#------------------------------------------------------------------------------ #$Date: 2020-11-06 14:22:04 +0200 (Fri, 06 Nov 2020) $ #$Revision: 258860 $ #$URL: file:///home/coder/svn-repositories/cod/cif/7/70/52/7705298.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_7705298 loop_ _publ_author_name 'Exp\'osito, J Emilio' 'Aull\'on, Gabriel' 'Bardaj\'i, Manuel' 'Miguel, Jes\'us A' 'Espinet, Pablo' _publ_section_title ; Fluorescent perylenylpyridine complexes: an experimental and theoretical study. ; _journal_issue 38 _journal_name_full 'Dalton transactions (Cambridge, England : 2003)' _journal_page_first 13326 _journal_page_last 13338 _journal_paper_doi 10.1039/d0dt02494e _journal_volume 49 _journal_year 2020 _chemical_formula_moiety 'C31 H23 N O2 Pt' _chemical_formula_sum 'C31 H23 N O2 Pt' _chemical_formula_weight 636.59 _space_group_crystal_system orthorhombic _space_group_IT_number 61 _space_group_name_Hall '-P 2ac 2ab' _space_group_name_H-M_alt 'P b c a' _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 90 _cell_angle_beta 90 _cell_angle_gamma 90 _cell_formula_units_Z 8 _cell_length_a 7.8450(2) _cell_length_b 19.7471(6) _cell_length_c 29.7999(10) _cell_measurement_reflns_used 5988 _cell_measurement_temperature 293 _cell_measurement_theta_max 29.4836 _cell_measurement_theta_min 2.0462 _cell_volume 4616.5(2) _computing_cell_refinement ; CrysAlisPro, Oxford Diffraction Ltd., Version 1.171.34.44 (release 25-10-2010 CrysAlis171 .NET) (compiled Oct 25 2010,18:11:34) ; _computing_data_collection ; CrysAlisPro, Oxford Diffraction Ltd., Version 1.171.34.44 (release 25-10-2010 CrysAlis171 .NET) (compiled Oct 25 2010,18:11:34) ; _computing_data_reduction ; CrysAlisPro, Oxford Diffraction Ltd., Version 1.171.34.44 (release 25-10-2010 CrysAlis171 .NET) (compiled Oct 25 2010,18:11:34) ; _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_area_resol_mean 10.4757 _diffrn_measured_fraction_theta_full 1.000 _diffrn_measured_fraction_theta_max 0.875 _diffrn_measurement_details ; #__ type_ start__ end____ width___ exp.time_ 1 omega 2.00 102.00 1.0000 88.1700 omega____ theta____ kappa____ phi______ frames - 12.4346 0.0000 60.0000 100 #__ type_ start__ end____ width___ exp.time_ 2 omega -75.00 -20.00 1.0000 88.1700 omega____ theta____ kappa____ phi______ frames - 12.4346 0.0000 60.0000 55 ; _diffrn_measurement_device_type 'SuperNova, Dual, Cu at zero, Atlas' _diffrn_measurement_method '\w scans' _diffrn_orient_matrix_UB_11 -0.0697561000 _diffrn_orient_matrix_UB_12 -0.0056582000 _diffrn_orient_matrix_UB_13 0.0146749000 _diffrn_orient_matrix_UB_21 0.0141918000 _diffrn_orient_matrix_UB_22 0.0320024000 _diffrn_orient_matrix_UB_23 0.0101462000 _diffrn_orient_matrix_UB_31 -0.0557526000 _diffrn_orient_matrix_UB_32 0.0152497000 _diffrn_orient_matrix_UB_33 -0.0157759000 _diffrn_radiation_monochromator mirror _diffrn_radiation_type MoK\a _diffrn_radiation_wavelength 0.71073 _diffrn_reflns_av_R_equivalents 0.0291 _diffrn_reflns_av_unetI/netI 0.0343 _diffrn_reflns_Laue_measured_fraction_full 1.000 _diffrn_reflns_Laue_measured_fraction_max 0.875 _diffrn_reflns_limit_h_max 10 _diffrn_reflns_limit_h_min -8 _diffrn_reflns_limit_k_max 26 _diffrn_reflns_limit_k_min -17 _diffrn_reflns_limit_l_max 40 _diffrn_reflns_limit_l_min -40 _diffrn_reflns_number 17667 _diffrn_reflns_point_group_measured_fraction_full 1.000 _diffrn_reflns_point_group_measured_fraction_max 0.875 _diffrn_reflns_theta_full 25.242 _diffrn_reflns_theta_max 29.548 _diffrn_reflns_theta_min 2.063 _diffrn_source 'SuperNova (Mo) X-ray Source' _exptl_absorpt_coefficient_mu 6.109 _exptl_absorpt_correction_T_max 0.882 _exptl_absorpt_correction_T_min 0.624 _exptl_absorpt_correction_type analytical _exptl_absorpt_process_details ; CrysAlisPro, Oxford Diffraction Ltd., Version 1.171.34.44 (release 25-10-2010 CrysAlis171 .NET) (compiled Oct 25 2010,18:11:34) Analytical numeric absorption correction using a multifaceted crystal model based on expressions derived by R.C. Clark & J.S. Reid. (Clark, R. C. & Reid, J. S. (1995). Acta Cryst. A51, 887-897) ; _exptl_crystal_colour red _exptl_crystal_colour_primary red _exptl_crystal_density_diffrn 1.832 _exptl_crystal_description block _exptl_crystal_F_000 2480 _exptl_crystal_size_max 0.3654 _exptl_crystal_size_mid 0.1218 _exptl_crystal_size_min 0.0403 _refine_diff_density_max 0.552 _refine_diff_density_min -0.824 _refine_diff_density_rms 0.091 _refine_ls_extinction_method none _refine_ls_goodness_of_fit_ref 1.069 _refine_ls_hydrogen_treatment constr _refine_ls_matrix_type full _refine_ls_number_parameters 319 _refine_ls_number_reflns 5650 _refine_ls_number_restraints 0 _refine_ls_restrained_S_all 1.069 _refine_ls_R_factor_all 0.0574 _refine_ls_R_factor_gt 0.0325 _refine_ls_shift/su_max 0.001 _refine_ls_shift/su_mean 0.000 _refine_ls_structure_factor_coef Fsqd _refine_ls_weighting_details 'w=1/[\s^2^(Fo^2^)+(0.0165P)^2^+2.4096P] where P=(Fo^2^+2Fc^2^)/3' _refine_ls_weighting_scheme calc _refine_ls_wR_factor_gt 0.0530 _refine_ls_wR_factor_ref 0.0596 _reflns_Friedel_coverage 0.000 _reflns_number_gt 4078 _reflns_number_total 5650 _reflns_threshold_expression 'I > 2\s(I)' _cod_data_source_file d0dt02494e2.cif _cod_data_source_block 9 _cod_depositor_comments 'Adding full bibliography for 7705296--7705301.cif.' _cod_database_code 7705298 _shelx_shelxl_version_number 2018/3 _chemical_oxdiff_formula 'C31 H23 N O2 Pt' _chemical_oxdiff_usercomment 'diclorom hexa' _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 99.89 _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) ; _shelx_res_file ; TITL je239_a.res in Pbca je239.res created by SHELXL-2018/3 at 17:19:19 on 08-Jul-2020 REM Old TITL JE239 in Pbca REM SHELXT solution