#------------------------------------------------------------------------------ #$Date: 2024-05-22 04:53:43 +0300 (Wed, 22 May 2024) $ #$Revision: 291979 $ #$URL: file:///home/coder/svn-repositories/cod/cif/2/02/31/2023135.cif $ #------------------------------------------------------------------------------ # # This file is available in the Crystallography Open Database (COD), # http://www.crystallography.net/. The original data for this entry # were provided by IUCr Journals, http://journals.iucr.org/. # # The file may be used within the scientific community so long as # proper attribution is given to the journal article from which the # data were obtained. # data_2023135 loop_ _publ_author_name 'Chi, Nguyen Thi Thanh' 'Van Thong, Pham' 'Thang, Nguyen Manh' 'Thao, Pham Ngoc' 'Van Meervelt, Luc' _publ_section_title ; Synthesis and crystal structures of three organoplatinum(II) complexes bearing natural arylolefin and quinoline derivatives ; _journal_coeditor_code PK2707 _journal_issue 6 _journal_name_full 'Acta Crystallographica Section E Crystallographic Communications' _journal_paper_doi 10.1107/S2056989024004572 _journal_volume 80 _journal_year 2024 _chemical_formula_iupac '[Pt (C15 H19 O4) (C10 H6N O2 )]' _chemical_formula_moiety 'C25 H25 N O6 Pt' _chemical_formula_sum 'C25 H25 N O6 Pt' _chemical_formula_weight 630.55 _chemical_name_systematic '[4-Methoxy-5-(2-oxo-2-propoxyethoxy)-2-(prop-2-en-1-yl)phenyl](quinoline-2-carboxylato)platinum(II)' _space_group_crystal_system monoclinic _space_group_IT_number 14 _space_group_name_Hall '-P 2yn' _space_group_name_H-M_alt 'P 1 21/n 1' _atom_sites_solution_hydrogens geom _audit_creation_method ; Olex2 1.2 (compiled 2015.09.30 svn.r3233 for OlexSys, GUI svn.r5103) ; _cell_angle_alpha 90 _cell_angle_beta 102.014(5) _cell_angle_gamma 90 _cell_formula_units_Z 4 _cell_length_a 8.2857(4) _cell_length_b 18.5001(9) _cell_length_c 14.6282(7) _cell_measurement_reflns_used 8290 _cell_measurement_temperature 100.02(10) _cell_measurement_theta_max 28.9900 _cell_measurement_theta_min 2.8450 _cell_volume 2193.19(19) _computing_cell_refinement ; CrysAlisPro (Rigaku OD, 2022) ; _computing_data_collection ; CrysAlisPro (Rigaku OD, 2022) ; _computing_data_reduction ; CrysAlisPro (Rigaku OD, 2022) ; _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 ; ShelXS (Sheldrick, 2008) ; _diffrn_ambient_temperature 100.02(10) _diffrn_detector 'CCD plate' _diffrn_detector_area_resol_mean 15.9631 _diffrn_measured_fraction_theta_full 1.000 _diffrn_measured_fraction_theta_max 0.910 _diffrn_measurement_device 'four-circle diffractometer' _diffrn_measurement_device_type 'SuperNova, Single source at offset, Eos' _diffrn_measurement_method '\w scans' _diffrn_radiation_monochromator mirror _diffrn_radiation_probe x-ray _diffrn_radiation_type MoK\a _diffrn_radiation_wavelength 0.71073 _diffrn_reflns_av_R_equivalents 0.0569 _diffrn_reflns_av_unetI/netI 0.0486 _diffrn_reflns_limit_h_max 11 _diffrn_reflns_limit_h_min -11 _diffrn_reflns_limit_k_max 24 _diffrn_reflns_limit_k_min -25 _diffrn_reflns_limit_l_max 19 _diffrn_reflns_limit_l_min -19 _diffrn_reflns_number 23965 _diffrn_reflns_theta_full 26.000 _diffrn_reflns_theta_max 29.126 _diffrn_reflns_theta_min 2.618 _diffrn_source 'micro-focus sealed X-ray tube' _exptl_absorpt_coefficient_mu 6.441 _exptl_absorpt_correction_T_max 1.00000 _exptl_absorpt_correction_T_min 