Supplementary Material (ESI) for Dalton Transactions This journal is (c) The Royal Society of Chemistry 2006 data_global _journal_name_full 'Dalton Trans.' _journal_coden_cambridge 0222 _publ_contact_author_name 'Thomas Kaden' _publ_contact_author_address ; Department of Chemistry University of Basel Spitalstr. 51 Basel 4056 SWITZERLAND ; _publ_section_title ; Cu2+ and Pt2+ complexes of pyrazole and triazole based dinucleating ligands ; loop_ _publ_author_name Th.Kaden A.Eisenwiener M.Neuburger _publ_contact_author_email TH.KADEN@UNIBAS.CH # Attachment 'publish.cif' data_ae16_173k _database_code_depnum_ccdc_archive 'CCDC 623209' _audit_creation_date 06-08-23 _audit_creation_method CRYSTALS_ver_12.84 _oxford_structure_analysis_title '8221622 ae16_173k' _chemical_name_systematic ? _chemical_melting_point ? _cell_length_a 7.9171(10) _cell_length_b 14.8595(12) _cell_length_c 17.201(2) _cell_angle_alpha 102.126(9) _cell_angle_beta 91.064(12) _cell_angle_gamma 95.307(7) _cell_volume 1968.4(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' 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' I -0.4742 1.8119 20.1472 4.3470 18.9949 0.3814 7.5138 27.7660 2.2735 66.8776 4.0712 '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' _cell_formula_units_Z 4 # Given Formula = C11 H21 I3 N4 O2 Pt2 # Dc = 3.42 Fooo = 1784.00 Mu = 189.13 M = 2024.41 # Found Formula = C11 H21 I3 N4 O2 Pt2 # Dc = 3.42 FOOO = 1784.00 Mu = 189.13 M = 2024.41 _chemical_formula_sum 'C11 H21 I3 N4 O2 Pt2' _chemical_formula_moiety 'C11 H21 I3 N4 O2 Pt2' _chemical_compound_source ? _chemical_formula_weight 1012.21 _cell_measurement_reflns_used 0 _cell_measurement_theta_min 0 _cell_measurement_theta_max 0 _cell_measurement_temperature 173 _exptl_crystal_description plate _exptl_crystal_colour orange _exptl_crystal_size_min 0.04 _exptl_crystal_size_mid 0.04 _exptl_crystal_size_max 0.22 _exptl_crystal_density_diffrn 3.415 _exptl_crystal_density_meas ? # Non-dispersive F(000): _exptl_crystal_F_000 1784.000 _exptl_absorpt_coefficient_mu 18.913 # Sheldrick geometric approximatio 0.47 0.47 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_process_details 'DENZO/SCALEPACK (Otwinowski & Minor, 1997)' _exptl_absorpt_correction_T_min 0.43 _exptl_absorpt_correction_T_max 0.47 # For a Kappa CCD, set Tmin to 1.0 and # Tmax to the ratio of max:min frame scales in scale_all.log _diffrn_measurement_device_type 'Nonius KappaCCD' _diffrn_radiation_monochromator graphite _diffrn_radiation_type 'Mo K\a' _diffrn_radiation_wavelength 0.71073 _diffrn_measurement_method '\f & \w scans' # If a reference occurs more than once, delete the author # and date from subsequent references. _computing_data_collection 'COLLECT (Nonius, 1997-2001).' _computing_cell_refinement 'DENZO/SCALEPACK (Otwinowski & Minor, 1997)' _computing_data_reduction 'DENZO/SCALEPACK (Otwinowski & Minor, 1997)' _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 173 _diffrn_reflns_number 72280 _reflns_number_total 9033 _diffrn_reflns_av_R_equivalents 0.133 # Number of reflections with Friedels Law is 9033 # Number of reflections without Friedels Law is 0 # Theoretical number of reflections is about 9044 _diffrn_reflns_theta_min 