in Pbca REM R1 0.120, Rweak 0.002, Alpha 0.086, Orientation as input REM Formula found by SHELXT: C30 N3 O2 Pt CELL 0.71073 7.845 19.7471 29.7999 90 90 90 ZERR 8 0.0002 0.0006 0.001 0 0 0 LATT 1 SYMM 0.5-X,-Y,0.5+Z SYMM -X,0.5+Y,0.5-Z SYMM 0.5+X,0.5-Y,-Z SFAC C H N O Pt UNIT 248 184 8 16 8 L.S. 20 PLAN 10 TEMP 19.85 BOND $H list 4 fmap 2 acta REM REM REM WGHT 0.016500 2.409600 FVAR 0.13726 PT1 5 0.552655 0.494774 0.659047 11.00000 0.04392 0.02600 = 0.05107 -0.00402 -0.00195 0.00106 O1 4 0.603812 0.485058 0.593441 11.00000 0.06120 0.02940 = 0.05038 -0.00290 0.00347 0.00458 O2 4 0.607094 0.392502 0.670077 11.00000 0.05967 0.02761 = 0.05309 -0.00038 0.00345 0.00633 N1 3 0.501429 0.514947 0.722744 11.00000 0.04314 0.03172 = 0.04986 -0.00434 -0.00555 0.00084 C1 1 0.443011 0.623084 0.692973 11.00000 0.03961 0.03048 = 0.04137 -0.00493 -0.00409 -0.00134 C2 1 0.493649 0.590981 0.653521 11.00000 0.03968 0.02771 = 0.05194 -0.00405 -0.00913 0.00360 C3 1 0.499643 0.628029 0.613332 11.00000 0.04800 0.02955 = 0.04594 -0.00963 -0.00348 0.00338 AFIX 43 H3 2 0.533104 0.606021 0.587185 11.00000 -1.20000 AFIX 0 C4 1 0.457842 0.695778 0.611127 11.00000 0.03141 0.03170 = 0.04748 -0.00805 -0.00445 -0.00086 C5 1 0.391529 0.728312 0.650293 11.00000 0.02982 0.03028 = 0.04051 -0.00624 -0.00530 -0.00046 C6 1 0.377601 0.691172 0.691484 11.00000 0.03474 0.03261 = 0.04229 -0.00839 -0.00566 -0.00091 C7 1 0.293692 0.722468 0.727702 11.00000 0.04680 0.03814 = 0.04318 -0.00273 -0.00279 0.00217 AFIX 43 H7 2 0.274227 0.698039 0.753887 11.00000 -1.20000 AFIX 0 C8 1 0.240473 0.788109 0.724978 11.00000 0.05101 0.04616 = 0.04782 -0.01196 -0.00009 0.01077 AFIX 43 H8 2 0.187605 0.807970 0.749616 11.00000 -1.20000 AFIX 0 C9 1 0.263653 0.825779 0.686210 11.00000 0.04575 0.03218 = 0.05326 -0.00797 -0.00432 0.00664 AFIX 43 H9 2 0.230500 0.870987 0.685651 11.00000 -1.20000 AFIX 0 C10 1 0.335049 0.797177 0.648549 11.00000 0.03130 0.03154 = 0.04402 -0.00502 -0.00745 0.00194 C11 1 0.350010 0.835318 0.606164 11.00000 0.03461 0.03307 = 0.04424 -0.00182 -0.00908 0.00110 C12 1 0.421403 0.803586 0.567790 11.00000 0.02995 0.03447 = 0.04887 -0.00525 -0.00513 -0.00092 C13 1 0.477030 0.734773 0.569345 11.00000 0.03124 0.03610 = 0.04332 -0.00291 -0.00073 -0.00173 C14 1 0.549117 0.707419 0.531184 11.00000 0.04457 0.04452 = 0.05839 -0.00232 0.00411 0.00861 AFIX 43 H14 2 0.591773 0.663511 0.532306 11.00000 -1.20000 AFIX 0 C15 1 0.560211 0.743369 0.490976 11.00000 0.05374 0.05614 = 0.05017 -0.00735 0.01339 0.00489 AFIX 43 H15 2 0.605892 0.722678 0.465651 11.00000 -1.20000 AFIX 0 C16 1 0.504883 0.808145 0.488635 11.00000 0.05326 0.06056 = 0.04358 0.00531 0.00564 0.00016 AFIX 43 H16 2 0.512362 0.831703 0.461684 11.00000 -1.20000 AFIX 0 C17 1 0.435720 0.840239 0.526955 11.00000 0.03913 0.04099 = 0.05117 0.00226 -0.00219 0.00100 C18 1 0.375925 0.907824 0.525249 11.00000 