# Electronic Supplementary Material (ESI) for Chemical Communications # This journal is © The Royal Society of Chemistry 2013 ####################################################################### # # Cambridge Crystallographic Data Centre # CCDC # ####################################################################### # # This CIF contains data from an original supplementary publication # deposited with the CCDC, and may include chemical, crystal, # experimental, refinement, atomic coordinates, # anisotropic displacement parameters and molecular geometry data, # as required by the journal to which it was submitted. # # This CIF is provided on the understanding that it is used for bona # fide research purposes only. It may contain copyright material # of the CCDC or of third parties, and may not be copied or further # disseminated in any form, whether machine-readable or not, # except for the purpose of generating routine backup copies # on your local computer system. # # For further information on the CCDC, data deposition and # data retrieval see: # www.ccdc.cam.ac.uk # # Bona fide researchers may freely download Mercury and enCIFer # from this site to visualise CIF-encoded structures and # to carry out CIF format checking respectively. # data_kimura4 #============================================================================== # CHEMICAL DATA _chemical_formula_sum 'C22 H26 B2 F8 O2 Pd3' _chemical_formula_moiety 'C22 H26 B2 F8 O2 Pd3' _chemical_formula_weight 815.25 _chemical_melting_point ? #============================================================================== # CRYSTAL DATA _symmetry_cell_setting monoclinic _symmetry_space_group_name_H-M 'P 1 21/n 1' _symmetry_space_group_name_Hall '-P 2yn' _symmetry_Int_Tables_number 14 loop_ _symmetry_equiv_pos_site_id _symmetry_equiv_pos_as_xyz 1 +X,+Y,+Z 2 1/2-X,1/2+Y,1/2-Z 3 -X,-Y,-Z 4 1/2+X,1/2-Y,1/2+Z #------------------------------------------------------------------------------ _cell_length_a 10.0392(6) _cell_length_b 16.3516(10) _cell_length_c 14.6824(8) _cell_angle_alpha 90.0000 _cell_angle_beta 93.4204(16) _cell_angle_gamma 90.0000 _cell_volume 2405.9(3) _cell_formula_units_Z 4 _cell_measurement_reflns_used 16098 _cell_measurement_theta_min 3.04 _cell_measurement_theta_max 27.45 _cell_measurement_temperature 123 #------------------------------------------------------------------------------ _exptl_crystal_description block _exptl_crystal_colour orange _exptl_crystal_size_max 0.200 _exptl_crystal_size_mid 0.200 _exptl_crystal_size_min 0.100 _exptl_crystal_density_diffrn 2.251 _exptl_crystal_density_meas ? _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1576.00 _exptl_absorpt_coefficient_mu 2.303 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_process_details 'ABSCOR (Rigaku, 1995)' _exptl_absorpt_correction_T_min 0.321 _exptl_absorpt_correction_T_max 0.794 #============================================================================== # EXPERIMENTAL DATA _diffrn_ambient_temperature 123 _diffrn_radiation_type 'Mo K\a' _diffrn_radiation_wavelength 0.71075 _diffrn_measurement_device_type 'Rigaku R-AXIS RAPID' _diffrn_measurement_method \w _diffrn_detector_area_resol_mean 10.000 _diffrn_reflns_number 22511 _diffrn_reflns_av_R_equivalents 0.0545 _diffrn_reflns_theta_max 27.45 _diffrn_reflns_theta_full 27.44 _diffrn_measured_fraction_theta_max 0.997 _diffrn_measured_fraction_theta_full 0.997 _diffrn_reflns_limit_h_min -13 _diffrn_reflns_limit_h_max 11 _diffrn_reflns_limit_k_min -21 _diffrn_reflns_limit_k_max 21 _diffrn_reflns_limit_l_min -19 _diffrn_reflns_limit_l_max 18 _diffrn_standards_number 0 _diffrn_standards_interval_count . _diffrn_standards_decay_% ? #============================================================================== # REFINEMENT DATA _refine_special_details ; Refinement was performed using reflections with F > 3.0 sigma(F). The weighted R-factor(wR), goodness of fit (S) and R-factor (gt) are based on F, with F set to zero for negative F. The threshold expression of F > 3.0 sigma(F) is used only for calculating R-factor (gt). ; _reflns_number_total 5472 _reflns_number_gt 4221 _reflns_threshold_expression F>3.0\s(F) _refine_ls_structure_factor_coef F _refine_ls_R_factor_gt 0.0540 _refine_ls_wR_factor_ref 0.0602 _refine_ls_number_restraints ? _refine_ls_hydrogen_treatment constr _refine_ls_number_reflns 4221 _refine_ls_number_parameters 356 _refine_ls_goodness_of_fit_ref 1.077 _refine_ls_weighting_scheme calc _refine_ls_weighting_details ; Chebychev polynomial with 3 parameters (Carruthers & Watkin, 1979) 7.7161 -1.2418 5.1639 ; _atom_sites_solution_hydrogens geom _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _refine_ls_shift/su_max 0.000 _refine_diff_density_max 7.330 _refine_diff_density_min -0.946 _refine_ls_extinction_method none _refine_ls_extinction_coef ? 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 for Crystallography (1992, Vol. C, Tables 4.2.6.8 and 6.1.1.4) ; H H 0.0000 0.0000 ; International Tables for Crystallography (1992, Vol. C, Table 6.1.1.4) ; B B 0.0013 0.0007 ; International Tables for Crystallography (1992, Vol. C, Tables 4.2.6.8 and 6.1.1.4) ; F F 0.0171 0.0103 ; International Tables for Crystallography (1992, Vol. C, Tables 4.2.6.8 and 6.1.1.4) ; O O 0.0106 0.0060 ; International Tables for Crystallography (1992, Vol. C, Tables 4.2.6.8 and 6.1.1.4) ; Pd Pd -0.9988 1.0072 ; International Tables for Crystallography (1992, Vol. C, Tables 4.2.6.8 and 6.1.1.4) ; #============================================================================== # ATOMIC COORDINATES AND THERMAL PARAMETERS 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 0.91762(5) 0.49897(3) 0.24389(3) 0.02188(13) Uani 1.0 4 d . . . Pd2 Pd 1.16859(5) 0.43394(3) 0.26038(3) 0.01915(13) Uani 1.0 4 d . . . Pd3 Pd 1.17364(5) 0.60086(3) 0.24828(3) 0.01868(13) Uani 1.0 4 d . . . F1 F 0.3559(5) 0.2997(3) 0.4593(3) 0.0318(11) Uani 1.0 4 d . . . F2 F 0.3408(6) 0.2748(4) 0.6104(4) 0.0491(16) Uani 1.0 4 d . . . F3 F 0.4163(5) 0.3982(3) 0.5621(3) 0.0354(12) Uani 1.0 4 d . . . F4 F 0.5427(5) 0.2841(3) 0.5529(3) 0.0319(12) Uani 1.0 4 d . . . F5 F 0.4664(9) 0.4038(5) -0.0243(5) 0.082(3) Uani 1.0 4 d . . . F6 F 0.3326(6) 0.3000(4) 0.0002(5) 0.0583(18) Uani 1.0 4 d . . . F7 F 0.3907(7) 0.3323(6) -0.1428(5) 0.072(3) Uani 1.0 4 d . . . F8 F 0.5417(7) 0.2768(6) -0.0432(5) 0.081(3) Uani 1.0 4 d . . . O1 O 1.2855(6) 0.3181(4) 0.2694(4) 0.0339(14) Uani 1.0 4 d . . . O2 O 1.0981(6) 0.2027(4) 0.2501(4) 0.0405(17) Uani 1.0 4 d . . . C1 C 0.9099(7) 0.5992(5) 0.3540(5) 0.0277(18) Uani 1.0 4 d . . . C2 C 0.8828(7) 0.5186(5) 0.3839(5) 0.0275(18) Uani 1.0 4 d . . . C3 C 0.9589(7) 0.4457(5) 0.3872(5) 0.0244(17) Uani 1.0 4 d . . . C4 C 1.0985(7) 0.4264(5) 0.3996(5) 0.0241(17) Uani 1.0 4 d . . . C5 C 1.2157(7) 0.4743(5) 0.4010(4) 0.0217(16) Uani 1.0 4 d . . . C6 C 1.2422(7) 0.5594(5) 0.3926(4) 0.0219(16) Uani 1.0 4 d . . . C7 C 1.1646(7) 0.6319(5) 0.3894(5) 0.0227(16) Uani 1.0 4 d . . . C8 C 1.0330(7) 0.6472(4) 0.3562(5) 0.0251(17) Uani 1.0 4 d . . . C9 C 0.9149(7) 0.5828(5) 0.1185(5) 0.0252(17) Uani 1.0 4 d . . . C10 C 0.8861(7) 0.5009(5) 0.0997(5) 0.0259(17) Uani 1.0 4 d . . . C11 C 0.9648(8) 0.4278(5) 0.1142(5) 0.0260(17) Uani 1.0 4 d . . . C12 C 1.1037(7) 0.4078(5) 0.1180(4) 0.0225(16) Uani 1.0 4 d . . . C13 C 1.2225(7) 0.4559(5) 0.1189(4) 0.0214(16) Uani 1.0 4 d . . . C14 C 1.2490(7) 0.5406(4) 0.1182(4) 0.0190(15) Uani 1.0 4 d . . . C15 C 1.1699(7) 0.6137(4) 0.1030(5) 0.0210(16) Uani 1.0 4 d . . . C16 C 1.0375(7) 0.6312(4) 0.1203(5) 0.0221(16) Uani 1.0 4 d . . . C17 C 0.5782(8) 0.4182(5) 0.3548(6) 0.0308(19) Uani 1.0 4 d . . . C18 C 0.5487(7) 0.4657(5) 0.2766(6) 0.0333(19) Uani 1.0 4 d . . . C19 C 0.5808(7) 0.4341(5) 0.1916(5) 0.0302(19) Uani 1.0 4 d . . . C20 C 0.6414(8) 0.3584(5) 0.1860(6) 0.032(2) Uani 1.0 4 d . . . C21 C 0.6738(8) 0.3138(5) 0.2651(6) 0.034(2) Uani 1.0 4 d . . . C22 C 0.6395(8) 0.3432(5) 0.3492(5) 0.0315(19) Uani 1.0 4 d . . . B1 B 0.4118(8) 0.3138(5) 0.5459(5) 0.0215(18) Uani 1.0 4 d . . . B2 B 0.4342(9) 0.3260(6) -0.0502(7) 0.033(3) Uani 1.0 4 d . . . H1 H 0.8277 0.6337 0.3463 0.0333 Uiso 1.0 4 calc R . . H2 H 0.7961 0.5125 0.4057 0.0331 Uiso 1.0 4 calc R . . H3 H 0.9022 0.3967 0.3976 0.0295 Uiso 1.0 4 calc R . . H4 H 1.1151 0.3695 0.4062 0.0288 Uiso 1.0 4 calc R . . H5 H 1.2943 0.4425 0.4113 0.0259 Uiso 1.0 4 calc R . . H6 H 1.3388 0.5719 0.4064 0.0262 Uiso 1.0 4 calc R . . H7 H 1.2093 0.6784 0.4152 0.0273 Uiso 1.0 4 calc R . . H8 H 1.0141 0.7071 0.3497 0.0299 Uiso 1.0 4 calc R . . H9 H 0.8333 0.6178 