#------------------------------------------------------------------------------ #$Date: 2019-12-03 04:03:01 +0200 (Tue, 03 Dec 2019) $ #$Revision: 244869 $ #$URL: file:///home/coder/svn-repositories/cod/cif/7/12/56/7125642.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_7125642 loop_ _publ_author_name 'Takahashi, Rina' 'Kubota, Koji' 'Ito, Hajime' _publ_section_title ; Air- and moisture-stable Xantphos-ligated palladium dialkyl complex as a precatalyst for cross-coupling reactions ; _journal_name_full 'Chemical Communications' _journal_paper_doi 10.1039/C9CC06946A _journal_year 2019 _chemical_formula_moiety 'C47 H54 O P2 Pd Si2' _chemical_formula_sum 'C47 H54 O P2 Pd Si2' _chemical_formula_weight 859.42 _space_group_crystal_system monoclinic _space_group_IT_number 15 _space_group_name_Hall '-C 2yc' _space_group_name_H-M_alt 'C 1 2/c 1' _atom_sites_solution_hydrogens geom _atom_sites_solution_primary direct _audit_creation_date 2019-07-18 _audit_creation_method ; Olex2 1.2 (compiled 2018.05.29 svn.r3508 for OlexSys, GUI svn.r5506) ; _audit_update_record ; 2019-07-18 deposited with the CCDC. 2019-11-20 downloaded from the CCDC. ; _cell_angle_alpha 90 _cell_angle_beta 97.720(2) _cell_angle_gamma 90 _cell_formula_units_Z 8 _cell_length_a 20.6034(4) _cell_length_b 11.5855(2) _cell_length_c 35.7054(8) _cell_measurement_reflns_used 39298 _cell_measurement_temperature 123(2) _cell_measurement_theta_max 29.1650 _cell_measurement_theta_min 2.3390 _cell_volume 8445.7(3) _computing_cell_refinement 'CrysAlisPro 1.171.40.45a (Rigaku OD, 2019)' _computing_data_collection 'CrysAlisPro 1.171.40.45a (Rigaku OD, 2019)' _computing_data_reduction 'CrysAlisPro 1.171.40.45a (Rigaku OD, 2019)' _computing_molecular_graphics 'Olex2 (Dolomanov et al., 2009)' _computing_publication_material 'Olex2 (Dolomanov et al., 2009)' _computing_structure_refinement 'ShelXL (Sheldrick, 2015)' _computing_structure_solution 'ShelXS (Sheldrick, 2008)' _diffrn_ambient_temperature 123(2) _diffrn_detector 'CCD plate' _diffrn_detector_area_resol_mean 5.8140 _diffrn_measured_fraction_theta_full 0.999 _diffrn_measured_fraction_theta_max 0.999 _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 -43.00 6.00 0.50 11.15 -- 5.00 17.00-124.00 98 2 \w -8.00 17.00 0.50 11.15 -- -7.30 17.00-124.00 50 3 \w 52.00 77.00 0.50 11.15 -- 5.00 60.00 90.00 50 4 \w -23.00 3.00 0.50 11.15 -- 5.00 60.00 90.00 52 5 \w -50.00 -24.00 0.50 11.15 -- 5.00 60.00 150.00 52 6 \w 11.00 37.00 0.50 11.15 -- 5.00 60.00 150.00 52 7 \w -77.00 -51.00 0.50 11.15 -- 5.00 60.00 90.00 52 8 \w 14.00 64.00 0.50 11.15 -- -7.30 60.00-120.00 100 9 \w -97.00 -8.00 0.50 11.15 -- -7.30 60.00-120.00 178 10 \w -97.00 62.00 0.50 11.15 -- -7.30 43.00 150.00 318 ; _diffrn_measurement_device 'four-circle diffractometer' _diffrn_measurement_device_type 'XtaLAB AFC11 (RCD3): quarter-chi single' _diffrn_measurement_method '\w scans' _diffrn_orient_matrix_type 'CrysAlisPro convention (1999,Acta A55,543-557)' _diffrn_orient_matrix_UB_11 0.0107261000 _diffrn_orient_matrix_UB_12 -0.0145491000 _diffrn_orient_matrix_UB_13 -0.0174669000 _diffrn_orient_matrix_UB_21 0.0329161000 _diffrn_orient_matrix_UB_22 0.0098976000 _diffrn_orient_matrix_UB_23 0.0080405000 _diffrn_orient_matrix_UB_31 0.0029420000 _diffrn_orient_matrix_UB_32 -0.0586289000 _diffrn_orient_matrix_UB_33 0.0056729000 _diffrn_radiation_monochromator mirror _diffrn_radiation_probe x-ray _diffrn_radiation_type MoK\a _diffrn_radiation_wavelength 0.71073 _diffrn_reflns_av_R_equivalents 0.0720 _diffrn_reflns_av_unetI/netI 0.0388 _diffrn_reflns_Laue_measured_fraction_full 0.999 _diffrn_reflns_Laue_measured_fraction_max 0.999 _diffrn_reflns_limit_h_max 23 _diffrn_reflns_limit_h_min -24 _diffrn_reflns_limit_k_max 13 _diffrn_reflns_limit_k_min -12 _diffrn_reflns_limit_l_max 43 _diffrn_reflns_limit_l_min -43 _diffrn_reflns_number 53737 _diffrn_reflns_point_group_measured_fraction_full 0.999 _diffrn_reflns_point_group_measured_fraction_max 0.999 _diffrn_reflns_theta_full 25.242 _diffrn_reflns_theta_max 25.350 _diffrn_reflns_theta_min 2.138 _diffrn_source 'Rotating-anode X-ray tube (dual wavelength)' _diffrn_source_type 'Rigaku (Mo) X-ray DW Source' _exptl_absorpt_coefficient_mu 0.607 _exptl_absorpt_correction_T_max 1.00000 _exptl_absorpt_correction_T_min 0.46150 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_process_details ; CrysAlisPro 1.171.40.45a (Rigaku Oxford Diffraction, 2019) Empirical absorption correction using spherical harmonics, implemented in SCALE3 ABSPACK scaling algorithm. ; _exptl_crystal_colour yellow _exptl_crystal_colour_primary yellow _exptl_crystal_density_diffrn 1.352 _exptl_crystal_description plate _exptl_crystal_F_000 3584 _exptl_crystal_size_max 0.55 _exptl_crystal_size_mid 0.09 _exptl_crystal_size_min 0.08 _refine_diff_density_max 0.757 _refine_diff_density_min -0.599 _refine_diff_density_rms 0.073 _refine_ls_extinction_method none _refine_ls_goodness_of_fit_ref 1.075 _refine_ls_hydrogen_treatment constr _refine_ls_matrix_type full _refine_ls_number_parameters 486 _refine_ls_number_reflns 7717 _refine_ls_number_restraints 0 _refine_ls_restrained_S_all 1.075 _refine_ls_R_factor_all 0.0381 _refine_ls_R_factor_gt 0.0337 _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^)+(0.0354P)^2^+19.6876P] where P=(Fo^2^+2Fc^2^)/3' _refine_ls_weighting_scheme calc _refine_ls_wR_factor_gt 0.0821 _refine_ls_wR_factor_ref 0.0840 _reflns_Friedel_coverage 0.000 _reflns_number_gt 7014 _reflns_number_total 7717 _reflns_threshold_expression 'I > 2\s(I)' _cod_data_source_file c9cc06946a2.cif _cod_data_source_block tkh-1 _cod_database_code 7125642 _shelx_shelxl_version_number 2018/1 _chemical_oxdiff_formula 'C H O P Pd' _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 99.93 _reflns_odcompleteness_iscentric 1 _reflns_odcompleteness_theta 25.30 _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.a Secondary CH2 refined with riding coordinates: C46(H46A,H46B), C42(H42A,H42B) 2.b Aromatic/amide H refined with riding coordinates: C35(H35), C37(H37), C4(H4), C22(H22), C5(H5), C25(H25), C31(H31), C3(H3), C21(H21), C39(H39), C26(H26), C16(H16), C19(H19), C15(H15), C38(H38), C20(H20), C34(H34), C32(H32), C17(H17), C33(H33), C41(H41), C23(H23), C29(H29), C40(H40), C28(H28), C50(H50) 2.c Idealised Me refined as rotating group: C44(H44A,H44B,H44C), C48(H48A,H48B,H48C), C47(H47A,H47B,H47C), C45(H45A,H45B, H45C), C9(H9A,H9B,H9C), C43(H43A,H43B,H43C), C49(H49A,H49B,H49C), C10(H10A, H10B,H10C) ; _shelx_res_file ; TITL TKH-1 in C2/c #15 tkh-1.res created by SHELXL-2018/1 at 16:38:41 on 18-Jul-2019 REM reset to C2/c #15 CELL 0.71073 20.6034 11.5855 35.7054 90 97.72 90 ZERR 8 0.0004 0.0002 0.0008 0 0.002 0 LATT 7 SYMM -X,+Y,0.5-Z SFAC C H O P Pd Si UNIT 376 432 8 16 8 16 L.S. 20 PLAN 20 BOND fmap 2 acta OMIT 1 1 0 OMIT -1 1 2 OMIT 2 0 0 OMIT 0 0 4 OMIT 1 1 2 OMIT -1 1 1 REM REM REM WGHT 0.035400 19.687601 FVAR 0.16603 PD1 5 0.083088 0.016258 0.124795 11.00000 0.01001 0.01363 = 0.01385 -0.00078 0.00164 -0.00045 P2 4 0.160497 0.146192 0.102333 11.00000 0.01092 0.01400 = 0.01473 0.00001 0.00113 -0.00021 P3 4 0.154488 -0.139566 0.152289 11.00000 0.01234 0.01535 = 0.01379 0.00017 0.00217 -0.00018 SI1 6 -0.009248 0.172794 0.175046 11.00000 0.01404 0.02004 = 0.01728 -0.00241 0.00312 0.00092 SI2 6 -0.010046 -0.138123 0.070612 11.00000 0.01502 0.01934 = 0.01745 -0.00366 0.00340 -0.00207 O1 3 0.241999 -0.049786 0.104011 11.00000 0.01667 0.01336 = 0.01567 0.00007 0.00401 0.00132 C11 1 0.250596 -0.167870 0.105717 11.00000 0.01293 0.01354 = 0.01571 -0.00003 -0.00105 0.00022 