0.66867 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_process_details ; (CrysAlisPro; Rigaku OD, 2022) ; _exptl_crystal_colour orange _exptl_crystal_density_diffrn 1.910 _exptl_crystal_description block _exptl_crystal_F_000 1232 _exptl_crystal_size_max 0.4 _exptl_crystal_size_mid 0.4 _exptl_crystal_size_min 0.3 _refine_diff_density_max 2.158 _refine_diff_density_min -1.726 _refine_ls_extinction_method none _refine_ls_goodness_of_fit_ref 1.051 _refine_ls_hydrogen_treatment constr _refine_ls_matrix_type full _refine_ls_number_parameters 300 _refine_ls_number_reflns 5366 _refine_ls_number_restraints 0 _refine_ls_restrained_S_all 1.051 _refine_ls_R_factor_all 0.0415 _refine_ls_R_factor_gt 0.0334 _refine_ls_shift/su_max 0.003 _refine_ls_shift/su_mean 0.000 _refine_ls_structure_factor_coef Fsqd _refine_ls_weighting_details 'w=1/[\s^2^(Fo^2^)+(0.0204P)^2^+5.0718P] where P=(Fo^2^+2Fc^2^)/3' _refine_ls_weighting_scheme calc _refine_ls_wR_factor_gt 0.0653 _refine_ls_wR_factor_ref 0.0701 _reflns_number_gt 4652 _reflns_number_total 5366 _reflns_threshold_expression 'I > 2\s(I)' _iucr_refine_instructions_details ; chi53.res created by SHELXL-2014/7 TITL CHI53 in P21/n #14 REM reset to P21/n #14 CELL 0.71073 8.285668 18.500123 14.62815 90 102.0136 90 ZERR 4 0.000387 0.000916 0.000737 0 0.0048 0 LATT 1 SYMM 0.5-X,0.5+Y,0.5-Z SFAC C H N O Pt UNIT 100 100 4 24 4 L.S. 10 PLAN 10 BOND MORE -1 BOND $H CONF fmap 2 acta 52 REM REM REM WGHT 0.020400 5.071800 FVAR 2.71569 PT1 5 -0.055604 0.616389 0.093446 11.00000 0.01864 0.01974 = 0.01431 0.00078 0.00582 0.00199 C2 1 -0.315475 0.627442 0.069326 11.00000 0.01881 0.02393 = 0.02278 -0.00171 0.00412 0.00260 AFIX 23 H2A 2 -0.377566 0.608222 0.010791 11.00000 -1.20000 H2B 2 -0.366410 0.617992 0.122125 11.00000 -1.20000 AFIX 0 C3 1 -0.245013 0.696676 0.065606 11.00000 0.01877 0.02597 = 0.01590 0.00280 0.00241 0.00765 AFIX 13 H3 2 -0.263109 0.719386 0.003783 11.00000 -1.20000 AFIX 0 C4 1 -0.222558 0.747591 0.148027 11.00000 0.02703 0.01477 = 0.02645 -0.00263 0.00197 0.00210 AFIX 23 H4A 2 -0.328623 0.767121 0.153803 11.00000 -1.20000 H4B 2 -0.151973 0.787525 0.138539 11.00000 -1.20000 AFIX 0 C5 1 -0.145448 0.707152 0.236395 11.00000 0.01897 0.01574 = 0.01916 0.00214 0.00172 -0.00280 C6 1 -0.061858 0.644202 0.224301 11.00000 0.01665 0.01787 = 0.01554 0.00013 0.00533 -0.00118 C7 1 0.016723 0.604757 0.302690 11.00000 0.01841 0.01910 = 0.02252 0.00047 0.00765 0.00524 AFIX 43 H7 2 0.071696 0.562148 0.294666 11.00000 -1.20000 AFIX 0 C8 1 0.013417 0.628584 0.392197 11.00000 0.01952 0.02284 = 0.01586 0.00130 0.00547 -0.00036 C9 1 -0.074794 0.691566 0.404439 11.00000 0.01861 0.01619 = 0.01994 -0.00263 0.00575 -0.00330 C10 1 -0.152363 0.730853 0.326843 11.00000 0.02077 0.01484 = 0.02247 -0.00355 0.00438 0.00191 AFIX 43 H10 2 -0.209120 0.773005 0.334687 11.00000 -1.20000 AFIX 0 O11 4 -0.079191 0.708543 0.495404 11.00000 0.02989 0.01660 = 0.01640 -0.00258 0.00638 0.00457 C12 1 -0.163511 0.772926 0.510588 11.00000 0.02635 0.02293 = 0.02497 -0.00563 0.00509 0.00585 AFIX 137 H12A 2 -0.115154 0.813346 0.485046 11.00000 -1.50000 H12B 2 -0.154580 0.779997 0.576467 11.00000 -1.50000 H12C 2 -0.277742 0.768915 0.480504 11.00000 -1.50000 AFIX 0 O13 4 0.091552 0.595618 0.473937 11.00000 0.03147 0.02327 = 0.01351 0.00139 0.00432 0.01147 C14 1 0.181193 0.532094 0.465084 11.00000 0.02759 0.02074 = 0.01935 0.00232 0.00935 