#------------------------------------------------------------------------------ #$Date: 2019-11-08 04:15:30 +0200 (Fri, 08 Nov 2019) $ #$Revision: 225338 $ #$URL: file:///home/coder/svn-repositories/cod/cif/1/55/03/1550338.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_1550338 loop_ _publ_author_name 'Xia, Jian' 'Zhang, Yixin' 'Hu, Xiaoqiang' 'Ma, Xin' 'Cui, Lei' 'Zhang, Jianfu' 'Jian, Zhongbao' _publ_section_title ; Sterically very bulky aliphatic/aromatic phosphine-sulfonate palladium catalysts for ethylene polymerization and copolymerization with polar monomers ; _journal_issue 4 _journal_name_full 'Polymer Chemistry' _journal_page_first 546 _journal_paper_doi 10.1039/C8PY01568F _journal_volume 10 _journal_year 2019 _chemical_absolute_configuration ad _chemical_formula_sum 'C34 H38 F2 N O3 P Pd S' _chemical_formula_weight 716.08 _space_group_crystal_system orthorhombic _space_group_IT_number 19 _space_group_name_Hall 'P 2ac 2ab' _space_group_name_H-M_alt 'P 21 21 21' _symmetry_space_group_name_Hall 'P 2ac 2ab' _symmetry_space_group_name_H-M 'P 21 21 21' _atom_sites_solution_hydrogens geom _audit_creation_method SHELXL-2014/7 _audit_update_record ; 2018-09-29 deposited with the CCDC. 2018-12-06 downloaded from the CCDC. ; _cell_angle_alpha 90 _cell_angle_beta 90 _cell_angle_gamma 90 _cell_formula_units_Z 4 _cell_length_a 9.1697(6) _cell_length_b 9.5203(6) _cell_length_c 36.333(2) _cell_measurement_reflns_used 2276 _cell_measurement_temperature 185(2) _cell_measurement_theta_max 19.6671 _cell_measurement_theta_min 2.2114 _cell_volume 3171.8(3) _computing_cell_refinement 'Bruker SMART' _computing_data_collection 'Bruker SMART' _computing_data_reduction 'Bruker SAINT' _computing_molecular_graphics 'Bruker SHELXTL' _computing_publication_material 'Bruker SHELXTL' _computing_structure_refinement 'Bruker SHELXTL' _computing_structure_solution 'Bruker SHELXTL' _diffrn_ambient_temperature 185(2) _diffrn_measured_fraction_theta_full 1.000 _diffrn_measured_fraction_theta_max 1.000 _diffrn_measurement_device_type 'CCD area detector' _diffrn_measurement_method 'phi and omega scans' _diffrn_radiation_monochromator graphite _diffrn_radiation_source 'sealed tube' _diffrn_radiation_type MoK\a _diffrn_radiation_wavelength 0.71073 _diffrn_reflns_av_R_equivalents 0.0751 _diffrn_reflns_av_unetI/netI 0.0869 _diffrn_reflns_Laue_measured_fraction_full 1.000 _diffrn_reflns_Laue_measured_fraction_max 1.000 _diffrn_reflns_limit_h_max 10 _diffrn_reflns_limit_h_min -10 _diffrn_reflns_limit_k_max 11 _diffrn_reflns_limit_k_min -11 _diffrn_reflns_limit_l_max 22 _diffrn_reflns_limit_l_min -43 _diffrn_reflns_number 16352 _diffrn_reflns_point_group_measured_fraction_full 1.000 _diffrn_reflns_point_group_measured_fraction_max 1.000 _diffrn_reflns_theta_full 25.000 _diffrn_reflns_theta_max 25.000 _diffrn_reflns_theta_min 2.211 _exptl_absorpt_coefficient_mu 0.749 _exptl_absorpt_correction_type none _exptl_crystal_colour transparent _exptl_crystal_density_diffrn 1.500 _exptl_crystal_description plate _exptl_crystal_F_000 1472 _exptl_crystal_size_max 0.310 _exptl_crystal_size_mid 0.200 _exptl_crystal_size_min 0.050 _refine_diff_density_max 0.674 _refine_diff_density_min -0.412 _refine_diff_density_rms 0.085 _refine_ls_abs_structure_details ; Flack x determined using 1553 quotients [(I+)-(I-)]/[(I+)+(I-)] (Parsons, Flack and Wagner, Acta Cryst. B69 (2013) 249-259). ; _refine_ls_abs_structure_Flack -0.03(3) _refine_ls_extinction_method none _refine_ls_goodness_of_fit_ref 0.964 _refine_ls_hydrogen_treatment 'riding mode' _refine_ls_matrix_type full _refine_ls_number_parameters 388 _refine_ls_number_reflns 5595 _refine_ls_number_restraints 0 _refine_ls_restrained_S_all 0.964 _refine_ls_R_factor_all 0.0662 _refine_ls_R_factor_gt 0.0468 _refine_ls_shift/su_max 0.000 _refine_ls_shift/su_mean 0.000 _refine_ls_structure_factor_coef Fsqd _refine_ls_weighting_details 'w=1/[\s^2^(Fo^2^)+(0.0369P)^2^] where P=(Fo^2^+2Fc^2^)/3' _refine_ls_weighting_scheme calc _refine_ls_wR_factor_gt 0.0837 _refine_ls_wR_factor_ref 0.0898 _reflns_Friedel_coverage 0.745 _reflns_Friedel_fraction_full 1.000 _reflns_Friedel_fraction_max 1.000 _reflns_number_gt 4534 _reflns_number_total 5595 _reflns_threshold_expression 'I > 2\s(I)' _cod_data_source_file c8py01568f2.cif _cod_data_source_block 1 _cod_depositor_comments 'Adding full bibliography for 1550337--1550338.cif.' _cod_original_cell_volume 3171.9(4) _cod_database_code 1550338 _shelx_shelxl_version_number 2014/7 _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. ; _shelx_estimated_absorpt_t_min 0.801 _shelx_estimated_absorpt_t_max 0.964 _shelx_res_file ; 1.res created by SHELXL-2014/7 TITL 1 in P2(1)2(1)2(1) CELL 0.71073 9.1697 9.5203 36.3335 90.000 90.000 90.000 ZERR 4.00 0.0006 0.0006 0.0023 0.000 0.000 0.000 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 P S PD F O UNIT 136 152 4 4 4 4 8 12 L.S. 10 BOND FMAP 2 PLAN 10 omit 0 50 acta size 0.31 0.20 0.05 WGHT 0.036900 FVAR 0.35433 N1 3 0.628861 0.408642 0.158249 11.00000 0.01648 0.03194 = 0.02669 0.00046 0.00091 0.00326 S1 5 0.245359 0.303042 0.199124 11.00000 0.02622 0.02928 = 0.02420 -0.00470 0.00137 0.00136 PD1 6 0.467107 0.274041 0.136778 11.00000 0.02126 0.02822 = 0.02158 0.00016 0.00018 -0.00062 P1 4 0.285088 0.145646 0.113634 11.00000 0.02437 0.02235 = 0.02009 0.00011 0.00112 -0.00025 F1 7 0.179452 -0.288272 0.153098 11.00000 0.06562 0.04036 = 0.04042 0.00373 -0.01351 -0.01272 F2 7 0.583072 0.004482 0.172191 11.00000 0.03679 0.05126 = 0.04337 -0.00056 -0.00450 0.00199 C1 