0.0003(14) 0.0027(14) -0.0011(15) C4 0.0249(17) 0.0253(18) 0.0305(19) -0.0017(16) 0.0030(14) -0.0074(15) C5 0.0194(16) 0.031(2) 0.0307(19) -0.0014(16) -0.0009(13) -0.0048(15) C6 0.0196(15) 0.0228(18) 0.0280(18) 0.0013(14) -0.0016(13) 0.0003(13) N7 0.0196(14) 0.0199(15) 0.0357(17) -0.0006(13) 0.0007(12) -0.0018(11) N8 0.0196(14) 0.0229(16) 0.0346(17) 0.0014(13) -0.0036(12) -0.0039(12) N9 0.0284(16) 0.0315(19) 0.054(2) -0.0151(18) -0.0036(15) 0.0001(16) _refine_ls_extinction_method None loop_ _geom_bond_atom_site_label_1 _geom_bond_site_symmetry_1 _geom_bond_atom_site_label_2 _geom_bond_site_symmetry_2 _geom_bond_distance _geom_bond_publ_flag Pt1 . N8 . 2.814(3) yes Pt1 . N7 . 2.034(3) yes Pt1 . N1 . 2.008(3) yes Pt1 . N8 5_656 2.814(3) yes Pt1 . N1 5_656 2.008(3) yes Pt1 . N7 5_656 2.034(3) yes N1 . C6 . 1.349(4) yes N1 . C2 . 1.354(5) yes C2 . C3 . 1.387(5) yes C2 . C2 5_656 1.472(7) yes C3 . H31 . 1.000 no C3 . C4 . 1.391(5) yes C4 . H41 . 1.000 no C4 . C5 . 1.378(6) yes C5 . H51 . 1.000 no C5 . C6 . 1.381(5) yes C6 . H61 . 1.000 no N7 . N8 . 1.190(4) yes N8 . N9 . 1.150(5) yes loop_ _geom_angle_atom_site_label_1 _geom_angle_site_symmetry_1 _geom_angle_atom_site_label_2 _geom_angle_site_symmetry_2 _geom_angle_atom_site_label_3 _geom_angle_site_symmetry_3 _geom_angle _geom_angle_publ_flag N8 . Pt1 . N7 . 21.65(10) yes N8 . Pt1 . N1 . 161.08(11) yes N7 . Pt1 . N1 . 174.36(12) yes N8 . Pt1 . N8 5_656 63.35(13) yes N7 . Pt1 . N8 5_656 74.90(11) yes N1 . Pt1 . N8 5_656 110.74(11) yes N8 . Pt1 . N1 5_656 110.74(11) yes N7 . Pt1 . N1 5_656 94.17(13) yes N1 . Pt1 . N1 5_656 80.40(17) yes N8 5_656 Pt1 . N1 5_656 161.08(11) yes N8 . Pt1 . N7 5_656 74.90(11) yes N7 . Pt1 . N7 5_656 91.29(18) yes N1 . Pt1 . N7 5_656 94.17(13) yes N8 5_656 Pt1 . N7 5_656 21.65(10) yes N1 5_656 Pt1 . N7 5_656 174.36(12) yes C6 . N1 . C2 . 120.0(3) yes C6 . N1 . Pt1 . 124.5(3) yes C2 . N1 . Pt1 . 115.3(2) yes C3 . C2 . N1 . 121.0(3) yes C3 . C2 . C2 5_656 124.6(2) yes N1 . C2 . C2 5_656 114.38(18) yes H31 . C3 . C4 . 120.557 no H31 . C3 . C2 . 120.557 no C4 . C3 . C2 . 118.9(4) yes H41 . C4 . C5 . 120.255 no H41 . C4 . C3 . 120.255 no C5 . C4 . C3 . 119.5(4) yes H51 . C5 . C6 . 120.234 no H51 . C5 . C4 . 120.234 no C6 . C5 . C4 . 119.5(3) yes H61 . C6 . N1 . 119.466 no H61 . C6 . C5 . 119.466 no N1 . C6 . C5 . 121.1(3) yes N8 . N7 . Pt1 . 119.3(2) yes N9 . N8 . Pt1 . 145.7(3) yes N9 . N8 . N7 . 175.2(4) yes Pt1 . N8 . N7 . 39.09(18) yes #===END data_fm185a _database_code_depnum_ccdc_archive 'CCDC 709184' _audit_creation_date 06-04-14 _audit_creation_method CRYSTALS_ver_12.82 _oxford_structure_analysis_title 'trial in I2' _chemical_name_systematic ? _chemical_melting_point ? _cell_length_a 11.6121(5) _cell_length_b 3.8371(2) _cell_length_c 14.1714(9) _cell_angle_alpha 90 _cell_angle_beta 102.756(2) _cell_angle_gamma 90 _cell_volume 615.85(6) _symmetry_cell_setting Monoclinic _symmetry_space_group_name_H-M 'I 1 2 1 ' _symmetry_space_group_name_Hall 'I 2y' loop_ _symmetry_equiv_pos_as_xyz x,y,z x+1/2,y+1/2,z+1/2 -x,y,-z -x+1/2,y+1/2,-z+1/2 loop_ _atom_type_symbol _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_Cromer_Mann_a1 _atom_type_scat_Cromer_Mann_b1 _atom_type_scat_Cromer_Mann_a2 _atom_type_scat_Cromer_Mann_b2 _atom_type_scat_Cromer_Mann_a3 _atom_type_scat_Cromer_Mann_b3 _atom_type_scat_Cromer_Mann_a4 _atom_type_scat_Cromer_Mann_b4 _atom_type_scat_Cromer_Mann_c _atom_type_scat_source C 0.0033 0.0016 2.3100 20.8439 1.0200 10.2075 1.5886 0.5687 0.8650 51.6512 0.2156 'International Tables Vol C 4.2.6.8 and 6.1.1.4' H 0.0000 0.0000 0.4930 10.5109 0.3229 26.1257 0.1402 3.1424 0.0408 57.7998 0.0030 'International Tables Vol C 4.2.6.8 and 6.1.1.4' N 0.0061 0.0033 12.2126 0.0057 3.1322 9.8933 2.0125 28.9975 1.1663 0.5826 -11.5290 'International Tables Vol C 4.2.6.8 and 6.1.1.4' Pt -1.7033 8.3905 27.0059 1.5129 17.7639 8.8117 15.7131 0.4246 5.7837 38.6103 11.6883 'International Tables Vol C 4.2.6.8 and 6.1.1.4' _cell_formula_units_Z 2 # Given Formula = C10 H10 N8 Pt1 # Dc = 2.36 Fooo = 408.00 Mu = 113.92 M = 218.67 # Found Formula = C10 H10 N8 Pt1 # Dc = 2.36 FOOO = 408.00 Mu = 113.92 M = 218.67 _chemical_formula_sum 'C10 H10 N8 Pt1' _chemical_formula_moiety 'C10 H10 N8 Pt1' _chemical_compound_source ? _chemical_formula_weight 437.33 _cell_measurement_reflns_used 2896 _cell_measurement_theta_min 5 _cell_measurement_theta_max 58 _cell_measurement_temperature 150 _exptl_crystal_description needle _exptl_crystal_colour yellow _exptl_crystal_size_min 0.05 _exptl_crystal_size_mid 0.15 _exptl_crystal_size_max 0.51 _exptl_crystal_density_diffrn 2.358 _exptl_crystal_density_meas ? # Non-dispersive F(000): _exptl_crystal_F_000 408.000 _exptl_absorpt_coefficient_mu 11.392 # Sheldrick geometric approximatio 0.18 0.57 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_process_details 'SADABS (Siemens, 1996)' _exptl_absorpt_correction_T_min 0.20 _exptl_absorpt_correction_T_max 0.57 _diffrn_measurement_device_type 'Bruker SMART' _diffrn_radiation_monochromator graphite _diffrn_radiation_type 'Mo K\a' _diffrn_radiation_wavelength 0.71073 _diffrn_measurement_method \w _computing_data_collection 'SMART (Siemens, 1993)' _computing_data_reduction 'SAINT (Siemens ,1995)' _computing_cell_refinement 'SAINT (Siemens ,1995)' _computing_structure_solution 'SIR92 (Altomare et al., 1994)' _computing_structure_refinement 'CRYSTALS (Betteridge et al., 2003)' _computing_publication_material 'CRYSTALS (Betteridge et al., 2003)' _computing_molecular_graphics 'CAMERON (Watkin et al., 1996)' _diffrn_standards_interval_time ? _diffrn_standards_interval_count ? _diffrn_standards_number 0 _diffrn_standards_decay_% ? _diffrn_ambient_temperature 150 _diffrn_reflns_number 2838 _reflns_number_total 1429 _diffrn_reflns_av_R_equivalents 0.045 # Number of reflections with Friedels Law is 1429 # Number of reflections without Friedels Law is 1429 # Theoretical number of reflections is about 805 _diffrn_reflns_theta_min 2.058 _diffrn_reflns_theta_max 28.826 _diffrn_measured_fraction_theta_max 0.916 _diffrn_reflns_theta_full 27.097 _diffrn_measured_fraction_theta_full 0.997 _diffrn_reflns_limit_h_min -15 _diffrn_reflns_limit_h_max 15 _diffrn_reflns_limit_k_min -5 _diffrn_reflns_limit_k_max 5 _diffrn_reflns_limit_l_min -18 _diffrn_reflns_limit_l_max 18 _reflns_limit_h_min -15 _reflns_limit_h_max 14 _reflns_limit_k_min -5 _reflns_limit_k_max 5 _reflns_limit_l_min 0 _reflns_limit_l_max 18 _oxford_diffrn_Wilson_B_factor 1.10 _oxford_diffrn_Wilson_scale 5.51 _atom_sites_solution_primary direct #heavy,direct,difmap,geom # _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_diff_density_min -1.43 _refine_diff_density_max 4.09 _refine_ls_number_reflns 1423 _refine_ls_number_restraints 13 _refine_ls_number_parameters 71 #_refine_ls_R_factor_ref 0.0264 _refine_ls_wR_factor_ref 0.0690 _refine_ls_goodness_of_fit_ref 1.0246 #_reflns_number_all 1423 _refine_ls_R_factor_all 