0.00875 AFIX 23 H14A 2 0.249904 0.539235 0.419646 11.00000 -1.20000 H14B 2 0.106147 0.492369 0.444222 11.00000 -1.20000 AFIX 0 C15 1 0.286416 0.515406 0.559173 11.00000 0.02251 0.02239 = 0.01934 0.00336 0.01137 0.00690 O16 4 0.308118 0.554138 0.625973 11.00000 0.04542 0.03639 = 0.01753 -0.00439 0.00399 0.01765 O17 4 0.356228 0.450002 0.556678 11.00000 0.03182 0.02057 = 0.02481 0.00285 0.00502 0.00709 C18 1 0.447632 0.422098 0.646400 11.00000 0.02851 0.02990 = 0.02053 0.00902 0.00622 0.00687 AFIX 23 H18A 2 0.374752 0.416070 0.689853 11.00000 -1.20000 H18B 2 0.535717 0.455001 0.673637 11.00000 -1.20000 AFIX 0 C19 1 0.517733 0.349670 0.624925 11.00000 0.03986 0.01613 = 0.03412 0.00362 0.00907 -0.00005 AFIX 23 H19A 2 0.601328 0.357122 0.588268 11.00000 -1.20000 H19B 2 0.430681 0.320184 0.588572 11.00000 -1.20000 AFIX 0 C20 1 0.593383 0.310882 0.715653 11.00000 0.03749 0.02727 = 0.03653 0.00686 0.00052 -0.00175 AFIX 137 H20A 2 0.644991 0.266960 0.701642 11.00000 -1.50000 H20B 2 0.508435 0.299720 0.749143 11.00000 -1.50000 H20C 2 0.674372 0.341536 0.753320 11.00000 -1.50000 AFIX 0 N21 3 0.007240 0.590038 -0.041622 11.00000 0.02001 0.01662 = 0.01430 0.00168 0.00673 0.00018 C22 1 -0.071730 0.604604 -0.133050 11.00000 0.03033 0.01379 = 0.01955 -0.00212 0.00661 -0.00508 C23 1 -0.240646 0.624038 -0.154301 11.00000 0.03033 0.02068 = 0.01837 -0.00336 0.00651 0.00155 AFIX 43 H23 2 -0.298078 0.628601 -0.106334 11.00000 -1.20000 AFIX 0 C24 1 -0.320816 0.636262 -0.245385 11.00000 0.03664 0.02879 = 0.01956 0.00302 -0.00218 0.00298 AFIX 43 H24 2 -0.432562 0.647700 -0.258532 11.00000 -1.20000 AFIX 0 C25 1 -0.234560 0.631554 -0.318972 11.00000 0.05048 0.01989 = 0.01735 0.00399 0.00106 0.00162 AFIX 43 H25 2 -0.288786 0.640769 -0.380169 11.00000 -1.20000 AFIX 0 C26 1 -0.071636 0.613456 -0.299851 11.00000 0.04417 0.01924 = 0.01971 -0.00248 0.00983 -0.00935 AFIX 43 H26 2 -0.014392 0.611651 -0.348156 11.00000 -1.20000 AFIX 0 C27 1 0.011140 0.597473 -0.208117 11.00000 0.03599 0.01475 = 0.01980 -0.00573 0.01289 -0.01043 C28 1 0.176978 0.571834 -0.187318 11.00000 0.03689 0.02337 = 0.02386 -0.00911 0.01890 -0.00522 AFIX 43 H28 2 0.235919 0.567485 -0.234640 11.00000 -1.20000 AFIX 0 C29 1 0.248800 0.553718 -0.097778 11.00000 0.02306 0.02113 = 0.02686 -0.00513 0.01149 -0.00510 AFIX 43 H29 2 0.354703 0.534386 -0.083951 11.00000 -1.20000 AFIX 0 C30 1 0.160442 0.564680 -0.026534 11.00000 0.02385 0.01361 = 0.02490 -0.00446 0.01008 -0.00479 C31 1 0.245595 0.548903 0.073146 11.00000 0.02069 0.01747 = 0.02088 -0.00453 0.00625 -0.00265 O32 4 0.382566 0.521078 0.090199 11.00000 0.01929 0.02660 = 0.03017 -0.00096 0.00673 0.00151 O33 4 0.163824 0.567003 0.137029 11.00000 0.01954 0.02701 = 0.01474 -0.00075 0.00337 0.00201 HKLF 4 REM CHI53 in P21/n #14 REM R1 = 0.0334 for 4652 Fo > 4sig(Fo) and 0.0415 for all 5366 data REM 300 parameters refined using 0 restraints END WGHT 0.0204 5.0723 REM Highest difference peak 2.158, deepest hole -1.726, 1-sigma level 0.162 Q1 1 -0.0119 0.6523 0.1038 11.00000 0.05 2.16 Q2 1 0.0249 0.6153 0.1631 11.00000 0.05 1.51 Q3 1 0.0621 0.6165 0.0985 11.00000 0.05 1.26 Q4 1 0.4359 0.3480 0.5932 11.00000 0.05 1.23 Q5 1 -0.1738 0.6156 0.0893 11.00000 0.05 1.22 Q6 1 -0.0199 0.6179 0.0426 11.00000 0.05 1.11 Q7 1 -0.1388 0.6170 0.0210 11.00000 0.05 1.07 Q8 1 -0.0958 0.6169 0.1449 11.00000 0.05 0.96 Q9 1 -0.0526 0.6954 0.0848 11.00000 0.05 0.90 Q10 1 