1 0.128186 0.166632 0.182019 11.00000 0.02032 0.03316 = 0.02058 0.00516 0.00062 0.00343 C2 1 0.143721 0.101886 0.147709 11.00000 0.02864 0.02294 = 0.01350 0.00641 -0.00272 0.00433 C3 1 0.045943 -0.005711 0.139132 11.00000 0.02962 0.02907 = 0.02584 0.00398 0.00170 -0.00873 AFIX 43 H3A 2 0.056715 -0.053512 0.116976 11.00000 -1.20000 AFIX 0 C4 1 -0.065648 -0.043221 0.162372 11.00000 0.04452 0.02986 = 0.03971 0.00094 0.00052 -0.01353 AFIX 43 H4A 2 -0.130402 -0.113636 0.155467 11.00000 -1.20000 AFIX 0 C5 1 -0.082127 0.022678 0.195745 11.00000 0.03766 0.04662 = 0.04139 0.00797 0.01314 -0.00868 AFIX 43 H5A 2 -0.156819 -0.002730 0.211730 11.00000 -1.20000 AFIX 0 C6 1 0.015093 0.127550 0.204911 11.00000 0.02859 0.04148 = 0.02819 -0.00410 0.00841 -0.00175 AFIX 43 H6A 2 0.004060 0.173580 0.227315 11.00000 -1.20000 AFIX 0 C7 1 0.183678 0.235620 0.075451 11.00000 0.02865 0.02732 = 0.01654 0.00276 0.00294 -0.00220 AFIX 13 H7A 2 0.247852 0.233390 0.053891 11.00000 -1.20000 AFIX 0 C8 1 0.033049 0.179825 0.062451 11.00000 0.03011 0.02306 = 0.02552 0.00508 -0.00305 -0.00571 AFIX 13 H8A 2 -0.029924 0.179300 0.084243 11.00000 -1.20000 AFIX 0 C9 1 -0.036711 0.281812 0.035219 11.00000 0.04116 0.03118 = 0.03347 0.00774 -0.01611 -0.00236 AFIX 23 H9A 2 -0.134518 0.249349 0.029644 11.00000 -1.20000 H9B 2 0.018854 0.280022 0.012506 11.00000 -1.20000 AFIX 0 C10 1 -0.045442 0.433046 0.048826 11.00000 0.04471 0.02567 = 0.02771 0.00909 -0.00907 0.00422 AFIX 23 H10A 2 -0.088190 0.491640 0.029836 11.00000 -1.20000 H10B 2 -0.107836 0.437490 0.070354 11.00000 -1.20000 AFIX 0 C11 1 0.103125 0.487505 0.058412 11.00000 0.03903 0.02359 = 0.02747 0.00365 -0.00698 -0.00196 AFIX 13 H11A 2 0.163353 0.482488 0.036169 11.00000 -1.20000 AFIX 0 C12 1 0.172585 0.391861 0.087393 11.00000 0.04144 0.02569 = 0.02604 -0.00156 -0.00255 -0.00311 AFIX 23 H12A 2 0.115585 0.397364 0.109836 11.00000 -1.20000 H12B 2 0.269701 0.426385 0.092886 11.00000 -1.20000 AFIX 0 C13 1 0.029474 0.029543 0.046865 11.00000 0.04098 0.02413 = 0.02388 -0.00349 -0.01020 -0.00095 AFIX 13 H13A 2 0.093732 -0.027730 0.062334 11.00000 -1.20000 AFIX 0 C14 1 -0.121730 -0.034185 0.049325 11.00000 0.04725 0.02355 = 0.05822 0.00045 -0.01369 -0.00816 AFIX 33 H14A 2 -0.156830 -0.026965 0.074146 11.00000 -1.50000 H14B 2 -0.186520 0.015326 0.033125 11.00000 -1.50000 H14C 2 -0.117585 -0.131271 0.042262 11.00000 -1.50000 AFIX 0 C15 1 0.086919 0.018685 0.007300 11.00000 0.06506 0.03763 = 0.03924 -0.00627 -0.01703 0.00372 AFIX 33 H15A 2 0.182628 0.059244 0.005985 11.00000 -1.50000 H15B 2 0.091501 -0.078289 0.000150 11.00000 -1.50000 H15C 2 0.022566 0.068307 -0.008987 11.00000 -1.50000 AFIX 0 C16 1 0.100055 0.638121 0.070788 11.00000 0.08017 0.02640 = 0.05099 0.00833 -0.02747 -0.00432 AFIX 33 H16A 2 0.197278 0.668233 