0.0264 _refine_ls_wR_factor_all 0.0690 # No actual I/u(I) cutoff was used for refinement. The # threshold below is used for "_gt" information ONLY: _reflns_threshold_expression I>2.00u(I) _reflns_number_gt 1423 _refine_ls_R_factor_gt 0.0264 _refine_ls_wR_factor_gt 0.0690 _refine_ls_shift/su_max 0.004000 _refine_ls_abs_structure_Flack 0.51(3) _refine_ls_abs_structure_details 'Flack, 0 Friedel-pairs' # choose from: rm (reference molecule of known chirality), # ad (anomolous dispersion - Flack), rmad (rm and ad), # syn (from synthesis), unk (unknown) or . (not applicable). _chemical_absolute_configuration ad _refine_ls_structure_factor_coef Fsqd _refine_ls_matrix_type full _refine_ls_hydrogen_treatment refu # none, undef, noref, refall, # refxyz, refU, constr or mixed _refine_ls_weighting_scheme calc _refine_ls_weighting_details ; Method, part 1, Chebychev polynomial, (Watkin, 1994, Prince, 1982) [weight] = 1.0/[A~0~*T~0~(x)+A~1~*T~1~(x) ... +A~n-1~]*T~n-1~(x)] where A~i~ are the Chebychev coefficients listed below and x= Fcalc/Fmax Method = Robust Weighting (Prince, 1982) W = [weight] * [1-(deltaF/6*sigmaF)^2^]^2^ A~i~ are: 767. -882. 579. ; _publ_section_exptl_refinement ; 129_ALERT_4_A Unusual Space group Specified .................. I 1 2 1 128_ALERT_4_C Non-standard setting of Space group C2 .... I2 120_ALERT_1_C Reported SPGR I 1 2 1 Inconsistent with Explicit I2 The non-standard setting reduces the beta angle substantially (ca. 120 to 102 degrees, and therefore reduces correlations. 374_ALERT_2_A Long N - N Bond N9 - N10 ... 1.52 Ang. Although long, this N-N distance is not the longest. The data may also be bias due to the Pt sitting at the origin. 301_ALERT_3_B Main Residue Disorder ......................... 39.00 Perc. This is caused by a disordered pyr ring. 033_ALERT_2_C Flack Parameter Value Deviates from Zero ....... 0.51 060_ALERT_3_C Ratio Tmax/Tmin (Exp-to-Rep) (too) Large ....... 1.41 094_ALERT_2_C Ratio of Maximum / Minimum Residual Density .... 2.86 795_ALERT_4_C C-Atom in CIF Coordinate List out of Sequence .. C12 797_ALERT_4_C N-Atom in CIF Coordinate List out of Sequence .. N1 No action taken. 912_ALERT_3_C # Missing FCF Reflections Above STH/L=0.6 ...... 78 #=============================================================================== Resolution & Completeness Statistics (Cumulative) #=============================================================================== Theta sin(th)/Lambda Complete Expected Measured Missing #------------------------------------------------------------------------------- 20.82 0.500 1.000 386 386 0 23.01 0.550 1.000 502 502 0 25.24 0.600 1.000 645 645 0 #----------------------------------------------------------- ACTA Min. Res. ---- 27.51 0.650 0.994 803 798 5 28.83 0.678 0.916 925 847 78 ; # Insert your own references if required - in alphabetical order _publ_section_references ; Altomare, A., Cascarano, G., Giacovazzo G., Guagliardi A., Burla M.C., Polidori, G. & Camalli, M. (1994). J. Appl. Cryst. (27), 435-435 Betteridge, P.W., Carruthers, J.R., Cooper, R.I., Prout, K., & Watkin, D.J. (2003). J. Appl. Cryst. 36, 1487. Prince, E. Mathematical Techniques in Crystallography and Materials Science Springer-Verlag, New York, 1982. Siemens Industrial Automation, Inc (1993). SMART: Area-Detector Software Package; Madison, WI. Siemens Industrial Automation, Inc (1995). SAINT: Area-Detector Integration Software.; Madison, WI. Siemens Industrial Automation, Inc (1996). SADABS: Area-Detector Absorption Correction;: Madison, WI. Watkin D.J. (1994). Acta Cryst, A50, 411-437 Watkin, D.J., Prout, C.K. & Pearce, L.J. (1996). CAMERON, Chemical Crystallography Laboratory, OXFORD, UK. ; # Uequiv = arithmetic mean of Ui i.e. Ueqiv = (U1+U2+U3)/3 # Replace last . with number of unfound hydrogen atomsattached to an atom. # ..._refinement_flags_... # . no refinement constraints S special position constraint on site # G rigid group refinement of site R riding atom # D distance or angle restraint on site T thermal displacement constraints # U Uiso or Uij restraint (rigid bond) P partial occupancy constraint 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_occupancy _atom_site_adp_type _atom_site_refinement_flags_posn _atom_site_refinement_flags_adp _atom_site_refinement_flags_occupancy _atom_site_disorder_assembly _atom_site_disorder_group _atom_site_attached_hydrogens Pt1 Pt 1.0000 0.1250(11) 1.0000 0.0145 1.0000 Uani S T . . . . N8 N 1.1697(6) -0.027(2) 1.0544(5) 0.0208 1.0000 Uani . . . . . . N9 N 1.2323(6) -0.1636(19) 1.0095(5) 0.0196 1.0000 Uani D . . . . . N1 N 0.9889(17) 0.189(7) 1.1372(16) 0.0156 0.5346(7) Uani D . P . 1 . C2 C 1.079(2) 0.350(5) 1.1994(13) 0.0156 0.5346(7) Uani D . P . 1 . C3 C 1.0843(16) 0.430(4) 1.2962(12) 0.0156 0.5346(7) Uani D . P . 1 . C4 C 0.9923(14) 0.307(3) 1.3368(13) 0.0156 0.5346(7) Uani D . P . 1 . C5 C 0.8985(16) 0.141(7) 1.2743(13) 0.0156 0.5346(7) Uani D . P . 1 . C6 C 0.901(2) 0.076(8) 1.1781(14) 0.0156 0.5346(7) Uani D . P . 1 . C13 C 1.0815(18) -0.134(5) 1.3012(15) 0.0156 0.4654(7) Uani D . P . 2 . C12 C 1.083(2) -0.131(6) 1.2029(14) 0.0156 0.4654(7) Uani D . P . 2 . C16 C 0.897(2) 0.162(10) 1.1703(16) 0.0156 0.4654(7) Uani D . P . 2 . N11 N 0.991(2) 0.029(8) 1.142(2) 0.0156 0.4654(7) Uani D . P . 2 . C14 C 0.9824(17) -0.010(5) 1.3318(16) 0.0156 0.4654(7) Uani D . P . 2 . C15 C 0.8894(19) 0.150(6) 1.2673(15) 0.0156 0.4654(7) Uani D . P . 2 . N10 N 1.3023(7) -0.450(2) 0.9735(6) 0.0325 1.0000 Uani . . . . . . H111 H 1.1429 -0.2335 1.1804 0.0185 0.4650(7) Uani . . P . 2 . H112 H 1.1454 -0.2183 1.3456 0.0185 0.4650(7) Uani . . P . 2 . H113 H 0.9788 -0.0332 1.3959 0.0185 0.4650(7) Uani . . P . 2 . H114 H 0.8260 0.2430 1.2878 0.0185 0.4650(7) Uani . . P . 2 . H115 H 0.8362 0.2624 1.1253 0.0185 0.4650(7) Uani . . P . 2 . H11 H 1.1431 0.4127 1.1750 0.0185 0.5350(7) Uani . . P . 1 . H12 H 1.1458 0.5583 1.3320 0.0185 0.5350(7) Uani . . P . 1 . H13 H 0.9936 0.3348 1.4013 0.0185 0.5350(7) Uani . . P . 1 . H14 H 0.8340 0.0713 1.2973 0.0185 0.5350(7) Uani . . P . 1 . H15 H 0.8398 -0.0482 1.1406 0.0185 0.5350(7) Uani . . P . 1 . 