#------------------------------------------------------------------------------ #$Date: 2020-08-29 04:40:53 +0300 (Sat, 29 Aug 2020) $ #$Revision: 255724 $ #$URL: file:///home/coder/svn-repositories/cod/cif/7/70/53/7705300.cif $ #------------------------------------------------------------------------------ # # This file is available in the Crystallography Open Database (COD), # http://www.crystallography.net/ # # All data on this site have been placed in the public domain by the # contributors. # data_7705300 loop_ _publ_author_name 'Exp\'osito, J. Emilio' 'Aull\'on, Gabriel' 'Bardaji, Manuel' 'Miguel, Jesus Angel' 'Espinet, Pablo' _publ_section_title ; Fluorescent perylenylpyridine complexes: an experimental and theoretical study ; _journal_name_full 'Dalton Transactions' _journal_paper_doi 10.1039/D0DT02494E _journal_year 2020 _chemical_formula_moiety 'C32 H26 I N O2 Pt' _chemical_formula_sum 'C32 H26 I N O2 Pt' _chemical_formula_weight 778.53 _space_group_crystal_system triclinic _space_group_IT_number 2 _space_group_name_Hall '-P 1' _space_group_name_H-M_alt 'P -1' _atom_sites_solution_hydrogens geom _atom_sites_solution_primary dual _audit_creation_date 2020-07-08 _audit_creation_method ; Olex2 1.2 (compiled 2018.05.29 svn.r3508 for OlexSys, GUI svn.r5506) ; _audit_update_record ; 2020-07-10 deposited with the CCDC. 2020-08-28 downloaded from the CCDC. ; _cell_angle_alpha 80.964(3) _cell_angle_beta 84.500(4) _cell_angle_gamma 81.117(4) _cell_formula_units_Z 2 _cell_length_a 7.7315(5) _cell_length_b 12.3683(5) _cell_length_c 13.9478(4) _cell_measurement_reflns_used 4809 _cell_measurement_temperature 293 _cell_measurement_theta_max 28.3090 _cell_measurement_theta_min 2.6590 _cell_volume 1297.91(11) _computing_cell_refinement ; CrysAlisPro, Agilent Technologies, Version 1.171.37.31 (release 14-01-2014 CrysAlis171 .NET) (compiled Jan 14 2014,18:38:05) ; _computing_data_collection ; CrysAlisPro, Agilent Technologies, Version 1.171.37.31 (release 14-01-2014 CrysAlis171 .NET) (compiled Jan 14 2014,18:38:05) ; _computing_data_reduction ; CrysAlisPro, Agilent Technologies, Version 1.171.37.31 (release 14-01-2014 CrysAlis171 .NET) (compiled Jan 14 2014,18:38:05) ; _computing_molecular_graphics 'Olex2 (Dolomanov et al., 2009)' _computing_publication_material 'Olex2 (Dolomanov et al., 2009)' _computing_structure_refinement 'ShelXL (Sheldrick, 2015)' _computing_structure_solution 'ShelXT (Sheldrick, 2015)' _diffrn_ambient_temperature 293 _diffrn_detector 'CCD plate' _diffrn_detector_area_resol_mean 10.4757 _diffrn_detector_type Atlas _diffrn_measured_fraction_theta_full 1.000 _diffrn_measured_fraction_theta_max 0.827 _diffrn_measurement_details ; #__ type_ start__ end____ width___ exp.time_ 1 omega -38.00 60.00 1.0000 2.6900 omega____ theta____ kappa____ phi______ frames - -9.9495 57.0000 150.0000 98 #__ type_ start__ end____ width___ exp.time_ 2 omega -78.00 11.00 1.0000 2.6900 omega____ theta____ kappa____ phi______ frames - -9.9495 -57.0000 0.0000 89 #__ type_ start__ end____ width___ exp.time_ 3 omega -10.00 78.00 1.0000 2.6900 omega____ theta____ kappa____ phi______ frames - 11.9027 77.0000 -90.0000 88 ; _diffrn_measurement_device 'four-circle diffractometer' _diffrn_measurement_device_type 'SuperNova, Dual, Cu at zero, Atlas' _diffrn_measurement_method '\w scans' _diffrn_orient_matrix_UB_11 0.0672584000 _diffrn_orient_matrix_UB_12 -0.0436515000 _diffrn_orient_matrix_UB_13 -0.0097312000 _diffrn_orient_matrix_UB_21 -0.0511452000 _diffrn_orient_matrix_UB_22 -0.0389465000 _diffrn_orient_matrix_UB_23 0.0269430000 _diffrn_orient_matrix_UB_31 -0.0391051000 _diffrn_orient_matrix_UB_32 -0.0043405000 _diffrn_orient_matrix_UB_33 -0.0429563000 _diffrn_radiation_monochromator mirror _diffrn_radiation_probe x-ray _diffrn_radiation_type MoK\a _diffrn_radiation_wavelength 0.71073 _diffrn_reflns_av_R_equivalents 0.0289 _diffrn_reflns_av_unetI/netI 0.0567 _diffrn_reflns_Laue_measured_fraction_full 1.000 _diffrn_reflns_Laue_measured_fraction_max 0.827 _diffrn_reflns_limit_h_max 8 _diffrn_reflns_limit_h_min -9 _diffrn_reflns_limit_k_max 16 _diffrn_reflns_limit_k_min -14 _diffrn_reflns_limit_l_max 19 _diffrn_reflns_limit_l_min -14 _diffrn_reflns_number 10089 _diffrn_reflns_point_group_measured_fraction_full 1.000 _diffrn_reflns_point_group_measured_fraction_max 0.827 _diffrn_reflns_theta_full 25.242 _diffrn_reflns_theta_max 29.626 _diffrn_reflns_theta_min 2.077 _diffrn_source 'SuperNova (Mo) X-ray Source' _exptl_absorpt_coefficient_mu 6.626 _exptl_absorpt_correction_T_max 0.756 _exptl_absorpt_correction_T_min 0.434 _exptl_absorpt_correction_type gaussian _exptl_absorpt_process_details ; CrysAlisPro, Agilent Technologies, Version 1.171.37.31 (release 14-01-2014 CrysAlis171 .NET) (compiled Jan 14 2014,18:38:05) Numerical absorption correction based on gaussian integration over a multifaceted crystal model Empirical absorption correction using spherical harmonics, implemented in SCALE3 ABSPACK scaling algorithm. ; _exptl_crystal_colour red _exptl_crystal_colour_primary red _exptl_crystal_density_diffrn 1.992 _exptl_crystal_description prism _exptl_crystal_F_000 744 _exptl_crystal_size_max 0.3042 _exptl_crystal_size_mid 0.2468 _exptl_crystal_size_min 0.0645 _refine_diff_density_max 0.583 _refine_diff_density_min -1.220 _refine_diff_density_rms 0.153 _refine_ls_extinction_method none _refine_ls_goodness_of_fit_ref 1.036 _refine_ls_hydrogen_treatment constr _refine_ls_matrix_type full _refine_ls_number_parameters 338 _refine_ls_number_reflns 6049 _refine_ls_number_restraints 0 _refine_ls_restrained_S_all 1.036 _refine_ls_R_factor_all 0.0482 _refine_ls_R_factor_gt 0.0356 _refine_ls_shift/su_max 0.000 _refine_ls_shift/su_mean 0.000 _refine_ls_structure_factor_coef Fsqd _refine_ls_weighting_details 'w=1/[\s^2^(Fo^2^)+(0.0257P)^2^] where P=(Fo^2^+2Fc^2^)/3' _refine_ls_weighting_scheme calc _refine_ls_wR_factor_gt 0.0673 _refine_ls_wR_factor_ref 0.0751 _reflns_Friedel_coverage 0.000 _reflns_number_gt 5087 _reflns_number_total 6049 _reflns_threshold_expression 'I > 2\s(I)' _cod_data_source_file