#------------------------------------------------------------------------------ #$Date: 2020-08-21 04:44:32 +0300 (Fri, 21 Aug 2020) $ #$Revision: 255506 $ #$URL: file:///home/coder/svn-repositories/cod/cif/7/70/52/7705230.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_7705230 loop_ _publ_author_name 'Silva, D\'ebora Eduarda Soares' 'Becceneri, Amanda Blanque' 'Santiago, Jo\~ao Victor Biagi' 'Neto, Jos\'e Anchieta Gomes' 'Ellena, Javier A.' 'Cominetti, Marcia Regina' 'Pereira, Jos\'e Clayston Melo' 'Hannon, Michael John' 'Vieira de Godoy Netto, Adelino' _publ_section_title ; Silver(I) complexes of 3-methoxy-4-hydroxybenzaldehyde thiosemicarbazones and triphenylphosphine: structural, cytotoxic and apoptotic studies ; _journal_name_full 'Dalton Transactions' _journal_paper_doi 10.1039/D0DT01134G _journal_year 2020 _chemical_formula_moiety 'C51 H52 Ag Cl N4 O3 P2 S, 0.25[C2H3N]' _chemical_formula_sum 'C50 H53 Ag Cl2 N5 O3 P2 S0.12' _chemical_formula_weight 1016.69 _chemical_name_systematic DS05 _space_group_crystal_system monoclinic _space_group_IT_number 15 _space_group_name_Hall '-I 2ya' _space_group_name_H-M_alt 'I 1 2/a 1' _atom_sites_solution_hydrogens geom _atom_sites_solution_primary dual _audit_creation_date 2019-09-30 _audit_creation_method ; Olex2 1.3 (compiled 2019.09.11 svn.r3662 for OlexSys, GUI svn.r5938) ; _audit_update_record ; 2020-03-23 deposited with the CCDC. 2020-08-19 downloaded from the CCDC. ; _cell_angle_alpha 90 _cell_angle_beta 100.785(3) _cell_angle_gamma 90 _cell_formula_units_Z 8 _cell_length_a 25.4270(9) _cell_length_b 12.1243(5) _cell_length_c 33.2299(10) _cell_measurement_reflns_used 15348 _cell_measurement_temperature 293(2) _cell_measurement_theta_max 28.5650 _cell_measurement_theta_min 2.9600 _cell_volume 10063.3(6) _computing_cell_refinement 'CrysAlisPro 1.171.39.35c (Rigaku OD, 2017)' _computing_data_collection 'CrysAlisPro 1.171.39.35c (Rigaku OD, 2017)' _computing_data_reduction 'CrysAlisPro 1.171.39.35c (Rigaku OD, 2017)' _computing_molecular_graphics 'Olex2 1.3 (Dolomanov et al., 2009)' _computing_publication_material 'Olex2 1.3 (Dolomanov et al., 2009)' _computing_structure_refinement 'XL n/a (Sheldrick, 2008)' _computing_structure_solution 'ShelXT n/a (Sheldrick, 2015)' _diffrn_ambient_temperature 293(2) _diffrn_detector 'CCD plate' _diffrn_measured_fraction_theta_full 0.999 _diffrn_measured_fraction_theta_max 0.996 _diffrn_measurement_details ; List of Runs (angles in degrees, time in seconds): # Type Start End Width t~exp~ \w \q \k \f Frames #-------------------------------------------------------------------------- 1 \w 33.00 66.00 1.00 42.01 -- 27.63 54.00 -30.00 33 2 \w -69.00 118.00 1.00 42.01 -- 27.63 54.00 90.00 187 3 \w -46.00 -20.00 1.00 42.01 -- 27.63 54.00 -30.00 26 ; _diffrn_measurement_device 'two-circle diffractometer' _diffrn_measurement_device_type 'XtaLAB Mini (ROW)' _diffrn_measurement_method '\w scans' _diffrn_orient_matrix_type 'CrysAlisPro convention (1999,Acta A55,543-557)' _diffrn_orient_matrix_UB_11 0.0011852000 _diffrn_orient_matrix_UB_12 0.0558922000 _diffrn_orient_matrix_UB_13 0.0063572000 _diffrn_orient_matrix_UB_21 -0.0052502000 _diffrn_orient_matrix_UB_22 0.0171394000 _diffrn_orient_matrix_UB_23 -0.0207926000 _diffrn_orient_matrix_UB_31 -0.0278643000 _diffrn_orient_matrix_UB_32 -0.0006529000 _diffrn_orient_matrix_UB_33 0.0000428000 _diffrn_radiation_monochromator graphite _diffrn_radiation_probe x-ray _diffrn_radiation_type 'Mo K\a' _diffrn_radiation_wavelength 0.71073 _diffrn_reflns_av_R_equivalents 0.0257 _diffrn_reflns_av_unetI/netI 0.0390 _diffrn_reflns_Laue_measured_fraction_full 0.999 _diffrn_reflns_Laue_measured_fraction_max 0.996 _diffrn_reflns_limit_h_max 33 _diffrn_reflns_limit_h_min -32 _diffrn_reflns_limit_k_max 13 _diffrn_reflns_limit_k_min -15 _diffrn_reflns_limit_l_max 43 _diffrn_reflns_limit_l_min -42 _diffrn_reflns_number 23269 _diffrn_reflns_point_group_measured_fraction_full 0.999 _diffrn_reflns_point_group_measured_fraction_max 0.996 _diffrn_reflns_theta_full 25.242 _diffrn_reflns_theta_max 27.500 _diffrn_reflns_theta_min 2.515 _diffrn_source 'fine-focus sealed X-ray tube' _diffrn_source_type 'Rigaku (Mo) X-ray Source' _exptl_absorpt_coefficient_mu 0.621 _exptl_absorpt_correction_T_max 1.00000 _exptl_absorpt_correction_T_min 0.96167 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_process_details ; CrysAlisPro 1.171.39.35c (Rigaku Oxford Diffraction, 2017) Empirical absorption correction using spherical harmonics, implemented in SCALE3 ABSPACK scaling algorithm. ; _exptl_crystal_colour 'clear light colourless' _exptl_crystal_colour_lustre clear _exptl_crystal_colour_modifier light _exptl_crystal_colour_primary colourless _exptl_crystal_density_diffrn 1.342 _exptl_crystal_description block _exptl_crystal_F_000 4200 _exptl_crystal_size_max 0.35 _exptl_crystal_size_mid 0.28 _exptl_crystal_size_min 0.2 _refine_diff_density_max 0.445 _refine_diff_density_min -0.397 _refine_diff_density_rms 0.051 _refine_ls_extinction_method none _refine_ls_goodness_of_fit_ref 1.060 _refine_ls_hydrogen_treatment constr _refine_ls_matrix_type full _refine_ls_number_parameters 569 _refine_ls_number_reflns 11513 _refine_ls_number_restraints 0 _refine_ls_restrained_S_all 1.060 _refine_ls_R_factor_all 0.0628 _refine_ls_R_factor_gt 0.0366 _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^)+(0.0233P)^2^+9.7236P] where P=(Fo^2^+2Fc^2^)/3' _refine_ls_weighting_scheme calc _refine_ls_wR_factor_gt 0.0722 _refine_ls_wR_factor_ref 0.0882 _reflns_Friedel_coverage 0.000 _reflns_number_gt 8224 _reflns_number_total 11513 _reflns_threshold_expression 'I > 2\s(I)' _cod_data_source_file d0dt01134g2.cif _cod_data_source_block ds05_2 _cod_database_code 7705230 _shelx_shelxl_version_number 2018/3 _chemical_oxdiff_formula 'C51 H51 N4 O3 Cl1 P2 S1 Ag1 ' _chemical_oxdiff_usercomment 'Debora