3.052 _diffrn_reflns_theta_max 27.500 _diffrn_measured_fraction_theta_max 0.998 _diffrn_reflns_theta_full 27.500 _diffrn_measured_fraction_theta_full 0.998 _diffrn_reflns_limit_h_min -10 _diffrn_reflns_limit_h_max 10 _diffrn_reflns_limit_k_min -19 _diffrn_reflns_limit_k_max 18 _diffrn_reflns_limit_l_min -22 _diffrn_reflns_limit_l_max 22 _reflns_limit_h_min -10 _reflns_limit_h_max 10 _reflns_limit_k_min -19 _reflns_limit_k_max 18 _reflns_limit_l_min 0 _reflns_limit_l_max 22 _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 -2.85 _refine_diff_density_max 4.18 _refine_ls_number_reflns 4375 _refine_ls_number_restraints 616 _refine_ls_number_parameters 453 #_refine_ls_R_factor_ref 0.0536 _refine_ls_wR_factor_ref 0.0609 _refine_ls_goodness_of_fit_ref 1.0272 #_reflns_number_all 9014 _refine_ls_R_factor_all 0.1011 _refine_ls_wR_factor_all 0.0991 # The I/u(I) cutoff below was used for refinement as # well as the _gt R-factors: _reflns_threshold_expression I>3.0\s(I) _reflns_number_gt 4375 _refine_ls_R_factor_gt 0.0536 _refine_ls_wR_factor_gt 0.0609 _refine_ls_shift/su_max 0.007952 # 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 F _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 ; 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: 3.79 0.702 2.71 ; _publ_section_abstract # Text of the abstract # (a) The Abstract must be self-contained and comprehensible # without the rest of the paper. This means no references # to atom names or to compound numbers; compounds must be # identified as the title compound, or by name or by some other # means such as derivatives of each other (e.g. "the # corresponding ketone"). # (b) The chemical formula of "the title compound" must be given. # (c) Any crystallographic molecular symmetry should be # mentioned, and also the presence of more than one molecule # in the asymmetric unit (i.e. anything other than Z'=1). ; ? ; _publ_section_comment # Text of the paper # Note that atoms are referenced as N2, not N(2) or N~2~ # If text containing () occur within (), the outer ones should be [] # Figures should be referenced as Fih. ; ? ; _publ_section_acknowledgements # Acknowledgments ; ? ; _publ_section_figure_captions # Captions to figures - Start each caption on a new line after a blank line ; Fig. 1. The title compound with displacement ellipsoids drawn at the 50% probability level. H atoms are shown as spheres of arbitary radius. ; _publ_section_exptl_refinement # Some potentially useful phrases are donated by Bill Clegg: ; In the absence of significant anomalous scattering, Friedel pairs were merged. The absolute configuration was arbitrarily assigned. The relatively large ratio of minimum to maximum corrections applied in the multiscan process (1:nnn) reflect changes in the illuminated volume of the crystal. Changes in illuminated volume were kept to a minimum, and were taken into account (G\"orbitz, 1999) by the multi-scan inter-frame scaling (DENZO/SCALEPACK, Otwinowski & Minor, 1997). G\"orbitz, C. H. (1999). Acta Cryst. B55, 1090-1098. The H atoms were all located in a difference map, but those attached to carbon atoms were repositioned geometrically. The H atoms were initially