#------------------------------------------------------------------------------ #$Date: 2017-04-22 05:09:35 +0300 (Sat, 22 Apr 2017) $ #$Revision: 195681 $ #$URL: file:///home/coder/svn-repositories/cod/cif/7/04/27/7042748.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_7042748 loop_ _publ_author_name 'Kashid, Vitthal S.' 'Radhakrishna, Latchupatula' 'Balakrishna, Maravanji Shivaramaiah' _publ_section_title ; First examples of tri- and tetraphosphametacyclophanes: synthesis and isolation of an unusual hexapalladium complex containing pincer units with Pd---P covalent bonds ; _journal_name_full 'Dalton Trans.' _journal_paper_doi 10.1039/C7DT00737J _journal_year 2017 _chemical_formula_moiety 'C44 H36 Cl6 N2 O4 P4 Pd6' _chemical_formula_sum 'C44 H36 Cl6 N2 O4 P4 Pd6' _chemical_formula_weight 1631.73 _space_group_crystal_system triclinic _space_group_IT_number 2 _space_group_name_Hall '-P 1' _space_group_name_H-M_alt 'P -1' _symmetry_space_group_name_Hall '-P 1' _symmetry_space_group_name_H-M 'P -1' _atom_sites_solution_hydrogens geom _audit_creation_method SHELXL-2014/7 _audit_update_record ; 2017-02-11 deposited with the CCDC. 2017-04-20 downloaded from the CCDC. ; _cell_angle_alpha 102.789(2) _cell_angle_beta 95.8839(19) _cell_angle_gamma 113.851(2) _cell_formula_units_Z 1 _cell_length_a 10.0974(2) _cell_length_b 10.1677(3) _cell_length_c 13.9117(3) _cell_measurement_reflns_used 18735 _cell_measurement_temperature 150(2) _cell_measurement_theta_max 31.1890 _cell_measurement_theta_min 2.2500 _cell_volume 1244.02(6) _computing_structure_refinement 'SHELXL-2014/7 (Sheldrick, 2014)' _diffrn_ambient_temperature 150(2) _diffrn_detector_area_resol_mean 28.5714 _diffrn_measured_fraction_theta_full 0.999 _diffrn_measured_fraction_theta_max 0.999 _diffrn_measurement_device_type 'Rigaku saturn 724' _diffrn_measurement_method \w _diffrn_radiation_type MoK\a _diffrn_radiation_wavelength 0.71073 _diffrn_reflns_av_R_equivalents 0.0426 _diffrn_reflns_av_unetI/netI 0.0271 _diffrn_reflns_Laue_measured_fraction_full 0.999 _diffrn_reflns_Laue_measured_fraction_max 0.999 _diffrn_reflns_limit_h_max 12 _diffrn_reflns_limit_h_min -12 _diffrn_reflns_limit_k_max 12 _diffrn_reflns_limit_k_min -12 _diffrn_reflns_limit_l_max 16 _diffrn_reflns_limit_l_min -16 _diffrn_reflns_number 22657 _diffrn_reflns_point_group_measured_fraction_full 0.999 _diffrn_reflns_point_group_measured_fraction_max 0.999 _diffrn_reflns_theta_full 24.998 _diffrn_reflns_theta_max 24.998 _diffrn_reflns_theta_min 2.288 _exptl_absorpt_coefficient_mu 2.618 _exptl_absorpt_correction_T_max 1.00000 _exptl_absorpt_correction_T_min 0.48285 _exptl_absorpt_correction_type numerical _exptl_absorpt_process_details 'NUMABS RIGAKU 1999' _exptl_crystal_colour red _exptl_crystal_density_diffrn 2.178 _exptl_crystal_density_method 'not measured' _exptl_crystal_description prism _exptl_crystal_F_000 784 _exptl_crystal_size_max 0.160 _exptl_crystal_size_mid 0.064 _exptl_crystal_size_min 