Javier 24-09-2019' _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 99.80 _reflns_odcompleteness_iscentric 1 _reflns_odcompleteness_theta 26.32 _olex2_refinement_description ; 1. Fixed Uiso At 1.2 times of: All C(H) groups, All C(H,H) groups, All N(H) groups, All N(H,H) groups At 1.5 times of: All C(H,H,H) groups 2.a Secondary CH2 refined with riding coordinates: C10(H10A,H10B), C9(H9A,H9B), C12(H12A,H12B), C16(H16A,H16B), C15(H15A,H15B), C13(H13A,H13B) 2.b Aromatic/amide H refined with riding coordinates: N19(H19), C2(H2), C30(H30), C5(H5), C17(H17), C4(H4), C29(H29), C33(H33), C35(H35), C43(H43), C53(H53), C39(H39), C34(H34), C59(H59), C26(H26), C37(H37), C28(H28), C63(H63), C42(H42), C57(H57), C27(H27), C41(H41), C54(H54), C50(H50), C36(H36), C55(H55), C62(H62), C40(H40), C60(H60), C46(H46), C61(H61), C56(H56), C49(H49), C47(H47), C48(H48) 2.c X=CH2 refined with riding coordinates: N22(H22A,H22B) 2.d Idealised Me refined as rotating group: C24(H24A,H24B,H24C) ; _smtbx_masks_void_probe_radius 1.2 _smtbx_masks_void_truncation_radius 1.2 _shelx_res_file ; TITL ds05_2_a.res in I2/a ds05_2.res created by SHELXL-2018/3 at 14:29:41 on 30-Sep-2019 REM Old TITL DS05_2 in I2/a REM SHELXT solution in I2/a REM R1 0.168, Rweak 0.015, Alpha 0.030, Orientation as input REM Formula found by SHELXT: C46 N8 O4 P Cl3 Ag CELL 0.71073 25.427 12.1243 33.2299 90 100.785 90 ZERR 8 0.0009 0.0005 0.001 0 0.003 0 LATT 2 SYMM 0.5-X,+Y,-Z SFAC C H Ag Cl N O P S UNIT 400 424 8 16 40 24 16 1 L.S. 3 PLAN 13 TEMP 20(2) CONF BOND $H LIST 6 ABIN MORE -1 fmap 2 acta OMIT -10 55 REM REM REM WGHT 0.023300 9.723600 FVAR 0.73406 AG1 3 0.411146 0.649228 0.610740 11.00000 0.04573 0.06475 = 0.04169 0.00886 0.00834 -0.00982 S21 8 0.329858 0.690004 0.645717 11.00000 0.04900 0.04416 = 0.04998 0.00624 0.01934 -0.00282 P31 7 0.490709 0.739734 0.653041 11.00000 0.04000 0.05695 = 0.04314 0.00161 0.00518 -0.00722 CL44 4 0.432373 0.440662 0.618845 11.00000 0.07048 0.06676 = 0.06778 0.01317 0.03619 0.00992 P51 7 0.389400 0.709584 0.538351 11.00000 0.04143 0.09361 = 0.03796 0.01826 0.00658 -0.00871 O8 6 0.304922 -0.098899 0.748451 11.00000 0.04236 0.04137 = 0.05149 0.01122 0.01324 0.00658 O23 6 0.229553 0.044274 0.735049 11.00000 0.03725 0.05099 = 0.06384 0.01689 0.02022 0.00408 N11 5 0.321528 -0.249546 0.820051 11.00000 0.04491 0.04100 = 0.03917 0.00294 0.00830 0.00421 O14 6 0.354236 -0.299061 0.905091 11.00000 0.07447 0.09633 = 0.04148 0.00693 0.00913 0.02162 N22 5 0.265416 0.573274 0.682465 11.00000 0.04847 0.04804 = 0.06487 0.01305 0.02956 0.00452 AFIX 93 H22A 2 0.254904 0.512775 0.691920 11.00000 -1.20000 H22B 2 0.248587 0.633758 0.684826 11.00000 -1.20000 AFIX 0 N19 5 0.332265 0.478382 0.661286 11.00000 0.05514 0.04253 = 0.08111 0.01544 0.04028 0.00169 AFIX 43 H19 2 0.359947 0.476783 0.649872 11.00000 -1.20000 AFIX 0 N18 5 0.314071 0.382158 0.676296 11.00000 0.05460 0.04174 = 0.07318 0.01161 0.03359 -0.00126 C6 1 0.315716 -0.007186 0.728246 11.00000 0.04008 0.04078 = 0.04188 0.00171 0.00901 0.00094 C20 1 0.307258 0.573296 0.664385 11.00000 0.03778 0.04806 = 0.03852 0.00413 0.01251 -0.00205 C7 1 0.275002 0.072392 0.721233 11.00000 0.03820 0.04270 = 0.04105 0.00142 0.01271 0.00024 C32 1 0.493711 0.752452 0.707925 11.00000 0.04441 0.05385 = 0.04701 0.00428 0.00840 0.00111 C10 1 0.326474 -0.276281 0.777901 11.00000 0.05338 0.04078 = 0.03973 0.00024 0.00595 0.00671 AFIX 23 H10A 2 0.291932 -0.301384 0.763257 11.00000 -1.20000 H10B 2 0.351437 -0.337066 0.778620 11.00000 -1.20000 AFIX 0 C9 1 0.344933 -0.183346 0.754370 11.00000 0.04810 0.04746 = 0.04226 0.00518 0.01245 0.01116 AFIX 23 H9A 2 0.378398 -0.153886 0.769349 11.00000 -1.20000 H9B 2 0.350916 -0.209780 0.728045 11.00000 -1.20000 AFIX 0 C38 1 0.498599 0.880425 0.636601 11.00000 0.05474 0.05790 = 0.04227 0.00164 0.00240 -0.00837 C2 1 0.282747 0.169979 0.702826 11.00000 0.04482 0.04079 = 0.05748 0.00704 0.01996 0.00533 AFIX 43 H2 2 0.255569 0.222385 0.698378 11.00000 -1.20000 AFIX 0 C3 1 0.331452 0.191459 0.690620 11.00000 0.05520 0.04211 = 0.06826 0.00750 0.03099 0.00031 C25 1 0.553812 0.675499 0.648232 11.00000 0.04132 0.05634 = 0.04719 -0.00026 0.00438 -0.00375 C24 1 0.183130 0.110118 0.721661 11.00000 0.03891 0.05940 = 0.07333 0.00794 0.01441 0.00627 AFIX 137 H24A 2 0.176246 0.114828 0.692304 11.00000 -1.50000 H24B 2 0.188935 0.182780 0.733108 11.00000 -1.50000 H24C 2 0.152947 0.077087 0.730553 11.00000 -1.50000 AFIX 0 C30 1 0.597019 0.663875 0.679873 11.00000 0.05205 0.06768 = 0.04534 -0.00121 0.00322 -0.00221 AFIX 43 H30 2 0.594006 0.684405 0.706312 11.00000 -1.20000 AFIX 0 C5 1 0.362890 0.012405 0.714757 11.00000 0.04405 0.04613 = 0.07045 0.00630 0.02264 0.00922 AFIX 43 H5 2 0.389626 -0.040968 0.718159 11.00000 -1.20000 AFIX 0 C52 1 0.448182 0.722127 0.514476 11.00000 0.04368 0.11240 = 0.03938 0.02671 0.00451 -0.00954 C17 1 0.343182 0.297967 0.674385 11.00000 0.05953 0.05181 = 0.08776 0.01261 0.04343 0.00151 AFIX 43 H17 2 0.373067 0.304752 0.662156 11.00000 -1.20000 AFIX 0 C58 1 0.345533 0.616888 0.504877 11.00000 0.04206 0.11280 = 0.04269 0.00982 0.01157 -0.01389 C12 1 0.372613 -0.212464 0.843805 11.00000 0.05566 0.06860 = 0.04682 -0.00306 0.00864 -0.00330 AFIX 23 H12A 2 0.382233 -0.142246 0.833206 11.00000 -1.20000 H12B 2 0.400308 -0.265437 0.841051 11.00000 -1.20000 AFIX 0 C16 1 0.304365 -0.348721 0.838874 11.00000 0.06386 0.05244 = 0.05190 0.00865 0.01051 -0.00173 AFIX 23 H16A 2 0.328467 -0.408916 0.835883 11.00000 -1.20000 H16B 2 0.268777 -0.369179 0.824789 11.00000 -1.20000 AFIX 0 C4 1 0.370354 0.111598 0.696160 11.00000 0.04950 0.05286 = 0.08747 0.01068 0.03703 0.00446 AFIX 43 H4 2 0.402353 0.124478 0.687227 11.00000 -1.20000 AFIX 0 C29 1 0.644740 0.621863 0.672440 11.00000 0.05058 0.07920 = 0.06313 0.00379 -0.00292 0.01016 AFIX 43 H29 2 0.673665 0.614059 0.693973 11.00000 -1.20000 AFIX 0 C33 1 0.473711 0.667779 0.727930 