0.076603 11.00000 -1.50000 H16B 2 0.061398 0.695788 0.051433 11.00000 -1.50000 H16C 2 0.039528 0.646541 0.092234 11.00000 -1.50000 AFIX 0 C17 1 0.361065 -0.019461 0.096711 11.00000 0.02268 0.02746 = 0.01788 0.00193 0.00113 0.00058 C18 1 0.401029 -0.032428 0.059999 11.00000 0.04527 0.02781 = 0.02460 0.00117 0.00514 0.00780 AFIX 43 H18A 2 0.376140 0.039911 0.043985 11.00000 -1.20000 AFIX 0 C19 1 0.474680 -0.145061 0.046021 11.00000 0.07012 0.04493 = 0.02649 0.00005 0.00789 0.02248 AFIX 43 H19A 2 0.496638 -0.149345 0.021057 11.00000 -1.20000 AFIX 0 C20 1 0.516038 -0.251919 0.069132 11.00000 0.08112 0.05323 = 0.03075 -0.01434 0.00626 0.03356 AFIX 43 H20A 2 0.568063 -0.328368 0.060104 11.00000 -1.20000 AFIX 0 C21 1 0.479623 -0.244579 0.105793 11.00000 0.07853 0.03460 = 0.02990 0.00433 -0.00167 0.02310 AFIX 43 H21A 2 0.506465 -0.317639 0.121375 11.00000 -1.20000 AFIX 0 C22 1 0.403822 -0.130885 0.120125 11.00000 0.03889 0.02390 = 0.02747 -0.00153 -0.00950 0.00674 C23 1 0.377259 -0.135246 0.160907 11.00000 0.03699 0.02460 = 0.01916 -0.00196 -0.00542 0.01467 C24 1 0.272686 -0.220066 0.176649 11.00000 0.04151 0.02631 = 0.03302 0.00495 -0.00406 0.00634 C25 1 0.255950 -0.242420 0.213486 11.00000 0.05319 0.03550 = 0.02961 0.00755 0.00410 0.00150 AFIX 43 H25A 2 0.183437 -0.301384 0.222516 11.00000 -1.20000 AFIX 0 C26 1 0.351220 -0.173813 0.236828 11.00000 0.06637 0.04459 = 0.02198 -0.00128 -0.00085 0.00549 AFIX 43 H26A 2 0.342547 -0.186838 0.262101 11.00000 -1.20000 AFIX 0 C27 1 0.458305 -0.086919 0.223548 11.00000 0.03708 0.04826 = 0.02545 -0.00491 -0.00989 0.00902 AFIX 43 H27A 2 0.520873 -0.039622 0.239430 11.00000 -1.20000 AFIX 0 C28 1 0.470275 -0.071920 0.186100 11.00000 0.03577 0.03071 = 0.03418 0.00469 0.00130 0.00497 C29 1 0.557856 0.289862 0.086151 11.00000 0.03591 0.04894 = 0.03143 -0.00286 0.00175 -0.01492 AFIX 33 H29A 2 0.502730 0.234603 0.068978 11.00000 -1.50000 H29B 2 0.557407 0.386351 0.078476 11.00000 -1.50000 H29C 2 0.656463 0.256135 0.086992 11.00000 -1.50000 AFIX 0 C30 1 0.773153 0.392901 0.154079 11.00000 0.02903 0.03550 = 0.03903 -0.00865 -0.00328 0.00480 AFIX 43 H30A 2 0.807042 0.319514 0.139511 11.00000 -1.20000 AFIX 0 C31 1 0.872861 0.480173 0.170337 11.00000 0.02638 0.05177 = 0.04525 -0.00193 -0.01038 -0.00072 AFIX 43 H31A 2 0.972216 0.465425 0.166949 11.00000 -1.20000 AFIX 0 C32 1 0.824215 0.590494 0.191852 11.00000 0.04457 0.03867 = 0.04335 0.00771 -0.01061 -0.01571 AFIX 43 H32A 2 0.889800 0.652596 0.202641 11.00000 -1.20000 AFIX 0 C33 1 0.677096 0.606001 0.196870 11.00000 0.04413 0.02224 = 0.03809 -0.00316 -0.00705 0.00304 AFIX 43 H33A 2 0.641090 0.677808 0.211655 11.00000 -1.20000 AFIX 0 C34 1 0.582537 0.513469 0.179665 11.00000 0.02864 0.02915 = 0.02770 0.01279 0.00115 0.00365 AFIX 43 H34A 2 0.482769 