d0dt02494e2.cif _cod_data_source_block 10 _cod_original_cell_volume 1297.91(10) _cod_database_code 7705300 _shelx_shelxl_version_number 2018/3 _chemical_oxdiff_formula 'C32 H26 I N O2 Pt' _chemical_oxdiff_usercomment 'RED DICLORME/ETER' _shelx_space_group_comment ; The symmetry employed for this shelxl refinement is uniquely defined by the following loop, which should always be used as a source of symmetry information in preference to the above space-group names. They are only intended as comments. ; _reflns_odcompleteness_completeness 99.92 _reflns_odcompleteness_iscentric 1 _reflns_odcompleteness_theta 26.32 _olex2_refinement_description ; 1. Fixed Uiso At 1.2 times of: All C(H) groups At 1.5 times of: All C(H,H,H) groups 2.a Aromatic/amide H refined with riding coordinates: C3(H3), C7(H7), C8(H8), C9(H9), C14(H14), C15(H15), C16(H16), C18(H18), C19(H19), C20(H20), C22(H22), C24(H24), C25(H25), C29(H29) 2.b Idealised Me refined as rotating group: C26(H26A,H26B,H26C), C27(H27A,H27B,H27C), C31(H31A,H31B,H31C), C45(H45A,H45B, H45C) ; _shelx_res_file ; TITL exp_1201 in P-1 je273.res created by SHELXL-2018/3 at 17:20:50 on 08-Jul-2020 REM P-1 (#2 in standard setting) CELL 0.71073 7.731511 12.368332 13.9478 80.9641 84.5004 81.1173 ZERR 2 0.000469 0.000472 0.000387 0.0027 0.0035 0.0041 LATT 1 SFAC C H I N O Pt UNIT 64 52 2 2 4 2 L.S. 20 PLAN 6 TEMP 19.85 BOND fmap 2 acta REM REM REM WGHT 0.025700 FVAR 2.56208 PT1 6 0.058463 0.291899 0.243580 11.00000 0.03840 0.02678 = 0.02794 -0.00457 0.00421 -0.00687 I1 3 0.364381 0.250342 0.342643 11.00000 0.04875 0.05208 = 0.04308 -0.00455 -0.00651 -0.00970 O1 5 0.112382 0.442935 0.180056 11.00000 0.04504 0.03159 = 0.03347 -0.00096 0.00650 -0.00774 O2 5 -0.080387 0.358807 0.364555 11.00000 0.05186 0.03468 = 0.03224 -0.00497 0.00979 -0.00701 N1 4 0.002010 0.139597 0.289943 11.00000 0.03990 0.02848 = 0.03142 -0.00515 0.00301 -0.00397 C1 1 0.161419 0.104726 0.141057 11.00000 0.02880 0.03338 = 0.02671 -0.00382 -0.00177 -0.00500 C2 1 0.174184 0.216402 0.134091 11.00000 0.03179 0.02647 = 0.02767 -0.00655 0.00057 -0.00076 C3 1 0.256841 0.272138 0.051310 11.00000 0.03467 0.02458 = 0.03392 -0.00451 0.00104 -0.00487 AFIX 43 H3 2 0.268771 0.346070 0.049843 11.00000 -1.20000 AFIX 0 C4 1 0.321232 0.220206 -0.028345 11.00000 0.03159 0.02586 = 0.02876 0.00131 -0.00553 -0.00058 C5 1 0.299674 0.107447 -0.027245 11.00000 0.02593 0.03341 = 0.02959 0.00015 -0.00528 0.00118 C6 1 0.219605 0.047699 0.059129 11.00000 0.02816 0.03196 = 0.03039 -0.00532 -0.00524 -0.00420 C7 1 0.192440 -0.061260 0.054173 11.00000 0.04921 0.03317 = 0.03243 -0.00402 -0.00289 -0.01073 AFIX 43 H7 2 0.134273 -0.100213 0.106752 11.00000 -1.20000 AFIX 0 C8 1 0.249240 -0.110635 -0.025593 11.00000 0.07010 0.02686 = 0.04135 -0.01258 -0.00670 -0.00927 AFIX 43 H8 2 0.234103 -0.183850 -0.025232 11.00000 -1.20000 AFIX 0 C9 1 0.329030 -0.054709 -0.107336 11.00000 0.04529 0.03926 = 0.03314 -0.01452 -0.00113 -0.00448 AFIX 43 H9 2 0.367728 -0.090836 -0.160757 11.00000 -1.20000 AFIX 0 C10 1 0.351845 0.054414 -0.110426 11.00000 0.02700 0.03578 = 0.03244 -0.00783 -0.00499 0.00186 C11 1 0.426717 0.116752 -0.199921 11.00000 0.03382 0.04353 = 0.02669 -0.00372 -0.00310 0.00016 C12 1 0.450998 0.228066 -0.200201 11.00000 0.02917 0.04037 = 0.02761 0.00037 0.00020 0.00231 C13 1 0.405876 0.281156 -0.114888 11.00000 0.03184 0.03537 = 0.02971 0.00411 -0.00120 -0.00161 C14 1 0.440037 0.388007 -0.117271 11.00000 0.04238 0.03743 = 0.03920 0.00059 0.00499 -0.00536 AFIX 43 H14 2 0.413311 0.422272 -0.061857 11.00000 -1.20000 AFIX 0 C15 1 0.514864 0.445849 -0.202548 11.00000 0.03988 0.03986 = 0.05359 0.00417 0.00668 -0.00788 AFIX 43 H15 2 0.539188 0.517135 -0.202329 11.00000 -1.20000 AFIX 0 C16 1 0.551245 0.399007 -0.283921 11.00000 0.04374 0.05375 = 0.04161 0.01212 0.00836 -0.00484 AFIX 43 H16 2 0.595539 0.439855 -0.340140 11.00000 -1.20000 AFIX 0 C17 1 0.524144 0.289804 -0.286391 11.00000 0.03614 0.05012 = 0.03500 0.00334 -0.00010 -0.00009 C18 1 0.559651 0.239757 -0.371071 11.00000 0.04907 0.06324 = 0.03051 0.00187 0.00450 -0.00114 AFIX 43 H18 2 0.601239 0.280009 -0.428357 11.00000 -1.20000 AFIX 0 C19 1 0.534200 0.133255 -0.370705 11.00000 0.06310 0.07422 = 0.03171 -0.01384 0.00815 -0.00250 AFIX 43 H19 2 0.559745 0.100927 -0.427216 11.00000 -1.20000 AFIX 0 C20 1 0.469193 0.072099 -0.284735 11.00000 0.05199 0.05270 = 0.03633 -0.01403 0.00251 -0.00243 AFIX 43 H20 2 0.454488 -0.001005 -0.285349 11.00000 -1.20000 AFIX 0 C21 1 0.075051 0.059981 0.234321 11.00000 0.03247 0.03355 = 0.02941 -0.00208 -0.00531 -0.00908 C22 1 0.061690 -0.049565 0.273365 11.00000 0.05007 0.03161 = 0.03260 -0.00604 0.00323 -0.00797 AFIX 43 H22 2 0.120961 -0.105972 0.240734 11.00000 -1.20000 AFIX 0 C23 1 -0.037327 -0.076593 0.359305 11.00000 0.04842 0.03660 = 0.03436 -0.00230 -0.00184 -0.01537 C24 1 -0.121927 0.007371 0.407463 11.00000 0.05661 0.04310 = 0.03359 -0.00347 0.01245 -0.01610 AFIX 43 H24 2 -0.194856 -0.008203 0.463355 11.00000 -1.20000 AFIX 0 C25 1 -0.098081 0.114469 0.372512 11.00000 0.04731 0.03631 = 0.03902 -0.00834 0.01214 -0.01051 AFIX 43 H25 2 -0.152223 0.170946 0.406587 11.00000 -1.20000 AFIX 0 C26 1 -0.051661 -0.196062 0.398688 11.00000 0.07093 0.03721 = 0.04943 0.00175 0.01037 -0.01718 AFIX 137 H26A 2 -0.052242 -0.206623 0.468386 11.00000 -1.50000 H26B 2 0.046673 -0.242724 0.372536 11.00000 -1.50000 H26C 2 -0.158525 -0.214772 0.380172 11.00000 -1.50000 AFIX 0 C27 1 0.068190 0.635159 0.139200 11.00000 0.04469 0.03997 = 0.04989 0.00203 -0.00160 -0.00186 AFIX 137 H27A 2 0.190178 0.629340 0.116853 11.00000 -1.50000 H27B 2 0.036543 0.698944 0.171856 11.00000 -1.50000 H27C 2 -0.001571 0.642388 0.084587 11.00000 -1.50000 AFIX 0 C28 1 0.035994 0.533165 0.208512 11.00000 0.04130 0.02541 = 0.03573 -0.00446 -0.00717 -0.00445 C29 1 -0.067892 0.544397 0.293887 11.00000 0.05227 0.03348 = 0.04157 -0.01173 0.00079 -0.00689 AFIX 43 H29 2 -0.110655 0.616544 0.303991 11.00000 -1.20000 AFIX 0 C30 1 -0.116944 0.460963 0.367102 11.00000 0.04407 0.03131 = 0.03115 -0.00906 -0.00014 -0.00037 C31 1 -0.224439 0.494200 0.455838 11.00000 0.06764 