11.00000 0.06906 0.06494 = 0.06006 0.00208 0.01595 -0.00916 AFIX 43 H33 2 0.458437 0.606771 0.713254 11.00000 -1.20000 AFIX 0 C35 1 0.496744 0.761419 0.791625 11.00000 0.06949 0.09265 = 0.05065 0.00350 0.01508 0.01784 AFIX 43 H35 2 0.498134 0.764113 0.819774 11.00000 -1.20000 AFIX 0 C45 1 0.358813 0.845027 0.530436 11.00000 0.04758 0.10059 = 0.05937 0.03065 0.00326 -0.00301 C43 1 0.545260 0.922129 0.626863 11.00000 0.06446 0.07421 = 0.06986 0.00693 0.00447 -0.02082 AFIX 43 H43 2 0.575878 0.878528 0.630551 11.00000 -1.20000 AFIX 0 C53 1 0.461626 0.643196 0.488589 11.00000 0.05432 0.11411 = 0.06092 0.02993 0.01885 0.00578 AFIX 43 H53 2 0.439354 0.582606 0.481619 11.00000 -1.20000 AFIX 0 C15 1 0.303707 -0.331354 0.883554 11.00000 0.07592 0.07876 = 0.05571 0.01686 0.02541 0.01102 AFIX 23 H15A 2 0.277577 -0.275042 0.886459 11.00000 -1.20000 H15B 2 0.293000 -0.399234 0.895208 11.00000 -1.20000 AFIX 0 C39 1 0.454024 0.947794 0.630679 11.00000 0.07566 0.07183 = 0.06746 0.01296 0.01266 0.00416 AFIX 43 H39 2 0.422097 0.921388 0.636807 11.00000 -1.20000 AFIX 0 C34 1 0.476154 0.672688 0.770005 11.00000 0.07714 0.08529 = 0.06479 0.01764 0.02791 -0.00060 AFIX 43 H34 2 0.463393 0.613884 0.783374 11.00000 -1.20000 AFIX 0 C59 1 0.352517 0.505777 0.511716 11.00000 0.05521 0.11835 = 0.06086 -0.00348 0.00884 -0.01383 AFIX 43 H59 2 0.378777 0.481065 0.533150 11.00000 -1.20000 AFIX 0 C26 1 0.559094 0.641221 0.609607 11.00000 0.05692 0.10664 = 0.04670 -0.00866 -0.00090 0.01320 AFIX 43 H26 2 0.529855 0.645380 0.588160 11.00000 -1.20000 AFIX 0 C37 1 0.513936 0.841978 0.730486 11.00000 0.11081 0.06392 = 0.05029 0.00123 0.00995 -0.02189 AFIX 43 H37 2 0.527041 0.901239 0.717573 11.00000 -1.20000 AFIX 0 C28 1 0.649893 0.591736 0.633906 11.00000 0.05805 0.08828 = 0.07299 -0.00213 0.01550 0.01934 AFIX 43 H28 2 0.682381 0.564981 0.628986 11.00000 -1.20000 AFIX 0 C13 1 0.369350 -0.200088 0.888285 11.00000 0.07572 0.09332 = 0.04916 -0.01417 0.00567 -0.00303 AFIX 23 H13A 2 0.403931 -0.176891 0.903473 11.00000 -1.20000 H13B 2 0.343517 -0.143088 0.891105 11.00000 -1.20000 AFIX 0 C63 1 0.304490 0.651461 0.473882 11.00000 0.05147 0.14160 = 0.04436 0.02422 0.00515 -0.01775 AFIX 43 H63 2 0.298462 0.726424 0.469190 11.00000 -1.20000 AFIX 0 C42 1 0.546839 1.027824 0.611725 11.00000 0.11092 0.08376 = 0.07649 0.01494 0.00688 -0.04515 AFIX 43 H42 2 0.578468 1.054916 0.605285 11.00000 -1.20000 AFIX 0 C57 1 0.482252 0.811459 0.525221 11.00000 0.06070 0.14281 = 0.05742 0.01467 0.01190 -0.02897 AFIX 43 H57 2 0.473839 0.865092 0.542999 11.00000 -1.20000 AFIX 0 C27 1 0.606854 0.601137 0.602439 11.00000 0.07620 0.12123 = 0.05677 -0.01264 0.01446 0.02372 AFIX 43 H27 2 0.610072 0.580206 0.576084 11.00000 -1.20000 AFIX 0 C41 1 0.502557 1.092348 0.606194 11.00000 0.15460 0.07112 = 0.06379 0.02088 -0.00999 -0.01969 AFIX 43 H41 2 0.503876 1.163297 0.595792 11.00000 -1.20000 AFIX 0 C54 1 0.508220 0.652979 0.472694 11.00000 0.07056 0.14082 = 0.07980 0.03610 0.03488 0.02245 AFIX 43 H54 2 0.516966 0.599976 0.454814 11.00000 -1.20000 AFIX 0 C50 1 0.363758 0.912681 0.497675 11.00000 0.07283 0.11370 = 0.06785 0.04043 0.00272 -0.01226 AFIX 43 H50 2 0.381797 0.887347 0.477587 11.00000 -1.20000 AFIX 0 C36 1 0.515269 0.846039 0.772328 11.00000 0.12166 0.07426 = 0.05291 -0.01000 0.00675 -0.00816 AFIX 43 H36 2 0.529119 0.907933 0.787153 11.00000 -1.20000 AFIX 0 C55 1 0.541021 0.741531 0.483687 11.00000 0.05199 0.17384 = 0.09523 0.05928 0.02851 0.00464 AFIX 43 H55 2 0.572443 0.748016 0.473361 11.00000 -1.20000 AFIX 0 C62 1 0.272560 0.575236 0.449974 11.00000 0.05867 0.19608 = 0.04378 0.01552 0.00206 -0.03346 AFIX 43 H62 2 0.245210 0.599100 0.429182 11.00000 -1.20000 AFIX 0 C40 1 0.456098 1.053776 0.615799 11.00000 0.11738 0.07818 = 0.08416 0.01643 0.00256 0.02036 AFIX 43 H40 2 0.425914 1.098621 0.612350 11.00000 -1.20000 AFIX 0 C60 1 0.320765 0.429926 0.486954 11.00000 0.07500 0.13151 = 0.08989 -0.02427 0.01801 -0.02505 AFIX 43 H60 2 0.326700 0.354720 0.491034 11.00000 -1.20000 AFIX 0 C46 1 0.331242 0.884558 0.559191 11.00000 0.08344 0.11844 = 0.11013 0.05592 0.03927 0.03542 AFIX 43 H46 2 0.327027 0.839589 0.581038 11.00000 -1.20000 AFIX 0 C61 1 0.280779 0.466308 0.456579 11.00000 0.07031 0.19158 = 0.06024 -0.02191 0.01450 -0.04685 AFIX 43 H61 2 0.259025 0.415570 0.440305 11.00000 -1.20000 AFIX 0 C56 1 0.528521 0.820292 0.509450 11.00000 0.05739 0.16608 = 0.08999 0.03308 0.01536 -0.03368 AFIX 43 H56 2 0.551213 0.880230 0.516450 11.00000 -1.20000 AFIX 0 C49 1 0.342268 1.016346 0.494761 11.00000 0.08417 0.12940 = 0.12892 0.07716 0.00069 -0.00902 AFIX 43 H49 2 0.345573 1.061002 0.472616 11.00000 -1.20000 AFIX 0 C47 1 0.309751 0.988669 0.556532 11.00000 0.12183 0.15226 = 0.18034 0.07750 0.07365 0.06294 AFIX 43 H47 2 0.291274 1.013860 0.576378 11.00000 -1.20000 AFIX 0 C48 1 0.315738 1.055039 0.524452 11.00000 0.10539 0.12833 = 0.19832 0.08126 0.03890 0.03968 AFIX 43 H48 2 0.301914 1.126260 0.522668 11.00000 -1.20000 AFIX 0 HKLF 4 REM ds05_2_a.res in I2/a REM wR2 = 0.088182, GooF = S = 1.05956, Restrained GooF = 1.05956 for all data REM R1 = 0.036601 for 8224 Fo > 4sig(Fo) and 0.062794 for all 11513 data REM 569 parameters refined using 0 restraints END WGHT 0.0233 9.7283 REM Highest difference peak 0.445, deepest hole -0.397, 1-sigma level 0.051 Q1 1 0.4315 0.7041 0.6823 11.00000 0.05 0.44 Q2 1 0.3289 0.6064 0.6461 11.00000 0.05 0.43 Q3 1 0.4100 1.0527 0.6104 11.00000 0.05 0.40 Q4 1 0.4313 0.5875 0.6819 11.00000 0.05 0.35 Q5 1 0.3960 0.4240 0.6036 11.00000 0.05 0.35 Q6 1 0.2647 0.1517 0.6672 11.00000 0.05 0.31 Q7 1 0.3291 0.7359 0.5655 11.00000 0.05 0.31 Q8 1 0.4946 0.6891 0.5766 11.00000 0.05 0.31 Q9 1 0.5297 0.7156 0.6510 11.00000 0.05 0.29 Q10 1 0.4950 0.5995 0.5706 11.00000 0.05 0.29 Q11 1 0.4376 0.6384 0.6054 11.00000 0.05 0.29 Q12 1 0.4091 0.7466 0.6091 11.00000 0.05 0.29 Q13 1 0.3900 0.5848 0.5369 11.00000 0.05 0.29 ; _shelx_res_checksum 17130 _shelx_fab_file ; 0 0 -42 -0.0229 0.6159 0 0 -40 1.6406 0.0789 0 0 -38 1.7131 -0.6835 0 0 -36 -0.1143 -0.3667 0 0 -34 -1.4058 0.7239 0 0 -32 -0.8585 0.7265 0 0 -30 -0.4436 -0.7111 0 0 -28 -0.6444 -1.2911 0 0 -26 0.6755 0.2192 0 0 -24 2.3996 1.4688 0 0 -22 2.1308 0.3050 0 0 -20 1.1795 -1.4412 0 0 -18 -1.3526 -0.8406 0 0 -16 -6.4488 1.3870 0 0 -14 -3.4085 1.7494 0 0 -12 13.0803 -0.6577 0 0 -10 19.0630 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1.3827 -0.0112 30 3 -13 0.7944 0.0102 30 3 -11 -0.3627 0.0349 30 3 -9 -0.2440 0.0255 30 3 -7 1.3241 -0.0206 30 3 -5 0.9885 -0.0318 30 3 -3 -1.5306 0.0100 30 3 -1 -2.3840 0.0282 30 3 1 -1.1723 -0.0055 30 3 3 -0.4890 -0.0363 30 3 5 -0.2917 -0.0247 30 3 7 0.1209 0.0146 30 4 -20 0.5038 -0.0854 30 4 -18 -0.7151 -0.0117 30 4 -16 -0.8053 0.0916 30 4 -14 1.3647 0.0613 30 4 -12 0.9847 -0.0742 30 4 -10 -1.5211 -0.1142 30 4 -8 -1.6372 0.0274 30 4 -6 -0.0705 0.1432 30 4 -4 0.4662 0.0383 30 4 -2 0.3691 -0.1220 30 4 0 0.1482 -0.0729 30 4 2 -0.2497 0.1034 30 4 4 -0.0153 0.1177 30 4 6 0.4845 -0.0555 30 5 -17 0.9401 -0.0041 30 5 -15 -2.3328 -0.0016 30 5 -13 -4.0390 -0.0103 30 5 -11 0.3157 -0.0161 30 5 -9 2.4572 -0.0070 30 5 -7 -1.1635 0.0026 30 5 -5 -2.1191 0.0054 30 5 -3 1.5635 0.0035 30 5 -1 3.0129 -0.0018 30 5 1 1.1601 -0.0012 30 5 3 -0.1173 0.0082 30 6 -14 2.6225 -0.0289 30 6 -12 0.3059 0.0653 30 6 -10 -1.8998 0.0629 30 6 -8 0.2082 -0.0433 30 6 -6 1.8696 -0.0909 30 6 -4 -0.6502 -0.0017 30 6 -2 -2.1320 0.0896 30 6 0 -0.2753 0.0362 31 1 -22 -1.4010 0.0884 31 1 -20 -0.2135 0.0774 31 1 -18 2.1504 -0.0419 31 1 -16 2.6269 -0.0869 31 1 -14 -0.1287 0.0313 31 1 -12 -1.1513 0.1359 31 1 -10 1.3057 0.0324 31 1 -8 2.1568 -0.1446 31 1 -6 -0.0589 -0.1225 31 1 -4 -1.9701 0.0659 31 1 -2 -2.2883 0.1321 31 1 0 -0.5874 -0.0228 31 1 2 2.3638 -0.1541 31 1 4 2.0648 -0.0440 31 1 6 -1.5460 0.1415 31 2 -21 0.3943 0.0410 31 2 -19 1.1411 0.0129 31 2 -17 0.3391 -0.0314 31 2 -15 0.0048 -0.0226 31 2 -13 0.7174 0.0134 31 2 -11 0.7270 0.0281 31 2 -9 0.2506 0.0031 31 2 -7 0.1845 -0.0359 31 2 -5 -0.5158 -0.0261 31 2 -3 -1.3268 0.0235 31 2 -1 -0.6312 0.0248 31 2 1 -0.1100 -0.0263 31 2 3 -0.9471 -0.0394 31 2 5 -0.7948 0.0091 31 3 -18 -1.0218 0.0474 31 3 -16 -0.2290 0.0823 31 3 -14 1.6216 -0.0278 31 3 -12 0.6726 -0.1067 31 3 -10 -2.4632 -0.0214 31 3 -8 -2.3174 0.1161 31 3 -6 0.8260 0.0966 31 3 -4 1.9017 -0.0667 31 3 -2 0.2724 -0.1199 31 3 0 -1.1777 0.0368 31 3 2 -1.1429 0.1550 31 3 4 0.2551 0.0311 31 4 -17 -0.2420 0.0181 31 4 -15 -2.4560 0.0201 31 4 -13 -3.2258 -0.0124 31 4 -11 -0.0271 -0.0359 31 4 -9 1.6258 -0.0099 31 4 -7 -1.6985 0.0297 31 4 -5 -2.6494 0.0221 31 4 -3 2.1440 -0.0169 31 4 -1 4.9013 -0.0234 31 4 1 2.1976 0.0092 31 5 -12 0.1685 0.0976 31 5 -10 0.0907 0.0316 31 5 -8 0.8175 -0.0924 31 5 -6 1.2937 -0.0767 31 5 -4 0.0383 0.0601 31 5 -2 -1.2494 0.0966 32 0 -18 2.0541 -0.1074 32 0 -16 2.7900 -0.0141 32 0 -14 -0.5309 0.1177 32 0 -12 -1.6665 0.0673 32 0 -10 2.1130 -0.1059 32 0 -8 3.2389 -0.1395 32 0 -6 -0.6786 0.0226 32 0 -4 -3.3638 0.1283 32 0 -2 -2.7526 0.0163 32 0 0 -0.3755 -0.1259 32 0 2 2.9771 -0.0638 32 1 -17 -0.4137 -0.0332 32 1 -15 -0.7565 -0.0132 32 1 -13 0.9089 0.0192 32 1 -11 1.1539 0.0063 32 1 -9 -0.1333 -0.0324 32 1 -7 -0.6019 -0.0354 32 1 -5 -0.6988 0.0039 32 1 -3 -0.7753 0.0257 32 1 -1 0.2491 -0.0042 32 1 1 0.7333 -0.0338 32 2 -16 -0.2899 0.0038 32 2 -14 1.0284 -0.1078 32 2 -12 -0.0847 -0.0577 32 2 -10 -2.9079 0.1040 32 2 -8 -2.4779 0.1345 32 2 -6 1.5580 -0.0230 32 2 -4 3.6330 -0.1307 32 2 -2 1.4498 -0.0233 32 2 0 -1.7966 0.1313 32 3 -13 -1.4158 0.0005 32 3 -11 -0.5096 -0.0087 32 3 -9 0.2432 0.0048 32 3 -7 -1.1732 0.0227 32 3 -5 -1.4664 0.0074 32 3 -3 1.8207 -0.0235 0 0 0 0.0 0.0 ; _shelx_fab_checksum 90628 _olex2_submission_special_instructions 'No special instructions were received' _oxdiff_exptl_absorpt_empirical_details ; Empirical correction (ABSPACK) includes: - Absorption correction using spherical harmonics - Frame scaling ; _oxdiff_exptl_absorpt_empirical_full_max 1.051 _oxdiff_exptl_absorpt_empirical_full_min 0.958 loop_ _space_group_symop_operation_xyz 'x, y, z' '-x+1/2, y, -z' 'x+1/2, y+1/2, z+1/2' '-x+1, y+1/2, -z+1/2' '-x, -y, -z' 'x-1/2, -y, z' '-x+1/2, -y+1/2, -z+1/2' 'x, -y+1/2, z+1/2' 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 Ag1 Ag 0.41115(2) 0.64923(2) 0.61074(2) 0.05070(7) Uani 1 1 d . . . . . S21 S 0.32986(3) 0.69000(5) 0.64572(2) 0.04641(16) Uani 1 1 d . . . . . P31 P 0.49071(3) 0.73973(6) 0.65304(2) 0.04703(17) Uani 1 1 d . . . . . Cl44 Cl 0.43237(3) 0.44066(7) 0.61885(2) 0.0653(2) Uani 1 1 d . . . . . P51 P 0.38940(3) 0.70958(8) 0.53835(2) 0.0578(2) Uani 1 1 d . . . . . O8 O 0.30492(6) -0.09890(14) 0.74845(5) 0.0445(4) Uani 1 1 d . . . . . O23 O 0.22955(6) 0.04427(15) 0.73505(6) 0.0493(4) Uani 1 1 d . . . . . N11 N 0.32153(8) -0.24955(17) 0.82005(6) 0.0416(5) Uani 1 1 d . . . . . O14 O 0.35424(9) -0.2991(2) 0.90509(6) 0.0710(6) Uani 1 1 d . . . . . N22 N 0.26542(8) 0.57327(19) 0.68247(7) 0.0513(6) Uani 1 1 d . . . . . H22A H 0.254904 0.512775 0.691920 0.062 Uiso 1 1 calc R U . . . H22B H 0.248587 0.633758 0.684826 0.062 Uiso 1 1 calc R U . . . N19 N 0.33227(9) 0.47838(18) 0.66129(7) 0.0560(6) Uani 1 1 d . . . . . H19 H 0.359947 0.476783 0.649872 0.067 Uiso 1 1 calc R U . . . N18 N 0.31407(9) 0.38216(18) 0.67630(7) 0.0537(6) Uani 1 1 d . . . . . C6 C 0.31572(9) -0.0072(2) 0.72825(7) 0.0407(5) Uani 1 1 d . . . . . C20 C 0.30726(9) 0.5733(2) 0.66438(7) 0.0408(6) Uani 1 1 d . . . . . C7 C 0.27500(9) 0.0724(2) 0.72123(7) 0.0400(5) Uani 1 1 d . . . . . C32 C 0.49371(10) 0.7525(2) 0.70792(8) 0.0484(6) Uani 1 1 d . . . . . C10 C 0.32647(11) -0.2763(2) 0.77790(7) 0.0450(6) Uani 1 1 d . . . . . H10A H 0.291932 -0.301384 0.763257 0.054 Uiso 1 1 calc R U . . . H10B H 0.351437 -0.337066 0.778620 0.054 Uiso 1 1 calc R U . . . C9 C 0.34493(10) -0.1833(2) 0.75437(8) 0.0454(6) Uani 