0.03 _refine_diff_density_max 0.839 _refine_diff_density_min -0.526 _refine_diff_density_rms 0.122 _refine_ls_extinction_method none _refine_ls_goodness_of_fit_ref 1.061 _refine_ls_hydrogen_treatment constr _refine_ls_matrix_type full _refine_ls_number_parameters 326 _refine_ls_number_reflns 4353 _refine_ls_number_restraints 36 _refine_ls_restrained_S_all 1.060 _refine_ls_R_factor_all 0.0284 _refine_ls_R_factor_gt 0.0252 _refine_ls_shift/su_max 0.001 _refine_ls_shift/su_mean 0.000 _refine_ls_structure_factor_coef Fsqd _refine_ls_weighting_details 'w=1/[\s^2^(Fo^2^)+(0.0318P)^2^+2.2641P] where P=(Fo^2^+2Fc^2^)/3' _refine_ls_weighting_scheme calc _refine_ls_wR_factor_gt 0.0626 _refine_ls_wR_factor_ref 0.0646 _reflns_Friedel_coverage 0.000 _reflns_number_gt 4043 _reflns_number_total 4353 _reflns_threshold_expression 'I > 2\s(I)' _cod_data_source_file c7dt00737j2.cif _cod_data_source_block MSB-VSK-294 _cod_original_cell_volume 1244.01(6) _cod_database_code 7042748 _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_res_file ; msb-vsk-294_mo.res created by SHELXL-2014/7 TITL msb-vsk-294_mo_a.res in P-1 REM Old TITL MSB-VSK-294_Mo in P-1 #2 REM SHELXT solution in P-1 REM R1 0.082, Rweak 0.005, Alpha 0.039, Orientation as input REM Formula found by SHELXT: C23 N O2 P2 Cl3 Pd3 CELL 0.71073 10.097373 10.167654 13.911733 102.7886 95.8839 113.8514 ZERR 1 0.000231 0.000252 0.000333 0.0021 0.0019 0.0023 LATT 1 SFAC C H Cl N O P Pd UNIT 44 36 6 2 4 4 6 ISOR 0.001 0.001 C20A C20 C21 C21A C22A C22 L.S. 10 PLAN 20 BOND $H LIST 6 MORE -1 CONF fmap 2 acta 52 OMIT -3 50 OMIT 0 0 1 OMIT 0 -1 1 OMIT 1 0 0 OMIT 1 -1 1 REM REM REM WGHT 0.031800 2.264100 FVAR 0.37090 0.50056 PD2 7 0.532000 0.263809 0.278051 11.00000 0.01891 0.01554 = 0.01547 0.00257 0.00398 0.00853 PD1 7 0.320930 0.432901 0.461028 11.00000 0.02003 0.01539 = 0.01542 0.00335 0.00320 0.00934 PD3 7 0.464943 -0.086131 0.112736 11.00000 0.03270 0.01882 = 0.02087 0.00403 0.00763 0.01199 CL1 3 0.282717 0.199931 0.474047 11.00000 0.03569 0.01838 = 0.02807 0.00717 0.00676 0.01472 CL3 3 0.663880 0.112534 0.243023 11.00000 0.02467 0.02158 = 0.03682 -0.00103 0.00399 0.01263 P2 6 0.268027 0.535157 0.612179 11.00000 0.01906 0.01663 = 0.01684 0.00370 0.00426 0.00820 P1 6 0.395847 0.389488 0.312660 11.00000 0.02063 0.01846 = 0.01652 0.00295 0.00360 0.01075 CL2 3 0.325000 0.048532 0.161932 11.00000 0.02545 0.02190 = 0.03746 -0.00496 -0.00232 0.01064 O1 5 0.566925 0.635748 0.256197 11.00000 0.03036 0.03237 = 0.02797 0.01344 0.01192 0.01582 O2 5 0.074565 0.655700 0.570565 11.00000 0.02579 0.03621 = 0.02753 0.00652 0.00567 0.02009 N1 4 0.335807 0.627201 0.431468 11.00000 0.01857 0.01817 = 0.01404 0.00162 -0.00055 0.00940 C5 1 0.266468 0.702835 0.478509 11.00000 0.01939 0.02237 = 0.01396 0.00018 -0.00140 0.00913 C4 1 0.273122 0.833115 0.460914 11.00000 0.03156 0.02343 = 0.02558 0.00387 0.00417 0.01830 AFIX 43 H4 2 0.221498 0.881088 0.492914 11.00000 -1.20000 AFIX 0 C7 1 0.136182 0.435721 