#------------------------------------------------------------------------------ #$Date: 2021-10-09 04:04:11 +0300 (Sat, 09 Oct 2021) $ #$Revision: 269873 $ #$URL: file:///home/coder/svn-repositories/cod/cif/1/56/48/1564892.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_1564892 loop_ _publ_author_name 'P\'erez-Ortega, Ignacio' 'Albeniz, Ana Carmen' _publ_section_title ; Highly Efficient Vinylic Addition Polymerization of 5-Vinyl-2-Norbornene using Benzylic Palladium Complexes as Precatalysts ; _journal_name_full 'Polymer Chemistry' _journal_paper_doi 10.1039/D1PY01165K _journal_year 2021 _chemical_formula_moiety 'C34 H44 F5 N P Pd, B F4' _chemical_formula_sum 'C34 H44 B F9 N P Pd' _chemical_formula_weight 785.88 _space_group_crystal_system triclinic _space_group_IT_number 2 _space_group_name_Hall '-P 1' _space_group_name_H-M_alt 'P -1' _atom_sites_solution_hydrogens mixed _atom_sites_solution_primary dual _audit_creation_date 2021-08-10 _audit_creation_method ; Olex2 1.2 (compiled 2018.05.29 svn.r3508 for OlexSys, GUI svn.r5506) ; _audit_update_record ; 2021-08-27 deposited with the CCDC. 2021-10-06 downloaded from the CCDC. ; _cell_angle_alpha 109.041(6) _cell_angle_beta 91.911(6) _cell_angle_gamma 107.037(5) _cell_formula_units_Z 2 _cell_length_a 10.3004(6) _cell_length_b 13.2588(7) _cell_length_c 16.2684(14) _cell_measurement_reflns_used 3209 _cell_measurement_temperature 298 _cell_measurement_theta_max 23.4530 _cell_measurement_theta_min 3.6960 _cell_volume 1987.5(3) _computing_cell_refinement 'CrysAlisPro 1.171.39.45g (Rigaku OD, 2018)' _computing_data_collection 'CrysAlisPro 1.171.39.45g (Rigaku OD, 2018)' _computing_data_reduction 'CrysAlisPro 1.171.39.45g (Rigaku OD, 2018)' _computing_molecular_graphics 'Olex2 (Dolomanov et al., 2009)' _computing_publication_material 'Olex2 (Dolomanov et al., 2009)' _computing_structure_refinement 'ShelXL (Sheldrick, 2015)' _computing_structure_solution 'ShelXT (Sheldrick, 2015)' _diffrn_ambient_temperature 298.0 _diffrn_detector_area_resol_mean 10.4757 _diffrn_detector_type Atlas _diffrn_measured_fraction_theta_full 0.992 _diffrn_measured_fraction_theta_max 0.818 _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 -35.00 63.00 1.00 26.45 -- -10.48 57.00 -90.00 98 2 \w -75.00 15.00 1.00 26.45 -- -10.48 -57.00 120.00 90 3 \w 34.00 100.00 1.00 26.45 -- 12.36-178.00 120.00 66 ; _diffrn_measurement_device 'four-circle diffractometer' _diffrn_measurement_device_type 'SuperNova, Dual, Cu at home/near, Atlas' _diffrn_measurement_method '\w scans' _diffrn_radiation_type MoK\a _diffrn_radiation_wavelength 0.71073 _diffrn_reflns_av_R_equivalents 0.0374 _diffrn_reflns_av_unetI/netI 0.0892 _diffrn_reflns_Laue_measured_fraction_full 0.992 _diffrn_reflns_Laue_measured_fraction_max 0.818 _diffrn_reflns_limit_h_max 14 _diffrn_reflns_limit_h_min -10 _diffrn_reflns_limit_k_max 16 _diffrn_reflns_limit_k_min -18 _diffrn_reflns_limit_l_max 20 _diffrn_reflns_limit_l_min -21 _diffrn_reflns_number 13942 _diffrn_reflns_point_group_measured_fraction_full 0.992 _diffrn_reflns_point_group_measured_fraction_max 0.818 _diffrn_reflns_theta_full 25.242 _diffrn_reflns_theta_max 29.534 _diffrn_reflns_theta_min 3.433 _exptl_absorpt_coefficient_mu 0.571 _exptl_absorpt_correction_T_max 1.000 _exptl_absorpt_correction_T_min 0.367 _exptl_absorpt_correction_type gaussian _exptl_absorpt_process_details ; CrysAlisPro 1.171.39.45g (Rigaku Oxford Diffraction, 2018) Numerical absorption correction based on gaussian integration over a multifaceted crystal model Empirical absorption correction using spherical harmonics, implemented in SCALE3 ABSPACK scaling algorithm. ; _exptl_crystal_colour 'clear light yellow' _exptl_crystal_colour_lustre clear _exptl_crystal_colour_modifier light _exptl_crystal_colour_primary yellow _exptl_crystal_density_diffrn 1.313 _exptl_crystal_description block _exptl_crystal_F_000 804 _exptl_crystal_size_max 0.362 _exptl_crystal_size_mid 0.181 _exptl_crystal_size_min 0.111 _refine_diff_density_max 0.458 _refine_diff_density_min -0.612 _refine_diff_density_rms 0.069 _refine_ls_extinction_method none _refine_ls_goodness_of_fit_ref 1.005 _refine_ls_hydrogen_treatment mixed _refine_ls_matrix_type full _refine_ls_number_parameters 456 _refine_ls_number_reflns 9092 _refine_ls_number_restraints 1 _refine_ls_restrained_S_all 1.005 _refine_ls_R_factor_all 0.0965 _refine_ls_R_factor_gt 0.0547 _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^)+(0.0383P)^2^] where P=(Fo^2^+2Fc^2^)/3' _refine_ls_weighting_scheme calc _refine_ls_wR_factor_gt 0.0980 _refine_ls_wR_factor_ref 0.1218 _reflns_Friedel_coverage 0.000 _reflns_number_gt 5689 _reflns_number_total 9092 _reflns_threshold_expression 'I > 2\s(I)' _cod_data_source_file d1py01165k2.cif _cod_data_source_block 4-BF4 _cod_original_cell_volume 1987.5(2) _cod_database_code 1564892 _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. ; _olex2_refinement_description ; 1. Fixed Uiso At 1.2 times of: All C(H) groups, All C(H,H) groups At 1.5 times of: All C(H,H,H) groups 2. Restrained distances F13A-F12A 2 with sigma of 0.02 3. Others Fixed Sof: F11A(0.5) F11B(0.5) F12A(0.5) F12B(0.5) F13A(0.5) F13B(0.5) 4.a Ternary CH refined with riding coordinates: C7(H7), C17(H17), C23(H23), C29(H29) 4.b Secondary CH2 refined with riding coordinates: C8(H8A,H8B), C18(H18A,H18B), C19(H19A,H19B), C20(H20A,H20B), C21(H21A,H21B), C22(H22A,H22B), C24(H24A,H24B), C25(H25A,H25B), C26(H26A,H26B), C27(H27A,H27B), C28(H28A,H28B), C30(H30A,H30B), C31(H31A,H31B), C32(H32A,H32B), C33(H33A, H33B), C34(H34A,H34B) 4.c Aromatic/amide H refined with riding coordinates: C3(H3), C4(H4), C5(H5), C6(H6) 4.d Idealised Me refined as rotating group: C16(H16A,H16B,H16C) ; _shelx_res_file ; 1563b.res created by SHELXL-2014/7 TITL 1563b_a.res in P-1 REM Old TITL 1563b in P1 REM SHELXT solution in P-1 REM R1 0.177, Rweak 0.019, Alpha 0.081, Orientation as input REM Formula found by SHELXT: C33 B N10 F7 P Pd CELL 0.71073 10.3004 13.2588 16.2684 109.041 91.911 107.037 ZERR 2 0.0006 0.0007 0.0014 0.006 0.006 0.005 LATT 1 SFAC C H B F N P Pd UNIT 68 88 2 18 2 2 2 DFIX 2 F13A F12A L.S. 13 PLAN 1 TEMP 24.85 CONF list 4 MORE -1 BOND $H ABIN fmap 2 53 acta REM REM REM WGHT 0.038300 FVAR 0.47902 C1 1 0.695358 0.272014 0.392380 11.00000 0.06529 0.05733 = 0.05617 0.03377 -0.00485 0.00567 F1 4 0.575224 -0.053448 0.149830 11.00000 0.11214 0.07430 = 0.08664 0.01992 0.02254 0.01776 N1 5 0.699556 0.543939 0.362112 11.00000 0.10702 0.05002 = 0.05397 0.01653 0.00950 0.02548 P1 6 0.697914 0.358268 0.167373 11.00000 0.03466 0.03898 = 0.04075 0.01415 0.00084 0.01032 PD1 7 0.672513 0.370022 0.308974 11.00000 0.05770 0.04372 = 0.04296 0.01520 0.00261 0.01363 C2 1 0.614266 0.332031 0.440149 11.00000 0.07314 0.08073 = 0.05513 0.03471 0.00260 0.01713 H2 2 0.527259 0.315823 0.417358 11.00000 0.04367 F2 4 0.541360 -0.251008 0.171394 11.00000 0.16303 0.06496 = 0.17769 0.02600 0.04508 0.04142 C3 1 0.668857 0.413511 0.523724 11.00000 0.13005 0.08057 = 0.04686 0.01984 0.00525 0.02228 AFIX 43 H3 2 0.615045 0.453338 0.555423 11.00000 -1.20000 AFIX 0 F3 4 0.441302 -0.286404 0.314387 11.00000 0.14672 0.07708 = 0.19935 0.08399 -0.00789 0.01266 C4 1 0.799160 0.434534 0.558499 11.00000 0.14480 0.08761 = 0.06498 0.02469 -0.03450 0.00498 AFIX 43 H4 2 0.833813 0.488100 0.614292 11.00000 -1.20000 AFIX 0 F4 4 0.368628 -0.122412 0.433690 11.00000 0.19184 0.13328 = 0.10831 0.07665 0.03194 0.01403 C5 1 0.880421 0.378113 0.512728 11.00000 0.10034 0.10739 = 0.09244 0.03697 -0.04521 0.00706 AFIX 43 H5 2 0.969958 0.393897 0.537604 11.00000 -1.20000 AFIX 0 F5 4 0.398074 0.073284 0.411316 11.00000 0.15375 0.09740 = 0.08887 0.02795 0.04292 0.03548 C6 1 0.831777 0.298396 0.430485 11.00000 0.08352 0.08014 = 0.08372 0.03956 -0.01367 0.01816 AFIX 43 H6 2 0.888912 0.261538 0.399664 11.00000 -1.20000 AFIX 0 C7 1 0.648070 0.206605 0.299103 11.00000 0.05533 0.05211 = 0.06284 0.02933 -0.00007 0.01262 AFIX 13 H7 2 0.717223 0.177524 0.268724 11.00000 -1.20000 AFIX 0 C8 1 0.503966 0.126823 0.265626 11.00000 0.06669 0.05340 = 0.06723 0.02373 -0.00360 0.01474 AFIX 23 H8A 2 0.483138 0.112319 0.203439 11.00000 -1.20000 H8B 2 0.439864 0.161363 0.295979 11.00000 -1.20000 AFIX 0 C9 1 0.486643 0.016492 0.279784 11.00000 0.06192 0.04757 = 0.05647 0.01654 -0.00545 0.00545 C10 1 0.436372 -0.004855 0.350411 11.00000 0.08825 0.07095 = 0.07257 0.02615 0.00935 0.01446 C11 1 0.420207 -0.107635 0.362248 11.00000 0.10382 0.08022 = 0.08234 0.04781 -0.00037 -0.00063 C12 1 0.457068 -0.188398 0.302361 11.00000 0.09030 0.06154 = 0.12543 0.04997 -0.00437 0.00721 C13 1 0.507565 -0.169511 0.232392 11.00000 0.08456 0.05032 = 0.11846 0.02335 0.00713 0.01371 C14 1 0.523634 -0.068753 0.221314 11.00000 0.07242 0.05759 = 0.07460 0.02637 0.00184 0.00764 C15 1 0.715039 0.633959 0.398372 11.00000 0.11018 0.06068 = 0.05070 0.02064 0.01208 0.02689 C16 1 0.737786 0.754063 0.445807 11.00000 0.25424 0.05234 = 0.10422 0.00425 0.00934 0.03971 AFIX 137 H16A 2 0.727527 0.790009 0.404576 11.00000 -1.50000 H16B 2 0.828745 0.788644 0.478036 11.00000 -1.50000 H16C 2 0.671965 0.762102 0.485836 11.00000 -1.50000 AFIX 0 C17 1 0.835484 0.487718 0.173930 11.00000 0.04183 0.04860 = 0.04870 0.02071 -0.00222 0.00512 AFIX 13 H17 2 0.798794 0.547860 0.204987 11.00000 -1.20000 AFIX 0 C18 1 0.965988 0.512838 0.234899 11.00000 0.04768 0.06115 = 0.06587 0.02758 -0.02062 0.00051 AFIX 23 H18A 2 0.941724 0.503649 0.289729 11.00000 -1.20000 H18B 2 1.012985 0.459428 0.207894 11.00000 -1.20000 AFIX 0 C19 1 1.061067 0.631224 0.253608 11.00000 0.06753 0.08666 = 0.09487 0.04217 -0.02944 -0.02141 AFIX 23 H19A 2 1.020290 0.684279 0.290095 11.00000 -1.20000 H19B 2 1.146944 0.641031 0.286471 11.00000 -1.20000 AFIX 0 C20 1 1.089952 0.657618 0.172944 11.00000 0.05878 0.07828 = 0.09472 0.04706 -0.00743 -0.00925 AFIX 23 H20A 2 1.146162 0.614578 0.141908 11.00000 -1.20000 H20B 2 1.141885 0.736939 0.189425 11.00000 -1.20000 AFIX 0 C21 1 0.961445 0.631469 0.112252 11.00000 0.06096 0.06964 = 0.07286 0.04249 0.00306 0.00136 AFIX 23 H21A 2 0.986090 0.642337 0.057992 11.00000 -1.20000 H21B 2 0.912441 0.683237 0.139380 11.00000 -1.20000 AFIX 0 C22 1 0.867212 0.509827 0.091437 11.00000 0.05452 0.07342 = 0.05950 0.02877 0.00137 0.00383 AFIX 23 H22A 2 0.782573 