0.05938 0.04465 = 0.05751 0.00563 0.00003 0.00944 AFIX 43 H18 2 0.385267 0.932330 0.498712 11.00000 -1.20000 AFIX 0 C19 1 0.305424 0.937080 0.561785 11.00000 0.06708 0.03657 = 0.06409 0.00289 -0.00598 0.01225 AFIX 43 H19 2 0.265522 0.981356 0.560126 11.00000 -1.20000 AFIX 0 C20 1 0.292113 0.901255 0.602005 11.00000 0.04986 0.04032 = 0.05154 -0.00556 -0.00710 0.01044 AFIX 43 H20 2 0.242906 0.922292 0.626740 11.00000 -1.20000 AFIX 0 C21 1 0.463825 0.581288 0.733373 11.00000 0.03840 0.03210 = 0.05126 -0.00531 -0.00468 -0.00264 C22 1 0.462820 0.599721 0.778091 11.00000 0.04422 0.04060 = 0.04905 -0.00638 -0.00366 0.00250 AFIX 43 H22 2 0.447550 0.645152 0.785264 11.00000 -1.20000 AFIX 0 C23 1 0.483382 0.553945 0.812564 11.00000 0.04525 0.04840 = 0.05025 -0.00159 -0.00373 0.00206 C24 1 0.504795 0.486444 0.800316 11.00000 0.06470 0.04883 = 0.05127 0.00982 -0.00262 0.00648 AFIX 43 H24 2 0.510386 0.453044 0.822269 11.00000 -1.20000 AFIX 0 C25 1 0.517609 0.469269 0.755967 11.00000 0.05632 0.03383 = 0.05820 0.00415 -0.00245 0.00288 AFIX 43 H25 2 0.538300 0.424287 0.748499 11.00000 -1.20000 AFIX 0 C26 1 0.487242 0.576661 0.860574 11.00000 0.07926 0.06328 = 0.04884 0.00157 -0.00898 0.00589 AFIX 137 H26A 2 0.602951 0.585147 0.869422 11.00000 -1.50000 H26B 2 0.439564 0.541943 0.879309 11.00000 -1.50000 H26C 2 0.421681 0.617433 0.863724 11.00000 -1.50000 AFIX 0 C27 1 0.665910 0.436079 0.524309 11.00000 0.08033 0.04170 = 0.05072 0.00303 0.00412 0.01086 AFIX 137 H27A 2 0.562227 0.452493 0.511101 11.00000 -1.50000 H27B 2 0.693729 0.392725 0.511707 11.00000 -1.50000 H27C 2 0.756589 0.467427 0.518276 11.00000 -1.50000 AFIX 0 C28 1 0.642820 0.429206 0.573939 11.00000 0.04394 0.03406 = 0.05379 -0.00137 0.00492 0.00307 C29 1 0.660321 0.366203 0.593819 11.00000 0.05063 0.02995 = 0.05469 -0.00207 0.00574 0.00800 AFIX 43 H29 2 0.687640 0.330459 0.574813 11.00000 -1.20000 AFIX 0 C30 1 0.641607 0.350417 0.639026 11.00000 0.03899 0.03288 = 0.06027 -0.00136 0.00376 0.00913 C31 1 0.657349 0.278103 0.653279 11.00000 0.07622 0.03618 = 0.06349 0.00541 0.01547 0.01821 AFIX 137 H31A 2 0.762797 0.271860 0.669093 11.00000 -1.50000 H31B 2 0.655505 0.249405 0.627281 11.00000 -1.50000 H31C 2 0.563854 0.266606 0.672617 11.00000 -1.50000 AFIX 0 HKLF 4 REM je239_a.res in Pbca REM wR2 = 0.0596, GooF = S = 1.069, Restrained GooF = 1.069 for all data REM R1 = 0.0325 for 4078 Fo > 4sig(Fo) and 0.0574 for all 5650 data REM 319 parameters refined using 0 restraints END WGHT 0.0165 2.4093 REM Highest difference peak 0.552, deepest hole -0.824, 1-sigma level 0.091 Q1 1 0.6053 0.5099 0.6364 11.00000 0.05 0.55 Q2 1 0.4180 0.4926 0.6509 11.00000 0.05 0.51 Q3 1 0.6351 0.5233 0.6523 11.00000 0.05 0.48 Q4 1 0.6667 0.2721 0.6811 11.00000 0.05 0.45 Q5 1 0.3561 0.8597 0.6138 11.00000 0.05 0.40 Q6 1 0.6955 0.4834 0.6525 11.00000 0.05 0.38 Q7 1 0.3061 0.8145 