0.680543 11.00000 0.01992 0.02428 = 0.02030 0.00718 0.00333 0.00791 C8 1 0.074968 0.510342 0.744679 11.00000 0.02571 0.02350 = 0.02955 0.00322 0.00780 0.00689 AFIX 43 H8 2 0.099229 0.610847 0.751103 11.00000 -1.20000 AFIX 0 C2 1 0.428395 0.813927 0.346287 11.00000 0.03021 0.02365 = 0.02102 0.00979 0.00376 0.00969 AFIX 43 H2 2 0.485392 0.850803 0.301385 11.00000 -1.20000 AFIX 0 C9 1 -0.021959 0.434423 0.798725 11.00000 0.02853 0.03272 = 0.02725 0.00039 0.00944 0.01187 AFIX 43 H9 2 -0.064582 0.483405 0.840318 11.00000 -1.20000 AFIX 0 C19 1 0.097566 0.222442 0.215377 11.00000 0.02867 0.03355 = 0.02956 -0.00117 0.00360 0.01505 AFIX 43 H19 2 0.081712 0.203156 0.276557 11.00000 -1.20000 AFIX 0 C10 1 -0.055136 0.287984 0.791157 11.00000 0.02867 0.04122 = 0.03126 0.01889 0.00831 0.00676 AFIX 43 H10 2 -0.118556 0.238565 0.828957 11.00000 -1.20000 AFIX 0 C3 1 0.357413 0.891737 0.395146 11.00000 0.04400 0.02030 = 0.02857 0.00847 0.00572 0.01913 AFIX 43 H3 2 0.366362 0.981480 0.383878 11.00000 -1.20000 AFIX 0 C16 1 0.140636 0.282177 0.032539 11.00000 0.04959 0.04601 = 0.02049 -0.00312 -0.00423 0.02863 AFIX 43 H16 2 0.153795 0.304582 -0.028105 11.00000 -1.20000 AFIX 0 C11 1 0.004314 0.212168 0.728028 11.00000 0.03709 0.02937 = 0.04430 0.01877 0.01219 0.01219 AFIX 43 H11 2 -0.019891 0.112002 0.722874 11.00000 -1.20000 AFIX 0 C12 1 0.100443 0.286115 0.672234 11.00000 0.02556 0.02374 = 0.03358 0.00748 0.00765 0.01050 AFIX 43 H12 2 0.140640 0.235571 0.629521 11.00000 -1.20000 AFIX 0 C1 1 0.413985 0.682009 0.364636 11.00000 0.01913 0.02095 = 0.01686 0.00367 0.00063 0.00894 C13 1 0.478635 0.588277 0.306879 11.00000 0.02016 0.02326 = 0.01769 0.00463 -0.00023 0.01018 C15 1 0.259589 0.346602 0.115161 11.00000 0.03608 0.03523 = 0.02180 0.00033 0.00082 0.02106 AFIX 43 H15 2 0.353637 0.409200 0.109154 11.00000 -1.20000 AFIX 0 C6 1 0.182478 0.638522 0.553604 11.00000 0.01835 0.02185 = 0.01819 -0.00132 -0.00041 0.00838 PART 2 C20 1 0.540213 -0.240589 0.055012 10.50000 0.05004 0.05001 = 0.05072 0.01287 0.01169 0.02288 AFIX 23 H20A 2 0.637053 -0.200109 0.038487 10.50000 -1.20000 H20B 2 0.526966 -0.316929 0.089297 10.50000 -1.20000 AFIX 0 PART 0 C18 1 -0.018996 0.156559 0.130989 11.00000 0.02484 0.04013 = 0.04786 -0.00919 0.00138 0.01425 AFIX 43 H18 2 -0.113334 0.092323 0.135472 11.00000 -1.20000 AFIX 0 C14 1 0.237315 0.317024 0.206814 11.00000 0.02645 0.02454 = 0.01931 -0.00018 -0.00035 0.01622 C17 1 0.005595 0.186565 0.041401 11.00000 0.04363 0.05583 = 0.03180 -0.01971 -0.01864 0.03141 AFIX 43 H17 2 -0.072497 0.140051 -0.014792 11.00000 -1.20000 AFIX 0 PART 2 C22 1 0.329932 -0.269425 -0.012539 -21.00000 0.03591 0.03484 = 0.03397 0.00990 0.00758 0.01442 AFIX 23 H22A 2 0.256509 -0.354924 0.002550 -21.00000 -1.20000 H22B 2 0.289733 -0.244945 -0.068744 -21.00000 -1.20000 AFIX 0 C21 1 0.432019 -0.269088 -0.013181 -21.00000 0.03784 0.03658 = 0.03661 0.01033 0.00851 0.01656 AFIX 13 H21 2 0.470718 -0.228176 -0.067312 -21.00000 -1.20000 AFIX 0 PART 0 