data_global #============================================================================== # 1. SUBMISSION DETAILS _publ_contact_author_name 'Prof. Dr. Franc Meyer' _publ_contact_author_address ; Institut f\"ur Anorganische Chemie Georg August Universit\"at G\"ottingen Tammannstra\&se 4 D-37077 G\"ottingen Germany ; _publ_contact_author_email 'franc.meyer@chemie.uni-goettingen.de' _publ_contact_author_fax '49(551)393063' _publ_contact_author_phone '49(551)393012' _publ_requested_journal 'Organometallics' _publ_requested_coeditor_name ? #============================================================================== # 3. TITLE AND AUTHOR LIST _publ_section_title ; A Convenient Synthetic Route to Palladium Complexes of Unconventional N-Heterocyclic Carbenes Derived from Pyridazine and Phthalazine ; loop_ _publ_author_name _publ_author_address 'Guo, Tongxun' ; Institut f\"ur Anorganische Chemie Georg-August-Universit\"at G\"ottingen Tammannstra\&se 4 D-37077 G\"ottingen Germany ; 'Dechert, Sebastian' ; Institut f\"ur Anorganische Chemie Georg-August-Universit\"at G\"ottingen Tammannstra\&se 4 D-37077 G\"ottingen Germany ; 'Meyer, Steffen' ; Institut f\"ur Anorganische Chemie Georg-August-Universit\"at G\"ottingen Tammannstra\&se 4 D-37077 G\"ottingen Germany ; 'Meyer, Franc' ; Institut f\"ur Anorganische Chemie Georg-August-Universit\"at G\"ottingen Tammannstra\&se 4 D-37077 G\"ottingen Germany ; #============================================================================== data_1-togu15 _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety 'C42 H37 Cl2 N2 P2 Pd +, B F4 -' _chemical_formula_sum 'C42 H37 B Cl2 F4 N2 P2 Pd' _chemical_formula_weight 895.79 loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source 'C' 'C' 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'H' 'H' 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'N' 'N' 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' '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' 'Cl' 'Cl' 0.1484 0.1585 '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' _symmetry_cell_setting Monoclinic _symmetry_space_group_name_H-M 'P 21/c' loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, y+1/2, -z+1/2' '-x, -y, -z' 'x, -y-1/2, z-1/2' _cell_length_a 14.2981(4) _cell_length_b 10.7660(2) _cell_length_c 25.5110(7) _cell_angle_alpha 90.00 _cell_angle_beta 92.774(2) _cell_angle_gamma 90.00 _cell_volume 3922.39(17) _cell_formula_units_Z 4 _cell_measurement_temperature 133(2) _cell_measurement_reflns_used 46183 _cell_measurement_theta_min 1.43 _cell_measurement_theta_max 25.64 _exptl_crystal_description block _exptl_crystal_colour colorless _exptl_crystal_size_max 0.38 _exptl_crystal_size_mid 0.08 _exptl_crystal_size_min 0.07 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.517 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1816 _exptl_absorpt_coefficient_mu 0.744 _exptl_absorpt_correction_type numerical _exptl_absorpt_correction_T_min 0.6353 _exptl_absorpt_correction_T_max 0.8886 _exptl_absorpt_process_details 'X-RED (Stoe & Cie, 2002)' _exptl_special_details ; ? ; _diffrn_ambient_temperature 133(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'Stoe IPDS II' _diffrn_measurement_method \w _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 46183 _diffrn_reflns_av_R_equivalents 0.0685 _diffrn_reflns_av_sigmaI/netI 0.0327 _diffrn_reflns_limit_h_min -17 _diffrn_reflns_limit_h_max 17 _diffrn_reflns_limit_k_min -13 _diffrn_reflns_limit_k_max 12 _diffrn_reflns_limit_l_min -30 _diffrn_reflns_limit_l_max 30 _diffrn_reflns_theta_min 1.43 _diffrn_reflns_theta_max 25.64 _reflns_number_total 7391 _reflns_number_gt 6544 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'X-AREA (Stoe & Cie, 2002)' _computing_cell_refinement 'X-AREA (Stoe & Cie, 2002)' _computing_data_reduction 'X-AREA (Stoe & Cie, 2002)' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'DIAMOND (Brandenburg, 2001)' _computing_publication_material 'SHELXL-97 (Sheldrick, 1997)' _refine_special_details ; Refinement of F^2^ against ALL reflections. The weighted R-factor wR and goodness of fit S are based on F^2^, conventional R-factors R are based on F, with F set to zero for negative F^2^. The threshold expression of F^2^ > 2sigma(F^2^) is used only for calculating R-factors(gt) etc. and is not relevant to the choice of reflections for refinement. R-factors based on F^2^ are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger. ; _refine_ls_structure_factor_coef Fsqd _refine_ls_matrix_type full _refine_ls_weighting_scheme calc _refine_ls_weighting_details 'calc w=1/[\s^2^(Fo^2^)+(0.0315P)^2^+3.2015P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment constr _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 7391 _refine_ls_number_parameters 504 _refine_ls_number_restraints 58 _refine_ls_R_factor_all 0.0347 _refine_ls_R_factor_gt 0.0282 _refine_ls_wR_factor_ref 0.0682 _refine_ls_wR_factor_gt 0.0660 _refine_ls_goodness_of_fit_ref 1.017 _refine_ls_restrained_S_all 1.027 _refine_ls_shift/su_max 0.003 _refine_ls_shift/su_mean 0.000 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_symmetry_multiplicity _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group Pd1 Pd 0.657760(10) 0.377650(15) 0.398759(6) 0.01488(6) Uani 1 1 d . . . Cl1 Cl 0.59718(4) 0.33940(6) 0.48089(2) 0.02378(12) Uani 1 1 d . . . Cl2 Cl 0.82586(5) 0.51722(8) 0.17711(3) 0.04517(18) Uani 1 1 d . . . P1 P 0.52685(4) 0.27965(5) 0.35939(2) 0.01528(11) Uani 1 1 d . . . P2 P 0.80037(4) 0.43717(5) 0.43961(2) 0.01687(12) Uani 1 1 d . . . N1 N 0.69174(12) 0.52148(18) 0.30328(7) 0.0185(4) Uani 1 1 d . . . N2 N 0.72586(13) 0.55418(19) 0.25651(8) 0.0227(4) Uani 1 1 d . . . C1 C 0.70859(14) 0.4149(2) 0.32899(8) 0.0168(4) Uani 1 1 d . . . C2 C 0.76621(15) 0.3285(2) 0.30371(9) 0.0199(4) Uani 1 1 d . . . H2 H 0.7793 0.2502 0.3196 0.024 Uiso 1 1 calc R . . C3 C 0.80299(16) 0.3565(2) 0.25694(10) 0.0251(5) Uani 1 1 d . . . H3 H 0.8421 0.2998 0.2397 0.030 Uiso 1 1 calc R . . C4 C 0.78029(16) 0.4734(2) 0.23538(9) 0.0251(5) Uani 1 1 d . . . C5 C 0.62886(16) 0.6198(2) 0.32251(10) 0.0251(5) Uani 1 1 d . . . H5A H 0.5966 0.5881 0.3533 0.030 Uiso 1 1 calc R . . H5B H 0.5805 0.6396 0.2947 0.030 Uiso 1 1 calc R . . C6 C 0.6813(2) 0.7363(3) 0.33778(13) 0.0399(7) Uani 1 1 d . . . H6A H 0.7201 0.7212 0.3698 0.060 Uiso 1 1 calc R . . H6B H 0.6366 0.8031 0.3440 0.060 Uiso 1 1 calc R . . H6C H 0.7213 0.7607 0.3094 0.060 Uiso 1 1 calc R . . C11 C 0.41481(14) 0.3573(2) 0.36096(9) 0.0178(4) Uani 1 1 d . . . C12 C 0.40172(15) 0.4538(2) 0.39619(8) 0.0188(4) Uani 1 1 d . . . H12 H 0.4524 0.4808 0.4188 0.023 Uiso 1 1 calc R . . C13 C 0.31492(15) 0.5104(2) 0.39830(9) 0.0212(5) Uani 1 1 d . . . H13 H 0.3061 0.5760 0.4225 0.025 Uiso 1 1 calc R . . C14 C 0.24095(16) 0.4714(2) 0.36516(9) 0.0242(5) Uani 1 1 d . . . H14 H 0.1816 0.5105 0.3667 0.029 Uiso 1 1 calc R . . C15 C 0.25330(16) 0.3752(2) 0.32975(9) 0.0245(5) Uani 1 1 d . . . H15 H 0.2024 0.3486 0.3072 0.029 Uiso 1 1 calc R . . C16 C 0.33992(15) 0.3184(2) 0.32746(9) 0.0216(5) Uani 1 1 d . . . H16 H 0.3486 0.2530 0.3032 0.026 Uiso 1 1 calc R . . C17 C 0.51300(16) 0.1281(2) 0.38946(8) 0.0196(4) Uani 1 1 d . . . C18 C 0.42542(17) 0.0781(2) 0.39928(9) 0.0236(5) Uani 1 1 d . . . H18 H 0.3698 0.1209 0.3882 0.028 Uiso 1 1 calc R . . C19 C 0.42021(19) -0.0352(2) 0.42541(10) 0.0303(6) Uani 1 1 d . . . H19 H 0.3608 -0.0690 0.4326 0.036 Uiso 1 1 calc R . . C20 C 0.5004(2) -0.0985(2) 0.44084(10) 0.0336(6) Uani 1 1 d . . . H20 H 0.4961 -0.1752 0.4589 0.040 Uiso 1 1 calc R . . C21 C 0.58707(19) -0.0509(2) 0.43015(10) 0.0306(5) Uani 1 1 d . . . H21 H 0.6422 -0.0962 0.4398 0.037 Uiso 1 1 calc R . . C22 C 0.59366(17) 0.0634(2) 0.40521(9) 0.0250(5) Uani 1 1 d . . . H22 H 0.6534 0.0973 0.3989 0.030 Uiso 1 1 calc R . . C23 C 0.54414(14) 0.2522(2) 0.29027(8) 0.0172(4) Uani 1 1 d . . . C24 C 0.59231(15) 0.1483(2) 0.27331(9) 0.0199(5) Uani 1 1 d . . . H24 H 0.6062 0.0818 0.2969 0.024 Uiso 1 1 calc R . . C25 C 0.62009(16) 0.1418(2) 0.22198(10) 0.0239(5) Uani 1 1 d . . . H25 H 0.6531 0.0709 0.2107 0.029 Uiso 1 1 calc R . . C26 C 0.60001(16) 0.2379(2) 