0.6200 11.00000 0.05 0.37 Q8 1 0.5728 0.4259 0.6583 11.00000 0.05 0.37 Q9 1 0.3973 0.8716 0.5215 11.00000 0.05 0.37 Q10 1 0.3826 0.8121 0.6301 11.00000 0.05 0.35 ; _shelx_res_checksum 47424 _olex2_submission_special_instructions 'No special instructions were received' loop_ _space_group_symop_operation_xyz 'x, y, z' '-x+1/2, -y, z+1/2' '-x, y+1/2, -z+1/2' 'x+1/2, -y+1/2, -z' '-x, -y, -z' 'x-1/2, y, -z-1/2' 'x, -y-1/2, z-1/2' '-x-1/2, y-1/2, 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 0.55265(2) 0.49477(2) 0.65905(2) 0.04033(6) Uani 1 1 d . . . . . O1 O 0.6038(4) 0.48506(12) 0.59344(9) 0.0470(7) Uani 1 1 d . . . . . O2 O 0.6071(4) 0.39250(12) 0.67008(9) 0.0468(7) Uani 1 1 d . . . . . N1 N 0.5014(4) 0.51495(15) 0.72274(11) 0.0416(8) Uani 1 1 d . . . . . C1 C 0.4430(5) 0.62308(17) 0.69297(12) 0.0372(9) Uani 1 1 d . . . . . C2 C 0.4936(5) 0.59098(18) 0.65352(13) 0.0398(9) Uani 1 1 d . . . . . C3 C 0.4996(5) 0.62803(17) 0.61333(13) 0.0412(9) Uani 1 1 d . . . . . H3 H 0.533104 0.606021 0.587185 0.049 Uiso 1 1 calc R . . . . C4 C 0.4578(4) 0.69578(17) 0.61113(12) 0.0369(9) Uani 1 1 d . . . . . C5 C 0.3915(4) 0.72831(17) 0.65029(12) 0.0335(8) Uani 1 1 d . . . . . C6 C 0.3776(5) 0.69117(17) 0.69148(12) 0.0365(9) Uani 1 1 d . . . . . C7 C 0.2937(5) 0.72247(18) 0.72770(13) 0.0427(9) Uani 1 1 d . . . . . H7 H 0.274227 0.698039 0.753887 0.051 Uiso 1 1 calc R . . . . C8 C 0.2405(5) 0.7881(2) 0.72498(13) 0.0483(10) Uani 1 1 d . . . . . H8 H 0.187605 0.807970 0.749616 0.058 Uiso 1 1 calc R . . . . C9 C 0.2637(5) 0.82578(18) 0.68621(13) 0.0437(10) Uani 1 1 d . . . . . H9 H 0.230500 0.870987 0.685651 0.052 Uiso 1 1 calc R . . . . C10 C 0.3350(5) 0.79718(17) 0.64855(12) 0.0356(9) Uani 1 1 d . . . . . C11 C 0.3500(5) 0.83532(17) 0.60616(12) 0.0373(9) Uani 1 1 d . . . . . C12 C 0.4214(4) 0.80359(18) 0.56779(13) 0.0378(9) Uani 1 1 d . . . . . C13 C 0.4770(5) 0.73477(18) 0.56935(12) 0.0369(9) Uani 1 1 d . . . . . C14 C 0.5491(5) 0.7074(2) 0.53118(14) 0.0492(10) Uani 1 1 d . . . . . H14 H 0.591773 0.663511 0.532306 0.059 Uiso 1 1 calc R . . . . C15 C 0.5602(5) 0.7434(2) 0.49098(14) 0.0533(11) Uani 1 1 d . . . . . H15 H 0.605892 0.722678 0.465651 0.064 Uiso 1 1 calc R . . . . C16 C 0.5049(5) 0.8081(2) 0.48864(13) 0.0525(11) Uani 1 1 d . . . . . H16 H 0.512362 0.831703 0.461684 0.063 Uiso 1 1 calc R . . . . C17 C 0.4357(5) 0.84024(19) 0.52696(14) 0.0438(9) Uani 1 1 d . . . . . C18 C 0.3759(5) 0.9078(2) 0.52525(15) 0.0538(11) Uani 1 1 d . . . . . H18 H 0.385267 0.932330 0.498712 0.065 Uiso 1 1 calc R . . . . C19 C 0.3054(6) 0.9371(2) 0.56178(14) 0.0559(12) Uani 1 1 d . . . . . H19 H 0.265522 0.981356 0.560126 0.067 Uiso 1 1 calc R . . . . C20 C 0.2921(5) 0.90125(19) 0.60200(14) 0.0472(10) Uani 1 1 d . . . . . H20 H 0.242906 0.922292 0.626740 0.057 Uiso 1 1 calc R . . . . C21 C 0.4638(5) 0.58129(18) 0.73337(13) 