0.524831 0.183174 11.00000 -1.20000 AFIX 0 O1 8 0.394561 0.250306 0.192694 11.00000 0.02298 0.03308 = 0.02125 -0.00352 -0.00122 0.00381 O3 8 0.213502 0.314860 0.237627 11.00000 0.03945 0.05836 = 0.02186 -0.01190 0.00447 -0.00609 O2 8 0.215917 0.426659 0.177712 11.00000 0.03599 0.02608 = 0.04187 0.00127 -0.00243 0.00200 HKLF 4 REM 1 in P2(1)2(1)2(1) REM R1 = 0.0468 for 4534 Fo > 4sig(Fo) and 0.0662 for all 5595 data REM 388 parameters refined using 0 restraints END WGHT 0.0330 0.0000 REM Highest difference peak 0.674, deepest hole -0.412, 1-sigma level 0.085 Q1 1 0.5304 0.2674 0.1121 11.00000 0.05 0.62 Q2 1 0.3977 0.2522 0.1586 11.00000 0.05 0.61 Q3 1 0.3955 0.2454 0.1129 11.00000 0.05 0.59 Q4 1 0.5253 0.2429 0.1648 11.00000 0.05 0.59 Q5 1 0.4111 0.2190 0.1626 11.00000 0.05 0.53 Q6 1 0.5192 0.1868 0.1375 11.00000 0.05 0.51 Q7 1 0.4080 0.3129 0.1630 11.00000 0.05 0.50 Q8 1 0.4166 0.3217 0.1060 11.00000 0.05 0.49 Q9 1 0.4495 0.3792 0.1367 11.00000 0.05 0.48 Q10 1 0.4057 0.1814 0.1324 11.00000 0.05 0.45 ; _shelx_res_checksum 18972 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' 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 N1 N 0.6289(6) 0.4086(6) 0.15825(17) 0.0250(15) Uani 1 1 d . . S1 S 0.2454(2) 0.3030(2) 0.19912(5) 0.0266(5) Uani 1 1 d . . Pd1 Pd 0.46711(6) 0.27404(6) 0.13678(2) 0.02369(16) Uani 1 1 d . . P1 P 0.2851(2) 0.1456(2) 0.11363(5) 0.0223(5) Uani 1 1 d . . F1 F 0.1795(5) -0.2883(5) 0.15310(12) 0.0488(13) Uani 1 1 d . . F2 F 0.5831(5) 0.0045(5) 0.17219(14) 0.0438(14) Uani 1 1 d . . C1 C 0.1282(8) 0.1666(8) 0.1820(2) 0.0247(18) Uani 1 1 d . . C2 C 0.1437(8) 0.1019(7) 0.14771(19) 0.0217(18) Uani 1 1 d . . C3 C 0.0459(8) -0.0057(7) 0.1391(2) 0.0282(17) Uani 1 1 d . . H3A H 0.0567 -0.0535 0.1170 0.034 Uiso 1 1 calc R U C4 C -0.0656(9) -0.0432(8) 0.1624(2) 0.038(2) Uani 1 1 d . . H4A H -0.1304 -0.1136 0.1555 0.046 Uiso 1 1 calc R U C5 C -0.0821(9) 0.0227(9) 0.1957(3) 0.042(2) Uani 1 1 d . . H5A H -0.1568 -0.0027 0.2117 0.050 Uiso 1 1 calc R U C6 C 0.0151(8) 0.1276(8) 0.2049(2) 0.033(2) Uani 1 1 d . . H6A H 0.0041 0.1736 0.2273 0.039 Uiso 1 1 calc R U C7 C 0.1837(7) 0.2356(8) 0.07545(18) 0.0242(17) Uani 1 1 d . . H7A H 0.2479 0.2334 0.0539 0.029 Uiso 1 1 calc R U C8 C 0.0330(9) 0.1798(7) 0.0625(2) 0.0262(17) Uani 1 1 d . . H8A H -0.0299 0.1793 0.0842 0.031 Uiso 1 1 calc R U C9 C -0.0367(9) 0.2818(7) 0.0352(2) 0.0353(18) Uani 1 1 d . . H9A H -0.1345 0.2493 0.0296 0.042 Uiso 1 1 calc R U H9B H 0.0189 0.2800 0.0125 0.042 Uiso 1 1 calc R U C10 C -0.0454(10) 0.4330(7) 0.0488(2) 0.033(2) Uani 1 1 d . . H10A H -0.0882 0.4916 0.0298 0.039 Uiso 1 1 calc R U H10B H -0.1078 0.4375 0.0704 0.039 Uiso 1 1 calc R U C11 C 0.1031(9) 0.4875(8) 0.0584(2) 0.030(2) Uani 1 1 d . . H11A H 0.1634 0.4825 0.0362 0.036 Uiso 