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 0.01172(15) 0.02169(17) 0.00953(15) 0.0000 0.00127(8) 0.0000 N8 0.013(3) 0.035(3) 0.013(3) -0.006(2) 0.000(2) 0.003(2) N9 0.023(3) 0.021(3) 0.015(3) -0.001(2) 0.005(2) -0.002(2) N1 0.0154(7) 0.0154(7) 0.0154(7) -0.0014(7) 0.0023(7) -0.0014(7) C2 0.0154(7) 0.0154(7) 0.0154(7) -0.0014(7) 0.0023(7) -0.0014(7) C3 0.0154(7) 0.0154(7) 0.0154(7) -0.0014(7) 0.0023(7) -0.0014(7) C4 0.0154(7) 0.0154(7) 0.0154(7) -0.0014(7) 0.0023(7) -0.0014(7) C5 0.0154(7) 0.0154(7) 0.0154(7) -0.0014(7) 0.0023(7) -0.0014(7) C6 0.0154(7) 0.0154(7) 0.0154(7) -0.0014(7) 0.0023(7) -0.0014(7) C13 0.0154(7) 0.0154(7) 0.0154(7) -0.0014(7) 0.0023(7) -0.0014(7) C12 0.0154(7) 0.0154(7) 0.0154(7) -0.0014(7) 0.0023(7) -0.0014(7) C16 0.0154(7) 0.0154(7) 0.0154(7) -0.0014(7) 0.0023(7) -0.0014(7) N11 0.0154(7) 0.0154(7) 0.0154(7) -0.0014(7) 0.0023(7) -0.0014(7) C14 0.0154(7) 0.0154(7) 0.0154(7) -0.0014(7) 0.0023(7) -0.0014(7) C15 0.0154(7) 0.0154(7) 0.0154(7) -0.0014(7) 0.0023(7) -0.0014(7) N10 0.022(3) 0.049(9) 0.029(3) 0.006(3) 0.010(2) -0.011(3) H111 0.0185(7) 0.0185(7) 0.0185(7) 0.0000(7) 0.0041(7) 0.0000(7) H112 0.0185(7) 0.0185(7) 0.0185(7) 0.0000(7) 0.0041(7) 0.0000(7) H113 0.0185(7) 0.0185(7) 0.0185(7) 0.0000(7) 0.0041(7) 0.0000(7) H114 0.0185(7) 0.0185(7) 0.0185(7) 0.0000(7) 0.0041(7) 0.0000(7) H115 0.0185(7) 0.0185(7) 0.0185(7) 0.0000(7) 0.0041(7) 0.0000(7) H11 0.0185(7) 0.0185(7) 0.0185(7) 0.0000(7) 0.0041(7) 0.0000(7) H12 0.0185(7) 0.0185(7) 0.0185(7) 0.0000(7) 0.0041(7) 0.0000(7) H13 0.0185(7) 0.0185(7) 0.0185(7) 0.0000(7) 0.0041(7) 0.0000(7) H14 0.0185(7) 0.0185(7) 0.0185(7) 0.0000(7) 0.0041(7) 0.0000(7) H15 0.0185(7) 0.0185(7) 0.0185(7) 0.0000(7) 0.0041(7) 0.0000(7) _refine_ls_extinction_method None _oxford_refine_ls_scale 0.4406(12) loop_ _geom_bond_atom_site_label_1 _geom_bond_site_symmetry_1 _geom_bond_atom_site_label_2 _geom_bond_site_symmetry_2 _geom_bond_distance _geom_bond_publ_flag Pt1 . N8 3_757 2.036(7) yes Pt1 . N1 3_757 1.992(19) yes Pt1 . N8 . 2.036(7) yes Pt1 . N1 . 1.992(19) yes N8 . N9 . 1.188(10) yes N9 . N10 . 1.521(11) yes N1 . C2 . 1.357(9) yes N1 . C6 . 1.354(8) yes C2 . C3 . 1.394(9) yes C2 . H11 . 0.920 no C3 . C4 . 1.402(9) yes C3 . H12 . 0.921 no C4 . C5 . 1.397(10) yes C4 . H13 . 0.918 no C5 . C6 . 1.391(8) yes C5 . H14 . 0.920 no C6 . H15 . 0.919 no C13 . C12 . 1.396(9) yes C13 . C14 . 1.400(9) yes C13 . H112 . 0.919 no C12 . N11 . 1.357(9) yes C12 . H111 . 0.919 no C16 . N11 . 1.354(9) yes C16 . C15 . 1.397(9) yes C16 . H115 . 0.921 no C14 . C15 . 1.394(9) yes C14 . H113 . 0.922 no C15 . H114 . 0.920 no loop_ _geom_angle_atom_site_label_1 _geom_angle_site_symmetry_1 _geom_angle_atom_site_label_2 _geom_angle_site_symmetry_2 _geom_angle_atom_site_label_3 _geom_angle_site_symmetry_3 _geom_angle _geom_angle_publ_flag N8 3_757 Pt1 . N1 3_757 86.1(7) yes N8 3_757 Pt1 . N8 . 146.7(4) yes N1 3_757 Pt1 . N8 . 98.0(5) yes N8 3_757 Pt1 . N1 . 98.0(5) yes N1 3_757 Pt1 . N1 . 165.8(17) yes N8 . Pt1 . N1 . 86.1(7) yes Pt1 . N8 . N9 . 125.4(5) yes N8 . N9 . N10 . 159.1(7) yes Pt1 . N1 . C2 . 118.9(14) yes Pt1 . N1 . C6 . 126.6(13) yes C2 . N1 . C6 . 114(2) yes N1 . C2 . C3 . 127(2) yes N1 . C2 . H11 . 116.5 no C3 . C2 . H11 . 116.6 no C2 . C3 . C4 . 117.2(18) yes C2 . C3 . H12 . 121.4 no C4 . C3 . H12 . 121.5 no C3 . C4 . C5 . 116.9(17) yes C3 . C4 . H13 . 121.5 no C5 . C4 . H13 . 121.6 no C4 . C5 . C6 . 121.4(18) yes C4 . C5 . H14 . 119.3 no C6 . C5 . H14 . 119.2 no C5 . C6 . N1 . 123(2) yes C5 . C6 . H15 . 118.7 no N1 . C6 . H15 . 118.5 no C12 . C13 . C14 . 120(2) yes C12 . C13 . H112 . 120.2 no C14 . C13 . H112 . 120.1 no C13 . C12 . N11 . 118(2) yes C13 . C12 . H111 . 121.2 no N11 . C12 . H111 . 121.2 no N11 . C16 . C15 . 121(3) yes N11 . C16 . H115 . 119.8 no C15 . C16 . H115 . 119.6 no C12 . N11 . C16 . 124(3) yes C12 . N11 . Pt1 . 120.1(17) yes C16 . N11 . Pt1 . 116.0(17) yes C13 . C14 . C15 . 121(2) yes C13 . C14 . H113 . 119.4 no C15 . C14 . H113 . 119.4 no C16 . C15 . C14 . 117(2) yes C16 . C15 . H114 . 121.5 no C14 . C15 . H114 . 121.5 no #===END data_ps0564 _database_code_depnum_ccdc_archive 'CCDC 709185' _audit_creation_method SHELXL-97 _audit_creation_date 05-12-19 _chemical_compound_source 'Fiona Mackay FM05D' _exptl_crystal_recrystallization_method ; >From water at 4degC. ; _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety '[Pt(Bipy)(OAc)(N3)]' _chemical_formula_sum 'C14 H14 N8 O4 Pt' _chemical_formula_weight 553.42 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 Pbcn _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, y, -z+1/2' 'x+1/2, -y+1/2, -z' '-x, -y, -z' 'x-1/2, y-1/2, -z-1/2' 'x, -y, z-1/2' '-x-1/2, y-1/2, z' _cell_length_a 8.0488(4) _cell_length_b 14.1103(7) _cell_length_c 15.3280(7) _cell_angle_alpha 90.00 _cell_angle_beta 90.00 _cell_angle_gamma 90.00 _cell_volume 1740.82(15) _cell_formula_units_Z 4 _cell_measurement_temperature 150(2) _cell_measurement_reflns_used 5495 _cell_measurement_theta_min 2.5 _cell_measurement_theta_max 20.5 _exptl_crystal_description 'plate deveopled in (001)' _exptl_crystal_colour Yellow _exptl_crystal_size_max 0.84 _exptl_crystal_size_mid 0.55 _exptl_crystal_size_min 0.04 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 2.112 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1056 _exptl_absorpt_coefficient_mu 8.101 _exptl_absorpt_correction_type 'Integration + Multiscan' _exptl_absorpt_correction_T_min 0.05796 _exptl_absorpt_correction_T_max 0.72506 _exptl_absorpt_process_details 'Sadabs Tmin/max = 0.718' _exptl_special_details ; Data collection strategy optimised with COSMO. Oxford Crysosystems LT device. ; _diffrn_ambient_temperature 150(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'Bruker Smart Apex ccd' _diffrn_measurement_method 'Omega and Phi' _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 21880 _diffrn_reflns_av_R_equivalents 0.0377 _diffrn_reflns_av_sigmaI/netI 0.0215 _diffrn_reflns_limit_h_min -11 _diffrn_reflns_limit_h_max 10 _diffrn_reflns_limit_k_min -19 _diffrn_reflns_limit_k_max 18 _diffrn_reflns_limit_l_min -18 _diffrn_reflns_limit_l_max 21 _diffrn_reflns_theta_min 2.66 _diffrn_reflns_theta_max 29.61 _reflns_number_total 2307 _reflns_number_gt 1738 _reflns_threshold_expression >2sigma(I) _computing_data_collection Smart _computing_cell_refinement Saint _computing_data_reduction Saint _computing_structure_solution DIRDIF _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics XP _computing_publication_material 'XCIF, PLATON' _refine_special_details ; Ligands: 1: azide 2: Bipy 3: acetate The Pt sits on a 2-fold axis. Two stage absorption correction. Gaussian integration first, with residual errors treated with the Multiscan procedure Sadabs. Checkcif output: 761_ALERT_1_A CIF Contains no X-H Bonds ...................... ? 762_ALERT_1_A CIF Contains no X-Y-H or H-Y-H Angles .......... ? No action taken. 063_ALERT_3_B Crystal Probably too Large for Beam Size ....... 0.84 mm The sample crystallised as plates which shattered when cut. 912_ALERT_3_B # Missing FCF Reflections Above STH/L=0.6 ...... 140 The data collection strategy used aimed to achieve a complete data set to 2\q = 54 deg. Some higher angle data were collected in the process and these have been included in the refinement. #=============================================================================== Resolution & Completeness Statistics (Cumulative) #=============================================================================== Theta sin(th)/Lambda Complete Expected Measured Missing #------------------------------------------------------------------------------- 20.82 0.500 1.000 912 912 0 23.01 0.550 1.000 1214 1214 0 25.24 0.600 1.000 1582 1582 0 #----------------------------------------------------------- ACTA Min. Res. ---- 27.51 0.650 1.000 2001 2000 1 29.61 0.695 0.943 2447 2307 140 042_ALERT_1_C Calc. and Rep. MoietyFormula Strings Differ .... ? The one given is more chemically meaningful. 