C35 1 0.077895 -0.338754 0.147782 11.00000 0.02586 0.02174 = 0.02447 -0.00162 0.00680 -0.00271 AFIX 43 H35 2 0.081003 -0.334132 0.122080 11.00000 -1.20000 AFIX 0 C46 1 0.001287 -0.090911 0.121075 11.00000 0.01324 0.01965 = 0.01619 -0.00168 0.00382 -0.00426 AFIX 23 H46A 2 0.009210 -0.156449 0.137976 11.00000 -1.20000 H46B 2 -0.036782 -0.049128 0.127089 11.00000 -1.20000 AFIX 0 C1 1 0.198568 0.092867 0.061704 11.00000 0.01253 0.01771 = 0.01543 -0.00324 0.00141 -0.00403 C44 1 -0.078980 0.278896 0.173185 11.00000 0.01882 0.03809 = 0.02202 -0.00742 -0.00093 0.00927 AFIX 137 H44A 2 -0.066361 0.350618 0.162794 11.00000 -1.50000 H44B 2 -0.089450 0.291674 0.198255 11.00000 -1.50000 H44C 2 -0.116638 0.248428 0.157559 11.00000 -1.50000 AFIX 0 C2 1 0.238236 -0.003000 0.067954 11.00000 0.01301 0.01656 = 0.01535 -0.00035 0.00067 -0.00433 C30 1 0.110001 -0.257208 0.172400 11.00000 0.01212 0.01808 = 0.02131 0.00380 0.00406 0.00346 C37 1 0.170798 -0.009988 0.218460 11.00000 0.01783 0.02059 = 0.02294 0.00144 0.00267 0.00225 AFIX 43 H37 2 0.125867 0.001831 0.213073 11.00000 -1.20000 AFIX 0 C4 1 0.227386 0.095079 -0.001556 11.00000 0.02462 0.02640 = 0.01508 0.00346 0.00226 -0.00336 AFIX 43 H4 2 0.222819 0.127604 -0.025579 11.00000 -1.20000 AFIX 0 C22 1 0.121768 0.485361 0.071341 11.00000 0.03390 0.01632 = 0.02719 0.00011 0.00397 0.00195 AFIX 43 H22 2 0.140488 0.557649 0.076490 11.00000 -1.20000 AFIX 0 C18 1 0.124179 0.279770 0.081155 11.00000 0.01404 0.01787 = 0.01617 0.00087 0.00552 0.00488 C42 1 0.013267 0.147192 0.126919 11.00000 0.01461 0.01739 = 0.01696 0.00111 0.00314 0.00441 AFIX 23 H42A 2 0.030276 0.218378 0.117754 11.00000 -1.20000 H42B 2 -0.025976 0.127063 0.110026 11.00000 -1.20000 AFIX 0 C7 1 0.323487 -0.146193 0.055866 11.00000 0.01538 0.02045 = 0.02283 -0.00178 0.00687 0.00124 C5 1 0.267497 0.000099 0.006226 11.00000 0.02091 0.02644 = 0.01805 -0.00332 0.00704 -0.00243 AFIX 43 H5 2 0.289852 -0.030073 -0.012515 11.00000 -1.20000 AFIX 0 C12 1 0.291638 -0.221525 0.083289 11.00000 0.01268 0.02112 = 0.01770 -0.00410 0.00054 -0.00204 C25 1 0.224069 0.223834 0.170605 11.00000 0.01830 0.02325 = 0.02259 -0.00116 0.00418 -0.00299 AFIX 43 H25 2 0.183771 0.210391 0.178813 11.00000 -1.20000 AFIX 0 C24 1 0.232017 0.199722 0.133541 11.00000 0.01367 0.01402 = 0.01789 0.00060 -0.00044 -0.00153 C14 1 0.216050 -0.224395 0.131226 11.00000 0.01211 0.01723 = 0.01618 -0.00259 -0.00003 0.00135 C31 1 0.103816 -0.265356 0.210478 11.00000 0.02120 0.02393 = 0.02094 0.00231 0.00301 -0.00139 AFIX 43 H31 2 0.125023 -0.212179 0.227407 11.00000 -1.20000 AFIX 0 C3 1 0.193750 0.142805 0.025932 11.00000 0.01755 0.01865 = 0.01885 0.00210 0.00058 -0.00213 AFIX 43 H3 2 0.168000 0.208139 0.020443 11.00000 -1.20000 AFIX 0 C21 1 0.064754 0.475327 0.046477 11.00000 0.03116 0.02520 = 0.02020 0.00671 0.00570 0.01281 AFIX 43 H21 2 0.044856 0.540810 0.035060 11.00000 -1.20000 AFIX 0 C39 1 0.272194 0.023954 0.258261 11.00000 0.03089 0.03681 = 0.02094 -0.00832 -0.00127 -0.00681 AFIX 43 H39 2 0.295541 0.057463 0.279615 11.00000 -1.20000 AFIX 0 C26 1 0.275344 0.267758 0.195682 11.00000 0.03171 0.03116 = 0.01780 -0.00431 0.00183 -0.00761 AFIX 43 H26 2 0.269140 0.284593 0.220420 11.00000 -1.20000 AFIX 0 C6 1 0.274770 -0.050928 0.041909 11.00000 0.01361 0.01774 = 0.01977 -0.00201 0.00306 -0.00270 C48 1 -0.054032 -0.023834 0.039922 11.00000 0.02291 0.02879 = 0.02320 -0.00332 -0.00235 -0.00034 AFIX 137 H48A 2 -0.095734 -0.008729 0.048102 11.00000 -1.50000 H48B 2 -0.060532 -0.049800 0.014157 11.00000 -1.50000 H48C 2 -0.028374 0.045602 0.041776 11.00000 -1.50000 AFIX 0 C47 1 0.067521 -0.170830 0.050501 11.00000 0.02070 0.02225 = 0.02221 -0.00103 0.00889 0.00005 AFIX 137 H47A 2 0.093494 -0.102001 0.050626 11.00000 -1.50000 H47B 2 0.056985 -0.198160 0.025027 11.00000 -1.50000 H47C 2 0.091765 -0.229059 0.065561 11.00000 -1.50000 AFIX 0 C16 1 0.302522 -0.338829 0.089276 11.00000 0.01578 0.01974 = 0.02512 -0.00537 0.00466 0.00173 AFIX 43 H16 2 0.329230 -0.378759 0.074693 11.00000 -1.20000 AFIX 0 C45 1 0.059278 0.242935 0.206671 11.00000 0.01726 0.02186 = 0.02060 -0.00252 0.00241 0.00155 AFIX 137 H45A 2 0.076763 0.305391 0.193458 11.00000 -1.50000 H45B 2 0.093113 0.187225 0.213966 11.00000 -1.50000 H45C 2 0.043121 0.272178 0.228818 11.00000 -1.50000 AFIX 0 C19 1 0.066822 0.270460 0.055674 11.00000 0.01712 0.02347 = 0.01807 0.00183 0.00409 -0.00110 AFIX 43 H19 2 0.048290 0.198228 0.050136 11.00000 -1.20000 AFIX 0 C36 1 0.202877 -0.076912 0.194163 11.00000 0.01958 0.01534 = 0.01434 0.00113 0.00316 -0.00016 C9 1 0.384632 -0.087666 0.077598 11.00000 0.01619 0.02716 = 0.02868 0.00095 0.00642 -0.00076 AFIX 137 H9A 2 0.372261 -0.045213 0.098619 11.00000 -1.50000 H9B 2 0.403399 -0.035882 0.061013 11.00000 -1.50000 H9C 2 0.416235 -0.145530 0.086667 11.00000 -1.50000 AFIX 0 C15 1 0.230125 -0.341709 0.137274 11.00000 0.01810 0.02030 = 0.01959 0.00180 0.00265 -0.00141 AFIX 43 H15 2 0.210130 -0.382624 0.154998 11.00000 -1.20000 AFIX 0 C43 1 -0.038097 0.041930 0.198868 11.00000 0.03012 0.03123 = 0.02311 -0.00309 0.01147 -0.00762 AFIX 137 H43A 2 -0.048344 0.062762 0.223428 11.00000 -1.50000 H43B 2 -0.004209 -0.015513 0.201438 11.00000 -1.50000 H43C 2 -0.076516 0.011498 0.183941 11.00000 -1.50000 AFIX 0 C38 1 0.205309 0.039237 0.250652 11.00000 0.03158 0.02323 = 0.02053 -0.00386 0.00587 -0.00067 AFIX 43 H38 2 0.183388 0.082323 0.267004 11.00000 -1.20000 AFIX 0 C20 1 0.037242 0.367915 0.038553 11.00000 0.01859 0.03287 = 0.01862 0.00461 0.00219 0.00561 AFIX 43 H20 2 -0.001134 0.360989 0.021727 11.00000 -1.20000 AFIX 0 C34 1 0.041351 -0.426748 0.161125 11.00000 0.03030 0.02221 = 0.03537 -0.00329 0.00727 -0.00606 AFIX 43 H34 2 0.021123 -0.481641 0.144478 11.00000 -1.20000 AFIX 0 C32 1 0.066222 -0.352241 0.223591 11.00000 0.02785 0.03289 = 0.02414 0.00706 0.00898 -0.00191 AFIX 43 H32 2 0.062020 -0.356184 0.249170 11.00000 -1.20000 AFIX 0 C17 1 0.273772 -0.397108 0.116930 11.00000 0.02096 0.01259 = 0.03130 -0.00095 0.00321 0.00170 AFIX 43 H17 2 0.283986 -0.474305 0.121831 11.00000 -1.20000 AFIX 0 C33 1 0.035063 -0.432746 0.198946 11.00000 0.02575 0.02237 = 0.03977 0.00698 0.01264 -0.00423 AFIX 43 H33 2 0.009947 -0.490747 0.207861 11.00000 -1.20000 AFIX 0 C49 1 -0.062546 -0.271526 0.063130 11.00000 0.02814 0.02521 = 0.02401 -0.00792 0.00847 -0.01083 AFIX 137 H49A 2 -0.043956 -0.331614 0.079729 11.00000 -1.50000 H49B 2 -0.064477 -0.296629 0.037380 11.00000 -1.50000 H49C 2 -0.105945 -0.254282 0.068469 11.00000 -1.50000 AFIX 0 C10 1 0.344661 -0.216943 0.023142 11.00000 0.02661 0.02524 = 0.02594 -0.00243 0.01142 0.00550 AFIX 137 H10A 2 0.377105 -0.272486 0.033001 11.00000 -1.50000 H10B 2 0.362760 -0.166235 0.005969 11.00000 -1.50000 H10C 2 0.307339 -0.256281 0.010026 11.00000 -1.50000 AFIX 0 C41 1 0.270218 -0.091437 0.202292 11.00000 0.01851 0.03359 = 0.02208 -0.00779 0.00428 0.00069 AFIX 43 H41 2 0.292455 -0.135179 0.186259 11.00000 -1.20000 AFIX 0 C23 1 0.151315 0.388055 0.088705 11.00000 0.02089 0.01783 = 0.02141 -0.00069 0.00076 0.00105 AFIX 43 H23 2 0.189635 0.395584 0.105544 11.00000 -1.20000 AFIX 0 C29 1 0.292932 0.218460 0.121960 11.00000 0.01929 0.03218 = 0.01972 -0.00502 0.00436 -0.00665 AFIX 43 H29 2 0.299191 0.202195 0.097192 11.00000 -1.20000 AFIX 0 C40 1 0.304343 -0.041036 0.234171 11.00000 0.01653 0.04606 = 0.02991 -0.00888 -0.00164 -0.00004 AFIX 43 H40 2 0.349432 -0.051141 0.239384 11.00000 -1.20000 AFIX 0 C28 1 0.344347 0.261211 0.147104 11.00000 0.01828 0.04365 = 0.02905 -0.00409 0.00464 -0.01240 AFIX 43 H28 2 0.385020 0.272988 0.139169 11.00000 -1.20000 AFIX 0 C50 1 0.335568 0.286472 