1 1 calc R U C12 C 0.1726(9) 0.3919(7) 0.0874(2) 0.031(2) Uani 1 1 d . . H12A H 0.1156 0.3974 0.1098 0.037 Uiso 1 1 calc R U H12B H 0.2697 0.4264 0.0929 0.037 Uiso 1 1 calc R U C13 C 0.0295(10) 0.0295(7) 0.0469(2) 0.0297(19) Uani 1 1 d . . H13A H 0.0937 -0.0277 0.0623 0.036 Uiso 1 1 calc R U C14 C -0.1217(10) -0.0342(8) 0.0493(3) 0.043(2) Uani 1 1 d . . H14A H -0.1568 -0.0270 0.0741 0.065 Uiso 1 1 calc R U H14B H -0.1865 0.0153 0.0331 0.065 Uiso 1 1 calc R U H14C H -0.1176 -0.1313 0.0423 0.065 Uiso 1 1 calc R U C15 C 0.0869(10) 0.0187(9) 0.0073(2) 0.047(3) Uani 1 1 d . . H15A H 0.1826 0.0592 0.0060 0.071 Uiso 1 1 calc R U H15B H 0.0915 -0.0783 0.0001 0.071 Uiso 1 1 calc R U H15C H 0.0226 0.0683 -0.0090 0.071 Uiso 1 1 calc R U C16 C 0.1001(11) 0.6381(8) 0.0708(2) 0.053(3) Uani 1 1 d . . H16A H 0.1973 0.6682 0.0766 0.079 Uiso 1 1 calc R U H16B H 0.0614 0.6958 0.0514 0.079 Uiso 1 1 calc R U H16C H 0.0395 0.6465 0.0922 0.079 Uiso 1 1 calc R U C17 C 0.3611(8) -0.0195(8) 0.0967(2) 0.0227(18) Uani 1 1 d . . C18 C 0.4010(9) -0.0324(8) 0.0600(2) 0.033(2) Uani 1 1 d . . H18A H 0.3761 0.0399 0.0440 0.039 Uiso 1 1 calc R U C19 C 0.4747(11) -0.1451(9) 0.0460(2) 0.047(2) Uani 1 1 d . . H19A H 0.4966 -0.1493 0.0211 0.057 Uiso 1 1 calc R U C20 C 0.5160(10) -0.2519(9) 0.0691(2) 0.055(3) Uani 1 1 d . . H20A H 0.5681 -0.3284 0.0601 0.066 Uiso 1 1 calc R U C21 C 0.4796(10) -0.2446(8) 0.1058(2) 0.048(2) Uani 1 1 d . . H21A H 0.5065 -0.3176 0.1214 0.057 Uiso 1 1 calc R U C22 C 0.4038(9) -0.1309(8) 0.1201(2) 0.030(2) Uani 1 1 d . . C23 C 0.3773(9) -0.1352(8) 0.1609(2) 0.0269(19) Uani 1 1 d . . C24 C 0.2727(8) -0.2201(8) 0.1766(2) 0.0336(19) Uani 1 1 d . . C25 C 0.2560(9) -0.2424(9) 0.2135(2) 0.039(2) Uani 1 1 d . . H25A H 0.1834 -0.3014 0.2225 0.047 Uiso 1 1 calc R U C26 C 0.3512(10) -0.1738(9) 0.2368(2) 0.044(2) Uani 1 1 d . . H26A H 0.3425 -0.1868 0.2621 0.053 Uiso 1 1 calc R U C27 C 0.4583(10) -0.0869(8) 0.2235(2) 0.037(2) Uani 1 1 d . . H27A H 0.5209 -0.0396 0.2394 0.044 Uiso 1 1 calc R U C28 C 0.4703(10) -0.0719(8) 0.1861(2) 0.0336(19) Uani 1 1 d . . C29 C 0.5579(8) 0.2899(9) 0.08615(19) 0.039(2) Uani 1 1 d . . H29A H 0.5027 0.2346 0.0690 0.058 Uiso 1 1 calc R U H29B H 0.5574 0.3864 0.0785 0.058 Uiso 1 1 calc R U H29C H 0.6565 0.2561 0.0870 0.058 Uiso 1 1 calc R U C30 C 0.7732(8) 0.3929(9) 0.1541(2) 0.035(2) Uani 1 1 d . . H30A H 0.8070 0.3195 0.1395 0.041 Uiso 1 1 calc R U C31 C 0.8729(9) 0.4802(9) 0.1703(3) 0.041(2) Uani 1 1 d . . H31A H 0.9722 0.4654 0.1669 0.049 Uiso 1 1 calc R U C32 C 0.8242(10) 0.5905(9) 0.1919(2) 0.042(2) Uani 1 1 d . . H32A H 0.8898 0.6526 0.2026 0.051 Uiso 1 1 calc R U C33 C 0.6771(9) 0.6060(8) 0.1969(2) 0.035(2) Uani 1 1 d . . H33A H 0.6411 0.6778 0.2117 0.042 Uiso 1 1 calc R U C34 C 0.5825(9) 0.5135(8) 0.1797(2) 0.028(2) Uani 1 1 d . . H34A H 0.4828 0.5248 0.1832 0.034 Uiso 1 1 calc R U O1 O 0.3946(5) 0.2503(5) 0.19269(12) 0.0258(12) Uani 1 1 d . . O3 O 0.2135(6) 0.3149(6) 0.23763(14) 0.0399(15) Uani 1 1 d . . O2 O 0.2159(6) 0.4267(5) 0.17771(15) 0.0346(14) Uani 1 1 d . . 