0.18713(9) 0.0250(5) Uani 1 1 d . . . H26 H 0.6193 0.2329 0.1521 0.030 Uiso 1 1 calc R . . C27 C 0.55155(16) 0.3417(2) 0.20357(9) 0.0237(5) Uani 1 1 d . . . H27 H 0.5377 0.4078 0.1797 0.028 Uiso 1 1 calc R . . C28 C 0.52358(15) 0.3488(2) 0.25466(9) 0.0199(4) Uani 1 1 d . . . H28 H 0.4902 0.4197 0.2657 0.024 Uiso 1 1 calc R . . C31 C 0.79605(15) 0.5798(2) 0.47694(9) 0.0193(4) Uani 1 1 d . . . C32 C 0.70941(16) 0.6307(2) 0.48760(9) 0.0216(5) Uani 1 1 d . . . H32 H 0.6534 0.5918 0.4745 0.026 Uiso 1 1 calc R . . C33 C 0.70481(17) 0.7381(2) 0.51736(9) 0.0236(5) Uani 1 1 d . . . H33 H 0.6456 0.7722 0.5248 0.028 Uiso 1 1 calc R . . C34 C 0.78601(18) 0.7957(2) 0.53630(9) 0.0269(5) Uani 1 1 d . . . H34 H 0.7825 0.8687 0.5570 0.032 Uiso 1 1 calc R . . C35 C 0.87289(18) 0.7469(2) 0.52510(10) 0.0287(5) Uani 1 1 d . . . H35 H 0.9287 0.7874 0.5375 0.034 Uiso 1 1 calc R . . C36 C 0.87761(16) 0.6389(2) 0.49580(10) 0.0254(5) Uani 1 1 d . . . H36 H 0.9369 0.6048 0.4885 0.030 Uiso 1 1 calc R . . C37 C 0.89357(14) 0.4577(2) 0.39393(9) 0.0197(4) Uani 1 1 d . . . C38 C 0.90159(15) 0.5712(2) 0.36775(9) 0.0233(5) Uani 1 1 d . . . H38 H 0.8678 0.6416 0.3789 0.028 Uiso 1 1 calc R . . C39 C 0.95896(16) 0.5811(3) 0.32546(10) 0.0283(5) Uani 1 1 d . . . H39 H 0.9640 0.6582 0.3077 0.034 Uiso 1 1 calc R . . C40 C 1.00897(16) 0.4789(3) 0.30901(10) 0.0319(6) Uani 1 1 d . . . H40 H 1.0471 0.4854 0.2796 0.038 Uiso 1 1 calc R . . C41 C 1.00292(16) 0.3674(3) 0.33571(10) 0.0307(6) Uani 1 1 d . . . H41 H 1.0382 0.2978 0.3251 0.037 Uiso 1 1 calc R . . C42 C 0.94565(15) 0.3565(2) 0.37799(10) 0.0246(5) Uani 1 1 d . . . H42 H 0.9421 0.2796 0.3961 0.030 Uiso 1 1 calc R . . C43 C 0.84035(14) 0.3134(2) 0.48383(9) 0.0200(4) Uani 1 1 d . . . C44 C 0.83576(16) 0.1915(2) 0.46482(10) 0.0250(5) Uani 1 1 d . . . H44 H 0.8085 0.1758 0.4308 0.030 Uiso 1 1 calc R . . C45 C 0.87038(17) 0.0937(2) 0.49504(11) 0.0297(5) Uani 1 1 d . . . H45 H 0.8687 0.0116 0.4814 0.036 Uiso 1 1 calc R . . C46 C 0.90775(18) 0.1163(3) 0.54550(11) 0.0328(6) Uani 1 1 d . . . H46 H 0.9319 0.0495 0.5664 0.039 Uiso 1 1 calc R . . C47 C 0.90986(17) 0.2357(3) 0.56528(10) 0.0303(6) Uani 1 1 d . . . H47 H 0.9337 0.2502 0.6002 0.036 Uiso 1 1 calc R . . C48 C 0.87726(15) 0.3352(2) 0.53443(9) 0.0237(5) Uani 1 1 d . . . H48 H 0.8803 0.4175 0.5479 0.028 Uiso 1 1 calc R . . B1A B 0.8808(3) 0.0089(4) 0.33178(18) 0.0437(11) Uani 0.831(4) 1 d PD A 1 F1A F 0.79648(19) 0.0295(3) 0.35435(12) 0.0659(9) Uani 0.831(4) 1 d PD A 1 F2A F 0.8877(2) 0.0910(3) 0.29004(10) 0.0764(10) Uani 0.831(4) 1 d PD A 1 F3A F 0.95402(19) 0.0442(3) 0.36841(12) 0.0612(7) Uani 0.831(4) 1 d PD A 1 F4A F 0.8942(4) -0.1093(4) 0.31520(19) 0.0863(13) Uani 0.831(4) 1 d PD A 1 B1B B 0.8701(12) -0.0289(15) 0.3438(6) 0.0437(11) Uani 0.169(4) 1 d PD A 2 F1B F 0.8616(8) -0.0987(11) 0.3877(5) 0.0659(9) Uani 0.169(4) 1 d PD A 2 F2B F 0.7871(12) 0.0320(17) 0.3349(7) 0.0764(10) Uani 0.169(4) 1 d PD A 2 F3B F 0.9394(11) 0.0561(16) 0.3474(6) 0.0612(7) Uani 0.169(4) 1 d PD A 2 F4B F 0.882(2) -0.107(2) 0.3023(8) 0.0863(13) Uani 0.169(4) 1 d PD 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 Pd1 0.01495(8) 0.01593(9) 0.01371(9) 0.00048(6) 0.00035(6) -0.00101(6) Cl1 0.0268(3) 0.0294(3) 0.0154(2) 0.0008(2) 0.0031(2) -0.0070(2) Cl2 0.0549(4) 0.0531(5) 0.0294(3) 0.0119(3) 0.0220(3) 0.0049(3) P1 0.0159(2) 0.0153(3) 0.0147(3) -0.0003(2) 0.00069(19) -0.0011(2) P2 0.0151(2) 0.0182(3) 0.0171(3) 0.0001(2) -0.0004(2) -0.0003(2) N1 0.0170(8) 0.0204(10) 0.0183(9) 0.0025(7) 0.0015(7) 0.0003(7) N2 0.0240(9) 0.0256(11) 0.0187(9) 0.0046(8) 0.0028(7) -0.0023(8) C1 0.0144(9) 0.0181(11) 0.0176(10) -0.0007(8) -0.0022(8) -0.0037(8) C2 0.0187(10) 0.0204(11) 0.0206(11) -0.0015(9) 0.0000(8) -0.0001(9) C3 0.0218(11) 0.0282(13) 0.0258(12) -0.0049(10) 0.0038(9) 0.0004(9) C4 0.0241(11) 0.0319(14) 0.0195(11) 0.0020(10) 0.0036(9) -0.0044(10) C5 0.0260(11) 0.0223(12) 0.0272(12) 0.0047(10) 0.0053(9) 0.0077(10) C6 0.0374(14) 0.0299(15) 0.0516(18) -0.0141(13) -0.0069(13) 0.0080(12) C11 0.0176(10) 0.0176(11) 0.0183(11) 0.0029(8) 0.0015(8) -0.0012(8) C12 0.0215(10) 0.0199(11) 0.0151(10) 0.0020(8) 0.0005(8) -0.0029(9) C13 0.0247(11) 0.0221(12) 0.0172(10) -0.0003(9) 0.0048(9) 0.0019(9) C14 0.0193(10) 0.0300(13) 0.0234(12) 0.0028(10) 0.0033(9) 0.0035(9) C15 0.0189(10) 0.0301(13) 0.0241(12) -0.0016(10) -0.0007(9) -0.0039(9) C16 0.0204(10) 0.0230(12) 0.0215(11) -0.0028(9) 0.0027(9) -0.0025(9) C17 0.0273(11) 0.0163(11) 0.0155(10) -0.0019(8) 0.0028(8) -0.0016(9) C18 0.0284(11) 0.0215(12) 0.0214(11) -0.0045(9) 0.0071(9) -0.0025(9) C19 0.0429(14) 0.0226(13) 0.0268(13) -0.0030(10) 0.0153(11) -0.0115(11) C20 0.0605(17) 0.0205(13) 0.0203(12) 0.0041(10) 0.0067(11) -0.0043(12) C21 0.0444(15) 0.0236(13) 0.0235(12) 0.0037(10) -0.0002(11) 0.0034(11) C22 0.0291(12) 0.0228(12) 0.0227(12) 0.0019(9) -0.0005(9) -0.0003(10) C23 0.0164(10) 0.0171(11) 0.0179(10) -0.0017(8) -0.0002(8) -0.0038(8) C24 0.0236(11) 0.0166(11) 0.0196(11) -0.0005(8) 0.0006(9) -0.0031(8) C25 0.0270(11) 0.0193(12) 0.0256(12) -0.0049(9) 0.0046(9) -0.0029(9) C26 0.0290(12) 0.0280(13) 0.0183(11) -0.0012(10) 0.0047(9) -0.0075(10) C27 0.0290(12) 0.0227(12) 0.0192(11) 0.0017(9) -0.0003(9) -0.0039(9) C28 0.0226(10) 0.0167(11) 0.0203(11) -0.0010(9) -0.0012(8) -0.0007(8) C31 0.0223(10) 0.0183(11) 0.0174(10) 0.0025(9) 0.0003(8) -0.0008(9) C32 0.0240(11) 0.0224(12) 0.0182(11) 0.0045(9) 0.0000(9) -0.0008(9) C33 0.0307(12) 0.0211(12) 0.0193(11) 0.0030(9) 0.0039(9) 0.0056(9) C34 0.0414(14) 0.0175(12) 0.0217(12) 0.0006(9) 0.0005(10) -0.0017(10) C35 0.0306(12) 0.0245(13) 0.0305(13) -0.0004(10) -0.0046(10) -0.0067(10) C36 0.0230(11) 0.0246(13) 0.0283(13) -0.0007(10) -0.0023(9) -0.0015(9) C37 0.0147(9) 0.0261(12) 0.0179(10) 0.0009(9) -0.0021(8) -0.0015(9) C38 0.0195(10) 0.0262(12) 0.0239(12) 0.0018(10) -0.0021(9) -0.0013(9) C39 0.0251(12) 0.0347(14) 0.0251(12) 0.0058(11) 0.0003(10) -0.0071(10) C40 0.0183(11) 0.0517(17) 0.0259(13) -0.0005(12) 0.0020(9) -0.0048(11) C41 0.0176(11) 0.0411(15) 0.0335(14) -0.0047(12) 0.0031(10) 0.0042(10) C42 0.0176(10) 0.0283(13) 0.0277(12) 0.0016(10) -0.0017(9) 0.0015(9) C43 0.0167(10) 0.0215(12) 0.0220(11) 0.0024(9) 0.0015(8) -0.0002(9) C44 0.0272(11) 0.0236(13) 0.0240(12) 0.0012(10) -0.0007(9) -0.0034(10) C45 0.0333(13) 0.0210(13) 0.0348(14) 0.0048(10) 0.0014(11) 0.0007(10) C46 0.0324(13) 0.0312(14) 0.0346(14) 0.0164(12) -0.0010(11) 0.0012(11) C47 0.0302(12) 0.0379(15) 0.0224(12) 0.0079(11) -0.0032(10) -0.0044(11) C48 0.0207(11) 0.0274(13) 0.0227(12) 0.0005(10) -0.0002(9) -0.0029(9) B1A 0.043(2) 0.045(3) 0.044(3) -0.007(2) 0.0103(18) 0.013(2) F1A 0.0502(13) 0.0784(19) 0.071(2) -0.0298(18) 0.0205(13) -0.0014(13) F2A 0.117(2) 0.0610(17) 0.0539(16) 0.0065(13) 0.0259(15) 0.0448(16) F3A 0.0547(14) 0.0737(17) 0.054(2) 0.0011(16) -0.0075(13) 0.0165(12) F4A 0.109(3) 0.0359(12) 0.119(3) -0.0173(19) 0.058(3) 0.0019(14) B1B 0.043(2) 0.045(3) 0.044(3) -0.007(2) 0.0103(18) 0.013(2) F1B 0.0502(13) 0.0784(19) 0.071(2) -0.0298(18) 0.0205(13) -0.0014(13) F2B 0.117(2) 0.0610(17) 0.0539(16) 0.0065(13) 0.0259(15) 0.0448(16) F3B 0.0547(14) 0.0737(17) 0.054(2) 0.0011(16) -0.0075(13) 0.0165(12) F4B 0.109(3) 0.0359(12) 0.119(3) -0.0173(19) 0.058(3) 0.0019(14) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; 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 Pd1 C1 1.996(2) . ? Pd1 P1 2.3331(5) . ? Pd1 P2 2.3343(5) . ? Pd1 Cl1 2.3422(5) . ? Cl2 C4 1.718(2) . ? P1 C11 1.809(2) . ? P1 C23 1.817(2) . ? P1 C17 1.817(2) . ? P2 C31 1.810(2) . ? P2 C43 1.820(2) . ? P2 C37 1.826(2) . ? N1 C1 1.337(3) . ? N1 N2 1.357(3) . ? N1 C5 1.487(3) . ? N2 C4 1.301(3) . ? C1 C2 1.419(3) . ? C2 C3 1.361(3) . ? C3 C4 1.405(4) . ? C5 C6 1.503(4) . ? C11 C12 1.392(3) . ? C11 C16 1.401(3) . ? C12 C13 1.386(3) . ? C13 C14 1.387(3) . ? C14 C15 1.391(3) . ? C15 C16 1.385(3) . ? C17 C22 1.390(3) . ? C17 C18 1.397(3) . ? C18 C19 1.394(4) . ? C19 C20 1.374(4) . ? C20 C21 1.380(4) . ? C21 C22 1.390(4) . ? C23 C24 1.394(3) . ? C23 C28 1.403(3) . ? C24 C25 1.388(3) . ? C25 C26 1.385(3) . ? C26 C27 1.391(3) . ? C27 C28 1.384(3) . ? C31 C36 1.393(3) . ? C31 C32 1.393(3) . ? C32 C33 1.386(3) . ? C33 C34 1.383(3) . ? C34 C35 1.391(4) . ? C35 C36 1.386(4) . ? C37 C42 1.391(3) . ? C37 C38 1.400(3) . ? C38 C39 1.391(3) . ? C39 C40 1.388(4) . ? C40 C41 1.385(4) . ? C41 C42 1.390(4) . ? C43 C48 1.391(3) . ? C43 C44 1.399(3) . ? C44 C45 1.382(3) . ? C45 C46 1.391(4) . ? C46 C47 1.380(4) . ? C47 C48 1.397(4) . ? B1A F4A 1.357(6) . ? B1A F1A 1.379(5) . ? B1A F2A 1.391(5) . ? B1A F3A 1.420(5) . ? B1B F3B 1.348(14) . ? B1B F1B 1.359(14) . ? B1B F2B 1.366(14) . ? B1B F4B 1.367(14) . ? 