refined with soft restraints on the bond lengths and angles to regularise their geometry (C---H in the range 0.93--0.98, N---H in the range 0.86--0.89 N---H to 0.86 O---H = 0.82 \%A) and U~iso~(H) (in the range 1.2-1.5 times U~eq~ of the parent atom), after which the positions were refined with riding constraints. ; _publ_section_exptl_prep # Brief details or a reference. Include solvent if known ; ? ; # 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. Nonius (1997-2001). COLLECT. Nonius BV, Delft, The Netherlands. Otwinowski, Z. & Minor, W. (1997). Methods in Enzymology, Vol. 276, edited by C. W. Carter Jr & R. M. Sweet, pp. 307--326. New York: Academic Press. Prince, E. Mathematical Techniques in Crystallography and Materials Science Springer-Verlag, New York, 1982. 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 0.67223(8) 0.37248(5) 0.18682(4) 0.0320 1.0000 Uani . . . . . . Pt2 Pt 0.62138(8) 0.63241(5) 0.26167(4) 0.0317 1.0000 Uani . . . . . . Pt3 Pt 0.17920(10) 0.37213(6) 0.23617(5) 0.0432 1.0000 Uani . . . . . . Pt4 Pt 0.11944(9) 0.62965(5) 0.31423(4) 0.0376 1.0000 Uani . . . . . . I1 I 0.68833(18) 0.27025(9) 0.04489(8) 0.0470 1.0000 Uani . . . . . . I2 I 0.63614(15) 0.51637(8) 0.12923(7) 0.0364 1.0000 Uani . . . . . . I3 I 0.59365(17) 0.76439(9) 0.18559(8) 0.0472 1.0000 Uani . . . . . . I4 I 0.2242(3) 0.24034(12) 0.31051(11) 0.0737 1.0000 Uani . . . . . . I5 I 0.13325(17) 0.48244(10) 0.36829(8) 0.0458 1.0000 Uani . . . . . . I6 I 0.09599(18) 0.72631(11) 0.45774(8) 0.0549 1.0000 Uani . . . . . . N1 N 0.689(2) 0.2713(10) 0.2538(11) 0.0521 1.0000 Uani D U . . . . N2 N 0.6616(18) 0.4451(10) 0.2955(8) 0.0323 1.0000 Uani . . . . . . N3 N 0.6348(18) 0.5354(10) 0.3215(9) 0.0338 1.0000 Uani . . . . . . N4 N 0.628(3) 0.7091(11) 0.3806(10) 0.0566 1.0000 Uani . . . . . . N5 N 0.213(3) 0.3021(15) 0.1194(13) 0.0753 1.0000 Uani . . . . . . N6 N 0.1581(18) 0.4696(11) 0.1763(9) 0.0387 1.0000 Uani . . . . . . N7 N 0.1330(19) 0.5617(11) 0.2051(8) 0.0383 1.0000 Uani . . . . . . N8 N 0.126(2) 0.7341(12) 0.2494(12) 0.0598 1.0000 Uani D U . . . . C1 C 0.702(3) 0.3099(14) 0.3418(13) 0.0534 1.0000 Uani . . . . . . C2 C 0.670(2) 0.4077(12) 0.3571(12) 0.0382 1.0000 Uani . . . . . . C3 C 0.652(2) 0.4720(10) 0.4256(10) 0.0287 1.0000 Uani . . . . . . C4 C 0.633(2) 0.5545(11) 0.3992(10) 0.0293 1.0000 Uani . . . . . . C5 C 0.601(2) 0.6487(12) 0.4349(12) 0.0392 1.0000 Uani . . . . . . C6 C 0.193(2) 0.3584(13) 0.0604(11) 0.0406 1.0000 Uani . . . . . . C7 C 0.168(2) 0.4543(14) 0.0993(11) 0.0403 1.0000 Uani . . . . . . C8 C 0.149(2) 0.5372(13) 0.0753(11) 0.0368 1.0000 Uani . . . . . . C9 C 0.127(2) 0.6012(13) 0.1455(10) 0.0363 1.0000 Uani . . . . . . C10 C 0.097(2) 0.6996(12) 0.1636(13) 0.0437 1.0000 Uani . . . . . . C41 C 0.564(3) 0.7981(14) 0.3974(15) 0.0660 1.0000 Uani . . . . . . C42 C 0.598(4) 0.8539(15) 0.4818(17) 0.0780 1.0000 Uani . . . . . . O41 O 0.752(4) 0.900(2) 0.4766(17) 0.1733 1.0000 Uani . . . . . . C43 C 0.808(7) 0.953(3) 0.553(3) 0.1679 1.0000 Uani . . . . . . C51 C 0.170(5) 0.2064(14) 0.0966(16) 0.0934 1.0000 Uani . . . . . . C52 C 0.200(3) 0.1561(16) 0.0169(14) 0.0674 1.0000 Uani . . . . . . O51 O 0.224(5) 0.0730(16) 0.0160(15) 