PART 1 C22A 1 0.297961 -0.295796 0.015467 21.00000 0.04467 0.04359 = 0.04411 0.01150 0.01127 0.01813 AFIX 23 H22C 2 0.214798 -0.349102 0.043335 21.00000 -1.20000 H22D 2 0.269499 -0.299330 -0.054145 21.00000 -1.20000 AFIX 0 C21A 1 0.418091 -0.310391 0.039222 21.00000 0.03641 0.03458 = 0.03524 0.00980 0.00813 0.01568 AFIX 13 H21A 2 0.401272 -0.362656 0.091366 21.00000 -1.20000 AFIX 0 C20A 1 0.578879 -0.216297 0.060772 10.50000 0.01490 0.01506 = 0.01607 0.00166 0.00467 0.00773 AFIX 23 H20C 2 0.623063 -0.198903 0.003325 10.50000 -1.20000 H20D 2 0.639193 -0.231635 0.112040 10.50000 -1.20000 AFIX 0 HKLF 4 REM msb-vsk-294_mo_a.res in P-1 REM R1 = 0.0252 for 4043 Fo > 4sig(Fo) and 0.0284 for all 4353 data REM 326 parameters refined using 36 restraints END WGHT 0.0317 2.2667 REM Highest difference peak 0.839, deepest hole -0.526, 1-sigma level 0.122 Q1 1 0.2404 -0.2951 -0.0121 11.00000 0.05 0.84 Q2 1 0.5674 -0.0483 0.1154 11.00000 0.05 0.83 Q3 1 0.4339 0.2035 0.2791 11.00000 0.05 0.67 Q4 1 0.4218 0.4964 0.4564 11.00000 0.05 0.66 Q5 1 0.3405 0.3827 0.4146 11.00000 0.05 0.66 Q6 1 0.6380 0.3327 0.2812 11.00000 0.05 0.61 Q7 1 0.2227 0.3685 0.4558 11.00000 0.05 0.56 Q8 1 0.1046 0.1147 0.5232 11.00000 0.05 0.55 Q9 1 0.5345 -0.2171 0.0129 11.00000 0.05 0.53 Q10 1 0.3568 -0.3644 -0.0346 11.00000 0.05 0.52 Q11 1 0.3209 -0.3793 -0.1520 11.00000 0.05 0.51 Q12 1 0.6049 -0.1581 0.0395 11.00000 0.05 0.43 Q13 1 0.0238 0.1195 0.1776 11.00000 0.05 0.42 Q14 1 0.3530 -0.1639 0.1147 11.00000 0.05 0.42 Q15 1 0.3009 0.7859 0.4999 11.00000 0.05 0.41 Q16 1 0.2530 1.0619 0.2979 11.00000 0.05 0.41 Q17 1 0.6769 -0.2531 -0.0636 11.00000 0.05 0.39 Q18 1 0.0845 0.1393 0.7429 11.00000 0.05 0.38 Q19 1 0.0875 0.3608 0.6584 11.00000 0.05 0.38 Q20 1 0.4414 0.4991 0.3061 11.00000 0.05 0.37 ; _shelx_res_checksum 43538 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 Pd2 Pd 0.53200(3) 0.26381(3) 0.27805(2) 0.01663(8) Uani 1 1 d . . . . . Pd1 Pd 0.32093(3) 0.43290(3) 0.46103(2) 0.01666(8) Uani 1 1 d . . . . . Pd3 Pd 0.46494(3) -0.08613(3) 0.11274(2) 0.02406(9) Uani 1 1 d . . . . . Cl1 Cl 0.28272(11) 0.19993(10) 0.47405(7) 0.0263(2) Uani 1 1 d . . . . . Cl3 Cl 0.66388(10) 0.11253(10) 0.24302(8) 0.0287(2) Uani 1 1 d . . . . . P2 P 0.26803(10) 0.53516(10) 0.61218(7) 0.01756(19) Uani 1 1 d . . . . . P1 P 0.39585(10) 0.38949(10) 0.31266(7) 0.01821(19) Uani 1 1 d . . . . . Cl2 Cl 0.32500(10) 0.04853(10) 0.16193(8) 0.0313(2) Uani 1 1 d . . . . . O1 O 0.5669(3) 0.6357(3) 0.2562(2) 0.0283(6) Uani 1 1 d . . . . . O2 O 0.0746(3) 0.6557(3) 0.5706(2) 0.0281(6) Uani 1 1 d . . . . . N1 N 0.3358(3) 0.6272(3) 0.4315(2) 0.0173(6) Uani 1 1 d . . . . . C5 C 0.2665(4) 0.7028(4) 0.4785(3) 0.0199(7) Uani 1 1 d . . . . . C4 C 0.2731(4) 0.8331(4) 0.4609(3) 0.0254(8) Uani 1 1 d . . . . . H4 H 0.2215 0.8811 0.4929 0.031 Uiso 1 1 calc R U . . . C7 C 0.1362(4) 0.4357(4) 0.6805(3) 0.0221(8) Uani 1 1 d . . . . . C8 C 0.0750(4) 0.5103(4) 0.7447(3) 0.0282(9) Uani 1 1 d . . . . . H8 H 0.0992 