0.497430 0.055951 11.00000 -1.20000 H22B 2 0.911725 0.457759 0.057900 11.00000 -1.20000 AFIX 0 C23 1 0.735439 0.232188 0.096336 11.00000 0.03789 0.04148 = 0.05080 0.01359 0.00486 0.01240 AFIX 13 H23 2 0.666044 0.167681 0.102909 11.00000 -1.20000 AFIX 0 C24 1 0.873512 0.226269 0.128174 11.00000 0.04646 0.06359 = 0.06238 0.01874 0.00487 0.02476 AFIX 23 H24A 2 0.880455 0.238698 0.190542 11.00000 -1.20000 H24B 2 0.947335 0.285131 0.119323 11.00000 -1.20000 AFIX 0 C25 1 0.888134 0.110890 0.077979 11.00000 0.07209 0.07643 = 0.09188 0.02594 0.01718 0.04592 AFIX 23 H25A 2 0.977032 0.109320 0.098020 11.00000 -1.20000 H25B 2 0.818101 0.052567 0.090201 11.00000 -1.20000 AFIX 0 C26 1 0.874403 0.087532 -0.018519 11.00000 0.07555 0.06173 = 0.09923 0.01088 0.02106 0.03714 AFIX 23 H26A 2 0.878109 0.012334 -0.048728 11.00000 -1.20000 H26B 2 0.950898 0.140667 -0.031252 11.00000 -1.20000 AFIX 0 C27 1 0.741167 0.096598 -0.052764 11.00000 0.07214 0.05744 = 0.06573 -0.00014 0.00778 0.02030 AFIX 23 H27A 2 0.664857 0.036305 -0.047856 11.00000 -1.20000 H27B 2 0.739964 0.087535 -0.114438 11.00000 -1.20000 AFIX 0 C28 1 0.723198 0.210209 -0.001900 11.00000 0.05223 0.05196 = 0.05018 0.00959 0.00503 0.01715 AFIX 23 H28A 2 0.792554 0.269983 -0.012974 11.00000 -1.20000 H28B 2 0.633915 0.210608 -0.022435 11.00000 -1.20000 AFIX 0 C29 1 0.544896 0.360138 0.106342 11.00000 0.03693 0.05176 = 0.04772 0.02177 0.00253 0.01508 AFIX 13 H29 2 0.567077 0.362745 0.048802 11.00000 -1.20000 AFIX 0 C30 1 0.502582 0.464066 0.153673 11.00000 0.04849 0.05962 = 0.08639 0.01898 0.00078 0.02829 AFIX 23 H30A 2 0.481305 0.463925 0.211279 11.00000 -1.20000 H30B 2 0.578033 0.532063 0.161510 11.00000 -1.20000 AFIX 0 C31 1 0.376739 0.462985 0.099861 11.00000 0.05405 0.07518 = 0.10649 0.03786 0.00176 0.03481 AFIX 23 H31A 2 0.350015 0.528165 0.130815 11.00000 -1.20000 H31B 2 0.400187 0.467977 0.043745 11.00000 -1.20000 AFIX 0 C32 1 0.258055 0.357313 0.084533 11.00000 0.04334 0.10309 = 0.08513 0.04835 0.00514 0.02827 AFIX 23 H32A 2 0.181240 0.357446 0.048463 11.00000 -1.20000 H32B 2 0.229361 0.355332 0.140330 11.00000 -1.20000 AFIX 0 C33 1 0.298706 0.253191 0.038966 11.00000 0.04213 0.07690 = 0.08477 0.02813 -0.01135 0.00414 AFIX 23 H33A 2 0.222615 0.186051 0.032285 11.00000 -1.20000 H33B 2 0.318867 0.251580 -0.019180 11.00000 -1.20000 AFIX 0 C34 1 0.423734 0.253061 0.091362 11.00000 0.04044 0.05285 = 0.07501 0.02582 -0.00156 0.00618 AFIX 23 H34A 2 0.449494 0.187541 0.059921 11.00000 -1.20000 H34B 2 0.401117 0.248150 0.147638 11.00000 -1.20000 AFIX 0 B1 3 0.204515 0.267030 0.308210 11.00000 0.08958 0.11495 = 0.10350 0.04437 0.02289 0.04940 F10 4 0.199787 0.173073 0.239712 11.00000 0.12567 0.14893 = 0.16731 0.00063 0.02707 0.03715 PART 1 F11A 4 0.119707 0.252335 0.368037 10.50000 0.13906 0.21413 = 0.15172 0.05789 0.08431 0.04585 PART 0 PART 2 F11B 4 0.226554 0.241215 0.374088 10.50000 0.17182 0.39211 = 0.17862 0.20945 -0.02997 -0.00880 PART 0 PART 1 F12A 4 0.171759 0.337396 0.275415 10.50000 0.23401 0.28102 = 0.11814 0.07894 0.03191 0.18560 PART 0 PART 2 F12B 4 0.097004 0.292868 0.299148 10.50000 0.10299 0.34907 = 0.14725 -0.05734 -0.05370 0.14666 PART 0 PART 1 F13A 4 0.323730 0.319581 0.351419 10.50000 0.08709 0.18945 = 0.23440 -0.03059 -0.06462 0.07641 PART 0 PART 2 F13B 4 0.324326 0.346671 0.311038 10.50000 0.13991 0.14134 = 0.14689 0.00543 0.04837 -0.00731 HKLF 4 REM 1563b_a.res in P-1 REM R1 = 0.0547 for 5689 Fo > 4sig(Fo) and 0.0965 for all 9092 data REM 456 parameters refined using 1 restraints END WGHT 0.0383 0.0000 REM Highest difference peak 0.458, deepest hole -0.612, 1-sigma level 0.069 Q1 1 0.8056 0.5668 0.1376 11.00000 0.05 0.46 ; _shelx_res_checksum 97845 _shelx_fab_file ; -14 8 1 -0.2309 0.0038 -13 -1 2 0.3582 -0.0056 -13 -1 3 -0.4837 0.0111 -13 -1 4 -0.7802 -0.0008 -13 -1 5 0.8424 -0.0101 -13 0 1 0.2148 -0.0001 -13 0 2 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0.4195 0.0031 11 -8 6 0.2842 0.0006 11 -8 7 0.2078 -0.0018 11 -8 8 -1.4715 0.0047 11 -8 9 1.4939 -0.0003 11 -8 10 -0.3699 0.0038 11 -7 0 -0.2447 -0.0043 11 -7 1 -1.8203 0.0013 11 -7 2 0.4046 0.0059 11 -7 3 0.6677 -0.0057 11 -7 4 -0.7367 0.0010 11 -7 5 0.6336 -0.0003 11 -7 6 -0.1318 -0.0033 11 -7 7 0.3823 0.0011 11 -7 8 -1.3960 -0.0013 11 -7 9 1.1132 0.0040 11 -6 0 1.0234 -0.0045 11 -6 1 -1.3766 -0.0026 11 -6 2 0.0636 0.0057 11 -6 3 -0.2142 -0.0025 11 -6 4 -0.2874 0.0011 11 -6 5 1.2907 0.0020 11 -6 6 -0.5470 -0.0025 11 -6 7 0.3113 -0.0014 11 -6 8 -1.1516 -0.0020 11 -6 9 1.0885 0.0038 11 -5 0 1.1455 -0.0003 11 -5 1 -0.5763 -0.0032 11 -5 2 0.3142 0.0014 11 -5 3 -0.9169 0.0013 11 -5 4 -0.4381 -0.0025 11 -5 5 1.4329 0.0009 11 -5 6 -0.3711 0.0026 11 -5 7 0.1188 -0.0031 11 -5 8 -0.7501 0.0023 11 -5 9 1.1989 -0.0017 11 -5 10 -0.4349 0.0053 11 -5 11 -0.5048 0.0020 11 -5 12 -0.5341 -0.0190 11 -4 0 0.5729 0.0030 11 -4 1 -0.0647 -0.0009 11 -4 2 0.5460 -0.0030 11 -4 3 -0.8759 0.0040 11 -4 4 -0.4327 -0.0000 11 -4 5 0.7560 -0.0032 11 -4 6 0.1367 -0.0002 11 -4 7 -0.5587 -0.0013 11 -4 8 -0.1387 0.0046 11 -4 9 1.2119 -0.0040 11 -4 10 -0.4451 0.0144 11 -4 11 -0.3753 0.0007 11 -4 12 0.1311 -0.0276 11 -3 0 -0.0502 0.0029 