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 C1 Pd1 P1 91.50(6) . . ? C1 Pd1 P2 89.72(6) . . ? P1 Pd1 P2 168.99(2) . . ? C1 Pd1 Cl1 178.51(7) . . ? P1 Pd1 Cl1 88.962(19) . . ? P2 Pd1 Cl1 90.10(2) . . ? C11 P1 C23 105.01(10) . . ? C11 P1 C17 106.91(10) . . ? C23 P1 C17 106.64(10) . . ? C11 P1 Pd1 118.31(7) . . ? C23 P1 Pd1 110.33(7) . . ? C17 P1 Pd1 109.01(7) . . ? C31 P2 C43 108.24(11) . . ? C31 P2 C37 106.13(11) . . ? C43 P2 C37 105.49(10) . . ? C31 P2 Pd1 114.62(7) . . ? C43 P2 Pd1 108.49(7) . . ? C37 P2 Pd1 113.39(7) . . ? C1 N1 N2 126.13(19) . . ? C1 N1 C5 123.10(18) . . ? N2 N1 C5 110.74(18) . . ? C4 N2 N1 116.0(2) . . ? N1 C1 C2 115.8(2) . . ? N1 C1 Pd1 123.03(16) . . ? C2 C1 Pd1 121.20(16) . . ? C3 C2 C1 120.7(2) . . ? C2 C3 C4 116.7(2) . . ? N2 C4 C3 124.6(2) . . ? N2 C4 Cl2 115.75(19) . . ? C3 C4 Cl2 119.65(19) . . ? N1 C5 C6 112.18(19) . . ? C12 C11 C16 119.6(2) . . ? C12 C11 P1 120.39(16) . . ? C16 C11 P1 119.96(17) . . ? C13 C12 C11 120.1(2) . . ? C12 C13 C14 120.1(2) . . ? C13 C14 C15 120.3(2) . . ? C16 C15 C14 119.9(2) . . ? C15 C16 C11 120.0(2) . . ? C22 C17 C18 119.5(2) . . ? C22 C17 P1 117.80(17) . . ? C18 C17 P1 122.61(18) . . ? C19 C18 C17 119.5(2) . . ? C20 C19 C18 120.5(2) . . ? C19 C20 C21 120.3(2) . . ? C20 C21 C22 120.0(2) . . ? C21 C22 C17 120.2(2) . . ? C24 C23 C28 119.0(2) . . ? C24 C23 P1 121.63(17) . . ? C28 C23 P1 118.29(17) . . ? C25 C24 C23 120.1(2) . . ? C26 C25 C24 120.5(2) . . ? C25 C26 C27 119.9(2) . . ? C28 C27 C26 119.9(2) . . ? C27 C28 C23 120.5(2) . . ? C36 C31 C32 119.4(2) . . ? C36 C31 P2 121.30(18) . . ? C32 C31 P2 119.31(17) . . ? C33 C32 C31 120.1(2) . . ? C34 C33 C32 120.3(2) . . ? C33 C34 C35 120.1(2) . . ? C36 C35 C34 119.7(2) . . ? C35 C36 C31 120.5(2) . . ? C42 C37 C38 119.1(2) . . ? C42 C37 P2 120.63(18) . . ? C38 C37 P2 119.29(17) . . ? C39 C38 C37 120.1(2) . . ? C40 C39 C38 120.4(2) . . ? C41 C40 C39 119.5(2) . . ? C40 C41 C42 120.5(2) . . ? C41 C42 C37 120.3(2) . . ? C48 C43 C44 119.3(2) . . ? C48 C43 P2 123.03(18) . . ? C44 C43 P2 117.63(17) . . ? C45 C44 C43 120.8(2) . . ? C44 C45 C46 119.6(2) . . ? C47 C46 C45 120.1(2) . . ? C46 C47 C48 120.5(2) . . ? C43 C48 C47 119.6(2) . . ? F4A B1A F1A 114.8(5) . . ? F4A B1A F2A 109.9(4) . . ? F1A B1A F2A 108.2(4) . . ? F4A B1A F3A 110.3(4) . . ? F1A B1A F3A 108.3(3) . . ? F2A B1A F3A 104.8(4) . . ? F3B B1B F1B 114.4(12) . . ? F3B B1B F2B 108.4(12) . . ? F1B B1B F2B 106.8(11) . . ? F3B B1B F4B 110.4(12) . . ? F1B B1B F4B 108.6(12) . . ? F2B B1B F4B 107.9(13) . . ? _diffrn_measured_fraction_theta_max 0.997 _diffrn_reflns_theta_full 25.64 _diffrn_measured_fraction_theta_full 0.997 _refine_diff_density_max 0.664 _refine_diff_density_min -0.447 _refine_diff_density_rms 0.061 #============================================================================== data_2-togu21 _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety 'C46 H39 Cl2 N2 P2 Pd +, B F4 -, C H2 Cl2' _chemical_formula_sum 'C47 H41 B Cl4 F4 N2 P2 Pd' _chemical_formula_weight 1030.77 loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source 'C' 'C' 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'H' 'H' 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'N' 'N' 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' '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' 'P' 'P' 0.1023 0.0942 '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' 'Pd' 'Pd' -0.9988 1.0072 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting Orthorhombic _symmetry_space_group_name_H-M 'P n m a' loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x+1/2, -y, z+1/2' '-x, y+1/2, -z' 'x+1/2, -y+1/2, -z+1/2' '-x, -y, -z' 'x-1/2, y, -z-1/2' 'x, -y-1/2, z' '-x-1/2, y-1/2, z-1/2' _cell_length_a 20.2183(4) _cell_length_b 14.8686(4) _cell_length_c 15.0359(3) _cell_angle_alpha 90.00 _cell_angle_beta 90.00 _cell_angle_gamma 90.00 _cell_volume 4520.06(18) _cell_formula_units_Z 4 _cell_measurement_temperature 133(2) _cell_measurement_reflns_used 51589 _cell_measurement_theta_min 1.69 _cell_measurement_theta_max 26.77 _exptl_crystal_description block _exptl_crystal_colour colorless _exptl_crystal_size_max 0.2 _exptl_crystal_size_mid 0.18 _exptl_crystal_size_min 0.16 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.515 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 2088 _exptl_absorpt_coefficient_mu 0.771 _exptl_absorpt_correction_type numerical _exptl_absorpt_correction_T_min 0.7482 _exptl_absorpt_correction_T_max 0.9079 _exptl_absorpt_process_details 'X-RED (Stoe & Cie, 2002)' _exptl_special_details ; ? ; _diffrn_ambient_temperature 133(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'Stoe IPDS II' _diffrn_measurement_method \w _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 51589 _diffrn_reflns_av_R_equivalents 0.0662 _diffrn_reflns_av_sigmaI/netI 0.0298 _diffrn_reflns_limit_h_min -25 _diffrn_reflns_limit_h_max 25 _diffrn_reflns_limit_k_min -18 _diffrn_reflns_limit_k_max 18 _diffrn_reflns_limit_l_min -19 _diffrn_reflns_limit_l_max 18 _diffrn_reflns_theta_min 1.69 _diffrn_reflns_theta_max 26.77 _reflns_number_total 4987 _reflns_number_gt 4277 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'X-AREA (Stoe & Cie, 2002)' _computing_cell_refinement 'X-AREA (Stoe & Cie, 2002)' _computing_data_reduction 'X-AREA (Stoe & Cie, 2002)' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'DIAMOND (Brandenburg, 2001)' _computing_publication_material 'SHELXL-97 (Sheldrick, 1997)' _refine_special_details ; Refinement of F^2^ against ALL reflections. The weighted R-factor wR and goodness of fit S are based on F^2^, conventional R-factors R are based on F, with F set to zero for negative F^2^. The threshold expression of F^2^ > 2sigma(F^2^) is used only for calculating R-factors(gt) etc. and is not relevant to the choice of reflections for refinement. R-factors based on F^2^ are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger. ; _refine_ls_structure_factor_coef Fsqd _refine_ls_matrix_type full _refine_ls_weighting_scheme calc _refine_ls_weighting_details 'calc w=1/[\s^2^(Fo^2^)+(0.0583P)^2^+10.2999P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment constr _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 4987 _refine_ls_number_parameters 308 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0637 _refine_ls_R_factor_gt 0.0508 _refine_ls_wR_factor_ref 0.1246 _refine_ls_wR_factor_gt 0.1181 _refine_ls_goodness_of_fit_ref 1.072 _refine_ls_restrained_S_all 1.072 _refine_ls_shift/su_max 0.001 _refine_ls_shift/su_mean 0.000 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_symmetry_multiplicity _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group Pd1 Pd 0.284397(18) 0.2500 0.34551(2) 0.01979(11) Uani 1 2 d S . . Cl1 Cl 0.47907(9) 0.2500 0.68408(12) 0.0560(5) Uani 1 2 d S . . Cl2 Cl 0.21288(6) 0.2500 0.22220(8) 0.0272(3) Uani 1 2 d S . . N1 N 0.3285(2) 0.2500 0.5301(3) 0.0272(9) Uani 1 2 d S . . N2 N 0.3691(3) 0.2500 0.6036(3) 0.0376(11) Uani 1 2 d S . . P1 P 0.28681(4) 0.40760(6) 0.34671(6) 0.02108(19) Uani 1 1 d . . . C1 C 0.3490(2) 0.2500 0.4453(3) 0.0228(10) Uani 1 2 d S . . C2 C 0.4184(2) 0.2500 0.4295(4) 0.0263(10) Uani 1 2 d S . . C3 C 0.4436(3) 0.2500 0.3423(4) 0.0335(12) Uani 1 2 d S . . H3 H 0.4146 0.2500 0.2926 0.040 Uiso 1 2 calc SR . . C4 C 0.5108(3) 0.2500 0.3308(5) 0.0491(17) Uani 1 2 d S . . H4 H 0.5284 0.2500 0.2722 0.059 Uiso 1 2 calc SR . . C5 C 0.5541(3) 0.2500 0.4037(5) 0.0528(18) Uani 1 2 d S . . H5 H 0.6005 0.2500 0.3939 0.063 Uiso 1 2 calc SR . . C6 C 0.5300(3) 0.2500 0.4894(5) 0.0471(16) Uani 1 2 d S . . H6 H 0.5593 0.2500 0.5388 0.057 Uiso 1 2 calc SR . . C7 C 0.4618(3) 0.2500 0.5024(4) 