0.6108 0.7511 0.034 Uiso 1 1 calc R U . . . C2 C 0.4284(4) 0.8139(4) 0.3463(3) 0.0253(8) Uani 1 1 d . . . . . H2 H 0.4854 0.8508 0.3014 0.030 Uiso 1 1 calc R U . . . C9 C -0.0220(4) 0.4344(5) 0.7987(3) 0.0312(9) Uani 1 1 d . . . . . H9 H -0.0646 0.4834 0.8403 0.037 Uiso 1 1 calc R U . . . C19 C 0.0976(4) 0.2224(5) 0.2154(3) 0.0322(9) Uani 1 1 d . . . . . H19 H 0.0817 0.2032 0.2766 0.039 Uiso 1 1 calc R U . . . C10 C -0.0551(5) 0.2880(5) 0.7912(3) 0.0351(10) Uani 1 1 d . . . . . H10 H -0.1186 0.2386 0.8290 0.042 Uiso 1 1 calc R U . . . C3 C 0.3574(5) 0.8917(4) 0.3951(3) 0.0292(9) Uani 1 1 d . . . . . H3 H 0.3664 0.9815 0.3839 0.035 Uiso 1 1 calc R U . . . C16 C 0.1406(5) 0.2822(5) 0.0325(3) 0.0393(11) Uani 1 1 d . . . . . H16 H 0.1538 0.3046 -0.0281 0.047 Uiso 1 1 calc R U . . . C11 C 0.0043(5) 0.2122(5) 0.7280(3) 0.0360(10) Uani 1 1 d . . . . . H11 H -0.0199 0.1120 0.7229 0.043 Uiso 1 1 calc R U . . . C12 C 0.1004(4) 0.2861(4) 0.6722(3) 0.0278(9) Uani 1 1 d . . . . . H12 H 0.1406 0.2356 0.6295 0.033 Uiso 1 1 calc R U . . . C1 C 0.4140(4) 0.6820(4) 0.3646(3) 0.0195(7) Uani 1 1 d . . . . . C13 C 0.4786(4) 0.5883(4) 0.3069(3) 0.0207(8) Uani 1 1 d . . . . . C15 C 0.2596(5) 0.3466(5) 0.1152(3) 0.0310(9) Uani 1 1 d . . . . . H15 H 0.3536 0.4092 0.1092 0.037 Uiso 1 1 calc R U . . . C6 C 0.1825(4) 0.6385(4) 0.5536(3) 0.0212(8) Uani 1 1 d . . . . . C20 C 0.5402(17) -0.2406(17) 0.0550(11) 0.050(5) Uani 0.5 1 d . U P A 2 H20A H 0.6371 -0.2001 0.0385 0.060 Uiso 0.5 1 calc R U P A 2 H20B H 0.5270 -0.3169 0.0893 0.060 Uiso 0.5 1 calc R U P A 2 C18 C -0.0190(5) 0.1566(5) 0.1310(4) 0.0420(11) Uani 1 1 d . . . . . H18 H -0.1133 0.0923 0.1355 0.050 Uiso 1 1 calc R U . . . C14 C 0.2373(4) 0.3170(4) 0.2068(3) 0.0233(8) Uani 1 1 d . . . . . C17 C 0.0056(5) 0.1866(6) 0.0414(4) 0.0483(13) Uani 1 1 d . . . . . H17 H -0.0725 0.1401 -0.0148 0.058 Uiso 1 1 calc R U . . . C22 C 0.3299(13) -0.2694(11) -0.0125(8) 0.035(3) Uani 0.499(14) 1 d . U P A 2 H22A H 0.2565 -0.3549 0.0025 0.042 Uiso 0.499(14) 1 calc R U P A 2 H22B H 0.2897 -0.2449 -0.0687 0.042 Uiso 0.499(14) 1 calc R U P A 2 C21 C 0.4320(10) -0.2691(10) -0.0132(8) 0.037(3) Uani 0.499(14) 1 d . U P A 2 H21 H 0.4707 -0.2282 -0.0673 0.044 Uiso 0.499(14) 1 calc R U P A 2 C22A C 0.2980(13) -0.2958(13) 0.0155(10) 0.045(3) Uani 0.501(14) 1 d . U P A 1 H22C H 0.2148 -0.3491 0.0433 0.054 Uiso 0.501(14) 1 calc R U P A 1 H22D H 0.2695 -0.2993 -0.0541 0.054 Uiso 0.501(14) 1 calc R U P A 1 C21A C 0.4181(10) -0.3104(10) 0.0392(7) 0.035(3) Uani 0.501(14) 1 d . U P A 1 H21A H 0.4013 -0.3627 0.0914 0.042 Uiso 0.501(14) 1 calc R U P A 1 C20A C 0.5789(11) -0.2163(11) 0.0608(7) 0.015(2) Uani 0.5 1 d . U P A 1 H20C H 0.6231 -0.1989 0.0033 0.018 Uiso 0.5 1 calc R U P A 1 H20D H 0.6392 -0.2316 0.1120 0.018 Uiso 0.5 1 calc R U P A 1 loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 Pd2 0.01891(15) 0.01554(14) 0.01547(15) 0.00257(11) 0.00398(11) 0.00853(11) Pd1 0.02003(15) 0.01539(14) 0.01542(15) 0.00335(11) 