0.05184 = 0.04165 -0.01174 0.01152 -0.00869 AFIX 137 H31A 2 -0.334593 0.466190 0.461258 11.00000 -1.50000 H31B 2 -0.245295 0.573400 0.450432 11.00000 -1.50000 H31C 2 -0.162245 0.464288 0.512632 11.00000 -1.50000 AFIX 0 C45 1 -0.169665 0.327182 0.173064 11.00000 0.04614 0.03728 = 0.05091 -0.01144 -0.00215 -0.00329 AFIX 137 H45A 2 -0.257306 0.370531 0.210130 11.00000 -1.50000 H45B 2 -0.210493 0.259462 0.166396 11.00000 -1.50000 H45C 2 -0.147694 0.368026 0.109746 11.00000 -1.50000 AFIX 0 HKLF 4 REM exp_1201 in P-1 REM wR2 = 0.0751, GooF = S = 1.036, Restrained GooF = 1.036 for all data REM R1 = 0.0356 for 5087 Fo > 4sig(Fo) and 0.0482 for all 6049 data REM 338 parameters refined using 0 restraints END WGHT 0.0257 0.0000 REM Highest difference peak 0.583, deepest hole -1.220, 1-sigma level 0.153 Q1 1 0.0020 0.2026 0.3066 11.00000 0.05 0.58 Q2 1 0.1492 0.2155 0.3794 11.00000 0.05 0.55 Q3 1 0.1968 -0.2215 0.2613 11.00000 0.05 0.54 Q4 1 -0.4754 0.5627 0.4624 11.00000 0.05 0.53 Q5 1 -0.0429 0.6792 0.1205 11.00000 0.05 0.52 Q6 1 0.5373 0.3774 -0.0009 11.00000 0.05 0.52 ; _shelx_res_checksum 63185 _olex2_submission_special_instructions 'No special instructions were received' loop_ _space_group_symop_operation_xyz 'x, y, z' '-x, -y, -z' 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_site_symmetry_order _atom_site_calc_flag _atom_site_refinement_flags_posn _atom_site_refinement_flags_adp _atom_site_refinement_flags_occupancy _atom_site_disorder_assembly _atom_site_disorder_group Pt1 Pt 0.05846(3) 0.29190(2) 0.24358(2) 0.03117(7) Uani 1 1 d . . . . . I1 I 0.36438(6) 0.25034(3) 0.34264(2) 0.04775(11) Uani 1 1 d . . . . . O1 O 0.1124(5) 0.4429(3) 0.1801(2) 0.0375(9) Uani 1 1 d . . . . . O2 O -0.0804(5) 0.3588(3) 0.3646(2) 0.0403(9) Uani 1 1 d . . . . . N1 N 0.0020(6) 0.1396(3) 0.2899(3) 0.0336(10) Uani 1 1 d . . . . . C1 C 0.1614(7) 0.1047(4) 0.1411(3) 0.0296(11) Uani 1 1 d . . . . . C2 C 0.1742(7) 0.2164(4) 0.1341(3) 0.0289(10) Uani 1 1 d . . . . . C3 C 0.2568(7) 0.2721(4) 0.0513(3) 0.0312(11) Uani 1 1 d . . . . . H3 H 0.268771 0.346070 0.049843 0.037 Uiso 1 1 calc R . . . . C4 C 0.3212(7) 0.2202(4) -0.0283(3) 0.0295(11) Uani 1 1 d . . . . . C5 C 0.2997(7) 0.1074(4) -0.0272(3) 0.0305(11) Uani 1 1 d . . . . . C6 C 0.2196(7) 0.0477(4) 0.0591(3) 0.0299(11) Uani 1 1 d . . . . . C7 C 0.1924(8) -0.0613(4) 0.0542(3) 0.0378(13) Uani 1 1 d . . . . . H7 H 0.134273 -0.100213 0.106752 0.045 Uiso 1 1 calc R . . . . C8 C 0.2492(9) -0.1106(4) -0.0256(4) 0.0448(15) Uani 1 1 d . . . . . H8 H 0.234103 -0.183850 -0.025232 0.054 Uiso 1 1 calc R . . . . C9 C 0.3290(8) -0.0547(4) -0.1073(3) 0.0385(13) Uani 1 1 d . . . . . H9 H 0.367728 -0.090836 -0.160757 0.046 Uiso 1 1 calc R . . . . C10 C 0.3518(7) 0.0544(4) -0.1104(3) 0.0319(11) Uani 1 1 d . . . . . C11 C 0.4267(7) 0.1168(4) -0.1999(3) 0.0354(12) Uani 1 1 d . . . . . C12 C 0.4510(7) 0.2281(4) -0.2002(3) 0.0339(12) Uani 1 1 d . . . . . C13 C 0.4059(7) 0.2812(4) -0.1149(3) 0.0337(12) Uani 1 1 d . . . . . C14 C 0.4400(8) 0.3880(4) -0.1173(4) 0.0409(13) Uani 1 1 d . . . . . H14 H 0.413311 0.422272 -0.061857 0.049 Uiso 1 1 calc R . . . . C15 C 0.5149(8) 0.4458(5) -0.2025(4) 0.0461(14) Uani 1 1 d . . . . . H15 H 0.539188 0.517135 -0.202329 0.055 Uiso 1 1 calc R . . . . C16 C 0.5512(8) 0.3990(5) -0.2839(4) 0.0494(16) Uani 1 1 d . . . . . H16 H 0.595539 0.439855 -0.340140 0.059 Uiso 1 1 calc R . . . . C17 C 0.5241(8) 0.2898(5) -0.2864(4) 0.0423(13) Uani 1 1 d . . . . . C18 C 0.5597(8) 0.2398(5) -0.3711(4) 0.0498(16) Uani 1 1 d . . . . . H18 H 0.601239 0.280009 -0.428357 0.060 Uiso 1 1 calc R . . . . C19 C 0.5342(9) 0.1333(6) -0.3707(4) 0.0572(18) Uani 1 1 d . . . . . H19 H 0.559745 0.100927 -0.427216 0.069 Uiso 1 1 calc R . . . . C20 C 0.4692(8) 0.0721(5) -0.2847(4) 0.0471(15) Uani 1 1 d . . . . . H20 H 0.454488 -0.001005 -0.285349 0.057 Uiso 1 1 calc R . . . . C21 C 0.0751(7) 0.0600(4) 0.2343(3) 0.0314(11) Uani 1 1 d . . . . . C22 C 0.0617(8) -0.0496(4) 0.2734(3) 0.0381(13) Uani 1 1 d . . . . . H22 H 0.120961 -0.105972 0.240734 0.046 Uiso 1 1 calc R . . . . C23 C -0.0373(8) -0.0766(4) 0.3593(3) 0.0392(13) Uani 1 1 d . . . . . C24 C -0.1219(8) 0.0074(4) 0.4075(4) 0.0447(14) Uani 1 1 d . . . . . H24 H -0.194856 -0.008203 0.463355 0.054 Uiso 1 1 calc R . . . . C25 C -0.0981(8) 0.1145(4) 0.3725(4) 0.0411(13) Uani 1 1 d . . . . . H25 H -0.152223 0.170946 0.406587 0.049 Uiso 1 1 calc R . . . . C26 C -0.0517(9) -0.1961(4) 0.3987(4) 0.0534(17) Uani 1 1 d . . . . . H26A H -0.052242 -0.206623 0.468386 0.080 Uiso 1 1 calc GR . . . . H26B H 0.046673 -0.242724 0.372536 0.080 Uiso 1 1 calc GR . . . . H26C H -0.158525 -0.214772 0.380172 0.080 Uiso 1 1 calc GR . . . . C27 C 0.0682(8) 0.6352(4) 0.1392(4) 0.0463(14) Uani 1 1 d . . . . . H27A H 0.190178 0.629340 0.116853 0.070 Uiso 1 1 calc GR . . . . H27B H 0.036543 0.698944 0.171856 0.070 Uiso 1 1 calc GR . . . . H27C H -0.001571 0.642388 0.084587 0.070 Uiso 1 1 calc GR . . . . C28 C 0.0360(7) 0.5332(4) 0.2085(3) 0.0339(12) Uani 1 1 d . . . . . C29 C -0.0679(8) 0.5444(4) 0.2939(4) 0.0419(13) Uani 1 1 d . . . . . H29 H -0.110655 0.616544 0.303991 0.050 Uiso 1 1 calc R . . . . C30 C -0.1169(7) 0.4610(4) 0.3671(3) 0.0357(12) Uani 1 1 d . . . . . C31 C -0.2244(9) 0.4942(5) 0.4558(4) 0.0542(17) Uani 1 1 d . . . . . H31A H -0.334593 0.466190 0.461258 0.081 Uiso 1 1 calc GR . . . . H31B H -0.245295 0.573400 0.450432 0.081 Uiso 1 1 calc GR . . . . H31C H -0.162245 0.464288 0.512632 0.081 Uiso 1 1 calc GR . . . . C45 C -0.1697(8) 0.3272(5) 0.1731(4) 0.0446(14) Uani 1 1 d . . . . . H45A H -0.257306 0.370531 0.210130 0.067 Uiso 1 1 calc GR . . . . H45B H -0.210493 0.259462 0.166396 0.067 Uiso 1 1 calc GR . . . . H45C H -0.147694 0.368026 0.109746 0.067 Uiso 1 1 calc GR . . . . 