0.0358(13) Uani 1 2 d S . . C8 C 0.4313(3) 0.2500 0.5884(4) 0.0395(14) Uani 1 2 d S . . C9 C 0.2575(3) 0.2500 0.5522(4) 0.0398(14) Uani 1 2 d S . . H9A H 0.2371 0.3036 0.5245 0.048 Uiso 0.50 1 calc PR . . H9B H 0.2371 0.1964 0.5245 0.048 Uiso 0.50 1 calc PR . . C10 C 0.2411(4) 0.2500 0.6437(5) 0.083(3) Uani 1 2 d S . . H10A H 0.2769 0.2217 0.6776 0.125 Uiso 0.50 1 calc PR . . H10B H 0.2000 0.2162 0.6527 0.125 Uiso 0.50 1 calc PR . . H10C H 0.2350 0.3121 0.6640 0.125 Uiso 0.50 1 calc PR . . C11 C 0.33774(17) 0.4525(2) 0.2580(2) 0.0239(7) Uani 1 1 d . . . C12 C 0.35102(18) 0.4007(3) 0.1824(2) 0.0271(7) Uani 1 1 d . . . H12 H 0.3355 0.3405 0.1794 0.033 Uiso 1 1 calc R . . C13 C 0.3866(2) 0.4362(3) 0.1119(3) 0.0343(9) Uani 1 1 d . . . H13 H 0.3960 0.4001 0.0613 0.041 Uiso 1 1 calc R . . C14 C 0.4083(2) 0.5243(3) 0.1152(3) 0.0383(10) Uani 1 1 d . . . H14 H 0.4315 0.5493 0.0662 0.046 Uiso 1 1 calc R . . C15 C 0.3962(2) 0.5761(3) 0.1902(3) 0.0381(9) Uani 1 1 d . . . H15 H 0.4117 0.6364 0.1924 0.046 Uiso 1 1 calc R . . C16 C 0.3619(2) 0.5410(3) 0.2614(3) 0.0315(8) Uani 1 1 d . . . H16 H 0.3546 0.5768 0.3129 0.038 Uiso 1 1 calc R . . C17 C 0.20523(17) 0.4587(2) 0.3375(2) 0.0245(7) Uani 1 1 d . . . C18 C 0.1993(2) 0.5488(3) 0.3120(3) 0.0339(9) Uani 1 1 d . . . H18 H 0.2374 0.5814 0.2937 0.041 Uiso 1 1 calc R . . C19 C 0.1383(2) 0.5909(3) 0.3131(3) 0.0453(11) Uani 1 1 d . . . H19 H 0.1345 0.6520 0.2956 0.054 Uiso 1 1 calc R . . C20 C 0.0831(2) 0.5439(3) 0.3397(3) 0.0446(11) Uani 1 1 d . . . H20 H 0.0413 0.5731 0.3414 0.054 Uiso 1 1 calc R . . C21 C 0.0881(2) 0.4537(3) 0.3643(3) 0.0385(10) Uani 1 1 d . . . H21 H 0.0497 0.4213 0.3817 0.046 Uiso 1 1 calc R . . C22 C 0.14933(19) 0.4114(3) 0.3633(2) 0.0308(8) Uani 1 1 d . . . H22 H 0.1529 0.3501 0.3802 0.037 Uiso 1 1 calc R . . C23 C 0.31962(17) 0.4593(2) 0.4474(2) 0.0228(7) Uani 1 1 d . . . C24 C 0.2774(2) 0.4917(3) 0.5130(3) 0.0362(9) Uani 1 1 d . . . H24 H 0.2309 0.4902 0.5039 0.043 Uiso 1 1 calc R . . C25 C 0.3025(2) 0.5261(4) 0.5915(3) 0.0468(12) Uani 1 1 d . . . H25 H 0.2730 0.5481 0.6356 0.056 Uiso 1 1 calc R . . C26 C 0.3695(2) 0.5289(3) 0.6067(3) 0.0396(10) Uani 1 1 d . . . H26 H 0.3863 0.5524 0.6609 0.048 Uiso 1 1 calc R . . C27 C 0.4120(2) 0.4973(3) 0.5425(3) 0.0374(9) Uani 1 1 d . . . H27 H 0.4583 0.4988 0.5527 0.045 Uiso 1 1 calc R . . C28 C 0.38766(19) 0.4631(3) 0.4626(3) 0.0322(8) Uani 1 1 d . . . H28 H 0.4175 0.4422 0.4184 0.039 Uiso 1 1 calc R . . B1 B 0.5256(4) 0.2500 0.9689(5) 0.0404(16) Uani 1 2 d S . . F1 F 0.5167(3) 0.2500 0.8742(3) 0.0667(13) Uani 1 2 d S . . F2 F 0.49668(16) 0.17299(19) 0.9967(2) 0.0592(8) Uani 1 1 d . . . F3 F 0.5927(2) 0.2500 0.9834(3) 0.0578(11) Uani 1 2 d S . . C31 C 0.2326(6) 0.2500 0.9923(6) 0.089(3) Uani 1 2 d S . . H31A H 0.2186 0.3037 1.0263 0.107 Uiso 0.50 1 calc PR . . H31B H 0.2186 0.1963 1.0263 0.107 Uiso 0.50 1 calc PR . . Cl3 Cl 0.19227(9) 0.2500 0.89012(13) 0.0532(4) Uani 1 2 d S . . Cl4 Cl 0.31749(12) 0.2500 0.98440(13) 0.0695(6) Uani 1 2 d S . . 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 0.01893(18) 0.02143(19) 0.01900(18) 0.000 -0.00241(14) 0.000 Cl1 0.0447(9) 0.0805(13) 0.0429(9) 0.000 -0.0180(7) 0.000 Cl2 0.0286(6) 0.0308(6) 0.0221(5) 0.000 -0.0076(5) 0.000 N1 0.025(2) 0.037(2) 0.020(2) 0.000 -0.0029(17) 0.000 N2 0.035(3) 0.052(3) 0.026(2) 0.000 -0.008(2) 0.000 P1 0.0202(4) 0.0226(4) 0.0205(4) -0.0018(3) 0.0011(3) 0.0004(3) C1 0.025(2) 0.020(2) 0.024(2) 0.000 -0.001(2) 0.000 C2 0.019(2) 0.029(3) 0.031(3) 0.000 -0.004(2) 0.000 C3 0.029(3) 0.040(3) 0.032(3) 0.000 0.003(2) 0.000 C4 0.029(3) 0.069(5) 0.049(4) 0.000 0.010(3) 0.000 C5 0.027(3) 0.062(4) 0.069(5) 0.000 0.010(3) 0.000 C6 0.032(3) 0.058(4) 0.051(4) 0.000 -0.006(3) 0.000 C7 0.023(3) 0.041(3) 0.043(3) 0.000 -0.005(2) 0.000 C8 0.036(3) 0.047(3) 0.036(3) 0.000 -0.015(3) 0.000 C9 0.032(3) 0.064(4) 0.023(3) 0.000 0.003(2) 0.000 C10 0.043(4) 0.180(11) 0.027(3) 0.000 0.005(3) 0.000 C11 0.0216(17) 0.0287(17) 0.0214(16) -0.0015(14) 0.0009(13) 0.0022(14) C12 0.0251(18) 0.0304(18) 0.0258(17) -0.0026(14) 0.0015(14) 0.0016(15) C13 0.0297(19) 0.050(2) 0.0232(18) -0.0038(17) 0.0051(15) 0.0000(18) C14 0.028(2) 0.057(3) 0.031(2) 0.0099(19) 0.0045(16) -0.0089(18) C15 0.032(2) 0.038(2) 0.045(2) 0.0051(19) 0.0047(18) -0.0097(18) C16 0.033(2) 0.0293(18) 0.033(2) -0.0032(15) 0.0049(16) -0.0052(16) C17 0.0239(17) 0.0285(17) 0.0212(16) -0.0036(14) -0.0013(13) 0.0006(14) C18 0.0279(19) 0.0259(18) 0.048(2) -0.0021(17) -0.0037(17) 0.0034(15) C19 0.036(2) 0.034(2) 0.066(3) -0.005(2) -0.005(2) 0.0115(19) C20 0.031(2) 0.056(3) 0.047(3) -0.009(2) -0.0014(19) 0.018(2) C21 0.0253(19) 0.061(3) 0.029(2) 0.0011(19) 0.0022(15) 0.0005(19) C22 0.0274(19) 0.040(2) 0.0246(18) 0.0038(15) 0.0013(15) 0.0004(16) C23 0.0238(17) 0.0253(17) 0.0194(15) -0.0008(13) 0.0020(13) -0.0011(14) C24 0.0276(19) 0.056(3) 0.0250(18) -0.0058(18) 0.0038(15) 0.0017(18) C25 0.037(2) 0.078(3) 0.0253(19) -0.018(2) 0.0039(17) 0.004(2) C26 0.041(2) 0.053(3) 0.0243(19) -0.0100(18) -0.0001(17) -0.007(2) C27 0.029(2) 0.051(2) 0.033(2) -0.0100(19) -0.0051(16) -0.0082(18) C28 0.0246(18) 0.044(2) 0.0280(19) -0.0116(17) 0.0008(15) -0.0020(16) B1 0.039(4) 0.025(3) 0.057(4) 0.000 0.010(3) 0.000 F1 0.100(4) 0.058(3) 0.042(2) 0.000 0.004(2) 0.000 F2 0.0597(18) 0.0444(15) 0.0734(19) 0.0143(14) 0.0096(15) -0.0114(14) F3 0.039(2) 0.055(2) 0.079(3) 0.000 0.002(2) 0.000 C31 0.121(9) 0.110(8) 0.037(4) 0.000 0.000(5) 0.000 Cl3 0.0547(10) 0.0466(9) 0.0582(11) 0.000 0.0012(8) 0.000 Cl4 0.0768(14) 0.0892(15) 0.0424(10) 0.000 -0.0114(9) 0.000 _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; 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 Pd1 C1 1.989(5) . ? Pd1 P1 2.3438(8) 7_565 ? Pd1 P1 2.3439(8) . ? Pd1 Cl2 2.3513(12) . ? Cl1 C8 1.732(6) . ? N1 C1 1.340(6) . ? N1 N2 1.377(6) . ? N1 C9 1.473(7) . ? N2 C8 1.278(8) . ? P1 C11 1.812(4) . ? P1 C17 1.821(4) . ? P1 C23 1.823(4) . ? C1 C2 1.423(7) . ? C2 C7 1.404(8) . ? C2 C3 1.406(8) . ? C3 C4 1.369(8) . ? C4 C5 1.404(10) . ? C5 C6 1.378(10) . ? C6 C7 1.391(8) . ? C7 C8 1.434(9) . ? C9 C10 1.415(9) . ? C11 C12 1.399(5) . ? C11 C16 1.404(5) . ? C12 C13 1.386(5) . ? C13 C14 1.382(6) . ? C14 C15 1.387(6) . ? C15 C16 1.379(6) . ? C17 C22 1.387(5) . ? C17 C18 1.399(5) . ? C18 C19 1.382(6) . ? C19 C20 1.376(7) . ? C20 C21 1.395(7) . ? C21 C22 1.389(6) . ? C23 C24 1.391(5) . ? C23 C28 1.396(5) . ? C24 C25 1.382(6) . ? C25 C26 1.376(6) . ? C26 C27 1.373(6) . ? C27 C28 1.395(5) . ? B1 F2 1.352(5) . ? B1 F2 1.352(5) 7_565 ? B1 F3 1.374(8) . ? B1 F1 1.436(9) . ? C31 Cl4 1.721(12) . ? C31 Cl3 1.739(9) . ? 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 C1 Pd1 P1 88.89(2) . 7_565 ? C1 Pd1 P1 88.89(2) . . ? P1 Pd1 P1 177.46(5) 7_565 . ? C1 Pd1 Cl2 176.94(15) . . ? P1 Pd1 Cl2 91.08(2) 7_565 . ? P1 Pd1 Cl2 91.08(2) . . ? C1 N1 N2 125.4(5) . . ? C1 N1 C9 121.0(4) . . ? N2 N1 C9 113.6(4) . . ? C8 N2 N1 116.3(5) . . ? C11 P1 C17 107.74(16) . . ? C11 P1 C23 104.41(16) . . ? C17 P1 C23 102.52(16) . . ? C11 P1 Pd1 112.01(12) . . ? C17 P1 Pd1 113.45(12) . . ? C23 P1 Pd1 115.80(12) . . ? N1 C1 C2 117.6(5) . . ? N1 C1 Pd1 121.0(4) . . ? C2 C1 Pd1 121.4(4) . . ? C7 C2 C3 120.0(5) . . ? C7 C2 C1 119.1(5) . . ? C3 C2 C1 120.9(5) . . ? C4 C3 C2 118.5(6) . . ? C3 C4 C5 121.4(6) . . ? C6 C5 C4 120.6(6) . . ? C5 C6 C7 118.8(6) . . ? C6 C7 C2 120.7(6) . . ? C6 C7 C8 123.5(6) . . ? C2 C7 C8 115.8(5) . . ? N2 C8 C7 125.8(5) . . ? N2 C8 Cl1 113.6(5) . . ? C7 C8 Cl1 120.6(5) . . ? C10 C9 N1 116.6(6) . . ? C12 C11 C16 118.6(3) . . ? C12 C11 P1 120.2(3) . . ? C16 C11 P1 121.1(3) . . ? C13 C12 C11 120.8(4) . . ? C14 C13 C12 119.9(4) . . ? C13 C14 C15 120.0(4) . . ? C16 C15 C14 120.6(4) . . ? C15 C16 C11 120.1(4) . . ? C22 C17 C18 119.5(3) . . ? C22 C17 P1 120.3(3) . . ? C18 C17 P1 119.9(3) . . ? C19 C18 C17 120.4(4) . . ? C20 C19 C18 119.9(4) . . ? C19 C20 C21 120.4(4) . . ? C22 C21 C20 119.8(4) . . ? C17 C22 C21 120.0(4) . . ? C24 C23 C28 118.3(3) . . ? C24 C23 P1 120.8(3) . . ? C28 C23 P1 120.8(3) . . ? C25 C24 C23 120.6(4) . . ? C26 C25 C24 120.9(4) . . ? C27 C26 C25 119.3(4) . . ? C26 C27 C28 120.7(4) . . ? C27 C28 C23 120.2(4) . . ? F2 B1 F2 115.8(6) . 