0.1583 1.0000 Uani . . . . . . C53 C 0.255(7) 0.019(3) -0.057(3) 0.1837 1.0000 Uani . . . . . . C81 C 0.060(3) 0.8210(13) 0.2793(14) 0.0634 1.0000 Uani D U . . . . C82 C 0.069(3) 0.8948(15) 0.2377(14) 0.0600 1.0000 Uani D U . . . . C11 C 0.652(7) 0.1746(16) 0.220(3) 0.0518 0.378(6) Uani D U P . . . C12 C 0.721(7) 0.105(3) 0.254(2) 0.0517 0.378(6) Uani D U P . . . O11 O 0.658(5) 0.109(2) 0.331(2) 0.0501 0.378(6) Uani D U P . . . C13 C 0.741(7) 0.050(3) 0.372(3) 0.0510 0.378(6) Uani D U P . . . C110 C 0.778(4) 0.1919(17) 0.2260(19) 0.0541 0.622(6) Uani D U P . . . C120 C 0.786(3) 0.125(2) 0.275(2) 0.0545 0.622(6) Uani D U P . . . O110 O 0.616(3) 0.0899(15) 0.2842(16) 0.0551 0.622(6) Uani D U P . . . C130 C 0.617(5) 0.030(2) 0.339(2) 0.0579 0.622(6) Uani D U P . . . O81 O 0.092(6) 0.904(4) 0.1581(19) 0.0603 0.264(9) Uani D U P . . . C83 C 0.254(8) 0.948(6) 0.146(6) 0.0598 0.264(9) Uani D U P . . . O810 O 0.241(3) 0.9124(14) 0.2292(17) 0.0818 0.736(9) Uani D U P . . . C830 C 0.279(5) 0.969(2) 0.173(2) 0.0835 0.736(9) Uani D U P . . . H11 H 0.8137 0.3045 0.3621 0.0675 1.0000 Uiso . . . . . . H12 H 0.6193 0.2762 0.3677 0.0675 1.0000 Uiso . . . . . . H31 H 0.6521 0.4630 0.4792 0.0338 1.0000 Uiso . . . . . . H51 H 0.6754 0.6711 0.4809 0.0424 1.0000 Uiso . . . . . . H52 H 0.4850 0.6487 0.4507 0.0424 1.0000 Uiso . . . . . . H61 H 0.2935 0.3588 0.0298 0.0500 1.0000 Uiso . . . . . . H62 H 0.0968 0.3323 0.0258 0.0500 1.0000 Uiso . . . . . . H81 H 0.1500 0.5477 0.0221 0.0461 1.0000 Uiso . . . . . . H101 H 0.1735 0.7337 0.1352 0.0493 1.0000 Uiso . . . . . . H102 H -0.0181 0.7062 0.1485 0.0493 1.0000 Uiso . . . . . . H1 H 0.5744 0.2432 0.2480 0.0627 1.0000 Uiso . . . . . . H111 H 0.6891 0.1654 0.1662 0.0624 0.3781 Uiso . . . . . . H112 H 0.5309 0.1621 0.2194 0.0624 0.3781 Uiso . . . . . . H121 H 0.8425 0.1160 0.2576 0.0623 0.3781 Uiso . . . . . . H122 H 0.6876 0.0452 0.2212 0.0623 0.3781 Uiso . . . . . . H131 H 0.6957 0.0543 0.4242 0.0629 0.3781 Uiso . . . . . . H132 H 0.8603 0.0691 0.3773 0.0629 0.3781 Uiso . . . . . . H133 H 0.7216 -0.0125 0.3426 0.0629 0.3781 Uiso . . . . . . H1101 H 0.8931 0.2140 0.2180 0.0655 0.6219 Uiso . . . . . . H1102 H 0.7252 0.1601 0.1758 0.0655 0.6219 Uiso . . . . . . H1201 H 0.8380 0.1539 0.3260 0.0664 0.6219 Uiso . . . . . . H1202 H 0.8493 0.0758 0.2499 0.0664 0.6219 Uiso . . . . . . H1301 H 0.5022 0.0057 0.3460 0.0712 0.6219 Uiso . . . . . . H1302 H 0.6650 0.0639 0.3897 0.0712 0.6219 Uiso . . . . . . H1303 H 0.6828 -0.0203 0.3191 0.0712 0.6219 Uiso . . . . . . H2 H 0.7479 0.7268 0.3894 0.0706 1.0000 Uiso . . . . . . H411 H 0.6152 0.8337 0.3618 0.0800 1.0000 Uiso . . . . . . H412 H 0.4436 0.7889 0.3872 0.0800 1.0000 Uiso . . . . . . H421 H 0.5136 0.8959 0.4968 0.0891 1.0000 Uiso . . . . . . H422 H 0.6024 0.8143 0.5192 0.0891 1.0000 Uiso . . . . . . H431 H 0.9166 0.9856 0.5498 0.1940 1.0000 Uiso . . . . . . H432 H 0.7274 0.9964 0.5722 0.1940 1.0000 Uiso . . . . . . H433 H 0.8163 0.9124 0.5897 0.1940 1.0000 Uiso . . . . . . H3 H 0.3347 0.3030 0.1211 0.0948 1.0000 Uiso . . . . . . H511 H 0.2312 0.1788 0.1326 0.1127 1.0000 Uiso . . . . . . H512 H 0.0502 0.1962 0.1041 0.1127 1.0000 Uiso . . . . . . H521 H 0.2979 0.1859 -0.0026 0.0811 1.0000 Uiso . . . . . . H522 H 0.1025 0.1570 -0.0172 0.0811 1.0000 Uiso . . . . . . H531 H 0.2719 -0.0419 -0.0508 0.2371 1.0000 Uiso . . . . . . H532 H 0.3554 0.0460 -0.0774 0.2371 1.0000 Uiso . . . . . . H533 H 0.1603 0.0169 -0.0930 0.2371 1.0000 Uiso . . . . . . H4 H 0.2456 0.7532 0.2520 0.0722 1.0000 Uiso . . . . . . H811 H 0.1182 0.8458 0.3298 0.0770 1.0000 Uiso . . . . . . H812 H -0.0580 0.8065 0.2871 0.0770 1.0000 Uiso . . . . . . H821 H 0.1592 0.9369 0.2663 0.0734 1.0000 Uiso . . . . . . H822 H -0.0376 0.9200 0.2491 0.0734 1.0000 Uiso . . . . . . H831 H 0.2614 0.9517 0.0912 0.0734 0.2636 Uiso . . . . . . H832 H 0.2675 1.0091 0.1789 0.0734 0.2636 Uiso . . . . . . H833 H 0.3413 0.9129 0.1599 0.0734 0.2636 Uiso . . . . . . H8301 H 0.3994 0.9789 0.1695 0.1055 0.7364 Uiso . . . . . . H8302 H 0.2332 1.0271 0.1904 0.1055 0.7364 Uiso . . . . . . H8303 H 0.2287 0.9384 0.1221 0.1055 0.7364 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 0.0338(4) 0.0277(3) 0.0345(4) 0.0050(3) 0.0011(3) 0.0064(3) Pt2 0.0310(3) 0.0279(4) 0.0373(4) 0.0073(3) 0.0026(3) 0.0078(3) Pt3 0.0489(5) 0.0426(4) 0.0394(4) 0.0121(3) -0.0006(3) 0.0053(3) Pt4 0.0316(4) 0.0436(4) 0.0354(4) 0.0041(3) 0.0013(3) 0.0024(3) I1 0.0626(8) 0.0359(7) 0.0395(7) 0.0002(5) 0.0037(6) 0.0073(6) I2 0.0447(7) 0.0310(6) 0.0348(6) 0.0083(5) 0.0054(5) 0.0075(5) I3 0.0576(8) 0.0357(7) 0.0540(8) 0.0176(6) 0.0033(6) 0.0150(6) I4 0.1096(14) 0.0624(10) 0.0596(10) 0.0287(8) 0.0031(9) 0.0267(9) I5 0.0490(7) 0.0521(8) 0.0362(7) 0.0102(6) -0.0008(5) 0.0031(6) I6 0.0568(8) 0.0648(9) 0.0392(7) -0.0021(7) 0.0015(6) 0.0162(7) N1 0.073(6) 0.032(6) 0.052(7) 0.007(5) 0.010(6) 0.011(5) N2 0.035(6) 0.032(7) 0.032(7) 0.013(6) -0.002(6) -0.002(6) N3 0.041(7) 0.034(7) 0.030(7) 0.009(6) 0.006(6) 0.011(6) N4 0.106(10) 0.027(7) 0.044(9) 0.018(7) -0.005(8) 0.019(8) N5 0.113(10) 0.064(10) 0.059(10) 0.027(9) 0.001(10) 0.034(10) N6 0.037(7) 0.051(9) 0.026(7) 0.000(6) 0.005(6) 0.008(6) N7 0.049(7) 0.048(8) 0.016(6) 0.004(6) -0.001(6) 0.005(7) N8 0.075(7) 0.048(7) 0.057(8) 0.013(7) 0.009(7) 0.008(6) C1 0.083(10) 0.035(9) 0.051(10) 0.019(8) -0.008(9) 0.029(8) C2 0.033(7) 0.030(8) 0.049(10) 0.004(7) 0.008(7) -0.003(7) C3 0.038(7) 0.015(6) 0.032(8) -0.001(6) -0.007(7) 0.010(6) C4 0.036(7) 0.020(7) 0.029(8) -0.002(6) 0.004(6) 0.004(6) C5 0.032(7) 0.027(8) 0.047(9) -0.016(7) 0.009(7) -0.005(6) C6 0.060(9) 0.035(8) 0.031(8) 0.014(7) -0.004(8) 0.006(8) C7 0.029(7) 0.048(9) 0.039(9) -0.003(8) 0.008(7) 0.004(7) C8 0.022(7) 0.047(9) 0.046(9) 0.022(8) 0.005(7) 0.001(7) C9 0.032(7) 0.041(9) 0.026(8) -0.014(7) 0.001(6) 0.000(7) C10 0.043(8) 0.024(8) 0.056(10) -0.011(7) -0.015(8) 0.011(7) C41 0.103(11) 0.027(9) 0.070(12) 0.011(9) 0.031(11) 0.010(9) C42 0.120(11) 0.023(9) 0.080(13) -0.015(9) 0.033(12) 0.001(10) O41 0.249(12) 0.150(14) 0.108(13) 0.059(12) -0.068(13) -0.109(13) C43 0.281(13) 0.079(14) 0.124(16) 0.024(14) -0.078(16) -0.071(15) C51 0.208(12) 0.013(8) 0.061(12) 0.009(8) 0.003(13) 0.016(11) C52 0.108(11) 0.051(11) 0.044(10) 0.000(9) 0.006(10) 0.034(10) O51 0.334(12) 0.079(11) 0.090(12) 0.038(10) 0.079(13) 0.104(12) C53 0.331(13) 0.094(13) 0.167(16) 0.055(13) 0.143(15) 0.146(13) C81 0.070(7) 0.054(6) 