220_ALERT_2_C Large Non-Solvent N Ueq(max)/Ueq(min) ... 2.60 Ratio The terminal N-atom of the N3- is librating; this is normal for this ligand. 230_ALERT_2_C Hirshfeld Test Diff for O13 - C13 .. 5.05 su No action. Ton Spek; often happens with bonds between heavy & light atoms with good data sets. Probably inadequate modelling of bonding density. 795_ALERT_4_C C-Atom in CIF Coordinate List out of Sequence .. C13 797_ALERT_4_C N-Atom in CIF Coordinate List out of Sequence .. N12 No action taken. ; _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^)+(0.0226P)^2^+2.9003P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary Patterson _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geometric/difmap _refine_ls_hydrogen_treatment 'riding/rotating group (Me)' _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 2307 _refine_ls_number_parameters 124 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0380 _refine_ls_R_factor_gt 0.0243 _refine_ls_wR_factor_ref 0.0582 _refine_ls_wR_factor_gt 0.0531 _refine_ls_goodness_of_fit_ref 1.112 _refine_ls_restrained_S_all 1.112 _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 0.0000 0.233929(12) 0.2500 0.02279(7) Uani 1 2 d S . . N11 N 0.0744(4) 0.3357(2) 0.1657(2) 0.0379(8) Uani 1 1 d . . . N21 N -0.0244(4) 0.4008(3) 0.1554(2) 0.0439(9) Uani 1 1 d . . . N31 N -0.1082(6) 0.4651(3) 0.1425(3) 0.0683(13) Uani 1 1 d . . . N12 N 0.0658(4) 0.1236(2) 0.17198(19) 0.0264(6) Uani 1 1 d . . . C22 C 0.1378(4) 0.1338(3) 0.0938(2) 0.0353(9) Uani 1 1 d . . . H22 H 0.1555 0.1955 0.0707 0.042 Uiso 1 1 calc R . . C32 C 0.1867(5) 0.0549(4) 0.0465(3) 0.0479(12) Uani 1 1 d . . . H32 H 0.2389 0.0622 -0.0087 0.057 Uiso 1 1 calc R . . C42 C 0.1589(6) -0.0334(4) 0.0800(3) 0.0567(14) Uani 1 1 d . . . H42 H 0.1897 -0.0880 0.0476 0.068 Uiso 1 1 calc R . . C52 C 0.0866(6) -0.0432(3) 0.1605(3) 0.0505(12) Uani 1 1 d . . . H52 H 0.0690 -0.1045 0.1844 0.061 Uiso 1 1 calc R . . C62 C 0.0393(4) 0.0370(3) 0.2067(3) 0.0341(9) Uani 1 1 d . . . O13 O -0.2394(3) 0.23290(17) 0.21048(16) 0.0278(5) Uani 1 1 d . . . O23 O -0.1884(3) 0.2219(2) 0.06582(17) 0.0424(7) Uani 1 1 d . . . C13 C -0.2818(4) 0.2213(2) 0.1279(2) 0.0289(8) Uani 1 1 d . . . C23 C -0.4660(4) 0.2052(3) 0.1166(3) 0.0388(9) Uani 1 1 d . . . H23A H -0.5042 0.2377 0.0637 0.058 Uiso 1 1 calc R . . H23B H -0.5254 0.2304 0.1673 0.058 Uiso 1 1 calc R . . H23C H -0.4878 0.1371 0.1113 0.058 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 0.02105(10) 0.02340(11) 0.02393(10) 0.000 -0.00011(7) 0.000 N11 0.0390(17) 0.0376(19) 0.0372(18) 0.0106(15) -0.0011(15) -0.0126(16) N21 0.049(2) 0.038(2) 0.044(2) 0.0134(16) -0.0193(16) -0.0164(18) N31 0.080(3) 0.044(2) 0.082(3) 0.022(2) -0.038(3) -0.002(2) N12 0.0205(12) 0.0306(16) 0.0280(15) -0.0040(13) -0.0023(12) 0.0010(13) C22 0.0235(16) 0.056(3) 0.0268(19) -0.0078(17) 0.0006(14) 0.0015(17) C32 0.0325(19) 0.077(3) 0.034(2) -0.022(2) -0.0061(17) 0.016(2) C42 0.052(3) 0.065(3) 0.054(3) -0.036(3) -0.023(2) 0.030(2) C52 0.059(3) 0.034(2) 0.059(3) -0.013(2) -0.025(2) 0.017(2) C62 0.0308(18) 0.0294(18) 0.042(2) -0.0067(17) -0.0133(16) 0.0054(15) O13 0.0229(11) 0.0347(14) 0.0258(13) 0.0007(11) -0.0018(11) 0.0010(10) O23 0.0390(15) 0.0603(19) 0.0279(14) 0.0017(13) -0.0003(12) -0.0017(14) C13 0.0280(18) 0.0225(17) 0.036(2) 0.0033(15) 0.0000(15) 0.0024(14) C23 0.034(2) 0.041(2) 0.042(2) 0.002(2) -0.0081(15) -0.0027(17) _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 O13 2.020(2) 3 ? Pt1 O13 2.020(2) . ? Pt1 N11 2.022(3) 3 ? Pt1 N11 2.022(3) . ? Pt1 N12 2.033(3) . ? Pt1 N12 2.033(3) 3 ? N11 N21 1.225(5) . ? N21 N31 1.147(5) . ? N12 C22 1.338(4) . ? N12 C62 1.350(5) . ? C22 C32 1.386(6) . ? C32 C42 1.367(7) . ? C42 C52 1.370(7) . ? C52 C62 1.388(5) . ? C62 C62 1.471(8) 3 ? O13 C13 1.320(4) . ? O23 C13 1.213(4) . ? C13 C23 1.510(5) . ? 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 O13 Pt1 O13 179.18(14) 3 . ? O13 Pt1 N11 95.50(12) 3 3 ? O13 Pt1 N11 85.08(12) . 3 ? O13 Pt1 N11 85.08(12) 3 . ? O13 Pt1 N11 95.50(12) . . ? N11 Pt1 N11 89.5(2) 3 . ? O13 Pt1 N12 85.55(11) 3 . ? O13 Pt1 N12 93.82(11) . . ? N11 Pt1 N12 175.25(13) 3 . ? N11 Pt1 N12 95.22(14) . . ? O13 Pt1 N12 93.82(11) 3 3 ? O13 Pt1 N12 85.55(11) . 3 ? N11 Pt1 N12 95.22(14) 3 3 ? N11 Pt1 N12 175.25(13) . 3 ? N12 Pt1 N12 80.07(17) . 3 ? N21 N11 Pt1 115.0(3) . . ? N31 N21 N11 175.2(5) . . ? C22 N12 C62 121.2(3) . . ? C22 N12 Pt1 123.8(3) . . ? C62 N12 Pt1 114.8(3) . . ? N12 C22 C32 120.3(4) . . ? C42 C32 C22 119.3(4) . . ? C32 C42 C52 120.0(4) . . ? C42 C52 C62 119.6(4) . . ? N12 C62 C52 119.6(4) . . ? N12 C62 C62 115.1(2) . 3 ? C52 C62 C62 125.4(3) . 3 ? C13 O13 Pt1 122.3(2) . . ? O23 C13 O13 126.3(3) . . ? O23 C13 C23 121.3(4) . . ? O13 C13 C23 112.5(3) . . ? _diffrn_measured_fraction_theta_max 0.943 _diffrn_reflns_theta_full 27.51 _diffrn_measured_fraction_theta_full 1.000 _refine_diff_density_max 1.267 _refine_diff_density_min -0.891 _refine_diff_density_rms 0.107 #===END data_ps6014 _database_code_depnum_ccdc_archive 'CCDC 709186' _audit_creation_date 06-02-20 _audit_creation_method CRYSTALS_ver_12.83 _chemical_compound_source 'F.Mackay FM38D' _exptl_crystal_recrystallization_method ; >From water at 4 deg C ; _oxford_structure_analysis_title 'ps6014 in P2/n' _chemical_name_systematic ? _chemical_melting_point ? _cell_length_a 7.03030(10) _cell_length_b 11.7849(2) _cell_length_c 11.3271(2) _cell_angle_alpha 90 _cell_angle_beta 101.2360(10) _cell_angle_gamma 90 _cell_volume 920.48(3) _symmetry_cell_setting Monoclinic _symmetry_space_group_name_H-M P2/n _symmetry_space_group_name_Hall '-P 2yac' loop_ _symmetry_equiv_pos_as_xyz x,y,z -x,-y,-z -x+1/2,y,-z+1/2 x+1/2,-y,z+1/2 loop_ _atom_type_symbol _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_Cromer_Mann_a1 _atom_type_scat_Cromer_Mann_b1 _atom_type_scat_Cromer_Mann_a2 _atom_type_scat_Cromer_Mann_b2 _atom_type_scat_Cromer_Mann_a3 _atom_type_scat_Cromer_Mann_b3 _atom_type_scat_Cromer_Mann_a4 _atom_type_scat_Cromer_Mann_b4 _atom_type_scat_Cromer_Mann_c _atom_type_scat_source C 0.0033 0.0016 2.3100 20.8439 1.0200 10.2075 1.5886 0.5687 0.8650 51.6512 0.2156 'International Tables Vol C 4.2.6.8 and 6.1.1.4' H 0.0000 0.0000 0.4930 10.5109 0.3229 26.1257 0.1402 3.1424 0.0408 57.7998 0.0030 'International Tables Vol C 4.2.6.8 and 6.1.1.4' N 0.0061 0.0033 12.2126 0.0057 3.1322 9.8933 2.0125 28.9975 1.1663 0.5826 -11.5290 'International Tables Vol C 4.2.6.8 and 6.1.1.4' O 0.0106 0.0060 3.0485 13.2771 2.2868 5.7011 1.5463 0.3239 0.8670 32.9089 0.2508 'International Tables Vol C 4.2.6.8 and 6.1.1.4' Pt -1.7033 8.3905 27.0059 1.5129 17.7639 8.8117 15.7131 0.4246 5.7837 38.6103 11.6883 'International Tables Vol C 4.2.6.8 and 