0.1129 0.0300 Uiso 1.0 4 calc R . . H10 H 0.8003 0.4916 0.0707 0.0309 Uiso 1.0 4 calc R . . H11 H 0.9085 0.3775 0.1066 0.0310 Uiso 1.0 4 calc R . . H12 H 1.1202 0.3506 0.1180 0.0269 Uiso 1.0 4 calc R . . H13 H 1.3012 0.4234 0.1228 0.0260 Uiso 1.0 4 calc R . . H14 H 1.3460 0.5517 0.1119 0.0228 Uiso 1.0 4 calc R . . H15 H 1.2161 0.6574 0.0763 0.0254 Uiso 1.0 4 calc R . . H16 H 1.0186 0.6911 0.1154 0.0262 Uiso 1.0 4 calc R . . H17 H 0.5552 0.4385 0.4124 0.0372 Uiso 1.0 4 calc R . . H18 H 0.5083 0.5180 0.2807 0.0396 Uiso 1.0 4 calc R . . H19 H 0.5611 0.4649 0.1376 0.0364 Uiso 1.0 4 calc R . . H20 H 0.6611 0.3370 0.1282 0.0394 Uiso 1.0 4 calc R . . H21 H 0.7187 0.2629 0.2610 0.0407 Uiso 1.0 4 calc R . . H22 H 0.6585 0.3118 0.4028 0.0378 Uiso 1.0 4 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_12 _atom_site_aniso_U_13 _atom_site_aniso_U_23 Pd1 0.0156(3) 0.0339(3) 0.0161(3) -0.00059(19) 0.00044(17) 0.00261(18) Pd2 0.0239(3) 0.0175(3) 0.0157(3) 0.00273(18) -0.00125(17) 0.00048(17) Pd3 0.0204(3) 0.0179(3) 0.0176(3) -0.00277(18) 0.00030(17) -0.00046(17) F1 0.036(3) 0.025(2) 0.032(3) 0.0015(18) -0.0127(18) -0.0077(17) F2 0.050(3) 0.048(3) 0.052(3) 0.008(3) 0.024(3) 0.018(3) F3 0.048(3) 0.019(2) 0.038(3) 0.0059(19) -0.012(2) -0.0064(18) F4 0.022(2) 0.035(3) 0.038(3) 0.0086(17) -0.0032(17) 0.0001(19) F5 0.120(7) 0.058(4) 0.073(5) -0.041(5) 0.045(5) -0.015(4) F6 0.045(4) 0.047(3) 0.086(5) -0.002(3) 0.032(3) 0.017(3) F7 0.049(4) 0.117(6) 0.049(4) 0.019(4) -0.010(3) -0.007(4) F8 0.053(4) 0.119(7) 0.073(5) 0.050(4) 0.017(4) 0.017(5) O1 0.039(3) 0.027(3) 0.034(3) 0.012(3) -0.011(3) -0.003(3) O2 0.043(4) 0.047(4) 0.030(3) 0.005(3) -0.005(3) 0.002(3) C1 0.020(4) 0.042(4) 0.021(4) 0.012(3) 0.003(3) -0.003(3) C2 0.020(4) 0.044(5) 0.019(3) -0.001(3) 0.004(3) 0.000(3) C3 0.019(3) 0.039(4) 0.016(3) -0.010(3) 0.004(3) -0.002(3) C4 0.027(4) 0.025(4) 0.020(3) -0.004(3) -0.001(3) 0.003(3) C5 0.024(4) 0.027(4) 0.014(3) 0.002(3) -0.002(3) -0.001(3) C6 0.020(4) 0.029(4) 0.016(3) -0.001(3) -0.001(3) -0.005(3) C7 0.022(4) 0.027(4) 0.019(3) -0.002(3) 0.002(3) -0.007(3) C8 0.024(4) 0.021(4) 0.030(4) 0.008(3) -0.002(3) -0.006(3) C9 0.016(4) 0.041(4) 0.018(3) 0.004(3) -0.003(3) 0.008(3) C10 0.019(3) 0.041(4) 0.017(3) -0.009(3) -0.004(3) 0.000(3) C11 0.035(4) 0.026(4) 0.017(3) -0.010(3) -0.002(3) -0.002(3) C12 0.030(4) 0.023(4) 0.014(3) 0.002(3) -0.000(3) -0.004(3) C13 0.020(3) 0.031(4) 0.013(3) 0.008(3) 0.005(3) -0.001(3) C14 0.019(3) 0.022(3) 0.016(3) 0.002(3) 0.000(3) -0.004(3) C15 0.024(4) 0.019(3) 0.021(3) -0.002(3) 0.006(3) 0.003(3) C16 0.024(4) 0.021(3) 0.021(3) 0.005(3) -0.006(3) 0.006(3) C17 0.023(4) 0.036(4) 0.034(4) -0.009(3) 0.007(3) -0.011(3) C18 0.021(4) 0.033(4) 0.045(5) 0.000(3) -0.004(3) -0.018(4) C19 0.020(4) 0.046(5) 0.025(4) -0.002(3) 0.005(3) 0.003(3) C20 0.030(4) 0.038(5) 0.030(4) -0.004(3) 0.011(3) -0.002(3) C21 0.032(4) 0.034(5) 0.036(4) -0.001(3) 0.004(3) -0.000(3) C22 0.028(4) 0.036(4) 0.030(4) -0.007(3) -0.000(3) -0.001(3) B1 0.023(4) 0.017(4) 0.024(4) 0.001(3) 0.001(3) 0.002(3) B2 0.028(5) 0.033(5) 0.038(5) 0.003(4) 0.002(4) 0.001(4) #============================================================================== _computing_data_collection 'RAPID AUTO (Rigaku, ????)' _computing_cell_refinement 'RAPID AUTO' _computing_data_reduction 'RAPID AUTO' _computing_structure_solution 'SIR92 (Altomare, et al., 1994)' _computing_structure_refinement 'CRYSTALS (Carruthers, et al., 1999)' _computing_publication_material 'CrystalStructure 4.0 (Rigaku, 2010)' _computing_molecular_graphics 'CrystalStructure 4.0' #============================================================================== # MOLECULAR GEOMETRY _geom_special_details ; ENTER SPECIAL DETAILS OF THE MOLECULAR GEOMETRY ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_publ_flag _geom_bond_site_symmetry_1 _geom_bond_site_symmetry_2 Pd1 Pd2 2.7321(8) yes . . Pd1 C1 2.306(8) yes . . Pd1 C2 2.130(7) yes . . Pd1 C3 2.291(7) yes . . Pd1 C9 2.294(7) yes . . Pd1 C10 2.122(7) yes . . Pd1 C11 2.305(7) yes . . Pd2 Pd3 2.7359(8) yes . . Pd2 O1 2.228(6) yes . . Pd2 C4 2.204(7) yes . . Pd2 C5 2.193(6) yes . . Pd2 C12 2.194(6) yes . . Pd2 C13 2.207(6) yes . . Pd3 C6 2.291(6) yes . . Pd3 C7 2.140(7) yes . . Pd3 C8 2.312(7) yes . . Pd3 C14 2.316(6) yes . . Pd3 C15 2.142(7) yes . . Pd3 C16 2.310(7) yes . . F1 B1 1.378(9) yes . . F2 B1 1.375(10) yes . . F3 B1 1.401(9) yes . . F4 B1 1.400(9) yes . . F5 B2 1.361(12) yes . . F6 B2 1.363(12) yes . . F7 B2 1.408(11) yes . . F8 B2 1.345(12) yes . . C1 C2 1.420(11) yes . . C1 C8 1.464(10) yes . . C2 C3 1.414(11) yes . . C3 C4 1.438(10) yes . . C4 C5 1.413(10) yes . . C5 C6 1.422(10) yes . . C6 C7 1.418(10) yes . . C7 C8 1.404(10) yes . . C9 C10 1.394(11) yes . . C9 C16 1.462(10) yes . . C10 C11 1.442(11) yes . . C11 C12 1.430(11) yes . . C12 C13 1.428(10) yes . . C13 C14 1.412(10) yes . . C14 C15 1.444(10) yes . . C15 C16 1.398(10) yes . . C17 C18 1.403(12) yes . . C17 C22 1.376(11) yes . . C18 C19 1.405(12) yes . . C19 C20 1.384(12) yes . . C20 C21 1.393(11) yes . . C21 C22 1.388(12) yes . . C1 H1 1.000 no . . C2 H2 0.950 no . . C3 H3 1.000 no . . C4 H4 0.950 no . . C5 H5 0.950 no . . C6 H6 1.000 no . . C7 H7 0.950 no . . C8 H8 1.000 no . . C9 H9 1.000 no . . C10 H10 0.950 no . . C11 H11 1.000 no . . C12 H12 0.950 no . . C13 H13 0.950 no . . C14 H14 1.000 no . . C15 H15 0.950 no . . C16 H16 1.000 no . . C17 H17 0.950 no . . C18 H18 0.950 no . . C19 H19 0.950 no . . C20 H20 0.950 no . . C21 H21 0.950 no . . C22 H22 0.950 no . . loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_publ_flag _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_2 _geom_angle_site_symmetry_3 Pd2 Pd1 C1 106.49(18) yes . . . Pd2 Pd1 C2 100.17(19) yes . . . Pd2 Pd1 C3 69.85(17) yes . . . Pd2 Pd1 C9 105.68(17) yes . . . Pd2 Pd1 C10 100.13(19) yes . . . Pd2 Pd1 C11 69.07(19) yes . . . C1 Pd1 C2 37.1(3) yes . . . C1 Pd1 C3 68.8(3) yes . . . C1 Pd1 C9 98.0(3) yes . . . C1 Pd1 C10 132.8(3) yes . . . C1 Pd1 C11 162.7(3) yes . . . C2 Pd1 C3 37.1(3) yes . . . C2 Pd1 C9 133.6(3) yes . . . C2 Pd1 C10 159.6(3) yes . . . C2 Pd1 C11 158.0(3) yes . . . C3 Pd1 C9 163.1(3) yes . . . C3 Pd1 C10 158.4(3) yes . . . C3 Pd1 C11 122.1(3) yes . . . C9 Pd1 C10 36.5(3) yes . . . C9 Pd1 C11 68.4(3) yes . . . C10 Pd1 C11 37.7(3) yes . . . Pd1 Pd2 Pd3 68.070(19) yes . . . Pd1 Pd2 O1 144.69(15) yes . . . Pd1 Pd2 C4 76.13(18) yes . . . Pd1 Pd2 C5 96.44(18) yes . . . Pd1 Pd2 C12 76.80(19) yes . . . Pd1 Pd2 C13 97.48(17) yes . . . Pd3 Pd2 O1 147.15(15) yes . . . Pd3 Pd2 C4 97.12(19) yes . . . Pd3 Pd2 C5 75.93(18) yes . . . Pd3 Pd2 C12 97.94(18) yes . . . Pd3 Pd2 C13 76.72(19) yes . . . O1 Pd2 C4 95.4(3) yes . . . O1 Pd2 C5 96.7(3) yes . . . O1 Pd2 C12 91.0(3) yes . . . O1 Pd2 C13 92.1(3) yes . . . C4 Pd2 C5 37.5(3) yes . . . C4 Pd2 C12 141.2(3) yes . . . C4 Pd2 C13 172.5(3) yes . . . C5 Pd2 C12 172.3(3) yes . . . C5 Pd2 C13 141.8(3) yes . . . C12 Pd2 C13 37.9(3) yes . . . Pd2 Pd3 C6 69.52(17) yes . . . Pd2 Pd3 C7 99.87(19) yes . . . Pd2 Pd3 C8 105.57(17) yes . . . Pd2 Pd3 C14 68.75(17) yes . . . Pd2 Pd3 C15 99.37(18) yes . . . Pd2 Pd3 C16 104.74(17) yes . . . C6 Pd3 C7 37.1(3) yes . . . C6 Pd3 C8 68.0(3) yes . . . C6 Pd3 C14 122.8(3) yes . . . C6 Pd3 C15 159.5(3) yes . . . C6 Pd3 C16 161.1(3) yes . . . C7 Pd3 C8 36.5(3) yes . . . C7 Pd3 C14 159.1(3) yes . . . C7 Pd3 C15 160.4(3) yes . . . C7 Pd3 C16 132.8(3) yes . . . C8 Pd3 C14 161.4(3) yes . . . C8 Pd3 C15 132.5(3) yes . . . C8 Pd3 C16 97.5(3) yes . . . C14 Pd3 C15 37.6(3) yes . . . C14 Pd3 C16 68.1(3) yes . . . C15 Pd3 C16 36.3(3) yes . . . Pd1 C1 C2 64.7(4) yes . . . Pd1 C1 C8 109.5(5) yes . . . C2 C1 C8 132.0(7) yes . . . Pd1 C2 C1 78.2(4) yes . . . Pd1 C2 C3 77.7(4) yes . . . C1 C2 C3 132.8(7) yes . . . Pd1 C3 C2 65.3(4) yes . . . Pd1 C3 C4 108.7(5) yes . . . C2 C3 C4 135.2(7) yes . . . Pd2 C4 C3 103.5(5) yes . . . Pd2 C4 C5 70.8(4) yes . . . C3 C4 C5 133.2(7) yes . . . Pd2 C5 C4 71.7(4) yes . . . Pd2 C5 C6 104.1(4) yes . . . C4 C5 C6 134.5(7) yes . . . Pd3 C6 C5 108.8(4) yes . . . Pd3 C6 C7 65.6(4) yes . . . C5 C6 C7 135.6(7) yes . . . Pd3 C7 C6 77.2(4) yes . . . Pd3 C7 C8 78.4(4) yes . . . C6 C7 C8 131.7(7) yes . . . Pd3 C8 C1 111.0(5) yes . . . Pd3 C8 C7 65.1(4) yes . . . C1 C8 C7 133.4(7) yes . . . Pd1 C9 C10 65.0(4) yes . . . Pd1 C9 C16 109.8(5) yes . . . C10 C9 C16 133.5(7) yes . . . Pd1 C10 C9 78.4(4) yes . . . Pd1 C10 C11 78.0(4) yes . . . C9 C10 C11 131.4(7) yes . . . Pd1 C11 C10 64.2(4) yes . . . Pd1 C11 C12 109.3(5) yes . . . C10 C11 C12 136.0(7) yes . . . Pd2 C12 C11 103.1(5) yes . . . Pd2 C12 C13 