1 1 d . . . . . H9A H 0.378398 -0.153886 0.769349 0.055 Uiso 1 1 calc R U . . . H9B H 0.350916 -0.209780 0.728045 0.055 Uiso 1 1 calc R U . . . C38 C 0.49860(11) 0.8804(2) 0.63660(8) 0.0525(7) Uani 1 1 d . . . . . C2 C 0.28275(10) 0.1700(2) 0.70283(8) 0.0464(6) Uani 1 1 d . . . . . H2 H 0.255569 0.222385 0.698378 0.056 Uiso 1 1 calc R U . . . C3 C 0.33145(11) 0.1915(2) 0.69062(9) 0.0527(7) Uani 1 1 d . . . . . C25 C 0.55381(10) 0.6755(2) 0.64823(8) 0.0488(6) Uani 1 1 d . . . . . C24 C 0.18313(10) 0.1101(2) 0.72166(9) 0.0567(7) Uani 1 1 d . . . . . H24A H 0.176246 0.114828 0.692304 0.085 Uiso 1 1 calc R U . . . H24B H 0.188935 0.182780 0.733108 0.085 Uiso 1 1 calc R U . . . H24C H 0.152947 0.077087 0.730553 0.085 Uiso 1 1 calc R U . . . C30 C 0.59702(11) 0.6639(2) 0.67987(8) 0.0558(7) Uani 1 1 d . . . . . H30 H 0.594006 0.684405 0.706312 0.067 Uiso 1 1 calc R U . . . C5 C 0.36289(10) 0.0124(2) 0.71476(9) 0.0520(7) Uani 1 1 d . . . . . H5 H 0.389626 -0.040968 0.718159 0.062 Uiso 1 1 calc R U . . . C52 C 0.44818(11) 0.7221(3) 0.51448(8) 0.0656(9) Uani 1 1 d . . . . . C17 C 0.34318(12) 0.2980(2) 0.67438(10) 0.0625(8) Uani 1 1 d . . . . . H17 H 0.373067 0.304752 0.662156 0.075 Uiso 1 1 calc R U . . . C58 C 0.34553(11) 0.6169(3) 0.50488(8) 0.0654(9) Uani 1 1 d . . . . . C12 C 0.37261(11) -0.2125(3) 0.84381(8) 0.0571(7) Uani 1 1 d . . . . . H12A H 0.382233 -0.142246 0.833206 0.069 Uiso 1 1 calc R U . . . H12B H 0.400308 -0.265437 0.841051 0.069 Uiso 1 1 calc R U . . . C16 C 0.30436(12) -0.3487(2) 0.83887(8) 0.0561(7) Uani 1 1 d . . . . . H16A H 0.328467 -0.408916 0.835883 0.067 Uiso 1 1 calc R U . . . H16B H 0.268777 -0.369179 0.824789 0.067 Uiso 1 1 calc R U . . . C4 C 0.37035(11) 0.1116(2) 0.69616(10) 0.0601(8) Uani 1 1 d . . . . . H4 H 0.402353 0.124478 0.687227 0.072 Uiso 1 1 calc R U . . . C29 C 0.64474(12) 0.6219(3) 0.67244(10) 0.0661(8) Uani 1 1 d . . . . . H29 H 0.673665 0.614059 0.693973 0.079 Uiso 1 1 calc R U . . . C33 C 0.47371(12) 0.6678(3) 0.72793(9) 0.0642(8) Uani 1 1 d . . . . . H33 H 0.458437 0.606771 0.713254 0.077 Uiso 1 1 calc R U . . . C35 C 0.49674(13) 0.7614(3) 0.79162(10) 0.0704(9) Uani 1 1 d . . . . . H35 H 0.498134 0.764113 0.819774 0.085 Uiso 1 1 calc R U . . . C45 C 0.35881(12) 0.8450(3) 0.53044(10) 0.0701(9) Uani 1 1 d . . . . . C43 C 0.54526(13) 0.9221(3) 0.62686(10) 0.0706(9) Uani 1 1 d . . . . . H43 H 0.575878 0.878528 0.630551 0.085 Uiso 1 1 calc R U . . . C53 C 0.46163(12) 0.6432(3) 0.48859(10) 0.0754(10) Uani 1 1 d . . . . . H53 H 0.439354 0.582606 0.481619 0.090 Uiso 1 1 calc R U . . . C15 C 0.30371(13) -0.3314(3) 0.88355(9) 0.0684(9) Uani 1 1 d . . . . . H15A H 0.277577 -0.275042 0.886459 0.082 Uiso 1 1 calc R U . . . H15B H 0.293000 -0.399234 0.895208 0.082 Uiso 1 1 calc R U . . . C39 C 0.45402(14) 0.9478(3) 0.63068(10) 0.0717(9) Uani 1 1 d . . . . . H39 H 0.422097 0.921388 0.636807 0.086 Uiso 1 1 calc R U . . . C34 C 0.47615(14) 0.6727(3) 0.77000(10) 0.0738(9) Uani 1 1 d . . . . . H34 H 0.463393 0.613884 0.783374 0.089 Uiso 1 1 calc R U . . . C59 C 0.35252(13) 0.5058(4) 0.51172(10) 0.0784(10) Uani 1 1 d . . . . . H59 H 0.378777 0.481065 0.533150 0.094 Uiso 1 1 calc R U . . . C26 C 0.55909(12) 0.6412(3) 0.60961(9) 0.0715(9) Uani 1 1 d . . . . . H26 H 0.529855 0.645380 0.588160 0.086 Uiso 1 1 calc R U . . . C37 C 0.51394(15) 0.8420(3) 0.73049(10) 0.0757(10) Uani 1 1 d . . . . . H37 H 0.527041 0.901239 0.717573 0.091 Uiso 1 1 calc R U . . . C28 C 0.64989(13) 0.5917(3) 0.63391(10) 0.0727(9) Uani 1 1 d . . . . . H28 H 0.682381 0.564981 0.628986 0.087 Uiso 1 1 calc R U . . . C13 C 0.36935(14) -0.2001(3) 0.88828(9) 0.0735(9) Uani 1 1 d . . . . . H13A H 0.403931 -0.176891 0.903473 0.088 Uiso 1 1 calc R U . . . H13B H 0.343517 -0.143088 0.891105 0.088 Uiso 1 1 calc R U . . . C63 C 0.30449(12) 0.6515(4) 0.47388(9) 0.0796(11) Uani 1 1 d . . . . . H63 H 0.298462 0.726424 0.469190 0.096 Uiso 1 1 calc R U . . . C42 C 0.54684(19) 1.0278(3) 0.61173(12) 0.0918(12) Uani 1 1 d . . . . . H42 H 0.578468 1.054916 0.605285 0.110 Uiso 1 1 calc R U . . . C57 C 0.48225(13) 0.8115(4) 0.52522(10) 0.0869(12) Uani 1 1 d . . . . . H57 H 0.473839 0.865092 0.542999 0.104 Uiso 1 1 calc R U . . . C27 C 0.60685(14) 0.6011(3) 0.60244(10) 0.0845(11) Uani 1 1 d . . . . . H27 H 0.610072 0.580206 0.576084 0.101 Uiso 1 1 calc R U . . . C41 C 0.5026(2) 1.0923(3) 0.60619(11) 0.1004(14) Uani 1 1 d . . . . . H41 H 0.503876 1.163297 0.595792 0.121 Uiso 1 1 calc R U . . . C54 C 0.50822(15) 0.6530(4) 0.47269(12) 0.0944(13) Uani 1 1 d . . . . . H54 H 0.516966 0.599976 0.454814 0.113 Uiso 1 1 calc R U . . . C50 C 0.36376(14) 0.9127(4) 0.49768(11) 0.0861(12) Uani 1 1 d . . . . . H50 H 0.381797 0.887347 0.477587 0.103 Uiso 1 1 calc R U . . . C36 C 0.51527(16) 0.8460(3) 0.77233(10) 0.0842(11) Uani 1 1 d . . . . . H36 H 0.529119 0.907933 0.787153 0.101 Uiso 1 1 calc R U . . . C55 C 0.54102(15) 0.7415(5) 0.48369(14) 0.1051(17) Uani 1 1 d . . . . . H55 H 0.572443 0.748016 0.473361 0.126 Uiso 1 1 calc R U . . . C62 C 0.27256(15) 0.5752(5) 0.44997(11) 0.1005(16) Uani 1 1 d . . . . . H62 H 0.245210 0.599100 0.429182 0.121 Uiso 1 1 calc R U . . . C40 C 0.4561(2) 1.0538(3) 0.61580(12) 0.0953(12) Uani 1 1 d . . . . . H40 H 0.425914 1.098621 0.612350 0.114 Uiso 1 1 calc R U . . . C60 C 0.32077(15) 0.4299(4) 0.48695(13) 0.0985(13) Uani 1 1 d . . . . . H60 H 0.326700 0.354720 0.491034 0.118 Uiso 1 1 calc R U . . . C46 C 0.33124(15) 0.8846(4) 0.55919(13) 0.1013(14) Uani 1 1 d . . . . . H46 H 0.327027 0.839589 0.581038 0.122 Uiso 1 1 calc R U . . . C61 C 0.28078(17) 0.4663(5) 0.45658(12) 0.1071(17) Uani 1 1 d . . . . . H61 H 0.259025 0.415570 0.440305 0.128 Uiso 1 1 calc R U . . . C56 C 0.52852(15) 0.8203(4) 0.50945(13) 0.1043(16) Uani 1 1 d . . . . . H56 H 0.551213 0.880230 0.516450 0.125 Uiso 1 1 calc R U . . . C49 C 0.34227(18) 1.0163(4) 0.49476(16) 0.1167(18) Uani 1 1 d . . . . . H49 H 0.345573 1.061002 0.472616 0.140 Uiso 1 1 calc R U . . . C47 C 0.3098(2) 0.9887(5) 0.55653(18) 0.146(2) Uani 1 1 d . . . . . H47 H 0.291274 1.013860 0.576378 0.175 Uiso 1 1 calc R U . . . C48 C 0.3157(2) 1.0550(5) 0.5245(2) 0.143(2) Uani 1 1 d . . . . . H48 H 0.301914 1.126260 0.522668 0.171 Uiso 1 1 calc R U . . . 