0.1793 0.6156 -0.2760 11.00000 0.05 0.90 REM The information below was added by Olex2. REM REM R1 = 0.0334 for 4652 Fo > 4sig(Fo) and 0.0415 for all 24410 data REM n/a parameters refined using n/a restraints REM Highest difference peak 2.16, deepest hole -1.73 REM Mean Shift 0, Max Shift -0.003. REM +++ Tabular Listing of Refinement Information +++ REM R1_all = 0.0415 REM R1_gt = 0.0334 REM wR_ref = 0.0701 REM GOOF = 1.051 REM Shift_max = -0.003 REM Shift_mean = 0 REM Reflections_all = 24410 REM Reflections_gt = 4652 REM Parameters = n/a REM Hole = -1.73 REM Peak = 2.16 REM Flack = n/a ; _cod_data_source_file pk2707.cif _cod_data_source_block II _cod_original_cell_volume 2193.18(19) _cod_database_code 2023135 _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. ; loop_ _space_group_symop_operation_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_site_type_symbol _atom_site_label _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_calc_flag _atom_site_occupancy _atom_site_disorder_assembly _atom_site_disorder_group Pt Pt1 -0.05560(2) 0.61639(2) 0.09345(2) 0.01722(6) Uani d 1 . . C C2 -0.3155(5) 0.6274(2) 0.0693(3) 0.0219(9) Uani d 1 . . H H2A -0.3776 0.6082 0.0108 0.026 Uiso calc 1 . . H H2B -0.3664 0.6180 0.1221 0.026 Uiso calc 1 . . C C3 -0.2450(5) 0.6967(2) 0.0656(3) 0.0204(9) Uani d 1 . . H H3 -0.2631 0.7194 0.0038 0.024 Uiso calc 1 . . C C4 -0.2226(6) 0.7476(2) 0.1480(3) 0.0233(10) Uani d 1 . . H H4A -0.3286 0.7671 0.1538 0.028 Uiso calc 1 . . H H4B -0.1520 0.7875 0.1385 0.028 Uiso calc 1 . . C C5 -0.1454(5) 0.7072(2) 0.2364(3) 0.0183(9) Uani d 1 . . C C6 -0.0619(5) 0.6442(2) 0.2243(3) 0.0164(8) Uani d 1 . . C C7 0.0167(5) 0.6048(2) 0.3027(3) 0.0195(9) Uani d 1 . . H H7 0.0717 0.5621 0.2947 0.023 Uiso calc 1 . . C C8 0.0134(5) 0.6286(2) 0.3922(3) 0.0191(9) Uani d 1 . . C C9 -0.0748(5) 0.6916(2) 0.4044(3) 0.0180(9) Uani d 1 . . C C10 -0.1524(5) 0.7309(2) 0.3268(3) 0.0194(9) Uani d 1 . . H H10 -0.2091 0.7730 0.3347 0.023 Uiso calc 1 . . O O11 -0.0792(4) 0.70854(15) 0.4954(2) 0.0207(6) Uani d 1 . . C C12 -0.1635(6) 0.7729(2) 0.5106(3) 0.0248(10) Uani d 1 . . H H12A -0.1152 0.8133 0.4850 0.037 Uiso calc 1 . . H H12B -0.1546 0.7800 0.5765 0.037 Uiso calc 1 . . H H12C -0.2777 0.7689 0.4805 0.037 Uiso calc 1 . . O O13 0.0916(4) 0.59562(16) 0.4739(2) 0.0228(7) Uani d 1 . . C C14 0.1812(6) 0.5321(2) 0.4651(3) 0.0219(9) Uani d 1 . . H H14A 0.2499 0.5392 0.4196 0.026 Uiso calc 1 . . H H14B 0.1061 0.4924 0.4442 0.026 Uiso calc 1 . . C C15 0.2864(5) 0.5154(2) 0.5592(3) 0.0204(9) Uani d 1 . . O O16 0.3081(4) 0.55414(18) 0.6260(2) 0.0335(8) Uani d 1 . . O O17 0.3562(4) 0.45000(16) 0.5567(2) 0.0259(7) Uani d 1 . . C C18 0.4476(6) 0.4221(2) 0.6464(3) 0.0262(10) Uani d 1 . . H H18A 0.3748 0.4161 0.6899 0.031 Uiso calc 1 . . H H18B 0.5357 0.4550 0.6736 0.031 Uiso calc 1 . . C C19 0.5177(6) 0.3497(2) 0.6249(3) 0.0298(11) Uani d 1 . . H H19A 0.6013 0.3571 0.5883 0.036 Uiso calc 1 . . H H19B 0.4307 0.3202 0.5886 0.036 Uiso calc 1 . . C C20 0.5934(6) 0.3109(3) 0.7157(3) 0.0348(12) Uani d 1 . . H H20A 0.6450 0.2670 0.7016 0.052 Uiso calc 1 . . H H20B 0.5084 0.2997 0.7491 0.052 Uiso calc 1 . . H H20C 0.6744 0.3415 0.7533 0.052 Uiso calc 1 . . N N21 0.0072(4) 0.59004(18) -0.0416(2) 0.0165(7) Uani d 1 . . C C22 -0.0717(6) 0.6046(2) -0.1330(3) 0.0210(9) Uani d 1 . . C C23 -0.2406(6) 0.6240(2) -0.1543(3) 0.0229(10) Uani d 1 . . H H23 -0.2981 0.6286 -0.1063 0.027 Uiso calc 1 . . C C24 -0.3208(7) 0.6363(2) -0.2454(3) 0.0295(11) Uani d 1 . . H H24 -0.4326 0.6477 -0.2585 0.035 Uiso calc 1 . . C C25 -0.2346(7) 0.6316(2) -0.3190(3) 0.0301(11) Uani d 1 . . H H25 -0.2888 0.6408 -0.3802 0.036 Uiso calc 1 . . C C26 -0.0716(7) 0.6135(2) -0.2999(3) 0.0272(11) Uani d 1 . . H H26 -0.0144 0.6117 -0.3482 0.033 Uiso calc 1 . . C C27 0.0111(6) 0.5975(2) -0.2081(3) 0.0225(10) Uani d 1 . . C C28 0.1770(6) 0.5718(2) -0.1873(3) 0.0262(10) Uani d 1 . . H H28 0.2359 0.5675 -0.2346 0.031 Uiso calc 1 . . C C29 0.2488(6) 0.5537(2) -0.0978(3) 0.0228(10) Uani d 1 . . H H29 0.3547 0.5344 -0.0840 0.027 Uiso calc 1 . . C C30 0.1604(5) 0.5647(2) -0.0265(3) 0.0201(9) Uani d 1 . . C C31 0.2456(5) 0.5489(2) 0.0731(3) 0.0194(9) Uani d 1 . . O O32 0.3826(4) 0.52108(16) 0.0902(2) 0.0251(7) Uani d 1 . . O O33 0.1638(3) 0.56700(16) 0.13703(19) 0.0205(6) Uani d 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_12 _atom_site_aniso_U_13 _atom_site_aniso_U_23 Pt1 0.01864(10) 0.01974(10) 0.01431(10) 0.00199(6) 0.00582(7) 0.00078(6) C2 0.019(2) 0.024(2) 0.023(2) 0.0026(18) 0.0041(19) -0.0017(18) C3 0.019(2) 0.026(2) 0.016(2) 0.0077(18) 0.0024(17) 0.0028(17) C4 0.027(2) 0.015(2) 0.026(2) 0.0021(18) 0.002(2) -0.0026(17) C5 0.019(2) 0.0157(19) 0.019(2) -0.0028(17) 0.0017(17) 0.0021(16) C6 0.017(2) 0.0179(19) 0.016(2) -0.0012(17) 0.0053(16) 0.0001(16) C7 0.018(2) 0.019(2) 0.023(2) 0.0052(17) 0.0076(18) 0.0005(17) C8 0.020(2) 0.023(2) 0.016(2) -0.0004(18) 0.0055(17) 0.0013(17) C9 0.019(2) 0.0162(19) 0.020(2) -0.0033(17) 0.0058(18) -0.0026(16) C10 0.021(2) 0.0148(19) 0.022(2) 0.0019(17) 0.0044(18) -0.0035(17) O11 0.0299(17) 0.0166(14) 0.0164(15) 0.0046(13) 0.0064(13) -0.0026(12) C12 0.026(2) 0.023(2) 0.025(2) 0.0059(19) 0.005(2) -0.0056(19) O13 0.0315(18) 0.0233(15) 0.0135(15) 0.0115(14) 0.0043(13) 0.0014(12) C14 0.028(2) 0.021(2) 0.019(2) 0.0087(19) 0.0093(19) 0.0023(17) C15 0.023(2) 0.022(2) 0.019(2) 0.0069(18) 0.0114(18) 0.0034(17) O16 0.045(2) 0.0364(19) 0.0175(17) 0.0176(17) 0.0040(15) -0.0044(14) O17 0.0318(18) 0.0206(16) 0.0248(17) 0.0071(14) 0.0050(14) 0.0029(13) C18 0.029(3) 0.030(2) 0.021(2) 0.007(2) 0.0062(19) 0.0090(19) C19 0.040(3) 0.016(2) 0.034(3) 0.000(2) 0.009(2) 0.0036(19) C20 0.037(3) 0.027(3) 0.037(3) -0.002(2) 0.001(2) 0.007(2) N21 0.0200(18) 0.0166(17) 0.0143(17) 0.0002(14) 0.0067(14) 0.0017(13) C22 0.030(3) 0.0138(19) 0.020(2) -0.0051(18) 0.0066(19) -0.0021(16) C23 0.030(3) 0.021(2) 0.018(2) 0.0016(19) 0.007(2) -0.0034(17) C24 0.037(3) 0.029(2) 0.020(2) 0.003(2) -0.002(2) 0.0030(19) C25 0.050(3) 0.020(2) 0.017(2) 0.002(2) 0.001(2) 0.0040(18) C26 0.044(3) 0.019(2) 0.020(2) -0.009(2) 0.010(2) -0.0025(17) C27 0.036(3) 0.0148(19) 0.020(2) -0.0104(19) 0.013(2) -0.0057(17) C28 0.037(3) 0.023(2) 0.024(2) -0.005(2) 0.019(2) -0.0091(19) C29 0.023(2) 0.021(2) 0.027(2) -0.0051(18) 0.011(2) -0.0051(18) C30 0.024(2) 0.0136(19) 0.025(2) -0.0048(17) 0.0101(19) -0.0045(17) C31 0.021(2) 0.017(2) 0.021(2) -0.0026(17) 0.0062(18) -0.0045(17) O32 0.0193(16) 0.0266(17) 0.0302(18) 0.0015(14) 0.0067(14) -0.0010(14) O33 0.0195(16) 0.0270(16) 0.0147(15) 0.0020(13) 0.0034(12) -0.0008(12) 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_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle _geom_angle_publ_flag C2 Pt1 C3 . . 38.79(16) ? C2 Pt1 N21 . . 107.11(15) ? C3 Pt1 N21 . . 106.53(14) ? C6 Pt1 C2 . . 