0.0406(9) Uani 1 1 d . . . . . C22 C 0.4628(5) 0.59972(19) 0.77809(13) 0.0446(10) Uani 1 1 d . . . . . H22 H 0.447550 0.645152 0.785264 0.054 Uiso 1 1 calc R . . . . C23 C 0.4834(5) 0.5539(2) 0.81256(14) 0.0480(10) Uani 1 1 d . . . . . C24 C 0.5048(6) 0.4864(2) 0.80032(14) 0.0549(11) Uani 1 1 d . . . . . H24 H 0.510386 0.453044 0.822269 0.066 Uiso 1 1 calc R . . . . C25 C 0.5176(5) 0.4693(2) 0.75597(14) 0.0495(10) Uani 1 1 d . . . . . H25 H 0.538300 0.424287 0.748499 0.059 Uiso 1 1 calc R . . . . C26 C 0.4872(6) 0.5767(2) 0.86057(14) 0.0638(13) Uani 1 1 d . . . . . H26A H 0.602951 0.585147 0.869422 0.096 Uiso 1 1 calc GR . . . . H26B H 0.439564 0.541943 0.879309 0.096 Uiso 1 1 calc GR . . . . H26C H 0.421681 0.617433 0.863724 0.096 Uiso 1 1 calc GR . . . . C27 C 0.6659(6) 0.4361(2) 0.52431(13) 0.0576(12) Uani 1 1 d . . . . . H27A H 0.562227 0.452493 0.511101 0.086 Uiso 1 1 calc GR . . . . H27B H 0.693729 0.392725 0.511707 0.086 Uiso 1 1 calc GR . . . . H27C H 0.756589 0.467427 0.518276 0.086 Uiso 1 1 calc GR . . . . C28 C 0.6428(5) 0.42921(19) 0.57394(13) 0.0439(10) Uani 1 1 d . . . . . C29 C 0.6603(5) 0.36620(18) 0.59382(13) 0.0451(10) Uani 1 1 d . . . . . H29 H 0.687640 0.330459 0.574813 0.054 Uiso 1 1 calc R . . . . C30 C 0.6416(5) 0.35042(18) 0.63903(14) 0.0440(10) Uani 1 1 d . . . . . C31 C 0.6573(6) 0.27810(19) 0.65328(14) 0.0586(12) Uani 1 1 d . . . . . H31A H 0.762797 0.271860 0.669093 0.088 Uiso 1 1 calc GR . . . . H31B H 0.655505 0.249405 0.627281 0.088 Uiso 1 1 calc GR . . . . H31C H 0.563854 0.266606 0.672617 0.088 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 0.04392(10) 0.02600(8) 0.05107(10) -0.00402(7) -0.00195(8) 0.00106(6) O1 0.0612(18) 0.0294(14) 0.0504(16) -0.0029(12) 0.0035(14) 0.0046(13) O2 0.0597(18) 0.0276(13) 0.0531(17) -0.0004(12) 0.0034(15) 0.0063(13) N1 0.0431(18) 0.0317(16) 0.0499(19) -0.0043(14) -0.0055(16) 0.0008(14) C1 0.040(2) 0.0305(19) 0.041(2) -0.0049(15) -0.0041(19) -0.0013(17) C2 0.040(2) 0.0277(19) 0.052(2) -0.0041(17) -0.009(2) 0.0036(16) C3 0.048(2) 0.0295(19) 0.046(2) -0.0096(17) -0.003(2) 0.0034(17) C4 0.031(2) 0.0317(19) 0.047(2) -0.0081(16) -0.0044(19) -0.0009(16) C5 0.0298(19) 0.0303(19) 0.041(2) -0.0062(15) -0.0053(17) -0.0005(15) C6 0.035(2) 0.033(2) 0.042(2) -0.0084(16) -0.0057(19) -0.0009(17) C7 0.047(2) 0.038(2) 0.043(2) -0.0027(18) -0.003(2) 0.0022(18) C8 0.051(3) 0.046(2) 0.048(2) -0.012(2) 0.000(2) 0.011(2) C9 0.046(2) 0.032(2) 0.053(2) -0.0080(18) -0.004(2) 0.0066(18) C10 0.031(2) 0.0315(19) 0.044(2) -0.0050(15) -0.0074(18) 0.0019(16) C11 0.035(2) 0.0331(19) 0.044(2) -0.0018(16) -0.0091(19) 0.0011(17) C12 0.030(2) 0.034(2) 0.049(2) -0.0052(17) -0.0051(19) -0.0009(16) C13 0.031(2) 0.036(2) 0.043(2) -0.0029(16) -0.0007(18) -0.0017(16) C14 0.045(2) 0.045(2) 0.058(3) -0.002(2) 0.004(2) 0.009(2) C15 0.054(3) 0.056(3) 0.050(3) -0.007(2) 0.013(2) 