11 -3 1 0.1567 0.0019 11 -3 2 0.9050 -0.0034 11 -3 3 -0.6748 -0.0005 11 -3 4 -0.2153 0.0044 11 -3 5 0.0620 0.0003 11 -3 6 0.9064 -0.0045 11 -3 7 -1.3994 0.0010 11 -3 8 0.1263 -0.0017 11 -3 9 0.4302 -0.0055 11 -3 10 0.4890 0.0245 11 -3 11 -0.2321 0.0026 11 -3 12 0.2131 -0.0299 11 -2 0 -0.6175 0.0006 11 -2 1 -0.1958 -0.0010 11 -2 2 1.1769 0.0016 11 -2 3 -0.0865 -0.0029 11 -2 4 -0.2144 0.0002 11 -2 5 -0.2726 0.0015 11 -2 6 1.4538 -0.0007 11 -2 7 -1.5027 0.0049 11 -2 8 0.4069 -0.0058 11 -2 9 -0.8934 -0.0097 11 -2 10 0.3356 0.0269 11 -1 0 -0.7692 0.0033 11 -1 1 -0.6994 -0.0057 11 -1 2 0.4222 0.0001 11 -1 3 0.6389 0.0019 11 -1 4 -0.1061 -0.0032 11 -1 5 -0.3450 -0.0035 11 -1 6 1.4850 0.0025 11 -1 7 -1.2201 0.0020 11 -1 8 0.9818 -0.0033 11 -1 9 -1.0144 -0.0031 11 0 0 -0.1192 0.0057 11 0 1 -0.7747 -0.0001 11 0 2 -0.8809 -0.0037 11 0 3 0.5807 0.0030 11 0 4 0.4253 -0.0046 11 0 5 -0.6458 -0.0025 11 0 6 1.4212 0.0058 11 0 7 -0.9338 -0.0077 11 0 8 1.0477 -0.0130 11 1 0 1.5379 0.0003 11 1 1 -0.5049 0.0042 11 1 2 -1.6177 0.0002 11 1 3 -0.2589 0.0026 11 1 4 1.1637 -0.0061 11 1 5 -1.1504 0.0020 11 1 6 1.0739 0.0094 11 1 7 -0.3966 -0.0061 11 2 0 2.9993 -0.0012 11 2 1 0.2879 -0.0000 11 2 2 -1.3524 0.0002 11 2 3 -0.9950 -0.0036 11 2 4 1.1587 0.0001 11 2 5 -0.9920 0.0111 11 3 0 2.1446 0.0009 11 3 1 0.9688 0.0009 11 3 2 -0.2265 -0.0023 11 3 3 -0.5458 -0.0232 11 4 0 -0.1105 0.0051 12 -11 0 -1.4671 0.0027 12 -11 1 0.3614 0.0134 12 -11 2 -1.5106 -0.0104 12 -11 3 -0.3184 -0.0021 12 -11 4 2.4123 0.0155 12 -11 5 -0.1586 -0.0037 12 -10 0 -0.8694 -0.0052 12 -10 1 0.3007 -0.0005 12 -10 2 -1.6146 -0.0035 12 -10 3 -0.5832 0.0015 12 -10 4 1.5812 0.0010 12 -10 5 0.7818 0.0044 12 -10 6 -1.3396 0.0080 12 -9 0 -0.3912 -0.0010 12 -9 1 -0.4545 -0.0062 12 -9 2 -0.6888 -0.0013 12 -9 3 -0.2163 0.0043 12 -9 4 -0.2938 -0.0081 12 -9 5 1.0888 0.0049 12 -9 6 0.0423 0.0031 12 -9 7 0.2760 0.0015 12 -8 0 0.6102 -0.0003 12 -8 1 -1.4408 -0.0044 12 -8 2 -0.4955 0.0018 12 -8 3 0.8764 0.0033 12 -8 4 -1.2759 -0.0022 12 -8 5 0.6698 -0.0022 12 -8 6 0.4669 -0.0031 12 -8 7 0.5924 0.0032 12 -8 8 -1.6332 0.0010 12 -7 0 1.7113 -0.0041 12 -7 1 -1.1430 -0.0022 12 -7 2 -0.7892 0.0015 12 -7 3 0.6432 -0.0019 12 -7 4 -1.0739 0.0091 12 -7 5 0.9629 -0.0029 12 -7 6 0.1418 -0.0074 12 -7 7 0.2662 0.0011 12 -7 8 -1.0914 0.0028 12 -6 0 1.7623 -0.0066 12 -6 1 -0.3052 0.0028 12 -6 2 -0.1665 -0.0000 12 -6 3 -0.3530 -0.0067 12 -6 4 -1.2523 0.0067 12 -6 5 1.4978 0.0019 12 -6 6 0.3264 -0.0017 12 -6 7 -0.3411 -0.0037 12 -6 8 -0.8757 0.0027 12 -5 0 1.2544 -0.0074 12 -5 1 0.0518 0.0050 12 -5 2 0.3125 0.0003 12 -5 3 -0.3343 -0.0008 12 -5 4 -1.5067 -0.0032 12 -5 5 1.1734 -0.0016 12 -5 6 0.6268 0.0052 12 -4 0 0.6487 -0.0027 12 -4 1 0.5174 0.0028 12 -4 2 0.0195 -0.0028 12 -4 3 0.1035 0.0061 12 -4 4 -1.0552 -0.0017 12 -4 5 0.4729 -0.0058 12 -4 6 0.8349 0.0003 12 -4 7 -0.7637 0.0012 12 -4 8 -0.9757 0.0057 12 -4 9 1.2698 -0.0128 12 -3 0 -0.2370 0.0031 12 -3 1 0.5754 0.0009 12 -3 2 0.1085 -0.0029 12 -3 3 0.2645 0.0013 12 -3 4 -0.4746 0.0041 12 -3 5 -0.0374 -0.0018 12 -3 6 1.3042 -0.0089 12 -3 7 -1.0916 0.0104 12 -3 8 -0.6375 0.0011 12 -3 9 0.2433 -0.0160 12 -2 0 -0.5998 0.0048 12 -2 1 -0.4344 -0.0027 12 -2 2 0.3048 0.0020 12 -2 3 0.5098 -0.0047 12 -2 4 -0.2791 0.0042 12 -2 5 -0.1241 0.0012 12 -2 6 1.5973 -0.0139 12 -2 7 -1.2100 0.0156 12 -2 8 0.1876 0.0008 12 -2 9 -0.6939 -0.0153 12 -1 0 -0.1145 0.0038 12 -1 1 -1.1768 -0.0026 12 -1 2 -0.2927 0.0023 12 -1 3 0.6558 -0.0038 12 -1 4 -0.3821 0.0012 12 -1 5 0.1638 -0.0002 12 -1 6 1.5253 -0.0092 12 -1 7 -1.2024 0.0064 12 0 0 0.6795 -0.0029 12 0 1 -0.7793 0.0051 12 0 2 -1.1265 -0.0014 12 0 3 0.1437 0.0023 12 0 4 -0.1715 -0.0020 12 0 5 0.1576 -0.0055 12 0 6 1.2326 0.0057 12 1 0 1.7347 -0.0120 12 1 1 0.1973 0.0116 12 1 2 -1.1706 -0.0074 12 1 3 -1.1496 0.0061 12 1 4 0.5944 0.0010 12 2 0 2.2608 -0.0154 12 2 1 0.9529 0.0142 13 -10 0 -0.3364 0.0032 13 -10 1 0.4968 -0.0063 13 -10 2 -1.6639 -0.0075 13 -9 0 0.5849 0.0101 13 -9 1 -0.3511 -0.0171 13 -9 2 -1.2441 -0.0028 13 -9 3 0.6513 0.0201 13 -9 4 -1.1262 -0.0152 13 -8 0 1.9367 0.0123 13 -8 1 -0.5507 -0.0193 13 -8 2 -1.6301 -0.0049 13 -8 3 1.2150 0.0196 13 -8 4 -1.1377 -0.0037 13 -8 5 0.4751 -0.0038 13 -7 0 2.0031 0.0088 13 -7 1 0.2746 -0.0093 13 -7 2 -1.3212 -0.0063 13 -7 3 0.5627 0.0016 13 -7 4 -1.1838 0.0085 13 -7 5 0.8956 0.0001 13 -6 0 1.2619 -0.0030 13 -6 1 0.4989 0.0026 13 -6 2 -0.3565 0.0033 13 -6 3 0.1210 -0.0094 13 -6 4 -1.3528 -0.0001 13 -6 5 0.6454 0.0018 13 -6 6 0.8680 0.0013 13 -5 0 1.0335 -0.0097 13 -5 1 0.5679 0.0032 13 -5 2 -0.3763 0.0081 13 -5 3 0.2408 0.0015 13 -5 4 -0.8919 -0.0104 13 -5 5 0.1483 -0.0051 13 -5 6 0.7976 0.0048 13 -4 0 0.6351 -0.0041 13 -4 1 1.2132 0.0034 13 -4 2 -0.9455 0.0016 13 -4 3 0.3057 0.0095 13 -4 4 -0.3120 -0.0072 13 -4 5 0.0759 -0.0061 13 -4 6 0.5850 -0.0020 13 -3 0 0.0313 0.0001 13 -3 1 1.1519 0.0045 13 -3 2 -1.0464 0.0016 13 -3 3 0.4100 0.0038 13 -3 4 -0.0853 -0.0024 13 -3 5 -0.0011 0.0005 13 -2 0 0.2259 0.0018 13 -2 1 0.1284 -0.0011 13 -2 2 -0.9472 0.0062 13 -2 3 0.6039 -0.0021 13 -2 4 -0.2436 -0.0005 13 -2 5 0.0095 0.0063 13 -1 0 0.7230 0.0029 13 -1 1 -0.5566 -0.0011 13 -1 2 -1.0142 