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 Ag1 0.04573(12) 0.06475(14) 0.04169(11) 0.00886(10) 0.00834(8) -0.00982(10) S21 0.0490(4) 0.0442(4) 0.0500(4) 0.0062(3) 0.0193(3) -0.0028(3) P31 0.0400(3) 0.0570(4) 0.0431(4) 0.0016(3) 0.0052(3) -0.0072(3) Cl44 0.0705(5) 0.0668(5) 0.0678(5) 0.0132(4) 0.0362(4) 0.0099(4) P51 0.0414(4) 0.0936(6) 0.0380(4) 0.0183(4) 0.0066(3) -0.0087(4) O8 0.0424(9) 0.0414(10) 0.0515(10) 0.0112(8) 0.0132(8) 0.0066(8) O23 0.0372(9) 0.0510(11) 0.0638(11) 0.0169(9) 0.0202(8) 0.0041(8) N11 0.0449(11) 0.0410(12) 0.0392(11) 0.0029(9) 0.0083(9) 0.0042(10) O14 0.0745(15) 0.0963(17) 0.0415(11) 0.0069(11) 0.0091(10) 0.0216(13) N22 0.0485(12) 0.0480(13) 0.0649(14) 0.0130(11) 0.0296(11) 0.0045(11) N19 0.0551(13) 0.0425(13) 0.0811(17) 0.0154(12) 0.0403(12) 0.0017(11) N18 0.0546(13) 0.0417(12) 0.0732(16) 0.0116(11) 0.0336(12) -0.0013(11) C6 0.0401(13) 0.0408(14) 0.0419(13) 0.0017(11) 0.0090(10) 0.0009(11) C20 0.0378(12) 0.0481(15) 0.0385(13) 0.0041(11) 0.0125(10) -0.0020(12) C7 0.0382(12) 0.0427(14) 0.0411(13) 0.0014(11) 0.0127(10) 0.0002(11) C32 0.0444(14) 0.0539(17) 0.0470(15) 0.0043(13) 0.0084(11) 0.0011(13) C10 0.0534(15) 0.0408(14) 0.0397(13) 0.0002(11) 0.0060(11) 0.0067(12) C9 0.0481(14) 0.0475(15) 0.0423(14) 0.0052(11) 0.0125(11) 0.0112(12) C38 0.0547(16) 0.0579(18) 0.0423(14) 0.0016(13) 0.0024(12) -0.0084(14) C2 0.0448(14) 0.0408(15) 0.0575(16) 0.0070(12) 0.0200(12) 0.0053(12) C3 0.0552(16) 0.0421(15) 0.0683(18) 0.0075(13) 0.0310(14) 0.0003(13) C25 0.0413(14) 0.0563(17) 0.0472(15) -0.0003(12) 0.0044(11) -0.0037(13) C24 0.0389(14) 0.0594(18) 0.0733(19) 0.0079(15) 0.0144(13) 0.0063(14) C30 0.0521(16) 0.0677(19) 0.0453(15) -0.0012(14) 0.0032(12) -0.0022(15) C5 0.0440(14) 0.0461(15) 0.0705(18) 0.0063(14) 0.0226(13) 0.0092(13) C52 0.0437(15) 0.112(3) 0.0394(15) 0.0267(17) 0.0045(12) -0.0095(18) C17 0.0595(18) 0.0518(17) 0.088(2) 0.0126(16) 0.0434(16) 0.0015(15) C58 0.0421(15) 0.113(3) 0.0427(15) 0.0098(17) 0.0116(12) -0.0139(18) C12 0.0557(17) 0.069(2) 0.0468(15) -0.0031(14) 0.0086(12) -0.0033(15) C16 0.0639(18) 0.0524(17) 0.0519(16) 0.0087(14) 0.0105(13) -0.0017(15) C4 0.0495(16) 0.0529(17) 0.087(2) 0.0107(16) 0.0370(15) 0.0045(14) C29 0.0506(17) 0.079(2) 0.0631(19) 0.0038(17) -0.0029(14) 0.0102(16) C33 0.0691(19) 0.065(2) 0.0601(19) 0.0021(15) 0.0160(15) -0.0092(16) C35 0.069(2) 0.093(3) 0.0506(18) 0.0035(19) 0.0151(15) 0.018(2) C45 0.0476(16) 0.101(3) 0.0594(18) 0.0307(18) 0.0033(14) -0.0030(17) C43 0.064(2) 0.074(2) 0.070(2) 0.0069(17) 0.0045(16) -0.0208(18) C53 0.0543(18) 0.114(3) 0.0609(19) 0.030(2) 0.0188(15) 0.0058(19) C15 0.076(2) 0.079(2) 0.0557(18) 0.0169(16) 0.0254(16) 0.0110(18) C39 0.076(2) 0.072(2) 0.067(2) 0.0130(18) 0.0127(17) 0.0042(19) C34 0.077(2) 0.085(3) 0.065(2) 0.0176(19) 0.0279(17) -0.001(2) C59 0.0552(19) 0.118(3) 0.061(2) -0.003(2) 0.0088(15) -0.014(2) C26 0.0569(18) 0.107(3) 0.0467(16) -0.0087(17) -0.0009(13) 0.0132(19) C37 0.111(3) 0.064(2) 0.0503(18) 0.0012(16) 0.0100(17) -0.022(2) C28 0.0581(19) 0.088(2) 0.073(2) -0.0021(19) 0.0155(16) 0.0193(18) C13 0.076(2) 0.093(3) 0.0492(18) -0.0142(18) 0.0057(15) -0.003(2) C63 0.0515(17) 0.142(3) 0.0444(16) 0.024(2) 0.0052(13) -0.018(2) C42 0.111(3) 0.084(3) 0.076(3) 0.015(2) 0.007(2) -0.045(3) C57 0.061(2) 0.143(4) 0.057(2) 0.015(2) 0.0119(15) -0.029(2) C27 0.076(2) 0.121(3) 0.057(2) -0.013(2) 0.0145(17) 0.024(2) C41 0.155(4) 0.071(3) 0.064(2) 0.021(2) -0.010(3) -0.020(3) C54 0.071(2) 0.141(4) 0.080(2) 0.036(3) 0.035(2) 0.022(3) C50 0.073(2) 0.114(3) 0.068(2) 0.040(2) 0.0027(17) -0.012(2) C36 0.122(3) 0.074(2) 0.0529(19) -0.0100(18) 0.0067(19) -0.008(2) C55 0.052(2) 0.174(5) 0.095(3) 0.059(3) 0.029(2) 0.005(3) C62 0.059(2) 0.196(5) 0.0438(19) 0.016(3) 0.0021(15) -0.033(3) C40 0.117(3) 0.078(3) 0.084(3) 0.016(2) 0.003(2) 0.020(3) C60 0.075(2) 0.132(4) 0.090(3) -0.024(3) 0.018(2) -0.025(3) C46 0.083(3) 0.118(3) 0.110(3) 0.056(3) 0.039(2) 0.035(3) C61 0.070(3) 0.192(5) 0.060(2) -0.022(3) 0.015(2) -0.047(3) C56 0.057(2) 0.166(5) 0.090(3) 0.033(3) 0.015(2) -0.034(3) C49 0.084(3) 0.129(4) 0.129(4) 0.077(3) 0.001(3) -0.009(3) C47 0.122(4) 0.152(5) 0.180(6) 0.078(4) 0.074(4) 0.063(4) C48 0.105(4) 0.128(4) 0.198(6) 0.081(5) 0.039(4) 0.040(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' Ag Ag -0.8971 1.1015 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Cl Cl 0.1484 0.1585 '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' P P 0.1023 0.0942 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' S S 0.1246 0.1234 '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 _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag P31 Ag1 S21 107.06(2) . . ? P31 Ag1 Cl44 103.89(3) . . ? Cl44 Ag1 S21 107.86(2) . . ? P51 Ag1 S21 109.04(2) . . ? P51 Ag1 P31 115.35(3) . . ? P51 Ag1 Cl44 113.21(3) . . ? C20 S21 Ag1 111.00(9) . . ? C32 P31 Ag1 118.73(9) . . ? C38 P31 Ag1 111.60(9) . . ? C38 P31 C32 103.66(13) . . ? C38 P31 C25 103.14(13) . . ? C25 P31 Ag1 113.49(9) . . ? C25 P31 C32 104.63(12) . . ? C52 P51 Ag1 113.26(9) . . ? C58 P51 Ag1 114.41(11) . . ? C58 P51 C52 104.19(15) . . ? C58 P51 C45 105.93(16) . . ? C45 P51 Ag1 114.83(11) . . ? C45 P51 C52 103.02(15) . . ? C6 O8 C9 116.82(18) . . ? C7 O23 C24 117.33(19) . . ? C12 N11 C10 111.0(2) . . ? C12 N11 C16 109.2(2) . . ? C16 N11 C10 108.3(2) . . ? C15 O14 C13 109.1(2) . . ? H22A N22 H22B 120.0 . . ? C20 N22 H22A 120.0 . . ? C20 N22 H22B 120.0 . . ? N18 N19 H19 119.8 . . ? C20 N19 H19 119.8 . . ? C20 N19 N18 120.4(2) . . ? C17 N18 N19 115.0(2) . . ? O8 C6 C7 115.8(2) . . ? O8 C6 C5 