0.183914 11.00000 0.02487 0.03092 = 0.02548 -0.00143 -0.00586 -0.01272 AFIX 43 H50 2 0.370064 0.315924 0.200659 11.00000 -1.20000 AFIX 0 HKLF 4 REM TKH-1 in C2/c #15 REM R1 = 0.0337 for 7014 Fo > 4sig(Fo) and 0.0381 for all 7717 data REM 486 parameters refined using 0 restraints END WGHT 0.0328 20.5355 REM Highest difference peak 0.757, deepest hole -0.599, 1-sigma level 0.073 Q1 1 0.0881 0.0186 0.1009 11.00000 0.05 0.76 Q2 1 0.0876 0.0991 0.1242 11.00000 0.05 0.70 Q3 1 0.0398 0.0591 0.1184 11.00000 0.05 0.68 Q4 1 0.0384 -0.0289 0.1205 11.00000 0.05 0.63 Q5 1 0.1281 0.0579 0.1316 11.00000 0.05 0.61 Q6 1 0.0796 0.0181 0.1499 11.00000 0.05 0.61 Q7 1 0.1263 -0.0173 0.1307 11.00000 0.05 0.49 Q8 1 -0.0415 -0.2031 0.0668 11.00000 0.05 0.47 Q9 1 0.0783 -0.0742 0.1300 11.00000 0.05 0.46 Q10 1 0.0344 0.2250 0.1858 11.00000 0.05 0.45 Q11 1 0.1191 0.0973 0.1015 11.00000 0.05 0.43 Q12 1 0.1510 0.1367 0.1287 11.00000 0.05 0.42 Q13 1 -0.0474 0.2241 0.1739 11.00000 0.05 0.42 Q14 1 0.0018 0.1677 0.1497 11.00000 0.05 0.41 Q15 1 0.1392 0.2273 0.0932 11.00000 0.05 0.41 Q16 1 0.2023 0.1902 0.1128 11.00000 0.05 0.40 Q17 1 0.1873 -0.1928 0.1402 11.00000 0.05 0.39 Q18 1 0.1174 -0.0859 0.1444 11.00000 0.05 0.39 Q19 1 0.1274 -0.2019 0.1640 11.00000 0.05 0.38 Q20 1 0.2460 -0.1854 0.1255 11.00000 0.05 0.38 ; _shelx_res_checksum 2177 _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 3.693 _oxdiff_exptl_absorpt_empirical_full_min 0.323 loop_ _space_group_symop_operation_xyz 'x, y, z' '-x, y, -z+1/2' 'x+1/2, y+1/2, z' '-x+1/2, y+1/2, -z+1/2' '-x, -y, -z' 'x, -y, z-1/2' '-x+1/2, -y+1/2, -z' 'x+1/2, -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 Pd1 Pd 0.08309(2) 0.01626(2) 0.12479(2) 0.01249(7) Uani 1 1 d . P2 P 0.16050(3) 0.14619(5) 0.10233(2) 0.01327(14) Uani 1 1 d . P3 P 0.15449(3) -0.13957(5) 0.15229(2) 0.01379(14) Uani 1 1 d . Si1 Si -0.00925(3) 0.17279(6) 0.17505(2) 0.01703(15) Uani 1 1 d . Si2 Si -0.01005(3) -0.13812(6) 0.07061(2) 0.01716(15) Uani 1 1 d . O1 O 0.24200(8) -0.04979(14) 0.10401(4) 0.0151(3) Uani 1 1 d . C11 C 0.25060(11) -0.1679(2) 0.10572(7) 0.0143(5) Uani 1 1 d . C35 C 0.07789(13) -0.3388(2) 0.14778(8) 0.0237(6) Uani 1 1 d . H35 H 0.081003 -0.334132 0.122080 0.028 Uiso 1 1 calc R C46 C 0.00129(11) -0.0909(2) 0.12107(7) 0.0162(5) Uani 1 1 d . H46A H 0.009210 -0.156449 0.137976 0.019 Uiso 1 1 calc R H46B H -0.036782 -0.049128 0.127089 0.019 Uiso 1 1 calc R C1 C 0.19857(11) 0.0929(2) 0.06170(7) 0.0153(5) Uani 1 1 d . C44 C -0.07898(13) 0.2789(3) 0.17319(8) 0.0266(6) Uani 1 1 d . H44A H -0.066361 0.350618 0.162794 0.040 Uiso 1 1 calc GR H44B H -0.089450 0.291674 0.198255 0.040 Uiso 1 1 calc GR H44C H -0.116638 0.248428 0.157559 0.040 Uiso 1 1 calc GR C2 C 0.23824(12) -0.0030(2) 0.06795(7) 0.0151(5) Uani 1 1 d . C30 C 0.11000(11) -0.2572(2) 0.17240(7) 0.0170(5) Uani 1 1 d . C37 C 0.17080(13) -0.0100(2) 0.21846(7) 0.0205(5) Uani 1 1 d . H37 H 0.125867 0.001831 0.213073 0.025 Uiso 1 1 calc R C4 C 0.22739(13) 0.0951(2) -0.00156(7) 0.0221(6) Uani 1 1 d . H4 H 0.222819 0.127604 -0.025579 0.026 Uiso 1 1 calc R C22 C 0.12177(14) 0.4854(2) 0.07134(8) 0.0258(6) Uani 1 1 d . H22 H 0.140488 0.557649 0.076490 0.031 Uiso 1 1 calc R C18 C 0.12418(11) 0.2798(2) 0.08115(7) 0.0157(5) Uani 1 1 d . C42 C 0.01327(12) 0.1472(2) 0.12692(7) 0.0162(5) Uani 1 1 d . H42A H 0.030276 0.218378 0.117754 0.019 Uiso 1 1 calc R H42B H -0.025976 0.127063 0.110026 0.019 Uiso 1 1 calc R C7 C 0.32349(12) -0.1462(2) 0.05587(7) 0.0192(5) Uani 1 1 d . C5 C 0.26750(13) 0.0001(2) 0.00623(7) 0.0214(6) Uani 1 1 d . H5 H 0.289852 -0.030073 -0.012515 0.026 Uiso 1 1 calc R C12 C 0.29164(12) -0.2215(2) 0.08329(7) 0.0173(5) Uani 1 1 d . C25 C 0.22407(13) 0.2238(2) 0.17060(7) 0.0212(5) Uani 1 1 d . H25 H 0.183771 0.210391 0.178813 0.025 Uiso 1 1 calc R C24 C 