0.0039 13 -1 3 0.7934 -0.0025 13 -1 4 -0.8126 -0.0010 13 0 0 0.8328 -0.0073 13 0 1 -0.2955 0.0094 13 0 2 -1.0955 -0.0017 14 -8 0 1.3119 0.0217 14 -8 1 0.0144 -0.0194 14 -8 2 -0.7385 -0.0174 14 -7 0 0.8159 0.0153 14 -7 1 0.1704 -0.0051 14 -7 2 -0.1450 -0.0103 14 -7 3 0.0054 0.0062 14 -6 1 -0.1172 -0.0015 14 -6 2 0.1912 0.0069 14 -6 3 0.0065 0.0018 14 -5 2 -0.0870 0.0079 14 -5 3 -0.2429 0.0113 0 0 0 0.0 0.0 ; _shelx_fab_checksum 73651 _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 ; loop_ _space_group_symop_operation_xyz 'x, y, z' '-x, -y, -z' loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_occupancy _atom_site_site_symmetry_order _atom_site_calc_flag _atom_site_refinement_flags_posn _atom_site_refinement_flags_adp _atom_site_refinement_flags_occupancy _atom_site_disorder_assembly _atom_site_disorder_group C1 C 0.6954(5) 0.2720(3) 0.3924(3) 0.0596(11) Uani 1 1 d . . . . . F1 F 0.5752(3) -0.0534(2) 0.1498(2) 0.0958(9) Uani 1 1 d . . . . . N1 N 0.6996(4) 0.5439(3) 0.3621(3) 0.0708(11) Uani 1 1 d . . . . . P1 P 0.69791(9) 0.35827(7) 0.16737(7) 0.0386(2) Uani 1 1 d . . . . . Pd1 Pd 0.67251(3) 0.37002(2) 0.30897(2) 0.04887(12) Uani 1 1 d . . . . . C2 C 0.6143(6) 0.3320(4) 0.4401(4) 0.0688(13) Uani 1 1 d . . . . . H2 H 0.527(4) 0.316(3) 0.417(3) 0.044(11) Uiso 1 1 d . . . . . F2 F 0.5414(4) -0.2510(2) 0.1714(3) 0.1379(15) Uani 1 1 d . . . . . C3 C 0.6689(7) 0.4135(4) 0.5237(4) 0.0893(16) Uani 1 1 d . . . . . H3 H 0.6150 0.4533 0.5554 0.107 Uiso 1 1 calc R . . . . F3 F 0.4413(4) -0.2864(2) 0.3144(3) 0.1381(15) Uani 1 1 d . . . . . C4 C 0.7992(8) 0.4345(5) 0.5585(4) 0.108(2) Uani 1 1 d . . . . . H4 H 0.8338 0.4881 0.6143 0.130 Uiso 1 1 calc R . . . . F4 F 0.3686(4) -0.1224(3) 0.4337(3) 0.1442(15) Uani 1 1 d . . . . . C5 C 0.8804(7) 0.3781(5) 0.5127(5) 0.107(2) Uani 1 1 d . . . . . H5 H 0.9700 0.3939 0.5376 0.129 Uiso 1 1 calc R . . . . F5 F 0.3981(4) 0.0733(3) 0.4113(2) 0.1151(12) Uani 1 1 d . . . . . C6 C 0.8318(5) 0.2984(4) 0.4305(4) 0.0822(15) Uani 1 1 d . . . . . H6 H 0.8889 0.2615 0.3997 0.099 Uiso 1 1 calc R . . . . C7 C 0.6481(4) 0.2066(3) 0.2991(3) 0.0557(11) Uani 1 1 d . . . . . H7 H 0.7172 0.1775 0.2687 0.067 Uiso 1 1 calc R . . . . C8 C 0.5040(4) 0.1268(3) 0.2656(3) 0.0632(12) Uani 1 1 d . . . . . H8A H 0.4831 0.1123 0.2034 0.076 Uiso 1 1 calc R . . . . H8B H 0.4399 0.1614 0.2960 0.076 Uiso 1 1 calc R . . . . C9 C 0.4866(4) 0.0165(3) 0.2798(3) 0.0589(11) Uani 1 1 d . . . . . C10 C 0.4364(5) -0.0049(4) 0.3504(4) 0.0796(14) Uani 1 1 d . . . . . C11 C 0.4202(6) -0.1076(5) 0.3622(4) 0.0911(17) Uani 1 1 d . . . . . C12 C 0.4571(6) -0.1884(4) 0.3024(5) 0.0924(19) Uani 1 1 d . . . . . C13 C 0.5076(5) -0.1695(4) 0.2324(5) 0.0881(17) Uani 1 1 d . . . . . C14 C 0.5236(5) -0.0688(4) 0.2213(4) 0.0707(13) Uani 1 1 d . . . . . C15 C 0.7150(5) 0.6340(4) 0.3984(3) 0.0737(14) Uani 1 1 d . . . . . C16 C 0.7378(9) 0.7541(4) 0.4458(5) 0.146(3) Uani 1 1 d . . . . . H16A H 0.7275 0.7900 0.4046 0.218 Uiso 1 1 calc GR . . . . H16B H 0.8287 0.7886 0.4780 0.218 Uiso 1 1 calc GR . . . . H16C H 0.6720 0.7621 0.4858 0.218 Uiso 1 1 calc GR . . . . C17 C 0.8355(4) 0.4877(3) 0.1739(3) 0.0478(9) Uani 1 1 d . . . . . H17 H 0.7988 0.5479 0.2050 0.057 Uiso 1 1 calc R . . . . C18 C 0.9660(4) 0.5128(3) 0.2349(3) 0.0615(12) Uani 1 1 d . . . . . H18A H 0.9417 0.5036 0.2897 0.074 Uiso 1 1 calc R . . . . H18B H 1.0130 0.4594 0.2079 0.074 Uiso 1 1 calc R . . . . C19 C 1.0611(5) 0.6312(4) 0.2536(4) 0.0920(17) Uani 1 1 d . . . . . H19A H 1.0203 0.6843 0.2901 0.110 Uiso 1 1 calc R . . . . H19B H 1.1469 0.6410 0.2865 0.110 Uiso 1 1 calc R . . . . C20 C 1.0900(5) 0.6576(4) 0.1729(4) 0.0806(15) Uani 1 1 d . . . . . H20A H 1.1462 0.6146 0.1419 0.097 Uiso 1 1 calc R . . . . H20B H 1.1419 0.7369 0.1894 0.097 Uiso 1 1 calc R . . . . C21 C 0.9614(4) 0.6315(4) 0.1123(3) 0.0680(13) Uani 1 1 d . . . . . H21A H 0.9861 0.6423 0.0580 0.082 Uiso 1 1 calc R . . . . H21B H 0.9124 0.6832 0.1394 0.082 Uiso 1 1 calc R . . . . C22 C 0.8672(4) 0.5098(4) 0.0914(3) 0.0651(12) Uani 1 1 d . . . . . H22A H 0.7826 0.4974 0.0560 0.078 Uiso 1 1 calc R . . . . H22B H 0.9117 0.4578 0.0579 0.078 Uiso 1 1 calc R . . . . C23 C 0.7354(3) 0.2322(3) 0.0963(3) 0.0442(9) Uani 1 1 d . . . . . H23 H 0.6660 0.1677 0.1029 0.053 Uiso 1 1 calc R . . . . C24 C 0.8735(4) 0.2263(3) 0.1282(3) 0.0568(11) Uani 1 1 d . . . . . H24A H 0.8805 0.2387 0.1905 0.068 Uiso 1 1 calc R . . . . H24B H 0.9473 0.2851 0.1193 0.068 Uiso 1 1 calc R . . . . C25 C 0.8881(5) 0.1109(4) 0.0780(4) 0.0759(15) Uani 1 1 d . . . . . H25A H 0.9770 0.1093 0.0980 0.091 Uiso 1 1 calc R . . . . H25B H 0.8181 0.0526 0.0902 0.091 Uiso 1 1 calc R . . . . C26 C 0.8744(5) 0.0875(4) -0.0185(4) 0.0797(16) Uani 1 1 d . . . . . H26A H 0.8781 0.0123 -0.0487 0.096 Uiso 1 1 calc R . . . . H26B H 0.9509 0.1407 -0.0313 0.096 Uiso 1 1 calc R . . . . C27 C 0.7412(5) 0.0966(3) -0.0528(3) 0.0709(13) Uani 1 1 d . . . . . H27A H 0.6649 0.0363 -0.0479 0.085 Uiso 1 1 calc R . . . . H27B H 0.7400 0.0875 -0.1144 0.085 Uiso 1 1 calc R . . . . C28 C 0.7232(4) 0.2102(3) -0.0019(3) 0.0536(10) Uani 1 1 d . . . . . H28A H 0.7926 0.2700 -0.0130 0.064 Uiso 1 1 calc