0.068(7) 0.014(6) 0.009(7) 0.015(6) C82 0.059(6) 0.053(7) 0.072(7) 0.015(6) 0.014(7) 0.016(6) C11 0.073(7) 0.030(6) 0.053(8) 0.006(7) 0.012(8) 0.015(7) C12 0.072(7) 0.027(7) 0.057(8) 0.004(7) 0.014(8) 0.018(8) O11 0.072(7) 0.024(8) 0.059(8) 0.009(8) 0.014(8) 0.021(8) C13 0.071(9) 0.025(9) 0.061(10) 0.010(9) 0.015(10) 0.023(9) C110 0.069(7) 0.039(6) 0.056(7) 0.008(6) 0.010(7) 0.016(6) C120 0.067(7) 0.039(7) 0.060(8) 0.011(6) 0.010(7) 0.017(7) O110 0.066(6) 0.038(7) 0.066(8) 0.015(7) 0.006(7) 0.016(6) C130 0.069(8) 0.042(9) 0.067(9) 0.018(7) 0.006(9) 0.014(8) O81 0.060(7) 0.053(9) 0.071(8) 0.014(8) 0.012(9) 0.020(8) C83 0.061(8) 0.052(11) 0.071(10) 0.015(10) 0.013(10) 0.020(10) O810 0.067(8) 0.035(8) 0.156(12) 0.043(8) 0.016(10) 0.018(7) C830 0.068(9) 0.039(9) 0.157(12) 0.044(9) 0.020(10) 0.017(8) _refine_ls_extinction_method None _oxford_refine_ls_scale 0.2661(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 . I1 . 2.6026(15) yes Pt1 . I2 . 2.5743(13) yes Pt1 . N1 . 2.090(17) yes Pt1 . N2 . 1.960(15) yes Pt2 . I2 . 2.5639(14) yes Pt2 . I3 . 2.5989(14) yes Pt2 . N3 . 1.948(14) yes Pt2 . N4 . 2.119(18) yes Pt3 . I4 . 2.6002(18) yes Pt3 . I5 . 2.5611(16) yes Pt3 . N5 . 2.09(2) yes Pt3 . N6 . 1.963(16) yes Pt4 . I5 . 2.5605(16) yes Pt4 . I6 . 2.6015(16) yes Pt4 . N7 . 1.946(14) yes Pt4 . N8 . 2.091(18) yes N1 . C1 . 1.50(3) yes N1 . C11 . 1.433(18) yes N1 . C110 . 1.430(16) yes N1 . H1 . 0.960 no N2 . N3 . 1.360(19) yes N2 . C2 . 1.30(2) yes N3 . C4 . 1.31(2) yes N4 . C5 . 1.43(3) yes N4 . C41 . 1.43(3) yes N4 . H2 . 0.960 no N5 . C6 . 1.46(2) yes N5 . C51 . 1.40(3) yes N5 . H3 . 0.960 no N6 . N7 . 1.39(2) yes N6 . C7 . 1.30(2) yes N7 . C9 . 1.29(2) yes N8 . C10 . 1.46(3) yes N8 . C81 . 1.433(16) yes N8 . H4 . 0.960 no C1 . C2 . 1.47(2) yes C1 . H11 . 0.960 no C1 . H12 . 0.960 no C2 . C3 . 1.37(2) yes C3 . C4 . 1.41(2) yes C3 . H31 . 0.960 no C4 . C5 . 1.45(2) yes C5 . H51 . 0.960 no C5 . H52 . 0.960 no C6 . C7 . 1.48(3) yes C6 . H61 . 0.960 no C6 . H62 . 0.960 no C7 . C8 . 1.40(3) yes C8 . C9 . 1.40(3) yes C8 . H81 . 0.960 no C9 . C10 . 1.47(2) yes C10 . H101 . 0.960 no C10 . H102 . 0.960 no C41 . C42 . 1.52(4) yes C41 . H411 . 0.960 no C41 . H412 . 0.960 no C42 . O41 . 1.35(4) yes C42 . H421 . 0.960 no C42 . H422 . 0.960 no O41 . C43 . 1.43(5) yes C43 . H431 . 0.960 no C43 . H432 . 0.960 no C43 . H433 . 0.960 no C51 . C52 . 1.45(3) yes C51 . H511 . 0.960 no C51 . H512 . 0.960 no C52 . O51 . 1.26(3) yes C52 . H521 . 0.960 no C52 . H522 . 0.960 no O51 . C53 . 1.38(5) yes C53 . H531 . 0.960 no C53 . H532 . 0.960 no C53 . H533 . 0.960 no C81 . C82 . 1.428(16) yes C81 . H811 . 0.960 no C81 . H812 . 0.960 no C82 . O81 . 1.417(18) yes C82 . O810 . 1.38(3) yes C82 . H821 . 0.960 no C82 . H822 . 0.960 no C11 . C12 . 1.433(18) yes C11 . H111 . 0.960 no C11 . H112 . 0.960 no C12 . O11 . 1.422(18) yes C12 . H121 . 0.960 no C12 . H122 . 0.960 no O11 . C13 . 1.425(18) yes C13 . H131 . 0.960 no C13 . H132 . 0.960 no C13 . H133 . 0.960 no C110 . C120 . 1.437(17) yes C110 . H1101 . 0.960 no C110 . H1102 . 0.960 no C120 . O110 . 1.420(17) yes C120 . H1201 . 0.960 no C120 . H1202 . 0.960 no O110 . C130 . 1.431(17) yes C130 . H1301 . 