7_565 ? F2 B1 F3 112.2(4) . . ? F2 B1 F3 112.2(4) 7_565 . ? F2 B1 F1 104.6(4) . . ? F2 B1 F1 104.6(4) 7_565 . ? F3 B1 F1 106.4(6) . . ? Cl4 C31 Cl3 114.0(5) . . ? _diffrn_measured_fraction_theta_max 0.996 _diffrn_reflns_theta_full 26.77 _diffrn_measured_fraction_theta_full 0.996 _refine_diff_density_max 1.340 _refine_diff_density_min -1.182 _refine_diff_density_rms 0.093 #============================================================================== data_3-togu13 _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety 'C24 H22 Cl3 N2 P Pd' _chemical_formula_sum 'C24 H22 Cl3 N2 P Pd' _chemical_formula_weight 582.16 loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source 'C' 'C' 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'H' 'H' 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'N' 'N' 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'P' 'P' 0.1023 0.0942 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'Cl' 'Cl' 0.1484 0.1585 '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' _symmetry_cell_setting Triclinic _symmetry_space_group_name_H-M 'P -1' loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, -y, -z' _cell_length_a 9.6593(9) _cell_length_b 10.9025(10) _cell_length_c 13.1195(12) _cell_angle_alpha 114.633(6) _cell_angle_beta 106.394(7) _cell_angle_gamma 89.521(7) _cell_volume 1195.33(19) _cell_formula_units_Z 2 _cell_measurement_temperature 133(2) _cell_measurement_reflns_used 11278 _cell_measurement_theta_min 1.79 _cell_measurement_theta_max 27.15 _exptl_crystal_description block _exptl_crystal_colour yellow _exptl_crystal_size_max 0.4 _exptl_crystal_size_mid 0.25 _exptl_crystal_size_min 0.19 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.617 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 584 _exptl_absorpt_coefficient_mu 1.193 _exptl_absorpt_correction_type numerical _exptl_absorpt_correction_T_min 0.6456 _exptl_absorpt_correction_T_max 0.7913 _exptl_absorpt_process_details 'X-RED (Stoe & Cie, 2002)' _exptl_special_details ; ? ; _diffrn_ambient_temperature 133(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'Stoe IPDS II' _diffrn_measurement_method \w _diffrn_detector_area_resol_mean ? _diffrn_reflns_number 11278 _diffrn_reflns_av_R_equivalents 0.0277 _diffrn_reflns_av_sigmaI/netI 0.0237 _diffrn_reflns_limit_h_min -12 _diffrn_reflns_limit_h_max 10 _diffrn_reflns_limit_k_min -13 _diffrn_reflns_limit_k_max 13 _diffrn_reflns_limit_l_min -16 _diffrn_reflns_limit_l_max 16 _diffrn_reflns_theta_min 1.79 _diffrn_reflns_theta_max 27.15 _reflns_number_total 5116 _reflns_number_gt 4681 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'X-AREA (Stoe & Cie, 2002)' _computing_cell_refinement 'X-AREA (Stoe & Cie, 2002)' _computing_data_reduction 'X-AREA (Stoe & Cie, 2002)' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'DIAMOND (Brandenburg, 2001)' _computing_publication_material 'SHELXL-97 (Sheldrick, 1997)' _refine_special_details ; Refinement of F^2^ against ALL reflections. The weighted R-factor wR and goodness of fit S are based on F^2^, conventional R-factors R are based on F, with F set to zero for negative F^2^. The threshold expression of F^2^ > 2sigma(F^2^) is used only for calculating R-factors(gt) etc. and is not relevant to the choice of reflections for refinement. R-factors based on F^2^ are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger. ; _refine_ls_structure_factor_coef Fsqd _refine_ls_matrix_type full _refine_ls_weighting_scheme calc _refine_ls_weighting_details 'calc w=1/[\s^2^(Fo^2^)+(0.0289P)^2^+0.5507P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment constr _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 5116 _refine_ls_number_parameters 281 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0259 _refine_ls_R_factor_gt 0.0217 _refine_ls_wR_factor_ref 0.0548 _refine_ls_wR_factor_gt 0.0535 _refine_ls_goodness_of_fit_ref 1.031 _refine_ls_restrained_S_all 1.031 _refine_ls_shift/su_max 0.000 _refine_ls_shift/su_mean 0.000 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_symmetry_multiplicity _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group Pd1 Pd 0.209398(13) 0.150328(13) 0.176180(10) 0.01618(5) Uani 1 1 d . . . Cl1 Cl 0.29371(5) 0.14684(5) 0.02214(4) 0.02726(10) Uani 1 1 d . . . Cl2 Cl 0.17144(5) 0.38005(4) 0.23379(4) 0.02306(9) Uani 1 1 d . . . Cl3 Cl 0.29703(8) -0.47904(6) 0.01355(5) 0.05253(18) Uani 1 1 d . . . P1 P 0.13447(5) 0.15505(4) 0.32614(4) 0.01629(9) Uani 1 1 d . . . N1 N 0.36198(17) -0.08972(16) 0.14157(13) 0.0217(3) Uani 1 1 d . . . N2 N 0.38435(19) -0.22176(17) 0.10897(14) 0.0280(3) Uani 1 1 d . . . C1 C 0.23254(19) -0.04466(18) 0.12557(14) 0.0190(3) Uani 1 1 d . . . C2 C 0.1093(2) -0.14761(19) 0.06331(15) 0.0225(4) Uani 1 1 d . . . H2 H 0.0163 -0.1220 0.0489 0.027 Uiso 1 1 calc R . . C3 C 0.1254(2) -0.2817(2) 0.02492(16) 0.0284(4) Uani 1 1 d . . . H3 H 0.0462 -0.3492 -0.0177 0.034 Uiso 1 1 calc R . . C4 C 0.2671(2) -0.3121(2) 0.05294(16) 0.0307(4) Uani 1 1 d . . . C5 C 0.50224(19) 0.0035(2) 0.19889(17) 0.0267(4) Uani 1 1 d . . . H5A H 0.4837 0.0919 0.2009 0.032 Uiso 1 1 calc R . . H5B H 0.5678 -0.0326 0.1525 0.032 Uiso 1 1 calc R . . C6 C 0.5737(2) 0.0196(2) 0.32283(17) 0.0312(4) Uani 1 1 d . . . H6A H 0.5125 0.0623 0.3706 0.047 Uiso 1 1 calc R . . H6B H 0.6660 0.0751 0.3551 0.047 Uiso 1 1 calc R . . H6C H 0.5881 -0.0682 0.3215 0.047 Uiso 1 1 calc R . . C7 C 0.09253(19) -0.01074(17) 0.32157(14) 0.0184(3) Uani 1 1 d . . . C8 C -0.0479(2) -0.08291(18) 0.26090(16) 0.0226(4) Uani 1 1 d . . . H8 H -0.1235 -0.0400 0.2339 0.027 Uiso 1 1 calc R . . C9 C -0.0754(2) -0.2175(2) 0.24065(17) 0.0290(4) Uani 1 1 d . . . H9 H -0.1687 -0.2640 0.1997 0.035 Uiso 1 1 calc R . . C10 C 0.0348(3) -0.2818(2) 0.28097(19) 0.0325(4) Uani 1 1 d . . . H10 H 0.0172 -0.3720 0.2669 0.039 Uiso 1 1 calc R . . C11 C 0.1739(2) -0.2100(2) 0.34334(19) 0.0333(4) Uani 1 1 d . . . H11 H 0.2483 -0.2526 0.3724 0.040 Uiso 1 1 calc R . . C12 C 0.2032(2) -0.0760(2) 0.36289(16) 0.0258(4) Uani 1 1 d . . . H12 H 0.2968 -0.0302 0.4036 0.031 Uiso 1 1 calc R . . C13 C -0.03106(18) 0.23215(17) 0.33082(16) 0.0192(3) Uani 1 1 d . . . C14 C -0.0539(2) 0.32118(19) 0.43554(17) 0.0267(4) Uani 1 1 d . . . H14 H 0.0176 0.3433 0.5071 0.032 Uiso 1 1 calc R . . C15 C -0.1833(2) 0.3767(2) 0.4328(2) 0.0351(5) Uani 1 1 d . . . H15 H -0.1985 0.4370 0.5027 0.042 Uiso 1 1 calc R . . C16 C -0.2900(2) 0.3427(2) 0.3267(2) 0.0374(5) Uani 1 1 d . . . H16 H -0.3772 0.3796 0.3255 0.045 Uiso 1 1 calc R . . C17 C -0.2680(2) 0.2540(2) 0.2218(2) 0.0330(4) Uani 1 1 d . . . H17 H -0.3402 0.2314 0.1505 0.040 Uiso 1 1 calc R . . C18 C -0.1383(2) 0.1993(2) 0.22400(17) 0.0252(4) Uani 1 1 d . . . H18 H -0.1227 0.1405 0.1539 0.030 Uiso 1 1 calc R . . C19 C 0.27519(19) 0.24785(17) 0.46591(14) 0.0194(3) Uani 1 1 d . . . C20 C 0.39824(19) 0.31785(17) 0.46802(15) 0.0194(3) Uani 1 1 d . . . H20 H 0.4056 0.3174 0.3987 0.023 Uiso 1 1 calc R . . C21 C 0.5092(2) 0.38792(18) 0.57347(16) 0.0228(4) Uani 1 1 d . . . H21 H 0.5910 0.4332 0.5743 0.027 Uiso 1 1 calc R . . C22 C 0.4976(2) 0.39005(19) 0.67688(16) 0.0258(4) Uani 1 1 d . . . H22 H 0.5710 0.4378 0.7475 0.031 Uiso 1 1 calc R . . C23 C 0.3756(2) 0.3204(2) 0.67537(16) 0.0283(4) Uani 1 1 d . . . H23 H 0.3684 0.3222 0.7452 0.034 Uiso 1 1 calc R . . C24 C 0.2649(2) 0.2484(2) 0.57045(16) 0.0255(4) Uani 1 1 d . . . H24 H 0.1847 0.2011 0.5698 0.031 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 0.01504(7) 0.01834(7) 0.01481(7) 0.00648(5) 0.00513(5) 0.00167(5) Cl1 0.0262(2) 0.0387(3) 0.0218(2) 0.01491(18) 0.01157(17) 0.00473(19) Cl2 0.0246(2) 0.0193(2) 0.0234(2) 0.00919(16) 0.00459(16) 0.00114(16) Cl3 0.0770(5) 0.0237(3) 0.0324(3) 0.0015(2) -0.0021(3) 0.0178(3) P1 0.0160(2) 0.0165(2) 0.01589(19) 0.00597(16) 0.00586(15) 0.00215(16) N1 0.0221(7) 0.0250(8) 0.0178(7) 0.0075(6) 0.0087(6) 0.0062(6) N2 0.0338(9) 0.0263(8) 0.0204(7) 0.0063(6) 0.0093(7) 0.0134(7) C1 0.0204(8) 0.0227(8) 0.0146(7) 0.0074(6) 0.0073(6) 0.0046(7) C2 0.0222(8) 0.0253(9) 0.0173(8) 0.0075(7) 0.0045(7) 0.0012(7) C3 0.0353(10) 0.0247(9) 0.0174(8) 0.0057(7) 0.0017(7) -0.0019(8) C4 0.0457(12) 0.0222(9) 