71.5(4) yes . . . C11 C12 C13 133.4(7) yes . . . Pd2 C13 C12 70.6(4) yes . . . Pd2 C13 C14 102.9(4) yes . . . C12 C13 C14 134.3(7) yes . . . Pd3 C14 C13 109.9(5) yes . . . Pd3 C14 C15 64.7(4) yes . . . C13 C14 C15 135.3(6) yes . . . Pd3 C15 C14 77.8(4) yes . . . Pd3 C15 C16 78.4(4) yes . . . C14 C15 C16 131.4(6) yes . . . Pd3 C16 C9 110.8(5) yes . . . Pd3 C16 C15 65.3(4) yes . . . C9 C16 C15 134.0(7) yes . . . C18 C17 C22 121.2(8) yes . . . C17 C18 C19 118.4(8) yes . . . C18 C19 C20 120.4(7) yes . . . C19 C20 C21 120.1(8) yes . . . C20 C21 C22 120.1(8) yes . . . C17 C22 C21 119.8(8) yes . . . F1 B1 F2 111.0(6) yes . . . F1 B1 F3 109.3(6) yes . . . F1 B1 F4 109.8(6) yes . . . F2 B1 F3 110.6(6) yes . . . F2 B1 F4 108.1(6) yes . . . F3 B1 F4 108.0(6) yes . . . F5 B2 F6 108.3(8) yes . . . F5 B2 F7 104.8(8) yes . . . F5 B2 F8 111.2(8) yes . . . F6 B2 F7 110.4(7) yes . . . F6 B2 F8 113.3(8) yes . . . F7 B2 F8 108.6(8) yes . . . Pd1 C1 H1 112.593 no . . . C2 C1 H1 112.737 no . . . C8 C1 H1 112.885 no . . . Pd1 C2 H2 120.963 no . . . C1 C2 H2 113.427 no . . . C3 C2 H2 113.819 no . . . Pd1 C3 H3 111.811 no . . . C2 C3 H3 111.693 no . . . C4 C3 H3 111.334 no . . . Pd2 C4 H4 94.920 no . . . C3 C4 H4 113.058 no . . . C5 C4 H4 113.661 no . . . Pd2 C5 H5 96.621 no . . . C4 C5 H5 112.417 no . . . C6 C5 H5 113.068 no . . . Pd3 C6 H6 111.209 no . . . C5 C6 H6 111.504 no . . . C7 C6 H6 111.088 no . . . Pd3 C7 H7 121.969 no . . . C6 C7 H7 114.294 no . . . C8 C7 H7 114.008 no . . . Pd3 C8 H8 112.087 no . . . C1 C8 H8 111.614 no . . . C7 C8 H8 112.188 no . . . Pd1 C9 H9 112.254 no . . . C10 C9 H9 112.037 no . . . C16 C9 H9 112.079 no . . . Pd1 C10 H10 121.402 no . . . C9 C10 H10 114.425 no . . . C11 C10 H10 114.119 no . . . Pd1 C11 H11 111.352 no . . . C10 C11 H11 111.323 no . . . C12 C11 H11 111.119 no . . . Pd2 C12 H12 98.658 no . . . C11 C12 H12 113.264 no . . . C13 C12 H12 113.340 no . . . Pd2 C13 H13 95.878 no . . . C12 C13 H13 112.577 no . . . C14 C13 H13 113.099 no . . . Pd3 C14 H14 111.579 no . . . C13 C14 H14 111.259 no . . . C15 C14 H14 111.525 no . . . Pd3 C15 H15 120.299 no . . . C14 C15 H15 114.099 no . . . C16 C15 H15 114.477 no . . . Pd3 C16 H16 111.671 no . . . C9 C16 H16 111.945 no . . . C15 C16 H16 111.457 no . . . C18 C17 H17 118.991 no . . . C22 C17 H17 119.855 no . . . C17 C18 H18 121.052 no . . . C19 C18 H18 120.580 no . . . C18 C19 H19 120.006 no . . . C20 C19 H19 119.596 no . . . C19 C20 H20 119.965 no . . . C21 C20 H20 119.983 no . . . C20 C21 H21 119.609 no . . . C22 C21 H21 120.264 no . . . C17 C22 H22 120.014 no . . . C21 C22 H22 120.155 no . . . loop_ _geom_contact_atom_site_label_1 _geom_contact_atom_site_label_2 _geom_contact_distance _geom_contact_publ_flag _geom_contact_site_symmetry_1 _geom_contact_site_symmetry_2 C1 C4 3.444(11) no . . C1 C6 3.413(10) no . . C2 C5 3.414(10) no . . C2 C7 3.379(10) no . . C3 C6 3.395(10) no . . C3 C8 3.415(10) no . . C4 C7 3.429(10) no . . C5 C8 3.413(10) no . . C9 C12 3.432(11) no . . C9 C14 3.424(10) no . . C10 C13 3.452(10) no . . C10 C15 3.391(10) no . . C11 C14 3.396(10) no . . C11 C16 3.405(10) no . . C12 C15 3.441(10) no . . C13 C16 3.417(10) no . . C17 C20 2.772(11) no . . C18 C21 2.792(12) no . . C19 C22 2.783(11) no . . Pd1 C19 3.582(7) no . . Pd3 O1 3.587(6) no . 2_755 Pd3 O2 2.832(7) no . 2_755 F1 F8 3.391(9) no . 4_455 F1 O1 2.851(7) no . 1_455 F1 C4 3.387(9) no . 1_455 F1 C5 3.275(8) no . 1_455 F1 C15 3.182(8) no . 2_645 F1 C16 3.202(8) no . 2_645 F1 C17 3.391(9) no . . F1 C22 3.432(9) no . . F2 O2 3.222(8) no . 4_455 F2 C1 3.319(10) no . 3_666 F2 C11 3.538(9) no . 4_455 F2 C20 3.203(10) no . 4_455 F2 C21 3.245(10) no . 4_455 F3 C1 3.567(9) no . 3_666 F3 C2 3.431(9) no . 3_666 F3 C5 3.260(8) no . 1_455 F3 C6 3.522(8) no . 3_766 F3 C17 3.551(10) no . . F3 C17 3.240(9) no . 3_666 F3 C18 3.253(10) no . 3_666 F4 F6 3.352(8) no . 4_555 F4 O2 2.924(7) no . 4_455 F4 C6 3.413(8) no . 3_766 F4 C7 3.308(8) no . 3_766 F4 C12 3.327(8) no . 4_455 F4 C22 3.342(9) no . . F5 F5 3.286(10) no . 3_665 F5 C13 3.429(11) no . 1_455 F5 C14 3.369(11) no . 3_765 F5 C19 3.344(11) no . . F5 C20 3.540(11) no . . F6 F4 3.352(8) no . 4_454 F6 C7 3.191(10) no . 2_645 F6 C8 3.488(9) no . 2_645 F6 C9 3.517(9) no . 3_665 F6 C12 3.442(10) no . 1_455 F6 C13 3.314(10) no . 1_455 F7 O2 2.743(9) no . 4_454 F7 C9 3.406(10) no . 3_665 F7 C21 3.454(11) no . 4_454 F8 F1 3.391(9) no . 4_554 F8 O2 3.138(9) no . 4_454 F8 C4 3.483(12) no . 4_454 F8 C8 3.583(11) no . 2_645 F8 C15 3.559(10) no . 3_765 O1 Pd3 3.587(6) no . 2_745 O1 F1 2.851(7) no . 1_655 O1 O2 2.668(9) no . . O1 C17 3.527(10) no . 1_655 O1 C18 3.575(10) no . 1_655 O2 Pd3 2.832(7) no . 2_745 O2 F2 3.222(8) no . 4_554 O2 F4 2.924(7) no . 4_554 O2 F7 2.743(9) no . 4_555 O2 F8 3.138(9) no . 4_555 O2 O1 2.668(9) no . . O2 C6 3.586(9) no . 2_745 O2 C7 3.434(9) no . 2_745 O2 C14 3.573(9) no . 2_745 O2 C15 3.407(9) no . 2_745 O2 B1 3.449(10) no . 4_554 O2 B2 3.479(11) no . 4_555 C1 F2 3.319(10) no . 3_666 C1 F3 3.567(9) no . 3_666 C2 F3 3.431(9) no . 3_666 C2 C4 3.298(10) no . 3_766 C2 C5 3.366(10) no . 3_766 C2 C17 3.475(11) no . . C4 F1 3.387(9) no . 1_655 C4 F8 3.483(12) no . 4_555 C4 C2 3.298(10) no . 3_766 C5 F1 3.275(8) no . 1_655 C5 F3 3.260(8) no . 1_655 C5 C2 3.366(10) no . 3_766 C6 F3 3.522(8) no . 3_766 C6 F4 3.413(8) no . 3_766 C6 O2 3.586(9) no . 2_755 C7 F4 3.308(8) no . 3_766 C7 F6 3.191(10) no . 2_655 C7 O2 3.434(9) no . 2_755 C8 F6 3.488(9) no . 2_655 C8 F8 3.583(11) no . 2_655 C9 F6 3.517(9) no . 3_665 C9 F7 3.406(10) no . 3_665 C9 C12 3.470(9) no . 3_765 C10 C12 3.535(10) no . 3_765 C10 C13 3.402(9) no . 3_765 C10 C14 3.467(9) no . 3_765 C10 C15 3.532(10) no . 3_765 C10 C19 3.592(10) no . . C11 F2 3.538(9) no . 4_554 C11 C15 3.455(9) no . 3_765 C11 C16 3.574(9) no . 3_765 C12 F4 3.327(8) no . 4_554 C12 F6 3.442(10) no . 1_655 C12 C9 3.470(9) no . 3_765 C12 C10 3.535(10) no . 3_765 C13 F5 3.429(11) no . 1_655 C13 F6 3.314(10) no . 1_655 C13 C10 3.402(9) no . 3_765 C14 F5 3.369(11) no . 3_765 C14 O2 3.573(9) no . 2_755 C14 C10 3.467(9) no . 3_765 C15 F1 3.182(8) no . 2_655 C15 F8 3.559(10) no . 3_765 C15 O2 3.407(9) no . 2_755 C15 C10 3.532(10) no . 3_765 C15 C11 3.455(9) no . 3_765 C16 F1 3.202(8) no . 2_655 C16 C11 3.574(9) no . 3_765 C17 F1 3.391(9) no . . C17 F3 3.551(10) no . . C17 F3 3.240(9) no . 3_666 C17 O1 3.527(10) no . 1_455 C17 C2 3.475(11) no . . C18 F3 3.253(10) no . 3_666 C18 O1 3.575(10) no . 1_455 C19 Pd1 3.582(7) no . . C19 F5 3.344(11) no . . C19 C10 3.592(10) no . . C20 F2 3.203(10) no . 4_554 C20 F5 3.540(11) no . . C21 F2 3.245(10) no . 4_554 C21 F7 3.454(11) no . 4_555 C22 F1 3.432(9) no . . C22 F4 3.342(9) no . . B1 O2 3.449(10) no . 4_455 B2 O2 3.479(11) no . 4_454 Pd2 H3 3.4958 no . . Pd2 H6 3.4883 no . . Pd2 H11 3.4736 no . . Pd2 H14 3.4778 no . . O1 H4 2.8417 no . . O1 H5 2.9090 no . . O1 H12 2.7462 no . . O1 H13 2.7684 no . . C1 H3 3.3737 no . . C1 H7 3.3461 no . . C1 H9 3.5897 no . . C2 H4 3.3762 no . . C2 H8 3.4014 no . . C3 H1 3.3828 no . . C3 H5 3.3653 no . . C4 H2 3.3519 no . . C4 H6 3.3848 no . . C5 H3 3.3911 no . . C5 H7 3.3439 no . . C6 H4 3.3675 no . . C6 H8 3.3624 no . . C7 H1 3.4036 no . . C7 H5 3.3673 no . . C8 H2 3.3537 no . . C8 H6 3.3498 no . . C9 H11 3.3608 no . . C9 H15 3.3525 no . . C10 H12 3.4003 no . . C10 H16 3.3853 no . . C11 H9 3.3763 no . . C11 H13 3.3723 no . . C12 H10 3.3749 no . . C12 H14 3.3892 no . . C13 H11 3.3979 no . . C13 H15 3.3546 no . . C14 H12 3.3661 no . . C14 H16 3.3757 no . . C15 H9 3.3916 no . . C15 H13 3.3843 no . . C16 H10 3.3466 no . . C16 H14 3.3686 no . . C17 H19 3.2735 no . . C17 H21 3.2500 no . . C18 H20 3.2767 no . . C18 H22 3.2765 no . . C19 H17 3.2675 no . . C19 H21 3.2591 no . . C20 H18 3.2775 no . . C20 H22 3.2677 no . . C21 H17 3.2494 no . . C21 H19 3.2606 no . . C22 H18 3.2788 no . . C22 H20 3.2656 no . . H1 H2 2.1955 no . . H1 H8 2.2209 no . . H1 H9 3.4404 no . . H2 H3 2.1790 no . . H3 H4 2.1792 no . . H4 H5 2.1567 no . . H5 H6 2.1644 no . . H6 H7 2.1824 no . . H7 H8 2.1816 no . . H8 H16 3.4522 no . . H9 H10 2.1741 no . . H9 H16 2.2114 no . . H10 H11 2.2070 no . . H11 H12 2.1679 no . . H12 H13 2.1696 no . . H13 H14 2.1528 no . . H14 H15 2.2101 no . . H15 H16 2.1682 no . . H17 H18 2.3537 no . . H17 H22 2.3241 no . . H18 H19 2.3629 no . . H19 H20 2.3273 no . . H20 H21 2.3373 no . . H21 H22 2.3438 no . . F1 H4 2.7440 no . 1_455 F1 H5 2.5060 no . 1_455 F1 H15 2.4820 no . 2_645 F1 H16 2.4712 no . 2_645 F1 H17 3.1293 no . . F1 H22 3.2023 no . . F2 H1 2.3741 no . 3_666 F2 H11 2.5835 no . 4_455 F2 H12 3.4709 no . 