R . . . . H28B H 0.6339 0.2106 -0.0224 0.064 Uiso 1 1 calc R . . . . C29 C 0.5449(3) 0.3601(3) 0.1063(3) 0.0443(9) Uani 1 1 d . . . . . H29 H 0.5671 0.3627 0.0488 0.053 Uiso 1 1 calc R . . . . C30 C 0.5026(4) 0.4641(3) 0.1537(3) 0.0643(13) Uani 1 1 d . . . . . H30A H 0.4813 0.4639 0.2113 0.077 Uiso 1 1 calc R . . . . H30B H 0.5780 0.5321 0.1615 0.077 Uiso 1 1 calc R . . . . C31 C 0.3767(4) 0.4630(4) 0.0999(4) 0.0740(15) Uani 1 1 d . . . . . H31A H 0.3500 0.5282 0.1308 0.089 Uiso 1 1 calc R . . . . H31B H 0.4002 0.4680 0.0437 0.089 Uiso 1 1 calc R . . . . C32 C 0.2581(4) 0.3573(4) 0.0845(3) 0.0722(14) Uani 1 1 d . . . . . H32A H 0.1812 0.3574 0.0485 0.087 Uiso 1 1 calc R . . . . H32B H 0.2294 0.3553 0.1403 0.087 Uiso 1 1 calc R . . . . C33 C 0.2987(4) 0.2532(4) 0.0390(3) 0.0720(13) Uani 1 1 d . . . . . H33A H 0.2226 0.1861 0.0323 0.086 Uiso 1 1 calc R . . . . H33B H 0.3189 0.2516 -0.0192 0.086 Uiso 1 1 calc R . . . . C34 C 0.4237(4) 0.2531(3) 0.0914(3) 0.0575(11) Uani 1 1 d . . . . . H34A H 0.4495 0.1875 0.0599 0.069 Uiso 1 1 calc R . . . . H34B H 0.4011 0.2482 0.1476 0.069 Uiso 1 1 calc R . . . . B1 B 0.2045(9) 0.2670(8) 0.3082(6) 0.097(2) Uani 1 1 d . . . . . F10 F 0.1998(4) 0.1731(4) 0.2397(4) 0.1630(18) Uani 1 1 d . . . . . F11A F 0.120(2) 0.2523(11) 0.3680(13) 0.171(5) Uani 0.5 1 d . . P A 1 F11B F 0.227(2) 0.2412(16) 0.3741(10) 0.243(9) Uani 0.5 1 d . . P A 2 F12A F 0.172(2) 0.3374(18) 0.2754(10) 0.185(7) Uani 0.5 1 d D . P A 1 F12B F 0.0970(16) 0.293(2) 0.2991(13) 0.222(13) Uani 0.5 1 d . . P A 2 F13A F 0.3237(16) 0.320(2) 0.3514(16) 0.192(11) Uani 0.5 1 d D . P A 1 F13B F 0.3243(19) 0.3467(18) 0.3110(13) 0.166(9) Uani 0.5 1 d . . P A 2 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 C1 0.065(3) 0.057(2) 0.056(3) 0.034(2) -0.005(2) 0.006(2) F1 0.112(2) 0.0743(18) 0.087(3) 0.0199(18) 0.023(2) 0.0178(17) N1 0.107(3) 0.050(2) 0.054(3) 0.017(2) 0.009(2) 0.025(2) P1 0.0347(5) 0.0390(5) 0.0407(6) 0.0142(4) 0.0008(4) 0.0103(4) Pd1 0.0577(2) 0.04372(17) 0.0430(2) 0.01520(14) 0.00261(15) 0.01363(14) C2 0.073(3) 0.081(3) 0.055(4) 0.035(3) 0.003(3) 0.017(3) F2 0.163(3) 0.0650(18) 0.178(4) 0.026(2) 0.045(3) 0.041(2) C3 0.130(5) 0.081(4) 0.047(4) 0.020(3) 0.005(4) 0.022(4) F3 0.147(3) 0.077(2) 0.199(5) 0.084(3) -0.008(3) 0.013(2) C4 0.145(6) 0.088(4) 0.065(5) 0.025(4) -0.034(4) 0.005(4) F4 0.192(4) 0.133(3) 0.108(4) 0.077(3) 0.032(3) 0.014(3) C5 0.100(5) 0.107(5) 0.092(6) 0.037(4) -0.045(4) 0.007(4) F5 0.154(3) 0.097(2) 0.089(3) 0.028(2) 0.043(2) 0.035(2) C6 0.084(4) 0.080(3) 0.084(5) 0.040(3) -0.014(3) 0.018(3) C7 0.055(2) 0.052(2) 0.063(3) 0.029(2) 0.000(2) 0.013(2) C8 0.067(3) 0.053(2) 0.067(4) 0.024(2) -0.004(2) 0.015(2) C9 0.062(3) 0.048(2) 0.056(3) 0.017(2) -0.005(2) 0.005(2) C10 0.088(4) 0.071(3) 0.073(4) 0.026(3) 0.009(3) 0.014(3) C11 0.104(4) 0.080(4) 0.082(5) 0.048(4) 0.000(4) -0.001(3) C12 0.090(4) 0.062(3) 0.125(6) 0.050(4) -0.004(4) 0.007(3) C13 0.085(4) 0.050(3) 0.118(6) 0.023(3) 0.007(4) 0.014(3) C14 0.072(3) 0.058(3) 0.075(4) 0.026(3) 0.002(3) 0.008(2) C15 0.110(4) 0.061(3) 0.051(3) 0.021(3) 0.012(3) 0.027(3) C16 0.254(9) 0.052(3) 0.104(6) 0.004(3) 0.009(6) 0.040(5) C17 0.042(2) 0.049(2) 0.049(3) 0.021(2) -0.0022(19) 0.0051(18) C18 0.048(2) 0.061(2) 0.066(3) 0.028(2) -0.021(2) 0.001(2) C19 0.068(3) 0.087(3) 0.095(5) 0.042(3) -0.029(3) -0.021(3) C20 0.059(3) 0.078(3) 0.095(5) 0.047(3) -0.007(3) -0.009(2) C21 0.061(3) 0.070(3) 0.073(4) 0.042(3) 0.003(3) 0.001(2) C22 0.055(3) 0.073(3) 0.060(3) 0.029(3) 0.001(2) 0.004(2) C23 0.0379(19) 0.0415(19) 0.051(3) 0.0136(19) 0.0049(18) 0.0124(17) C24 0.046(2) 0.064(2) 0.062(3) 0.019(2) 0.005(2) 0.025(2) C25 0.072(3) 0.076(3) 0.092(5) 0.026(3) 0.017(3) 0.046(3) C26 0.076(3) 0.062(3) 0.099(5) 0.011(3) 0.021(3) 0.037(3) C27 0.072(3) 0.057(3) 0.066(4) 0.000(2) 0.008(3) 0.020(2) C28 0.052(2) 0.052(2) 0.050(3) 0.010(2) 0.005(2) 0.017(2) C29 0.0369(19) 0.052(2) 0.048(3) 0.022(2) 0.0025(18) 0.0151(17) C30 0.048(2) 0.060(2) 0.086(4) 0.019(3) 0.001(2) 0.028(2) C31 0.054(3) 0.075(3) 0.106(5) 0.038(3) 0.002(3) 0.035(3) C32 0.043(2) 0.103(4) 0.085(4) 0.048(3) 0.005(2) 0.028(3) C33 0.042(2) 0.077(3) 0.085(4) 0.028(3) -0.011(2) 0.004(2) C34 0.040(2) 0.053(2) 0.075(4) 0.026(2) -0.002(2) 0.0062(19) B1 0.090(6) 0.115(6) 0.103(7) 0.044(6) 0.023(6) 0.049(5) F10 0.126(3) 0.149(3) 0.167(5) 0.001(4) 0.027(3) 0.037(3) F11A 0.139(10) 0.214(10) 0.152(13) 0.058(10) 0.084(11) 0.046(10) F11B 0.172(14) 0.39(2) 0.179(14) 0.209(16) -0.030(12) -0.009(16) F12A 0.234(19) 0.281(16) 0.118(9) 0.079(10) 0.032(12) 0.186(17) F12B 0.103(9) 0.35(3) 0.147(17) -0.057(15) -0.054(9) 0.147(14) F13A 0.087(11) 0.189(17) 0.23(2) -0.031(13) -0.065(12) 0.076(12) F13B 0.140(15) 0.141(10) 0.147(14) 0.005(9) 0.048(12) -0.007(9) 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' B B 0.0013 0.0007 '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' 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' Pd Pd -0.9988 1.0072 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' loop_ _exptl_crystal_face_index_h _exptl_crystal_face_index_k _exptl_crystal_face_index_l _exptl_crystal_face_perp_dist -7 18 -12 0.0904 7 -18 12 0.0904 -5 -1 -18 0.1501 5 1 18 0.1501 12 2 -11 0.0557 -12 -2 11 0.0557 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 C2 C1 Pd1 80.0(2) . . ? C2 C1 C6 117.8(5) . . ? C2 C1 C7 118.5(4) . . ? C6 C1 Pd1 113.9(3) . . ? C6 C1 C7 121.9(5) . . ? C7 C1 Pd1 64.39(19) . . ? C15 N1 Pd1 172.6(4) . . ? C17 P1 Pd1 106.42(14) . . ? C17 P1 C23 110.31(17) . . ? C23 P1 Pd1 116.58(12) . . ? C29 P1 Pd1 113.06(12) . . ? C29 P1 C17 105.43(15) . . ? C29 P1 C23 104.55(17) . . ? C1 Pd1 P1 136.23(13) . . ? C1 Pd1 C2 35.04(16) . . ? N1 Pd1 C1 122.17(17) . . ? N1 Pd1 P1 97.76(10) . . ? N1 Pd1 C2 95.70(16) . . ? P1 Pd1 C2 165.36(14) . . ? C7 Pd1 C1 39.83(16) . . ? C7 Pd1 N1 161.56(16) . . ? C7 Pd1 P1 100.51(13) . . ? C7 Pd1 C2 66.42(18) . . ? C1 C2 Pd1 65.0(2) . . ? C1 C2 H2 119(3) . . ? C1 C2 C3 119.8(5) . . ? Pd1 C2 H2 85(2) . . ? C3 C2 Pd1 121.3(3) . . ? C3 C2 H2 121(3) . . ? C2 C3 H3 119.8 . . ? C4 C3 C2 120.4(6) . . ? C4 C3 H3 119.8 . . ? C3 C4 H4 119.6 . . ? C3 C4 C5 120.8(6) . . ? C5 C4 H4 119.6 . . ? C4 C5 H5 119.6 . . ? C4 C5 C6 120.8(6) . . ? C6 C5 H5 119.6 . . ? C1 C6 H6 119.8 . . ? C5 C6 C1 120.3(5) . . ? C5 C6 H6 119.8 . . ? C1 C7 Pd1 75.8(2) . . ? C1 C7 H7 113.0 . . ? C1 C7 C8 122.3(4) . . ? Pd1 C7 H7 113.0 . . ? C8 C7 Pd1 114.4(2) . . ? C8 C7 H7 113.0 . . ? C7 C8 H8A 109.4 . . ? C7 C8 H8B 109.4 . . ? C7 C8 C9 111.1(3) . . ? H8A C8 H8B 108.0 . . ? C9 C8 H8A 109.4 . . ? C9 C8 H8B 109.4 . . ? C10 C9 C8 122.9(4) . . ? C10 C9 C14 115.5(4) . . ? C14 C9 C8 121.5(4) . . ? F5 C10 C9 120.0(4) . . ? F5 C10 C11 117.8(5) . . ? C9 C10 C11 122.2(5) . . ? F4 C11 C10 118.5(6) . . ? F4 C11 C12 121.9(5) . . ? C12 C11 C10 119.6(5) . . ? F3 C12 C11 119.1(6) . . ? C13 C12 F3 121.4(6) . . ? C13 C12 C11 119.5(4) . . ? F2 C13 C14 119.7(6) . . ? C12 C13 F2 119.7(5) . . ? C12 C13 C14 120.6(5) . . ? F1 C14 C9 119.0(4) . . ? F1 C14 C13 118.5(5) . . ? C13 C14 C9 122.5(5) . . ? N1 C15 C16 179.0(6) . . ? C15 C16 H16A 109.5 . . ? C15 C16 H16B 109.5 . . ? C15 C16 H16C 109.5 . . ? H16A C16 H16B 109.5 . . ? H16A C16 H16C 109.5 . . ? H16B C16 H16C 109.5 . . ? P1 C17 H17 103.2 . . ? C18 C17 P1 114.0(2) . . ? C18 C17 H17 103.2 . . ? C22 C17 P1 119.1(3) . . ? C22 C17 H17 103.2 . . ? C22 C17 C18 111.7(3) . . ? C17 C18 H18A 109.4 . . ? C17 C18 H18B 109.4 . . ? H18A C18 H18B 108.0 . . ? C19 C18 C17 111.3(3) . . ? C19 C18 H18A 109.4 . . ? C19 C18 H18B 109.4 . . ? C18 C19 H19A 108.9 . . ? C18 C19 H19B 108.9 . . ? H19A C19 H19B 107.8 . . ? C20 C19 C18 113.2(5) . . ? C20 C19 H19A 108.9 . . ? C20 C19 H19B 108.9 . . ? C19 C20 H20A 109.0 . . ? C19 C20 H20B 109.0 . . ? C19 C20 C21 112.7(4) . . ? H20A C20 H20B 107.8 . . ? C21 C20 H20A 109.0 . . ? C21 C20 H20B 109.0 . . ? C20 C21 H21A 109.3 . . ? C20 C21 H21B 109.3 . . ? C20 C21 C22 111.5(3) . . ? H21A C21 H21B 108.0 . . ? C22 C21 H21A 109.3 . . ? C22 C21 H21B 109.3 . . ? C17 C22 C21 110.7(4) . . ? C17 C22 H22A 109.5 . . ? C17 C22 H22B 109.5 . . ? C21 C22 H22A 109.5 . . ? C21 C22 H22B 109.5 . . ? H22A C22 H22B 108.1 . . ? P1 C23 H23 105.5 . . ? C24 C23 P1 112.6(3) . . ? C24 C23 H23 105.5 . . ? C28 C23 P1 117.3(2) . . ? C28 C23 H23 105.5 . . ? C28 C23 C24 109.6(3) . . ? C23 C24 H24A 109.5 . . ? C23 C24 H24B 109.5 . . ? C23 C24 C25 110.6(3) . . ? H24A C24 H24B 108.1 . . ? C25 C24 H24A 109.5 . . ? C25 C24 H24B 109.5 . . ? C24 C25 H25A 109.4 . . ? C24 C25 H25B 109.4 . . ? H25A C25 H25B 108.0 . . ? C26 C25 C24 111.1(3) . . ? C26 C25 H25A 109.4 . . ? C26 C25 H25B 109.4 . . ? C25 C26 H26A 109.2 . . ? C25 C26 H26B 109.2 . . ? C25 C26 C27 111.9(4) . . ? H26A C26 H26B 107.9 . . ? C27 C26 H26A 109.2 . . ? C27 C26 H26B 109.2 . . ? C26 C27 H27A 109.3 . . ? C26 C27 H27B 109.3 . . ? C26 C27 C28 111.8(4) . . ? H27A C27 H27B 107.9 . . ? C28 C27 H27A 109.3 . . ? C28 C27 H27B 109.3 . . ? C23 C28 C27 111.1(3) . . ? C23 C28 H28A 109.4 . . ? C23 C28 H28B 109.4 . . ? C27 C28 H28A 109.4 . . ? C27 C28 H28B 109.4 . . ? H28A C28 H28B 108.0 . . ? P1 C29 H29 108.1 . . ? C30 C29 P1 112.0(3) . . ? C30 C29 H29 108.1 . . ? C34 C29 P1 111.0(2) . . ? C34 C29 H29 108.1 . . ? C34 C29 C30 109.4(3) . . ? C29 C30 H30A 109.6 . . ? C29 C30 H30B 109.6 . . ? H30A C30 H30B 108.2 . . ? C31 C30 C29 110.1(4) . . ? C31 C30 H30A 109.6 . . ? C31 C30 H30B 109.6 . . ? C30 C31 H31A 109.4 . . ? C30 C31 H31B 109.4 . . ? H31A C31 H31B 108.0 . . ? C32 C31 C30 111.3(3) . . ? C32 C31 H31A 109.4 . . ? C32 C31 H31B 109.4 . . ? C31 C32 H32A 109.5 . . ? C31 C32 H32B 109.5 . . ? C31 C32 C33 110.6(3) . . ? H32A C32 H32B 108.1 . . ? C33 C32 H32A 109.5 . . ? C33 C32 H32B 109.5 . . ? C32 C33 H33A 109.4 . . ? C32 C33 H33B 109.4 . . ? H33A C33 H33B 108.0 . . ? C34 C33 C32 111.1(4) . . ? C34 C33 H33A 109.4 . . ? C34 C33 H33B 109.4 . . ? C29 C34 H34A 109.4 . . ? C29 C34 H34B 109.4 . . ? C33 C34 C29 111.0(3) . . ? C33 C34 H34A 109.4 . . ? C33 C34 H34B 109.4 . . ? H34A C34 H34B 108.0 . . ? F11A B1 F10 116.7(9) . . ? F11B B1 F10 102.8(11) . . ? F11B B1 F12B 118.2(14) . . ? F11B B1 F13B 103.1(12) . . ? F12A B1 F10 107.8(11) . . ? F12A B1 F11A 106.9(10) . . ? F12B B1 F10 109.8(11) . . ? F12B B1 F13B 115.4(16) . . ? F13A B1 F10 112.7(10) . . ? F13A B1 F11A 106.0(14) . . ? F13A B1 F12A 106.2(14) . . ? F13B B1 F10 106.1(10) . . ? 