6.1.1.4' _cell_formula_units_Z 2 # Given Formula = C10 H14 N8 O4 Pt1 # Dc = 1.82 Fooo = 552.00 Mu = 76.50 M = 252.68 # Found Formula = C16 H14 N8 O4 Pt1 # Dc = 2.08 FOOO = 552.00 Mu = 76.65 M = 288.71 _chemical_formula_sum 'C16 H14 N8 O4 Pt1' _chemical_formula_moiety '[Pt(phen)(N3)2(OAc)2]' _chemical_formula_weight 577.43 _cell_measurement_reflns_used 9919 _cell_measurement_theta_min 3 _cell_measurement_theta_max 30 _cell_measurement_temperature 150 _exptl_crystal_description block _exptl_crystal_colour yellow _exptl_crystal_size_min 0.15 _exptl_crystal_size_mid 0.20 _exptl_crystal_size_max 0.35 _exptl_crystal_density_diffrn 2.083 _exptl_crystal_density_meas ? # Non-dispersive F(000): _exptl_crystal_F_000 552 _exptl_absorpt_coefficient_mu 7.665 # Sheldrick geometric approximatio 0.22 0.32 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_process_details 'SADABS (Siemens, 1996)' _exptl_absorpt_correction_T_min 0.17 _exptl_absorpt_correction_T_max 0.32 _diffrn_measurement_device_type 'Bruker SMART' _diffrn_radiation_monochromator graphite _diffrn_radiation_type 'Mo K\a' _diffrn_radiation_wavelength 0.71073 _diffrn_measurement_method 'phi & omega scans' # If a reference occurs more than once, delete the author # and date from subsequent references. _computing_data_collection 'SMART (Siemens, 1993)' _computing_data_reduction SAINT _computing_cell_refinement 'SAINT (Siemens ,1995)' _computing_structure_solution 'DIRDIF-96 (Beurskens et al., 1996)' _computing_structure_refinement 'CRYSTALS (Betteridge et al., 2003)' _computing_publication_material 'CRYSTALS (Betteridge et al., 2003)' _computing_molecular_graphics 'CAMERON (Watkin et al., 1996)' _diffrn_standards_interval_time ? _diffrn_standards_interval_count ? _diffrn_standards_number 0 _diffrn_standards_decay_% ? _diffrn_ambient_temperature 150 _diffrn_reflns_number 14648 _reflns_number_total 2454 _diffrn_reflns_av_R_equivalents 0.027 # Number of reflections with Friedels Law is 2454 # Number of reflections without Friedels Law is 0 # Theoretical number of reflections is about 2575 _diffrn_reflns_reduction_process ; Merged with SORTAV R.H. Blessing, (1987) Cryst. Rev. 1, 3-58 ; _diffrn_reflns_theta_min 1.728 _diffrn_reflns_theta_max 29.544 _diffrn_measured_fraction_theta_max 0.950 _diffrn_reflns_theta_full 28.067 _diffrn_measured_fraction_theta_full 0.999 _diffrn_reflns_limit_h_min -9 _diffrn_reflns_limit_h_max 9 _diffrn_reflns_limit_k_min 0 _diffrn_reflns_limit_k_max 16 _diffrn_reflns_limit_l_min 0 _diffrn_reflns_limit_l_max 15 _reflns_limit_h_min -9 _reflns_limit_h_max 9 _reflns_limit_k_min 0 _reflns_limit_k_max 16 _reflns_limit_l_min 0 _reflns_limit_l_max 15 _atom_sites_solution_primary Patterson # _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_diff_density_min -1.23 _refine_diff_density_max 1.98 _refine_ls_number_reflns 2453 _refine_ls_number_restraints 20 _refine_ls_number_parameters 142 #_refine_ls_R_factor_ref 0.0316 _refine_ls_wR_factor_ref 0.0690 _refine_ls_goodness_of_fit_ref 1.1174 #_reflns_number_all 2453 _refine_ls_R_factor_all 0.0316 _refine_ls_wR_factor_all 0.0690 # No actual I/u(I) cutoff was used for refinement. The # threshold below is used for "_gt" information ONLY: _reflns_threshold_expression I>2.0\s(I) _reflns_number_gt 2402 _refine_ls_R_factor_gt 0.0305 _refine_ls_wR_factor_gt 0.0685 _refine_ls_shift/su_max 0.007449 # choose from: rm (reference molecule of known chirality), # ad (anomolous dispersion - Flack), rmad (rm and ad), # syn (from synthesis), unk (unknown) or . (not applicable). _chemical_absolute_configuration . _refine_ls_structure_factor_coef Fsqd _refine_ls_matrix_type full _refine_ls_hydrogen_treatment 'noref/restrained refall' _refine_ls_weighting_scheme calc _refine_ls_weighting_details ; Method= Modified Sheldrick w=1/[\s^2^(F^2^) + ( 0.03P)^2^ + 2.97P] ,where P=(max(Fo^2^,0) + 2Fc^2^)/3 ; _publ_section_exptl_refinement ; H atoms placed geometrically on the phen after each cycle. The methyl group based on C22 was restrained to have local 3-fold symmetry; a single overall U[iso] was also refined for these atoms. 732_ALERT_1_A Angle Calc 109(2), Rep 109.44(6) ...... 9.90 su-Rat C12 -C22 -H221 1.555 1.555 1.555 732_ALERT_1_A Angle Calc 110(2), Rep 109.44(6) ...... 9.90 su-Rat C12 -C22 -H222 1.555 1.555 1.555 732_ALERT_1_A Angle Calc 109(3), Rep 109.51(6) ...... 9.90 su-Rat H221 -C22 -H222 1.555 1.555 1.555 732_ALERT_1_A Angle Calc 109.4(15), Rep 109.44(6) ...... 9.90 su-Rat C12 -C22 -H223 1.555 1.555 1.555 732_ALERT_1_A Angle Calc 110(4), Rep 109.51(6) ...... 9.90 su-Rat H221 -C22 -H223 1.555 1.555 1.555 732_ALERT_1_A Angle Calc 110(4), Rep 109.50(6) ...... 9.90 su-Rat H222 -C22 -H223 1.555 1.555 1.555 731_ALERT_1_B Bond Calc 0.97(4), Rep 0.973(7) ...... 5.71 su-Rat C22 -H222 1.555 1.555 731_ALERT_1_B Bond Calc 0.97(3), Rep 0.973(7) ...... 4.29 su-Rat C22 -H223 1.555 1.555 731_ALERT_1_C Bond Calc 0.97(2), Rep 0.973(7) ...... 2.86 su-Rat C22 -H221 1.555 1.555 The use of restraints in the refinement mean that off diagonal terms in the variance-covariance matrix are significant, and the diagonal approximation used in Platon/Checkcif is badly in error. 912_ALERT_3_B # Missing FCF Reflections Above STH/L=0.6 ...... 129 The data collection strategy used aimed to achieve a complete data set to 2\q = 54 deg. Some higher angle data were collected in the process and these have been included in the refinement. #=============================================================================== Resolution & Completeness Statistics (Cumulative) #=============================================================================== Theta sin(th)/Lambda Complete Expected Measured Missing #------------------------------------------------------------------------------- 20.82 0.500 1.000 964 964 0 23.01 0.550 1.000 1288 1288 0 25.24 0.600 1.000 1684 1684 0 #----------------------------------------------------------- ACTA Min. Res. ---- 27.51 0.650 1.000 2117 2117 0 29.54 0.694 0.950 2583 2454 129 128_ALERT_4_C Non-standard setting of Space group P2/c .... P2/n 164_ALERT_4_C Nr. of Refined C-H H-Atoms in Heavy-At Struct... 3 232_ALERT_2_C Hirshfeld Test Diff (M-X) Pt1 - N13 .. 5.06 su 797_ALERT_4_C N-Atom in CIF Coordinate List out of Sequence .. N13 No action. ; # Insert your own references if required - in alphabetical order _publ_section_references ; Betteridge, P.W., Carruthers, J.R., Cooper, R.I., Prout, K. & Watkin, D.J. (2003). J. Appl. Cryst. 