0.00320(11) 0.00934(11) Pd3 0.03270(17) 0.01882(16) 0.02087(16) 0.00403(12) 0.00763(13) 0.01199(13) Cl1 0.0357(5) 0.0184(4) 0.0281(5) 0.0072(4) 0.0068(4) 0.0147(4) Cl3 0.0247(5) 0.0216(5) 0.0368(6) -0.0010(4) 0.0040(4) 0.0126(4) P2 0.0191(4) 0.0166(4) 0.0168(5) 0.0037(4) 0.0043(4) 0.0082(4) P1 0.0206(5) 0.0185(5) 0.0165(5) 0.0029(4) 0.0036(4) 0.0107(4) Cl2 0.0255(5) 0.0219(5) 0.0375(6) -0.0050(4) -0.0023(4) 0.0106(4) O1 0.0304(14) 0.0324(15) 0.0280(15) 0.0134(12) 0.0119(12) 0.0158(12) O2 0.0258(14) 0.0362(16) 0.0275(15) 0.0065(12) 0.0057(12) 0.0201(13) N1 0.0186(14) 0.0182(15) 0.0140(15) 0.0016(12) -0.0005(12) 0.0094(12) C5 0.0194(17) 0.0224(19) 0.0140(18) 0.0002(14) -0.0014(14) 0.0091(15) C4 0.032(2) 0.023(2) 0.026(2) 0.0039(16) 0.0042(17) 0.0183(17) C7 0.0199(18) 0.0243(19) 0.0203(19) 0.0072(16) 0.0033(15) 0.0079(15) C8 0.026(2) 0.023(2) 0.030(2) 0.0032(17) 0.0078(17) 0.0069(16) C2 0.030(2) 0.0237(19) 0.021(2) 0.0098(16) 0.0038(16) 0.0097(16) C9 0.029(2) 0.033(2) 0.027(2) 0.0004(18) 0.0094(17) 0.0119(18) C19 0.029(2) 0.034(2) 0.030(2) -0.0012(18) 0.0036(17) 0.0150(18) C10 0.029(2) 0.041(3) 0.031(2) 0.019(2) 0.0083(18) 0.0068(19) C3 0.044(2) 0.020(2) 0.029(2) 0.0085(17) 0.0057(18) 0.0191(18) C16 0.050(3) 0.046(3) 0.020(2) -0.0031(19) -0.0042(19) 0.029(2) C11 0.037(2) 0.029(2) 0.044(3) 0.019(2) 0.012(2) 0.0122(19) C12 0.026(2) 0.024(2) 0.034(2) 0.0075(17) 0.0077(17) 0.0105(16) C1 0.0191(17) 0.0209(18) 0.0169(18) 0.0037(15) 0.0006(14) 0.0089(15) C13 0.0202(18) 0.0233(19) 0.0177(19) 0.0046(15) -0.0002(15) 0.0102(15) C15 0.036(2) 0.035(2) 0.022(2) 0.0003(17) 0.0008(17) 0.0211(19) C6 0.0183(18) 0.0218(19) 0.0182(19) -0.0013(15) -0.0004(14) 0.0084(15) C20 0.050(5) 0.050(5) 0.051(5) 0.0129(17) 0.0117(14) 0.023(2) C18 0.025(2) 0.040(3) 0.048(3) -0.009(2) 0.001(2) 0.0143(19) C14 0.0265(19) 0.0245(19) 0.0193(19) -0.0002(15) -0.0003(15) 0.0162(16) C17 0.044(3) 0.056(3) 0.032(3) -0.020(2) -0.019(2) 0.031(3) C22 0.036(3) 0.035(3) 0.034(3) 0.0099(12) 0.0076(11) 0.0144(14) C21 0.038(3) 0.037(3) 0.037(3) 0.0103(13) 0.0085(12) 0.0166(16) C22A 0.045(3) 0.044(3) 0.044(3) 0.0115(13) 0.0113(12) 0.0181(15) C21A 0.036(3) 0.035(3) 0.035(3) 0.0098(12) 0.0081(12) 0.0157(16) C20A 0.015(2) 0.015(2) 0.016(2) 0.0017(11) 0.0047(11) 0.0077(13) 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' Cl Cl 0.1484 0.1585 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' P P 0.1023 0.0942 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Pd Pd -0.9988 1.0072 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 P1 Pd2 P2 88.55(3) . 