4_455 F2 H15 3.3665 no . 2_645 F2 H20 2.5928 no . 4_455 F2 H21 2.6641 no . 4_455 F3 H1 2.9106 no . 3_666 F3 H2 2.6496 no . 3_666 F3 H5 2.5691 no . 1_455 F3 H6 2.5223 no . 3_766 F3 H17 2.7527 no . . F3 H17 2.7091 no . 3_666 F3 H18 2.7505 no . 3_666 F4 H6 2.6894 no . 3_766 F4 H7 2.5802 no . 3_766 F4 H11 3.0905 no . 4_455 F4 H12 2.5064 no . 4_455 F4 H16 2.9352 no . 2_645 F4 H17 3.2663 no . . F4 H22 2.5913 no . . F5 H9 3.2254 no . 3_665 F5 H10 3.2147 no . 3_665 F5 H13 2.8197 no . 1_455 F5 H14 3.4046 no . 1_455 F5 H14 2.4527 no . 3_765 F5 H15 3.4690 no . 3_765 F5 H19 2.6984 no . . F5 H19 2.7196 no . 3_665 F5 H20 3.0842 no . . F6 H7 2.3955 no . 2_645 F6 H8 3.0216 no . 2_645 F6 H9 2.6472 no . 3_665 F6 H12 2.9422 no . 1_455 F6 H13 2.7343 no . 1_455 F6 H22 2.8547 no . 4_454 F7 H9 2.4553 no . 3_665 F7 H14 3.2627 no . 3_765 F7 H18 3.3714 no . 3_665 F7 H19 3.3513 no . 3_665 F7 H21 2.6673 no . 4_454 F7 H22 3.4096 no . 4_454 F8 H3 3.2589 no . 4_454 F8 H4 2.6234 no . 4_454 F8 H8 3.1426 no . 2_645 F8 H14 3.2080 no . 3_765 F8 H15 2.7290 no . 3_765 F8 H20 2.8949 no . . O1 H7 3.5480 no . 2_745 O1 H8 3.2895 no . 2_745 O1 H15 3.4703 no . 2_745 O1 H16 3.2620 no . 2_745 O2 H4 3.5595 no . . O2 H6 3.2305 no . 2_745 O2 H7 3.2171 no . 2_745 O2 H12 3.1160 no . . O2 H14 3.2229 no . 2_745 O2 H15 3.1565 no . 2_745 O2 H18 3.2275 no . 2_645 C1 H4 3.5817 no . 3_766 C1 H21 3.3796 no . 2_655 C2 H4 3.5829 no . 3_766 C2 H17 3.5880 no . . C4 H2 3.1516 no . 3_766 C5 H2 2.8558 no . 3_766 C5 H17 3.4525 no . 1_655 C5 H18 3.5885 no . 1_655 C6 H2 3.2309 no . 3_766 C6 H3 3.5563 no . 3_766 C6 H17 3.4119 no . 3_766 C6 H18 3.2885 no . 1_655 C7 H3 3.2716 no . 3_766 C7 H22 3.5585 no . 3_766 C8 H21 3.5209 no . 2_655 C10 H19 3.3943 no . . C10 H20 3.5460 no . . C11 H15 3.5284 no . 3_765 C11 H20 3.4084 no . . C12 H9 3.5111 no . 3_765 C12 H10 3.4105 no . 3_765 C13 H10 2.9100 no . 3_765 C13 H19 3.3969 no . 1_655 C14 H10 2.8383 no . 3_765 C14 H18 3.4448 no . 1_655 C14 H19 3.3652 no . 1_655 C15 H10 3.1066 no . 3_765 C15 H11 3.1330 no . 3_765 C16 H11 3.4103 no . 3_765 C16 H22 3.5536 no . 2_655 C17 H2 2.7437 no . . C17 H3 3.2948 no . . C17 H5 3.0420 no . 1_455 C17 H6 3.5895 no . 1_455 C17 H6 3.5587 no . 3_766 C18 H2 3.1278 no . . C18 H5 3.3448 no . 1_455 C18 H6 3.4016 no . 1_455 C18 H13 3.3290 no . 1_455 C18 H14 3.3731 no . 1_455 C19 H10 3.0585 no . . C19 H13 2.9320 no . 1_455 C19 H14 3.2079 no . 1_455 C20 H8 2.9562 no . 2_645 C20 H10 3.2367 no . . C20 H11 3.0035 no . . C21 H1 3.3687 no . 2_645 C21 H3 3.2170 no . . C21 H8 3.0103 no . 2_645 C21 H11 3.5646 no . . C21 H16 3.3523 no . 2_645 C22 H2 3.2653 no . . C22 H3 2.8285 no . . C22 H16 3.0126 no . 2_645 B1 H1 3.0786 no . 3_666 B1 H5 3.0720 no . 1_455 B1 H6 3.1693 no . 3_766 B1 H11 3.2544 no . 4_455 B1 H12 3.5306 no . 4_455 B1 H15 3.3362 no . 2_645 B1 H16 3.2127 no . 2_645 B1 H17 3.2252 no . . B1 H22 3.3417 no . . B2 H7 3.4887 no . 2_645 B2 H8 3.5405 no . 2_645 B2 H9 2.9339 no . 3_665 B2 H13 3.3428 no . 1_455 B2 H14 3.1506 no . 3_765 B2 H15 3.5644 no . 3_765 B2 H20 3.3719 no . . H1 F2 2.3741 no . 3_666 H1 F3 2.9106 no . 3_666 H1 C21 3.3687 no . 2_655 H1 B1 3.0786 no . 3_666 H1 H20 3.3465 no . 2_655 H1 H21 2.6600 no . 2_655 H2 F3 2.6496 no . 3_666 H2 C4 3.1516 no . 3_766 H2 C5 2.8558 no . 3_766 H2 C6 3.2309 no . 3_766 H2 C17 2.7437 no . . H2 C18 3.1278 no . . H2 C22 3.2653 no . . H2 H4 3.4434 no . 3_766 H2 H5 2.9793 no . 3_766 H2 H6 3.4344 no . 3_766 H2 H17 2.7118 no . . H2 H18 3.3299 no . . H2 H22 3.5599 no . . H3 F8 3.2589 no . 4_555 H3 C6 3.5563 no . 3_766 H3 C7 3.2716 no . 3_766 H3 C17 3.2948 no . . H3 C21 3.2170 no . . H3 C22 2.8285 no . . H3 H7 3.2689 no . 3_766 H3 H17 3.5697 no . . H3 H21 3.4300 no . . H3 H22 2.8187 no . . H4 F1 2.7440 no . 1_655 H4 F8 2.6234 no . 4_555 H4 O2 3.5595 no . . H4 C1 3.5817 no . 3_766 H4 C2 3.5829 no . 3_766 H4 H2 3.4434 no . 3_766 H5 F1 2.5060 no . 1_655 H5 F3 2.5691 no . 1_655 H5 C17 3.0420 no . 1_655 H5 C18 3.3448 no . 1_655 H5 B1 3.0720 no . 1_655 H5 H2 2.9793 no . 3_766 H5 H17 2.6191 no . 1_655 H5 H17 3.5077 no . 3_766 H5 H18 3.2108 no . 1_655 H6 F3 2.5223 no . 3_766 H6 F4 2.6894 no . 3_766 H6 O2 3.2305 no . 2_755 H6 C17 3.5895 no . 1_655 H6 C17 3.5587 no . 3_766 H6 C18 3.4016 no . 1_655 H6 B1 3.1693 no . 3_766 H6 H2 3.4344 no . 3_766 H6 H17 3.0760 no . 1_655 H6 H17 2.8104 no . 3_766 H6 H18 2.7301 no . 1_655 H6 H22 3.3845 no . 3_766 H7 F4 2.5802 no . 3_766 H7 F6 2.3955 no . 2_655 H7 O1 3.5480 no . 2_755 H7 O2 3.2171 no . 2_755 H7 B2 3.4887 no . 2_655 H7 H3 3.2689 no . 3_766 H7 H12 3.3457 no . 2_755 H7 H22 2.9165 no . 3_766 H8 F6 3.0216 no . 2_655 H8 F8 3.1426 no . 2_655 H8 O1 3.2895 no . 2_755 H8 C20 2.9562 no . 2_655 H8 C21 3.0103 no . 2_655 H8 B2 3.5405 no . 2_655 H8 H20 2.7892 no . 2_655 H8 H21 2.9117 no . 2_655 H9 F5 3.2254 no . 3_665 H9 F6 2.6472 no . 3_665 H9 F7 2.4553 no . 3_665 H9 C12 3.5111 no . 3_765 H9 B2 2.9339 no . 3_665 H9 H12 3.4879 no . 3_765 H9 H21 3.0728 no . 2_655 H9 H22 3.1813 no . 2_655 H10 F5 3.2147 no . 3_665 H10 C12 3.4105 no . 3_765 H10 C13 2.9100 no . 3_765 H10 C14 2.8383 no . 3_765 H10 C15 3.1066 no . 3_765 H10 C19 3.0585 no . . H10 C20 3.2367 no . . H10 H13 3.2706 no . 3_765 H10 H14 3.0626 no . 3_765 H10 H15 3.2533 no . 3_765 H10 H19 2.6837 no . . H10 H20 3.0333 no . . H11 F2 2.5835 no . 4_554 H11 F4 3.0905 no . 4_554 H11 C15 3.1330 no . 3_765 H11 C16 3.4103 no . 3_765 H11 C20 3.0035 no . . H11 C21 3.5646 no . . H11 B1 3.2544 no . 4_554 H11 H15 2.9489 no . 3_765 H11 H16 3.5644 no . 3_765 H11 H20 2.6078 no . . H11 H21 3.5773 no . . H12 F2 3.4709 no . 4_554 H12 F4 2.5064 no . 4_554 H12 F6 2.9422 no . 1_655 H12 O2 3.1160 no . . H12 B1 3.5306 no . 4_554 H12 H7 3.3457 no . 2_745 H12 H9 3.4879 no . 3_765 H13 F5 2.8197 no . 1_655 H13 F6 2.7343 no . 1_655 H13 C18 3.3290 no . 1_655 H13 C19 2.9320 no . 1_655 H13 B2 3.3428 no . 1_655 H13 H10 3.2706 no . 3_765 H13 H18 3.3933 no . 1_655 H13 H19 2.6922 no . 1_655 H14 F5 3.4046 no . 1_655 H14 F5 2.4527 no . 3_765 H14 F7 3.2627 no . 3_765 H14 F8 3.2080 no . 3_765 H14 O2 3.2229 no . 2_755 H14 C18 3.3731 no . 1_655 H14 C19 3.2079 no . 1_655 H14 B2 3.1506 no . 3_765 H14 H10 3.0626 no . 3_765 H14 H18 2.9361 no . 1_655 H14 H19 2.5924 no . 1_655 H15 F1 2.4820 no . 2_655 H15 F2 3.3665 no . 2_655 H15 F5 3.4690 no . 3_765 H15 F8 2.7290 no . 3_765 H15 O1 3.4703 no . 2_755 H15 O2 3.1565 no . 2_755 H15 C11 3.5284 no . 3_765 H15 B1 3.3362 no . 2_655 H15 B2 3.5644 no . 3_765 H15 H10 3.2533 no . 3_765 H15 H11 2.9489 no . 3_765 H15 H20 3.3143 no . 3_765 H16 F1 2.4712 no . 2_655 H16 F4 2.9352 no . 2_655 H16 O1 3.2620 no . 2_755 H16 C21 3.3523 no . 2_655 H16 C22 3.0126 no . 2_655 H16 B1 3.2127 no . 2_655 H16 H11 3.5644 no . 3_765 H16 H21 3.2957 no . 2_655 H16 H22 2.6587 no . 2_655 H17 F1 3.1293 no . . H17 F3 2.7527 no . . H17 F3 2.7091 no . 3_666 H17 F4 3.2663 no . . H17 C2 3.5880 no . . H17 C5 3.4525 no . 1_455 H17 C6 3.4119 no . 3_766 H17 B1 3.2252 no . . H17 H2 2.7118 no . . H17 H3 3.5697 no . . H17 H5 2.6191 no . 1_455 H17 H5 3.5077 no . 3_766 H17 H6 3.0760 no . 1_455 H17 H6 2.8104 no . 3_766 H17 H17 3.4981 no . 3_666 H18 F3 2.7505 no . 3_666 H18 F7 3.3714 no . 3_665 H18 O2 3.2275 no . 2_655 H18 C5 3.5885 no . 1_455 H18 C6 3.2885 no . 1_455 H18 C14 3.4448 no . 1_455 H18 H2 3.3299 no . . H18 H5 3.2108 no . 1_455 H18 H6 2.7301 no . 1_455 H18 H13 3.3933 no . 1_455 H18 H14 2.9361 no . 1_455 H19 F5 2.6984 no . . H19 F5 2.7196 no . 3_665 H19 F7 3.3513 no . 3_665 H19 C10 3.3943 no . . H19 C13 3.3969 no . 1_455 H19 C14 3.3652 no . 1_455 H19 H10 2.6837 no . . H19 H13 2.6922 no . 1_455 H19 H14 2.5924 no . 1_455 H20 F2 2.5928 no . 4_554 H20 F5 3.0842 no . . H20 F8 2.8949 no . . H20 C10 3.5460 no . . H20 C11 3.4084 no . . H20 B2 3.3719 no . . H20 H1 3.3465 no . 2_645 H20 H8 2.7892 no . 2_645 H20 H10 3.0333 no . . H20 H11 2.6078 no . . H20 H15 3.3143 no . 3_765 H21 F2 2.6641 no . 4_554 H21 F7 2.6673 no . 4_555 H21 C1 3.3796 no . 2_645 H21 C8 3.5209 no . 2_645 H21 H1 2.6600 no . 2_645 H21 H3 3.4300 no . . H21 H8 2.9117 no . 2_645 H21 H9 3.0728 no . 2_645 H21 H11 3.5773 no . . H21 H16 3.2957 no . 2_645 H22 F1 3.2023 no . . H22 F4 2.5913 no . . H22 F6 2.8547 no . 4_555 H22 F7 3.4096 no . 4_555 H22 C7 3.5585 no . 3_766 H22 C16 3.5536 no . 2_645 H22 B1 3.3417 no . . H22 H2 3.5599 no . . H22 H3 2.8187 no . . H22 H6 3.3845 no . 3_766 H22 H7 2.9165 no . 3_766 H22 H9 3.1813 no . 2_645 H22 H16 2.6587 no . 