125.0(2) . . ? C5 C6 C7 119.2(2) . . ? N22 C20 S21 121.8(2) . . ? N22 C20 N19 118.4(2) . . ? N19 C20 S21 119.80(17) . . ? O23 C7 C6 114.7(2) . . ? C2 C7 O23 124.8(2) . . ? C2 C7 C6 120.5(2) . . ? C33 C32 P31 118.2(2) . . ? C37 C32 P31 124.0(2) . . ? C37 C32 C33 117.7(3) . . ? N11 C10 H10A 108.5 . . ? N11 C10 H10B 108.5 . . ? N11 C10 C9 115.1(2) . . ? H10A C10 H10B 107.5 . . ? C9 C10 H10A 108.5 . . ? C9 C10 H10B 108.5 . . ? O8 C9 C10 109.0(2) . . ? O8 C9 H9A 109.9 . . ? O8 C9 H9B 109.9 . . ? C10 C9 H9A 109.9 . . ? C10 C9 H9B 109.9 . . ? H9A C9 H9B 108.3 . . ? C43 C38 P31 124.2(2) . . ? C39 C38 P31 117.7(2) . . ? C39 C38 C43 117.9(3) . . ? C7 C2 H2 119.9 . . ? C7 C2 C3 120.1(2) . . ? C3 C2 H2 119.9 . . ? C2 C3 C17 121.9(3) . . ? C4 C3 C2 119.0(2) . . ? C4 C3 C17 119.0(2) . . ? C30 C25 P31 124.6(2) . . ? C30 C25 C26 118.5(3) . . ? C26 C25 P31 116.9(2) . . ? O23 C24 H24A 109.5 . . ? O23 C24 H24B 109.5 . . ? O23 C24 H24C 109.5 . . ? H24A C24 H24B 109.5 . . ? H24A C24 H24C 109.5 . . ? H24B C24 H24C 109.5 . . ? C25 C30 H30 119.9 . . ? C25 C30 C29 120.2(3) . . ? C29 C30 H30 119.9 . . ? C6 C5 H5 120.1 . . ? C6 C5 C4 119.8(2) . . ? C4 C5 H5 120.1 . . ? C53 C52 P51 122.3(3) . . ? C53 C52 C57 119.2(3) . . ? C57 C52 P51 118.3(3) . . ? N18 C17 C3 122.3(2) . . ? N18 C17 H17 118.8 . . ? C3 C17 H17 118.8 . . ? C59 C58 P51 117.5(2) . . ? C59 C58 C63 118.4(3) . . ? C63 C58 P51 124.1(3) . . ? N11 C12 H12A 109.5 . . ? N11 C12 H12B 109.5 . . ? N11 C12 C13 110.8(2) . . ? H12A C12 H12B 108.1 . . ? C13 C12 H12A 109.5 . . ? C13 C12 H12B 109.5 . . ? N11 C16 H16A 109.3 . . ? N11 C16 H16B 109.3 . . ? N11 C16 C15 111.6(2) . . ? H16A C16 H16B 108.0 . . ? C15 C16 H16A 109.3 . . ? C15 C16 H16B 109.3 . . ? C3 C4 C5 121.2(2) . . ? C3 C4 H4 119.4 . . ? C5 C4 H4 119.4 . . ? C30 C29 H29 119.7 . . ? C28 C29 C30 120.7(3) . . ? C28 C29 H29 119.7 . . ? C32 C33 H33 119.8 . . ? C32 C33 C34 120.3(3) . . ? C34 C33 H33 119.8 . . ? C34 C35 H35 120.2 . . ? C36 C35 H35 120.2 . . ? C36 C35 C34 119.6(3) . . ? C50 C45 P51 123.3(3) . . ? C46 C45 P51 118.4(3) . . ? C46 C45 C50 118.2(4) . . ? C38 C43 H43 119.7 . . ? C42 C43 C38 120.6(4) . . ? C42 C43 H43 119.7 . . ? C52 C53 H53 119.7 . . ? C52 C53 C54 120.6(4) . . ? C54 C53 H53 119.7 . . ? O14 C15 C16 111.4(2) . . ? O14 C15 H15A 109.4 . . ? O14 C15 H15B 109.4 . . ? C16 C15 H15A 109.4 . . ? C16 C15 H15B 109.4 . . ? H15A C15 H15B 108.0 . . ? C38 C39 H39 119.5 . . ? C38 C39 C40 121.1(4) . . ? C40 C39 H39 119.5 . . ? C33 C34 H34 119.6 . . ? C35 C34 C33 120.8(3) . . ? C35 C34 H34 119.6 . . ? C58 C59 H59 119.7 . . ? C58 C59 C60 120.6(4) . . ? C60 C59 H59 119.7 . . ? C25 C26 H26 119.6 . . ? C27 C26 C25 120.8(3) . . ? C27 C26 H26 119.6 . . ? C32 C37 H37 119.5 . . ? C32 C37 C36 121.1(3) . . ? C36 C37 H37 119.5 . . ? C29 C28 H28 120.3 . . ? C29 C28 C27 119.5(3) . . ? C27 C28 H28 120.3 . . ? O14 C13 C12 112.0(3) . . ? O14 C13 H13A 109.2 . . ? O14 C13 H13B 109.2 . . ? C12 C13 H13A 109.2 . . ? C12 C13 H13B 109.2 . . ? H13A C13 H13B 107.9 . . ? C58 C63 H63 119.8 . . ? C62 C63 C58 120.3(4) . . ? C62 C63 H63 119.8 . . ? C43 C42 H42 119.8 . . ? C41 C42 C43 120.4(4) . . ? C41 C42 H42 119.8 . . ? C52 C57 H57 120.1 . . ? C56 C57 C52 119.8(4) . . ? C56 C57 H57 120.1 . . ? C26 C27 H27 119.8 . . ? C28 C27 C26 120.3(3) . . ? C28 C27 H27 119.8 . . ? C42 C41 H41 119.8 . . ? C42 C41 C40 120.3(4) . . ? C40 C41 H41 119.8 . . ? C53 C54 H54 120.4 . . ? C55 C54 C53 119.1(4) . . ? C55 C54 H54 120.4 . . ? C45 C50 H50 119.8 . . ? C49 C50 C45 120.4(4) . . ? C49 C50 H50 119.8 . . ? C35 C36 C37 120.5(3) . . ? C35 C36 H36 119.7 . . ? C37 C36 H36 119.7 . . ? C54 C55 H55 119.4 . . ? C56 C55 C54 121.2(4) . . ? C56 C55 H55 119.4 . . ? C63 C62 H62 119.8 . . ? C61 C62 C63 120.4(4) . . ? C61 C62 H62 119.8 . . ? C39 C40 H40 120.1 . . ? C41 C40 C39 119.7(4) . . ? C41 C40 H40 120.1 . . ? C59 C60 H60 120.2 . . ? C61 C60 C59 119.6(5) . . ? C61 C60 H60 120.2 . . ? C45 C46 H46 119.1 . . ? C47 C46 C45 121.7(4) . . ? C47 C46 H46 119.1 . . ? C62 C61 C60 120.5(5) . . ? C62 C61 H61 119.7 . . ? C60 C61 H61 119.7 . . ? C57 C56 H56 119.9 . . ? C55 C56 C57 120.1(4) . . ? C55 C56 H56 119.9 . . ? C50 C49 H49 119.8 . . ? C50 C49 C48 120.4(4) . . ? C48 C49 H49 119.8 . . ? C46 C47 H47 120.3 . . ? C48 C47 C46 119.4(5) . . ? C48 C47 H47 120.3 . . ? C49 C48 H48 120.0 . . ? C47 C48 C49 119.9(5) . . ? C47 C48 H48 120.0 . . ? 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 Ag1 S21 2.6013(7) . ? Ag1 P31 2.4917(7) . ? Ag1 Cl44 2.5892(8) . ? Ag1 P51 2.4759(7) . ? S21 C20 1.688(3) . ? P31 C32 1.818(3) . ? P31 C38 1.814(3) . ? P31 C25 1.817(3) . ? P51 C52 1.825(3) . ? P51 C58 1.811(3) . ? P51 C45 1.815(4) . ? O8 C6 1.353(3) . ? O8 C9 1.431(3) . ? O23 C7 1.364(3) . ? O23 C24 1.425(3) . ? N11 C10 1.466(3) . ? N11 C12 1.459(3) . ? N11 C16 1.459(3) . ? O14 C15 1.404(4) . ? O14 C13 1.407(4) . ? N22 H22A 0.8600 . ? N22 H22B 0.8600 . ? N22 C20 1.316(3) . ? N19 H19 0.8600 . ? N19 N18 1.382(3) . ? N19 C20 1.328(3) . ? N18 C17 1.269(3) . ? C6 C7 1.402(3) . ? C6 C5 1.377(3) . ? C7 C2 1.363(3) . ? C32 C33 1.371(4) . ? C32 C37 1.364(4) . ? C10 H10A 0.9700 . ? C10 H10B 0.9700 . ? C10 C9 1.496(3) . ? C9 H9A 0.9700 . ? C9 H9B 0.9700 . ? C38 C43 1.383(4) . ? C38 C39 1.381(4) . ? C2 H2 0.9300 . ? C2 C3 1.398(3) . ? C3 C17 1.452(4) . ? C3 C4 1.372(4) . ? C25 C30 1.378(4) . ? C25 C26 1.379(4) . ? C24 H24A 0.9600 . ? C24 H24B 0.9600 . ? C24 H24C 0.9600 . ? C30 H30 0.9300 . ? C30 C29 1.380(4) . ? C5 H5 0.9300 . ? C5 C4 1.381(4) . ? C52 C53 1.372(5) . ? C52 C57 1.391(5) . ? C17 H17 0.9300 . ? C58 C59 1.372(5) . ? C58 C63 1.387(4) . ? C12 H12A 0.9700 . ? C12 H12B 0.9700 . ? C12 C13 1.503(4) . ? C16 H16A 0.9700 . ? C16 H16B 0.9700 . ? C16 C15 1.503(4) . ? C4 H4 0.9300 . ? C29 H29 0.9300 . ? C29 C28 1.361(4) . ? C33 H33 0.9300 . ? C33 C34 1.389(4) . ? C35 H35 0.9300 . ? C35 C34 1.344(5) . ? C35 C36 1.341(5) . ? C45 C50 1.387(4) . ? C45 C46 1.373(5) . ? C43 