36, 1487. Beurskens, P.T., Beurskens, G., Bosman, W.P., de Gelder, R., Garcia Granda, S., Gould, R.O., Israel, R. & Smits J.M.M. (1996). University of Nijmegen, Toernooiveld 1, 6525 ED Nijmegen, The Netherlands. Larson, A.C. (1970) Crystallographic Computing, Ed Ahmed, F.R., Munksgaard, Copenhagen, 291-294. Siemens Industrial Automation, Inc (1993). SMART: Area-Detector Software Package; Madison, WI. Siemens Industrial Automation, Inc (1995). SAINT: Area-Detector Integration Software.; Madison, WI. Siemens Industrial Automation, Inc (1996). SADABS: Area-Detector Absorption Correction;: Madison, WI. Watkin, D.J., Prout, C.K. & Pearce, L.J. (1996). CAMERON, Chemical Crystallography Laboratory, Oxford, UK. ; # Uequiv = arithmetic mean of Ui i.e. Ueqiv = (U1+U2+U3)/3 # Replace last . with number of unfound hydrogen atomsattached to an atom. # ..._refinement_flags_... # . no refinement constraints S special position constraint on site # G rigid group refinement of site R riding atom # D distance or angle restraint on site T thermal displacement constraints # U Uiso or Uij restraint (rigid bond) P partial occupancy constraint 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_occupancy _atom_site_adp_type _atom_site_refinement_flags_posn _atom_site_refinement_flags_adp _atom_site_refinement_flags_occupancy _atom_site_disorder_assembly _atom_site_disorder_group _atom_site_attached_hydrogens Pt1 Pt 0.2500 0.145251(17) 0.2500 0.0283 1.0000 Uani S T . . . . N11 N 0.0381(6) 0.0299(3) 0.1904(4) 0.0455 1.0000 Uani . . . . . . N21 N 0.0808(6) -0.0550(4) 0.1479(3) 0.0406 1.0000 Uani . . . . . . N31 N 0.1044(8) -0.1424(4) 0.1069(5) 0.0593 1.0000 Uani . . . . . . O12 O 0.1644(5) 0.1233(3) 0.4069(3) 0.0425 1.0000 Uani . . . . . . O22 O 0.1817(6) 0.2999(3) 0.4767(3) 0.0543 1.0000 Uani . . . . . . C12 C 0.1528(6) 0.1991(4) 0.4870(4) 0.0364 1.0000 Uani D . . . . . C22 C 0.0897(9) 0.1495(5) 0.5957(5) 0.0518 1.0000 Uani D . . . . . N13 N 0.4351(5) 0.2774(3) 0.3068(3) 0.0328 1.0000 Uani . . . . . . C23 C 0.6175(7) 0.2726(4) 0.3660(4) 0.0406 1.0000 Uani . . . . . . C33 C 0.7221(8) 0.3711(5) 0.4040(5) 0.0491 1.0000 Uani . . . . . . C43 C 0.6373(9) 0.4750(5) 0.3785(5) 0.0513 1.0000 Uani . . . . . . C53 C 0.4460(8) 0.4816(4) 0.3146(4) 0.0436 1.0000 Uani . . . . . . C63 C 0.3485(7) 0.3804(4) 0.2807(4) 0.0331 1.0000 Uani . . . . . . C73 C 0.3405(9) 0.5865(4) 0.2805(5) 0.0559 1.0000 Uani . . . . . . H221 H 0.100(8) 0.2071(17) 0.658(2) 0.12(2) 1.0000 Uiso D . . . . . H222 H 0.173(6) 0.086(3) 0.626(3) 0.12(2) 1.0000 Uiso D . . . . . H223 H -0.044(3) 0.124(5) 0.5735(14) 0.12(2) 1.0000 Uiso D . . . . . H23 H 0.6781 0.2008 0.3827 0.0495 1.0000 Uiso . . . . . . H33 H 0.8517 0.3660 0.4475 0.0594 1.0000 Uiso . . . . . . H43 H 0.7078 0.5423 0.4040 0.0640 1.0000 Uiso . . . . . . H73 H 0.4033 0.6568 0.3024 0.0704 1.0000 Uiso . . . . . . 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 0.03969(13) 0.01817(11) 0.02749(12) 0.0000 0.00791(8) 0.0000 N11 0.052(2) 0.0305(19) 0.055(2) -0.0072(18) 0.0117(19) -0.0084(17) N21 0.048(2) 0.041(2) 0.0315(18) 0.0032(16) 0.0040(15) -0.0062(18) N31 0.071(3) 0.040(2) 0.065(3) -0.024(2) 0.007(2) -0.003(2) O12 0.062(2) 0.0325(15) 0.0369(17) 0.0042(13) 0.0186(15) -0.0053(15) O22 0.083(3) 0.0368(18) 0.051(2) -0.0106(16) 0.0324(19) -0.0130(18) C12 0.039(2) 0.034(2) 0.037(2) 0.0024(17) 0.0085(17) -0.0008(18) C22 0.065(3) 0.057(3) 0.037(3) 0.010(2) 0.018(2) -0.002(3) N13 0.0474(19) 0.0277(16) 0.0251(16) 0.0027(13) 0.0120(14) -0.0013(15) C23 0.049(2) 0.041(2) 0.033(2) 0.0026(19) 0.0120(18) -0.005(2) C33 0.056(3) 0.057(3) 0.036(2) -0.003(2) 0.012(2) -0.019(2) C43 0.072(3) 0.044(3) 0.044(3) -0.014(2) 0.026(2) -0.028(3) C53 0.074(3) 0.029(2) 0.034(2) -0.0043(18) 0.028(2) -0.010(2) C63 0.050(2) 0.0266(18) 0.0254(19) -0.0009(15) 0.0150(17) -0.0022(17) C73 0.104(5) 0.0202(19) 0.052(3) -0.0092(19) 0.037(3) -0.014(2) _refine_ls_extinction_method None _oxford_refine_ls_scale 1.062(3) loop_ _geom_bond_atom_site_label_1 _geom_bond_site_symmetry_1 _geom_bond_atom_site_label_2 _geom_bond_site_symmetry_2 _geom_bond_distance _geom_bond_publ_flag Pt1 . N13 3_555 2.052(4) yes Pt1 . N11 3_555 2.032(4) yes Pt1 . O12 3_555 2.001(3) yes Pt1 . N21 3_555 2.790(4) yes Pt1 . N11 . 2.032(4) yes Pt1 . O12 . 2.001(3) yes Pt1 . N13 . 2.052(4) yes N11 . N21 . 1.175(6) yes N21 . N31 . 1.154(6) yes O12 . C12 . 1.288(6) yes O22 . C12 . 1.215(6) yes C12 . C22 . 1.506(5) yes C22 . H221 . 0.973(7) no C22 . H222 . 0.973(7) no C22 . H223 . 0.973(7) no N13 . C23 . 1.327(6) yes N13 . C63 . 1.364(5) yes C23 . C33 . 1.397(7) yes C23 . H23 . 0.950 no C33 . C43 . 1.368(8) yes C33 . H33 . 0.949 no C43 . C53 . 1.400(8) yes C43 . H43 . 0.950 no C53 . C63 . 1.392(6) yes C53 . C73 . 1.454(7) yes C63 . C63 3_555 1.423(9) yes C73 . C73 3_555 1.324(13) yes C73 . H73 . 0.949 no loop_ _geom_angle_atom_site_label_1 _geom_angle_site_symmetry_1 _geom_angle_atom_site_label_2 _geom_angle_site_symmetry_2 _geom_angle_atom_site_label_3 _geom_angle_site_symmetry_3 _geom_angle _geom_angle_publ_flag N13 3_555 Pt1 . N11 3_555 172.40(16) yes N13 3_555 Pt1 . O12 3_555 95.84(13) yes N11 3_555 Pt1 . O12 3_555 83.17(16) yes N13 3_555 Pt1 . N21 3_555 164.89(13) yes N11 3_555 Pt1 . N21 3_555 21.72(15) yes O12 3_555 Pt1 . N21 3_555 94.64(12) yes N13 3_555 Pt1 . N11 . 91.40(16) yes N11 3_555 Pt1 . N11 . 96.1(2) yes O12 3_555 Pt1 . N11 . 86.90(16) yes N21 3_555 Pt1 . N11 . 78.33(15) yes N13 3_555 Pt1 . N21 . 108.62(13) yes N11 3_555 Pt1 . N21 . 78.33(15) yes O12 3_555 Pt1 . N21 . 72.54(13) yes N21 3_555 Pt1 . N21 . 64.47(16) yes N13 3_555 Pt1 . O12 . 95.44(14) yes N11 3_555 Pt1 . O12 . 86.90(16) yes O12 3_555 Pt1 . O12 . 165.12(19) yes N21 3_555 Pt1 . O12 . 72.54(13) yes N11 . Pt1 . O12 . 83.17(16) yes N13 3_555 Pt1 . N13 . 81.2(2) yes N11 3_555 Pt1 . N13 . 91.40(16) yes O12 3_555 Pt1 . N13 . 95.44(14) yes N21 3_555 Pt1 . N13 . 108.62(13) yes N11 . Pt1 . N13 . 172.40(16) yes N21 . Pt1 . O12 . 94.64(12) yes N21 . Pt1 . N13 . 164.89(13) yes O12 . Pt1 . N13 . 95.84(13) yes Pt1 . N11 . N21 . 118.5(4) yes N11 . N21 . N31 . 173.1(5) yes Pt1 . N21 . N31 . 146.9(4) yes Pt1 . O12 . C12 . 127.4(3) yes O12 . C12 . O22 . 125.2(4) yes O12 . C12 . C22 . 112.1(4) yes O22 . C12 . C22 . 122.7(4) yes C12 . C22 . H221 . 109.44(6) no C12 . C22 . H222 . 109.44(6) no H221 . C22 . H222 . 109.51(6) no C12 . C22 . H223 . 109.44(6) no H221 . C22 . H223 . 109.51(6) no H222 . C22 . H223 . 109.50(6) no Pt1 . N13 . C23 . 128.1(3) yes Pt1 . N13 . C63 . 112.2(3) yes C23 . N13 . C63 . 119.6(4) yes N13 . C23 . C33 . 121.2(5) yes N13 . C23 . H23 . 119.4 no C33 . C23 . H23 . 119.4 no C23 . C33 . C43 . 119.8(5) yes C23 . C33 . H33 . 120.1 no C43 . C33 . H33 . 120.1 no C33 . C43 . C53 . 119.7(4) yes C33 . C43 . H43 . 120.1 no C53 . C43 . H43 . 120.2 no C43 . C53 . C63 . 117.8(5) yes C43 . C53 . C73 . 125.0(5) yes C63 . C53 . C73 . 117.2(5) yes C63 3_555 C63 . C53 . 121.0(3) yes C63 3_555 C63 . N13 . 117.2(2) yes C53 . C63 . N13 . 121.8(4) yes C53 . C73 . C73 3_555 121.8(3) yes C53 . C73 . H73 . 119.0 no C73 3_555 C73 . H73 . 