0.0176(8) 0.0047(7) 0.0065(8) 0.0107(8) C5 0.0158(8) 0.0349(10) 0.0295(9) 0.0134(8) 0.0079(7) 0.0044(7) C6 0.0284(10) 0.0293(10) 0.0295(10) 0.0114(8) 0.0015(8) 0.0023(8) C7 0.0223(8) 0.0175(8) 0.0168(7) 0.0062(6) 0.0097(6) 0.0031(6) C8 0.0230(9) 0.0222(9) 0.0235(8) 0.0092(7) 0.0094(7) 0.0030(7) C9 0.0330(10) 0.0238(9) 0.0297(9) 0.0078(8) 0.0143(8) -0.0025(8) C10 0.0492(13) 0.0196(9) 0.0367(10) 0.0131(8) 0.0233(9) 0.0059(8) C11 0.0386(11) 0.0329(11) 0.0393(11) 0.0222(9) 0.0177(9) 0.0163(9) C12 0.0242(9) 0.0283(9) 0.0267(9) 0.0127(8) 0.0093(7) 0.0059(7) C13 0.0181(8) 0.0168(8) 0.0252(8) 0.0089(7) 0.0106(7) 0.0035(6) C14 0.0271(9) 0.0207(8) 0.0294(9) 0.0045(7) 0.0142(8) 0.0000(7) C15 0.0347(11) 0.0221(9) 0.0505(13) 0.0079(9) 0.0279(10) 0.0071(8) C16 0.0296(11) 0.0318(11) 0.0680(15) 0.0293(11) 0.0282(11) 0.0165(9) C17 0.0229(9) 0.0422(12) 0.0471(12) 0.0307(10) 0.0121(8) 0.0092(8) C18 0.0228(9) 0.0298(10) 0.0296(9) 0.0172(8) 0.0108(7) 0.0073(7) C19 0.0199(8) 0.0181(8) 0.0181(8) 0.0064(6) 0.0051(6) 0.0038(6) C20 0.0201(8) 0.0188(8) 0.0201(8) 0.0087(6) 0.0068(6) 0.0051(6) C21 0.0187(8) 0.0216(8) 0.0273(9) 0.0113(7) 0.0047(7) 0.0030(7) C22 0.0251(9) 0.0231(9) 0.0217(8) 0.0072(7) 0.0003(7) 0.0047(7) C23 0.0339(10) 0.0305(10) 0.0193(8) 0.0104(7) 0.0068(7) 0.0025(8) C24 0.0267(9) 0.0284(9) 0.0214(8) 0.0103(7) 0.0078(7) -0.0003(7) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; 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 Pd1 C1 1.9772(18) . ? Pd1 P1 2.2618(5) . ? Pd1 Cl2 2.3540(5) . ? Pd1 Cl1 2.3693(5) . ? Cl3 C4 1.719(2) . ? P1 C13 1.8046(18) . ? P1 C19 1.8175(17) . ? P1 C7 1.8284(18) . ? N1 C1 1.333(2) . ? N1 N2 1.355(2) . ? N1 C5 1.498(2) . ? N2 C4 1.318(3) . ? C1 C2 1.433(2) . ? C2 C3 1.357(3) . ? C3 C4 1.389(3) . ? C5 C6 1.510(3) . ? C7 C12 1.387(3) . ? C7 C8 1.407(2) . ? C8 C9 1.391(3) . ? C9 C10 1.372(3) . ? C10 C11 1.396(3) . ? C11 C12 1.391(3) . ? C13 C18 1.391(3) . ? C13 C14 1.391(2) . ? C14 C15 1.382(3) . ? C15 C16 1.380(4) . ? C16 C17 1.388(3) . ? C17 C18 1.381(3) . ? C19 C24 1.400(3) . ? C19 C20 1.405(2) . ? C20 C21 1.394(2) . ? C21 C22 1.383(3) . ? C22 C23 1.398(3) . ? C23 C24 1.392(3) . ? 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 C1 Pd1 P1 90.86(5) . . ? C1 Pd1 Cl2 177.65(5) . . ? P1 Pd1 Cl2 88.342(17) . . ? C1 Pd1 Cl1 89.15(5) . . ? P1 Pd1 Cl1 178.626(16) . . ? Cl2 Pd1 Cl1 91.700(18) . . ? C13 P1 C19 109.20(8) . . ? C13 P1 C7 104.15(8) . . ? C19 P1 C7 105.25(8) . . ? C13 P1 Pd1 111.95(6) . . ? C19 P1 Pd1 110.23(6) . . ? C7 P1 Pd1 115.63(6) . . ? C1 N1 N2 125.49(16) . . ? C1 N1 C5 122.64(16) . . ? N2 N1 C5 111.87(15) . . ? C4 N2 N1 116.28(17) . . ? N1 C1 C2 115.61(16) . . ? N1 C1 Pd1 122.93(13) . . ? C2 C1 Pd1 121.39(13) . . ? C3 C2 C1 121.41(18) . . ? C2 C3 C4 116.06(18) . . ? N2 C4 C3 125.05(18) . . ? N2 C4 Cl3 115.77(16) . . ? C3 C4 Cl3 119.18(16) . . ? N1 C5 C6 111.59(16) . . ? C12 C7 C8 118.50(17) . . ? C12 C7 P1 120.24(14) . . ? C8 C7 P1 120.60(14) . . ? C9 C8 C7 121.05(18) . . ? C10 C9 C8 120.14(19) . . ? C9 C10 C11 119.16(19) . . ? C12 C11 C10 121.27(19) . . ? C7 C12 C11 119.86(18) . . ? C18 C13 C14 119.94(17) . . ? C18 C13 P1 117.35(14) . . ? C14 C13 P1 122.71(14) . . ? C15 C14 C13 119.75(19) . . ? C16 C15 C14 120.1(2) . . ? C15 C16 C17 120.53(19) . . ? C18 C17 C16 119.6(2) . . ? C17 C18 C13 120.11(19) . . ? C24 C19 C20 119.59(16) . . ? C24 C19 P1 121.44(14) . . ? C20 C19 P1 118.96(13) . . ? C21 C20 C19 120.31(16) . . ? C22 C21 C20 119.94(17) . . ? C21 C22 C23 120.04(17) . . ? C24 C23 C22 120.65(18) . . ? C23 C24 C19 119.46(18) . . ? _diffrn_measured_fraction_theta_max 0.966 _diffrn_reflns_theta_full 27.15 _diffrn_measured_fraction_theta_full 0.966 _refine_diff_density_max 0.526 _refine_diff_density_min -0.372 _refine_diff_density_rms 0.056 #============================================================================== data_4-togu22 _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety 'C47 H44 Cl N4 P2 Pd +, B F4 -, C H2 Cl2' _chemical_formula_sum 'C48 H46 B Cl3 F4 N4 P2 Pd' _chemical_formula_weight 1040.39 loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source 'C' 'C' 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'H' 'H' 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'N' 'N' 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' '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' 'P' 'P' 0.1023 0.0942 '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' 'Pd' 'Pd' -0.9988 1.0072 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting Monoclinic _symmetry_space_group_name_H-M 'P 21/c' loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, y+1/2, -z+1/2' '-x, -y, -z' 'x, -y-1/2, z-1/2' _cell_length_a 14.2960(5) _cell_length_b 10.4914(2) _cell_length_c 32.2000(12) _cell_angle_alpha 90.00 _cell_angle_beta 97.243(3) _cell_angle_gamma 90.00 _cell_volume 4791.0(3) _cell_formula_units_Z 4 _cell_measurement_temperature 133(2) _cell_measurement_reflns_used 45238 _cell_measurement_theta_min 1.27 _cell_measurement_theta_max 25.69 _exptl_crystal_description block _exptl_crystal_colour colorless _exptl_crystal_size_max 0.5 _exptl_crystal_size_mid 0.13 _exptl_crystal_size_min 0.05 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.442 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 2120 _exptl_absorpt_coefficient_mu 0.675 _exptl_absorpt_correction_type numerical _exptl_absorpt_correction_T_min 0.8053 _exptl_absorpt_correction_T_max 0.9608 _exptl_absorpt_process_details 'X-RED (Stoe & Cie, 2002)' _exptl_special_details ; ? ; _diffrn_ambient_temperature 133(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'Stoe IPDS II' _diffrn_measurement_method \w _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 45238 _diffrn_reflns_av_R_equivalents 0.0929 _diffrn_reflns_av_sigmaI/netI 0.0537 _diffrn_reflns_limit_h_min -17 _diffrn_reflns_limit_h_max 17 _diffrn_reflns_limit_k_min -10 _diffrn_reflns_limit_k_max 12 _diffrn_reflns_limit_l_min -39 _diffrn_reflns_limit_l_max 39 _diffrn_reflns_theta_min 1.27 _diffrn_reflns_theta_max 25.69 _reflns_number_total 9032 _reflns_number_gt 7334 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'X-AREA (Stoe & Cie, 2002)' _computing_cell_refinement 'X-AREA (Stoe & Cie, 2002)' _computing_data_reduction 'X-AREA (Stoe & Cie, 2002)' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'DIAMOND (Brandenburg, 2001)' _computing_publication_material 'SHELXL-97 (Sheldrick, 1997)' _refine_special_details ; Refinement of F^2^ against ALL reflections. The weighted R-factor wR and goodness of fit S are based on F^2^, conventional R-factors R are based on F, with F set to zero for negative F^2^. The threshold expression of F^2^ > 2sigma(F^2^) is used only for calculating R-factors(gt) etc. and is not relevant to the choice of reflections for refinement. R-factors based on F^2^ are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger. ; _refine_ls_structure_factor_coef Fsqd _refine_ls_matrix_type full _refine_ls_weighting_scheme calc _refine_ls_weighting_details 'calc w=1/[\s^2^(Fo^2^)+(0.0819P)^2^+3.6783P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment constr _refine_ls_extinction_method SHELXL _refine_ls_extinction_coef 0.0019(3) _refine_ls_extinction_expression 'Fc^*^=kFc[1+0.001xFc^2^\l^3^/sin(2\q)]^-1/4^' _refine_ls_number_reflns 9032 _refine_ls_number_parameters 598 _refine_ls_number_restraints 70 _refine_ls_R_factor_all 0.0669 _refine_ls_R_factor_gt 0.0528 _refine_ls_wR_factor_ref 0.1437 _refine_ls_wR_factor_gt 0.1352 _refine_ls_goodness_of_fit_ref 1.047 _refine_ls_restrained_S_all 1.059 _refine_ls_shift/su_max 0.002 _refine_ls_shift/su_mean 0.000 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_symmetry_multiplicity _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group Pd1 Pd 0.163763(19) 0.31651(3) 0.658820(8) 0.02671(11) Uani 1 1 d . . . Cl1 Cl 0.01630(7) 0.25185(10) 0.67601(3) 0.0368(2) Uani 1 1 d . . . P1 P 0.09021(7) 0.38621(9) 0.59446(3) 0.0273(2) Uani 1 1 d . . . P2 P 0.24224(7) 0.23630(10) 0.72167(3) 0.0298(2) Uani 1 1 d . . . N1 N 0.3204(2) 0.4914(3) 0.64917(9) 0.0314(7) Uani 1 1 d . . . N2 N 0.4050(2) 0.5335(3) 0.64044(10) 