2_666 P1 Pd2 Cl2 92.89(3) . . P2 Pd2 Cl2 178.56(3) 2_666 . P1 Pd2 Cl3 175.69(3) . . P2 Pd2 Cl3 94.27(3) 2_666 . Cl2 Pd2 Cl3 84.29(3) . . N1 Pd1 P1 84.63(8) . . N1 Pd1 Cl1 172.49(8) . . P1 Pd1 Cl1 91.36(3) . . N1 Pd1 P2 82.94(8) . . P1 Pd1 P2 166.74(3) . . Cl1 Pd1 P2 101.49(3) . . C20 Pd3 C22 61.0(5) . . C21A Pd3 C22A 35.6(4) . . C21A Pd3 C20A 40.4(3) . . C22A Pd3 C20A 74.2(4) . . C20 Pd3 C21 34.9(5) . . C22 Pd3 C21 28.1(4) . . C20 Pd3 Cl2 167.3(4) . . C22 Pd3 Cl2 107.2(3) . . C21A Pd3 Cl2 136.5(2) . . C22A Pd3 Cl2 102.4(3) . . C20A Pd3 Cl2 176.4(3) . . C21 Pd3 Cl2 134.4(2) . . C20 Pd3 Cl3 106.9(4) . . C22 Pd3 Cl3 167.0(3) . . C21A Pd3 Cl3 133.7(3) . . C22A Pd3 Cl3 166.6(3) . . C20A Pd3 Cl3 98.4(3) . . C21 Pd3 Cl3 138.9(2) . . Cl2 Pd3 Cl3 85.23(3) . . Pd3 Cl3 Pd2 94.61(3) . . C7 P2 C6 105.50(16) . . C7 P2 Pd2 110.48(12) . 2_666 C6 P2 Pd2 98.99(11) . 2_666 C7 P2 Pd1 127.50(13) . . C6 P2 Pd1 93.55(12) . . Pd2 P2 Pd1 114.15(4) 2_666 . C14 P1 C13 96.57(16) . . C14 P1 Pd2 108.93(12) . . C13 P1 Pd2 115.97(12) . . C14 P1 Pd1 109.38(12) . . C13 P1 Pd1 97.20(12) . . Pd2 P1 Pd1 124.88(4) . . Pd3 Cl2 Pd2 95.08(3) . . C5 N1 C1 118.3(3) . . C5 N1 Pd1 120.4(2) . . C1 N1 Pd1 121.3(2) . . N1 C5 C4 122.4(3) . . N1 C5 C6 116.3(3) . . C4 C5 C6 121.3(3) . . C5 C4 C3 119.2(3) . . C5 C4 H4 120.4 . . C3 C4 H4 120.4 . . C12 C7 C8 119.7(3) . . C12 C7 P2 119.9(3) . . C8 C7 P2 120.4(3) . . C9 C8 C7 119.8(4) . . C9 C8 H8 120.1 . . C7 C8 H8 120.1 . . C1 C2 C3 119.6(3) . . C1 C2 H2 120.2 . . C3 C2 H2 120.2 . . C10 C9 C8 120.2(4) . . C10 C9 H9 119.9 . . C8 C9 H9 119.9 . . C14 C19 C18 119.1(4) . . C14 C19 H19 120.5 . . C18 C19 H19 120.5 . . C9 C10 C11 120.8(4) . . C9 C10 H10 119.6 . . C11 C10 H10 119.6 . . C4 C3 C2 118.6(3) . . C4 C3 H3 120.7 . . C2 C3 H3 120.7 . . C17 C16 C15 119.3(4) . . C17 C16 H16 120.3 . . C15 C16 H16 120.3 . . C10 C11 C12 119.8(4) . . C10 C11 H11 120.1 . . C12 C11 H11 120.1 . . C7 C12 C11 119.7(4) . . C7 C12 H12 120.1 . . C11 C12 H12 120.1 . . N1 C1 C2 121.9(3) . . N1 C1 C13 117.0(3) . . C2 C1 C13 121.0(3) . . O1 C13 C1 122.1(3) . . O1 C13 P1 124.4(3) . . C1 C13 P1 113.3(2) . . C16 C15 C14 119.8(4) . . C16 C15 H15 120.1 . . C14 C15 H15 120.1 . . O2 C6 C5 121.7(3) . . O2 C6 P2 127.2(3) . . C5 C6 P2 111.1(2) . . C21 C20 Pd3 76.2(8) . . C21 C20 H20A 115.8 . . Pd3 C20 H20A 115.8 . . C21 C20 H20B 115.8 . . Pd3 C20 H20B 115.8 . . H20A C20 H20B 112.8 . . C17 C18 C19 119.9(4) . . C17 C18 H18 120.0 . . C19 C18 H18 120.0 . . C19 C14 C15 120.0(4) . . C19 C14 P1 119.8(3) . . C15 C14 P1 119.9(3) . . C16 C17 C18 121.7(4) . . C16 C17 H17 119.1 . . C18 C17 H17 119.1 . . C21 C22 Pd3 78.3(8) . . C21 C22 H22A 115.5 . . Pd3 C22 H22A 115.5 . . C21 C22 H22B 115.5 . . Pd3 C22 H22B 115.5 . . H22A C22 H22B 112.5 . . C22 C21 C20 133.7(13) . . C22 C21 Pd3 73.5(7) . . C20 C21 Pd3 68.9(8) . . C22 C21 H21 108.4 . . C20 C21 H21 108.4 . . Pd3 C21 H21 108.4 . . C21A C22A Pd3 71.2(6) . . C21A C22A H22C 116.5 . . Pd3 C22A H22C 116.5 . . C21A C22A H22D 116.5 . . Pd3 C22A H22D 116.5 . . H22C C22A H22D 113.5 . . C22A C21A C20A 137.3(9) . . C22A C21A Pd3 73.2(6) . . C20A C21A Pd3 70.7(5) . . C22A C21A H21A 105.6 . . C20A C21A H21A 105.6 . . Pd3 C21A H21A 105.6 . . C21A C20A Pd3 68.8(5) . . C21A C20A H20C 116.8 . . Pd3 C20A H20C 116.8 . . C21A C20A H20D 116.8 . . Pd3 C20A H20D 116.8 . . H20C C20A H20D 113.8 . . loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 