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 N1 0.016(3) 0.032(4) 0.027(4) 0.000(3) 0.001(3) 0.003(3) S1 0.0262(10) 0.0293(12) 0.0242(11) -0.0047(9) 0.0014(9) 0.0014(8) Pd1 0.0213(3) 0.0282(3) 0.0216(3) 0.0002(3) 0.0002(3) -0.0006(3) P1 0.0244(11) 0.0224(11) 0.0201(12) 0.0001(9) 0.0011(9) -0.0003(9) F1 0.066(3) 0.040(3) 0.040(3) 0.004(2) -0.014(2) -0.013(3) F2 0.037(3) 0.051(3) 0.043(4) -0.001(3) -0.004(3) 0.002(3) C1 0.020(4) 0.033(5) 0.021(5) 0.005(3) 0.001(3) 0.003(3) C2 0.029(4) 0.023(4) 0.013(5) 0.006(3) -0.003(3) 0.004(3) C3 0.030(4) 0.029(4) 0.026(4) 0.004(4) 0.002(5) -0.009(4) C4 0.045(6) 0.030(5) 0.040(6) 0.001(4) 0.001(4) -0.014(4) C5 0.038(5) 0.047(6) 0.041(6) 0.008(5) 0.013(4) -0.009(4) C6 0.029(5) 0.041(5) 0.028(5) -0.004(4) 0.008(4) -0.002(4) C7 0.029(4) 0.027(4) 0.017(4) 0.003(3) 0.003(3) -0.002(4) C8 0.030(4) 0.023(4) 0.026(4) 0.005(3) -0.003(4) -0.006(4) C9 0.041(4) 0.031(4) 0.033(5) 0.008(4) -0.016(4) -0.002(5) C10 0.045(5) 0.026(4) 0.028(5) 0.009(3) -0.009(5) 0.004(5) C11 0.039(5) 0.024(5) 0.027(5) 0.004(4) -0.007(4) -0.002(4) C12 0.041(5) 0.026(5) 0.026(5) -0.002(4) -0.003(4) -0.003(4) C13 0.041(5) 0.024(4) 0.024(5) -0.003(3) -0.010(4) -0.001(5) C14 0.047(6) 0.024(5) 0.058(7) 0.000(4) -0.014(5) -0.008(4) C15 0.065(7) 0.038(5) 0.039(6) -0.006(4) -0.017(5) 0.004(5) C16 0.080(7) 0.026(5) 0.051(7) 0.008(4) -0.027(5) -0.004(5) C17 0.023(4) 0.027(4) 0.018(5) 0.002(3) 0.001(3) 0.001(3) C18 0.045(5) 0.028(5) 0.025(5) 0.001(4) 0.005(4) 0.008(4) C19 0.070(7) 0.045(5) 0.026(5) 0.000(4) 0.008(5) 0.022(6) C20 0.081(7) 0.053(6) 0.031(5) -0.014(4) 0.006(5) 0.034(6) C21 0.079(6) 0.035(5) 0.030(5) 0.004(4) -0.002(4) 0.023(5) C22 0.039(5) 0.024(4) 0.027(5) -0.002(4) -0.009(4) 0.007(4) C23 0.037(5) 0.025(5) 0.019(5) -0.002(4) -0.005(4) 0.015(4) C24 0.042(5) 0.026(4) 0.033(5) 0.005(4) -0.004(4) 0.006(4) C25 0.053(5) 0.036(5) 0.030(5) 0.008(4) 0.004(4) 0.001(5) C26 0.066(7) 0.045(6) 0.022(5) -0.001(4) -0.001(5) 0.005(5) C27 0.037(5) 0.048(5) 0.025(5) -0.005(4) -0.010(5) 0.009(5) C28 0.036(5) 0.031(4) 0.034(5) 0.005(4) 0.001(5) 0.005(5) C29 0.036(5) 0.049(5) 0.031(5) -0.003(4) 0.002(4) -0.015(4) C30 0.029(5) 0.035(5) 0.039(6) -0.009(4) -0.003(4) 0.005(4) C31 0.026(5) 0.052(6) 0.045(7) -0.002(5) -0.010(4) -0.001(5) C32 0.045(6) 0.039(6) 0.043(6) 0.008(5) -0.011(5) -0.016(5) C33 0.044(5) 0.022(5) 0.038(6) -0.003(4) -0.007(4) 0.003(4) C34 0.029(5) 0.029(5) 0.028(5) 0.013(4) 0.001(4) 0.004(4) O1 0.023(2) 0.033(3) 0.021(3) -0.004(2) -0.001(2) 0.004(2) O3 