84.62(17) ? C6 Pt1 C3 . . 80.72(16) ? C6 Pt1 N21 . . 167.94(15) ? C6 Pt1 O33 . . 90.88(14) ? O33 Pt1 C2 . . 156.21(14) ? O33 Pt1 C3 . . 162.41(14) ? O33 Pt1 N21 . . 79.46(12) ? Pt1 C2 H2A . . 116.5 ? Pt1 C2 H2B . . 116.5 ? H2A C2 H2B . . 113.5 ? C3 C2 Pt1 . . 71.3(2) ? C3 C2 H2A . . 116.5 ? C3 C2 H2B . . 116.5 ? Pt1 C3 H3 . . 116.0 ? C2 C3 Pt1 . . 69.9(2) ? C2 C3 H3 . . 116.0 ? C2 C3 C4 . . 121.2(4) ? C4 C3 Pt1 . . 108.5(3) ? C4 C3 H3 . . 116.0 ? C3 C4 H4A . . 109.8 ? C3 C4 H4B . . 109.8 ? C3 C4 C5 . . 109.5(3) ? H4A C4 H4B . . 108.2 ? C5 C4 H4A . . 109.8 ? C5 C4 H4B . . 109.8 ? C6 C5 C4 . . 116.1(4) ? C6 C5 C10 . . 120.1(4) ? C10 C5 C4 . . 123.8(4) ? C5 C6 Pt1 . . 117.0(3) ? C5 C6 C7 . . 119.6(4) ? C7 C6 Pt1 . . 123.5(3) ? C6 C7 H7 . . 119.7 ? C8 C7 C6 . . 120.7(4) ? C8 C7 H7 . . 119.7 ? C7 C8 C9 . . 119.8(4) ? O13 C8 C7 . . 125.5(4) ? O13 C8 C9 . . 114.8(4) ? C10 C9 C8 . . 119.6(4) ? O11 C9 C8 . . 115.6(4) ? O11 C9 C10 . . 124.8(4) ? C5 C10 H10 . . 119.9 ? C9 C10 C5 . . 120.2(4) ? C9 C10 H10 . . 119.9 ? C9 O11 C12 . . 117.1(3) ? O11 C12 H12A . . 109.5 ? O11 C12 H12B . . 109.5 ? O11 C12 H12C . . 109.5 ? H12A C12 H12B . . 109.5 ? H12A C12 H12C . . 109.5 ? H12B C12 H12C . . 109.5 ? C8 O13 C14 . . 116.8(3) ? O13 C14 H14A . . 110.2 ? O13 C14 H14B . . 110.2 ? O13 C14 C15 . . 107.7(3) ? H14A C14 H14B . . 108.5 ? C15 C14 H14A . . 110.2 ? C15 C14 H14B . . 110.2 ? O16 C15 C14 . . 125.9(4) ? O16 C15 O17 . . 124.7(4) ? O17 C15 C14 . . 109.4(4) ? C15 O17 C18 . . 115.9(3) ? O17 C18 H18A . . 110.6 ? O17 C18 H18B . . 110.6 ? O17 C18 C19 . . 105.9(4) ? H18A C18 H18B . . 108.7 ? C19 C18 H18A . . 110.6 ? C19 C18 H18B . . 110.6 ? C18 C19 H19A . . 109.7 ? C18 C19 H19B . . 109.7 ? C18 C19 C20 . . 109.9(4) ? H19A C19 H19B . . 108.2 ? C20 C19 H19A . . 109.7 ? C20 C19 H19B . . 109.7 ? C19 C20 H20A . . 109.5 ? C19 C20 H20B . . 109.5 ? C19 C20 H20C . . 109.5 ? H20A C20 H20B . . 109.5 ? H20A C20 H20C . . 109.5 ? H20B C20 H20C . . 109.5 ? C22 N21 Pt1 . . 132.1(3) ? C30 N21 Pt1 . . 109.0(3) ? C30 N21 C22 . . 118.1(4) ? N21 C22 C23 . . 120.5(4) ? N21 C22 C27 . . 121.4(4) ? C23 C22 C27 . . 118.0(4) ? C22 C23 H23 . . 119.7 ? C24 C23 C22 . . 120.6(4) ? C24 C23 H23 . . 119.7 ? C23 C24 H24 . . 119.7 ? C23 C24 C25 . . 120.5(5) ? C25 C24 H24 . . 119.7 ? C24 C25 H25 . . 120.2 ? C26 C25 C24 . . 119.7(4) ? C26 C25 H25 . . 120.2 ? C25 C26 H26 . . 119.5 ? C25 C26 C27 . . 120.9(5) ? C27 C26 H26 . . 119.5 ? C22 C27 C28 . . 117.8(4) ? C26 C27 C22 . . 120.1(5) ? C26 C27 C28 . . 122.1(4) ? C27 C28 H28 . . 120.1 ? C29 C28 C27 . . 119.7(4) ? C29 C28 H28 . . 120.1 ? C28 C29 H29 . . 120.5 ? C28 C29 C30 . . 119.1(4) ? C30 C29 H29 . . 120.5 ? N21 C30 C29 . . 123.7(4) ? N21 C30 C31 . . 117.8(4) ? C29 C30 C31 . . 118.5(4) ? O32 C31 C30 . . 120.3(4) ? O32 C31 O33 . . 124.0(4) ? O33 C31 C30 . . 115.7(4) ? C31 O33 Pt1 . . 117.2(3) ? loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_site_symmetry_2 _geom_bond_distance _geom_bond_publ_flag Pt1 C2 . 2.118(4) ? Pt1 C3 . 2.138(4) ? Pt1 C6 . 1.993(4) ? Pt1 N21 . 2.200(3) ? Pt1 O33 . 2.016(3) ? C2 H2A . 0.9700 ? C2 H2B . 0.9700 ? C2 C3 . 1.413(6) ? C3 H3 . 0.9800 ? C3 C4 . 1.511(6) ? C4 H4A . 0.9700 ? C4 H4B . 0.9700 ? C4 C5 . 1.515(6) ? C5 C6 . 1.385(6) ? C5 C10 . 1.406(6) ? C6 C7 . 1.400(6) ? C7 H7 . 0.9300 ? C7 C8 . 1.387(6) ? C8 C9 . 1.407(6) ? C8 O13 . 1.378(5) ? C9 C10 . 1.388(6) ? C9 O11 . 1.375(5) ? C10 H10 . 