0.0343(7) Uani 1 1 d . . . N3 N 0.5445(2) 0.4970(4) 0.61410(10) 0.0392(8) Uani 1 1 d . . . N4 N 0.6124(3) 0.4070(4) 0.60976(11) 0.0445(9) Uani 1 1 d . . . C1 C 0.2865(3) 0.3734(4) 0.64283(10) 0.0306(8) Uani 1 1 d . . . C2 C 0.3452(3) 0.2869(4) 0.62336(11) 0.0321(8) Uani 1 1 d . . . H2 H 0.3248 0.2019 0.6176 0.039 Uiso 1 1 calc R . . C3 C 0.4291(3) 0.3257(4) 0.61314(11) 0.0348(9) Uani 1 1 d . . . H3 H 0.4683 0.2698 0.5998 0.042 Uiso 1 1 calc R . . C4 C 0.4567(3) 0.4517(4) 0.62298(11) 0.0331(9) Uani 1 1 d . . . C5 C 0.5755(3) 0.6214(5) 0.60997(13) 0.0450(11) Uani 1 1 d . . . C6 C 0.6672(3) 0.6076(6) 0.60260(14) 0.0511(12) Uani 1 1 d . . . H6 H 0.7096 0.6745 0.5981 0.061 Uiso 1 1 calc R . . C7 C 0.6874(3) 0.4757(6) 0.60289(13) 0.0486(12) Uani 1 1 d . . . C8 C 0.5168(4) 0.7364(5) 0.61097(18) 0.0575(13) Uani 1 1 d . . . H8A H 0.5489 0.8089 0.5998 0.086 Uiso 1 1 calc R . . H8B H 0.5065 0.7544 0.6399 0.086 Uiso 1 1 calc R . . H8C H 0.4559 0.7224 0.5939 0.086 Uiso 1 1 calc R . . C9 C 0.7757(3) 0.4103(7) 0.59523(16) 0.0637(15) Uani 1 1 d . . . H9A H 0.7690 0.3183 0.5992 0.096 Uiso 1 1 calc R . . H9B H 0.8284 0.4423 0.6149 0.096 Uiso 1 1 calc R . . H9C H 0.7882 0.4270 0.5665 0.096 Uiso 1 1 calc R . . C10 C 0.2666(3) 0.5953(4) 0.66710(13) 0.0390(9) Uani 1 1 d . . . H10A H 0.2579 0.6668 0.6469 0.047 Uiso 1 1 calc R . . H10B H 0.2034 0.5631 0.6714 0.047 Uiso 1 1 calc R . . C11 C 0.3153(4) 0.6422(6) 0.70730(17) 0.0651(15) Uani 1 1 d . . . H11A H 0.3148 0.5756 0.7286 0.098 Uiso 1 1 calc R . . H11B H 0.2828 0.7180 0.7160 0.098 Uiso 1 1 calc R . . H11C H 0.3806 0.6640 0.7040 0.098 Uiso 1 1 calc R . . C21 C 0.1727(3) 0.4200(4) 0.55695(10) 0.0297(8) Uani 1 1 d . . . C22 C 0.2157(3) 0.5387(4) 0.55548(12) 0.0359(9) Uani 1 1 d . . . H22 H 0.1948 0.6083 0.5708 0.043 Uiso 1 1 calc R . . C23 C 0.2892(3) 0.5553(5) 0.53162(13) 0.0431(10) Uani 1 1 d . . . H23 H 0.3187 0.6363 0.5309 0.052 Uiso 1 1 calc R . . C24 C 0.3200(3) 0.4555(5) 0.50888(13) 0.0471(11) Uani 1 1 d . . . H24 H 0.3701 0.4675 0.4925 0.056 Uiso 1 1 calc R . . C25 C 0.2770(3) 0.3383(5) 0.51024(13) 0.0460(11) Uani 1 1 d . . . H25 H 0.2974 0.2694 0.4945 0.055 Uiso 1 1 calc R . . C26 C 0.2049(3) 0.3195(4) 0.53414(11) 0.0374(9) Uani 1 1 d . . . H26 H 0.1768 0.2377 0.5351 0.045 Uiso 1 1 calc R . . C27 C 0.0215(3) 0.5312(4) 0.59824(11) 0.0301(8) Uani 1 1 d . . . C28 C -0.0030(3) 0.5678(4) 0.63755(12) 0.0346(9) Uani 1 1 d . . . H28 H 0.0177 0.5187 0.6618 0.042 Uiso 1 1 calc R . . C29 C -0.0574(3) 0.6753(4) 0.64076(14) 0.0415(10) Uani 1 1 d . . . H29 H -0.0742 0.7000 0.6672 0.050 Uiso 1 1 calc R . . C30 C -0.0873(3) 0.7471(4) 0.60563(15) 0.0432(10) Uani 1 1 d . . . H30 H -0.1242 0.8214 0.6081 0.052 Uiso 1 1 calc R . . C31 C -0.0640(3) 0.7114(4) 0.56664(14) 0.0408(10) Uani 1 1 d . . . H31 H -0.0854 0.7605 0.5425 0.049 Uiso 1 1 calc R . . C32 C -0.0094(3) 0.6040(4) 0.56320(12) 0.0333(8) Uani 1 1 d . . . H32 H 0.0071 0.5799 0.5366 0.040 Uiso 1 1 calc R . . C33 C 0.0135(3) 0.2647(4) 0.56847(11) 0.0299(8) Uani 1 1 d . . . C34 C -0.0601(3) 0.2930(4) 0.53732(11) 0.0326(8) Uani 1 1 d . . . H34 H -0.0751 0.3794 0.5305 0.039 Uiso 1 1 calc R . . C35 C -0.1117(3) 0.1957(4) 0.51611(13) 0.0409(10) Uani 1 1 d . . . H35 H -0.1620 0.2153 0.4949 0.049 Uiso 1 1 calc R . . C36 C -0.0895(3) 0.0698(5) 0.52593(14) 0.0460(11) Uani 1 1 d . . . H36 H -0.1247 0.0028 0.5115 0.055 Uiso 1 1 calc R . . C37 C -0.0163(4) 0.0419(4) 0.55658(15) 0.0492(11) Uani 1 1 d . . . H37 H -0.0008 -0.0446 0.5630 0.059 Uiso 1 1 calc R . . C38 C 0.0349(3) 0.1380(4) 0.57810(13) 0.0399(9) Uani 1 1 d . . . H38 H 0.0847 0.1176 0.5995 0.048 Uiso 1 1 calc R . . C41 C 0.3685(3) 0.2161(4) 0.72014(11) 0.0335(9) Uani 1 1 d . . . C42 C 0.4315(3) 0.3186(4) 0.72705(11) 0.0352(9) Uani 1 1 d . . . H42 H 0.4110 0.3963 0.7381 0.042 Uiso 1 1 calc R . . C43 C 0.5237(3) 0.3076(5) 0.71782(13) 0.0435(10) Uani 1 1 d . . . H43 H 0.5659 0.3775 0.7227 0.052 Uiso 1 1 calc R . . C44 C 0.5540(3) 0.1948(5) 0.70159(14) 0.0472(11) Uani 1 1 d . . . H44 H 0.6165 0.1876 0.6948 0.057 Uiso 1 1 calc R . . C45 C 0.4927(3) 0.0930(5) 0.69533(13) 0.0452(11) Uani 1 1 d . . . H45 H 0.5139 0.0153 0.6845 0.054 Uiso 1 1 calc R . . C46 C 0.4004(3) 0.1021(4) 0.70460(12) 0.0381(9) Uani 1 1 d . . . H46 H 0.3593 0.0309 0.7004 0.046 Uiso 1 1 calc R . . C47 C 0.2275(3) 0.3383(4) 0.76618(12) 0.0342(9) Uani 1 1 d . . . C48 C 0.2958(3) 0.3485(5) 0.80104(12) 0.0420(10) Uani 1 1 d . . . H48 H 0.3521 0.2997 0.8027 0.050 Uiso 1 1 calc R . . C49 C 0.2806(4) 0.4312(5) 0.83347(13) 0.0496(12) Uani 1 1 d . . . H49 H 0.3278 0.4405 0.8568 0.060 Uiso 1 1 calc R . . C50 C 0.1977(4) 0.4997(5) 0.83203(14) 0.0496(12) Uani 1 1 d . . . H50 H 0.1878 0.5551 0.8544 0.060 Uiso 1 1 calc R . . C51 C 0.1290(4) 0.4874(4) 0.79777(14) 0.0451(11) Uani 1 1 d . . . H51 H 0.0715 0.5335 0.7967 0.054 Uiso 1 1 calc R . . C52 C 0.1445(3) 0.4072(4) 0.76494(13) 0.0365(9) Uani 1 1 d . . . H52 H 0.0977 0.3996 0.7414 0.044 Uiso 1 1 calc R . . C53 C 0.2005(3) 0.0785(4) 0.73359(12) 0.0360(9) Uani 1 1 d . . . C54 C 0.2049(4) 0.0336(5) 0.77432(15) 0.0584(14) Uani 1 1 d . . . H54 H 0.2309 0.0854 0.7971 0.070 Uiso 1 1 calc R . . C55 C 0.1716(6) -0.0863(6) 0.78153(18) 0.078(2) Uani 1 1 d . . . H55 H 0.1756 -0.1177 0.8094 0.094 Uiso 1 1 calc R . . C56 C 0.1323(4) -0.1616(5) 0.7485(2) 0.0661(16) Uani 1 1 d . . . H56 H 0.1076 -0.2433 0.7538 0.079 Uiso 1 1 calc R . . C57 C 0.1291(4) -0.1184(5) 0.70865(18) 0.0543(12) Uani 1 1 d . . . H57 H 0.1042 -0.1713 0.6860 0.065 Uiso 1 1 calc R . . C58 C 0.1617(3) 0.0018(4) 0.70085(15) 0.0442(10) Uani 1 1 d . . . H58 H 0.1576 0.0321 0.6729 0.053 Uiso 1 1 calc R . . B1A B 0.2602(5) 0.9086(6) 0.5950(2) 0.0530(19) Uani 0.794(4) 1 d PD A 1 F1A F 0.3229(4) 0.9087(7) 0.63096(15) 0.127(3) Uani 0.794(4) 1 d PD A 1 F2A F 0.2951(5) 0.8330(5) 0.56645(14) 0.0886(17) Uani 0.794(4) 1 d PD A 1 F3A F 0.1756(3) 0.8562(5) 0.60221(16) 0.0915(15) Uani 0.794(4) 1 d PD A 1 F4A F 0.2439(4) 1.0283(4) 0.5821(3) 0.177(5) Uani 0.794(4) 1 d PD A 1 B1B B 0.2951(12) 0.9497(16) 0.5868(5) 0.0530(19) Uani 0.206(4) 1 d PD A 2 F1B F 0.2520(13) 0.9873(17) 0.6197(6) 0.177(5) Uani 0.206(4) 1 d PD A 2 F2B F 0.2898(18) 0.8236(16) 0.5818(7) 0.0886(17) Uani 0.206(4) 1 d PD A 2 F3B F 0.3856(10) 0.9872(19) 0.5929(5) 0.0915(15) Uani 0.206(4) 1 d PD A 2 F4B F 0.2488(15) 1.006(2) 0.5527(5) 0.127(3) Uani 0.206(4) 1 d PD A 2 C61A C 0.6257(9) 0.1067(16) 0.5140(4) 0.157(9) Uani 0.694(5) 1 d PD B 3 H61A H 0.6814 0.1589 0.5098 0.189 Uiso 0.694(5) 1 calc PR B 3 H61B H 0.6110 0.0557 0.4881 0.189 Uiso 0.694(5) 1 calc PR B 3 Cl2A Cl 0.6671(4) -0.0032(5) 0.55247(10) 0.142(2) Uani 0.694(5) 1 d PD B 3 Cl3A Cl 0.5352(7) 0.2129(8) 0.5131(3) 0.1180(18) Uani 0.694(5) 1 d PD B 3 C61B C 0.613(2) 0.188(3) 0.5370(11) 0.157(9) Uani 0.306(5) 1 d PD B 4 H61C H 0.6375 0.2528 0.5578 0.189 Uiso 0.306(5) 1 calc PR B 4 H61D H 0.6609 0.1764 0.5178 0.189 Uiso 0.306(5) 1 calc PR B 4 Cl2B Cl 0.6067(9) 0.0475(12) 0.5636(2) 0.142(2) Uani 0.306(5) 1 d PD B 4 Cl3B Cl 0.5178(18) 0.252(2) 0.5086(8) 0.1180(18) Uani 0.306(5) 1 d PD B 4 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 0.02907(17) 0.02766(17) 0.02355(15) 0.00219(11) 0.00389(11) -0.00099(11) Cl1 0.0334(5) 0.0391(6) 0.0393(5) 0.0068(4) 0.0095(4) -0.0038(4) P1 0.0312(5) 0.0256(5) 0.0249(4) 0.0009(4) 0.0025(4) -0.0016(4) P2 0.0352(5) 0.0301(5) 0.0240(4) 0.0017(4) 0.0036(4) 0.0007(4) N1 0.0328(17) 0.0329(18) 0.0285(15) 0.0005(13) 0.0039(13) -0.0018(14) N2 0.0309(17) 0.0386(19) 0.0337(16) 0.0030(15) 0.0046(13) -0.0084(15) N3 0.0326(18) 0.049(2) 0.0365(17) 0.0036(16) 0.0071(14) -0.0075(16) N4 0.0335(19) 0.060(3) 0.0408(18) -0.0064(18) 0.0079(15) -0.0025(17) C1 0.042(2) 0.0278(19) 0.0198(15) 0.0017(14) -0.0025(15) 0.0033(17) C2 0.034(2) 0.035(2) 0.0276(17) -0.0021(16) 0.0033(15) -0.0015(17) C3 0.033(2) 0.043(2) 0.0285(17) -0.0032(17) 0.0060(15) 0.0028(18) C4 0.0256(18) 0.045(2) 0.0276(17) 0.0056(17) 0.0007(14) -0.0033(17) C5 0.043(2) 0.057(3) 0.035(2) 0.001(2) 0.0048(18) -0.014(2) C6 0.042(2) 0.068(4) 0.044(2) 0.001(2) 0.0084(19) -0.019(2) C7 0.034(2) 0.081(4) 0.032(2) -0.007(2) 0.0072(17) -0.010(2) C8 0.053(3) 0.048(3) 0.071(3) 0.011(3) 0.007(2) -0.016(2) C9 0.037(3) 