Pd2 P1 2.2448(9) . Pd2 P2 2.2881(9) 2_666 Pd2 Cl2 2.4108(10) . Pd2 Cl3 2.4154(9) . Pd1 N1 2.056(3) . Pd1 P1 2.2835(9) . Pd1 Cl1 2.2930(9) . Pd1 P2 2.3451(9) . Pd3 C20 2.055(15) . Pd3 C22 2.095(10) . Pd3 C21A 2.113(9) . Pd3 C22A 2.137(11) . Pd3 C20A 2.139(9) . Pd3 C21 2.139(9) . Pd3 Cl2 2.3849(10) . Pd3 Cl3 2.3983(10) . P2 C7 1.815(4) . P2 C6 1.866(4) . P2 Pd2 2.2881(9) 2_666 P1 C14 1.832(4) . P1 C13 1.873(4) . O1 C13 1.207(4) . O2 C6 1.209(4) . N1 C5 1.348(5) . N1 C1 1.350(5) . C5 C4 1.376(5) . C5 C6 1.508(5) . C4 C3 1.381(6) . C4 H4 0.9300 . C7 C12 1.388(5) . C7 C8 1.395(5) . C8 C9 1.384(5) . C8 H8 0.9300 . C2 C1 1.374(5) . C2 C3 1.386(6) . C2 H2 0.9300 . C9 C10 1.364(6) . C9 H9 0.9300 . C19 C14 1.385(6) . C19 C18 1.394(6) . C19 H19 0.9300 . C10 C11 1.381(6) . C10 H10 0.9300 . C3 H3 0.9300 . C16 C17 1.355(7) . C16 C15 1.393(6) . C16 H16 0.9300 . C11 C12 1.390(6) . C11 H11 0.9300 . C12 H12 0.9300 . C1 C13 1.501(5) . C15 C14 1.393(5) . C15 H15 0.9300 . C20 C21 1.260(17) . C20 H20A 0.9700 . C20 H20B 0.9700 . C18 C17 1.371(7) . C18 H18 0.9300 . C17 H17 0.9300 . C22 C21 1.030(13) . C22 H22A 0.9700 . C22 H22B 0.9700 . C21 H21 0.9800 . C22A C21A 1.299(14) . C22A H22C 0.9700 . C22A H22D 0.9700 . C21A C20A 1.469(13) . C21A H21A 0.9800 . C20A H20C 0.9700 . C20A H20D 0.9700 . 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 C1 N1 C5 C4 -0.2(5) . Pd1 N1 C5 C4 -179.9(3) . C1 N1 C5 C6 -179.1(3) . Pd1 N1 C5 C6 1.2(4) . N1 C5 C4 C3 -2.1(6) . C6 C5 C4 C3 176.8(3) . C6 P2 C7 C12 134.4(3) . Pd2 P2 C7 C12 -119.6(3) 2_666 Pd1 P2 C7 C12 27.3(4) . C6 P2 C7 C8 -48.3(3) . Pd2 P2 C7 C8 57.8(3) 2_666 Pd1 P2 C7 C8 -155.3(3) . C12 C7 C8 C9 -0.6(6) . P2 C7 C8 C9 -178.0(3) . C7 C8 C9 C10 1.5(6) . C8 C9 C10 C11 -1.5(6) . C5 C4 C3 C2 2.3(6) . C1 C2 C3 C4 -0.3(6) . C9 C10 C11 C12 0.7(7) . C8 C7 C12 C11 -0.1(6) . P2 C7 C12 C11 177.3(3) . C10 C11 C12 C7 0.1(6) . C5 N1 C1 C2 2.2(5) . Pd1 N1 C1 C2 -178.1(3) . C5 N1 C1 C13 -174.8(3) . Pd1 N1 C1 C13 4.9(4) . C3 C2 C1 N1 -2.0(6) . C3 C2 C1 C13 174.9(3) . N1 C1 C13 O1 -169.4(3) . C2 C1 C13 O1 13.6(5) . N1 C1 C13 P1 15.8(4) . C2 C1 C13 P1 -161.2(3) . C14 P1 C13 O1 -88.8(3) . Pd2 P1 C13 O1 26.0(4) . Pd1 P1 C13 O1 160.6(3) . C14 P1 C13 C1 85.9(3) . Pd2 P1 C13 C1 -159.3(2) . Pd1 P1 C13 C1 -24.7(3) . C17 C16 C15 C14 -2.6(6) . N1 C5 C6 O2 -150.8(3) . C4 C5 C6 O2 30.2(5) . N1 C5 C6 P2 29.3(4) . C4 C5 C6 P2 -149.6(3) . C7 P2 C6 O2 10.8(4) . Pd2 P2 C6 O2 -103.5(3) 2_666 Pd1 P2 C6 O2 141.4(3) . C7 P2 C6 C5 -169.3(2) . Pd2 P2 C6 C5 76.4(2) 2_666 Pd1 P2 C6 C5 -38.8(2) . C14 C19 C18 C17 -0.4(6) . C18 C19 C14 C15 0.7(6) . C18 C19 C14 P1 -173.7(3) . C16 C15 C14 C19 0.7(6) . C16 C15 C14 P1 175.2(3) . C13 P1 C14 C19 -135.7(3) . Pd2 P1 C14 C19 104.0(3) . Pd1 P1 C14 C19 -35.6(3) . C13 P1 C14 C15 49.9(3) . Pd2 P1 C14 C15 -70.5(3) . Pd1 P1 C14 C15 149.9(3) . C15 C16 C17 C18 3.0(7) . C19 C18 C17 C16 -1.5(7) . Pd3 C22 C21 C20 36.6(16) . Pd3 C20 C21 C22 -37.8(16) . Pd3 C22A C21A C20A -33.4(13) . C22A C21A C20A Pd3 34.0(13) .