0.23202(11) 0.1997(2) 0.13354(7) 0.0154(5) Uani 1 1 d . C14 C 0.21605(11) -0.2244(2) 0.13123(7) 0.0153(5) Uani 1 1 d . C31 C 0.10382(13) -0.2654(2) 0.21048(7) 0.0220(6) Uani 1 1 d . H31 H 0.125023 -0.212179 0.227407 0.026 Uiso 1 1 calc R C3 C 0.19375(12) 0.1428(2) 0.02593(7) 0.0185(5) Uani 1 1 d . H3 H 0.168000 0.208139 0.020443 0.022 Uiso 1 1 calc R C21 C 0.06475(14) 0.4753(2) 0.04648(7) 0.0253(6) Uani 1 1 d . H21 H 0.044856 0.540810 0.035060 0.030 Uiso 1 1 calc R C39 C 0.27219(15) 0.0240(3) 0.25826(8) 0.0300(7) Uani 1 1 d . H39 H 0.295541 0.057463 0.279615 0.036 Uiso 1 1 calc R C26 C 0.27534(14) 0.2678(2) 0.19568(8) 0.0270(6) Uani 1 1 d . H26 H 0.269140 0.284593 0.220420 0.032 Uiso 1 1 calc R C6 C 0.27477(12) -0.0509(2) 0.04191(7) 0.0170(5) Uani 1 1 d . C48 C -0.05403(14) -0.0238(2) 0.03992(8) 0.0255(6) Uani 1 1 d . H48A H -0.095734 -0.008729 0.048102 0.038 Uiso 1 1 calc GR H48B H -0.060532 -0.049800 0.014157 0.038 Uiso 1 1 calc GR H48C H -0.028374 0.045602 0.041776 0.038 Uiso 1 1 calc GR C47 C 0.06752(12) -0.1708(2) 0.05050(7) 0.0212(5) Uani 1 1 d . H47A H 0.093494 -0.102001 0.050626 0.032 Uiso 1 1 calc GR H47B H 0.056985 -0.198160 0.025027 0.032 Uiso 1 1 calc GR H47C H 0.091765 -0.229059 0.065561 0.032 Uiso 1 1 calc GR C16 C 0.30252(12) -0.3388(2) 0.08928(7) 0.0200(5) Uani 1 1 d . H16 H 0.329230 -0.378759 0.074693 0.024 Uiso 1 1 calc R C45 C 0.05928(12) 0.2429(2) 0.20667(7) 0.0199(5) Uani 1 1 d . H45A H 0.076763 0.305391 0.193458 0.030 Uiso 1 1 calc GR H45B H 0.093113 0.187225 0.213966 0.030 Uiso 1 1 calc GR H45C H 0.043121 0.272178 0.228818 0.030 Uiso 1 1 calc GR C19 C 0.06682(12) 0.2705(2) 0.05567(7) 0.0194(5) Uani 1 1 d . H19 H 0.048290 0.198228 0.050136 0.023 Uiso 1 1 calc R C36 C 0.20288(12) -0.0769(2) 0.19416(7) 0.0163(5) Uani 1 1 d . C9 C 0.38463(12) -0.0877(2) 0.07760(8) 0.0237(6) Uani 1 1 d . H9A H 0.372261 -0.045213 0.098619 0.036 Uiso 1 1 calc GR H9B H 0.403399 -0.035882 0.061013 0.036 Uiso 1 1 calc GR H9C H 0.416235 -0.145530 0.086667 0.036 Uiso 1 1 calc GR C15 C 0.23012(12) -0.3417(2) 0.13727(7) 0.0193(5) Uani 1 1 d . H15 H 0.210130 -0.382624 0.154998 0.023 Uiso 1 1 calc R C43 C -0.03810(14) 0.0419(2) 0.19887(8) 0.0274(6) Uani 1 1 d . H43A H -0.048344 0.062762 0.223428 0.041 Uiso 1 1 calc GR H43B H -0.004209 -0.015513 0.201438 0.041 Uiso 1 1 calc GR H43C H -0.076516 0.011498 0.183941 0.041 Uiso 1 1 calc GR C38 C 0.20531(14) 0.0392(2) 0.25065(7) 0.0249(6) Uani 1 1 d . H38 H 0.183388 0.082323 0.267004 0.030 Uiso 1 1 calc R C20 C 0.03724(13) 0.3679(2) 0.03855(7) 0.0234(6) Uani 1 1 d . H20 H -0.001134 0.360989 0.021727 0.028 Uiso 1 1 calc R C34 C 0.04135(14) -0.4267(2) 0.16112(8) 0.0290(6) Uani 1 1 d . H34 H 0.021123 -0.481641 0.144478 0.035 Uiso 1 1 calc R C32 C 0.06622(14) -0.3522(2) 0.22359(8) 0.0278(6) Uani 1 1 d . H32 H 0.062020 -0.356184 0.249170 0.033 Uiso 1 1 calc R C17 C 0.27377(12) -0.3971(2) 0.11693(8) 0.0216(6) Uani 1 1 d . H17 H 0.283986 -0.474305 0.121831 0.026 Uiso 1 1 calc R C33 C 0.03506(14) -0.4327(2) 0.19895(8) 0.0285(6) Uani 1 1 d . H33 H 0.009947 -0.490747 0.207861 0.034 Uiso 1 1 calc R C49 C -0.06255(14) -0.2715(2) 0.06313(8) 0.0253(6) Uani 1 1 d . H49A H -0.043956 -0.331614 0.079729 0.038 Uiso 1 1 calc GR H49B H -0.064477 -0.296629 0.037380 0.038 Uiso 1 1 calc GR H49C H -0.105945 -0.254282 0.068469 0.038 Uiso 1 1 calc GR C10 C 0.34466(14) -0.2169(2) 0.02314(8) 0.0252(6) Uani 1 1 d . H10A H 0.377105 -0.272486 0.033001 0.038 Uiso 1 1 calc GR H10B H 0.362760 -0.166235 0.005969 0.038 Uiso 1 1 calc GR H10C H 0.307339 -0.256281 0.010026 0.038 Uiso 1 1 calc GR C41 C 0.27022(13) -0.0914(2) 0.20229(7) 0.0246(6) Uani 1 1 d . H41 H 0.292455 -0.135179 0.186259 0.030 Uiso 1 1 calc R C23 C 0.15132(13) 0.3881(2) 0.08871(7) 0.0202(5) Uani 1 1 d . H23 H 0.189635 0.395584 0.105544 0.024 Uiso 