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 0.03840(13) 0.02678(11) 0.02794(10) -0.00457(7) 0.00421(8) -0.00687(8) I1 0.0488(3) 0.0521(2) 0.04308(19) -0.00455(16) -0.00651(16) -0.00970(19) O1 0.045(2) 0.0316(19) 0.0335(17) -0.0010(15) 0.0065(16) -0.0077(17) O2 0.052(3) 0.035(2) 0.0322(17) -0.0050(15) 0.0098(16) -0.0070(18) N1 0.040(3) 0.028(2) 0.031(2) -0.0052(17) 0.0030(18) -0.0040(19) C1 0.029(3) 0.033(3) 0.027(2) -0.004(2) -0.0018(19) -0.005(2) C2 0.032(3) 0.026(2) 0.028(2) -0.0066(19) 0.0006(19) -0.001(2) C3 0.035(3) 0.025(2) 0.034(2) -0.005(2) 0.001(2) -0.005(2) C4 0.032(3) 0.026(2) 0.029(2) 0.0013(19) -0.006(2) -0.001(2) C5 0.026(3) 0.033(3) 0.030(2) 0.000(2) -0.0053(19) 0.001(2) C6 0.028(3) 0.032(3) 0.030(2) -0.005(2) -0.005(2) -0.004(2) C7 0.049(4) 0.033(3) 0.032(2) -0.004(2) -0.003(2) -0.011(2) C8 0.070(5) 0.027(3) 0.041(3) -0.013(2) -0.007(3) -0.009(3) C9 0.045(4) 0.039(3) 0.033(3) -0.015(2) -0.001(2) -0.004(3) C10 0.027(3) 0.036(3) 0.032(2) -0.008(2) -0.005(2) 0.002(2) C11 0.034(3) 0.044(3) 0.027(2) -0.004(2) -0.003(2) 0.000(2) C12 0.029(3) 0.040(3) 0.028(2) 0.000(2) 0.000(2) 0.002(2) C13 0.032(3) 0.035(3) 0.030(2) 0.004(2) -0.001(2) -0.002(2) C14 0.042(4) 0.037(3) 0.039(3) 0.001(2) 0.005(2) -0.005(3) C15 0.040(4) 0.040(3) 0.054(3) 0.004(3) 0.007(3) -0.008(3) C16 0.044(4) 0.054(4) 0.042(3) 0.012(3) 0.008(3) -0.005(3) C17 0.036(3) 0.050(3) 0.035(3) 0.003(2) 0.000(2) 0.000(3) C18 0.049(4) 0.063(4) 0.031(3) 0.002(3) 0.005(2) -0.001(3) C19 0.063(5) 0.074(5) 0.032(3) -0.014(3) 0.008(3) -0.002(4) C20 0.052(4) 0.053(4) 0.036(3) -0.014(3) 0.003(3) -0.002(3) C21 0.032(3) 0.034(3) 0.029(2) -0.002(2) -0.005(2) -0.009(2) C22 0.050(4) 0.032(3) 0.033(2) -0.006(2) 0.003(2) -0.008(3) C23 0.048(4) 0.037(3) 0.034(3) -0.002(2) -0.002(2) -0.015(3) C24 0.057(4) 0.043(3) 0.034(3) -0.003(2) 0.012(2) -0.016(3) C25 0.047(4) 0.036(3) 0.039(3) -0.008(2) 0.012(2) -0.011(3) C26 0.071(5) 0.037(3) 0.049(3) 0.002(3) 0.010(3) -0.017(3) C27 0.045(4) 0.040(3) 0.050(3) 0.002(3) -0.002(3) -0.002(3) C28 0.041(3) 0.025(2) 0.036(3) -0.004(2) -0.007(2) -0.004(2) C29 0.052(4) 0.033(3) 0.042(3) -0.012(2) 0.001(3) -0.007(3) C30 0.044(4) 0.031(3) 0.031(2) -0.009(2) 0.000(2) 0.000(2) C31 0.068(5) 0.052(4) 0.042(3) -0.012(3) 0.012(3) -0.009(3) C45 0.046(4) 0.037(3) 0.051(3) -0.011(2) -0.002(3) -0.003(3) loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' I I -0.4742 1.8119 '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' loop_ _exptl_crystal_face_index_h _exptl_crystal_face_index_k _exptl_crystal_face_index_l _exptl_crystal_face_perp_dist _exptl_oxdiff_crystal_face_indexfrac_h _exptl_oxdiff_crystal_face_indexfrac_k _exptl_oxdiff_crystal_face_indexfrac_l _exptl_oxdiff_crystal_face_x _exptl_oxdiff_crystal_face_y _exptl_oxdiff_crystal_face_z 1 0 -19 0.0451 1.0375 0.0033 -18.9910 0.2544 -0.5649 0.7752 -1 0 19 0.0195 -1.0375 -0.0033 18.9910 -0.2544 0.5649 -0.7752 10 8 2 0.1232 9.9985 8.0037 2.0034 0.3036 -0.7691 -0.5118 -10 -8 -5 0.1202 -9.9926 -8.0032 -5.0021 -0.2741 0.6880 0.6404 1 16 -4 0.1128 1.0121 16.0032 -4.0002 -0.5916 -0.7828 0.0628 -6 -6 -17 0.1009 -5.9683 -5.9999 -16.9949 0.0259 0.0810 0.9895 2 -12 12 0.0758 1.9733 -12.0030 11.9977 0.5399 0.6898 -0.5404 5 -1 18 0.0524 4.9645 -1.0015 17.9950 0.2025 0.2699 -0.9628 -4 13 -8 0.1451 -3.9810 13.0019 -8.0007 -0.7575 -0.5183 0.4429 2 16 -6 0.0980 2.0161 16.0038 -5.9987 -0.5046 -0.8880 0.1094 