0.100(5) 0.055(3) -0.012(3) 0.013(2) -0.003(3) C10 0.037(2) 0.029(2) 0.051(2) -0.0065(18) 0.0046(18) -0.0008(17) C11 0.062(3) 0.067(4) 0.063(3) -0.028(3) -0.002(3) 0.015(3) C21 0.0327(19) 0.033(2) 0.0225(16) 0.0031(15) -0.0007(14) -0.0005(16) C22 0.038(2) 0.038(2) 0.0308(18) 0.0058(17) 0.0031(16) -0.0042(18) C23 0.044(2) 0.048(3) 0.037(2) 0.0103(19) 0.0024(18) -0.013(2) C24 0.039(2) 0.072(3) 0.032(2) 0.001(2) 0.0100(17) -0.008(2) C25 0.045(2) 0.063(3) 0.032(2) -0.009(2) 0.0102(18) 0.003(2) C26 0.044(2) 0.042(2) 0.0263(17) -0.0029(17) 0.0028(16) -0.0016(19) C27 0.0310(19) 0.0272(19) 0.0319(18) -0.0011(15) 0.0033(15) -0.0036(16) C28 0.039(2) 0.031(2) 0.0343(19) -0.0026(16) 0.0074(16) -0.0047(18) C29 0.045(2) 0.034(2) 0.048(2) -0.0078(19) 0.0117(19) -0.0028(19) C30 0.041(2) 0.026(2) 0.063(3) -0.006(2) 0.007(2) 0.0034(18) C31 0.041(2) 0.031(2) 0.047(2) 0.0034(18) -0.0063(19) -0.0009(18) C32 0.038(2) 0.025(2) 0.0354(19) -0.0022(16) -0.0002(16) -0.0025(17) C33 0.0310(19) 0.0279(19) 0.0314(18) -0.0004(15) 0.0060(15) 0.0004(16) C34 0.035(2) 0.031(2) 0.0320(18) -0.0017(16) 0.0034(16) -0.0002(17) C35 0.039(2) 0.041(2) 0.041(2) -0.0025(19) -0.0020(18) -0.0034(19) C36 0.049(3) 0.039(2) 0.049(2) -0.005(2) 0.000(2) -0.014(2) C37 0.064(3) 0.026(2) 0.055(3) -0.001(2) -0.001(2) -0.006(2) C38 0.047(2) 0.031(2) 0.040(2) 0.0031(18) -0.0008(18) -0.0003(19) C41 0.039(2) 0.037(2) 0.0237(16) 0.0038(16) 0.0000(15) 0.0021(18) C42 0.035(2) 0.040(2) 0.0298(18) -0.0015(17) 0.0000(16) 0.0017(18) C43 0.043(2) 0.053(3) 0.034(2) 0.0044(19) 0.0002(18) -0.006(2) C44 0.037(2) 0.064(3) 0.041(2) 0.004(2) 0.0040(19) 0.010(2) C45 0.045(2) 0.049(3) 0.041(2) 0.002(2) 0.0056(19) 0.010(2) C46 0.042(2) 0.036(2) 0.0362(19) 0.0016(17) 0.0033(17) 0.0074(19) C47 0.044(2) 0.031(2) 0.0281(17) 0.0014(16) 0.0058(16) -0.0028(18) C48 0.051(3) 0.047(3) 0.0288(18) 0.0000(18) 0.0079(18) 0.000(2) C49 0.062(3) 0.055(3) 0.032(2) -0.008(2) 0.008(2) -0.005(2) C50 0.076(3) 0.039(3) 0.038(2) -0.0076(19) 0.022(2) -0.007(2) C51 0.056(3) 0.033(2) 0.049(2) 0.0003(19) 0.017(2) 0.005(2) C52 0.041(2) 0.032(2) 0.038(2) 0.0012(17) 0.0101(17) 0.0043(18) C53 0.040(2) 0.034(2) 0.0360(19) 0.0037(17) 0.0115(17) 0.0036(18) C54 0.095(4) 0.047(3) 0.038(2) 0.003(2) 0.025(2) -0.005(3) C55 0.141(6) 0.047(3) 0.058(3) 0.012(3) 0.053(4) -0.007(4) C56 0.082(4) 0.035(3) 0.092(4) 0.003(3) 0.049(3) -0.008(3) C57 0.050(3) 0.035(2) 0.077(3) -0.002(2) 0.009(2) 0.001(2) C58 0.043(2) 0.036(2) 0.052(2) 0.000(2) 0.001(2) -0.001(2) B1A 0.073(5) 0.025(4) 0.061(4) -0.009(3) 0.008(4) 0.000(3) F1A 0.095(4) 0.203(7) 0.075(3) -0.067(4) -0.014(3) -0.007(4) F2A 0.098(3) 0.099(3) 0.064(4) -0.040(3) -0.007(3) 0.019(2) F3A 0.074(3) 0.104(4) 0.095(3) 0.018(3) 0.008(2) -0.017(3) F4A 0.078(3) 0.031(3) 0.414(15) 0.046(5) -0.009(6) 0.011(2) B1B 0.073(5) 0.025(4) 0.061(4) -0.009(3) 0.008(4) 0.000(3) F1B 0.078(3) 0.031(3) 0.414(15) 0.046(5) -0.009(6) 0.011(2) F2B 0.098(3) 0.099(3) 0.064(4) -0.040(3) -0.007(3) 0.019(2) F3B 0.074(3) 0.104(4) 0.095(3) 0.018(3) 0.008(2) -0.017(3) F4B 0.095(4) 0.203(7) 0.075(3) -0.067(4) -0.014(3) -0.007(4) C61A 0.079(7) 0.28(2) 0.109(11) 0.115(14) 0.009(8) -0.019(11) Cl2A 0.185(5) 0.180(4) 0.0611(16) 0.034(2) 0.0178(18) -0.079(4) Cl3A 0.125(4) 0.140(6) 0.098(3) -0.029(3) 0.048(3) -0.037(3) C61B 0.079(7) 0.28(2) 0.109(11) 0.115(14) 0.009(8) -0.019(11) Cl2B 0.185(5) 0.180(4) 0.0611(16) 0.034(2) 0.0178(18) -0.079(4) Cl3B 0.125(4) 0.140(6) 0.098(3) -0.029(3) 0.048(3) -0.037(3) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; 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 Pd1 C1 1.982(4) . ? Pd1 P1 2.3208(9) . ? Pd1 P2 2.3431(10) . ? Pd1 Cl1 2.3463(10) . ? P1 C33 1.816(4) . ? P1 C27 1.823(4) . ? P1 C21 1.826(4) . ? P2 C53 1.817(4) . ? P2 C47 1.822(4) . ? P2 C41 1.824(4) . ? N1 C1 1.336(5) . ? N1 N2 1.350(4) . ? N1 C10 1.491(5) . ? N2 C4 1.305(5) . ? N3 N4 1.374(5) . ? N3 C5 1.390(6) . ? N3 C4 1.405(5) . ? N4 C7 1.334(6) . ? C1 C2 1.433(6) . ? C2 C3 1.346(6) . ? C3 C4 1.405(6) . ? C5 C6 1.370(7) . ? C5 C8 1.471(8) . ? C6 C7 1.413(8) . ? C7 C9 1.485(7) . ? C10 C11 1.475(7) . ? C21 C22 1.392(6) . ? C21 C26 1.396(6) . ? C22 C23 1.389(6) . ? C23 C24 1.381(7) . ? C24 C25 1.378(7) . ? C25 C26 1.376(6) . ? C27 C32 1.388(5) . ? C27 C28 1.409(5) . ? C28 C29 1.381(6) . ? C29 C30 1.382(7) . ? C30 C31 1.390(6) . ? C31 C32 1.383(6) . ? C33 C38 1.390(6) . ? C33 C34 1.391(5) . ? C34 C35 1.388(6) . ? C35 C36 1.386(6) . ? C36 C37 1.376(7) . ? C37 C38 1.380(6) . ? C41 C46 1.396(6) . ? C41 C42 1.402(6) . ? C42 C43 1.393(6) . ? C43 C44 1.385(7) . ? C44 C45 1.380(7) . ? C45 C46 1.392(6) . ? C47 C52 1.385(6) . ? C47 C48 1.396(6) . ? C48 C49 1.395(6) . ? C49 C50 1.383(7) . ? C50 C51 1.388(7) . ? C51 C52 1.391(6) . ? C53 C58 1.385(6) . ? C53 C54 1.388(6) . ? C54 C55 1.375(8) . ? C55 C56 1.385(9) . ? C56 C57 1.358(8) . ? C57 C58 1.379(7) . ? B1A F4A 1.334(7) . ? B1A F2A 1.356(8) . ? B1A F1A 1.371(8) . ? B1A F3A 1.375(8) . ? B1B F2B 1.334(15) . ? B1B F3B 1.343(15) . ? B1B F4B 1.345(15) . ? B1B F1B 1.350(15) . ? C61A Cl3A 1.706(12) . ? C61A Cl2A 1.740(9) . ? C61B Cl3B 1.677(16) . ? C61B Cl2B 1.711(16) . ? 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 C1 Pd1 P1 89.40(10) . . ? C1 Pd1 P2 89.39(10) . . ? P1 Pd1 P2 176.54(4) . . ? C1 Pd1 Cl1 178.38(10) . . ? P1 Pd1 Cl1 88.99(3) . . ? P2 Pd1 Cl1 92.24(4) . . ? C33 P1 C27 108.51(18) . . ? C33 P1 C21 103.57(17) . . ? C27 P1 C21 106.27(18) . . ? C33 P1 Pd1 111.70(13) . . ? C27 P1 Pd1 112.98(12) . . ? C21 P1 Pd1 113.21(12) . . ? C53 P2 C47 107.17(18) . . ? C53 P2 C41 104.64(19) . . ? C47 P2 C41 107.60(19) . . ? C53 P2 Pd1 112.04(14) . . ? C47 P2 Pd1 112.23(14) . . ? C41 P2 Pd1 112.70(12) . . ? C1 N1 N2 126.0(3) . . ? C1 N1 C10 122.8(3) . . ? N2 N1 C10 111.1(3) . . ? C4 N2 N1 116.5(3) . . ? N4 N3 C5 113.4(4) . . ? N4 N3 C4 116.7(4) . . ? C5 N3 C4 129.8(4) . . ? C7 N4 N3 103.8(4) . . ? N1 C1 C2 115.6(4) . . ? N1 C1 Pd1 123.7(3) . . ? C2 C1 Pd1 120.7(3) . . ? C3 C2 C1 120.3(4) . . ? C2 C3 C4 117.5(4) . . ? N2 C4 C3 123.9(4) . . ? N2 C4 N3 115.7(4) . . ? C3 C4 N3 120.3(4) . . ? C6 C5 N3 103.9(5) . . ? C6 C5 C8 130.7(5) . . ? N3 C5 C8 125.3(4) . . ? C5 C6 C7 107.6(4) . . ? N4 C7 C6 111.3(4) . . ? N4 C7 C9 119.7(5) . . ? C6 C7 C9 129.0(5) . . ? C11 C10 N1 112.0(4) . . ? C22 C21 C26 118.8(4) . . ? C22 C21 P1 121.4(3) . . ? C26 C21 P1 119.0(3) . . ? C23 C22 C21 120.0(4) . . ? C24 C23 C22 120.8(4) . . ? C25 C24 C23 119.1(4) . . ? C26 C25 C24 120.9(4) . . ? C25 C26 C21 120.4(4) . . ? C32 C27 C28 119.3(4) . . ? C32 C27 P1 121.6(3) . . ? C28 C27 P1 119.0(3) . . ? C29 C28 C27 119.7(4) . . ? C28 C29 C30 120.2(4) . . ? C29 C30 C31 120.5(4) . . ? C32 C31 C30 119.6(4) . . ? C31 C32 C27 120.6(4) . . ? C38 C33 C34 119.4(4) . . ? C38 C33 P1 117.7(3) . . ? C34 C33 P1 122.7(3) . . ? C35 C34 C33 120.3(4) . . ? C36 C35 C34 119.8(4) . . ? C37 C36 C35 119.9(4) . . ? C36 C37 C38 120.8(4) . . ? C37 C38 C33 119.9(4) . . ? C46 C41 C42 118.8(4) . . ? C46 C41 P2 118.6(3) . . ? C42 C41 P2 121.6(3) . . ? C43 C42 C41 120.6(4) . . ? C44 C43 C42 120.0(4) . . ? C45 C44 C43 119.6(4) . . ? C44 C45 C46 121.1(4) . . ? C45 C46 C41 119.9(4) . . ? C52 C47 C48 119.5(4) . . ? C52 C47 P2 117.9(3) . . ? C48 C47 P2 122.6(3) . . ? C49 C48 C47 119.4(4) . . ? C50 C49 C48 120.8(4) . . ? C49 C50 C51 119.8(4) . . ? C50 C51 C52 119.7(4) . . ? C47 C52 C51 120.8(4) . . ? C58 C53 C54 119.2(4) . . ? C58 C53 P2 118.6(3) . . ? C54 C53 P2 122.1(4) . . ? C55 C54 C53 119.7(5) . . ? C54 C55 C56 120.6(5) . . ? C57 C56 C55 119.8(5) . . ? C56 C57 C58 120.4(5) . . ? C57 C58 C53 120.3(5) . . ? F4A B1A F2A 113.8(7) . . ? F4A B1A F1A 109.5(7) . . ? F2A B1A F1A 108.4(6) . . ? F4A B1A F3A 107.8(6) . . ? F2A B1A F3A 106.7(6) . . ? F1A B1A F3A 110.6(6) . . ? F2B B1B F3B 110.3(12) . . ? F2B B1B F4B 108.8(12) . . ? F3B B1B F4B 110.9(12) . . ? F2B B1B F1B 111.1(12) . . ? F3B B1B F1B 109.0(12) . . ? F4B B1B F1B 106.7(12) . . ? Cl3A C61A Cl2A 129.3(8) . . ? Cl3B C61B Cl2B 122.1(17) . . ? _diffrn_measured_fraction_theta_max 0.992 _diffrn_reflns_theta_full 25.69 _diffrn_measured_fraction_theta_full 0.992 _refine_diff_density_max 1.173 _refine_diff_density_min -1.519 _refine_diff_density_rms 0.092