2_645 #============================================================================== #============================================================================== # Additional structures and associated data_? identifiers # should be added at this point if there is more than one # structure analysis in the CIF. #============================================================================== # End of CIF #============================================================================== _database_code_depnum_ccdc_archive 'CCDC 904367' ####################################################################### # # Cambridge Crystallographic Data Centre # CCDC # ####################################################################### # # This CIF contains data from an original supplementary publication # deposited with the CCDC, and may include chemical, crystal, # experimental, refinement, atomic coordinates, # anisotropic displacement parameters and molecular geometry data, # as required by the journal to which it was submitted. # # This CIF is provided on the understanding that it is used for bona # fide research purposes only. It may contain copyright material # of the CCDC or of third parties, and may not be copied or further # disseminated in any form, whether machine-readable or not, # except for the purpose of generating routine backup copies # on your local computer system. # # For further information on the CCDC, data deposition and # data retrieval see: # www.ccdc.cam.ac.uk # # Bona fide researchers may freely download Mercury and enCIFer # from this site to visualise CIF-encoded structures and # to carry out CIF format checking respectively. # data_1 _vrf_PLAT051_1 ; PROBLEM: Mu(calc) and Mu(CIF) Ratio Differs from 1.0 by . 10.38 % RESPONSE: This structure was treated via PLATON's SQUEEZE procedure. 4 CH2Cl2 molecules per unit cell that were omitted from the model were included in the formula for calculation of the intensive properties. ; _vrf_CHEMW03_1 ; PROBLEM: The ratio of given/expected molecular weight as calculated from the _atom_site* data lies outside the range 0.95 <> 1.05 RESPONSE: This structure was treated via PLATON's SQUEEZE procedure. 4 CH2Cl2 molecules per unit cell that were omitted from the model were included in the formula for calculation of the intensive properties. ; _vrf_PLAT041_1 ; PROBLEM: Calc. and Reported SumFormula Strings Differ RESPONSE: This structure was treated via PLATON's SQUEEZE procedure. 4 CH2Cl2 molecules per unit cell that were omitted from the model were included in the formula for calculation of the intensive properties. ; _vrf_PLAT068_1 ; PROBLEM: Reported F000 Differs from Calcd (or Missing)...RESPONSE: This structure was treated via PLATON's SQUEEZE procedure. 4 CH2Cl2 molecules per unit cell that were omitted from the model were included in the formula for calculation of the intensive properties. ; _vrf_FORMU01_1 ; PROBLEM: There is a discrepancy between the atom counts in the _chemical_formula_sum and the formula from the _atom_site* data. RESPONSE: This structure was treated via PLATON's SQUEEZE procedure. 4 CH2Cl2 molecules per unit cell that were omitted from the model were included in the formula for calculation of the intensive properties. ; _vrf_CELLZ01_1 ; PROBLEM: Difference between formula and atom_site contents detected. RESPONSE: This structure was treated via PLATON's SQUEEZE procedure. 4 CH2Cl2 molecules per unit cell that were omitted from the model were included in the formula for calculation of the intensive properties. ; _vrf_PLAT044_1 ; PROBLEM: Calculated and Reported Dx Differ .............. 0.0758 Check RESPONSE: This structure was treated via PLATON's SQUEEZE procedure. 4 CH2Cl2 molecules per unit cell that were omitted from the model were included in the formula for calculation of the intensive properties. ; _vrf_PLAT605_1 ; PROBLEM: Structure Contains Solvent Accessible VOIDS of . 261 A**3 RESPONSE: This structure was treated via PLATON's SQUEEZE procedure. Please see the "SQUEEZE RESULTS" in this CIF for details. ; _vrf_PLAT869_1 ; PROBLEM: ALERTS Related to the use of SQUEEZE Suppressed ! Info RESPONSE: This structure was treated via PLATON's SQUEEZE procedure. Please see the "SQUEEZE RESULTS" in this CIF for details. ; _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety 'C80 H68 P4 Pd2, 2(B F4), C H2 Cl2' _chemical_formula_sum 'C81 H70 B2 Cl2 F8 P4 Pd2' _chemical_formula_weight 1624.57 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' P P 0.1023 0.0942 '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' Pd Pd -0.9988 1.0072 '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' _symmetry_cell_setting monoclinic _symmetry_space_group_name_H-M 'C 1 2/c 1' _symmetry_space_group_name_Hall '-C 2yc' _symmetry_Int_Tables_number 15 loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, y, -z+1/2' 'x+1/2, y+1/2, z' '-x+1/2, y+1/2, -z+1/2' '-x, -y, -z' 'x, -y, z-1/2' '-x+1/2, -y+1/2, -z' 'x+1/2, -y+1/2, z-1/2' _cell_length_a 25.3856(12) _cell_length_b 24.7751(10) _cell_length_c 11.8833(6) _cell_angle_alpha 90.00 _cell_angle_beta 93.6780(10) _cell_angle_gamma 90.00 _cell_volume 7458.4(6) _cell_formula_units_Z 4 _cell_measurement_reflns_used 15270 _cell_measurement_theta_min 3.09 _cell_measurement_theta_max 27.48 _cell_measurement_temperature 123 _exptl_crystal_description platelet _exptl_crystal_colour brown _exptl_crystal_size_max 0.10 _exptl_crystal_size_mid 0.10 _exptl_crystal_size_min 0.10 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.447 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 3296 _exptl_absorpt_coefficient_mu 0.703 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.9330 _exptl_absorpt_correction_T_max 0.9330 _exptl_absorpt_process_details 'ABSCOR (Rigaku, 1995)' _exptl_special_details ; ? ; _diffrn_ambient_temperature 123(2) _diffrn_radiation_wavelength 0.71075 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'Mo K\a' _diffrn_measurement_method \w _diffrn_detector_area_resol_mean 10.000 _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 36530 _diffrn_reflns_av_R_equivalents 0.0764 _diffrn_reflns_av_sigmaI/netI 0.0688 _diffrn_reflns_limit_h_min -32 _diffrn_reflns_limit_h_max 32 _diffrn_reflns_limit_k_min -31 _diffrn_reflns_limit_k_max 32 _diffrn_reflns_limit_l_min -15 _diffrn_reflns_limit_l_max 15 _diffrn_reflns_theta_min 3.08 _diffrn_reflns_theta_max 27.48 _reflns_number_total 8540 _reflns_number_gt 5150 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'RAPID AUTO (Rigaku)' _computing_cell_refinement 'RAPID AUTO' _computing_data_reduction 'RAPID AUTO' _computing_structure_solution 'SIR92 (Altomare, et al., 1994)' _computing_structure_refinement 'SHELXL97 (Sheldrick, 2008)' _computing_publication_material 'CrystalStructure 4.0 (Rigaku, 2010)' _computing_molecular_graphics 'CrystalStructure 4.0' _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^)+(0.2000P)^2^+0.0000P] 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 8540 _refine_ls_number_parameters 408 _refine_ls_number_restraints 58 _refine_ls_R_factor_all 0.1153 _refine_ls_R_factor_gt 0.0727 _refine_ls_wR_factor_ref 0.2643 _refine_ls_wR_factor_gt 0.2067 _refine_ls_goodness_of_fit_ref 0.913 _refine_ls_restrained_S_all 0.914 _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 0.417306(18) 0.333051(17) 0.33543(3) 0.0442(2) Uani 1 1 d . . . P1 P 0.35061(6) 0.39708(6) 0.34070(12) 0.0455(4) Uani 1 1 d . . . P2 P 0.37106(8) 0.25323(7) 0.29859(13) 0.0538(4) Uani 1 1 d . . . F1 F 0.1586(8) 0.4404(7) 0.7852(16) 0.295(8) Uiso 1 1 d D . . F2 F 0.1565(11) 0.4890(10) 0.932(2) 0.424(14) Uiso 1 1 d D . . F3 F 0.1571(8) 0.5225(8) 0.7692(18) 0.325(9) Uiso 1 1 d D . . F4 F 0.0896(10) 0.4795(11) 0.796(3) 0.457(16) Uiso 1 1 d D . . C1 C 0.4968(2) 0.2944(2) 0.3114(4) 0.0449(12) Uani 1 1 d . . . H1 H 0.4992 0.2572 0.3440 0.054 Uiso 1 1 calc R . . C2 C 0.5003(2) 0.3344(2) 0.3957(5) 0.0444(13) Uani 1 1 d . . . H2 H 0.5155 0.3237 0.4673 0.053 Uiso 1 1 calc R . . C3 C 0.4837(3) 0.3890(2) 0.3856(5) 0.0479(13) Uani 1 1 d . . . H3 H 0.4790 0.4051 0.4614 0.057 Uiso 1 1 calc R . . C4 C 0.4919(2) 0.4307(2) 0.3029(5) 0.0450(12) Uani 1 1 d . . . H4 H 0.4841 0.4659 0.3292 0.054 Uiso 1 1 calc R . . C5 C 0.3124(3) 0.4001(3) 0.4656(5) 0.0558(17) Uani 1 1 d . . . C6 C 0.3239(3) 0.3637(3) 0.5541(5) 0.0640(19) Uani 1 1 d . . . H6 H 0.3484 0.3351 0.5468 0.077 Uiso 1 1 calc R . . C7 C 0.2981(4) 0.3712(4) 0.6542(6) 0.084(3) Uani 1 1 d . . . H7 H 0.3045 0.3468 0.7154 0.100 Uiso 1 1 calc R . . C8 C 0.2636(4) 0.4135(4) 0.6639(7) 0.092(3) Uani 1 1 d . . . H8 H 0.2470 0.4184 0.7325 0.110 Uiso 1 1 calc R . . C9 C 0.2529(3) 0.4483(4) 0.5784(7) 0.077(2) Uani 1 1 d . . . H9 H 0.2287 0.4770 0.5871 0.093 Uiso 1 1 calc R . . C10 C 0.2772(3) 0.4425(3) 0.4773(6) 0.0620(18) Uani 