11 -1 3 0.0753 10.9942 -0.9974 3.0050 0.7538 -0.4425 -0.5547 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 O1 Pt1 I1 92.21(11) . . ? O1 Pt1 O2 91.53(13) . . ? O1 Pt1 C45 86.81(19) . . ? O2 Pt1 I1 89.63(11) . . ? N1 Pt1 I1 92.02(13) . . ? N1 Pt1 O1 173.06(14) . . ? N1 Pt1 O2 94.00(14) . . ? N1 Pt1 C45 89.1(2) . . ? C2 Pt1 I1 92.41(15) . . ? C2 Pt1 O1 93.93(16) . . ? C2 Pt1 O2 174.09(16) . . ? C2 Pt1 N1 80.39(17) . . ? C2 Pt1 C45 89.4(2) . . ? C45 Pt1 I1 178.02(16) . . ? C45 Pt1 O2 88.67(19) . . ? C28 O1 Pt1 123.1(3) . . ? C30 O2 Pt1 123.0(3) . . ? C21 N1 Pt1 116.2(3) . . ? C25 N1 Pt1 122.6(3) . . ? C25 N1 C21 121.2(4) . . ? C2 C1 C6 119.7(4) . . ? C2 C1 C21 113.0(4) . . ? C6 C1 C21 127.2(4) . . ? C1 C2 Pt1 116.2(3) . . ? C1 C2 C3 120.8(4) . . ? C3 C2 Pt1 122.8(3) . . ? C4 C3 C2 121.8(4) . . ? C3 C4 C5 119.3(4) . . ? C3 C4 C13 120.6(4) . . ? C5 C4 C13 120.1(4) . . ? C4 C5 C6 119.5(4) . . ? C10 C5 C4 120.7(4) . . ? C10 C5 C6 119.8(4) . . ? C1 C6 C5 118.7(4) . . ? C7 C6 C1 124.1(4) . . ? C7 C6 C5 117.1(4) . . ? C8 C7 C6 121.5(5) . . ? C7 C8 C9 121.5(5) . . ? C8 C9 C10 120.6(5) . . ? C5 C10 C11 119.8(4) . . ? C9 C10 C5 119.4(4) . . ? C9 C10 C11 120.8(4) . . ? C12 C11 C10 119.4(4) . . ? C20 C11 C10 122.5(5) . . ? C20 C11 C12 118.1(5) . . ? C11 C12 C13 121.3(4) . . ? C11 C12 C17 120.1(4) . . ? C17 C12 C13 118.6(5) . . ? C12 C13 C4 118.6(4) . . ? C14 C13 C4 122.3(4) . . ? C14 C13 C12 119.1(4) . . ? C13 C14 C15 120.9(5) . . ? C16 C15 C14 120.6(5) . . ? C15 C16 C17 121.7(5) . . ? C16 C17 C12 119.0(5) . . ? C18 C17 C12 118.5(5) . . ? C18 C17 C16 122.5(5) . . ? C19 C18 C17 121.0(5) . . ? C18 C19 C20 119.9(5) . . ? C11 C20 C19 122.2(6) . . ? N1 C21 C1 113.4(4) . . ? N1 C21 C22 117.1(4) . . ? C22 C21 C1 129.5(5) . . ? C23 C22 C21 121.8(5) . . ? C22 C23 C26 120.4(5) . . ? C24 C23 C22 118.5(4) . . ? C24 C23 C26 121.1(5) . . ? C25 C24 C23 119.5(5) . . ? N1 C25 C24 121.4(5) . . ? O1 C28 C27 113.9(4) . . ? O1 C28 C29 127.1(4) . . ? C29 C28 C27 119.0(5) . . ? C28 C29 C30 128.3(5) . . ? O2 C30 C29 125.4(5) . . ? O2 C30 C31 116.1(4) . . ? C29 C30 C31 118.5(5) . . ? loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag Pt1 I1 2.7920(5) . ? Pt1 O1 2.024(3) . ? Pt1 O2 2.122(3) . ? Pt1 N1 1.994(4) . ? Pt1 C2 1.983(4) . ? Pt1 C45 2.056(6) . ? O1 C28 1.282(6) . ? O2 C30 1.257(6) . ? N1 C21 1.369(6) . ? N1 C25 1.346(6) . ? C1 C2 1.387(6) . ? C1 C6 1.436(6) . ? C1 C21 1.472(6) . ? C2 C3 1.400(6) . ? C3 C4 1.384(6) . ? C4 C5 1.427(7) . ? C4 C13 1.473(6) . ? C5 C6 1.449(6) . ? C5 C10 1.417(7) . ? C6 C7 1.409(7) . ? C7 C8 1.357(7) . ? C8 C9 1.381(7) . ? C9 C10 1.381(7) . ? C10 C11 1.478(6) . ? C11 C12 1.417(7) . ? C11 C20 1.374(7) . ? C12 C13 1.437(7) . ? C12 C17 1.436(6) . ? C13 C14 1.382(7) . ? C14 C15 1.411(7) . ? C15 C16 1.341(8) . ? C16 C17 1.405(8) . ? C17 C18 1.403(8) . ? C18 C19 1.361(8) . ? C19 C20 1.407(8) . ? C21 C22 1.394(7) . ? C22 C23 1.383(7) . ? C23 C24 1.372(8) . ? C23 C26 1.510(7) . ? C24 C25 1.372(7) . ? C27 C28 1.502(6) . ? C28 C29 1.384(7) . ? C29 C30 1.403(7) . ? C30 C31 1.500(7) . ?