0.005(2) C16 0.053(3) 0.061(3) 0.044(3) 0.005(2) 0.006(2) 0.000(2) C17 0.039(2) 0.041(2) 0.051(2) 0.0023(18) -0.002(2) 0.0010(18) C18 0.059(3) 0.045(2) 0.058(3) 0.006(2) 0.000(2) 0.009(2) C19 0.067(3) 0.037(2) 0.064(3) 0.003(2) -0.006(3) 0.012(2) C20 0.050(3) 0.040(2) 0.052(2) -0.0056(19) -0.007(2) 0.0104(19) C21 0.038(2) 0.0321(19) 0.051(2) -0.0053(17) -0.005(2) -0.0026(17) C22 0.044(2) 0.041(2) 0.049(2) -0.0064(18) -0.004(2) 0.0025(19) C23 0.045(2) 0.048(2) 0.050(3) -0.002(2) -0.004(2) 0.002(2) C24 0.065(3) 0.049(3) 0.051(3) 0.010(2) -0.003(2) 0.006(2) C25 0.056(3) 0.034(2) 0.058(3) 0.0041(19) -0.002(2) 0.0029(19) C26 0.079(3) 0.063(3) 0.049(3) 0.002(2) -0.009(3) 0.006(3) C27 0.080(3) 0.042(2) 0.051(3) 0.0030(19) 0.004(3) 0.011(2) C28 0.044(2) 0.034(2) 0.054(2) -0.0014(18) 0.005(2) 0.0031(18) C29 0.051(3) 0.030(2) 0.055(3) -0.0021(17) 0.006(2) 0.0080(18) C30 0.039(2) 0.033(2) 0.060(3) -0.0014(19) 0.004(2) 0.0091(18) C31 0.076(3) 0.036(2) 0.063(3) 0.0054(19) 0.015(3) 0.018(2) 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' 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 0 -2 42 0.0181 0.0083 -2.0418 42.0011 0.6273 0.3608 -0.6942 0 2 -42 0.0222 -0.0083 2.0418 -42.0011 -0.6273 -0.3608 0.6942 -10 14 2 0.1642 -10.0108 13.9887 2.0465 0.6492 0.3263 0.7392 10 -14 -3 0.1110 10.0106 -13.9877 -3.0466 -0.6638 -0.3364 -0.7234 0 -23 24 0.0266 0.0101 -23.0428 23.9828 0.4816 -0.4941 -0.7303 1 23 -24 0.0297 0.9906 23.0449 -23.9863 -0.5514 0.5083 0.6746 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 O2 91.15(10) . . ? N1 Pt1 O1 173.88(11) . . ? N1 Pt1 O2 94.88(11) . . ? C2 Pt1 O1 93.33(13) . . ? C2 Pt1 O2 175.42(13) . . ? C2 Pt1 N1 80.67(14) . . ? C28 O1 Pt1 124.8(2) . . ? C30 O2 Pt1 124.1(2) . . ? C21 N1 Pt1 117.0(3) . . ? C25 N1 Pt1 123.5(3) . . ? C25 N1 C21 119.2(3) . . ? C2 C1 C6 120.0(3) . . ? C2 C1 C21 113.8(3) . . ? C6 C1 C21 126.1(3) . . ? C1 C2 Pt1 115.9(3) . . ? C1 C2 C3 119.5(3) . . ? C3 C2 Pt1 124.6(3) . . ? C2 C3 H3 118.7 . . ? C4 C3 C2 122.6(4) . . ? C4 C3 H3 118.7 . . ? C3 C4 C5 118.9(3) . . ? C3 C4 C13 121.6(3) . . ? C5 C4 C13 119.5(3) . . ? C4 C5 C6 119.8(3) . . ? C4 C5 C10 120.7(3) . . ? C10 C5 C6 119.6(3) . . ? C5 C6 C1 118.5(3) . . ? C7 C6 C1 123.6(3) . . ? C7 C6 C5 117.9(3) . . ? C6 C7 H7 119.5 . . ? C8 C7 C6 121.0(4) . . ? C8 C7 H7 119.5 . . ? C7 C8 H8 119.4 . . ? C7 C8 C9 121.3(4) . . ? C9 C8 H8 119.4 . . ? C8 C9 H9 119.6 . . ? C10 C9 C8 120.9(3) . . ? C10 C9 H9 119.6 . . ? C5 C10 C11 119.4(3) . . ? C9 C10 C5 119.1(3) . . ? C9 C10 C11 121.4(3) . . ? C12 C11 C10 119.7(3) . . ? C20 C11 C10 122.0(3) . . ? C20 C11 C12 118.2(3) . . ? C11 C12 C13 121.0(3) . . ? C11 C12 C17 119.8(3) . . ? C17 C12 C13 119.2(3) . . ? C12 C13 C4 119.6(3) . . ? C14 C13 C4 122.3(3) . . ? C14 C13 C12 118.1(3) . . ? C13 C14 H14 118.9 . . ? C13 C14 C15 122.3(4) . . ? C15 C14 H14 118.9 . . ? C14 C15 H15 119.8 . . ? C16 C15 C14 120.4(4) . . ? C16 C15 H15 119.8 . . ? C15 C16 H16 119.8 . . ? C15 C16 C17 120.4(4) . . ? C17 C16 H16 119.8 . . ? C16 C17 C12 119.6(4) . . ? C16 C17 C18 121.4(4) . . ? C18 C17 C12 119.0(4) . . ? C17 C18 H18 119.7 . . ? C19 C18 C17 120.7(4) . . ? C19 C18 H18 119.7 . . ? C18 C19 H19 119.8 . . ? C18 C19 C20 120.4(4) . . ? C20 C19 H19 119.8 . . ? C11 C20 C19 121.9(4) . . ? C11 C20 H20 119.0 . . ? C19 C20 H20 119.0 . . ? N1 C21 C1 111.7(3) . . ? N1 C21 C22 118.2(3) . . ? C22 C21 C1 129.9(3) . . ? C21 C22 H22 118.5 . . ? C23 C22 C21 123.1(4) . . ? C23 C22 H22 118.5 . . ? C22 C23 C24 116.5(4) . . ? C22 C23 C26 121.2(4) . . ? C24 C23 C26 122.3(4) . . ? C23 C24 H24 120.0 . . ? C25 C24 C23 120.0(4) . . ? C25 C24 H24 120.0 . . ? N1 C25 C24 122.5(4) . . ? N1 C25 H25 118.7 . . ? C24 C25 H25 118.7 . . ? C23 C26 H26A 109.5 . . ? C23 C26 H26B 109.5 . . ? C23 C26 H26C 109.5 . . ? H26A C26 H26B 109.5 . . ? H26A C26 H26C 109.5 . . ? H26B C26 H26C 109.5 . . ? H27A C27 H27B 109.5 . . ? H27A C27 H27C 109.5 . . ? H27B C27 H27C 109.5 . . ? C28 C27 H27A 109.5 . . ? C28 C27 H27B 109.5 . . ? C28 C27 H27C 109.5 . . ? O1 C28 C27 113.5(3) . . ? O1 C28 C29 127.0(4) . . ? C29 C28 C27 119.5(3) . . ? C28 C29 H29 116.4 . . ? C28 C29 C30 127.3(4) . . ? C30 C29 H29 116.4 . . ? O2 C30 C29 125.5(3) . . ? O2 C30 C31 115.8(4) . . ? C29 C30 C31 118.7(3) . . ? C30 C31 H31A 109.5 . . ? C30 C31 H31B 109.5 . . ? C30 C31 H31C 109.5 . . ? H31A C31 H31B 109.5 . . ? H31A C31 H31C 109.5 . . ? H31B C31 H31C 109.5 . . ? 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 O1 2.005(3) . ? Pt1 O2 2.090(2) . ? Pt1 N1 1.981(3) . ? Pt1 C2 1.962(4) . ? O1 C28 1.284(4) . ? O2 C30 1.273(4) . ? N1 C21 1.380(4) . ? N1 C25 1.345(5) . ? C1 C2 1.394(5) . ? C1 C6 1.440(5) . ? C1 C21 1.469(5) . ? C2 C3 1.404(5) . ? C3 H3 0.9300 . ? C3 C4 1.379(5) . ? C4 C5 1.430(5) . ? C4 C13 1.472(5) . ? C5 C6 1.434(5) . ? C5 C10 1.431(5) . ? C6 C7 1.407(5) . ? C7 H7 0.9300 . ? C7 C8 1.364(5) . ? C8 H8 0.9300 . ? C8 C9 1.386(5) . ? C9 H9 0.9300 . ? C9 C10 1.376(5) . ? C10 C11 1.475(5) . ? C11 C12 1.419(5) . ? C11 C20 1.385(5) . ? C12 C13 1.428(5) . ? C12 C17 1.420(5) . ? C13 C14 1.380(5) . ? C14 H14 0.9300 . ? C14 C15 1.395(5) . ? C15 H15 0.9300 . ? C15 C16 1.353(6) . ? C16 H16 0.9300 . ? C16 C17 1.414(6) . ? C17 C18 1.416(5) . ? C18 H18 0.9300 . ? C18 C19 1.351(5) . ? C19 H19 0.9300 . ? C19 C20 1.396(5) . ? C20 H20 0.9300 . ? C21 C22 1.381(5) . ? C22 H22 0.9300 . ? C22 C23 1.378(5) . ? C23 C24 1.392(5) . ? C23 C26 1.500(6) . ? C24 H24 0.9300 . ? C24 C25 1.368(6) . ? C25 H25 0.9300 . ? C26 H26A 0.9600 . ? C26 H26B 0.9600 . ? C26 H26C 0.9600 . ? C27 H27A 0.9600 . ? C27 H27B 0.9600 . ? C27 H27C 0.9600 . ? C27 C28 1.496(5) . ? C28 C29 1.385(5) . ? C29 H29 0.9300 . ? C29 C30 1.391(5) . ? C30 C31 1.495(5) . ? C31 H31A 0.9600 . ? C31 H31B 0.9600 . ? C31 H31C 0.9600 . ?