1 1 calc R C29 C 0.29293(13) 0.2185(2) 0.12196(7) 0.0236(6) Uani 1 1 d . H29 H 0.299191 0.202195 0.097192 0.028 Uiso 1 1 calc R C40 C 0.30434(14) -0.0410(3) 0.23417(8) 0.0313(7) Uani 1 1 d . H40 H 0.349432 -0.051141 0.239384 0.038 Uiso 1 1 calc R C28 C 0.34435(13) 0.2612(3) 0.14710(8) 0.0302(7) Uani 1 1 d . H28 H 0.385020 0.272988 0.139169 0.036 Uiso 1 1 calc R C50 C 0.33557(13) 0.2865(2) 0.18391(8) 0.0279(6) Uani 1 1 d . H50 H 0.370064 0.315924 0.200659 0.034 Uiso 1 1 calc R 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 Pd1 0.01001(11) 0.01363(11) 0.01385(11) -0.00078(7) 0.00164(7) -0.00045(7) P2 0.0109(3) 0.0140(3) 0.0147(3) 0.0000(2) 0.0011(2) -0.0002(2) P3 0.0123(3) 0.0153(3) 0.0138(3) 0.0002(2) 0.0022(2) -0.0002(2) Si1 0.0140(3) 0.0200(4) 0.0173(3) -0.0024(3) 0.0031(3) 0.0009(3) Si2 0.0150(3) 0.0193(4) 0.0174(3) -0.0037(3) 0.0034(3) -0.0021(3) O1 0.0167(9) 0.0134(8) 0.0157(8) 0.0001(7) 0.0040(7) 0.0013(7) C11 0.0129(12) 0.0135(12) 0.0157(12) 0.0000(9) -0.0011(9) 0.0002(9) C35 0.0259(14) 0.0217(14) 0.0245(14) -0.0016(11) 0.0068(11) -0.0027(11) C46 0.0132(12) 0.0196(13) 0.0162(12) -0.0017(10) 0.0038(9) -0.0043(10) C1 0.0125(12) 0.0177(12) 0.0154(12) -0.0032(10) 0.0014(9) -0.0040(10) C44 0.0188(14) 0.0381(17) 0.0220(14) -0.0074(12) -0.0009(10) 0.0093(12) C2 0.0130(12) 0.0166(12) 0.0154(12) -0.0003(9) 0.0007(9) -0.0043(9) C30 0.0121(12) 0.0181(13) 0.0213(13) 0.0038(10) 0.0041(9) 0.0035(10) C37 0.0178(13) 0.0206(13) 0.0229(14) 0.0014(10) 0.0027(10) 0.0022(10) C4 0.0246(14) 0.0264(14) 0.0151(12) 0.0035(10) 0.0023(10) -0.0034(11) C22 0.0339(16) 0.0163(13) 0.0272(15) 0.0001(11) 0.0040(12) 0.0020(11) C18 0.0140(12) 0.0179(13) 0.0162(12) 0.0009(10) 0.0055(9) 0.0049(10) C42 0.0146(12) 0.0174(13) 0.0170(12) 0.0011(10) 0.0031(9) 0.0044(10) C7 0.0154(12) 0.0204(13) 0.0228(13) -0.0018(10) 0.0069(10) 0.0012(10) C5 0.0209(14) 0.0264(14) 0.0180(13) -0.0033(11) 0.0070(10) -0.0024(11) C12 0.0127(12) 0.0211(13) 0.0177(12) -0.0041(10) 0.0005(9) -0.0020(10) C25 0.0183(13) 0.0233(14) 0.0226(14) -0.0012(11) 0.0042(10) -0.0030(11) C24 0.0137(12) 0.0140(12) 0.0179(12) 0.0006(10) -0.0004(9) -0.0015(9) C14 0.0121(12) 0.0172(12) 0.0162(12) -0.0026(10) 0.0000(9) 0.0013(9) C31 0.0212(13) 0.0239(14) 0.0209(13) 0.0023(11) 0.0030(10) -0.0014(11) C3 0.0176(13) 0.0186(13) 0.0188(13) 0.0021(10) 0.0006(10) -0.0021(10) C21 0.0312(15) 0.0252(15) 0.0202(13) 0.0067(11) 0.0057(11) 0.0128(12) C39 0.0309(16) 0.0368(17) 0.0209(14) -0.0083(12) -0.0013(12) -0.0068(13) C26 0.0317(16) 0.0312(15) 0.0178(13) -0.0043(11) 0.0018(11) -0.0076(12) C6 0.0136(12) 0.0177(12) 0.0198(13) -0.0020(10) 0.0031(10) -0.0027(10) C48 0.0229(14) 0.0288(15) 0.0232(14) -0.0033(11) -0.0023(11) -0.0003(11) C47 0.0207(13) 0.0223(14) 0.0222(13) -0.0010(11) 0.0089(10) 0.0000(11) C16 0.0158(13) 0.0197(13) 0.0251(14) -0.0054(11) 0.0047(10) 0.0017(10) C45 0.0173(13) 0.0219(14) 0.0206(13) -0.0025(10) 0.0024(10) 0.0016(10) C19 0.0171(13) 0.0235(14) 0.0181(13) 0.0018(10) 0.0041(10) -0.0011(10) C36 0.0196(13) 0.0153(12) 0.0143(12) 0.0011(9) 0.0032(9) -0.0002(10) C9 0.0162(13) 0.0272(15) 0.0287(15) 0.0010(11) 0.0064(11) -0.0008(11) C15 0.0181(13) 0.0203(13) 0.0196(13) 0.0018(10) 0.0027(10) -0.0014(10) C43 0.0301(16) 0.0312(16) 0.0231(14) -0.0031(12) 0.0115(12) -0.0076(12) C38 0.0316(16) 0.0232(14) 0.0205(13) -0.0039(11) 0.0059(11) -0.0007(12) C20 0.0186(13) 0.0329(16) 0.0186(13) 0.0046(11) 0.0022(10) 0.0056(11) C34 0.0303(16) 0.0222(15) 0.0354(16) -0.0033(12) 0.0073(12) -0.0061(12) C32 0.0278(15) 0.0329(16) 0.0241(14) 0.0071(12) 0.0090(11) -0.0019(12) C17 0.0210(13) 0.0126(12) 0.0313(15) -0.0009(11) 0.0032(11) 0.0017(10) C33 0.0257(15) 0.0224(15) 0.0398(17) 0.0070(12) 0.0126(12) -0.0042(12) C49 0.0281(15) 0.0252(14) 0.0240(14) -0.0079(11) 0.0085(11) -0.0108(12) C10 0.0266(15) 