119.2 no #===END data_ps6040 _database_code_depnum_ccdc_archive 'CCDC 709187' _chemical_compound_source 'F. Mackay' _exptl_crystal_recrystallization_method ; Recrystallisation from water at 4 degrees celsius. ; _audit_creation_date 06-08-25 _audit_creation_method CRYSTALS_ver_12.84 _chemical_name_systematic ? _chemical_melting_point ? _cell_length_a 6.9480(3) _cell_length_b 8.2197(4) _cell_length_c 8.6473(4) _cell_angle_alpha 92.136(3) _cell_angle_beta 111.574(3) _cell_angle_gamma 101.038(3) _cell_volume 447.61(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 loop_ _atom_type_symbol _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_Cromer_Mann_a1 _atom_type_scat_Cromer_Mann_b1 _atom_type_scat_Cromer_Mann_a2 _atom_type_scat_Cromer_Mann_b2 _atom_type_scat_Cromer_Mann_a3 _atom_type_scat_Cromer_Mann_b3 _atom_type_scat_Cromer_Mann_a4 _atom_type_scat_Cromer_Mann_b4 _atom_type_scat_Cromer_Mann_c _atom_type_scat_source C 0.0033 0.0016 2.3100 20.8439 1.0200 10.2075 1.5886 0.5687 0.8650 51.6512 0.2156 'International Tables Vol C 4.2.6.8 and 6.1.1.4' H 0.0000 0.0000 0.4930 10.5109 0.3229 26.1257 0.1402 3.1424 0.0408 57.7998 0.0030 'International Tables Vol C 4.2.6.8 and 6.1.1.4' N 0.0061 0.0033 12.2126 0.0057 3.1322 9.8933 2.0125 28.9975 1.1663 0.5826 -11.5290 'International Tables Vol C 4.2.6.8 and 6.1.1.4' O 0.0106 0.0060 3.0485 13.2771 2.2868 5.7011 1.5463 0.3239 0.8670 32.9089 0.2508 'International Tables Vol C 4.2.6.8 and 6.1.1.4' Pt -1.7033 8.3905 27.0059 1.5129 17.7639 8.8117 15.7131 0.4246 5.7837 38.6103 11.6883 'International Tables Vol C 4.2.6.8 and 6.1.1.4' _cell_formula_units_Z 1 # Given Formula = C14 H16 N8 O4 Pt1 # Dc = 2.06 Fooo = 266.00 Mu = 78.77 M = 277.71 # Found Formula = C14 H16 N8 O4 Pt1 # Dc = 2.06 FOOO = 266.00 Mu = 78.77 M = 277.71 _chemical_formula_sum 'C14 H16 N8 O4 Pt1' _chemical_formula_moiety '[Pt(py)2(OAc)2(N3)2]' _chemical_formula_weight 555.42 _cell_measurement_reflns_used 3172 _cell_measurement_theta_min 3 _cell_measurement_theta_max 26 _cell_measurement_temperature 150 _exptl_crystal_description plate _exptl_crystal_colour yellow _exptl_crystal_size_min 0.01 _exptl_crystal_size_mid 0.23 _exptl_crystal_size_max 0.24 _exptl_crystal_density_diffrn 2.060 _exptl_crystal_density_meas ? # Non-dispersive F(000): _exptl_crystal_F_000 266 _exptl_absorpt_coefficient_mu 7.877 # Sheldrick geometric approximatio 0.16 0.92 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_process_details 'SADABS version 2006/1' _exptl_absorpt_correction_T_min 0.39 _exptl_absorpt_correction_T_max 0.92 _exptl_special_details ; Used Oxford Cryosystems low temperature device. ; _diffrn_measurement_device_type 'Bruker SMART Apex CCD' _diffrn_radiation_monochromator graphite _diffrn_radiation_type 'Mo K\a' _diffrn_radiation_wavelength 0.71073 _diffrn_measurement_method '\f & \w scans' _computing_data_collection 'SMART (Siemens, 1993)' _computing_cell_refinement 'SAINT (Siemens ,1995)' _computing_data_reduction 'SAINT (Siemens ,1995)' _computing_structure_solution 'SIR92 (Altomare et al., 1994)' _computing_structure_refinement 'CRYSTALS (Betteridge et al., 2003)' _computing_publication_material 'CRYSTALS (Betteridge et al., 2003)' _computing_molecular_graphics 'CAMERON (Watkin et al., 1996)' _diffrn_standards_interval_time ? _diffrn_standards_interval_count ? _diffrn_standards_number 0 _diffrn_standards_decay_% ? _diffrn_ambient_temperature 150 _diffrn_reflns_number 5315 _reflns_number_total 2121 _diffrn_reflns_av_R_equivalents 0.041 # Number of reflections with Friedels Law is 2121 # Number of reflections without Friedels Law is 0 # Theoretical number of reflections is about 2341 _diffrn_reflns_theta_min 2.542 _diffrn_reflns_theta_max 28.824 _diffrn_measured_fraction_theta_max 0.905 _diffrn_reflns_theta_full 25.077 _diffrn_measured_fraction_theta_full 0.993 _diffrn_reflns_limit_h_min -9 _diffrn_reflns_limit_h_max 9 _diffrn_reflns_limit_k_min -10 _diffrn_reflns_limit_k_max 10 _diffrn_reflns_limit_l_min -11 _diffrn_reflns_limit_l_max 11 _reflns_limit_h_min -9 _reflns_limit_h_max 8 _reflns_limit_k_min -10 _reflns_limit_k_max 10 _reflns_limit_l_min 0 _reflns_limit_l_max 11 _oxford_diffrn_Wilson_B_factor 0.00 _oxford_diffrn_Wilson_scale 0.00 _atom_sites_solution_primary direct #heavy,direct,difmap,geom # _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_diff_density_min -1.86 _refine_diff_density_max 3.20 _refine_ls_number_reflns 2121 _refine_ls_number_restraints 0 _refine_ls_number_parameters 125 #_refine_ls_R_factor_ref 0.0350 _refine_ls_wR_factor_ref 0.0913 _refine_ls_goodness_of_fit_ref 0.9345 #_reflns_number_all 2121 _refine_ls_R_factor_all 0.0350 _refine_ls_wR_factor_all 0.0913 # No actual I/u(I) cutoff was used for refinement. The # threshold below is used for "_gt" information ONLY: _reflns_threshold_expression I>2.0\s(I) _reflns_number_gt 2118 _refine_ls_R_factor_gt 0.0350 _refine_ls_wR_factor_gt 0.0914 _refine_ls_shift/su_max 0.000021 # choose from: rm (reference molecule of known chirality), # ad (anomolous dispersion - Flack), rmad (rm and ad), # syn (from synthesis), unk (unknown) or . (not applicable). _chemical_absolute_configuration . _refine_ls_structure_factor_coef Fsqd _refine_ls_matrix_type full _refine_ls_hydrogen_treatment constr # none, undef, noref, refall, # refxyz, refU, constr or mixed _refine_ls_weighting_scheme calc _refine_ls_weighting_details ; Method, part 1, Chebychev polynomial, (Watkin, 1994, Prince, 1982) [weight] = 1.0/[A~0~*T~0~(x)+A~1~*T~1~(x) ... +A~n-1~]*T~n-1~(x)] where A~i~ are the Chebychev coefficients listed below and x= Fcalc/Fmax Method = Robust Weighting (Prince, 1982) W = [weight] * [1-(deltaF/6*sigmaF)^2^]^2^ A~i~ are: -0.104E+04 0.201E+04 -0.119E+04 572. -150. ; _refine_special_details ; The hydrogen atoms were placed geometrically then refined subject to geometric and X-H distance restraints and finally constrained to ride on their host atom. Analysis using the program ROTAX in CRYSTALS showed that the crystal was twinned by the following twin law: [ -1.000 0.000 0.000] [ 0.000 -1.000 0.000] [ 0.969 0.235 1.000] The twin element scales were refined and they refined to 0.806 and 0.194(5). There are two azides and two acetate ligands per complex which each have a charge of 1-, giving an overall negative charge of 4-. The central Pt atom must therefore be Pt4+. Numbering Scheme #=============== Pt: Pt1 Pyridine: N1*-C6* [*=1] Acetate: C1*-C4* [*=2] Azide: N1*-N3* [*=3] Checkcif output: 060_ALERT_3_A Ratio Tmax/Tmin (Exp-to-Rep) (too) Large ....... 2.26 Sadabs corrects for all systematic errors that lead to disparities in the intensities of equivalent data. It is possible that the larger than expected range of transmission is accounted for by crystal decay or absorption by the mounting fibre. 342_ALERT_3_C Low Bond Precision on C-C bonds (x 1000) Ang ... 11 Noted but no action taken. 042_ALERT_1_C Calc. and Rep. MoietyFormula Strings Differ .... ? 