0.960 no C130 . H1302 . 0.960 no C130 . H1303 . 0.960 no O81 . C83 . 1.422(18) yes C83 . H831 . 0.960 no C83 . H832 . 0.960 no C83 . H833 . 0.960 no O810 . C830 . 1.421(17) yes C830 . H8301 . 0.960 no C830 . H8302 . 0.960 no C830 . H8303 . 0.960 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 I1 . Pt1 . I2 . 91.38(5) yes I1 . Pt1 . N1 . 99.2(4) yes I2 . Pt1 . N1 . 169.2(4) yes I1 . Pt1 . N2 . 177.7(4) yes I2 . Pt1 . N2 . 90.9(4) yes N1 . Pt1 . N2 . 78.5(6) yes I2 . Pt2 . I3 . 90.21(5) yes I2 . Pt2 . N3 . 91.5(4) yes I3 . Pt2 . N3 . 177.6(4) yes I2 . Pt2 . N4 . 169.3(4) yes I3 . Pt2 . N4 . 100.0(4) yes N3 . Pt2 . N4 . 78.4(6) yes I4 . Pt3 . I5 . 90.56(6) yes I4 . Pt3 . N5 . 99.4(5) yes I5 . Pt3 . N5 . 170.0(5) yes I4 . Pt3 . N6 . 176.4(4) yes I5 . Pt3 . N6 . 91.9(4) yes N5 . Pt3 . N6 . 78.1(7) yes I5 . Pt4 . I6 . 90.58(5) yes I5 . Pt4 . N7 . 91.8(5) yes I6 . Pt4 . N7 . 177.5(5) yes I5 . Pt4 . N8 . 168.5(5) yes I6 . Pt4 . N8 . 100.5(5) yes N7 . Pt4 . N8 . 77.2(7) yes Pt1 . I2 . Pt2 . 97.64(5) yes Pt3 . I5 . Pt4 . 97.68(5) yes Pt1 . N1 . C1 . 113.2(11) yes Pt1 . N1 . C11 . 122(2) yes C1 . N1 . C11 . 123(3) yes Pt1 . N1 . C110 . 121.3(15) yes C1 . N1 . C110 . 116.0(19) yes C11 . N1 . C110 . 41(2) yes Pt1 . N1 . H1 . 100.3 no C1 . N1 . H1 . 100.3 no C11 . N1 . H1 . 59.3 no C110 . N1 . H1 . 100.3 no Pt1 . N2 . N3 . 130.0(11) yes Pt1 . N2 . C2 . 121.8(12) yes N3 . N2 . C2 . 108.0(15) yes N2 . N3 . Pt2 . 129.6(11) yes N2 . N3 . C4 . 109.4(13) yes Pt2 . N3 . C4 . 120.7(12) yes Pt2 . N4 . C5 . 110.7(11) yes Pt2 . N4 . C41 . 119.6(14) yes C5 . N4 . C41 . 119.7(18) yes Pt2 . N4 . H2 . 100.6 no C5 . N4 . H2 . 100.6 no C41 . N4 . H2 . 100.6 no Pt3 . N5 . C6 . 113.5(14) yes Pt3 . N5 . C51 . 120.3(18) yes C6 . N5 . C51 . 118(2) yes Pt3 . N5 . H3 . 99.3 no C6 . N5 . H3 . 99.3 no C51 . N5 . H3 . 99.3 no Pt3 . N6 . N7 . 128.5(11) yes Pt3 . N6 . C7 . 122.2(14) yes N7 . N6 . C7 . 109.3(16) yes N6 . N7 . Pt4 . 129.8(11) yes N6 . N7 . C9 . 108.0(14) yes Pt4 . N7 . C9 . 122.2(13) yes Pt4 . N8 . C10 . 113.7(12) yes Pt4 . N8 . C81 . 122.1(14) yes C10 . N8 . C81 . 114.0(17) yes Pt4 . N8 . H4 . 100.7 no C10 . N8 . H4 . 100.7 no C81 . N8 . H4 . 100.7 no N1 . C1 . C2 . 109.1(15) yes N1 . C1 . H11 . 109.6 no C2 . C1 . H11 . 109.6 no N1 . C1 . H12 . 109.6 no C2 . C1 . H12 . 109.6 no H11 . C1 . H12 . 109.5 no C1 . C2 . N2 . 116.6(17) yes C1 . C2 . C3 . 132.9(18) yes N2 . C2 . C3 . 110.4(16) yes C2 . C3 . C4 . 104.3(15) yes C2 . C3 . H31 . 127.9 no C4 . C3 . H31 . 127.9 no C3 . C4 . N3 . 107.8(14) yes C3 . C4 . C5 . 136.8(16) yes N3 . C4 . C5 . 115.1(16) yes C4 . C5 . N4 . 111.7(15) yes C4 . C5 . H51 . 108.9 no N4 . C5 . H51 . 108.9 no C4 . C5 . H52 . 108.9 no N4 . C5 . H52 . 108.9 no H51 . C5 . H52 . 109.5 no N5 . C6 . C7 . 110.8(17) yes N5 . C6 . H61 . 109.1 no C7 . C6 . H61 . 109.1 no N5 . C6 . H62 . 109.1 no C7 . C6 . H62 . 109.1 no H61 . C6 . H62 . 109.5 no C6 . C7 . N6 . 115.2(18) yes C6 . C7 . C8 . 136.7(18) yes N6 . C7 . C8 . 108.1(17) yes C7 . C8 . C9 . 104.9(16) yes C7 . C8 . H81 . 127.5 no C9 . C8 . H81 . 127.5 no C8 . C9 . N7 . 109.7(16) yes C8 . C9 . C10 . 133.9(18) yes N7 . C9 . C10 . 116.4(16) yes C9 . C10 . N8 . 107.6(16) yes C9 . C10 . H101 . 