1 1 d . . . H10 H 0.2698 0.4672 0.4171 0.074 Uiso 1 1 calc R . . C11 C 0.3756(2) 0.4664(2) 0.3430(5) 0.0442(12) Uani 1 1 d . . . C12 C 0.3976(3) 0.4853(2) 0.4477(5) 0.0502(14) Uani 1 1 d . . . H12 H 0.3957 0.4635 0.5131 0.060 Uiso 1 1 calc R . . C13 C 0.4215(3) 0.5347(2) 0.4560(5) 0.0502(14) Uani 1 1 d . . . H13 H 0.4357 0.5471 0.5272 0.060 Uiso 1 1 calc R . . C14 C 0.4252(3) 0.5667(3) 0.3620(6) 0.0544(15) Uani 1 1 d . . . H14 H 0.4432 0.6003 0.3675 0.065 Uiso 1 1 calc R . . C15 C 0.4023(3) 0.5491(2) 0.2590(5) 0.0550(15) Uani 1 1 d . . . H15 H 0.4034 0.5716 0.1945 0.066 Uiso 1 1 calc R . . C16 C 0.3777(2) 0.4992(2) 0.2495(5) 0.0459(12) Uani 1 1 d . . . H16 H 0.3624 0.4876 0.1786 0.055 Uiso 1 1 calc R . . C17 C 0.3064(3) 0.3934(2) 0.2139(5) 0.0501(14) Uani 1 1 d . . . C18 C 0.3300(3) 0.3888(3) 0.1121(5) 0.0565(15) Uani 1 1 d . . . H18 H 0.3673 0.3863 0.1112 0.068 Uiso 1 1 calc R . . C19 C 0.2986(3) 0.3880(3) 0.0104(6) 0.070(2) Uani 1 1 d . . . H19 H 0.3146 0.3858 -0.0596 0.084 Uiso 1 1 calc R . . C20 C 0.2451(3) 0.3903(3) 0.0128(6) 0.0691(19) Uani 1 1 d . . . H20 H 0.2238 0.3898 -0.0559 0.083 Uiso 1 1 calc R . . C21 C 0.2214(3) 0.3934(3) 0.1137(6) 0.0693(19) Uani 1 1 d . . . H21 H 0.1840 0.3939 0.1143 0.083 Uiso 1 1 calc R . . C22 C 0.2521(3) 0.3958(3) 0.2147(5) 0.0541(15) Uani 1 1 d . . . H22 H 0.2358 0.3991 0.2841 0.065 Uiso 1 1 calc R . . C23 C 0.3000(3) 0.2542(3) 0.2720(6) 0.0607(17) Uani 1 1 d . . . C24 C 0.2741(3) 0.2404(3) 0.1688(6) 0.0660(19) Uani 1 1 d . . . H24 H 0.2939 0.2272 0.1093 0.079 Uiso 1 1 calc R . . C25 C 0.2194(3) 0.2457(3) 0.1524(6) 0.073(2) Uani 1 1 d . . . H25 H 0.2024 0.2368 0.0814 0.088 Uiso 1 1 calc R . . C26 C 0.1899(3) 0.2637(3) 0.2386(6) 0.074(2) Uani 1 1 d . . . H26 H 0.1527 0.2673 0.2272 0.089 Uiso 1 1 calc R . . C27 C 0.2154(3) 0.2764(3) 0.3421(6) 0.0652(19) Uani 1 1 d . . . H27 H 0.1953 0.2886 0.4018 0.078 Uiso 1 1 calc R . . C28 C 0.2691(3) 0.2716(3) 0.3597(6) 0.0594(17) Uani 1 1 d . . . H28 H 0.2856 0.2801 0.4315 0.071 Uiso 1 1 calc R . . C29 C 0.3820(3) 0.2084(3) 0.4191(6) 0.0592(16) Uani 1 1 d . . . C30 C 0.3572(4) 0.1574(3) 0.4173(7) 0.069(2) Uani 1 1 d . . . H30 H 0.3347 0.1469 0.3541 0.083 Uiso 1 1 calc R . . C31 C 0.3658(4) 0.1229(3) 0.5076(8) 0.089(3) Uani 1 1 d . . . H31 H 0.3492 0.0885 0.5065 0.107 Uiso 1 1 calc R . . C32 C 0.3993(4) 0.1383(4) 0.6019(8) 0.086(3) Uani 1 1 d . . . H32 H 0.4063 0.1140 0.6629 0.103 Uiso 1 1 calc R . . C33 C 0.4211(4) 0.1878(4) 0.6042(7) 0.074(2) Uani 1 1 d . . . H33 H 0.4420 0.1991 0.6692 0.089 Uiso 1 1 calc R . . C34 C 0.4136(3) 0.2232(3) 0.5120(5) 0.0626(18) Uani 1 1 d . . . H34 H 0.4305 0.2575 0.5140 0.075 Uiso 1 1 calc R . . C35 C 0.3968(3) 0.2191(3) 0.1795(6) 0.0686(18) Uani 1 1 d U . . C36 C 0.4215(5) 0.1693(3) 0.1885(10) 0.097(3) Uani 1 1 d U . . H36 H 0.4227 0.1502 0.2580 0.116 Uiso 1 1 calc R . . C37 C 0.4443(6) 0.1475(5) 0.0968(11) 0.134(4) Uani 1 1 d U . . H37 H 0.4618 0.1136 0.1038 0.161 Uiso 1 1 calc R . . C38 C 0.4420(6) 0.1746(5) -0.0062(11) 0.121(4) Uani 1 1 d U . . H38 H 0.4573 0.1590 -0.0694 0.145 Uiso 1 1 calc R . . C39 C 0.4174(4) 0.2244(5) -0.0159(7) 0.095(3) Uani 1 1 d U . . H39 H 0.4167 0.2432 -0.0857 0.115 Uiso 1 1 calc R . . C40 C 0.3936(3) 0.2472(4) 0.0752(6) 0.0717(19) Uani 1 1 d U . . H40 H 0.3756 0.2808 0.0677 0.086 Uiso 1 1 calc R . . B1 B 0.1400(12) 0.4840(10) 0.827(2) 0.31(2) Uiso 1 1 d D . . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 Pd1 0.0490(3) 0.0498(3) 0.0346(3) -0.00179(15) 0.00871(19) -0.01144(18) P1 0.0463(9) 0.0555(8) 0.0356(7) -0.0047(6) 0.0106(6) -0.0115(7) P2 0.0651(11) 0.0556(9) 0.0411(8) -0.0028(6) 0.0061(7) -0.0205(8) C1 0.046(3) 0.052(3) 0.038(3) 0.006(2) 0.011(2) 0.002(2) C2 0.035(3) 0.052(3) 0.045(3) 0.002(2) -0.004(2) -0.007(2) C3 0.053(4) 0.052(3) 0.040(3) -0.005(2) 0.013(3) -0.010(3) C4 0.038(3) 0.048(3) 0.050(3) -0.001(2) 0.012(2) -0.010(2) C5 0.055(4) 0.077(4) 0.036(3) -0.007(3) 0.012(3) -0.031(3) C6 0.076(5) 0.080(4) 0.038(3) -0.009(3) 0.015(3) -0.037(4) C7 0.122(8) 0.086(5) 0.045(4) -0.009(3) 0.028(4) -0.045(5) C8 0.093(7) 0.121(7) 0.067(5) -0.041(5) 0.040(5) -0.056(6) C9 0.073(5) 0.092(6) 0.070(5) -0.021(4) 0.032(4) -0.030(4) C10 0.059(4) 0.072(4) 0.058(4) -0.016(3) 0.029(3) -0.015(3) C11 0.030(3) 0.057(3) 0.046(3) -0.005(2) 0.008(2) -0.002(2) C12 0.052(4) 0.058(3) 0.041(3) -0.009(2) 0.011(3) -0.009(3) C13 0.046(3) 0.059(3) 0.046(3) -0.008(3) 0.009(3) -0.004(3) C14 0.055(4) 0.049(3) 0.059(4) -0.008(3) 0.004(3) -0.005(3) C15 0.062(4) 0.054(3) 0.049(3) 0.004(3) 0.010(3) 0.005(3) C16 0.047(3) 0.048(3) 0.043(3) 0.000(2) 0.010(2) -0.003(2) C17 0.059(4) 0.057(3) 0.034(3) -0.007(2) 0.006(3) -0.007(3) C18 0.057(4) 0.068(4) 0.045(3) -0.006(3) 0.008(3) -0.011(3) C19 0.081(6) 0.087(5) 0.043(4) -0.008(3) 0.008(3) -0.015(4) C20 0.071(5) 0.077(4) 0.058(4) -0.006(3) -0.011(4) -0.010(4) C21 0.062(5) 0.080(5) 0.065(5) -0.009(4) -0.004(4) -0.005(4) C22 0.049(4) 0.067(4) 0.047(3) -0.005(3) 0.008(3) -0.010(3) C23 0.076(5) 0.057(3) 0.050(4) 0.004(3) 0.010(3) -0.029(3) C24 0.070(5) 0.085(5) 0.044(3) -0.002(3) 0.009(3) -0.034(4) C25 0.071(5) 0.108(6) 0.040(3) 0.004(3) 0.000(3) -0.044(4) C26 0.069(5) 0.097(5) 0.056(4) 0.014(4) 0.002(4) -0.037(4) C27 0.062(5) 0.089(5) 0.046(3) 0.002(3) 0.009(3) -0.027(4) C28 0.066(5) 0.060(4) 0.054(4) -0.002(3) 0.009(3) -0.024(3) C29 0.066(4) 0.057(4) 0.055(4) 0.008(3) 0.012(3) -0.008(3) C30 0.079(6) 0.056(4) 0.072(5) 0.006(3) 0.006(4) -0.018(3) C31 0.113(8) 0.064(4) 0.092(6) 0.013(4) 0.018(6) -0.023(5) C32 0.096(7) 0.093(6) 0.069(5) 0.030(5) 0.007(5) -0.014(5) C33 0.077(6) 0.091(5) 0.054(4) 0.015(4) 0.000(4) -0.024(4) C34 0.071(5) 0.072(4) 0.045(3) 0.002(3) 0.003(3) -0.020(4) C35 0.076(5) 0.070(4) 0.061(4) -0.011(3) 0.009(4) -0.022(3) C36 0.129(9) 0.066(5) 0.100(6) -0.013(4) 0.046(6) -0.012(4) C37 0.199(13) 0.090(6) 0.121(8) -0.040(5) 0.071(8) -0.002(7) C38 0.132(10) 0.143(8) 0.092(6) -0.054(6) 0.043(7) -0.027(6) C39 0.091(7) 0.137(7) 0.061(4) -0.029(5) 0.020(4) -0.050(5) C40 0.072(5) 0.104(5) 0.039(3) -0.015(3) 0.006(3) -0.038(4) _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 C2 2.182(6) . ? Pd1 C3 2.234(6) . ? Pd1 C1 2.268(6) . ? Pd1 P1 2.3239(17) . ? Pd1 P2 2.3269(16) . ? P1 C5 1.826(6) . ? P1 C11 1.830(6) . ? P1 C17 1.823(6) . ? P2 C23 1.811(8) . ? P2 C35 1.807(8) . ? P2 C29 1.819(7) . ? F1 B1 1.291(18) . ? F2 B1 1.297(18) . ? F3 B1 1.271(18) . ? F4 B1 1.315(18) . ? C1 C2 1.408(8) . ? C1 C1 1.480(10) 2_655 ? C1 H1 1.0000 . ? C2 C3 1.419(8) . ? C2 H2 0.9500 . ? C3 C4 1.451(8) . ? C3 H3 1.0000 . ? C4 C4 1.347(11) 2_655 ? C4 H4 0.9500 . ? C5 C6 1.400(10) . ? C5 C10 1.394(11) . ? C6 C7 1.407(10) . ? C6 H6 0.9500 . ? C7 C8 1.377(15) . ? C7 H7 0.9500 . ? C8 C9 1.347(14) . ? C8 H8 0.9500 . ? C9 C10 1.392(9) . ? C9 H9 0.9500 . ? C10 H10 0.9500 . ? C11 C12 1.410(8) . ? C11 C16 1.381(8) . ? C12 C13 1.368(8) . ? C12 H12 0.9500 . ? C13 C14 1.377(9) . ? C13 H13 0.9500 . ? C14 C15 1.391(9) . ? C14 H14 0.9500 . ? C15 C16 1.386(9) . ? C15 H15 0.9500 . ? C16 H16 0.9500 . ? C17 C22 1.380(9) . ? C17 C18 1.389(8) . ? C18 C19 1.404(10) . ? C18 H18 0.9500 . ? C19 C20 1.364(11) . ? C19 H19 0.9500 . ? C20 C21 1.377(11) . ? C20 H20 0.9500 . ? C21 C22 1.391(10) . ? C21 H21 0.9500 . ? C22 H22 0.9500 . ? C23 C24 1.396(10) . ? C23 C28 1.412(10) . ? C24 C25 1.395(12) . ? C24 H24 0.9500 . ? C25 C26 1.382(11) . ? C25 H25 0.9500 . ? C26 C27 1.389(10) . ? C26 H26 0.9500 . ? C27 C28 1.371(11) . ? C27 H27 0.9500 . ? C28 H28 0.9500 . ? C29 C34 1.372(10) . ? C29 C30 1.411(9) . ? C30 C31 1.378(11) . ? C30 H30 0.9500 . ? C31 C32 1.415(13) . ? C31 H31 0.9500 . ? C32 C33 1.345(12) . ? C32 H32 0.9500 . ? C33 C34 1.407(10) . ? C33 H33 0.9500 . ? C34 H34 0.9500 . ? C35 C36 1.386(13) . ? C35 C40 1.420(11) . ? C36 C37 1.376(14) . ? C36 H36 0.9500 . ? C37 C38 1.395(19) . ? C37 H37 0.9500 . ? C38 C39 1.384(17) . ? C38 H38 0.9500 . ? C39 C40 1.394(11) . ? C39 H39 0.9500 . ? C40 H40 0.9500 . ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag C2 Pd1 C3 37.5(2) . . ? C2 Pd1 C1 36.8(2) . . ? C3 Pd1 C1 68.5(2) . . ? C2 Pd1 P1 132.12(15) . . ? C3 Pd1 P1 96.20(17) . . ? C1 Pd1 P1 161.31(15) . . ? C2 Pd1 P2 122.67(15) . . ? C3 Pd1 P2 160.15(18) . . ? C1 Pd1 P2 93.41(16) . . ? P1 Pd1 P2 103.04(6) . . ? C5 P1 C11 98.7(3) . . ? C5 P1 C17 110.1(3) . . ? C11 P1 C17 104.7(3) . . ? C5 P1 Pd1 118.4(3) . . ? C11 P1 Pd1 112.83(19) . . ? C17 P1 Pd1 110.8(2) . . ? C23 P2 C35 106.0(3) . . ? C23 P2 C29 104.2(3) . . ? C35 P2 C29 106.7(4) . . ? C23 P2 Pd1 120.4(2) . . ? C35 P2 Pd1 110.0(2) . . ? C29 P2 Pd1 108.7(2) . . ? C2 C1 C1 134.1(3) . 