0.0252(14) 0.0259(14) -0.0024(11) 0.0114(11) 0.0055(11) C41 0.0185(13) 0.0336(16) 0.0221(14) -0.0078(11) 0.0043(10) 0.0007(11) C23 0.0209(13) 0.0178(13) 0.0214(13) -0.0007(10) 0.0008(10) 0.0010(10) C29 0.0193(13) 0.0322(15) 0.0197(13) -0.0050(11) 0.0044(10) -0.0066(11) C40 0.0165(14) 0.0461(18) 0.0299(15) -0.0089(13) -0.0016(11) 0.0000(13) C28 0.0183(14) 0.0437(18) 0.0290(15) -0.0041(13) 0.0046(11) -0.0124(12) C50 0.0249(15) 0.0309(16) 0.0255(15) -0.0014(12) -0.0059(11) -0.0127(12) loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 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' Pd Pd -0.9988 1.0072 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Si Si 0.0817 0.0704 '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 P2 Pd1 P3 101.85(2) C46 Pd1 P2 156.62(7) C46 Pd1 P3 91.35(7) C46 Pd1 C42 83.14(10) C42 Pd1 P2 92.75(7) C42 Pd1 P3 153.62(7) C1 P2 Pd1 115.02(8) C18 P2 Pd1 114.36(8) C18 P2 C1 98.69(11) C24 P2 Pd1 121.58(8) C24 P2 C1 101.50(11) C24 P2 C18 102.42(11) C30 P3 Pd1 113.47(8) C30 P3 C14 99.81(11) C14 P3 Pd1 129.70(8) C36 P3 Pd1 105.47(8) C36 P3 C30 102.70(11) C36 P3 C14 102.44(11) C42 Si1 C44 110.75(12) C42 Si1 C45 111.39(11) C42 Si1 C43 115.05(12) C45 Si1 C44 104.35(12) C45 Si1 C43 109.70(12) C43 Si1 C44 104.88(13) C46 Si2 C48 110.20(12) C46 Si2 C47 115.20(11) C46 Si2 C49 111.84(11) C48 Si2 C47 106.79(12) C48 Si2 C49 105.87(13) C47 Si2 C49 106.39(12) C11 O1 C2 114.74(18) O1 C11 C12 120.2(2) O1 C11 C14 114.9(2) C12 C11 C14 124.9(2) C34 C35 C30 120.9(2) Si2 C46 Pd1 103.38(11) C2 C1 P2 116.58(18) C2 C1 C3 116.8(2) C3 C1 P2 126.58(19) O1 C2 C6 119.8(2) C1 C2 O1 115.0(2) C1 C2 C6 125.2(2) C35 C30 P3 118.31(19) C31 C30 P3 123.3(2) C31 C30 C35 118.3(2) C38 C37 C36 120.7(2) C5 C4 C3 121.1(2) C21 C22 C23 120.3(3) C19 C18 P2 117.76(19) C23 C18 P2 123.47(19) C23 C18 C19 118.8(2) Si1 C42 Pd1 113.90(12) C12 C7 C6 107.59(19) C12 C7 C9 108.7(2) C12 C7 C10 111.9(2) C6 C7 C9 107.6(2) C6 C7 C10 112.2(2) C10 C7 C9 108.7(2) C4 C5 C6 120.6(2) C11 C12 C7 117.6(2) C11 C12 C16 116.6(2) C16 C12 C7 125.8(2) C24 C25 C26 120.9(2) C25 C24 P2 117.46(18) C25 C24 C29 118.7(2) C29 C24 P2 123.81(19) C11 C14 P3 117.15(18) C11 C14 C15 116.3(2) C15 C14 P3 126.46(19) C30 C31 C32 120.6(3) C4 C3 C1 120.1(2) C22 C21 C20 119.9(2) C38 C39 C40 119.9(3) C50 C26 C25 120.0(3) C2 C6 C7 117.5(2) C2 C6 C5 116.2(2) C5 C6 C7 126.1(2) C12 C16 C17 120.5(2) C20 C19 C18 120.6(2) C37 C36 P3 118.46(19) C41 C36 P3 122.78(18) C41 C36 C37 118.7(2) C17 C15 C14 120.2(2) C39 C38 C37 119.8(2) C21 C20 C19 120.0(2) C33 C34 C35 120.0(3) C33 C32 C31 120.5(3) C15 C17 C16 121.0(2) C34 C33 C32 119.7(3) C40 C41 C36 120.2(2) C22 C23 C18 120.5(2) C28 C29 C24 120.4(2) C39 C40 C41 120.7(3) C50 C28 C29 120.4(2) C26 C50 C28 119.6(2) loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance Pd1 P2 2.4076(6) Pd1 P3 2.4493(6) Pd1 C46 2.083(2) Pd1 C42 2.099(2) P2 C1 1.846(2) P2 C18 1.837(2) P2 C24 1.832(2) P3 C30 1.841(2) P3 C14 1.843(2) P3 C36 1.832(2) Si1 C44 1.885(3) Si1 C42 1.863(2) Si1 C45 1.871(3) Si1 C43 1.874(3) Si2 C46 1.867(2) Si2 C48 1.873(3) Si2 C47 1.877(2) Si2 C49 1.885(3) O1 C11 1.380(3) O1 C2 1.389(3) C11 C12 1.387(3) C11 C14 1.393(3) C35 C30 1.395(4) C35 C34 1.389(4) C1 C2 1.379(4) C1 C3 1.394(3) C2 C6 1.388(3) C30 C31 1.386(4) C37 C36 1.395(3) C37 C38 1.390(4) C4 C5 1.382(4) C4 C3 1.390(4) C22 C21 1.379(4) C22 C23 1.387(4) C18 C19 1.395(4) C18 C23 1.385(4) C7 C12 1.524(3) C7 C6 1.530(4) C7 C9 1.545(4) C7 C10 1.538(3) C5 C6 1.394(4) C12 C16 1.389(4) C25 C24 1.384(3) C25 C26 1.387(4) C24 C29 1.390(3) C14 C15 1.400(4) C31 C32 1.389(4) C21 C20 1.381(4) C39 C38 1.380(4) C39 C40 1.378(4) C26 C50 1.380(4) C16 C17 1.392(4) C19 C20 1.386(4) C36 C41 1.389(4) C15 C17 1.387(4) C34 C33 1.376(4) C32 C33 1.380(4) C41 C40 1.384(4) C29 C28 1.385(4) C28 C50 1.382(4)