0.039(3) 0.058(4) 0.022(3) -0.012(3) 0.004(3) -0.006(3) O2 0.036(4) 0.026(3) 0.042(4) 0.001(3) -0.002(3) 0.002(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' N N 0.0061 0.0033 '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' Pd Pd -0.9988 1.0072 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' F F 0.0171 0.0103 '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' loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle C30 N1 C34 117.6(7) C30 N1 Pd1 125.8(5) C34 N1 Pd1 116.5(5) O3 S1 O2 115.2(3) O3 S1 O1 111.7(3) O2 S1 O1 111.5(3) O3 S1 C1 105.8(3) O2 S1 C1 107.0(3) O1 S1 C1 104.7(3) C29 Pd1 N1 90.1(3) C29 Pd1 O1 173.6(3) N1 Pd1 O1 86.1(2) C29 Pd1 P1 90.3(2) N1 Pd1 P1 175.70(18) O1 Pd1 P1 93.84(13) C17 P1 C2 107.5(3) C17 P1 C7 109.5(3) C2 P1 C7 104.6(3) C17 P1 Pd1 108.2(2) C2 P1 Pd1 113.4(2) C7 P1 Pd1 113.5(2) C6 C1 C2 119.7(7) C6 C1 S1 115.8(6) C2 C1 S1 124.5(6) C1 C2 C3 117.2(7) C1 C2 P1 124.9(6) C3 C2 P1 117.9(6) C4 C3 C2 122.1(8) C5 C4 C3 120.4(8) C4 C5 C6 118.2(8) C5 C6 C1 122.4(8) C8 C7 C12 110.7(6) C8 C7 P1 120.6(5) C12 C7 P1 105.3(5) C9 C8 C7 110.6(6) C9 C8 C13 110.1(6) C7 C8 C13 116.7(7) C8 C9 C10 114.4(6) C11 C10 C9 110.8(7) C10 C11 C16 112.5(7) C10 C11 C12 109.4(6) C16 C11 C12 111.7(7) C11 C12 C7 113.9(6) C15 C13 C14 110.0(7) C15 C13 C8 113.6(6) C14 C13 C8 111.7(7) C18 C17 C22 116.0(7) C18 C17 P1 120.0(6) C22 C17 P1 123.3(6) C19 C18 C17 123.9(8) C18 C19 C20 119.4(8) C21 C20 C19 119.2(7) C20 C21 C22 121.7(7) C21 C22 C17 119.9(8) C21 C22 C23 115.5(7) C17 C22 C23 124.7(7) C24 C23 C28 114.1(7) C24 C23 C22 122.6(7) C28 C23 C22 122.6(8) C23 C24 F1 116.9(7) C23 C24 C25 125.2(8) F1 C24 C25 117.9(7) C24 C25 C26 117.2(8) C27 C26 C25 121.5(8) C26 C27 C28 118.0(8) F2 C28 C23 117.0(7) F2 C28 C27 119.0(8) C23 C28 C27 124.0(9) N1 C30 C31 122.9(8) C30 C31 C32 119.3(8) C31 C32 C33 118.3(8) C34 C33 C32 119.2(8) N1 C34 C33 122.6(8) S1 O1 Pd1 113.6(2) loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance N1 C30 1.340(9) N1 C34 1.335(9) N1 Pd1 2.110(6) S1 O3 1.434(5) S1 O2 1.436(6) S1 O1 1.476(4) S1 C1 1.796(8) Pd1 C29 2.025(7) Pd1 O1 2.150(4) Pd1 P1 2.233(2) P1 C17 1.826(8) P1 C2 1.840(7) P1 C7 1.877(7) F1 C24 1.373(8) F2 C28 1.362(9) C1 C6 1.380(10) C1 C2 1.398(9) C2 C3 1.397(9) C3 C4 1.374(10) C4 C5 1.374(12) C5 C6 1.379(11) C7 C8 1.553(10) C7 C12 1.553(10) C8 C9 1.527(9) C8 C13 1.539(9) C9 C10 1.524(9) C10 C11 1.499(11) C11 C16 1.503(11) C11 C12 1.531(10) C13 C15 1.534(11) C13 C14 1.516(12) C17 C18 1.389(10) C17 C22 1.415(10) C18 C19 1.365(10) C19 C20 1.373(11) C20 C21 1.375(10) C21 C22 1.388(10) C22 C23 1.502(10) C23 C24 1.378(11) C23 C28 1.389(11) C24 C25 1.364(10) C25 C26 1.382(11) C26 C27 1.372(12) C27 C28 1.372(10) C30 C31 1.369(11) C31 C32 1.383(12) C32 C33 1.369(12) C33 C34 1.385(11)