0.9300 ? O11 C12 . 1.422(5) ? C12 H12A . 0.9600 ? C12 H12B . 0.9600 ? C12 H12C . 0.9600 ? O13 C14 . 1.411(5) ? C14 H14A . 0.9700 ? C14 H14B . 0.9700 ? C14 C15 . 1.500(6) ? C15 O16 . 1.195(5) ? C15 O17 . 1.345(5) ? O17 C18 . 1.466(5) ? C18 H18A . 0.9700 ? C18 H18B . 0.9700 ? C18 C19 . 1.519(6) ? C19 H19A . 0.9700 ? C19 H19B . 0.9700 ? C19 C20 . 1.524(6) ? C20 H20A . 0.9600 ? C20 H20B . 0.9600 ? C20 H20C . 0.9600 ? N21 C22 . 1.387(5) ? N21 C30 . 1.328(5) ? C22 C23 . 1.415(6) ? C22 C27 . 1.417(6) ? C23 H23 . 0.9300 ? C23 C24 . 1.378(6) ? C24 H24 . 0.9300 ? C24 C25 . 1.413(7) ? C25 H25 . 0.9300 ? C25 C26 . 1.362(7) ? C26 H26 . 0.9300 ? C26 C27 . 1.405(6) ? C27 C28 . 1.425(7) ? C28 H28 . 0.9300 ? C28 C29 . 1.363(6) ? C29 H29 . 0.9300 ? C29 C30 . 1.407(6) ? C30 C31 . 1.510(6) ? C31 O32 . 1.224(5) ? C31 O33 . 1.307(5) ? loop_ _geom_hbond_atom_site_label_D _geom_hbond_atom_site_label_H _geom_hbond_atom_site_label_A _geom_hbond_site_symmetry_D _geom_hbond_site_symmetry_H _geom_hbond_site_symmetry_A _geom_hbond_distance_DH _geom_hbond_distance_HA _geom_hbond_distance_DA _geom_hbond_angle_DHA _geom_hbond_publ_flag C20 H20C O33 1_555 1_555 3_666 0.96 2.52 3.462(6) 168 y C28 H28 O16 1_555 1_555 1_554 0.93 2.26 3.159(5) 164 y C29 H29 O32 1_555 1_555 3_665 0.93 2.43 3.334(6) 166 y C18 H18A Cg1 1_555 1_555 3_566 0.97 2.97 3.711(5) 134 y C20 H20A Cg2 1_555 1_555 2_545 0.96 2.78 3.605(6) 144 y loop_ _geom_torsion_atom_site_label_1 _geom_torsion_atom_site_label_2 _geom_torsion_atom_site_label_3 _geom_torsion_atom_site_label_4 _geom_torsion_site_symmetry_1 _geom_torsion_site_symmetry_2 _geom_torsion_site_symmetry_3 _geom_torsion_site_symmetry_4 _geom_torsion _geom_torsion_publ_flag Pt1 C2 C3 C4 . . . . -100.0(4) ? Pt1 C3 C4 C5 . . . . -30.0(4) ? Pt1 C6 C7 C8 . . . . 177.3(3) ? Pt1 N21 C22 C23 . . . . -18.3(6) ? Pt1 N21 C22 C27 . . . . 164.5(3) ? Pt1 N21 C30 C29 . . . . -169.3(3) ? Pt1 N21 C30 C31 . . . . 8.9(4) ? C2 C3 C4 C5 . . . . 47.2(5) ? C3 C4 C5 C6 . . . . 21.0(5) ? C3 C4 C5 C10 . . . . -160.3(4) ? C4 C5 C6 Pt1 . . . . 0.0(5) ? C4 C5 C6 C7 . . . . 178.3(4) ? C4 C5 C10 C9 . . . . -178.3(4) ? C5 C6 C7 C8 . . . . -0.8(6) ? C6 C5 C10 C9 . . . . 0.4(6) ? C6 C7 C8 C9 . . . . 2.4(6) ? C6 C7 C8 O13 . . . . -177.4(4) ? C7 C8 C9 C10 . . . . -2.5(6) ? C7 C8 C9 O11 . . . . 176.3(4) ? C7 C8 O13 C14 . . . . -0.4(6) ? C8 C9 C10 C5 . . . . 1.2(6) ? C8 C9 O11 C12 . . . . 178.3(4) ? C8 O13 C14 C15 . . . . 167.0(4) ? C9 C8 O13 C14 . . . . 179.8(4) ? C10 C5 C6 Pt1 . . . . -178.8(3) ? C10 C5 C6 C7 . . . . -0.5(6) ? C10 C9 O11 C12 . . . . -2.9(6) ? O11 C9 C10 C5 . . . . -177.5(4) ? O13 C8 C9 C10 . . . . 177.3(4) ? O13 C8 C9 O11 . . . . -4.0(5) ? O13 C14 C15 O16 . . . . -9.7(6) ? O13 C14 C15 O17 . . . . 171.5(3) ? C14 C15 O17 C18 . . . . -173.1(4) ? C15 O17 C18 C19 . . . . -178.4(4) ? O16 C15 O17 C18 . . . . 8.0(6) ? O17 C18 C19 C20 . . . . -171.5(4) ? N21 C22 C23 C24 . . . . -177.9(4) ? N21 C22 C27 C26 . . . . -179.2(4) ? N21 C22 C27 C28 . . . . 2.6(6) ? N21 C30 C31 O32 . . . . 175.2(4) ? N21 C30 C31 O33 . . . . -5.0(5) ? C22 N21 C30 C29 . . . . 1.9(6) ? C22 N21 C30 C31 . . . . -180.0(3) ? C22 C23 C24 C25 . . . . -1.8(7) ? C22 C27 C28 C29 . . . . 1.4(6) ? C23 C22 C27 C26 . . . . 3.5(6) ? C23 C22 C27 C28 . . . . -174.7(4) ? C23 C24 C25 C26 . . . . 1.2(7) ? C24 C25 C26 C27 . . . . 1.7(7) ? C25 C26 C27 C22 . . . . -4.1(6) ? C25 C26 C27 C28 . . . . 