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 C1 Pd1 2.212(4) . ? C1 C2 1.401(6) . ? C1 C6 1.412(6) . ? C1 C7 1.462(6) . ? F1 C14 1.345(5) . ? N1 Pd1 2.109(3) . ? N1 C15 1.105(5) . ? P1 Pd1 2.2868(10) . ? P1 C17 1.847(3) . ? P1 C23 1.851(3) . ? P1 C29 1.845(3) . ? Pd1 C2 2.404(5) . ? Pd1 C7 2.058(3) . ? C2 H2 0.89(4) . ? C2 C3 1.402(7) . ? F2 C13 1.348(6) . ? C3 H3 0.9300 . ? C3 C4 1.351(8) . ? F3 C12 1.341(5) . ? C4 H4 0.9300 . ? C4 C5 1.364(8) . ? F4 C11 1.342(6) . ? C5 H5 0.9300 . ? C5 C6 1.371(8) . ? F5 C10 1.344(6) . ? C6 H6 0.9300 . ? C7 H7 0.9800 . ? C7 C8 1.506(5) . ? C8 H8A 0.9700 . ? C8 H8B 0.9700 . ? C8 C9 1.515(5) . ? C9 C10 1.354(6) . ? C9 C14 1.379(6) . ? C10 C11 1.401(6) . ? C11 C12 1.350(8) . ? C12 C13 1.333(8) . ? C13 C14 1.369(6) . ? C15 C16 1.468(6) . ? C16 H16A 0.9600 . ? C16 H16B 0.9600 . ? C16 H16C 0.9600 . ? C17 H17 0.9800 . ? C17 C18 1.528(5) . ? C17 C22 1.491(5) . ? C18 H18A 0.9700 . ? C18 H18B 0.9700 . ? C18 C19 1.511(6) . ? C19 H19A 0.9700 . ? C19 H19B 0.9700 . ? C19 C20 1.482(7) . ? C20 H20A 0.9700 . ? C20 H20B 0.9700 . ? C20 C21 1.506(6) . ? C21 H21A 0.9700 . ? C21 H21B 0.9700 . ? C21 C22 1.537(6) . ? C22 H22A 0.9700 . ? C22 H22B 0.9700 . ? C23 H23 0.9800 . ? C23 C24 1.530(5) . ? C23 C28 1.522(5) . ? C24 H24A 0.9700 . ? C24 H24B 0.9700 . ? C24 C25 1.536(5) . ? C25 H25A 0.9700 . ? C25 H25B 0.9700 . ? C25 C26 1.491(7) . ? C26 H26A 0.9700 . ? C26 H26B 0.9700 . ? C26 C27 1.516(6) . ? C27 H27A 0.9700 . ? C27 H27B 0.9700 . ? C27 C28 1.532(5) . ? C28 H28A 0.9700 . ? C28 H28B 0.9700 . ? C29 H29 0.9800 . ? C29 C30 1.537(5) . ? C29 C34 1.532(5) . ? C30 H30A 0.9700 . ? C30 H30B 0.9700 . ? C30 C31 1.534(5) . ? C31 H31A 0.9700 . ? C31 H31B 0.9700 . ? C31 C32 1.506(6) . ? C32 H32A 0.9700 . ? C32 H32B 0.9700 . ? C32 C33 1.524(6) . ? C33 H33A 0.9700 . ? C33 H33B 0.9700 . ? C33 C34 1.521(5) . ? C34 H34A 0.9700 . ? C34 H34B 0.9700 . ? B1 F10 1.361(9) . ? B1 F11A 1.352(13) . ? B1 F11B 1.259(14) . ? B1 F12A 1.329(15) . ? B1 F12B 1.269(13) . ? B1 F13A 1.268(18) . ? B1 F13B 1.357(19) . ? 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 C1 C2 C3 C4 0.0(7) . . . . ? C1 C7 C8 C9 -78.8(5) . . . . ? P1 C17 C18 C19 -167.1(4) . . . . ? P1 C17 C22 C21 167.9(3) . . . . ? P1 C23 C24 C25 169.6(3) . . . . ? P1 C23 C28 C27 -173.5(3) . . . . ? P1 C29 C30 C31 179.1(3) . . . . ? P1 C29 C34 C33 -178.5(3) . . . . ? Pd1 C1 C2 C3 -113.2(4) . . . . ? Pd1 C1 C6 C5 92.9(5) . . . . ? Pd1 C1 C7 C8 -110.1(3) . . . . ? Pd1 P1 C17 C18 50.3(3) . . . . ? Pd1 P1 C17 C22 -174.4(3) . . . . ? Pd1 P1 C23 C24 -64.0(3) . . . . ? Pd1 P1 C23 C28 167.5(2) . . . . ? Pd1 P1 C29 C30 55.3(3) . . . . ? Pd1 P1 C29 C34 -67.4(3) . . . . ? Pd1 C2 C3 C4 -77.2(6) . . . . ? Pd1 C7 C8 C9 -166.9(3) . . . . ? C2 C1 C6 C5 1.8(7) . . . . ? C2 C1 C7 Pd1 61.3(3) . . . . ? C2 C1 C7 C8 -48.8(5) . . . . ? C2 C3 C4 C5 0.8(9) . . . . ? F2 C13 C14 F1 -1.0(8) . . . . ? F2 C13 C14 C9 177.8(5) . . . . ? C3 C4 C5 C6 -0.3(9) . . . . ? F3 C12 C13 F2 1.2(9) . . . . ? F3 C12 C13 C14 -179.7(5) . . . . ? C4 C5 C6 C1 -1.1(8) . . . . ? F4 C11 C12 F3 0.2(9) . . . . ? F4 C11 C12 C13 179.9(6) . . . . ? F5 C10 C11 F4 -0.5(8) . . . . ? F5 C10 C11 C12 179.8(5) . . . . ? C6 C1 C2 Pd1 111.9(4) . . . . ? C6 C1 C2 C3 -1.3(6) . . . . ? C6 C1 C7 Pd1 -103.4(4) . . . . ? C6 C1 C7 C8 146.5(4) . . . . ? C7 C1 C2 Pd1 -53.5(3) . . . . ? C7 C1 C2 C3 -166.6(4) . . . . ? C7 C1 C6 C5 166.6(4) . . . . ? C7 C8 C9 C10 95.5(5) . . . . ? C7 C8 C9 C14 -83.5(5) . . . . ? C8 C9 C10 F5 0.7(8) . . . . ? C8 C9 C10 C11 179.6(5) . . . . ? C8 C9 C14 F1 -0.5(7) . . . . ? C8 C9 C14 C13 -179.3(5) . . . . ? C9 C10 C11 F4 -179.5(5) . . . . ? C9 C10 C11 C12 0.8(9) . . . . ? C10 C9 C14 F1 -179.6(4) . . . . ? C10 C9 C14 C13 1.6(7) . . . . ? C10 C11 C12 F3 179.9(5) . . . . ? C10 C11 C12 C13 -0.4(9) . . . . ? C11 C12 C13 F2 -178.4(5) . . . . ? C11 C12 C13 C14 0.7(9) . . . . ? C12 C13 C14 F1 179.9(5) . . . . ? C12 C13 C14 C9 -1.3(8) . . . . ? C14 C9 C10 F5 179.7(5) . . . . ? C14 C9 C10 C11 -1.4(8) . . . . ? C17 P1 C23 C24 57.5(3) . . . . ? C17 P1 C23 C28 -71.0(3) . . . . ? C17 P1 C29 C30 -60.6(3) . . . . ? C17 P1 C29 C34 176.8(3) . . . . ? C17 C18 C19 C20 -51.9(6) . . . . ? C18 C17 C22 C21 -55.8(4) . . . . ? C18 C19 C20 C21 51.8(6) . . . . ? C19 C20 C21 C22 -52.8(6) . . . . ? C20 C21 C22 C17 54.9(5) . . . . ? C22 C17 C18 C19 54.3(5) . . . . ? C23 P1 C17 C18 -77.1(3) . . . . ? C23 P1 C17 C22 58.3(3) . . . . ? C23 P1 C29 C30 -176.9(3) . . . . ? C23 P1 C29 C34 60.4(3) . . . . ? C23 C24 C25 C26 57.7(5) . . . . ? C24 C23 C28 C27 56.5(4) . . . . ? C24 C25 C26 C27 -55.3(5) . . . . ? C25 C26 C27 C28 53.9(5) . . . . ? C26 C27 C28 C23 -54.6(5) . . . . ? C28 C23 C24 C25 -58.0(4) . . . . ? C29 P1 C17 C18 170.6(3) . . . . ? C29 P1 C17 C22 -54.1(3) . . . . ? C29 P1 C23 C24 170.4(3) . . . . ? C29 P1 C23 C28 41.9(3) . . . . ? C29 C30 C31 C32 58.1(5) . . . . ? C30 C29 C34 C33 57.4(5) . . . . ? C30 C31 C32 C33 -56.9(6) . . . . ? C31 C32 C33 C34 56.3(5) . . . . ? C32 C33 C34 C29 -57.0(5) . . . . ? C34 C29 C30 C31 -57.4(4) . . . . ? 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 0.000 0.000 0.500 319.0 74.5 ?