109.9 no N8 . C10 . H101 . 109.9 no C9 . C10 . H102 . 109.9 no N8 . C10 . H102 . 109.9 no H101 . C10 . H102 . 109.5 no N4 . C41 . C42 . 116(2) yes N4 . C41 . H411 . 107.9 no C42 . C41 . H411 . 107.9 no N4 . C41 . H412 . 107.9 no C42 . C41 . H412 . 107.9 no H411 . C41 . H412 . 109.5 no C41 . C42 . O41 . 102(2) yes C41 . C42 . H421 . 111.3 no O41 . C42 . H421 . 111.3 no C41 . C42 . H422 . 111.3 no O41 . C42 . H422 . 111.3 no H421 . C42 . H422 . 109.5 no C42 . O41 . C43 . 109(3) yes O41 . C43 . H431 . 109.5 no O41 . C43 . H432 . 109.4 no H431 . C43 . H432 . 109.5 no O41 . C43 . H433 . 109.5 no H431 . C43 . H433 . 109.5 no H432 . C43 . H433 . 109.5 no N5 . C51 . C52 . 121(2) yes N5 . C51 . H511 . 106.5 no C52 . C51 . H511 . 106.5 no N5 . C51 . H512 . 106.5 no C52 . C51 . H512 . 106.5 no H511 . C51 . H512 . 109.5 no C51 . C52 . O51 . 112(2) yes C51 . C52 . H521 . 108.9 no O51 . C52 . H521 . 108.9 no C51 . C52 . H522 . 108.9 no O51 . C52 . H522 . 108.9 no H521 . C52 . H522 . 109.5 no C52 . O51 . C53 . 116(3) yes O51 . C53 . H531 . 109.5 no O51 . C53 . H532 . 109.5 no H531 . C53 . H532 . 109.5 no O51 . C53 . H533 . 109.5 no H531 . C53 . H533 . 109.5 no H532 . C53 . H533 . 109.5 no N8 . C81 . C82 . 123.4(19) yes N8 . C81 . H811 . 105.9 no C82 . C81 . H811 . 105.9 no N8 . C81 . H812 . 105.9 no C82 . C81 . H812 . 105.9 no H811 . C81 . H812 . 109.5 no C81 . C82 . O81 . 136(3) yes C81 . C82 . O810 . 102.7(18) yes O81 . C82 . O810 . 73(2) yes C81 . C82 . H821 . 102.5 no O81 . C82 . H821 . 102.5 no O810 . C82 . H821 . 44.0 no C81 . C82 . H822 . 102.5 no O81 . C82 . H822 . 102.5 no O810 . C82 . H822 . 147.1 no H821 . C82 . H822 . 109.5 no N1 . C11 . C12 . 122(4) yes N1 . C11 . H111 . 106.3 no C12 . C11 . H111 . 106.3 no N1 . C11 . H112 . 106.3 no C12 . C11 . H112 . 106.3 no H111 . C11 . H112 . 109.5 no C11 . C12 . O11 . 109(4) yes C11 . C12 . H121 . 109.5 no O11 . C12 . H121 . 109.5 no C11 . C12 . H122 . 109.5 no O11 . C12 . H122 . 109.5 no H121 . C12 . H122 . 109.5 no C12 . O11 . C13 . 111(3) yes O11 . C13 . H131 . 109.5 no O11 . C13 . H132 . 109.5 no H131 . C13 . H132 . 109.5 no O11 . C13 . H133 . 109.5 no H131 . C13 . H133 . 109.5 no H132 . C13 . H133 . 109.5 no N1 . C110 . C120 . 118(2) yes N1 . C110 . H1101 . 107.2 no C120 . C110 . H1101 . 107.2 no N1 . C110 . H1102 . 107.2 no C120 . C110 . H1102 . 107.2 no H1101 . C110 . H1102 . 109.5 no C110 . C120 . O110 . 107(3) yes C110 . C120 . H1201 . 110.1 no O110 . C120 . H1201 . 110.1 no C110 . C120 . H1202 . 110.1 no O110 . C120 . H1202 . 110.1 no H1201 . C120 . H1202 . 109.5 no C120 . O110 . C130 . 109(2) yes O110 . C130 . H1301 . 109.5 no O110 . C130 . H1302 . 109.5 no H1301 . C130 . H1302 . 109.5 no O110 . C130 . H1303 . 109.5 no H1301 . C130 . H1303 . 109.5 no H1302 . C130 . H1303 . 109.5 no C82 . O81 . C83 . 114(5) yes O81 . C83 . H831 . 109.5 no O81 . C83 . H832 . 109.5 no H831 . C83 . H832 . 109.5 no O81 . C83 . H833 . 109.5 no H831 . C83 . H833 . 109.5 no H832 . C83 . H833 . 109.5 no C82 . O810 . C830 . 113(2) yes O810 . C830 . H8301 . 109.5 no O810 . C830 . H8302 . 109.5 no H8301 . C830 . H8302 . 109.5 no O810 . C830 . H8303 . 109.5 no H8301 . C830 . H8303 . 109.5 no H8302 . C830 . H8303 . 109.5 no