174.0(4) ? C26 C27 C28 C29 . . . . -176.7(4) ? C27 C22 C23 C24 . . . . -0.6(6) ? C27 C28 C29 C30 . . . . -3.6(6) ? C28 C29 C30 N21 . . . . 2.0(6) ? C28 C29 C30 C31 . . . . -176.1(4) ? C29 C30 C31 O32 . . . . -6.5(6) ? C29 C30 C31 O33 . . . . 173.3(4) ? C30 N21 C22 C23 . . . . 173.0(4) ? C30 N21 C22 C27 . . . . -4.2(6) ? C30 C31 O33 Pt1 . . . . -2.6(4) ? O32 C31 O33 Pt1 . . . . 177.2(3) ? loop_ _refln_index_h _refln_index_k _refln_index_l _refln_F_squared_meas _refln_F_squared_sigma 0 0 2 208206 3820.35 0 0 2 212623 3744.24 0 0 -2 204167 3730.33 0 0 -3 612.825 280.237 0 0 3 257.075 148.846 0 0 -3 237.449 199.473 0 0 3 296.901 270.46 0 0 -4 357401 6989.39 0 0 4 359017 7227.93 0 0 4 355938 6934.77 0 0 4 352158 4140.17 0 0 -4 345356 6779.3 0 0 4 340882 5821.19 0 0 -4 354779 4225.14 0 0 5 66.5376 168.365 0 0 5 241.789 216.578 0 0 5 -115.225 100.84 0 0 -5 351.044 438.631 0 0 5 91.594 214.626 0 0 -5 40.2067 109.461 0 0 -5 21.2686 223.201 0 0 -5 238.13 312.862 0 0 6 393823 9378.67 0 0 6 385705 8923.32 0 0 6 354741 7493.15 0 0 -6 362778 8921.69 0 0 6 369742 5088.88 0 0 -6 393105 9044.03 0 0 -6 375458 5232.69 0 0 7 492.803 214.727 0 0 7 215.676 377.483 0 0 -7 410.156 613.197 0 0 -7 249.176 100.578 0 0 7 335.797 140.121 0 0 7 336.125 187.441 0 0 -8 850.527 681.667 0 0 8 701.127 250.43 0 0 8 736.4 440.289 0 0 8 600.798 124.021 0 0 8 336.541 326.584 0 0 9 248.665 113.877 0 0 9 -507.72 604.479 0 0 9 602 322 0 0 -9 601.656 674.67 0 0 -10 210459 8963.26 0 0 10 205786 4374.97 0 0 10 212408 9175.78 0 0 10 217558 8898.95 0 0 -11 688.48 780.342 0 0 11 413.297 430.947 0 0 12 90859.7 6405.43 0 0 -12 83651.5 6259.99 0 0 -13 -362.555 661.733 0 0 13 2662.97 1278.8 0 0 -14 11930.6 2582.94 0 0 -15 1391.21 919.966 0 0 -16 87977.7 7646.55 0 0 -17 87.5146 283.135 0 0 -18 20183.6 3941.21 0 1 -2 121358 2627.54 0 1 2 125431 2985.42 0 1 2 130011 3315.46 0 -1 -2 117537 2823.75 0 1 2 120511 2872.11 0 -1 -2 128240 2998.48 0 -1 -2 120752 3225.56 0 -1 -2 119533 2826.74 0 -1 -2 122744 3235 0 -1 2 126364 2716.29 0 1 2 119431 2821.43 0 -1 3 17958.2 1303.35 0 -1 -3 18570.4 1503.99 0 -1 -3 19609.3 1436.62 0 1 3 17206.2 1291.48 0 -1 -3 16897.1 1234.86 0 -1 3 17719.6 932.711 0 1 -3 17065.3 1241.61 0 -1 -3 17895.5 1450.64 0 1 3 18124.9 1371.39 0 1 3 18068.3 1287.98 0 -1 -3 19102.2 885.46 0 1 3 19149 1510.55 0 -1 -3 17012.6 1301.34 0 1 4 136720 4226.72 0 -1 -4 145182 2742.1 0 -1 -4 134808 4260.22 0 -1 -4 141386 4594.54 0 1 4 147274 4492.64 0 1 4 137094 4086.6 0 -1 4 135451 2882.69 0 -1 4 140299 4299.17 0 -1 4 140725 4368.93 0 -1 -4 147684 4557.76 0 1 4 147172 4813.02 0 1 -4 141076 4215.71 0 -1 -4 135614 4670.98 0 -1 5 359464 5138.15 0 -1 -5 376200 8384.77 0 -1 -5 384714 8196.46 0 1 5 366595 4526.43 0 1 -5 373328 8001.34 0 -1 5 373515 8008.75 0 -1 -5 366339 7881.87 0 1 5 383056 8227.92 0 -1 5 380790 8058.92 0 -1 -5 379683 4881.6 0 1 5 376782 8669.07 0 -1 -5 367963 8486.24 0 1 5 362534 7349.45 0 1 -5 379736 7793.9 0 -1 6 43365.3 3004.17 0 -1 -6 39950.1 2861.49 0 -1 -6 40366 1738.53 0 -1 6 38245.5 1772.16 0 -1 6 39767.2 2864.78 0 1 6 38037.4 2599.52 0 -1 -6 40668.8 3008.72 0 1 -6 41056.5 2845.1 0 1 6 39556.2 3072.56 0 -1 -6 39763 3052.16 0 1 6 39286.2 1571.02 0 1 6 40206.5 2912.49 0 1 7 97664.3 5227.16 0 1 7 99444.4 4958.3 0 -1 7 91640.3 2889.39 0 1 7 94568.1 4420.39 0 1 -7 91716 4757.39 0 -1 7 91198.7 3901.61 0 -1 7 98601.2 4955.72 0 -1 7 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