H43 0.9300 . ? C43 C42 1.380(5) . ? C53 H53 0.9300 . ? C53 C54 1.390(4) . ? C15 H15A 0.9700 . ? C15 H15B 0.9700 . ? C39 H39 0.9300 . ? C39 C40 1.381(5) . ? C34 H34 0.9300 . ? C59 H59 0.9300 . ? C59 C60 1.388(5) . ? C26 H26 0.9300 . ? C26 C27 1.370(4) . ? C37 H37 0.9300 . ? C37 C36 1.385(4) . ? C28 H28 0.9300 . ? C28 C27 1.370(4) . ? C13 H13A 0.9700 . ? C13 H13B 0.9700 . ? C63 H63 0.9300 . ? C63 C62 1.379(5) . ? C42 H42 0.9300 . ? C42 C41 1.355(6) . ? C57 H57 0.9300 . ? C57 C56 1.379(5) . ? C27 H27 0.9300 . ? C41 H41 0.9300 . ? C41 C40 1.363(6) . ? C54 H54 0.9300 . ? C54 C55 1.367(6) . ? C50 H50 0.9300 . ? C50 C49 1.367(6) . ? C36 H36 0.9300 . ? C55 H55 0.9300 . ? C55 C56 1.359(6) . ? C62 H62 0.9300 . ? C62 C61 1.349(6) . ? C40 H40 0.9300 . ? C60 H60 0.9300 . ? C60 C61 1.365(6) . ? C46 H46 0.9300 . ? C46 C47 1.372(6) . ? C61 H61 0.9300 . ? C56 H56 0.9300 . ? C49 H49 0.9300 . ? C49 C48 1.378(7) . ? C47 H47 0.9300 . ? C47 C48 1.367(6) . ? C48 H48 0.9300 . ? 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 _geom_torsion_site_symmetry_1 _geom_torsion_site_symmetry_2 _geom_torsion_site_symmetry_3 _geom_torsion_site_symmetry_4 _geom_torsion_publ_flag Ag1 S21 C20 N22 -178.18(18) . . . . ? Ag1 S21 C20 N19 2.4(2) . . . . ? Ag1 P31 C32 C33 36.7(3) . . . . ? Ag1 P31 C32 C37 -142.2(2) . . . . ? Ag1 P31 C38 C43 -127.1(2) . . . . ? Ag1 P31 C38 C39 48.1(3) . . . . ? Ag1 P31 C25 C30 -143.4(2) . . . . ? Ag1 P31 C25 C26 39.9(3) . . . . ? Ag1 P51 C52 C53 101.5(2) . . . . ? Ag1 P51 C52 C57 -74.1(3) . . . . ? Ag1 P51 C58 C59 -37.6(3) . . . . ? Ag1 P51 C58 C63 140.2(2) . . . . ? Ag1 P51 C45 C50 152.0(3) . . . . ? Ag1 P51 C45 C46 -25.2(3) . . . . ? P31 C32 C33 C34 178.6(2) . . . . ? P31 C32 C37 C36 -179.7(3) . . . . ? P31 C38 C43 C42 175.2(3) . . . . ? P31 C38 C39 C40 -176.0(3) . . . . ? P31 C25 C30 C29 -174.8(2) . . . . ? P31 C25 C26 C27 174.1(3) . . . . ? P51 C52 C53 C54 -176.6(2) . . . . ? P51 C52 C57 C56 176.5(3) . . . . ? P51 C58 C59 C60 -179.2(3) . . . . ? P51 C58 C63 C62 -179.4(2) . . . . ? P51 C45 C50 C49 -176.3(3) . . . . ? P51 C45 C46 C47 176.1(4) . . . . ? O8 C6 C7 O23 -1.5(3) . . . . ? O8 C6 C7 C2 177.0(2) . . . . ? O8 C6 C5 C4 -176.9(3) . . . . ? O23 C7 C2 C3 178.5(2) . . . . ? N11 C10 C9 O8 -65.8(3) . . . . ? N11 C12 C13 O14 57.7(4) . . . . ? N11 C16 C15 O14 -57.6(3) . . . . ? N19 N18 C17 C3 176.9(3) . . . . ? N18 N19 C20 S21 -179.8(2) . . . . ? N18 N19 C20 N22 0.8(4) . . . . ? C6 O8 C9 C10 178.8(2) . . . . ? C6 C7 C2 C3 0.2(4) . . . . ? C6 C5 C4 C3 -0.3(5) . . . . ? C20 N19 N18 C17 -175.1(3) . . . . ? C7 C6 C5 C4 2.7(4) . . . . ? C7 C2 C3 C17 -174.2(3) . . . . ? C7 C2 C3 C4 2.2(4) . . . . ? C32 P31 C38 C43 104.0(3) . . . . ? C32 P31 C38 C39 -80.8(2) . . . . ? C32 P31 C25 C30 -12.5(3) . . . . ? C32 P31 C25 C26 170.8(2) . . . . ? C32 C33 C34 C35 1.8(5) . . . . ? C32 C37 C36 C35 0.2(6) . . . . ? C10 N11 C12 C13 -172.2(2) . . . . ? C10 N11 C16 C15 174.2(2) . . . . ? C9 O8 C6 C7 177.3(2) . . . . ? C9 O8 C6 C5 -3.0(4) . . . . ? C38 P31 C32 C33 161.2(2) . . . . ? C38 P31 C32 C37 -17.8(3) . . . . ? C38 P31 C25 C30 95.7(3) . . . . ? C38 P31 C25 C26 -81.0(3) . . . . ? C38 C43 C42 C41 0.0(6) . . . . ? C38 C39 C40 C41 1.0(6) . . . . ? C2 C3 C17 N18 11.4(5) . . . . ? C2 C3 C4 C5 -2.2(5) . . . . ? C25 P31 C32 C33 -91.1(2) . . . . ? C25 P31 C32 C37 90.0(3) . . . . ? C25 P31 C38 C43 -4.9(3) . . . . ? C25 P31 C38 C39 170.3(2) . . . . ? C25 C30 C29 C28 0.2(5) . . . . ? C25 C26 C27 C28 1.7(6) . . . . ? C24 O23 C7 C6 -167.4(2) . . . . ? C24 O23 C7 C2 14.2(4) . . . . ? C30 C25 C26 C27 -2.9(5) . . . . ? C30 C29 C28 C27 -1.4(6) . . . . ? C5 C6 C7 O23 178.8(2) . . . . ? C5 C6 C7 C2 -2.7(4) . . . . ? C52 P51 C58 C59 86.6(3) . . . . ? C52 P51 C58 C63 -95.6(3) . . . . ? C52 P51 C45 C50 28.4(3) . . . . ? C52 P51 C45 C46 -148.8(3) . . . . ? C52 C53 C54 C55 1.0(5) . . . . ? C52 C57 C56 C55 -0.5(6) . . . . ? C17 C3 C4 C5 174.4(3) . . . . ? C58 P51 C52 C53 -23.4(3) . . . . ? C58 P51 C52 C57 161.0(3) . . . . ? C58 P51 C45 C50 -80.7(3) . . . . ? C58 P51 C45 C46 102.1(3) . . . . ? C58 C59 C60 C61 -2.7(5) . . . . ? C58 C63 C62 C61 0.2(6) . . . . ? C12 N11 C10 C9 -59.0(3) . . . . ? C12 N11 C16 C15 53.3(3) . . . . ? C16 N11 C10 C9 -178.8(2) . . . . ? C16 N11 C12 C13 -52.9(3) . . . . ? C4 C3 C17 N18 -165.1(3) . . . . ? C29 C28 C27 C26 0.4(6) . . . . ? C33 C32 C37 C36 1.4(5) . . . . ? C45 P51 C52 C53 -133.8(3) . . . . ? C45 P51 C52 C57 50.6(3) . . . . ? C45 P51 C58 C59 -165.1(2) . . . . ? C45 P51 C58 C63 12.7(3) . . . . ? C45 C50 C49 C48 0.4(7) . . . . ? C45 C46 C47 C48 0.1(9) . . . . ? C43 C38 C39 C40 -0.5(5) . . . . ? C43 C42 C41 C40 0.5(6) . . . . ? C53 C52 C57 C56 0.8(5) . . . . ? C53 C54 C55 C56 -0.7(6) . . . . ? C15 O14 C13 C12 -60.0(3) . . . . ? C39 C38 C43 C42 0.0(5) . . . . ? C34 C35 C36 C37 -0.8(6) . . . . ? C59 C58 C63 C62 -1.7(5) . . . . ? C59 C60 C61 C62 1.2(6) . . . . ? C26 C25 C30 C29 1.9(5) . . . . ? C37 C32 C33 C34 -2.4(5) . . . . ? C13 O14 C15 C16 59.5(3) . . . . ? C63 C58 C59 C60 2.9(5) . . . . ? C63 C62 C61 C60 0.0(6) . . . . ? C42 C41 C40 C39 -0.9(6) . . . . ? C57 C52 C53 C54 -1.1(5) . . . . ? C54 C55 C56 C57 0.4(6) . . . . ? C50 C45 C46 C47 -1.2(7) . . . . ? C50 C49 C48 C47 -1.5(9) . . . . ? C36 C35 C34 C33 -0.2(5) . . . . ? C46 C45 C50 C49 0.9(6) . . . . ? C46 C47 C48 C49 1.2(9) . . . . ? loop_ _smtbx_masks_void_nr _smtbx_masks_void_average_x _smtbx_masks_void_average_y _smtbx_masks_void_average_z _smtbx_masks_void_volume _smtbx_masks_void_count_electrons _smtbx_masks_void_content 1 0.241 0.200 0.589 94.4 5.9 '0.25 acetonitrile' 2 0.241 0.300 0.089 94.4 5.9 '0.25 acetonitrile' 3 0.259 0.200 0.411 94.4 5.5 '0.25 acetonitrile' 4 0.259 0.300 0.911 94.4 5.5 '0.25 acetonitrile' 5 0.741 0.700 0.089 94.4 5.9 '0.25 acetonitrile' 6 0.741 0.800 0.589 94.4 5.9 '0.25 acetonitrile' 7 0.759 0.700 0.911 94.4 5.5 '0.25 acetonitrile' 8 0.759 0.800 0.411 94.4 5.5 '0.25 acetonitrile'