795_ALERT_4_C C-Atom in CIF Coordinate List out of Sequence .. C12 The moiety formula and atom list given are intended to be more chemically significant. #=============================================================================== Resolution & Completeness Statistics (Cumulative) #=============================================================================== Theta sin(th)/Lambda Complete Expected Measured Missing #------------------------------------------------------------------------------- 20.82 0.500 0.995 933 928 5 23.01 0.550 0.995 1246 1240 6 25.24 0.600 0.993 1621 1610 11 #----------------------------------------------------------- ACTA Min. Res. ---- 27.51 0.650 0.983 2058 2023 35 28.82 0.678 0.905 2344 2121 223 ; # End of 'script/refcif.dat' # Insert your own references if required - in alphabetical order _publ_section_references ; Altomare, A., Cascarano, G., Giacovazzo, G., Guagliardi, A., Burla, M.C., Polidori, G. & Camalli, M. (1994). J. Appl. Cryst. 27, 435. Betteridge, P.W., Carruthers, J.R., Cooper, R.I., Prout, K. & Watkin, D.J. (2003). J. Appl. Cryst. 36, 1487. Larson, A.C. (1970) Crystallographic Computing, Ed Ahmed, F.R., Munksgaard, Copenhagen, 291-294. Prince, E. Mathematical Techniques in Crystallography and Materials Science Springer-Verlag, New York, 1982. Siemens Industrial Automation, Inc (1993). SMART: Area-Detector Software Package; Madison, WI. Siemens Industrial Automation, Inc (1995). SAINT: Area-Detector Integration Software.; Madison, WI. Siemens Industrial Automation, Inc (1996). SADABS: Area-Detector Absorption Correction;: Madison, WI. Watkin D.J. (1994). Acta Cryst, A50, 411-437. Watkin, D.J., Prout, C.K. & Pearce, L.J. (1996). CAMERON, Chemical Crystallography Laboratory, Oxford, UK. ; # Uequiv = arithmetic mean of Ui i.e. Ueqiv = (U1+U2+U3)/3 # Replace last . with number of unfound hydrogen atomsattached to an atom. # ..._refinement_flags_... # . no refinement constraints S special position constraint on site # G rigid group refinement of site R riding atom # D distance or angle restraint on site T thermal displacement constraints # U Uiso or Uij restraint (rigid bond) P partial occupancy constraint 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_occupancy _atom_site_adp_type _atom_site_refinement_flags_posn _atom_site_refinement_flags_adp _atom_site_refinement_flags_occupancy _atom_site_disorder_assembly _atom_site_disorder_group _atom_site_attached_hydrogens Pt1 Pt 0.0000 0.0000 0.0000 0.0185 1.0000 Uani S . . . . . N11 N -0.1109(8) -0.1955(7) 0.1033(7) 0.0244 1.0000 Uani . . . . . . C21 C 0.0225(11) -0.2907(9) 0.1880(9) 0.0292 1.0000 Uani . . . . . . C31 C -0.0464(12) -0.4231(9) 0.2620(10) 0.0333 1.0000 Uani . . . . . . C41 C -0.2530(13) -0.4590(9) 0.2515(10) 0.0351 1.0000 Uani . . . . . . C51 C -0.3892(11) -0.3611(9) 0.1647(9) 0.0321 1.0000 Uani . . . . . . C61 C -0.3146(11) -0.2320(8) 0.0903(9) 0.0273 1.0000 Uani . . . . . . C12 C 0.3154(10) 0.2137(9) 0.3015(9) 0.0281 1.0000 Uani . . . . . . O22 O 0.2372(8) 0.0586(6) 0.2262(6) 0.0296 1.0000 Uani . . . . . . O32 O 0.2762(9) 0.3405(7) 0.2432(7) 0.0375 1.0000 Uani . . . . . . C42 C 0.4661(13) 0.2162(11) 0.4804(10) 0.0392 1.0000 Uani . . . . . . N13 N 0.1864(9) -0.1338(7) -0.0627(7) 0.0281 1.0000 Uani . . . . . . N23 N 0.1563(10) -0.1480(8) -0.2117(9) 0.0332 1.0000 Uani . . . . . . N33 N 0.1371(14) -0.1665(10) -0.3485(10) 0.0477 1.0000 Uani . . . . . . H21 H 0.1624 -0.2661 0.1963 0.0338 1.0000 Uiso R . . . . . H31 H 0.0467 -0.4884 0.3189 0.0410 1.0000 Uiso R . . . . . H41 H -0.3007 -0.5476 0.3015 0.0419 1.0000 Uiso R . . . . . H51 H -0.5281 -0.3823 0.1569 0.0380 1.0000 Uiso R . . . . . H61 H -0.4075 -0.1690 0.0282 0.0328 1.0000 Uiso R . . . . . H421 H 0.5145 0.3293 0.5343 0.0560 1.0000 Uiso R . . . . . H422 H 0.5856 0.1718 0.4819 0.0561 1.0000 Uiso R . . . . . H423 H 0.3917 0.1488 0.5383 0.0560 1.0000 Uiso 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 0.01404(16) 0.01796(16) 0.02257(17) 0.00169(11) 0.00616(12) 0.00334(11) N11 0.019(2) 0.024(2) 0.027(3) 0.000(2) 0.005(2) 0.0050(19) C21 0.023(3) 0.028(3) 0.034(3) 0.003(3) 0.007(3) 0.007(2) C31 0.034(4) 0.032(3) 0.036(4) 0.009(3) 0.013(3) 0.011(3) C41 0.040(4) 0.028(3) 0.038(4) 0.006(3) 0.018(3) 0.003(3) C51 0.025(3) 0.033(3) 0.037(4) -0.003(3) 0.014(3) 0.000(3) C61 0.025(3) 0.027(3) 0.030(3) 0.001(2) 0.010(2) 0.006(2) C12 0.018(3) 0.031(3) 0.033(3) -0.002(3) 0.010(2) 0.002(2) O22 0.027(2) 0.028(2) 0.027(2) -0.0015(18) 0.0048(18) 0.0038(19) O32 0.036(3) 0.029(3) 0.044(3) 0.003(2) 0.013(2) 0.004(2) C42 0.037(4) 0.042(4) 0.032(4) -0.002(3) 0.008(3) 0.006(3) N13 0.024(3) 0.030(3) 0.031(3) 0.008(2) 0.010(2) 0.007(2) N23 0.031(3) 0.027(3) 0.047(4) 0.002(2) 0.020(3) 0.009(2) N33 0.062(5) 0.049(4) 0.041(4) 0.001(3) 0.029(4) 0.015(4) _refine_ls_extinction_method None _oxford_refine_ls_scale 0.930(6) loop_ _oxford_twin_element_scale_factors 0.806(5) 0.194(5) loop_ _geom_bond_atom_site_label_1 _geom_bond_site_symmetry_1 _geom_bond_atom_site_label_2 _geom_bond_site_symmetry_2 _geom_bond_distance _geom_bond_publ_flag Pt1 . N13 2_555 2.049(6) yes Pt1 . N11 2_555 2.028(6) yes Pt1 . O22 2_555 2.007(5) yes Pt1 . N11 . 2.028(6) yes Pt1 . O22 . 2.007(5) yes Pt1 . N13 . 2.049(6) yes N11 . C21 . 1.353(8) yes N11 . C61 . 1.351(8) yes C21 . C31 . 1.379(10) yes C21 . H21 . 0.929 no C31 . C41 . 1.376(11) yes C31 . H31 . 0.931 no C41 . C51 . 1.386(11) yes C41 . H41 . 0.929 no C51 . C61 . 1.377(10) yes C51 . H51 . 0.924 no C61 . H61 . 0.931 no C12 . O22 . 1.325(8) yes C12 . O32 . 1.209(9) yes C12 . C42 . 1.512(10) yes C42 . H421 . 0.964 no C42 . H422 . 0.965 no C42 . H423 . 0.963 no N13 . N23 . 1.224(9) yes N23 . N33 . 1.142(10) yes loop_ _geom_angle_atom_site_label_1 _geom_angle_site_symmetry_1 _geom_angle_atom_site_label_2 _geom_angle_site_symmetry_2 _geom_angle_atom_site_label_3 _geom_angle_site_symmetry_3 _geom_angle _geom_angle_publ_flag N13 2_555 Pt1 . N11 2_555 90.7(2) yes N13 2_555 Pt1 . O22 2_555 86.4(2) yes N11 2_555 Pt1 . O22 2_555 84.4(2) yes N13 2_555 Pt1 . N11 . 89.3(2) yes N11 2_555 Pt1 . N11 . 179.994 yes O22 2_555 Pt1 . N11 . 95.6(2) yes N13 2_555 Pt1 . O22 . 93.6(2) yes N11 2_555 Pt1 . O22 . 95.6(2) yes O22 2_555 Pt1 . O22 . 179.994 yes N11 . Pt1 . O22 . 84.4(2) yes N13 2_555 Pt1 . N13 . 179.994 yes N11 2_555 Pt1 . N13 . 89.3(2) yes O22 2_555 Pt1 . N13 . 93.6(2) yes N11 . Pt1 . N13 . 90.7(2) yes O22 . Pt1 . N13 . 86.4(2) yes Pt1 . N11 . C21 . 119.3(5) yes Pt1 . N11 . C61 . 121.4(5) yes C21 . N11 . C61 . 119.3(6) yes N11 . C21 . C31 . 120.9(6) yes N11 . C21 . H21 . 119.3 no C31 . C21 . H21 . 119.8 no C21 . C31 . C41 . 120.0(7) yes C21 . C31 . H31 . 120.0 no C41 . C31 . H31 . 120.0 no C31 . C41 . C51 . 119.0(7) yes C31 . C41 . H41 . 120.6 no C51 . C41 . H41 . 120.4 no C41 . C51 . C61 . 119.1(7) yes C41 . C51 . H51 . 120.4 no C61 . C51 . H51 . 120.5 no C51 . C61 . N11 . 121.7(6) yes C51 . C61 . H61 . 119.1 no N11 . C61 . H61 . 119.1 no O22 . C12 . O32 . 127.5(7) yes O22 . C12 . C42 . 110.8(6) yes O32 . C12 . C42 . 121.7(7) yes C12 . O22 . Pt1 . 122.8(4) yes C12 . C42 . H421 . 109.3 no C12 . C42 . H422 . 109.9 no H421 . C42 . H422 . 109.9 no C12 . C42 . H423 . 108.8 no H421 . C42 . H423 . 109.4 no H422 . C42 . H423 . 109.6 no Pt1 . N13 . N23 . 114.9(5) yes N13 . N23 . N33 . 176.0(8) yes