2_655 ? C2 C1 Pd1 68.2(3) . . ? C1 C1 Pd1 106.2(5) 2_655 . ? C2 C1 H1 112.0 . . ? C1 C1 H1 112.0 2_655 . ? Pd1 C1 H1 112.0 . . ? C1 C2 C3 127.3(6) . . ? C1 C2 Pd1 74.9(4) . . ? C3 C2 Pd1 73.3(4) . . ? C1 C2 H2 116.3 . . ? C3 C2 H2 116.3 . . ? Pd1 C2 H2 128.1 . . ? C2 C3 C4 133.0(5) . . ? C2 C3 Pd1 69.3(3) . . ? C4 C3 Pd1 113.6(4) . . ? C2 C3 H3 110.9 . . ? C4 C3 H3 110.9 . . ? Pd1 C3 H3 110.9 . . ? C4 C4 C3 134.2(3) 2_655 . ? C4 C4 H4 112.9 2_655 . ? C3 C4 H4 112.9 . . ? C6 C5 C10 121.0(6) . . ? C6 C5 P1 119.2(6) . . ? C10 C5 P1 119.3(5) . . ? C5 C6 C7 117.7(8) . . ? C5 C6 H6 121.1 . . ? C7 C6 H6 121.1 . . ? C8 C7 C6 120.2(8) . . ? C8 C7 H7 119.9 . . ? C6 C7 H7 119.9 . . ? C7 C8 C9 121.6(7) . . ? C7 C8 H8 119.2 . . ? C9 C8 H8 119.2 . . ? C10 C9 C8 120.4(9) . . ? C10 C9 H9 119.8 . . ? C8 C9 H9 119.8 . . ? C9 C10 C5 119.1(8) . . ? C9 C10 H10 120.5 . . ? C5 C10 H10 120.5 . . ? C12 C11 C16 118.8(5) . . ? C12 C11 P1 116.2(4) . . ? C16 C11 P1 124.8(4) . . ? C13 C12 C11 120.6(6) . . ? C13 C12 H12 119.7 . . ? C11 C12 H12 119.7 . . ? C14 C13 C12 120.7(6) . . ? C14 C13 H13 119.7 . . ? C12 C13 H13 119.7 . . ? C13 C14 C15 119.1(6) . . ? C13 C14 H14 120.4 . . ? C15 C14 H14 120.4 . . ? C16 C15 C14 120.8(6) . . ? C16 C15 H15 119.6 . . ? C14 C15 H15 119.6 . . ? C15 C16 C11 120.0(6) . . ? C15 C16 H16 120.0 . . ? C11 C16 H16 120.0 . . ? C22 C17 C18 119.8(6) . . ? C22 C17 P1 123.6(4) . . ? C18 C17 P1 116.5(5) . . ? C17 C18 C19 119.8(7) . . ? C17 C18 H18 120.1 . . ? C19 C18 H18 120.1 . . ? C20 C19 C18 119.5(7) . . ? C20 C19 H19 120.2 . . ? C18 C19 H19 120.2 . . ? C19 C20 C21 120.8(7) . . ? C19 C20 H20 119.6 . . ? C21 C20 H20 119.6 . . ? C20 C21 C22 120.1(7) . . ? C20 C21 H21 119.9 . . ? C22 C21 H21 119.9 . . ? C17 C22 C21 119.8(6) . . ? C17 C22 H22 120.1 . . ? C21 C22 H22 120.1 . . ? C24 C23 C28 118.0(7) . . ? C24 C23 P2 123.9(6) . . ? C28 C23 P2 118.0(5) . . ? C23 C24 C25 120.5(7) . . ? C23 C24 H24 119.7 . . ? C25 C24 H24 119.7 . . ? C26 C25 C24 120.6(7) . . ? C26 C25 H25 119.7 . . ? C24 C25 H25 119.7 . . ? C25 C26 C27 119.0(8) . . ? C25 C26 H26 120.5 . . ? C27 C26 H26 120.5 . . ? C28 C27 C26 121.2(7) . . ? C28 C27 H27 119.4 . . ? C26 C27 H27 119.4 . . ? C27 C28 C23 120.5(7) . . ? C27 C28 H28 119.7 . . ? C23 C28 H28 119.7 . . ? C34 C29 C30 119.3(7) . . ? C34 C29 P2 121.4(5) . . ? C30 C29 P2 119.3(6) . . ? C31 C30 C29 119.6(8) . . ? C31 C30 H30 120.2 . . ? C29 C30 H30 120.2 . . ? C30 C31 C32 120.5(7) . . ? C30 C31 H31 119.8 . . ? C32 C31 H31 119.8 . . ? C33 C32 C31 119.2(7) . . ? C33 C32 H32 120.4 . . ? C31 C32 H32 120.4 . . ? C32 C33 C34 121.2(7) . . ? C32 C33 H33 119.4 . . ? C34 C33 H33 119.4 . . ? C29 C34 C33 120.2(7) . . ? C29 C34 H34 119.9 . . ? C33 C34 H34 119.9 . . ? C36 C35 C40 120.4(8) . . ? C36 C35 P2 122.8(7) . . ? C40 C35 P2 116.8(6) . . ? C35 C36 C37 119.9(11) . . ? C35 C36 H36 120.0 . . ? C37 C36 H36 120.0 . . ? C38 C37 C36 120.7(12) . . ? C38 C37 H37 119.7 . . ? C36 C37 H37 119.7 . . ? C37 C38 C39 119.7(10) . . ? C37 C38 H38 120.1 . . ? C39 C38 H38 120.1 . . ? C40 C39 C38 120.9(10) . . ? C40 C39 H39 119.6 . . ? C38 C39 H39 119.6 . . ? C39 C40 C35 118.3(10) . . ? C39 C40 H40 120.8 . . ? C35 C40 H40 120.8 . . ? F1 B1 F3 106(2) . . ? F1 B1 F4 101(2) . . ? F3 B1 F4 106(2) . . ? F1 B1 F2 111(2) . . ? F3 B1 F2 111(2) . . ? F4 B1 F2 122(3) . . ? loop_ _geom_torsion_atom_site_label_1 _geom_torsion_atom_site_label_2 _geom_torsion_atom_site_label_3 _geom_torsion_atom_site_label_4 _geom_torsion _geom_torsion_site_symmetry_1 _geom_torsion_site_symmetry_2 _geom_torsion_site_symmetry_3 _geom_torsion_site_symmetry_4 _geom_torsion_publ_flag C2 Pd1 P1 C5 -87.0(3) . . . . ? C3 Pd1 P1 C5 -99.1(3) . . . . ? C1 Pd1 P1 C5 -132.9(5) . . . . ? P2 Pd1 P1 C5 76.0(2) . . . . ? C2 Pd1 P1 C11 27.5(3) . . . . ? C3 Pd1 P1 C11 15.4(3) . . . . ? C1 Pd1 P1 C11 -18.5(5) . . . . ? P2 Pd1 P1 C11 -169.5(2) . . . . ? C2 Pd1 P1 C17 144.5(3) . . . . ? C3 Pd1 P1 C17 132.5(3) . . . . ? C1 Pd1 P1 C17 98.6(5) . . . . ? P2 Pd1 P1 C17 -52.5(2) . . . . ? C2 Pd1 P2 C23 169.5(3) . . . . ? C3 Pd1 P2 C23 169.8(5) . . . . ? C1 Pd1 P2 C23 -166.6(3) . . . . ? P1 Pd1 P2 C23 4.5(3) . . . . ? C2 Pd1 P2 C35 -66.9(4) . . . . ? C3 Pd1 P2 C35 -66.6(5) . . . . ? C1 Pd1 P2 C35 -43.0(3) . . . . ? P1 Pd1 P2 C35 128.1(3) . . . . ? C2 Pd1 P2 C29 49.6(3) . . . . ? C3 Pd1 P2 C29 49.8(5) . . . . ? C1 Pd1 P2 C29 73.4(3) . . . . ? P1 Pd1 P2 C29 -115.5(3) . . . . ? C3 Pd1 C1 C2 26.2(3) . . . . ? P1 Pd1 C1 C2 62.8(6) . . . . ? P2 Pd1 C1 C2 -145.4(3) . . . . ? C2 Pd1 C1 C1 -131.6(4) . . . 2_655 ? C3 Pd1 C1 C1 -105.4(3) . . . 2_655 ? P1 Pd1 C1 C1 -68.8(6) . . . 2_655 ? P2 Pd1 C1 C1 83.0(2) . . . 2_655 ? C1 C1 C2 C3 37.3(13) 2_655 . . . ? Pd1 C1 C2 C3 -54.5(6) . . . . ? C1 C1 C2 Pd1 91.8(9) 2_655 . . . ? C3 Pd1 C2 C1 -137.5(5) . . . . ? P1 Pd1 C2 C1 -157.4(2) . . . . ? P2 Pd1 C2 C1 42.4(4) . . . . ? C1 Pd1 C2 C3 137.5(5) . . . . ? P1 Pd1 C2 C3 -19.9(4) . . . . ? P2 Pd1 C2 C3 179.8(3) . . . . ? C1 C2 C3 C4 -48.2(11) . . . . ? Pd1 C2 C3 C4 -103.4(7) . . . . ? C1 C2 C3 Pd1 55.2(6) . . . . ? C1 Pd1 C3 C2 -25.8(3) . . . . ? P1 Pd1 C3 C2 165.3(3) . . . . ? P2 Pd1 C3 C2 -0.4(7) . . . . ? C2 Pd1 C3 C4 129.1(6) . . . . ? C1 Pd1 C3 C4 103.3(5) . . . . ? P1 Pd1 C3 C4 -65.7(4) . . . . ? P2 Pd1 C3 C4 128.7(4) . . . . ? C2 C3 C4 C4 16.2(14) . . . 2_655 ? Pd1 C3 C4 C4 -66.9(11) . . . 2_655 ? C11 P1 C5 C6 -122.4(5) . . . . ? C17 P1 C5 C6 128.3(5) . . . . ? Pd1 P1 C5 C6 -0.4(6) . . . . ? C11 P1 C5 C10 49.6(6) . . . . ? C17 P1 C5 C10 -59.7(6) . . . . ? Pd1 P1 C5 C10 171.5(5) . . . . ? C10 C5 C6 C7 0.9(10) . . . . ? P1 C5 C6 C7 172.7(5) . . . . ? C5 C6 C7 C8 -1.2(11) . . . . ? C6 C7 C8 C9 1.1(13) . . . . ? C7 C8 C9 C10 -0.7(13) . . . . ? C8 C9 C10 C5 0.4(11) . . . . ? C6 C5 C10 C9 -0.5(10) . . . . ? P1 C5 C10 C9 -172.3(5) . . . . ? C5 P1 C11 C12 47.6(5) . . . . ? C17 P1 C11 C12 161.2(5) . . . . ? Pd1 P1 C11 C12 -78.3(5) . . . . ? C5 P1 C11 C16 -137.1(5) . . . . ? C17 P1 C11 C16 -23.5(6) . . . . ? Pd1 P1 C11 C16 97.0(5) . . . . ? C16 C11 C12 C13 -1.4(9) . . . . ? P1 C11 C12 C13 174.2(5) . . . . ? C11 C12 C13 C14 -0.8(10) . . . . ? C12 C13 C14 C15 2.7(10) . . . . ? C13 C14 C15 C16 -2.5(10) . . . . ? C14 C15 C16 C11 0.3(10) . . . . ? C12 C11 C16 C15 1.6(9) . . . . ? P1 C11 C16 C15 -173.6(5) . . . . ? C5 P1 C17 C22 3.5(7) . . . . ? C11 P1 C17 C22 -101.8(6) . . . . ? Pd1 P1 C17 C22 136.3(5) . . . . ? C5 P1 C17 C18 -177.7(5) . . . . ? C11 P1 C17 C18 77.1(5) . . . . ? Pd1 P1 C17 C18 -44.8(5) . . . . ? C22 C17 C18 C19 1.5(10) . . . . ? P1 C17 C18 C19 -177.4(5) . . . . ? C17 C18 C19 C20 -1.6(11) . . . . ? C18 C19 C20 C21 -0.1(12) . . . . ? C19 C20 C21 C22 1.9(12) . . . . ? C18 C17 C22 C21 0.3(10) . . . . ? P1 C17 C22 C21 179.1(5) . . . . ? C20 C21 C22 C17 -2.0(11) . . . . ? C35 P2 C23 C24 -11.1(7) . . . . ? C29 P2 C23 C24 -123.4(6) . . . . ? Pd1 P2 C23 C24 114.4(6) . . . . ? C35 P2 C23 C28 170.9(5) . . . . ? C29 P2 C23 C28 58.5(6) . . . . ? Pd1 P2 C23 C28 -63.6(5) . . . . ? C28 C23 C24 C25 2.4(10) . . . . ? P2 C23 C24 C25 -175.6(6) . . . . ? C23 C24 C25 C26 -1.3(11) . . . . ? C24 C25 C26 C27 -0.1(12) . . . . ? C25 C26 C27 C28 0.4(11) . . . . ? C26 C27 C28 C23 0.8(11) . . . . ? C24 C23 C28 C27 -2.2(10) . . . . ? P2 C23 C28 C27 176.0(5) . . . . ? C23 P2 C29 C34 -130.2(7) . . . . ? C35 P2 C29 C34 117.9(7) . . . . ? Pd1 P2 C29 C34 -0.6(7) . . . . ? C23 P2 C29 C30 49.6(7) . . . . ? C35 P2 C29 C30 -62.3(7) . . . . ? Pd1 P2 C29 C30 179.1(6) . . . . ? C34 C29 C30 C31 -1.2(13) . . . . ? P2 C29 C30 C31 179.1(7) . . . . ? C29 C30 C31 C32 0.1(15) . . . . ? C30 C31 C32 C33 2.3(16) . . . . ? C31 C32 C33 C34 -3.5(15) . . . . ? C30 C29 C34 C33 0.0(12) . . . . ? P2 C29 C34 C33 179.7(7) . . . . ? C32 C33 C34 C29 2.5(14) . . . . ? C23 P2 C35 C36 -113.1(8) . . . . ? C29 P2 C35 C36 -2.4(9) . . . . ? Pd1 P2 C35 C36 115.3(8) . . . . ? C23 P2 C35 C40 70.6(6) . . . . ? C29 P2 C35 C40 -178.8(6) . . . . ? Pd1 P2 C35 C40 -61.1(6) . . . . ? C40 C35 C36 C37 1.8(16) . . . . ? P2 C35 C36 C37 -174.5(10) . . . . ? C35 C36 C37 C38 -1(2) . . . . ? C36 C37 C38 C39 1(2) . . . . ? C37 C38 C39 C40 -1.6(18) . . . . ? C38 C39 C40 C35 2.2(13) . . . . ? C36 C35 C40 C39 -2.3(12) . . . . ? P2 C35 C40 C39 174.2(6) . . . . ? _diffrn_measured_fraction_theta_max 0.998 _diffrn_reflns_theta_full 27.48 _diffrn_measured_fraction_theta_full 0.998 _refine_diff_density_max 0.980 _refine_diff_density_min -1.791 _refine_diff_density_rms 0.142 # SQUEEZE RESULTS (APPEND TO CIF) # Note: Data are Listed for all Voids in the P1 Unit Cell # i.e. Centre of Gravity, Solvent Accessible Volume, # Recovered number of Electrons in the Void and # Details about the Squeezed Material loop_ _platon_squeeze_void_nr _platon_squeeze_void_average_x _platon_squeeze_void_average_y _platon_squeeze_void_average_z _platon_squeeze_void_volume _platon_squeeze_void_count_electrons _platon_squeeze_void_content 1 0.500 0.000 -0.022 259 37 ' ' 2 1.000 0.500 0.022 259 37 ' ' 3 1.000 0.183 0.250 88 27 ' ' 4 0.500 0.683 0.250 88 27 ' ' 5 0.500 0.317 0.750 88 27 ' ' 6 1.000 0.817 0.750 88 27 ' ' _platon_squeeze_details ; The cell contains 4 methylene chloride molecules which have been treated as a diffuse contribution to the overall scattering without specific atom positions by SQUEEZE/PLATON. ; _iucr_refine_instructions_details ; TITL COT-BPd3PPh3 CELL 0.71075 25.38563 24.77510 11.88330 90.000 93.678 90.000 ZERR 4 0.00119 0.00096 0.00056 0.000 0.001 0.000 LATT 7 SYMM -X, +Y, .50-Z SFAC C H P B F PD CL UNIT 324 280 16 8 32 8 8 SHEL 99999.000000 0.000000 L.S. 20 FMAP 2 PLAN -10 WPDB -2 HTAB BOND $H CONF LIST 4 TEMP -150.0 ACTA SIZE 0.100 0.100 0.100 DELU 0.0100 0.0100 C35 C36 C37 C38 C39 C40 SIMU 0.0400 0.0800 C35 C36 C37 C38 C39 C40 DFIX 1.3400 0.0200 B1 F1 DFIX 1.3400 0.0200 B1 F2 DFIX 1.3400 0.0200 B1 F4 DFIX 1.3400 0.0200 B1 F3 DANG 2.1076 0.0400 F1 F3 DANG 2.1211 0.0400 F1 F2 DANG 2.1137 0.0400 F1 F4 DANG 2.1382 0.0400 F2 F3 DANG 2.1441 0.0400 F2 F4 DANG 2.1219 0.0400 F3 F4 WGHT 0.200000 FVAR 2.33142 PD1 6 0.417306 0.333051 0.335430 11.00000 0.04905 0.04985 = 0.03459 -0.00179 0.00871 -0.01144 P1 3 0.350610 0.397081 0.340695 11.00000 0.04630 0.05555 = 0.03562 -0.00465 0.01061 -0.01154 P2 3 0.371064 0.253229 0.298592 11.00000 0.06506 0.05556 = 0.04108 -0.00283 0.00613 -0.02053 F1 5 0.158585 0.440447 0.785204 11.00000 0.29457 F2 5 0.156454 0.489001 0.932402 11.00000 0.42369 F3 5 0.157085 0.522522 0.769200 11.00000 0.32462 F4 5 0.089581 0.479544 0.795804 11.00000 0.45650 C1 1 0.496800 0.294374 0.311438 11.00000 0.04585 0.05171 = 0.03821 0.00558 0.01124 0.00168 AFIX 13 H1 2 0.499249 0.257179 0.344038 11.00000 -1.20000 AFIX 0 C2 1 0.500313 0.334405 0.395657 11.00000 0.03507 0.05186 = 0.04534 0.00167 -0.00412 -0.00689 AFIX 43 H2 2 0.515500 0.323671 0.467323 11.00000 -1.20000 AFIX 0 C3 1 0.483721 0.389001 0.385567 11.00000 0.05270 0.05229 = 0.03991 -0.00463 0.01346 -0.00978 AFIX 13 H3 2 0.479012 0.405121 0.461415 11.00000 -1.20000 AFIX 0 C4 1 0.491907 0.430744 0.302885 11.00000 0.03802 0.04789 = 0.05017 -0.00050 0.01176 -0.00966 AFIX 43 H4 2 0.484128 0.465887 0.329160 11.00000 -1.20000 AFIX 0 C5 1 0.312434 0.400060 0.465647 11.00000 0.05535 0.07696 = 0.03627 -0.00680 0.01154 -0.03144 C6 1 0.323945 0.363746 0.554114 11.00000 0.07588 0.07971 = 0.03772 -0.00932 0.01478 -0.03683 AFIX 43 H6 2 0.348354 0.335091 0.546775 11.00000 -1.20000 AFIX 0 C7 1 0.298123 0.371151 0.654237 11.00000 0.12194 0.08609 = 0.04543 -0.00896 0.02824 -0.04529 AFIX 43 H7 2 0.304496 0.346820 0.715385 11.00000 -1.20000 AFIX 0 C8 1 0.263649 0.413543 0.663885 11.00000 0.09259 0.12076 = 0.06665 -0.04133 0.04005 -0.05635 AFIX 43 H8 2 0.247009 0.418373 0.732535 11.00000 -1.20000 AFIX 0 C9 1 0.252935 0.448333 0.578406 11.00000 0.07289 0.09244 = 0.07028 -0.02121 0.03232 -0.02960 AFIX 43 H9 2 0.228688 0.477007 0.587143 11.00000 -1.20000 AFIX 0 C10 1 0.277187 0.442521 0.477298 11.00000 0.05934 0.07212 = 0.05781 -0.01561 0.02927 -0.01498 AFIX 43 H10 2 0.269812 0.467158 0.417080 11.00000 -1.20000 AFIX 0 C11 1 0.375629 0.466372 0.343037 11.00000 0.02983 0.05740 = 0.04608 -0.00511 0.00795 -0.00168 C12 1 0.397561 0.485265 0.447716 11.00000 0.05240 0.05848 = 0.04095 -0.00852 0.01139 -0.00852 AFIX 43 H12 2 0.395691 0.463473 0.513118 11.00000 -1.20000 AFIX 0 C13 1 0.421513 0.534703 0.455956 11.00000 0.04636 0.05889 = 0.04622 -0.00848 0.00872 -0.00445 AFIX 43 H13 2 0.435740 0.547098 0.527212 11.00000 -1.20000 AFIX 0 C14 1 0.425205 0.566669 0.362028 11.00000 0.05486 0.04912 = 0.05917 -0.00808 0.00396 -0.00520 AFIX 43 H14 2 0.443181 0.600291 0.367469 11.00000 -1.20000 AFIX 0 C15 1 0.402262 0.549081 0.259023 11.00000 0.06243 0.05448 = 0.04880 0.00360 0.00990 0.00521 AFIX 43 H15 2 0.403434 0.571557 0.194460 11.00000 -1.20000 AFIX 0 C16 1 0.377728 0.499188 0.249459 11.00000 0.04709 0.04818 = 0.04320 -0.00031 0.00979 -0.00306 AFIX 43 H16 2 0.362357 0.487555 0.178584 11.00000 -1.20000 AFIX 0 C17 1 0.306395 0.393374 0.213887 11.00000 0.05896 0.05729 = 0.03447 -0.00707 0.00633 -0.00731 C18 1 0.330030 0.388830 0.112053 11.00000 0.05712 0.06812 = 0.04498 -0.00581 0.00811 -0.01094 AFIX 43 H18 2 0.367343 0.386296 0.111207 11.00000 -1.20000 AFIX 0 C19 1 0.298639 0.387993 0.010394 11.00000 0.08061 0.08684 = 0.04292 -0.00844 0.00834 -0.01495 AFIX 43 H19 2 0.314619 0.385821 -0.059596 11.00000 -1.20000 AFIX 0 C20 1 0.245055 0.390318 0.012817 11.00000 0.07118 0.07667 = 0.05758 -0.00636 -0.01145 -0.00961 AFIX 43 H20 2 0.223793 0.389818 -0.055941 11.00000 -1.20000 AFIX 0 C21 1 0.221378 0.393382 0.113695 11.00000 0.06158 0.08017 = 0.06505 -0.00883 -0.00422 -0.00497 AFIX 43 H21 2 0.183976 0.393856 0.114256 11.00000 -1.20000 AFIX 0 C22 1 0.252108 0.395785 0.214733 11.00000 0.04861 0.06732 = 0.04691 -0.00510 0.00842 -0.01019 AFIX 43 H22 2 0.235782 0.399075 0.284138 11.00000 -1.20000 AFIX 0 C23 1 0.300034 0.254246 0.271951 11.00000 0.07603 0.05698 = 0.04998 0.00389 0.00997 -0.02910 C24 1 0.274117 0.240373 0.168820 11.00000 0.06978 0.08459 = 0.04428 -0.00220 0.00872 -0.03389 AFIX 43 H24 2 0.293868 0.227235 0.109334 11.00000 -1.20000 AFIX 0 C25 1 0.219443 0.245652 0.152430 11.00000 0.07111 0.10793 = 0.04007 0.00440 0.00048 -0.04404 AFIX 43 H25 2 0.202376 0.236770 0.081357 11.00000 -1.20000 AFIX 0 C26 1 0.189879 0.263678 0.238600 11.00000 0.06910 0.09705 = 0.05641 0.01418 0.00159 -0.03655 AFIX 43 H26 2 0.152666 0.267325 0.227222 11.00000 -1.20000 AFIX 0 C27 1 0.215404 0.276380 0.342092 11.00000 0.06152 0.08927 = 0.04555 0.00244 0.00912 -0.02717 AFIX 43 H27 2 0.195271 0.288578 0.401801 11.00000 -1.20000 AFIX 0 C28 1 0.269103 0.271645 0.359689 11.00000 0.06556 0.05964 = 0.05366 -0.00218 0.00918 -0.02386 AFIX 43 H28 2 0.285645 0.280136 0.431484 11.00000 -1.20000 AFIX 0 C29 1 0.381964 0.208406 0.419111 11.00000 0.06622 0.05695 = 0.05534 0.00809 0.01176 -0.00776 C30 1 0.357189 0.157400 0.417272 11.00000 0.07888 0.05600 = 0.07182 0.00580 0.00576 -0.01792 AFIX 43 H30 2 0.334663 0.146895 0.354142 11.00000 -1.20000 AFIX 0 C31 1 0.365847 0.122900 0.507564 11.00000 0.11310 0.06418 = 0.09180 0.01270 0.01766 -0.02339 AFIX 43 H31 2 0.349231 0.088530 0.506455 11.00000 -1.20000 AFIX 0 C32 1 0.399320 0.138327 0.601906 11.00000 0.09626 0.09313 = 0.06911 0.02960 0.00718 -0.01432 AFIX 43 H32 2 0.406289 0.114028 0.662893 11.00000 -1.20000 AFIX 0 C33 1 0.421150 0.187831 0.604158 11.00000 0.07683 0.09065 = 0.05448 0.01473 0.00007 -0.02425 AFIX 43 H33 2 0.442021 0.199085 0.669154 11.00000 -1.20000 AFIX 0 C34 1 0.413610 0.223219 0.511957 11.00000 0.07128 0.07190 = 0.04457 0.00232 0.00267 -0.02020 AFIX 43 H34 2 0.430472 0.257469 0.513963 11.00000 -1.20000 AFIX 0 C35 1 0.396836 0.219111 0.179510 11.00000 0.07577 0.06993 = 0.06059 -0.01061 0.00878 -0.02175 C36 1 0.421539 0.169261 0.188538 11.00000 0.12930 0.06641 = 0.10043 -0.01262 0.04646 -0.01188 AFIX 43 H36 2 0.422750 0.150154 0.257968 11.00000 -1.20000 AFIX 0 C37 1 0.444314 0.147471 0.096818 11.00000 0.19927 0.08973 = 0.12083 -0.04022 0.07121 -0.00200 AFIX 43 H37 2 0.461771 0.113604 0.103758 11.00000 -1.20000 AFIX 0 C38 1 0.442020 0.174609 -0.006199 11.00000 0.13214 0.14267 = 0.09174 -0.05439 0.04309 -0.02702 AFIX 43 H38 2 0.457314 0.158997 -0.069437 11.00000 -1.20000 AFIX 0 C39 1 0.417383 0.224356 -0.015949 11.00000 0.09085 0.13702 = 0.06059 -0.02908 0.02048 -0.04961 AFIX 43 H39 2 0.416687 0.243177 -0.085680 11.00000 -1.20000 AFIX 0 C40 1 0.393560 0.247237 0.075206 11.00000 0.07225 0.10422 = 0.03899 -0.01513 0.00551 -0.03829 AFIX 43 H40 2 0.375588 0.280804 0.067699 11.00000 -1.20000 AFIX 0 B1 4 0.140023 0.483977 0.827300 11.00000 0.31457 HKLF 4 REM COT-BPd3PPh3 REM R1 = 0.0727 for 5150 Fo > 4sig(Fo) and 0.1153 for all 8540 data REM 408 parameters refined using 58 restraints END WGHT 0.1391 0.0000 REM Highest difference peak 0.980, deepest hole -1.791, 1-sigma level 0.142 Q1 1 0.4721 0.3314 0.3770 11.00000 0.05 0.98 Q2 1 0.3705 0.3140 0.2861 11.00000 0.05 0.94 Q3 1 0.4110 0.2908 0.2667 11.00000 0.05 0.92 Q4 1 0.4221 0.2760 0.3339 11.00000 0.05 0.76 Q5 1 0.3896 0.2909 0.3587 11.00000 0.05 0.75 Q6 1 0.3618 0.3409 0.3064 11.00000 0.05 0.72 Q7 1 0.4099 0.3771 0.2698 11.00000 0.05 0.72 Q8 1 0.4380 0.3831 0.3178 11.00000 0.05 0.71 Q9 1 0.4252 0.2896 0.4029 11.00000 0.05 0.70 Q10 1 0.2204 0.4925 0.8225 11.00000 0.05 0.66 ; _database_code_depnum_ccdc_archive 'CCDC 962478'